Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Jennifer L. White' 'Joseph M. Tanski' 'Daniel Rabinovich' _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Prof Daniel Rabinovich' _publ_contact_author_address ; Chemistry The University of North Carolina at Charlotte 9201 University City Blvd Charlotte North Carolina 28223 UNITED STATES OF AMERICA ; _publ_contact_author_email 'DRABINOV@EMAIL.UNCC.EDU' _publ_section_title ; Bulky tris(mercaptoimidazolyl)borates: synthesis and molecular structures of the group 12 metal complexes (TmtBu)MBr (M = Zn, Cd, Hg) ; data_danzns20 _database_code_CSD 176312 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H37 B Br N7 S3 Zn' _chemical_formula_weight 663.87 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.6992(8) _cell_length_b 33.035(3) _cell_length_c 10.2817(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.407(2) _cell_angle_gamma 90.00 _cell_volume 3107.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 238(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 2.303 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6559 _exptl_absorpt_correction_T_max 0.8024 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 238(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20156 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6938 _reflns_number_gt 6016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6938 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.735 _refine_ls_restrained_S_all 1.735 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.17567(3) 0.126240(9) 0.42519(3) 0.03068(11) Uani 1 1 d . . . Br Br 0.04004(3) 0.160209(10) 0.54623(4) 0.05098(12) Uani 1 1 d . . . B B 0.4123(3) 0.07476(10) 0.2780(3) 0.0353(7) Uani 1 1 d . . . S1 S 0.33217(7) 0.170745(19) 0.36253(7) 0.03059(15) Uani 1 1 d . . . S2 S 0.33076(7) 0.07883(2) 0.57736(7) 0.03464(17) Uani 1 1 d . . . S3 S 0.04404(7) 0.09211(2) 0.22009(8) 0.03790(17) Uani 1 1 d . . . N11 N 0.3502(2) 0.11111(7) 0.1816(2) 0.0345(5) Uani 1 1 d . . . N12 N 0.2543(3) 0.16801(7) 0.0790(2) 0.0347(5) Uani 1 1 d . . . N21 N 0.5111(2) 0.08849(6) 0.4238(2) 0.0312(5) Uani 1 1 d . . . N22 N 0.6060(2) 0.11170(7) 0.6349(2) 0.0337(5) Uani 1 1 d . . . N31 N 0.2901(2) 0.04419(7) 0.2817(2) 0.0331(5) Uani 1 1 d . . . N32 N 0.0907(2) 0.01012(7) 0.2672(2) 0.0327(5) Uani 1 1 d . . . C11 C 0.3118(3) 0.14951(8) 0.2034(3) 0.0296(5) Uani 1 1 d . . . C12 C 0.3145(3) 0.10595(10) 0.0413(3) 0.0432(7) Uani 1 1 d . . . H12A H 0.3298 0.0823 -0.0027 0.052 Uiso 1 1 calc R . . C13 C 0.2542(4) 0.14043(10) -0.0224(3) 0.0440(7) Uani 1 1 d . . . H13A H 0.2186 0.1449 -0.1181 0.053 Uiso 1 1 calc R . . C14 C 0.1932(3) 0.21038(8) 0.0514(3) 0.0377(6) Uani 1 1 d . . . C15 C 0.1416(4) 0.21808(11) -0.1032(3) 0.0597(9) Uani 1 1 d . . . H15A H 0.0644 0.1991 -0.1491 0.089 Uiso 1 1 calc R . . H15B H 0.2228 0.2145 -0.1374 0.089 Uiso 1 1 calc R . . H15C H 0.1048 0.2455 -0.1217 0.089 Uiso 1 1 calc R . . C16 C 0.3140(3) 0.24082(9) 0.1218(4) 0.0476(8) Uani 1 1 d . . . H16A H 0.3487 0.2361 0.2205 0.071 Uiso 1 1 calc R . . H16B H 0.2755 0.2681 0.1033 0.071 Uiso 1 1 calc R . . H16C H 0.3943 0.2376 0.0863 0.071 Uiso 1 1 calc R . . C17 C 0.0630(3) 0.21407(10) 0.1022(3) 0.0464(7) Uani 1 1 d . . . H17A H 0.0949 0.2095 0.2009 0.070 Uiso 1 1 calc R . . H17B H -0.0103 0.1941 0.0560 0.070 Uiso 1 1 calc R . . H17C H 0.0213 0.2410 0.0820 0.070 Uiso 1 1 calc R . . C21 C 0.4871(3) 0.09334(8) 0.5444(3) 0.0295(5) Uani 1 1 d . . . C22 C 0.6474(3) 0.10425(9) 0.4383(3) 0.0391(7) Uani 1 1 d . . . H22A H 0.6918 0.1048 0.3697 0.047 Uiso 1 1 calc R . . C23 C 0.7053(3) 0.11853(8) 0.5669(3) 0.0399(7) Uani 1 1 d . . . H23A H 0.7971 0.1310 0.6043 0.048 Uiso 1 1 calc R . . C24 C 0.6230(3) 0.12780(10) 0.7770(3) 0.0437(7) Uani 1 1 d . . . C25 C 0.5113(4) 0.16103(11) 0.7650(4) 0.0567(9) Uani 1 1 d . . . H25A H 0.5256 0.1825 0.7064 0.085 Uiso 1 1 calc R . . H25B H 0.5233 0.1718 0.8558 0.085 Uiso 1 1 calc R . . H25C H 0.4136 0.1500 0.7251 0.085 Uiso 1 1 calc R . . C26 C 0.7772(4) 0.14526(15) 0.8402(5) 0.0772(13) Uani 1 1 d . . . H26A H 0.7902 0.1675 0.7836 0.116 Uiso 1 1 calc R . . H26B H 