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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 # # # ################################################################################ ############################################################################## # # # This CIF contains the data in a paper accepted for publication in Acta # # Crystallographica Section B. It has been peer reviewed under the auspices # # of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary may be obtained from # # ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1. # # # # Software is freely available for graphical display of the structure(s) in # # this CIF. For information consult the CIF home page http://www.iucr.org/ # # cif/home.html # # # # Copyright International Union of Crystallography # # # ############################################################################## data_global _audit_creation_method 'Jana2000 Version : 04/11/2005' _journal_date_recd_electronic 2006-01-05 _journal_date_accepted 2006-03-20 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 2006 _journal_volume 62 _journal_issue 4 _journal_page_first 556 _journal_page_last 566 _journal_paper_doi https://doi.org/10.1107/S0108768106010238 _journal_paper_category FA _journal_coeditor_code SN5033 _publ_contact_author_name 'Lukas Palatinus' _publ_contact_author_address ;Academy of Sciences of the Czech Republic Institute of Physics Na Slovance 2 182 21 Praha 8 Czech Republic ; _publ_contact_author_email 'palat@fzu.cz' _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ;The incommensurately and commensurately modulated crystal structures of chromium(II) diphosphate ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_address 'Palatinus, Lukas' ;Academy of Sciences of the Czech Republic Institute of Physics Na Slovance 2 182 21 Praha 8 Czechia ; 'Dusek, Michal' ;Academy of Sciences of the Czech Republic Institute of Physics Na Slovance 2 182 21 Praha 8 Czechia ; 'Glaum, Robert' ;Department of Inorganic Chemistry University of Bonn Gerhard-Domagk-Strasse 1 D-53121 Bonn Germany ; 'El Bali, Brahim' ;Laboratory of Mineral Solid Chemistry Department of Chemistry Faculty of Sciences Po Box 624 60000 Oujda Morocco ; data_alpha2-Cr2P2O7 _chemical_name_common 'chromium(II) diphosphate' _chemical_formula_moiety ? _chemical_formula_sum 'Cr2 O7 P2' _chemical_formula_structural 'Cr2 (P2 O7)' _chemical_formula_iupac 'Cr2 (P2 O7)' _chemical_formula_weight 277.9 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_ssg_name 'C2/m(\a0\g)0s' loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2,-x3,1/2-x4 3 -x1,-x2,-x3,-x4 4 x1,-x2,x3,1/2+x4 5 1/2+x1,1/2+x2,x3,x4 6 1/2-x1,1/2+x2,-x3,1/2-x4 7 1/2-x1,1/2-x2,-x3,-x4 8 1/2+x1,1/2-x2,x3,1/2+x4 _cell_length_a 7.0192 _cell_length_b 8.4063 _cell_length_c 4.6264 _cell_angle_alpha 90 _cell_angle_beta 108.6111 _cell_angle_gamma 90 _cell_volume 258.7078 _cell_formula_units_Z 2 _cell_measurement_reflns_used 3302 _cell_measurement_theta_min 4.58 _cell_measurement_theta_max 36.03 _cell_measurement_temperature 298 _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 -0.361(1) 0.00000 0.471(1) _exptl_crystal_type_of_structure mod _exptl_crystal_description column _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 3.5667 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 268 _exptl_absorpt_coefficient_mu 4.799 _exptl_absorpt_correction_type 'gaussian' _exptl_absorpt_process_details ;CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta Analytical numeric absorption correction using a multifaceted crystal model. ; _exptl_absorpt_correction_T_min 0.43451 _exptl_absorpt_correction_T_max 0.67729 _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'X-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Oxford Diffraction CCD' _diffrn_measurement_method 'Rotation method data acquisition using \w scans' _diffrn_detector_area_resol_mean 8.3438 _diffrn_reflns_number 20404 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_unetI/netI 0.0077 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_reduction_process ;Integration of the CCD images was done by program Crysalis RED (Oxford diffraction, 2004). The same program was used for indexing of the crystal shape, its refinement, absorption correction and