# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1829 data_cmt10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H13 N2 S' _chemical_formula_weight 217.30 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' '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 7.5661(5) _cell_length_b 20.7403(14) _cell_length_c 7.3572(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.0000(10) _cell_angle_gamma 90.00 _cell_volume 1154.52(13) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 0.249 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9292 _exptl_absorpt_correction_T_max 0.9756 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 8574 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.25 _reflns_number_total 2681 _reflns_number_gt 2327 _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^)+(0.0619P)^2^+0.4441P] 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 0.0000(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2681 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.083 _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 S S 0.34666(6) 0.59295(2) 0.55159(6) 0.04014(16) Uani 1 1 d . . . N1 N 0.19533(17) 0.58754(6) 0.21501(18) 0.0316(3) Uani 1 1 d . . . N2 N 0.36967(18) 0.50709(6) 0.26983(19) 0.0354(3) Uani 1 1 d . . . C11 C 0.30422(19) 0.56199(7) 0.3436(2) 0.0309(3) Uani 1 1 d . . . C12 C 0.3019(2) 0.49829(9) 0.0969(2) 0.0414(4) Uani 1 1 d . . . H12 H 0.3265 0.4637 0.0185 0.050 Uiso 1 1 calc R . . C13 C 0.1946(2) 0.54817(9) 0.0616(2) 0.0405(4) Uani 1 1 d . . . H13 H 0.1309 0.5553 -0.0462 0.049 Uiso 1 1 calc R . . C21 C 0.09197(19) 0.64541(7) 0.2369(2) 0.0301(3) Uani 1 1 d . . . C22 C -0.07702(19) 0.64008(8) 0.3117(2) 0.0317(3) Uani 1 1 d . . . C23 C -0.1748(2) 0.69648(8) 0.3306(2) 0.0339(3) Uani 1 1 d . . . H23 H -0.2896 0.6941 0.3790 0.041 Uiso 1 1 calc R . . C24 C -0.1081(2) 0.75618(8) 0.2801(2) 0.0348(3) Uani 1 1 d . . . C25 C 0.0605(2) 0.75913(8) 0.2048(2) 0.0362(4) Uani 1 1 d . . . H25 H 0.1061 0.7993 0.1691 0.043 Uiso 1 1 calc R . . C26 C 0.1633(2) 0.70415(8) 0.1811(2) 0.0336(3) Uani 1 1 d . . . C32 C -0.1482(2) 0.57592(9) 0.3730(3) 0.0438(4) Uani 1 1 d . . . H32A H -0.0838 0.5616 0.4796 0.066 Uiso 1 1 calc R . . H32B H -0.1341 0.5446 0.2762 0.066 Uiso 1 1 calc R . . H32C H -0.2725 0.5802 0.4026 0.066 Uiso 1 1 calc R . . C34 C -0.2143(3) 0.81699(9) 0.3114(3) 0.0483(4) Uani 1 1 d . . . H34A H -0.1541 0.8533 0.2558 0.072 Uiso 1 1 calc R . . H34B H -0.2263 0.8245 0.4410 0.072 Uiso 1 1 calc R . . H34C H -0.3305 0.8122 0.2575 0.072 Uiso 1 1 calc R . . C36 C 0.3450(2) 0.70796(10) 0.0978(3) 0.0473(4) Uani 1 1 d . . . H36A H 0.4313 0.6909 0.1826 0.071 Uiso 1 1 calc R . . H36B H 0.3731 0.7526 0.0707 0.071 Uiso 1 1 calc R . . H36C H 0.3476 0.6829 -0.0134 0.071 Uiso 1 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 S 0.0467(3) 0.0377(2) 0.0360(2) -0.00503(16) -0.00943(17) 0.01495(17) N1 0.0310(6) 0.0323(7) 0.0315(6) 0.0013(5) -0.0030(5) 0.0028(5) N2 0.0374(7) 0.0323(7) 0.0367(7) -0.0016(5) 0.0003(5) 0.0056(5) C11 0.0284(7) 0.0301(7) 0.0343(7) 0.0035(6) 0.0001(6) 0.0024(5) C12 0.0449(9) 0.0407(9) 0.0384(9) -0.0076(7) -0.0011(7) 0.0041(7) C13 0.0425(9) 0.0445(9) 0.0345(8) -0.0049(7) -0.0054(7) 0.0033(7) C21 0.0281(7) 0.0311(7) 0.0309(7) 0.0032(6) -0.0049(5) 0.0026(5) C22 0.0305(7) 0.0362(8) 0.0284(7) 0.0018(6) -0.0033(5) -0.0021(6) C23 0.0294(7) 0.0428(9) 0.0295(7) 0.0001(6) -0.0024(6) 0.0028(6) C24 0.0395(8) 0.0370(8) 0.0279(7) 0.0003(6) -0.0072(6) 0.0077(6) C25 0.0408(9) 0.0321(8) 0.0359(8) 0.0076(6) -0.0073(6) -0.0009(6) C26 0.0294(7) 0.0374(8) 0.0340(8) 0.0068(6) -0.0047(6) -0.0004(6) C32 0.0410(9) 0.0396(9) 0.0508(10) 0.0044(8) 0.0055(7) -0.0074(7) C34 0.0594(11) 0.0441(10) 0.0413(9) 0.0002(8) -0.0026(8) 0.0178(8) C36 0.0334(9) 0.0487(10) 0.0598(11) 0.0147(9) 0.0032(8) -0.0034(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S C11 1.6899(16) . ? N1 C11 1.3620(19) . ? N1 C13 1.393(2) . ? N1 C21 1.4415(18) . ? N2 C11 1.3553(19) . ? N2 C12 1.384(2) . ? C12 C13 1.340(2) . ? C21 C26 1.394(2) . ? C21 C22 1.396(2) . ? C22 C23 1.391(2) . ? C22 C32 1.505(2) . ? C23 C24 1.388(2) . ? C24 C25 1.391(2) . ? C24 C34 1.513(2) . ? C25 C26 1.391(2) . ? C26 C36 1.507(2) . ? 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 C11 N1 C13 109.71(13) . . ? C11 N1 C21 125.06(13) . . ? C13 N1 C21 125.20(13) . . ? C11 N2 C12 110.11(13) . . ? N2 C11 N1 105.63(13) . . ? N2 C11 S 127.77(12) . . ? N1 C11 S 126.60(12) . . ? C13 C12 N2 107.48(15) . . ? C12 C13 N1 107.06(15) . . ? C26 C21 C22 122.64(14) . . ? C26 C21 N1 119.00(13) . . ? C22 C21 N1 118.36(13) . . ? C23 C22 C21 117.39(14) . . ? C23 C22 C32 121.55(14) . . ? C21 C22 C32 121.04(14) . . ? C24 C23 C22 121.99(15) . . ? C23 C24 C25 118.64(14) . . ? C23 C24 C34 120.63(16) . . ? C25 C24 C34 120.70(16) . . ? C26 C25 C24 121.74(15) . . ? C25 C26 C21 117.58(14) . . ? C25 C26 C36 121.19(15) . . ? C21 C26 C36 121.23(14) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.702 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.049 data_new2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H46 B N5 O3 S2 Zn' _chemical_formula_weight 809.14 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 24.777(5) _cell_length_b 9.4508(16) _cell_length_c 18.736(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4387.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 223(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 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8733 _exptl_absorpt_correction_T_max 0.9660 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 22015 _diffrn_reflns_av_R_equivalents 0.1629 _diffrn_reflns_av_sigmaI/netI 0.2344 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9177 _reflns_number_gt 2970 _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^)+(0.0057P)^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 0.00008(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(2) _refine_ls_number_reflns 9177 _refine_ls_number_parameters 503 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2641 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.171 _refine_ls_shift/su_mean 0.021 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 0.27028(3) 0.99626(9) 0.90466(10) 0.0645(3) Uani 1 1 d . . . S11 S 0.30912(12) 0.9560(3) 1.01259(14) 0.0722(10) Uani 1 1 d . . . S21 S 0.30721(13) 0.9598(3) 0.79549(14) 0.0763(11) Uani 1 1 d . . . N1 N 0.2151(4) 1.2178(8) 0.8919(5) 0.068(3) Uani 1 1 d . . . N11 N 0.2913(3) 0.6861(10) 0.9615(4) 0.053(2) Uani 1 1 d . . . N12 N 0.3484(3) 0.7030(8) 1.0496(4) 0.061(2) Uani 1 1 d . . . N21 N 0.2752(3) 0.6875(9) 0.8271(4) 0.056(2) Uani 1 1 d . . . N22 N 0.3168(3) 0.7143(8) 0.7248(4) 0.058(2) Uani 1 1 d . . . O1 O 0.2647(3) 1.2312(5) 0.8996(5) 0.0765(18) Uani 1 1 d . . . O2 O 0.1958(2) 1.0945(5) 0.8988(5) 0.0811(16) Uani 1 1 d . . . O3 O 0.1839(3) 1.3191(6) 0.8815(3) 0.093(2) Uani 1 1 d . . . B B 0.2479(4) 0.7040(8) 0.9020(8) 0.052(3) Uani 1 1 d . . . H2 H 0.2088(15) 0.621(4) 0.915(3) 0.014(14) Uiso 1 1 d . . . H1 H 0.2336(19) 0.841(5) 0.911(4) 0.045(15) Uiso 1 1 d . . . C11 C 0.3149(4) 0.7736(10) 1.0066(5) 0.047(3) Uani 1 1 d . . . C12 C 0.3098(4) 0.5517(10) 0.9780(5) 0.072(3) Uani 1 1 d . . . H12A H 0.2991 0.4682 0.9548 0.086 Uiso 1 1 calc R . . C13 C 0.3453(4) 0.5582(9) 1.0322(5) 0.070(3) Uani 1 1 d . . . H13A H 0.3639 0.4828 1.0537 0.084 Uiso 1 1 calc R . . C21 C 0.2988(4) 0.7869(12) 0.7856(6) 0.062(3) Uani 1 1 d . . . C22 C 0.2778(4) 0.5584(9) 0.7911(5) 0.066(3) Uani 1 1 d . . . H22A H 0.2632 0.4726 0.8077 0.079 Uiso 1 1 calc R . . C23 C 0.3040(4) 0.5753(9) 0.7300(4) 0.065(3) Uani 1 1 d . . . H23A H 0.3122 0.5043 0.6966 0.078 Uiso 1 1 calc R . . C31 C 0.3797(4) 0.7577(9) 1.1082(6) 0.049(3) Uani 1 1 d . . . C32 C 0.4341(5) 0.7961(13) 1.0924(7) 0.074(4) Uani 1 1 d . . . C33 C 0.4649(4) 0.8424(10) 1.1512(7) 0.083(3) Uani 1 1 d . . . H33A H 0.5016 0.8638 1.1443 0.100 Uiso 1 1 calc R . . C34 C 0.4430(6) 0.8575(11) 1.2194(6) 0.079(4) Uani 1 1 d . . . C35 C 0.3898(5) 0.8157(11) 1.2291(6) 0.082(3) Uani 1 1 d . . . H35A H 0.3751 0.8198 1.2753 0.098 Uiso 1 1 calc R . . C36 C 0.3574(4) 0.7684(11) 1.1742(6) 0.062(3) Uani 1 1 