data_bohseite _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al2 H2 Be2 Ca4 O28 Si9' _chemical_formula_weight 935.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Be' 'Be' 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 63 _space_group_name_H-M_alt 'C m c m' _space_group_name_Hall '-C 2c 2' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 23.204(6) _cell_length_b 4.9442(9) _cell_length_c 19.418(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2227.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1720 _cell_measurement_theta_min 4 _cell_measurement_theta_max 60 _exptl_crystal_description Anhedral _exptl_crystal_colour White _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.788 _exptl_crystal_F_000 1864 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 55 microns _exptl_crystal_size_mid 25 microns _exptl_crystal_size_min 10 microns _exptl_absorpt_coefficient_mu 1.675 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type Rotating-anode 3-crcle diffractometer _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12244 _diffrn_reflns_av_unetI/netI 0.0152 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.098 _diffrn_reflns_theta_max 30.038 _diffrn_reflns_theta_full 2.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.000 _reflns_number_total 1709 _reflns_number_gt 1532 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ATOMS _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+6.8857P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1709 _refine_ls_number_parameters 126 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.08134(2) 0.26204(7) 0.15444(2) 0.01150(11) Uani 0.980(2) 1 d . . P . . T1 Si 0.0000 0.77189(17) 0.2500 0.0060(3) Uani 0.970(5) 4 d S T . . . T2 Be 0.12393(12) 0.8292(6) 0.2500 0.0094(9) Uani 0.992(17) 2 d S T . . . T3S Si 0.0000 0.7180(3) 0.39642(7) 0.0086(5) Uani 0.255(5) 2 d S T P . . T3B Be 0.0000 0.7180(3) 0.39642(7) 0.0086(5) Uani 0.745(5) 2 d S T P . . T4 Al 0.09241(3) 0.5000 0.0000 0.00502(19) Uani 0.997(4) 2 d S T . . . T5 Si 0.17013(3) 0.0000 0.0000 0.00883(13) Uani 1 2 d S T P . . T6 Si 0.21379(2) 0.86856(9) 0.14481(2) 0.00789(11) Uani 1 1 d . . . . . O1 O 0.0000 0.5755(3) 0.18179(8) 0.0091(3) Uani 1 2 d S T P . . O2 O 0.0000 0.0370(3) 0.10746(9) 0.0123(3) Uani 1 2 d DS T P . . O3 O 0.05770(5) 0.5939(3) 0.06791(6) 0.0147(2) Uani 1 1 d . . . . . O4 O 0.13069(5) 0.2439(2) 0.03214(6) 0.0139(2) Uani 1 1 d . . . . . O5 O 0.20837(5) 0.8794(3) 0.06143(6) 0.0135(2) Uani 1 1 d . . . . . O6 O 0.23274(5) 0.5644(2) 0.16632(6) 0.0115(2) Uani 1 1 d . . . . . O7 O 0.15423(5) 0.9478(2) 0.18036(6) 0.0121(2) Uani 1 1 d . . . . . O8 O 0.12132(7) 0.4998(3) 0.2500 0.0115(3) Uani 1 2 d DS T P . . O9 O 0.05769(6) 0.9610(3) 0.2500 0.0087(3) Uani 1 2 d S T P . . H8 H 0.1614(6) 0.437(8) 0.2500 0.059(14) Uiso 1 2 d DS . P . . H2 H 0.0000 0.100(10) 0.0596(9) 