data_shelx _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H0 Be3.20 Ca0.61 F0 Na3.39 O7 Si1.80' _chemical_formula_weight 293.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ca' 'Ca' 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Be' 'Be' 0.0038 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 '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' _space_group_crystal_system tetragonal _space_group_IT_number 113 _space_group_name_H-M_alt 'P -4 21 m' _space_group_name_Hall 'P -4 2ab' _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' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 7.4007(2) _cell_length_b 7.4007(2) _cell_length_c 4.9608(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 271.705(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.590 _exptl_crystal_F_000 287 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 13.422 _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 ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4586 _diffrn_reflns_av_unetI/netI 0.0083 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 8.471 _diffrn_reflns_theta_max 71.862 _diffrn_reflns_theta_full 67.684 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 297 _reflns_number_gt 297 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.588 _reflns_Friedel_fraction_max 1.000 _reflns_Friedel_fraction_full 1.000 _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-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion twin. ; _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^)+(0.0139P)^2^+0.2137P] 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_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.54(3) _chemical_absolute_configuration ? _refine_ls_number_reflns 297 _refine_ls_number_parameters 43 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0160 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0413 _refine_ls_wR_factor_gt 0.0413 _refine_ls_goodness_of_fit_ref 1.320 _refine_ls_restrained_S_all 1.318 _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 Ca1 Ca 0.65951(9) 0.15951(9) 0.0123(2) 0.0113(3) Uani 0.726(5) 2 d S T P . . Si1 Si 0.0000 0.0000 -0.5000 0.0078(5) Uani 0.822(12) 4 d S T P . . Be1 Be 0.0000 0.0000 -0.5000 0.0078(5) Uani 0.178(12) 4 d S T P . . Si2 Si 0.35744(17) 0.14256(17) -0.4484(3) 0.0054(6) Uani 0.404(8) 2 d S T P . . Be2 Be 0.35744(17) 0.14256(17) -0.4484(3) 0.0054(6) Uani 0.596(8) 2 d S T P . . O1 O 0.5000 0.0000 -0.3220(8) 0.0123(9) Uani 1 4 d S T P . . O2 O 0.1614(3) 0.0856(3) -0.3135(4) 0.0133(5) Uani 1 1 d . . . . . O3 O 0.3568(3) 0.1432(3) -0.7696(5) 0.0123(7) Uani 1 2 d DS T P . . H1 H 0.373(19) 0.225(12) -0.889(19) 0.00(5) Uiso 0.21(7) 1 d D . . . . 