d . . . C41 C 0.3414(6) 0.7817(11) 0.6634(5) 0.067(3) Uani 1 1 d . . . C42 C 0.3969(5) 0.8099(10) 0.6656(6) 0.063(3) Uani 1 1 d . . . C43 C 0.4172(4) 0.8767(11) 0.6064(6) 0.065(3) Uani 1 1 d . . . H43A H 0.4543 0.8969 0.6046 0.078 Uiso 1 1 calc R . . C44 C 0.3847(5) 0.9159(10) 0.5482(5) 0.071(3) Uani 1 1 d . . . C45 C 0.3312(4) 0.8858(9) 0.5507(5) 0.066(3) Uani 1 1 d . . . H45A H 0.3094 0.9109 0.5116 0.079 Uiso 1 1 calc R . . C46 C 0.3081(4) 0.8213(9) 0.6071(5) 0.051(2) Uani 1 1 d . . . C52 C 0.4579(4) 0.7802(10) 1.0178(5) 0.107(4) Uani 1 1 d . . . H52A H 0.4386 0.7066 0.9923 0.160 Uiso 1 1 calc R . . H52B H 0.4957 0.7548 1.0215 0.160 Uiso 1 1 calc R . . H52C H 0.4545 0.8690 0.9923 0.160 Uiso 1 1 calc R . . C54 C 0.4798(4) 0.9125(9) 1.2785(5) 0.104(4) Uani 1 1 d . . . H54A H 0.4617 0.9882 1.3040 0.157 Uiso 1 1 calc R . . H54B H 0.5130 0.9481 1.2577 0.157 Uiso 1 1 calc R . . H54C H 0.4880 0.8361 1.3113 0.157 Uiso 1 1 calc R . . C56 C 0.3006(4) 0.7286(11) 1.1889(5) 0.086(4) Uani 1 1 d . . . H56A H 0.2776 0.7650 1.1513 0.129 Uiso 1 1 calc R . . H56B H 0.2896 0.7685 1.2343 0.129 Uiso 1 1 calc R . . H56C H 0.2976 0.6264 1.1908 0.129 Uiso 1 1 calc R . . C62 C 0.4323(4) 0.7709(12) 0.7261(6) 0.079(4) Uani 1 1 d . . . H62A H 0.4304 0.6696 0.7340 0.119 Uiso 1 1 calc R . . H62B H 0.4205 0.8201 0.7688 0.119 Uiso 1 1 calc R . . H62C H 0.4692 0.7975 0.7152 0.119 Uiso 1 1 calc R . . C64 C 0.4105(3) 1.0013(12) 0.4855(4) 0.104(3) Uani 1 1 d . . . H64A H 0.3865 0.9989 0.4445 0.155 Uiso 1 1 calc R . . H64B H 0.4449 0.9594 0.4727 0.155 Uiso 1 1 calc R . . H64C H 0.4160 1.0986 0.5002 0.155 Uiso 1 1 calc R . . C66 C 0.2486(3) 0.7853(10) 0.6074(5) 0.077(3) Uani 1 1 d . . . H66A H 0.2289 0.8572 0.6337 0.116 Uiso 1 1 calc R . . H66B H 0.2433 0.6940 0.6299 0.116 Uiso 1 1 calc R . . H66C H 0.2354 0.7818 0.5587 0.116 Uiso 1 1 calc R . . C71 C 0.4016(9) 1.286(3) 0.894(2) 0.230(16) Uani 1 1 d . . . H71A H 0.3684 1.2422 0.8831 0.276 Uiso 1 1 calc R . . C72 C 0.4212(10) 1.398(4) 0.8683(13) 0.23(2) Uani 1 1 d . . . H72A H 0.3968 1.4415 0.8368 0.279 Uiso 1 1 calc R . . C73 C 0.4630(13) 1.466(2) 0.8732(10) 0.166(9) Uani 1 1 d . . . H73A H 0.4685 1.5477 0.8453 0.200 Uiso 1 1 calc R . . C74 C 0.4999(9) 1.423(3) 0.9186(16) 0.170(8) Uani 1 1 d . . . H74A H 0.5317 1.4762 0.9245 0.205 Uiso 1 1 calc R . . C75 C 0.4931(11) 1.309(3) 0.9552(9) 0.159(8) Uani 1 1 d . . . H75A H 0.5196 1.2753 0.9870 0.191 Uiso 1 1 calc R . . C76 C 0.4451(16) 1.2381(19) 0.9453(12) 0.172(10) Uani 1 1 d . . . H76A H 0.4389 1.1556 0.9721 0.207 Uiso 1 1 calc R . . C81 C 0.3744(9) 1.207(2) 1.2240(18) 0.203(15) Uani 1 1 d . . . H81A H 0.3575 1.1197 1.2330 0.243 Uiso 1 1 calc R . . C82 C 0.3704(8) 1.308(3) 1.2766(11) 0.174(9) Uani 1 1 d . . . H82A H 0.3501 1.2966 1.3186 0.208 Uiso 1 1 calc R . . C83 C 0.3979(7) 1.421(2) 1.2618(11) 0.129(6) Uani 1 1 d . . . H83A H 0.3970 1.4939 1.2957 0.155 Uiso 1 1 calc R . . C84 C 0.4271(6) 1.4426(17) 1.2036(12) 0.100(5) Uani 1 1 d . . . H84A H 0.4454 1.5278 1.1946 0.120 Uiso 1 1 calc R . . C85 C 0.4279(7) 1.334(3) 1.1597(13) 0.155(10) Uani 1 1 d . . . H85A H 0.4535 1.3436 1.1229 0.185 Uiso 1 1 calc R . . C86 C 0.4016(14) 1.221(4) 1.1568(14) 0.223(19) Uani 1 1 d . . . H86A H 0.3999 1.1580 1.1181 0.268 Uiso 1 1 calc R . . C91 C 0.1323(11) -0.074(2) 0.0530(10) 0.162(12) Uani 1 1 d . . . H91A H 0.1395 -0.0180 0.0124 0.194 Uiso 1 1 calc R . . C92 C 0.1621(9) -0.191(3) 0.0731(10) 0.158(10) Uani 1 1 d . . . H92A H 0.1914 -0.2155 0.0438 0.190 Uiso 1 1 calc R . . C93 C 0.1536(6) -0.2702(16) 0.1278(11) 0.109(7) Uani 1 1 d . . . H93A H 0.1739 -0.3526 0.1357 0.131 Uiso 1 1 calc R . . C94 C 0.1152(9) -0.2311(18) 0.1721(9) 0.109(6) Uani 1 1 d . . . H94A H 0.1122 -0.2785 0.2160 0.131 Uiso 1 1 calc R . . C95 C 0.0809(5) -0.129(2) 0.1579(10) 0.097(5) Uani 1 1 d . . . H95A H 0.0506 -0.1115 0.1868 0.116 Uiso 1 1 calc R . . C96 C 0.0917(7) -0.0492(18) 0.0991(12) 0.111(6) Uani 1 1 d . . . H96A H 0.0691 0.0286 0.0900 0.134 Uiso 1 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 Zn 0.0946(6) 0.0495(4) 0.0493(5) -0.0028(9) 0.0007(11) 0.0070(6) S11 0.110(3) 0.050(2) 0.057(2) -0.0066(17) -0.018(2) -0.004(2) S21 0.123(3) 0.047(2) 0.058(2) -0.0049(17) 0.017(2) -0.003(2) N1 0.125(8) 0.037(4) 0.041(6) -0.024(5) 0.009(6) 0.009(6) N11 0.069(6) 0.052(6) 0.039(5) 0.002(5) 0.000(4) -0.009(5) N12 0.081(6) 0.044(5) 0.059(6) 0.008(5) 0.014(5) 0.001(5) N21 0.079(6) 0.036(5) 0.053(6) -0.008(4) 0.003(5) -0.003(5) N22 0.079(6) 0.045(5) 0.051(6) -0.006(5) 0.003(5) -0.010(5) O1 0.104(5) 0.052(3) 0.073(4) 0.005(6) 0.006(6) -0.016(4) O2 0.117(4) 0.056(3) 0.071(4) 0.009(6) -0.010(6) -0.007(3) O3 0.164(7) 0.063(4) 0.054(5) -0.014(3) -0.009(4) 0.038(4) B 0.073(8) 0.043(5) 0.041(6) 0.024(9) 0.013(9) -0.008(5) C11 0.062(7) 0.032(6) 0.047(7) 0.017(5) 0.002(5) 0.012(5) C12 0.128(10) 0.045(7) 0.042(7) -0.001(5) -0.005(7) -0.005(6) C13 0.093(8) 0.054(7) 0.064(7) 0.001(5) -0.001(6) 0.012(6) C21 0.057(7) 0.079(9) 0.048(7) 0.012(7) 0.003(5) -0.018(6) C22 0.096(8) 0.047(6) 0.054(6) 0.000(5) -0.015(7) -0.006(6) C23 0.113(8) 0.049(6) 0.033(6) -0.007(4) 0.024(6) 0.010(5) C31 0.060(8) 0.039(6) 0.049(6) 0.004(5) -0.023(7) -0.011(5) C32 0.069(9) 0.079(9) 0.074(9) 0.018(7) 0.026(7) 0.026(7) C33 0.077(8) 0.074(7) 0.099(9) 0.014(7) -0.030(8) -0.026(6) C34 0.122(11) 0.061(7) 0.055(8) 0.010(6) -0.035(9) 0.019(7) C35 0.064(9) 0.103(9) 0.079(9) -0.027(7) 0.006(7) -0.012(7) C36 0.061(8) 0.080(8) 0.044(7) -0.014(6) 0.001(7) -0.019(6) C41 0.111(10) 0.060(7) 0.029(7) 0.002(5) 0.009(8) 0.000(7) C42 0.064(9) 0.053(7) 0.071(9) -0.006(6) 0.015(8) -0.003(6) C43 0.051(7) 0.080(8) 0.065(8) -0.016(7) 0.022(7) 0.002(6) C44 0.100(10) 0.073(7) 0.041(7) -0.010(5) 0.030(7) -0.005(7) C45 0.079(8) 0.062(6) 0.056(7) -0.004(5) 0.018(6) -0.008(6) C46 0.060(7) 0.057(6) 0.035(6) -0.004(5) 0.003(6) 0.001(6) C52 0.100(8) 0.121(9) 0.099(9) 0.002(7) 0.040(7) 0.008(7) C54 0.123(9) 0.104(8) 0.086(8) 0.010(6) -0.039(7) -0.040(7) C56 0.092(9) 0.115(10) 0.050(7) -0.010(7) 0.006(6) -0.019(7) C62 0.068(9) 0.062(8) 0.108(10) 0.006(8) -0.011(7) -0.007(6) C64 0.131(9) 0.103(7) 0.077(7) -0.009(7) 0.028(6) -0.004(8) C66 0.083(8) 0.097(8) 0.053(6) 0.004(6) -0.014(5) -0.002(6) C71 0.104(19) 0.27(3) 0.32(4) -0.17(3) 0.09(2) -0.021(17) C72 0.054(14) 0.46(6) 0.19(2) -0.13(3) -0.024(13) 0.01(2) C73 0.20(2) 0.22(2) 0.086(12) -0.001(12) -0.018(14) 0.05(2) C74 0.22(2) 0.125(16) 0.16(2) -0.070(16) -0.03(2) 0.024(15) C75 0.23(3) 0.115(15) 0.130(13) 0.000(13) -0.053(13) 0.060(17) C76 0.27(3) 0.094(13) 0.155(19) -0.020(12) 0.11(2) -0.024(18) C81 0.131(19) 0.073(12) 0.40(4) 0.02(2) -0.17(3) 0.001(12) C82 0.169(18) 0.147(18) 0.21(2) 0.057(19) 0.084(15) 0.015(16) C83 0.118(15) 0.119(16) 0.151(17) 0.015(12) 0.033(12) 0.033(11) C84 0.077(10) 0.085(12) 0.137(15) 0.008(11) 0.001(10) 0.007(8) C85 0.099(15) 0.21(3) 0.153(18) -0.075(18) -0.020(12) 0.078(15) C86 0.29(4) 0.21(3) 0.17(2) -0.11(2) -0.17(2) 0.16(3) C91 0.24(3) 0.18(2) 0.062(12) -0.006(13) 0.001(15) -0.15(2) C92 0.18(2) 0.24(3) 0.055(12) -0.026(13) 0.033(12) -0.091(19) C93 0.055(10) 0.110(13) 0.164(19) -0.092(14) 0.010(10) 0.001(8) C94 0.127(15) 0.082(11) 0.118(15) 0.023(10) -0.077(14) -0.059(10) C95 0.049(9) 0.129(15) 0.113(15) -0.033(11) 0.018(9) -0.016(10) C96 0.123(15) 0.088(12) 0.123(15) -0.013(12) -0.060(11) 0.023(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn H1 1.73(5) . ? Zn O2 2.068(5) . ? Zn O1 2.226(5) . ? Zn S21 2.267(3) . ? Zn S11 2.272(3) . ? Zn N1 2.513(8) . ? S11 C11 1.733(10) . ? S21 C21 1.658(12) . ? N1 O1 1.245(8) . ? N1 O3 1.245(8) . ? N1 O2 1.266(7) . ? N11 C11 1.318(11) . ? N11 C12 1.385(10) . ? N11 B 1.559(14) . ? N12 C11 1.335(10) . ? N12 C13 1.408(9) . ? N12 C31 1.442(10) . ? N21 C21 1.353(11) . ? N21 C22 1.396(10) . ? N21 B 1.565(15) . ? N22 C23 1.354(9) . ? N22 C21 1.402(11) . ? N22 C41 1.450(11) . ? B H2 1.27(4) . ? B H1 1.35(5) . ? C12 C13 1.344(10) . ? C22 C23 1.326(10) . ? C31 C36 1.358(12) . ? C31 C32 1.428(12) . ? C32 C33 1.410(14) . ? C32 C52 1.522(12) . ? C33 C34 1.394(13) . ? C34 C35 1.389(12) . ? C34 C54 1.525(13) . ? C35 C36 1.378(12) . ? C36 C56 1.482(12) . ? C41 C46 1.390(12) . ? C41 C42 1.401(13) . ? C42 