# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Carsten Knapp' _publ_contact_author_email CARSTEN.KNAPP@AC.UNI-FREIBURG.DE _publ_section_title ; Synthesis and Characterization of Synthetically Useful Salts of the Weakly-Coordinating Dianion [B12Cl12]2- ; loop_ _publ_author_name 'Carsten Knapp' 'Vanessa Geis' 'Kristin Guttsche' 'Harald Scherer' 'Rabiya Uzin' # Attachment 'cif_files.cif' data_ck008 _database_code_depnum_ccdc_archive 'CCDC 710773' _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_ck014 _database_code_depnum_ccdc_archive 'CCDC 710774' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C19 H15), B12 Cl12, 2(C2 H4 Cl2)' _chemical_formula_sum 'C42 H38 B12 Cl16' _chemical_formula_weight 1239.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' B B 0.0013 0.0007 '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 9.9318(2) _cell_length_b 14.9879(4) _cell_length_c 17.9243(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.6220(10) _cell_angle_gamma 90.00 _cell_volume 2667.08(11) _cell_formula_units_Z 2 _cell_measurement_temperature 114(2) _cell_measurement_reflns_used 9919 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.46 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8358 _exptl_absorpt_correction_T_max 0.9470 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 114(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_type 'Bruker APEX II CCD area detector' _diffrn_measurement_method 'APEXII (Bruker, 2005)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62722 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.57 _reflns_number_total 6807 _reflns_number_gt 5751 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Saint V7.23A (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'Sadabs 2004/1 (Bruker AXS BV, 1997-2004)' _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^)+(0.0402P)^2^+1.1219P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6807 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.92594(16) 0.55877(11) 0.06807(9) 0.0174(3) Uani 1 1 d . . . Cl1 Cl 0.84921(4) 0.62069(2) 0.14046(2) 0.02371(9) Uani 1 1 d . . . B2 B 0.87395(16) 0.57058(11) -0.02756(9) 0.0179(3) Uani 1 1 d . . . Cl2 Cl 0.74078(4) 0.64499(3) -0.05494(2) 0.02642(9) Uani 1 1 d . . . B3 B 1.03540(16) 0.61028(11) 0.00369(9) 0.0180(3) Uani 1 1 d . . . Cl3 Cl 1.07537(4) 0.72669(2) 0.00884(2) 0.02334(9) Uani 1 1 d . . . B4 B 1.10129(16) 0.53433(11) 0.07200(9) 0.0180(3) Uani 1 1 d . . . Cl4 Cl 1.20430(4) 0.57282(3) 0.14895(2) 0.02449(9) Uani 1 1 d . . . B5 B 0.98176(16) 0.44731(11) 0.08283(9) 0.0181(3) Uani 1 1 d . . . Cl5 Cl 0.96323(4) 0.39253(2) 0.17063(2) 0.02529(9) Uani 1 1 d . . . B6 B 0.84099(16) 0.46958(11) 0.02134(9) 0.0183(3) Uani 1 1 d . . . Cl6 Cl 0.67332(4) 0.43814(3) 0.04379(2) 0.02687(9) Uani 1 1 d . . . C1 C 0.70843(15) 0.94270(10) 0.16934(8) 0.0198(3) Uani 1 1 d . . . C2 C 0.66958(15) 1.03557(10) 0.16896(8) 0.0211(3) Uani 1 1 d . . . C3 C 0.76771(16) 1.10156(11) 0.15746(9) 0.0247(3) Uani 1 1 d . . . H3 H 0.8597 1.0850 0.1542 0.0357(14) Uiso 1 1 calc R . . C4 C 0.73157(18) 1.18999(11) 0.15083(9) 0.0292(4) Uani 1 1 d . . . H4 H 0.7978 1.2339 0.1410 0.0357(14) Uiso 1 1 calc R . . C5 C 0.59869(19) 1.21449(11) 0.15848(10) 0.0314(4) Uani 1 1 d . . . H5 H 0.5736 1.2754 0.1533 0.0357(14) Uiso 1 1 calc R . . C6 C 0.50140(18) 1.15103(12) 0.17371(10) 0.0307(4) Uani 1 1 d . . . H6 H 0.4111 1.1690 0.1812 0.0357(14) Uiso 1 1 calc R . . C7 C 0.53566(16) 1.06208(11) 0.17797(9) 0.0250(3) Uani 1 1 d . . . H7 H 0.4684 1.0186 0.1870 0.0357(14) Uiso 1 1 calc R . . C8 C 0.84057(15) 0.91793(10) 0.19833(9) 0.0210(3) Uani 1 1 d . . . C9 C 0.89605(15) 0.96242(10) 0.26117(9) 0.0232(3) Uani 1 1 d . . . H9 H 0.8462 1.0080 0.2847 0.0357(14) Uiso 1 1 calc R . . C10 C 1.02263(16) 0.93998(11) 0.28857(9) 0.0256(3) Uani 1 1 d . . . H10 H 1.0586 0.9687 0.3320 0.0357(14) Uiso 1 1 calc R . . C11 C 1.09741(16) 0.87560(11) 0.25287(10) 0.0276(3) Uani 1 1 d . . . H11 H 1.1859 0.8620 0.2709 0.0357(14) Uiso 1 1 calc R . . C12 C 1.04420(16) 0.83080(11) 0.19094(10) 0.0273(3) Uani 1 1 d . . . H12 H 1.0960 0.7865 0.1670 0.0357(14) Uiso 1 1 calc R . . C13 C 0.91593(16) 0.85070(10) 0.16406(9) 0.0233(3) Uani 1 1 d . . . H13 H 0.8787 0.8190 0.1225 0.0357(14) Uiso 1 1 calc R . . C14 C 0.61867(15) 0.87612(10) 0.13887(9) 0.0225(3) Uani 1 1 d . . . C15 C 0.62249(16) 0.78840(11) 0.16669(9) 0.0253(3) Uani 1 1 d . . . H15 H 0.6856 0.7728 0.2053 0.0357(14) Uiso 1 1 calc R . . C16 C 0.53494(17) 0.72497(12) 0.13806(11) 0.0331(4) Uani 1 1 d . . . H16 H 0.5362 0.6663 0.1580 0.0357(14) Uiso 1 1 calc R . . C17 C 0.44570(18) 0.74615(13) 0.08073(12) 0.0390(4) Uani 1 1 d . . . H17 H 0.3866 0.7017 0.0608 0.0357(14) Uiso 1 1 calc R . . C18 C 0.44142(19) 0.83197(13) 0.05175(11) 0.0382(4) Uani 1 1 d . . . H18 H 0.3803 0.8458 0.0117 0.0357(14) Uiso 1 1 calc R . . C19 C 0.52502(17) 0.89683(12) 0.08063(10) 0.0299(4) Uani 1 1 d . . . H19 H 0.5200 0.9559 0.0614 0.0357(14) Uiso 1 1 calc R . . Cl7 Cl 0.37935(5) 0.66865(3) 0.30994(3) 0.04394(12) Uani 1 1 d . . . Cl8 Cl 0.31396(6) 0.49305(4) 0.49389(3) 0.05389(15) Uani 1 1 d . . . C20 C 0.3487(4) 0.6277(3) 0.4037(2) 0.0422(8) Uani 0.60 1 d P A 1 H20A H 0.4219 0.6476 0.4384 0.067(5) Uiso 0.60 1 calc PR A 1 H20B H 0.2625 0.6519 0.4213 0.067(5) Uiso 0.60 1 calc PR A 1 C21 C 0.3431(3) 0.5295(2) 0.40209(19) 0.0375(7) Uani 0.60 1 d P A 1 H21A H 0.4292 0.5049 0.3846 0.067(5) Uiso 0.60 1 calc PR A 1 H21B H 0.2695 0.5092 0.3678 0.067(5) Uiso 0.60 1 calc PR A 1 C20A C 0.3501(4) 0.5728(3) 0.3604(3) 0.0297(9) Uani 0.40 1 d P A 2 H20C H 0.2664 0.5436 0.3414 0.067(5) Uiso 0.40 1 calc PR A 2 H20D H 0.4257 0.5305 0.3547 0.067(5) Uiso 0.40 1 calc PR A 2 C21A C 0.3368(6) 0.5962(4) 0.4406(3) 0.0437(13) Uani 0.40 1 d P A 2 H21C H 0.2584 0.6360 0.4468 0.067(5) Uiso 0.40 1 calc PR A 2 H21D H 0.4187 0.6278 0.4591 0.067(5) Uiso 0.40 1 calc PR A 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 0.0180(7) 0.0162(7) 0.0179(8) -0.0020(6) 0.0009(6) 0.0005(6) Cl1 0.02732(18) 0.02093(17) 0.02311(18) -0.00472(14) 0.00466(14) 0.00171(14) B2 0.0177(7) 0.0168(7) 0.0192(8) -0.0013(6) -0.0013(6) 0.0018(6) Cl2 0.02486(18) 0.02393(19) 0.0301(2) -0.00036(15) -0.00562(15) 0.00699(14) B3 0.0195(7) 0.0150(7) 0.0196(8) -0.0012(6) 0.0000(6) -0.0019(6) Cl3 0.02873(18) 0.01471(16) 0.02654(19) -0.00146(13) 0.00029(14) -0.00279(13) B4 0.0187(7) 0.0167(7) 0.0185(8) -0.0023(6) -0.0022(6) -0.0003(6) Cl4 0.02425(18) 0.02515(18) 0.02363(18) -0.00483(14) -0.00707(14) -0.00025(14) B5 0.0214(7) 0.0157(7) 0.0171(8) -0.0004(6) 0.0002(6) -0.0006(6) Cl5 0.0355(2) 0.02104(18) 0.01943(18) 0.00282(14) 0.00264(14) -0.00134(14) B6 0.0178(7) 0.0173(7) 0.0198(8) -0.0020(6) 0.0007(6) -0.0016(6) Cl6 0.01954(17) 0.0286(2) 0.0327(2) -0.00531(16) 0.00497(14) -0.00591(14) C1 0.0214(7) 0.0206(7) 0.0173(7) -0.0001(6) 0.0003(5) -0.0020(5) C2 0.0237(7) 0.0201(7) 0.0195(7) -0.0009(6) -0.0014(6) -0.0009(6) C3 0.0248(7) 0.0244(8) 0.0249(8) -0.0019(6) 0.0013(6) -0.0034(6) C4 0.0380(9) 0.0224(8) 0.0273(8) -0.0018(6) 0.0033(7) -0.0056(7) C5 0.0434(10) 0.0201(8) 0.0308(9) -0.0016(7) 0.0015(7) 0.0045(7) C6 0.0276(8) 0.0292(9) 0.0351(9) -0.0034(7) -0.0016(7) 0.0060(7) C7 0.0232(7) 0.0249(8) 0.0268(8) -0.0008(6) -0.0023(6) -0.0008(6) C8 0.0199(7) 0.0192(7) 0.0236(7) 0.0003(6) -0.0009(6) -0.0019(5) C9 0.0241(7) 0.0213(7) 0.0242(8) -0.0022(6) -0.0008(6) -0.0024(6) C10 0.0245(8) 0.0261(8) 0.0258(8) 0.0003(6) -0.0039(6) -0.0054(6) C11 0.0217(7) 0.0309(8) 0.0300(9) 0.0055(7) -0.0024(6) -0.0012(6) C12 0.0255(8) 0.0253(8) 0.0312(9) 0.0009(7) 0.0025(6) 0.0037(6) C13 0.0262(8) 0.0200(7) 0.0237(8) -0.0026(6) 0.0001(6) -0.0006(6) C14 0.0221(7) 0.0215(7) 0.0238(8) -0.0029(6) -0.0013(6) -0.0012(6) C15 0.0242(7) 0.0218(7) 0.0298(8) -0.0011(6) -0.0011(6) -0.0003(6) C16 0.0290(8) 0.0208(8) 0.0497(11) -0.0044(7) 0.0026(8) -0.0042(6) C17 0.0294(9) 0.0313(9) 0.0557(12) -0.0164(9) -0.0062(8) -0.0075(7) C18 0.0339(9) 0.0380(10) 0.0418(11) -0.0089(8) -0.0162(8) -0.0002(8) C19 0.0328(9) 0.0258(8) 0.0305(9) -0.0017(7) -0.0093(7) 0.0009(7) Cl7 0.0415(3) 0.0413(3) 0.0489(3) 0.0058(2) -0.0007(2) 0.0001(2) Cl8 0.0571(3) 0.0629(4) 0.0422(3) 0.0042(3) 0.0105(2) -0.0156(3) C20 0.046(2) 0.041(2) 0.040(2) -0.0102(17) -0.0057(16) 0.0024(16) C21 0.0397(17) 0.0383(18) 0.0345(17) -0.0082(15) 0.0031(13) -0.0039(14) C20A 0.026(2) 0.024(2) 0.040(3) -0.005(2) 0.0038(18) -0.0041(16) C21A 0.063(4) 0.035(3) 0.034(3) -0.002(2) 0.009(3) -0.011(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 B5 1.778(2) . ? B1 B6 1.778(2) . ? B1 B4 1.779(2) . ? B1 B3 1.783(2) . ? B1 Cl1 1.7838(16) . ? B1 B2 1.785(2) . ? B2 B4 1.783(2) 3_765 ? B2 B6 1.784(2) . ? B2 B5 1.785(2) 3_765 ? B2 B3 1.786(2) . ? B2 Cl2 1.7879(16) . ? B3 B5 1.779(2) 3_765 ? B3 B6 1.781(2) 3_765 ? B3 B4 1.783(2) . ? B3 Cl3 1.7911(17) . ? B4 B5 1.778(2) . ? B4 B2 1.783(2) 3_765 ? B4 B6 1.785(2) 3_765 ? B4 Cl4 1.7894(16) . ? B5 B3 1.779(2) 3_765 ? B5 B2 1.785(2) 3_765 ? B5 B6 1.787(2) . ? B5 Cl5 1.7891(17) . ? B6 B3 1.781(2) 3_765 ? B6 B4 1.785(2) 3_765 ? B6 Cl6 1.7874(16) . ? C1 C14 1.436(2) . ? C1 C2 1.444(2) . ? C1 C8 1.446(2) . ? C2 C7 1.402(2) . ? C2 C3 1.408(2) . ? C3 C4 1.377(2) . ? C3 H3 0.9500 . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 C7 1.377(2) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.407(2) . ? C8 C9 1.408(2) . ? C9 C10 1.378(2) . ? C9 H9 0.9500 . ? C10 C11 1.385(2) . ? C10 H10 0.9500 . ? C11 C12 1.389(2) . ? C11 H11 0.9500 . ? C12 C13 1.382(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.406(2) . ? C14 C19 1.413(2) . ? C15 C16 1.378(2) . ? C15 H15 0.9500 . ? C16 C17 1.375(3) . ? C16 H16 0.9500 . ? C17 C18 1.387(3) . ? C17 H17 0.9500 . ? C18 C19 1.370(2) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? Cl7 C20A 1.727(5) . ? Cl7 C20 1.822(4) . ? Cl8 C21 1.765(4) . ? Cl8 C21A 1.834(6) . ? C20 C21 1.474(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C20A C21A 1.490(7) . ? C20A H20C 0.9900 . ? C20A H20D 0.9900 . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? 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 B6 60.35(9) . . ? B5 B1 B4 59.98(9) . . ? B6 B1 B4 108.35(11) . . ? B5 B1 B3 108.05(11) . . ? B6 B1 B3 108.09(11) . . ? B4 B1 B3 60.05(9) . . ? B5 B1 Cl1 121.23(11) . . ? B6 B1 Cl1 121.81(10) . . ? B4 B1 Cl1 121.08(11) . . ? B3 B1 Cl1 121.75(10) . . ? B5 B1 B2 108.47(11) . . ? B6 B1 B2 60.11(9) . . ? B4 B1 B2 108.34(11) . . ? B3 B1 B2 60.05(9) . . ? Cl1 B1 B2 121.94(10) . . ? B4 B2 B6 60.05(9) 3_765 . ? B4 B2 B1 107.56(11) 3_765 . ? B6 B2 B1 59.75(9) . . ? B4 B2 B5 59.77(9) 3_765 3_765 ? B6 B2 B5 107.84(11) . 3_765 ? B1 B2 B5 107.64(11) . 3_765 ? B4 B2 B3 107.46(11) 3_765 . ? B6 B2 B3 107.71(11) . . ? B1 B2 B3 59.93(9) . . ? B5 B2 B3 59.76(9) 3_765 . ? B4 B2 Cl2 122.53(10) 3_765 . ? B6 B2 Cl2 121.29(10) . . ? B1 B2 Cl2 121.14(10) . . ? B5 B2 Cl2 122.72(11) 3_765 . ? B3 B2 Cl2 121.94(11) . . ? B5 B3 B6 60.27(9) 3_765 3_765 ? B5 B3 B4 108.25(11) 3_765 . ? B6 B3 B4 60.11(9) 3_765 . ? B5 B3 B1 107.99(11) 3_765 . ? B6 B3 B1 108.02(11) 3_765 . ? B4 B3 B1 59.86(9) . . ? B5 B3 B2 60.12(9) 3_765 . ? B6 B3 B2 108.44(11) 3_765 . ? B4 B3 B2 108.16(11) . . ? B1 B3 B2 60.02(9) . . ? B5 B3 Cl3 122.22(11) 3_765 . ? B6 B3 Cl3 120.95(10) 3_765 . ? B4 B3 Cl3 120.67(10) . . ? B1 B3 Cl3 121.77(11) . . ? B2 B3 Cl3 122.44(11) . . ? B5 B4 B1 59.96(9) . . ? B5 B4 B3 108.07(11) . . ? B1 B4 B3 60.09(9) . . ? B5 B4 B2 60.19(9) . 3_765 ? B1 B4 B2 108.13(11) . 3_765 ? B3 B4 B2 108.00(11) . 3_765 ? B5 B4 B6 108.15(11) . 3_765 ? B1 B4 B6 108.04(11) . 3_765 ? B3 B4 B6 59.90(9) . 3_765 ? B2 B4 B6 60.02(9) 3_765 3_765 ? B5 B4 Cl4 121.42(11) . . ? B1 B4 Cl4 120.12(11) . . ? B3 B4 Cl4 120.95(11) . . ? B2 B4 Cl4 123.07(11) 3_765 . ? B6 B4 Cl4 122.77(11) 3_765 . ? B1 B5 B4 60.05(9) . . ? B1 B5 B3 107.72(11) . 3_765 ? B4 B5 B3 107.97(11) . 3_765 ? B1 B5 B2 108.09(11) . 3_765 ? B4 B5 B2 60.04(9) . 3_765 ? B3 B5 B2 60.13(9) 3_765 3_765 ? B1 B5 B6 59.83(9) . . ? B4 B5 B6 107.99(11) . . ? B3 B5 B6 59.93(9) 3_765 . ? B2 B5 B6 108.18(11) 3_765 . ? B1 B5 Cl5 121.53(11) . . ? B4 B5 Cl5 121.22(11) . . ? B3 B5 Cl5 122.31(11) 3_765 . ? B2 B5 Cl5 121.55(11) 3_765 . ? B6 B5 Cl5 122.01(11) . . ? B1 B6 B3 107.62(11) . 3_765 ? B1 B6 B2 60.15(9) . . ? B3 B6 B2 108.00(11) 3_765 . ? B1 B6 B4 107.79(11) . 3_765 ? B3 B6 B4 59.99(9) 3_765 3_765 ? B2 B6 B4 59.94(9) . 3_765 ? B1 B6 B5 59.82(9) . . ? B3 B6 B5 59.81(9) 3_765 . ? B2 B6 B5 108.07(11) . . ? B4 B6 B5 107.79(11) 3_765 . ? B1 B6 Cl6 121.67(11) . . ? B3 B6 Cl6 122.19(11) 3_765 . ? B2 B6 Cl6 121.29(11) . . ? B4 B6 Cl6 121.89(11) 3_765 . ? B5 B6 Cl6 121.97(11) . . ? C14 C1 C2 120.34(13) . . ? C14 C1 C8 120.37(14) . . ? C2 C1 C8 119.25(13) . . ? C7 C2 C3 118.73(14) . . ? C7 C2 C1 121.79(14) . . ? C3 C2 C1 119.46(14) . . ? C4 C3 C2 120.59(15) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.66(16) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 120.66(16) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 120.11(16) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C2 120.11(15) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? C13 C8 C9 119.18(14) . . ? C13 C8 C1 121.04(14) . . ? C9 C8 C1 119.77(14) . . ? C10 C9 C8 120.13(15) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.05(15) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 120.61(15) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 120.03(15) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 119.94(15) . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C15 C14 C19 118.55(15) . . ? C15 C14 C1 120.31(14) . . ? C19 C14 C1 121.14(14) . . ? C16 C15 C14 120.17(16) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.38(17) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.41(16) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 120.29(17) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C14 120.16(16) . . ? C18 C19 H19 119.9 . . ? C14 C19 H19 119.9 . . ? C21 C20 Cl7 109.0(3) . . ? C21 C20 H20A 109.9 . . ? Cl7 C20 H20A 109.9 . . ? C21 C20 H20B 109.9 . . ? Cl7 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? C20 C21 Cl8 107.3(3) . . ? C20 C21 H21A 110.2 . . ? Cl8 C21 H21A 110.2 . . ? C20 C21 H21B 110.2 . . ? Cl8 C21 H21B 110.2 . . ? H21A C21 H21B 108.5 . . ? C21A C20A Cl7 109.3(3) . . ? C21A C20A H20C 109.8 . . ? Cl7 C20A H20C 109.8 . . ? C21A C20A H20D 109.8 . . ? Cl7 C20A H20D 109.8 . . ? H20C C20A H20D 108.3 . . ? C20A C21A Cl8 108.7(4) . . ? C20A C21A H21C 110.0 . . ? Cl8 C21A H21C 110.0 . . ? C20A C21A H21D 110.0 . . ? Cl8 C21A H21D 110.0 . . ? H21C C21A H21D 108.3 . . ? 