# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Chemical Sciences' _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Gerard Parkin' _publ_contact_author_email PARKIN@COLUMBIA.EDU _publ_section_title ; Tris(2-mercapto-1-t-butylimidazolyl) hydroborato Gallium Derivatives: Synthesis of Di- and Trigallium Compounds in a Sulfur-Rich Coordination Environment ; _publ_author_name 'Gerard Parkin' # Attachment '- TmGaGaCl3 (148s20).cif' data_148s20 _database_code_depnum_ccdc_archive 'CCDC 763457' #TrackingRef '- TmGaGaCl3 (148s20).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H34 B Cl3 Ga2 N6 S3' _chemical_formula_weight 723.32 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 Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 15.7834(8) _cell_length_b 15.7834(8) _cell_length_c 21.1015(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4552.4(4) _cell_formula_units_Z 6 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 7275 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 31.98 _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 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 2.269 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.8049 _exptl_absorpt_correction_T_max 0.8950 _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 22482 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 32.71 _reflns_number_total 3530 _reflns_number_gt 2011 _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^)+(0.0191P)^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 3530 _refine_ls_number_parameters 220 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.139 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.6667 0.3333 0.03191(3) 0.01849(17) Uani 0.4949(6) 3 d SP . 1 Ga2 Ga 0.6667 0.3333 -0.08229(3) 0.02102(18) Uani 0.4949(6) 3 d SP . 1 S1 S 0.6287(3) 0.4439(4) 0.0809(3) 0.0226(6) Uani 0.4949(6) 1 d P . 1 Cl1 Cl 0.77012(7) 0.47847(7) -0.12297(4) 0.0337(2) Uani 0.4949(6) 1 d P . 1 B1 B 0.6667 0.3333 0.2097(3) 0.0177(14) Uani 0.4949(6) 3 d SPD . 1 H1 H 0.6667 0.3333 0.2624(10) 0.021 Uiso 0.4949(6) 3 d SPD . 1 C11 C 0.5497(3) 0.3717(2) 0.13768(15) 0.0202(7) Uani 0.4949(6) 1 d P . 1 N11 N 0.5735(2) 0.3371(2) 0.18893(12) 0.0210(6) Uani 0.4949(6) 1 d P . 1 N12 N 0.4531(2) 0.3437(2) 0.14145(15) 0.0227(7) Uani 0.4949(6) 1 d P . 1 C12 C 0.4908(3) 0.2890(3) 0.22609(16) 0.0255(8) Uani 0.4949(6) 1 d P . 1 H12A H 0.4868 0.2585 0.2657 0.031 Uiso 0.4949(6) 1 calc PR . 1 C13 C 0.4170(3) 0.2924(3) 0.19708(16) 0.0266(8) Uani 0.4949(6) 1 d P . 1 H13A H 0.3517 0.2646 0.2121 0.032 Uiso 0.4949(6) 1 calc PR . 1 C14 C 0.3923(17) 0.3552(15) 0.0924(9) 0.023(2) Uani 0.4949(6) 1 d P . 1 C15 C 0.4342(11) 0.4678(9) 0.0821(8) 0.041(5) Uani 0.4949(6) 1 d P . 1 H15A H 0.5007 0.4973 0.0650 0.062 Uiso 0.4949(6) 1 calc PR . 1 H15B H 0.4357 0.4987 0.1227 0.062 Uiso 0.4949(6) 1 calc PR . 1 H15C H 0.3924 0.4777 0.0522 0.062 Uiso 0.4949(6) 1 calc PR . 1 C16 C 0.2860(3) 0.3114(3) 0.1167(2) 0.0355(10) Uani 0.4949(6) 1 d P . 1 H16A H 0.2458 0.3182 0.0839 0.053 Uiso 0.4949(6) 1 calc PR . 1 H16B H 0.2855 0.3463 0.1550 0.053 Uiso 0.4949(6) 1 calc PR . 1 H16C H 0.2594 0.2420 0.1266 0.053 Uiso 0.4949(6) 1 calc PR . 1 C17 C 0.3913(3) 0.3021(4) 0.0319(2) 0.0392(11) Uani 0.4949(6) 1 d P . 1 H17A H 0.4581 0.3305 0.0155 0.059 Uiso 0.4949(6) 1 calc PR . 1 H17B H 0.3498 0.3091 0.0002 0.059 Uiso 0.4949(6) 1 calc PR . 1 H17C H 0.3654 0.2326 0.0411 0.059 Uiso 0.4949(6) 1 calc PR . 1 Ga3 Ga 0.6667 0.3333 0.14234(3) 0.02385(18) Uani 0.5051(6) 3 d SP . 2 Ga4 Ga 0.6667 0.3333 0.25632(3) 0.02702(19) Uani 0.5051(6) 3 d SP . 2 S2 S 0.6299(4) 0.4438(5) 0.0943(3) 0.0355(11) Uani 0.5051(6) 1 d P . 2 Cl2 Cl 0.52565(8) 0.30942(8) 0.29631(4) 0.0413(3) Uani 0.5051(6) 1 d P . 2 B2 B 0.6667 0.3333 -0.0338(3) 0.0203(14) Uani 0.5051(6) 3 d SPD . 2 H2 H 0.6667 0.3333 -0.0860(10) 0.024 Uiso 0.5051(6) 3 d SPD . 2 C21 C 0.5469(3) 0.3673(3) 0.03775(16) 0.0253(8) Uani 0.5051(6) 1 d P . 2 N21 N 0.5706(2) 0.3310(2) -0.01335(13) 0.0250(6) Uani 0.5051(6) 1 d P . 2 N22 N 0.4495(2) 0.3368(2) 0.03402(16) 0.0287(8) Uani 0.5051(6) 1 d P . 2 C22 C 0.4879(3) 0.2788(3) -0.04897(18) 0.0317(9) Uani 0.5051(6) 1 d P . 2 H22A H 0.4837 0.2459 -0.0875 0.038 Uiso 0.5051(6) 1 calc PR . 2 C23 C 0.4133(3) 0.2820(3) -0.02033(19) 0.0358(9) Uani 0.5051(6) 1 d P . 2 H23A H 0.3476 0.2518 -0.0350 0.043 Uiso 0.5051(6) 1 calc PR . 2 C24 C 0.3880(19) 0.3587(18) 0.0793(9) 0.036(4) Uani 0.5051(6) 1 d P . 2 C25 C 0.4286(12) 0.4662(12) 0.0824(9) 0.052(5) Uani 0.5051(6) 1 d P . 2 H25A H 0.3903 0.4809 0.1125 0.077 Uiso 0.5051(6) 1 calc PR . 2 H25B H 0.4253 0.4907 0.0404 0.077 Uiso 0.5051(6) 1 calc PR . 2 H25C H 0.4969 0.4980 0.0965 0.077 Uiso 0.5051(6) 1 calc PR . 2 C26 C 0.2850(3) 0.3122(4) 0.0559(3) 0.0661(15) Uani 0.5051(6) 1 d P . 2 H26A H 0.2571 0.2411 0.0539 0.099 Uiso 0.5051(6) 1 calc PR . 2 H26B H 0.2843 0.3373 0.0136 0.099 Uiso 0.5051(6) 1 calc PR . 2 H26C H 0.2462 0.3277 0.0849 0.099 Uiso 0.5051(6) 1 calc PR . 2 C27 C 0.3916(5) 0.3145(5) 0.1449(3) 0.0690(19) Uani 0.5051(6) 1 d P . 2 H27A H 0.3604 0.2432 0.1413 0.104 Uiso 0.5051(6) 1 calc PR . 2 H27B H 0.3568 0.3311 0.1766 0.104 Uiso 0.5051(6) 1 calc PR . 2 H27C H 0.4599 0.3415 0.1580 0.104 Uiso 0.5051(6) 1 calc PR . 2 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 Ga1 0.0207(2) 0.0207(2) 0.0141(4) 0.000 0.000 0.01035(12) Ga2 0.0243(3) 0.0243(3) 0.0145(4) 0.000 0.000 0.01215(13) S1 0.0201(9) 0.0191(9) 0.0290(17) 0.0028(10) 0.0012(9) 0.0100(7) Cl1 0.0349(6) 0.0308(5) 0.0332(5) 0.0087(4) 0.0077(4) 0.0147(5) B1 0.023(2) 0.023(2) 0.006(3) 0.000 0.000 0.0117(11) C11 0.0253(19) 0.0201(17) 0.0169(16) -0.0002(13) 0.0041(13) 0.0126(15) N11 0.0287(17) 0.0218(15) 0.0128(13) 0.0010(11) 0.0039(12) 0.0128(13) N12 0.0226(17) 0.0240(17) 0.0252(17) 0.0043(13) 0.0049(14) 0.0144(15) C12 0.029(2) 0.029(2) 0.0174(17) 0.0041(14) 0.0074(14) 0.0136(17) C13 0.027(2) 0.030(2) 0.0239(19) 0.0046(15) 0.0081(15) 0.0155(17) C14 0.019(3) 0.029(4) 0.025(6) 0.007(4) 0.000(4) 0.014(3) C15 0.051(8) 0.032(6) 0.059(11) 0.017(6) 0.014(6) 0.035(6) C16 0.024(2) 0.040(2) 0.043(3) 0.0113(19) 0.0054(18) 0.0168(19) C17 0.031(3) 0.054(3) 0.026(2) 0.004(2) 0.001(2) 0.016(3) Ga3 0.0276(3) 0.0276(3) 0.0163(4) 0.000 0.000 0.01381(13) Ga4 0.0328(3) 0.0328(3) 0.0154(3) 0.000 0.000 0.01642(14) S2 0.0428(12) 0.0325(12) 0.038(2) -0.0102(14) -0.0136(12) 0.0239(10) Cl2 0.0365(6) 0.0631(7) 0.0266(5) -0.0054(5) -0.0007(4) 0.0267(6) B2 0.025(2) 0.025(2) 0.011(3) 0.000 0.000 0.0125(11) C21 0.028(2) 0.0254(19) 0.0244(18) 0.0042(15) 0.0007(14) 0.0146(16) N21 0.0333(18) 0.0245(15) 0.0198(15) 0.0008(12) -0.0032(13) 0.0163(14) N22 0.0236(18) 0.0258(19) 0.037(2) 0.0029(14) 0.0015(16) 0.0123(16) C22 0.036(2) 0.028(2) 0.034(2) -0.0061(16) -0.0121(17) 0.0188(19) C23 0.024(2) 0.029(2) 0.046(3) 0.0013(18) -0.0092(18) 0.0071(17) C24 0.035(5) 0.051(5) 0.034(8) 0.020(5) 0.010(5) 0.031(4) C25 0.029(6) 0.067(9) 0.063(12) 0.012(7) -0.002(6) 0.026(6) C26 0.034(3) 0.066(4) 0.099(5) 0.002(3) 0.014(3) 0.025(3) C27 0.086(5) 0.098(5) 0.057(4) 0.041(3) 0.040(4) 0.071(4) _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 Ga1 S1 2.348(7) 3_665 ? Ga1 S1 2.348(7) 2_655 ? Ga1 S1 2.348(7) . ? Ga1 Ga2 2.4098(9) . ? Ga2 Cl1 2.2159(10) 3_665 ? Ga2 Cl1 2.2159(10) . ? Ga2 Cl1 2.2159(10) 2_655 ? S1 C11 1.693(6) . ? B1 H1 1.11(2) . ? B1 N11 1.563(3) 2_655 ? B1 N11 1.563(3) 3_665 ? B1 N11 1.563(3) . ? C11 N11 1.347(4) . ? C11 N12 1.360(4) . ? N11 C12 1.381(4) . ? N12 C13 1.377(5) . ? N12 C14 1.48(2) . ? C12 C13 1.340(5) . ? C14 C17 1.52(2) . ? C14 C16 1.55(2) . ? C14 C15 1.57(2) . ? Ga3 S2 2.327(7) 3_665 ? Ga3 S2 2.327(7) 2_655 ? Ga3 S2 2.327(7) . ? Ga3 Ga4 2.4051(10) . ? Ga4 Cl2 2.2291(10) 2_655 ? Ga4 Cl2 2.2291(10) 3_665 ? Ga4 Cl2 2.2291(10) . ? S2 C21 1.738(7) . ? B2 H2 1.10(2) . ? B2 N21 1.558(3) 2_655 ? B2 N21 1.558(3) 3_665 ? B2 N21 1.558(3) . ? C21 N21 1.359(4) . ? C21 N22 1.364(5) . ? N21 C22 1.369(4) . ? N22 C23 1.377(5) . ? N22 C24 1.52(3) . ? C22 C23 1.346(5) . ? C24 C25 1.49(3) . ? C24 C26 1.49(2) . ? C24 C27 1.564(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 S1 Ga1 S1 102.09(17) 3_665 2_655 ? S1 Ga1 S1 102.08(17) 3_665 . ? S1 Ga1 S1 102.08(17) 2_655 . ? S1 Ga1 Ga2 116.12(14) 3_665 . ? S1 Ga1 Ga2 116.12(14) 2_655 . ? S1 Ga1 Ga2 116.12(14) . . ? Cl1 Ga2 Cl1 105.95(3) 3_665 . ? Cl1 Ga2 Cl1 105.95(3) 3_665 2_655 ? Cl1 Ga2 Cl1 105.96(3) . 2_655 ? Cl1 Ga2 Ga1 112.79(3) 3_665 . ? Cl1 Ga2 Ga1 112.79(3) . . ? Cl1 Ga2 Ga1 112.79(3) 2_655 . ? C11 S1 Ga1 100.8(3) . . ? H1 B1 N11 106.3(2) . 2_655 ? H1 B1 N11 106.3(2) . 3_665 ? N11 B1 N11 112.5(2) 2_655 3_665 ? H1 B1 N11 106.3(2) . . ? N11 B1 N11 112.5(2) 2_655 . ? N11 B1 N11 112.5(2) 3_665 . ? N11 C11 N12 108.4(3) . . ? N11 C11 S1 125.4(3) . . ? N12 C11 S1 126.1(3) . . ? C11 N11 C12 107.5(3) . . ? C11 N11 B1 134.3(3) . . ? C12 N11 B1 118.0(3) . . ? C11 N12 C13 108.0(3) . . ? C11 N12 C14 127.4(9) . . ? C13 N12 C14 124.3(9) . . ? C13 C12 N11 108.7(3) . . ? C12 C13 N12 107.5(3) . . ? N12 C14 C17 110.2(16) . . ? N12 C14 C16 109.7(12) . . ? C17 C14 C16 108.8(12) . . ? N12 C14 C15 107.6(13) . . ? C17 C14 C15 112.9(13) . . ? C16 C14 C15 107.5(17) . . ? S2 Ga3 S2 102.46(18) 3_665 2_655 ? S2 Ga3 S2 102.46(18) 3_665 . ? S2 Ga3 S2 102.46(18) 2_655 . ? S2 Ga3 Ga4 115.80(15) 3_665 . ? S2 Ga3 Ga4 115.80(15) 2_655 . ? S2 Ga3 Ga4 115.80(15) . . ? Cl2 Ga4 Cl2 106.56(3) 2_655 3_665 ? Cl2 Ga4 Cl2 106.56(3) 2_655 . ? Cl2 Ga4 Cl2 106.56(3) 3_665 . ? Cl2 Ga4 Ga3 112.25(3) 2_655 . ? Cl2 Ga4 Ga3 112.25(3) 3_665 . ? Cl2 Ga4 Ga3 112.25(3) . . ? C21 S2 Ga3 99.3(3) . . ? H2 B2 N21 106.0(3) . 2_655 ? H2 B2 N21 106.0(3) . 3_665 ? N21 B2 N21 112.7(2) 2_655 3_665 ? H2 B2 N21 106.0(3) . . ? N21 B2 N21 112.7(2) 2_655 . ? N21 B2 N21 112.7(2) 3_665 . ? N21 C21 N22 107.8(3) . . ? N21 C21 S2 124.6(3) . . ? N22 C21 S2 127.6(4) . . ? C21 N21 C22 107.9(3) . . ? C21 N21 B2 132.8(3) . . ? C22 N21 B2 119.1(3) . . ? C21 N22 C23 108.0(3) . . ? C21 N22 C24 128.2(9) . . ? C23 N22 C24 123.7(9) . . ? C23 C22 N21 108.7(3) . . ? C22 C23 N22 107.5(3) . . ? C25 C24 C26 108.5(17) . . ? C25 C24 N22 109.1(17) . . ? C26 C24 N22 110.0(14) . . ? C25 C24 C27 112.3(16) . . ? C26 C24 C27 110.3(15) . . ? N22 C24 C27 106.6(15) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 32.71 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.397 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.063 # Attachment '- TmGaGaI3(C6H6) (14s10).cif' data_14s10_2 _database_code_depnum_ccdc_archive 'CCDC 763458' #TrackingRef '- TmGaGaI3(C6H6) (14s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H40 B Ga2 I3 N6 S3' _chemical_formula_weight 1075.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 17.1401(10) _cell_length_b 11.9049(7) _cell_length_c 19.0672(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.6150(10) _cell_angle_gamma 90.00 _cell_volume 3824.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9568 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 32.32 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 4.021 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2383 _exptl_absorpt_correction_T_max 0.5002 _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 64566 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 32.75 _reflns_number_total 13386 _reflns_number_gt 11647 _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 bond has 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^)+(0.0266P)^2^+3.2293P] 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 13386 _refine_ls_number_parameters 382 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Ga1 Ga 0.216749(11) 1.217630(16) 0.188379(10) 0.01566(4) Uani 1 1 d . . . Ga2 Ga 0.186537(11) 1.028047(16) 0.221539(10) 0.01603(4) Uani 1 1 d . . . I1 I 0.201385(8) 0.913860(10) 0.107248(6) 0.02195(3) Uani 1 1 d . . . I2 I 0.289504(8) 0.940982(12) 0.324458(7) 0.02611(3) Uani 1 1 d . . . I3 I 0.049975(8) 0.983483(15) 0.251538(8) 0.03393(4) Uani 1 1 d . . . S1 S 0.28417(2) 1.19689(4) 0.09302(2) 0.01726(8) Uani 1 1 d . . . S2 S 0.30002(3) 1.33222(4) 0.26878(2) 0.01864(8) Uani 1 1 d . . . S3 S 0.11083(2) 1.33608(4) 0.14663(2) 0.01733(8) Uani 1 1 d . . . B B 0.27366(11) 1.48149(16) 0.11121(10) 0.0161(3) Uani 1 1 d D . . H1 H 0.2877(14) 1.5595(15) 0.0866(12) 0.019 Uiso 1 1 d D . . N11 N 0.34892(9) 1.40651(12) 0.12216(8) 0.0159(3) Uani 1 1 d . . . C11 C 0.35864(10) 1.29427(14) 0.12010(9) 0.0157(3) Uani 1 1 d . . . N12 N 0.43695(8) 1.27018(12) 0.14298(8) 0.0170(3) Uani 1 1 d . . . C12 C 0.42259(10) 1.45443(15) 0.14611(10) 0.0190(3) Uani 1 1 d . . . H12A H 0.4332 1.5325 0.1523 0.023 Uiso 1 1 calc R . . C13 C 0.47674(10) 1.37105(16) 0.15922(10) 0.0198(3) Uani 1 1 d . . . H13A H 0.5320 1.3799 0.1764 0.024 Uiso 1 1 calc R . . C14 C 0.47556(10) 1.15556(15) 0.15187(10) 0.0193(3) Uani 1 1 d . . . C15 C 0.56352(11) 1.17131(18) 0.18479(12) 0.0277(4) Uani 1 1 d . . . H15A H 0.5681 1.2072 0.2316 0.042 Uiso 1 1 calc R . . H15B H 0.5888 1.2188 0.1535 0.042 Uiso 1 1 calc R . . H15C H 0.5898 1.0979 0.1903 0.042 Uiso 1 1 calc R . . C16 C 0.46819(12) 1.09943(16) 0.07890(11) 0.0242(4) Uani 1 1 d . . . H16A H 0.4120 1.0890 0.0581 0.036 Uiso 1 1 calc R . . H16B H 0.4947 1.0262 0.0844 0.036 Uiso 1 1 calc R . . H16C H 0.4931 1.1471 0.0474 0.036 Uiso 1 1 calc R . . C17 C 0.43679(12) 1.08477(17) 0.20309(11) 0.0249(4) Uani 1 1 d . . . H17A H 0.3805 1.0737 0.1828 0.037 Uiso 1 1 calc R . . H17B H 0.4417 1.1237 0.2490 0.037 Uiso 1 1 calc R . . H17C H 0.4633 1.0116 0.2103 0.037 Uiso 1 1 calc R . . N21 N 0.25049(9) 1.51480(12) 0.18369(8) 0.0163(3) Uani 1 1 d . . . C21 C 0.25649(10) 1.46259(14) 0.24733(9) 0.0161(3) Uani 1 1 d . . . C22 C 0.21331(12) 1.61690(15) 0.18821(10) 0.0225(3) Uani 1 1 d . . . H22A H 0.2010 1.6706 0.1510 0.027 Uiso 1 1 calc R . . N22 N 0.22440(10) 1.53057(13) 0.29191(8) 0.0199(3) Uani 1 1 d . . . C23 C 0.19750(13) 1.62699(17) 0.25460(11) 0.0254(4) Uani 1 1 d . . . H23A H 0.1724 1.6891 0.2725 0.030 Uiso 1 1 calc R . . C24 C 0.21806(12) 1.50971(18) 0.36895(10) 0.0247(4) Uani 1 1 d . . . C25 C 0.17346(17) 1.6084(2) 0.39437(13) 0.0407(6) Uani 1 1 d . . . H25A H 0.1201 1.6131 0.3653 0.061 Uiso 1 1 calc R . . H25B H 0.2023 1.6783 0.3896 0.061 Uiso 1 1 calc R . . H25C H 0.1694 1.5972 0.4445 0.061 Uiso 1 1 calc R . . C26 C 0.30110(13) 1.5027(2) 0.41436(11) 0.0307(4) Uani 1 1 d . . . H26A H 0.3297 1.5728 0.4099 0.046 Uiso 1 1 calc R . . H26B H 0.3300 1.4398 0.3979 0.046 Uiso 1 1 calc R . . H26C H 0.2970 1.4908 0.4644 0.046 Uiso 1 1 calc R . . C27 C 0.17095(14) 1.4024(2) 0.37397(12) 0.0349(5) Uani 1 1 d . . . H27A H 0.1181 1.4097 0.3442 0.052 Uiso 1 1 calc R . . H27B H 0.1657 1.3898 0.4237 0.052 Uiso 1 1 calc R . . H27C H 0.1988 1.3387 0.3573 0.052 Uiso 1 1 calc R . . C31 C 0.13710(10) 1.37276(14) 0.06593(9) 0.0152(3) Uani 1 1 d . . . N31 N 0.20275(9) 1.43120(13) 0.05810(8) 0.0162(3) Uani 1 1 d . . . N32 N 0.09523(8) 1.34785(13) 0.00026(8) 0.0165(3) Uani 1 1 d . . . C32 C 0.20200(11) 1.44196(16) -0.01430(9) 0.0195(3) Uani 1 1 d . . . H32A H 0.2412 1.4788 -0.0353 0.023 Uiso 1 1 calc R . . C33 C 0.13600(11) 1.39107(16) -0.05008(9) 0.0195(3) Uani 1 1 d . . . H33A H 0.1204 1.3859 -0.1004 0.023 Uiso 1 1 calc R . . C34 C 0.01735(10) 1.28443(15) -0.01789(10) 0.0188(3) Uani 1 1 d . . . C35 C -0.00659(12) 1.28005(18) -0.09940(10) 0.0262(4) Uani 1 1 d . . . H35A H -0.0130 1.3567 -0.1184 0.039 Uiso 1 1 calc R . . H35B H -0.0568 1.2393 -0.1125 0.039 Uiso 1 1 calc R . . H35C H 0.0348 1.2414 -0.1194 0.039 Uiso 1 1 calc R . . C36 C -0.04688(11) 1.34785(17) 0.01186(11) 0.0246(4) Uani 1 1 d . . . H36A H -0.0326 1.3510 0.0640 0.037 Uiso 1 1 calc R . . H36B H -0.0978 1.3089 -0.0019 0.037 Uiso 1 1 calc R . . H36C H -0.0515 1.4243 -0.0074 0.037 Uiso 1 1 calc R . . C37 C 0.02806(12) 1.16492(16) 0.01176(11) 0.0236(4) Uani 1 1 d . . . H37A H 0.0430 1.1678 0.0639 0.035 Uiso 1 1 calc R . . H37B H 0.0699 1.1269 -0.0080 0.035 Uiso 1 1 calc R . . H37C H -0.0219 1.1234 -0.0016 0.035 Uiso 1 1 calc R . . C41 C 0.43882(16) 1.8438(2) 0.50173(13) 0.0428(6) Uani 1 1 d . . . H41A H 0.4168 1.8849 0.4601 0.051 Uiso 1 1 calc R . . C42 C 0.39122(15) 1.7734(2) 0.53277(16) 0.0450(7) Uani 1 1 d . . . H42A H 0.3366 1.7661 0.5123 0.054 Uiso 1 1 calc R . . C43 C 0.42231(15) 1.7134(2) 0.59342(16) 0.0410(6) Uani 1 1 d . . . H43A H 0.3892 1.6652 0.6148 0.049 Uiso 1 1 calc R . . C44 C 0.50226(14) 1.72404(19) 0.62292(13) 0.0341(5) Uani 1 1 d . . . H44A H 0.5240 1.6829 0.6646 0.041 Uiso 1 1 calc R . . C45 C 0.55040(13) 1.79449(18) 0.59178(12) 0.0299(4) Uani 1 1 d . . . H45A H 0.6051 1.8014 0.6120 0.036 Uiso 1 1 calc R . . C46 C 0.51875(16) 1.8550(2) 0.53105(12) 0.0349(5) Uani 1 1 d . . . H46A H 0.5515 1.9037 0.5097 0.042 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 Ga1 0.01602(8) 0.01377(8) 0.01685(8) 0.00194(6) 0.00216(6) -0.00087(6) Ga2 0.01631(8) 0.01442(8) 0.01703(8) 0.00143(6) 0.00223(7) -0.00133(6) I1 0.02865(6) 0.01839(5) 0.01916(5) -0.00200(4) 0.00536(4) -0.00440(4) I2 0.02466(6) 0.03362(7) 0.01851(6) 0.00348(4) -0.00011(4) 0.00774(5) I3 0.02018(6) 0.05171(9) 0.03160(7) -0.01129(6) 0.00922(5) -0.01244(6) S1 0.01486(17) 0.01626(18) 0.02083(19) -0.00272(14) 0.00378(14) -0.00279(14) S2 0.02122(19) 0.01567(18) 0.01688(18) 0.00221(14) -0.00211(15) 0.00037(14) S3 0.01513(17) 0.02102(19) 0.01641(18) 0.00359(14) 0.00440(14) 0.00139(14) B 0.0157(8) 0.0159(8) 0.0162(8) 0.0021(6) 0.0020(6) -0.0003(6) N11 0.0148(6) 0.0150(6) 0.0175(6) -0.0001(5) 0.0016(5) -0.0015(5) C11 0.0138(7) 0.0170(7) 0.0167(7) -0.0011(6) 0.0035(6) -0.0019(5) N12 0.0136(6) 0.0171(7) 0.0201(7) -0.0011(5) 0.0024(5) -0.0005(5) C12 0.0170(7) 0.0184(8) 0.0212(8) -0.0012(6) 0.0026(6) -0.0038(6) C13 0.0153(7) 0.0205(8) 0.0233(8) -0.0033(6) 0.0026(6) -0.0040(6) C14 0.0156(7) 0.0189(8) 0.0236(8) 0.0016(6) 0.0042(6) 0.0023(6) C15 0.0176(8) 0.0278(10) 0.0367(11) 0.0002(8) 0.0022(7) 0.0042(7) C16 0.0255(9) 0.0204(8) 0.0280(9) -0.0024(7) 0.0082(7) 0.0020(7) C17 0.0256(9) 0.0244(9) 0.0254(9) 0.0072(7) 0.0066(7) 0.0029(7) N21 0.0191(6) 0.0133(6) 0.0165(6) 0.0013(5) 0.0030(5) 0.0008(5) C21 0.0169(7) 0.0145(7) 0.0158(7) 0.0011(5) 0.0004(6) -0.0012(5) C22 0.0309(9) 0.0155(8) 0.0212(8) 0.0015(6) 0.0050(7) 0.0052(7) N22 0.0229(7) 0.0206(7) 0.0163(7) -0.0001(5) 0.0036(6) 0.0009(6) C23 0.0330(10) 0.0199(8) 0.0241(9) 0.0008(7) 0.0072(7) 0.0068(7) C24 0.0242(9) 0.0343(10) 0.0162(8) 0.0002(7) 0.0053(7) -0.0015(7) C25 0.0460(14) 0.0540(15) 0.0248(10) -0.0022(10) 0.0134(10) 0.0149(12) C26 0.0273(10) 0.0464(13) 0.0174(8) -0.0033(8) 0.0013(7) -0.0045(9) C27 0.0273(10) 0.0491(14) 0.0299(11) 0.0103(9) 0.0092(8) -0.0097(9) C31 0.0142(7) 0.0153(7) 0.0161(7) 0.0023(5) 0.0028(5) 0.0021(5) N31 0.0153(6) 0.0190(7) 0.0141(6) 0.0023(5) 0.0025(5) 0.0004(5) N32 0.0147(6) 0.0180(7) 0.0165(6) 0.0004(5) 0.0016(5) 0.0011(5) C32 0.0210(8) 0.0241(8) 0.0138(7) 0.0031(6) 0.0048(6) -0.0001(6) C33 0.0207(8) 0.0236(8) 0.0140(7) 0.0004(6) 0.0028(6) 0.0005(6) C34 0.0148(7) 0.0187(8) 0.0218(8) -0.0006(6) 0.0004(6) 0.0008(6) C35 0.0243(9) 0.0312(10) 0.0209(8) -0.0004(7) -0.0016(7) -0.0040(7) C36 0.0161(8) 0.0244(9) 0.0326(10) -0.0019(7) 0.0023(7) 0.0026(6) C37 0.0221(8) 0.0184(8) 0.0300(9) 0.0018(7) 0.0034(7) 0.0003(6) C41 0.0472(14) 0.0472(14) 0.0277(11) -0.0108(10) -0.0097(10) 0.0230(12) C42 0.0272(11) 0.0459(14) 0.0547(16) -0.0264(12) -0.0113(10) 0.0150(10) C43 0.0300(11) 0.0306(11) 0.0614(17) -0.0104(11) 0.0058(11) -0.0022(9) C44 0.0318(11) 0.0271(10) 0.0398(12) 0.0037(9) -0.0030(9) -0.0003(8) C45 0.0297(10) 0.0266(10) 0.0297(10) -0.0009(8) -0.0041(8) 0.0016(8) C46 0.0456(13) 0.0318(11) 0.0258(10) -0.0009(8) 0.0028(9) 0.0093(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 Ga1 S3 2.3207(5) . ? Ga1 S2 2.3329(5) . ? Ga1 S1 2.3402(5) . ? Ga1 Ga2 2.4254(3) . ? Ga2 I3 2.5653(3) . ? Ga2 I2 2.6008(2) . ? Ga2 I1 2.6203(3) . ? S1 C11 1.7311(17) . ? S2 C21 1.7380(17) . ? S3 C31 1.7369(17) . ? B H1 1.087(16) . ? B N11 1.551(2) . ? B N31 1.552(2) . ? B N21 1.558(2) . ? N11 C11 1.348(2) . ? N11 C12 1.384(2) . ? C11 N12 1.363(2) . ? N12 C13 1.388(2) . ? N12 C14 1.512(2) . ? C12 C13 1.351(3) . ? C14 C16 1.528(3) . ? C14 C17 1.531(3) . ? C14 C15 1.534(3) . ? N21 C21 1.350(2) . ? N21 C22 1.382(2) . ? C21 N22 1.361(2) . ? C22 C23 1.348(3) . ? N22 C23 1.384(2) . ? N22 C24 1.513(2) . ? C24 C27 1.524(3) . ? C24 C26 1.526(3) . ? C24 C25 1.529(3) . ? C31 N31 1.354(2) . ? C31 N32 1.356(2) . ? N31 C32 1.384(2) . ? N32 C33 1.386(2) . ? N32 C34 1.517(2) . ? C32 C33 1.352(3) . ? C34 C36 1.528(3) . ? C34 C37 1.530(3) . ? C34 C35 1.533(3) . ? C41 C42 1.377(4) . ? C41 C46 1.387(4) . ? C42 C43 1.380(4) . ? C43 C44 1.388(3) . ? C44 C45 1.385(3) . ? C45 C46 1.386(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 S3 Ga1 S2 102.436(17) . . ? S3 Ga1 S1 105.349(17) . . ? S2 Ga1 S1 104.026(17) . . ? S3 Ga1 Ga2 117.630(14) . . ? S2 Ga1 Ga2 120.465(14) . . ? S1 Ga1 Ga2 105.312(14) . . ? Ga1 Ga2 I3 119.866(10) . . ? Ga1 Ga2 I2 114.820(9) . . ? I3 Ga2 I2 105.638(9) . . ? Ga1 Ga2 I1 101.996(9) . . ? I3 Ga2 I1 108.092(8) . . ? I2 Ga2 I1 105.331(9) . . ? C11 S1 Ga1 98.06(6) . . ? C21 S2 Ga1 100.57(6) . . ? C31 S3 Ga1 98.19(6) . . ? H1 B N11 107.8(13) . . ? H1 B N31 104.9(13) . . ? N11 B N31 113.45(14) . . ? H1 B N21 106.1(13) . . ? N11 B N21 111.63(14) . . ? N31 B N21 112.34(14) . . ? C11 N11 C12 107.94(14) . . ? C11 N11 B 132.13(14) . . ? C12 N11 B 119.53(14) . . ? N11 C11 N12 108.59(14) . . ? N11 C11 S1 125.75(13) . . ? N12 C11 S1 125.66(13) . . ? C11 N12 C13 107.70(14) . . ? C11 N12 C14 127.61(14) . . ? C13 N12 C14 124.67(14) . . ? C13 C12 N11 108.19(15) . . ? C12 C13 N12 107.57(15) . . ? N12 C14 C16 109.36(15) . . ? N12 C14 C17 109.61(14) . . ? C16 C14 C17 111.55(16) . . ? N12 C14 C15 108.20(15) . . ? C16 C14 C15 109.65(16) . . ? C17 C14 C15 108.39(16) . . ? C21 N21 C22 107.96(15) . . ? C21 N21 B 133.66(15) . . ? C22 N21 B 118.35(14) . . ? N21 C21 N22 108.36(15) . . ? N21 C21 S2 125.51(13) . . ? N22 C21 S2 126.11(13) . . ? C23 C22 N21 108.16(16) . . ? C21 N22 C23 107.87(15) . . ? C21 N22 C24 128.19(16) . . ? C23 N22 C24 123.94(16) . . ? C22 C23 N22 107.65(17) . . ? N22 C24 C27 109.40(17) . . ? N22 C24 C26 109.48(16) . . ? C27 C24 C26 111.59(19) . . ? N22 C24 C25 108.12(17) . . ? C27 C24 C25 108.8(2) . . ? C26 C24 C25 109.33(19) . . ? N31 C31 N32 108.64(14) . . ? N31 C31 S3 125.67(13) . . ? N32 C31 S3 125.69(13) . . ? C31 N31 C32 107.59(14) . . ? C31 N31 B 133.87(14) . . ? C32 N31 B 118.52(14) . . ? C31 N32 C33 108.03(14) . . ? C31 N32 C34 127.81(14) . . ? C33 N32 C34 124.16(14) . . ? C33 C32 N31 108.36(16) . . ? C32 C33 N32 107.38(15) . . ? N32 C34 C36 109.47(14) . . ? N32 C34 C37 109.76(14) . . ? C36 C34 C37 111.59(16) . . ? N32 C34 C35 107.95(15) . . ? C36 C34 C35 108.45(15) . . ? C37 C34 C35 109.54(16) . . ? C42 C41 C46 120.3(2) . . ? C41 C42 C43 120.5(2) . . ? C42 C43 C44 119.5(3) . . ? C45 C44 C43 120.2(2) . . ? C44 C45 C46 120.0(2) . . ? C45 C46 C41 119.5(3) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 32.75 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.384 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.097 # Attachment '- TmGaGaI3 (ky267s10).cif' data_backup _database_code_depnum_ccdc_archive 'CCDC 763459' #TrackingRef '- TmGaGaI3 (ky267s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H40 B Ga2 I3 N8 S3' _chemical_formula_weight 1079.