# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Alan Welch' _publ_contact_author_email A.J.WELCH@HW.AC.UK _publ_section_title ; Adducts of the supraicosahedral stannacarborane 1,6-Me2-4,1,6-closo-SnC2B10H10; synthetic, structural and computational studies ; loop_ _publ_author_name 'Alan Welch' 'Peter D. Abram' 'David Ellis' 'Stuart A. Macgregor' 'David Mckay' 'Georgina Rosair' ; R.Sancho ; # Attachment 'Compound_1_revised.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 697455' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 B10 N2 Sn' _chemical_formula_weight 447.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.9073(8) _cell_length_b 16.9367(14) _cell_length_c 14.7949(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.924(4) _cell_angle_gamma 90.00 _cell_volume 1970.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 149 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 19.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 1.297 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7375 _exptl_absorpt_correction_T_max 0.8292 _exptl_absorpt_process_details TWINABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8404 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.30 _reflns_number_total 5927 _reflns_number_gt 4487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 (Bruker, 2006)' _computing_data_reduction 'APEX2 (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2003)' _computing_publication_material 'SHELXTL (Bruker, 2003)' _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. Twinned crystal, refined as two domains. Domain 2 rotated from first domain by 177.2 degrees about reciprocal axis 0.000 1.000 0.033 and real axis 0.010 1.000 0.045 Twin law to convert hkl from first to -0.994 0.000 0.026 this domain (SHELXL TWIN matrix): 0.024 0.997 0.089 -0.090 0.066 -1.001 ; _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^)+(0.0486P)^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 5928 _refine_ls_number_parameters 278 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _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 Sn4 Sn 1.07941(3) 0.177553(14) 0.776848(17) 0.01421(9) Uani 1 1 d . . . C1 C 0.8937(4) 0.2365(2) 0.6273(2) 0.0178(9) Uani 1 1 d . . . B2 B 0.8493(5) 0.3044(2) 0.6868(3) 0.0195(10) Uani 1 1 d D . . H2 H 0.908(4) 0.3670(13) 0.681(2) 0.023 Uiso 1 1 d D . . B3 B 0.8361(5) 0.1503(3) 0.6368(3) 0.0176(10) Uani 1 1 d D . . H3 H 0.876(4) 0.1109(16) 0.5849(18) 0.021 Uiso 1 1 d D . . B5 B 0.6696(5) 0.2296(3) 0.6090(3) 0.0200(10) Uani 1 1 d . . . H5 H 0.629(4) 0.2410(19) 0.539(3) 0.024 Uiso 1 1 d . . . C6 C 0.7667(5) 0.2939(2) 0.7844(2) 0.0178(8) Uani 1 1 d . . . B7 B 0.7915(6) 0.1197(3) 0.7518(3) 0.0188(10) Uani 1 1 d D . . H7 H 0.839(4) 0.0602(13) 0.772(2) 0.023 Uiso 1 1 d D . . B8 B 0.6283(5) 0.1318(3) 0.6635(3) 0.0192(10) Uani 1 1 d D . . H8 H 0.566(4) 0.0828(15) 0.626(2) 0.023 Uiso 1 1 d D . . B9 B 0.6156(5) 0.3046(2) 0.6974(3) 0.0176(10) Uani 1 1 d D . . H9 H 0.564(4) 0.3642(13) 0.680(2) 0.021 Uiso 1 1 d D . . B10 B 0.7758(5) 0.2026(2) 0.8270(3) 0.0173(10) Uani 1 1 d D . . H10 H 0.814(4) 0.1991(18) 0.9004(13) 0.021 Uiso 1 1 d D . . B11 B 0.5082(5) 0.2149(3) 0.6857(3) 0.0188(10) Uani 1 1 d D . . H11 H 0.377(3) 0.221(2) 0.656(2) 0.023 Uiso 1 1 d D . . B12 B 0.5789(6) 0.2535(3) 0.7955(3) 