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 B5 B1 B2 B4 -0.25(15) . . . 3_765 ? B6 B1 B2 B4 -37.73(11) . . . 3_765 ? B4 B1 B2 B4 63.33(15) . . . 3_765 ? B3 B1 B2 B4 100.39(12) . . . 3_765 ? Cl1 B1 B2 B4 -148.72(11) . . . 3_765 ? B5 B1 B2 B6 37.49(11) . . . . ? B4 B1 B2 B6 101.07(12) . . . . ? B3 B1 B2 B6 138.13(12) . . . . ? Cl1 B1 B2 B6 -110.98(13) . . . . ? B5 B1 B2 B5 -63.28(15) . . . 3_765 ? B6 B1 B2 B5 -100.76(12) . . . 3_765 ? B4 B1 B2 B5 0.30(15) . . . 3_765 ? B3 B1 B2 B5 37.36(11) . . . 3_765 ? Cl1 B1 B2 B5 148.25(11) . . . 3_765 ? B5 B1 B2 B3 -100.64(12) . . . . ? B6 B1 B2 B3 -138.13(12) . . . . ? B4 B1 B2 B3 -37.06(11) . . . . ? Cl1 B1 B2 B3 110.89(13) . . . . ? B5 B1 B2 Cl2 147.99(11) . . . . ? B6 B1 B2 Cl2 110.50(13) . . . . ? B4 B1 B2 Cl2 -148.43(11) . . . . ? B3 B1 B2 Cl2 -111.38(13) . . . . ? Cl1 B1 B2 Cl2 -0.48(18) . . . . ? B5 B1 B3 B5 63.74(15) . . . 3_765 ? B6 B1 B3 B5 -0.10(15) . . . 3_765 ? B4 B1 B3 B5 101.08(12) . . . 3_765 ? Cl1 B1 B3 B5 -148.79(11) . . . 3_765 ? B2 B1 B3 B5 -37.61(11) . . . 3_765 ? B5 B1 B3 B6 0.02(15) . . . 3_765 ? B6 B1 B3 B6 -63.82(15) . . . 3_765 ? B4 B1 B3 B6 37.36(11) . . . 3_765 ? Cl1 B1 B3 B6 147.48(11) . . . 3_765 ? B2 B1 B3 B6 -101.33(12) . . . 3_765 ? B5 B1 B3 B4 -37.34(11) . . . . ? B6 B1 B3 B4 -101.18(12) . . . . ? Cl1 B1 B3 B4 110.12(13) . . . . ? B2 B1 B3 B4 -138.69(12) . . . . ? B5 B1 B3 B2 101.35(12) . . . . ? B6 B1 B3 B2 37.50(11) . . . . ? B4 B1 B3 B2 138.69(12) . . . . ? Cl1 B1 B3 B2 -111.19(13) . . . . ? B5 B1 B3 Cl3 -146.87(11) . . . . ? B6 B1 B3 Cl3 149.29(11) . . . . ? B4 B1 B3 Cl3 -109.52(13) . . . . ? Cl1 B1 B3 Cl3 0.60(18) . . . . ? B2 B1 B3 Cl3 111.79(13) . . . . ? B4 B2 B3 B5 37.41(11) 3_765 . . 3_765 ? B6 B2 B3 B5 100.73(12) . . . 3_765 ? B1 B2 B3 B5 137.98(12) . . . 3_765 ? Cl2 B2 B3 B5 -111.96(13) . . . 3_765 ? B4 B2 B3 B6 0.04(15) 3_765 . . 3_765 ? B6 B2 B3 B6 63.36(15) . . . 3_765 ? B1 B2 B3 B6 100.60(12) . . . 3_765 ? B5 B2 B3 B6 -37.38(11) 3_765 . . 3_765 ? Cl2 B2 B3 B6 -149.33(11) . . . 3_765 ? B4 B2 B3 B4 -63.64(15) 3_765 . . . ? B6 B2 B3 B4 -0.32(15) . . . . ? B1 B2 B3 B4 36.93(11) . . . . ? B5 B2 B3 B4 -101.05(12) 3_765 . . . ? Cl2 B2 B3 B4 146.99(11) . . . . ? B4 B2 B3 B1 -100.57(12) 3_765 . . . ? B6 B2 B3 B1 -37.25(11) . . . . ? B5 B2 B3 B1 -137.98(12) 3_765 . . . ? Cl2 B2 B3 B1 110.07(13) . . . . ? B4 B2 B3 Cl3 148.73(11) 3_765 . . . ? B6 B2 B3 Cl3 -147.96(11) . . . . ? B1 B2 B3 Cl3 -110.71(13) . . . . ? B5 B2 B3 Cl3 111.31(13) 3_765 . . . ? Cl2 B2 B3 Cl3 -0.64(18) . . . . ? B6 B1 B4 B5 -37.49(11) . . . . ? B3 B1 B4 B5 -138.24(12) . . . . ? Cl1 B1 B4 B5 110.55(13) . . . . ? B2 B1 B4 B5 -101.18(12) . . . . ? B5 B1 B4 B3 138.24(12) . . . . ? B6 B1 B4 B3 100.75(12) . . . . ? Cl1 B1 B4 B3 -111.22(13) . . . . ? B2 B1 B4 B3 37.06(11) . . . . ? B5 B1 B4 B2 37.48(11) . . . 3_765 ? B6 B1 B4 B2 -0.01(15) . . . 3_765 ? B3 B1 B4 B2 -100.76(12) . . . 3_765 ? Cl1 B1 B4 B2 148.02(11) . . . 3_765 ? B2 B1 B4 B2 -63.70(15) . . . 3_765 ? B5 B1 B4 B6 100.96(12) . . . 3_765 ? B6 B1 B4 B6 63.48(15) . . . 3_765 ? B3 B1 B4 B6 -37.27(11) . . . 3_765 ? Cl1 B1 B4 B6 -148.49(11) . . . 3_765 ? B2 B1 B4 B6 -0.21(15) . . . 3_765 ? B5 B1 B4 Cl4 -111.14(13) . . . . ? B6 B1 B4 Cl4 -148.63(11) . . . . ? B3 B1 B4 Cl4 110.62(13) . . . . ? Cl1 B1 B4 Cl4 -0.60(18) . . . . ? B2 B1 B4 Cl4 147.68(11) . . . . ? B5 B3 B4 B5 -63.30(15) 3_765 . . . ? B6 B3 B4 B5 -100.93(12) 3_765 . . . ? B1 B3 B4 B5 37.34(11) . . . . ? B2 B3 B4 B5 0.34(15) . . . . ? Cl3 B3 B4 B5 148.66(11) . . . . ? B5 B3 B4 B1 -100.64(12) 3_765 . . . ? B6 B3 B4 B1 -138.27(12) 3_765 . . . ? B2 B3 B4 B1 -37.00(11) . . . . ? Cl3 B3 B4 B1 111.32(13) . . . . ? B5 B3 B4 B2 0.35(15) 3_765 . . 3_765 ? B6 B3 B4 B2 -37.29(10) 3_765 . . 3_765 ? B1 B3 B4 B2 100.99(12) . . . 3_765 ? B2 B3 B4 B2 63.99(15) . . . 3_765 ? Cl3 B3 B4 B2 -147.69(11) . . . 3_765 ? B5 B3 B4 B6 37.63(11) 3_765 . . 3_765 ? B1 B3 B4 B6 138.27(12) . . . 3_765 ? B2 B3 B4 B6 101.27(12) . . . 3_765 ? Cl3 B3 B4 B6 -110.41(13) . . . 3_765 ? B5 B3 B4 Cl4 150.09(11) 3_765 . . . ? B6 B3 B4 Cl4 112.46(13) 3_765 . . . ? B1 B3 B4 Cl4 -109.27(13) . . . . ? B2 B3 B4 Cl4 -146.27(11) . . . . ? Cl3 B3 B4 Cl4 2.05(18) . . . . ? B6 B1 B5 B4 138.35(12) . . . . ? B3 B1 B5 B4 37.37(11) . . . . ? Cl1 B1 B5 B4 -110.30(13) . . . . ? B2 B1 B5 B4 100.97(12) . . . . ? B6 B1 B5 B3 37.41(11) . . . 3_765 ? B4 B1 B5 B3 -100.93(12) . . . 3_765 ? B3 B1 B5 B3 -63.56(15) . . . 3_765 ? Cl1 B1 B5 B3 148.77(11) . . . 3_765 ? B2 B1 B5 B3 0.03(15) . . . 3_765 ? B6 B1 B5 B2 100.95(12) . . . 3_765 ? B4 B1 B5 B2 -37.40(11) . . . 3_765 ? B3 B1 B5 B2 -0.03(15) . . . 3_765 ? Cl1 B1 B5 B2 -147.70(11) . . . 3_765 ? B2 B1 B5 B2 63.57(15) . . . 3_765 ? B4 B1 B5 B6 -138.35(12) . . . . ? B3 B1 B5 B6 -100.97(12) . . . . ? Cl1 B1 B5 B6 111.36(13) . . . . ? B2 B1 B5 B6 -37.38(11) . . . . ? B6 B1 B5 Cl5 -111.26(13) . . . . ? B4 B1 B5 Cl5 110.39(13) . . . . ? B3 B1 B5 Cl5 147.76(11) . . . . ? Cl1 B1 B5 Cl5 0.10(18) . . . . ? B2 B1 B5 Cl5 -148.64(11) . . . . ? B3 B4 B5 B1 -37.39(11) . . . . ? B2 B4 B5 B1 -138.21(12) 3_765 . . . ? B6 B4 B5 B1 -100.77(12) 3_765 . . . ? Cl4 B4 B5 B1 109.03(13) . . . . ? B1 B4 B5 B3 100.51(12) . . . 3_765 ? B3 B4 B5 B3 63.12(15) . . . 3_765 ? B2 B4 B5 B3 -37.70(11) 3_765 . . 3_765 ? B6 B4 B5 B3 -0.26(15) 3_765 . . 3_765 ? Cl4 B4 B5 B3 -150.46(11) . . . 3_765 ? B1 B4 B5 B2 138.21(12) . . . 3_765 ? B3 B4 B5 B2 100.82(12) . . . 3_765 ? B6 B4 B5 B2 37.44(11) 3_765 . . 3_765 ? Cl4 B4 B5 B2 -112.76(13) . . . 3_765 ? B1 B4 B5 B6 37.17(11) . . . . ? B3 B4 B5 B6 -0.23(15) . . . . ? B2 B4 B5 B6 -101.04(12) 3_765 . . . ? B6 B4 B5 B6 -63.60(15) 3_765 . . . ? Cl4 B4 B5 B6 146.19(11) . . . . ? B1 B4 B5 Cl5 -110.88(13) . . . . ? B3 B4 B5 Cl5 -148.27(11) . . . . ? B2 B4 B5 Cl5 110.91(13) 3_765 . . . ? B6 B4 B5 Cl5 148.35(11) 3_765 . . . ? Cl4 B4 B5 Cl5 -1.85(18) . . . . ? B5 B1 B6 B3 -37.34(11) . . . 3_765 ? B4 B1 B6 B3 -0.01(15) . . . 3_765 ? B3 B1 B6 B3 63.57(15) . . . 3_765 ? Cl1 B1 B6 B3 -147.76(11) . . . 3_765 ? B2 B1 B6 B3 101.05(12) . . . 3_765 ? B5 B1 B6 B2 -138.38(12) . . . . ? B4 B1 B6 B2 -101.06(12) . . . . ? B3 B1 B6 B2 -37.48(11) . . . . ? Cl1 B1 B6 B2 111.19(13) . . . . ? B5 B1 B6 B4 -100.64(12) . . . 3_765 ? B4 B1 B6 B4 -63.32(15) . . . 3_765 ? B3 B1 B6 B4 0.26(15) . . . 3_765 ? Cl1 B1 B6 B4 148.93(11) . . . 3_765 ? B2 B1 B6 B4 37.74(11) . . . 3_765 ? B4 B1 B6 B5 37.32(11) . . . . ? B3 B1 B6 B5 100.90(12) . . . . ? Cl1 B1 B6 B5 -110.43(13) . . . . ? B2 B1 B6 B5 138.38(12) . . . . ? B5 B1 B6 Cl6 111.16(13) . . . . ? B4 B1 B6 Cl6 148.49(11) . . . . ? B3 B1 B6 Cl6 -147.94(11) . . . . ? Cl1 B1 B6 Cl6 0.73(18) . . . . ? B2 B1 B6 Cl6 -110.46(13) . . . . ? B4 B2 B6 B1 137.67(11) 3_765 . . . ? B5 B2 B6 B1 100.41(12) 3_765 . . . ? B3 B2 B6 B1 37.33(11) . . . . ? Cl2 B2 B6 B1 -110.24(13) . . . . ? B4 B2 B6 B3 37.27(11) 3_765 . . 3_765 ? B1 B2 B6 B3 -100.40(12) . . . 3_765 ? B5 B2 B6 B3 0.02(15) 3_765 . . 3_765 ? B3 B2 B6 B3 -63.07(15) . . . 3_765 ? Cl2 B2 B6 B3 149.36(11) . . . 3_765 ? B1 B2 B6 B4 -137.67(11) . . . 3_765 ? B5 B2 B6 B4 -37.25(11) 3_765 . . 3_765 ? B3 B2 B6 B4 -100.34(12) . . . 3_765 ? Cl2 B2 B6 B4 112.09(13) . . . 3_765 ? B4 B2 B6 B5 100.52(12) 3_765 . . . ? B1 B2 B6 B5 -37.15(11) . . . . ? B5 B2 B6 B5 63.26(15) 3_765 . . . ? B3 B2 B6 B5 0.18(15) . . . . ? Cl2 B2 B6 B5 -147.39(11) . . . . ? B4 B2 B6 Cl6 -111.26(13) 3_765 . . . ? B1 B2 B6 Cl6 111.07(13) . . . . ? B5 B2 B6 Cl6 -148.51(11) 3_765 . . . ? B3 B2 B6 Cl6 148.40(11) . . . . ? Cl2 B2 B6 Cl6 0.83(18) . . . . ? B4 B5 B6 B1 -37.26(11) . . . . ? B3 B5 B6 B1 -138.03(12) 3_765 . . . ? B2 B5 B6 B1 -100.78(12) 3_765 . . . ? Cl5 B5 B6 B1 110.48(13) . . . . ? B1 B5 B6 B3 138.03(12) . . . 3_765 ? B4 B5 B6 B3 100.76(12) . . . 3_765 ? B2 B5 B6 B3 37.25(11) 3_765 . . 3_765 ? Cl5 B5 B6 B3 -111.49(13) . . . 3_765 ? B1 B5 B6 B2 37.30(11) . . . . ? B4 B5 B6 B2 0.03(15) . . . . ? B3 B5 B6 B2 -100.73(12) 3_765 . . . ? B2 B5 B6 B2 -63.48(15) 3_765 . . . ? Cl5 B5 B6 B2 147.78(11) . . . . ? B1 B5 B6 B4 100.63(12) . . . 3_765 ? B4 B5 B6 B4 63.37(15) . . . 3_765 ? B3 B5 B6 B4 -37.39(11) 3_765 . . 3_765 ? B2 B5 B6 B4 -0.14(15) 3_765 . . 3_765 ? Cl5 B5 B6 B4 -148.89(11) . . . 3_765 ? B1 B5 B6 Cl6 -110.66(13) . . . . ? B4 B5 B6 Cl6 -147.93(11) . . . . ? B3 B5 B6 Cl6 111.31(13) 3_765 . . . ? B2 B5 B6 Cl6 148.56(11) 3_765 . . . ? Cl5 B5 B6 Cl6 -0.18(18) . . . . ? C14 C1 C2 C7 34.3(2) . . . . ? C8 C1 C2 C7 -147.90(15) . . . . ? C14 C1 C2 C3 -144.16(15) . . . . ? C8 C1 C2 C3 33.7(2) . . . . ? C7 C2 C3 C4 -3.8(2) . . . . ? C1 C2 C3 C4 174.73(15) . . . . ? C2 C3 C4 C5 2.6(3) . . . . ? C3 C4 C5 C6 0.8(3) . . . . ? C4 C5 C6 C7 -3.0(3) . . . . ? C5 C6 C7 C2 1.7(3) . . . . ? C3 C2 C7 C6 1.6(2) . . . . ? C1 C2 C7 C6 -176.88(15) . . . . ? C14 C1 C8 C13 36.7(2) . . . . ? C2 C1 C8 C13 -141.08(15) . . . . ? C14 C1 C8 C9 -144.19(15) . . . . ? C2 C1 C8 C9 38.0(2) . . . . ? C13 C8 C9 C10 -0.1(2) . . . . ? C1 C8 C9 C10 -179.18(14) . . . . ? C8 C9 C10 C11 2.1(2) . . . . ? C9 C10 C11 C12 -2.3(3) . . . . ? C10 C11 C12 C13 0.4(3) . . . . ? C11 C12 C13 C8 1.6(2) . . . . ? C9 C8 C13 C12 -1.8(2) . . . . ? C1 C8 C13 C12 177.31(15) . . . . ? C2 C1 C14 C15 -151.09(15) . . . . ? C8 C1 C14 C15 31.1(2) . . . . ? C2 C1 C14 C19 28.9(2) . . . . ? C8 C1 C14 C19 -148.87(16) . . . . ? C19 C14 C15 C16 -0.9(2) . . . . ? C1 C14 C15 C16 179.09(15) . . . . ? C14 C15 C16 C17 1.8(3) . . . . ? C15 C16 C17 C18 -0.9(3) . . . . ? C16 C17 C18 C19 -0.8(3) . . . . ? C17 C18 C19 C14 1.7(3) . . . . ? C15 C14 C19 C18 -0.8(3) . . . . ? C1 C14 C19 C18 179.20(17) . . . . ? C20A Cl7 C20 C21 4.4(3) . . . . ? Cl7 C20 C21 Cl8 179.80(17) . . . . ? C21A Cl8 C21 C20 -0.4(4) . . . . ? C20 Cl7 C20A C21A -1.1(4) . . . . ? Cl7 C20A C21A Cl8 -177.3(3) . . . . ? C21 Cl8 C21A C20A 3.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.57 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.419 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.059 #===END data_ck001 _database_code_depnum_ccdc_archive 'CCDC 710775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C19 H15), (B12 Cl12), 2(O2 S)' _chemical_formula_sum 'C38 H30 B12 Cl12 O4 S2' _chemical_formula_weight 1169.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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' '-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 16.205(3) _cell_length_b 16.617(3) _cell_length_c 19.010(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.60(3) _cell_angle_gamma 90.00 _cell_volume 4995.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(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 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 0.790 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.688 _exptl_absorpt_correction_T_max 0.851 _exptl_absorpt_process_details ; March 2001 T Higashi ; _exptl_special_details ; ???? ; _diffrn_ambient_temperature 173(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_measurement_details ; scan: Number of images: 90 Slice: 20.0000 - 200.0000 Image width: 2.0000 Exp time: 138.0000 Rotation axis: Omega Omega: 0.0000 Chi: 15.0000 Phi: 0.0000 XTD: 127.4000 2theta: 0.0000 scan: Number of images: 54 Slice: 74.0000 - 182.0000 Image width: 2.0000 Exp time: 138.0000 Rotation axis: Omega Omega: 0.0000 Chi: 15.0000 Phi: 180.0000 XTD: 127.4000 2theta: 0.0000 scan: Number of images: 22 Slice: 108.0000 - 152.0000 Image width: 2.0000 Exp time: 138.0000 Rotation axis: Omega Omega: 0.0000 Chi: 15.0000 Phi: 90.0000 XTD: 127.4000 2theta: 0.0000 scan: Number of images: 15 Slice: 30.0000 - 60.0000 Image width: 2.0000 Exp time: 138.0000 Rotation axis: Omega Omega: 0.0000 Chi: 0.0000 Phi: 270.0000 XTD: 127.4000 2theta: 0.0000 scan: Number of images: 15 Slice: 40.0000 - 70.0000 Image width: 2.0000 Exp time: 138.0000 Rotation axis: Omega Omega: 0.0000 Chi: 15.0000 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 43480 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _reflns_number_total 5725 _reflns_number_gt 4697 _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^)+(0.0457P)^2^+5.5202P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5725 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Cl1 Cl 0.03174(3) 0.25389(3) 0.48861(3) 0.02375(11) Uani 1 1 d . . . B1 B 0.14399(13) 0.25234(12) 0.49453(12) 0.0183(4) Uani 1 1 d . . . Cl2 Cl 0.12394(3) 0.14093(3) 0.35938(2) 0.02464(12) Uani 1 1 d . . . B2 B 0.18898(13) 0.19688(12) 0.43162(11) 0.0183(4) Uani 1 1 d . . . Cl3 Cl 0.13127(3) 0.36226(3) 0.35861(3) 0.02572(12) Uani 1 1 d . . . B3 B 0.19171(13) 0.30434(12) 0.43100(11) 0.0187(4) Uani 1 1 d . . . Cl4 Cl 0.16792(3) 0.43192(3) 0.54586(3) 0.02641(12) Uani 1 1 d . . . B4 B 0.20968(13) 0.33824(12) 0.52241(12) 0.0186(4) Uani 1 1 d . . . Cl5 Cl 0.18392(3) 0.25348(3) 0.66331(2) 0.02257(11) Uani 1 1 d . . . B5 B 0.21770(13) 0.25182(12) 0.57931(12) 0.0181(4) Uani 1 1 d . . . Cl6 Cl 0.15671(3) 0.07434(3) 0.54859(3) 0.02400(11) Uani 1 1 d . . . B6 B 0.20490(13) 0.16469(12) 0.52312(11) 0.0182(4) Uani 1 1 d . . . C1 C 0.76211(12) 0.16396(12) 0.33447(10) 0.0199(4) Uani 1 1 d . . . C2 C 0.67757(12) 0.15196(12) 0.34562(10) 0.0207(4) Uani 1 1 d . . . C3 C 0.61817(13) 0.21529(12) 0.33300(11) 0.0244(4) Uani 1 1 d . . . H3 H 0.6337 0.2662 0.3173 0.0281(15) Uiso 1 1 calc R . . C4 C 0.53728(13) 0.20319(13) 0.34351(11) 0.0284(4) Uani 1 1 d . . . H4 H 0.4971 0.2456 0.3341 0.0281(15) Uiso 1 1 calc R . . C5 C 0.51459(13) 0.12920(13) 0.36777(12) 0.0298(5) Uani 1 1 d . . . H5 H 0.4588 0.1213 0.3745 0.0281(15) Uiso 1 1 calc R . . C6 C 0.57258(13) 0.06705(13) 0.38211(12) 0.0298(5) Uani 1 1 d . . . H6 H 0.5569 0.0171 0.3998 0.0281(15) Uiso 