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 Ca1 0.0125(4) 0.0125(4) 0.0090(5) 0.0004(3) 0.0004(3) -0.0038(4) Si1 0.0060(6) 0.0060(6) 0.0115(9) 0.000 0.000 0.000 Be1 0.0060(6) 0.0060(6) 0.0115(9) 0.000 0.000 0.000 Si2 0.0055(7) 0.0055(7) 0.0053(9) 0.0001(5) -0.0001(5) -0.0012(6) Be2 0.0055(7) 0.0055(7) 0.0053(9) 0.0001(5) -0.0001(5) -0.0012(6) O1 0.0132(12) 0.0132(12) 0.0105(19) 0.000 0.000 0.0046(15) O2 0.0103(9) 0.0147(11) 0.0149(9) -0.0028(8) 0.0007(8) -0.0011(8) O3 0.0133(9) 0.0133(9) 0.0102(12) 0.0005(7) -0.0005(7) -0.0039(11) _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 Ca1 O1 2.353(3) . ? Ca1 O3 2.391(3) 4_654 ? Ca1 O2 2.407(2) 5 ? Ca1 O2 2.407(2) 4_655 ? Ca1 O3 2.491(2) 3_656 ? Ca1 O3 2.491(2) 1_556 ? Ca1 O2 2.767(2) 7 ? Ca1 O2 2.767(2) 3_655 ? Ca1 Be2 2.9954(18) 4_655 ? Ca1 Si2 2.9954(18) 4_655 ? Ca1 Si2 3.1993(16) . ? Si1 O2 1.6385(19) 2_554 ? Si1 O2 1.6385(19) 3 ? Si1 O2 1.6385(19) 4_554 ? Si1 O2 1.6385(19) . ? Si2 O3 1.594(3) . ? Si2 O1 1.618(2) . ? Si2 O2 1.652(2) . ? Si2 O2 1.652(2) 7 ? Si2 Ca1 2.9954(18) 2_565 ? Si2 Ca1 3.1993(16) 3_655 ? Si2 Ca1 3.4808(19) 2_564 ? Si2 Ca1 3.4889(18) 3_654 ? Si2 Ca1 3.4889(18) 1_554 ? O1 Be2 1.618(2) 3_655 ? O1 Si2 1.618(2) 3_655 ? O1 Ca1 2.353(3) 3_655 ? O2 Ca1 2.407(2) 2_565 ? O2 Ca1 2.767(2) 3_655 ? O3 Ca1 2.391(3) 2_564 ? O3 Ca1 2.491(2) 3_654 ? O3 Ca1 2.491(2) 1_554 ? O3 H1 0.86(3) . ? 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 O1 Ca1 O3 104.96(10) . 4_654 ? O1 Ca1 O2 146.49(5) . 5 ? O3 Ca1 O2 80.22(8) 4_654 5 ? O1 Ca1 O2 146.49(5) . 4_655 ? O3 Ca1 O2 80.22(8) 4_654 4_655 ? O2 Ca1 O2 66.74(10) 5 4_655 ? O1 Ca1 O3 80.25(8) . 3_656 ? O3 Ca1 O3 142.93(6) 4_654 3_656 ? O2 Ca1 O3 115.81(9) 5 3_656 ? O2 Ca1 O3 76.92(7) 4_655 3_656 ? O1 Ca1 O3 80.25(8) . 1_556 ? O3 Ca1 O3 142.93(6) 4_654 1_556 ? O2 Ca1 O3 76.92(7) 5 1_556 ? O2 Ca1 O3 115.81(9) 4_655 1_556 ? O3 Ca1 O3 73.97(12) 3_656 1_556 ? O1 Ca1 O2 59.99(5) . 7 ? O3 Ca1 O2 79.27(6) 4_654 7 ? O2 Ca1 O2 89.50(9) 5 7 ? O2 Ca1 O2 150.88(4) 4_655 7 ? O3 Ca1 O2 130.73(7) 3_656 7 ? O3 Ca1 O2 71.79(8) 1_556 7 ? O1 Ca1 O2 59.99(5) . 