# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/210 data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; Unit cell dimensions were determined from reflections taken from three sets of 30 frames (at 0.3\% steps in \w) at 10 seconds. A full hemisphere of reciprocal space was scanned by 0.3\% \w steps at \f = 0, 90 and 180\% at 20 seconds per frame with the area detector held at 2\q = -27\%. The crystal-to-detector distance was 4.974 cm. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analysing the duplicate reflections. No decay was observed. A monoclinic setting opposed to the orthorhomic setting where again two molecules were found over centres of symmetry. The monoclinic Refinement led to better convergence, residuals and agreement factors. Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement parameters 1.2 times U~iso~ value of their attached carbon for aromatic hydrogens and 1.5 U~iso~ for methyl hydrogens. ; _publ_section_references ; Siemens (1995a). SMART and SAINT Area-Detector Control and Integration Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Siemens (1995b). SHELXTL. Version 5.03 Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H36 B22 Cl2 N2 S4' _chemical_formula_weight 597.35 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.683(3) _cell_length_b 22.229(5) _cell_length_c 10.367(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.485(14) _cell_angle_gamma 90.00 _cell_volume 3153.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method ? _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.480 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 19667 _diffrn_reflns_av_R_equivalents 0.1179 _diffrn_reflns_av_sigmaI/netI 0.1934 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.34 _reflns_number_total 7015 _reflns_number_observed 3404 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995a)' _computing_cell_refinement 'SAINT (Siemens, 1995a)' _computing_data_reduction 'SAINT (Siemens, 1995a)' _computing_structure_solution 'SHELXTL (Siemens, 1995b)' _computing_structure_refinement 'SHELXTL (Siemens, 1995b)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995b)' _computing_publication_material 'SHELXTL (Siemens, 1995b)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1084P)^2^+0.0000P] 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 'see above' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7015 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1481 _refine_ls_R_factor_obs 0.0790 _refine_ls_wR_factor_all 0.2195 _refine_ls_wR_factor_obs 0.1895 _refine_ls_goodness_of_fit_all 0.875 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 0.875 _refine_ls_restrained_S_obs 1.097 _refine_ls_shift/esd_max 0.007 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group S1 S -0.0044(2) 0.39303(6) 0.52951(14) 0.0233(4) Uani 1 d . . S2 S -0.0021(2) 0.49812(6) 0.73117(14) 0.0220(4) Uani 1 d . . S3 S 0.3899(2) 0.55630(9) 0.3652(2) 0.0205(5) Uani 1 d . . S4 S 0.6181(2) 0.55162(8) 0.3680(2) 0.0209(5) Uani 1 d . . Cl1 Cl -0.17153(14) 0.49209(8) 0.5185(2) 0.0295(5) Uani 1 d . . Cl2 Cl 0.5071(2) 0.59161(6) 0.62186(14) 0.0266(4) Uani 1 d . . B1 B -0.0315(6) 0.4786(3) 0.5548(8) 0.023(2) Uani 1 d . . B2 B 0.5026(8) 0.5371(3) 0.4701(6) 0.020(2) Uani 1 d . . B10 B -0.0726(8) 0.3072(4) 0.7506(10) 0.026(2) Uani 1 d . . H10 H -0.1157(8) 0.2761(4) 0.6871(10) 0.031 Uiso 1 calc R . B11 B 0.0592(8) 0.3070(4) 0.7526(10) 0.026(2) Uani 1 d . . H11 H 0.1019(8) 0.2753(4) 0.6908(10) 0.031 Uiso 1 calc R . B12 B -0.0067(9) 0.2819(3) 0.8916(7) 0.030(2) Uani 1 d . . H12 H -0.0071(9) 0.2334(3) 0.9214(7) 0.036 Uiso 1 calc R . B13 B 0.0989(8) 0.3292(4) 0.9113(9) 0.025(2) Uani 1 d . . H13 H 0.1681(8) 0.3114(4) 0.9553(9) 0.030 Uiso 1 calc R . B14 B -0.0052(9) 0.3432(3) 1.0079(7) 0.027(2) Uani 1 d . . H14 H -0.0043(9) 0.3348(3) 1.1144(7) 0.032 Uiso 1 calc R . B15 B 0.0597(8) 0.4049(4) 0.9386(9) 0.028(3) Uani 1 d . . H15 H 0.1025(8) 0.4377(4) 0.9985(9) 0.034 Uiso 1 calc R . B16 B -0.0708(8) 0.4054(4) 0.9383(9) 0.026(2) Uani 1 d . . H16 H -0.1128(8) 0.4385(4) 0.9977(9) 0.032 Uiso 1 calc R . B17 B -0.1134(8) 0.3820(4) 0.7805(9) 0.022(2) Uani 1 d . . H17 H -0.1829(8) 0.3996(4) 0.7369(9) 0.027 Uiso 1 calc R . B18 B 0.1015(8) 0.3823(4) 0.7833(10) 0.022(2) Uani 1 d . . H18 H 0.1710(8) 0.4001(4) 0.7415(10) 0.026 Uiso 1 calc R . B19 B -0.1128(8) 0.3288(4) 0.9106(9) 0.023(2) Uani 1 d . . H19 H -0.1818(8) 0.3111(4) 0.9538(9) 0.028 Uiso 1 calc R . B20 B 0.4012(8) 0.6151(4) 0.0957(9) 0.025(2) Uiso 1 d . . H20 H 0.3296(8) 0.5965(4) 0.0610(9) 0.030 Uiso 1 calc R . B21 B 0.4051(8) 0.6764(4) 0.2091(9) 0.024(2) Uani 1 d . . H21 H 0.3368(8) 0.6971(4) 0.2479(9) 0.028 Uiso 1 calc R . B22 B 0.4442(9) 0.6866(4) 0.0450(10) 0.034(3) Uani 1 d . . H22 H 0.4019(9) 0.7148(4) -0.0256(10) 0.041 Uiso 1 calc R . B23 B 0.5755(8) 0.6849(4) 0.0461(9) 0.029(3) Uani 1 d . . H23 H 0.6191(8) 0.7122(4) -0.0235(9) 0.035 Uiso 1 calc R . B24 B 0.6178(8) 0.6720(4) 0.2091(9) 0.024(2) Uani 1 d . . H24 H 0.6890(8) 0.6898(4) 0.2470(9) 0.029 Uiso 1 calc R . B25 B 0.6154(8) 0.6109(4) 0.0971(8) 0.025(2) Uani 1 d . . H25 H 0.6849(8) 0.5895(4) 0.0635(8) 0.030 Uiso 1 calc R . B26 B 0.5100(8) 0.6681(3) 0.3084(7) 0.021(2) Uani 1 d . . H26 H 0.5106(8) 0.6835(3) 0.4113(7) 0.025 Uiso 1 calc R . B27 B 0.5037(9) 0.5674(3) 0.1236(6) 0.023(2) Uani 1 d . . H27 H 0.5001(9) 0.5177(3) 0.1064(6) 0.027 Uiso 1 calc R . B28 B 0.5115(9) 0.7195(3) 0.1765(7) 0.027(2) Uani 1 d . . H28 H 0.5133(9) 0.7694(3) 0.1919(7) 0.033 Uiso 1 calc R . B29 B 0.5062(9) 0.6198(3) -0.0054(7) 0.029(2) Uani 1 d . . H29 H 0.5049(9) 0.6044(3) -0.1082(7) 0.035 Uiso 1 calc R . C3 C 0.4484(7) 0.6050(3) 0.2494(8) 0.023(2) Uani 1 d . . C1 C -0.0056(7) 0.3676(2) 0.6945(5) 0.0204(15) Uani 1 d . . C4 C 0.5674(6) 0.6032(3) 0.2515(7) 0.018(2) Uani 1 d . . C2 C -0.0055(8) 0.4240(3) 0.8025(5) 0.022(2) Uani 1 d . . C5 C 0.2401(10) 0.6018(6) 0.7727(11) 0.079(4) Uani 1 d . . H5A H 0.2594(53) 0.5608(14) 0.7966(31) 0.118 Uiso 1 calc R . H5B H 0.1689(11) 0.6055(35) 0.7770(21) 0.118 Uiso 1 calc R . H5C H 0.2705(47) 0.6305(24) 0.8327(15) 0.118 Uiso 1 calc R . C6 C 0.2581(9) 0.6771(5) 0.5967(12) 0.068(4) Uani 1 d . . H6A H 0.2678(52) 0.6790(8) 0.5032(16) 0.102 Uiso 1 calc R . H6B H 0.3055(36) 0.7035(7) 0.6401(53) 0.102 Uiso 1 calc R . H6C H 0.1917(19) 0.6903(12) 0.6171(63) 0.102 Uiso 1 calc R . C7 C 0.7611(9) 0.6794(4) 0.5946(12) 0.065(4) Uani 1 d . . H7A H 0.7359(46) 0.6860(9) 0.5070(28) 0.098 Uiso 1 calc R . H7B H 0.8313(10) 0.6878(10) 0.5972(64) 0.098 Uiso 1 calc R . H7C H 0.7273(43) 0.7062(4) 0.6546(42) 0.098 Uiso 1 calc R . C8 C 0.7625(9) 0.6017(6) 0.7721(11) 0.072(4) Uani 1 d . . H8A H 0.7580(54) 0.5582(7) 0.7861(17) 0.107 Uiso 1 calc R . H8B H 0.7137(33) 0.6222(28) 0.8250(12) 0.107 Uiso 1 calc R . H8C H 0.8280(22) 0.6157(30) 0.7964(21) 0.107 Uiso 1 calc R . N1 N 0.2724(6) 0.6146(3) 0.6414(8) 0.042(2) Uani 1 d . . H1A H 0.2394(6) 0.5894(3) 0.5858(8) 0.050 Uiso 1 calc R . H1B H 0.3378(6) 0.6055(3) 0.6361(8) 0.050 Uiso 1 calc R . N2 N 0.7436(6) 0.6153(3) 0.6331(8) 0.042(2) Uani 1 d . . H2A H 0.6798(6) 0.6057(3) 0.6138(8) 0.051 Uiso 1 calc R . H2B H 0.7829(6) 0.5910(3) 0.5840(8) 0.051 Uiso 1 calc R . 