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0854(10) _cell_length_b 11.1373(10) _cell_length_c 16.5062(14) _cell_angle_alpha 76.4550(10) _cell_angle_beta 83.6380(10) _cell_angle_gamma 80.9820(10) _cell_volume 1950.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9836 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 32.56 _exptl_crystal_description block _exptl_crystal_colour color _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 3.943 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3842 _exptl_absorpt_correction_T_max 0.5893 _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 33854 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 32.73 _reflns_number_total 13314 _reflns_number_gt 11507 _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 bond has been restrained to 1.1 Angstroms and disorder of the GaI3 unit was modeled. ; _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^+3.0207P] 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 13314 _refine_ls_number_parameters 401 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0779 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga -0.30332(2) 0.89949(2) 0.791259(16) 0.01653(5) Uani 1 1 d . A . Ga2 Ga -0.51771(2) 0.89613(3) 0.779120(16) 0.01856(6) Uani 1 1 d . . . I1 I -0.59512(8) 1.04491(6) 0.64356(6) 0.0316(3) Uani 0.758(11) 1 d P A 1 I2 I -0.55242(9) 0.67107(9) 0.77283(5) 0.0265(2) Uani 0.758(11) 1 d P A 1 I3 I -0.65079(13) 0.9623(2) 0.90259(8) 0.0343(2) Uani 0.758(11) 1 d P A 1 I4 I -0.5994(4) 1.0320(7) 0.6411(3) 0.0751(15) Uani 0.242(11) 1 d P A 2 I5 I -0.5518(4) 0.6684(4) 0.7837(5) 0.0604(11) Uani 0.242(11) 1 d P A 2 I6 I -0.6481(4) 0.9749(6) 0.8984(3) 0.0427(10) Uani 0.242(11) 1 d P A 2 B B 0.0256(2) 0.8924(3) 0.81129(16) 0.0188(4) Uani 1 1 d D A . H1 H 0.1237(16) 0.887(3) 0.814(2) 0.023 Uiso 1 1 d D . . S1 S -0.26027(5) 1.02056(5) 0.87857(4) 0.01923(11) Uani 1 1 d . . . S2 S -0.19925(6) 0.70266(5) 0.84725(4) 0.01949(11) Uani 1 1 d . . . S3 S -0.19052(5) 0.97572(5) 0.66659(3) 0.01808(10) Uani 1 1 d . . . C11 C -0.1413(2) 1.0904(2) 0.81806(14) 0.0183(4) Uani 1 1 d . A . N11 N -0.02955(18) 1.03203(19) 0.79690(12) 0.0182(4) Uani 1 1 d . . . C12 C 0.0387(2) 1.1219(2) 0.75055(15) 0.0232(5) Uani 1 1 d . A . H12A H 0.1206 1.1071 0.7275 0.028 Uiso 1 1 calc R . . N12 N -0.1442(2) 1.21454(19) 0.78589(13) 0.0216(4) Uani 1 1 d . . . C13 C -0.0309(2) 1.2342(2) 0.74359(16) 0.0248(5) Uani 1 1 d . A . H13A H -0.0068 1.3123 0.7151 0.030 Uiso 1 1 calc R . . C14 C -0.2490(3) 1.3168(2) 0.79371(17) 0.0260(5) Uani 1 1 d . A . C15 C -0.2751(3) 1.3238(3) 0.88554(19) 0.0324(6) Uani 1 1 d . . . H15A H -0.3464 1.3863 0.8914 0.049 Uiso 1 1 calc R A . H15B H -0.2036 1.3472 0.9051 0.049 Uiso 1 1 calc R . . H15C H -0.2919 1.2422 0.9190 0.049 Uiso 1 1 calc R . . C16 C -0.3621(3) 1.2925(3) 0.7578(2) 0.0335(6) Uani 1 1 d . . . H16A H -0.4318 1.3545 0.7680 0.050 Uiso 1 1 calc R A . H16B H -0.3813 1.2088 0.7848 0.050 Uiso 1 1 calc R . . H16C H -0.3455 1.2987 0.6975 0.050 Uiso 1 1 calc R . . C17 C -0.2116(3) 1.4406(3) 0.7421(2) 0.0424(8) Uani 1 1 d . . . H17A H -0.1404 1.4592 0.7649 0.064 Uiso 1 1 calc R A . H17B H -0.2799 1.5075 0.7446 0.064 Uiso 1 1 calc R . . H17C H -0.1905 1.4342 0.6839 0.064 Uiso 1 1 calc R . . C21 C -0.1181(2) 0.7457(2) 0.91751(14) 0.0185(4) Uani 1 1 d . A . N21 N -0.02746(18) 0.81838(19) 0.89643(12) 0.0187(4) Uani 1 1 d . . . N22 N -0.13539(19) 0.71430(19) 1.00242(12) 0.0199(4) Uani 1 1 d . . . C22 C 0.0122(2) 0.8337(3) 0.96941(15) 0.0240(5) Uani 1 1 d . A . H22A H 0.0751 0.8806 0.9731 0.029 Uiso 1 1 calc R . . C23 C -0.0540(2) 0.7706(3) 1.03458(16) 0.0247(5) Uani 1 1 d . A . H23A H -0.0463 0.7655 1.0921 0.030 Uiso 1 1 calc R . . C24 C -0.2220(2) 0.6295(3) 1.05480(16) 0.0245(5) Uani 1 1 d . A . C25 C -0.2094(3) 0.6229(3) 1.14701(17) 0.0344(6) Uani 1 1 d . . . H25A H -0.2341 0.7058 1.1589 0.052 Uiso 1 1 calc R A . H25B H -0.1239 0.5941 1.1596 0.052 Uiso 1 1 calc R . . H25C H -0.2619 0.5646 1.1817 0.052 Uiso 1 1 calc R . . C26 C -0.1858(3) 0.4990(3) 1.03728(18) 0.0306(6) Uani 1 1 d . . . H26A H -0.2429 0.4435 1.0696 0.046 Uiso 1 1 calc R A . H26B H -0.1025 0.4666 1.0535 0.046 Uiso 1 1 calc R . . H26C H -0.1888 0.5034 0.9775 0.046 Uiso 1 1 calc R . . C27 C -0.3549(3) 0.6821(3) 1.03554(19) 0.0324(6) Uani 1 1 d . . . H27A H -0.4103 0.6261 1.0695 0.049 Uiso 1 1 calc R A . H27B H -0.3640 0.6892 0.9762 0.049 Uiso 1 1 calc R . . H27C H -0.3752 0.7646 1.0487 0.049 Uiso 1 1 calc R . . C31 C -0.0689(2) 0.8560(2) 0.67814(14) 0.0174(4) Uani 1 1 d . A . N31 N 0.01267(18) 0.83255(19) 0.73678(12) 0.0189(4) Uani 1 1 d . . . C32 C 0.0930(2) 0.7278(3) 0.72684(16) 0.0248(5) Uani 1 1 d . A . H32A H 0.1600 0.6907 0.7596 0.030 Uiso 1 1 calc R . . N32 N -0.04210(19) 0.7680(2) 0.63159(13) 0.0199(4) Uani 1 1 d . . . C33 C 0.0598(3) 0.6873(3) 0.66261(17) 0.0269(5) Uani 1 1 d . A . H33A H 0.0988 0.6167 0.6423 0.032 Uiso 1 1 calc R . . C34 C -0.1044(2) 0.7585(3) 0.55666(15) 0.0235(5) Uani 1 1 d . A . C35 C -0.2405(3) 0.7493(3) 0.58083(18) 0.0284(5) Uani 1 1 d . . . H35A H -0.2779 0.8206 0.6044 0.043 Uiso 1 1 calc R A . H35B H -0.2493 0.6717 0.6224 0.043 Uiso 1 1 calc R . . H35C H -0.2814 0.7495 0.5311 0.043 Uiso 1 1 calc R . . C36 C -0.0847(3) 0.8708(3) 0.48660(17) 0.0321(6) Uani 1 1 d . . . H36A H -0.1179 0.9473 0.5055 0.048 Uiso 1 1 calc R A . H36B H -0.1265 0.8670 0.4382 0.048 Uiso 1 1 calc R . . H36C H 0.0032 0.8706 0.4708 0.048 Uiso 1 1 calc R . . C37 C -0.04943(16) 0.63823(16) 0.52682(11) 0.0376(7) Uani 1 1 d . . . H37A H -0.0601 0.5655 0.5724 0.056 Uiso 1 1 calc R A . H37B H 0.0381 0.6402 0.5104 0.056 Uiso 1 1 calc R . . H37C H -0.0914 0.6329 0.4788 0.056 Uiso 1 1 calc R . . N41 N -0.18373(16) 0.60366(16) 0.35196(11) 0.0383(6) Uani 1 1 d R . . C41 C -0.28013(16) 0.60058(16) 0.37028(11) 0.0349(6) Uani 1 1 d R . . C42 C -0.41165(16) 0.60198(16) 0.40171(11) 0.0701(14) Uani 1 1 d R . . H42A H -0.4542 0.5651 0.3666 0.105 Uiso 1 1 d R . . H42B H -0.4494 0.6882 0.3998 0.105 Uiso 1 1 d R . . H42C H -0.4177 0.5536 0.4594 0.105 Uiso 1 1 d R . . C51 C -0.6971(3) 0.7182(4) 0.4952(2) 0.0453(8) Uani 1 1 d . . . N51 N -0.7189(4) 0.6404(4) 0.4662(2) 0.0627(10) Uani 1 1 d . . . C52 C -0.6679(5) 0.8148(4) 0.5323(3) 0.0572(10) Uani 1 1 d . . . H52A H -0.7032 0.8028 0.5903 0.086 Uiso 1 1 calc R . . H52B H -0.7020 0.8966 0.5006 0.086 Uiso 1 1 calc R . . H52C H -0.5787 0.8103 0.5312 0.086 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 Ga1 0.01396(11) 0.01856(12) 0.01779(11) -0.00466(9) -0.00078(8) -0.00370(8) Ga2 0.01404(11) 0.02177(12) 0.02021(12) -0.00461(9) -0.00067(9) -0.00397(9) I1 0.0322(3) 0.0280(5) 0.0286(3) 0.00698(15) -0.0114(2) -0.00011(15) I2 0.0224(3) 0.0188(2) 0.0387(5) -0.00476(17) -0.00553(15) -0.00414(18) I3 0.0258(3) 0.0592(5) 0.0259(3) -0.0224(2) 0.0073(2) -0.0164(3) I4 0.0484(14) 0.117(3) 0.0424(14) 0.0093(14) -0.0010(10) -0.0014(15) I5 0.0347(12) 0.0342(13) 0.119(3) -0.0245(15) 0.0010(14) -0.0167(9) I6 0.0305(12) 0.0499(12) 0.057(2) -0.0371(13) 0.0174(9) -0.0111(8) B 0.0173(11) 0.0223(12) 0.0175(11) -0.0059(9) -0.0004(8) -0.0037(9) S1 0.0196(2) 0.0201(3) 0.0197(2) -0.0081(2) 0.00423(19) -0.0060(2) S2 0.0231(3) 0.0175(2) 0.0195(2) -0.00427(19) -0.0053(2) -0.0047(2) S3 0.0173(2) 0.0197(2) 0.0161(2) -0.00345(19) -0.00041(18) -0.00029(19) C11 0.0199(10) 0.0194(10) 0.0177(9) -0.0068(8) -0.0003(8) -0.0062(8) N11 0.0178(8) 0.0204(9) 0.0180(8) -0.0057(7) 0.0012(7) -0.0067(7) C12 0.0230(11) 0.0280(12) 0.0201(10) -0.0038(9) 0.0014(8) -0.0126(9) N12 0.0247(10) 0.0186(9) 0.0223(9) -0.0050(7) 0.0006(8) -0.0064(7) C13 0.0276(12) 0.0241(12) 0.0236(11) -0.0034(9) 0.0026(9) -0.0116(9) C14 0.0308(13) 0.0190(11) 0.0289(12) -0.0061(9) -0.0030(10) -0.0036(9) C15 0.0394(15) 0.0272(13) 0.0337(14) -0.0162(11) -0.0038(12) 0.0014(11) C16 0.0350(15) 0.0301(14) 0.0360(15) -0.0086(11) -0.0107(12) 0.0012(11) C17 0.0496(19) 0.0187(13) 0.054(2) -0.0036(13) 0.0066(16) -0.0042(12) C21 0.0210(10) 0.0179(10) 0.0169(9) -0.0036(8) -0.0036(8) -0.0026(8) N21 0.0181(9) 0.0215(9) 0.0173(8) -0.0048(7) -0.0033(7) -0.0037(7) N22 0.0228(9) 0.0207(9) 0.0169(8) -0.0041(7) -0.0025(7) -0.0042(7) C22 0.0249(11) 0.0289(12) 0.0205(10) -0.0065(9) -0.0039(9) -0.0078(9) C23 0.0275(12) 0.0294(13) 0.0192(10) -0.0044(9) -0.0062(9) -0.0082(10) C24 0.0266(12) 0.0259(12) 0.0204(11) -0.0020(9) 0.0012(9) -0.0086(9) C25 0.0433(16) 0.0415(16) 0.0203(12) -0.0048(11) 0.0026(11) -0.0176(13) C26 0.0398(15) 0.0235(12) 0.0276(13) -0.0025(10) 0.0012(11) -0.0086(11) C27 0.0260(13) 0.0357(15) 0.0349(14) -0.0064(12) 0.0035(11) -0.0087(11) C31 0.0171(9) 0.0187(10) 0.0158(9) -0.0050(8) 0.0010(7) -0.0008(8) N31 0.0164(8) 0.0214(9) 0.0185(9) -0.0063(7) -0.0007(7) 0.0006(7) C32 0.0204(11) 0.0271(12) 0.0258(11) -0.0089(9) -0.0034(9) 0.0056(9) N32 0.0200(9) 0.0220(9) 0.0196(9) -0.0098(7) -0.0021(7) -0.0007(7) C33 0.0259(12) 0.0255(12) 0.0294(12) -0.0116(10) -0.0036(10) 0.0058(9) C34 0.0261(11) 0.0282(12) 0.0206(10) -0.0129(9) -0.0024(9) -0.0052(9) C35 0.0259(12) 0.0315(13) 0.0320(13) -0.0117(11) -0.0029(10) -0.0090(10) C36 0.0355(14) 0.0440(16) 0.0197(11) -0.0093(11) 0.0008(10) -0.0129(12) C37 0.0387(16) 0.0401(17) 0.0408(16) -0.0252(14) -0.0015(13) -0.0021(13) N41 0.0364(14) 0.0387(15) 0.0386(14) -0.0079(11) 0.0014(11) -0.0056(11) C41 0.0360(15) 0.0341(15) 0.0346(15) -0.0065(12) -0.0079(12) -0.0031(12) C42 0.0327(19) 0.057(3) 0.110(4) 0.002(3) -0.010(2) -0.0025(17) C51 0.0400(18) 0.058(2) 0.0327(16) -0.0026(15) 0.0007(13) -0.0041(16) N51 0.060(2) 0.075(3) 0.052(2) -0.0144(19) 0.0078(17) -0.016(2) C52 0.069(3) 0.063(3) 0.0381(19) -0.0043(18) -0.0081(18) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 S1 2.3211(6) . ? Ga1 S3 2.3373(6) . ? Ga1 S2 2.3421(7) . ? Ga1 Ga2 2.4138(4) . ? Ga2 I6 2.553(4) . ? Ga2 I3 2.5632(13) . ? Ga2 I4 2.591(4) . ? Ga2 I1 2.5946(8) . ? Ga2 I5 2.605(4) . ? Ga2 I2 2.6220(11) . ? B H1 1.086(17) . ? B N11 1.552(3) . ? B N21 1.558(3) . ? B N31 1.559(3) . ? S1 C11 1.735(2) . ? S2 C21 1.735(2) . ? S3 C31 1.734(2) . ? C11 N11 1.355(3) . ? C11 N12 1.356(3) . ? N11 C12 1.381(3) . ? C12 C13 1.350(4) . ? N12 C13 1.391(3) . ? N12 C14 1.512(3) . ? C14 C15 1.529(4) . ? C14 C16 1.531(4) . ? C14 C17 1.532(4) . ? C21 N21 1.353(3) . ? C21 N22 1.362(3) . ? N21 C22 1.382(3) . ? N22 C23 1.388(3) . ? N22 C24 1.510(3) . ? C22 C23 1.350(4) . ? C24 C25 1.528(4) . ? C24 C26 1.532(4) . ? C24 C27 1.536(4) . ? C31 N31 1.351(3) . ? C31 N32 1.360(3) . ? N31 C32 1.382(3) . ? C32 C33 1.351(4) . ? N32 C33 1.393(3) . ? N32 C34 1.514(3) . ? C34 C36 1.517(4) . ? C34 C35 1.530(4) . ? C34 C37 1.548(3) . ? N41 C41 1.0815 . ? C41 C42 1.4913 . ? C51 N51 1.150(6) . ? C51 C52 1.450(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ga1 S3 102.44(2) . . ? S1 Ga1 S2 102.84(2) . . ? S3 Ga1 S2 105.81(2) . . ? S1 Ga1 Ga2 115.871(19) . . ? S3 Ga1 Ga2 115.428(19) . . ? S2 Ga1 Ga2 113.003(19) . . ? Ga1 Ga2 I6 110.37(11) . . ? Ga1 Ga2 I3 111.30(3) . . ? I6 Ga2 I3 3.3(2) . . ? Ga1 Ga2 I4 114.19(13) . . ? I6 Ga2 I4 106.87(15) . . ? I3 Ga2 I4 108.89(12) . . ? Ga1 Ga2 I1 112.17(2) . . ? I6 Ga2 I1 105.13(13) . . ? I3 Ga2 I1 107.31(4) . . ? I4 Ga2 I1 3.8(2) . . ? Ga1 Ga2 I5 108.85(10) . . ? I6 Ga2 I5 109.83(18) . . ? I3 Ga2 I5 106.62(15) . . ? I4 Ga2 I5 106.62(12) . . ? I1 Ga2 I5 110.45(17) . . ? Ga1 Ga2 I2 109.57(2) . . ? I6 Ga2 I2 112.65(17) . . ? I3 Ga2 I2 109.48(5) . . ? I4 Ga2 I2 103.05(19) . . ? I1 Ga2 I2 106.88(2) . . ? I5 Ga2 I2 3.85(19) . . ? H1 B N11 107.4(17) . . ? H1 B N21 107.9(17) . . ? N11 B N21 110.40(19) . . ? H1 B N31 104.9(17) . . ? N11 B N31 113.16(19) . . ? N21 B N31 112.7(2) . . ? C11 S1 Ga1 99.75(8) . . ? C21 S2 Ga1 98.26(8) . . ? C31 S3 Ga1 96.79(8) . . ? N11 C11 N12 108.6(2) . . ? N11 C11 S1 126.34(18) . . ? N12 C11 S1 125.03(18) . . ? C11 N11 C12 107.7(2) . . ? C11 N11 B 132.5(2) . . ? C12 N11 B 119.7(2) . . ? C13 C12 N11 108.4(2) . . ? C11 N12 C13 107.9(2) . . ? C11 N12 C14 127.7(2) . . ? C13 N12 C14 124.4(2) . . ? C12 C13 N12 107.4(2) . . ? N12 C14 C15 109.2(2) . . ? N12 C14 C16 109.9(2) . . ? C15 C14 C16 111.5(3) . . ? N12 C14 C17 108.4(2) . . ? C15 C14 C17 109.7(2) . . ? C16 C14 C17 108.0(3) . . ? N21 C21 N22 108.5(2) . . ? N21 C21 S2 125.20(17) . . ? N22 C21 S2 126.28(18) . . ? C21 N21 C22 107.9(2) . . ? C21 N21 B 133.1(2) . . ? C22 N21 B 118.7(2) . . ? C21 N22 C23 107.7(2) . . ? C21 N22 C24 127.8(2) . . ? C23 N22 C24 124.5(2) . . ? C23 C22 N21 108.2(2) . . ? C22 C23 N22 107.7(2) . . ? N22 C24 C25 108.7(2) . . ? N22 C24 C26 108.5(2) . . ? C25 C24 C26 109.0(2) . . ? N22 C24 C27 110.1(2) . . ? C25 C24 C27 108.5(2) . . ? C26 C24 C27 111.9(2) . . ? N31 C31 N32 108.8(2) . . ? N31 C31 S3 125.41(17) . . ? N32 C31 S3 125.80(18) . . ? C31 N31 C32 107.9(2) . . ? C31 N31 B 133.5(2) . . ? C32 N31 B 118.5(2) . . ? C33 C32 N31 108.3(2) . . ? C31 N32 C33 107.6(2) . . ? C31 N32 C34 128.1(2) . . ? C33 N32 C34 124.2(2) . . ? C32 C33 N32 107.5(2) . . ? N32 C34 C36 108.6(2) . . ? N32 C34 C35 110.0(2) . . ? C36 C34 C35 112.1(2) . . ? N32 C34 C37 110.46(19) . . ? C36 C34 C37 109.1(2) . . ? C35 C34 C37 106.5(2) . . ? N41 C41 C42 174.8 . . ? N51 C51 C52 179.0(5) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 32.73 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.253 _refine_diff_density_min -1.374 _refine_diff_density_rms 0.101 # Attachment '- TmGaIGaI2GaI2 (14s).cif' data_14s _database_code_depnum_ccdc_archive 'CCDC 763460' #TrackingRef '- TmGaIGaI2GaI2 (14s).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H80 B2 Ga4 I5 N16 S6' _chemical_formula_weight 2032.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 30.236(4) _cell_length_b 10.3955(13) _cell_length_c 27.107(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.589(2) _cell_angle_gamma 90.00 _cell_volume 7976.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9866 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.19 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3948 _exptl_absorpt_coefficient_mu 3.470 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5437 _exptl_absorpt_correction_T_max 0.9030 _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 83123 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0952 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.03 _reflns_number_total 14088 _reflns_number_gt 8823 _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. One tert-butyl group has been restrained and refined isotropically. The small crystal diffracted weakly and thereby contributed to a higher R-value. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.287 0.441 0.136 521 358 ' ' 2 0.713 0.517 -0.136 521 375 ' ' 3 0.713 1.042 0.364 521 374 ' ' 4 0.287 0.215 0.636 521 358 ' ' _platon_squeeze_details ; The unit cell contains 16 acetonitrile molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _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^)+(0.1728P)^2^+92.4944P] 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 14088 _refine_ls_number_parameters 635 _refine_ls_number_restraints 257 _refine_ls_R_factor_all 0.1471 _refine_ls_R_factor_gt 0.1116 _refine_ls_wR_factor_ref 0.3103 _refine_ls_wR_factor_gt 0.2935 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.090 _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 Ga1 Ga 0.38337(8) -1.39897(18) 0.83751(10) 0.0415(6) Uani 1 1 d . . . Ga2 Ga 0.31981(7) -1.52465(16) 0.84653(8) 0.0251(4) Uani 1 1 d . . . Ga3 Ga 0.25062(6) -1.41649(15) 0.85064(7) 0.0213(4) Uani 1 1 d . . . Ga4 Ga 0.03686(7) -0.45124(17) 0.52550(7) 0.0230(4) Uani 1 1 d . . . I1 I 0.44702(6) -1.53187(13) 0.81344(9) 0.0723(6) Uani 1 1 d . . . I2 I 0.34947(5) -1.67268(11) 0.93018(5) 0.0383(3) Uani 1 1 d . . . I3 I 0.29216(5) -1.66740(11) 0.76057(5) 0.0353(3) Uani 1 1 d . . . I4 I 0.19734(4) -1.29825(11) 0.76645(4) 0.0323(3) Uani 1 1 d . . . I5 I 0.19252(5) -1.55989(11) 0.88035(6) 0.0417(4) Uani 1 1 d . . . S1 S 0.4386(2) -1.2788(6) 0.9031(3) 0.072(2) Uani 1 1 d . . . S2 S 0.3572(2) -1.2600(6) 0.7635(2) 0.0518(14) Uani 1 1 d U . . S3 S 0.26872(14) -1.2603(4) 0.91936(15) 0.0214(9) Uani 1 1 d U . . S4 S 0.03199(16) -0.2301(4) 0.51922(16) 0.0274(10) Uani 1 1 d . . . S5 S 0.06598(16) -0.4952(4) 0.61479(15) 0.0256(9) Uani 1 1 d . . . S6 S 0.09750(15) -0.5094(4) 0.49783(17) 0.0254(9) Uani 1 1 d U . . B1 B 0.3394(7) -1.1314(17) 0.8681(8) 0.029(4) Uani 1 1 d DU . . H1 H 0.3296(10) -1.2286(18) 0.8522(11) 0.035 Uiso 1 1 d D . . B2 B 0.1477(5) -0.2845(15) 0.5960(6) 0.013(3) Uani 1 1 d DU . . H2 H 0.1810(7) -0.240(2) 0.6193(10) 0.016 Uiso 1 1 d D . . N11 N 0.3714(4) -1.1278(12) 0.9215(5) 0.020(3) Uani 1 1 d DU . . C11 C 0.4132(8) -1.197(2) 0.9423(8) 0.047(5) Uani 1 1 d U A . C12 C 0.3651(7) -1.0629(16) 0.9656(7) 0.034(4) Uani 1 1 d . . . H12A H 0.3397 -1.0070 0.9635 0.041 Uiso 1 1 calc R . . N12 N 0.4314(7) -1.1720(18) 0.9966(7) 0.055(5) Uani 1 1 d U . . C13 C 0.3995(6) -1.0928(18) 1.0085(8) 0.035(4) Uani 1 1 d U A . H13A H 0.4024 -1.0648 1.0429 0.042 Uiso 1 1 calc R . . C14 C 0.4698(8) -1.252(2) 1.0424(14) 0.070 Uiso 0.50(3) 1 d PD A 1 C15 C 0.5146(11) -1.230(3) 1.0323(18) 0.070 Uiso 0.50(3) 1 d PD A 1 H15A H 0.5124 -1.2711 0.9989 0.105 Uiso 0.50(3) 1 calc PR A 1 H15B H 0.5411 -1.2681 1.0610 0.105 Uiso 0.50(3) 1 calc PR A 1 H15C H 0.5199 -1.1379 1.0303 0.105 Uiso 0.50(3) 1 calc PR A 1 C16 C 0.4709(18) -1.192(4) 1.0927(19) 0.070 Uiso 0.50(3) 1 d PD A 1 H16A H 0.4396 -1.1986 1.0957 0.105 Uiso 0.50(3) 1 calc PR A 1 H16B H 0.4794 -1.1006 1.0928 0.105 Uiso 0.50(3) 1 calc PR A 1 H16C H 0.4942 -1.2355 1.1225 0.105 Uiso 0.50(3) 1 calc PR A 1 C17 C 0.4572(18) -1.392(3) 1.040(2) 0.070 Uiso 0.50(3) 1 d PD A 1 H17A H 0.4538 -1.4258 1.0051 0.105 Uiso 0.50(3) 1 calc PR A 1 H17B H 0.4273 -1.4017 1.0460 0.105 Uiso 0.50(3) 1 calc PR A 1 H17C H 0.4821 -1.4387 1.0671 0.105 Uiso 0.50(3) 1 calc PR A 1 C104 C 0.4792(10) -1.223(2) 1.0269(16) 0.070 Uiso 0.50(3) 1 d PD A 2 C105 C 0.476(2) -1.369(4) 1.023(2) 0.070 Uiso 0.50(3) 1 d PD A 2 H10A H 0.5062 -1.4072 1.0439 0.105 Uiso 0.50(3) 1 calc PR A 2 H10B H 0.4665 -1.3960 0.9866 0.105 Uiso 0.50(3) 1 calc PR A 2 H10C H 0.4516 -1.3986 1.0377 0.105 Uiso 0.50(3) 1 calc PR A 2 C106 C 0.491(2) -1.174(5) 1.0830(19) 0.070 Uiso 0.50(3) 1 d PD A 2 H10D H 0.5216 -1.2063 1.1054 0.105 Uiso 0.50(3) 1 calc PR A 2 H10E H 0.4665 -1.2035 1.0967 0.105 Uiso 0.50(3) 1 calc PR A 2 H10F H 0.4913 -1.0794 1.0830 0.105 Uiso 0.50(3) 1 calc PR A 2 C107 C 0.5186(17) -1.156(5) 1.014(2) 0.070 Uiso 0.50(3) 1 d PD A 2 H10G H 0.5492 -1.1921 1.0357 0.105 Uiso 0.50(3) 1 calc PR A 2 H10H H 0.5180 -1.0639 1.0208 0.105 Uiso 0.50(3) 1 calc PR A 2 H10I H 0.5139 -1.1698 0.9765 0.105 Uiso 0.50(3) 1 calc PR A 2 N21 N 0.3608(5) -1.0623(13) 0.8317(6) 0.035(4) Uani 1 1 d D . . C21 C 0.3723(6) -1.1075(17) 0.7907(7) 0.033(4) Uani 1 1 d U . . N22 N 0.3980(5) -1.0190(14) 0.7771(6) 0.034(4) Uani 1 1 d U . . C22 C 0.3799(6) -0.9411(16) 0.8450(7) 0.026(4) Uani 1 1 d U . . H22A H 0.3775 -0.8870 0.8722 0.031 Uiso 1 1 calc R . . C23 C 0.4023(8) -0.916(2) 0.8119(8) 0.046(5) Uani 1 1 d U . . H23A H 0.4190 -0.8384 0.8118 0.056 Uiso 1 1 calc R . . C24 C 0.4215(10) -1.033(3) 0.7360(11) 0.069(7) Uani 1 1 d U . . C25 C 0.4499(8) -0.908(2) 0.7396(9) 0.056(6) Uani 1 1 d U . . H25A H 0.4282 -0.8361 0.7256 0.084 Uiso 1 1 calc R . . H25B H 0.4707 -0.9175 0.7190 0.084 Uiso 1 1 calc R . . H25C H 0.4691 -0.8910 0.7765 0.084 Uiso 1 1 calc R . . C26 C 0.4579(10) -1.139(3) 0.7528(12) 0.086(8) Uani 1 1 d U . . H26A H 0.4418 -1.2222 0.7502 0.128 Uiso 1 1 calc R . . H26B H 0.4787 -1.1249 0.7893 0.128 Uiso 1 1 calc R . . H26C H 0.4767 -1.1395 0.7298 0.128 Uiso 1 1 calc R . . C27 C 0.3858(10) -1.047(3) 0.6827(12) 0.085(8) Uani 1 1 d U . . H27A H 0.3698 -1.1306 0.6802 0.128 Uiso 1 1 calc R . . H27B H 0.4013 -1.0439 0.6565 0.128 Uiso 1 1 calc R . . H27C H 0.3625 -0.9779 0.6760 0.128 Uiso 1 1 calc R . . N31 N 0.2907(5) -1.0671(13) 0.8623(5) 0.025(3) Uani 1 1 d DU . . C31 C 0.2611(5) -1.1157(15) 0.8850(6) 0.020(3) Uani 1 1 d U . . N32 N 0.2247(5) -1.0312(13) 0.8768(5) 0.023(3) Uani 1 1 d U . . C32 C 0.2731(6) -0.9540(15) 0.8414(6) 0.023(4) Uani 1 1 d U . . H32A H 0.2882 -0.8973 0.8248 0.028 Uiso 1 1 calc R . . C33 C 0.2328(6) -0.9313(16) 0.8465(7) 0.027(4) Uani 1 1 d U . . H33A H 0.2126 -0.8602 0.8323 0.033 Uiso 1 1 calc R . . C34 C 0.1856(5) -1.0387(14) 0.8981(6) 0.015(3) Uani 1 1 d U . . C35 C 0.2076(7) -1.0401(19) 0.9601(7) 0.037(5) Uani 1 1 d . . . H35A H 0.1822 -1.0361 0.9747 0.056 Uiso 1 1 calc R . . H35B H 0.2285 -0.9657 0.9723 0.056 Uiso 1 1 calc R . . H35C H 0.2257 -1.1194 0.9719 0.056 Uiso 1 1 calc R . . C36 C 0.1562(7) -0.9194(18) 0.8812(8) 0.040(5) Uani 1 1 d . . . H36A H 0.1308 -0.9203 0.8958 0.060 Uiso 1 1 calc R . . H36B H 0.1424 -0.9167 0.8426 0.060 Uiso 1 1 calc R . . H36C H 0.1761 -0.8435 0.8941 0.060 Uiso 1 1 calc R . . C37 C 0.1543(7) -1.1514(17) 0.8745(8) 0.039(5) Uani 1 1 d . . . H37A H 0.1275 -1.1522 0.8869 0.058 Uiso 1 1 calc R . . H37B H 0.1724 -1.2312 0.8851 0.058 Uiso 1 1 calc R . . H37C H 0.1426 -1.1443 0.8360 0.058 Uiso 1 1 calc R . . N41 N 0.1294(5) -0.2258(11) 0.5420(5) 0.020(3) Uani 1 1 d D . . C41 C 0.0838(5) -0.2031(13) 0.5077(5) 0.010(3) Uani 1 1 d U . . C42 C 0.1603(6) -0.1861(14) 0.5175(7) 0.024(4) Uani 1 1 d . . . H42A H 0.1939 -0.1903 0.5315 0.029 Uiso 1 1 calc R . . N42 N 0.0870(5) -0.1498(11) 0.4616(5) 0.023(3) Uani 1 1 d . . . C43 C 0.1335(6) -0.1409(16) 0.4705(7) 0.029(4) Uani 1 1 d . . . H43A H 0.1460 -0.1059 0.4457 0.035 Uiso 1 1 calc R . . C44 C 0.0451(6) -0.1135(16) 0.4122(6) 0.024(4) Uani 1 1 d U . . C45 C 0.0648(9) -0.065(2) 0.3731(9) 0.058(6) Uani 1 1 d . . . H45A H 0.0848 -0.1309 0.3660 0.087 Uiso 1 1 calc R . . H45B H 0.0837 0.0125 0.3870 0.087 Uiso 1 1 calc R . . H45C H 0.0389 -0.0432 0.3404 0.087 Uiso 1 1 calc R . . C46 C 0.0182(7) -0.236(2) 0.3888(8) 0.042(5) Uani 1 1 d . . . H46A H 0.0075 -0.2775 0.4150 0.063 Uiso 1 1 calc R . . H46B H 0.0390 -0.2943 0.3788 0.063 Uiso 1 1 calc R . . H46C H -0.0092 -0.2140 0.3576 0.063 Uiso 1 1 calc R . . C47 C 0.0158(7) -0.010(2) 0.4257(8) 0.045(5) Uani 1 1 d U . . H47A H 0.0028 -0.0443 0.4515 0.068 Uiso 1 1 calc R . . H47B H -0.0101 0.0155 0.3937 0.068 Uiso 1 1 calc R . . H47C H 0.0358 0.0643 0.4407 0.068 Uiso 1 1 calc R . . N51 N 0.1143(4) -0.2655(12) 0.6285(5) 0.016(3) Uani 1 1 d DU . . C51 C 0.0827(6) -0.3430(15) 0.6394(6) 0.022(3) Uani 1 1 d U . . N52 N 0.0660(5) -0.2709(13) 0.6703(5) 0.024(3) Uani 1 1 d U . . C52 C 0.1152(6) -0.1506(16) 