# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1878 data_tony _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H17 B N6 S2 Zn' _chemical_formula_weight 385.62 _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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.6828(14) _cell_length_b 12.1699(10) _cell_length_c 18.895(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3376.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.33 _cell_measurement_theta_max 12.49 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .3 _exptl_crystal_size_mid .6 _exptl_crystal_size_min .5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method ? _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.705 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1649 _exptl_absorpt_correction_T_max 0.1915 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 2944 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2944 _reflns_number_observed 1905 _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 2 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^)+(0.0407P)^2^+1.8018P] 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 0.0014(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2942 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_obs 0.0449 _refine_ls_wR_factor_all 0.1172 _refine_ls_wR_factor_obs 0.0966 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_goodness_of_fit_obs 1.100 _refine_ls_restrained_S_all 1.054 _refine_ls_restrained_S_obs 1.100 _refine_ls_shift/esd_max -0.472 _refine_ls_shift/esd_mean 0.011 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 0.58194(4) 0.16225(5) 0.62704(3) 0.0397(2) Uani 1 d . . S1 S 0.58850(9) 0.20205(12) 0.50250(7) 0.0445(3) Uani 1 d . . S2 S 0.53661(9) 0.32885(11) 0.68630(7) 0.0443(3) Uani 1 d . . N11 N 0.7551(3) 0.3071(3) 0.5169(2) 0.0350(9) Uani 1 d . . N12 N 0.7358(3) 0.2185(4) 0.4181(2) 0.0431(10) Uani 1 d . . N21 N 0.6563(3) 0.4302(3) 0.5928(2) 0.0356(10) Uani 1 d . . N22 N 0.5262(3) 0.5140(4) 0.6083(2) 0.0472(11) Uani 1 d . . N31 N 0.7613(3) 0.2747(3) 0.6496(2) 0.0376(10) Uani 1 d . . N32 N 0.7146(3) 0.1793(3) 0.6578(2) 0.0398(10) Uani 1 d . . C1 C 0.5087(3) 0.0283(4) 0.6467(3) 0.0423(12) Uani 1 d . . H1A H 0.4485(3) 0.0374(4) 0.6277(3) 0.063 Uiso 1 calc R . H1B H 0.5050(3) 0.0168(4) 0.6969(3) 0.063 Uiso 1 calc R . H1C H 0.5372(3) -0.0341(4) 0.6249(3) 0.063 Uiso 1 calc R . C11 C 0.6960(3) 0.2444(4) 0.4801(2) 0.0341(11) Uani 1 d . . C12 C 0.8322(3) 0.3198(5) 0.4762(3) 0.0476(14) Uani 1 d . . H12A H 0.8838(3) 0.3596(5) 0.4888(3) 0.057 Uiso 1 calc R . C13 C 0.8204(4) 0.2657(5) 0.4162(3) 0.058(2) Uani 1 d . . H13A H 0.8621(4) 0.2607(5) 0.3793(3) 0.069 Uiso 1 calc R . C14 C 0.6962(4) 0.1522(5) 0.3621(3) 0.067(2) Uani 1 d . . H14A H 0.7418(8) 0.1366(29) 0.3271(11) 0.101 Uiso 1 calc R . H14B H 0.6468(19) 0.1917(15) 0.3406(15) 0.101 Uiso 1 calc R . H14C H 0.6738(26) 0.0846(15) 0.3816(5) 0.101 Uiso 1 calc R . C21 C 0.5763(3) 0.4246(4) 0.6278(2) 0.0365(11) Uani 1 d . . C22 C 0.6544(4) 0.5236(4) 0.5512(3) 0.0497(14) Uani 1 d . . H22A H 0.7008(4) 0.5469(4) 0.5213(3) 0.060 Uiso 1 calc R . C23 C 0.5752(4) 0.5745(4) 0.5610(3) 0.0526(14) Uani 1 d . . H23A H 0.5566(4) 0.6395(4) 0.5395(3) 0.063 Uiso 1 calc R . C24 C 0.4363(4) 0.5431(5) 0.6347(3) 0.067(2) Uani 1 d . . H24A H 0.4114(13) 0.4824(14) 0.6607(20) 0.101 Uiso 1 calc R . H24B H 0.3971(9) 0.5604(35) 0.5956(4) 0.101 Uiso 1 calc R . H24C H 0.4411(5) 0.6059(22) 0.6653(19) 0.101 Uiso 1 calc R . C31 C 0.8363(3) 0.2699(5) 0.6904(3) 0.0481(14) Uani 1 d . . H31A H 0.8804(3) 0.3244(5) 0.6938(3) 0.058 Uiso 1 calc R . C32 C 0.8372(4) 0.1729(5) 0.7257(3) 0.058(2) Uani 1 d . . H32A H 0.8808(4) 0.1482(5) 0.7577(3) 0.069 Uiso 1 calc R . C33 C 0.7603(4) 0.1194(5) 0.7042(3) 0.0491(13) Uani 1 d . . H33A H 0.7424(4) 0.0503(5) 0.7200(3) 0.059 Uiso 1 calc R . B B 0.7459(4) 0.3610(5) 0.5916(3) 0.0369(13) Uani 1 d . . H H 0.8014(30) 0.4224(38) 0.5988(23) 0.041(13) 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 0.0377(3) 0.0385(3) 0.0431(3) 0.0024(3) 0.0010(3) -0.0049(3) S1 0.0359(7) 0.0604(8) 0.0371(7) 0.0002(6) -0.0012(6) -0.0136(6) S2 0.0468(7) 0.0423(7) 0.0438(7) -0.0016(6) 0.0103(6) 0.0008(6) N11 0.029(2) 0.038(2) 0.039(2) 0.002(2) -0.001(2) -0.003(2) N12 0.041(2) 0.052(3) 0.036(2) -0.002(2) 0.005(2) -0.008(2) N21 0.035(2) 0.031(2) 0.041(2) 0.003(2) 0.002(2) -0.004(2) N22 0.046(3) 0.044(3) 0.051(3) -0.002(2) -0.004(2) 0.005(2) N31 0.030(2) 0.045(3) 0.038(2) -0.005(2) -0.007(2) -0.005(2) N32 0.043(2) 0.040(3) 0.036(2) 0.000(2) -0.004(2) 0.004(2) C1 0.038(3) 0.039(3) 0.050(3) 0.001(2) 0.011(2) -0.006(2) C11 0.033(2) 0.036(3) 0.034(3) 0.007(2) 0.000(2) 0.000(2) C12 0.032(3) 0.063(4) 0.048(3) 0.004(3) 0.001(2) -0.008(3) C13 0.049(3) 0.075(4) 0.049(4) 0.005(3) 0.020(3) -0.001(3) C14 0.073(4) 0.081(5) 0.047(3) -0.020(3) 0.008(3) -0.010(4) C21 0.041(3) 0.034(3) 0.034(3) -0.009(2) -0.007(2) 0.003(2) C22 0.054(3) 0.042(3) 0.053(3) 0.010(3) -0.001(3) -0.009(3) C23 0.060(4) 0.037(3) 0.060(4) 0.009(3) -0.008(3) 0.003(3) C24 0.053(4) 0.072(4) 0.078(4) 0.001(4) 0.002(3) 0.027(3) C31 0.039(3) 0.063(4) 0.042(3) -0.009(3) -0.010(3) -0.002(3) C32 0.058(4) 0.074(4) 0.041(3) -0.001(3) -0.020(3) 0.010(3) C33 0.054(3) 0.049(3) 0.044(3) 0.000(3) -0.001(3) 0.013(3) B 0.028(3) 0.041(3) 0.042(3) -0.002(3) -0.004(3) -0.010(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 C1 1.988(4) . ? Zn N32 2.043(4) . ? Zn S1 2.4044(14) . ? Zn S2 2.4099(14) . ? S1 C11 1.714(5) . ? S2 C21 1.708(5) . ? N11 C11 1.348(6) . ? N11 C12 1.377(6) . ? N11 B 1.562(7) . ? N12 C11 1.345(6) . ? N12 C13 1.369(7) . ? N12 C14 1.452(7) . ? N21 C21 1.349(6) . ? N21 C22 1.382(6) . ? N21 B 1.563(7) . ? N22 C23 1.363(7) . ? N22 C21 1.365(6) . ? N22 C24 1.454(6) . ? N31 C31 1.345(6) . ? N31 N32 1.357(5) . ? N31 B 1.534(7) . ? N32 