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 S1 0.0498(12) 0.0059(7) 0.0143(7) -0.0011(5) 0.0013(12) 0.0000(10) S2 0.0448(11) 0.0057(7) 0.0154(7) 0.0002(5) -0.0008(11) -0.0009(10) S3 0.0338(13) 0.0130(9) 0.0147(10) 0.0030(8) 0.0004(9) -0.0027(9) S4 0.0359(13) 0.0118(9) 0.0152(10) 0.0030(8) -0.0005(9) 0.0006(9) Cl1 0.0349(11) 0.0179(9) 0.0356(12) -0.0052(9) -0.0010(10) 0.0000(9) Cl2 0.0555(13) 0.0112(7) 0.0132(7) -0.0036(5) 0.0017(11) -0.0010(11) B1 0.040(7) 0.007(4) 0.023(4) 0.001(3) -0.003(4) 0.004(3) B2 0.039(5) 0.007(3) 0.013(3) -0.003(2) -0.016(5) 0.005(5) B10 0.046(7) 0.008(4) 0.024(5) 0.004(4) 0.005(5) -0.006(4) B11 0.046(7) 0.004(4) 0.028(5) 0.005(4) -0.001(5) 0.005(4) B12 0.051(6) 0.014(4) 0.024(4) 0.007(3) 0.001(6) 0.000(5) B13 0.036(6) 0.015(5) 0.025(6) 0.005(4) -0.004(4) 0.002(4) B14 0.046(5) 0.012(3) 0.021(4) 0.006(3) 0.000(5) -0.001(5) B15 0.059(8) 0.010(4) 0.016(5) 0.004(4) 0.000(5) 0.006(5) B16 0.044(7) 0.019(5) 0.017(5) 0.008(4) 0.010(4) 0.000(5) B17 0.030(6) 0.014(5) 0.022(5) -0.001(4) 0.006(4) -0.003(4) B18 0.028(6) 0.014(4) 0.024(5) 0.003(4) 0.002(4) 0.003(4) B19 0.035(6) 0.014(4) 0.022(5) 0.008(4) 0.002(4) -0.001(4) B21 0.034(6) 0.012(4) 0.025(5) 0.005(4) 0.001(4) 0.010(4) B22 0.064(8) 0.014(4) 0.024(6) 0.008(4) 0.001(5) 0.007(5) B23 0.056(8) 0.015(4) 0.016(5) 0.008(4) 0.013(5) -0.003(5) B24 0.039(6) 0.010(4) 0.024(5) 0.004(4) 0.002(4) -0.003(4) B25 0.047(7) 0.020(4) 0.008(4) 0.004(3) 0.014(4) 0.000(4) B26 0.038(6) 0.006(3) 0.019(3) 0.000(2) -0.004(5) 0.005(4) B27 0.043(5) 0.012(3) 0.013(3) -0.001(3) 0.007(5) 0.005(5) B28 0.047(7) 0.011(3) 0.023(4) 0.007(3) 0.005(5) -0.002(5) B29 0.049(6) 0.023(4) 0.016(4) 0.003(3) 0.000(5) 0.000(5) C3 0.048(6) 0.008(4) 0.013(4) 0.005(3) 0.002(4) -0.002(4) C1 0.040(4) 0.005(3) 0.016(3) 0.000(2) -0.003(4) 0.002(4) C4 0.033(5) 0.009(4) 0.012(4) -0.002(3) 0.004(3) -0.002(3) C2 0.043(5) 0.012(3) 0.013(3) 0.002(2) 0.008(4) 0.002(4) C5 0.126(13) 0.080(10) 0.030(7) -0.009(6) 0.008(7) -0.013(9) C6 0.108(11) 0.029(6) 0.068(9) 0.001(6) -0.007(8) 0.001(6) C7 0.103(10) 0.020(5) 0.073(9) 0.003(5) 0.012(8) -0.005(6) C8 0.108(11) 0.067(9) 0.040(8) -0.007(6) -0.001(7) 0.017(8) N1 0.057(5) 0.025(4) 0.043(5) -0.014(4) 0.014(4) -0.006(4) N2 0.068(6) 0.019(4) 0.040(5) -0.014(4) -0.023(5) 0.013(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 S1 C1 1.802(6) . ? S1 B1 1.956(8) . ? S2 C2 1.808(6) . ? S2 B1 1.919(8) . ? S3 C3 1.809(8) . ? S3 B2 1.926(10) . ? S3 Cl1 3.406(3) 3_566 ? S4 C4 1.800(8) . ? S4 B2 1.937(11) . ? S4 Cl1 3.520(3) 1_655 ? Cl1 B1 1.972(9) . ? Cl2 B2 1.986(6) . ? B1 B1 1.72(2) 3_566 ? B2 B2 1.765(12) 3_666 ? B10 C1 1.729(11) . ? B10 B17 1.782(13) . ? B10 B12 1.801(13) . ? B10 B11 1.803(12) . ? B10 B19 1.816(14) . ? B10 H10 1.12 . ? B11 C1 1.720(11) . ? B11 B12 1.795(13) . ? B11 B13 1.798(14) . ? B11 B18 1.800(13) . ? B11 H11 1.12 . ? B12 B13 1.80(2) . ? B12 B19 1.799(15) . ? B12 B14 1.820(10) . ? B12 H12 1.12 . ? B13 B14 1.78(2) . ? B13 B18 1.777(13) . ? B13 B15 1.789(13) . ? B13 H13 1.12 . ? B14 B15 1.788(13) . ? B14 B16 1.797(13) . ? B14 B19 1.81(2) . ? B14 H14 1.12 . ? B15 C2 1.715(12) . ? B15 B16 1.785(13) . ? B15 B18 1.785(13) . ? B15 H15 1.12 . ? B16 C2 1.724(11) . ? B16 B17 1.809(14) . ? B16 B19 1.821(13) . ? B16 H16 1.12 . ? B17 C1 1.760(13) . ? B17 C2 1.760(14) . ? B17 B19 1.794(13) . ? B17 H17 1.12 . ? B18 C2 1.744(13) . ? B18 C1 1.754(14) . ? B18 H18 1.12 . ? B19 H19 1.12 . ? B20 C3 1.729(13) . ? B20 B22 1.776(14) . ? B20 B27 1.780(14) . ? B20 B29 1.789(15) . ? B20 B21 1.799(13) . ? B20 H20 1.12 . ? B21 C3 1.743(11) . ? B21 B26 1.769(14) . ? B21 B28 1.778(15) . ? B21 B22 1.802(14) . ? B21 H21 1.12 . ? B22 B29 1.790(13) . ? B22 B28 1.795(14) . ? B22 B23 1.796(14) . ? B22 H22 1.12 . ? B23 B28 1.791(13) . ? B23 B24 1.804(14) . ? B23 B29 1.806(14) . ? B23 B25 1.811(13) . ? B23 H23 1.12 . ? B24 C4 1.737(11) . ? B24 B25 1.788(13) . ? B24 B26 1.808(14) . ? B24 B28 1.827(15) . ? B24 H24 1.12 . ? B25 C4 1.744(11) . ? B25 B27 1.831(15) . ? B25 B29 1.84(2) . ? B25 H25 1.12 . ? B26 C3 1.744(11) . ? B26 C4 1.748(11) . ? B26 B28 1.782(10) . ? B26 H26 1.12 . ? B27 C3 1.729(11) . ? B27 C4 1.769(11) . ? B27 B29 1.775(10) . ? B27 H27 1.12 . ? B28 H28 1.12 . ? B29 H29 1.12 . ? C3 C4 1.628(10) . ? C1 C2 1.680(8) . ? C5 N1 1.463(13) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 N1 1.476(12) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 N2 1.498(11) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 N2 1.493(13) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? N1 H1A 0.92 . ? N1 H1B 0.92 . ? N2 H2A 0.92 . ? N2 H2B 0.92 . ? 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 C1 S1 B1 100.0(3) . . ? C2 S2 B1 100.2(3) . . ? C3 S3 B2 98.7(4) . . ? C3 S3 Cl1 144.9(3) . 3_566 ? B2 S3 Cl1 115.5(3) . 3_566 ? C4 S4 B2 99.2(3) . . ? C4 S4 Cl1 147.8(3) . 1_655 ? B2 S4 Cl1 111.3(2) . 1_655 ? B1 B1 S2 113.7(7) 3_566 . ? B1 B1 S1 110.7(7) 3_566 . ? S2 B1 S1 108.0(4) . . ? B1 B1 Cl1 106.4(6) 3_566 . ? S2 B1 Cl1 110.1(4) . . ? S1 B1 Cl1 107.9(4) . . ? B2 B2 S3 111.8(8) 3_666 . ? B2 B2 S4 112.5(8) 3_666 . ? S3 B2 S4 107.9(3) . . ? B2 B2 Cl2 107.1(5) 3_666 . ? S3 B2 Cl2 109.4(4) . . ? S4 B2 Cl2 108.1(5) . . ? C1 B10 B17 60.1(5) . . ? C1 B10 B12 104.7(7) . . ? B17 B10 B12 107.8(7) . . ? C1 B10 B11 58.2(5) . . ? B17 B10 B11 108.4(7) . . ? B12 B10 B11 59.7(6) . . ? C1 B10 B19 105.5(6) . . ? B17 B10 B19 59.8(5) . . ? B12 B10 B19 59.6(6) . . ? B11 B10 B19 107.5(8) . . ? C1 B10 H10 124.1(4) . . ? B17 B10 H10 120.9(5) . . ? B12 B10 H10 122.7(4) . . ? B11 B10 H10 121.8(5) . . ? B19 B10 H10 122.5(5) . . ? C1 B11 B12 105.3(7) . . ? C1 B11 B13 104.8(6) . . ? B12 B11 B13 60.1(6) . . ? C1 B11 B18 59.7(5) . . ? B12 B11 B18 108.1(7) . . ? B13 B11 B18 59.2(5) . . ? C1 B11 B10 58.7(6) . . ? B12 B11 B10 60.1(6) . . ? B13 B11 B10 107.7(8) . . ? B18 B11 B10 108.6(7) . . ? C1 B11 H11 124.2(4) . . ? B12 B11 H11 122.1(4) . . ? B13 B11 H11 122.8(5) . . ? B18 B11 H11 121.2(5) . . ? B10 B11 H11 121.4(5) . . ? B11 B12 B13 60.0(6) . . ? B11 B12 B19 108.6(6) . . ? B13 B12 B19 107.2(5) . . ? B11 B12 B10 60.2(4) . . ? B13 B12 B10 107.8(6) . . ? B19 B12 B10 60.6(6) . . ? B11 B12 B14 107.2(6) . . ? B13 B12 B14 58.8(6) . . ? B19 B12 B14 59.9(6) . . ? B10 B12 B14 107.8(6) . . ? B11 B12 H12 121.5(4) . . ? B13 B12 H12 122.5(4) . . ? B19 B12 H12 121.4(4) . . ? B10 B12 H12 121.4(4) . . ? B14 B12 H12 122.5(3) . . ? B14 B13 B18 109.0(7) . . ? B14 B13 B15 60.2(5) . . ? B18 B13 B15 60.1(5) . . ? B14 B13 B11 109.1(7) . . ? B18 B13 B11 60.5(5) . . ? B15 B13 B11 108.4(7) . . ? B14 B13 B12 61.2(5) . . ? B18 B13 B12 109.0(7) . . ? B15 B13 B12 109.1(7) . . ? B11 B13 B12 59.9(5) . . ? B14 B13 H13 120.8(4) . . ? B18 B13 H13 121.2(5) . . ? B15 B13 H13 121.5(5) . . ? B11 B13 H13 121.5(5) . . ? B12 B13 H13 121.0(4) . . ? B13 B14 B15 60.3(5) . . ? B13 B14 B16 108.0(6) . . ? B15 B14 B16 59.7(4) . . ? B13 B14 B19 108.0(5) . . ? B15 B14 B19 108.5(6) . . ? B16 B14 B19 60.7(6) . . ? B13 B14 B12 60.0(6) . . ? B15 B14 B12 108.2(6) . . ? B16 B14 B12 107.9(6) . . ? B19 B14 B12 59.5(6) . . ? B13 B14 H14 121.7(4) . . ? B15 B14 H14 121.5(4) . . ? B16 B14 H14 121.6(4) . . ? B19 B14 H14 121.5(4) . . ? B12 B14 H14 121.9(3) . . ? C2 B15 B16 59.0(6) . . ? C2 B15 B18 59.7(5) . . ? B16 B15 B18 109.2(8) . . ? C2 B15 B14 105.3(7) . . ? B16 B15 B14 60.4(6) . . ? B18 B15 B14 108.1(6) . . ? C2 B15 B13 104.9(6) . . ? B16 B15 B13 107.9(8) . . ? B18 B15 B13 59.6(5) . . ? B14 B15 B13 59.5(5) . . ? C2 B15 H15 124.2(4) . . ? B16 B15 H15 121.0(5) . . ? B18 B15 H15 120.9(5) . . ? B14 B15 H15 122.4(4) . . ? B13 B15 H15 122.9(5) . . ? C2 B16 B15 58.5(6) . . ? C2 B16 B14 104.6(7) . . ? B15 B16 B14 59.9(6) . . ? C2 B16 B17 59.7(5) . . ? B15 B16 B17 108.3(8) . . ? B14 B16 B17 107.3(7) . . ? C2 B16 B19 105.1(6) . . ? B15 B16 B19 108.0(7) . . ? B14 B16 B19 59.9(5) . . ? B17 B16 B19 59.2(5) . . ? C2 B16 H16 124.3(4) . . ? B15 B16 H16 121.4(5) . . ? B14 B16 H16 122.8(4) . . ? B17 B16 H16 121.5(5) . . ? B19 B16 H16 122.5(4) . . ? C1 B17 C2 57.0(4) . . ? C1 B17 B10 58.4(5) . . ? C2 B17 B10 104.6(7) . . ? C1 B17 B19 105.2(7) . . ? C2 B17 B19 104.7(7) . . ? B10 B17 B19 61.1(5) . . ? C1 B17 B16 104.2(7) . . ? C2 B17 B16 57.7(5) . . ? B10 B17 B16 109.1(7) . . ? B19 B17 B16 60.7(5) . . ? C1 B17 H17 124.8(4) . . ? C2 B17 H17 125.1(4) . . ? B10 B17 H17 121.5(5) . . ? B19 B17 H17 