1 1 calc R . . C7 C 0.65387(13) 0.07746(12) 0.37067(11) 0.0246(4) Uani 1 1 d . . . H7 H 0.6933 0.0344 0.3797 0.0281(15) Uiso 1 1 calc R . . C8 C 0.80597(12) 0.09790(11) 0.31025(10) 0.0196(4) Uani 1 1 d . . . C9 C 0.76086(13) 0.03684(12) 0.26597(11) 0.0252(4) Uani 1 1 d . . . H9 H 0.7013 0.0411 0.2496 0.0281(15) Uiso 1 1 calc R . . C10 C 0.80307(13) -0.02874(13) 0.24652(11) 0.0279(4) Uani 1 1 d . . . H10 H 0.7726 -0.0695 0.2167 0.0281(15) Uiso 1 1 calc R . . C11 C 0.88946(13) -0.03515(12) 0.27042(11) 0.0263(4) Uani 1 1 d . . . H11 H 0.9181 -0.0812 0.2580 0.0281(15) Uiso 1 1 calc R . . C12 C 0.93502(13) 0.02503(12) 0.31242(11) 0.0238(4) Uani 1 1 d . . . H12 H 0.9947 0.0204 0.3277 0.0281(15) Uiso 1 1 calc R . . C13 C 0.89461(12) 0.09123(11) 0.33213(10) 0.0208(4) Uani 1 1 d . . . H13 H 0.9263 0.1325 0.3604 0.0281(15) Uiso 1 1 calc R . . C14 C 0.80297(12) 0.24118(11) 0.35012(10) 0.0208(4) Uani 1 1 d . . . C15 C 0.86161(12) 0.26920(12) 0.31084(11) 0.0225(4) Uani 1 1 d . . . H15 H 0.8733 0.2382 0.2722 0.0281(15) Uiso 1 1 calc R . . C16 C 0.90210(12) 0.34200(12) 0.32875(11) 0.0253(4) Uani 1 1 d . . . H16 H 0.9408 0.3614 0.3017 0.0281(15) Uiso 1 1 calc R . . C17 C 0.88653(13) 0.38669(12) 0.38594(12) 0.0280(4) Uani 1 1 d . . . H17 H 0.9159 0.4359 0.3987 0.0281(15) Uiso 1 1 calc R . . C18 C 0.82841(13) 0.36036(12) 0.42491(11) 0.0274(4) Uani 1 1 d . . . H18 H 0.8179 0.3916 0.4639 0.0281(15) Uiso 1 1 calc R . . C19 C 0.78614(12) 0.28888(12) 0.40694(10) 0.0235(4) Uani 1 1 d . . . H19 H 0.7454 0.2715 0.4329 0.0281(15) Uiso 1 1 calc R . . S1 S 0.91700(4) 0.09615(3) 0.54064(3) 0.03374(14) Uani 1 1 d . . . O1 O 0.84540(11) 0.13146(10) 0.49454(9) 0.0381(4) Uani 1 1 d . . . O2 O 0.92581(13) 0.10680(11) 0.61620(9) 0.0498(5) 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 Cl1 0.0167(2) 0.0297(2) 0.0259(2) -0.00031(19) 0.00693(18) -0.00054(18) B1 0.0162(9) 0.0195(10) 0.0205(10) -0.0013(8) 0.0066(8) -0.0016(8) Cl2 0.0235(2) 0.0282(2) 0.0223(2) -0.00723(18) 0.00517(19) -0.00808(19) B2 0.0174(10) 0.0190(10) 0.0192(10) -0.0047(8) 0.0059(8) -0.0033(8) Cl3 0.0236(2) 0.0282(2) 0.0253(2) 0.00367(19) 0.00521(19) 0.00258(19) B3 0.0172(10) 0.0197(10) 0.0198(10) 0.0010(8) 0.0056(8) -0.0002(8) Cl4 0.0304(3) 0.0191(2) 0.0329(3) -0.00315(18) 0.0138(2) 0.00285(18) B4 0.0198(10) 0.0148(9) 0.0229(10) -0.0030(8) 0.0086(8) 0.0001(8) Cl5 0.0205(2) 0.0295(2) 0.0198(2) -0.00214(18) 0.00897(18) -0.00086(18) B5 0.0164(9) 0.0197(10) 0.0195(10) -0.0012(8) 0.0068(8) -0.0007(8) Cl6 0.0267(2) 0.0192(2) 0.0281(2) 0.00150(18) 0.0103(2) -0.00484(18) B6 0.0176(10) 0.0165(9) 0.0219(10) -0.0021(8) 0.0069(8) -0.0030(8) C1 0.0187(9) 0.0251(9) 0.0156(9) 0.0015(7) 0.0031(7) 0.0001(7) C2 0.0185(9) 0.0260(9) 0.0187(9) -0.0023(7) 0.0060(7) -0.0011(8) C3 0.0236(10) 0.0260(10) 0.0245(10) 0.0009(8) 0.0069(8) 0.0006(8) C4 0.0220(10) 0.0326(11) 0.0322(11) -0.0021(9) 0.0092(9) 0.0055(8) C5 0.0207(10) 0.0380(12) 0.0341(11) -0.0039(9) 0.0134(9) -0.0015(9) C6 0.0265(11) 0.0291(11) 0.0374(12) -0.0003(9) 0.0144(9) -0.0042(9) C7 0.0220(10) 0.0253(10) 0.0285(10) -0.0005(8) 0.0096(8) 0.0001(8) C8 0.0209(9) 0.0208(9) 0.0190(9) 0.0006(7) 0.0083(7) -0.0010(7) C9 0.0206(10) 0.0283(10) 0.0274(10) -0.0029(8) 0.0068(8) -0.0027(8) C10 0.0286(11) 0.0268(10) 0.0297(11) -0.0085(8) 0.0094(9) -0.0062(8) C11 0.0304(11) 0.0231(10) 0.0289(10) -0.0042(8) 0.0144(9) 0.0013(8) C12 0.0208(9) 0.0256(10) 0.0271(10) 0.0009(8) 0.0096(8) 0.0011(8) C13 0.0202(9) 0.0224(9) 0.0211(9) -0.0003(7) 0.0072(7) -0.0024(7) C14 0.0182(9) 0.0243(10) 0.0198(9) 0.0013(7) 0.0037(7) 0.0026(7) C15 0.0200(9) 0.0254(9) 0.0228(10) -0.0002(8) 0.0062(8) 0.0009(8) C16 0.0189(9) 0.0282(10) 0.0289(10) 0.0037(8) 0.0052(8) -0.0010(8) C17 0.0233(10) 0.0227(10) 0.0363(12) -0.0024(9) 0.0030(9) -0.0016(8) C18 0.0278(11) 0.0257(10) 0.0281(11) -0.0056(8) 0.0052(9) 0.0035(8) C19 0.0230(10) 0.0254(10) 0.0229(10) 0.0001(8) 0.0068(8) 0.0043(8) S1 0.0365(3) 0.0308(3) 0.0349(3) -0.0025(2) 0.0101(2) 0.0047(2) O1 0.0410(9) 0.0393(9) 0.0338(8) 0.0036(7) 0.0080(7) 0.0041(7) O2 0.0691(13) 0.0439(10) 0.0340(9) 0.0041(8) 0.0061(9) 0.0165(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 B1 1.798(2) . ? B1 B6 1.777(3) . ? B1 B5 1.785(3) . ? B1 B2 1.786(3) . ? B1 B4 1.790(3) . ? B1 B3 1.792(3) . ? Cl2 B2 1.797(2) . ? B2 B4 1.782(3) 7_556 ? B2 B6 1.784(3) . ? B2 B3 1.786(3) . ? B2 B5 1.787(3) 7_556 ? Cl3 B3 1.786(2) . ? B3 B5 1.786(3) 7_556 ? B3 B6 1.787(3) 7_556 ? B3 B4 1.789(3) . ? Cl4 B4 1.792(2) . ? B4 B5 1.785(3) . ? B4 B6 1.786(3) 7_556 ? Cl5 B5 1.798(2) . ? B5 B6 1.784(3) . ? Cl6 B6 1.806(2) . ? C1 C8 1.437(3) . ? C1 C14 1.445(3) . ? C1 C2 1.445(3) . ? C2 C7 1.410(3) . ? C2 C3 1.411(3) . ? C3 C4 1.383(3) . ? C3 H3 0.9500 . ? C4 C5 1.390(3) . ? C4 H4 0.9500 . ? C5 C6 1.383(3) . ? C5 H5 0.9500 . ? C6 C7 1.392(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.410(3) . ? C8 C9 1.416(3) . ? C9 C10 1.379(3) . ? C9 H9 0.9500 . ? C10 C11 1.378(3) . ? C10 H10 0.9500 . ? C11 C12 1.388(3) . ? C11 H11 0.9500 . ? C12 C13 1.374(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.410(3) . ? C14 C19 1.414(3) . ? C15 C16 1.383(3) . ? C15 H15 0.9500 . ? C16 C17 1.385(3) . ? C16 H16 0.9500 . ? C17 C18 1.390(3) . ? C17 H17 0.9500 . ? C18 C19 1.377(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? S1 O1 1.4196(17) . ? S1 O2 1.4230(18) . ? 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 60.14(12) . . ? B6 B1 B2 60.08(12) . . ? B5 B1 B2 108.15(15) . . ? B6 B1 B4 107.95(15) . . ? B5 B1 B4 59.92(12) . . ? B2 B1 B4 107.84(14) . . ? B6 B1 B3 107.99(15) . . ? B5 B1 B3 107.98(14) . . ? B2 B1 B3 59.89(12) . . ? B4 B1 B3 59.93(12) . . ? B6 B1 Cl1 121.19(13) . . ? B5 B1 Cl1 121.69(14) . . ? B2 B1 Cl1 121.37(14) . . ? B4 B1 Cl1 122.35(13) . . ? B3 B1 Cl1 122.03(14) . . ? B4 B2 B6 60.12(12) 7_556 . ? B4 B2 B3 108.01(14) 7_556 . ? B6 B2 B3 107.92(14) . . ? B4 B2 B1 107.92(15) 7_556 . ? B6 B2 B1 59.69(12) . . ? B3 B2 B1 60.20(11) . . ? B4 B2 B5 60.03(12) 7_556 7_556 ? B6 B2 B5 108.08(15) . 7_556 ? B3 B2 B5 59.97(11) . 7_556 ? B1 B2 B5 108.13(14) . 7_556 ? B4 B2 Cl2 121.96(13) 7_556 . ? B6 B2 Cl2 121.73(13) . . ? B3 B2 Cl2 121.56(14) . . ? B1 B2 Cl2 121.43(14) . . ? B5 B2 Cl2 121.87(14) 7_556 . ? B5 B3 B2 60.04(12) 7_556 . ? B5 B3 Cl3 121.51(14) 7_556 . ? B2 B3 Cl3 122.24(14) . . ? B5 B3 B6 59.91(12) 7_556 7_556 ? B2 B3 B6 107.85(14) . 7_556 ? Cl3 B3 B6 121.25(14) . 7_556 ? B5 B3 B4 107.92(15) 7_556 . ? B2 B3 B4 107.90(14) . . ? Cl3 B3 B4 121.62(14) . . ? B6 B3 B4 59.92(12) 7_556 . ? B5 B3 B1 107.93(14) 7_556 . ? B2 B3 B1 59.90(11) . . ? Cl3 B3 B1 122.29(14) . . ? B6 B3 B1 107.84(15) 7_556 . ? B4 B3 B1 60.00(12) . . ? B2 B4 B5 60.13(12) 7_556 . ? B2 B4 B6 59.99(12) 7_556 7_556 ? B5 B4 B6 108.05(14) . 7_556 ? B2 B4 B3 108.09(14) 7_556 . ? B5 B4 B3 108.06(14) . . ? B6 B4 B3 59.99(12) 7_556 . ? B2 B4 B1 107.99(14) 7_556 . ? B5 B4 B1 59.87(12) . . ? B6 B4 B1 107.96(14) 7_556 . ? B3 B4 B1 60.08(12) . . ? B2 B4 Cl4 121.35(13) 7_556 . ? B5 B4 Cl4 121.98(14) . . ? B6 B4 Cl4 121.25(13) 7_556 . ? B3 B4 Cl4 121.65(14) . . ? B1 B4 Cl4 122.26(14) . . ? B6 B5 B1 59.72(12) . . ? B6 B5 B4 107.84(15) . . ? B1 B5 B4 60.20(12) . . ? B6 B5 B3 60.08(12) . 7_556 ? B1 B5 B3 107.92(15) . 7_556 ? B4 B5 B3 107.86(14) . 7_556 ? B6 B5 B2 107.95(14) . 7_556 ? B1 B5 B2 108.02(15) . 7_556 ? B4 B5 B2 59.84(12) . 7_556 ? B3 B5 B2 59.99(12) 7_556 7_556 ? B6 B5 Cl5 121.74(13) . . ? B1 B5 Cl5 121.91(14) . . ? B4 B5 Cl5 121.99(13) . . ? B3 B5 Cl5 121.49(14) 7_556 . ? B2 B5 Cl5 121.69(14) 7_556 . ? B1 B6 B2 60.23(12) . . ? B1 B6 B5 60.15(12) . . ? B2 B6 B5 108.28(14) . . ? B1 B6 B4 108.16(14) . 7_556 ? B2 B6 B4 59.89(12) . 7_556 ? B5 B6 B4 108.12(14) . 7_556 ? B1 B6 B3 108.20(14) . 7_556 ? B2 B6 B3 108.08(14) . 7_556 ? B5 B6 B3 60.00(12) . 7_556 ? B4 B6 B3 60.09(12) 7_556 7_556 ? B1 B6 Cl6 121.30(13) . . ? B2 B6 Cl6 122.11(13) . . ? B5 B6 Cl6 120.96(13) . . ? B4 B6 Cl6 122.22(13) 7_556 . ? B3 B6 Cl6 121.50(14) 7_556 . ? C8 C1 C14 120.52(17) . . ? C8 C1 C2 119.51(17) . . ? C14 C1 C2 119.93(17) . . ? C7 C2 C3 119.11(18) . . ? C7 C2 C1 120.51(17) . . ? C3 C2 C1 120.37(18) . . ? C4 C3 C2 119.99(19) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.26(19) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 120.55(19) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 120.1(2) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C2 119.92(19) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C13 C8 C9 118.67(17) . . ? C13 C8 C1 120.58(17) . . ? C9 C8 C1 120.71(17) . . ? C10 C9 C8 120.25(18) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.01(19) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.57(19) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 120.58(19) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C8 119.87(18) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? C15 C14 C19 118.96(18) . . ? C15 C14 C1 121.07(17) . . ? C19 C14 C1 119.95(18) . . ? C16 C15 C14 119.81(18) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.30(19) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 120.69(19) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 119.85(19) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C14 120.34(19) . . ? C18 C19 H19 119.8 . . ? C14 C19 H19 119.8 . . ? O1 S1 O2 117.40(11) . . ? 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 B4 -37.29(14) . . . 7_556 ? B5 B1 B2 B4 0.22(19) . . . 7_556 ? B4 B1 B2 B4 63.57(19) . . . 7_556 ? B3 B1 B2 B4 100.91(15) . . . 7_556 ? Cl1 B1 B2 B4 -147.71(14) . . . 7_556 ? B5 B1 B2 B6 37.51(13) . . . . ? B4 B1 B2 B6 100.86(16) . . . . ? B3 B1 B2 B6 138.20(15) . . . . ? Cl1 B1 B2 B6 -110.42(16) . . . . ? B6 B1 B2 B3 -138.20(15) . . . . ? B5 B1 B2 B3 -100.69(15) . . . . ? B4 B1 B2 B3 -37.34(14) . . . . ? Cl1 B1 B2 B3 111.38(17) . . . . ? B6 B1 B2 B5 -100.77(16) . . . 7_556 ? B5 B1 B2 B5 -63.26(19) . . . 7_556 ? B4 B1 B2 B5 0.1(2) . . . 7_556 ? B3 B1 B2 B5 37.43(14) . . . 7_556 ? Cl1 B1 B2 B5 148.80(14) . . . 7_556 ? B6 B1 B2 Cl2 110.89(17) . . . . ? B5 B1 B2 Cl2 148.40(14) . . . . ? B4 B1 B2 Cl2 -148.25(14) . . . . ? B3 B1 B2 Cl2 -110.91(17) . . . . ? Cl1 B1 B2 Cl2 0.5(2) . . . . ? B4 B2 B3 B5 37.39(14) 7_556 . . 7_556 ? B6 B2 B3 B5 100.94(16) . . . 7_556 ? B1 B2 B3 B5 138.16(16) . . . 7_556 ? Cl2 B2 B3 B5 -111.14(17) . . . 7_556 ? B4 B2 B3 Cl3 147.86(14) 7_556 . . . ? B6 B2 B3 Cl3 -148.59(14) . . . . ? B1 B2 B3 Cl3 -111.38(17) . . . . ? B5 B2 B3 Cl3 110.46(17) 7_556 . . . ? Cl2 B2 B3 Cl3 -0.7(2) . . . . ? B4 B2 B3 B6 -0.08(19) 7_556 . . 7_556 ? B6 B2 B3 B6 63.47(19) . . . 7_556 ? B1 B2 B3 B6 100.68(16) . . . 7_556 ? B5 B2 B3 B6 -37.48(14) 7_556 . . 7_556 ? Cl2 B2 B3 B6 -148.62(14) . . . 7_556 ? B4 B2 B3 B4 -63.38(19) 7_556 . . . ? B6 B2 B3 B4 0.17(19) . . . . ? B1 B2 B3 B4 37.38(14) . . . . ? B5 B2 B3 B4 -100.77(16) 7_556 . . . ? Cl2 B2 B3 B4 148.08(14) . . . . ? B4 B2 B3 B1 -100.77(16) 7_556 . . . ? B6 B2 B3 B1 -37.22(14) . . . . ? B5 B2 B3 B1 -138.16(16) 7_556 . . . ? Cl2 B2 B3 B1 110.70(17) . . . . ? B6 B1 B3 B5 0.00(19) . . . 7_556 ? B5 B1 B3 B5 63.57(19) . . . 7_556 ? B2 B1 B3 B5 -37.40(14) . . . 7_556 ? B4 B1 B3 B5 100.75(16) . . . 7_556 ? Cl1 B1 B3 B5 -147.71(14) . . . 7_556 ? B6 B1 B3 B2 37.40(14) . . . . ? B5 B1 B3 B2 100.98(15) . . . . ? B4 B1 B3 B2 138.15(15) . . . . ? Cl1 B1 B3 B2 -110.31(17) . . . . ? B6 B1 B3 Cl3 148.69(14) . . . . ? B5 B1 B3 Cl3 -147.74(14) . . . . ? B2 B1 B3 Cl3 111.28(17) . . . . ? B4 B1 B3 Cl3 -110.56(17) . . . . ? Cl1 B1 B3 Cl3 1.0(2) . . . . ? B6 B1 B3 B6 -63.29(19) . . . 7_556 ? B5 B1 B3 B6 0.28(19) . . . 7_556 ? B2 B1 B3 B6 -100.70(15) . . . 7_556 ? B4 B1 B3 B6 37.45(14) . . . 7_556 ? Cl1 B1 B3 B6 148.99(14) . . . 7_556 ? B6 B1 B3 B4 -100.75(16) . . . . ? B5 B1 B3 B4 -37.17(13) . . . . ? B2 B1 B3 B4 -138.15(15) . . . . ? Cl1 B1 B3 B4 111.54(16) . . . . ? B5 B3 B4 B2 -0.01(19) 7_556 . . 7_556 ? B2 B3 B4 B2 63.43(19) . . . 7_556 ? Cl3 B3 B4 B2 -147.57(14) . . . 7_556 ? B6 B3 B4 B2 -37.24(14) 7_556 . . 7_556 ? B1 B3 B4 B2 100.77(15) . . . 7_556 ? B5 B3 B4 B5 -63.61(19) 7_556 . . . ? B2 B3 B4 B5 -0.17(19) . . . . ? Cl3 B3 B4 B5 148.83(14) . . . . ? B6 B3 B4 B5 -100.84(15) 7_556 . . . ? B1 B3 B4 B5 37.17(14) . . . . ? B5 B3 B4 B6 37.23(13) 7_556 . . 7_556 ? B2 B3 B4 B6 100.67(15) . . . 7_556 ? Cl3 B3 B4 B6 -110.34(17) . . . 7_556 ? B1 B3 B4 B6 138.01(15) . . . 7_556 ? B5 B3 B4 B1 -100.78(15) 7_556 . . . ? B2 B3 B4 B1 -37.34(14) . . . . ? Cl3 B3 B4 B1 111.65(17) . . . . ? B6 B3 B4 B1 -138.01(15) 7_556 . . . ? B5 B3 B4 Cl4 147.59(14) 7_556 . . . ? B2 B3 B4 Cl4 -148.98(14) . . . . ? Cl3 B3 B4 Cl4 0.0(2) . . . . ? B6 B3 B4 Cl4 110.35(16) 7_556 . . . ? B1 B3 B4 Cl4 -111.64(17) . . . . ? B6 B1 B4 B2 -0.13(19) . . . 7_556 ? B5 B1 B4 B2 37.45(14) . . . 7_556 ? B2 B1 B4 B2 -63.61(19) . . . 7_556 ? B3 B1 B4 B2 -100.93(16) . . . 7_556 ? Cl1 B1 B4 B2 148.05(14) . . . 7_556 ? B6 B1 B4 B5 -37.58(14) . . . . ? B2 B1 B4 B5 -101.06(16) . . . . ? B3 B1 B4 B5 -138.38(15) . . . . ? Cl1 B1 B4 B5 110.60(17) . . . . ? B6 B1 B4 B6 63.3(2) . . . 7_556 ? B5 B1 B4 B6 100.87(16) . . . 7_556 ? B2 B1 B4 B6 -0.2(2) . . . 7_556 ? B3 B1 B4 B6 -37.52(14) . . . 7_556 ? Cl1 B1 B4 B6 -148.54(14) . . . 7_556 ? B6 B1 B4 B3 100.80(16) . . . . ? B5 B1 B4 B3 138.38(15) . . . . ? B2 B1 B4 B3 37.32(14) . . . . ? Cl1 B1 B4 B3 -111.02(17) . . . . ? B6 B1 B4 Cl4 -148.54(14) . . . . ? B5 B1 B4 Cl4 -110.96(17) . . . . ? B2 B1 B4 Cl4 147.97(14) . . . . ? B3 B1 B4 Cl4 110.65(17) . . . . ? Cl1 B1 B4 Cl4 -0.4(2) . . . . ? B2 B1 B5 B6 -37.49(13) . . . . ? B4 B1 B5 B6 -138.01(15) . . . . ? B3 B1 B5 B6 -100.83(16) . . . . ? Cl1 B1 B5 B6 110.32(16) . . . . ? B6 B1 B5 B4 138.01(15) . . . . ? B2 B1 B5 B4 100.52(15) . . . . ? B3 B1 B5 B4 37.18(13) . . . . ? Cl1 B1 B5 B4 -111.67(16) . . . . ? B6 B1 B5 B3 37.27(13) . . . 7_556 ? B2 B1 B5 B3 -0.22(19) . . . 7_556 ? B4 B1 B5 B3 -100.74(15) . . . 7_556 ? B3 B1 B5 B3 -63.56(19) . . . 7_556 ? Cl1 B1 B5 B3 147.59(13) . . . 7_556 ? B6 B1 B5 B2 100.68(15) . . . 7_556 ? B2 B1 B5 B2 63.19(19) . . . 7_556 ? B4 B1 B5 B2 -37.33(13) . . . 7_556 ? B3 B1 B5 B2 -0.15(19) . . . 7_556 ? Cl1 B1 B5 B2 -149.00(13) . . . 