3_655 ? O3 Ca1 O2 79.27(6) 4_654 3_655 ? O2 Ca1 O2 150.88(4) 5 3_655 ? O2 Ca1 O2 89.50(9) 4_655 3_655 ? O3 Ca1 O2 71.79(8) 3_656 3_655 ? O3 Ca1 O2 130.73(7) 1_556 3_655 ? O2 Ca1 O2 106.66(9) 7 3_655 ? O1 Ca1 Be2 178.57(9) . 4_655 ? O3 Ca1 Be2 76.48(7) 4_654 4_655 ? O2 Ca1 Be2 33.41(5) 5 4_655 ? O2 Ca1 Be2 33.41(5) 4_655 4_655 ? O3 Ca1 Be2 98.61(6) 3_656 4_655 ? O3 Ca1 Be2 98.61(6) 1_556 4_655 ? O2 Ca1 Be2 120.54(5) 7 4_655 ? O2 Ca1 Be2 120.54(5) 3_655 4_655 ? O1 Ca1 Si2 178.57(9) . 4_655 ? O3 Ca1 Si2 76.48(7) 4_654 4_655 ? O2 Ca1 Si2 33.41(5) 5 4_655 ? O2 Ca1 Si2 33.41(5) 4_655 4_655 ? O3 Ca1 Si2 98.61(6) 3_656 4_655 ? O3 Ca1 Si2 98.61(6) 1_556 4_655 ? O2 Ca1 Si2 120.54(5) 7 4_655 ? O2 Ca1 Si2 120.54(5) 3_655 4_655 ? Be2 Ca1 Si2 0.00(9) 4_655 4_655 ? O1 Ca1 Si2 29.12(3) . . ? O3 Ca1 Si2 95.23(7) 4_654 . ? O2 Ca1 Si2 118.58(6) 5 . ? O2 Ca1 Si2 172.51(7) 4_655 . ? O3 Ca1 Si2 103.95(6) 3_656 . ? O3 Ca1 Si2 71.34(6) 1_556 . ? O2 Ca1 Si2 31.09(5) 7 . ? O2 Ca1 Si2 83.79(6) 3_655 . ? Be2 Ca1 Si2 151.26(3) 4_655 . ? Si2 Ca1 Si2 151.26(3) 4_655 . ? O2 Si1 O2 108.59(7) 2_554 3 ? O2 Si1 O2 111.25(15) 2_554 4_554 ? O2 Si1 O2 108.59(7) 3 4_554 ? O2 Si1 O2 108.59(7) 2_554 . ? O2 Si1 O2 111.25(15) 3 . ? O2 Si1 O2 108.59(7) 4_554 . ? O3 Si2 O1 113.0(2) . . ? O3 Si2 O2 113.78(11) . . ? O1 Si2 O2 104.43(12) . . ? O3 Si2 O2 113.78(11) . 7 ? O1 Si2 O2 104.43(12) . 7 ? O2 Si2 O2 106.50(16) . 7 ? O3 Si2 Ca1 136.02(15) . 2_565 ? O1 Si2 Ca1 110.97(15) . 2_565 ? O2 Si2 Ca1 53.34(8) . 2_565 ? O2 Si2 Ca1 53.34(8) 7 2_565 ? O3 Si2 Ca1 135.73(10) . . ? O1 Si2 Ca1 45.04(9) . . ? O2 Si2 Ca1 109.52(10) . . ? O2 Si2 Ca1 59.87(8) 7 . ? Ca1 Si2 Ca1 78.85(4) 2_565 . ? O3 Si2 Ca1 135.73(10) . 3_655 ? O1 Si2 Ca1 45.04(9) . 3_655 ? O2 Si2 Ca1 59.86(8) . 3_655 ? O2 Si2 Ca1 109.52(10) 7 3_655 ? Ca1 Si2 Ca1 78.85(4) 2_565 3_655 ? Ca1 Si2 Ca1 62.91(4) . 3_655 ? O3 Si2 Ca1 36.30(12) . 2_564 ? O1 Si2 Ca1 149.31(15) . 2_564 ? O2 Si2 Ca1 93.63(9) . 2_564 ? O2 Si2 Ca1 93.63(9) 7 2_564 ? Ca1 Si2 Ca1 99.72(5) 2_565 2_564 ? Ca1 Si2 Ca1 148.38(2) . 2_564 ? Ca1 Si2 Ca1 148.38(2) 3_655 2_564 ? O3 Si2 Ca1 40.07(8) . 3_654 ? O1 Si2 Ca1 84.42(13) . 3_654 ? O2 Si2 Ca1 96.63(8) . 3_654 ? O2 Si2 Ca1 151.93(10) 7 3_654 ? Ca1 Si2 Ca1 148.18(3) 2_565 3_654 ? Ca1 Si2 Ca1 126.73(5) . 3_654 ? Ca1 Si2 Ca1 95.66(3) 3_655 3_654 ? Ca1 Si2 Ca1 68.79(3) 2_564 3_654 ? O3 Si2 Ca1 40.07(8) . 1_554 ? O1 Si2 Ca1 84.42(13) . 1_554 ? O2 Si2 Ca1 151.93(10) . 1_554 ? O2 Si2 Ca1 96.63(8) 7 1_554 ? Ca1 Si2 Ca1 148.18(3) 2_565 1_554 ? Ca1 Si2 Ca1 95.66(3) . 