# Copyright The Royal Society of Chemistry, 1998 # MANUSCRIPT 8/02753F data_trim _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Cl6 O3 Si3' _chemical_formula_weight 344.97 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.388(2) _cell_length_b 8.646(5) _cell_length_c 11.155(4) _cell_angle_alpha 77.77(5) _cell_angle_beta 77.58(3) _cell_angle_gamma 72.93(4) _cell_volume 567.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 1.02 _exptl_crystal_size_mid 1.01 _exptl_crystal_size_min 0.68 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method ? _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 1.795 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2156 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0126 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1962 _reflns_number_observed 1836 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+0.5715P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1960 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_obs 0.0334 _refine_ls_wR_factor_all 0.0937 _refine_ls_wR_factor_obs 0.0897 _refine_ls_goodness_of_fit_all 1.109 _refine_ls_goodness_of_fit_obs 1.111 _refine_ls_restrained_S_all 1.121 _refine_ls_restrained_S_obs 1.111 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cl11 Cl 0.30332(14) -0.00514(9) 0.37603(7) 0.0352(2) Uani 1 d . . Cl32 Cl 0.22333(12) -0.55893(9) 0.37688(7) 0.0321(2) Uani 1 d . . Cl31 Cl 0.76267(12) -0.69922(9) 0.32801(7) 0.0321(2) Uani 1 d . . Cl21 Cl 0.23490(13) -0.18315(10) -0.01189(7) 0.0343(2) Uani 1 d . . Cl22 Cl 0.77655(13) -0.30036(10) -0.07505(7) 0.0343(2) Uani 1 d . . Si3 Si 0.50888(13) -0.50342(9) 0.29735(7) 0.0214(2) Uani 1 d . . Si2 Si 0.51438(13) -0.27131(9) 0.06097(7) 0.0220(2) Uani 1 d . . Si1 Si 0.54967(14) -0.17023(9) 0.29202(7) 0.0237(2) Uani 1 d . . O12 O 0.5306(4) -0.1469(2) 0.1468(2) 0.0300(5) Uani 1 d . . O13 O 0.5320(4) -0.3533(2) 0.3544(2) 0.0292(5) Uani 1 d . . Cl12 Cl 0.84145(13) -0.14182(10) 0.30870(7) 0.0352(2) Uani 1 d . . O23 O 0.5123(4) -0.4451(2) 0.1493(2) 0.0268(5) Uani 1 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 Cl11 0.0432(5) 0.0296(4) 0.0318(4) -0.0101(3) -0.0065(3) -0.0037(3) Cl32 0.0299(4) 0.0377(4) 0.0296(4) -0.0053(3) -0.0021(3) -0.0124(3) Cl31 0.0317(4) 0.0288(4) 0.0315(4) -0.0037(3) -0.0058(3) -0.0016(3) Cl21 0.0335(4) 0.0353(4) 0.0367(4) -0.0045(3) -0.0139(3) -0.0077(3) Cl22 0.0333(4) 0.0436(5) 0.0281(4) -0.0088(3) 0.0015(3) -0.0156(3) Si3 0.0303(4) 0.0181(4) 0.0175(4) -0.0032(3) -0.0046(3) -0.0081(3) Si2 0.0314(4) 0.0219(4) 0.0159(4) -0.0029(3) -0.0057(3) -0.0104(3) Si1 0.0369(5) 0.0193(4) 0.0187(4) -0.0041(3) -0.0078(3) -0.0101(3) O12 0.0524(14) 0.0215(11) 0.0209(11) -0.0006(8) -0.0110(9) -0.0152(9) O13 0.0496(13) 0.0233(11) 0.0196(10) -0.0015(8) -0.0093(9) -0.0156(9) Cl12 0.0376(4) 0.0361(4) 0.0370(4) -0.0057(3) -0.0112(3) -0.0136(3) O23 0.0441(12) 0.0217(10) 0.0196(10) -0.0046(8) -0.0085(8) -0.0128(9) _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 Cl11 Si1 2.001(2) . ? Cl32 Si3 1.9955(13) . ? Cl31 Si3 1.998(2) . ? Cl21 Si2 1.9979(13) . ? Cl22 Si2 1.9978(14) . ? Si3 O13 1.617(2) . ? Si3 O23 1.619(2) . ? Si2 O23 1.615(2) . ? Si2 O12 1.622(2) . ? Si1 O13 1.615(2) . ? Si1 O12 1.616(2) . ? Si1 Cl12 2.0016(13) . ? 