7_556 ? B6 B1 B5 Cl5 -110.73(16) . . . . ? B2 B1 B5 Cl5 -148.22(14) . . . . ? B4 B1 B5 Cl5 111.26(16) . . . . ? B3 B1 B5 Cl5 148.43(14) . . . . ? Cl1 B1 B5 Cl5 -0.4(2) . . . . ? B2 B4 B5 B6 -100.80(15) 7_556 . . . ? B6 B4 B5 B6 -63.35(19) 7_556 . . . ? B3 B4 B5 B6 0.10(19) . . . . ? B1 B4 B5 B6 37.37(14) . . . . ? Cl4 B4 B5 B6 148.79(14) . . . . ? B2 B4 B5 B1 -138.17(15) 7_556 . . . ? B6 B4 B5 B1 -100.71(16) 7_556 . . . ? B3 B4 B5 B1 -37.26(14) . . . . ? Cl4 B4 B5 B1 111.42(17) . . . . ? B2 B4 B5 B3 -37.34(14) 7_556 . . 7_556 ? B6 B4 B5 B3 0.12(19) 7_556 . . 7_556 ? B3 B4 B5 B3 63.57(19) . . . 7_556 ? B1 B4 B5 B3 100.83(16) . . . 7_556 ? Cl4 B4 B5 B3 -147.74(14) . . . 7_556 ? B6 B4 B5 B2 37.46(14) 7_556 . . 7_556 ? B3 B4 B5 B2 100.91(16) . . . 7_556 ? B1 B4 B5 B2 138.17(15) . . . 7_556 ? Cl4 B4 B5 B2 -110.41(17) . . . 7_556 ? B2 B4 B5 Cl5 110.70(17) 7_556 . . . ? B6 B4 B5 Cl5 148.16(14) 7_556 . . . ? B3 B4 B5 Cl5 -148.39(14) . . . . ? B1 B4 B5 Cl5 -111.13(17) . . . . ? Cl4 B4 B5 Cl5 0.3(2) . . . . ? B5 B1 B6 B2 -138.15(15) . . . . ? B4 B1 B6 B2 -100.66(16) . . . . ? B3 B1 B6 B2 -37.32(14) . . . . ? Cl1 B1 B6 B2 110.71(17) . . . . ? B2 B1 B6 B5 138.15(15) . . . . ? B4 B1 B6 B5 37.49(14) . . . . ? B3 B1 B6 B5 100.83(16) . . . . ? Cl1 B1 B6 B5 -111.14(17) . . . . ? B5 B1 B6 B4 -100.90(15) . . . 7_556 ? B2 B1 B6 B4 37.25(14) . . . 7_556 ? B4 B1 B6 B4 -63.42(19) . . . 7_556 ? B3 B1 B6 B4 -0.07(19) . . . 7_556 ? Cl1 B1 B6 B4 147.96(14) . . . 7_556 ? B5 B1 B6 B3 -37.30(14) . . . 7_556 ? B2 B1 B6 B3 100.85(16) . . . 7_556 ? B4 B1 B6 B3 0.18(19) . . . 7_556 ? B3 B1 B6 B3 63.53(19) . . . 7_556 ? Cl1 B1 B6 B3 -148.44(14) . . . 7_556 ? B5 B1 B6 Cl6 110.20(17) . . . . ? B2 B1 B6 Cl6 -111.65(16) . . . . ? B4 B1 B6 Cl6 147.69(14) . . . . ? B3 B1 B6 Cl6 -148.97(14) . . . . ? Cl1 B1 B6 Cl6 -0.9(2) . . . . ? B4 B2 B6 B1 138.33(15) 7_556 . . . ? B3 B2 B6 B1 37.44(14) . . . . ? B5 B2 B6 B1 100.85(15) 7_556 . . . ? Cl2 B2 B6 B1 -110.41(17) . . . . ? B4 B2 B6 B5 100.79(15) 7_556 . . . ? B3 B2 B6 B5 -0.10(19) . . . . ? B1 B2 B6 B5 -37.54(14) . . . . ? B5 B2 B6 B5 63.31(19) 7_556 . . . ? Cl2 B2 B6 B5 -147.96(14) . . . . ? B3 B2 B6 B4 -100.89(15) . . . 7_556 ? B1 B2 B6 B4 -138.33(15) . . . 7_556 ? B5 B2 B6 B4 -37.48(13) 7_556 . . 7_556 ? Cl2 B2 B6 B4 111.26(17) . . . 7_556 ? B4 B2 B6 B3 37.28(14) 7_556 . . 7_556 ? B3 B2 B6 B3 -63.61(19) . . . 7_556 ? B1 B2 B6 B3 -101.05(15) . . . 7_556 ? B5 B2 B6 B3 -0.20(19) 7_556 . . 7_556 ? Cl2 B2 B6 B3 148.53(14) . . . 7_556 ? B4 B2 B6 Cl6 -111.33(16) 7_556 . . . ? B3 B2 B6 Cl6 147.78(14) . . . . ? B1 B2 B6 Cl6 110.33(17) . . . . ? B5 B2 B6 Cl6 -148.81(14) 7_556 . . . ? Cl2 B2 B6 Cl6 -0.1(2) . . . . ? B4 B5 B6 B1 -37.58(14) . . . . ? B3 B5 B6 B1 -138.34(15) 7_556 . . . ? B2 B5 B6 B1 -100.80(16) 7_556 . . . ? Cl5 B5 B6 B1 111.01(17) . . . . ? B1 B5 B6 B2 37.58(14) . . . . ? B4 B5 B6 B2 0.00(19) . . . . ? B3 B5 B6 B2 -100.76(16) 7_556 . . . ? B2 B5 B6 B2 -63.22(19) 7_556 . . . ? Cl5 B5 B6 B2 148.59(14) . . . . ? B1 B5 B6 B4 100.97(16) . . . 7_556 ? B4 B5 B6 B4 63.39(19) . . . 7_556 ? B3 B5 B6 B4 -37.36(14) 7_556 . . 7_556 ? B2 B5 B6 B4 0.17(19) 7_556 . . 7_556 ? Cl5 B5 B6 B4 -148.01(14) . . . 7_556 ? B1 B5 B6 B3 138.34(15) . . . 7_556 ? B4 B5 B6 B3 100.76(16) . . . 7_556 ? B2 B5 B6 B3 37.53(14) 7_556 . . 7_556 ? Cl5 B5 B6 B3 -110.65(17) . . . 7_556 ? B1 B5 B6 Cl6 -110.74(16) . . . . ? B4 B5 B6 Cl6 -148.32(14) . . . . ? B3 B5 B6 Cl6 110.92(17) 7_556 . . . ? B2 B5 B6 Cl6 148.46(14) 7_556 . . . ? Cl5 B5 B6 Cl6 0.3(2) . . . . ? C8 C1 C2 C7 33.9(3) . . . . ? C14 C1 C2 C7 -143.95(19) . . . . ? C8 C1 C2 C3 -147.46(18) . . . . ? C14 C1 C2 C3 34.7(3) . . . . ? C7 C2 C3 C4 -1.6(3) . . . . ? C1 C2 C3 C4 179.72(18) . . . . ? C2 C3 C4 C5 1.2(3) . . . . ? C3 C4 C5 C6 0.4(3) . . . . ? C4 C5 C6 C7 -1.6(3) . . . . ? C5 C6 C7 C2 1.1(3) . . . . ? C3 C2 C7 C6 0.5(3) . . . . ? C1 C2 C7 C6 179.14(19) . . . . ? C14 C1 C8 C13 30.2(3) . . . . ? C2 C1 C8 C13 -147.62(18) . . . . ? C14 C1 C8 C9 -151.94(18) . . . . ? C2 C1 C8 C9 30.3(3) . . . . ? C13 C8 C9 C10 1.8(3) . . . . ? C1 C8 C9 C10 -176.16(19) . . . . ? C8 C9 C10 C11 0.2(3) . . . . ? C9 C10 C11 C12 -1.8(3) . . . . ? C10 C11 C12 C13 1.3(3) . . . . ? C11 C12 C13 C8 0.7(3) . . . . ? C9 C8 C13 C12 -2.2(3) . . . . ? C1 C8 C13 C12 175.71(18) . . . . ? C8 C1 C14 C15 33.2(3) . . . . ? C2 C1 C14 C15 -148.96(19) . . . . ? C8 C1 C14 C19 -144.96(18) . . . . ? C2 C1 C14 C19 32.8(3) . . . . ? C19 C14 C15 C16 0.6(3) . . . . ? C1 C14 C15 C16 -177.60(18) . . . . ? C14 C15 C16 C17 1.3(3) . . . . ? C15 C16 C17 C18 -1.8(3) . . . . ? C16 C17 C18 C19 0.4(3) . . . . ? C17 C18 C19 C14 1.5(3) . . . . ? C15 C14 C19 C18 -2.0(3) . . . . ? C1 C14 C19 C18 176.25(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.441 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.066 # Attachment 'cif_files_ESI_revised.cif' data_ck006-2 _database_code_depnum_ccdc_archive 'CCDC 715825' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B12 Cl12, O2 S, 2(N O)' _chemical_formula_sum 'B12 Cl12 N2 O4 S' _chemical_formula_weight 679.20 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' N N 0.0061 0.0033 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.5023(19) _cell_length_b 15.218(3) _cell_length_c 15.758(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2278.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 113(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 red _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 1.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.520 _exptl_absorpt_correction_T_max 0.820 _exptl_absorpt_process_details ; March 2001 T Higashi ; _exptl_special_details ; March 2001 T Higashi ; _diffrn_ambient_temperature 113(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 8862 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4776 _reflns_number_gt 4431 _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. The disordered NO+ cations were partly refined isotropically. ; _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^+5.8560P] 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 none _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.09(10) _refine_ls_number_reflns 4776 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 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 0.6471(5) 0.0684(3) 0.7871(3) 0.0109(9) Uani 1 1 d . . . Cl1 Cl 0.53339(11) -0.01202(7) 0.83399(6) 0.0186(2) Uani 1 1 d . . . B2 B 0.6289(5) 0.0999(3) 0.6792(3) 0.0117(9) Uani 1 1 d . . . Cl2 Cl 0.49465(10) 0.05509(6) 0.61166(6) 0.0164(2) Uani 1 1 d . . . B3 B 0.7789(5) 0.0386(3) 0.7124(3) 0.0126(9) Uani 1 1 d . . . Cl3 Cl 0.80615(12) -0.07351(6) 0.68109(7) 0.0190(2) Uani 1 1 d . . . B4 B 0.8283(5) 0.0775(3) 0.8152(3) 0.0126(9) Uani 1 1 d . . . Cl4 Cl 0.90737(11) 0.00941(6) 0.89481(6) 0.0175(2) Uani 1 1 d . . . B5 B 0.7084(5) 0.1624(3) 0.8449(3) 0.0110(8) Uani 1 1 d . . . Cl5 Cl 0.65943(11) 0.17991(6) 0.95327(6) 0.0156(2) Uani 1 1 d . . . B6 B 0.5847(5) 0.1770(3) 0.7605(3) 0.0127(9) Uani 1 1 d . . . Cl6 Cl 0.40701(11) 0.21084(7) 0.77971(6) 0.0187(2) Uani 1 1 d . . . B7 B 0.7997(5) 0.1273(3) 0.6384(3) 0.0119(9) Uani 1 1 d . . . Cl7 Cl 0.84510(11) 0.10956(7) 0.53027(6) 0.0173(2) Uani 1 1 d . . . B8 B 0.9229(5) 0.1137(3) 0.7244(3) 0.0111(9) Uani 1 1 d . . . Cl8 Cl 1.10130(11) 0.07922(7) 0.70713(7) 0.0185(2) Uani 1 1 d . . . B9 B 0.8801(5) 0.1905(3) 0.8053(3) 0.0117(9) Uani 1 1 d . . . Cl9 Cl 1.01111(11) 0.23616(6) 0.87323(6) 0.0164(2) Uani 1 1 d . . . B10 B 0.7292(5) 0.2512(3) 0.7715(3) 0.0114(9) Uani 1 1 d . . . Cl10 Cl 0.70183(11) 0.36386(6) 0.80296(6) 0.0174(2) Uani 1 1 d . . . B11 B 0.6803(5) 0.2127(3) 0.6693(3) 0.0117(9) Uani 1 1 d . . . Cl11 Cl 0.59876(11) 0.28336(6) 0.59276(6) 0.0168(2) Uani 1 1 d . . . B12 B 0.8619(5) 0.2215(3) 0.6968(3) 0.0120(9) Uani 1 1 d . . . Cl12 Cl 0.97356(11) 0.30129(6) 0.64759(7) 0.0199(2) Uani 1 1 d . . . N1 N 0.8091(8) 0.6905(4) 0.9220(4) 0.0710(19) Uani 1 1 d . . . O1 O 0.7246(7) 0.7217(4) 0.9037(4) 0.0231(13) Uiso 0.60 1 d P A 1 O1A O 0.7039(9) 0.7040(6) 0.9327(6) 0.0211(19) Uiso 0.40 1 d P A 2 N2 N 0.4848(6) 0.3603(5) 0.9524(5) 0.0457(17) Uani 1 1 d . . . O2 O 0.4141(9) 0.3355(6) 0.9367(5) 0.054(2) Uani 0.75 1 d P . . O2A O 0.3961(19) 0.3974(10) 0.9559(8) 0.034(4) Uani 0.25 1 d P . . S1 S 0.85618(14) 0.45010(8) 0.99545(8) 0.0310(3) Uani 1 1 d . . . O3 O 0.7815(4) 0.5322(2) 0.9917(2) 0.0362(9) Uani 1 1 d . . . O4 O 0.7803(5) 0.3752(3) 1.0210(3) 0.0588(13) 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(2) 0.010(2) 0.013(2) 0.0013(16) -0.0024(17) -0.0012(18) Cl1 0.0204(5) 0.0168(5) 0.0185(5) 0.0021(4) 0.0015(4) -0.0089(4) B2 0.011(2) 0.010(2) 0.014(2) -0.0026(16) 0.0005(16) 0.0005(18) Cl2 0.0155(5) 0.0183(5) 0.0153(4) -0.0031(4) -0.0054(4) -0.0034(4) B3 0.016(2) 0.010(2) 0.012(2) -0.0017(16) -0.0005(17) 0.0009(19) Cl3 0.0253(5) 0.0098(4) 0.0218(5) -0.0047(4) -0.0031(4) 0.0024(4) B4 0.017(2) 0.0094(19) 0.012(2) 0.0010(16) -0.0025(18) 0.0013(19) Cl4 0.0229(5) 0.0134(4) 0.0163(5) 0.0031(4) -0.0064(4) 0.0028(4) B5 0.014(2) 0.013(2) 0.0066(19) -0.0024(15) -0.0004(16) 0.0006(19) Cl5 0.0184(5) 0.0178(5) 0.0107(4) -0.0017(3) 0.0014(4) 0.0008(4) B6 0.016(2) 0.014(2) 0.0080(19) -0.0005(16) 0.0016(17) 0.0028(19) Cl6 0.0105(5) 0.0256(5) 0.0200(5) -0.0028(4) 0.0001(4) 0.0039(4) B7 0.014(2) 0.013(2) 0.008(2) -0.0009(15) 0.0018(17) -0.002(2) Cl7 0.0200(5) 0.0210(5) 0.0110(5) -0.0019(4) 0.0026(4) -0.0003(4) B8 0.009(2) 0.013(2) 0.011(2) -0.0013(16) -0.0012(16) 0.0010(18) Cl8 0.0097(5) 0.0225(5) 0.0233(5) 0.0005(4) 0.0017(4) 0.0037(4) B9 0.013(2) 0.010(2) 0.012(2) -0.0006(16) -0.0011(17) -0.0062(18) Cl9 0.0164(5) 0.0172(5) 0.0158(5) -0.0007(4) -0.0055(4) -0.0057(4) B10 0.015(2) 0.010(2) 0.009(2) 0.0005(16) -0.0025(17) -0.0011(19) Cl10 0.0248(5) 0.0085(4) 0.0189(5) -0.0017(3) -0.0025(4) 0.0027(4) B11 0.012(2) 0.012(2) 0.011(2) 0.0002(16) -0.0016(17) 0.0004(19) Cl11 0.0194(5) 0.0153(5) 0.0155(5) 0.0035(4) -0.0040(4) 0.0038(4) B12 0.010(2) 0.011(2) 0.016(2) 0.0000(16) -0.0003(17) -0.0005(18) Cl12 0.0207(5) 0.0171(5) 0.0219(5) 0.0042(4) 0.0035(4) -0.0071(4) N1 0.105(5) 0.055(4) 0.052(4) -0.022(3) 0.024(4) -0.026(4) N2 0.035(3) 0.048(4) 0.053(4) 0.021(3) 0.018(3) 0.022(3) O2 0.062(5) 0.055(5) 0.044(4) -0.009(3) 0.028(4) 0.012(4) O2A 0.054(11) 0.037(9) 0.011(6) 0.006(6) -0.009(7) -0.015(8) S1 0.0304(7) 0.0340(7) 0.0286(6) 0.0027(5) -0.0088(5) -0.0047(6) O3 0.0299(19) 0.047(2) 0.032(2) 0.0054(16) -0.0095(16) 0.0070(17) O4 0.096(4) 0.047(2) 0.033(2) -0.0057(19) 0.010(2) -0.037(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 B2 1.774(6) . ? B1 B3 1.777(6) . ? B1 B4 1.783(6) . ? B1 Cl1 1.792(4) . ? B1 B5 1.794(6) . ? B1 B6 1.805(6) . ? B2 B3 1.783(6) . ? B2 B6 1.786(6) . ? B2 B11 1.791(6) . ? B2 B7 1.795(6) . ? B2 Cl2 1.796(5) . ? B3 B4 1.788(6) . ? B3 B8 1.793(6) . ? B3 Cl3 1.794(4) . ? B3 B7 1.795(6) . ? B4 B8 1.777(6) . ? B4 B5 1.785(6) . ? B4 Cl4 1.792(4) . ? B4 B9 1.795(6) . ? B5 B6 1.788(6) . ? B5 B10 1.790(6) . ? B5 Cl5 1.790(4) . ? B5 B9 1.798(6) . ? B6 B11 1.786(6) . ? B6 B10 1.787(6) . ? B6 Cl6 1.791(5) . ? B7 Cl7 1.779(4) . ? B7 B11 1.792(6) . ? B7 B8 1.802(6) . ? B7 B12 1.802(6) . ? B8 B9 1.777(6) . ? B8 B12 1.793(6) . ? B8 Cl8 1.795(5) . ? B9 B12 1.782(6) . ? B9 Cl9 1.783(4) . ? B9 B10 1.787(6) . ? B10 B11 1.776(6) . ? B10 B12 1.784(6) . ? B10 Cl10 1.803(4) . ? B11 B12 1.784(6) . ? B11 Cl11 1.792(4) . ? B12 Cl12 1.790(5) . ? N1 O1 0.976(8) . ? N1 O1A 1.034(11) . ? N2 O2 0.809(8) . ? N2 O2A 1.015(18) . ? S1 O4 1.407(4) . ? S1 O3 1.438(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 B2 B1 B3 60.3(2) . . ? B2 B1 B4 108.1(3) . . ? B3 B1 B4 60.3(3) . . ? B2 B1 Cl1 121.4(3) . . ? B3 B1 Cl1 121.6(3) . . ? B4 B1 Cl1 122.2(3) . . ? B2 B1 B5 107.6(3) . . ? B3 B1 B5 108.1(3) . . ? B4 B1 B5 59.9(2) . . ? Cl1 B1 B5 122.1(3) . . ? B2 B1 B6 59.9(2) . . ? B3 B1 B6 108.2(3) . . ? B4 B1 B6 107.7(3) . . ? Cl1 B1 B6 121.5(3) . . ? B5 B1 B6 59.6(2) . . ? B1 B2 B3 59.9(3) . . ? B1 B2 B6 60.9(2) . . ? B3 B2 B6 108.8(3) . . ? B1 B2 B11 108.5(3) . . ? B3 B2 B11 108.0(3) . . ? B6 B2 B11 59.9(2) . . ? B1 B2 B7 108.5(3) . . ? B3 B2 B7 60.2(2) . . ? B6 B2 B7 108.5(3) . . ? B11 B2 B7 60.0(2) . . ? B1 B2 Cl2 122.3(3) . . ? B3 B2 Cl2 122.9(3) . . ? B6 B2 Cl2 120.5(3) . . ? B11 B2 Cl2 120.4(3) . . ? B7 B2 Cl2 121.2(3) . . ? B1 B3 B2 59.8(2) . . ? B1 B3 B4 60.0(2) . . ? B2 B3 B4 107.6(3) . . ? B1 B3 B8 107.8(3) . . ? B2 B3 B8 107.9(3) . . ? B4 B3 B8 59.5(2) . . ? B1 B3 Cl3 121.8(3) . . ? B2 B3 Cl3 122.2(3) . . ? B4 B3 Cl3 121.8(3) . . ? B8 B3 Cl3 121.7(3) . . ? B1 B3 B7 108.4(3) . . ? B2 B3 B7 60.2(2) . . ? B4 B3 B7 108.1(3) . . ? B8 B3 B7 60.3(3) . . ? Cl3 B3 B7 121.4(3) . . ? B8 B4 B1 108.2(3) . . ? B8 B4 B5 108.0(3) . . ? B1 B4 B5 60.3(3) . . ? B8 B4 B3 60.4(3) . . ? B1 B4 B3 59.7(2) . . ? B5 B4 B3 108.0(3) . . ? B8 B4 Cl4 122.1(3) . . ? B1 B4 Cl4 122.2(3) . . ? B5 B4 Cl4 120.2(3) . . ? B3 B4 Cl4 123.6(3) . . ? B8 B4 B9 59.7(2) . . ? B1 B4 B9 108.5(3) . . ? B5 B4 B9 60.3(2) . . ? B3 B4 B9 108.1(3) . . ? Cl4 B4 B9 120.0(3) . . ? B4 B5 B6 108.3(3) . . ? B4 B5 B10 107.9(3) . . ? B6 B5 B10 59.9(2) . . ? B4 B5 Cl5 121.6(3) . . ? B6 B5 Cl5 121.3(3) . . ? B10 B5 Cl5 122.2(3) . . ? B4 B5 B1 59.8(2) . . ? B6 B5 B1 60.5(2) . . ? B10 B5 B1 108.1(3) . . ? Cl5 B5 B1 121.2(3) . . ? B4 B5 B9 60.1(3) . . ? B6 B5 B9 108.0(3) . . ? B10 B5 B9 59.8(2) . . ? Cl5 B5 B9 122.1(3) . . ? B1 B5 B9 107.9(3) . . ? B11 B6 B2 60.2(2) . . ? B11 B6 B10 59.6(2) . . ? B2 B6 B10 107.7(3) . . ? B11 B6 B5 107.5(3) . . ? B2 B6 B5 107.3(3) . . ? B10 B6 B5 60.1(2) . . ? B11 B6 Cl6 121.9(3) . . ? B2 B6 Cl6 122.1(3) . . ? B10 B6 Cl6 121.7(3) . . ? B5 B6 Cl6 122.0(3) . . ? B11 B6 B1 107.3(3) . . ? B2 B6 B1 59.2(3) . . ? B10 B6 B1 107.7(3) . . ? B5 B6 B1 59.9(2) . . ? Cl6 B6 B1 122.3(3) . . ? Cl7 B7 B11 121.6(3) . . ? Cl7 B7 B3 122.3(3) . . ? B11 B7 B3 107.4(3) . . ? Cl7 B7 B2 121.8(3) . . ? B11 B7 B2 59.9(2) . . ? B3 B7 B2 59.5(2) . . ? Cl7 B7 B8 123.0(3) . . ? B11 B7 B8 106.9(3) . . ? B3 B7 B8 59.8(2) . . ? B2 B7 B8 106.9(3) . . ? Cl7 B7 B12 122.0(3) . . ? B11 B7 B12 59.5(2) . . ? B3 B7 B12 107.6(3) . . ? B2 B7 B12 107.3(3) . . ? B8 