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#\#CIF_1.0 ################################################################################ # # # This CIF is a part of the B-IncStrDB # # (Bilbao Incommensurate Structures Database) # # http://www.cryst.ehu.eus/bincstrdb/ # # # # Please note that the structure of the CIF file may differ from the one # # deposited, as it may have been modified to comply with the standard. The # # file has been validated against official dictionaries as well as local # # dictionaries including non-standard data names used by SHELXL (Sheldrick, # # G. M. (2008). Acta Cryst. A 64, 112-122) and JANA (Petricek, V., Dusek, M. # # and Palatinus, L. (2014), Z. Kristallogr. 229, 345-352). # # # # For comments and/or criticisms, please e-mail to administrador-bcs@ehu.es # # # ################################################################################ data_global #======================================================================= _audit_creation_method 'Jana2020 1.3.52' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_paper_category ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full 'Acta Crystallographica Section B' _journal_year 2024 _journal_volume 80 _journal_issue ? _journal_page_first 105 _journal_page_last 116 _journal_paper_doi https://doi.org/10.1107/S205252062400146X #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name 'Plana-Ruiz, Sergi' _publ_contact_author_address ;Servei de Recursos Cientifics i Tecnics, Universitat Rovira i Virgili, Avinguda Paisos Catalans 26, Tarragona, Catalonia 43007, Spain and Institut fur Angewandte Geowissenschaften, Technische Universitat Darmstadt, Petersenstrasse 23, Darmstadt, Hessen 64287, Germany ; _publ_contact_author_email sergi.plana@urv.cat _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Acta Crystallographica Section B' _publ_requested_category ? #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Three-dimensional electron diffraction on clinkers: the belite \a^'^~<i>H</i>~ incommensurate modulated structure ; loop_ _publ_author_name _publ_author_address 'Plana-Ruiz, Sergi ' ;Servei de Recursos Cientifics i Tecnics, Universitat Rovira i Virgili, Avinguda Paisos Catalans 26, Tarragona, Catalonia 43007, Spain and Institut fur Angewandte Geowissenschaften, Technische Universitat Darmstadt, Petersenstrasse 23, Darmstadt, Hessen 64287, Germany ; 'Gotz, Emilia' ;Institut fur Angewandte Geowissenschaften, Technische Universitat Darmstadt, Petersenstrasse 23, Darmstadt, Hessen 64287, Germany ; 'Neumann, Thomas' ;Schwenk Zement GmbH & Co. Kg, Laudenbacher Weg 5, Karlstadt, Bavaria 97753, Germany ; 'Schwesig, Peter' ;Master Builders Solutions Deutschland GmbH, Dr.-Albert-Frank-Strasse 32, Trostberg, Bavaria 83308, Germany ; 'Kolb, Ute' ;Institut fur Anorganische Chemie und Analytische Chemie, Johannes Gutenberg University of Mainz, Duesbergweg 10-14, Mainz, Rheinland-Pfalz 55128, Germany ; #======================================================================= data_0k_average_dyn #data_I #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Ca8 O16 Si4' _chemical_formula_weight 689 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P n m a' _space_group_name_Hall '-P -2xabc;-2yb;-2zac' _space_group_IT_number 62 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,-y,z+1/2 3 -x,y+1/2,-z 4 x+1/2,-y+1/2,-z+1/2 5 -x,-y,-z 6 x+1/2,y,-z+1/2 7 x,-y+1/2,z 8 -x+1/2,y+1/2,z+1/2 _cell_length_a 6.776 _cell_length_b 5.496 _cell_length_c 9.252 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 344.5527 _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 3.3204 _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 0 _exptl_crystal_description 'Nanocrystals of up to 500 nm in size' #======================================================================= # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 293 _diffrn_radiation_type electron _diffrn_radiation_wavelength 0.0197 _diffrn_measurement_device 'FEI Tecnai F30' _diffrn_measurement_device_type 'TEM' _diffrn_detector 'Gatan UltraScan4000' _diffrn_reflns_number 10028 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_radiation_probe electron #======================================================================= # 8. REFINEMENT DATA _refine_special_details ? _reflns_number_total 2439 _reflns_number_gt 1709 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_gt 0.0562 _refine_ls_R_factor_all 0.0787 _refine_ls_wR_factor_ref 0.0585 _refine_ls_goodness_of_fit_ref 2.03 _refine_ls_goodness_of_fit_gt 1.77 _refine_ls_number_reflns 2439 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_shift/su_max 0.0325 _refine_ls_shift/su_mean 0.0029 _refine_ls_extinction_method 'none' loop_ _atom_type_symbol _atom_type_scat_source Ca International_Tables_Vol_C O International_Tables_Vol_C Si International_Tables_Vol_C #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.66658(12) 0.75 0.5706(2) Uani 0.0251(6) 4 1 d . . . Ca2 Ca 0.49080(11) 0.25 0.79563(19) Uani 0.0161(5) 4 1 d . . . Si1 Si 0.78069(16) 0.25 0.4128(3) Uani 0.0158(7) 4 1 d . . . O1 O 0.7521(6) 0.5203(6) 0.8014(7) Uani 0.0258(18) 8 0.621(4) d . . . O2 O 0.6574(3) 0.3219(4) 0.5622(7) Uani 0.030(2) 8 0.5 d . . . O3 O 1.0073(3) 0.3122(5) 0.4500(7) Uani 0.024(2) 8 0.5 d . . . O1_2 O 0.8219(9) 0.5103(11) 0.8563(14) Uani 0.0258(18) 8 0.379(2) d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ca1 Ca 0.0123(4) 0.0387(6) 0.0244(17) 0 -0.0005(6) 0 Ca2 Ca 0.0090(4) 0.0275(5) 0.0118(14) 0 -0.0004(5) 0 Si1 Si 0.0114(5) 0.0201(7) 0.016(2) 0 0.0002(7) 0 O1 O 0.026(2) 0.0194(9) 0.032(5) -0.0089(13) 0.0070(18) -0.0099(17) O2 O 0.0141(11) 0.037(2) 0.039(6) -0.0012(8) 0.0088(17) 0.0096(17) O3 O 0.0159(11) 0.042(3) 0.014(5) -0.0063(8) 0.0023(15) -0.0050(14) O1_2 O 0.026(2) 0.0194(9) 0.032(5) -0.0089(13) 0.0070(18) -0.0099(17) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ca1 Ca1 . 3_646 3.7887(11) ? Ca1 Ca1 . 3_656 3.7887(11) ? Ca1 Ca2 . . 3.6476(15) ? Ca1 Ca2 . 1_565 3.6476(15) ? Ca1 Ca2 . 2_664 3.444(2) ? Ca1 Ca2 . 3_656 3.552(2) ? Ca1 Ca2 . 4_556 3.7296(11) ? Ca1 Ca2 . 4_566 3.7296(11) ? Ca1 Si1 . . 3.2064(16) ? Ca1 Si1 . 1_565 3.2064(16) ? Ca1 Si1 . 2_665 3.186(3) ? Ca1 Si1 . 3_656 3.0346(14) ? Ca1 O2 . . 2.355(2) ? Ca1 O2 . 7_565 2.355(2) ? Ca1 O3 . 3_756 2.244(2) ? Ca1 O3 . 5_766 2.244(2) ? Ca1 O1_2 . 2_664 2.446(11) ? Ca1 O1_2 . 8_654 2.446(11) ? Ca2 Ca2 . 4_456 3.4916(12) ? Ca2 Ca2 . 4_556 3.4916(12) ? Ca2 Si1 . 4_456 3.050(3) ? Ca2 O1 . . 2.312(4) ? Ca2 O1 . 4_456 2.373(4) ? Ca2 O1 . 6_456 2.373(4) ? Ca2 O1 . 7_555 2.312(4) ? Ca2 O3 . 4_456 2.381(7) ? Ca2 O3 . 6_456 2.381(7) ? Ca2 O1_2 . 4_456 2.309(9) ? Ca2 O1_2 . 6_456 2.309(9) ? Si1 O1 . 2_664 1.645(5) ? Si1 O1 . 8_644 1.645(5) ? Si1 O2 . . 1.663(6) ? Si1 O2 . 7_555 1.663(6) ? Si1 O3 . . 1.610(3) ? Si1 O3 . 7_555 1.610(3) ? Si1 O1_2 . 2_664 1.579(7) ? Si1 O1_2 . 8_644 1.579(7) ? O1 O1_2 . . 0.696(12) ? O2 O2 . 7_555 0.790(3) ? O3 O3 . 7_555 0.684(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Ca1 Ca1 Ca1 3_646 . 3_656 92.99(3) ? Ca1 Ca1 Ca2 3_646 . . 57.03(3) ? Ca1 Ca1 Ca2 3_646 . 1_565 123.28(3) ? Ca1 Ca1 Ca2 3_646 . 2_664 98.45(5) ? Ca1 Ca1 Ca2 3_646 . 3_656 59.48(3) ? Ca1 Ca1 Ca2 3_646 . 4_556 86.043(18) ? Ca1 Ca1 Ca2 3_646 . 4_566 178.93(5) ? Ca1 Ca1 Si1 3_646 . . 50.58(3) ? Ca1 Ca1 Si1 3_646 . 1_565 127.47(7) ? Ca1 Ca1 Si1 3_646 . 2_665 114.17(4) ? Ca1 Ca1 Si1 3_646 . 3_656 54.72(3) ? Ca1 Ca1 O2 3_646 . . 41.26(9) ? Ca1 Ca1 O2 3_646 . 7_565 134.23(10) ? Ca1 Ca1 O3 3_646 . 3_756 131.91(11) ? Ca1 Ca1 O3 3_646 . 5_766 116.55(10) ? Ca1 Ca1 O1_2 3_646 . 2_664 46.79(16) ? Ca1 Ca1 O1_2 3_646 . 8_654 99.4(2) ? Ca1 Ca1 Ca2 3_656 . . 123.28(3) ? Ca1 Ca1 Ca2 3_656 . 1_565 57.03(3) ? Ca1 Ca1 Ca2 3_656 . 2_664 98.45(5) ? Ca1 Ca1 Ca2 3_656 . 3_656 59.48(3) ? Ca1 Ca1 Ca2 3_656 . 4_556 178.93(5) ? Ca1 Ca1 Ca2 3_656 . 4_566 86.043(18) ? Ca1 Ca1 Si1 3_656 . . 127.47(7) ? Ca1 Ca1 Si1 3_656 . 1_565 50.58(3) ? Ca1 Ca1 Si1 3_656 . 2_665 114.17(4) ? Ca1 Ca1 Si1 3_656 . 3_656 54.72(3) ? Ca1 Ca1 O2 3_656 . . 134.23(10) ? Ca1 Ca1 O2 3_656 . 7_565 41.26(9) ? Ca1 Ca1 O3 3_656 . 3_756 116.55(10) ? Ca1 Ca1 O3 3_656 . 5_766 131.91(11) ? Ca1 Ca1 O1_2 3_656 . 2_664 99.4(2) ? Ca1 Ca1 O1_2 3_656 . 8_654 46.79(16) ? Ca2 Ca1 Ca2 . . 1_565 97.77(5) ? Ca2 Ca1 Ca2 . . 2_664 129.92(2) ? Ca2 Ca1 Ca2 . . 3_656 116.51(3) ? Ca2 Ca1 Ca2 . . 4_556 56.48(2) ? Ca2 Ca1 Ca2 . . 4_566 123.92(6) ? Ca2 Ca1 Si1 . . . 72.12(4) ? Ca2 Ca1 Si1 . . 1_565 169.84(6) ? Ca2 Ca1 Si1 . . 2_665 57.96(4) ? Ca2 Ca1 Si1 . . 3_656 69.21(4) ? Ca2 Ca1 O2 . . . 42.06(14) ? Ca2 Ca1 O2 . . 7_565 139.72(15) ? Ca2 Ca1 O3 . . 3_756 119.00(12) ? Ca2 Ca1 O3 . . 5_766 104.79(11) ? Ca2 Ca1 O1_2 . . 2_664 91.9(2) ? Ca2 Ca1 O1_2 . . 8_654 156.02(19) ? Ca2 Ca1 Ca2 1_565 . 2_664 129.92(2) ? Ca2 Ca1 Ca2 1_565 . 3_656 116.51(3) ? Ca2 Ca1 Ca2 1_565 . 4_556 123.92(6) ? Ca2 Ca1 Ca2 1_565 . 4_566 56.48(2) ? Ca2 Ca1 Si1 1_565 . . 169.84(6) ? Ca2 Ca1 Si1 1_565 . 1_565 72.12(4) ? Ca2 Ca1 Si1 1_565 . 2_665 57.96(4) ? Ca2 Ca1 Si1 1_565 . 3_656 69.21(4) ? Ca2 Ca1 O2 1_565 . . 139.72(15) ? Ca2 Ca1 O2 1_565 . 7_565 42.06(14) ? Ca2 Ca1 O3 1_565 . 3_756 104.79(11) ? Ca2 Ca1 O3 1_565 . 5_766 119.00(12) ? Ca2 Ca1 O1_2 1_565 . 2_664 156.02(19) ? Ca2 Ca1 O1_2 1_565 . 8_654 91.9(2) ? Ca2 Ca1 Ca2 2_664 . 3_656 59.85(4) ? Ca2 Ca1 Ca2 2_664 . 4_556 81.26(3) ? Ca2 Ca1 Ca2 2_664 . 4_566 81.26(3) ? Ca2 Ca1 Si1 2_664 . . 60.07(4) ? Ca2 Ca1 Si1 2_664 . 1_565 60.07(4) ? Ca2 Ca1 Si1 2_664 . 2_665 131.18(4) ? Ca2 Ca1 Si1 2_664 . 3_656 135.28(8) ? Ca2 Ca1 O2 2_664 . . 89.62(13) ? Ca2 Ca1 O2 2_664 . 7_565 89.62(13) ? Ca2 Ca1 O3 2_664 . 3_756 43.41(17) ? Ca2 Ca1 O3 2_664 . 5_766 43.41(17) ? Ca2 Ca1 O1_2 2_664 . 2_664 51.67(17) ? Ca2 Ca1 O1_2 2_664 . 8_654 51.67(17) ? Ca2 Ca1 Ca2 3_656 . 4_556 119.56(4) ? Ca2 Ca1 Ca2 3_656 . 4_566 119.56(4) ? Ca2 Ca1 Si1 3_656 . . 68.78(5) ? Ca2 Ca1 Si1 3_656 . 1_565 68.78(5) ? Ca2 Ca1 Si1 3_656 . 2_665 168.97(4) ? Ca2 Ca1 Si1 3_656 . 3_656 75.43(6) ? Ca2 Ca1 O2 3_656 . . 87.74(16) ? Ca2 Ca1 O2 3_656 . 7_565 87.74(16) ? Ca2 Ca1 O3 3_656 . 3_756 102.39(17) ? Ca2 Ca1 O3 3_656 . 5_766 102.39(17) ? Ca2 Ca1 O1_2 3_656 . 2_664 40.2(2) ? Ca2 Ca1 O1_2 3_656 . 8_654 40.2(2) ? Ca2 Ca1 Ca2 4_556 . 4_566 94.92(3) ? Ca2 Ca1 Si1 4_556 . . 51.51(5) ? Ca2 Ca1 Si1 4_556 . 1_565 129.83(3) ? Ca2 Ca1 Si1 4_556 . 2_665 66.68(4) ? Ca2 Ca1 Si1 4_556 . 3_656 124.86(4) ? Ca2 Ca1 O2 4_556 . . 44.79(9) ? Ca2 Ca1 O2 4_556 . 7_565 139.70(10) ? Ca2 Ca1 O3 4_556 . 3_756 63.92(10) ? Ca2 Ca1 O3 4_556 . 5_766 48.39(11) ? Ca2 Ca1 O1_2 4_556 . 2_664 79.59(19) ? Ca2 Ca1 O1_2 4_556 . 8_654 132.93(17) ? Ca2 Ca1 Si1 4_566 . . 129.83(3) ? Ca2 Ca1 Si1 4_566 . 1_565 51.51(5) ? Ca2 Ca1 Si1 4_566 . 2_665 66.68(4) ? Ca2 Ca1 Si1 4_566 . 3_656 124.86(4) ? Ca2 Ca1 O2 4_566 . . 139.70(10) ? Ca2 Ca1 O2 4_566 . 7_565 44.79(9) ? Ca2 Ca1 O3 4_566 . 3_756 48.39(11) ? Ca2 Ca1 O3 4_566 . 5_766 63.92(10) ? Ca2 Ca1 O1_2 4_566 . 2_664 132.93(17) ? Ca2 Ca1 O1_2 4_566 . 8_654 79.59(19) ? Si1 Ca1 Si1 . . 1_565 117.97(7) ? Si1 Ca1 Si1 . . 2_665 115.18(5) ? Si1 Ca1 Si1 . . 3_656 105.30(4) ? Si1 Ca1 O2 . . . 30.12(14) ? Si1 Ca1 O2 . . 7_565 147.95(17) ? Si1 Ca1 O3 . . 3_756 81.63(10) ? Si1 Ca1 O3 . . 5_766 66.00(10) ? Si1 Ca1 O1_2 . . 2_664 28.6(2) ? Si1 Ca1 O1_2 . . 8_654 97.2(2) ? Si1 Ca1 Si1 1_565 . 2_665 115.18(5) ? Si1 Ca1 Si1 1_565 . 3_656 105.30(4) ? Si1 Ca1 O2 1_565 . . 147.95(17) ? Si1 Ca1 O2 1_565 . 7_565 30.12(14) ? Si1 Ca1 O3 1_565 . 3_756 66.00(10) ? Si1 Ca1 O3 1_565 . 5_766 81.63(10) ? Si1 Ca1 O1_2 1_565 . 2_664 97.2(2) ? Si1 Ca1 O1_2 1_565 . 8_654 28.6(2) ? Si1 Ca1 Si1 2_665 . 3_656 93.54(7) ? Si1 Ca1 O2 2_665 . . 92.05(16) ? Si1 Ca1 O2 2_665 . 7_565 92.05(16) ? Si1 Ca1 O3 2_665 . 3_756 88.51(17) ? Si1 Ca1 O3 2_665 . 5_766 88.51(17) ? Si1 Ca1 O1_2 2_665 . 2_664 143.3(2) ? Si1 Ca1 O1_2 2_665 . 8_654 143.3(2) ? Si1 Ca1 O2 3_656 . . 88.58(5) ? Si1 Ca1 O2 3_656 . 7_565 88.58(5) ? Si1 Ca1 O3 3_656 . 3_756 171.01(8) ? Si1 Ca1 O3 3_656 . 5_766 171.01(8) ? Si1 Ca1 O1_2 3_656 . 2_664 94.18(15) ? Si1 Ca1 O1_2 3_656 . 8_654 94.18(15) ? O2 Ca1 O2 . . 7_565 175.15(19) ? O2 Ca1 O3 . . 3_756 100.10(9) ? O2 Ca1 O3 . . 5_766 82.59(9) ? O2 Ca1 O1_2 . . 2_664 52.4(3) ? O2 Ca1 O1_2 . . 8_654 123.9(3) ? O2 Ca1 O3 7_565 . 3_756 82.59(9) ? O2 Ca1 O3 7_565 . 5_766 100.10(9) ? O2 Ca1 O1_2 7_565 . 2_664 123.9(3) ? O2 Ca1 O1_2 7_565 . 8_654 52.4(3) ? O3 Ca1 O3 3_756 . 5_766 17.52(10) ? O3 Ca1 O1_2 3_756 . 2_664 89.4(2) ? O3 Ca1 O1_2 3_756 . 8_654 79.1(2) ? O3 Ca1 O1_2 5_766 . 2_664 79.1(2) ? O3 Ca1 O1_2 5_766 . 8_654 89.4(2) ? O1_2 Ca1 O1_2 2_664 . 8_654 71.6(3) ? Ca1 Ca2 Ca1 1_545 . . 97.77(5) ? Ca1 Ca2 Ca1 1_545 . 2_665 101.62(3) ? Ca1 Ca2 Ca1 1_545 . 3_646 63.49(4) ? Ca1 Ca2 Ca1 1_545 . 4_456 80.02(2) ? Ca1 Ca2 Ca1 1_545 . 4_466 159.53(5) ? Ca1 Ca2 Ca2 1_545 . 4_456 100.30(4) ? Ca1 Ca2 Ca2 1_545 . 4_556 62.94(3) ? Ca1 Ca2 Si1 1_545 . 4_456 131.09(3) ? Ca1 Ca2 O1 1_545 . . 104.31(12) ? Ca1 Ca2 O1 1_545 . 4_456 62.28(11) ? Ca1 Ca2 O1 1_545 . 6_456 118.58(15) ? Ca1 Ca2 O1 1_545 . 7_555 43.86(15) ? Ca1 Ca2 O3 1_545 . 4_456 116.15(7) ? Ca1 Ca2 O3 1_545 . 6_456 131.08(7) ? Ca1 Ca2 O1_2 1_545 . 4_456 49.28(17) ? Ca1 Ca2 O1_2 1_545 . 6_456 106.3(3) ? Ca1 Ca2 Ca1 . . 2_665 101.62(3) ? Ca1 Ca2 Ca1 . . 3_646 63.49(4) ? Ca1 Ca2 Ca1 . . 4_456 159.53(5) ? Ca1 Ca2 Ca1 . . 4_466 80.02(2) ? Ca1 Ca2 Ca2 . . 4_456 100.30(4) ? Ca1 Ca2 Ca2 . . 4_556 62.94(3) ? Ca1 Ca2 Si1 . . 4_456 131.09(3) ? Ca1 Ca2 O1 . . . 43.86(15) ? Ca1 Ca2 O1 . . 4_456 118.58(15) ? Ca1 Ca2 O1 . . 6_456 62.28(11) ? Ca1 Ca2 O1 . . 7_555 104.31(12) ? Ca1 Ca2 O3 . . 4_456 131.08(7) ? Ca1 Ca2 O3 . . 6_456 116.15(7) ? Ca1 Ca2 O1_2 . . 4_456 106.3(3) ? Ca1 Ca2 O1_2 . . 6_456 49.28(17) ? Ca1 Ca2 Ca1 2_665 . 3_646 155.09(4) ? Ca1 Ca2 Ca1 2_665 . 4_456 98.74(4) ? Ca1 Ca2 Ca1 2_665 . 4_466 98.74(4) ? Ca1 Ca2 Ca2 2_665 . 4_456 146.38(6) ? Ca1 Ca2 Ca2 2_665 . 4_556 61.61(4) ? Ca1 Ca2 Si1 2_665 . 4_456 70.21(5) ? Ca1 Ca2 O1 2_665 . . 57.77(15) ? Ca1 Ca2 O1 2_665 . 4_456 137.65(13) ? Ca1 Ca2 O1 2_665 . 6_456 137.65(13) ? Ca1 Ca2 O1 2_665 . 7_555 57.77(15) ? Ca1 Ca2 O3 2_665 . 4_456 40.37(6) ? Ca1 Ca2 O3 2_665 . 6_456 40.37(6) ? Ca1 Ca2 O1_2 2_665 . 4_456 141.60(19) ? Ca1 Ca2 O1_2 2_665 . 6_456 141.60(19) ? Ca1 Ca2 Ca1 3_646 . 4_456 98.03(4) ? Ca1 Ca2 Ca1 3_646 . 4_466 98.03(4) ? Ca1 Ca2 Ca2 3_646 . 4_456 58.54(4) ? Ca1 Ca2 Ca2 3_646 . 4_556 93.48(5) ? Ca1 Ca2 Si1 3_646 . 4_456 134.71(4) ? Ca1 Ca2 O1 3_646 . . 104.59(17) ? Ca1 Ca2 O1 3_646 . 4_456 55.56(15) ? Ca1 Ca2 O1 3_646 . 6_456 55.56(15) ? Ca1 Ca2 O1 3_646 . 7_555 104.59(17) ? Ca1 Ca2 O3 3_646 . 4_456 163.14(6) ? Ca1 Ca2 O3 3_646 . 6_456 163.14(6) ? Ca1 Ca2 O1_2 3_646 . 4_456 43.2(3) ? Ca1 Ca2 O1_2 3_646 . 6_456 43.2(3) ? Ca1 Ca2 Ca1 4_456 . 4_466 94.92(3) ? Ca1 Ca2 Ca2 4_456 . 4_456 60.57(2) ? Ca1 Ca2 Ca2 4_456 . 4_556 130.679(16) ? Ca1 Ca2 Si1 4_456 . 4_456 55.36(3) ? Ca1 Ca2 O1 4_456 . . 156.48(16) ? Ca1 Ca2 O1 4_456 . 4_456 42.49(15) ? Ca1 Ca2 O1 4_456 . 6_456 100.68(10) ? Ca1 Ca2 O1 4_456 . 7_555 88.28(10) ? Ca1 Ca2 O3 4_456 . 4_456 66.04(7) ? Ca1 Ca2 O3 4_456 . 6_456 78.78(8) ? Ca1 Ca2 O1_2 4_456 . 4_456 56.9(3) ? Ca1 Ca2 O1_2 4_456 . 6_456 111.50(16) ? Ca1 Ca2 Ca2 4_466 . 4_456 60.57(2) ? Ca1 Ca2 Ca2 4_466 . 4_556 130.679(16) ? Ca1 Ca2 Si1 4_466 . 4_456 55.36(3) ? Ca1 Ca2 O1 4_466 . . 88.28(10) ? Ca1 Ca2 O1 4_466 . 4_456 100.68(10) ? Ca1 Ca2 O1 4_466 . 6_456 42.49(15) ? Ca1 Ca2 O1 4_466 . 7_555 156.48(16) ? Ca1 Ca2 O3 4_466 . 4_456 78.78(8) ? Ca1 Ca2 O3 4_466 . 6_456 66.04(7) ? Ca1 Ca2 O1_2 4_466 . 4_456 111.50(16) ? Ca1 Ca2 O1_2 4_466 . 6_456 56.9(3) ? Ca2 Ca2 Ca2 4_456 . 4_556 152.01(7) ? Ca2 Ca2 Si1 4_456 . 4_456 76.17(5) ? Ca2 Ca2 O1 4_456 . . 138.48(10) ? Ca2 Ca2 O1 4_456 . 4_456 41.15(9) ? Ca2 Ca2 O1 4_456 . 6_456 41.15(9) ? Ca2 Ca2 O1 4_456 . 7_555 138.48(10) ? Ca2 Ca2 O3 4_456 . 4_456 106.54(7) ? Ca2 Ca2 O3 4_456 . 6_456 106.54(7) ? Ca2 Ca2 O1_2 4_456 . 4_456 51.09(16) ? Ca2 Ca2 O1_2 4_456 . 6_456 51.09(16) ? Ca2 Ca2 Si1 4_556 . 4_456 131.82(6) ? Ca2 Ca2 O1 4_556 . . 42.48(10) ? Ca2 Ca2 O1 4_556 . 4_456 124.75(13) ? Ca2 Ca2 O1 4_556 . 6_456 124.75(13) ? Ca2 Ca2 O1 4_556 . 7_555 42.48(10) ? Ca2 Ca2 O3 4_556 . 