0.6532(6) 0.027(4) Uani 1 1 d U . . H52A H 0.1332 -0.0778 0.6506 0.033 Uiso 1 1 calc R . . C53 C 0.0884(6) -0.1554(16) 0.6803(6) 0.024(4) Uani 1 1 d U . . H53A H 0.0848 -0.0905 0.7033 0.029 Uiso 1 1 calc R . . C54 C 0.0293(6) -0.3183(16) 0.6950(6) 0.025(4) Uani 1 1 d U . . C55 C 0.0245(6) -0.2165(15) 0.7337(6) 0.023(4) Uani 1 1 d U . . H55A H 0.0026 -0.2473 0.7505 0.035 Uiso 1 1 calc R . . H55B H 0.0124 -0.1365 0.7146 0.035 Uiso 1 1 calc R . . H55C H 0.0555 -0.2005 0.7607 0.035 Uiso 1 1 calc R . . C56 C 0.0480(6) -0.4382(16) 0.7281(7) 0.032(4) Uani 1 1 d . . . H56A H 0.0501 -0.5090 0.7051 0.048 Uiso 1 1 calc R . . H56B H 0.0265 -0.4624 0.7465 0.048 Uiso 1 1 calc R . . H56C H 0.0794 -0.4205 0.7540 0.048 Uiso 1 1 calc R . . C57 C -0.0173(6) -0.3403(17) 0.6507(7) 0.032(4) Uani 1 1 d U . . H57A H -0.0138 -0.4098 0.6279 0.048 Uiso 1 1 calc R . . H57B H -0.0269 -0.2612 0.6299 0.048 Uiso 1 1 calc R . . H57C H -0.0415 -0.3641 0.6654 0.048 Uiso 1 1 calc R . . N61 N 0.1612(4) -0.4329(11) 0.5943(5) 0.017(3) Uani 1 1 d DU . . C61 C 0.1433(6) -0.5299(15) 0.5569(6) 0.022(3) Uani 1 1 d U . . N62 N 0.1676(5) -0.6376(12) 0.5768(6) 0.033(4) Uani 1 1 d . . . C62 C 0.1959(5) -0.4854(14) 0.6352(6) 0.022(4) Uani 1 1 d . . . H62A H 0.2145 -0.4401 0.6659 0.026 Uiso 1 1 calc R . . C63 C 0.2003(7) -0.609(2) 0.6265(8) 0.044(5) Uani 1 1 d U . . H63A H 0.2219 -0.6672 0.6498 0.053 Uiso 1 1 calc R . . C64 C 0.1587(7) -0.7738(17) 0.5525(8) 0.041(5) Uani 1 1 d . . . C65 C 0.1102(6) -0.8161(17) 0.5558(7) 0.032(4) Uani 1 1 d U . . H65A H 0.1124 -0.8171 0.5927 0.048 Uiso 1 1 calc R . . H65B H 0.1022 -0.9024 0.5407 0.048 Uiso 1 1 calc R . . H65C H 0.0856 -0.7552 0.5359 0.048 Uiso 1 1 calc R . . C66 C 0.1597(9) -0.7735(18) 0.4990(9) 0.058(7) Uani 1 1 d . . . H66A H 0.1559 -0.8616 0.4853 0.086 Uiso 1 1 calc R . . H66B H 0.1900 -0.7388 0.4995 0.086 Uiso 1 1 calc R . . H66C H 0.1339 -0.7198 0.4764 0.086 Uiso 1 1 calc R . . C67 C 0.1963(12) -0.860(3) 0.5921(13) 0.099(10) Uani 1 1 d U . . H67A H 0.1929 -0.8540 0.6267 0.149 Uiso 1 1 calc R . . H67B H 0.2279 -0.8303 0.5949 0.149 Uiso 1 1 calc R . . H67C H 0.1919 -0.9490 0.5798 0.149 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 Ga1 0.0385(13) 0.0168(10) 0.0820(17) -0.0027(10) 0.0374(12) 0.0016(9) Ga2 0.0284(10) 0.0112(8) 0.0365(11) 0.0039(8) 0.0124(9) 0.0033(7) Ga3 0.0267(10) 0.0101(8) 0.0279(10) 0.0033(7) 0.0107(8) 0.0010(7) Ga4 0.0322(11) 0.0230(9) 0.0138(9) -0.0062(7) 0.0082(8) -0.0036(8) I1 0.0718(11) 0.0271(7) 0.1515(18) -0.0053(9) 0.0809(13) 0.0044(7) I2 0.0493(8) 0.0270(6) 0.0351(7) 0.0031(5) 0.0104(6) 0.0141(6) I3 0.0507(8) 0.0222(6) 0.0329(7) 0.0023(5) 0.0144(6) 0.0015(5) I4 0.0424(7) 0.0274(6) 0.0220(6) 0.0019(5) 0.0049(5) 0.0086(5) I5 0.0628(9) 0.0146(6) 0.0656(9) -0.0044(6) 0.0448(8) -0.0091(6) S1 0.026(3) 0.053(4) 0.133(6) -0.023(4) 0.023(3) 0.010(3) S2 0.0542(16) 0.0507(16) 0.0523(16) -0.0009(9) 0.0208(10) -0.0002(9) S3 0.0225(12) 0.0189(11) 0.0218(12) 0.0013(8) 0.0066(9) -0.0014(8) S4 0.034(2) 0.028(2) 0.018(2) 0.0007(17) 0.0066(18) 0.0073(19) S5 0.039(3) 0.023(2) 0.014(2) -0.0068(16) 0.0082(18) -0.0080(18) S6 0.0273(12) 0.0250(12) 0.0244(12) -0.0031(9) 0.0095(9) 0.0016(9) B1 0.029(5) 0.029(5) 0.029(5) 0.0000(10) 0.0102(18) 0.0002(10) B2 0.013(3) 0.013(3) 0.013(3) -0.0001(10) 0.0044(15) 0.0000(10) N11 0.020(3) 0.020(3) 0.021(3) 0.0001(10) 0.0068(14) 0.0002(10) C11 0.047(5) 0.047(5) 0.047(5) -0.0001(10) 0.016(2) 0.0000(10) C12 0.040(11) 0.020(9) 0.045(11) 0.004(8) 0.016(9) 0.001(8) N12 0.055(5) 0.055(5) 0.055(5) -0.0001(10) 0.0189(19) 0.0003(10) C13 0.035(4) 0.035(4) 0.035(4) 0.0002(10) 0.0120(18) -0.0002(10) N21 0.039(9) 0.023(7) 0.056(10) 0.009(7) 0.034(8) 0.004(7) C21 0.033(4) 0.033(4) 0.033(4) -0.0001(10) 0.0119(17) 0.0000(10) N22 0.034(4) 0.034(4) 0.034(4) 0.0001(10) 0.0124(16) 0.0001(10) C22 0.026(4) 0.025(4) 0.026(4) -0.0001(10) 0.0090(16) -0.0001(10) C23 0.046(5) 0.046(5) 0.046(5) -0.0002(10) 0.016(2) 0.0003(10) C24 0.069(7) 0.069(7) 0.069(7) 0.0000(10) 0.025(3) 0.0000(10) C25 0.056(6) 0.056(6) 0.056(6) 0.0001(10) 0.020(2) -0.0001(10) C26 0.086(8) 0.086(8) 0.086(8) 0.0001(10) 0.030(3) 0.0000(10) C27 0.085(8) 0.085(8) 0.085(8) 0.0000(10) 0.030(3) -0.0001(10) N31 0.025(3) 0.025(3) 0.025(3) 0.0000(10) 0.0085(14) 0.0000(10) C31 0.020(3) 0.020(3) 0.020(3) -0.0001(10) 0.0068(15) 0.0000(10) N32 0.023(3) 0.023(3) 0.023(3) 0.0002(10) 0.0084(14) -0.0004(10) C32 0.024(4) 0.023(4) 0.023(4) 0.0002(10) 0.0082(16) 0.0000(10) C33 0.027(4) 0.027(4) 0.027(4) 0.0003(10) 0.0096(16) -0.0001(10) C34 0.015(3) 0.015(3) 0.014(3) -0.0001(10) 0.0050(14) 0.0000(10) C35 0.040(11) 0.045(12) 0.030(10) -0.006(9) 0.018(9) 0.012(9) C36 0.036(11) 0.036(11) 0.059(13) 0.003(10) 0.030(10) 0.017(9) C37 0.047(12) 0.029(10) 0.040(11) -0.022(9) 0.015(10) -0.013(9) N41 0.027(8) 0.008(6) 0.025(7) -0.003(5) 0.011(6) -0.001(5) C41 0.010(3) 0.010(3) 0.010(3) 0.0000(7) 0.0036(12) 0.0001(7) C42 0.030(9) 0.007(7) 0.033(10) -0.006(7) 0.008(8) 0.005(7) N42 0.036(8) 0.007(6) 0.030(8) -0.002(6) 0.015(7) 0.006(6) C43 0.024(9) 0.027(9) 0.046(11) 0.016(8) 0.025(9) 0.005(7) C44 0.024(4) 0.024(4) 0.024(4) -0.0004(10) 0.0086(16) 0.0005(10) C45 0.089(19) 0.028(11) 0.059(15) 0.000(10) 0.030(14) -0.012(11) C46 0.038(11) 0.047(12) 0.038(11) -0.010(9) 0.010(9) 0.009(10) C47 0.045(5) 0.045(5) 0.045(5) 0.0001(10) 0.016(2) 0.0004(10) N51 0.017(3) 0.016(3) 0.016(3) -0.0005(10) 0.0056(13) 0.0002(10) C51 0.022(4) 0.022(4) 0.022(4) 0.0001(10) 0.0078(15) 0.0003(10) N52 0.024(3) 0.024(3) 0.023(3) 0.0001(10) 0.0086(14) 0.0001(10) C52 0.027(4) 0.027(4) 0.027(4) -0.0002(10) 0.0097(16) 0.0001(10) C53 0.024(4) 0.024(4) 0.024(4) 0.0000(10) 0.0085(16) 0.0004(10) C54 0.025(4) 0.025(4) 0.025(4) 0.0000(10) 0.0089(16) 0.0000(10) C55 0.023(4) 0.023(4) 0.023(4) -0.0001(10) 0.0084(15) 0.0001(10) C56 0.033(10) 0.022(9) 0.045(11) -0.010(8) 0.018(9) -0.005(8) C57 0.032(4) 0.032(4) 0.032(4) -0.0001(10) 0.0115(17) 0.0003(10) N61 0.017(3) 0.017(3) 0.017(3) -0.0003(10) 0.0058(13) 0.0003(10) C61 0.022(4) 0.021(4) 0.022(4) -0.0001(10) 0.0075(15) -0.0001(10) N62 0.045(9) 0.010(7) 0.039(9) 0.002(6) 0.010(7) -0.006(6) C62 0.022(9) 0.014(8) 0.019(8) 0.006(6) -0.005(7) 0.002(7) C63 0.044(5) 0.044(5) 0.044(5) -0.0003(10) 0.016(2) 0.0001(10) C64 0.044(12) 0.019(9) 0.048(12) -0.005(9) 0.003(10) -0.005(8) C65 0.032(4) 0.032(4) 0.032(4) 0.0000(10) 0.0115(17) -0.0004(10) C66 0.101(19) 0.014(9) 0.077(17) -0.011(10) 0.055(15) -0.016(11) C67 0.099(10) 0.099(10) 0.100(10) -0.0001(10) 0.035(4) 0.0000(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 Ga1 S1 2.328(7) . ? Ga1 S2 2.370(6) . ? Ga1 Ga2 2.406(3) . ? Ga1 I1 2.631(2) . ? Ga2 Ga3 2.412(2) . ? Ga2 I2 2.624(2) . ? Ga2 I3 2.638(2) . ? Ga3 S3 2.385(4) . ? Ga3 I4 2.594(2) . ? Ga3 I5 2.637(2) . ? Ga4 S6 2.293(5) . ? Ga4 S4 2.306(5) . ? Ga4 S5 2.312(4) . ? Ga4 Ga4 2.396(4) 3_546 ? S1 C11 1.74(2) . ? S2 C21 1.740(19) . ? S3 C31 1.740(16) . ? S4 C41 1.726(14) . ? S5 C51 1.723(16) . ? S6 C61 1.722(16) . ? B1 H1 1.098(16) . ? B1 N11 1.43(2) . ? B1 N21 1.53(2) . ? B1 N31 1.58(2) . ? B2 H2 1.087(16) . ? B2 N41 1.50(2) . ? B2 N51 1.568(19) . ? B2 N61 1.601(19) . ? N11 C11 1.39(2) . ? N11 C12 1.44(2) . ? C11 N12 1.40(3) . ? C12 C13 1.30(3) . ? N12 C13 1.39(3) . ? N12 C104 1.49(3) . ? N12 C14 1.60(4) . ? C14 C17 1.49(3) . ? C14 C16 1.49(3) . ? C14 C15 1.49(3) . ? C104 C106 1.52(3) . ? C104 C105 1.52(3) . ? C104 C107 1.52(3) . ? N21 C21 1.36(2) . ? N21 C22 1.38(2) . ? C21 N22 1.34(2) . ? N22 C23 1.40(3) . ? N22 C24 1.53(3) . ? C22 C23 1.33(3) . ? C24 C27 1.48(4) . ? C24 C26 1.52(4) . ? C24 C25 1.54(3) . ? N31 C32 1.33(2) . ? N31 C31 1.35(2) . ? C31 N32 1.36(2) . ? N32 C33 1.40(2) . ? N32 C34 1.490(19) . ? C32 C33 1.30(2) . ? C34 C37 1.50(2) . ? C34 C36 1.50(2) . ? C34 C35 1.57(2) . ? N41 C42 1.38(2) . ? N41 C41 1.385(18) . ? C41 N42 1.400(19) . ? C42 C43 1.33(2) . ? N42 C43 1.34(2) . ? N42 C44 1.53(2) . ? C44 C45 1.48(3) . ? C44 C47 1.52(2) . ? C44 C46 1.52(3) . ? N51 C51 1.36(2) . ? N51 C52 1.36(2) . ? C51 N52 1.35(2) . ? N52 C53 1.36(2) . ? N52 C54 1.57(2) . ? C52 C53 1.27(2) . ? C54 C57 1.51(2) . ? C54 C56 1.52(2) . ? C54 C55 1.53(2) . ? N61 C62 1.345(19) . ? N61 C61 1.40(2) . ? C61 N62 1.34(2) . ? N62 C63 1.39(2) . ? N62 C64 1.54(2) . ? C62 C63 1.32(3) . ? C64 C66 1.46(3) . ? C64 C67 1.54(4) . ? C64 C65 1.56(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 Ga1 S2 104.8(3) . . ? S1 Ga1 Ga2 126.7(2) . . ? S2 Ga1 Ga2 112.07(18) . . ? S1 Ga1 I1 94.64(16) . . ? S2 Ga1 I1 99.55(17) . . ? Ga2 Ga1 I1 114.84(9) . . ? Ga1 Ga2 Ga3 119.23(9) . . ? Ga1 Ga2 I2 111.33(10) . . ? Ga3 Ga2 I2 105.78(8) . . ? Ga1 Ga2 I3 103.41(9) . . ? Ga3 Ga2 I3 107.01(9) . . ? I2 Ga2 I3 109.83(7) . . ? S3 Ga3 Ga2 112.90(13) . . ? S3 Ga3 I4 105.39(11) . . ? Ga2 Ga3 I4 117.43(9) . . ? S3 Ga3 I5 98.10(11) . . ? Ga2 Ga3 I5 115.62(8) . . ? I4 Ga3 I5 105.20(8) . . ? S6 Ga4 S4 106.06(17) . . ? S6 Ga4 S5 103.67(17) . . ? S4 Ga4 S5 105.39(16) . . ? S6 Ga4 Ga4 112.86(15) . 3_546 ? S4 Ga4 Ga4 110.91(16) . 3_546 ? S5 Ga4 Ga4 117.06(15) . 3_546 ? C11 S1 Ga1 112.2(8) . . ? C21 S2 Ga1 103.7(7) . . ? C31 S3 Ga3 102.7(5) . . ? C41 S4 Ga4 97.9(5) . . ? C51 S5 Ga4 100.1(6) . . ? C61 S6 Ga4 101.7(6) . . ? H1 B1 N11 115(2) . . ? H1 B1 N21 107(2) . . ? N11 B1 N21 110.5(15) . . ? H1 B1 N31 104(2) . . ? N11 B1 N31 111.4(14) . . ? N21 B1 N31 109.2(14) . . ? H2 B2 N41 110.0(18) . . ? H2 B2 N51 105.5(18) . . ? N41 B2 N51 114.0(12) . . ? H2 B2 N61 103.7(18) . . ? N41 B2 N61 111.9(11) . . ? N51 B2 N61 111.0(11) . . ? C11 N11 B1 126.2(15) . . ? C11 N11 C12 105.8(14) . . ? B1 N11 C12 127.7(14) . . ? N11 C11 N12 107.2(17) . . ? N11 C11 S1 122.7(15) . . ? N12 C11 S1 129.6(17) . . ? C13 C12 N11 109.5(16) . . ? C13 N12 C11 107.7(18) . . ? C13 N12 C104 135(2) . . ? C11 N12 C104 117(2) . . ? C13 N12 C14 120.1(18) . . ? C11 N12 C14 128.8(19) . . ? C104 N12 C14 24.2(15) . . ? C12 C13 N12 109.7(18) . . ? C17 C14 C16 112.0(14) . . ? C17 C14 C15 112.0(14) . . ? C16 C14 C15 112.0(14) . . ? C17 C14 N12 111(3) . . ? C16 C14 N12 105(3) . . ? C15 C14 N12 104(2) . . ? N12 C104 C106 105(3) . . ? N12 C104 C105 107(3) . . ? C106 C104 C105 113(4) . . ? N12 C104 C107 113(3) . . ? C106 C104 C107 99(3) . . ? C105 C104 C107 119(4) . . ? C21 N21 C22 109.0(14) . . ? C21 N21 B1 130.5(14) . . ? C22 N21 B1 119.4(14) . . ? N22 C21 N21 109.1(16) . . ? N22 C21 S2 127.0(14) . . ? N21 C21 S2 123.8(14) . . ? C21 N22 C23 105.5(16) . . ? C21 N22 C24 127.1(17) . . ? C23 N22 C24 127.1(17) . . ? C23 C22 N21 105.7(16) . . ? C22 C23 N22 110.7(18) . . ? C27 C24 C26 115(2) . . ? C27 C24 N22 111(2) . . ? C26 C24 N22 109(2) . . ? C27 C24 C25 111(2) . . ? C26 C24 C25 105(2) . . ? N22 C24 C25 106(2) . . ? C32 N31 C31 107.3(13) . . ? C32 N31 B1 129.4(14) . . ? C31 N31 B1 122.9(13) . . ? N31 C31 N32 108.1(13) . . ? N31 C31 S3 125.7(12) . . ? N32 C31 S3 126.2(12) . . ? C31 N32 C33 106.0(13) . . ? C31 N32 C34 127.5(13) . . ? C33 N32 C34 126.4(13) . . ? C33 C32 N31 111.3(15) . . ? C32 C33 N32 107.1(15) . . ? N32 C34 C37 110.0(13) . . ? N32 C34 C36 107.7(12) . . ? C37 C34 C36 107.3(14) . . ? N32 C34 C35 108.6(12) . . ? C37 C34 C35 114.5(14) . . ? C36 C34 C35 108.4(14) . . ? C42 N41 C41 108.0(12) . . ? C42 N41 B2 120.5(12) . . ? C41 N41 B2 131.5(12) . . ? N41 C41 N42 107.6(12) . . ? N41 C41 S4 127.1(10) . . ? N42 C41 S4 125.2(11) . . ? C43 C42 N41 106.0(14) . . ? C43 N42 C41 105.2(13) . . ? C43 N42 C44 129.2(13) . . ? C41 N42 C44 125.7(13) . . ? C42 C43 N42 113.2(15) . . ? C45 C44 C47 110.4(16) . . ? C45 C44 C46 106.2(15) . . ? C47 C44 C46 114.8(15) . . ? C45 C44 N42 107.1(15) . . ? C47 C44 N42 109.7(14) . . ? C46 C44 N42 108.4(13) . . ? C51 N51 C52 107.8(13) . . ? C51 N51 B2 133.5(12) . . ? C52 N51 B2 118.7(12) . . ? N52 C51 N51 104.5(13) . . ? N52 C51 S5 128.9(12) . . ? N51 C51 S5 126.4(12) . . ? C51 N52 C53 110.4(13) . . ? C51 N52 C54 124.6(13) . . ? C53 N52 C54 124.8(13) . . ? C53 C52 N51 110.0(15) . . ? C52 C53 N52 107.0(15) . . ? C57 C54 C56 113.2(14) . . ? C57 C54 C55 111.3(14) . . ? C56 C54 C55 105.5(13) . . ? C57 C54 N52 108.1(13) . . ? C56 C54 N52 109.6(13) . . ? C55 C54 N52 109.1(13) . . ? C62 N61 C61 107.2(12) . . ? C62 N61 B2 119.9(12) . . ? C61 N61 B2 132.8(12) . . ? N62 C61 N61 107.0(13) . . ? N62 C61 S6 128.6(13) . . ? N61 C61 S6 124.4(12) . . ? C61 N62 C63 108.1(15) . . ? C61 N62 C64 127.2(15) . . ? C63 N62 C64 124.5(15) . . ? C63 C62 N61 110.3(16) . . ? C62 C63 N62 107.4(17) . . ? C66 C64 C67 115(2) . . ? C66 C64 N62 111.1(15) . . ? C67 C64 N62 105.0(18) . . ? C66 C64 C65 113.8(17) . . ? C67 C64 C65 105.9(19) . . ? N62 C64 C65 105.0(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.780 _refine_diff_density_min -2.858 _refine_diff_density_rms 0.352 # Attachment '- TmGa(GaI2)GaTmI (32s20).cif' data_32s20 _database_code_depnum_ccdc_archive 'CCDC 763461' #TrackingRef '- TmGa(GaI2)GaTmI (32s20).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H74 B2 Ga3 I3 N14 S6' _chemical_formula_weight 1627.03 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' 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 Pba2 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' _cell_length_a 14.953(2) _cell_length_b 20.106(3) _cell_length_c 11.2381(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3378.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9870 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 31.91 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 2.785 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4021 _exptl_absorpt_correction_T_max 0.7681 _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 56451 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 32.63 _reflns_number_total 11786 _reflns_number_gt 9698 _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^)+(0.0614P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.011(10) _refine_ls_number_reflns 11786 _refine_ls_number_parameters 343 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0979 _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 Ga1 Ga 1.87812(2) 0.062940(18) -0.19962(4) 0.01977(8) Uani 1 1 d . . . Ga2 Ga 2.0000 0.0000 -0.10537(5) 0.01850(10) Uani 1 2 d S . . I1 I 2.083519(18) 0.085588(14) 0.03242(3) 0.03662(7) Uani 1 1 d . . . I2 I 2.00971(4) 0.39621(3) -0.73768(6) 0.04101(14) Uani 0.50 1 d P . . S1 S 1.73036(6) 0.03959(5) -0.13916(8) 0.02458(17) Uani 1 1 d . . . S2 S 1.88064(6) 0.17916(4) -0.17499(8) 0.02293(17) Uani 1 1 d . . . S3 S 1.86929(6) 0.05190(4) -0.40729(8) 0.02283(16) Uani 1 1 d . . . B B 1.6956(3) 0.15941(19) -0.3565(4) 0.0241(8) Uani 1 1 d . . . H1 H 1.643(3) 0.189(2) -0.398(4) 0.029 Uiso 1 1 d . . . N1 N 2.2415(5) 0.6206(3) 0.3817(6) 0.0742(18) Uani 1 1 d . . . C1 C 2.2382(4) 0.5733(3) 0.3300(5) 0.0501(13) Uani 1 1 d . . . C2 C 2.2419(5) 0.5077(3) 0.2703(7) 0.078(2) Uani 1 1 d . . . H2A H 2.1819 0.4954 0.2429 0.116 Uiso 1 1 calc R . . H2B H 2.2637 0.4742 0.3266 0.116 Uiso 1 1 calc R . . H2C H 2.2826 0.5101 0.2021 0.116 Uiso 1 1 calc R . . N11 N 1.6683(2) 0.08480(14) -0.3562(3) 0.0229(6) Uani 1 1 d . . . C11 C 1.6786(2) 0.03448(17) -0.2769(3) 0.0225(7) Uani 1 1 d . . . C12 C 1.6274(2) 0.05943(18) -0.4561(4) 0.0270(7) Uani 1 1 d . . . H12A H 1.6128 0.0838 -0.5260 0.032 Uiso 1 1 calc R . . N12 N 1.6427(2) -0.02124(15) -0.3258(3) 0.0268(7) Uani 1 1 d . . . C13 C 1.6114(3) -0.00562(18) -0.4381(4) 0.0273(8) Uani 1 1 d . . . H13A H 1.5838 -0.0354 -0.4926 0.033 Uiso 1 1 calc R . . C14 C 1.6345(3) -0.08988(18) -0.2698(5) 0.0346(10) Uani 1 1 d . . . C15 C 1.5867(3) -0.1359(2) -0.3574(5) 0.0395(10) Uani 1 1 d . . . H15A H 1.5273 -0.1179 -0.3753 0.059 Uiso 1 1 calc R . . H15B H 1.5805 -0.1802 -0.3220 0.059 Uiso 1 1 calc R . . H15C H 1.6216 -0.1390 -0.4309 0.059 Uiso 1 1 calc R . . C16 C 1.7293(3) -0.1176(2) -0.2473(5) 0.0400(11) Uani 1 1 d . . . H16A H 1.7607 -0.0890 -0.1903 0.060 Uiso 1 1 calc R . . H16B H 1.7626 -0.1187 -0.3224 0.060 Uiso 1 1 calc R . . H16C H 1.7249 -0.1628 -0.2150 0.060 Uiso 1 1 calc R . . C17 C 1.5784(3) -0.0831(2) -0.1564(5) 0.0402(11) Uani 1 1 d . . . H17A H 1.5200 -0.0639 -0.1762 0.060 Uiso 1 1 calc R . . H17B H 1.6094 -0.0540 -0.0999 0.060 Uiso 1 1 calc R . . H17C H 1.5698 -0.1271 -0.1205 0.060 Uiso 1 1 calc R . . C21 C 1.7686(2) 0.19396(17) -0.1471(3) 0.0217(6) Uani 1 1 d . . . N21 N 1.7011(2) 0.18896(14) -0.2288(3) 0.0230(6) Uani 1 1 d . . . C22 C 1.6227(3) 0.20797(19) -0.1723(4) 0.0288(8) Uani 1 1 d . . . H22A H 1.5651 0.2091 -0.2080 0.035 Uiso 1 1 calc R . . N22 N 1.7328(2) 0.21572(15) -0.0429(3) 0.0251(6) Uani 1 1 d . . . C23 C 1.6412(3) 0.2245(2) -0.0588(4) 0.0294(8) Uani 1 1 d . . . H23A H 1.5996 0.2394 -0.0007 0.035 Uiso 1 1 calc R . . C24 C 1.7799(3) 0.2241(2) 0.0756(3) 0.0278(7) Uani 1 1 d . . . C25 C 1.8511(3) 0.2784(2) 0.0645(4) 0.0398(10) Uani 1 1 d . . . H25A H 1.8224 0.3206 0.0435 0.060 Uiso 1 1 calc R . . H25B H 1.8939 0.2660 0.0023 0.060 Uiso 1 1 calc R . . H25C H 1.8825 0.2832 0.1405 0.060 Uiso 1 1 calc R . . C26 C 1.8181(3) 0.1574(2) 0.1144(4) 0.0391(10) Uani 1 1 d . . . H26A H 1.8635 0.1429 0.0571 0.059 Uiso 1 1 calc R . . H26B H 1.7701 0.1243 0.1179 0.059 Uiso 1 1 calc R . . H26C H 1.8455 0.1620 0.1933 0.059 Uiso 1 1 calc R . . C27 C 1.7109(3) 0.2470(2) 0.1670(4) 0.0363(9) Uani 1 1 d . . . H27A H 1.6858 0.2899 0.1423 0.054 Uiso 1 1 calc R . . H27B H 1.7397 0.2519 0.2448 0.054 Uiso 1 1 calc R . . H27C H 1.6628 0.2140 0.1725 0.054 Uiso 1 1 calc R . . N31 N 1.7808(2) 0.17114(14) -0.4315(3) 0.0225(6) Uani 1 1 d . . . C31 C 1.8538(2) 0.13395(16) -0.4526(3) 0.0222(6) Uani 1 1 d . . . C32 C 1.7922(3) 0.23168(17) -0.4877(3) 0.0274(8) Uani 1 1 d . . . H32A H 1.7507 0.2675 -0.4878 0.033 Uiso 1 1 calc R . . N32 N 1.9118(2) 0.17022(15) -0.5190(3) 0.0240(6) Uani 1 1 d . . . C33 C 1.8732(3) 0.23117(19) -0.5429(4) 0.0290(8) Uani 1 1 d . . . H33A H 1.8983 0.2661 -0.5890 0.035 Uiso 1 1 calc R . . C34 C 2.0048(3) 0.1508(2) -0.5564(4) 0.0318(8) Uani 1 1 d . . . C35 C 2.0009(3) 0.0902(2) -0.6361(4) 0.0347(9) Uani 1 1 d . . . H35A H 1.9644 0.1002 -0.7062 0.052 Uiso 1 1 calc R . . H35B H 1.9743 0.0530 -0.5923 0.052 Uiso 1 1 calc R . . H35C H 2.0616 0.0782 -0.6613 0.052 Uiso 1 1 calc R . . C36 C 2.0463(3) 0.2085(2) -0.6262(5) 0.0429(11) Uani 1 1 d . . . H36A H 2.0499 0.2479 -0.5749 0.064 Uiso 1 1 calc R . . H36B H 2.0089 0.2186 -0.6956 0.064 Uiso 1 1 calc R . . H36C H 2.1064 0.1961 -0.6527 0.064 Uiso 1 1 calc R . . C37 C 2.0619(3) 0.1392(3) -0.4435(4) 0.0424(11) Uani 1 1 d . . . H37A H 2.0620 0.1797 -0.3949 0.064 Uiso 1 1 calc R . . H37B H 2.1233 0.1282 -0.4666 0.064 Uiso 1 1 calc R . . H37C H 2.0365 0.1024 -0.3974 0.064 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 Ga1 0.02038(16) 0.01662(15) 0.02230(17) 0.00284(14) -0.00067(14) 0.00149(13) Ga2 0.0203(2) 0.0189(2) 0.0163(2) 0.000 0.000 0.00292(19) I1 0.03436(13) 0.04007(14) 0.03544(13) -0.01814(12) -0.00562(12) -0.00018(11) I2 0.0385(3) 0.0363(3) 0.0482(3) -0.0076(3) -0.0108(3) -0.0058(2) S1 0.0220(4) 0.0236(4) 0.0282(4) 0.0046(3) -0.0014(3) -0.0026(3) S2 0.0215(4) 0.0194(4) 0.0279(4) -0.0013(3) -0.0009(3) -0.0003(3) S3 0.0295(4) 0.0167(4) 0.0224(4) 0.0027(3) 0.0006(3) 0.0028(3) B 0.030(2) 0.0157(16) 0.0261(18) -0.0013(14) -0.0051(15) 0.0016(14) N1 0.111(5) 0.037(3) 0.074(4) -0.011(2) 0.034(4) -0.004(3) C1 0.046(3) 0.045(3) 0.059(3) 0.001(2) 0.007(2) 0.002(2) C2 0.090(5) 0.066(4) 0.076(5) -0.040(3) 0.034(4) -0.038(4) N11 0.0224(14) 0.0193(13) 0.0269(15) -0.0011(11) -0.0036(12) 0.0019(11) C11 0.0196(14) 0.0184(14) 0.0296(17) -0.0006(12) -0.0022(13) 0.0013(12) C12 0.0273(17) 0.0225(16) 0.0311(19) -0.0026(15) -0.0052(15) 0.0022(13) N12 0.0244(14) 0.0174(13) 0.0387(19) -0.0012(12) -0.0051(13) -0.0004(11) C13 0.0232(16) 0.0227(16) 0.036(2) -0.0065(14) -0.0055(14) 0.0022(13) C14 0.0265(18) 0.0151(16) 0.062(3) 0.0050(16) -0.0044(18) -0.0025(13) C15 0.036(2) 0.0182(17) 0.064(3) -0.0018(18) -0.009(2) -0.0010(15) C16 0.0281(19) 0.025(2) 0.067(3) 0.0034(19) -0.008(2) 0.0037(15) C17 0.029(2) 0.029(2) 0.062(3) 0.0080(19) 0.0001(19) -0.0089(16) C21 0.0249(16) 0.0176(15) 0.0225(15) 0.0010(12) -0.0019(13) -0.0009(12) N21 0.0247(14) 0.0174(12) 0.0269(15) 0.0004(11) -0.0031(12) 0.0013(11) C22 0.0243(16) 0.0273(17) 0.035(2) -0.0006(15) -0.0016(15) 0.0027(14) N22 0.0271(15) 0.0214(14) 0.0268(15) -0.0031(12) -0.0024(12) 0.0029(11) C23 0.0239(17) 0.0320(19) 0.0324(19) -0.0033(16) 0.0028(15) 0.0023(15) C24 0.0319(19) 0.0285(18) 0.0230(16) -0.0004(14) -0.0014(14) 0.0018(15) C25 0.044(2) 0.042(2) 0.034(2) -0.0102(18) -0.0023(18) -0.014(2) C26 0.043(2) 0.040(2) 0.034(2) 0.0055(18) -0.0016(18) 0.0142(19) C27 0.042(2) 0.041(2) 0.0260(19) -0.0016(16) -0.0009(17) 0.0093(18) N31 0.0307(15) 0.0141(12) 0.0227(14) 0.0016(10) -0.0047(11) 0.0007(11) C31 0.0281(16) 0.0182(14) 0.0204(16) -0.0003(12) -0.0038(13) 0.0008(12) C32 0.039(2) 0.0145(14) 0.0281(19) 0.0041(12) -0.0048(15) 0.0010(13) N32 0.0327(16) 0.0195(14) 0.0197(13) 0.0043(11) -0.0023(12) -0.0010(11) C33 0.043(2) 0.0190(16) 0.0247(17) 0.0053(13) -0.0039(15) -0.0001(15) C34 0.035(2) 0.031(2) 0.0290(19) 0.0083(16) 0.0007(16) -0.0051(16) C35 0.040(2) 0.032(2) 0.032(2) 0.0002(16) 0.0075(18) 0.0033(16) C36 0.045(3) 0.038(2) 0.046(3) 0.015(2) 0.008(2) -0.0055(19) C37 0.032(2) 0.051(3) 0.043(3) 0.010(2) -0.0059(18) -0.0063(19) _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 Ga1 S3 2.3481(10) . ? Ga1 S2 2.3534(10) . ? Ga1 S1 2.3589(10) . ? Ga1 Ga2 2.4586(5) . ? Ga2 Ga1 2.4586(5) 2_955 ? Ga2 I1 2.6303(5) 2_955 ? Ga2 I1 2.6303(5) . ? S1 C11 1.733(4) . ? S2 C21 1.730(4) . ? S3 C31 1.742(3) . ? B H1 1.10(5) . ? B N31 1.546(6) . ? B N11 1.555(5) . ? B N21 1.556(5) . ? N1 C1 1.115(8) . ? C1 C2 1.481(8) . ? N11 C11 1.357(5) . ? N11 C12 1.377(5) . ? C11 N12 1.358(5) . ? C12 C13 1.345(5) . ? N12 C13 1.382(5) . ? N12 C14 1.522(5) . ? C14 C15 1.528(6) . ? C14 C17 1.532(7) . ? C14 C16 1.546(6) . ? C21 N22 1.360(5) . ? C21 N21 1.367(5) . ? N21 C22 1.388(5) . ? C22 C23 1.346(6) . ? N22 C23 1.393(5) . ? N22 C24 1.516(5) . ? C24 C26 1.522(6) . ? C24 C27 1.527(6) . ? C24 C25 1.530(6) . ? N31 C31 1.344(5) . ? N31 C32 1.382(4) . ? C31 N32 1.358(5) . ? C32 C33 1.360(6) . ? N32 C33 1.381(5) . ? N32 C34 1.504(5) . ? C34 C35 1.512(6) . ? C34 C36 1.532(6) . ? C34 C37 1.547(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Ga1 S2 102.22(3) . . ? S3 Ga1 S1 102.40(4) . . ? S2 Ga1 S1 100.30(3) . . ? S3 Ga1 Ga2 114.91(3) . . ? S2 Ga1 Ga2 116.65(3) . . ? S1 Ga1 Ga2 117.89(3) . . ? Ga1 Ga2 Ga1 128.96(3) . 2_955 ? Ga1 Ga2 I1 103.792(15) . 