C43 1.373(13) . ? C42 C62 1.480(13) . ? C43 C44 1.404(12) . ? C44 C45 1.358(11) . ? C44 C64 1.562(11) . ? C45 C46 1.348(10) . ? C46 C66 1.513(10) . ? C71 C72 1.26(4) . ? C71 C76 1.52(4) . ? C72 C73 1.22(2) . ? C73 C74 1.315(18) . ? C74 C75 1.29(2) . ? C75 C76 1.38(2) . ? C81 C82 1.38(2) . ? C81 C86 1.43(4) . ? C82 C83 1.291(19) . ? C83 C84 1.326(17) . ? C84 C85 1.31(2) . ? C85 C86 1.25(3) . ? C91 C96 1.35(2) . ? C91 C92 1.39(3) . ? C92 C93 1.285(18) . ? C93 C94 1.316(18) . ? C94 C95 1.314(16) . ? C95 C96 1.360(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H1 Zn O2 85.2(16) . . ? H1 Zn O1 144.7(16) . . ? O2 Zn O1 59.7(2) . . ? H1 Zn S21 98(3) . . ? O2 Zn S21 112.4(3) . . ? O1 Zn S21 97.9(3) . . ? H1 Zn S11 91(2) . . ? O2 Zn S11 120.0(3) . . ? O1 Zn S11 103.4(3) . . ? S21 Zn S11 127.35(8) . . ? H1 Zn N1 115.3(16) . . ? O2 Zn N1 30.1(2) . . ? O1 Zn N1 29.69(18) . . ? S21 Zn N1 105.1(2) . . ? S11 Zn N1 117.1(2) . . ? C11 S11 Zn 98.3(4) . . ? C21 S21 Zn 101.6(4) . . ? O1 N1 O3 123.6(8) . . ? O1 N1 O2 116.9(8) . . ? O3 N1 O2 119.4(9) . . ? O1 N1 Zn 62.3(4) . . ? O3 N1 Zn 173.3(7) . . ? O2 N1 Zn 55.1(4) . . ? C11 N11 C12 106.6(8) . . ? C11 N11 B 134.1(9) . . ? C12 N11 B 119.2(9) . . ? C11 N12 C13 108.2(9) . . ? C11 N12 C31 128.0(9) . . ? C13 N12 C31 123.6(9) . . ? C21 N21 C22 108.1(8) . . ? C21 N21 B 129.3(9) . . ? C22 N21 B 122.6(8) . . ? C23 N22 C21 110.0(8) . . ? C23 N22 C41 125.6(8) . . ? C21 N22 C41 124.3(8) . . ? N1 O1 Zn 88.0(5) . . ? N1 O2 Zn 94.8(5) . . ? H2 B H1 111(3) . . ? H2 B N11 109(2) . . ? H1 B N11 101(3) . . ? H2 B N21 116(3) . . ? H1 B N21 109(3) . . ? N11 B N21 109.4(7) . . ? N11 C11 N12 110.3(9) . . ? N11 C11 S11 129.0(9) . . ? N12 C11 S11 120.6(9) . . ? C13 C12 N11 110.1(8) . . ? C12 C13 N12 104.7(8) . . ? N21 C21 N22 105.3(9) . . ? N21 C21 S21 132.4(9) . . ? N22 C21 S21 122.3(8) . . ? C23 C22 N21 109.5(8) . . ? C22 C23 N22 107.1(8) . . ? C36 C31 C32 123.7(10) . . ? C36 C31 N12 120.1(10) . . ? C32 C31 N12 116.2(11) . . ? C33 C32 C31 115.3(10) . . ? C33 C32 C52 122.6(11) . . ? C31 C32 C52 122.0(12) . . ? C34 C33 C32 122.5(11) . . ? C35 C34 C33 117.4(11) . . ? C35 C34 C54 124.7(12) . . ? C33 C34 C54 117.9(12) . . ? C36 C35 C34 123.2(11) . . ? C31 C36 C35 117.8(11) . . ? C31 C36 C56 122.5(10) . . ? C35 C36 C56 119.7(10) . . ? C46 C41 C42 123.6(11) . . ? C46 C41 N22 118.1(11) . . ? C42 C41 N22 118.2(11) . . ? C43 C42 C41 115.0(11) . . ? C43 C42 C62 121.1(11) . . ? C41 C42 C62 123.9(11) . . ? C42 C43 C44 122.6(10) . . ? C45 C44 C43 118.6(10) . . ? C45 C44 C64 122.2(11) . . ? C43 C44 C64 119.1(11) . . ? C46 C45 C44 122.4(10) . . ? C45 C46 C41 117.7(10) . . ? C45 C46 C66 121.1(10) . . ? C41 C46 C66 121.0(10) . . ? C72 C71 C76 102(3) . . ? C73 C72 C71 138(4) . . ? C72 C73 C74 118(3) . . ? C75 C74 C73 121(2) . . ? C74 C75 C76 117(2) . . ? C75 C76 C71 124(2) . . ? C82 C81 C86 127(2) . . ? C83 C82 C81 112(2) . . ? C82 C83 C84 126(2) . . ? C85 C84 C83 113.7(19) . . ? C86 C85 C84 133(3) . . ? C85 C86 C81 107(2) . . ? C96 C91 C92 111(2) . . ? C93 C92 C91 127(2) . . ? C92 C93 C94 117.3(19) . . ? C95 C94 C93 123.1(16) . . ? C94 C95 C96 116.4(15) . . ? C91 C96 C95 124.9(18) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.405 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.057 data_newck10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H56 B2 Li2 N8 S4' _chemical_formula_weight 908.75 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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1350(12) _cell_length_b 16.526(3) _cell_length_c 20.404(3) _cell_angle_alpha 106.379(3) _cell_angle_beta 101.143(3) _cell_angle_gamma 97.605(2) _cell_volume 2530.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9347 _exptl_absorpt_correction_T_max 0.9775 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 13163 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.1595 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 28.26 _reflns_number_total 10289 _reflns_number_gt 4484 _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^)+(0.0400P)^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 0.0008(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10289 _refine_ls_number_parameters 606 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1870 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.037 _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 Li1 Li 0.9981(9) 0.9046(4) 0.4737(4) 0.0478(19) Uani 1 1 d . . . Li2 Li 0.0579(10) 0.4066(5) 0.0136(4) 0.059(2) Uani 1 1 d . . . B1 B 0.9669(6) 0.8561(3) 0.3282(3) 0.0370(12) Uani 1 1 d . . . B2 B 0.2856(7) 0.4398(3) 0.1620(3) 0.0439(13) Uani 1 1 d . . . S1 S 0.78244(14) 0.98423(7) 0.43822(5) 0.0418(3) Uani 1 1 d . . . S2 S 0.88839(14) 0.75728(7) 0.45014(5) 0.0440(3) Uani 1 1 d . . . S3 S -0.10225(15) 0.32516(8) 0.06842(6) 0.0519(4) Uani 1 1 d . . . S4 S 0.19882(14) 0.56157(8) 0.05848(6) 0.0444(3) Uani 1 1 d . . . N11 N 0.8874(4) 0.9330(2) 0.31502(17) 0.0364(8) Uani 1 1 d . . . N12 N 0.7442(4) 1.0369(2) 0.32192(17) 0.0398(9) Uani 1 1 d . . . N21 N 0.8149(4) 0.7825(2) 0.32005(17) 0.0355(8) Uani 1 1 d . . . N22 N 0.6225(4) 0.6885(2) 0.33525(17) 0.0368(8) Uani 1 1 d . . . N31 N 0.1836(4) 0.3640(2) 0.17784(17) 0.0390(9) Uani 1 1 d . . . N32 N -0.0126(4) 0.2569(2) 0.17343(17) 0.0401(9) Uani 1 1 d . . . N41 N 0.1896(4) 0.5174(2) 0.17815(16) 0.0380(9) Uani 1 1 d . . . N42 N 0.0445(4) 0.6171(2) 0.16545(17) 0.0372(8) Uani 1 1 d . . . C11 C 0.8089(5) 0.9849(3) 0.3573(2) 0.0346(10) Uani 1 1 d . . . C12 C 0.7865(6) 1.0177(3) 0.2574(2) 0.0514(12) Uani 1 1 d . . . H12J H 0.7589 1.0444 0.2229 0.062 Uiso 1 1 calc R . . C13 C 0.8735(6) 0.9544(3) 0.2536(2) 0.0487(12) Uani 1 1 d . . . H13J H 0.9182 0.9285 0.2155 0.058 Uiso 1 1 calc R . . C21 C 0.7749(5) 0.7448(2) 0.3674(2) 0.0364(10) Uani 1 1 d . . . C22 C 0.6873(5) 0.7484(3) 0.2581(2) 0.0462(12) Uani 1 1 d . . . H22A H 0.6842 0.7631 0.2167 0.055 Uiso 1 1 calc R . . C23 C 0.5693(6) 0.6910(3) 0.2675(2) 0.0475(12) Uani 1 1 d . . . H23A H 0.4688 0.6583 0.2342 0.057 Uiso 1 1 calc R . . C31 C 0.6468(5) 1.1003(3) 0.3469(2) 0.0390(11) Uani 1 1 d . . . C32 C 0.4760(5) 1.0746(3) 0.3455(2) 0.0472(12) Uani 1 1 d . . . C33 C 0.3861(5) 1.1378(3) 0.3702(2) 0.0503(12) Uani 1 1 d . . . H33A H 0.2708 1.1214 0.3700 0.060 Uiso 1 1 calc R . . C34 C 0.4616(5) 1.2245(3) 0.3950(2) 0.0386(10) Uani 1 1 d . . . C35 C 0.6315(5) 1.2475(3) 0.3945(2) 0.0405(11) Uani 1 1 d . . . H35A H 0.6836 1.3061 0.4109 0.049 Uiso 1 1 calc R . . C36 C 0.7274(5) 1.1864(3) 0.3706(2) 0.0380(10) Uani 1 1 d . . . C41 C 0.5202(5) 0.6436(3) 0.3694(2) 0.0356(10) Uani 1 1 d . . . C42 C 0.5474(5) 0.5635(3) 0.3724(2) 0.0390(11) Uani 1 1 d . . . C43 C 0.4359(5) 0.5189(3) 0.4004(2) 0.0444(11) Uani 1 1 d . . . H43A H 0.4514 0.4646 0.4034 0.053 Uiso 1 1 calc R . . C44 C 0.3025(6) 0.5530(3) 0.4240(2) 0.0454(11) Uani 1 1 d . . . C45 C 0.2833(5) 0.6334(3) 0.4210(2) 0.0459(11) Uani 1 1 d . . . H45A H 0.1940 0.6568 0.4374 0.055 Uiso 1 1 calc R . . C46 C 0.3916(5) 0.6814(3) 0.3946(2) 0.0423(11) Uani 1 1 d . . . C52 C 0.3884(6) 0.9810(3) 0.3191(3) 0.0744(16) Uani 1 1 d . . . H52A H 0.4289 0.9508 0.2791 0.112 Uiso 1 1 calc R . . H52B H 0.2658 0.9765 0.3048 0.112 Uiso 1 1 calc R . . H52C H 0.4142 0.9555 0.3563 0.112 Uiso 1 1 calc R . . C54 C 0.3634(5) 1.2921(3) 0.4229(2) 0.0487(12) Uani 1 1 d . . . H54A H 0.2885 1.3017 0.3839 0.073 Uiso 1 1 calc R . . H54B H 0.4428 1.3454 0.4510 0.073 Uiso 1 1 calc R . . H54C H 0.2957 1.2729 0.4520 0.073 Uiso 1 1 calc R . . C56 C 0.9113(5) 1.2144(3) 0.3725(2) 0.0548(13) Uani 1 1 d . . . H56A H 0.9780 1.1770 0.3898 0.082 Uiso 1 1 calc R . . H56B H 0.9524 1.2732 0.4035 0.082 Uiso 1 1 calc R . . H56C H 0.9226 1.2113 0.3254 0.082 Uiso 1 1 calc R . . C62 C 0.6918(5) 0.5265(3) 0.3471(2) 0.0535(13) Uani 1 1 d . . . H62A H 0.6792 0.5214 0.2978 0.080 Uiso 1 1 calc R . . H62B H 0.6894 0.4700 0.3528 0.080 Uiso 1 1 calc R . . H62C H 0.7999 0.5641 0.3744 0.080 Uiso 1 1 calc R . . C64 C 0.1787(6) 0.5015(3) 0.4521(3) 0.0707(15) Uani 1 1 d . . . H64A H 0.1038 0.5374 0.4717 0.106 Uiso 1 1 calc R . . H64B H 0.2429 0.4828 0.4885 0.106 Uiso 1 1 calc R . . H64C H 0.1109 0.4516 0.4140 0.106 Uiso 