data scaling. ; _diffrn_reflns_limit_index_m_1_max 4 _diffrn_reflns_limit_index_m_1_min -4 _reflns_number_total 2409 _reflns_number_gt 1433 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0577 _refine_ls_goodness_of_fit_ref 1.61 _refine_ls_restrained_S_all ? _refine_ls_number_reflns 2409 _refine_ls_number_parameters 179 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0004F^2^)' _refine_ls_shift/su_max 0.0070 _refine_ls_shift/su_mean 0.0008 _refine_diff_density_max 0.52 _refine_diff_density_min -0.49 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 0.059(10) loop_ _reflns_class_code _reflns_class_description _reflns_class_number_total _reflns_class_number_gt _reflns_class_R_factor_gt _reflns_class_wR_factor_all Main 'Main reflections' 283 278 0.0165 0.0408 Sat1 '1st-order satellites' 495 455 0.0177 0.0308 Sat2 '2nd-order satellites' 569 421 0.0329 0.0498 Sat3 '3rd-order satellites' 495 183 0.0905 0.1823 Sat4 '4th-order satellites' 567 96 0.1962 0.3688 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr 0.321 0.624 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' P 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'Crysalis CCD (Oxford diffraction, 2004)' _computing_cell_refinement 'Crysalis CCD (Oxford diffraction, 2004)' _computing_data_reduction 'Crysalis CCD (Oxford diffraction, 2004)' _computing_structure_solution '(BayMEM; van Smaalen et al., 2003)' _computing_structure_refinement '(Jana2000; Petricek et al., 2000)' _computing_molecular_graphics '(Diamond; Brandenburg et al., 2005)' _computing_publication_material '(Jana2000; Petricek et al., 2000)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P P 0.8028(13) -0.0194(14) 0.5834(10) 0.0059(2) Uani d . 1 . . P P(a) 0.790(3) -0.015(2) 0.574(4) 0.007(3) Uani d . 0.5 . . P P(b) 0.820(2) 0.0057(19) 0.589(4) 0.003(2) Uani d . 1 . . O O1 0.6374(2) 0 0.2773(3) 0.0087(4) Uani d . 1 . . O O2 1 -0.0643(3) 0.5 0.0176(6) Uani d . 1 . . O O2(a) 1.0004(13) -0.0540(9) 0.531(2) 0.026(3) Uani d . 0.5 . . O O3 0.80616(16) -0.14655(13) 0.7588(3) 0.0129(4) Uani d . 1 . . O O3(a) 0.8427(15) -0.1478(14) 0.732(3) 0.029(4) Uani d . 0.5 . . O O3(b) 0.7616(11) -0.1500(12) 0.772(2) 0.001(2) Uani d . 0.5 . . Cr Cr 0.5 -0.18787(7) 0 0.00773(16) Uani d . 1 . . Cr Cr(a) 0.4743(10) -0.1898(3) 0.019(2) 0.0113(14) Uani d . 0.5 . . loop_ _atom_site_aniso_label _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 _atom_site_aniso_type_symbol P 0.0056(4) 0.0059(4) 0.0047(4) -0.0003(3) -0.0004(3) 0.0001(3) P P(a) 0.000(5) 0.007(4) 0.015(3) -0.006(3) 0.003(3) -0.014(2) P P(b) -0.008(3) 0.002(4) 0.008(2) -0.004(3) -0.0098(19) -0.003(3) P O1 0.0098(7) 0.0060(6) 0.0082(7) 0 -0.0002(6) 0 O O2 0.0086(9) 0.0231(11) 0.0231(10) 0 0.0079(7) 0 O O2(a) 0.010(3) 0.054(7) 0.022(4) 0.000(5) 0.015(3) -0.011(5) O O3 0.0149(6) 0.0099(5) 0.0112(5) 0.0026(4) 0.0004(4) 0.0026(4) O O3(a) 0.036(7) 0.012(5) 0.020(5) 0.012(6) -0.019(5) -0.005(4) O O3(b) -0.003(4) 0.004(3) 0.000(3) 0.005(3) -0.004(3) -0.002(2) O Cr 0.0083(2) 0.0047(2) 0.0072(2) 0 -0.00176(16) 0 Cr Cr(a) 0.014(3) 0.0036(7) 0.012(2) -0.0017(8) -0.0015(17) 0.0007(9) Cr loop_ _atom_site_Fourier_wave_vector_seq_id _atom_site_Fourier_wave_vector_x _atom_site_Fourier_wave_vector_y _atom_site_Fourier_wave_vector_z 1 -0.361 0.0000 0.471 2 -0.722 0.0000 0.942 3 -1.083 0.0000 1.413 4 -1.444 0.0000 1.884 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 Px1 P x 1 Py1 P y 1 Pz1 P z 1 Px2 P x 2 Py2 P y 2 Pz2 P z 2 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O1x2 O1 x 2 O1y2 O1 y 2 O1z2 O1 z 2 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O3x1 O3 x 1 O3y1 O3 y 1 O3z1 O3 z 1 O3x2 O3 x 2 O3y2 O3 y 2 O3z2 O3 z 2 O3x3 O3 x 3 O3y3 O3 y 3 O3z3 O3 z 3 Crx1 Cr x 1 Cry1 Cr y 1 Crz1 Cr z 1 Crx2 Cr x 2 Cry2 Cr y 2 Crz2 Cr z 2 Crx3 Cr x 3 Cry3 Cr y 3 Crz3 Cr z 3 Crx4 Cr x 4 Cry4 Cr y 4 Crz4 Cr z 4 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Px1 0.0013(13) -0.010(2) Py1 0.0044(14) -0.008(2) Pz1 0.0061(10) 0.0052(17) Px2 0.0023(10) 0.0019(12) Py2 0.0062(12) 0.0051(14) Pz2 0.0014(8) 0.0030(9) O1x1 0 0 O1y1 -0.00141(15) 0.00644(15) O1z1 0 0 O1x2 0.00170(16) -0.00539(17) O1y2 0 0 O1z2 -0.0017(2) 0.0004(2) O2x1 0.0062(3) 0 O2y1 0 0.0109(3) O2z1 0.0439(4) 0 O3x1 -0.01704(17) 0.00896(19) O3y1 -0.00273(13) -0.00236(16) O3z1 