4_456 101.16(7) ? Ca2 Ca2 O3 4_556 . 6_456 101.16(7) ? Ca2 Ca2 O1_2 4_556 . 4_456 109.5(2) ? Ca2 Ca2 O1_2 4_556 . 6_456 109.5(2) ? Si1 Ca2 O1 4_456 . . 109.70(17) ? Si1 Ca2 O1 4_456 . 4_456 90.94(15) ? Si1 Ca2 O1 4_456 . 6_456 90.94(15) ? Si1 Ca2 O1 4_456 . 7_555 109.70(17) ? Si1 Ca2 O3 4_456 . 4_456 31.54(6) ? Si1 Ca2 O3 4_456 . 6_456 31.54(6) ? Si1 Ca2 O1_2 4_456 . 4_456 107.9(3) ? Si1 Ca2 O1_2 4_456 . 6_456 107.9(3) ? O1 Ca2 O1 . . 4_456 158.9(2) ? O1 Ca2 O1 . . 6_456 97.38(14) ? O1 Ca2 O1 . . 7_555 79.97(13) ? O1 Ca2 O3 . . 4_456 91.92(18) ? O1 Ca2 O3 . . 6_456 81.31(18) ? O1 Ca2 O1_2 . . 4_456 142.3(3) ? O1 Ca2 O1_2 . . 6_456 89.7(2) ? O1 Ca2 O1 4_456 . 6_456 77.53(14) ? O1 Ca2 O1 4_456 . 7_555 97.38(14) ? O1 Ca2 O3 4_456 . 4_456 108.43(16) ? O1 Ca2 O3 4_456 . 6_456 119.73(17) ? O1 Ca2 O1_2 4_456 . 4_456 17.0(3) ? O1 Ca2 O1_2 4_456 . 6_456 79.6(2) ? O1 Ca2 O1 6_456 . 7_555 158.9(2) ? O1 Ca2 O3 6_456 . 4_456 119.73(17) ? O1 Ca2 O3 6_456 . 6_456 108.43(16) ? O1 Ca2 O1_2 6_456 . 4_456 79.6(2) ? O1 Ca2 O1_2 6_456 . 6_456 17.0(3) ? O1 Ca2 O3 7_555 . 4_456 81.31(18) ? O1 Ca2 O3 7_555 . 6_456 91.92(18) ? O1 Ca2 O1_2 7_555 . 4_456 89.7(2) ? O1 Ca2 O1_2 7_555 . 6_456 142.3(3) ? O3 Ca2 O3 4_456 . 6_456 16.51(10) ? O3 Ca2 O1_2 4_456 . 4_456 122.4(3) ? O3 Ca2 O1_2 4_456 . 6_456 135.6(3) ? O3 Ca2 O1_2 6_456 . 4_456 135.6(3) ? O3 Ca2 O1_2 6_456 . 6_456 122.4(3) ? O1_2 Ca2 O1_2 4_456 . 6_456 76.6(3) ? Ca1 Si1 Ca1 1_545 . . 117.97(8) ? Ca1 Si1 Ca1 1_545 . 2_664 118.65(5) ? Ca1 Si1 Ca1 1_545 . 3_646 74.70(3) ? Ca1 Si1 Ca2 1_545 . 4_556 73.13(6) ? Ca1 Si1 O1 1_545 . 2_664 155.58(16) ? Ca1 Si1 O1 1_545 . 8_644 66.1(2) ? Ca1 Si1 O2 1_545 . . 72.78(11) ? Ca1 Si1 O2 1_545 . 7_555 45.30(9) ? Ca1 Si1 O3 1_545 . . 108.33(17) ? Ca1 Si1 O3 1_545 . 7_555 87.17(14) ? Ca1 Si1 O1_2 1_545 . 2_664 139.4(3) ? Ca1 Si1 O1_2 1_545 . 8_644 47.9(4) ? Ca1 Si1 Ca1 . . 2_664 118.65(5) ? Ca1 Si1 Ca1 . . 3_646 74.70(3) ? Ca1 Si1 Ca2 . . 4_556 73.13(6) ? Ca1 Si1 O1 . . 2_664 66.1(2) ? Ca1 Si1 O1 . . 8_644 155.58(16) ? Ca1 Si1 O2 . . . 45.30(9) ? Ca1 Si1 O2 . . 7_555 72.78(11) ? Ca1 Si1 O3 . . . 87.17(14) ? Ca1 Si1 O3 . . 7_555 108.33(17) ? Ca1 Si1 O1_2 . . 2_664 47.9(4) ? Ca1 Si1 O1_2 . . 8_644 139.4(3) ? Ca1 Si1 Ca1 2_664 . 3_646 99.34(7) ? Ca1 Si1 Ca2 2_664 . 4_556 145.74(5) ? Ca1 Si1 O1 2_664 . 2_664 52.6(2) ? Ca1 Si1 O1 2_664 . 8_644 52.6(2) ? Ca1 Si1 O2 2_664 . . 151.93(16) ? Ca1 Si1 O2 2_664 . 7_555 151.93(16) ? Ca1 Si1 O3 2_664 . . 96.1(2) ? Ca1 Si1 O3 2_664 . 7_555 96.1(2) ? Ca1 Si1 O1_2 2_664 . 2_664 73.8(5) ? Ca1 Si1 O1_2 2_664 . 8_644 73.8(5) ? Ca1 Si1 Ca2 3_646 . 4_556 114.92(9) ? Ca1 Si1 O1 3_646 . 2_664 84.08(15) ? Ca1 Si1 O1 3_646 . 8_644 84.08(15) ? Ca1 Si1 O2 3_646 . . 57.05(13) ? Ca1 Si1 O2 3_646 . 7_555 57.05(13) ? Ca1 Si1 O3 3_646 . . 160.3(2) ? Ca1 Si1 O3 3_646 . 7_555 160.3(2) ? Ca1 Si1 O1_2 3_646 . 2_664 65.0(2) ? Ca1 Si1 O1_2 3_646 . 8_644 65.0(2) ? Ca2 Si1 O1 4_556 . 2_664 128.11(18) ? Ca2 Si1 O1 4_556 . 8_644 128.11(18) ? Ca2 Si1 O2 4_556 . . 59.95(16) ? Ca2 Si1 O2 4_556 . 7_555 59.95(16) ? Ca2 Si1 O3 4_556 . . 50.6(2) ? Ca2 Si1 O3 4_556 . 7_555 50.6(2) ? Ca2 Si1 O1_2 4_556 . 2_664 119.9(4) ? Ca2 Si1 O1_2 4_556 . 8_644 119.9(4) ? O1 Si1 O1 2_664 . 8_644 100.3(3) ? O1 Si1 O2 2_664 . . 105.7(2) ? O1 Si1 O2 2_664 . 7_555 129.5(2) ? O1 Si1 O3 2_664 . . 95.7(2) ? O1 Si1 O3 2_664 . 7_555 115.2(2) ? O1 Si1 O1_2 2_664 . 2_664 24.8(4) ? O1 Si1 O1_2 2_664 . 8_644 111.9(5) ? O1 Si1 O2 8_644 . . 129.5(2) ? O1 Si1 O2 8_644 . 7_555 105.7(2) ? O1 Si1 O3 8_644 . . 115.2(2) ? O1 Si1 O3 8_644 . 7_555 95.7(2) ? O1 Si1 O1_2 8_644 . 2_664 111.9(5) ? O1 Si1 O1_2 8_644 . 8_644 24.8(4) ? O2 Si1 O2 . . 7_555 27.50(13) ? O2 Si1 O3 . . . 104.5(3) ? O2 Si1 O3 . . 7_555 110.6(3) ? O2 Si1 O1_2 . . 2_664 81.7(5) ? O2 Si1 O1_2 . . 8_644 104.6(4) ? O2 Si1 O3 7_555 . . 110.6(3) ? O2 Si1 O3 7_555 . 7_555 104.5(3) ? O2 Si1 O1_2 7_555 . 2_664 104.6(4) ? O2 Si1 O1_2 7_555 . 8_644 81.7(5) ? O3 Si1 O3 . . 7_555 24.51(14) ? O3 Si1 O1_2 . . 2_664 108.3(3) ? O3 Si1 O1_2 . . 8_644 131.9(3) ? O3 Si1 O1_2 7_555 . 2_664 131.9(3) ? O3 Si1 O1_2 7_555 . 8_644 108.3(3) ? O1_2 Si1 O1_2 2_664 . 8_644 113.1(4) ? Ca2 O1 Ca2 . . 4_556 96.37(14) ? Ca2 O1 Si1 . . 2_665 113.8(2) ? Ca2 O1 O1_2 . . . 119.1(8) ? Ca2 O1 Si1 4_556 . 2_665 144.1(3) ? Ca2 O1 O1_2 4_556 . . 76.3(8) ? Si1 O1 O1_2 2_665 . . 72.3(8) ? Ca1 O2 Si1 . . . 104.6(2) ? Ca1 O2 O2 . . 7_555 177.6(6) ? Si1 O2 O2 . . 7_555 76.3(6) ? Ca1 O3 Ca2 3_746 . 4_556 96.22(18) ? Ca1 O3 Si1 3_746 . . 152.7(3) ? Ca1 O3 O3 3_746 . 7_555 81.2(3) ? Ca2 O3 Si1 4_556 . . 97.8(2) ? Ca2 O3 O3 4_556 . 7_555 81.7(8) ? Si1 O3 O3 . . 7_555 77.7(3) ? Ca1 O1_2 Ca2 2_665 . 4_556 96.6(2) ? Ca1 O1_2 Si1 2_665 . 2_665 103.5(6) ? Ca1 O1_2 O1 2_665 . . 131.2(8) ? Ca2 O1_2 Si1 4_556 . 2_665 159.5(7) ? Ca2 O1_2 O1 4_556 . . 86.6(10) ? Si1 O1_2 O1 2_665 . . 82.9(6) ? #======================================================================= # CIFX: Changed following block name from global data_0k_modulated_dyn #data_I #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Ca8 O16 Si4' _chemical_formula_weight 689 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system orthorhombic _space_group_ssg_name 'Pnma(\a00)0ss' loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1+1/2,-x2,x3+1/2,-x4+1/2 3 -x1,x2+1/2,-x3,-x4+1/2 4 x1+1/2,-x2+1/2,-x3+1/2,x4 5 -x1,-x2,-x3,-x4 6 x1+1/2,x2,-x3+1/2,x4+1/2 7 x1,-x2+1/2,x3,x4+1/2 8 -x1+1/2,x2+1/2,x3+1/2,-x4 _cell_length_a 6.776 _cell_length_b 5.496 _cell_length_c 9.252 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 344.5527 _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.372500 0.000000 0.000000 _cell_formula_units_Z 1 _cell_measurement_temperature 293 _cell_special_details ? _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 3.3204 _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 0 _exptl_crystal_description 'Nanocrystals of up to 500 nm in size' #======================================================================= # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 293 _diffrn_radiation_type electron _diffrn_radiation_wavelength 0.0197 _diffrn_measurement_device 'FEI Tecnai F30' _diffrn_measurement_device_type 'TEM' _diffrn_detector 'Gatan UltraScan4000' _diffrn_reflns_number 29908 _diffrn_reflns_theta_min 0.1 _diffrn_reflns_theta_max 0.79 _diffrn_reflns_theta_full 0.72 _diffrn_measured_fraction_theta_max 0.8 _diffrn_measured_fraction_theta_full 0.8 _diffrn_reflns_av_unetI/netI 0.0758 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_index_m_1_min -1 _diffrn_reflns_limit_index_m_1_max 1 _diffrn_radiation_probe electron #======================================================================= # 8. REFINEMENT DATA _refine_special_details ? _reflns_number_total 7296 _reflns_number_gt 3733 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.1228 _refine_ls_wR_factor_gt 0.1122 _refine_ls_R_factor_all 0.1824 _refine_ls_wR_factor_ref 0.1197 _refine_ls_goodness_of_fit_ref 2.38 _refine_ls_goodness_of_fit_gt 3.10 _refine_ls_number_reflns 7296 _refine_ls_number_parameters 126 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_shift/su_max 0.0401 _refine_ls_shift/su_mean 0.0059 _refine_diff_density_max 21.89 _refine_diff_density_min -5.27 _refine_ls_extinction_method 'none' loop_ _atom_type_symbol _atom_type_scat_source Ca International_Tables_Vol_C O International_Tables_Vol_C Si International_Tables_Vol_C #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 1.16654(15) 0.75 0.5714(2) Uiso 0.0130(3) 4 1 d . . . Ca2 Ca 1.00881(13) 0.75 0.2045(2) Uiso 0.0069(3) 4 1 d . . . Si1 Si 0.7195(2) 0.75 0.5881(4) Uiso 0.0100(4) 4 1 d . . . O1 O 0.7772(3) 0.9827(3) 0.6781(5) Uiso 0.0150(5) 8 1 d . . . O2 O 0.8422(4) 0.6772(5) 0.4352(7) Uiso 0.0215(7) 8 0.5 d . . . O3 O 0.4913(4) 0.8101(4) 0.5485(6) Uiso 0.0194(7) 8 0.5 d . . . loop_ _atom_site_Fourier_wave_vector_seq_id _atom_site_Fourier_wave_vector_q1_coeff 1 1 loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w O2 0.0025(18) 0.5 O3 0.715(2) 0.5 loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Ca1x1 Ca1 x 1 Ca1y1 Ca1 y 1 Ca1z1 Ca1 z 1 Ca2x1 Ca2 x 1 Ca2y1 Ca2 y 1 Ca2z1 Ca2 z 1 Si1x1 Si1 x 1 Si1y1 Si1 y 1 Si1z1 Si1 z 1 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Ca1x1 0 0 Ca1y1 0.0281(3) -0.0237(3) Ca1z1 0 0 Ca2x1 0 0 Ca2y1 -0.0154(3) -0.0325(3) Ca2z1 0 0 Si1x1 0 0 Si1y1 -0.0170(4) -0.0178(4) Si1z1 0 0 O1x1 0.0382(5) -0.0264(5) O1y1 0.0049(5) -0.0207(5) O1z1 -0.0365(7) 0.0096(8) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_ssg_symmetry_1 _geom_bond_site_ssg_symmetry_2 _geom_bond_distance_av _geom_bond_distance_min _geom_bond_distance_max _geom_bond_publ_flag Ca1 Ca1 . 3_7465 3.793(2) 3.660(2) 3.931(2) ? Ca1 Ca1 . 3_7565 3.795(2) 3.660(2) 3.931(2) ? Ca1 Ca2 . . 3.561(3) 3.559(3) 3.563(3) ? Ca1 Ca2 . 2_7655 3.731(2) 3.493(2) 3.980(2) ? Ca1 Ca2 . 2_7755 3.734(2) 3.493(2) 3.980(2) ? Ca1 Ca2 . 3_7465 3.642(3) 3.638(3) 3.646(3) ? Ca1 Ca2 . 3_7565 3.642(3) 3.638(3) 3.646(3) ? Ca1 Ca2 . 4_5655 3.451(2) 3.449(2) 3.454(2) ? Ca1 Si1 . . 3.0343(17) 3.0332(17) 3.0354(17) ? Ca1 Si1 . 3_7465 3.213(3) 3.136(3) 3.291(3) ? Ca1 Si1 . 3_7565 3.214(3) 3.136(3) 3.291(3) ? Ca1 Si1 . 4_5665 3.175(4) 3.171(4) 3.179(4) ? Ca1 O1 . 3_7465 2.765(7) 2.340(7) 3.206(7) ? Ca1 O1 . 4_5665 2.751(7) 2.258(8) 3.259(8) ? Ca1 O1 . 5_7765 2.773(7) 2.340(7) 3.206(7) ? Ca1 O1 . 6_5565 2.761(7) 2.258(8) 3.259(8) ? Ca1 O2 . 3_7565 2.450(3) 2.225(3) 2.551(3) ? Ca1 O2 . 5_7665 2.448(3) 2.225(3) 2.551(3) ? Ca1 O3 . 1_6555 2.246(3) 2.215(3) 2.274(3) ? Ca1 O3 . 7_6655 2.246(3) 2.215(3) 2.274(3) ? Ca2 Ca2 . 4_4655 3.4988(14) 3.4911(14) 3.5066(14) ? Ca2 Ca2 . 4_5655 3.4987(14) 3.4910(14) 3.5066(14) ? Ca2 Si1 . 2_6645 3.332(3) 3.153(3) 3.516(3) ? Ca2 Si1 . 2_6745 3.335(3) 3.153(3) 3.516(3) ? Ca2 Si1 . 4_5655 3.068(4) 3.061(4) 3.076(4) ? Ca2 O1 . 2_6745 2.473(4) 2.370(4) 2.615(4) ? Ca2 O1 . 3_7465 2.357(5) 2.325(6) 2.410(6) ? Ca2 O1 . 5_7765 2.357(5) 2.325(6) 2.410(6) ? Ca2 O1 . 8_6445 2.473(4) 2.370(4) 2.615(4) ? Ca2 O2 . . 2.437(6) 2.423(6) 2.472(6) ? Ca2 O2 . 7_5655 2.437(6) 2.423(6) 2.472(6) ? Ca2 O3 . 4_5655 2.388(6) 2.361(6) 2.403(6) ? Ca2 O3 . 6_5555 2.388(6) 2.361(6) 2.403(6) ? Si1 O1 . . 1.611(6) 1.564(6) 1.669(6) ? Si1 O1 . 7_5655 1.611(6) 1.564(6) 1.669(6) ? Si1 O2 . . 1.682(6) 1.662(6) 1.721(6) ? Si1 O2 . 7_5655 1.683(6) 1.662(6) 1.721(6) ? Si1 O3 . . 1.618(3) 1.601(3) 1.651(3) ? Si1 O3 . 7_5655 1.617(3) 1.601(3) 1.651(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_ssg_symmetry_1 _geom_angle_site_ssg_symmetry_2 _geom_angle_site_ssg_symmetry_3 _geom_angle_av _geom_angle_min _geom_angle_max _geom_angle_publ_flag Ca1 Ca1 Ca1 3_7465 . 3_7565 92.77(5) 92.70(5) 92.84(5) ? Ca1 Ca1 Ca2 3_7465 . . 59.26(5) 57.97(5) 60.46(5) ? Ca1 Ca1 Ca2 3_7465 . 2_7655 86.29(5) 82.51(4) 90.06(5) ? Ca1 Ca1 Ca2 3_7465 . 2_7755 177.32(6) 175.27(6) 179.28(7) ? Ca1 Ca1 Ca2 3_7465 . 3_7465 57.18(5) 55.95(5) 58.45(5) ? Ca1 Ca1 Ca2 3_7465 . 3_7565 123.38(4) 122.19(4) 124.53(4) ? Ca1 Ca1 Ca2 3_7465 . 4_5655 98.22(6) 95.97(6) 100.46(6) ? Ca1 Ca1 Si1 3_7465 . . 54.78(6) 53.96(6) 55.62(6) ? Ca1 Ca1 Si1 3_7465 . 3_7465 50.52(4) 48.75(4) 52.31(4) ? Ca1 Ca1 Si1 3_7465 . 3_7565 127.01(9) 125.84(8) 128.11(9) ? Ca1 Ca1 Si1 3_7465 . 4_5665 114.44(7) 111.22(7) 117.53(7) ? Ca1 Ca1 O1 3_7465 . 3_7465 53.17(9) 48.02(11) 57.64(8) ? Ca1 Ca1 O1 3_7465 . 4_5665 96.74(10) 96.31(12) 97.17(9) ? Ca1 Ca1 O1 3_7465 . 5_7765 100.01(13) 98.38(14) 101.28(12) ? Ca1 Ca1 O1 3_7465 . 6_5565 142.08(13) 137.17(14) 146.11(12) ? Ca1 Ca1 O2 3_7465 . 3_7565 133.32(11) 132.48(11) 135.21(11) ? Ca1 Ca1 O2 3_7465 . 5_7665 40.55(9) 39.78(9) 42.39(9) ? Ca1 Ca1 O3 3_7465 . 1_6555 132.89(12) 126.94(12) 136.12(12) ? Ca1 Ca1 O3 3_7465 . 7_6655 114.69(11) 111.09(10) 121.01(11) ? Ca1 Ca1 Ca2 3_7565 . . 59.24(5) 57.97(5) 60.46(5) ? Ca1 Ca1 Ca2 3_7565 . 2_7655 177.34(6) 175.27(6) 179.28(7) ? Ca1 Ca1 Ca2 3_7565 . 2_7755 86.22(5) 82.51(4) 90.06(5) ? Ca1 Ca1 Ca2 3_7565 . 3_7465 123.40(4) 122.19(4) 124.53(4) ? Ca1 Ca1 Ca2 3_7565 . 3_7565 57.16(5) 55.95(5) 58.45(5) ? Ca1 Ca1 Ca2 3_7565 . 4_5655 98.20(6) 95.97(6) 100.46(6) ? Ca1 Ca1 Si1 3_7565 . . 54.76(6) 53.96(6) 55.62(6) ? Ca1 Ca1 Si1 3_7565 . 3_7465 127.02(9) 125.84(8) 128.11(9) ? Ca1 Ca1 Si1 3_7565 . 3_7565 50.49(4) 48.75(4) 52.31(4) ? Ca1 Ca1 Si1 3_7565 . 4_5665 114.39(7) 111.22(7) 117.53(7) ? Ca1 Ca1 O1 3_7565 . 3_7465 99.99(13) 98.38(14) 101.28(12) ? Ca1 Ca1 O1 3_7565 . 4_5665 142.02(13) 137.17(14) 146.11(12) ? Ca1 Ca1 O1 3_7565 . 5_7765 53.22(9) 48.02(11) 57.64(8) ? Ca1 Ca1 O1 3_7565 . 6_5565 96.75(10) 96.31(12) 97.17(9) ? Ca1 Ca1 O2 3_7565 . 3_7565 40.55(9) 39.78(9) 42.39(9) ? Ca1 Ca1 O2 3_7565 . 5_7665 133.32(11) 132.48(11) 135.21(11) ? Ca1 Ca1 O3 3_7565 . 1_6555 114.62(11) 111.09(10) 121.01(11) ? Ca1 Ca1 O3 3_7565 . 7_6655 132.83(12) 126.94(12) 136.12(12) ? Ca2 Ca1 Ca2 . . 2_7655 119.56(6) 116.38(6) 122.58(7) ? Ca2 Ca1 Ca2 . . 2_7755 119.50(6) 116.38(6) 122.58(7) ? Ca2 Ca1 Ca2 . . 3_7465 116.44(6) 113.93(6) 118.91(6) ? Ca2 Ca1 Ca2 . . 3_7565 116.41(6) 113.93(6) 118.91(6) ? Ca2 Ca1 Ca2 . . 4_5655 59.84(5) 59.72(5) 59.96(5) ? Ca2 Ca1 Si1 . . . 75.41(8) 75.37(8) 75.46(8) ? Ca2 Ca1 Si1 . . 3_7465 68.55(7) 66.30(7) 70.75(8) ? Ca2 Ca1 Si1 . . 3_7565 68.52(7) 66.30(7) 70.75(8) ? Ca2 Ca1 Si1 . . 4_5665 168.56(5) 168.11(5) 169.03(5) ? Ca2 Ca1 O1 . . 3_7465 40.96(11) 40.55(13) 41.44(10) ? Ca2 Ca1 O1 . . 4_5665 152.26(12) 149.78(11) 154.56(13) ? Ca2 Ca1 O1 . . 5_7765 40.96(11) 40.55(13) 41.44(10) ? Ca2 Ca1 O1 . . 6_5565 152.21(12) 149.78(11) 154.56(13) ? Ca2 Ca1 O2 . . 3_7565 86.48(15) 85.29(15) 89.25(15) ? Ca2 Ca1 O2 . . 5_7665 86.49(15) 85.29(15) 89.25(15) ? Ca2 Ca1 O3 . . 1_6555 101.45(16) 101.10(16) 101.99(16) ? Ca2 Ca1 O3 . . 7_6655 101.46(16) 101.10(16) 101.99(16) ? Ca2 Ca1 Ca2 2_7655 . 2_7755 94.70(4) 94.48(4) 94.93(4) ? Ca2 Ca1 Ca2 2_7655 . 3_7465 56.63(4) 54.56(4) 58.85(4) ? Ca2 Ca1 Ca2 2_7655 . 3_7565 123.98(7) 121.80(8) 126.00(7) ? Ca2 Ca1 Ca2 2_7655 . 4_5655 81.18(5) 79.20(5) 83.05(5) ? Ca2 Ca1 Si1 2_7655 . . 125.00(7) 121.28(7) 128.67(8) ? Ca2 Ca1 Si1 2_7655 . 3_7465 51.79(6) 49.06(6) 54.64(7) ? Ca2 Ca1 Si1 2_7655 . 3_7565 129.67(5) 127.16(5) 132.01(4) ? Ca2 Ca1 Si1 2_7655 . 4_5665 66.66(6) 64.97(6) 68.14(6) ? Ca2 Ca1 O1 2_7655 . 3_7465 78.90(12) 75.93(11) 82.16(13) ? Ca2 Ca1 O1 2_7655 . 4_5665 39.08(12) 35.85(11) 43.08(13) ? Ca2 Ca1 O1 2_7655 . 5_7765 126.15(10) 121.71(9) 131.55(12) ? Ca2 Ca1 O1 2_7655 . 6_5565 84.36(10) 81.07(9) 87.67(12) ? Ca2 Ca1 O2 2_7655 . 3_7565 138.60(10) 135.64(10) 142.63(11) ? Ca2 Ca1 O2 2_7655 . 5_7665 43.94(9) 41.17(9) 48.11(10) ? Ca2 Ca1 O3 2_7655 . 1_6555 65.11(9) 61.85(9) 66.59(9) ? Ca2 Ca1 O3 2_7655 . 7_6655 47.52(10) 46.03(10) 50.61(10) ? Ca2 Ca1 Ca2 2_7755 . 3_7465 124.00(7) 121.80(8) 126.00(7) ? Ca2 Ca1 Ca2 2_7755 . 3_7565 56.60(4) 54.56(4) 58.85(4) ? Ca2 Ca1 Ca2 2_7755 . 4_5655 81.17(5) 79.20(5) 83.05(5) ? Ca2 Ca1 Si1 2_7755 . . 124.93(7) 121.28(7) 128.67(8) ? Ca2 Ca1 Si1 2_7755 . 3_7465 129.69(5) 127.16(5) 132.01(4) ? Ca2 Ca1 Si1 2_7755 . 3_7565 51.75(6) 49.06(6) 54.64(7) ? Ca2 Ca1 Si1 2_7755 . 4_5665 66.64(6) 64.97(6) 68.14(6) ? Ca2 Ca1 O1 2_7755 . 3_7465 126.21(10) 121.71(9) 131.55(12) ? Ca2 Ca1 O1 2_7755 . 4_5665 84.42(10) 81.07(9) 87.67(12) ? Ca2 Ca1 O1 2_7755 . 5_7765 78.84(12) 75.93(11) 82.16(13) ? Ca2 Ca1 O1 2_7755 . 6_5565 39.03(12) 35.85(11) 43.08(13) ? Ca2 Ca1 O2 2_7755 . 3_7565 43.91(9) 41.17(9) 48.11(10) ? Ca2 Ca1 O2 2_7755 . 5_7665 138.64(10) 135.64(10) 142.63(11) ? Ca2 Ca1 O3 2_7755 . 1_6555 47.49(10) 46.03(10) 50.61(10) ? Ca2 Ca1 O3 2_7755 . 7_6655 65.08(9) 61.85(9) 66.59(9) ? Ca2 Ca1 Ca2 3_7465 . 3_7565 97.97(6) 97.97(6) 97.97(6) ? Ca2 Ca1 Ca2 3_7465 . 4_5655 129.86(6) 126.65(6) 133.05(6) ? Ca2 Ca1 Si1 3_7465 . . 69.23(6) 67.46(6) 70.97(6) ? Ca2 Ca1 Si1 3_7465 . 3_7465 72.24(7) 71.34(7) 73.13(7) ? Ca2 Ca1 Si1 3_7465 . 3_7565 170.12(8) 169.25(8) 171.03(8) ? Ca2 Ca1 Si1 3_7465 . 4_5665 58.10(6) 54.55(6) 61.63(6) ? Ca2 Ca1 O1 3_7465 . 3_7465 96.68(12) 93.98(13) 99.05(10) ? Ca2 Ca1 O1 3_7465 . 4_5665 42.01(9) 39.54(10) 44.09(7) ? Ca2 Ca1 O1 3_7465 . 5_7765 156.81(13) 154.03(13) 158.76(12) ? Ca2 Ca1 O1 3_7465 . 6_5565 87.47(13) 83.34(14) 91.04(12) ? Ca2 Ca1 O2 3_7465 . 