0.07(2) Uiso 0.745(5) 2 d DS . P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.01086(16) 0.01389(18) 0.00976(16) 0.00148(12) -0.00057(10) -0.00077(11) T1 0.0046(4) 0.0071(4) 0.0063(4) 0.000 0.000 0.000 T2 0.0078(14) 0.0103(14) 0.0100(14) 0.000 0.000 -0.0001(10) T3S 0.0080(7) 0.0107(8) 0.0070(7) -0.0005(5) 0.000 0.000 T3B 0.0080(7) 0.0107(8) 0.0070(7) -0.0005(5) 0.000 0.000 T4 0.0055(3) 0.0059(3) 0.0036(3) 0.0004(2) 0.000 0.000 T5 0.0085(3) 0.0104(3) 0.0075(3) -0.0004(2) 0.000 0.000 T6 0.00714(19) 0.0091(2) 0.00740(19) 0.00071(15) 0.00081(14) 0.00036(14) O1 0.0103(7) 0.0097(7) 0.0073(7) -0.0007(6) 0.000 0.000 O2 0.0123(7) 0.0099(7) 0.0147(8) 0.0007(6) 0.000 0.000 O3 0.0140(5) 0.0170(6) 0.0131(6) 0.0013(5) 0.0046(4) 0.0045(4) O4 0.0132(5) 0.0151(6) 0.0132(5) -0.0014(5) 0.0005(4) 0.0038(4) O5 0.0137(5) 0.0186(6) 0.0081(5) 0.0009(4) -0.0003(4) 0.0028(5) O6 0.0114(5) 0.0103(5) 0.0129(5) 0.0015(4) 0.0023(4) 0.0019(4) O7 0.0100(5) 0.0144(6) 0.0118(5) 0.0026(4) 0.0036(4) 0.0029(4) O8 0.0087(7) 0.0099(7) 0.0158(7) 0.000 0.000 -0.0002(6) O9 0.0063(7) 0.0092(7) 0.0106(7) 0.000 0.000 -0.0007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca O7 2.3509(12) 1_545 ? Ca O2 2.3733(12) . ? Ca O8 2.3844(11) . ? Ca O3 2.4115(13) . ? Ca O9 2.4414(12) 1_545 ? Ca O1 2.4993(12) . ? Ca O4 2.6380(13) . ? Ca T2 3.000(2) 1_545 ? Ca T3B 3.1016(13) 10_556 ? Ca T3S 3.1016(13) 10_556 ? Ca T4 3.2316(8) . ? Ca T3B 3.4311(14) 10_546 ? Ca H8 2.76(2) . ? Ca H2 2.75(3) . ? T1 O9 1.6328(16) . ? T1 O9 1.6328(16) 3 ? T1 O1 1.6422(16) . ? T1 O1 1.6422(16) 10_556 ? T1 Ca 3.5887(8) 10_566 ? T1 Ca 3.5887(8) 1_565 ? T1 Ca 3.5887(8) 3_565 ? T1 Ca 3.5887(8) 12_565 ? T2 O8 1.630(3) . ? T2 O7 1.633(2) 10_556 ? T2 O7 1.633(2) . ? T2 O9 1.669(3) . ? T2 Ca 3.000(2) 10_566 ? T2 Ca 3.000(2) 1_565 ? T2 Ca 3.505(3) 10_556 ? T3S O2 1.579(2) 10_566 ? T3S O3 1.6275(15) 10_556 ? T3S O3 1.6275(15) 3 ? T3S O1 1.674(2) 10_556 ? T3S Ca 3.1016(13) 3 ? T3S Ca 3.1016(13) 10_556 ? T3S Ca 3.4311(14) 10_566 ? T3S Ca 3.4311(14) 3_565 ? T4 O3 1.6133(12) . ? T4 O3 1.6134(12) 4_565 ? T4 O4 1.6679(13) . ? T4 O4 1.6679(13) 4_565 ? T4 Ca 3.2316(8) 4_565 ? T5 O5 1.6017(12) 1_545 ? T5 O5 1.6017(12) 4_565 ? T5 O4 1.6374(12) 4 ? T5 O4 1.6374(12) . ? T6 O7 1.5938(12) . ? T6 O6 1.6216(13) . ? T6 O5 1.6248(13) . ? T6 O6 1.6284(12) 16 ? O1 T3B 1.674(2) 10_556 ? O1 T3S 1.674(2) 10_556 ? O1 Ca 2.4993(12) 12 ? O2 T3B 1.579(2) 10_546 ? O2 T3S 1.579(2) 10_546 ? O2 Ca 2.3733(12) 12 ? O2 H2 0.9799(11) . ? O3 T3B 1.6276(14) 10_556 ? O3 T3S 1.6276(14) 10_556 ? O5 T5 1.6017(12) 1_565 ? O6 T6 1.6283(12) 16_545 ? O7 Ca 2.3510(12) 1_565 ? O8 Ca 2.3845(11) 10_556 ? O8 H8 0.9799(11) . ? O9 Ca 2.4415(11) 10_566 ? O9 Ca 2.4415(11) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Ca O2 110.16(5) 1_545 . ? O7 Ca O8 83.06(5) 1_545 . ? O2 Ca O8 147.10(5) . . ? O7 Ca O3 139.67(4) 1_545 . ? O2 Ca O3 82.55(5) . . ? O8 Ca O3 107.18(5) . . ? O7 Ca O9 66.17(5) 1_545 1_545 ? O2 Ca O9 80.07(5) . 