#------------------------------------------------------------------------------ #$Date: 2016-02-16 20:30:59 +0000 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: svn://www.crystallography.net/cod/cif/4/11/63/4116317.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4116317 loop_ _publ_author_name 'John Reglinski' 'Mark D. Spicer' 'Mark Garner' 'Alan R. Kennedy' _publ_contact_author ; Dr. J. Reglinski Department of Pure and Applied Chemistry University of Strathclyde 295 Cathedral Street GLASGOW G1 1XL UK ; _publ_section_title ; Structural Consequences of the Use of Hard and Soft Tripodal Ligands during Metathesis Reactions: Synthesis of the [Bis(hydrotris(methimazolyl)borato]bismuth(III) [Bis(hydrotris(pyrazolyl)borato]sodiate ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 2317 _journal_page_last 2318 _journal_paper_doi 10.1021/ja983637f _journal_volume 121 _journal_year 1999 _chemical_formula_analytical 'C24 H32 B2 Bi0.5 cl5 N12 Na0.5 S3' _chemical_formula_sum 'C48 H64 B4 Bi Cl10 N24 Na S6' _chemical_formula_weight 899.65 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_date 'Tue Oct 6 13:34:56 1998' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 109.21(3) _cell_angle_beta 95.38(3) _cell_angle_gamma 114.22(2) _cell_formula_units_Z 2 _cell_length_a 12.968(4) _cell_length_b 13.279(5) _cell_length_c 12.825(3) _cell_measurement_reflns_used 20 _cell_measurement_temperature 123.2 _cell_measurement_theta_max 20.4 _cell_measurement_theta_min 13.5 _cell_volume 1833.6(12) _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_data_reduction teXsan _computing_publication_material teXsan _computing_structure_refinement teXsan _computing_structure_solution SIR-92 _diffrn_ambient_temperature 123.2 _diffrn_measurement_device AFC7S _diffrn_measurement_method 'omega/2-theta scans' _diffrn_orient_matrix_UB_11 -0.00214 _diffrn_orient_matrix_UB_12 -0.07680 _diffrn_orient_matrix_UB_13 -0.00210 _diffrn_orient_matrix_UB_21 -0.03501 _diffrn_orient_matrix_UB_22 -0.03894 _diffrn_orient_matrix_UB_23 -0.08476 _diffrn_orient_matrix_UB_31 0.08039 _diffrn_orient_matrix_UB_32 0.02723 _diffrn_orient_matrix_UB_33 -0.01215 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoKalpha _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 3.19 _diffrn_reflns_av_sigmaI/netI 0.051 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7014 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% -1.99 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 29.94 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.636 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_meas 0.000 _exptl_crystal_description