1 1 calc R . . C66 C 0.3710(6) 0.7709(3) 0.3942(3) 0.0631(14) Uani 1 1 d . . . H66A H 0.4822 0.8090 0.4105 0.095 Uiso 1 1 calc R . . H66B H 0.2984 0.7919 0.4250 0.095 Uiso 1 1 calc R . . H66C H 0.3192 0.7691 0.3466 0.095 Uiso 1 1 calc R . . C81 C 0.0271(5) 0.3166(3) 0.1410(2) 0.0397(11) Uani 1 1 d . . . C82 C 0.2399(6) 0.3330(3) 0.2325(2) 0.0476(12) Uani 1 1 d . . . H82A H 0.3447 0.3550 0.2663 0.057 Uiso 1 1 calc R . . C83 C 0.1214(5) 0.2666(3) 0.2299(2) 0.0458(12) Uani 1 1 d . . . H83A H 0.1284 0.2333 0.2605 0.055 Uiso 1 1 calc R . . C91 C 0.1426(5) 0.5635(3) 0.1352(2) 0.0343(10) Uani 1 1 d . . . C92 C 0.1213(6) 0.5434(3) 0.2359(2) 0.0468(12) Uani 1 1 d . . . H92A H 0.1356 0.5217 0.2741 0.056 Uiso 1 1 calc R . . C93 C 0.0319(6) 0.6041(3) 0.2290(2) 0.0474(12) Uani 1 1 d . . . H93A H -0.0276 0.6324 0.2608 0.057 Uiso 1 1 calc R . . C101 C -0.1708(5) 0.1959(3) 0.1535(2) 0.0380(10) Uani 1 1 d . . . C102 C -0.1832(6) 0.1152(3) 0.1074(2) 0.0461(12) Uani 1 1 d . . . C103 C -0.3356(7) 0.0551(3) 0.0922(2) 0.0559(13) Uani 1 1 d . . . H10A H -0.3472 -0.0001 0.0603 0.067 Uiso 1 1 calc R . . C104 C -0.4682(6) 0.0745(3) 0.1225(3) 0.0531(13) Uani 1 1 d . . . C105 C -0.4512(6) 0.1565(4) 0.1670(3) 0.0593(14) Uani 1 1 d . . . H10B H -0.5416 0.1710 0.1876 0.071 Uiso 1 1 calc R . . C106 C -0.3027(6) 0.2190(3) 0.1826(2) 0.0474(12) Uani 1 1 d . . . C111 C -0.0605(5) 0.6619(3) 0.1282(2) 0.0401(11) Uani 1 1 d . . . C112 C -0.2315(5) 0.6246(3) 0.0979(2) 0.0406(11) Uani 1 1 d . . . C113 C -0.3297(6) 0.6664(3) 0.0592(2) 0.0494(12) Uani 1 1 d . . . H11A H -0.4457 0.6420 0.0381 0.059 Uiso 1 1 calc R . . C114 C -0.2590(6) 0.7438(3) 0.0513(2) 0.0554(13) Uani 1 1 d . . . C115 C -0.0905(6) 0.7788(3) 0.0830(2) 0.0529(12) Uani 1 1 d . . . H11B H -0.0433 0.8312 0.0780 0.063 Uiso 1 1 calc R . . C116 C 0.0148(6) 0.7404(3) 0.1227(2) 0.0441(11) Uani 1 1 d . . . C122 C -0.0403(7) 0.0920(3) 0.0735(3) 0.0864(18) Uani 1 1 d . . . H12A H -0.0238 0.1266 0.0431 0.130 Uiso 1 1 calc R . . H12B H -0.0689 0.0315 0.0458 0.130 Uiso 1 1 calc R . . H12C H 0.0641 0.1029 0.1097 0.130 Uiso 1 1 calc R . . C124 C -0.6246(6) 0.0066(3) 0.1101(3) 0.0905(19) Uani 1 1 d . . . H12D H -0.6558 0.0110 0.1544 0.136 Uiso 1 1 calc R . . H12E H -0.5999 -0.0500 0.0910 0.136 Uiso 1 1 calc R . . H12F H -0.7185 0.0151 0.0771 0.136 Uiso 1 1 calc R . . C126 C -0.2899(6) 0.3092(3) 0.2311(3) 0.0729(16) Uani 1 1 d . . . H12G H -0.1728 0.3323 0.2583 0.109 Uiso 1 1 calc R . . H12H H -0.3643 0.3074 0.2627 0.109 Uiso 1 1 calc R . . H12I H -0.3244 0.3457 0.2033 0.109 Uiso 1 1 calc R . . C132 C -0.3113(5) 0.5407(3) 0.1055(2) 0.0495(12) Uani 1 1 d . . . H13A H -0.2395 0.4988 0.0945 0.074 Uiso 1 1 calc R . . H13B H -0.4236 0.5192 0.0735 0.074 Uiso 1 1 calc R . . H13C H -0.3219 0.5502 0.1535 0.074 Uiso 1 1 calc R . . C134 C -0.3678(7) 0.7848(4) 0.0051(3) 0.098(2) Uani 1 1 d . . . H13D H -0.4411 0.7401 -0.0358 0.147 Uiso 1 1 calc R . . H13E H -0.2939 0.8232 -0.0100 0.147 Uiso 1 1 calc R . . H13F H -0.4377 0.8171 0.0318 0.147 Uiso 1 1 calc R . . C136 C 0.2009(6) 0.7801(3) 0.1545(2) 0.0587(13) Uani 1 1 d . . . H13G H 0.2320 0.7779 0.2022 0.088 Uiso 1 1 calc R . . H13H H 0.2212 0.8396 0.1552 0.088 Uiso 1 1 calc R . . H13I H 0.2695 0.7485 0.1266 0.088 Uiso 1 1 calc R . . H1B H 1.057(4) 0.878(2) 0.3873(16) 0.031(9) Uiso 1 1 d . . . H2A H 0.425(4) 0.4539(19) 0.1967(15) 0.024(9) Uiso 1 1 d . . . H2B H 0.289(4) 0.417(2) 0.1060(17) 0.026(9) Uiso 1 1 d . . . H1A H 1.040(4) 0.8367(19) 0.2840(16) 0.028(9) 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 Li1 0.055(5) 0.035(5) 0.044(4) 0.006(4) 0.004(4) 0.005(4) Li2 0.064(5) 0.053(5) 0.054(5) 0.011(4) 0.016(4) 0.002(4) B1 0.039(3) 0.034(3) 0.036(3) 0.008(2) 0.012(2) 0.005(2) B2 0.038(3) 0.044(4) 0.049(4) 0.012(3) 0.010(3) 0.010(3) S1 0.0463(7) 0.0433(7) 0.0356(6) 0.0137(6) 0.0089(5) 0.0067(6) S2 0.0450(7) 0.0412(7) 0.0414(7) 0.0159(6) 0.0025(5) -0.0004(5) S3 0.0494(8) 0.0575(9) 0.0458(7) 0.0254(6) -0.0004(6) -0.0023(6) S4 0.0440(7) 0.0508(8) 0.0418(7) 0.0177(6) 0.0161(5) 0.0051(6) N11 0.047(2) 0.031(2) 0.033(2) 0.0102(17) 0.0140(17) 0.0057(17) N12 0.048(2) 0.036(2) 0.038(2) 0.0148(18) 0.0070(18) 0.0149(18) N21 0.037(2) 0.030(2) 0.037(2) 0.0090(17) 0.0096(17) 0.0020(16) N22 0.037(2) 0.035(2) 0.034(2) 0.0089(17) 0.0056(17) 0.0003(17) N31 0.038(2) 0.039(2) 0.038(2) 0.0127(18) 0.0053(17) 0.0044(18) N32 0.043(2) 0.039(2) 0.040(2) 0.0151(18) 0.0100(18) 0.0051(18) N41 0.040(2) 0.042(2) 0.027(2) 0.0087(18) 0.0061(16) 0.0010(17) N42 0.042(2) 0.036(2) 0.031(2) 0.0076(17) 0.0107(17) 0.0011(17) C11 0.039(3) 0.032(3) 0.029(2) 0.008(2) 0.004(2) 0.002(2) C12 0.065(3) 0.057(3) 0.038(3) 0.021(3) 0.014(2) 0.017(3) C13 0.063(3) 0.052(3) 0.039(3) 0.016(2) 0.024(2) 0.018(3) C21 0.037(3) 0.026(2) 0.048(3) 0.011(2) 0.011(2) 0.009(2) C22 0.050(3) 0.045(3) 0.035(3) 0.009(2) 0.002(2) 0.003(2) C23 0.047(3) 0.041(3) 0.043(3) 0.007(2) 0.003(2) -0.003(2) C31 0.040(3) 0.037(3) 0.041(3) 0.017(2) 0.005(2) 0.007(2) C32 0.038(3) 0.035(3) 0.061(3) 0.016(2) 0.001(2) -0.005(2) C33 0.032(3) 0.043(3) 0.078(3) 0.023(3) 0.013(2) 0.004(2) C34 0.043(3) 0.037(3) 0.040(3) 0.016(2) 0.010(2) 0.013(2) C35 0.049(3) 0.031(3) 0.042(3) 0.011(2) 0.015(2) 0.003(2) C36 0.039(3) 0.042(3) 0.036(2) 0.020(2) 0.006(2) 0.004(2) C41 0.031(2) 0.029(3) 0.042(3) 0.010(2) 0.006(2) 0.000(2) C42 0.039(3) 0.033(3) 0.039(3) 0.002(2) 0.008(2) 0.008(2) C43 0.049(3) 0.029(3) 0.052(3) 0.013(2) 0.009(2) 0.000(2) C44 0.045(3) 0.043(3) 0.046(3) 0.014(2) 0.011(2) 0.001(2) C45 0.040(3) 0.052(3) 0.044(3) 0.011(2) 0.010(2) 0.012(2) C46 0.035(3) 0.041(3) 0.044(3) 0.010(2) 0.004(2) 0.004(2) C52 0.048(3) 0.043(3) 0.113(4) 0.015(3) -0.001(3) -0.006(3) C54 0.051(3) 0.047(3) 0.051(3) 0.020(2) 0.014(2) 0.007(2) C56 0.046(3) 0.058(3) 0.061(3) 0.023(3) 0.013(2) 0.001(2) C62 0.055(3) 0.036(3) 0.067(3) 0.010(2) 0.017(3) 0.012(2) C64 0.063(3) 0.076(4) 0.081(4) 0.037(3) 0.029(3) 0.001(3) C66 0.063(3) 0.048(3) 0.090(4) 0.027(3) 0.030(3) 0.024(3) C81 0.044(3) 0.042(3) 0.038(3) 0.016(2) 0.012(2) 0.012(2) C82 0.042(3) 0.055(3) 0.042(3) 0.019(2) -0.003(2) 0.005(2) C83 0.048(3) 0.053(3) 0.042(3) 0.025(2) 0.009(2) 0.011(2) C91 0.034(2) 0.034(3) 0.028(2) 0.004(2) 0.0064(19) -0.002(2) C92 0.058(3) 0.051(3) 0.030(3) 0.010(2) 0.015(2) 0.009(3) C93 0.060(3) 0.047(3) 0.033(3) 0.005(2) 0.020(2) 0.007(3) C101 0.046(3) 0.034(3) 0.040(3) 0.017(2) 0.014(2) 0.010(2) C102 0.050(3) 0.046(3) 0.043(3) 0.015(2) 0.012(2) 0.009(3) C103 0.069(4) 0.044(3) 0.047(3) 0.011(2) 0.003(3) 0.009(3) C104 0.055(3) 0.051(4) 0.053(3) 0.030(3) -0.001(3) 0.000(3) C105 0.042(3) 0.072(4) 0.083(4) 0.046(3) 0.023(3) 0.017(3) C106 0.053(3) 0.041(3) 0.056(3) 0.020(2) 0.018(3) 0.017(3) C111 0.044(3) 0.040(3) 0.033(2) 0.004(2) 0.011(2) 0.008(2) C112 0.043(3) 0.038(3) 0.039(3) 0.003(2) 0.018(2) 0.010(2) C113 0.044(3) 0.047(3) 0.049(3) 0.006(3) 0.008(2) 0.009(2) C114 0.062(3) 0.048(3) 0.057(3) 0.015(3) 0.013(3) 0.018(3) C115 0.073(4) 0.035(3) 0.049(3) 0.012(2) 0.017(3) 0.005(3) C116 0.049(3) 0.041(3) 0.036(3) 0.005(2) 0.011(2) 0.002(2) C122 0.084(4) 0.077(4) 0.086(4) -0.006(3) 0.037(3) 0.020(3) C124 0.066(4) 0.086(5) 0.111(5) 0.052(4) -0.002(3) -0.022(3) C126 0.078(4) 0.054(4) 0.099(4) 0.020(3) 0.046(3) 0.026(3) C132 0.049(3) 0.048(3) 0.046(3) 0.010(2) 0.013(2) -0.003(2) C134 0.096(5) 0.079(5) 0.130(5) 0.057(4) 0.005(4) 0.029(4) C136 0.059(3) 0.046(3) 0.064(3) 0.015(3) 0.014(3) -0.006(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 Li1 H1B 1.86(3) . ? Li1 S2 2.356(7) . ? Li1 S1 2.413(7) 2_776 ? Li1 S1 2.448(7) . ? Li1 B1 2.798(9) . ? Li1 Li1 3.026(14) 2_776 ? Li2 H2B 2.34(3) . ? Li2 S3 2.389(8) . ? Li2 S4 2.491(8) . ? Li2 S4 2.518(8) 2_565 ? Li2 Li2 3.501(16) 2_565 ? B1 H1A 1.17(3) . ? B1 H1B 1.21(3) . ? B1 N21 1.563(5) . ? B1 N11 1.565(6) . ? B2 H2B 1.11(3) . ? B2 H2A 1.17(3) . ? B2 N31 1.555(6) . ? B2 N41 1.577(6) . ? S1 C11 1.708(4) . ? S1 Li1 2.413(7) 2_776 ? S2 C21 1.702(4) . ? S3 C81 1.696(4) . ? S4 C91 1.707(4) . ? S4 Li2 2.518(8) 2_565 ? N11 C11 1.353(4) . ? N11 C13 1.383(5) . ? N12 C11 1.364(5) . ? N12 C12 1.385(5) . ? N12 C31 1.435(5) . ? N21 C21 1.354(5) . ? N21 C22 1.389(5) . ? N22 C21 1.368(5) . ? N22 C23 1.380(5) . ? N22 C41 1.442(5) . ? N31 C81 1.354(5) . ? N31 C82 1.379(5) . ? N32 C81 1.371(5) . ? N32 C83 1.380(5) . ? N32 C101 1.436(5) . ? N41 C91 1.348(5) . ? N41 C92 1.383(5) . ? N42 C91 1.368(5) . ? N42 C93 1.393(5) . ? N42 C111 1.446(5) . ? C12 C13 1.332(5) . ? C22 C23 1.339(5) . ? C31 C36 1.390(5) . ? C31 C32 1.391(5) . ? C32 C33 1.389(6) . ? C32 C52 1.510(6) . ? C33 C34 1.387(5) . ? C34 C35 1.386(5) . ? C34 C54 1.505(5) . ? C35 C36 1.394(5) . ? C36 C56 1.495(5) . ? C41 C42 1.387(5) . ? C41 C46 1.396(5) . ? C42 C43 1.397(5) . ? C42 C62 1.507(5) . ? C43 C44 1.392(5) . ? C44 C45 1.376(6) . ? C44 C64 1.530(6) . ? C45 C46 1.390(5) . ? C46 C66 1.512(6) . ? C82 C83 1.343(5) . ? C92 C93 1.337(5) . ? C101 C106 1.370(5) . ? C101 C102 1.376(5) . ? C102 C103 1.404(6) . ? C102 C122 1.502(6) . ? C103 C104 1.374(6) . ? C104 C105 1.374(6) . ? C104 C124 1.510(6) . ? C105 C106 1.402(6) . ? C106 C126 1.517(6) . ? C111 C112 1.387(5) . ? C111 C116 1.403(5) . ? C112 C113 1.395(5) . ? C112 C132 1.514(5) . ? C113 C114 1.397(6) . ? C114 C115 1.367(6) . ? C114 C134 1.525(6) . ? C115 C116 1.400(6) . ? C116 C136 1.503(5) . ? 