0.8487 0.1243 0.8445 0.116 Uiso 1 1 calc R . . H26C H 0.7904 0.1551 0.9325 0.116 Uiso 1 1 calc R . . C27 C 0.6058(4) 0.09308(12) 0.8690(3) 0.0582(9) Uani 1 1 d . . . H27A H 0.5085 0.0817 0.8309 0.087 Uiso 1 1 calc R . . H27B H 0.6202 0.1033 0.9610 0.087 Uiso 1 1 calc R . . H27C H 0.6779 0.0723 0.8732 0.087 Uiso 1 1 calc R . . C31 C 0.1439(3) 0.04785(8) 0.2555(3) 0.0311(5) Uani 1 1 d . . . C32 C 0.3280(3) 0.00427(8) 0.3133(3) 0.0407(7) Uani 1 1 d . . . H32A H 0.4229 -0.0065 0.3369 0.049 Uiso 1 1 calc R . . C33 C 0.2069(3) -0.01668(8) 0.3049(3) 0.0397(6) Uani 1 1 d . . . H33A H 0.2019 -0.0445 0.3215 0.048 Uiso 1 1 calc R . . C34 C -0.0676(3) -0.00207(9) 0.2356(3) 0.0360(6) Uani 1 1 d . . . C35 C -0.1493(3) 0.00676(12) 0.0825(3) 0.0528(9) Uani 1 1 d . . . H35A H -0.1043 -0.0083 0.0261 0.079 Uiso 1 1 calc R . . H35B H -0.1445 0.0355 0.0652 0.079 Uiso 1 1 calc R . . H35C H -0.2507 -0.0014 0.0595 0.079 Uiso 1 1 calc R . . C36 C -0.1365(4) 0.02050(11) 0.3274(3) 0.0518(8) Uani 1 1 d . . . H36A H -0.0831 0.0144 0.4233 0.078 Uiso 1 1 calc R . . H36B H -0.2375 0.0121 0.3055 0.078 Uiso 1 1 calc R . . H36C H -0.1328 0.0494 0.3120 0.078 Uiso 1 1 calc R . . C37 C -0.0736(4) -0.04740(9) 0.2596(3) 0.0469(7) Uani 1 1 d . . . H37A H -0.0225 -0.0534 0.3560 0.070 Uiso 1 1 calc R . . H37B H -0.0274 -0.0618 0.2028 0.070 Uiso 1 1 calc R . . H37C H -0.1747 -0.0559 0.2354 0.070 Uiso 1 1 calc R . . H1 H 0.486(3) 0.0600(9) 0.227(3) 0.039(8) Uiso 1 1 d . . . C2S C 0.7027(6) 0.22153(19) 0.3692(7) 0.1045(18) Uani 1 1 d . . . C1S C 0.6944(8) 0.2055(4) 0.2424(11) 0.196(5) Uani 1 1 d . . . N1S N 0.6865(12) 0.1918(7) 0.1398(11) 0.410(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.02883(16) 0.03071(17) 0.03331(19) -0.00099(13) 0.01142(13) 0.00020(12) Br 0.04644(19) 0.0515(2) 0.0672(2) -0.00897(16) 0.03529(17) -0.00059(14) B 0.0359(15) 0.0305(15) 0.0419(18) -0.0027(14) 0.0160(14) 0.0019(12) S1 0.0400(4) 0.0272(3) 0.0255(3) -0.0020(3) 0.0121(3) -0.0038(3) S2 0.0274(3) 0.0406(4) 0.0369(4) 0.0086(3) 0.0120(3) -0.0023(3) S3 0.0344(3) 0.0275(3) 0.0425(4) -0.0019(3) 0.0003(3) 0.0033(3) N11 0.0446(13) 0.0323(12) 0.0301(12) -0.0032(10) 0.0173(10) -0.0021(10) N12 0.0459(13) 0.0327(12) 0.0264(12) 0.0012(10) 0.0132(10) -0.0040(10) N21 0.0262(10) 0.0282(11) 0.0414(13) 0.0025(10) 0.0140(10) 0.0003(8) N22 0.0278(11) 0.0320(12) 0.0378(13) 0.0025(10) 0.0065(10) 0.0004(9) N31 0.0347(11) 0.0248(11) 0.0369(13) -0.0012(9) 0.0081(10) 0.0024(9) N32 0.0388(12) 0.0273(11) 0.0286(12) -0.0007(9) 0.0066(10) -0.0007(9) C11 0.0364(13) 0.0288(13) 0.0262(13) 0.0013(11) 0.0138(11) -0.0027(10) C12 0.0610(19) 0.0411(17) 0.0297(15) -0.0094(13) 0.0180(14) -0.0025(14) C13 0.0628(19) 0.0454(17) 0.0267(15) -0.0049(13) 0.0185(14) -0.0028(15) C14 0.0481(16) 0.0309(14) 0.0316(15) 0.0036(12) 0.0098(13) -0.0017(12) C15 0.088(3) 0.051(2) 0.0330(17) 0.0123(15) 0.0116(17) 0.0039(19) C16 0.0502(17) 0.0310(15) 0.060(2) 0.0099(14) 0.0155(16) -0.0057(13) C17 0.0380(15) 0.0479(18) 0.0459(18) -0.0044(15) 0.0039(13) -0.0003(13) C21 0.0244(11) 0.0260(12) 0.0357(15) 0.0065(11) 0.0069(11) 0.0015(10) C22 0.0299(13) 0.0381(16) 0.0542(19) 0.0061(14) 0.0205(13) 0.0006(11) C23 0.0236(12) 0.0375(15) 0.058(2) 0.0043(14) 0.0124(13) -0.0011(11) C24 0.0380(15) 0.0480(18) 0.0380(16) -0.0056(14) 0.0032(13) -0.0001(13) C25 0.057(2) 0.051(2) 0.058(2) -0.0087(16) 0.0122(17) 0.0082(15) C26 0.049(2) 0.098(3) 0.070(3) -0.029(2) -0.0002(19) -0.014(2) C27 0.065(2) 0.067(2) 0.0355(18) 0.0062(17) 0.0076(16) 0.0093(18) C31 0.0359(14) 0.0256(13) 0.0271(13) -0.0008(10) 0.0041(11) 0.0002(10) C32 0.0397(15) 0.0278(14) 0.0515(19) 0.0018(13) 0.0112(13) 0.0047(11) C33 0.0457(16) 0.0259(13) 0.0456(18) 0.0042(12) 0.0127(14) 0.0029(12) C34 0.0385(14) 0.0389(15) 0.0294(14) -0.0022(12) 0.0098(12) -0.0061(12) C35 0.0440(17) 0.068(2) 0.0357(17) 0.0005(16) -0.0008(14) -0.0157(16) C36 0.0581(19) 0.054(2) 0.051(2) -0.0089(16) 0.0279(16) -0.0024(15) C37 0.0548(18) 0.0419(17) 0.0480(19) -0.0039(14) 0.0224(15) -0.0133(14) C2S 0.080(3) 0.110(5) 0.101(4) -0.003(4) -0.001(3) 0.002(3) C1S 0.077(4) 0.359(16) 0.148(8) 0.090(10) 0.034(5) 0.065(7) N1S 0.167(9) 