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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 _publ_section_keywords 'Al/Si ordering, vacancy ordering, ceramics, superspace' _audit_creation_method 'Jana2006 Version : 20/11/2017' _journal_date_recd_electronic 2018-03-02 _journal_date_accepted 2018-05-17 _journal_coeditor_code GQ5008 _journal_techeditor_code M180746 _iucr_compatibility_tag ACTA95 _journal_paper_category FA _publ_contact_author_name 'Paul Benjamin Klar' _publ_contact_author_address ;Departamento de Fisica de la Materia Condensada Facultad de Ciencia y Tecnologia Universidad del Pais Vasco UPV/EHU Apdo 644 Bilbao 48080 Spain ; _publ_contact_author_email paulbenjamin.klar@ehu.eus _publ_requested_journal IUCrJ _journal_name_full 'IUCrJ' _journal_volume 5 _journal_year 2018 _journal_page_first 497 _journal_page_last 509 _journal_paper_doi https://doi.org/10.1107/S2052252518007467 _publ_section_title 'Exploiting superspace to clarify vacancy and Al/Si ordering in mullite' _publ_section_title_footnote ? loop_ _publ_author_name _publ_author_address 'Klar, Paul Benjamin' ;Dpto de Fisica de la Materia Condensada, Facultad de Ciencia y Tecnologia Universidad del Pais Vasco UPV/EHU Apdo 644 Bilbao 48080 Spain ; 'Etxebarria, Inigo' ;Dpto de Fisica Aplicada II, Facultad de Ciencia y Tecnologia Universidad del Pais Vasco UPV/EHU Apdo 644 Bilbao 48080 Spain ; 'Madariaga, Gotzon' ;Dpto de Fisica de la Materia Condensada, Facultad de Ciencia y Tecnologia Universidad del Pais Vasco UPV/EHU Apdo 644 Bilbao 48080 Spain ; _publ_section_references ; Petricek, V., Dusek, M. & Palatinus, L. (2014). Z. Kristallogr. 229(5), 345-352. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. ; data_SA1 _database_code_depnum_ccdc_archive 'CCDC 1843794' _chemical_name_common Mullite _chemical_formula_sum 'Al4.857 O9.571 Si1.143' _chemical_formula_weight 316.3 _chemical_compound_source 'Sigma Aldrich' _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Pbam(\a01/2)0ss loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,-x2,x3,x3-x4+1/2 3 -x1+1/2,x2+1/2,-x3,-x4+1/2 4 x1+1/2,-x2+1/2,-x3,-x3+x4 5 -x1,-x2,-x3,-x4 6 x1,x2,-x3,-x3+x4+1/2 7 x1+1/2,-x2+1/2,x3,x4+1/2 8 -x1+1/2,x2+1/2,x3,x3-x4 _cell_length_a 7.5787(7) _cell_length_b 7.6707(4) _cell_length_c 2.88360(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 167.635(19) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.298800 0.000000 0.500000 _cell_formula_units_Z 1 _cell_measurement_reflns_used 2027 _cell_measurement_theta_min 4.06 _cell_measurement_theta_max 31.88 _cell_measurement_temperature 293 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 3.133 _exptl_crystal_F_000 156 _exptl_absorpt_coefficient_mu 1.08 _exptl_crystal_description 'irregularly shaped block' _exptl_crystal_size_max 0.056 _exptl_crystal_size_mid 0.051 _exptl_crystal_size_min 0.034 _exptl_crystal_size_rad 0.029 _exptl_crystal_colour colorless _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 1 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? _diffrn_ambient_temperature 293 _diffrn_source synchrotron _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7231 _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'dectris-CrysAlisPro-abstract goniometer imported dectris images' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.8 _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'polymer loop' _diffrn_reflns_number 3363 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 32.02 _diffrn_reflns_theta_full 23.49 _diffrn_measured_fraction_theta_max 0.77 _diffrn_measured_fraction_theta_full 0.95 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_unetI/netI 0.0034 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_limit_index_m_1_min -1 _diffrn_reflns_limit_index_m_1_max 1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 678 _reflns_number_gt 555 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_gt 0.1028 _refine_ls_R_factor_all 0.0384 _refine_ls_wR_factor_ref 0.1044 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_goodness_of_fit_gt 1.12 _refine_ls_number_reflns 678 _refine_ls_number_parameters 101 _refine_ls_number_constraints 33 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0081000002I^2^) _refine_ls_shift/su_max 0.0003 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_max 0.37 _refine_diff_density_min -0.33 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al 0.0680 0.0545 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0119 0.0065 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0865 0.0746 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_structure_refinement Jana2006 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 Al1 Al 0 0 0 Uani 0.0109(3) 2 1 d ? ? ? Al2 Al 0.14896(9) 0.33959(6) 0.5 Uani 0.0121(3) 4 0.5 d ? ? ? Si2 Si 0.14896(9) 0.33959(6) 0.5 Uani 0.0121(3) 4 0.286(2) d ? ? ? Al3 Al 0.2630(4) 0.2056(3) 0.5 Uani 0.0112(7) 4 0.214(2) d ? ? ? O1 O 0.35894(15) 0.42166(14) 0.5 Uani 0.0168(4) 4 1 d ? ? ? O2 O 0.12752(15) 0.21786(19) 0 Uani 0.0175(4) 4 1 d ? ? ? O3 O 0 0.5 0.5 Uani 0.020(3) 2 0.357(7) d ? ? ? O4 O 0.449(2) 0.0509(12) 0.5 Uani 0.017(3) 4 0.214(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 Al1 Al 0.0144(7) 0.0105(4) 0.0078(4) 0.00108(19) 0 0 Al2 Al 0.0151(6) 0.0119(4) 0.0092(4) -0.00092(17) 0 0 Si2 Si 0.0151(6) 0.0119(4) 0.0092(4) -0.00092(17) 0 0 Al3 Al 0.0116(16) 0.0138(10) 0.0082(8) 0.0005(9) 0 0 O1 O 0.0215(9) 0.0216(5) 0.0073(4) -0.0051(4) 0 0 O2 O 0.0210(8) 0.0169(6) 0.0145(4) -0.0057(4) 0 0 O3 O 0.019(7) 0.017(6) 0.025(3) 0.000(3) 0 0 O4 O 0.025(9) 0.009(4) 0.016(2) -0.0012(17) 0 0 loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 loop_ _jana_atom_site_occ_Fourier_absolute_site_label _jana_atom_site_occ_Fourier_absolute Al2 0.5 Si2 0.286(2) Al3 0.214(2) O3 0.357(7) O4 0.214(2) loop_ _atom_site_occ_Fourier_id _atom_site_occ_Fourier_atom_site_label _atom_site_occ_Fourier_wave_vector_seq_id Al2o1 Al2 1 Si2o1 Si2 1 Al3o1 Al3 1 O3o1 O3 1 O4o1 O4 1 loop_ _atom_site_occ_Fourier_param_id _atom_site_occ_Fourier_param_cos _atom_site_occ_Fourier_param_sin Al2o1 0.0486(5) 0.01396(14) Si2o1 0.0486(5) 0.01396(14) Al3o1 -0.0891(9) -0.0479(5) O3o1 -0.01838(19) 0 O4o1 -0.0674(7) -0.0755(8) 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 Al1x1 Al1 x 1 Al1y1 Al1 y 1 Al1z1 Al1 z 1 Al2x1 Al2 x 1 Al2y1 Al2 y 1 Al2z1 Al2 z 1 Si2x1 Si2 x 1 Si2y1 Si2 y 1 Si2z1 Si2 z 1 Al3x1 Al3 x 1 Al3y1 Al3 y 1 Al3z1 Al3 z 1 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O3x1 O3 x 1 O3y1 O3 y 1 O3z1 O3 z 1 O4x1 O4 x 1 O4y1 O4 y 1 O4z1 O4 z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Al1x1 0 0 Al1y1 0 0 Al1z1 0 -0.00471(7) Al2x1 0.00050(3) -0.00131(3) Al2y1 -0.00010(3) -0.00152(3) Al2z1 0 0 Si2x1 0.00050(3) -0.00131(3) Si2y1 -0.00010(3) -0.00152(3) Si2z1 0 0 Al3x1 0.0009(2) -0.00078(15) Al3y1 0.00052(18) -0.00089(13) Al3z1 0 0 O1x1 -0.00180(6) -0.00230(5) O1y1 0.00428(6) 0.00234(5) O1z1 0 0 O2x1 0 0 O2y1 0 0 O2z1 -0.00653(12) -0.00285(11) O3x1 0 -0.0029(5) O3y1 0 0.0034(4) O3z1 0 0 O4x1 -0.0015(10) 0.0004(10) O4y1 0.0006(8) 0.0000(6) O4z1 0 0 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 Al1U111 Al1 U11 1 Al1U221 Al1 U22 1 Al1U331 Al1 U33 1 Al1U121 Al1 U12 1 Al1U131 Al1 U13 1 Al1U231 Al1 U23 1 Al2U111 Al2 U11 1 Al2U221 Al2 U22 1 Al2U331 Al2 U33 1 Al2U121 Al2 U12 1 Al2U131 Al2 U13 1 Al2U231 Al2 U23 1 Si2U111 Si2 U11 1 Si2U221 Si2 U22 1 Si2U331 Si2 U33 1 Si2U121 Si2 U12 1 Si2U131 Si2 U13 1 Si2U231 Si2 U23 1 Al3U111 Al3 U11 1 Al3U221 Al3 U22 1 Al3U331 Al3 U33 1 Al3U121 Al3 U12 1 Al3U131 Al3 U13 1 Al3U231 Al3 U23 1 O1U111 O1 U11 1 O1U221 O1 U22 1 O1U331 O1 U33 1 O1U121 O1 U12 1 O1U131 O1 U13 1 O1U231 O1 U23 1 O2U111 O2 U11 1 O2U221 O2 U22 1 O2U331 O2 U33 1 O2U121 O2 U12 1 O2U131 O2 U13 1 O2U231 O2 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 O4U111 O4 U11 1 O4U221 O4 U22 1 O4U331 O4 U33 1 O4U121 O4 U12 1 O4U131 O4 U13 1 O4U231 O4 U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Al1U111 0 0 Al1U221 0 0 Al1U331 0 0 Al1U121 0 0 Al1U131 0.00016(8) 0 Al1U231 -0.00025(6) 0 Al2U111 -0.00093(15) 0.00014(13) Al2U221 -0.00094(11) 0.00158(9) Al2U331 0.00065(9) 0.00044(7) Al2U121 0.00014(8) -0.00005(8) Al2U131 0 0 Al2U231 0 0 Si2U111 -0.00093(15) 0.00014(13) Si2U221 -0.00094(11) 0.00158(9) Si2U331 0.00065(9) 0.00044(7) Si2U121 0.00014(8) -0.00005(8) Si2U131 0 0 Si2U231 0 0 Al3U111 0.0022(9) 0.0018(6) Al3U221 0.0035(6) 0.0012(4) Al3U331 0.0012(5) 0.0005(3) Al3U121 0.0004(5) -0.0001(4) Al3U131 0 0 Al3U231 0 0 O1U111 -0.0008(2) -0.0010(2) O1U221 0.0005(2) 0.00018(19) O1U331 0.00013(13) 0.00004(14) O1U121 0.00093(16) 0.00060(17) O1U131 0 0 O1U231 0 0 O2U111 0 0 O2U221 0 0 O2U331 0 0 O2U121 0 0 O2U131 -0.00041(16) -0.00009(16) O2U231 -0.00019(13) -0.00014(13) O3U111 -0.002(3) 0 O3U221 0.003(3) 0 O3U331 0.0042(10) 0 O3U121 0 0 O3U131 0 0 O3U231 0 0 O4U111 0.006(4) 0.003(4) O4U221 0.000(3) 0.0009(19) O4U331 -0.0030(11) 0.0001(11) O4U121 0 0 O4U131 0 0 O4U231 0 0 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 Al1 O1 ? 3_5455 1.8931(8) 1.8858(8) 1.9007(8) ? Al1 O1 ? 3_5465 1.8931(8) 1.8858(8) 1.9007(8) ? Al1 O1 ? 4_4555 1.8931(8) 1.8858(8) 1.9007(8) ? Al1 O1 ? 4_4565 1.8931(8) 1.8858(8) 1.9007(8) ? Al1 O2 ? ? 1.9305(14) 1.9304(14) 1.9306(14) ? Al1 O2 ? 2_5555 1.9305(14) 1.9304(14) 1.9306(14) ? Al2 O1 ? ? 1.7117(14) 1.7027(15) 1.7205(15) ? Al2 O2 ? ? 1.7256(9) 1.7144(9) 1.7367(9) ? Al2 O2 ? 1_5565 1.7256(9) 1.7144(9) 1.7367(9) ? Al2 O3 ? ? 1.6703(19) 1.635(3) 1.705(3) ? Al2 O4 ? 3_5565 1.781(12) 1.773(13) 1.789(13) ? Al2 O4 ? 4_4565 1.736(16) 1.730(16) 1.741(16) ? Si2 O1 ? ? 1.7117(14) 1.7027(15) 1.7205(15) ? Si2 O2 ? ? 1.7256(9) 1.7144(9) 1.7367(9) ? Si2 O2 ? 1_5565 1.7256(9) 1.7144(9) 1.7367(9) ? Si2 O3 ? ? 1.6703(19) 1.635(3) 1.705(3) ? Si2 O4 ? 3_5565 1.781(12) 1.773(13) 1.789(13) ? Si2 O4 ? 4_4565 1.736(16) 1.730(16) 1.741(16) ? Al3 O1 ? ? 1.810(3) 1.786(3) 1.834(3) ? Al3 O2 ? ? 1.7726(19) 1.761(2) 1.785(2) ? Al3 O2 ? 1_5565 1.7726(19) 1.761(2) 1.785(2) ? Al3 O4 ? ? 1.841(15) 1.827(16) 1.855(16) ? 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 O1 Al1 O1 3_5455 ? 3_5465 99.24(4) 99.23(4) 99.26(4) ? O1 Al1 O1 3_5455 ? 4_4555 80.77(4) 79.99(4) 81.58(4) ? O1 Al1 O1 3_5455 ? 4_4565 178.83(6) 178.14(5) 180.0(5) ? O1 Al1 O2 3_5455 ? ? 89.55(4) 88.36(4) 90.74(4) ? O1 Al1 O2 3_5455 ? 2_5555 90.45(4) 89.64(4) 91.25(4) ? O1 Al1 O1 3_5465 ? 4_4555 178.83(6) 178.14(5) 180.0(5) ? O1 Al1 O1 3_5465 ? 4_4565 80.77(4) 79.99(4) 81.58(4) ? O1 Al1 O2 3_5465 ? ? 89.54(4) 88.36(4) 90.74(4) ? O1 Al1 O2 3_5465 ? 2_5555 90.46(4) 89.64(4) 91.25(4) ? O1 Al1 O1 4_4555 ? 4_4565 99.24(4) 99.23(4) 99.26(4) ? O1 Al1 O2 4_4555 ? ? 90.46(4) 89.64(4) 91.25(4) ? O1 Al1 O2 4_4555 ? 2_5555 89.54(4) 88.36(4) 90.74(4) ? O1 Al1 O2 4_4565 ? ? 90.45(4) 89.64(4) 91.25(4) ? O1 Al1 O2 4_4565 ? 2_5555 89.55(4) 88.36(4) 90.74(4) ? O2 Al1 O2 ? ? 2_5555 179.63(7) 179.401(18) 180.0(5) ? O1 Al2 O2 ? ? ? 106.65(5) 105.71(5) 107.62(5) ? O1 Al2 O2 ? ? 1_5565 106.65(5) 105.71(5) 107.62(5) ? O1 Al2 O3 ? ? ? 110.95(12) 109.21(12) 112.69(13) ? O1 Al2 O4 ? ? 3_5565 92.9(5) 91.7(5) 94.2(5) ? O1 Al2 O4 ? ? 4_4565 129.4(4) 127.4(4) 131.5(4) ? O2 Al2 O2 ? ? 1_5565 113.37(6) 111.91(6) 114.80(6) ? O2 Al2 O3 ? ? ? 109.57(7) 109.45(7) 109.68(7) ? O2 Al2 O4 ? ? 3_5565 116.95(19) 116.65(18) 117.3(2) ? O2 Al2 O4 ? ? 4_4565 100.3(2) 100.0(2) 100.7(2) ? O2 Al2 O3 1_5565 ? ? 109.57(7) 109.45(7) 109.68(7) ? O2 Al2 O4 1_5565 ? 3_5565 116.95(19) 116.65(18) 117.3(2) ? O2 Al2 O4 1_5565 ? 4_4565 100.3(2) 100.0(2) 100.7(2) ? O3 Al2 O4 ? ? 3_5565 18.0(5) 17.6(5) 18.5(5) ? O3 Al2 O4 ? ? 4_4565 18.5(4) 18.1(4) 18.9(4) ? O4 Al2 O4 3_5565 ? 4_4565 36.5(7) 35.7(7) 37.3(7) ? O1 Si2 O2 ? ? ? 106.65(5) 105.71(5) 107.62(5) ? O1 Si2 O2 ? ? 1_5565 106.65(5) 105.71(5) 107.62(5) ? O1 Si2 O3 ? ? ? 110.95(12) 109.21(12) 112.69(13) ? O1 Si2 O4 ? ? 3_5565 92.9(5) 91.7(5) 94.2(5) ? O1 Si2 O4 ? ? 4_4565 129.4(4) 127.4(4) 131.5(4) ? O2 Si2 O2 ? ? 1_5565 113.37(6) 111.91(6) 114.80(6) ? O2 Si2 O3 ? ? ? 109.57(7) 109.45(7) 109.68(7) ? O2 Si2 O4 ? ? 3_5565 116.95(19) 116.65(18) 117.3(2) ? O2 Si2 O4 ? ? 4_4565 100.3(2) 100.0(2) 100.7(2) ? O2 Si2 O3 1_5565 ? ? 109.57(7) 109.45(7) 109.68(7) ? O2 Si2 O4 1_5565 ? 3_5565 116.95(19) 116.65(18) 117.3(2) ? O2 Si2 O4 1_5565 ? 4_4565 100.3(2) 100.0(2) 100.7(2) ? O3 Si2 O4 ? ? 3_5565 18.0(5) 17.6(5) 18.5(5) ? O3 Si2 O4 ? ? 4_4565 18.5(4) 18.1(4) 18.9(4) ? O4 Si2 O4 3_5565 ? 4_4565 36.5(7) 35.7(7) 37.3(7) ? O1 Al3 O2 ? ? ? 100.62(11) 99.92(11) 101.35(11) ? O1 Al3 O2 ? ? 1_5565 100.62(11) 99.92(11) 101.35(11) ? O1 Al3 O4 ? ? ? 106.5(5) 105.1(5) 107.9(5) ? O2 Al3 O2 ? ? 1_5565 108.88(17) 107.66(17) 110.07(17) ? O2 Al3 O4 ? ? ? 118.47(19) 118.36(18) 118.6(2) ? O2 Al3 O4 1_5565 ? ? 118.47(19) 118.36(18) 118.6(2) ? Al1 O1 Al1 3_5555 ? 3_5565 99.21(6) 98.39(6) 100.06(6) ? Al1 O1 Al2 3_5555 ? ? 129.91(3) 129.45(3) 130.38(3) ? Al1 O1 Si2 3_5555 ? ? 129.91(3) 129.45(3) 130.38(3) ? Al1 O1 Al3 3_5555 ? ? 121.17(6) 119.57(6) 122.76(6) ? Al1 O1 Al2 3_5565 ? ? 129.91(3) 129.45(3) 130.38(3) ? Al1 O1 Si2 3_5565 ? ? 129.91(3) 129.45(3) 130.38(3) ? Al1 O1 Al3 3_5565 ? ? 121.17(6) 119.57(6) 122.76(6) ? Al2 O1 Si2 ? ? ? 0.0(5) 0.0(5) 0.0(5) ? Al2 O1 Al3 ? ? ? 44.71(10) 44.31(10) 45.10(10) ? Si2 O1 Al3 ? ? ? 44.71(10) 44.31(10) 45.10(10) ? Al1 O2 Al2 ? ? 1_5545 121.05(4) 119.65(4) 122.44(4) ? Al1 O2 Al2 ? ? ? 121.03(4) 119.65(4) 122.44(4) ? Al1 O2 Si2 ? ? 