# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Parkin, Gerard' _publ_contact_author_name 'Gerard Parkin' _publ_contact_author_address ; Havemeyer Hall MC3115, 3000 Broadway New York United States 10027 ; _publ_contact_author_email PARKIN@COLUMBIA.EDU # Attachment '- Bm2InBr (ky291s10).cif' data_ky291s10 _database_code_depnum_ccdc_archive 'CCDC 776950' #TrackingRef '- Bm2InBr (ky291s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H52.50 B2 Br In N9.50 S4' _chemical_formula_weight 902.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 21.2905(17) _cell_length_b 11.3455(9) _cell_length_c 18.8012(15) _cell_angle_alpha 90.00 _cell_angle_beta 112.6590(10) _cell_angle_gamma 90.00 _cell_volume 4190.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9947 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 32.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 1.751 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5793 _exptl_absorpt_correction_T_max 0.7209 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56199 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10403 _reflns_number_gt 8728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to be 1.1 angstroms. The bonds of one acetonitrile molecule have been restrained. ; _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^)+(0.0402P)^2^+9.7791P] 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 10403 _refine_ls_number_parameters 448 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.104 _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 0.258605(10) -0.002868(18) 0.139891(11) 0.01647(6) Uani 1 1 d . . . Br Br 0.348318(16) 0.15183(3) 0.217791(19) 0.02808(8) Uani 1 1 d . . . S1 S 0.17107(4) 0.00105(7) 0.19917(4) 0.02360(15) Uani 1 1 d . . . S2 S 0.34015(4) -0.16222(7) 0.22916(4) 0.02220(15) Uani 1 1 d . . . S3 S 0.19117(4) 0.17653(6) 0.05830(4) 0.01861(14) Uani 1 1 d . . . S4 S 0.29579(4) -0.08917(7) 0.03942(4) 0.02346(16) Uani 1 1 d . . . B1 B 0.18693(18) -0.2820(3) 0.1632(2) 0.0225(7) Uani 1 1 d D . . H1 H 0.1762(18) -0.210(2) 0.1209(17) 0.027 Uiso 1 1 d D . . H2 H 0.1470(15) -0.350(3) 0.145(2) 0.027 Uiso 1 1 d D . . B2 B 0.13078(18) -0.0486(3) -0.0610(2) 0.0220(7) Uani 1 1 d D . . H3 H 0.1499(17) -0.104(3) -0.0089(15) 0.026 Uiso 1 1 d D . . H4 H 0.0964(16) -0.101(3) -0.1096(16) 0.026 Uiso 1 1 d D . . N11 N 0.19449(13) -0.2293(2) 0.24271(14) 0.0211(5) Uani 1 1 d . . . C11 C 0.19232(14) -0.1163(3) 0.26288(17) 0.0202(6) Uani 1 1 d . . . C12 C 0.21069(18) -0.2973(3) 0.30821(19) 0.0280(7) Uani 1 1 d . . . H12A H 0.2160 -0.3805 0.3108 0.034 Uiso 1 1 calc R . . N12 N 0.20634(14) -0.1117(2) 0.33992(15) 0.0237(5) Uani 1 1 d . . . C13 C 0.21777(19) -0.2258(3) 0.36778(19) 0.0301(7) Uani 1 1 d . . . H13A H 0.2287 -0.2494 0.4197 0.036 Uiso 1 1 calc R . . C14 C 0.21341(19) -0.0039(3) 0.3891(2) 0.0303(7) Uani 1 1 d . . . C15 C 0.2281(3) -0.0429(4) 0.4722(2) 0.0478(10) Uani 1 1 d . . . H15A H 0.2707 -0.0879 0.4920 0.072 Uiso 1 1 calc R . . H15B H 0.1907 -0.0925 0.4730 0.072 Uiso 1 1 calc R . . H15C H 0.2324 0.0267 0.5045 0.072 Uiso 1 1 calc R . . C16 C 0.2733(2) 0.0687(4) 0.3880(3) 0.0439(9) Uani 1 1 d . . . H16A H 0.2648 0.0924 0.3350 0.066 Uiso 1 1 calc R . . H16B H 0.3149 0.0213 0.4084 0.066 Uiso 1 1 calc R . . H16C H 0.2787 0.1392 0.4200 0.066 Uiso 1 1 calc R . . C17 C 0.1472(2) 0.0664(4) 0.3600(2) 0.0398(9) Uani 1 1 d . . . H17A H 0.1382 0.0958 0.3080 0.060 Uiso 1 1 calc R . . H17B H 0.1512 0.1331 0.3946 0.060 Uiso 1 1 calc R . . H17C H 0.1096 0.0155 0.3588 0.060 Uiso 1 1 calc R . . C21 C 0.31703(15) -0.3053(3) 0.19783(16) 0.0216(6) Uani 1 1 d . . . N21 N 0.25377(13) -0.3505(2) 0.17602(14) 0.0223(5) Uani 1 1 d . . . N22 N 0.35992(13) -0.3948(2) 0.19729(15) 0.0249(5) Uani 1 1 d . . . C22 C 0.25735(18) -0.4694(3) 0.16362(18) 0.0275(7) Uani 1 1 d . . . H22A H 0.2201 -0.5228 0.1482 0.033 Uiso 1 1 calc R . . C23 C 0.32214(18) -0.4975(3) 0.1769(2) 0.0303(7) Uani 1 1 d . . . H23A H 0.3390 -0.5738 0.1731 0.036 Uiso 1 1 calc R . . C24 C 0.43503(17) -0.3865(3) 0.2139(2) 0.0307(7) Uani 1 1 d . . . C25 C 0.4612(2) -0.5079(4) 0.2039(3) 0.0519(11) Uani 1 1 d . . . H25A H 0.4374 -0.5343 0.1506 0.078 Uiso 1 1 calc R . . H25B H 0.4529 -0.5640 0.2389 0.078 Uiso 1 1 calc R . . H25C H 0.5102 -0.5035 0.2158 0.078 Uiso 1 1 calc R . . C26 C 0.47286(17) -0.3471(4) 0.2970(2) 0.0376(9) Uani 1 1 d . . . H26A H 0.5219 -0.3456 0.3088 0.056 Uiso 1 1 calc R . . H26B H 0.4635 -0.4024 0.3318 0.056 Uiso 1 1 calc R . . H26C H 0.4576 -0.2681 0.3040 0.056 Uiso 1 1 calc R . . C27 C 0.44577(19) -0.3005(4) 0.1569(2) 0.0395(9) Uani 1 1 d . . . H27A H 0.4228 -0.3306 0.1043 0.059 Uiso 1 1 calc R . . H27B H 0.4946 -0.2925 0.1687 0.059 Uiso 1 1 calc R . . H27C H 0.4268 -0.2234 0.1612 0.059 Uiso 1 1 calc R . . C31 C 0.10713(14) 0.1361(3) 0.00783(16) 0.0183(5) Uani 1 1 d . . . N31 N 0.08662(12) 0.0504(2) -0.04590(14) 0.0192(5) Uani 1 1 d . . . N32 N 0.05065(12) 0.1903(2) 0.01007(14) 0.0183(5) Uani 1 1 d . . . C32 C 0.01653(15) 0.0527(3) -0.07911(17) 0.0226(6) Uani 1 1 d . . . H32A H -0.0112 0.0022 -0.1192 0.027 Uiso 1 1 calc R . . C33 C -0.00614(15) 0.1384(3) -0.04533(17) 0.0217(6) Uani 1 1 d . . . H33A H -0.0523 0.1593 -0.0572 0.026 Uiso 1 1 calc R . . C34 C 0.04783(15) 0.2946(3) 0.05841(17) 0.0204(6) Uani 1 1 d . . . C35 C 0.07563(16) 0.4013(3) 0.03062(19) 0.0261(6) Uani 1 1 d . . . H35A H 0.1225 0.3854 0.0359 0.039 Uiso 1 1 calc R . . H35B H 0.0750 0.4703 0.0617 0.039 Uiso 1 1 calc R . . H35C H 0.0473 0.4167 -0.0236 0.039 Uiso 1 1 calc R . . C36 C 0.08875(17) 0.2699(3) 0.14391(18) 0.0262(6) Uani 1 1 d . . . H36A H 0.1364 0.2550 0.1522 0.039 Uiso 1 1 calc R . . H36B H 0.0699 0.2006 0.1598 0.039 Uiso 1 1 calc R . . H36C H 0.0861 0.3383 0.1745 0.039 Uiso 1 1 calc R . . C37 C -0.02611(16) 0.3159(3) 0.04738(19) 0.0247(6) Uani 1 1 d . . . H37A H -0.0527 0.3363 -0.0066 0.037 Uiso 1 1 calc R . . H37B H -0.0283 0.3809 0.0807 0.037 Uiso 1 1 calc R . . H37C H -0.0448 0.2443 0.0609 0.037 Uiso 1 1 calc R . . C41 C 0.25656(15) -0.0038(3) -0.04263(16) 0.0200(6) Uani 1 1 d . . . N41 N 0.18887(13) 0.0080(2) -0.08068(14) 0.0196(5) Uani 1 1 d . . . N42 N 0.28853(13) 0.0587(2) -0.08069(14) 0.0215(5) Uani 1 1 d . . . C42 C 0.17799(16) 0.0808(3) -0.14306(17) 0.0220(6) Uani 1 1 d . . . H42A H 0.1348 0.1049 -0.1794 0.026 Uiso 1 1 calc R . . C43 C 0.23871(16) 0.1121(3) -0.14390(17) 0.0238(6) Uani 1 1 d . . . H43A H 0.2461 0.1614 -0.1808 0.029 Uiso 1 1 calc R . . C44 C 0.36407(16) 0.0707(3) -0.05931(19) 0.0287(7) Uani 1 1 d . . . C45 C 0.3947(2) -0.0519(4) -0.0574(2) 0.0432(10) Uani 1 1 d . . . H45A H 0.3746 -0.0878 -0.1087 0.065 Uiso 1 1 calc R . . H45B H 0.3850 -0.1015 -0.0201 0.065 Uiso 1 1 calc R . . H45C H 0.4440 -0.0451 -0.0422 0.065 Uiso 1 1 calc R . . C46 C 0.39485(18) 0.1348(4) 0.0182(2) 0.0389(9) Uani 1 1 d . . . H46A H 0.4441 0.1423 0.0332 0.058 Uiso 1 1 calc R . . H46B H 0.3856 0.0897 0.0575 0.058 Uiso 1 1 calc R . . H46C H 0.3745 0.2134 0.0135 0.058 Uiso 1 1 calc R . . C47 C 0.37645(19) 0.1433(4) -0.1207(2) 0.0376(8) Uani 1 1 d . . . H47A H 0.3593 0.1003 -0.1697 0.056 Uiso 1 1 calc R . . H47B H 0.4254 0.1574 -0.1050 0.056 Uiso 1 1 calc R . . H47C H 0.3526 0.2189 -0.1271 0.056 Uiso 1 1 calc R . . C51 C -0.03071(19) 0.1261(4) 0.2769(2) 0.0407(9) Uani 1 1 d . . . N51 N -0.0299(2) 0.0289(4) 0.2905(3) 0.0692(14) Uani 1 1 d . . . C52 C -0.0309(2) 0.2505(4) 0.2582(2) 0.0424(9) Uani 1 1 d . . . H52A H -0.0461 0.2969 0.2925 0.064 Uiso 1 1 calc R . . H52B H -0.0619 0.2635 0.2046 0.064 Uiso 1 1 calc R . . H52C H 0.0152 0.2748 0.2649 0.064 Uiso 1 1 calc R . . N61 N 0.4147(4) -0.3355(8) -0.0559(5) 0.073(3) Uiso 0.50 1 d PD A -1 C61 C 0.4648(4) -0.3877(7) -0.0345(4) 0.0429(18) Uiso 0.50 1 d PD A -1 C62 C 0.5275(5) -0.4544(12) 0.0087(8) 0.096(4) Uiso 0.50 1 d PD A -1 H62A H 0.5495 -0.4779 -0.0264 0.144 Uiso 0.50 1 calc PR A -1 H62B H 0.5161 -0.5249 0.0314 0.144 Uiso 0.50 1 calc PR A -1 H62C H 0.5587 -0.4047 0.0498 0.144 Uiso 0.50 1 calc PR A -1 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 0.01710(10) 0.01993(10) 0.01283(9) 0.00038(7) 0.00627(7) 0.00003(7) Br 0.02227(15) 0.03104(17) 0.02941(17) -0.00920(13) 0.00827(12) -0.00671(12) S1 0.0226(3) 0.0278(4) 0.0246(4) 0.0112(3) 0.0137(3) 0.0072(3) S2 0.0192(3) 0.0236(4) 0.0200(3) 0.0031(3) 0.0035(3) 0.0014(3) S3 0.0178(3) 0.0191(3) 0.0180(3) 0.0001(3) 0.0059(3) 0.0003(3) S4 0.0308(4) 0.0255(4) 0.0154(3) 0.0027(3) 0.0104(3) 0.0095(3) B1 0.0204(15) 0.0278(17) 0.0179(15) 0.0005(13) 0.0058(12) -0.0005(13) B2 0.0277(17) 0.0182(15) 0.0228(16) -0.0018(13) 0.0126(14) -0.0007(13) N11 0.0221(12) 0.0244(13) 0.0192(12) 0.0029(10) 0.0106(10) -0.0003(10) C11 0.0175(13) 0.0246(15) 0.0204(14) 0.0050(11) 0.0095(11) 0.0015(11) C12 0.0366(18) 0.0239(16) 0.0260(16) 0.0075(13) 0.0148(14) 0.0015(13) N12 0.0286(13) 0.0260(13) 0.0188(12) 0.0025(10) 0.0117(10) 0.0008(11) C13 0.0424(19) 0.0284(17) 0.0221(15) 0.0086(13) 0.0154(14) 0.0039(15) C14 0.0390(18) 0.0301(17) 0.0243(16) -0.0023(13) 0.0148(14) 0.0015(15) C15 0.074(3) 0.047(2) 0.0240(18) -0.0030(17) 0.0213(19) 0.006(2) C16 0.046(2) 0.042(2) 0.044(2) -0.0127(18) 0.0174(18) -0.0121(18) C17 0.048(2) 0.042(2) 0.038(2) 0.0010(17) 0.0250(18) 0.0140(18) C21 0.0208(14) 0.0278(16) 0.0150(13) 0.0038(11) 0.0054(11) 0.0031(12) N21 0.0222(12) 0.0272(13) 0.0161(11) 0.0000(10) 0.0060(10) 0.0001(10) N22 0.0245(13) 0.0283(14) 0.0216(13) 0.0021(11) 0.0086(10) 0.0053(11) C22 0.0333(17) 0.0268(16) 0.0192(14) -0.0026(12) 0.0067(13) -0.0006(13) C23 0.0355(18) 0.0283(17) 0.0257(16) -0.0009(13) 0.0102(14) 0.0055(14) C24 0.0236(15) 0.041(2) 0.0292(17) 0.0083(15) 0.0119(13) 0.0103(14) C25 0.038(2) 0.052(3) 0.069(3) 0.003(2) 0.024(2) 0.0199(19) C26 0.0221(16) 0.063(3) 0.0255(17) 0.0105(17) 0.0065(13) 0.0062(16) C27 0.0300(18) 0.063(3) 0.0304(18) 0.0111(18) 0.0170(15) 0.0098(17) C31 0.0201(13) 0.0190(13) 0.0165(13) 0.0029(10) 0.0079(11) 0.0008(11) N31 0.0207(12) 0.0211(12) 0.0168(11) -0.0015(9) 0.0081(10) -0.0020(10) N32 0.0185(11) 0.0191(12) 0.0168(11) 0.0006(9) 0.0062(9) 0.0015(9) C32 0.0215(14) 0.0252(15) 0.0180(13) -0.0010(12) 0.0041(11) -0.0023(12) C33 0.0186(13) 0.0235(15) 0.0204(14) 0.0014(11) 0.0046(11) -0.0006(11) C34 0.0244(14) 0.0174(14) 0.0205(14) 0.0003(11) 0.0096(12) 0.0024(11) C35 0.0270(15) 0.0205(15) 0.0317(17) 0.0022(12) 0.0123(13) 0.0014(12) C36 0.0318(16) 0.0257(16) 0.0205(14) -0.0013(12) 0.0094(13) 0.0072(13) C37 0.0238(15) 0.0224(15) 0.0304(16) 0.0013(12) 0.0133(13) 0.0036(12) C41 0.0249(14) 0.0219(14) 0.0146(12) -0.0002(11) 0.0094(11) 0.0048(12) N41 0.0246(12) 0.0199(12) 0.0160(11) -0.0012(9) 0.0096(10) 0.0019(10) N42 0.0224(12) 0.0270(13) 0.0162(11) -0.0001(10) 0.0087(10) 0.0008(10) C42 0.0265(15) 0.0225(14) 0.0153(13) 0.0003(11) 0.0062(11) 0.0025(12) C43 0.0280(15) 0.0269(16) 0.0164(13) 0.0025(11) 0.0084(12) 0.0000(12) C44 0.0219(15) 0.043(2) 0.0228(15) 0.0016(14) 0.0099(12) 0.0007(14) C45 0.035(2) 0.058(3) 0.046(2) 0.007(2) 0.0258(18) 0.0147(19) C46 0.0271(17) 0.061(3) 0.0252(17) -0.0036(17) 0.0065(14) -0.0071(17) C47 0.0325(18) 0.056(2) 0.0289(17) 0.0032(17) 0.0169(15) -0.0070(17) C51 0.0298(18) 0.056(3) 0.0333(19) 0.0096(18) 0.0084(15) -0.0073(17) N51 0.045(2) 0.071(3) 0.073(3) 0.037(2) 0.002(2) -0.009(2) C52 0.048(2) 0.046(2) 0.041(2) -0.0132(18) 0.0244(19) -0.0083(18) _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 S4 2.5112(8) . ? In S1 2.5134(8) . ? In Br 2.5920(4) . ? In S2 2.6181(8) . ? In S3 2.6192(7) . ? S1 C11 1.731(3) . ? S2 C21 1.732(3) . ? S3 C31 1.733(3) . ? S4 C41 1.738(3) . ? B1 H2 1.099(18) . ? B1 H1 1.102(18) . ? B1 N21 1.557(4) . ? B1 N11 1.559(4) . ? B2 H4 1.100(18) . ? B2 H3 1.102(18) . ? B2 N41 1.559(4) . ? B2 N31 1.560(4) . ? N11 C11 1.343(4) . ? N11 C12 1.380(4) . ? C11 N12 1.363(4) . ? C12 C13 1.344(5) . ? N12 C13 1.382(4) . ? N12 C14 1.506(4) . ? C14 C16 1.525(5) . ? C14 C17 1.526(5) . ? C14 C15 1.535(5) . ? C21 N21 1.349(4) . ? C21 N22 1.369(4) . ? N21 C22 1.376(4) . ? N22 C23 1.384(4) . ? N22 C24 1.510(4) . ? C22 C23 1.342(5) . ? C24 C26 1.523(5) . ? C24 C25 1.525(5) . ? C24 C27 1.530(5) . ? C31 N31 1.347(4) . ? C31 N32 1.366(4) . ? N31 C32 1.378(4) . ? N32 C33 1.387(4) . ? N32 C34 1.507(4) . ? C32 C33 1.348(4) . ? C34 C35 1.526(4) . ? C34 C37 1.526(4) . ? C34 C36 1.531(4) . ? C41 N41 1.346(4) . ? C41 N42 1.362(4) . ? N41 C42 1.379(4) . ? N42 C43 1.390(4) . ? N42 C44 1.506(4) . ? C42 C43 1.347(4) . ? C44 C47 1.522(5) . ? C44 C45 1.532(6) . ? C44 C46 1.532(5) . ? C51 N51 1.131(6) . ? C51 C52 1.454(6) . ? N61 C61 1.1475(10) . ? C61 C62 1.4776(10) . ? 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 S4 In S1 147.45(3) . . ? S4 In Br 108.17(2) . . ? S1 In Br 104.38(2) . . ? S4 In S2 83.66(3) . . ? S1 In S2 98.61(2) . . ? Br In S2 86.73(2) . . ? S4 In S3 97.06(2) . . ? S1 In S3 85.02(2) . . ? Br In S3 85.589(19) . . ? S2 In S3 172.12(2) . . ? C11 S1 In 104.63(10) . . ? C21 S2 In 113.43(10) . . ? C31 S3 In 109.40(10) . . ? C41 S4 In 105.52(10) . . ? H2 B1 H1 112(3) . . ? H2 B1 N21 104.4(19) . . ? H1 B1 N21 113.8(19) . . ? H2 B1 N11 110.3(19) . . ? H1 B1 N11 109.0(19) . . ? N21 B1 N11 107.0(2) . . ? H4 B2 H3 109(3) . . ? H4 B2 N41 111.2(19) . . ? H3 B2 N41 113.0(19) . . ? H4 B2 N31 106.6(19) . . ? H3 B2 N31 107.0(19) . . ? N41 B2 N31 109.6(2) . . ? C11 N11 C12 107.8(3) . . ? C11 N11 B1 129.4(3) . . ? C12 N11 B1 122.6(3) . . ? N11 C11 N12 108.6(3) . . ? N11 C11 S1 124.6(2) . . ? N12 C11 S1 126.7(2) . . ? C13 C12 N11 108.4(3) . . ? C11 N12 C13 107.5(3) . . ? C11 N12 C14 127.8(3) . . ? C13 N12 C14 124.5(3) . . ? C12 C13 N12 107.6(3) . . ? N12 C14 C16 108.5(3) . . ? N12 C14 C17 110.1(3) . . ? C16 C14 C17 112.0(3) . . ? N12 C14 C15 108.8(3) . . ? C16 C14 C15 109.0(3) . . ? C17 C14 C15 108.3(3) . . ? N21 C21 N22 107.8(3) . . ? N21 C21 S2 125.4(2) . . ? N22 C21 S2 126.5(2) . . ? C21 N21 C22 108.1(3) . . ? C21 N21 B1 127.1(3) . . ? C22 N21 B1 124.8(3) . . ? C21 N22 C23 108.0(3) . . ? C21 N22 C24 127.5(3) . . ? C23 N22 C24 124.5(3) . . ? C23 C22 N21 108.7(3) . . ? C22 C23 N22 107.3(3) . . ? N22 C24 C26 109.3(3) . . ? N22 C24 C25 109.1(3) . . ? C26 C24 C25 108.5(3) . . ? N22 C24 C27 109.1(3) . . ? C26 C24 C27 111.7(3) . . ? C25 C24 C27 109.2(3) . . ? N31 C31 N32 108.3(2) . . ? N31 C31 S3 124.7(2) . . ? N32 C31 S3 126.8(2) . . ? C31 N31 C32 107.9(2) . . ? C31 N31 B2 127.7(3) . . ? C32 N31 B2 123.7(3) . . ? C31 N32 C33 108.0(2) . . ? C31 N32 C34 127.8(2) . . ? C33 N32 C34 124.1(2) . . ? C33 C32 N31 108.7(3) . . ? C32 C33 N32 107.1(3) . . ? N32 C34 C35 107.8(2) . . ? N32 C34 C37 108.8(2) . . ? C35 C34 C37 110.1(2) . . ? N32 C34 C36 110.5(2) . . ? C35 C34 C36 111.5(3) . . ? C37 C34 C36 108.2(2) . . ? N41 C41 N42 108.6(2) . . ? N41 C41 S4 125.2(2) . . ? N42 C41 S4 126.2(2) . . ? C41 N41 C42 107.8(2) . . ? C41 N41 B2 128.1(3) . . ? C42 N41 B2 124.0(3) . . ? C41 N42 C43 107.8(2) . . ? C41 N42 C44 127.3(3) . . ? C43 N42 C44 125.0(3) . . ? C43 C42 N41 108.7(3) . . ? C42 C43 N42 107.2(3) . . ? N42 C44 C47 109.0(3) . . ? N42 C44 C45 109.0(3) . . ? C47 C44 C45 108.2(3) . . ? N42 C44 C46 108.6(3) . . ? C47 C44 C46 109.3(3) . . ? C45 C44 C46 112.8(3) . . ? N51 C51 C52 178.6(5) . . ? N61 C61 C62 167.9(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.317 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.107 # Attachment '- BmBut2InCl (ky285s10).cif' data_ky285s10 _database_code_depnum_ccdc_archive 'CCDC 776951' #TrackingRef '- BmBut2InCl (ky285s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H54 B2 Cl In N10 S4' _chemical_formula_weight 878.98 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3310(7) _cell_length_b 11.3612(8) _cell_length_c 18.9319(13) _cell_angle_alpha 102.7120(10) _cell_angle_beta 91.8870(10) _cell_angle_gamma 90.7230(10) _cell_volume 2166.