# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name G.Parkin D.Buccella J.G.Melnick K.Yurkerwich _publ_contact_author_name 'G. Parkin' _publ_contact_author_email PARKIN@COLUMBIA.EDU data_ky11s10 _database_code_depnum_ccdc_archive 'CCDC 680244' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H46 B2 F15 In N6 S3' _chemical_formula_weight 1260.56 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' F F 0.0171 0.0103 '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' In In -0.7276 1.3100 '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 12.1353(6) _cell_length_b 12.5348(6) _cell_length_c 20.0186(10) _cell_angle_alpha 81.9890(10) _cell_angle_beta 77.8270(10) _cell_angle_gamma 70.8120(10) _cell_volume 2803.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 6411 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 28.24 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8349 _exptl_absorpt_correction_T_max 0.8854 _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 18618 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 26.37 _reflns_number_total 11342 _reflns_number_gt 9894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11342 _refine_ls_number_parameters 708 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0935 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_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_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 In In 0.028929(11) -0.165540(12) -0.239663(7) 0.03311(6) Uani 1 1 d . . . S1 S 0.04003(4) -0.00934(4) -0.33757(3) 0.03733(12) Uani 1 1 d . . . S2 S -0.17820(4) -0.05812(5) -0.18055(3) 0.03771(12) Uani 1 1 d . . . S3 S -0.03661(5) -0.29064(5) -0.30466(3) 0.03902(12) Uani 1 1 d . . . B1 B -0.2331(2) -0.0315(2) -0.34523(14) 0.0428(6) Uani 1 1 d D . . H1 H -0.3096(18) 0.006(2) -0.3780(12) 0.058(7) Uiso 1 1 d D . . B2 B 0.1864(2) -0.2470(2) -0.17702(13) 0.0361(5) Uani 1 1 d . . . C11 C -0.10117(17) 0.08619(17) -0.31815(10) 0.0363(4) Uani 1 1 d . . . N11 N -0.20255(15) 0.07084(15) -0.32619(9) 0.0393(4) Uani 1 1 d . . . N12 N -0.12794(16) 0.18943(16) -0.29418(10) 0.0430(4) Uani 1 1 d . . . C12 C -0.29491(19) 0.1658(2) -0.30510(13) 0.0494(6) Uani 1 1 d . . . H12A H -0.3756 0.1775 -0.3048 0.059 Uiso 1 1 calc R . . C13 C -0.2504(2) 0.2383(2) -0.28516(14) 0.0516(6) Uani 1 1 d . . . H13A H -0.2939 0.3091 -0.2682 0.062 Uiso 1 1 calc R . . C14 C -0.0456(2) 0.2433(2) -0.27483(13) 0.0509(6) Uani 1 1 d . . . C15 C -0.1169(3) 0.3620(3) -0.2525(2) 0.0797(9) Uani 1 1 d . . . H15A H -0.1517 0.4083 -0.2903 0.119 Uiso 1 1 calc R . . H15B H -0.0650 0.3962 -0.2387 0.119 Uiso 1 1 calc R . . H15C H -0.1794 0.3568 -0.2141 0.119 Uiso 1 1 calc R . . C16 C 0.0496(3) 0.2538(3) -0.33649(15) 0.0640(7) Uani 1 1 d . . . H16A H 0.0956 0.1790 -0.3512 0.096 Uiso 1 1 calc R . . H16B H 0.1015 0.2892 -0.3238 0.096 Uiso 1 1 calc R . . H16C H 0.0123 0.2997 -0.3736 0.096 Uiso 1 1 calc R . . C17 C 0.0093(3) 0.1712(3) -0.21512(14) 0.0646(7) Uani 1 1 d . . . H17A H 0.0553 0.0961 -0.2292 0.097 Uiso 1 1 calc R . . H17B H -0.0531 0.1655 -0.1769 0.097 Uiso 1 1 calc R . . H17C H 0.0606 0.2062 -0.2013 0.097 Uiso 1 1 calc R . . C21 C -0.26414(16) -0.11456(18) -0.21502(11) 0.0372(4) Uani 1 1 d . . . N21 N -0.28229(14) -0.09720(16) -0.28042(10) 0.0401(4) Uani 1 1 d . . . N22 N -0.32706(15) -0.18327(16) -0.18008(10) 0.0434(4) Uani 1 1 d . . . C22 C -0.35555(19) -0.1582(2) -0.28643(13) 0.0492(6) Uani 1 1 d . . . H22A H -0.3816 -0.1624 -0.3267 0.059 Uiso 1 1 calc R . . C23 C -0.3830(2) -0.2100(2) -0.22570(14) 0.0524(6) Uani 1 1 d . . . H23A H -0.4320 -0.2568 -0.2155 0.063 Uiso 1 1 calc R . . C24 C -0.3330(2) -0.2282(2) -0.10545(13) 0.0528(6) Uani 1 1 d . . . C25 C -0.2097(2) -0.3069(3) -0.09609(16) 0.0680(8) Uani 1 1 d . . . H25A H -0.1537 -0.2642 -0.1066 0.102 Uiso 1 1 calc R . . H25B H -0.1850 -0.3673 -0.1267 0.102 Uiso 1 1 calc R . . H25C H -0.2124 -0.3391 -0.0490 0.102 Uiso 1 1 calc R . . C26 C -0.3772(3) -0.1308(3) -0.05916(15) 0.0706(8) Uani 1 1 d . . . H26A H -0.3223 -0.0868 -0.0691 0.106 Uiso 1 1 calc R . . H26B H -0.3825 -0.1607 -0.0116 0.106 Uiso 1 1 calc R . . H26C H -0.4548 -0.0827 -0.0672 0.106 Uiso 1 1 calc R . . C27 C -0.4197(3) -0.2973(3) -0.08893(18) 0.0803(10) Uani 1 1 d . . . H27A H -0.3917 -0.3602 -0.1179 0.120 Uiso 1 1 calc R . . H27B H -0.4973 -0.2493 -0.0972 0.120 Uiso 1 1 calc R . . H27C H -0.4253 -0.3261 -0.0412 0.120 Uiso 1 1 calc R . . N31 N -0.12933(16) -0.11004(16) -0.39299(9) 0.0407(4) Uani 1 1 d . . . C31 C -0.04575(19) -0.21009(19) -0.38182(11) 0.0389(5) Uani 1 1 d . . . N32 N 0.02848(17) -0.23795(18) -0.44261(9) 0.0464(4) Uani 1 1 d . . . C32 C -0.1063(2) -0.0758(2) -0.46221(12) 0.0520(6) Uani 1 1 d . . . H32A H -0.1509 -0.0092 -0.4842 0.062 Uiso 1 1 calc R . . C33 C -0.0104(2) -0.1530(2) -0.49216(12) 0.0543(6) Uani 1 1 d . . . H33A H 0.0246 -0.1501 -0.5387 0.065 Uiso 1 1 calc R . . C34 C 0.1362(2) -0.3415(2) -0.45544(13) 0.0570(6) Uani 1 1 d . . . C35 C 0.0966(3) -0.4465(3) -0.4399(2) 0.0850(10) Uani 1 1 d . . . H35A H 0.0601 -0.4514 -0.3920 0.127 Uiso 1 1 calc R . . H35B H 0.1647 -0.5131 -0.4492 0.127 Uiso 1 1 calc R . . H35C H 0.0396 -0.4420 -0.4684 0.127 Uiso 1 1 calc R . . C36 C 0.1942(3) -0.3316(4) -0.53156(16) 0.0908(11) Uani 1 1 d . . . H36A H 0.1389 -0.3308 -0.5604 0.136 Uiso 1 1 calc R . . H36B H 0.2651 -0.3958 -0.5408 0.136 Uiso 1 1 calc R . . H36C H 0.2151 -0.2620 -0.5414 0.136 Uiso 1 1 calc R . . C37 C 0.2253(2) -0.3418(3) -0.41243(16) 0.0712(8) Uani 1 1 d . . . H37A H 0.1911 -0.3480 -0.3642 0.107 Uiso 1 1 calc R . . H37B H 0.2457 -0.2720 -0.4232 0.107 Uiso 1 1 calc R . . H37C H 0.2962 -0.4058 -0.4224 0.107 Uiso 1 1 calc R . . C41 C 0.25049(17) -0.36937(17) -0.20863(11) 0.0361(4) Uani 1 1 d . . . F41 F 0.07278(11) -0.41805(12) -0.17930(7) 0.0492(3) Uani 1 1 d . . . C42 C 0.18842(18) -0.44507(19) -0.20978(11) 0.0399(5) Uani 1 1 d . . . F42 F 0.16703(16) -0.61206(14) -0.23947(10) 0.0758(5) Uani 1 1 d . . . F43 F 0.39845(18) -0.67445(14) -0.30428(11) 0.0878(6) Uani 1 1 d . . . C43 C 0.2345(2) -0.5453(2) -0.24076(14) 0.0512(6) Uani 1 1 d . . . F44 F 0.53342(13) -0.54031(15) -0.30278(10) 0.0792(5) Uani 1 1 d . . . C44 C 0.3508(2) -0.5771(2) -0.27310(14) 0.0568(6) Uani 1 1 d . . . C45 C 0.4176(2) -0.5084(2) -0.27264(14) 0.0519(6) Uani 1 1 d . . . F45 F 0.44429(11) -0.34991(12) -0.24082(9) 0.0605(4) Uani 1 1 d . . . C46 C 0.36866(18) -0.40903(19) -0.24054(12) 0.0433(5) Uani 1 1 d . . . C51 C 0.11407(18) -0.24930(19) -0.09913(11) 0.0395(5) Uani 1 1 d . . . F52 F 0.02060(12) -0.05129(11) -0.11056(7) 0.0498(3) Uani 1 1 d . . . C52 C 0.0317(2) -0.15130(19) -0.07266(12) 0.0434(5) Uani 1 1 d . . . F53 F -0.12275(15) -0.04919(15) 0.00946(9) 0.0757(5) Uani 1 1 d . . . C53 C -0.0433(2) -0.1476(2) -0.01056(13) 0.0544(6) Uani 1 1 d . . . F54 F -0.11356(17) -0.24546(19) 0.09050(8) 0.0885(6) Uani 1 1 d . . . C54 C -0.0382(2) -0.2458(3) 0.03048(12) 0.0607(7) Uani 1 1 d . . . F55 F 0.05196(19) -0.44123(17) 0.04949(9) 0.0887(6) Uani 1 1 d . . . C55 C 0.0435(3) -0.3449(2) 0.00910(13) 0.0590(7) Uani 1 1 d . . . F56 F 0.19917(14) -0.44656(13) -0.06909(8) 0.0651(4) Uani 1 1 d . . . C56 C 0.1185(2) -0.3446(2) -0.05367(12) 0.0492(5) Uani 1 1 d . . . C61 C 0.25983(17) -0.15628(18) -0.19691(12) 0.0406(5) Uani 1 1 d . . . F61 F 0.26460(13) -0.13069(14) -0.08206(9) 0.0654(4) Uani 1 1 d . . . C62 C 0.2858(2) -0.1003(2) -0.14969(15) 0.0519(6) Uani 1 1 d . . . F63 F 0.4177(2) 0.10080(18) -0.25422(17) 0.1266(10) Uani 1 1 d . . . C63 C 0.3359(2) -0.0135(2) -0.1679(2) 0.0706(9) Uani 1 1 d . . . F64 F 0.37790(17) -0.00777(19) -0.35203(12) 0.1021(7) Uani 1 1 d . . . C64 C 0.3653(3) 0.0187(2) -0.2356(2) 0.0810(11) Uani 1 1 d . . . C65 C 0.3461(2) -0.0362(3) -0.28512(19) 0.0707(9) Uani 1 1 d . . . C66 C 0.29546(18) -0.1210(2) -0.26470(14) 0.0490(6) Uani 1 1 d . . . F66 F 0.28060(12) -0.17387(14) -0.31557(7) 0.0569(4) Uani 1 1 d . . . F67 F 0.35802(17) 0.03700(17) -0.11935(14) 0.1052(8) Uani 1 1 d . . . C101 C 0.6973(8) -0.2261(8) -0.5106(4) 0.188(4) Uani 1 1 d . . . H10C H 0.7483 -0.1856 -0.5345 0.225 Uiso 1 1 calc R . . C102 C 0.7195(6) -0.2852(7) -0.4531(4) 0.163(3) Uani 1 1 d . . . H10B H 0.7862 -0.2867 -0.4357 0.195 Uiso 1 1 calc R . . C103 C 0.6454(5) -0.3458(5) -0.4174(3) 0.1301(18) Uani 1 1 d . . . H10A H 0.6596 -0.3862 -0.3753 0.156 Uiso 1 1 calc R . . C104 C 0.5559(5) -0.3457(8) -0.4436(4) 0.207(4) Uani 1 1 d . . . H10D H 0.5071 -0.3890 -0.4206 0.248 Uiso 1 1 calc R . . C105 C 0.5313(8) -0.2857(11) -0.5021(6) 0.324(9) Uani 1 1 d . . . H10F H 0.4660 -0.2868 -0.5200 0.389 Uiso 1 1 calc R . . C106 C 0.6015(10) -0.2230(10) -0.5356(5) 0.265(6) Uani 1 1 d . . . H10E H 0.5834 -0.1779 -0.5759 0.318 Uiso 1 1 calc R . . C201 C 0.4824(4) -0.6566(6) -0.1139(2) 0.1148(17) Uani 1 1 d . . . H20D H 0.4101 -0.6331 -0.1300 0.138 Uiso 1 1 calc R . . C202 C 0.5534(6) -0.7744(5) -0.1118(2) 0.121(2) Uani 1 1 d . . . H20F H 0.5308 -0.8301 -0.1275 0.145 Uiso 1 1 calc R . . C203 C 0.6572(4) -0.8010(3) -0.0853(2) 0.0996(13) Uani 1 1 d . . . H20E H 0.7062 -0.8767 -0.0829 0.119 Uiso 1 1 calc R . . C204 C 0.6887(4) -0.7215(4) -0.0632(2) 0.0908(11) Uani 1 1 d . . . H20B H 0.7579 -0.7421 -0.0441 0.109 Uiso 1 1 calc R . . C205 C 0.6232(4) -0.6137(4) -0.0680(2) 0.0949(11) Uani 1 1 d . . . H20C H 0.6491 -0.5588 -0.0541 0.114 Uiso 1 1 calc R . . C206 C 0.5223(4) -0.5810(4) -0.0920(2) 0.0994(12) Uani 1 1 d . . . H20A H 0.4777 -0.5038 -0.0939 0.119 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 In 0.03129(9) 0.03480(9) 0.03431(9) -0.00006(6) -0.01055(6) -0.00973(6) S1 0.0338(2) 0.0372(3) 0.0404(3) 0.0028(2) -0.0078(2) -0.0119(2) S2 0.0342(2) 0.0404(3) 0.0403(3) -0.0055(2) -0.0054(2) -0.0138(2) S3 0.0473(3) 0.0372(3) 0.0362(3) -0.0004(2) -0.0117(2) -0.0161(2) B1 0.0404(12) 0.0449(14) 0.0484(14) 0.0039(11) -0.0193(11) -0.0160(11) B2 0.0350(10) 0.0315(12) 0.0442(13) -0.0018(10) -0.0143(9) -0.0093(9) C11 0.0372(10) 0.0342(11) 0.0362(11) 0.0032(8) -0.0071(8) -0.0111(8) N11 0.0356(8) 0.0377(10) 0.0446(10) 0.0031(8) -0.0132(7) -0.0099(7) N12 0.0430(9) 0.0371(10) 0.0489(11) 0.0016(8) -0.0111(8) -0.0127(8) C12 0.0365(10) 0.0443(13) 0.0623(15) 0.0032(11) -0.0116(10) -0.0067(10) C13 0.0450(12) 0.0381(12) 0.0647(16) -0.0053(11) -0.0087(11) -0.0035(10) C14 0.0594(14) 0.0444(13) 0.0565(14) -0.0058(11) -0.0140(11) -0.0231(11) C15 0.084(2) 0.0522(18) 0.113(3) -0.0210(17) -0.0217(19) -0.0269(16) C16 0.0725(17) 0.0652(18) 0.0685(17) -0.0003(14) -0.0108(14) -0.0431(15) C17 0.0806(18) 0.0686(19) 0.0567(16) -0.0045(13) -0.0259(14) -0.0307(15) C21 0.0299(9) 0.0352(11) 0.0460(12) -0.0017(9) -0.0063(8) -0.0101(8) N21 0.0322(8) 0.0445(10) 0.0480(10) -0.0025(8) -0.0106(7) -0.0159(8) N22 0.0343(8) 0.0416(10) 0.0551(11) -0.0007(9) -0.0052(8) -0.0157(8) C22 0.0396(11) 0.0550(15) 0.0621(15) -0.0075(12) -0.0148(10) -0.0220(11) C23 0.0402(11) 0.0542(15) 0.0716(17) -0.0028(12) -0.0114(11) -0.0260(11) C24 0.0498(13) 0.0517(14) 0.0543(14) 0.0101(11) -0.0035(11) -0.0216(11) C25 0.0624(16) 0.0614(18) 0.0734(19) 0.0201(14) -0.0184(14) -0.0163(14) C26 0.0767(19) 0.073(2) 0.0538(16) -0.0014(14) 0.0105(14) -0.0266(16) C27 0.0739(19) 0.083(2) 0.090(2) 0.0228(18) -0.0079(17) -0.0484(18) N31 0.0470(9) 0.0445(10) 0.0370(9) 0.0024(8) -0.0154(8) -0.0199(8) C31 0.0458(11) 0.0434(12) 0.0357(11) -0.0021(9) -0.0135(9) -0.0212(9) N32 0.0543(11) 0.0539(12) 0.0342(10) -0.0065(8) -0.0093(8) -0.0189(9) C32 0.0679(15) 0.0546(15) 0.0392(12) 0.0068(11) -0.0215(11) -0.0234(13) C33 0.0704(16) 0.0616(16) 0.0341(12) 0.0010(11) -0.0111(11) -0.0255(13) C34 0.0611(14) 0.0595(16) 0.0452(14) -0.0144(12) -0.0032(11) -0.0116(12) C35 0.096(2) 0.0600(19) 0.098(3) -0.0341(18) -0.005(2) -0.0194(17) C36 0.087(2) 0.115(3) 0.0500(17) -0.0203(18) 0.0039(16) -0.009(2) C37 0.0529(14) 0.089(2) 0.0637(18) -0.0124(16) -0.0104(13) -0.0085(15) C41 0.0376(10) 0.0325(10) 0.0398(11) 0.0003(8) -0.0146(8) -0.0095(8) F41 0.0429(6) 0.0504(8) 0.0586(8) 0.0033(6) -0.0108(6) -0.0222(6) C42 0.0407(10) 0.0362(11) 0.0452(12) 0.0043(9) -0.0159(9) -0.0131(9) F42 0.0936(12) 0.0503(9) 0.1028(13) -0.0098(9) -0.0283(10) -0.0396(9) F43 0.1061(14) 0.0444(9) 0.1042(14) -0.0314(9) -0.0090(11) -0.0072(9) C43 0.0643(15) 0.0357(12) 0.0626(15) -0.0013(11) -0.0239(12) -0.0208(11) F44 0.0507(8) 0.0589(10) 0.1044(14) -0.0141(9) 0.0064(8) 0.0055(7) C44 0.0707(16) 0.0336(12) 0.0613(16) -0.0105(11) -0.0154(13) -0.0045(11) C45 0.0437(12) 0.0412(13) 0.0604(15) -0.0042(11) -0.0075(11) -0.0003(10) F45 0.0336(6) 0.0498(8) 0.1007(11) -0.0085(8) -0.0146(7) -0.0134(6) C46 0.0381(10) 0.0368(12) 0.0561(14) -0.0012(10) -0.0149(10) -0.0098(9) C51 0.0410(10) 0.0401(12) 0.0408(11) -0.0030(9) -0.0172(9) -0.0109(9) F52 0.0573(8) 0.0375(7) 0.0557(8) -0.0075(6) -0.0181(6) -0.0094(6) C52 0.0491(12) 0.0421(12) 0.0424(12) -0.0053(9) -0.0183(10) -0.0115(10) F53 0.0760(10) 0.0741(11) 0.0648(10) -0.0304(9) -0.0022(8) -0.0033(9) C53 0.0548(13) 0.0620(16) 0.0460(13) -0.0183(12) -0.0117(11) -0.0100(12) F54 0.0940(13) 0.1213(17) 0.0413(9) -0.0080(9) 0.0051(8) -0.0313(12) C54 0.0654(15) 0.081(2) 0.0347(12) -0.0058(12) -0.0092(11) -0.0211(15) F55 0.1131(15) 0.0823(13) 0.0561(10) 0.0272(9) -0.0136(10) -0.0250(11) C55 0.0717(16) 0.0621(17) 0.0406(13) 0.0103(12) -0.0165(12) -0.0190(14) F56 0.0753(10) 0.0450(8) 0.0589(9) 0.0074(7) -0.0173(7) 0.0015(7) C56 0.0557(13) 0.0459(13) 0.0441(13) 0.0013(10) -0.0182(10) -0.0094(11) C61 0.0316(9) 0.0300(10) 0.0614(14) -0.0025(9) -0.0159(9) -0.0067(8) F61 0.0616(9) 0.0719(10) 0.0730(11) -0.0288(8) -0.0245(8) -0.0173(8) C62 0.0373(11) 0.0412(13) 