1_545 ? O8 Ca O9 78.26(5) . 1_545 ? O3 Ca O9 153.29(5) . 1_545 ? O7 Ca O1 155.16(5) 1_545 . ? O2 Ca O1 76.82(5) . . ? O8 Ca O1 79.79(5) . . ? O3 Ca O1 63.54(5) . . ? O9 Ca O1 92.69(5) 1_545 . ? O7 Ca O4 81.84(4) 1_545 . ? O2 Ca O4 89.04(5) . . ? O8 Ca O4 123.26(5) . . ? O3 Ca O4 59.65(4) . . ? O9 Ca O4 139.55(5) 1_545 . ? O1 Ca O4 122.70(5) . . ? O7 Ca T2 32.78(5) 1_545 1_545 ? O2 Ca T2 99.51(7) . 1_545 ? O8 Ca T2 75.05(6) . 1_545 ? O3 Ca T2 172.39(5) . 1_545 ? O9 Ca T2 33.79(6) 1_545 1_545 ? O1 Ca T2 124.03(6) . 1_545 ? O4 Ca T2 112.93(5) . 1_545 ? O7 Ca T3B 170.48(4) 1_545 10_556 ? O2 Ca T3B 74.60(5) . 10_556 ? O8 Ca T3B 97.25(5) . 10_556 ? O3 Ca T3B 31.27(4) . 10_556 ? O9 Ca T3B 123.26(4) 1_545 10_556 ? O1 Ca T3B 32.59(4) . 10_556 ? O4 Ca T3B 90.13(4) . 10_556 ? T2 Ca T3B 156.34(5) 1_545 10_556 ? O7 Ca T3S 170.48(4) 1_545 10_556 ? O2 Ca T3S 74.60(5) . 10_556 ? O8 Ca T3S 97.25(5) . 10_556 ? O3 Ca T3S 31.27(4) . 10_556 ? O9 Ca T3S 123.26(4) 1_545 10_556 ? O1 Ca T3S 32.59(4) . 10_556 ? O4 Ca T3S 90.13(4) . 10_556 ? T2 Ca T3S 156.34(5) 1_545 10_556 ? T3B Ca T3S 0.00(6) 10_556 10_556 ? O7 Ca T4 112.46(3) 1_545 . ? O2 Ca T4 82.95(4) . . ? O8 Ca T4 120.78(4) . . ? O3 Ca T4 28.82(3) . . ? O9 Ca T4 160.94(3) 1_545 . ? O1 Ca T4 91.80(4) . . ? O4 Ca T4 30.96(3) . . ? T2 Ca T4 143.86(4) 1_545 . ? T3B Ca T4 59.22(3) 10_556 . ? T3S Ca T4 59.22(3) 10_556 . ? O7 Ca T3B 86.52(4) 1_545 10_546 ? O2 Ca T3B 23.70(4) . 10_546 ? O8 Ca T3B 145.53(4) . 10_546 ? O3 Ca T3B 101.99(4) . 10_546 ? O9 Ca T3B 67.49(4) 1_545 10_546 ? O1 Ca T3B 97.58(4) . 10_546 ? O4 Ca T3B 87.30(4) . 10_546 ? T2 Ca T3B 78.46(6) 1_545 10_546 ? T3B Ca T3B 98.25(3) 10_556 10_546 ? T3S Ca T3B 98.25(3) 10_556 10_546 ? T4 Ca T3B 93.55(3) . 10_546 ? O7 Ca H8 65.2(6) 1_545 . ? O2 Ca H8 159.9(6) . . ? O8 Ca H8 20.3(3) . . ? O3 Ca H8 114.0(8) . . ? O9 Ca H8 80.3(7) 1_545 . ? O1 Ca H8 99.8(4) . . ? O4 Ca H8 108.9(3) . . ? T2 Ca H8 65.6(8) 1_545 . ? T3B Ca H8 113.3(7) 10_556 . ? T3S Ca H8 113.3(7) 10_556 . ? T4 Ca H8 117.1(6) . . ? T3B Ca H8 143.9(8) 10_546 . ? O7 Ca H2 116.4(10) 1_545 . ? O2 Ca H2 20.3(4) . . ? O8 Ca H2 158.4(8) . . ? O3 Ca H2 64.9(8) . . ? O9 Ca H2 100.2(5) 1_545 . ? O1 Ca H2 78.7(9) . . ? O4 Ca H2 71.7(2) . . ? T2 Ca H2 115.6(9) 1_545 . ? T3B Ca H2 65.2(10) 10_556 . ? T3S Ca H2 65.2(10) 10_556 . ? T4 Ca H2 62.6(4) . . ? T3B Ca H2 37.2(8) 10_546 . ? H8 Ca H2 178.5(11) . . ? O9 T1 O9 110.15(12) . 3 ? O9 T1 O1 109.78(4) . . ? O9 T1 O1 109.78(4) 3 . ? O9 T1 O1 109.78(4) . 10_556 ? O9 T1 O1 109.78(4) 3 10_556 ? O1 T1 O1 107.51(12) . 10_556 ? O9 T1 Ca 35.13(3) . 10_566 ? O9 T1 Ca 92.56(6) 3 10_566 ? O1 T1 Ca 144.71(3) . 10_566 ? O1 T1 Ca 88.98(5) 10_556 10_566 ? O9 T1 Ca 35.13(3) . 1_565 ? O9 T1 Ca 92.56(6) 3 1_565 ? O1 T1 Ca 88.98(5) . 