1_554 ? Ca1 Si2 Ca1 126.73(5) 3_655 1_554 ? Ca1 Si2 Ca1 68.79(3) 2_564 1_554 ? Ca1 Si2 Ca1 57.18(4) 3_654 1_554 ? Si2 O1 Be2 134.4(3) . 3_655 ? Si2 O1 Si2 134.4(3) . 3_655 ? Be2 O1 Si2 0.00(12) 3_655 3_655 ? Si2 O1 Ca1 105.84(8) . . ? Be2 O1 Ca1 105.84(8) 3_655 . ? Si2 O1 Ca1 105.84(8) 3_655 . ? Si2 O1 Ca1 105.84(8) . 3_655 ? Be2 O1 Ca1 105.84(8) 3_655 3_655 ? Si2 O1 Ca1 105.84(8) 3_655 3_655 ? Ca1 O1 Ca1 90.38(14) . 3_655 ? Si1 O2 Si2 120.68(13) . . ? Si1 O2 Ca1 130.49(11) . 2_565 ? Si2 O2 Ca1 93.25(10) . 2_565 ? Si1 O2 Ca1 115.18(9) . 3_655 ? Si2 O2 Ca1 89.05(10) . 3_655 ? Ca1 O2 Ca1 98.86(7) 2_565 3_655 ? Si2 O3 Ca1 120.46(17) . 2_564 ? Si2 O3 Ca1 115.60(12) . 3_654 ? Ca1 O3 Ca1 107.52(8) 2_564 3_654 ? Si2 O3 Ca1 115.60(12) . 1_554 ? Ca1 O3 Ca1 107.52(8) 2_564 1_554 ? Ca1 O3 Ca1 84.18(10) 3_654 1_554 ? Si2 O3 H1 134(9) . . ? Ca1 O3 H1 46(10) 2_564 . ? Ca1 O3 H1 110(9) 3_654 . ? Ca1 O3 H1 62(10) 1_554 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Si2 O1 Be2 0.000(0) . . . 3_655 ? O2 Si2 O1 Be2 124.17(10) . . . 3_655 ? O2 Si2 O1 Be2 -124.17(10) 7 . . 3_655 ? Ca1 Si2 O1 Be2 180.000(0) 2_565 . . 3_655 ? Ca1 Si2 O1 Be2 -132.49(10) . . . 3_655 ? Ca1 Si2 O1 Be2 132.49(10) 3_655 . . 3_655 ? Ca1 Si2 O1 Be2 0.000(1) 2_564 . . 3_655 ? Ca1 Si2 O1 Be2 28.74(2) 3_654 . . 3_655 ? Ca1 Si2 O1 Be2 -28.74(2) 1_554 . . 3_655 ? O3 Si2 O1 Si2 0.000(0) . . . 3_655 ? O2 Si2 O1 Si2 124.17(10) . . . 3_655 ? O2 Si2 O1 Si2 -124.17(10) 7 . . 3_655 ? Ca1 Si2 O1 Si2 180.000(0) 2_565 . . 3_655 ? Ca1 Si2 O1 Si2 -132.49(10) . . . 3_655 ? Ca1 Si2 O1 Si2 132.49(10) 3_655 . . 3_655 ? Ca1 Si2 O1 Si2 0.000(1) 2_564 . . 3_655 ? Ca1 Si2 O1 Si2 28.74(2) 3_654 . . 3_655 ? Ca1 Si2 O1 Si2 -28.74(2) 1_554 . . 3_655 ? O3 Si2 O1 Ca1 132.49(10) . . . . ? O2 Si2 O1 Ca1 -103.34(11) . . . . ? O2 Si2 O1 Ca1 8.31(16) 7 . . . ? Ca1 Si2 O1 Ca1 -47.51(10) 2_565 . . . ? Ca1 Si2 O1 Ca1 -95.03(19) 3_655 . . . ? Ca1 Si2 O1 Ca1 132.49(10) 2_564 . . . ? Ca1 Si2 O1 Ca1 161.22(10) 3_654 . . . ? Ca1 Si2 O1 Ca1 103.75(10) 1_554 . . . ? O3 Si2 O1 Ca1 -132.49(10) . . . 3_655 ? O2 Si2 O1 Ca1 -8.31(16) . . . 3_655 ? O2 Si2 O1 Ca1 103.34(11) 7 . . 3_655 ? Ca1 Si2 O1 Ca1 47.51(10) 2_565 . . 3_655 ? Ca1 Si2 O1 Ca1 95.03(19) . . . 3_655 ? Ca1 Si2 O1 Ca1 -132.49(10) 2_564 . . 3_655 ? Ca1 Si2 O1 Ca1 -103.75(10) 3_654 . . 3_655 ? Ca1 Si2 O1 Ca1 -161.22(10) 1_554 . . 3_655 ? O2 Si1 O2 Si2 48.08(17) 2_554 . . . ? O2 Si1 O2 Si2 167.53(17) 3 . . . ? O2 Si1 O2 Si2 -73.02(18) 4_554 . . . ? O2 Si1 O2 Ca1 174.46(16) 2_554 . . 