1_5545 121.05(4) 119.65(4) 122.44(4) ? Al1 O2 Si2 ? ? ? 121.03(4) 119.65(4) 122.44(4) ? Al1 O2 Al3 ? ? 1_5545 104.14(10) 103.14(10) 105.12(10) ? Al1 O2 Al3 ? ? ? 104.12(10) 103.14(10) 105.12(10) ? Al2 O2 Al2 1_5545 ? ? 113.36(8) 113.35(8) 113.36(8) ? Al2 O2 Si2 1_5545 ? 1_5545 0.0(5) 0.0(5) 0.0(5) ? Al2 O2 Si2 1_5545 ? ? 113.36(8) 113.35(8) 113.36(8) ? Al2 O2 Al3 1_5545 ? 1_5545 45.12(8) 44.78(8) 45.45(9) ? Al2 O2 Al3 1_5545 ? ? 130.82(11) 130.70(11) 130.95(11) ? Al2 O2 Si2 ? ? 1_5545 113.36(8) 113.35(8) 113.36(8) ? Al2 O2 Si2 ? ? ? 0.0(5) 0.0(5) 0.0(5) ? Al2 O2 Al3 ? ? 1_5545 130.82(11) 130.70(11) 130.95(11) ? Al2 O2 Al3 ? ? ? 45.11(8) 44.78(8) 45.45(9) ? Si2 O2 Si2 1_5545 ? ? 113.36(8) 113.35(8) 113.36(8) ? Si2 O2 Al3 1_5545 ? 1_5545 45.12(8) 44.78(8) 45.45(9) ? Si2 O2 Al3 1_5545 ? ? 130.82(11) 130.70(11) 130.95(11) ? Si2 O2 Al3 ? ? 1_5545 130.82(11) 130.70(11) 130.95(11) ? Si2 O2 Al3 ? ? ? 45.11(8) 44.78(8) 45.45(9) ? Al3 O2 Al3 1_5545 ? ? 108.87(13) 108.86(13) 108.87(13) ? Al2 O3 Al2 ? ? 2_5655 179.28(15) 178.9(2) 180.0(5) ? Al2 O3 Si2 ? ? ? 0.0(5) 0.0(5) 0.0(5) ? Al2 O3 Si2 ? ? 2_5655 179.28(15) 178.9(2) 180.0(5) ? Al2 O3 Si2 2_5655 ? ? 179.28(15) 178.9(2) 180.0(5) ? Al2 O3 Si2 2_5655 ? 2_5655 0.0(5) 0.0(5) 0.0(5) ? Si2 O3 Si2 ? ? 2_5655 179.28(15) 178.9(2) 180.0(5) ? Al2 O4 Al2 3_5465 ? 4_5565 143.5(9) 142.3(9) 144.7(9) ? Al2 O4 Si2 3_5465 ? 3_5465 0.0(5) 0.0(5) 0.0(5) ? Al2 O4 Si2 3_5465 ? 4_5565 143.5(9) 142.3(9) 144.7(9) ? Al2 O4 Al3 3_5465 ? ? 105.6(9) 104.8(9) 106.5(9) ? Al2 O4 Si2 4_5565 ? 3_5465 143.5(9) 142.3(9) 144.7(9) ? Al2 O4 Si2 4_5565 ? 4_5565 0.0(5) 0.0(5) 0.0(5) ? Al2 O4 Al3 4_5565 ? ? 110.9(6) 110.2(6) 111.5(6) ? Si2 O4 Si2 3_5465 ? 4_5565 143.5(9) 142.3(9) 144.7(9) ? Si2 O4 Al3 3_5465 ? ? 105.6(9) 104.8(9) 106.5(9) ? Si2 O4 Al3 4_5565 ? ? 110.9(6) 110.2(6) 111.5(6) ? data_SA2 _database_code_depnum_ccdc_archive 'CCDC 1843795' _audit_creation_method 'Jana2006 Version : 20/11/2017' _chemical_name_common Mullite _chemical_formula_sum 'Al4.832 O9.584 Si1.168' _chemical_formula_weight 316.5 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Pbam(\a01/2)0ss loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,-x2,x3,x3-x4+1/2 3 -x1+1/2,x2+1/2,-x3,-x4+1/2 4 x1+1/2,-x2+1/2,-x3,-x3+x4 5 -x1,-x2,-x3,-x4 6 x1,x2,-x3,-x3+x4+1/2 7 x1+1/2,-x2+1/2,x3,x4+1/2 8 -x1+1/2,x2+1/2,x3,x3-x4 _cell_length_a 7.577(2) _cell_length_b 7.6727(18) _cell_length_c 2.8804(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 167.46(8) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.301000 0.000000 0.500000 _cell_formula_units_Z 1 _cell_measurement_reflns_used 1568 _cell_measurement_theta_max 31.98 _cell_measurement_theta_min 4.06 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 3.1387 _exptl_crystal_F_000 156 _exptl_absorpt_coefficient_mu 1.082 _exptl_crystal_description 'irregularly shaped block' _cell_measurement_temperature 293 _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device_type 'dectris-CrysAlisPro-abstract goniometer imported dectris images' _diffrn_ambient_temperature 293 _diffrn_source synchrotron _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7231 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_detector 'CCD plate' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 3079 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 31.87 _diffrn_reflns_theta_full 21.76 _diffrn_measured_fraction_theta_full 0.96 _diffrn_measured_fraction_theta_max 0.9 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_unetI/netI 0.0051 _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 -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_limit_index_m_1_min -1 _diffrn_reflns_limit_index_m_1_max 1 _reflns_number_total 768 _reflns_number_gt 544 _reflns_threshold_expression I>3\s(I) _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_gt 0.0846 _refine_ls_R_factor_all 0.0347 _refine_ls_wR_factor_ref 0.0885 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_goodness_of_fit_gt 1.27 _refine_ls_number_reflns 768 _refine_ls_number_parameters 101 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0035999999I^2^) _refine_ls_shift/su_max 0.0004 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_max 0.35 _refine_diff_density_min -0.39 _refine_ls_extinction_method none _refine_ls_number_constraints 33 _refine_ls_structure_factor_coef Fsqd loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al 0.0680 0.0545 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0119 0.0065 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0865 0.0746 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_structure_refinement Jana2006 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 Al1 Al 0 0 0 Uani 0.00863(17) 2 1 d ? ? ? Al2 Al 0.14885(5) 0.33985(4) 0.5 Uani 0.00933(17) 4 0.5 d ? ? ? Si2 Si 0.14885(5) 0.33985(4) 0.5 Uani 0.00933(17) 4 0.2920(19) d ? ? ? Al3 Al 0.2626(2) 0.2043(2) 0.5 Uani 0.0086(4) 4 0.2080(19) d ? ? ? O1 O 0.35912(10) 0.42179(11) 0.5 Uani 0.0151(2) 4 1 d ? ? ? O2 O 0.12766(11) 0.21705(13) 0 Uani 0.0161(2) 4 1 d ? ? ? O3 O 0 0.5 0.5 Uani 0.0196(19) 2 0.376(6) d ? ? ? O4 O 0.4483(9) 0.0466(9) 0.5 Uani 0.0114(17) 4 0.2080(19) 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 Al1 Al 0.0085(3) 0.0089(3) 0.0085(3) 0.00056(12) 0 0 Al2 Al 0.0070(3) 0.0107(3) 0.0102(3) -0.00055(10) 0 0 Si2 Si 0.0070(3) 0.0107(3) 0.0102(3) -0.00055(10) 0 0 Al3 Al 0.0066(7) 0.0109(8) 0.0084(7) 0.0005(5) 0 0 O1 O 0.0147(4) 0.0221(4) 0.0086(4) -0.0079(3) 0 0 O2 O 0.0159(4) 0.0173(4) 0.0150(4) -0.0072(3) 0 0 O3 O 0.008(4) 0.019(4) 0.0317(18) 0.0023(18) 0 0 O4 O 0.005(4) 0.011(3) 0.0182(18) 0.0004(12) 0 0 loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 loop_ _jana_atom_site_occ_Fourier_absolute_site_label _jana_atom_site_occ_Fourier_absolute Al2 0.5 Si2 0.2920(19) Al3 0.2080(19) O3 0.376(6) O4 0.2080(19) loop_ _atom_site_occ_Fourier_id _atom_site_occ_Fourier_atom_site_label _atom_site_occ_Fourier_wave_vector_seq_id Al2o1 Al2 1 Si2o1 Si2 1 Al3o1 Al3 1 O3o1 O3 1 O4o1 O4 1 loop_ _atom_site_occ_Fourier_param_id _atom_site_occ_Fourier_param_cos _atom_site_occ_Fourier_param_sin Al2o1 0.0341(3) 0.00987(8) Si2o1 0.0341(3) 0.00987(8) Al3o1 -0.0625(5) -0.0339(3) O3o1 -0.01212(10) 0 O4o1 -0.0470(4) -0.0533(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 Al1x1 Al1 x 1 Al1y1 Al1 y 1 Al1z1 Al1 z 1 Al2x1 Al2 x 1 Al2y1 Al2 y 1 Al2z1 Al2 z 1 Si2x1 Si2 x 1 Si2y1 Si2 y 1 Si2z1 Si2 z 1 Al3x1 Al3 x 1 Al3y1 Al3 y 1 Al3z1 Al3 z 1 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O3x1 O3 x 1 O3y1 O3 y 1 O3z1 O3 z 1 O4x1 O4 x 1 O4y1 O4 y 1 O4z1 O4 z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Al1x1 0 0 Al1y1 0 0 Al1z1 0 -0.00305(6) Al2x1 0.00037(2) -0.00084(2) Al2y1 -0.00012(2) -0.00096(2) Al2z1 