0.0208(10) Uani 1 1 d D . . H12 H 0.504(4) 0.2763(19) 0.8476(19) 0.025 Uiso 1 1 d D . . B13 B 0.5911(6) 0.1509(3) 0.7765(3) 0.0209(10) Uani 1 1 d D . . H13 H 0.508(4) 0.1111(17) 0.812(2) 0.025 Uiso 1 1 d D . . C11 C 0.9862(5) 0.2575(2) 0.5450(3) 0.0234(9) Uani 1 1 d . . . H11A H 0.9441 0.3083 0.5200 0.035 Uiso 1 1 calc R . . H11B H 0.9653 0.2164 0.4986 0.035 Uiso 1 1 calc R . . H11C H 1.1085 0.2614 0.5635 0.035 Uiso 1 1 calc R . . C61 C 0.8092(5) 0.3638(2) 0.8494(3) 0.0302(10) Uani 1 1 d . . . H61A H 0.9187 0.3542 0.8851 0.045 Uiso 1 1 calc R . . H61B H 0.7201 0.3691 0.8904 0.045 Uiso 1 1 calc R . . H61C H 0.8157 0.4124 0.8141 0.045 Uiso 1 1 calc R . . N41 N 1.1500(3) 0.07069(16) 0.87925(19) 0.0139(7) Uani 1 1 d . . . N42 N 1.1800(4) 0.06588(16) 0.7001(2) 0.0155(7) Uani 1 1 d . . . C40 C 1.1541(5) 0.0802(2) 0.9693(3) 0.0192(9) Uani 1 1 d . . . H40 H 1.1127 0.1281 0.9919 0.023 Uiso 1 1 calc R . . C41 C 1.2164(4) 0.0229(2) 1.0306(3) 0.0202(9) Uani 1 1 d . . . H41 H 1.2168 0.0309 1.0942 0.024 Uiso 1 1 calc R . . C42 C 1.2778(5) -0.0461(2) 0.9970(3) 0.0233(9) Uani 1 1 d . . . H42 H 1.3232 -0.0861 1.0376 0.028 Uiso 1 1 calc R . . C43 C 1.2733(5) -0.0569(2) 0.9052(3) 0.0205(9) Uani 1 1 d . . . H43 H 1.3136 -0.1047 0.8815 0.025 Uiso 1 1 calc R . . C44 C 1.2092(4) 0.0027(2) 0.8465(2) 0.0163(8) Uani 1 1 d . . . C45 C 1.2083(4) -0.0024(2) 0.7463(2) 0.0155(8) Uani 1 1 d . . . C46 C 1.2393(5) -0.0717(2) 0.7018(3) 0.0217(9) Uani 1 1 d . . . H46 H 1.2542 -0.1198 0.7347 0.026 Uiso 1 1 calc R . . C47 C 1.2486(5) -0.0708(2) 0.6092(3) 0.0228(9) Uani 1 1 d . . . H47 H 1.2681 -0.1183 0.5777 0.027 Uiso 1 1 calc R . . C48 C 1.2293(5) 0.0000(2) 0.5627(3) 0.0208(9) Uani 1 1 d . . . H48 H 1.2394 0.0026 0.4993 0.025 Uiso 1 1 calc R . . C49 C 1.1949(4) 0.0667(2) 0.6112(2) 0.0165(8) Uani 1 1 d . . . H49 H 1.1812 0.1156 0.5797 0.020 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 Sn4 0.01444(14) 0.01417(13) 0.01411(15) -0.00036(11) 0.00196(10) -0.00196(12) C1 0.0102(19) 0.029(2) 0.014(2) 0.0045(16) -0.0011(16) -0.0022(16) B2 0.016(2) 0.021(2) 0.021(3) 0.0080(19) 0.004(2) 0.0012(18) B3 0.011(2) 0.028(2) 0.015(2) -0.0059(19) 0.0060(18) 0.0069(18) B5 0.017(2) 0.028(3) 0.015(3) 0.0004(19) 0.003(2) 0.0019(19) C6 0.019(2) 0.0211(19) 0.013(2) -0.0012(16) 0.0022(17) -0.0014(16) B7 0.019(2) 0.020(2) 0.018(2) 0.0029(19) 0.0049(19) -0.0063(19) B8 0.014(2) 0.027(3) 0.016(2) 0.0002(19) 0.0027(19) -0.0019(19) B9 0.016(2) 0.017(2) 0.020(3) -0.0011(18) 0.0055(19) 0.0027(17) B10 0.019(2) 0.023(2) 0.010(2) 0.0032(18) 0.0042(19) -0.0017(17) B11 0.012(2) 0.026(2) 0.019(3) 0.002(2) 0.0039(19) -0.0009(19) B12 0.019(2) 0.030(3) 0.014(3) 0.0011(19) 0.003(2) -0.0027(19) B13 0.016(2) 0.025(2) 0.021(3) 0.008(2) -0.0003(19) -0.0020(19) C11 0.026(2) 0.024(2) 0.020(2) 0.0028(17) 0.0035(18) -0.0035(17) C61 0.032(3) 0.028(2) 0.030(3) -0.0036(19) 0.003(2) -0.0005(19) N41 0.0117(16) 0.0173(16) 0.0124(17) 0.0001(13) -0.0001(13) -0.0033(12) N42 0.0127(16) 0.0170(16) 0.0167(18) 0.0006(13) 0.0006(13) -0.0040(12) C40 0.017(2) 0.023(2) 0.018(2) -0.0004(17) 0.0024(17) -0.0032(16) C41 0.020(2) 0.026(2) 0.016(2) 0.0047(17) 0.0019(17) -0.0065(17) C42 0.023(2) 0.025(2) 0.021(2) 0.0053(17) -0.0018(18) -0.0024(17) C43 0.022(2) 0.0146(19) 0.025(2) -0.0008(16) 0.0011(18) 0.0004(16) C44 0.018(2) 0.0134(18) 