0.0805(19) -0.0137(12) -0.0190(11) -0.0078(10) F63 0.0888(14) 0.0612(12) 0.241(3) 0.0147(15) -0.0264(17) -0.0507(11) C63 0.0472(13) 0.0414(14) 0.132(3) -0.0243(17) -0.0253(16) -0.0125(12) F64 0.0766(12) 0.1010(15) 0.1200(17) 0.0489(13) -0.0089(11) -0.0441(11) C64 0.0498(15) 0.0397(15) 0.157(4) 0.0032(19) -0.0201(19) -0.0221(12) C65 0.0427(13) 0.0529(16) 0.109(3) 0.0248(17) -0.0138(14) -0.0175(12) C66 0.0321(10) 0.0424(13) 0.0704(16) 0.0069(11) -0.0157(10) -0.0092(9) F66 0.0467(7) 0.0699(10) 0.0502(8) 0.0055(7) -0.0077(6) -0.0173(7) F67 0.0766(11) 0.0768(13) 0.188(2) -0.0589(14) -0.0376(13) -0.0292(10) C101 0.212(8) 0.250(9) 0.146(6) -0.094(7) 0.090(6) -0.175(8) C102 0.134(4) 0.227(8) 0.168(6) -0.133(6) 0.035(5) -0.102(5) C103 0.132(4) 0.140(5) 0.130(4) -0.044(4) -0.008(3) -0.052(4) C104 0.108(4) 0.288(10) 0.222(8) 0.133(7) -0.047(5) -0.107(5) C105 0.203(8) 0.457(18) 0.350(14) 0.267(14) -0.140(9) -0.216(11) C106 0.279(12) 0.332(14) 0.225(10) 0.137(9) -0.056(8) -0.204(11) C201 0.115(3) 0.175(5) 0.068(2) 0.044(3) -0.039(2) -0.070(4) C202 0.198(6) 0.151(5) 0.056(2) -0.022(3) 0.006(3) -0.122(5) C203 0.121(3) 0.071(2) 0.090(3) -0.025(2) 0.018(2) -0.022(2) C204 0.091(2) 0.092(3) 0.085(2) -0.003(2) -0.0055(19) -0.030(2) C205 0.120(3) 0.078(3) 0.091(3) 0.006(2) -0.017(2) -0.042(2) C206 0.114(3) 0.070(2) 0.103(3) 0.023(2) -0.022(2) -0.024(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 In B2 2.374(2) . ? In S2 2.5488(5) . ? In S3 2.5709(5) . ? In S1 2.5856(5) . ? S1 C11 1.738(2) . ? S2 C21 1.729(2) . ? S3 C31 1.727(2) . ? B1 H1 1.181(16) . ? B1 N31 1.552(3) . ? B1 N21 1.554(3) . ? B1 N11 1.562(3) . ? B2 C51 1.622(3) . ? B2 C61 1.624(3) . ? B2 C41 1.624(3) . ? C11 N11 1.351(3) . ? C11 N12 1.357(3) . ? N11 C12 1.384(3) . ? N12 C13 1.391(3) . ? N12 C14 1.512(3) . ? C12 C13 1.338(4) . ? C14 C16 1.526(4) . ? C14 C17 1.526(4) . ? C14 C15 1.530(4) . ? C21 N21 1.349(3) . ? C21 N22 1.361(3) . ? N21 C22 1.381(3) . ? N22 C23 1.379(3) . ? N22 C24 1.517(3) . ? C22 C23 1.327(4) . ? C24 C26 1.521(4) . ? C24 C25 1.530(4) . ? C24 C27 1.530(4) . ? N31 C31 1.354(3) . ? N31 C32 1.390(3) . ? C31 N32 1.365(3) . ? N32 C33 1.383(3) . ? N32 C34 1.515(3) . ? C32 C33 1.333(4) . ? C34 C35 1.516(4) . ? C34 C37 1.517(4) . ? C34 C36 1.545(4) . ? C41 C46 1.395(3) . ? C41 C42 1.397(3) . ? F41 C42 1.357(2) . ? C42 C43 1.373(3) . ? F42 C43 1.344(3) . ? F43 C44 1.345(3) . ? C43 C44 1.374(4) . ? F44 C45 1.356(3) . ? C44 C45 1.366(4) . ? C45 C46 1.376(3) . ? F45 C46 1.355(3) . ? C51 C56 1.391(3) . ? C51 C52 1.393(3) . ? F52 C52 1.354(3) . ? C52 C53 1.374(3) . ? F53 C53 1.344(3) . ? C53 C54 1.372(4) . ? F54 C54 1.348(3) . ? C54 C55 1.367(4) . ? F55 C55 1.343(3) . ? C55 C56 1.388(4) . ? F56 C56 1.359(3) . ? C61 C66 1.391(3) . ? C61 C62 1.394(3) . ? F61 C62 1.348(3) . ? C62 C63 1.384(4) . ? F63 C64 1.352(3) . ? C63 F67 1.346(4) . ? C63 C64 1.364(5) . ? F64 C65 1.345(4) . ? C64 C65 1.379(5) . ? C65 C66 1.371(4) . ? C66 F66 1.361(3) . ? C101 C102 1.308(11) . ? C101 C106 1.347(12) . ? C102 C103 1.386(8) . ? C103 C104 1.301(8) . ? C104 C105 1.335(9) . ? C105 C106 1.359(10) . ? C201 C206 1.354(7) . ? C201 C202 1.445(7) . ? C202 C203 1.391(7) . ? C203 C204 1.334(6) . ? C204 C205 1.325(6) . ? C205 C206 1.327(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 B2 In S2 121.10(6) . . ? B2 In S3 120.43(6) . . ? S2 In S3 96.307(17) . . ? B2 In S1 120.85(6) . . ? S2 In S1 94.803(17) . . ? S3 In S1 97.288(18) . . ? C11 S1 In 100.26(7) . . ? C21 S2 In 100.92(7) . . ? C31 S3 In 99.75(7) . . ? H1 B1 N31 105.0(13) . . ? H1 B1 N21 107.1(13) . . ? N31 B1 N21 112.76(19) . . ? H1 B1 N11 106.9(13) . . ? N31 B1 N11 112.94(18) . . ? N21 B1 N11 111.59(19) . . ? C51 B2 C61 116.06(18) . . ? C51 B2 C41 115.84(18) . . ? C61 B2 C41 116.02(18) . . ? C51 B2 In 101.30(13) . . ? C61 B2 In 101.81(13) . . ? C41 B2 In 102.09(13) . . ? N11 C11 N12 108.60(18) . . ? N11 C11 S1 125.38(16) . . ? N12 C11 S1 126.00(16) . . ? C11 N11 C12 107.49(18) . . ? C11 N11 B1 133.73(18) . . ? C12 N11 B1 118.36(18) . . ? C11 N12 C13 107.74(19) . . ? C11 N12 C14 128.53(18) . . ? C13 N12 C14 123.6(2) . . ? C13 C12 N11 108.7(2) . . ? C12 C13 N12 107.4(2) . . ? N12 C14 C16 110.0(2) . . ? N12 C14 C17 108.7(2) . . ? C16 C14 C17 111.3(2) . . ? N12 C14 C15 109.1(2) . . ? C16 C14 C15 108.6(2) . . ? C17 C14 C15 109.2(2) . . ? N21 C21 N22 108.10(18) . . ? N21 C21 S2 126.38(16) . . ? N22 C21 S2 125.51(17) . . ? C21 N21 C22 107.67(19) . . ? C21 N21 B1 133.21(18) . . ? C22 N21 B1 119.02(19) . . ? C21 N22 C23 107.61(19) . . ? C21 N22 C24 127.64(19) . . ? C23 N22 C24 124.71(19) . . ? C23 C22 N21 108.5(2) . . ? C22 C23 N22 108.1(2) . . ? N22 C24 C26 110.4(2) . . ? N22 C24 C25 108.1(2) . . ? C26 C24 C25 112.3(3) . . ? N22 C24 C27 108.3(2) . . ? C26 C24 C27 108.9(2) . . ? C25 C24 C27 108.6(2) . . ? C31 N31 C32 107.47(19) . . ? C31 N31 B1 133.34(18) . . ? C32 N31 B1 119.11(19) . . ? N31 C31 N32 108.15(19) . . ? N31 C31 S3 126.06(17) . . ? N32 C31 S3 125.77(18) . . ? C31 N32 C33 107.9(2) . . ? C31 N32 C34 127.4(2) . . ? C33 N32 C34 124.7(2) . . ? C33 C32 N31 108.6(2) . . ? C32 C33 N32 107.9(2) . . ? N32 C34 C35 108.9(2) . . ? N32 C34 C37 109.3(2) . . ? C35 C34 C37 112.7(3) . . ? N32 C34 C36 107.8(2) . . ? C35 C34 C36 110.4(3) . . ? C37 C34 C36 107.7(3) . . ? C46 C41 C42 112.2(2) . . ? C46 C41 B2 125.54(19) . . ? C42 C41 B2 122.13(18) . . ? F41 C42 C43 116.4(2) . . ? F41 C42 C41 118.5(2) . . ? C43 C42 C41 125.1(2) . . ? F42 C43 C44 120.1(2) . . ? F42 C43 C42 120.6(2) . . ? C44 C43 C42 119.3(2) . . ? F43 C44 C45 120.5(2) . . ? F43 C44 C43 120.8(3) . . ? C45 C44 C43 118.8(2) . . ? F44 C45 C44 119.3(2) . . ? F44 C45 C46 120.3(2) . . ? C44 C45 C46 120.3(2) . . ? F45 C46 C45 115.3(2) . . ? F45 C46 C41 120.5(2) . . ? C45 C46 C41 124.2(2) . . ? C56 C51 C52 112.6(2) . . ? C56 C51 B2 126.3(2) . . ? C52 C51 B2 120.94(19) . . ? F52 C52 C53 116.1(2) . . ? F52 C52 C51 119.0(2) . . ? C53 C52 C51 124.9(2) . . ? F53 C53 C54 120.0(2) . . ? F53 C53 C52 120.5(2) . . ? C54 C53 C52 119.5(2) . . ? F54 C54 C55 120.2(3) . . ? F54 C54 C53 120.8(3) . . ? C55 C54 C53 119.0(2) . . ? F55 C55 C54 119.8(2) . . ? F55 C55 C56 120.6(3) . . ? C54 C55 C56 119.6(2) . . ? F56 C56 C55 115.0(2) . . ? F56 C56 C51 120.7(2) . . ? C55 C56 C51 124.2(2) . . ? C66 C61 C62 113.4(2) . . ? C66 C61 B2 121.7(2) . . ? C62 C61 B2 124.7(2) . . ? F61 C62 C63 115.9(3) . . ? F61 C62 C61 120.5(2) . . ? C63 C62 C61 123.6(3) . . ? F67 C63 C64 120.2(3) . . ? F67 C63 C62 120.2(3) . . ? C64 C63 C62 119.6(3) . . ? F63 C64 C63 120.2(4) . . ? F63 C64 C65 119.8(4) . . ? C63 C64 C65 119.9(3) . . ? F64 C65 C66 120.8(3) . . ? F64 C65 C64 120.6(3) . . ? C66 C65 C64 118.6(3) . . ? F66 C66 C65 116.3(3) . . ? F66 C66 C61 118.8(2) . . ? C65 C66 C61 124.9(3) . . ? C102 C101 C106 120.2(7) . . ? C101 C102 C103 120.5(7) . . ? C104 C103 C102 118.6(7) . . ? C103 C104 C105 121.9(7) . . ? C104 C105 C106 119.4(9) . . ? C101 C106 C105 119.3(9) . . ? C206 C201 C202 118.4(4) . . ? C203 C202 C201 116.3(4) . . ? C204 C203 C202 121.5(4) . . ? C205 C204 C203 120.5(4) . . ? C204 C205 C206 122.0(4) . . ? C205 C206 C201 121.2(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.692 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.059 # Attachment 'TmInS4_-_KY.cif' data_ky _database_code_depnum_ccdc_archive 'CCDC 680245' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H34 B In N6 S7' _chemical_formula_weight 720.59 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' In In -0.7276 1.3100 '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)/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 11.6446(6) _cell_length_b 16.4002(9) _cell_length_c 16.1622(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.0260(10) _cell_angle_gamma 90.00 _cell_volume 3084.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 5004 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.24 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7862 _exptl_absorpt_correction_T_max 0.9281 _exptl_absorpt_process_details sadabs _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 21665 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.33 _reflns_number_total 7135 _reflns_number_gt 5470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7135 _refine_ls_number_parameters 366 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _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 In In 0.871910(14) 0.407910(11) 0.760878(11) 0.03775(7) Uani 1 1 d D . . B B 0.6597(3) 0.5973(2) 0.7575(2) 0.0426(7) Uani 1 1 d . . . H1 H 0.611(2) 0.6484(17) 0.7597(15) 0.042(7) Uiso 1 1 d . . . S1 S 0.75573(6) 0.45160(5) 0.62471(4) 0.04495(17) Uani 1 1 d . A . S2 S 0.68485(6) 0.40457(4) 0.84290(4) 0.04093(15) Uani 1 1 d . A . S3 S 0.94484(5) 0.54769(4) 0.79718(4) 0.04105(15) Uani 1 1 d . A . S4 S 0.99117(13) 0.34524(19) 0.88174(9) 0.0453(6) Uani 0.672(2) 1 d PD A 1 S5 S 1.10527(11) 0.27164(9) 0.82398(8) 0.0600(4) Uani 0.672(2) 1 d PD A 1 S6 S 1.13955(10) 0.33247(9) 0.71714(8) 0.0645(5) Uani 0.672(2) 1 d PD A 1 S7 S 0.9802(2) 0.33081(19) 0.65453(9) 0.0550(8) Uani 0.672(2) 1 d PD A 1 S4A S 1.0012(4) 0.3416(6) 0.8742(2) 0.091(3) Uani 0.328(2) 1 d PD A 2 S5A S 1.1445(2) 0.33360(19) 0.80499(19) 0.0714(10) Uani 0.328(2) 1 d PD A 2 S6A S 1.0922(2) 0.25886(16) 0.70963(17) 0.0676(9) Uani 0.328(2) 1 d PD A 2 S7A S 0.9696(7) 0.3317(6) 0.64863(18) 0.097(3) Uani 0.328(2) 1 d PD A 2 N11 N 0.59006(17) 0.53217(13) 0.70819(13) 0.0394(5) Uani 1 1 d . A . C11 C 0.6189(2) 0.47100(16) 0.65689(15) 0.0376(5) Uani 1 1 d . . . N12 N 0.52187(19) 0.42888(14) 0.63436(14) 0.0423(5) Uani 1 1 d . A . C12 C 0.4730(2) 0.52682(19) 0.71857(18) 0.0508(7) Uani 1 1 d . . . H12A H 0.4299 0.5615 0.7518 0.061 Uiso 1 1 calc R A . C13 C 0.4311(2) 0.46466(19) 0.67398(18) 0.0522(7) Uani 1 1 d . A . H13A H 0.3538 0.4480 0.6701 0.063 Uiso 1 1 calc R . . C14 C 0.5112(3) 0.35668(18) 0.57712(19) 0.0545(7) Uani 1 1 d . . . C15 C 0.5510(3) 0.3810(2) 0.4921(2) 0.0656(9) Uani 1 1 d . A . H15A H 0.5050 0.4263 0.4712 0.098 Uiso 1 1 calc R . . H15B H 0.5424 0.3351 0.4546 0.098 Uiso 1 1 calc R . . H15C H 0.6311 0.3972 0.4962 0.098 Uiso 1 1 calc R . . C16 C 0.5809(4) 0.2861(2) 0.6144(3) 0.0865(12) Uani 1 1 d . A . H16A H 0.5527 0.2729 0.6686 0.130 Uiso 1 1 calc R . . H16B H 0.6612 0.3016 0.6197 0.130 Uiso 1 1 calc R . . H16C H 0.5730 0.2388 0.5786 0.130 Uiso 1 1 calc R . . C17 C 0.3853(3) 0.3318(2) 0.5688(2) 0.0722(10) Uani 1 1 d . A . H17A H 0.3586 0.3156 0.6225 0.108 Uiso 1 1 calc R . . H17B H 0.3772 0.2865 0.5305 0.108 Uiso 1 1 calc R . . H17C H 0.3400 0.3776 0.5481 0.108 Uiso 1 1 calc R . . N21 N 0.68519(19) 0.57239(14) 0.84919(14) 0.0419(5) Uani 1 1 d . A . C21 C 0.6940(2) 0.49989(16) 0.88868(16) 0.0393(6) Uani 1 1 d . . . N22 N 0.71152(18) 0.51554(15) 0.97137(13) 0.0441(5) Uani 1 1 d . A . C22 C 0.6981(2) 0.63303(19) 0.90799(18) 0.0511(7) Uani 1 1 d . . . H22A H 0.6954 0.6894 0.8974 0.061 Uiso 1 1 calc R A . C23 C 0.7149(3) 0.59888(19) 0.98180(19) 0.0545(8) Uani 1 1 d . A . H23A H 0.7269 0.6266 1.0323 0.065 Uiso 1 1 calc R . . C24 C 0.7170(2) 0.4553(2) 1.04263(17) 0.0548(8) Uani 1 1 d . . . C25 C 0.6046(3) 0.4094(2) 1.0435(2) 0.0719(10) Uani 1 1 d . A . H25A H 0.5948 0.3779 0.9930 0.108 Uiso 1 1 calc R . . H25B H 0.5417 0.4478 1.0474 0.108 Uiso 1 1 calc R . . H25C H 0.6051 0.3729 1.0908 0.108 Uiso 1 1 calc R . . C26 C 0.8191(3) 0.3989(2) 1.0335(2) 0.0774(12) Uani 1 1 d . A . H26A H 0.8089 0.3674 0.9830 0.116 Uiso 1 1 calc R . . H26B H 0.8249 0.3623 1.0806 0.116 Uiso 1 1 calc R . . H26C H 0.8888 0.4311 1.0310 0.116 Uiso 1 1 calc R . . C27 C 0.7349(3) 0.5025(2) 1.12361(18) 0.0713(10) Uani 1 1 d . A . H27A H 0.7385 0.4646 1.1697 0.107 Uiso 1 1 calc R . . H27B H 0.6713 0.5399 1.1302 0.107 Uiso 1 1 calc R . . H27C H 0.8062 0.5330 1.1223 0.107 Uiso 1 1 calc R . . N31 N 0.76819(19) 0.62551(13) 0.71201(13) 0.0422(5) Uani 1 1 d . A . C31 C 0.8810(2) 0.60777(15) 0.71993(16) 0.0406(6) Uani 1 1 d . . . N32 N 0.93700(19) 0.64733(14) 0.65911(13) 0.0457(5) Uani 1 1 d . A . C32 C 0.7530(3) 0.67707(18) 0.64556(19) 0.0551(7) Uani 1 1 d . . . H32A H 0.6828 0.6996 0.6265 0.066 Uiso 1 1 calc R A . C33 C 0.8555(3) 0.6897(2) 0.61258(19) 0.0588(8) Uani 1 1 d . A . H33A H 0.8693 0.7219 0.5658 0.071 Uiso 1 1 calc R . . C34 C 1.0637(3) 0.6452(2) 0.64161(18) 0.0563(8) Uani 1 1 d . . . C35 C 1.0957(4) 0.5610(3) 0.6164(3) 0.1014(15) Uani 1 1 d . A . H35A H 1.0827 0.5236 0.6616 0.152 Uiso 1 1 calc R . . H35B H 1.1762 0.5598 0.6030 0.152 Uiso 1 1 calc R . . H35C H 1.0490 0.5449 0.5682 0.152 Uiso 1 1 calc R . . C36 C 1.1310(3) 0.6731(3) 0.7176(2) 0.0958(15) Uani 1 1 d . A . H36A H 1.1206 0.6346 0.7622 0.144 Uiso 1 1 calc R . . H36B H 1.1040 0.7265 0.7340 0.144 Uiso 1 1 calc R . . H36C H 1.2119 0.6763 0.7055 0.144 Uiso 1 1 calc R . . C37 C 1.0867(3) 0.7058(3) 0.5726(2) 0.0822(12) Uani 1 1 d . A . H37A H 1.1679 0.7054 0.5612 0.123 Uiso 1 1 calc R . . H37B H 1.0644 0.7601 0.5898 0.123 Uiso 1 1 calc R . . H37C H 1.0425 0.6905 0.5231 0.123 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 In 0.03344(11) 0.03828(12) 0.04149(12) 0.00225(8) 0.00061(7) 0.00269(7) B 0.0425(16) 0.0421(17) 0.0426(17) -0.0006(13) -0.0048(12) 0.0082(14) S1 0.0377(3) 0.0599(4) 0.0372(3) -0.0021(3) -0.0002(3) 0.0065(3) S2 0.0396(3) 0.0423(4) 0.0411(4) 0.0009(3) 0.0053(3) -0.0012(3) S3 0.0403(3) 0.0432(4) 0.0390(3) 0.0079(3) -0.0075(3) -0.0056(3) S4 0.0377(8) 0.0584(13) 0.0398(10) 0.0106(9) 0.0029(7) 0.0137(8) S5 0.0517(7) 0.0640(9) 0.0646(8) 0.0121(6) 0.0074(5) 0.0242(6) S6 0.0420(6) 0.0967(12) 0.0555(8) 0.0079(7) 0.0121(5) 