0 0 Si2x1 0.00037(2) -0.00084(2) Si2y1 -0.00012(2) -0.00096(2) Si2z1 0 0 Al3x1 0.00063(11) -0.00064(9) Al3y1 -0.00008(10) -0.00081(9) Al3z1 0 0 O1x1 -0.00121(4) -0.00157(4) O1y1 0.00276(4) 0.00164(4) O1z1 0 0 O2x1 0 0 O2y1 0 0 O2z1 -0.00431(11) -0.00194(10) O3x1 0 -0.0017(3) O3y1 0 0.0018(3) O3z1 0 0 O4x1 -0.0014(6) 0.0004(4) O4y1 -0.0008(6) -0.0013(4) O4z1 0 0 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 Al1U111 Al1 U11 1 Al1U221 Al1 U22 1 Al1U331 Al1 U33 1 Al1U121 Al1 U12 1 Al1U131 Al1 U13 1 Al1U231 Al1 U23 1 Al2U111 Al2 U11 1 Al2U221 Al2 U22 1 Al2U331 Al2 U33 1 Al2U121 Al2 U12 1 Al2U131 Al2 U13 1 Al2U231 Al2 U23 1 Si2U111 Si2 U11 1 Si2U221 Si2 U22 1 Si2U331 Si2 U33 1 Si2U121 Si2 U12 1 Si2U131 Si2 U13 1 Si2U231 Si2 U23 1 Al3U111 Al3 U11 1 Al3U221 Al3 U22 1 Al3U331 Al3 U33 1 Al3U121 Al3 U12 1 Al3U131 Al3 U13 1 Al3U231 Al3 U23 1 O1U111 O1 U11 1 O1U221 O1 U22 1 O1U331 O1 U33 1 O1U121 O1 U12 1 O1U131 O1 U13 1 O1U231 O1 U23 1 O2U111 O2 U11 1 O2U221 O2 U22 1 O2U331 O2 U33 1 O2U121 O2 U12 1 O2U131 O2 U13 1 O2U231 O2 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 O4U111 O4 U11 1 O4U221 O4 U22 1 O4U331 O4 U33 1 O4U121 O4 U12 1 O4U131 O4 U13 1 O4U231 O4 U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Al1U111 0 0 Al1U221 0 0 Al1U331 0 0 Al1U121 0 0 Al1U131 0.00017(6) 0 Al1U231 -0.00011(7) 0 Al2U111 -0.00021(8) 0.00017(7) Al2U221 -0.00026(8) 0.00118(8) Al2U331 0.00094(8) 0.00039(7) Al2U121 0.00012(6) -0.00004(6) Al2U131 0 0 Al2U231 0 0 Si2U111 -0.00021(8) 0.00017(7) Si2U221 -0.00026(8) 0.00118(8) Si2U331 0.00094(8) 0.00039(7) Si2U121 0.00012(6) -0.00004(6) Si2U131 0 0 Si2U231 0 0 Al3U111 0.0008(4) 0.0005(3) Al3U221 0.0009(4) 0.0003(4) Al3U331 -0.0013(4) -0.0007(3) Al3U121 0.0003(3) -0.0005(3) Al3U131 0 0 Al3U231 0 0 O1U111 -0.00058(17) -0.00062(17) O1U221 0.00012(18) 0.00009(18) O1U331 0.00028(13) 0.00023(14) O1U121 0.00069(14) 0.00071(13) O1U131 0 0 O1U231 0 0 O2U111 0 0 O2U221 0 0 O2U331 0 0 O2U121 0 0 O2U131 -0.00013(12) -0.00004(12) O2U231 -0.00021(13) -0.00020(13) O3U111 -0.001(3) 0 O3U221 0.000(2) 0 O3U331 0.0044(10) 0 O3U121 0 0 O3U131 0 0 O3U231 0 0 O4U111 -0.001(2) -0.0014(15) O4U221 0.0004(18) -0.0008(12) O4U331 -0.0015(10) -0.0022(9) O4U121 0 0 O4U131 0 0 O4U231 0 0 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 Al1 Al1 ? 1_5545 2.88040(12) 2.8628(2) 2.8980(2) ? Al1 Al1 ? 1_5565 2.88040(12) 2.8628(2) 2.8980(2) ? Al1 Al3 ? 1_5545 2.9137(18) 2.9049(18) 2.9224(18) ? Al1 Al3 ? ? 2.9135(18) 2.9049(18) 2.9224(18) ? Al1 Al3 ? 2_5545 2.9135(18) 2.9049(18) 2.9224(18) ? Al1 Al3 ? 2_5555 2.9137(18) 2.9049(18) 2.9224(18) ? Al2 Al2 ? 1_5545 2.880436(3) 2.880405(4) 2.880466(4) ? Al2 Al2 ? 1_5565 2.880436(3) 2.880405(4) 2.880466(4) ? Al2 Si2 ? ? 0 0 0 ? Al2 Al3 ? ? 1.3510(18) 1.3496(18) 1.3525(18) ? Al2 Al3 ? 3_5565 2.8754(17) 2.8716(18) 2.8790(18) ? Al2 Al3 ? 4_4565 2.946(3) 2.935(3) 2.957(3) ? Al2 O3 ? ? 1.6681(15) 1.648(3) 1.687(3) ? Si2 Al3 ? ? 1.3510(18) 1.3496(18) 1.3525(18) ? Si2 O3 ? ? 1.6681(15) 1.648(3) 1.687(3) ? Al3 Al3 ? 1_5545 2.880430(11) 2.880410(14) 2.880448(14) ? Al3 Al3 ? 1_5565 2.880430(11) 2.880410(14) 2.880448(14) ? O3 O4 ? 3_5565 0.530(8) 0.521(9) 0.539(9) ? O3 O4 ? 4_4565 0.530(8) 0.521(9) 0.539(9) ? O4 O4 ? 2_6555 1.060(11) 1.051(12) 1.069(12) ? 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 Al1 Al1 Al1 1_5545 ? 1_5565 180.0(5) 180.0(5) 180.0(5) ? Al1 Al1 Al3 1_5545 ? 1_5545 60.38(2) 60.21(2) 60.54(2) ? Al1 Al1 Al3 1_5545 ? ? 119.62(2) 119.46(2) 119.79(2) ? Al1 Al1 Al3 1_5545 ? 2_5545 60.38(2) 60.21(2) 60.54(2) ? Al1 Al1 Al3 1_5545 ? 2_5555 119.62(2) 119.46(2) 119.79(2) ? Al1 Al1 Al3 1_5565 ? 1_5545 119.62(2) 119.46(2) 119.79(2) ? Al1 Al1 Al3 1_5565 ? ? 60.38(2) 60.21(2) 60.54(2) ? Al1 Al1 Al3 1_5565 ? 2_5545 119.62(2) 119.46(2) 119.79(2) ? Al1 Al1 Al3 1_5565 ? 2_5555 60.38(2) 60.21(2) 60.54(2) ? Al3 Al1 Al3 1_5545 ? ? 59.25(3) 59.25(3) 59.25(3) ? Al3 Al1 Al3 1_5545 ? 2_5545 120.75(3) 120.47(3) 121.04(3) ? Al3 Al1 Al3 1_5545 ? 2_5555 179.80(12) 179.67(3) 180.0(5) ? Al3 Al1 Al3 ? ? 2_5545 179.80(12) 179.67(3) 180.0(5) ? Al3 Al1 Al3 ? ? 2_5555 120.75(3) 120.47(3) 121.04(3) ? Al3 Al1 Al3 2_5545 ? 2_5555 59.25(3) 59.25(3) 59.25(3) ? Al2 Al2 Al2 1_5545 ? 1_5565 179.461(19) 179.223(19) 179.784(19) ? Al2 Al2 Si2 1_5545 ? ? 0 0 0 ? Al2 Al2 Al3 1_5545 ? ? 90.000(11) 89.881(11) 90.119(11) ? Al2 Al2 Al3 1_5545 ? 3_5565 89.996(10) 89.656(10) 90.343(10) ? Al2 Al2 Al3 1_5545 ? 4_4565 90.003(12) 89.698(12) 90.302(12) ? Al2 Al2 O3 1_5545 ? ? 89.999(11) 89.888(11) 90.112(11) ? Al2 Al2 Si2 1_5565 ? ? 0 0 0 ? Al2 Al2 Al3 1_5565 ? ? 90.000(11) 89.881(11) 90.119(11) ? Al2 Al2 Al3 1_5565 ? 3_5565 89.996(10) 89.656(10) 90.343(10) ? Al2 Al2 Al3 1_5565 ? 4_4565 90.003(12) 89.698(12) 90.302(12) ? Al2 Al2 O3 1_5565 ? ? 89.999(11) 89.888(11) 90.112(11) ? Si2 Al2 Al3 ? ? ? 0 0 0 ? Si2 Al2 Al3 ? ? 3_5565 0 0 0 ? Si2 Al2 Al3 ? ? 4_4565 0 0 0 ? Si2 Al2 O3 ? ? ? 0 0 0 ? Al3 Al2 Al3 ? ? 3_5565 126.87(9) 126.61(9) 127.13(9) ? Al3 Al2 Al3 ? ? 4_4565 123.04(9) 122.90(8) 123.19(8) ? Al3 Al2 O3 ? ? ? 177.09(12) 176.71(12) 177.46(12) ? Al3 Al2 Al3 3_5565 ? 4_4565 110.09(5) 109.91(5) 110.26(5) ? Al3 Al2 O3 3_5565 ? ? 56.04(9) 55.89(9) 56.20(9) ? Al3 Al2 O3 4_4565 ? ? 54.05(9) 53.72(9) 54.37(9) ? Al2 Si2 Al3 ? ? ? 0 0 0 ? Al2 Si2 O3 ? ? ? 0 0 0 ? Al3 Si2 O3 ? ? ? 177.09(12) 176.71(12) 177.46(12) ? Al1 Al3 Al1 ? ? 1_5565 59.25(4) 58.92(4) 59.58(4) ? Al1 Al3 Al2 ? ? ? 88.77(8) 88.67(8) 88.88(8) ? Al1 Al3 Al2 ? ? 3_5465 68.68(4) 68.47(4) 68.88(4) ? Al1 Al3 Al2 ? ? 4_5565 128.07(5) 127.98(5) 128.16(5) ? Al1 Al3 Si2 ? ? ? 88.77(8) 88.67(8) 88.88(8) ? Al1 Al3 Al3 ? ? 1_5545 60.38(4) 60.07(4) 60.68(4) ? Al1 Al3 Al3 ? ? 1_5565 119.63(6) 119.20(6) 120.05(6) ? Al1 Al3 Al2 1_5565 ? ? 88.77(8) 88.67(8) 88.88(8) ? Al1 Al3 Al2 1_5565 ? 3_5465 68.68(4) 68.47(4) 68.88(4) ? Al1 Al3 Al2 1_5565 ? 4_5565 128.07(5) 127.98(5) 128.16(5) ? Al1 Al3 Si2 1_5565 ? ? 88.77(8) 88.67(8) 88.88(8) ? Al1 Al3 Al3 1_5565 ? 1_5545 119.63(6) 119.20(6) 120.05(6) ? Al1 Al3 Al3 1_5565 ? 1_5565 60.38(4) 60.07(4) 60.68(4) ? Al2 Al3 Al2 ? ? 3_5465 153.86(11) 153.71(11) 154.00(11) ? Al2 Al3 Al2 ? ? 4_5565 136.23(10) 136.14(10) 136.33(10) ? Al2 Al3 Si2 ? ? ? 0.0(5) 0.0(5) 0.0(5) ? Al2 Al3 Al3 ? ? 1_5545 90.00(5) 89.85(5) 90.15(5) ? Al2 Al3 Al3 ? ? 1_5565 90.00(5) 89.85(5) 90.15(5) ? Al2 Al3 Al2 3_5465 ? 4_5565 69.91(4) 69.74(4) 70.08(4) ? Al2 Al3 Si2 3_5465 ? ? 153.86(11) 153.71(11) 154.00(11) ? Al2 Al3 Al3 3_5465 ? 1_5545 90.00(5) 89.79(5) 90.21(5) ? Al2 Al3 Al3 3_5465 ? 1_5565 90.00(5) 89.79(5) 90.21(5) ? Al2 Al3 Si2 4_5565 ? ? 136.23(10) 136.14(10) 136.33(10) ? Al2 Al3 Al3 4_5565 ? 1_5545 90.00(5) 89.75(5) 90.25(5) ? Al2 Al3 Al3 4_5565 ? 1_5565 90.00(5) 89.75(5) 90.25(5) ? Si2 Al3 Al3 ? ? 