C33 1.323(6) . ? C12 C13 1.322(8) . ? C22 C23 1.330(7) . ? C31 C32 1.356(8) . ? C32 C33 1.366(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 C1 Zn N32 123.1(2) . . ? C1 Zn S1 111.68(15) . . ? N32 Zn S1 102.68(12) . . ? C1 Zn S2 117.00(14) . . ? N32 Zn S2 92.62(12) . . ? S1 Zn S2 107.24(5) . . ? C11 S1 Zn 109.8(2) . . ? C21 S2 Zn 100.3(2) . . ? C11 N11 C12 107.7(4) . . ? C11 N11 B 130.4(4) . . ? C12 N11 B 121.9(4) . . ? C11 N12 C13 108.6(4) . . ? C11 N12 C14 126.2(4) . . ? C13 N12 C14 125.3(5) . . ? C21 N21 C22 107.6(4) . . ? C21 N21 B 135.5(4) . . ? C22 N21 B 116.8(4) . . ? C23 N22 C21 108.8(4) . . ? C23 N22 C24 124.9(5) . . ? C21 N22 C24 126.2(5) . . ? C31 N31 N32 108.1(4) . . ? C31 N31 B 124.0(4) . . ? N32 N31 B 126.3(4) . . ? C33 N32 N31 106.9(4) . . ? C33 N32 Zn 128.0(4) . . ? N31 N32 Zn 122.4(3) . . ? N12 C11 N11 107.6(4) . . ? N12 C11 S1 123.0(4) . . ? N11 C11 S1 129.4(4) . . ? C13 C12 N11 108.4(5) . . ? C12 C13 N12 107.8(5) . . ? N21 C21 N22 107.3(4) . . ? N21 C21 S2 130.4(4) . . ? N22 C21 S2 122.3(4) . . ? C23 C22 N21 108.7(5) . . ? C22 C23 N22 107.5(5) . . ? N31 C31 C32 109.2(5) . . ? C31 C32 C33 105.1(5) . . ? N32 C33 C32 110.7(5) . . ? N31 B N11 110.2(4) . . ? N31 B N21 118.8(4) . . ? N11 B N21 108.2(4) . . ? _refine_diff_density_max 0.326 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.073 data_2cks10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H44 B2 Cl N12 O4 S6 Tl' _chemical_formula_weight 1378.81 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8480(6) _cell_length_b 12.0738(7) _cell_length_c 22.1239(12) _cell_angle_alpha 90.2960(10) _cell_angle_beta 97.4230(10) _cell_angle_gamma 109.7240(10) _cell_volume 2950.1(3) _cell_formula_units_Z 2 _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 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 3.050 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5806 _exptl_absorpt_correction_T_max 0.7501 _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 20600 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.33 _reflns_number_total 12786 _reflns_number_gt 10116 _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^)+(0.0566P)^2^+5.8937P] 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 0.00065(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12786 _refine_ls_number_parameters 725 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl1 Tl 0.0000 0.5000 0.0000 0.02775(8) Uani 1 2 d S . . Tl2 Tl 0.0000 0.5000 0.5000 0.02852(8) Uani 1 2 d S . . S1 S -0.00653(10) 0.70004(10) 0.05158(5) 0.0294(2) Uani 1 1 d . . . S2 S 0.00347(10) 0.40539(10) 0.10906(5) 0.0320(2) Uani 1 1 d . . . S3 S 0.24206(10) 0.57914(10) 0.01580(6) 0.0320(3) Uani 1 1 d . . . S4 S -0.01944(10) 0.54619(11) 0.38156(5) 0.0314(2) Uani 1 1 d . . . S5 S 0.03459(11) 0.72501(11) 0.53475(6) 0.0325(2) Uani 1 1 d . . . S6 S 0.23961(10) 0.54442(11) 0.50462(6) 0.0318(2) Uani 1 1 d . . . N11 N 0.0969(3) 0.6813(3) 0.16951(17) 0.0303(8) Uani 1 1 d . . . N12 N -0.0897(4) 0.6800(4) 0.16110(19) 0.0368(9) Uani 1 1 d . . . N21 N 0.2320(3) 0.5549(3) 0.16058(18) 0.0312(8) Uani 1 1 d . . . N22 N 0.2186(4) 0.3727(4) 0.1419(2) 0.0392(10) Uani 1 1 d . . . N31 N 0.2733(3) 0.7501(3) 0.10702(19) 0.0331(9) Uani 1 1 d . . . N32 N 0.3294(4) 0.8178(4) 0.0204(2) 0.0389(10) Uani 1 1 d . . . N71 N 0.2227(3) 0.6842(4) 0.38607(18) 0.0330(9) Uani 1 1 d . . . N72 N 0.1725(4) 0.5099(4) 0.34049(18) 0.0350(9) Uani 1 1 d . . . N81 N 0.1120(4) 0.8131(3) 0.42573(18) 0.0316(8) Uani 1 1 d . . . N82 N -0.0666(4) 0.8157(4) 0.43910(19) 0.0341(9) Uani 1 1 d . . . N91 N 0.2913(3) 0.7843(3) 0.49411(19) 0.0326(9) Uani 1 1 d . . . N92 N 0.3395(4) 0.7331(4) 0.58623(19) 0.0358(9) Uani 1 1 d . . . Cl Cl 0.60408(15) 0.87038(15) 0.28877(9) 0.0609(4) Uani 1 1 d . . . O1 O 0.7234(6) 0.9173(7) 0.2798(4) 0.134(3) Uani 1 1 d . . . O2 O 0.5367(9) 0.9169(12) 0.2527(8) 0.277(9) Uani 1 1 d . . . O3 O 0.5890(13) 0.8950(8) 0.3472(5) 0.236(7) Uani 1 1 d . . . O4 O 0.5562(6) 0.7478(5) 0.2808(3) 0.114(2) Uani 1 1 d . . . C11 C 0.0020(4) 0.6830(4) 0.1290(2) 0.0288(9) Uani 1 1 d . . . C12 C 0.0636(5) 0.6781(5) 0.2273(2) 0.0392(11) Uani 1 1 d . . . H12A H 0.1132 0.6769 0.2639 0.047 Uiso 1 1 calc R . . C13 C -0.0506(5) 0.6768(5) 0.2227(2) 0.0451(13) Uani 1 1 d . . . H13A H -0.0956 0.6741 0.2550 0.054 Uiso 1 1 calc R . . C21 C 0.1545(4) 0.4480(4) 0.1371(2) 0.0308(10) Uani 1 1 d . . . C22 C 0.3431(5) 0.5442(5) 0.1803(3) 0.0418(12) Uani 1 1 d . . . H22A H 0.4124 0.6053 0.1986 0.050 Uiso 1 1 calc R . . C23 C 0.3362(5) 0.4329(5) 0.1692(3) 0.0487(14) Uani 1 1 d . . . H23A H 0.3988 0.4016 0.1782 0.058 Uiso 1 1 calc R . . C31 C 0.2800(4) 0.7176(4) 0.0497(2) 0.0307(10) Uani 1 1 d . . . C32 C 0.3182(5) 0.8719(5) 0.1131(3) 0.0437(13) Uani 1 1 d . . . H32A H 0.3234 0.9173 0.1487 0.052 Uiso 1 1 calc R . . C33 C 0.3529(6) 0.9148(5) 0.0604(3) 0.0489(14) Uani 1 1 d . . . H33A H 0.3866 0.9946 0.0520 0.059 Uiso 1 1 calc R . . C41 C -0.2085(4) 0.6755(5) 0.1363(2) 0.0397(12) Uani 1 1 d . . . C42 C -0.2446(6) 0.7686(6) 0.1460(4) 0.068(2) Uani 1 1 d . . . H42A H -0.1923 0.8366 0.1688 0.082 Uiso 1 1 calc R . . C43 C -0.3638(8) 0.7604(9) 0.1208(5) 0.100(3) Uani 1 1 d . . . H43A H -0.3912 0.8239 0.1262 0.120 Uiso 1 1 calc R . . C44 C -0.4389(6) 0.6592(9) 0.0883(4) 0.083(3) Uani 1 1 d . . . H44A H -0.5177 0.6538 0.0714 0.100 Uiso 1 1 calc R . . C45 C -0.3999(6) 0.5662(8) 0.0805(3) 0.071(2) Uani 1 1 d . . . H45A H -0.4522 0.4975 0.0583 0.085 Uiso 1 1 calc R . . C46 C -0.2851(5) 0.5723(6) 0.1049(3) 0.0535(15) Uani 1 1 d . . . H46A H -0.2589 0.5078 0.1004 0.064 Uiso 1 1 calc R . . C51 C 0.1793(5) 0.2534(5) 0.1170(3) 0.0510(15) Uani 1 1 d . . . C52 C 0.2069(8) 0.2354(7) 0.0599(4) 0.077(2) Uani 1 1 d . . . H52A H 0.2475 0.2995 0.0377 0.093 Uiso 1 1 calc R . . C53 C 0.1737(11) 0.1218(9) 0.0360(5) 