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9875 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 32.61 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8849 _exptl_absorpt_correction_T_max 0.8849 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30397 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10733 _reflns_number_gt 9421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0279P)^2^+0.6642P] 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 10733 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0598 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 In In 0.033942(11) 0.208638(10) 0.257839(6) 0.01478(4) Uani 1 1 d . . . Cl Cl 0.17592(5) 0.03826(4) 0.21496(2) 0.02831(10) Uani 1 1 d . . . S1 S 0.15583(4) 0.38901(4) 0.32895(2) 0.02028(9) Uani 1 1 d . . . S2 S 0.07084(4) 0.25320(4) 0.12946(2) 0.01825(9) Uani 1 1 d . . . S3 S 0.02717(4) 0.12477(4) 0.37367(2) 0.02060(9) Uani 1 1 d . . . S4 S -0.19843(4) 0.17722(4) 0.21746(2) 0.02272(10) Uani 1 1 d . . . B1 B -0.0333(2) 0.5209(2) 0.22450(12) 0.0231(4) Uani 1 1 d . . . H1 H -0.063(2) 0.6191(19) 0.2303(11) 0.028 Uiso 1 1 d . . . H2 H -0.067(2) 0.4791(18) 0.2680(11) 0.028 Uiso 1 1 d . . . B2 B -0.2051(2) 0.32986(19) 0.39016(11) 0.0214(4) Uani 1 1 d . . . H3 H -0.2763(19) 0.3984(18) 0.4169(11) 0.026 Uiso 1 1 d . . . H4 H -0.1562(19) 0.3608(18) 0.3472(11) 0.026 Uiso 1 1 d . . . N11 N 0.11808(14) 0.52049(13) 0.22538(8) 0.0214(3) Uani 1 1 d . . . C11 C 0.20007(17) 0.46730(15) 0.26468(9) 0.0188(3) Uani 1 1 d . . . N12 N 0.32342(14) 0.48754(13) 0.24624(9) 0.0223(3) Uani 1 1 d . . . C12 C 0.19008(19) 0.57303(18) 0.18058(12) 0.0301(4) Uani 1 1 d . . . H12A H 0.1565 0.6159 0.1465 0.036 Uiso 1 1 calc R . . C13 C 0.31620(19) 0.55371(18) 0.19301(12) 0.0310(4) Uani 1 1 d . . . H13A H 0.3872 0.5805 0.1696 0.037 Uiso 1 1 calc R . . C14 C 0.44704(17) 0.44534(17) 0.27681(11) 0.0270(4) Uani 1 1 d . . . C15 C 0.4449(2) 0.30745(18) 0.25927(13) 0.0348(5) Uani 1 1 d . . . H15A H 0.4355 0.2772 0.2067 0.052 Uiso 1 1 calc R . . H15B H 0.3719 0.2780 0.2827 0.052 Uiso 1 1 calc R . . H15C H 0.5261 0.2787 0.2771 0.052 Uiso 1 1 calc R . . C16 C 0.4579(2) 0.4989(2) 0.35813(12) 0.0365(5) Uani 1 1 d . . . H16A H 0.3857 0.4687 0.3819 0.055 Uiso 1 1 calc R . . H16B H 0.4549 0.5871 0.3668 0.055 Uiso 1 1 calc R . . H16C H 0.5400 0.4754 0.3779 0.055 Uiso 1 1 calc R . . C17 C 0.56192(19) 0.4898(2) 0.24037(14) 0.0408(6) Uani 1 1 d . . . H17A H 0.5534 0.4582 0.1879 0.061 Uiso 1 1 calc R . . H17B H 0.6426 0.4615 0.2591 0.061 Uiso 1 1 calc R . . H17C H 0.5635 0.5782 0.2508 0.061 Uiso 1 1 calc R . . C21 C -0.05675(16) 0.33907(15) 0.10962(9) 0.0172(3) Uani 1 1 d . . . N21 N -0.08726(14) 0.44917(13) 0.14845(8) 0.0191(3) Uani 1 1 d . . . C22 C -0.19198(17) 0.48912(17) 0.11406(10) 0.0235(4) Uani 1 1 d . . . H22A H -0.2335 0.5640 0.1298 0.028 Uiso 1 1 calc R . . N22 N -0.14145(14) 0.30954(13) 0.05103(8) 0.0191(3) Uani 1 1 d . . . C23 C -0.22566(18) 0.40432(17) 0.05428(10) 0.0248(4) Uani 1 1 d . . . H23A H -0.2946 0.4087 0.0205 0.030 Uiso 1 1 calc R . . C24 C -0.14199(17) 0.19895(17) -0.01010(9) 0.0216(4) Uani 1 1 d . . . C25 C -0.25936(18) 0.20284(19) -0.06076(10) 0.0275(4) Uani 1 1 d . . . H25A H -0.3388 0.1917 -0.0359 0.041 Uiso 1 1 calc R . . H25B H -0.2538 0.1382 -0.1043 0.041 Uiso 1 1 calc R . . H25C H -0.2607 0.2811 -0.0745 0.041 Uiso 1 1 calc R . . C26 C -0.01775(18) 0.20078(19) -0.05167(10) 0.0275(4) Uani 1 1 d . . . H26A H 0.0574 0.1951 -0.0197 0.041 Uiso 1 1 calc R . . H26B H -0.0117 0.2762 -0.0685 0.041 Uiso 1 1 calc R . . H26C H -0.0193 0.1322 -0.0934 0.041 Uiso 1 1 calc R . . C27 C -0.1552(2) 0.08462(17) 0.01919(10) 0.0272(4) Uani 1 1 d . . . H27A H -0.0791 0.0776 0.0502 0.041 Uiso 1 1 calc R . . H27B H -0.1618 0.0141 -0.0213 0.041 Uiso 1 1 calc R . . H27C H -0.2334 0.0888 0.0475 0.041 Uiso 1 1 calc R . . N31 N -0.10587(14) 0.31356(13) 0.45118(8) 0.0177(3) Uani 1 1 d . . . C31 C -0.00290(16) 0.24111(15) 0.44665(9) 0.0169(3) Uani 1 1 d . . . N32 N 0.06833(14) 0.27159(13) 0.51046(8) 0.0186(3) Uani 1 1 d . . . C32 C -0.10002(17) 0.38977(16) 0.51902(9) 0.0215(4) Uani 1 1 d . . . H32A H -0.1611 0.4499 0.5369 0.026 Uiso 1 1 calc R . . C33 C 0.00607(17) 0.36500(16) 0.55559(9) 0.0216(4) Uani 1 1 d . . . H33A H 0.0334 0.4042 0.6035 0.026 Uiso 1 1 calc R . . C34 C 0.19462(17) 0.21866(18) 0.52957(10) 0.0240(4) Uani 1 1 d . . . C35 C 0.1743(2) 0.08480(19) 0.52728(11) 0.0331(5) Uani 1 1 d . . . H35A H 0.1073 0.0745 0.5610 0.050 Uiso 1 1 calc R . . H35B H 0.2556 0.0511 0.5413 0.050 Uiso 1 1 calc R . . H35C H 0.1469 0.0427 0.4781 0.050 Uiso 1 1 calc R . . C36 C 0.2379(2) 0.2827(2) 0.60676(11) 0.0334(5) Uani 1 1 d . . . H36A H 0.1713 0.2712 0.6405 0.050 Uiso 1 1 calc R . . H36B H 0.2506 0.3691 0.6091 0.050 Uiso 1 1 calc R . . H36C H 0.3195 0.2488 0.6201 0.050 Uiso 1 1 calc R . . C37 C 0.29678(19) 0.2418(2) 0.47758(13) 0.0412(6) Uani 1 1 d . . . H37A H 0.2690 0.2030 0.4278 0.062 Uiso 1 1 calc R . . H37B H 0.3794 0.2084 0.4898 0.062 Uiso 1 1 calc R . . H37C H 0.3075 0.3289 0.4817 0.062 Uiso 1 1 calc R . . N41 N -0.27800(13) 0.20805(13) 0.35755(8) 0.0183(3) Uani 1 1 d . . . C41 C -0.27832(16) 0.14109(16) 0.28947(9) 0.0178(3) Uani 1 1 d . . . C42 C -0.35987(17) 0.15242(17) 0.39665(10) 0.0222(4) Uani 1 1 d . . . H42A H -0.3775 0.1803 0.4464 0.027 Uiso 1 1 calc R . . N42 N -0.35943(14) 0.04399(13) 0.28471(8) 0.0190(3) Uani 1 1 d . . . C43 C -0.41067(17) 0.05210(17) 0.35266(10) 0.0235(4) Uani 1 1 d . . . H43A H -0.4705 -0.0031 0.3656 0.028 Uiso 1 1 calc R . . C44 C -0.38755(18) -0.05719(16) 0.21977(10) 0.0238(4) Uani 1 1 d . . . C45 C -0.44807(19) -0.00692(18) 0.15823(10) 0.0267(4) Uani 1 1 d . . . H45A H -0.5313 0.0293 0.1730 0.040 Uiso 1 1 calc R . . H45B H -0.4619 -0.0724 0.1152 0.040 Uiso 1 1 calc R . . H45C H -0.3899 0.0547 0.1469 0.040 Uiso 1 1 calc R . . C46 C -0.4866(2) -0.14433(18) 0.23999(12) 0.0347(5) Uani 1 1 d . . . H46A H -0.4482 -0.1823 0.2772 0.052 Uiso 1 1 calc R . . H46B H -0.5117 -0.2067 0.1969 0.052 Uiso 1 1 calc R . . H46C H -0.5633 -0.0998 0.2588 0.052 Uiso 1 1 calc R . . C47 C -0.2618(2) -0.1234(2) 0.19897(13) 0.0380(5) Uani 1 1 d . . . H47A H -0.2267 -0.1534 0.2403 0.057 Uiso 1 1 calc R . . H47B H -0.1987 -0.0678 0.1855 0.057 Uiso 1 1 calc R . . H47C H -0.2793 -0.1915 0.1578 0.057 Uiso 1 1 calc R . . C51 C -0.2940(2) 0.17296(19) 0.61727(12) 0.0368(5) Uani 1 1 d . . . N51 N -0.3914(2) 0.1672(2) 0.58686(13) 0.0554(6) Uani 1 1 d . . . C52 C -0.1703(2) 0.1804(2) 0.65734(14) 0.0431(6) Uani 1 1 d . . . H52A H -0.1008 0.1566 0.6234 0.065 Uiso 1 1 calc R . . H52B H -0.1726 0.1262 0.6910 0.065 Uiso 1 1 calc R . . H52C H -0.1542 0.2635 0.6846 0.065 Uiso 1 1 calc R . . C61 C -0.4211(2) 0.6614(2) 0.02172(14) 0.0405(6) Uani 1 1 d . . . N61 N -0.4599(2) 0.62501(19) 0.06767(12) 0.0467(5) Uani 1 1 d . . . C62 C -0.3752(4) 0.7123(4) -0.0372(2) 0.1003(14) Uani 1 1 d . . . H62A H -0.3764 0.6494 -0.0819 0.150 Uiso 1 1 calc R . . H62B H -0.2865 0.7438 -0.0254 0.150 Uiso 1 1 calc R . . H62C H -0.4317 0.7779 -0.0439 0.150 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 0.01466(6) 0.01524(6) 0.01377(6) 0.00181(4) -0.00015(4) 0.00074(4) Cl 0.0373(3) 0.0267(2) 0.0205(2) 0.00308(18) 0.00461(18) 0.0164(2) S1 0.0225(2) 0.0198(2) 0.0171(2) 0.00145(16) -0.00278(16) -0.00313(17) S2 0.0176(2) 0.0223(2) 0.01568(19) 0.00575(16) 0.00080(15) 0.00508(16) S3 0.0284(2) 0.0188(2) 0.0148(2) 0.00368(16) 0.00255(17) 0.00604(17) S4 0.0164(2) 0.0360(3) 0.0159(2) 0.00676(18) -0.00204(16) -0.00618(18) B1 0.0182(10) 0.0243(10) 0.0250(10) 0.0023(8) -0.0047(8) 0.0020(8) B2 0.0206(10) 0.0228(10) 0.0198(10) 0.0039(8) -0.0061(8) 0.0006(8) N11 0.0187(7) 0.0185(7) 0.0273(8) 0.0061(6) -0.0042(6) -0.0012(6) C11 0.0187(8) 0.0146(8) 0.0215(9) 0.0011(7) -0.0037(7) -0.0015(6) N12 0.0162(7) 0.0201(8) 0.0312(9) 0.0074(6) -0.0018(6) -0.0014(6) C12 0.0279(10) 0.0275(10) 0.0395(12) 0.0184(9) -0.0041(9) -0.0031(8) C13 0.0249(10) 0.0314(11) 0.0420(12) 0.0193(9) 0.0021(9) -0.0038(8) C14 0.0144(8) 0.0255(10) 0.0413(12) 0.0085(8) -0.0043(8) 0.0021(7) C15 0.0254(10) 0.0258(10) 0.0533(14) 0.0085(10) -0.0002(9) 0.0080(8) C16 0.0229(10) 0.0399(12) 0.0435(13) 0.0047(10) -0.0139(9) -0.0015(9) C17 0.0176(10) 0.0434(13) 0.0640(16) 0.0174(12) 0.0015(10) -0.0005(9) C21 0.0150(8) 0.0205(8) 0.0173(8) 0.0067(7) 0.0009(6) 0.0006(6) N21 0.0163(7) 0.0193(7) 0.0218(7) 0.0051(6) -0.0015(6) 0.0016(6) C22 0.0185(9) 0.0225(9) 0.0295(10) 0.0062(8) -0.0013(7) 0.0064(7) N22 0.0162(7) 0.0229(8) 0.0182(7) 0.0044(6) -0.0004(6) 0.0031(6) C23 0.0200(9) 0.0270(10) 0.0278(10) 0.0073(8) -0.0040(7) 0.0059(7) C24 0.0193(9) 0.0270(9) 0.0163(8) -0.0001(7) 0.0001(7) 0.0028(7) C25 0.0216(9) 0.0356(11) 0.0231(9) 0.0019(8) -0.0020(7) 0.0029(8) C26 0.0228(9) 0.0412(12) 0.0186(9) 0.0065(8) 0.0023(7) 0.0042(8) C27 0.0323(10) 0.0234(9) 0.0236(9) 0.0006(8) 0.0004(8) -0.0007(8) N31 0.0167(7) 0.0189(7) 0.0164(7) 0.0015(6) -0.0008(5) 0.0013(6) C31 0.0177(8) 0.0185(8) 0.0148(8) 0.0045(6) 0.0007(6) -0.0009(6) N32 0.0167(7) 0.0213(7) 0.0172(7) 0.0035(6) -0.0017(6) 0.0004(6) C32 0.0221(9) 0.0217(9) 0.0181(8) -0.0014(7) -0.0001(7) 0.0025(7) C33 0.0248(9) 0.0219(9) 0.0154(8) -0.0014(7) -0.0015(7) -0.0015(7) C34 0.0182(9) 0.0332(10) 0.0227(9) 0.0113(8) -0.0023(7) 0.0045(7) C35 0.0383(12) 0.0327(11) 0.0296(11) 0.0100(9) -0.0062(9) 0.0103(9) C36 0.0278(10) 0.0430(12) 0.0285(11) 0.0083(9) -0.0129(8) 0.0003(9) C37 0.0163(9) 0.0746(17) 0.0410(13) 0.0300(12) 0.0021(9) 0.0053(10) N41 0.0148(7) 0.0230(7) 0.0165(7) 0.0035(6) -0.0025(5) 0.0009(6) C41 0.0128(8) 0.0236(9) 0.0171(8) 0.0051(7) -0.0020(6) -0.0003(6) C42 0.0192(9) 0.0302(10) 0.0180(8) 0.0067(7) 0.0022(7) 0.0019(7) N42 0.0172(7) 0.0206(7) 0.0188(7) 0.0035(6) -0.0014(6) -0.0009(6) C43 0.0194(9) 0.0309(10) 0.0228(9) 0.0112(8) 0.0023(7) -0.0023(7) C44 0.0233(9) 0.0216(9) 0.0240(9) -0.0002(7) -0.0022(7) -0.0016(7) C45 0.0261(10) 0.0298(10) 0.0215(9) 0.0013(8) -0.0058(7) -0.0066(8) C46 0.0423(12) 0.0255(10) 0.0349(11) 0.0053(9) -0.0047(9) -0.0113(9) C47 0.0338(12) 0.0309(11) 0.0430(13) -0.0057(10) -0.0025(10) 0.0084(9) C51 0.0509(14) 0.0282(11) 0.0344(12) 0.0108(9) 0.0179(11) 0.0070(10) N51 0.0540(14) 0.0652(16) 0.0519(14) 0.0223(12) 0.0083(11) 0.0051(12) C52 0.0508(15) 0.0299(12) 0.0489(14) 0.0091(10) 0.0057(11) 0.0014(10) C61 0.0237(11) 0.0479(14) 0.0404(13) -0.0109(11) 0.0021(9) 0.0052(10) N61 0.0412(12) 0.0460(12) 0.0503(13) 0.0058(10) -0.0073(10) 0.0104(9) C62 0.094(3) 0.136(4) 0.068(2) 0.011(2) 0.040(2) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In Cl 2.4527(5) . ? In S1 2.4913(5) . ? In S4 2.4925(5) . ? In S3 2.5787(5) . ? In S2 2.6281(5) . ? S1 C11 1.7271(18) . ? S2 C21 1.7295(17) . ? S3 C31 1.7284(17) . ? S4 C41 1.7379(17) . ? B1 H2 1.10(2) . ? B1 H1 1.14(2) . ? B1 N11 1.564(2) . ? B1 N21 1.571(2) . ? B2 H4 1.09(2) . ? B2 H3 1.13(2) . ? B2 N41 1.559(2) . ? B2 N31 1.562(2) . ? N11 C11 1.344(2) . ? N11 C12 1.372(2) . ? C11 N12 1.362(2) . ? N12 C13 1.384(2) . ? N12 C14 1.511(2) . ? C12 C13 1.346(3) . ? C14 C16 1.526(3) . ? C14 C17 1.527(3) . ? C14 C15 1.528(3) . ? C21 N21 1.351(2) . ? C21 N22 1.369(2) . ? N21 C22 1.377(2) . ? C22 C23 1.348(3) . ? N22 C23 1.385(2) . ? N22 C24 1.509(2) . ? C24 C27 1.527(3) . ? C24 C25 1.528(2) . ? C24 C26 1.530(2) . ? N31 C31 1.347(2) . ? N31 C32 1.381(2) . ? C31 N32 1.368(2) . ? N32 C33 1.387(2) . ? N32 C34 1.510(2) . ? C32 C33 1.343(2) . ? C34 C35 1.524(3) . ? C34 C37 1.525(3) . ? C34 C36 1.532(3) . ? N41 C41 1.345(2) . ? N41 C42 1.377(2) . ? C41 N42 1.362(2) . ? C42 C43 1.344(3) . ? N42 C43 1.392(2) . ? N42 C44 1.505(2) . ? C44 C45 1.526(3) . ? C44 C47 1.529(3) . ? C44 C46 1.530(3) . ? C51 N51 1.136(3) . ? C51 C52 1.456(4) . ? C61 N61 1.125(3) . ? C61 C62 1.454(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 112.230(17) . . ? Cl In S4 115.983(17) . . ? S1 In S4 131.657(16) . . ? Cl In S3 84.248(15) . . ? S1 In S3 88.805(15) . . ? S4 In S3 99.076(15) . . ? Cl In S2 83.456(15) . . ? S1 In S2 96.513(15) . . ? S4 In S2 85.701(14) . . ? S3 In S2 167.683(14) . . ? C11 S1 In 104.12(6) . . ? C21 S2 In 107.55(6) . . ? C31 S3 In 109.22(6) . . ? C41 S4 In 106.01(6) . . ? H2 B1 H1 113.7(15) . . ? H2 B1 N11 109.1(11) . . ? H1 B1 N11 106.9(10) . . ? H2 B1 N21 110.8(11) . . ? H1 B1 N21 107.1(10) . . ? N11 B1 N21 109.00(15) . . ? H4 B2 H3 111.0(15) . . ? H4 B2 N41 109.3(11) . . ? H3 B2 N41 109.4(10) . . ? H4 B2 N31 110.8(11) . . ? H3 B2 N31 106.2(10) . . ? N41 B2 N31 110.10(15) . . ? C11 N11 C12 107.93(15) . . ? C11 N11 B1 128.78(16) . . ? C12 N11 B1 123.21(16) . . ? N11 C11 N12 108.55(15) . . ? N11 C11 S1 125.47(14) . . ? N12 C11 S1 125.98(13) . . ? C11 N12 C13 107.53(15) . . ? C11 N12 C14 127.15(15) . . ? C13 N12 C14 125.32(16) . . ? C13 C12 N11 108.62(17) . . ? C12 C13 N12 107.35(17) . . ? N12 C14 C16 109.00(16) . . ? N12 C14 C17 108.77(16) . . ? C16 C14 C17 109.25(17) . . ? N12 C14 C15 108.56(15) . . ? C16 C14 C15 112.38(18) . . ? C17 C14 C15 108.82(17) . . ? N21 C21 N22 108.20(14) . . ? N21 C21 S2 125.54(13) . . ? N22 C21 S2 126.23(13) . . ? C21 N21 C22 107.98(14) . . ? C21 N21 B1 130.22(15) . . ? C22 N21 B1 121.37(15) . . ? C23 C22 N21 108.61(16) . . ? C21 N22 C23 107.73(15) . . ? C21 N22 C24 127.95(14) . . ? C23 N22 C24 124.21(14) . . ? C22 C23 N22 107.49(16) . . ? N22 C24 C27 110.49(14) . . ? N22 C24 C25 108.75(14) . . ? C27 C24 C25 107.58(15) . . ? N22 C24 C26 108.54(15) . . ? C27 C24 C26 111.93(16) . . ? C25 C24 C26 109.49(15) . . ? C31 N31 C32 107.69(14) . . ? C31 N31 B2 129.04(14) . . ? C32 N31 B2 122.56(14) . . ? N31 C31 N32 108.43(14) . . ? N31 C31 S3 124.90(13) . . ? N32 C31 S3 126.59(13) . . ? C31 N32 C33 107.70(14) . . ? C31 N32 C34 127.60(15) . . ? C33 N32 C34 124.66(14) . . ? C33 C32 N31 108.88(15) . . ? C32 C33 N32 107.30(15) . . ? N32 C34 C35 109.51(15) . . ? N32 C34 C37 108.87(15) . . ? C35 C34 C37 112.52(18) . . ? N32 C34 C36 108.49(15) . . ? C35 C34 C36 108.65(16) . . ? C37 C34 C36 108.71(17) . . ? C41 N41 C42 107.92(14) . . ? C41 N41 B2 128.88(15) . . ? C42 N41 B2 123.17(15) . . ? N41 C41 N42 108.68(15) . . ? N41 C41 S4 125.99(13) . . ? N42 C41 S4 125.18(13) . . ? C43 C42 N41 108.62(16) . . ? C41 N42 C43 107.42(14) . . ? C41 N42 C44 127.59(15) . . ? C43 N42 C44 124.96(15) . . ? C42 C43 N42 107.36(16) . . ? N42 C44 C45 109.71(15) . . ? N42 C44 C47 108.60(15) . . ? C45 C44 C47 112.70(17) . . ? N42 C44 C46 108.68(15) . . ? C45 C44 C46 107.58(16) . . ? C47 C44 C46 109.50(17) . . ? N51 C51 C52 179.1(3) . . ? N61 C61 C62 177.6(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.665 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.065 # Attachment '- BmBut2InI (KY283S10).cif' data_ky283s10 _database_code_depnum_ccdc_archive 'CCDC 776952' #TrackingRef '- BmBut2InI (KY283S10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H54 B2 I In N10 S4' _chemical_formula_weight 970.43 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4479(11) _cell_length_b 11.2540(12) _cell_length_c 19.202(2) _cell_angle_alpha 100.971(2) _cell_angle_beta 91.700(2) _cell_angle_gamma 90.610(2) _cell_volume 2215.