# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Derendorf, Janis' 'Ke\~A\"Yler, Mathias' 'Knapp, Carsten' 'R\~A1/4hle, Monika' 'Schulz, Christoph' _publ_contact_author_name 'Knapp, Carsten' _publ_contact_author_email carsten.knapp@ac.uni-freiburg.de _publ_section_title ; Alkali Metal-Sulfur Dioxide Complexes Stabilized by Halogenated closo-Dodecaborate Anions ; # Attachment '- cif.cif' data_ck-cs-01 _database_code_depnum_ccdc_archive 'CCDC 730909' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B12 Cl12, 8(O2 S), 2(Li)' _chemical_formula_sum 'B12 Cl12 Li2 O16 S8' _chemical_formula_weight 1081.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.964(2) _cell_length_b 10.285(2) _cell_length_c 10.325(2) _cell_angle_alpha 116.41(3) _cell_angle_beta 94.82(3) _cell_angle_gamma 101.32(3) _cell_volume 911.4(4) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 27.45 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.970 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 1.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.719 _exptl_absorpt_correction_T_max 0.931 _exptl_absorpt_process_details ; March 2001 T Higashi ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS Spider' _diffrn_measurement_method fsFind.ref _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17995 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4159 _reflns_number_gt 3058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+1.4756P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0034(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4159 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.4021(5) 0.3466(5) 0.3456(4) 0.0167(9) Uani 1 1 d . . . Cl1 Cl 0.30069(10) 0.18087(10) 0.18216(10) 0.0213(2) Uani 1 1 d . . . B2 B 0.3440(4) 0.4108(5) 0.5177(4) 0.0165(9) Uani 1 1 d . . . Cl2 Cl 0.18118(10) 0.31533(11) 0.53484(10) 0.0226(2) Uani 1 1 d . . . B3 B 0.4897(4) 0.3310(5) 0.4936(4) 0.0167(9) Uani 1 1 d . . . Cl3 Cl 0.48114(10) 0.15114(10) 0.48622(10) 0.0223(2) Uani 1 1 d . . . B4 B 0.5881(4) 0.3884(5) 0.3839(4) 0.0151(8) Uani 1 1 d . . . Cl4 Cl 0.67854(10) 0.26958(11) 0.25752(10) 0.0243(2) Uani 1 1 d . . . B5 B 0.5039(4) 0.5052(5) 0.3377(4) 0.0157(8) Uani 1 1 d . . . Cl5 Cl 0.51020(10) 0.50910(11) 0.16692(10) 0.0229(2) Uani 1 1 d . . . B6 B 0.3543(4) 0.5201(5) 0.4211(4) 0.0146(8) Uani 1 1 d . . . Cl6 Cl 0.19979(10) 0.54352(10) 0.33862(10) 0.0221(2) Uani 1 1 d . . . Li1 Li 0.1608(8) 0.0885(8) 0.7573(8) 0.0354(18) Uani 1 1 d . . . O1 O 0.1717(3) -0.0447(3) 0.5457(3) 0.0352(7) Uani 1 1 d . . . S1 S 0.17089(11) -0.10003(12) 0.39294(11) 0.0267(2) Uani 1 1 d . . . O2 O 0.0528(3) -0.0990(4) 0.3062(3) 0.0413(8) Uani 1 1 d . . . O3 O 0.0912(3) -0.0543(3) 0.8296(4) 0.0358(7) Uani 1 1 d . . . S2 S 0.03141(11) -0.19364(12) 0.82856(12) 0.0264(2) Uani 1 1 d . . . O4 O 0.0474(3) -0.1942(4) 0.9658(4) 0.0454(9) Uani 1 1 d . . . O5 O 0.3761(3) 0.1156(3) 0.8148(3) 0.0334(7) Uani 1 1 d . . . S3 S 0.50701(12) 0.11583(12) 0.88201(12) 0.0302(3) Uani 1 1 d . . . O6 O 0.6307(3) 0.1952(3) 0.8630(3) 0.0380(8) Uani 1 1 d . . . O7 O 0.1974(3) 0.3056(3) 0.9041(3) 0.0301(7) Uani 1 1 d . . . S4 S 0.18109(12) 0.45383(12) 0.95159(12) 0.0302(3) Uani 1 1 d . . . O8 O 0.0734(4) 0.4708(4) 0.8668(4) 0.0520(10) Uani 1 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 B1 0.023(2) 0.018(2) 0.0101(19) 0.0064(17) 0.0044(17) 0.0084(18) Cl1 0.0212(5) 0.0174(5) 0.0170(4) 0.0029(4) -0.0003(4) 0.0020(4) B2 0.020(2) 0.014(2) 0.017(2) 0.0073(17) 0.0069(17) 0.0059(17) Cl2 0.0192(5) 0.0240(5) 0.0244(5) 0.0130(4) 0.0056(4) 0.0010(4) B3 0.020(2) 0.019(2) 0.014(2) 0.0095(17) 0.0014(17) 0.0063(18) Cl3 0.0257(5) 0.0171(5) 0.0269(5) 0.0130(4) 0.0028(4) 0.0058(4) B4 0.014(2) 0.017(2) 0.015(2) 0.0070(17) 0.0033(16) 0.0053(17) Cl4 0.0232(5) 0.0229(5) 0.0228(5) 0.0056(4) 0.0076(4) 0.0090(4) B5 0.018(2) 0.015(2) 0.017(2) 0.0091(17) 0.0047(17) 0.0060(17) Cl5 0.0264(5) 0.0286(5) 0.0176(5) 0.0148(4) 0.0049(4) 0.0055(4) B6 0.015(2) 0.020(2) 0.0121(19) 0.0091(17) 0.0033(16) 0.0070(17) Cl6 0.0193(5) 0.0222(5) 0.0258(5) 0.0127(4) -0.0011(4) 0.0067(4) Li1 0.040(4) 0.027(4) 0.035(4) 0.013(3) 0.003(3) 0.002(3) O1 0.0417(19) 0.0362(18) 0.0271(16) 0.0158(14) 0.0050(14) 0.0071(15) S1 0.0254(6) 0.0264(6) 0.0260(5) 0.0105(5) 0.0055(4) 0.0060(4) O2 0.0375(19) 0.044(2) 0.0329(17) 0.0162(16) -0.0081(14) 0.0027(16) O3 0.0319(17) 0.0288(17) 0.053(2) 0.0220(16) 0.0139(15) 0.0113(14) S2 0.0236(5) 0.0249(5) 0.0284(5) 0.0109(5) 0.0061(4) 0.0052(4) O4 0.047(2) 0.061(2) 0.0406(19) 0.0319(18) 0.0124(16) 0.0198(18) O5 0.0285(17) 0.0339(17) 0.0321(17) 0.0102(14) 0.0047(13) 0.0099(14) S3 0.0333(6) 0.0273(6) 0.0278(6) 0.0126(5) 0.0028(5) 0.0052(5) O6 0.0316(17) 0.0334(18) 0.0389(18) 0.0107(15) 0.0079(14) 0.0026(14) O7 0.0288(16) 0.0265(16) 0.0336(16) 0.0136(14) 0.0046(13) 0.0066(13) S4 0.0332(6) 0.0308(6) 0.0273(6) 0.0127(5) 0.0062(5) 0.0122(5) O8 0.051(2) 0.069(3) 0.051(2) 0.033(2) 0.0093(18) 0.035(2) _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 B1 B3 1.780(6) . ? B1 B6 1.782(6) . ? B1 B5 1.783(6) . ? B1 B4 1.786(6) . ? B1 B2 1.791(6) . ? B1 Cl1 1.803(4) . ? B2 B3 1.786(6) . ? B2 Cl2 1.790(4) . ? B2 B4 1.795(6) 2_666 ? B2 B5 1.797(6) 2_666 ? B2 B6 1.799(6) . ? B3 B4 1.774(6) . ? B3 B6 1.781(6) 2_666 ? B3 B5 1.790(6) 2_666 ? B3 Cl3 1.802(4) . ? B4 B6 1.782(6) 2_666 ? B4 B5 1.792(6) . ? B4 Cl4 1.794(4) . ? B4 B2 1.795(6) 2_666 ? B5 B6 1.782(6) . ? B5 Cl5 1.788(4) . ? B5 B3 1.790(6) 2_666 ? B5 B2 1.797(6) 2_666 ? B6 B3 1.781(6) 2_666 ? B6 B4 1.782(6) 2_666 ? B6 Cl6 1.806(4) . ? Li1 O3 1.964(8) . ? Li1 O7 1.998(8) . ? Li1 O1 2.024(8) . ? Li1 O5 2.106(8) . ? Li1 O2 2.212(8) 2_556 ? O1 S1 1.418(3) . ? S1 O2 1.422(3) . ? O2 Li1 2.212(8) 2_556 ? O3 S2 1.435(3) . ? S2 O4 1.415(3) . ? O5 S3 1.424(3) . ? S3 O6 1.419(3) . ? O7 S4 1.427(3) . ? S4 O8 1.415(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 B3 B1 B6 108.1(3) . . ? B3 B1 B5 108.1(3) . . ? B6 B1 B5 60.0(2) . . ? B3 B1 B4 59.6(2) . . ? B6 B1 B4 108.0(3) . . ? B5 B1 B4 60.3(2) . . ? B3 B1 B2 60.0(2) . . ? B6 B1 B2 60.5(2) . . ? B5 B1 B2 108.7(3) . . ? B4 B1 B2 108.0(3) . . ? B3 B1 Cl1 120.6(3) . . ? B6 B1 Cl1 123.0(3) . . ? B5 B1 Cl1 122.0(3) . . ? B4 B1 Cl1 120.8(3) . . ? B2 B1 Cl1 121.6(3) . . ? B3 B2 Cl2 121.6(3) . . ? B3 B2 B1 59.7(2) . . ? Cl2 B2 B1 121.5(3) . . ? B3 B2 B4 107.3(3) . 2_666 ? Cl2 B2 B4 122.9(3) . 2_666 ? B1 B2 B4 107.0(3) . 2_666 ? B3 B2 B5 60.0(2) . 2_666 ? Cl2 B2 B5 122.1(3) . 2_666 ? B1 B2 B5 107.6(3) . 2_666 ? B4 B2 B5 59.9(2) 2_666 2_666 ? B3 B2 B6 107.1(3) . . ? Cl2 B2 B6 122.5(3) . . ? B1 B2 B6 59.5(2) . . ? B4 B2 B6 59.5(2) 2_666 . ? B5 B2 B6 107.3(3) 2_666 . ? B4 B3 B1 60.3(2) . . ? B4 B3 B6 60.2(2) . 2_666 ? B1 B3 B6 108.4(3) . 2_666 ? B4 B3 B2 108.8(3) . . ? B1 B3 B2 60.3(2) . . ? B6 B3 B2 108.5(3) 2_666 . ? B4 B3 B5 108.2(3) . 2_666 ? B1 B3 B5 108.4(3) . 2_666 ? B6 B3 B5 59.8(2) 2_666 2_666 ? B2 B3 B5 60.3(2) . 2_666 ? B4 B3 Cl3 120.8(3) . . ? B1 B3 Cl3 121.8(3) . . ? B6 B3 Cl3 120.9(3) 2_666 . ? B2 B3 Cl3 121.9(3) . . ? B5 B3 Cl3 121.8(3) 2_666 . ? B3 B4 B6 60.1(2) . 2_666 ? B3 B4 B1 60.0(2) . . ? B6 B4 B1 108.1(3) 2_666 . ? B3 B4 B5 108.0(3) . . ? B6 B4 B5 108.3(3) 2_666 . ? B1 B4 B5 59.8(2) . . ? B3 B4 Cl4 122.1(3) . . ? B6 B4 Cl4 122.9(3) 2_666 . ? B1 B4 Cl4 120.7(3) . . ? B5 B4 Cl4 120.5(3) . . ? B3 B4 B2 108.5(3) . 2_666 ? B6 B4 B2 60.4(2) 2_666 2_666 ? B1 B4 B2 108.1(3) . 2_666 ? B5 B4 B2 60.1(2) . 2_666 ? Cl4 B4 B2 121.7(3) . 2_666 ? B6 B5 B1 60.0(2) . . ? B6 B5 Cl5 122.6(3) . . ? B1 B5 Cl5 121.7(3) . . ? B6 B5 B3 59.8(2) . 2_666 ? B1 B5 B3 107.6(3) . 2_666 ? Cl5 B5 B3 122.7(3) . 2_666 ? B6 B5 B4 107.8(3) . . ? B1 B5 B4 59.9(2) . . ? Cl5 B5 B4 121.2(3) . . ? B3 B5 B4 107.3(3) 2_666 . ? B6 B5 B2 108.0(3) . 2_666 ? B1 B5 B2 108.2(3) . 2_666 ? Cl5 B5 B2 121.1(3) . 2_666 ? B3 B5 B2 59.7(2) 2_666 2_666 ? B4 B5 B2 60.0(2) . 2_666 ? B3 B6 B5 60.3(2) 2_666 . ? B3 B6 B1 108.0(3) 2_666 . ? B5 B6 B1 60.0(2) . . ? B3 B6 B4 59.7(2) 2_666 2_666 ? B5 B6 B4 108.2(3) . 2_666 ? B1 B6 B4 108.0(3) . 2_666 ? B3 B6 B2 108.0(3) 2_666 . ? B5 B6 B2 108.4(3) . . ? B1 B6 B2 60.0(2) . . ? B4 B6 B2 60.2(2) 2_666 . ? B3 B6 Cl6 121.4(3) 2_666 . ? B5 B6 Cl6 121.6(3) . . ? B1 B6 Cl6 122.3(3) . . ? B4 B6 Cl6 121.3(3) 2_666 . ? B2 B6 Cl6 121.7(3) . . ? O3 Li1 O7 115.3(4) . . ? O3 Li1 O1 103.9(3) . . ? O7 Li1 O1 140.8(4) . . ? O3 Li1 O5 98.4(3) . . ? O7 Li1 O5 86.3(3) . . ? O1 Li1 O5 88.0(3) . . ? O3 Li1 O2 91.8(3) . 2_556 ? O7 Li1 O2 86.5(3) . 2_556 ? O1 Li1 O2 92.6(3) . 2_556 ? O5 Li1 O2 169.3(4) . 2_556 ? S1 O1 Li1 162.3(3) . . ? O1 S1 O2 116.8(2) . . ? S1 O2 Li1 159.4(3) . 2_556 ? S2 O3 Li1 160.0(3) . . ? O4 S2 O3 116.9(2) . . ? S3 O5 Li1 162.6(3) . . ? O6 S3 O5 118.5(2) . . ? S4 O7 Li1 153.0(3) . . ? O8 S4 O7 117.3(2) . . ? 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 B6 B1 B2 B3 -137.6(3) . . . . ? B5 B1 B2 B3 -100.6(3) . . . . ? B4 B1 B2 B3 -36.7(3) . . . . ? Cl1 B1 B2 B3 109.6(3) . . . . ? B3 B1 B2 Cl2 -110.7(3) . . . . ? B6 B1 B2 Cl2 111.7(3) . . . . ? B5 B1 B2 Cl2 148.7(3) . . . . ? B4 B1 B2 Cl2 -147.4(3) . . . . ? Cl1 B1 B2 Cl2 -1.1(4) . . . . ? B3 B1 B2 B4 100.5(3) . . . 2_666 ? B6 B1 B2 B4 -37.1(3) . . . 2_666 ? B5 B1 B2 B4 -0.1(4) . . . 2_666 ? B4 B1 B2 B4 63.8(4) . . . 2_666 ? Cl1 B1 B2 B4 -149.9(3) . . . 2_666 ? B3 B1 B2 B5 37.5(3) . . . 2_666 ? B6 B1 B2 B5 -100.1(3) . . . 2_666 ? B5 B1 B2 B5 -63.1(4) . . . 2_666 ? B4 B1 B2 B5 0.8(4) . . . 2_666 ? Cl1 B1 B2 B5 147.1(3) . . . 2_666 ? B3 B1 B2 B6 137.6(3) . . . . ? B5 B1 B2 B6 37.0(3) . . . . ? B4 B1 B2 B6 100.9(3) . . . . ? Cl1 B1 B2 B6 -112.8(3) . . . . ? B6 B1 B3 B4 -100.7(3) . . . . ? B5 B1 B3 B4 -37.3(3) . . . . ? B2 B1 B3 B4 -138.8(3) . . . . ? Cl1 B1 B3 B4 110.0(3) . . . . ? B6 B1 B3 B6 -63.2(4) . . . 2_666 ? B5 B1 B3 B6 0.3(4) . . . 2_666 ? B4 B1 B3 B6 37.5(3) . . . 2_666 ? B2 B1 B3 B6 -101.3(3) . . . 2_666 ? Cl1 B1 B3 B6 147.6(3) . . . 2_666 ? B6 B1 B3 B2 38.1(3) . . . . ? B5 B1 B3 B2 101.5(3) . . . . ? B4 B1 B3 B2 138.8(3) . . . . ? Cl1 B1 B3 B2 -111.1(3) . . . . ? B6 B1 B3 B5 0.3(4) . . . 2_666 ? B5 B1 B3 B5 63.7(4) . . . 2_666 ? B4 B1 B3 B5 101.0(3) . . . 2_666 ? B2 B1 B3 B5 -37.8(3) . . . 2_666 ? Cl1 B1 B3 B5 -149.0(3) . . . 2_666 ? B6 B1 B3 Cl3 149.4(3) . . . . ? B5 B1 B3 Cl3 -147.2(3) . . . . ? B4 B1 B3 Cl3 -109.9(3) . . . . ? B2 B1 B3 Cl3 111.3(3) . . . . ? Cl1 B1 B3 Cl3 0.1(5) . . . . ? Cl2 B2 B3 B4 147.8(3) . . . . ? B1 B2 B3 B4 37.2(3) . . . . ? B4 B2 B3 B4 -62.8(4) 2_666 . . . ? B5 B2 B3 B4 -100.7(3) 2_666 . . . ? B6 B2 B3 B4 -0.2(4) . . . . ? Cl2 B2 B3 B1 110.6(3) . . . . ? B4 B2 B3 B1 -100.0(3) 2_666 . . . ? B5 B2 B3 B1 -137.9(3) 2_666 . . . ? B6 B2 B3 B1 -37.4(3) . . . . ? Cl2 B2 B3 B6 -148.3(3) . . . 2_666 ? B1 B2 B3 B6 101.1(3) . . . 2_666 ? B4 B2 B3 B6 1.2(4) 2_666 . . 2_666 ? B5 B2 B3 B6 -36.8(3) 2_666 . . 2_666 ? B6 B2 B3 B6 63.7(4) . . . 2_666 ? Cl2 B2 B3 B5 -111.4(3) . . . 2_666 ? B1 B2 B3 B5 137.9(3) . . . 2_666 ? B4 B2 B3 B5 38.0(3) 2_666 . . 2_666 ? B6 B2 B3 B5 100.5(3) . . . 2_666 ? Cl2 B2 B3 Cl3 -0.4(4) . . . . ? B1 B2 B3 Cl3 -111.0(3) . . . . ? B4 B2 B3 Cl3 149.0(3) 2_666 . . . ? B5 B2 B3 Cl3 111.0(3) 2_666 . . . ? B6 B2 B3 Cl3 -148.4(3) . . . . ? B1 B3 B4 B6 138.2(3) . . . 2_666 ? B2 B3 B4 B6 101.0(3) . . . 2_666 ? B5 B3 B4 B6 37.0(3) 2_666 . . 2_666 ? Cl3 B3 B4 B6 -110.3(3) . . . 2_666 ? B6 B3 B4 B1 -138.2(3) 2_666 . . . ? B2 B3 B4 B1 -37.2(3) . . . . ? B5 B3 B4 B1 -101.2(3) 2_666 . . . ? Cl3 B3 B4 B1 111.4(3) . . . . ? B1 B3 B4 B5 37.0(3) . . . . ? B6 B3 B4 B5 -101.2(3) 2_666 . . . ? B2 B3 B4 B5 -0.2(4) . . . . ? B5 B3 B4 B5 -64.2(4) 2_666 . . . ? Cl3 B3 B4 B5 148.5(3) . . . . ? B1 B3 B4 Cl4 -109.5(3) . . . . ? B6 B3 B4 Cl4 112.3(3) 2_666 . . . ? B2 B3 B4 Cl4 -146.7(3) . . . . ? B5 B3 B4 Cl4 149.3(3) 2_666 . . . ? Cl3 B3 B4 Cl4 2.0(4) . . . . ? B1 B3 B4 B2 100.7(3) . . . 2_666 ? B6 B3 B4 B2 -37.5(3) 2_666 . . 2_666 ? B2 B3 B4 B2 63.5(4) . . . 2_666 ? B5 B3 B4 B2 -0.5(4) 2_666 . . 2_666 ? Cl3 B3 B4 B2 -147.9(3) . . . 2_666 ? B6 B1 B4 B3 100.8(3) . . . . ? B5 B1 B4 B3 138.5(3) . . . . ? B2 B1 B4 B3 36.9(3) . . . . ? Cl1 B1 B4 B3 -109.8(3) . . . . ? B3 B1 B4 B6 -37.4(3) . . . 2_666 ? B6 B1 B4 B6 63.4(4) . . . 2_666 ? B5 B1 B4 B6 101.0(3) . . . 2_666 ? B2 B1 B4 B6 -0.6(4) . . . 2_666 ? Cl1 B1 B4 B6 -147.2(3) . . . 2_666 ? B3 B1 B4 B5 -138.5(3) . . . . ? B6 B1 B4 B5 -37.7(3) . . . . ? B2 B1 B4 B5 -101.6(3) . . . . ? Cl1 B1 B4 B5 111.8(3) . . . . ? B3 B1 B4 Cl4 111.8(3) . . . . ? B6 B1 B4 Cl4 -147.4(3) . . . . ? B5 B1 B4 Cl4 -109.7(3) . . . . ? B2 B1 B4 Cl4 148.6(3) . . . . ? Cl1 B1 B4 Cl4 2.0(4) . . . . ? B3 B1 B4 B2 -101.3(3) . . . 2_666 ? B6 B1 B4 B2 -0.5(4) . . . 2_666 ? B5 B1 B4 B2 37.1(3) . . . 2_666 ? B2 B1 B4 B2 -64.5(4) . . . 2_666 ? Cl1 B1 B4 B2 148.9(3) . . . 2_666 ? B3 B1 B5 B6 -100.8(3) . . . . ? B4 B1 B5 B6 -137.8(3) . . . . ? B2 B1 B5 B6 -37.2(3) . . . . ? Cl1 B1 B5 B6 112.4(3) . . . . ? B3 B1 B5 Cl5 147.2(3) . . . . ? B6 B1 B5 Cl5 -112.0(3) . . . . ? B4 B1 B5 Cl5 110.2(3) . . . . ? B2 B1 B5 Cl5 -149.2(3) . . . . ? Cl1 B1 B5 Cl5 0.4(4) . . . . ? B3 B1 B5 B3 -63.2(4) . . . 2_666 ? B6 B1 B5 B3 37.7(3) . . . 2_666 ? B4 B1 B5 B3 -100.2(3) . . . 2_666 ? B2 B1 B5 B3 0.4(4) . . . 2_666 ? Cl1 B1 B5 B3 150.1(3) . . . 2_666 ? B3 B1 B5 B4 37.0(3) . . . . ? B6 B1 B5 B4 137.8(3) . . . . ? B2 B1 B5 B4 100.6(3) . . . . ? Cl1 B1 B5 B4 -109.8(3) . . . . ? B3 B1 B5 B2 -0.1(4) . . . 2_666 ? B6 B1 B5 B2 100.7(3) . . . 2_666 ? B4 B1 B5 B2 -37.1(3) . . . 2_666 ? B2 B1 B5 B2 63.5(4) . . . 2_666 ? Cl1 B1 B5 B2 -146.9(3) . . . 2_666 ? B3 B4 B5 B6 0.5(4) . . . . ? B6 B4 B5 B6 -63.1(4) 2_666 . . . ? B1 B4 B5 B6 37.6(3) . . . . ? Cl4 B4 B5 B6 147.6(3) . . . . ? B2 B4 B5 B6 -100.9(3) 2_666 . . . ? B3 B4 B5 B1 -37.1(3) . . . . ? B6 B4 B5 B1 -100.8(3) 2_666 . . . ? Cl4 B4 B5 B1 110.0(3) . . . . ? B2 B4 B5 B1 -138.6(3) 2_666 . . . ? B3 B4 B5 Cl5 -148.2(3) . . . . ? B6 B4 B5 Cl5 148.1(3) 2_666 . . . ? B1 B4 B5 Cl5 -111.1(3) . . . . ? Cl4 B4 B5 Cl5 -1.1(4) . . . . ? B2 B4 B5 Cl5 110.3(3) 2_666 . . . ? B3 B4 B5 B3 63.5(4) . . . 2_666 ? B6 B4 B5 B3 -0.1(4) 2_666 . . 2_666 ? B1 B4 B5 B3 100.7(3) . . . 2_666 ? Cl4 B4 B5 B3 -149.3(3) . . . 2_666 ? B2 B4 B5 B3 -37.9(3) 2_666 . . 2_666 ? B3 B4 B5 B2 101.4(3) . . . 2_666 ? B6 B4 B5 B2 37.8(3) 2_666 . . 2_666 ? B1 B4 B5 B2 138.6(3) . . . 2_666 ? Cl4 B4 B5 B2 -111.5(3) . . . 2_666 ? B1 B5 B6 B3 137.6(3) . . . 2_666 ? Cl5 B5 B6 B3 -111.8(3) . . . 2_666 ? B4 B5 B6 B3 100.0(3) . . . 2_666 ? B2 B5 B6 B3 36.6(3) 2_666 . . 2_666 ? Cl5 B5 B6 B1 110.6(3) . . . . ? B3 B5 B6 B1 -137.6(3) 2_666 . . . ? B4 B5 B6 B1 -37.6(3) . . . . ? B2 B5 B6 B1 -101.0(3) 2_666 . . . ? B1 B5 B6 B4 100.7(3) . . . 2_666 ? Cl5 B5 B6 B4 -148.7(3) . . . 2_666 ? B3 B5 B6 B4 -36.9(3) 2_666 . . 2_666 ? B4 B5 B6 B4 63.1(4) . . . 2_666 ? B2 B5 B6 B4 -0.3(4) 2_666 . . 2_666 ? B1 B5 B6 B2 37.0(3) . . . . ? Cl5 B5 B6 B2 147.6(3) . . . . ? B3 B5 B6 B2 -100.7(3) 2_666 . . . ? B4 B5 B6 B2 -0.6(4) . . . . ? B2 B5 B6 B2 -64.0(4) 2_666 . . . ? B1 B5 B6 Cl6 -111.7(3) . . . . ? Cl5 B5 B6 Cl6 -1.1(5) . . . . ? B3 B5 B6 Cl6 110.7(3) 2_666 . . . ? B4 B5 B6 Cl6 -149.3(3) . . . . ? B2 B5 B6 Cl6 147.3(3) 2_666 . . . ? B3 B1 B6 B3 62.9(4) . . . 2_666 ? B5 B1 B6 B3 -38.0(3) . . . 2_666 ? B4 B1 B6 B3 -0.2(4) . . . 2_666 ? B2 B1 B6 B3 100.8(3) . . . 2_666 ? Cl1 B1 B6 B3 -148.8(3) . . . 2_666 ? B3 B1 B6 B5 100.9(3) . . . . ? B4 B1 B6 B5 37.8(3) . . . . ? B2 B1 B6 B5 138.8(3) . . . . ? Cl1 B1 B6 B5 -110.8(3) . . . . ? B3 B1 B6 B4 -0.2(4) . . . 2_666 ? B5 B1 B6 B4 -101.1(3) . . . 2_666 ? B4 B1 B6 B4 -63.3(4) . . . 2_666 ? B2 B1 B6 B4 37.7(3) . . . 2_666 ? Cl1 B1 B6 B4 148.1(3) . . . 2_666 ? B3 B1 B6 B2 -37.9(3) . . . . ? B5 B1 B6 B2 -138.8(3) . . . . ? B4 B1 B6 B2 -100.9(3) . . . . ? Cl1 B1 B6 B2 110.5(3) . . . . ? B3 B1 B6 Cl6 -148.6(3) . . . . ? B5 B1 B6 Cl6 110.5(3) . . . . ? B4 B1 B6 Cl6 148.4(3) . . . . ? B2 B1 B6 Cl6 -110.7(3) . . . . ? Cl1 B1 B6 Cl6 -0.2(5) . . . . ? B3 B2 B6 B3 -63.3(4) . . . 2_666 ? Cl2 B2 B6 B3 149.0(3) . . . 2_666 ? B1 B2 B6 B3 -100.8(3) . . . 2_666 ? B4 B2 B6 B3 37.1(3) 2_666 . . 2_666 ? B5 B2 B6 B3 -0.2(4) 2_666 . . 2_666 ? B3 B2 B6 B5 0.5(4) . . . . ? Cl2 B2 B6 B5 -147.2(3) . . . . ? B1 B2 B6 B5 -37.0(3) . . . . ? B4 B2 B6 B5 101.0(3) 2_666 . . . ? B5 B2 B6 B5 63.6(4) 2_666 . . . ? B3 B2 B6 B1 37.5(3) . . . . ? Cl2 B2 B6 B1 -110.2(3) . . . . ? B4 B2 B6 B1 137.9(3) 2_666 . . . ? B5 B2 B6 B1 100.6(3) 2_666 . . . ? B3 B2 B6 B4 -100.4(3) . . . 2_666 ? Cl2 B2 B6 B4 111.9(3) . . . 2_666 ? B1 B2 B6 B4 -137.9(3) . . . 2_666 ? B5 B2 B6 B4 -37.3(3) 2_666 . . 2_666 ? B3 B2 B6 Cl6 149.2(3) . . . . ? Cl2 B2 B6 Cl6 1.5(4) . . . . ? B1 B2 B6 Cl6 111.6(3) . . . . ? B4 B2 B6 Cl6 -110.4(3) 2_666 . . . ? B5 B2 B6 Cl6 -147.8(3) 2_666 . . . ? O3 Li1 O1 S1 149.9(8) . . . . ? O7 Li1 O1 S1 -30.4(15) . . . . ? O5 Li1 O1 S1 -112.0(10) . . . . ? O2 Li1 O1 S1 57.3(11) 2_556 . . . ? Li1 O1 S1 O2 -51.9(10) . . . . ? O1 S1 O2 Li1 -17.2(9) . . . 2_556 ? O7 Li1 O3 S2 167.6(6) . . . . ? O1 Li1 O3 S2 -12.6(11) . . . . ? O5 Li1 O3 S2 -102.6(8) . . . . ? O2 Li1 O3 S2 80.6(9) 2_556 . . . ? Li1 O3 S2 O4 165.9(8) . . . . ? O3 Li1 O5 S3 -18.7(11) . . . . ? O7 Li1 O5 S3 96.4(9) . . . . ? O1 Li1 O5 S3 -122.4(9) . . . . ? O2 Li1 O5 S3 144.0(18) 2_556 . . . ? Li1 O5 S3 O6 -167.7(9) . . . . ? O3 Li1 O7 S4 -126.2(6) . . . . ? O1 Li1 O7 S4 54.0(11) . . . . ? O5 Li1 O7 S4 136.3(5) . . . . ? O2 Li1 O7 S4 -35.8(7) 2_556 . . . ? Li1 O7 S4 O8 13.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.623 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.135 #===END data_ck-mk-02 _database_code_depnum_ccdc_archive 'CCDC 778600' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B12 Cl12, 4(O2 S), 2(Na)' _chemical_formula_sum 'B12 Cl12 Na2 O8 S4' _chemical_formula_weight 857.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.990(2) _cell_length_b 11.603(2) _cell_length_c 12.550(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.32(3) _cell_angle_gamma 90.00 _cell_volume 1435.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 1.510 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; March 2001 T Higashi ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS Spider' _diffrn_measurement_method fsFind.ref _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23470 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2820 _reflns_number_gt 2200 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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. Part of the SO2 molecules are disordered over two sites with occupancies of 0.5. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+1.1026P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2820 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.0802(3) 0.6231(2) 0.5458(2) 0.0155(6) Uani 1 1 d . . . Cl1 Cl 0.16580(6) 0.75370(5) 0.59502(5) 0.02111(15) Uani 1 1 d . . . B2 B 0.0715(3) 0.3750(2) 0.5508(2) 0.0179(6) Uani 1 1 d . . . Cl2 Cl 0.14959(7) 0.24345(5) 0.60565(6) 0.03242(19) Uani 1 1 d . . . B3 B -0.0824(3) 0.4276(2) 0.5882(2) 0.0165(6) Uani 1 1 d . . . Cl3 Cl -0.17170(7) 0.35112(6) 0.67870(6) 0.03276(18) Uani 1 1 d . . . B4 B 0.1718(3) 0.4961(2) 0.5247(2) 0.0164(6) Uani 1 1 d . . . Cl4 Cl 0.35328(6) 0.49233(5) 0.55119(6) 0.02673(16) Uani 1 1 d . . . B5 B 0.0737(3) 0.5015(2) 0.6318(2) 0.0173(6) Uani 1 1 d . . . Cl5 Cl 0.15443(7) 0.50560(6) 0.77041(5) 0.03376(18) Uani 1 1 d . . . B6 B -0.0769(3) 0.5811(2) 0.5845(2) 0.0170(6) Uani 1 1 d . . . Cl6 Cl -0.15615(7) 0.66812(6) 0.67543(6) 0.0346(2) Uani 1 1 d . . . Na1 Na 0.42677(11) 0.30522(9) 0.70479(9) 0.0300(3) Uani 1 1 d . . . O1 O 0.5547(2) 0.45900(18) 0.79176(19) 0.0440(6) Uani 1 1 d . A . S1 S 0.62184(10) 0.53419(7) 0.86861(8) 0.0507(3) Uani 1 1 d . . . O2A O 0.7594(4) 0.5038(4) 0.9280(3) 0.0417(11) Uani 0.50 1 d P A 1 O2B O 0.5619(5) 0.5017(4) 0.9710(4) 0.0540(13) Uani 0.50 1 d P . 2 O3 O 0.4990(2) 0.77874(19) 0.44461(17) 0.0421(6) Uani 1 1 d . . . S2A S 0.4956(6) 0.8060(3) 0.5555(4) 0.0354(8) Uani 0.50 1 d P B 1 O4A O 0.5248(4) 0.7104(4) 0.6267(4) 0.0432(11) Uani 0.50 1 d P B 1 S2B S 0.5123(6) 0.8404(4) 0.5387(5) 0.0382(9) Uani 0.50 1 d P B 2 O4B O 0.6063(5) 0.9323(4) 0.5453(4) 0.0471(12) Uani 0.50 1 d P B 2 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 B1 0.0140(14) 0.0136(14) 0.0190(15) 0.0005(11) 0.0029(12) -0.0019(11) Cl1 0.0213(3) 0.0166(3) 0.0254(4) -0.0047(2) 0.0039(3) -0.0051(3) B2 0.0138(14) 0.0134(14) 0.0257(17) 0.0020(11) 0.0013(13) -0.0008(11) Cl2 0.0205(4) 0.0171(3) 0.0551(5) 0.0116(3) -0.0078(3) 0.0001(3) B3 0.0174(14) 0.0175(14) 0.0151(15) -0.0012(11) 0.0039(12) -0.0040(11) Cl3 0.0372(4) 0.0420(4) 0.0206(4) 0.0018(3) 0.0092(3) -0.0205(3) B4 0.0136(13) 0.0143(13) 0.0208(14) -0.0006(12) 0.0019(11) -0.0013(11) Cl4 0.0125(3) 0.0244(3) 0.0426(4) 0.0030(3) 0.0022(3) 0.0002(3) B5 0.0184(14) 0.0193(14) 0.0136(13) 0.0006(12) 0.0004(11) -0.0040(12) Cl5 0.0405(4) 0.0412(4) 0.0159(3) 0.0053(3) -0.0067(3) -0.0203(3) B6 0.0145(14) 0.0166(14) 0.0214(16) -0.0039(11) 0.0070(12) -0.0034(11) Cl6 0.0298(4) 0.0327(4) 0.0462(5) -0.0229(3) 0.0210(3) -0.0077(3) Na1 0.0283(6) 0.0347(6) 0.0260(6) 0.0019(5) 0.0012(5) 0.0003(5) O1 0.0360(12) 0.0364(12) 0.0563(15) -0.0024(11) -0.0024(11) -0.0014(10) S1 0.0561(6) 0.0276(4) 0.0615(6) -0.0096(4) -0.0108(5) 0.0104(4) O2A 0.035(2) 0.046(3) 0.042(3) -0.007(2) -0.001(2) 0.002(2) O2B 0.076(4) 0.037(3) 0.050(3) -0.009(2) 0.012(3) 0.002(3) O3 0.0396(13) 0.0545(14) 0.0319(13) -0.0052(10) 0.0055(10) 0.0077(11) S2A 0.0350(16) 0.033(2) 0.039(2) -0.0117(15) 0.0084(13) 0.0021(15) O4A 0.037(3) 0.049(3) 0.041(3) -0.004(2) 0.000(2) -0.006(2) S2B 0.0422(17) 0.045(3) 0.0293(15) -0.0043(16) 0.0114(11) -0.0040(17) O4B 0.053(3) 0.046(3) 0.041(3) -0.009(2) 0.002(2) -0.012(2) _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 B1 B4 1.777(4) . ? B1 B2 1.781(4) 3_566 ? B1 B6 1.784(4) . ? B1 B5 1.785(4) . ? B1 B3 1.786(4) 3_566 ? B1 Cl1 1.799(3) . ? Cl1 Na1 2.8771(14) 2_556 ? B2 B1 1.781(4) 3_566 ? B2 B6 1.783(4) 3_566 ? B2 B5 1.784(4) . ? B2 B3 1.786(4) . ? B2 B4 1.787(4) . ? B2 Cl2 1.799(3) . ? Cl2 Na1 2.9348(15) . ? B3 B6 1.783(4) . ? B3 B4 1.783(4) 3_566 ? B3 B5 1.787(4) . ? B3 Cl3 1.788(3) . ? B4 B6 1.778(4) 3_566 ? B4 B5 1.788(4) . ? B4 Cl4 1.790(3) . ? Cl4 Na1 2.9172(13) . ? B5 B6 1.784(4) . ? B5 Cl5 1.795(3) . ? B6 B4 1.778(4) 3_566 ? B6 B2 1.783(4) 3_566 ? B6 Cl6 1.800(3) . ? Cl6 Na1 2.9876(15) 2_556 ? Na1 O3 2.338(2) 3_666 ? Na1 O1 2.357(2) . ? Na1 Cl1 2.8771(14) 2_546 ? Na1 Cl6 2.9876(14) 2_546 ? O1 S1 1.390(2) . ? S1 O2A 1.495(4) . ? S1 O2B 1.550(5) . ? O2B O2B 1.534(10) 3_667 ? O3 S2B 1.369(6) . ? O3 S2A 1.433(6) . ? O3 Na1 2.338(2) 3_666 ? S2A O4A 1.424(6) . ? S2B O4B 1.415(6) . ? 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 B4 B1 B2 108.11(19) . 3_566 ? B4 B1 B6 108.11(18) . . ? B2 B1 B6 60.00(16) 3_566 . ? B4 B1 B5 60.26(15) . . ? B2 B1 B5 108.15(19) 3_566 . ? B6 B1 B5 59.97(15) . . ? B4 B1 B3 60.08(16) . 3_566 ? B2 B1 B3 60.12(16) 3_566 3_566 ? B6 B1 B3 108.21(19) . 3_566 ? B5 B1 B3 108.45(19) . 3_566 ? B4 B1 Cl1 121.44(18) . . ? B2 B1 Cl1 121.91(18) 3_566 . ? B6 B1 Cl1 121.78(18) . . ? B5 B1 Cl1 121.31(18) . . ? B3 B1 Cl1 121.55(17) 3_566 . ? B1 Cl1 Na1 105.83(9) . 2_556 ? B1 B2 B6 60.10(15) 3_566 3_566 ? B1 B2 B5 107.99(19) 3_566 . ? B6 B2 B5 107.97(19) 3_566 . ? B1 B2 B3 60.07(15) 3_566 . ? B6 B2 B3 108.3(2) 3_566 . ? B5 B2 B3 60.07(15) . . ? B1 B2 B4 107.83(19) 3_566 . ? B6 B2 B4 59.75(15) 3_566 . ? B5 B2 B4 60.09(15) . . ? B3 B2 B4 108.15(19) . . ? B1 B2 Cl2 122.61(18) 3_566 . ? B6 B2 Cl2 121.90(18) 3_566 . ? B5 B2 Cl2 121.04(19) . . ? B3 B2 Cl2 121.84(18) . . ? B4 B2 Cl2 121.08(18) . . ? B2 Cl2 Na1 106.01(10) . . ? B6 B3 B4 59.80(16) . 3_566 ? B6 B3 B1 107.4(2) . 3_566 ? B4 B3 B1 59.72(15) 3_566 3_566 ? B6 B3 B2 107.62(19) . . ? B4 B3 B2 107.57(19) 3_566 . ? B1 B3 B2 59.81(15) 3_566 . ? B6 B3 B5 59.95(16) . . ? B4 B3 B5 107.75(19) 3_566 . ? B1 B3 B5 107.63(19) 3_566 . ? B2 B3 B5 59.89(16) . . ? B6 B3 Cl3 122.19(19) . . ? B4 B3 Cl3 120.93(18) 3_566 . ? B1 B3 Cl3 121.21(18) 3_566 . ? B2 B3 Cl3 122.44(18) . . ? B5 B3 Cl3 122.97(18) . . ? B1 B4 B6 108.04(19) . 3_566 ? B1 B4 B3 60.20(15) . 3_566 ? B6 B4 B3 60.10(15) 3_566 3_566 ? B1 B4 B2 107.92(19) . . ? B6 B4 B2 60.00(16) 3_566 . ? B3 B4 B2 108.23(19) 3_566 . ? B1 B4 B5 60.08(15) . . ? B6 B4 B5 107.99(19) 3_566 . ? B3 B4 B5 108.41(19) 3_566 . ? B2 B4 B5 59.86(15) . . ? B1 B4 Cl4 121.57(18) . . ? B6 B4 Cl4 121.86(18) 3_566 . ? B3 B4 Cl4 121.41(18) 3_566 . ? B2 B4 Cl4 121.85(18) . . ? B5 B4 Cl4 121.55(18) . . ? B4 Cl4 Na1 106.25(10) . . ? B2 B5 B6 107.74(19) . . ? B2 B5 B1 107.72(18) . . ? B6 B5 B1 60.01(15) . . ? B2 B5 B3 60.05(15) . . ? B6 B5 B3 59.93(15) . . ? B1 B5 B3 108.04(19) . . ? B2 B5 B4 60.05(15) . . ? B6 B5 B4 107.66(19) . . ? B1 B5 B4 59.66(15) . . ? B3 B5 B4 108.10(19) . . ? B2 B5 Cl5 122.41(18) . . ? B6 B5 Cl5 122.07(18) . . ? B1 B5 Cl5 120.72(18) . . ? B3 B5 Cl5 122.82(18) . . ? B4 B5 Cl5 120.97(18) . . ? B4 B6 B2 60.24(16) 3_566 3_566 ? B4 B6 B3 60.10(16) 3_566 . ? B2 B6 B3 108.4(2) 3_566 . ? B4 B6 B5 108.13(19) 3_566 . ? B2 B6 B5 108.11(19) 3_566 . ? B3 B6 B5 60.12(16) . . ? B4 B6 B1 108.06(19) 3_566 . ? B2 B6 B1 59.90(15) 3_566 . ? B3 B6 B1 108.20(19) . . ? B5 B6 B1 60.02(15) . . ? B4 B6 Cl6 122.52(18) 3_566 . ? B2 B6 Cl6 121.89(19) 3_566 . ? B3 B6 Cl6 121.67(18) . . ? B5 B6 Cl6 120.89(19) . . ? B1 B6 Cl6 121.06(18) . . ? B6 Cl6 Na1 103.73(10) . 