0.116(4) Uani 1 1 d . . . H53A H 0.1918 0.1084 -0.0029 0.140 Uiso 1 1 calc R . . C54 C 0.1171(9) 0.0310(8) 0.0667(7) 0.119(5) Uani 1 1 d . . . H54A H 0.0965 -0.0459 0.0497 0.143 Uiso 1 1 calc R . . C55 C 0.0886(11) 0.0474(9) 0.1219(9) 0.160(7) Uani 1 1 d . . . H55A H 0.0460 -0.0181 0.1426 0.192 Uiso 1 1 calc R . . C56 C 0.1221(10) 0.1638(7) 0.1501(6) 0.124(5) Uani 1 1 d . . . H56A H 0.1050 0.1764 0.1893 0.149 Uiso 1 1 calc R . . C61 C 0.3537(5) 0.8273(5) -0.0419(3) 0.0444(13) Uani 1 1 d . . . C62 C 0.4359(6) 0.7821(5) -0.0608(3) 0.0569(16) Uani 1 1 d . . . H62A H 0.4734 0.7406 -0.0341 0.068 Uiso 1 1 calc R . . C63 C 0.4629(8) 0.7989(6) -0.1201(4) 0.078(2) Uani 1 1 d . . . H63A H 0.5183 0.7678 -0.1340 0.094 Uiso 1 1 calc R . . C64 C 0.4085(9) 0.8610(7) -0.1585(4) 0.083(3) Uani 1 1 d . . . H64A H 0.4276 0.8726 -0.1984 0.099 Uiso 1 1 calc R . . C65 C 0.3276(8) 0.9057(7) -0.1395(4) 0.082(3) Uani 1 1 d . . . H65A H 0.2915 0.9486 -0.1661 0.098 Uiso 1 1 calc R . . C66 C 0.2976(6) 0.8875(6) -0.0795(3) 0.0638(18) Uani 1 1 d . . . H66A H 0.2402 0.9163 -0.0660 0.077 Uiso 1 1 calc R . . C71 C 0.1287(4) 0.5822(4) 0.3703(2) 0.0300(9) Uani 1 1 d . . . C72 C 0.3245(5) 0.6738(5) 0.3650(2) 0.0416(12) Uani 1 1 d . . . H72A H 0.4017 0.7321 0.3694 0.050 Uiso 1 1 calc R . . C73 C 0.2940(5) 0.5672(5) 0.3376(3) 0.0437(13) Uani 1 1 d . . . H73A H 0.3457 0.5367 0.3196 0.052 Uiso 1 1 calc R . . C81 C 0.0296(4) 0.7861(4) 0.4649(2) 0.0303(10) Uani 1 1 d . . . C82 C 0.0655(5) 0.8576(4) 0.3747(2) 0.0388(11) Uani 1 1 d . . . H82A H 0.1042 0.8823 0.3402 0.047 Uiso 1 1 calc R . . C83 C -0.0444(5) 0.8595(5) 0.3826(2) 0.0411(12) Uani 1 1 d . . . H83A H -0.0962 0.8856 0.3551 0.049 Uiso 1 1 calc R . . C91 C 0.2908(4) 0.6906(4) 0.5276(2) 0.0314(10) Uani 1 1 d . . . C92 C 0.3389(5) 0.8853(5) 0.5329(3) 0.0421(12) Uani 1 1 d . . . H92A H 0.3489 0.9625 0.5214 0.050 Uiso 1 1 calc R . . C93 C 0.3681(5) 0.8543(5) 0.5892(3) 0.0433(13) Uani 1 1 d . . . H93A H 0.4017 0.9051 0.6242 0.052 Uiso 1 1 calc R . . C101 C 0.1057(5) 0.3904(5) 0.3187(2) 0.0378(11) Uani 1 1 d . . . C102 C 0.0118(6) 0.3666(5) 0.2726(3) 0.0500(14) Uani 1 1 d . . . H10B H -0.0084 0.4283 0.2537 0.060 Uiso 1 1 calc R . . C103 C -0.0543(6) 0.2497(6) 0.2538(3) 0.0633(18) Uani 1 1 d . . . H10E H -0.1190 0.2324 0.2217 0.076 Uiso 1 1 calc R . . C104 C -0.0254(7) 0.1600(6) 0.2816(3) 0.0652(19) Uani 1 1 d . . . H10D H -0.0723 0.0813 0.2698 0.078 Uiso 1 1 calc R . . C105 C 0.0723(8) 0.1850(6) 0.3269(3) 0.069(2) Uani 1 1 d . . . H10C H 0.0943 0.1231 0.3444 0.082 Uiso 1 1 calc R . . C106 C 0.1385(6) 0.3004(6) 0.3468(3) 0.0544(15) Uani 1 1 d . . . H10A H 0.2039 0.3176 0.3785 0.065 Uiso 1 1 calc R . . C111 C -0.1744(5) 0.8020(5) 0.4657(3) 0.0381(11) Uani 1 1 d . . . C112 C -0.2803(5) 0.7159(6) 0.4415(3) 0.0563(16) Uani 1 1 d . . . H11E H -0.2823 0.6658 0.4084 0.068 Uiso 1 1 calc R . . C113 C -0.3851(6) 0.7043(7) 0.4672(4) 0.076(2) Uani 1 1 d . . . H11A H -0.4589 0.6466 0.4510 0.091 Uiso 1 1 calc R . . C114 C -0.3809(6) 0.7772(7) 0.5164(4) 0.066(2) Uani 1 1 d . . . H11B H -0.4514 0.7682 0.5339 0.079 Uiso 1 1 calc R . . C115 C -0.2743(6) 0.8625(6) 0.5396(3) 0.0574(16) Uani 1 1 d . . . H11D H -0.2720 0.9124 0.5729 0.069 Uiso 1 1 calc R . . C116 C -0.1698(5) 0.8758(5) 0.5145(3) 0.0466(13) Uani 1 1 d . . . H11C H -0.0965 0.9344 0.5305 0.056 Uiso 1 1 calc R . . C121 C 0.3508(4) 0.6637(5) 0.6377(2) 0.0381(11) Uani 1 1 d . . . C122 C 0.4135(5) 0.5862(6) 0.6372(3) 0.0475(13) Uani 1 1 d . . . H12F H 0.4530 0.5806 0.6037 0.057 Uiso 1 1 calc R . . C123 C 0.4180(5) 0.5171(6) 0.6862(3) 0.0573(16) Uani 1 1 d . . . H12D H 0.4582 0.4621 0.6854 0.069 Uiso 1 1 calc R . . C124 C 0.3639(5) 0.5278(6) 0.7366(3) 0.0592(17) Uani 1 1 d . . . H12B H 0.3679 0.4812 0.7702 0.071 Uiso 1 1 calc R . . C125 C 0.3039(6) 0.6077(7) 0.7370(3) 0.0620(18) Uani 1 1 d . . . H12E H 0.2678 0.6161 0.7714 0.074 Uiso 1 1 calc R . . C126 C 0.2962(5) 0.6756(6) 0.6876(3) 0.0498(14) Uani 1 1 d . . . H12C H 0.2543 0.7293 0.6880 0.060 Uiso 1 1 calc R . . B1 B 0.2238(5) 0.6799(5) 0.1623(3) 0.0314(11) Uani 1 1 d . . . H1A H 0.2781 0.7223 0.1992 0.038 Uiso 1 1 calc R . . B2 B 0.2356(5) 0.7938(5) 0.4276(3) 0.0327(11) Uani 1 1 d . . . H2A H 0.2918 0.8638 0.4110 0.039 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 Tl1 0.02616(13) 0.02673(13) 0.02623(14) -0.00081(9) -0.00079(9) 0.00528(9) Tl2 0.02595(13) 0.03102(14) 0.02710(14) 0.00497(10) 0.00577(9) 0.00696(10) S1 0.0328(6) 0.0296(6) 0.0259(6) 0.0006(4) 0.0022(4) 0.0114(5) S2 0.0298(5) 0.0324(6) 0.0298(6) 0.0045(5) -0.0011(5) 0.0072(5) S3 0.0280(5) 0.0289(6) 0.0353(6) -0.0050(5) 0.0023(5) 0.0058(4) S4 0.0269(5) 0.0397(6) 0.0266(6) 0.0035(5) 0.0043(4) 0.0098(5) S5 0.0346(6) 0.0352(6) 0.0294(6) 0.0035(5) 0.0069(5) 0.0131(5) S6 0.0275(5) 0.0333(6) 0.0338(6) 0.0019(5) 0.0032(5) 0.0097(5) N11 0.033(2) 0.032(2) 0.025(2) -0.0029(15) -0.0004(16) 0.0109(16) N12 0.034(2) 0.045(2) 0.031(2) -0.0008(18) 0.0047(17) 0.0135(19) N21 0.0291(19) 0.034(2) 0.028(2) -0.0025(16) -0.0048(16) 0.0100(16) N22 0.037(2) 0.035(2) 0.047(3) -0.0008(19) -0.0040(19) 0.0171(18) N31 0.0292(19) 0.029(2) 0.038(2) -0.0041(17) 0.0024(17) 0.0060(16) N32 0.038(2) 0.028(2) 0.045(3) -0.0042(18) 0.0078(19) 0.0021(17) N71 0.030(2) 0.040(2) 0.029(2) 0.0066(17) 0.0090(16) 0.0100(17) N72 0.036(2) 0.041(2) 0.029(2) 0.0011(17) 0.0084(17) 0.0135(18) N81 0.034(2) 0.030(2) 0.030(2) 0.0066(16) 0.0055(17) 0.0098(16) N82 0.034(2) 0.037(2) 0.032(2) 0.0038(17) 0.0043(17) 0.0124(17) N91 0.0280(19) 0.031(2) 0.035(2) 0.0007(17) 0.0021(17) 0.0066(16) N92 0.033(2) 0.040(2) 0.033(2) -0.0022(18) 0.0001(17) 0.0117(18) Cl 0.0562(9) 0.0533(9) 0.0685(11) 0.0143(8) 0.0123(8) 0.0110(7) O1 0.059(4) 0.145(7) 0.160(7) 0.018(5) 0.003(4) -0.009(4) O2 0.114(7) 0.301(15) 0.43(2) 0.273(15) 0.033(10) 0.083(8) O3 0.357(16) 0.100(6) 