0.017(2) -0.0002(15) -0.0007(16) -0.0038(15) C45 0.015(2) 0.0146(19) 0.017(2) -0.0031(16) 0.0005(16) -0.0022(15) C46 0.022(2) 0.0183(19) 0.025(2) 0.0005(17) 0.0019(18) 0.0025(16) C47 0.023(2) 0.025(2) 0.020(2) -0.0094(18) 0.0007(18) -0.0003(17) C48 0.016(2) 0.028(2) 0.018(2) -0.0052(17) 0.0012(17) -0.0024(16) C49 0.014(2) 0.021(2) 0.015(2) 0.0006(16) 0.0006(16) -0.0024(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn4 N42 2.384(3) . ? Sn4 N41 2.389(3) . ? Sn4 B7 2.471(4) . ? Sn4 B10 2.620(4) . ? Sn4 C1 2.717(3) . ? Sn4 B3 2.717(4) . ? Sn4 B2 3.033(4) . ? Sn4 C6 3.173(4) . ? C1 B2 1.512(6) . ? C1 C11 1.526(5) . ? C1 B3 1.541(6) . ? C1 B5 1.769(6) . ? B2 C6 1.654(6) . ? B2 B9 1.871(6) . ? B2 H2 1.165(18) . ? B3 B8 1.757(6) . ? B3 B7 1.847(6) . ? B3 B5 1.896(6) . ? B3 H3 1.088(18) . ? B5 B11 1.810(6) . ? B5 B8 1.885(6) . ? B5 B9 1.904(6) . ? B5 H5 1.07(4) . ? C6 C61 1.540(5) . ? C6 B12 1.659(6) . ? C6 B10 1.669(5) . ? C6 B9 1.672(5) . ? B7 B13 1.744(6) . ? B7 B8 1.751(6) . ? B7 B10 1.804(6) . ? B7 H7 1.107(18) . ? B8 B11 1.748(6) . ? B8 B13 1.757(6) . ? B8 H8 1.089(18) . ? B9 B12 1.739(6) . ? B9 B11 1.740(6) . ? B9 H9 1.108(18) . ? B10 B13 1.799(6) . ? B10 B12 1.799(6) . ? B10 H10 1.099(18) . ? B11 B12 1.786(6) . ? B11 B13 1.796(6) . ? B11 H11 1.090(18) . ? B12 B13 1.764(7) . ? B12 H12 1.092(18) . ? B13 H13 1.111(18) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? N41 C40 1.338(5) . ? N41 C44 1.351(4) . ? N42 C49 1.333(4) . ? N42 C45 1.350(4) . ? C40 C41 1.384(5) . ? C40 H40 0.9500 . ? C41 C42 1.378(5) . ? C41 H41 0.9500 . ? C42 C43 1.368(5) . ? C42 H42 0.9500 . ? C43 C44 1.392(5) . ? C43 H43 0.9500 . ? C44 C45 1.485(5) . ? C45 C46 1.380(5) . ? C46 C47 1.379(5) . ? C46 H46 0.9500 . ? C47 C48 1.383(5) . ? C47 H47 0.9500 . ? C48 C49 1.381(5) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? 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 N42 Sn4 N41 68.51(10) . . ? N42 Sn4 B7 87.81(12) . . ? N41 Sn4 B7 86.90(12) . . ? N42 Sn4 B10 128.62(11) . . ? N41 Sn4 B10 95.97(11) . . ? B7 Sn4 B10 41.37(14) . . ? N42 Sn4 C1 94.73(11) . . ? N41 Sn4 C1 150.03(10) . . ? B7 Sn4 C1 67.13(12) . . ? B10 Sn4 C1 74.75(12) . . ? N42 Sn4 B3 75.34(11) . . ? N41 Sn4 B3 117.09(11) . . ? B7 Sn4 B3 41.37(14) . . ? B10 Sn4 B3 69.27(13) . . ? C1 Sn4 B3 32.94(12) . . ? N42 Sn4 B2 124.55(11) . . ? N41 Sn4 B2 154.86(11) . . ? B7 Sn4 B2 73.33(13) . . ? B10 Sn4 B2 58.92(12) . . ? C1 Sn4 B2 29.83(11) . . ? B3 Sn4 B2 55.95(12) . . ? N42 Sn4 C6 143.97(9) . . ? N41 Sn4 C6 125.46(10) . . ? B7 Sn4 C6 62.74(12) . . ? B10 Sn4 C6 31.68(11) . . ? C1 Sn4 C6 56.11(10) . . ? B3 Sn4 C6 68.85(11) . . ? B2 Sn4 C6 30.80(11) . . ? B2 C1 C11 116.6(3) . . ? B2 C1 B3 125.4(3) . . ? C11 C1 B3 117.7(3) . . ? B2 C1 B5 81.4(3) . . ? C11 C1 B5 116.7(3) . . ? B3 C1 B5 69.5(2) . . ? B2 C1 Sn4 86.8(2) . . ? C11 C1 Sn4 118.2(2) . . ? B3 C1 Sn4 73.5(2) . . ? B5 C1 Sn4 123.3(2) . . ? C1 B2 C6 124.3(3) . . ? C1 B2 B9 110.0(3) . . ? C6 B2 B9 56.2(2) . . ? C1 B2 Sn4 63.40(19) . . ? C6 B2 Sn4 79.3(2) . . ? B9 B2 Sn4 121.2(2) . . ? C1 B2 H2 121.9(18) . . ? C6 B2 H2 111.2(18) . . ? B9 B2 H2 114.3(17) . . ? Sn4 B2 H2 116.8(17) . . ? C1 B3 B8 118.8(3) . . ? C1 B3 B7 115.9(3) . . ? B8 B3 B7 58.1(2) . . ? C1 B3 B5 60.9(2) . . ? B8 B3 B5 62.0(2) . . ? B7 B3 B5 101.8(3) . . ? C1 B3 Sn4 73.5(2) . . ? B8 B3 Sn4 117.6(2) . . ? B7 B3 Sn4 