plate _exptl_crystal_F_000 900.00 _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.450 _exptl_crystal_size_min 0.100 _refine_diff_density_max 1.70 _refine_diff_density_min -2.75 _refine_ls_extinction_coef 1.60513 _refine_ls_extinction_method Zachariasen_type_2_gaussian_isotropic _refine_ls_goodness_of_fit_obs 1.412 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 431 _refine_ls_number_reflns 5047 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_obs 0.0538 _refine_ls_shift/esd_max 0.195 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme unit _refine_ls_wR_factor_all 0.1093 _refine_ls_wR_factor_obs 0.0641 _reflns_number_observed 5047 _reflns_number_total 6413 _reflns_observed_criterion 2.00 _cod_data_source_file ja983637f.cif _cod_data_source_block C48H64B4BiCl10N24NaS6 _cod_original_cell_volume 1833(1) _cod_original_sg_symbol_H-M 'P -1 ' _cod_original_formula_sum 'C48 H64 B4 Bi Cl10 N24 Na S6 ' _cod_database_code 4116317 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Bi(1) 0.0230(3) 0.0309(3) 0.0122(3) 0.0116(2) 0.0074(2) 0.0106(2) Cl(1) 0.063(2) 0.084(3) 0.082(3) 0.030(2) 0.010(2) -0.029(2) Cl(2) 0.064(2) 0.110(3) 0.107(3) 0.034(2) 0.031(2) 0.072(3) Cl(3) 0.084(2) 0.050(2) 0.038(2) 0.016(2) 0.025(2) 0.009(1) Cl(4) 0.044(2) 0.042(2) 0.038(1) 0.012(1) 0.006(1) 0.008(1) Cl(5) 0.145(5) 0.139(5) 0.118(4) 0.058(4) 0.022(4) 0.050(4) S(1) 0.030(1) 0.031(1) 0.023(1) 0.014(1) 0.0105(9) 0.016(1) S(2) 0.029(1) 0.033(1) 0.016(1) 0.012(1) 0.0039(9) 0.0083(10) S(3) 0.024(1) 0.031(1) 0.017(1) 0.013(1) 0.0070(9) 0.0100(9) Na(1) 0.031(3) 0.024(3) 0.023(3) 0.011(2) 0.003(2) 0.005(2) N(1) 0.024(4) 0.028(4) 0.015(3) 0.013(3) 0.011(3) 0.012(3) N(2) 0.022(4) 0.036(4) 0.024(4) 0.012(3) 0.007(3) 0.016(3) N(3) 0.026(4) 0.023(4) 0.015(3) 0.010(3) 0.009(3) 0.009(3) N(4) 0.031(4) 0.027(4) 0.018(4) 0.015(4) 0.008(3) 0.007(3) N(5) 0.025(4) 0.023(4) 0.011(3) 0.011(3) 0.006(3) 0.007(3) N(6) 0.023(4) 0.023(4) 0.016(3) 0.007(3) 0.003(3) 0.006(3) N(7) 0.022(4) 0.027(4) 0.019(4) 0.008(3) 0.003(3) 0.010(3) N(8) 0.035(4) 0.023(4) 0.024(4) 0.011(4) 0.004(3) 0.007(3) N(9) 0.028(4) 0.021(4) 0.021(4) 0.009(3) 0.008(3) 0.010(3) N(10) 0.026(4) 0.035(5) 0.021(4) 0.014(4) 0.003(3) 0.011(3) N(11) 0.021(4) 0.027(4) 0.027(4) 0.009(3) 0.004(3) 0.012(3) N(12) 0.027(4) 0.038(5) 0.026(4) 0.014(4) 0.004(3) 0.007(4) C(1) 0.023(5) 0.025(5) 0.022(4) 0.013(4) 0.010(4) 0.009(4) C(2) 0.030(5) 0.030(5) 0.024(5) 0.009(4) 0.013(4) 0.014(4) C(3) 0.020(5) 0.040(6) 0.028(5) 0.009(4) 0.009(4) 0.017(4) C(4) 0.030(5) 0.065(8) 0.041(6) 0.025(5) 0.009(5) 0.033(6) C(5) 0.028(5) 0.029(5) 0.014(4) 0.015(4) 0.009(3) 0.013(4) C(6) 