2_955 ? Ga1 Ga2 I1 105.595(15) 2_955 2_955 ? Ga1 Ga2 I1 105.595(15) . . ? Ga1 Ga2 I1 103.793(15) 2_955 . ? I1 Ga2 I1 107.87(3) 2_955 . ? C11 S1 Ga1 99.97(12) . . ? C21 S2 Ga1 100.17(12) . . ? C31 S3 Ga1 102.02(12) . . ? H1 B N31 106(2) . . ? H1 B N11 110(2) . . ? N31 B N11 111.4(3) . . ? H1 B N21 103(3) . . ? N31 B N21 113.6(3) . . ? N11 B N21 112.3(3) . . ? N1 C1 C2 173.5(8) . . ? C11 N11 C12 108.1(3) . . ? C11 N11 B 133.7(3) . . ? C12 N11 B 118.2(3) . . ? N11 C11 N12 107.7(3) . . ? N11 C11 S1 126.3(3) . . ? N12 C11 S1 125.9(3) . . ? C13 C12 N11 108.4(4) . . ? C11 N12 C13 108.4(3) . . ? C11 N12 C14 127.8(3) . . ? C13 N12 C14 123.8(3) . . ? C12 C13 N12 107.4(3) . . ? N12 C14 C15 108.7(4) . . ? N12 C14 C17 107.9(3) . . ? C15 C14 C17 109.5(4) . . ? N12 C14 C16 108.7(3) . . ? C15 C14 C16 108.4(4) . . ? C17 C14 C16 113.5(4) . . ? N22 C21 N21 108.1(3) . . ? N22 C21 S2 126.3(3) . . ? N21 C21 S2 125.4(3) . . ? C21 N21 C22 107.2(3) . . ? C21 N21 B 133.4(3) . . ? C22 N21 B 118.8(3) . . ? C23 C22 N21 109.1(3) . . ? C21 N22 C23 108.5(3) . . ? C21 N22 C24 127.5(3) . . ? C23 N22 C24 123.8(3) . . ? C22 C23 N22 107.0(3) . . ? N22 C24 C26 109.2(3) . . ? N22 C24 C27 108.1(3) . . ? C26 C24 C27 109.1(3) . . ? N22 C24 C25 109.3(3) . . ? C26 C24 C25 113.0(4) . . ? C27 C24 C25 108.1(4) . . ? C31 N31 C32 108.0(3) . . ? C31 N31 B 132.9(3) . . ? C32 N31 B 119.0(3) . . ? N31 C31 N32 108.5(3) . . ? N31 C31 S3 125.7(3) . . ? N32 C31 S3 125.8(3) . . ? C33 C32 N31 108.1(3) . . ? C31 N32 C33 108.4(3) . . ? C31 N32 C34 127.2(3) . . ? C33 N32 C34 124.3(3) . . ? C32 C33 N32 106.9(3) . . ? N32 C34 C35 109.8(3) . . ? N32 C34 C36 108.6(3) . . ? C35 C34 C36 108.8(4) . . ? N32 C34 C37 108.6(3) . . ? C35 C34 C37 112.7(4) . . ? C36 C34 C37 108.1(4) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 32.63 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.885 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.127 # Attachment 'k2-Tm2GaI--tm2gais10-.cif.txt' data_tm2gais10 _database_code_depnum_ccdc_archive 'CCDC 763462' #TrackingRef 'k2-Tm2GaI--tm2gais10-.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H84 B2 Ga I N12 S6' _chemical_formula_weight 1335.95 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.730(5) _cell_length_b 11.539(2) _cell_length_c 19.666(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.550(3) _cell_angle_gamma 90.00 _cell_volume 6363.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 3092 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 21.86 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 1.161 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9336 _exptl_absorpt_correction_T_max 0.9772 _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 33678 _diffrn_reflns_av_R_equivalents 0.0997 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5626 _reflns_number_gt 3976 _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. ; _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^)+(0.0463P)^2^+35.5581P] 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 5626 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1222 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.5000 0.24331(6) 0.2500 0.01765(19) Uani 1 2 d S . . I I 0.5000 0.47068(5) 0.2500 0.03379(17) Uani 1 2 d S . . S1 S 0.55053(4) 0.14344(12) 0.19358(6) 0.0209(3) Uani 1 1 d . . . S2 S 0.55439(4) 0.27609(11) 0.36787(6) 0.0193(3) Uani 1 1 d . . . S3 S 0.68289(5) -0.10803(11) 0.45117(7) 0.0246(3) Uani 1 1 d . . . B B 0.5828(2) 0.0069(5) 0.3431(3) 0.0175(12) Uani 1 1 d . . . H1 H 0.5480(17) 0.006(4) 0.311(2) 0.021 Uiso 1 1 d . . . C11 C 0.60492(16) 0.1475(4) 0.2530(2) 0.0168(10) Uani 1 1 d . . . N11 N 0.61629(14) 0.0892(3) 0.3138(2) 0.0174(9) Uani 1 1 d . . . N12 N 0.64264(14) 0.2149(3) 0.2468(2) 0.0184(9) Uani 1 1 d . . . C12 C 0.66133(17) 0.1218(4) 0.3466(3) 0.0199(11) Uani 1 1 d . . . H12A H 0.6781 0.0949 0.3908 0.024 Uiso 1 1 calc R . . C13 C 0.67784(18) 0.1979(5) 0.3062(3) 0.0226(11) Uani 1 1 d . . . H13A H 0.7083 0.2338 0.3164 0.027 Uiso 1 1 calc R . . C14 C 0.64901(18) 0.2846(4) 0.1843(3) 0.0239(12) Uani 1 1 d . . . C15 C 0.6445(2) 0.2022(5) 0.1227(3) 0.0351(14) Uani 1 1 d . . . H15A H 0.6125 0.1680 0.1122 0.053 Uiso 1 1 calc R . . H15B H 0.6684 0.1405 0.1344 0.053 Uiso 1 1 calc R . . H15C H 0.6497 0.2450 0.0820 0.053 Uiso 1 1 calc R . . C16 C 0.61280(19) 0.3820(4) 0.1697(3) 0.0295(13) Uani 1 1 d . . . H16A H 0.5805 0.3494 0.1598 0.044 Uiso 1 1 calc R . . H16B H 0.6176 0.4268 0.1294 0.044 Uiso 1 1 calc R . . H16C H 0.6169 0.4328 0.2105 0.044 Uiso 1 1 calc R . . C17 C 0.69897(19) 0.3360(5) 0.1997(3) 0.0330(14) Uani 1 1 d . . . H17A H 0.7025 0.3893 0.2393 0.050 Uiso 1 1 calc R . . H17B H 0.7041 0.3782 0.1587 0.050 Uiso 1 1 calc R . . H17C H 0.7225 0.2735 0.2111 0.050 Uiso 1 1 calc R . . N21 N 0.57589(13) 0.0529(3) 0.4147(2) 0.0170(9) Uani 1 1 d . . . C21 C 0.56059(16) 0.1612(4) 0.4257(2) 0.0167(10) Uani 1 1 d . . . N22 N 0.55195(13) 0.1642(3) 0.4918(2) 0.0178(9) Uani 1 1 d . . . C22 C 0.57571(18) -0.0118(4) 0.4732(3) 0.0231(12) Uani 1 1 d . . . H22A H 0.5845 -0.0911 0.4795 0.028 Uiso 1 1 calc R . . C23 C 0.56109(17) 0.0552(4) 0.5202(3) 0.0223(11) Uani 1 1 d . . . H23A H 0.5576 0.0316 0.5651 0.027 Uiso 1 1 calc R . . C24 C 0.53575(18) 0.2665(4) 0.5284(3) 0.0220(11) Uani 1 1 d . . . C25 C 0.5322(2) 0.2280(5) 0.6020(3) 0.0359(14) Uani 1 1 d . . . H25A H 0.5084 0.1662 0.5986 0.054 Uiso 1 1 calc R . . H25B H 0.5227 0.2940 0.6272 0.054 Uiso 1 1 calc R . . H25C H 0.5633 0.1992 0.6272 0.054 Uiso 1 1 calc R . . C26 C 0.48668(18) 0.3071(5) 0.4888(3) 0.0278(12) Uani 1 1 d . . . H26A H 0.4887 0.3321 0.4419 0.042 Uiso 1 1 calc R . . H26B H 0.4760 0.3722 0.5136 0.042 Uiso 1 1 calc R . . H26C H 0.4638 0.2432 0.4854 0.042 Uiso 1 1 calc R . . C27 C 0.57262(19) 0.3627(5) 0.5344(3) 0.0314(13) Uani 1 1 d . . . H27A H 0.5750 0.3880 0.4877 0.047 Uiso 1 1 calc R . . H27B H 0.6037 0.3339 0.5596 0.047 Uiso 1 1 calc R . . H27C H 0.5629 0.4284 0.5598 0.047 Uiso 1 1 calc R . . N31 N 0.60050(14) -0.1211(3) 0.3497(2) 0.0185(9) Uani 1 1 d . . . C31 C 0.64020(17) -0.1727(4) 0.3898(2) 0.0179(11) Uani 1 1 d . . . N32 N 0.63757(14) -0.2886(3) 0.3723(2) 0.0201(9) Uani 1 1 d . . . C32 C 0.57496(18) -0.2053(5) 0.3080(3) 0.0245(12) Uani 1 1 d . . . H32A H 0.5460 -0.1929 0.2748 0.029 Uiso 1 1 calc R . . C33 C 0.59688(18) -0.3063(5) 0.3212(3) 0.0270(12) Uani 1 1 d . . . H33A H 0.5865 -0.3781 0.2995 0.032 Uiso 1 1 calc R . . C34 C 0.67284(19) -0.3825(4) 0.4019(3) 0.0242(12) Uani 1 1 d . . . C35 C 0.6754(2) -0.3925(5) 0.4804(3) 0.0365(15) Uani 1 1 d . . . H35A H 0.6438 -0.4110 0.4884 0.055 Uiso 1 1 calc R . . H35B H 0.6864 -0.3187 0.5031 0.055 Uiso 1 1 calc R . . H35C H 0.6979 -0.4541 0.5000 0.055 Uiso 1 1 calc R . . C36 C 0.6553(2) -0.4966(5) 0.3677(3) 0.0410(16) Uani 1 1 d . . . H36A H 0.6535 -0.4913 0.3175 0.061 Uiso 1 1 calc R . . H36B H 0.6236 -0.5137 0.3760 0.061 Uiso 1 1 calc R . . H36C H 0.6774 -0.5586 0.3875 0.061 Uiso 1 1 calc R . . C37 C 0.72152(18) -0.3542(5) 0.3872(3) 0.0302(13) Uani 1 1 d . . . H37A H 0.7188 -0.3484 0.3367 0.045 Uiso 1 1 calc R . . H37B H 0.7442 -0.4158 0.4061 0.045 Uiso 1 1 calc R . . H37C H 0.7329 -0.2803 0.4092 0.045 Uiso 1 1 calc R . . C41 C 0.68125(18) -0.1844(5) 0.1624(3) 0.0293(13) Uani 1 1 d . . . C42 C 0.69282(19) -0.3010(5) 0.1671(3) 0.0304(13) Uani 1 1 d . . . H42A H 0.6916 -0.3424 0.2084 0.036 Uiso 1 1 calc R . . C43 C 0.70612(19) -0.3579(5) 0.1126(3) 0.0332(13) Uani 1 1 d . . . H43A H 0.7147 -0.4374 0.1170 0.040 Uiso 1 1 calc R . . C44 C 0.7069(2) -0.2994(5) 0.0519(3) 0.0395(15) Uani 1 1 d . . . H44A H 0.7156 -0.3385 0.0140 0.047 Uiso 1 1 calc R . . C45 C 0.6953(3) -0.1862(6) 0.0468(3) 0.0504(18) Uani 1 1 d . . . H45A H 0.6962 -0.1455 0.0051 0.060 Uiso 1 1 calc R . . C46 C 0.6824(2) -0.1291(5) 0.1006(3) 0.0377(15) Uani 1 1 d . . . H46A H 0.6741 -0.0494 0.0955 0.045 Uiso 1 1 calc R . . C47 C 0.6679(2) -0.1207(6) 0.2215(3) 0.0503(18) Uani 1 1 d . . . H47A H 0.6689 -0.1739 0.2606 0.075 Uiso 1 1 calc R . . H47B H 0.6356 -0.0893 0.2065 0.075 Uiso 1 1 calc R . . H47C H 0.6904 -0.0570 0.2362 0.075 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 0.0138(4) 0.0190(4) 0.0195(4) 0.000 0.0022(3) 0.000 I 0.0327(3) 0.0291(3) 0.0352(3) 0.000 -0.0024(2) 0.000 S1 0.0189(6) 0.0304(7) 0.0123(6) -0.0010(6) 0.0006(5) 0.0018(6) S2 0.0198(6) 0.0190(6) 0.0174(6) 0.0007(5) 0.0000(5) -0.0014(5) S3 0.0271(7) 0.0209(7) 0.0206(7) -0.0016(5) -0.0062(6) 0.0009(6) B 0.018(3) 0.019(3) 0.016(3) 0.000(2) 0.004(2) 0.003(2) C11 0.017(2) 0.020(3) 0.014(2) 0.001(2) 0.004(2) 0.006(2) N11 0.018(2) 0.018(2) 0.017(2) -0.0008(17) 0.0058(18) 0.0019(17) N12 0.018(2) 0.022(2) 0.016(2) 0.0053(17) 0.0054(17) 0.0043(18) C12 0.017(3) 0.023(3) 0.018(3) 0.004(2) -0.001(2) 0.004(2) C13 0.017(3) 0.032(3) 0.019(3) 0.002(2) 0.003(2) 0.001(2) C14 0.028(3) 0.025(3) 0.021(3) 0.006(2) 0.009(2) 0.000(2) C15 0.045(4) 0.039(3) 0.026(3) 0.002(3) 0.019(3) -0.003(3) C16 0.034(3) 0.023(3) 0.029(3) 0.008(2) 0.002(3) 0.004(2) C17 0.028(3) 0.037(4) 0.038(3) 0.014(3) 0.014(3) 0.003(3) N21 0.016(2) 0.018(2) 0.016(2) 0.0012(17) 0.0013(17) -0.0013(17) C21 0.009(2) 0.022(3) 0.018(2) -0.004(2) 0.0012(19) -0.005(2) N22 0.015(2) 0.023(2) 0.015(2) 0.0006(17) 0.0031(17) -0.0002(17) C22 0.025(3) 0.024(3) 0.022(3) 0.008(2) 0.009(2) 0.002(2) C23 0.026(3) 0.028(3) 0.015(3) 0.008(2) 0.010(2) 0.000(2) C24 0.022(3) 0.028(3) 0.016(3) -0.002(2) 0.004(2) 0.003(2) C25 0.037(3) 0.046(4) 0.025(3) -0.004(3) 0.008(3) 0.012(3) C26 0.023(3) 0.035(3) 0.025(3) -0.004(2) 0.004(2) 0.006(3) C27 0.033(3) 0.030(3) 0.028(3) -0.009(3) 0.001(2) 0.002(3) N31 0.015(2) 0.024(2) 0.016(2) -0.0028(18) 0.0033(17) -0.0027(17) C31 0.018(3) 0.020(3) 0.016(3) -0.002(2) 0.005(2) 0.000(2) N32 0.021(2) 0.019(2) 0.020(2) -0.0044(18) 0.0038(18) -0.0001(18) C32 0.017(3) 0.032(3) 0.022(3) -0.008(2) -0.001(2) -0.006(2) C33 0.021(3) 0.025(3) 0.033(3) -0.013(2) 0.003(2) -0.006(2) C34 0.031(3) 0.018(3) 0.024(3) 0.000(2) 0.007(2) 0.004(2) C35 0.059(4) 0.024(3) 0.030(3) 0.009(3) 0.017(3) 0.005(3) C36 0.051(4) 0.026(3) 0.043(4) -0.004(3) 0.004(3) 0.003(3) C37 0.031(3) 0.037(3) 0.023(3) 0.004(3) 0.005(2) 0.014(3) C41 0.022(3) 0.039(3) 0.026(3) -0.007(3) 0.004(2) -0.002(2) C42 0.030(3) 0.035(3) 0.022(3) 0.010(3) -0.004(2) -0.009(3) C43 0.029(3) 0.026(3) 0.043(4) -0.006(3) 0.003(3) -0.003(3) C44 0.049(4) 0.041(4) 0.032(3) -0.014(3) 0.016(3) -0.012(3) C45 0.085(5) 0.038(4) 0.031(4) 0.005(3) 0.018(4) -0.008(4) C46 0.045(4) 0.027(3) 0.040(4) 0.003(3) 0.007(3) 0.001(3) C47 0.046(4) 0.059(5) 0.048(4) -0.014(3) 0.016(3) 0.003(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 S1 2.3166(13) 2_655 ? Ga S1 2.3167(13) . ? Ga S2 2.5266(12) 2_655 ? Ga S2 2.5266(12) . ? Ga I 2.6235(10) . ? S1 C11 1.737(5) . ? S2 C21 1.730(5) . ? S3 C31 1.696(5) . ? B H1 1.06(5) . ? B N11 1.550(7) . ? B N21 1.556(7) . ? B N31 1.559(7) . ? C11 N11 1.349(6) . ? C11 N12 1.361(6) . ? N11 C12 1.367(6) . ? N12 C13 1.382(6) . ? N12 C14 1.513(6) . ? C12 C13 1.339(7) . ? C14 C16 1.516(7) . ? C14 C15 1.523(7) . ? C14 C17 1.521(7) . ? N21 C21 1.358(6) . ? N21 C22 1.373(6) . ? C21 N22 1.377(6) . ? N22 C23 1.378(6) . ? N22 C24 1.508(6) . ? C22 C23 1.339(7) . ? C24 C27 1.521(7) . ? C24 C26 1.529(7) . ? C24 C25 1.539(7) . ? N31 C31 1.374(6) . ? N31 C32 1.376(6) . ? C31 N32 1.379(6) . ? N32 C33 1.381(6) . ? N32 C34 1.511(6) . ? C32 C33 1.323(7) . ? C34 C36 1.514(7) . ? C34 C37 1.524(7) . ? C34 C35 1.534(7) . ? C41 C46 1.378(8) . ? C41 C42 1.383(8) . ? C41 C47 1.495(8) . ? C42 C43 1.380(8) . ? C43 C44 1.376(8) . ? C44 C45 1.346(9) . ? C45 C46 1.365(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ga S1 120.34(7) 2_655 . ? S1 Ga S2 100.77(4) 2_655 2_655 ? S1 Ga S2 87.82(4) . 2_655 ? S1 Ga S2 87.83(4) 2_655 . ? S1 Ga S2 100.77(4) . . ? S2 Ga S2 162.78(6) 2_655 . ? S1 Ga I 119.83(4) 2_655 . ? S1 Ga I 119.83(4) . . ? S2 Ga I 81.39(3) 2_655 . ? S2 Ga I 81.39(3) . . ? C11 S1 Ga 103.29(16) . . ? C21 S2 Ga 116.29(16) . . ? H1 B N11 111(3) . . ? H1 B N21 105(3) . . ? N11 B N21 109.8(4) . . ? H1 B N31 107(3) . . ? N11 B N31 113.1(4) . . ? N21 B N31 110.6(4) . . ? N11 C11 N12 108.7(4) . . ? N11 C11 S1 126.3(4) . . ? N12 C11 S1 124.9(3) . . ? C11 N11 C12 107.6(4) . . ? C11 N11 B 125.8(4) . . ? C12 N11 B 126.4(4) . . ? C11 N12 C13 107.1(4) . . ? C11 N12 C14 128.1(4) . . ? C13 N12 C14 124.5(4) . . ? C13 C12 N11 108.7(4) . . ? C12 C13 N12 107.8(4) . . ? N12 C14 C16 110.4(4) . . ? N12 C14 C15 108.0(4) . . ? C16 C14 C15 112.1(5) . . ? N12 C14 C17 108.7(4) . . ? C16 C14 C17 109.2(4) . . ? C15 C14 C17 108.4(4) . . ? C21 N21 C22 107.9(4) . . ? C21 N21 B 124.5(4) . . ? C22 N21 B 126.7(4) . . ? N21 C21 N22 107.7(4) . . ? N21 C21 S2 126.3(4) . . ? N22 C21 S2 126.0(4) . . ? C21 N22 C23 107.6(4) . . ? C21 N22 C24 127.4(4) . . ? C23 N22 C24 125.0(4) . . ? C23 C22 N21 108.9(4) . . ? C22 C23 N22 108.0(4) . . ? N22 C24 C27 109.1(4) . . ? N22 C24 C26 110.0(4) . . ? C27 C24 C26 111.4(4) . . ? N22 C24 C25 108.2(4) . . ? C27 C24 C25 109.0(4) . . ? C26 C24 C25 109.0(4) . . ? C31 N31 C32 107.7(4) . . ? C31 N31 B 132.4(4) . . ? C32 N31 B 119.9(4) . . ? N31 C31 N32 106.5(4) . . ? N31 C31 S3 126.8(4) . . ? N32 C31 S3 126.6(4) . . ? C31 N32 C33 108.5(4) . . ? C31 N32 C34 127.1(4) . . ? C33 N32 C34 124.4(4) . . ? C33 C32 N31 109.6(4) . . ? C32 C33 N32 107.7(4) . . ? C36 C34 N32 108.8(4) . . ? C36 C34 C37 109.4(5) . . ? N32 C34 C37 109.8(4) . . ? C36 C34 C35 108.7(4) . . ? N32 C34 C35 108.9(4) . . ? C37 C34 C35 111.2(5) . . ? C46 C41 C42 117.2(5) . . ? C46 C41 C47 121.1(6) . . ? C42 C41 C47 121.6(5) . . ? C43 C42 C41 120.9(5) . . ? C44 C43 C42 120.0(6) . . ? C45 C44 C43 119.3(6) . . ? C44 C45 C46 121.0(6) . . ? C45 C46 C41 121.5(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.667 _refine_diff_density_min -1.175 _refine_diff_density_rms 0.108 # Attachment '- TmGaBCF (sqp).cif' data_sqp _database_code_depnum_ccdc_archive 'CCDC 763463' #TrackingRef '- TmGaBCF (sqp).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H43 B2 F15 Ga N9 S3' _chemical_formula_weight 1182.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 16.5444(8) _cell_length_b 16.5444(8) _cell_length_c 11.2559(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2668.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9962 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 30.43 _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.727 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9114 _exptl_absorpt_correction_T_max 0.9509 _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 42826 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 30.50 _reflns_number_total 5435 _reflns_number_gt 4185 _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 bond has been restrained to 1.1 Angstroms. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.002 655.5 131.6 _platon_squeeze_details ; The unit cell contains 6 acetonitrile molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _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^+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 5435 _refine_ls_number_parameters 200 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 0.3333 0.6667 -0.37511(2) 0.01413(7) Uani 1 3 d S . . S S 0.40046(2) 0.81309(2) -0.47071(3) 0.01734(8) Uani 1 1 d . . . B1 B 0.3333 0.6667 -0.7113(3) 0.0213(6) Uani 1 3 d SD . . H1 H 0.3333 0.6667 -0.8069(15) 0.026 Uiso 1 3 d SD . . B2 B 0.3333 0.6667 -0.1817(2) 0.0162(5) Uani 1 3 d S . . F1 F 0.26581(6) 0.49546(6) -0.02191(8) 0.0249(2) Uani 1 1 d . . . F2 F 0.09074(7) 0.36921(7) 0.01800(9) 0.0329(2) Uani 1 1 d . . . F3 F -0.05180(6) 0.38438(7) -0.07946(9) 0.0334(2) Uani 1 1 d . . . F4 F -0.01156(6) 0.53797(7) -0.21318(8) 0.0315(2) Uani 1 1 d . . . F5 F 0.16539(6) 0.66894(6) -0.25247(7) 0.02097(19) Uani 1 1 d . . . N11 N 0.29853(9) 0.73414(9) -0.67276(10) 0.0197(3) Uani 1 1 d . . . C11 C 0.32030(10) 0.79396(10) -0.58072(13) 0.0182(3) Uani 1 1 d . . . N12 N 0.26865(9) 0.83687(9) -0.59072(11) 0.0204(3) Uani 1 1 d . . . C12 C 0.23160(11) 0.73946(12) -0.74064(14) 0.0255(3) Uani 1 1 d . . . H12A H 0.2033 0.7043 -0.8105 0.031 Uiso 1 1 calc R . . C13 C 0.21337(12) 0.80220(12) -0.69165(14) 0.0264(3) Uani 1 1 d . . . H13A H 0.1705 0.8199 -0.7205 0.032 Uiso 1 1 calc R . . C14 C 0.26905(11) 0.90948(11) -0.50886(14) 0.0229(3) Uani 1 1 d . . . C15 C 0.36715(12) 0.99413(11) -0.50385(16) 0.0294(4) Uani 1 1 d . . . H15A H 0.3868 1.0198 -0.5840 0.044 Uiso 1 1 calc R . . H15B H 0.4105 0.9753 -0.4724 0.044 Uiso 1 1 calc R . . H15C H 0.3672 1.0417 -0.4520 0.044 Uiso 1 1 calc R . . C16 C 0.23461(12) 0.86647(12) -0.38631(14) 0.0285(4) Uani 1 1 d . . . H16A H 0.1716 0.8125 -0.3931 0.043 Uiso 1 1 calc R . . H16B H 0.2335 0.9129 -0.3334 0.043 Uiso 1 1 calc R . . H16C H 0.2767 0.8464 -0.3537 0.043 Uiso 1 1 calc R . . C17 C 0.20251(13) 0.93938(12) -0.55930(17) 0.0345(4) Uani 1 1 d . . . H17A H 0.1393 0.8853 -0.5630 0.052 Uiso 1 1 calc R . . H17B H 0.2228 0.9648 -0.6393 0.052 Uiso 1 1 calc R . . H17C H 0.2026 0.9873 -0.5080 0.052 Uiso 1 1 calc R . . C21 C 0.22667(10) 0.58824(10) -0.14561(12) 0.0168(3) Uani 1 1 d . . . C22 C 0.20062(10) 0.50999(10) -0.07519(13) 0.0193(3) Uani 1 1 d . . . C23 C 0.10935(11) 0.44247(11) -0.05239(13) 0.0227(3) Uani 1 1 d . . . C24 C 0.03731(10) 0.45003(11) -0.10055(14) 0.0236(3) Uani 1 1 d . . . C25 C 0.05798(10) 0.52685(11) -0.16884(13) 0.0213(3) Uani 1 1 d . . . C26 C 0.15017(10) 0.59299(10) -0.18820(12) 0.0178(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga 0.01615(9) 0.01615(9) 0.01007(12) 0.000 0.000 0.00808(5) S 0.01929(18) 0.01634(17) 0.01466(16) 0.00080(13) -0.00228(13) 0.00760(14) B1 0.0256(9) 0.0256(9) 0.0126(13) 0.000 0.000 0.0128(5) B2 0.0191(8) 0.0191(8) 0.0106(12) 0.000 0.000 0.0095(4) F1 0.0256(5) 0.0300(5) 0.0204(4) 0.0091(4) 0.0002(4) 0.0148(4) F2 0.0336(6) 0.0263(5) 0.0322(5) 0.0150(4) 0.0068(4) 0.0100(4) F3 0.0198(5) 0.0330(5) 0.0340(5) 0.0057(4) 0.0044(4) 0.0032(4) F4 0.0202(5) 0.0434(6) 0.0315(5) 0.0064(4) 0.0005(4) 0.0163(4) F5 0.0244(5) 0.0245(5) 0.0179(4) 0.0042(3) 0.0020(3) 0.0152(4) N11 0.0227(6) 0.0235(7) 0.0126(6) 0.0015(5) -0.0021(5) 0.0115(5) C11 0.0189(7) 0.0173(7) 0.0160(7) 0.0039(5) 0.0008(5) 0.0074(6) N12 0.0228(7) 0.0195(6) 0.0192(6) 0.0035(5) -0.0007(5) 0.0107(5) C12 0.0261(8) 0.0321(9) 0.0174(7) 0.0026(6) -0.0056(6) 0.0138(7) C13 0.0262(8) 0.0313(9) 0.0227(8) 0.0045(7) -0.0052(6) 0.0151(7) C14 0.0258(8) 0.0181(7) 0.0263(8) 0.0014(6) 0.0024(6) 0.0122(6) C15 0.0276(9) 0.0177(8) 0.0407(10) 0.0028(7) 0.0060(7) 0.0095(7) C16 0.0305(9) 0.0259(8) 0.0289(9) 0.0018(7) 0.0070(7) 0.0139(7) C17 0.0331(10) 0.0282(9) 0.0488(11) 0.0026(8) -0.0007(8) 0.0202(8) C21 0.0201(7) 0.0200(7) 0.0100(6) -0.0006(5) 0.0014(5) 0.0100(6) C22 0.0218(7) 0.0236(8) 0.0139(7) 0.0004(5) 0.0005(5) 0.0124(6) C23 0.0271(8) 0.0220(8) 0.0165(7) 0.0041(6) 0.0038(6) 0.0103(7) C24 0.0169(7) 0.0250(8) 0.0202(7) 0.0000(6) 0.0044(6) 0.0039(6) C25 0.0180(7) 0.0301(8) 0.0169(7) -0.0014(6) -0.0007(6) 0.0129(7) C26 0.0222(7) 0.0195(7) 0.0125(6) 0.0014(5) 0.0019(5) 0.0109(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga B2 2.177(3) . ? Ga S 2.3599(4) 2_665 ? Ga S 2.3599(4) . ? Ga S 2.3599(4) 3_565 ? S C11 1.7241(15) . ? B1 H1 1.076(17) . ? B1 N11 1.5522(15) . ? B1 N11 1.5521(15) 2_665 ? B1 N11 1.5521(15) 3_565 ? B2 C21 1.6348(16) 3_565 ? B2 C21 1.6348(16) . ? B2 C21 1.6348(16) 2_665 ? F1 C22 1.3564(17) . ? F2 C23 1.3484(17) . ? F3 C24 1.3446(17) . ? F4 C25 1.3483(17) . ? F5 C26 1.3599(16) . ? N11 C11 1.3512(18) . ? N11 C12 1.3840(19) . ? C11 N12 1.3615(19) . ? N12 C13 1.3898(19) . ? N12 C14 1.5113(19) . ? C12 C13 1.336(2) . ? C14 C17 1.524(2) . ? C14 C15 1.525(2) . ? C14 C16 1.526(2) . ? C21 C22 1.390(2) . ? C21 C26 1.392(2) . ? C22 C23 1.381(2) . ? C23 C24 1.371(2) . ? C24 C25 1.374(2) . ? C25 C26 1.379(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B2 Ga S 117.128(10) . 2_665 ? B2 Ga S 117.127(10) . . ? S Ga S 100.844(13) 2_665 . ? B2 Ga S 117.128(10) . 3_565 ? S Ga S 100.843(13) 2_665 3_565 ? S Ga S 100.844(13) . 3_565 ? C11 S Ga 102.42(5) . . ? H1 B1 N11 106.25(11) . . ? H1 B1 N11 106.25(11) . 2_665 ? N11 B1 N11 112.49(10) . 2_665 ? H1 B1 N11 106.25(11) . 3_565 ? N11 B1 N11 112.49(10) . 3_565 ? N11 B1 N11 112.49(10) 2_665 3_565 ? C21 B2 C21 114.05(8) 3_565 . ? C21 B2 C21 114.05(8) 3_565 2_665 ? C21 B2 C21 114.05(8) . 2_665 ? C21 B2 Ga 104.38(10) 3_565 . ? C21 B2 Ga 104.38(10) . . ? C21 B2 Ga 104.38(10) 2_665 . ? C11 N11 C12 107.79(13) . . ? C11 N11 B1 133.03(13) . . ? C12 N11 B1 119.18(14) . . ? N11 C11 N12 108.15(12) . . ? N11 C11 S 125.74(11) . . ? N12 C11 S 126.11(11) . . ? C11 N12 C13 107.90(13) . . ? C11 N12 C14 127.56(12) . . ? C13 N12 C14 124.53(13) . . ? C13 C12 N11 108.67(14) . . ? C12 C13 N12 107.48(14) . . ? N12 C14 C17 108.30(13) . . ? N12 C14 C15 109.41(12) . . ? C17 C14 C15 108.99(13) . . ? N12 C14 C16 109.17(12) . . ? C17 C14 C16 109.03(14) . . ? C15 C14 C16 111.88(14) . . ? C22 C21 C26 112.44(13) . . ? C22 C21 B2 126.14(13) . . ? C26 C21 B2 121.39(12) . . ? F1 C22 C23 114.78(13) . . ? F1 C22 C21 120.90(13) . . ? C23 C22 C21 124.32(14) . . ? F2 C23 C24 119.74(14) . . ? F2 C23 C22 120.15(14) . . ? C24 C23 C22 120.11(14) . . ? F3 C24 C23 120.58(14) . . ? F3 C24 C25 120.74(14) . . ? C23 C24 C25 118.68(14) . . ? F4 C25 C24 119.90(14) . . ? F4 C25 C26 120.92(14) . . ? C24 C25 C26 119.16(14) . . ? F5 C26 C25 115.95(13) . . ? F5 C26 C21 118.81(13) . . ? C25 C26 C21 125.23(13) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.387 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.060 # Attachment '- TmGaSGaCl3 (ky165s10).cif' data_ky165s10 _database_code_depnum_ccdc_archive 'CCDC 763464' #TrackingRef '- TmGaSGaCl3 (ky165s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H40 B Cl3 Ga2 N6 S4' _chemical_formula_weight 833.49 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8552(7) _cell_length_b 12.7781(5) _cell_length_c 18.4005(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.1800(10) _cell_angle_gamma 90.00 _cell_volume 3669.