0.0155(2) -0.0150(3) O3x2 -0.00256(17) -0.00714(17) O3y2 0.00085(14) -0.00076(13) O3z2 0.0045(3) 0.0044(2) O3x3 0.00108(18) -0.00048(16) O3y3 0.00017(16) -0.00096(13) O3z3 -0.0022(3) -0.0006(2) Crx1 0.01167(6) 0 Cry1 0 0.00186(12) Crz1 -0.01339(8) 0 Crx2 0 -0.00341(5) Cry2 -0.00049(12) 0 Crz2 0 0.00189(6) Crx3 0.00077(7) 0 Cry3 0 -0.00032(11) Crz3 -0.00131(8) 0 Crx4 0 0.00048(9) Cry4 -0.00039(12) 0 Crz4 0 0.00040(10) loop_ _atom_site_U_Fourier_id _atom_site_U_Fourier_atom_site_label _atom_site_U_Fourier_tens_elem _atom_site_U_Fourier_wave_vector_seq_id PU111 P U11 1 PU221 P U22 1 PU331 P U33 1 PU121 P U12 1 PU131 P U13 1 PU231 P U23 1 O3U111 O3 U11 1 O3U221 O3 U22 1 O3U331 O3 U33 1 O3U121 O3 U12 1 O3U131 O3 U13 1 O3U231 O3 U23 1 CrU111 Cr U11 1 CrU221 Cr U22 1 CrU331 Cr U33 1 CrU121 Cr U12 1 CrU131 Cr U13 1 CrU231 Cr U23 1 CrU112 Cr U11 2 CrU222 Cr U22 2 CrU332 Cr U33 2 CrU122 Cr U12 2 CrU132 Cr U13 2 CrU232 Cr U23 2 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin PU111 -0.0004(3) 0.0000(4) PU221 0.0011(4) 0.0003(4) PU331 0.0013(3) -0.0021(4) PU121 0.0001(3) 0.0004(3) PU131 0.0010(2) -0.0005(3) PU231 -0.0004(2) -0.0006(3) O3U111 -0.0048(6) 0.0048(6) O3U221 0.0000(5) 0.0002(6) O3U331 -0.0004(5) 0.0027(5) O3U121 -0.0001(4) -0.0001(5) O3U131 0.0033(4) -0.0020(4) O3U231 0.0000(4) 0.0002(4) CrU111 0 -0.0005(2) CrU221 0 -0.00010(19) CrU331 0 0.0016(2) CrU121 0.00021(12) 0 CrU131 0 0.00071(16) CrU231 -0.00012(12) 0 CrU112 0.0017(2) 0 CrU222 -0.0002(2) 0 CrU332 0.0012(2) 0 CrU122 0 -0.00028(12) CrU132 -0.00058(16) 0 CrU232 0 -0.00009(12) loop_ _atom_site_displace_special_func_atom_site_label _atom_site_displace_special_func_sawtooth_ax _atom_site_displace_special_func_sawtooth_ay _atom_site_displace_special_func_sawtooth_az _atom_site_displace_special_func_sawtooth_c _atom_site_displace_special_func_sawtooth_w O3 -0.0327 -0.0044 0.0057 0.69188(13) 0.9160(14) Cr -0.0238 0 0.0133 0.25 0.9163(16) loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w P 0.8605(7) 0.4160(14) P(a) 1.111(2) 0.0840(14) P(b) 1.107(2) 0.0840(14) O2 0.75 0.4160(14) O2(a) 1.0144(11) 0.0840(14) O3(a) 1.1659(13) 0.0840(14) O3(b) 1.2140(11) 0.0840(14) Cr(a) 0.7680(11) 0.0837(16) 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_publ_flag _geom_bond_distance_max _geom_bond_distance_min _geom_bond_distance_av P O1 . . yes 1.54(5) 1.52(3) 1.53(4) P O2 . . yes 1.61(5) 1.59(7) 1.60(6) P O3 . . yes 1.55(8) 1.43(5) 1.51(7) P O3 . 4_555 yes 1.57(8) 1.46(10) 1.49(8) Cr O1 . . yes 2.104(3) 2.046(2) 2.079(2) Cr O1 . 3_655 yes 2.104(3) 2.046(2) 2.080(2) Cr O3 . 1_554 yes 3.431(5) 2.378(5) 2.708(4) Cr O3 . 7_646 yes 2.048(4) 1.981(4) 2.023(4) Cr O3 . 2_656 yes 3.431(5) 2.378(5) 2.716(4) Cr O3 . 8_444 yes 2.048(4) 1.981(4) 2.023(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_publ_flag _geom_angle_max _geom_angle_min _geom_angle_av O1 P O2 . . . yes 109(3) 101.0(16) 105(2) O1 P O3 . . . yes 117(3) 110(5) 112(4) O1 P O3 . . 7_646 yes 69(3) 64(3) 66(3) O1 P O3 . . 2_757 yes 168(3) 163(5) 165(4) O1 P O3 . . 6_656 yes 64(3) 59(3) 62(3) O1 P O3 . . 4_555 yes 113(6) 108(5) 111(5) O2 P O3 . . . yes 109(3) 101(5) 103(4) O2 P O3 . . 7_646 yes 82(2) 69(3) 77(3) O2 P O3 . . 2_757 yes 78.1(14) 66.9(16) 72.7(17) O2 P O3 . . 6_656 yes 105(3) 90(2) 101(3) O2 P O3 . . 4_555 yes 113(4) 106(4) 111(4) O3 P O3 . . 7_646 yes 67(3) 60(3) 63(3) O3 P O3 . . 2_757 yes 57.2(14) 53.8(11) 55.9(13) O3 P O3 . . 6_656 yes 160(3) 153(3) 155(4) O3 P O3 . . 4_555 yes 115(3) 112.6(18) 114(3) O3 P O3 4_555 . . yes 115(3) 112.6(18) 114(2) O3 P O3 4_555 . 7_646 yes 177(4) 170(3) 172(3) O3 P O3 4_555 . 2_757 yes 84.4(14) 82.5(11) 83.2(14) O3 P O3 4_555 . 6_656 yes 56(2) 53.1(16) 54(2) O1 Cr O1 . . 3_655 yes 81.67(9) 78.94(8) 79.93(9) O1 Cr O2 . . 7_645 yes 147.94(10) 138.77(12) 141.28(11) O1 Cr O2 . . 7_646 yes 100.21(15) 94.15(16) 96.19(15) O1 Cr O3 . . 1_554 yes 89.29(11) 76.40(9) 83.86(11) O1 Cr O3 . . . yes 45.31(8) 44.08(7) 44.72(7) O1 Cr O3 . . 7_646 yes 97.00(11) 92.75(11) 95.19(11) O1 Cr O3 . . 2_655 yes 125.25(10) 122.09(10) 123.75(10) O1 Cr O3 . . 2_656 yes 91.00(11) 79.29(9) 85.76(11) O1 Cr O3 . . 8_444 yes 169.20(15) 160.22(15) 165.17(15) O1 Cr O1 3_655 . . yes 81.67(9) 78.94(8) 79.93(9) O1 Cr O2 3_655 . 7_645 yes 100.18(15) 94.15(16) 96.10(15) O1 Cr O2 3_655 . 