0.034(5) 0.035(5) 0.019(4) 0.016(4) 0.007(4) 0.018(4) C(7) 0.030(5) 0.036(5) 0.024(5) 0.016(4) 0.006(4) 0.015(4) C(8) 0.042(6) 0.031(6) 0.033(5) 0.020(5) 0.011(5) -0.001(4) C(9) 0.021(4) 0.022(4) 0.008(4) 0.007(4) -0.001(3) 0.003(3) C(10) 0.026(5) 0.025(5) 0.016(4) 0.008(4) 0.002(4) 0.002(4) C(11) 0.030(5) 0.024(5) 0.018(4) 0.013(4) 0.004(4) 0.005(4) C(12) 0.030(5) 0.033(6) 0.034(5) 0.008(5) 0.011(4) 0.015(5) C(13) 0.030(5) 0.038(6) 0.018(4) 0.010(4) 0.001(4) 0.008(4) C(14) 0.032(5) 0.041(6) 0.032(5) 0.007(5) 0.001(4) 0.021(5) C(15) 0.035(6) 0.037(6) 0.040(6) 0.015(5) 0.006(5) 0.023(5) C(16) 0.037(5) 0.023(5) 0.029(5) 0.016(4) 0.011(4) 0.015(4) C(17) 0.028(5) 0.046(6) 0.035(5) 0.020(5) 0.015(4) 0.029(5) C(18) 0.024(5) 0.039(6) 0.022(5) 0.011(4) 0.004(4) 0.016(4) C(19) 0.030(5) 0.041(6) 0.052(6) 0.018(5) 0.015(5) 0.028(5) C(20) 0.049(7) 0.060(8) 0.056(7) 0.033(6) 0.032(6) 0.040(6) C(21) 0.047(6) 0.066(8) 0.029(5) 0.037(6) 0.017(5) 0.022(5) C(22) 0.058(8) 0.043(7) 0.041(6) 0.016(6) 0.015(6) 0.005(5) C(23) 0.047(6) 0.047(7) 0.035(6) 0.021(6) 0.015(5) 0.024(5) B(1) 0.034(6) 0.032(6) 0.011(4) 0.019(5) 0.011(4) 0.011(4) B(2) 0.028(5) 0.024(5) 0.021(5) 0.012(5) 0.009(4) 0.009(4) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Bi(1) 0.5000 0.0000 0.5000 0.0216 Uij Cl(1) 0.3935(3) -0.5746(4) 0.6990(4) 0.0966 Uij Cl(2) 0.2767(3) -0.4290(4) 0.7035(4) 0.0874 Uij Cl(3) -0.1090(3) -0.2397(3) 1.2725(3) 0.0644 Uij Cl(4) -0.0835(2) -0.4225(3) 1.0915(2) 0.0466 Uij Cl(5) 0.9692(6) 0.3667(6) 0.5880(5) 0.1380 Uij S(1) 0.3979(2) 0.1237(2) 0.6375(2) 0.0263 Uij S(2) 0.3658(2) -0.2058(2) 0.5375(2) 0.0275 Uij S(3) 0.6830(2) 0.0787(2) 0.6897(2) 0.0237 Uij Na(1) 0.0000 0.0000 1.0000 0.0285 Uij N(1) 0.3376(6) -0.0262(6) 0.7554(6) 0.0210 Uij N(2) 0.1916(6) -0.0483(7) 0.6356(6) 0.0265 Uij N(3) 0.4888(6) -0.1037(6) 0.7662(6) 0.0213 Uij N(4) 0.5226(7) -0.2427(7) 0.6525(6) 0.0254 Uij N(5) 0.5549(6) 0.1244(6) 0.8455(5) 0.0198 Uij N(6) 0.6871(6) 0.2845(6) 0.8309(6) 0.0225 Uij N(7) -0.1352(6) -0.2318(7) 0.7392(6) 0.0241 Uij N(8) -0.0960(7) -0.1101(7) 0.7872(6) 0.0290 Uij N(9) -0.0117(6) -0.2685(6) 0.8753(6) 0.0234 Uij N(10) 0.0551(7) -0.1600(7) 0.9653(6) 0.0279 Uij N(11) -0.2124(6) -0.2927(7) 0.8955(6) 0.0258 Uij N(12) -0.1855(7) -0.1850(7) 0.9804(6) 0.0324 Uij C(1) 0.3089(7) 0.0133(8) 0.6777(7) 0.0225 Uij C(2) 0.2349(8) -0.1131(8) 0.7605(8) 0.0286 Uij C(3) 0.1445(8) -0.1262(9) 0.6869(8) 0.0300 Uij C(4) 0.1258(9) -0.037(1) 0.5460(9) 0.0407 Uij C(5) 0.4624(8) -0.1816(8) 0.6555(7) 0.0215 Uij C(6) 0.5676(8) -0.1189(9) 0.8320(7) 0.0272 Uij C(7) 0.5896(8) -0.2046(9) 0.7618(8) 0.0291 Uij C(8) 0.5155(9) -0.3368(9) 0.5490(8) 