1_565 ? O1 T1 Ca 144.71(3) 10_556 1_565 ? Ca T1 Ca 62.27(2) 10_566 1_565 ? O9 T1 Ca 92.56(6) . 3_565 ? O9 T1 Ca 35.13(3) 3 3_565 ? O1 T1 Ca 144.71(3) . 3_565 ? O1 T1 Ca 88.98(5) 10_556 3_565 ? Ca T1 Ca 63.46(2) 10_566 3_565 ? Ca T1 Ca 95.05(3) 1_565 3_565 ? O9 T1 Ca 92.56(6) . 12_565 ? O9 T1 Ca 35.13(3) 3 12_565 ? O1 T1 Ca 88.98(5) . 12_565 ? O1 T1 Ca 144.71(3) 10_556 12_565 ? Ca T1 Ca 95.05(3) 10_566 12_565 ? Ca T1 Ca 63.46(2) 1_565 12_565 ? Ca T1 Ca 62.27(2) 3_565 12_565 ? O8 T2 O7 112.02(13) . 10_556 ? O8 T2 O7 112.02(13) . . ? O7 T2 O7 111.79(19) 10_556 . ? O8 T2 O9 110.84(18) . . ? O7 T2 O9 104.84(13) 10_556 . ? O7 T2 O9 104.85(13) . . ? O8 T2 Ca 134.48(9) . 10_566 ? O7 T2 Ca 51.20(8) 10_556 10_566 ? O7 T2 Ca 113.44(15) . 10_566 ? O9 T2 Ca 54.43(7) . 10_566 ? O8 T2 Ca 134.48(9) . 1_565 ? O7 T2 Ca 113.44(15) 10_556 1_565 ? O7 T2 Ca 51.20(8) . 1_565 ? O9 T2 Ca 54.43(7) . 1_565 ? Ca T2 Ca 76.42(7) 10_566 1_565 ? O8 T2 Ca 35.90(5) . . ? O7 T2 Ca 147.91(14) 10_556 . ? O7 T2 Ca 88.30(8) . . ? O9 T2 Ca 93.02(11) . . ? Ca T2 Ca 143.65(10) 10_566 . ? Ca T2 Ca 98.65(4) 1_565 . ? O8 T2 Ca 35.90(5) . 10_556 ? O7 T2 Ca 88.30(8) 10_556 10_556 ? O7 T2 Ca 147.91(14) . 10_556 ? O9 T2 Ca 93.02(11) . 10_556 ? Ca T2 Ca 98.65(4) 10_566 10_556 ? Ca T2 Ca 143.65(10) 1_565 10_556 ? Ca T2 Ca 63.94(6) . 10_556 ? O2 T3S O3 113.39(8) 10_566 10_556 ? O2 T3S O3 113.39(8) 10_566 3 ? O3 T3S O3 110.70(12) 10_556 3 ? O2 T3S O1 112.15(12) 10_566 10_556 ? O3 T3S O1 103.14(8) 10_556 10_556 ? O3 T3S O1 103.14(8) 3 10_556 ? O2 T3S Ca 135.30(5) 10_566 3 ? O3 T3S Ca 111.22(8) 10_556 3 ? O3 T3S Ca 50.27(6) 3 3 ? O1 T3S Ca 53.51(5) 10_556 3 ? O2 T3S Ca 135.30(5) 10_566 10_556 ? O3 T3S Ca 50.27(6) 10_556 10_556 ? O3 T3S Ca 111.22(8) 3 10_556 ? O1 T3S Ca 53.51(5) 10_556 10_556 ? Ca T3S Ca 74.97(4) 3 10_556 ? O2 T3S Ca 37.18(3) 10_566 10_566 ? O3 T3S Ca 88.03(6) 10_556 10_566 ? O3 T3S Ca 150.53(8) 3 10_566 ? O1 T3S Ca 93.94(7) 10_556 10_566 ? Ca T3S Ca 144.38(5) 3 10_566 ? Ca T3S Ca 98.25(3) 10_556 10_566 ? O2 T3S Ca 37.18(3) 10_566 3_565 ? O3 T3S Ca 150.53(8) 10_556 3_565 ? O3 T3S Ca 88.03(6) 3 3_565 ? O1 T3S Ca 93.94(7) 10_556 3_565 ? Ca T3S Ca 98.25(3) 3 3_565 ? Ca T3S Ca 144.38(5) 10_556 3_565 ? Ca T3S Ca 66.75(3) 10_566 3_565 ? O3 T4 O3 120.11(10) . 4_565 ? O3 T4 O4 100.28(6) . . ? O3 T4 O4 110.68(6) 4_565 . ? O3 T4 O4 110.68(6) . 4_565 ? O3 T4 O4 100.28(6) 4_565 4_565 ? O4 T4 O4 115.65(9) . 4_565 ? O3 T4 Ca 127.89(5) . 4_565 ? O3 T4 Ca 46.10(4) 4_565 4_565 ? O4 T4 Ca 131.75(4) . 4_565 ? O4 T4 Ca 54.46(4) 4_565 4_565 ? O3 T4 Ca 46.10(4) . . ? O3 T4 Ca 127.88(5) 4_565 . ? O4 T4 Ca 54.46(4) . . ? O4 T4 Ca 131.75(4) 4_565 . ? Ca T4 Ca 170.88(3) 4_565 . ? O5 T5 O5 112.73(9) 1_545 4_565 ? O5 T5 O4 108.63(6) 1_545 4 ? O5 T5 O4 107.45(6) 4_565 4 ? O5 T5 O4 107.45(6) 1_545 . ? O5 T5 O4 108.63(6) 4_565 . ? O4 T5 O4 112.02(9) 4 . ? O7 T6 O6 110.59(6) . . ? O7 T6 O5 110.87(6) . . ? O6 T6 O5 107.96(6) . . ? O7 T6 O6 113.80(7) . 