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9899 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 30.92 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.453 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5302 _exptl_absorpt_correction_T_max 0.8683 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30576 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10947 _reflns_number_gt 8768 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to be 1.1 angstroms. The ADPs of one acetonitrile molecule have been restrained. ; _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^)+(0.0647P)^2^+3.2327P] 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 10947 _refine_ls_number_parameters 464 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 0.03481(2) 0.22451(2) 0.259029(13) 0.02065(8) Uani 1 1 d . . . I I 0.17526(3) 0.01908(2) 0.204874(15) 0.03488(9) Uani 1 1 d . . . S1 S 0.15446(9) 0.39786(8) 0.33381(5) 0.02486(19) Uani 1 1 d . . . S2 S 0.08283(10) 0.29426(9) 0.13960(5) 0.0282(2) Uani 1 1 d . . . S3 S 0.02164(10) 0.13099(8) 0.37197(5) 0.02378(19) Uani 1 1 d . . . S4 S -0.19628(9) 0.21052(9) 0.22197(5) 0.0256(2) Uani 1 1 d . . . B1 B -0.0270(5) 0.5533(4) 0.2386(2) 0.0280(9) Uani 1 1 d D . . H1 H -0.058(4) 0.648(2) 0.242(2) 0.034 Uiso 1 1 d D . . H2 H -0.069(4) 0.511(4) 0.2807(19) 0.034 Uiso 1 1 d D . . B2 B -0.2080(4) 0.3394(4) 0.3932(2) 0.0256(9) Uani 1 1 d D . . H3 H -0.164(4) 0.373(4) 0.3491(17) 0.031 Uiso 1 1 d D . . H4 H -0.274(4) 0.404(3) 0.422(2) 0.031 Uiso 1 1 d D . . N11 N 0.1218(3) 0.5514(3) 0.24053(17) 0.0254(7) Uani 1 1 d . . . C11 C 0.2004(4) 0.4878(3) 0.2756(2) 0.0237(7) Uani 1 1 d . . . N12 N 0.3240(3) 0.5093(3) 0.25829(19) 0.0278(7) Uani 1 1 d . . . C12 C 0.1948(4) 0.6126(4) 0.2000(2) 0.0333(9) Uani 1 1 d . . . H12A H 0.1633 0.6638 0.1696 0.040 Uiso 1 1 calc R . . C13 C 0.3191(4) 0.5875(4) 0.2109(3) 0.0362(10) Uani 1 1 d . . . H13A H 0.3904 0.6181 0.1898 0.043 Uiso 1 1 calc R . . C14 C 0.4437(4) 0.4592(4) 0.2861(2) 0.0325(9) Uani 1 1 d . . . C15 C 0.4402(5) 0.3205(4) 0.2644(3) 0.0422(11) Uani 1 1 d . . . H15A H 0.4309 0.2976 0.2126 0.063 Uiso 1 1 calc R . . H15B H 0.3676 0.2877 0.2862 0.063 Uiso 1 1 calc R . . H15C H 0.5201 0.2878 0.2805 0.063 Uiso 1 1 calc R . . C16 C 0.4547(4) 0.5016(4) 0.3659(3) 0.0412(11) Uani 1 1 d . . . H16A H 0.3816 0.4699 0.3880 0.062 Uiso 1 1 calc R . . H16B H 0.4551 0.5902 0.3772 0.062 Uiso 1 1 calc R . . H16C H 0.5344 0.4720 0.3841 0.062 Uiso 1 1 calc R . . C17 C 0.5592(4) 0.5078(5) 0.2532(3) 0.0480(13) Uani 1 1 d . . . H17A H 0.5548 0.4791 0.2017 0.072 Uiso 1 1 calc R . . H17B H 0.6380 0.4791 0.2730 0.072 Uiso 1 1 calc R . . H17C H 0.5592 0.5965 0.2637 0.072 Uiso 1 1 calc R . . C21 C -0.0462(4) 0.3795(4) 0.1235(2) 0.0267(8) Uani 1 1 d . . . N21 N -0.0807(3) 0.4858(3) 0.16410(17) 0.0260(7) Uani 1 1 d . . . C22 C -0.1880(4) 0.5247(4) 0.1330(2) 0.0323(9) Uani 1 1 d . . . H22A H -0.2327 0.5968 0.1504 0.039 Uiso 1 1 calc R . . N22 N -0.1322(3) 0.3532(3) 0.06714(18) 0.0300(7) Uani 1 1 d . . . C23 C -0.2200(4) 0.4435(5) 0.0731(2) 0.0379(10) Uani 1 1 d . . . H23A H -0.2903 0.4484 0.0413 0.045 Uiso 1 1 calc R . . C24 C -0.1279(4) 0.2486(4) 0.0047(2) 0.0357(10) Uani 1 1 d . . . C25 C -0.2474(5) 0.2535(6) -0.0424(3) 0.0518(14) Uani 1 1 d . . . H25A H -0.3239 0.2419 -0.0159 0.078 Uiso 1 1 calc R . . H25B H -0.2443 0.1894 -0.0846 0.078 Uiso 1 1 calc R . . H25C H -0.2508 0.3325 -0.0568 0.078 Uiso 1 1 calc R . . C26 C -0.0097(5) 0.2642(5) -0.0368(2) 0.0444(12) Uani 1 1 d . . . H26A H 0.0671 0.2595 -0.0070 0.067 Uiso 1 1 calc R . . H26B H -0.0114 0.3432 -0.0512 0.067 Uiso 1 1 calc R . . H26C H -0.0084 0.2000 -0.0792 0.067 Uiso 1 1 calc R . . C27 C -0.1312(6) 0.1284(5) 0.0295(3) 0.0518(14) Uani 1 1 d . . . H27A H -0.0555 0.1227 0.0600 0.078 Uiso 1 1 calc R . . H27B H -0.1315 0.0620 -0.0117 0.078 Uiso 1 1 calc R . . H27C H -0.2087 0.1229 0.0563 0.078 Uiso 1 1 calc R . . N31 N -0.1073(3) 0.3174(3) 0.45019(16) 0.0228(6) Uani 1 1 d . . . C31 C -0.0050(4) 0.2449(3) 0.44405(19) 0.0219(7) Uani 1 1 d . . . N32 N 0.0682(3) 0.2717(3) 0.50555(16) 0.0220(6) Uani 1 1 d . . . C32 C -0.0990(4) 0.3903(4) 0.5165(2) 0.0268(8) Uani 1 1 d . . . H32A H -0.1590 0.4499 0.5351 0.032 Uiso 1 1 calc R . . C33 C 0.0082(4) 0.3633(3) 0.5508(2) 0.0263(8) Uani 1 1 d . . . H33A H 0.0371 0.4002 0.5974 0.032 Uiso 1 1 calc R . . C34 C 0.1913(4) 0.2157(4) 0.5236(2) 0.0266(8) Uani 1 1 d . . . C35 C 0.1677(5) 0.0821(4) 0.5239(2) 0.0360(10) Uani 1 1 d . . . H35A H 0.1011 0.0736 0.5577 0.054 Uiso 1 1 calc R . . H35B H 0.2470 0.0462 0.5381 0.054 Uiso 1 1 calc R . . H35C H 0.1397 0.0404 0.4763 0.054 Uiso 1 1 calc R . . C36 C 0.2396(5) 0.2786(4) 0.5974(2) 0.0385(10) Uani 1 1 d . . . H36A H 0.1758 0.2688 0.6323 0.058 Uiso 1 1 calc R . . H36B H 0.2539 0.3649 0.5978 0.058 Uiso 1 1 calc R . . H36C H 0.3203 0.2423 0.6094 0.058 Uiso 1 1 calc R . . C37 C 0.2919(4) 0.2343(5) 0.4702(3) 0.0433(12) Uani 1 1 d . . . H37A H 0.2621 0.1955 0.4224 0.065 Uiso 1 1 calc R . . H37B H 0.3726 0.1981 0.4822 0.065 Uiso 1 1 calc R . . H37C H 0.3055 0.3211 0.4720 0.065 Uiso 1 1 calc R . . N41 N -0.2755(3) 0.2182(3) 0.35751(17) 0.0232(6) Uani 1 1 d . . . C41 C -0.2705(3) 0.1590(3) 0.2900(2) 0.0224(7) Uani 1 1 d . . . C42 C -0.3521(4) 0.1517(4) 0.3935(2) 0.0305(9) Uani 1 1 d . . . H42A H -0.3720 0.1729 0.4422 0.037 Uiso 1 1 calc R . . N42 N -0.3426(3) 0.0554(3) 0.28344(18) 0.0269(7) Uani 1 1 d . . . C43 C -0.3940(4) 0.0521(4) 0.3482(2) 0.0330(9) Uani 1 1 d . . . H43A H -0.4489 -0.0094 0.3589 0.040 Uiso 1 1 calc R . . C44 C -0.3628(4) -0.0410(4) 0.2179(2) 0.0343(9) Uani 1 1 d . . . C45 C -0.4309(4) 0.0119(4) 0.1598(2) 0.0361(10) Uani 1 1 d . . . H45A H -0.5125 0.0462 0.1771 0.054 Uiso 1 1 calc R . . H45B H -0.4472 -0.0521 0.1181 0.054 Uiso 1 1 calc R . . H45C H -0.3770 0.0756 0.1469 0.054 Uiso 1 1 calc R . . C46 C -0.4491(6) -0.1401(4) 0.2364(3) 0.0502(13) Uani 1 1 d . . . H46A H -0.4069 -0.1757 0.2736 0.075 Uiso 1 1 calc R . . H46B H -0.4652 -0.2030 0.1941 0.075 Uiso 1 1 calc R . . H46C H -0.5306 -0.1052 0.2534 0.075 Uiso 1 1 calc R . . C47 C -0.2332(5) -0.0942(4) 0.1949(3) 0.0484(13) Uani 1 1 d . . . H47A H -0.1927 -0.1266 0.2339 0.073 Uiso 1 1 calc R . . H47B H -0.1780 -0.0306 0.1828 0.073 Uiso 1 1 calc R . . H47C H -0.2458 -0.1593 0.1534 0.073 Uiso 1 1 calc R . . C51 C -0.3162(5) 0.1628(4) 0.6080(3) 0.0392(11) Uani 1 1 d . . . N51 N -0.4179(5) 0.1556(5) 0.5863(3) 0.0697(15) Uani 1 1 d . . . C52 C -0.1842(6) 0.1718(5) 0.6347(3) 0.0518(13) Uani 1 1 d . . . H52A H -0.1275 0.1809 0.5963 0.078 Uiso 1 1 calc R . . H52B H -0.1624 0.0983 0.6525 0.078 Uiso 1 1 calc R . . H52C H -0.1738 0.2423 0.6733 0.078 Uiso 1 1 calc R . . C61 C -0.4218(7) 0.6630(7) 0.0188(4) 0.0689(17) Uani 1 1 d U . . N61 N -0.4516(7) 0.6395(7) 0.0689(4) 0.093(2) Uani 1 1 d U . . C62 C -0.3934(14) 0.6950(13) -0.0460(7) 0.159(5) Uani 1 1 d U . . H62A H -0.3996 0.6230 -0.0838 0.238 Uiso 1 1 calc R . . H62B H -0.3063 0.7292 -0.0431 0.238 Uiso 1 1 calc R . . H62C H -0.4544 0.7553 -0.0563 0.238 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 0.01956(13) 0.02025(13) 0.02144(13) 0.00253(9) -0.00014(9) -0.00308(9) I 0.03905(17) 0.02874(15) 0.03514(16) 0.00057(11) 0.00562(12) 0.00889(11) S1 0.0272(5) 0.0227(4) 0.0238(4) 0.0030(3) -0.0025(4) -0.0048(4) S2 0.0308(5) 0.0301(5) 0.0239(4) 0.0053(4) 0.0022(4) 0.0026(4) S3 0.0292(5) 0.0203(4) 0.0220(4) 0.0042(3) 0.0010(4) 0.0031(4) S4 0.0215(5) 0.0313(5) 0.0243(4) 0.0072(4) -0.0022(3) -0.0050(4) B1 0.028(2) 0.030(2) 0.025(2) 0.0029(17) -0.0040(17) 0.0034(18) B2 0.025(2) 0.023(2) 0.028(2) 0.0061(16) -0.0040(17) 0.0002(17) N11 0.0247(17) 0.0224(15) 0.0291(16) 0.0059(12) -0.0031(13) -0.0040(13) C11 0.0214(18) 0.0209(17) 0.0279(19) 0.0034(14) -0.0025(15) -0.0024(14) N12 0.0225(17) 0.0225(16) 0.0385(19) 0.0071(13) -0.0021(14) -0.0057(13) C12 0.037(2) 0.027(2) 0.038(2) 0.0137(17) -0.0028(18) -0.0056(17) C13 0.032(2) 0.031(2) 0.047(3) 0.0128(19) 0.0041(19) -0.0119(18) C14 0.0169(18) 0.030(2) 0.050(3) 0.0068(18) -0.0029(17) -0.0012(15) C15 0.028(2) 0.030(2) 0.067(3) 0.004(2) 0.000(2) 0.0015(18) C16 0.025(2) 0.042(3) 0.055(3) 0.010(2) -0.013(2) -0.0051(19) C17 0.022(2) 0.042(3) 0.080(4) 0.014(3) 0.004(2) -0.0061(19) C21 0.027(2) 0.030(2) 0.0245(18) 0.0077(15) 0.0013(15) -0.0043(16) N21 0.0229(16) 0.0275(17) 0.0285(17) 0.0078(13) -0.0002(13) -0.0031(13) C22 0.023(2) 0.040(2) 0.035(2) 0.0118(18) -0.0011(17) 0.0024(17) N22 0.0255(17) 0.0381(19) 0.0258(17) 0.0052(14) -0.0020(13) -0.0066(15) C23 0.027(2) 0.057(3) 0.031(2) 0.011(2) -0.0031(17) -0.005(2) C24 0.036(2) 0.046(3) 0.0226(19) 0.0002(17) -0.0004(17) -0.0096(19) C25 0.036(3) 0.077(4) 0.035(3) -0.007(2) -0.004(2) -0.005(3) C26 0.040(3) 0.067(3) 0.025(2) 0.002(2) 0.0044(19) -0.004(2) C27 0.071(4) 0.045(3) 0.035(3) -0.005(2) 0.001(2) -0.016(3) N31 0.0212(16) 0.0230(15) 0.0232(15) 0.0016(12) 0.0027(12) 0.0015(12) C31 0.0224(18) 0.0200(17) 0.0240(17) 0.0067(13) 0.0004(14) -0.0039(14) N32 0.0193(15) 0.0220(15) 0.0242(15) 0.0041(12) -0.0026(12) -0.0017(12) C32 0.028(2) 0.0262(19) 0.0239(18) -0.0014(14) 0.0000(15) 0.0049(15) C33 0.031(2) 0.0228(18) 0.0231(18) -0.0002(14) -0.0029(15) -0.0008(15) C34 0.0237(19) 0.033(2) 0.0241(18) 0.0096(15) -0.0031(15) 0.0019(16) C35 0.045(3) 0.028(2) 0.036(2) 0.0093(17) -0.0069(19) 0.0049(19) C36 0.033(2) 0.042(2) 0.040(2) 0.0078(19) -0.0155(19) -0.0001(19) C37 0.019(2) 0.071(3) 0.047(3) 0.030(2) 0.0033(19) 0.006(2) N41 0.0175(15) 0.0260(16) 0.0272(16) 0.0079(13) 0.0000(12) -0.0010(12) C41 0.0170(17) 0.0222(17) 0.0289(18) 0.0076(14) -0.0026(14) -0.0017(14) C42 0.023(2) 0.040(2) 0.031(2) 0.0142(17) 0.0007(16) 0.0002(17) N42 0.0229(16) 0.0246(16) 0.0333(18) 0.0065(13) -0.0040(13) -0.0067(13) C43 0.027(2) 0.037(2) 0.038(2) 0.0159(18) -0.0015(17) -0.0078(17) C44 0.033(2) 0.0231(19) 0.045(2) 0.0007(17) -0.0044(19) -0.0083(17) C45 0.033(2) 0.035(2) 0.038(2) 0.0000(18) -0.0059(18) -0.0120(18) C46 0.061(3) 0.029(2) 0.060(3) 0.010(2) -0.009(3) -0.018(2) C47 0.043(3) 0.030(2) 0.066(3) -0.007(2) -0.005(2) 0.010(2) C51 0.046(3) 0.030(2) 0.044(3) 0.0136(19) 0.014(2) 0.003(2) N51 0.049(3) 0.068(4) 0.101(4) 0.036(3) 0.012(3) 0.004(3) C52 0.060(4) 0.032(3) 0.062(3) 0.005(2) 0.002(3) 0.003(2) C61 0.0673(19) 0.0697(19) 0.0693(19) 0.0123(10) 0.0028(10) 0.0031(10) N61 0.092(2) 0.093(2) 0.093(2) 0.0170(10) 0.0015(10) 0.0035(10) C62 0.158(5) 0.159(5) 0.159(5) 0.0307(14) 0.0056(10) 0.0027(10) _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 S4 2.4915(10) . ? In S1 2.4911(9) . ? In S3 2.5909(10) . ? In S2 2.6214(10) . ? In I 2.7977(4) . ? S1 C11 1.720(4) . ? S2 C21 1.717(4) . ? S3 C31 1.730(4) . ? S4 C41 1.726(4) . ? B1 H2 1.107(19) . ? B1 H1 1.112(19) . ? B1 N11 1.555(6) . ? B1 N21 1.572(5) . ? B2 H4 1.092(19) . ? B2 H3 1.098(19) . ? B2 N31 1.551(5) . ? B2 N41 1.556(5) . ? N11 C11 1.343(5) . ? N11 C12 1.374(5) . ? C11 N12 1.373(5) . ? N12 C13 1.381(5) . ? N12 C14 1.503(5) . ? C12 C13 1.351(6) . ? C14 C16 1.515(7) . ? C14 C17 1.523(6) . ? C14 C15 1.537(6) . ? C21 N21 1.357(5) . ? C21 N22 1.371(5) . ? N21 C22 1.370(5) . ? C22 C23 1.357(6) . ? N22 C23 1.367(6) . ? N22 C24 1.514(5) . ? C24 C26 1.516(6) . ? C24 C27 1.518(7) . ? C24 C25 1.528(7) . ? N31 C31 1.346(5) . ? N31 C32 1.377(5) . ? C31 N32 1.370(5) . ? N32 C33 1.384(5) . ? N32 C34 1.498(5) . ? C32 C33 1.349(6) . ? C34 C35 1.523(6) . ? C34 C36 1.527(6) . ? C34 C37 1.529(6) . ? N41 C41 1.343(5) . ? N41 C42 1.376(5) . ? C41 N42 1.365(5) . ? C42 C43 1.342(6) . ? N42 C43 1.376(5) . ? N42 C44 1.505(5) . ? C44 C45 1.522(6) . ? C44 C46 1.528(6) . ? C44 C47 1.530(7) . ? C51 N51 1.126(7) . ? C51 C52 1.452(8) . ? C61 N61 1.098(9) . ? C61 C62 1.397(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 In S1 128.44(3) . . ? S4 In S3 98.89(3) . . ? S1 In S3 87.22(3) . . ? S4 In S2 88.23(3) . . ? S1 In S2 93.99(3) . . ? S3 In S2 169.90(3) . . ? S4 In I 114.44(3) . . ? S1 In I 117.10(3) . . ? S3 In I 84.96(2) . . ? S2 In I 85.56(2) . . ? C11 S1 In 104.95(13) . . ? C21 S2 In 105.07(13) . . ? C31 S3 In 109.02(12) . . ? C41 S4 In 104.20(13) . . ? H2 B1 H1 112(3) . . ? H2 B1 N11 112(2) . . ? H1 B1 N11 109(2) . . ? H2 B1 N21 109(2) . . ? H1 B1 N21 104(2) . . ? N11 B1 N21 109.8(3) . . ? H4 B2 H3 112(3) . . ? H4 B2 N31 105(2) . . ? H3 B2 N31 112(2) . . ? H4 B2 N41 113(2) . . ? H3 B2 N41 104(2) . . ? N31 B2 N41 110.5(3) . . ? C11 N11 C12 108.3(3) . . ? C11 N11 B1 128.7(3) . . ? C12 N11 B1 122.9(3) . . ? N11 C11 N12 108.2(3) . . ? N11 C11 S1 125.9(3) . . ? N12 C11 S1 125.9(3) . . ? C11 N12 C13 107.5(3) . . ? C11 N12 C14 126.8(3) . . ? C13 N12 C14 125.7(3) . . ? C13 C12 N11 108.3(4) . . ? C12 C13 N12 107.6(4) . . ? N12 C14 C16 109.1(3) . . ? N12 C14 C17 109.0(4) . . ? C16 C14 C17 108.5(4) . . ? N12 C14 C15 109.3(3) . . ? C16 C14 C15 112.5(4) . . ? C17 C14 C15 108.5(4) . . ? N21 C21 N22 107.6(4) . . ? N21 C21 S2 126.0(3) . . ? N22 C21 S2 126.4(3) . . ? C21 N21 C22 107.8(3) . . ? C21 N21 B1 130.4(3) . . ? C22 N21 B1 121.3(3) . . ? C23 C22 N21 108.8(4) . . ? C23 N22 C21 108.6(4) . . ? C23 N22 C24 124.1(4) . . ? C21 N22 C24 127.1(4) . . ? C22 C23 N22 107.1(4) . . ? N22 C24 C26 108.5(4) . . ? N22 C24 C27 110.8(3) . . ? C26 C24 C27 112.5(5) . . ? N22 C24 C25 108.0(4) . . ? C26 C24 C25 109.3(4) . . ? C27 C24 C25 107.6(4) . . ? C31 N31 C32 107.6(3) . . ? C31 N31 B2 130.0(3) . . ? C32 N31 B2 121.6(3) . . ? N31 C31 N32 108.7(3) . . ? N31 C31 S3 124.7(3) . . ? N32 C31 S3 126.5(3) . . ? C31 N32 C33 107.6(3) . . ? C31 N32 C34 128.3(3) . . ? C33 N32 C34 124.1(3) . . ? C33 C32 N31 109.0(3) . . ? C32 C33 N32 107.2(3) . . ? N32 C34 C35 109.3(3) . . ? N32 C34 C36 109.2(3) . . ? C35 C34 C36 108.9(3) . . ? N32 C34 C37 109.4(3) . . ? C35 C34 C37 111.8(4) . . ? C36 C34 C37 108.2(4) . . ? C41 N41 C42 108.1(3) . . ? C41 N41 B2 128.7(3) . . ? C42 N41 B2 123.2(3) . . ? N41 C41 N42 107.9(3) . . ? N41 C41 S4 126.0(3) . . ? N42 C41 S4 126.0(3) . . ? C43 C42 N41 108.6(4) . . ? C41 N42 C43 108.2(3) . . ? C41 N42 C44 127.0(3) . . ? C43 N42 C44 124.8(3) . . ? C42 C43 N42 107.3(4) . . ? N42 C44 C45 109.9(3) . . ? N42 C44 C46 108.1(4) . . ? C45 C44 C46 108.0(4) . . ? N42 C44 C47 108.9(3) . . ? C45 C44 C47 112.3(4) . . ? C46 C44 C47 109.5(4) . . ? N51 C51 C52 178.8(6) . . ? N61 C61 C62 175.7(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.481 _refine_diff_density_min -1.073 _refine_diff_density_rms 0.132 # Attachment '- BmButAlCl2 (ky292s10).cif' data_ky292s10 _database_code_depnum_ccdc_archive 'CCDC 776953' #TrackingRef '- BmButAlCl2 (ky292s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 Al B Cl2 N4 S2' _chemical_formula_weight 421.18 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.4813(6) _cell_length_b 12.4010(6) _cell_length_c 28.5197(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4060.