122.2(5) . . ? B16 B17 H17 122.1(5) . . ? C2 B18 C1 57.4(5) . . ? C2 B18 B13 104.2(7) . . ? C1 B18 B13 104.3(7) . . ? C2 B18 B15 58.1(5) . . ? C1 B18 B15 104.6(7) . . ? B13 B18 B15 60.3(5) . . ? C2 B18 B11 104.2(7) . . ? C1 B18 B11 57.9(5) . . ? B13 B18 B11 60.3(5) . . ? B15 B18 B11 108.4(7) . . ? C2 B18 H18 125.0(4) . . ? C1 B18 H18 124.8(4) . . ? B13 B18 H18 123.0(5) . . ? B15 B18 H18 121.9(5) . . ? B11 B18 H18 122.2(5) . . ? B17 B19 B12 107.4(7) . . ? B17 B19 B14 107.5(7) . . ? B12 B19 B14 60.6(5) . . ? B17 B19 B10 59.1(5) . . ? B12 B19 B10 59.7(5) . . ? B14 B19 B10 107.7(7) . . ? B17 B19 B16 60.1(5) . . ? B12 B19 B16 107.8(7) . . ? B14 B19 B16 59.4(5) . . ? B10 B19 B16 107.0(6) . . ? B17 B19 H19 122.2(5) . . ? B12 B19 H19 121.6(4) . . ? B14 B19 H19 121.7(4) . . ? B10 B19 H19 122.4(5) . . ? B16 B19 H19 122.1(4) . . ? C3 B20 B22 105.5(7) . . ? C3 B20 B27 59.0(5) . . ? B22 B20 B27 108.6(7) . . ? C3 B20 B29 104.6(7) . . ? B22 B20 B29 60.3(5) . . ? B27 B20 B29 59.6(5) . . ? C3 B20 B21 59.2(5) . . ? B22 B20 B21 60.5(5) . . ? B27 B20 B21 109.0(7) . . ? B29 B20 B21 108.6(7) . . ? C3 B20 H20 124.5(4) . . ? B22 B20 H20 121.8(5) . . ? B27 B20 H20 121.1(4) . . ? B29 B20 H20 122.5(4) . . ? B21 B20 H20 120.7(5) . . ? C3 B21 B26 59.5(5) . . ? C3 B21 B28 105.0(7) . . ? B26 B21 B28 60.3(5) . . ? C3 B21 B20 58.4(5) . . ? B26 B21 B20 108.7(6) . . ? B28 B21 B20 107.7(7) . . ? C3 B21 B22 103.8(6) . . ? B26 B21 B22 108.4(7) . . ? B28 B21 B22 60.2(5) . . ? B20 B21 B22 59.1(5) . . ? C3 B21 H21 124.9(4) . . ? B26 B21 H21 120.6(4) . . ? B28 B21 H21 122.2(4) . . ? B20 B21 H21 121.8(5) . . ? B22 B21 H21 122.9(5) . . ? B20 B22 B29 60.2(5) . . ? B20 B22 B28 108.0(7) . . ? B29 B22 B28 108.6(7) . . ? B20 B22 B23 108.2(8) . . ? B29 B22 B23 60.5(6) . . ? B28 B22 B23 59.8(6) . . ? B20 B22 B21 60.4(5) . . ? B29 B22 B21 108.4(6) . . ? B28 B22 B21 59.2(6) . . ? B23 B22 B21 107.2(8) . . ? B20 B22 H22 121.5(5) . . ? B29 B22 H22 121.1(4) . . ? B28 B22 H22 121.9(4) . . ? B23 B22 H22 121.9(5) . . ? B21 B22 H22 122.1(5) . . ? B28 B23 B22 60.0(6) . . ? B28 B23 B24 61.1(6) . . ? B22 B23 B24 108.8(8) . . ? B28 B23 B29 108.0(7) . . ? B22 B23 B29 59.6(6) . . ? B24 B23 B29 108.3(6) . . ? B28 B23 B25 108.6(6) . . ? B22 B23 B25 108.7(7) . . ? B24 B23 B25 59.3(5) . . ? B29 B23 B25 61.1(5) . . ? B28 B23 H23 121.3(4) . . ? B22 B23 H23 121.5(5) . . ? B24 B23 H23 121.4(5) . . ? B29 B23 H23 121.6(4) . . ? B25 B23 H23 121.3(4) . . ? C4 B24 B25 59.3(5) . . ? C4 B24 B23 104.5(7) . . ? B25 B24 B23 60.5(5) . . ? C4 B24 B26 59.0(4) . . ? B25 B24 B26 108.8(7) . . ? B23 B24 B26 106.5(7) . . ? C4 B24 B28 103.8(7) . . ? B25 B24 B28 108.0(7) . . ? B23 B24 B28 59.1(5) . . ? B26 B24 B28 58.7(5) . . ? C4 B24 H24 124.7(4) . . ? B25 B24 H24 120.5(5) . . ? B23 B24 H24 123.0(5) . . ? B26 B24 H24 121.9(4) . . ? B28 B24 H24 123.4(4) . . ? C4 B25 B24 58.9(5) . . ? C4 B25 B23 104.0(6) . . ? B24 B25 B23 60.2(5) . . ? C4 B25 B27 59.3(4) . . ? B24 B25 B27 108.3(6) . . ? B23 B25 B27 105.8(7) . . ? C4 B25 B29 103.3(7) . . ? B24 B25 B29 107.6(7) . . ? B23 B25 B29 59.4(5) . . ? B27 B25 B29 57.9(5) . . ? C4 B25 H25 124.9(4) . . ? B24 B25 H25 120.9(5) . . ? B23 B25 H25 123.3(4) . . ? B27 B25 H25 122.3(4) . . ? B29 B25 H25 123.7(4) . . ? C3 B26 C4 55.6(4) . . ? C3 B26 B21 59.5(5) . . ? C4 B26 B21 104.7(6) . . ? C3 B26 B28 104.8(6) . . ? C4 B26 B28 105.2(6) . . ? B21 B26 B28 60.1(5) . . ? C3 B26 B24 103.5(5) . . ? C4 B26 B24 58.5(5) . . ? B21 B26 B24 109.0(5) . . ? B28 B26 B24 61.2(5) . . ? C3 B26 H26 125.4(4) . . ? C4 B26 H26 125.0(4) . . ? B21 B26 H26 121.4(4) . . ? B28 B26 H26 122.3(3) . . ? B24 B26 H26 121.9(4) . . ? C3 B27 C4 55.4(4) . . ? C3 B27 B29 105.2(5) . . ? C4 B27 B29 104.9(6) . . ? C3 B27 B20 59.0(5) . . ? C4 B27 B20 103.6(5) . . ? B29 B27 B20 60.4(6) . . ? C3 B27 B25 103.2(5) . . ? C4 B27 B25 57.9(5) . . ? B29 B27 B25 61.2(6) . . ? B20 B27 B25 108.6(5) . . ? C3 B27 H27 125.3(4) . . ? C4 B27 H27 125.7(3) . . ? B29 B27 H27 122.0(3) . . ? B20 B27 H27 121.9(4) . . ? B25 B27 H27 122.2(4) . . ? B21 B28 B26 59.6(5) . . ? B21 B28 B23 108.5(6) . . ? B26 B28 B23 108.2(6) . . ? B21 B28 B22 60.6(6) . . ? B26 B28 B22 108.2(6) . . ? B23 B28 B22 60.1(5) . . ? B21 B28 B24 107.8(5) . . ? B26 B28 B24 60.1(5) . . ? B23 B28 B24 59.8(6) . . ? B22 B28 B24 107.9(6) . . ? B21 B28 H28 121.6(4) . . ? B26 B28 H28 121.7(3) . . ? B23 B28 H28 121.5(4) . . ? B22 B28 H28 121.5(4) . . ? B24 B28 H28 121.9(4) . . ? B27 B29 B20 59.9(6) . . ? B27 B29 B22 108.2(6) . . ? B20 B29 B22 59.5(6) . . ? B27 B29 B23 108.4(6) . . ? B20 B29 B23 107.2(6) . . ? B22 B29 B23 59.9(5) . . ? B27 B29 B25 60.9(5) . . ? B20 B29 B25 107.9(5) . . ? B22 B29 B25 107.9(6) . . ? B23 B29 B25 59.6(6) . . ? B27 B29 H29 121.1(3) . . ? B20 B29 H29 122.3(4) . . ? B22 B29 H29 121.9(4) . . ? B23 B29 H29 122.0(4) . . ? B25 B29 H29 121.6(4) . . ? C4 C3 B27 63.5(6) . . ? C4 C3 B20 112.4(7) . . ? B27 C3 B20 62.0(5) . . ? C4 C3 B21 111.4(7) . . ? B27 C3 B21 114.2(6) . . ? B20 C3 B21 62.4(5) . . ? C4 C3 B26 62.3(5) . . ? B27 C3 B26 116.1(7) . . ? B20 C3 B26 113.2(6) . . ? B21 C3 B26 61.0(5) . . ? C4 C3 S3 115.1(6) . . ? B27 C3 S3 114.2(5) . . ? B20 C3 S3 121.7(6) . . ? B21 C3 S3 123.5(6) . . ? B26 C3 S3 117.6(5) . . ? C2 C1 B11 110.7(6) . . ? C2 C1 B10 110.6(6) . . ? B11 C1 B10 63.0(4) . . ? C2 C1 B18 61.0(5) . . ? B11 C1 B18 62.4(5) . . ? B10 C1 B18 114.3(6) . . ? C2 C1 B17 61.5(5) . . ? B11 C1 B17 113.4(6) . . ? B10 C1 B17 61.4(5) . . ? B18 C1 B17 113.6(5) . . ? C2 C1 S1 113.5(4) . . ? B11 C1 S1 124.7(5) . . ? B10 C1 S1 124.9(5) . . ? B18 C1 S1 115.2(6) . . ? B17 C1 S1 116.0(6) . . ? C3 C4 B24 111.9(7) . . ? C3 C4 B25 111.7(7) . . ? B24 C4 B25 61.8(5) . . ? C3 C4 B26 62.1(5) . . ? B24 C4 B26 62.5(5) . . ? B25 C4 B26 113.8(6) . . ? C3 C4 B27 61.0(6) . . ? B24 C4 B27 113.6(6) . . ? B25 C4 B27 62.8(5) . . ? B26 C4 B27 113.9(6) . . ? C3 C4 S4 113.9(6) . . ? B24 C4 S4 125.4(6) . . ? B25 C4 S4 122.1(6) . . ? B26 C4 S4 118.1(5) . . ? B27 C4 S4 113.7(4) . . ? C1 C2 B15 111.2(5) . . ? C1 C2 B16 111.6(6) . . ? B15 C2 B16 62.5(4) . . ? C1 C2 B18 61.6(5) . . ? B15 C2 B18 62.1(5) . . ? B16 C2 B18 114.1(6) . . ? C1 C2 B17 61.5(5) . . ? B15 C2 B17 113.9(6) . . ? B16 C2 B17 62.6(6) . . ? B18 C2 B17 114.1(5) . . ? C1 C2 S2 114.0(4) . . ? B15 C2 S2 123.1(6) . . ? B16 C2 S2 124.6(5) . . ? B18 C2 S2 114.3(6) . . ? B17 C2 S2 117.1(6) . . ? N1 C5 H5A 109.5(6) . . ? N1 C5 H5B 109.5(7) . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5(6) . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 H6A 109.5(6) . . ? N1 C6 H6B 109.5(6) . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5(6) . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 H7A 109.5(5) . . ? N2 C7 H7B 109.5(6) . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5(6) . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5(5) . . ? N2 C8 H8B 109.5(6) . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5(6) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 N1 C6 115.8(9) . . ? C5 N1 H1A 108.3(6) . . ? C6 N1 H1A 108.3(6) . . ? C5 N1 H1B 108.3(7) . . ? C6 N1 H1B 108.3(6) . . ? H1A N1 H1B 107.4 . . ? C8 N2 C7 115.1(8) . . ? C8 N2 H2A 108.5(6) . . ? C7 N2 H2A 108.5(6) . . ? C8 N2 H2B 108.5(6) . . ? C7 N2 H2B 108.5(6) . . ? H2A N2 H2B 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 S2 B1 B1 -142.9(7) . . . 3_566 ? C2 S2 B1 S1 -19.7(5) . . . . ? C2 S2 B1 Cl1 97.9(5) . . . . ? C1 S1 B1 B1 144.2(7) . . . 3_566 ? C1 S1 B1 S2 19.2(5) . . . . ? C1 S1 B1 Cl1 -99.8(5) . . . . ? C3 S3 B2 B2 -145.5(7) . . . 3_666 ? Cl1 S3 B2 B2 42.6(8) 3_566 . . 3_666 ? C3 S3 B2 S4 -21.3(4) . . . . ? Cl1 S3 B2 S4 166.8(2) 3_566 . . . ? C3 S3 B2 Cl2 96.1(5) . . . . ? Cl1 S3 B2 Cl2 -75.8(4) 3_566 . . . ? C4 S4 B2 B2 145.7(6) . . . 3_666 ? Cl1 S4 B2 B2 -44.7(7) 1_655 . . 