16 ? O6 T6 O6 106.18(4) . 16 ? O5 T6 O6 107.15(6) . 16 ? T1 O1 T3B 118.87(11) . 10_556 ? T1 O1 T3S 118.87(11) . 10_556 ? T3B O1 T3S 0.00(10) 10_556 10_556 ? T1 O1 Ca 122.55(5) . . ? T3B O1 Ca 93.91(6) 10_556 . ? T3S O1 Ca 93.91(6) 10_556 . ? T1 O1 Ca 122.55(5) . 12 ? T3B O1 Ca 93.91(6) 10_556 12 ? T3S O1 Ca 93.91(6) 10_556 12 ? Ca O1 Ca 98.08(6) . 12 ? T3B O2 T3S 0.00(10) 10_546 10_546 ? T3B O2 Ca 119.12(5) 10_546 . ? T3S O2 Ca 119.12(5) 10_546 . ? T3B O2 Ca 119.12(5) 10_546 12 ? T3S O2 Ca 119.12(5) 10_546 12 ? Ca O2 Ca 105.36(7) . 12 ? T3B O2 H2 106(3) 10_546 . ? T3S O2 H2 106(3) 10_546 . ? Ca O2 H2 102.4(19) . . ? Ca O2 H2 102.4(19) 12 . ? T4 O3 T3B 150.10(10) . 10_556 ? T4 O3 T3S 150.10(10) . 10_556 ? T3B O3 T3S 0.00(13) 10_556 10_556 ? T4 O3 Ca 105.08(6) . . ? T3B O3 Ca 98.47(7) 10_556 . ? T3S O3 Ca 98.47(7) 10_556 . ? T5 O4 T4 135.58(8) . . ? T5 O4 Ca 127.65(6) . . ? T4 O4 Ca 94.58(5) . . ? T5 O5 T6 142.88(8) 1_565 . ? T6 O6 T6 133.79(8) . 16_545 ? T6 O7 T2 130.06(13) . . ? T6 O7 Ca 133.91(7) . 1_565 ? T2 O7 Ca 96.02(11) . 1_565 ? T2 O8 Ca 120.47(7) . . ? T2 O8 Ca 120.47(7) . 10_556 ? Ca O8 Ca 102.20(6) . 10_556 ? T2 O8 H8 106(3) . . ? Ca O8 H8 102.3(15) . . ? Ca O8 H8 102.3(15) 10_556 . ? T1 O9 T2 122.11(14) . . ? T1 O9 Ca 122.23(5) . 10_566 ? T2 O9 Ca 91.78(8) . 10_566 ? T1 O9 Ca 122.23(5) . 1_565 ? T2 O9 Ca 91.78(8) . 1_565 ? Ca O9 Ca 98.94(6) 10_566 1_565 ? _refine_diff_density_max 0.379 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.081 _shelxl_version_number 2014-3 _shelx_res_file ; TITL bavenite in Cmcm CELL 0.71073 23.204 4.9442 19.418 90.000 90.000 90.000 ZERR 4.00 0.006 0.0009 0.005 0.000 0.000 0.000 LATT 7 SYMM -X, -Y, 0.5+Z SYMM -X, Y, 0.5-Z SYMM X, -Y, -Z SFAC BE H O AL SI CA UNIT 8 8 112 8 36 16 OMIT 2 0 0 OMIT -2 0 0 HTAB L.S. 10 BOND $H FMAP 2 PLAN 20 ACTA 4 WGHT 0.026400 6.885700 FVAR 0.23780 0.25514 0.98020 0.03124 CA 6 0.081337 0.262044 0.154437 31.00000 0.01086 0.01389 = 0.00976 0.00148 -0.00057 -0.00077 T1 5 0.000000 0.771893 0.250000 0.24262 0.00456 0.00706 = 0.00633 0.00000 0.00000 0.00000 T2 1 0.123925 0.829211 0.250000 0.49601 0.00783 0.01034 = 0.01001 0.00000 0.00000 -0.00013 T3S 5 0.000000 0.718017 0.396423 20.50000 0.00799 0.01073 = 0.00697 -0.00053 0.00000 0.00000 T3B 1 0.000000 0.718017 0.396423 -20.50000 0.00799 0.01073 = 0.00697 -0.00053 0.00000 0.00000 T4 4 0.092408 0.500000 0.000000 0.49864 0.00551 0.00592 = 0.00364 0.00038 0.00000 0.00000 T5 5 0.170134 0.000000 0.000000 10.50000 0.00851 0.01045 = 0.00754 -0.00043 0.00000 0.00000 T6 5 0.213787 0.868564 0.144814 11.00000 0.00714 0.00912 = 0.00740 0.00071 0.00081 0.00036 O1 3 0.000000 0.575525 0.181792 10.50000 0.01031 0.00972 = 0.00726 -0.00067 0.00000 0.00000 O2 3 0.000000 0.036982 0.107461 10.50000 0.01227 0.00994 = 0.01475 0.00074 0.00000 0.00000 