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 O13 Si3 O23 107.79(11) . . ? O13 Si3 Cl32 109.66(10) . . ? O23 Si3 Cl32 110.00(9) . . ? O13 Si3 Cl31 109.85(10) . . ? O23 Si3 Cl31 109.87(10) . . ? Cl32 Si3 Cl31 109.65(6) . . ? O23 Si2 O12 107.45(11) . . ? O23 Si2 Cl22 109.71(10) . . ? O12 Si2 Cl22 110.12(10) . . ? O23 Si2 Cl21 109.85(9) . . ? O12 Si2 Cl21 109.85(10) . . ? Cl22 Si2 Cl21 109.83(6) . . ? O13 Si1 O12 107.60(11) . . ? O13 Si1 Cl11 110.04(10) . . ? O12 Si1 Cl11 110.04(10) . . ? O13 Si1 Cl12 109.82(10) . . ? O12 Si1 Cl12 110.04(10) . . ? Cl11 Si1 Cl12 109.28(6) . . ? Si1 O12 Si2 132.45(13) . . ? Si1 O13 Si3 132.24(13) . . ? Si2 O23 Si3 132.20(13) . . ? _refine_diff_density_max 0.594 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.093 #===end data_tetr _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Cl2 O Si' _chemical_formula_weight 114.99 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.9820(10) _cell_length_b 8.088(2) _cell_length_c 8.156(2) _cell_angle_alpha 77.43(2) _cell_angle_beta 81.18(2) _cell_angle_gamma 72.680(10) _cell_volume 366.02(14) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.087 _exptl_crystal_density_method ? _exptl_crystal_F_000 224 _exptl_absorpt_coefficient_mu 1.856 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1506 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1346 _reflns_number_observed 1305 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.3770P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1346 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_obs 0.0254 _refine_ls_wR_factor_all 0.0697 _refine_ls_wR_factor_obs 0.0693 _refine_ls_goodness_of_fit_all 1.222 _refine_ls_goodness_of_fit_obs 1.235 _refine_ls_restrained_S_all 1.222 _refine_ls_restrained_S_obs 1.235 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cl12 Cl 0.43066(11) 0.71593(8) 0.10029(7) 0.0231(2) Uani 1 d . . Cl11 Cl -0.12575(11) 0.87701(7) 0.21330(7) 0.0225(2) Uani 1 d . . Si1 Si 0.10898(12) 0.68544(7) 0.10997(7) 0.0130(2) Uani 1 d . . Cl22 Cl 0.28644(11) 0.11746(7) 0.32896(7) 0.0240(2) Uani 1 d . . Cl21 Cl -0.25692(12) 0.33492(9) 0.42029(7) 0.0296(2) Uani 1 d . . Si2 Si 0.02172(12) 0.32315(7) 0.24929(7) 0.0127(2) Uani 1 d . . O2 O 0.1017(3) 0.4990(2) 0.2232(2) 0.0212(4) Uani 1 d . . O1 O 0.0475(3) 0.6963(2) -0.0752(2) 0.0226(4) Uani 1 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 Cl12 0.0140(5) 0.0269(3) 0.0301(3) -0.0064(2) -0.0010(2) -0.0077(2) Cl11 0.0178(4) 0.0207(3) 0.0287(3) -0.0099(2) 0.0010(2) -0.0025(2) Si1 0.0149(5) 0.0124(3) 0.0134(3) -0.0026(2) -0.0026(2) -0.0054(2) Cl22 0.0209(4) 0.0193(3) 0.0255(3) -0.0003(2) -0.0035(2) 0.0017(2) Cl21 0.0187(4) 0.0380(3) 0.0234(3) 0.0012(2) 0.0049(2) -0.0030(3) Si2 0.0152(4) 0.0121(3) 0.0109(2) -0.0007(2) -0.0018(2) -0.0045(2) O2 0.0307(12) 0.0177(8) 0.0188(7) 0.0007(6) -0.0071(7) -0.0124(7) O1 0.0342(13) 0.0207(8) 0.0178(7) -0.0023(6) -0.0084(7) -0.0126(7) _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 Cl12 Si1 1.9993(10) . ? Cl11 Si1 1.9981(9) . ? Si1 O1 1.587(2) . ? Si1 O2 1.597(2) . ? Cl22 Si2 1.9935(9) . ? Cl21 Si2 1.9957(10) . ? Si2 O1 1.590(2) 2_565 ? Si2 O2 1.593(2) . ? O1 Si2 1.590(2) 2_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 O1 Si1 O2 110.22(9) . . ? O1 Si1 Cl11 109.19(7) . . ? O2 Si1 Cl11 109.32(8) . . ? O1 Si1 Cl12 109.67(8) . . ? O2 Si1 Cl12 109.15(8) . . ? Cl11 Si1 Cl12 109.26(4) . . ? O1 Si2 O2 109.37(9) 2_565 . ? O1 Si2 Cl22 109.92(7) 2_565 . ? O2 Si2 Cl22 109.09(8) . . ? O1 Si2 Cl21 109.17(8) 2_565 . ? O2 Si2 Cl21 109.59(8) . . ? Cl22 Si2 Cl21 109.68(4) . . ? Si2 O2 Si1 148.53(11) . . ? Si1 O1 Si2 170.73(12) . 2_565 ? _refine_diff_density_max 0.269 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.094 #===end