0.90(3) 0.158(9) -0.050(15) 0.042(8) 0.144(14) _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 Zn S1 2.3517(7) . ? Zn S3 2.3578(8) . ? Zn S2 2.3663(8) . ? Zn Br 2.3720(4) . ? B N11 1.546(4) . ? B N21 1.554(4) . ? B N31 1.567(4) . ? S1 C11 1.730(3) . ? S2 C21 1.728(2) . ? S3 C31 1.724(3) . ? N11 C11 1.362(3) . ? N11 C12 1.377(3) . ? N12 C11 1.359(3) . ? N12 C13 1.384(4) . ? N12 C14 1.510(4) . ? N21 C21 1.345(3) . ? N21 C22 1.382(3) . ? N22 C21 1.360(3) . ? N22 C23 1.384(3) . ? N22 C24 1.511(4) . ? N31 C31 1.358(3) . ? N31 C32 1.379(3) . ? N32 C31 1.370(3) . ? N32 C33 1.383(3) . ? N32 C34 1.515(3) . ? C12 C13 1.347(4) . ? C14 C15 1.520(4) . ? C14 C17 1.524(4) . ? C14 C16 1.531(4) . ? C22 C23 1.339(4) . ? C24 C25 1.518(4) . ? C24 C27 1.531(5) . ? C24 C26 1.532(5) . ? C32 C33 1.341(4) . ? C34 C36 1.520(4) . ? C34 C37 1.522(4) . ? C34 C35 1.537(4) . ? C2S C1S 1.384(12) . ? C1S N1S 1.127(14) . ? 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 S1 Zn S3 105.12(3) . . ? S1 Zn S2 105.58(2) . . ? S3 Zn S2 108.13(3) . . ? S1 Zn Br 111.65(2) . . ? S3 Zn Br 117.75(2) . . ? S2 Zn Br 107.93(2) . . ? N11 B N21 112.1(2) . . ? N11 B N31 112.3(2) . . ? N21 B N31 113.2(2) . . ? C11 S1 Zn 97.13(9) . . ? C21 S2 Zn 95.36(9) . . ? C31 S3 Zn 96.74(9) . . ? C11 N11 C12 107.5(2) . . ? C11 N11 B 133.4(2) . . ? C12 N11 B 118.9(2) . . ? C11 N12 C13 108.1(2) . . ? C11 N12 C14 127.4(2) . . ? C13 N12 C14 124.5(2) . . ? C21 N21 C22 107.9(2) . . ? C21 N21 B 133.1(2) . . ? C22 N21 B 118.4(2) . . ? C21 N22 C23 107.6(2) . . ? C21 N22 C24 127.8(2) . . ? C23 N22 C24 124.1(2) . . ? C31 N31 C32 108.1(2) . . ? C31 N31 B 133.3(2) . . ? C32 N31 B 118.5(2) . . ? C31 N32 C33 108.1(2) . . ? C31 N32 C34 127.4(2) . . ? C33 N32 C34 124.3(2) . . ? N12 C11 N11 108.2(2) . . ? N12 C11 S1 126.2(2) . . ? N11 C11 S1 125.6(2) . . ? C13 C12 N11 108.8(3) . . ? C12 C13 N12 107.4(3) . . ? N12 C14 C15 108.9(2) . . ? N12 C14 C17 109.2(2) . . ? C15 C14 C17 108.8(3) . . ? N12 C14 C16 109.2(2) . . ? C15 C14 C16 108.6(3) . . ? C17 C14 C16 112.1(3) . . ? N21 C21 N22 108.4(2) . . ? N21 C21 S2 125.41(19) . . ? N22 C21 S2 126.1(2) . . ? C23 C22 N21 108.1(2) . . ? C22 C23 N22 107.9(2) . . ? N22 C24 C25 109.3(3) . . ? N22 C24 C27 109.5(3) . . ? C25 C24 C27 111.7(3) . . ? N22 C24 C26 108.7(3) . . ? C25 C24 C26 109.4(3) . . ? C27 C24 C26 108.1(3) . . ? N31 C31 N32 107.5(2) . . ? N31 C31 S3 126.4(2) . . ? N32 C31 S3 126.1(2) . . ? C33 C32 N31 108.6(2) . . ? C32 C33 N32 107.6(2) . . ? N32 C34 C36 111.1(2) . . ? N32 C34 C37 108.5(2) . . ? C36 C34 C37 109.5(3) . . ? N32 C34 C35 108.1(2) . . ? C36 C34 C35 111.1(3) . . ? C37 C34 C35 108.6(2) . . ? N1S C1S C2S 178.7(19) . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 0.872 _refine_diff_density_min -0.991 _refine_diff_density_rms 0.068 #===END data_dancds10 _database_code_CSD 176313 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H37 B Br Cd N7 S3' _chemical_formula_weight 710.90 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 '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 9.8222(7) _cell_length_b 32.991(2) _cell_length_c 10.4059(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.7690(10) _cell_angle_gamma 90.00 _cell_volume 3152.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.95 _exptl_crystal_size_mid 0.72 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 2.183 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.2309 _exptl_absorpt_correction_T_max 0.4205 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20883 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.24 _reflns_number_total 7056 _reflns_number_gt 6290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7056 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1295 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.188 _refine_ls_shift/su_mean 0.008 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.34091(2) 0.126761(6) 0.57494(2) 0.03369(11) Uani 1 1 d . . . Br Br 0.47502(4) 0.161691(12) 0.43779(4) 0.05384(14) Uani 1 1 d . . . B B 0.0904(4) 0.07499(10) 0.7199(3) 0.0357(7) Uani 1 1 d . . . H111 H 0.013(4) 0.0604(11) 0.763(4) 0.039(9) Uiso 