2_565 ? O2 Si1 O2 Ca1 -66.10(12) 3 . . 2_565 ? O2 Si1 O2 Ca1 53.35(8) 4_554 . . 2_565 ? O2 Si1 O2 Ca1 -56.85(3) 2_554 . . 3_655 ? O2 Si1 O2 Ca1 62.60(7) 3 . . 3_655 ? O2 Si1 O2 Ca1 -177.95(12) 4_554 . . 3_655 ? O3 Si2 O2 Si1 11.5(2) . . . . ? O1 Si2 O2 Si1 -112.22(17) . . . . ? O2 Si2 O2 Si1 137.63(10) 7 . . . ? Ca1 Si2 O2 Si1 142.17(17) 2_565 . . . ? Ca1 Si2 O2 Si1 -159.14(10) . . . . ? Ca1 Si2 O2 Si1 -119.01(14) 3_655 . . . ? Ca1 Si2 O2 Si1 42.75(13) 2_564 . . . ? Ca1 Si2 O2 Si1 -26.30(14) 3_654 . . . ? Ca1 Si2 O2 Si1 -6.6(3) 1_554 . . . ? O3 Si2 O2 Ca1 -130.71(15) . . . 2_565 ? O1 Si2 O2 Ca1 105.61(14) . . . 2_565 ? O2 Si2 O2 Ca1 -4.54(16) 7 . . 2_565 ? Ca1 Si2 O2 Ca1 58.69(8) . . . 2_565 ? Ca1 Si2 O2 Ca1 98.82(7) 3_655 . . 2_565 ? Ca1 Si2 O2 Ca1 -99.42(6) 2_564 . . 2_565 ? Ca1 Si2 O2 Ca1 -168.47(6) 3_654 . . 2_565 ? Ca1 Si2 O2 Ca1 -148.79(17) 1_554 . . 2_565 ? O3 Si2 O2 Ca1 130.47(14) . . . 3_655 ? O1 Si2 O2 Ca1 6.79(14) . . . 3_655 ? O2 Si2 O2 Ca1 -103.36(11) 7 . . 3_655 ? Ca1 Si2 O2 Ca1 -98.82(7) 2_565 . . 3_655 ? Ca1 Si2 O2 Ca1 -40.13(8) . . . 3_655 ? Ca1 Si2 O2 Ca1 161.76(5) 2_564 . . 3_655 ? Ca1 Si2 O2 Ca1 92.71(5) 3_654 . . 3_655 ? Ca1 Si2 O2 Ca1 112.39(19) 1_554 . . 3_655 ? O1 Si2 O3 Ca1 180.000(0) . . . 2_564 ? O2 Si2 O3 Ca1 61.12(12) . . . 2_564 ? O2 Si2 O3 Ca1 -61.12(12) 7 . . 2_564 ? Ca1 Si2 O3 Ca1 0.000(1) 2_565 . . 2_564 ? Ca1 Si2 O3 Ca1 -131.62(12) . . . 2_564 ? Ca1 Si2 O3 Ca1 131.62(12) 3_655 . . 2_564 ? Ca1 Si2 O3 Ca1 131.99(10) 3_654 . . 2_564 ? Ca1 Si2 O3 Ca1 -131.99(10) 1_554 . . 2_564 ? O1 Si2 O3 Ca1 48.01(10) . . . 3_654 ? O2 Si2 O3 Ca1 -70.86(19) . . . 3_654 ? O2 Si2 O3 Ca1 166.89(10) 7 . . 3_654 ? Ca1 Si2 O3 Ca1 -131.99(10) 2_565 . . 3_654 ? Ca1 Si2 O3 Ca1 96.39(7) . . . 3_654 ? Ca1 Si2 O3 Ca1 -0.4(2) 3_655 . . 3_654 ? Ca1 Si2 O3 Ca1 -131.99(10) 2_564 . . 3_654 ? Ca1 Si2 O3 Ca1 96.0(2) 1_554 . . 3_654 ? O1 Si2 O3 Ca1 -48.01(10) . . . 1_554 ? O2 Si2 O3 Ca1 -166.89(10) . . . 1_554 ? O2 Si2 O3 Ca1 70.87(19) 7 . . 1_554 ? Ca1 Si2 O3 Ca1 131.99(10) 2_565 . . 1_554 ? Ca1 Si2 O3 Ca1 0.4(2) . . . 1_554 ? Ca1 Si2 O3 Ca1 -96.39(7) 3_655 . . 1_554 ? Ca1 Si2 O3 Ca1 131.99(10) 2_564 . . 1_554 ? Ca1 Si2 O3 Ca1 -96.0(2) 3_654 . . 