0.0378 Uij C(9) 0.6391(7) 0.1622(8) 0.7890(6) 0.0192 Uij C(10) 0.5541(8) 0.2263(8) 0.9213(7) 0.0258 Uij C(11) 0.6336(8) 0.3255(8) 0.9123(7) 0.0252 Uij C(12) 0.7780(9) 0.3608(9) 0.7923(8) 0.0345 Uij C(13) -0.1809(8) -0.2769(9) 0.6239(7) 0.0321 Uij C(14) -0.1729(9) -0.1831(10) 0.5961(8) 0.0374 Uij C(15) -0.1193(9) -0.0820(9) 0.6996(9) 0.0358 Uij C(16) 0.0436(8) -0.3380(8) 0.8584(8) 0.0274 Uij C(17) 0.1493(8) -0.2723(9) 0.9410(8) 0.0312 Uij C(18) 0.1522(8) -0.1640(9) 1.0046(7) 0.0290 Uij C(19) -0.3110(9) -0.3831(10) 0.8971(9) 0.0373 Uij C(20) -0.348(1) -0.334(1) 0.988(1) 0.0459 Uij C(21) -0.2691(10) -0.212(1) 1.0366(9) 0.0417 Uij C(22) 0.354(1) -0.471(1) 0.7829(10) 0.0531 Uij C(23) -0.0433(10) -0.269(1) 1.1597(9) 0.0412 Uij C(24) 0.943(1) 0.454(2) 0.513(1) 0.029(3) Uij C(25) 0.954(2) 0.427(2) 0.483(2) 0.12(1) Uij C(26) 0.927(3) 0.488(3) 0.540(3) 0.22(1) Uij B(1) 0.4557(9) -0.0022(10) 0.8241(8) 0.0236 Uij B(2) -0.1361(9) -0.3059(9) 0.8089(8) 0.0248 Uij H(1) 0.2298 -0.1597 0.8059 0.0263 Uij H(2) 0.0616 -0.1782 0.6741 0.0285 Uij H(3) 0.5023 0.2245 0.9711 0.0195 Uij H(4) 0.6451 0.4066 0.9514 0.0248 Uij H(5) -0.2129 -0.3594 0.5698 0.0378 Uij H(6) -0.1979 -0.1852 0.5221 0.0369 Uij H(7) -0.1028 0.0029 0.7096 0.0375 Uij H(8) 0.0121 -0.4195 0.8018 0.0182 Uij H(9) 0.2093 -0.2976 0.9495 0.0276 Uij H(10) 0.2191 -0.0990 1.0683 0.0271 Uij H(11) -0.3515 -0.4704 0.8449 0.0376 Uij H(12) -0.4136 -0.3737 1.0143 0.0449 Uij H(13) -0.2763 -0.1524 1.1028 0.0379 Uij H(14) 0.6056 -0.0759 0.9122 0.0249 Uij H(15) 0.6448 -0.2323 0.7853 0.0243 Uij H(16) 0.3142 -0.5017 0.8313 0.0615 Uij H(17) 0.4294 -0.3985 0.8330 0.0615 Uij H(18) -0.0637 -0.2410 1.1043 0.0386 Uij H(19) 0.0426 -0.2233 1.1884 0.0386 Uij H(20) 0.1366 0.0464 0.5699 0.0408 Uij H(21) 0.1490 -0.0545 0.4767 0.0408 Uij H(22) 0.0428 -0.0875 0.5290 0.0408 Uij H(23) 0.4354 -0.4028 0.5136 0.0372 Uij H(24) 0.5389 -0.3068 0.4918 0.0372 Uij H(25) 0.5633 -0.3725 0.5636 0.0372 Uij H(26) 0.8491 0.3528 0.8070 0.0306 Uij H(27) 0.7545 0.3388 0.7120 0.0306 Uij H(28) 0.7998 0.4442 0.8319 0.0306 Uij H(29) 0.4462 -0.0083 0.9025 0.0387 Uij H(30) -0.1705 -0.3975 0.7535 0.0387 Uij loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.003 0.002 'International Tables' H 0 60 0.000 0.000 'International Tables' Cl 0 2 0.148 0.159 'International Tables' S 0 12 0.125 0.123 'International Tables' B 0 2 0.001 0.001 'International Tables' N 0 16 0.006 0.003 'International Tables' Bi 0 2 -4.108 10.257 'International Tables' Na 0 2 0.036 0.025 'International Tables' O 0 2 0.011 0.006 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -3 4 5 -3 -1 0 -4 2 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag S(1) Bi(1) S(1) 180.0 yes S(1) Bi(1) S(2) 89.81(7) yes S(1) Bi(1) S(2) 90.19(7) yes S(1) Bi(1) S(3) 91.31(6) yes S(1) Bi(1) S(3) 88.69(6) yes S(1) Bi(1) S(2) 90.19(7) yes S(1) Bi(1) S(2) 89.81(7) yes S(1) Bi(1) S(3) 88.69(6) yes S(1) Bi(1) S(3) 91.31(6) yes S(2) Bi(1) S(2) 180.0 yes S(2) Bi(1) S(3) 90.72(6) yes S(2) Bi(1) S(3) 89.28(6) yes S(2) Bi(1) S(3) 89.28(6) yes S(2) Bi(1) S(3) 90.72(6) yes S(3) Bi(1) S(3) 180.0 yes C(24) Cl(5) C(25) 15.9(9) yes Bi(1) S(1) C(1) 100.0(3) yes Bi(1) S(2) C(5) 99.6(3) yes Bi(1) S(3) C(9) 97.1(3) yes N(8) Na(1) N(8) 180.0 yes N(8) Na(1) N(10) 82.7(2) yes N(8) Na(1) N(10) 97.3(2) yes N(8) Na(1) N(12) 75.6(2) yes N(8) Na(1) N(12) 104.4(2) yes N(8) Na(1) N(10) 97.3(2) yes N(8) Na(1) N(10) 82.7(2) yes N(8) Na(1) N(12) 104.4(2) yes N(8) Na(1) N(12) 75.6(2) yes N(10) Na(1) N(10) 180.0000(1) yes N(10) Na(1) N(12) 74.9(3) yes N(10) Na(1) N(12) 105.1(3) yes N(10) Na(1) N(12) 105.1(3) yes N(10) Na(1) N(12) 74.9(3) yes N(12) Na(1) N(12) 180.0 yes C(1) N(1) C(2) 107.8(7) yes C(1) N(1) B(1) 133.2(7) yes C(2) N(1) B(1) 118.7(7) yes C(1) N(2) C(3) 109.9(7) yes C(1) N(2) C(4) 124.7(8) yes C(3) N(2) C(4) 125.4(8) yes C(5) N(3) C(6) 107.8(7) yes C(5) N(3) B(1) 132.9(7) yes C(6) N(3) B(1) 119.0(7) yes C(5) N(4) C(7) 109.7(7) yes C(5) N(4) C(8) 124.1(8) yes C(7) N(4) C(8) 126.2(8) yes C(9) N(5) C(10) 107.5(7) yes C(9) N(5) B(1) 132.4(7) yes C(10) N(5) B(1) 119.0(7) yes C(9) N(6) C(11) 110.3(7) yes C(9) N(6) C(12) 124.6(7) yes C(11) N(6) C(12) 125.0(8) yes N(8) N(7) C(13) 110.5(7) yes N(8) N(7) B(2) 123.5(7) yes C(13) N(7) B(2) 125.9(8) yes Na(1) N(8) N(7) 117.6(5) yes Na(1) N(8) C(15) 137.4(6) yes N(7) N(8) C(15) 104.9(7) yes N(10) N(9) C(16) 110.9(7) yes N(10) N(9) B(2) 122.6(7) yes C(16) N(9) B(2) 126.4(7) yes Na(1) N(10) N(9) 119.8(5) yes Na(1) N(10) C(18) 134.1(6) yes N(9) N(10) C(18) 105.1(7) yes N(12) N(11) C(19) 111.2(8) yes N(12) N(11) B(2) 122.6(7) yes C(19) N(11) B(2) 126.1(8) yes Na(1) N(12) N(11) 117.7(5) yes Na(1) N(12) C(21) 137.9(7) yes N(11) N(12) C(21) 104.3(8) yes S(1) C(1) N(1) 129.5(7) yes S(1) C(1) N(2) 123.2(7) yes N(1) C(1) N(2) 107.2(7) yes N(1) C(2) C(3) 108.3(8) yes N(1) C(2) H(1) 125.4 no C(3) C(2) H(1) 126.1 no N(2) C(3) C(2) 106.7(8) yes N(2) C(3) H(2) 126.1 no C(2) C(3) H(2) 127.1 no N(2) C(4) H(20) 111.1 no N(2) C(4) H(21) 113.2 no N(2) C(4) H(22) 111.8 no H(20) C(4) H(21) 106.3 no H(20) C(4) H(22) 105.6 no H(21) C(4) H(22) 108.4 no S(2) C(5) N(3) 128.3(7) yes S(2) C(5) N(4) 123.8(6) yes N(3) C(5) N(4) 107.8(7) yes N(3) C(6) C(7) 108.1(8) yes N(3) C(6) H(14) 128.8 no C(7) C(6) H(14) 123.0 no N(4) C(7) C(6) 106.6(8) yes