1 1 d . . . S1 S 0.16237(8) 0.17210(2) 0.63351(7) 0.03274(17) Uani 1 1 d . . . S2 S 0.16921(8) 0.07383(2) 0.42181(7) 0.03628(18) Uani 1 1 d . . . S3 S 0.46169(8) 0.09027(2) 0.80154(8) 0.03814(19) Uani 1 1 d . . . N11 N 0.1512(3) 0.11240(8) 0.8140(3) 0.0355(5) Uani 1 1 d . . . N12 N 0.2496(3) 0.16908(8) 0.9160(2) 0.0362(5) Uani 1 1 d . . . N21 N -0.0065(3) 0.08826(7) 0.5709(3) 0.0329(5) Uani 1 1 d . . . N22 N -0.0983(3) 0.11085(8) 0.3592(3) 0.0363(5) Uani 1 1 d . . . N31 N 0.2119(3) 0.04437(7) 0.7221(3) 0.0356(5) Uani 1 1 d . . . N32 N 0.4077(3) 0.00951(7) 0.7371(2) 0.0351(5) Uani 1 1 d . . . C11 C 0.1883(3) 0.15036(9) 0.7919(3) 0.0318(6) Uani 1 1 d . . . C12 C 0.1900(4) 0.10732(11) 0.9548(3) 0.0460(8) Uani 1 1 d . . . H12A H 0.1763 0.0837 0.9990 0.055 Uiso 1 1 calc R . . C13 C 0.2501(4) 0.14173(10) 1.0168(3) 0.0447(7) Uani 1 1 d . . . H13A H 0.2863 0.1465 1.1120 0.054 Uiso 1 1 calc R . . C14 C 0.3137(4) 0.21106(9) 0.9443(3) 0.0394(7) Uani 1 1 d . . . C15 C 0.3714(6) 0.21866(14) 1.0984(4) 0.0639(11) Uani 1 1 d . . . H15A H 0.4477 0.1993 1.1431 0.096 Uiso 1 1 calc R . . H15B H 0.2929 0.2157 1.1337 0.096 Uiso 1 1 calc R . . H15C H 0.4105 0.2459 1.1166 0.096 Uiso 1 1 calc R . . C16 C 0.1945(4) 0.24230(10) 0.8762(4) 0.0497(8) Uani 1 1 d . . . H16A H 0.1162 0.2393 0.9117 0.075 Uiso 1 1 calc R . . H16B H 0.1571 0.2380 0.7775 0.075 Uiso 1 1 calc R . . H16C H 0.2350 0.2694 0.8962 0.075 Uiso 1 1 calc R . . C17 C 0.4408(4) 0.21407(11) 0.8920(4) 0.0455(7) Uani 1 1 d . . . H17A H 0.5136 0.1938 0.9375 0.068 Uiso 1 1 calc R . . H17B H 0.4839 0.2409 0.9117 0.068 Uiso 1 1 calc R . . H17C H 0.4055 0.2094 0.7935 0.068 Uiso 1 1 calc R . . C21 C 0.0186(3) 0.09166(9) 0.4523(3) 0.0316(6) Uani 1 1 d . . . C22 C -0.1406(3) 0.10558(10) 0.5526(4) 0.0412(7) Uani 1 1 d . . . H22A H -0.1850 0.1072 0.6189 0.049 Uiso 1 1 calc R . . C23 C -0.1958(4) 0.11969(10) 0.4237(4) 0.0441(7) Uani 1 1 d . . . H23A H -0.2852 0.1332 0.3840 0.053 Uiso 1 1 calc R . . C24 C -0.1140(4) 0.12554(11) 0.2175(4) 0.0480(8) Uani 1 1 d . . . C25 C 0.0034(5) 0.15775(13) 0.2310(4) 0.0591(10) Uani 1 1 d . . . H25A H 0.0990 0.1456 0.2716 0.089 Uiso 1 1 calc R . . H25B H -0.0067 0.1797 0.2891 0.089 Uiso 1 1 calc R . . H25C H -0.0082 0.1683 0.1407 0.089 Uiso 1 1 calc R . . C26 C -0.2640(5) 0.14544(18) 0.1527(5) 0.0773(14) Uani 1 1 d . . . H26A H -0.3394 0.1255 0.1433 0.116 Uiso 1 1 calc R . . H26B H -0.2743 0.1561 0.0628 0.116 Uiso 1 1 calc R . . H26C H -0.2733 0.1674 0.2111 0.116 Uiso 1 1 calc R . . C27 C -0.1045(5) 0.09019(14) 0.1276(4) 0.0610(10) Uani 1 1 d . . . H27A H -0.0100 0.0773 0.1672 0.092 Uiso 1 1 calc R . . H27B H -0.1170 0.1000 0.0362 0.092 Uiso 1 1 calc R . . H27C H -0.1803 0.0707 0.1219 0.092 Uiso 1 1 calc R . . C31 C 0.3562(3) 0.04697(8) 0.7526(3) 0.0321(6) Uani 1 1 d . . . C32 C 0.1706(4) 0.00447(9) 0.6858(4) 0.0433(7) Uani 1 1 d . . . H32A H 0.0755 -0.0059 0.6601 0.052 Uiso 1 1 calc R . . C33 C 0.2896(4) -0.01671(9) 0.6938(4) 0.0439(7) Uani 1 1 d . . . H33A H 0.2926 -0.0444 0.6737 0.053 Uiso 1 1 calc R . . C34 C 0.5630(4) -0.00345(9) 0.7678(3) 0.0375(6) Uani 1 1 d . . . C35 C 0.6480(4) 0.00274(13) 0.9221(3) 0.0517(9) Uani 1 1 d . . . H35A H 0.6489 0.0313 0.9443 0.077 Uiso 1 1 calc R . . H35B H 0.7472 -0.0067 0.9443 0.077 Uiso 1 1 calc R . . H35C H 0.6016 -0.0125 0.9750 0.077 Uiso 1 1 calc R . . C36 C 0.6314(5) 0.02055(13) 0.6814(4) 0.0562(9) Uani 1 1 d . . . H36A H 0.5757 0.0163 0.5847 0.084 Uiso 1 1 calc R . . H36B H 0.7307 0.0115 0.7015 0.084 Uiso 1 1 calc R . . H36C H 0.6312 0.0492 0.7029 0.084 Uiso 1 1 calc R . . C37 C 0.5662(5) -0.04828(11) 0.7353(4) 0.0507(8) Uani 1 1 d . . . H37A H 0.5131 -0.0527 0.6382 0.076 Uiso 1 1 calc R . . H37B H 0.5213 -0.0637 0.7889 0.076 Uiso 1 1 calc R . . H37C H 0.6664 -0.0570 0.7580 0.076 Uiso 1 1 calc R . . C2S C -0.1954(7) 0.2227(2) 0.6398(9) 0.113(3) Uani 1 1 d . . . H2SA H -0.2004 0.2518 0.6506 0.169 Uiso 1 1 calc R . . H2SB H -0.2813 0.2137 0.5650 0.169 Uiso 1 1 calc R . . H2SC H -0.1090 0.2161 0.6194 0.169 Uiso 1 1 calc R . . C1S C -0.1888(9) 0.2026(5) 0.7673(12) 0.176(6) Uani 1 1 d . . . N1S N -0.1857(16) 0.1870(8) 0.8583(13) 