B7 B12 59.7(2) . . ? B9 B8 B4 60.7(2) . . ? B9 B8 B3 108.7(3) . . ? B4 B8 B3 60.1(2) . . ? B9 B8 B12 59.9(3) . . ? B4 B8 B12 108.4(3) . . ? B3 B8 B12 108.1(3) . . ? B9 B8 Cl8 121.1(3) . . ? B4 B8 Cl8 120.6(3) . . ? B3 B8 Cl8 121.2(3) . . ? B12 B8 Cl8 122.4(3) . . ? B9 B8 B7 108.4(3) . . ? B4 B8 B7 108.2(3) . . ? B3 B8 B7 59.9(2) . . ? B12 B8 B7 60.2(2) . . ? Cl8 B8 B7 122.2(3) . . ? B8 B9 B12 60.5(2) . . ? B8 B9 Cl9 121.8(3) . . ? B12 B9 Cl9 122.7(3) . . ? B8 B9 B10 108.1(3) . . ? B12 B9 B10 60.0(2) . . ? Cl9 B9 B10 122.5(3) . . ? B8 B9 B4 59.7(2) . . ? B12 B9 B4 108.1(3) . . ? Cl9 B9 B4 120.8(3) . . ? B10 B9 B4 107.6(3) . . ? B8 B9 B5 107.5(3) . . ? B12 B9 B5 107.9(3) . . ? Cl9 B9 B5 121.2(3) . . ? B10 B9 B5 59.9(2) . . ? B4 B9 B5 59.6(2) . . ? B11 B10 B12 60.1(2) . . ? B11 B10 B6 60.1(2) . . ? B12 B10 B6 108.6(3) . . ? B11 B10 B9 108.0(3) . . ? B12 B10 B9 59.9(2) . . ? B6 B10 B9 108.5(3) . . ? B11 B10 B5 107.9(3) . . ? B12 B10 B5 108.2(3) . . ? B6 B10 B5 60.0(2) . . ? B9 B10 B5 60.3(2) . . ? B11 B10 Cl10 121.7(3) . . ? B12 B10 Cl10 121.7(3) . . ? B6 B10 Cl10 121.1(3) . . ? B9 B10 Cl10 121.7(3) . . ? B5 B10 Cl10 121.6(3) . . ? B10 B11 B12 60.1(2) . . ? B10 B11 B6 60.2(2) . . ? B12 B11 B6 108.6(3) . . ? B10 B11 B2 108.0(3) . . ? B12 B11 B2 108.3(3) . . ? B6 B11 B2 59.9(2) . . ? B10 B11 B7 108.7(3) . . ? B12 B11 B7 60.5(3) . . ? B6 B11 B7 108.7(3) . . ? B2 B11 B7 60.1(2) . . ? B10 B11 Cl11 121.7(3) . . ? B12 B11 Cl11 122.5(3) . . ? B6 B11 Cl11 120.3(3) . . ? B2 B11 Cl11 121.1(3) . . ? B7 B11 Cl11 121.7(3) . . ? B9 B12 B10 60.2(2) . . ? B9 B12 B11 107.9(3) . . ? B10 B12 B11 59.7(2) . . ? B9 B12 Cl12 122.5(3) . . ? B10 B12 Cl12 122.2(3) . . ? B11 B12 Cl12 121.3(3) . . ? B9 B12 B8 59.6(2) . . ? B10 B12 B8 107.5(3) . . ? B11 B12 B8 107.6(3) . . ? Cl12 B12 B8 122.3(3) . . ? B9 B12 B7 108.1(3) . . ? B10 B12 B7 107.9(3) . . ? B11 B12 B7 60.0(2) . . ? Cl12 B12 B7 120.9(3) . . ? B8 B12 B7 60.2(2) . . ? O4 S1 O3 117.5(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 B4 B1 B2 B3 38.0(3) . . . . ? Cl1 B1 B2 B3 -111.0(4) . . . . ? B5 B1 B2 B3 101.2(3) . . . . ? B6 B1 B2 B3 138.3(3) . . . . ? B3 B1 B2 B6 -138.3(3) . . . . ? B4 B1 B2 B6 -100.3(3) . . . . ? Cl1 B1 B2 B6 110.7(4) . . . . ? B5 B1 B2 B6 -37.1(3) . . . . ? B3 B1 B2 B11 -100.6(3) . . . . ? B4 B1 B2 B11 -62.6(4) . . . . ? Cl1 B1 B2 B11 148.4(3) . . . . ? B5 B1 B2 B11 0.7(4) . . . . ? B6 B1 B2 B11 37.7(3) . . . . ? B3 B1 B2 B7 -37.0(3) . . . . ? B4 B1 B2 B7 1.0(4) . . . . ? Cl1 B1 B2 B7 -148.0(3) . . . . ? B5 B1 B2 B7 64.3(4) . . . . ? B6 B1 B2 B7 101.3(3) . . . . ? B3 B1 B2 Cl2 112.1(3) . . . . ? B4 B1 B2 Cl2 150.1(3) . . . . ? Cl1 B1 B2 Cl2 1.1(5) . . . . ? B5 B1 B2 Cl2 -146.7(3) . . . . ? B6 B1 B2 Cl2 -109.6(4) . . . . ? B4 B1 B3 B2 -137.7(3) . . . . ? Cl1 B1 B3 B2 110.7(3) . . . . ? B5 B1 B3 B2 -100.3(3) . . . . ? B6 B1 B3 B2 -37.2(3) . . . . ? B2 B1 B3 B4 137.7(3) . . . . ? Cl1 B1 B3 B4 -111.7(3) . . . . ? B5 B1 B3 B4 37.4(3) . . . . ? B6 B1 B3 B4 100.4(3) . . . . ? B2 B1 B3 B8 100.8(3) . . . . ? B4 B1 B3 B8 -36.9(3) . . . . ? Cl1 B1 B3 B8 -148.6(3) . . . . ? B5 B1 B3 B8 0.5(4) . . . . ? B6 B1 B3 B8 63.5(4) . . . . ? B2 B1 B3 Cl3 -111.4(4) . . . . ? B4 B1 B3 Cl3 111.0(4) . . . . ? Cl1 B1 B3 Cl3 -0.7(5) . . . . ? B5 B1 B3 Cl3 148.3(3) . . . . ? B6 B1 B3 Cl3 -148.6(3) . . . . ? B2 B1 B3 B7 37.0(3) . . . . ? B4 B1 B3 B7 -100.7(3) . . . . ? Cl1 B1 B3 B7 147.6(3) . . . . ? B5 B1 B3 B7 -63.3(4) . . . . ? B6 B1 B3 B7 -0.3(4) . . . . ? B6 B2 B3 B1 37.9(3) . . . . ? B11 B2 B3 B1 101.3(3) . . . . ? B7 B2 B3 B1 138.9(3) . . . . ? Cl2 B2 B3 B1 -111.2(4) . . . . ? B1 B2 B3 B4 -37.7(3) . . . . ? B6 B2 B3 B4 0.1(4) . . . . ? B11 B2 B3 B4 63.6(4) . . . . ? B7 B2 B3 B4 101.2(3) . . . . ? Cl2 B2 B3 B4 -148.9(3) . . . . ? B1 B2 B3 B8 -100.6(3) . . . . ? B6 B2 B3 B8 -62.7(4) . . . . ? B11 B2 B3 B8 0.8(4) . . . . ? B7 B2 B3 B8 38.3(3) . . . . ? Cl2 B2 B3 B8 148.3(3) . . . . ? B1 B2 B3 Cl3 110.7(4) . . . . ? B6 B2 B3 Cl3 148.5(3) . . . . ? B11 B2 B3 Cl3 -148.0(3) . . . . ? B7 B2 B3 Cl3 -110.4(4) . . . . ? Cl2 B2 B3 Cl3 -0.5(5) . . . . ? B1 B2 B3 B7 -138.9(3) . . . . ? B6 B2 B3 B7 -101.0(3) . . . . ? B11 B2 B3 B7 -37.6(3) . . . . ? Cl2 B2 B3 B7 109.9(4) . . . . ? B2 B1 B4 B8 -0.6(4) . . . . ? B3 B1 B4 B8 37.4(3) . . . . ? Cl1 B1 B4 B8 148.1(3) . . . . ? B5 B1 B4 B8 -100.8(3) . . . . ? B6 B1 B4 B8 -63.9(4) . . . . ? B2 B1 B4 B5 100.2(3) . . . . ? B3 B1 B4 B5 138.2(3) . . . . ? Cl1 B1 B4 B5 -111.1(3) . . . . ? B6 B1 B4 B5 37.0(3) . . . . ? B2 B1 B4 B3 -38.0(3) . . . . ? Cl1 B1 B4 B3 110.7(4) . . . . ? B5 B1 B4 B3 -138.2(3) . . . . ? B6 B1 B4 B3 -101.2(3) . . . . ? B2 B1 B4 Cl4 -150.8(3) . . . . ? B3 B1 B4 Cl4 -112.9(4) . . . . ? Cl1 B1 B4 Cl4 -2.2(5) . . . . ? B5 B1 B4 Cl4 108.9(4) . . . . ? B6 B1 B4 Cl4 145.9(3) . . . . ? B2 B1 B4 B9 62.6(4) . . . . ? B3 B1 B4 B9 100.6(3) . . . . ? Cl1 B1 B4 B9 -148.7(3) . . . . ? B5 B1 B4 B9 -37.6(3) . . . . ? B6 B1 B4 B9 -0.7(4) . . . . ? B1 B3 B4 B8 -138.4(3) . . . . ? B2 B3 B4 B8 -100.8(3) . . . . ? Cl3 B3 B4 B8 110.6(4) . . . . ? B7 B3 B4 B8 -37.2(3) . . . . ? B2 B3 B4 B1 37.6(3) . . . . ? B8 B3 B4 B1 138.4(3) . . . . ? Cl3 B3 B4 B1 -111.0(4) . . . . ? B7 B3 B4 B1 101.3(3) . . . . ? B1 B3 B4 B5 -37.5(3) . . . . ? B2 B3 B4 B5 0.1(4) . . . . ? B8 B3 B4 B5 100.9(3) . . . . ? Cl3 B3 B4 B5 -148.5(3) . . . . ? B7 B3 B4 B5 63.7(4) . . . . ? B1 B3 B4 Cl4 110.7(4) . . . . ? B2 B3 B4 Cl4 148.4(3) . . . . ? B8 B3 B4 Cl4 -110.8(4) . . . . ? Cl3 B3 B4 Cl4 -0.2(5) . . . . ? B7 B3 B4 Cl4 -148.0(3) . . . . ? B1 B3 B4 B9 -101.3(3) . . . . ? B2 B3 B4 B9 -63.7(4) . . . . ? B8 B3 B4 B9 37.1(3) . . . . ? Cl3 B3 B4 B9 147.7(3) . . . . ? B7 B3 B4 B9 0.0(4) . . . . ? B8 B4 B5 B6 63.6(4) . . . . ? B1 B4 B5 B6 -37.5(3) . . . . ? B3 B4 B5 B6 -0.3(4) . . . . ? Cl4 B4 B5 B6 -149.8(3) . . . . ? B9 B4 B5 B6 100.7(3) . . . . ? B8 B4 B5 B10 0.2(4) . . . . ? B1 B4 B5 B10 -100.9(3) . . . . ? B3 B4 B5 B10 -63.7(4) . . . . ? Cl4 B4 B5 B10 146.8(3) . . . . ? B9 B4 B5 B10 37.3(3) . . . . ? B8 B4 B5 Cl5 -148.6(3) . . . . ? B1 B4 B5 Cl5 110.3(4) . . . . ? B3 B4 B5 Cl5 147.5(3) . . . . ? Cl4 B4 B5 Cl5 -2.0(5) . . . . ? B9 B4 B5 Cl5 -111.5(4) . . . . ? B8 B4 B5 B1 101.1(3) . . . . ? B3 B4 B5 B1 37.2(3) . . . . ? Cl4 B4 B5 B1 -112.3(4) . . . . ? B9 B4 B5 B1 138.2(3) . . . . ? B8 B4 B5 B9 -37.1(3) . . . . ? B1 B4 B5 B9 -138.2(3) . . . . ? B3 B4 B5 B9 -101.0(3) . . . . ? Cl4 B4 B5 B9 109.5(4) . . . . ? B2 B1 B5 B4 -101.2(3) . . . . ? B3 B1 B5 B4 -37.5(3) . . . . ? Cl1 B1 B5 B4 111.3(4) . . . . ? B6 B1 B5 B4 -138.4(3) . . . . ? B2 B1 B5 B6 37.2(3) . . . . ? B3 B1 B5 B6 100.9(3) . . . . ? B4 B1 B5 B6 138.4(3) . . . . ? Cl1 B1 B5 B6 -110.3(4) . . . . ? B2 B1 B5 B10 -0.6(4) . . . . ? B3 B1 B5 B10 63.1(4) . . . . ? B4 B1 B5 B10 100.6(3) . . . . ? Cl1 B1 B5 B10 -148.1(3) . . . . ? B6 B1 B5 B10 -37.8(3) . . . . ? B2 B1 B5 Cl5 148.0(3) . . . . ? B3 B1 B5 Cl5 -148.3(3) . . . . ? B4 B1 B5 Cl5 -110.8(3) . . . . ? Cl1 B1 B5 Cl5 0.5(5) . . . . ? B6 B1 B5 Cl5 110.8(4) . . . . ? B2 B1 B5 B9 -63.8(4) . . . . ? B3 B1 B5 B9 -0.1(4) . . . . ? B4 B1 B5 B9 37.4(3) . . . . ? Cl1 B1 B5 B9 148.7(3) . . . . ? B6 B1 B5 B9 -101.0(3) . . . . ? B1 B2 B6 B11 137.8(3) . . . . ? B3 B2 B6 B11 100.4(3) . . . . ? B7 B2 B6 B11 36.5(3) . . . . ? Cl2 B2 B6 B11 -109.7(3) . . . . ? B1 B2 B6 B10 100.5(3) . . . . ? B3 B2 B6 B10 63.0(4) . . . . ? B11 B2 B6 B10 -37.4(3) . . . . ? B7 B2 B6 B10 -0.9(4) . . . . ? Cl2 B2 B6 B10 -147.1(3) . . . . ? B1 B2 B6 B5 37.1(3) . . . . ? B3 B2 B6 B5 -0.3(4) . . . . ? B11 B2 B6 B5 -100.7(3) . . . . ? B7 B2 B6 B5 -64.2(4) . . . . ? Cl2 B2 B6 B5 149.6(3) . . . . ? B1 B2 B6 Cl6 -111.1(4) . . . . ? B3 B2 B6 Cl6 -148.6(3) . . . . ? B11 B2 B6 Cl6 111.0(4) . . . . ? B7 B2 B6 Cl6 147.5(3) . . . . ? Cl2 B2 B6 Cl6 1.3(5) . . . . ? B3 B2 B6 B1 -37.4(3) . . . . ? B11 B2 B6 B1 -137.8(3) . . . . ? B7 B2 B6 B1 -101.4(3) . . . . ? Cl2 B2 B6 B1 112.5(3) . . . . ? B4 B5 B6 B11 -63.0(4) . . . . ? B10 B5 B6 B11 37.4(3) . . . . ? Cl5 B5 B6 B11 149.1(3) . . . . ? B1 B5 B6 B11 -100.2(3) . . . . ? B9 B5 B6 B11 0.6(4) . . . . ? B4 B5 B6 B2 0.4(4) . . . . ? B10 B5 B6 B2 100.8(3) . . . . ? Cl5 B5 B6 B2 -147.6(3) . . . . ? B1 B5 B6 B2 -36.8(3) . . . . ? B9 B5 B6 B2 64.0(4) . . . . ? B4 B5 B6 B10 -100.5(3) . . . . ? Cl5 B5 B6 B10 111.6(3) . . . . ? B1 B5 B6 B10 -137.7(3) . . . . ? B9 B5 B6 B10 -36.9(3) . . . . ? B4 B5 B6 Cl6 148.7(3) . . . . ? B10 B5 B6 Cl6 -110.8(4) . . . . ? Cl5 B5 B6 Cl6 0.8(5) . . . . ? B1 B5 B6 Cl6 111.5(4) . . . . ? B9 B5 B6 Cl6 -147.7(3) . . . . ? B4 B5 B6 B1 37.2(3) . . . . ? B10 B5 B6 B1 137.7(3) . . . . ? Cl5 B5 B6 B1 -110.7(4) . . . . ? B9 B5 B6 B1 100.8(3) . . . . ? B2 B1 B6 B11 -37.6(3) . . . . ? B3 B1 B6 B11 -0.2(4) . . . . ? B4 B1 B6 B11 63.5(4) . . . . ? Cl1 B1 B6 B11 -148.1(3) . . . . ? B5 B1 B6 B11 100.6(3) . . . . ? B3 B1 B6 B2 37.4(3) . . . . ? B4 B1 B6 B2 101.1(3) . . . . ? Cl1 B1 B6 B2 -110.5(3) . . . . ? B5 B1 B6 B2 138.2(3) . . . . ? B2 B1 B6 B10 -100.4(3) . . . . ? B3 B1 B6 B10 -63.0(4) . . . . ? B4 B1 B6 B10 0.7(4) . . . . ? Cl1 B1 B6 B10 149.0(3) . . . . ? B5 B1 B6 B10 37.8(3) . . . . ? B2 B1 B6 B5 -138.2(3) . . . . ? B3 B1 B6 B5 -100.8(3) . . . . ? B4 B1 B6 B5 -37.1(3) . . . . ? Cl1 B1 B6 B5 111.3(3) . . . . ? B2 B1 B6 Cl6 110.8(4) . . . . ? B3 B1 B6 Cl6 148.2(3) . . . . ? B4 B1 B6 Cl6 -148.1(3) . . . . ? Cl1 B1 B6 Cl6 0.3(5) . . . . ? B5 B1 B6 Cl6 -111.0(3) . . . . ? B1 B3 B7 Cl7 -147.4(3) . . . . ? B2 B3 B7 Cl7 -110.6(4) . . . . ? B4 B3 B7 Cl7 149.1(3) . . . . ? B8 B3 B7 Cl7 112.2(4) . . . . ? Cl3 B3 B7 Cl7 1.1(5) . . . . ? B1 B3 B7 B11 0.6(4) . . . . ? B2 B3 B7 B11 37.4(3) . . . . ? B4 B3 B7 B11 -62.9(4) . . . . ? B8 B3 B7 B11 -99.8(3) . . . . ? Cl3 B3 B7 B11 149.1(3) . . . . ? B1 B3 B7 B2 -36.8(3) . . . . ? B4 B3 B7 B2 -100.3(3) . . . . ? B8 B3 B7 B2 -137.2(3) . . . . ? Cl3 B3 B7 B2 111.7(4) . . . . ? B1 B3 B7 B8 100.4(3) . . . . ? B2 B3 B7 B8 137.2(3) . . . . ? B4 B3 B7 B8 36.8(3) . . . . ? Cl3 B3 B7 B8 -111.1(4) . . . . ? B1 B3 B7 B12 63.4(4) . . . . ? B2 B3 B7 B12 100.1(3) . . . . ? B4 B3 B7 B12 -0.2(4) . . . . ? B8 B3 B7 B12 -37.1(3) . . . . ? Cl3 B3 B7 B12 -148.1(3) . . . . ? B1 B2 B7 Cl7 148.3(3) . . . . ? B3 B2 B7 Cl7 111.4(4) . . . . ? B6 B2 B7 Cl7 -147.1(3) . . . . ? B11 B2 B7 Cl7 -110.6(4) . . . . ? Cl2 B2 B7 Cl7 -1.2(5) . . . . ? B1 B2 B7 B11 -101.1(3) . . . . ? B3 B2 B7 B11 -137.9(3) . . . . ? B6 B2 B7 B11 -36.4(3) . . . . ? Cl2 B2 B7 B11 109.5(3) . . . . ? B1 B2 B7 B3 36.9(3) . . . . ? B6 B2 B7 B3 101.5(3) . . . . ? B11 B2 B7 B3 137.9(3) . . . . ? Cl2 B2 B7 B3 -112.6(3) . . . . ? B1 B2 B7 B8 -1.0(4) . . . . ? B3 B2 B7 B8 -37.9(3) . . . . ? B6 B2 B7 B8 63.6(4) . . . . ? B11 B2 B7 B8 100.1(3) . . . . ? Cl2 B2 B7 B8 -150.5(3) . . . . ? B1 B2 B7 B12 -63.8(4) . . . . ? B3 B2 B7 B12 -100.6(3) . . . . ? B6 B2 B7 B12 0.9(4) . . . . ? B11 B2 B7 B12 37.3(3) . . . . ? Cl2 B2 B7 B12 146.8(3) . . . . ? B1 B4 B8 B9 101.2(3) . . . . ? B5 B4 B8 B9 37.4(3) . . . . ? B3 B4 B8 B9 138.3(3) . . . . ? Cl4 B4 B8 B9 -108.5(4) . . . . ? B1 B4 B8 B3 -37.1(3) . . . . ? B5 B4 B8 B3 -100.9(3) . . . . ? Cl4 B4 B8 B3 113.2(4) . . . . ? B9 B4 B8 B3 -138.3(3) . . . . ? B1 B4 B8 B12 63.7(4) . . . . ? B5 B4 B8 B12 -0.1(4) . . . . ? B3 B4 B8 B12 100.8(3) . . . . ? Cl4 B4 B8 B12 -146.0(3) . . . . ? B9 B4 B8 B12 -37.5(3) . . . . ? B1 B4 B8 Cl8 -147.9(3) . . . . ? B5 B4 B8 Cl8 148.3(3) . . . . ? B3 B4 B8 Cl8 -110.8(3) . . . . ? Cl4 B4 B8 Cl8 2.4(5) . . . . ? B9 B4 B8 Cl8 110.9(3) . . . . ? B1 B4 B8 B7 0.0(4) . . . . ? B5 B4 B8 B7 -63.9(4) . . . . ? B3 B4 B8 B7 37.1(3) . . . . ? Cl4 B4 B8 B7 150.3(3) . . . . ? B9 B4 B8 B7 -101.3(3) . . . . ? B1 B3 B8 B9 -0.6(4) . . . . ? B2 B3 B8 B9 62.6(4) . . . . ? B4 B3 B8 B9 -37.7(3) . . . . ? Cl3 B3 B8 B9 -148.5(3) . . . . ? B7 B3 B8 B9 100.9(3) . . . . ? B1 B3 B8 B4 37.1(3) . . . . ? B2 B3 B8 B4 100.3(3) . . . . ? Cl3 B3 B8 B4 -110.8(4) . . . . ? B7 B3 B8 B4 138.6(3) . . . . ? B1 B3 B8 B12 -64.1(4) . . . . ? B2 B3 B8 B12 -0.9(4) . . . . ? B4 B3 B8 B12 -101.2(3) . . . . ? Cl3 B3 B8 B12 148.0(3) . . . . ? B7 B3 B8 B12 37.4(3) . . . . ? B1 B3 B8 Cl8 146.9(3) . . . . ? B2 B3 B8 Cl8 -150.0(3) . . . . ? B4 B3 B8 Cl8 109.7(4) . . . . ? Cl3 B3 B8 Cl8 -1.0(5) . . . . ? B7 B3 B8 Cl8 -111.7(3) . . . . ? B1 B3 B8 B7 -101.5(3) . . . . ? B2 B3 B8 B7 -38.3(3) . . . . ? B4 B3 B8 B7 -138.6(3) . . . . ? Cl3 B3 B8 B7 110.6(4) . . . . ? Cl7 B7 B8 B9 147.5(3) . . . . ? B11 B7 B8 B9 -0.7(4) . . . . ? B3 B7 B8 B9 -101.4(3) . . . . ? B2 B7 B8 B9 -63.6(4) . . . . ? B12 B7 B8 B9 36.9(3) . . . . ? Cl7 B7 B8 B4 -148.2(3) . . . . ? B11 B7 B8 B4 63.5(4) . . . . ? B3 B7 B8 B4 -37.1(3) . . . . ? B2 B7 B8 B4 0.6(4) . . . . ? B12 B7 B8 B4 101.2(3) . . . . ? Cl7 B7 B8 B3 -111.1(4) . . . . ? B11 B7 B8 B3 100.7(3) . . . . ? B2 B7 B8 B3 37.8(3) . . . . ? B12 B7 B8 B3 138.3(3) . . . . ? Cl7 B7 B8 B12 110.6(4) . . . . ? B11 B7 B8 B12 -37.6(3) . . . . ? B3 B7 B8 B12 -138.3(3) . . . . ? B2 B7 B8 B12 -100.5(3) . . . . ? Cl7 B7 B8 Cl8 -1.0(5) . . . . ? B11 B7 B8 Cl8 -149.2(3) . . . . ? B3 B7 B8 Cl8 110.1(4) . . . . ? B2 B7 B8 Cl8 147.9(3) . . . . ? B12 B7 B8 Cl8 -111.6(4) . . . . ? B4 B8 B9 B12 -138.1(3) . . . . ? B3 B8 B9 B12 -100.6(3) . . . . ? Cl8 B8 B9 B12 111.9(4) . . . . ? B7 B8 B9 B12 -37.0(3) . . . . ? B4 B8 B9 Cl9 109.6(4) . . . . ? B3 B8 B9 Cl9 147.1(3) . . . . ? B12 B8 B9 Cl9 -112.3(3) . . . . ? Cl8 B8 B9 Cl9 -0.4(5) . . . . ? B7 B8 B9 Cl9 -149.3(3) . . . . ? B4 B8 B9 B10 -100.2(3) . . . . ? B3 B8 B9 B10 -62.7(4) . . . . ? B12 B8 B9 B10 37.9(3) . . . . ? Cl8 B8 B9 B10 149.8(3) . . . . ? B7 B8 B9 B10 0.9(4) . . . . ? B3 B8 B9 B4 37.5(3) . . . . ? B12 B8 B9 B4 138.1(3) . . . . ? Cl8 B8 B9 B4 -110.0(4) . . . . ? B7 B8 B9 B4 101.0(3) . . . . ? B4 B8 B9 B5 -37.0(3) . . . . ? B3 B8 B9 B5 0.5(4) . . . . ? B12 B8 B9 B5 101.1(3) . . . . ? Cl8 B8 B9 B5 -147.0(3) . . . . ? B7 B8 B9 B5 64.1(4) . . . . ? B1 B4 B9 B8 -100.7(3) . . . . ? B5 B4 B9 B8 -138.3(3) . . . . ? B3 B4 B9 B8 -37.5(3) . . . . ? Cl4 B4 B9 B8 111.9(4) . . . . ? B8 B4 B9 B12 37.7(3) . . . . ? B1 B4 B9 B12 -62.9(4) . . . . ? B5 B4 B9 B12 -100.6(3) . . . . ? B3 B4 B9 B12 0.3(4) . . . . ? Cl4 B4 B9 B12 149.6(3) . . . . ? B8 B4 B9 Cl9 -111.3(4) . . . . ? B1 B4 B9 Cl9 148.1(3) . . . . ? B5 B4 B9 Cl9 110.4(3) . . . . ? B3 B4 B9 Cl9 -148.7(3) . . . . ? Cl4 B4 B9 Cl9 0.6(5) . . . . ? B8 B4 B9 B10 101.1(3) . . . . ? B1 B4 B9 B10 0.4(4) . . . . ? B5 B4 B9 B10 -37.3(3) . . . . ? B3 B4 B9 B10 63.6(4) . . . . ? Cl4 B4 B9 B10 -147.1(3) . . . . ? B8 B4 B9 B5 138.3(3) . . . . ? B1 B4 B9 B5 37.6(3) . . . . ? B3 B4 B9 B5 100.9(3) . . . . ? Cl4 B4 B9 B5 -109.8(3) . . . . ? B4 B5 B9 B8 37.0(3) . . . . ? B6 B5 B9 B8 -64.2(4) . . . . ? B10 B5 B9 B8 -101.1(3) . . . . ? Cl5 B5 B9 B8 147.6(3) . . . . ? B1 B5 B9 B8 -0.2(4) . . . . ? B4 B5 B9 B12 100.9(3) . . . . ? B6 B5 B9 B12 -0.4(4) . . . . ? B10 B5 B9 B12 -37.3(3) . . . . ? Cl5 B5 B9 B12 -148.5(3) . . . . ? B1 B5 B9 B12 63.6(4) . . . . ? B4 B5 B9 Cl9 -109.9(4) . . . . ? B6 B5 B9 Cl9 148.9(3) . . . . ? B10 B5 B9 Cl9 112.0(3) . . . . ? Cl5 B5 B9 Cl9 0.8(5) . . . . ? B1 B5 B9 Cl9 -147.1(3) . . . . ? B4 B5 B9 B10 138.1(3) . . . . ? B6 B5 B9 B10 36.9(3) . . . . ? Cl5 B5 B9 B10 -111.2(3) . . . . ? B1 B5 B9 B10 100.9(3) . . . . ? B6 B5 B9 B4 -101.2(3) . . . . ? B10 B5 B9 B4 -138.1(3) . . . . ? Cl5 B5 B9 B4 110.6(3) . . . . ? B1 B5 B9 B4 -37.2(3) . . . . ? B2 B6 B10 B11 37.6(3) . . . . ? B5 B6 B10 B11 137.8(3) . . . . ? Cl6 B6 B10 B11 -110.9(4) . . . . ? B1 B6 B10 B11 100.1(3) . . . . ? B11 B6 B10 B12 -37.0(3) . . . . ? B2 B6 B10 B12 0.6(4) . . . . ? B5 B6 B10 B12 100.8(3) . . . . ? Cl6 B6 B10 B12 -148.0(3) . . . . ? B1 B6 B10 B12 63.1(4) . . . . ? B11 B6 B10 B9 -100.6(3) . . . . ? B2 B6 B10 B9 -62.9(4) . . . . ? B5 B6 B10 B9 37.2(3) . . . . ? Cl6 B6 B10 B9 148.5(3) . . . . ? B1 B6 B10 B9 -0.4(4) . . . . ? B11 B6 B10 B5 -137.8(3) . . . . ? B2 B6 B10 B5 -100.2(3) . . . . ? Cl6 B6 B10 B5 111.3(3) . . . . ? B1 B6 B10 B5 -37.7(3) . . . . ? B11 B6 B10 Cl10 111.2(3) . . . . ? B2 B6 B10 Cl10 148.8(3) . . . . ? B5 B6 B10 Cl10 -111.0(3) . . . . ? Cl6 B6 B10 Cl10 0.3(5) . . . . ? B1 B6 B10 Cl10 -148.7(3) . . . . ? B8 B9 B10 B11 -0.6(4) . . . . ? B12 B9 B10 B11 37.5(3) . . . . ? Cl9 B9 B10 B11 149.3(3) . . . . ? B4 B9 B10 B11 -63.6(4) . . . . ? B5 B9 B10 B11 -100.8(3) . . . . ? B8 B9 B10 B12 -38.1(3) . . . . ? Cl9 B9 B10 B12 111.8(4) . . . . ? B4 B9 B10 B12 -101.1(3) . . . . ? B5 B9 B10 B12 -138.3(3) . . . . ? B8 B9 B10 B6 63.1(4) . . . . ? B12 B9 B10 B6 101.2(3) . . . . ? Cl9 B9 B10 B6 -147.0(3) . . . . ? B4 B9 B10 B6 0.0(4) . . . . ? B5 B9 B10 B6 -37.1(3) . . . . ? B8 B9 B10 B5 100.1(3) . . . . ? B12 B9 B10 B5 138.3(3) . . . . ? Cl9 B9 B10 B5 -109.9(3) . . . . ? B4 B9 B10 B5 37.1(3) . . . . ? B8 B9 B10 Cl10 -148.9(3) . . . . ? B12 B9 B10 Cl10 -110.8(4) . . . . ? Cl9 B9 B10 Cl10 1.1(5) . . . . ? B4 B9 B10 Cl10 148.1(3) . . . . ? B5 B9 B10 Cl10 111.0(3) . . . . ? B4 B5 B10 B11 63.5(4) . . . . ? B6 B5 B10 B11 -37.8(3) . . . . ? Cl5 B5 B10 B11 -148.0(3) . . . . ? B1 B5 B10 B11 0.3(4) . . . . ? B9 B5 B10 B11 100.9(3) . . . . ? B4 B5 B10 B12 -0.1(4) . . . . ? B6 B5 B10 B12 -101.4(3) . . . . ? Cl5 B5 B10 B12 148.4(3) . . . . ? B1 B5 B10 B12 -63.3(4) . . . . ? B9 B5 B10 B12 37.3(3) . . . . ? B4 B5 B10 B6 101.2(3) . . . . ? Cl5 B5 B10 B6 -110.2(4) . . . . ? B1 B5 B10 B6 38.1(3) . . . . ? B9 B5 B10 B6 138.7(3) . . . . ? B4 B5 B10 B9 -37.4(3) . . . . ? B6 B5 B10 B9 -138.7(3) . . . . ? Cl5 B5 B10 B9 111.1(4) . . . . ? B1 B5 B10 B9 -100.6(3) . . . . ? B4 B5 B10 Cl10 -148.5(3) . . . . ? B6 B5 B10 Cl10 110.2(4) . . . . ? Cl5 B5 B10 Cl10 0.0(5) . . . . ? B1 B5 B10 Cl10 148.3(3) . . . . ? B9 B5 B10 Cl10 -111.1(3) . . . . ? B6 B10 B11 B12 -138.8(3) . . . . ? B9 B10 B11 B12 -37.4(3) . . . . ? B5 B10 B11 B12 -101.1(3) . . . . ? Cl10 B10 B11 B12 110.9(4) . . . . ? B12 B10 B11 B6 138.8(3) . . . . ? B9 B10 B11 B6 101.5(3) . . . . ? B5 B10 B11 B6 37.7(3) . . . . ? Cl10 B10 B11 B6 -110.3(4) . . . . ? B12 B10 B11 B2 101.3(3) . . . . ? B6 B10 B11 B2 -37.6(3) . . . . ? B9 B10 B11 B2 63.9(4) . . . . ? B5 B10 B11 B2 0.1(4) . . . . ? Cl10 B10 B11 B2 -147.8(3) . . . . ? B12 B10 B11 B7 37.5(3) . . . . ? B6 B10 B11 B7 -101.3(3) . . . . ? B9 B10 B11 B7 0.2(4) . . . . ? B5 B10 B11 B7 -63.6(4) . . . . ? Cl10 B10 B11 B7 148.4(3) . . . . ? B12 B10 B11 Cl11 -111.9(4) . . . . ? B6 B10 B11 Cl11 109.3(4) . . . . ? B9 B10 B11 Cl11 -149.3(3) . . . . ? B5 B10 B11 Cl11 147.0(3) . . . . ? Cl10 B10 B11 Cl11 -1.0(5) . . . . ? B2 B6 B11 B10 -137.9(3) . . . . ? B5 B6 B11 B10 -37.6(3) . . . . ? Cl6 B6 B11 B10 110.7(4) . . . . ? B1 B6 B11 B10 -100.7(3) . . . . ? B2 B6 B11 B12 -100.9(3) . . . . ? B10 B6 B11 B12 37.0(3) . . . . ? B5 B6 B11 B12 -0.6(4) . . . . ? Cl6 B6 B11 B12 147.7(3) . . . . ? B1 B6 B11 B12 -63.7(4) . . . . ? B10 B6 B11 B2 137.9(3) . . . . ? B5 B6 B11 B2 100.3(3) . . . . ? Cl6 B6 B11 B2 -111.4(4) . . . . ? B1 B6 B11 B2 37.2(3) . . . . ? B2 B6 B11 B7 -36.6(3) . . . . ? B10 B6 B11 B7 101.3(3) . . . . ? B5 B6 B11 B7 63.7(4) . . . . ? Cl6 B6 B11 B7 -148.0(3) . . . . ? B1 B6 B11 B7 0.6(4) . . . . ? B2 B6 B11 Cl11 110.6(3) . . . . ? B10 B6 B11 Cl11 -111.5(3) . . . . ? B5 B6 B11 Cl11 -149.1(3) . . . . ? Cl6 B6 B11 Cl11 -0.8(5) . . . . ? B1 B6 B11 Cl11 147.8(3) . . . . ? B1 B2 B11 B10 -0.5(4) . . . . ? B3 B2 B11 B10 -64.0(4) . . . . ? B6 B2 B11 B10 37.7(3) . . . . ? B7 B2 B11 B10 -101.6(3) . . . . ? Cl2 B2 B11 B10 147.6(3) . . . . ? B1 B2 B11 B12 63.2(4) . . . . ? B3 B2 B11 B12 -0.3(4) . . . . ? B6 B2 B11 B12 101.4(3) . . . . ? B7 B2 B11 B12 -38.0(3) . . . . ? Cl2 B2 B11 B12 -148.8(3) . . . . ? B1 B2 B11 B6 -38.2(3) . . . . ? B3 B2 B11 B6 -101.7(3) . . . . ? B7 B2 B11 B6 -139.4(3) . . . . ? Cl2 B2 B11 B6 109.9(4) . . . . ? B1 B2 B11 B7 101.2(3) . . . . ? B3 B2 B11 B7 37.7(3) . . . . ? B6 B2 B11 B7 139.4(3) . . . . ? Cl2 B2 B11 B7 -110.8(3) . . . . ? B1 B2 B11 Cl11 -147.6(3) . . . . ? B3 B2 B11 Cl11 149.0(3) . . . . ? B6 B2 B11 Cl11 -109.4(4) . . . . ? B7 B2 B11 Cl11 111.3(3) . . . . ? Cl2 B2 B11 Cl11 0.5(5) . . . . ? Cl7 B7 B11 B10 -148.5(3) . . . . ? B3 B7 B11 B10 63.2(4) . . . . ? B2 B7 B11 B10 100.5(3) . . . . ? B8 B7 B11 B10 0.3(4) . . . . ? B12 B7 B11 B10 -37.4(3) . . . . ? Cl7 B7 B11 B12 -111.1(4) . . . . ? B3 B7 B11 B12 100.6(3) . . . . ? B2 B7 B11 B12 137.8(3) . . . . ? B8 B7 B11 B12 37.7(3) . . . . ? Cl7 B7 B11 B6 147.5(3) . . . . ? B3 B7 B11 B6 -0.7(4) . . . . ? B2 B7 B11 B6 36.5(3) . . . . ? B8 B7 B11 B6 -63.6(4) . . . . ? B12 B7 B11 B6 -101.3(3) . . . . ? Cl7 B7 B11 B2 111.0(4) . . . . ? B3 B7 B11 B2 -37.2(3) . . . . ? B8 B7 B11 B2 -100.1(3) . . . . ? B12 B7 B11 B2 -137.8(3) . . . . ? Cl7 B7 B11 Cl11 0.9(5) . . . . ? B3 B7 B11 Cl11 -147.4(3) . . . . ? B2 B7 B11 Cl11 -110.1(4) . . . . ? B8 B7 B11 Cl11 149.7(3) . . . . ? B12 B7 B11 Cl11 112.0(4) . . . . ? B8 B9 B12 B10 137.6(3) . . . . ? Cl9 B9 B12 B10 -111.5(4) . . . . ? B4 B9 B12 B10 100.2(3) . . . . ? B5 B9 B12 B10 37.2(3) . . . . ? B8 B9 B12 B11 100.3(3) . . . . ? Cl9 B9 B12 B11 -148.7(3) . . . . ? B10 B9 B12 B11 -37.3(3) . . . . ? B4 B9 B12 B11 63.0(4) . . . . ? B5 B9 B12 B11 0.0(4) . . . . ? B8 B9 B12 Cl12 -111.1(4) . . . . ? Cl9 B9 B12 Cl12 -0.2(5) . . . . ? B10 B9 B12 Cl12 111.3(4) . . . . ? B4 B9 B12 Cl12 -148.5(3) . . . . ? B5 B9 B12 Cl12 148.5(3) . . . . ? Cl9 B9 B12 B8 110.9(4) . . . . ? B10 B9 B12 B8 -137.6(3) . . . . ? B4 B9 B12 B8 -37.4(3) . . . . ? B5 B9 B12 B8 -100.4(3) . . . . ? B8 B9 B12 B7 37.0(3) . . . . ? Cl9 B9 B12 B7 147.9(3) . . . . ? B10 B9 B12 B7 -100.7(3) . . . . ? B4 B9 B12 B7 -0.4(4) . . . . ? B5 B9 B12 B7 -63.4(4) . . . . ? B11 B10 B12 B9 -138.1(3) . . . . ? B6 B10 B12 B9 -101.1(3) . . . . ? B5 B10 B12 B9 -37.5(3) . . . . ? Cl10 B10 B12 B9 110.9(3) . . . . ? B6 B10 B12 B11 37.0(3) . . . . ? B9 B10 B12 B11 138.1(3) . . . . ? B5 B10 B12 B11 100.6(3) . . . . ? Cl10 B10 B12 B11 -111.0(3) . . . . ? B11 B10 B12 Cl12 110.0(4) . . . . ? B6 B10 B12 Cl12 147.1(3) . . . . ? B9 B10 B12 Cl12 -111.8(4) . . . . ? B5 B10 B12 Cl12 -149.3(3) . . . . ? Cl10 B10 B12 Cl12 -0.9(5) . . . . ? B11 B10 B12 B8 -100.6(3) . . . . ? B6 B10 B12 B8 -63.5(4) . . . . ? B9 B10 B12 B8 37.6(3) . . . . ? B5 B10 B12 B8 0.1(4) . . . . ? Cl10 B10 B12 B8 148.4(3) . . . . ? B11 B10 B12 B7 -37.1(3) . . . . ? B6 B10 B12 B7 -0.1(4) . . . . ? B9 B10 B12 B7 101.0(3) . . . . ? B5 B10 B12 B7 63.5(4) . . . . ? Cl10 B10 B12 B7 -148.1(3) . . . . ? B10 B11 B12 B9 37.5(3) . . . . ? B6 B11 B12 B9 0.4(4) . . . . ? B2 B11 B12 B9 -63.2(4) . . . . ? B7 B11 B12 B9 -101.0(3) . . . . ? Cl11 B11 B12 B9 148.1(3) . . . . ? B6 B11 B12 B10 -37.1(3) . . . . ? B2 B11 B12 B10 -100.6(3) . . . . ? B7 B11 B12 B10 -138.5(3) . . . . ? Cl11 B11 B12 B10 110.6(4) . . . . ? B10 B11 B12 Cl12 -111.5(4) . . . . ? B6 B11 B12 Cl12 -148.6(3) . . . . ? B2 B11 B12 Cl12 147.8(3) . . . . ? B7 B11 B12 Cl12 110.0(4) . . . . ? Cl11 B11 B12 Cl12 -0.9(5) . . . . ? B10 B11 B12 B8 100.4(3) . . . . ? B6 B11 B12 B8 63.3(4) . . . . ? B2 B11 B12 B8 -0.3(4) . . . . ? B7 B11 B12 B8 -38.1(3) . . . . ? Cl11 B11 B12 B8 -149.0(3) . . . . ? B10 B11 B12 B7 138.5(3) . . . . ? B6 B11 B12 B7 101.4(3) . . . . ? B2 B11 B12 B7 37.8(3) . . . . ? Cl11 B11 B12 B7 -110.9(4) . . . . ? B4 B8 B12 B9 37.9(3) . . . . ? B3 B8 B12 B9 101.5(3) . . . . ? Cl8 B8 B12 B9 -109.8(4) . . . . ? B7 B8 B12 B9 138.8(3) . . . . ? B9 B8 B12 B10 -37.8(3) . . . . ? B4 B8 B12 B10 0.0(4) . . . . ? B3 B8 B12 B10 63.7(4) . . . . ? Cl8 B8 B12 B10 -147.7(3) . . . . ? B7 B8 B12 B10 101.0(3) . . . . ? B9 B8 B12 B11 -100.8(3) . . . . ? B4 B8 B12 B11 -62.9(4) . . . . ? B3 B8 B12 B11 0.7(4) . . . . ? Cl8 B8 B12 B11 149.4(3) . . . . ? B7 B8 B12 B11 38.0(3) . . . . ? B9 B8 B12 Cl12 111.5(4) . . . . ? B4 B8 B12 Cl12 149.4(3) . . . . ? B3 B8 B12 Cl12 -147.0(3) . . . . ? Cl8 B8 B12 Cl12 1.7(5) . . . . ? B7 B8 B12 Cl12 -109.7(4) . . . . ? B9 B8 B12 B7 -138.8(3) . . . . ? B4 B8 B12 B7 -100.9(3) . . . . ? B3 B8 B12 B7 -37.3(3) . . . . ? Cl8 B8 B12 B7 111.4(3) . . . . ? Cl7 B7 B12 B9 -149.0(3) . . . . ? B11 B7 B12 B9 100.6(3) . . . . ? B3 B7 B12 B9 0.4(4) . . . . ? B2 B7 B12 B9 63.1(4) . . . . ? B8 B7 B12 B9 -36.7(3) . . . . ? Cl7 B7 B12 B10 147.4(3) . . . . ? B11 B7 B12 B10 37.0(3) . . . . ? B3 B7 B12 B10 -63.2(4) . . . . ? B2 B7 B12 B10 -0.5(4) . . . . ? B8 B7 B12 B10 -100.3(3) . . . . ? Cl7 B7 B12 B11 110.4(4) . . . . ? B3 B7 B12 B11 -100.2(3) . . . . ? B2 B7 B12 B11 -37.5(3) . . . . ? B8 B7 B12 B11 -137.3(3) . . . . ? Cl7 B7 B12 Cl12 -0.3(5) . . . . ? B11 B7 B12 Cl12 -110.7(3) . . . . ? B3 B7 B12 Cl12 149.1(3) . . . . ? B2 B7 B12 Cl12 -148.1(3) . . . . ? B8 B7 B12 Cl12 112.0(3) . . . . ? Cl7 B7 B12 B8 -112.3(4) . . . . ? B11 B7 B12 B8 137.3(3) . . . . ? B3 B7 B12 B8 37.1(3) . . . . ? B2 B7 B12 B8 99.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.760 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.108 #===END data_ck012 _database_code_depnum_ccdc_archive 'CCDC 715826' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H30 N P2), B12 Cl12, 2(C H2 Cl2)' _chemical_formula_sum 'C74 H64 B12 Cl16 N2 P4' _chemical_formula_weight 1802.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 13.794(2) _cell_length_b 13.794(2) _cell_length_c 12.613(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2078.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 113(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 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 914 _exptl_absorpt_coefficient_mu 0.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8921 _exptl_absorpt_correction_T_max 0.9379 _exptl_absorpt_process_details ; March 2001 T Higashi ; _exptl_special_details ; March 2001 T Higashi ; _diffrn_ambient_temperature 113(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 18471 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 22.58 _reflns_number_total 1835 _reflns_number_gt 1485 _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. The [PPN]+ cations are disordered over three positions. The central N and the disordered P atoms were found from the difference Fourier map. Some C atoms of the disordered phenyl rings were also found and the missing atoms were added by AFIX command. All non-hydrogen atoms were refined anisotropically. In addition the structure contains disordered CH2Cl2 solvent molecules. All non-hydrogen atoms were found from the difference Fourier map and were refined anisotropically. ; _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^)+(0.0305P)^2^+1.4920P] 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 refU _refine_ls_extinction_method ? _refine_ls_number_reflns 1835 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Cl1 Cl 0.14612(6) 0.28632(6) 0.44813(6) 0.0427(3) Uani 1 1 d . . . Cl2 Cl 0.09007(6) 0.17774(6) 0.71901(6) 0.0434(3) Uani 1 1 d . . . B1 B 0.0712(3) 0.1396(2) 0.4751(3) 0.0343(8) Uani 1 1 d . . . B2 B 0.0436(3) 0.0861(3) 0.6072(3) 0.0352(8) Uani 1 1 d . . . P1 P 0.60268(18) 0.19815(18) 0.06749(17) 0.0325(5) Uani 0.33 1 d P . . N1 N 0.6667 0.3333 0.1078(4) 0.0623(14) Uani 1 3 d S . . P2 P 0.71943(18) 0.28028(18) 0.15460(17) 0.0334(5) Uani 0.33 1 d P . . C1 C 0.6934(6) 0.1737(6) -0.0152(5) 0.036(2) Uani 0.33 1 d PG A 1 C2 C 0.7006(7) 0.0776(6) -0.0071(6) 0.057(3) Uani 0.33 1 d PG A 1 H2 H 0.6575 0.0226 0.0446 0.072(6) Uiso 0.33 1 calc PR A 1 C3 C 0.7706(9) 0.0615(9) -0.0741(8) 0.069(4) Uani 0.33 1 d PG A 1 H3 H 0.7756 -0.0046 -0.0685 0.072(6) Uiso 0.33 1 calc PR A 1 C4 C 0.8334(11) 0.1415(11) -0.1493(9) 0.057(9) Uani 0.33 1 d PG A 1 H4 H 0.8816 0.1305 -0.1953 0.072(6) Uiso 0.33 1 calc PR A 1 C5 C 0.8262(10) 0.2377(10) -0.1574(10) 0.063(7) Uani 0.33 1 d PG A 1 H5 H 0.8693 0.2927 -0.2090 0.072(6) Uiso 0.33 1 calc PR A 1 C6 C 0.7561(7) 0.2538(7) -0.0904(7) 0.053(3) Uani 0.33 1 d PG A 1 H6 H 0.7512 0.3198 -0.0960 0.072(6) Uiso 0.33 1 calc PR A 1 C1A C 0.8252(13) 0.3080(9) -0.0074(11) 0.041(5) Uani 0.33 1 d PG B 2 C2A C 0.7872(12) 0.2010(11) 0.0308(11) 0.054(5) Uani 0.33 1 d PG B 2 H2A H 0.7534 0.1805 0.0989 0.072(6) Uiso 0.33 1 calc PR B 2 C3A C 0.7985(15) 0.1237(14) -0.0301(10) 0.056(5) Uani 0.33 1 d PG B 2 H3A H 0.7724 0.0502 -0.0039 0.072(6) Uiso 0.33 1 calc PR B 2 C4A C 0.8477(17) 0.1536(14) -0.1292(12) 0.049(12) Uani 0.33 1 d PG B 2 H4A H 0.8555 0.1006 -0.1710 0.072(6) Uiso 0.33 1 calc PR B 2 C5A C 0.8858(13) 0.2607(11) -0.1674(12) 0.064(5) Uani 0.33 1 d PG B 2 H5A H 0.9196 0.2812 -0.2355 0.072(6) Uiso 0.33 1 calc PR B 2 C6A C 0.8745(10) 0.3379(8) -0.1065(9) 0.045(3) Uani 0.33 1 d PG B 2 H6A H 0.9006 0.4114 -0.1327 0.072(6) Uiso 0.33 1 calc PR B 2 C1B C 0.7752(10) 0.2345(10) 0.0485(8) 0.040(4) Uani 0.33 1 d PG A 3 C2B C 0.7790(8) 0.1372(9) 0.0532(10) 0.047(3) Uani 0.33 1 d PG A 3 H2B H 0.7547 0.0923 0.1154 0.072(6) Uiso 0.33 1 calc PR A 3 C3B C 0.8178(14) 0.1046(11) -0.0317(14) 0.056(6) Uani 0.33 1 d PG A 3 H3B H 0.8205 0.0372 -0.0285 0.072(6) Uiso 0.33 1 calc PR A 3 C4B C 0.8528(17) 0.1693(14) -0.1214(13) 0.070(12) Uani 0.33 1 d PG A 3 H4B H 0.8798 0.1467 -0.1803 0.072(6) Uiso 0.33 1 calc PR A 3 C5B C 0.8490(14) 0.2666(13) -0.1261(11) 0.072(7) Uani 0.33 1 d PG A 3 H5B H 0.8733 0.3114 -0.1883 0.072(6) Uiso 0.33 1 calc PR A 3 C6B C 0.8102(11) 0.2992(10) -0.0412(10) 0.043(5) Uani 0.33 1 d PG A 3 H6B H 0.8076 0.3666 -0.0444 0.072(6) Uiso 0.33 1 calc PR A 3 C7 C 0.8984(6) 0.4563(7) 0.1757(6) 0.031(2) Uani 0.33 1 d PG C 4 C8 C 0.9767(9) 0.4230(8) 0.1919(8) 0.055(3) Uani 0.33 1 d PG C 4 H8 H 0.9832 0.3746 0.1424 0.072(6) Uiso 0.33 1 calc PR C 4 C9 C 1.0455(13) 0.4601(13) 0.2801(10) 0.073(8) Uani 0.33 1 d PG C 4 H9 H 1.0992 0.4372 0.2912 0.072(6) Uiso 0.33 1 calc PR C 4 C10 C 1.0360(14) 0.5306(15) 0.3522(12) 0.040(6) Uani 0.33 1 d PG C 4 H10 H 1.0833 0.5561 0.4127 0.072(6) Uiso 0.33 1 calc PR C 4 C11 C 0.9577(12) 0.5639(13) 0.3360(11) 0.047(5) Uani 0.33 1 d PG C 4 H11 H 0.9512 0.6123 0.3855 0.072(6) Uiso 0.33 1 calc PR C 4 C12 C 0.8889(8) 0.5268(10) 0.2478(8) 0.041(3) Uani 0.33 1 d PG C 4 H12 H 0.8352 0.5496 0.2367 0.072(6) Uiso 0.33 1 calc PR C 4 C7A C 0.8366(9) 0.4659(11) 0.2360(9) 0.037(4) Uani 0.33 1 d PG D 2 C8A C 0.8895(11) 0.4039(11) 0.2176(9) 0.042(4) Uani 0.33 1 d PG D 2 H8A H 0.8656 0.3518 0.1607 0.072(6) Uiso 0.33 1 calc PR D 2 C9A C 0.9775(13) 0.4184(14) 0.2824(11) 0.046(6) Uani 0.33 1 d PG D 2 H9A H 1.0136 0.3761 0.2698 0.072(6) Uiso 0.33 1 calc PR D 2 C10A C 1.0126(15) 0.4948(15) 0.3658(11) 0.082(11) Uani 0.33 1 d PG D 2 H10A H 1.0726 0.5046 0.4101 0.072(6) Uiso 0.33 1 calc PR D 2 C11A C 0.9597(15) 0.5567(12) 0.3843(8) 0.042(4) Uani 0.33 1 d PG D 2 H11A H 0.9836 0.6088 0.4411 0.072(6) Uiso 0.33 1 calc PR D 2 C12A C 0.8717(11) 0.5423(11) 0.3194(8) 0.044(4) Uani 0.33 1 d PG D 2 H12A H 0.8356 0.5845 0.3320 0.072(6) Uiso 0.33 1 calc PR D 2 C7B C 0.8330(8) 0.3769(10) 0.2363(8) 0.040(4) Uani 0.33 1 d PG E 3 C8B C 0.9280(10) 0.3697(9) 0.2504(10) 0.039(3) Uani 0.33 1 d PG E 3 H8B H 0.9353 0.3125 0.2156 0.072(6) Uiso 0.33 1 calc PR E 3 C9B C 1.0126(12) 0.4453(13) 0.3146(13) 0.051(6) Uani 0.33 1 d PG E 3 H9B H 1.0783 0.4403 0.3243 0.072(6) Uiso 0.33 1 calc PR E 3 C10B C 1.0022(12) 0.5280(15) 0.3648(15) 0.056(8) Uani 0.33 1 d PG E 3 H10B H 1.0606 0.5802 0.4092 0.072(6) Uiso 0.33 1 calc PR E 3 C11B C 0.9072(11) 0.5352(13) 0.3507(14) 0.057(6) Uani 0.33 1 d PG E 3 H11B H 0.8999 0.5924 0.3854 0.072(6) Uiso 0.33 1 calc PR E 3 C12B C 0.8226(10) 0.4596(12) 0.2865(10) 0.045(4) Uani 0.33 1 d PG E 3 H12B H 0.7569 0.4646 0.2768 0.072(6) Uiso 0.33 1 calc PR E 3 C20 C 0.7029(11) 0.325(5) 0.5443(9) 0.15(2) Uani 0.33 1 d P . . H20A H 0.6534 0.3521 0.5171 0.06(3) Uiso 0.33 1 calc PR . . H20B H 0.7786 0.3912 0.5370 0.06(3) Uiso 0.33 1 calc PR . . Cl21 Cl 0.7063(3) 0.2882(2) 0.4706(3) 0.0745(9) Uani 0.33 1 d P . . Cl22 Cl 0.6882(11) 0.3497(14) 0.6723(2) 0.132(4) Uani 0.33 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 Cl1 0.0446(5) 0.0317(4) 0.0480(5) 0.0026(3) 0.0021(3) 0.0161(4) Cl2 0.0451(5) 0.0427(5) 0.0424(5) -0.0086(3) -0.0038(3) 0.0219(4) B1 0.0340(18) 0.0272(18) 0.039(2) -0.0036(14) -0.0016(15) 0.0134(15) B2 0.0363(18) 0.0324(19) 0.038(2) -0.0010(15) -0.0011(15) 0.0176(15) P1 0.0322(12) 0.0321(12) 0.0314(12) -0.0112(10) -0.0074(10) 0.0146(10) N1 0.067(2) 0.067(2) 0.053(3) 0.000 0.000 0.0334(11) P2 0.0424(14) 0.0358(13) 0.0291(12) 0.0038(10) -0.0009(10) 0.0248(11) C1 0.034(5) 0.048(6) 0.026(5) -0.003(4) -0.007(4) 0.020(5) C2 0.066(8) 0.074(8) 0.057(7) -0.005(6) 0.005(7) 0.054(7) C3 0.083(12) 0.114(14) 0.049(9) -0.015(9) -0.003(8) 0.078(11) C4 0.055(13) 0.09(2) 0.034(11) -0.038(12) -0.010(9) 0.042(14) C5 0.047(10) 0.075(13) 0.035(11) -0.021(9) -0.002(8) 0.007(8) C6 0.052(8) 0.063(8) 0.039(8) -0.009(6) -0.001(6) 0.025(7) C1A 0.044(9) 0.054(10) 0.032(9) -0.005(8) -0.005(8) 0.029(8) C2A 0.067(10) 0.022(9) 0.069(11) 0.007(7) 0.028(7) 0.020(8) C3A 0.066(14) 0.051(9) 0.061(15) 0.000(8) 0.012(10) 0.038(9) C4A 0.05(2) 0.05(2) 0.05(2) -0.007(14) -0.012(17) 0.032(17) C5A 0.093(15) 0.056(10) 0.051(11) 0.005(8) 0.014(8) 0.044(11) C6A 0.056(8) 0.036(7) 0.040(8) -0.004(6) 0.003(6) 0.022(7) C1B 0.046(7) 0.033(9) 0.036(7) 0.006(7) -0.007(6) 0.016(7) C2B 0.034(6) 0.037(7) 0.067(9) -0.016(7) -0.002(6) 0.016(6) C3B 0.036(9) 0.059(11) 0.071(15) -0.020(9) 0.015(8) 0.023(9) C4B 0.07(2) 0.07(2) 0.05(2) -0.045(16) 0.023(15) 0.021(17) C5B 0.071(17) 0.094(19) 0.028(10) -0.003(12) 0.001(11) 0.025(17) C6B 0.059(13) 0.045(10) 0.019(8) 0.020(7) 0.022(10) 0.022(9) C7 0.030(5) 0.028(6) 0.039(6) 0.011(5) 0.010(5) 0.018(5) C8 0.063(9) 0.074(9) 0.044(8) -0.017(6) -0.018(6) 0.047(7) C9 0.092(15) 0.112(17) 0.061(15) -0.023(11) -0.023(11) 0.087(14) C10 0.047(13) 0.059(12) 0.030(8) -0.014(8) -0.002(8) 0.039(9) C11 0.035(11) 0.061(11) 0.027(11) -0.021(8) 0.000(8) 0.010(8) C12 0.036(8) 0.045(8) 0.047(8) 0.007(7) 0.017(7) 0.025(6) C7A 0.036(8) 0.027(9) 0.042(10) 0.004(8) 0.004(7) 0.011(7) C8A 0.066(15) 0.036(11) 0.037(10) -0.016(7) -0.026(9) 0.034(12) C9A 0.034(11) 0.065(11) 0.047(14) -0.029(10) -0.031(9) 0.029(10) C10A 0.09(2) 0.10(2) 0.06(2) -0.012(13) -0.042(17) 0.046(17) C11A 0.041(11) 0.045(8) 0.029(10) -0.007(7) -0.007(8) 0.014(8) C12A 0.053(9) 0.036(9) 0.033(10) 0.001(7) -0.008(7) 0.014(7) C7B 0.052(9) 0.050(9) 0.026(6) 0.009(5) 0.007(6) 0.031(8) C8B 0.040(9) 0.040(8) 0.038(9) -0.007(6) -0.014(6) 0.020(7) C9B 0.052(14) 0.063(14) 0.039(12) -0.017(10) -0.034(14) 0.029(12) C10B 0.018(13) 0.092(19) 0.044(15) -0.016(13) 0.009(10) 0.016(10) C11B 0.083(17) 0.058(12) 0.039(12) -0.002(8) -0.001(14) 0.041(12) C12B 0.059(9) 0.048(10) 0.032(9) 0.001(8) -0.001(7) 0.029(8) C20 0.044(10) 0.28(4) 0.042(7) -0.045(19) -0.006(7) 0.025(12) Cl21 0.107(2) 0.0584(17) 0.067(2) 0.0035(15) 0.0203(18) 0.0479(18) Cl22 0.109(5) 0.172(6) 0.0620(18) -0.068(4) -0.004(5) 0.030(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 Cl1 B1 1.785(3) . ? Cl2 B2 1.785(3) . ? B1 B1 1.783(4) 6_556 ? B1 B1 1.783(4) 5_556 ? B1 B2 1.785(4) . ? B1 B2 1.786(4) 5_556 ? B1 B2 1.792(4) 6_556 ? B2 B2 1.781(5) 2 ? B2 B2 1.781(5) 3 ? B2 B1 1.786(4) 6_556 ? B2 B1 1.792(4) 5_556 ? P1 N1 1.694(3) . ? P1 C1 1.786(7) . ? P1 C7 1.788(8) 3_665 ? P1 C1A 1.788(9) 3_665 ? P1 P2 1.806(3) . ? P1 P2 1.868(3) 3_665 ? P1 C6B 2.04(4) 3_665 ? P1 C1B 2.186(12) . ? P1 C1B 2.198(11) 3_665 ? P1 C7B 2.242(11) 3_665 ? P1 C8A 2.25(5) 3_665 ? P1 C7A 2.249(11) 3_665 ? N1 P2 1.395(3) . ? N1 P2 1.395(3) 3_665 ? N1 P2 1.395(3) 2_655 ? N1 P1 1.694(3) 2_655 ? N1 P1 1.694(3) 3_665 ? P2 C7A 1.788(10) 3_665 ? P2 C7B 1.790(10) . ? P2 C1B 1.807(10) . ? P2 P1 1.868(3) 2_655 ? P2 C12B 2.11(3) 3_665 ? P2 P2 2.190(4) 3_665 ? P2 P2 2.190(4) 2_655 ? P2 C8A 2.246(13) . ? P2 C12 2.34(3) 3_665 ? P2 C2A 2.352(10) . ? C1 C2 1.383(7) . ? C1 C6 1.383(7) . ? C2 C3 1.383(7) . ? C2 H2 0.9500 . ? C3 C4 1.383(7) . ? C3 H3 0.9500 . ? C4 C5 1.383(7) . ? C4 H4 0.9500 . ? C5 C6 1.383(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C1A C2A 1.384(9) . ? C1A C6A 1.384(9) . ? C1A P1 1.788(9) 2_655 ? C2A C3A 1.384(9) . ? C2A H2A 0.9500 . ? C3A C4A 1.384(9) . ? C3A H3A 0.9500 . ? C4A C5A 1.384(9) . ? C4A H4A 0.9500 . ? C5A C6A 1.384(9) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C1B C2B 1.370(8) . ? C1B C6B 1.370(8) . ? C1B P1 2.198(11) 2_655 ? C2B C3B 1.370(8) . ? C2B H2B 0.9500 . ? C3B C4B 1.370(8) . ? C3B H3B 0.9500 . ? C4B C5B 1.370(8) . ? C4B H4B 0.9500 . ? C5B C6B 1.370(8) . ? C5B H5B 0.9500 . ? C6B P1 2.042(12) 2_655 ? C6B H6B 0.9500 . ? C7 C8 1.384(9) . ? C7 C12 1.384(9) . ? C7 P1 1.788(8) 2_655 ? C8 C9 1.384(9) . ? C8 H8 0.9500 . ? C9 C10 1.384(9) . ? C9 H9 0.9500 . ? C10 C11 1.384(9) . ? C10 H10 0.9500 . ? C11 C12 1.384(9) . ? C11 H11 0.9500 . ? C12 P2 2.338(11) 2_655 ? C12 H12 0.9500 . ? C7A C8A 1.393(8) . ? C7A C12A 1.393(8) . ? C7A P2 1.788(10) 2_655 ? C7A P1 2.249(11) 2_655 ? C8A C9A 1.393(8) . ? C8A P1 2.248(12) 2_655 ? C8A H8A 0.9500 . ? C9A C10A 1.393(8) . ? C9A H9A 0.9500 . ? C10A C11A 1.393(8) . ? C10A H10A 0.9500 . ? C11A C12A 1.393(8) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C7B C8B 1.374(10) . ? C7B C12B 1.374(10) . ? C7B P1 2.242(11) 2_655 ? C7B P2 2.363(13) 2_655 ? C8B C9B 1.374(10) . ? C8B H8B 0.9500 . ? C9B C10B 1.374(10) . ? C9B H9B 0.9500 . ? C10B C11B 1.374(10) . ? C10B H10B 0.9500 . ? C11B C12B 1.374(10) . ? C11B H11B 0.9500 . ? C12B P2 2.112(12) 2_655 ? C12B H12B 0.9500 . ? C20 Cl21 1.07(4) . ? C20 Cl22 1.68(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? Cl21 C20 1.54(6) 3_665 ? Cl21 Cl21 1.756(5) 2_655 ? Cl21 Cl21 1.756(5) 3_665 ? Cl21 C20 1.765(19) 2_655 ? Cl22 Cl22 0.47(2) 3_665 ? Cl22 Cl22 0.47(2) 2_655 ? Cl22 C20 1.692(14) 2_655 ? Cl22 C20 1.82(2) 3_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 B1 B1 B1 108.3(2) 6_556 5_556 ? B1 B1 B2 60.1(2) 6_556 . ? B1 B1 B2 60.3(2) 5_556 . ? B1 B1 Cl1 121.8(2) 6_556 . ? B1 B1 Cl1 121.8(2) 5_556 . ? B2 B1 Cl1 122.0(2) . . ? B1 B1 B2 107.86(16) 6_556 5_556 ? B1 B1 B2 60.02(16) 5_556 5_556 ? B2 B1 B2 108.2(2) . 5_556 ? Cl1 B1 B2 121.4(2) . 5_556 ? B1 B1 B2 107.80(16) 5_556 6_556 ? B2 B1 B2 107.9(2) . 6_556 ? Cl1 B1 B2 121.6(2) . 6_556 ? B2 B1 B2 59.7(2) 5_556 6_556 ? B2 B2 B2 60.0 2 3 ? B2 B2 B1 108.19(16) 2 . ? B2 B2 B1 107.97(16) 3 . ? B2 B2 Cl2 122.07(15) 2 . ? B2 B2 Cl2 122.10(15) 3 . ? B1 B2 Cl2 121.2(2) . . ? B2 B2 B1 108.17(18) 3 6_556 ? B1 B2 B1 59.89(14) . 6_556 ? Cl2 B2 B1 121.6(2) . 6_556 ? B2 B2 B1 107.90(18) 2 5_556 ? Cl2 B2 B1 121.7(2) . 5_556 ? B1 B2 B1 107.7(3) 6_556 5_556 ? N1 P1 C1 110.8(3) . . ? N1 P1 C7 112.7(3) . 3_665 ? C1 P1 C7 108.6(4) . 3_665 ? N1 P1 C1A 106.4(5) . 3_665 ? C1 P1 C1A 109.2(5) . 3_665 ? C7 P1 C1A 109.0(6) 3_665 3_665 ? C1 P1 P2 89.1(2) . . ? C7 P1 P2 82.6(3) 3_665 . ? C1A P1 P2 152.7(5) 3_665 . ? C1 P1 P2 156.5(3) . 3_665 ? C7 P1 P2 84.7(3) 3_665 3_665 ? C1A P1 P2 83.2(4) 3_665 3_665 ? P2 P1 P2 73.16(15) . 3_665 ? N1 P1 C6B 103.1(9) . 3_665 ? C1 P1 C6B 100.8(7) . 3_665 ? C7 P1 C6B 120.1(9) 3_665 3_665 ? P2 P1 C6B 149.6(9) . 3_665 ? P2 P1 C6B 88.1(8) 3_665 3_665 ? N1 P1 C1B 82.7(3) . . ? C7 P1 C1B 100.7(4) 3_665 . ? C1A P1 C1B 141.8(5) 3_665 . ? P2 P1 C1B 52.8(3) . . ? P2 P1 C1B 123.9(3) 3_665 . ? C6B P1 C1B 131.1(8) 3_665 . ? N1 P1 C1B 82.3(3) . 3_665 ? C1 P1 C1B 137.9(4) . 3_665 ? C7 P1 C1B 101.7(4) 3_665 3_665 ? P2 P1 C1B 123.8(3) . 3_665 ? P2 P1 C1B 52.0(3) 3_665 3_665 ? C1B P1 C1B 156.5(4) . 3_665 ? N1 P1 C7B 82.3(3) . 3_665 ? C1 P1 C7B 137.6(4) . 3_665 ? C1A P1 C7B 104.7(6) 3_665 3_665 ? P2 P1 C7B 70.5(3) . 3_665 ? C6B P1 C7B 115.6(8) 3_665 3_665 ? C1B P1 C7B 113.3(4) . 3_665 ? C1B P1 C7B 82.3(4) 3_665 3_665 ? N1 P1 C8A 100.6(11) . 3_665 ? C1 P1 C8A 129.2(10) . 3_665 ? C1A P1 C8A 98.3(13) 3_665 3_665 ? P2 P1 C8A 84.2(13) . 3_665 ? C6B P1 C8A 109.9(14) 3_665 3_665 ? C1B P1 C8A 116.8(11) . 3_665 ? C1B P1 C8A 83.7(11) 3_665 3_665 ? N1 P1 C7A 84.3(3) . 3_665 ? C1 P1 C7A 107.9(4) . 3_665 ? C1A P1 C7A 134.1(6) 3_665 3_665 ? P2 P1 C7A 72.9(3) 3_665 3_665 ? C6B P1 C7A 145.5(8) 3_665 3_665 ? C1B P1 C7A 83.0(4) . 3_665 ? C1B P1 C7A 113.3(4) 3_665 3_665 ? P2 N1 P2 103.4(2) . 3_665 ? P2 N1 P2 103.4(2) . 2_655 ? P2 N1 P2 103.4(2) 3_665 2_655 ? P2 N1 P1 70.78(12) . . ? P2 N1 P1 73.70(12) 3_665 . ? P2 N1 P1 172.2(3) 2_655 . ? P2 N1 P1 73.70(12) . 2_655 ? P2 N1 P1 172.2(3) 3_665 2_655 ? P2 N1 P1 70.78(12) 2_655 2_655 ? P1 N1 P1 111.40(16) . 2_655 ? P2 N1 P1 172.2(3) . 3_665 ? P2 N1 P1 70.78(12) 3_665 3_665 ? P2 N1 P1 73.70(12) 2_655 3_665 ? P1 N1 P1 111.40(16) . 3_665 ? P1 N1 P1 111.40(16) 2_655 3_665 ? N1 P2 C7A 113.9(4) . 3_665 ? N1 P2 C7B 110.2(5) . . ? C7A P2 C7B 107.2(5) 3_665 . ? C7A P2 P1 77.5(4) 3_665 . ? C7B P2 P1 172.5(5) . . ? N1 P2 C1B 107.1(4) . . ? C7A P2 C1B 109.6(6) 3_665 . ? C7B P2 C1B 108.6(5) . . ? P1 P2 C1B 74.5(4) . . ? N1 P2 P1 60.50(13) . 2_655 ? C7A P2 P1 174.4(4) 3_665 2_655 ? C7B P2 P1 75.6(4) . 2_655 ? P1 P2 P1 99.24(17) . 2_655 ? C1B P2 P1 73.4(4) . 2_655 ? N1 P2 C12B 116.0(8) . 3_665 ? C7B P2 C12B 91.4(8) . 3_665 ? P1 P2 C12B 92.6(7) . 3_665 ? C1B P2 C12B 121.9(8) . 3_665 ? P1 P2 C12B 163.0(6) 2_655 3_665 ? C7A P2 P2 75.9(4) 3_665 3_665 ? C7B P2 P2 120.1(4) . 3_665 ? C1B P2 P2 126.9(3) . 3_665 ? P1 P2 P2 98.55(10) 2_655 3_665 ? C12B P2 P2 78.4(8) 3_665 3_665 ? C7A P2 P2 123.7(4) 3_665 2_655 ? C7B P2 P2 72.1(5) . 2_655 ? P1 P2 P2 100.53(11) . 2_655 ? C1B P2 P2 124.2(4) . 2_655 ? C12B P2 P2 113.8(7) 3_665 2_655 ? P2 P2 P2 60.0 3_665 2_655 ? N1 P2 C8A 111.8(3) . . ? C7A P2 C8A 118.3(5) 3_665 . ? P1 P2 C8A 163.2(3) . . ? C1B P2 C8A 93.5(5) . . ? C12B P2 C8A 103.8(8) 3_665 . ? P2 P2 C8A 131.6(3) 3_665 . ? P2 P2 C8A 76.2(3) 2_655 . ? N1 P2 C12 128.3(7) . 3_665 ? C7B P2 C12 105.0(8) . 3_665 ? P1 P2 C12 81.2(8) . 3_665 ? C1B P2 C12 95.7(10) . 3_665 ? P1 P2 C12 168.5(9) 2_655 3_665 ? P2 P2 C12 91.1(7) 3_665 3_665 ? P2 P2 C12 139.3(9) 2_655 3_665 ? C8A P2 C12 112.3(8) . 3_665 ? N1 P2 C2A 113.3(4) . . ? C7A P2 C2A 102.8(6) 3_665 . ? C7B P2 C2A 108.9(5) . . ? P1 P2 C2A 75.0(4) . . ? P1 P2 C2A 80.5(4) 2_655 . ? C12B P2 C2A 114.6(8) 3_665 . ? P2 P2 C2A 129.1(4) 3_665 . ? P2 P2 C2A 131.6(4) 2_655 . ? C8A P2 C2A 94.6(5) . . ? C12 P2 C2A 88.5(10) 3_665 . ? C2 C1 C6 120.0 . . ? C2 C1 P1 122.1(4) . . ? C6 C1 P1 117.9(4) . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C2A C1A C6A 120.0 . . ? C2A C1A P1 119.8(7) . 2_655 ? C6A C1A P1 120.0(7) . 2_655 ? C1A C2A C3A 120.0 . . ? C1A C2A P2 76.2(6) . . ? C3A C2A P2 161.9(7) . . ? C1A C2A H2A 120.0 . . ? C3A C2A H2A 120.0 . . ? C2A C3A C4A 120.0 . . ? C2A C3A H3A 120.0 . . ? C4A C3A H3A 120.0 . . ? C5A C4A C3A 120.0 . . ? C5A C4A H4A 120.0 . . ? C3A C4A H4A 120.0 . . ? C4A C5A C6A 120.0 . . ? C4A C5A H5A 120.0 . . ? C6A C5A H5A 120.0 . . ? C1A C6A C5A 120.0 . . ? C1A C6A H6A 120.0 . . ? C5A C6A H6A 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B P2 122.8(7) . . ? C6B C1B P2 117.2(7) . . ? C2B C1B P1 109.9(6) . . ? C6B C1B P1 103.2(5) . . ? C2B C1B P1 166.5(7) . 