3_7565 139.46(15) 139.43(14) 139.55(16) ? Ca2 Ca1 O2 3_7465 . 5_7665 41.57(13) 41.52(13) 41.67(15) ? Ca2 Ca1 O3 3_7465 . 1_6555 119.91(12) 115.21(12) 123.06(12) ? Ca2 Ca1 O3 3_7465 . 7_6655 104.46(11) 101.05(11) 109.34(12) ? Ca2 Ca1 Ca2 3_7565 . 4_5655 129.84(6) 126.65(6) 133.05(6) ? Ca2 Ca1 Si1 3_7565 . . 69.20(6) 67.46(6) 70.97(6) ? Ca2 Ca1 Si1 3_7565 . 3_7465 170.14(8) 169.25(8) 171.03(8) ? Ca2 Ca1 Si1 3_7565 . 3_7565 72.22(7) 71.34(7) 73.13(7) ? Ca2 Ca1 Si1 3_7565 . 4_5665 58.06(6) 54.55(6) 61.63(6) ? Ca2 Ca1 O1 3_7565 . 3_7465 156.78(13) 154.03(13) 158.76(12) ? Ca2 Ca1 O1 3_7565 . 4_5665 87.43(13) 83.34(14) 91.04(12) ? Ca2 Ca1 O1 3_7565 . 5_7765 96.70(12) 93.98(13) 99.05(10) ? Ca2 Ca1 O1 3_7565 . 6_5565 42.05(9) 39.54(10) 44.09(7) ? Ca2 Ca1 O2 3_7565 . 3_7565 41.57(13) 41.52(13) 41.67(15) ? Ca2 Ca1 O2 3_7565 . 5_7665 139.47(15) 139.43(14) 139.55(16) ? Ca2 Ca1 O3 3_7565 . 1_6555 104.40(11) 101.05(11) 109.34(12) ? Ca2 Ca1 O3 3_7565 . 7_6655 119.85(12) 115.21(12) 123.06(12) ? Ca2 Ca1 Si1 4_5655 . . 135.14(10) 135.05(10) 135.22(10) ? Ca2 Ca1 Si1 4_5655 . 3_7465 59.89(6) 56.55(6) 63.26(6) ? Ca2 Ca1 Si1 4_5655 . 3_7565 59.89(6) 56.55(6) 63.26(6) ? Ca2 Ca1 Si1 4_5655 . 4_5665 131.00(5) 130.76(5) 131.25(5) ? Ca2 Ca1 O1 4_5655 . 3_7465 45.12(9) 41.63(8) 49.26(11) ? Ca2 Ca1 O1 4_5655 . 4_5665 116.48(11) 110.64(11) 122.83(12) ? Ca2 Ca1 O1 4_5655 . 5_7765 45.06(9) 41.63(8) 49.26(11) ? Ca2 Ca1 O1 4_5655 . 6_5565 116.40(11) 110.64(11) 122.83(12) ? Ca2 Ca1 O2 4_5655 . 3_7565 90.19(13) 86.68(12) 93.12(14) ? Ca2 Ca1 O2 4_5655 . 5_7665 90.21(13) 86.68(12) 93.12(14) ? Ca2 Ca1 O3 4_5655 . 1_6555 43.45(15) 42.67(15) 43.89(15) ? Ca2 Ca1 O3 4_5655 . 7_6655 43.45(15) 42.67(15) 43.89(15) ? Si1 Ca1 Si1 . . 3_7465 105.29(7) 102.94(7) 107.60(7) ? Si1 Ca1 Si1 . . 3_7565 105.25(7) 102.94(7) 107.60(7) ? Si1 Ca1 Si1 . . 4_5665 93.54(9) 93.47(9) 93.62(9) ? Si1 Ca1 O1 . . 3_7465 99.99(11) 95.10(12) 104.30(11) ? Si1 Ca1 O1 . . 4_5665 102.86(12) 98.93(13) 106.23(11) ? Si1 Ca1 O1 . . 5_7765 100.03(11) 95.10(12) 104.30(11) ? Si1 Ca1 O1 . . 6_5565 102.91(12) 98.93(13) 106.23(11) ? Si1 Ca1 O2 . . 3_7565 87.28(9) 86.52(8) 88.65(9) ? Si1 Ca1 O2 . . 5_7665 87.29(9) 86.52(8) 88.65(9) ? Si1 Ca1 O3 . . 1_6555 168.89(12) 164.42(11) 176.42(15) ? Si1 Ca1 O3 . . 7_6655 168.98(12) 164.42(11) 176.42(15) ? Si1 Ca1 Si1 3_7465 . 3_7565 117.54(10) 117.52(10) 117.56(10) ? Si1 Ca1 Si1 3_7465 . 4_5665 115.44(9) 111.35(9) 119.45(9) ? Si1 Ca1 O1 3_7465 . 3_7465 29.67(12) 29.32(12) 30.16(14) ? Si1 Ca1 O1 3_7465 . 4_5665 85.90(13) 82.46(12) 89.87(14) ? Si1 Ca1 O1 3_7465 . 5_7765 92.27(13) 89.65(12) 95.23(15) ? Si1 Ca1 O1 3_7465 . 6_5565 135.95(11) 134.83(10) 137.46(13) ? Si1 Ca1 O2 3_7465 . 3_7565 147.56(16) 147.27(16) 148.11(18) ? Si1 Ca1 O2 3_7465 . 5_7665 30.13(14) 29.84(13) 30.67(15) ? Si1 Ca1 O3 3_7465 . 1_6555 81.84(10) 77.04(10) 85.29(10) ? Si1 Ca1 O3 3_7465 . 7_6655 65.35(10) 61.87(10) 70.09(10) ? Si1 Ca1 Si1 3_7565 . 4_5665 115.38(9) 111.35(9) 119.45(9) ? Si1 Ca1 O1 3_7565 . 3_7465 92.30(13) 89.65(12) 95.23(15) ? Si1 Ca1 O1 3_7565 . 4_5665 135.97(11) 134.83(10) 137.46(13) ? Si1 Ca1 O1 3_7565 . 5_7765 29.67(12) 29.32(12) 30.16(14) ? Si1 Ca1 O1 3_7565 . 6_5565 85.86(13) 82.46(12) 89.87(14) ? Si1 Ca1 O2 3_7565 . 3_7565 30.12(14) 29.84(13) 30.67(15) ? Si1 Ca1 O2 3_7565 . 5_7665 147.56(16) 147.27(16) 148.11(18) ? Si1 Ca1 O3 3_7565 . 1_6555 65.29(10) 61.87(10) 70.09(10) ? Si1 Ca1 O3 3_7565 . 7_6655 81.78(10) 77.04(10) 85.29(10) ? Si1 Ca1 O1 4_5665 . 3_7465 144.45(13) 140.61(13) 148.52(14) ? Si1 Ca1 O1 4_5665 . 4_5665 29.74(12) 29.15(11) 30.42(13) ? Si1 Ca1 O1 4_5665 . 5_7765 144.38(13) 140.61(13) 148.52(14) ? Si1 Ca1 O1 4_5665 . 6_5565 29.73(12) 29.15(11) 30.42(13) ? Si1 Ca1 O2 4_5665 . 3_7565 90.97(16) 87.55(15) 95.59(17) ? Si1 Ca1 O2 4_5665 . 5_7665 91.00(16) 87.55(15) 95.59(17) ? Si1 Ca1 O3 4_5665 . 1_6555 88.98(16) 88.16(16) 89.39(16) ? Si1 Ca1 O3 4_5665 . 7_6655 88.99(16) 88.16(16) 89.39(16) ? O1 Ca1 O1 3_7465 . 4_5665 115.04(16) 111.56(15) 119.18(18) ? O1 Ca1 O1 3_7465 . 5_7765 64.81(16) 64.19(16) 65.43(16) ? O1 Ca1 O1 3_7465 . 6_5565 156.45(13) 150.10(12) 161.81(14) ? O1 Ca1 O2 3_7465 . 3_7565 121.3(2) 119.93(19) 122.1(2) ? O1 Ca1 O2 3_7465 . 5_7665 57.30(17) 55.58(18) 58.15(17) ? O1 Ca1 O3 3_7465 . 1_6555 86.65(16) 79.61(16) 89.97(17) ? O1 Ca1 O3 3_7465 . 7_6655 69.39(16) 67.02(15) 75.36(16) ? O1 Ca1 O1 4_5665 . 5_7765 156.45(13) 150.10(12) 161.81(14) ? O1 Ca1 O1 4_5665 . 6_5565 55.52(14) 55.30(14) 55.72(14) ? O1 Ca1 O2 4_5665 . 3_7565 119.67(19) 116.76(19) 121.81(19) ? O1 Ca1 O2 4_5665 . 5_7665 64.61(17) 62.18(16) 66.82(19) ? O1 Ca1 O3 4_5665 . 1_6555 84.14(16) 77.43(16) 89.89(17) ? O1 Ca1 O3 4_5665 . 7_6655 75.15(17) 69.29(16) 82.29(18) ? O1 Ca1 O1 5_7765 . 6_5565 114.98(16) 111.56(15) 119.18(18) ? O1 Ca1 O2 5_7765 . 3_7565 57.30(17) 55.58(18) 58.15(17) ? O1 Ca1 O2 5_7765 . 5_7665 121.3(2) 119.93(19) 122.1(2) ? O1 Ca1 O3 5_7765 . 1_6555 69.36(16) 67.02(15) 75.36(16) ? O1 Ca1 O3 5_7765 . 7_6655 86.62(16) 79.61(16) 89.97(17) ? O1 Ca1 O2 6_5565 . 3_7565 64.60(16) 62.18(16) 66.82(19) ? O1 Ca1 O2 6_5565 . 5_7665 119.68(19) 116.76(19) 121.81(19) ? O1 Ca1 O3 6_5565 . 1_6555 75.05(17) 69.29(16) 82.29(18) ? O1 Ca1 O3 6_5565 . 7_6655 84.03(16) 77.43(16) 89.89(17) ? O2 Ca1 O3 3_7565 . 1_6555 80.60(10) 77.66(10) 86.06(11) ? O2 Ca1 O3 3_7565 . 7_6655 95.47(10) 94.81(10) 96.28(10) ? O2 Ca1 O3 5_7665 . 1_6555 95.47(10) 94.81(10) 96.28(10) ? O2 Ca1 O3 5_7665 . 7_6655 80.66(10) 77.66(10) 86.06(11) ? Ca1 Ca2 Ca1 . . 2_7645 97.87(5) 95.20(5) 100.46(6) ? Ca1 Ca2 Ca1 . . 2_7745 97.90(5) 95.20(5) 100.46(6) ? Ca1 Ca2 Ca1 . . 3_7465 63.56(5) 61.09(5) 66.07(5) ? Ca1 Ca2 Ca1 . . 3_7565 63.59(5) 61.09(5) 66.07(5) ? Ca1 Ca2 Ca1 . . 4_4655 155.15(5) 155.06(5) 155.25(5) ? Ca1 Ca2 Ca2 . . 4_4655 93.53(6) 93.39(6) 93.67(6) ? Ca1 Ca2 Ca2 . . 4_5655 58.53(5) 58.45(5) 58.61(5) ? Ca1 Ca2 Si1 . . 2_6645 116.63(8) 113.76(8) 119.42(8) ? Ca1 Ca2 Si1 . . 2_6745 116.64(8) 113.76(8) 119.42(8) ? Ca1 Ca2 Si1 . . 4_5655 134.40(5) 134.06(5) 134.74(5) ? Ca1 Ca2 O1 . . 2_6745 109.1(2) 98.2(2) 119.20(19) ? Ca1 Ca2 O1 . . 3_7465 50.84(18) 40.44(16) 61.40(19) ? Ca1 Ca2 O1 . . 5_7765 51.03(18) 40.44(16) 61.40(19) ? Ca1 Ca2 O1 . . 8_6445 109.1(2) 98.2(2) 119.20(19) ? Ca1 Ca2 O2 . . . 46.21(10) 45.54(10) 47.00(10) ? Ca1 Ca2 O2 . . 7_5655 46.22(10) 45.54(10) 47.00(10) ? Ca1 Ca2 O3 . . 4_5655 161.45(8) 159.49(8) 164.91(7) ? Ca1 Ca2 O3 . . 6_5555 161.49(8) 159.49(8) 164.91(7) ? Ca1 Ca2 Ca1 2_7645 . 2_7745 94.71(5) 94.48(5) 94.93(4) ? Ca1 Ca2 Ca1 2_7645 . 3_7465 79.99(5) 76.92(5) 83.29(5) ? Ca1 Ca2 Ca1 2_7645 . 3_7565 159.32(6) 158.20(6) 160.13(6) ? Ca1 Ca2 Ca1 2_7645 . 4_4655 98.79(6) 96.30(6) 101.17(6) ? Ca1 Ca2 Ca2 2_7645 . 4_4655 130.82(5) 123.67(5) 137.88(5) ? Ca1 Ca2 Ca2 2_7645 . 4_5655 60.36(4) 57.83(4) 62.69(4) ? Ca1 Ca2 Si1 2_7645 . 2_6645 64.01(5) 60.39(4) 67.69(5) ? Ca1 Ca2 Si1 2_7645 . 2_6745 140.63(9) 138.61(9) 142.55(9) ? Ca1 Ca2 Si1 2_7645 . 4_5655 55.34(6) 52.55(6) 58.00(6) ? Ca1 Ca2 O1 2_7645 . 2_6745 151.15(19) 139.67(16) 161.9(2) ? Ca1 Ca2 O1 2_7645 . 3_7465 47.53(18) 38.90(19) 56.17(17) ? Ca1 Ca2 O1 2_7645 . 5_7765 104.53(10) 98.95(10) 110.45(10) ? Ca1 Ca2 O1 2_7645 . 8_6445 89.41(11) 80.36(11) 97.92(11) ? Ca1 Ca2 O2 2_7645 . . 119.83(9) 113.06(9) 122.80(9) ? Ca1 Ca2 O2 2_7645 . 7_5655 129.60(10) 126.76(10) 135.69(11) ? Ca1 Ca2 O3 2_7645 . 4_5655 64.56(8) 63.48(8) 66.55(8) ? Ca1 Ca2 O3 2_7645 . 6_5555 80.35(9) 78.63(9) 81.30(9) ? Ca1 Ca2 Ca1 2_7745 . 3_7465 159.32(6) 158.20(6) 160.13(6) ? Ca1 Ca2 Ca1 2_7745 . 3_7565 80.01(5) 76.92(5) 83.29(5) ? Ca1 Ca2 Ca1 2_7745 . 4_4655 98.75(6) 96.30(6) 101.17(6) ? Ca1 Ca2 Ca2 2_7745 . 4_4655 130.75(5) 123.67(5) 137.88(5) ? Ca1 Ca2 Ca2 2_7745 . 4_5655 60.37(4) 57.83(4) 62.69(4) ? Ca1 Ca2 Si1 2_7745 . 2_6645 140.61(9) 138.61(9) 142.55(9) ? Ca1 Ca2 Si1 2_7745 . 2_6745 63.99(5) 60.39(4) 67.69(5) ? Ca1 Ca2 Si1 2_7745 . 4_5655 55.32(6) 52.55(6) 58.00(6) ? Ca1 Ca2 O1 2_7745 . 2_6745 89.33(11) 80.36(11) 97.92(11) ? Ca1 Ca2 O1 2_7745 . 3_7465 104.60(10) 98.95(10) 110.45(10) ? Ca1 Ca2 O1 2_7745 . 5_7765 47.37(18) 38.90(19) 56.17(17) ? Ca1 Ca2 O1 2_7745 . 8_6445 151.08(19) 139.67(16) 161.9(2) ? Ca1 Ca2 O2 2_7745 . . 129.52(10) 126.76(10) 135.69(11) ? Ca1 Ca2 O2 2_7745 . 7_5655 119.75(9) 113.06(9) 122.80(9) ? Ca1 Ca2 O3 2_7745 . 4_5655 80.35(9) 78.63(9) 81.30(9) ? Ca1 Ca2 O3 2_7745 . 6_5555 64.56(8) 63.48(8) 66.55(8) ? Ca1 Ca2 Ca1 3_7465 . 3_7565 97.97(6) 97.97(6) 97.97(6) ? Ca1 Ca2 Ca1 3_7465 . 4_4655 101.67(5) 99.13(5) 104.16(5) ? Ca1 Ca2 Ca2 3_7465 . 4_4655 63.06(4) 58.47(4) 67.61(4) ? Ca1 Ca2 Ca2 3_7465 . 4_5655 100.31(6) 96.19(5) 104.43(6) ? Ca1 Ca2 Si1 3_7465 . 2_6645 53.92(7) 52.70(7) 55.20(7) ? Ca1 Ca2 Si1 3_7465 . 2_6745 130.87(5) 129.73(5) 131.91(5) ? Ca1 Ca2 Si1 3_7465 . 4_5655 130.98(7) 125.32(7) 136.65(8) ? Ca1 Ca2 O1 3_7465 . 2_6745 104.53(14) 100.15(13) 108.90(14) ? Ca1 Ca2 O1 3_7465 . 3_7465 57.50(12) 48.44(11) 66.68(13) ? Ca1 Ca2 O1 3_7465 . 5_7765 114.28(19) 106.23(18) 121.95(19) ? Ca1 Ca2 O1 3_7465 . 8_6445 48.91(17) 37.17(18) 60.09(15) ? Ca1 Ca2 O2 3_7465 . . 41.81(8) 36.65(8) 44.27(7) ? Ca1 Ca2 O2 3_7465 . 7_5655 56.29(8) 53.76(8) 61.38(8) ? Ca1 Ca2 O3 3_7465 . 4_5655 113.56(9) 111.93(9) 117.14(9) ? Ca1 Ca2 O3 3_7465 . 6_5555 133.19(9) 129.79(9) 134.75(9) ? Ca1 Ca2 Ca1 3_7565 . 4_4655 101.63(5) 99.13(5) 104.16(5) ? Ca1 Ca2 Ca2 3_7565 . 4_4655 62.99(4) 58.47(4) 67.61(4) ? Ca1 Ca2 Ca2 3_7565 . 4_5655 100.33(6) 96.19(5) 104.43(6) ? Ca1 Ca2 Si1 3_7565 . 2_6645 130.85(5) 129.73(5) 131.91(5) ? Ca1 Ca2 Si1 3_7565 . 2_6745 53.90(7) 52.70(7) 55.20(7) ? Ca1 Ca2 Si1 3_7565 . 4_5655 130.98(7) 125.32(7) 136.65(8) ? Ca1 Ca2 O1 3_7565 . 2_6745 48.83(17) 37.17(18) 60.09(15) ? Ca1 Ca2 O1 3_7565 . 3_7465 114.13(19) 106.23(18) 121.95(19) ? Ca1 Ca2 O1 3_7565 . 5_7765 57.62(12) 48.44(11) 66.68(13) ? Ca1 Ca2 O1 3_7565 . 8_6445 104.46(14) 100.15(13) 108.90(14) ? Ca1 Ca2 O2 3_7565 . . 56.22(8) 53.76(8) 61.38(8) ? Ca1 Ca2 O2 3_7565 . 7_5655 41.74(8) 36.65(8) 44.27(7) ? Ca1 Ca2 O3 3_7565 . 4_5655 133.21(9) 129.79(9) 134.75(9) ? Ca1 Ca2 O3 3_7565 . 6_5555 113.58(9) 111.93(9) 117.14(9) ? Ca1 Ca2 Ca2 4_4655 . 4_4655 61.63(5) 61.54(5) 61.73(5) ? Ca1 Ca2 Ca2 4_4655 . 4_5655 145.99(8) 145.71(7) 146.26(8) ? Ca1 Ca2 Si1 4_4655 . 2_6645 56.50(6) 54.91(6) 58.10(6) ? Ca1 Ca2 Si1 4_4655 . 2_6745 56.47(6) 54.91(6) 58.10(6) ? Ca1 Ca2 Si1 4_4655 . 4_5655 70.10(6) 69.94(6) 70.27(6) ? Ca1 Ca2 O1 4_4655 . 2_6745 52.89(17) 42.70(16) 63.69(18) ? Ca1 Ca2 O1 4_4655 . 3_7465 139.23(15) 132.27(17) 146.53(14) ? Ca1 Ca2 O1 4_4655 . 5_7765 139.09(15) 132.27(17) 146.53(14) ? Ca1 Ca2 O1 4_4655 . 8_6445 52.87(17) 42.70(16) 63.69(18) ? Ca1 Ca2 O2 4_4655 . . 109.51(10) 108.63(10) 110.07(10) ? Ca1 Ca2 O2 4_4655 . 7_5655 109.50(10) 108.63(10) 110.07(10) ? Ca1 Ca2 O3 4_4655 . 4_5655 40.28(7) 39.47(7) 41.01(7) ? Ca1 Ca2 O3 4_4655 . 6_5555 40.27(7) 39.47(7) 41.01(7) ? Ca2 Ca2 Ca2 4_4655 . 4_5655 151.42(8) 150.70(8) 152.13(8) ? Ca2 Ca2 Si1 4_4655 . 2_6645 68.09(5) 64.47(5) 71.54(5) ? Ca2 Ca2 Si1 4_4655 . 2_6745 68.04(5) 64.47(5) 71.54(5) ? Ca2 Ca2 Si1 4_4655 . 4_5655 131.30(8) 130.80(8) 131.80(8) ? Ca2 Ca2 O1 4_4655 . 2_6745 42.26(12) 41.52(12) 43.38(11) ? Ca2 Ca2 O1 4_4655 . 3_7465 119.05(15) 108.70(14) 129.90(16) ? Ca2 Ca2 O1 4_4655 . 5_7765 119.13(15) 108.70(14) 129.90(16) ? Ca2 Ca2 O1 4_4655 . 8_6445 42.25(12) 41.52(12) 43.38(11) ? Ca2 Ca2 O2 4_4655 . . 48.67(9) 48.07(9) 49.43(9) ? Ca2 Ca2 O2 4_4655 . 7_5655 48.66(9) 48.07(9) 49.43(9) ? Ca2 Ca2 O3 4_4655 . 4_5655 100.18(8) 99.60(8) 101.16(8) ? Ca2 Ca2 O3 4_4655 . 6_5555 100.18(8) 99.60(8) 101.16(8) ? Ca2 Ca2 Si1 4_5655 . 2_6645 121.95(6) 115.76(6) 128.07(6) ? Ca2 Ca2 Si1 4_5655 . 2_6745 121.94(6) 115.76(6) 128.07(6) ? Ca2 Ca2 Si1 4_5655 . 4_5655 75.95(6) 75.74(6) 76.16(6) ? Ca2 Ca2 O1 4_5655 . 2_6745 142.11(11) 126.30(12) 157.27(10) ? Ca2 Ca2 O1 4_5655 . 3_7465 44.96(10) 42.57(9) 48.34(11) ? Ca2 Ca2 O1 4_5655 . 5_7765 44.91(10) 42.57(9) 48.34(11) ? Ca2 Ca2 O1 4_5655 . 8_6445 142.20(11) 126.30(12) 157.27(10) ? Ca2 Ca2 O2 4_5655 . . 104.15(11) 103.43(11) 104.38(11) ? Ca2 Ca2 O2 4_5655 . 7_5655 104.14(11) 103.43(11) 104.38(11) ? Ca2 Ca2 O3 4_5655 . 4_5655 105.98(8) 105.21(8) 107.18(8) ? Ca2 Ca2 O3 4_5655 . 6_5555 105.99(8) 105.21(8) 107.18(8) ? Si1 Ca2 Si1 2_6645 . 2_6745 110.99(7) 110.88(7) 111.11(7) ? Si1 Ca2 Si1 2_6645 . 4_5655 85.99(8) 81.36(8) 90.58(9) ? Si1 Ca2 O1 2_6645 . 2_6745 95.72(11) 86.13(10) 105.80(12) ? Si1 Ca2 O1 2_6645 . 3_7465 85.51(12) 80.44(12) 90.52(12) ? Si1 Ca2 O1 2_6645 . 5_7765 161.78(14) 157.99(17) 168.62(14) ? Si1 Ca2 O1 2_6645 . 8_6445 27.14(13) 23.25(15) 30.65(10) ? Si1 Ca2 O2 2_6645 . . 87.96(10) 83.27(10) 90.24(10) ? Si1 Ca2 O2 2_6645 . 7_5655 99.92(9) 97.80(9) 104.04(9) ? Si1 Ca2 O3 2_6645 . 4_5655 60.81(9) 59.41(9) 64.09(9) ? Si1 Ca2 O3 2_6645 . 6_5555 78.56(10) 75.36(10) 80.01(10) ? Si1 Ca2 Si1 2_6745 . 4_5655 85.99(8) 81.36(8) 90.58(9) ? Si1 Ca2 O1 2_6745 . 2_6745 27.08(13) 23.25(15) 30.65(10) ? Si1 Ca2 O1 2_6745 . 3_7465 161.72(14) 157.99(17) 168.62(14) ? Si1 Ca2 O1 2_6745 . 5_7765 85.45(12) 80.44(12) 90.52(12) ? Si1 Ca2 O1 2_6745 . 8_6445 95.64(11) 86.13(10) 105.80(12) ? Si1 Ca2 O2 2_6745 . . 99.86(9) 97.80(9) 104.04(9) ? Si1 Ca2 O2 2_6745 . 7_5655 87.89(10) 83.27(10) 90.24(10) ? Si1 Ca2 O3 2_6745 . 4_5655 78.59(10) 75.36(10) 80.01(10) ? Si1 Ca2 O3 2_6745 . 6_5555 60.84(9) 59.41(9) 64.09(9) ? Si1 Ca2 O1 4_5655 . 2_6745 105.9(2) 104.06(19) 107.7(2) ? Si1 Ca2 O1 4_5655 . 3_7465 97.02(18) 87.72(19) 106.50(17) ? Si1 Ca2 O1 4_5655 . 5_7765 96.84(18) 87.72(19) 106.50(17) ? Si1 Ca2 O1 4_5655 . 8_6445 105.9(2) 104.06(19) 107.7(2) ? Si1 Ca2 O2 4_5655 . . 175.81(10) 165.45(10) 180 ? Si1 Ca2 O2 4_5655 . 7_5655 175.68(10) 165.45(10) 180 ? Si1 Ca2 O3 4_5655 . 4_5655 31.45(7) 30.98(7) 32.22(8) ? Si1 Ca2 O3 4_5655 . 6_5555 31.46(7) 30.98(7) 32.22(8) ? O1 Ca2 O1 2_6745 . 3_7465 154.2(2) 147.8(3) 164.8(3) ? O1 Ca2 O1 2_6745 . 5_7765 98.56(15) 82.16(16) 114.72(14) ? O1 Ca2 O1 2_6745 . 8_6445 74.93(12) 73.89(12) 75.96(12) ? O1 Ca2 O2 2_6745 . . 75.42(19) 72.54(18) 81.52(19) ? O1 Ca2 O2 2_6745 . 7_5655 72.4(2) 63.4(2) 76.23(18) ? O1 Ca2 O3 2_6745 . 4_5655 83.32(19) 80.71(17) 89.5(2) ? O1 Ca2 O3 2_6745 . 6_5555 79.3(2) 74.6(2) 81.6(2) ? O1 Ca2 O1 3_7465 . 5_7765 79.44(16) 78.10(16) 80.75(16) ? O1 Ca2 O1 3_7465 . 8_6445 98.62(15) 82.16(16) 114.72(14) ? O1 Ca2 O2 3_7465 . . 84.69(19) 74.17(18) 89.44(19) ? O1 Ca2 O2 3_7465 . 7_5655 81.60(19) 76.87(18) 92.3(2) ? O1 Ca2 O3 3_7465 . 4_5655 110.84(19) 104.57(19) 121.67(18) ? O1 Ca2 O3 3_7465 . 6_5555 127.48(19) 115.98(19) 135.56(18) ? O1 Ca2 O1 5_7765 . 8_6445 154.4(2) 147.8(3) 164.8(3) ? O1 Ca2 O2 5_7765 . . 81.61(19) 76.87(18) 92.3(2) ? O1 Ca2 O2 5_7765 . 7_5655 84.70(19) 74.17(18) 89.44(19) ? O1 Ca2 O3 5_7765 . 4_5655 127.33(19) 115.98(19) 135.56(18) ? O1 Ca2 O3 5_7765 . 6_5555 110.72(19) 104.57(19) 121.67(18) ? O1 Ca2 O2 8_6445 . . 72.5(2) 63.4(2) 76.23(18) ? O1 Ca2 O2 8_6445 . 7_5655 75.50(19) 72.54(18) 81.52(19) ? O1 Ca2 O3 8_6445 . 4_5655 79.4(2) 74.6(2) 81.6(2) ? O1 Ca2 O3 8_6445 . 6_5555 83.37(19) 80.71(17) 89.5(2) ? O2 Ca2 O3 . . 4_5655 143.60(12) 141.47(12) 145.71(12) ? O2 Ca2 O3 . . 6_5555 148.97(11) 148.61(11) 149.57(11) ? O2 Ca2 O3 7_5655 . 4_5655 148.97(11) 148.61(11) 149.57(11) ? O2 Ca2 O3 7_5655 . 6_5555 143.57(12) 141.47(12) 145.71(12) ? Ca1 Si1 Ca1 . . 3_7465 74.71(6) 72.52(6) 76.94(6) ? Ca1 Si1 Ca1 . . 3_7565 74.74(6) 72.52(6) 76.94(6) ? Ca1 Si1 Ca1 . . 4_4665 99.49(9) 99.42(9) 99.55(9) ? Ca1 Si1 Ca2 . . 2_6655 118.74(8) 118.20(8) 119.26(8) ? Ca1 Si1 Ca2 . . 2_6755 118.75(8) 118.20(8) 119.26(8) ? Ca1 Si1 Ca2 . . 4_4655 114.88(11) 114.80(11) 114.96(11) ? Ca1 Si1 O1 . . . 77.31(16) 63.27(16) 90.93(16) ? Ca1 Si1 O1 . . 7_5655 77.10(16) 63.27(16) 90.93(16) ? Ca1 Si1 O2 . . . 57.87(14) 56.88(14) 58.93(13) ? Ca1 Si1 O2 . . 7_5655 57.89(14) 56.88(14) 58.93(13) ? Ca1 Si1 O3 . . . 159.8(2) 157.1(2) 162.3(3) ? Ca1 Si1 O3 . . 7_5655 159.9(2) 157.1(2) 162.3(3) ? Ca1 Si1 Ca1 3_7465 . 3_7565 117.54(11) 117.52(11) 117.56(11) ? Ca1 Si1 Ca1 3_7465 . 4_4665 118.96(10) 114.60(9) 123.23(10) ? Ca1 Si1 Ca2 3_7465 . 2_6655 63.65(6) 61.14(6) 66.20(6) ? Ca1 Si1 Ca2 3_7465 . 2_6755 164.73(8) 163.75(7) 165.50(9) ? Ca1 Si1 Ca2 3_7465 . 