0.351(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd 0.03326(16) 0.03230(15) 0.03681(15) 0.00126(7) 0.01404(11) -0.00080(8) Br 0.0520(2) 0.0535(2) 0.0701(3) 0.01119(17) 0.03896(19) 0.00256(15) B 0.0438(18) 0.0281(15) 0.0371(15) 0.0022(12) 0.0166(14) -0.0018(13) S1 0.0424(4) 0.0269(3) 0.0299(3) 0.0018(2) 0.0139(3) 0.0035(3) S2 0.0306(4) 0.0382(4) 0.0403(4) -0.0087(3) 0.0129(3) 0.0024(3) S3 0.0389(4) 0.0274(4) 0.0391(4) -0.0004(3) 0.0027(3) -0.0036(3) N11 0.0477(15) 0.0277(12) 0.0339(11) 0.0008(9) 0.0180(11) 0.0012(10) N12 0.0467(15) 0.0308(12) 0.0313(11) -0.0028(9) 0.0143(11) 0.0020(10) N21 0.0296(12) 0.0284(12) 0.0416(12) -0.0019(9) 0.0138(10) 0.0006(9) N22 0.0293(12) 0.0330(13) 0.0432(13) -0.0028(10) 0.0086(10) 0.0000(10) N31 0.0410(14) 0.0242(12) 0.0389(12) 0.0013(9) 0.0107(11) -0.0030(10) N32 0.0415(13) 0.0267(12) 0.0338(11) -0.0008(9) 0.0092(10) 0.0028(10) C11 0.0387(15) 0.0288(13) 0.0307(12) 0.0010(10) 0.0158(11) 0.0051(11) C12 0.069(2) 0.0386(17) 0.0366(14) 0.0071(13) 0.0256(15) 0.0057(15) C13 0.066(2) 0.0400(18) 0.0311(14) 0.0021(12) 0.0206(14) 0.0045(15) C14 0.0492(18) 0.0308(15) 0.0346(14) -0.0034(11) 0.0104(13) 0.0023(13) C15 0.087(3) 0.059(2) 0.0373(17) -0.0159(16) 0.0119(18) -0.011(2) C16 0.053(2) 0.0309(16) 0.063(2) -0.0067(14) 0.0166(17) 0.0080(14) C17 0.0403(17) 0.0442(18) 0.0457(17) 0.0030(14) 0.0073(14) 0.0024(14) C21 0.0266(13) 0.0296(14) 0.0372(14) -0.0076(11) 0.0096(11) -0.0003(10) C22 0.0323(15) 0.0377(17) 0.0575(18) -0.0056(14) 0.0208(14) 0.0011(12) C23 0.0268(15) 0.0384(16) 0.065(2) -0.0035(14) 0.0133(14) 0.0038(12) C24 0.0409(19) 0.053(2) 0.0390(16) 0.0053(14) 0.0007(14) -0.0050(14) C25 0.056(2) 0.054(2) 0.058(2) 0.0109(17) 0.0097(18) -0.0127(18) C26 0.050(2) 0.097(4) 0.071(3) 0.031(3) 0.003(2) 0.013(2) C27 0.069(3) 0.068(3) 0.0382(17) -0.0067(16) 0.0084(17) -0.006(2) C31 0.0390(15) 0.0255(13) 0.0282(11) 0.0024(10) 0.0076(11) -0.0014(11) C32 0.0479(18) 0.0241(14) 0.0545(18) -0.0030(13) 0.0139(14) -0.0070(12) C33 0.0506(19) 0.0236(14) 0.0536(18) -0.0037(12) 0.0134(15) -0.0041(12) C34 0.0443(16) 0.0343(15) 0.0342(13) 0.0038(11) 0.0141(12) 0.0075(12) C35 0.050(2) 0.058(2) 0.0392(16) 0.0026(14) 0.0070(15) 0.0154(16) C36 0.063(2) 0.055(2) 0.057(2) 0.0090(17) 0.0297(18) 0.0027(18) C37 0.063(2) 0.0406(18) 0.0551(19) 0.0018(15) 0.0295(17) 0.0114(16) C2S 0.070(4) 0.104(5) 0.135(6) -0.006(4) 0.000(4) -0.002(3) C1S 0.077(5) 0.327(19) 0.116(7) -0.015(9) 0.025(5) -0.037(7) N1S 0.222(14) 0.71(4) 0.120(9) 0.103(15) 0.060(9) -0.022(17) _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 Cd S3 2.5363(8) . ? Cd Br 2.5364(4) . ? Cd S1 2.5380(8) . ? Cd S2 2.5548(8) . ? B N11 1.557(4) . ? B N31 1.557(4) . ? B N21 1.566(4) . ? S1 C11 1.732(3) . ? S2 C21 1.723(3) . ? S3 C31 1.732(3) . ? N11 C11 1.347(4) . ? N11 C12 1.387(4) . ? N12 C11 1.364(4) . ? N12 C13 1.382(4) . ? N12 C14 1.506(4) . ? N21 C21 1.347(4) . ? N21 C22 1.385(4) . ? N22 C21 1.367(4) . ? N22 C23 1.381(4) . ? N22 C24 1.508(5) . ? N31 C31 1.341(4) . ? N31 C32 1.390(4) . ? N32 C31 1.366(4) . ? N32 C33 1.388(4) . ? N32 C34 1.505(4) . ? C12 C13 1.336(5) . ? C14 C15 1.520(4) . ? C14 C16 1.532(5) . ? C14 C17 1.533(5) . ? C22 C23 1.339(5) . ? C24 C27 1.519(6) . ? C24 C26 1.534(6) . ? C24 C25 1.537(5) . ? C32 C33 1.338(5) . ? C34 C37 1.520(5) . ? C34 C36 1.521(5) . ? C34 C35 1.538(4) . ? C2S C1S 1.465(14) . ? C1S N1S 1.068(17) . ? 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 S3 Cd Br 125.01(2) . . ? S3 Cd S1 101.05(3) . . ? Br Cd S1 114.10(2) . . ? S3 Cd S2 104.07(3) . . ? Br Cd S2 108.62(2) . . ? S1 Cd S2 101.13(2) . . ? N11 B N31 112.6(3) . . ? N11 B N21 111.3(2) . . ? N31 B N21 112.9(2) . . ? C11 S1 Cd 95.94(10) . . ? C21 S2 Cd 94.12(9) . . ? C31 S3 Cd 94.84(9) . . ? C11 N11 C12 107.7(3) . . ? C11 N11 B 134.1(2) . . ? C12 N11 B 118.0(3) . . ? C11 N12 C13 107.7(3) . . ? C11 N12 C14 127.9(2) . . ? C13 N12 C14 124.3(3) . . ? C21 N21 C22 108.2(3) . . ? C21 N21 B 133.3(2) . . ? C22 N21 B 117.8(3) . . ? C21 N22 C23 107.9(3) . . ? C21 N22 C24 127.6(3) . . ? C23 N22 C24 124.0(3) . . ? C31 N31 C32 107.9(3) . . ? C31 N31 B 134.6(2) . . ? C32 N31 B 