7_646 yes 147.89(10) 138.77(12) 141.23(11) O1 Cr O3 3_655 . 1_554 yes 91.00(11) 79.29(9) 85.90(10) O1 Cr O3 3_655 . . yes 125.25(10) 122.10(10) 123.71(10) O1 Cr O3 3_655 . 7_646 yes 169.21(15) 160.22(15) 165.23(15) O1 Cr O3 3_655 . 2_655 yes 45.31(8) 44.09(7) 44.72(7) O1 Cr O3 3_655 . 2_656 yes 89.29(11) 76.39(9) 83.72(11) O1 Cr O3 3_655 . 8_444 yes 97.00(11) 92.74(11) 95.19(11) O3 Cr O3 1_554 . . yes 104.58(10) 89.55(10) 94.31(10) O3 Cr O3 1_554 . 7_646 yes 84.22(14) 78.50(15) 80.28(15) O3 Cr O3 1_554 . 2_655 yes 87.63(9) 74.64(9) 84.07(10) O3 Cr O3 1_554 . 2_656 yes 166.7(2) 163.83(13) 165.32(14) O3 Cr O3 1_554 . 8_444 yes 112.07(14) 106.52(16) 110.00(15) O3 Cr O3 7_646 . 1_554 yes 84.22(14) 78.50(15) 80.28(15) O3 Cr O3 7_646 . . yes 57.02(12) 53.82(12) 54.98(12) O3 Cr O3 7_646 . 2_655 yes 137.29(14) 131.45(14) 135.75(14) O3 Cr O3 7_646 . 2_656 yes 112.07(14) 106.52(16) 110.06(15) O3 Cr O3 7_646 . 8_444 yes 94.89(16) 91.43(16) 92.60(16) O3 Cr O3 2_656 . 1_554 yes 166.7(2) 163.83(13) 165.32(14) O3 Cr O3 2_656 . . yes 87.59(9) 74.64(9) 83.96(10) O3 Cr O3 2_656 . 7_646 yes 112.07(14) 106.52(16) 110.06(15) O3 Cr O3 2_656 . 2_655 yes 104.58(10) 89.55(10) 94.18(10) O3 Cr O3 2_656 . 8_444 yes 84.22(14) 78.50(15) 80.34(15) O3 Cr O3 8_444 . 1_554 yes 112.07(14) 106.52(16) 110.00(15) O3 Cr O3 8_444 . . yes 137.29(14) 131.45(14) 135.68(14) O3 Cr O3 8_444 . 7_646 yes 94.89(16) 91.43(16) 92.60(16) O3 Cr O3 8_444 . 2_655 yes 57.02(12) 53.82(12) 54.95(12) O3 Cr O3 8_444 . 2_656 yes 84.22(14) 78.50(15) 80.34(15) P O2 P . . 2_756 yes 155(3) 143(4) 146(4) data_alpha1-Cr2P2O7_superspace _chemical_name_common 'chromium(II) diphosphate' _chemical_formula_moiety ? _chemical_formula_sum 'Cr2 O7 P2' _chemical_formula_structural 'Cr2 (P2 O7)' _chemical_formula_iupac 'Cr2 (P2 O7)' _chemical_formula_weight 277.9 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_ssg_name 'C2/m(\a0\g)0s' loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2,-x3,1/2-x4 3 -x1,-x2,-x3,-x4 4 x1,-x2,x3,1/2+x4 5 1/2+x1,1/2+x2,x3,x4 6 1/2-x1,1/2+x2,-x3,1/2-x4 7 1/2-x1,1/2-x2,-x3,-x4 8 1/2+x1,1/2-x2,x3,1/2+x4 _cell_length_a 7.0464 _cell_length_b 8.4073 _cell_length_c 4.6394 _cell_angle_alpha 90 _cell_angle_beta 108.708 _cell_angle_gamma 90 _cell_volume 260.3224 _cell_formula_units_Z 2 _cell_measurement_reflns_used 4589 _cell_measurement_theta_min 2.8084 _cell_measurement_theta_max 26.4976 _cell_measurement_temperature 140 _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 -0.33330 0.00000 0.50000 _exptl_crystal_type_of_structure mod _exptl_crystal_description 'irregular column' _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 3.5446 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 268 _exptl_absorpt_coefficient_mu 4.769 _exptl_absorpt_correction_type 'gaussian' _exptl_absorpt_process_details ;CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta Analytical numeric absorption correction using a multifaceted crystal model. ; _exptl_absorpt_correction_T_min 0.43451 _exptl_absorpt_correction_T_max 0.67729 _exptl_special_details ? _diffrn_ambient_temperature 140 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'X-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Oxford Diffraction CCD' _diffrn_measurement_method 'Rotation method data acquisition using \w scans' _diffrn_detector_area_resol_mean 8.3438 _diffrn_reflns_number 13281 _diffrn_reflns_av_R_equivalents 0.0143 _diffrn_reflns_av_unetI/netI 0.0050 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 26.56 _diffrn_reflns_theta_full 26.56 _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_reduction_process ; Integration of the CCD images was done by program Crysalis RED (Oxford diffraction, 2004). The same program was used for indexing of the crystal shape, its refinement, absorption correction and data scaling. ; _diffrn_reflns_limit_index_m_1_max 3 _diffrn_reflns_limit_index_m_1_min -3 _reflns_number_total 1598 _reflns_number_gt 1466 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_all 0.0248 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0435 _refine_ls_goodness_of_fit_ref 1.71 _refine_ls_restrained_S_all ? _refine_ls_number_reflns 1598 _refine_ls_number_parameters 105 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0004F^2^)' _refine_ls_shift/su_max 