1_554 ? _refine_diff_density_max 0.207 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.048 _shelxl_version_number 2013-4 _shelx_res_file ; TITL s15mtw103 in P-421m #113 CELL 1.54184 7.4007 7.4007 4.9608 90.000 90.000 90.000 ZERR 2.00 0.0002 0.0002 0.0002 0.000 0.000 0.000 LATT -1 SYMM Y, - X, - Z SYMM - X, - Y, Z SYMM - Y, X, - Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM 1/2 - X, 1/2 + Y, - Z SYMM 1/2 - Y, 1/2 - X, Z SYMM 1/2 + Y, 1/2 + X, Z SFAC CA NA SI BE O F H UNIT 1.21 6.79 3.6 6.4 14 0 0 LIST 4 MERG 2 TWIN EXYZ BE2 SI2 EADP BE2 SI2 EXYZ BE1 SI1 EADP BE1 SI1 DFIX 0.860 0.020 O3 H1 FMAP 2 PLAN 20 BOND BOND $H HTAB CONF L.S. 6 TEMP -123.00 ACTA WGHT 0.013900 0.213700 BASF 0.53513 FVAR 17.69062 0.72561 0.82242 0.40447 CA1 1 0.659505 0.159505 0.012257 20.50000 0.01254 0.01254 = 0.00895 0.00044 0.00044 -0.00376 SI1 3 0.000000 0.000000 -0.500000 30.25000 0.00602 0.00602 = 0.01150 0.00000 0.00000 0.00000 BE1 4 0.000000 0.000000 -0.500000 -30.25000 0.00602 0.00602 = 0.01150 0.00000 0.00000 0.00000 SI2 3 0.357439 0.142561 -0.448393 40.50000 0.00546 0.00546 = 0.00534 0.00006 -0.00006 -0.00124 BE2 4 0.357439 0.142561 -0.448393 -40.50000 0.00546 0.00546 = 0.00534 0.00006 -0.00006 -0.00124 O1 5 0.500000 0.000000 -0.322042 10.25000 0.01320 0.01320 = 0.01049 0.00000 0.00000 0.00458 O2 5 0.161449 0.085592 -0.313515 11.00000 0.01027 0.01473 = 0.01489 -0.00280 0.00068 -0.00112 O3 5 0.356846 0.143154 -0.769618 10.50000 0.01327 0.01327 = 0.01024 0.00054 -0.00054 -0.00393 H1 7 0.373246 0.224977 -0.888853 0.21490 0.00453 HKLF 4 REM s15mtw103 in P-421m #113 REM R1 = 0.0160 for 297 Fo > 4sig(Fo) and 0.0160 for all 297 data REM 43 parameters refined using 1 restraints END WGHT 0.0139 0.2137 REM Instructions for potential hydrogen bonds EQIV $1 -y+1/2, -x+1/2, z-1 HTAB O3 O2_$1 REM Highest difference peak 0.207, deepest hole -0.203, 1-sigma level 0.048 Q1 1 0.5000 0.0000 -0.1273 10.25000 0.05 0.21 Q2 1 0.7551 0.1048 -0.0062 11.00000 0.05 0.17 Q3 1 0.1480 0.0064 -0.1544 11.00000 0.05 0.16 Q4 1 0.1588 0.0511 -0.1213 11.00000 0.05 0.16 Q5 1 0.5951 0.0951 -0.3907 10.50000 0.05 0.15 Q6 1 0.5050 0.1596 -0.8657 11.00000 0.05 0.14 Q7 1 0.5736 0.0736 -0.0297 10.50000 0.05 0.14 Q8 1 0.2488 0.0921 -0.4380 11.00000 0.05 0.13 Q9 1 0.3172 0.2261 -0.3295 11.00000 0.05 0.13 Q10 1 0.0595 0.1551 -0.3819 11.00000 0.05 0.12 Q11 1 0.0878 0.2237 -0.2729 11.00000 0.05 0.12 Q12 1 0.4353 0.0647 -0.4274 10.50000 0.05 0.11 Q13 1 0.3541 -0.0223 -0.7482 11.00000 0.05 0.10 Q14 1 0.5085 0.4047 -0.9482 11.00000 0.05 0.10 Q15 1 0.0125 0.1316 -0.3617 11.00000 0.05 0.10 Q16 1 0.2765 0.0685 -0.6724 11.00000 0.05 0.09 Q17 1 0.0919 0.0050 -0.3788 11.00000 0.05 0.09 Q18 1 0.5000 0.0000 -0.5619 10.25000 0.05 0.09 Q19 1 0.6794 0.1794 -0.2616 10.50000 0.05 0.08 Q20 1 0.2861 0.2139 -0.7292 10.50000 0.05 0.08 ; _shelx_res_checksum 38455 _shelx_hkl_file ; 0 0 1 125783. 