N(4) C(7) H(15) 127.6 no C(6) C(7) H(15) 125.8 no N(4) C(8) H(23) 111.7 no N(4) C(8) H(24) 111.8 no N(4) C(8) H(25) 112.5 no H(23) C(8) H(24) 106.2 no H(23) C(8) H(25) 106.5 no H(24) C(8) H(25) 107.8 no S(3) C(9) N(5) 129.0(6) yes S(3) C(9) N(6) 124.3(6) yes N(5) C(9) N(6) 106.6(7) yes N(5) C(10) C(11) 109.7(8) yes N(5) C(10) H(3) 124.2 no C(11) C(10) H(3) 126.1 no N(6) C(11) C(10) 105.8(8) yes N(6) C(11) H(4) 128.6 no C(10) C(11) H(4) 125.5 no N(6) C(12) H(26) 110.4 no N(6) C(12) H(27) 111.9 no N(6) C(12) H(28) 111.9 no H(26) C(12) H(27) 106.9 no H(26) C(12) H(28) 106.8 no H(27) C(12) H(28) 108.8 no N(7) C(13) C(14) 108.0(8) yes N(7) C(13) H(5) 127.2 no C(14) C(13) H(5) 124.7 no C(13) C(14) C(15) 104.7(8) yes C(13) C(14) H(6) 128.6 no C(15) C(14) H(6) 126.8 no N(8) C(15) C(14) 111.9(9) yes N(8) C(15) H(7) 123.2 no C(14) C(15) H(7) 124.8 no N(9) C(16) C(17) 107.0(8) yes N(9) C(16) H(8) 125.9 no C(17) C(16) H(8) 127.0 no C(16) C(17) C(18) 105.4(8) yes C(16) C(17) H(9) 126.1 no C(18) C(17) H(9) 128.5 no N(10) C(18) C(17) 111.6(8) yes N(10) C(18) H(10) 125.8 no C(17) C(18) H(10) 122.6 no N(11) C(19) C(20) 107.3(9) yes N(11) C(19) H(11) 128.9 no C(20) C(19) H(11) 123.8 no C(19) C(20) C(21) 105.2(9) yes C(19) C(20) H(12) 128.2 no C(21) C(20) H(12) 126.6 no N(12) C(21) C(20) 111.8(9) yes N(12) C(21) H(13) 124.9 no C(20) C(21) H(13) 123.2 no Cl(1) C(22) Cl(2) 113.2(7) yes Cl(1) C(22) H(16) 108.7 no Cl(1) C(22) H(17) 105.8 no Cl(2) C(22) H(16) 112.8 no Cl(2) C(22) H(17) 109.3 no H(16) C(22) H(17) 106.7 no Cl(3) C(23) Cl(4) 112.1(6) yes Cl(3) C(23) H(18) 110.4 no Cl(3) C(23) H(19) 110.4 no Cl(4) C(23) H(18) 109.5 no Cl(4) C(23) H(19) 108.5 no H(18) C(23) H(19) 105.7 no Cl(5) C(24) C(24) 116(1) yes Cl(5) C(24) C(25) 80(3) yes Cl(5) C(24) C(25) 121(1) yes Cl(5) C(24) C(26) 112(3) yes Cl(5) C(24) C(26) 106(1) yes C(24) C(24) C(25) 74(3) yes C(24) C(24) C(25) 17(1) yes C(24) C(24) C(26) 100(3) yes C(24) C(24) C(26) 18(1) yes C(25) C(24) C(25) 92(3) yes C(25) C(24) C(26) 166(6) yes C(25) C(24) C(26) 56(3) yes C(25) C(24) C(26) 83(3) yes C(25) C(24) C(26) 36(1) yes C(26) C(24) C(26) 119(3) yes Cl(5) C(25) C(24) 83(3) yes Cl(5) C(25) C(24) 121(1) yes Cl(5) C(25) C(25) 116(2) yes Cl(5) C(25) C(26) 90(2) yes Cl(5) C(25) C(26) 117(1) yes C(24) C(25) C(24) 87(3) yes C(24) C(25) C(25) 70(3) yes C(24) C(25) C(26) 7(3) yes C(24) C(25) C(26) 108(4) yes C(24) C(25) C(25) 17.6(10) yes C(24) C(25) C(26) 85(2) yes C(24) C(25) C(26) 21(1) yes C(25) C(25) C(26) 67(2) yes C(25) C(25) C(26) 38(1) yes C(26) C(25) C(26) 106(2) yes C(24) C(26) C(24) 60(3) yes C(24) C(26) C(25) 6(2) yes C(24) C(26) C(25) 75(3) yes C(24) C(26) C(25) 