2_556 ? O3 Na1 O1 117.93(9) 3_666 . ? O3 Na1 Cl1 143.36(7) 3_666 2_546 ? O1 Na1 Cl1 88.83(7) . 2_546 ? O3 Na1 Cl4 81.87(7) 3_666 . ? O1 Na1 Cl4 78.59(7) . . ? Cl1 Na1 Cl4 130.51(4) 2_546 . ? O3 Na1 Cl2 87.60(7) 3_666 . ? O1 Na1 Cl2 141.69(7) . . ? Cl1 Na1 Cl2 84.54(4) 2_546 . ? Cl4 Na1 Cl2 77.43(4) . . ? O3 Na1 Cl6 82.22(7) 3_666 2_546 ? O1 Na1 Cl6 81.72(7) . 2_546 ? Cl1 Na1 Cl6 77.22(4) 2_546 2_546 ? Cl4 Na1 Cl6 145.01(4) . 2_546 ? Cl2 Na1 Cl6 132.64(5) . 2_546 ? S1 O1 Na1 163.96(16) . . ? O1 S1 O2A 119.95(19) . . ? O1 S1 O2B 102.4(2) . . ? O2A S1 O2B 88.7(3) . . ? O2B O2B S1 148.1(5) 3_667 . ? S2B O3 Na1 155.6(3) . 3_666 ? S2A O3 Na1 158.7(3) . 3_666 ? O4A S2A O3 113.7(4) . . ? O3 S2B O4B 114.5(4) . . ? 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 B4 B1 Cl1 Na1 -119.64(19) . . . 2_556 ? B2 B1 Cl1 Na1 96.30(19) 3_566 . . 2_556 ? B6 B1 Cl1 Na1 24.2(2) . . . 2_556 ? B5 B1 Cl1 Na1 -47.6(2) . . . 2_556 ? B3 B1 Cl1 Na1 168.46(17) 3_566 . . 2_556 ? B1 B2 Cl2 Na1 163.76(18) 3_566 . . . ? B6 B2 Cl2 Na1 91.1(2) 3_566 . . . ? B5 B2 Cl2 Na1 -51.9(2) . . . . ? B3 B2 Cl2 Na1 -123.69(19) . . . . ? B4 B2 Cl2 Na1 19.7(2) . . . . ? B1 B2 B3 B6 -100.3(2) 3_566 . . . ? B6 B2 B3 B6 -63.0(3) 3_566 . . . ? B5 B2 B3 B6 37.66(19) . . . . ? B4 B2 B3 B6 0.3(3) . . . . ? Cl2 B2 B3 B6 147.7(2) . . . . ? B1 B2 B3 B4 -37.24(17) 3_566 . . 3_566 ? B6 B2 B3 B4 0.1(2) 3_566 . . 3_566 ? B5 B2 B3 B4 100.7(2) . . . 3_566 ? B4 B2 B3 B4 63.3(3) . . . 3_566 ? Cl2 B2 B3 B4 -149.23(19) . . . 3_566 ? B6 B2 B3 B1 37.29(17) 3_566 . . 3_566 ? B5 B2 B3 B1 138.0(2) . . . 3_566 ? B4 B2 B3 B1 100.5(2) . . . 3_566 ? Cl2 B2 B3 B1 -112.0(2) . . . 3_566 ? B1 B2 B3 B5 -138.0(2) 3_566 . . . ? B6 B2 B3 B5 -100.7(2) 3_566 . . . ? B4 B2 B3 B5 -37.41(18) . . . . ? Cl2 B2 B3 B5 110.1(2) . . . . ? B1 B2 B3 Cl3 109.9(2) 3_566 . . . ? B6 B2 B3 Cl3 147.20(18) 3_566 . . . ? B5 B2 B3 Cl3 -112.1(2) . . . . ? B4 B2 B3 Cl3 -149.54(19) . . . . ? Cl2 B2 B3 Cl3 -2.1(3) . . . . ? B2 B1 B4 B6 -0.2(2) 3_566 . . 3_566 ? B6 B1 B4 B6 63.3(3) . . . 3_566 ? B5 B1 B4 B6 100.8(2) . . . 3_566 ? B3 B1 B4 B6 -37.74(18) 3_566 . . 3_566 ? Cl1 B1 B4 B6 -148.58(19) . . . 3_566 ? B2 B1 B4 B3 37.55(18) 3_566 . . 3_566 ? B6 B1 B4 B3 101.0(2) . . . 3_566 ? B5 B1 B4 B3 138.54(19) . . . 3_566 ? Cl1 B1 B4 B3 -110.8(2) . . . 3_566 ? B2 B1 B4 B2 -63.6(3) 3_566 . . . ? B6 B1 B4 B2 -0.1(3) . . . . ? B5 B1 B4 B2 37.37(18) . . . . ? B3 B1 B4 B2 -101.2(2) 3_566 . . . ? Cl1 B1 B4 B2 147.99(19) . . . . ? B2 B1 B4 B5 -101.0(2) 3_566 . . . ? B6 B1 B4 B5 -37.51(18) . . . . ? B3 B1 B4 B5 -138.54(19) 3_566 . . . ? Cl1 B1 B4 B5 110.6(2) . . . . ? B2 B1 B4 Cl4 148.22(19) 3_566 . . . ? B6 B1 B4 Cl4 -148.30(19) . . . . ? B5 B1 B4 Cl4 -110.8(2) . . . . ? B3 B1 B4 Cl4 110.7(2) 3_566 . . . ? Cl1 B1 B4 Cl4 -0.2(3) . . . . ? B1 B2 B4 B1 63.4(3) 3_566 . . . ? B6 B2 B4 B1 100.9(2) 3_566 . . . ? B5 B2 B4 B1 -37.46(18) . . . . ? B3 B2 B4 B1 -0.1(3) . . . . ? Cl2 B2 B4 B1 -147.8(2) . . . . ? B1 B2 B4 B6 -37.47(18) 3_566 . . 3_566 ? B5 B2 B4 B6 -138.4(2) . . . 3_566 ? B3 B2 B4 B6 -101.0(2) . . . 3_566 ? Cl2 B2 B4 B6 111.3(2) . . . 3_566 ? B1 B2 B4 B3 -0.2(3) 3_566 . . 3_566 ? B6 B2 B4 B3 37.23(18) 3_566 . . 3_566 ? B5 B2 B4 B3 -101.1(2) . . . 3_566 ? B3 B2 B4 B3 -63.7(3) . . . 3_566 ? Cl2 B2 B4 B3 148.51(19) . . . 3_566 ? B1 B2 B4 B5 100.9(2) 3_566 . . . ? B6 B2 B4 B5 138.4(2) 3_566 . . . ? B3 B2 B4 B5 37.40(18) . . . . ? Cl2 B2 B4 B5 -110.4(2) . . . . ? B1 B2 B4 Cl4 -148.51(19) 3_566 . . . ? B6 B2 B4 Cl4 -111.0(2) 3_566 . . . ? B5 B2 B4 Cl4 110.6(2) . . . . ? B3 B2 B4 Cl4 147.99(19) . . . . ? Cl2 B2 B4 Cl4 0.2(3) . . . . ? B1 B4 Cl4 Na1 123.63(18) . . . . ? B6 B4 Cl4 Na1 -92.3(2) 3_566 . . . ? B3 B4 Cl4 Na1 -164.32(17) 3_566 . . . ? B2 B4 Cl4 Na1 -20.1(2) . . . . ? B5 B4 Cl4 Na1 51.7(2) . . . . ? B1 B2 B5 B6 -0.1(2) 3_566 . . . ? B6 B2 B5 B6 63.5(3) 3_566 . . . ? B3 B2 B5 B6 -37.68(18) . . . . ? B4 B2 B5 B6 100.6(2) . . . . ? Cl2 B2 B5 B6 -149.02(18) . . . . ? B1 B2 B5 B1 -63.4(2) 3_566 . . . ? B6 B2 B5 B1 0.1(2) 3_566 . . . ? B3 B2 B5 B1 -101.0(2) . . . . ? B4 B2 B5 B1 37.23(18) . . . . ? Cl2 B2 B5 B1 147.64(19) . . . . ? B1 B2 B5 B3 37.61(18) 3_566 . . . ? B6 B2 B5 B3 101.1(2) 3_566 . . . ? B4 B2 B5 B3 138.2(2) . . . . ? Cl2 B2 B5 B3 -111.3(2) . . . . ? B1 B2 B5 B4 -100.6(2) 3_566 . . . ? B6 B2 B5 B4 -37.10(18) 3_566 . . . ? B3 B2 B5 B4 -138.2(2) . . . . ? Cl2 B2 B5 B4 110.4(2) . . . . ? B1 B2 B5 Cl5 149.63(19) 3_566 . . . ? B6 B2 B5 Cl5 -146.83(19) 3_566 . . . ? B3 B2 B5 Cl5 112.0(2) . . . . ? B4 B2 B5 Cl5 -109.7(2) . . . . ? Cl2 B2 B5 Cl5 0.7(3) . . . . ? B4 B1 B5 B2 -37.40(18) . . . . ? B2 B1 B5 B2 63.5(3) 3_566 . . . ? B6 B1 B5 B2 100.6(2) . . . . ? B3 B1 B5 B2 -0.2(2) 3_566 . . . ? Cl1 B1 B5 B2 -148.22(19) . . . . ? B4 B1 B5 B6 -138.05(19) . . . . ? B2 B1 B5 B6 -37.13(18) 3_566 . . . ? B3 B1 B5 B6 -100.8(2) 3_566 . . . ? Cl1 B1 B5 B6 111.1(2) . . . . ? B4 B1 B5 B3 -100.8(2) . . . . ? B2 B1 B5 B3 0.1(3) 3_566 . . . ? B6 B1 B5 B3 37.21(18) . . . . ? B3 B1 B5 B3 -63.6(3) 3_566 . . . ? Cl1 B1 B5 B3 148.34(19) . . . . ? B2 B1 B5 B4 100.9(2) 3_566 . . . ? B6 B1 B5 B4 138.05(19) . . . . ? B3 B1 B5 B4 37.23(18) 3_566 . . . ? Cl1 B1 B5 B4 -110.8(2) . . . . ? B4 B1 B5 Cl5 110.2(2) . . . . ? B2 B1 B5 Cl5 -148.86(19) 3_566 . . . ? B6 B1 B5 Cl5 -111.7(2) . . . . ? B3 B1 B5 Cl5 147.45(19) 3_566 . . . ? Cl1 B1 B5 Cl5 -0.6(3) . . . . ? B6 B3 B5 B2 -137.7(2) . . . . ? B4 B3 B5 B2 -100.4(2) 3_566 . . . ? B1 B3 B5 B2 -37.40(18) 3_566 . . . ? Cl3 B3 B5 B2 111.3(2) . . . . ? B4 B3 B5 B6 37.31(18) 3_566 . . . ? B1 B3 B5 B6 100.3(2) 3_566 . . . ? B2 B3 B5 B6 137.7(2) . . . . ? Cl3 B3 B5 B6 -111.0(2) . . . . ? B6 B3 B5 B1 -37.25(18) . . . . ? B4 B3 B5 B1 0.1(3) 3_566 . . . ? B1 B3 B5 B1 63.1(3) 3_566 . . . ? B2 B3 B5 B1 100.5(2) . . . . ? Cl3 B3 B5 B1 -148.25(19) . . . . ? B6 B3 B5 B4 -100.3(2) . . . . ? B4 B3 B5 B4 -63.0(3) 3_566 . . . ? B1 B3 B5 B4 0.0(3) 3_566 . . . ? B2 B3 B5 B4 37.38(18) . . . . ? Cl3 B3 B5 B4 148.65(19) . . . . ? B6 B3 B5 Cl5 110.9(2) . . . . ? B4 B3 B5 Cl5 148.21(19) 3_566 . . . ? B1 B3 B5 Cl5 -148.78(19) 3_566 . . . ? B2 B3 B5 Cl5 -111.4(2) . . . . ? Cl3 B3 B5 Cl5 -0.1(3) . . . . ? B1 B4 B5 B2 138.11(19) . . . . ? B6 B4 B5 B2 37.22(18) 3_566 . . . ? B3 B4 B5 B2 100.8(2) 3_566 . . . ? Cl4 B4 B5 B2 -111.1(2) . . . . ? B1 B4 B5 B6 37.42(18) . . . . ? B6 B4 B5 B6 -63.5(2) 3_566 . . . ? B3 B4 B5 B6 0.2(2) 3_566 . . . ? B2 B4 B5 B6 -100.7(2) . . . . ? Cl4 B4 B5 B6 148.24(18) . . . . ? B6 B4 B5 B1 -100.9(2) 3_566 . . . ? B3 B4 B5 B1 -37.27(18) 3_566 . . . ? B2 B4 B5 B1 -138.11(19) . . . . ? Cl4 B4 B5 B1 110.8(2) . . . . ? B1 B4 B5 B3 100.7(2) . . . . ? B6 B4 B5 B3 -0.2(3) 3_566 . . . ? B3 B4 B5 B3 63.5(3) 3_566 . . . ? B2 B4 B5 B3 -37.38(18) . . . . ? Cl4 B4 B5 B3 -148.44(18) . . . . ? B1 B4 B5 Cl5 -109.8(2) . . . . ? B6 B4 B5 Cl5 149.29(19) 3_566 . . . ? B3 B4 B5 Cl5 -147.09(19) 3_566 . . . ? B2 B4 B5 Cl5 112.1(2) . . . . ? Cl4 B4 B5 Cl5 1.0(3) . . . . ? B1 B3 B6 B4 37.42(18) 3_566 . . 3_566 ? B2 B3 B6 B4 100.5(2) . . . 3_566 ? B5 B3 B6 B4 138.09(19) . . . 3_566 ? Cl3 B3 B6 B4 -109.7(2) . . . 3_566 ? B4 B3 B6 B2 -37.35(18) 3_566 . . 3_566 ? B1 B3 B6 B2 0.1(3) 3_566 . . 3_566 ? B2 B3 B6 B2 63.1(3) . . . 3_566 ? B5 B3 B6 B2 100.7(2) . . . 3_566 ? Cl3 B3 B6 B2 -147.00(19) . . . 3_566 ? B4 B3 B6 B5 -138.09(19) 3_566 . . . ? B1 B3 B6 B5 -100.7(2) 3_566 . . . ? B2 B3 B6 B5 -37.63(19) . . . . ? Cl3 B3 B6 B5 112.3(2) . . . . ? B4 B3 B6 B1 -100.8(2) 3_566 . . . ? B1 B3 B6 B1 -63.4(3) 3_566 . . . ? B2 B3 B6 B1 -0.3(3) . . . . ? B5 B3 B6 B1 37.29(19) . . . . ? Cl3 B3 B6 B1 149.54(19) . . . . ? B4 B3 B6 Cl6 112.0(2) 3_566 . . . ? B1 B3 B6 Cl6 149.37(19) 3_566 . . . ? B2 B3 B6 Cl6 -147.59(19) . . . . ? B5 B3 B6 Cl6 -110.0(2) . . . . ? Cl3 B3 B6 Cl6 2.3(3) . . . . ? B2 B5 B6 B4 0.2(3) . . . 3_566 ? B1 B5 B6 B4 100.8(2) . . . 3_566 ? B3 B5 B6 B4 -37.54(18) . . . 3_566 ? B4 B5 B6 B4 63.6(2) . . . 3_566 ? Cl5 B5 B6 B4 -149.64(19) . . . 3_566 ? B2 B5 B6 B2 -63.6(2) . . . 3_566 ? B1 B5 B6 B2 37.08(18) . . . 3_566 ? B3 B5 B6 B2 -101.3(2) . . . 3_566 ? B4 B5 B6 B2 -0.2(2) . . . 3_566 ? Cl5 B5 B6 B2 146.61(19) . . . 3_566 ? B2 B5 B6 B3 37.73(18) . . . . ? B1 B5 B6 B3 138.4(2) . . . . ? B4 B5 B6 B3 101.1(2) . . . . ? Cl5 B5 B6 B3 -112.1(2) . . . . ? B2 B5 B6 B1 -100.6(2) . . . . ? B3 B5 B6 B1 -138.4(2) . . . . ? B4 B5 B6 B1 -37.27(18) . . . . ? Cl5 B5 B6 B1 109.5(2) . . . . ? B2 B5 B6 Cl6 148.95(18) . . . . ? B1 B5 B6 Cl6 -110.4(2) . . . . ? B3 B5 B6 Cl6 111.2(2) . . . . ? B4 B5 B6 Cl6 -147.69(18) . . . . ? Cl5 B5 B6 Cl6 -0.9(3) . . . . ? B4 B1 B6 B4 -63.3(3) . . . 3_566 ? B2 B1 B6 B4 37.59(18) 3_566 . . 3_566 ? B5 B1 B6 B4 -100.9(2) . . . 3_566 ? B3 B1 B6 B4 0.3(3) 3_566 . . 3_566 ? Cl1 B1 B6 B4 148.70(19) . . . 3_566 ? B4 B1 B6 B2 -100.9(2) . . . 3_566 ? B5 B1 B6 B2 -138.5(2) . . . 3_566 ? B3 B1 B6 B2 -37.29(18) 3_566 . . 3_566 ? Cl1 B1 B6 B2 111.1(2) . . . 3_566 ? B4 B1 B6 B3 0.3(3) . . . . ? B2 B1 B6 B3 101.2(2) 3_566 . . . ? B5 B1 B6 B3 -37.34(19) . . . . ? B3 B1 B6 B3 63.9(3) 3_566 . . . ? Cl1 B1 B6 B3 -147.7(2) . . . . ? B4 B1 B6 B5 37.64(18) . . . . ? B2 B1 B6 B5 138.5(2) 3_566 . . . ? B3 B1 B6 B5 101.2(2) 3_566 . . . ? Cl1 B1 B6 B5 -110.4(2) . . . . ? B4 B1 B6 Cl6 147.79(19) . . . . ? B2 B1 B6 Cl6 -111.3(2) 3_566 . . . ? B5 B1 B6 Cl6 110.2(2) . . . . ? B3 B1 B6 Cl6 -148.62(19) 3_566 . . . ? Cl1 B1 B6 Cl6 -0.2(3) . . . . ? B4 B6 Cl6 Na1 -167.12(18) 3_566 . . 2_556 ? B2 B6 Cl6 Na1 -94.4(2) 3_566 . . 2_556 ? B3 B6 Cl6 Na1 120.4(2) . . . 2_556 ? B5 B6 Cl6 Na1 48.7(2) . . . 2_556 ? B1 B6 Cl6 Na1 -22.7(2) . . . 2_556 ? B4 Cl4 Na1 O3 111.24(11) . . . 3_666 ? B4 Cl4 Na1 O1 -128.00(11) . . . . ? B4 Cl4 Na1 Cl1 -49.52(11) . . . 2_546 ? B4 Cl4 Na1 Cl2 21.90(10) . . . . ? B4 Cl4 Na1 Cl6 174.99(11) . . . 2_546 ? B2 Cl2 Na1 O3 -104.01(12) . . . 3_666 ? B2 Cl2 Na1 O1 30.67(16) . . . . ? B2 Cl2 Na1 Cl1 111.82(10) . . . 2_546 ? B2 Cl2 Na1 Cl4 -21.80(10) . . . . ? B2 Cl2 Na1 Cl6 178.86(11) . . . 2_546 ? O3 Na1 O1 S1 -140.3(5) 3_666 . . . ? Cl1 Na1 O1 S1 13.6(5) 2_546 . . . ? Cl4 Na1 O1 S1 145.4(5) . . . . ? Cl2 Na1 O1 S1 93.2(5) . . . . ? Cl6 Na1 O1 S1 -63.7(5) 2_546 . . . ? Na1 O1 S1 O2A 79.9(6) . . . . ? Na1 O1 S1 O2B -15.8(6) . . . . ? O1 S1 O2B O2B -66.6(9) . . . 3_667 ? O2A S1 O2B O2B 172.9(9) . . . 3_667 ? S2B O3 S2A O4A -146.7(17) . . . . ? Na1 O3 S2A O4A -39.9(8) 3_666 . . . ? S2A O3 S2B O4B 156.5(18) . . . . ? Na1 O3 S2B O4B 34.1(9) 3_666 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.363 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.076 #===END data_ck-mk-04 _database_code_depnum_ccdc_archive 'CCDC 778601' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B12 Cl12, 8(O2 S), 2(K)' _chemical_formula_sum 'B12 Cl12 K2 O16 S8' _chemical_formula_weight 1145.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5370(19) _cell_length_b 20.104(4) _cell_length_c 10.242(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.48(3) _cell_angle_gamma 90.00 _cell_volume 1930.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.36 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.971 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 1.563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.848 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; March 2001 T Higashi ; _exptl_special_details ; March 2001 T Higashi ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector RX _diffrn_measurement_device_type 'Rigaku R-AXIS Spider' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79033 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0133 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4423 _reflns_number_gt 3908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+0.9479P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4423 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0248 _refine_ls_R_factor_gt 0.0199 _refine_ls_wR_factor_ref 0.0460 _refine_ls_wR_factor_gt 0.0447 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.63599(16) 0.49787(8) 0.63141(15) 0.0164(3) Uani 1 1 d . . . Cl1 Cl 0.77996(4) 0.497880(17) 0.77212(3) 0.02240(8) Uani 1 1 d . . . B2 B 0.62443(16) 0.56090(7) 0.50750(15) 0.0160(3) Uani 1 1 d . . . Cl2 Cl 0.75600(4) 0.625522(17) 0.51813(3) 0.02173(8) Uani 1 1 d . . . B3 B 0.66283(16) 0.47686(8) 0.46858(15) 0.0163(3) Uani 1 1 d . . . Cl3 Cl 0.83305(4) 0.452975(18) 0.43418(4) 0.02333(8) Uani 1 1 d . . . B4 B 0.56019(16) 0.42308(8) 0.55448(15) 0.0167(3) Uani 1 1 d . . . Cl4 Cl 0.62084(4) 0.341788(17) 0.61081(4) 0.02416(8) Uani 1 1 d . . . B5 B 0.45960(16) 0.47419(8) 0.64667(15) 0.0164(3) Uani 1 1 d . . . Cl5 Cl 0.41915(4) 0.447772(17) 0.80306(3) 0.02217(8) Uani 1 1 d . . . B6 B 0.49862(16) 0.55917(7) 0.61734(15) 0.0164(3) Uani 1 1 d . . . Cl6 Cl 0.49911(4) 0.621526(17) 0.74242(3) 0.02275(8) Uani 1 1 d . . . K1 K 0.14917(4) 0.345432(17) 0.14579(3) 0.02784(8) Uani 1 1 d . . . O1 O -0.00822(16) 0.25471(7) -0.01876(13) 0.0491(4) Uani 1 1 d . . . S1 S -0.11906(5) 0.22709(2) -0.11370(5) 0.03952(11) Uani 1 1 d . . . O2 O -0.07940(16) 0.19151(6) -0.22055(13) 0.0444(3) Uani 1 1 d . . . O3 O 0.29310(14) 0.23480(6) 0.27101(12) 0.0390(3) Uani 1 1 d . . . S2 S 0.40467(5) 0.22079(2) 0.37994(4) 0.03005(9) Uani 1 1 d . . . O4 O 0.36506(14) 0.19601(6) 0.49770(12) 0.0401(3) Uani 1 1 d . . . O5 O -0.10219(13) 0.42611(7) 0.09278(13) 0.0416(3) Uani 1 1 d . . . S3 S -0.24971(5) 0.41294(2) 0.05092(4) 0.03287(10) Uani 1 1 d . . . O6 O -0.28952(16) 0.35038(7) -0.00711(15) 0.0516(4) Uani 1 1 d . . . O7 O 0.10760(14) 0.40621(7) -0.10352(12) 0.0421(3) Uani 1 1 d . . . S4 S 0.05871(4) 0.40107(2) -0.24313(4) 0.03167(10) Uani 1 1 d . . . O8 O -0.01979(15) 0.34356(7) -0.29123(15) 0.0493(3) Uani 1 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 B1 0.0148(7) 0.0178(7) 0.0158(7) -0.0008(6) 0.0008(6) -0.0017(6) Cl1 0.01977(17) 0.02519(17) 0.01948(16) 0.00012(13) -0.00374(13) -0.00110(13) B2 0.0151(7) 0.0156(7) 0.0174(7) -0.0004(6) 0.0030(6) -0.0031(5) Cl2 0.02081(17) 0.02024(16) 0.02449(17) -0.00223(13) 0.00503(13) -0.00792(13) B3 0.0134(7) 0.0168(7) 0.0188(7) -0.0001(6) 0.0034(6) -0.0015(5) Cl3 0.01746(16) 0.02557(18) 0.02836(19) -0.00012(14) 0.00786(14) 0.00180(13) B4 0.0170(7) 0.0150(7) 0.0179(7) -0.0002(6) 0.0025(6) -0.0010(6) Cl4 0.02581(18) 0.01758(16) 0.02851(19) 0.00405(13) 0.00335(14) 0.00269(13) B5 0.0174(7) 0.0167(7) 0.0155(7) -0.0002(6) 0.0037(6) -0.0018(6) Cl5 0.02584(18) 0.02450(17) 0.01731(16) 0.00255(13) 0.00695(13) -0.00234(13) B6 0.0172(7) 0.0156(7) 0.0165(7) -0.0021(5) 0.0031(6) -0.0025(6) Cl6 0.02673(18) 0.02117(16) 0.02122(17) -0.00761(13) 0.00674(13) -0.00393(13) K1 0.02866(18) 0.02960(18) 0.02327(17) -0.00028(13) -0.00058(13) 0.00104(14) O1 0.0666(10) 0.0410(8) 0.0360(7) -0.0056(6) -0.0002(7) -0.0102(7) S1 0.0390(3) 0.0372(2) 0.0439(3) -0.0133(2) 0.0119(2) -0.00418(19) O2 0.0634(9) 0.0328(7) 0.0395(7) -0.0096(6) 0.0159(6) -0.0071(6) O3 0.0504(8) 0.0309(6) 0.0314(6) 0.0040(5) -0.0039(6) 0.0029(6) S2 0.0308(2) 0.0276(2) 0.0307(2) 0.00594(16) 0.00294(16) -0.00229(16) O4 0.0519(8) 0.0377(7) 0.0306(6) 0.0070(5) 0.0075(6) 0.0012(6) O5 0.0342(7) 0.0452(8) 0.0438(8) 0.0114(6) 0.0025(6) 0.0004(6) S3 0.0300(2) 0.0365(2) 0.0337(2) 0.00261(17) 0.01007(17) 0.00794(17) O6 0.0472(8) 0.0464(8) 0.0567(9) -0.0064(7) -0.0027(7) 0.0013(7) O7 0.0428(8) 0.0502(8) 0.0332(7) 0.0081(6) 0.0068(6) 0.0036(6) S4 0.0273(2) 0.0369(2) 0.0321(2) 0.01070(17) 0.00886(17) 0.00313(16) O8 0.0474(8) 0.0422(8) 0.0552(9) 0.0029(7) 0.0013(7) -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 B1 B5 1.782(2) . ? B1 B2 1.783(2) . ? B1 B3 1.783(2) . ? B1 B6 1.785(2) . ? B1 B4 1.788(2) . ? B1 Cl1 1.8007(16) . ? Cl1 K1 3.2984(8) 3_666 ? B2 B5 1.781(2) 3_666 ? B2 B6 1.788(2) . ? B2 B4 1.789(2) 3_666 ? B2 B3 1.789(2) . ? B2 Cl2 1.7956(15) . ? Cl2 K1 3.4460(9) 3_666 ? B3 B6 1.783(2) 3_666 ? B3 Cl3 1.7883(16) . ? B3 B4 1.793(2) . ? B3 B5 1.796(2) 3_666 ? B4 B6 1.783(2) 3_666 ? B4 B5 1.788(2) . ? B4 B2 1.789(2) 3_666 ? B4 Cl4 1.7936(16) . ? B5 B2 1.781(2) 3_666 ? B5 B6 1.786(2) . ? B5 Cl5 1.7947(16) . ? B5 B3 1.796(2) 3_666 ? B6 B3 1.783(2) 3_666 ? B6 B4 1.783(2) 3_666 ? B6 Cl6 1.7918(15) . ? Cl6 K1 3.4070(10) 3_666 ? K1 O1 2.7385(15) . ? K1 O7 2.7931(14) . ? K1 O3 2.7992(13) . ? K1 O5 2.8633(14) . ? K1 O2 2.8744(16) 4_566 ? K1 O4 2.8930(15) 4_565 ? K1 Cl1 3.2984(8) 3_666 ? K1 Cl6 3.4070(10) 3_666 ? K1 Cl2 3.4460(9) 3_666 ? O1 S1 1.4134(15) . ? S1 O2 1.4151(13) . ? O2 K1 2.8744(16) 4_565 ? O3 S2 1.4228(13) . ? S2 O4 1.4180(13) . ? O4 K1 2.8930(15) 4_566 ? O5 S3 1.4191(14) . ? S3 O6 1.4133(15) . ? O7 S4 1.4248(14) . ? S4 O8 1.4161(15) . ? 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 B5 B1 B2 108.37(11) . . ? B5 B1 B3 108.48(11) . . ? B2 B1 B3 60.23(9) . . ? B5 B1 B6 60.07(9) . . ? B2 B1 B6 60.15(9) . . ? B3 B1 B6 108.42(11) . . ? B5 B1 B4 60.10(9) . . ? B2 B1 B4 108.44(11) . . ? B3 B1 B4 60.27(9) . . ? B6 B1 B4 108.24(10) . . ? B5 B1 Cl1 121.63(10) . . ? B2 B1 Cl1 120.61(10) . . ? B3 B1 Cl1 122.02(10) . . ? B6 B1 Cl1 120.41(10) . . ? B4 B1 Cl1 122.76(10) . . ? B1 Cl1 K1 107.17(5) . 3_666 ? B5 B2 B1 108.01(10) 3_666 . ? B5 B2 B6 107.74(11) 3_666 . ? B1 B2 B6 60.00(9) . . ? B5 B2 B4 60.10(9) 3_666 3_666 ? B1 B2 B4 108.06(11) . 3_666 ? B6 B2 B4 59.80(9) . 3_666 ? B5 B2 B3 60.38(9) 3_666 . ? B1 B2 B3 59.91(9) . . ? B6 B2 B3 108.05(10) . . ? B4 B2 B3 108.61(10) 3_666 . ? B5 B2 Cl2 122.48(10) 3_666 . ? B1 B2 Cl2 121.27(10) . . ? B6 B2 Cl2 121.16(10) . . ? B4 B2 Cl2 121.54(10) 3_666 . ? B3 B2 Cl2 121.84(10) . . ? B2 Cl2 K1 103.69(5) . 3_666 ? B6 B3 B1 107.45(11) 3_666 . ? B6 B3 Cl3 121.82(10) 3_666 . ? B1 B3 Cl3 122.52(10) . . ? B6 B3 B2 107.48(11) 3_666 . ? B1 B3 B2 59.87(9) . . ? Cl3 B3 B2 121.83(10) . . ? B6 B3 B4 59.83(9) 3_666 . ? B1 B3 B4 59.99(9) . . ? Cl3 B3 B4 122.07(10) . . ? B2 B3 B4 107.94(11) . . ? B6 B3 B5 59.87(9) 3_666 3_666 ? B1 B3 B5 107.35(11) . 3_666 ? Cl3 B3 B5 121.52(10) . 3_666 ? B2 B3 B5 59.59(9) . 3_666 ? B4 B3 B5 107.77(10) . 3_666 ? B6 B4 B5 107.67(11) 3_666 . ? B6 B4 B1 107.22(11) 3_666 . ? B5 B4 B1 59.79(9) . . ? B6 B4 B2 60.07(9) 3_666 3_666 ? B5 B4 B2 59.74(9) . 3_666 ? B1 B4 B2 107.34(11) . 3_666 ? B6 B4 B3 59.80(9) 3_666 . ? B5 B4 B3 107.81(11) . . ? B1 B4 B3 59.74(8) . . ? B2 B4 B3 107.90(11) 3_666 . ? B6 B4 Cl4 121.66(10) 3_666 . ? B5 B4 Cl4 121.76(10) . . ? B1 B4 Cl4 122.93(10) . . ? B2 B4 Cl4 121.14(10) 3_666 . ? B3 B4 Cl4 122.30(10) . . ? B2 B5 B1 107.93(11) 3_666 . ? B2 B5 B6 107.68(10) 3_666 . ? B1 B5 B6 60.05(9) . . ? B2 B5 B4 60.16(9) 3_666 . ? B1 B5 B4 60.11(9) . . ? B6 B5 B4 108.22(11) . . ? B2 B5 Cl5 122.60(10) 3_666 . ? B1 B5 Cl5 121.11(10) . . ? B6 B5 Cl5 121.23(10) . . ? B4 B5 Cl5 121.62(10) . . ? B2 B5 B3 60.02(9) 3_666 3_666 ? B1 B5 B3 107.90(11) . 3_666 ? B6 B5 B3 59.70(9) . 3_666 ? B4 B5 B3 108.36(11) . 3_666 ? Cl5 B5 B3 121.96(10) . 3_666 ? B3 B6 B4 60.37(9) 3_666 3_666 ? B3 B6 B1 108.34(10) 3_666 . ? B4 B6 B1 108.20(11) 3_666 . ? B3 B6 B5 60.42(9) 3_666 . ? B4 B6 B5 108.64(10) 3_666 . ? B1 B6 B5 59.88(9) . . ? B3 B6 B2 108.40(11) 3_666 . ? B4 B6 B2 60.13(9) 3_666 . ? B1 B6 B2 59.85(9) . . ? B5 B6 B2 107.98(10) . . ? B3 B6 Cl6 121.80(10) 3_666 . ? B4 B6 Cl6 121.68(10) 3_666 . ? B1 B6 Cl6 121.25(10) . . ? B5 B6 Cl6 121.51(10) . . ? B2 B6 Cl6 121.43(10) . . ? B6 Cl6 K1 104.54(6) . 3_666 ? O1 K1 O7 75.99(5) . . ? O1 K1 O3 85.47(5) . . ? O7 K1 O3 137.96(4) . . ? O1 K1 O5 85.08(5) . . ? O7 K1 O5 66.68(4) . . ? O3 K1 O5 149.41(4) . . ? O1 K1 O2 75.09(5) . 4_566 ? O7 K1 O2 123.68(4) . 4_566 ? O3 K1 O2 85.85(4) . 4_566 ? O5 K1 O2 63.60(4) . 4_566 ? O1 K1 O4 81.27(4) . 4_565 ? O7 K1 O4 69.08(4) . 4_565 ? O3 K1 O4 71.03(4) . 4_565 ? O5 K1 O4 135.63(4) . 4_565 ? O2 K1 O4 148.09(4) 4_566 4_565 ? O1 K1 Cl1 148.97(3) . 3_666 ? O7 K1 Cl1 78.68(3) . 3_666 ? O3 K1 Cl1 125.55(3) . 3_666 ? O5 K1 Cl1 68.47(3) . 3_666 ? O2 K1 Cl1 105.27(3) 4_566 3_666 ? O4 K1 Cl1 106.04(3) 4_565 3_666 ? O1 K1 Cl6 137.11(4) . 3_666 ? O7 K1 Cl6 100.91(4) . 3_666 ? O3 K1 Cl6 68.29(3) . 3_666 ? O5 K1 Cl6 133.83(3) . 3_666 ? O2 K1 Cl6 132.53(3) 4_566 3_666 ? O4 K1 Cl6 58.75(3) 4_565 3_666 ? Cl1 K1 Cl6 65.452(12) 3_666 3_666 ? O1 K1 Cl2 137.94(3) . 3_666 ? O7 K1 Cl2 143.79(3) . 3_666 ? O3 K1 Cl2 70.08(3) . 3_666 ? O5 K1 Cl2 98.74(4) . 3_666 ? O2 K1 Cl2 69.64(4) 4_566 3_666 ? O4 K1 Cl2 119.34(3) 4_565 3_666 ? Cl1 K1 Cl2 65.113(11) 3_666 3_666 ? Cl6 K1 Cl2 64.39(3) 3_666 3_666 ? S1 O1 K1 160.52(9) . . ? O1 S1 O2 117.32(9) . . ? S1 O2 K1 146.23(8) . 4_565 ? S2 O3 K1 138.68(7) . . ? O4 S2 O3 117.36(8) . . ? S2 O4 K1 150.70(8) . 4_566 ? S3 O5 K1 134.55(8) . . ? O6 S3 O5 117.95(9) . . ? S4 O7 K1 148.41(8) . . ? O8 S4 O7 117.65(9) . . ? 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 B5 B1 Cl1 K1 -106.49(10) . . . 3_666 ? B2 B1 Cl1 K1 36.10(12) . . . 3_666 ? B3 B1 Cl1 K1 108.01(10) . . . 3_666 ? B6 B1 Cl1 K1 -35.04(12) . . . 3_666 ? B4 B1 Cl1 K1 -179.04(10) . . . 3_666 ? B5 B1 B2 B5 -63.32(14) . . . 3_666 ? B3 B1 B2 B5 37.91(10) . . . 3_666 ? B6 B1 B2 B5 -100.51(11) . . . 3_666 ? B4 B1 B2 B5 0.38(14) . . . 3_666 ? Cl1 B1 B2 B5 149.71(10) . . . 3_666 ? B5 B1 B2 B6 37.18(10) . . . . ? B3 B1 B2 B6 138.42(11) . . . . ? B4 B1 B2 B6 100.89(11) . . . . ? Cl1 B1 B2 B6 -109.79(12) . . . . ? B5 B1 B2 B4 0.24(14) . . . 3_666 ? B3 B1 B2 B4 101.47(11) . . . 3_666 ? B6 B1 B2 B4 -36.95(10) . . . 3_666 ? B4 B1 B2 B4 63.94(14) . . . 3_666 ? Cl1 B1 B2 B4 -146.73(10) . . . 3_666 ? B5 B1 B2 B3 -101.24(11) . . . . ? B6 B1 B2 B3 -138.42(11) . . . . ? B4 B1 B2 B3 -37.53(10) . . . . ? Cl1 B1 B2 B3 111.80(12) . . . . ? B5 B1 B2 Cl2 147.57(10) . . . . ? B3 B1 B2 Cl2 -111.19(12) . . . . ? B6 B1 B2 Cl2 110.39(12) . . . . ? B4 B1 B2 Cl2 -148.72(10) . . . . ? Cl1 B1 B2 Cl2 0.60(17) . . . . ? B5 B2 Cl2 K1 -179.11(10) 3_666 . . 3_666 ? B1 B2 Cl2 K1 -34.48(12) . . . 3_666 ? B6 B2 Cl2 K1 37.07(11) . . . 3_666 ? B4 B2 Cl2 K1 108.50(11) 3_666 . . 3_666 ? B3 B2 Cl2 K1 -106.22(11) . . . 3_666 ? B5 B1 B3 B6 0.58(14) . . . 3_666 ? B2 B1 B3 B6 -100.46(11) . . . 3_666 ? B6 B1 B3 B6 -63.11(14) . . . 3_666 ? B4 B1 B3 B6 37.82(10) . . . 3_666 ? Cl1 B1 B3 B6 150.02(10) . . . 3_666 ? B5 B1 B3 Cl3 -148.27(10) . . . . ? B2 B1 B3 Cl3 110.68(12) . . . . ? B6 B1 B3 Cl3 148.04(10) . . . . ? B4 B1 B3 Cl3 -111.03(12) . . . . ? Cl1 B1 B3 Cl3 1.17(17) . . . . ? B5 B1 B3 B2 101.04(12) . . . . ? B6 B1 B3 B2 37.35(10) . . . . ? B4 B1 B3 B2 138.28(11) . . . . ? Cl1 B1 B3 B2 -109.52(12) . . . . ? B5 B1 B3 B4 -37.24(10) . . . . ? B2 B1 B3 B4 -138.28(11) . . . . ? B6 B1 B3 B4 -100.93(11) . . . . ? Cl1 B1 B3 B4 112.20(12) . . . . ? B5 B1 B3 B5 63.65(14) . . . 3_666 ? B2 B1 B3 B5 -37.40(10) . . . 3_666 ? B6 B1 B3 B5 -0.04(14) . . . 3_666 ? B4 B1 B3 B5 100.89(11) . . . 3_666 ? Cl1 B1 B3 B5 -146.91(10) . . . 3_666 ? B5 B2 B3 B6 -37.35(10) 3_666 . . 3_666 ? B1 B2 B3 B6 100.42(12) . . . 3_666 ? B6 B2 B3 B6 63.22(14) . . . 3_666 ? B4 B2 B3 B6 -0.13(14) 3_666 . . 3_666 ? Cl2 B2 B3 B6 -149.33(10) . . . 3_666 ? B5 B2 B3 B1 -137.77(11) 3_666 . . . ? B6 B2 B3 B1 -37.19(10) . . . . ? B4 B2 B3 B1 -100.55(12) 3_666 . . . ? Cl2 B2 B3 B1 110.26(12) . . . . ? B5 B2 B3 Cl3 110.43(12) 3_666 . . . ? B1 B2 B3 Cl3 -111.80(13) . . . . ? B6 B2 B3 Cl3 -148.99(10) . . . . ? B4 B2 B3 Cl3 147.66(10) 3_666 . . . ? Cl2 B2 B3 Cl3 -1.54(17) . . . . ? B5 B2 B3 B4 -100.49(11) 3_666 . . . ? B1 B2 B3 B4 37.28(10) . . . . ? B6 B2 B3 B4 0.08(14) . . . . ? B4 B2 B3 B4 -63.27(14) 3_666 . . . ? Cl2 B2 B3 B4 147.54(10) . . . . ? B1 B2 B3 B5 137.77(11) . . . 3_666 ? B6 B2 B3 B5 100.57(11) . . . 3_666 ? B4 B2 B3 B5 37.22(10) 3_666 . . 3_666 ? Cl2 B2 B3 B5 -111.97(13) . . . 3_666 ? B5 B1 B4 B6 100.79(12) . . . 3_666 ? B2 B1 B4 B6 -0.25(14) . . . 3_666 ? B3 B1 B4 B6 -37.75(10) . . . 3_666 ? B6 B1 B4 B6 63.49(14) . . . 3_666 ? Cl1 B1 B4 B6 -148.77(11) . . . 3_666 ? B2 B1 B4 B5 -101.04(12) . . . . ? B3 B1 B4 B5 -138.54(11) . . . . ? B6 B1 B4 B5 -37.30(10) . . . . ? Cl1 B1 B4 B5 110.44(12) . . . . ? B5 B1 B4 B2 37.56(10) . . . 3_666 ? B2 B1 B4 B2 -63.48(14) . . . 3_666 ? B3 B1 B4 B2 -100.98(11) . . . 3_666 ? B6 B1 B4 B2 0.26(14) . . . 3_666 ? Cl1 B1 B4 B2 148.00(11) . . . 3_666 ? B5 B1 B4 B3 138.54(11) . . . . ? B2 B1 B4 B3 37.51(10) . . . . ? B6 B1 B4 B3 101.24(12) . . . . ? Cl1 B1 B4 B3 -111.01(13) . . . . ? B5 B1 B4 Cl4 -110.40(13) . . . . ? B2 B1 B4 Cl4 148.56(11) . . . . ? B3 B1 B4 Cl4 111.06(13) . . . . ? B6 B1 B4 Cl4 -147.70(11) . . . . ? Cl1 B1 B4 Cl4 0.04(17) . . . . ? B1 B3 B4 B6 137.42(11) . . . 3_666 ? Cl3 B3 B4 B6 -110.82(12) . . . 3_666 ? B2 B3 B4 B6 100.19(11) . . . 3_666 ? B5 B3 B4 B6 37.25(10) 3_666 . . 3_666 ? B6 B3 B4 B5 -100.48(11) 3_666 . . . ? B1 B3 B4 B5 36.94(10) . . . . ? Cl3 B3 B4 B5 148.70(10) . . . . ? B2 B3 B4 B5 -0.28(14) . . . . ? B5 B3 B4 B5 -63.23(14) 3_666 . . . ? B6 B3 B4 B1 -137.42(11) 3_666 . . . ? Cl3 B3 B4 B1 111.77(12) . . . . ? B2 B3 B4 B1 -37.22(10) . . . . ? B5 B3 B4 B1 -100.17(12) 3_666 . . . ? B6 B3 B4 B2 -37.38(10) 3_666 . . 