4_4655 72.95(8) 67.73(7) 78.11(8) ? Ca1 Si1 O1 3_7465 . . 149.91(18) 139.90(18) 158.2(2) ? Ca1 Si1 O1 3_7465 . 7_5655 59.3(3) 46.5(3) 72.4(2) ? Ca1 Si1 O2 3_7465 . . 46.97(12) 41.18(12) 50.19(12) ? Ca1 Si1 O2 3_7465 . 7_5655 70.75(14) 67.44(13) 76.47(14) ? Ca1 Si1 O3 3_7465 . . 106.20(18) 103.44(18) 110.78(18) ? Ca1 Si1 O3 3_7465 . 7_5655 88.53(16) 83.99(15) 91.18(16) ? Ca1 Si1 Ca1 3_7565 . 4_4665 118.88(10) 114.60(9) 123.23(10) ? Ca1 Si1 Ca2 3_7565 . 2_6655 164.71(8) 163.75(7) 165.50(9) ? Ca1 Si1 Ca2 3_7565 . 2_6755 63.60(6) 61.14(6) 66.20(6) ? Ca1 Si1 Ca2 3_7565 . 4_4655 72.86(8) 67.73(7) 78.11(8) ? Ca1 Si1 O1 3_7565 . . 59.5(3) 46.5(3) 72.4(2) ? Ca1 Si1 O1 3_7565 . 7_5655 149.76(18) 139.90(18) 158.2(2) ? Ca1 Si1 O2 3_7565 . . 70.66(14) 67.44(13) 76.47(14) ? Ca1 Si1 O2 3_7565 . 7_5655 46.88(12) 41.18(12) 50.19(12) ? Ca1 Si1 O3 3_7565 . . 88.50(16) 83.99(15) 91.18(16) ? Ca1 Si1 O3 3_7565 . 7_5655 106.18(18) 103.44(18) 110.78(18) ? Ca1 Si1 Ca2 4_4665 . 2_6655 68.03(7) 65.67(7) 70.24(8) ? Ca1 Si1 Ca2 4_4665 . 2_6755 67.99(7) 65.67(7) 70.24(8) ? Ca1 Si1 Ca2 4_4665 . 4_4655 145.10(6) 144.51(6) 145.71(6) ? Ca1 Si1 O1 4_4665 . . 60.3(3) 42.8(2) 78.3(3) ? Ca1 Si1 O1 4_4665 . 7_5655 60.5(3) 42.8(2) 78.3(3) ? Ca1 Si1 O2 4_4665 . . 152.10(17) 148.51(17) 155.35(17) ? Ca1 Si1 O2 4_4665 . 7_5655 152.04(17) 148.51(17) 155.35(17) ? Ca1 Si1 O3 4_4665 . . 97.2(2) 96.6(2) 97.4(2) ? Ca1 Si1 O3 4_4665 . 7_5655 97.2(2) 96.6(2) 97.4(2) ? Ca2 Si1 Ca2 2_6655 . 2_6755 110.99(7) 110.88(7) 111.11(7) ? Ca2 Si1 Ca2 2_6655 . 4_4655 93.97(7) 88.97(7) 98.78(7) ? Ca2 Si1 O1 2_6655 . . 127.6(3) 110.9(2) 144.4(3) ? Ca2 Si1 O1 2_6655 . 7_5655 44.96(16) 36.35(17) 55.06(16) ? Ca2 Si1 O2 2_6655 . . 108.30(14) 102.40(13) 113.29(15) ? Ca2 Si1 O2 2_6655 . 7_5655 133.52(17) 128.65(16) 139.10(18) ? Ca2 Si1 O3 2_6655 . . 77.98(13) 74.54(14) 82.05(13) ? Ca2 Si1 O3 2_6655 . 7_5655 58.03(15) 54.02(15) 61.25(15) ? Ca2 Si1 Ca2 2_6755 . 4_4655 93.88(7) 88.97(7) 98.78(7) ? Ca2 Si1 O1 2_6755 . . 44.80(16) 36.35(17) 55.06(16) ? Ca2 Si1 O1 2_6755 . 7_5655 127.8(3) 110.9(2) 144.4(3) ? Ca2 Si1 O2 2_6755 . . 133.42(17) 128.65(16) 139.10(18) ? Ca2 Si1 O2 2_6755 . 7_5655 108.20(14) 102.40(13) 113.29(15) ? Ca2 Si1 O3 2_6755 . . 58.01(15) 54.02(15) 61.25(15) ? Ca2 Si1 O3 2_6755 . 7_5655 77.96(13) 74.54(14) 82.05(13) ? Ca2 Si1 O1 4_4655 . . 124.8(3) 115.4(3) 135.2(2) ? Ca2 Si1 O1 4_4655 . 7_5655 124.9(3) 115.4(3) 135.2(2) ? Ca2 Si1 O2 4_4655 . . 58.95(16) 58.03(16) 60.02(17) ? Ca2 Si1 O2 4_4655 . 7_5655 58.93(16) 58.03(16) 60.02(17) ? Ca2 Si1 O3 4_4655 . . 50.4(2) 49.7(2) 50.7(2) ? Ca2 Si1 O3 4_4655 . 7_5655 50.4(2) 49.7(2) 50.7(2) ? O1 Si1 O1 . . 7_5655 110.1(4) 108.6(4) 111.6(4) ? O1 Si1 O2 . . . 109.2(3) 102.7(3) 121.0(3) ? O1 Si1 O2 . . 7_5655 108.6(3) 97.8(3) 115.1(2) ? O1 Si1 O3 . . . 106.6(2) 99.7(2) 110.4(2) ? O1 Si1 O3 . . 7_5655 113.6(2) 109.8(2) 121.4(2) ? O1 Si1 O2 7_5655 . . 108.7(3) 97.8(3) 115.1(2) ? O1 Si1 O2 7_5655 . 7_5655 109.2(3) 102.7(3) 121.0(3) ? O1 Si1 O3 7_5655 . . 113.7(2) 109.8(2) 121.4(2) ? O1 Si1 O3 7_5655 . 7_5655 106.7(2) 99.7(2) 110.4(2) ? O2 Si1 O3 . . . 109.0(3) 108.5(3) 109.2(3) ? O2 Si1 O3 . . 7_5655 105.5(3) 105.4(3) 105.6(3) ? O2 Si1 O3 7_5655 . . 105.5(3) 105.4(3) 105.6(3) ? O2 Si1 O3 7_5655 . 7_5655 109.0(3) 108.5(3) 109.2(3) ? Ca1 O1 Ca1 3_7565 . 4_4665 170.04(18) 162.29(16) 176.22(19) ? Ca1 O1 Ca2 3_7565 . 2_6755 81.99(16) 74.64(15) 88.17(15) ? Ca1 O1 Ca2 3_7565 . 3_7565 88.05(14) 77.34(14) 99.00(14) ? Ca1 O1 Si1 3_7565 . . 90.9(3) 77.8(3) 103.4(4) ? Ca1 O1 Ca2 4_4665 . 2_6755 89.2(2) 75.84(15) 103.2(2) ? Ca1 O1 Ca2 4_4665 . 3_7565 93.5(3) 86.5(2) 100.8(3) ? Ca1 O1 Si1 4_4665 . . 90.0(2) 72.6(2) 107.0(2) ? Ca2 O1 Ca2 2_6755 . 3_7565 92.82(16) 89.57(17) 94.95(15) ? Ca2 O1 Si1 2_6755 . . 108.1(2) 94.31(18) 120.2(3) ? Ca2 O1 Si1 3_7565 . . 150.4(3) 133.1(3) 166.8(3) ? Ca1 O2 Ca2 3_7465 . . 96.62(17) 94.20(16) 101.68(19) ? Ca1 O2 Si1 3_7465 . . 102.9(2) 99.7(2) 108.1(2) ? Ca2 O2 Si1 . . . 160.20(18) 149.97(17) 165.67(18) ? Ca1 O3 Ca2 1_4555 . 4_4655 96.28(17) 95.29(17) 97.89(18) ? Ca1 O3 Si1 1_4555 . . 152.9(3) 152.0(3) 153.3(3) ? Ca2 O3 Si1 4_4655 . . 98.2(2) 97.6(2) 99.0(2) ? #======================================================================= # 11. STRUCTURE-FACTOR LIST loop_ _reflns_scale_group_code _reflns_scale_meas_intensity 1 2218.069 2 2160.549 3 1966.437 4 1973.655 5 2078.317 6 2119.294 7 2399.007 8 2292.194 9 2368.509 10 2471.417 11 2383.873 12 2416.707 13 2557.724 14 2564.054 15 2591.537 16 2615.735 17 2538.021 18 2572.927 19 2676.160 20 2686.438 21 2585.484 22 2690.572 23 2780.469 24 2641.190 26 2795.803 27 2831.149 28 2800.775 29 2811.457 30 2785.775 31 2857.306 32 2839.958 33 2813.549 34 2759.520 35 2966.520 36 2931.655 37 2878.517 38 2853.720 39 2903.132 40 2903.629 41 2998.930 42 2966.000 43 2964.523 44 2997.545 45 3318.477 46 3029.382 47 2924.959 48 2834.339 49 2820.116 50 2858.280 51 2852.890 52 2902.905 53 2687.471 54 2830.195 55 2826.999 56 2845.632 57 2707.090 58 2891.662 59 2862.531 60 2868.099 61 2847.372 62 2772.515 63 2766.894 64 2818.046 65 2777.398 66 2676.086 67 2623.542 68 2637.985 69 2544.892 70 2573.444 71 2518.914 72 2530.089 73 2527.658 74 2543.937 75 2551.902 76 2540.140 77 2466.818 78 2338.681 79 2400.759 80 2385.618 81 2318.187 82 2315.833 83 2350.821 84 2371.641 85 2431.334 86 2542.173 87 2372.224 88 2177.449 89 2123.178 90 2140.829 91 2070.319 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_index_m_1 _refln_intensity_calc _refln_intensity_meas _refln_intensity_sigma _refln_scale_group_code _refln_include_status 4 5 -8 -1 42.15 -260.80 215.60 1 < 1 6 -8 -1 660.08 502.60 220.00 1 < 5 4 -7 -1 22.12 -255.90 224.60 1 < 2 5 -7 -1 160.98 289.80 243.90 1 < -4 6 -6 -1 163.62 158.50 188.70 1 < 9 1 -5 -1 49.98 87.80 213.10 1 < 6 2 -5 -1 219.52 -199.80 256.20 1 < 0 4 -5 -1 4188.70 3615.30 362.80 1 o -3 5 -5 -1 259.27 438.90 236.80 1 < 7 1 -4 -1 85.99 443.00 270.00 1 < 4 2 -4 -1 224.39 488.70 320.50 1 < -6 5 -4 -1 87.27 78.40 183.60 1 < -5 4 -3 -1 254.33 386.20 254.10 1 < 8 -1 -2 -1 142.22 120.20 243.40 1 < -1 2 -2 -1 36301.00 27283.60 828.60 1 o -4 3 -2 -1 3866.40 2662.50 365.70 1 o -7 3 -1 -1 616.53 475.40 241.20 1 < 9 -3 0 -1 29.77 10.10 200.70 1 < 7 -3 1 -1 449.09 -135.00 258.30 1 < 4 -2 1 -1 517.14 1083.70 433.70 1 < 1 -1 1 -1 1470.20 2510.60 823.10 1 o -8 1 2 -1 115.68 329.60 208.90 1 < 5 -4 3 -1 495.39 910.00 264.60 1 o 2 -3 3 -1 575.30 1010.10 397.90 1 < -1 -2 3 -1 3050.30 6328.90 556.50 1 o -4 -1 3 -1 317.14 181.40 339.80 1 < -7 -1 4 -1 228.41 903.80 233.10 1 o 3 -5 5 -1 1161.80 1399.70 262.70 1 o 0 -4 5 -1 2752.70 1966.60 355.60 1 o -3 -3 5 -1 2903.90 2532.20 360.50 1 o -6 -2 5 -1 696.18 628.10 240.90 1 < 1 -6 7 -1 378.97 385.70 205.40 1 < -2 -5 7 -1 1436.00 1637.10 275.00 1 o -5 -4 7 -1 42.09 457.30 207.50 1 < 4 5 -8 0 614.50 701.50 227.50 1 o -2 6 -7 0 185.06 255.60 207.70 1 < 8 2 -6 0 829.01 760.50 213.50 1 o 5 3 -6 0 7446.80 5659.90 385.20 1 o 2 4 -6 0 1794.00 1685.80 297.80 1 o -1 5 -6 0 3770.60 3856.70 330.90 1 o -4 6 -6 0 141.96 717.40 205.20 1 o 6 2 -5 0 676.20 256.30 250.90 1 < 3 3 -5 0 8984.70 9647.50 503.10 1 o 9 0 -4 0 124.06 508.30 211.20 1 < -6 5 -4 0 46.73 -107.50 206.50 1 < 7 0 -3 0 4478.10 3464.10 334.40 1 o -2 3 -3 0 4742.90 2921.00 393.80 1 o -8 4 -2 0 1290.00 1270.00 223.10 1 o 8 -2 -1 0 475.60 625.80 231.20 1 < -7 3 -1 0 1422.20 1164.00 261.40 1 o 6 -2 0 0 36672.00 37483.00 824.00 1 o -9 2 1 0 5335.90 5885.40 364.70 1 o 7 -4 2 0 795.65 1147.10 253.10 1 o 4 -3 2 0 8877.10 15805.80 591.00 1 o -5 0 2 0 25355.00 26640.90 711.10 1 o -8 0 3 0 1759.40 1116.60 255.70 1 o 5 -5 4 0 1131.20 1602.70 257.80 1 o -4 -2 4 0 3364.10 2574.50 369.90 1 o -7 -1 4 0 1746.30 2400.40 297.90 1 o 3 -6 6 0 152.26 -311.90 200.90 1 < -6 -3 6 0 329.44 588.30 231.90 1 < 1 -6 7 0 453.72 533.10 216.40 1 < -2 -5 7 0 448.92 796.20 240.70 1 o -2 -6 8 0 52.32 -72.30 209.20 1 < 0 6 -8 1 275.92 47.30 223.60 1 < 4 4 -7 1 32.20 173.50 219.70 1 < 1 5 -7 1 326.80 -63.00 227.00 1 < -2 6 -7 1 163.86 411.20 213.80 1 < -4 5 -5 1 36.65 371.10 226.40 1 < 6 1 -4 1 596.65 106.80 262.90 1 < 3 2 -4 1 57.24 418.30 339.90 1 < 0 3 -4 1 2826.40 918.30 383.70 1 < -3 4 -4 1 752.47 1608.20 316.50 1 o -5 3 -2 1 2044.40 1725.40 337.40 1 o 8 -2 -1 1 431.37 662.30 218.70 1 o 5 -1 -1 1 989.92 1857.40 401.70 1 o -1 1 -1 1 1279.10 113.40 802.70 1 < -7 2 0 1 831.24 965.60 312.60 1 o 6 -3 1 1 88.55 -529.30 272.70 1 < -6 1 1 1 730.72 788.20 361.40 1 < -9 1 2 1 34.49 110.70 207.20 1 < -5 -1 3 1 869.13 960.20 331.80 1 < 2 -4 4 1 715.29 1481.90 341.80 1 o -1 -3 4 1 665.32 135.50 406.20 1 < -7 -2 5 1 219.21 6.70 271.80 1 < 3 -6 6 1 51.58 -55.20 210.60 1 < 0 -5 6 1 1911.60 2596.90 300.00 1 o -3 -4 6 1 315.64 313.80 266.60 1 < -6 -4 7 1 126.61 500.60 195.10 1 < -2 -6 8 1 109.51 494.90 201.20 1 < -1 6 -7 -1 280.95 190.80 188.50 2 < 6 3 -6 -1 689.64 1186.50 244.10 2 o 3 4 -6 -1 414.47 633.00 239.60 2 < 0 5 -6 -1 2538.80 1854.90 274.60 2 o -3 5 -5 -1 105.86 250.50 203.00 2 < -2 4 -4 -1 324.08 1413.70 323.70 2 o 5 1 -3 -1 580.41 423.60 297.40 2 < -5 4 -3 -1 183.11 97.10 228.50 2 < -4 3 -2 -1 3433.50 1937.60 344.20 2 o 9 -2 -1 -1 30.16 -98.60 211.30 2 < 6 -1 -1 -1 694.88 565.60 340.10 2 < -7 3 -1 -1 672.69 670.00 218.30 2 o 7 -3 1 -1 442.82 257.50 220.70 2 < 4 -2 1 -1 700.45 1394.80 396.80 2 o 5 -4 3 -1 519.49 737.80 249.20 2 < 2 -3 3 -1 240.18 1534.30 358.00 2 o -4 -2 4 -1 1647.40 991.80 315.80 2 o 3 -5 5 -1 819.41 532.50 244.80 2 < -7 -2 5 -1 264.90 162.90 241.40 2 < 3 -6 6 -1 787.55 470.40 207.80 2 < 0 -5 6 -1 1520.10 1676.80 259.60 2 o -3 -4 6 -1 404.66 161.70 226.60 2 < -6 -4 7 -1 250.16 197.30 192.20 2 < 5 4 -7 0 2051.30 1448.30 243.60 2 o 2 5 -7 0 419.52 232.50 218.50 2 < -1 6 -7 0 483.07 269.10 195.90 2 < 6 3 -6 0 848.33 1053.40 230.20 2 o -4 6 -6 0 101.07 457.80 179.40 2 < -3 5 -5 0 803.07 946.40 227.60 2 o 7 1 -4 0 843.02 953.20 262.90 2 o 4 2 -4 0 419.37 70.40 313.70 2 < -6 5 -4 0 68.69 118.50 192.50 2 < -5 4 -3 0 1201.90 1163.20 249.10 2 o 8 -1 -2 0 646.01 91.70 219.60 2 < 5 0 -2 0 27509.00 28904.80 714.50 2 o 2 1 -2 0 21893.00 20829.80 733.50 2 o -8 4 -2 0 1736.00 1527.90 224.10 2 o -4 2 -1 0 33167.00 32169.70 772.00 2 o 6 -2 0 0 35869.00 46581.10 880.60 2 o -6 1 1 0 5747.10 5873.70 401.60 2 o 7 -4 2 0 1334.90 1421.40 256.40 2 o 4 -3 2 0 8294.50 10891.60 504.50 2 o 1 -2 2 0 57531.00 54155.30 1007.10 2 o -9 1 2 0 640.91 444.70 208.30 2 < -5 -1 3 0 1202.20 1668.60 335.40 2 o 5 -5 4 0 1541.20 1538.50 246.10 2 o 2 -4 4 0 4867.40 5591.00 408.40 2 o -1 -3 4 0 16513.00 15114.20 562.60 2 o -8 -1 4 0 1295.10 808.30 231.90 2 o -4 -3 5 0 312.24 409.20 282.40 2 < -7 -2 5 0 9127.00 6000.80 367.80 2 o 3 -6 6 0 153.79 51.30 195.10 2 < -7 -3 6 0 1040.90 543.20 212.30 2 < -3 -5 7 0 297.10 314.60 215.80 2 < -6 -4 7 0 555.60 633.10 201.80 2 o 4 5 -8 1 441.51 341.40 193.00 2 < 1 6 -8 1 48.29 -32.80 196.90 2 < 5 4 -7 1 39.84 103.00 194.10 2 < -1 5 -6 1 49.69 294.90 250.50 2 < -4 6 -6 1 277.57 492.40 177.60 2 < 6 2 -5 1 202.32 253.60 224.70 2 < 3 3 -5 1 2799.00 1158.50 342.50 2 o -3 4 -4 1 1223.60 1681.60 305.40 2 o -6 5 -4 1 104.13 322.30 199.60 2 < 4 1 -3 1 200.38 138.90 319.90 2 < 1 2 -3 1 3644.40 1986.20 502.80 2 o -5 3 -2 1 1376.20 1345.20 309.10 2 o 8 -2 -1 1 215.25 462.60 203.40 2 < -8 3 -1 1 105.62 -113.80 208.30 2 < -7 2 0 1 341.62 -90.50 244.70 2 < 6 -3 1 1 61.14 486.30 233.70 2 < -9 1 2 1 52.07 244.50 191.00 2 < 4 -4 3 1 586.47 801.70 262.80 2 o -2 -2 3 1 5299.70 5501.00 507.60 2 o -8 -1 4 1 91.85 -73.60 210.10 2 < 2 -5 5 1 44.40 123.80 237.70 2 < -1 -4 5 1 255.97 566.70 336.50 2 < -4 -3 5 1 2814.30 1986.10 312.60 2 o -7 -3 6 1 48.74 339.40 204.20 2 < 0 -6 7 1 14.65 101.70 176.20 2 < 6 4 -7 -1 47.53 348.20 188.20 3 < 3 5 -7 -1 176.05 110.10 209.10 3 < 0 6 -7 -1 55.03 57.30 185.30 3 < -3 6 -6 -1 104.01 -90.90 183.60 3 < 7 2 -5 -1 56.27 107.60 216.10 3 < 4 3 -5 -1 1544.20 1159.10 280.90 3 o 1 4 -5 -1 522.29 1018.20 289.60 3 o -2 4 -4 -1 391.32 539.40 288.90 3 < -5 5 -4 -1 276.35 604.00 189.00 3 o 2 2 -3 -1 4074.20 5033.40 652.20 3 o -4 3 -2 -1 2110.80 2764.40 350.20 3 o 9 -2 -1 -1 64.09 78.20 200.90 3 < 6 -1 -1 -1 497.28 708.60 302.90 3 < -7 3 -1 -1 374.20 226.80 213.20 3 < -3 1 0 -1 5382.50 2602.80 445.50 3 o 7 -3 1 -1 106.47 265.80 215.90 3 < 4 -2 1 -1 404.87 871.50 367.80 3 < -6 1 1 -1 270.13 622.00 272.60 3 < -2 -1 2 -1 7011.00 6414.20 529.90 3 o -9 1 2 -1 18.46 51.10 165.10 3 < -5 -1 3 -1 382.64 1327.10 302.70 3 o 5 -5 4 -1 242.93 111.40 201.70 3 < 2 -4 4 -1 1228.10 1001.40 314.50 3 o -1 -3 4 -1 586.76 1308.70 313.20 3 o -8 -1 4 -1 181.73 785.60 196.70 3 o -4 -3 5 -1 1495.10 1385.70 261.00 3 o -7 -3 6 -1 82.25 46.60 190.50 3 < 0 -6 7 -1 448.81 347.60 166.70 3 < -3 -5 7 -1 353.63 615.10 197.10 3 o 2 6 -8 0 70.96 -124.90 176.40 3 < 6 4 -7 0 330.72 154.10 208.50 3 < 7 2 -5 0 6324.00 4490.10 324.70 3 o 4 3 -5 0 160.25 733.90 262.80 3 < -3 5 -5 0 199.62 400.70 201.30 3 < -2 4 -4 0 14096.00 10508.00 483.60 3 o -6 5 -4 0 666.55 473.00 182.70 3 < 8 0 -3 0 3301.60 4024.10 314.30 3 o 5 1 -3 0 1656.80 1633.80 323.90 3 o -5 4 -3 0 761.28 1253.20 229.60 3 o -1 2 -2 0 98682.00 85005.30 1201.10 3 o -8 4 -2 0 537.96 648.20 207.50 3 o -4 2 -1 0 20670.00 24275.20 677.60 3 o 6 -2 0 0 23456.00 37376.60 802.80 3 o 7 -4 2 0 441.53 604.30 221.30 3 < 4 -3 2 0 8935.70 9809.00 465.20 3 o 7 -5 3 0 139.22 -38.80 188.50 3 < -2 -2 3 0 81217.00 80466.60 1164.40 3 o -9 0 3 0 209.86 257.60 182.80 3 < -5 -2 4 0 30836.00 28672.60 698.10 3 o 5 -6 5 0 164.95 47.00 189.00 3 < 2 -5 5 0 2624.40 2200.60 276.10 3 o -1 -4 5 0 5683.60 5888.40 393.90 3 o -8 -2 5 0 3790.20 4765.80 318.20 3 o -1 -5 6 0 2971.20 2891.10 274.20 3 o -4 -4 6 0 1872.60 547.80 220.10 3 < -1 6 -7 1 150.43 91.60 188.80 3 < 6 3 -6 1 570.18 204.50 210.40 3 < 3 4 -6 1 318.15 82.30 228.40 3 < -4 6 -6 1 313.87 191.10 178.00 3 < -3 5 -5 1 1731.90 994.30 229.50 3 o 7 1 -4 1 79.55 83.50 210.50 3 < 4 2 -4 1 1395.30 2124.90 307.80 3 o -6 5 -4 1 117.88 482.40 179.20 3 < -2 3 -3 1 1022.70 2013.40 351.60 3 o 8 -1 -2 1 74.85 87.40 209.20 3 < -5 3 -2 1 1183.30 1586.90 311.20 3 o -8 3 -1 1 181.12 152.40 211.20 3 < -7 2 0 1 505.89 468.10 220.50 3 < 6 -3 1 1 62.95 141.10 220.50 3 < 4 -4 3 1 315.12 320.40 261.50 3 < 1 -3 3 1 2126.60 2254.90 365.30 3 o -2 -3 4 1 2761.90 2252.20 357.80 3 o -5 -2 4 1 108.24 1633.20 329.30 3 o -9 -1 4 1 55.85 437.70 217.70 3 < -5 -3 5 1 89.54 496.40 253.80 3 < -8 -2 5 1 207.92 247.00 210.80 3 < 2 -6 6 1 193.87 -242.90 202.00 3 < -1 -5 6 1 409.87 700.50 215.90 3 o -8 -3 6 1 99.75 245.80 185.40 3 < -1 -6 7 1 71.32 -85.10 186.80 3 < -4 -5 7 1 106.97 331.20 185.20 3 < 0 6 -7 -1 31.96 111.30 172.40 4 < 4 4 -6 -1 76.39 -20.20 203.30 4 < 1 5 -6 -1 58.68 221.80 206.90 4 < 8 2 -5 -1 137.48 204.20 208.90 4 < -2 5 -5 -1 118.42 390.10 197.10 4 < 8 1 -4 -1 133.67 -65.30 205.60 4 < 5 2 -4 -1 208.26 173.20 301.50 4 < 2 3 -4 -1 2430.40 2115.00 328.20 4 o -5 5 -4 -1 70.04 118.30 186.10 4 < -1 3 -3 -1 1704.70 2508.30 327.30 4 o 9 -1 -2 -1 54.13 279.10 196.60 4 < -4 3 -2 -1 2011.10 1643.50 315.00 4 o 0 1 -1 -1 3250.80 2206.00 697.40 4 o -7 3 -1 -1 1599.40 272.20 194.70 4 < -3 1 0 -1 5403.40 3455.70 434.70 4 o -7 2 0 -1 239.71 157.90 189.30 4 < 7 -3 1 -1 301.96 319.90 208.90 4 < 4 -2 1 -1 546.13 1346.80 373.20 4 o -6 1 1 -1 1340.80 837.30 260.90 4 o -2 -2 3 -1 232.32 3429.70 496.20 4 o 5 -5 4 -1 498.98 -195.20 202.10 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12666.00 13186.30 530.30 89 o 5 1 7 0 3992.70 4540.50 362.80 89 o 3 3 8 0 1772.80 2341.90 277.60 89 o -1 6 8 0 475.57 401.00 212.60 89 < 4 3 9 0 1549.50 1465.90 243.20 89 o 5 3 10 0 77.58 155.90 190.40 89 < -4 -3 -9 1 24.21 -93.80 201.80 89 < 1 -6 -8 1 26.16 225.80 173.40 89 < 2 -6 -7 1 1451.50 1303.60 215.50 89 o -5 -1 -7 1 42.99 366.30 250.20 89 < 0 -4 -6 1 541.55 909.40 270.20 89 o -2 -2 -5 1 1023.80 434.00 343.40 89 < -6 1 -5 1 939.82 926.90 269.70 89 o 4 -5 -3 1 192.47 86.60 239.00 89 < -7 3 -3 1 167.50 235.70 207.40 89 < 5 -5 -2 1 306.66 698.90 223.50 89 o 2 -3 -2 1 484.34 701.20 369.00 89 < 3 -3 -1 1 3128.80 3668.50 396.90 89 o -4 2 -1 1 870.12 -188.70 363.20 89 < 1 -1 0 1 8739.90 2952.60 727.10 89 o -7 5 0 1 547.02 397.60 202.10 89 < 7 -4 2 1 430.32 386.00 208.50 89 < 0 1 2 