58(2) yes C(24) C(26) C(25) 15(1) yes C(25) C(26) C(25) 73(2) yes N(1) B(1) N(3) 112.0(7) yes N(1) B(1) N(5) 111.1(7) yes N(1) B(1) H(29) 108.7 no N(3) B(1) N(5) 111.6(7) yes N(3) B(1) H(29) 103.0 no N(5) B(1) H(29) 110.0 no N(7) B(2) N(9) 112.5(7) yes N(7) B(2) N(11) 110.1(7) yes N(7) B(2) H(30) 109.7 no N(9) B(2) N(11) 109.2(7) yes N(9) B(2) H(30) 105.5 no N(11) B(2) H(30) 109.8 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Bi(1) S(1) 2.806(2) yes Bi(1) S(1) 2.806(2) yes Bi(1) S(2) 2.802(2) yes Bi(1) S(2) 2.802(2) yes Bi(1) S(3) 2.802(2) yes Bi(1) S(3) 2.802(2) yes Cl(1) C(22) 1.74(1) yes Cl(2) C(22) 1.73(1) yes Cl(3) C(23) 1.76(1) yes Cl(4) C(23) 1.75(1) yes Cl(5) C(24) 1.83(2) yes Cl(5) C(25) 1.82(3) yes S(1) C(1) 1.722(9) yes S(2) C(5) 1.719(8) yes S(3) C(9) 1.704(8) yes Na(1) N(8) 2.525(7) yes Na(1) N(8) 2.525(7) yes Na(1) N(10) 2.431(8) yes Na(1) N(10) 2.431(8) yes Na(1) N(12) 2.553(8) yes Na(1) N(12) 2.553(8) yes N(1) C(1) 1.36(1) yes N(1) C(2) 1.38(1) yes N(1) B(1) 1.54(1) yes N(2) C(1) 1.34(1) yes N(2) C(3) 1.37(1) yes N(2) C(4) 1.45(1) yes N(3) C(5) 1.36(1) yes N(3) C(6) 1.39(1) yes N(3) B(1) 1.56(1) yes N(4) C(5) 1.33(1) yes N(4) C(7) 1.39(1) yes N(4) C(8) 1.46(1) yes N(5) C(9) 1.38(1) yes N(5) C(10) 1.39(1) yes N(5) B(1) 1.55(1) yes N(6) C(9) 1.36(1) yes N(6) C(11) 1.39(1) yes N(6) C(12) 1.46(1) yes N(7) N(8) 1.36(1) yes N(7) C(13) 1.36(1) yes N(7) B(2) 1.53(1) yes N(8) C(15) 1.34(1) yes N(9) N(10) 1.36(1) yes N(9) C(16) 1.36(1) yes N(9) B(2) 1.54(1) yes N(10) C(18) 1.34(1) yes N(11) N(12) 1.36(1) yes N(11) C(19) 1.36(1) yes N(11) B(2) 1.57(1) yes N(12) C(21) 1.35(1) yes C(2) C(3) 1.35(1) yes C(2) H(1) 0.968 no C(3) H(2) 0.971 no C(4) H(20) 0.987 no C(4) H(21) 0.951 no C(4) H(22) 0.961 no C(6) C(7) 1.35(1) yes C(6) H(14) 0.956 no C(7) H(15) 0.994 no C(8) H(23) 0.978 no C(8) H(24) 0.962 no C(8) H(25) 0.959 no C(10) C(11) 1.35(1) yes C(10) H(3) 0.969 no C(11) H(4) 0.965 no C(12) H(26) 0.979 no C(12) H(27) 0.953 no C(12) H(28) 0.954 no C(13) C(14) 1.37(1) yes C(13) H(5) 0.963 no C(14) C(15) 1.39(1) yes C(14) H(6) 0.962 no C(15) H(7) 1.018 no C(16) C(17) 1.38(1) yes C(16) H(8) 0.964 no C(17) C(18) 1.38(1) yes C(17) H(9) 0.977 no C(18) H(10) 0.976 no C(19) C(20) 1.37(1) yes C(19) H(11) 0.996 no C(20) C(21) 1.38(2) yes C(20) H(12) 0.958 no C(21) H(13) 0.997 no C(22) H(16) 0.937 no C(22) H(17) 0.996 no C(23) H(18) 0.964 no C(23) H(19) 0.982 no C(24) C(24) 1.64(3) yes C(24) C(25) 0.51(3) yes C(24) C(25) 1.58(2) yes C(24) C(26) 0.59(3) yes C(24) C(26) 1.84(3) yes C(25) C(25) 1.67(5) yes C(25) C(26) 1.09(3) yes C(25) C(26) 1.62(3) yes B(1) H(29) 1.049 no B(2) H(30) 1.053 no