3_666 ? B1 B3 B4 B2 100.03(12) . . . 3_666 ? Cl3 B3 B4 B2 -148.20(10) . . . 3_666 ? B2 B3 B4 B2 62.81(14) . . . 3_666 ? B5 B3 B4 B2 -0.13(14) 3_666 . . 3_666 ? B6 B3 B4 Cl4 110.52(12) 3_666 . . . ? B1 B3 B4 Cl4 -112.07(12) . . . . ? Cl3 B3 B4 Cl4 -0.30(17) . . . . ? B2 B3 B4 Cl4 -149.29(10) . . . . ? B5 B3 B4 Cl4 147.77(10) 3_666 . . . ? B2 B1 B5 B2 63.27(14) . . . 3_666 ? B3 B1 B5 B2 -0.58(14) . . . 3_666 ? B6 B1 B5 B2 100.49(11) . . . 3_666 ? B4 B1 B5 B2 -37.89(10) . . . 3_666 ? Cl1 B1 B5 B2 -150.16(10) . . . 3_666 ? B2 B1 B5 B6 -37.22(10) . . . . ? B3 B1 B5 B6 -101.07(12) . . . . ? B4 B1 B5 B6 -138.38(11) . . . . ? Cl1 B1 B5 B6 109.35(12) . . . . ? B2 B1 B5 B4 101.16(11) . . . . ? B3 B1 B5 B4 37.31(10) . . . . ? B6 B1 B5 B4 138.38(11) . . . . ? Cl1 B1 B5 B4 -112.27(12) . . . . ? B2 B1 B5 Cl5 -147.78(10) . . . . ? B3 B1 B5 Cl5 148.37(10) . . . . ? B6 B1 B5 Cl5 -110.56(12) . . . . ? B4 B1 B5 Cl5 111.06(12) . . . . ? Cl1 B1 B5 Cl5 -1.21(17) . . . . ? B2 B1 B5 B3 -0.15(14) . . . 3_666 ? B3 B1 B5 B3 -64.00(14) . . . 3_666 ? B6 B1 B5 B3 37.07(10) . . . 3_666 ? B4 B1 B5 B3 -101.31(11) . . . 3_666 ? Cl1 B1 B5 B3 146.42(10) . . . 3_666 ? B6 B4 B5 B2 37.62(10) 3_666 . . 3_666 ? B1 B4 B5 B2 137.65(11) . . . 3_666 ? B3 B4 B5 B2 100.73(11) . . . 3_666 ? Cl4 B4 B5 B2 -110.06(12) . . . 3_666 ? B6 B4 B5 B1 -100.03(11) 3_666 . . . ? B2 B4 B5 B1 -137.65(11) 3_666 . . . ? B3 B4 B5 B1 -36.91(10) . . . . ? Cl4 B4 B5 B1 112.29(12) . . . . ? B6 B4 B5 B6 -62.74(14) 3_666 . . . ? B1 B4 B5 B6 37.29(10) . . . . ? B2 B4 B5 B6 -100.36(11) 3_666 . . . ? B3 B4 B5 B6 0.38(14) . . . . ? Cl4 B4 B5 B6 149.59(10) . . . . ? B6 B4 B5 Cl5 149.73(10) 3_666 . . . ? B1 B4 B5 Cl5 -110.24(12) . . . . ? B2 B4 B5 Cl5 112.11(12) 3_666 . . . ? B3 B4 B5 Cl5 -147.16(10) . . . . ? Cl4 B4 B5 Cl5 2.05(17) . . . . ? B6 B4 B5 B3 0.50(14) 3_666 . . 3_666 ? B1 B4 B5 B3 100.53(11) . . . 3_666 ? B2 B4 B5 B3 -37.12(10) 3_666 . . 3_666 ? B3 B4 B5 B3 63.61(14) . . . 3_666 ? Cl4 B4 B5 B3 -147.18(10) . . . 3_666 ? B5 B1 B6 B3 -37.49(10) . . . 3_666 ? B2 B1 B6 B3 101.07(12) . . . 3_666 ? B3 B1 B6 B3 63.68(14) . . . 3_666 ? B4 B1 B6 B3 -0.18(14) . . . 3_666 ? Cl1 B1 B6 B3 -148.82(10) . . . 3_666 ? B5 B1 B6 B4 -101.44(11) . . . 3_666 ? B2 B1 B6 B4 37.12(10) . . . 3_666 ? B3 B1 B6 B4 -0.26(14) . . . 3_666 ? B4 B1 B6 B4 -64.12(14) . . . 3_666 ? Cl1 B1 B6 B4 147.24(10) . . . 3_666 ? B2 B1 B6 B5 138.56(11) . . . . ? B3 B1 B6 B5 101.17(11) . . . . ? B4 B1 B6 B5 37.32(10) . . . . ? Cl1 B1 B6 B5 -111.33(12) . . . . ? B5 B1 B6 B2 -138.56(11) . . . . ? B3 B1 B6 B2 -37.39(10) . . . . ? B4 B1 B6 B2 -101.24(11) . . . . ? Cl1 B1 B6 B2 110.11(12) . . . . ? B5 B1 B6 Cl6 110.78(12) . . . . ? B2 B1 B6 Cl6 -110.66(12) . . . . ? B3 B1 B6 Cl6 -148.05(10) . . . . ? B4 B1 B6 Cl6 148.09(10) . . . . ? Cl1 B1 B6 Cl6 -0.55(16) . . . . ? B2 B5 B6 B3 37.47(10) 3_666 . . 3_666 ? B1 B5 B6 B3 138.37(11) . . . 3_666 ? B4 B5 B6 B3 101.05(11) . . . 3_666 ? Cl5 B5 B6 B3 -111.26(12) . . . 3_666 ? B2 B5 B6 B4 -0.22(14) 3_666 . . 3_666 ? B1 B5 B6 B4 100.68(12) . . . 3_666 ? B4 B5 B6 B4 63.37(14) . . . 3_666 ? Cl5 B5 B6 B4 -148.95(10) . . . 3_666 ? B3 B5 B6 B4 -37.69(10) 3_666 . . 3_666 ? B2 B5 B6 B1 -100.90(12) 3_666 . . . ? B4 B5 B6 B1 -37.32(10) . . . . ? Cl5 B5 B6 B1 110.37(12) . . . . ? B3 B5 B6 B1 -138.37(11) 3_666 . . . ? B2 B5 B6 B2 -63.91(14) 3_666 . . . ? B1 B5 B6 B2 36.99(10) . . . . ? B4 B5 B6 B2 -0.33(14) . . . . ? Cl5 B5 B6 B2 147.36(10) . . . . ? B3 B5 B6 B2 -101.38(11) 3_666 . . . ? B2 B5 B6 Cl6 148.74(10) 3_666 . . . ? B1 B5 B6 Cl6 -110.35(12) . . . . ? B4 B5 B6 Cl6 -147.67(10) . . . . ? Cl5 B5 B6 Cl6 0.02(17) . . . . ? B3 B5 B6 Cl6 111.28(13) 3_666 . . . ? B5 B2 B6 B3 -0.01(14) 3_666 . . 3_666 ? B1 B2 B6 B3 -100.97(11) . . . 3_666 ? B4 B2 B6 B3 37.64(10) 3_666 . . 3_666 ? B3 B2 B6 B3 -63.82(14) . . . 3_666 ? Cl2 B2 B6 B3 148.46(10) . . . 3_666 ? B5 B2 B6 B4 -37.65(10) 3_666 . . 3_666 ? B1 B2 B6 B4 -138.61(11) . . . 3_666 ? B3 B2 B6 B4 -101.46(11) . . . 3_666 ? Cl2 B2 B6 B4 110.82(12) . . . 3_666 ? B5 B2 B6 B1 100.96(11) 3_666 . . . ? B4 B2 B6 B1 138.61(11) 3_666 . . . ? B3 B2 B6 B1 37.15(10) . . . . ? Cl2 B2 B6 B1 -110.57(12) . . . . ? B5 B2 B6 B5 63.95(14) 3_666 . . . ? B1 B2 B6 B5 -37.01(10) . . . . ? B4 B2 B6 B5 101.60(11) 3_666 . . . ? B3 B2 B6 B5 0.15(14) . . . . ? Cl2 B2 B6 B5 -147.57(10) . . . . ? B5 B2 B6 Cl6 -148.67(10) 3_666 . . . ? B1 B2 B6 Cl6 110.37(12) . . . . ? B4 B2 B6 Cl6 -111.02(12) 3_666 . . . ? B3 B2 B6 Cl6 147.52(10) . . . . ? Cl2 B2 B6 Cl6 -0.20(17) . . . . ? B3 B6 Cl6 K1 178.04(10) 3_666 . . 3_666 ? B4 B6 Cl6 K1 -109.47(11) 3_666 . . 3_666 ? B1 B6 Cl6 K1 34.01(12) . . . 3_666 ? B5 B6 Cl6 K1 105.56(11) . . . 3_666 ? B2 B6 Cl6 K1 -37.46(12) . . . 3_666 ? O7 K1 O1 S1 -53.4(3) . . . . ? O3 K1 O1 S1 164.6(3) . . . . ? O5 K1 O1 S1 13.8(3) . . . . ? O2 K1 O1 S1 77.7(3) 4_566 . . . ? O4 K1 O1 S1 -123.9(3) 4_565 . . . ? Cl1 K1 O1 S1 -17.2(3) 3_666 . . . ? Cl6 K1 O1 S1 -144.4(3) 3_666 . . . ? Cl2 K1 O1 S1 111.4(3) 3_666 . . . ? K1 O1 S1 O2 128.9(3) . . . . ? O1 S1 O2 K1 -7.60(18) . . . 4_565 ? O1 K1 O3 S2 -178.82(13) . . . . ? O7 K1 O3 S2 117.95(11) . . . . ? O5 K1 O3 S2 -106.46(13) . . . . ? O2 K1 O3 S2 -103.48(12) 4_566 . . . ? O4 K1 O3 S2 98.86(12) 4_565 . . . ? Cl1 K1 O3 S2 2.35(14) 3_666 . . . ? Cl6 K1 O3 S2 35.83(11) 3_666 . . . ? Cl2 K1 O3 S2 -33.64(11) 3_666 . . . ? K1 O3 S2 O4 103.75(12) . . . . ? O3 S2 O4 K1 0.23(19) . . . 4_566 ? O1 K1 O5 S3 23.26(11) . . . . ? O7 K1 O5 S3 100.12(11) . . . . ? O3 K1 O5 S3 -49.20(15) . . . . ? O2 K1 O5 S3 -52.52(10) 4_566 . . . ? O4 K1 O5 S3 95.46(11) 4_565 . . . ? Cl1 K1 O5 S3 -173.31(12) 3_666 . . . ? Cl6 K1 O5 S3 -177.24(8) 3_666 . . . ? Cl2 K1 O5 S3 -114.53(11) 3_666 . . . ? K1 O5 S3 O6 -17.12(15) . . . . ? O1 K1 O7 S4 -8.69(15) . . . . ? O3 K1 O7 S4 57.84(18) . . . . ? O5 K1 O7 S4 -99.34(16) . . . . ? O2 K1 O7 S4 -69.69(16) 4_566 . . . ? O4 K1 O7 S4 77.18(15) 4_565 . . . ? Cl1 K1 O7 S4 -170.60(16) 3_666 . . . ? Cl6 K1 O7 S4 127.44(15) 3_666 . . . ? Cl2 K1 O7 S4 -171.37(12) 3_666 . . . ? K1 O7 S4 O8 10.47(19) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.230 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.050 #===END data_ck-mk-06 _database_code_depnum_ccdc_archive 'CCDC 778602' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B12 Cl12, 4(O2 S), 2(Rb)' _chemical_formula_sum 'B12 Cl12 O8 Rb2 S4' _chemical_formula_weight 982.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 21.501(4) _cell_length_b 9.2983(19) _cell_length_c 15.361(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3071.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.19 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 4.533 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.549 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; March 2001 T Higashi ; _exptl_special_details ; March 2001 T Higashi ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector RX _diffrn_measurement_device_type 'Rigaku R-AXIS Spider' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 97793 _diffrn_reflns_av_R_equivalents 0.0901 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5386 _reflns_number_gt 4900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+6.3326P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00124(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(7) _refine_ls_number_reflns 5386 _refine_ls_number_parameters 344 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rb1 Rb 0.43237(3) 0.27911(6) 0.66174(4) 0.04200(17) Uani 1 1 d . . . Rb2 Rb 0.68782(3) 0.23219(6) 0.41686(4) 0.03803(16) Uani 1 1 d . . . B1 B 0.7948(3) 0.5561(7) 0.5735(4) 0.0246(13) Uani 1 1 d . . . Cl1 Cl 0.77985(7) 0.37366(14) 0.60424(9) 0.0315(3) Uani 1 1 d . . . B2 B 0.8448(3) 0.6677(7) 0.6380(4) 0.0260(14) Uani 1 1 d . . . Cl2 Cl 0.88234(6) 0.59892(15) 0.73335(9) 0.0314(3) Uani 1 1 d . . . B3 B 0.8689(3) 0.6117(7) 0.5333(4) 0.0282(15) Uani 1 1 d . . . Cl3 Cl 0.93103(6) 0.48539(15) 0.51588(10) 0.0333(3) Uani 1 1 d . . . B4 B 0.8021(3) 0.6115(7) 0.4624(4) 0.0286(15) Uani 1 1 d . . . Cl4 Cl 0.79626(7) 0.48561(16) 0.37471(10) 0.0357(3) Uani 1 1 d . . . B5 B 0.7375(3) 0.6678(7) 0.5253(4) 0.0283(14) Uani 1 1 d . . . Cl5 Cl 0.66040(7) 0.60393(16) 0.50321(10) 0.0344(3) Uani 1 1 d . . . B6 B 0.7635(3) 0.7039(6) 0.6350(4) 0.0245(14) Uani 1 1 d . . . Cl6 Cl 0.71443(6) 0.67823(14) 0.72730(10) 0.0311(3) Uani 1 1 d . . . B7 B 0.8831(3) 0.7908(6) 0.5665(4) 0.0248(13) Uani 1 1 d . . . Cl7 Cl 0.96043(6) 0.85449(15) 0.58869(10) 0.0322(3) Uani 1 1 d . . . B8 B 0.8561(3) 0.7558(6) 0.4584(4) 0.0249(13) Uani 1 1 d . . . Cl8 Cl 0.90734(7) 0.78133(16) 0.36764(9) 0.0351(3) Uani 1 1 d . . . B9 B 0.7755(3) 0.7923(7) 0.4545(4) 0.0271(14) Uani 1 1 d . . . Cl9 Cl 0.73778(7) 0.85890(16) 0.35832(10) 0.0363(3) Uani 1 1 d . . . B10 B 0.7511(3) 0.8482(7) 0.5604(4) 0.0266(14) Uani 1 1 d . . . Cl10 Cl 0.69013(6) 0.97568(15) 0.57700(10) 0.0345(3) Uani 1 1 d . . . B11 B 0.8187(3) 0.8482(7) 0.6297(5) 0.0284(14) Uani 1 1 d . . . Cl11 Cl 0.82575(7) 0.97274(14) 0.71805(10) 0.0337(3) Uani 1 1 d . . . B12 B 0.8246(3) 0.9028(7) 0.5178(4) 0.0273(14) Uani 1 1 d . . . Cl12 Cl 0.84045(7) 1.08556(14) 0.48700(10) 0.0325(3) Uani 1 1 d . . . O1 O 0.9201(2) 0.5166(5) 0.9250(3) 0.0516(12) Uani 1 1 d . . . S1 S 0.93835(8) 0.3698(2) 0.92642(12) 0.0458(4) Uani 1 1 d . . . O2 O 0.9364(2) 0.2913(6) 0.8472(3) 0.0577(14) Uani 1 1 d . . . O3 O 0.6249(2) 0.2741(5) 0.5928(3) 0.0533(13) Uani 1 1 d . . . S2 S 0.61810(7) 0.37402(18) 0.66209(12) 0.0426(4) Uani 1 1 d . . . O4 O 0.5572(2) 0.4237(5) 0.6821(3) 0.0487(12) Uani 1 1 d . . . O5 O 0.5357(2) 1.0553(5) 0.6998(4) 0.0644(15) Uani 1 1 d . . . S3 S 0.55838(10) 0.9175(2) 0.71808(17) 0.0712(6) Uani 1 1 d . . . O6 O 0.5421(3) 0.8498(7) 0.7957(4) 0.092(2) Uani 1 1 d . . . O7 O 0.4963(3) 0.3191(6) 0.4871(4) 0.0650(14) Uani 1 1 d . . . S4 S 0.50292(9) 0.39042(19) 0.40538(14) 0.0537(5) Uani 1 1 d . . . O8 O 0.5634(3) 0.4015(8) 0.3728(5) 0.100(2) Uani 1 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 Rb1 0.0414(3) 0.0376(3) 0.0470(4) -0.0017(3) -0.0019(3) 0.0049(3) Rb2 0.0409(3) 0.0385(3) 0.0346(3) 0.0013(3) -0.0012(3) -0.0067(3) B1 0.021(3) 0.028(3) 0.025(3) 0.002(3) 0.002(3) 0.004(2) Cl1 0.0338(8) 0.0228(7) 0.0379(8) 0.0034(6) 0.0023(6) -0.0004(6) B2 0.026(3) 0.027(3) 0.026(3) -0.002(3) 0.003(3) 0.005(3) Cl2 0.0317(7) 0.0376(7) 0.0249(7) 0.0045(6) -0.0040(6) 0.0039(6) B3 0.026(3) 0.029(3) 0.029(4) 0.006(3) 0.002(3) -0.001(3) Cl3 0.0300(8) 0.0306(7) 0.0393(8) 0.0008(6) 0.0055(6) 0.0083(6) B4 0.024(3) 0.034(4) 0.027(3) 0.000(3) -0.001(3) -0.002(3) Cl4 0.0434(8) 0.0348(8) 0.0289(8) -0.0075(6) 0.0003(7) -0.0064(6) B5 0.028(3) 0.028(3) 0.029(4) 0.001(3) 0.002(3) 0.005(3) Cl5 0.0272(7) 0.0355(7) 0.0405(9) 0.0057(6) -0.0060(7) -0.0052(6) B6 0.024(3) 0.028(3) 0.022(3) 0.002(2) -0.004(3) -0.001(3) Cl6 0.0318(8) 0.0338(7) 0.0276(7) 0.0039(6) 0.0055(6) 0.0004(6) B7 0.025(3) 0.028(3) 0.021(3) 0.001(3) -0.006(3) -0.003(3) Cl7 0.0256(7) 0.0339(7) 0.0372(8) -0.0012(6) -0.0027(6) -0.0044(6) B8 0.025(3) 0.023(3) 0.026(3) -0.002(3) -0.002(3) 0.001(3) Cl8 0.0358(8) 0.0427(9) 0.0268(8) 0.0021(6) 0.0074(6) -0.0032(6) B9 0.023(3) 0.031(3) 0.027(3) -0.001(3) 0.000(3) -0.001(3) Cl9 0.0380(8) 0.0420(8) 0.0290(8) 0.0092(7) -0.0087(7) -0.0009(6) B10 0.030(3) 0.026(3) 0.024(3) 0.002(3) 0.002(3) 0.001(3) Cl10 0.0307(7) 0.0317(7) 0.0410(9) 0.0057(6) 0.0028(7) 0.0097(6) B11 0.028(3) 0.024(3) 0.032(4) 0.005(3) -0.005(3) -0.002(3) Cl11 0.0388(8) 0.0320(7) 0.0304(8) -0.0074(6) 0.0043(7) -0.0037(6) B12 0.028(4) 0.025(3) 0.029(4) 0.006(3) -0.001(3) 0.002(3) Cl12 0.0357(8) 0.0243(7) 0.0376(8) 0.0042(6) 0.0018(7) -0.0018(6) O1 0.045(3) 0.062(3) 0.048(3) 0.010(3) -0.007(2) 0.009(2) S1 0.0349(9) 0.0570(11) 0.0455(10) 0.0131(9) -0.0067(8) -0.0030(7) O2 0.043(3) 0.074(4) 0.056(3) -0.005(3) 0.011(2) -0.001(2) O3 0.054(3) 0.039(3) 0.067(4) -0.005(2) 0.007(3) 0.003(2) S2 0.0347(8) 0.0500(9) 0.0433(10) 0.0092(8) 0.0005(8) -0.0014(7) O4 0.045(3) 0.055(3) 0.046(3) 0.010(2) 0.000(2) 0.015(2) O5 0.054(3) 0.049(3) 0.090(4) 0.014(3) -0.013(3) -0.002(2) S3 0.0610(13) 0.0667(13) 0.0860(17) 0.0204(12) 0.0272(13) 0.0091(10) O6 0.080(4) 0.109(5) 0.085(5) 0.045(4) -0.021(4) -0.033(4) O7 0.070(4) 0.064(3) 0.061(4) -0.006(3) 0.002(3) -0.003(3) S4 0.0459(10) 0.0485(10) 0.0667(13) -0.0123(9) 0.0066(9) -0.0008(8) O8 0.068(4) 0.127(6) 0.106(5) -0.042(5) 0.039(4) -0.044(4) _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 Rb1 O2 2.925(5) 3_455 ? Rb1 O4 3.017(5) . ? Rb1 O7 3.038(6) . ? Rb1 O5 3.100(5) 1_545 ? Rb1 Cl3 3.3271(17) 3_455 ? Rb1 Cl11 3.3657(15) 3_465 ? Rb1 Cl12 3.5629(17) 3_465 ? Rb1 Cl7 3.6373(17) 3_465 ? Rb1 Cl1 3.6812(17) 3_455 ? Rb1 Cl2 3.8370(16) 3_455 ? Rb2 O3 3.047(5) . ? Rb2 O1 3.068(4) 4_644 ? Rb2 O8 3.177(7) . ? Rb2 Cl4 3.3776(16) . ? Rb2 Cl10 3.4267(16) 1_545 ? Rb2 Cl2 3.4289(16) 4_644 ? Rb2 Cl6 3.6260(17) 4_644 ? Rb2 Cl12 3.7133(17) 1_545 ? Rb2 Cl1 3.7324(17) . ? Rb2 Cl9 3.7429(18) 1_545 ? Rb2 Cl5 3.7490(17) . ? Rb2 Cl11 3.7967(17) 4_644 ? B1 B5 1.774(8) . ? B1 B3 1.785(9) . ? B1 B4 1.789(9) . ? B1 Cl1 1.790(6) . ? B1 B2 1.792(9) . ? B1 B6 1.798(8) . ? Cl1 Rb1 3.6812(17) 3 ? B2 B3 1.768(9) . ? B2 B11 1.774(9) . ? B2 B6 1.780(8) . ? B2 B7 1.788(9) . ? B2 Cl2 1.790(6) . ? Cl2 Rb2 3.4289(16) 4_655 ? Cl2 Rb1 3.8370(16) 3 ? B3 B7 1.768(9) . ? B3 B8 1.787(9) . ? B3 Cl3 1.799(7) . ? B3 B4 1.804(9) . ? Cl3 Rb1 3.3271(17) 3 ? B4 B5 1.770(9) . ? B4 B8 1.776(9) . ? B4 B9 1.780(9) . ? B4 Cl4 1.789(7) . ? B5 B9 1.786(9) . ? B5 B10 1.786(9) . ? B5 Cl5 1.793(7) . ? B5 B6 1.808(9) . ? B6 Cl6 1.784(6) . ? B6 B10 1.785(9) . ? B6 B11 1.792(9) . ? Cl6 Rb2 3.6260(17) 4_655 ? B7 B11 1.774(9) . ? B7 B8 1.789(9) . ? B7 B12 1.796(9) . ? B7 Cl7 1.797(6) . ? Cl7 Rb1 3.6373(17) 3_565 ? B8 B9 1.767(9) . ? B8 B12 1.777(9) . ? B8 Cl8 1.793(7) . ? B9 B12 1.766(9) . ? B9 B10 1.787(9) . ? B9 Cl9 1.795(7) . ? Cl9 Rb2 3.7429(18) 1_565 ? B10 B12 1.785(9) . ? B10 Cl10 1.786(6) . ? B10 B11 1.801(9) . ? Cl10 Rb2 3.4267(16) 1_565 ? B11 Cl11 1.791(7) . ? B11 B12 1.796(9) . ? Cl11 Rb1 3.3657(16) 3_565 ? Cl11 Rb2 3.7967(17) 4_655 ? B12 Cl12 1.797(6) . ? Cl12 Rb1 3.5629(17) 3_565 ? Cl12 Rb2 3.7133(17) 1_565 ? O1 S1 1.421(5) . ? O1 Rb2 3.068(4) 4_655 ? S1 O2 1.419(5) . ? O2 Rb1 2.925(5) 3 ? O3 S2 1.420(5) . ? S2 O4 1.423(5) . ? O5 S3 1.399(5) . ? O5 Rb1 3.100(5) 1_565 ? S3 O6 1.393(6) . ? O7 S4 1.426(6) . ? S4 O8 1.397(6) . ? 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 O2 Rb1 O4 88.44(13) 3_455 . ? O2 Rb1 O7 151.00(14) 3_455 . ? O4 Rb1 O7 68.56(14) . . ? O2 Rb1 O5 69.21(14) 3_455 1_545 ? O4 Rb1 O5 69.03(12) . 1_545 ? O7 Rb1 O5 85.65(15) . 1_545 ? O2 Rb1 Cl3 119.39(11) 3_455 3_455 ? O4 Rb1 Cl3 114.00(9) . 3_455 ? O7 Rb1 Cl3 59.96(11) . 3_455 ? O5 Rb1 Cl3 68.72(11) 1_545 3_455 ? O2 Rb1 Cl11 85.59(10) 3_455 3_465 ? O4 Rb1 Cl11 105.88(9) . 3_465 ? O7 Rb1 Cl11 116.83(11) . 3_465 ? O5 Rb1 Cl11 154.16(11) 1_545 3_465 ? Cl3 Rb1 Cl11 132.37(4) 3_455 3_465 ? O2 Rb1 Cl12 146.03(9) 3_455 3_465 ? O4 Rb1 Cl12 114.44(9) . 3_465 ? O7 Rb1 Cl12 62.76(11) . 3_465 ? O5 Rb1 Cl12 140.96(11) 1_545 3_465 ? Cl3 Rb1 Cl12 75.46(4) 3_455 3_465 ? Cl11 Rb1 Cl12 64.77(4) 3_465 3_465 ? O2 Rb1 Cl7 120.35(11) 3_455 3_465 ? O4 Rb1 Cl7 57.79(8) . 3_465 ? O7 Rb1 Cl7 62.48(11) . 3_465 ? O5 Rb1 Cl7 124.60(10) 1_545 3_465 ? Cl3 Rb1 Cl7 119.08(4) 3_455 3_465 ? Cl11 Rb1 Cl7 63.26(3) 3_465 3_465 ? Cl12 Rb1 Cl7 61.89(3) 3_465 3_465 ? O2 Rb1 Cl1 99.99(10) 3_455 3_455 ? O4 Rb1 Cl1 171.46(9) . 3_455 ? O7 Rb1 Cl1 103.79(11) . 3_455 ? O5 Rb1 Cl1 115.14(10) 1_545 3_455 ? Cl3 Rb1 Cl1 62.97(3) 3_455 3_455 ? Cl11 Rb1 Cl1 73.71(4) 3_465 3_455 ? Cl12 Rb1 Cl1 57.41(3) 3_465 3_455 ? Cl7 Rb1 Cl1 115.80(3) 3_465 3_455 ? O2 Rb1 Cl2 61.57(11) 3_455 3_455 ? O4 Rb1 Cl2 128.89(9) . 3_455 ? O7 Rb1 Cl2 119.48(11) . 3_455 ? O5 Rb1 Cl2 62.10(9) 1_545 3_455 ? Cl3 Rb1 Cl2 60.89(4) 3_455 3_455 ? Cl11 Rb1 Cl2 111.31(4) 3_465 3_455 ? Cl12 Rb1 Cl2 112.58(3) 3_465 3_455 ? Cl7 Rb1 Cl2 173.21(3) 3_465 3_455 ? Cl1 Rb1 Cl2 57.69(3) 3_455 3_455 ? O3 Rb2 O1 73.23(13) . 4_644 ? O3 Rb2 O8 75.61(15) . . ? O1 Rb2 O8 72.30(14) 4_644 . ? O3 Rb2 Cl4 112.79(9) . . ? O1 Rb2 Cl4 170.23(10) 4_644 . ? O8 Rb2 Cl4 101.23(12) . . ? O3 Rb2 Cl10 57.24(9) . 1_545 ? O1 Rb2 Cl10 61.76(9) 4_644 1_545 ? O8 Rb2 Cl10 120.66(12) . 1_545 ? Cl4 Rb2 Cl10 127.82(4) . 1_545 ? O3 Rb2 Cl2 125.44(10) . 4_644 ? O1 Rb2 Cl2 57.66(9) 4_644 4_644 ? O8 Rb2 Cl2 68.50(12) . 4_644 ? Cl4 Rb2 Cl2 113.47(4) . 4_644 ? Cl10 Rb2 Cl2 110.18(4) 1_545 4_644 ? O3 Rb2 Cl6 170.85(10) . 4_644 ? O1 Rb2 Cl6 112.37(10) 4_644 4_644 ? O8 Rb2 Cl6 112.68(13) . 4_644 ? Cl4 Rb2 Cl6 62.77(4) . 4_644 ? Cl10 Rb2 Cl6 118.15(4) 1_545 4_644 ? Cl2 Rb2 Cl6 62.92(4) 4_644 4_644 ? O3 Rb2 Cl12 100.50(10) . 1_545 ? O1 Rb2 Cl12 114.60(9) 4_644 1_545 ? O8 Rb2 Cl12 171.08(12) . 1_545 ? Cl4 Rb2 Cl12 72.64(4) . 1_545 ? Cl10 Rb2 Cl12 61.54(3) 1_545 1_545 ? Cl2 Rb2 Cl12 119.65(4) 4_644 1_545 ? Cl6 Rb2 Cl12 70.73(4) 4_644 1_545 ? O3 Rb2 Cl1 60.43(10) . . ? O1 Rb2 Cl1 126.83(10) 4_644 . ? O8 Rb2 Cl1 115.85(12) . . ? Cl4 Rb2 Cl1 62.36(4) . . ? Cl10 Rb2 Cl1 71.58(4) 1_545 . ? Cl2 Rb2 Cl1 174.04(4) 4_644 . ? Cl6 Rb2 Cl1 111.15(4) 4_644 . ? Cl12 Rb2 Cl1 55.75(3) 1_545 . ? O3 Rb2 Cl9 117.33(9) . 1_545 ? O1 Rb2 Cl9 67.72(9) 4_644 1_545 ? O8 Rb2 Cl9 130.54(12) . 1_545 ? Cl4 Rb2 Cl9 113.75(4) . 1_545 ? Cl10 Rb2 Cl9 61.50(4) 1_545 1_545 ? Cl2 Rb2 Cl9 66.02(3) 4_644 1_545 ? Cl6 Rb2 Cl9 60.82(3) 4_644 1_545 ? Cl12 Rb2 Cl9 58.38(3) 1_545 1_545 ? Cl1 Rb2 Cl9 111.10(3) . 1_545 ? O3 Rb2 Cl5 59.90(9) . . ? O1 Rb2 Cl5 117.97(10) 4_644 . ? O8 Rb2 Cl5 59.07(12) . . ? Cl4 Rb2 Cl5 62.17(4) . . ? Cl10 Rb2 Cl5 112.96(4) 1_545 . ? Cl2 Rb2 Cl5 123.70(4) 4_644 . ? Cl6 Rb2 Cl5 120.19(3) 4_644 . ? Cl12 Rb2 Cl5 112.02(3) 1_545 . ? Cl1 Rb2 Cl5 59.04(3) . . ? Cl9 Rb2 Cl5 170.11(4) 1_545 . ? O3 Rb2 Cl11 127.14(9) . 4_644 ? O1 Rb2 Cl11 111.09(9) 4_644 4_644 ? O8 Rb2 Cl11 58.13(13) . 4_644 ? Cl4 Rb2 Cl11 59.19(4) . 4_644 ? Cl10 Rb2 Cl11 171.34(4) 1_545 4_644 ? Cl2 Rb2 Cl11 61.17(3) 4_644 4_644 ? Cl6 Rb2 Cl11 58.67(3) 4_644 4_644 ? Cl12 Rb2 Cl11 121.17(4) 1_545 4_644 ? Cl1 Rb2 Cl11 116.96(3) . 4_644 ? Cl9 Rb2 Cl11 112.03(4) 1_545 4_644 ? Cl5 Rb2 Cl11 74.30(4) . 4_644 ? B5 B1 B3 107.8(4) . . ? B5 B1 B4 59.6(4) . . ? B3 B1 B4 60.6(3) . . ? B5 B1 Cl1 122.7(4) . . ? B3 B1 Cl1 121.8(4) . . ? B4 B1 Cl1 122.7(4) . . ? B5 B1 B2 108.0(4) . . ? B3 B1 B2 59.2(4) . . ? B4 B1 B2 108.0(4) . . ? Cl1 B1 B2 120.7(4) . . ? B5 B1 B6 60.8(3) . . ? B3 B1 B6 107.1(4) . . ? B4 B1 B6 108.3(4) . . ? Cl1 B1 B6 121.2(4) . . ? B2 B1 B6 59.4(3) . . ? B1 Cl1 Rb1 105.6(2) . 3 ? B1 Cl1 Rb2 103.1(2) . . ? Rb1 Cl1 Rb2 121.42(4) 3 . ? B3 B2 B11 107.8(5) . . ? B3 B2 B6 108.7(4) . . ? B11 B2 B6 60.6(3) . . ? B3 B2 B7 59.6(4) . . ? B11 B2 B7 59.7(4) . . ? B6 B2 B7 108.4(4) . . ? B3 B2 Cl2 120.5(4) . . ? B11 B2 Cl2 122.7(4) . . ? B6 B2 Cl2 122.1(4) . . ? B7 B2 Cl2 121.6(4) . . ? B3 B2 B1 60.2(4) . . ? B11 B2 B1 108.5(4) . . ? B6 B2 B1 60.5(3) . . ? B7 B2 B1 107.9(4) . . ? Cl2 B2 B1 121.1(4) . . ? B2 Cl2 Rb2 110.2(2) . 4_655 ? B2 Cl2 Rb1 102.6(2) . 3 ? Rb2 Cl2 Rb1 133.64(4) 4_655 3 ? B7 B3 B2 60.7(4) . . ? B7 B3 B1 109.1(4) . . ? B2 B3 B1 60.6(4) . . ? B7 B3 B8 60.4(4) . . ? B2 B3 B8 108.6(4) . . ? B1 B3 B8 107.6(4) . . ? B7 B3 Cl3 122.0(4) . . ? B2 B3 Cl3 123.0(4) . . ? B1 B3 Cl3 121.7(4) . . ? B8 B3 Cl3 120.6(4) . . ? B7 B3 B4 108.3(4) . . ? B2 B3 B4 108.4(4) . . ? B1 B3 B4 59.8(4) . . ? B8 B3 B4 59.3(3) . . ? Cl3 B3 B4 120.1(4) . . ? B3 Cl3 Rb1 112.9(2) . 3 ? B5 B4 B8 108.0(5) . . ? B5 B4 B9 60.4(4) . . ? B8 B4 B9 59.6(3) . . ? B5 B4 Cl4 123.3(4) . . ? B8 B4 Cl4 120.9(4) . . ? B9 B4 Cl4 123.0(4) . . ? B5 B4 B1 59.8(3) . . ? B8 B4 B1 107.9(5) . . ? B9 B4 B1 108.0(5) . . ? Cl4 B4 B1 121.6(4) . . ? B5 B4 B3 107.2(5) . . ? B8 B4 B3 59.9(3) . . ? B9 B4 B3 107.2(4) . . ? Cl4 B4 B3 120.7(4) . . ? B1 B4 B3 59.6(3) . . ? B4 Cl4 Rb2 111.1(2) . . ? B4 B5 B1 60.7(4) . . ? B4 B5 B9 60.1(4) . . ? B1 B5 B9 108.4(4) . . ? B4 B5 B10 108.3(5) . . ? B1 B5 B10 108.0(5) . . ? B9 B5 B10 60.0(4) . . ? B4 B5 Cl5 121.6(4) . . ? B1 B5 Cl5 121.9(4) . . ? B9 B5 Cl5 121.5(4) . . ? B10 B5 Cl5 121.3(4) . . ? B4 B5 B6 108.7(4) . . ? B1 B5 B6 60.3(3) . . ? B9 B5 B6 107.8(4) . . ? B10 B5 B6 59.5(3) . . ? Cl5 B5 B6 121.6(4) . . ? B5 Cl5 Rb2 103.1(2) . . ? B2 B6 Cl6 122.4(4) . . ? B2 B6 B10 107.8(4) . . ? Cl6 B6 B10 121.5(4) . . ? B2 B6 B11 59.6(3) . . ? Cl6 B6 B11 121.9(4) . . ? B10 B6 B11 60.5(3) . . ? B2 B6 B1 60.1(3) . . ? Cl6 B6 B1 122.5(4) . . ? B10 B6 B1 107.0(4) . . ? B11 B6 B1 107.5(4) . . ? B2 B6 B5 107.0(4) . . ? Cl6 B6 B5 122.2(4) . . ? B10 B6 B5 59.6(3) . . ? B11 B6 B5 107.5(4) . . ? B1 B6 B5 58.9(3) . . ? B6 Cl6 Rb2 106.1(2) . 4_655 ? B3 B7 B11 107.8(4) . . ? B3 B7 B2 59.6(3) . . ? B11 B7 B2 59.8(3) . . ? B3 B7 B8 60.3(3) . . ? B11 B7 B8 108.0(4) . . ? B2 B7 B8 107.7(4) . . ? B3 B7 B12 107.8(4) . . ? B11 B7 B12 60.4(4) . . ? B2 B7 B12 107.7(4) . . ? B8 B7 B12 59.4(3) . . ? B3 B7 Cl7 121.7(4) . . ? B11 B7 Cl7 121.3(4) . . ? B2 B7 Cl7 121.4(4) . . ? B8 B7 Cl7 122.4(4) . . ? B12 B7 Cl7 122.4(4) . . ? B7 Cl7 Rb1 102.3(2) . 3_565 ? B9 B8 B4 60.3(4) . . ? B9 B8 B12 59.8(3) . . ? B4 B8 B12 108.3(4) . . ? B9 B8 B3 108.5(4) . . ? B4 B8 B3 60.8(4) . . ? B12 B8 B3 107.7(4) . . ? B9 B8 B7 108.4(4) . . ? B4 B8 B7 108.5(4) . . ? B12 B8 B7 60.5(3) . . ? B3 B8 B7 59.2(4) . . ? B9 B8 Cl8 123.4(4) . . ? B4 B8 Cl8 121.9(4) . . ? B12 B8 Cl8 122.1(4) . . ? B3 B8 Cl8 120.3(4) . . ? B7 B8 Cl8 119.9(4) . . ? B12 B9 B8 60.4(3) . . ? B12 B9 B4 108.6(4) . . ? B8 B9 B4 60.1(3) . . ? B12 B9 B5 108.4(5) . . ? B8 B9 B5 107.6(4) . . ? B4 B9 B5 59.5(4) . . ? B12 B9 B10 60.3(4) . . ? B8 B9 B10 108.2(5) . . ? B4 B9 B10 107.8(4) . . ? B5 B9 B10 60.0(4) . . ? B12 B9 Cl9 121.5(4) . . ? B8 B9 Cl9 122.5(4) . . ? B4 B9 Cl9 121.8(4) . . ? B5 B9 Cl9 121.2(4) . . ? B10 B9 Cl9 121.1(4) . . ? B9 Cl9 Rb2 104.6(2) . 1_565 ? B12 B10 B6 108.5(4) . . ? B12 B10 Cl10 120.9(4) . . ? B6 B10 Cl10 121.1(4) . . ? B12 B10 B5 107.6(4) . . ? B6 B10 B5 60.8(3) . . ? Cl10 B10 B5 123.1(4) . . ? B12 B10 B9 59.3(4) . . ? B6 B10 B9 108.8(4) . . ? Cl10 B10 B9 122.6(4) . . ? B5 B10 B9 60.0(3) . . ? B12 B10 B11 60.1(4) . . ? B6 B10 B11 60.0(3) . . ? Cl10 B10 B11 120.5(4) . . ? B5 B10 B11 108.1(4) . . ? B9 B10 B11 107.5(4) . . ? B10 Cl10 Rb2 111.7(2) . 1_565 ? B7 B11 B2 60.5(4) . . ? B7 B11 Cl11 122.9(4) . . ? B2 B11 Cl11 122.0(4) . . ? B7 B11 B6 108.5(4) . . ? B2 B11 B6 59.9(3) . . ? Cl11 B11 B6 120.3(4) . . ? B7 B11 B12 60.4(4) . . ? B2 B11 B12 108.3(5) . . ? Cl11 B11 B12 122.4(4) . . ? B6 B11 B12 107.6(4) . . ? B7 B11 B10 107.9(5) . . ? B2 B11 B10 107.3(4) . . ? Cl11 B11 B10 121.1(4) . . ? B6 B11 B10 59.6(3) . . ? B12 B11 B10 59.5(4) . . ? B11 Cl11 Rb1 107.8(2) . 3_565 ? B11 Cl11 Rb2 102.8(2) . 4_655 ? Rb1 Cl11 Rb2 131.53(5) 3_565 4_655 ? B9 B12 B8 59.8(4) . . ? B9 B12 B10 60.4(4) . . ? B8 B12 B10 107.8(4) . . ? B9 B12 B11 108.7(4) . . ? B8 B12 B11 107.5(4) . . ? B10 B12 B11 60.4(4) . . ? B9 B12 B7 108.1(4) . . ? B8 B12 B7 60.1(3) . . ? B10 B12 B7 107.6(4) . . ? B11 B12 B7 59.2(4) . . ? B9 B12 Cl12 121.2(4) . . ? B8 B12 Cl12 121.3(4) . . ? B10 B12 Cl12 122.2(4) . . ? B11 B12 Cl12 122.2(4) . . ? B7 B12 Cl12 121.7(4) . . ? B12 Cl12 Rb1 103.9(2) . 3_565 ? B12 Cl12 Rb2 104.9(2) . 1_565 ? Rb1 Cl12 Rb2 125.39(4) 3_565 1_565 ? S1 O1 Rb2 146.9(3) . 4_655 ? O2 S1 O1 118.2(3) . . ? S1 O2 Rb1 162.0(3) . 3 ? S2 O3 Rb2 142.5(3) . . ? O3 S2 O4 117.9(3) . . ? S2 O4 Rb1 130.7(3) . . ? S3 O5 Rb1 154.4(3) . 1_565 ? O6 S3 O5 119.9(4) . . ? S4 O7 Rb1 151.5(3) . . ? O8 S4 O7 116.2(4) . . ? S4 O8 Rb2 132.1(5) . . ? 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 B5 B1 Cl1 Rb1 170.7(4) . . . 3 ? B3 B1 Cl1 Rb1 25.1(5) . . . 3 ? B4 B1 Cl1 Rb1 98.3(4) . . . 3 ? B2 B1 Cl1 Rb1 -45.5(4) . . . 3 ? B6 B1 Cl1 Rb1 -116.1(4) . . . 3 ? B5 B1 Cl1 Rb2 42.3(5) . . . . ? B3 B1 Cl1 Rb2 -103.2(4) . . . . ? B4 B1 Cl1 Rb2 -30.0(5) . . . . ? B2 B1 Cl1 Rb2 -173.8(4) . . . . ? B6 B1 Cl1 Rb2 115.6(4) . . . . ? O3 Rb2 Cl1 B1 -111.0(2) . . . . ? O1 Rb2 Cl1 B1 -144.0(2) 4_644 . . . ? O8 Rb2 Cl1 B1 -57.4(2) . . . . ? Cl4 Rb2 Cl1 B1 32.1(2) . . . . ? Cl10 Rb2 Cl1 B1 -173.2(2) 1_545 . . . ? Cl6 Rb2 Cl1 B1 72.9(2) 4_644 . . . ? Cl12 Rb2 Cl1 B1 119.2(2) 1_545 . . . ? Cl9 Rb2 Cl1 B1 138.7(2) 1_545 . . . ? Cl5 Rb2 Cl1 B1 -40.4(2) . . . . ? Cl11 Rb2 Cl1 B1 8.3(2) 4_644 . . . ? O3 Rb2 Cl1 Rb1 131.27(11) . . . 3 ? O1 Rb2 Cl1 Rb1 98.33(12) 4_644 . . 3 ? O8 Rb2 Cl1 Rb1 -175.06(13) . . . 3 ? Cl4 Rb2 Cl1 Rb1 -85.61(5) . . . 3 ? Cl10 Rb2 Cl1 Rb1 69.09(5) 1_545 . . 3 ? Cl6 Rb2 Cl1 Rb1 -44.76(5) 4_644 . . 3 ? Cl12 Rb2 Cl1 Rb1 1.48(4) 1_545 . . 3 ? Cl9 Rb2 Cl1 Rb1 20.97(6) 1_545 . . 3 ? Cl5 Rb2 Cl1 Rb1 -158.13(6) . . . 3 ? Cl11 Rb2 Cl1 Rb1 -109.38(5) 4_644 . . 