0.194(10) -0.061(6) 0.178(11) -0.044(8) O4 0.113(5) 0.071(4) 0.143(6) -0.020(4) 0.035(5) 0.005(4) C11 0.030(2) 0.025(2) 0.030(2) -0.0007(18) 0.0029(18) 0.0076(18) C12 0.044(3) 0.045(3) 0.027(3) 0.001(2) 0.001(2) 0.015(2) C13 0.047(3) 0.064(4) 0.025(3) 0.000(2) 0.008(2) 0.019(3) C21 0.033(2) 0.031(2) 0.028(2) 0.0026(18) 0.0009(19) 0.0121(19) C22 0.033(3) 0.049(3) 0.042(3) -0.006(2) -0.007(2) 0.016(2) C23 0.037(3) 0.049(3) 0.062(4) -0.006(3) -0.008(3) 0.022(2) C31 0.024(2) 0.029(2) 0.037(3) -0.0031(19) 0.0019(19) 0.0067(18) C32 0.048(3) 0.032(3) 0.046(3) -0.009(2) 0.005(3) 0.007(2) C33 0.060(4) 0.027(3) 0.053(4) -0.004(2) 0.009(3) 0.006(2) C41 0.030(2) 0.055(3) 0.037(3) 0.000(2) 0.008(2) 0.016(2) C42 0.046(3) 0.064(4) 0.096(6) -0.007(4) 0.005(4) 0.024(3) C43 0.066(5) 0.102(7) 0.157(10) 0.025(7) 0.030(6) 0.055(5) C44 0.037(3) 0.131(8) 0.080(6) 0.021(5) 0.008(4) 0.028(4) C45 0.036(3) 0.111(6) 0.054(4) -0.015(4) -0.002(3) 0.013(4) C46 0.043(3) 0.072(4) 0.044(3) -0.013(3) 0.003(3) 0.019(3) C51 0.041(3) 0.036(3) 0.078(5) 0.002(3) -0.002(3) 0.019(2) C52 0.119(7) 0.054(4) 0.061(5) -0.012(3) -0.019(5) 0.044(5) C53 0.177(11) 0.075(6) 0.101(7) -0.040(6) -0.053(7) 0.074(7) C54 0.078(6) 0.049(5) 0.216(14) -0.038(7) -0.043(7) 0.028(5) C55 0.127(10) 0.045(5) 0.32(2) 0.026(9) 0.112(12) 0.016(6) C56 0.146(9) 0.052(5) 0.200(12) 0.036(6) 0.114(9) 0.033(5) C61 0.046(3) 0.030(3) 0.044(3) 0.002(2) 0.007(2) -0.004(2) C62 0.071(4) 0.042(3) 0.058(4) 0.003(3) 0.028(3) 0.011(3) C63 0.107(6) 0.051(4) 0.073(5) -0.009(4) 0.044(5) 0.010(4) C64 0.120(7) 0.055(4) 0.046(4) -0.007(3) 0.020(5) -0.009(5) C65 0.098(6) 0.064(5) 0.051(4) 0.011(4) -0.008(4) -0.006(4) C66 0.062(4) 0.058(4) 0.061(4) 0.010(3) 0.002(3) 0.008(3) C71 0.031(2) 0.036(2) 0.024(2) 0.0065(18) 0.0069(18) 0.0121(19) C72 0.032(2) 0.051(3) 0.041(3) 0.007(2) 0.014(2) 0.010(2) C73 0.037(3) 0.055(3) 0.043(3) 0.002(3) 0.016(2) 0.017(2) C81 0.031(2) 0.030(2) 0.029(2) 0.0018(18) 0.0019(19) 0.0103(19) C82 0.043(3) 0.037(3) 0.035(3) 0.008(2) 0.004(2) 0.013(2) C83 0.048(3) 0.042(3) 0.035(3) 0.008(2) 0.000(2) 0.018(2) C91 0.020(2) 0.039(3) 0.033(3) -0.001(2) 0.0039(18) 0.0074(18) C92 0.039(3) 0.036(3) 0.045(3) -0.001(2) -0.003(2) 0.007(2) C93 0.043(3) 0.040(3) 0.042(3) -0.007(2) 0.001(2) 0.010(2) C101 0.042(3) 0.041(3) 0.032(3) 0.000(2) 0.012(2) 0.014(2) C102 0.054(3) 0.049(3) 0.044(3) -0.003(3) 0.002(3) 0.017(3) C103 0.059(4) 0.057(4) 0.065(4) -0.019(3) 0.004(3) 0.010(3) C104 0.083(5) 0.040(3) 0.065(5) -0.008(3) 0.026(4) 0.005(3) C105 0.107(6) 0.045(4) 0.057(4) 0.007(3) 0.016(4) 0.030(4) C106 0.069(4) 0.057(4) 0.043(3) 0.005(3) 0.003(3) 0.030(3) C111 0.033(2) 0.039(3) 0.046(3) 0.011(2) 0.006(2) 0.018(2) C112 0.036(3) 0.056(4) 0.072(4) -0.002(3) -0.002(3) 0.013(3) C113 0.031(3) 0.071(5) 0.117(7) 0.012(5) 0.002(4) 0.010(3) C114 0.043(3) 0.071(5) 0.099(6) 0.035(4) 0.030(4) 0.031(3) C115 0.062(4) 0.060(4) 0.064(4) 0.015(3) 0.027(3) 0.032(3) C116 0.045(3) 0.045(3) 0.053(4) 0.004(3) 0.013(3) 0.016(2) C121 0.029(2) 0.048(3) 0.031(3) 0.000(2) -0.001(2) 0.008(2) C122 0.038(3) 0.067(4) 0.039(3) 0.008(3) 0.003(2) 0.022(3) C123 0.044(3) 0.073(4) 0.056(4) 0.017(3) -0.002(3) 0.023(3) C124 0.044(3) 0.074(5) 0.046(4) 0.015(3) -0.006(3) 0.008(3) C125 0.055(4) 0.085(5) 0.032(3) -0.001(3) 0.006(3) 0.007(3) C126 0.050(3) 0.058(4) 0.039(3) -0.006(3) 0.005(3) 0.015(3) B1 0.028(2) 0.033(3) 0.029(3) -0.005(2) -0.006(2) 0.008(2) B2 0.029(3) 0.033(3) 0.034(3) 0.005(2) 0.008(2) 0.007(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 Tl1 S3 2.6736(11) 2_565 ? Tl1 S3 2.6736(11) . ? Tl1 S2 2.6763(12) . ? Tl1 S2 2.6763(12) 2_565 ? Tl1 S1 2.6949(11) . ? Tl1 S1 2.6949(11) 2_565 ? Tl2 S4 2.6789(12) 2_566 ? Tl2 S4 2.6789(12) . ? Tl2 S6 2.6934(11) 2_566 ? Tl2 S6 2.6934(11) . ? Tl2 S5 2.6991(12) . ? Tl2 S5 2.6991(12) 2_566 ? S1 C11 1.719(5) . ? S2 C21 1.715(5) . ? S3 C31 1.718(5) . ? S4 C71 1.712(5) . ? S5 C81 1.719(5) . ? S6 C91 1.711(5) . ? N11 C11 1.350(6) . ? N11 C12 1.383(6) . ? N11 B1 1.538(6) . ? N12 C11 1.365(6) . ? N12 C13 1.387(7) . ? N12 C41 1.426(6) . ? N21 C21 1.360(6) . ? N21 C22 1.382(6) . ? N21 B1 1.545(7) . ? N22 C21 1.364(6) . ? N22 C23 1.389(7) . ? N22 C51 1.438(7) . ? N31 C31 1.345(6) . ? N31 C32 1.384(6) . ? N31 B1 1.555(7) . ? N32 C31 1.362(6) . ? N32 C33 1.392(7) . ? N32 C61 1.442(7) . ? N71 C71 1.359(6) . ? N71 C72 1.391(6) . ? N71 B2 1.561(7) . ? N72 C71 1.362(6) . ? N72 C73 1.381(6) . ? N72 C101 1.436(7) . ? N81 C81 1.348(6) . ? N81 C82 1.383(6) . ? N81 B2 1.553(6) . ? N82 C81 1.364(6) . ? N82 C83 1.381(7) . ? N82 C111 1.434(6) . ? N91 C91 1.354(6) . ? N91 C92 1.393(7) . ? N91 B2 1.554(7) . ? N92 C91 1.371(6) . ? N92 C93 1.385(7) . ? N92 C121 1.436(7) . ? Cl O2 1.316(8) . ? Cl O3 1.373(8) . ? Cl O1 1.375(6) . ? Cl O4 1.396(6) . ? C12 C13 1.338(8) . ? C22 C23 1.338(8) . ? C32 C33 1.336(8) . ? C41 C42 1.355(8) . ? C41 C46 1.387(8) . ? C42 C43 1.420(10) . ? C43 C44 1.376(13) . ? C44 C45 1.368(11) . ? C45 C46 1.375(9) . ? C51 C56 1.345(10) . ? C51 C52 1.379(10) . ? C52 C53 1.375(11) . ? C53 C54 1.319(16) . ? C54 C55 1.340(18) . ? C55 C56 1.439(15) . ? C61 C66 1.360(9) . ? C61 C62 1.372(8) . ? C62 C63 1.391(9) . ? C63 C64 1.375(12) . ? C64 C65 1.355(12) . ? C65 C66 1.418(10) . ? C72 C73 1.333(8) . ? C82 C83 1.343(7) . ? C92 C93 1.339(8) . ? C101 C102 1.360(8) . ? C101 C106 1.396(8) . ? C102 C103 1.394(9) . ? C103 C104 1.368(10) . ? C104 C105 1.377(10) . ? C105 C106 1.385(9) . ? C111 C112 1.372(8) . ? C111 C116 1.381(8) . ? C112 C113 1.398(9) . ? C113 C114 1.381(11) . ? C114 C115 1.367(10) . ? C115 C116 1.383(8) . ? C121 C122 1.377(8) . ? C121 C126 1.381(8) . ? C122 C123 1.379(8) . ? C123 C124 1.381(9) . ? C124 C125 1.378(10) . ? C125 C126 1.381(9) . ? 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 Tl1 S3 180.0 2_565 . ? S3 Tl1 S2 90.45(4) 2_565 . ? S3 Tl1 S2 89.55(4) . . ? S3 Tl1 S2 89.55(4) 2_565 2_565 ? S3 Tl1 S2 90.45(4) . 