3_666 ? C4 S4 B2 S3 21.9(4) . . . . ? Cl1 S4 B2 S3 -168.5(2) 1_655 . . . ? C4 S4 B2 Cl2 -96.3(4) . . . . ? Cl1 S4 B2 Cl2 73.2(3) 1_655 . . . ? C1 B10 B11 C1 0.0 . . . . ? _refine_diff_density_max 1.115 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.140 #=END data_[NH2Me2]2[S2C2B10H10] _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; Unit cell dimensions were determined from reflections taken from three sets of 30 frames (at 0.3\% steps in \w) at 10 seconds. A full hemisphere of reciprocal space was scanned by 0.3\% \w steps at \f = 0, 90 and 180\% at 20 seconds per frame with the area detector held at 2\q = -27\%. The crystal-to-detector distance was 4.974 cm. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analysing the duplicate reflections. No decay was observed. Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement parameters 1.2 times U~iso~ value of their attached carbon for aromatic hydrogens and 1.5 U~iso~ for methyl hydrogens. ; _publ_section_references ; Siemens (1995a). SMART and SAINT Area-Detector Control and Integration Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Siemens (1995b). SHELXTL. Version 5.03 Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H29 B10 N3 S2' _chemical_formula_weight 339.56 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2~1~/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.209(4) _cell_length_b 8.974(4) _cell_length_c 19.784(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.14(4) _cell_angle_gamma 90.00 _cell_volume 1984.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 97 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method ? _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 11867 _diffrn_reflns_av_R_equivalents 0.1682 _diffrn_reflns_av_sigmaI/netI 0.2469 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4503 _reflns_number_observed 1983 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995a)' _computing_cell_refinement 'SAINT (Siemens, 1995a)' _computing_data_reduction 'SAINT (Siemens, 1995a)' _computing_structure_solution 'SHELXTL (Siemens, 1995b)' _computing_structure_refinement 'SHELXTL (Siemens, 1995b)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995b)' _computing_publication_material 'SHELXTL (Siemens, 1995b)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+2.1530P] whereP={Max(Fo^2^,0)+2Fc^2^}/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4503 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2283 _refine_ls_R_factor_obs 0.0931 _refine_ls_wR_factor_all 0.1908 _refine_ls_wR_factor_obs 0.1406 _refine_ls_goodness_of_fit_all 1.009 _refine_ls_goodness_of_fit_obs 1.146 _refine_ls_restrained_S_all 1.009 _refine_ls_restrained_S_obs 1.146 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group S1 S 0.94522(13) 0.7430(2) 0.42302(7) 0.0263(4) Uani 1 d . . S2 S 0.92589(12) 0.79991(14) 0.24978(7) 0.0225(4) Uani 1 d . . B10 B 0.8130(6) 0.5481(6) 0.3194(3) 0.0196(14) Uani 1 d . . H10 H 0.8959(6) 0.4804(6) 0.3144(3) 0.023 Uiso 1 calc R . B11 B 0.6672(6) 0.4707(7) 0.3146(3) 0.025(2) Uani 1 d . . H11 H 0.6508(6) 0.3487(7) 0.3066(3) 0.030 Uiso 1 calc R . B12 B 0.5672(6) 0.6106(7) 0.2788(3) 0.0238(15) Uani 1 d . . H12 H 0.4836(6) 0.5813(7) 0.2472(3) 0.029 Uiso 1 calc R . B13 B 0.5791(6) 0.5821(7) 0.3671(3) 0.029(2) Uani 1 d . . H13 H 0.5028(6) 0.5341(7) 0.3935(3) 0.035 Uiso 1 calc R . B14 B 0.5748(5) 0.7662(7) 0.3344(3) 0.0247(15) Uani 1 d . . H14 H 0.4963(5) 0.8416(7) 0.3394(3) 0.030 Uiso 1 calc R . B15 B 0.7236(6) 0.8351(7) 0.3394(3) 0.0229(15) Uani 1 d . . H15 H 0.7474(6) 0.9553(7) 0.3474(3) 0.027 Uiso 1 calc R . B16 B 0.7115(6) 0.5864(7) 0.2482(3) 0.0243(15) Uani 1 d . . H16 H 0.7240(6) 0.5405(7) 0.1966(3) 0.029 Uiso 1 calc R . B17 B 0.7316(6) 0.5398(7) 0.3928(3) 0.027(2) Uani 1 d . . H17 H 0.7571(6) 0.4623(7) 0.4358(3) 0.033 Uiso 1 calc R . B18 B 0.6746(6) 0.7216(7) 0.4060(3) 0.026(2) Uani 1 d . . H18 H 0.6616(6) 0.7669(7) 0.4577(3) 0.031 Uiso 1 calc R . B19 B 0.6545(6) 0.7682(6) 0.2613(3) 0.0243(15) Uani 1 d . . H19 H 0.6286(6) 0.8450(6) 0.2181(3) 0.029 Uiso 1 calc R . C1 C 0.8111(5) 0.6939(5) 0.3774(2) 0.0208(12) Uani 1 d . . C2 C 0.7988(4) 0.7241(5) 0.2849(2) 0.0197(12) Uani 1 d . . N1 N 0.6632(6) 0.1525(7) 0.5129(3) 0.064(2) Uani 1 d . . C4 C 0.4962(6) 0.1664(7) 0.4164(3) 0.046(2) Uani 1 d . . H4A H 0.4191(7) 0.1426(43) 0.4343(5) 0.069 Uiso 1 calc R . H4B H 0.5125(19) 0.0951(32) 0.3807(9) 0.069 Uiso 1 calc R . H4A H 0.4933(24) 0.2675(14) 0.3976(14) 0.069 Uiso 1 calc R . C5 C 1.1217(5) 1.0673(6) 0.4184(3) 0.0312(15) Uani 1 d . . H5A H 1.1705(15) 0.9839(24) 0.4042(11) 0.047 Uiso 1 calc R . H5B H 1.1004(5) 1.0509(37) 0.4650(4) 0.047 Uiso 1 calc R . H5C H 1.1672(16) 1.1602(16) 0.4161(13) 0.047 Uiso 1 calc R . C6 C 0.9199(5) 1.1802(6) 0.3989(3) 0.0335(15) Uani 1 d . . H6A H 0.8913(22) 1.1387(19) 0.4406(9) 0.050 Uiso 1 calc R . H6B H 0.8524(14) 1.1911(29) 0.3649(7) 0.050 Uiso 1 calc R . H6C H 0.9563(9) 1.2779(12) 0.4085(16) 0.050 Uiso 1 calc R . C7 C 1.2112(6) 0.5091(6) 0.4111(3) 0.038(2) Uani 1 d . . H7A H 1.1510(8) 0.4513(33) 0.4333(10) 0.057 Uiso 1 calc R . H7B H 1.2444(29) 0.5859(7) 0.4423(8) 0.057 Uiso 1 calc R . H7C H 1.2754(21) 0.4426(31) 0.3986(4) 0.057 Uiso 1 calc R . C8 C 1.2355(5) 0.6823(6) 0.3147(3) 0.036(2) Uani 1 d . . H8A H 1.1904(9) 0.7323(28) 0.2769(11) 0.053 Uiso 1 calc R . H8B H 1.3010(17) 0.6246(8) 0.2974(15) 0.053 Uiso 1 calc R . H8C H 1.2685(23) 0.7571(23) 0.3470(5) 0.053 Uiso 1 calc R . C3 C 0.5906(6) 0.1575(6) 0.4708(3) 0.037(2) Uani 1 d . . N3 N 1.0108(4) 1.0778(5) 0.3725(2) 0.0278(12) Uani 1 d . . H3A H 0.9779(4) 0.9843(5) 0.3669(2) 0.033 Uiso 1 calc R . H3B H 1.0303(4) 1.1111(5) 0.3308(2) 0.033 Uiso 1 calc R . N2 N 1.1547(4) 0.5808(5) 0.3493(2) 0.0260(11) Uani 1 d . . H2A H 1.0891(4) 0.6341(5) 0.3609(2) 0.031 Uiso 1 calc R . H2B H 1.1280(4) 0.5077(5) 0.3193(2) 0.031 Uiso 1 calc R . 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 S1 0.0262(8) 0.0312(8) 0.0209(7) -0.0030(6) -0.0024(6) 0.0006(7) S2 0.0234(8) 0.0234(8) 0.0209(8) 0.0026(6) 0.0028(6) -0.0023(6) B10 0.027(4) 0.013(3) 0.019(3) 0.002(2) 0.003(3) 0.004(3) B11 0.027(4) 0.021(3) 0.028(4) -0.001(3) 0.005(3) -0.001(3) B12 0.020(4) 0.024(4) 0.028(4) -0.004(3) 0.004(3) -0.001(3) B13 0.025(4) 0.028(4) 0.034(4) -0.001(3) 0.006(3) -0.005(3) B14 0.015(3) 0.024(4) 0.035(4) -0.001(3) 0.005(3) 0.002(3) B15 0.026(4) 0.020(3) 0.024(4) 0.003(3) 0.005(3) -0.001(3) B16 0.025(4) 0.022(4) 0.025(4) -0.001(3) -0.003(3) -0.005(3) B17 0.035(4) 0.023(4) 0.025(4) 0.001(3) 0.007(3) -0.001(3) B18 0.026(4) 0.030(4) 0.022(4) -0.006(3) 0.008(3) 0.004(3) B19 0.027(4) 0.017(3) 0.028(4) 0.000(3) -0.004(3) -0.001(3) C1 0.028(3) 0.020(3) 0.014(3) -0.004(2) -0.001(2) 0.004(2) C2 0.021(3) 0.023(3) 0.016(3) -0.002(2) 0.004(2) 0.000(2) N1 0.063(5) 0.068(5) 0.059(4) -0.002(3) -0.013(4) 0.006(3) C4 0.062(5) 0.045(4) 0.030(4) -0.001(3) -0.001(4) -0.010(4) C5 0.030(4) 0.036(4) 0.027(4) -0.003(3) 0.000(3) 0.001(3) C6 0.036(4) 0.032(3) 0.033(4) 0.003(3) 0.004(3) 0.009(3) C7 0.044(4) 0.039(4) 0.031(4) 0.005(3) -0.003(3) -0.002(3) C8 0.032(4) 0.029(3) 0.046(4) 0.005(3) 0.005(3) -0.006(3) C3 0.042(4) 0.032(4) 0.038(4) -0.007(3) 0.009(3) -0.007(3) N3 0.035(3) 0.023(3) 0.025(3) 0.002(2) 0.002(2) -0.002(2) N2 0.022(3) 0.028(3) 0.028(3) -0.009(2) 0.002(2) 0.002(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 S1 C1 1.753(5) . ? S2 C2 1.766(5) . ? B10 C2 1.724(7) . ? B10 C1 1.741(7) . ? B10 B17 1.771(9) . ? B10 B11 1.772(9) . ? B10 B16 1.780(8) . ? B11 B17 1.771(9) . ? B11 B16 1.773(9) . ? B11 B13 1.789(9) . ? B11 B12 1.794(9) . ? B12 B13 1.763(9) . ? B12 B19 1.768(9) . ? B12 B14 1.776(8) . ? B12 B16 1.780(9) . ? B13 B14 1.774(9) . ? B13 B18 1.785(9) . ? B13 B17 1.788(9) . ? B14 B19 1.755(9) . ? B14 B15 1.775(9) . ? B14 B18 1.785(8) . ? B15 C2 1.731(8) . ? B15 C1 1.739(8) . ? B15 B19 1.782(8) . ? B15 B18 1.783(9) . ? B16 C2 1.706(8) . ? B16 B19 1.778(9) . ? B17 C1 1.685(8) . ? B17 B18 1.778(9) . ? B18 C1 1.688(8) . ? B19 C2 1.698(8) . ? C1 C2 1.844(7) . ? N1 C3 1.122(7) . ? C4 C3 1.457(8) . ? C5 N3 1.487(6) . ? C6 N3 1.494(7) . ? C7 N2 1.483(6) . ? C8 N2 1.486(7) . ? 