62.16(18) . . ? B5 B3 Sn4 117.8(2) . . ? C1 B3 H3 114.0(18) . . ? B8 B3 H3 113.2(18) . . ? B7 B3 H3 125.2(18) . . ? B5 B3 H3 121.7(18) . . ? Sn4 B3 H3 114.2(18) . . ? C1 B5 B11 132.3(3) . . ? C1 B5 B8 102.0(3) . . ? B11 B5 B8 56.4(2) . . ? C1 B5 B3 49.6(2) . . ? B11 B5 B3 106.6(3) . . ? B8 B5 B3 55.4(2) . . ? C1 B5 B9 98.2(3) . . ? B11 B5 B9 55.8(2) . . ? B8 B5 B9 103.4(3) . . ? B3 B5 B9 121.6(3) . . ? C1 B5 H5 109.3(19) . . ? B11 B5 H5 118.2(19) . . ? B8 B5 H5 121.7(18) . . ? B3 B5 H5 118.0(19) . . ? B9 B5 H5 118.6(19) . . ? C61 C6 B2 112.5(3) . . ? C61 C6 B12 113.2(3) . . ? B2 C6 B12 124.7(3) . . ? C61 C6 B10 118.5(3) . . ? B2 C6 B10 115.1(3) . . ? B12 C6 B10 65.5(3) . . ? C61 C6 B9 119.3(3) . . ? B2 C6 B9 68.4(3) . . ? B12 C6 B9 62.9(2) . . ? B10 C6 B9 113.0(3) . . ? C61 C6 Sn4 112.2(2) . . ? B2 C6 Sn4 69.93(19) . . ? B12 C6 Sn4 117.1(2) . . ? B10 C6 Sn4 55.55(18) . . ? B9 C6 Sn4 122.6(2) . . ? B13 B7 B8 60.3(3) . . ? B13 B7 B10 60.9(2) . . ? B8 B7 B10 106.1(3) . . ? B13 B7 B3 111.8(3) . . ? B8 B7 B3 58.4(2) . . ? B10 B7 B3 112.4(3) . . ? B13 B7 Sn4 133.8(3) . . ? B8 B7 Sn4 131.4(3) . . ? B10 B7 Sn4 73.7(2) . . ? B3 B7 Sn4 76.5(2) . . ? B13 B7 H7 120.8(19) . . ? B8 B7 H7 120.8(18) . . ? B10 B7 H7 126.0(18) . . ? B3 B7 H7 114.2(19) . . ? Sn4 B7 H7 92.1(18) . . ? B11 B8 B7 109.1(3) . . ? B11 B8 B13 61.7(2) . . ? B7 B8 B13 59.6(3) . . ? B11 B8 B3 116.0(3) . . ? B7 B8 B3 63.5(2) . . ? B13 B8 B3 115.7(3) . . ? B11 B8 B5 59.6(2) . . ? B7 B8 B5 106.0(3) . . ? B13 B8 B5 107.4(3) . . ? B3 B8 B5 62.6(2) . . ? B11 B8 H8 118.9(18) . . ? B7 B8 H8 123.6(18) . . ? B13 B8 H8 121.0(19) . . ? B3 B8 H8 114.0(19) . . ? B5 B8 H8 122.7(18) . . ? C6 B9 B12 58.1(2) . . ? C6 B9 B11 106.5(3) . . ? B12 B9 B11 61.8(3) . . ? C6 B9 B2 55.3(2) . . ? B12 B9 B2 108.7(3) . . ? B11 B9 B2 117.8(3) . . ? C6 B9 B5 105.2(3) . . ? B12 B9 B5 108.0(3) . . ? B11 B9 B5 59.4(2) . . ? B2 B9 B5 69.3(2) . . ? C6 B9 H9 119.5(18) . . ? B12 B9 H9 123.6(18) . . ? B11 B9 H9 127.3(18) . . ? B2 B9 H9 109.2(18) . . ? B5 B9 H9 123.7(18) . . ? C6 B10 B13 107.0(3) . . ? C6 B10 B12 57.0(2) . . ? B13 B10 B12 58.7(2) . . ? C6 B10 B7 119.4(3) . . ? B13 B10 B7 57.9(2) . . ? B12 B10 B7 109.0(3) . . ? C6 B10 Sn4 92.8(2) . . ? B13 B10 Sn4 122.1(3) . . ? B12 B10 Sn4 143.0(3) . . ? B7 B10 Sn4 64.90(19) . . ? C6 B10 H10 115.0(17) . . ? B13 B10 H10 120.9(18) . . ? B12 B10 H10 115.2(18) . . ? B7 B10 H10 122.5(17) . . ? Sn4 B10 H10 96.0(19) . . ? B9 B11 B8 116.9(3) . . ? B9 B11 B12 59.1(3) . . ? B8 B11 B12 109.9(3) . . ? B9 B11 B13 108.4(3) . . ? B8 B11 B13 59.4(2) . . ? B12 B11 B13 59.0(3) . . ? B9 B11 B5 64.8(3) . . ? B8 B11 B5 63.9(3) . . ? B12 B11 B5 110.2(3) . . ? B13 B11 B5 109.0(3) . . ? B9 B11 H11 113.2(18) . . ? B8 B11 H11 120.7(18) . . ? B12 B11 H11 122.2(19) . . ? B13 B11 H11 128.3(19) . . ? B5 B11 H11 115.7(19) . . ? C6 B12 B9 58.9(2) . . ? C6 B12 B13 109.0(3) . . ? B9 B12 B13 109.9(3) . . ? C6 B12 B11 105.1(3) . . ? B9 B12 B11 59.2(2) . . ? B13 B12 B11 60.8(2) . . ? C6 B12 B10 57.5(2) . . ? B9 B12 B10 103.9(3) . . ? B13 B12 B10 60.6(2) . . ? B11 B12 B10 104.0(3) . . ? C6 B12 H12 118.9(19) . . ? B9 B12 H12 124.3(19) . . ? B13 B12 H12 120.2(19) . . ? B11 B12 H12 129.0(19) . . ? B10 B12 H12 120.4(19) . . ? B7 B13 B8 60.0(3) . . ? B7 B13 B12 113.4(3) . . ? B8 B13 B12 110.5(3) . . ? B7 B13 B11 107.2(3) . . ? B8 B13 B11 