O3 3 0.057701 0.593873 0.067910 11.00000 0.01402 0.01696 = 0.01309 0.00125 0.00458 0.00450 O4 3 0.130685 0.243874 0.032136 11.00000 0.01324 0.01514 = 0.01318 -0.00135 0.00051 0.00375 O5 3 0.208368 0.879450 0.061434 11.00000 0.01375 0.01860 = 0.00807 0.00095 -0.00032 0.00281 O6 3 0.232740 0.564393 0.166321 11.00000 0.01143 0.01032 = 0.01289 0.00155 0.00229 0.00191 O7 3 0.154226 0.947850 0.180363 11.00000 0.01003 0.01441 = 0.01177 0.00259 0.00355 0.00293 O8 3 0.121317 0.499774 0.250000 10.50000 0.00869 0.00993 = 0.01579 0.00000 0.00000 -0.00024 O9 3 0.057695 0.960952 0.250000 10.50000 0.00632 0.00916 = 0.01063 0.00000 0.00000 -0.00066 H8 2 0.161385 0.437170 0.250000 10.50000 0.05888 H2 2 0.000000 0.100389 0.059647 -20.50000 0.06778 DFIX 0.98 0.001 H8 O8 DFIX 0.98 0.001 H2 O2 EXYZ T3S T3B EADP T3S T3B HKLF 4 REM bavenite in Cmcm REM R1 = 0.0217 for 1532 Fo > 4sig(Fo) and 0.0257 for all 1709 data REM 126 parameters refined using 2 restraints END WGHT 0.0292 5.2662 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.379, deepest hole -0.372, 1-sigma level 0.081 Q1 1 0.1527 0.1520 0.0167 11.00000 0.05 0.38 Q2 1 0.2618 0.5229 0.1583 11.00000 0.05 0.38 Q3 1 0.1789 0.9223 0.1633 11.00000 0.05 0.37 Q4 1 0.0000 0.6377 0.2205 10.50000 0.05 0.36 Q5 1 0.1204 0.3682 0.0004 11.00000 0.05 0.34 Q6 1 0.0340 0.8915 0.2500 10.50000 0.05 0.32 Q7 1 0.0000 0.6248 0.3608 10.50000 0.05 0.30 Q8 1 0.2261 0.7165 0.1553 11.00000 0.05 0.29 Q9 1 0.1072 0.3747 0.0267 11.00000 0.05 0.28 Q10 1 0.0822 0.5876 0.0377 11.00000 0.05 0.27 Q11 1 0.0000 0.0824 0.1498 10.50000 0.05 0.27 Q12 1 0.1859 0.9136 0.0369 11.00000 0.05 0.27 Q13 1 0.1186 0.6342 0.2500 10.50000 0.05 0.27 Q14 1 0.0000 -0.0897 0.0948 10.50000 0.05 0.26 Q15 1 0.0489 0.8395 0.2319 11.00000 0.05 0.25 Q16 1 0.0914 0.1352 0.1419 11.00000 0.05 0.25 Q17 1 0.2094 0.9444 0.0893 11.00000 0.05 0.25 Q18 1 0.0242 0.0744 0.1140 11.00000 0.05 0.25 Q19 1 0.0318 0.5856 0.0887 11.00000 0.05 0.23 Q20 1 0.1121 0.3683 0.2908 11.00000 0.05 0.22 ; _shelx_res_checksum 98914 _shelx_hkl_file ; -2 0 0 -0.5233 0.7973 2 0 0 -0.6866 0.7966 -4 0 0 1.7918 0.7126 4 0 0 0.8343 0.9945 -6 0 0 1351.51 20.35 6 0 0 1349.03 21.27 -8 0 0 20.346 1.689 8 0 0 20.721 1.645 -10 0 0 1994.36 35.35 10 0 0 1983.30 31.58 -12 0 0 1387.84 26.54 12 0 0 1403.39 23.76 -14 0 0 9708.75 171.05 14 0 0 9999.00 145.69 -16 0 0 148.01 7.50 16 0 0 152.64 6.37 -18 0 0 747.70 18.27 18 0 0 759.11 16.18 -20 0 0 44.701 4.758 20 0 0 58.328 4.910 -22 0 0 518.32 13.35 22 0 0 533.96 14.54 -24 0 0 4073.56 65.28 24 0 0 4184.45 77.49 -26 0 0 29.904 5.960 26 0 0 25.501 5.415 -28 0 0 12.754 5.617 28 0 0 1.6234 5.6065 -30 0 0 98.904 12.233 30 0 0 110.81 12.47 -32 0 0 127.19 14.12 32 0 0 115.48 13.67 -1 -1 0 10.902 1.801 1 -1 0 9.7926 1.6430 -1 1 0 10.112 1.136 1 1 0 11.573 0.823 -3 -1 0 3863.21 55.69 3 -1 0 3839.06 55.35 -3 1 0 3865.91 45.37 3 1 0 3819.95 