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 C2 B10 C1 64.3(3) . . ? C2 B10 B17 109.0(4) . . ? C1 B10 B17 57.4(3) . . ? C2 B10 B11 106.2(4) . . ? C1 B10 B11 106.0(4) . . ? B17 B10 B11 60.0(4) . . ? C2 B10 B16 58.2(3) . . ? C1 B10 B16 109.8(4) . . ? B17 B10 B16 108.6(5) . . ? B11 B10 B16 59.9(3) . . ? B17 B11 B10 60.0(3) . . ? B17 B11 B16 108.9(4) . . ? B10 B11 B16 60.3(3) . . ? B17 B11 B13 60.3(4) . . ? B10 B11 B13 107.2(4) . . ? B16 B11 B13 107.4(4) . . ? B17 B11 B12 107.7(4) . . ? B10 B11 B12 107.1(4) . . ? B16 B11 B12 59.9(4) . . ? B13 B11 B12 58.9(3) . . ? B13 B12 B19 107.9(4) . . ? B13 B12 B14 60.2(4) . . ? B19 B12 B14 59.3(3) . . ? B13 B12 B16 108.3(4) . . ? B19 B12 B16 60.1(3) . . ? B14 B12 B16 107.6(4) . . ? B13 B12 B11 60.4(4) . . ? B19 B12 B11 107.4(4) . . ? B14 B12 B11 107.7(4) . . ? B16 B12 B11 59.5(3) . . ? B12 B13 B14 60.3(4) . . ? B12 B13 B18 109.0(5) . . ? B14 B13 B18 60.2(3) . . ? B12 B13 B17 108.3(5) . . ? B14 B13 B17 107.5(4) . . ? B18 B13 B17 59.7(3) . . ? B12 B13 B11 60.7(4) . . ? B14 B13 B11 108.1(5) . . ? B18 B13 B11 107.6(5) . . ? B17 B13 B11 59.3(4) . . ? B19 B14 B13 108.0(4) . . ? B19 B14 B15 60.6(3) . . ? B13 B14 B15 107.7(4) . . ? B19 B14 B12 60.1(3) . . ? B13 B14 B12 59.5(3) . . ? B15 B14 B12 108.1(5) . . ? B19 B14 B18 109.2(4) . . ? B13 B14 B18 60.2(3) . . ? B15 B14 B18 60.1(3) . . ? B12 B14 B18 108.3(4) . . ? C2 B15 C1 64.2(3) . . ? C2 B15 B14 105.3(4) . . ? C1 B15 B14 105.6(4) . . ? C2 B15 B19 57.8(3) . . ? C1 B15 B19 109.0(4) . . ? B14 B15 B19 59.1(3) . . ? C2 B15 B18 108.8(4) . . ? C1 B15 B18 57.3(3) . . ? B14 B15 B18 60.2(3) . . ? B19 B15 B18 108.1(4) . . ? C2 B16 B11 107.0(4) . . ? C2 B16 B19 58.3(3) . . ? B11 B16 B19 107.9(5) . . ? C2 B16 B10 59.2(3) . . ? B11 B16 B10 59.9(3) . . ? B19 B16 B10 106.1(4) . . ? C2 B16 B12 105.9(4) . . ? B11 B16 B12 60.7(4) . . ? B19 B16 B12 59.6(3) . . ? B10 B16 B12 107.4(5) . . ? C1 B17 B10 60.4(3) . . ? C1 B17 B11 108.5(4) . . ? B10 B17 B11 60.1(4) . . ? C1 B17 B18 58.3(3) . . ? B10 B17 B18 107.1(4) . . ? B11 B17 B18 108.8(4) . . ? C1 B17 B13 106.4(4) . . ? B10 B17 B13 107.3(4) . . ? B11 B17 B13 60.4(4) . . ? B18 B17 B13 60.1(4) . . ? C1 B18 B17 58.1(3) . . ? C1 B18 B15 60.1(3) . . ? B17 B18 B15 106.4(4) . . ? C1 B18 B13 106.4(4) . . ? B17 B18 B13 60.2(4) . . ? B15 B18 B13 106.9(4) . . ? C1 B18 B14 107.4(4) . . ? B17 B18 B14 107.5(4) . . ? B15 B18 B14 59.7(3) . . ? B13 B18 B14 59.6(3) . . ? C2 B19 B14 107.6(4) . . ? C2 B19 B12 106.8(4) . . ? B14 B19 B12 60.6(4) . . ? C2 B19 B16 58.7(3) . . ? B14 B19 B16 108.7(4) . . ? B12 B19 B16 60.3(3) . . ? C2 B19 B15 59.6(3) . . ? B14 B19 B15 60.3(3) . . ? B12 B19 B15 108.2(4) . . ? B16 B19 B15 107.3(4) . . ? B17 C1 B18 63.6(4) . . ? B17 C1 B15 112.7(4) . . ? B18 C1 B15 62.7(3) . . ? B17 C1 B10 62.2(3) . . ? B18 C1 B10 112.7(4) . . ? B15 C1 B10 107.3(4) . . ? B17 C1 S1 123.9(4) . . ? B18 C1 S1 123.7(4) . . ? B15 C1 S1 118.4(4) . . ? B10 C1 S1 118.5(4) . . ? B17 C1 C2 107.3(4) . . ? B18 C1 C2 107.8(4) . . ? B15 C1 C2 57.7(3) . . ? B10 C1 C2 57.4(3) . . ? S1 C1 C2 118.3(3) . . ? B19 C2 B16 63.0(3) . . ? B19 C2 B10 112.4(4) . . ? B16 C2 B10 62.5(3) . . ? B19 C2 B15 62.6(3) . . ? B16 C2 B15 113.1(4) . . ? B10 C2 B15 108.4(4) . . ? B19 C2 S2 125.6(4) . . ? B16 C2 S2 124.5(4) . . ? B10 C2 S2 117.1(3) . . ? B15 C2 S2 117.8(3) . . ? B19 C2 C1 108.0(4) . . ? B16 C2 C1 108.4(4) . . ? B10 C2 C1 58.3(3) . . ? B15 C2 C1 58.1(3) . . ? S2 C2 C1 116.3(3) . . ? N1 C3 C4 179.1(7) . . ? C5 N3 C6 112.8(4) . . ? C7 N2 C8 114.1(4) . . ? _refine_diff_density_max 0.464 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.094 #=END data_5 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; Unit cell dimensions were determined from reflections taken from three sets of 30 frames (at 0.3\% steps in \w) at 10 seconds. A full hemisphere of reciprocal space was scanned by 0.3\% \w steps at \f = 0, 90 and 180\% at 20 seconds per frame with the area detector held at 2\q = -27\%. The crystal-to-detector distance was 4.974 cm. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analysing the duplicate reflections. No decay was observed. Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement parameters 1.2 times U~iso~ value of their attached carbon for aromatic hydrogens and 1.5 U~iso~ for methyl hydrogens. ; _publ_section_references ; Sheldrick, G (1997). SADABS (Siemens Area Detector Absorption Program), Univeristy of Gottigen, Germany. Siemens (1995a). SMART and SAINT Area-Detector Control and Integration Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Siemens (1995b). SHELXTL. Version 5.03 Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H62 B32 Cl2 N4 Se6' _chemical_formula_weight 1177.26 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' '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~/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.521(6) _cell_length_b 21.945(5) _cell_length_c 11.965(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.803(14) _cell_angle_gamma 90.00 _cell_volume 4977.5(21) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 67 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method ? _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 4.541 _exptl_absorpt_correction_type 'multi-scan SADABS: Sheldrick (1997)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25918 _diffrn_reflns_av_R_equivalents 0.0882 _diffrn_reflns_av_sigmaI/netI 0.1114 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8754 _reflns_number_observed 4813 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995a)' _computing_cell_refinement 'SAINT (Siemens, 1995a)' _computing_data_reduction 'SAINT (Siemens, 1995a)' _computing_structure_solution 'SHELXTL (Siemens, 1995b)' _computing_structure_refinement 'SHELXTL (Siemens, 1995b)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995b)' _computing_publication_material 'SHELXTL (Siemens, 1995b)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 57 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+1.1743P] whereP={Max(Fo^2^,0)+2Fc^2^)}/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8697 _refine_ls_number_parameters 531 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1433 _refine_ls_R_factor_obs 0.0674 _refine_ls_wR_factor_all 0.1829 _refine_ls_wR_factor_obs 0.1440 _refine_ls_goodness_of_fit_all 1.019 _refine_ls_goodness_of_fit_obs 1.135 _refine_ls_restrained_S_all 1.048 _refine_ls_restrained_S_obs 1.135 _refine_ls_shift/esd_max 0.007 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Se1 Se 1.17744(5) 0.46441(4) 1.55845(7) 0.0245(3) Uani 1 d . . Se2 Se 1.32338(6) 0.46543(4) 1.44207(8) 0.0337(3) Uani 1 d . . Se3 Se 1.33585(6) 0.62627(5) 1.47453(8) 0.0347(3) Uani 1 d . . Se4 Se 1.32751(5) 0.55117(4) 1.71715(7) 0.0275(3) Uani 1 d . . Se5 Se 1.18253(5) 0.54725(4) 1.30938(7) 0.0261(3) Uani 1 d . . Se6 Se 1.18314(6) 0.62352(5) 1.59120(8) 0.0353(3) Uani 1 d . . C1 C 1.2118(5) 0.3870(4) 1.5172(7) 0.017(2) Uani 1 d . . C2 C 1.2824(5) 0.3867(4) 1.4625(7) 0.027(2) Uani 1 d . . C3 C 1.4020(5) 0.6520(4) 1.6134(7) 0.029(2) Uani 1 d . . C4 C 1.3978(5) 0.6162(4) 1.7324(7) 0.026(2) Uani 1 d . . C5 C 1.1147(6) 0.6108(4) 1.3233(7) 0.029(2) Uani 1 d . . C6 C 1.1157(5) 0.6440(4) 1.4489(7) 0.025(2) Uani 1 d . . B1 B 1.2359(8) 0.5193(7) 1.4764(11) 0.058(5) Uani 1 d . . B2 B 1.2680(8) 0.5751(8) 1.5491(11) 0.061(5) Uani 1 d . . B10 B 1.2906(6) 0.3615(5) 1.6015(9) 0.028(3) Uani 1 d . . H10 H 1.3208(6) 