58.9(3) . . ? B12 B13 B11 60.2(2) . . ? B7 B13 B10 61.2(2) . . ? B8 B13 B10 106.1(3) . . ? B12 B13 B10 60.6(2) . . ? B11 B13 B10 103.6(3) . . ? B7 B13 H13 120.5(18) . . ? B8 B13 H13 120.2(19) . . ? B12 B13 H13 118.6(19) . . ? B11 B13 H13 122.2(18) . . ? B10 B13 H13 126.4(18) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C61 H61A 109.5 . . ? C6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C40 N41 C44 119.0(3) . . ? C40 N41 Sn4 121.4(2) . . ? C44 N41 Sn4 119.0(2) . . ? C49 N42 C45 118.8(3) . . ? C49 N42 Sn4 122.0(2) . . ? C45 N42 Sn4 118.9(2) . . ? N41 C40 C41 122.6(4) . . ? N41 C40 H40 118.7 . . ? C41 C40 H40 118.7 . . ? C42 C41 C40 118.2(4) . . ? C42 C41 H41 120.9 . . ? C40 C41 H41 120.9 . . ? C43 C42 C41 119.8(4) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 119.5(3) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? N41 C44 C43 120.8(3) . . ? N41 C44 C45 116.2(3) . . ? C43 C44 C45 122.9(3) . . ? N42 C45 C46 121.0(3) . . ? N42 C45 C44 116.1(3) . . ? C46 C45 C44 122.9(3) . . ? C47 C46 C45 119.7(4) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C48 119.4(4) . . ? C46 C47 H47 120.3 . . ? C48 C47 H47 120.3 . . ? C49 C48 C47 117.9(4) . . ? C49 C48 H48 121.1 . . ? C47 C48 H48 121.1 . . ? N42 C49 C48 123.1(3) . . ? N42 C49 H49 118.4 . . ? C48 C49 H49 118.4 . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.680 _refine_diff_density_min -1.175 _refine_diff_density_rms 0.115 # Attachment 'Compound_2.cif' data_x81634 _database_code_depnum_ccdc_archive 'CCDC 697456' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H24 B10 N2 Sn, C4 H8 O' _chemical_formula_sum 'C20 H32 B10 N2 O Sn' _chemical_formula_weight 543.27 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' Sn Sn -0.6537 1.4246 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.7876(14) _cell_length_b 19.350(3) _cell_length_c 16.543(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.301(7) _cell_angle_gamma 90.00 _cell_volume 2485.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1258 _cell_measurement_theta_min 3.36 _cell_measurement_theta_max 30.18 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.046 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 0.828 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67045 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 30.62 _reflns_number_total 7628 _reflns_number_gt 6075 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+3.2194P] 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 7628 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Sn4 Sn 0.30994(2) 0.273910(8) 0.389929(10) 0.01286(5) Uani 1 1 d . . . C1 C 0.5589(3) 0.24792(16) 0.28668(16) 0.0221(5) Uani 1 1 d . . . B2 B 0.5253(4) 0.17212(18) 0.3022(2) 0.0264(7) Uani 1 1 d . . . H2 H 0.467(4) 0.1394(17) 0.251(2) 0.032 Uiso 1 1 d . . . B3 B 0.6421(4) 0.29764(17) 0.35098(18) 0.0185(5) Uani 1 1 d . . . H3 H 0.672(4) 0.3484(16) 0.3303(18) 0.022 Uiso 1 1 d . . . B5 B 0.7661(4) 0.21552(19) 0.3224(2) 0.0277(7) Uani 1 1 d . . . H5 H 0.850(5) 0.2212(17) 0.273(2) 0.033 Uiso 1 1 d . . . C6 C 0.5117(4) 0.13792(14) 0.39271(18) 0.0247(6) Uani 1 1 d . . . B7 B 0.6027(4) 0.27766(14) 0.45741(16) 0.0149(5) Uani 1 1 d . . . H7 H 0.580(4) 0.3222(15) 0.4998(17) 0.018 Uiso 1 1 d . . . B8 B 0.8051(4) 0.26538(16) 0.42066(19) 0.0197(6) Uani 1 1 d . . . H8 H 0.903(4) 