2_565 ? S2 Tl1 S2 180.00(5) . 2_565 ? S3 Tl1 S1 87.95(3) 2_565 . ? S3 Tl1 S1 92.05(3) . . ? S2 Tl1 S1 90.61(4) . . ? S2 Tl1 S1 89.39(4) 2_565 . ? S3 Tl1 S1 92.05(3) 2_565 2_565 ? S3 Tl1 S1 87.95(3) . 2_565 ? S2 Tl1 S1 89.39(4) . 2_565 ? S2 Tl1 S1 90.61(4) 2_565 2_565 ? S1 Tl1 S1 180.00(4) . 2_565 ? S4 Tl2 S4 180.000(13) 2_566 . ? S4 Tl2 S6 91.15(4) 2_566 2_566 ? S4 Tl2 S6 88.85(4) . 2_566 ? S4 Tl2 S6 88.85(4) 2_566 . ? S4 Tl2 S6 91.15(4) . . ? S6 Tl2 S6 180.00(5) 2_566 . ? S4 Tl2 S5 87.91(4) 2_566 . ? S4 Tl2 S5 92.09(4) . . ? S6 Tl2 S5 87.88(4) 2_566 . ? S6 Tl2 S5 92.12(4) . . ? S4 Tl2 S5 92.09(4) 2_566 2_566 ? S4 Tl2 S5 87.91(4) . 2_566 ? S6 Tl2 S5 92.12(4) 2_566 2_566 ? S6 Tl2 S5 87.88(4) . 2_566 ? S5 Tl2 S5 180.0 . 2_566 ? C11 S1 Tl1 106.84(15) . . ? C21 S2 Tl1 103.90(17) . . ? C31 S3 Tl1 103.59(16) . . ? C71 S4 Tl2 99.85(16) . . ? C81 S5 Tl2 100.55(16) . . ? C91 S6 Tl2 99.00(15) . . ? C11 N11 C12 108.0(4) . . ? C11 N11 B1 132.9(4) . . ? C12 N11 B1 119.1(4) . . ? C11 N12 C13 108.7(4) . . ? C11 N12 C41 126.5(4) . . ? C13 N12 C41 124.8(4) . . ? C21 N21 C22 108.4(4) . . ? C21 N21 B1 133.7(4) . . ? C22 N21 B1 117.5(4) . . ? C21 N22 C23 109.3(4) . . ? C21 N22 C51 127.0(4) . . ? C23 N22 C51 123.3(4) . . ? C31 N31 C32 108.1(4) . . ? C31 N31 B1 133.2(4) . . ? C32 N31 B1 118.6(4) . . ? C31 N32 C33 108.9(4) . . ? C31 N32 C61 127.6(4) . . ? C33 N32 C61 123.5(4) . . ? C71 N71 C72 108.1(4) . . ? C71 N71 B2 131.7(4) . . ? C72 N71 B2 119.6(4) . . ? C71 N72 C73 109.1(4) . . ? C71 N72 C101 125.8(4) . . ? C73 N72 C101 125.0(4) . . ? C81 N81 C82 108.2(4) . . ? C81 N81 B2 131.6(4) . . ? C82 N81 B2 120.0(4) . . ? C81 N82 C83 108.9(4) . . ? C81 N82 C111 125.7(4) . . ? C83 N82 C111 125.3(4) . . ? C91 N91 C92 108.0(4) . . ? C91 N91 B2 132.2(4) . . ? C92 N91 B2 119.2(4) . . ? C91 N92 C93 108.9(4) . . ? C91 N92 C121 126.1(4) . . ? C93 N92 C121 124.8(4) . . ? O2 Cl O3 105.9(10) . . ? O2 Cl O1 110.7(6) . . ? O3 Cl O1 111.5(7) . . ? O2 Cl O4 109.4(8) . . ? O3 Cl O4 105.1(5) . . ? O1 Cl O4 113.8(5) . . ? N11 C11 N12 107.5(4) . . ? N11 C11 S1 129.4(4) . . ? N12 C11 S1 122.9(4) . . ? C13 C12 N11 108.9(5) . . ? C12 C13 N12 106.9(5) . . ? N21 C21 N22 106.7(4) . . ? N21 C21 S2 129.7(4) . . ? N22 C21 S2 123.5(4) . . ? C23 C22 N21 109.0(5) . . ? C22 C23 N22 106.6(5) . . ? N31 C31 N32 107.4(4) . . ? N31 C31 S3 129.7(4) . . ? N32 C31 S3 122.8(4) . . ? C33 C32 N31 109.1(5) . . ? C32 C33 N32 106.4(5) . . ? C42 C41 C46 122.3(6) . . ? C42 C41 N12 119.8(5) . . ? C46 C41 N12 117.8(5) . . ? C41 C42 C43 118.1(7) . . ? C44 C43 C42 119.7(8) . . ? C45 C44 C43 120.5(7) . . ? C44 C45 C46 120.6(7) . . ? C45 C46 C41 118.7(6) . . ? C56 C51 C52 122.3(7) . . ? C56 C51 N22 120.1(7) . . ? C52 C51 N22 117.6(6) . . ? C53 C52 C51 118.6(9) . . ? C54 C53 C52 121.3(11) . . ? C53 C54 C55 120.6(9) . . ? C54 C55 C56 121.0(10) . . ? C51 C56 C55 116.1(11) . . ? C66 C61 C62 122.1(6) . . ? C66 C61 N32 117.7(6) . . ? C62 C61 N32 120.2(6) . . ? C61 C62 C63 118.8(7) . . ? C64 C63 C62 120.0(8) . . ? C65 C64 C63 120.9(8) . . ? C64 C65 C66 119.7(8) . . ? C61 C66 C65 118.5(8) . . ? N71 C71 N72 106.9(4) . . ? N71 C71 S4 129.1(4) . . ? N72 C71 S4 124.0(4) . . ? C73 C72 N71 108.5(5) . . ? C72 C73 N72 107.4(4) . . ? N81 C81 N82 107.4(4) . . ? N81 C81 S5 129.7(4) . . ? N82 C81 S5 123.0(4) . . ? C83 C82 N81 108.7(5) . . ? C82 C83 N82 106.8(5) . . ? N91 C91 N92 107.2(4) . . ? N91 C91 S6 128.8(4) . . ? N92 C91 S6 124.0(4) . . ? C93 C92 N91 108.8(5) . . ? C92 C93 N92 107.0(5) . . ? C102 C101 C106 121.4(6) . . ? C102 C101 N72 120.3(5) . . ? C106 C101 N72 118.3(5) . . ? C101 C102 C103 119.2(6) . . ? C104 C103 C102 120.4(7) . . ? C103 C104 C105 120.0(6) . . ? C104 C105 C106 120.6(6) . . ? C105 C106 C101 118.3(6) . . ? C112 C111 C116 121.5(5) . . ? C112 C111 N82 118.9(5) . . ? C116 C111 N82 119.6(5) . . ? C111 C112 C113 118.5(7) . . ? C114 C113 C112 120.3(6) . . ? C115 C114 C113 120.2(6) . . ? C114 C115 C116 120.4(6) . . ? C111 C116 C115 119.2(6) . . ? C122 C121 C126 120.7(5) . . ? C122 C121 N92 121.0(5) . . ? C126 C121 N92 118.3(5) . . ? C121 C122 C123 119.5(6) . . ? C122 C123 C124 120.6(6) . . ? C125 C124 C123 119.2(6) . . ? C124 C125 C126 120.9(6) . . ? C121 C126 C125 119.1(6) . . ? N11 B1 N21 113.6(4) . . ? N11 B1 N31 111.7(4) . . ? N21 B1 N31 111.8(4) . . ? N81 B2 N91 111.5(4) . . ? N81 B2 N71 110.8(4) . . ? N91 B2 N71 111.7(4) . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 3.517 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.122 data_tls10 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H20 B N6 S2 Tl' _chemical_formula_weight 539.65 _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' 'B' 'B' 0.0013 0.0007 '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 7.6486(4) _cell_length_b 14.5166(7) _cell_length_c 16.9156(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.8220(10) _cell_angle_gamma 90.00 _cell_volume 1838.3(2) _cell_formula_units_Z 4 _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 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_method ? _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 9.019 _exptl_absorpt_correction_type SADABS _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 15768 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4226 _reflns_number_observed 3888 _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 2 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^)+(0.0274P)^2^+2.1748P] 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 0.00128(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4224 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_obs 0.0228 _refine_ls_wR_factor_all 0.0578 _refine_ls_wR_factor_obs 0.0557 _refine_ls_goodness_of_fit_all 1.021 _refine_ls_goodness_of_fit_obs 1.042 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.042 _refine_ls_shift/esd_max 0.129 _refine_ls_shift/esd_mean 0.002 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 0.29975(2) 0.704933(8) 0.082772(7) 0.02941(6) Uani 1 d . . C1 C 0.4704(5) 0.6502(3) 0.0077(2) 0.0421(9) Uani 1 d . . H1A H 0.4492(29) 0.6829(14) -0.0433(7) 0.063 Uiso 1 calc R . H1B H 0.4446(28) 0.5853(6) -0.0020(15) 0.063 Uiso 1 calc R . H1C H 0.5943(6) 0.6576(19) 0.0347(8) 0.063 Uiso 1 calc R . C2 C 0.1789(6) 0.7168(3) 0.1866(2) 0.0400(9) Uani 1 d . . H2A H 0.0502(6) 0.7202(19) 0.1691(2) 0.060 Uiso 1 calc R . H2B H 0.2221(28) 0.7721(10) 0.2164(9) 0.060 Uiso 1 calc R . H2C H 0.2101(30) 0.6634(9) 0.2211(8) 0.060 Uiso 1 calc R . S1 S -0.01994(12) 0.68524(6) -0.02564(6) 0.0347(2) Uani 1 d . . S2 S 0.34526(11) 0.88865(5) 0.06016(5) 0.0283(2) Uani 1 d . . N11 N 0.0932(4) 0.7509(2) -0.16108(15) 0.0253(5) Uani 1 d . . N12 N 0.0538(4) 0.6018(2) -0.1586(2) 0.0321(6) Uani 1 d . . N21 N 0.3362(3) 0.8640(2) -0.10318(15) 0.0233(5) Uani 1 d . . N22 N 0.6048(3) 0.8741(2) -0.0279(2) 0.0263(5) Uani 1 d . . N31 N 0.0595(3) 0.9210(2) -0.2011(2) 0.0262(5) Uani 1 d . . N32 N 0.1083(4) 0.9186(2) -0.2751(2) 0.0316(6) Uani 1 d . . C11 C 0.0462(4) 0.6809(2) -0.1163(2) 0.0262(6) Uani 1 d . . C12 C 0.1270(5) 0.7137(2) -0.2311(2) 0.0344(8) Uani 1 d . . H12A H 0.1615(5) 0.7471(2) -0.2730(2) 0.041 Uiso 1 calc R . C13 C 0.1029(5) 0.6219(2) -0.2302(2) 0.0367(8) Uani 1 d . . H13A H 0.1170(5) 0.5798(2) -0.2707(2) 0.044 Uiso 1 calc R . C14 C 0.0216(6) 0.5098(2) -0.1305(3) 0.0459(9) Uani 1 d . . H14A H 0.0568(38) 0.4643(3) -0.1662(11) 0.069 Uiso 1 calc R . H14B H -0.1043(9) 0.5027(8) -0.1302(18) 0.069 Uiso 1 calc R . H14C H 0.0911(32) 0.5010(8) -0.0762(7) 0.069 Uiso 1 calc R . C21 C 0.4272(4) 0.8760(2) -0.0263(2) 0.0222(6) Uani 1 d . . C22 C 0.4599(4) 0.8542(2) -0.1522(2) 0.0292(7) Uani 1 d . . H22A H 0.4329(4) 0.8449(2) -0.2084(2) 0.035 Uiso 1 calc R . C23 C 0.6248(4) 0.8602(2) -0.1059(2) 0.0302(7) Uani 1 d . . H23A H 0.7333(4) 0.8557(2) -0.1236(2) 0.036 Uiso 1 calc R . C24 C 0.7506(4) 0.8868(3) 0.0415(2) 0.0379(8) Uani 1 d . . H24A H 0.7314(19) 0.8476(14) 0.0854(6) 0.057 Uiso 1 calc R . H24B H 0.7547(23) 0.9507(5) 0.0585(10) 0.057 Uiso 1 calc R . H24C H 0.8627(6) 0.8704(18) 0.0268(5) 0.057 Uiso 1 calc R . C31 C -0.0463(4) 0.9950(2) -0.1969(2) 0.0334(7) Uani 1 d . . H31A H -0.0961(4) 1.0114(2) -0.1524(2) 0.040 Uiso 1 calc R . C32 C -0.0682(5) 1.0418(3) -0.2690(2) 0.0418(9) Uani 1 d . . H32B H -0.1344(5) 1.0959(3) -0.2839(2) 0.050 Uiso 1 calc R . C33 C 0.0292(5) 0.9915(2) -0.3147(2) 0.0377(8) Uani 1 d . . H33A H 0.0383(5) 1.0072(2) -0.3677(2) 0.045 Uiso 1 calc R . B B 0.1295(4) 0.8532(2) -0.1319(2) 0.0229(6) Uani 1 d . . H1 H 0.0663(46) 0.8680(24) -0.0861(21) 0.025(9) 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 0.03584(9) 0.02999(8) 0.02476(9) 0.00368(5) 0.01171(6) 0.00326(5) C1 0.050(2) 0.038(2) 0.043(2) 0.003(2) 0.021(2) 0.012(2) C2 0.049(2) 0.044(2) 0.031(2) 0.000(2) 0.019(2) -0.004(2) S1 0.0326(4) 0.0399(4) 0.0341(5) 0.0047(4) 0.0122(4) -0.0050(3) S2 0.0382(4) 0.0291(4) 0.0188(3) -0.0021(3) 0.0085(3) 0.0005(3) N11 0.0265(12) 0.0274(13) 0.0198(12) 0.0013(11) -0.0005(10) 0.0013(10) N12 0.0321(14) 0.0279(14) 0.0323(15) 0.0002(12) -0.0027(12) -0.0009(11) N21 0.0226(12) 0.0294(13) 0.0182(12) 0.0003(10) 0.0046(10) -0.0012(10) N22 0.0236(12) 0.0298(13) 0.0240(13) 0.0014(11) 0.0016(10) -0.0012(10) N31 0.0254(12) 0.0276(13) 0.0243(13) 0.0003(11) 0.0020(10) 0.0007(10) N32 0.042(2) 0.0314(14) 0.0205(13) 0.0028(11) 0.0055(12) -0.0002(12) C11 0.0200(14) 0.0306(15) 0.025(2) 0.0012(13) -0.0030(12) -0.0029(12) C12 0.046(2) 0.033(2) 0.022(2) -0.0029(13) -0.0004(15) 0.0052(14) C13 0.046(2) 0.031(2) 0.029(2) -0.0039(15) -0.0009(15) 0.004(2) C14 0.048(2) 0.029(2) 0.058(3) 0.005(2) 0.004(2) -0.003(2) C21 0.0237(13) 0.0224(13) 0.0194(13) 0.0011(12) 0.0017(11) -0.0016(11) C22 0.0266(15) 0.043(2) 0.0194(14) 0.0009(13) 0.0075(12) 0.0009(13) C23 0.0234(15) 0.039(2) 0.030(2) 0.0007(14) 0.0101(13) -0.0005(13) C24 0.029(2) 0.045(2) 0.035(2) -0.006(2) -0.0056(14) -0.0019(15) C31 0.028(2) 0.031(2) 0.038(2) -0.0037(15) -0.0008(14) 0.0032(13) C32 0.044(2) 0.030(2) 0.044(2) 0.004(2) -0.008(2) 0.0037(15) C33 0.048(2) 0.033(2) 0.027(2) 0.0059(14) -0.0040(15) -0.008(2) B 0.022(2) 0.028(2) 0.0183(15) 0.0012(13) 0.0025(13) 0.0017(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl C1 2.150(3) . ? Tl C2 2.152(3) . ? Tl S2 2.7266(8) . ? Tl S1 2.7543(10) . ? S1 C11 1.712(3) . ? S2 C21 1.715(3) . ? N11 C11 1.360(4) . ? N11 C12 1.373(4) . ? N11 B 1.572(4) . ? N12 C11 1.360(4) . ? N12 C13 1.370(5) . ? N12 C14 1.456(4) . ? N21 C21 1.355(4) . ? N21 C22 1.387(4) . ? N21 B 1.564(4) . ? N22 C21 1.364(4) . ? N22 C23 1.374(4) . ? N22 C24 1.456(4) . ? N31 C31 1.355(4) . ? N31 N32 1.377(4) . ? N31 B 1.539(4) . ? N32 C33 1.331(4) . ? C12 C13 1.346(5) . ? C22 C23 1.344(5) . ? C31 C32 1.377(5) . ? C32 C33 1.386(6) . ? 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 Tl C2 157.7(2) . . ? C1 Tl S2 99.69(11) . . ? C2 Tl S2 97.17(10) . . ? C1 Tl S1 97.59(12) . . ? C2 Tl S1 94.62(12) . . ? S2 Tl S1 97.44(3) . . ? C11 S1 Tl 102.43(10) . . ? C21 S2 Tl 95.43(10) . . ? C11 N11 C12 107.7(3) . . ? C11 N11 B 125.6(3) . . ? C12 N11 B 126.2(3) . . ? C11 N12 C13 109.6(3) . . ? C11 N12 C14 125.0(3) . . ? C13 N12 C14 125.4(3) . . ? C21 N21 C22 107.9(2) . . ? C21 N21 B 126.8(2) . . ? C22 N21 B 125.0(3) . . ? C21 N22 C23 109.3(3) . . ? C21 N22 C24 125.6(3) . . ? C23 N22 C24 125.1(3) . . ? C31 N31 N32 110.1(3) . . ? C31 N31 B 125.8(3) . . ? N32 N31 B 123.9(2) . . ? C33 N32 N31 105.0(3) . . ? N11 C11 N12 107.1(3) . . ? N11 C11 S1 129.2(3) . . ? N12 C11 S1 123.7(2) . . ? C13 C12 N11 109.2(3) . . ? C12 C13 N12 106.4(3) . . ? N21 C21 N22 107.2(2) . . ? N21 C21 S2 128.8(2) . . ? N22 C21 S2 124.0(2) . . ? C23 C22 N21 108.6(3) . . ? C22 C23 N22 107.0(3) . . ? N31 C31 C32 108.0(3) . . ? C31 C32 C33 104.6(3) . . ? N32 C33 C32 112.2(3) . . ? N31 B N21 110.2(2) . . ? N31 B N11 110.7(2) . . ? N21 B N11 107.1(2) . . ? _refine_diff_density_max 1.215 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.104 data_tls10-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H45 B2 Cl3 N12 S6 Tl2' _chemical_formula_weight 1603.10 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' 'Cl' 'Cl' 0.1484 0.1585 '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 10.3343(9) _cell_length_b 10.6394(10) _cell_length_c 14.8014(14) _cell_angle_alpha 103.389(2) _cell_angle_beta 95.630(2) _cell_angle_gamma 100.605(2) _cell_volume 1539.