49.75 -5 -1 0 5983.06 100.51 5 -1 0 6124.39 89.44 -5 1 0 6161.08 77.09 5 1 0 6170.00 72.62 -7 -1 0 248.94 7.24 7 -1 0 271.56 6.64 -7 1 0 268.63 5.22 7 1 0 260.99 5.49 -9 -1 0 501.89 11.63 9 -1 0 504.12 10.32 -9 1 0 510.88 9.79 9 1 0 506.19 9.89 -11 -1 0 36.198 3.750 11 -1 0 43.303 3.295 -11 1 0 39.582 3.003 11 1 0 44.345 3.246 -13 -1 0 8.8790 3.0648 13 -1 0 14.862 2.557 -13 1 0 10.252 2.397 13 1 0 12.654 2.308 -15 -1 0 129.03 7.25 15 -1 0 135.25 5.83 -15 1 0 137.70 5.78 15 1 0 123.87 5.71 -17 -1 0 336.57 11.59 17 -1 0 364.41 10.70 -17 1 0 352.95 9.97 17 1 0 341.36 9.48 -19 -1 0 1440.71 29.99 19 -1 0 1385.42 30.96 -19 1 0 1432.02 25.46 19 1 0 1380.36 30.34 -21 -1 0 1634.84 33.78 21 -1 0 1623.37 35.10 -21 1 0 1609.15 28.74 21 1 0 1568.72 34.46 -23 -1 0 138.15 9.22 23 -1 0 165.50 10.37 -23 1 0 158.65 8.01 23 1 0 145.61 9.30 -25 -1 0 22.715 7.398 25 -1 0 29.456 5.737 -25 1 0 21.209 6.712 25 1 0 20.889 5.022 -27 -1 0 26.638 6.309 27 -1 0 11.433 5.284 -27 1 0 17.209 6.770 27 1 0 11.155 4.859 -29 -1 0 216.35 13.41 29 -1 0 226.77 16.33 -29 1 0 216.80 16.04 29 1 0 213.54 12.90 -31 -1 0 169.28 12.70 31 -1 0 185.36 15.73 -31 1 0 187.34 11.60 31 1 0 150.59 11.73 0 -2 0 380.23 9.51 0 2 0 416.70 7.20 -2 -2 0 1038.40 17.45 2 -2 0 1051.83 16.87 -2 2 0 1050.63 15.17 2 2 0 1039.11 13.81 -4 -2 0 331.82 7.60 4 -2 0 322.78 9.05 -4 2 0 321.17 6.32 4 2 0 321.52 6.17 -6 -2 0 1343.26 22.23 6 -2 0 1387.09 22.46 -6 2 0 1362.93 19.40 6 2 0 1358.04 22.13 -8 -2 0 2.5754 1.6984 8 -2 0 2.1227 1.6924 -8 2 0 1.7256 1.3026 8 2 0 -0.4970 1.5690 -10 -2 0 924.64 19.20 10 -2 0 935.04 17.16 -10 2 0 946.27 13.76 10 2 0 916.18 16.93 -12 -2 0 6.8558 2.3850 12 -2 0 10.773 2.650 -12 2 0 7.5280 1.8705 12 2 0 11.897 2.275 -14 -2 0 1541.09 26.24 14 -2 0 1571.71 27.49 -14 2 0 1580.71 22.93 14 2 0 1539.87 31.59 -16 -2 0 151.52 8.66 16 -2 0 166.00 7.30 -16 2 0 173.94 5.82 16 2 0 164.93 8.36 -18 -2 0 2049.80 40.89 18 -2 0 2117.45 36.09 -18 2 0 2053.48 33.65 18 2 0 2060.60 41.68 -20 -2 0 431.00 14.39 20 -2 0 454.35 14.88 -20 2 0 463.96 11.44 20 2 0 448.01 14.45 -22 -2 0 63.963 7.295 22 -2 0 56.359 6.670 -22 2 0 72.196 5.413 22 2 0 66.118 6.712 -24 -2 0 702.64 20.71 24 -2 0 748.90 21.50 -24 2 0 760.49 19.19 24 2 0 690.41 23.91 -26 -2 0 519.05 21.91 26 -2 0 518.86 23.32 -26 2 0 497.66 15.62 26 2 0 472.30 17.26 -28 -2 0 190.32 15.66 28 -2 0 189.64 16.49 -28 2 0 206.89 11.29 28 2 0 191.38 12.49 -30 -2 0 193.98 16.87 30 -2 0 265.36 19.90 -30 2 0 218.30 17.00 30 2 0 216.73 13.89 -1 -3 0 7.4757 3.0345 1 -3 0 10.387 2.456 -1 3 0 15.251 2.024 1 3 0 12.525 1.606 -3 -3 0 387.02 8.99 3 -3 0 384.03 10.81 -3 3 0 398.54 8.01 3 3 0 396.79 8.85 -5 -3 0 12.469 2.613 5 -3 0 8.5472 2.8834 -5 3 0 14.313 2.263 5 3 0 13.021 1.796 -7 -3 0 1197.98 21.56 7 -3 0 1228.29 26.09 -7 3 0 1214.26 18.67 7 3 0 1212.95 19.24 -9 -3 0 3631.09 65.53 9 -3 0 3600.46 67.83 -9 3 0 3747.71 49.67 9 