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 H1B Li1 S2 89.0(10) . . ? H1B Li1 S1 110.3(10) . 2_776 ? S2 Li1 S1 137.3(3) . 2_776 ? H1B Li1 S1 93.9(10) . . ? S2 Li1 S1 113.6(3) . . ? S1 Li1 S1 103.0(3) 2_776 . ? H1B Li1 B1 19.4(10) . . ? S2 Li1 B1 83.5(2) . . ? S1 Li1 B1 125.8(3) 2_776 . ? S1 Li1 B1 79.1(2) . . ? H1B Li1 Li1 109.3(10) . 2_776 ? S2 Li1 Li1 155.5(5) . 2_776 ? S1 Li1 Li1 52.0(2) 2_776 2_776 ? S1 Li1 Li1 51.0(2) . 2_776 ? B1 Li1 Li1 108.3(4) . 2_776 ? H2B Li2 S3 84.5(8) . . ? H2B Li2 S4 75.2(8) . . ? S3 Li2 S4 129.0(3) . . ? H2B Li2 S4 162.0(8) . 2_565 ? S3 Li2 S4 95.3(3) . 2_565 ? S4 Li2 S4 91.3(3) . 2_565 ? H2B Li2 Li2 120.2(8) . 2_565 ? S3 Li2 Li2 121.0(4) . 2_565 ? S4 Li2 Li2 45.97(19) . 2_565 ? S4 Li2 Li2 45.34(19) 2_565 2_565 ? H1A B1 H1B 114(2) . . ? H1A B1 N21 111.5(15) . . ? H1B B1 N21 109.2(15) . . ? H1A B1 N11 104.5(15) . . ? H1B B1 N11 110.4(15) . . ? N21 B1 N11 107.0(3) . . ? H1A B1 Li1 144.6(15) . . ? H1B B1 Li1 30.8(14) . . ? N21 B1 Li1 87.9(3) . . ? N11 B1 Li1 97.1(3) . . ? H2B B2 H2A 109(2) . . ? H2B B2 N31 107.0(17) . . ? H2A B2 N31 106.6(15) . . ? H2B B2 N41 112.1(16) . . ? H2A B2 N41 114.4(15) . . ? N31 B2 N41 107.6(4) . . ? C11 S1 Li1 108.0(2) . 2_776 ? C11 S1 Li1 102.2(2) . . ? Li1 S1 Li1 77.0(3) 2_776 . ? C21 S2 Li1 93.6(2) . . ? C81 S3 Li2 110.1(2) . . ? C91 S4 Li2 86.5(2) . . ? C91 S4 Li2 103.5(2) . 2_565 ? Li2 S4 Li2 88.7(3) . 2_565 ? C11 N11 C13 108.1(3) . . ? C11 N11 B1 127.3(3) . . ? C13 N11 B1 124.4(3) . . ? C11 N12 C12 108.7(4) . . ? C11 N12 C31 125.7(3) . . ? C12 N12 C31 125.6(3) . . ? C21 N21 C22 108.5(3) . . ? C21 N21 B1 130.2(3) . . ? C22 N21 B1 121.2(3) . . ? C21 N22 C23 109.1(3) . . ? C21 N22 C41 125.6(3) . . ? C23 N22 C41 124.7(3) . . ? C81 N31 C82 108.1(3) . . ? C81 N31 B2 126.9(4) . . ? C82 N31 B2 125.0(4) . . ? C81 N32 C83 109.2(3) . . ? C81 N32 C101 125.5(3) . . ? C83 N32 C101 125.2(3) . . ? C91 N41 C92 107.7(3) . . ? C91 N41 B2 126.7(4) . . ? C92 N41 B2 125.2(4) . . ? C91 N42 C93 108.6(3) . . ? C91 N42 C111 123.5(3) . . ? C93 N42 C111 126.2(4) . . ? N11 C11 N12 107.2(3) . . ? N11 C11 S1 127.9(3) . . ? N12 C11 S1 124.8(3) . . ? C13 C12 N12 107.2(4) . . ? C12 C13 N11 108.8(4) . . ? N21 C21 N22 106.8(3) . . ? N21 C21 S2 129.4(3) . . ? N22 C21 S2 123.7(3) . . ? C23 C22 N21 108.3(4) . . ? C22 C23 N22 107.3(4) . . ? C36 C31 C32 122.2(4) . . ? C36 C31 N12 118.0(4) . . ? C32 C31 N12 119.7(4) . . ? C33 C32 C31 118.0(4) . . ? C33 C32 C52 119.9(4) . . ? C31 C32 C52 122.0(4) . . ? C34 C33 C32 121.8(4) . . ? C35 C34 C33 118.3(4) . . ? C35 C34 C54 120.5(4) . . ? C33 C34 C54 121.2(4) . . ? C34 C35 C36 122.1(4) . . ? C31 C36 C35 117.5(4) . . ? C31 C36 C56 122.4(4) . . ? C35 C36 C56 120.1(4) . . ? C42 C41 C46 123.0(4) . . ? C42 C41 N22 119.0(4) . . ? C46 C41 N22 117.8(4) . . ? C41 C42 C43 117.2(4) . . ? C41 C42 C62 121.4(4) . . ? C43 C42 C62 121.4(4) . . ? C44 C43 C42 121.6(4) . . ? C45 C44 C43 118.8(4) . . ? C45 C44 C64 120.7(4) . . ? C43 C44 C64 120.5(4) . . ? C44 C45 C46 122.2(4) . . ? C45 C46 C41 117.1(4) . . ? C45 C46 C66 121.1(4) . . ? C41 C46 C66 121.9(4) . . ? N31 C81 N32 106.9(3) . . ? N31 C81 S3 128.9(3) . . ? N32 C81 S3 124.2(3) . . ? C83 C82 N31 109.3(4) . . ? C82 C83 N32 106.5(4) . . ? N41 C91 N42 107.7(3) . . ? N41 C91 S4 127.9(3) . . ? N42 C91 S4 124.3(3) . . ? C93 C92 N41 109.6(4) . . ? C92 C93 N42 106.3(4) . . ? C106 C101 C102 122.2(4) . . ? C106 C101 N32 118.9(4) . . ? C102 C101 N32 118.9(4) . . ? C101 C102 C103 117.7(4) . . ? C101 C102 C122 121.5(4) . . ? C103 C102 C122 120.7(4) . . ? C104 C103 C102 122.0(5) . . ? C105 C104 C103 118.1(4) . . ? C105 C104 C124 120.8(5) . . ? C103 C104 C124 121.0(5) . . ? C104 C105 C106 121.8(4) . . ? C101 C106 C105 118.2(4) . . ? C101 C106 C126 121.6(4) . . ? C105 C106 C126 120.2(4) . . ? C112 C111 C116 122.5(4) . . ? C112 C111 N42 118.5(4) . . ? C116 C111 N42 119.0(4) . . ? C111 C112 C113 118.1(4) . . ? C111 C112 C132 121.7(4) . . ? C113 C112 C132 120.2(4) . . ? C112 C113 C114 121.3(4) . . ? C115 C114 C113 118.5(4) . . ? C115 C114 C134 121.7(5) . . ? C113 C114 C134 119.7(5) . . ? C114 C115 C116 123.0(4) . . ? C115 C116 C111 116.6(4) . . ? C115 C116 C136 120.9(4) . . ? C111 C116 C136 122.5(4) . . ? _diffrn_measured_fraction_theta_max 0.821 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.821 _refine_diff_density_max 0.318 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.057 data_sss10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 B2 N8 S4 Zn' _chemical_formula_weight 543.66 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3268(13) _cell_length_b 14.3927(19) _cell_length_c 18.520(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.811(2) _cell_angle_gamma 90.00 _cell_volume 2480.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 228(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 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.348 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7743 _exptl_absorpt_correction_T_max 0.8770 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 228(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 15634 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.15 _reflns_number_total 5607 _reflns_number_gt 3367 _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^)+(0.0487P)^2^+0.1145P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5607 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.315 _refine_ls_shift/su_mean 0.007 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 0.13518(4) 0.25026(3) 0.012870(19) 0.03377(12) Uani 1 1 d . . . S1 S 0.27501(10) 0.38349(6) 0.03332(5) 0.0481(3) Uani 1 1 d . . . S2 S -0.03381(8) 0.22041(6) 0.09812(5) 0.0408(2) Uani 1 1 d . . . S3 S 0.26562(9) 0.11210(6) 0.01889(5) 0.0453(2) Uani 1 1 d . . . S4 S 0.01368(9) 0.28107(7) -0.09908(5) 0.0463(2) Uani 1 1 d . . . N11 N 0.3810(3) 0.32497(16) 0.16904(13) 0.0312(6) Uani 1 1 d . . . N12 N 0.5447(3) 0.34844(18) 0.09200(14) 0.0403(7) Uani 1 1 d . . . N21 N 0.1899(3) 0.21025(18) 0.20411(13) 0.0348(6) Uani 1 1 d . . . N22 N 0.0906(3) 0.07629(18) 0.17450(14) 0.0383(6) Uani 1 1 d . . . N31 N 0.4395(3) 0.16334(18) -0.09048(15) 0.0420(7) Uani 1 1 d . . . N32 N 0.5545(3) 0.12325(18) 0.01210(15) 0.0429(7) Uani 1 1 d . . . N41 N 0.2799(3) 0.2854(2) -0.15792(15) 0.0444(7) Uani 1 1 d . . . N42 N 0.1695(3) 0.4200(2) -0.15665(16) 0.0539(8) Uani 1 1 d . . . C11 C 0.4026(3) 0.3496(2) 0.10036(16) 0.0337(7) Uani 1 1 d . . . C12 C 0.5151(3) 0.3091(2) 0.20374(17) 0.0377(8) Uani 1 1 d . . . H12A H 0.5325 0.2913 0.2524 0.045 Uiso 1 1 calc R . . C13 C 0.6157(4) 0.3231(2) 0.15682(19) 0.0444(8) Uani 1 1 d . . . H13A H 0.7155 0.3169 0.1661 0.053 Uiso 1 1 calc R . . C14 C 0.6145(4) 0.3728(3) 0.0257(2) 0.0582(11) Uani 1 1 d . . . H14A H 0.5556 0.3516 -0.0162 0.087 Uiso 1 1 calc R . . H14B H 0.7081 0.3433 0.0264 0.087 Uiso 1 1 calc R . . H14C H 0.6260 0.4397 0.0232 0.087 Uiso 1 1 calc R . . C21 C 0.0862(3) 0.1692(2) 0.16085(15) 0.0312(7) Uani 1 1 d . . . C22 C 0.2572(4) 0.1418(2) 0.24587(19) 0.0475(9) Uani 1 1 d . . . H22A H 