1830.39 94 0 0 1 126357. 2760.75 93 0 0 -1 120948. 2147.26 18 0 0 -1 124463. 1790.44 95 0 0 -1 130296. 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3801.59 444.990 31 8 3 1 3575.49 444.892 89 -3 -8 2 7763.72 529.070 27 3 8 2 6884.25 503.286 42 -8 -3 2 7453.63 512.019 74 8 3 2 7547.92 506.785 42 -3 8 -2 6067.75 494.200 65 -8 3 -2 6576.56 469.013 38 3 -8 -2 5749.96 490.883 56 4 8 -1 22218.9 845.093 43 4 8 -1 21227.6 833.897 68 -4 -8 -1 20293.3 800.908 25 8 -4 1 21295.7 867.304 40 4 -8 1 20099.4 895.888 67 8 -4 1 18947.2 810.092 66 -8 4 1 20000.0 804.349 38 8 4 -1 21566.7 819.711 64 4 -8 1 21045.8 935.616 59 -8 -4 -1 19622.4 770.400 31 -4 -8 0 12767.3 696.528 25 4 8 0 12268.8 680.160 68 8 4 0 13004.1 674.330 68 8 -4 0 11660.9 713.049 40 4 -8 0 11852.5 755.063 67 8 -4 0 9769.05 585.332 66 -4 8 0 12369.0 741.727 65 -8 4 0 12238.7 693.387 38 8 4 0 13325.7 666.315 64 -4 8 0 10420.3 648.539 36 4 -8 0 12164.8 784.395 59 4 -8 0 11034.5 703.081 56 -8 -4 0 12900.8 679.335 31 8 -4 0 10973.4 634.221 91 -4 -8 1 21509.4 839.919 25 8 4 1 19728.4 770.724 68 -4 8 -1 20662.9 910.803 65 -8 4 -1 21635.7 858.026 38 4 -8 -1 21448.2 962.917 59 -8 -4 1 20477.1 806.861 31 9 0 0 583.466 188.910 42 9 0 0 999.601 232.374 39 -9 0 0 672.175 196.387 63 0 -9 0 562.095 221.286 55 0 -9 0 975.401 256.336 54 0 9 0 867.592 267.929 33 0 -9 0 592.599 204.850 53 9 0 0 607.168 198.534 89 9 0 1 28570.9 921.236 42 -9 0 1 28041.1 900.191 37 9 0 -1 28952.8 930.588 89 9 1 0 32647.4 1000.65 39 -9 -1 0 33399.7 1007.71 63 -9 1 0 36759.3 1043.30 63 1 -9 0 35636.3 1137.84 55 -1 9 0 37093.3 1175.75 33 1 -9 0 37364.0 1172.75 54 1 9 0 32467.1 1097.79 33 -1 -9 0 33248.0 1063.20 53 9 -1 0 36761.6 1078.31 90 9 1 0 33685.7 1018.71 89 0 0 0 0.00 0.00 0 TITL s15mtw103 in P-42(1)m REM P-42(1)m (#113 in standard setting) CELL 1.54184 7.400719 7.400719 4.960797 90.0000 90.0000 90.0000 ZERR 1.00 0.000158 0.000158 0.000191 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z SYMM y,-x,-z SYMM -y, x,-z SYMM -x+1/2, y+1/2,-z SYMM x+1/2,-y+1/2,-z SYMM -y+1/2,-x+1/2, z SYMM y+1/2, x+1/2, z SFAC Be O Na Si Ca UNIT 1.00 7.00 1.00 2.00 2.00 TREF HKLF 4 END ; _shelx_hkl_checksum 88241