3 0 3732.89 56.80 -11 -3 0 486.09 13.85 11 -3 0 524.51 15.79 -11 3 0 504.43 10.17 11 3 0 505.01 11.63 -13 -3 0 272.24 10.37 13 -3 0 263.84 11.14 -13 3 0 267.98 8.35 13 3 0 269.16 8.40 -15 -3 0 46.371 5.522 15 -3 0 49.710 6.079 -15 3 0 50.282 4.489 15 3 0 45.647 4.380 -17 -3 0 621.14 17.84 17 -3 0 672.60 19.23 -17 3 0 636.18 14.82 17 3 0 641.81 15.23 -19 -3 0 76.755 7.349 19 -3 0 79.066 7.840 -19 3 0 91.818 6.235 19 3 0 86.983 7.264 -21 -3 0 22.092 5.459 21 -3 0 32.312 7.673 -21 3 0 27.170 4.984 21 3 0 26.427 5.264 -23 -3 0 171.74 11.17 23 -3 0 167.84 14.93 -23 3 0 156.99 12.83 23 3 0 154.56 10.47 -25 -3 0 69.603 8.433 25 -3 0 75.038 11.082 -25 3 0 77.709 10.139 25 3 0 62.694 7.537 -27 -3 0 43.153 9.858 27 -3 0 23.723 9.361 -27 3 0 36.679 8.467 27 3 0 19.714 6.033 -29 -3 0 6.7680 7.9479 29 -3 0 24.609 9.447 -29 3 0 8.9562 7.4477 29 3 0 5.3104 7.0585 0 -4 0 1634.64 34.24 0 4 0 1583.54 24.23 -2 -4 0 2227.46 44.97 2 -4 0 2341.67 45.80 -2 4 0 2312.79 32.90 2 4 0 2225.70 43.46 -4 -4 0 2431.91 47.00 4 -4 0 2371.30 59.62 -4 4 0 2397.46 34.42 4 4 0 2403.44 45.91 -6 -4 0 57.712 6.009 6 -4 0 52.280 7.965 -6 4 0 61.756 4.019 6 4 0 60.493 5.616 -8 -4 0 75.134 6.627 8 -4 0 79.215 9.514 -8 4 0 81.362 5.359 8 4 0 70.410 5.598 -10 -4 0 14.760 4.229 10 -4 0 17.477 6.257 -10 4 0 16.475 3.376 10 4 0 19.489 3.991 -12 -4 0 4699.51 84.32 12 -4 0 4677.16 108.97 -12 4 0 4778.27 71.44 12 4 0 4637.50 84.56 -14 -4 0 99.310 9.881 14 -4 0 95.123 11.110 -14 4 0 113.37 6.73 14 4 0 88.041 7.288 -16 -4 0 155.89 10.17 16 -4 0 160.56 14.33 -16 4 0 159.51 8.25 16 4 0 156.63 9.55 -18 -4 0 511.62 17.02 18 -4 0 521.77 24.97 -18 4 0 509.66 13.86 18 4 0 479.74 16.16 -20 -4 0 184.79 11.62 20 -4 0 200.87 16.44 -20 4 0 207.32 10.09 20 4 0 230.34 14.89 -22 -4 0 739.66 22.32 22 -4 0 768.75 45.68 -22 4 0 754.77 26.77 22 4 0 678.86 26.50 -24 -4 0 446.33 17.47 24 -4 0 427.48 36.15 -24 4 0 448.68 20.78 24 4 0 453.97 21.56 -26 -4 0 474.96 23.39 26 -4 0 510.22 39.40 -26 4 0 533.02 23.42 26 4 0 506.91 23.64 -1 -5 0 23.660 5.462 1 -5 0 31.952 5.881 -1 5 0 26.002 3.663 1 5 0 28.024 4.719 -3 -5 0 66.199 9.050 3 -5 0 81.152 8.091 -3 5 0 78.580 5.652 3 5 0 71.762 6.657 -5 -5 0 133.12 9.46 5 -5 0 136.23 10.12 -5 5 0 131.65 7.27 5 5 0 162.57 9.51 -7 -5 0 715.88 20.79 7 -5 0 689.29 21.33 -7 5 0 725.66 16.52 7 5 0 713.59 19.77 -9 -5 0 633.66 19.76 9 -5 0 668.51 26.70 -9 5 0 683.04 16.20 9 5 0 673.56 23.60 -11 -5 0 27.590 5.864 11 -5 0 9.9717 6.8970 -11 5 0 20.954 4.146 11 5 0 13.594 5.524 -13 -5 0 -2.931 5.252 13 -5 0 10.147 7.294 -13 5 0 6.3498 3.5717 13 5 0 5.9920 5.6194 -15 -5 0 16.795 6.589 15 -5 0 4.4105 7.5359 -15 5 0 11.151 4.116 15 5 0 17.399 6.614 -17 -5 0 1204.54 31.52 17 -5 0 1312.76 42.84 -17 5 0 1278.74 26.22 17 5 0 1230.30 38.44 -19 -5 0 3.9230 5.6031 19 -5 0 -2.317 8.348 -19 5 0 6.1049 4.4187 19 5 0 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