0.0012 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_max 0.35 _refine_diff_density_min -0.34 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 0.039(9) loop_ _reflns_class_code _reflns_class_description _reflns_class_number_total _reflns_class_number_gt _reflns_class_R_factor_gt _reflns_class_wR_factor_all Main 'Main reflections' 283 280 0.0169 0.0418 Sat1 '1st-order satellites' 497 479 0.0188 0.0359 Sat2 '2nd-order satellites' 571 503 0.0265 0.0438 Sat3 '3rd-order satellites' 247 204 0.0475 0.0746 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr 0.321 0.624 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' P 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'Crysalis CCD (Oxford diffraction, 2004)' _computing_cell_refinement 'Crysalis CCD (Oxford diffraction, 2004)' _computing_data_reduction 'Crysalis CCD (Oxford diffraction, 2004)' _computing_structure_solution '(BayMEM; van Smaalen et al., 2003)' _computing_structure_refinement '(Jana2000; Petricek et al., 2000)' _computing_molecular_graphics '(Diamond; Brandenburg et al., 2005)' _computing_publication_material '(Jana2000; Petricek et al., 2000)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P P 0.80598(6) -0.01568(5) 0.58475(10) 0.00406(17) Uani d . 1 . . O O1 0.63867(18) 0 0.2766(3) 0.0057(4) Uani d . 1 . . O O2 1 -0.07145(17) 0.5 0.0086(5) Uani d . 1 . . O O3 0.80778(14) -0.14622(11) 0.7572(2) 0.0075(3) Uani d . 1 . . Cr Cr 0.5 -0.18740(3) 0 0.00463(14) Uani d . 1 . . loop_ _atom_site_aniso_label _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 _atom_site_aniso_type_symbol P 0.0032(3) 0.0044(2) 0.0041(3) -0.00011(13) 0.0005(2) 0.00005(13) P O1 0.0058(6) 0.0044(6) 0.0058(7) 0 0.0004(5) 0 O O2 0.0046(7) 0.0120(7) 0.0102(7) 0 0.0036(5) 0 O O3 0.0071(5) 0.0070(4) 0.0071(5) 0.0006(3) 0.0004(4) 0.0010(4) O Cr 0.0048(2) 0.0031(2) 0.0044(2) 0 -0.00074(15) 0 Cr loop_ _atom_site_Fourier_wave_vector_seq_id _atom_site_Fourier_wave_vector_x _atom_site_Fourier_wave_vector_y _atom_site_Fourier_wave_vector_z 1 -0.33333 0.00000 0.50000 2 -0.66667 0.00000 1.00000 3 -1.00000 0.00000 1.50000 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 Px1 P x 1 Py1 P y 1 Pz1 P z 1 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O1x2 O1 x 2 O1y2 O1 y 2 O1z2 O1 z 2 O1x3 O1 x 3 O1y3 O1 y 3 O1z3 O1 z 3 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O3x1 O3 x 1 O3y1 O3 y 1 O3z1 O3 z 1 O3x2 O3 x 2 O3y2 O3 y 2 O3z2 O3 z 2 Crx1 Cr x 1 Cry1 Cr y 1 Crz1 Cr z 1 Crx2 Cr x 2 Cry2 Cr y 2 Crz2 Cr z 2 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Px1 -0.00194(4) -0.00676(6) Py1 -0.00216(3) 0.00053(5) Pz1 0.00462(6) 0.01073(9) O1x1 0 0 O1y1 -0.00195(15) 0.00742(14) O1z1 0 0 O1x2 0.00244(15) -0.00775(15) O1y2 0 0 O1z2 -0.0001(2) 0.0005(2) O1x3 0 0 O1y3 0 -0.00087(8) O1z3 0 0 O2x1 0.00649(18) 0 O2y1 0 0.01002(16) O2z1 0.0469(3) 0 O3x1 -0.0126(3) 0.00806(18) O3y1 0.0009(2) -0.00409(13) O3z1 0.0182(5) -0.0169(3) O3x2 -0.00107(16) -0.00529(18) O3y2 0.00268(12) 0.00150(13) O3z2 0.0055(2) 0.0073(3) Crx1 0.01625(11) 0 Cry1 0 0.00182(3) Crz1 -0.01952(16) 0 Crx2 0 -0.00590(7) Cry2 -0.00070(3) 0 Crz2 0 0.00551(10) loop_ _atom_site_U_Fourier_id _atom_site_U_Fourier_atom_site_label _atom_site_U_Fourier_tens_elem _atom_site_U_Fourier_wave_vector_seq_id O3U111 O3 U11 1 O3U221 O3 U22 1 O3U331 O3 U33 1 O3U121 O3 U12 1 O3U131 O3 U13 1 O3U231 O3 U23 1 O3U112 O3 U11 2 O3U222 O3 U22 2 O3U332 O3 U33 2 O3U122 O3 U12 2 O3U132 O3 U13 2 O3U232 O3 U23 2 CrU111 Cr U11 1 CrU221 Cr U22 1 CrU331 Cr U33 1 CrU121 Cr U12 1 CrU131 Cr U13 1 CrU231 Cr U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin O3U111 -0.0021(5) 0.0025(4) O3U221 0.0001(4) -0.0009(4) O3U331 -0.0005(5) 0.0012(4) O3U121 -0.0001(4) -0.0007(3) O3U131 0.0016(4) -0.0012(3) O3U231 -0.0003(4) -0.0006(3) O3U112 -0.0006(4) -0.0009(4) O3U222 -0.0003(4) -0.0004(4) O3U332 -0.0003(4) -0.0003(4) O3U122 -0.0002(3) 0.0001(3) O3U132 0.0005(3) 0.0008(3) O3U232 0.0002(3) -0.0001(3) CrU111 0 -0.00109(14) CrU221 0 0.00002(12) CrU331 0 0.00013(14) CrU121 0.00029(11) 0 CrU131 0 0.00041(10) CrU231 -0.00011(10) 0 loop_ _atom_site_displace_special_func_atom_site_label _atom_site_displace_special_func_sawtooth_ax _atom_site_displace_special_func_sawtooth_ay _atom_site_displace_special_func_sawtooth_az _atom_site_displace_special_func_sawtooth_c _atom_site_displace_special_func_sawtooth_w O3 -0.0513(5) -0.0117(3) 0.0055(7) 0.69266(12) 1 Cr -0.02552(16) 0 0.0089(2) 0.25 1 loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w P 0.85705(6) 0.5 O2 0.75 0.5 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_publ_flag _geom_bond_distance_max _geom_bond_distance_min _geom_bond_distance_av P O1 . . yes 1.5409(17) 1.5335(17) 1.5379(17) P O2 . . yes 1.608(2) 1.597(2) 1.601(2) P O3 . . yes 1.521(4) 1.513(3) 1.518(4) P O3 . 