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9978 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 31.80 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 1.943 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6973 _exptl_absorpt_correction_T_max 0.8294 _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 61896 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 31.81 _reflns_number_total 12471 _reflns_number_gt 8906 _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 bond has 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^)+(0.0433P)^2^+2.0375P] 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 12471 _refine_ls_number_parameters 391 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Ga1 Ga 0.309986(15) 0.752302(18) 0.809869(13) 0.01437(6) Uani 1 1 d . . . Ga2 Ga 0.320418(17) 1.02558(2) 0.761126(14) 0.01857(6) Uani 1 1 d . . . S1 S 0.40757(3) 0.62859(4) 0.86151(3) 0.01564(10) Uani 1 1 d . . . S2 S 0.23072(3) 0.80044(4) 0.89834(3) 0.01621(11) Uani 1 1 d . . . S3 S 0.21684(4) 0.65759(4) 0.72351(3) 0.01873(11) Uani 1 1 d . . . S4 S 0.38791(4) 0.87315(4) 0.76773(3) 0.02044(12) Uani 1 1 d . . . Cl1 Cl 0.29483(5) 1.08658(5) 0.86682(4) 0.03237(15) Uani 1 1 d . . . Cl2 Cl 0.40734(4) 1.13334(5) 0.71853(4) 0.03138(15) Uani 1 1 d . . . Cl3 Cl 0.19798(4) 1.03150(7) 0.68251(4) 0.03782(17) Uani 1 1 d . . . B B 0.21470(16) 0.5300(2) 0.88884(13) 0.0160(5) Uani 1 1 d D . . H1 H 0.1853(15) 0.4651(16) 0.9150(13) 0.019 Uiso 1 1 d D . . C11 C 0.36683(14) 0.61325(16) 0.94215(11) 0.0143(4) Uani 1 1 d . . . N11 N 0.29101(12) 0.56858(14) 0.94745(10) 0.0151(4) Uani 1 1 d . . . N12 N 0.40737(12) 0.64065(14) 1.01073(10) 0.0160(4) Uani 1 1 d . . . C12 C 0.28423(15) 0.56790(19) 1.02145(12) 0.0199(4) Uani 1 1 d . . . H12A H 0.2374 0.5407 1.0414 0.024 Uiso 1 1 calc R . . C13 C 0.35469(16) 0.61191(19) 1.06021(12) 0.0212(5) Uani 1 1 d . . . H13A H 0.3666 0.6217 1.1122 0.025 Uiso 1 1 calc R . . C14 C 0.48975(14) 0.70194(18) 1.03085(12) 0.0181(4) Uani 1 1 d . . . C15 C 0.56345(15) 0.6431(2) 1.00570(14) 0.0240(5) Uani 1 1 d . . . H15A H 0.5712 0.5751 1.0306 0.036 Uiso 1 1 calc R . . H15B H 0.6163 0.6841 1.0182 0.036 Uiso 1 1 calc R . . H15C H 0.5502 0.6324 0.9522 0.036 Uiso 1 1 calc R . . C16 C 0.47649(16) 0.81057(18) 0.99434(13) 0.0227(5) Uani 1 1 d . . . H16A H 0.4323 0.8487 1.0147 0.034 Uiso 1 1 calc R . . H16B H 0.4583 0.8023 0.9409 0.034 Uiso 1 1 calc R . . H16C H 0.5304 0.8498 1.0042 0.034 Uiso 1 1 calc R . . C17 C 0.50948(16) 0.7131(2) 1.11450(13) 0.0250(5) Uani 1 1 d . . . H17A H 0.5168 0.6436 1.1372 0.037 Uiso 1 1 calc R . . H17B H 0.4620 0.7494 1.1314 0.037 Uiso 1 1 calc R . . H17C H 0.5623 0.7537 1.1287 0.037 Uiso 1 1 calc R . . C21 C 0.14195(14) 0.71983(17) 0.87336(12) 0.0153(4) Uani 1 1 d . . . N21 N 0.14259(12) 0.61409(14) 0.87176(10) 0.0158(4) Uani 1 1 d . . . C22 C 0.05970(15) 0.58041(19) 0.84814(12) 0.0195(4) Uani 1 1 d . . . H22A H 0.0418 0.5096 0.8414 0.023 Uiso 1 1 calc R . . N22 N 0.05951(12) 0.75262(15) 0.85239(10) 0.0165(4) Uani 1 1 d . . . C23 C 0.00835(15) 0.66511(19) 0.83626(13) 0.0203(5) Uani 1 1 d . . . H23A H -0.0519 0.6647 0.8198 0.024 Uiso 1 1 calc R . . C24 C 0.02597(15) 0.86342(19) 0.85050(13) 0.0199(4) Uani 1 1 d . . . C25 C 0.06944(16) 0.9296(2) 0.79869(14) 0.0253(5) Uani 1 1 d . . . H25A H 0.0577 0.8995 0.7489 0.038 Uiso 1 1 calc R . . H25B H 0.1314 0.9305 0.8166 0.038 Uiso 1 1 calc R . . H25C H 0.0471 1.0012 0.7973 0.038 Uiso 1 1 calc R . . C26 C 0.04117(17) 0.9067(2) 0.92882(14) 0.0264(5) Uani 1 1 d . . . H26A H 0.0108 0.8634 0.9598 0.040 Uiso 1 1 calc R . . H26B H 0.0198 0.9788 0.9282 0.040 Uiso 1 1 calc R . . H26C H 0.1027 0.9059 0.9489 0.040 Uiso 1 1 calc R . . C27 C -0.07031(16) 0.8607(2) 0.82018(17) 0.0326(6) Uani 1 1 d . . . H27A H -0.0800 0.8327 0.7698 0.049 Uiso 1 1 calc R . . H27B H -0.0937 0.9317 0.8197 0.049 Uiso 1 1 calc R . . H27C H -0.0989 0.8158 0.8516 0.049 Uiso 1 1 calc R . . N31 N 0.24106(12) 0.48744(14) 0.81734(10) 0.0151(3) Uani 1 1 d . . . C31 C 0.24745(13) 0.53106(17) 0.75155(12) 0.0152(4) Uani 1 1 d . . . C32 C 0.26854(14) 0.38501(17) 0.81630(12) 0.0172(4) Uani 1 1 d . . . H32A H 0.2705 0.3359 0.8553 0.021 Uiso 1 1 calc R . . N32 N 0.27891(12) 0.45822(15) 0.70974(10) 0.0162(4) Uani 1 1 d . . . C33 C 0.29216(15) 0.36650(18) 0.75032(13) 0.0189(4) Uani 1 1 d . . . H33A H 0.3138 0.3026 0.7347 0.023 Uiso 1 1 calc R . . C34 C 0.30455(16) 0.47216(19) 0.63491(13) 0.0221(5) Uani 1 1 d . . . C35 C 0.22757(19) 0.5071(2) 0.57798(14) 0.0307(6) Uani 1 1 d . . . H35A H 0.1830 0.4532 0.5730 0.046 Uiso 1 1 calc R . . H35B H 0.2455 0.5179 0.5302 0.046 Uiso 1 1 calc R . . H35C H 0.2049 0.5728 0.5942 0.046 Uiso 1 1 calc R . . C36 C 0.3359(2) 0.3676(2) 0.61056(15) 0.0344(6) Uani 1 1 d . . . H36A H 0.2882 0.3178 0.6020 0.052 Uiso 1 1 calc R . . H36B H 0.3813 0.3404 0.6492 0.052 Uiso 1 1 calc R . . H36C H 0.3586 0.3771 0.5648 0.052 Uiso 1 1 calc R . . C37 C 0.3780(2) 0.5503(3) 0.64411(17) 0.0404(7) Uani 1 1 d . . . H37A H 0.3954 0.5620 0.5963 0.061 Uiso 1 1 calc R . . H37B H 0.4265 0.5225 0.6792 0.061 Uiso 1 1 calc R . . H37C H 0.3592 0.6166 0.6628 0.061 Uiso 1 1 calc R . . C41 C 0.0776(3) 0.1646(3) 0.49951(17) 0.0545(11) Uani 1 1 d . . . H41A H 0.1034 0.1271 0.5422 0.065 Uiso 1 1 calc R . . C42 C -0.0076(2) 0.1481(3) 0.46915(18) 0.0459(8) Uani 1 1 d . . . H42A H -0.0404 0.0993 0.4914 0.055 Uiso 1 1 calc R . . C43 C -0.0449(2) 0.2015(3) 0.40740(16) 0.0400(7) Uani 1 1 d . . . H43A H -0.1035 0.1900 0.3869 0.048 Uiso 1 1 calc R . . C44 C 0.0026(2) 0.2719(3) 0.37511(17) 0.0404(7) Uani 1 1 d . . . H44A H -0.0236 0.3086 0.3321 0.049 Uiso 1 1 calc R . . C45 C 0.0872(2) 0.2900(3) 0.4040(2) 0.0429(8) Uani 1 1 d . . . H45A H 0.1194 0.3387 0.3810 0.051 Uiso 1 1 calc R . . C46 C 0.1253(2) 0.2369(3) 0.4668(2) 0.0542(10) Uani 1 1 d . . . H46A H 0.1837 0.2496 0.4876 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 Ga1 0.01612(11) 0.01244(11) 0.01439(11) 0.00155(9) 0.00227(8) -0.00022(9) Ga2 0.02102(13) 0.01547(12) 0.02063(12) 0.00165(9) 0.00748(10) 0.00124(10) S1 0.0159(2) 0.0174(2) 0.0143(2) 0.00214(19) 0.00454(19) 0.0025(2) S2 0.0136(2) 0.0152(2) 0.0196(3) -0.0029(2) 0.0023(2) -0.00060(19) S3 0.0238(3) 0.0137(2) 0.0167(2) 0.00123(19) -0.0019(2) 0.0002(2) S4 0.0223(3) 0.0152(2) 0.0257(3) 0.0032(2) 0.0095(2) 0.0008(2) Cl1 0.0367(4) 0.0315(3) 0.0334(3) -0.0122(3) 0.0185(3) -0.0069(3) Cl2 0.0355(4) 0.0183(3) 0.0466(4) 0.0063(3) 0.0242(3) 0.0009(2) Cl3 0.0249(3) 0.0614(5) 0.0267(3) 0.0096(3) 0.0032(3) 0.0108(3) B 0.0175(11) 0.0148(11) 0.0158(11) -0.0006(9) 0.0032(9) -0.0002(9) C11 0.0152(10) 0.0133(9) 0.0143(9) 0.0023(7) 0.0024(8) 0.0028(8) N11 0.0169(9) 0.0156(9) 0.0133(8) 0.0012(7) 0.0037(7) 0.0004(7) N12 0.0171(9) 0.0163(9) 0.0143(8) 0.0003(7) 0.0019(7) 0.0017(7) C12 0.0229(11) 0.0226(11) 0.0152(10) 0.0021(8) 0.0063(9) 0.0014(9) C13 0.0252(12) 0.0262(12) 0.0131(10) 0.0014(9) 0.0061(9) -0.0001(10) C14 0.0179(11) 0.0170(10) 0.0181(10) 0.0000(8) -0.0004(8) 0.0007(8) C15 0.0165(11) 0.0270(13) 0.0273(12) -0.0025(10) 0.0002(9) 0.0032(9) C16 0.0260(12) 0.0160(10) 0.0247(12) -0.0008(9) 0.0010(10) -0.0010(9) C17 0.0227(12) 0.0309(13) 0.0194(11) -0.0035(10) -0.0016(9) -0.0013(10) C21 0.0144(10) 0.0160(10) 0.0153(9) -0.0015(8) 0.0024(8) 0.0006(8) N21 0.0144(9) 0.0154(9) 0.0173(8) -0.0002(7) 0.0019(7) -0.0012(7) C22 0.0182(11) 0.0218(11) 0.0192(10) -0.0037(8) 0.0055(9) -0.0057(9) N22 0.0128(8) 0.0182(9) 0.0183(8) -0.0018(7) 0.0025(7) 0.0017(7) C23 0.0141(10) 0.0267(12) 0.0197(10) -0.0016(9) 0.0023(8) -0.0038(9) C24 0.0158(10) 0.0218(11) 0.0223(11) 0.0018(9) 0.0037(9) 0.0063(9) C25 0.0256(13) 0.0253(12) 0.0252(12) 0.0077(10) 0.0047(10) 0.0055(10) C26 0.0289(13) 0.0244(12) 0.0276(12) -0.0022(10) 0.0093(10) 0.0051(10) C27 0.0181(12) 0.0345(15) 0.0436(16) 0.0032(12) 0.0014(11) 0.0091(11) N31 0.0170(9) 0.0128(8) 0.0152(8) 0.0005(7) 0.0019(7) -0.0004(7) C31 0.0135(10) 0.0153(10) 0.0156(9) -0.0001(8) -0.0006(8) -0.0014(8) C32 0.0199(11) 0.0133(10) 0.0177(10) 0.0031(8) 0.0014(8) 0.0016(8) N32 0.0173(9) 0.0160(9) 0.0153(8) 0.0002(7) 0.0027(7) 0.0003(7) C33 0.0217(11) 0.0137(10) 0.0212(11) -0.0004(8) 0.0037(9) 0.0036(8) C34 0.0258(12) 0.0238(12) 0.0184(10) 0.0023(9) 0.0083(9) -0.0001(10) C35 0.0407(16) 0.0342(14) 0.0173(11) 0.0008(10) 0.0052(11) 0.0069(12) C36 0.0475(18) 0.0341(15) 0.0257(13) 0.0006(11) 0.0179(12) 0.0107(13) C37 0.0396(17) 0.0476(18) 0.0390(16) -0.0018(14) 0.0204(14) -0.0152(14) C41 0.080(3) 0.057(2) 0.0257(15) -0.0022(15) 0.0078(16) 0.044(2) C42 0.068(2) 0.0354(17) 0.0377(17) 0.0027(13) 0.0192(16) 0.0119(16) C43 0.0466(18) 0.0403(17) 0.0321(15) -0.0027(13) 0.0040(13) -0.0074(14) C44 0.0420(18) 0.0418(17) 0.0360(16) 0.0072(13) 0.0024(13) -0.0010(14) C45 0.0342(16) 0.0321(16) 0.062(2) -0.0064(15) 0.0074(15) -0.0005(13) C46 0.0419(19) 0.059(2) 0.055(2) -0.0323(19) -0.0076(16) 0.0222(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 S4 2.2024(6) . ? Ga1 S1 2.2970(6) . ? Ga1 S2 2.3089(6) . ? Ga1 S3 2.3111(6) . ? Ga2 Cl2 2.1890(7) . ? Ga2 Cl1 2.1984(7) . ? Ga2 Cl3 2.2079(7) . ? Ga2 S4 2.2153(6) . ? S1 C11 1.731(2) . ? S2 C21 1.739(2) . ? S3 C31 1.740(2) . ? B H1 1.102(16) . ? B N31 1.548(3) . ? B N11 1.552(3) . ? B N21 1.560(3) . ? C11 N11 1.350(3) . ? C11 N12 1.357(3) . ? N11 C12 1.385(3) . ? N12 C13 1.389(3) . ? N12 C14 1.512(3) . ? C12 C13 1.339(3) . ? C14 C17 1.522(3) . ? C14 C15 1.528(3) . ? C14 C16 1.540(3) . ? C21 N21 1.352(3) . ? C21 N22 1.362(3) . ? N21 C22 1.378(3) . ? C22 C23 1.349(3) . ? N22 C23 1.382(3) . ? N22 C24 1.511(3) . ? C24 C26 1.523(3) . ? C24 C25 1.527(3) . ? C24 C27 1.530(3) . ? N31 C31 1.353(3) . ? N31 C32 1.381(3) . ? C31 N32 1.357(3) . ? C32 C33 1.353(3) . ? N32 C33 1.386(3) . ? N32 C34 1.513(3) . ? C34 C37 1.520(4) . ? C34 C36 1.521(4) . ? C34 C35 1.528(4) . ? C41 C42 1.383(5) . ? C41 C46 1.396(6) . ? C42 C43 1.367(4) . ? C43 C44 1.374(4) . ? C44 C45 1.373(4) . ? C45 C46 1.384(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 S4 Ga1 S1 104.44(2) . . ? S4 Ga1 S2 118.07(2) . . ? S1 Ga1 S2 107.61(2) . . ? S4 Ga1 S3 117.07(2) . . ? S1 Ga1 S3 103.06(2) . . ? S2 Ga1 S3 105.25(2) . . ? Cl2 Ga2 Cl1 108.66(3) . . ? Cl2 Ga2 Cl3 106.27(3) . . ? Cl1 Ga2 Cl3 106.80(3) . . ? Cl2 Ga2 S4 104.13(2) . . ? Cl1 Ga2 S4 115.22(3) . . ? Cl3 Ga2 S4 115.23(3) . . ? C11 S1 Ga1 96.11(7) . . ? C21 S2 Ga1 99.90(7) . . ? C31 S3 Ga1 99.89(7) . . ? Ga1 S4 Ga2 109.89(3) . . ? H1 B N31 107.8(14) . . ? H1 B N11 105.9(14) . . ? N31 B N11 114.06(18) . . ? H1 B N21 104.8(13) . . ? N31 B N21 111.66(18) . . ? N11 B N21 112.00(18) . . ? N11 C11 N12 108.87(18) . . ? N11 C11 S1 125.58(16) . . ? N12 C11 S1 125.51(17) . . ? C11 N11 C12 107.38(18) . . ? C11 N11 B 132.77(18) . . ? C12 N11 B 119.65(19) . . ? C11 N12 C13 107.48(19) . . ? C11 N12 C14 127.45(18) . . ? C13 N12 C14 124.75(18) . . ? C13 C12 N11 108.6(2) . . ? C12 C13 N12 107.7(2) . . ? N12 C14 C17 108.09(19) . . ? N12 C14 C15 110.16(18) . . ? C17 C14 C15 108.72(19) . . ? N12 C14 C16 108.34(18) . . ? C17 C14 C16 110.1(2) . . ? C15 C14 C16 111.3(2) . . ? N21 C21 N22 108.18(19) . . ? N21 C21 S2 126.08(17) . . ? N22 C21 S2 125.74(17) . . ? C21 N21 C22 107.97(19) . . ? C21 N21 B 133.82(19) . . ? C22 N21 B 118.19(19) . . ? C23 C22 N21 108.4(2) . . ? C21 N22 C23 108.02(19) . . ? C21 N22 C24 127.67(19) . . ? C23 N22 C24 124.22(19) . . ? C22 C23 N22 107.4(2) . . ? N22 C24 C26 108.83(19) . . ? N22 C24 C25 109.71(18) . . ? C26 C24 C25 112.1(2) . . ? N22 C24 C27 108.1(2) . . ? C26 C24 C27 109.5(2) . . ? C25 C24 C27 108.4(2) . . ? C31 N31 C32 107.73(18) . . ? C31 N31 B 133.65(19) . . ? C32 N31 B 118.55(18) . . ? N31 C31 N32 108.53(18) . . ? N31 C31 S3 125.96(17) . . ? N32 C31 S3 125.47(16) . . ? C33 C32 N31 108.43(19) . . ? C31 N32 C33 108.09(18) . . ? C31 N32 C34 128.29(19) . . ? C33 N32 C34 123.38(19) . . ? C32 C33 N32 107.21(19) . . ? N32 C34 C37 107.4(2) . . ? N32 C34 C36 108.61(19) . . ? C37 C34 C36 109.0(2) . . ? N32 C34 C35 110.4(2) . . ? C37 C34 C35 112.8(2) . . ? C36 C34 C35 108.6(2) . . ? C42 C41 C46 119.5(3) . . ? C43 C42 C41 120.5(3) . . ? C42 C43 C44 119.8(3) . . ? C45 C44 C43 121.1(3) . . ? C44 C45 C46 119.6(3) . . ? C45 C46 C41 119.6(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 31.81 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.992 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.103 # Attachment '- TmGaClGaCl4 (CH3CN) (14s10).cif' data_14s10 _database_code_depnum_ccdc_archive 'CCDC 763465' #TrackingRef '- TmGaClGaCl4 (CH3CN) (14s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H37 B Cl5 Ga2 N7 S3' _chemical_formula_weight 835.28 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 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 16.0697(7) _cell_length_b 17.5534(8) _cell_length_c 26.6647(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.1970(10) _cell_angle_gamma 90.00 _cell_volume 7490.6(6) _cell_formula_units_Z 8 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9955 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 32.40 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 1.988 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.3817 _exptl_absorpt_correction_T_max 0.5035 _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 127603 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 32.65 _reflns_number_total 26197 _reflns_number_gt 22182 _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. Although there are solvent accessible voids, there were no Q peaks to suggest that they are occupied. ; _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^)+(0.0322P)^2^+5.0714P] 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 26197 _refine_ls_number_parameters 747 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Ga1 Ga 0.974753(10) 0.313795(9) 0.069193(6) 0.01932(3) Uani 1 1 d . . . Ga2 Ga 0.371087(9) 0.306021(8) 0.261746(6) 0.01740(3) Uani 1 1 d . . . Ga3 Ga 0.796151(10) 0.525299(9) 0.294508(6) 0.02222(3) Uani 1 1 d . . . Ga4 Ga 0.500088(11) 0.656694(11) 0.072383(6) 0.02731(4) Uani 1 1 d . . . Cl1 Cl 1.09109(2) 0.30633(2) 0.033819(15) 0.03027(8) Uani 1 1 d . . . Cl2 Cl 0.26202(2) 0.28060(2) 0.301024(14) 0.02539(7) Uani 1 1 d . . . Cl3 Cl 0.70476(2) 0.61688(2) 0.295953(14) 0.02398(6) Uani 1 1 d . . . Cl4 Cl 0.80634(2) 0.50423(2) 0.214690(14) 0.02696(7) Uani 1 1 d . . . Cl5 Cl 0.91449(3) 0.56176(3) 0.332800(17) 0.03714(9) Uani 1 1 d . . . Cl6 Cl 0.75205(3) 0.42296(3) 0.329357(19) 0.04197(10) Uani 1 1 d . . . Cl7 Cl 0.47822(4) 0.72870(3) 0.136459(19) 0.05131(13) Uani 1 1 d . . . Cl8 Cl 0.62459(3) 0.68052(3) 0.049880(19) 0.04318(11) Uani 1 1 d . . . Cl9 Cl 0.48964(4) 0.53800(3) 0.09334(2) 0.05199(13) Uani 1 1 d . . . Cl10 Cl 0.40897(3) 0.68624(3) 0.009968(17) 0.04054(10) Uani 1 1 d . . . S1 S 0.96093(2) 0.423057(19) 0.113744(13) 0.01948(6) Uani 1 1 d . . . S2 S 0.86220(2) 0.30891(2) 0.011200(13) 0.02377(7) Uani 1 1 d . . . S3 S 0.96893(2) 0.21333(2) 0.122422(14) 0.02318(7) Uani 1 1 d . . . S4 S 0.34529(2) 0.395744(19) 0.200472(13) 0.01888(6) Uani 1 1 d . . . S5 S 0.47617(2) 0.35057(2) 0.316877(13) 0.02046(6) Uani 1 1 d . . . S6 S 0.41338(2) 0.199959(19) 0.221517(13) 0.02079(6) Uani 1 1 d . . . B1 B 0.78719(9) 0.31268(8) 0.12812(5) 0.0165(2) Uani 1 1 d . . . H1 H 0.7305(11) 0.3107(10) 0.1465(7) 0.020 Uiso 1 1 d . . . B2 B 0.55118(9) 0.34425(9) 0.19970(6) 0.0199(3) Uani 1 1 d . . . H2 H 0.6068(12) 0.3565(11) 0.1810(7) 0.024 Uiso 1 1 d . . . C11 C 0.92845(8) 0.37878(7) 0.16705(5) 0.0166(2) Uani 1 1 d . . . N11 N 0.85851(7) 0.33654(6) 0.16860(4) 0.01628(19) Uani 1 1 d . . . C12 C 0.85632(9) 0.31106(8) 0.21745(5) 0.0194(2) Uani 1 1 d . . . H12A H 0.8139 0.2801 0.2295 0.023 Uiso 1 1 calc R . . N12 N 0.97019(7) 0.38008(6) 0.21354(4) 0.0176(2) Uani 1 1 d . . . C13 C 0.92474(9) 0.33754(8) 0.24529(5) 0.0207(2) Uani 1 1 d . . . H13A H 0.9390 0.3286 0.2802 0.025 Uiso 1 1 calc R . . C14 C 1.05274(8) 0.41784(8) 0.22935(5) 0.0215(2) Uani 1 1 d . . . C15 C 1.04702(10) 0.50347(9) 0.21853(7) 0.0290(3) Uani 1 1 d . . . H15A H 1.0034 0.5260 0.2373 0.043 Uiso 1 1 calc R . . H15B H 1.0331 0.5116 0.1824 0.043 Uiso 1 1 calc R . . H15C H 1.1008 0.5275 0.2290 0.043 Uiso 1 1 calc R . . C16 C 1.07286(10) 0.40647(10) 0.28602(6) 0.0293(3) Uani 1 1 d . . . H16A H 1.0294 0.4305 0.3041 0.044 Uiso 1 1 calc R . . H16B H 1.1271 0.4297 0.2966 0.044 Uiso 1 1 calc R . . H16C H 1.0751 0.3519 0.2936 0.044 Uiso 1 1 calc R . . C17 C 1.12041(9) 0.37932(10) 0.20141(7) 0.0300(3) Uani 1 1 d . . . H17A H 1.1226 0.3249 0.2097 0.045 Uiso 1 1 calc R . . H17B H 1.1747 0.4027 0.2116 0.045 Uiso 1 1 calc R . . H17C H 1.1073 0.3856 0.1650 0.045 Uiso 1 1 calc R . . N21 N 0.77246(7) 0.37146(6) 0.08459(4) 0.0181(2) Uani 1 1 d . . . C21 C 0.80021(8) 0.37595(8) 0.03847(5) 0.0200(2) Uani 1 1 d . . . C22 C 0.72451(9) 0.43551(8) 0.09138(6) 0.0226(3) Uani 1 1 d . . . H22A H 0.6972 0.4472 0.1206 0.027 Uiso 1 1 calc R . . N22 N 0.77083(8) 0.44162(7) 0.01630(5) 0.0235(2) Uani 1 1 d . . . C23 C 0.72320(9) 0.47839(9) 0.04947(6) 0.0269(3) Uani 1 1 d . . . H23A H 0.6947 0.5254 0.0437 0.032 Uiso 1 1 calc R . . C24 C 0.79129(11) 0.47332(11) -0.03360(6) 0.0339(4) Uani 1 1 d . . . C25 C 0.74153(13) 0.54760(13) -0.04329(9) 0.0485(5) Uani 1 1 d . . . H25A H 0.7581 0.5844 -0.0166 0.073 Uiso 1 1 calc R . . H25B H 0.6816 0.5369 -0.0435 0.073 Uiso 1 1 calc R . . H25C H 0.7531 0.5688 -0.0759 0.073 Uiso 1 1 calc R . . C26 C 0.76593(15) 0.41694(15) -0.07568(7) 0.0501(6) Uani 1 1 d . . . H26A H 0.7982 0.3698 -0.0701 0.075 Uiso 1 1 calc R . . H26B H 0.7771 0.4391 -0.1081 0.075 Uiso 1 1 calc R . . H26C H 0.7062 0.4056 -0.0759 0.075 Uiso 1 1 calc R . . C27 C 0.88494(11) 0.49080(11) -0.03009(7) 0.0380(4) Uani 1 1 d . . . H27A H 0.8989 0.5270 -0.0026 0.057 Uiso 1 1 calc R . . H27B H 0.8993 0.5130 -0.0619 0.057 Uiso 1 1 calc R . . H27C H 0.9166 0.4436 -0.0234 0.057 Uiso 1 1 calc R . . C31 C 0.86652(9) 0.18763(7) 0.10263(5) 0.0199(2) Uani 1 1 d . . . N31 N 0.79878(7) 0.23136(6) 0.10702(4) 0.0177(2) Uani 1 1 d . . . N32 N 0.84198(9) 0.12160(7) 0.07955(5) 0.0245(2) Uani 1 1 d . . . C32 C 0.72975(9) 0.19176(8) 0.08631(6) 0.0238(3) Uani 1 1 d . . . H32A H 0.6735 0.2090 0.0844 0.029 Uiso 1 1 calc R . . C33 C 0.75620(11) 0.12410(9) 0.06929(6) 0.0275(3) Uani 1 1 d . . . H33A H 0.7220 0.0854 0.0532 0.033 Uiso 1 1 calc R . . C34 C 0.89765(13) 0.05774(9) 0.06474(8) 0.0382(4) Uani 1 1 d . . . C35 C 0.95335(19) 0.08982(12) 0.02561(11) 0.0663(9) Uani 1 1 d . . . H35A H 0.9902 0.1293 0.0413 0.100 Uiso 1 1 calc R . . H35B H 0.9181 0.1119 -0.0026 0.100 Uiso 1 1 calc R . . H35C H 0.9872 0.0487 0.0132 0.100 Uiso 1 1 calc R . . C36 C 0.84223(16) -0.00536(10) 0.04016(8) 0.0478(5) Uani 1 1 d . . . H36A H 0.8082 -0.0274 0.0652 0.072 Uiso 1 1 calc R . . H36B H 0.8774 -0.0451 0.0273 0.072 Uiso 1 1 calc R . . H36C H 0.8056 0.0160 0.0123 0.072 Uiso 1 1 calc R . . C37 C 0.94674(14) 0.02567(10) 0.11122(10) 0.0499(6) Uani 1 1 d . . . H37A H 0.9830 0.0654 0.1271 0.075 Uiso 1 1 calc R . . H37B H 0.9810 -0.0172 0.1016 0.075 Uiso 1 1 calc R . . H37C H 0.9080 0.0080 0.1351 0.075 Uiso 1 1 calc R . . N41 N 0.51447(7) 0.42294(7) 0.21238(4) 0.0191(2) Uani 1 1 d . . . C41 C 0.43578(8) 0.44833(7) 0.21560(5) 0.0171(2) Uani 1 1 d . . . N42 N 0.43945(7) 0.52089(6) 0.23288(4) 0.0187(2) Uani 1 1 d . . . C42 C 0.56844(9) 0.48144(8) 0.22759(6) 0.0235(3) Uani 1 1 d . . . H42A H 0.6277 0.4796 0.2290 0.028 Uiso 1 1 calc R . . C43 C 0.52264(9) 0.54166(8) 0.24016(6) 0.0238(3) Uani 1 1 d . . . H43A H 0.5437 0.5896 0.2519 0.029 Uiso 1 1 calc R . . C44 C 0.36743(9) 0.57051(8) 0.24550(5) 0.0216(2) Uani 1 1 d . . . C45 C 0.30731(11) 0.58086(9) 0.19846(6) 0.0304(3) Uani 1 1 d . . . H45A H 0.3370 0.6040 0.1718 0.046 Uiso 1 1 calc R . . H45B H 0.2612 0.6141 0.2062 0.046 Uiso 1 1 calc R . . H45C H 0.2851 0.5311 0.1871 0.046 Uiso 1 1 calc R . . C46 C 0.32548(11) 0.53375(10) 0.28865(6) 0.0313(3) Uani 1 1 d . . . H46A H 0.3010 0.4848 0.2775 0.047 Uiso 1 1 calc R . . H46B H 0.2814 0.5674 0.2988 0.047 Uiso 1 1 calc R . . H46C H 0.3671 0.5254 0.3173 0.047 Uiso 1 1 calc R . . C47 C 0.40168(11) 0.64861(9) 0.26214(6) 0.0290(3) Uani 1 1 d . . . H47A H 0.4269 0.6730 0.2341 0.043 Uiso 1 1 calc R . . H47B H 0.4441 0.6425 0.2907 0.043 Uiso 1 1 calc R . . H47C H 0.3560 0.6805 0.2723 0.043 Uiso 1 1 calc R . . N51 N 0.57846(7) 0.29622(7) 0.24738(4) 0.0199(2) Uani 1 1 d . . . C51 C 0.55446(8) 0.29487(8) 0.29458(5) 0.0193(2) Uani 1 1 d . . . N52 N 0.59957(7) 0.24076(7) 0.32150(5) 0.0217(2) Uani 1 1 d . . . C52 C 0.63920(9) 0.24126(8) 0.24439(6) 0.0228(3) Uani 1 1 d . . . H52A H 0.6667 0.2294 0.2153 0.027 Uiso 1 1 calc R . . C53 C 0.65289(9) 0.20731(9) 0.28977(6) 0.0250(3) Uani 1 1 d . . . H53A H 0.6919 0.1677 0.2984 0.030 Uiso 1 1 calc R . . C54 C 0.59534(10) 0.22003(9) 0.37618(6) 0.0254(3) Uani 1 1 d . . . C55 C 0.50817(11) 0.18948(10) 0.38390(7) 0.0334(3) Uani 1 1 d . . . H55A H 0.4961 0.1451 0.3621 0.050 Uiso 1 1 calc R . . H55B H 0.4665 0.2293 0.3753 0.050 Uiso 1 1 calc R . . H55C H 0.5061 0.1745 0.4192 0.050 Uiso 1 1 calc R . . C56 C 0.61821(13) 0.29031(10) 0.40831(6) 0.0349(4) Uani 1 1 d . . . H56A H 0.5771 0.3307 0.4000 0.052 Uiso 1 1 calc R . . H56B H 0.6739 0.3082 0.4016 0.052 Uiso 1 1 calc R . . H56C H 0.6183 0.2771 0.4440 0.052 Uiso 1 1 calc R . . C57 C 0.65882(13) 0.15678(12) 0.38979(7) 0.0404(4) Uani 1 1 d . . . H57A H 0.6442 0.1117 0.3692 0.061 Uiso 1 1 calc R . . H57B H 0.6582 0.1438 0.4255 0.061 Uiso 1 1 calc R . . H57C H 0.7148 0.1743 0.3834 0.061 Uiso 1 1 calc R . . C61 C 0.43469(9) 0.24377(8) 0.16542(5) 0.0198(2) Uani 1 1 d . . . N61 N 0.49247(8) 0.29873(7) 0.16093(4) 0.0204(2) Uani 1 1 d . . . C62 C 0.49060(10) 0.31790(9) 0.11048(6) 0.0262(3) Uani 1 1 d . . . H62A H 0.5247 0.3551 0.0965 0.031 Uiso 1 1 calc R . . N62 N 0.39669(8) 0.22815(7) 0.11894(5) 0.0239(2) Uani 1 1 d . . . C63 C 0.43228(11) 0.27484(10) 0.08463(6) 0.0295(3) Uani 1 1 d . . . H63A H 0.4180 0.2761 0.0493 0.035 Uiso 1 1 calc R . . C64 C 0.32552(11) 0.17363(10) 0.10542(6) 0.0296(3) Uani 1 1 d . . . C65 C 0.24915(11) 0.20041(11) 0.13095(7) 0.0356(4) Uani 1 1 d . . . H65A H 0.2618 0.1989 0.1676 0.053 Uiso 1 1 calc R . . H65B H 0.2017 0.1668 0.1212 0.053 Uiso 1 1 calc R . . H65C H 0.2351 0.2527 0.1204 0.053 Uiso 1 1 calc R . . C66 C 0.35299(13) 0.09278(10) 0.12077(8) 0.0393(4) Uani 1 1 d . . . H66A H 0.3662 0.0906 0.1574 0.059 Uiso 1 1 calc R . . H66B H 0.4026 0.0790 0.1040 0.059 Uiso 1 1 calc R . . H66C H 0.3077 0.0570 0.1108 0.059 Uiso 1 1 calc R . . C67 C 0.30380(14) 0.17616(13) 0.04823(7) 0.0441(5) Uani 1 1 d . . . H67A H 0.2844 0.2274 0.0383 0.066 Uiso 1 1 calc R . . H67B H 0.2595 0.1391 0.0387 0.066 Uiso 1 1 calc R . . H67C H 0.3535 0.1636 0.0312 0.066 Uiso 1 1 calc R . . N71 N 0.3237(2) 0.43714(16) 0.40334(10) 0.0875(9) Uani 1 1 d . . . C71 C 0.27441(18) 0.39512(15) 0.41283(9) 0.0547(6) Uani 1 1 d . . . C72 C 0.21127(18) 0.34184(19) 0.42596(10) 0.0683(7) Uani 1 1 d . . . H72A H 0.2383 0.2970 0.4421 0.102 Uiso 1 1 calc R . . H72B H 0.1770 0.3262 0.3954 0.102 Uiso 1 1 calc R . . H72C H 0.1757 0.3662 0.4493 0.102 Uiso 1 1 calc R . . N81 N 0.61648(16) 0.00457(15) 0.00897(10) 0.0703(6) Uani 1 1 d . . . C81 C 0.58703(17) -0.03915(16) 0.03500(10) 0.0578(6) Uani 1 1 d . . . C82 C 0.5491(2) -0.09375(16) 0.06674(11) 0.0669(7) Uani 1 1 d . . . H82A H 0.4897 -0.0992 0.0554 0.100 Uiso 1 1 calc R . . H82B H 0.5550 -0.0758 0.1017 0.100 Uiso 1 1 calc R . . H82C H 0.5769 -0.1432 0.0646 0.100 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 Ga1 0.02009(7) 0.01974(7) 0.01926(7) 0.00016(5) 0.00802(5) 0.00017(5) Ga2 0.01658(6) 0.01702(6) 0.01904(7) -0.00034(5) 0.00407(5) -0.00039(5) Ga3 0.02088(7) 0.02206(7) 0.02423(7) -0.00193(6) 0.00476(6) 0.00097(6) Ga4 0.02998(8) 0.02958(9) 0.02241(8) 0.00267(6) 0.00265(6) -0.00068(7) Cl1 0.02570(16) 0.03585(19) 0.03168(18) -0.00210(15) 0.01592(14) -0.00003(14) Cl2 0.02183(15) 0.02702(16) 0.02870(16) -0.00226(13) 0.00982(12) -0.00526(12) Cl3 0.02065(14) 0.02169(14) 0.03030(16) -0.00828(12) 0.00608(12) -0.00045(11) Cl4 0.03027(17) 0.02486(16) 0.02651(16) -0.00704(13) 0.00681(13) 0.00378(13) Cl5 0.02393(17) 0.0504(2) 0.0360(2) -0.00382(18) -0.00323(15) 