3 ? B5 B1 B2 B3 -100.4(5) . . . . ? B4 B1 B2 B3 -37.5(4) . . . . ? Cl1 B1 B2 B3 111.0(5) . . . . ? B6 B1 B2 B3 -138.5(5) . . . . ? B5 B1 B2 B11 -0.1(6) . . . . ? B3 B1 B2 B11 100.3(5) . . . . ? B4 B1 B2 B11 62.8(5) . . . . ? Cl1 B1 B2 B11 -148.6(4) . . . . ? B6 B1 B2 B11 -38.2(4) . . . . ? B5 B1 B2 B6 38.1(4) . . . . ? B3 B1 B2 B6 138.5(5) . . . . ? B4 B1 B2 B6 101.0(5) . . . . ? Cl1 B1 B2 B6 -110.4(5) . . . . ? B5 B1 B2 B7 -63.4(5) . . . . ? B3 B1 B2 B7 37.1(4) . . . . ? B4 B1 B2 B7 -0.4(5) . . . . ? Cl1 B1 B2 B7 148.1(4) . . . . ? B6 B1 B2 B7 -101.4(5) . . . . ? B5 B1 B2 Cl2 149.9(4) . . . . ? B3 B1 B2 Cl2 -109.7(5) . . . . ? B4 B1 B2 Cl2 -147.2(4) . . . . ? Cl1 B1 B2 Cl2 1.4(7) . . . . ? B6 B1 B2 Cl2 111.8(5) . . . . ? B3 B2 Cl2 Rb2 -177.4(4) . . . 4_655 ? B11 B2 Cl2 Rb2 39.7(5) . . . 4_655 ? B6 B2 Cl2 Rb2 -33.6(5) . . . 4_655 ? B7 B2 Cl2 Rb2 111.7(4) . . . 4_655 ? B1 B2 Cl2 Rb2 -106.0(4) . . . 4_655 ? B3 B2 Cl2 Rb1 -30.7(5) . . . 3 ? B11 B2 Cl2 Rb1 -173.6(4) . . . 3 ? B6 B2 Cl2 Rb1 113.1(4) . . . 3 ? B7 B2 Cl2 Rb1 -101.6(4) . . . 3 ? B1 B2 Cl2 Rb1 40.7(4) . . . 3 ? B11 B2 B3 B7 36.7(4) . . . . ? B6 B2 B3 B7 100.8(5) . . . . ? Cl2 B2 B3 B7 -111.1(5) . . . . ? B1 B2 B3 B7 138.3(4) . . . . ? B11 B2 B3 B1 -101.6(5) . . . . ? B6 B2 B3 B1 -37.5(4) . . . . ? B7 B2 B3 B1 -138.3(4) . . . . ? Cl2 B2 B3 B1 110.7(5) . . . . ? B11 B2 B3 B8 -1.5(6) . . . . ? B6 B2 B3 B8 62.7(5) . . . . ? B7 B2 B3 B8 -38.2(4) . . . . ? Cl2 B2 B3 B8 -149.2(4) . . . . ? B1 B2 B3 B8 100.1(5) . . . . ? B11 B2 B3 Cl3 147.8(4) . . . . ? B6 B2 B3 Cl3 -148.1(4) . . . . ? B7 B2 B3 Cl3 111.1(5) . . . . ? Cl2 B2 B3 Cl3 0.0(7) . . . . ? B1 B2 B3 Cl3 -110.6(5) . . . . ? B11 B2 B3 B4 -64.3(5) . . . . ? B6 B2 B3 B4 -0.2(6) . . . . ? B7 B2 B3 B4 -101.1(5) . . . . ? Cl2 B2 B3 B4 147.9(4) . . . . ? B1 B2 B3 B4 37.2(4) . . . . ? B5 B1 B3 B7 62.8(6) . . . . ? B4 B1 B3 B7 100.5(5) . . . . ? Cl1 B1 B3 B7 -147.2(4) . . . . ? B2 B1 B3 B7 -37.9(4) . . . . ? B6 B1 B3 B7 -1.3(6) . . . . ? B5 B1 B3 B2 100.7(5) . . . . ? B4 B1 B3 B2 138.4(4) . . . . ? Cl1 B1 B3 B2 -109.3(5) . . . . ? B6 B1 B3 B2 36.6(4) . . . . ? B5 B1 B3 B8 -1.2(6) . . . . ? B4 B1 B3 B8 36.5(4) . . . . ? Cl1 B1 B3 B8 148.8(4) . . . . ? B2 B1 B3 B8 -101.9(5) . . . . ? B6 B1 B3 B8 -65.3(5) . . . . ? B5 B1 B3 Cl3 -146.5(4) . . . . ? B4 B1 B3 Cl3 -108.8(5) . . . . ? Cl1 B1 B3 Cl3 3.5(7) . . . . ? B2 B1 B3 Cl3 112.8(5) . . . . ? B6 B1 B3 Cl3 149.4(4) . . . . ? B5 B1 B3 B4 -37.7(4) . . . . ? Cl1 B1 B3 B4 112.3(5) . . . . ? B2 B1 B3 B4 -138.4(4) . . . . ? B6 B1 B3 B4 -101.8(5) . . . . ? B7 B3 Cl3 Rb1 112.1(4) . . . 3 ? B2 B3 Cl3 Rb1 38.5(5) . . . 3 ? B1 B3 Cl3 Rb1 -34.9(5) . . . 3 ? B8 B3 Cl3 Rb1 -175.8(4) . . . 3 ? B4 B3 Cl3 Rb1 -105.9(4) . . . 3 ? B3 B1 B4 B5 -137.6(5) . . . . ? Cl1 B1 B4 B5 111.5(5) . . . . ? B2 B1 B4 B5 -100.7(5) . . . . ? B6 B1 B4 B5 -37.8(4) . . . . ? B5 B1 B4 B8 100.8(5) . . . . ? B3 B1 B4 B8 -36.8(4) . . . . ? Cl1 B1 B4 B8 -147.7(4) . . . . ? B2 B1 B4 B8 0.1(6) . . . . ? B6 B1 B4 B8 62.9(5) . . . . ? B5 B1 B4 B9 37.8(4) . . . . ? B3 B1 B4 B9 -99.8(5) . . . . ? Cl1 B1 B4 B9 149.3(4) . . . . ? B2 B1 B4 B9 -62.9(5) . . . . ? B6 B1 B4 B9 0.0(6) . . . . ? B5 B1 B4 Cl4 -112.9(5) . . . . ? B3 B1 B4 Cl4 109.6(5) . . . . ? Cl1 B1 B4 Cl4 -1.3(7) . . . . ? B2 B1 B4 Cl4 146.4(4) . . . . ? B6 B1 B4 Cl4 -150.7(4) . . . . ? B5 B1 B4 B3 137.6(5) . . . . ? Cl1 B1 B4 B3 -110.9(5) . . . . ? B2 B1 B4 B3 36.9(4) . . . . ? B6 B1 B4 B3 99.7(5) . . . . ? B7 B3 B4 B5 -64.4(5) . . . . ? B2 B3 B4 B5 0.0(6) . . . . ? B1 B3 B4 B5 37.6(4) . . . . ? B8 B3 B4 B5 -101.2(5) . . . . ? Cl3 B3 B4 B5 149.0(4) . . . . ? B7 B3 B4 B8 36.8(4) . . . . ? B2 B3 B4 B8 101.2(5) . . . . ? B1 B3 B4 B8 138.8(5) . . . . ? Cl3 B3 B4 B8 -109.9(5) . . . . ? B7 B3 B4 B9 -0.8(6) . . . . ? B2 B3 B4 B9 63.6(5) . . . . ? B1 B3 B4 B9 101.2(5) . . . . ? B8 B3 B4 B9 -37.6(4) . . . . ? Cl3 B3 B4 B9 -147.5(4) . . . . ? B7 B3 B4 Cl4 147.1(4) . . . . ? B2 B3 B4 Cl4 -148.5(4) . . . . ? B1 B3 B4 Cl4 -110.9(5) . . . . ? B8 B3 B4 Cl4 110.3(5) . . . . ? Cl3 B3 B4 Cl4 0.4(7) . . . . ? B7 B3 B4 B1 -101.9(5) . . . . ? B2 B3 B4 B1 -37.6(4) . . . . ? B8 B3 B4 B1 -138.8(5) . . . . ? Cl3 B3 B4 B1 111.4(5) . . . . ? B5 B4 Cl4 Rb2 -35.1(5) . . . . ? B8 B4 Cl4 Rb2 179.4(4) . . . . ? B9 B4 Cl4 Rb2 -109.0(4) . . . . ? B1 B4 Cl4 Rb2 37.3(5) . . . . ? B3 B4 Cl4 Rb2 108.3(4) . . . . ? O8 Rb2 Cl4 B4 78.9(3) . . . . ? Cl10 Rb2 Cl4 B4 -65.4(2) 1_545 . . . ? Cl2 Rb2 Cl4 B4 150.2(2) 4_644 . . . ? Cl6 Rb2 Cl4 B4 -171.2(2) 4_644 . . . ? Cl12 Rb2 Cl4 B4 -94.4(2) 1_545 . . . ? Cl1 Rb2 Cl4 B4 -34.5(2) . . . . ? Cl9 Rb2 Cl4 B4 -136.8(2) 1_545 . . . ? Cl5 Rb2 Cl4 B4 33.2(2) . . . . ? Cl11 Rb2 Cl4 B4 120.8(2) 4_644 . . . ? B8 B4 B5 B1 -100.6(5) . . . . ? B9 B4 B5 B1 -137.9(5) . . . . ? Cl4 B4 B5 B1 110.0(5) . . . . ? B3 B4 B5 B1 -37.5(4) . . . . ? B8 B4 B5 B9 37.3(4) . . . . ? Cl4 B4 B5 B9 -112.1(5) . . . . ? B1 B4 B5 B9 137.9(5) . . . . ? B3 B4 B5 B9 100.4(5) . . . . ? B8 B4 B5 B10 0.2(6) . . . . ? B9 B4 B5 B10 -37.1(4) . . . . ? Cl4 B4 B5 B10 -149.1(4) . . . . ? B1 B4 B5 B10 100.9(5) . . . . ? B3 B4 B5 B10 63.4(5) . . . . ? B8 B4 B5 Cl5 147.9(4) . . . . ? B9 B4 B5 Cl5 110.7(5) . . . . ? Cl4 B4 B5 Cl5 -1.4(7) . . . . ? B1 B4 B5 Cl5 -111.4(5) . . . . ? B3 B4 B5 Cl5 -148.9(4) . . . . ? B8 B4 B5 B6 -62.9(5) . . . . ? B9 B4 B5 B6 -100.2(5) . . . . ? Cl4 B4 B5 B6 147.7(4) . . . . ? B1 B4 B5 B6 37.7(4) . . . . ? B3 B4 B5 B6 0.2(6) . . . . ? B3 B1 B5 B4 38.1(4) . . . . ? Cl1 B1 B5 B4 -111.5(5) . . . . ? B2 B1 B5 B4 100.7(5) . . . . ? B6 B1 B5 B4 138.2(4) . . . . ? B3 B1 B5 B9 0.4(6) . . . . ? B4 B1 B5 B9 -37.7(4) . . . . ? Cl1 B1 B5 B9 -149.3(4) . . . . ? B2 B1 B5 B9 63.0(5) . . . . ? B6 B1 B5 B9 100.4(5) . . . . ? B3 B1 B5 B10 -63.2(5) . . . . ? B4 B1 B5 B10 -101.3(5) . . . . ? Cl1 B1 B5 B10 147.2(4) . . . . ? B2 B1 B5 B10 -0.6(6) . . . . ? B6 B1 B5 B10 36.9(4) . . . . ? B3 B1 B5 Cl5 149.1(4) . . . . ? B4 B1 B5 Cl5 111.0(5) . . . . ? Cl1 B1 B5 Cl5 -0.5(7) . . . . ? B2 B1 B5 Cl5 -148.3(4) . . . . ? B6 B1 B5 Cl5 -110.8(5) . . . . ? B3 B1 B5 B6 -100.0(5) . . . . ? B4 B1 B5 B6 -138.2(4) . . . . ? Cl1 B1 B5 B6 110.3(5) . . . . ? B2 B1 B5 B6 -37.5(4) . . . . ? B4 B5 Cl5 Rb2 31.5(5) . . . . ? B1 B5 Cl5 Rb2 -41.4(5) . . . . ? B9 B5 Cl5 Rb2 103.4(4) . . . . ? B10 B5 Cl5 Rb2 175.1(4) . . . . ? B6 B5 Cl5 Rb2 -113.7(4) . . . . ? O3 Rb2 Cl5 B5 111.9(3) . . . . ? O1 Rb2 Cl5 B5 158.6(2) 4_644 . . . ? O8 Rb2 Cl5 B5 -157.4(3) . . . . ? Cl4 Rb2 Cl5 B5 -32.4(2) . . . . ? Cl10 Rb2 Cl5 B5 89.5(2) 1_545 . . . ? Cl2 Rb2 Cl5 B5 -133.3(2) 4_644 . . . ? Cl6 Rb2 Cl5 B5 -57.5(2) 4_644 . . . ? Cl12 Rb2 Cl5 B5 22.3(2) 1_545 . . . ? Cl1 Rb2 Cl5 B5 40.4(2) . . . . ? Cl11 Rb2 Cl5 B5 -95.5(2) 4_644 . . . ? B3 B2 B6 Cl6 149.0(4) . . . . ? B11 B2 B6 Cl6 -110.7(5) . . . . ? B7 B2 B6 Cl6 -147.8(4) . . . . ? Cl2 B2 B6 Cl6 1.5(7) . . . . ? B1 B2 B6 Cl6 111.6(5) . . . . ? B3 B2 B6 B10 -62.4(5) . . . . ? B11 B2 B6 B10 37.9(4) . . . . ? B7 B2 B6 B10 0.8(6) . . . . ? Cl2 B2 B6 B10 150.1(4) . . . . ? B1 B2 B6 B10 -99.8(5) . . . . ? B3 B2 B6 B11 -100.3(5) . . . . ? B7 B2 B6 B11 -37.1(4) . . . . ? Cl2 B2 B6 B11 112.2(5) . . . . ? B1 B2 B6 B11 -137.7(5) . . . . ? B3 B2 B6 B1 37.3(4) . . . . ? B11 B2 B6 B1 137.7(5) . . . . ? B7 B2 B6 B1 100.6(5) . . . . ? Cl2 B2 B6 B1 -110.2(5) . . . . ? B3 B2 B6 B5 0.4(6) . . . . ? B11 B2 B6 B5 100.7(5) . . . . ? B7 B2 B6 B5 63.6(5) . . . . ? Cl2 B2 B6 B5 -147.1(4) . . . . ? B1 B2 B6 B5 -37.0(4) . . . . ? B5 B1 B6 B2 -137.8(4) . . . . ? B3 B1 B6 B2 -36.5(4) . . . . ? B4 B1 B6 B2 -100.5(5) . . . . ? Cl1 B1 B6 B2 109.6(5) . . . . ? B5 B1 B6 Cl6 110.7(5) . . . . ? B3 B1 B6 Cl6 -148.0(4) . . . . ? B4 B1 B6 Cl6 148.0(4) . . . . ? Cl1 B1 B6 Cl6 -1.9(7) . . . . ? B2 B1 B6 Cl6 -111.5(5) . . . . ? B5 B1 B6 B10 -36.7(4) . . . . ? B3 B1 B6 B10 64.6(5) . . . . ? B4 B1 B6 B10 0.6(6) . . . . ? Cl1 B1 B6 B10 -149.3(4) . . . . ? B2 B1 B6 B10 101.1(5) . . . . ? B5 B1 B6 B11 -100.3(5) . . . . ? B3 B1 B6 B11 1.0(6) . . . . ? B4 B1 B6 B11 -63.0(5) . . . . ? Cl1 B1 B6 B11 147.1(4) . . . . ? B2 B1 B6 B11 37.5(4) . . . . ? B3 B1 B6 B5 101.2(5) . . . . ? B4 B1 B6 B5 37.3(4) . . . . ? Cl1 B1 B6 B5 -112.6(5) . . . . ? B2 B1 B6 B5 137.8(4) . . . . ? B4 B5 B6 B2 -0.3(6) . . . . ? B1 B5 B6 B2 37.5(4) . . . . ? B9 B5 B6 B2 -63.9(5) . . . . ? B10 B5 B6 B2 -101.0(5) . . . . ? Cl5 B5 B6 B2 148.8(4) . . . . ? B4 B5 B6 Cl6 -149.1(4) . . . . ? B1 B5 B6 Cl6 -111.2(5) . . . . ? B9 B5 B6 Cl6 147.4(4) . . . . ? B10 B5 B6 Cl6 110.3(5) . . . . ? Cl5 B5 B6 Cl6 0.1(7) . . . . ? B4 B5 B6 B10 100.7(5) . . . . ? B1 B5 B6 B10 138.6(5) . . . . ? B9 B5 B6 B10 37.1(4) . . . . ? Cl5 B5 B6 B10 -110.2(5) . . . . ? B4 B5 B6 B11 62.3(5) . . . . ? B1 B5 B6 B11 100.2(5) . . . . ? B9 B5 B6 B11 -1.3(6) . . . . ? B10 B5 B6 B11 -38.3(4) . . . . ? Cl5 B5 B6 B11 -148.5(4) . . . . ? B4 B5 B6 B1 -37.9(4) . . . . ? B9 B5 B6 B1 -101.5(5) . . . . ? B10 B5 B6 B1 -138.6(5) . . . . ? Cl5 B5 B6 B1 111.2(5) . . . . ? B2 B6 Cl6 Rb2 28.8(5) . . . 4_655 ? B10 B6 Cl6 Rb2 -115.6(4) . . . 4_655 ? B11 B6 Cl6 Rb2 -43.1(5) . . . 4_655 ? B1 B6 Cl6 Rb2 101.6(4) . . . 4_655 ? B5 B6 Cl6 Rb2 172.7(4) . . . 4_655 ? B2 B3 B7 B11 -36.7(4) . . . . ? B1 B3 B7 B11 1.1(6) . . . . ? B8 B3 B7 B11 100.9(5) . . . . ? Cl3 B3 B7 B11 -149.5(4) . . . . ? B4 B3 B7 B11 64.6(5) . . . . ? B1 B3 B7 B2 37.8(4) . . . . ? B8 B3 B7 B2 137.7(5) . . . . ? Cl3 B3 B7 B2 -112.8(5) . . . . ? B4 B3 B7 B2 101.3(5) . . . . ? B2 B3 B7 B8 -137.7(5) . . . . ? B1 B3 B7 B8 -99.8(5) . . . . ? Cl3 B3 B7 B8 109.6(5) . . . . ? B4 B3 B7 B8 -36.3(4) . . . . ? B2 B3 B7 B12 -100.5(5) . . . . ? B1 B3 B7 B12 -62.7(5) . . . . ? B8 B3 B7 B12 37.1(4) . . . . ? Cl3 B3 B7 B12 146.7(4) . . . . ? B4 B3 B7 B12 0.8(6) . . . . ? B2 B3 B7 Cl7 110.4(5) . . . . ? B1 B3 B7 Cl7 148.2(4) . . . . ? B8 B3 B7 Cl7 -112.0(5) . . . . ? Cl3 B3 B7 Cl7 -2.4(7) . . . . ? B4 B3 B7 Cl7 -148.3(4) . . . . ? B11 B2 B7 B3 -138.8(5) . . . . ? B6 B2 B7 B3 -101.3(5) . . . . ? Cl2 B2 B7 B3 109.2(5) . . . . ? B1 B2 B7 B3 -37.3(4) . . . . ? B3 B2 B7 B11 138.8(5) . . . . ? B6 B2 B7 B11 37.4(4) . . . . ? Cl2 B2 B7 B11 -112.0(5) . . . . ? B1 B2 B7 B11 101.4(5) . . . . ? B3 B2 B7 B8 37.9(4) . . . . ? B11 B2 B7 B8 -100.9(5) . . . . ? B6 B2 B7 B8 -63.4(5) . . . . ? Cl2 B2 B7 B8 147.1(4) . . . . ? B1 B2 B7 B8 0.6(5) . . . . ? B3 B2 B7 B12 100.6(5) . . . . ? B11 B2 B7 B12 -38.2(4) . . . . ? B6 B2 B7 B12 -0.7(6) . . . . ? Cl2 B2 B7 B12 -150.2(4) . . . . ? B1 B2 B7 B12 63.3(5) . . . . ? B3 B2 B7 Cl7 -110.8(5) . . . . ? B11 B2 B7 Cl7 110.4(5) . . . . ? B6 B2 B7 Cl7 147.9(4) . . . . ? Cl2 B2 B7 Cl7 -1.6(7) . . . . ? B1 B2 B7 Cl7 -148.1(4) . . . . ? B3 B7 Cl7 Rb1 -176.9(4) . . . 3_565 ? B11 B7 Cl7 Rb1 -34.1(5) . . . 3_565 ? B2 B7 Cl7 Rb1 -105.5(4) . . . 3_565 ? B8 B7 Cl7 Rb1 110.4(4) . . . 3_565 ? B12 B7 Cl7 Rb1 38.5(5) . . . 3_565 ? B5 B4 B8 B9 -37.6(4) . . . . ? Cl4 B4 B8 B9 112.6(5) . . . . ? B1 B4 B8 B9 -100.8(5) . . . . ? B3 B4 B8 B9 -137.5(5) . . . . ? B5 B4 B8 B12 -0.7(6) . . . . ? B9 B4 B8 B12 37.0(4) . . . . ? Cl4 B4 B8 B12 149.5(4) . . . . ? B1 B4 B8 B12 -63.8(5) . . . . ? B3 B4 B8 B12 -100.5(5) . . . . ? B5 B4 B8 B3 99.8(5) . . . . ? B9 B4 B8 B3 137.5(5) . . . . ? Cl4 B4 B8 B3 -110.0(5) . . . . ? B1 B4 B8 B3 36.7(4) . . . . ? B5 B4 B8 B7 63.4(5) . . . . ? B9 B4 B8 B7 101.1(5) . . . . ? Cl4 B4 B8 B7 -146.3(4) . . . . ? B1 B4 B8 B7 0.3(6) . . . . ? B3 B4 B8 B7 -36.4(4) . . . . ? B5 B4 B8 Cl8 -150.7(4) . . . . ? B9 B4 B8 Cl8 -113.1(5) . . . . ? Cl4 B4 B8 Cl8 -0.5(7) . . . . ? B1 B4 B8 Cl8 146.1(4) . . . . ? B3 B4 B8 Cl8 109.5(5) . . . . ? B7 B3 B8 B9 -100.9(5) . . . . ? B2 B3 B8 B9 -62.5(6) . . . . ? B1 B3 B8 B9 1.5(6) . . . . ? Cl3 B3 B8 B9 147.3(4) . . . . ? B4 B3 B8 B9 38.3(4) . . . . ? B7 B3 B8 B4 -139.1(5) . . . . ? B2 B3 B8 B4 -100.8(5) . . . . ? B1 B3 B8 B4 -36.7(4) . . . . ? Cl3 B3 B8 B4 109.0(5) . . . . ? B7 B3 B8 B12 -37.6(4) . . . . ? B2 B3 B8 B12 0.7(6) . . . . ? B1 B3 B8 B12 64.8(5) . . . . ? Cl3 B3 B8 B12 -149.5(4) . . . . ? B4 B3 B8 B12 101.5(5) . . . . ? B2 B3 B8 B7 38.3(4) . . . . ? B1 B3 B8 B7 102.4(5) . . . . ? Cl3 B3 B8 B7 -111.9(5) . . . . ? B4 B3 B8 B7 139.1(5) . . . . ? B7 B3 B8 Cl8 108.9(5) . . . . ? B2 B3 B8 Cl8 147.2(4) . . . . ? B1 B3 B8 Cl8 -148.7(4) . . . . ? Cl3 B3 B8 Cl8 -3.0(7) . . . . ? B4 B3 B8 Cl8 -112.0(5) . . . . ? B3 B7 B8 B9 101.0(5) . . . . ? B11 B7 B8 B9 0.3(6) . . . . ? B2 B7 B8 B9 63.4(5) . . . . ? B12 B7 B8 B9 -37.1(4) . . . . ? Cl7 B7 B8 B9 -148.3(4) . . . . ? B3 B7 B8 B4 37.1(4) . . . . ? B11 B7 B8 B4 -63.6(5) . . . . ? B2 B7 B8 B4 -0.5(6) . . . . ? B12 B7 B8 B4 -101.0(5) . . . . ? Cl7 B7 B8 B4 147.8(4) . . . . ? B3 B7 B8 B12 138.1(5) . . . . ? B11 B7 B8 B12 37.4(4) . . . . ? B2 B7 B8 B12 100.5(5) . . . . ? Cl7 B7 B8 B12 -111.2(5) . . . . ? B11 B7 B8 B3 -100.7(5) . . . . ? B2 B7 B8 B3 -37.6(4) . . . . ? B12 B7 B8 B3 -138.1(5) . . . . ? Cl7 B7 B8 B3 110.7(5) . . . . ? B3 B7 B8 Cl8 -109.6(5) . . . . ? B11 B7 B8 Cl8 149.7(4) . . . . ? B2 B7 B8 Cl8 -147.2(4) . . . . ? B12 B7 B8 Cl8 112.3(5) . . . . ? Cl7 B7 B8 Cl8 1.1(7) . . . . ? B4 B8 B9 B12 138.7(5) . . . . ? B3 B8 B9 B12 100.2(5) . . . . ? B7 B8 B9 B12 37.4(4) . . . . ? Cl8 B8 B9 B12 -110.7(5) . . . . ? B12 B8 B9 B4 -138.7(5) . . . . ? B3 B8 B9 B4 -38.5(4) . . . . ? B7 B8 B9 B4 -101.3(5) . . . . ? Cl8 B8 B9 B4 110.7(5) . . . . ? B4 B8 B9 B5 37.2(4) . . . . ? B12 B8 B9 B5 -101.5(5) . . . . ? B3 B8 B9 B5 -1.3(6) . . . . ? B7 B8 B9 B5 -64.1(5) . . . . ? Cl8 B8 B9 B5 147.8(4) . . . . ? B4 B8 B9 B10 100.6(5) . . . . ? B12 B8 B9 B10 -38.1(4) . . . . ? B3 B8 B9 B10 62.1(5) . . . . ? B7 B8 B9 B10 -0.7(6) . . . . ? Cl8 B8 B9 B10 -148.8(4) . . . . ? B4 B8 B9 Cl9 -110.8(5) . . . . ? B12 B8 B9 Cl9 110.5(5) . . . . ? B3 B8 B9 Cl9 -149.3(4) . . . . ? B7 B8 B9 Cl9 147.9(4) . . . . ? Cl8 B8 B9 Cl9 -0.1(7) . . . . ? B5 B4 B9 B12 100.8(5) . . . . ? B8 B4 B9 B12 -37.3(4) . . . . ? Cl4 B4 B9 B12 -146.6(4) . . . . ? B1 B4 B9 B12 63.3(5) . . . . ? B3 B4 B9 B12 0.5(6) . . . . ? B5 B4 B9 B8 138.1(5) . . . . ? Cl4 B4 B9 B8 -109.3(5) . . . . ? B1 B4 B9 B8 100.6(5) . . . . ? B3 B4 B9 B8 37.8(4) . . . . ? B8 B4 B9 B5 -138.1(5) . . . . ? Cl4 B4 B9 B5 112.7(5) . . . . ? B1 B4 B9 B5 -37.5(4) . . . . ? B3 B4 B9 B5 -100.3(5) . . . . ? B5 B4 B9 B10 36.9(4) . . . . ? B8 B4 B9 B10 -101.1(5) . . . . ? Cl4 B4 B9 B10 149.6(4) . . . . ? B1 B4 B9 B10 -0.6(6) . . . . ? B3 B4 B9 B10 -63.4(5) . . . . ? B5 B4 B9 Cl9 -110.0(5) . . . . ? B8 B4 B9 Cl9 111.9(5) . . . . ? Cl4 B4 B9 Cl9 2.6(7) . . . . ? B1 B4 B9 Cl9 -147.5(4) . . . . ? B3 B4 B9 Cl9 149.6(4) . . . . ? B4 B5 B9 B12 -101.3(5) . . . . ? B1 B5 B9 B12 -63.3(6) . . . . ? B10 B5 B9 B12 37.4(4) . . . . ? Cl5 B5 B9 B12 147.9(4) . . . . ? B6 B5 B9 B12 0.5(6) . . . . ? B4 B5 B9 B8 -37.4(4) . . . . ? B1 B5 B9 B8 0.6(6) . . . . ? B10 B5 B9 B8 101.2(5) . . . . ? Cl5 B5 B9 B8 -148.3(4) . . . . ? B6 B5 B9 B8 64.3(5) . . . . ? B1 B5 B9 B4 38.0(4) . . . . ? B10 B5 B9 B4 138.6(5) . . . . ? Cl5 B5 B9 B4 -110.9(5) . . . . ? B6 B5 B9 B4 101.8(5) . . . . ? B4 B5 B9 B10 -138.6(5) . . . . ? B1 B5 B9 B10 -100.6(5) . . . . ? Cl5 B5 B9 B10 110.5(5) . . . . ? B6 B5 B9 B10 -36.9(4) . . . . ? B4 B5 B9 Cl9 111.0(5) . . . . ? B1 B5 B9 Cl9 149.0(4) . . . . ? B10 B5 B9 Cl9 -110.3(5) . . . . ? Cl5 B5 B9 Cl9 0.1(7) . . . . ? B6 B5 B9 Cl9 -147.2(4) . . . . ? B12 B9 Cl9 Rb2 -40.0(5) . . . 1_565 ? B8 B9 Cl9 Rb2 -112.8(4) . . . 1_565 ? B4 B9 Cl9 Rb2 174.7(4) . . . 1_565 ? B5 B9 Cl9 Rb2 103.5(4) . . . 1_565 ? B10 B9 Cl9 Rb2 32.0(5) . . . 1_565 ? B2 B6 B10 B12 -0.6(6) . . . . ? Cl6 B6 B10 B12 148.3(4) . . . . ? B11 B6 B10 B12 36.9(4) . . . . ? B1 B6 B10 B12 -63.9(5) . . . . ? B5 B6 B10 B12 -100.2(5) . . . . ? B2 B6 B10 Cl10 -147.1(4) . . . . ? Cl6 B6 B10 Cl10 1.8(7) . . . . ? B11 B6 B10 Cl10 -109.6(5) . . . . ? B1 B6 B10 Cl10 149.5(4) . . . . ? B5 B6 B10 Cl10 113.2(5) . . . . ? B2 B6 B10 B5 99.7(5) . . . . ? Cl6 B6 B10 B5 -111.4(5) . . . . ? B11 B6 B10 B5 137.2(5) . . . . ? B1 B6 B10 B5 36.4(4) . . . . ? B2 B6 B10 B9 62.4(5) . . . . ? Cl6 B6 B10 B9 -148.7(4) . . . . ? B11 B6 B10 B9 99.8(5) . . . . ? B1 B6 B10 B9 -1.0(6) . . . . ? B5 B6 B10 B9 -37.3(4) . . . . ? B2 B6 B10 B11 -37.5(4) . . . . ? Cl6 B6 B10 B11 111.4(5) . . . . ? B1 B6 B10 B11 -100.8(5) . . . . ? B5 B6 B10 B11 -137.2(5) . . . . ? B4 B5 B10 B12 0.3(6) . . . . ? B1 B5 B10 B12 64.6(5) . . . . ? B9 B5 B10 B12 -36.7(4) . . . . ? Cl5 B5 B10 B12 -147.5(5) . . . . ? B6 B5 B10 B12 101.8(5) . . . . ? B4 B5 B10 B6 -101.4(5) . . . . ? B1 B5 B10 B6 -37.2(4) . . . . ? B9 B5 B10 B6 -138.5(5) . . . . ? Cl5 B5 B10 B6 110.7(5) . . . . ? B4 B5 B10 Cl10 148.5(5) . . . . ? B1 B5 B10 Cl10 -147.3(4) . . . . ? B9 B5 B10 Cl10 111.4(5) . . . . ? Cl5 B5 B10 Cl10 0.7(7) . . . . ? B6 B5 B10 Cl10 -110.1(5) . . . . ? B4 B5 B10 B9 37.1(4) . . . . ? B1 B5 B10 B9 101.3(5) . . . . ? Cl5 B5 B10 B9 -110.8(5) . . . . ? B6 B5 B10 B9 138.5(5) . . . . ? B4 B5 B10 B11 -63.1(5) . . . . ? B1 B5 B10 B11 1.1(6) . . . . ? B9 B5 B10 B11 -100.2(5) . . . . ? Cl5 B5 B10 B11 149.0(5) . . . . ? B6 B5 B10 B11 38.3(4) . . . . ? B8 B9 B10 B12 38.2(4) . . . . ? B4 B9 B10 B12 101.7(5) . . . . ? B5 B9 B10 B12 138.4(5) . . . . ? Cl9 B9 B10 B12 -111.0(5) . . . . ? B12 B9 B10 B6 -100.7(5) . . . . ? B8 B9 B10 B6 -62.6(5) . . . . ? B4 B9 B10 B6 1.0(6) . . . . ? B5 B9 B10 B6 37.7(4) . . . . ? Cl9 B9 B10 B6 148.2(4) . . . . ? B12 B9 B10 Cl10 109.2(5) . . . . ? B8 B9 B10 Cl10 147.4(4) . . . . ? B4 B9 B10 Cl10 -149.1(4) . . . . ? B5 B9 B10 Cl10 -112.3(5) . . . . ? Cl9 B9 B10 Cl10 -1.8(7) . . . . ? B12 B9 B10 B5 -138.4(5) . . . . ? B8 B9 B10 B5 -100.3(5) . . . . ? B4 B9 B10 B5 -36.7(4) . . . . ? Cl9 B9 B10 B5 110.5(5) . . . . ? B12 B9 B10 B11 -37.3(4) . . . . ? B8 B9 B10 B11 0.9(6) . . . . ? B4 B9 B10 B11 64.4(5) . . . . ? B5 B9 B10 B11 101.2(5) . . . . ? Cl9 B9 B10 B11 -148.3(4) . . . . ? B12 B10 Cl10 Rb2 36.8(5) . . . 1_565 ? B6 B10 Cl10 Rb2 179.2(4) . . . 1_565 ? B5 B10 Cl10 Rb2 -107.4(4) . . . 1_565 ? B9 B10 Cl10 Rb2 -34.3(5) . . . 1_565 ? B11 B10 Cl10 Rb2 108.0(4) . . . 1_565 ? B3 B7 B11 B2 36.7(4) . . . . ? B8 B7 B11 B2 100.4(5) . . . . ? B12 B7 B11 B2 137.4(5) . . . . ? Cl7 B7 B11 B2 -110.6(5) . . . . ? B3 B7 B11 Cl11 147.7(4) . . . . ? B2 B7 B11 Cl11 111.1(5) . . . . ? B8 B7 B11 Cl11 -148.5(4) . . . . ? B12 B7 B11 Cl11 -111.6(5) . . . . ? Cl7 B7 B11 Cl11 0.5(7) . . . . ? B3 B7 B11 B6 -0.5(6) . . . . ? B2 B7 B11 B6 -37.2(4) . . . . ? B8 B7 B11 B6 63.3(5) . . . . ? B12 B7 B11 B6 100.2(5) . . . . ? Cl7 B7 B11 B6 -147.7(4) . . . . ? B3 B7 B11 B12 -100.7(5) . . . . ? B2 B7 B11 B12 -137.4(5) . . . . ? B8 B7 B11 B12 -37.0(4) . . . . ? Cl7 B7 B11 B12 112.0(5) . . . . ? B3 B7 B11 B10 -63.5(5) . . . . ? B2 B7 B11 B10 -100.2(5) . . . . ? B8 B7 B11 B10 0.2(6) . . . . ? B12 B7 B11 B10 37.2(4) . . . . ? Cl7 B7 B11 B10 149.2(4) . . . . ? B3 B2 B11 B7 -36.7(4) . . . . ? B6 B2 B11 B7 -138.5(4) . . . . ? Cl2 B2 B11 B7 110.2(5) . . . . ? B1 B2 B11 B7 -100.3(5) . . . . ? B3 B2 B11 Cl11 -149.1(4) . . . . ? B6 B2 B11 Cl11 109.0(5) . . . . ? B7 B2 B11 Cl11 -112.5(5) . . . . ? Cl2 B2 B11 Cl11 -2.2(7) . . . . ? B1 B2 B11 Cl11 147.2(4) . . . . ? B3 B2 B11 B6 101.8(5) . . . . ? B7 B2 B11 B6 138.5(4) . . . . ? Cl2 B2 B11 B6 -111.3(5) . . . . ? B1 B2 B11 B6 38.2(4) . . . . ? B3 B2 B11 B12 1.6(6) . . . . ? B6 B2 B11 B12 -100.2(5) . . . . ? B7 B2 B11 B12 38.3(4) . . . . ? Cl2 B2 B11 B12 148.5(4) . . . . ? B1 B2 B11 B12 -62.0(5) . . . . ? B3 B2 B11 B10 64.5(6) . . . . ? B6 B2 B11 B10 -37.4(4) . . . . ? B7 B2 B11 B10 101.1(5) . . . . ? Cl2 B2 B11 B10 -148.6(4) . . . . ? B1 B2 B11 B10 0.8(6) . . . . ? B2 B6 B11 B7 37.4(4) . . . . ? Cl6 B6 B11 B7 148.9(4) . . . . ? B10 B6 B11 B7 -100.3(5) . . . . ? B1 B6 B11 B7 -0.3(6) . . . . ? B5 B6 B11 B7 -62.4(5) . . . . ? Cl6 B6 B11 B2 111.5(5) . . . . ? B10 B6 B11 B2 -137.8(5) . . . . ? B1 B6 B11 B2 -37.8(4) . . . . ? B5 B6 B11 B2 -99.8(5) . . . . ? B2 B6 B11 Cl11 -111.7(5) . . . . ? Cl6 B6 B11 Cl11 -0.3(7) . . . . ? B10 B6 B11 Cl11 110.5(5) . . . . ? B1 B6 B11 Cl11 -149.5(4) . . . . ? B5 B6 B11 Cl11 148.5(4) . . . . ? B2 B6 B11 B12 101.3(5) . . . . ? Cl6 B6 B11 B12 -147.2(4) . . . . ? B10 B6 B11 B12 -36.4(4) . . . . ? B1 B6 B11 B12 63.6(5) . . . . ? B5 B6 B11 B12 1.5(6) . . . . ? B2 B6 B11 B10 137.8(5) . . . . ? Cl6 B6 B11 B10 -110.8(5) . . . . ? B1 B6 B11 B10 100.0(5) . . . . ? B5 B6 B11 B10 38.0(4) . . . . ? B12 B10 B11 B7 -37.6(4) . . . . ? B6 B10 B11 B7 101.3(5) . . . . ? Cl10 B10 B11 B7 -148.0(4) . . . . ? B5 B10 B11 B7 62.7(5) . . . . ? B9 B10 B11 B7 -0.7(6) . . . . ? B12 B10 B11 B2 -101.4(5) . . . . ? B6 B10 B11 B2 37.5(4) . . . . ? Cl10 B10 B11 B2 148.2(4) . . . . ? B5 B10 B11 B2 -1.1(6) . . . . ? B9 B10 B11 B2 -64.5(5) . . . . ? B12 B10 B11 Cl11 111.8(5) . . . . ? B6 B10 B11 Cl11 -109.3(5) . . . . ? Cl10 B10 B11 Cl11 1.4(7) . . . . ? B5 B10 B11 Cl11 -147.9(4) . . . . ? B9 B10 B11 Cl11 148.7(4) . . . . ? B12 B10 B11 B6 -138.9(5) . . . . ? Cl10 B10 B11 B6 110.6(5) . . . . ? B5 B10 B11 B6 -38.7(4) . . . . ? B9 B10 B11 B6 -102.0(5) . . . . ? B6 B10 B11 B12 138.9(5) . . . . ? Cl10 B10 B11 B12 -110.4(5) . . . . ? B5 B10 B11 B12 100.3(5) . . . . ? B9 B10 B11 B12 36.9(4) . . . . ? B7 B11 Cl11 Rb1 37.7(5) . . . 3_565 ? B2 B11 Cl11 Rb1 111.0(4) . . . 3_565 ? B6 B11 Cl11 Rb1 -177.7(4) . . . 3_565 ? B12 B11 Cl11 Rb1 -35.7(5) . . . 3_565 ? B10 B11 Cl11 Rb1 -107.1(4) . . . 3_565 ? B7 B11 Cl11 Rb2 -104.3(4) . . . 4_655 ? B2 B11 Cl11 Rb2 -31.0(5) . . . 4_655 ? B6 B11 Cl11 Rb2 40.3(5) . . . 4_655 ? B12 B11 Cl11 Rb2 -177.7(4) . . . 4_655 ? B10 B11 Cl11 Rb2 110.9(4) . . . 4_655 ? B4 B9 B12 B8 37.2(4) . . . . ? B5 B9 B12 B8 100.3(5) . . . . ? B10 B9 B12 B8 137.5(5) . . . . ? Cl9 B9 B12 B8 -112.1(5) . . . . ? B8 B9 B12 B10 -137.5(5) . . . . ? B4 B9 B12 B10 -100.4(5) . . . . ? B5 B9 B12 B10 -37.2(4) . . . . ? Cl9 B9 B12 B10 110.3(5) . . . . ? B8 B9 B12 B11 -99.8(5) . . . . ? B4 B9 B12 B11 -62.7(5) . . . . ? B5 B9 B12 B11 0.4(6) . . . . ? B10 B9 B12 B11 37.7(4) . . . . ? Cl9 B9 B12 B11 148.0(4) . . . . ? B8 B9 B12 B7 -37.1(4) . . . . ? B4 B9 B12 B7 0.0(6) . . . . ? B5 B9 B12 B7 63.1(5) . . . . ? B10 B9 B12 B7 100.4(5) . . . . ? Cl9 B9 B12 B7 -149.3(4) . . . . ? B8 B9 B12 Cl12 110.5(5) . . . . ? B4 B9 B12 Cl12 147.7(4) . . . . ? B5 B9 B12 Cl12 -149.2(4) . . . . ? B10 B9 B12 Cl12 -111.9(5) . . . . ? Cl9 B9 B12 Cl12 -1.6(7) . . . . ? B4 B8 B12 B9 -37.2(4) . . . . ? B3 B8 B12 B9 -101.5(5) . . . . ? B7 B8 B12 B9 -138.6(5) . . . . ? Cl8 B8 B12 B9 112.8(5) . . . . ? B9 B8 B12 B10 38.1(4) . . . . ? B4 B8 B12 B10 0.9(6) . . . . ? B3 B8 B12 B10 -63.4(5) . . . . ? B7 B8 B12 B10 -100.5(5) . . . . ? Cl8 B8 B12 B10 150.9(4) . . . . ? B9 B8 B12 B11 101.8(5) . . . . ? B4 B8 B12 B11 64.6(5) . . . . ? B3 B8 B12 B11 0.3(6) . . . . ? B7 B8 B12 B11 -36.7(4) . . . . ? Cl8 B8 B12 B11 -145.4(4) . . . . ? B9 B8 B12 B7 138.6(5) . . . . ? B4 B8 B12 B7 101.4(5) . . . . ? B3 B8 B12 B7 37.1(4) . . . . ? Cl8 B8 B12 B7 -108.7(5) . . . . ? B9 B8 B12 Cl12 -110.4(5) . . . . ? B4 B8 B12 Cl12 -147.5(4) . . . . ? B3 B8 B12 Cl12 148.1(4) . . . . ? B7 B8 B12 Cl12 111.1(5) . . . . ? Cl8 B8 B12 Cl12 2.4(7) . . . . ? B6 B10 B12 B9 101.4(5) . . . . ? Cl10 B10 B12 B9 -112.0(5) . . . . ? B5 B10 B12 B9 37.1(4) . . . . ? B11 B10 B12 B9 138.2(4) . . . . ? B6 B10 B12 B8 63.6(6) . . . . ? Cl10 B10 B12 B8 -149.8(4) . . . . ? B5 B10 B12 B8 -0.8(6) . . . . ? B9 B10 B12 B8 -37.8(4) . . . . ? B11 B10 B12 B8 100.4(5) . . . . ? B6 B10 B12 B11 -36.9(4) . . . . ? Cl10 B10 B12 B11 109.8(5) . . . . ? B5 B10 B12 B11 -101.2(5) . . . . ? B9 B10 B12 B11 -138.2(4) . . . . ? B6 B10 B12 B7 0.1(6) . . . . ? Cl10 B10 B12 B7 146.8(4) . . . . ? B5 B10 B12 B7 -64.2(5) . . . . ? B9 B10 B12 B7 -101.3(5) . . . . ? B11 B10 B12 B7 37.0(4) . . . . ? B6 B10 B12 Cl12 -148.3(4) . . . . ? Cl10 B10 B12 Cl12 -1.7(7) . . . . ? B5 B10 B12 Cl12 147.3(4) . . . . ? B9 B10 B12 Cl12 110.3(5) . . . . ? B11 B10 B12 Cl12 -111.5(5) . . . . ? B7 B11 B12 B9 100.4(5) . . . . ? B2 B11 B12 B9 62.1(5) . . . . ? Cl11 B11 B12 B9 -147.3(4) . . . . ? B6 B11 B12 B9 -1.2(6) . . . . ? B10 B11 B12 B9 -37.7(4) . . . . ? B7 B11 B12 B8 37.2(4) . . . . ? B2 B11 B12 B8 -1.2(6) . . . . ? Cl11 B11 B12 B8 149.4(4) . . . . ? B6 B11 B12 B8 -64.5(5) . . . . ? B10 B11 B12 B8 -101.0(5) . . . . ? B7 B11 B12 B10 138.1(5) . . . . ? B2 B11 B12 B10 99.8(5) . . . . ? Cl11 B11 B12 B10 -109.6(5) . . . . ? B6 B11 B12 B10 36.5(4) . . . . ? B2 B11 B12 B7 -38.4(4) . . . . ? Cl11 B11 B12 B7 112.3(5) . . . . ? B6 B11 B12 B7 -101.6(5) . . . . ? B10 B11 B12 B7 -138.1(5) . . . . ? B7 B11 B12 Cl12 -110.3(5) . . . . ? B2 B11 B12 Cl12 -148.7(4) . . . . ? Cl11 B11 B12 Cl12 1.9(7) . . . . ? B6 B11 B12 Cl12 148.0(4) . . . . ? B10 B11 B12 Cl12 111.5(5) . . . . ? B3 B7 B12 B9 -0.5(6) . . . . ? B11 B7 B12 B9 -101.3(5) . . . . ? B2 B7 B12 B9 -63.5(5) . . . . ? B8 B7 B12 B9 37.0(4) . . . . ? Cl7 B7 B12 B9 148.3(4) . . . . ? B3 B7 B12 B8 -37.5(4) . . . . ? B11 B7 B12 B8 -138.4(4) . . . . ? B2 B7 B12 B8 -100.5(5) . . . . ? Cl7 B7 B12 B8 111.3(5) . . . . ? B3 B7 B12 B10 63.3(5) . . . . ? B11 B7 B12 B10 -37.5(4) . . . . ? B2 B7 B12 B10 0.4(6) . . . . ? B8 B7 B12 B10 100.9(5) . . . . ? Cl7 B7 B12 B10 -147.9(4) . . . . ? B3 B7 B12 B11 100.8(5) . . . . ? B2 B7 B12 B11 37.9(4) . . . . ? B8 B7 B12 B11 138.4(4) . . . . ? Cl7 B7 B12 B11 -110.3(5) . . . . ? B3 B7 B12 Cl12 -148.0(4) . . . . ? B11 B7 B12 Cl12 111.2(5) . . . . ? B2 B7 B12 Cl12 149.0(4) . . . . ? B8 B7 B12 Cl12 -110.5(5) . . . . ? Cl7 B7 B12 Cl12 0.8(7) . . . . ? B9 B12 Cl12 Rb1 175.7(4) . . . 3_565 ? B8 B12 Cl12 Rb1 -112.9(4) . . . 