1_5545 90.00(5) 89.85(5) 90.15(5) ? Si2 Al3 Al3 ? ? 1_5565 90.00(5) 89.85(5) 90.15(5) ? Al3 Al3 Al3 1_5545 ? 1_5565 179.50(9) 179.34(8) 179.69(9) ? Al2 O3 Al2 ? ? 2_5655 179.60(14) 179.37(17) 180.0(5) ? Al2 O3 Si2 ? ? ? 0.0(5) 0.0(5) 0.0(5) ? Al2 O3 Si2 ? ? 2_5655 179.60(14) 179.37(17) 180.0(5) ? Al2 O3 O4 ? ? 3_5565 89.8(8) 87.1(9) 92.5(8) ? Al2 O3 O4 ? ? 4_4565 90.2(8) 86.9(9) 93.5(9) ? Al2 O3 Si2 2_5655 ? ? 179.60(14) 179.37(17) 180.0(5) ? Al2 O3 Si2 2_5655 ? 2_5655 0.0(5) 0.0(5) 0.0(5) ? Al2 O3 O4 2_5655 ? 3_5565 90.2(8) 86.9(9) 93.5(9) ? Al2 O3 O4 2_5655 ? 4_4565 89.8(8) 87.1(9) 92.5(8) ? Si2 O3 Si2 ? ? 2_5655 179.60(14) 179.37(17) 180.0(5) ? Si2 O3 O4 ? ? 3_5565 89.8(8) 87.1(9) 92.5(8) ? Si2 O3 O4 ? ? 4_4565 90.2(8) 86.9(9) 93.5(9) ? Si2 O3 O4 2_5655 ? 3_5565 90.2(8) 86.9(9) 93.5(9) ? Si2 O3 O4 2_5655 ? 4_4565 89.8(8) 87.1(9) 92.5(8) ? O4 O3 O4 3_5565 ? 4_4565 176.5(12) 174.6(13) 180.0(5) ? O3 O4 O4 3_5465 ? 2_6555 1.7(6) 0.0(5) 2.8(7) ? data_SA3 _database_code_depnum_ccdc_archive 'CCDC 1843796' _audit_creation_method 'Jana2006 Version : 20/11/2017' _chemical_formula_sum 'Al4.868 O9.566 Si1.132' _chemical_formula_weight 316.2 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Pbam(\a01/2)0ss loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,-x2,x3,x3-x4+1/2 3 -x1+1/2,x2+1/2,-x3,-x4+1/2 4 x1+1/2,-x2+1/2,-x3,-x3+x4 5 -x1,-x2,-x3,-x4 6 x1,x2,-x3,-x3+x4+1/2 7 x1+1/2,-x2+1/2,x3,x4+1/2 8 -x1+1/2,x2+1/2,x3,x3-x4 _cell_length_a 7.5768(13) _cell_length_b 7.6760(16) _cell_length_c 2.8833(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 167.69(8) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.306800 0.000000 0.500000 _cell_formula_units_Z 1 _cell_measurement_reflns_used 982 _cell_measurement_theta_max 31.9 _cell_measurement_theta_min 4.06 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 3.131 _exptl_crystal_F_000 156 _exptl_absorpt_coefficient_mu 1.079 _exptl_crystal_description 'irregularly shaped block' _cell_measurement_temperature 293 _diffrn_ambient_temperature 293 _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device_type 'dectris-CrysAlisPro-abstract goniometer imported dectris images' _diffrn_source synchrotron _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7231 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_detector 'CCD plate' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 3299 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 31.58 _diffrn_reflns_theta_full 23 _diffrn_measured_fraction_theta_full 0.96 _diffrn_measured_fraction_theta_max 0.79 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_unetI/netI 0.0115 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_limit_index_m_1_min -1 _diffrn_reflns_limit_index_m_1_max 1 _reflns_number_total 667 _reflns_number_gt 382 _reflns_threshold_expression I>3\s(I) _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_gt 0.1056 _refine_ls_R_factor_all 0.0423 _refine_ls_wR_factor_ref 0.1105 _refine_ls_goodness_of_fit_ref 1.44 _refine_ls_goodness_of_fit_gt 1.95 _refine_ls_number_reflns 667 _refine_ls_number_parameters 101 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0025000002I^2^) _refine_ls_shift/su_max 0.0001 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_max 0.43 _refine_diff_density_min -0.46 _refine_ls_extinction_method none _refine_ls_number_constraints 33 _refine_ls_structure_factor_coef Fsqd loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al 0.0680 0.0545 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0119 0.0065 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0865 0.0746 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_structure_refinement Jana2006 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 Al1 Al 0 0 0 Uani 0.0089(3) 2 1 d ? ? ? Al2 Al 0.14905(5) 0.34005(5) 0.5 Uani 0.0096(3) 4 0.5 d ? ? ? Si2 Si 0.14905(5) 0.34005(5) 0.5 Uani 0.0096(3) 4 0.283(3) d ? ? ? Al3 Al 0.2624(2) 0.2058(2) 0.5 Uani 0.0105(6) 4 0.217(3) d ? ? ? O1 O 0.35841(11) 0.42165(16) 0.5 Uani 0.0166(4) 4 1 d ? ? ? O2 O 0.12754(11) 0.21837(15) 0 Uani 0.0173(4) 4 1 d ? ? ? O3 O 0 0.5 0.5 Uani 0.017(3) 2 0.349(8) d ? ? ? O4 O 0.4534(10) 0.0482(9) 0.5 Uani 0.0120(19) 4 0.217(3) 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 Al1 Al 0.0128(3) 0.0056(3) 0.0082(7) 0.00085(13) 0 0 Al2 Al 0.0117(4) 0.0073(3) 0.0099(8) -0.00061(13) 0 0 Si2 Si 0.0117(4) 0.0073(3) 0.0099(8) -0.00061(13) 0 0 Al3 Al 0.0131(7) 0.0114(8) 0.0069(16) 0.0008(6) 0 0 O1 O 0.0200(5) 0.0196(5) 0.0101(10) -0.0087(3) 0 0 O2 O 0.0211(4) 0.0125(5) 0.0183(9) -0.0060(3) 0 0 O3 O 0.019(5) 0.008(4) 0.023(4) -0.006(2) 0 0 O4 O 0.011(4) 0.004(3) 0.020(3) -0.0017(17) 0 0 loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 loop_ _jana_atom_site_occ_Fourier_absolute_site_label _jana_atom_site_occ_Fourier_absolute Al2 0.5 Si2 0.283(3) Al3 0.217(3) O3 0.349(8) O4 0.217(3) loop_ _atom_site_occ_Fourier_id _atom_site_occ_Fourier_atom_site_label _atom_site_occ_Fourier_wave_vector_seq_id Al2o1 Al2 1 Si2o1 Si2 1 Al3o1 Al3 1 O3o1 O3 1 O4o1 O4 1 loop_ _atom_site_occ_Fourier_param_id _atom_site_occ_Fourier_param_cos _atom_site_occ_Fourier_param_sin Al2o1 0.0129(2) 0.00382(7) Si2o1 0.0129(2) 0.00382(7) Al3o1 -0.0236(4) -0.0131(2) O3o1 -0.00379(7) 0 O4o1 -0.0173(3) -0.0207(4) 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 Al1x1 Al1 x 1 Al1y1 Al1 y 1 Al1z1 Al1 z 1 Al2x1 Al2 x 1 Al2y1 Al2 y 1 Al2z1 Al2 z 1 Si2x1 Si2 x 1 Si2y1 Si2 y 1 Si2z1 Si2 z 1 Al3x1 Al3 x 1 Al3y1 Al3 y 1 Al3z1 Al3 z 1 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O3x1 O3 x 1 O3y1 O3 y 1 O3z1 O3 z 1 O4x1 O4 x 1 O4y1 O4 y 1 O4z1 O4 z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Al1x1 0 0 Al1y1 0 0 Al1z1 0 -0.00138(8) Al2x1 0.00016(4) -0.00047(4) Al2y1 -0.00008(2) -0.00047(2) Al2z1 0 0 Si2x1 0.00016(4) -0.00047(4) Si2y1 -0.00008(2) -0.00047(2) Si2z1 0 0 Al3x1 0.00049(17) 0.00004(15) Al3y1 0.00029(8) -0.00026(9) Al3z1 0 0 O1x1 -0.00058(8) -0.00072(8) O1y1 0.00129(4) 0.00073(4) O1z1 0 0 O2x1 0 0 O2y1 0 0 O2z1 -0.00207(15) -0.00109(14) O3x1 0 -0.0016(5) O3y1 0 0.0013(3) O3z1 0 0 O4x1 -0.0008(7) 0.0003(5) O4y1 -0.0007(5) -0.0004(3) O4z1 0 0 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 Al1U111 Al1 U11 1 Al1U221 Al1 U22 1 Al1U331 Al1 U33 1 Al1U121 Al1 U12 1 Al1U131 Al1 U13 1 Al1U231 Al1 U23 1 Al2U111 Al2 U11 1 Al2U221 Al2 U22 1 Al2U331 Al2 U33 1 Al2U121 Al2 U12 1 Al2U131 Al2 U13 1 Al2U231 Al2 U23 1 Si2U111 Si2 U11 1 Si2U221 Si2 U22 1 Si2U331 Si2 U33 1 Si2U121 Si2 U12 1 Si2U131 Si2 U13 1 Si2U231 Si2 U23 1 Al3U111 Al3 U11 1 Al3U221 Al3 U22 1 Al3U331 Al3 U33 1 Al3U121 Al3 U12 1 Al3U131 Al3 U13 1 Al3U231 Al3 U23 1 O1U111 O1 U11 1 O1U221 O1 U22 1 O1U331 O1 U33 1 O1U121 O1 U12 1 O1U131 O1 U13 1 O1U231 O1 