0.3037(17) 0.4328(19) 0.024 Uiso 1 1 d . . . B9 B 0.7066(4) 0.12697(19) 0.3567(2) 0.0320(8) Uani 1 1 d . . . H9 H 0.735(5) 0.0790(18) 0.328(2) 0.038 Uiso 1 1 d . . . B10 B 0.5157(4) 0.19282(15) 0.47058(18) 0.0191(6) Uani 1 1 d . . . H10 H 0.430(4) 0.1849(16) 0.5198(19) 0.023 Uiso 1 1 d . . . B11 B 0.8498(4) 0.17634(18) 0.4170(2) 0.0265(7) Uani 1 1 d . . . H11 H 0.983(4) 0.1610(17) 0.423(2) 0.032 Uiso 1 1 d . . . B12 B 0.6817(4) 0.12935(17) 0.4599(2) 0.0272(7) Uani 1 1 d . . . H12 H 0.678(4) 0.0836(18) 0.496(2) 0.033 Uiso 1 1 d . . . B13 B 0.7371(4) 0.21213(15) 0.49883(18) 0.0185(6) Uani 1 1 d . . . H13 H 0.802(4) 0.2157(15) 0.5589(19) 0.022 Uiso 1 1 d . . . C11 C 0.5322(4) 0.27378(19) 0.19980(17) 0.0327(7) Uani 1 1 d . . . H11A H 0.5504 0.2357 0.1624 0.049 Uiso 1 1 calc R . . H11B H 0.6145 0.3109 0.1912 0.049 Uiso 1 1 calc R . . H11C H 0.4146 0.2914 0.1898 0.049 Uiso 1 1 calc R . . C61 C 0.3860(4) 0.07756(16) 0.3909(2) 0.0398(8) Uani 1 1 d . . . H61A H 0.2691 0.0944 0.3765 0.060 Uiso 1 1 calc R . . H61B H 0.3905 0.0558 0.4445 0.060 Uiso 1 1 calc R . . H61C H 0.4176 0.0436 0.3506 0.060 Uiso 1 1 calc R . . N41 N 0.2221(2) 0.31991(11) 0.51680(12) 0.0141(4) Uani 1 1 d . . . N42 N 0.3231(3) 0.39768(11) 0.39246(12) 0.0162(4) Uani 1 1 d . . . C40 C 0.1666(3) 0.28121(13) 0.57587(16) 0.0175(5) Uani 1 1 d . . . H40 H 0.1660 0.2324 0.5696 0.021 Uiso 1 1 calc R . . C41 C 0.1093(3) 0.30916(15) 0.64674(16) 0.0233(6) Uani 1 1 d . . . H41 H 0.0721 0.2797 0.6879 0.028 Uiso 1 1 calc R . . C42 C 0.1070(4) 0.37940(16) 0.65638(16) 0.0245(6) Uani 1 1 d . . . H42 H 0.0679 0.3991 0.7043 0.029 Uiso 1 1 calc R . . C43 C 0.1630(3) 0.42241(14) 0.59485(15) 0.0196(5) Uani 1 1 d . . . C44 C 0.1641(4) 0.49683(15) 0.59868(16) 0.0243(6) Uani 1 1 d . . . H44 H 0.1269 0.5191 0.6454 0.029 Uiso 1 1 calc R . . C45 C 0.2167(4) 0.53542(14) 0.53746(17) 0.0237(6) Uani 1 1 d . . . H45 H 0.2162 0.5844 0.5419 0.028 Uiso 1 1 calc R . . C46 C 0.2734(3) 0.50398(13) 0.46591(16) 0.0189(5) Uani 1 1 d . . . C47 C 0.3260(3) 0.54207(14) 0.39922(17) 0.0228(5) Uani 1 1 d . . . H47 H 0.3273 0.5911 0.4008 0.027 Uiso 1 1 calc R . . C48 C 0.3751(4) 0.50785(14) 0.33213(17) 0.0242(6) Uani 1 1 d . . . H48 H 0.4115 0.5330 0.2871 0.029 Uiso 1 1 calc R . . C49 C 0.3712(3) 0.43527(14) 0.33065(16) 0.0204(5) Uani 1 1 d . . . H49 H 0.4042 0.4121 0.2836 0.024 Uiso 1 1 calc R . . C50 C 0.2747(3) 0.43108(12) 0.45973(15) 0.0147(4) Uani 1 1 d . . . C51 C 0.2195(3) 0.39000(12) 0.52549(14) 0.0145(4) Uani 1 1 d . . . C1S C 0.7966(12) 0.9228(3) 0.3792(5) 0.0387(19) Uani 0.539(9) 1 d P A 1 H1S1 H 0.7549 0.9023 0.4290 0.046 Uiso 0.539(9) 1 calc PR A 1 H1S2 H 0.7085 0.9556 0.3562 0.046 Uiso 0.539(9) 1 calc PR A 1 C3S C 0.9942(18) 0.8828(6) 0.2918(9) 0.031(3) Uani 0.539(9) 1 d P A 1 H3S1 H 0.9864 0.8802 0.2318 0.038 Uiso 0.539(9) 1 calc PR A 1 H3S2 H 1.0784 0.8480 0.3136 0.038 Uiso 0.539(9) 1 calc PR A 1 C4S C 1.0477(9) 0.9528(3) 0.3190(5) 0.0359(18) Uani 0.539(9) 1 d P A 1 H4S1 H 1.0043 0.9884 0.2797 0.043 Uiso 0.539(9) 1 calc PR A 1 H4S2 H 1.1747 0.9564 0.3271 0.043 Uiso 0.539(9) 1 calc PR A 1 C5S C 0.9644(9) 0.9600(4) 0.3992(4) 0.0330(17) Uani 0.539(9) 1 d P A 1 H5S1 H 1.0339 0.9372 0.4441 0.040 Uiso 0.539(9) 1 calc PR A 1 H5S2 H 0.9458 1.0090 0.4131 0.040 Uiso 0.539(9) 1 calc PR A 1 C1T C 0.8856(12) 0.9184(4) 0.3835(5) 0.0291(18) Uani 