3_565 ? B10 B12 Cl12 Rb1 103.2(5) . . . 3_565 ? B11 B12 Cl12 Rb1 30.2(5) . . . 3_565 ? B7 B12 Cl12 Rb1 -40.9(5) . . . 3_565 ? B9 B12 Cl12 Rb2 42.7(5) . . . 1_565 ? B8 B12 Cl12 Rb2 114.0(4) . . . 1_565 ? B10 B12 Cl12 Rb2 -29.9(5) . . . 1_565 ? B11 B12 Cl12 Rb2 -102.8(4) . . . 1_565 ? B7 B12 Cl12 Rb2 -174.0(4) . . . 1_565 ? Rb2 O1 S1 O2 75.8(6) 4_655 . . . ? O1 S1 O2 Rb1 19.1(10) . . . 3 ? O1 Rb2 O3 S2 -160.3(5) 4_644 . . . ? O8 Rb2 O3 S2 -84.8(5) . . . . ? Cl4 Rb2 O3 S2 11.5(5) . . . . ? Cl10 Rb2 O3 S2 132.9(5) 1_545 . . . ? Cl2 Rb2 O3 S2 -134.5(4) 4_644 . . . ? Cl12 Rb2 O3 S2 87.0(5) 1_545 . . . ? Cl1 Rb2 O3 S2 46.7(4) . . . . ? Cl9 Rb2 O3 S2 146.7(4) 1_545 . . . ? Cl5 Rb2 O3 S2 -22.5(4) . . . . ? Cl11 Rb2 O3 S2 -56.2(5) 4_644 . . . ? Rb2 O3 S2 O4 120.2(4) . . . . ? O3 S2 O4 Rb1 29.5(4) . . . . ? O2 Rb1 O4 S2 99.7(3) 3_455 . . . ? O7 Rb1 O4 S2 -62.2(3) . . . . ? O5 Rb1 O4 S2 31.4(3) 1_545 . . . ? Cl3 Rb1 O4 S2 -22.0(4) 3_455 . . . ? Cl11 Rb1 O4 S2 -175.3(3) 3_465 . . . ? Cl12 Rb1 O4 S2 -106.3(3) 3_465 . . . ? Cl7 Rb1 O4 S2 -132.4(4) 3_465 . . . ? Cl2 Rb1 O4 S2 49.1(4) 3_455 . . . ? Rb1 O5 S3 O6 -63.9(9) 1_565 . . . ? O2 Rb1 O7 S4 -145.0(6) 3_455 . . . ? O4 Rb1 O7 S4 -105.2(7) . . . . ? O5 Rb1 O7 S4 -174.3(7) 1_545 . . . ? Cl3 Rb1 O7 S4 117.8(7) 3_455 . . . ? Cl11 Rb1 O7 S4 -7.7(7) 3_465 . . . ? Cl12 Rb1 O7 S4 29.4(6) 3_465 . . . ? Cl7 Rb1 O7 S4 -41.4(6) 3_465 . . . ? Cl1 Rb1 O7 S4 70.8(7) 3_455 . . . ? Cl2 Rb1 O7 S4 131.2(6) 3_455 . . . ? Rb1 O7 S4 O8 146.8(6) . . . . ? O7 S4 O8 Rb2 18.6(6) . . . . ? O3 Rb2 O8 S4 -39.4(5) . . . . ? O1 Rb2 O8 S4 37.2(5) 4_644 . . . ? Cl4 Rb2 O8 S4 -150.3(5) . . . . ? Cl10 Rb2 O8 S4 -2.7(5) 1_545 . . . ? Cl2 Rb2 O8 S4 98.7(5) 4_644 . . . ? Cl6 Rb2 O8 S4 144.7(4) 4_644 . . . ? Cl1 Rb2 O8 S4 -85.8(5) . . . . ? Cl9 Rb2 O8 S4 74.4(5) 1_545 . . . ? Cl5 Rb2 O8 S4 -102.7(5) . . . . ? Cl11 Rb2 O8 S4 167.2(5) 4_644 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.413 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.091 #===END data_ck008new _database_code_depnum_ccdc_archive 'CCDC 710773' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(B12 Cl12), (O2 S1), 2(Cs)' _chemical_formula_sum 'B12 Cl12 Cs2 O2 S1' _chemical_formula_weight 885.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 10.1432(14) _cell_length_b 10.1432(14) _cell_length_c 20.668(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1841.5(5) _cell_formula_units_Z 3 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 27.45 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1218 _exptl_absorpt_coefficient_mu 4.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4187 _exptl_absorpt_correction_T_max 0.4187 _exptl_absorpt_process_details ; March 2001 T Higashi ; _exptl_special_details ; ???? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS Spider' _diffrn_measurement_method fsFind.ref _diffrn_detector_area_resol_mean 10.0000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3466 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 936 _reflns_number_gt 833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+25.9639P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 936 _refine_ls_number_parameters 52 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.253 _refine_ls_restrained_S_all 1.253 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cs1 Cs 0.6667 0.3333 0.05680(3) 0.02067(16) Uani 1 3 d S . . Cl1 Cl 0.87901(14) 0.33645(14) 0.20014(6) 0.0209(3) Uani 1 1 d . . . B1 B 0.7684(6) 0.3325(6) 0.2680(3) 0.0142(10) Uani 1 1 d . . . Cl2 Cl 1.01024(12) 0.66476(12) 0.30236(6) 0.0190(3) Uani 1 1 d . . . B2 B 0.8323(6) 0.4956(6) 0.3181(3) 0.0131(10) Uani 1 1 d . . . O1 O 0.6667 0.3333 0.8933(4) 0.054(2) Uani 1 3 d S . . S1 S 0.606(11) 0.334(18) 0.834(4) 0.040(10) Uani 0.17 1 d 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 Cs1 0.01848(19) 0.01848(19) 0.0251(3) 0.000 0.000 0.00924(10) Cl1 0.0200(6) 0.0229(6) 0.0213(7) -0.0014(5) 0.0050(5) 0.0119(5) B1 0.011(2) 0.014(2) 0.016(3) -0.002(2) 0.001(2) 0.006(2) Cl2 0.0117(5) 0.0117(5) 0.0294(7) 0.0021(5) 0.0018(5) 0.0026(4) B2 0.009(2) 0.011(2) 0.021(3) 0.004(2) 0.003(2) 0.0055(19) O1 0.057(4) 0.057(4) 0.047(6) 0.000 0.000 0.0287(18) S1 0.04(4) 0.04(2) 0.047(6) 0.020(6) 0.013(16) 0.03(3) _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 Cs1 O1 3.379(9) 1_554 ? Cs1 Cl2 3.4945(12) 15_545 ? Cs1 Cl2 3.4945(12) 14_455 ? Cs1 Cl2 3.4946(12) 13_665 ? Cs1 Cl1 3.6537(15) . ? Cs1 Cl1 3.6537(15) 3_665 ? Cs1 Cl1 3.6537(15) 2_655 ? Cs1 Cl2 3.7373(13) 7_444 ? Cs1 Cl2 3.7374(13) 9_664 ? Cs1 Cl2 3.7374(13) 8_644 ? Cl1 B1 1.784(5) . ? B1 B2 1.777(7) . ? B1 B2 1.778(8) 17 ? B1 B1 1.794(9) 3_665 ? B1 B1 1.794(9) 2_655 ? B1 B2 1.795(7) 3_665 ? Cl2 B2 1.792(5) . ? Cl2 Cs1 3.4946(12) 13_665 ? Cl2 Cs1 3.7373(13) 4 ? B2 B2 1.778(6) 18_545 ? B2 B2 1.778(6) 17 ? B2 B1 1.778(8) 18_545 ? B2 B1 1.795(7) 2_655 ? O1 S1 1.37(9) 2_655 ? O1 S1 1.37(9) 3_665 ? O1 S1 1.37(9) . ? O1 S1 1.40(8) 17_556 ? O1 S1 1.40(8) 18_546 ? O1 S1 1.40(8) 16_656 ? O1 Cs1 3.379(9) 1_556 ? S1 O1 1.40(8) 16_656 ? 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 Cs1 Cl2 81.22(2) 1_554 15_545 ? O1 Cs1 Cl2 81.22(2) 1_554 14_455 ? Cl2 Cs1 Cl2 117.713(12) 15_545 14_455 ? O1 Cs1 Cl2 81.22(2) 1_554 13_665 ? Cl2 Cs1 Cl2 117.712(12) 15_545 13_665 ? Cl2 Cs1 Cl2 117.711(12) 14_455 13_665 ? O1 Cs1 Cl1 144.18(2) 1_554 . ? Cl2 Cs1 Cl1 62.97(3) 15_545 . ? Cl2 Cs1 Cl1 113.98(3) 14_455 . ? Cl2 Cs1 Cl1 114.81(3) 13_665 . ? O1 Cs1 Cl1 144.18(2) 1_554 3_665 ? Cl2 Cs1 Cl1 114.81(3) 15_545 3_665 ? Cl2 Cs1 Cl1 62.97(3) 14_455 3_665 ? Cl2 Cs1 Cl1 113.98(3) 13_665 3_665 ? Cl1 Cs1 Cl1 60.90(3) . 3_665 ? O1 Cs1 Cl1 144.18(2) 1_554 2_655 ? Cl2 Cs1 Cl1 113.98(3) 15_545 2_655 ? Cl2 Cs1 Cl1 114.81(3) 14_455 2_655 ? Cl2 Cs1 Cl1 62.97(3) 13_665 2_655 ? Cl1 Cs1 Cl1 60.90(3) . 2_655 ? Cl1 Cs1 Cl1 60.90(3) 3_665 2_655 ? O1 Cs1 Cl2 60.96(2) 1_554 7_444 ? Cl2 Cs1 Cl2 142.16(2) 15_545 7_444 ? Cl2 Cs1 Cl2 60.63(3) 14_455 7_444 ? Cl2 Cs1 Cl2 58.55(3) 13_665 7_444 ? Cl1 Cs1 Cl2 154.86(3) . 7_444 ? Cl1 Cs1 Cl2 98.12(3) 3_665 7_444 ? Cl1 Cs1 Cl2 97.72(3) 2_655 7_444 ? O1 Cs1 Cl2 60.96(2) 1_554 9_664 ? Cl2 Cs1 Cl2 58.55(3) 15_545 9_664 ? Cl2 Cs1 Cl2 142.16(2) 14_455 9_664 ? Cl2 Cs1 Cl2 60.64(3) 13_665 9_664 ? Cl1 Cs1 Cl2 97.72(3) . 9_664 ? Cl1 Cs1 Cl2 154.86(3) 3_665 9_664 ? Cl1 Cs1 Cl2 98.12(3) 2_655 9_664 ? Cl2 Cs1 Cl2 98.43(3) 7_444 9_664 ? O1 Cs1 Cl2 60.96(2) 1_554 8_644 ? Cl2 Cs1 Cl2 60.63(3) 15_545 8_644 ? Cl2 Cs1 Cl2 58.55(3) 14_455 8_644 ? Cl2 Cs1 Cl2 142.16(2) 13_665 8_644 ? Cl1 Cs1 Cl2 98.12(3) . 8_644 ? Cl1 Cs1 Cl2 97.72(3) 3_665 8_644 ? Cl1 Cs1 Cl2 154.86(3) 2_655 8_644 ? Cl2 Cs1 Cl2 98.43(3) 7_444 8_644 ? Cl2 Cs1 Cl2 98.43(3) 9_664 8_644 ? B1 Cl1 Cs1 106.01(18) . . ? B2 B1 B2 60.0(2) . 17 ? B2 B1 Cl1 120.3(3) . . ? B2 B1 Cl1 121.2(3) 17 . ? B2 B1 B1 108.1(3) . 3_665 ? B2 B1 B1 107.5(3) 17 3_665 ? Cl1 B1 B1 123.1(2) . 3_665 ? B2 B1 B1 60.4(3) . 2_655 ? B2 B1 B1 108.1(3) 17 2_655 ? Cl1 B1 B1 121.5(3) . 2_655 ? B1 B1 B1 60.000(1) 3_665 2_655 ? B2 B1 B2 107.5(4) . 3_665 ? B2 B1 B2 59.7(2) 17 3_665 ? Cl1 B1 B2 123.3(3) . 3_665 ? B1 B1 B2 59.4(3) 3_665 3_665 ? B1 B1 B2 107.3(3) 2_655 3_665 ? B2 Cl2 Cs1 116.99(16) . 13_665 ? B2 Cl2 Cs1 112.17(17) . 4 ? Cs1 Cl2 Cs1 121.45(3) 13_665 4 ? B1 B2 B2 108.3(3) . 18_545 ? B1 B2 B2 60.0(3) . 17 ? B2 B2 B2 108.2(4) 18_545 17 ? B1 B2 B1 108.8(4) . 18_545 ? B2 B2 B1 60.0(4) 18_545 18_545 ? B2 B2 B1 60.6(4) 17 18_545 ? B1 B2 Cl2 120.6(3) . . ? B2 B2 Cl2 123.0(3) 18_545 . ? B2 B2 Cl2 120.2(3) 17 . ? B1 B2 Cl2 121.2(4) 18_545 . ? B1 B2 B1 60.3(4) . 2_655 ? B2 B2 B1 59.7(3) 18_545 2_655 ? B2 B2 B1 108.1(3) 17 2_655 ? B1 B2 B1 108.0(4) 18_545 2_655 ? Cl2 B2 B1 122.7(3) . 2_655 ? S1 O1 Cs1 153.1(12) . 1_556 ? O1 S1 O1 126.7(15) . 16_656 ? 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 O1 Cs1 Cl1 B1 -179.31(18) 1_554 . . . ? Cl2 Cs1 Cl1 B1 179.84(19) 15_545 . . . ? Cl2 Cs1 Cl1 B1 -70.01(18) 14_455 . . . ? Cl2 Cs1 Cl1 B1 70.01(18) 13_665 . . . ? Cl1 Cs1 Cl1 B1 -34.77(18) 3_665 . . . ? Cl1 Cs1 Cl1 B1 36.14(18) 2_655 . . . ? Cl2 Cs1 Cl1 B1 1.6(2) 7_444 . . . ? Cl2 Cs1 Cl1 B1 131.16(18) 9_664 . . . ? Cl2 Cs1 Cl1 B1 -129.12(18) 8_644 . . . ? Cs1 Cl1 B1 B2 -109.8(4) . . . . ? Cs1 Cl1 B1 B2 179.1(3) . . . 17 ? Cs1 Cl1 B1 B1 34.5(5) . . . 3_665 ? Cs1 Cl1 B1 B1 -38.1(5) . . . 2_655 ? Cs1 Cl1 B1 B2 107.1(4) . . . 3_665 ? B2 B1 B2 B2 -101.0(5) 17 . . 18_545 ? Cl1 B1 B2 B2 148.2(4) . . . 18_545 ? B1 B1 B2 B2 -0.8(5) 3_665 . . 18_545 ? B1 B1 B2 B2 36.9(4) 2_655 . . 18_545 ? B2 B1 B2 B2 -63.5(5) 3_665 . . 18_545 ? Cl1 B1 B2 B2 -110.8(4) . . . 17 ? B1 B1 B2 B2 100.2(3) 3_665 . . 17 ? B1 B1 B2 B2 137.8(3) 2_655 . . 17 ? B2 B1 B2 B2 37.48(17) 3_665 . . 17 ? B2 B1 B2 B1 -37.4(4) 17 . . 18_545 ? Cl1 B1 B2 B1 -148.1(3) . . . 18_545 ? B1 B1 B2 B1 62.8(5) 3_665 . . 18_545 ? B1 B1 B2 B1 100.5(5) 2_655 . . 18_545 ? B2 B1 B2 B1 0.1(5) 3_665 . . 18_545 ? B2 B1 B2 Cl2 109.5(4) 17 . . . ? Cl1 B1 B2 Cl2 -1.3(6) . . . . ? B1 B1 B2 Cl2 -150.3(3) 3_665 . . . ? B1 B1 B2 Cl2 -112.6(4) 2_655 . . . ? B2 B1 B2 Cl2 147.0(4) 3_665 . . . ? B2 B1 B2 B1 -137.8(3) 17 . . 2_655 ? Cl1 B1 B2 B1 111.4(4) . . . 2_655 ? B1 B1 B2 B1 -37.7(2) 3_665 . . 2_655 ? B2 B1 B2 B1 -100.4(3) 3_665 . . 2_655 ? Cs1 Cl2 B2 B1 122.4(3) 13_665 . . . ? Cs1 Cl2 B2 B1 -90.5(4) 4 . . . ? Cs1 Cl2 B2 B2 -22.5(6) 13_665 . . 18_545 ? Cs1 Cl2 B2 B2 124.6(5) 4 . . 18_545 ? Cs1 Cl2 B2 B2 -166.7(4) 13_665 . . 17 ? Cs1 Cl2 B2 B2 -19.6(6) 4 . . 17 ? Cs1 Cl2 B2 B1 -94.8(4) 13_665 . . 18_545 ? Cs1 Cl2 B2 B1 52.3(4) 4 . . 18_545 ? Cs1 Cl2 B2 B1 50.1(4) 13_665 . . 2_655 ? Cs1 Cl2 B2 B1 -162.7(3) 4 . . 2_655 ? S1 O1 S1 S1 -94(6) 2_655 . . 17_556 ? S1 O1 S1 S1 -29(7) 3_665 . . 17_556 ? S1 O1 S1 S1 -123(14) 18_546 . . 17_556 ? S1 O1 S1 S1 -62(7) 16_656 . . 17_556 ? Cs1 O1 S1 S1 118(7) 1_556 . . 17_556 ? S1 O1 S1 S1 29(7) 2_655 . . 18_546 ? S1 O1 S1 S1 94(7) 3_665 . . 18_546 ? S1 O1 S1 S1 123(14) 17_556 . . 18_546 ? S1 O1 S1 S1 62(7) 16_656 . . 18_546 ? Cs1 O1 S1 S1 -118(7) 1_556 . . 18_546 ? S1 O1 S1 S1 65.9(7) 3_665 . . 2_655 ? S1 O1 S1 S1 94(6) 17_556 . . 2_655 ? S1 O1 S1 S1 -29(7) 18_546 . . 2_655 ? S1 O1 S1 S1 32.9(4) 16_656 . . 2_655 ? Cs1 O1 S1 S1 -147.1(4) 1_556 . . 2_655 ? S1 O1 S1 S1 -65.9(5) 2_655 . . 3_665 ? S1 O1 S1 S1 29(7) 17_556 . . 3_665 ? S1 O1 S1 S1 -94(7) 18_546 . . 3_665 ? S1 O1 S1 S1 -32.9(2) 16_656 . . 3_665 ? Cs1 O1 S1 S1 147.1(4) 1_556 . . 3_665 ? S1 O1 S1 S1 -32.93(14) 2_655 . . 16_656 ? S1 O1 S1 S1 32.9(4) 3_665 . . 16_656 ? S1 O1 S1 S1 62(7) 17_556 . . 16_656 ? S1 O1 S1 S1 -62(7) 18_546 . . 16_656 ? Cs1 O1 S1 S1 180.00(16) 1_556 . . 16_656 ? S1 O1 S1 O1 -32.9(3) 2_655 . . 16_656 ? S1 O1 S1 O1 32.9(3) 3_665 . . 16_656 ? S1 O1 S1 O1 62(7) 17_556 . . 16_656 ? S1 O1 S1 O1 -62(7) 18_546 . . 16_656 ? S1 O1 S1 O1 0.000(13) 16_656 . . 16_656 ? Cs1 O1 S1 O1 180.00(18) 1_556 . . 16_656 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.566 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.145 #===END data_ck-mk-07 _database_code_depnum_ccdc_archive 'CCDC 778603' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B12 Br12, 8(O2 S), 2(Na)' _chemical_formula_sum 'B12 Br12 Na2 O16 S8' _chemical_formula_weight 1647.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.811(2) _cell_length_b 20.979(4) _cell_length_c 9.980(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.46(3) _cell_angle_gamma 90.00 _cell_volume 1997.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 23.99 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 12.523 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.156 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'March 2001 T Higashi' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 ; Crystal Goniometer ; _diffrn_measurement_device_type ; Rigaku RAXIS conversion ; _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_details ; scan: Number of images: 45 Slice: 20.0000 - 200.0000 Image width: 4.0000 Exp time: 60.0000 Rotation axis: Omega Omega: 0.0000 Chi: 54.0000 Phi: 0.0000 XTD: 127.4000 2theta: 0.0000 scan: Number of images: 45 Slice: 20.0000 - 200.0000 Image width: 4.0000 Exp time: 60.0000 Rotation axis: Omega Omega: 0.0000 Chi: 0.0000 Phi: 180.0000 XTD: 127.4000 2theta: 0.0000 scan: Number of images: 45 Slice: 20.0000 - 200.0000 Image width: 4.0000 Exp time: 60.0000 Rotation axis: Omega Omega: 0.0000 Chi: 0.0000 Phi: 0.0000 XTD: 127.4000 2theta: 0.0000 scan: Number of images: 41 Slice: 20.0000 - 184.0000 Image width: 4.0000 Exp time: 60.0000 Rotation axis: Omega Omega: 0.0000 Chi: 54.0000 Phi: 180.0000 XTD: 127.4000 2theta: 0.0000 scan: Number of images: 40 Slice: 24.0000 - 184.0000 Image width: 4.0000 Exp time: 60.0000 Rotation axis: Omega Omega: 0.0000 Chi: 54.0000 Phi: 90.0000 XTD: 127.4000 2theta: 0.0000 scan: Number of images: 40 Slice: 22.0000 - 182.0000 Image width: 4.0000 Exp time: 60.0000 Rotation axis: Omega Omega: 0.0000 Chi: 54.0000 Phi: 270.0000 XTD: 127.4000 2theta: 0.0000 ; _diffrn_detector_area_resol_mean 10.0000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62210 _diffrn_reflns_av_R_equivalents 0.0925 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 23.99 _reflns_number_total 3126 _reflns_number_gt 2707 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0098P)^2^+6.2974P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3126 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.57232(5) 0.55333(2) 0.67582(5) 0.03003(14) Uani 1 1 d . . . Br2 Br 0.83339(5) 0.45055(2) 0.93064(5) 0.02915(13) Uani 1 1 d . . . Br3 Br 0.76820(5) 0.62250(2) 1.02704(5) 0.03127(14) Uani 1 1 d . . . Br4 Br 0.37961(5) 0.66044(2) 0.88484(5) 0.03289(14) Uani 1 1 d . . . Br5 Br 0.20394(5) 0.50554(2) 0.70313(5) 0.03192(14) Uani 1 1 d . . . Br6 Br 0.48257(5) 0.38095(2) 0.73195(5) 0.03152(14) Uani 1 1 d . . . B1 B 0.5343(6) 0.5252(3) 0.8493(6) 0.0253(12) Uani 1 1 d . . . B2 B 0.6558(6) 0.4767(3) 0.9683(6) 0.0251(12) Uani 1 1 d . . . B3 B 0.6251(6) 0.5563(3) 1.0117(6) 0.0250(12) Uani 1 1 d . . . B4 B 0.4430(5) 0.5749(3) 0.9470(6) 0.0237(12) Uani 1 1 d . . . B5 B 0.3623(5) 0.5041(3) 0.8633(5) 0.0233(12) Uani 1 1 d . . . B6 B 0.4926(6) 0.4445(3) 0.8765(6) 0.0243(12) Uani 1 1 d . . . S1 S -0.10324(18) 0.23122(8) 0.4122(2) 0.0676(5) Uani 1 1 d . . . O2 O -0.0734(8) 0.2000(3) 0.2962(5) 0.118(3) Uani 1 1 d . . . O1 O 0.0078(4) 0.26407(18) 0.4964(4) 0.0498(10) Uani 1 1 d . . . S3 S -0.22810(15) 0.39693(8) 0.56909(15) 0.0448(4) Uani 1 1 d . . . O5 O -0.0785(4) 0.4026(2) 0.6030(4) 0.0533(11) Uani 1 1 d . . . O6 O -0.2861(4) 0.3390(2) 0.5091(4) 0.0533(11) Uani 1 1 d . . . S4 S 0.06614(14) 0.40316(7) 0.26856(15) 0.0400(3) Uani 1 1 d . . . O7 O 0.1155(4) 0.40666(19) 0.4151(4) 0.0475(10) Uani 1 1 d . . . O8 O 0.0018(4) 0.34539(19) 0.2136(4) 0.0542(11) Uani 1 1 d . . . S2 S 0.37990(15) 0.22754(7) 0.85968(15) 0.0398(3) Uani 1 1 d . . . O3 O 0.2732(4) 0.25019(18) 0.7489(4) 0.0462(10) Uani 1 1 d . . . O4 O 0.3370(4) 0.20078(18) 0.9734(4) 0.0513(11) Uani 1 1 d . . . Na1 Na 0.1497(2) 0.34442(11) 0.6261(2) 0.0544(6) Uani 1 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 Br1 0.0308(3) 0.0378(3) 0.0236(3) 0.0034(2) 0.0105(2) -0.0015(2) Br2 0.0231(3) 0.0352(3) 0.0312(3) -0.0002(2) 0.0105(2) 0.0020(2) Br3 0.0285(3) 0.0324(3) 0.0354(3) -0.0045(2) 0.0124(2) -0.0089(2) Br4 0.0337(3) 0.0288(3) 0.0375(3) 0.0055(2) 0.0110(2) 0.0036(2) Br5 0.0253(3) 0.0430(3) 0.0249(3) -0.0009(2) 0.0008(2) -0.0010(2) Br6 0.0333(3) 0.0342(3) 0.0294(3) -0.0101(2) 0.0120(2) -0.0061(2) B1 0.026(3) 0.028(3) 0.022(3) 0.003(2) 0.007(2) -0.002(2) B2 0.025(3) 0.028(3) 0.023(3) 0.000(2) 0.008(2) -0.005(2) B3 0.024(3) 0.027(3) 0.025(3) -0.006(2) 0.007(2) -0.004(2) B4 0.022(3) 0.027(3) 0.024(3) 0.001(2) 0.008(2) 0.003(2) B5 0.023(3) 0.025(3) 0.023(3) 0.001(2) 0.006(2) -0.003(2) B6 0.026(3) 0.028(3) 0.019(3) -0.001(2) 0.004(2) -0.005(2) S1 0.0533(10) 0.0492(10) 0.0906(15) -0.0171(10) -0.0033(10) 0.0018(8) O2 0.225(8) 0.062(3) 0.052(3) -0.008(3) 0.004(4) -0.043(4) O1 0.055(3) 0.049(2) 0.040(2) 0.0009(19) 0.001(2) -0.007(2) S3 0.0434(8) 0.0560(10) 0.0387(8) 0.0005(7) 0.0172(7) 0.0010(7) O5 0.041(2) 0.078(3) 0.045(3) -0.001(2) 0.017(2) -0.010(2) O6 0.042(2) 0.055(3) 0.060(3) -0.005(2) 0.005(2) 0.001(2) S4 0.0332(7) 0.0510(9) 0.0384(8) 0.0072(7) 0.0140(6) 0.0056(6) O7 0.038(2) 0.065(3) 0.040(2) 0.002(2) 0.0088(18) -0.0012(19) O8 0.067(3) 0.045(2) 0.046(3) 0.002(2) 0.005(2) 0.004(2) S2 0.0416(8) 0.0384(8) 0.0379(8) 0.0021(6) 0.0061(7) -0.0020(6) O3 0.056(2) 0.044(2) 0.034(2) 0.0016(18) 0.0014(19) -0.0060(19) O4 0.073(3) 0.042(2) 0.040(2) 0.0065(19) 0.017(2) 0.003(2) Na1 0.0560(15) 0.0460(14) 0.0493(15) 0.0061(11) -0.0122(12) -0.0002(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 Br1 B1 1.945(6) . ? Br2 B2 1.945(5) . ? Br3 B3 1.955(5) . ? Br4 B4 1.953(5) . ? Br5 B5 1.953(5) . ? Br6 B6 1.950(5) . ? B1 B6 1.779(7) . ? B1 B5 1.782(7) . ? B1 B3 1.782(8) . ? B1 B2 1.792(8) . ? B1 B4 1.801(8) . ? B2 B3 1.769(8) . ? B2 B5 1.777(7) 3_667 ? B2 B6 1.782(7) . ? B2 B4 1.791(7) 3_667 ? B3 B5 1.763(8) 3_667 ? B3 B6 1.783(7) 3_667 ? B3 B4 1.795(7) . ? B4 B6 1.774(7) 3_667 ? B4 B2 1.791(7) 3_667 ? B4 B5 1.795(7) . ? B5 B3 1.763(8) 3_667 ? B5 B6 1.772(7) . ? B5 B2 1.777(7) 3_667 ? B6 B4 1.774(7) 3_667 ? B6 B3 1.783(7) 3_667 ? S1 O1 1.394(4) . ? S1 O2 1.419(6) . ? S3 O6 1.415(4) . ? S3 O5 1.432(4) . ? S4 O8 1.417(4) . ? S4 O7 1.431(4) . ? S2 O4 1.416(4) . ? S2 O3 1.416(4) . ? 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 B6 B1 B5 59.7(3) . . ? B6 B1 B3 107.1(4) . . ? B5 B1 B3 107.6(4) . . ? B6 B1 B2 59.9(3) . . ? B5 B1 B2 107.6(4) . . ? B3 B1 B2 59.4(3) . . ? B6 B1 B4 107.9(4) . . ? B5 B1 B4 60.1(3) . . ? B3 B1 B4 60.1(3) . . ? B2 B1 B4 107.9(4) . . ? B6 B1 Br1 121.5(4) . . ? B5 B1 Br1 121.8(3) . . ? B3 B1 Br1 122.7(3) . . ? B2 B1 Br1 121.8(3) . . ? B4 B1 Br1 121.9(3) . . ? B3 B2 B5 59.6(3) . 3_667 ? B3 B2 B6 107.5(4) . . ? B5 B2 B6 107.3(4) 3_667 . ? B3 B2 B4 108.3(4) . 3_667 ? B5 B2 B4 60.4(3) 3_667 3_667 ? B6 B2 B4 59.5(3) . 3_667 ? B3 B2 B1 60.0(3) . . ? B5 B2 B1 107.5(4) 3_667 . ? B6 B2 B1 59.7(3) . . ? B4 B2 B1 107.9(4) 3_667 . ? B3 B2 Br2 121.6(3) . . ? B5 B2 Br2 122.5(3) 3_667 . ? B6 B2 Br2 122.1(3) . . ? B4 B2 Br2 121.9(3) 3_667 . ? B1 B2 Br2 121.3(3) . . ? B5 B3 B2 60.4(3) 3_667 . ? B5 B3 B1 108.6(4) 3_667 . ? B2 B3 B1 60.6(3) . . ? B5 B3 B6 60.0(3) 3_667 3_667 ? B2 B3 B6 108.4(4) . 3_667 ? B1 B3 B6 107.8(4) . 3_667 ? B5 B3 B4 108.1(4) 3_667 . ? B2 B3 B4 109.2(4) . . ? B1 B3 B4 60.5(3) . . ? B6 B3 B4 59.5(3) 3_667 . ? B5 B3 Br3 121.6(3) 3_667 . ? B2 B3 Br3 122.0(3) . . ? B1 B3 Br3 121.9(3) . . ? B6 B3 Br3 121.1(3) 3_667 . ? B4 B3 Br3 120.7(3) . . ? B6 B4 B2 60.0(3) 3_667 3_667 ? B6 B4 B5 106.8(4) 3_667 . ? B2 B4 B5 59.4(3) 3_667 . ? B6 B4 B3 59.9(3) 3_667 . ? B2 B4 B3 107.6(4) 3_667 . ? B5 B4 B3 106.4(4) . . ? B6 B4 B1 107.3(4) 3_667 . ? B2 B4 B1 107.3(4) 3_667 . ? B5 B4 B1 59.4(3) . . ? B3 B4 B1 59.4(3) . . ? B6 B4 Br4 122.6(3) 3_667 . ? B2 B4 Br4 122.5(3) 3_667 . ? B5 B4 Br4 122.6(3) . . ? B3 B4 Br4 122.1(3) . . ? B1 B4 Br4 121.4(3) . . ? B3 B5 B6 60.6(3) 3_667 . ? B3 B5 B2 60.0(3) 3_667 3_667 ? B6 B5 B2 108.6(4) . 3_667 ? B3 B5 B1 108.8(4) 3_667 . ? B6 B5 B1 60.1(3) . . ? B2 B5 B1 108.8(4) 3_667 . ? B3 B5 B4 108.4(4) 3_667 . ? B6 B5 B4 108.5(4) . . ? B2 B5 B4 60.2(3) 3_667 . ? B1 B5 B4 60.5(3) . . ? B3 B5 Br5 120.1(3) 3_667 . ? B6 B5 Br5 119.6(3) . . ? B2 B5 Br5 122.4(3) 3_667 . ? B1 B5 Br5 121.3(3) . . ? B4 B5 Br5 123.3(3) . . ? B5 B6 B4 108.6(4) . 3_667 ? B5 B6 B1 60.2(3) . . ? B4 B6 B1 109.2(4) 3_667 . ? B5 B6 B2 108.5(4) . . ? B4 B6 B2 60.5(3) 3_667 . ? B1 B6 B2 60.4(3) . . ? B5 B6 B3 59.5(3) . 3_667 ? B4 B6 B3 60.6(3) 3_667 3_667 ? B1 B6 B3 108.1(4) . 3_667 ? B2 B6 B3 108.5(4) . 3_667 ? B5 B6 Br6 121.1(3) . . ? B4 B6 Br6 121.5(3) 3_667 . ? B1 B6 Br6 120.8(3) . . ? B2 B6 Br6 121.6(3) . . ? B3 B6 Br6 121.9(3) 3_667 . ? O1 S1 O2 116.1(4) . . ? O6 S3 O5 117.4(3) . . ? O8 S4 O7 117.0(3) . . ? O4 S2 O3 117.1(3) . . ? 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 B6 B1 B2 B3 -137.6(4) . . . . ? B5 B1 B2 B3 -100.3(4) . . . . ? B4 B1 B2 B3 -36.9(3) . . . . ? Br1 B1 B2 B3 111.8(4) . . . . ? B6 B1 B2 B5 -100.1(4) . . . 3_667 ? B5 B1 B2 B5 -62.9(5) . . . 3_667 ? B3 B1 B2 B5 37.5(3) . . . 3_667 ? B4 B1 B2 B5 0.6(5) . . . 3_667 ? Br1 B1 B2 B5 149.3(3) . . . 3_667 ? B5 B1 B2 B6 37.2(4) . . . . ? B3 B1 B2 B6 137.6(4) . . . . ? B4 B1 B2 B6 100.7(4) . . . . ? Br1 B1 B2 B6 -110.6(4) . . . . ? B6 B1 B2 B4 -36.4(4) . . . 3_667 ? B5 B1 B2 B4 0.8(5) . . . 3_667 ? B3 B1 B2 B4 101.2(4) . . . 3_667 ? B4 B1 B2 B4 64.3(5) . . . 3_667 ? Br1 B1 B2 B4 -147.0(4) . . . 3_667 ? B6 B1 B2 Br2 111.4(4) . . . . ? B5 B1 B2 Br2 148.7(3) . . . . ? B3 B1 B2 Br2 -111.0(4) . . . . ? B4 B1 B2 Br2 -147.9(3) . . . . ? Br1 B1 B2 Br2 0.8(6) . . . . ? B6 B2 B3 B5 100.1(4) . . . 3_667 ? B4 B2 B3 B5 37.2(3) 3_667 . . 3_667 ? B1 B2 B3 B5 137.8(4) . . . 3_667 ? Br2 B2 B3 B5 -111.8(4) . . . 3_667 ? B5 B2 B3 B1 -137.8(4) 3_667 . . . ? B6 B2 B3 B1 -37.6(3) . . . . ? B4 B2 B3 B1 -100.5(4) 3_667 . . . ? Br2 B2 B3 B1 110.4(4) . . . . ? B5 B2 B3 B6 -37.2(3) 3_667 . . 3_667 ? B6 B2 B3 B6 62.9(5) . . . 3_667 ? B4 B2 B3 B6 0.0(5) 3_667 . . 3_667 ? B1 B2 B3 B6 100.5(4) . . . 3_667 ? Br2 B2 B3 B6 -149.0(3) . . . 3_667 ? B5 B2 B3 B4 -100.4(4) 3_667 . . . ? B6 B2 B3 B4 -0.3(5) . . . . ? B4 B2 B3 B4 -63.2(5) 3_667 . . . ? B1 B2 B3 B4 37.4(4) . . . . ? Br2 B2 B3 B4 147.8(4) . . . . ? B5 B2 B3 Br3 110.9(4) 3_667 . . . ? B6 B2 B3 Br3 -149.0(4) . . . . ? B4 B2 B3 Br3 148.1(4) 3_667 . . . ? B1 B2 B3 Br3 -111.3(4) . . . . ? Br2 B2 B3 Br3 -0.9(6) . . . . ? B6 B1 B3 B5 -0.4(5) . . . 3_667 ? B5 B1 B3 B5 62.4(5) . . . 3_667 ? B2 B1 B3 B5 -38.0(3) . . . 3_667 ? B4 B1 B3 B5 100.8(4) . . . 3_667 ? Br1 B1 B3 B5 -148.4(4) . . . 3_667 ? B6 B1 B3 B2 37.6(3) . . . . ? B5 B1 B3 B2 100.5(4) . . . . ? B4 B1 B3 B2 138.8(4) . . . . ? Br1 B1 B3 B2 -110.3(4) . . . . ? B6 B1 B3 B6 -63.9(5) . . . 3_667 ? B5 B1 B3 B6 -1.1(5) . . . 3_667 ? B2 B1 B3 B6 -101.5(4) . . . 3_667 ? B4 B1 B3 B6 37.3(4) . . . 3_667 ? Br1 B1 B3 B6 148.2(4) . . . 3_667 ? B6 B1 B3 B4 -101.2(4) . . . . ? B5 B1 B3 B4 -38.3(3) . . . . ? B2 B1 B3 B4 -138.8(4) . . . . ? Br1 B1 B3 B4 110.9(4) . . . . ? B6 B1 B3 Br3 149.0(4) . . . . ? B5 B1 B3 Br3 -148.1(4) . . . . ? B2 B1 B3 Br3 111.4(4) . . . . ? B4 B1 B3 Br3 -109.8(4) . . . . ? Br1 B1 B3 Br3 1.1(6) . . . . ? B5 B3 B4 B6 36.5(4) 3_667 . . 3_667 ? B2 B3 B4 B6 100.6(4) . . . 3_667 ? B1 B3 B4 B6 138.0(4) . . . 3_667 ? Br3 B3 B4 B6 -110.3(4) . . . 3_667 ? B5 B3 B4 B2 -1.4(5) 3_667 . . 3_667 ? B2 B3 B4 B2 62.7(5) . . . 3_667 ? B1 B3 B4 B2 100.1(4) . . . 3_667 ? B6 B3 B4 B2 -37.8(4) 3_667 . . 3_667 ? Br3 B3 B4 B2 -148.1(3) . . . 3_667 ? B5 B3 B4 B5 -63.8(5) 3_667 . . . ? B2 B3 B4 B5 0.3(5) . . . . ? B1 B3 B4 B5 37.7(3) . . . . ? B6 B3 B4 B5 -100.2(4) 3_667 . . . ? Br3 B3 B4 B5 149.5(3) . . . . ? B5 B3 B4 B1 -101.5(4) 3_667 . . . ? B2 B3 B4 B1 -37.4(4) . . . . ? B6 B3 B4 B1 -138.0(4) 3_667 . . . ? Br3 B3 B4 B1 111.8(4) . . . . ? B5 B3 B4 Br4 148.3(3) 3_667 . . . ? B2 B3 B4 Br4 -147.5(4) . . . . ? B1 B3 B4 Br4 -110.1(4) . . . . ? B6 B3 B4 Br4 111.9(4) 3_667 . . . ? Br3 B3 B4 Br4 1.6(6) . . . . ? B6 B1 B4 B6 62.4(5) . . . 3_667 ? B5 B1 B4 B6 99.6(4) . . . 3_667 ? B3 B1 B4 B6 -37.4(3) . . . 3_667 ? B2 B1 B4 B6 -0.8(5) . . . 3_667 ? Br1 B1 B4 B6 -149.5(3) . . . 3_667 ? B6 B1 B4 B2 -0.7(5) . . . 3_667 ? B5 B1 B4 B2 36.5(3) . . . 3_667 ? B3 B1 B4 B2 -100.5(4) . . . 3_667 ? B2 B1 B4 B2 -64.0(5) . . . 3_667 ? Br1 B1 B4 B2 147.4(3) . . . 3_667 ? B6 B1 B4 B5 -37.2(3) . . . . ? B3 B1 B4 B5 -137.0(4) . . . . ? B2 B1 B4 B5 -100.4(4) . . . . ? Br1 B1 B4 B5 110.9(4) . . . . ? B6 B1 B4 B3 99.8(4) . . . . ? B5 B1 B4 B3 137.0(4) . . . . ? B2 B1 B4 B3 36.5(3) . . . . ? Br1 B1 B4 B3 -112.1(4) . . . . ? B6 B1 B4 Br4 -149.0(3) . . . . ? B5 B1 B4 Br4 -111.8(4) . . . . ? B3 B1 B4 Br4 111.2(4) . . . . ? B2 B1 B4 Br4 147.7(3) . . . . ? Br1 B1 B4 Br4 -0.9(6) . . . . ? B6 B1 B5 B3 37.3(4) . . . 3_667 ? B3 B1 B5 B3 -62.6(5) . . . 3_667 ? B2 B1 B5 B3 0.0(5) . . . 3_667 ? B4 B1 B5 B3 -100.9(4) . . . 3_667 ? Br1 B1 B5 B3 147.9(4) . . . 3_667 ? B3 B1 B5 B6 -99.9(4) . . . . ? B2 B1 B5 B6 -37.3(3) . . . . ? B4 B1 B5 B6 -138.2(4) . . . . ? Br1 B1 B5 B6 110.5(4) . . . . ? B6 B1 B5 B2 101.1(4) . . . 3_667 ? B3 B1 B5 B2 1.2(5) . . . 3_667 ? B2 B1 B5 B2 63.8(5) . . . 3_667 ? B4 B1 B5 B2 -37.2(4) . . . 3_667 ? Br1 B1 B5 B2 -148.4(4) . . . 3_667 ? B6 B1 B5 B4 138.2(4) . . . . ? B3 B1 B5 B4 38.3(4) . . . . ? B2 B1 B5 B4 100.9(4) . . . . ? Br1 B1 B5 B4 -111.2(4) . . . . ? B6 B1 B5 Br5 -108.5(4) . . . . ? B3 B1 B5 Br5 151.6(3) . . . . ? B2 B1 B5 Br5 -145.8(4) . . . . ? B4 B1 B5 Br5 113.3(4) . . . . ? Br1 B1 B5 Br5 2.0(6) . . . . ? B6 B4 B5 B3 1.1(5) 3_667 . . 3_667 ? B2 B4 B5 B3 -37.1(3) 3_667 . . 3_667 ? B3 B4 B5 B3 63.9(5) . . . 3_667 ? B1 B4 B5 B3 101.7(4) . . . 3_667 ? Br4 B4 B5 B3 -148.4(3) . . . 3_667 ? B6 B4 B5 B6 -63.1(5) 3_667 . . . ? B2 B4 B5 B6 -101.3(4) 3_667 . . . ? B3 B4 B5 B6 -0.2(5) . . . . ? B1 B4 B5 B6 37.5(3) . . . . ? Br4 B4 B5 B6 147.4(3) . . . . ? B6 B4 B5 B2 38.2(3) 3_667 . . 