U23 1 O2U111 O2 U11 1 O2U221 O2 U22 1 O2U331 O2 U33 1 O2U121 O2 U12 1 O2U131 O2 U13 1 O2U231 O2 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 O4U111 O4 U11 1 O4U221 O4 U22 1 O4U331 O4 U33 1 O4U121 O4 U12 1 O4U131 O4 U13 1 O4U231 O4 U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Al1U111 0 0 Al1U221 0 0 Al1U331 0 0 Al1U121 0 0 Al1U131 -0.00009(13) 0 Al1U231 -0.00015(7) 0 Al2U111 -0.00075(16) -0.00015(16) Al2U221 -0.00040(7) 0.00055(8) Al2U331 -0.00002(14) 0.00010(14) Al2U121 -0.00009(9) -0.00007(8) Al2U131 0 0 Al2U231 0 0 Si2U111 -0.00075(16) -0.00015(16) Si2U221 -0.00040(7) 0.00055(8) Si2U331 -0.00002(14) 0.00010(14) Si2U121 -0.00009(9) -0.00007(8) Si2U131 0 0 Si2U231 0 0 Al3U111 0.0035(6) 0.0029(6) Al3U221 0.0020(3) 0.0012(3) Al3U331 0.0003(6) 0.0007(5) Al3U121 0.0005(3) -0.0003(3) Al3U131 0 0 Al3U231 0 0 O1U111 -0.0007(4) -0.0002(3) O1U221 0.00014(17) -0.00003(17) O1U331 0.0002(2) 0.0003(3) O1U121 0.00051(19) 0.00027(18) O1U131 0 0 O1U231 0 0 O2U111 0 0 O2U221 0 0 O2U331 0 0 O2U121 0 0 O2U131 0.0000(2) -0.0002(2) O2U231 -0.00003(14) -0.00012(13) O3U111 0.000(3) 0 O3U221 -0.003(2) 0 O3U331 0.0028(16) 0 O3U121 0 0 O3U131 0 0 O3U231 0 0 O4U111 0.004(2) -0.0012(18) O4U221 0.0032(18) 0.0006(10) O4U331 -0.0005(18) 0.0006(14) O4U121 0 0 O4U131 0 0 O4U231 0 0 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 Al1 Al1 ? 1_5545 2.88330(17) 2.8753(3) 2.8913(3) ? Al1 Al1 ? 1_5565 2.88330(17) 2.8753(3) 2.8913(3) ? Al1 Al3 ? 1_5545 2.9198(19) 2.9170(19) 2.9225(19) ? Al1 Al3 ? ? 2.9197(19) 2.9170(19) 2.9225(19) ? Al1 Al3 ? 2_5545 2.9197(19) 2.9170(19) 2.9225(19) ? Al1 Al3 ? 2_5555 2.9198(19) 2.9170(19) 2.9225(19) ? Al2 Al2 ? 1_5545 2.8833098(16) 2.883301(2) 2.883318(2) ? Al2 Al2 ? 1_5565 2.8833098(16) 2.883301(2) 2.883318(2) ? Al2 Si2 ? ? 0 0 0 ? Al2 Al3 ? ? 1.342(2) 1.341(2) 1.343(2) ? Al2 Al3 ? 3_5565 2.8863(18) 2.8834(18) 2.8891(18) ? Al2 Al3 ? 4_4565 2.951(3) 2.947(3) 2.954(3) ? Al2 O3 ? ? 1.6683(18) 1.653(3) 1.683(3) ? Si2 Al3 ? ? 1.342(2) 1.341(2) 1.343(2) ? Si2 O3 ? ? 1.6683(18) 1.653(3) 1.683(3) ? Al3 Al3 ? 1_5545 2.883308(6) 2.883302(9) 2.883314(9) ? Al3 Al3 ? 1_5565 2.883308(6) 2.883302(9) 2.883314(9) ? O3 O4 ? 3_5565 0.512(8) 0.510(8) 0.514(8) ? O3 O4 ? 4_4565 0.512(8) 0.510(8) 0.514(8) ? O4 O4 ? 2_6555 1.024(11) 1.022(12) 1.025(12) ? 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 Al1 Al1 Al1 1_5545 ? 1_5565 180.0(5) 180.0(5) 180.0(5) ? Al1 Al1 Al3 1_5545 ? 1_5545 60.41(2) 60.31(2) 60.52(2) ? Al1 Al1 Al3 1_5545 ? ? 119.59(2) 119.48(2) 119.69(2) ? Al1 Al1 Al3 1_5545 ? 2_5545 60.41(2) 60.31(2) 60.52(2) ? Al1 Al1 Al3 1_5545 ? 2_5555 119.59(2) 119.48(2) 119.69(2) ? Al1 Al1 Al3 1_5565 ? 1_5545 119.59(2) 119.48(2) 119.69(2) ? Al1 Al1 Al3 1_5565 ? ? 60.41(2) 60.31(2) 60.52(2) ? Al1 Al1 Al3 1_5565 ? 2_5545 119.59(2) 119.48(2) 119.69(2) ? Al1 Al1 Al3 1_5565 ? 2_5555 60.41(2) 60.31(2) 60.52(2) ? Al3 Al1 Al3 1_5545 ? ? 59.18(3) 59.18(3) 59.18(3) ? Al3 Al1 Al3 1_5545 ? 2_5545 120.82(3) 120.62(4) 121.02(3) ? Al3 Al1 Al3 1_5545 ? 2_5555 179.88(16) 179.79(3) 180.0(5) ? Al3 Al1 Al3 ? ? 2_5545 179.88(16) 179.79(3) 180.0(5) ? Al3 Al1 Al3 ? ? 2_5555 120.82(3) 120.62(4) 121.02(3) ? Al3 Al1 Al3 2_5545 ? 2_5555 59.18(3) 59.18(3) 59.18(3) ? Al2 Al2 Al2 1_5545 ? 1_5565 179.72(2) 179.60(2) 179.90(2) ? Al2 Al2 Si2 1_5545 ? ? 0 0 0 ? Al2 Al2 Al3 1_5545 ? ? 90.000(13) 89.947(13) 90.052(13) ? Al2 Al2 Al3 1_5545 ? 3_5565 89.998(12) 89.828(12) 90.172(12) ? Al2 Al2 Al3 1_5545 ? 4_4565 90.002(14) 89.837(13) 90.163(13) ? Al2 Al2 O3 1_5545 ? ? 90.000(13) 89.949(13) 90.051(13) ? Al2 Al2 Si2 1_5565 ? ? 0 0 0 ? Al2 Al2 Al3 1_5565 ? ? 90.000(13) 89.947(13) 90.052(13) ? Al2 Al2 Al3 1_5565 ? 3_5565 89.998(12) 89.828(12) 90.172(12) ? Al2 Al2 Al3 1_5565 ? 4_4565 90.002(14) 89.837(13) 90.163(13) ? Al2 Al2 O3 1_5565 ? ? 90.000(13) 89.949(13) 90.051(13) ? Si2 Al2 Al3 ? ? ? 0 0 0 ? Si2 Al2 Al3 ? ? 3_5565 0 0 0 ? Si2 Al2 Al3 ? ? 4_4565 0 0 0 ? Si2 Al2 O3 ? ? ? 0 0 0 ? Al3 Al2 Al3 ? ? 3_5565 126.76(10) 126.50(10) 127.03(10) ? Al3 Al2 Al3 ? ? 4_4565 122.95(9) 122.65(9) 123.25(9) ? Al3 Al2 O3 ? ? ? 177.19(14) 176.90(14) 177.46(14) ? Al3 Al2 Al3 3_5565 ? 4_4565 110.29(6) 110.26(5) 110.32(5) ? Al3 Al2 O3 3_5565 ? ? 56.05(12) 55.97(12) 56.14(12) ? Al3 Al2 O3 4_4565 ? ? 54.24(12) 54.15(12) 54.32(12) ? Al2 Si2 Al3 ? ? ? 0 0 0 ? Al2 Si2 O3 ? ? ? 0 0 0 ? Al3 Si2 O3 ? ? ? 177.19(14) 176.90(14) 177.46(14) ? Al1 Al3 Al1 ? ? 1_5565 59.18(4) 58.97(4) 59.38(4) ? Al1 Al3 Al2 ? ? ? 88.85(9) 88.64(9) 89.05(9) ? Al1 Al3 Al2 ? ? 3_5465 68.42(4) 68.33(4) 68.51(4) ? Al1 Al3 Al2 ? ? 4_5565 127.70(5) 127.65(5) 127.75(5) ? Al1 Al3 Si2 ? ? ? 88.85(9) 88.64(9) 89.05(9) ? Al1 Al3 Al3 ? ? 1_5545 60.41(4) 60.32(4) 60.51(4) ? Al1 Al3 Al3 ? ? 1_5565 119.59(7) 119.31(7) 119.86(7) ? Al1 Al3 Al2 1_5565 ? ? 88.85(9) 88.64(9) 89.05(9) ? Al1 Al3 Al2 1_5565 ? 3_5465 68.42(4) 68.33(4) 68.51(4) ? Al1 Al3 Al2 1_5565 ? 4_5565 127.70(5) 127.65(5) 127.75(5) ? Al1 Al3 Si2 1_5565 ? ? 88.85(9) 88.64(9) 89.05(9) ? Al1 Al3 Al3 1_5565 ? 1_5545 119.59(7) 119.31(7) 119.86(7) ? Al1 Al3 Al3 1_5565 ? 1_5565 60.41(4) 60.32(4) 60.51(4) ? Al2 Al3 Al2 ? ? 3_5465 153.65(12) 153.45(12) 153.85(12) ? Al2 Al3 Al2 ? ? 4_5565 136.64(11) 136.37(11) 136.91(11) ? Al2 Al3 Si2 ? ? ? 0.0(5) 0.0(5) 0.0(5) ? Al2 Al3 Al3 ? ? 1_5545 90.00(5) 89.93(5) 90.07(5) ? Al2 Al3 Al3 ? ? 1_5565 90.00(5) 89.93(5) 90.07(5) ? Al2 Al3 Al2 3_5465 ? 4_5565 69.71(5) 69.64(5) 69.78(5) ? Al2 Al3 Si2 3_5465 ? ? 153.65(12) 153.45(12) 153.85(12) ? Al2 Al3 Al3 3_5465 ? 1_5545 90.00(5) 89.91(5) 90.09(5) ? Al2 Al3 Al3 3_5465 ? 1_5565 90.00(5) 89.91(5) 90.09(5) ? Al2 Al3 Si2 4_5565 ? ? 136.64(11) 136.37(11) 136.91(11) ? Al2 Al3 Al3 4_5565 ? 1_5545 90.00(6) 89.86(6) 90.14(6) ? Al2 Al3 Al3 4_5565 ? 1_5565 90.00(6) 89.86(6) 90.14(6) ? Si2 Al3 Al3 ? ? 1_5545 90.00(5) 89.93(5) 90.07(5) ? Si2 Al3 Al3 ? ? 1_5565 90.00(5) 89.93(5) 90.07(5) ? Al3 Al3 Al3 1_5545 ? 1_5565 179.74(9) 179.65(10) 179.85(9) ? Al2 O3 Al2 ? ? 2_5655 179.9(2) 179.8(2) 180.0(5) ? Al2 O3 Si2 ? ? ? 0.0(5) 0.0(5) 0.0(5) ? Al2 O3 Si2 ? ? 2_5655 179.9(2) 179.8(2) 180.0(5) ? Al2 O3 O4 ? ? 3_5565 93.7(9) 91.7(9) 95.7(9) ? Al2 O3 O4 ? ? 4_4565 86.3(9) 84.1(9) 88.4(9) ? Al2 O3 Si2 2_5655 ? ? 179.9(2) 179.8(2) 180.0(5) ? Al2 O3 Si2 2_5655 ? 2_5655 0.0(5) 0.0(5) 0.0(5) ? Al2 O3 O4 2_5655 ? 3_5565 86.3(9) 84.1(9) 88.4(9) ? Al2 O3 O4 2_5655 ? 4_4565 93.7(9) 91.7(9) 95.7(9) ? Si2 O3 Si2 ? ? 2_5655 179.9(2) 179.8(2) 180.0(5) ? Si2 O3 O4 ? ? 3_5565 93.7(9) 91.7(9) 95.7(9) ? Si2 O3 O4 ? ? 4_4565 86.3(9) 84.1(9) 88.4(9) ? Si2 O3 O4 2_5655 ? 3_5565 86.3(9) 84.1(9) 88.4(9) ? Si2 O3 O4 2_5655 ? 4_4565 93.7(9) 91.7(9) 95.7(9) ? O4 O3 O4 3_5565 ? 4_4565 177.6(13) 176.3(14) 180.0(5) ? O3 O4 O4 3_5465 ? 