0.0157(6) S7 0.0626(13) 0.0592(16) 0.0432(13) -0.0057(11) 0.0021(9) 0.0196(11) S4A 0.100(4) 0.101(5) 0.074(4) 0.025(3) 0.018(3) 0.056(3) S5A 0.0417(13) 0.074(2) 0.098(2) -0.0276(18) -0.0057(13) 0.0102(13) S6A 0.0510(14) 0.0557(17) 0.096(2) -0.0236(14) 0.0001(13) 0.0128(12) S7A 0.115(6) 0.112(6) 0.062(4) -0.026(4) -0.017(3) 0.047(4) N11 0.0339(11) 0.0474(13) 0.0367(11) 0.0006(10) -0.0016(8) 0.0038(9) C11 0.0349(12) 0.0434(14) 0.0340(13) 0.0062(11) -0.0035(10) 0.0032(11) N12 0.0421(12) 0.0443(12) 0.0400(12) 0.0031(10) -0.0042(9) -0.0015(10) C12 0.0380(14) 0.0632(19) 0.0514(17) -0.0023(14) 0.0055(12) 0.0060(13) C13 0.0358(14) 0.066(2) 0.0551(18) 0.0053(15) 0.0004(12) -0.0023(14) C14 0.0605(18) 0.0427(16) 0.0591(19) -0.0007(14) -0.0125(14) -0.0008(14) C15 0.080(2) 0.067(2) 0.0494(19) -0.0156(16) -0.0040(16) -0.0042(18) C16 0.092(3) 0.0414(18) 0.124(3) 0.014(2) -0.026(2) 0.0030(19) C17 0.068(2) 0.062(2) 0.086(3) -0.0057(19) -0.0169(18) -0.0159(18) N21 0.0394(12) 0.0448(13) 0.0414(13) -0.0026(10) 0.0006(9) 0.0014(10) C21 0.0325(12) 0.0477(15) 0.0381(13) -0.0011(12) 0.0036(10) 0.0004(11) N22 0.0379(11) 0.0585(15) 0.0362(12) -0.0011(10) 0.0032(9) 0.0043(10) C22 0.0556(17) 0.0474(17) 0.0501(17) -0.0129(14) 0.0010(13) -0.0016(14) C23 0.0542(18) 0.063(2) 0.0463(17) -0.0152(14) -0.0007(13) 0.0043(15) C24 0.0472(16) 0.081(2) 0.0363(15) 0.0047(15) 0.0045(12) 0.0114(15) C25 0.070(2) 0.091(3) 0.055(2) 0.0151(18) 0.0109(17) -0.0063(19) C26 0.081(3) 0.103(3) 0.0483(19) 0.0095(18) -0.0008(17) 0.046(2) C27 0.066(2) 0.107(3) 0.0408(17) -0.0016(18) 0.0050(15) 0.011(2) N31 0.0445(12) 0.0387(12) 0.0428(12) 0.0069(10) -0.0065(9) -0.0031(10) C31 0.0475(15) 0.0376(14) 0.0362(14) 0.0027(11) -0.0047(11) -0.0096(11) N32 0.0494(13) 0.0473(13) 0.0397(12) 0.0095(10) -0.0059(9) -0.0126(11) C32 0.0580(18) 0.0506(17) 0.0556(18) 0.0181(14) -0.0141(14) 0.0011(14) C33 0.068(2) 0.0606(19) 0.0472(17) 0.0237(15) -0.0109(14) -0.0120(16) C34 0.0513(17) 0.066(2) 0.0519(18) 0.0131(15) 0.0008(13) -0.0172(15) C35 0.087(3) 0.088(3) 0.133(4) -0.003(3) 0.052(3) -0.004(2) C36 0.075(2) 0.144(4) 0.067(2) 0.030(2) -0.0141(19) -0.065(3) C37 0.074(2) 0.111(3) 0.061(2) 0.032(2) 0.0062(18) -0.027(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 In S3 2.5070(7) . ? In S7A 2.5088(12) . ? In S7 2.5091(10) . ? In S4A 2.5705(12) . ? In S4 2.5708(10) . ? In S2 2.5903(7) . ? In S1 2.6414(7) . ? B H1 1.01(3) . ? B N11 1.545(4) . ? B N31 1.554(4) . ? B N21 1.555(4) . ? S1 C11 1.724(2) . ? S2 C21 1.731(3) . ? S3 C31 1.737(3) . ? S4 S5 2.045(2) . ? S5 S6 2.0457(15) . ? S6 S7 2.082(3) . ? S4A S5A 2.045(2) . ? S5A S6A 2.0451(17) . ? S6A S7A 2.082(3) . ? N11 C11 1.351(3) . ? N11 C12 1.382(3) . ? C11 N12 1.363(3) . ? N12 C13 1.386(3) . ? N12 C14 1.505(4) . ? C12 C13 1.331(4) . ? C14 C15 1.519(4) . ? C14 C17 1.523(4) . ? C14 C16 1.525(4) . ? N21 C21 1.352(3) . ? N21 C22 1.380(4) . ? C21 N22 1.369(3) . ? N22 C23 1.378(4) . ? N22 C24 1.517(4) . ? C22 C23 1.326(4) . ? C24 C25 1.511(5) . ? C24 C26 1.517(4) . ? C24 C27 1.529(4) . ? N31 C31 1.347(3) . ? N31 C32 1.373(3) . ? C31 N32 1.363(3) . ? N32 C33 1.378(4) . ? N32 C34 1.512(4) . ? C32 C33 1.340(4) . ? C34 C35 1.490(5) . ? C34 C36 1.505(5) . ? C34 C37 1.524(4) . ? 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 In S7A 117.8(3) . . ? S3 In S7 116.54(9) . . ? S7A In S7 3.51(13) . . ? S3 In S4A 92.0(3) . . ? S7A In S4A 92.00(15) . . ? S7 In S4A 88.78(13) . . ? S3 In S4 91.05(8) . . ? S7A In S4 95.95(9) . . ? S7 In S4 92.75(6) . . ? S4A In S4 4.07(11) . . ? S3 In S2 100.58(2) . . ? S7A In S2 140.4(3) . . ? S7 In S2 142.36(9) . . ? S4A In S2 96.23(9) . . ? S4 In S2 92.53(4) . . ? S3 In S1 96.10(2) . . ? S7A In S1 76.39(7) . . ? S7 In S1 79.68(4) . . ? S4A In S1 167.99(17) . . ? S4 In S1 171.33(7) . . ? S2 In S1 90.97(2) . . ? H1 B N11 107.6(15) . . ? H1 B N31 103.7(15) . . ? N11 B N31 112.5(2) . . ? H1 B N21 105.8(14) . . ? N11 B N21 112.9(2) . . ? N31 B N21 113.5(2) . . ? C11 S1 In 104.50(8) . . ? C21 S2 In 99.18(8) . . ? C31 S3 In 102.58(9) . . ? S5 S4 In 103.37(7) . . ? S4 S5 S6 104.29(8) . . ? S5 S6 S7 101.92(10) . . ? S6 S7 In 96.97(8) . . ? S5A S4A In 96.11(11) . . ? S6A S5A S4A 102.9(3) . . ? S5A S6A S7A 101.2(2) . . ? S6A S7A In 105.32(12) . . ? C11 N11 C12 107.1(2) . . ? C11 N11 B 133.8(2) . . ? C12 N11 B 118.9(2) . . ? N11 C11 N12 108.6(2) . . ? N11 C11 S1 125.06(19) . . ? N12 C11 S1 126.3(2) . . ? C11 N12 C13 107.5(2) . . ? C11 N12 C14 127.8(2) . . ? C13 N12 C14 124.7(2) . . ? C13 C12 N11 109.1(2) . . ? C12 C13 N12 107.7(2) . . ? N12 C14 C15 109.1(2) . . ? N12 C14 C17 108.8(3) . . ? C15 C14 C17 108.3(3) . . ? N12 C14 C16 108.9(3) . . ? C15 C14 C16 112.4(3) . . ? C17 C14 C16 109.2(3) . . ? C21 N21 C22 107.7(2) . . ? C21 N21 B 133.6(2) . . ? C22 N21 B 118.6(2) . . ? N21 C21 N22 107.6(2) . . ? N21 C21 S2 126.2(2) . . ? N22 C21 S2 126.2(2) . . ? C21 N22 C23 107.9(2) . . ? C21 N22 C24 128.3(2) . . ? C23 N22 C24 123.6(2) . . ? C23 C22 N21 108.9(3) . . ? C22 C23 N22 107.8(3) . . ? C25 C24 N22 108.6(2) . . ? C25 C24 C26 112.3(3) . . ? N22 C24 C26 109.5(2) . . ? C25 C24 C27 109.7(3) . . ? N22 C24 C27 108.7(3) . . ? C26 C24 C27 108.0(3) . . ? C31 N31 C32 107.8(2) . . ? C31 N31 B 134.2(2) . . ? C32 N31 B 118.0(2) . . ? N31 C31 N32 108.6(2) . . ? N31 C31 S3 125.59(19) . . ? N32 C31 S3 125.8(2) . . ? C31 N32 C33 107.2(2) . . ? C31 N32 C34 128.2(2) . . ? C33 N32 C34 124.6(2) . . ? C33 C32 N31 108.3(3) . . ? C32 C33 N32 108.1(2) . . ? C35 C34 C36 112.1(4) . . ? C35 C34 N32 109.1(3) . . ? C36 C34 N32 108.9(3) . . ? C35 C34 C37 110.6(3) . . ? C36 C34 C37 107.3(3) . . ? N32 C34 C37 108.6(3) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.594 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.064 # Attachment 'TmIn_-_TMINS10.CIF' data_tmins10 _database_code_depnum_ccdc_archive 'CCDC 680246' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H37 B In N6 S3' _chemical_formula_weight 631.41 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 13.5112(4) _cell_length_b 13.5112(4) _cell_length_c 28.6753(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4533.4(3) _cell_formula_units_Z 6 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 7291 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1950 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7510 _exptl_absorpt_correction_T_max 0.8232 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 10804 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.58 _reflns_number_total 2445 _reflns_number_gt 2116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2445 _refine_ls_number_parameters 103 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.1330 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _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 In In 0.0000 0.0000 0.305325(9) 0.05517(16) Uani 1 3 d S . . S S 0.16151(4) 0.16458(5) 0.24797(2) 0.05001(19) Uani 1 1 d . . . B B 0.0000 0.0000 0.15592(15) 0.0482(8) Uani 1 3 d SD . . N11 N 0.02620(15) 0.12025(15) 0.17105(7) 0.0478(4) Uani 1 1 d . . . N12 N 0.06027(16) 0.27628(15) 0.20776(7) 0.0526(4) Uani 1 1 d . . . C11 C 0.08012(16) 0.18674(16) 0.20838(8) 0.0454(4) Uani 1 1 d . . . C12 C -0.0256(2) 0.1704(2) 0.14646(9) 0.0563(5) Uani 1 1 d . . . H12A H -0.0671 0.1427 0.1190 0.068 Uiso 1 1 calc R . . C13 C -0.0059(2) 0.2643(2) 0.16865(10) 0.0620(6) Uani 1 1 d . . . H13A H -0.0317 0.3137 0.1597 0.074 Uiso 1 1 calc R . . C14 C 0.0966(2) 0.3694(2) 0.24330(11) 0.0631(6) Uani 1 1 d . . . C15 C 0.0479(3) 0.3168(3) 0.29079(10) 0.0764(8) Uani 1 1 d . . . H15A H 0.0787 0.2694 0.3003 0.115 Uiso 1 1 calc R . . H15B H -0.0338 0.2713 0.2887 0.115 Uiso 1 1 calc R . . H15C H 0.0682 0.3765 0.3133 0.115 Uiso 1 1 calc R . . C16 C 0.0463(4) 0.4450(3) 0.22976(12) 0.0898(10) Uani 1 1 d . . . H16A H -0.0357 0.4000 0.2297 0.135 Uiso 1 1 calc R . . H16B H 0.0726 0.4762 0.1992 0.135 Uiso 1 1 calc R . . H16C H 0.0703 0.5061 0.2519 0.135 Uiso 1 1 calc R . . C17 C 0.2262(3) 0.4393(2) 0.24395(13) 0.0833(9) Uani 1 1 d . . . H17A H 0.2566 0.3914 0.2531 0.125 Uiso 1 1 calc R . . H17B H 0.2503 0.5010 0.2657 0.125 Uiso 1 1 calc R . . H17C H 0.2536 0.4695 0.2134 0.125 Uiso 1 1 calc R . . C100 C 0.039(3) -0.074(2) -0.0006(6) 0.300(7) Uiso 1 1 d . . . H10A H 0.0666 -0.1251 -0.0022 0.360 Uiso 1 1 calc R . . H1 H 0.0000 0.0000 0.1189(7) 0.070(14) Uiso 1 3 d SD . . 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 In 0.06390(19) 0.06390(19) 0.0377(2) 0.000 0.000 0.03195(9) S 0.0493(3) 0.0541(3) 0.0473(3) -0.0002(2) -0.0068(2) 0.0264(2) B 0.0525(12) 0.0525(12) 0.040(2) 0.000 0.000 0.0263(6) N11 0.0496(9) 0.0492(9) 0.0440(9) 0.0044(7) -0.0027(7) 0.0244(7) N12 0.0546(9) 0.0453(9) 0.0566(11) 0.0041(8) -0.0039(8) 0.0240(8) C11 0.0435(9) 0.0447(9) 0.0462(11) 0.0049(8) 0.0005(8) 0.0206(7) C12 0.0539(11) 0.0585(12) 0.0529(13) 0.0109(10) -0.0083(10) 0.0253(10) C13 0.0605(13) 0.0580(12) 0.0712(17) 0.0111(11) -0.0094(11) 0.0324(11) C14 0.0737(15) 0.0506(12) 0.0669(16) -0.0028(10) -0.0038(12) 0.0325(11) C15 0.101(2) 0.0759(17) 0.0656(18) -0.0044(13) 0.0089(15) 0.0538(16) C16 0.129(3) 0.0676(17) 0.092(2) -0.0054(16) -0.010(2) 0.0634(19) C17 0.0761(17) 0.0584(15) 0.088(2) -0.0197(14) -0.0054(15) 0.0134(12) _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 In S 2.7493(6) . ? In S 2.7493(6) 2 ? In S 2.7493(6) 3 ? S C11 1.708(2) . ? B H1 1.063(19) . ? B N11 1.542(2) 2 ? B N11 1.542(2) . ? B N11 1.542(2) 3 ? N11 C11 1.352(3) . ? N11 C12 1.386(3) . ? N12 C11 1.364(3) . ? N12 C13 1.392(3) . ? N12 C14 1.498(3) . ? C12 C13 1.322(4) . ? C14 C17 1.518(4) . ? C14 C15 1.525(4) . ? C14 C16 1.534(4) . ? C100 C100 1.350(8) 12 ? C100 C100 1.350(8) 11 ? 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 S In S 87.898(18) . 2 ? S In S 87.898(18) . 3 ? S In S 87.898(18) 2 3 ? C11 S In 102.66(7) . . ? H1 B N11 106.34(17) . 2 ? H1 B N11 106.34(17) . . ? N11 B N11 112.41(15) 2 . ? H1 B N11 106.34(17) . 3 ? N11 B N11 112.41(15) 2 3 ? N11 B N11 112.41(15) . 3 ? C11 N11 C12 108.30(18) . . ? C11 N11 B 133.3(2) . . ? C12 N11 B 117.8(2) . . ? C11 N12 C13 107.9(2) . . ? C11 N12 C14 127.5(2) . . ? C13 N12 C14 124.6(2) . . ? N11 C11 N12 107.41(18) . . ? N11 C11 S 126.15(16) . . ? N12 C11 S 126.41(16) . . ? C13 C12 N11 108.4(2) . . ? C12 C13 N12 108.0(2) . . ? N12 C14 C17 108.8(2) . . ? N12 C14 C15 109.4(2) . . ? C17 C14 C15 111.9(3) . . ? N12 C14 C16 108.6(2) . . ? C17 C14 C16 110.3(3) . . ? C15 C14 C16 107.7(2) . . ? C100 C100 C100 119.94(15) 12 11 ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 28.58 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.725 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.071 # Attachment 'TmTl_-_tmtls20.cif' data_kya _database_code_depnum_ccdc_archive 'CCDC 680247' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H37 B N6 S3 Tl' _chemical_formula_weight 720.96 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.6625(11) _cell_length_b 15.6152(12) _cell_length_c 15.6517(11) _cell_angle_alpha 69.9950(10) _cell_angle_beta 67.7660(10) _cell_angle_gamma 71.1020(10) _cell_volume 3038.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 5.545 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2870 _exptl_absorpt_correction_T_max 0.2870 _exptl_absorpt_process_details sadabs _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 20094 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.10 _reflns_number_total 12871 _reflns_number_gt 9304 _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^)+(0.0300P)^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 0.00027(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12871 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.012 _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 Tl1 Tl 0.624036(14) 0.522489(14) 0.391874(12) 0.04754(7) Uani 1 1 d . . . Tl2 Tl 1.032423(15) -0.098125(13) 0.115997(13) 0.04856(7) Uani 1 1 d . . . S1 S 0.54204(10) 0.34940(9) 0.48157(8) 0.0469(3) Uani 1 1 d . . . S2 S 0.52279(11) 0.63222(12) 0.22483(10) 0.0710(5) Uani 1 1 d . . . S3 S 0.18996(9) 0.58792(8) 0.53518(8) 0.0453(3) Uani 1 1 d . . . S4 S 0.97095(9) 0.00181(9) 0.27852(8) 0.0478(3) Uani 1 1 d . . . S5 S 1.16950(10) 0.00489(8) -0.08361(9) 0.0492(3) Uani 1 1 d . . . S6 S 0.91515(10) 0.28203(9) -0.03962(9) 0.0525(3) Uani 1 1 d . . . N11 N 0.4607(2) 0.4146(2) 0.3340(2) 0.0331(8) Uani 1 1 d . . . N12 N 0.5823(3) 0.2879(2) 0.3226(2) 0.0375(8) Uani 1 1 d . . . N21 N 0.3510(2) 0.5701(2) 0.2843(2) 0.0347(8) Uani 1 1 d . . . N22 N 0.3710(3) 0.6711(2) 0.1445(2) 0.0380(9) Uani 1 1 d . . . N31 N 0.2833(3) 0.4521(2) 0.4386(2) 0.0351(8) Uani 1 1 d . . . N32 N 0.1467(3) 0.4199(2) 0.5566(2) 0.0365(8) Uani 1 1 d . . . N41 N 1.1285(3) 0.0736(2) 0.1447(2) 0.0365(8) Uani 1 1 d . . . N42 N 1.1735(3) -0.0332(3) 0.2652(2) 0.0423(9) Uani 1 1 d . . . N51 N 1.1493(3) 0.1585(2) -0.0262(2) 0.0336(8) Uani 1 1 d . . . N52 N 1.2705(3) 0.1487(2) -0.1601(2) 0.0408(9) Uani 1 1 d . . . N61 N 1.0057(3) 0.2270(2) 0.0986(2) 0.0331(8) Uani 1 1 d . . . N62 N 0.9031(2) 0.3663(2) 0.0947(2) 0.0340(8) Uani 1 1 d . . . B1 B 0.3767(4) 0.4957(4) 0.3729(3) 0.0345(11) Uani 1 1 d . . . H1 H 0.404(2) 0.526(2) 0.416(2) 0.010(8) Uiso 1 1 d . . . B2 B 1.0677(4) 0.1339(3) 0.0720(3) 0.0337(11) Uani 1 1 d . . . H2 H 1.022(3) 0.090(2) 0.068(2) 0.020(9) Uiso 1 1 d . . . C11 C 0.5285(3) 0.3509(3) 0.3770(3) 0.0340(10) Uani 1 1 d . . . C12 C 0.4714(3) 0.3905(3) 0.2534(3) 0.0406(11) Uani 1 1 d . . . H12A H 0.4332 0.4227 0.2107 0.049 Uiso 1 1 calc R . . C13 C 0.5454(3) 0.3133(3) 0.2462(3) 0.0425(11) Uani 1 1 d . . . H13A H 0.5681 