3_667 ? B3 B4 B5 B2 101.0(4) . . . 3_667 ? B1 B4 B5 B2 138.8(4) . . . 3_667 ? Br4 B4 B5 B2 -111.3(4) . . . 3_667 ? B6 B4 B5 B1 -100.6(4) 3_667 . . . ? B2 B4 B5 B1 -138.8(4) 3_667 . . . ? B3 B4 B5 B1 -37.7(3) . . . . ? Br4 B4 B5 B1 109.9(4) . . . . ? B6 B4 B5 Br5 149.4(3) 3_667 . . . ? B2 B4 B5 Br5 111.2(4) 3_667 . . . ? B3 B4 B5 Br5 -147.8(4) . . . . ? B1 B4 B5 Br5 -110.0(4) . . . . ? Br4 B4 B5 Br5 -0.1(6) . . . . ? B3 B5 B6 B4 -36.9(3) 3_667 . . 3_667 ? B2 B5 B6 B4 0.4(5) 3_667 . . 3_667 ? B1 B5 B6 B4 101.9(4) . . . 3_667 ? B4 B5 B6 B4 64.3(5) . . . 3_667 ? Br5 B5 B6 B4 -146.8(3) . . . 3_667 ? B3 B5 B6 B1 -138.8(4) 3_667 . . . ? B2 B5 B6 B1 -101.5(4) 3_667 . . . ? B4 B5 B6 B1 -37.7(4) . . . . ? Br5 B5 B6 B1 111.3(4) . . . . ? B3 B5 B6 B2 -101.0(4) 3_667 . . . ? B2 B5 B6 B2 -63.8(5) 3_667 . . . ? B1 B5 B6 B2 37.8(4) . . . . ? B4 B5 B6 B2 0.1(5) . . . . ? Br5 B5 B6 B2 149.0(3) . . . . ? B2 B5 B6 B3 37.3(3) 3_667 . . 3_667 ? B1 B5 B6 B3 138.8(4) . . . 3_667 ? B4 B5 B6 B3 101.1(4) . . . 3_667 ? Br5 B5 B6 B3 -110.0(4) . . . 3_667 ? B3 B5 B6 Br6 111.1(4) 3_667 . . . ? B2 B5 B6 Br6 148.4(3) 3_667 . . . ? B1 B5 B6 Br6 -110.1(4) . . . . ? B4 B5 B6 Br6 -147.8(3) . . . . ? Br5 B5 B6 Br6 1.2(5) . . . . ? B3 B1 B6 B5 100.7(4) . . . . ? B2 B1 B6 B5 138.1(4) . . . . ? B4 B1 B6 B5 37.4(3) . . . . ? Br1 B1 B6 B5 -110.9(4) . . . . ? B5 B1 B6 B4 -101.0(4) . . . 3_667 ? B3 B1 B6 B4 -0.3(5) . . . 3_667 ? B2 B1 B6 B4 37.1(4) . . . 3_667 ? B4 B1 B6 B4 -63.6(5) . . . 3_667 ? Br1 B1 B6 B4 148.1(4) . . . 3_667 ? B5 B1 B6 B2 -138.1(4) . . . . ? B3 B1 B6 B2 -37.4(3) . . . . ? B4 B1 B6 B2 -100.7(4) . . . . ? Br1 B1 B6 B2 111.0(4) . . . . ? B5 B1 B6 B3 -36.7(3) . . . 3_667 ? B3 B1 B6 B3 64.1(5) . . . 3_667 ? B2 B1 B6 B3 101.4(4) . . . 3_667 ? B4 B1 B6 B3 0.7(5) . . . 3_667 ? Br1 B1 B6 B3 -147.6(3) . . . 3_667 ? B5 B1 B6 Br6 110.6(4) . . . . ? B3 B1 B6 Br6 -148.7(3) . . . . ? B2 B1 B6 Br6 -111.3(4) . . . . ? B4 B1 B6 Br6 147.9(3) . . . . ? Br1 B1 B6 Br6 -0.3(6) . . . . ? B3 B2 B6 B5 0.1(5) . . . . ? B5 B2 B6 B5 62.9(5) 3_667 . . . ? B4 B2 B6 B5 101.4(4) 3_667 . . . ? B1 B2 B6 B5 -37.7(4) . . . . ? Br2 B2 B6 B5 -147.8(3) . . . . ? B3 B2 B6 B4 -101.3(4) . . . 3_667 ? B5 B2 B6 B4 -38.5(3) 3_667 . . 3_667 ? B1 B2 B6 B4 -139.1(4) . . . 3_667 ? Br2 B2 B6 B4 110.8(4) . . . 3_667 ? B3 B2 B6 B1 37.8(4) . . . . ? B5 B2 B6 B1 100.6(4) 3_667 . . . ? B4 B2 B6 B1 139.1(4) 3_667 . . . ? Br2 B2 B6 B1 -110.1(4) . . . . ? B3 B2 B6 B3 -63.0(5) . . . 3_667 ? B5 B2 B6 B3 -0.2(5) 3_667 . . 3_667 ? B4 B2 B6 B3 38.4(4) 3_667 . . 3_667 ? B1 B2 B6 B3 -100.7(4) . . . 3_667 ? Br2 B2 B6 B3 149.2(4) . . . 3_667 ? B3 B2 B6 Br6 147.8(4) . . . . ? B5 B2 B6 Br6 -149.4(3) 3_667 . . . ? B4 B2 B6 Br6 -110.9(4) 3_667 . . . ? B1 B2 B6 Br6 110.0(4) . . . . ? Br2 B2 B6 Br6 -0.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.747 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.106 #===END data_ck-mr-04 _database_code_depnum_ccdc_archive 'CCDC 778604' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B12 I12, 8(O2 S), 2(Na)' _chemical_formula_sum 'B12 I12 Na2 O16 S8' _chemical_formula_weight 2210.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 19.834(4) _cell_length_b 20.079(4) _cell_length_c 11.421(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4548.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 35.0 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3896 _exptl_absorpt_coefficient_mu 8.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.197 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; March 2001 T Higashi ; _exptl_special_details ; Rigaku CrystalClear-SM Expert 2.0 r1 ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector RX _diffrn_measurement_device_type 'Rigaku R-AXIS Spider' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 10.0000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 195674 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5363 _reflns_number_gt 5190 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+15.7724P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5363 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0403 _refine_ls_wR_factor_gt 0.0400 _refine_ls_goodness_of_fit_ref 1.282 _refine_ls_restrained_S_all 1.282 _refine_ls_shift/su_max 0.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.21288(17) 0.17740(18) 0.3951(3) 0.0148(7) Uani 1 1 d . . . I1 I 0.187671(12) 0.085133(11) 0.48263(2) 0.02493(6) Uani 1 1 d . . . B2 B 0.1606(2) 0.2500 0.4058(4) 0.0146(9) Uani 1 2 d S . . I2 I 0.069609(15) 0.2500 0.51086(3) 0.02015(7) Uani 1 2 d S . . B3 B 0.16616(17) 0.20561(17) 0.2697(3) 0.0138(6) Uani 1 1 d . . . I3 I 0.082804(10) 0.148976(11) 0.198300(19) 0.02090(5) Uani 1 1 d . . . B4 B 0.25128(17) 0.17812(18) 0.2539(3) 0.0138(6) Uani 1 1 d . . . I4 I 0.276290(11) 0.086666(11) 0.16168(2) 0.02166(5) Uani 1 1 d . . . B5 B 0.29810(17) 0.20566(18) 0.3794(3) 0.0145(7) Uani 1 1 d . . . I5 I 0.382243(11) 0.149039(11) 0.44710(2) 0.02241(5) Uani 1 1 d . . . B6 B 0.2413(2) 0.2500 0.4731(4) 0.0158(10) Uani 1 2 d S . . I6 I 0.251376(17) 0.2500 0.66085(3) 0.02628(8) Uani 1 2 d S . . B7 B 0.2228(2) 0.2500 0.1766(4) 0.0137(9) Uani 1 2 d S . . I7 I 0.210761(15) 0.2500 -0.01228(3) 0.02124(7) Uani 1 2 d S . . B8 B 0.3040(2) 0.2500 0.2433(4) 0.0116(9) Uani 1 2 d S . . I8 I 0.398022(14) 0.2500 0.14828(3) 0.01658(6) Uani 1 2 d S . . O1 O 0.6118(3) 0.0303(2) 0.5420(4) 0.0862(16) Uani 1 1 d . . . S1 S 0.65851(8) 0.06026(7) 0.61678(12) 0.0553(3) Uani 1 1 d . . . O2 O 0.63230(18) 0.09317(18) 0.7165(3) 0.0492(8) Uani 1 1 d . . . O3 O 0.8159(2) 0.0771(2) 0.7054(4) 0.0712(12) Uani 1 1 d . . . S2 S 0.85701(7) 0.04737(6) 0.78872(12) 0.0495(3) Uani 1 1 d . . . O4 O 0.92823(18) 0.05315(16) 0.7783(3) 0.0495(8) Uani 1 1 d . . . O5 O 0.47349(17) 0.08565(17) 0.0046(3) 0.0453(8) Uani 1 1 d . . . S3 S 0.45589(5) 0.07534(4) 0.12309(9) 0.02724(19) Uani 1 1 d . . . O6 O 0.45241(17) 0.00842(15) 0.1629(3) 0.0465(8) Uani 1 1 d . . . O7 O 0.53093(17) 0.18967(17) 0.6426(3) 0.0471(8) Uani 1 1 d . . . S4 S 0.53018(7) 0.2500 0.57824(12) 0.0296(3) Uani 1 2 d S . . O8 O 0.92652(16) 0.18998(15) 0.6676(3) 0.0400(7) Uani 1 1 d . . . S5 S 0.88963(6) 0.2500 0.65164(11) 0.0236(2) Uani 1 2 d S . . Na1 Na 0.52200(9) 0.10933(8) 0.81069(15) 0.0363(4) Uani 1 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 B1 0.0142(16) 0.0152(16) 0.0149(16) 0.0014(13) -0.0003(13) 0.0003(13) I1 0.02729(12) 0.02096(11) 0.02655(12) 0.01017(9) 0.00300(9) -0.00306(9) B2 0.012(2) 0.018(2) 0.014(2) 0.000 0.0005(18) 0.000 I2 0.01452(13) 0.02919(16) 0.01676(14) 0.000 0.00500(11) 0.000 B3 0.0124(15) 0.0158(16) 0.0131(16) -0.0024(13) -0.0009(12) -0.0006(13) I3 0.01645(10) 0.02612(11) 0.02012(11) -0.00302(9) -0.00171(8) -0.00698(8) B4 0.0124(15) 0.0156(16) 0.0134(16) -0.0010(13) 0.0000(12) -0.0011(13) I4 0.02026(10) 0.01671(10) 0.02800(12) -0.00780(9) 0.00267(9) 0.00025(8) B5 0.0119(15) 0.0184(16) 0.0133(16) 0.0008(13) -0.0015(12) -0.0006(13) I5 0.01713(10) 0.02504(11) 0.02505(11) 0.00741(9) -0.00360(8) 0.00449(8) B6 0.013(2) 0.022(3) 0.013(2) 0.000 -0.0001(18) 0.000 I6 0.02505(16) 0.0440(2) 0.00983(14) 0.000 -0.00216(12) 0.000 B7 0.013(2) 0.016(2) 0.013(2) 0.000 0.0023(18) 0.000 I7 0.01852(14) 0.03561(18) 0.00959(13) 0.000 0.00010(11) 0.000 B8 0.010(2) 0.014(2) 0.011(2) 0.000 0.0006(17) 0.000 I8 0.01319(13) 0.01901(14) 0.01755(14) 0.000 0.00417(11) 0.000 O1 0.157(5) 0.051(2) 0.051(2) 0.001(2) -0.012(3) -0.009(3) S1 0.0656(9) 0.0608(8) 0.0394(7) 0.0115(6) 0.0157(6) 0.0174(7) O2 0.053(2) 0.060(2) 0.0342(17) 0.0022(16) 0.0061(15) -0.0013(17) O3 0.056(2) 0.066(3) 0.091(3) -0.006(2) -0.001(2) -0.015(2) S2 0.0628(8) 0.0373(6) 0.0484(7) -0.0078(5) 0.0138(6) -0.0193(6) O4 0.055(2) 0.0367(18) 0.057(2) 0.0025(16) 0.0148(17) -0.0010(15) O5 0.0473(18) 0.051(2) 0.0378(17) 0.0050(15) 0.0024(15) 0.0021(16) S3 0.0258(4) 0.0209(4) 0.0350(5) -0.0010(4) -0.0026(4) 0.0025(4) O6 0.0460(18) 0.0281(15) 0.065(2) 0.0132(15) 0.0084(16) 0.0093(14) O7 0.0446(18) 0.053(2) 0.0440(19) 0.0182(16) 0.0024(15) -0.0067(16) S4 0.0285(7) 0.0395(8) 0.0206(6) 0.000 0.0029(5) 0.000 O8 0.0480(18) 0.0308(16) 0.0411(17) 0.0052(13) 0.0031(14) 0.0070(13) S5 0.0174(5) 0.0321(7) 0.0213(6) 0.000 0.0006(5) 0.000 Na1 0.0428(9) 0.0280(8) 0.0382(9) 0.0047(7) 0.0081(8) 0.0044(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 B1 B4 1.784(5) . ? B1 B5 1.792(5) . ? B1 B2 1.793(5) . ? B1 B3 1.798(5) . ? B1 B6 1.799(5) . ? B1 I1 2.164(4) . ? B2 B6 1.774(7) . ? B2 B1 1.793(5) 7_565 ? B2 B3 1.796(6) 7_565 ? B2 B3 1.796(6) . ? B2 I2 2.168(5) . ? I2 Na1 3.6089(18) 4_456 ? I2 Na1 3.6089(18) 6_557 ? B3 B3 1.783(7) 7_565 ? B3 B4 1.785(5) . ? B3 B7 1.786(5) . ? B3 I3 2.166(3) . ? B4 B7 1.784(5) . ? B4 B8 1.786(4) . ? B4 B5 1.795(5) . ? B4 I4 2.174(4) . ? B5 B5 1.780(7) 7_565 ? B5 B6 1.791(6) . ? B5 B8 1.794(6) . ? B5 I5 2.162(3) . ? B6 B5 1.791(6) 7_565 ? B6 B1 1.799(5) 7_565 ? B6 I6 2.154(5) . ? B7 B8 1.781(7) . ? B7 B4 1.784(5) 7_565 ? B7 B3 1.786(5) 7_565 ? B7 I7 2.170(5) . ? B8 B4 1.786(4) 7_565 ? B8 B5 1.794(6) 7_565 ? B8 I8 2.158(5) . ? O1 S1 1.396(5) . ? S1 O2 1.415(4) . ? O2 Na1 2.459(4) . ? O3 S2 1.388(5) . ? S2 O4 1.422(4) . ? O4 Na1 2.401(4) 6_657 ? O5 S3 1.412(3) . ? O5 Na1 2.461(4) 1_554 ? S3 O6 1.420(3) . ? O6 Na1 2.437(3) 5_656 ? O7 S4 1.417(3) . ? O7 Na1 2.513(3) . ? S4 O7 1.417(3) 7_565 ? O8 S5 1.422(3) . ? O8 Na1 2.504(3) 6_657 ? S5 O8 1.422(3) 7_565 ? Na1 O4 2.401(4) 6_557 ? Na1 O6 2.437(3) 5_656 ? Na1 O5 2.461(4) 1_556 ? Na1 O8 2.504(3) 6_557 ? Na1 I2 3.6089(18) 6_657 ? 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 B4 B1 B5 60.26(19) . . ? B4 B1 B2 107.6(3) . . ? B5 B1 B2 107.1(3) . . ? B4 B1 B3 59.79(19) . . ? B5 B1 B3 107.8(2) . . ? B2 B1 B3 60.0(2) . . ? B4 B1 B6 107.9(3) . . ? B5 B1 B6 59.9(2) . . ? B2 B1 B6 59.2(2) . . ? B3 B1 B6 107.5(3) . . ? B4 B1 I1 121.5(2) . . ? B5 B1 I1 122.4(2) . . ? B2 B1 I1 122.1(2) . . ? B3 B1 I1 121.2(2) . . ? B6 B1 I1 122.5(2) . . ? B6 B2 B1 60.56(19) . 7_565 ? B6 B2 B1 60.56(19) . . ? B1 B2 B1 108.8(3) 7_565 . ? B6 B2 B3 108.7(3) . 7_565 ? B1 B2 B3 60.13(19) 7_565 7_565 ? B1 B2 B3 108.0(3) . 7_565 ? B6 B2 B3 108.7(3) . . ? B1 B2 B3 108.0(3) 7_565 . ? B1 B2 B3 60.13(19) . . ? B3 B2 B3 59.5(3) 7_565 . ? B6 B2 I2 120.7(3) . . ? B1 B2 I2 121.28(19) 7_565 . ? B1 B2 I2 121.28(19) . . ? B3 B2 I2 122.0(2) 7_565 . ? B3 B2 I2 122.0(2) . . ? B2 I2 Na1 122.04(6) . 4_456 ? B2 I2 Na1 122.04(6) . 6_557 ? Na1 I2 Na1 103.01(6) 4_456 6_557 ? B3 B3 B4 108.01(16) 7_565 . ? B3 B3 B7 60.06(14) 7_565 . ? B4 B3 B7 59.9(2) . . ? B3 B3 B2 60.24(14) 7_565 . ? B4 B3 B2 107.4(3) . . ? B7 B3 B2 107.8(2) . . ? B3 B3 B1 108.36(16) 7_565 . ? B4 B3 B1 59.71(19) . . ? B7 B3 B1 107.9(3) . . ? B2 B3 B1 59.8(2) . . ? B3 B3 I3 121.67(9) 7_565 . ? B4 B3 I3 121.4(2) . . ? B7 B3 I3 121.2(2) . . ? B2 B3 I3 122.7(2) . . ? B1 B3 I3 121.9(2) . . ? B1 B4 B7 108.6(3) . . ? B1 B4 B3 60.49(19) . . ? B7 B4 B3 60.1(2) . . ? B1 B4 B8 108.5(3) . . ? B7 B4 B8 59.9(2) . . ? B3 B4 B8 108.1(2) . . ? B1 B4 B5 60.1(2) . . ? B7 B4 B5 108.0(3) . . ? B3 B4 B5 108.3(2) . . ? B8 B4 B5 60.1(2) . . ? B1 B4 I4 121.9(2) . . ? B7 B4 I4 121.0(2) . . ? B3 B4 I4 121.7(2) . . ? B8 B4 I4 121.1(2) . . ? B5 B4 I4 121.9(2) . . ? B5 B5 B6 60.20(14) 7_565 . ? B5 B5 B1 108.46(16) 7_565 . ? B6 B5 B1 60.3(2) . . ? B5 B5 B8 60.25(14) 7_565 . ? B6 B5 B8 108.2(2) . . ? B1 B5 B8 107.8(3) . . ? B5 B5 B4 107.95(16) 7_565 . ? B6 B5 B4 107.7(3) . . ? B1 B5 B4 59.64(19) . . ? B8 B5 B4 59.7(2) . . ? B5 B5 I5 121.72(9) 7_565 . ? B6 B5 I5 122.2(2) . . ? B1 B5 I5 121.7(2) . . ? B8 B5 I5 121.4(2) . . ? B4 B5 I5 121.5(2) . . ? B2 B6 B5 108.0(3) . 7_565 ? B2 B6 B5 108.0(3) . . ? B5 B6 B5 59.6(3) 7_565 . ? B2 B6 B1 60.22(19) . 7_565 ? B5 B6 B1 59.89(19) 7_565 7_565 ? B5 B6 B1 107.7(3) . 7_565 ? B2 B6 B1 60.22(19) . . ? B5 B6 B1 107.7(3) 7_565 . ? B5 B6 B1 59.89(19) . . ? B1 B6 B1 108.3(3) 7_565 . ? B2 B6 I6 121.0(3) . . ? B5 B6 I6 122.4(2) 7_565 . ? B5 B6 I6 122.4(2) . . ? B1 B6 I6 121.48(19) 7_565 . ? B1 B6 I6 121.48(19) . . ? B8 B7 B4 60.14(19) . 7_565 ? B8 B7 B4 60.14(19) . . ? B4 B7 B4 108.0(3) 7_565 . ? B8 B7 B3 108.3(3) . . ? B4 B7 B3 107.9(3) 7_565 . ? B4 B7 B3 60.01(19) . . ? B8 B7 B3 108.3(3) . 7_565 ? B4 B7 B3 60.01(19) 7_565 7_565 ? B4 B7 B3 107.9(3) . 7_565 ? B3 B7 B3 59.9(3) . 7_565 ? B8 B7 I7 121.7(3) . . ? B4 B7 I7 121.81(19) 7_565 . ? B4 B7 I7 121.81(19) . . ? B3 B7 I7 121.5(2) . . ? B3 B7 I7 121.5(2) 7_565 . ? B7 B8 B4 60.01(18) . . ? B7 B8 B4 60.01(18) . 7_565 ? B4 B8 B4 107.8(3) . 7_565 ? B7 B8 B5 108.2(3) . 7_565 ? B4 B8 B5 107.7(3) . 7_565 ? B4 B8 B5 60.18(19) 7_565 7_565 ? B7 B8 B5 108.2(3) . . ? B4 B8 B5 60.18(19) . . ? B4 B8 B5 107.7(3) 7_565 . ? B5 B8 B5 59.5(3) 7_565 . ? B7 B8 I8 124.4(3) . . ? B4 B8 I8 122.66(18) . . ? B4 B8 I8 122.66(18) 7_565 . ? B5 B8 I8 119.4(2) 7_565 . ? B5 B8 I8 119.4(2) . . ? O1 S1 O2 116.7(3) . . ? S1 O2 Na1 137.8(2) . . ? O3 S2 O4 119.4(2) . . ? S2 O4 Na1 147.5(2) . 6_657 ? S3 O5 Na1 170.7(2) . 1_554 ? O5 S3 O6 117.2(2) . . ? S3 O6 Na1 161.4(2) . 5_656 ? S4 O7 Na1 160.8(2) . . ? O7 S4 O7 117.5(3) 7_565 . ? S5 O8 Na1 161.8(2) . 6_657 ? O8 S5 O8 115.9(3) 7_565 . ? O4 Na1 O6 76.00(13) 6_557 5_656 ? O4 Na1 O2 116.23(14) 6_557 . ? O6 Na1 O2 74.99(12) 5_656 . ? O4 Na1 O5 89.27(13) 6_557 1_556 ? O6 Na1 O5 77.44(12) 5_656 1_556 ? O2 Na1 O5 135.72(13) . 1_556 ? O4 Na1 O8 76.10(12) 6_557 6_557 ? O6 Na1 O8 140.60(13) 5_656 6_557 ? O2 Na1 O8 143.25(13) . 6_557 ? O5 Na1 O8 74.95(12) 1_556 6_557 ? O4 Na1 O7 91.89(13) 6_557 . ? O6 Na1 O7 134.64(14) 5_656 . ? O2 Na1 O7 71.81(12) . . ? O5 Na1 O7 147.01(14) 1_556 . ? O8 Na1 O7 73.37(12) 6_557 . ? O4 Na1 I2 144.04(10) 6_557 6_657 ? O6 Na1 I2 129.41(11) 5_656 6_657 ? O2 Na1 I2 96.75(10) . 6_657 ? O5 Na1 I2 75.24(9) 1_556 6_657 ? O8 Na1 I2 68.64(8) 6_557 6_657 ? O7 Na1 I2 84.86(10) . 6_657 ? 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 B4 B1 B2 B6 -100.8(3) . . . . ? B5 B1 B2 B6 -37.3(3) . . . . ? B3 B1 B2 B6 -138.4(3) . . . . ? I1 B1 B2 B6 111.4(3) . . . . ? B4 B1 B2 B1 -62.8(4) . . . 7_565 ? B5 B1 B2 B1 0.6(4) . . . 7_565 ? B3 B1 B2 B1 -100.4(3) . . . 7_565 ? B6 B1 B2 B1 38.0(3) . . . 7_565 ? I1 B1 B2 B1 149.37(17) . . . 7_565 ? B4 B1 B2 B3 0.9(3) . . . 7_565 ? B5 B1 B2 B3 64.4(3) . . . 7_565 ? B3 B1 B2 B3 -36.7(2) . . . 7_565 ? B6 B1 B2 B3 101.7(3) . . . 7_565 ? I1 B1 B2 B3 -146.9(2) . . . 7_565 ? B4 B1 B2 B3 37.6(2) . . . . ? B5 B1 B2 B3 101.1(3) . . . . ? B6 B1 B2 B3 138.4(3) . . . . ? I1 B1 B2 B3 -110.2(3) . . . . ? B4 B1 B2 I2 149.1(3) . . . . ? B5 B1 B2 I2 -147.4(3) . . . . ? B3 B1 B2 I2 111.5(3) . . . . ? B6 B1 B2 I2 -110.1(4) . . . . ? I1 B1 B2 I2 1.3(4) . . . . ? B6 B2 I2 Na1 67.41(8) . . . 4_456 ? B1 B2 I2 Na1 -4.7(4) 7_565 . . 4_456 ? B1 B2 I2 Na1 139.5(2) . . . 4_456 ? B3 B2 I2 Na1 -76.8(3) 7_565 . . 4_456 ? B3 B2 I2 Na1 -148.42(16) . . . 4_456 ? B6 B2 I2 Na1 -67.41(8) . . . 6_557 ? B1 B2 I2 Na1 -139.5(2) 7_565 . . 6_557 ? B1 B2 I2 Na1 4.7(4) . . . 6_557 ? B3 B2 I2 Na1 148.42(16) 7_565 . . 6_557 ? B3 B2 I2 Na1 76.8(3) . . . 6_557 ? B6 B2 B3 B3 -101.1(2) . . . 7_565 ? B1 B2 B3 B3 -36.96(16) 7_565 . . 7_565 ? B1 B2 B3 B3 -138.8(2) . . . 7_565 ? I2 B2 B3 B3 110.9(2) . . . 7_565 ? B6 B2 B3 B4 0.1(3) . . . . ? B1 B2 B3 B4 64.2(3) 7_565 . . . ? B1 B2 B3 B4 -37.5(2) . . . . ? B3 B2 B3 B4 101.2(2) 7_565 . . . ? I2 B2 B3 B4 -147.9(2) . . . . ? B6 B2 B3 B7 -63.1(3) . . . . ? B1 B2 B3 B7 1.0(3) 7_565 . . . ? B1 B2 B3 B7 -100.8(3) . . . . ? B3 B2 B3 B7 38.0(3) 7_565 . . . ? I2 B2 B3 B7 148.9(2) . . . . ? B6 B2 B3 B1 37.6(2) . . . . ? B1 B2 B3 B1 101.8(3) 7_565 . . . ? B3 B2 B3 B1 138.8(2) 7_565 . . . ? I2 B2 B3 B1 -110.3(2) . . . . ? B6 B2 B3 I3 148.3(2) . . . . ? B1 B2 B3 I3 -147.5(2) 7_565 . . . ? B1 B2 B3 I3 110.7(3) . . . . ? B3 B2 B3 I3 -110.59(19) 7_565 . . . ? I2 B2 B3 I3 0.4(3) . . . . ? B4 B1 B3 B3 -100.57(17) . . . 7_565 ? B5 B1 B3 B3 -62.8(2) . . . 7_565 ? B2 B1 B3 B3 37.09(18) . . . 7_565 ? B6 B1 B3 B3 0.4(3) . . . 7_565 ? I1 B1 B3 B3 148.64(15) . . . 7_565 ? B5 B1 B3 B4 37.8(2) . . . . ? B2 B1 B3 B4 137.7(3) . . . . ? B6 B1 B3 B4 100.9(3) . . . . ? I1 B1 B3 B4 -110.8(3) . . . . ? B4 B1 B3 B7 -37.0(2) . . . . ? B5 B1 B3 B7 0.8(3) . . . . ? B2 B1 B3 B7 100.6(3) . . . . ? B6 B1 B3 B7 63.9(3) . . . . ? I1 B1 B3 B7 -147.8(2) . . . . ? B4 B1 B3 B2 -137.7(3) . . . . ? B5 B1 B3 B2 -99.9(3) . . . . ? B6 B1 B3 B2 -36.7(3) . . . . ? I1 B1 B3 B2 111.6(3) . . . . ? B4 B1 B3 I3 110.4(3) . . . . ? B5 B1 B3 I3 148.2(2) . . . . ? B2 B1 B3 I3 -112.0(3) . . . . ? B6 B1 B3 I3 -148.7(2) . . . . ? I1 B1 B3 I3 -0.4(3) . . . . ? B5 B1 B4 B7 -100.5(3) . . . . ? B2 B1 B4 B7 -0.5(3) . . . . ? B3 B1 B4 B7 37.3(2) . . . . ? B6 B1 B4 B7 -63.0(3) . . . . ? I1 B1 B4 B7 147.6(2) . . . . ? B5 B1 B4 B3 -137.8(3) . . . . ? B2 B1 B4 B3 -37.7(2) . . . . ? B6 B1 B4 B3 -100.2(3) . . . . ? I1 B1 B4 B3 110.3(3) . . . . ? B5 B1 B4 B8 -37.0(2) . . . . ? B2 B1 B4 B8 63.0(3) . . . . ? B3 B1 B4 B8 100.8(3) . . . . ? B6 B1 B4 B8 0.5(3) . . . . ? I1 B1 B4 B8 -148.9(2) . . . . ? B2 B1 B4 B5 100.1(3) . . . . ? B3 B1 B4 B5 137.8(3) . . . . ? B6 B1 B4 B5 37.6(2) . . . . ? I1 B1 B4 B5 -111.9(3) . . . . ? B5 B1 B4 I4 111.1(3) . . . . ? B2 B1 B4 I4 -148.8(2) . . . . ? B3 B1 B4 I4 -111.1(3) . . . . ? B6 B1 B4 I4 148.7(2) . . . . ? I1 B1 B4 I4 -0.8(3) . . . . ? B3 B3 B4 B1 101.17(17) 7_565 . . . ? B7 B3 B4 B1 138.5(3) . . . . ? B2 B3 B4 B1 37.6(2) . . . . ? I3 B3 B4 B1 -111.1(3) . . . . ? B3 B3 B4 B7 -37.37(18) 7_565 . . . ? B2 B3 B4 B7 -100.9(3) . . . . ? B1 B3 B4 B7 -138.5(3) . . . . ? I3 B3 B4 B7 110.4(3) . . . . ? B3 B3 B4 B8 -0.3(3) 7_565 . . . ? B7 B3 B4 B8 37.1(3) . . . . ? B2 B3 B4 B8 -63.9(3) . . . . ? B1 B3 B4 B8 -101.5(3) . . . . ? I3 B3 B4 B8 147.5(2) . . . . ? B3 B3 B4 B5 63.4(2) 7_565 . . . ? B7 B3 B4 B5 100.7(3) . . . . ? B2 B3 B4 B5 -0.2(3) . . . . ? B1 B3 B4 B5 -37.8(2) . . . . ? I3 B3 B4 B5 -148.9(2) . . . . ? B3 B3 B4 I4 -147.47(16) 7_565 . . . ? B7 B3 B4 I4 -110.1(3) . . . . ? B2 B3 B4 I4 149.0(2) . . . . ? B1 B3 B4 I4 111.4(3) . . . . ? I3 B3 B4 I4 0.3(4) . . . . ? B4 B1 B5 B5 100.42(17) . . . 7_565 ? B2 B1 B5 B5 -0.4(3) . . . 7_565 ? B3 B1 B5 B5 62.8(2) . . . 7_565 ? B6 B1 B5 B5 -37.42(19) . . . 7_565 ? I1 B1 B5 B5 -149.01(16) . . . 7_565 ? B4 B1 B5 B6 137.8(3) . . . . ? B2 B1 B5 B6 37.0(3) . . . . ? B3 B1 B5 B6 100.3(3) . . . . ? I1 B1 B5 B6 -111.6(3) . . . . ? B4 B1 B5 B8 36.7(2) . . . . ? B2 B1 B5 B8 -64.1(3) . . . . ? B3 B1 B5 B8 -0.9(3) . . . . ? B6 B1 B5 B8 -101.2(3) . . . . ? I1 B1 B5 B8 147.2(2) . . . . ? B2 B1 B5 B4 -100.8(3) . . . . ? B3 B1 B5 B4 -37.6(2) . . . . ? B6 B1 B5 B4 -137.8(3) . . . . ? I1 B1 B5 B4 110.6(3) . . . . ? B4 B1 B5 I5 -110.5(3) . . . . ? B2 B1 B5 I5 148.7(2) . . . . ? B3 B1 B5 I5 -148.1(2) . . . . ? B6 B1 B5 I5 111.6(3) . . . . ? I1 B1 B5 I5 0.1(4) . . . . ? B1 B4 B5 B5 -101.30(17) . . . 7_565 ? B7 B4 B5 B5 0.2(3) . . . 7_565 ? B3 B4 B5 B5 -63.3(2) . . . 7_565 ? B8 B4 B5 B5 37.49(17) . . . 7_565 ? I4 B4 B5 B5 147.58(16) . . . 7_565 ? B1 B4 B5 B6 -37.7(2) . . . . ? B7 B4 B5 B6 63.8(3) . . . . ? B3 B4 B5 B6 0.3(3) . . . . ? B8 B4 B5 B6 101.1(3) . . . . ? I4 B4 B5 B6 -148.8(2) . . . . ? B7 B4 B5 B1 101.5(3) . . . . ? B3 B4 B5 B1 38.0(2) . . . . ? B8 B4 B5 B1 138.8(3) . . . . ? I4 B4 B5 B1 -111.1(3) . . . . ? B1 B4 B5 B8 -138.8(3) . . . . ? B7 B4 B5 B8 -37.2(3) . . . . ? B3 B4 B5 B8 -100.8(3) . . . . ? I4 B4 B5 B8 110.1(3) . . . . ? B1 B4 B5 I5 110.8(3) . . . . ? B7 B4 B5 I5 -147.7(2) . . . . ? B3 B4 B5 I5 148.8(2) . . . . ? B8 B4 B5 I5 -110.4(3) . . . . ? I4 B4 B5 I5 -0.3(4) . . . . ? B1 B2 B6 B5 -37.5(2) 7_565 . . 7_565 ? B1 B2 B6 B5 100.5(3) . . . 7_565 ? B3 B2 B6 B5 -0.1(3) 7_565 . . 7_565 ? B3 B2 B6 B5 63.1(2) . . . 7_565 ? I2 B2 B6 B5 -148.51(17) . . . 7_565 ? B1 B2 B6 B5 -100.5(3) 7_565 . . . ? B1 B2 B6 B5 37.5(2) . . . . ? B3 B2 B6 B5 -63.1(2) 7_565 . . . ? B3 B2 B6 B5 0.1(3) . . . . ? I2 B2 B6 B5 148.51(17) . . . . ? B1 B2 B6 B1 138.0(4) . . . 7_565 ? B3 B2 B6 B1 37.4(2) 7_565 . . 7_565 ? B3 B2 B6 B1 100.6(3) . . . 7_565 ? I2 B2 B6 B1 -110.98(18) . . . 7_565 ? B1 B2 B6 B1 -138.0(4) 7_565 . . . ? B3 B2 B6 B1 -100.6(3) 7_565 . . . ? B3 B2 B6 B1 -37.4(2) . . . . ? I2 B2 B6 B1 110.98(18) . . . . ? B1 B2 B6 I6 110.98(18) 7_565 . . . ? B1 B2 B6 I6 -110.98(18) . . . . ? B3 B2 B6 I6 148.40(17) 7_565 . . . ? B3 B2 B6 I6 -148.40(17) . . . . ? I2 B2 B6 I6 0.0 . . . . ? B5 B5 B6 B2 100.7(2) 7_565 . . . ? B1 B5 B6 B2 -37.7(2) . . . . ? B8 B5 B6 B2 62.8(3) . . . . ? B4 B5 B6 B2 -0.2(3) . . . . ? I5 B5 B6 B2 -148.5(2) . . . . ? B1 B5 B6 B5 -138.4(2) . . . 7_565 ? B8 B5 B6 B5 -37.9(3) . . . 7_565 ? B4 B5 B6 B5 -100.9(2) . . . 7_565 ? I5 B5 B6 B5 110.81(19) . . . 7_565 ? B5 B5 B6 B1 37.10(16) 7_565 . . 7_565 ? B1 B5 B6 B1 -101.3(3) . . . 7_565 ? B8 B5 B6 B1 -0.8(3) . . . 7_565 ? B4 B5 B6 B1 -63.8(3) . . . 7_565 ? I5 B5 B6 B1 147.9(2) . . . 7_565 ? B5 B5 B6 B1 138.4(2) 7_565 . . . ? B8 B5 B6 B1 100.5(3) . . . . ? B4 B5 B6 B1 37.4(2) . . . . ? I5 B5 B6 B1 -110.8(3) . . . . ? B5 B5 B6 I6 -111.4(2) 7_565 . . . ? B1 B5 B6 I6 110.3(2) . . . . ? B8 B5 B6 I6 -149.2(2) . . . . ? B4 B5 B6 I6 147.7(2) . . . . ? I5 B5 B6 I6 -0.5(3) . . . . ? B4 B1 B6 B2 100.2(3) . . . . ? B5 B1 B6 B2 137.9(3) . . . . ? B3 B1 B6 B2 37.1(3) . . . . ? I1 B1 B6 B2 -110.7(3) . . . . ? B4 B1 B6 B5 -0.8(3) . . . 7_565 ? B5 B1 B6 B5 37.0(2) . . . 7_565 ? B2 B1 B6 B5 -101.0(3) . . . 7_565 ? B3 B1 B6 B5 -63.9(3) . . . 7_565 ? I1 B1 B6 B5 148.3(2) . . . 7_565 ? B4 B1 B6 B5 -37.8(2) . . . . ? B2 B1 B6 B5 -137.9(3) . . . . ? B3 B1 B6 B5 -100.9(3) . . . . ? I1 B1 B6 B5 111.4(3) . . . . ? B4 B1 B6 B1 62.5(4) . . . 7_565 ? B5 B1 B6 B1 100.3(3) . . . 7_565 ? B2 B1 B6 B1 -37.7(3) . . . 7_565 ? B3 B1 B6 B1 -0.6(4) . . . 7_565 ? I1 B1 B6 B1 -148.37(17) . . . 7_565 ? B4 B1 B6 I6 -149.6(3) . . . . ? B5 B1 B6 I6 -111.8(3) . . . . ? B2 B1 B6 I6 110.2(4) . . . . ? B3 B1 B6 I6 147.3(2) . . . . ? I1 B1 B6 I6 -0.5(4) . . . . ? B1 B4 B7 B8 101.0(3) . . . . ? B3 B4 B7 B8 138.5(3) . . . . ? B5 B4 B7 B8 37.4(3) . . . . ? I4 B4 B7 B8 -110.3(3) . . . . ? B1 B4 B7 B4 63.3(4) . . . 7_565 ? B3 B4 B7 B4 100.7(3) . . . 7_565 ? B8 B4 B7 B4 -37.8(3) . . . 7_565 ? B5 B4 B7 B4 -0.4(4) . . . 7_565 ? I4 B4 B7 B4 -148.08(17) . . . 7_565 ? B1 B4 B7 B3 -37.4(2) . . . . ? B8 B4 B7 B3 -138.5(3) . . . . ? B5 B4 B7 B3 -101.1(3) . . . . ? I4 B4 B7 B3 111.2(3) . . . . ? B1 B4 B7 B3 -0.2(3) . . . 7_565 ? B3 B4 B7 B3 37.3(2) . . . 7_565 ? B8 B4 B7 B3 -101.2(3) . . . 7_565 ? B5 B4 B7 B3 -63.8(3) . . . 7_565 ? I4 B4 B7 B3 148.5(2) . . . 7_565 ? B1 B4 B7 I7 -148.0(3) . . . . ? B3 B4 B7 I7 -110.6(3) . . . . ? B8 B4 B7 I7 110.9(3) . . . . ? B5 B4 B7 I7 148.3(2) . . . . ? I4 B4 B7 I7 0.6(4) . . . . ? B3 B3 B7 B8 101.0(2) 7_565 . . . ? B4 B3 B7 B8 -37.3(2) . . . . ? B2 B3 B7 B8 62.9(3) . . . . ? B1 B3 B7 B8 -0.3(3) . . . . ? I3 B3 B7 B8 -148.0(2) . . . . ? B3 B3 B7 B4 37.34(16) 7_565 . . 7_565 ? B4 B3 B7 B4 -100.9(3) . . . 7_565 ? B2 B3 B7 B4 -0.7(3) . . . 7_565 ? B1 B3 B7 B4 -64.0(3) . . . 7_565 ? I3 B3 B7 B4 148.4(2) . . . 7_565 ? B3 B3 B7 B4 138.2(2) 7_565 . . . ? B2 B3 B7 B4 100.1(3) . . . . ? B1 B3 B7 B4 36.9(2) . . . . ? I3 B3 B7 B4 -110.7(3) . . . . ? B4 B3 B7 B3 -138.2(2) . . . 7_565 ? B2 B3 B7 B3 -38.1(3) . . . 7_565 ? B1 B3 B7 B3 -101.3(2) . . . 7_565 ? I3 B3 B7 B3 111.06(18) . . . 7_565 ? B3 B3 B7 I7 -110.7(2) 7_565 . . . ? B4 B3 B7 I7 111.1(2) . . . . ? B2 B3 B7 I7 -148.7(2) . . . . ? B1 B3 B7 I7 148.0(2) . . . . ? I3 B3 B7 I7 0.4(3) . . . . ? B4 B7 B8 B4 137.8(3) 7_565 . . . ? B3 B7 B8 B4 37.2(2) . . . . ? B3 B7 B8 B4 100.6(3) 7_565 . . . ? I7 B7 B8 B4 -111.09(17) . . . . ? B4 B7 B8 B4 -137.8(3) . . . 7_565 ? B3 B7 B8 B4 -100.6(3) . . . 7_565 ? B3 B7 B8 B4 -37.2(2) 7_565 . . 7_565 ? I7 B7 B8 B4 111.09(17) . . . 7_565 ? B4 B7 B8 B5 37.4(2) 7_565 . . 7_565 ? B4 B7 B8 B5 -100.4(3) . . . 7_565 ? B3 B7 B8 B5 -63.2(2) . . . 7_565 ? B3 B7 B8 B5 0.2(3) 7_565 . . 7_565 ? I7 B7 B8 B5 148.52(17) . . . 7_565 ? B4 B7 B8 B5 100.4(3) 7_565 . . . ? B4 B7 B8 B5 -37.4(2) . . . . ? B3 B7 B8 B5 -0.2(3) . . . . ? B3 B7 B8 B5 63.2(2) 7_565 . . . ? I7 B7 B8 B5 -148.52(17) . . . . ? B4 B7 B8 I8 -111.09(17) 7_565 . . . ? B4 B7 B8 I8 111.09(17) . . . . ? B3 B7 B8 I8 148.29(16) . . . . ? B3 B7 B8 I8 -148.29(16) 7_565 . . . ? I7 B7 B8 I8 0.0 . . . . ? B1 B4 B8 B7 -101.2(3) . . . . ? B3 B4 B8 B7 -37.2(3) . . . . ? B5 B4 B8 B7 -138.3(3) . . . . ? I4 B4 B8 B7 110.3(3) . . . . ? B1 B4 B8 B4 -63.6(4) . . . 7_565 ? B7 B4 B8 B4 37.6(3) . . . 7_565 ? B3 B4 B8 B4 0.5(4) . . . 7_565 ? B5 B4 B8 B4 -100.6(3) . . . 7_565 ? I4 B4 B8 B4 147.90(17) . . . 7_565 ? B1 B4 B8 B5 -0.1(3) . . . 7_565 ? B7 B4 B8 B5 101.2(3) . . . 7_565 ? B3 B4 B8 B5 64.0(3) . . . 7_565 ? B5 B4 B8 B5 -37.1(2) . . . 7_565 ? I4 B4 B8 B5 -148.6(2) . . . 7_565 ? B1 B4 B8 B5 37.0(2) . . . . ? B7 B4 B8 B5 138.3(3) . . . . ? B3 B4 B8 B5 101.1(3) . . . . ? I4 B4 B8 B5 -111.5(3) . . . . ? B1 B4 B8 I8 144.8(3) . . . . ? B7 B4 B8 I8 -113.9(3) . . . . ? B3 B4 B8 I8 -151.1(2) . . . . ? B5 B4 B8 I8 107.8(3) . . . . ? I4 B4 B8 I8 -3.7(4) . . . . ? B5 B5 B8 B7 -100.8(2) 7_565 . . . ? B6 B5 B8 B7 -63.0(3) . . . . ? B1 B5 B8 B7 0.7(3) . . . . ? B4 B5 B8 B7 37.4(2) . . . . ? I5 B5 B8 B7 148.02(19) . . . . ? B5 B5 B8 B4 -138.2(2) 7_565 . . . ? B6 B5 B8 B4 -100.3(3) . . . . ? B1 B5 B8 B4 -36.7(2) . . . . ? I5 B5 B8 B4 110.7(3) . . . . ? B5 B5 B8 B4 -37.40(16) 7_565 . . 