117.5(3) . . ? C31 N32 C33 107.5(3) . . ? C31 N32 C34 128.4(3) . . ? C33 N32 C34 124.0(3) . . ? N11 C11 N12 108.3(2) . . ? N11 C11 S1 126.2(2) . . ? N12 C11 S1 125.5(2) . . ? C13 C12 N11 108.4(3) . . ? C12 C13 N12 107.9(3) . . ? N12 C14 C15 109.4(3) . . ? N12 C14 C16 109.3(3) . . ? C15 C14 C16 108.4(3) . . ? N12 C14 C17 109.1(3) . . ? C15 C14 C17 108.5(3) . . ? C16 C14 C17 112.2(3) . . ? N21 C21 N22 107.9(2) . . ? N21 C21 S2 126.1(2) . . ? N22 C21 S2 126.0(2) . . ? C23 C22 N21 108.0(3) . . ? C22 C23 N22 108.0(3) . . ? N22 C24 C27 110.4(3) . . ? N22 C24 C26 108.4(3) . . ? C27 C24 C26 108.5(4) . . ? N22 C24 C25 108.7(3) . . ? C27 C24 C25 112.3(4) . . ? C26 C24 C25 108.5(4) . . ? N31 C31 N32 108.6(2) . . ? N31 C31 S3 126.5(2) . . ? N32 C31 S3 124.9(2) . . ? C33 C32 N31 108.3(3) . . ? C32 C33 N32 107.8(3) . . ? N32 C34 C37 109.2(3) . . ? N32 C34 C36 110.7(3) . . ? C37 C34 C36 109.0(3) . . ? N32 C34 C35 108.5(2) . . ? C37 C34 C35 108.4(3) . . ? C36 C34 C35 111.0(3) . . ? N1S C1S C2S 178(2) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 1.313 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.069 #===END data_zibas10 _database_code_CSD 176314 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H40 B Br Hg N6 S3' _chemical_formula_weight 836.14 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.7024(10) _cell_length_b 10.8838(6) _cell_length_c 35.013(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.7900(10) _cell_angle_gamma 90.00 _cell_volume 6698.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 6.002 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.3798 _exptl_absorpt_correction_T_max 0.7147 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22430 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 28.23 _reflns_number_total 7692 _reflns_number_gt 5353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00021(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7692 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg Hg 0.417941(12) 0.833811(18) 0.137624(6) 0.04120(9) Uani 1 1 d . . . Br Br 0.53989(4) 0.95752(6) 0.142328(19) 0.0690(2) Uani 1 1 d . . . B B 0.2362(3) 0.6432(5) 0.11848(16) 0.0319(13) Uani 1 1 d . . . S1 S 0.29034(8) 0.95021(12) 0.13302(4) 0.0426(3) Uani 1 1 d . . . S2 S 0.39673(7) 0.66746(12) 0.18590(4) 0.0392(3) Uani 1 1 d . . . S3 S 0.39959(8) 0.70002(11) 0.07547(4) 0.0361(3) Uani 1 1 d . . . N11 N 0.2283(2) 0.7538(3) 0.09010(11) 0.0290(9) Uani 1 1 d . . . N12 N 0.2297(2) 0.9244(3) 0.05635(11) 0.0343(10) Uani 1 1 d . . . N21 N 0.2426(2) 0.6817(3) 0.16188(11) 0.0344(9) Uani 1 1 d . . . N22 N 0.2740(3) 0.7410(4) 0.22163(12) 0.0454(11) Uani 1 1 d . . . N31 N 0.3009(2) 0.5533(3) 0.10983(11) 0.0301(9) Uani 1 1 d . . . N32 N 0.4068(2) 0.4588(3) 0.10014(11) 0.0345(10) Uani 1 1 d . . . C1S C 0.5000 0.3971(9) 0.2500 0.068(3) Uani 1 2 d S . . H1SA H 0.5000 0.4834 0.2500 0.082 Uiso 1 2 calc SR . . C2S C 0.4647(5) 0.3373(7) 0.2192(2) 0.081(2) Uani 1 1 d . . . H2SA H 0.4397 0.3816 0.1984 0.098 Uiso 1 1 calc R . . C3S C 0.4655(5) 0.2121(8) 0.2185(3) 0.088(2) Uani 1 1 d . . . H3SA H 0.4428 0.1697 0.1967 0.106 Uiso 1 1 calc R . . C4S C 0.5000 0.1473(9) 0.2500 0.100(5) Uani 1 2 d S . . H4SA H 0.5000 0.0609 0.2500 0.121 Uiso 1 2 calc SR . . C5S C -0.0160(3) 0.5845(5) -0.02934(17) 0.0522(15) Uani 1 1 d . . . H5SA H -0.0270 0.6415 -0.0494 0.063 Uiso 1 1 calc R . . C6S C 0.0177(4) 0.6226(5) 0.00591(19) 0.0560(16) Uani 1 1 d . . . H6SA H 0.0299 0.7060 0.0101 0.067 Uiso 1 1 calc R . . C7S C 0.0339(3) 0.5384(6) 0.03529(17) 0.0559(16) Uani 1 1 d . . . H7SA H 0.0571 0.5647 0.0594 0.067 Uiso 1 1 calc R . . C11 C 0.2486(3) 0.8733(4) 0.09185(14) 0.0346(11) Uani 1 1 d . . . C12 C 0.1968(3) 0.7309(5) 0.05301(14) 0.0350(12) Uani 1 1 d . . . H12A H 0.1773 0.6547 0.0439 0.042 Uiso 1 1 calc R . . C13 C 0.1978(3) 0.8336(5) 0.03173(15) 0.0389(12) Uani 1 1 d . . . H13A H 0.1805 0.8422 0.0054 0.047 Uiso 1 1 calc R . . C14 C 0.2453(3) 1.0537(4) 0.04345(16) 0.0419(13) Uani 1 1 d . . . C15 C 0.2034(3) 1.1453(5) 0.06603(19) 0.0558(16) Uani 1 1 d . . . H15A H 0.2227 1.1403 0.0931 0.084 Uiso 1 1 calc R . . H15B H 0.1494 1.1266 0.0627 