0.2819 0.1977 0.051 Uiso 1 1 calc R . . C14 C 0.6668(4) 0.2047(3) 0.3404(3) 0.0483(12) Uani 1 1 d . . . C15 C 0.7081(4) 0.1608(4) 0.2557(4) 0.0665(16) Uani 1 1 d . . . H15A H 0.7360 0.2054 0.1981 0.100 Uiso 1 1 calc R . . H15B H 0.6538 0.1439 0.2484 0.100 Uiso 1 1 calc R . . H15C H 0.7606 0.1053 0.2668 0.100 Uiso 1 1 calc R . . C16 C 0.7508(4) 0.2357(4) 0.3479(4) 0.0611(15) Uani 1 1 d . . . H16A H 0.7252 0.2632 0.4018 0.092 Uiso 1 1 calc R . . H16B H 0.7750 0.2816 0.2898 0.092 Uiso 1 1 calc R . . H16C H 0.8060 0.1821 0.3568 0.092 Uiso 1 1 calc R . . C17 C 0.6245(5) 0.1343(4) 0.4307(4) 0.0743(18) Uani 1 1 d . . . H17A H 0.5979 0.1622 0.4844 0.112 Uiso 1 1 calc R . . H17B H 0.6778 0.0795 0.4416 0.112 Uiso 1 1 calc R . . H17C H 0.5708 0.1163 0.4238 0.112 Uiso 1 1 calc R . . C21 C 0.4127(3) 0.6255(3) 0.2179(3) 0.0367(10) Uani 1 1 d . . . C22 C 0.2710(3) 0.5813(3) 0.2521(3) 0.0452(12) Uani 1 1 d . . . H22A H 0.2168 0.5511 0.2848 0.054 Uiso 1 1 calc R . . C23 C 0.2836(3) 0.6418(3) 0.1669(3) 0.0460(12) Uani 1 1 d . . . H23A H 0.2406 0.6613 0.1288 0.055 Uiso 1 1 calc R . . C24 C 0.4160(4) 0.7356(3) 0.0513(3) 0.0483(12) Uani 1 1 d . . . C25 C 0.5148(5) 0.6816(5) -0.0019(4) 0.101(3) Uani 1 1 d . . . H25A H 0.5620 0.6599 0.0350 0.151 Uiso 1 1 calc R . . H25B H 0.5428 0.7218 -0.0632 0.151 Uiso 1 1 calc R . . H25C H 0.5032 0.6283 -0.0115 0.151 Uiso 1 1 calc R . . C26 C 0.4299(6) 0.8194(4) 0.0698(4) 0.093(2) Uani 1 1 d . . . H26A H 0.3649 0.8528 0.1032 0.139 Uiso 1 1 calc R . . H26B H 0.4585 0.8607 0.0096 0.139 Uiso 1 1 calc R . . H26C H 0.4752 0.7981 0.1085 0.139 Uiso 1 1 calc R . . C27 C 0.3451(4) 0.7697(4) -0.0085(3) 0.0690(16) Uani 1 1 d . . . H27A H 0.2815 0.8057 0.0239 0.103 Uiso 1 1 calc R . . H27B H 0.3330 0.7165 -0.0179 0.103 Uiso 1 1 calc R . . H27C H 0.3750 0.8087 -0.0698 0.103 Uiso 1 1 calc R . . C31 C 0.2053(3) 0.4853(3) 0.5105(3) 0.0321(9) Uani 1 1 d . . . C32 C 0.2712(4) 0.3670(3) 0.4405(3) 0.0440(11) Uani 1 1 d . . . H32A H 0.3140 0.3290 0.3989 0.053 Uiso 1 1 calc R . . C33 C 0.1881(4) 0.3481(3) 0.5114(3) 0.0452(11) Uani 1 1 d . . . H33A H 0.1623 0.2949 0.5277 0.054 Uiso 1 1 calc R . . C34 C 0.0599(3) 0.4177(3) 0.6469(3) 0.0454(12) Uani 1 1 d . . . C35 C 0.0161(4) 0.3347(4) 0.6702(4) 0.0692(16) Uani 1 1 d . . . H35A H -0.0089 0.3398 0.6191 0.104 Uiso 1 1 calc R . . H35B H -0.0390 0.3330 0.7293 0.104 Uiso 1 1 calc R . . H35C H 0.0681 0.2778 0.6772 0.104 Uiso 1 1 calc R . . C36 C 0.1007(4) 0.4110(5) 0.7256(3) 0.079(2) Uani 1 1 d . . . H36A H 0.1526 0.3540 0.7329 0.119 Uiso 1 1 calc R . . H36B H 0.0461 0.4101 0.7850 0.119 Uiso 1 1 calc R . . H36C H 0.1294 0.4645 0.7091 0.119 Uiso 1 1 calc R . . C37 C -0.0223(4) 0.5069(4) 0.6331(4) 0.0678(16) Uani 1 1 d . . . H37A H -0.0470 0.5095 0.5826 0.102 Uiso 1 1 calc R . . H37B H 0.0057 0.5610 0.6160 0.102 Uiso 1 1 calc R . . H37C H -0.0776 0.5066 0.6919 0.102 Uiso 1 1 calc R . . C41 C 1.0933(3) 0.0132(3) 0.2297(3) 0.0362(10) Uani 1 1 d . . . C42 C 1.2293(4) 0.0672(4) 0.1298(4) 0.0510(12) Uani 1 1 d . . . H42A H 1.2713 0.1025 0.0775 0.061 Uiso 1 1 calc R . . C43 C 1.2566(4) 0.0023(4) 0.2026(4) 0.0548(13) Uani 1 1 d . . . H43A H 1.3214 -0.0163 0.2100 0.066 Uiso 1 1 calc R . . C44 C 1.1766(4) -0.1155(4) 0.3513(3) 0.0519(13) Uani 1 1 d . . . C45 C 1.2820(4) -0.1484(5) 0.3585(4) 0.081(2) Uani 1 1 d . . . H45A H 1.3278 -0.1689 0.3020 0.122 Uiso 1 1 calc R . . H45B H 1.2842 -0.2002 0.4145 0.122 Uiso 1 1 calc R . . H45C H 1.3022 -0.0976 0.3639 0.122 Uiso 1 1 calc R . . C46 C 1.1469(5) -0.1930(4) 0.3381(4) 0.0740(18) Uani 1 1 d . . . H46A H 1.1938 -0.2113 0.2808 0.111 Uiso 1 1 calc R . . H46B H 1.0791 -0.1712 0.3323 0.111 Uiso 1 1 calc R . . H46C H 1.1487 -0.2463 0.3928 0.111 Uiso 1 1 calc R . . C47 C 1.1049(4) -0.0828(4) 0.4405(3) 0.0725(17) Uani 1 1 d . . . H47A H 1.0365 -0.0613 0.4362 0.109 Uiso 1 1 calc R . . H47B H 1.1255 -0.0320 0.4454 0.109 Uiso 1 1 calc R . . H47C H 1.1072 -0.1344 0.4966 0.109 Uiso 1 1 calc R . . C51 C 1.1976(3) 0.1059(3) -0.0902(3) 0.0353(10) Uani 1 1 d . . . C52 C 1.1935(3) 0.2343(3) -0.0568(3) 0.0421(11) Uani 1 1 d . . . H52A H 1.1739 0.2822 -0.0258 0.051 Uiso 1 1 calc R . . C53 C 1.2682(4) 0.2280(3) -0.1375(3) 0.0483(12) Uani 1 1 d . . . H53A H 1.3114 0.2696 -0.1725 0.058 Uiso 1 1 calc R . . C54 C 1.3471(4) 0.1151(4) -0.2462(4) 0.0593(15) Uani 1 1 d . . . C55 C 1.4116(5) 0.1870(5) -0.3048(4) 0.099(3) Uani 1 1 d . . . H55A H 1.4485 0.1914 -0.2669 0.149 Uiso 1 1 calc R . . H55B H 1.3684 0.2475 -0.3231 0.149 Uiso 1 1 calc R . . H55C H 1.4591 0.1680 -0.3615 0.149 Uiso 1 1 calc R . . C56 C 1.4134(4) 0.0213(4) -0.2108(4) 0.0804(19) Uani 1 1 d . . . H56A H 1.4487 0.0291 -0.1736 0.121 Uiso 1 1 calc R . . H56B H 1.4622 -0.0016 -0.2650 0.121 Uiso 1 1 calc R . . H56C H 1.3714 -0.0234 -0.1714 0.121 Uiso 1 1 calc R . . C57 C 1.2897(5) 0.1082(4) -0.3072(4) 0.0775(19) Uani 1 1 d . . . H57A H 1.2486 0.0624 -0.2706 0.116 Uiso 1 1 calc R . . H57B H 1.3378 0.0893 -0.3639 0.116 Uiso 1 1 calc R . . H57C H 1.2465 0.1687 -0.3258 0.116 Uiso 1 1 calc R . . C61 C 0.9405(3) 0.2926(3) 0.0532(3) 0.0341(10) Uani 1 1 d . . . C62 C 1.0074(3) 0.2599(3) 0.1693(3) 0.0396(11) Uani 1 1 d . . . H62A H 1.0457 0.2280 0.2120 0.048 Uiso 1 1 calc R . . C63 C 0.9457(3) 0.3445(3) 0.1669(3) 0.0406(11) Uani 1 1 d . . . H63A H 0.9333 0.3826 0.2072 0.049 Uiso 1 1 calc R . . C64 C 0.8268(3) 0.4547(3) 0.0693(3) 0.0414(11) Uani 1 1 d . . . C65 C 0.8069(4) 0.5161(4) 0.1336(4) 0.0633(15) Uani 1 1 d . . . H65A H 0.7804 0.4833 0.1994 0.095 Uiso 1 1 calc R . . H65B H 0.7580 0.5732 0.1177 0.095 Uiso 1 1 calc R . . H65C H 0.8695 0.5312 0.1249 0.095 Uiso 1 1 calc R . . C66 C 0.7286(4) 0.4294(4) 0.0864(4) 0.0600(14) Uani 1 1 d . . . H66A H 0.7039 0.3970 0.1528 0.090 Uiso 1 1 calc R . . H66B H 0.7403 0.3891 0.0462 0.090 Uiso 1 1 calc R . . H66C H 0.6787 0.4860 0.0712 0.090 Uiso 1 1 calc R . . C67 C 0.8691(4) 0.5069(4) -0.0340(4) 0.0626(15) Uani 1 1 d . . . H67A H 0.9310 0.5226 -0.0416 0.094 Uiso 1 1 calc R . . H67B H 0.8200 0.5637 -0.0502 0.094 Uiso 1 1 calc R . . H67C H 0.8832 0.4675 -0.0758 0.094 Uiso 1 1 calc R . . C101 C 0.1640(14) 0.2557(10) 0.3159(15) 0.154(6) Uani 1 1 d . . . H10A H 0.1211 0.3056 0.2856 0.185 Uiso 1 1 calc R . . C102 C 0.2601(18) 0.2376(11) 0.2715(8) 0.166(5) Uani 1 1 d . . . H10B H 0.2836 0.2731 0.2089 0.199 Uiso 1 1 calc R . . C103 C 0.3251(10) 0.1728(11) 0.3096(14) 0.153(5) Uani 1 1 d . . . H10C H 0.3938 0.1604 0.2742 0.183 Uiso 1 1 calc R . . C104 C 0.2935(17) 0.1240(9) 0.3992(17) 0.182(7) Uani 1 1 d . . . H10D H 0.3402 0.0794 0.4292 0.218 Uiso 1 1 calc R . . C105 C 0.189(2) 0.1398(13) 0.4492(11) 0.209(12) Uani 1 1 d . . . H10F H 0.1626 0.1065 0.5123 0.250 Uiso 1 1 calc R . . C106 C 0.1271(12) 0.2093(13) 0.3969(16) 0.173(8) Uani 1 1 d . . . H10G H 0.0565 0.2207 0.4241 0.208 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 0.04492(12) 0.06079(14) 0.03756(10) -0.01241(9) -0.01315(8) -0.01168(10) Tl2 0.05764(14) 0.04036(12) 0.05117(11) -0.01014(9) -0.01704(10) -0.01605(10) S1 0.0563(8) 0.0469(7) 0.0394(6) -0.0117(5) -0.0251(6) -0.0005(6) S2 0.0591(9) 0.0939(12) 0.0644(8) 0.0230(8) -0.0372(7) -0.0459(9) S3 0.0446(7) 0.0389(7) 0.0511(6) -0.0146(6) -0.0122(6) -0.0067(6) S4 0.0388(7) 0.0510(8) 0.0453(6) -0.0075(6) -0.0086(5) -0.0090(6) S5 0.0526(8) 0.0376(7) 0.0584(7) -0.0210(6) -0.0050(6) -0.0158(6) S6 0.0629(8) 0.0484(8) 0.0567(7) -0.0231(6) -0.0371(7) 0.0076(7) N11 0.0304(19) 0.039(2) 0.0297(16) -0.0077(15) -0.0104(15) -0.0065(17) N12 0.038(2) 0.038(2) 0.0360(18) -0.0097(16) -0.0120(16) -0.0069(18) N21 0.0302(19) 0.041(2) 0.0315(17) -0.0027(16) -0.0127(15) -0.0081(17) N22 0.035(2) 0.041(2) 0.0326(17) -0.0030(16) -0.0128(16) -0.0056(18) N31 0.038(2) 0.037(2) 0.0343(18) -0.0069(16) -0.0130(16) -0.0120(17) N32 0.036(2) 0.039(2) 0.0355(18) -0.0077(17) -0.0105(16) -0.0108(18) N41 0.035(2) 0.031(2) 0.0430(19) -0.0047(16) -0.0177(17) -0.0044(17) N42 0.043(2) 0.039(2) 0.043(2) -0.0086(18) -0.0191(18) 0.0003(19) N51 0.035(2) 0.0252(19) 0.0375(18) -0.0067(15) -0.0086(16) -0.0067(16) N52 0.043(2) 0.033(2) 0.0407(19) -0.0112(17) -0.0033(17) -0.0107(18) N61 0.034(2) 0.0293(19) 0.0370(18) -0.0100(15) -0.0124(16) -0.0050(16) N62 0.0305(19) 0.0296(19) 0.0409(18) -0.0133(16) -0.0088(16) -0.0029(16) B1 0.037(3) 0.035(3) 0.033(2) -0.003(2) -0.015(2) -0.009(2) B2 0.034(3) 0.029(3) 0.037(2) -0.006(2) -0.014(2) -0.004(2) C11 0.032(2) 0.035(2) 0.033(2) -0.0061(19) -0.0073(18) -0.010(2) C12 0.040(3) 0.054(3) 0.032(2) -0.011(2) -0.015(2) -0.009(2) C13 0.042(3) 0.053(3) 0.038(2) -0.017(2) -0.014(2) -0.009(2) C14 0.044(3) 0.036(3) 0.055(3) -0.012(2) -0.014(2) 0.003(2) C15 0.070(4) 0.052(3) 0.070(3) -0.031(3) -0.026(3) 0.018(3) C16 0.046(3) 0.068(4) 0.068(3) -0.020(3) -0.022(3) -0.001(3) C17 0.095(5) 0.038(3) 0.070(4) 0.007(3) -0.025(3) -0.012(3) C21 0.036(2) 0.042(3) 0.033(2) -0.0070(19) -0.0133(19) -0.008(2) C22 0.033(3) 0.056(3) 0.047(3) -0.002(2) -0.019(2) -0.014(2) C23 0.035(3) 0.058(3) 0.047(3) -0.003(2) -0.025(2) -0.008(2) C24 0.053(3) 0.050(3) 0.033(2) 0.002(2) -0.014(2) -0.012(3) C25 0.079(5) 0.101(5) 0.046(3) 0.010(3) 0.015(3) 0.007(4) C26 0.161(7) 0.070(4) 0.064(4) 0.018(3) -0.049(4) -0.066(5) C27 0.083(4) 0.065(4) 0.045(3) 0.010(3) -0.027(3) -0.015(3) C31 0.031(2) 0.035(2) 0.031(2) -0.0063(18) -0.0132(18) -0.007(2) C32 0.046(3) 0.045(3) 0.045(2) -0.020(2) -0.009(2) -0.012(2) C33 0.050(3) 0.042(3) 0.049(3) -0.012(2) -0.013(2) -0.018(2) C34 0.038(3) 0.057(3) 0.037(2) -0.004(2) -0.009(2) -0.016(2) C35 0.060(4) 0.076(4) 0.063(3) -0.009(3) 0.001(3) -0.037(3) C36 0.067(4) 0.140(6) 0.033(3) -0.003(3) -0.015(3) -0.047(4) C37 0.033(3) 0.080(4) 0.077(4) -0.024(3) 0.000(3) -0.012(3) C41 0.039(3) 0.030(2) 0.041(2) -0.015(2) -0.014(2) 0.000(2) C42 0.034(3) 0.053(3) 0.058(3) -0.004(3) -0.013(2) -0.012(2) C43 0.038(3) 0.060(3) 0.065(3) -0.014(3) -0.026(3) 0.000(3) C44 0.061(3) 0.052(3) 0.039(2) -0.007(2) -0.025(2) 0.001(3) C45 0.071(4) 0.090(5) 0.062(3) 0.003(3) -0.037(3) 0.007(4) C46 0.114(5) 0.036(3) 0.071(4) 0.007(3) -0.052(4) -0.010(3) C47 0.079(4) 0.093(5) 0.045(3) -0.020(3) -0.022(3) -0.011(4) C51 0.036(2) 0.029(2) 0.040(2) -0.0069(19) -0.014(2) -0.004(2) C52 0.048(3) 0.031(2) 0.049(3) -0.010(2) -0.012(2) -0.013(2) C53 0.054(3) 0.035(3) 0.051(3) -0.008(2) -0.006(2) -0.019(2) C54 0.060(3) 0.049(3) 0.052(3) -0.016(3) 0.010(3) -0.019(3) C55 0.111(6) 0.080(5) 0.075(4) -0.029(4) 0.041(4) -0.051(4) C56 0.051(4) 0.066(4) 0.097(5) -0.032(4) 0.003(3) 0.004(3) C57 0.109(5) 0.063(4) 0.051(3) -0.019(3) -0.017(3) -0.009(4) C61 0.034(2) 0.029(2) 0.038(2) -0.0086(19) -0.0124(19) -0.003(2) C62 0.044(3) 0.042(3) 0.040(2) -0.013(2) -0.019(2) -0.008(2) C63 0.044(3) 0.041(3) 0.041(2) -0.017(2) -0.012(2) -0.010(2) C64 0.033(2) 0.030(2) 0.057(3) -0.015(2) -0.012(2) 0.000(2) C65 0.061(4) 0.043(3) 0.083(4) -0.030(3) -0.020(3) 0.004(3) C66 0.037(3) 0.047(3) 0.099(4) -0.024(3) -0.024(3) -0.002(2) C67 0.064(4) 0.041(3) 0.063(3) 0.004(3) -0.019(3) -0.006(3) C101 0.138(11) 0.175(14) 0.222(17) -0.120(15) -0.099(11) 0.000(11) C102 0.232(18) 0.135(12) 0.126(9) -0.061(8) -0.041(12) -0.019(12) C103 0.122(9) 0.100(9) 0.223(17) -0.075(10) -0.021(10) -0.010(8) C104 0.27(2) 0.073(7) 0.222(18) -0.004(10) -0.126(16) -0.034(11) C105 0.40(3) 0.144(14) 0.118(10) -0.033(9) -0.022(15) -0.18(2) C106 0.161(13) 0.200(18) 0.187(16) -0.102(13) 0.033(12) -0.123(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl1 S1 2.9921(14) . ? Tl1 H1 3.10(3) . ? Tl1 S3 3.1109(12) 2_666 ? Tl1 S1 3.1242(12) 2_666 ? Tl2 H2 2.74(3) . ? Tl2 S5 2.9968(14) 2_755 ? Tl2 S4 3.1285(13) . ? S1 C11 1.713(4) . ? S1 Tl1 3.1242(12) 2_666 ? S2 C21 1.697(4) . ? S3 C31 1.700(4) . ? S3 Tl1 3.1109(12) 2_666 ? S4 C41 1.706(5) . ? S5 C51 1.717(4) . ? S5 Tl2 2.9968(14) 2_755 ? S6 C61 1.699(4) . ? N11 C11 1.356(5) . ? N11 C12 1.376(5) . ? N11 B1 1.563(6) . ? N12 C11 1.370(5) . ? N12 C13 1.380(5) . ? N12 C14 1.507(6) . ? N21 C21 1.352(5) . ? N21 C22 1.384(5) . ? N21 B1 1.558(5) . ? N22 C21 1.375(5) . ? N22 C23 1.380(5) . ? N22 C24 1.508(5) . ? N31 C31 1.372(5) . ? N31 C32 1.387(5) . ? N31 B1 1.568(6) . ? N32 C31 1.377(5) . ? N32 C33 1.379(5) . ? N32 C34 1.501(5) . ? N41 C41 1.364(5) . ? N41 C42 1.381(5) . ? N41 B2 1.572(6) . ? N42 C41 1.374(5) . ? N42 C43 1.383(6) . ? N42 C44 1.514(6) . ? N51 C51 1.352(5) . ? N51 C52 1.387(5) . ? N51 B2 1.563(6) . ? N52 C51 1.365(5) . ? N52 C53 1.387(6) . ? N52 C54 1.519(6) . ? N61 C61 1.360(5) . ? N61 C62 1.381(5) . ? N61 B2 1.546(6) . ? N62 C61 1.371(5) . ? N62 C63 1.383(5) . ? N62 C64 1.509(5) . ? B1 H1 1.17(3) . ? B2 H2 1.12(3) . ? C12 C13 1.341(6) . ? C14 C16 1.517(7) . ? C14 C17 1.518(7) . ? C14 C15 1.529(6) . ? C22 C23 1.330(6) . ? C24 C27 1.509(7) . ? C24 C25 1.510(7) . ? C24 C26 1.521(7) . ? C32 C33 1.337(6) . ? C34 C35 1.504(7) . ? C34 C36 1.522(6) . ? C34 C37 1.530(7) . ? C42 C43 1.333(6) . ? C44 C45 1.498(7) . ? C44 C46 1.509(7) . ? C44 C47 1.532(6) . ? C52 C53 1.331(6) . ? C54 C55 1.526(7) . ? C54 C56 1.525(7) . ? C54 C57 1.539(8) . ? C62 C63 1.336(6) . ? C64 C65 1.508(6) . ? C64 C66 1.518(6) . ? C64 C67 1.527(6) . ? C101 C106 1.238(17) . ? C101 C102 1.297(15) . ? C102 C103 1.296(16) . ? C103 C104 1.330(17) . ? C104 C105 1.42(2) . ? C105 C106 1.41(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 S1 Tl1 H1 58.3(6) . . ? S1 Tl1 S3 88.07(3) . 2_666 ? H1 Tl1 S3 144.5(5) . 2_666 ? S1 Tl1 S1 98.68(3) . 2_666 ? H1 Tl1 S1 64.9(6) . 2_666 ? S3 Tl1 S1 114.93(3) 2_666 2_666 ? H2 Tl2 S5 74.6(7) . 2_755 ? H2 Tl2 S4 61.0(7) . . ? S5 Tl2 S4 89.70(3) 2_755 . ? C11 S1 Tl1 92.31(15) . . ? C11 S1 Tl1 119.12(15) . 