2_655 ? C1B C2B C3B 120.0 . . ? C1B C2B H2B 120.0 . . ? C3B C2B H2B 120.0 . . ? C4B C3B C2B 120.0 . . ? C4B C3B H3B 120.0 . . ? C2B C3B H3B 120.0 . . ? C3B C4B C5B 120.0 . . ? C3B C4B H4B 120.0 . . ? C5B C4B H4B 120.0 . . ? C6B C5B C4B 120.0 . . ? C6B C5B H5B 120.0 . . ? C4B C5B H5B 120.0 . . ? C5B C6B C1B 120.0 . . ? C5B C6B P1 158.2(7) . 2_655 ? C5B C6B H6B 120.0 . . ? C1B C6B H6B 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 P1 121.9(6) . 2_655 ? C12 C7 P1 118.0(6) . 2_655 ? C9 C8 C7 120.0 . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 120.0 . . ? C11 C12 P2 156.6(5) . 2_655 ? C7 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C8A C7A C12A 120.0 . . ? C8A C7A P2 118.2(8) . 2_655 ? C12A C7A P2 121.7(8) . 2_655 ? C8A C7A P1 71.9(6) . 2_655 ? C12A C7A P1 157.8(7) . 2_655 ? C9A C8A C7A 120.0 . . ? C9A C8A P2 145.2(7) . . ? C7A C8A P2 81.7(7) . . ? C9A C8A P1 157.8(8) . 2_655 ? C7A C8A P1 72.0(6) . 2_655 ? C9A C8A H8A 120.0 . . ? C7A C8A H8A 120.0 . . ? P2 C8A H8A 47.4 . . ? P1 C8A H8A 51.9 2_655 . ? C8A C9A C10A 120.0 . . ? C8A C9A H9A 120.0 . . ? C10A C9A H9A 120.0 . . ? C11A C10A C9A 120.0 . . ? C11A C10A H10A 120.0 . . ? C9A C10A H10A 120.0 . . ? C10A C11A C12A 120.0 . . ? C10A C11A H11A 120.0 . . ? C12A C11A H11A 120.0 . . ? C7A C12A C11A 120.0 . . ? C7A C12A H12A 120.0 . . ? C11A C12A H12A 120.0 . . ? C8B C7B C12B 120.0 . . ? C8B C7B P2 122.2(9) . . ? C12B C7B P2 117.8(9) . . ? C8B C7B P1 113.9(6) . 2_655 ? C12B C7B P1 100.8(8) . 2_655 ? C8B C7B P2 155.5(5) . 2_655 ? C7B C8B C9B 120.0 . . ? C7B C8B H8B 120.0 . . ? C9B C8B H8B 120.0 . . ? C8B C9B C10B 120.0 . . ? C8B C9B H9B 120.0 . . ? C10B C9B H9B 120.0 . . ? C11B C10B C9B 120.0 . . ? C11B C10B H10B 120.0 . . ? C9B C10B H10B 120.0 . . ? C12B C11B C10B 120.0 . . ? C12B C11B H11B 120.0 . . ? C10B C11B H11B 120.0 . . ? C11B C12B C7B 120.0 . . ? C11B C12B P2 145.6(8) . 2_655 ? C7B C12B P2 82.5(8) . 2_655 ? C11B C12B H12B 120.0 . . ? C7B C12B H12B 120.0 . . ? Cl21 C20 Cl22 165(5) . . ? Cl21 C20 H20A 94.6 . . ? Cl22 C20 H20A 94.6 . . ? Cl21 C20 H20B 94.6 . . ? Cl22 C20 H20B 94.6 . . ? H20A C20 H20B 103.2 . . ? C20 Cl21 Cl21 60(3) . 2_655 ? C20 Cl21 Cl21 64.4(7) 3_665 2_655 ? C20 Cl21 Cl21 72.8(15) . 3_665 ? Cl21 Cl21 Cl21 60.000(1) 2_655 3_665 ? Cl21 Cl21 C20 51.9(18) 3_665 2_655 ? Cl22 Cl22 Cl22 60.000(6) 3_665 2_655 ? Cl22 Cl22 C20 83(2) 3_665 . ? Cl22 Cl22 C20 99.3(10) 2_655 . ? Cl22 Cl22 C20 98(2) 3_665 2_655 ? Cl22 Cl22 C20 81(2) 2_655 2_655 ? Cl22 Cl22 C20 66.0(9) 3_665 3_665 ? Cl22 Cl22 C20 67(2) 2_655 3_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 B1 B1 B2 B2 -100.5(2) 5_556 . . 2 ? Cl1 B1 B2 B2 148.5(2) . . . 2 ? B1 B1 B2 B2 101.0(2) 6_556 . . 3 ? Cl1 B1 B2 B2 -148.1(2) . . . 3 ? B1 B1 B2 Cl2 -110.9(2) 6_556 . . . ? B1 B1 B2 Cl2 111.0(2) 5_556 . . . ? B2 B1 B2 Cl2 148.6(2) 5_556 . . . ? B2 B1 B2 Cl2 -148.3(2) 6_556 . . . ? B1 B1 B2 B1 -138.08(18) 5_556 . . 6_556 ? Cl1 B1 B2 B1 110.9(3) . . . 6_556 ? B2 B1 B2 B1 -100.55(14) 5_556 . . 6_556 ? B1 B1 B2 B1 138.08(18) 6_556 . . 5_556 ? Cl1 B1 B2 B1 -111.0(3) . . . 5_556 ? B2 B1 B2 B1 100.67(13) 6_556 . . 5_556 ? C1A P1 N1 P2 173.6(5) 3_665 . . . ? P2 P1 N1 P2 110.9(3) 3_665 . . . ? C6B P1 N1 P2 -174.9(7) 3_665 . . . ? C1B P1 N1 P2 153.7(3) 3_665 . . . ? C1 P1 N1 P2 -178.7(3) . . . 3_665 ? P2 P1 N1 P2 -110.9(3) . . . 3_665 ? C1B P1 N1 P2 -155.3(3) . . . 3_665 ? C7 P1 N1 P1 117.0(4) 3_665 . . 2_655 ? C1A P1 N1 P1 -123.6(5) 3_665 . . 2_655 ? P2 P1 N1 P1 173.8(4) 3_665 . . 2_655 ? C6B P1 N1 P1 -112.1(7) 3_665 . . 2_655 ? C1B P1 N1 P1 -143.4(3) 3_665 . . 2_655 ? C7B P1 N1 P1 133.3(4) 3_665 . . 2_655 ? C8A P1 N1 P1 134.4(11) 3_665 . . 2_655 ? C7A P1 N1 P1 102.1(4) 3_665 . . 2_655 ? C1 P1 N1 P1 120.1(3) . . . 3_665 ? C7 P1 N1 P1 -117.9(4) 3_665 . . 3_665 ? P2 P1 N1 P1 -172.1(3) . . . 3_665 ? C1B P1 N1 P1 143.5(4) . . . 3_665 ? C7B P1 N1 P1 -101.6(4) 3_665 . . 3_665 ? C8A P1 N1 P1 -100.5(11) 3_665 . . 3_665 ? C7A P1 N1 P1 -132.8(4) 3_665 . . 3_665 ? P2 N1 P2 C7A 114.7(4) 2_655 . . 3_665 ? P1 N1 P2 C7A 179.7(5) 2_655 . . 3_665 ? P2 N1 P2 C7B -113.4(3) 3_665 . . . ? P1 N1 P2 C7B 179.4(4) . . . . ? P1 N1 P2 P1 -120.3(2) 2_655 . . . ? P2 N1 P2 C1B 128.6(5) 3_665 . . . ? P2 N1 P2 C1B -123.9(5) 2_655 . . . ? P2 N1 P2 P1 -172.6(3) 3_665 . . 2_655 ? P1 N1 P2 P1 120.3(2) . . . 2_655 ? P2 N1 P2 C12B 96.1(7) 2_655 . . 3_665 ? P1 N1 P2 C12B -78.6(7) . . . 3_665 ? P1 N1 P2 C12B 161.1(7) 2_655 . . 3_665 ? P2 N1 P2 P2 107.5(4) 2_655 . . 3_665 ? P1 N1 P2 P2 172.6(3) 2_655 . . 3_665 ? P2 N1 P2 P2 -107.5(4) 3_665 . . 2_655 ? P1 N1 P2 P2 -174.7(3) . . . 2_655 ? P2 N1 P2 C8A -130.3(3) 3_665 . . . ? P1 N1 P2 C8A 162.6(4) . . . . ? P2 N1 P2 C12 124.0(11) 2_655 . . 3_665 ? P1 N1 P2 C12 -171.0(12) 2_655 . . 3_665 ? P2 N1 P2 C2A 124.2(5) 3_665 . . . ? P2 N1 P2 C2A -128.3(5) 2_655 . . . ? C1 P1 P2 N1 120.0(3) . . . . ? C7 P1 P2 N1 -131.1(4) 3_665 . . . ? C1B P1 P2 N1 119.4(4) . . . . ? C7B P1 P2 N1 -97.8(4) 3_665 . . . ? C8A P1 P2 N1 -110.4(10) 3_665 . . . ? C7A P1 P2 N1 -125.8(5) 3_665 . . . ? N1 P1 P2 C7A 125.8(5) . . . 3_665 ? C1 P1 P2 C7A -114.1(5) . . . 3_665 ? C1A P1 P2 C7A 112.3(11) 3_665 . . 3_665 ? P2 P1 P2 C7A 81.4(4) 3_665 . . 3_665 ? C6B P1 P2 C7A 135.6(15) 3_665 . . 3_665 ? C1B P1 P2 C7A -114.7(6) . . . 3_665 ? C1B P1 P2 C7A 93.9(5) 3_665 . . 3_665 ? N1 P1 P2 C1B -119.4(4) . . . . ? C7 P1 P2 C1B 109.5(5) 3_665 . . . ? C1A P1 P2 C1B -133.0(12) 3_665 . . . ? P2 P1 P2 C1B -163.8(4) 3_665 . . . ? C6B P1 P2 C1B -109.6(16) 3_665 . . . ? C1B P1 P2 C1B -151.3(6) 3_665 . . . ? C7B P1 P2 C1B 142.7(5) 3_665 . . . ? C8A P1 P2 C1B 130.2(10) 3_665 . . . ? C7A P1 P2 C1B 114.7(6) 3_665 . . . ? C1 P1 P2 P1 70.4(2) . . . 2_655 ? C7 P1 P2 P1 179.3(3) 3_665 . . 2_655 ? P2 P1 P2 P1 -93.98(12) 3_665 . . 2_655 ? C1B P1 P2 P1 -81.5(3) 3_665 . . 2_655 ? C7B P1 P2 P1 -147.4(3) 3_665 . . 2_655 ? C8A P1 P2 P1 -160.0(9) 3_665 . . 2_655 ? C7A P1 P2 P1 -175.4(4) 3_665 . . 2_655 ? N1 P1 P2 C12B 118.2(8) . . . 3_665 ? C1 P1 P2 C12B -121.8(8) . . . 3_665 ? C1A P1 P2 C12B 104.6(13) 3_665 . . 3_665 ? P2 P1 P2 C12B 73.8(8) 3_665 . . 3_665 ? C6B P1 P2 C12B 127.9(16) 3_665 . . 3_665 ? C1B P1 P2 C12B -122.4(8) . . . 3_665 ? C1B P1 P2 C12B 86.2(8) 3_665 . . 3_665 ? C1 P1 P2 P2 164.4(3) . . . 3_665 ? C7 P1 P2 P2 -86.7(3) 3_665 . . 3_665 ? C1B P1 P2 P2 163.8(4) . . . 3_665 ? C7A P1 P2 P2 -81.4(4) 3_665 . . 3_665 ? C1 P1 P2 P2 123.4(2) . . . 2_655 ? C7 P1 P2 P2 -127.7(3) 3_665 . . 2_655 ? C1B P1 P2 P2 122.8(4) . . . 2_655 ? C7B P1 P2 P2 -94.5(3) 3_665 . . 2_655 ? C8A P1 P2 P2 -107.0(9) 3_665 . . 2_655 ? C7A P1 P2 P2 -122.5(4) 3_665 . . 2_655 ? C7 P1 P2 C8A 155.2(11) 3_665 . . . ? C1A P1 P2 C8A -87.3(16) 3_665 . . . ? P2 P1 P2 C8A -118.1(11) 3_665 . . . ? C1B P1 P2 C8A -105.6(12) 3_665 . . . ? C7B P1 P2 C8A -171.5(13) 3_665 . . . ? C8A P1 P2 C8A 175.9(10) 3_665 . . . ? C7A P1 P2 C8A 160.5(10) 3_665 . . . ? N1 P1 P2 C12 142.1(9) . . . 3_665 ? C1 P1 P2 C12 -97.9(9) . . . 3_665 ? C1A P1 P2 C12 128.5(14) 3_665 . . 3_665 ? P2 P1 P2 C12 97.7(9) 3_665 . . 3_665 ? C6B P1 P2 C12 151.9(16) 3_665 . . 3_665 ? C1B P1 P2 C12 -98.5(9) . . . 3_665 ? C1B P1 P2 C12 110.2(9) 3_665 . . 3_665 ? C7A P1 P2 C12 16.2(10) 3_665 . . 3_665 ? N1 P1 P2 C2A -127.1(4) . . . . ? C7 P1 P2 C2A 101.8(5) 3_665 . . . ? C1A P1 P2 C2A -140.7(13) 3_665 . . . ? P2 P1 P2 C2A -171.5(4) 3_665 . . . ? C6B P1 P2 C2A -117.3(15) 3_665 . . . ? C1B P1 P2 C2A -159.0(5) 3_665 . . . ? C7B P1 P2 C2A 135.1(5) 3_665 . . . ? C8A P1 P2 C2A 122.5(10) 3_665 . . . ? C7A P1 P2 C2A 107.1(6) 3_665 . . . ? N1 P1 C1 C2 139.0(4) . . . . ? C1A P1 C1 C2 -104.1(7) 3_665 . . . ? P2 P1 C1 C2 96.5(4) . . . . ? P2 P1 C1 C2 136.7(6) 3_665 . . . ? C6B P1 C1 C2 -112.4(10) 3_665 . . . ? C1B P1 C1 C2 97.3(7) . . . . ? C1B P1 C1 C2 -119.2(6) 3_665 . . . ? C7 P1 C1 C6 -166.5(5) 3_665 . . . ? C1B P1 C1 C6 -83.8(7) . . . . ? C7B P1 C1 C6 -143.8(6) 3_665 . . . ? C8A P1 C1 C6 -166.4(17) 3_665 . . . ? C7A P1 C1 C6 -132.7(5) 3_665 . . . ? P1 C1 C2 C3 178.9(6) . . . . ? P1 C1 C6 C5 -178.9(6) . . . . ? P1 C1A C2A C3A 175.7(13) 2_655 . . . ? C6A C1A C2A P2 -171.2(10) . . . . ? C7A P2 C2A C1A 171.7(6) 3_665 . . . ? C7B P2 C2A C1A -74.8(6) . . . . ? P1 P2 C2A C1A 98.5(5) . . . . ? C12B P2 C2A C1A -175.5(9) 3_665 . . . ? P2 P2 C2A C1A 89.6(6) 3_665 . . . ? C12 P2 C2A C1A 179.8(9) 3_665 . . . ? N1 P2 C2A C3A -107(3) . . . . ? C7A P2 C2A C3A 17(3) 3_665 . . . ? C7B P2 C2A C3A 130(3) . . . . ? C1B P2 C2A C3A -141(7) . . . . ? P1 P2 C2A C3A -158(3) 2_655 . . . ? P2 P2 C2A C3A -65(3) 3_665 . . . ? P2 P2 C2A C3A -147(2) 2_655 . . . ? C8A P2 C2A C3A 137(3) . . . . ? P2 C2A C3A C4A 151(3) . . . . ? P1 C1A C6A C5A -175.7(13) 2_655 . . . ? N1 P2 C1B C2B -145.0(7) . . . . ? C7B P2 C1B C2B 96.0(9) . . . . ? P1 P2 C1B C2B -91.1(8) . . . . ? P1 P2 C1B C2B 164.0(8) 2_655 . . . ? P2 P2 C1B C2B -107.7(8) 3_665 . . . ? P2 P2 C1B C2B 176.6(6) 2_655 . . . ? C8A P2 C1B C2B 100.8(8) . . . . ? C7A P2 C1B C6B 156.4(6) 3_665 . . . ? C7B P2 C1B C6B -86.7(7) . . . . ? P1 P2 C1B C6B 86.1(5) . . . . ? P1 P2 C1B C6B -18.7(5) 2_655 . . . ? C12B P2 C1B C6B 169.4(10) 3_665 . . . ? C8A P2 C1B C6B -81.9(6) . . . . ? C12 P2 C1B C6B 165.3(9) 3_665 . . . ? C2A P2 C1B C6B 180(5) . . . . ? C7A P2 C1B P1 70.3(5) 3_665 . . . ? C7B P2 C1B P1 -172.9(5) . . . . ? P1 P2 C1B P1 -104.9(2) 2_655 . . . ? C12B P2 C1B P1 83.3(9) 3_665 . . . ? P2 P2 C1B P1 -92.3(3) 2_655 . . . ? C8A P2 C1B P1 -168.0(4) . . . . ? C12 P2 C1B P1 79.2(8) 3_665 . . . ? C2A P2 C1B P1 93(5) . . . . ? N1 P2 C1B P1 51.0(2) . . . 2_655 ? C7A P2 C1B P1 175.1(4) 3_665 . . 2_655 ? P1 P2 C1B P1 104.9(2) . . . 2_655 ? C12B P2 C1B P1 -171.8(9) 3_665 . . 2_655 ? P2 P2 C1B P1 88.3(4) 3_665 . . 2_655 ? C12 P2 C1B P1 -176.0(8) 3_665 . . 2_655 ? C2A P2 C1B P1 -162(5) . . . 2_655 ? N1 P1 C1B C2B 156.5(6) . . . . ? C1A P1 C1B C2B -96.2(10) 3_665 . . . ? P2 P1 C1B C2B 116.6(7) . . . . ? P2 P1 C1B C2B 135.3(5) 3_665 . . . ? C6B P1 C1B C2B -102.6(14) 3_665 . . . ? C1B P1 C1B C2B -153.1(12) 3_665 . . . ? C7 P1 C1B C6B 173.8(6) 3_665 . . . ? P2 P1 C1B C6B -114.2(7) . . . . ? P2 P1 C1B C6B -95.5(5) 3_665 . . . ? C7B P1 C1B C6B -152.7(5) 3_665 . . . ? C8A P1 C1B C6B -172.5(13) 3_665 . . . ? C7A P1 C1B C6B -159.5(6) 3_665 . . . ? C1 P1 C1B P2 -179.0(7) . . . . ? C7 P1 C1B P2 -72.0(4) 3_665 . . . ? C1A P1 C1B P2 147.2(9) 3_665 . . . ? C6B P1 C1B P2 140.8(12) 3_665 . . . ? C1B P1 C1B P2 90.3(13) 3_665 . . . ? C1 P1 C1B P1 127.8(6) . . . 2_655 ? C7 P1 C1B P1 -125.2(3) 3_665 . . 2_655 ? C1A P1 C1B P1 93.9(10) 3_665 . . 2_655 ? C6B P1 C1B P1 87.6(13) 3_665 . . 2_655 ? C7B P1 C1B P1 -91.7(4) 3_665 . . 2_655 ? C8A P1 C1B P1 -111.5(12) 3_665 . . 2_655 ? C7A P1 C1B P1 -98.5(4) 3_665 . . 2_655 ? P2 C1B C2B C3B 177.2(10) . . . . ? P1 C1B C2B C3B 119.4(7) . . . . ? P1 C1B C2B C3B -109(3) 2_655 . . . ? C4B C5B C6B P1 140(2) . . . 2_655 ? P2 C1B C6B C5B -177.3(10) . . . . ? P1 C1B C6B C5B -122.7(8) . . . . ? P1 C1B C6B C5B 165.9(8) 2_655 . . . ? C2B C1B C6B P1 -165.9(8) . . . 2_655 ? P1 C1B C6B P1 71.4(5) . . . 2_655 ? P1 C7 C8 C9 -176.3(8) 2_655 . . . ? P1 C7 C12 C11 176.4(8) 2_655 . . . ? C8 C7 C12 P2 -159.7(6) . . . 2_655 ? P1 C7 C12 P2 16.7(4) 2_655 . . 2_655 ? C10 C11 C12 P2 122.8(14) . . . 2_655 ? P2 C7A C8A C9A -177.0(11) 2_655 . . . ? P1 C7A C8A C9A 159.5(8) 2_655 . . . ? C12A C7A C8A P2 151.0(8) . . . . ? C12A C7A C8A P1 -159.5(8) . . . 2_655 ? N1 P2 C8A C9A 165.8(11) . . . . ? C7B P2 C8A C9A 79(3) . . . . ? P1 P2 C8A C9A -127.8(12) . . . . ? C1B P2 C8A C9A -84.1(12) . . . . ? P1 P2 C8A C9A -154.1(12) 2_655 . . . ? C12B P2 C8A C9A 40.0(13) 3_665 . . . ? P2 P2 C8A C9A 126.6(11) 3_665 . . . ? P2 P2 C8A C9A 151.5(12) 2_655 . . . ? C2A P2 C8A C9A -76.8(12) . . . . ? C7A P2 C8A C7A -102.2(8) 3_665 . . . ? P1 P2 C8A C7A 99.6(11) . . . . ? C1B P2 C8A C7A 143.3(6) . . . . ? P1 P2 C8A C7A 73.3(5) 2_655 . . . ? C12B P2 C8A C7A -92.6(8) 3_665 . . . ? C12 P2 C8A C7A -119.0(10) 3_665 . . . ? C2A P2 C8A C7A 150.7(6) . . . . ? C7A P2 C8A P1 -175.5(5) 3_665 . . 2_655 ? C7B P2 C8A P1 -127(2) . . . 2_655 ? C12B P2 C8A P1 -165.9(8) 3_665 . . 2_655 ? P2 P2 C8A P1 -79.3(3) 3_665 . . 2_655 ? C12 P2 C8A P1 167.7(10) 3_665 . . 2_655 ? C2A P2 C8A P1 77.4(4) . . . 2_655 ? P2 C8A C9A C10A -122.7(13) . . . . ? P1 C8A C9A C10A 118.0(16) 2_655 . . . ? P2 C7A C12A C11A 176.8(11) 2_655 . . . ? P1 C7A C12A C11A -118(2) 2_655 . . . ? N1 P2 C7B C8B -148.2(6) . . . . ? C7A P2 C7B C8B 87.3(6) 3_665 . . . ? P1 P2 C7B C8B -97.7(6) 2_655 . . . ? C12B P2 C7B C8B 93.4(11) 3_665 . . . ? P2 P2 C7B C8B 170.7(5) 3_665 . . . ? P2 P2 C7B C8B -152.0(7) 2_655 . . . ? C7A P2 C7B C12B -92.1(8) 3_665 . . . ? C1B P2 C7B C12B 149.5(6) . . . . ? P1 P2 C7B C12B 82.9(6) 2_655 . . . ? C12B P2 C7B C12B -86.1(9) 3_665 . . . ? C8A P2 C7B C12B 131(3) . . . . ? C12 P2 C7B C12B -109.0(11) 3_665 . . . ? C2A P2 C7B C12B 157.3(6) . . . . ? C7A P2 C7B P1 -175.0(5) 3_665 . . 2_655 ? C12B P2 C7B P1 -168.9(8) 3_665 . . 2_655 ? P2 P2 C7B P1 -91.6(2) 3_665 . . 2_655 ? C12 P2 C7B P1 168.1(9) 3_665 . . 2_655 ? C2A P2 C7B P1 74.4(5) . . . 2_655 ? C7A P2 C7B P2 -120.7(5) 3_665 . . 2_655 ? C1B P2 C7B P2 120.9(4) . . . 2_655 ? C12B P2 C7B P2 -114.6(8) 3_665 . . 2_655 ? C8A P2 C7B P2 103(2) . . . 2_655 ? C12 P2 C7B P2 -137.6(9) 3_665 . . 2_655 ? C2A P2 C7B P2 128.8(4) . . . 2_655 ? P2 C7B C8B C9B -179.4(9) . . . . ? P1 C7B C8B C9B 119.6(8) 2_655 . . . ? P2 C7B C8B C9B 88.6(17) 2_655 . . . ? C10B C11B C12B P2 -125.0(12) . . . 2_655 ? P2 C7B C12B C11B 179.4(9) . . . . ? P1 C7B C12B C11B -126.0(6) 2_655 . . . ? P2 C7B C12B C11B -152.2(6) 2_655 . . . ? C8B C7B C12B P2 152.1(6) . . . 2_655 ? Cl22 C20 Cl21 C20 84(6) . . . 3_665 ? Cl22 C20 Cl21 C20 143(7) . . . 2_655 ? Cl21 C20 Cl22 C20 -147(6) . . . 2_655 ? Cl21 C20 Cl22 C20 -86(6) . . . 3_665 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 22.58 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.222 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.038