1 21540.00 14913.40 856.50 89 o -4 4 2 1 309.10 903.60 299.80 89 o 6 -2 4 1 432.55 417.30 247.40 89 < 7 -2 5 1 264.59 -98.00 240.50 89 < 0 3 5 1 3920.70 4147.60 420.50 89 o -4 6 5 1 323.05 556.90 211.30 89 < -1 5 7 1 699.09 171.20 230.90 89 < 4 2 8 1 318.34 835.20 251.00 89 o 0 5 8 1 250.38 283.80 226.70 89 < 5 2 9 1 104.28 114.60 208.60 89 < 1 5 9 1 1166.40 2053.20 257.90 89 o -3 -3 -9 -1 566.08 20.30 223.70 90 < 2 -6 -8 -1 49.21 195.60 172.10 90 < -5 -1 -8 -1 104.37 141.60 213.10 90 < 3 -6 -7 -1 235.85 480.10 201.90 90 < 0 -4 -7 -1 181.38 120.30 234.40 90 < -2 -2 -6 -1 297.41 -408.80 313.80 90 < -6 1 -6 -1 313.10 183.70 209.90 90 < 4 -5 -4 -1 418.81 924.50 244.60 90 o -7 3 -4 -1 52.62 236.00 185.60 90 < 5 -5 -3 -1 46.53 -102.10 235.70 90 < 2 -3 -3 -1 452.70 483.00 343.60 90 < -4 2 -2 -1 4861.90 4320.30 401.60 90 o -1 1 0 -1 9810.90 3114.90 708.80 90 o -5 4 0 -1 3085.60 1479.30 265.90 90 o 7 -4 1 -1 389.66 1052.60 240.70 90 o 8 -4 2 -1 182.22 480.00 224.30 90 < 5 -2 2 -1 5296.40 9050.40 484.00 90 o -2 3 2 -1 248.83 490.00 343.90 90 < -3 5 4 -1 78.07 571.90 215.60 90 < 2 2 5 -1 990.63 694.60 352.00 90 < 8 -1 7 -1 46.49 316.30 197.40 90 < 1 4 7 -1 179.68 -39.50 245.60 90 < 6 1 8 -1 78.10 16.50 219.80 90 < 7 1 9 -1 18.03 211.20 202.60 90 < 5 3 10 -1 7.61 281.90 179.50 90 < -2 -4 -9 0 1537.30 1689.20 270.50 90 o -4 -2 -8 0 363.59 560.00 242.80 90 < 1 -5 -7 0 300.28 676.80 221.80 90 o 2 -5 -6 0 3486.00 2459.20 272.60 90 o -5 0 -6 0 4773.10 5809.30 398.90 90 o 0 -3 -5 0 16669.00 12440.40 553.70 90 o -7 2 -5 0 8410.10 6376.70 387.00 90 o -2 -1 -4 0 8732.70 7736.00 517.10 90 o -6 2 -4 0 4248.30 3504.20 322.30 90 o 4 -4 -2 0 8592.80 9233.10 472.30 90 o -7 4 -2 0 1121.10 1024.70 241.00 90 o -5 3 -1 0 5731.80 7212.30 432.80 90 o -6 5 1 0 1340.90 1121.20 244.90 90 o 6 -3 2 0 2694.70 3175.00 322.80 90 o -1 2 2 0 81048.00 71774.10 1162.30 90 o -5 5 2 0 629.96 803.10 234.50 90 o 7 -3 3 0 517.09 950.00 238.40 90 o 4 -1 3 0 34436.00 41148.10 871.20 90 o 5 -1 4 0 19945.00 20710.00 648.40 90 o -2 4 4 0 4784.40 6244.70 418.10 90 o 3 1 5 0 9143.40 10882.70 512.60 90 o -3 6 6 0 140.98 899.10 217.20 90 o 2 3 7 0 1007.70 1165.80 286.30 90 o -2 6 7 0 386.84 333.90 217.20 90 < 7 0 8 0 1954.40 1566.80 243.30 90 o 1 5 9 0 414.06 742.80 231.30 90 o -6 -2 -10 1 71.26 9.00 187.20 90 < -1 -5 -9 1 250.42 163.50 206.90 90 < 0 -5 -8 1 560.61 781.20 217.50 90 o -3 -3 -8 1 325.84 -79.80 244.60 90 < 3 -6 -6 1 127.00 221.00 183.70 90 < -4 -1 -6 1 189.00 497.90 292.80 90 < -8 2 -6 1 131.96 -360.40 201.70 90 < 4 -6 -5 1 1253.60 661.70 230.90 90 < 1 -4 -5 1 2218.00 2809.00 346.50 90 o -6 1 -5 1 798.94 1140.30 255.30 90 o -1 -2 -4 1 158.26 839.80 410.10 90 < -7 3 -3 1 50.25 -54.80 197.60 90 < 5 -5 -2 1 71.52 413.10 240.90 90 < 6 -5 -1 1 116.55 663.80 235.70 90 < 3 -3 -1 1 2670.90 4205.70 397.50 90 o -4 2 -1 1 1539.60 1002.50 356.80 90 < -7 5 0 1 956.57 359.10 218.30 90 < -5 4 1 1 2273.50 2612.10 320.30 90 o -6 6 3 1 415.28 250.60 179.60 90 < 6 -2 4 1 561.79 651.80 272.00 90 < -1 3 4 1 1230.70 507.00 353.60 90 < -5 6 4 1 224.98 48.70 196.60 90 < 7 -2 5 1 262.82 2612.50 313.50 90 o -2 5 6 1 2150.90 1636.20 263.40 90 o 3 2 7 1 182.92 1001.10 284.80 90 o 4 2 8 1 105.56 521.80 232.80 90 < 2 4 9 1 11.74 716.10 229.00 90 o 3 4 10 1 464.64 427.30 230.40 90 < -2 -4 -10 -1 191.80 461.40 190.80 91 < -5 -2 -10 -1 54.31 158.40 190.20 91 < -4 -2 -9 -1 968.69 690.50 215.30 91 o 1 -5 -8 -1 374.36 508.00 217.80 91 < -2 -3 -8 -1 95.66 254.20 228.80 91 < -4 -1 -7 -1 418.10 465.60 252.60 91 < 4 -6 -6 -1 288.03 341.70 191.60 91 < 5 -6 -5 -1 241.04 615.50 210.30 91 < 2 -4 -5 -1 1736.40 2790.00 337.30 91 o -5 1 -5 -1 360.42 439.50 278.10 91 < -7 3 -4 -1 93.13 90.80 189.10 91 < 5 -5 -3 -1 214.86 576.50 228.70 91 < 6 -5 -2 -1 234.08 700.70 225.40 91 o 3 -3 -2 -1 440.53 1445.90 336.90 91 o -4 2 -2 -1 3640.80 3880.60 402.30 91 o -6 4 -1 -1 250.74 153.10 207.10 91 < -1 1 0 -1 10272.00 3751.00 707.20 91 o 7 -4 1 -1 273.39 721.50 239.30 91 o -3 3 1 -1 3054.50 2896.80 401.30 91 o 8 -4 2 -1 178.29 -78.60 215.10 91 < -4 5 3 -1 289.76 426.90 203.50 91 < 6 -1 5 -1 1102.70 306.60 289.50 91 < -1 4 5 -1 2329.90 2001.80 337.40 91 o 7 -1 6 -1 105.54 -132.60 232.60 91 < 4 1 6 -1 265.96 798.80 310.80 91 < 5 1 7 -1 40.10 30.60 269.60 91 < -2 6 7 -1 1484.80 787.90 221.70 91 o 3 3 8 -1 391.83 -186.90 254.80 91 < 1 5 9 -1 251.66 -89.80 227.30 91 < 6 2 10 -1 112.65 72.20 196.10 91 < -1 -5 -10 0 101.16 -14.00 186.10 91 < -3 -3 -9 0 77.16 596.30 211.10 91 < 2 -6 -8 0 282.12 144.30 191.70 91 < -5 -1 -8 0 1819.10 955.20 235.60 91 o -7 1 -7 0 728.46 193.90 206.70 91 < 3 -5 -5 0 677.51 632.70 221.90 91 < -8 3 -5 0 615.98 218.00 192.70 91 < 1 -3 -4 0 10142.00 10162.80 514.50 91 o -6 2 -4 0 2641.60 2803.20 322.90 91 o 4 -4 -2 0 8968.00 9889.70 471.90 91 o -3 1 -2 0 4583.10 3024.60 481.50 91 o -7 4 -2 0 1348.70 489.50 227.20 91 < 5 -4 -1 0 1010.00 1186.50 280.90 91 o 2 -2 -1 0 44813.00 52093.90 1005.50 91 o -5 3 -1 0 6092.00 4718.30 395.20 91 o -6 5 1 0 1176.10 1209.30 250.00 91 o 6 -3 2 0 1757.80 1548.70 271.50 91 o 7 -3 3 0 1383.40 1794.60 276.30 91 o 4 -1 3 0 39603.00 45417.10 910.60 91 o -3 4 3 0 6689.10 5508.60 415.00 91 o 2 1 4 0 4971.70 6173.60 503.60 91 o 0 3 5 0 17521.00 13375.50 573.10 91 o -4 6 5 0 529.73 339.50 201.80 91 < 8 -2 6 0 499.37 -216.10 214.90 91 < 6 0 7 0 3566.30 2423.90 307.40 91 o -1 5 7 0 2006.80 1672.30 259.00 91 o 4 2 8 0 144.31 -257.50 245.60 91 < 2 4 9 0 1454.60 1084.80 254.20 91 o 3 4 10 0 184.80 90.50 208.50 91 < -2 -4 -9 1 1128.30 769.60 223.80 91 o -4 -2 -8 1 169.81 -22.70 231.30 91 < 1 -5 -7 1 105.26 85.80 217.30 91 < -1 -3 -6 1 413.41 494.50 315.20 91 < -8 2 -6 1 84.68 -20.10 192.30 91 < 5 -6 -4 1 152.80 220.50 212.50 91 < 2 -4 -4 1 700.94 1080.60 301.10 91 o -5 1 -4 1 418.45 744.30 305.00 91 < 0 -2 -3 1 13993.00 13391.70 645.20 91 o -7 3 -3 1 130.89 -561.70 234.40 91 < 6 -5 -1 1 247.76 880.40 228.40 91 o -4 2 -1 1 940.96 1307.70 351.10 91 o 7 -5 0 1 75.38 512.30 203.80 91 < -5 4 1 1 2208.10 1143.50 273.80 91 o 5 -2 3 1 415.90 419.30 296.30 91 < -2 3 3 1 187.41 499.20 342.30 91 < -6 6 3 1 313.10 223.40 176.70 91 < 6 -2 4 1 562.73 563.60 248.80 91 < -4 5 4 1 243.42 428.20 232.30 91 < 1 2 5 1 2358.90 2804.80 386.90 91 o -3 5 5 1 1113.20 675.90 249.60 91 < 7 -1 7 1 98.78 228.10 204.20 91 < 0 4 7 1 391.63 664.00 244.10 91 < 5 1 8 1 22.84 -136.60 224.30 91 < -2 6 8 1 34.06 66.50 200.30 91 < 6 1 9 1 81.41 99.90 215.10 91 < 3 3 9 1 491.14 179.40 221.10 91 < 4 3 10 1 50.52 -30.90 194.50 91 < #======================================================================= data_2p5K_average_dyn #data_I #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Ca8 O16 Si4' _chemical_formula_weight 689 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P n m a' _space_group_name_Hall '-P -2xabc;-2yb;-2zac' _space_group_IT_number 62 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,-y,z+1/2 3 -x,y+1/2,-z 4 x+1/2,-y+1/2,-z+1/2 5 -x,-y,-z 6 x+1/2,y,-z+1/2 7 x,-y+1/2,z 8 -x+1/2,y+1/2,z+1/2 _cell_length_a 6.765 _cell_length_b 5.514 _cell_length_c 9.25 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 345.0454 _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 3.3157 _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 0 _exptl_crystal_description 'Nanocrystals of up to 500 nm in size' #======================================================================= # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 293 _diffrn_radiation_type electron _diffrn_radiation_wavelength 0.0197 _diffrn_measurement_device 'FEI Tecnai F30' _diffrn_measurement_device_type 'TEM' _diffrn_detector 'Gatan UltraScan4000' _diffrn_reflns_number 10062 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_radiation_probe electron #======================================================================= # 8. REFINEMENT DATA _refine_special_details ? _reflns_number_total 1995 _reflns_number_gt 1488 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_gt 0.0607 _refine_ls_R_factor_all 0.0708 _refine_ls_wR_factor_ref 0.0623 _refine_ls_goodness_of_fit_ref 2.37 _refine_ls_goodness_of_fit_gt 2.09 _refine_ls_number_reflns 1995 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_shift/su_max 0.0417 _refine_ls_shift/su_mean 0.0057 _refine_ls_extinction_method 'none' loop_ _atom_type_symbol _atom_type_scat_source Ca International_Tables_Vol_C O International_Tables_Vol_C Si International_Tables_Vol_C #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.16773(15) 0.75 0.42906(13) Uani 0.0256(5) 4 1 d . . . Ca2 Ca 0.50905(13) 0.75 0.70488(13) Uani 0.0172(4) 4 1 d . . . Si1 Si 0.28113(18) 0.25 0.58717(17) Uani 0.0170(6) 4 1 d . . . O1 O 0.7470(7) 0.4794(8) 0.8050(5) Uani 0.0313(14) 8 0.647(5) d . . . O2 O 0.4946(5) 0.770(4) 0.4509(4) Uani 0.095(3) 8 0.5 d . . . O3 O 0.1579(4) 0.3184(9) 0.4389(4) Uani 0.032(2) 8 0.5 d . . . O1_2 O 0.6761(12) 0.4871(16) 0.8553(12) Uani 0.0313(14) 8 0.353(2) d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ca1 Ca 0.0156(5) 0.0412(11) 0.0200(8) 0 0.0016(5) 0 Ca2 Ca 0.0114(5) 0.0286(8) 0.0117(6) 0 -0.0009(4) 0 Si1 Si 0.0146(7) 0.0258(13) 0.0106(10) 0 -0.0008(6) 0 O1 O 0.030(2) 0.0249(19) 0.039(3) -0.0082(18) -0.0135(17) 0.0129(19) O2 O 0.0247(17) 0.239(10) 0.020(2) 0.067(6) 0.0038(14) 0.007(7) O3 O 0.0181(13) 0.060(6) 0.018(2) 0.0032(17) -0.0090(12) -0.0079(17) O1_2 O 0.030(2) 0.0249(19) 0.039(3) -0.0082(18) -0.0135(17) 0.0129(19) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ca1 Ca1 . 3_546 3.8044(10) ? Ca1 Ca1 . 3_556 3.8044(10) ? Ca1 Ca2 . . 3.4411(15) ? Ca1 Ca2 . 2_564 3.6512(11) ? Ca1 Ca2 . 2_574 3.6512(11) ? Ca1 Ca2 . 3_646 3.7306(10) ? Ca1 Ca2 . 3_656 3.7306(10) ? Ca1 Ca2 . 4_466 3.5521(17) ? Ca1 Si1 . . 3.2138(10) ? Ca1 Si1 . 1_565 3.2138(10) ? Ca1 Si1 . 2_564 3.181(2) ? Ca1 Si1 . 3_556 3.0402(16) ? Ca1 O2 . . 2.223(4) ? Ca1 O2 . 7_565 2.223(4) ? Ca1 O3 . . 2.383(5) ? Ca1 O3 . 7_565 2.383(5) ? Ca2 Ca2 . 4_466 3.4840(13) ? Ca2 Ca2 . 4_566 3.4840(13) ? Ca2 Si1 . 3_656 3.0517(19) ? Ca2 O1 . . 2.382(5) ? Ca2 O1 . 4_466 2.319(5) ? Ca2 O1 . 6_456 2.319(5) ? Ca2 O1 . 7_565 2.382(5) ? Ca2 O2 . . 2.354(4) ? Ca2 O2 . 7_565 2.354(4) ? Ca2 O1_2 . . 2.305(10) ? Ca2 O1_2 . 7_565 2.305(10) ? Si1 O1 . 4_456 1.627(5) ? Si1 O1 . 6_456 1.627(5) ? Si1 O2 . 3_646 1.561(4) ? Si1 O2 . 5_666 1.561(4) ? Si1 O3 . . 1.649(4) ? Si1 O3 . 7_555 1.649(4) ? Si1 O1_2 . 4_456 1.580(9) ? Si1 O1_2 . 6_456 1.580(9) ? O1 O1_2 . . 0.670(11) ? O2 O2 . 7_565 0.22(3) ? O3 O3 . 7_555 0.754(7) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Ca1 Ca1 Ca1 3_546 . 3_556 92.89(3) ? Ca1 Ca1 Ca2 3_546 . . 98.31(3) ? Ca1 Ca1 Ca2 3_546 . 2_564 56.86(2) ? Ca1 Ca1 Ca2 3_546 . 2_574 123.21(3) ? Ca1 Ca1 Ca2 3_546 . 3_646 85.908(16) ? Ca1 Ca1 Ca2 3_546 . 3_656 178.75(3) ? Ca1 Ca1 Ca2 3_546 . 4_466 59.40(2) ? Ca1 Ca1 Si1 3_546 . . 50.49(3) ? Ca1 Ca1 Si1 3_546 . 1_565 127.38(5) ? Ca1 Ca1 Si1 3_546 . 2_564 114.07(3) ? Ca1 Ca1 Si1 3_546 . 3_556 54.64(2) ? Ca1 Ca1 O2 3_546 . . 126.7(5) ? Ca1 Ca1 O2 3_546 . 7_565 121.7(5) ? Ca1 Ca1 O3 3_546 . . 41.09(7) ? Ca1 Ca1 O3 3_546 . 7_565 133.95(8) ? Ca1 Ca1 Ca2 3_556 . . 98.31(3) ? Ca1 Ca1 Ca2 3_556 . 2_564 123.21(3) ? Ca1 Ca1 Ca2 3_556 . 2_574 56.86(2) ? Ca1 Ca1 Ca2 3_556 . 3_646 178.75(3) ? Ca1 Ca1 Ca2 3_556 . 3_656 85.908(16) ? Ca1 Ca1 Ca2 3_556 . 4_466 59.40(2) ? Ca1 Ca1 Si1 3_556 . . 127.38(5) ? Ca1 Ca1 Si1 3_556 . 1_565 50.49(3) ? Ca1 Ca1 Si1 3_556 . 2_564 114.07(3) ? Ca1 Ca1 Si1 3_556 . 3_556 54.64(2) ? Ca1 Ca1 O2 3_556 . . 121.7(5) ? Ca1 Ca1 O2 3_556 . 7_565 126.7(5) ? Ca1 Ca1 O3 3_556 . . 133.95(8) ? Ca1 Ca1 O3 3_556 . 7_565 41.09(7) ? Ca2 Ca1 Ca2 . . 2_564 129.857(19) ? Ca2 Ca1 Ca2 . . 2_574 129.857(19) ? Ca2 Ca1 Ca2 . . 3_646 81.54(3) ? Ca2 Ca1 Ca2 . . 3_656 81.54(3) ? Ca2 Ca1 Ca2 . . 4_466 59.74(3) ? Ca2 Ca1 Si1 . . . 60.16(3) ? Ca2 Ca1 Si1 . . 1_565 60.16(3) ? Ca2 Ca1 Si1 . . 2_564 131.61(4) ? Ca2 Ca1 Si1 . . 3_556 134.98(5) ? Ca2 Ca1 O2 . . . 42.71(10) ? Ca2 Ca1 O2 . . 7_565 42.71(10) ? Ca2 Ca1 O3 . . . 89.45(8) ? Ca2 Ca1 O3 . . 7_565 89.45(8) ? Ca2 Ca1 Ca2 2_564 . 2_574 98.07(3) ? Ca2 Ca1 Ca2 2_564 . 3_646 56.31(2) ? Ca2 Ca1 Ca2 2_564 . 3_656 124.15(4) ? Ca2 Ca1 Ca2 2_564 . 4_466 116.26(3) ? Ca2 Ca1 Si1 2_564 . . 71.87(3) ? Ca2 Ca1 Si1 2_564 . 1_565 169.87(4) ? Ca2 Ca1 Si1 2_564 . 2_564 58.07(3) ? Ca2 Ca1 Si1 2_564 . 3_556 69.20(3) ? Ca2 Ca1 O2 2_564 . . 114.5(5) ? Ca2 Ca1 O2 2_564 . 7_565 109.9(5) ? Ca2 Ca1 O3 2_564 . . 42.12(9) ? Ca2 Ca1 O3 2_564 . 7_565 140.07(9) ? Ca2 Ca1 Ca2 2_574 . 3_646 124.15(4) ? Ca2 Ca1 Ca2 2_574 . 3_656 56.31(2) ? Ca2 Ca1 Ca2 2_574 . 4_466 116.26(3) ? Ca2 Ca1 Si1 2_574 . . 169.87(4) ? Ca2 Ca1 Si1 2_574 . 1_565 71.87(3) ? Ca2 Ca1 Si1 2_574 . 2_564 58.07(3) ? Ca2 Ca1 Si1 2_574 . 3_556 69.20(3) ? Ca2 Ca1 O2 2_574 . . 109.9(5) ? Ca2 Ca1 O2 2_574 . 7_565 114.5(5) ? Ca2 Ca1 O3 2_574 . . 140.07(9) ? Ca2 Ca1 O3 2_574 . 7_565 42.12(9) ? Ca2 Ca1 Ca2 3_646 . 3_656 95.30(3) ? Ca2 Ca1 Ca2 3_646 . 4_466 119.58(3) ? Ca2 Ca1 Si1 3_646 . . 51.48(3) ? Ca2 Ca1 Si1 3_646 . 1_565 130.18(4) ? Ca2 Ca1 Si1 3_646 . 2_564 66.80(3) ? Ca2 Ca1 Si1 3_646 . 3_556 124.68(3) ? Ca2 Ca1 O2 3_646 . . 58.9(5) ? Ca2 Ca1 O2 3_646 . 7_565 53.9(5) ? Ca2 Ca1 O3 3_646 . . 44.83(7) ? Ca2 Ca1 O3 3_646 . 7_565 140.11(8) ? Ca2 Ca1 Ca2 3_656 . 4_466 119.58(3) ? Ca2 Ca1 Si1 3_656 . . 130.18(4) ? Ca2 Ca1 Si1 3_656 . 1_565 51.48(3) ? Ca2 Ca1 Si1 3_656 . 2_564 66.80(3) ? Ca2 Ca1 Si1 3_656 . 3_556 124.68(3) ? Ca2 Ca1 O2 3_656 . . 53.9(5) ? Ca2 Ca1 O2 3_656 . 7_565 58.9(5) ? Ca2 Ca1 O3 3_656 . . 140.11(8) ? Ca2 Ca1 O3 3_656 . 7_565 44.83(7) ? Ca2 Ca1 Si1 4_466 . . 68.80(3) ? Ca2 Ca1 Si1 4_466 . 1_565 68.80(3) ? Ca2 Ca1 Si1 4_466 . 2_564 168.65(4) ? Ca2 Ca1 Si1 4_466 . 3_556 75.24(4) ? Ca2 Ca1 O2 4_466 . . 102.35(10) ? Ca2 Ca1 O2 4_466 . 7_565 102.35(10) ? Ca2 Ca1 O3 4_466 . . 87.43(9) ? Ca2 Ca1 O3 4_466 . 7_565 87.43(9) ? Si1 Ca1 Si1 . . 1_565 118.15(5) ? Si1 Ca1 Si1 . . 2_564 115.24(3) ? Si1 Ca1 Si1 . . 3_556 105.12(3) ? Si1 Ca1 O2 . . . 76.3(5) ? Si1 Ca1 O2 . . 7_565 71.3(5) ? Si1 Ca1 O3 . . . 29.82(9) ? Si1 Ca1 O3 . . 7_565 147.80(10) ? Si1 Ca1 Si1 1_565 . 2_564 115.24(3) ? Si1 Ca1 Si1 1_565 . 3_556 105.12(3) ? Si1 Ca1 O2 1_565 . . 71.3(5) ? Si1 Ca1 O2 1_565 . 7_565 76.3(5) ? Si1 Ca1 O3 1_565 . . 147.80(10) ? Si1 Ca1 O3 1_565 . 7_565 29.82(9) ? Si1 Ca1 Si1 2_564 . 3_556 93.41(5) ? Si1 Ca1 O2 2_564 . . 88.98(10) ? Si1 Ca1 O2 2_564 . 7_565 88.98(10) ? Si1 Ca1 O3 2_564 . . 92.35(9) ? Si1 Ca1 O3 2_564 . 7_565 92.35(9) ? Si1 Ca1 O2 3_556 . . 176.3(4) ? Si1 Ca1 O2 3_556 . 7_565 176.3(4) ? Si1 Ca1 O3 3_556 . . 88.51(7) ? Si1 Ca1 O3 3_556 . 7_565 88.51(7) ? O2 Ca1 O2 . . 7_565 5.7(8) ? O2 Ca1 O3 . . . 94.2(6) ? O2 Ca1 O3 . . 7_565 88.6(6) ? O2 Ca1 O3 7_565 . . 88.6(6) ? O2 Ca1 O3 7_565 . 7_565 94.2(6) ? O3 Ca1 O3 . . 7_565 174.58(13) ? Ca1 Ca2 Ca1 . . 2_565 101.61(3) ? Ca1 Ca2 Ca1 . . 2_575 101.61(3) ? Ca1 Ca2 Ca1 . . 3_646 98.46(3) ? Ca1 Ca2 Ca1 . . 3_656 98.46(3) ? Ca1 Ca2 Ca1 . . 4_566 155.44(4) ? Ca1 Ca2 Ca2 . . 4_466 61.72(3) ? Ca1 Ca2 Ca2 . . 4_566 146.01(4) ? Ca1 Ca2 Si1 . . 3_656 69.86(4) ? Ca1 Ca2 O1 . . . 137.87(11) ? Ca1 Ca2 O1 . . 4_466 57.17(12) ? Ca1 Ca2 O1 . . 6_456 57.17(12) ? Ca1 Ca2 O1 . . 7_565 137.87(11) ? Ca1 Ca2 O2 . . . 39.84(9) ? Ca1 Ca2 O2 . . 7_565 39.84(9) ? Ca1 Ca2 O1_2 . . . 140.9(2) ? Ca1 Ca2 O1_2 . . 7_565 140.9(2) ? Ca1 Ca2 Ca1 2_565 . 2_575 98.07(3) ? Ca1 Ca2 Ca1 2_565 . 3_646 79.78(2) ? Ca1 Ca2 Ca1 2_565 . 3_656 159.82(4) ? Ca1 Ca2 Ca1 2_565 . 4_566 63.74(3) ? Ca1 Ca2 Ca2 2_565 . 4_466 62.99(2) ? Ca1 Ca2 Ca2 2_565 . 4_566 100.48(3) ? Ca1 Ca2 Si1 2_565 . 3_656 130.93(2) ? Ca1 Ca2 O1 2_565 . . 61.81(11) ? Ca1 Ca2 O1 2_565 . 4_466 104.94(12) ? Ca1 Ca2 O1 2_565 . 6_456 44.45(12) ? Ca1 Ca2 O1 2_565 . 7_565 118.26(12) ? Ca1 Ca2 O2 2_565 . . 126.1(5) ? Ca1 Ca2 O2 2_565 . 7_565 121.2(5) ? Ca1 Ca2 O1_2 2_565 . . 48.9(2) ? Ca1 Ca2 O1_2 2_565 . 7_565 107.0(3) ? Ca1 Ca2 Ca1 2_575 . 3_646 159.82(4) ? Ca1 Ca2 Ca1 2_575 . 3_656 79.78(2) ? Ca1 Ca2 Ca1 2_575 . 4_566 63.74(3) ? Ca1 Ca2 Ca2 2_575 . 4_466 62.99(2) ? Ca1 Ca2 Ca2 2_575 . 4_566 100.48(3) ? Ca1 Ca2 Si1 2_575 . 3_656 130.93(2) ? Ca1 Ca2 O1 2_575 . . 118.26(12) ? Ca1 Ca2 O1 2_575 . 4_466 44.45(12) ? Ca1 Ca2 O1 2_575 . 6_456 104.94(12) ? Ca1 Ca2 O1 2_575 . 