2_666 ? Tl1 S1 Tl1 81.32(3) . 2_666 ? C31 S3 Tl1 82.46(14) . 2_666 ? C41 S4 Tl2 82.51(14) . . ? C51 S5 Tl2 95.35(15) . 2_755 ? C11 N11 C12 108.2(3) . . ? C11 N11 B1 126.8(3) . . ? C12 N11 B1 124.7(3) . . ? C11 N12 C13 107.8(3) . . ? C11 N12 C14 127.6(3) . . ? C13 N12 C14 124.6(4) . . ? C21 N21 C22 108.3(3) . . ? C21 N21 B1 124.4(3) . . ? C22 N21 B1 126.7(4) . . ? C21 N22 C23 108.1(3) . . ? C21 N22 C24 126.8(4) . . ? C23 N22 C24 124.9(3) . . ? C31 N31 C32 107.9(4) . . ? C31 N31 B1 126.7(4) . . ? C32 N31 B1 125.1(4) . . ? C31 N32 C33 108.1(3) . . ? C31 N32 C34 127.9(4) . . ? C33 N32 C34 123.6(4) . . ? C41 N41 C42 108.4(4) . . ? C41 N41 B2 125.9(4) . . ? C42 N41 B2 125.5(4) . . ? C41 N42 C43 107.8(4) . . ? C41 N42 C44 127.4(4) . . ? C43 N42 C44 124.5(4) . . ? C51 N51 C52 107.9(3) . . ? C51 N51 B2 127.2(4) . . ? C52 N51 B2 124.5(3) . . ? C51 N52 C53 108.4(4) . . ? C51 N52 C54 127.5(4) . . ? C53 N52 C54 123.9(4) . . ? C61 N61 C62 108.0(3) . . ? C61 N61 B2 124.7(3) . . ? C62 N61 B2 127.3(3) . . ? C61 N62 C63 107.9(3) . . ? C61 N62 C64 126.7(3) . . ? C63 N62 C64 125.4(3) . . ? H1 B1 N21 112.7(15) . . ? H1 B1 N11 111.2(15) . . ? N21 B1 N11 106.0(3) . . ? H1 B1 N31 110.8(15) . . ? N21 B1 N31 109.8(3) . . ? N11 B1 N31 105.9(3) . . ? H2 B2 N61 115.1(17) . . ? H2 B2 N51 110.1(17) . . ? N61 B2 N51 107.2(3) . . ? H2 B2 N41 108.6(17) . . ? N61 B2 N41 109.9(3) . . ? N51 B2 N41 105.5(3) . . ? N11 C11 N12 107.6(3) . . ? N11 C11 S1 125.6(3) . . ? N12 C11 S1 126.7(3) . . ? C13 C12 N11 108.4(4) . . ? C12 C13 N12 107.9(4) . . ? N12 C14 C16 110.1(4) . . ? N12 C14 C17 108.8(4) . . ? C16 C14 C17 111.5(5) . . ? N12 C14 C15 107.9(4) . . ? C16 C14 C15 109.0(4) . . ? C17 C14 C15 109.4(4) . . ? N21 C21 N22 107.2(4) . . ? N21 C21 S2 125.1(3) . . ? N22 C21 S2 127.7(3) . . ? C23 C22 N21 108.5(4) . . ? C22 C23 N22 108.0(4) . . ? N22 C24 C27 109.0(4) . . ? N22 C24 C25 108.9(4) . . ? C27 C24 C25 108.2(4) . . ? N22 C24 C26 109.9(4) . . ? C27 C24 C26 108.9(5) . . ? C25 C24 C26 111.8(5) . . ? N31 C31 N32 107.1(3) . . ? N31 C31 S3 124.2(3) . . ? N32 C31 S3 128.7(3) . . ? C33 C32 N31 108.4(4) . . ? C32 C33 N32 108.4(4) . . ? N32 C34 C35 109.9(4) . . ? N32 C34 C36 107.4(4) . . ? C35 C34 C36 110.5(4) . . ? N32 C34 C37 109.2(4) . . ? C35 C34 C37 108.7(4) . . ? C36 C34 C37 111.1(5) . . ? N41 C41 N42 107.1(4) . . ? N41 C41 S4 124.3(3) . . ? N42 C41 S4 128.7(3) . . ? C43 C42 N41 108.1(4) . . ? C42 C43 N42 108.6(4) . . ? C45 C44 C46 109.6(5) . . ? C45 C44 N42 108.9(4) . . ? C46 C44 N42 108.6(4) . . ? C45 C44 C47 109.1(4) . . ? C46 C44 C47 112.1(5) . . ? N42 C44 C47 108.4(4) . . ? N51 C51 N52 107.5(4) . . ? N51 C51 S5 125.3(3) . . ? N52 C51 S5 127.2(3) . . ? C53 C52 N51 108.8(4) . . ? C52 C53 N52 107.3(4) . . ? N52 C54 C55 108.4(4) . . ? N52 C54 C56 108.4(4) . . ? C55 C54 C56 110.0(5) . . ? N52 C54 C57 108.6(4) . . ? C55 C54 C57 109.0(5) . . ? C56 C54 C57 112.4(5) . . ? N61 C61 N62 107.5(3) . . ? N61 C61 S6 124.3(3) . . ? N62 C61 S6 128.2(3) . . ? C63 C62 N61 108.6(4) . . ? C62 C63 N62 108.0(4) . . ? C65 C64 N62 108.8(4) . . ? C65 C64 C66 108.5(4) . . ? N62 C64 C66 109.0(4) . . ? C65 C64 C67 108.9(4) . . ? N62 C64 C67 109.6(4) . . ? C66 C64 C67 112.1(4) . . ? C106 C101 C102 122.1(17) . . ? C103 C102 C101 123.0(15) . . ? C102 C103 C104 119.3(14) . . ? C103 C104 C105 119.4(16) . . ? C106 C105 C104 114.7(16) . . ? C101 C106 C105 121.3(18) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.051 _refine_diff_density_min -1.140 _refine_diff_density_rms 0.089 # Attachment 'k2-Tm2InCl_-_TINCS10P.CIF' data_tincs10p _database_code_depnum_ccdc_archive 'CCDC 680248' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H77 B2 Cl In N12 S6' _chemical_formula_weight 1222.50 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.367(3) _cell_length_b 11.6180(14) _cell_length_c 19.433(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.393(2) _cell_angle_gamma 90.00 _cell_volume 6230.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 3580 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.26 _exptl_crystal_description Needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2556 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9363 _exptl_absorpt_correction_T_max 0.9868 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 49218 _diffrn_reflns_av_R_equivalents 0.1076 _diffrn_reflns_av_sigmaI/netI 0.0971 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 30.60 _reflns_number_total 9575 _reflns_number_gt 5763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9575 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.250 -0.250 0.500 320.1 63.1 2 0.250 0.250 1.000 320.2 63.1 3 0.750 -0.250 0.000 320.1 63.1 4 0.750 0.250 0.500 320.1 63.1 _platon_squeeze_details ; The unite cell contains 6 benzene molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; 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 In In 0.0000 0.75858(2) 0.7500 0.02318(8) Uani 1 2 d S . . Cl Cl 0.0000 0.54654(8) 0.7500 0.0376(3) Uani 1 2 d S . . B B 0.08389(11) 0.9868(3) 0.70895(16) 0.0275(7) Uani 1 1 d . . . H1 H 0.0460(8) 0.9831(18) 0.7225(11) 0.019(6) Uiso 1 1 d . . . S1 S 0.05811(2) 0.86478(6) 0.84699(3) 0.02946(17) Uani 1 1 d . . . S2 S 0.05583(2) 0.72057(6) 0.66259(3) 0.02863(17) Uani 1 1 d . . . S3 S 0.18424(3) 1.11582(6) 0.67273(4) 0.03166(17) Uani 1 1 d . . . N11 N 0.11984(7) 0.90592(19) 0.75965(11) 0.0268(5) Uani 1 1 d . . . C11 C 0.11093(9) 0.8529(2) 0.81704(13) 0.0262(6) Uani 1 1 d . . . N12 N 0.14972(7) 0.78515(18) 0.84556(11) 0.0266(5) Uani 1 1 d . . . C12 C 0.16428(9) 0.8685(2) 0.75102(14) 0.0295(6) Uani 1 1 d . . . H12A H 0.1791 0.8908 0.7140 0.035 Uiso 1 1 calc R . . C13 C 0.18309(10) 0.7952(2) 0.80394(14) 0.0307(7) Uani 1 1 d . . . H13A H 0.2136 0.7574 0.8113 0.037 Uiso 1 1 calc R . . C14 C 0.15837(10) 0.7193(2) 0.91472(14) 0.0334(7) Uani 1 1 d . . . C15 C 0.20770(10) 0.6605(3) 0.92579(15) 0.0431(8) Uani 1 1 d . . . H15A H 0.2330 0.7189 0.9286 0.065 Uiso 1 1 calc R . . H15B H 0.2078 0.6087 0.8860 0.065 Uiso 1 1 calc R . . H15C H 0.2140 0.6161 0.9699 0.065 Uiso 1 1 calc R . . C16 C 0.15929(12) 0.8056(3) 0.97389(14) 0.0447(8) Uani 1 1 d . . . H16A H 0.1850 0.8621 0.9746 0.067 Uiso 1 1 calc R . . H16B H 0.1654 0.7651 1.0193 0.067 Uiso 1 1 calc R . . H16C H 0.1280 0.8452 0.9659 0.067 Uiso 1 1 calc R . . C17 C 0.11954(11) 0.6268(2) 0.91129(15) 0.0406(8) Uani 1 1 d . . . H17A H 0.1208 0.5725 0.8732 0.061 Uiso 1 1 calc R . . H17B H 0.0875 0.6631 0.9020 0.061 Uiso 1 1 calc R . . H17C H 0.1254 0.5855 0.9565 0.061 Uiso 1 1 calc R . . N21 N 0.07705(7) 0.94318(18) 0.63140(11) 0.0256(5) Uani 1 1 d . . . C21 C 0.06099(9) 0.8364(2) 0.60910(13) 0.0259(6) Uani 1 1 d . . . N22 N 0.05074(7) 0.83564(19) 0.53659(10) 0.0264(5) Uani 1 1 d . . . C22 C 0.07617(10) 1.0098(2) 0.57232(13) 0.0303(6) Uani 1 1 d . . . H22A H 0.0853 1.0885 0.5725 0.036 Uiso 1 1 calc R . . C23 C 0.06014(9) 0.9445(2) 0.51459(14) 0.0304(7) Uani 1 1 d . . . H23A H 0.0560 0.9690 0.4669 0.036 Uiso 1 1 calc R . . C24 C 0.03434(10) 0.7344(2) 0.48816(13) 0.0323(6) Uani 1 1 d . . . C25 C 0.07226(11) 0.6405(3) 0.50323(15) 0.0452(8) Uani 1 1 d . . . H25A H 0.0715 0.6027 0.5480 0.068 Uiso 1 1 calc R . . H25B H 0.1044 0.6742 0.5065 0.068 Uiso 1 1 calc R . . H25C H 0.0655 0.5837 0.4649 0.068 Uiso 1 1 calc R . . C26 C 0.02849(11) 0.7753(3) 0.41138(13) 0.0411(8) Uani 1 1 d . . . H26A H 0.0597 0.8038 0.4048 0.062 Uiso 1 1 calc R . . H26B H 0.0044 0.8373 0.4014 0.062 Uiso 1 1 calc R . . H26C H 0.0176 0.7109 0.3790 0.062 Uiso 1 1 calc R . . C27 C -0.01458(11) 0.6923(3) 0.49775(15) 0.0422(8) Uani 1 1 d . . . H27A H -0.0100 0.6490 0.5421 0.063 Uiso 1 1 calc R . . H27B H -0.0295 0.6423 0.4580 0.063 Uiso 1 1 calc R . . H27C H -0.0357 0.7585 0.4993 0.063 Uiso 1 1 calc R . . C31 C 0.13810(9) 1.1739(2) 0.70308(13) 0.0254(6) Uani 1 1 d . . . N31 N 0.09912(7) 1.11404(19) 0.71621(10) 0.0267(5) Uani 1 1 d . . . N32 N 0.13158(8) 1.28733(18) 0.71848(11) 0.0285(5) Uani 1 1 d . . . C32 C 0.07020(10) 1.1922(3) 0.74140(14) 0.0339(7) Uani 1 1 d . . . H32A H 0.0412 1.1737 0.7556 0.041 Uiso 1 1 calc R . . C33 C 0.08927(10) 1.2974(3) 0.74257(14) 0.0366(7) Uani 1 1 d . . . H33A H 0.0764 1.3663 0.7571 0.044 Uiso 1 1 calc R . . C34 C 0.16482(11) 1.3862(2) 0.71359(15) 0.0362(7) Uani 1 1 d . . . C35 C 0.17198(14) 1.3961(3) 0.63830(17) 0.0630(11) Uani 1 1 d . . . H35A H 0.1406 1.4091 0.6054 0.095 Uiso 1 1 calc R . . H35B H 0.1863 1.3247 0.6256 0.095 Uiso 1 1 calc R . . H35C H 0.1936 1.4608 0.6356 0.095 Uiso 1 1 calc R . . C36 C 0.14197(13) 1.4973(3) 0.7322(2) 0.0666(11) Uani 1 1 d . . . H36A H 0.1113 1.5109 0.6978 0.100 Uiso 1 1 calc R . . H36B H 0.1641 1.5618 0.7312 0.100 Uiso 1 1 calc R . . H36C H 0.1359 1.4906 0.7797 0.100 Uiso 1 1 calc R . . C37 C 0.21262(10) 1.3674(3) 0.76669(15) 0.0420(8) Uani 1 1 d . . . H37A H 0.2277 1.2963 0.7550 0.063 Uiso 1 1 calc R . . H37B H 0.2068 1.3610 0.8143 0.063 Uiso 1 1 calc R . . H37C H 0.2342 1.4326 0.7650 0.063 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 In 0.02003(13) 0.02929(17) 0.01873(13) 0.000 0.00145(10) 0.000 Cl 0.0432(6) 0.0274(6) 0.0477(6) 0.000 0.0216(5) 0.000 B 0.0238(17) 0.0369(19) 0.0209(16) 0.0037(14) 0.0036(13) 0.0004(14) S1 0.0231(4) 0.0463(5) 0.0174(3) -0.0020(3) 0.0015(3) -0.0030(3) S2 0.0317(4) 0.0300(4) 0.0252(4) 0.0056(3) 0.0086(3) 0.0054(3) S3 0.0315(4) 0.0330(4) 0.0338(4) -0.0040(3) 0.0143(3) 0.0013(3) N11 0.0214(12) 0.0385(14) 0.0198(12) 0.0033(10) 0.0034(10) -0.0020(10) C11 0.0190(13) 0.0387(16) 0.0172(13) -0.0022(12) -0.0030(11) -0.0033(12) N12 0.0200(11) 0.0363(14) 0.0203(11) 0.0045(9) -0.0018(9) -0.0015(10) C12 0.0236(15) 0.0382(18) 0.0261(15) 0.0036(13) 0.0046(12) -0.0024(12) C13 0.0225(14) 0.0394(17) 0.0278(15) 0.0047(12) 0.0007(12) 0.0009(12) C14 0.0326(16) 0.0425(19) 0.0218(14) 0.0098(13) -0.0006(12) 0.0007(13) C15 0.0402(18) 0.055(2) 0.0313(17) 0.0138(15) 0.0018(14) 0.0059(16) C16 0.049(2) 0.058(2) 0.0201(15) 0.0030(14) -0.0058(14) 0.0028(16) C17 0.0413(18) 0.046(2) 0.0349(17) 0.0102(14) 0.0104(15) -0.0019(15) N21 0.0234(12) 0.0321(13) 0.0192(11) 0.0060(10) 0.0009(9) 0.0019(10) C21 0.0224(14) 0.0318(16) 0.0226(14) 0.0040(12) 0.0031(11) 0.0055(12) N22 0.0238(12) 0.0343(14) 0.0188(11) 0.0018(10) 0.0003(9) 0.0002(10) C22 0.0326(16) 0.0312(16) 0.0253(15) 0.0056(13) 0.0030(13) 0.0002(13) C23 0.0322(16) 0.0333(17) 0.0222(14) 0.0098(12) -0.0005(12) 0.0000(13) C24 0.0359(16) 0.0320(17) 0.0263(14) -0.0010(13) 0.0021(12) -0.0035(14) C25 0.058(2) 0.044(2) 0.0309(17) -0.0068(15) 0.0046(16) 0.0088(17) C26 0.0479(18) 0.047(2) 0.0240(15) -0.0040(14) 0.0002(13) -0.0064(15) C27 0.0434(19) 0.0443(19) 0.0333(17) -0.0003(14) -0.0024(15) -0.0091(15) C31 0.0275(15) 0.0312(16) 0.0158(13) -0.0009(11) 0.0016(11) 0.0050(12) N31 0.0212(12) 0.0401(14) 0.0174(11) -0.0042(10) 0.0015(9) 0.0043(10) N32 0.0266(12) 0.0304(14) 0.0260(12) -0.0050(10) 0.0009(10) 0.0047(10) C32 0.0232(15) 0.053(2) 0.0237(15) -0.0069(14) 0.0018(12) 0.0083(14) C33 0.0302(17) 0.0450(19) 0.0303(16) -0.0126(14) -0.0016(13) 0.0148(14) C34 0.0434(18) 0.0312(17) 0.0330(17) -0.0025(13) 0.0068(15) 0.0027(14) C35 0.099(3) 0.047(2) 0.041(2) 0.0093(17) 0.014(2) -0.006(2) C36 0.067(3) 0.038(2) 0.091(3) -0.012(2) 0.010(2) 0.0122(19) C37 0.0368(18) 0.045(2) 0.0435(19) -0.0073(15) 0.0076(15) -0.0051(15) _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 In Cl 2.4636(10) . ? In S1 2.5204(7) . ? In S1 2.5204(7) 2_556 ? In S2 2.6143(7) . ? In S2 2.6143(7) 2_556 ? B H1 1.16(2) . ? B N31 1.538(4) . ? B N11 1.558(4) . ? B N21 1.559(4) . ? S1 C11 1.734(3) . ? S2 C21 1.727(3) . ? S3 C31 1.695(3) . ? N11 C11 1.348(3) . ? N11 C12 1.380(3) . ? C11 N12 1.362(3) . ? N12 C13 1.385(3) . ? N12 C14 1.516(3) . ? C12 C13 1.347(3) . ? C14 C16 1.521(4) . ? C14 C15 1.527(4) . ? C14 C17 1.530(4) . ? N21 C21 1.357(3) . ? N21 C22 1.380(3) . ? C21 N22 1.371(3) . ? N22 C23 1.381(3) . ? N22 C24 1.511(3) . ? C22 C23 1.343(3) . ? C24 C25 1.512(4) . ? C24 C27 1.523(4) . ? C24 C26 1.538(3) . ? C31 N32 1.373(3) . ? C31 N31 1.379(3) . ? N31 C32 1.387(3) . ? N32 C33 1.391(3) . ? N32 C34 1.503(3) . ? C32 C33 1.335(4) . ? C34 C37 1.518(4) . ? C34 C36 1.525(4) . ? C34 C35 1.527(4) . ? 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 Cl In S1 119.307(18) . . ? Cl In S1 119.307(18) . 2_556 ? S1 In S1 121.39(4) . 2_556 ? Cl In S2 80.273(16) . . ? S1 In S2 100.31(2) . . ? S1 In S2 89.23(2) 2_556 . ? Cl In S2 80.273(16) . 2_556 ? S1 In S2 89.23(2) . 2_556 ? S1 In S2 100.31(2) 2_556 2_556 ? S2 In S2 160.55(3) . 