2_6555 1.2(7) 0.0(5) 1.9(7) ? data_QG _database_code_depnum_ccdc_archive 'CCDC 1843797' _chemical_name_common Mullite _chemical_formula_sum 'Al4.853 O9.574 Si1.147' _chemical_formula_weight 316.3 _chemical_compound_source 'Sigma Aldrich' _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Pbam(\a01/2)0ss loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,-x2,x3,x3-x4+1/2 3 -x1+1/2,x2+1/2,-x3,-x4+1/2 4 x1+1/2,-x2+1/2,-x3,-x3+x4 5 -x1,-x2,-x3,-x4 6 x1,x2,-x3,-x3+x4+1/2 7 x1+1/2,-x2+1/2,x3,x4+1/2 8 -x1+1/2,x2+1/2,x3,x3-x4 _cell_length_a 7.577(2) _cell_length_b 7.6738(19) _cell_length_c 2.8823(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 167.59(8) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.294800 0.000000 0.500000 _cell_formula_units_Z 1 _cell_measurement_reflns_used 1039 _cell_measurement_theta_min 4.07 _cell_measurement_theta_max 31.8 _cell_measurement_temperature 293 _exptl_crystal_density_diffrn 3.1343 _exptl_crystal_F_000 156 _exptl_absorpt_coefficient_mu 1.08 _exptl_crystal_description 'irregularly shaped block' _exptl_crystal_size_rad 0.05 _exptl_crystal_colour colorless _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_type_of_structure mod _exptl_absorpt_correction_T_min 0.569 _exptl_absorpt_correction_T_max 1 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? _diffrn_ambient_temperature 293 _diffrn_source synchrotron _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7231 _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'dectris-CrysAlisPro-abstract goniometer imported dectris images' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.8 _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'polymer loop' _diffrn_reflns_number 3576 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 31.93 _diffrn_reflns_theta_full 27.35 _diffrn_measured_fraction_theta_max 0.91 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_av_unetI/netI 0.0087 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_limit_index_m_1_min -1 _diffrn_reflns_limit_index_m_1_max 1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 797 _reflns_number_gt 454 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_gt 0.0916 _refine_ls_R_factor_all 0.0310 _refine_ls_wR_factor_ref 0.0971 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_goodness_of_fit_gt 1.37 _refine_ls_number_reflns 797 _refine_ls_number_parameters 101 _refine_ls_number_constraints 33 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0035999999I^2^) _refine_ls_shift/su_max 0.0006 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_max 0.28 _refine_diff_density_min -0.30 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al 0.0680 0.0545 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0119 0.0065 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0865 0.0746 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_structure_refinement Jana2006 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 Al1 Al 0 0 0 Uani 0.01054(17) 2 1 d ? ? ? Al2 Al 0.14908(4) 0.33987(4) 0.5 Uani 0.01046(17) 4 0.5 d ? ? ? Si2 Si 0.14908(4) 0.33987(4) 0.5 Uani 0.01046(17) 4 0.2868(17) d ? ? ? Al3 Al 0.26226(19) 0.2054(2) 0.5 Uani 0.0121(4) 4 0.2132(17) d ? ? ? O1 O 0.35879(9) 0.42178(11) 0.5 Uani 0.0165(3) 4 1 d ? ? ? O2 O 0.12793(9) 0.21778(13) 0 Uani 0.0173(2) 4 1 d ? ? ? O3 O 0 0.5 0.5 Uani 0.021(2) 2 0.360(5) d ? ? ? O4 O 0.4543(9) 0.0499(8) 0.5 Uani 0.0124(16) 4 0.2132(17) 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 Al1 Al 0.0128(3) 0.0098(3) 0.0090(3) 0.00056(12) 0 0 Al2 Al 0.0118(3) 0.0096(3) 0.0100(3) -0.00058(10) 0 0 Si2 Si 0.0118(3) 0.0096(3) 0.0100(3) -0.00058(10) 0 0 Al3 Al 0.0133(6) 0.0120(7) 0.0110(7) 0.0002(5) 0 0 O1 O 0.0193(4) 0.0201(4) 0.0099(5) -0.0076(3) 0 0 O2 O 0.0208(3) 0.0155(4) 0.0155(4) -0.0062(3) 0 0 O3 O 0.020(4) 0.017(4) 0.026(2) -0.0076(18) 0 0 O4 O 0.015(3) 0.006(3) 0.0159(18) -0.0020(17) 0 0 loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 loop_ _jana_atom_site_occ_Fourier_absolute_site_label _jana_atom_site_occ_Fourier_absolute Al2 0.5 Si2 0.2868(17) Al3 0.2132(17) O3 0.360(5) O4 0.2132(17) loop_ _atom_site_occ_Fourier_id _atom_site_occ_Fourier_atom_site_label _atom_site_occ_Fourier_wave_vector_seq_id Al2o1 Al2 1 Si2o1 Si2 1 Al3o1 Al3 1 O3o1 O3 1 O4o1 O4 1 loop_ _atom_site_occ_Fourier_param_id _atom_site_occ_Fourier_param_cos _atom_site_occ_Fourier_param_sin Al2o1 0.0197(2) 0.00558(7) Si2o1 0.0197(2) 0.00558(7) Al3o1 -0.0362(5) -0.0191(2) O3o1 -0.00826(10) 0 O4o1 -0.0273(3) -0.0305(4) 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 Al1x1 Al1 x 1 Al1y1 Al1 y 1 Al1z1 Al1 z 1 Al2x1 Al2 x 1 Al2y1 Al2 y 1 Al2z1 Al2 z 1 Si2x1 Si2 x 1 Si2y1 Si2 y 1 Si2z1 Si2 z 1 Al3x1 Al3 x 1 Al3y1 Al3 y 1 Al3z1 Al3 z 1 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O3x1 O3 x 1 O3y1 O3 y 1 O3z1 O3 z 1 O4x1 O4 x 1 O4y1 O4 y 1 O4z1 O4 z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Al1x1 0 0 Al1y1 0 0 Al1z1 0 -0.00201(9) Al2x1 0.00021(3) -0.00054(3) Al2y1 -0.00012(3) -0.00065(3) Al2z1 0 0 Si2x1 0.00021(3) -0.00054(3) Si2y1 -0.00012(3) -0.00065(3) Si2z1 0 0 Al3x1 0.00049(14) -0.00035(13) Al3y1 0.00016(13) -0.00060(12) Al3z1 0 0 O1x1 -0.00079(6) -0.00104(7) O1y1 0.00171(6) 0.00088(6) O1z1 0 0 O2x1 0 0 O2y1 0 0 O2z1 -0.00271(14) -0.00114(14) O3x1 0 -0.0007(5) O3y1 0 0.0008(5) O3z1 0 0 O4x1 0.0007(8) 0.0012(5) O4y1 0.0004(8) 0.0002(4) O4z1 0 0 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 Al1U111 Al1 U11 1 Al1U221 Al1 U22 1 Al1U331 Al1 U33 1 Al1U121 Al1 U12 1 Al1U131 Al1 U13 1 Al1U231 Al1 U23 1 Al2U111 Al2 U11 1 Al2U221 Al2 U22 1 Al2U331 Al2 U33 1 Al2U121 Al2 U12 1 Al2U131 Al2 U13 1 Al2U231 Al2 U23 1 Si2U111 Si2 U11 1 Si2U221 Si2 U22 1 Si2U331 Si2 U33 1 Si2U121 Si2 U12 1 Si2U131 Si2 U13 1 Si2U231 Si2 U23 1 Al3U111 Al3 U11 1 Al3U221 Al3 U22 1 Al3U331 Al3 U33 1 Al3U121 Al3 U12 1 Al3U131 Al3 U13 1 Al3U231 Al3 U23 1 O1U111 O1 U11 1 O1U221 O1 U22 1 O1U331 O1 U33 1 O1U121 O1 U12 1 O1U131 O1 U13 1 O1U231 O1 U23 1 O2U111 O2 U11 1 O2U221 O2 U22 1 O2U331 O2 U33 1 O2U121 O2 U12 1 O2U131 O2 U13 1 O2U231 O2 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 O4U111 O4 U11 1 O4U221 O4 U22 1 O4U331 O4 U33 1 O4U121 O4 U12 1 O4U131 O4 U13 1 O4U231 O4 U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Al1U111 0 0 Al1U221 0 0 Al1U331 0 0 Al1U121 0 0 Al1U131 0.00009(11) 0 Al1U231 -0.00009(10) 0 Al2U111 -0.00037(13) 0.00007(12) Al2U221 -0.00059(11) 0.00067(13) Al2U331 0.00003(12) 0.00017(12) Al2U121 0.00001(10) -0.00014(10) Al2U131 0 0 Al2U231 0 0 Si2U111 -0.00037(13) 0.00007(12) Si2U221 -0.00059(11) 0.00067(13) Si2U331 0.00003(12) 0.00017(12) Si2U121 0.00001(10) -0.00014(10) Si2U131 0 0 Si2U231 0 0 Al3U111 0.0019(5) 0.0013(5) Al3U221 0.0026(5) 0.0018(5) Al3U331 0.0008(5) 0.0007(4) Al3U121 0.0010(4) -0.0005(4) Al3U131 0 0 Al3U231 0 0 O1U111 -0.0008(3) -0.0003(3) O1U221 0.0002(3) 0.0001(3) O1U331 0.0000(2) 0.0001(2) O1U121 0.0005(2) 0.0000(2) O1U131 0 0 O1U231 0 0 O2U111 0 0 O2U221 0 0 O2U331 0 0 O2U121 0 0 O2U131 -0.00012(19) -0.00023(19) O2U231 -0.0003(2) 0.00015(19) O3U111 -0.003(3) 0 O3U221 0.002(4) 0 O3U331 0.0015(17) 0 O3U121 0 0 O3U131 0 0 O3U231 0 0 O4U111 0.005(3) 0.0009(19) O4U221 0.000(3) -0.0002(15) O4U331 -0.0012(16) 0.0002(13) O4U121 0 0 O4U131 0 0 O4U231 0 0 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 Al1 O1 ? 