4_555 yes 1.509(3) 1.490(4) 1.498(4) Cr O1 . . yes 2.1088(17) 2.0586(18) 2.0809(18) Cr O1 . 3_655 yes 2.1088(17) 2.0586(18) 2.0809(18) Cr O3 . 1_554 yes 3.487(6) 2.366(3) 2.769(5) Cr O3 . 7_646 yes 2.049(3) 1.977(4) 2.023(4) Cr O3 . 2_656 yes 3.486(6) 2.366(3) 2.769(5) Cr O3 . 8_444 yes 2.049(3) 1.977(4) 2.023(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_publ_flag _geom_angle_max _geom_angle_min _geom_angle_av O1 P O2 . . . yes 107.08(10) 103.35(10) 105.42(10) O1 P O3 . . . yes 111.92(18) 110.95(14) 111.36(15) O1 P O3 . . 7_646 yes 67.19(11) 64.47(10) 65.99(10) O1 P O3 . . 2_757 yes 165.67(11) 164.79(10) 165.09(11) O1 P O3 . . 6_656 yes 63.94(9) 60.17(9) 62.27(9) O1 P O3 . . 4_555 yes 111.78(18) 110.38(13) 111.05(15) O2 P O3 . . . yes 105.37(16) 102.2(2) 103.5(2) O2 P O3 . . 7_646 yes 79.66(19) 70.48(14) 76.35(15) O2 P O3 . . 2_757 yes 78.09(8) 68.27(11) 73.57(9) O2 P O3 . . 6_656 yes 105.35(13) 97.08(13) 102.42(15) O2 P O3 . . 4_555 yes 111.47(16) 110.5(2) 111.0(2) O3 P O3 . . 7_646 yes 67.4(2) 60.24(11) 62.95(17) O3 P O3 . . 2_757 yes 57.91(19) 54.52(10) 55.87(15) O3 P O3 . . 6_656 yes 157.50(14) 152.09(18) 154.01(18) O3 P O3 . . 4_555 yes 114.4(2) 113.4(2) 113.9(2) O3 P O3 4_555 . . yes 114.4(2) 113.4(2) 113.9(2) O3 P O3 4_555 . 7_646 yes 177.41(14) 169.3(2) 172.36(19) O3 P O3 4_555 . 2_757 yes 83.73(13) 81.21(16) 82.45(15) O3 P O3 4_555 . 6_656 yes 55.00(12) 52.71(15) 54.15(15) O1 Cr O1 . . 3_655 yes 81.90(7) 79.13(6) 80.26(6) O1 Cr O2 . . 7_645 yes 144.11(7) 136.57(9) 139.44(8) O1 Cr O2 . . 7_646 yes 97.78(10) 92.58(9) 95.41(9) O1 Cr O3 . . 1_554 yes 90.43(8) 75.35(8) 83.15(9) O1 Cr O3 . . . yes 45.46(6) 44.18(6) 44.78(7) O1 Cr O3 . . 7_646 yes 96.55(10) 92.88(13) 94.95(10) O1 Cr O3 . . 2_655 yes 125.63(7) 121.59(9) 123.69(7) O1 Cr O3 . . 2_656 yes 92.54(9) 78.71(9) 85.76(9) O1 Cr O3 . . 8_444 yes 170.14(16) 161.13(14) 166.28(14) O1 Cr O1 3_655 . . yes 81.90(7) 79.13(6) 80.26(6) O1 Cr O2 3_655 . 7_645 yes 97.79(10) 92.57(9) 95.41(9) O1 Cr O2 3_655 . 7_646 yes 144.12(7) 136.56(9) 139.45(8) O1 Cr O3 3_655 . 1_554 yes 92.54(9) 78.70(9) 85.76(9) O1 Cr O3 3_655 . . yes 125.63(7) 121.58(9) 123.69(7) O1 Cr O3 3_655 . 7_646 yes 170.15(16) 161.13(14) 166.28(14) O1 Cr O3 3_655 . 2_655 yes 45.46(6) 44.17(6) 44.78(7) O1 Cr O3 3_655 . 2_656 yes 90.43(8) 75.35(8) 83.15(9) O1 Cr O3 3_655 . 8_444 yes 96.55(10) 92.88(13) 94.95(10) O3 Cr O3 1_554 . . yes 105.42(11) 90.18(11) 94.79(10) O3 Cr O3 1_554 . 7_646 yes 84.60(18) 78.87(17) 81.00(15) O3 Cr O3 1_554 . 2_655 yes 87.76(11) 73.55(11) 83.77(10) O3 Cr O3 1_554 . 2_656 yes 166.56(14) 164.11(8) 165.37(10) O3 Cr O3 1_554 . 8_444 yes 112.14(17) 106.60(18) 109.39(15) O3 Cr O3 7_646 . 1_554 yes 84.60(17) 78.87(18) 81.00(15) O3 Cr O3 7_646 . . yes 57.36(17) 53.29(13) 54.90(12) O3 Cr O3 7_646 . 2_655 yes 137.13(13) 131.02(16) 135.65(13) O3 Cr O3 7_646 . 2_656 yes 112.14(19) 106.60(17) 109.39(15) O3 Cr O3 7_646 . 8_444 yes 94.19(17) 90.91(9) 92.28(13) O3 Cr O3 2_656 . 1_554 yes 166.56(14) 164.11(8) 165.37(10) O3 Cr O3 2_656 . . yes 87.77(11) 73.54(11) 83.77(10) O3 Cr O3 2_656 . 7_646 yes 112.14(17) 106.60(18) 109.39(15) O3 Cr O3 2_656 . 2_655 yes 105.42(11) 90.18(11) 94.79(10) O3 Cr O3 2_656 . 8_444 yes 84.60(18) 78.86(17) 80.99(15) O3 Cr O3 8_444 . 1_554 yes 112.14(19) 106.60(17) 109.39(15) O3 Cr O3 8_444 . . yes 137.12(13) 131.02(16) 135.65(13) O3 Cr O3 8_444 . 7_646 yes 94.19(18) 90.91(10) 92.28(13) O3 Cr O3 8_444 . 2_655 yes 57.35(17) 53.30(13) 54.90(12) O3 Cr O3 8_444 . 2_656 yes 84.60(17) 78.86(18) 80.99(15) P O2 P . . 