0.084 Uiso 1 1 calc R . . H15C H 0.2113 1.2277 0.0567 0.084 Uiso 1 1 calc R . . C16 C 0.3308(3) 1.0748(5) 0.04739(18) 0.0577(16) Uani 1 1 d . . . H16A H 0.3514 1.0681 0.0742 0.087 Uiso 1 1 calc R . . H16B H 0.3411 1.1562 0.0380 0.087 Uiso 1 1 calc R . . H16C H 0.3543 1.0136 0.0325 0.087 Uiso 1 1 calc R . . C17 C 0.2140(4) 1.0647(5) 0.00095(17) 0.0631(18) Uani 1 1 d . . . H17A H 0.2402 1.0071 -0.0140 0.095 Uiso 1 1 calc R . . H17B H 0.2220 1.1477 -0.0079 0.095 Uiso 1 1 calc R . . H17C H 0.1600 1.0464 -0.0022 0.095 Uiso 1 1 calc R . . C21 C 0.3019(3) 0.6989(4) 0.18963(14) 0.0351(12) Uani 1 1 d . . . C22 C 0.1769(3) 0.7107(5) 0.17711(15) 0.0441(13) Uani 1 1 d . . . H22A H 0.1274 0.7051 0.1641 0.053 Uiso 1 1 calc R . . C23 C 0.1947(3) 0.7482(6) 0.21356(16) 0.0536(15) Uani 1 1 d . . . H23A H 0.1605 0.7744 0.2305 0.064 Uiso 1 1 calc R . . C24 C 0.3179(4) 0.7824(7) 0.25950(17) 0.0616(17) Uani 1 1 d . . . C25 C 0.3616(5) 0.6751(7) 0.2791(2) 0.089(3) Uani 1 1 d . . . H25A H 0.3262 0.6108 0.2842 0.134 Uiso 1 1 calc R . . H25B H 0.3894 0.7026 0.3031 0.134 Uiso 1 1 calc R . . H25C H 0.3971 0.6434 0.2624 0.134 Uiso 1 1 calc R . . C26 C 0.2625(5) 0.8334(9) 0.2863(2) 0.111(3) Uani 1 1 d . . . H26A H 0.2283 0.7686 0.2925 0.167 Uiso 1 1 calc R . . H26B H 0.2333 0.9002 0.2736 0.167 Uiso 1 1 calc R . . H26C H 0.2910 0.8634 0.3098 0.167 Uiso 1 1 calc R . . C27 C 0.3708(5) 0.8888(7) 0.2506(2) 0.088(2) Uani 1 1 d . . . H27A H 0.3406 0.9556 0.2385 0.132 Uiso 1 1 calc R . . H27B H 0.4061 0.8600 0.2333 0.132 Uiso 1 1 calc R . . H27C H 0.3991 0.9177 0.2743 0.132 Uiso 1 1 calc R . . C31 C 0.3688(3) 0.5686(4) 0.09630(13) 0.0291(11) Uani 1 1 d . . . C32 C 0.2961(3) 0.4323(4) 0.12129(14) 0.0372(12) Uani 1 1 d . . . H32A H 0.2545 0.3966 0.1315 0.045 Uiso 1 1 calc R . . C33 C 0.3599(3) 0.3750(5) 0.11557(15) 0.0426(13) Uani 1 1 d . . . H33A H 0.3713 0.2920 0.1210 0.051 Uiso 1 1 calc R . . C34 C 0.4877(3) 0.4342(5) 0.09325(15) 0.0428(13) Uani 1 1 d . . . C35 C 0.5404(3) 0.5135(6) 0.12073(17) 0.0554(16) Uani 1 1 d . . . H35A H 0.5300 0.5996 0.1152 0.083 Uiso 1 1 calc R . . H35B H 0.5929 0.4955 0.1174 0.083 Uiso 1 1 calc R . . H35C H 0.5319 0.4958 0.1470 0.083 Uiso 1 1 calc R . . C36 C 0.5058(4) 0.2984(5) 0.10175(19) 0.0601(17) Uani 1 1 d . . . H36A H 0.4996 0.2806 0.1283 0.090 Uiso 1 1 calc R . . H36B H 0.5579 0.2815 0.0973 0.090 Uiso 1 1 calc R . . H36C H 0.4715 0.2472 0.0849 0.090 Uiso 1 1 calc R . . C37 C 0.4991(3) 0.4559(6) 0.05124(16) 0.0558(16) Uani 1 1 d . . . H37A H 0.4887 0.5413 0.0447 0.084 Uiso 1 1 calc R . . H37B H 0.4647 0.4037 0.0349 0.084 Uiso 1 1 calc R . . H37C H 0.5512 0.4365 0.0475 0.084 Uiso 1 1 calc R . . H1 H 0.181(3) 0.591(4) 0.1091(12) 0.036(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg 0.03776(13) 0.04294(12) 0.04222(14) -0.00130(10) 0.00189(9) -0.01084(10) Br 0.0635(4) 0.0836(5) 0.0561(4) 0.0135(3) -0.0085(3) -0.0429(4) B 0.030(3) 0.034(3) 0.032(3) 0.000(2) 0.004(2) -0.005(2) S1 0.0472(9) 0.0379(7) 0.0407(8) -0.0097(6) -0.0029(6) -0.0008(6) S2 0.0326(7) 0.0495(7) 0.0353(7) 0.0038(6) 0.0034(6) 0.0002(6) S3 0.0394(8) 0.0367(6) 0.0334(7) 0.0021(5) 0.0101(6) -0.0071(5) N11 0.027(2) 0.032(2) 0.027(2) -0.0021(16) 0.0012(17) -0.0031(17) N12 0.032(2) 0.036(2) 0.034(2) 0.0016(18) 0.0013(19) 0.0019(18) N21 0.032(2) 0.044(2) 0.027(2) 0.0011(18) 0.0049(18) 0.0013(19) N22 0.041(3) 0.061(3) 0.036(3) -0.008(2) 0.009(2) -0.004(2) N31 0.032(2) 0.033(2) 0.025(2) 0.0000(17) 0.0062(18) -0.0061(18) N32 0.032(2) 0.035(2) 0.037(2) -0.0030(18) 0.0046(19) 0.0016(18) C1S 0.073(7) 0.053(5) 0.080(8) 0.000 0.017(6) 0.000 C2S 0.087(6) 0.089(6) 0.070(5) 0.010(4) 0.016(4) 0.005(5) C3S 0.085(6) 0.081(6) 0.099(7) -0.034(5) 0.015(5) -0.009(5) C4S 0.090(10) 0.045(6) 0.178(15) 0.000 0.062(10) 0.000 C5S 0.049(4) 0.058(4) 0.050(4) 0.007(3) 0.010(3) -0.007(3) C6S 0.057(4) 0.047(3) 0.065(4) -0.009(3) 0.011(3) -0.017(3) C7S 0.050(4) 0.075(4) 0.044(4) -0.013(3) 0.008(3) -0.020(3) C11 0.029(3) 0.039(2) 0.037(3) -0.001(2) 0.007(2) 0.005(2) C12 0.031(3) 0.039(3) 0.035(3) -0.010(2) 0.003(2) -0.003(2) C13 0.035(3) 0.046(3) 0.035(3) -0.001(2) 0.001(2) 0.001(2) C14 0.043(3) 