2_556 ? H1 B N31 105.6(11) . . ? H1 B N11 109.8(11) . . ? N31 B N11 113.1(2) . . ? H1 B N21 107.0(11) . . ? N31 B N21 111.7(2) . . ? N11 B N21 109.4(2) . . ? C11 S1 In 100.17(8) . . ? C21 S2 In 114.08(9) . . ? C11 N11 C12 108.0(2) . . ? C11 N11 B 125.3(2) . . ? C12 N11 B 126.5(2) . . ? N11 C11 N12 108.2(2) . . ? N11 C11 S1 125.7(2) . . ? N12 C11 S1 126.1(2) . . ? C11 N12 C13 108.1(2) . . ? C11 N12 C14 127.0(2) . . ? C13 N12 C14 124.6(2) . . ? C13 C12 N11 108.5(2) . . ? C12 C13 N12 107.2(2) . . ? N12 C14 C16 108.0(2) . . ? N12 C14 C15 107.8(2) . . ? C16 C14 C15 109.5(2) . . ? N12 C14 C17 110.4(2) . . ? C16 C14 C17 112.5(2) . . ? C15 C14 C17 108.6(2) . . ? C21 N21 C22 107.9(2) . . ? C21 N21 B 124.3(2) . . ? C22 N21 B 126.6(2) . . ? N21 C21 N22 108.0(2) . . ? N21 C21 S2 126.08(19) . . ? N22 C21 S2 125.9(2) . . ? C21 N22 C23 107.6(2) . . ? C21 N22 C24 127.3(2) . . ? C23 N22 C24 125.0(2) . . ? C23 C22 N21 108.4(2) . . ? C22 C23 N22 108.1(2) . . ? N22 C24 C25 109.8(2) . . ? N22 C24 C27 109.4(2) . . ? C25 C24 C27 111.9(2) . . ? N22 C24 C26 108.2(2) . . ? C25 C24 C26 108.9(2) . . ? C27 C24 C26 108.7(2) . . ? N32 C31 N31 106.8(2) . . ? N32 C31 S3 127.7(2) . . ? N31 C31 S3 125.5(2) . . ? C31 N31 C32 107.5(2) . . ? C31 N31 B 133.5(2) . . ? C32 N31 B 119.0(2) . . ? C31 N32 C33 108.9(2) . . ? C31 N32 C34 127.0(2) . . ? C33 N32 C34 124.1(2) . . ? C33 C32 N31 109.6(3) . . ? C32 C33 N32 107.2(2) . . ? N32 C34 C37 108.8(2) . . ? N32 C34 C36 108.9(3) . . ? C37 C34 C36 108.8(2) . . ? N32 C34 C35 110.0(2) . . ? C37 C34 C35 111.5(3) . . ? C36 C34 C35 108.8(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.60 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.620 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.091 # Attachment 'k2-Tm2InN3_-_ky_Tm2InN3_.cif' data_kyb _database_code_depnum_ccdc_archive 'CCDC 680249' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H80 B2 In N15 S6' _chemical_formula_weight 1268.13 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.0261(17) _cell_length_b 12.0762(8) _cell_length_c 19.4918(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.905(2) _cell_angle_gamma 90.00 _cell_volume 6455.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 3019 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.65 _exptl_crystal_description Needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9418 _exptl_absorpt_correction_T_max 0.9880 _exptl_absorpt_process_details sadabs _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 22743 _diffrn_reflns_av_R_equivalents 0.1027 _diffrn_reflns_av_sigmaI/netI 0.1582 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.27 _reflns_number_total 7555 _reflns_number_gt 3617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7555 _refine_ls_number_parameters 355 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1675 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.003 _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 In In 0.0000 0.77055(3) 0.2500 0.03490(14) Uani 1 2 d S . . B B 0.08459(17) 0.9847(5) 0.2091(2) 0.0424(14) Uani 1 1 d . . . H1 H 0.0500(11) 0.976(2) 0.2218(15) 0.038(10) Uiso 1 1 d . . . S1 S 0.05833(3) 0.86647(9) 0.34709(5) 0.0427(3) Uani 1 1 d . . . S2 S 0.05829(4) 0.72989(9) 0.16372(5) 0.0435(3) Uani 1 1 d . . . S3 S 0.18243(4) 1.12097(10) 0.17076(6) 0.0581(4) Uani 1 1 d . . . N1 N -0.0082(3) 0.5860(4) 0.2394(3) 0.0301(15) Uiso 0.50 1 d PD . . N2 N 0.0064(3) 0.5310(5) 0.2890(3) 0.057(2) Uiso 0.50 1 d PD . . N3 N 0.0142(3) 0.4753(7) 0.3386(4) 0.118(3) Uiso 0.50 1 d PD . . N11 N 0.12054(10) 0.9096(3) 0.25865(15) 0.0374(8) Uani 1 1 d . . . C11 C 0.11217(13) 0.8569(3) 0.31589(19) 0.0358(10) Uani 1 1 d . . . C12 C 0.16552(13) 0.8746(3) 0.2486(2) 0.0453(12) Uani 1 1 d . . . H12A H 0.1806 0.8974 0.2121 0.054 Uiso 1 1 calc R . . N12 N 0.15039(11) 0.7912(3) 0.34207(15) 0.0397(9) Uani 1 1 d . . . C13 C 0.18412(14) 0.8028(3) 0.2993(2) 0.0470(12) Uani 1 1 d . . . H13A H 0.2144 0.7669 0.3051 0.056 Uiso 1 1 calc R . . C14 C 0.15888(14) 0.7245(4) 0.4089(2) 0.0466(11) Uani 1 1 d . . . C15 C 0.11983(16) 0.6358(4) 0.4040(2) 0.0658(14) Uani 1 1 d . . . H15A H 0.0881 0.6706 0.3984 0.099 Uiso 1 1 calc R . . H15B H 0.1260 0.5916 0.4465 0.099 Uiso 1 1 calc R . . H15C H 0.1205 0.5885 0.3640 0.099 Uiso 1 1 calc R . . C16 C 0.15860(17) 0.8016(4) 0.4701(2) 0.0721(15) Uani 1 1 d . . . H16A H 0.1270 0.8375 0.4641 0.108 Uiso 1 1 calc R . . H16B H 0.1838 0.8573 0.4719 0.108 Uiso 1 1 calc R . . H16C H 0.1648 0.7595 0.5134 0.108 Uiso 1 1 calc R . . C17 C 0.20879(15) 0.6685(4) 0.4185(2) 0.0764(16) Uani 1 1 d . . . H17A H 0.2340 0.7245 0.4219 0.115 Uiso 1 1 calc R . . H17B H 0.2095 0.6210 0.3785 0.115 Uiso 1 1 calc R . . H17C H 0.2146 0.6243 0.4610 0.115 Uiso 1 1 calc R . . N21 N 0.07843(10) 0.9440(3) 0.13211(16) 0.0354(8) Uani 1 1 d . . . C21 C 0.06310(12) 0.8415(3) 0.1097(2) 0.0341(10) Uani 1 1 d . . . N22 N 0.05380(11) 0.8403(3) 0.03834(17) 0.0402(9) Uani 1 1 d . . . C22 C 0.07779(14) 1.0083(4) 0.0734(2) 0.0466(11) Uani 1 1 d . . . H22A H 0.0862 1.0836 0.0733 0.056 Uiso 1 1 calc R . . C23 C 0.06319(14) 0.9450(4) 0.0169(2) 0.0496(12) Uani 1 1 d . . . H23A H 0.0599 0.9683 -0.0299 0.059 Uiso 1 1 calc R . . C24 C 0.03840(15) 0.7439(4) -0.0099(2) 0.0501(12) Uani 1 1 d . . . C25 C 0.03221(17) 0.7834(4) -0.0860(2) 0.0760(15) Uani 1 1 d . . . H25A H 0.0067 0.8390 -0.0955 0.114 Uiso 1 1 calc R . . H25B H 0.0234 0.7211 -0.1174 0.114 Uiso 1 1 calc R . . H25C H 0.0626 0.8151 -0.0931 0.114 Uiso 1 1 calc R . . C26 C -0.01049(15) 0.6988(4) 0.0007(2) 0.0654(14) Uani 1 1 d . . . H26A H -0.0350 0.7566 -0.0092 0.098 Uiso 1 1 calc R . . H26B H -0.0073 0.6742 0.0488 0.098 Uiso 1 1 calc R . . H26C H -0.0203 0.6369 -0.0308 0.098 Uiso 1 1 calc R . . C27 C 0.07816(17) 0.6557(4) 0.0046(2) 0.0763(16) Uani 1 1 d . . . H27A H 0.1086 0.6868 -0.0030 0.114 Uiso 1 1 calc R . . H27B H 0.0689 0.5935 -0.0268 0.114 Uiso 1 1 calc R . . H27C H 0.0823 0.6308 0.0527 0.114 Uiso 1 1 calc R . . N31 N 0.09720(11) 1.1088(3) 0.21693(15) 0.0393(9) Uani 1 1 d . . . C31 C 0.13475(14) 1.1711(4) 0.20226(19) 0.0389(11) Uani 1 1 d . . . N32 N 0.12635(12) 1.2797(3) 0.21878(17) 0.0498(9) Uani 1 1 d . . . C32 C 0.06705(15) 1.1790(4) 0.2454(2) 0.0533(13) Uani 1 1 d . . . H32A H 0.0391 1.1573 0.2616 0.064 Uiso 1 1 calc R . . C33 C 0.08401(15) 1.2816(4) 0.2459(2) 0.0596(13) Uani 1 1 d . . . H33A H 0.0699 1.3447 0.2618 0.072 Uiso 1 1 calc R . . C34 C 0.15629(19) 1.3788(4) 0.2109(3) 0.0624(14) Uani 1 1 d . . . C35 C 0.13020(18) 1.4819(4) 0.2287(3) 0.110(2) Uani 1 1 d . . . H35A H 0.1258 1.4771 0.2767 0.165 Uiso 1 1 calc R . . H35B H 0.0986 1.4875 0.1972 0.165 Uiso 1 1 calc R . . H35C H 0.1495 1.5468 0.2234 0.165 Uiso 1 1 calc R . . C36 C 0.20441(17) 1.3696(4) 0.2617(3) 0.0862(17) Uani 1 1 d . . . H36A H 0.1988 1.3645 0.3091 0.129 Uiso 1 1 calc R . . H36B H 0.2240 1.4345 0.2577 0.129 Uiso 1 1 calc R . . H36C H 0.2214 1.3038 0.2512 0.129 Uiso 1 1 calc R . . C37 C 0.1626(2) 1.3876(4) 0.1352(3) 0.110(2) Uani 1 1 d . . . H37A H 0.1794 1.3224 0.1233 0.165 Uiso 1 1 calc R . . H37B H 0.1816 1.4531 0.1300 0.165 Uiso 1 1 calc R . . H37C H 0.1309 1.3929 0.1041 0.165 Uiso 1 1 calc R . . C101 C 0.1882(4) 1.0923(7) 0.4815(8) 0.149(4) Uani 1 1 d . . . H10A H 0.1616 1.0824 0.5034 0.179 Uiso 1 1 calc R . . C102 C 0.1805(5) 1.1000(14) 0.4072(12) 0.241(12) Uani 1 1 d . . . H10B H 0.1493 1.0964 0.3781 0.289 Uiso 1 1 calc R . . C103 C 0.2199(7) 1.1124(13) 0.3825(8) 0.245(13) Uani 1 1 d . . . H10C H 0.2163 1.1156 0.3335 0.293 Uiso 1 1 calc R . . C104 C 0.2622(6) 1.1205(8) 0.4189(8) 0.183(7) Uani 1 1 d . . . H10D H 0.2885 1.1327 0.3966 0.219 Uiso 1 1 calc R . . C105 C 0.2708(3) 1.1120(6) 0.4892(8) 0.142(4) Uani 1 1 d . . . H10E H 0.3028 1.1152 0.5159 0.170 Uiso 1 1 calc R . . C106 C 0.2334(5) 1.0992(5) 0.5199(4) 0.117(2) Uani 1 1 d . . . H10F H 0.2386 1.0948 0.5690 0.140 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 In 0.0314(2) 0.0411(3) 0.0325(3) 0.000 0.00740(19) 0.000 B 0.030(3) 0.065(4) 0.034(3) 0.003(3) 0.011(2) -0.003(3) S1 0.0340(6) 0.0676(9) 0.0267(6) -0.0027(6) 0.0067(5) -0.0035(6) S2 0.0496(7) 0.0428(7) 0.0423(7) 0.0081(6) 0.0191(5) 0.0086(6) S3 0.0573(8) 0.0567(9) 0.0712(9) -0.0074(7) 0.0389(7) -0.0043(6) N11 0.030(2) 0.054(2) 0.028(2) 0.0086(18) 0.0042(16) 0.0027(17) C11 0.028(2) 0.052(3) 0.026(2) 0.004(2) 0.0005(19) -0.003(2) C12 0.026(2) 0.065(3) 0.046(3) 0.011(3) 0.010(2) 0.003(2) N12 0.036(2) 0.052(3) 0.029(2) 0.0107(18) 0.0024(16) 0.0003(18) C13 0.033(2) 0.062(4) 0.048(3) 0.011(2) 0.012(2) 0.006(2) C14 0.044(3) 0.052(3) 0.039(3) 0.012(3) -0.002(2) -0.006(3) C15 0.076(4) 0.060(4) 0.063(3) 0.019(3) 0.018(3) 0.000(3) C16 0.090(4) 0.086(4) 0.031(3) 0.005(3) -0.008(3) 0.008(3) C17 0.061(3) 0.100(4) 0.067(4) 0.038(3) 0.009(3) 0.023(3) N21 0.034(2) 0.039(2) 0.031(2) 0.0082(18) 0.0034(16) -0.0041(17) C21 0.027(2) 0.049(3) 0.028(3) 0.007(2) 0.0086(18) 0.005(2) N22 0.044(2) 0.047(3) 0.031(2) 0.0032(19) 0.0096(17) -0.0036(18) C22 0.056(3) 0.045(3) 0.039(3) 0.013(3) 0.010(2) -0.001(2) C23 0.061(3) 0.056(4) 0.032(3) 0.008(3) 0.008(2) -0.003(3) C24 0.056(3) 0.053(4) 0.042(3) -0.004(3) 0.013(2) 0.003(3) C25 0.099(4) 0.094(4) 0.035(3) -0.011(3) 0.014(3) -0.014(3) C26 0.062(3) 0.073(4) 0.060(3) -0.010(3) 0.008(3) -0.015(3) C27 0.083(4) 0.073(4) 0.079(4) -0.009(3) 0.031(3) 0.024(3) N31 0.029(2) 0.055(3) 0.034(2) 0.0003(18) 0.0078(16) 0.0030(18) C31 0.039(3) 0.050(3) 0.028(3) 0.000(2) 0.006(2) -0.001(2) N32 0.047(2) 0.050(3) 0.054(2) -0.010(2) 0.0134(18) 0.006(2) C32 0.033(3) 0.074(4) 0.055(3) -0.007(3) 0.012(2) 0.009(3) C33 0.048(3) 0.063(4) 0.069(3) -0.017(3) 0.014(3) 0.015(3) C34 0.073(4) 0.043(3) 0.073(4) -0.013(3) 0.019(3) -0.005(3) C35 0.104(5) 0.054(4) 0.173(6) -0.026(4) 0.034(4) 0.005(3) C36 0.066(4) 0.089(5) 0.104(5) -0.026(4) 0.018(4) -0.024(3) C37 0.191(7) 0.056(4) 0.090(5) 0.004(3) 0.045(4) -0.031(4) C101 0.091(8) 0.094(6) 0.270(13) -0.020(9) 0.056(8) -0.011(6) C102 0.177(13) 0.097(8) 0.36(3) -0.059(12) -0.160(17) 0.025(9) C103 0.39(3) 0.149(12) 0.117(9) -0.057(8) -0.121(15) 0.099(18) C104 0.32(2) 0.094(7) 0.182(11) 0.037(9) 0.172(13) 0.064(10) C105 0.064(5) 0.084(6) 0.264(15) 0.036(8) 0.003(7) 0.013(4) C106 0.153(8) 0.080(5) 0.105(6) 0.004(4) -0.007(7) 0.004(6) _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 In N1 2.245(5) . ? In N1 2.245(5) 2 ? In S1 2.5137(11) 2 ? In S1 2.5137(11) . ? In S2 2.6215(9) . ? In S2 2.6215(9) 2 ? B H1 1.05(3) . ? B N11 1.539(6) . ? B N31 1.541(6) . ? B N21 1.554(5) . ? S1 C11 1.743(4) . ? S2 C21 1.733(4) . ? S3 C31 1.693(4) . ? N1 N1 0.550(13) 2 ? N1 N2 0.872(8) 2 ? N1 N2 1.1744(10) . ? N2 N1 0.872(8) 2 ? N2 N3 1.1612(10) . ? N2 N2 1.487(13) 2 ? N11 C11 1.347(4) . ? N11 C12 1.382(4) . ? C11 N12 1.346(4) . ? C12 C13 1.337(5) . ? N12 C13 1.390(4) . ? N12 C14 1.509(5) . ? C14 C16 1.514(5) . ? C14 C15 1.520(5) . ? C14 C17 1.530(5) . ? N21 C21 1.353(4) . ? N21 C22 1.380(4) . ? C21 N22 1.361(4) . ? N22 C23 1.375(5) . ? N22 C24 1.503(5) . ? C22 C23 1.333(5) . ? C24 C27 1.525(5) . ? C24 C26 1.527(5) . ? C24 C25 1.533(5) . ? N31 C31 1.371(4) . ? N31 C32 1.390(4) . ? C31 N32 1.382(5) . ? N32 C33 1.395(5) . ? N32 C34 1.488(5) . ? C32 C33 1.326(5) . ? C34 C36 1.504(6) . ? C34 C35 1.519(6) . ? C34 C37 1.526(6) . ? C101 C106 1.333(9) . ? C101 C102 1.423(17) . ? C102 C103 1.30(2) . ? C103 C104 1.255(15) . ? C104 C105 1.346(11) . ? C105 C106 1.319(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 N1 In N1 14.1(3) . 2 ? N1 In S1 110.48(16) . 2 ? N1 In S1 124.39(16) 2 2 ? N1 In S1 124.39(16) . . ? N1 In S1 110.48(16) 2 . ? S1 In S1 125.12(5) 2 . ? N1 In S2 79.6(2) . . ? N1 In S2 78.9(2) 2 . ? S1 In S2 89.88(3) 2 . ? S1 In S2 100.07(3) . . ? N1 In S2 78.9(2) . 2 ? N1 In S2 79.6(2) 2 2 ? S1 In S2 100.07(3) 2 2 ? S1 In S2 89.88(3) . 2 ? S2 In S2 158.41(5) . 2 ? H1 B N11 108.1(17) . . ? H1 B N31 105.9(17) . . ? N11 B N31 113.8(4) . . ? H1 B N21 105.8(17) . . ? N11 B N21 110.4(4) . . ? N31 B N21 112.4(3) . . ? C11 S1 In 100.49(13) . . ? C21 S2 In 112.41(13) . . ? N1 N1 N2 109.3(13) 2 2 ? N1 N1 N2 44.5(8) 2 . ? N2 N1 N2 92.0(10) 2 . ? N1 N1 In 82.96(16) 2 . ? N2 N1 In 142.8(8) 2 . ? N2 N1 In 118.3(5) . . ? N1 N2 N3 160.6(13) 2 . ? N1 N2 N1 26.2(8) 2 . ? N3 N2 N1 170.7(9) . . ? N1 N2 N2 52.1(7) 2 2 ? N3 N2 N2 144.6(6) . 2 ? N1 N2 N2 35.9(4) . 2 ? C11 N11 C12 107.0(3) . . ? C11 N11 B 126.6(3) . . ? C12 N11 B 126.1(3) . . ? N11 C11 N12 109.4(3) . . ? N11 C11 S1 124.7(3) . . ? N12 C11 S1 125.8(3) . . ? C13 C12 N11 108.8(3) . . ? C11 N12 C13 107.4(3) . . ? C11 N12 C14 127.8(3) . . ? C13 N12 C14 124.5(3) . . ? C12 C13 N12 107.4(3) . . ? N12 C14 C16 109.0(4) . . ? N12 C14 C15 109.8(3) . . ? C16 C14 C15 111.3(4) . . ? N12 C14 C17 108.5(3) . . ? C16 C14 C17 109.3(4) . . ? C15 C14 C17 108.9(4) . . ? C21 N21 C22 107.3(3) . . ? C21 N21 B 124.5(3) . . ? C22 N21 B 127.0(4) . . ? N21 C21 N22 108.7(3) . . ? N21 C21 S2 125.1(3) . . ? N22 C21 S2 126.2(3) . . ? C21 N22 C23 107.0(3) . . ? C21 N22 C24 128.1(4) . . ? C23 N22 C24 124.8(3) . . ? C23 C22 N21 108.2(4) . . ? C22 C23 N22 108.8(4) . . ? N22 C24 C27 108.7(4) . . ? N22 C24 C26 110.0(3) . . ? C27 C24 C26 111.6(4) . . ? N22 C24 C25 108.9(4) . . ? C27 C24 C25 109.2(4) . . ? C26 C24 C25 108.4(4) . . ? C31 N31 C32 107.8(4) . . ? C31 N31 B 133.1(3) . . ? C32 N31 B 119.2(3) . . ? N31 C31 N32 107.2(3) . . ? N31 C31 S3 125.2(3) . . ? N32 C31 S3 127.5(3) . . ? C31 N32 C33 107.7(4) . . ? C31 N32 C34 127.8(3) . . ? C33 N32 C34 124.6(4) . . ? C33 C32 N31 109.0(4) . . ? C32 C33 N32 108.2(4) . . ? N32 C34 C36 108.7(4) . . ? N32 C34 C35 109.1(4) . . ? C36 C34 C35 108.6(4) . . ? N32 C34 C37 109.6(4) . . ? C36 C34 C37 112.0(4) . . ? C35 C34 C37 108.7(5) . . ? C106 C101 C102 119.6(11) . . ? C103 C102 C101 115.0(16) . . ? C104 C103 C102 125(2) . . ? C103 C104 C105 121.3(14) . . ? C106 C105 C104 118.6(9) . . ? C105 C106 C101 120.3(9) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.830 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.085 # Attachment 'k3-Tm2InCl_-_ky95s40__[Tm2In]+Cl-_.cif' data_ky95s40 _database_code_depnum_ccdc_archive 'CCDC 680250' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H77 B2 Cl In N15 S6' _chemical_formula_weight 1228.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 '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 15.5243(10) _cell_length_b 15.9024(10) _cell_length_c 25.6301(16) _cell_angle_alpha 90.00 _cell_angle_beta 102.2800(10) _cell_angle_gamma 90.00 _cell_volume 6182.