0.461(9) 1 d P A 2 H1T1 H 0.9186 0.8980 0.4374 0.035 Uiso 0.461(9) 1 calc PR A 2 H1T2 H 0.7726 0.9415 0.3856 0.035 Uiso 0.461(9) 1 calc PR A 2 C2T C 1.0265(17) 0.8680(6) 0.2785(9) 0.023(2) Uani 0.461(9) 1 d P A 2 H2T1 H 0.9971 0.8819 0.2215 0.028 Uiso 0.461(9) 1 calc PR A 2 H2T2 H 1.0831 0.8222 0.2787 0.028 Uiso 0.461(9) 1 calc PR A 2 C3T C 1.1483(8) 0.9221(3) 0.3217(4) 0.0217(16) Uani 0.461(9) 1 d P A 2 H3T1 H 1.2284 0.9002 0.3634 0.026 Uiso 0.461(9) 1 calc PR A 2 H3T2 H 1.2153 0.9473 0.2826 0.026 Uiso 0.461(9) 1 calc PR A 2 C4T C 1.0215(10) 0.9695(4) 0.3598(6) 0.0273(17) Uani 0.461(9) 1 d P A 2 H4T1 H 0.9722 1.0040 0.3204 0.033 Uiso 0.461(9) 1 calc PR A 2 H4T2 H 1.0760 0.9937 0.4078 0.033 Uiso 0.461(9) 1 calc PR A 2 O1S O 0.8253(10) 0.8704(6) 0.3224(8) 0.0335(18) Uani 0.539(9) 1 d P A 1 O1T O 0.8774(10) 0.8651(7) 0.3209(8) 0.0241(17) Uani 0.461(9) 1 d P 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 Sn4 0.01081(8) 0.01332(8) 0.01438(8) -0.00116(6) 0.00046(5) -0.00003(6) C1 0.0132(11) 0.0352(14) 0.0178(12) -0.0075(11) 0.0007(9) 0.0067(10) B2 0.0170(13) 0.0341(18) 0.0271(15) -0.0162(14) -0.0040(12) 0.0085(13) B3 0.0123(12) 0.0267(15) 0.0168(13) -0.0010(11) 0.0038(10) 0.0009(11) B5 0.0157(14) 0.044(2) 0.0239(15) -0.0113(14) 0.0020(12) 0.0077(13) C6 0.0204(13) 0.0165(12) 0.0354(15) -0.0067(11) -0.0091(11) 0.0036(10) B7 0.0153(12) 0.0148(12) 0.0147(11) -0.0025(10) 0.0016(9) -0.0008(10) B8 0.0133(12) 0.0251(16) 0.0203(13) -0.0043(11) -0.0014(10) 0.0030(11) B9 0.0239(16) 0.0301(18) 0.0396(19) -0.0200(15) -0.0140(14) 0.0137(14) B10 0.0177(13) 0.0162(14) 0.0230(14) -0.0007(11) -0.0017(11) 0.0015(10) B11 0.0217(15) 0.0304(17) 0.0265(15) -0.0091(14) -0.0040(12) 0.0110(13) B12 0.0238(15) 0.0179(15) 0.0378(18) -0.0023(13) -0.0106(13) 0.0052(12) B13 0.0157(13) 0.0200(14) 0.0192(13) -0.0008(10) -0.0024(10) 0.0013(10) C11 0.0226(14) 0.059(2) 0.0166(12) -0.0035(13) 0.0020(10) 0.0001(14) C61 0.0350(17) 0.0187(15) 0.063(2) -0.0081(15) -0.0127(16) -0.0022(13) N41 0.0110(9) 0.0162(9) 0.0151(9) 0.0005(8) 0.0006(7) -0.0005(8) N42 0.0161(10) 0.0156(10) 0.0168(9) 0.0014(8) 0.0017(8) 0.0027(8) C40 0.0134(11) 0.0179(12) 0.0214(12) 0.0028(10) 0.0027(9) -0.0006(9) C41 0.0202(13) 0.0318(15) 0.0187(12) 0.0042(11) 0.0065(10) -0.0018(11) C42 0.0227(13) 0.0334(15) 0.0175(12) -0.0058(11) 0.0030(10) 0.0007(11) C43 0.0165(12) 0.0229(13) 0.0189(12) -0.0061(10) -0.0012(9) -0.0004(10) C44 0.0267(14) 0.0226(13) 0.0233(13) -0.0121(10) 0.0008(11) 0.0004(11) C45 0.0240(13) 0.0159(12) 0.0303(14) -0.0075(10) -0.0036(11) -0.0003(10) C46 0.0158(11) 0.0159(12) 0.0243(12) -0.0012(10) -0.0036(10) -0.0002(9) C47 0.0219(13) 0.0142(12) 0.0311(15) 0.0030(10) -0.0054(11) -0.0006(10) C48 0.0281(14) 0.0196(13) 0.0246(13) 0.0097(10) 0.0006(11) -0.0033(11) C49 0.0236(13) 0.0203(13) 0.0177(12) 0.0050(10) 0.0047(10) -0.0007(10) C50 0.0109(10) 0.0140(11) 0.0191(11) -0.0002(9) -0.0007(9) 0.0001(8) C51 0.0109(10) 0.0166(11) 0.0154(11) -0.0018(9) -0.0014(8) -0.0003(9) C1S 0.037(4) 0.024(3) 0.058(5) 0.009(3) 0.028(4) 0.002(3) C3S 0.040(6) 0.020(5) 0.033(6) -0.004(3) -0.004(4) 0.009(4) C4S 0.031(4) 0.028(4) 0.050(4) -0.008(3) 0.013(3) -0.010(3) C5S 0.030(3) 0.041(4) 0.026(3) -0.003(3) -0.005(3) 0.013(3) C1T 0.023(4) 0.033(4) 0.033(4) 0.006(3) 0.012(3) -0.001(4) C2T 0.026(5) 0.015(5) 0.027(5) -0.003(4) -0.001(4) -0.013(4) C3T 