0.3863(5) 1.6797(9) 0.033 Uiso 1 calc R . B11 B 1.3341(7) 0.3237(5) 1.5096(10) 0.032(3) Uani 1 d . . H11 H 1.3931(7) 0.3229(5) 1.5267(10) 0.039 Uiso 1 calc R . B12 B 1.2883(7) 0.2815(5) 1.5926(10) 0.037(3) Uani 1 d . . H12 H 1.3169(7) 0.2515(5) 1.6644(10) 0.044 Uiso 1 calc R . B13 B 1.2797(6) 0.2612(5) 1.4481(10) 0.030(3) Uani 1 d . . H13 H 1.3030(6) 0.2179(5) 1.4239(10) 0.036 Uiso 1 calc R . B14 B 1.2047(6) 0.2612(5) 1.5056(10) 0.031(3) Uani 1 d . . H14 H 1.1775(6) 0.2181(5) 1.5205(10) 0.037 Uiso 1 calc R . B15 B 1.1986(7) 0.2896(5) 1.3646(9) 0.033(3) Uani 1 d . . H15 H 1.1678(7) 0.2651(5) 1.2866(9) 0.040 Uiso 1 calc R . B16 B 1.1564(7) 0.3294(5) 1.4595(9) 0.031(3) Uani 1 d . . H16 H 1.0976(7) 0.3321(5) 1.4438(9) 0.037 Uiso 1 calc R . B17 B 1.2036(6) 0.3708(5) 1.3729(9) 0.030(3) Uani 1 d . . H17 H 1.1768(6) 0.4012(5) 1.3005(9) 0.036 Uiso 1 calc R . B18 B 1.2123(6) 0.3240(5) 1.6016(9) 0.026(3) Uani 1 d . . H18 H 1.1905(6) 0.3232(5) 1.6801(9) 0.031 Uiso 1 calc R . B19 B 1.2776(7) 0.3293(5) 1.3657(9) 0.032(3) Uani 1 d . . H19 H 1.2995(7) 0.3317(5) 1.2875(9) 0.039 Uiso 1 calc R . B20 B 1.3678(7) 0.6900(5) 1.7142(9) 0.034(3) Uani 1 d . . H20 H 1.3113(7) 0.7040(5) 1.7012(9) 0.041 Uiso 1 calc R . B21 B 1.4242(7) 0.7270(5) 1.6411(10) 0.033(3) Uani 1 d . . H21 H 1.4051(7) 0.7657(5) 1.5806(10) 0.040 Uiso 1 calc R . B22 B 1.4378(7) 0.7348(6) 1.7933(11) 0.042(3) Uani 1 d . . H22 H 1.4285(7) 0.7790(6) 1.8342(11) 0.050 Uiso 1 calc R . B23 B 1.5125(7) 0.7239(5) 1.7306(11) 0.042(3) Uani 1 d . . H23 H 1.5520(7) 0.7607(5) 1.7292(11) 0.050 Uiso 1 calc R . B24 B 1.5070(7) 0.6853(6) 1.8593(11) 0.043(4) Uani 1 d . . H24 H 1.5432(7) 0.6975(6) 1.9439(11) 0.051 Uiso 1 calc R . B25 B 1.5385(7) 0.6445(6) 1.7508(11) 0.042(3) Uani 1 d . . H25 H 1.5946(7) 0.6293(6) 1.7638(11) 0.050 Uiso 1 calc R . B26 B 1.4797(6) 0.6084(5) 1.8235(10) 0.035(3) Uani 1 d . . H26 H 1.4969(6) 0.5692(5) 1.8837(10) 0.042 Uiso 1 calc R . B27 B 1.4674(7) 0.6011(5) 1.6713(10) 0.036(3) Uani 1 d . . H27 H 1.4757(7) 0.5568(5) 1.6300(10) 0.043 Uiso 1 calc R . B28 B 1.4871(7) 0.6708(6) 1.6144(11) 0.041(3) Uani 1 d . . H28 H 1.5091(7) 0.6729(6) 1.5362(11) 0.049 Uiso 1 calc R . B29 B 1.4175(7) 0.6631(5) 1.8487(10) 0.033(3) Uani 1 d . . H29 H 1.3940(7) 0.6593(5) 1.9252(10) 0.040 Uiso 1 calc R . B30 B 1.0501(7) 0.5917(5) 1.3944(10) 0.033(3) Uani 1 d . . H30 H 1.0452(7) 0.5461(5) 1.4337(10) 0.040 Uiso 1 calc R . B31 B 1.0302(7) 0.6048(5) 1.2419(9) 0.029(3) Uani 1 d . . H31 H 1.0111(7) 0.5669(5) 1.1797(9) 0.035 Uiso 1 calc R . B32 B 0.9752(7) 0.6367(5) 1.3252(9) 0.028(3) Uani 1 d . . H32 H 0.9200(7) 0.6205(5) 1.3190(9) 0.034 Uiso 1 calc R . B33 B 0.9999(7) 0.6793(5) 1.2126(9) 0.032(3) Uani 1 d . . H33 H 0.9608(7) 0.6913(5) 1.1308(9) 0.039 Uiso 1 calc R . B34 B 0.9978(7) 0.7148(6) 1.3459(10) 0.039(3) Uani 1 d . . H34 H 0.9573(7) 0.7498(6) 1.3525(10) 0.047 Uiso 1 calc R . B35 B 1.0683(7) 0.7297(5) 1.2779(9) 0.031(3) Uani 1 d . . H35 H 1.0746(7) 0.7755(5) 1.2407(9) 0.037 Uiso 1 calc R . B36 B 1.0876(7) 0.7179(5) 1.4280(10) 0.033(3) Uani 1 d . . H36 H 1.1068(7) 0.7556(5) 1.4907(10) 0.039 Uiso 1 calc R . B37 B 1.1430(6) 0.6851(5) 1.3459(9) 0.027(3) Uani 1 d . . H37 H 1.1988(6) 0.7002(5) 1.3541(9) 0.032 Uiso 1 calc R . B38 B 1.0319(7) 0.6614(5) 1.4577(10) 0.035(3) Uani 1 d . . H38 H 1.0147(7) 0.6617(5) 1.5406(10) 0.042 Uiso 1 calc R . B39 B 1.0874(7) 0.6615(5) 1.2115(9) 0.029(3) Uani 1 d . . H39 H 1.1065(7) 0.6614(5) 1.1304(9) 0.035 Uiso 1 calc R . N1 N 1.2454(5) 0.4428(3) 0.9879(6) 0.030(2) Uani 1 d . . H1A H 1.2843(5) 0.4669(3) 0.9895(6) 0.036 Uiso 1 calc R . H1B H 1.2083(5) 0.4682(3) 0.9901(6) 0.036 Uiso 1 calc R . C7 C 1.2283(7) 0.4089(5) 0.8781(8) 0.049(3) Uani 1 d . . H7A H 1.2153(41) 0.4377(5) 0.8139(9) 0.073 Uiso 1 calc R . H7B H 1.1887(25) 0.3813(26) 0.8770(28) 0.073 Uiso 1 calc R . H7C H 1.2695(13) 0.3852(27) 0.8704(31) 0.073 Uiso 1 calc R . C8 C 1.2601(6) 0.4044(4) 1.0922(8) 0.040(3) Uani 1 d . . H8A H 1.2159(7) 0.3866(24) 1.1024(32) 0.059 Uiso 1 calc R . H8B H 1.2815(33) 0.4293(8) 1.1594(11) 0.059 Uiso 1 calc R . H8C H 1.2927(27) 0.3716(18) 1.0839(25) 0.059 Uiso 1 calc R . N2 N 1.0273(5) 0.4407(3) 1.1631(6) 0.032(2) Uani 1 d . . H2A H 1.0669(5) 0.4650(3) 1.1803(6) 0.039 Uiso 1 calc R . H2B H 0.9929(5) 0.4616(3) 1.1112(6) 0.039 Uiso 1 calc R . C9 C 1.0028(7) 0.4314(5) 1.2691(8) 0.049(3) Uani 1 d . . H9A H 0.9783(34) 0.4681(13) 1.2856(35) 0.073 Uiso 1 calc R . H9B H 1.0434(7) 0.4233(33) 1.3334(14) 0.073 Uiso 1 calc R . H9C H 0.9704(30) 0.3966(21) 1.2589(23) 0.073 Uiso 1 calc R . C10 C 1.0442(6) 0.3847(5) 1.1075(10) 0.053(3) Uani 1 d . . H10A H 1.0591(38) 0.3953(5) 1.0373(36) 0.080 Uiso 1 calc R . H10B H 1.0023(13) 0.3586(16) 1.0878(58) 0.080 Uiso 1 calc R . H10C H 1.0824(27) 0.3629(18) 1.1605(26) 0.080 Uiso 1 calc R . N3 N 0.7548(4) 0.3821(4) 0.9583(7) 0.037(2) Uani 1 d . . H3A H 0.7184(4) 0.4093(4) 0.9548(7) 0.044 Uiso 1 calc R . H3B H 0.7918(4) 0.4032(4) 0.9415(7) 0.044 Uiso 1 calc R . C11 C 0.7316(7) 0.3360(5) 0.8699(9) 0.060(4) Uani 1 d . . H11A H 0.7151(40) 0.3558(6) 0.7949(14) 0.091 Uiso 1 calc R . H11B H 0.6930(28) 0.3122(24) 0.8877(38) 0.091 Uiso 1 calc R . H11C H 0.7711(12) 0.3088(22) 0.8676(47) 0.091 Uiso 1 calc R . C12 C 0.7771(6) 0.3592(6) 1.0765(9) 0.057(4) Uani 1 d . . H12A H 0.7915(40) 0.3934(7) 1.1294(12) 0.085 Uiso 1 calc R . H12B H 0.8170(27) 0.3312(29) 1.0824(19) 0.085 Uiso 1 calc R . H12C H 0.7378(14) 0.3375(31) 1.0966(25) 0.085 Uiso 1 calc R . N4 N 1.4821(5) 0.4461(4) 1.7773(7) 0.041(2) Uani 1 d . . H4A H 1.4452(5) 0.4713(4) 1.7441(7) 0.050 Uiso 1 calc R . H4B H 1.5169(5) 0.4702(4) 1.8213(7) 0.050 Uiso 1 calc R . C13 C 1.5098(8) 0.4188(5) 1.6849(10) 0.071(4) Uani 1 d . . H13A H 1.5298(43) 0.4508(8) 1.6452(51) 0.106 Uiso 1 calc R . H13B H 1.4714(12) 0.3983(34) 1.6300(41) 0.106 Uiso 1 calc R . H13C H 1.5466(33) 0.3892(30) 1.7180(13) 0.106 Uiso 1 calc R . C14 C 1.4575(7) 0.4037(5) 1.8543(9) 0.063(4) Uani 1 d . . H14A H 1.4193(30) 0.3785(26) 1.8093(14) 0.095 Uiso 1 calc R . H14B H 1.4402(40) 0.4268(5) 1.9120(44) 0.095 Uiso 1 calc R . H14C H 1.4966(13) 0.3775(25) 1.8929(53) 0.095 Uiso 1 calc R . Cl1 Cl 1.11390(15) 0.52149(11) 0.9976(2) 0.0376(7) Uani 1 d . . Cl2 Cl 1.6262(2) 0.47089(12) 1.9480(2) 0.0454(7) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0323(7) 0.0196(5) 0.0234(5) 0.0034(4) 0.0102(4) 0.0017(4) Se2 0.0519(8) 0.0204(6) 0.0375(6) 0.0021(4) 0.0276(5) 0.0034(5) Se3 0.0242(7) 0.0457(7) 0.0337(6) 0.0061(5) 0.0059(5) -0.0125(5) Se4 0.0239(6) 0.0356(6) 0.0208(5) 0.0039(4) 0.0008(4) -0.0102(5) Se5 0.0243(6) 0.0324(6) 0.0201(5) 0.0027(4) 0.0023(4) 0.0037(5) Se6 0.0269(7) 0.0442(7) 0.0385(6) 0.0079(5) 0.0154(5) 0.0129(5) C1 0.012(5) 0.015(5) 0.025(5) 0.001(3) 0.008(4) 0.001(4) C2 0.021(6) 0.032(6) 0.034(5) 0.014(4) 0.020(4) 0.015(5) C3 0.017(6) 0.038(6) 0.032(5) 0.011(4) 0.004(4) -0.002(5) C4 0.010(6) 0.038(6) 0.025(5) 0.011(4) -0.006(4) -0.004(4) C5 0.032(7) 0.025(6) 0.032(5) 0.004(4) 0.013(5) 0.000(5) C6 0.032(7) 0.016(5) 0.033(5) -0.007(4) 0.019(5) 0.001(4) B1 0.041(10) 0.077(11) 0.046(8) 0.025(7) -0.007(7) -0.041(8) B2 0.033(10) 0.105(13) 0.038(8) 0.016(8) -0.005(7) -0.018(9) B10 0.015(7) 0.039(7) 0.028(6) 0.011(5) 0.003(5) 0.000(5) B11 0.024(8) 0.015(6) 0.059(8) 0.005(5) 0.013(6) 0.015(5) B12 0.025(8) 0.033(7) 0.051(7) 0.017(6) 0.004(6) 0.009(6) B13 0.017(7) 0.024(7) 0.052(7) 0.008(5) 0.013(6) 0.003(5) B14 0.014(7) 0.027(7) 0.051(7) -0.002(5) 0.007(6) 0.002(5) B15 0.046(9) 0.029(7) 0.026(6) -0.002(5) 0.011(6) 0.004(6) B16 0.031(8) 0.018(6) 0.042(7) -0.007(5) 0.007(6) 0.003(5) B17 0.016(7) 0.046(8) 0.024(6) -0.002(5) -0.004(5) 0.006(6) B18 0.020(7) 0.019(6) 0.037(6) 0.006(5) 0.004(5) 0.004(5) B19 0.027(8) 0.044(8) 0.029(6) 0.000(5) 0.012(5) 0.010(6) B20 0.019(7) 0.044(8) 0.032(6) 0.012(5) -0.008(5) 0.011(6) B21 