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 778 _exptl_absorpt_coefficient_mu 5.609 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4000 _exptl_absorpt_correction_T_max 0.6039 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11080 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.34 _reflns_number_total 6814 _reflns_number_gt 4612 _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^)+(0.0156P)^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 0.00000(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6814 _refine_ls_number_parameters 384 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 2.345 _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 Tl Tl 1.63305(2) 0.87722(2) 0.506828(16) 0.05147(10) Uani 1 1 d . . . S1 S 1.73748(12) 0.97639(13) 0.74221(9) 0.0514(4) Uani 1 1 d . . . S2 S 1.40817(12) 1.30868(11) 0.69964(9) 0.0439(3) Uani 1 1 d . . . S3 S 1.33014(14) 0.82194(12) 0.48805(9) 0.0523(3) Uani 1 1 d . . . N11 N 1.5182(3) 1.0596(3) 0.7996(2) 0.0335(9) Uani 1 1 d . . . N12 N 1.6910(4) 1.1183(4) 0.9100(3) 0.0419(10) Uani 1 1 d . . . N21 N 1.3014(3) 1.0577(3) 0.7070(2) 0.0325(9) Uani 1 1 d . . . N22 N 1.1611(3) 1.1883(3) 0.7251(3) 0.0340(9) Uani 1 1 d . . . N31 N 1.3970(3) 0.8547(3) 0.6766(3) 0.0320(8) Uani 1 1 d . . . N32 N 1.3281(3) 0.6484(3) 0.5976(3) 0.0376(9) Uani 1 1 d . . . Cl1 Cl 2.4204(3) 1.3740(3) 1.1204(3) 0.0870(10) Uani 0.50 1 d P A -1 Cl2 Cl 2.2640(3) 1.5501(3) 1.0677(2) 0.0782(9) Uani 0.50 1 d P A -1 Cl3 Cl 2.5024(18) 1.5133(17) 0.9842(8) 0.095(2) Uani 0.50 1 d P A -1 C1 C 2.4240(10) 1.5218(10) 1.0871(8) 0.059(3) Uani 0.50 1 d P A -1 H1A H 2.4778 1.5956 1.1382 0.071 Uiso 0.50 1 calc PR A -1 C11 C 1.6489(4) 1.0550(4) 0.8184(3) 0.0334(11) Uani 1 1 d . . . C12 C 1.4809(5) 1.1245(5) 0.8819(4) 0.0477(13) Uani 1 1 d . . . H12A H 1.3959 1.1415 0.8890 0.057 Uiso 1 1 calc R . . C13 C 1.5853(5) 1.1588(5) 0.9493(4) 0.0529(14) Uani 1 1 d . . . H13A H 1.5866 1.2027 1.0124 0.063 Uiso 1 1 calc R . . C21 C 1.2894(4) 1.1841(4) 0.7117(3) 0.0331(10) Uani 1 1 d . . . C22 C 1.1820(4) 0.9851(4) 0.7163(3) 0.0417(12) Uani 1 1 d . . . H22A H 1.1639 0.8948 0.7152 0.050 Uiso 1 1 calc R . . C23 C 1.0954(4) 1.0647(4) 0.7273(3) 0.0461(13) Uani 1 1 d . . . H23A H 1.0058 1.0405 0.7350 0.055 Uiso 1 1 calc R . . C31 C 1.3530(4) 0.7756(4) 0.5902(3) 0.0351(11) Uani 1 1 d . . . C32 C 1.4009(5) 0.7750(5) 0.7386(4) 0.0469(13) Uani 1 1 d . . . H32A H 1.4289 0.8050 0.8037 0.056 Uiso 1 1 calc R . . C33 C 1.3584(5) 0.6489(4) 0.6905(3) 0.0451(12) Uani 1 1 d . . . H33A H 1.3505 0.5746 0.7152 0.054 Uiso 1 1 calc R . . C41 C 1.8215(5) 1.1412(4) 0.9597(3) 0.0408(12) Uani 1 1 d . . . C42 C 1.9272(5) 1.2112(5) 0.9295(4) 0.0552(14) Uani 1 1 d . . . H42A H 1.9140 1.2412 0.8750 0.066 Uiso 1 1 calc R . . C43 C 2.0529(5) 1.2365(5) 0.9801(4) 0.0621(15) Uani 1 1 d . . . H43A H 2.1257 1.2835 0.9596 0.075 Uiso 1 1 calc R . . C44 C 2.0728(6) 1.1941(5) 1.0598(4) 0.0600(15) Uani 1 1 d . . . H44A H 2.1588 1.2114 1.0935 0.072 Uiso 1 1 calc R . . C45 C 1.9678(6) 1.1267(5) 1.0902(4) 0.0568(14) Uani 1 1 d . . . H45A H 1.9813 1.0980 1.1452 0.068 Uiso 1 1 calc R . . C46 C 1.8415(5) 1.1006(5) 1.0405(3) 0.0509(13) Uani 1 1 d . . . H46A H 1.7690 1.0548 1.0620 0.061 Uiso 1 1 calc R . . C51 C 1.1012(4) 1.3021(4) 0.7395(3) 0.0348(11) Uani 1 1 d . . . C52 C 0.9776(5) 1.2886(5) 0.6894(3) 0.0454(12) Uani 1 1 d . . . H52A H 0.9367 1.2093 0.6447 0.054 Uiso 1 1 calc R . . C53 C 0.9148(5) 1.3942(5) 0.7065(4) 0.0578(15) Uani 1 1 d . . . H53A H 0.8301 1.3866 0.6735 0.069 Uiso 1 1 calc R . . C54 C 0.9761(6) 1.5106(5) 0.7717(4) 0.0610(15) Uani 1 1 d . . . H54A H 0.9336 1.5824 0.7826 0.073 Uiso 1 1 calc R . . C55 C 1.0993(5) 1.5213(5) 0.8205(4) 0.0536(14) Uani 1 1 d . . . H55A H 1.1410 1.6009 0.8645 0.064 Uiso 1 1 calc R . . C56 C 1.1624(4) 1.4169(4) 0.8057(3) 0.0420(12) Uani 1 1 d . . . H56A H 1.2459 1.4238 0.8402 0.050 Uiso 1 1 calc R . . C61 C 1.2711(5) 0.5315(4) 0.5237(3) 0.0387(11) Uani 1 1 d . . . C62 C 1.1549(5) 0.4525(5) 0.5340(4) 0.0510(13) Uani 1 1 d . . . H62A H 1.1137 0.4762 0.5874 0.061 Uiso 1 1 calc R . . C63 C 1.0993(6) 0.3374(5) 0.4646(5) 0.0690(17) Uani 1 1 d . . . H63A H 1.0196 0.2831 0.4708 0.083 Uiso 1 1 calc R . . C64 C 1.1601(6) 0.3029(5) 0.3873(4) 0.0597(15) Uani 1 1 d . . . H64A H 1.1207 0.2259 0.3399 0.072 Uiso 1 1 calc R . . C65 C 1.2771(6) 0.3789(5) 0.3784(4) 0.0600(15) Uani 1 1 d . . . H65A H 1.3193 0.3530 0.3258 0.072 Uiso 1 1 calc R . . C66 C 1.3346(5) 0.4959(5) 0.4475(4) 0.0483(13) Uani 1 1 d . . . H66A H 1.4153 0.5489 0.4418 0.058 Uiso 1 1 calc R . . B B 1.4338(5) 1.0081(5) 0.7015(4) 0.0330(13) Uani 1 1 d . . . H1 H 1.482(3) 1.041(3) 0.648(2) 0.023(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 Tl 0.05903(15) 0.05032(14) 0.05377(15) 0.02404(10) 0.01163(10) 0.01811(10) S1 0.0376(7) 0.0647(9) 0.0466(9) -0.0055(7) 0.0085(6) 0.0214(7) S2 0.0431(7) 0.0330(7) 0.0605(9) 0.0185(6) 0.0168(6) 0.0074(6) S3 0.0710(10) 0.0390(7) 0.0453(9) 0.0179(6) -0.0012(7) 0.0042(7) N11 0.034(2) 0.033(2) 0.035(2) 