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9771 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 32.53 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.573 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8246 _exptl_absorpt_correction_T_max 0.9189 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 66807 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 32.74 _reflns_number_total 7281 _reflns_number_gt 6423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to 1.1 angstroms. ; _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^)+(0.0350P)^2^+1.7132P] 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 7281 _refine_ls_number_parameters 223 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Al Al 0.95876(3) -0.02177(2) 0.626943(11) 0.01566(6) Uani 1 1 d . . . Cl1 Cl 0.85148(2) 0.11643(2) 0.617382(9) 0.02455(6) Uani 1 1 d . . . Cl2 Cl 0.86997(2) -0.15851(2) 0.654769(9) 0.02056(5) Uani 1 1 d . . . S1 S 1.09544(2) 0.031256(19) 0.679067(9) 0.01688(5) Uani 1 1 d . . . S2 S 1.03844(2) -0.06662(2) 0.557132(8) 0.01852(5) Uani 1 1 d . . . B B 1.22631(9) -0.18499(9) 0.63124(4) 0.01674(18) Uani 1 1 d D . . H1 H 1.2990(11) -0.2401(11) 0.6330(5) 0.020 Uiso 1 1 d D . . H2 H 1.2436(13) -0.1061(10) 0.6161(4) 0.020 Uiso 1 1 d D . . N11 N 1.17931(7) -0.17573(6) 0.68296(3) 0.01445(14) Uani 1 1 d . . . C11 C 1.12603(8) -0.09287(7) 0.70482(3) 0.01390(15) Uani 1 1 d . . . N12 N 1.10459(7) -0.12080(6) 0.75017(3) 0.01487(14) Uani 1 1 d . . . C12 C 1.19171(9) -0.25760(8) 0.71526(3) 0.01758(17) Uani 1 1 d . . . H12A H 1.2265 -0.3258 0.7094 0.021 Uiso 1 1 calc R . . C13 C 1.14615(9) -0.22484(8) 0.75668(3) 0.01783(17) Uani 1 1 d . . . H13A H 1.1432 -0.2654 0.7849 0.021 Uiso 1 1 calc R . . C14 C 1.04312(8) -0.05546(8) 0.78742(3) 0.01701(17) Uani 1 1 d . . . C15 C 1.11029(10) 0.04906(9) 0.79619(4) 0.0244(2) Uani 1 1 d . . . H15A H 1.1164 0.0898 0.7668 0.037 Uiso 1 1 calc R . . H15B H 1.1885 0.0319 0.8077 0.037 Uiso 1 1 calc R . . H15C H 1.0690 0.0925 0.8196 0.037 Uiso 1 1 calc R . . C16 C 0.91790(9) -0.03469(9) 0.77143(4) 0.02169(19) Uani 1 1 d . . . H16A H 0.8796 -0.1036 0.7646 0.033 Uiso 1 1 calc R . . H16B H 0.9186 0.0100 0.7431 0.033 Uiso 1 1 calc R . . H16C H 0.8753 0.0028 0.7963 0.033 Uiso 1 1 calc R . . C17 C 1.04007(10) -0.12134(10) 0.83270(4) 0.0248(2) Uani 1 1 d . . . H17A H 0.9879 -0.1832 0.8287 0.037 Uiso 1 1 calc R . . H17B H 1.0117 -0.0760 0.8584 0.037 Uiso 1 1 calc R . . H17C H 1.1187 -0.1471 0.8400 0.037 Uiso 1 1 calc R . . N21 N 1.13227(7) -0.24432(7) 0.60023(3) 0.01593(14) Uani 1 1 d . . . C21 C 1.05337(8) -0.20335(8) 0.57005(3) 0.01578(16) Uani 1 1 d . . . N22 N 0.98875(8) -0.28537(7) 0.55179(3) 0.01833(16) Uani 1 1 d . . . C22 C 1.11720(10) -0.35464(8) 0.60120(4) 0.02113(19) Uani 1 1 d . . . H22A H 1.1612 -0.4042 0.6194 0.025 Uiso 1 1 calc R . . C23 C 1.02882(10) -0.38024(9) 0.57171(4) 0.0228(2) Uani 1 1 d . . . H23A H 0.9996 -0.4506 0.5658 0.027 Uiso 1 1 calc R . . C24 C 0.89867(9) -0.27966(10) 0.51305(4) 0.0231(2) Uani 1 1 d . . . C25 C 0.80010(10) -0.20222(11) 0.52595(4) 0.0278(2) Uani 1 1 d . . . H25A H 0.8324 -0.1304 0.5321 0.042 Uiso 1 1 calc R . . H25B H 0.7603 -0.2285 0.5541 0.042 Uiso 1 1 calc R . . H25C H 0.7445 -0.1980 0.5000 0.042 Uiso 1 1 calc R . . C26 C 0.84630(11) -0.39179(11) 0.50631(5) 0.0333(3) Uani 1 1 d . . . H26A H 0.7885 -0.3895 0.4810 0.050 Uiso 1 1 calc R . . H26B H 0.8086 -0.4149 0.5355 0.050 Uiso 1 1 calc R . . H26C H 0.9081 -0.4429 0.4981 0.050 Uiso 1 1 calc R . . C27 C 0.96111(11) -0.24416(14) 0.46825(4) 0.0339(3) Uani 1 1 d . . . H27A H 0.9943 -0.1721 0.4728 0.051 Uiso 1 1 calc R . . H27B H 0.9054 -0.2423 0.4422 0.051 Uiso 1 1 calc R . . H27C H 1.0236 -0.2953 0.4610 0.051 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 Al 0.01518(13) 0.01569(13) 0.01610(13) 0.00182(10) -0.00043(10) 0.00083(10) Cl1 0.02632(12) 0.02322(12) 0.02412(12) 0.00369(9) -0.00060(9) 0.00990(9) Cl2 0.01997(11) 0.02027(11) 0.02143(11) 0.00138(8) 0.00221(8) -0.00478(8) S1 0.01903(11) 0.01316(10) 0.01846(11) 0.00096(8) -0.00250(8) -0.00170(8) S2 0.02039(11) 0.02018(11) 0.01499(10) 0.00342(8) 0.00041(8) 0.00152(8) B 0.0141(4) 0.0213(5) 0.0148(4) -0.0012(4) 0.0005(3) 0.0002(4) N11 0.0133(3) 0.0153(3) 0.0147(3) -0.0006(3) -0.0010(3) 0.0007(3) C11 0.0125(4) 0.0146(4) 0.0146(4) 0.0003(3) -0.0011(3) -0.0009(3) N12 0.0141(3) 0.0160(3) 0.0145(3) -0.0001(3) 0.0005(3) 0.0009(3) C12 0.0198(4) 0.0160(4) 0.0169(4) 0.0006(3) -0.0006(3) 0.0033(3) C13 0.0209(4) 0.0162(4) 0.0164(4) 0.0019(3) 0.0008(3) 0.0026(3) C14 0.0156(4) 0.0194(4) 0.0160(4) -0.0028(3) 0.0021(3) 0.0014(3) C15 0.0259(5) 0.0242(5) 0.0230(5) -0.0080(4) 0.0017(4) -0.0054(4) C16 0.0153(4) 0.0255(5) 0.0243(5) -0.0029(4) 0.0022(3) 0.0031(4) C17 0.0261(5) 0.0308(5) 0.0176(4) 0.0020(4) 0.0060(4) 0.0046(4) N21 0.0176(4) 0.0169(3) 0.0132(3) -0.0007(3) -0.0001(3) 0.0010(3) C21 0.0154(4) 0.0195(4) 0.0124(4) -0.0007(3) 0.0010(3) 0.0002(3) N22 0.0185(4) 0.0226(4) 0.0139(3) -0.0025(3) -0.0004(3) -0.0017(3) C22 0.0293(5) 0.0175(4) 0.0166(4) -0.0006(3) -0.0012(4) 0.0015(4) C23 0.0303(5) 0.0193(4) 0.0187(4) -0.0026(3) -0.0007(4) -0.0032(4) C24 0.0169(4) 0.0366(6) 0.0157(4) -0.0044(4) -0.0023(3) -0.0026(4) C25 0.0179(5) 0.0385(6) 0.0271(5) -0.0018(5) -0.0034(4) 0.0006(4) C26 0.0262(5) 0.0397(7) 0.0340(6) -0.0156(5) -0.0043(5) -0.0054(5) C27 0.0246(5) 0.0633(9) 0.0139(4) -0.0006(5) -0.0017(4) -0.0042(5) _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 Al Cl1 2.1280(4) . ? Al Cl2 2.1317(4) . ? Al S1 2.2594(4) . ? Al S2 2.2606(4) . ? S1 C11 1.7413(10) . ? S2 C21 1.7435(10) . ? B H1 1.080(12) . ? B H2 1.088(11) . ? B N11 1.5750(13) . ? B N21 1.5778(14) . ? N11 C11 1.3485(12) . ? N11 C12 1.3782(12) . ? C11 N12 1.3616(12) . ? N12 C13 1.3880(12) . ? N12 C14 1.5109(12) . ? C12 C13 1.3543(13) . ? C14 C17 1.5284(15) . ? C14 C15 1.5289(15) . ? C14 C16 1.5301(14) . ? N21 C21 1.3489(12) . ? N21 C22 1.3792(13) . ? C21 N22 1.3625(13) . ? N22 C23 1.3850(14) . ? N22 C24 1.5151(13) . ? C22 C23 1.3557(15) . ? C24 C26 1.5271(17) . ? C24 C25 1.5293(16) . ? C24 C27 1.5298(16) . ? 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 Cl1 Al Cl2 114.305(17) . . ? Cl1 Al S1 104.591(16) . . ? Cl2 Al S1 108.584(16) . . ? Cl1 Al S2 108.635(16) . . ? Cl2 Al S2 109.005(16) . . ? S1 Al S2 111.714(16) . . ? C11 S1 Al 99.23(3) . . ? C21 S2 Al 95.34(3) . . ? H1 B H2 116.5(11) . . ? H1 B N11 105.5(7) . . ? H2 B N11 111.6(7) . . ? H1 B N21 105.1(8) . . ? H2 B N21 108.8(7) . . ? N11 B N21 108.94(8) . . ? C11 N11 C12 107.41(8) . . ? C11 N11 B 130.08(8) . . ? C12 N11 B 122.47(8) . . ? N11 C11 N12 109.10(8) . . ? N11 C11 S1 124.76(7) . . ? N12 C11 S1 126.09(7) . . ? C11 N12 C13 107.54(8) . . ? C11 N12 C14 128.02(8) . . ? C13 N12 C14 124.40(8) . . ? C13 C12 N11 108.79(8) . . ? C12 C13 N12 107.15(8) . . ? N12 C14 C17 108.54(8) . . ? N12 C14 C15 109.52(8) . . ? C17 C14 C15 109.06(9) . . ? N12 C14 C16 108.65(8) . . ? C17 C14 C16 108.67(8) . . ? C15 C14 C16 112.33(9) . . ? C21 N21 C22 107.59(8) . . ? C21 N21 B 129.91(8) . . ? C22 N21 B 122.49(8) . . ? N21 C21 N22 109.17(9) . . ? N21 C21 S2 124.55(7) . . ? N22 C21 S2 126.28(7) . . ? C21 N22 C23 107.25(8) . . ? C21 N22 C24 127.99(9) . . ? C23 N22 C24 124.44(9) . . ? C23 C22 N21 108.28(9) . . ? C22 C23 N22 107.71(9) . . ? N22 C24 C26 108.54(10) . . ? N22 C24 C25 111.04(9) . . ? C26 C24 C25 108.10(9) . . ? N22 C24 C27 107.62(9) . . ? C26 C24 C27 109.96(10) . . ? C25 C24 C27 111.54(11) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 32.74 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.533 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.058 # Attachment '- BmButGa(I)Ga(I)BmBut (14s10).cif' data_14s10 _database_code_depnum_ccdc_archive 'CCDC 776954' #TrackingRef '- BmButGa(I)Ga(I)BmBut (14s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H48 B2 Ga2 I2 N8 S4' _chemical_formula_weight 1039.84 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.873(9) _cell_length_b 18.840(17) _cell_length_c 12.499(12) _cell_angle_alpha 90.00 _cell_angle_beta 110.952(14) _cell_angle_gamma 90.00 _cell_volume 2171(3) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 2651 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.39 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 2.884 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8460 _exptl_absorpt_correction_T_max 0.9446 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14470 _diffrn_reflns_av_R_equivalents 0.1535 _diffrn_reflns_av_sigmaI/netI 0.1414 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3828 _reflns_number_gt 2297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to be 1.1 angstroms. The ADPs of several carbon atoms have been restrained. ; _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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3828 _refine_ls_number_parameters 214 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.034 _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 Ga Ga -0.99617(11) -0.46554(5) 1.41932(9) 0.0222(3) Uani 1 1 d . . . I I -1.17051(7) -0.51062(4) 1.22155(6) 0.0323(2) Uani 1 1 d . . . S1 S -1.0697(3) -0.34998(13) 1.4359(2) 0.0283(6) Uani 1 1 d . . . S2 S -0.7617(2) -0.46333(13) 1.4181(2) 0.0276(6) Uani 1 1 d . . . B B -0.8809(12) -0.3127(6) 1.2688(12) 0.035(3) Uani 1 1 d D . . H1 H -0.835(9) -0.271(3) 1.230(7) 0.042 Uiso 1 1 d D . . H2 H -0.821(9) -0.305(5) 1.361(3) 0.042 Uiso 1 1 d D . . C11 C -1.1322(10) -0.3182(5) 1.3026(8) 0.026(2) Uani 1 1 d U . . N11 N -1.0494(8) -0.3036(4) 1.2361(7) 0.027(2) Uani 1 1 d . . . C12 C -1.1398(10) -0.2745(5) 1.1320(9) 0.028(2) Uani 1 1 d . . . H12A H -1.1104 -0.2599 1.0708 0.034 Uiso 1 1 calc R . . N12 N -1.2736(8) -0.2978(4) 1.2375(7) 0.0242(19) Uani 1 1 d . . . C13 C -1.2759(11) -0.2708(5) 1.1331(9) 0.032(3) Uani 1 1 d . . . H13A H -1.3586 -0.2529 1.0733 0.039 Uiso 1 1 calc R . . C14 C -1.4026(10) -0.2990(5) 1.2752(8) 0.027(2) Uani 1 1 d . . . C15 C -1.3743(12) -0.2511(5) 1.3796(10) 0.041(3) Uani 1 1 d . . . H15A H -1.4577 -0.2530 1.4046 0.062 Uiso 1 1 calc R . . H15B H -1.3598 -0.2022 1.3593 0.062 Uiso 1 1 calc R . . H15C H -1.2873 -0.2675 1.4418 0.062 Uiso 1 1 calc R . . C16 C -1.5355(11) -0.2739(6) 1.1758(10) 0.042(3) Uani 1 1 d . . . H16A H -1.6207 -0.2753 1.1986 0.063 Uiso 1 1 calc R . . H16B H -1.5514 -0.3050 1.1096 0.063 Uiso 1 1 calc R . . H16C H -1.5199 -0.2252 1.1554 0.063 Uiso 1 1 calc R . . C17 C -1.4320(11) -0.3750(5) 1.3039(10) 0.039(3) Uani 1 1 d . . . H17A H -1.5156 -0.3754 1.3287 0.059 Uiso 1 1 calc R . . H17B H -1.3466 -0.3934 1.3656 0.059 Uiso 1 1 calc R . . H17C H -1.4527 -0.4050 1.2358 0.059 Uiso 1 1 calc R . . N21 N -0.8484(8) -0.3860(4) 1.2189(7) 0.0219(18) Uani 1 1 d . . . C21 C -0.7934(9) -0.4467(5) 1.2751(8) 0.020(2) Uani 1 1 d U . . N22 N -0.7664(8) -0.4927(4) 1.1988(7) 0.0235(18) Uani 1 1 d . . . C22 C -0.8578(10) -0.3934(5) 1.1086(9) 0.027(2) Uani 1 1 d . . . H22A H -0.8932 -0.3585 1.0503 0.033 Uiso 1 1 calc R . . C23 C -0.8091(10) -0.4581(5) 1.0951(9) 0.031(2) Uani 1 1 d . . . H23A H -0.8049 -0.4768 1.0257 0.037 Uiso 1 1 calc R . . C24 C -0.7019(11) -0.5669(5) 1.2223(9) 0.033(3) Uani 1 1 d . . . C25 C -0.8092(11) -0.6148(5) 1.2528(12) 0.054(4) Uani 1 1 d . . . H25A H -0.8142 -0.5998 1.3263 0.081 Uiso 1 1 calc R . . H25B H -0.7762 -0.6642 1.2584 0.081 Uiso 1 1 calc R . . H25C H -0.9056 -0.6109 1.1930 0.081 Uiso 1 1 calc R . . C26 C -0.6888(13) -0.5949(6) 1.1126(10) 0.050(3) Uani 1 1 d U . . H26A H -0.6399 -0.6410 1.1274 0.075 Uiso 1 1 calc R . . H26B H -0.6323 -0.5614 1.0854 0.075 Uiso 1 1 calc R . . H26C H -0.7857 -0.6002 1.0542 0.075 Uiso 1 1 calc R . . C27 C -0.5532(11) -0.5647(5) 1.3149(9) 0.037(3) Uani 1 1 d . . . H27A H -0.5628 -0.5540 1.3887 0.056 Uiso 1 1 calc R . . H27B H -0.4949 -0.5277 1.2969 0.056 Uiso 1 1 calc R . . H27C H -0.5056 -0.6108 1.3194 0.056 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 Ga 0.0218(6) 0.0270(6) 0.0177(6) 0.0045(5) 0.0069(5) 0.0044(4) I 0.0270(4) 0.0440(4) 0.0246(4) -0.0071(3) 0.0076(3) -0.0008(3) S1 0.0210(13) 0.0315(15) 0.0279(16) -0.0068(12) 0.0032(12) 0.0036(10) S2 0.0192(13) 0.0390(15) 0.0241(15) 0.0030(12) 0.0070(11) 0.0052(10) B 0.022(6) 0.021(7) 0.060(10) -0.003(6) 0.013(6) -0.008(5) C11 0.026(2) 0.026(2) 0.026(2) -0.0010(10) 0.0095(12) 0.0003(10) N11 0.020(5) 0.025(5) 0.038(6) -0.001(4) 0.012(4) 0.000(3) C12 0.025(6) 0.028(6) 0.033(7) 0.009(5) 0.012(5) 0.003(4) N12 0.025(5) 0.016(4) 0.032(5) 0.001(4) 0.012(4) 0.004(3) C13 0.038(6) 0.030(6) 0.028(7) 0.015(5) 0.011(5) 0.005(4) C14 0.028(6) 0.029(6) 0.024(6) -0.002(5) 0.009(5) -0.003(4) C15 0.050(7) 0.028(6) 0.055(8) -0.005(6) 0.032(7) 0.003(5) C16 0.032(6) 0.045(7) 0.052(8) 0.006(6) 0.019(6) 0.006(5) C17 0.021(6) 0.039(7) 0.058(8) 0.010(6) 0.014(6) 0.004(4) N21 0.020(4) 0.025(5) 0.022(5) 0.006(4) 0.010(4) 0.001(3) C21 0.010(5) 0.028(6) 0.023(6) -0.002(5) 0.008(4) -0.007(4) N22 0.025(4) 0.014(4) 0.029(5) 0.003(4) 0.006(4) -0.001(3) C22 0.025(5) 0.028(6) 0.033(7) 0.011(5) 0.015(5) 0.007(4) C23 0.030(6) 0.033(6) 0.032(7) 0.001(5) 0.016(5) 0.005(4) C24 0.036(6) 0.027(6) 0.042(7) -0.003(5) 0.022(6) -0.003(4) C25 0.031(7) 0.021(6) 0.107(12) 0.016(7) 0.022(7) 0.006(5) C26 0.050(3) 0.049(3) 0.050(3) -0.0007(10) 0.0178(15) 0.0009(10) C27 0.033(6) 0.026(6) 0.052(8) 0.003(5) 0.015(6) 0.003(5) _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 Ga S2 2.321(3) . ? Ga S1 2.327(3) . ? Ga Ga 2.423(3) 3_348 ? Ga I 2.598(2) . ? S1 C11 1.667(10) . ? S2 C21 1.729(9) . ? B H1 1.10(2) . ? B H2 1.11(2) . ? B N11 1.574(13) . ? B N21 1.595(14) . ? C11 N11 1.386(11) . ? C11 N12 1.395(12) . ? N11 C12 1.400(12) . ? C12 C13 1.351(12) . ? N12 C13 1.393(12) . ? N12 C14 1.508(11) . ? C14 C16 1.524(14) . ? C14 C15 1.528(13) . ? C14 C17 1.529(13) . ? N21 C21 1.351(11) . ? N21 C22 1.355(12) . ? C21 N22 1.383(11) . ? N22 C23 1.376(12) . ? N22 C24 1.521(12) . ? C22 C23 1.343(13) . ? C24 C27 1.510(13) . ? C24 C26 1.516(14) . ? C24 C25 1.540(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ga S1 109.11(10) . . ? S2 Ga Ga 110.09(9) . 3_348 ? S1 Ga Ga 108.89(10) . 3_348 ? S2 Ga I 108.81(9) . . ? S1 Ga I 105.60(8) . . ? Ga Ga I 114.17(9) 3_348 . ? C11 S1 Ga 105.3(3) . . ? C21 S2 Ga 101.4(3) . . ? H1 B H2 102(7) . . ? H1 B N11 112(5) . . ? H2 B N11 112(5) . . ? H1 B N21 106(5) . . ? H2 B N21 114(5) . . ? N11 B N21 109.5(8) . . ? N11 C11 N12 106.1(8) . . ? N11 C11 S1 125.7(7) . . ? N12 C11 S1 128.1(7) . . ? C11 N11 C12 108.6(7) . . ? C11 N11 B 128.2(9) . . ? C12 N11 B 123.1(8) . . ? C13 C12 N11 108.5(9) . . ? C13 N12 C11 109.0(8) . . ? C13 N12 C14 124.4(8) . . ? C11 N12 C14 126.5(8) . . ? C12 C13 N12 107.9(9) . . ? N12 C14 C16 108.5(8) . . ? N12 C14 C15 109.9(8) . . ? C16 C14 C15 110.7(8) . . ? N12 C14 C17 109.9(7) . . ? C16 C14 C17 107.6(8) . . ? C15 C14 C17 110.1(8) . . ? C21 N21 C22 108.1(8) . . ? C21 N21 B 129.1(9) . . ? C22 N21 B 122.5(8) . . ? N21 C21 N22 108.3(8) . . ? N21 C21 S2 125.5(7) . . ? N22 C21 S2 126.2(7) . . ? C23 N22 C21 106.4(7) . . ? C23 N22 C24 125.7(8) . . ? C21 N22 C24 127.9(8) . . ? C23 C22 N21 108.9(9) . . ? C22 C23 N22 108.3(9) . . ? C27 C24 C26 109.2(8) . . ? C27 C24 N22 110.3(8) . . ? C26 C24 N22 108.1(8) . . ? C27 C24 C25 113.1(9) . . ? C26 C24 C25 108.0(9) . . ? N22 C24 C25 107.9(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.191 _refine_diff_density_min -0.922 _refine_diff_density_rms 0.179 # Attachment '- BmButGaCl2 (61s10).cif' data_61s10 _database_code_depnum_ccdc_archive 'CCDC 776955' #TrackingRef '- BmButGaCl2 (61s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 B Cl2 Ga N4 S2' _chemical_formula_weight 463.92 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.4551(5) _cell_length_b 12.3855(5) _cell_length_c 28.4550(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4037.