7_565 61.81(11) ? Ca1 Ca2 O2 2_575 . . 121.2(5) ? Ca1 Ca2 O2 2_575 . 7_565 126.1(5) ? Ca1 Ca2 O1_2 2_575 . . 107.0(3) ? Ca1 Ca2 O1_2 2_575 . 7_565 48.9(2) ? Ca1 Ca2 Ca1 3_646 . 3_656 95.30(3) ? Ca1 Ca2 Ca1 3_646 . 4_566 98.02(3) ? Ca1 Ca2 Ca2 3_646 . 4_466 130.438(18) ? Ca1 Ca2 Ca2 3_646 . 4_566 60.69(2) ? Ca1 Ca2 Si1 3_646 . 3_656 55.49(2) ? Ca1 Ca2 O1 3_646 . . 43.13(11) ? Ca1 Ca2 O1 3_646 . 4_466 155.58(12) ? Ca1 Ca2 O1 3_646 . 6_456 87.68(11) ? Ca1 Ca2 O1 3_646 . 7_565 101.30(11) ? Ca1 Ca2 O2 3_646 . . 74.2(4) ? Ca1 Ca2 O2 3_646 . 7_565 70.0(4) ? Ca1 Ca2 O1_2 3_646 . . 56.5(3) ? Ca1 Ca2 O1_2 3_646 . 7_565 112.2(2) ? Ca1 Ca2 Ca1 3_656 . 4_566 98.02(3) ? Ca1 Ca2 Ca2 3_656 . 4_466 130.438(18) ? Ca1 Ca2 Ca2 3_656 . 4_566 60.69(2) ? Ca1 Ca2 Si1 3_656 . 3_656 55.49(2) ? Ca1 Ca2 O1 3_656 . . 101.30(11) ? Ca1 Ca2 O1 3_656 . 4_466 87.68(11) ? Ca1 Ca2 O1 3_656 . 6_456 155.58(12) ? Ca1 Ca2 O1 3_656 . 7_565 43.13(11) ? Ca1 Ca2 O2 3_656 . . 70.0(4) ? Ca1 Ca2 O2 3_656 . 7_565 74.2(4) ? Ca1 Ca2 O1_2 3_656 . . 112.2(2) ? Ca1 Ca2 O1_2 3_656 . 7_565 56.5(3) ? Ca1 Ca2 Ca2 4_566 . 4_466 93.73(4) ? Ca1 Ca2 Ca2 4_566 . 4_566 58.55(3) ? Ca1 Ca2 Si1 4_566 . 3_656 134.69(4) ? Ca1 Ca2 O1 4_566 . . 54.92(11) ? Ca1 Ca2 O1 4_566 . 4_466 105.58(12) ? Ca1 Ca2 O1 4_566 . 6_456 105.58(12) ? Ca1 Ca2 O1 4_566 . 7_565 54.92(11) ? Ca1 Ca2 O2 4_566 . . 164.56(13) ? Ca1 Ca2 O2 4_566 . 7_565 164.56(13) ? Ca1 Ca2 O1_2 4_566 . . 43.7(3) ? Ca1 Ca2 O1_2 4_566 . 7_565 43.7(3) ? Ca2 Ca2 Ca2 4_466 . 4_566 152.28(5) ? Ca2 Ca2 Si1 4_466 . 3_656 131.58(5) ? Ca2 Ca2 O1 4_466 . . 124.26(12) ? Ca2 Ca2 O1 4_466 . 4_466 42.88(11) ? Ca2 Ca2 O1 4_466 . 6_456 42.88(11) ? Ca2 Ca2 O1 4_466 . 7_565 124.26(12) ? Ca2 Ca2 O2 4_466 . . 101.47(9) ? Ca2 Ca2 O2 4_466 . 7_565 101.47(9) ? Ca2 Ca2 O1_2 4_466 . . 109.3(2) ? Ca2 Ca2 O1_2 4_466 . 7_565 109.3(2) ? Ca2 Ca2 Si1 4_566 . 3_656 76.14(4) ? Ca2 Ca2 O1 4_566 . . 41.48(11) ? Ca2 Ca2 O1 4_566 . 4_466 138.73(11) ? Ca2 Ca2 O1 4_566 . 6_456 138.73(11) ? Ca2 Ca2 O1 4_566 . 7_565 41.48(11) ? Ca2 Ca2 O2 4_566 . . 106.23(9) ? Ca2 Ca2 O2 4_566 . 7_565 106.23(9) ? Ca2 Ca2 O1_2 4_566 . . 51.6(2) ? Ca2 Ca2 O1_2 4_566 . 7_565 51.6(2) ? Si1 Ca2 O1 3_656 . . 91.71(12) ? Si1 Ca2 O1 3_656 . 4_466 108.71(12) ? Si1 Ca2 O1 3_656 . 6_456 108.71(12) ? Si1 Ca2 O1 3_656 . 7_565 91.71(12) ? Si1 Ca2 O2 3_656 . . 30.21(10) ? Si1 Ca2 O2 3_656 . 7_565 30.21(10) ? Si1 Ca2 O1_2 3_656 . . 107.8(2) ? Si1 Ca2 O1_2 3_656 . 7_565 107.8(2) ? O1 Ca2 O1 . . 4_466 159.21(17) ? O1 Ca2 O1 . . 6_456 97.41(16) ? O1 Ca2 O1 . . 7_565 77.56(16) ? O1 Ca2 O2 . . . 116.4(4) ? O1 Ca2 O2 . . 7_565 112.7(4) ? O1 Ca2 O1_2 . . . 16.3(3) ? O1 Ca2 O1_2 . . 7_565 80.1(2) ? O1 Ca2 O1 4_466 . 6_456 80.10(16) ? O1 Ca2 O1 4_466 . 7_565 97.41(16) ? O1 Ca2 O2 4_466 . . 84.2(4) ? O1 Ca2 O2 4_466 . 7_565 87.7(4) ? O1 Ca2 O1_2 4_466 . . 143.4(3) ? O1 Ca2 O1_2 4_466 . 7_565 89.7(2) ? O1 Ca2 O1 6_456 . 7_565 159.21(17) ? O1 Ca2 O2 6_456 . . 87.7(4) ? O1 Ca2 O2 6_456 . 7_565 84.2(4) ? O1 Ca2 O1_2 6_456 . . 89.7(2) ? O1 Ca2 O1_2 6_456 . 7_565 143.4(3) ? O1 Ca2 O2 7_565 . . 112.7(4) ? O1 Ca2 O2 7_565 . 7_565 116.4(4) ? O1 Ca2 O1_2 7_565 . . 80.1(2) ? O1 Ca2 O1_2 7_565 . 7_565 16.3(3) ? O2 Ca2 O2 . . 7_565 5.4(8) ? O2 Ca2 O1_2 . . . 130.7(5) ? O2 Ca2 O1_2 . . 7_565 126.4(5) ? O2 Ca2 O1_2 7_565 . . 126.4(5) ? O2 Ca2 O1_2 7_565 . 7_565 130.7(5) ? O1_2 Ca2 O1_2 . . 7_565 77.9(3) ? Ca1 Si1 Ca1 1_545 . . 118.15(5) ? Ca1 Si1 Ca1 1_545 . 2_565 118.58(3) ? Ca1 Si1 Ca1 1_545 . 3_546 74.88(3) ? Ca1 Si1 Ca2 1_545 . 3_646 73.03(4) ? Ca1 Si1 O1 1_545 . 4_456 65.05(16) ? Ca1 Si1 O1 1_545 . 6_456 155.77(18) ? Ca1 Si1 O2 1_545 . 3_646 100.9(7) ? Ca1 Si1 O2 1_545 . 5_666 93.9(7) ? Ca1 Si1 O3 1_545 . . 72.36(17) ? Ca1 Si1 O3 1_545 . 7_555 45.93(17) ? Ca1 Si1 O1_2 1_545 . 4_456 48.4(4) ? Ca1 Si1 O1_2 1_545 . 6_456 139.1(3) ? Ca1 Si1 Ca1 . . 2_565 118.58(3) ? Ca1 Si1 Ca1 . . 3_546 74.88(3) ? Ca1 Si1 Ca2 . . 3_646 73.03(4) ? Ca1 Si1 O1 . . 4_456 155.77(18) ? Ca1 Si1 O1 . . 6_456 65.05(16) ? Ca1 Si1 O2 . . 3_646 93.9(7) ? Ca1 Si1 O2 . . 5_666 100.9(7) ? Ca1 Si1 O3 . . . 45.93(17) ? Ca1 Si1 O3 . . 7_555 72.36(17) ? Ca1 Si1 O1_2 . . 4_456 139.1(3) ? Ca1 Si1 O1_2 . . 6_456 48.4(4) ? Ca1 Si1 Ca1 2_565 . 3_546 99.07(5) ? Ca1 Si1 Ca2 2_565 . 3_646 146.04(5) ? Ca1 Si1 O1 2_565 . 4_456 53.57(17) ? Ca1 Si1 O1 2_565 . 6_456 53.57(17) ? Ca1 Si1 O2 2_565 . 3_646 96.81(15) ? Ca1 Si1 O2 2_565 . 5_666 96.81(15) ? Ca1 Si1 O3 2_565 . . 151.87(14) ? Ca1 Si1 O3 2_565 . 7_555 151.87(14) ? Ca1 Si1 O1_2 2_565 . 4_456 73.4(4) ? Ca1 Si1 O1_2 2_565 . 6_456 73.4(4) ? Ca1 Si1 Ca2 3_546 . 3_646 114.89(6) ? Ca1 Si1 O1 3_546 . 4_456 83.60(17) ? Ca1 Si1 O1 3_546 . 6_456 83.60(17) ? Ca1 Si1 O2 3_546 . 3_646 163.6(2) ? Ca1 Si1 O2 3_546 . 5_666 163.6(2) ? Ca1 Si1 O3 3_546 . . 56.90(11) ? Ca1 Si1 O3 3_546 . 7_555 56.90(11) ? Ca1 Si1 O1_2 3_546 . 4_456 64.4(3) ? Ca1 Si1 O1_2 3_546 . 6_456 64.4(3) ? Ca2 Si1 O1 3_646 . 4_456 127.49(17) ? Ca2 Si1 O1 3_646 . 6_456 127.49(17) ? Ca2 Si1 O2 3_646 . 3_646 49.34(15) ? Ca2 Si1 O2 3_646 . 5_666 49.34(15) ? Ca2 Si1 O3 3_646 . . 59.92(12) ? Ca2 Si1 O3 3_646 . 7_555 59.92(12) ? Ca2 Si1 O1_2 3_646 . 4_456 120.5(4) ? Ca2 Si1 O1_2 3_646 . 6_456 120.5(4) ? O1 Si1 O1 4_456 . 6_456 102.0(2) ? O1 Si1 O2 4_456 . 3_646 109.3(7) ? O1 Si1 O2 4_456 . 5_666 102.8(7) ? O1 Si1 O3 4_456 . . 128.0(2) ? O1 Si1 O3 4_456 . 7_555 105.1(2) ? O1 Si1 O1_2 4_456 . 4_456 24.0(4) ? O1 Si1 O1_2 4_456 . 6_456 111.9(4) ? O1 Si1 O2 6_456 . 3_646 102.8(7) ? O1 Si1 O2 6_456 . 5_666 109.3(7) ? O1 Si1 O3 6_456 . . 105.1(2) ? O1 Si1 O3 6_456 . 7_555 128.0(2) ? O1 Si1 O1_2 6_456 . 4_456 111.9(4) ? O1 Si1 O1_2 6_456 . 6_456 24.0(4) ? O2 Si1 O2 3_646 . 5_666 8.1(11) ? O2 Si1 O3 3_646 . . 106.7(3) ? O2 Si1 O3 3_646 . 7_555 108.7(3) ? O2 Si1 O1_2 3_646 . 4_456 124.8(8) ? O2 Si1 O1_2 3_646 . 6_456 117.0(8) ? O2 Si1 O3 5_666 . . 108.7(3) ? O2 Si1 O3 5_666 . 7_555 106.7(3) ? O2 Si1 O1_2 5_666 . 4_456 117.0(8) ? O2 Si1 O1_2 5_666 . 6_456 124.8(8) ? O3 Si1 O3 . . 7_555 26.4(2) ? O3 Si1 O1_2 . . 4_456 104.0(4) ? O3 Si1 O1_2 . . 6_456 82.2(4) ? O3 Si1 O1_2 7_555 . 4_456 82.2(4) ? O3 Si1 O1_2 7_555 . 6_456 104.0(4) ? O1_2 Si1 O1_2 4_456 . 6_456 111.6(5) ? Ca2 O1 Ca2 . . 4_566 95.64(16) ? Ca2 O1 Si1 . . 4_556 145.2(3) ? Ca2 O1 O1_2 . . . 75.3(9) ? Ca2 O1 Si1 4_566 . 4_556 114.6(2) ? Ca2 O1 O1_2 4_566 . . 122.3(9) ? Si1 O1 O1_2 4_556 . . 74.0(9) ? Ca1 O2 Ca2 . . . 97.45(15) ? Ca1 O2 Si1 . . 3_656 160.5(5) ? Ca1 O2 O2 . . 7_565 87.2(14) ? Ca2 O2 Si1 . . 3_656 100.5(2) ? Ca2 O2 O2 . . 7_565 87.3(15) ? Si1 O2 O2 3_656 . 7_565 85.9(15) ? Ca1 O3 Si1 . . . 104.3(2) ? Ca1 O3 O3 . . 7_555 177.3(4) ? Si1 O3 O3 . . 7_555 76.8(4) ? Ca2 O1_2 Si1 . . 4_556 160.7(6) ? Ca2 O1_2 O1 . . . 88.4(10) ? Si1 O1_2 O1 4_556 . . 81.9(9) ? #======================================================================= #======================================================================= data_2p5K_modulated_dyn #data_I #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Ca8 O16 Si4' _chemical_formula_weight 689 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system orthorhombic _space_group_ssg_name 'Pnma(\a00)0ss' loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1+1/2,-x2,x3+1/2,-x4+1/2 3 -x1,x2+1/2,-x3,-x4+1/2 4 x1+1/2,-x2+1/2,-x3+1/2,x4 5 -x1,-x2,-x3,-x4 6 x1+1/2,x2,-x3+1/2,x4+1/2 7 x1,-x2+1/2,x3,x4+1/2 8 -x1+1/2,x2+1/2,x3+1/2,-x4 _cell_length_a 6.765 _cell_length_b 5.514 _cell_length_c 9.25 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 345.0454 _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.379500 0.000000 0.000000 _cell_formula_units_Z 1 _cell_measurement_temperature 293 _cell_special_details ? _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 3.3157 _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 0 _exptl_crystal_description 'Nanocrystals of up to 500 nm in size' #======================================================================= # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 293 _diffrn_radiation_type electron _diffrn_radiation_wavelength 0.0197 _diffrn_measurement_device 'FEI Tecnai F30' _diffrn_measurement_device_type 'TEM' _diffrn_detector 'Gatan UltraScan4000' _diffrn_reflns_number 18230 _diffrn_reflns_theta_min 0.1 _diffrn_reflns_theta_max 0.79 _diffrn_reflns_theta_full 0.7 _diffrn_measured_fraction_theta_max 0.86 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_unetI/netI 0.0483 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_index_m_1_min -1 _diffrn_reflns_limit_index_m_1_max 1 _diffrn_radiation_probe electron #======================================================================= # 8. REFINEMENT DATA _refine_special_details ? _reflns_number_total 6997 _reflns_number_gt 3076 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0964 _refine_ls_wR_factor_gt 0.0985 _refine_ls_R_factor_all 0.1694 _refine_ls_wR_factor_ref 0.1049 _refine_ls_goodness_of_fit_ref 2.22 _refine_ls_goodness_of_fit_gt 3.14 _refine_ls_number_reflns 6997 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_shift/su_max 0.0248 _refine_ls_shift/su_mean 0.0043 _refine_ls_extinction_method 'none' loop_ _atom_type_symbol _atom_type_scat_source Ca International_Tables_Vol_C O International_Tables_Vol_C Si International_Tables_Vol_C #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.49106(12) 0.75 0.20467(11) Uiso 0.0091(2) 4 1 d . . . Ca2 Ca 0.83234(13) 0.75 -0.07067(11) Uiso 0.0169(3) 4 1 d . . . Si1 Si 0.21886(16) 0.25 0.41267(15) Uiso 0.0101(3) 4 1 d . . . O1 O 0.2760(3) 0.4818(4) 0.3217(2) Uiso 0.0278(5) 8 1 d . . . O2 O 0.6575(3) 0.8153(5) 0.4402(3) Uiso 0.0261(6) 8 0.5 d . . . O3 O 0.5086(3) 0.8056(5) -0.0482(3) Uiso 0.0270(7) 8 0.5 d . . . loop_ _atom_site_Fourier_wave_vector_seq_id _atom_site_Fourier_wave_vector_q1_coeff 1 1 loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w O2 0.496(2) 0.5 O3 0.777(2) 0.5 loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Ca1x1 Ca1 x 1 Ca1y1 Ca1 y 1 Ca1z1 Ca1 z 1 Ca2x1 Ca2 x 1 Ca2y1 Ca2 y 1 Ca2z1 Ca2 z 1 Si1x1 Si1 x 1 Si1y1 Si1 y 1 Si1z1 Si1 z 1 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Ca1x1 0 0 Ca1y1 -0.0105(4) 0.0274(3) Ca1z1 0 0 Ca2x1 0 0 Ca2y1 -0.0231(3) -0.0174(4) Ca2z1 0 0 Si1x1 0 0 Si1y1 0.0209(5) 0.0141(5) Si1z1 0 0 O1x1 -0.0333(4) 0.0257(4) O1y1 -0.0025(6) 0.0194(6) O1z1 -0.0292(3) 0.0106(4) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_ssg_symmetry_1 _geom_bond_site_ssg_symmetry_2 _geom_bond_distance_av _geom_bond_distance_min _geom_bond_distance_max _geom_bond_publ_flag Ca1 Ca1 . 4_4655 3.4900(11) 3.4849(11) 3.4952(11) ? Ca1 Ca1 . 4_5655 3.4901(11) 3.4849(11) 3.4952(11) ? Ca1 Ca2 . . 3.4394(13) 3.4375(13) 3.4412(13) ? Ca1 Ca2 . 2_6655 3.654(2) 3.637(2) 3.670(2) ? Ca1 Ca2 . 2_6755 3.653(2) 3.637(2) 3.670(2) ? Ca1 Ca2 . 3_6455 3.734(2) 3.549(2) 3.922(2) ? Ca1 Ca2 . 3_6555 3.733(2) 3.549(2) 3.922(2) ? Ca1 Ca2 . 4_4655 3.5531(14) 3.5517(14) 3.5545(14) ? Ca1 Si1 . 2_5645 3.0568(16) 3.0515(16) 3.0622(16) ? Ca1 Si1 . 4_5555 3.342(3) 3.195(3) 3.487(3) ? Ca1 Si1 . 4_5655 3.339(3) 3.195(3) 3.487(3) ? Ca1 O1 . . 2.357(4) 2.318(4) 2.420(4) ? Ca1 O1 . 4_5655 2.464(4) 2.359(4) 2.595(4) ? Ca1 O1 . 6_5555 2.463(4) 2.359(4) 2.595(4) ? Ca1 O1 . 7_5655 2.357(4) 2.318(4) 2.420(4) ? Ca1 O3 . . 2.377(3) 2.358(3) 2.388(3) ? Ca1 O3 . 7_5655 2.377(3) 2.358(3) 2.388(3) ? Ca2 Ca2 . 3_7455 3.804(2) 3.688(2) 3.920(2) ? Ca2 Ca2 . 3_7555 3.802(2) 3.688(2) 3.920(2) ? Ca2 Si1 . 2_6645 3.0413(14) 3.0401(14) 3.0425(14) ? Ca2 Si1 . 3_6555 3.1844(17) 3.1824(17) 3.1864(17) ? Ca2 Si1 . 4_5555 3.214(3) 3.181(3) 3.246(3) ? Ca2 Si1 . 4_5655 3.213(3) 3.181(3) 3.246(3) ? Ca2 O1 . 3_6555 2.755(4) 2.340(4) 3.173(4) ? Ca2 O1 . 4_5655 2.767(4) 2.415(4) 3.130(4) ? Ca2 O1 . 5_6655 2.752(4) 2.340(4) 3.173(4) ? Ca2 O1 . 6_5555 2.771(4) 2.415(4) 3.130(4) ? Ca2 O2 . 2_6745 2.481(4) 2.309(4) 2.559(4) ? Ca2 O2 . 8_6445 2.479(4) 2.309(4) 2.559(4) ? Ca2 O3 . . 2.228(2) 2.206(2) 2.249(2) ? Ca2 O3 . 7_5655 2.228(2) 2.206(2) 2.249(2) ? Si1 O1 . . 1.606(5) 1.579(5) 1.638(5) ? Si1 O1 . 7_5555 1.606(5) 1.579(5) 1.638(5) ? Si1 O2 . 3_6465 1.627(3) 1.613(3) 1.663(3) ? Si1 O2 . 5_6665 1.628(3) 1.613(3) 1.663(3) ? Si1 O3 . 2_5655 1.609(2) 1.590(3) 1.641(3) ? Si1 O3 . 8_5455 1.609(2) 1.590(3) 1.641(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_ssg_symmetry_1 _geom_angle_site_ssg_symmetry_2 _geom_angle_site_ssg_symmetry_3 _geom_angle_av _geom_angle_min _geom_angle_max _geom_angle_publ_flag Ca1 Ca1 Ca1 4_4655 . 4_5655 151.70(4) 151.24(4) 152.18(4) ? Ca1 Ca1 Ca2 4_4655 . . 145.96(4) 145.77(4) 146.15(4) ? Ca1 Ca1 Ca2 4_4655 . 2_6655 100.39(4) 97.05(4) 103.73(4) ? Ca1 Ca1 Ca2 4_4655 . 2_6755 100.40(4) 97.05(4) 103.73(4) ? Ca1 Ca1 Ca2 4_4655 . 3_6455 60.65(4) 58.48(4) 62.70(4) ? Ca1 Ca1 Ca2 4_4655 . 3_6555 60.66(4) 58.48(4) 62.70(4) ? Ca1 Ca1 Ca2 4_4655 . 4_4655 58.45(3) 58.40(3) 58.50(3) ? Ca1 Ca1 Si1 4_4655 . 2_5645 76.05(3) 75.91(3) 76.19(3) ? Ca1 Ca1 Si1 4_4655 . 4_5555 121.75(6) 117.02(6) 126.47(6) ? Ca1 Ca1 Si1 4_4655 . 4_5655 121.79(6) 117.02(6) 126.47(6) ? Ca1 Ca1 O1 4_4655 . . 44.82(10) 42.43(10) 48.02(10) ? Ca1 Ca1 O1 4_4655 . 4_5655 142.03(12) 128.52(11) 154.78(11) ? Ca1 Ca1 O1 4_4655 . 6_5555 141.85(12) 128.52(11) 154.78(11) ? Ca1 Ca1 O1 4_4655 . 7_5655 44.86(10) 42.43(10) 48.02(10) ? Ca1 Ca1 O3 4_4655 . . 106.16(6) 105.61(6) 107.06(6) ? Ca1 Ca1 O3 4_4655 . 7_5655 106.16(6) 105.61(6) 107.06(6) ? Ca1 Ca1 Ca2 4_5655 . . 61.69(3) 61.63(3) 61.75(3) ? Ca1 Ca1 Ca2 4_5655 . 2_6655 62.95(4) 59.38(4) 66.62(4) ? Ca1 Ca1 Ca2 4_5655 . 2_6755 63.02(4) 59.38(4) 66.62(4) ? Ca1 Ca1 Ca2 4_5655 . 3_6455 130.47(6) 124.97(6) 136.03(6) ? Ca1 Ca1 Ca2 4_5655 . 3_6555 130.56(6) 124.97(6) 136.03(6) ? Ca1 Ca1 Ca2 4_5655 . 4_4655 93.68(3) 93.59(3) 93.76(3) ? Ca1 Ca1 Si1 4_5655 . 2_5645 131.39(4) 131.07(4) 131.70(4) ? Ca1 Ca1 Si1 4_5655 . 4_5555 68.24(4) 65.30(4) 71.17(4) ? Ca1 Ca1 Si1 4_5655 . 4_5655 68.30(4) 65.30(4) 71.17(4) ? Ca1 Ca1 O1 4_5655 . . 119.23(11) 110.32(10) 128.31(11) ? Ca1 Ca1 O1 4_5655 . 4_5655 42.40(10) 41.51(10) 43.77(10) ? Ca1 Ca1 O1 4_5655 . 6_5555 42.42(10) 41.51(10) 43.77(10) ? Ca1 Ca1 O1 4_5655 . 7_5655 119.24(11) 110.32(10) 128.31(11) ? Ca1 Ca1 O3 4_5655 . . 100.37(6) 99.95(6) 101.12(6) ? Ca1 Ca1 O3 4_5655 . 7_5655 100.37(6) 99.95(6) 101.12(6) ? Ca2 Ca1 Ca2 . . 2_6655 101.62(4) 99.54(5) 103.72(4) ? Ca2 Ca1 Ca2 . . 2_6755 101.66(4) 99.54(5) 103.72(4) ? Ca2 Ca1 Ca2 . . 3_6455 98.48(4) 96.51(4) 100.45(4) ? Ca2 Ca1 Ca2 . . 3_6555 98.52(4) 96.51(4) 100.45(4) ? Ca2 Ca1 Ca2 . . 4_4655 155.36(3) 155.29(3) 155.42(3) ? Ca2 Ca1 Si1 . . 2_5645 69.97(3) 69.85(3) 70.09(3) ? Ca2 Ca1 Si1 . . 4_5555 56.54(5) 55.48(5) 57.58(5) ? Ca2 Ca1 Si1 . . 4_5655 56.56(5) 55.48(5) 57.58(5) ? Ca2 Ca1 O1 . . . 139.05(12) 133.66(12) 144.86(12) ? Ca2 Ca1 O1 . . 4_5655 53.00(10) 44.53(10) 62.08(10) ? Ca2 Ca1 O1 . . 6_5555 53.10(10) 44.53(10) 62.08(10) ? Ca2 Ca1 O1 . . 7_5655 139.15(12) 133.66(12) 144.86(12) ? Ca2 Ca1 O3 . . . 40.06(6) 39.45(6) 40.58(6) ? Ca2 Ca1 O3 . . 7_5655 40.06(6) 39.45(6) 40.58(6) ? Ca2 Ca1 Ca2 2_6655 . 2_6755 97.99(4) 97.99(4) 97.99(4) ? Ca2 Ca1 Ca2 2_6655 . 3_6455 79.87(5) 77.57(5) 82.30(5) ? Ca2 Ca1 Ca2 2_6655 . 3_6555 159.68(3) 158.88(4) 160.31(3) ? Ca2 Ca1 Ca2 2_6655 . 4_4655 63.69(4) 61.66(4) 65.72(4) ? Ca2 Ca1 Si1 2_6655 . 2_5645 130.96(8) 126.26(8) 135.68(8) ? Ca2 Ca1 Si1 2_6655 . 4_5555 53.93(4) 52.81(4) 55.12(4) ? Ca2 Ca1 Si1 2_6655 . 4_5655 131.03(4) 130.27(4) 131.74(4) ? Ca2 Ca1 O1 2_6655 . . 57.56(10) 49.65(10) 65.37(10) ? Ca2 Ca1 O1 2_6655 . 4_5655 104.71(10) 100.92(10) 108.58(10) ? Ca2 Ca1 O1 2_6655 . 6_5555 48.59(10) 38.78(10) 58.18(10) ? Ca2 Ca1 O1 2_6655 . 7_5655 114.46(11) 107.92(11) 120.84(11) ? Ca2 Ca1 O3 2_6655 . . 132.30(9) 129.63(9) 133.57(9) ? Ca2 Ca1 O3 2_6655 . 7_5655 114.42(9) 113.10(9) 117.21(10) ? Ca2 Ca1 Ca2 2_6755 . 3_6455 159.68(3) 158.88(4) 160.31(3) ? Ca2 Ca1 Ca2 2_6755 . 3_6555 79.88(5) 77.57(5) 82.30(5) ? Ca2 Ca1 Ca2 2_6755 . 4_4655 63.68(4) 61.66(4) 65.72(4) ? Ca2 Ca1 Si1 2_6755 . 2_5645 130.99(8) 126.26(8) 135.68(8) ? Ca2 Ca1 Si1 2_6755 . 4_5555 131.04(4) 130.27(4) 131.74(4) ? Ca2 Ca1 Si1 2_6755 . 4_5655 53.95(4) 52.81(4) 55.12(4) ? Ca2 Ca1 O1 2_6755 . . 114.54(11) 107.92(11) 120.84(11) ? Ca2 Ca1 O1 2_6755 . 