0.028(8) 0.028(7) 0.041(7) 0.003(5) 0.005(6) -0.008(6) B22 0.036(9) 0.029(7) 0.055(8) 0.004(6) 0.002(7) -0.012(6) B23 0.036(9) 0.021(7) 0.061(8) 0.008(6) -0.001(7) -0.006(6) B24 0.028(8) 0.039(8) 0.051(8) 0.007(6) -0.011(6) -0.006(6) B25 0.014(7) 0.045(8) 0.061(8) 0.011(6) 0.000(6) 0.008(6) B26 0.009(7) 0.038(8) 0.049(7) 0.001(6) -0.010(5) -0.004(5) B27 0.035(9) 0.031(7) 0.045(7) 0.007(5) 0.018(6) 0.014(6) B28 0.022(8) 0.038(8) 0.065(9) 0.007(6) 0.011(7) -0.014(6) B29 0.026(8) 0.036(8) 0.034(6) 0.001(5) -0.001(5) 0.000(6) B30 0.029(8) 0.025(7) 0.051(7) -0.004(5) 0.022(6) -0.009(6) B31 0.033(8) 0.027(7) 0.026(6) -0.015(5) 0.002(5) -0.002(5) B32 0.025(7) 0.017(6) 0.044(7) -0.007(5) 0.009(5) 0.000(5) B33 0.028(8) 0.034(7) 0.032(6) -0.005(5) 0.002(5) 0.006(6) B34 0.033(9) 0.035(8) 0.047(7) -0.004(6) 0.004(6) -0.001(6) B35 0.028(8) 0.028(7) 0.037(7) 0.001(5) 0.009(5) 0.004(6) B36 0.033(8) 0.023(7) 0.043(7) -0.007(5) 0.011(6) -0.007(6) B37 0.024(7) 0.018(6) 0.039(6) -0.008(5) 0.008(5) -0.011(5) B38 0.037(9) 0.028(7) 0.045(7) -0.009(5) 0.018(6) 0.002(6) B39 0.038(8) 0.023(6) 0.025(6) 0.003(4) 0.002(5) 0.003(5) N1 0.039(6) 0.021(4) 0.032(4) 0.001(3) 0.011(4) -0.004(4) C7 0.068(10) 0.042(7) 0.036(6) 0.002(5) 0.013(6) 0.011(6) C8 0.045(8) 0.033(6) 0.035(6) -0.001(5) -0.001(5) -0.007(5) N2 0.029(6) 0.013(4) 0.046(5) -0.002(4) -0.008(4) 0.002(4) C9 0.053(9) 0.059(8) 0.027(6) 0.013(5) -0.002(5) -0.005(6) C10 0.037(8) 0.037(7) 0.076(8) 0.000(6) -0.007(6) 0.005(6) N3 0.024(6) 0.028(5) 0.058(6) 0.006(4) 0.007(4) 0.008(4) C11 0.052(10) 0.075(9) 0.059(8) -0.028(7) 0.022(7) -0.037(7) C12 0.035(8) 0.087(10) 0.054(7) 0.004(7) 0.021(6) 0.021(7) N4 0.041(7) 0.026(5) 0.046(5) -0.001(4) -0.012(5) -0.002(4) C13 0.090(13) 0.051(9) 0.057(8) -0.009(6) -0.010(8) 0.012(8) C14 0.050(10) 0.067(9) 0.054(8) 0.016(6) -0.024(7) -0.015(7) Cl1 0.032(2) 0.039(2) 0.0371(14) -0.0014(11) -0.0009(12) 0.0064(13) Cl2 0.030(2) 0.037(2) 0.062(2) 0.0062(13) -0.0041(14) -0.0051(13) _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 Se1 C1 1.934(8) . ? Se1 B1 2.063(13) . ? Se2 C2 1.943(10) . ? Se2 B1 2.19(2) . ? Se3 C3 1.929(9) . ? Se3 B2 2.092(15) . ? Se4 C4 1.957(9) . ? Se4 B2 2.134(13) . ? Se5 C5 1.957(10) . ? Se5 B1 2.112(12) . ? Se6 C6 1.940(9) . ? Se6 B2 2.13(2) . ? C1 C2 1.661(12) . ? C1 B16 1.700(14) . ? C1 B18 1.710(12) . ? C1 B10 1.719(14) . ? C1 B17 1.732(13) . ? C2 B17 1.689(14) . ? C2 B19 1.699(14) . ? C2 B10 1.723(13) . ? C2 B11 1.725(13) . ? C3 C4 1.645(12) . ? C3 B28 1.71(2) . ? C3 B27 1.712(15) . ? C3 B21 1.716(15) . ? C3 B20 1.73(2) . ? C4 B29 1.701(14) . ? C4 B26 1.716(14) . ? C4 B20 1.720(15) . ? C4 B27 1.72(2) . ? C5 C6 1.666(12) . ? C5 B31 1.709(15) . ? C5 B37 1.722(14) . ? C5 B39 1.724(13) . ? C5 B30 1.731(15) . ? C6 B38 1.71(2) . ? C6 B36 1.711(14) . ? C6 B37 1.711(13) . ? C6 B30 1.727(15) . ? B1 B2 1.55(2) . ? B10 B18 1.74(2) . ? B10 B11 1.75(2) . ? B10 B12 1.76(2) . ? B11 B12 1.75(2) . ? B11 B13 1.78(2) . ? B11 B19 1.81(2) . ? B12 B13 1.76(2) . ? B12 B14 1.77(2) . ? B12 B18 1.78(2) . ? B13 B14 1.76(2) . ? B13 B15 1.77(2) . ? B13 B19 1.78(2) . ? B14 B15 1.78(2) . ? B14 B18 1.778(15) . ? B14 B16 1.78(2) . ? B15 B19 1.77(2) . ? B15 B16 1.78(2) . ? B15 B17 1.78(2) . ? B16 B17 1.79(2) . ? B16 B18 1.79(2) . ? B17 B19 1.73(2) . ? B20 B21 1.76(2) . ? B20 B22 1.76(2) . ? B20 B29 1.771(14) . ? B21 B22 1.78(2) . ? B21 B23 1.80(2) . ? B21 B28 1.82(2) . ? B22 B24 1.77(2) . ? B22 B29 1.79(2) . ? B22 B23 1.81(2) . ? B23 B24 1.78(2) . ? B23 B28 1.79(2) . ? B23 B25 1.81(2) . ? B24 B29 1.79(2) . ? B24 B26 1.79(2) . ? B24 B25 1.80(2) . ? B25 B27 1.76(2) . ? B25 B26 1.78(2) . ? B25 B28 1.79(2) . ? B26 B29 1.78(2) . ? B26 B27 1.79(2) . ? B27 B28 1.75(2) . ? B30 B38 1.78(2) . ? B30 B32 1.79(2) . ? B30 B31 1.80(2) . ? B31 B33 1.74(2) . ? B31 B39 1.77(2) . ? B31 B32 1.77(2) . ? B32 B34 1.77(2) . ? B32 B38 1.79(2) . ? B32 B33 1.80(2) . ? B33 B39 1.76(2) . ? B33 B35 1.77(2) . ? B33 B34 1.78(2) . ? B34 B38 1.78(2) . ? B34 B35 1.79(2) . ? B34 B36 1.79(2) . ? B35 B36 1.76(2) . ? B35 B39 1.775(15) . ? B35 B37 1.78(2) . ? B36 B38 1.74(2) . ? B36 B37 1.78(2) . ? B37 B39 1.789(15) . ? N1 C8 1.476(10) . ? N1 C7 1.478(11) . ? N2 C9 1.472(12) . ? N2 C10 1.473(12) . ? N3 C11 1.457(12) . ? N3 C12 1.466(12) . ? N4 C13 1.468(14) . ? N4 C14 1.469(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Se1 B1 97.3(6) . . ? C2 Se2 B1 95.4(4) . . ? C3 Se3 B2 98.7(5) . . ? C4 Se4 B2 96.9(5) . . ? C5 Se5 B1 108.5(6) . . ? C6 Se6 B2 108.1(4) . . ? C2 C1 B16 110.1(7) . . ? C2 C1 B18 110.0(7) . . ? B16 C1 B18 63.4(6) . . ? C2 C1 B10 61.3(6) . . ? B16 C1 B10 113.0(7) . . ? B18 C1 B10 60.9(6) . . ? C2 C1 B17 59.7(6) . . ? B16 C1 B17 62.8(6) . . ? B18 C1 B17 114.1(7) . . ? B10 C1 B17 112.0(7) . . ? C2 C1 Se1 118.4(6) . . ? B16 C1 Se1 122.1(7) . . ? B18 C1 Se1 120.8(6) . . ? B10 C1 Se1 116.9(6) . . ? B17 C1 Se1 118.6(6) . . ? C1 C2 B17 62.3(6) . . ? C1 C2 B19 110.8(8) . . ? B17 C2 B19 61.3(6) . . ? C1 C2 B10 61.0(6) . . ? B17 C2 B10 114.0(8) . . ? B19 C2 B10 113.4(7) . . ? C1 C2 B11 110.5(7) . . ? B17 C2 B11 114.5(8) . . ? B19 C2 B11 64.0(6) . . ? B10 C2 B11 61.0(6) . . ? C1 C2 Se2 116.8(6) . . ? B17 C2 Se2 116.4(6) . . ? B19 C2 Se2 122.1(6) . . ? B10 C2 Se2 117.4(7) . . ? B11 C2 Se2 121.9(7) . . ? C4 C3 B28 111.0(7) . . ? C4 C3 B27 61.7(6) . . ? B28 C3 B27 61.7(7) . . ? C4 C3 B21 110.7(7) . . ? B28 C3 B21 64.3(7) . . ? B27 C3 B21 114.7(8) . . ? C4 C3 B20 61.3(6) . . ? B28 C3 B20 114.5(8) . . ? B27 C3 B20 114.1(7) . . ? B21 C3 B20 61.5(7) . . ? C4 C3 Se3 116.4(6) . . ? B28 C3 Se3 121.8(7) . . ? B27 C3 Se3 116.0(7) . . ? B21 C3 Se3 122.2(6) . . ? B20 C3 Se3 116.9(7) . . ? C3 C4 B29 111.7(8) . . ? C3 C4 B26 111.4(8) . . ? B29 C4 B26 63.0(6) . . ? C3 C4 B20 61.7(6) . . ? B29 C4 B20 62.4(6) . . ? B26 C4 B20 114.3(8) . . ? C3 C4 B27 61.1(6) . . ? B29 C4 B27 114.6(8) . . ? B26 C4 B27 62.6(7) . . ? B20 C4 B27 114.0(8) . . ? C3 C4 Se4 116.5(6) . . ? B29 C4 Se4 122.4(7) . . ? B26 C4 Se4 120.9(6) . . ? B20 C4 Se4 117.8(7) . . ? B27 C4 Se4 115.3(7) . . ? C6 C5 B31 110.5(8) . . ? C6 C5 B37 60.6(6) . . ? B31 C5 B37 113.1(8) . . ? C6 C5 B39 110.7(7) . . ? B31 C5 B39 61.9(6) . . ? B37 C5 B39 62.6(6) . . ? C6 C5 B30 61.1(6) . . ? B31 C5 B30 62.9(7) . . ? B37 C5 B30 113.3(7) . . ? B39 C5 B30 114.3(8) . . ? C6 C5 Se5 121.7(6) . . ? B31 C5 Se5 118.6(6) . . ? B37 C5 Se5 119.3(7) . . ? B39 C5 Se5 118.9(6) . . ? B30 C5 Se5 117.2(6) . . ? C5 C6 B38 110.4(8) . . ? C5 C6 B36 110.4(7) . . ? B38 C6 B36 61.2(7) . . ? C5 C6 B37 61.3(5) . . ? B38 C6 B37 113.2(8) . . ? B36 C6 B37 62.6(6) . . ? C5 C6 B30 61.3(6) . . ? B38 C6 B30 62.4(7) . . ? B36 C6 B30 113.0(8) . . ? B37 C6 B30 114.1(7) . . ? C5 C6 Se6 123.4(6) . . ? B38 C6 Se6 117.2(6) . . ? B36 C6 Se6 118.3(6) . . ? B37 C6 Se6 119.5(7) . . ? B30 C6 Se6 117.7(6) . . ? B2 B1 Se1 113.0(10) . . ? B2 B1 Se5 110.2(9) . . ? Se1 B1 Se5 114.5(6) . . ? B2 B1 Se2 107.7(10) . . ? Se1 B1 Se2 108.6(7) . . ? Se5 B1 Se2 102.1(6) . . ? B1 B2 Se3 113.4(10) . . ? B1 B2 Se6 107.2(10) . . ? Se3 B2 Se6 116.2(8) . . ? B1 B2 Se4 113.1(10) . . ? Se3 B2 Se4 106.0(6) . . ? Se6 B2 Se4 100.3(6) . . ? C1 B10 C2 57.7(5) . . ? C1 B10 B18 59.3(6) . . ? C2 B10 B18 105.9(8) . . ? C1 B10 B11 106.6(7) . . ? C2 B10 B11 59.6(6) . . ? B18 B10 B11 109.6(9) . . ? C1 B10 B12 106.4(8) . . ? C2 B10 B12 105.5(8) . . ? B18 B10 B12 61.1(7) . . ? B11 B10 B12 59.9(7) . . ? C2 B11 B10 59.4(6) . . ? C2 B11 B12 105.7(8) . . ? B10 B11 B12 60.3(7) . . ? C2 B11 B13 103.8(8) . . ? B10 B11 B13 107.1(9) . . ? B12 B11 B13 59.5(7) . . ? C2 B11 B19 57.3(6) . . ? B10 B11 B19 106.7(8) . . ? B12 B11 B19 107.2(9) . . ? B13 B11 B19 59.5(6) . . ? B11 B12 B13 61.1(7) . . ? B11 B12 B10 59.8(6) . . ? B13 B12 B10 107.9(8) . . ? B11 B12 B14 108.9(8) . . ? B13 B12 B14 59.9(6) . . ? B10 B12 B14 107.1(8) . . ? B11 