2_756 yes 144.9(2) 140.1(4) 143.3(3) data_alpha1-Cr2P2O7_supercell _chemical_name_common 'chromium(II) diphosphate' _chemical_formula_moiety ? _chemical_formula_sum 'Cr2 O7 P2' _chemical_formula_structural 'Cr2 (P2 O7)' _chemical_formula_iupac 'Cr2 (P2 O7)' _chemical_formula_weight 277.9 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'I2/c' _space_group_name_Hall -I2yc loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,1/2+z 6 1/2-x,1/2+y,-z 7 1/2-x,1/2-y,1/2-z 8 1/2+x,1/2-y,z _cell_length_a 21.1392 _cell_length_b 8.4073 _cell_length_c 9.2788 _cell_angle_alpha 90 _cell_angle_beta 108.708 _cell_angle_gamma 90 _cell_volume 1561.934 _cell_formula_units_Z 12 _cell_measurement_reflns_used 4589 _cell_measurement_theta_min 2.8084 _cell_measurement_theta_max 26.4976 _cell_measurement_temperature 140 _exptl_crystal_type_of_structure cryst _exptl_crystal_description 'irregular column' _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 3.5446 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 4.769 _exptl_absorpt_correction_type 'gaussian' _exptl_absorpt_process_details ;CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta Analytical numeric absorption correction using a multifaceted crystal model. ; _exptl_absorpt_correction_T_min 0.43451 _exptl_absorpt_correction_T_max 0.67729 _exptl_special_details ? _diffrn_ambient_temperature 140 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'X-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Oxford Diffraction CCD' _diffrn_measurement_method 'Rotation method data acquisition using \w scans' _diffrn_detector_area_resol_mean 8.3438 _diffrn_reflns_number 13281 _diffrn_reflns_av_R_equivalents 0.0143 _diffrn_reflns_av_unetI/netI 0.0050 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 26.56 _diffrn_reflns_theta_full 26.56 _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_reduction_process ; Integration of the CCD images was done by program Crysalis RED (Oxford diffraction, 2004). The same program was used for indexing of the crystal shape, its refinement, absorption correction and data scaling. ; _refine_special_details ;This sturcutre was obtained by transformation of the superspace struture model into the supercell description. It has not been refined, only zero refinement cycles have been run to obtain the R-factors. For this reason also the standard deviations of the atomic positions and distances are missing. For the refinement details interested reader should refer to the CIF of the modulated structure model, that has been deposited together with this CIF. ; _reflns_number_total 1598 _reflns_number_gt 1466 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_all 2.48 _refine_ls_R_factor_gt 2.05 _refine_ls_wR_factor_gt 3.96 _refine_ls_wR_factor_ref 4.35 _refine_ls_goodness_of_fit_ref 1.74 _refine_ls_restrained_S_all ? _refine_ls_number_reflns ? _refine_ls_number_parameters ? _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0004F^2^)' _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? _refine_diff_density_max ? _refine_diff_density_min ? _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 0.03852 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr 0.321 0.624 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' P 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'Crysalis CCD (Oxford diffraction, 2004)' _computing_cell_refinement 'Crysalis CCD (Oxford diffraction, 2004)' _computing_data_reduction 'Crysalis CCD (Oxford diffraction, 2004)' _computing_structure_solution '(BayMEM; van Smaalen et al., 2003)' _computing_structure_refinement '(Jana2000; Petricek et al., 2000)' _computing_molecular_graphics '(Diamond; Brandenburg et al., 2005)' _computing_publication_material '(Jana2000; Petricek et al., 2000)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P P-1 0.26637 -0.016404 0.298253 0.0041 Uani d . 1 . . P P-2 0.605125 -0.012662 0.283663 0.0041 Uani d . 1 . . P P-3 0.9363 -0.017968 0.790748 0.0041 Uani d . 1 . . O O1-1 0.215454 -0.004228 0.138077 0.0057 Uani d . 1 . . O O1-2 0.544184 -0.001568 0.138518 0.0057 Uani d . 1 . . O O1-3 0.879031 0.008382 0.138295 0.0057 Uani d . 1 . . O O2-1 0.335982 -0.066992 0.278751 0.0086 Uani d . 1 . . O O2-2 1 -0.083281 0.75 0.0086 Uani d . 1 . . O O3-1 0.251667 -0.155888 0.386693 0.0065 Uani d . 1 . . O O3-2 0.597313 -0.147007 0.385089 0.0068 Uani d . 1 . . O O3-3 0.950247 -0.141609 0.365348 0.0093 Uani d . 1 . . O O3-4 0.271849 -0.140358 0.880569 0.0068 Uani d . 1 . . O O3-5 0.621092 -0.143655 0.862703 0.0098 Uani d . 