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9314 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 32.19 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.839 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5654 _exptl_absorpt_correction_T_max 0.8820 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 52776 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5016 _reflns_number_gt 4289 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to be 1.1 angstroms. ; _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^)+(0.0579P)^2^+10.3680P] 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 5016 _refine_ls_number_parameters 223 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1202 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Ga Ga 0.45783(3) 0.01838(3) 0.626413(11) 0.02104(10) Uani 1 1 d . . . Cl1 Cl 0.34611(8) -0.11969(8) 0.61773(3) 0.0399(2) Uani 1 1 d . . . Cl2 Cl 0.36922(7) 0.15812(7) 0.65504(3) 0.03122(18) Uani 1 1 d . . . S1 S 0.59630(6) -0.03445(5) 0.67914(2) 0.01975(15) Uani 1 1 d . . . S2 S 0.53874(6) 0.06607(6) 0.55617(2) 0.02351(16) Uani 1 1 d . . . B B 0.7263(3) 0.1823(3) 0.63086(10) 0.0186(6) Uani 1 1 d D . . H1 H 0.746(3) 0.1031(18) 0.6157(11) 0.022 Uiso 1 1 d D . . H2 H 0.796(2) 0.241(2) 0.6320(12) 0.022 Uiso 1 1 d D . . N11 N 0.67913(19) 0.17304(18) 0.68283(8) 0.0158(4) Uani 1 1 d . . . C11 C 0.6259(2) 0.0901(2) 0.70483(9) 0.0160(5) Uani 1 1 d . . . N12 N 0.60493(19) 0.11795(18) 0.75015(8) 0.0162(4) Uani 1 1 d . . . C12 C 0.6914(2) 0.2549(2) 0.71508(10) 0.0195(5) Uani 1 1 d . . . H12A H 0.7262 0.3233 0.7092 0.023 Uiso 1 1 calc R . . C13 C 0.6459(3) 0.2222(2) 0.75653(10) 0.0205(5) Uani 1 1 d . . . H13A H 0.6426 0.2630 0.7848 0.025 Uiso 1 1 calc R . . C14 C 0.5437(2) 0.0526(2) 0.78763(10) 0.0198(5) Uani 1 1 d . . . C15 C 0.6110(3) -0.0521(3) 0.79622(11) 0.0281(6) Uani 1 1 d . . . H15A H 0.5714 -0.0945 0.8206 0.042 Uiso 1 1 calc R . . H15B H 0.6905 -0.0350 0.8066 0.042 Uiso 1 1 calc R . . H15C H 0.6144 -0.0940 0.7670 0.042 Uiso 1 1 calc R . . C16 C 0.4180(3) 0.0324(3) 0.77162(11) 0.0256(6) Uani 1 1 d . . . H16A H 0.3786 0.1016 0.7666 0.038 Uiso 1 1 calc R . . H16B H 0.3763 -0.0087 0.7958 0.038 Uiso 1 1 calc R . . H16C H 0.4185 -0.0088 0.7422 0.038 Uiso 1 1 calc R . . C17 C 0.5405(3) 0.1191(3) 0.83278(11) 0.0294(7) Uani 1 1 d . . . H17A H 0.4962 0.1856 0.8273 0.044 Uiso 1 1 calc R . . H17B H 0.6203 0.1372 0.8423 0.044 Uiso 1 1 calc R . . H17C H 0.5028 0.0770 0.8577 0.044 Uiso 1 1 calc R . . N21 N 0.6325(2) 0.24299(19) 0.60009(8) 0.0177(4) Uani 1 1 d . . . C21 C 0.5533(2) 0.2025(2) 0.56971(9) 0.0189(5) Uani 1 1 d . . . N22 N 0.4891(2) 0.2847(2) 0.55170(8) 0.0227(5) Uani 1 1 d . . . C22 C 0.6181(3) 0.3532(2) 0.60113(10) 0.0248(6) Uani 1 1 d . . . H22A H 0.6627 0.4025 0.6193 0.030 Uiso 1 1 calc R . . C23 C 0.5298(3) 0.3793(3) 0.57190(11) 0.0272(6) Uani 1 1 d . . . H23A H 0.5008 0.4499 0.5662 0.033 Uiso 1 1 calc R . . C24 C 0.3979(3) 0.2795(3) 0.51293(11) 0.0304(7) Uani 1 1 d . . . C25 C 0.4595(3) 0.2429(4) 0.46803(12) 0.0434(9) Uani 1 1 d . . . H25A H 0.4028 0.2387 0.4423 0.065 Uiso 1 1 calc R . . H25B H 0.4945 0.1716 0.4731 0.065 Uiso 1 1 calc R . . H25C H 0.5208 0.2948 0.4599 0.065 Uiso 1 1 calc R . . C26 C 0.2996(3) 0.2016(3) 0.52634(13) 0.0377(8) Uani 1 1 d . . . H26A H 0.2427 0.1979 0.5007 0.057 Uiso 1 1 calc R . . H26B H 0.2610 0.2275 0.5549 0.057 Uiso 1 1 calc R . . H26C H 0.3323 0.1297 0.5320 0.057 Uiso 1 1 calc R . . C27 C 0.3462(3) 0.3924(3) 0.50663(14) 0.0432(9) Uani 1 1 d . . . H27A H 0.2887 0.3912 0.4811 0.065 Uiso 1 1 calc R . . H27B H 0.4086 0.4434 0.4989 0.065 Uiso 1 1 calc R . . H27C H 0.3080 0.4149 0.5359 0.065 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 Ga 0.01893(17) 0.02215(17) 0.02204(17) 0.00054(12) -0.00072(11) -0.00193(12) Cl1 0.0414(5) 0.0393(5) 0.0389(5) -0.0047(4) -0.0008(4) -0.0133(4) Cl2 0.0282(4) 0.0322(4) 0.0333(4) 0.0012(3) 0.0028(3) 0.0061(3) S1 0.0215(3) 0.0141(3) 0.0236(3) -0.0009(2) -0.0017(3) 0.0019(2) S2 0.0253(4) 0.0267(4) 0.0185(3) -0.0050(3) -0.0010(3) -0.0039(3) B 0.0155(13) 0.0246(15) 0.0156(13) 0.0026(11) -0.0001(10) -0.0004(11) N11 0.0137(10) 0.0180(10) 0.0155(10) 0.0007(8) -0.0016(8) -0.0002(8) C11 0.0117(11) 0.0172(12) 0.0192(12) 0.0000(10) -0.0009(9) 0.0012(9) N12 0.0144(10) 0.0180(10) 0.0162(10) 0.0000(8) 0.0008(8) -0.0006(8) C12 0.0197(13) 0.0177(12) 0.0210(13) -0.0004(10) -0.0011(10) -0.0026(10) C13 0.0243(13) 0.0190(12) 0.0181(13) -0.0022(10) 0.0001(10) -0.0038(10) C14 0.0172(12) 0.0226(13) 0.0197(13) 0.0044(10) 0.0036(10) -0.0016(10) C15 0.0282(15) 0.0291(15) 0.0271(15) 0.0117(12) 0.0025(12) 0.0064(12) C16 0.0169(13) 0.0295(15) 0.0305(15) 0.0046(12) 0.0045(11) -0.0018(11) C17 0.0312(16) 0.0363(17) 0.0207(14) -0.0005(12) 0.0092(12) -0.0059(13) N21 0.0191(11) 0.0197(11) 0.0145(10) 0.0003(8) 0.0003(8) -0.0011(9) C21 0.0186(12) 0.0241(13) 0.0139(11) 0.0019(10) 0.0011(9) -0.0012(10) N22 0.0208(11) 0.0312(13) 0.0161(11) 0.0059(9) 0.0000(9) 0.0018(10) C22 0.0338(16) 0.0211(13) 0.0193(13) 0.0018(11) 0.0001(12) -0.0009(12) C23 0.0361(17) 0.0235(14) 0.0221(14) 0.0047(11) 0.0016(12) 0.0062(12) C24 0.0194(13) 0.050(2) 0.0220(14) 0.0108(13) -0.0038(11) 0.0012(13) C25 0.0322(18) 0.079(3) 0.0186(15) 0.0046(17) -0.0069(13) 0.0007(18) C26 0.0220(15) 0.055(2) 0.0364(18) 0.0061(16) -0.0065(13) -0.0030(15) C27 0.0305(17) 0.055(2) 0.044(2) 0.0233(18) -0.0072(15) 0.0068(16) _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 Ga Cl1 2.1501(9) . ? Ga Cl2 2.1655(8) . ? Ga S1 2.2792(8) . ? Ga S2 2.2809(8) . ? S1 C11 1.740(3) . ? S2 C21 1.741(3) . ? B H2 1.082(18) . ? B H1 1.094(18) . ? B N21 1.577(4) . ? B N11 1.579(4) . ? N11 C11 1.349(3) . ? N11 C12 1.375(3) . ? C11 N12 1.356(3) . ? N12 C13 1.385(3) . ? N12 C14 1.512(3) . ? C12 C13 1.352(4) . ? C14 C17 1.526(4) . ? C14 C15 1.529(4) . ? C14 C16 1.531(4) . ? N21 C21 1.350(3) . ? N21 C22 1.375(4) . ? C21 N22 1.356(4) . ? N22 C23 1.386(4) . ? N22 C24 1.521(4) . ? C22 C23 1.349(4) . ? C24 C27 1.529(5) . ? C24 C25 1.529(5) . ? C24 C26 1.531(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 Cl1 Ga Cl2 113.57(4) . . ? Cl1 Ga S1 105.16(3) . . ? Cl2 Ga S1 107.94(3) . . ? Cl1 Ga S2 110.31(3) . . ? Cl2 Ga S2 108.25(3) . . ? S1 Ga S2 111.61(3) . . ? C11 S1 Ga 99.09(9) . . ? C21 S2 Ga 95.54(9) . . ? H2 B H1 118(3) . . ? H2 B N21 101.4(19) . . ? H1 B N21 110.3(18) . . ? H2 B N11 105.9(18) . . ? H1 B N11 111.9(18) . . ? N21 B N11 108.8(2) . . ? C11 N11 C12 107.4(2) . . ? C11 N11 B 130.1(2) . . ? C12 N11 B 122.5(2) . . ? N11 C11 N12 109.1(2) . . ? N11 C11 S1 124.6(2) . . ? N12 C11 S1 126.2(2) . . ? C11 N12 C13 107.6(2) . . ? C11 N12 C14 128.1(2) . . ? C13 N12 C14 124.3(2) . . ? C13 C12 N11 108.7(2) . . ? C12 C13 N12 107.2(2) . . ? N12 C14 C17 108.4(2) . . ? N12 C14 C15 109.4(2) . . ? C17 C14 C15 109.6(3) . . ? N12 C14 C16 108.3(2) . . ? C17 C14 C16 108.4(2) . . ? C15 C14 C16 112.6(3) . . ? C21 N21 C22 107.6(2) . . ? C21 N21 B 129.5(2) . . ? C22 N21 B 122.9(2) . . ? N21 C21 N22 109.1(2) . . ? N21 C21 S2 124.5(2) . . ? N22 C21 S2 126.4(2) . . ? C21 N22 C23 107.2(2) . . ? C21 N22 C24 128.0(3) . . ? C23 N22 C24 124.6(3) . . ? C23 C22 N21 108.3(3) . . ? C22 C23 N22 107.8(3) . . ? N22 C24 C27 108.2(3) . . ? N22 C24 C25 107.6(2) . . ? C27 C24 C25 110.6(3) . . ? N22 C24 C26 110.5(2) . . ? C27 C24 C26 108.7(3) . . ? C25 C24 C26 111.2(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.765 _refine_diff_density_min -1.310 _refine_diff_density_rms 0.102 # Attachment '- BmButGaI2 (KY286S10).cif' data_ky286s10 _database_code_depnum_ccdc_archive 'CCDC 776956' #TrackingRef '- BmButGaI2 (KY286S10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 B Ga I2 N4 S2' _chemical_formula_weight 646.82 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 13.6133(16) _cell_length_b 14.6412(18) _cell_length_c 11.4378(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2279.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9940 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 30.06 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 4.103 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6176 _exptl_absorpt_correction_T_max 0.9224 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35083 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 30.48 _reflns_number_total 3593 _reflns_number_gt 2663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to be 1.1 angstroms. ; _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^)+(0.0233P)^2^+0.5935P] 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 3593 _refine_ls_number_parameters 119 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Ga Ga 0.32252(3) 0.7500 1.00722(4) 0.02087(10) Uani 1 2 d S . . I1 I 0.154256(19) 0.7500 0.91256(2) 0.02376(7) Uani 1 2 d S . . I2 I 0.47541(2) 0.7500 0.88019(2) 0.03392(8) Uani 1 2 d S . . S S 0.34084(5) 0.61813(5) 1.11059(6) 0.02432(15) Uani 1 1 d . . . B B 0.2200(3) 0.7500 1.3016(4) 0.0205(9) Uani 1 2 d SD . . H1 H 0.3002(14) 0.7500 1.293(3) 0.025 Uiso 1 2 d SD . . H2 H 0.190(3) 0.7500 1.391(2) 0.025 Uiso 1 2 d SD . . N1 N 0.17817(16) 0.66202(15) 1.23989(19) 0.0207(5) Uani 1 1 d . . . C1 C 0.2227(2) 0.60428(18) 1.1652(2) 0.0192(5) Uani 1 1 d . . . N2 N 0.16202(17) 0.53288(15) 1.14354(18) 0.0212(5) Uani 1 1 d . . . C2 C 0.0878(2) 0.6263(2) 1.2653(3) 0.0290(7) Uani 1 1 d . . . H2A H 0.0403 0.6531 1.3155 0.035 Uiso 1 1 calc R . . C3 C 0.0773(2) 0.5471(2) 1.2074(3) 0.0287(6) Uani 1 1 d . . . H3A H 0.0217 0.5080 1.2099 0.034 Uiso 1 1 calc R . . C4 C 0.1817(2) 0.45064(19) 1.0671(2) 0.0263(6) Uani 1 1 d . . . C5 C 0.0910(3) 0.3901(2) 1.0671(3) 0.0365(8) Uani 1 1 d . . . H5A H 0.0772 0.3696 1.1470 0.055 Uiso 1 1 calc R . . H5B H 0.1025 0.3369 1.0169 0.055 Uiso 1 1 calc R . . H5C H 0.0347 0.4247 1.0373 0.055 Uiso 1 1 calc R . . C6 C 0.2684(3) 0.3986(2) 1.1181(3) 0.0424(8) Uani 1 1 d . . . H6A H 0.2530 0.3798 1.1983 0.064 Uiso 1 1 calc R . . H6B H 0.3265 0.4380 1.1185 0.064 Uiso 1 1 calc R . . H6C H 0.2815 0.3444 1.0703 0.064 Uiso 1 1 calc R . . C7 C 0.2007(2) 0.4819(2) 0.9415(2) 0.0293(7) Uani 1 1 d . . . H7A H 0.2591 0.5210 0.9395 0.044 Uiso 1 1 calc R . . H7B H 0.1438 0.5164 0.9129 0.044 Uiso 1 1 calc R . . H7C H 0.2113 0.4284 0.8915 0.044 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 Ga 0.0152(2) 0.0284(2) 0.0190(2) 0.000 0.00148(15) 0.000 I1 0.01981(12) 0.02620(14) 0.02527(13) 0.000 -0.00454(10) 0.000 I2 0.02194(14) 0.0510(2) 0.02887(15) 0.000 0.00942(11) 0.000 S 0.0179(3) 0.0276(4) 0.0275(4) 0.0000(3) -0.0001(3) 0.0040(3) B 0.025(2) 0.018(2) 0.018(2) 0.000 -0.0033(17) 0.000 N1 0.0228(12) 0.0217(12) 0.0177(11) 0.0015(9) 0.0020(9) -0.0001(9) C1 0.0230(14) 0.0202(14) 0.0144(12) 0.0036(10) -0.0012(10) 0.0017(11) N2 0.0257(12) 0.0200(11) 0.0180(11) 0.0001(9) -0.0005(9) -0.0012(10) C2 0.0263(15) 0.0318(16) 0.0288(16) -0.0005(13) 0.0092(12) -0.0046(12) C3 0.0270(16) 0.0295(17) 0.0295(15) 0.0007(12) 0.0068(12) -0.0085(12) C4 0.0368(16) 0.0190(14) 0.0232(14) -0.0028(11) -0.0003(12) 0.0040(12) C5 0.056(2) 0.0238(16) 0.0302(17) -0.0009(13) -0.0013(15) -0.0111(15) C6 0.059(2) 0.0248(17) 0.0430(19) -0.0033(14) -0.0129(17) 0.0139(16) C7 0.0406(18) 0.0253(16) 0.0219(15) -0.0052(12) -0.0003(12) 0.0019(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga S 2.2777(8) 7_575 ? Ga S 2.2777(8) . ? Ga I1 2.5336(5) . ? Ga I2 2.5383(5) . ? S C1 1.738(3) . ? B H1 1.097(18) . ? B H2 1.103(18) . ? B N1 1.575(3) . ? B N1 1.575(3) 7_575 ? N1 C1 1.346(3) . ? N1 C2 1.368(3) . ? C1 N2 1.355(3) . ? N2 C3 1.381(4) . ? N2 C4 1.512(3) . ? C2 C3 1.342(4) . ? C4 C5 1.521(4) . ? C4 C6 1.521(4) . ? C4 C7 1.531(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 S Ga S 115.91(4) 7_575 . ? S Ga I1 108.72(2) 7_575 . ? S Ga I1 108.71(2) . . ? S Ga I2 101.97(2) 7_575 . ? S Ga I2 101.97(2) . . ? I1 Ga I2 119.78(2) . . ? C1 S Ga 100.61(9) . . ? H1 B H2 117(3) . . ? H1 B N1 108.7(11) . . ? H2 B N1 106.6(11) . . ? H1 B N1 108.7(11) . 7_575 ? H2 B N1 106.6(11) . 7_575 ? N1 B N1 109.7(3) . 7_575 ? C1 N1 C2 107.4(2) . . ? C1 N1 B 129.5(3) . . ? C2 N1 B 122.9(3) . . ? N1 C1 N2 109.1(2) . . ? N1 C1 S 124.9(2) . . ? N2 C1 S 126.0(2) . . ? C1 N2 C3 107.2(2) . . ? C1 N2 C4 127.8(2) . . ? C3 N2 C4 125.0(2) . . ? C3 C2 N1 108.7(3) . . ? C2 C3 N2 107.6(2) . . ? N2 C4 C5 108.7(2) . . ? N2 C4 C6 108.4(2) . . ? C5 C4 C6 109.8(3) . . ? N2 C4 C7 109.5(2) . . ? C5 C4 C7 108.1(2) . . ? C6 C4 C7 112.3(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.797 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.125 # Attachment '- BmButIn(mim)Cl (14s10).cif' data_14s10_BmButIn(mim)Cl _database_code_depnum_ccdc_archive 'CCDC 776957' #TrackingRef '- BmButIn(mim)Cl (14s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H35 B Cl In N6 S3' _chemical_formula_weight 628.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 24.951(3) _cell_length_b 12.0422(16) _cell_length_c 19.097(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.109(2) _cell_angle_gamma 90.00 _cell_volume 5693.8(13) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9804 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 32.04 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 1.165 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5935 _exptl_absorpt_correction_T_max 0.9440 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 58883 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10017 _reflns_number_gt 8547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to be 1.1 angstroms. The ADPs of several carbon atoms have been restrained. ; _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^+261.0000P] 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 0.00039(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10017 _refine_ls_number_parameters 608 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0986 _refine_ls_wR_factor_ref 0.3161 _refine_ls_wR_factor_gt 0.3102 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.179 _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 In1 In 0.11060(4) 0.54577(8) 0.17518(5) 0.0215(3) Uani 1 1 d . . . In2 In 0.38583(4) 1.03008(8) 0.14224(5) 0.0214(3) Uani 1 1 d . . . Cl1 Cl 0.13982(15) 0.3644(3) 0.1345(2) 0.0309(8) Uani 1 1 d . . . Cl2 Cl 0.35915(15) 0.8520(3) 0.0863(2) 0.0320(8) Uani 1 1 d . . . S1 S 0.15307(14) 0.5148(3) 0.29752(19) 0.0236(7) Uani 1 1 d . . . S2 S 0.01467(15) 0.4925(3) 0.1554(2) 0.0268(8) Uani 1 1 d . . . S3 S 0.15917(17) 0.6695(3) 0.0980(2) 0.0307(9) Uani 1 1 d . . . S4 S 0.48168(15) 0.9763(3) 0.1521(2) 0.0277(8) Uani 1 1 d . . . S5 S 0.34435(14) 0.9984(3) 0.25204(19) 0.0246(7) Uani 1 1 d . . . S6 S 0.33507(17) 1.1590(3) 0.0538(2) 0.0319(9) Uani 1 1 d . . . B1 B 0.0251(6) 0.5619(15) 0.3291(9) 0.026(3) Uani 1 1 d D . . H1 H 0.008(6) 0.544(13) 0.378(5) 0.031 Uiso 1 1 d D . . H2 H 0.031(7) 0.472(3) 0.326(8) 0.031 Uiso 1 1 d D . . B2 B 0.4743(6) 1.0398(15) 0.3223(9) 0.024(3) Uani 1 1 d D . . H3 H 0.494(6) 1.037(13) 0.377(3) 0.029 Uiso 1 1 d D . . H4 H 0.457(6) 0.961(7) 0.301(8) 0.029 Uiso 1 1 d D . . N11 N 0.0757(5) 0.6386(10) 0.3538(6) 0.024(3) Uani 1 1 d . . . C11 C 0.1276(5) 0.6267(11) 0.3404(7) 0.018(3) Uani 1 1 d . . . N12 N 0.1556(4) 0.7128(9) 0.3725(6) 0.020(2) Uani 1 1 d . . . C12 C 0.0714(6) 0.7331(12) 0.3913(7) 0.026(3) Uani 1 1 d . . . H12A H 0.0390 0.7615 0.4057 0.031 Uiso 1 1 calc R . . C13 C 0.1199(6) 0.7795(12) 0.4048(8) 0.027(3) Uani 1 1 d . . . H13A H 0.1286 0.8453 0.4312 0.033 Uiso 1 1 calc R . . C14 C 0.2157(6) 0.7364(13) 0.3720(8) 0.027(3) Uani 1 1 d . . . C15 C 0.2260(7) 0.7562(15) 0.2971(8) 0.038(4) Uani 1 1 d . . . H15A H 0.2040 0.8189 0.2775 0.057 Uiso 1 1 calc R . . H15B H 0.2163 0.6895 0.2689 0.057 Uiso 1 1 calc R . . H15C H 0.2643 0.7731 0.2960 0.057 Uiso 1 1 calc R . . C16 C 0.2491(6) 0.6398(15) 0.4075(9) 0.040(4) Uani 1 1 d . . . H16A H 0.2407 0.5715 0.3804 0.060 Uiso 1 1 calc R . . H16B H 0.2402 0.6298 0.4557 0.060 Uiso 1 1 calc R . . H16C H 0.2877 0.6565 0.4090 0.060 Uiso 1 1 calc R . . C17 C 0.2290(7) 0.8411(15) 0.4158(10) 0.046(4) Uani 1 1 d . . . H17A H 0.2082 0.9037 0.3938 0.069 Uiso 1 1 calc R . . H17B H 0.2677 0.8571 0.4181 0.069 Uiso 1 1 calc R . . H17C H 0.2196 0.8296 0.4636 0.069 Uiso 1 1 calc R . . C21 C -0.0156(5) 0.6006(11) 0.1962(7) 0.020(3) Uani 1 1 d . . . N21 N -0.0115(4) 0.6197(9) 0.2662(6) 0.021(2) Uani 1 1 d . . . N22 N -0.0524(5) 0.6740(9) 0.1629(6) 0.025(3) Uani 1 1 d . . . C22 C -0.0456(5) 0.7064(12) 0.2773(8) 0.026(3) Uani 1 1 d . . . H22A H -0.0506 0.7373 0.3218 0.031 Uiso 1 1 calc R . . C23 C -0.0707(6) 0.7400(12) 0.2136(8) 0.026(3) Uani 1 1 d . . . H23A H -0.0962 0.7986 0.2056 0.031 Uiso 1 1 calc R . . C24 C -0.0714(6) 0.6846(13) 0.0855(8) 0.031(3) Uani 1 1 d . . . C25 C -0.1003(7) 0.5759(14) 0.0601(8) 0.037(4) Uani 1 1 d . . . H25A H -0.0748 0.5139 0.0667 0.056 Uiso 1 1 calc R . . H25B H -0.1142 0.5825 0.0100 0.056 Uiso 1 1 calc R . . H25C H -0.1304 0.5623 0.0874 0.056 Uiso 1 1 calc R . . C26 C -0.1122(8) 0.7782(16) 0.0739(10) 0.048(5) Uani 1 1 d . . . H26A H -0.1432 0.7616 0.0991 0.072 Uiso 1 1 calc R . . H26B H -0.1245 0.7855 0.0234 0.072 Uiso 1 1 calc R . . H26C H -0.0954 0.8478 0.0918 0.072 Uiso 1 1 calc R . . C27 C -0.0229(8) 0.7090(17) 0.0448(10) 0.049(5) Uani 1 1 d . . . H27A H 0.0031 0.6478 0.0517 0.073 Uiso 1 1 calc R . . H27B H -0.0054 0.7781 0.0623 0.073 Uiso 1 1 calc R . . H27C H -0.0357 0.7167 -0.0056 0.073 Uiso 1 1 calc R . . N31 N 0.0955(5) 0.7353(10) 0.1916(6) 0.023(2) Uani 1 1 d . . . C31 C 0.1286(6) 0.7694(12) 0.1459(7) 0.023(3) Uani 1 1 d . . . N32 N 0.1327(5) 0.8827(9) 0.1474(6) 0.022(2) Uani 1 1 d . . . C32 C 0.0766(6) 0.8290(12) 0.2209(8) 0.026(3) Uani 1 1 d . . . H32A H 0.0507 0.8293 0.2535 0.031 Uiso 1 1 calc R . . C33 C 0.1002(6) 0.9229(12) 0.1966(7) 0.025(3) Uani 1 1 d U . . H33A H 0.0955 0.9978 0.2103 0.029 Uiso 1 1 calc R . . C34 C 0.1626(6) 0.9598(12) 0.1006(7) 0.023(3) Uani 1 1 d U . . C35 C 0.1576(8) 1.0758(13) 0.1245(10) 0.041(4) Uani 1 1 d . . . H35A H 0.1196 1.0985 0.1166 0.061 Uiso 1 1 calc R . . H35B H 0.1791 1.1246 0.0978 0.061 Uiso 1 1 calc R . . H35C H 0.1707 1.0811 0.1749 0.061 Uiso 1 1 calc R . . C36 C 0.2227(6) 0.9236(15) 0.1139(10) 