4_5655 48.74(10) 38.78(10) 58.18(10) ? Ca2 Ca1 O1 2_6755 . 6_5555 104.78(10) 100.92(10) 108.58(10) ? Ca2 Ca1 O1 2_6755 . 7_5655 57.52(10) 49.65(10) 65.37(10) ? Ca2 Ca1 O3 2_6755 . . 114.43(9) 113.10(9) 117.21(10) ? Ca2 Ca1 O3 2_6755 . 7_5655 132.31(9) 129.63(9) 133.57(9) ? Ca2 Ca1 Ca2 3_6455 . 3_6555 95.14(4) 95.01(4) 95.27(4) ? Ca2 Ca1 Ca2 3_6455 . 4_4655 97.99(4) 95.89(4) 100.02(4) ? Ca2 Ca1 Si1 3_6455 . 2_5645 55.39(5) 52.99(5) 57.70(5) ? Ca2 Ca1 Si1 3_6455 . 4_5555 63.50(4) 60.95(4) 66.08(5) ? Ca2 Ca1 Si1 3_6455 . 4_5655 140.49(4) 138.88(4) 142.09(4) ? Ca2 Ca1 O1 3_6455 . . 47.37(11) 40.25(10) 54.78(11) ? Ca2 Ca1 O1 3_6455 . 4_5655 151.10(11) 141.55(10) 160.46(11) ? Ca2 Ca1 O1 3_6455 . 6_5555 88.80(11) 81.24(10) 96.11(10) ? Ca2 Ca1 O1 3_6455 . 7_5655 104.91(10) 99.80(10) 110.21(10) ? Ca2 Ca1 O3 3_6455 . . 79.63(7) 78.11(8) 80.46(7) ? Ca2 Ca1 O3 3_6455 . 7_5655 65.13(7) 64.24(7) 66.74(7) ? Ca2 Ca1 Ca2 3_6555 . 4_4655 97.98(4) 95.89(4) 100.02(4) ? Ca2 Ca1 Si1 3_6555 . 2_5645 55.41(5) 52.99(5) 57.70(5) ? Ca2 Ca1 Si1 3_6555 . 4_5555 140.49(4) 138.88(4) 142.09(4) ? Ca2 Ca1 Si1 3_6555 . 4_5655 63.53(4) 60.95(4) 66.08(5) ? Ca2 Ca1 O1 3_6555 . . 104.87(10) 99.80(10) 110.21(10) ? Ca2 Ca1 O1 3_6555 . 4_5655 88.92(11) 81.24(10) 96.11(10) ? Ca2 Ca1 O1 3_6555 . 6_5555 151.24(11) 141.55(10) 160.46(11) ? Ca2 Ca1 O1 3_6555 . 7_5655 47.46(11) 40.25(10) 54.78(11) ? Ca2 Ca1 O3 3_6555 . . 65.13(7) 64.24(7) 66.74(7) ? Ca2 Ca1 O3 3_6555 . 7_5655 79.65(7) 78.11(8) 80.46(7) ? Ca2 Ca1 Si1 4_4655 . 2_5645 134.44(4) 134.20(4) 134.67(4) ? Ca2 Ca1 Si1 4_4655 . 4_5555 116.72(6) 114.66(6) 118.72(6) ? Ca2 Ca1 Si1 4_4655 . 4_5655 116.73(6) 114.66(6) 118.72(6) ? Ca2 Ca1 O1 4_4655 . . 51.09(11) 42.40(11) 59.67(10) ? Ca2 Ca1 O1 4_4655 . 4_5655 109.26(11) 100.18(11) 117.59(10) ? Ca2 Ca1 O1 4_4655 . 6_5555 109.17(11) 100.18(11) 117.59(10) ? Ca2 Ca1 O1 4_4655 . 7_5655 51.00(11) 42.40(11) 59.67(10) ? Ca2 Ca1 O3 4_4655 . . 162.04(8) 160.60(8) 164.68(7) ? Ca2 Ca1 O3 4_4655 . 7_5655 162.05(8) 160.60(8) 164.68(7) ? Si1 Ca1 Si1 2_5645 . 4_5555 85.80(6) 81.89(6) 89.73(6) ? Si1 Ca1 Si1 2_5645 . 4_5655 85.82(6) 81.89(6) 89.73(6) ? Si1 Ca1 O1 2_5645 . . 96.85(11) 89.48(11) 104.58(11) ? Si1 Ca1 O1 2_5645 . 4_5655 105.90(11) 104.55(10) 106.78(12) ? Si1 Ca1 O1 2_5645 . 6_5555 105.91(11) 104.55(10) 106.78(12) ? Si1 Ca1 O1 2_5645 . 7_5655 96.95(11) 89.48(11) 104.58(11) ? Si1 Ca1 O3 2_5645 . . 31.40(6) 30.86(6) 32.12(6) ? Si1 Ca1 O3 2_5645 . 7_5655 31.40(6) 30.86(6) 32.12(6) ? Si1 Ca1 Si1 4_5555 . 4_5655 111.20(5) 111.13(5) 111.28(5) ? Si1 Ca1 O1 4_5555 . . 85.18(11) 81.51(11) 88.89(11) ? Si1 Ca1 O1 4_5555 . 4_5655 96.03(10) 87.56(10) 105.13(10) ? Si1 Ca1 O1 4_5555 . 6_5555 26.84(10) 23.47(10) 30.24(9) ? Si1 Ca1 O1 4_5555 . 7_5655 162.25(12) 159.42(12) 167.31(12) ? Si1 Ca1 O3 4_5555 . . 77.80(8) 74.94(8) 79.07(8) ? Si1 Ca1 O3 4_5555 . 7_5655 61.46(8) 60.25(8) 64.28(8) ? Si1 Ca1 O1 4_5655 . . 162.32(12) 159.42(12) 167.31(12) ? Si1 Ca1 O1 4_5655 . 4_5655 26.90(10) 23.47(10) 30.24(9) ? Si1 Ca1 O1 4_5655 . 6_5555 96.17(10) 87.56(10) 105.13(10) ? Si1 Ca1 O1 4_5655 . 7_5655 85.24(11) 81.51(11) 88.89(11) ? Si1 Ca1 O3 4_5655 . . 61.46(8) 60.25(8) 64.28(8) ? Si1 Ca1 O3 4_5655 . 7_5655 77.80(8) 74.94(8) 79.07(8) ? O1 Ca1 O1 . . 4_5655 155.20(14) 149.29(14) 164.00(14) ? O1 Ca1 O1 . . 6_5555 98.29(15) 84.53(14) 111.90(15) ? O1 Ca1 O1 . . 7_5655 79.40(14) 78.42(14) 80.38(14) ? O1 Ca1 O3 . . . 126.33(12) 116.84(12) 133.44(13) ? O1 Ca1 O3 . . 7_5655 111.77(13) 106.32(12) 120.92(14) ? O1 Ca1 O1 4_5655 . 6_5555 75.30(13) 74.51(13) 76.07(13) ? O1 Ca1 O1 4_5655 . 7_5655 98.45(15) 84.53(14) 111.90(14) ? O1 Ca1 O3 4_5655 . . 79.39(12) 75.58(11) 81.14(12) ? O1 Ca1 O3 4_5655 . 7_5655 83.60(11) 81.55(11) 88.45(12) ? O1 Ca1 O1 6_5555 . 7_5655 155.10(14) 149.29(15) 164.00(14) ? O1 Ca1 O3 6_5555 . . 83.60(11) 81.55(11) 88.45(12) ? O1 Ca1 O3 6_5555 . 7_5655 79.38(12) 75.58(11) 81.14(12) ? O1 Ca1 O3 7_5655 . . 111.86(13) 106.32(12) 120.92(14) ? O1 Ca1 O3 7_5655 . 7_5655 126.43(12) 116.84(12) 133.44(13) ? Ca1 Ca2 Ca1 . . 2_6645 129.90(6) 127.46(7) 132.28(6) ? Ca1 Ca2 Ca1 . . 2_6745 129.85(6) 127.46(7) 132.28(6) ? Ca1 Ca2 Ca1 . . 3_6455 81.48(4) 79.85(4) 83.02(4) ? Ca1 Ca2 Ca1 . . 3_6555 81.45(4) 79.85(4) 83.02(4) ? Ca1 Ca2 Ca1 . . 4_5655 59.86(3) 59.78(3) 59.94(3) ? Ca1 Ca2 Ca2 . . 3_7455 98.42(4) 96.59(4) 100.23(4) ? Ca1 Ca2 Ca2 . . 3_7555 98.39(4) 96.59(4) 100.23(4) ? Ca1 Ca2 Si1 . . 2_6645 135.08(4) 135.03(4) 135.13(4) ? Ca1 Ca2 Si1 . . 3_6555 131.41(4) 131.27(4) 131.56(4) ? Ca1 Ca2 Si1 . . 4_5555 60.20(5) 57.41(5) 62.93(5) ? Ca1 Ca2 Si1 . . 4_5655 60.14(5) 57.41(5) 62.93(5) ? Ca1 Ca2 O1 . . 3_6555 116.74(9) 111.63(8) 122.45(10) ? Ca1 Ca2 O1 . . 4_5655 45.11(8) 41.84(7) 48.88(9) ? Ca1 Ca2 O1 . . 5_6655 116.82(9) 111.63(8) 122.45(10) ? Ca1 Ca2 O1 . . 6_5555 45.08(8) 41.84(7) 48.88(9) ? Ca1 Ca2 O2 . . 2_6745 89.57(8) 86.74(8) 91.94(8) ? Ca1 Ca2 O2 . . 8_6445 89.61(8) 86.74(8) 91.94(8) ? Ca1 Ca2 O3 . . . 43.37(8) 42.78(8) 43.69(8) ? Ca1 Ca2 O3 . . 7_5655 43.37(8) 42.78(8) 43.69(8) ? Ca1 Ca2 Ca1 2_6645 . 2_6745 97.99(4) 97.99(4) 97.99(4) ? Ca1 Ca2 Ca1 2_6645 . 3_6455 56.37(3) 54.89(3) 57.94(4) ? Ca1 Ca2 Ca1 2_6645 . 3_6555 124.04(4) 122.29(4) 125.67(4) ? Ca1 Ca2 Ca1 2_6645 . 4_5655 116.30(5) 114.27(5) 118.35(5) ? Ca1 Ca2 Ca2 2_6645 . 3_7455 56.87(4) 55.75(3) 58.04(4) ? Ca1 Ca2 Ca2 2_6645 . 3_7555 123.18(3) 122.24(3) 124.09(3) ? Ca1 Ca2 Si1 2_6645 . 2_6645 69.17(5) 67.40(5) 70.96(5) ? Ca1 Ca2 Si1 2_6645 . 3_6555 58.03(5) 55.34(5) 60.69(5) ? Ca1 Ca2 Si1 2_6645 . 4_5555 71.90(5) 71.36(5) 72.46(5) ? Ca1 Ca2 Si1 2_6645 . 4_5655 169.83(6) 169.29(6) 170.37(6) ? Ca1 Ca2 O1 2_6645 . 3_6555 87.42(9) 83.96(10) 90.46(8) ? Ca1 Ca2 O1 2_6645 . 4_5655 157.01(10) 154.43(10) 158.98(9) ? Ca1 Ca2 O1 2_6645 . 5_6655 41.83(8) 39.34(10) 44.00(7) ? Ca1 Ca2 O1 2_6645 . 6_5555 96.50(10) 94.30(11) 98.37(9) ? Ca1 Ca2 O2 2_6645 . 2_6745 140.07(7) 139.95(8) 140.33(7) ? Ca1 Ca2 O2 2_6645 . 8_6445 42.21(7) 42.09(7) 42.47(7) ? Ca1 Ca2 O3 2_6645 . . 119.32(9) 115.62(9) 121.84(9) ? Ca1 Ca2 O3 2_6645 . 7_5655 105.07(9) 102.40(9) 108.92(10) ? Ca1 Ca2 Ca1 2_6745 . 3_6455 124.02(4) 122.29(4) 125.67(4) ? Ca1 Ca2 Ca1 2_6745 . 3_6555 56.35(3) 54.89(3) 57.94(4) ? Ca1 Ca2 Ca1 2_6745 . 4_5655 116.33(5) 114.27(5) 118.35(5) ? Ca1 Ca2 Ca2 2_6745 . 3_7455 123.19(3) 122.24(3) 124.09(3) ? Ca1 Ca2 Ca2 2_6745 . 3_7555 56.88(4) 55.75(3) 58.04(4) ? Ca1 Ca2 Si1 2_6745 . 2_6645 69.19(5) 67.40(5) 70.96(5) ? Ca1 Ca2 Si1 2_6745 . 3_6555 57.99(5) 55.34(5) 60.69(5) ? Ca1 Ca2 Si1 2_6745 . 4_5555 169.82(6) 169.29(6) 170.37(6) ? Ca1 Ca2 Si1 2_6745 . 4_5655 71.91(5) 71.36(5) 72.46(5) ? Ca1 Ca2 O1 2_6745 . 3_6555 41.84(8) 39.34(10) 44.00(7) ? Ca1 Ca2 O1 2_6745 . 4_5655 96.47(10) 94.30(11) 98.37(9) ? Ca1 Ca2 O1 2_6745 . 5_6655 87.36(9) 83.96(10) 90.46(8) ? Ca1 Ca2 O1 2_6745 . 6_5555 157.05(10) 154.43(10) 158.98(9) ? Ca1 Ca2 O2 2_6745 . 2_6745 42.21(7) 42.09(7) 42.47(7) ? Ca1 Ca2 O2 2_6745 . 8_6445 140.07(7) 139.95(8) 140.33(7) ? Ca1 Ca2 O3 2_6745 . . 105.05(9) 102.40(9) 108.92(10) ? Ca1 Ca2 O3 2_6745 . 7_5655 119.29(9) 115.62(9) 121.84(9) ? Ca1 Ca2 Ca1 3_6455 . 3_6555 95.14(4) 95.01(4) 95.27(3) ? Ca1 Ca2 Ca1 3_6455 . 4_5655 119.63(5) 117.36(5) 121.82(5) ? Ca1 Ca2 Ca2 3_6455 . 3_7455 85.99(5) 83.09(5) 88.88(5) ? Ca1 Ca2 Ca2 3_6455 . 3_7555 177.99(5) 176.02(5) 179.71(4) ? Ca1 Ca2 Si1 3_6455 . 2_6645 124.70(7) 121.96(7) 127.39(7) ? Ca1 Ca2 Si1 3_6455 . 3_6555 66.76(5) 65.57(5) 67.85(5) ? Ca1 Ca2 Si1 3_6455 . 4_5555 51.55(4) 49.61(4) 53.57(4) ? Ca1 Ca2 Si1 3_6455 . 4_5655 130.08(4) 128.10(4) 131.99(4) ? Ca1 Ca2 O1 3_6455 . 3_6555 84.62(9) 81.67(8) 87.64(10) ? Ca1 Ca2 O1 3_6455 . 4_5655 126.53(9) 122.38(8) 131.25(10) ? Ca1 Ca2 O1 3_6455 . 5_6655 39.09(9) 36.24(8) 42.56(10) ? Ca1 Ca2 O1 3_6455 . 6_5555 78.67(9) 76.33(8) 81.29(10) ? Ca1 Ca2 O2 3_6455 . 2_6745 139.66(7) 137.36(7) 142.72(7) ? Ca1 Ca2 O2 3_6455 . 8_6445 44.60(6) 42.38(6) 47.72(7) ? Ca1 Ca2 O3 3_6455 . . 64.66(8) 61.88(9) 65.98(8) ? Ca1 Ca2 O3 3_6455 . 7_5655 48.45(8) 47.14(8) 51.12(8) ? Ca1 Ca2 Ca1 3_6555 . 4_5655 119.63(5) 117.36(5) 121.82(5) ? Ca1 Ca2 Ca2 3_6555 . 3_7455 177.97(5) 176.02(5) 179.71(4) ? Ca1 Ca2 Ca2 3_6555 . 3_7555 85.97(5) 83.09(5) 88.88(5) ? Ca1 Ca2 Si1 3_6555 . 2_6645 124.70(7) 121.96(7) 127.39(7) ? Ca1 Ca2 Si1 3_6555 . 3_6555 66.73(5) 65.57(5) 67.85(5) ? Ca1 Ca2 Si1 3_6555 . 4_5555 130.11(4) 128.10(4) 131.99(4) ? Ca1 Ca2 Si1 3_6555 . 4_5655 51.52(4) 49.61(4) 53.57(4) ? Ca1 Ca2 O1 3_6555 . 3_6555 39.04(9) 36.24(8) 42.56(10) ? Ca1 Ca2 O1 3_6555 . 4_5655 78.69(9) 76.33(8) 81.29(10) ? Ca1 Ca2 O1 3_6555 . 5_6655 84.65(9) 81.67(8) 87.64(10) ? Ca1 Ca2 O1 3_6555 . 6_5555 126.46(9) 122.38(8) 131.25(10) ? Ca1 Ca2 O2 3_6555 . 2_6745 44.55(6) 42.38(6) 47.72(7) ? Ca1 Ca2 O2 3_6555 . 8_6445 139.71(7) 137.36(7) 142.72(7) ? Ca1 Ca2 O3 3_6555 . . 48.44(8) 47.14(8) 51.12(8) ? Ca1 Ca2 O3 3_6555 . 7_5655 64.66(8) 61.88(9) 65.98(8) ? Ca1 Ca2 Ca2 4_5655 . 3_7455 59.43(4) 58.52(4) 60.31(4) ? Ca1 Ca2 Ca2 4_5655 . 3_7555 59.44(4) 58.52(4) 60.31(4) ? Ca1 Ca2 Si1 4_5655 . 2_6645 75.27(3) 75.24(4) 75.31(3) ? Ca1 Ca2 Si1 4_5655 . 3_6555 168.49(4) 168.32(4) 168.66(4) ? Ca1 Ca2 Si1 4_5655 . 4_5555 68.80(5) 66.94(5) 70.70(5) ? Ca1 Ca2 Si1 4_5655 . 4_5655 68.83(5) 66.94(5) 70.70(5) ? Ca1 Ca2 O1 4_5655 . 3_6555 152.21(11) 150.68(10) 153.59(12) ? Ca1 Ca2 O1 4_5655 . 4_5655 41.18(9) 40.50(10) 41.93(8) ? Ca1 Ca2 O1 4_5655 . 5_6655 152.21(11) 150.68(10) 153.59(12) ? Ca1 Ca2 O1 4_5655 . 6_5555 41.19(9) 40.50(10) 41.93(8) ? Ca1 Ca2 O2 4_5655 . 2_6745 86.02(8) 85.00(8) 88.33(8) ? Ca1 Ca2 O2 4_5655 . 8_6445 86.00(8) 85.00(8) 88.33(8) ? Ca1 Ca2 O3 4_5655 . . 101.77(8) 101.53(8) 102.16(8) ? Ca1 Ca2 O3 4_5655 . 7_5655 101.77(8) 101.53(8) 102.16(8) ? Ca2 Ca2 Ca2 3_7455 . 3_7555 92.91(4) 92.86(4) 92.96(4) ? Ca2 Ca2 Si1 3_7455 . 2_6645 54.63(5) 53.80(5) 55.42(5) ? Ca2 Ca2 Si1 3_7455 . 3_6555 114.03(6) 111.88(6) 116.10(6) ? Ca2 Ca2 Si1 3_7455 . 4_5555 50.52(4) 49.15(4) 51.95(4) ? Ca2 Ca2 Si1 3_7455 . 4_5655 127.44(4) 126.31(4) 128.50(4) ? Ca2 Ca2 O1 3_7455 . 3_6555 141.62(9) 137.44(11) 145.13(8) ? Ca2 Ca2 O1 3_7455 . 4_5655 100.44(9) 98.88(10) 101.78(8) ? Ca2 Ca2 O1 3_7455 . 5_6655 96.36(10) 95.49(11) 97.19(9) ? Ca2 Ca2 O1 3_7455 . 6_5555 53.43(8) 48.77(9) 57.44(8) ? Ca2 Ca2 O2 3_7455 . 2_6745 132.93(7) 132.21(7) 134.54(7) ? Ca2 Ca2 O2 3_7455 . 8_6445 40.04(6) 39.38(6) 41.63(6) ? Ca2 Ca2 O3 3_7455 . . 132.29(10) 127.47(10) 135.01(9) ? Ca2 Ca2 O3 3_7455 . 7_5655 115.69(10) 112.73(10) 120.81(10) ? Ca2 Ca2 Si1 3_7555 . 2_6645 54.64(5) 53.80(5) 55.42(5) ? Ca2 Ca2 Si1 3_7555 . 3_6555 114.00(6) 111.88(6) 116.10(6) ? Ca2 Ca2 Si1 3_7555 . 4_5555 127.43(4) 126.31(4) 128.50(4) ? Ca2 Ca2 Si1 3_7555 . 4_5655 50.54(4) 49.15(4) 51.95(4) ? Ca2 Ca2 O1 3_7555 . 3_6555 96.38(10) 95.49(11) 97.19(9) ? Ca2 Ca2 O1 3_7555 . 4_5655 53.35(8) 48.77(9) 57.44(8) ? Ca2 Ca2 O1 3_7555 . 5_6655 141.57(9) 137.44(11) 145.13(8) ? Ca2 Ca2 O1 3_7555 . 6_5555 100.46(9) 98.88(10) 101.78(8) ? Ca2 Ca2 O2 3_7555 . 2_6745 40.05(6) 39.38(6) 41.63(6) ? Ca2 Ca2 O2 3_7555 . 8_6445 132.92(7) 132.21(7) 134.54(7) ? Ca2 Ca2 O3 3_7555 . . 115.66(10) 112.73(10) 120.81(10) ? Ca2 Ca2 O3 3_7555 . 7_5655 132.27(10) 127.47(10) 135.01(9) ? Si1 Ca2 Si1 2_6645 . 3_6555 93.36(4) 93.30(4) 93.41(4) ? Si1 Ca2 Si1 2_6645 . 4_5555 105.15(7) 102.95(7) 107.37(7) ? Si1 Ca2 Si1 2_6645 . 4_5655 105.18(7) 102.95(7) 107.37(7) ? Si1 Ca2 O1 2_6645 . 3_6555 102.67(9) 98.58(10) 106.26(8) ? Si1 Ca2 O1 2_6645 . 4_5655 100.03(9) 95.94(10) 103.64(8) ? Si1 Ca2 O1 2_6645 . 5_6655 102.61(9) 98.58(10) 106.26(8) ? Si1 Ca2 O1 2_6645 . 6_5555 100.10(9) 95.94(10) 103.64(8) ? Si1 Ca2 O2 2_6645 . 2_6745 87.16(8) 86.23(8) 89.28(8) ? Si1 Ca2 O2 2_6645 . 8_6445 87.15(8) 86.23(8) 89.28(8) ? Si1 Ca2 O3 2_6645 . . 169.54(12) 166.21(12) 175.67(12) ? Si1 Ca2 O3 2_6645 . 7_5655 169.57(12) 166.21(12) 175.67(12) ? Si1 Ca2 Si1 3_6555 . 4_5555 115.24(7) 112.56(8) 117.87(8) ? Si1 Ca2 Si1 3_6555 . 4_5655 115.20(7) 112.56(8) 117.87(8) ? Si1 Ca2 O1 3_6555 . 3_6555 29.72(10) 29.47(11) 29.94(9) ? Si1 Ca2 O1 3_6555 . 4_5655 144.31(12) 142.00(12) 146.86(12) ? Si1 Ca2 O1 3_6555 . 5_6655 29.72(10) 29.47(11) 29.94(9) ? Si1 Ca2 O1 3_6555 . 6_5555 144.34(12) 142.00(12) 146.86(12) ? Si1 Ca2 O2 3_6555 . 2_6745 92.44(9) 89.61(9) 95.52(9) ? Si1 Ca2 O2 3_6555 . 8_6445 92.49(9) 89.61(9) 95.52(9) ? Si1 Ca2 O3 3_6555 . . 89.27(8) 88.73(8) 89.50(8) ? Si1 Ca2 O3 3_6555 . 7_5655 89.28(8) 88.73(8) 89.50(8) ? Si1 Ca2 Si1 4_5555 . 4_5655 118.17(5) 118.17(5) 118.18(5) ? Si1 Ca2 O1 4_5555 . 3_6555 136.01(10) 134.63(9) 137.62(11) ? Si1 Ca2 O1 4_5555 . 4_5655 92.82(10) 90.69(9) 95.12(11) ? Si1 Ca2 O1 4_5555 . 5_6655 85.68(10) 83.10(9) 88.57(12) ? Si1 Ca2 O1 4_5555 . 6_5555 29.67(9) 29.29(9) 30.32(10) ? Si1 Ca2 O2 4_5555 . 2_6745 147.46(8) 147.33(8) 147.77(8) ? Si1 Ca2 O2 4_5555 . 8_6445 29.47(7) 29.34(7) 29.78(7) ? Si1 Ca2 O3 4_5555 . . 81.37(9) 77.39(9) 84.32(9) ? Si1 Ca2 O3 4_5555 . 7_5655 66.09(9) 63.17(9) 70.01(9) ? Si1 Ca2 O1 4_5655 . 3_6555 85.64(10) 83.10(9) 88.57(12) ? Si1 Ca2 O1 4_5655 . 4_5655 29.67(9) 29.29(9) 30.32(10) ? Si1 Ca2 O1 4_5655 . 5_6655 136.01(10) 134.63(9) 137.62(11) ? Si1 Ca2 O1 4_5655 . 6_5555 92.78(10) 90.69(9) 95.12(11) ? Si1 Ca2 O2 4_5655 . 2_6745 29.47(7) 29.34(7) 29.78(7) ? Si1 Ca2 O2 4_5655 . 8_6445 147.46(8) 147.33(8) 147.77(8) ? Si1 Ca2 O3 4_5655 . . 66.06(9) 63.17(9) 70.01(9) ? Si1 Ca2 O3 4_5655 . 7_5655 81.35(9) 77.39(9) 84.32(9) ? O1 Ca2 O1 3_6555 . 4_5655 114.87(14) 112.29(12) 117.91(15) ? O1 Ca2 O1 3_6555 . 5_6655 55.57(13) 55.41(12) 55.72(13) ? O1 Ca2 O1 3_6555 . 6_5555 156.64(11) 150.69(10) 162.08(12) ? O1 Ca2 O2 3_6555 . 2_6745 65.46(11) 63.68(11) 66.96(13) ? O1 Ca2 O2 3_6555 . 8_6445 120.67(12) 118.50(13) 122.13(12) ? O1 Ca2 O3 3_6555 . . 75.89(11) 70.46(10) 82.01(12) ? O1 Ca2 O3 3_6555 . 7_5655 83.63(11) 77.99(10) 89.21(11) ? O1 Ca2 O1 4_5655 . 5_6655 156.76(11) 150.69(10) 162.08(12) ? O1 Ca2 O1 4_5655 . 6_5555 65.16(12) 64.68(12) 65.64(13) ? O1 Ca2 O2 4_5655 . 2_6745 56.24(11) 54.81(11) 56.89(10) ? O1 Ca2 O2 4_5655 . 8_6445 120.68(12) 119.63(11) 121.13(13) ? O1 Ca2 O3 4_5655 . . 70.04(10) 67.89(10) 75.34(11) ? O1 Ca2 O3 4_5655 . 7_5655 85.90(11) 79.78(11) 88.78(11) ? O1 Ca2 O1 5_6655 . 6_5555 114.90(14) 112.29(12) 117.91(15) ? O1 Ca2 O2 5_6655 . 2_6745 120.64(12) 118.50(13) 122.13(12) ? O1 Ca2 O2 5_6655 . 8_6445 65.49(11) 63.68(11) 66.96(13) ? O1 Ca2 O3 5_6655 . . 83.68(11) 77.99(10) 89.21(11) ? O1 Ca2 O3 5_6655 . 7_5655 75.94(11) 70.46(10) 82.01(12) ? O1 Ca2 O2 6_5555 . 2_6745 120.67(12) 119.63(11) 121.13(13) ? O1 Ca2 O2 6_5555 . 8_6445 56.25(11) 54.81(11) 56.89(10) ? O1 Ca2 O3 6_5555 . . 85.90(11) 79.78(11) 88.78(11) ? O1 Ca2 O3 6_5555 . 7_5655 70.04(10) 67.89(10) 75.34(11) ? O2 Ca2 O3 2_6745 . . 81.68(11) 79.37(10) 85.87(11) ? O2 Ca2 O3 2_6745 . 7_5655 95.98(11) 95.38(11) 96.74(11) ? O2 Ca2 O3 8_6445 . . 95.98(11) 95.38(11) 96.74(11) ? O2 Ca2 O3 8_6445 . 7_5655 81.75(11) 79.37(10) 85.87(11) ? Ca1 Si1 Ca1 2_5655 . 4_4555 94.11(6) 89.99(6) 98.23(6) ? Ca1 Si1 Ca1 2_5655 . 4_4655 94.18(6) 89.99(6) 98.23(6) ? Ca1 Si1 Ca2 2_5655 . 2_6655 114.81(5) 114.71(5) 114.90(5) ? Ca1 Si1 Ca2 2_5655 . 3_6455 145.64(5) 145.25(5) 146.02(4) ? Ca1 Si1 Ca2 2_5655 . 4_4555 73.03(5) 68.80(5) 77.34(6) ? Ca1 Si1 Ca2 2_5655 . 4_4655 73.10(5) 68.80(5) 77.34(6) ? Ca1 Si1 O1 2_5655 . . 125.38(19) 117.17(18) 134.07(19) ? Ca1 Si1 O1 2_5655 . 7_5555 125.22(19) 117.17(18) 134.07(19) ? Ca1 Si1 O2 2_5655 . 3_6465 59.90(10) 59.24(9) 60.70(10) ? Ca1 Si1 O2 2_5655 . 5_6665 59.90(10) 59.24(9) 60.70(10) ? Ca1 Si1 O3 2_5655 . 2_5655 50.32(11) 49.80(10) 50.65(11) ? Ca1 Si1 O3 2_5655 . 8_5455 50.31(11) 49.80(10) 50.65(11) ? Ca1 Si1 Ca1 4_4555 . 4_4655 111.21(4) 111.13(4) 111.28(5) ? Ca1 Si1 Ca2 4_4555 . 2_6655 118.53(8) 116.97(8) 120.05(8) ? Ca1 Si1 Ca2 4_4555 . 3_6455 68.05(5) 66.48(5) 69.55(5) ? Ca1 Si1 Ca2 4_4555 . 4_4555 63.27(6) 61.45(6) 65.18(6) ? Ca1 Si1 Ca2 4_4555 . 4_4655 165.02(5) 164.23(5) 165.67(5) ? Ca1 Si1 O1 4_4555 . . 127.16(16) 112.61(16) 141.61(16) ? Ca1 Si1 O1 4_4555 . 7_5555 44.18(14) 36.77(14) 52.79(14) ? Ca1 Si1 O2 4_4555 . 3_6465 131.75(16) 127.96(16) 138.09(15) ? Ca1 Si1 O2 4_4555 . 5_6665 110.58(15) 104.14(15) 114.57(16) ? Ca1 Si1 O3 4_4555 . 