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9223 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 32.39 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7745 _exptl_absorpt_correction_T_max 0.8771 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 102183 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 32.47 _reflns_number_total 21156 _reflns_number_gt 12750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21156 _refine_ls_number_parameters 670 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.1698 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _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 In1 In 0.5000 0.5000 0.5000 0.01328(6) Uani 1 2 d S . . In2 In 0.0000 0.5000 0.0000 0.01348(6) Uani 1 2 d S . . Cl Cl 0.24752(3) 0.32824(4) 0.751753(19) 0.02106(12) Uani 1 1 d . . . B1 B 0.39191(16) 0.60056(16) 0.61772(10) 0.0187(5) Uani 1 1 d D . . H1 H 0.3655(16) 0.6332(14) 0.6497(8) 0.022 Uiso 1 1 d D . . B2 B 0.10230(16) 0.58894(16) -0.12317(10) 0.0182(5) Uani 1 1 d D . . H2 H 0.1220(16) 0.6151(15) -0.1583(8) 0.022 Uiso 1 1 d D . . S1 S 0.33681(3) 0.46602(3) 0.51070(2) 0.01541(11) Uani 1 1 d . . . S2 S 0.47499(3) 0.65964(3) 0.50991(2) 0.01459(10) Uani 1 1 d . . . S3 S 0.56858(3) 0.48099(3) 0.60155(2) 0.01590(11) Uani 1 1 d . . . S4 S -0.07550(3) 0.47756(4) -0.10013(2) 0.01647(11) Uani 1 1 d . . . S5 S 0.02937(3) 0.65767(3) -0.01339(2) 0.01517(11) Uani 1 1 d . . . S6 S 0.16147(3) 0.46191(3) -0.01267(2) 0.01566(11) Uani 1 1 d . . . C11 C 0.29036(13) 0.56028(13) 0.52331(9) 0.0164(4) Uani 1 1 d . . . N11 N 0.31712(12) 0.60877(12) 0.56706(8) 0.0184(4) Uani 1 1 d . . . N12 N 0.21696(12) 0.59814(12) 0.49239(8) 0.0201(4) Uani 1 1 d . . . C12 C 0.26073(15) 0.67711(14) 0.56355(10) 0.0248(5) Uani 1 1 d . . . H12A H 0.2648 0.7209 0.5891 0.030 Uiso 1 1 calc R . . C13 C 0.19964(16) 0.67116(15) 0.51818(11) 0.0276(5) Uani 1 1 d . . . H13A H 0.1530 0.7097 0.5059 0.033 Uiso 1 1 calc R . . C14 C 0.15996(14) 0.56681(15) 0.44141(10) 0.0221(5) Uani 1 1 d . . . C15 C 0.08772(16) 0.63168(17) 0.42144(11) 0.0333(6) Uani 1 1 d . . . H15A H 0.1147 0.6849 0.4142 0.050 Uiso 1 1 calc R . . H15B H 0.0530 0.6405 0.4487 0.050 Uiso 1 1 calc R . . H15C H 0.0491 0.6111 0.3886 0.050 Uiso 1 1 calc R . . C16 C 0.11725(17) 0.48399(17) 0.45254(12) 0.0300(6) Uani 1 1 d . . . H16A H 0.1632 0.4422 0.4653 0.045 Uiso 1 1 calc R . . H16B H 0.0786 0.4637 0.4196 0.045 Uiso 1 1 calc R . . H16C H 0.0825 0.4930 0.4798 0.045 Uiso 1 1 calc R . . C17 C 0.21466(16) 0.55674(18) 0.39904(10) 0.0304(6) Uani 1 1 d . . . H17A H 0.2613 0.5153 0.4111 0.046 Uiso 1 1 calc R . . H17B H 0.2412 0.6109 0.3932 0.046 Uiso 1 1 calc R . . H17C H 0.1767 0.5376 0.3656 0.046 Uiso 1 1 calc R . . C21 C 0.51601(13) 0.67809(12) 0.57700(8) 0.0140(4) Uani 1 1 d . . . N21 N 0.47579(12) 0.65271(11) 0.61604(7) 0.0164(3) Uani 1 1 d . . . N22 N 0.58995(12) 0.72186(11) 0.60017(7) 0.0160(3) Uani 1 1 d . . . C22 C 0.52596(15) 0.67903(15) 0.66420(9) 0.0209(4) Uani 1 1 d . . . H22A H 0.5131 0.6689 0.6983 0.025 Uiso 1 1 calc R . . C23 C 0.59628(16) 0.72149(15) 0.65504(9) 0.0217(5) Uani 1 1 d . . . H23A H 0.6417 0.7465 0.6812 0.026 Uiso 1 1 calc R . . C24 C 0.66224(14) 0.76388(13) 0.57854(8) 0.0170(4) Uani 1 1 d . . . C25 C 0.74712(15) 0.71537(16) 0.60047(10) 0.0264(5) Uani 1 1 d . . . H25A H 0.7411 0.6576 0.5869 0.040 Uiso 1 1 calc R . . H25B H 0.7582 0.7145 0.6396 0.040 Uiso 1 1 calc R . . H25C H 0.7965 0.7429 0.5890 0.040 Uiso 1 1 calc R . . C26 C 0.67026(15) 0.85476(14) 0.59917(9) 0.0212(4) Uani 1 1 d . . . H26A H 0.6155 0.8851 0.5847 0.032 Uiso 1 1 calc R . . H26B H 0.7195 0.8826 0.5878 0.032 Uiso 1 1 calc R . . H26C H 0.6809 0.8546 0.6383 0.032 Uiso 1 1 calc R . . C27 C 0.64555(15) 0.76617(14) 0.51781(9) 0.0198(4) Uani 1 1 d . . . H27A H 0.6403 0.7086 0.5039 0.030 Uiso 1 1 calc R . . H27B H 0.6948 0.7945 0.5067 0.030 Uiso 1 1 calc R . . H27C H 0.5908 0.7969 0.5037 0.030 Uiso 1 1 calc R . . N31 N 0.41404(13) 0.50851(11) 0.63485(8) 0.0175(4) Uani 1 1 d . . . C31 C 0.48296(14) 0.45782(14) 0.63252(8) 0.0175(4) Uani 1 1 d . . . C32 C 0.36032(15) 0.46724(16) 0.66325(9) 0.0237(5) Uani 1 1 d . . . H32A H 0.3068 0.4884 0.6704 0.028 Uiso 1 1 calc R . . N32 N 0.47400(13) 0.38594(12) 0.66006(8) 0.0214(4) Uani 1 1 d . . . C33 C 0.39652(16) 0.39210(16) 0.67895(10) 0.0262(5) Uani 1 1 d . . . H33A H 0.3735 0.3509 0.6991 0.031 Uiso 1 1 calc R . . C34 C 0.53851(17) 0.31468(15) 0.67385(10) 0.0251(5) Uani 1 1 d . . . C35 C 0.62573(19) 0.34869(18) 0.70575(11) 0.0381(7) Uani 1 1 d . . . H35A H 0.6502 0.3889 0.6839 0.057 Uiso 1 1 calc R . . H35B H 0.6672 0.3021 0.7160 0.057 Uiso 1 1 calc R . . H35C H 0.6158 0.3769 0.7380 0.057 Uiso 1 1 calc R . . C36 C 0.55054(19) 0.27032(16) 0.62300(10) 0.0312(6) Uani 1 1 d . . . H36A H 0.5756 0.3098 0.6009 0.047 Uiso 1 1 calc R . . H36B H 0.4932 0.2503 0.6030 0.047 Uiso 1 1 calc R . . H36C H 0.5905 0.2224 0.6325 0.047 Uiso 1 1 calc R . . C37 C 0.5010(2) 0.25188(18) 0.70813(13) 0.0464(8) Uani 1 1 d . . . H37A H 0.4932 0.2795 0.7410 0.070 Uiso 1 1 calc R . . H37B H 0.5418 0.2045 0.7172 0.070 Uiso 1 1 calc R . . H37C H 0.4439 0.2313 0.6883 0.070 Uiso 1 1 calc R . . C41 C 0.00518(14) 0.44924(14) -0.13377(8) 0.0171(4) Uani 1 1 d . . . N41 N 0.07643(13) 0.49585(11) -0.13735(8) 0.0178(4) Uani 1 1 d . . . N42 N 0.00842(13) 0.37596(12) -0.16117(8) 0.0207(4) Uani 1 1 d . . . C42 C 0.12652(15) 0.44998(15) -0.16588(9) 0.0230(5) Uani 1 1 d . . . H42A H 0.1810 0.4673 -0.1736 0.028 Uiso 1 1 calc R . . C43 C 0.08522(15) 0.37649(15) -0.18095(9) 0.0239(5) Uani 1 1 d . . . H43A H 0.1049 0.3333 -0.2012 0.029 Uiso 1 1 calc R . . C44 C -0.06085(17) 0.30861(15) -0.17383(10) 0.0265(5) Uani 1 1 d . . . C45 C -0.0330(2) 0.24571(18) -0.21220(12) 0.0431(8) Uani 1 1 d . . . H45A H 0.0232 0.2198 -0.1950 0.065 Uiso 1 1 calc R . . H45B H -0.0260 0.2750 -0.2447 0.065 Uiso 1 1 calc R . . H45C H -0.0781 0.2020 -0.2214 0.065 Uiso 1 1 calc R . . C46 C -0.14858(18) 0.34789(19) -0.20182(11) 0.0360(6) Uani 1 1 d . . . H46A H -0.1675 0.3888 -0.1779 0.054 Uiso 1 1 calc R . . H46B H -0.1933 0.3037 -0.2109 0.054 Uiso 1 1 calc R . . H46C H -0.1411 0.3763 -0.2345 0.054 Uiso 1 1 calc R . . C47 C -0.0681(2) 0.26358(17) -0.12247(11) 0.0365(6) Uani 1 1 d . . . H47A H -0.0108 0.2394 -0.1058 0.055 Uiso 1 1 calc R . . H47B H -0.1121 0.2186 -0.1307 0.055 Uiso 1 1 calc R . . H47C H -0.0861 0.3038 -0.0978 0.055 Uiso 1 1 calc R . . N51 N 0.02089(12) 0.64395(11) -0.12048(7) 0.0166(3) Uani 1 1 d . . . C51 C -0.01472(13) 0.67414(12) -0.08030(8) 0.0148(4) Uani 1 1 d . . . N52 N -0.08767(12) 0.71962(12) -0.10249(7) 0.0174(4) Uani 1 1 d . . . C52 C -0.03156(16) 0.66958(15) -0.16828(9) 0.0218(5) Uani 1 1 d . . . H52A H -0.0220 0.6566 -0.2028 0.026 Uiso 1 1 calc R . . C53 C -0.09859(15) 0.71610(15) -0.15788(9) 0.0216(4) Uani 1 1 d . . . H53A H -0.1445 0.7416 -0.1834 0.026 Uiso 1 1 calc R . . C54 C -0.15688(14) 0.76522(14) -0.07978(9) 0.0183(4) Uani 1 1 d . . . C55 C -0.16313(16) 0.85529(14) -0.10170(10) 0.0232(5) Uani 1 1 d . . . H55A H -0.1070 0.8844 -0.0887 0.035 Uiso 1 1 calc R . . H55B H -0.2104 0.8854 -0.0896 0.035 Uiso 1 1 calc R . . H55C H -0.1760 0.8537 -0.1408 0.035 Uiso 1 1 calc R . . C56 C -0.13608(15) 0.77020(14) -0.01886(9) 0.0214(4) Uani 1 1 d . . . H56A H -0.1319 0.7132 -0.0039 0.032 Uiso 1 1 calc R . . H56B H -0.1831 0.8010 -0.0070 0.032 Uiso 1 1 calc R . . H56C H -0.0799 0.7995 -0.0066 0.032 Uiso 1 1 calc R . . C57 C -0.24377(15) 0.71879(16) -0.09928(10) 0.0265(5) Uani 1 1 d . . . H57A H -0.2388 0.6615 -0.0848 0.040 Uiso 1 1 calc R . . H57B H -0.2571 0.7164 -0.1384 0.040 Uiso 1 1 calc R . . H57C H -0.2912 0.7486 -0.0871 0.040 Uiso 1 1 calc R . . N61 N 0.18117(12) 0.59804(12) -0.07515(8) 0.0188(4) Uani 1 1 d . . . C61 C 0.20921(13) 0.55286(13) -0.02983(8) 0.0160(4) Uani 1 1 d . . . C62 C 0.23995(15) 0.66282(15) -0.07588(10) 0.0240(5) Uani 1 1 d . . . H62A H 0.2359 0.7038 -0.1033 0.029 Uiso 1 1 calc R . . N62 N 0.28543(12) 0.58986(12) -0.00216(8) 0.0194(4) Uani 1 1 d . . . C63 C 0.30384(15) 0.65854(15) -0.03153(10) 0.0248(5) Uani 1 1 d . . . H63A H 0.3526 0.6956 -0.0220 0.030 Uiso 1 1 calc R . . C64 C 0.34411(14) 0.56201(14) 0.04955(9) 0.0202(4) Uani 1 1 d . . . C65 C 0.29154(16) 0.56000(18) 0.09342(10) 0.0285(5) Uani 1 1 d . . . H65A H 0.2682 0.6162 0.0977 0.043 Uiso 1 1 calc R . . H65B H 0.3300 0.5423 0.1271 0.043 Uiso 1 1 calc R . . H65C H 0.2426 0.5201 0.0837 0.043 Uiso 1 1 calc R . . C66 C 0.38285(17) 0.47648(17) 0.04120(11) 0.0297(5) Uani 1 1 d . . . H66A H 0.4164 0.4805 0.0130 0.045 Uiso 1 1 calc R . . H66B H 0.3351 0.4356 0.0308 0.045 Uiso 1 1 calc R . . H66C H 0.4220 0.4582 0.0745 0.045 Uiso 1 1 calc R . . C67 C 0.41925(16) 0.62547(17) 0.06528(11) 0.0298(6) Uani 1 1 d . . . H67A H 0.4539 0.6273 0.0375 0.045 Uiso 1 1 calc R . . H67B H 0.4573 0.6084 0.0992 0.045 Uiso 1 1 calc R . . H67C H 0.3947 0.6813 0.0692 0.045 Uiso 1 1 calc R . . C71 C -0.6780(3) 0.5808(3) -0.21699(15) 0.0577(10) Uani 1 1 d . . . N71 N -0.7281(3) 0.6324(3) -0.23699(17) 0.0809(12) Uani 1 1 d . . . C72 C -0.6150(3) 0.5145(2) -0.19392(16) 0.0618(11) Uani 1 1 d . . . H72A H -0.6392 0.4594 -0.2064 0.093 Uiso 1 1 calc R . . H72B H -0.6048 0.5167 -0.1549 0.093 Uiso 1 1 calc R . . H72C H -0.5591 0.5233 -0.2051 0.093 Uiso 1 1 calc R . . C81 C -0.3391(2) 0.56376(19) -0.23209(14) 0.0491(8) Uani 1 1 d . . . N81 N -0.4024(2) 0.5512(2) -0.21634(13) 0.0672(9) Uani 1 1 d . . . C82 C -0.2603(2) 0.5795(3) -0.25269(14) 0.0624(12) Uani 1 1 d . . . H82A H -0.2504 0.6403 -0.2540 0.094 Uiso 1 1 calc R . . H82B H -0.2680 0.5560 -0.2887 0.094 Uiso 1 1 calc R . . H82C H -0.2095 0.5530 -0.2293 0.094 Uiso 1 1 calc R . . C91 C 0.0147(2) 0.51312(19) -0.28940(13) 0.0452(8) Uani 1 1 d . . . N91 N -0.0546(2) 0.5189(2) -0.27975(14) 0.0669(9) Uani 1 1 d . . . C92 C 0.1014(3) 0.5069(2) -0.30180(16) 0.0470(9) Uani 1 1 d . . . H92A H 0.0959 0.5107 -0.3405 0.071 Uiso 1 1 calc R . . H92B H 0.1282 0.4529 -0.2889 0.071 Uiso 1 1 calc R . . H92C H 0.1386 0.5529 -0.2843 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 In1 0.01386(11) 0.01237(11) 0.01432(11) -0.00010(7) 0.00457(8) 0.00132(7) In2 0.01375(11) 0.01268(11) 0.01475(11) -0.00016(7) 0.00471(8) -0.00163(7) Cl 0.0169(2) 0.0287(3) 0.0174(2) 0.0003(2) 0.00318(19) 0.0003(2) B1 0.0181(11) 0.0198(12) 0.0207(12) -0.0052(9) 0.0102(10) -0.0025(9) B2 0.0174(11) 0.0194(11) 0.0192(11) 0.0035(9) 0.0072(9) -0.0007(9) S1 0.0130(2) 0.0132(2) 0.0207(3) -0.00118(19) 0.00501(19) 0.00152(18) S2 0.0170(2) 0.0124(2) 0.0140(2) -0.00030(17) 0.00242(19) 0.00120(18) S3 0.0144(2) 0.0182(2) 0.0156(2) 0.00247(19) 0.00448(19) -0.00016(19) S4 0.0146(2) 0.0194(2) 0.0162(2) -0.00289(19) 0.00501(19) -0.00059(19) S5 0.0172(2) 0.0129(2) 0.0149(2) 0.00029(18) 0.00230(19) -0.00183(18) S6 0.0133(2) 0.0136(2) 0.0209(3) 0.00107(19) 0.00540(19) -0.00146(18) C11 0.0127(9) 0.0151(9) 0.0219(10) -0.0008(8) 0.0051(8) 0.0025(7) N11 0.0140(8) 0.0170(9) 0.0259(10) -0.0044(7) 0.0079(7) 0.0001(7) N12 0.0143(8) 0.0165(9) 0.0287(10) -0.0025(7) 0.0027(7) 0.0025(7) C12 0.0205(11) 0.0185(11) 0.0367(14) -0.0072(10) 0.0092(10) 0.0036(9) C13 0.0201(11) 0.0204(11) 0.0416(15) -0.0050(10) 0.0047(10) 0.0062(9) C14 0.0145(10) 0.0210(11) 0.0289(12) -0.0017(9) 0.0006(9) 0.0033(8) C15 0.0214(12) 0.0307(14) 0.0433(16) 0.0030(12) -0.0031(11) 0.0082(10) C16 0.0213(12) 0.0276(12) 0.0391(15) -0.0010(11) 0.0017(11) -0.0057(10) C17 0.0211(12) 0.0422(15) 0.0267(13) 0.0022(11) 0.0024(10) 0.0036(11) C21 0.0154(9) 0.0114(9) 0.0154(9) -0.0017(7) 0.0038(7) 0.0008(7) N21 0.0174(8) 0.0159(8) 0.0170(8) -0.0028(7) 0.0064(7) -0.0007(7) N22 0.0170(8) 0.0160(8) 0.0160(8) -0.0021(7) 0.0054(7) -0.0040(7) C22 0.0242(11) 0.0246(11) 0.0147(10) -0.0040(8) 0.0064(8) -0.0068(9) C23 0.0245(11) 0.0240(11) 0.0163(10) -0.0041(8) 0.0036(9) -0.0077(9) C24 0.0161(10) 0.0164(10) 0.0189(10) 0.0000(8) 0.0044(8) -0.0016(8) C25 0.0198(11) 0.0298(13) 0.0304(13) 0.0032(10) 0.0072(10) 0.0046(10) C26 0.0210(11) 0.0173(10) 0.0254(11) -0.0031(8) 0.0055(9) -0.0031(8) C27 0.0231(11) 0.0197(10) 0.0181(10) -0.0004(8) 0.0081(8) -0.0036(8) N31 0.0165(9) 0.0214(9) 0.0161(9) -0.0003(7) 0.0072(7) -0.0043(7) C31 0.0197(10) 0.0195(10) 0.0141(9) -0.0002(8) 0.0051(8) -0.0030(8) C32 0.0190(11) 0.0323(13) 0.0226(11) 0.0006(10) 0.0110(9) -0.0069(9) N32 0.0262(10) 0.0214(9) 0.0189(9) 0.0043(7) 0.0098(8) -0.0039(8) C33 0.0270(12) 0.0291(13) 0.0259(12) 0.0033(10) 0.0136(10) -0.0071(10) C34 0.0339(13) 0.0217(11) 0.0212(11) 0.0072(9) 0.0091(10) 0.0039(10) C35 0.0428(17) 0.0338(15) 0.0303(14) 0.0032(11) -0.0091(12) 0.0066(13) C36 0.0443(16) 0.0251(13) 0.0241(12) 0.0019(10) 0.0070(11) 0.0066(11) C37 0.065(2) 0.0303(15) 0.0525(19) 0.0197(14) 0.0329(17) 0.0070(14) C41 0.0176(10) 0.0205(10) 0.0136(9) -0.0005(8) 0.0040(8) 0.0022(8) N41 0.0142(9) 0.0244(10) 0.0166(9) 0.0005(7) 0.0071(7) 0.0031(7) N42 0.0240(10) 0.0199(9) 0.0196(9) -0.0042(7) 0.0073(8) 0.0014(8) C42 0.0204(11) 0.0293(12) 0.0219(11) 0.0023(9) 0.0104(9) 0.0065(9) C43 0.0251(12) 0.0255(12) 0.0233(11) -0.0017(9) 0.0100(9) 0.0084(9) C44 0.0362(14) 0.0209(11) 0.0247(12) -0.0064(9) 0.0115(10) -0.0043(10) C45 0.061(2) 0.0284(14) 0.0449(17) -0.0183(13) 0.0227(15) -0.0089(14) C46 0.0323(14) 0.0390(15) 0.0335(14) -0.0114(12) 0.0001(11) -0.0101(12) C47 0.0521(18) 0.0274(14) 0.0322(14) -0.0007(11) 0.0139(13) -0.0077(12) N51 0.0159(8) 0.0172(8) 0.0176(8) 0.0030(7) 0.0055(7) 0.0005(7) C51 0.0156(9) 0.0124(9) 0.0167(9) 0.0008(7) 0.0042(8) -0.0027(7) N52 0.0179(9) 0.0186(9) 0.0159(8) 0.0027(7) 0.0039(7) 0.0022(7) C52 0.0249(11) 0.0261(12) 0.0151(10) 0.0045(8) 0.0057(9) 0.0059(9) C53 0.0223(11) 0.0242(11) 0.0181(10) 0.0042(9) 0.0036(9) 0.0048(9) C54 0.0170(10) 0.0175(10) 0.0214(10) 0.0005(8) 0.0059(8) 