1 . . O O3-6 0.923398 -0.148771 0.891108 0.0059 Uani d . 1 . . Cr Cr-1 0.17817 -0.188629 -0.010977 0.005 Uani d . 1 . . Cr Cr-2 0.490328 -0.188103 0.011986 0.0046 Uani d . 1 . . Cr Cr-3 0.835755 -0.185473 -0.003236 0.0042 Uani d . 1 . . loop_ _atom_site_aniso_label _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 _atom_site_aniso_type_symbol P-1 0.003168 0.004376 0.004109 -0.000111 0.000455 0.000052 P P-2 0.003168 0.004376 0.004109 -0.000111 0.000455 0.000052 P P-3 0.003168 0.004376 0.004109 -0.000111 0.000455 0.000052 P O1-1 0.005788 0.00439 0.005764 0 0.000374 0 O O1-2 0.005788 0.00439 0.005764 0 0.000374 0 O O1-3 0.005788 0.00439 0.005764 0 0.000374 0 O O2-1 0.00459 0.011956 0.010189 0 0.003619 0 O O2-2 0.00459 0.011956 0.010189 0 0.003619 0 O O3-1 0.006032 0.006037 0.007129 0.000102 0.001703 0.000363 O O3-2 0.00522 0.008336 0.006186 0.001441 0.001088 0.001437 O O3-3 0.010033 0.006571 0.007982 0.000222 -0.001703 0.001243 O O3-4 0.006133 0.006997 0.006413 0.0011 0.000722 0.001613 O O3-5 0.010744 0.006496 0.008714 0.000077 -0.001872 0.000303 O O3-6 0.004427 0.007455 0.006171 0.00058 0.002246 0.00113 O Cr-1 0.005768 0.003058 0.004253 0.000145 -0.001105 -0.000056 Cr Cr-2 0.004813 0.003072 0.004359 -0.00029 -0.00074 0.000112 Cr Cr-3 0.003879 0.00309 0.004469 0.000145 -0.000383 -0.000056 Cr 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 P-1 O1-1 . . 1.5335 yes P-1 O2-1 . . 1.5968 yes P-1 O3-1 . . 1.5195 yes P-1 O3-4 . 4_554 1.509 yes P-2 O1-2 . . 1.5392 yes P-2 O2-1 . 2_655 1.5989 yes P-2 O3-2 . . 1.5127 yes P-2 O3-5 . 4_554 1.49 yes P-3 O1-3 . 4_555 1.541 yes P-3 O2-2 . . 1.6076 yes P-3 O3-3 . 4_555 1.495 yes P-3 O3-6 . . 1.5211 yes Cr-1 O1-1 . . 2.0587 yes Cr-1 O1-3 . 3_655 2.0586 yes Cr-1 O3-1 . 7_545 2.035 yes Cr-1 O3-4 . 1_554 2.5253 yes Cr-1 O3-5 . 8_444 1.9775 yes Cr-2 O1-2 . . 2.068 yes Cr-2 O1-2 . 3_655 2.0909 yes Cr-2 O3-2 . 2_655 2.3662 yes Cr-2 O3-3 . 7_645 2.0015 yes Cr-2 O3-6 . 8_444 2.0304 yes Cr-3 O1-1 . 3_655 2.1005 yes Cr-3 O1-3 . . 2.1088 yes Cr-3 O3-1 . 2_655 2.4348 yes Cr-3 O3-2 . 7_645 2.0475 yes Cr-3 O3-4 . 8_544 2.0487 yes Cr-3 O3-6 . 1_554 2.3778 yes 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 O1-1 P-1 O2-1 . . . 107.085 yes O1-1 P-1 O3-1 . . . 111.924 yes O1-1 P-1 O3-4 . . 4_554 110.385 yes O2-1 P-1 O3-1 . . . 102.193 yes O2-1 P-1 O3-4 . . 4_554 111.474 yes O3-1 P-1 O3-4 . . 4_554 113.359 yes O1-2 P-2 O2-1 . . 2_655 103.343 yes O1-2 P-2 O3-2 . . . 111.214 yes O1-2 P-2 O3-5 . . 4_554 111.785 yes O2-1 P-2 O3-2 2_655 . . 105.372 yes O2-1 P-2 O3-5 2_655 . 4_554 110.517 yes O3-2 P-2 O3-5 . . 4_554 113.893 yes O1-3 P-3 O2-2 4_555 . . 105.823 yes O1-3 P-3 O3-3 4_555 . 4_555 110.995 yes O1-3 P-3 O3-6 4_555 . . 110.944 yes O2-2 P-3 O3-3 . . 4_555 111.085 yes O2-2 P-3 O3-6 . . . 103.017 yes O3-3 P-3 O3-6 4_555 . . 114.38 yes O1-1 Cr-1 O1-3 . . 3_655 81.895 yes O1-1 Cr-1 O3-1 . . 7_545 92.902 yes O1-1 Cr-1 O3-4 . . 1_554 88.081 yes O1-1 Cr-1 O3-5 . . 8_444 164.681 yes O1-3 Cr-1 O3-1 3_655 . 7_545 170.146 yes O1-3 Cr-1 O3-4 3_655 . 1_554 92.543 yes O1-3 Cr-1 O3-5 3_655 . 8_444 92.885 yes O3-1 Cr-1 O3-4 7_545 . 1_554 78.866 yes O3-1 Cr-1 O3-5 7_545 . 8_444 94.192 yes O3-4 Cr-1 O3-5 1_554 . 8_444 106.604 yes O1-2 Cr-2 O1-2 . . 3_655 79.131 yes O1-2 Cr-2 O3-2 . . 2_655 91.138 yes O1-2 Cr-2 O3-3 . . 7_645 95.093 yes O1-2 Cr-2 O3-6 . . 8_444 170.072 yes O1-2 Cr-2 O1-2 3_655 . . 79.131 yes O1-2 Cr-2 O3-2 3_655 . 2_655 90.434 yes O1-2 Cr-2 O3-3 3_655 . 7_645 161.128 yes O1-2 Cr-2 O3-6 3_655 . 8_444 96.555 yes O3-2 Cr-2 O3-3 2_655 . 7_645 107.745 yes O3-2 Cr-2 O3-6 2_655 . 8_444 79.893 yes O3-3 Cr-2 O3-6 7_645 . 8_444 91.721 yes O1-1 Cr-3 O1-3 3_655 . . 79.739 yes O1-1 Cr-3 O3-1 3_655 . 2_655 82.381 yes O1-1 Cr-3 O3-2 3_655 . 7_645 167.637 yes O1-1 Cr-3 O3-4 3_655 . 8_544 95.875 yes O1-1 Cr-3 O3-6 3_655 . 1_554 88.666 yes O1-3 Cr-3 O3-1 . . 2_655 83.335 yes O1-3 Cr-3 O3-2 . . 7_645 96.369 yes O1-3 Cr-3 O3-4 . . 8_544 163.993 yes O1-3 Cr-3 O3-6 . . 1_554 85.223 yes O3-1 Cr-3 O3-2 2_655 . 7_645 108.969 yes O3-1 Cr-3 O3-4 2_655 . 8_544 80.819 yes O3-1 Cr-3 O3-6 2_655 . 1_554 166.557 yes O3-2 Cr-3 O3-4 7_645 . 8_544 90.912 yes O3-2 Cr-3 O3-6 7_645 . 1_554 79.281 yes O3-4 Cr-3 O3-6 8_544 . 1_554 110.196 yes P-1 O2-1 P-2 . . 2_655 144.871 yes P-3 O2-2 P-3 . . 2_756 140.055 yes