2_5655 58.42(13) 54.56(12) 62.24(13) ? Ca1 Si1 O3 4_4555 . 8_5455 77.77(13) 73.85(13) 81.70(12) ? Ca1 Si1 Ca2 4_4655 . 2_6655 118.55(8) 116.97(8) 120.05(8) ? Ca1 Si1 Ca2 4_4655 . 3_6455 68.06(5) 66.48(5) 69.55(5) ? Ca1 Si1 Ca2 4_4655 . 4_4555 165.01(5) 164.23(5) 165.67(5) ? Ca1 Si1 Ca2 4_4655 . 4_4655 63.29(6) 61.45(6) 65.18(6) ? Ca1 Si1 O1 4_4655 . . 44.17(14) 36.77(14) 52.79(14) ? Ca1 Si1 O1 4_4655 . 7_5555 127.28(16) 112.61(16) 141.61(16) ? Ca1 Si1 O2 4_4655 . 3_6465 110.65(15) 104.14(15) 114.57(16) ? Ca1 Si1 O2 4_4655 . 5_6665 131.82(16) 127.96(16) 138.09(15) ? Ca1 Si1 O3 4_4655 . 2_5655 77.84(13) 73.85(13) 81.70(12) ? Ca1 Si1 O3 4_4655 . 8_5455 58.49(13) 54.56(12) 62.24(13) ? Ca2 Si1 Ca2 2_6655 . 3_6455 99.19(4) 99.14(4) 99.24(4) ? Ca2 Si1 Ca2 2_6655 . 4_4555 74.83(5) 72.64(5) 77.04(5) ? Ca2 Si1 Ca2 2_6655 . 4_4655 74.84(5) 72.64(5) 77.04(5) ? Ca2 Si1 O1 2_6655 . . 77.47(14) 64.81(14) 90.05(14) ? Ca2 Si1 O1 2_6655 . 7_5555 77.40(14) 64.81(14) 90.05(14) ? Ca2 Si1 O2 2_6655 . 3_6465 56.56(9) 55.82(9) 57.41(9) ? Ca2 Si1 O2 2_6655 . 5_6665 56.57(9) 55.82(9) 57.41(9) ? Ca2 Si1 O3 2_6655 . 2_5655 159.92(14) 156.82(15) 163.08(13) ? Ca2 Si1 O3 2_6655 . 8_5455 159.98(14) 156.82(15) 163.08(13) ? Ca2 Si1 Ca2 3_6455 . 4_4555 118.55(8) 115.56(8) 121.56(9) ? Ca2 Si1 Ca2 3_6455 . 4_4655 118.57(8) 115.56(8) 121.56(9) ? Ca2 Si1 O1 3_6455 . . 59.77(16) 45.10(16) 74.68(16) ? Ca2 Si1 O1 3_6455 . 7_5555 59.88(16) 45.10(16) 74.68(16) ? Ca2 Si1 O2 3_6455 . 3_6465 152.09(12) 148.70(13) 154.05(11) ? Ca2 Si1 O2 3_6455 . 5_6665 152.06(12) 148.70(13) 154.05(11) ? Ca2 Si1 O3 3_6455 . 2_5655 97.16(11) 96.60(11) 97.37(11) ? Ca2 Si1 O3 3_6455 . 8_5455 97.16(11) 96.60(11) 97.37(11) ? Ca2 Si1 Ca2 4_4555 . 4_4655 118.17(5) 118.17(5) 118.18(5) ? Ca2 Si1 O1 4_4555 . . 150.30(15) 141.75(14) 157.55(15) ? Ca2 Si1 O1 4_4555 . 7_5555 59.44(17) 48.03(16) 71.31(17) ? Ca2 Si1 O2 4_4555 . 3_6465 69.57(13) 66.88(13) 75.19(13) ? Ca2 Si1 O2 4_4555 . 5_6665 48.70(13) 43.15(12) 51.45(13) ? Ca2 Si1 O3 4_4555 . 2_5655 88.54(14) 83.94(13) 92.08(14) ? Ca2 Si1 O3 4_4555 . 8_5455 106.10(14) 102.63(14) 110.72(14) ? Ca2 Si1 O1 4_4655 . . 59.57(17) 48.03(16) 71.31(17) ? Ca2 Si1 O1 4_4655 . 7_5555 150.28(15) 141.75(14) 157.55(15) ? Ca2 Si1 O2 4_4655 . 3_6465 48.76(13) 43.15(12) 51.45(13) ? Ca2 Si1 O2 4_4655 . 5_6665 69.63(13) 66.88(13) 75.19(13) ? Ca2 Si1 O3 4_4655 . 2_5655 106.17(14) 102.63(14) 110.72(14) ? Ca2 Si1 O3 4_4655 . 8_5455 88.61(14) 83.94(13) 92.08(14) ? O1 Si1 O1 . . 7_5555 109.2(2) 108.1(2) 110.3(2) ? O1 Si1 O2 . . 3_6465 108.6(2) 97.0(2) 114.7(2) ? O1 Si1 O2 . . 5_6665 109.21(19) 103.27(19) 121.4(2) ? O1 Si1 O3 . . 2_5655 113.86(19) 110.62(19) 119.91(18) ? O1 Si1 O3 . . 8_5455 106.2(2) 99.0(2) 109.7(2) ? O1 Si1 O2 7_5555 . 3_6465 109.21(19) 103.27(19) 121.4(2) ? O1 Si1 O2 7_5555 . 5_6665 108.6(2) 97.0(2) 114.7(2) ? O1 Si1 O3 7_5555 . 2_5655 106.2(2) 99.0(2) 109.7(2) ? O1 Si1 O3 7_5555 . 8_5455 113.94(19) 110.62(19) 119.91(18) ? O2 Si1 O3 3_6465 . 2_5655 109.91(15) 109.59(15) 110.08(15) ? O2 Si1 O3 3_6465 . 8_5455 107.07(15) 106.78(15) 107.17(15) ? O2 Si1 O3 5_6665 . 2_5655 107.06(15) 106.78(15) 107.17(15) ? O2 Si1 O3 5_6665 . 8_5455 109.91(15) 109.59(15) 110.08(15) ? Ca1 O1 Ca1 . . 4_4655 92.77(15) 90.18(14) 94.72(15) ? Ca1 O1 Ca2 . . 3_6455 93.57(14) 88.02(12) 99.11(14) ? Ca1 O1 Ca2 . . 4_4655 87.72(13) 78.52(11) 97.09(16) ? Ca1 O1 Si1 . . . 151.8(2) 135.7(2) 165.7(2) ? Ca1 O1 Ca2 4_4655 . 3_6455 89.54(12) 77.83(10) 101.84(14) ? Ca1 O1 Ca2 4_4655 . 4_4655 81.83(12) 76.02(11) 86.63(13) ? Ca1 O1 Si1 4_4655 . . 108.96(18) 96.97(16) 119.6(2) ? Ca2 O1 Ca2 3_6455 . 4_4655 170.43(16) 163.23(14) 176.13(18) ? Ca2 O1 Si1 3_6455 . . 90.51(18) 75.46(15) 105.4(2) ? Ca2 O1 Si1 4_4655 . . 90.76(18) 79.23(16) 101.72(18) ? Ca2 O2 Si1 2_6755 . 3_6565 101.78(16) 98.99(16) 107.34(16) ? Ca1 O3 Ca2 . . . 96.57(10) 95.87(10) 97.77(10) ? Ca1 O3 Si1 . . 2_5645 98.29(13) 97.68(13) 99.26(13) ? Ca2 O3 Si1 . . 2_5645 153.47(19) 152.99(19) 154.15(19) ? #======================================================================= # 11. STRUCTURE-FACTOR LIST loop_ _reflns_scale_group_code _reflns_scale_meas_intensity 1 1651.776 2 1833.813 3 1816.246 4 1807.815 5 1843.636 6 1781.734 7 1463.507 8 1559.401 9 1888.312 10 2114.812 11 1833.786 12 2134.342 13 1529.731 14 1913.313 15 1840.094 16 2232.380 17 2447.929 18 2403.092 19 2274.559 20 2440.015 21 2443.558 22 2431.555 23 2421.281 24 2434.466 25 2583.624 26 2588.034 27 2645.633 28 2500.499 29 2460.698 30 2378.010 31 2535.155 32 2687.140 33 2491.165 34 2498.590 35 2709.748 36 2599.946 37 2782.911 38 2707.786 39 2613.713 40 2689.598 41 2672.220 42 2704.431 43 2897.679 44 2927.739 45 2992.746 46 2955.105 47 2671.620 48 2749.739 49 2891.949 50 2759.412 53 2595.964 54 2566.094 55 2727.311 56 2754.604 57 2788.100 58 2850.892 59 2957.136 60 2748.148 61 2901.210 62 2813.815 63 2703.875 64 2702.659 65 2696.135 66 2638.767 67 2720.913 68 2788.854 69 2740.292 70 2623.969 71 2548.027 72 2459.221 73 2484.484 74 2433.313 75 2478.958 76 2602.389 77 2565.495 78 2502.925 79 2578.182 80 2438.276 81 2475.874 82 2406.860 83 2433.852 84 2219.281 85 2066.016 86 2029.081 87 2115.372 88 1986.562 89 1857.882 90 1808.228 91 1713.704 92 1473.552 93 1501.986 94 1399.324 95 1350.996 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_index_m_1 _refln_intensity_calc _refln_intensity_meas _refln_intensity_sigma _refln_scale_group_code _refln_include_status 2 1 -8 -1 287.36 294.60 162.70 1 < 7 3 -8 -1 114.28 395.70 142.80 1 < -3 -1 -7 -1 261.26 19.80 152.30 1 < 2 1 -7 -1 1352.60 2257.30 244.10 1 o 7 3 -7 -1 36.38 130.10 149.60 1 < -3 -1 -6 -1 390.25 302.60 158.30 1 < 5 2 -4 -1 36.79 508.80 169.80 1 < 5 2 -3 -1 665.62 645.60 201.70 1 o -5 -2 -2 -1 60.99 3.40 165.60 1 < -5 -2 -1 -1 311.38 129.20 147.60 1 < 3 1 1 -1 15334.00 13636.60 531.40 1 o 8 3 1 -1 78.08 204.50 150.50 1 < -2 -1 2 -1 6119.30 5563.20 352.40 1 o -7 -3 4 -1 10.36 39.50 113.70 1 < -7 -3 5 -1 45.18 80.70 114.70 1 < 6 2 5 -1 134.49 66.80 171.80 1 < -7 -3 6 -1 151.25 47.10 116.00 1 < 6 2 6 -1 195.24 147.70 154.70 1 < 6 2 7 -1 16.84 141.40 140.70 1 < -4 -2 8 -1 108.54 -66.90 123.60 1 < 6 2 8 -1 13.45 163.10 165.80 1 < -4 -2 9 -1 157.64 -144.00 133.20 1 < -4 -2 10 -1 92.72 198.90 128.10 1 < 4 1 11 -1 6.43 36.90 132.20 1 < 4 1 12 -1 32.83 -7.20 129.90 1 < -4 -1 -11 0 705.60 592.20 150.60 1 o -4 -1 -10 0 17.45 -94.40 124.80 1 < -1 0 -9 0 3680.20 3522.50 268.90 1 o 4 2 -9 0 2116.10 1850.10 222.70 1 o -1 0 -8 0 154.83 567.90 166.60 1 o 4 2 -8 0 181.33 92.90 150.60 1 < -6 -2 -7 0 295.71 213.10 136.10 1 < -6 -2 -6 0 604.00 653.70 159.80 1 o -6 -2 -5 0 438.26 202.90 138.30 1 < 2 1 -5 0 1649.30 2410.20 271.20 1 o 7 3 -5 0 1441.10 1898.40 220.30 1 o -3 -1 -4 0 51388.00 52587.60 912.20 1 o 7 3 -4 0 94.17 -76.30 131.40 1 < -3 -1 -3 0 227.14 312.90 208.10 1 < 5 2 -1 0 5661.10 5646.30 337.10 1 o -5 -2 2 0 4353.20 4103.20 290.80 1 o -5 -2 3 0 8523.00 7409.80 361.50 1 o 3 1 4 0 52744.00 62182.30 1000.80 1 o 3 1 5 0 6391.40 5242.70 358.80 1 o -2 -1 6 0 9300.40 8326.00 374.90 1 o 3 1 6 0 2986.10 3583.80 283.30 1 o -2 -1 7 0 880.67 1404.80 200.50 1 o 1 0 10 0 223.46 800.90 181.60 1 o 1 0 11 0 161.17 252.00 150.90 1 < 1 1 -10 1 29.58 169.20 127.00 1 < -4 -1 -9 1 31.94 124.70 136.70 1 < 1 1 -9 1 442.77 810.00 183.60 1 o -4 -1 -8 1 142.93 -41.90 140.80 1 < 6 3 -8 1 135.94 110.20 126.40 1 < 4 2 -6 1 279.05 185.90 163.60 1 < 4 2 -5 1 785.19 498.10 190.10 1 < -6 -2 -4 1 548.62 640.70 171.60 1 o -6 -2 -3 1 1220.30 355.50 160.60 1 < 2 1 -2 1 6976.40 5863.30 382.40 1 o 7 3 -2 1 18.43 -281.10 147.60 1 < 7 3 -1 1 368.96 554.80 153.10 1 o -3 -1 0 1 4030.80 2893.70 289.80 1 o 7 3 0 1 312.25 -3.10 147.10 1 < 5 2 3 1 36.55 208.30 171.60 1 < 5 2 4 1 39.28 -208.90 161.90 1 < -5 -2 5 1 500.79 100.70 163.90 1 < 5 2 5 1 19.87 50.50 161.40 1 < -5 -2 6 1 191.04 10.10 145.10 1 < -5 -2 7 1 124.30 61.30 123.70 1 < -5 -2 8 1 117.17 174.90 129.60 1 < 3 1 8 1 17.68 92.20 157.80 1 < 3 1 9 1 71.28 208.10 149.10 1 < -2 -1 10 1 37.14 1.60 141.50 1 < 3 1 10 1 16.60 -1.70 131.00 1 < -2 -1 11 1 26.04 145.70 125.40 1 < 3 1 11 1 15.04 -241.90 137.00 1 < 3 1 12 1 2.58 122.40 135.10 1 < -4 -1 -11 -1 2.88 73.10 125.70 2 < 7 3 -8 -1 160.02 311.90 141.80 2 < -6 -2 -7 -1 14.67 20.70 122.30 2 < 2 1 -7 -1 1520.80 2334.40 238.80 2 o 7 3 -7 -1 36.39 -19.40 134.60 2 < -3 -1 -6 -1 381.69 200.90 154.70 2 < -3 -1 -5 -1 470.51 574.40 166.90 2 o 5 2 -4 -1 35.38 490.00 167.40 2 < 5 2 -3 -1 961.85 715.80 209.50 2 o -5 -2 -1 -1 382.31 314.10 162.10 2 < 8 3 -1 -1 89.81 19.40 147.10 2 < -5 -2 0 -1 601.65 586.80 171.90 2 o 3 1 0 -1 4834.60 4180.30 362.60 2 o -2 -1 2 -1 8832.20 6457.80 375.00 2 o 6 2 4 -1 517.10 535.30 199.60 2 < -7 -3 5 -1 141.47 29.30 109.70 2 < 6 2 5 -1 251.19 497.00 181.90 2 < -7 -3 6 -1 95.10 46.90 121.60 2 < -4 -2 7 -1 57.01 -33.00 132.70 2 < -4 -2 8 -1 92.12 22.10 128.80 2 < -4 -2 9 -1 127.12 62.10 150.60 2 < 4 1 9 -1 23.02 291.50 144.60 2 < -1 -1 10 -1 25.86 -10.70 134.80 2 < 4 1 10 -1 53.59 -39.80 129.10 2 < 4 1 11 -1 8.32 -190.30 137.40 2 < -4 -1 -10 0 12.00 1.30 118.80 2 < 1 1 -10 0 26.08 15.30 131.10 2 < -4 -1 -9 0 1085.00 852.00 177.60 2 o 4 2 -9 0 3628.40 3667.40 276.10 2 o 4 2 -8 0 138.83 112.10 150.40 2 < -1 0 -7 0 8914.10 10164.50 407.90 2 o -6 -2 -5 0 230.39 290.40 141.90 2 < 7 3 -5 0 1694.10 1806.40 216.80 2 o -6 -2 -4 0 1862.40 2521.40 236.00 2 o 2 1 -4 0 5487.20 5502.80 339.80 2 o 7 3 -4 0 41.39 -33.10 136.30 2 < -3 -1 -3 0 531.76 685.70 214.80 2 o 5 2 -1 0 5442.00 5570.90 344.00 2 o -5 -2 2 0 8204.90 8131.10 386.30 2 o -5 -2 3 0 7692.10 7843.80 382.40 2 o 3 1 3 0 579.74 556.40 217.60 2 < 3 1 4 0 61055.00 70860.60 1064.80 2 o -2 -1 5 0 1984.40 2049.50 251.80 2 o -2 -1 6 0 11559.00 10696.50 415.80 2 o 6 2 7 0 703.50 648.10 174.40 2 o 1 0 8 0 1143.30 1629.50 215.10 2 o 6 2 8 0 3359.80 4715.30 318.20 2 o 1 0 9 0 3800.40 3574.30 280.20 2 o 6 2 9 0 1021.90 482.70 177.40 2 < 1 0 10 0 468.28 642.80 184.20 2 o 1 1 -9 1 898.20 888.00 195.40 2 o 1 1 -8 1 162.26 325.70 156.60 2 < 6 3 -8 1 153.85 124.80 139.90 2 < -4 -1 -7 1 39.68 51.90 137.90 2 < 4 2 -6 1 319.46 266.80 163.70 2 < 4 2 -5 1 932.62 720.80 196.10 2 o -6 -2 -3 1 338.87 154.00 168.80 2 < -6 -2 -2 1 270.31 125.90 155.30 2 < 2 1 -2 1 10044.00 6463.00 412.20 2 o 7 3 -2 1 37.23 -5.00 143.30 2 < 7 3 -1 1 314.93 291.80 155.30 2 < -3 -1 0 1 5674.30 3969.10 320.90 2 o 5 2 2 1 417.88 23.40 200.90 2 < 5 2 3 1 191.22 130.00 175.10 2 < -5 -2 5 1 357.74 -6.80 173.10 2 < -5 -2 6 1 381.34 373.90 146.80 2 < 3 1 6 1 347.89 185.10 186.60 2 < -5 -2 7 1 65.09 43.20 130.50 2 < 3 1 7 1 247.29 143.30 174.20 2 < -2 -1 8 1 625.93 253.00 159.50 2 < 3 1 8 1 19.97 -178.50 153.90 2 < -2 -1 9 1 211.00 482.00 156.00 2 o -2 -1 10 1 137.47 176.00 139.10 2 < -4 -1 -10 -1 13.75 158.70 123.50 3 < -4 -1 -9 -1 68.91 -118.10 120.60 3 < 4 2 -9 -1 13.01 74.70 154.60 3 < 7 3 -8 -1 157.70 231.30 140.10 3 < 7 3 -7 -1 96.07 97.10 135.10 3 < 2 1 -6 -1 2013.00 2452.10 258.60 3 o -6 -2 -5 -1 264.66 420.80 139.80 3 o -3 -1 -4 -1 399.67 434.70 184.50 3 < 5 2 -4 -1 35.33 -15.60 180.40 3 < 8 3 -2 -1 181.57 477.00 151.40 3 o 8 3 -1 -1 12.51 347.60 133.90 3 < 3 1 0 -1 4786.30 4349.80 347.20 3 o -5 -2 1 -1 507.70 381.20 172.80 3 < -2 -1 2 -1 6995.20 5928.70 367.40 3 o 6 2 2 -1 213.96 230.10 168.30 3 < 6 2 3 -1 295.78 57.30 165.30 3 < -7 -3 6 -1 243.50 83.40 114.40 3 < 4 1 6 -1 139.00 -126.60 166.00 3 < -4 -2 7 -1 17.02 113.20 131.00 3 < 4 1 7 -1 67.20 178.60 156.10 3 < -4 -2 8 -1 104.97 111.30 127.70 3 < -1 -1 9 -1 780.65 673.10 159.80 3 o -1 -1 10 -1 52.87 -46.20 129.80 3 < -2 0 -11 0 2088.80 2584.20 230.30 3 o 1 1 -10 0 32.93 55.30 130.40 3 < 1 1 -9 0 1816.90 1529.30 222.90 3 o -4 -1 -8 0 1093.30 697.00 177.40 3 o 4 2 -8 0 408.28 307.60 144.20 3 < -4 -1 -7 0 491.15 451.20 152.70 3 < 4 2 -7 0 1937.00 800.10 192.60 3 o -1 0 -6 0 9602.50 10558.70 436.70 3 o 7 3 -6 0 495.12 571.60 162.40 3 o 7 3 -5 0 1319.90 1872.90 216.20 3 o 2 1 -4 0 4732.40 4685.10 321.50 3 o -6 -2 -3 0 3799.60 3871.20 281.70 3 o -3 -1 -2 0 1360.50 1224.80 249.30 3 o 5 2 -2 0 5610.00 6741.60 369.50 3 o 3 1 2 0 1540.00 1211.20 238.10 3 o -5 -2 3 0 9159.00 7942.90 370.90 3 o -5 -2 4 0 22050.00 22913.90 597.10 3 o -2 -1 5 0 1720.30 2109.10 255.10 3 o 6 2 5 0 195.23 35.70 155.70 3 < 6 2 6 0 669.38 990.40 190.10 3 o 1 0 7 0 7404.80 8570.30 391.60 3 o 4 1 9 0 1503.60 1477.40 197.60 3 o -4 -2 10 0 1164.60 888.30 149.60 3 o 4 1 10 0 62.08 -66.60 133.40 3 < 4 1 11 0 1674.30 1789.60 205.00 3 o -5 -1 -11 1 15.46 52.30 116.70 3 < -5 -1 -10 1 64.84 37.50 114.90 3 < 1 1 -8 1 38.72 -101.70 150.50 3 < 6 3 -8 1 134.70 27.60 130.60 3 < 1 1 -7 1 564.48 667.70 180.40 3 o -7 -2 -6 1 81.49 65.10 115.40 3 < 4 2 -6 1 394.17 335.50 162.10 3 < -4 -1 -5 1 793.28 1086.80 197.10 3 o 4 2 -5 1 744.41 988.70 196.80 3 o 7 3 -3 1 125.76 166.00 149.50 3 < 2 1 -2 1 7158.00 6743.10 404.00 3 o 7 3 -2 1 32.47 119.70 148.80 3 < -6 -2 -1 1 33.95 115.10 141.60 3 < 5 2 0 1 469.31 869.30 195.20 3 o -3 -1 1 1 18330.00 17148.90 557.80 3 o 5 2 1 1 390.26 -251.60 181.00 3 < -8 -3 5 1 62.47 239.50 118.10 3 < -5 -2 5 1 247.66 758.20 192.30 3 o 3 1 5 1 452.03 156.10 189.10 3 < -8 -3 6 1 44.90 326.20 108.40 3 o -5 -2 6 1 178.35 191.00 144.60 3 < -5 -2 7 1 46.84 33.20 120.30 3 < -2 -1 7 1 1252.20 1447.60 206.50 3 o 6 2 7 1 32.26 82.30 142.60 3 < -2 -1 8 1 348.00 121.40 140.40 3 < 6 2 8 1 13.02 -110.60 159.00 3 < 6 2 9 1 74.62 70.70 143.90 3 < 1 1 -10 -1 72.82 80.10 120.90 4 < 4 2 -9 -1 36.65 137.20 139.30 4 < -4 -1 -8 -1 75.64 2.00 121.90 4 < 7 3 -8 -1 178.80 118.50 139.80 4 < -4 -1 -7 -1 773.08 295.20 135.60 4 < 7 3 -7 -1 23.28 25.00 131.80 4 < 2 1 -6 -1 2047.60 2369.60 240.90 4 o -6 -2 -4 -1 252.42 234.70 138.60 4 < 5 2 -4 -1 50.47 182.40 157.20 4 < -6 -2 -3 -1 40.69 416.10 154.50 4 < -3 -1 -3 -1 797.06 784.80 189.50 4 o 8 3 -3 -1 194.84 280.90 148.50 4 < 8 3 -2 -1 333.23 335.60 150.80 4 < -5 -2 1 -1 257.67 330.60 154.80 4 < 6 2 1 -1 83.71 234.80 163.60 4 < -5 -2 2 -1 38.47 55.50 146.40 4 < -2 -1 2 -1 7717.20 6268.10 357.00 4 o 4 1 5 -1 873.79 865.80 208.30 4 o -7 -3 6 -1 320.41 244.10 105.60 4 < -4 -2 7 -1 37.62 82.30 120.30 4 < 7 2 7 -1 86.41 141.10 135.90 4 < -4 -2 8 -1 66.04 -178.60 126.90 4 < -1 -1 8 -1 68.43 35.60 138.90 4 < 7 2 8 -1 32.56 196.80 136.00 4 < -1 -1 9 -1 1051.70 700.20 168.10 4 o 5 1 11 -1 19.23 55.80 131.20 4 < -5 -1 -11 0 164.52 217.00 124.60 4 < -5 -1 -10 0 173.87 287.90 126.20 4 < -2 0 -10 0 193.24 157.80 126.30 4 < 1 1 -9 0 1013.40 737.40 173.60 4 o 4 2 -8 0 183.34 211.00 144.60 4 < 4 2 -7 0 165.70 248.00 135.40 4 < -4 -1 -6 0 9801.60 9623.00 392.10 4 o 7 3 -6 0 486.72 554.20 155.40 4 o -1 0 -5 0 65200.00 73624.90 1036.60 4 o 7 3 -5 0 1279.90 1558.20 198.60 4 o 2 1 -4 0 4236.80 4483.00 319.10 4 o -6 -2 -2 0 310.73 321.80 144.20 4 < 5 2 -2 0 6941.70 7488.30 372.00 4 o -6 -2 -1 0 441.13 531.10 150.50 4 o -3 -1 -1 0 21954.00 20680.30 585.10 4 o -5 -2 3 0 10966.00 9283.30 382.80 4 o 6 2 3 0 3569.90 3443.80 272.10 4 o -5 -2 4 0 21337.00 24413.60 599.20 4 o -2 -1 4 0 5553.70 4929.30 300.60 4 o 6 2 4 0 2592.90 2477.00 242.70 4 o 1 0 6 0 9947.40 12386.10 464.00 4 o 4 1 7 0 438.37 394.30 172.70 4 < 4 1 8 0 1135.80 939.80 181.70 4 o -4 -2 9 0 1687.40 1339.70 191.40 4 o -4 -2 10 0 1575.30 723.40 155.80 4 o -1 -1 10 0 312.08 110.60 132.60 4 < -1 -1 11 0 259.07 238.00 127.80 4 < -5 -1 -9 1 21.10 -74.80 127.40 4 < -5 -1 -8 1 208.85 120.70 122.10 4 < 6 3 -8 1 164.78 63.80 138.30 4 < 1 1 -7 1 38.61 129.30 151.00 4 < 4 2 -6 1 224.51 427.00 165.70 4 < -7 -2 -5 1 7.64 79.90 145.30 4 < 4 2 -5 1 842.16 399.40 174.80 4 < -7 -2 -4 1 8.82 45.50 124.10 4 < -4 -1 -4 1 22.64 433.90 157.40 4 < 7 3 -4 1 28.70 64.60 135.40 4 < 7 3 -3 1 39.49 -48.30 144.20 4 < 2 1 -2 1 7389.10 6510.80 395.20 4 o 5 2 0 1 469.75 734.50 178.10 4 o -6 -2 1 1 65.16 216.30 137.20 4 < -3 -1 1 1 14808.00 13836.10 498.50 4 o 3 1 4 1 368.31 203.10 209.10 4 < -5 -2 5 1 378.54 519.00 170.40 4 o 6 2 5 1 88.98 222.90 142.10 4 < -8 -3 6 1 134.60 9.50 106.30 4 < -5 -2 6 1 231.35 -16.70 138.10 4 < 6 2 6 1 13.54 233.80 138.10 4 < -2 -1 7 1 1389.10 1339.90 205.40 4 o 4 1 9 1 114.64 -6.30 135.10 4 < 4 1 10 1 16.02 -189.40 137.40 4 < 4 1 11 1 3.04 -140.70 125.30 4 < -5 -1 -10 -1 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