0.039(4) Uani 1 1 d . . . H36A H 0.2365 0.9354 0.1636 0.058 Uiso 1 1 calc R . . H36B H 0.2439 0.9677 0.0841 0.058 Uiso 1 1 calc R . . H36C H 0.2257 0.8447 0.1023 0.058 Uiso 1 1 calc R . . C37 C 0.1375(8) 0.9418(13) 0.0247(9) 0.040(4) Uani 1 1 d . . . H37A H 0.0995 0.9646 0.0196 0.061 Uiso 1 1 calc R . . H37B H 0.1399 0.8630 0.0126 0.061 Uiso 1 1 calc R . . H37C H 0.1570 0.9862 -0.0070 0.061 Uiso 1 1 calc R . . N41 N 0.5091(4) 1.1023(10) 0.2715(6) 0.022(2) Uani 1 1 d . . . C41 C 0.5132(5) 1.0850(11) 0.2028(7) 0.020(3) Uani 1 1 d . . . N42 N 0.5481(4) 1.1590(10) 0.1803(6) 0.024(2) Uani 1 1 d . . . C42 C 0.5430(6) 1.1881(12) 0.2931(8) 0.029(3) Uani 1 1 d . . . H42A H 0.5485 1.2177 0.3395 0.035 Uiso 1 1 calc R . . C43 C 0.5675(6) 1.2242(13) 0.2380(9) 0.031(3) Uani 1 1 d . . . H43A H 0.5930 1.2829 0.2386 0.037 Uiso 1 1 calc R . . C44 C 0.5656(7) 1.1709(14) 0.1078(9) 0.036(4) Uani 1 1 d . . . C45 C 0.5942(8) 1.0622(15) 0.0910(10) 0.044(4) Uani 1 1 d . . . H45A H 0.5689 1.0000 0.0910 0.066 Uiso 1 1 calc R . . H45B H 0.6253 1.0495 0.1269 0.066 Uiso 1 1 calc R . . H45C H 0.6067 1.0682 0.0445 0.066 Uiso 1 1 calc R . . C46 C 0.6049(7) 1.2665(15) 0.1075(9) 0.041(4) Uani 1 1 d . . . H46A H 0.6367 1.2518 0.1418 0.061 Uiso 1 1 calc R . . H46B H 0.5874 1.3352 0.1204 0.061 Uiso 1 1 calc R . . H46C H 0.6160 1.2743 0.0603 0.061 Uiso 1 1 calc R . . C47 C 0.5171(7) 1.1943(17) 0.0537(9) 0.045(4) Uani 1 1 d . . . H47A H 0.4913 1.1329 0.0532 0.067 Uiso 1 1 calc R . . H47B H 0.5290 1.2020 0.0069 0.067 Uiso 1 1 calc R . . H47C H 0.4997 1.2633 0.0661 0.067 Uiso 1 1 calc R . . N51 N 0.4240(5) 1.1150(10) 0.3334(6) 0.024(3) Uani 1 1 d . . . C51 C 0.3724(6) 1.1043(11) 0.3042(7) 0.021(3) Uani 1 1 d . . . N52 N 0.3428(5) 1.1917(10) 0.3291(7) 0.028(3) Uani 1 1 d . . . C52 C 0.4282(6) 1.2080(14) 0.3761(8) 0.032(3) Uani 1 1 d . . . H52A H 0.4603 1.2349 0.4025 0.038 Uiso 1 1 calc R . . C53 C 0.3796(7) 1.2534(13) 0.3738(8) 0.034(4) Uani 1 1 d . . . H53A H 0.3713 1.3180 0.3988 0.040 Uiso 1 1 calc R . . C54 C 0.2843(6) 1.2208(13) 0.3101(8) 0.028(3) Uani 1 1 d . . . C55 C 0.2749(6) 1.2438(15) 0.2310(8) 0.035(4) Uani 1 1 d . . . H55A H 0.2979 1.3056 0.2198 0.053 Uiso 1 1 calc R . . H55B H 0.2369 1.2633 0.2173 0.053 Uiso 1 1 calc R . . H55C H 0.2838 1.1774 0.2052 0.053 Uiso 1 1 calc R . . C56 C 0.2486(6) 1.1256(15) 0.3297(9) 0.038(4) Uani 1 1 d . . . H56A H 0.2567 1.0585 0.3040 0.056 Uiso 1 1 calc R . . H56B H 0.2106 1.1455 0.3172 0.056 Uiso 1 1 calc R . . H56C H 0.2557 1.1118 0.3806 0.056 Uiso 1 1 calc R . . C57 C 0.2716(7) 1.3249(14) 0.3513(10) 0.040(4) Uani 1 1 d . . . H57A H 0.2944 1.3865 0.3390 0.060 Uiso 1 1 calc R . . H57B H 0.2789 1.3100 0.4020 0.060 Uiso 1 1 calc R . . H57C H 0.2335 1.3447 0.3392 0.060 Uiso 1 1 calc R . . N61 N 0.4018(5) 1.2202(10) 0.1660(7) 0.028(3) Uani 1 1 d . . . C61 C 0.3661(5) 1.2571(11) 0.1121(7) 0.023(3) Uani 1 1 d . . . N62 N 0.3601(5) 1.3714(10) 0.1163(6) 0.024(3) Uani 1 1 d . . . C62 C 0.4201(6) 1.3124(13) 0.2035(8) 0.028(3) Uani 1 1 d . . . H62A H 0.4458 1.3116 0.2445 0.034 Uiso 1 1 calc R . . C63 C 0.3969(6) 1.4025(13) 0.1745(8) 0.032(4) Uani 1 1 d . . . H63A H 0.4040 1.4764 0.1905 0.039 Uiso 1 1 calc R . . C64 C 0.3295(6) 1.4478(13) 0.0665(8) 0.031(4) Uani 1 1 d . . . C65 C 0.2713(8) 1.4027(19) 0.0487(12) 0.060(6) Uani 1 1 d . . . H65A H 0.2542 1.3972 0.0921 0.090 Uiso 1 1 calc R . . H65B H 0.2724 1.3291 0.0270 0.090 Uiso 1 1 calc R . . H65C H 0.2503 1.4534 0.0157 0.090 Uiso 1 1 calc R . . C66 C 0.3557(10) 1.456(2) -0.0021(12) 0.064(6) Uani 1 1 d U . . H66A H 0.3928 1.4829 0.0086 0.096 Uiso 1 1 calc R . . H66B H 0.3349 1.5070 -0.0347 0.096 Uiso 1 1 calc R . . H66C H 0.3560 1.3820 -0.0239 0.096 Uiso 1 1 calc R . . C67 C 0.3256(12) 1.559(2) 0.0971(15) 0.082(7) Uani 1 1 d U . . H67A H 0.3620 1.5898 0.1096 0.124 Uiso 1 1 calc R . . H67B H 0.3074 1.5543 0.1396 0.124 Uiso 1 1 calc R . . H67C H 0.3049 1.6080 0.0626 0.124 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 0.0238(5) 0.0155(5) 0.0259(5) -0.0003(4) 0.0061(4) 0.0011(4) In2 0.0217(5) 0.0188(5) 0.0229(5) -0.0004(4) -0.0003(4) -0.0001(4) Cl1 0.0333(19) 0.0214(17) 0.039(2) -0.0042(15) 0.0081(16) 0.0043(14) Cl2 0.0305(19) 0.0257(18) 0.038(2) -0.0062(15) -0.0003(15) -0.0027(15) S1 0.0192(16) 0.0201(17) 0.0316(19) 0.0005(14) 0.0029(14) 0.0015(13) S2 0.0247(18) 0.0203(17) 0.035(2) -0.0043(15) 0.0033(15) 0.0003(14) S3 0.043(2) 0.0195(17) 0.033(2) -0.0016(15) 0.0189(17) -0.0001(16) S4 0.0226(18) 0.0229(18) 0.038(2) -0.0053(15) 0.0034(15) 0.0016(14) S5 0.0212(17) 0.0265(18) 0.0263(18) -0.0045(14) 0.0037(14) -0.0045(14) S6 0.042(2) 0.0249(19) 0.0255(18) -0.0005(15) -0.0077(16) -0.0004(16) B1 0.018(8) 0.033(9) 0.026(8) 0.003(7) -0.001(6) -0.002(7) B2 0.011(7) 0.037(9) 0.026(8) 0.003(7) 0.001(6) -0.001(6) N11 0.022(6) 0.025(6) 0.026(6) 0.002(5) 0.003(5) 0.004(5) C11 0.015(6) 0.020(6) 0.018(6) 0.005(5) -0.002(5) -0.002(5) N12 0.018(6) 0.024(6) 0.017(5) -0.005(5) -0.002(4) -0.003(5) C12 0.025(7) 0.033(8) 0.019(7) 0.002(6) 0.006(6) 0.006(6) C13 0.037(8) 0.016(7) 0.029(7) -0.003(6) 0.002(6) 0.002(6) C14 0.018(7) 0.031(8) 0.031(8) -0.003(6) 0.001(6) -0.009(6) C15 0.033(9) 0.045(10) 0.036(9) 0.002(8) 0.007(7) -0.016(8) C16 0.024(8) 0.047(10) 0.046(10) 0.006(8) -0.009(7) -0.003(7) C17 0.041(10) 0.044(10) 0.052(11) -0.016(9) -0.003(8) -0.020(8) C21 0.014(6) 0.022(7) 0.023(7) -0.003(5) 0.007(5) -0.006(5) N21 0.015(5) 0.017(6) 0.034(7) 0.000(5) 0.009(5) -0.003(4) N22 0.027(6) 0.017(6) 0.030(6) 0.001(5) 0.003(5) 0.001(5) C22 0.018(7) 0.024(7) 0.037(8) 0.002(6) 0.009(6) -0.002(6) C23 0.019(7) 0.022(7) 0.035(8) 0.006(6) 0.002(6) 0.001(6) C24 0.030(8) 0.029(8) 0.034(8) -0.002(7) 0.002(6) 0.007(6) C25 0.040(9) 0.039(9) 0.029(8) -0.002(7) -0.010(7) -0.001(8) C26 0.048(11) 0.047(11) 0.047(10) 0.012(9) -0.009(9) 0.017(9) C27 0.055(12) 0.055(12) 0.038(10) 0.015(9) 0.016(9) -0.005(9) N31 0.019(6) 0.022(6) 0.028(6) 0.002(5) 0.000(5) -0.003(5) C31 0.023(7) 0.027(7) 0.020(7) -0.004(6) 0.005(5) -0.001(6) N32 0.026(6) 0.017(6) 0.024(6) -0.004(5) 0.006(5) -0.002(5) C32 0.025(7) 0.023(7) 0.032(8) 0.004(6) 0.007(6) 0.004(6) C33 0.024(3) 0.025(3) 0.025(3) 0.0001(10) 0.0033(11) 0.0004(10) C34 0.023(3) 0.023(3) 0.023(3) 0.0002(10) 0.0029(11) -0.0005(10) C35 0.057(11) 0.017(7) 0.051(10) -0.003(7) 0.021(9) -0.011(7) C36 0.025(8) 0.041(9) 0.052(10) 0.009(8) 0.013(7) -0.003(7) C37 0.068(12) 0.021(8) 0.040(9) -0.006(7) 0.038(9) -0.003(8) N41 0.014(5) 0.023(6) 0.028(6) -0.002(5) -0.002(5) 0.005(5) C41 0.011(6) 0.021(7) 0.028(7) 0.004(6) 0.002(5) 0.000(5) N42 0.016(6) 0.026(6) 0.029(6) -0.004(5) 0.000(5) -0.001(5) C42 0.023(7) 0.026(8) 0.036(8) -0.006(6) -0.003(6) 0.009(6) C43 0.019(7) 0.029(8) 0.045(9) -0.006(7) 0.001(6) 0.000(6) C44 0.030(8) 0.032(9) 0.046(10) 0.009(7) 0.007(7) -0.003(7) C45 0.047(10) 0.043(10) 0.045(10) -0.006(8) 0.019(8) 0.002(8) C46 0.040(9) 0.041(10) 0.045(10) 0.003(8) 0.018(8) -0.009(8) C47 0.038(10) 0.061(12) 0.034(9) 0.006(8) 0.000(7) -0.007(9) N51 0.027(6) 0.019(6) 0.026(6) -0.002(5) 0.000(5) -0.003(5) C51 0.026(7) 0.021(7) 0.016(6) -0.002(5) 0.003(5) 0.000(6) N52 0.022(6) 0.026(6) 0.034(7) -0.002(5) -0.002(5) 0.004(5) C52 0.029(8) 0.043(9) 0.022(7) -0.008(7) -0.006(6) 0.004(7) C53 0.042(9) 0.028(8) 0.029(8) -0.012(7) -0.002(7) 0.006(7) C54 0.027(8) 0.029(8) 0.029(8) -0.007(6) 0.001(6) 0.004(6) C55 0.030(8) 0.042(9) 0.033(8) 0.009(7) 0.003(7) 0.015(7) C56 0.022(8) 0.045(10) 0.046(10) 0.008(8) 0.005(7) -0.004(7) C57 0.035(9) 0.036(9) 0.049(10) -0.009(8) 0.002(8) 0.014(7) N61 0.027(6) 0.024(6) 0.032(7) 0.005(5) 0.000(5) -0.001(5) C61 0.020(7) 0.019(7) 0.030(7) 0.004(6) 0.011(6) 0.003(5) N62 0.028(6) 0.025(6) 0.020(6) 0.002(5) 0.002(5) 0.000(5) C62 0.026(7) 0.033(8) 0.023(7) -0.001(6) -0.011(6) -0.011(6) C63 0.038(9) 0.022(7) 0.034(8) 0.001(6) -0.009(7) -0.013(7) C64 0.036(8) 0.033(8) 0.021(7) 0.005(6) -0.008(6) 0.019(7) C65 0.048(12) 0.065(14) 0.060(13) 0.022(11) -0.015(10) 0.007(10) C66 0.064(6) 0.064(6) 0.064(6) 0.0002(10) 0.0078(12) 0.0001(10) C67 0.083(7) 0.082(7) 0.082(7) 0.0000(10) 0.0099(14) 0.0001(10) _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 N31 2.341(12) . ? In1 Cl1 2.459(4) . ? In1 S2 2.461(4) . ? In1 S1 2.471(4) . ? In1 S3 2.510(4) . ? In2 N61 2.359(12) . ? In2 Cl2 2.451(4) . ? In2 S4 2.462(4) . ? In2 S5 2.480(4) . ? In2 S6 2.518(4) . ? S1 C11 1.737(14) . ? S2 C21 1.736(14) . ? S3 C31 1.742(14) . ? S4 C41 1.756(14) . ? S5 C51 1.713(14) . ? S6 C61 1.738(15) . ? B1 H2 1.10(2) . ? B1 H1 1.10(2) . ? B1 N21 1.58(2) . ? B1 N11 1.59(2) . ? B2 H4 1.1000(10) . ? B2 H3 1.10(2) . ? B2 N41 1.571(19) . ? B2 N51 1.58(2) . ? N11 C12 1.355(19) . ? N11 C11 1.358(17) . ? C11 N12 1.355(17) . ? N12 C13 1.398(18) . ? N12 C14 1.529(17) . ? C12 C13 1.33(2) . ? C14 C15 1.50(2) . ? C14 C17 1.53(2) . ? C14 C16 1.54(2) . ? C21 N21 1.349(18) . ? C21 N22 1.374(18) . ? N21 C22 1.379(18) . ? N22 C23 1.372(19) . ? N22 C24 1.500(19) . ? C22 C23 1.36(2) . ? C24 C26 1.52(2) . ? C24 C25 1.54(2) . ? C24 C27 1.54(2) . ? N31 C31 1.339(18) . ? N31 C32 1.369(19) . ? C31 N32 1.369(18) . ? N32 C33 1.402(18) . ? N32 C34 1.543(17) . ? C32 C33 1.38(2) . ? C34 C35 1.48(2) . ? C34 C37 1.52(2) . ? C34 C36 1.55(2) . ? N41 C41 1.345(18) . ? N41 C42 1.366(19) . ? C41 N42 1.354(17) . ? N42 C43 1.390(19) . ? N42 C44 1.51(2) . ? C42 C43 1.35(2) . ? C44 C46 1.51(2) . ? C44 C47 1.52(2) . ? C44 C45 1.54(2) . ? N51 C51 1.345(18) . ? N51 C52 1.381(19) . ? C51 N52 1.403(18) . ? N52 C53 1.39(2) . ? N52 C54 1.501(18) . ? C52 C53 1.33(2) . ? C54 C55 1.52(2) . ? C54 C56 1.53(2) . ? C54 C57 1.53(2) . ? N61 C61 1.351(19) . ? N61 C62 1.368(19) . ? C61 N62 1.388(18) . ? N62 C63 1.403(19) . ? N62 C64 1.468(17) . ? C62 C63 1.32(2) . ? C64 C67 1.47(3) . ? C64 C66 1.54(3) . ? C64 C65 1.55(3) . ? 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 N31 In1 Cl1 165.3(3) . . ? N31 In1 S2 96.0(3) . . ? Cl1 In1 S2 92.35(12) . . ? N31 In1 S1 94.4(3) . . ? Cl1 In1 S1 93.19(12) . . ? S2 In1 S1 113.62(13) . . ? N31 In1 S3 66.2(3) . . ? Cl1 In1 S3 99.09(13) . . ? S2 In1 S3 126.56(14) . . ? S1 In1 S3 117.56(13) . . ? N61 In2 Cl2 164.5(3) . . ? N61 In2 S4 95.8(3) . . ? Cl2 In2 S4 90.69(13) . . ? N61 In2 S5 93.7(3) . . ? Cl2 In2 S5 96.57(13) . . ? S4 In2 S5 113.47(13) . . ? N61 In2 S6 65.8(3) . . ? Cl2 In2 S6 99.23(13) . . ? S4 In2 S6 128.05(14) . . ? S5 In2 S6 115.74(14) . . ? C11 S1 In1 100.9(4) . . ? C21 S2 In1 101.8(4) . . ? C31 S3 In1 80.1(5) . . ? C41 S4 In2 102.1(4) . . ? C51 S5 In2 101.1(5) . . ? C61 S6 In2 80.9(5) . . ? H2 B1 H1 85(10) . . ? H2 B1 N21 118(9) . . ? H1 B1 N21 119(9) . . ? H2 B1 N11 119(9) . . ? H1 B1 N11 104(9) . . ? N21 B1 N11 109.5(12) . . ? H4 B2 H3 116(10) . . ? H4 B2 N41 114(8) . . ? H3 B2 N41 113(8) . . ? H4 B2 N51 105(8) . . ? H3 B2 N51 99(8) . . ? N41 B2 N51 108.5(12) . . ? C12 N11 C11 109.1(12) . . ? C12 N11 B1 122.3(12) . . ? C11 N11 B1 128.6(12) . . ? N12 C11 N11 106.5(12) . . ? N12 C11 S1 127.5(10) . . ? N11 C11 S1 125.7(10) . . ? C11 N12 C13 108.6(11) . . ? C11 N12 C14 126.2(11) . . ? C13 N12 C14 125.2(11) . . ? C13 C12 N11 109.1(13) . . ? C12 C13 N12 106.7(12) . . ? C15 C14 C17 109.9(14) . . ? C15 C14 N12 108.5(11) . . ? C17 C14 N12 107.3(12) . . ? C15 C14 C16 113.1(14) . . ? C17 C14 C16 108.3(13) . . ? N12 C14 C16 109.5(12) . . ? N21 C21 N22 108.2(11) . . ? N21 C21 S2 126.0(11) . . ? N22 C21 S2 125.4(10) . . ? C21 N21 C22 108.0(12) . . ? C21 N21 B1 130.2(12) . . ? C22 N21 B1 121.8(12) . . ? C23 N22 C21 107.9(11) . . ? C23 N22 C24 123.7(12) . . ? C21 N22 C24 128.4(12) . . ? C23 C22 N21 108.2(13) . . ? C22 C23 N22 107.6(12) . . ? N22 C24 C26 109.3(13) . . ? N22 C24 C25 108.4(12) . . ? C26 C24 C25 107.7(14) . . ? N22 C24 C27 110.0(13) . . ? C26 C24 C27 109.8(15) . . ? C25 C24 C27 111.6(14) . . ? C31 N31 C32 106.7(12) . . ? C31 N31 In1 95.1(9) . . ? C32 N31 In1 158.0(10) . . ? N31 C31 N32 110.0(12) . . ? N31 C31 S3 118.4(11) . . ? N32 C31 S3 131.6(11) . . ? C31 N32 C33 108.1(11) . . ? C31 N32 C34 128.9(11) . . ? C33 N32 C34 122.8(11) . . ? N31 C32 C33 110.7(12) . . ? C32 C33 N32 104.4(12) . . ? C35 C34 C37 112.8(13) . . ? C35 C34 N32 108.9(12) . . ? C37 C34 N32 107.1(11) . . ? C35 C34 C36 109.4(13) . . ? C37 C34 C36 113.0(13) . . ? N32 C34 C36 105.3(11) . . ? C41 N41 C42 106.9(12) . . ? C41 N41 B2 130.0(12) . . ? C42 N41 B2 123.0(12) . . ? N41 C41 N42 109.8(12) . . ? N41 C41 S4 124.8(10) . . ? N42 C41 S4 125.2(10) . . ? C41 N42 C43 107.1(12) . . ? C41 N42 C44 128.7(12) . . ? C43 N42 C44 124.2(12) . . ? C43 C42 N41 109.4(13) . . ? C42 C43 N42 106.8(13) . . ? N42 C44 C46 109.6(14) . . ? N42 C44 C47 110.2(13) . . ? C46 C44 C47 108.6(14) . . ? N42 C44 C45 107.7(13) . . ? C46 C44 C45 109.1(14) . . ? C47 C44 C45 111.6(16) . . ? C51 N51 C52 108.8(12) . . ? C51 N51 B2 128.6(12) . . ? C52 N51 B2 122.7(12) . . ? N51 C51 N52 107.7(11) . . ? N51 C51 S5 127.9(11) . . ? N52 C51 S5 124.1(10) . . ? C53 N52 C51 105.9(12) . . ? C53 N52 C54 125.0(12) . . ? C51 N52 C54 129.1(12) . . ? C53 C52 N51 108.2(13) . . ? C52 C53 N52 109.4(13) . . ? N52 C54 C55 108.0(12) . . ? N52 C54 C56 110.1(12) . . ? C55 C54 C56 110.9(13) . . ? N52 C54 C57 108.8(12) . . ? C55 C54 C57 110.1(13) . . ? C56 C54 C57 108.9(13) . . ? C61 N61 C62 106.1(12) . . ? C61 N61 In2 95.3(9) . . ? C62 N61 In2 157.8(10) . . ? N61 C61 N62 110.4(13) . . ? N61 C61 S6 117.7(10) . . ? N62 C61 S6 131.9(11) . . ? C61 N62 C63 104.2(12) . . ? C61 N62 C64 129.5(12) . . ? C63 N62 C64 125.7(12) . . ? C63 C62 N61 110.4(12) . . ? C62 C63 N62 108.8(13) . . ? N62 C64 C67 111.6(15) . . ? N62 C64 C66 110.5(14) . . ? C67 C64 C66 109.8(18) . . ? N62 C64 C65 108.7(14) . . ? C67 C64 C65 107.5(17) . . ? C66 C64 C65 108.7(15) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.706 _refine_diff_density_min -2.052 _refine_diff_density_rms 0.248 # Attachment '- BmButTlMe2 (ky305s10).cif' data_ky305s10 _database_code_depnum_ccdc_archive 'CCDC 776958' #TrackingRef '- BmButTlMe2 (ky305s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H33 B N5 S2 Tl' _chemical_formula_weight 598.79 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.2742(6) _cell_length_b 13.6250(6) _cell_length_c 25.4330(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4946.4(4) _cell_formula_units_Z 8 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9665 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 32.36 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 6.711 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4534 _exptl_absorpt_correction_T_max 0.7751 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81600 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 32.44 _reflns_number_total 8825 _reflns_number_gt 6259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0176P)^2^+7.6322P] 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 8825 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Tl Tl 0.563720(7) 0.313454(7) 0.227585(4) 0.02086(3) Uani 1 1 d . . . S1 S 0.39376(5) 0.41209(5) 0.20885(3) 0.02076(13) Uani 1 1 d . . . S2 S 0.14279(5) 0.29476(5) 0.37231(3) 0.02362(14) Uani 1 1 d . . . B B 0.3546(2) 0.2896(2) 0.31863(13) 0.0223(6) Uani 1 1 d . . . H1 H 0.431(2) 0.307(2) 0.3132(13) 0.027 Uiso 1 1 d . . . H2 H 0.342(2) 0.223(2) 0.3445(12) 0.027 Uiso 1 1 d . . . C1 C 0.5111(2) 0.1656(2) 0.22606(15) 0.0308(7) Uani 1 1 d . . . H1A H 0.5628 0.1197 0.2322 0.046 Uiso 1 1 calc R . . H1B H 0.4828 0.1523 0.1917 0.046 Uiso 1 1 calc R . . H1C H 0.4638 0.1575 0.2536 0.046 Uiso 1 1 calc R . . C2 C 0.6306(2) 0.4477(2) 0.24963(14) 0.0279(6) Uani 1 1 d . . . H2A H 0.6961 0.4346 0.2589 0.042 Uiso 1 1 calc R . . H2B H 0.5982 0.4761 0.2800 0.042 Uiso 1 1 calc R . . H2C H 0.6283 0.4939 0.2201 0.042 Uiso 1 1 calc R . . C11 C 0.32514(18) 0.3091(2) 0.21700(10) 0.0186(5) Uani 1 1 d . . . N11 N 0.31152(16) 0.26411(16) 0.26377(9) 0.0187(5) Uani 1 1 d . . . N12 N 0.27768(16) 0.25716(17) 0.17936(10) 0.0216(5) Uani 1 1 d . . . C12 C 0.2566(2) 0.1819(2) 