0.3332 0.1511 0.2811 0.057 Uiso 1 1 calc R . . C23 C 0.1965(4) 0.0593(2) 0.22806(19) 0.0525(10) Uani 1 1 d . . . H23A H 0.2217 0.0012 0.2484 0.063 Uiso 1 1 calc R . . C24 C 0.0035(4) 0.0056(3) 0.1374(2) 0.0610(11) Uani 1 1 d . . . H24A H 0.0392 -0.0553 0.1519 0.091 Uiso 1 1 calc R . . H24B H 0.0082 0.0129 0.0856 0.091 Uiso 1 1 calc R . . H24C H -0.0954 0.0119 0.1500 0.091 Uiso 1 1 calc R . . C31 C 0.4225(3) 0.1358(2) -0.02108(17) 0.0358(8) Uani 1 1 d . . . C32 C 0.5867(4) 0.1667(3) -0.0975(2) 0.0542(10) Uani 1 1 d . . . H32A H 0.6305 0.1841 -0.1398 0.065 Uiso 1 1 calc R . . C33 C 0.6562(4) 0.1416(3) -0.0358(2) 0.0559(10) Uani 1 1 d . . . H33A H 0.7564 0.1372 -0.0267 0.067 Uiso 1 1 calc R . . C34 C 0.5836(4) 0.0917(3) 0.08711(19) 0.0549(10) Uani 1 1 d . . . H34A H 0.5058 0.1111 0.1159 0.082 Uiso 1 1 calc R . . H34B H 0.6731 0.1186 0.1069 0.082 Uiso 1 1 calc R . . H34C H 0.5911 0.0244 0.0880 0.082 Uiso 1 1 calc R . . C41 C 0.1594(4) 0.3285(2) -0.13859(16) 0.0410(8) Uani 1 1 d . . . C42 C 0.3660(5) 0.3518(3) -0.1871(2) 0.0649(11) Uani 1 1 d . . . H42A H 0.4571 0.3413 -0.2044 0.078 Uiso 1 1 calc R . . C43 C 0.2975(5) 0.4339(3) -0.1865(2) 0.0728(13) Uani 1 1 d . . . H43A H 0.3316 0.4907 -0.2036 0.087 Uiso 1 1 calc R . . C44 C 0.0644(4) 0.4918(3) -0.1430(3) 0.0767(14) Uani 1 1 d . . . H44A H 0.0491 0.4936 -0.0918 0.115 Uiso 1 1 calc R . . H44B H -0.0256 0.4779 -0.1701 0.115 Uiso 1 1 calc R . . H44C H 0.0998 0.5516 -0.1581 0.115 Uiso 1 1 calc R . . B1 B 0.2373(4) 0.3153(3) 0.2075(2) 0.0370(9) Uani 1 1 d . . . B2 B 0.3225(5) 0.1793(3) -0.1533(2) 0.0467(10) Uani 1 1 d . . . H1A H 0.149(3) 0.3595(19) 0.1856(14) 0.034(8) Uiso 1 1 d . . . H2B H 0.381(3) 0.1519(18) -0.2048(14) 0.030(7) Uiso 1 1 d . . . H1B H 0.261(3) 0.332(2) 0.2701(15) 0.039(8) Uiso 1 1 d . . . H2A H 0.227(3) 0.139(2) -0.1431(15) 0.036(8) 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 Zn 0.0310(2) 0.0392(2) 0.03038(19) 0.00364(16) -0.00361(14) -0.00055(18) S1 0.0553(6) 0.0437(5) 0.0429(5) 0.0150(4) -0.0145(4) -0.0144(4) S2 0.0237(4) 0.0562(6) 0.0422(5) 0.0071(4) -0.0011(4) 0.0015(4) S3 0.0427(5) 0.0419(5) 0.0523(5) 0.0119(4) 0.0109(4) 0.0075(4) S4 0.0377(5) 0.0605(6) 0.0385(5) 0.0082(4) -0.0133(4) -0.0007(4) N11 0.0364(15) 0.0282(14) 0.0281(14) -0.0012(11) -0.0031(11) -0.0033(12) N12 0.0438(18) 0.0351(16) 0.0423(17) -0.0014(12) 0.0057(14) -0.0078(13) N21 0.0377(16) 0.0321(14) 0.0339(15) 0.0028(12) -0.0023(12) -0.0004(12) N22 0.0380(16) 0.0359(16) 0.0407(16) 0.0021(12) -0.0002(13) -0.0080(13) N31 0.0413(17) 0.0412(17) 0.0442(17) -0.0044(13) 0.0079(13) 0.0009(13) N32 0.0367(17) 0.0407(17) 0.0510(18) -0.0031(13) 0.0015(14) 0.0034(13) N41 0.0551(19) 0.0439(17) 0.0343(16) 0.0014(13) 0.0034(14) -0.0051(15) N42 0.062(2) 0.0442(19) 0.0541(19) 0.0037(15) -0.0052(17) 0.0001(16) C11 0.0379(19) 0.0261(17) 0.0362(18) -0.0006(13) -0.0052(15) -0.0086(14) C12 0.040(2) 0.0351(19) 0.0361(18) -0.0001(14) -0.0092(16) -0.0012(15) C13 0.038(2) 0.041(2) 0.052(2) -0.0032(17) -0.0106(17) -0.0009(17) C14 0.054(2) 0.064(3) 0.058(3) 0.0049(19) 0.017(2) -0.015(2) C21 0.0257(17) 0.0383(19) 0.0297(16) 0.0023(14) 0.0032(13) -0.0012(14) C22 0.048(2) 0.043(2) 0.049(2) 0.0135(17) -0.0150(17) -0.0056(18) C23 0.055(2) 0.037(2) 0.063(2) 0.0134(17) -0.017(2) -0.0013(18) C24 0.063(3) 0.048(2) 0.070(3) 0.000(2) -0.008(2) -0.021(2) C31 0.0386(19) 0.0286(17) 0.0406(19) -0.0058(14) 0.0047(15) 0.0041(14) C32 0.050(2) 0.055(2) 0.060(3) -0.0052(19) 0.023(2) -0.0043(19) C33 0.039(2) 0.057(2) 0.071(3) -0.003(2) 0.004(2) 0.0014(19) C34 0.054(2) 0.053(2) 0.055(2) -0.0032(18) -0.0131(19) 0.0081(19) C41 0.051(2) 0.042(2) 0.0277(17) 0.0034(15) -0.0116(15) -0.0021(17) C42 0.079(3) 0.053(3) 0.066(3) 0.011(2) 0.026(2) -0.005(2) C43 0.089(4) 0.049(3) 0.083(3) 0.014(2) 0.020(3) -0.012(2) C44 0.074(3) 0.043(2) 0.110(4) -0.001(2) -0.011(3) 0.010(2) B1 0.046(2) 0.026(2) 0.039(2) -0.0058(16) 0.0008(18) -0.0041(18) B2 0.056(3) 0.045(2) 0.039(2) -0.0032(19) 0.005(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 Zn S3 2.3298(10) . ? Zn S1 2.3357(10) . ? Zn S4 2.3382(9) . ? Zn S2 2.3436(9) . ? Zn H2A 3.46(3) . ? Zn H1A 3.56(3) . ? Zn B2 3.780(4) . ? Zn B1 3.785(4) . ? Zn H1B 4.97(3) . ? Zn H2B 4.97(3) . ? S1 C11 1.732(3) . ? S2 C21 1.724(3) . ? S3 C31 1.717(3) . ? S4 C41 1.726(4) . ? N11 C11 1.349(4) . ? N11 C12 1.387(4) . ? N11 B1 1.566(5) . ? N12 C11 1.344(4) . ? N12 C13 1.381(4) . ? N12 C14 1.470(4) . ? N21 C21 1.350(4) . ? N21 C22 1.378(4) . ? N21 B1 1.575(4) . ? N22 C21 1.361(4) . ? N22 C23 1.374(4) . ? N22 C24 1.446(4) . ? N31 C31 1.365(4) . ? N31 C32 1.389(4) . ? N31 B2 1.559(5) . ? N32 C31 1.351(4) . ? N32 C33 1.366(4) . ? N32 C34 1.470(4) . ? N41 C41 1.352(4) . ? N41 C42 1.381(4) . ? N41 B2 1.579(5) . ? N42 C43 1.363(5) . ? N42 C41 1.364(4) . ? N42 C44 1.458(5) . ? C12 C13 1.335(4) . ? C22 C23 1.347(5) . ? C32 C33 1.327(5) . ? C42 C43 1.344(5) . ? 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 Zn S1 114.13(4) . . ? S3 Zn S4 115.16(4) . . ? S1 Zn S4 102.74(3) . . ? S3 Zn S2 100.59(3) . . ? S1 Zn S2 115.75(4) . . ? S4 Zn S2 108.91(3) . . ? S3 Zn H2A 59.2(4) . . ? S1 Zn H2A 110.3(5) . . ? S4 Zn H2A 58.7(4) . . ? S2 Zn H2A 133.9(5) . . ? S3 Zn H1A 110.2(5) . . ? S1 Zn H1A 60.3(4) . . ? S4 Zn H1A 134.4(5) . . ? S2 Zn H1A 57.5(4) . . ? H2A Zn H1A 163.4(6) . . ? S3 Zn B2 62.63(7) . . ? S1 Zn B2 94.05(7) . . ? S4 Zn B2 63.39(7) . . ? S2 Zn B2 150.13(7) . . ? H2A Zn B2 16.5(5) . . ? H1A Zn B2 149.3(4) . . ? S3 Zn B1 93.89(6) . . ? S1 Zn B1 62.62(6) . . ? S4 Zn B1 150.95(7) . . ? S2 Zn B1 62.71(6) . . ? H2A Zn B1 148.1(5) . . ? H1A Zn B1 16.8(4) . . ? B2 Zn B1 137.90(9) . . ? S3 Zn H1B 93.9(3) . . ? S1 Zn H1B 63.7(3) . . ? S4 Zn H1B 150.9(3) . . ? S2 Zn H1B 61.6(3) . . ? H2A Zn H1B 148.6(5) . . ? H1A Zn H1B 16.6(5) . . ? B2 Zn H1B 138.8(3) . . ? B1 Zn H1B 1.2(3) . . ? S3 Zn H2B 61.9(3) . . ? S1 Zn H2B 94.8(3) . . ? S4 Zn H2B 63.7(3) . . ? S2 Zn H2B 149.4(3) . . ? H2A Zn H2B 15.9(6) . . ? H1A Zn H2B 149.6(5) . . ? B2 Zn H2B 0.9(3) . . ? B1 Zn H2B 137.9(3) . . ? H1B Zn H2B 138.8(4) . . ? C11 S1 Zn 103.59(10) . . ? C21 S2 Zn 95.55(10) . . ? C31 S3 Zn 105.51(11) . . ? C41 S4 Zn 95.85(10) . . ? C11 N11 C12 107.1(3) . . ? C11 N11 B1 129.7(3) . . ? C12 N11 B1 123.2(3) . . ? C11 N12 C13 108.8(3) . . ? C11 N12 C14 126.0(3) . . ? C13 N12 C14 125.1(3) . . ? C21 N21 C22 107.6(3) . . ? C21 N21 B1 129.2(3) . . ? C22 N21 B1 123.2(3) . . ? C21 N22 C23 108.7(3) . . ? C21 N22 C24 126.4(3) . . ? C23 N22 C24 124.8(3) . . ? C31 N31 C32 106.1(3) . . ? C31 N31 B2 128.8(3) . . ? C32 N31 B2 124.9(3) . . ? C31 N32 C33 109.3(3) . . ? C31 N32 C34 125.2(3) . . ? C33 N32 C34 125.5(3) . . ? C41 N41 C42 107.6(3) . . ? C41 N41 B2 129.7(3) . . ? C42 N41 B2 122.7(3) . . ? C43 N42 C41 108.6(3) . . ? C43 N42 C44 125.6(3) . . ? C41 N42 C44 125.7(3) . . ? N12 C11 N11 108.4(3) . . ? N12 C11 S1 123.8(2) . . ? N11 C11 S1 127.7(2) . . ? C13 C12 N11 108.9(3) . . ? C12 C13 N12 106.8(3) . . ? N21 C21 N22 108.0(3) . . ? N21 C21 S2 128.3(2) . . ? N22 C21 S2 123.7(2) . . ? C23 C22 N21 108.9(3) . . ? C22 C23 N22 106.8(3) . . ? N32 C31 N31 107.9(3) . . ? N32 C31 S3 123.7(3) . . ? N31 C31 S3 128.3(2) . . ? C33 C32 N31 109.8(3) . . ? C32 C33 N32 107.0(3) . . ? N41 C41 N42 107.8(3) . . ? N41 C41 S4 128.5(3) . . ? N42 C41 S4 123.7(3) . . ? C43 C42 N41 108.4(4) . . ? C42 C43 N42 107.6(4) . . ? N11 B1 N21 108.3(3) . . ? N11 B1 Zn 75.94(16) . . ? N21 B1 Zn 70.85(15) . . ? N31 B2 N41 110.1(3) . . ? N31 B2 Zn 76.72(18) . . ? N41 B2 Zn 69.77(17) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 28.15 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.395 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.064 data_tls10 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H24 B2 N8 S4 Tl2' _chemical_formula_weight 887.03 _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' 'Tl' 'Tl' -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.5696(4) _cell_length_b 14.1642(7) _cell_length_c 11.3006(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.9660(10) _cell_angle_gamma 90.00 _cell_volume 1272.11(10) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.316 _exptl_crystal_density_method ? _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 13.002 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8986 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 28.27 _reflns_number_total 2865 _reflns_number_observed 2558 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0162P)^2^+3.9895P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2865 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_obs 0.0292 _refine_ls_wR_factor_all 0.0644 _refine_ls_wR_factor_obs 0.0616 _refine_ls_goodness_of_fit_all 1.128 _refine_ls_goodness_of_fit_obs 1.146 _refine_ls_restrained_S_all 1.128 _refine_ls_restrained_S_obs 1.146 _refine_ls_shift/esd_max 0.000 _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 Tl Tl 0.49026(3) 0.151855(14) 0.03026(2) 0.03394(9) Uani 1 d . . S1 S 0.2803(2) -0.21079(10) -0.3167(2) 0.0400(3) Uani 1 d . . S2 S 0.7621(2) 0.00841(10) 0.01590(12) 0.0332(3) Uani 1 d . . N11 N 0.1134(5) -0.0440(3) -0.3324(4) 0.0278(9) Uani 1 d . . N12 N 0.3788(5) -0.0260(3) -0.3038(4) 0.0227(8) Uani 1 d . . N21 N 0.8295(5) 0.1505(3) -0.1196(4) 0.0294(9) Uani 1 d . . N22 N 0.6705(4) 0.0415(3) -0.2432(4) 0.0224(8) Uani 1 d . . C11 C 0.2565(6) -0.0910(3) -0.3193(4) 0.0254(10) Uani 1 d . . C12 C 0.1457(6) 0.0519(4) -0.3230(5) 0.0324(11) Uani 1 d . . H12A H 0.0689(6) 0.1004(4) -0.3270(5) 0.039 Uiso 1 calc R . C13 C 0.3079(6) 0.0624(3) -0.3071(5) 0.0292(10) Uani 1 d . . H13A H 0.3644(6) 0.1204(3) -0.2995(5) 0.035 Uiso 1 calc R . C14 C -0.0450(6) -0.0865(5) -0.3419(6) 0.0402(13) Uani 1 d . . H14A H -0.1273(6) -0.0372(5) -0.3507(6) 0.060 Uiso 1 calc R . H14B H -0.0284(6) -0.1230(5) -0.2655(6) 0.060 Uiso 1 calc R . H14C H -0.0852(6) -0.1276(5) -0.4159(6) 0.060 Uiso 1 calc R . C21 C 0.7530(6) 0.0666(3) -0.1193(4) 0.0243(9) Uani 1 d . . C22 C 0.7981(7) 0.1784(4) -0.2427(5) 0.0332(11) Uani 1 d . . H22A H 0.8371(7) 0.2335(4) -0.2689(5) 0.040 Uiso 1 calc R . C23 C 0.6998(6) 0.1107(4) -0.3189(5) 0.0291(10) Uani 1 d . . H23A H 0.6583(6) 0.1106(4) -0.4085(5) 0.035 Uiso 1 calc R . C24 C 0.9369(8) 0.2008(4) -0.0059(6) 0.0445(15) Uani 1 d . . H24A H 0.9765(8) 0.2588(4) -0.0306(6) 0.067 Uiso 1 calc R . H24B H 1.0324(8) 0.1615(4) 0.0419(6) 0.067 Uiso 1 calc R . H24C H 0.8733(8) 0.2155(4) 0.0470(6) 0.067 Uiso 1 calc R . B B 0.5628(6) -0.0477(4) -0.2937(5) 0.0238(10) Uani 1 d . . H01 H 0.5642(70) -0.0599(41) -0.3952(54) 0.036(15) Uiso 1 d . . H02 H 0.6074(79) -0.1139(46) -0.2252(60) 0.046(17) Uiso 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 Tl 0.03446(12) 0.02699(12) 0.03772(13) 0.00813(9) 0.01045(8) 0.00100(8) S1 0.0283(6) 0.0215(6) 0.0648(9) -0.0106(6) 0.0109(6) -0.0069(5) S2 0.0357(7) 0.0356(7) 0.0272(6) 0.0002(5) 0.0104(5) -0.0087(5) N11 0.020(2) 0.036(2) 0.026(2) -0.001(2) 0.0061(15) 0.001(2) N12 0.023(2) 0.016(2) 0.027(2) -0.001(2) 0.0072(15) 0.0024(15) N21 0.028(2) 0.022(2) 0.035(2) -0.005(2) 0.009(2) -0.010(2) N22 0.020(2) 0.019(2) 0.028(2) -0.002(2) 0.0093(15) -0.002(2) C11 0.022(2) 0.023(2) 0.027(2) -0.005(2) 0.005(2) -0.003(2) C12 0.029(2) 0.031(3) 0.036(3) 0.003(2) 0.011(2) 0.007(2) C13 0.031(2) 0.019(2) 0.037(3) 0.003(2) 0.013(2) 0.006(2) C14 0.018(2) 0.054(4) 0.048(3) -0.004(3) 0.012(2) -0.001(2) C21 0.020(2) 0.024(2) 0.028(2) -0.004(2) 0.009(2) -0.003(2) C22 0.034(3) 0.023(2) 0.043(3) 0.004(2) 0.015(2) -0.004(2) C23 0.031(2) 0.023(2) 0.032(2) 0.002(2) 0.010(2) -0.001(2) C24 0.046(3) 0.037(3) 0.047(3) -0.018(3) 0.013(3) -0.023(3) B 0.020(2) 0.018(2) 0.033(3) -0.004(2) 0.010(2) -0.003(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 Tl S2 3.0426(13) 3_655 ? Tl S2 3.1406(15) . ? S1 C11 1.707(5) . ? S2 C21 1.712(5) . ? S2 Tl 3.0426(13) 3_655 ? N11 C11 1.355(6) . ? N11 C12 1.382(7) . ? N11 C14 1.452(6) . ? N12 C11 1.357(6) . ? N12 C13 1.386(6) . ? N12 B 1.568(6) . ? N21 C21 1.358(6) . ? N21 C22 1.372(7) . ? N21 C24 1.456(6) . ? N22 C21 1.358(6) . ? N22 C23 1.385(6) . ? N22 B 1.542(6) . ? C12 C13 1.342(7) . ? C22 C23 1.351(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 S2 Tl S2 90.10(4) 3_655 . ? C21 S2 Tl 114.5(2) . 3_655 ? C21 S2 Tl 87.0(2) . . ? Tl S2 Tl 89.90(4) 3_655 . ? C11 N11 C12 109.1(4) . . ? C11 N11 C14 125.9(5) . . ? C12 N11 C14 124.6(4) . . ? C11 N12 C13 107.5(4) . . ? C11 N12 B 125.7(4) . . ? C13 N12 B 126.7(4) . . ? C21 N21 C22 110.0(4) . . ? C21 N21 C24 124.9(5) . . ? C22 N21 C24 125.0(4) . . ? C21 N22 C23 107.8(4) . . ? C21 N22 B 127.2(4) . . ? C23 N22 B 125.0(4) . . ? N11 C11 N12 107.7(4) . . ? N11 C11 S1 126.0(4) . . ? N12 C11 S1 126.2(4) . . ? C13 C12 N11 106.7(4) . . ? C12 C13 N12 108.9(5) . . ? N21 C21 N22 107.0(4) . . ? N21 C21 S2 124.2(4) . . ? N22 C21 S2 128.7(4) . . ? C23 C22 N21 106.3(5) . . ? C22 C23 N22 108.8(4) . . ? N22 B N12 108.2(4) . . ? _refine_diff_density_max 1.208 _refine_diff_density_min -1.239 _refine_diff_density_rms 0.134 data_zni _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H12 B I N4 S2 Zn' _chemical_formula_weight 431.42 _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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.362(2) _cell_length_b 9.937(2) _cell_length_c 13.483(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.31(2) _cell_angle_gamma 90.00 _cell_volume 1427.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 4.57 _cell_measurement_theta_max 12.46 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .3 _exptl_crystal_size_mid .5 _exptl_crystal_size_min .4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method ? _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 4.158 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5359 _exptl_absorpt_correction_T_max 0.7101 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3085 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 24.00 _reflns_number_total 2226 _reflns_number_observed 1720 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0364P)^2^+1.8137P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2226 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_obs 0.0353 _refine_ls_wR_factor_all 0.0879 _refine_ls_wR_factor_obs 0.0799 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_goodness_of_fit_obs 1.089 _refine_ls_restrained_S_all 1.042 _refine_ls_restrained_S_obs 1.089 _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 Zn Zn 0.52589(8) -0.89593(7) 0.86847(5) 0.0478(3) Uani 1 d . . I I 0.69405(4) -0.99254(5) 1.03158(3) 0.0575(2) Uani 1 d . . S1 S 0.4476(2) -1.03711(14) 0.72673(11) 0.0445(4) Uani 1 d . . S2 S 0.4300(2) -0.69154(14) 0.86183(12) 0.0423(4) Uani 1 d . . N11 N 0.5103(4) -0.8213(4) 0.6247(3) 0.0298(10) Uani 1 d . . N12 N 0.3611(4) -0.9497(5) 0.5251(3) 0.0361(11) Uani 1 d . . N21 N 0.5705(4) -0.6141(4) 0.7392(3) 0.0309(10) Uani 1 d . . N22 N 0.4696(4) -0.4517(4) 0.7840(3) 0.0306(10) Uani 1 d . . C11 C 0.4404(5) -0.9310(5) 0.6240(4) 0.0306(12) Uani 1 d . . C12 C 0.4717(6) -0.7727(6) 0.5219(4) 0.0408(14) Uani 1 d . . H12A H 0.5044(6) -0.6975(6) 0.4995(4) 0.049 Uiso 1 calc R . C13 C 0.3807(6) -0.8507(6) 0.4609(4) 0.044(2) Uani 1 d . . H13A H 0.3382(6) -0.8406(6) 0.3887(4) 0.052 Uiso 1 calc R . C14 C 0.2667(6) -1.0566(7) 0.4902(5) 0.052(2) Uani 1 d . . H14A H 0.2221(6) -1.0480(7) 0.4156(5) 0.079 Uiso 1 calc R . H14B H 0.2089(6) -1.0492(7) 0.5275(5) 0.079 Uiso 1 calc R . H14C H 0.3075(6) -1.1427(7) 0.5045(5) 0.079 Uiso 1 calc R . C21 C 0.4931(5) -0.5859(5) 0.7921(4) 0.0293(12) Uani 1 d . . C22 C 0.5954(6) -0.4948(5) 0.6976(5) 0.0375(13) Uani 1 d . . H22A H 0.6466(6) -0.4851(5) 0.6572(5) 0.045 Uiso 1 calc R . C23 C 0.5332(6) -0.3955(5) 0.7252(4) 0.0374(14) Uani 1 d . . H23A H 0.5334(6) -0.3051(5) 0.7075(4) 0.045 Uiso 1 calc R . C24 C 0.3886(6) -0.3789(6) 0.8296(5) 0.046(2) Uani 1 d . . H24A H 0.3879(6) -0.2850(6) 0.8125(5) 0.069 Uiso 1 calc R . H24B H 0.4200(6) -0.3897(6) 0.9051(5) 0.069 Uiso 1 calc R . H24C H 0.3049(6) -0.4141(6) 0.8013(5) 0.069 Uiso 1 calc R . B B 0.6168(6) -0.7533(6) 0.7180(5) 0.0298(14) Uani 1 d . . H1 H 0.6361(42) -0.8205(44) 0.7884(35) 0.022(12) Uiso 1 d . . H2 H 0.6992(40) -0.7351(40) 0.6934(31) 0.012(11) Uiso 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 0.0710(6) 0.0318(4) 0.0279(4) 0.0003(3) 0.0009(3) 0.0144(4) I 0.0460(3) 0.0783(4) 0.0406(3) 