B12 B18 107.6(8) . . ? B13 B12 B18 108.0(8) . . ? B10 B12 B18 58.8(6) . . ? B14 B12 B18 60.1(6) . . ? B12 B13 B14 60.4(7) . . ? B12 B13 B15 109.1(8) . . ? B14 B13 B15 60.3(6) . . ? B12 B13 B11 59.4(7) . . ? B14 B13 B11 107.9(8) . . ? B15 B13 B11 109.0(8) . . ? B12 B13 B19 108.4(8) . . ? B14 B13 B19 107.7(8) . . ? B15 B13 B19 59.6(6) . . ? B11 B13 B19 61.1(6) . . ? B13 B14 B12 59.6(7) . . ? B13 B14 B15 60.1(7) . . ? B12 B14 B15 108.3(9) . . ? B13 B14 B18 107.7(8) . . ? B12 B14 B18 60.1(6) . . ? B15 B14 B18 108.5(8) . . ? B13 B14 B16 107.8(8) . . ? B12 B14 B16 108.4(8) . . ? B15 B14 B16 60.0(6) . . ? B18 B14 B16 60.4(6) . . ? B19 B15 B13 60.6(7) . . ? B19 B15 B14 107.8(8) . . ? B13 B15 B14 59.5(6) . . ? B19 B15 B16 106.8(8) . . ? B13 B15 B16 107.5(8) . . ? B14 B15 B16 60.2(6) . . ? B19 B15 B17 58.2(6) . . ? B13 B15 B17 106.9(8) . . ? B14 B15 B17 107.9(8) . . ? B16 B15 B17 60.3(6) . . ? C1 B16 B15 106.1(9) . . ? C1 B16 B14 105.1(8) . . ? B15 B16 B14 59.8(6) . . ? C1 B16 B17 59.5(6) . . ? B15 B16 B17 60.0(7) . . ? B14 B16 B17 107.4(9) . . ? C1 B16 B18 58.6(6) . . ? B15 B16 B18 107.7(9) . . ? B14 B16 B18 59.6(6) . . ? B17 B16 B18 107.6(8) . . ? C2 B17 B19 59.7(6) . . ? C2 B17 C1 58.1(5) . . ? B19 B17 C1 106.2(7) . . ? C2 B17 B15 105.8(8) . . ? B19 B17 B15 60.4(7) . . ? C1 B17 B15 104.5(7) . . ? C2 B17 B16 104.7(7) . . ? B19 B17 B16 108.3(8) . . ? C1 B17 B16 57.7(6) . . ? B15 B17 B16 59.8(6) . . ? C1 B18 B10 59.8(6) . . ? C1 B18 B14 104.9(7) . . ? B10 B18 B14 107.7(8) . . ? C1 B18 B12 106.0(8) . . ? B10 B18 B12 60.1(7) . . ? B14 B18 B12 59.7(6) . . ? C1 B18 B16 58.0(5) . . ? B10 B18 B16 107.7(8) . . ? B14 B18 B16 59.9(6) . . ? B12 B18 B16 107.7(8) . . ? C2 B19 B17 59.1(6) . . ? C2 B19 B15 106.1(8) . . ? B17 B19 B15 61.4(7) . . ? C2 B19 B13 104.7(7) . . ? B17 B19 B13 108.9(9) . . ? B15 B19 B13 59.9(7) . . ? C2 B19 B11 58.7(6) . . ? B17 B19 B11 108.3(8) . . ? B15 B19 B11 107.8(8) . . ? B13 B19 B11 59.4(6) . . ? C4 B20 C3 57.0(6) . . ? C4 B20 B21 105.3(9) . . ? C3 B20 B21 59.0(6) . . ? C4 B20 B22 105.1(8) . . ? C3 B20 B22 105.4(9) . . ? B21 B20 B22 60.9(7) . . ? C4 B20 B29 58.3(6) . . ? C3 B20 B29 104.7(8) . . ? B21 B20 B29 109.5(9) . . ? B22 B20 B29 60.8(6) . . ? C3 B21 B20 59.6(6) . . ? C3 B21 B22 105.0(8) . . ? B20 B21 B22 59.7(7) . . ? C3 B21 B23 103.9(8) . . ? B20 B21 B23 108.1(8) . . ? B22 B21 B23 60.6(7) . . ? C3 B21 B28 57.7(6) . . ? B20 B21 B28 107.6(8) . . ? B22 B21 B28 107.6(9) . . ? B23 B21 B28 59.3(7) . . ? B20 B22 B24 108.0(9) . . ? B20 B22 B21 59.5(7) . . ? B24 B22 B21 108.0(10) . . ? B20 B22 B29 59.8(6) . . ? B24 B22 B29 60.4(7) . . ? B21 B22 B29 107.6(8) . . ? B20 B22 B23 107.6(9) . . ? B24 B22 B23 59.8(7) . . ? B21 B22 B23 60.1(7) . . ? B29 B22 B23 108.0(9) . . ? B24 B23 B28 107.4(9) . . ? B24 B23 B21 106.6(9) . . ? B28 B23 B21 61.0(7) . . ? B24 B23 B22 59.0(7) . . ? B28 B23 B22 107.9(9) . . ? B21 B23 B22 59.3(7) . . ? B24 B23 B25 60.1(7) . . ? B28 B23 B25 59.7(7) . . ? B21 B23 B25 108.3(8) . . ? B22 B23 B25 107.5(9) . . ? B22 B24 B23 61.2(7) . . ? B22 B24 B29 60.4(7) . . ? B23 B24 B29 109.1(8) . . ? B22 B24 B26 108.7(9) . . ? B23 B24 B26 108.5(9) . . ? B29 B24 B26 59.8(7) . . ? B22 B24 B25 109.8(9) . . ? B23 B24 B25 60.8(7) . . ? B29 B24 B25 108.0(9) . . ? B26 B24 B25 59.5(7) . . ? B27 B25 B26 60.5(7) . . ? B27 B25 B28 59.1(6) . . ? B26 B25 B28 107.6(9) . . ? B27 B25 B24 107.3(9) . . ? B26 B25 B24 59.9(7) . . ? B28 B25 B24 106.4(9) . . ? B27 B25 B23 106.7(8) . . ? B26 B25 B23 107.4(9) . . ? B28 B25 B23 59.5(7) . . ? B24 B25 B23 59.1(7) . . ? C4 B26 B25 104.9(8) . . ? C4 B26 B29 58.1(6) . . ? B25 B26 B29 109.0(9) . . ? C4 B26 B27 58.8(6) . . ? B25 B26 B27 59.2(7) . . ? B29 B26 B27 107.5(8) . . ? C4 B26 B24 103.7(8) . . ? B25 B26 B24 60.6(7) . . ? B29 B26 B24 60.0(7) . . ? B27 B26 B24 106.8(9) . . ? C3 B27 C4 57.3(6) . . ? C3 B27 B28 59.1(6) . . ? C4 B27 B28 105.4(8) . . ? C3 B27 B25 106.3(8) . . ? C4 B27 B25 105.5(8) . . ? B28 B27 B25 61.4(7) . . ? C3 B27 B26 105.1(8) . . ? C4 B27 B26 58.5(6) . . ? B28 B27 B26 109.2(9) . . ? B25 B27 B26 60.3(7) . . ? C3 B28 B27 59.2(7) . . ? C3 B28 B23 104.6(9) . . ? B27 B28 B23 108.1(9) . . ? C3 B28 B25 105.1(8) . . ? B27 B28 B25 59.5(7) . . ? B23 B28 B25 60.8(7) . . ? C3 B28 B21 58.1(7) . . ? B27 B28 B21 107.7(9) . . ? B23 B28 B21 59.8(7) . . ? B25 B28 B21 108.2(9) . . ? C4 B29 B20 59.3(6) . . ? C4 B29 B26 58.9(6) . . ? B20 B29 B26 108.5(8) . . ? C4 B29 B22 104.9(8) . . ? B20 B29 B22 59.4(7) . . ? B26 B29 B22 108.1(10) . . ? C4 B29 B24 104.5(9) . . ? B20 B29 B24 106.7(9) . . ? B26 B29 B24 60.2(7) . . ? B22 B29 B24 59.3(7) . . ? C6 B30 C5 57.6(6) . . ? C6 B30 B38 58.3(6) . . ? C5 B30 B38 104.2(8) . . ? C6 B30 B32 105.0(8) . . ? C5 B30 B32 104.4(8) . . ? B38 B30 B32 60.0(6) . . ? C6 B30 B31 103.8(8) . . ? C5 B30 B31 57.9(6) . . ? B38 B30 B31 106.2(8) . . ? B32 B30 B31 59.2(6) . . ? C5 B31 B33 106.1(8) . . ? C5 B31 B39 59.5(6) . . ? B33 B31 B39 60.0(7) . . ? C5 B31 B32 106.3(7) . . ? B33 B31 B32 61.4(6) . . ? B39 B31 B32 109.6(8) . . ? C5 B31 B30 59.1(6) . . ? B33 B31 B30 109.6(7) . . ? B39 B31 B30 109.1(8) . . ? B32 B31 B30 60.4(6) . . ? B34 B32 B31 107.2(9) . . ? B34 B32 B38 60.2(6) . . ? B31 B32 B38 106.7(9) . . ? B34 B32 B30 108.6(8) . . ? B31 B32 B30 60.4(6) . . ? B38 B32 B30 59.6(6) . . ? B34 B32 B33 60.0(6) . . ? B31 B32 B33 58.5(6) . . ? B38 B32 B33 106.7(8) . . ? B30 B32 B33 107.2(8) . . ? B31 B33 B39 60.6(7) . . ? B31 B33 B35 108.3(8) . . ? B39 B33 B35 60.5(7) . . ? B31 B33 B34 108.0(8) . . ? B39 B33 B34 109.5(8) . . ? B35 B33 B34 60.5(6) . . ? B31 B33 B32 60.1(6) . . ? B39 B33 B32 109.0(8) . . ? B35 B33 B32 107.7(8) . . ? B34 B33 B32 59.3(6) . . ? B32 B34 B33 60.7(7) . . ? B32 B34 B38 60.4(6) . . ? B33 B34 B38 107.4(9) . . ? B32 B34 B35 107.8(9) . . ? B33 B34 B35 59.3(7) . . ? B38 B34 B35 105.7(9) . . ? B32 B34 B36 106.9(9) . . ? B33 B34 B36 106.2(9) . . ? B38 B34 B36 58.2(7) . . ? B35 B34 B36 59.0(7) . . ? B36 B35 B33 108.3(8) . . ? B36 B35 B39 108.4(8) . . ? B33 B35 B39 59.4(7) . . ? B36 B35 B37 60.2(6) . . ? B33 B35 B37 107.9(8) . . ? B39 B35 B37 60.4(6) . . ? B36 B35 B34 60.7(7) . . ? B33 B35 B34 60.3(7) . . ? B39 B35 B34 108.4(8) . . ? B37 B35 B34 109.1(8) . . ? C6 B36 B38 59.3(6) . . ? C6 B36 B35 105.7(7) . . ? B38 B36 B35 108.7(8) . . ? C6 B36 B37 58.7(6) . . ? B38 B36 B37 108.4(8) . . ? B35 B36 B37 60.4(6) . . ? C6 B36 B34 106.4(8) . . ? B38 B36 B34 60.6(7) . . ? B35 B36 B34 60.3(7) . . ? B37 B36 B34 109.0(8) . . ? C6 B37 C5 58.0(5) . . ? C6 B37 B36 58.7(6) . . ? C5 B37 B36 104.8(8) . . ? C6 B37 B35 104.9(8) . . ? C5 B37 B35 104.5(8) . . ? B36 B37 B35 59.4(6) . . ? C6 B37 B39 105.6(8) . . ? C5 B37 B39 58.8(6) . . ? B36 B37 B39 107.2(9) . . ? B35 B37 B39 59.6(6) . . ? C6 B38 B36 59.5(7) . . ? C6 B38 B30 59.3(6) . . ? B36 B38 B30 109.1(9) . . ? C6 B38 B34 107.0(9) . . ? B36 B38 B34 61.2(7) . . ? B30 B38 B34 108.7(8) . . ? C6 B38 B32 106.1(8) . . ? B36 B38 B32 108.6(8) . . ? B30 B38 B32 60.4(6) . . ? B34 B38 B32 59.5(6) . . ? C5 B39 B33 105.0(8) . . ? C5 B39 B31 58.6(6) . . ? B33 B39 B31 59.4(7) . . ? C5 B39 B35 104.8(7) . . ? B33 B39 B35 60.0(7) . . ? B31 B39 B35 106.9(9) . . ? C5 B39 B37 58.7(6) . . ? B33 B39 B37 108.1(8) . . ? B31 B39 B37 107.2(7) . . ? B35 B39 B37 60.0(6) . . ? C8 N1 C7 114.9(7) . . ? C9 N2 C10 115.2(8) . . ? C11 N3 C12 115.5(9) . . ? C13 N4 C14 116.6(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se1 B1 B2 Se3 174.1(7) . . . . ? Se1 B1 B2 Se4 53.3(14) . . . . ? Se1 B1 B2 Se6 -56.3(11) . . . . ? Se2 B1 B2 Se3 54.2(11) . . . . ? Se2 B1 B2 Se4 -66.6(10) . . . . ? Se2 B1 B2 Se6 -176..2(5) . . . . ? Se5 B1 B2 Se3 -56.4(13) . . . . ? Se5 B1 B2 Se4 -177.2(7) . . . . ? Se5 B1 B2 Se6 73.2(10) . . . . ? _refine_diff_density_max 2.062 _refine_diff_density_min -1.472 _refine_diff_density_rms 0.162