0.25517(12) 0.0244(6) Uani 1 1 d . . . H12A H 0.2369 0.1363 0.2812 0.029 Uiso 1 1 calc R . . C13 C 0.2358(2) 0.1775(2) 0.20360(12) 0.0260(6) Uani 1 1 d . . . H13A H 0.1989 0.1286 0.1869 0.031 Uiso 1 1 calc R . . C14 C 0.2730(2) 0.2796(2) 0.12151(12) 0.0305(7) Uani 1 1 d . . . C15 C 0.3708(3) 0.2705(3) 0.09820(13) 0.0378(8) Uani 1 1 d . . . H15A H 0.4123 0.3190 0.1145 0.057 Uiso 1 1 calc R . . H15B H 0.3680 0.2821 0.0602 0.057 Uiso 1 1 calc R . . H15C H 0.3952 0.2044 0.1048 0.057 Uiso 1 1 calc R . . C16 C 0.2087(3) 0.2046(3) 0.09525(15) 0.0449(9) Uani 1 1 d . . . H16A H 0.1454 0.2103 0.1099 0.067 Uiso 1 1 calc R . . H16B H 0.2327 0.1383 0.1017 0.067 Uiso 1 1 calc R . . H16C H 0.2066 0.2170 0.0573 0.067 Uiso 1 1 calc R . . C17 C 0.2313(3) 0.3817(3) 0.11396(13) 0.0405(9) Uani 1 1 d . . . H17A H 0.2720 0.4305 0.1307 0.061 Uiso 1 1 calc R . . H17B H 0.1690 0.3842 0.1300 0.061 Uiso 1 1 calc R . . H17C H 0.2262 0.3959 0.0763 0.061 Uiso 1 1 calc R . . C21 C 0.2261(2) 0.3867(2) 0.37089(11) 0.0194(5) Uani 1 1 d . . . N21 N 0.30789(16) 0.38120(17) 0.34463(9) 0.0195(5) Uani 1 1 d . . . N22 N 0.22087(17) 0.47703(17) 0.39436(9) 0.0197(5) Uani 1 1 d . . . C22 C 0.3536(2) 0.4697(2) 0.35034(11) 0.0244(6) Uani 1 1 d . . . H22A H 0.4124 0.4862 0.3353 0.029 Uiso 1 1 calc R . . C23 C 0.3009(2) 0.5288(2) 0.38086(11) 0.0251(6) Uani 1 1 d . . . H23A H 0.3159 0.5939 0.3912 0.030 Uiso 1 1 calc R . . C24 C 0.1449(2) 0.5152(2) 0.42972(11) 0.0239(6) Uani 1 1 d . . . C25 C 0.1302(3) 0.4439(3) 0.47555(12) 0.0345(7) Uani 1 1 d . . . H25A H 0.1097 0.3801 0.4619 0.052 Uiso 1 1 calc R . . H25B H 0.0823 0.4701 0.4993 0.052 Uiso 1 1 calc R . . H25C H 0.1892 0.4357 0.4948 0.052 Uiso 1 1 calc R . . C26 C 0.1766(3) 0.6133(2) 0.45282(12) 0.0318(7) Uani 1 1 d . . . H26A H 0.1867 0.6605 0.4243 0.048 Uiso 1 1 calc R . . H26B H 0.2352 0.6040 0.4723 0.048 Uiso 1 1 calc R . . H26C H 0.1283 0.6383 0.4767 0.048 Uiso 1 1 calc R . . C27 C 0.0557(2) 0.5297(2) 0.39751(12) 0.0293(6) Uani 1 1 d . . . H27A H 0.0358 0.4666 0.3828 0.044 Uiso 1 1 calc R . . H27B H 0.0680 0.5760 0.3688 0.044 Uiso 1 1 calc R . . H27C H 0.0062 0.5559 0.4202 0.044 Uiso 1 1 calc R . . N31 N 0.1249(3) 0.5449(3) 0.01341(18) 0.0695(12) Uani 1 1 d . . . C31 C 0.0766(3) 0.5939(4) -0.0107(2) 0.0559(11) Uani 1 1 d . . . C32 C 0.0154(4) 0.6547(4) -0.0417(2) 0.0753(15) Uani 1 1 d . . . H32A H 0.0522 0.6900 -0.0682 0.113 Uiso 1 1 calc R . . H32B H -0.0164 0.7020 -0.0189 0.113 Uiso 1 1 calc R . . H32C H -0.0313 0.6135 -0.0593 0.113 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 Tl 0.01709(5) 0.01605(4) 0.02944(5) -0.00053(4) 0.00129(5) 0.00055(4) S1 0.0188(3) 0.0179(3) 0.0255(3) 0.0025(3) 0.0007(3) -0.0001(3) S2 0.0214(3) 0.0192(3) 0.0302(4) 0.0031(3) 0.0006(3) -0.0017(3) B 0.0221(15) 0.0243(15) 0.0207(15) 0.0032(12) 0.0001(13) 0.0073(12) C1 0.0221(14) 0.0159(13) 0.054(2) 0.0017(13) 0.0058(15) -0.0018(10) C2 0.0222(14) 0.0204(13) 0.0410(18) -0.0052(13) -0.0036(13) 0.0044(11) C11 0.0179(12) 0.0158(11) 0.0220(13) -0.0024(10) -0.0012(9) 0.0022(10) N11 0.0177(10) 0.0177(10) 0.0208(12) -0.0004(8) 0.0035(9) 0.0033(9) N12 0.0218(11) 0.0202(11) 0.0229(12) -0.0027(9) -0.0012(10) -0.0023(9) C12 0.0227(13) 0.0171(12) 0.0334(15) 0.0005(12) 0.0060(11) 0.0000(11) C13 0.0236(14) 0.0214(14) 0.0330(16) -0.0030(12) 0.0020(12) -0.0040(12) C14 0.0375(18) 0.0333(16) 0.0206(15) -0.0043(12) -0.0072(13) 0.0017(14) C15 0.044(2) 0.048(2) 0.0215(16) -0.0027(15) 0.0060(14) 0.0026(17) C16 0.053(2) 0.046(2) 0.035(2) -0.0126(16) -0.0148(17) -0.0058(18) C17 0.055(2) 0.041(2) 0.0255(17) 0.0025(15) -0.0146(16) 0.0078(18) C21 0.0224(13) 0.0185(12) 0.0173(13) 0.0023(10) 0.0001(11) 0.0014(10) N21 0.0199(11) 0.0216(11) 0.0170(11) 0.0007(9) 0.0020(9) -0.0001(9) N22 0.0238(12) 0.0190(11) 0.0164(11) -0.0009(9) 0.0018(9) -0.0008(9) C22 0.0225(14) 0.0275(15) 0.0233(15) 0.0029(11) 0.0028(11) -0.0044(12) C23 0.0327(16) 0.0219(14) 0.0207(14) 0.0002(11) 0.0006(12) -0.0044(12) C24 0.0294(15) 0.0251(14) 0.0172(13) 0.0017(11) 0.0034(11) 0.0056(12) C25 0.0414(19) 0.0385(18) 0.0235(16) 0.0085(14) 0.0116(14) 0.0071(15) C26 0.046(2) 0.0279(16) 0.0215(15) -0.0059(12) 0.0010(14) 0.0067(14) C27 0.0298(16) 0.0307(15) 0.0274(15) 0.0004(12) 0.0051(13) 0.0058(13) N31 0.052(2) 0.074(3) 0.082(3) -0.006(2) -0.014(2) 0.003(2) C31 0.044(2) 0.060(3) 0.064(3) -0.008(2) -0.008(2) -0.006(2) C32 0.065(3) 0.065(3) 0.096(4) 0.009(3) -0.018(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl C2 2.138(3) . ? Tl C1 2.150(3) . ? Tl S2 2.7918(8) 6_656 ? Tl S1 2.8141(7) . ? S1 C11 1.724(3) . ? S2 C21 1.727(3) . ? S2 Tl 2.7918(8) 6_556 ? B H1 1.13(3) . ? B H2 1.14(3) . ? B N21 1.562(4) . ? B N11 1.564(4) . ? C11 N11 1.352(3) . ? C11 N12 1.369(3) . ? N11 C12 1.385(4) . ? N12 C13 1.384(4) . ? N12 C14 1.504(4) . ? C12 C13 1.346(4) . ? C14 C15 1.522(5) . ? C14 C17 1.525(5) . ? C14 C16 1.528(5) . ? C21 N21 1.348(4) . ? C21 N22 1.369(3) . ? N21 C22 1.378(4) . ? N22 C23 1.386(4) . ? N22 C24 1.501(4) . ? C22 C23 1.348(4) . ? C24 C27 1.527(4) . ? C24 C26 1.528(4) . ? C24 C25 1.532(4) . ? N31 C31 1.140(6) . ? C31 C32 1.439(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Tl C1 164.18(13) . . ? C2 Tl S2 97.82(9) . 6_656 ? C1 Tl S2 92.25(10) . 6_656 ? C2 Tl S1 91.21(8) . . ? C1 Tl S1 98.24(9) . . ? S2 Tl S1 103.77(2) 6_656 . ? C11 S1 Tl 94.62(9) . . ? C21 S2 Tl 101.13(9) . 6_556 ? H1 B H2 113(2) . . ? H1 B N21 107.0(16) . . ? H2 B N21 109.2(16) . . ? H1 B N11 108.6(17) . . ? H2 B N11 106.0(16) . . ? N21 B N11 112.8(2) . . ? N11 C11 N12 108.1(2) . . ? N11 C11 S1 123.8(2) . . ? N12 C11 S1 128.1(2) . . ? C11 N11 C12 108.0(2) . . ? C11 N11 B 128.9(2) . . ? C12 N11 B 122.9(2) . . ? C11 N12 C13 107.9(2) . . ? C11 N12 C14 126.9(2) . . ? C13 N12 C14 125.2(2) . . ? C13 C12 N11 108.3(3) . . ? C12 C13 N12 107.7(3) . . ? N12 C14 C15 108.9(3) . . ? N12 C14 C17 109.0(3) . . ? C15 C14 C17 112.5(3) . . ? N12 C14 C16 108.6(3) . . ? C15 C14 C16 109.1(3) . . ? C17 C14 C16 108.7(3) . . ? N21 C21 N22 108.2(2) . . ? N21 C21 S2 124.5(2) . . ? N22 C21 S2 127.3(2) . . ? C21 N21 C22 108.0(2) . . ? C21 N21 B 128.6(2) . . ? C22 N21 B 122.8(2) . . ? C21 N22 C23 107.7(2) . . ? C21 N22 C24 127.7(2) . . ? C23 N22 C24 124.6(2) . . ? C23 C22 N21 108.6(3) . . ? C22 C23 N22 107.4(3) . . ? N22 C24 C27 109.0(2) . . ? N22 C24 C26 108.6(3) . . ? C27 C24 C26 109.9(2) . . ? N22 C24 C25 109.6(2) . . ? C27 C24 C25 112.1(3) . . ? C26 C24 C25 107.6(3) . . ? N31 C31 C32 179.1(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 32.44 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.207 _refine_diff_density_min -1.511 _refine_diff_density_rms 0.130 # Attachment '- BmGaBr2 (ky290s10).cif' data_ky290s10 _database_code_depnum_ccdc_archive 'CCDC 776959' #TrackingRef '- BmGaBr2 (ky290s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 B Br2 Ga N4 S2' _chemical_formula_weight 552.84 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.5227(5) _cell_length_b 12.6478(5) _cell_length_c 28.7910(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4195.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9842 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 31.49 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 5.324 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3495 _exptl_absorpt_correction_T_max 0.6181 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 67705 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 31.51 _reflns_number_total 6981 _reflns_number_gt 5908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to 1.1 angstroms. ; _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^)+(0.0252P)^2^+3.1245P] 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 6981 _refine_ls_number_parameters 223 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Ga Ga 0.965555(16) -0.026044(15) 0.625836(7) 0.01429(4) Uani 1 1 d . . . Br1 Br 0.841721(17) 0.117196(15) 0.617658(7) 0.02305(5) Uani 1 1 d . . . Br2 Br 0.871598(15) -0.174461(14) 0.655363(6) 0.01800(4) Uani 1 1 d . . . S1 S 1.10270(4) 0.02590(3) 0.678109(16) 0.01673(8) Uani 1 1 d . . . S2 S 1.04723(4) -0.06912(4) 0.556228(16) 0.01841(9) Uani 1 1 d . . . B B 1.22938(17) -0.18820(17) 0.63090(7) 0.0171(4) Uani 1 1 d D . . H1 H 1.3019(17) -0.2444(16) 0.6327(8) 0.021 Uiso 1 1 d D . . H2 H 1.250(2) -0.1105(13) 0.6164(7) 0.021 Uiso 1 1 d D . . N11 N 1.18126(12) -0.17870(12) 0.68203(5) 0.0143(3) Uani 1 1 d . . . C11 C 1.12906(14) -0.09662(13) 0.70354(6) 0.0135(3) Uani 1 1 d . . . N12 N 1.10362(12) -0.12457(12) 0.74795(5) 0.0147(3) Uani 1 1 d . . . C12 C 1.18891(16) -0.25992(14) 0.71378(6) 0.0177(3) Uani 1 1 d . . . H12A H 1.2219 -0.3275 0.7081 0.021 Uiso 1 1 calc R . . C13 C 1.14153(16) -0.22752(14) 0.75451(6) 0.0177(3) Uani 1 1 d . . . H13A H 1.1355 -0.2678 0.7823 0.021 Uiso 1 1 calc R . . C14 C 1.04223(15) -0.05929(15) 0.78465(6) 0.0174(3) Uani 1 1 d . . . C15 C 1.11203(18) 0.04103(16) 0.79399(7) 0.0252(4) Uani 1 1 d . . . H15A H 1.1187 0.0821 0.7653 0.038 Uiso 1 1 calc R . . H15B H 1.1897 0.0219 0.8051 0.038 Uiso 1 1 calc R . . H15C H 1.0725 0.0835 0.8177 0.038 Uiso 1 1 calc R . . C16 C 0.91900(16) -0.03544(16) 0.76827(7) 0.0214(4) Uani 1 1 d . . . H16A H 0.8788 -0.1019 0.7613 0.032 Uiso 1 1 calc R . . H16B H 0.9220 0.0085 0.7403 0.032 Uiso 1 1 calc R . . H16C H 0.8770 0.0024 0.7928 0.032 Uiso 1 1 calc R . . C17 C 1.03596(19) -0.12442(18) 0.82920(7) 0.0259(4) Uani 1 1 d . . . H17A H 0.9842 -0.1849 0.8245 0.039 Uiso 1 1 calc R . . H17B H 1.0060 -0.0803 0.8545 0.039 Uiso 1 1 calc R . . H17C H 1.1137 -0.1499 0.8373 0.039 Uiso 1 1 calc R . . N21 N 1.13574(13) -0.24480(12) 0.59955(5) 0.0160(3) Uani 1 1 d . . . C21 C 1.05967(15) -0.20351(14) 0.56874(6) 0.0159(3) Uani 1 1 d . . . N22 N 0.99490(14) -0.28277(13) 0.55018(5) 0.0185(3) Uani 1 1 d . . . C22 C 1.11727(18) -0.35268(15) 0.60064(7) 0.0213(4) Uani 1 1 d . . . H22A H 1.1582 -0.4020 0.6194 0.026 Uiso 1 1 calc R . . C23 C 1.03122(18) -0.37601(16) 0.57059(7) 0.0226(4) Uani 1 1 d . . . H23A H 1.0009 -0.4445 0.5645 0.027 Uiso 1 1 calc R . . C24 C 0.90668(17) -0.27511(18) 0.51113(7) 0.0234(4) Uani 1 1 d . . . C25 C 0.80800(17) -0.20010(18) 0.52412(8) 0.0262(4) Uani 1 1 d . . . H25A H 0.8396 -0.1295 0.5302 0.039 Uiso 1 1 calc R . . H25B H 0.7689 -0.2263 0.5521 0.039 Uiso 1 1 calc R . . H25C H 0.7522 -0.1964 0.4985 0.039 Uiso 1 1 calc R . . C26 C 0.85545(19) -0.38486(19) 0.50307(9) 0.0334(5) Uani 1 1 d . . . H26A H 0.7983 -0.3815 0.4779 0.050 Uiso 1 1 calc R . . H26B H 0.8176 -0.4095 0.5316 0.050 Uiso 1 1 calc R . . H26C H 0.9176 -0.4341 0.4945 0.050 Uiso 1 1 calc R . . C27 C 0.97060(19) -0.2381(2) 0.46763(7) 0.0339(5) Uani 1 1 d . . . H27A H 1.0024 -0.1672 0.4729 0.051 Uiso 1 1 calc R . . H27B H 0.9165 -0.2360 0.4414 0.051 Uiso 1 1 calc R . . H27C H 1.0340 -0.2872 0.4606 0.051 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 Ga 0.01312(8) 0.01385(9) 0.01590(9) 0.00208(7) -0.00003(7) 0.00080(7) Br1 0.02364(9) 0.02182(9) 0.02368(10) 0.00556(7) 0.00246(7) 0.00988(7) Br2 0.01733(8) 0.01705(8) 0.01961(9) 0.00082(7) 0.00178(6) -0.00426(6) S1 0.01756(19) 0.01257(18) 0.0201(2) 0.00090(16) -0.00238(16) -0.00233(15) S2 0.0186(2) 0.0210(2) 0.0156(2) 0.00414(16) 0.00145(16) 0.00166(16) B 0.0132(8) 0.0223(9) 0.0159(9) -0.0016(7) 0.0000(7) 0.0008(7) N11 0.0123(6) 0.0152(6) 0.0155(7) -0.0010(5) -0.0015(5) 0.0008(5) C11 0.0110(7) 0.0137(7) 0.0159(8) 0.0002(6) -0.0014(6) -0.0007(6) N12 0.0136(6) 0.0150(6) 0.0153(7) 0.0001(5) -0.0002(5) 0.0007(5) C12 0.0188(8) 0.0154(7) 0.0190(8) 0.0001(7) -0.0020(7) 0.0035(6) C13 0.0198(8) 0.0166(8) 0.0168(8) 0.0020(6) -0.0004(7) 0.0023(6) C14 0.0149(8) 0.0198(8) 0.0175(8) -0.0030(7) 0.0013(6) 0.0021(6) C15 0.0243(9) 0.0279(10) 0.0235(10) -0.0105(8) 0.0008(7) -0.0049(8) C16 0.0143(8) 0.0260(9) 0.0239(9) -0.0032(8) 0.0015(7) 0.0041(7) C17 0.0270(10) 0.0334(11) 0.0173(9) 0.0018(8) 0.0051(7) 0.0061(8) N21 0.0156(7) 0.0191(7) 0.0134(7) -0.0016(6) 0.0001(5) 0.0023(6) C21 0.0146(7) 0.0195(8) 0.0136(8) -0.0009(6) 0.0015(6) 0.0017(6) N22 0.0173(7) 0.0238(8) 0.0143(7) -0.0036(6) -0.0005(6) -0.0005(6) C22 0.0284(10) 0.0171(8) 0.0183(9) -0.0024(7) -0.0007(7) 0.0031(7) C23 0.0296(10) 0.0185(8) 0.0196(9) -0.0032(7) -0.0002(8) -0.0012(7) C24 0.0164(8) 0.0381(11) 0.0157(9) -0.0036(8) -0.0020(7) -0.0023(8) C25 0.0166(8) 0.0370(11) 0.0252(10) 0.0006(8) -0.0026(7) 0.0002(8) C26 0.0267(10) 0.0407(13) 0.0329(12) -0.0158(10) -0.0060(9) -0.0037(9) C27 0.0234(10) 0.0630(16) 0.0152(9) -0.0003(10) -0.0009(8) -0.0044(10) _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 Ga S1 2.2790(5) . ? Ga S2 2.2801(5) . ? Ga Br1 2.3181(3) . ? Ga Br2 2.3278(3) . ? S1 C11 1.7406(17) . ? S2 C21 1.7434(19) . ? B H2 1.094(15) . ? B H1 1.098(15) . ? B N11 1.578(3) . ? B N21 1.578(3) . ? N11 C11 1.350(2) . ? N11 C12 1.378(2) . ? C11 N12 1.358(2) . ? N12 C13 1.386(2) . ? N12 C14 1.516(2) . ? C12 C13 1.357(3) . ? C14 C15 1.526(3) . ? C14 C17 1.526(3) . ? C14 C16 1.526(3) . ? N21 C21 1.352(2) . ? N21 C22 1.381(2) . ? C21 N22 1.359(2) . ? N22 C23 1.382(3) . ? N22 C24 1.519(2) . ? C22 C23 1.349(3) . ? C24 C26 1.526(3) . ? C24 C27 1.527(3) . ? C24 C25 1.527(3) . ? 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 Ga S2 111.289(19) . . ? S1 Ga Br1 105.582(14) . . ? S2 Ga Br1 110.581(15) . . ? S1 Ga Br2 108.288(14) . . ? S2 Ga Br2 108.680(15) . . ? Br1 Ga Br2 112.398(11) . . ? C11 S1 Ga 98.17(6) . . ? C21 S2 Ga 94.89(6) . . ? H2 B H1 115.8(17) . . ? H2 B N11 111.4(11) . . ? H1 B N11 105.8(12) . . ? H2 B N21 109.7(12) . . ? H1 B N21 104.7(12) . . ? N11 B N21 109.13(14) . . ? C11 N11 C12 107.30(15) . . ? C11 N11 B 130.02(15) . . ? C12 N11 B 122.67(15) . . ? N11 C11 N12 109.14(15) . . ? N11 C11 S1 124.70(13) . . ? N12 C11 S1 126.15(13) . . ? C11 N12 C13 107.74(14) . . ? C11 N12 C14 127.95(15) . . ? C13 N12 C14 124.30(15) . . ? C13 C12 N11 108.81(16) . . ? C12 C13 N12 107.01(16) . . ? N12 C14 C15 109.25(15) . . ? N12 C14 C17 108.30(15) . . ? C15 C14 C17 109.00(16) . . ? N12 C14 C16 109.05(15) . . ? C15 C14 C16 112.36(16) . . ? C17 C14 C16 108.80(16) . . ? C21 N21 C22 107.25(15) . . ? C21 N21 B 130.03(16) . . ? C22 N21 B 122.71(15) . . ? N21 C21 N22 109.21(16) . . ? N21 C21 S2 124.43(14) . . ? N22 C21 S2 126.35(14) . . ? C21 N22 C23 107.21(15) . . ? C21 N22 C24 127.69(16) . . ? C23 N22 C24 124.87(16) . . ? C23 C22 N21 108.35(17) . . ? C22 C23 N22 107.98(17) . . ? N22 C24 C26 108.26(17) . . ? N22 C24 C27 107.70(15) . . ? C26 C24 C27 109.93(18) . . ? N22 C24 C25 110.89(16) . . ? C26 C24 C25 108.32(17) . . ? C27 C24 C25 111.69(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.820 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.092 # Attachment '- BmMeAlCl2 (ky142s10).cif' data_ky142s10 _database_code_depnum_ccdc_archive 'CCDC 776960' #TrackingRef '- BmMeAlCl2 (ky142s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 Al B Cl2 N4 S2' _chemical_formula_weight 337.03 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.3215(5) _cell_length_b 13.0872(9) _cell_length_c 13.3622(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1455.21(17) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9095 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 32.67 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8598 _exptl_absorpt_correction_T_max 0.8921 _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_reflns_number 19240 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0088 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1884 _reflns_number_gt 1795 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to be 1.1 angstroms. ; _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^)+(0.0381P)^2^+0.6790P] 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 1884 _refine_ls_number_parameters 92 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0227 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Al Al -0.28551(6) 0.2500 1.57654(3) 0.01445(12) Uani 1 2 d S . . Cl1 Cl -0.46536(5) 0.2500 1.46254(3) 0.02176(11) Uani 1 2 d S . . Cl2 Cl -0.38049(5) 0.2500 1.72465(3) 0.02253(11) Uani 1 2 d S . . S S -0.14216(3) 0.10459(2) 1.56340(2) 0.01849(9) Uani 1 1 d . . . B B 0.0656(2) 0.2500 1.39695(14) 0.0176(3) Uani 1 2 d SD . . H11 H 0.169(2) 0.2500 1.3441(14) 0.021 Uiso 1 2 d SD . . H12 H 0.098(3) 0.2500 1.4768(12) 0.021 Uiso 1 2 d SD . . N1 N -0.03892(11) 0.15310(7) 1.37208(7) 0.01620(19) Uani 1 1 d . . . C1 C -0.12818(13) 0.09499(8) 1.43355(8) 0.0157(2) Uani 1 1 d . . . N2 N -0.20208(12) 0.02206(7) 1.37914(7) 0.0185(2) Uani 1 1 d . . . C2 C -0.05787(15) 0.11482(9) 1.27630(8) 0.0207(2) Uani 1 1 d . . . H2 H -0.0087 0.1412 1.2175 0.025 Uiso 1 1 calc R . . C3 C -0.15822(15) 0.03352(9) 1.28041(9) 0.0220(2) Uani 1 1 d . . . H3 H -0.1919 -0.0077 1.2258 0.026 Uiso 1 1 calc R . . C4 C -0.30549(16) -0.05931(10) 1.41749(10) 0.0264(3) Uani 1 1 d . . . H4B H -0.3517 -0.0974 1.3613 0.040 Uiso 1 1 calc R . . H4A H -0.3921 -0.0294 1.4576 0.040 Uiso 1 1 calc R . . H4C H -0.2419 -0.1057 1.4593 0.040 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 Al 0.0167(2) 0.0134(2) 0.0133(2) 0.000 0.00070(16) 0.000 Cl1 0.0217(2) 0.0244(2) 0.01919(19) 0.000 -0.00517(14) 0.000 Cl2 0.0294(2) 0.0227(2) 0.01549(18) 0.000 0.00610(14) 0.000 S 0.02381(16) 0.01539(15) 0.01628(15) 0.00295(9) 0.00293(10) 0.00418(10) B 0.0169(7) 0.0136(7) 0.0222(8) 0.000 0.0007(7) 0.000 N1 0.0189(4) 0.0135(4) 0.0162(4) -0.0003(3) 0.0014(3) 0.0017(3) C1 0.0162(5) 0.0128(5) 0.0181(5) 0.0001(4) 0.0009(4) 0.0030(4) N2 0.0178(4) 0.0144(4) 0.0232(5) -0.0018(4) 0.0000(4) 0.0006(3) C2 0.0278(6) 0.0182(5) 0.0160(5) -0.0014(4) 0.0006(4) 0.0026(4) C3 0.0262(6) 0.0192(5) 0.0207(5) -0.0039(4) -0.0033(4) 0.0021(5) C4 0.0236(6) 0.0183(5) 0.0372(7) -0.0013(5) 0.0027(5) -0.0057(5) _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 Al Cl2 2.1311(6) . ? Al Cl1 2.1355(6) . ? Al S 2.2528(4) 7_565 ? Al S 2.2528(4) . ? S C1 1.7435(11) . ? B H12 1.100(15) . ? B H11 1.113(15) . ? B N1 1.5733(14) . ? B N1 1.5733(14) 7_565 ? N1 C1 1.3434(14) . ? N1 C2 1.3834(14) . ? C1 N2 1.3483(15) . ? N2 C3 1.3770(15) . ? N2 C4 1.4618(15) . ? C2 C3 1.3536(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Al Cl1 113.74(3) . . ? Cl2 Al S 105.592(16) . 