0.0063(18) 0.0114(18) 0.0114(17) N12 0.039(2) 0.053(3) 0.035(3) 0.007(2) 0.008(2) 0.019(2) N21 0.028(2) 0.0211(19) 0.051(3) 0.0122(18) 0.0095(18) 0.0053(16) N22 0.032(2) 0.0228(19) 0.051(3) 0.0113(18) 0.0078(18) 0.0096(17) N31 0.039(2) 0.028(2) 0.034(2) 0.0132(19) 0.0109(18) 0.0103(17) N32 0.048(2) 0.023(2) 0.042(3) 0.0098(19) 0.0018(19) 0.0065(17) Cl1 0.087(2) 0.071(2) 0.107(3) 0.032(2) -0.006(2) 0.0260(18) Cl2 0.0575(19) 0.0581(18) 0.118(3) 0.0170(18) 0.0080(18) 0.0201(15) Cl3 0.103(2) 0.124(6) 0.070(7) 0.022(4) 0.040(5) 0.050(4) C1 0.045(6) 0.053(7) 0.071(8) 0.005(6) -0.016(6) 0.012(5) C11 0.032(3) 0.033(3) 0.036(3) 0.009(2) 0.009(2) 0.007(2) C12 0.045(3) 0.062(3) 0.046(3) 0.015(3) 0.021(3) 0.028(3) C13 0.058(4) 0.071(4) 0.033(3) 0.004(3) 0.016(3) 0.031(3) C21 0.031(3) 0.032(2) 0.037(3) 0.009(2) 0.005(2) 0.009(2) C22 0.035(3) 0.030(3) 0.065(4) 0.017(2) 0.018(2) 0.009(2) C23 0.033(3) 0.034(3) 0.071(4) 0.014(3) 0.014(3) 0.003(2) C31 0.034(3) 0.033(3) 0.042(3) 0.012(2) 0.011(2) 0.011(2) C32 0.062(3) 0.045(3) 0.043(3) 0.023(3) 0.014(3) 0.021(3) C33 0.065(3) 0.033(3) 0.044(3) 0.018(2) 0.009(3) 0.016(2) C41 0.047(3) 0.046(3) 0.030(3) 0.004(2) 0.007(2) 0.017(2) C42 0.056(4) 0.073(4) 0.045(4) 0.027(3) 0.006(3) 0.021(3) C43 0.052(4) 0.080(4) 0.055(4) 0.021(3) 0.007(3) 0.011(3) C44 0.063(4) 0.066(4) 0.043(4) 0.000(3) -0.009(3) 0.021(3) C45 0.081(4) 0.050(3) 0.042(3) 0.014(3) -0.002(3) 0.023(3) C46 0.066(4) 0.051(3) 0.036(3) 0.010(3) 0.003(3) 0.015(3) C51 0.039(3) 0.034(3) 0.036(3) 0.010(2) 0.011(2) 0.015(2) C52 0.040(3) 0.044(3) 0.051(3) 0.007(3) 0.003(3) 0.013(2) C53 0.060(4) 0.058(4) 0.062(4) 0.011(3) 0.000(3) 0.040(3) C54 0.074(4) 0.050(3) 0.063(4) 0.003(3) 0.004(3) 0.041(3) C55 0.070(4) 0.036(3) 0.050(4) -0.002(3) 0.002(3) 0.019(3) C56 0.041(3) 0.041(3) 0.041(3) 0.002(2) 0.000(2) 0.014(2) C61 0.045(3) 0.031(3) 0.045(3) 0.013(2) 0.003(2) 0.016(2) C62 0.055(3) 0.037(3) 0.059(4) 0.008(3) 0.013(3) 0.008(3) C63 0.063(4) 0.037(3) 0.101(5) 0.013(3) -0.003(4) 0.008(3) C64 0.060(4) 0.041(3) 0.069(4) -0.003(3) -0.016(3) 0.020(3) C65 0.074(4) 0.049(3) 0.058(4) 0.003(3) 0.004(3) 0.032(3) C66 0.047(3) 0.047(3) 0.056(4) 0.015(3) 0.007(3) 0.021(3) B 0.038(3) 0.032(3) 0.038(3) 0.018(3) 0.017(3) 0.013(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 S3 3.0493(14) . ? Tl H1 3.13(3) . ? Tl S3 3.1351(12) 2_876 ? Tl S1 3.3995(14) . ? Tl B 3.853(5) . ? Tl S2 5.8120(12) . ? S1 C11 1.690(4) . ? S2 C21 1.688(4) . ? S3 C31 1.704(5) . ? S3 Tl 3.1351(12) 2_876 ? N11 C11 1.364(5) . ? N11 C12 1.382(5) . ? N11 B 1.541(6) . ? N12 C11 1.355(5) . ? N12 C13 1.378(5) . ? N12 C41 1.421(6) . ? N21 C21 1.360(5) . ? N21 C22 1.368(5) . ? N21 B 1.558(5) . ? N22 C21 1.368(5) . ? N22 C23 1.373(5) . ? N22 C51 1.441(5) . ? N31 C31 1.340(5) . ? N31 C32 1.388(5) . ? N31 B 1.552(6) . ? N32 C31 1.362(5) . ? N32 C33 1.379(5) . ? N32 C61 1.437(5) . ? Cl1 C1 1.748(10) . ? Cl2 C1 1.743(10) . ? Cl3 C1 1.786(14) . ? C12 C13 1.330(6) . ? C22 C23 1.337(5) . ? C32 C33 1.334(6) . ? C41 C46 1.372(6) . ? C41 C42 1.378(6) . ? C42 C43 1.382(7) . ? C43 C44 1.368(7) . ? C44 C45 1.361(7) . ? C45 C46 1.381(7) . ? C51 C56 1.375(6) . ? C51 C52 1.378(6) . ? C52 C53 1.384(6) . ? C53 C54 1.380(7) . ? C54 C55 1.372(7) . ? C55 C56 1.374(6) . ? C61 C66 1.374(6) . ? C61 C62 1.376(6) . ? C62 C63 1.388(7) . ? C63 C64 1.367(7) . ? C64 C65 1.362(7) . ? C65 C66 1.403(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 S3 Tl H1 57.6(6) . . ? S3 Tl S3 95.76(3) . 2_876 ? H1 Tl S3 64.2(6) . 2_876 ? S3 Tl S1 104.53(3) . . ? H1 Tl S1 57.0(6) . . ? S3 Tl S1 86.75(3) 2_876 . ? S3 Tl B 55.14(9) . . ? H1 Tl B 12.8(6) . . ? S3 Tl B 76.81(7) 2_876 . ? S1 Tl B 52.45(8) . . ? S3 Tl S2 64.35(3) . . ? H1 Tl S2 19.2(6) . . ? S3 Tl S2 45.43(3) 2_876 . ? S1 Tl S2 66.40(2) . . ? B Tl S2 32.02(7) . . ? C11 S1 Tl 122.40(17) . . ? C21 S2 Tl 83.09(13) . . ? C31 S3 Tl 84.67(14) . . ? C31 S3 Tl 119.73(16) . 2_876 ? Tl S3 Tl 84.24(3) . 2_876 ? C11 N11 C12 107.7(4) . . ? C11 N11 B 124.5(3) . . ? C12 N11 B 127.7(4) . . ? C11 N12 C13 108.7(4) . . ? C11 N12 C41 127.0(3) . . ? C13 N12 C41 124.3(4) . . ? C21 N21 C22 109.1(3) . . ? C21 N21 B 124.9(3) . . ? C22 N21 B 125.7(3) . . ? C21 N22 C23 109.0(3) . . ? C21 N22 C51 127.4(3) . . ? C23 N22 C51 123.5(3) . . ? C31 N31 C32 107.8(4) . . ? C31 N31 B 125.4(4) . . ? C32 N31 B 126.8(4) . . ? C31 N32 C33 108.7(4) . . ? C31 N32 C61 127.0(4) . . ? C33 N32 C61 124.1(4) . . ? Cl1 C1 Cl2 110.9(6) . . ? Cl1 C1 Cl3 108.6(7) . . ? Cl2 C1 Cl3 111.2(8) . . ? N12 C11 N11 107.3(3) . . ? N12 C11 S1 127.0(3) . . ? N11 C11 S1 125.7(3) . . ? C13 C12 N11 108.7(4) . . ? C12 C13 N12 107.7(4) . . ? N21 C21 N22 106.1(3) . . ? N21 C21 S2 126.6(3) . . ? N22 C21 S2 127.3(3) . . ? C23 C22 N21 108.2(4) . . ? C22 C23 N22 107.6(4) . . ? N31 C31 N32 107.7(4) . . ? N31 C31 S3 127.3(3) . . ? N32 C31 S3 124.9(4) . . ? C33 C32 N31 108.7(4) . . ? C32 C33 N32 107.0(4) . . ? C46 C41 C42 119.9(5) . . ? C46 C41 N12 120.3(4) . . ? C42 C41 N12 119.7(4) . . ? C41 C42 C43 119.2(5) . . ? C44 C43 C42 120.7(5) . . ? C45 C44 C43 119.9(5) . . ? C44 C45 C46 120.1(5) . . ? C41 C46 C45 120.1(5) . . ? C56 C51 C52 121.7(4) . . ? C56 C51 N22 120.5(4) . . ? C52 C51 N22 117.7(4) . . ? C51 C52 C53 118.6(5) . . ? C54 C53 C52 120.3(5) . . ? C55 C54 C53 119.8(4) . . ? C54 C55 C56 120.8(5) . . ? C55 C56 C51 118.8(4) . . ? C66 C61 C62 121.0(5) . . ? C66 C61 N32 120.8(4) . . ? C62 C61 N32 118.1(4) . . ? C61 C62 C63 119.3(5) . . ? C64 C63 C62 120.1(5) . . ? C65 C64 C63 120.6(5) . . ? C64 C65 C66 120.1(5) . . ? C61 C66 C65 118.8(5) . . ? N11 B N31 109.1(4) . . ? N11 B N21 107.8(3) . . ? N31 B N21 107.2(3) . . ? N11 B Tl 113.3(2) . . ? N31 B Tl 72.2(2) . . ? N21 B Tl 136.6(3) . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 0.621 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.100