7_565 ? B6 B5 B8 B4 0.4(3) . . . 7_565 ? B1 B5 B8 B4 64.1(3) . . . 7_565 ? B4 B5 B8 B4 100.8(3) . . . 7_565 ? I5 B5 B8 B4 -148.6(2) . . . 7_565 ? B6 B5 B8 B5 37.8(3) . . . 7_565 ? B1 B5 B8 B5 101.5(2) . . . 7_565 ? B4 B5 B8 B5 138.2(2) . . . 7_565 ? I5 B5 B8 B5 -111.15(18) . . . 7_565 ? B5 B5 B8 I8 108.8(2) 7_565 . . . ? B6 B5 B8 I8 146.7(2) . . . . ? B1 B5 B8 I8 -149.7(2) . . . . ? B4 B5 B8 I8 -113.0(2) . . . . ? I5 B5 B8 I8 -2.3(3) . . . . ? O1 S1 O2 Na1 4.8(4) . . . . ? O3 S2 O4 Na1 15.7(5) . . . 6_657 ? O5 S3 O6 Na1 38.1(8) . . . 5_656 ? Na1 O7 S4 O7 15.1(9) . . . 7_565 ? Na1 O8 S5 O8 -16.2(9) 6_657 . . 7_565 ? S1 O2 Na1 O4 2.8(4) . . . 6_557 ? S1 O2 Na1 O6 68.5(3) . . . 5_656 ? S1 O2 Na1 O5 121.8(3) . . . 1_556 ? S1 O2 Na1 O8 -99.5(4) . . . 6_557 ? S1 O2 Na1 O7 -80.1(3) . . . . ? S1 O2 Na1 I2 -162.4(3) . . . 6_657 ? S4 O7 Na1 O4 115.7(7) . . . 6_557 ? S4 O7 Na1 O6 -172.2(6) . . . 5_656 ? S4 O7 Na1 O2 -127.3(7) . . . . ? S4 O7 Na1 O5 24.1(8) . . . 1_556 ? S4 O7 Na1 O8 40.8(7) . . . 6_557 ? S4 O7 Na1 I2 -28.4(7) . . . 6_657 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.022 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.106 #===END data_ck-mr-03 _database_code_depnum_ccdc_archive 'CCDC 778605' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B12 H12, 6(O2 S), 2(H2 O), 2(Na)' _chemical_formula_sum 'B12 H16 Na2 O14 S6' _chemical_formula_weight 608.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' Na Na 0.0362 0.0249 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4514(17) _cell_length_b 8.7899(18) _cell_length_c 8.8497(18) _cell_angle_alpha 94.73(3) _cell_angle_beta 94.40(3) _cell_angle_gamma 104.93(3) _cell_volume 629.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 306 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.883 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; March 2001 T Higashi ; _exptl_special_details ; March 2001 T Higashi ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector RX _diffrn_measurement_device_type 'Rigaku R-AXIS Spider' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 10.0000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21127 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0117 _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 -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2471 _reflns_number_gt 2268 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+0.2824P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2471 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.43347(18) 0.16550(17) 0.49444(17) 0.0180(3) Uani 1 1 d . . . H1 H 0.3920 0.2694 0.4913 0.022 Uiso 1 1 d R . . B2 B 0.53798(18) 0.12567(17) 0.66304(17) 0.0189(3) Uani 1 1 d . . . H2 H 0.5636 0.2037 0.7683 0.023 Uiso 1 1 d R . . B3 B 0.33605(18) 0.00668(17) 0.59587(17) 0.0186(3) Uani 1 1 d . . . H3 H 0.2298 0.0135 0.6582 0.022 Uiso 1 1 d R . . B4 B 0.31861(18) -0.01907(18) 0.39290(17) 0.0189(3) Uani 1 1 d . . . H4 H 0.2034 -0.0341 0.3232 0.023 Uiso 1 1 d R . . B5 B 0.51126(18) 0.08397(18) 0.33461(17) 0.0189(3) Uani 1 1 d . . . H5 H 0.5181 0.1405 0.2268 0.023 Uiso 1 1 d R . . B6 B 0.64672(18) 0.17382(17) 0.50100(17) 0.0189(3) Uani 1 1 d . . . H6 H 0.7404 0.2876 0.4992 0.023 Uiso 1 1 d R . . S1 S 0.06113(4) 0.23627(4) 0.44748(4) 0.02725(10) Uani 1 1 d . . . O1 O 0.06099(15) 0.27785(17) 0.29686(14) 0.0463(3) Uani 1 1 d . . . O2 O 0.09031(14) 0.36249(17) 0.56614(15) 0.0492(4) Uani 1 1 d . . . S2 S 0.28070(5) 0.01458(5) 0.96959(4) 0.02810(10) Uani 1 1 d . . . O3 O 0.18156(17) -0.14251(15) 0.96953(14) 0.0453(3) Uani 1 1 d . . . O4 O 0.20198(18) 0.13772(16) 0.98036(15) 0.0501(3) Uani 1 1 d . . . S3 S 0.56613(5) 0.47175(4) 0.24835(4) 0.02995(10) Uani 1 1 d . . . O5 O 0.39731(14) 0.44020(14) 0.19468(15) 0.0417(3) Uani 1 1 d . . . O6 O 0.68268(16) 0.49609(17) 0.13983(15) 0.0518(4) Uani 1 1 d . . . O7 O 0.07194(15) 0.60423(13) 0.15607(13) 0.0293(2) Uani 1 1 d . . . H13 H 0.032(3) 0.600(3) 0.233(3) 0.059(7) Uiso 1 1 d . . . H14 H 0.156(3) 0.674(3) 0.180(3) 0.066(7) Uiso 1 1 d . . . Na1 Na 0.11637(8) 0.36509(7) 0.04900(7) 0.03320(16) Uani 1 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 B1 0.0183(7) 0.0180(7) 0.0185(7) 0.0023(5) 0.0013(5) 0.0065(6) B2 0.0189(7) 0.0198(7) 0.0173(7) -0.0001(5) 0.0000(5) 0.0052(6) B3 0.0166(7) 0.0206(7) 0.0189(7) 0.0019(6) 0.0028(5) 0.0048(6) B4 0.0162(7) 0.0207(7) 0.0187(7) 0.0007(6) -0.0011(5) 0.0044(6) B5 0.0196(7) 0.0213(7) 0.0167(7) 0.0033(6) 0.0020(5) 0.0065(6) B6 0.0163(7) 0.0181(7) 0.0209(7) 0.0014(6) 0.0009(5) 0.0025(6) S1 0.02073(18) 0.0336(2) 0.02549(19) 0.00321(15) 0.00124(13) 0.00412(14) O1 0.0334(6) 0.0702(9) 0.0340(7) 0.0194(6) 0.0034(5) 0.0072(6) O2 0.0256(6) 0.0649(9) 0.0508(8) -0.0217(7) 0.0024(5) 0.0095(6) S2 0.02822(19) 0.0331(2) 0.02389(19) -0.00201(14) 0.00211(14) 0.01151(15) O3 0.0599(8) 0.0392(7) 0.0331(6) 0.0100(5) 0.0055(6) 0.0044(6) O4 0.0706(9) 0.0478(7) 0.0419(7) -0.0024(6) 0.0070(6) 0.0358(7) S3 0.0298(2) 0.0289(2) 0.0275(2) 0.00494(15) -0.00151(15) 0.00192(15) O5 0.0326(6) 0.0384(7) 0.0529(8) 0.0130(6) -0.0054(5) 0.0075(5) O6 0.0408(7) 0.0690(9) 0.0408(7) 0.0173(6) 0.0084(6) 0.0013(6) O7 0.0297(6) 0.0277(6) 0.0281(6) 0.0004(5) 0.0033(5) 0.0038(5) Na1 0.0428(4) 0.0365(3) 0.0277(3) 0.0042(3) 0.0023(3) 0.0239(3) _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 B1 B3 1.778(2) . ? B1 B5 1.779(2) . ? B1 B6 1.781(2) . ? B1 B2 1.781(2) . ? B1 B4 1.788(2) . ? B1 H1 1.0609 . ? B2 B5 1.784(2) 2_656 ? B2 B3 1.784(2) . ? B2 B6 1.784(2) . ? B2 B4 1.787(2) 2_656 ? B2 H2 1.0822 . ? B3 B5 1.780(2) 2_656 ? B3 B4 1.782(2) . ? B3 B6 1.785(2) 2_656 ? B3 H3 1.1009 . ? B4 B5 1.784(2) . ? B4 B6 1.786(2) 2_656 ? B4 B2 1.787(2) 2_656 ? B4 H4 1.0835 . ? B5 B3 1.780(2) 2_656 ? B5 B2 1.784(2) 2_656 ? B5 B6 1.785(2) . ? B5 H5 1.1104 . ? B6 B3 1.785(2) 2_656 ? B6 B4 1.786(2) 2_656 ? B6 H6 1.1063 . ? S1 O1 1.4109(13) . ? S1 O2 1.4218(13) . ? O1 Na1 2.4225(15) . ? S2 O4 1.4096(13) . ? S2 O3 1.4185(14) . ? O4 Na1 2.3450(14) 1_556 ? S3 O5 1.4172(13) . ? S3 O6 1.4173(14) . ? O5 Na1 2.5135(15) . ? O6 Na1 2.6210(17) 2_665 ? O7 Na1 2.3643(14) . ? O7 Na1 2.3995(15) 2_565 ? O7 H13 0.78(3) . ? O7 H14 0.81(3) . ? Na1 O4 2.3450(14) 1_554 ? Na1 O7 2.3995(15) 2_565 ? Na1 O6 2.6210(17) 2_665 ? 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 B3 B1 B5 107.87(10) . . ? B3 B1 B6 108.21(10) . . ? B5 B1 B6 60.18(9) . . ? B3 B1 B2 60.16(9) . . ? B5 B1 B2 108.18(10) . . ? B6 B1 B2 60.10(9) . . ? B3 B1 B4 59.96(8) . . ? B5 B1 B4 60.03(9) . . ? B6 B1 B4 108.43(10) . . ? B2 B1 B4 108.36(10) . . ? B3 B1 H1 121.8 . . ? B5 B1 H1 121.9 . . ? B6 B1 H1 121.3 . . ? B2 B1 H1 121.3 . . ? B4 B1 H1 121.7 . . ? B1 B2 B5 107.66(11) . 2_656 ? B1 B2 B3 59.83(9) . . ? B5 B2 B3 59.85(9) 2_656 . ? B1 B2 B6 59.95(8) . . ? B5 B2 B6 107.87(10) 2_656 . ? B3 B2 B6 107.82(10) . . ? B1 B2 B4 107.90(10) . 2_656 ? B5 B2 B4 59.96(8) 2_656 2_656 ? B3 B2 B4 107.86(10) . 2_656 ? B6 B2 B4 60.04(8) . 2_656 ? B1 B2 H2 123.3 . . ? B5 B2 H2 120.8 2_656 . ? B3 B2 H2 122.4 . . ? B6 B2 H2 122.1 . . ? B4 B2 H2 120.5 2_656 . ? B1 B3 B5 107.99(10) . 2_656 ? B1 B3 B4 60.30(9) . . ? B5 B3 B4 108.22(10) 2_656 . ? B1 B3 B2 60.01(8) . . ? B5 B3 B2 60.07(8) 2_656 . ? B4 B3 B2 108.51(11) . . ? B1 B3 B6 108.29(10) . 2_656 ? B5 B3 B6 60.09(9) 2_656 2_656 ? B4 B3 B6 60.11(8) . 2_656 ? B2 B3 B6 108.39(10) . 2_656 ? B1 B3 H3 120.6 . . ? B5 B3 H3 122.4 2_656 . ? B4 B3 H3 121.4 . . ? B2 B3 H3 120.9 . . ? B6 B3 H3 122.5 2_656 . ? B3 B4 B5 107.46(10) . . ? B3 B4 B6 60.04(8) . 2_656 ? B5 B4 B6 107.73(10) . 2_656 ? B3 B4 B2 107.76(10) . 2_656 ? B5 B4 B2 59.93(8) . 2_656 ? B6 B4 B2 59.89(8) 2_656 2_656 ? B3 B4 B1 59.74(9) . . ? B5 B4 B1 59.74(9) . . ? B6 B4 B1 107.79(10) 2_656 . ? B2 B4 B1 107.71(10) 2_656 . ? B3 B4 H4 122.8 . . ? B5 B4 H4 122.0 . . ? B6 B4 H4 120.8 2_656 . ? B2 B4 H4 120.3 2_656 . ? B1 B4 H4 123.5 . . ? B1 B5 B3 107.93(10) . 2_656 ? B1 B5 B2 108.23(10) . 2_656 ? B3 B5 B2 60.08(9) 2_656 2_656 ? B1 B5 B4 60.23(9) . . ? B3 B5 B4 108.16(10) 2_656 . ? B2 B5 B4 60.11(9) 2_656 . ? B1 B5 B6 59.96(8) . . ? B3 B5 B6 60.11(8) 2_656 . ? B2 B5 B6 108.41(10) 2_656 . ? B4 B5 B6 108.42(10) . . ? B1 B5 H5 120.9 . . ? B3 B5 H5 122.4 2_656 . ? B2 B5 H5 122.2 2_656 . ? B4 B5 H5 121.3 . . ? B6 B5 H5 121.2 . . ? B1 B6 B2 59.95(8) . . ? B1 B6 B5 59.85(9) . . ? B2 B6 B5 107.79(10) . . ? B1 B6 B3 107.60(10) . 2_656 ? B2 B6 B3 107.74(10) . 2_656 ? B5 B6 B3 59.80(8) . 2_656 ? B1 B6 B4 107.92(10) . 2_656 ? B2 B6 B4 60.06(8) . 2_656 ? B5 B6 B4 107.78(10) . 2_656 ? B3 B6 B4 59.85(8) 2_656 2_656 ? B1 B6 H6 121.0 . . ? B2 B6 H6 122.4 . . ? B5 B6 H6 120.7 . . ? B3 B6 H6 122.1 2_656 . ? B4 B6 H6 123.0 2_656 . ? O1 S1 O2 116.72(9) . . ? S1 O1 Na1 169.23(8) . . ? O4 S2 O3 117.50(9) . . ? S2 O4 Na1 166.42(9) . 1_556 ? O5 S3 O6 117.98(8) . . ? S3 O5 Na1 168.26(9) . . ? S3 O6 Na1 161.03(10) . 2_665 ? Na1 O7 Na1 96.98(5) . 2_565 ? Na1 O7 H13 115.5(17) . . ? Na1 O7 H13 111.6(18) 2_565 . ? Na1 O7 H14 113.4(17) . . ? Na1 O7 H14 118.7(18) 2_565 . ? H13 O7 H14 101(2) . . ? O4 Na1 O7 168.97(5) 1_554 . ? O4 Na1 O7 107.77(6) 1_554 2_565 ? O7 Na1 O7 83.02(5) . 2_565 ? O4 Na1 O1 90.58(6) 1_554 . ? O7 Na1 O1 84.00(6) . . ? O7 Na1 O1 129.35(5) 2_565 . ? O4 Na1 O5 80.24(6) 1_554 . ? O7 Na1 O5 89.18(5) . . ? O7 Na1 O5 151.03(5) 2_565 . ? O1 Na1 O5 77.02(5) . . ? O4 Na1 O6 86.18(6) 1_554 2_665 ? O7 Na1 O6 94.03(6) . 2_665 ? O7 Na1 O6 78.13(5) 2_565 2_665 ? O1 Na1 O6 151.61(5) . 2_665 ? O5 Na1 O6 74.63(5) . 2_665 ? 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 B3 B1 B2 B5 37.36(10) . . . 2_656 ? B5 B1 B2 B5 -63.24(14) . . . 2_656 ? B6 B1 B2 B5 -100.83(11) . . . 2_656 ? B4 B1 B2 B5 0.33(13) . . . 2_656 ? B5 B1 B2 B3 -100.60(11) . . . . ? B6 B1 B2 B3 -138.18(11) . . . . ? B4 B1 B2 B3 -37.02(10) . . . . ? B3 B1 B2 B6 138.18(11) . . . . ? B5 B1 B2 B6 37.58(10) . . . . ? B4 B1 B2 B6 101.16(11) . . . . ? B3 B1 B2 B4 100.66(11) . . . 2_656 ? B5 B1 B2 B4 0.06(13) . . . 2_656 ? B6 B1 B2 B4 -37.52(10) . . . 2_656 ? B4 B1 B2 B4 63.64(14) . . . 2_656 ? B5 B1 B3 B5 63.59(14) . . . 2_656 ? B6 B1 B3 B5 -0.06(13) . . . 2_656 ? B2 B1 B3 B5 -37.54(10) . . . 2_656 ? B4 B1 B3 B5 101.15(11) . . . 2_656 ? B5 B1 B3 B4 -37.56(10) . . . . ? B6 B1 B3 B4 -101.21(11) . . . . ? B2 B1 B3 B4 -138.69(11) . . . . ? B5 B1 B3 B2 101.13(11) . . . . ? B6 B1 B3 B2 37.48(10) . . . . ? B4 B1 B3 B2 138.69(11) . . . . ? B5 B1 B3 B6 0.00(13) . . . 2_656 ? B6 B1 B3 B6 -63.65(14) . . . 2_656 ? B2 B1 B3 B6 -101.13(11) . . . 2_656 ? B4 B1 B3 B6 37.56(10) . . . 2_656 ? B5 B2 B3 B1 -138.04(11) 2_656 . . . ? B6 B2 B3 B1 -37.32(10) . . . . ? B4 B2 B3 B1 -100.73(11) 2_656 . . . ? B1 B2 B3 B5 138.04(11) . . . 2_656 ? B6 B2 B3 B5 100.72(11) . . . 2_656 ? B4 B2 B3 B5 37.30(10) 2_656 . . 2_656 ? B1 B2 B3 B4 37.21(10) . . . . ? B5 B2 B3 B4 -100.83(11) 2_656 . . . ? B6 B2 B3 B4 -0.11(13) . . . . ? B4 B2 B3 B4 -63.52(14) 2_656 . . . ? B1 B2 B3 B6 100.95(11) . . . 2_656 ? B5 B2 B3 B6 -37.09(10) 2_656 . . 2_656 ? B6 B2 B3 B6 63.63(14) . . . 2_656 ? B4 B2 B3 B6 0.21(13) 2_656 . . 2_656 ? B1 B3 B4 B5 37.33(10) . . . . ? B5 B3 B4 B5 -63.41(14) 2_656 . . . ? B2 B3 B4 B5 0.25(13) . . . . ? B6 B3 B4 B5 -100.79(11) 2_656 . . . ? B1 B3 B4 B6 138.12(10) . . . 2_656 ? B5 B3 B4 B6 37.37(10) 2_656 . . 2_656 ? B2 B3 B4 B6 101.03(11) . . . 2_656 ? B1 B3 B4 B2 100.54(11) . . . 2_656 ? B5 B3 B4 B2 -0.21(13) 2_656 . . 2_656 ? B2 B3 B4 B2 63.46(14) . . . 2_656 ? B6 B3 B4 B2 -37.58(10) 2_656 . . 2_656 ? B5 B3 B4 B1 -100.75(11) 2_656 . . . ? B2 B3 B4 B1 -37.08(10) . . . . ? B6 B3 B4 B1 -138.12(10) 2_656 . . . ? B5 B1 B4 B3 137.95(10) . . . . ? B6 B1 B4 B3 100.82(11) . . . . ? B2 B1 B4 B3 37.11(10) . . . . ? B3 B1 B4 B5 -137.95(10) . . . . ? B6 B1 B4 B5 -37.14(10) . . . . ? B2 B1 B4 B5 -100.84(11) . . . . ? B3 B1 B4 B6 -37.41(10) . . . 2_656 ? B5 B1 B4 B6 100.55(11) . . . 2_656 ? B6 B1 B4 B6 63.41(14) . . . 2_656 ? B2 B1 B4 B6 -0.29(13) . . . 2_656 ? B3 B1 B4 B2 -100.63(11) . . . 2_656 ? B5 B1 B4 B2 37.33(10) . . . 2_656 ? B6 B1 B4 B2 0.19(13) . . . 2_656 ? B2 B1 B4 B2 -63.51(14) . . . 2_656 ? B3 B1 B5 B3 -63.56(13) . . . 2_656 ? B6 B1 B5 B3 37.61(10) . . . 2_656 ? B2 B1 B5 B3 0.06(13) . . . 2_656 ? B4 B1 B5 B3 -101.08(11) . . . 2_656 ? B3 B1 B5 B2 0.00(13) . . . 2_656 ? B6 B1 B5 B2 101.16(11) . . . 2_656 ? B2 B1 B5 B2 63.61(14) . . . 2_656 ? B4 B1 B5 B2 -37.53(10) . . . 2_656 ? B3 B1 B5 B4 37.53(10) . . . . ? B6 B1 B5 B4 138.69(11) . . . . ? B2 B1 B5 B4 101.15(11) . . . . ? B3 B1 B5 B6 -101.16(11) . . . . ? B2 B1 B5 B6 -37.55(10) . . . . ? B4 B1 B5 B6 -138.69(11) . . . . ? B3 B4 B5 B1 -37.33(10) . . . . ? B6 B4 B5 B1 -100.65(11) 2_656 . . . ? B2 B4 B5 B1 -138.13(10) 2_656 . . . ? B3 B4 B5 B3 63.37(14) . . . 2_656 ? B6 B4 B5 B3 0.05(13) 2_656 . . 2_656 ? B2 B4 B5 B3 -37.43(10) 2_656 . . 2_656 ? B1 B4 B5 B3 100.70(11) . . . 2_656 ? B3 B4 B5 B2 100.80(11) . . . 2_656 ? B6 B4 B5 B2 37.48(10) 2_656 . . 2_656 ? B1 B4 B5 B2 138.13(10) . . . 2_656 ? B3 B4 B5 B6 -0.30(13) . . . . ? B6 B4 B5 B6 -63.62(14) 2_656 . . . ? B2 B4 B5 B6 -101.10(11) 2_656 . . . ? B1 B4 B5 B6 37.04(10) . . . . ? B3 B1 B6 B2 -37.51(10) . . . . ? B5 B1 B6 B2 -138.10(10) . . . . ? B4 B1 B6 B2 -101.03(11) . . . . ? B3 B1 B6 B5 100.59(11) . . . . ? B2 B1 B6 B5 138.10(10) . . . . ? B4 B1 B6 B5 37.07(10) . . . . ? B3 B1 B6 B3 63.20(13) . . . 2_656 ? B5 B1 B6 B3 -37.39(10) . . . 2_656 ? B2 B1 B6 B3 100.71(11) . . . 2_656 ? B4 B1 B6 B3 -0.32(13) . . . 2_656 ? B3 B1 B6 B4 0.03(13) . . . 2_656 ? B5 B1 B6 B4 -100.56(11) . . . 2_656 ? B2 B1 B6 B4 37.53(10) . . . 2_656 ? B4 B1 B6 B4 -63.50(14) . . . 2_656 ? B5 B2 B6 B1 100.47(11) 2_656 . . . ? B3 B2 B6 B1 37.26(10) . . . . ? B4 B2 B6 B1 138.02(11) 2_656 . . . ? B1 B2 B6 B5 -37.34(10) . . . . ? B5 B2 B6 B5 63.13(14) 2_656 . . . ? B3 B2 B6 B5 -0.08(13) . . . . ? B4 B2 B6 B5 100.68(11) 2_656 . . . ? B1 B2 B6 B3 -100.47(11) . . . 2_656 ? B5 B2 B6 B3 0.01(13) 2_656 . . 2_656 ? B3 B2 B6 B3 -63.20(14) . . . 2_656 ? B4 B2 B6 B3 37.55(9) 2_656 . . 2_656 ? B1 B2 B6 B4 -138.02(11) . . . 2_656 ? B5 B2 B6 B4 -37.54(10) 2_656 . . 2_656 ? B3 B2 B6 B4 -100.76(11) . . . 2_656 ? B3 B5 B6 B1 -137.96(10) 2_656 . . . ? B2 B5 B6 B1 -100.87(11) 2_656 . . . ? B4 B5 B6 B1 -37.15(10) . . . . ? B1 B5 B6 B2 37.38(10) . . . . ? B3 B5 B6 B2 -100.57(11) 2_656 . . . ? B2 B5 B6 B2 -63.48(14) 2_656 . . . ? B4 B5 B6 B2 0.23(13) . . . . ? B1 B5 B6 B3 137.96(10) . . . 2_656 ? B2 B5 B6 B3 37.09(10) 2_656 . . 2_656 ? B4 B5 B6 B3 100.80(11) . . . 2_656 ? B1 B5 B6 B4 100.80(11) . . . 2_656 ? B3 B5 B6 B4 -37.15(10) 2_656 . . 2_656 ? B2 B5 B6 B4 -0.07(13) 2_656 . . 2_656 ? B4 B5 B6 B4 63.65(14) . . . 2_656 ? O2 S1 O1 Na1 76.0(5) . . . . ? O3 S2 O4 Na1 123.1(4) . . . 1_556 ? O6 S3 O5 Na1 23.7(4) . . . . ? O5 S3 O6 Na1 82.5(3) . . . 2_665 ? Na1 O7 Na1 O4 168.2(3) 2_565 . . 1_554 ? Na1 O7 Na1 O7 0.0 2_565 . . 2_565 ? Na1 O7 Na1 O1 -130.93(6) 2_565 . . . ? Na1 O7 Na1 O5 152.04(6) 2_565 . . . ? Na1 O7 Na1 O6 77.51(5) 2_565 . . 2_665 ? S1 O1 Na1 O4 75.9(5) . . . 1_554 ? S1 O1 Na1 O7 -94.5(5) . . . . ? S1 O1 Na1 O7 -170.3(5) . . . 2_565 ? S1 O1 Na1 O5 -3.9(5) . . . . ? S1 O1 Na1 O6 -7.1(6) . . . 2_665 ? S3 O5 Na1 O4 47.2(4) . . . 1_554 ? S3 O5 Na1 O7 -135.9(4) . . . . ? S3 O5 Na1 O7 -62.0(4) . . . 2_565 ? S3 O5 Na1 O1 140.0(4) . . . . ? S3 O5 Na1 O6 -41.5(4) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.255 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.043 #===END data_ck-mr-02 _database_code_depnum_ccdc_archive 'CCDC 778606' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B12 I12, 8(O2 S), O, 2(Na)' _chemical_formula_sum 'B12 I12 Na2 O17 S8' _chemical_formula_weight 2226.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.634(2) _cell_length_b 11.167(2) _cell_length_c 20.045(4) _cell_angle_alpha 81.33(3) _cell_angle_beta 86.29(3) _cell_angle_gamma 78.57(3) _cell_volume 2304.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1964 _exptl_absorpt_coefficient_mu 8.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4838 _exptl_absorpt_correction_T_max 0.7275 _exptl_absorpt_process_details ; March 2001 T Higashi ; _exptl_special_details ; March 2001 T Higashi ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector RX _diffrn_measurement_device_type 'Rigaku R-AXIS Spider' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 10.0000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57527 _diffrn_reflns_av_R_equivalents 0.1094 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 23.50 _reflns_number_total 6793 _reflns_number_gt 5160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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. O17 represents a water molecule. The hydrogen atoms could not be located from the difference map. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6793 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B -0.0674(11) 0.8723(12) 0.0094(6) 0.022(3) Uani 1 1 d . . . I1 I -0.14782(8) 0.70703(7) 0.01978(4) 0.0336(2) Uani 1 1 d . . . B2 B 0.0144(13) 1.0562(14) 0.0737(6) 0.032(3) Uani 1 1 d . . . I2 I 0.03459(8) 1.12576(7) 0.16512(4) 0.0318(2) Uani 1 1 d . . . B3 B 0.1527(12) 0.9785(13) 0.0278(7) 0.030(3) Uani 1 1 d . . . I3 I 0.34492(7) 0.95988(7) 0.06243(4) 0.0334(2) Uani 1 1 d . . . B4 B -0.1219(13) 0.9901(12) 0.0590(6) 0.026(3) Uani 1 1 d . . . I4 I -0.27579(8) 0.98301(8) 0.13467(4) 0.0372(2) Uani 1 1 d . . . B5 B 0.0355(13) 0.8954(12) 0.0693(6) 0.026(3) Uani 1 1 d . . . I5 I 0.08597(8) 0.76206(7) 0.15907(4) 0.0336(2) Uani 1 1 d . . . B6 B 0.1023(13) 0.8657(13) -0.0123(6) 0.027(3) Uani 1 1 d . . . I6 I 0.22209(8) 0.68993(7) -0.02609(4) 0.0341(2) Uani 1 1 d . . . B7 B 0.0689(13) 0.1233(12) 0.5080(7) 0.029(3) Uani 1 1 d . . . I7 I 0.15459(8) 0.27849(7) 0.51833(4) 0.0340(2) Uani 1 1 d . . . B8 B 0.0253(13) 0.0949(12) 0.4281(6) 0.028(3) Uani 1 1 d . . . I8 I 0.05693(8) 0.21701(7) 0.33684(4) 0.0325(2) Uani 1 1 d . . . B9 B 0.1559(12) -0.0054(12) 0.4701(6) 0.027(3) Uani 1 1 d . . . I9 I 0.35289(7) -0.01725(8) 0.43443(4) 0.0341(2) Uani 1 1 d . . . B10 B 0.1133(13) -0.0249(13) 0.5597(6) 0.028(3) Uani 1 1 d . . . I10 I 0.26017(8) -0.04968(8) 0.63300(4) 0.0365(2) Uani 1 1 d . . . B11 B -0.0416(13) 0.0664(12) 0.5713(6) 0.024(3) Uani 1 1 d . . . I11 I -0.09404(8) 0.14805(7) 0.66234(4) 0.0325(2) Uani 1 1 d . . . B12 B -0.0990(12) 0.1432(11) 0.4893(6) 0.025(3) Uani 1 1 d . . . I12 I -0.21928(8) 0.32314(7) 0.47668(4) 0.0352(2) Uani 1 1 d . . . Na1 Na 0.3716(5) 0.3620(5) 0.2217(3) 0.0582(15) Uani 1 1 d . . . Na2 Na 0.7946(6) 0.5644(7) 0.2790(4) 0.098(3) Uani 1 1 d . . . O1 O -0.0180(11) 0.5470(10) 0.3364(6) 0.084(4) Uani 1 1 d . . . S1 S 0.1068(5) 0.5319(4) 0.3590(2) 0.0614(11) Uani 1 1 d . . . O2 O 0.2085(10) 0.5060(9) 0.3099(6) 0.074(3) Uani 1 1 d . . . O3 O 0.6350(11) 0.5933(12) 0.3755(6) 0.087(4) Uani 1 1 d . . . S2 S 0.5093(5) 0.6609(4) 0.3790(2) 0.0693(12) Uani 1 1 d . . . O4 O 0.4339(11) 0.6749(11) 0.3235(5) 0.081(3) Uani 1 1 d . . . O5 O 0.7178(11) 0.3858(11) 0.2735(6) 0.083(4) Uani 1 1 d . . . S3 S 0.7169(4) 0.2900(5) 0.2359(2) 0.0664(12) Uani 1 1 d . . . O6 O 0.5981(9) 0.2791(10) 0.2145(5) 0.061(3) Uani 1 1 d . . . O7 O 0.4310(10) 0.5548(9) 0.1867(5) 0.060(3) Uani 1 1 d . . . S4 S 0.4935(5) 0.6565(4) 0.1731(2) 0.0643(12) Uani 1 1 d . . . O8 O 0.6231(11) 0.6383(11) 0.1880(5) 0.076(3) Uani 1 1 d . . . O9 O 0.4149(9) 0.3504(11) 0.0976(5) 0.068(3) Uani 1 1 d . . . S5 S 0.4518(3) 0.3070(4) 0.03512(18) 0.0481(9) Uani 1 1 d . . . O10 O 0.4369(8) 0.3957(9) -0.0241(5) 0.055(3) Uani 1 1 d . . . O11 O 0.1611(9) 0.4089(9) 0.1795(5) 0.059(3) Uani 1 1 d . . . S6 S 0.0449(4) 0.4521(3) 0.14490(17) 0.0493(9) Uani 1 1 d . . . O12 O -0.0686(9) 0.4758(9) 0.1840(5) 0.058(3) Uani 1 1 d . . . O13 O 0.3651(10) 0.1490(9) 0.2328(5) 0.060(3) Uani 1 1 d . . . S7 S 0.3611(4) 0.0224(4) 0.24403(17) 0.0500(9) Uani 1 1 d . . . O14 O 0.4765(11) -0.0651(11) 0.2469(5) 0.084(4) Uani 1 1 d . . . O15 O 0.4356(9) 0.3030(9) 0.3427(5) 0.063(3) Uani 1 1 d . . . S8 S 0.4529(4) 0.3015(4) 0.41387(19) 0.0503(9) Uani 1 1 d . . . O16 O 0.4320(9) 0.4142(9) 0.4382(5) 0.062(3) Uani 1 1 d . . . O17 O 0.7768(12) 0.7634(11) 0.2847(6) 0.088(4) Uani 1 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 B1 0.010(7) 0.025(8) 0.035(8) -0.012(6) -0.005(5) -0.003(6) I1 0.0352(5) 0.0334(5) 0.0355(4) -0.0030(4) -0.0047(4) -0.0148(4) B2 0.030(8) 0.048(10) 0.026(7) -0.024(7) 0.002(6) -0.018(7) I2 0.0378(5) 0.0361(5) 0.0240(4) -0.0095(3) -0.0034(3) -0.0084(4) B3 0.017(7) 0.043(9) 0.033(8) 0.000(6) -0.003(6) -0.016(7) I3 0.0264(5) 0.0396(5) 0.0357(4) -0.0071(4) -0.0065(3) -0.0071(4) B4 0.026(8) 0.023(8) 0.030(7) -0.005(6) 0.002(6) -0.009(6) I4 0.0326(5) 0.0476(5) 0.0335(4) -0.0094(4) 0.0092(4) -0.0134(4) B5 0.043(9) 0.025(8) 0.018(6) -0.003(5) 0.005(6) -0.024(7) I5 0.0433(5) 0.0321(5) 0.0260(4) -0.0007(3) -0.0065(3) -0.0095(4) B6 0.026(8) 0.041(9) 0.019(7) -0.012(6) 0.006(5) -0.014(7) I6 0.0306(5) 0.0326(5) 0.0392(5) -0.0106(4) -0.0010(4) -0.0022(4) B7 0.031(8) 0.022(8) 0.032(8) 0.008(6) -0.002(6) -0.009(7) I7 0.0395(5) 0.0364(5) 0.0313(4) -0.0087(4) 0.0006(4) -0.0170(4) B8 0.037(8) 0.027(8) 0.020(7) -0.007(6) -0.005(6) -0.006(7) I8 0.0424(5) 0.0339(5) 0.0228(4) -0.0016(3) -0.0003(3) -0.0128(4) B9 0.021(8) 0.033(8) 0.025(7) 0.001(6) -0.004(6) -0.006(6) I9 0.0286(5) 0.0418(5) 0.0336(4) -0.0072(4) 0.0026(3) -0.0104(4) B10 0.030(8) 0.032(8) 0.022(7) 0.000(6) -0.009(6) -0.002(7) I10 0.0355(5) 0.0456(5) 0.0299(4) -0.0042(4) -0.0106(4) -0.0091(4) B11 0.032(8) 0.022(7) 0.017(6) -0.010(5) 0.001(6) 0.001(6) I11 0.0410(5) 0.0359(5) 0.0236(4) -0.0087(3) 0.0026(3) -0.0122(4) B12 0.025(8) 0.014(7) 0.033(7) 0.002(6) 0.004(6) 0.001(6) I12 0.0355(5) 0.0324(5) 0.0359(5) -0.0044(4) -0.0029(4) -0.0023(4) Na1 0.056(4) 0.062(4) 0.059(4) -0.005(3) -0.008(3) -0.018(3) Na2 0.055(5) 0.112(6) 0.146(7) -0.071(5) 0.005(4) -0.025(4) O1 0.076(9) 0.057(8) 0.133(11) -0.051(7) 0.013(7) -0.024(7) S1 0.088(3) 0.042(2) 0.057(2) -0.0091(19) -0.005(2) -0.016(2) O2 0.064(8) 0.055(7) 0.103(9) -0.020(6) 0.014(7) -0.013(6) O3 0.051(8) 0.130(11) 0.079(8) -0.019(7) 0.006(6) -0.017(8) S2 0.072(3) 0.061(3) 0.074(3) -0.024(2) 0.004(2) -0.001(2) O4 0.064(8) 0.109(10) 0.063(7) -0.018(7) -0.009(6) 0.006(7) O5 0.078(9) 0.078(9) 0.092(9) 0.015(7) -0.032(7) -0.027(7) S3 0.043(3) 0.085(3) 0.058(3) 0.006(2) 0.006(2) 0.003(2) O6 0.040(6) 0.083(8) 0.058(6) -0.008(5) -0.012(5) -0.004(6) O7 0.070(7) 0.051(6) 0.062(6) -0.002(5) -0.007(5) -0.025(6) S4 0.081(3) 0.045(3) 0.063(3) 0.0051(19) -0.016(2) -0.009(2) O8 0.062(8) 0.098(9) 0.077(8) -0.025(6) 0.007(6) -0.033(7) O9 0.053(7) 0.114(9) 0.047(6) -0.029(6) -0.001(5) -0.026(7) S5 0.038(2) 0.057(2) 0.052(2) -0.0084(19) -0.0034(17) -0.0133(19) O10 0.033(6) 0.068(7) 0.070(7) -0.009(5) -0.010(5) -0.022(5) O11 0.033(6) 0.059(7) 0.089(8) -0.014(6) -0.004(5) -0.017(5) S6 0.055(3) 0.051(2) 0.040(2) -0.0045(17) 0.0024(18) -0.008(2) O12 0.046(6) 0.049(6) 0.079(7) -0.014(5) 0.006(5) -0.010(5) O13 0.073(7) 0.058(7) 0.054(6) -0.002(5) 0.001(5) -0.033(6) S7 0.045(2) 0.061(3) 0.042(2) 0.0019(18) 0.0038(16) -0.012(2) O14 0.072(8) 0.091(9) 0.062(7) 0.011(6) 0.014(6) 0.024(7) O15 0.054(7) 0.064(7) 0.059(7) -0.008(5) 0.016(5) 0.015(5) S8 0.043(2) 0.049(2) 0.056(2) -0.0046(18) 0.0056(17) -0.0081(19) O16 0.050(7) 0.055(7) 0.083(8) -0.018(6) -0.005(5) -0.008(5) O17 0.103(10) 0.084(9) 0.078(8) 0.003(7) -0.002(7) -0.035(8) _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 B1 B4 1.753(18) . ? B1 B5 1.755(17) . ? B1 B3 1.808(19) 2_575 ? B1 B6 1.819(17) . ? B1 B2 1.841(18) 2_575 ? B1 I1 2.160(12) . ? B2 B5 1.779(19) . ? B2 B6 1.806(19) 2_575 ? B2 B4 1.810(17) . ? B2 B3 1.82(2) . ? B2 B1 1.841(18) 2_575 ? B2 I2 2.133(12) . ? B3 B4 1.763(18) 2_575 ? B3 B6 1.775(18) . ? B3 B5 1.788(16) . ? B3 B1 1.808(19) 2_575 ? B3 I3 2.161(12) . ? B4 B3 1.763(18) 2_575 ? B4 B6 1.779(18) 2_575 ? B4 B5 1.80(2) . ? B4 I4 2.163(13) . ? B5 B6 1.793(17) . ? B5 I5 2.178(13) . ? B6 B4 1.779(18) 2_575 ? B6 B2 1.806(19) 2_575 ? B6 I6 2.163(14) . ? B7 B8 1.785(18) . ? B7 B9 1.79(2) . ? B7 B11 1.804(17) . ? B7 B10 1.809(18) . ? B7 B12 1.811(18) . ? B7 I7 2.154(13) . ? B8 B11 1.772(18) 2_556 ? B8 B9 1.773(19) . ? B8 B10 1.787(18) 2_556 ? B8 B12 1.803(18) . ? B8 I8 2.161(12) . ? B9 B11 1.805(17) 2_556 ? B9 B10 1.815(17) . ? B9 B12 1.824(17) 2_556 ? B9 I9 2.155(13) . ? B10 B11 1.778(19) . ? B10 B8 1.787(18) 2_556 ? B10 B12 1.796(18) 2_556 ? B10 I10 2.162(12) . ? B11 B8 1.772(18) 2_556 ? B11 B9 1.805(17) 2_556 ? B11 B12 1.819(17) . ? B11 I11 2.155(12) . ? B12 B10 1.796(18) 2_556 ? B12 B9 1.824(17) 2_556 ? B12 I12 2.146(13) . ? Na1 O7 2.356(10) . ? Na1 O13 2.369(11) . ? Na1 O11 2.375(11) . ? Na1 O6 2.407(11) . ? Na1 O15 2.518(11) . ? Na1 O9 2.519(11) . ? Na1 O2 2.841(13) . ? Na2 O17 2.212(14) . ? Na2 O5 2.319(13) . ? Na2 O1 2.326(14) 1_655 ? Na2 O3 2.504(13) . ? Na2 O12 2.522(12) 1_655 ? Na2 O8 2.591(14) . ? O1 S1 1.399(12) . ? O1 Na2 2.326(14) 1_455 ? S1 O2 1.431(11) . ? O3 S2 1.401(12) . ? S2 O4 1.386(11) . ? O5 S3 1.400(13) . ? S3 O6 1.394(9) . ? O7 S4 1.410(9) . ? S4 O8 1.398(11) . ? O9 S5 1.414(10) . ? S5 O10 1.421(10) . ? O11 S6 1.419(10) . ? S6 O12 1.398(10) . ? O12 Na2 2.522(12) 1_455 ? O13 S7 1.407(10) . ? S7 O14 1.407(11) . ? O15 S8 1.447(10) . ? S8 O16 1.390(10) . ? 