0.037(3) 0.046(3) 0.008(2) 0.007(3) -0.001(2) C15 0.053(4) 0.038(3) 0.079(5) 0.001(3) 0.014(3) 0.004(3) C16 0.043(4) 0.057(4) 0.073(4) 0.017(3) 0.009(3) -0.006(3) C17 0.080(5) 0.055(4) 0.052(4) 0.018(3) -0.006(3) 0.000(3) C21 0.040(3) 0.039(3) 0.027(3) 0.000(2) 0.009(2) -0.003(2) C22 0.035(3) 0.059(3) 0.038(3) -0.003(3) 0.004(3) 0.002(3) C23 0.043(4) 0.078(4) 0.043(4) -0.010(3) 0.018(3) -0.002(3) C24 0.060(4) 0.093(5) 0.031(3) -0.015(3) 0.004(3) 0.000(4) C25 0.091(6) 0.129(7) 0.044(4) 0.009(4) -0.004(4) 0.003(5) C26 0.085(6) 0.194(10) 0.057(5) -0.066(6) 0.019(4) 0.004(6) C27 0.090(6) 0.102(6) 0.070(5) -0.040(4) -0.003(4) -0.020(5) C31 0.034(3) 0.032(2) 0.022(2) -0.0046(19) 0.004(2) -0.004(2) C32 0.047(3) 0.032(2) 0.035(3) 0.004(2) 0.011(2) -0.008(2) C33 0.051(4) 0.031(2) 0.046(3) 0.007(2) 0.007(3) 0.004(2) C34 0.036(3) 0.052(3) 0.040(3) -0.004(3) 0.003(3) 0.006(3) C35 0.043(4) 0.073(4) 0.050(4) 0.000(3) 0.005(3) 0.005(3) C36 0.053(4) 0.061(4) 0.067(4) 0.001(3) 0.011(3) 0.023(3) C37 0.051(4) 0.071(4) 0.049(4) 0.004(3) 0.018(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg Br 2.5330(6) . ? Hg S2 2.5349(13) . ? Hg S1 2.5782(15) . ? Hg S3 2.6067(13) . ? B N11 1.557(6) . ? B N31 1.563(7) . ? B N21 1.568(7) . ? S1 C11 1.753(5) . ? S2 C21 1.733(5) . ? S3 C31 1.723(5) . ? N11 C11 1.349(6) . ? N11 C12 1.374(6) . ? N12 C11 1.366(6) . ? N12 C13 1.387(6) . ? N12 C14 1.513(6) . ? N21 C21 1.357(6) . ? N21 C22 1.372(6) . ? N22 C21 1.357(6) . ? N22 C23 1.400(7) . ? N22 C24 1.524(7) . ? N31 C31 1.353(6) . ? N31 C32 1.381(6) . ? N32 C31 1.370(6) . ? N32 C33 1.386(6) . ? N32 C34 1.504(6) . ? C1S C2S 1.348(9) . ? C1S C2S 1.348(9) 2_655 ? C2S C3S 1.363(10) . ? C3S C4S 1.388(10) . ? C4S C3S 1.388(10) 2_655 ? C5S C6S 1.371(8) . ? C5S C7S 1.384(8) 5_565 ? C6S C7S 1.382(8) . ? C7S C5S 1.384(8) 5_565 ? C12 C13 1.345(7) . ? C14 C15 1.520(7) . ? C14 C16 1.521(7) . ? C14 C17 1.530(8) . ? C22 C23 1.342(7) . ? C24 C25 1.519(9) . ? C24 C26 1.539(9) . ? C24 C27 1.545(10) . ? C32 C33 1.326(7) . ? C34 C37 1.527(7) . ? C34 C35 1.527(7) . ? C34 C36 1.534(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 Br Hg S2 121.91(3) . . ? Br Hg S1 118.46(4) . . ? S2 Hg S1 101.24(4) . . ? Br Hg S3 111.86(3) . . ? S2 Hg S3 98.28(4) . . ? S1 Hg S3 101.57(4) . . ? N11 B N31 111.9(4) . . ? N11 B N21 113.7(4) . . ? N31 B N21 112.7(4) . . ? C11 S1 Hg 95.63(17) . . ? C21 S2 Hg 97.49(17) . . ? C31 S3 Hg 97.17(15) . . ? C11 N11 C12 107.1(4) . . ? C11 N11 B 135.5(4) . . ? C12 N11 B 117.3(4) . . ? C11 N12 C13 108.2(4) . . ? C11 N12 C14 128.1(4) . . ? C13 N12 C14 123.5(4) . . ? C21 N21 C22 108.1(4) . . ? C21 N21 B 133.7(4) . . ? C22 N21 B 118.1(4) . . ? C21 N22 C23 107.8(4) . . ? C21 N22 C24 128.3(5) . . ? C23 N22 C24 123.7(5) . . ? C31 N31 C32 107.9(4) . . ? C31 N31 B 133.8(4) . . ? C32 N31 B 117.9(4) . . ? C31 N32 C33 107.6(4) . . ? C31 N32 C34 127.3(4) . . ? C33 N32 C34 124.8(4) . . ? C2S C1S C2S 122.3(10) . 2_655 ? C1S C2S C3S 119.5(8) . . ? C2S C3S C4S 119.9(8) . . ? C3S C4S C3S 118.9(10) . 2_655 ? C6S C5S C7S 119.7(6) . 5_565 ? C5S C6S C7S 120.0(5) . . ? C6S C7S C5S 120.3(5) . 5_565 ? N11 C11 N12 108.4(4) . . ? N11 C11 S1 125.6(4) . . ? N12 C11 S1 126.0(4) . . ? C13 C12 N11 110.0(4) . . ? C12 C13 N12 106.2(4) . . ? N12 C14 C15 109.7(4) . . ? N12 C14 C16 109.2(4) . . ? C15 C14 C16 113.3(5) . . ? N12 C14 C17 107.8(4) . . ? C15 C14 C17 108.2(5) . . ? C16 C14 C17 108.5(5) . . ? N22 C21 N21 108.1(4) . . ? N22 C21 S2 125.4(4) . . ? N21 C21 S2 126.4(4) . . ? C23 C22 N21 108.9(5) . . ? C22 C23 N22 107.0(5) . . ? C25 C24 N22 110.2(5) . . ? C25 C24 C26 109.2(6) . . ? N22 C24 C26 109.9(5) . . ? C25 C24 C27 112.3(6) . . ? N22 C24 C27 107.8(5) . . ? C26 C24 C27 107.4(6) . . ? N31 C31 N32 107.7(4) . . ? N31 C31 S3 126.1(4) . . ? N32 C31 S3 126.1(4) . . ? C33 C32 N31 108.8(5) . . ? C32 C33 N32 108.0(4) . . ? N32 C34 C37 111.4(4) . . ? N32 C34 C35 108.7(4) . . ? C37 C34 C35 112.2(5) . . ? N32 C34 C36 108.8(4) . . ? C37 C34 C36 106.7(5) . . ? C35 C34 C36 108.9(5) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.042 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.111 #===END