3_5455 1.8926(7) 1.8890(7) 1.8964(7) ? Al1 O1 ? 3_5465 1.8927(7) 1.8890(7) 1.8964(7) ? Al1 O1 ? 4_4555 1.8927(7) 1.8890(7) 1.8964(7) ? Al1 O1 ? 4_4565 1.8926(7) 1.8890(7) 1.8964(7) ? Al1 O2 ? ? 1.9320(10) 1.9320(10) 1.9320(10) ? Al1 O2 ? 2_5555 1.9320(10) 1.9320(10) 1.9320(10) ? Al2 O1 ? ? 1.7089(14) 1.7050(14) 1.7129(14) ? Al2 O2 ? ? 1.7264(7) 1.7217(7) 1.7311(7) ? Al2 O2 ? 1_5565 1.7264(7) 1.7217(7) 1.7311(7) ? Al2 O3 ? ? 1.669(2) 1.661(4) 1.677(4) ? Al2 O4 ? 3_5565 1.792(8) 1.784(9) 1.801(9) ? Al2 O4 ? 4_4565 1.701(8) 1.691(9) 1.711(9) ? Si2 O1 ? ? 1.7089(14) 1.7050(14) 1.7129(14) ? Si2 O2 ? ? 1.7264(7) 1.7217(7) 1.7311(7) ? Si2 O2 ? 1_5565 1.7264(7) 1.7217(7) 1.7311(7) ? Si2 O3 ? ? 1.669(2) 1.661(4) 1.677(4) ? Si2 O4 ? 3_5565 1.792(8) 1.784(9) 1.801(9) ? Si2 O4 ? 4_4565 1.701(8) 1.691(9) 1.711(9) ? Al3 O1 ? ? 1.815(2) 1.805(2) 1.825(2) ? Al3 O2 ? ? 1.7670(12) 1.7622(12) 1.7717(12) ? Al3 O2 ? 1_5565 1.7670(12) 1.7622(12) 1.7717(12) ? Al3 O4 ? ? 1.881(8) 1.877(9) 1.886(9) ? 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 O1 Al1 O1 3_5455 ? 3_5465 99.19(4) 99.19(4) 99.19(4) ? O1 Al1 O1 3_5455 ? 4_4555 80.81(4) 80.49(4) 81.14(4) ? O1 Al1 O1 3_5455 ? 4_4565 179.52(7) 179.24(4) 180.0(5) ? O1 Al1 O2 3_5455 ? ? 89.47(3) 88.98(3) 89.96(4) ? O1 Al1 O2 3_5455 ? 2_5555 90.53(3) 90.21(3) 90.85(3) ? O1 Al1 O1 3_5465 ? 4_4555 179.52(7) 179.24(4) 180.0(5) ? O1 Al1 O1 3_5465 ? 4_4565 80.81(4) 80.49(4) 81.14(4) ? O1 Al1 O2 3_5465 ? ? 89.47(3) 88.98(3) 89.96(4) ? O1 Al1 O2 3_5465 ? 2_5555 90.53(3) 90.21(3) 90.85(3) ? O1 Al1 O1 4_4555 ? 4_4565 99.19(4) 99.19(4) 99.19(4) ? O1 Al1 O2 4_4555 ? ? 90.53(3) 90.21(3) 90.85(3) ? O1 Al1 O2 4_4555 ? 2_5555 89.47(3) 88.98(3) 89.96(4) ? O1 Al1 O2 4_4565 ? ? 90.53(3) 90.21(3) 90.85(3) ? O1 Al1 O2 4_4565 ? 2_5555 89.47(3) 88.98(3) 89.96(4) ? O2 Al1 O2 ? ? 2_5555 179.85(13) 179.74(2) 180.0(5) ? O1 Al2 O2 ? ? ? 106.61(3) 106.22(3) 107.01(3) ? O1 Al2 O2 ? ? 1_5565 106.61(3) 106.22(3) 107.01(3) ? O1 Al2 O3 ? ? ? 111.00(14) 110.27(14) 111.74(14) ? O1 Al2 O4 ? ? 3_5565 94.3(2) 93.6(2) 95.1(2) ? O1 Al2 O4 ? ? 4_4565 128.6(2) 127.9(2) 129.3(2) ? O2 Al2 O2 ? ? 1_5565 113.19(5) 112.59(5) 113.79(5) ? O2 Al2 O3 ? ? ? 109.68(7) 109.63(7) 109.72(7) ? O2 Al2 O4 ? ? 3_5565 116.59(9) 116.42(9) 116.76(9) ? O2 Al2 O4 ? ? 4_4565 100.91(13) 100.82(13) 100.99(13) ? O2 Al2 O3 1_5565 ? ? 109.68(7) 109.63(7) 109.72(7) ? O2 Al2 O4 1_5565 ? 3_5565 116.59(9) 116.42(9) 116.76(9) ? O2 Al2 O4 1_5565 ? 4_4565 100.91(13) 100.82(13) 100.99(13) ? O3 Al2 O4 ? ? 3_5565 16.7(3) 16.4(3) 17.0(3) ? O3 Al2 O4 ? ? 4_4565 17.6(3) 17.5(3) 17.7(3) ? O4 Al2 O4 3_5565 ? 4_4565 34.3(4) 34.1(3) 34.4(3) ? O1 Si2 O2 ? ? ? 106.61(3) 106.22(3) 107.01(3) ? O1 Si2 O2 ? ? 1_5565 106.61(3) 106.22(3) 107.01(3) ? O1 Si2 O3 ? ? ? 111.00(14) 110.27(14) 111.74(14) ? O1 Si2 O4 ? ? 3_5565 94.3(2) 93.6(2) 95.1(2) ? O1 Si2 O4 ? ? 4_4565 128.6(2) 127.9(2) 129.3(2) ? O2 Si2 O2 ? ? 1_5565 113.19(5) 112.59(5) 113.79(5) ? O2 Si2 O3 ? ? ? 109.68(7) 109.63(7) 109.72(7) ? O2 Si2 O4 ? ? 3_5565 116.59(9) 116.42(9) 116.76(9) ? O2 Si2 O4 ? ? 4_4565 100.91(13) 100.82(13) 100.99(13) ? O2 Si2 O3 1_5565 ? ? 109.68(7) 109.63(7) 109.72(7) ? O2 Si2 O4 1_5565 ? 3_5565 116.59(9) 116.42(9) 116.76(9) ? O2 Si2 O4 1_5565 ? 4_4565 100.91(13) 100.82(13) 100.99(13) ? O3 Si2 O4 ? ? 3_5565 16.7(3) 16.4(3) 17.0(3) ? O3 Si2 O4 ? ? 4_4565 17.6(3) 17.5(3) 17.7(3) ? O4 Si2 O4 3_5565 ? 4_4565 34.3(4) 34.1(3) 34.4(3) ? O1 Al3 O2 ? ? ? 100.53(8) 100.16(8) 100.90(8) ? O1 Al3 O2 ? ? 1_5565 100.53(8) 100.16(8) 100.90(8) ? O1 Al3 O4 ? ? ? 105.6(2) 105.2(2) 105.9(2) ? O2 Al3 O2 ? ? 1_5565 109.30(10) 108.77(10) 109.83(10) ? O2 Al3 O4 ? ? ? 118.67(11) 118.49(11) 118.85(11) ? O2 Al3 O4 1_5565 ? ? 118.67(11) 118.49(11) 118.85(11) ? Al1 O1 Al1 3_5555 ? 3_5565 99.18(5) 98.83(5) 99.54(5) ? Al1 O1 Al2 3_5555 ? ? 129.96(2) 129.75(2) 130.17(2) ? Al1 O1 Si2 3_5555 ? ? 129.96(2) 129.75(2) 130.17(2) ? Al1 O1 Al3 3_5555 ? ? 121.20(4) 120.54(4) 121.86(4) ? Al1 O1 Al2 3_5565 ? ? 129.96(2) 129.75(2) 130.17(2) ? Al1 O1 Si2 3_5565 ? ? 129.96(2) 129.75(2) 130.17(2) ? Al1 O1 Al3 3_5565 ? ? 121.20(4) 120.54(4) 121.86(4) ? Al2 O1 Si2 ? ? ? 0.0(5) 0.0(5) 0.0(5) ? Al2 O1 Al3 ? ? ? 44.65(6) 44.52(6) 44.77(6) ? Si2 O1 Al3 ? ? ? 44.65(6) 44.52(6) 44.77(6) ? Al1 O2 Al2 ? ? 1_5545 121.07(3) 120.48(3) 121.64(3) ? Al1 O2 Al2 ? ? ? 121.06(3) 120.48(3) 121.64(3) ? Al1 O2 Si2 ? ? 1_5545 121.07(3) 120.48(3) 121.64(3) ? Al1 O2 Si2 ? ? ? 121.06(3) 120.48(3) 121.64(3) ? Al1 O2 Al3 ? ? 1_5545 104.03(7) 103.56(7) 104.48(7) ? Al1 O2 Al3 ? ? ? 104.02(7) 103.56(7) 104.48(7) ? Al2 O2 Al2 1_5545 ? ? 113.19(6) 113.19(6) 113.19(6) ? Al2 O2 Si2 1_5545 ? 1_5545 0.0(5) 0.0(5) 0.0(5) ? Al2 O2 Si2 1_5545 ? ? 113.19(6) 113.19(6) 113.19(6) ? Al2 O2 Al3 1_5545 ? 1_5545 45.17(6) 45.05(6) 45.28(6) ? Al2 O2 Al3 1_5545 ? ? 131.05(7) 131.01(7) 131.09(7) ? Al2 O2 Si2 ? ? 1_5545 113.19(6) 113.19(6) 113.19(6) ? Al2 O2 Si2 ? ? ? 0.0(5) 0.0(5) 0.0(5) ? Al2 O2 Al3 ? ? 1_5545 131.05(7) 131.01(7) 131.09(7) ? Al2 O2 Al3 ? ? ? 45.17(6) 45.05(6) 45.28(6) ? Si2 O2 Si2 1_5545 ? ? 113.19(6) 113.19(6) 113.19(6) ? Si2 O2 Al3 1_5545 ? 1_5545 45.17(6) 45.05(6) 45.28(6) ? Si2 O2 Al3 1_5545 ? ? 131.05(7) 131.01(7) 131.09(7) ? Si2 O2 Al3 ? ? 1_5545 131.05(7) 131.01(7) 131.09(7) ? Si2 O2 Al3 ? ? ? 45.17(6) 45.05(6) 45.28(6) ? Al3 O2 Al3 1_5545 ? ? 109.30(8) 109.30(8) 109.30(8) ? Al2 O3 Al2 ? ? 2_5655 179.71(19) 179.5(3) 180.0(5) ? Al2 O3 Si2 ? ? ? 0.0(5) 0.0(5) 0.0(5) ? Al2 O3 Si2 ? ? 2_5655 179.71(19) 179.5(3) 180.0(5) ? Al2 O3 Si2 2_5655 ? ? 179.71(19) 179.5(3) 180.0(5) ? Al2 O3 Si2 2_5655 ? 2_5655 0.0(5) 0.0(5) 0.0(5) ? Si2 O3 Si2 ? ? 2_5655 179.71(19) 179.5(3) 180.0(5) ? Al2 O4 Al2 3_5465 ? 4_5565 145.7(5) 145.7(5) 145.8(5) ? Al2 O4 Si2 3_5465 ? 3_5465 0.0(5) 0.0(5) 0.0(5) ? Al2 O4 Si2 3_5465 ? 4_5565 145.7(5) 145.7(5) 145.8(5) ? Al2 O4 Al3 3_5465 ? ? 103.4(4) 103.0(4) 103.8(4) ? Al2 O4 Si2 4_5565 ? 3_5465 145.7(5) 145.7(5) 145.8(5) ? Al2 O4 Si2 4_5565 ? 4_5565 0.0(5) 0.0(5) 0.0(5) ? Al2 O4 Al3 4_5565 ? ? 110.8(4) 110.4(4) 111.3(4) ? Si2 O4 Si2 3_5465 ? 4_5565 145.7(5) 145.7(5) 145.8(5) ? Si2 O4 Al3 3_5465 ? ? 103.4(4) 103.0(4) 103.8(4) ? Si2 O4 Al3 4_5565 ? ? 110.8(4) 110.4(4) 111.3(4) ?