7_565 ? Cl1 Al S 108.392(16) . 7_565 ? Cl2 Al S 105.593(16) . . ? Cl1 Al S 108.391(16) . . ? S Al S 115.28(3) 7_565 . ? C1 S Al 100.01(4) . . ? H12 B H11 115.2(16) . . ? H12 B N1 109.9(6) . . ? H11 B N1 107.1(6) . . ? H12 B N1 109.9(6) . 7_565 ? H11 B N1 107.1(6) . 7_565 ? N1 B N1 107.43(13) . 7_565 ? C1 N1 C2 107.31(10) . . ? C1 N1 B 129.26(11) . . ? C2 N1 B 123.39(11) . . ? N1 C1 N2 108.86(10) . . ? N1 C1 S 127.20(9) . . ? N2 C1 S 123.86(9) . . ? C1 N2 C3 108.58(10) . . ? C1 N2 C4 126.52(10) . . ? C3 N2 C4 124.84(10) . . ? C3 C2 N1 108.51(10) . . ? C2 C3 N2 106.74(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.350 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.055 # Attachment '- BmMeGa(I)Ga(I)BmMe (ky129s10).cif' data_ky129s10 _database_code_depnum_ccdc_archive 'CCDC 776961' #TrackingRef '- BmMeGa(I)Ga(I)BmMe (ky129s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 B2 Ga2 I2 N8 S4' _chemical_formula_weight 871.53 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 12.149(3) _cell_length_b 11.964(3) _cell_length_c 11.163(3) _cell_angle_alpha 90.00 _cell_angle_beta 121.214(4) _cell_angle_gamma 90.00 _cell_volume 1387.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 2199 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 26.11 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 4.491 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6623 _exptl_absorpt_correction_T_max 0.8066 _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_reflns_number 9629 _diffrn_reflns_av_R_equivalents 0.1086 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1805 _reflns_number_gt 1205 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to be 1.1 angstroms. ; _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^)+(0.0420P)^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 1805 _refine_ls_number_parameters 86 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.015 _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 Ga Ga 0.88500(9) 0.5000 0.45055(10) 0.0160(2) Uani 1 2 d S . . I I 0.81076(6) 0.5000 0.63033(6) 0.02223(18) Uani 1 2 d S . . S S 0.78071(15) 0.34134(13) 0.32196(16) 0.0191(3) Uani 1 1 d . . . B B 0.7203(10) 0.5000 0.0406(10) 0.020(2) Uani 1 2 d SD . . H1 H 0.686(8) 0.5000 -0.072(3) 0.024 Uiso 1 2 d SD . . H2 H 0.645(6) 0.5000 0.067(9) 0.024 Uiso 1 2 d SD . . N1 N 0.8113(5) 0.3940(4) 0.0986(5) 0.0200(11) Uani 1 1 d . . . C1 C 0.8418(6) 0.3316(5) 0.2117(6) 0.0169(13) Uani 1 1 d . . . N2 N 0.9224(5) 0.2506(4) 0.2214(5) 0.0180(11) Uani 1 1 d . . . C2 C 0.8748(6) 0.3507(5) 0.0370(6) 0.0214(14) Uani 1 1 d . . . H2A H 0.8710 0.3785 -0.0447 0.026 Uiso 1 1 calc R . . C3 C 0.9433(6) 0.2617(5) 0.1130(6) 0.0211(14) Uani 1 1 d . . . H3A H 0.9963 0.2153 0.0947 0.025 Uiso 1 1 calc R . . C4 C 0.9828(6) 0.1651(5) 0.3315(6) 0.0199(13) Uani 1 1 d . . . H4A H 0.9528 0.1739 0.3973 0.030 Uiso 1 1 calc R . . H4B H 1.0765 0.1737 0.3818 0.030 Uiso 1 1 calc R . . H4C H 0.9592 0.0906 0.2889 0.030 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 Ga 0.0134(5) 0.0175(5) 0.0172(5) 0.000 0.0080(4) 0.000 I 0.0251(4) 0.0255(3) 0.0215(3) 0.000 0.0159(3) 0.000 S 0.0192(8) 0.0195(8) 0.0221(8) -0.0021(7) 0.0132(7) -0.0025(6) B 0.020(5) 0.024(5) 0.015(5) 0.000 0.008(4) 0.000 N1 0.019(3) 0.019(3) 0.017(3) -0.005(2) 0.006(2) -0.003(2) C1 0.015(3) 0.014(3) 0.018(3) -0.002(2) 0.006(3) -0.006(2) N2 0.021(3) 0.019(3) 0.013(3) -0.002(2) 0.008(2) -0.004(2) C2 0.026(4) 0.025(4) 0.019(3) -0.002(3) 0.016(3) -0.003(3) C3 0.025(3) 0.021(3) 0.020(3) -0.006(3) 0.013(3) -0.005(3) C4 0.019(3) 0.023(3) 0.019(3) 0.006(3) 0.011(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga S 2.3204(17) . ? Ga S 2.3204(17) 6_565 ? Ga Ga 2.4144(19) 5_766 ? Ga I 2.5917(12) . ? S C1 1.740(6) . ? B H2 1.10(2) . ? B H1 1.10(2) . ? B N1 1.583(8) . ? B N1 1.583(8) 6_565 ? N1 C1 1.343(7) . ? N1 C2 1.374(7) . ? C1 N2 1.341(8) . ? N2 C3 1.365(7) . ? N2 C4 1.471(7) . ? C2 C3 1.347(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 S Ga S 109.79(9) . 6_565 ? S Ga Ga 114.48(5) . 5_766 ? S Ga Ga 114.48(5) 6_565 5_766 ? S Ga I 100.45(5) . . ? S Ga I 100.45(5) 6_565 . ? Ga Ga I 115.51(6) 5_766 . ? C1 S Ga 101.3(2) . . ? H2 B H1 116(7) . . ? H2 B N1 113(2) . . ? H1 B N1 104(3) . . ? H2 B N1 113(2) . 6_565 ? H1 B N1 104(3) . 6_565 ? N1 B N1 106.4(7) . 6_565 ? C1 N1 C2 107.9(5) . . ? C1 N1 B 128.6(6) . . ? C2 N1 B 123.5(6) . . ? N2 C1 N1 108.2(5) . . ? N2 C1 S 123.6(4) . . ? N1 C1 S 128.1(5) . . ? C1 N2 C3 108.8(5) . . ? C1 N2 C4 126.7(5) . . ? C3 N2 C4 124.5(5) . . ? C3 C2 N1 107.9(5) . . ? C2 C3 N2 107.3(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.992 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.198 # Attachment '- BmMeGaI2 (fc2s10).cif' data_fc2s10 _database_code_depnum_ccdc_archive 'CCDC 776962' #TrackingRef '- BmMeGaI2 (fc2s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 B Ga I2 N4 S2' _chemical_formula_weight 562.67 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.8213(3) _cell_length_b 13.2681(5) _cell_length_c 14.3161(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1675.58(10) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 7626 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour colorless _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 2.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 5.564 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4024 _exptl_absorpt_correction_T_max 0.4024 _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_reflns_number 11074 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.10 _reflns_number_total 1935 _reflns_number_gt 1787 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to be 1.1 angstroms. ; _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^)+(0.0174P)^2^+0.7608P] 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 0.00203(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1935 _refine_ls_number_parameters 93 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0195 _refine_ls_R_factor_gt 0.0170 _refine_ls_wR_factor_ref 0.0405 _refine_ls_wR_factor_gt 0.0397 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _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 Ga Ga -0.27575(4) 0.2500 1.57726(2) 0.02810(9) Uani 1 2 d S . . I1 I -0.46952(3) 0.2500 1.445889(15) 0.04110(8) Uani 1 2 d S . . I2 I -0.39736(3) 0.2500 1.737284(14) 0.04040(8) Uani 1 2 d S . . S S -0.13719(7) 0.10519(4) 1.56574(4) 0.03772(14) Uani 1 1 d . . . B B 0.0572(5) 0.2500 1.4106(3) 0.0418(9) Uani 1 2 d SD . . H11 H 0.094(4) 0.2500 1.4839(15) 0.050 Uiso 1 2 d SD . . H12 H 0.151(3) 0.2500 1.358(2) 0.050 Uiso 1 2 d SD . . N1 N -0.0419(2) 0.15458(14) 1.38715(13) 0.0360(4) Uani 1 1 d . . . C1 C -0.1253(2) 0.09707(16) 1.44482(15) 0.0317(5) Uani 1 1 d . . . N2 N -0.1988(2) 0.02691(14) 1.39381(13) 0.0383(4) Uani 1 1 d . . . C2 C -0.0647(3) 0.11823(19) 1.29807(18) 0.0492(6) Uani 1 1 d . . . H2 H -0.0201 0.1441 1.2434 0.059 Uiso 1 1 calc R . . C3 C -0.1609(3) 0.03999(19) 1.30194(18) 0.0514(7) Uani 1 1 d . . . H3 H -0.1956 0.0015 1.2512 0.062 Uiso 1 1 calc R . . C4 C -0.2990(3) -0.0519(2) 1.4301(2) 0.0550(7) Uani 1 1 d . . . H4B H -0.3436 -0.0886 1.3784 0.082 Uiso 1 1 calc R . . H4A H -0.3787 -0.0213 1.4671 0.082 Uiso 1 1 calc R . . H4C H -0.2410 -0.0979 1.4687 0.082 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 Ga 0.03108(17) 0.02802(17) 0.02519(16) 0.000 0.00185(12) 0.000 I1 0.04196(13) 0.04576(14) 0.03557(12) 0.000 -0.01019(9) 0.000 I2 0.04698(14) 0.04418(13) 0.03004(11) 0.000 0.01066(8) 0.000 S 0.0464(3) 0.0341(3) 0.0327(3) 0.0053(2) 0.0031(2) 0.0102(2) B 0.038(2) 0.039(2) 0.049(2) 0.000 0.0091(17) 0.000 N1 0.0431(10) 0.0288(9) 0.0362(10) 0.0000(8) 0.0077(8) 0.0050(8) C1 0.0339(11) 0.0251(10) 0.0361(11) 0.0009(8) 0.0031(8) 0.0080(8) N2 0.0422(11) 0.0286(9) 0.0442(11) -0.0045(8) 0.0018(9) 0.0025(8) C2 0.0756(18) 0.0365(13) 0.0355(12) -0.0006(10) 0.0092(12) 0.0049(12) C3 0.0732(18) 0.0386(14) 0.0422(13) -0.0111(11) -0.0029(13) 0.0060(13) C4 0.0552(16) 0.0383(14) 0.0715(18) -0.0069(13) 0.0098(14) -0.0072(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 Ga S 2.2832(6) . ? Ga S 2.2832(6) 7_565 ? Ga I2 2.5296(4) . ? Ga I1 2.5414(4) . ? S C1 1.738(2) . ? B H11 1.097(18) . ? B H12 1.116(18) . ? B N1 1.575(3) 7_565 ? B N1 1.575(3) . ? N1 C1 1.343(3) . ? N1 C2 1.378(3) . ? C1 N2 1.349(3) . ? N2 C3 1.368(3) . ? N2 C4 1.464(3) . ? C2 C3 1.342(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 S Ga S 114.61(4) . 7_565 ? S Ga I2 107.005(16) . . ? S Ga I2 107.004(16) 7_565 . ? S Ga I1 107.854(18) . . ? S Ga I1 107.854(18) 7_565 . ? I2 Ga I1 112.644(15) . . ? C1 S Ga 99.01(7) . . ? H11 B H12 115(3) . . ? H11 B N1 111.5(10) . 7_565 ? H12 B N1 105.5(11) . 7_565 ? H11 B N1 111.5(10) . . ? H12 B N1 105.5(11) . . ? N1 B N1 107.0(3) 7_565 . ? C1 N1 C2 106.9(2) . . ? C1 N1 B 129.0(2) . . ? C2 N1 B 124.0(2) . . ? N1 C1 N2 108.81(19) . . ? N1 C1 S 127.60(18) . . ? N2 C1 S 123.56(17) . . ? C1 N2 C3 108.4(2) . . ? C1 N2 C4 126.2(2) . . ? C3 N2 C4 125.4(2) . . ? C3 C2 N1 109.0(2) . . ? C2 C3 N2 107.0(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.443 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.068 # Attachment '- BmMeInI2 (fc1s10).cif' data_fc1s10 _database_code_depnum_ccdc_archive 'CCDC 776963' #TrackingRef '- BmMeInI2 (fc1s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 B I2 In N4 S2' _chemical_formula_weight 607.77 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.9426(7) _cell_length_b 13.3473(11) _cell_length_c 14.5746(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1739.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 7925 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour colorless _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 2.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 5.136 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4265 _exptl_absorpt_correction_T_max 0.4265 _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_reflns_number 11492 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.10 _reflns_number_total 2003 _reflns_number_gt 1826 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The B-H bonds have been restrained to be 1.1 angstroms. ; _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^)+(0.0189P)^2^+0.9849P] 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 0.00182(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2003 _refine_ls_number_parameters 93 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0169 _refine_ls_wR_factor_ref 0.0420 _refine_ls_wR_factor_gt 0.0409 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 -0.28228(3) 0.2500 1.581357(14) 0.03078(7) Uani 1 2 d S . . I1 I -0.47935(3) 0.2500 1.440673(16) 0.04769(8) Uani 1 2 d S . . I2 I -0.41558(3) 0.2500 1.746746(15) 0.04539(8) Uani 1 2 d S . . S1 S -0.13340(8) 0.09610(5) 1.56300(4) 0.04192(15) Uani 1 1 d . . . B B 0.0420(5) 0.2500 1.4092(3) 0.0455(10) Uani 1 2 d SD . . H11 H 0.075(4) 0.2500 1.4816(15) 0.055 Uiso 1 2 d SD . . H12 H 0.136(3) 0.2500 1.360(2) 0.055 Uiso 1 2 d SD . . N1 N -0.0558(2) 0.15479(15) 1.38690(15) 0.0408(5) Uani 1 1 d . . . N2 N -0.2051(2) 0.02472(16) 1.39354(15) 0.0437(5) Uani 1 1 d . . . C1 C -0.1318(3) 0.09387(18) 1.44380(16) 0.0356(5) Uani 1 1 d . . . C2 C -0.0828(4) 0.1212(2) 1.29925(19) 0.0588(8) Uani 1 1 d . . . H2 H -0.0435 0.1493 1.2453 0.071 Uiso 1 1 calc R . . C3 C -0.1743(4) 0.0417(2) 1.3033(2) 0.0592(8) Uani 1 1 d . . . H3 H -0.2105 0.0046 1.2532 0.071 Uiso 1 1 calc R . . C4 C -0.2979(4) -0.0563(2) 1.4299(2) 0.0603(8) Uani 1 1 d . . . H4B H -0.3427 -0.0931 1.3795 0.091 Uiso 1 1 calc R . . H4A H -0.3762 -0.0283 1.4682 0.091 Uiso 1 1 calc R . . H4C H -0.2365 -0.1012 1.4662 0.091 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 0.03571(12) 0.03081(13) 0.02583(11) 0.000 0.00285(9) 0.000 I1 0.05022(15) 0.05559(16) 0.03727(13) 0.000 -0.01207(10) 0.000 I2 0.04906(15) 0.05537(16) 0.03174(12) 0.000 0.01178(9) 0.000 S1 0.0537(4) 0.0369(3) 0.0353(3) 0.0046(2) 0.0021(3) 0.0119(3) B 0.045(2) 0.038(2) 0.054(3) 0.000 0.0136(19) 0.000 N1 0.0535(12) 0.0306(11) 0.0382(10) 0.0001(8) 0.0086(9) 0.0043(9) N2 0.0508(13) 0.0322(11) 0.0482(12) -0.0065(9) 0.0026(10) 0.0013(9) C1 0.0404(12) 0.0293(12) 0.0371(12) -0.0010(9) 0.0040(10) 0.0081(10) C2 0.097(2) 0.0415(16) 0.0374(14) -0.0026(11) 0.0121(15) 0.0079(16) C3 0.093(2) 0.0410(16) 0.0438(15) -0.0114(12) -0.0043(15) 0.0042(15) C4 0.0583(18) 0.0418(16) 0.081(2) -0.0077(15) 0.0094(16) -0.0097(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 In S1 2.4624(7) 7_565 ? In S1 2.4624(7) . ? In I2 2.6891(3) . ? In I1 2.7037(4) . ? S1 C1 1.738(2) . ? B H11 1.096(19) . ? B H12 1.101(19) . ? B N1 1.577(4) 7_565 ? B N1 1.577(4) . ? N1 C1 1.345(3) . ? N1 C2 1.375(3) . ? N2 C1 1.349(3) . ? N2 C3 1.363(4) . ? N2 C4 1.463(4) . ? C2 C3 1.341(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 S1 In S1 113.07(4) 7_565 . ? S1 In I2 109.698(16) 7_565 . ? S1 In I2 109.698(16) . . ? S1 In I1 105.664(17) 7_565 . ? S1 In I1 105.664(17) . . ? I2 In I1 113.007(13) . . ? C1 S1 In 97.33(8) . . ? H11 B H12 114(3) . . ? H11 B N1 110.5(11) . 7_565 ? H12 B N1 106.8(12) . 7_565 ? H11 B N1 110.5(11) . . ? H12 B N1 106.8(12) . . ? N1 B N1 107.4(3) 7_565 . ? C1 N1 C2 106.7(2) . . ? C1 N1 B 129.8(3) . . ? C2 N1 B 123.5(3) . . ? C1 N2 C3 108.2(2) . . ? C1 N2 C4 125.8(2) . . ? C3 N2 C4 126.0(3) . . ? N1 C1 N2 108.9(2) . . ? N1 C1 S1 127.6(2) . . ? N2 C1 S1 123.41(19) . . ? C3 C2 N1 108.9(3) . . ? C2 C3 N2 107.3(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.559 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.072