0.0262(2) 0.0053(2) 0.0073(2) S1 0.0752(12) 0.0270(7) 0.0325(8) -0.0002(6) 0.0202(8) -0.0058(8) S2 0.0593(10) 0.0283(7) 0.0505(9) 0.0067(7) 0.0334(8) 0.0048(7) N11 0.038(3) 0.027(2) 0.024(2) -0.002(2) 0.011(2) 0.002(2) N12 0.034(3) 0.043(3) 0.029(2) -0.004(2) 0.009(2) 0.002(2) N21 0.034(3) 0.029(2) 0.029(2) 0.001(2) 0.010(2) 0.002(2) N22 0.037(3) 0.020(2) 0.036(2) 0.002(2) 0.014(2) 0.004(2) C11 0.037(3) 0.029(3) 0.028(3) -0.001(2) 0.014(3) 0.007(3) C12 0.051(4) 0.041(3) 0.030(3) 0.010(3) 0.014(3) 0.006(3) C13 0.050(4) 0.054(4) 0.026(3) 0.009(3) 0.014(3) 0.014(3) C14 0.041(4) 0.067(4) 0.047(4) -0.019(3) 0.013(3) -0.008(3) C21 0.031(3) 0.026(3) 0.026(3) 0.002(2) 0.005(2) 0.001(2) C22 0.048(3) 0.027(3) 0.045(3) 0.002(3) 0.026(3) -0.004(3) C23 0.049(4) 0.025(3) 0.039(3) 0.004(2) 0.017(3) -0.004(3) C24 0.057(4) 0.033(3) 0.052(4) 0.003(3) 0.025(3) 0.013(3) B 0.030(3) 0.032(3) 0.027(3) -0.002(3) 0.008(3) 0.000(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 Zn S1 2.287(2) . ? Zn S2 2.292(2) . ? Zn I 2.5479(9) . ? S1 C11 1.719(5) . ? S2 C21 1.723(5) . ? N11 C11 1.347(7) . ? N11 C12 1.387(6) . ? N11 B 1.564(7) . ? N12 C11 1.339(7) . ? N12 C13 1.378(7) . ? N12 C14 1.466(8) . ? N21 C21 1.340(7) . ? N21 C22 1.382(6) . ? N21 B 1.543(7) . ? N22 C21 1.357(7) . ? N22 C23 1.364(7) . ? N22 C24 1.463(7) . ? C12 C13 1.325(8) . ? C22 C23 1.339(8) . ? 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 S2 117.98(7) . . ? S1 Zn I 116.60(5) . . ? S2 Zn I 124.86(5) . . ? C11 S1 Zn 101.1(2) . . ? C21 S2 Zn 106.2(2) . . ? C11 N11 C12 107.1(4) . . ? C11 N11 B 130.1(4) . . ? C12 N11 B 122.7(5) . . ? C11 N12 C13 109.1(5) . . ? C11 N12 C14 125.8(5) . . ? C13 N12 C14 125.1(5) . . ? C21 N21 C22 107.5(4) . . ? C21 N21 B 128.0(4) . . ? C22 N21 B 124.3(4) . . ? C21 N22 C23 108.7(4) . . ? C21 N22 C24 125.9(4) . . ? C23 N22 C24 125.4(4) . . ? N12 C11 N11 108.1(4) . . ? N12 C11 S1 123.1(4) . . ? N11 C11 S1 128.9(4) . . ? C13 C12 N11 108.9(5) . . ? C12 C13 N12 106.8(5) . . ? N21 C21 N22 108.0(4) . . ? N21 C21 S2 129.6(4) . . ? N22 C21 S2 122.3(4) . . ? C23 C22 N21 108.5(5) . . ? C22 C23 N22 107.3(5) . . ? N21 B N11 108.6(4) . . ? _refine_diff_density_max 0.596 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.096 data_znme _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C9 H15 B N4 S2 Zn' _chemical_formula_weight 319.55 _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' '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' 'B' 'B' 0.0013 0.0007 '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 7.6520(10) _cell_length_b 13.822(3) _cell_length_c 13.469(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.588(7) _cell_angle_gamma 90.00 _cell_volume 1390.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 4.52 _cell_measurement_theta_max 10.45 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .1 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method ? _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 2.049 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4392 _exptl_absorpt_correction_T_max 0.5553 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1979 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.1289 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 22.50 _reflns_number_total 1784 _reflns_number_observed 992 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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^)+(0.0540P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1783 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_obs 0.0579 _refine_ls_wR_factor_all 0.1481 _refine_ls_wR_factor_obs 0.1164 _refine_ls_goodness_of_fit_all 1.014 _refine_ls_goodness_of_fit_obs 1.111 _refine_ls_restrained_S_all 1.016 _refine_ls_restrained_S_obs 1.111 _refine_ls_shift/esd_max 0.000 _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 Zn Zn 0.0933(2) 0.41136(10) 0.17501(9) 0.0478(5) Uani 1 d . . S1 S 0.0835(4) 0.3602(2) 0.3395(2) 0.0484(8) Uani 1 d . . S2 S 0.3985(4) 0.4502(2) 0.1802(2) 0.0447(8) Uani 1 d . . N11 N 0.1938(10) 0.5505(6) 0.3812(6) 0.038(2) Uani 1 d . . N12 N 0.2460(11) 0.4525(7) 0.5118(6) 0.049(2) Uani 1 d . . N21 N 0.2926(11) 0.6299(6) 0.2304(6) 0.039(2) Uani 1 d . . N22 N 0.5196(11) 0.6314(7) 0.1580(6) 0.041(2) Uani 1 d . . B B 0.1304(17) 0.5975(9) 0.2740(8) 0.040(3) Uani 1 d . . HA H 0.0657(102) 0.6630(61) 0.2773(56) 0.039(26) Uiso 1 d . . HB H 0.0615(86) 0.5319(48) 0.2113(46) 0.012(19) Uiso 1 d . . C1 C -0.0827(15) 0.3703(7) 0.0530(8) 0.065(4) Uani 1 d . . H1A H -0.0541(15) 0.3995(7) -0.0061(8) 0.098 Uiso 1 calc R . H1B H -0.2003(15) 0.3902(7) 0.0588(8) 0.098 Uiso 1 calc R . H1C H -0.0796(15) 0.3011(7) 0.0470(8) 0.098 Uiso 1 calc R . C11 C 0.1771(12) 0.4590(8) 0.4094(7) 0.037(3) Uani 1 d . . C12 C 0.2752(14) 0.6015(8) 0.4678(8) 0.057(3) Uani 1 d . . H12A H 0.3041(14) 0.6670(8) 0.4697(8) 0.069 Uiso 1 calc R . C13 C 0.3048(15) 0.5432(9) 0.5460(8) 0.056(3) Uani 1 d . . H13A H 0.3563(15) 0.5600(9) 0.6129(8) 0.067 Uiso 1 calc R . C14 C 0.2514(15) 0.3667(8) 0.5724(7) 0.062(3) Uani 1 d . . H14A H 0.3064(15) 0.3813(8) 0.6419(7) 0.093 Uiso 1 calc R . H14B H 0.3196(15) 0.3177(8) 0.5474(7) 0.093 Uiso 1 calc R . H14C H 0.1317(15) 0.3438(8) 0.5685(7) 0.093 Uiso 1 calc R . C21 C 0.3982(13) 0.5724(7) 0.1887(7) 0.034(2) Uani 1 d . . C22 C 0.3468(15) 0.7254(8) 0.2238(7) 0.049(3) Uani 1 d . . H22A H 0.2940(15) 0.7791(8) 0.2469(7) 0.059 Uiso 1 calc R . C23 C 0.4865(15) 0.7278(9) 0.1791(7) 0.053(3) Uani 1 d . . H23A H 0.5486(15) 0.7821(9) 0.1651(7) 0.063 Uiso 1 calc R . C24 C 0.6555(14) 0.5993(8) 0.1050(8) 0.059(3) Uani 1 d . . H24A H 0.7244(14) 0.6538(8) 0.0916(8) 0.089 Uiso 1 calc R . H24B H 0.5988(14) 0.5693(8) 0.0419(8) 0.089 Uiso 1 calc R . H24C H 0.7330(14) 0.5534(8) 0.1465(8) 0.089 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 Zn 0.0547(9) 0.0465(8) 0.0383(7) -0.0036(7) 0.0014(6) -0.0026(7) S1 0.053(2) 0.047(2) 0.046(2) 0.0011(14) 0.0125(14) -0.011(2) S2 0.050(2) 0.039(2) 0.047(2) -0.0035(13) 0.0138(14) 0.0053(14) N11 0.042(5) 0.039(6) 0.034(5) -0.009(4) 0.007(4) 0.000(4) N12 0.043(6) 0.061(7) 0.038(5) 0.000(5) 0.001(4) -0.003(5) N21 0.047(5) 0.030(5) 0.039(5) 0.002(4) 0.005(4) 0.004(5) N22 0.042(5) 0.044(6) 0.038(5) 0.004(4) 0.009(4) 0.003(5) B 0.053(8) 0.023(7) 0.046(7) -0.007(6) 0.017(6) 0.005(7) C1 0.075(9) 0.049(7) 0.061(8) 0.003(6) -0.009(7) -0.004(7) C11 0.029(6) 0.047(7) 0.036(6) 0.000(5) 0.011(5) 0.005(5) C12 0.065(8) 0.056(8) 0.054(7) -0.017(7) 0.021(6) -0.012(7) C13 0.067(8) 0.070(9) 0.033(6) -0.009(7) 0.015(6) -0.010(7) C14 0.057(8) 0.089(10) 0.039(7) 0.009(7) 0.008(6) -0.013(7) C21 0.038(6) 0.029(6) 0.033(5) 0.004(5) 0.003(5) 0.014(5) C22 0.068(9) 0.036(8) 0.041(7) 0.001(5) 0.007(6) 0.001(6) C23 0.051(8) 0.052(9) 0.052(7) 0.008(6) 0.005(6) 0.005(7) C24 0.048(7) 0.073(9) 0.062(7) -0.007(7) 0.024(6) 0.000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn C1 1.967(10) . ? Zn S1 2.342(3) . ? Zn S2 2.382(3) . ? S1 C11 1.724(10) . ? S2 C21 1.693(9) . ? N11 C11 1.335(11) . ? N11 C12 1.389(12) . ? N11 B 1.561(14) . ? N12 C11 1.367(11) . ? N12 C13 1.377(12) . ? N12 C14 1.435(12) . ? N21 C21 1.341(11) . ? N21 C22 1.392(12) . ? N21 B 1.550(14) . ? N22 C21 1.365(12) . ? N22 C23 1.396(13) . ? N22 C24 1.454(12) . ? C12 C13 1.307(14) . ? C22 C23 1.337(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 Zn S1 123.0(3) . . ? C1 Zn S2 125.3(4) . . ? S1 Zn S2 105.88(10) . . ? C11 S1 Zn 100.5(3) . . ? C21 S2 Zn 102.2(4) . . ? C11 N11 C12 107.2(8) . . ? C11 N11 B 129.0(8) . . ? C12 N11 B 123.8(9) . . ? C11 N12 C13 107.7(9) . . ? C11 N12 C14 125.8(10) . . ? C13 N12 C14 126.5(9) . . ? C21 N21 C22 108.6(9) . . ? C21 N21 B 126.4(9) . . ? C22 N21 B 124.9(9) . . ? C21 N22 C23 110.1(9) . . ? C21 N22 C24 124.9(9) . . ? C23 N22 C24 124.9(10) . . ? N21 B N11 110.9(8) . . ? N11 C11 N12 108.0(9) . . ? N11 C11 S1 130.4(7) . . ? N12 C11 S1 121.5(8) . . ? C13 C12 N11 109.3(10) . . ? C12 C13 N12 107.7(10) . . ? N21 C21 N22 106.5(8) . . ? N21 C21 S2 128.9(8) . . ? N22 C21 S2 124.4(8) . . ? C23 C22 N21 109.3(10) . . ? C22 C23 N22 105.4(10) . . ? _refine_diff_density_max 0.484 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.103