0.0024(8) C55 0.0229(11) 0.0190(11) 0.0282(12) 0.0041(9) 0.0067(9) 0.0034(9) C56 0.0237(11) 0.0202(11) 0.0218(11) -0.0014(8) 0.0083(9) 0.0044(9) C57 0.0209(11) 0.0310(13) 0.0289(13) -0.0025(10) 0.0079(10) -0.0045(10) N61 0.0161(8) 0.0178(9) 0.0237(9) 0.0043(7) 0.0071(7) -0.0008(7) C61 0.0124(9) 0.0158(9) 0.0208(10) 0.0013(8) 0.0055(8) -0.0022(7) C62 0.0206(11) 0.0203(11) 0.0320(13) 0.0072(9) 0.0078(9) -0.0057(9) N62 0.0148(8) 0.0171(9) 0.0261(10) 0.0020(7) 0.0041(7) -0.0043(7) C63 0.0186(11) 0.0228(11) 0.0333(13) 0.0055(10) 0.0063(10) -0.0067(9) C64 0.0138(10) 0.0202(10) 0.0251(11) 0.0013(9) 0.0009(8) -0.0023(8) C65 0.0227(12) 0.0397(14) 0.0229(12) -0.0001(10) 0.0046(10) -0.0039(10) C66 0.0213(12) 0.0249(12) 0.0410(15) -0.0004(11) 0.0024(11) 0.0053(10) C67 0.0191(11) 0.0304(13) 0.0364(14) -0.0013(11) -0.0017(10) -0.0079(10) C71 0.064(2) 0.057(2) 0.059(2) -0.0184(19) 0.029(2) -0.0348(19) N71 0.069(2) 0.063(3) 0.115(3) -0.013(2) 0.030(2) -0.015(2) C72 0.079(3) 0.055(2) 0.049(2) 0.0047(18) 0.008(2) -0.029(2) C81 0.057(2) 0.0353(16) 0.050(2) -0.0008(14) -0.0002(17) 0.0095(15) N81 0.078(2) 0.061(2) 0.067(2) 0.0179(17) 0.0247(19) 0.0174(19) C82 0.051(2) 0.044(2) 0.094(4) 0.0015(17) 0.018(2) -0.0008(15) C91 0.050(2) 0.0400(17) 0.0406(18) -0.0053(13) -0.0021(15) 0.0086(15) N91 0.0484(19) 0.083(2) 0.065(2) -0.0082(18) 0.0013(16) 0.0014(18) C92 0.050(2) 0.0419(18) 0.049(2) -0.0002(14) 0.0110(17) 0.0132(15) _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 In1 S2 2.5889(5) . ? In1 S2 2.5889(5) 3_666 ? In1 S3 2.6116(5) . ? In1 S3 2.6116(5) 3_666 ? In1 S1 2.6609(5) 3_666 ? In1 S1 2.6609(5) . ? In2 S5 2.5843(5) . ? In2 S5 2.5843(5) 3_565 ? In2 S4 2.6091(5) 3_565 ? In2 S4 2.6091(5) . ? In2 S6 2.6650(5) 3_565 ? In2 S6 2.6650(5) . ? B1 H1 1.119(15) . ? B1 N31 1.546(3) . ? B1 N21 1.552(3) . ? B1 N11 1.552(3) . ? B2 H2 1.093(16) . ? B2 N61 1.547(3) . ? B2 N51 1.551(3) . ? B2 N41 1.556(3) . ? S1 C11 1.724(2) . ? S2 C21 1.727(2) . ? S3 C31 1.727(2) . ? S4 C41 1.725(2) . ? S5 C51 1.726(2) . ? S6 C61 1.724(2) . ? C11 N11 1.351(3) . ? C11 N12 1.380(3) . ? N11 C12 1.386(3) . ? N12 C13 1.390(3) . ? N12 C14 1.499(3) . ? C12 C13 1.338(3) . ? C14 C17 1.523(3) . ? C14 C16 1.528(3) . ? C14 C15 1.530(3) . ? C21 N21 1.349(3) . ? C21 N22 1.365(3) . ? N21 C22 1.377(3) . ? N22 C23 1.389(3) . ? N22 C24 1.509(3) . ? C22 C23 1.346(3) . ? C24 C27 1.523(3) . ? C24 C25 1.527(3) . ? C24 C26 1.535(3) . ? N31 C31 1.351(3) . ? N31 C32 1.383(3) . ? C31 N32 1.366(3) . ? C32 C33 1.345(4) . ? N32 C33 1.392(3) . ? N32 C34 1.504(3) . ? C34 C35 1.524(4) . ? C34 C37 1.525(3) . ? C34 C36 1.528(3) . ? C41 N41 1.351(3) . ? C41 N42 1.367(3) . ? N41 C42 1.383(3) . ? N42 C43 1.391(3) . ? N42 C44 1.503(3) . ? C42 C43 1.349(3) . ? C44 C47 1.524(4) . ? C44 C45 1.528(3) . ? C44 C46 1.531(4) . ? N51 C51 1.356(3) . ? N51 C52 1.381(3) . ? C51 N52 1.362(3) . ? N52 C53 1.395(3) . ? N52 C54 1.512(3) . ? C52 C53 1.349(3) . ? C54 C57 1.526(3) . ? C54 C56 1.528(3) . ? C54 C55 1.534(3) . ? N61 C61 1.356(3) . ? N61 C62 1.379(3) . ? C61 N62 1.376(3) . ? C62 C63 1.342(3) . ? N62 C63 1.390(3) . ? N62 C64 1.506(3) . ? C64 C66 1.521(3) . ? C64 C65 1.524(3) . ? C64 C67 1.530(3) . ? C71 N71 1.171(5) . ? C71 C72 1.475(6) . ? C81 N81 1.157(4) . ? C81 C82 1.453(4) . ? C91 N91 1.157(4) . ? C91 C92 1.450(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 S2 In1 S2 180.0 . 3_666 ? S2 In1 S3 93.074(16) . . ? S2 In1 S3 86.926(16) 3_666 . ? S2 In1 S3 86.926(16) . 3_666 ? S2 In1 S3 93.074(16) 3_666 3_666 ? S3 In1 S3 180.0 . 3_666 ? S2 In1 S1 88.679(16) . 3_666 ? S2 In1 S1 91.321(16) 3_666 3_666 ? S3 In1 S1 86.041(16) . 3_666 ? S3 In1 S1 93.959(16) 3_666 3_666 ? S2 In1 S1 91.321(16) . . ? S2 In1 S1 88.679(16) 3_666 . ? S3 In1 S1 93.959(16) . . ? S3 In1 S1 86.041(16) 3_666 . ? S1 In1 S1 180.0 3_666 . ? S5 In2 S5 180.00(2) . 3_565 ? S5 In2 S4 86.727(17) . 3_565 ? S5 In2 S4 93.273(17) 3_565 3_565 ? S5 In2 S4 93.273(17) . . ? S5 In2 S4 86.727(17) 3_565 . ? S4 In2 S4 180.00(2) 3_565 . ? S5 In2 S6 89.583(16) . 3_565 ? S5 In2 S6 90.417(16) 3_565 3_565 ? S4 In2 S6 94.962(16) 3_565 3_565 ? S4 In2 S6 85.038(16) . 3_565 ? S5 In2 S6 90.417(16) . . ? S5 In2 S6 89.583(16) 3_565 . ? S4 In2 S6 85.038(16) 3_565 . ? S4 In2 S6 94.962(16) . . ? S6 In2 S6 180.00(3) 3_565 . ? H1 B1 N31 108.9(13) . . ? H1 B1 N21 102.3(13) . . ? N31 B1 N21 112.14(18) . . ? H1 B1 N11 104.4(13) . . ? N31 B1 N11 113.50(18) . . ? N21 B1 N11 114.49(19) . . ? H2 B2 N61 107.9(13) . . ? H2 B2 N51 101.3(14) . . ? N61 B2 N51 115.24(19) . . ? H2 B2 N41 105.8(13) . . ? N61 B2 N41 113.33(19) . . ? N51 B2 N41 112.00(18) . . ? C11 S1 In1 106.75(7) . . ? C21 S2 In1 103.47(7) . . ? C31 S3 In1 107.00(8) . . ? C41 S4 In2 107.78(7) . . ? C51 S5 In2 103.61(7) . . ? C61 S6 In2 107.87(7) . . ? N11 C11 N12 107.35(18) . . ? N11 C11 S1 125.78(16) . . ? N12 C11 S1 126.80(17) . . ? C11 N11 C12 108.36(19) . . ? C11 N11 B1 133.57(18) . . ? C12 N11 B1 118.02(19) . . ? C11 N12 C13 108.11(19) . . ? C11 N12 C14 128.16(18) . . ? C13 N12 C14 123.65(19) . . ? C13 C12 N11 108.8(2) . . ? C12 C13 N12 107.4(2) . . ? N12 C14 C17 109.96(18) . . ? N12 C14 C16 108.8(2) . . ? C17 C14 C16 111.9(2) . . ? N12 C14 C15 108.81(19) . . ? C17 C14 C15 108.2(2) . . ? C16 C14 C15 109.1(2) . . ? N21 C21 N22 108.00(17) . . ? N21 C21 S2 123.83(16) . . ? N22 C21 S2 128.13(15) . . ? C21 N21 C22 108.12(18) . . ? C21 N21 B1 134.74(18) . . ? C22 N21 B1 117.10(18) . . ? C21 N22 C23 108.06(17) . . ? C21 N22 C24 133.47(17) . . ? C23 N22 C24 118.41(17) . . ? C23 C22 N21 108.75(19) . . ? C22 C23 N22 107.06(19) . . ? N22 C24 C27 114.07(17) . . ? N22 C24 C25 106.98(17) . . ? C27 C24 C25 109.52(18) . . ? N22 C24 C26 107.60(17) . . ? C27 C24 C26 108.26(18) . . ? C25 C24 C26 110.39(19) . . ? C31 N31 C32 108.18(19) . . ? C31 N31 B1 133.05(18) . . ? C32 N31 B1 118.44(19) . . ? N31 C31 N32 107.92(18) . . ? N31 C31 S3 125.97(16) . . ? N32 C31 S3 126.09(17) . . ? C33 C32 N31 108.6(2) . . ? C31 N32 C33 108.14(19) . . ? C31 N32 C34 128.03(19) . . ? C33 N32 C34 123.54(19) . . ? C32 C33 N32 107.2(2) . . ? N32 C34 C35 109.3(2) . . ? N32 C34 C37 108.2(2) . . ? C35 C34 C37 109.1(2) . . ? N32 C34 C36 110.1(2) . . ? C35 C34 C36 111.4(2) . . ? C37 C34 C36 108.7(2) . . ? N41 C41 N42 108.22(18) . . ? N41 C41 S4 125.65(17) . . ? N42 C41 S4 126.12(17) . . ? C41 N41 C42 107.88(19) . . ? C41 N41 B2 132.88(18) . . ? C42 N41 B2 118.61(19) . . ? C41 N42 C43 108.06(19) . . ? C41 N42 C44 127.97(19) . . ? C43 N42 C44 123.70(19) . . ? C43 C42 N41 108.8(2) . . ? C42 C43 N42 107.0(2) . . ? N42 C44 C47 109.2(2) . . ? N42 C44 C45 108.5(2) . . ? C47 C44 C45 109.4(2) . . ? N42 C44 C46 109.6(2) . . ? C47 C44 C46 112.0(2) . . ? C45 C44 C46 108.1(2) . . ? C51 N51 C52 108.10(18) . . ? C51 N51 B2 134.54(18) . . ? C52 N51 B2 117.36(18) . . ? N51 C51 N52 107.94(18) . . ? N51 C51 S5 124.15(16) . . ? N52 C51 S5 127.90(16) . . ? C51 N52 C53 108.30(17) . . ? C51 N52 C54 133.62(18) . . ? C53 N52 C54 117.96(17) . . ? C53 C52 N51 108.7(2) . . ? C52 C53 N52 106.94(19) . . ? N52 C54 C57 107.03(18) . . ? N52 C54 C56 113.92(17) . . ? C57 C54 C56 109.87(18) . . ? N52 C54 C55 107.55(17) . . ? C57 C54 C55 110.44(19) . . ? C56 C54 C55 108.00(18) . . ? C61 N61 C62 108.34(18) . . ? C61 N61 B2 133.41(18) . . ? C62 N61 B2 118.23(18) . . ? N61 C61 N62 107.40(17) . . ? N61 C61 S6 125.85(16) . . ? N62 C61 S6 126.63(16) . . ? C63 C62 N61 108.8(2) . . ? C61 N62 C63 108.08(19) . . ? C61 N62 C64 128.37(18) . . ? C63 N62 C64 123.50(18) . . ? C62 C63 N62 107.4(2) . . ? N62 C64 C66 108.82(19) . . ? N62 C64 C65 109.69(18) . . ? C66 C64 C65 112.0(2) . . ? N62 C64 C67 108.81(18) . . ? C66 C64 C67 108.95(19) . . ? C65 C64 C67 108.5(2) . . ? N71 C71 C72 177.7(4) . . ? N81 C81 C82 179.1(4) . . ? N91 C91 C92 179.3(4) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 32.47 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.660 _refine_diff_density_min -1.134 _refine_diff_density_rms 0.086 data_tmins10p _database_code_depnum_ccdc_archive 'CCDC 681309' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H68 B2 I In N12 S6' _chemical_formula_weight 1196.78 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' 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' In In -0.7276 1.3100 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 11.8575(14) _cell_length_b 11.8575(14) _cell_length_c 26.003(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3166.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 4756 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 25.81 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8108 _exptl_absorpt_correction_T_max 0.8108 _exptl_absorpt_process_details SADABS _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 18257 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.27 _reflns_number_total 2518 _reflns_number_gt 1815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^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 0.0014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2518 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.333 0.666 0.250 337.2 46.9 2 -0.334 0.333 0.750 337.3 45.0 3 0.333 0.667 0.015 7.3 -0.2 4 0.333 0.667 0.485 7.3 -0.1 5 0.667 0.333 0.515 7.3 0.0 6 0.667 0.333 0.985 7.3 -0.1 _platon_squeeze_details ; The unit cell contains 2 benzene molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON ; 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 In In -1.0000 -1.0000 0.0000 0.03213(18) Uani 1 6 d S . . I I -0.3333 -0.6667 0.2500 0.04206(19) Uani 1 6 d S . . S S -0.89244(8) -0.78568(8) 0.05610(3) 0.0354(2) Uani 1 1 d . . . B B -1.0000 -1.0000 0.1581(2) 0.0332(14) Uani 1 3 d S . . H1 H -1.0000 -1.0000 0.192(2) 0.043(17) Uiso 1 3 d S . . N11 N -0.8589(3) -0.8969(3) 0.14339(8) 0.0312(6) Uani 1 1 d . . . N12 N -0.6793(3) -0.7244(3) 0.11799(9) 0.0339(6) Uani 1 1 d . . . C11 C -0.8083(3) -0.8036(3) 0.10687(9) 0.0310(7) Uani 1 1 d . . . C12 C -0.7586(3) -0.8781(3) 0.17636(10) 0.0378(8) Uani 1 1 d . . . H12A H -0.7668 -0.9310 0.2047 0.045 Uiso 1 1 calc R . . C13 C -0.6501(3) -0.7738(3) 0.16142(11) 0.0396(8) Uani 1 1 d . . . H13A H -0.5681 -0.7391 0.1772 0.048 Uiso 1 1 calc R . . C14 C -0.5793(3) -0.6057(3) 0.08955(12) 0.0416(8) Uani 1 1 d . . . C15 C -0.4524(4) -0.5412(4) 0.11941(16) 0.0642(11) Uani 1 1 d . . . H15A H -0.4199 -0.6014 0.1227 0.096 Uiso 1 1 calc R . . H15B H -0.4673 -0.5172 0.1533 0.096 Uiso 1 1 calc R . . H15C H -0.3889 -0.4638 0.1013 0.096 Uiso 1 1 calc R . . C16 C -0.5566(4) -0.6504(4) 0.03683(13) 0.0586(11) Uani 1 1 d . . . H16A H -0.5682 -0.7371 0.0400 0.088 Uiso 1 1 calc R . . H16B H -0.4687 -0.5905 0.0252 0.088 Uiso 1 1 calc R . . H16C H -0.6185 -0.6517 0.0121 0.088 Uiso 1 1 calc R . . C17 C -0.6263(4) -0.5064(4) 0.08526(15) 0.0532(10) Uani 1 1 d . . . H17A H -0.6366 -0.4799 0.1194 0.080 Uiso 1 1 calc R . . H17B H -0.7092 -0.5458 0.0674 0.080 Uiso 1 1 calc R . . H17C H -0.5628 -0.4308 0.0662 0.080 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 In 0.0386(2) 0.0386(2) 0.0192(2) 0.000 0.000 0.01929(12) I 0.0467(3) 0.0467(3) 0.0327(3) 0.000 0.000 0.02337(13) S 0.0438(5) 0.0380(5) 0.0244(3) -0.0010(3) -0.0074(3) 0.0204(4) B 0.039(2) 0.039(2) 0.021(2) 0.000 0.000 0.0196(11) N11 0.0359(15) 0.0377(15) 0.0230(10) -0.0034(10) -0.0050(10) 0.0206(13) N12 0.0355(16) 0.0357(16) 0.0298(11) -0.0004(11) -0.0040(11) 0.0173(13) C11 0.0374(18) 0.0348(18) 0.0245(12) -0.0017(12) -0.0011(12) 0.0207(15) C12 0.044(2) 0.048(2) 0.0268(14) 0.0012(14) -0.0063(14) 0.0273(18) C13 0.039(2) 0.049(2) 0.0331(14) 0.0007(15) -0.0073(14) 0.0241(18) C14 0.041(2) 0.039(2) 0.0415(16) 0.0028(15) 0.0011(15) 0.0171(17) C15 0.043(2) 0.057(3) 0.071(2) 0.002(2) -0.012(2) 0.009(2) C16 0.072(3) 0.057(3) 0.0464(18) 0.0067(18) 0.0204(19) 0.032(2) C17 0.060(3) 0.037(2) 0.062(2) 0.0011(18) 0.0014(19) 0.024(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 In S 2.6405(8) 7_335 ? In S 2.6405(8) . ? In S 2.6405(8) 9_455 ? In S 2.6405(8) 8_545 ? In S 2.6405(8) 2_345 ? In S 2.6405(8) 3_435 ? S C11 1.730(3) . ? B H1 0.88(5) . ? B N11 1.548(3) 3_435 ? B N11 1.548(3) . ? B N11 1.548(3) 2_345 ? N11 C11 1.350(4) . ? N11 C12 1.391(4) . ? N12 C11 1.367(4) . ? N12 C13 1.393(4) . ? N12 C14 1.505(4) . ? C12 C13 1.322(5) . ? C14 C15 1.517(5) . ? C14 C17 1.538(5) . ? C14 C16 1.542(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 S In S 180.0 7_335 . ? S In S 92.41(2) 7_335 9_455 ? S In S 87.59(2) . 9_455 ? S In S 92.41(2) 7_335 8_545 ? S In S 87.59(2) . 8_545 ? S In S 92.41(2) 9_455 8_545 ? S In S 87.59(2) 7_335 2_345 ? S In S 92.41(2) . 2_345 ? S In S 87.59(2) 9_455 2_345 ? S In S 180.00(5) 8_545 2_345 ? S In S 87.59(2) 7_335 3_435 ? S In S 92.41(2) . 3_435 ? S In S 180.0 9_455 3_435 ? S In S 87.59(2) 8_545 3_435 ? S In S 92.41(2) 2_345 3_435 ? C11 S In 109.52(11) . . ? H1 B N11 104.4(2) . 3_435 ? H1 B N11 104.4(2) . . ? N11 B N11 114.07(16) 3_435 . ? H1 B N11 104.4(2) . 2_345 ? N11 B N11 114.07(16) 3_435 2_345 ? N11 B N11 114.07(16) . 2_345 ? C11 N11 C12 108.0(3) . . ? C11 N11 B 133.1(3) . . ? C12 N11 B 118.3(3) . . ? C11 N12 C13 108.1(3) . . ? C11 N12 C14 128.8(2) . . ? C13 N12 C14 123.1(3) . . ? N11 C11 N12 107.5(2) . . ? N11 C11 S 126.2(2) . . ? N12 C11 S 126.3(2) . . ? C13 C12 N11 108.9(3) . . ? C12 C13 N12 107.5(3) . . ? N12 C14 C15 109.8(3) . . ? N12 C14 C17 109.5(3) . . ? C15 C14 C17 107.4(3) . . ? N12 C14 C16 107.9(3) . . ? C15 C14 C16 109.2(3) . . ? C17 C14 C16 113.0(3) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.344 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.077