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 B4 B1 B5 61.7(8) . . ? B4 B1 B3 59.3(7) . 2_575 ? B5 B1 B3 108.3(9) . 2_575 ? B4 B1 B6 109.4(8) . . ? B5 B1 B6 60.2(7) . . ? B3 B1 B6 107.5(8) 2_575 . ? B4 B1 B2 107.9(9) . 2_575 ? B5 B1 B2 107.5(8) . 2_575 ? B3 B1 B2 59.9(7) 2_575 2_575 ? B6 B1 B2 59.2(7) . 2_575 ? B4 B1 I1 122.5(8) . . ? B5 B1 I1 121.5(8) . . ? B3 B1 I1 122.8(7) 2_575 . ? B6 B1 I1 120.2(8) . . ? B2 B1 I1 121.1(7) 2_575 . ? B5 B2 B6 107.1(8) . 2_575 ? B5 B2 B4 60.2(7) . . ? B6 B2 B4 58.9(7) 2_575 . ? B5 B2 B3 59.5(7) . . ? B6 B2 B3 107.4(9) 2_575 . ? B4 B2 B3 107.4(8) . . ? B5 B2 B1 106.2(8) . 2_575 ? B6 B2 B1 59.8(7) 2_575 2_575 ? B4 B2 B1 106.2(8) . 2_575 ? B3 B2 B1 59.2(7) . 2_575 ? B5 B2 I2 122.3(8) . . ? B6 B2 I2 122.4(9) 2_575 . ? B4 B2 I2 122.8(8) . . ? B3 B2 I2 121.6(8) . . ? B1 B2 I2 122.7(7) 2_575 . ? B4 B3 B6 60.4(7) 2_575 . ? B4 B3 B5 108.1(8) 2_575 . ? B6 B3 B5 60.4(7) . . ? B4 B3 B1 58.8(7) 2_575 2_575 ? B6 B3 B1 107.2(9) . 2_575 ? B5 B3 B1 107.2(9) . 2_575 ? B4 B3 B2 108.3(9) 2_575 . ? B6 B3 B2 108.1(8) . . ? B5 B3 B2 59.0(7) . . ? B1 B3 B2 60.9(8) 2_575 . ? B4 B3 I3 120.8(8) 2_575 . ? B6 B3 I3 123.5(9) . . ? B5 B3 I3 124.2(8) . . ? B1 B3 I3 119.9(7) 2_575 . ? B2 B3 I3 120.8(8) . . ? B1 B4 B3 61.9(8) . 2_575 ? B1 B4 B6 109.5(9) . 2_575 ? B3 B4 B6 60.1(7) 2_575 2_575 ? B1 B4 B5 59.2(7) . . ? B3 B4 B5 108.3(9) 2_575 . ? B6 B4 B5 107.4(8) 2_575 . ? B1 B4 B2 107.8(9) . . ? B3 B4 B2 108.7(8) 2_575 . ? B6 B4 B2 60.4(7) 2_575 . ? B5 B4 B2 59.1(7) . . ? B1 B4 I4 122.9(7) . . ? B3 B4 I4 121.4(8) 2_575 . ? B6 B4 I4 119.9(8) 2_575 . ? B5 B4 I4 123.1(7) . . ? B2 B4 I4 120.2(7) . . ? B1 B5 B2 109.0(10) . . ? B1 B5 B3 109.4(8) . . ? B2 B5 B3 61.4(7) . . ? B1 B5 B6 61.7(7) . . ? B2 B5 B6 109.2(8) . . ? B3 B5 B6 59.4(7) . . ? B1 B5 B4 59.1(7) . . ? B2 B5 B4 60.8(7) . . ? B3 B5 B4 109.4(9) . . ? B6 B5 B4 108.6(9) . . ? B1 B5 I5 122.2(7) . . ? B2 B5 I5 119.9(7) . . ? B3 B5 I5 119.6(8) . . ? B6 B5 I5 121.0(9) . . ? B4 B5 I5 122.5(7) . . ? B3 B6 B4 59.5(7) . 2_575 ? B3 B6 B5 60.2(7) . . ? B4 B6 B5 107.2(9) 2_575 . ? B3 B6 B2 108.4(10) . 2_575 ? B4 B6 B2 60.6(7) 2_575 2_575 ? B5 B6 B2 107.4(10) . 2_575 ? B3 B6 B1 107.2(9) . . ? B4 B6 B1 108.5(10) 2_575 . ? B5 B6 B1 58.2(7) . . ? B2 B6 B1 61.0(7) 2_575 . ? B3 B6 I6 123.8(8) . . ? B4 B6 I6 124.5(8) 2_575 . ? B5 B6 I6 121.0(8) . . ? B2 B6 I6 120.8(8) 2_575 . ? B1 B6 I6 119.0(7) . . ? B8 B7 B9 59.4(8) . . ? B8 B7 B11 107.7(9) . . ? B9 B7 B11 107.8(8) . . ? B8 B7 B10 107.4(9) . . ? B9 B7 B10 60.6(7) . . ? B11 B7 B10 59.0(7) . . ? B8 B7 B12 60.2(7) . . ? B9 B7 B12 108.3(9) . . ? B11 B7 B12 60.4(7) . . ? B10 B7 B12 107.7(8) . . ? B8 B7 I7 122.2(7) . . ? B9 B7 I7 121.6(8) . . ? B11 B7 I7 122.0(8) . . ? B10 B7 I7 122.1(8) . . ? B12 B7 I7 121.3(8) . . ? B11 B8 B9 61.2(7) 2_556 . ? B11 B8 B7 109.2(9) 2_556 . ? B9 B8 B7 60.4(7) . . ? B11 B8 B10 59.9(7) 2_556 2_556 ? B9 B8 B10 109.4(9) . 2_556 ? B7 B8 B10 108.8(9) . 2_556 ? B11 B8 B12 108.5(9) 2_556 . ? B9 B8 B12 109.5(9) . . ? B7 B8 B12 60.6(7) . . ? B10 B8 B12 60.0(7) 2_556 . ? B11 B8 I8 121.8(7) 2_556 . ? B9 B8 I8 120.8(8) . . ? B7 B8 I8 120.7(7) . . ? B10 B8 I8 121.4(8) 2_556 . ? B12 B8 I8 120.6(8) . . ? B8 B9 B7 60.1(7) . . ? B8 B9 B11 59.4(7) . 2_556 ? B7 B9 B11 107.5(9) . 2_556 ? B8 B9 B10 107.6(9) . . ? B7 B9 B10 60.2(7) . . ? B11 B9 B10 106.9(8) 2_556 . ? B8 B9 B12 107.8(9) . 2_556 ? B7 B9 B12 107.9(9) . 2_556 ? B11 B9 B12 60.2(7) 2_556 2_556 ? B10 B9 B12 59.1(7) . 2_556 ? B8 B9 I9 123.5(8) . . ? B7 B9 I9 122.6(8) . . ? B11 B9 I9 122.3(8) 2_556 . ? B10 B9 I9 121.3(8) . . ? B12 B9 I9 120.2(8) 2_556 . ? B11 B10 B8 59.6(7) . 2_556 ? B11 B10 B12 108.6(9) . 2_556 ? B8 B10 B12 60.4(7) 2_556 2_556 ? B11 B10 B7 60.4(7) . . ? B8 B10 B7 107.8(9) 2_556 . ? B12 B10 B7 108.3(9) 2_556 . ? B11 B10 B9 107.8(9) . . ? B8 B10 B9 108.2(8) 2_556 . ? B12 B10 B9 60.7(7) 2_556 . ? B7 B10 B9 59.2(7) . . ? B11 B10 I10 121.8(8) . . ? B8 B10 I10 124.4(8) 2_556 . ? B12 B10 I10 122.4(8) 2_556 . ? B7 B10 I10 119.4(8) . . ? B9 B10 I10 120.0(8) . . ? B8 B11 B10 60.4(7) 2_556 . ? B8 B11 B7 108.6(9) 2_556 . ? B10 B11 B7 60.7(7) . . ? B8 B11 B9 59.4(7) 2_556 2_556 ? B10 B11 B9 108.4(9) . 2_556 ? B7 B11 B9 108.5(8) . 2_556 ? B8 B11 B12 108.0(8) 2_556 . ? B10 B11 B12 108.8(8) . . ? B7 B11 B12 60.0(7) . . ? B9 B11 B12 60.4(7) 2_556 . ? B8 B11 I11 120.8(7) 2_556 . ? B10 B11 I11 120.9(8) . . ? B7 B11 I11 122.1(8) . . ? B9 B11 I11 121.2(8) 2_556 . ? B12 B11 I11 122.1(8) . . ? B10 B12 B8 59.5(7) 2_556 . ? B10 B12 B7 107.2(9) 2_556 . ? B8 B12 B7 59.2(7) . . ? B10 B12 B11 107.1(8) 2_556 . ? B8 B12 B11 106.3(9) . . ? B7 B12 B11 59.6(7) . . ? B10 B12 B9 60.2(7) 2_556 2_556 ? B8 B12 B9 107.1(9) . 2_556 ? B7 B12 B9 107.3(9) . 2_556 ? B11 B12 B9 59.4(7) . 2_556 ? B10 B12 I12 123.1(8) 2_556 . ? B8 B12 I12 122.4(8) . . ? B7 B12 I12 120.9(7) . . ? B11 B12 I12 122.1(8) . . ? B9 B12 I12 122.9(8) 2_556 . ? O7 Na1 O13 162.1(4) . . ? O7 Na1 O11 98.7(4) . . ? O13 Na1 O11 89.4(4) . . ? O7 Na1 O6 85.2(4) . . ? O13 Na1 O6 80.6(4) . . ? O11 Na1 O6 153.1(4) . . ? O7 Na1 O15 105.2(4) . . ? O13 Na1 O15 81.7(4) . . ? O11 Na1 O15 127.9(4) . . ? O6 Na1 O15 75.6(3) . . ? O7 Na1 O9 80.1(4) . . ? O13 Na1 O9 86.1(4) . . ? O11 Na1 O9 77.8(4) . . ? O6 Na1 O9 76.7(4) . . ? O15 Na1 O9 151.1(4) . . ? O7 Na1 O2 80.2(4) . . ? O13 Na1 O2 117.7(4) . . ? O11 Na1 O2 71.8(4) . . ? O6 Na1 O2 134.9(4) . . ? O15 Na1 O2 67.7(4) . . ? O9 Na1 O2 140.5(4) . . ? O17 Na2 O5 155.0(6) . . ? O17 Na2 O1 83.4(4) . 1_655 ? O5 Na2 O1 118.1(5) . 1_655 ? O17 Na2 O3 78.3(5) . . ? O5 Na2 O3 85.3(5) . . ? O1 Na2 O3 98.9(5) 1_655 . ? O17 Na2 O12 118.2(5) . 1_655 ? O5 Na2 O12 77.6(4) . 1_655 ? O1 Na2 O12 88.1(4) 1_655 1_655 ? O3 Na2 O12 162.9(5) . 1_655 ? O17 Na2 O8 84.5(5) . . ? O5 Na2 O8 77.8(4) . . ? O1 Na2 O8 160.2(5) 1_655 . ? O3 Na2 O8 93.9(4) . . ? O12 Na2 O8 84.0(4) 1_655 . ? S1 O1 Na2 168.9(8) . 1_455 ? O1 S1 O2 116.0(7) . . ? S1 O2 Na1 156.2(6) . . ? S2 O3 Na2 132.2(7) . . ? O4 S2 O3 118.2(7) . . ? S3 O5 Na2 145.7(8) . . ? O6 S3 O5 116.7(7) . . ? S3 O6 Na1 143.3(7) . . ? S4 O7 Na1 166.6(7) . . ? O8 S4 O7 118.3(7) . . ? S4 O8 Na2 146.9(7) . . ? S5 O9 Na1 163.2(8) . . ? O9 S5 O10 117.2(7) . . ? S6 O11 Na1 169.4(6) . . ? O12 S6 O11 117.5(6) . . ? S6 O12 Na2 153.9(6) . 1_455 ? S7 O13 Na1 176.3(6) . . ? O13 S7 O14 119.7(7) . . ? S8 O15 Na1 164.7(6) . . ? O16 S8 O15 117.7(6) . . ? 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 B5 B2 B3 B4 100.6(9) . . . 2_575 ? B6 B2 B3 B4 0.7(11) 2_575 . . 2_575 ? B4 B2 B3 B4 62.7(12) . . . 2_575 ? B1 B2 B3 B4 -36.1(8) 2_575 . . 2_575 ? I2 B2 B3 B4 -147.9(8) . . . 2_575 ? B5 B2 B3 B6 36.7(9) . . . . ? B6 B2 B3 B6 -63.2(12) 2_575 . . . ? B4 B2 B3 B6 -1.2(12) . . . . ? B1 B2 B3 B6 -100.0(9) 2_575 . . . ? I2 B2 B3 B6 148.2(8) . . . . ? B6 B2 B3 B5 -99.9(9) 2_575 . . . ? B4 B2 B3 B5 -37.9(8) . . . . ? B1 B2 B3 B5 -136.7(9) 2_575 . . . ? I2 B2 B3 B5 111.5(10) . . . . ? B5 B2 B3 B1 136.7(9) . . . 2_575 ? B6 B2 B3 B1 36.8(8) 2_575 . . 2_575 ? B4 B2 B3 B1 98.8(9) . . . 2_575 ? I2 B2 B3 B1 -111.8(10) . . . 2_575 ? B5 B2 B3 I3 -113.9(10) . . . . ? B6 B2 B3 I3 146.2(8) 2_575 . . . ? B4 B2 B3 I3 -151.7(8) . . . . ? B1 B2 B3 I3 109.4(9) 2_575 . . . ? I2 B2 B3 I3 -2.4(14) . . . . ? B5 B1 B4 B3 137.2(8) . . . 2_575 ? B6 B1 B4 B3 99.3(9) . . . 2_575 ? B2 B1 B4 B3 36.5(8) 2_575 . . 2_575 ? I1 B1 B4 B3 -111.6(9) . . . 2_575 ? B5 B1 B4 B6 99.1(9) . . . 2_575 ? B3 B1 B4 B6 -38.1(8) 2_575 . . 2_575 ? B6 B1 B4 B6 61.2(12) . . . 2_575 ? B2 B1 B4 B6 -1.6(12) 2_575 . . 2_575 ? I1 B1 B4 B6 -149.7(8) . . . 2_575 ? B3 B1 B4 B5 -137.2(8) 2_575 . . . ? B6 B1 B4 B5 -37.9(8) . . . . ? B2 B1 B4 B5 -100.7(9) 2_575 . . . ? I1 B1 B4 B5 111.2(9) . . . . ? B5 B1 B4 B2 35.0(8) . . . . ? B3 B1 B4 B2 -102.2(9) 2_575 . . . ? B6 B1 B4 B2 -2.9(12) . . . . ? B2 B1 B4 B2 -65.7(12) 2_575 . . . ? I1 B1 B4 B2 146.2(8) . . . . ? B5 B1 B4 I4 -111.8(9) . . . . ? B3 B1 B4 I4 111.0(10) 2_575 . . . ? B6 B1 B4 I4 -149.7(8) . . . . ? B2 B1 B4 I4 147.5(8) 2_575 . . . ? I1 B1 B4 I4 -0.6(14) . . . . ? B5 B2 B4 B1 -35.0(8) . . . . ? B6 B2 B4 B1 102.7(10) 2_575 . . . ? B3 B2 B4 B1 2.5(12) . . . . ? B1 B2 B4 B1 64.6(12) 2_575 . . . ? I2 B2 B4 B1 -146.4(9) . . . . ? B5 B2 B4 B3 -100.6(10) . . . 2_575 ? B6 B2 B4 B3 37.2(9) 2_575 . . 2_575 ? B3 B2 B4 B3 -63.0(13) . . . 2_575 ? B1 B2 B4 B3 -1.0(13) 2_575 . . 2_575 ? I2 B2 B4 B3 148.0(9) . . . 2_575 ? B5 B2 B4 B6 -137.8(9) . . . 2_575 ? B3 B2 B4 B6 -100.2(10) . . . 2_575 ? B1 B2 B4 B6 -38.1(9) 2_575 . . 2_575 ? I2 B2 B4 B6 110.9(11) . . . 2_575 ? B6 B2 B4 B5 137.8(9) 2_575 . . . ? B3 B2 B4 B5 37.6(8) . . . . ? B1 B2 B4 B5 99.6(9) 2_575 . . . ? I2 B2 B4 B5 -111.4(11) . . . . ? B5 B2 B4 I4 112.8(9) . . . . ? B6 B2 B4 I4 -109.4(10) 2_575 . . . ? B3 B2 B4 I4 150.4(8) . . . . ? B1 B2 B4 I4 -147.5(8) 2_575 . . . ? I2 B2 B4 I4 1.5(14) . . . . ? B4 B1 B5 B2 -36.0(8) . . . . ? B3 B1 B5 B2 2.0(11) 2_575 . . . ? B6 B1 B5 B2 102.1(9) . . . . ? B2 B1 B5 B2 65.3(12) 2_575 . . . ? I1 B1 B5 B2 -148.7(8) . . . . ? B4 B1 B5 B3 -101.5(10) . . . . ? B3 B1 B5 B3 -63.5(13) 2_575 . . . ? B6 B1 B5 B3 36.6(9) . . . . ? B2 B1 B5 B3 -0.2(13) 2_575 . . . ? I1 B1 B5 B3 145.8(9) . . . . ? B4 B1 B5 B6 -138.1(9) . . . . ? B3 B1 B5 B6 -100.1(9) 2_575 . . . ? B2 B1 B5 B6 -36.8(9) 2_575 . . . ? I1 B1 B5 B6 109.2(10) . . . . ? B3 B1 B5 B4 38.0(8) 2_575 . . . ? B6 B1 B5 B4 138.1(9) . . . . ? B2 B1 B5 B4 101.3(10) 2_575 . . . ? I1 B1 B5 B4 -112.7(9) . . . . ? B4 B1 B5 I5 111.3(10) . . . . ? B3 B1 B5 I5 149.3(8) 2_575 . . . ? B6 B1 B5 I5 -110.6(11) . . . . ? B2 B1 B5 I5 -147.4(9) 2_575 . . . ? I1 B1 B5 I5 -1.4(13) . . . . ? B6 B2 B5 B1 -1.7(11) 2_575 . . . ? B4 B2 B5 B1 35.3(8) . . . . ? B3 B2 B5 B1 -102.3(9) . . . . ? B1 B2 B5 B1 -64.4(11) 2_575 . . . ? I2 B2 B5 B1 147.4(8) . . . . ? B6 B2 B5 B3 100.5(9) 2_575 . . . ? B4 B2 B5 B3 137.6(9) . . . . ? B1 B2 B5 B3 37.8(8) 2_575 . . . ? I2 B2 B5 B3 -110.4(10) . . . . ? B6 B2 B5 B6 64.0(12) 2_575 . . . ? B4 B2 B5 B6 101.0(10) . . . . ? B3 B2 B5 B6 -36.5(9) . . . . ? B1 B2 B5 B6 1.3(12) 2_575 . . . ? I2 B2 B5 B6 -146.9(8) . . . . ? B6 B2 B5 B4 -37.0(8) 2_575 . . . ? B3 B2 B5 B4 -137.6(9) . . . . ? B1 B2 B5 B4 -99.7(9) 2_575 . . . ? I2 B2 B5 B4 112.1(10) . . . . ? B6 B2 B5 I5 -149.9(8) 2_575 . . . ? B4 B2 B5 I5 -112.9(9) . . . . ? B3 B2 B5 I5 109.6(10) . . . . ? B1 B2 B5 I5 147.4(8) 2_575 . . . ? I2 B2 B5 I5 -0.8(13) . . . . ? B4 B3 B5 B1 0.8(13) 2_575 . . . ? B6 B3 B5 B1 -37.6(9) . . . . ? B1 B3 B5 B1 62.8(12) 2_575 . . . ? B2 B3 B5 B1 101.7(11) . . . . ? I3 B3 B5 B1 -150.0(9) . . . . ? B4 B3 B5 B2 -100.9(10) 2_575 . . . ? B6 B3 B5 B2 -139.2(10) . . . . ? B1 B3 B5 B2 -38.9(8) 2_575 . . . ? I3 B3 B5 B2 108.4(11) . . . . ? B4 B3 B5 B6 38.4(9) 2_575 . . . ? B1 B3 B5 B6 100.4(10) 2_575 . . . ? B2 B3 B5 B6 139.2(10) . . . . ? I3 B3 B5 B6 -112.4(11) . . . . ? B4 B3 B5 B4 -62.2(12) 2_575 . . . ? B6 B3 B5 B4 -100.6(10) . . . . ? B1 B3 B5 B4 -0.2(11) 2_575 . . . ? B2 B3 B5 B4 38.6(8) . . . . ? I3 B3 B5 B4 147.0(9) . . . . ? B4 B3 B5 I5 149.0(8) 2_575 . . . ? B6 B3 B5 I5 110.6(10) . . . . ? B1 B3 B5 I5 -149.0(8) 2_575 . . . ? B2 B3 B5 I5 -110.1(9) . . . . ? I3 B3 B5 I5 -1.8(14) . . . . ? B3 B4 B5 B1 -39.2(8) 2_575 . . . ? B6 B4 B5 B1 -102.7(9) 2_575 . . . ? B2 B4 B5 B1 -140.5(9) . . . . ? I4 B4 B5 B1 111.5(9) . . . . ? B1 B4 B5 B2 140.5(9) . . . . ? B3 B4 B5 B2 101.3(9) 2_575 . . . ? B6 B4 B5 B2 37.8(8) 2_575 . . . ? I4 B4 B5 B2 -108.0(9) . . . . ? B1 B4 B5 B3 101.5(9) . . . . ? B3 B4 B5 B3 62.4(11) 2_575 . . . ? B6 B4 B5 B3 -1.2(11) 2_575 . . . ? B2 B4 B5 B3 -38.9(8) . . . . ? I4 B4 B5 B3 -147.0(8) . . . . ? B1 B4 B5 B6 38.3(8) . . . . ? B3 B4 B5 B6 -0.8(11) 2_575 . . . ? B6 B4 B5 B6 -64.4(11) 2_575 . . . ? B2 B4 B5 B6 -102.1(9) . . . . ? I4 B4 B5 B6 149.8(7) . . . . ? B1 B4 B5 I5 -110.8(9) . . . . ? B3 B4 B5 I5 -149.9(7) 2_575 . . . ? B6 B4 B5 I5 146.5(7) 2_575 . . . ? B2 B4 B5 I5 108.8(9) . . . . ? I4 B4 B5 I5 0.7(12) . . . . ? B5 B3 B6 B4 137.3(10) . . . 2_575 ? B1 B3 B6 B4 36.9(8) 2_575 . . 2_575 ? B2 B3 B6 B4 101.2(10) . . . 2_575 ? I3 B3 B6 B4 -109.2(10) . . . 2_575 ? B4 B3 B6 B5 -137.3(10) 2_575 . . . ? B1 B3 B6 B5 -100.4(10) 2_575 . . . ? B2 B3 B6 B5 -36.1(9) . . . . ? I3 B3 B6 B5 113.5(10) . . . . ? B4 B3 B6 B2 -37.3(8) 2_575 . . 2_575 ? B5 B3 B6 B2 100.0(10) . . . 2_575 ? B1 B3 B6 B2 -0.4(11) 2_575 . . 2_575 ? B2 B3 B6 B2 63.9(11) . . . 2_575 ? I3 B3 B6 B2 -146.5(8) . . . 2_575 ? B4 B3 B6 B1 -101.7(10) 2_575 . . . ? B5 B3 B6 B1 35.5(9) . . . . ? B1 B3 B6 B1 -64.8(11) 2_575 . . . ? B2 B3 B6 B1 -0.6(12) . . . . ? I3 B3 B6 B1 149.0(8) . . . . ? B4 B3 B6 I6 113.4(9) 2_575 . . . ? B5 B3 B6 I6 -109.3(10) . . . . ? B1 B3 B6 I6 150.3(8) 2_575 . . . ? B2 B3 B6 I6 -145.4(8) . . . . ? I3 B3 B6 I6 4.2(13) . . . . ? B1 B5 B6 B3 139.2(10) . . . . ? B2 B5 B6 B3 37.4(9) . . . . ? B4 B5 B6 B3 102.0(9) . . . . ? I5 B5 B6 B3 -108.3(10) . . . . ? B1 B5 B6 B4 101.5(10) . . . 2_575 ? B2 B5 B6 B4 -0.4(12) . . . 2_575 ? B3 B5 B6 B4 -37.8(9) . . . 2_575 ? B4 B5 B6 B4 64.3(11) . . . 2_575 ? I5 B5 B6 B4 -146.1(8) . . . 2_575 ? B1 B5 B6 B2 37.6(8) . . . 2_575 ? B2 B5 B6 B2 -64.2(11) . . . 2_575 ? B3 B5 B6 B2 -101.6(10) . . . 2_575 ? B4 B5 B6 B2 0.4(11) . . . 2_575 ? I5 B5 B6 B2 150.1(8) . . . 2_575 ? B2 B5 B6 B1 -101.8(10) . . . . ? B3 B5 B6 B1 -139.2(10) . . . . ? B4 B5 B6 B1 -37.2(8) . . . . ? I5 B5 B6 B1 112.5(9) . . . . ? B1 B5 B6 I6 -107.0(9) . . . . ? B2 B5 B6 I6 151.2(8) . . . . ? B3 B5 B6 I6 113.8(10) . . . . ? B4 B5 B6 I6 -144.1(8) . . . . ? I5 B5 B6 I6 5.5(12) . . . . ? B4 B1 B6 B3 2.2(12) . . . . ? B5 B1 B6 B3 -36.4(8) . . . . ? B3 B1 B6 B3 65.1(11) 2_575 . . . ? B2 B1 B6 B3 101.9(10) 2_575 . . . ? I1 B1 B6 B3 -147.7(8) . . . . ? B4 B1 B6 B4 -60.6(12) . . . 2_575 ? B5 B1 B6 B4 -99.2(9) . . . 2_575 ? B3 B1 B6 B4 2.2(11) 2_575 . . 2_575 ? B2 B1 B6 B4 39.1(8) 2_575 . . 2_575 ? I1 B1 B6 B4 149.5(8) . . . 2_575 ? B4 B1 B6 B5 38.6(9) . . . . ? B3 B1 B6 B5 101.4(9) 2_575 . . . ? B2 B1 B6 B5 138.3(10) 2_575 . . . ? I1 B1 B6 B5 -111.3(9) . . . . ? B4 B1 B6 B2 -99.7(10) . . . 2_575 ? B5 B1 B6 B2 -138.3(10) . . . 2_575 ? B3 B1 B6 B2 -36.8(8) 2_575 . . 2_575 ? I1 B1 B6 B2 110.4(9) . . . 2_575 ? B4 B1 B6 I6 149.1(8) . . . . ? B5 B1 B6 I6 110.5(9) . . . . ? B3 B1 B6 I6 -148.1(8) 2_575 . . . ? B2 B1 B6 I6 -111.2(9) 2_575 . . . ? I1 B1 B6 I6 -0.9(12) . . . . ? B9 B7 B8 B11 38.4(8) . . . 2_556 ? B11 B7 B8 B11 -62.2(13) . . . 2_556 ? B10 B7 B8 B11 -0.1(12) . . . 2_556 ? B12 B7 B8 B11 -101.0(10) . . . 2_556 ? I7 B7 B8 B11 148.7(9) . . . 2_556 ? B11 B7 B8 B9 -100.6(9) . . . . ? B10 B7 B8 B9 -38.5(8) . . . . ? B12 B7 B8 B9 -139.4(9) . . . . ? I7 B7 B8 B9 110.3(10) . . . . ? B9 B7 B8 B10 102.2(10) . . . 2_556 ? B11 B7 B8 B10 1.5(13) . . . 2_556 ? B10 B7 B8 B10 63.6(13) . . . 2_556 ? B12 B7 B8 B10 -37.2(9) . . . 2_556 ? I7 B7 B8 B10 -147.5(9) . . . 2_556 ? B9 B7 B8 B12 139.4(9) . . . . ? B11 B7 B8 B12 38.7(9) . . . . ? B10 B7 B8 B12 100.9(9) . . . . ? I7 B7 B8 B12 -110.3(10) . . . . ? B9 B7 B8 I8 -110.4(10) . . . . ? B11 B7 B8 I8 149.0(8) . . . . ? B10 B7 B8 I8 -148.9(8) . . . . ? B12 B7 B8 I8 110.2(10) . . . . ? I7 B7 B8 I8 -0.1(14) . . . . ? B11 B8 B9 B7 -138.0(9) 2_556 . . . ? B10 B8 B9 B7 -101.1(10) 2_556 . . . ? B12 B8 B9 B7 -37.0(8) . . . . ? I8 B8 B9 B7 110.2(9) . . . . ? B7 B8 B9 B11 138.0(9) . . . 2_556 ? B10 B8 B9 B11 36.9(8) 2_556 . . 2_556 ? B12 B8 B9 B11 101.0(9) . . . 2_556 ? I8 B8 B9 B11 -111.8(9) . . . 2_556 ? B11 B8 B9 B10 -99.5(9) 2_556 . . . ? B7 B8 B9 B10 38.4(8) . . . . ? B10 B8 B9 B10 -62.7(12) 2_556 . . . ? B12 B8 B9 B10 1.4(12) . . . . ? I8 B8 B9 B10 148.6(8) . . . . ? B11 B8 B9 B12 -37.2(8) 2_556 . . 2_556 ? B7 B8 B9 B12 100.8(9) . . . 2_556 ? B10 B8 B9 B12 -0.3(12) 2_556 . . 2_556 ? B12 B8 B9 B12 63.8(12) . . . 2_556 ? I8 B8 B9 B12 -149.0(8) . . . 2_556 ? B11 B8 B9 I9 110.7(10) 2_556 . . . ? B7 B8 B9 I9 -111.4(10) . . . . ? B10 B8 B9 I9 147.6(8) 2_556 . . . ? B12 B8 B9 I9 -148.4(8) . . . . ? I8 B8 B9 I9 -1.1(13) . . . . ? B11 B7 B9 B8 100.4(9) . . . . ? B10 B7 B9 B8 137.0(9) . . . . ? B12 B7 B9 B8 36.5(8) . . . . ? I7 B7 B9 B8 -111.3(9) . . . . ? B8 B7 B9 B11 -37.2(8) . . . 2_556 ? B11 B7 B9 B11 63.2(11) . . . 2_556 ? B10 B7 B9 B11 99.8(9) . . . 2_556 ? B12 B7 B9 B11 -0.7(11) . . . 2_556 ? I7 B7 B9 B11 -148.5(8) . . . 2_556 ? B8 B7 B9 B10 -137.0(9) . . . . ? B11 B7 B9 B10 -36.6(8) . . . . ? B12 B7 B9 B10 -100.5(9) . . . . ? I7 B7 B9 B10 111.7(10) . . . . ? B8 B7 B9 B12 -100.7(9) . . . 2_556 ? B11 B7 B9 B12 -0.2(11) . . . 2_556 ? B10 B7 B9 B12 36.3(8) . . . 2_556 ? B12 B7 B9 B12 -64.2(11) . . . 2_556 ? I7 B7 B9 B12 148.0(8) . . . 2_556 ? B8 B7 B9 I9 112.9(9) . . . . ? B11 B7 B9 I9 -146.7(8) . . . . ? B10 B7 B9 I9 -110.2(9) . . . . ? B12 B7 B9 I9 149.4(8) . . . . ? I7 B7 B9 I9 1.5(13) . . . . ? B8 B7 B10 B11 -100.5(9) . . . . ? B9 B7 B10 B11 -138.5(9) . . . . ? B12 B7 B10 B11 -37.1(8) . . . . ? I7 B7 B10 B11 110.6(10) . . . . ? B8 B7 B10 B8 -63.0(12) . . . 2_556 ? B9 B7 B10 B8 -101.0(9) . . . 2_556 ? B11 B7 B10 B8 37.5(8) . . . 2_556 ? B12 B7 B10 B8 0.4(12) . . . 2_556 ? I7 B7 B10 B8 148.1(8) . . . 2_556 ? B8 B7 B10 B12 0.9(12) . . . 2_556 ? B9 B7 B10 B12 -37.1(8) . . . 2_556 ? B11 B7 B10 B12 101.4(10) . . . 2_556 ? B12 B7 B10 B12 64.3(12) . . . 2_556 ? I7 B7 B10 B12 -148.0(8) . . . 2_556 ? B8 B7 B10 B9 38.0(8) . . . . ? B11 B7 B10 B9 138.5(9) . . . . ? B12 B7 B10 B9 101.4(10) . . . . ? I7 B7 B10 B9 -110.9(10) . . . . ? B8 B7 B10 I10 147.4(8) . . . . ? B9 B7 B10 I10 109.4(10) . . . . ? B11 B7 B10 I10 -112.1(9) . . . . ? B12 B7 B10 I10 -149.2(8) . . . . ? I7 B7 B10 I10 -1.5(14) . . . . ? B8 B9 B10 B11 -1.2(11) . . . . ? B7 B9 B10 B11 37.2(8) . . . . ? B11 B9 B10 B11 -63.7(12) 2_556 . . . ? B12 B9 B10 B11 -101.7(9) 2_556 . . . ? I9 B9 B10 B11 149.4(8) . . . . ? B8 B9 B10 B8 61.9(12) . . . 2_556 ? B7 B9 B10 B8 100.2(10) . . . 2_556 ? B11 B9 B10 B8 -0.6(12) 2_556 . . 2_556 ? B12 B9 B10 B8 -38.7(9) 2_556 . . 2_556 ? I9 B9 B10 B8 -147.6(8) . . . 2_556 ? B8 B9 B10 B12 100.6(9) . . . 2_556 ? B7 B9 B10 B12 138.9(9) . . . 2_556 ? B11 B9 B10 B12 38.1(9) 2_556 . . 2_556 ? I9 B9 B10 B12 -108.9(10) . . . 2_556 ? B8 B9 B10 B7 -38.4(8) . . . . ? B11 B9 B10 B7 -100.9(10) 2_556 . . . ? B12 B9 B10 B7 -138.9(9) 2_556 . . . ? I9 B9 B10 B7 112.2(10) . . . . ? B8 B9 B10 I10 -146.8(8) . . . . ? B7 B9 B10 I10 -108.4(9) . . . . ? B11 B9 B10 I10 150.7(8) 2_556 . . . ? B12 B9 B10 I10 112.6(10) 2_556 . . . ? I9 B9 B10 I10 3.7(13) . . . . ? B12 B10 B11 B8 36.8(8) 2_556 . . 2_556 ? B7 B10 B11 B8 137.7(9) . . . 2_556 ? B9 B10 B11 B8 101.0(9) . . . 2_556 ? I10 B10 B11 B8 -114.1(9) . . . 2_556 ? B8 B10 B11 B7 -137.7(9) 2_556 . . . ? B12 B10 B11 B7 -100.9(9) 2_556 . . . ? B9 B10 B11 B7 -36.7(8) . . . . ? I10 B10 B11 B7 108.2(10) . . . . ? B8 B10 B11 B9 -36.4(8) 2_556 . . 2_556 ? B12 B10 B11 B9 0.4(11) 2_556 . . 2_556 ? B7 B10 B11 B9 101.3(9) . . . 2_556 ? B9 B10 B11 B9 64.6(11) . . . 2_556 ? I10 B10 B11 B9 -150.5(8) . . . 2_556 ? B8 B10 B11 B12 -100.5(9) 2_556 . . . ? B12 B10 B11 B12 -63.8(11) 2_556 . . . ? B7 B10 B11 B12 37.2(8) . . . . ? B9 B10 B11 B12 0.5(11) . . . . ? I10 B10 B11 B12 145.4(8) . . . . ? B8 B10 B11 I11 110.3(9) 2_556 . . . ? B12 B10 B11 I11 147.1(8) 2_556 . . . ? B7 B10 B11 I11 -112.0(9) . . . . ? B9 B10 B11 I11 -148.6(8) . . . . ? I10 B10 B11 I11 -3.7(13) . . . . ? B8 B7 B11 B8 61.9(12) . . . 2_556 ? B9 B7 B11 B8 -0.8(12) . . . 2_556 ? B10 B7 B11 B8 -38.1(8) . . . 2_556 ? B12 B7 B11 B8 100.5(9) . . . 2_556 ? I7 B7 B11 B8 -149.0(8) . . . 2_556 ? B8 B7 B11 B10 100.0(10) . . . . ? B9 B7 B11 B10 37.3(8) . . . . ? B12 B7 B11 B10 138.6(9) . . . . ? I7 B7 B11 B10 -110.8(10) . . . . ? B8 B7 B11 B9 -1.1(12) . . . 2_556 ? B9 B7 B11 B9 -63.9(12) . . . 2_556 ? B10 B7 B11 B9 -101.2(9) . . . 2_556 ? B12 B7 B11 B9 37.5(9) . . . 2_556 ? I7 B7 B11 B9 148.0(8) . . . 2_556 ? B8 B7 B11 B12 -38.6(9) . . . . ? B9 B7 B11 B12 -101.4(10) . . . . ? B10 B7 B11 B12 -138.6(9) . . . . ? I7 B7 B11 B12 110.5(10) . . . . ? B8 B7 B11 I11 -149.9(8) . . . . ? B9 B7 B11 I11 147.4(8) . . . . ? B10 B7 B11 I11 110.1(10) . . . . ? B12 B7 B11 I11 -111.3(10) . . . . ? I7 B7 B11 I11 -0.8(14) . . . . ? B11 B8 B12 B10 -36.6(8) 2_556 . . 2_556 ? B9 B8 B12 B10 -101.7(10) . . . 2_556 ? B7 B8 B12 B10 -138.6(9) . . . 2_556 ? I8 B8 B12 B10 111.0(9) . . . 2_556 ? B11 B8 B12 B7 102.1(9) 2_556 . . . ? B9 B8 B12 B7 36.9(8) . . . . ? B10 B8 B12 B7 138.6(9) 2_556 . . . ? I8 B8 B12 B7 -110.4(9) . . . . ? B11 B8 B12 B11 64.0(11) 2_556 . . . ? B9 B8 B12 B11 -1.1(11) . . . . ? B7 B8 B12 B11 -38.0(8) . . . . ? B10 B8 B12 B11 100.6(9) 2_556 . . . ? I8 B8 B12 B11 -148.4(7) . . . . ? B11 B8 B12 B9 1.8(12) 2_556 . . 2_556 ? B9 B8 B12 B9 -63.4(12) . . . 2_556 ? B7 B8 B12 B9 -100.3(9) . . . 2_556 ? B10 B8 B12 B9 38.3(8) 2_556 . . 2_556 ? I8 B8 B12 B9 149.3(7) . . . 2_556 ? B11 B8 B12 I12 -148.7(8) 2_556 . . . ? B9 B8 B12 I12 146.2(8) . . . . ? B7 B8 B12 I12 109.3(9) . . . . ? B10 B8 B12 I12 -112.1(10) 2_556 . . . ? I8 B8 B12 I12 -1.1(13) . . . . ? B8 B7 B12 B10 36.6(8) . . . 2_556 ? B9 B7 B12 B10 0.4(11) . . . 2_556 ? B11 B7 B12 B10 -100.1(9) . . . 2_556 ? B10 B7 B12 B10 -63.6(12) . . . 2_556 ? I7 B7 B12 B10 148.4(8) . . . 2_556 ? B9 B7 B12 B8 -36.2(8) . . . . ? B11 B7 B12 B8 -136.7(9) . . . . ? B10 B7 B12 B8 -100.3(10) . . . . ? I7 B7 B12 B8 111.8(9) . . . . ? B8 B7 B12 B11 136.7(9) . . . . ? B9 B7 B12 B11 100.5(9) . . . . ? B10 B7 B12 B11 36.5(8) . . . . ? I7 B7 B12 B11 -111.5(10) . . . . ? B8 B7 B12 B9 100.0(10) . . . 2_556 ? B9 B7 B12 B9 63.8(11) . . . 2_556 ? B11 B7 B12 B9 -36.7(8) . . . 2_556 ? B10 B7 B12 B9 -0.3(12) . . . 2_556 ? I7 B7 B12 B9 -148.3(8) . . . 2_556 ? B8 B7 B12 I12 -111.8(9) . . . . ? B9 B7 B12 I12 -147.9(8) . . . . ? B11 B7 B12 I12 111.5(9) . . . . ? B10 B7 B12 I12 148.0(8) . . . . ? I7 B7 B12 I12 0.0(13) . . . . ? B8 B11 B12 B10 -1.3(12) 2_556 . . 2_556 ? B10 B11 B12 B10 62.8(11) . . . 2_556 ? B7 B11 B12 B10 100.3(10) . . . 2_556 ? B9 B11 B12 B10 -38.2(8) 2_556 . . 2_556 ? I11 B11 B12 B10 -148.5(8) . . . 2_556 ? B8 B11 B12 B8 -63.7(11) 2_556 . . . ? B10 B11 B12 B8 0.4(11) . . . . ? B7 B11 B12 B8 37.8(8) . . . . ? B9 B11 B12 B8 -100.6(9) 2_556 . . . ? I11 B11 B12 B8 149.0(8) . . . . ? B8 B11 B12 B7 -101.5(10) 2_556 . . . ? B10 B11 B12 B7 -37.5(9) . . . . ? B9 B11 B12 B7 -138.4(9) 2_556 . . . ? I11 B11 B12 B7 111.2(10) . . . . ? B8 B11 B12 B9 36.9(9) 2_556 . . 2_556 ? B10 B11 B12 B9 101.0(9) . . . 2_556 ? B7 B11 B12 B9 138.4(9) . . . 2_556 ? I11 B11 B12 B9 -110.4(10) . . . 2_556 ? B8 B11 B12 I12 148.9(8) 2_556 . . . ? B10 B11 B12 I12 -147.0(8) . . . . ? B7 B11 B12 I12 -109.6(9) . . . . ? B9 B11 B12 I12 112.0(9) 2_556 . . . ? I11 B11 B12 I12 1.6(13) . . . . ? Na2 O1 S1 O2 1(4) 1_455 . . . ? O1 S1 O2 Na1 -70.9(19) . . . . ? O7 Na1 O2 S1 170.8(18) . . . . ? O13 Na1 O2 S1 -11(2) . . . . ? O11 Na1 O2 S1 68.1(18) . . . . ? O6 Na1 O2 S1 -116.3(17) . . . . ? O15 Na1 O2 S1 -78.2(18) . . . . ? O9 Na1 O2 S1 109.7(18) . . . . ? O17 Na2 O3 S2 65.7(10) . . . . ? O5 Na2 O3 S2 -95.3(10) . . . . ? O1 Na2 O3 S2 147.0(10) 1_655 . . . ? O12 Na2 O3 S2 -100(2) 1_655 . . . ? O8 Na2 O3 S2 -17.9(11) . . . . ? Na2 O3 S2 O4 31.5(13) . . . . ? O17 Na2 O5 S3 119.8(16) . . . . ? O1 Na2 O5 S3 -93.4(14) 1_655 . . . ? O3 Na2 O5 S3 169.0(13) . . . . ? O12 Na2 O5 S3 -12.4(13) 1_655 . . . ? O8 Na2 O5 S3 74.0(13) . . . . ? Na2 O5 S3 O6 -119.6(12) . . . . ? O5 S3 O6 Na1 -4.3(13) . . . . ? O7 Na1 O6 S3 52.9(10) . . . . ? O13 Na1 O6 S3 -138.0(11) . . . . ? O11 Na1 O6 S3 152.6(9) . . . . ? O15 Na1 O6 S3 -54.2(10) . . . . ? O9 Na1 O6 S3 133.8(11) . . . . ? O2 Na1 O6 S3 -18.0(13) . . . . ? O13 Na1 O7 S4 -64(3) . . . . ? O11 Na1 O7 S4 180(10) . . . . ? O6 Na1 O7 S4 -27(3) . . . . ? O15 Na1 O7 S4 46(3) . . . . ? O9 Na1 O7 S4 -104(3) . . . . ? O2 Na1 O7 S4 110(3) . . . . ? Na1 O7 S4 O8 8(3) . . . . ? O7 S4 O8 Na2 -56.0(16) . . . . ? O17 Na2 O8 S4 -99.9(14) . . . . ? O5 Na2 O8 S4 62.3(14) . . . . ? O1 Na2 O8 S4 -152.3(13) 1_655 . . . ? O3 Na2 O8 S4 -22.0(14) . . . . ? O12 Na2 O8 S4 140.9(13) 1_655 . . . ? O7 Na1 O9 S5 146(2) . . . . ? O13 Na1 O9 S5 -23(2) . . . . ? O11 Na1 O9 S5 -113(2) . . . . ? O6 Na1 O9 S5 58(2) . . . . ? O15 Na1 O9 S5 42(2) . . . . ? O2 Na1 O9 S5 -153.4(19) . . . . ? Na1 O9 S5 O10 -178.9(18) . . . . ? O7 Na1 O11 S6 31(4) . . . . ? O13 Na1 O11 S6 -133(4) . . . . ? O6 Na1 O11 S6 -66(4) . . . . ? O15 Na1 O11 S6 148(4) . . . . ? O9 Na1 O11 S6 -47(4) . . . . ? O2 Na1 O11 S6 107(4) . . . . ? Na1 O11 S6 O12 -139(4) . . . . ? O11 S6 O12 Na2 46.3(17) . . . 1_455 ? O7 Na1 O15 S8 52(3) . . . . ? O13 Na1 O15 S8 -145(2) . . . . ? O11 Na1 O15 S8 -62(3) . . . . ? O6 Na1 O15 S8 133(2) . . . . ? O9 Na1 O15 S8 149(2) . . . . ? O2 Na1 O15 S8 -20(2) . . . . ? Na1 O15 S8 O16 -20(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.452 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.222