0.00049(16) Cl6 0.0502(3) 0.02962(19) 0.0485(3) 0.01031(18) 0.0174(2) -0.00008(18) Cl7 0.0698(4) 0.0528(3) 0.0323(2) -0.0111(2) 0.0102(2) -0.0003(3) Cl8 0.02744(19) 0.0612(3) 0.0409(2) 0.0149(2) 0.00299(17) 0.00142(19) Cl9 0.0668(3) 0.0328(2) 0.0557(3) 0.0116(2) 0.0015(3) -0.0030(2) Cl10 0.0326(2) 0.0574(3) 0.03064(19) 0.00814(18) -0.00235(16) 0.00004(19) S1 0.02233(15) 0.01749(14) 0.01956(14) 0.00131(11) 0.00716(11) -0.00289(11) S2 0.02825(17) 0.02722(17) 0.01639(14) -0.00217(12) 0.00493(12) -0.00194(13) S3 0.02009(15) 0.02091(15) 0.02932(17) 0.00570(13) 0.00652(13) 0.00459(12) S4 0.01518(13) 0.01803(14) 0.02319(15) 0.00123(11) 0.00049(11) -0.00095(10) S5 0.01862(14) 0.02344(15) 0.01943(14) -0.00310(12) 0.00230(11) 0.00231(11) S6 0.02799(16) 0.01634(13) 0.01877(14) 0.00057(11) 0.00622(12) 0.00072(12) B1 0.0161(6) 0.0163(6) 0.0174(6) 0.0013(5) 0.0024(5) 0.0004(5) B2 0.0179(6) 0.0212(7) 0.0211(6) 0.0007(5) 0.0044(5) 0.0011(5) C11 0.0165(5) 0.0154(5) 0.0185(5) -0.0003(4) 0.0053(4) 0.0001(4) N11 0.0166(5) 0.0167(5) 0.0161(5) 0.0003(4) 0.0045(4) -0.0008(4) C12 0.0213(6) 0.0203(6) 0.0172(5) 0.0017(5) 0.0043(5) -0.0020(5) N12 0.0162(5) 0.0179(5) 0.0190(5) 0.0002(4) 0.0028(4) -0.0011(4) C13 0.0211(6) 0.0225(6) 0.0187(6) 0.0030(5) 0.0034(5) -0.0012(5) C14 0.0160(5) 0.0225(6) 0.0259(6) -0.0021(5) 0.0015(5) -0.0021(5) C15 0.0288(7) 0.0210(6) 0.0369(8) -0.0032(6) 0.0011(6) -0.0060(5) C16 0.0241(7) 0.0357(8) 0.0272(7) -0.0025(6) -0.0025(5) -0.0032(6) C17 0.0182(6) 0.0361(8) 0.0363(8) -0.0019(7) 0.0050(6) 0.0028(6) N21 0.0187(5) 0.0170(5) 0.0185(5) 0.0012(4) 0.0013(4) 0.0007(4) C21 0.0198(6) 0.0218(6) 0.0180(6) 0.0026(5) 0.0001(4) -0.0025(5) C22 0.0212(6) 0.0193(6) 0.0272(7) 0.0012(5) 0.0012(5) 0.0027(5) N22 0.0219(5) 0.0252(6) 0.0225(5) 0.0087(5) -0.0035(4) -0.0037(4) C23 0.0234(6) 0.0218(6) 0.0348(8) 0.0073(6) -0.0020(6) 0.0012(5) C24 0.0301(8) 0.0442(9) 0.0266(7) 0.0197(7) -0.0023(6) -0.0079(7) C25 0.0353(9) 0.0559(12) 0.0530(12) 0.0371(10) -0.0029(8) -0.0005(8) C26 0.0546(12) 0.0748(15) 0.0191(7) 0.0123(8) -0.0068(7) -0.0176(11) C27 0.0300(8) 0.0421(10) 0.0423(10) 0.0198(8) 0.0048(7) -0.0072(7) C31 0.0241(6) 0.0164(5) 0.0199(6) 0.0021(4) 0.0064(5) 0.0009(5) N31 0.0198(5) 0.0153(5) 0.0180(5) 0.0009(4) 0.0022(4) -0.0010(4) N32 0.0358(7) 0.0152(5) 0.0238(6) -0.0007(4) 0.0087(5) -0.0002(5) C32 0.0250(6) 0.0226(6) 0.0231(6) 0.0016(5) -0.0006(5) -0.0049(5) C33 0.0368(8) 0.0217(6) 0.0240(7) -0.0014(5) 0.0025(6) -0.0071(6) C34 0.0520(11) 0.0166(6) 0.0505(10) -0.0044(7) 0.0287(9) 0.0006(7) C35 0.098(2) 0.0300(9) 0.0821(17) -0.0201(10) 0.0698(16) -0.0157(11) C36 0.0759(15) 0.0202(7) 0.0515(11) -0.0108(7) 0.0289(11) -0.0081(8) C37 0.0419(10) 0.0203(8) 0.0891(17) 0.0069(9) 0.0157(11) 0.0107(7) N41 0.0160(5) 0.0201(5) 0.0216(5) 0.0016(4) 0.0035(4) -0.0005(4) C41 0.0160(5) 0.0171(5) 0.0182(5) 0.0024(4) 0.0013(4) -0.0005(4) N42 0.0179(5) 0.0177(5) 0.0203(5) 0.0006(4) 0.0004(4) -0.0009(4) C42 0.0170(6) 0.0240(6) 0.0295(7) 0.0004(5) 0.0015(5) -0.0046(5) C43 0.0205(6) 0.0218(6) 0.0286(7) -0.0003(5) -0.0010(5) -0.0046(5) C44 0.0228(6) 0.0195(6) 0.0220(6) -0.0010(5) -0.0013(5) 0.0039(5) C45 0.0318(8) 0.0223(7) 0.0343(8) -0.0001(6) -0.0117(6) 0.0056(6) C46 0.0349(8) 0.0307(8) 0.0300(7) -0.0025(6) 0.0118(6) 0.0029(6) C47 0.0331(8) 0.0214(7) 0.0311(7) -0.0048(6) -0.0042(6) 0.0025(6) N51 0.0159(5) 0.0224(5) 0.0216(5) 0.0006(4) 0.0032(4) 0.0028(4) C51 0.0171(5) 0.0208(6) 0.0202(6) -0.0003(5) 0.0021(4) 0.0006(4) N52 0.0210(5) 0.0226(5) 0.0212(5) 0.0015(4) 0.0002(4) 0.0021(4) C52 0.0179(6) 0.0235(6) 0.0275(7) -0.0011(5) 0.0052(5) 0.0037(5) C53 0.0207(6) 0.0248(7) 0.0296(7) 0.0009(5) 0.0026(5) 0.0061(5) C54 0.0294(7) 0.0255(7) 0.0209(6) 0.0042(5) -0.0001(5) -0.0004(5) C55 0.0363(8) 0.0328(8) 0.0316(8) 0.0059(6) 0.0056(7) -0.0072(7) C56 0.0486(10) 0.0329(8) 0.0219(7) 0.0007(6) -0.0042(7) -0.0090(7) C57 0.0450(10) 0.0428(10) 0.0326(9) 0.0125(7) -0.0013(7) 0.0137(8) C61 0.0233(6) 0.0183(6) 0.0186(6) -0.0010(4) 0.0054(5) 0.0020(5) N61 0.0222(5) 0.0213(5) 0.0182(5) 0.0009(4) 0.0052(4) 0.0012(4) C62 0.0309(7) 0.0290(7) 0.0195(6) 0.0026(5) 0.0073(5) -0.0020(6) N62 0.0289(6) 0.0243(6) 0.0189(5) -0.0013(4) 0.0042(4) -0.0020(5) C63 0.0367(8) 0.0346(8) 0.0177(6) 0.0018(6) 0.0053(6) -0.0040(6) C64 0.0335(8) 0.0303(7) 0.0245(7) -0.0023(6) 0.0002(6) -0.0082(6) C65 0.0283(8) 0.0421(9) 0.0360(9) 0.0044(7) 0.0011(6) -0.0046(7) C66 0.0508(11) 0.0262(8) 0.0407(9) -0.0083(7) 0.0030(8) -0.0063(7) C67 0.0526(12) 0.0522(11) 0.0264(8) -0.0056(8) -0.0032(8) -0.0180(9) N71 0.131(3) 0.0725(17) 0.0610(15) 0.0033(13) 0.0181(16) -0.0309(17) C71 0.0752(17) 0.0514(13) 0.0380(11) -0.0008(9) 0.0083(11) 0.0037(12) C72 0.0640(16) 0.094(2) 0.0481(13) -0.0012(14) 0.0110(12) -0.0138(15) N81 0.0653(14) 0.0698(15) 0.0756(16) -0.0143(13) 0.0056(12) -0.0245(12) C81 0.0561(14) 0.0549(14) 0.0618(15) -0.0124(12) 0.0017(11) -0.0092(11) C82 0.0801(19) 0.0583(15) 0.0626(16) -0.0011(13) 0.0086(14) -0.0159(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 Ga1 Cl1 2.1729(4) . ? Ga1 S3 2.2710(4) . ? Ga1 S2 2.2723(4) . ? Ga1 S1 2.2775(4) . ? Ga2 Cl2 2.1681(4) . ? Ga2 S5 2.2747(4) . ? Ga2 S4 2.2801(4) . ? Ga2 S6 2.2827(4) . ? Ga3 Cl6 2.1708(5) . ? Ga3 Cl5 2.1718(4) . ? Ga3 Cl3 2.1800(4) . ? Ga3 Cl4 2.1810(4) . ? Ga4 Cl9 2.1676(5) . ? Ga4 Cl10 2.1774(5) . ? Ga4 Cl7 2.1792(5) . ? Ga4 Cl8 2.1807(5) . ? S1 C11 1.7410(13) . ? S2 C21 1.7427(15) . ? S3 C31 1.7416(15) . ? S4 C41 1.7387(13) . ? S5 C51 1.7399(14) . ? S6 C61 1.7433(14) . ? B1 H1 1.075(18) . ? B1 N31 1.5517(18) . ? B1 N21 1.5551(18) . ? B1 N11 1.5589(18) . ? B2 H2 1.084(19) . ? B2 N41 1.5514(19) . ? B2 N51 1.5553(19) . ? B2 N61 1.556(2) . ? C11 N11 1.3501(16) . ? C11 N12 1.3551(17) . ? N11 C12 1.3808(16) . ? C12 C13 1.3521(19) . ? N12 C13 1.3857(17) . ? N12 C14 1.5084(17) . ? C14 C16 1.529(2) . ? C14 C17 1.530(2) . ? C14 C15 1.532(2) . ? N21 C21 1.3477(17) . ? N21 C22 1.3841(17) . ? C21 N22 1.3604(18) . ? C22 C23 1.346(2) . ? N22 C23 1.381(2) . ? N22 C24 1.5058(19) . ? C24 C26 1.524(3) . ? C24 C27 1.530(2) . ? C24 C25 1.539(3) . ? C31 N31 1.3456(17) . ? C31 N32 1.3541(18) . ? N31 C32 1.3812(18) . ? N32 C33 1.382(2) . ? N32 C34 1.509(2) . ? C32 C33 1.354(2) . ? C34 C37 1.516(3) . ? C34 C36 1.531(3) . ? C34 C35 1.541(3) . ? N41 C41 1.3508(17) . ? N41 C42 1.3810(18) . ? C41 N42 1.3539(17) . ? N42 C43 1.3824(18) . ? N42 C44 1.5105(18) . ? C42 C43 1.348(2) . ? C44 C45 1.523(2) . ? C44 C47 1.528(2) . ? C44 C46 1.528(2) . ? N51 C51 1.3495(18) . ? N51 C52 1.3797(17) . ? C51 N52 1.3597(18) . ? N52 C53 1.3878(19) . ? N52 C54 1.5104(19) . ? C52 C53 1.349(2) . ? C54 C56 1.528(2) . ? C54 C57 1.529(2) . ? C54 C55 1.531(2) . ? C61 N61 1.3518(18) . ? C61 N62 1.3589(18) . ? N61 C62 1.3843(18) . ? C62 C63 1.344(2) . ? N62 C63 1.3894(19) . ? N62 C64 1.510(2) . ? C64 C65 1.530(3) . ? C64 C66 1.531(3) . ? C64 C67 1.534(2) . ? N71 C71 1.127(4) . ? C71 C72 1.446(4) . ? N81 C81 1.164(4) . ? C81 C82 1.449(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 Cl1 Ga1 S3 108.071(16) . . ? Cl1 Ga1 S2 111.435(16) . . ? S3 Ga1 S2 108.706(15) . . ? Cl1 Ga1 S1 113.932(15) . . ? S3 Ga1 S1 108.451(14) . . ? S2 Ga1 S1 106.110(14) . . ? Cl2 Ga2 S5 110.113(15) . . ? Cl2 Ga2 S4 112.698(15) . . ? S5 Ga2 S4 107.564(14) . . ? Cl2 Ga2 S6 110.318(14) . . ? S5 Ga2 S6 110.419(14) . . ? S4 Ga2 S6 105.614(14) . . ? Cl6 Ga3 Cl5 110.40(2) . . ? Cl6 Ga3 Cl3 110.861(18) . . ? Cl5 Ga3 Cl3 109.692(17) . . ? Cl6 Ga3 Cl4 109.491(19) . . ? Cl5 Ga3 Cl4 111.641(17) . . ? Cl3 Ga3 Cl4 104.630(15) . . ? Cl9 Ga4 Cl10 111.32(2) . . ? Cl9 Ga4 Cl7 109.49(2) . . ? Cl10 Ga4 Cl7 108.43(2) . . ? Cl9 Ga4 Cl8 110.47(2) . . ? Cl10 Ga4 Cl8 108.311(19) . . ? Cl7 Ga4 Cl8 108.76(2) . . ? C11 S1 Ga1 95.77(4) . . ? C21 S2 Ga1 98.07(5) . . ? C31 S3 Ga1 95.91(5) . . ? C41 S4 Ga2 96.12(4) . . ? C51 S5 Ga2 95.94(5) . . ? C61 S6 Ga2 97.67(5) . . ? H1 B1 N31 105.7(10) . . ? H1 B1 N21 106.5(10) . . ? N31 B1 N21 110.79(11) . . ? H1 B1 N11 107.1(10) . . ? N31 B1 N11 113.16(11) . . ? N21 B1 N11 113.03(10) . . ? H2 B2 N41 105.6(10) . . ? H2 B2 N51 107.5(10) . . ? N41 B2 N51 112.89(11) . . ? H2 B2 N61 105.8(10) . . ? N41 B2 N61 112.49(11) . . ? N51 B2 N61 111.95(11) . . ? N11 C11 N12 109.01(11) . . ? N11 C11 S1 125.59(10) . . ? N12 C11 S1 125.39(10) . . ? C11 N11 C12 107.41(11) . . ? C11 N11 B1 133.49(11) . . ? C12 N11 B1 119.09(11) . . ? C13 C12 N11 108.52(12) . . ? C11 N12 C13 107.77(11) . . ? C11 N12 C14 127.80(11) . . ? C13 N12 C14 124.40(11) . . ? C12 C13 N12 107.29(12) . . ? N12 C14 C16 108.70(11) . . ? N12 C14 C17 108.39(12) . . ? C16 C14 C17 109.10(13) . . ? N12 C14 C15 110.03(11) . . ? C16 C14 C15 108.53(13) . . ? C17 C14 C15 112.03(13) . . ? C21 N21 C22 107.83(11) . . ? C21 N21 B1 132.79(11) . . ? C22 N21 B1 119.34(11) . . ? N21 C21 N22 108.40(12) . . ? N21 C21 S2 126.17(10) . . ? N22 C21 S2 125.43(11) . . ? C23 C22 N21 108.22(13) . . ? C21 N22 C23 107.96(12) . . ? C21 N22 C24 127.03(14) . . ? C23 N22 C24 124.83(13) . . ? C22 C23 N22 107.60(13) . . ? N22 C24 C26 110.20(14) . . ? N22 C24 C27 108.19(13) . . ? C26 C24 C27 111.79(18) . . ? N22 C24 C25 108.04(16) . . ? C26 C24 C25 109.04(16) . . ? C27 C24 C25 109.49(15) . . ? N31 C31 N32 108.86(12) . . ? N31 C31 S3 125.14(10) . . ? N32 C31 S3 125.98(11) . . ? C31 N31 C32 107.75(12) . . ? C31 N31 B1 132.92(11) . . ? C32 N31 B1 119.31(11) . . ? C31 N32 C33 107.88(12) . . ? C31 N32 C34 126.85(14) . . ? C33 N32 C34 125.19(14) . . ? C33 C32 N31 108.09(13) . . ? C32 C33 N32 107.42(13) . . ? N32 C34 C37 109.81(15) . . ? N32 C34 C36 108.29(16) . . ? C37 C34 C36 108.70(16) . . ? N32 C34 C35 107.47(14) . . ? C37 C34 C35 113.5(2) . . ? C36 C34 C35 108.99(17) . . ? C41 N41 C42 107.61(11) . . ? C41 N41 B2 133.18(12) . . ? C42 N41 B2 119.01(11) . . ? N41 C41 N42 108.66(11) . . ? N41 C41 S4 125.32(10) . . ? N42 C41 S4 126.02(10) . . ? C41 N42 C43 107.92(11) . . ? C41 N42 C44 127.42(11) . . ? C43 N42 C44 124.57(12) . . ? C43 C42 N41 108.28(12) . . ? C42 C43 N42 107.53(12) . . ? N42 C44 C45 109.08(12) . . ? N42 C44 C47 108.60(12) . . ? C45 C44 C47 108.48(12) . . ? N42 C44 C46 108.87(11) . . ? C45 C44 C46 112.35(13) . . ? C47 C44 C46 109.39(13) . . ? C51 N51 C52 107.77(12) . . ? C51 N51 B2 133.53(12) . . ? C52 N51 B2 118.69(11) . . ? N51 C51 N52 108.71(12) . . ? N51 C51 S5 125.83(10) . . ? N52 C51 S5 125.42(11) . . ? C51 N52 C53 107.63(12) . . ? C51 N52 C54 127.55(12) . . ? C53 N52 C54 124.81(12) . . ? C53 C52 N51 108.40(13) . . ? C52 C53 N52 107.48(12) . . ? N52 C54 C56 108.49(12) . . ? N52 C54 C57 108.46(13) . . ? C56 C54 C57 109.38(15) . . ? N52 C54 C55 109.62(12) . . ? C56 C54 C55 112.59(14) . . ? C57 C54 C55 108.22(14) . . ? N61 C61 N62 108.59(12) . . ? N61 C61 S6 125.49(11) . . ? N62 C61 S6 125.91(11) . . ? C61 N61 C62 107.74(12) . . ? C61 N61 B2 133.46(12) . . ? C62 N61 B2 118.64(12) . . ? C63 C62 N61 108.32(13) . . ? C61 N62 C63 107.68(12) . . ? C61 N62 C64 127.86(12) . . ? C63 N62 C64 124.39(13) . . ? C62 C63 N62 107.66(13) . . ? N62 C64 C65 108.65(13) . . ? N62 C64 C66 109.26(14) . . ? C65 C64 C66 112.91(15) . . ? N62 C64 C67 108.56(13) . . ? C65 C64 C67 108.29(16) . . ? C66 C64 C67 109.08(15) . . ? N71 C71 C72 178.9(3) . . ? N81 C81 C82 179.0(3) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 32.65 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.873 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.065 # Attachment '- TmGaClGaCl4 (CHCl3) (2s10p).cif' data_2s10p _database_code_depnum_ccdc_archive 'CCDC 763466' #TrackingRef '- TmGaClGaCl4 (CHCl3) (2s10p).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H36 B Cl11 Ga2 N6 S3' _chemical_formula_weight 1032.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0927(5) _cell_length_b 14.4146(7) _cell_length_c 16.1852(8) _cell_angle_alpha 98.2300(10) _cell_angle_beta 107.1550(10) _cell_angle_gamma 112.1170(10) _cell_volume 2194.38(18) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 8686 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.26 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 2.066 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.5762 _exptl_absorpt_correction_T_max 0.5762 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14599 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8883 _reflns_number_gt 7144 _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 bond has been restrained to 1.1 Angstroms. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.499 0.001 0.500 684 228 ' ' _platon_squeeze_details ; The unit cell contains 4 chloroform molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _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^)+(0.0783P)^2^+0.7021P] 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 8883 _refine_ls_number_parameters 347 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 Ga1 Ga -0.05255(3) 0.14903(2) 0.08940(2) 0.04187(11) Uani 1 1 d . . . Ga2 Ga 0.33459(4) 1.38445(3) 0.66105(3) 0.05706(13) Uani 1 1 d . . . S1 S -0.03699(8) 0.12436(7) 0.22737(6) 0.0568(2) Uani 1 1 d . . . S2 S 0.16614(7) 0.23678(5) 0.09011(5) 0.04347(17) Uani 1 1 d . . . S3 S -0.16307(7) 0.25439(6) 0.06783(5) 0.04287(17) Uani 1 1 d . . . Cl1 Cl -0.17512(9) 0.00253(7) -0.01719(7) 0.0697(3) Uani 1 1 d . . . Cl2 Cl 0.2451(2) 1.44868(16) 0.56148(12) 0.1302(6) Uani 1 1 d . . . Cl3 Cl 0.17081(13) 1.25445(11) 0.67712(10) 0.0985(4) Uani 1 1 d . . . Cl4 Cl 0.45910(13) 1.50347(10) 0.78987(8) 0.0918(4) Uani 1 1 d . . . Cl5 Cl 0.48116(13) 1.33761(9) 0.62416(8) 0.0784(3) Uani 1 1 d . . . B B 0.1388(3) 0.3913(3) 0.2615(2) 0.0430(7) Uani 1 1 d D . . H1 H 0.198(3) 0.4668(18) 0.3131(18) 0.052 Uiso 1 1 d D . . N11 N 0.1985(2) 0.31590(19) 0.29649(16) 0.0451(6) Uani 1 1 d . . . C11 C 0.1388(3) 0.2122(2) 0.29003(19) 0.0454(7) Uani 1 1 d . . . N12 N 0.2374(3) 0.1882(2) 0.34023(16) 0.0489(6) Uani 1 1 d . . . C12 C 0.3388(3) 0.3565(3) 0.3521(2) 0.0512(7) Uani 1 1 d . . . H12A H 0.4054 0.4257 0.3682 0.061 Uiso 1 1 calc R . . C13 C 0.3621(3) 0.2795(3) 0.3785(2) 0.0537(8) Uani 1 1 d . . . H13A H 0.4480 0.2859 0.4165 0.064 Uiso 1 1 calc R . . C14 C 0.2181(4) 0.0839(3) 0.3565(3) 0.0625(9) Uani 1 1 d . . . C15 C 0.1696(6) 0.0040(4) 0.2684(3) 0.0830(13) Uani 1 1 d . . . H15A H 0.0792 -0.0055 0.2294 0.124 Uiso 1 1 calc R . . H15B H 0.1624 -0.0613 0.2793 0.124 Uiso 1 1 calc R . . H15C H 0.2361 0.0276 0.2403 0.124 Uiso 1 1 calc R . . C16 C 0.3607(5) 0.0962(4) 0.4198(3) 0.0834(13) Uani 1 1 d . . . H16A H 0.3920 0.1471 0.4762 0.125 Uiso 1 1 calc R . . H16B H 0.4286 0.1189 0.3925 0.125 Uiso 1 1 calc R . . H16C H 0.3507 0.0303 0.4304 0.125 Uiso 1 1 calc R . . C17 C 0.1171(5) 0.0561(4) 0.4047(3) 0.0852(13) Uani 1 1 d . . . H17A H 0.0272 0.0483 0.3665 0.128 Uiso 1 1 calc R . . H17B H 0.1533 0.1107 0.4596 0.128 Uiso 1 1 calc R . . H17C H 0.1068 -0.0084 0.4186 0.128 Uiso 1 1 calc R . . N21 N 0.1638(2) 0.41526(18) 0.17550(16) 0.0398(5) Uani 1 1 d . . . C21 C 0.1692(3) 0.3596(2) 0.10377(19) 0.0373(6) Uani 1 1 d . . . N22 N 0.1805(2) 0.41613(19) 0.04388(16) 0.0420(5) Uani 1 1 d . . . C22 C 0.1736(3) 0.5089(2) 0.1614(2) 0.0503(7) Uani 1 1 d . . . H22A H 0.1731 0.5623 0.2008 0.060 Uiso 1 1 calc R . . C23 C 0.1841(4) 0.5101(2) 0.0807(2) 0.0510(7) Uani 1 1 d . . . H23A H 0.1923 0.5644 0.0545 0.061 Uiso 1 1 calc R . . C24 C 0.1830(3) 0.3837(3) -0.0492(2) 0.0516(7) Uani 1 1 d . . . C25 C 0.0437(4) 0.2910(4) -0.1084(2) 0.0721(11) Uani 1 1 d . . . H25A H -0.0317 0.3097 -0.1120 0.108 Uiso 1 1 calc R . . H25B H 0.0317 0.2335 -0.0830 0.108 Uiso 1 1 calc R . . H25C H 0.0429 0.2710 -0.1679 0.108 Uiso 1 1 calc R . . C26 C 0.3088(4) 0.3607(4) -0.0394(3) 0.0662(10) Uani 1 1 d . . . H26A H 0.3106 0.3400 -0.0980 0.099 Uiso 1 1 calc R . . H26B H 0.3012 0.3052 -0.0118 0.099 Uiso 1 1 calc R . . H26C H 0.3939 0.4223 -0.0024 0.099 Uiso 1 1 calc R . . C27 C 0.2003(5) 0.4751(4) -0.0891(3) 0.0760(11) Uani 1 1 d . . . H27A H 0.1216 0.4906 -0.0954 0.114 Uiso 1 1 calc R . . H27B H 0.2046 0.4571 -0.1473 0.114 Uiso 1 1 calc R . . H27C H 0.2856 0.5354 -0.0498 0.114 Uiso 1 1 calc R . . N31 N -0.0188(3) 0.3533(2) 0.24989(16) 0.0451(6) Uani 1 1 d . . . C31 C -0.1422(3) 0.2963(2) 0.17955(19) 0.0400(6) Uani 1 1 d . . . N32 N -0.2481(3) 0.2773(2) 0.21036(17) 0.0485(6) Uani 1 1 d . . . C32 C -0.0488(4) 0.3705(3) 0.3252(2) 0.0645(10) Uani 1 1 d . . . H32A H 0.0173 0.4081 0.3833 0.077 Uiso 1 1 calc R . . C33 C -0.1879(4) 0.3249(3) 0.3018(2) 0.0651(10) Uani 1 1 d . . . H33A H -0.2356 0.3252 0.3403 0.078 Uiso 1 1 calc R . . C34 C -0.4036(3) 0.2070(3) 0.1578(2) 0.0528(8) Uani 1 1 d . . . C35 C -0.4797(4) 0.2083(4) 0.2227(3) 0.0754(11) Uani 1 1 d . . . H35A H -0.4686 0.2778 0.2440 0.113 Uiso 1 1 calc R . . H35B H -0.4402 0.1864 0.2730 0.113 Uiso 1 1 calc R . . H35C H -0.5779 0.1614 0.1918 0.113 Uiso 1 1 calc R . . C36 C -0.4222(4) 0.0964(3) 0.1248(3) 0.0699(11) Uani 1 1 d . . . H36A H -0.3738 0.0949 0.0846 0.105 Uiso 1 1 calc R . . H36B H -0.5206 0.0500 0.0933 0.105 Uiso 1 1 calc R . . H36C H -0.3841 0.0745 0.1754 0.105 Uiso 1 1 calc R . . C37 C -0.4608(4) 0.2480(3) 0.0826(3) 0.0629(9) Uani 1 1 d . . . H37A H -0.4462 0.3178 0.1073 0.094 Uiso 1 1 calc R . . H37B H -0.5597 0.2037 0.0507 0.094 Uiso 1 1 calc R . . H37C H -0.4131 0.2486 0.0417 0.094 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 Ga1 0.03442(16) 0.03257(17) 0.04753(19) 0.00516(13) 0.00764(13) 0.01191(13) Ga2 0.0603(2) 0.0528(2) 0.0544(2) 0.01654(17) 0.01615(17) 0.02522(18) S1 0.0431(4) 0.0476(4) 0.0590(5) 0.0234(4) 0.0078(3) 0.0052(3) S2 0.0400(3) 0.0341(3) 0.0578(4) 0.0124(3) 0.0176(3) 0.0188(3) S3 0.0418(4) 0.0498(4) 0.0373(3) 0.0078(3) 0.0117(3) 0.0248(3) Cl1 0.0448(4) 0.0463(4) 0.0852(6) -0.0166(4) 0.0072(4) 0.0131(3) Cl2 0.1522(14) 0.1486(15) 0.1151(11) 0.0754(11) 0.0265(10) 0.0971(13) Cl3 0.0710(6) 0.0820(8) 0.1212(10) 0.0385(7) 0.0298(6) 0.0141(6) Cl4 0.0821(7) 0.0910(8) 0.0726(6) -0.0108(6) 0.0320(5) 0.0187(6) Cl5 0.0963(7) 0.0773(7) 0.0789(6) 0.0225(5) 0.0440(6) 0.0477(6) B 0.0399(15) 0.0389(16) 0.0365(15) 0.0027(13) 0.0090(12) 0.0107(13) N11 0.0364(12) 0.0419(13) 0.0416(12) 0.0123(10) 0.0057(10) 0.0087(10) C11 0.0422(14) 0.0440(16) 0.0396(14) 0.0146(12) 0.0097(12) 0.0121(12) N12 0.0504(14) 0.0503(15) 0.0405(13) 0.0178(11) 0.0114(11) 0.0196(12) C12 0.0397(15) 0.0553(18) 0.0433(16) 0.0090(14) 0.0109(12) 0.0110(14) C13 0.0445(16) 0.063(2) 0.0427(16) 0.0145(14) 0.0081(13) 0.0194(15) C14 0.073(2) 0.060(2) 0.058(2) 0.0293(17) 0.0199(17) 0.0334(18) C15 0.102(3) 0.063(2) 0.073(3) 0.018(2) 0.015(2) 0.039(2) C16 0.094(3) 0.073(3) 0.073(3) 0.026(2) 0.006(2) 0.045(2) C17 0.097(3) 0.088(3) 0.092(3) 0.061(3) 0.049(3) 0.040(3) N21 0.0366(11) 0.0349(12) 0.0452(12) 0.0104(10) 0.0138(9) 0.0148(9) C21 0.0337(12) 0.0314(13) 0.0445(14) 0.0086(11) 0.0136(11) 0.0140(10) N22 0.0444(12) 0.0414(13) 0.0475(13) 0.0174(10) 0.0221(10) 0.0211(11) C22 0.0578(18) 0.0370(15) 0.0616(19) 0.0137(13) 0.0266(15) 0.0239(14) C23 0.0621(19) 0.0398(16) 0.0625(19) 0.0222(14) 0.0303(16) 0.0263(14) C24 0.0559(18) 0.066(2) 0.0493(17) 0.0241(15) 0.0280(14) 0.0346(16) C25 0.067(2) 0.093(3) 0.0465(19) 0.0166(19) 0.0149(16) 0.032(2) C26 0.067(2) 0.095(3) 0.066(2) 0.032(2) 0.0384(18) 0.053(2) C27 0.103(3) 0.094(3) 0.073(2) 0.054(2) 0.054(2) 0.061(3) N31 0.0423(12) 0.0451(13) 0.0374(12) 0.0036(10) 0.0124(10) 0.0137(11) C31 0.0393(14) 0.0397(14) 0.0420(14) 0.0107(11) 0.0152(11) 0.0188(12) N32 0.0420(13) 0.0547(15) 0.0469(14) 0.0122(12) 0.0201(11) 0.0179(12) C32 0.0554(19) 0.075(2) 0.0425(17) 0.0019(16) 0.0190(14) 0.0124(17) C33 0.0545(19) 0.084(3) 0.0441(17) 0.0061(17) 0.0252(15) 0.0178(18) C34 0.0384(15) 0.0567(19) 0.0636(19) 0.0211(15) 0.0190(14) 0.0204(14) C35 0.052(2) 0.100(3) 0.078(3) 0.032(2) 0.0342(19) 0.028(2) C36 0.0448(17) 0.052(2) 0.103(3) 0.019(2) 0.0231(19) 0.0161(15) C37 0.0523(18) 0.067(2) 0.077(2) 0.0250(19) 0.0228(17) 0.0334(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 Cl1 2.1669(8) . ? Ga1 S2 2.2702(8) . ? Ga1 S1 2.2780(9) . ? Ga1 S3 2.2876(8) . ? Ga2 Cl2 2.1482(13) . ? Ga2 Cl4 2.1659(11) . ? Ga2 Cl3 2.1759(13) . ? Ga2 Cl5 2.1770(12) . ? S1 C11 1.744(3) . ? S2 C21 1.739(3) . ? S3 C31 1.739(3) . ? B H1 1.091(18) . ? B N21 1.557(4) . ? B N11 1.561(4) . ? B N31 1.565(4) . ? N11 C11 1.361(4) . ? N11 C12 1.383(4) . ? C11 N12 1.348(4) . ? N12 C13 1.386(4) . ? N12 C14 1.510(4) . ? C12 C13 1.330(5) . ? C14 C15 1.504(6) . ? C14 C17 1.514(6) . ? C14 C16 1.538(6) . ? N21 C21 1.344(4) . ? N21 C22 1.370(4) . ? C21 N22 1.356(4) . ? N22 C23 1.381(4) . ? N22 C24 1.523(4) . ? C22 C23 1.348(5) . ? C24 C25 1.516(5) . ? C24 C27 1.522(5) . ? C24 C26 1.522(5) . ? N31 C31 1.346(4) . ? N31 C32 1.368(4) . ? C31 N32 1.359(4) . ? N32 C33 1.374(4) . ? N32 C34 1.516(4) . ? C32 C33 1.333(5) . ? C34 C37 1.505(5) . ? C34 C36 1.521(5) . ? C34 C35 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 Ga1 S2 112.20(4) . . ? Cl1 Ga1 S1 111.52(4) . . ? S2 Ga1 S1 109.95(3) . . ? Cl1 Ga1 S3 109.19(3) . . ? S2 Ga1 S3 107.32(3) . . ? S1 Ga1 S3 106.41(3) . . ? Cl2 Ga2 Cl4 110.06(7) . . ? Cl2 Ga2 Cl3 110.96(7) . . ? Cl4 Ga2 Cl3 108.91(6) . . ? Cl2 Ga2 Cl5 109.67(7) . . ? Cl4 Ga2 Cl5 105.56(5) . . ? Cl3 Ga2 Cl5 111.53(6) . . ? C11 S1 Ga1 99.28(10) . . ? C21 S2 Ga1 97.14(9) . . ? C31 S3 Ga1 96.67(10) . . ? H1 B N21 104.6(18) . . ? H1 B N11 107.4(18) . . ? N21 B N11 113.6(3) . . ? H1 B N31 106.5(18) . . ? N21 B N31 112.5(2) . . ? N11 B N31 111.6(3) . . ? C11 N11 C12 107.1(3) . . ? C11 N11 B 133.6(2) . . ? C12 N11 B 119.1(3) . . ? N12 C11 N11 109.1(2) . . ? N12 C11 S1 125.3(2) . . ? N11 C11 S1 125.6(2) . . ? C11 N12 C13 107.0(3) . . ? C11 N12 C14 127.7(3) . . ? C13 N12 C14 125.2(3) . . ? C13 C12 N11 108.2(3) . . ? C12 C13 N12 108.7(3) . . ? C15 C14 N12 109.6(3) . . ? C15 C14 C17 113.7(4) . . ? N12 C14 C17 107.9(3) . . ? C15 C14 C16 109.2(4) . . ? N12 C14 C16 108.3(3) . . ? C17 C14 C16 107.9(4) . . ? C21 N21 C22 108.0(2) . . ? C21 N21 B 133.8(2) . . ? C22 N21 B 118.0(2) . . ? N21 C21 N22 108.6(2) . . ? N21 C21 S2 126.1(2) . . ? N22 C21 S2 125.2(2) . . ? C21 N22 C23 107.5(2) . . ? C21 N22 C24 128.0(2) . . ? C23 N22 C24 124.5(3) . . ? C23 C22 N21 108.2(3) . . ? C22 C23 N22 107.6(3) . . ? C25 C24 C27 109.2(3) . . ? C25 C24 C26 113.0(3) . . ? C27 C24 C26 108.7(3) . . ? C25 C24 N22 108.6(3) . . ? C27 C24 N22 108.0(3) . . ? C26 C24 N22 109.2(3) . . ? C31 N31 C32 107.3(3) . . ? C31 N31 B 133.9(2) . . ? C32 N31 B 118.6(2) . . ? N31 C31 N32 108.6(2) . . ? N31 C31 S3 125.8(2) . . ? N32 C31 S3 125.6(2) . . ? C31 N32 C33 107.5(3) . . ? C31 N32 C34 127.4(3) . . ? C33 N32 C34 124.8(3) . . ? C33 C32 N31 109.1(3) . . ? C32 C33 N32 107.6(3) . . ? C37 C34 N32 110.3(3) . . ? C37 C34 C36 113.2(3) . . ? N32 C34 C36 108.1(3) . . ? C37 C34 C35 108.6(3) . . ? N32 C34 C35 107.8(3) . . ? C36 C34 C35 108.7(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.748 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.070 # Attachment '- TmGaClGaCl4 (C6H6) (ky216s10).cif' data_nova _database_code_depnum_ccdc_archive 'CCDC 763467' #TrackingRef '- TmGaClGaCl4 (C6H6) (ky216s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H46 B Cl5 Ga2 N6 S3' _chemical_formula_weight 950.44 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9637(12) _cell_length_b 13.0055(13) _cell_length_c 16.595(3) _cell_angle_alpha 99.187(2) _cell_angle_beta 102.166(2) _cell_angle_gamma 113.5400(10) _cell_volume 2226.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9969 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 30.58 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 1.681 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8499 _exptl_absorpt_correction_T_max 0.9207 _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 36434 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0632 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 30.61 _reflns_number_total 13633 _reflns_number_gt 9436 _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^)+(0.0300P)^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 13633 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 Ga1 Ga 0.08622(2) 0.36530(2) 0.396462(14) 0.01881(6) Uani 1 1 d . . . Ga2 Ga -0.26220(2) 0.20964(2) 0.845033(15) 0.02338(6) Uani 1 1 d . . . S2 S -0.10700(5) 0.35371(5) 0.33087(3) 0.02074(11) Uani 1 1 d . . . S1 S 0.04690(5) 0.19066(5) 0.42568(3) 0.02040(11) Uani 1 1 d . . . S3 S 0.20363(5) 0.38729(5) 0.30340(3) 0.02244(12) Uani 1 1 d . . . Cl1 Cl 0.19034(6) 0.50511(5) 0.51387(4) 0.03224(14) Uani 1 1 d . . . Cl2 Cl -0.21822(6) 0.39281(5) 0.87997(4) 0.03489(14) Uani 1 1 d . . . Cl3 Cl -0.33278(5) 0.14137(5) 0.70576(3) 0.03151(13) Uani 1 1 d . . . Cl4 Cl -0.08847(5) 0.19119(5) 0.89009(3) 0.02635(12) Uani 1 1 d . . . Cl5 Cl -0.40278(6) 0.11011(6) 0.90136(4) 0.04321(17) Uani 1 1 d . . . B B -0.0750(2) 0.1312(2) 0.20726(15) 0.0199(5) Uani 1 1 d . . . H1 H -0.122(2) 0.0581(19) 0.1496(14) 0.024 Uiso 1 1 d . . . N11 N -0.14697(16) 0.09274(14) 0.27332(11) 0.0181(4) Uani 1 1 d . . . C11 C -0.11039(19) 0.11424(17) 0.35903(13) 0.0173(4) Uani 1 1 d . . . N12 N -0.21593(16) 0.06868(14) 0.38470(10) 0.0178(4) Uani 1 1 d . . . C12 C -0.27884(19) 0.03228(18) 0.24434(14) 0.0220(4) Uani 1 1 d . . . H12A H -0.3305 0.0058 0.1862 0.026 Uiso 1 1 calc R . . C13 C -0.3216(2) 0.01730(18) 0.31216(13) 0.0224(5) Uani 1 1 d . . . H13A H -0.4085 -0.0214 0.3107 0.027 Uiso 1 1 calc R . . C14 C -0.2232(2) 0.07871(19) 0.47517(13) 0.0213(4) Uani 1 1 d . . . C15 C -0.3628(2) 0.0112(2) 0.47115(15) 0.0299(5) Uani 1 1 d . . . H15A H -0.4137 0.0451 0.4418 0.045 Uiso 1 1 calc R . . H15B H -0.3691 0.0156 0.5294 0.045 Uiso 1 1 calc R . . H15C H -0.3953 -0.0705 0.4396 0.045 Uiso 1 1 calc R . . C16 C -0.1760(2) 0.2067(2) 0.52021(15) 0.0309(5) Uani 1 1 d . . . H16A H -0.0862 0.2507 0.5234 0.046 Uiso 1 1 calc R . . H16B H -0.1838 0.2140 0.5782 0.046 Uiso 1 1 calc R . . H16C H -0.2278 0.2377 0.4880 0.046 Uiso 1 1 calc R . . C17 C -0.1470(2) 0.0242(2) 0.52126(15) 0.0290(5) Uani 1 1 d . . . H17A H -0.0567 0.0666 0.5248 0.043 Uiso 1 1 calc R . . H17B H -0.1803 -0.0575 0.4895 0.043 Uiso 1 1 calc R . . H17C H -0.1547 0.0284 0.5792 0.043 Uiso 1 1 calc R . . N21 N -0.08705(16) 0.23771(15) 0.18348(10) 0.0189(4) Uani 1 1 d . . . C21 C -0.10272(19) 0.32672(18) 0.22555(12) 0.0184(4) Uani 1 1 d . . . N22 N -0.11474(16) 0.39293(15) 0.17234(11) 0.0193(4) Uani 1 1 d . . . C22 C -0.0878(2) 0.25080(19) 0.10248(13) 0.0232(5) Uani 1 1 d . . . H22A H -0.0779 0.2010 0.0590 0.028 Uiso 1 1 calc R . . C23 C -0.1047(2) 0.34483(19) 0.09500(13) 0.0237(5) Uani 1 1 d . . . H23A H -0.1091 0.3734 0.0458 0.028 Uiso 1 1 calc R . . C24 C -0.1364(2) 0.50027(18) 0.19100(13) 0.0207(4) Uani 1 1 d . . . C25 C -0.2556(2) 0.4702(2) 0.22038(14) 0.0262(5) Uani 1 1 d . . . H25A H -0.2420 0.4476 0.2738 0.039 Uiso 1 1 calc R . . H25B H -0.3292 0.4055 0.1762 0.039 Uiso 1 1 calc R . . H25C H -0.2723 0.5384 0.2300 0.039 Uiso 1 1 calc R . . C26 C -0.1599(2) 0.5353(2) 0.10807(15) 0.0293(5) Uani 1 1 d . . . H26A H -0.0841 0.5548 0.0884 0.044 Uiso 1 1 calc R . . H26B H -0.1768 0.6033 0.1182 0.044 Uiso 1 1 calc R . . H26C H -0.2338 0.4703 0.0643 0.044 Uiso 1 1 calc R . . C27 C -0.0167(2) 0.59772(19) 0.25842(15) 0.0282(5) Uani 1 1 d . . . H27A H 0.0571 0.6141 0.2368 0.042 Uiso 1 1 calc R . . H27B H -0.0016 0.5735 0.3110 0.042 Uiso 1 1 calc R . . H27C H -0.0288 0.6682 0.2707 0.042 Uiso 1 1 calc R . . N31 N 0.06578(16) 0.14946(15) 0.23572(11) 0.0196(4) Uani 1 1 d . . . C31 C 0.1801(2) 0.24365(18) 0.27522(13) 0.0199(4) Uani 1 1 d . . . N32 N 0.27234(17) 0.20725(15) 0.28882(11) 0.0223(4) Uani 1 1 d . . . C32 C 0.0880(2) 0.05298(19) 0.22423(14) 0.0234(5) Uani 1 1 d . . . H32A H 0.0247 -0.0252 0.1977 0.028 Uiso 1 1 calc R . . C33 C 0.2139(2) 0.08762(19) 0.25663(14) 0.0262(5) Uani 1 1 d . . . H33A H 0.2553 0.0387 0.2573 0.031 Uiso 1 1 calc R . . C34 C 0.4139(2) 0.2803(2) 0.33553(15) 0.0273(5) Uani 1 1 d . . . C35 C 0.4290(2) 0.3276(2) 0.42957(15) 0.0391(6) Uani 1 1 d . . . H35A H 0.3916 0.2625 0.4538 0.059 Uiso 1 1 calc R . . H35B H 0.3849 0.3767 0.4339 0.059 Uiso 1 1 calc R . . H35C H 0.5201 0.3741 0.4613 0.059 Uiso 1 1 calc R . . C36 C 0.4705(2) 0.3763(2) 0.29336(17) 0.0365(6) Uani 1 1 d . . . H36A H 0.4287 0.4273 0.2971 0.055 Uiso 1 1 calc R . . H36B H 0.4569 0.3415 0.2331 0.055 Uiso 1 1 calc R . . H36C H 0.5625 0.4219 0.3228 0.055 Uiso 1 1 calc R . . C37 C 0.4804(2) 0.2021(2) 0.3286(2) 0.0439(7) Uani 1 1 d . . . H37A H 0.4452 0.1397 0.3557 0.066 Uiso 1 1 calc R . . H37B H 0.5724 0.2484 0.3576 0.066 Uiso 1 1 calc R . . H37C H 0.4663 0.1679 0.2681 0.066 Uiso 1 1 calc R . . C41 C 0.7763(3) 0.7603(2) 0.33818(18) 0.0446(7) Uani 1 1 d . . . H41A H 0.8400 0.7769 0.3901 0.054 Uiso 1 1 calc R . . C42 C 0.6492(3) 0.7026(2) 0.33206(18) 0.0483(7) Uani 1 1 d . . . H42A H 0.6253 0.6785 0.3795 0.058 Uiso 1 1 calc R . . C43 C 0.5555(3) 0.6794(2) 0.25705(19) 0.0445(7) Uani 1 1 d . . . H43A H 0.4676 0.6405 0.2532 0.053 Uiso 1 1 calc R . . C44 C 0.5907(3) 0.7129(2) 0.18824(18) 0.0439(7) Uani 1 1 d . . . H44A H 0.5268 0.6968 0.1365 0.053 Uiso 1 1 calc R . . C45 C 0.7184(3) 0.7700(2) 0.19382(18) 0.0410(6) Uani 1 1 d . . . H45A H 0.7423 0.7926 0.1459 0.049 Uiso 1 1 calc R . . C46 C 0.8116(3) 0.7942(2) 0.26918(18) 0.0398(6) Uani 1 1 d . . . H46A H 0.8995 0.8340 0.2734 0.048 Uiso 1 1 calc R . . C51 C -0.5846(10) 0.2274(13) 0.0397(4) 0.049(3) Uani 0.523(17) 1 d PG A 1 H51A H -0.5197 0.2060 0.0316 0.058 Uiso 0.523(17) 1 calc PR A 1 C52 C -0.6990(14) 0.1444(8) 0.0443(7) 0.062(3) Uani 0.523(17) 1 d PG A 1 H52A H -0.7122 0.0663 0.0394 0.074 Uiso 0.523(17) 1 calc PR A 1 C53 C -0.7939(9) 0.1757(7) 0.0561(9) 0.067(5) Uani 0.523(17) 1 d PG A 1 H53A H -0.8721 0.1191 0.0592 0.080 Uiso 0.523(17) 1 calc PR A 1 C54 C -0.7745(6) 0.2900(9) 0.0633(7) 0.051(3) Uani 0.523(17) 1 d PG A 1 H54A H -0.8394 0.3114 0.0713 0.061 Uiso 0.523(17) 1 calc PR A 1 C55 C -0.6602(7) 0.3729(6) 0.0587(5) 0.0414(19) Uani 0.523(17) 1 d PG A 1 H55A H -0.6469 0.4510 0.0636 0.050 Uiso 0.523(17) 1 calc PR A 1 C56 C -0.5652(4) 0.3416(11) 0.0469(4) 0.045(3) Uani 0.523(17) 1 d PG A 1 H56A H -0.4871 0.3983 0.0437 0.054 Uiso 0.523(17) 1 calc PR A 1 C61 C -0.6190(7) 0.1645(12) 0.0376(4) 0.047(2) Uani 0.477(17) 1 d PG A 2 H61A H -0.5773 0.1164 0.0310 0.056 Uiso 0.477(17) 1 calc PR A 2 C62 C -0.7389(9) 0.1197(5) 0.0498(8) 0.045(2) Uani 0.477(17) 1 d PG A 2 H62A H -0.7791 0.0410 0.0516 0.054 Uiso 0.477(17) 1 calc PR A 2 C63 C -0.7999(9) 0.1900(10) 0.0595(10) 0.050(4) Uani 0.477(17) 1 d PG A 2 H63A H -0.8819 0.1594 0.0679 0.059 Uiso 0.477(17) 1 calc PR A 2 C64 C -0.7411(15) 0.3052(9) 0.0568(9) 0.063(4) Uani 0.477(17) 1 d PG A 2 H64A H -0.7828 0.3532 0.0634 0.076 Uiso 0.477(17) 1 calc PR A 2 C65 C -0.6212(14) 0.3500(6) 0.0446(5) 0.060(4) Uani 0.477(17) 1 d PG A 2 H65A H -0.5810 0.4287 0.0428 0.072 Uiso 0.477(17) 1 calc PR A 2 C66 C -0.5601(6) 0.2797(13) 0.0349(5) 0.051(4) Uani 0.477(17) 1 d PG A 2 H66A H -0.4782 0.3103 0.0265 0.062 Uiso 0.477(17) 1 calc PR A 2 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 Ga1 0.01886(12) 0.01969(12) 0.01538(11) 0.00181(9) 0.00472(9) 0.00758(10) Ga2 0.02096(13) 0.02792(14) 0.01775(12) 0.00248(10) 0.00490(10) 0.00944(11) S2 0.0239(3) 0.0286(3) 0.0142(2) 0.0053(2) 0.0074(2) 0.0155(2) S1 0.0160(3) 0.0226(3) 0.0195(3) 0.0063(2) 0.0027(2) 0.0067(2) S3 0.0239(3) 0.0190(3) 0.0247(3) 0.0042(2) 0.0116(2) 0.0085(2) Cl1 0.0308(3) 0.0309(3) 0.0229(3) -0.0062(2) 0.0034(2) 0.0095(3) Cl2 0.0426(4) 0.0337(3) 0.0297(3) 0.0025(3) 0.0062(3) 0.0231(3) Cl3 0.0281(3) 0.0384(3) 0.0182(3) 0.0008(2) 0.0036(2) 0.0097(3) Cl4 0.0256(3) 0.0301(3) 0.0232(3) 0.0039(2) 0.0064(2) 0.0142(2) Cl5 0.0255(3) 0.0622(5) 0.0358(3) 0.0193(3) 0.0122(3) 0.0101(3) B 0.0225(12) 0.0194(12) 0.0176(11) 0.0026(10) 0.0074(10) 0.0095(10) N11 0.0156(8) 0.0195(9) 0.0170(8) 0.0026(7) 0.0043(7) 0.0071(7) C11 0.0165(10) 0.0172(10) 0.0178(10) 0.0034(8) 0.0044(8) 0.0081(8) N12 0.0166(9) 0.0201(9) 0.0156(8) 0.0034(7) 0.0041(7) 0.0083(7) C12 0.0164(10) 0.0246(11) 0.0200(11) 0.0020(9) 0.0021(8) 0.0077(9) C13 0.0148(10) 0.0233(11) 0.0232(11) 0.0027(9) 0.0024(8) 0.0059(9) C14 0.0207(11) 0.0249(11) 0.0179(10) 0.0056(9) 0.0074(9) 0.0093(9) C15 0.0213(12) 0.0425(14) 0.0243(12) 0.0099(11) 0.0093(10) 0.0111(11) C16 0.0380(14) 0.0319(13) 0.0237(12) 0.0031(10) 0.0134(11) 0.0162(11) C17 0.0296(13) 0.0354(13) 0.0282(12) 0.0178(11) 0.0122(10) 0.0155(11) N21 0.0204(9) 0.0241(9) 0.0127(8) 0.0030(7) 0.0047(7) 0.0114(8) C21 0.0163(10) 0.0239(11) 0.0144(10) 0.0043(8) 0.0038(8) 0.0090(9) N22 0.0190(9) 0.0223(9) 0.0156(8) 0.0045(7) 0.0051(7) 0.0086(8) C22 0.0254(12) 0.0287(12) 0.0145(10) 0.0030(9) 0.0071(9) 0.0116(10) C23 0.0272(12) 0.0315(12) 0.0134(10) 0.0068(9) 0.0071(9) 0.0135(10) C24 0.0204(11) 0.0183(10) 0.0227(11) 0.0047(9) 0.0056(9) 0.0086(9) C25 0.0222(11) 0.0304(13) 0.0288(12) 0.0075(10) 0.0069(10) 0.0151(10) C26 0.0352(14) 0.0280(13) 0.0274(12) 0.0115(10) 0.0090(10) 0.0155(11) C27 0.0262(12) 0.0227(12) 0.0283(12) 0.0020(10) 0.0049(10) 0.0074(10) N31 0.0220(9) 0.0204(9) 0.0189(9) 0.0046(7) 0.0083(7) 0.0112(8) C31 0.0216(11) 0.0230(11) 0.0183(10) 0.0074(9) 0.0103(9) 0.0105(9) N32 0.0201(9) 0.0235(10) 0.0237(9) 0.0055(8) 0.0080(8) 0.0099(8) C32 0.0252(12) 0.0181(11) 0.0276(12) 0.0033(9) 0.0104(9) 0.0101(9) C33 0.0269(12) 0.0244(12) 0.0311(12) 0.0052(10) 0.0097(10) 0.0155(10) C34 0.0186(11) 0.0315(13) 0.0296(12) 0.0060(10) 0.0069(9) 0.0102(10) C35 0.0291(14) 0.0493(17) 0.0289(13) 0.0073(12) 0.0028(11) 0.0122(12) C36 0.0228(13) 0.0419(15) 0.0432(15) 0.0145(13) 0.0152(11) 0.0093(11) C37 0.0259(14) 0.0437(16) 0.0609(19) 0.0109(14) 0.0076(13) 0.0184(12) C41 0.0503(18) 0.0349(15) 0.0338(15) -0.0003(12) -0.0014(13) 0.0154(14) C42 0.065(2) 0.0443(17) 0.0323(15) 0.0065(13) 0.0177(15) 0.0219(16) C43 0.0405(16) 0.0364(15) 0.0518(18) 0.0050(14) 0.0118(14) 0.0164(13) C44 0.0457(17) 0.0391(16) 0.0404(16) 0.0101(13) -0.0009(13) 0.0200(14) C45 0.0552(18) 0.0328(15) 0.0400(15) 0.0131(12) 0.0132(14) 0.0241(14) C46 0.0407(16) 0.0271(14) 0.0479(17) 0.0064(12) 0.0087(13) 0.0154(12) C51 0.057(6) 0.070(9) 0.029(4) 0.011(5) 0.010(4) 0.042(6) C52 0.077(9) 0.048(5) 0.039(5) 0.008(4) 0.000(6) 0.017(5) C53 0.047(8) 0.090(10) 0.038(7) 0.019(7) 0.016(6) 0.004(7) C54 0.025(3) 0.078(8) 0.042(5) 0.019(4) 0.010(3) 0.015(4) C55 0.030(4) 0.069(5) 0.030(4) 0.021(3) 0.005(3) 0.025(3) C56 0.031(4) 0.079(8) 0.030(3) 0.016(4) 0.004(3) 0.031(4) C61 0.037(5) 0.057(7) 0.037(4) 0.013(5) 0.012(4) 0.012(5) C62 0.045(5) 0.059(5) 0.034(4) 0.012(4) 0.026(4) 0.020(4) C63 0.059(9) 0.065(9) 0.040(8) 0.015(6) 0.017(7) 0.042(8) C64 0.097(10) 0.085(9) 0.046(6) 0.034(6) 0.033(8) 0.065(9) C65 0.077(10) 0.051(5) 0.039(5) 0.018(4) 0.008(6) 0.018(6) C66 0.042(5) 0.056(8) 0.035(4) 0.020(5) 0.011(3) 0.000(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 Ga1 Cl1 2.1658(6) . ? Ga1 S2 2.2715(6) . ? Ga1 S3 2.2747(6) . ? Ga1 S1 2.2824(6) . ? Ga2 Cl5 2.1652(7) . ? Ga2 Cl2 2.1719(7) . ? Ga2 Cl4 2.1765(6) . ? Ga2 Cl3 2.1832(7) . ? S2 C21 1.742(2) . ? S1 C11 1.741(2) . ? S3 C31 1.741(2) . ? B H1 1.09(2) . ? B N21 1.550(3) . ? B N11 1.556(3) . ? B N31 1.558(3) . ? N11 C11 1.344(2) . ? N11 C12 1.381(3) . ? C11 N12 1.355(2) . ? N12 C13 1.386(3) . ? N12 C14 1.510(3) . ? C12 C13 1.342(3) . ? C14 C17 1.522(3) . ? C14 C16 1.524(3) . ? C14 C15 1.525(3) . ? N21 C21 1.354(3) . ? N21 C22 1.380(3) . ? C21 N22 1.353(3) . ? N22 C23 1.386(3) . ? N22 C24 1.516(3) . ? C22 C23 1.337(3) . ? C24 C26 1.523(3) . ? C24 C27 1.527(3) . ? C24 C25 1.528(3) . ? N31 C31 1.352(3) . ? N31 C32 1.376(3) . ? C31 N32 1.357(3) . ? N32 C33 1.380(3) . ? N32 C34 1.516(3) . ? C32 C33 1.342(3) . ? C34 C36 1.520(3) . ? C34 C37 1.525(3) . ? C34 C35 1.527(3) . ? C41 C42 1.373(4) . ? C41 C46 1.378(4) . ? C42 C43 1.385(4) . ? C43 C44 1.374(4) . ? C44 C45 1.381(4) . ? C45 C46 1.383(4) . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? 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 Ga1 S2 113.01(2) . . ? Cl1 Ga1 S3 110.35(2) . . ? S2 Ga1 S3 108.95(2) . . ? Cl1 Ga1 S1 109.72(2) . . ? S2 Ga1 S1 106.57(2) . . ? S3 Ga1 S1 108.06(2) . . ? Cl5 Ga2 Cl2 111.04(3) . . ? Cl5 Ga2 Cl4 108.91(3) . . ? Cl2 Ga2 Cl4 109.41(2) . . ? Cl5 Ga2 Cl3 110.06(3) . . ? Cl2 Ga2 Cl3 109.58(3) . . ? Cl4 Ga2 Cl3 107.78(2) . . ? C21 S2 Ga1 98.33(7) . . ? C11 S1 Ga1 96.81(7) . . ? C31 S3 Ga1 96.95(7) . . ? H1 B N21 108.0(11) . . ? H1 B N11 106.4(11) . . ? N21 B N11 111.06(17) . . ? H1 B N31 104.8(11) . . ? N21 B N31 113.24(17) . . ? N11 B N31 112.81(17) . . ? C11 N11 C12 107.67(17) . . ? C11 N11 B 133.82(17) . . ? C12 N11 B 118.18(17) . . ? N11 C11 N12 108.81(17) . . ? N11 C11 S1 125.24(15) . . ? N12 C11 S1 125.95(15) . . ? C11 N12 C13 107.62(17) . . ? C11 N12 C14 127.94(17) . . ? C13 N12 C14 124.24(17) . . ? C13 C12 N11 108.40(18) . . ? C12 C13 N12 107.50(18) . . ? N12 C14 C17 109.93(17) . . ? N12 C14 C16 108.73(17) . . ? C17 C14 C16 112.65(19) . . ? N12 C14 C15 108.39(17) . . ? C17 C14 C15 108.15(18) . . ? C16 C14 C15 108.89(18) . . ? C21 N21 C22 106.96(17) . . ? C21 N21 B 133.65(17) . . ? C22 N21 B 119.34(17) . . ? N22 C21 N21 108.84(17) . . ? N22 C21 S2 124.74(15) . . ? N21 C21 S2 126.42(16) . . ? C21 N22 C23 107.76(17) . . ? C21 N22 C24 127.59(17) . . ? C23 N22 C24 124.65(17) . . ? C23 C22 N21 109.07(19) . . ? C22 C23 N22 107.35(18) . . ? N22 C24 C26 108.00(17) . . ? N22 C24 C27 108.47(17) . . ? C26 C24 C27 110.24(18) . . ? N22 C24 C25 109.18(17) . . ? C26 C24 C25 108.51(18) . . ? C27 C24 C25 112.34(18) . . ? C31 N31 C32 107.42(17) . . ? C31 N31 B 134.03(18) . . ? C32 N31 B 118.48(17) . . ? N31 C31 N32 108.56(18) . . ? N31 C31 S3 125.34(16) . . ? N32 C31 S3 126.10(16) . . ? C31 N32 C33 107.79(18) . . ? C31 N32 C34 127.80(18) . . ? C33 N32 C34 124.31(18) . . ? C33 C32 N31 108.69(19) . . ? C32 C33 N32 107.54(19) . . ? N32 C34 C36 109.77(18) . . ? N32 C34 C37 108.48(19) . . ? C36 C34 C37 108.3(2) . . ? N32 C34 C35 108.00(18) . . ? C36 C34 C35 112.7(2) . . ? C37 C34 C35 109.5(2) . . ? C42 C41 C46 120.1(3) . . ? C41 C42 C43 120.4(3) . . ? C44 C43 C42 119.5(3) . . ? C43 C44 C45 120.4(3) . . ? C44 C45 C46 119.9(3) . . ? C41 C46 C45 119.7(3) . . ? C52 C51 C56 120.0 . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C62 C61 C66 120.0 . . ? C63 C62 C61 120.0 . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C66 C65 C64 120.0 . . ? C65 C66 C61 120.0 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.61 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.522 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.084 # Attachment '- TmGaGaTmI2 (nova).cif' data_nova_2 _database_code_depnum_ccdc_archive 'CCDC 763468' #TrackingRef '- TmGaGaTmI2 (nova).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H86 B2 Ga2 I2 N18 S6' _chemical_formula_weight 1594.63 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 Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 11.4967(17) _cell_length_b 11.4967(17) _cell_length_c 16.993(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1945.2(7) _cell_formula_units_Z 1 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9209 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 31.88 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 810 _exptl_absorpt_coefficient_mu 1.691 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5511 _exptl_absorpt_correction_T_max 0.7285 _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 31504 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 32.31 _reflns_number_total 4452 _reflns_number_gt 3705 _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.022 -0.014 0.000 633.1 109.5 2 0.333 0.667 0.496 13.3 3.5 3 0.667 0.333 0.504 13.3 4.6 _platon_squeeze_details ;The unit cell contains 6 acetonitrile molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON ; _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^)+(0.0663P)^2^+12.5804P] 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 0.0100(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4452 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1792 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.0000 1.0000 0.42905(4) 0.01779(18) Uani 1 3 d S . . I I 0.3333 0.6667 0.09921(3) 0.03270(18) Uani 1 3 d S . . S S -0.12807(10) 0.78799(10) 0.37480(6) 0.0210(2) Uani 1 1 d . . . B B 0.0000 1.0000 0.2155(5) 0.0235(15) Uani 1 3 d S . . H1 H 0.0000 1.0000 0.144(6) 0.028 Uiso 1 3 d S . . N1 N 0.0255(3) 0.8843(4) 0.2411(2) 0.0201(6) Uani 1 1 d . . . C1 C -0.0209(4) 0.7951(4) 0.3006(2) 0.0189(7) Uani 1 1 d . . . N2 N 0.0337(3) 0.7141(3) 0.2938(2) 0.0211(6) Uani 1 1 d . . . C2 C 0.1122(4) 0.8607(5) 0.1958(3) 0.0261(8) Uani 1 1 d . . . H2A H 0.1594 0.9096 0.1503 0.031 Uiso 1 1 calc R . . C3 C 0.1174(4) 0.7563(4) 0.2279(3) 0.0258(8) Uani 1 1 d . . . H3A H 0.1688 0.7182 0.2090 0.031 Uiso 1 1 calc R . . C4 C 0.0160(4) 0.6035(4) 0.3474(3) 0.0288(9) Uani 1 1 d . . . C5 C 0.0835(6) 0.5314(5) 0.3097(4) 0.0416(14) Uani 1 1 d . . . H5A H 0.0404 0.4929 0.2591 0.062 Uiso 1 1 calc R . . H5B H 0.0743 0.4595 0.3447 0.062 Uiso 1 1 calc R . . H5C H 0.1790 0.5957 0.3012 0.062 Uiso 1 1 calc R . . C6 C 0.0852(6) 0.6656(6) 0.4265(4) 0.0393(12) Uani 1 1 d . . . H6A H 0.1801 0.7311 0.4171 0.059 Uiso 1 1 calc R . . H6B H 0.0783 0.5945 0.4613 0.059 Uiso 1 1 calc R . . H6C H 0.0412 0.7105 0.4511 0.059 Uiso 1 1 calc R . . C7 C -0.1328(5) 0.5011(5) 0.3592(4) 0.0393(13) Uani 1 1 d . . . H7A H -0.1744 0.4641 0.3081 0.059 Uiso 1 1 calc R . . H7B H -0.1777 0.5453 0.3837 0.059 Uiso 1 1 calc R . . H7C H -0.1417 0.4284 0.3933 0.059 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 0.0172(2) 0.0172(2) 0.0189(3) 0.000 0.000 0.00862(11) I 0.0333(2) 0.0333(2) 0.0315(3) 0.000 0.000 0.01665(11) S 0.0179(4) 0.0149(4) 0.0269(5) 0.0004(3) 0.0051(3) 0.0059(3) B 0.022(2) 0.022(2) 0.026(4) 0.000 0.000 0.0111(11) N1 0.0181(14) 0.0207(15) 0.0218(15) -0.0010(12) 0.0036(12) 0.0098(13) C1 0.0130(15) 0.0166(15) 0.0257(18) -0.0027(13) -0.0025(13) 0.0064(13) N2 0.0155(14) 0.0149(14) 0.0323(18) -0.0039(12) 0.0003(13) 0.0071(12) C2 0.0222(19) 0.0240(19) 0.030(2) -0.0031(16) 0.0060(16) 0.0098(16) C3 0.0181(17) 0.0238(19) 0.037(2) -0.0041(17) 0.0032(16) 0.0118(15) C4 0.0189(18) 0.0157(17) 0.050(3) 0.0059(17) 0.0033(18) 0.0071(15) C5 0.033(2) 0.019(2) 0.079(4) 0.007(2) 0.009(3) 0.0166(19) C6 0.035(3) 0.033(3) 0.042(3) 0.010(2) -0.005(2) 0.011(2) C7 0.0180(19) 0.0178(19) 0.077(4) 0.007(2) 0.003(2) 0.0053(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 S 2.3172(11) 3_465 ? Ga S 2.3173(11) . ? Ga S 2.3173(11) 2_675 ? Ga Ga 2.4115(17) 4_576 ? S C1 1.736(4) . ? B H1 1.22(11) . ? B N1 1.561(4) 2_675 ? B N1 1.561(4) . ? B N1 1.561(4) 3_465 ? N1 C1 1.346(5) . ? N1 C2 1.389(5) . ? C1 N2 1.362(5) . ? N2 C3 1.397(6) . ? N2 C4 1.493(6) . ? C2 C3 1.347(7) . ? C4 C7 1.529(6) . ? C4 C5 1.530(7) . ? C4 C6 1.543(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S Ga S 105.22(4) 3_465 . ? S Ga S 105.23(4) 3_465 2_675 ? S Ga S 105.22(4) . 2_675 ? S Ga Ga 113.44(3) 3_465 4_576 ? S Ga Ga 113.44(3) . 4_576 ? S Ga Ga 113.44(3) 2_675 4_576 ? C1 S Ga 100.18(13) . . ? H1 B N1 106.2(3) . 2_675 ? H1 B N1 106.2(3) . . ? N1 B N1 112.5(3) 2_675 . ? H1 B N1 106.2(3) . 3_465 ? N1 B N1 112.5(3) 2_675 3_465 ? N1 B N1 112.5(3) . 3_465 ? C1 N1 C2 108.5(4) . . ? C1 N1 B 133.4(4) . . ? C2 N1 B 118.0(4) . . ? N1 C1 N2 108.3(4) . . ? N1 C1 S 125.6(3) . . ? N2 C1 S 126.1(3) . . ? C1 N2 C3 107.7(4) . . ? C1 N2 C4 128.1(4) . . ? C3 N2 C4 124.2(4) . . ? C3 C2 N1 107.8(4) . . ? C2 C3 N2 107.7(4) . . ? N2 C4 C7 111.0(4) . . ? N2 C4 C5 108.4(4) . . ? C7 C4 C5 108.2(4) . . ? N2 C4 C6 108.5(4) . . ? C7 C4 C6 111.2(5) . . ? C5 C4 C6 109.3(5) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 32.31 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.949 _refine_diff_density_min -2.060 _refine_diff_density_rms 0.175 # Attachment '- TmGaGaTm(GaCl4)2 (ky65s10).cif' data_ky65s10 _database_code_depnum_ccdc_archive 'CCDC 763469' #TrackingRef '- TmGaGaTm(GaCl4)2 (ky65s10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H80 B2 Cl8 Ga4 N12 O2 S6' _chemical_formula_weight 1633.70 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.241(7) _cell_length_b 11.857(7) _cell_length_c 15.252(9) _cell_angle_alpha 110.582(9) _cell_angle_beta 107.533(9) _cell_angle_gamma 94.069(9) _cell_volume 1778.7(18) _cell_formula_units_Z 1 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 4232 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.35 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 2.020 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6321 _exptl_absorpt_correction_T_max 0.9801 _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 16090 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.1339 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7261 _reflns_number_gt 4095 _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7261 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1247 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0870 _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 Ga1 Ga -1.01886(6) 2.03704(6) 1.43384(4) 0.01758(16) Uani 1 1 d . . . Ga2 Ga -0.27889(6) 1.66405(6) 0.83844(5) 0.02787(19) Uani 1 1 d . . . S1 S -0.83719(13) 2.12326(13) 1.42070(11) 0.0212(3) Uani 1 1 d . . . S2 S -1.13600(14) 2.19143(13) 1.45012(10) 0.0212(3) Uani 1 1 d . . . S3 S -1.13141(13) 1.89328(13) 1.27539(10) 0.0210(3) Uani 1 1 d . . . Cl1 Cl -0.34794(15) 1.65733(16) 0.68818(12) 0.0422(4) Uani 1 1 d . . . Cl2 Cl -0.28273(16) 1.84061(15) 0.94543(13) 0.0463(5) Uani 1 1 d . . . Cl3 Cl -0.39325(15) 1.51850(14) 0.85067(12) 0.0372(4) Uani 1 1 d . . . Cl4 Cl -0.08432(14) 1.63679(15) 0.86879(12) 0.0345(4) Uani 1 1 d . . . B B -1.0763(6) 2.1555(6) 1.2334(5) 0.0192(15) Uani 1 1 d . . . H1 H -1.093(5) 2.193(4) 1.174(4) 0.023 Uiso 1 1 d . . . O O -1.3501(4) 2.1692(4) 0.9638(3) 0.0388(12) Uani 1 1 d . . . C1 C -1.3899(6) 2.2630(6) 0.9867(5) 0.0329(16) Uani 1 1 d . . . C2 C -1.3155(7) 2.3739(6) 1.0772(5) 0.058(2) Uani 1 1 d . . . H2A H -1.2344 2.3564 1.1112 0.087 Uiso 1 1 calc R . . H2B H -1.3639 2.3962 1.1224 0.087 Uiso 1 1 calc R . . H2C H -1.2990 2.4421 1.0576 0.087 Uiso 1 1 calc R . . C3 C -1.5166(6) 2.2754(6) 0.9256(5) 0.0431(18) Uani 1 1 d . . . H3A H -1.5577 2.1977 0.8680 0.065 Uiso 1 1 calc R . . H3B H -1.5045 2.3410 0.9021 0.065 Uiso 1 1 calc R . . H3C H -1.5704 2.2957 0.9667 0.065 Uiso 1 1 calc R . . N11 N -0.9756(4) 2.2578(4) 1.3286(3) 0.0193(11) Uani 1 1 d . . . C11 C -0.8831(5) 2.2556(5) 1.4080(4) 0.0197(13) Uani 1 1 d . . . N12 N -0.8328(4) 2.3707(4) 1.4748(3) 0.0188(11) Uani 1 1 d . . . C12 C -0.9795(5) 2.3784(5) 1.3456(4) 0.0209(13) Uani 1 1 d . . . H12A H -1.0350 2.4075 1.3014 0.025 Uiso 1 1 calc R . . C13 C -0.8920(5) 2.4489(5) 1.4350(4) 0.0226(14) Uani 1 1 d . . . H13A H -0.8741 2.5361 1.4653 0.027 Uiso 1 1 calc R . . C14 C -0.7331(5) 2.4154(5) 1.5781(4) 0.0209(13) Uani 1 1 d . . . C15 C -0.7027(5) 2.5538(5) 1.6238(4) 0.0288(15) Uani 1 1 d . . . H15A H -0.7793 2.5847 1.6311 0.043 Uiso 1 1 calc R . . H15B H -0.6736 2.5844 1.5804 0.043 Uiso 1 1 calc R . . H15C H -0.6356 2.5823 1.6896 0.043 Uiso 1 1 calc R . . C16 C -0.6104(5) 2.3707(5) 1.5694(4) 0.0307(15) Uani 1 1 d . . . H16A H -0.6270 2.2807 1.5414 0.046 Uiso 1 1 calc R . . H16B H -0.5441 2.4022 1.6358 0.046 Uiso 1 1 calc R . . H16C H -0.5818 2.4009 1.5255 0.046 Uiso 1 1 calc R . . C17 C -0.7845(6) 2.3667(5) 1.6412(4) 0.0327(16) Uani 1 1 d . . . H17A H -0.8622 2.3972 1.6454 0.049 Uiso 1 1 calc R . . H17B H -0.7208 2.3946 1.7085 0.049 Uiso 1 1 calc R . . H17C H -0.8040 2.2767 1.6108 0.049 Uiso 1 1 calc R . . C21 C -1.2399(5) 2.1376(5) 1.3265(4) 0.0181(13) Uani 1 1 d . . . N21 N -1.2064(4) 2.1354(4) 1.2488(3) 0.0188(11) Uani 1 1 d . . . N22 N -1.3672(4) 2.0962(4) 1.2948(3) 0.0205(11) Uani 1 1 d . . . C22 C -1.3172(5) 2.0921(5) 1.1658(4) 0.0224(14) Uani 1 1 d . . . H22A H -1.3229 2.0806 1.0997 0.027 Uiso 1 1 calc R . . C23 C -1.4140(5) 2.0692(5) 1.1940(4) 0.0254(14) Uani 1 1 d . . . H23A H -1.5006 2.0393 1.1517 0.030 Uiso 1 1 calc R . . C24 C -1.4432(5) 2.0670(5) 1.3525(4) 0.0253(14) Uani 1 1 d . . . C25 C -1.3960(6) 1.9651(5) 1.3846(5) 0.0361(17) Uani 1 1 d . . . H25A H -1.4024 1.8929 1.3255 0.054 Uiso 1 1 calc R . . H25B H -1.4483 1.9428 1.4194 0.054 Uiso 1 1 calc R . . H25C H -1.3071 1.9941 1.4296 0.054 Uiso 1 1 calc R . . C26 C -1.4346(5) 2.1814(6) 1.4425(4) 0.0329(16) Uani 1 1 d . . . H26A H -1.4647 2.2454 1.4198 0.049 Uiso 1 1 calc R . . H26B H -1.3460 2.2114 1.4880 0.049 Uiso 1 1 calc R . . H26C H -1.4876 2.1610 1.4774 0.049 Uiso 1 1 calc R . . C27 C -1.5827(5) 2.0214(6) 1.2853(4) 0.0312(16) Uani 1 1 d . . . H27A H -1.5909 1.9481 1.2264 0.047 Uiso 1 1 calc R . . H27B H -1.6143 2.0859 1.2640 0.047 Uiso 1 1 calc R . . H27C H -1.6327 2.0009 1.3223 0.047 Uiso 1 1 calc R . . N31 N -1.0282(4) 2.0340(4) 1.1970(3) 0.0172(11) Uani 1 1 d . . . C31 C -1.0378(5) 1.9305(5) 1.2122(4) 0.0179(13) Uani 1 1 d . . . N32 N -0.9663(4) 1.8574(4) 1.1712(3) 0.0176(11) Uani 1 1 d . . . C32 C -0.9483(5) 2.0266(5) 1.1425(4) 0.0223(14) Uani 1 1 d . . . H32A H -0.9245 2.0873 1.1203 0.027 Uiso 1 1 calc R . . C33 C -0.9107(5) 1.9192(5) 1.1266(4) 0.0234(14) Uani 1 1 d . . . H33A H -0.8554 1.8900 1.0909 0.028 Uiso 1 1 calc R . . C34 C -0.9430(5) 1.7353(5) 1.1747(4) 0.0193(13) Uani 1 1 d . . . C35 C -0.8531(5) 1.6901(5) 1.1190(4) 0.0282(15) Uani 1 1 d . . . H35A H -0.8927 1.6784 1.0489 0.042 Uiso 1 1 calc R . . H35B H -0.8353 1.6118 1.1225 0.042 Uiso 1 1 calc R . . H35C H -0.7734 1.7510 1.1495 0.042 Uiso 1 1 calc R . . C36 C -1.0686(5) 1.6424(5) 1.1239(4) 0.0262(14) Uani 1 1 d . . . H36A H -1.1274 1.6713 1.1592 0.039 Uiso 1 1 calc R . . H36B H -1.0531 1.5628 1.1257 0.039 Uiso 1 1 calc R . . H36C H -1.1059 1.6335 1.0543 0.039 Uiso 1 1 calc R . . C37 C -0.8808(6) 1.7510(5) 1.2832(4) 0.0331(16) Uani 1 1 d . . . H37A H -0.9380 1.7803 1.3200 0.050 Uiso 1 1 calc R . . H37B H -0.8005 1.8110 1.3139 0.050 Uiso 1 1 calc R . . H37C H -0.8641 1.6719 1.2854 0.050 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 Ga1 0.0148(3) 0.0199(4) 0.0163(3) 0.0062(3) 0.0038(3) 0.0051(3) Ga2 0.0194(4) 0.0327(4) 0.0329(4) 0.0166(3) 0.0066(3) 0.0049(3) S1 0.0164(8) 0.0202(8) 0.0252(8) 0.0081(7) 0.0057(7) 0.0049(6) S2 0.0225(8) 0.0236(8) 0.0184(8) 0.0078(7) 0.0079(7) 0.0093(6) S3 0.0207(8) 0.0200(8) 0.0190(8) 0.0048(7) 0.0065(7) 0.0007(6) Cl1 0.0311(10) 0.0591(12) 0.0386(10) 0.0281(9) 0.0045(8) 0.0087(8) Cl2 0.0462(11) 0.0365(10) 0.0538(12) 0.0101(9) 0.0232(10) 0.0082(8) Cl3 0.0298(9) 0.0391(10) 0.0439(10) 0.0198(8) 0.0119(8) -0.0015(7) Cl4 0.0193(8) 0.0493(10) 0.0411(10) 0.0257(9) 0.0090(8) 0.0093(7) B 0.014(3) 0.029(4) 0.021(4) 0.013(3) 0.010(3) 0.006(3) O 0.037(3) 0.037(3) 0.034(3) 0.009(2) 0.007(2) 0.004(2) C1 0.027(4) 0.039(4) 0.030(4) 0.010(3) 0.013(3) -0.006(3) C2 0.040(5) 0.051(5) 0.054(5) -0.004(4) 0.008(4) 0.005(4) C3 0.040(4) 0.031(4) 0.050(5) 0.008(3) 0.016(4) -0.001(3) N11 0.019(3) 0.017(3) 0.021(3) 0.007(2) 0.006(2) 0.007(2) C11 0.012(3) 0.018(3) 0.024(3) 0.005(3) 0.005(3) -0.001(2) N12 0.014(3) 0.016(3) 0.022(3) 0.004(2) 0.004(2) 0.004(2) C12 0.020(3) 0.019(3) 0.026(3) 0.012(3) 0.008(3) 0.010(3) C13 0.027(4) 0.013(3) 0.030(4) 0.008(3) 0.013(3) 0.008(3) C14 0.015(3) 0.020(3) 0.018(3) 0.002(3) -0.001(3) 0.001(2) C15 0.022(3) 0.029(4) 0.027(4) 0.005(3) 0.004(3) 0.004(3) C16 0.019(3) 0.030(4) 0.029(4) 0.006(3) -0.002(3) 0.003(3) C17 0.035(4) 0.030(4) 0.022(3) 0.002(3) 0.006(3) 0.003(3) C21 0.016(3) 0.021(3) 0.018(3) 0.010(3) 0.005(3) 0.007(2) N21 0.011(2) 0.024(3) 0.019(3) 0.007(2) 0.004(2) 0.006(2) N22 0.012(2) 0.025(3) 0.022(3) 0.007(2) 0.006(2) 0.005(2) C22 0.017(3) 0.030(3) 0.014(3) 0.007(3) 0.000(3) 0.002(3) C23 0.012(3) 0.034(4) 0.028(4) 0.012(3) 0.003(3) 0.003(3) C24 0.017(3) 0.037(4) 0.030(4) 0.017(3) 0.013(3) 0.009(3) C25 0.030(4) 0.038(4) 0.055(5) 0.031(4) 0.019(4) 0.013(3) C26 0.022(3) 0.050(4) 0.034(4) 0.019(3) 0.015(3) 0.016(3) C27 0.016(3) 0.041(4) 0.039(4) 0.017(3) 0.011(3) 0.005(3) N31 0.011(2) 0.023(3) 0.013(2) 0.004(2) 0.003(2) -0.003(2) C31 0.015(3) 0.016(3) 0.015(3) 0.002(3) 0.001(3) 0.000(2) N32 0.015(2) 0.018(3) 0.020(3) 0.004(2) 0.011(2) 0.001(2) C32 0.015(3) 0.031(4) 0.018(3) 0.007(3) 0.004(3) 0.002(3) C33 0.014(3) 0.030(4) 0.022(3) 0.005(3) 0.007(3) 0.000(3) C34 0.021(3) 0.014(3) 0.018(3) 0.002(3) 0.005(3) 0.002(2) C35 0.026(4) 0.030(4) 0.036(4) 0.016(3) 0.015(3) 0.014(3) C36 0.025(3) 0.024(3) 0.030(4) 0.008(3) 0.013(3) 0.006(3) C37 0.030(4) 0.030(4) 0.031(4) 0.009(3) 0.004(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 Ga1 S3 2.3026(18) . ? Ga1 S1 2.3131(19) . ? Ga1 S2 2.3165(18) . ? Ga1 Ga1 2.4099(17) 2_398 ? Ga2 Cl1 2.157(2) . ? Ga2 Cl2 2.168(2) . ? Ga2 Cl4 2.168(2) . ? Ga2 Cl3 2.1729(19) . ? S1 C11 1.742(6) . ? S2 C21 1.746(5) . ? S3 C31 1.753(6) . ? B H1 1.11(5) . ? B N31 1.550(8) . ? B N11 1.562(8) . ? B N21 1.565(7) . ? O C1 1.205(7) . ? C1 C2 1.485(8) . ? C1 C3 1.498(9) . ? N11 C11 1.348(6) . ? N11 C12 1.367(6) . ? C11 N12 1.337(6) . ? N12 C13 1.382(7) . ? N12 C14 1.511(6) . ? C12 C13 1.342(7) . ? C14 C15 1.506(7) . ? C14 C17 1.508(8) . ? C14 C16 1.538(8) . ? C21 N21 1.339(6) . ? C21 N22 1.356(6) . ? N21 C22 1.385(6) . ? N22 C23 1.373(7) . ? N22 C24 1.501(7) . ? C22 C23 1.329(7) . ? C24 C26 1.524(8) . ? C24 C27 1.524(7) . ? C24 C25 1.528(8) . ? N31 C31 1.330(6) . ? N31 C32 1.383(6) . ? C31 N32 1.345(6) . ? N32 C33 1.390(7) . ? N32 C34 1.505(7) . ? C32 C33 1.334(7) . ? C34 C35 1.518(7) . ? C34 C36 1.525(7) . ? C34 C37 1.526(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Ga1 S1 104.62(7) . . ? S3 Ga1 S2 103.10(6) . . ? S1 Ga1 S2 103.27(7) . . ? S3 Ga1 Ga1 115.66(7) . 2_398 ? S1 Ga1 Ga1 114.86(6) . 2_398 ? S2 Ga1 Ga1 113.83(6) . 2_398 ? Cl1 Ga2 Cl2 110.98(8) . . ? Cl1 Ga2 Cl4 107.01(7) . . ? Cl2 Ga2 Cl4 109.47(7) . . ? Cl1 Ga2 Cl3 110.27(7) . . ? Cl2 Ga2 Cl3 109.60(8) . . ? Cl4 Ga2 Cl3 109.48(7) . . ? C11 S1 Ga1 99.52(19) . . ? C21 S2 Ga1 98.57(18) . . ? C31 S3 Ga1 98.67(18) . . ? H1 B N31 108(2) . . ? H1 B N11 105(3) . . ? N31 B N11 113.0(5) . . ? H1 B N21 106(3) . . ? N31 B N21 112.5(5) . . ? N11 B N21 111.0(4) . . ? O C1 C2 121.8(6) . . ? O C1 C3 122.2(6) . . ? C2 C1 C3 115.9(6) . . ? C11 N11 C12 107.3(4) . . ? C11 N11 B 133.4(5) . . ? C12 N11 B 119.2(5) . . ? N12 C11 N11 109.1(5) . . ? N12 C11 S1 125.8(4) . . ? N11 C11 S1 125.1(4) . . ? C11 N12 C13 107.8(5) . . ? C11 N12 C14 129.1(5) . . ? C13 N12 C14 123.1(4) . . ? C13 C12 N11 108.6(5) . . ? C12 C13 N12 107.2(5) . . ? C15 C14 C17 110.2(5) . . ? C15 C14 N12 109.8(4) . . ? C17 C14 N12 108.4(4) . . ? C15 C14 C16 107.8(5) . . ? C17 C14 C16 111.7(5) . . ? N12 C14 C16 109.0(4) . . ? N21 C21 N22 109.5(5) . . ? N21 C21 S2 125.0(4) . . ? N22 C21 S2 125.5(4) . . ? C21 N21 C22 106.6(4) . . ? C21 N21 B 134.3(5) . . ? C22 N21 B 118.6(5) . . ? C21 N22 C23 107.0(5) . . ? C21 N22 C24 127.9(5) . . ? C23 N22 C24 124.6(5) . . ? C23 C22 N21 108.6(5) . . ? C22 C23 N22 108.2(5) . . ? N22 C24 C26 110.9(5) . . ? N22 C24 C27 109.1(4) . . ? C26 C24 C27 107.8(5) . . ? N22 C24 C25 109.2(5) . . ? C26 C24 C25 111.2(5) . . ? C27 C24 C25 108.6(5) . . ? C31 N31 C32 107.3(5) . . ? C31 N31 B 134.2(5) . . ? C32 N31 B 118.3(5) . . ? N31 C31 N32 110.2(5) . . ? N31 C31 S3 125.1(4) . . ? N32 C31 S3 124.7(4) . . ? C31 N32 C33 106.4(4) . . ? C31 N32 C34 128.6(4) . . ? C33 N32 C34 125.0(4) . . ? C33 C32 N31 108.0(5) . . ? C32 C33 N32 108.2(5) . . ? N32 C34 C35 108.8(4) . . ? N32 C34 C36 109.6(4) . . ? C35 C34 C36 109.0(4) . . ? N32 C34 C37 109.5(4) . . ? C35 C34 C37 108.7(5) . . ? C36 C34 C37 111.2(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.137 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.128 # Attachment '- TmGaII (TMGAIS10).cif' data_tmgais10 _database_code_depnum_ccdc_archive 'CCDC 763470' #TrackingRef '- TmGaII (TMGAIS10).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H40 B Ga I2 N6 S3' _chemical_formula_weight 879.16 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 11.6794(5) _cell_length_b 16.3820(7) _cell_length_c 19.2080(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.4430(10) _cell_angle_gamma 90.00 _cell_volume 3673.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 7143 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.51 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 2.626 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.5064 _exptl_absorpt_correction_T_max 0.7792 _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 24641 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.73 _reflns_number_total 7759 _reflns_number_gt 5281 _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 ADPs of a solvent molecule of benzene 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^)+(0.0317P)^2^+3.0913P] 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 7759 _refine_ls_number_parameters 395 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.011 _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 0.29428(3) 0.14159(3) -0.10961(2) 0.03501(11) Uani 1 1 d . . . I1 I 0.32113(3) -0.004663(18) -0.070951(17) 0.06591(11) Uani 1 1 d . . . I2 I 0.21677(2) 0.500847(18) 0.035222(16) 0.04985(9) Uani 1 1 d . . . S1 S 0.45428(8) 0.18569(6) -0.16397(5) 0.0388(2) Uani 1 1 d . . . S2 S 0.26268(8) 0.22348(6) -0.01638(5) 0.0364(2) Uani 1 1 d . . . S3 S 0.14330(8) 0.15489(6) -0.18668(5) 0.0409(2) Uani 1 1 d . . . B B 0.2617(4) 0.3458(3) -0.1619(2) 0.0360(10) Uani 1 1 d . . . H1 H 0.252(3) 0.408(2) -0.1756(19) 0.043 Uiso 1 1 d . . . N11 N 0.3129(2) 0.30136(19) -0.22519(15) 0.0324(7) Uani 1 1 d . . . N12 N 0.4054(2) 0.22653(19) -0.30060(15) 0.0334(7) Uani 1 1 d . . . N21 N 0.3463(2) 0.34628(18) -0.09814(15) 0.0317(7) Uani 1 1 d . . . N22 N 0.4459(2) 0.32891(19) -0.00082(15) 0.0327(7) Uani 1 1 d . . . N31 N 0.1406(2) 0.31476(19) -0.14280(15) 0.0338(7) Uani 1 1 d . . . N32 N -0.0197(3) 0.2491(2) -0.12275(16) 0.0397(8) Uani 1 1 d . . . C11 C 0.3882(3) 0.2396(2) -0.23206(18) 0.0312(8) Uani 1 1 d . . . C12 C 0.2813(3) 0.3266(3) -0.29140(19) 0.0405(10) Uani 1 1 d . . . H12A H 0.2289 0.3686 -0.3024 0.049 Uiso 1 1 calc R . . C13 C 0.3377(3) 0.2814(3) -0.3374(2) 0.0424(10) Uani 1 1 d . . . H13A H 0.3322 0.2862 -0.3862 0.051 Uiso 1 1 calc R . . C14 C 0.4813(3) 0.1630(3) -0.3340(2) 0.0437(10) Uani 1 1 d . . . C15 C 0.6033(3) 0.1723(3) -0.3063(2) 0.0585(13) Uani 1 1 d . . . H15A H 0.6322 0.2257 -0.3189 0.088 Uiso 1 1 calc R . . H15B H 0.6510 0.1304 -0.3264 0.088 Uiso 1 1 calc R . . H15C H 0.6049 0.1669 -0.2561 0.088 Uiso 1 1 calc R . . C16 C 0.4797(4) 0.1777(3) -0.4124(2) 0.0666(14) Uani 1 1 d . . . H16A H 0.5111 0.2312 -0.4219 0.100 Uiso 1 1 calc R . . H16B H 0.4015 0.1748 -0.4304 0.100 Uiso 1 1 calc R . . H16C H 0.5255 0.1363 -0.4347 0.100 Uiso 1 1 calc R . . C17 C 0.4328(4) 0.0795(3) -0.3189(3) 0.0654(14) Uani 1 1 d . . . H17A H 0.4794 0.0381 -0.3406 0.098 Uiso 1 1 calc R . . H17B H 0.3549 0.0762 -0.3375 0.098 Uiso 1 1 calc R . . H17C H 0.4329 0.0707 -0.2690 0.098 Uiso 1 1 calc R . . C21 C 0.3532(3) 0.3030(2) -0.03895(18) 0.0303(8) Uani 1 1 d . . . C22 C 0.4362(3) 0.4009(2) -0.0970(2) 0.0383(9) Uani 1 1 d . . . H22A H 0.4520 0.4389 -0.1322 0.046 Uiso 1 1 calc R . . C23 C 0.4970(3) 0.3910(2) -0.0379(2) 0.0395(9) Uani 1 1 d . . . H23A H 0.5625 0.4207 -0.0239 0.047 Uiso 1 1 calc R . . C24 C 0.4896(3) 0.2979(3) 0.0690(2) 0.0396(9) Uani 1 1 d . . . C25 C 0.3938(4) 0.3024(3) 0.1215(2) 0.0559(12) Uani 1 1 d . . . H25A H 0.3307 0.2678 0.1060 0.084 Uiso 1 1 calc R . . H25B H 0.3673 0.3584 0.1251 0.084 Uiso 1 1 calc R . . H25C H 0.4224 0.2840 0.1666 0.084 Uiso 1 1 calc R . . C26 C 0.5325(4) 0.2111(3) 0.0598(2) 0.0547(12) Uani 1 1 d . . . H26A H 0.4691 0.1762 0.0453 0.082 Uiso 1 1 calc R . . H26B H 0.5652 0.1914 0.1036 0.082 Uiso 1 1 calc R . . H26C H 0.5905 0.2102 0.0245 0.082 Uiso 1 1 calc R . . C27 C 0.5879(4) 0.3522(3) 0.0939(3) 0.0647(14) Uani 1 1 d . . . H27A H 0.5599 0.4072 0.1009 0.097 Uiso 1 1 calc R . . H27B H 0.6468 0.3528 0.0592 0.097 Uiso 1 1 calc R . . H27C H 0.6197 0.3311 0.1374 0.097 Uiso 1 1 calc R . . C31 C 0.0856(3) 0.2428(2) -0.15007(19) 0.0351(9) Uani 1 1 d . . . C32 C 0.0679(3) 0.3673(3) -0.10876(19) 0.0413(10) Uani 1 1 d . . . H32A H 0.0844 0.4216 -0.0960 0.050 Uiso 1 1 calc R . . C33 C -0.0297(3) 0.3276(3) -0.0972(2) 0.0449(10) Uani 1 1 d . . . H33A H -0.0941 0.3493 -0.0755 0.054 Uiso 1 1 calc R . . C34 C -0.1090(4) 0.1835(3) -0.1154(2) 0.0524(12) Uani 1 1 d . . . C35 C -0.2161(4) 0.2230(4) -0.0846(3) 0.0843(18) Uani 1 1 d . . . H35A H -0.2475 0.2629 -0.1172 0.126 Uiso 1 1 calc R . . H35B H -0.1954 0.2497 -0.0411 0.126 Uiso 1 1 calc R . . H35C H -0.2729 0.1812 -0.0763 0.126 Uiso 1 1 calc R . . C36 C -0.0613(4) 0.1192(3) -0.0646(3) 0.0725(16) Uani 1 1 d . . . H36A H 0.0057 0.0938 -0.0841 0.109 Uiso 1 1 calc R . . H36B H -0.1192 0.0781 -0.0567 0.109 Uiso 1 1 calc R . . H36C H -0.0400 0.1451 -0.0207 0.109 Uiso 1 1 calc R . . C37 C -0.1408(4) 0.1486(3) -0.1864(2) 0.0654(14) Uani 1 1 d . . . H37A H -0.1716 0.1917 -0.2161 0.098 Uiso 1 1 calc R . . H37B H -0.1980 0.1063 -0.1813 0.098 Uiso 1 1 calc R . . H37C H -0.0732 0.1256 -0.2072 0.098 Uiso 1 1 calc R . . C41 C 0.1591(9) 0.0893(6) 0.1448(4) 0.095(4) Uani 0.534(14) 1 d PGU A 1 H41A H 0.1107 0.0977 0.1057 0.114 Uiso 0.534(14) 1 calc PR A 1 C42 C 0.1159(7) 0.0954(6) 0.2114(5) 0.094(4) Uani 0.534(14) 1 d PGU A 1 H42A H 0.0382 0.1080 0.2172 0.113 Uiso 0.534(14) 1 calc PR A 1 C43 C 0.1875(8) 0.0829(7) 0.2693(4) 0.090(5) Uani 0.534(14) 1 d PGU A 1 H43A H 0.1583 0.0870 0.3143 0.108 Uiso 0.534(14) 1 calc PR A 1 C44 C 0.3024(8) 0.0643(7) 0.2606(4) 0.105(5) Uani 0.534(14) 1 d PGU A 1 H44A H 0.3509 0.0558 0.2998 0.126 Uiso 0.534(14) 1 calc PR A 1 C45 C 0.3456(7) 0.0581(6) 0.1940(5) 0.091(4) Uani 0.534(14) 1 d PGU A 1 H45A H 0.4233 0.0455 0.1882 0.109 Uiso 0.534(14) 1 calc PR A 1 C46 C 0.2740(9) 0.0706(5) 0.1361(3) 0.072(4) Uani 0.534(14) 1 d PGU A 1 H46A H 0.3032 0.0665 0.0911 0.086 Uiso 0.534(14) 1 calc PR A 1 C51 C 0.0724(9) 0.0731(8) 0.2226(5) 0.110(5) Uani 0.466(14) 1 d PGU A 2 H51A H -0.0024 0.0730 0.2395 0.132 Uiso 0.466(14) 1 calc PR A 2 C52 C 0.1657(11) 0.0682(9) 0.2688(4) 0.116(8) Uani 0.466(14) 1 d PGU A 2 H52A H 0.1540 0.0647 0.3169 0.139 Uiso 0.466(14) 1 calc PR A 2 C53 C 0.2764(9) 0.0683(9) 0.2438(5) 0.107(6) Uani 0.466(14) 1 d PGU A 2 H53A H 0.3395 0.0650 0.2750 0.129 Uiso 0.466(14) 1 calc PR A 2 C54 C 0.2937(9) 0.0734(8) 0.1726(6) 0.138(7) Uani 0.466(14) 1 d PGU A 2 H54A H 0.3685 0.0735 0.1556 0.166 Uiso 0.466(14) 1 calc PR A 2 C55 C 0.2004(11) 0.0783(7) 0.1264(4) 0.068(4) Uani 0.466(14) 1 d PGU A 2 H55A H 0.2122 0.0818 0.0782 0.082 Uiso 0.466(14) 1 calc PR A 2 C56 C 0.0898(9) 0.0782(6) 0.1514(5) 0.088(5) Uani 0.466(14) 1 d PGU A 2 H56A H 0.0267 0.0816 0.1202 0.106 Uiso 0.466(14) 1 calc PR A 2 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 0.0402(2) 0.0283(2) 0.0366(2) -0.00015(19) 0.00237(17) 0.00205(19) I1 0.1063(3) 0.03067(17) 0.0606(2) 0.00413(15) -0.00036(18) 0.00726(17) I2 0.04149(15) 0.04790(18) 0.06051(19) -0.00939(15) 0.00859(12) -0.00118(13) S1 0.0346(5) 0.0466(6) 0.0354(5) 0.0059(5) 0.0016(4) 0.0101(5) S2 0.0405(5) 0.0344(5) 0.0344(5) -0.0003(4) 0.0069(4) -0.0063(4) S3 0.0399(5) 0.0377(6) 0.0449(6) -0.0108(5) -0.0026(4) 0.0011(5) B 0.039(2) 0.028(2) 0.041(3) 0.000(2) 0.0006(19) 0.005(2) N11 0.0337(16) 0.0321(18) 0.0313(17) 0.0045(14) -0.0024(13) 0.0024(14) N12 0.0325(16) 0.0399(19) 0.0277(17) -0.0029(14) -0.0001(13) 0.0012(14) N21 0.0336(16) 0.0300(18) 0.0318(17) -0.0004(14) 0.0046(13) -0.0006(14) N22 0.0326(16) 0.0329(18) 0.0328(17) -0.0019(14) 0.0036(13) 0.0010(14) N31 0.0315(16) 0.0356(19) 0.0343(17) -0.0029(15) 0.0001(13) 0.0057(14) N32 0.0324(17) 0.049(2) 0.0377(19) -0.0044(16) 0.0010(14) 0.0030(15) C11 0.0292(19) 0.032(2) 0.033(2) 0.0020(17) 0.0017(15) -0.0017(16) C12 0.045(2) 0.041(2) 0.035(2) 0.0022(18) -0.0074(18) 0.0055(19) C13 0.042(2) 0.055(3) 0.029(2) 0.000(2) -0.0028(17) 0.005(2) C14 0.040(2) 0.054(3) 0.037(2) -0.013(2) 0.0019(17) 0.007(2) C15 0.038(2) 0.079(4) 0.058(3) -0.013(3) 0.009(2) 0.011(2) C16 0.073(3) 0.087(4) 0.040(3) -0.011(3) 0.009(2) 0.021(3) C17 0.065(3) 0.055(3) 0.077(4) -0.020(3) 0.009(3) 0.001(3) C21 0.0324(19) 0.028(2) 0.031(2) -0.0040(16) 0.0060(15) 0.0029(16) C22 0.042(2) 0.034(2) 0.039(2) 0.0023(18) 0.0064(17) -0.0055(18) C23 0.037(2) 0.036(2) 0.046(2) -0.0022(19) 0.0019(18) -0.0073(18) C24 0.037(2) 0.045(3) 0.037(2) -0.0006(19) -0.0036(17) 0.0027(18) C25 0.064(3) 0.071(3) 0.033(2) -0.002(2) 0.003(2) 0.019(3) C26 0.054(3) 0.050(3) 0.060(3) 0.002(2) -0.004(2) 0.012(2) C27 0.066(3) 0.063(3) 0.063(3) 0.003(3) -0.027(2) -0.004(3) C31 0.034(2) 0.040(2) 0.031(2) -0.0013(17) -0.0021(16) 0.0041(17) C32 0.048(2) 0.039(2) 0.037(2) -0.0040(19) 0.0020(18) 0.013(2) C33 0.039(2) 0.057(3) 0.039(2) -0.002(2) 0.0059(18) 0.012(2) C34 0.042(2) 0.072(3) 0.044(3) -0.001(2) 0.0060(19) -0.014(2) C35 0.043(3) 0.123(5) 0.087(4) -0.015(4) 0.025(3) -0.013(3) C36 0.078(3) 0.083(4) 0.056(3) 0.014(3) -0.001(3) -0.030(3) C37 0.048(3) 0.093(4) 0.054(3) -0.007(3) -0.007(2) -0.020(3) C41 0.095(5) 0.095(5) 0.095(5) 0.0009(10) 0.0021(10) 0.0000(10) C42 0.094(4) 0.093(4) 0.095(4) 0.0000(10) 0.0028(10) 0.0004(10) C43 0.091(5) 0.090(5) 0.090(5) 0.0000(10) 0.0031(10) 0.0002(10) C44 0.105(5) 0.105(5) 0.105(5) 0.0001(10) 0.0017(10) -0.0004(10) C45 0.091(4) 0.091(4) 0.091(4) 0.0003(10) 0.0026(10) -0.0006(10) C46 0.073(4) 0.072(4) 0.071(4) 0.0006(10) 0.0017(10) -0.0012(10) C51 0.111(5) 0.110(6) 0.110(5) 0.0002(10) 0.0033(10) 0.0007(10) C52 0.116(8) 0.116(8) 0.115(8) -0.0006(10) 0.0029(10) 0.0003(10) C53 0.107(6) 0.107(6) 0.107(6) 0.0000(10) 0.0021(10) -0.0002(10) C54 0.138(7) 0.138(7) 0.138(7) 0.0002(10) 0.0036(10) -0.0005(10) C55 0.069(4) 0.068(4) 0.068(4) 0.0008(10) 0.0030(10) 0.0003(10) C56 0.088(5) 0.088(5) 0.088(5) 0.0003(10) 0.0024(10) 0.0006(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 S2 2.2751(11) . ? Ga S1 2.2809(11) . ? Ga S3 2.2840(10) . ? Ga I1 2.5255(5) . ? S1 C11 1.742(4) . ? S2 C21 1.740(4) . ? S3 C31 1.746(4) . ? B H1 1.06(4) . ? B N11 1.549(5) . ? B N21 1.554(5) . ? B N31 1.556(5) . ? N11 C11 1.350(4) . ? N11 C12 1.379(4) . ? N12 C11 1.354(4) . ? N12 C13 1.381(5) . ? N12 C14 1.519(5) . ? N21 C21 1.340(4) . ? N21 C22 1.379(4) . ? N22 C21 1.359(4) . ? N22 C23 1.385(5) . ? N22 C24 1.511(5) . ? N31 C31 1.348(5) . ? N31 C32 1.385(5) . ? N32 C31 1.353(5) . ? N32 C33 1.382(5) . ? N32 C34 1.506(5) . ? C12 C13 1.339(5) . ? C14 C17 1.511(6) . ? C14 C15 1.516(5) . ? C14 C16 1.526(6) . ? C22 C23 1.335(5) . ? C24 C27 1.520(6) . ? C24 C26 1.519(6) . ? C24 C25 1.526(5) . ? C32 C33 1.336(6) . ? C34 C37 1.517(6) . ? C34 C36 1.531(6) . ? C34 C35 1.539(6) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? 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 108.94(4) . . ? S2 Ga S3 108.42(4) . . ? S1 Ga S3 107.53(4) . . ? S2 Ga I1 110.45(3) . . ? S1 Ga I1 109.75(3) . . ? S3 Ga I1 111.67(3) . . ? C11 S1 Ga 98.72(12) . . ? C21 S2 Ga 97.69(12) . . ? C31 S3 Ga 96.74(12) . . ? H1 B N11 107(2) . . ? H1 B N21 105(2) . . ? N11 B N21 111.8(3) . . ? H1 B N31 106.1(19) . . ? N11 B N31 113.7(3) . . ? N21 B N31 112.3(3) . . ? C11 N11 C12 107.2(3) . . ? C11 N11 B 133.9(3) . . ? C12 N11 B 118.9(3) . . ? C11 N12 C13 107.3(3) . . ? C11 N12 C14 128.4(3) . . ? C13 N12 C14 124.3(3) . . ? C21 N21 C22 107.5(3) . . ? C21 N21 B 133.6(3) . . ? C22 N21 B 118.9(3) . . ? C21 N22 C23 107.4(3) . . ? C21 N22 C24 128.3(3) . . ? C23 N22 C24 124.2(3) . . ? C31 N31 C32 107.3(3) . . ? C31 N31 B 134.0(3) . . ? C32 N31 B 118.7(3) . . ? C31 N32 C33 107.1(3) . . ? C31 N32 C34 128.3(3) . . ? C33 N32 C34 124.4(3) . . ? N11 C11 N12 109.1(3) . . ? N11 C11 S1 125.8(3) . . ? N12 C11 S1 125.2(3) . . ? C13 C12 N11 108.6(4) . . ? C12 C13 N12 107.9(3) . . ? C17 C14 C15 112.2(4) . . ? C17 C14 N12 108.3(3) . . ? C15 C14 N12 109.7(3) . . ? C17 C14 C16 109.6(4) . . ? C15 C14 C16 108.5(4) . . ? N12 C14 C16 108.4(3) . . ? N21 C21 N22 108.8(3) . . ? N21 C21 S2 125.7(3) . . ? N22 C21 S2 125.4(3) . . ? C23 C22 N21 108.8(3) . . ? C22 C23 N22 107.4(3) . . ? N22 C24 C27 108.5(3) . . ? N22 C24 C26 108.4(3) . . ? C27 C24 C26 109.6(3) . . ? N22 C24 C25 109.4(3) . . ? C27 C24 C25 108.9(4) . . ? C26 C24 C25 111.9(4) . . ? N31 C31 N32 109.2(3) . . ? N31 C31 S3 125.1(3) . . ? N32 C31 S3 125.7(3) . . ? C33 C32 N31 108.1(4) . . ? C32 C33 N32 108.4(3) . . ? N32 C34 C37 109.8(3) . . ? N32 C34 C36 108.0(3) . . ? C37 C34 C36 113.0(4) . . ? N32 C34 C35 107.9(4) . . ? C37 C34 C35 108.7(4) . . ? C36 C34 C35 109.3(4) . . ? C42 C41 C46 120.0 . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C52 C51 C56 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C51 120.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.789 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.082