0.022(3) 0.022(3) 0.021(3) 0.003(2) 0.002(2) 0.002(2) C4T 0.027(4) 0.021(3) 0.034(5) 0.001(3) 0.005(3) 0.004(3) O1S 0.020(4) 0.024(3) 0.057(4) 0.008(2) 0.009(4) 0.000(4) O1T 0.010(4) 0.032(4) 0.032(3) -0.002(2) 0.006(4) -0.003(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 Sn4 N42 2.397(2) . ? Sn4 N41 2.425(2) . ? Sn4 B7 2.463(3) . ? Sn4 B10 2.547(3) . ? Sn4 C1 2.725(3) . ? Sn4 B3 2.750(3) . ? Sn4 B2 3.027(3) . ? Sn4 C6 3.064(3) . ? C1 B2 1.515(5) . ? C1 C11 1.521(4) . ? C1 B3 1.540(4) . ? C1 B5 1.790(4) . ? B2 C6 1.647(5) . ? B2 B9 1.838(5) . ? B2 B5 2.059(5) . ? B2 H2 1.13(3) . ? B3 B8 1.764(4) . ? B3 B7 1.851(4) . ? B3 B5 1.936(5) . ? B3 H3 1.07(3) . ? B5 B11 1.815(5) . ? B5 B9 1.874(6) . ? B5 B8 1.895(4) . ? B5 H5 1.09(4) . ? C6 C61 1.523(4) . ? C6 B10 1.668(4) . ? C6 B12 1.672(4) . ? C6 B9 1.684(5) . ? B7 B8 1.748(4) . ? B7 B13 1.751(4) . ? B7 B10 1.796(4) . ? B7 H7 1.13(3) . ? B8 B11 1.760(5) . ? B8 B13 1.766(4) . ? B8 H8 1.07(3) . ? B9 B11 1.728(5) . ? B9 B12 1.733(5) . ? B9 H9 1.07(4) . ? B10 B13 1.792(4) . ? B10 B12 1.801(4) . ? B10 H10 1.10(3) . ? B11 B12 1.784(5) . ? B11 B13 1.806(4) . ? B11 H11 1.07(3) . ? B12 B13 1.768(4) . ? B12 H12 1.06(3) . ? B13 H13 1.08(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? N41 C40 1.329(3) . ? N41 C51 1.364(3) . ? N42 C49 1.331(3) . ? N42 C50 1.364(3) . ? C40 C41 1.395(4) . ? C40 H40 0.9500 . ? C41 C42 1.369(4) . ? C41 H41 0.9500 . ? C42 C43 1.409(4) . ? C42 H42 0.9500 . ? C43 C51 1.407(3) . ? C43 C44 1.441(4) . ? C44 C45 1.347(4) . ? C44 H44 0.9500 . ? C45 C46 1.430(4) . ? C45 H45 0.9500 . ? C46 C47 1.413(4) . ? C46 C50 1.414(3) . ? C47 C48 1.371(4) . ? C47 H47 0.9500 . ? C48 C49 1.405(4) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 C51 1.439(3) . ? C1S O1S 1.411(14) . ? C1S C5S 1.506(10) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C3S O1S 1.465(14) . ? C3S C4S 1.477(14) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S C5S 1.525(10) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? C1T O1T 1.460(15) . ? C1T C4T 1.521(10) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T O1T 1.402(14) . ? C2T C3T 1.550(14) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.518(10) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? 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 N42 Sn4 N41 68.45(7) . . ? N42 Sn4 B7 85.74(8) . . ? N41 Sn4 B7 84.75(8) . . ? N42 Sn4 B10 125.58(8) . . ? N41 Sn4 B10 88.85(8) . . ? B7 Sn4 B10 41.96(10) . . ? N42 Sn4 C1 99.43(8) . . ? N41 Sn4 C1 150.50(7) . . ? B7 Sn4 C1 67.15(8) . . ? B10 Sn4 C1 76.44(9) . . ? N42 Sn4 B3 78.32(8) . . ? N41 Sn4 B3 118.21(8) . . ? B7 Sn4 B3 41.12(9) . . ? B10 Sn4 B3 70.12(10) . . ? C1 Sn4 B3 32.68(9) . . ? N42 Sn4 B2 129.34(9) . . ? N41 Sn4 B2 148.88(8) . . ? B7 Sn4 B2 73.09(9) . . ? B10 Sn4 B2 60.06(9) . . ? C1 Sn4 B2 29.96(10) . . ? B3 Sn4 B2 55.37(9) . . ? N42 Sn4 C6 146.78(7) . . ? N41 Sn4 C6 118.68(7) . . ? B7 Sn4 C6 64.04(8) . . ? B10 Sn4 C6 32.99(9) . . ? C1 Sn4 C6 57.50(9) . . ? B3 Sn4 C6 69.91(9) . . ? B2 Sn4 C6 31.37(9) . . ? B2 C1 C11 117.8(3) . . ? B2 C1 B3 123.8(2) . . ? C11 C1 B3 117.9(3) . . ? B2 C1 B5 76.6(2) . . ? C11 C1 B5 118.9(2) . . ? B3 C1 B5 70.64(19) . . ? B2 C1 Sn4 86.13(17) . . ? C11 C1 Sn4 118.58(18) . . ? B3 C1 Sn4 74.58(14) . . ? B5 C1 Sn4 121.57(17) . . ? C1 B2 C6 124.5(2) . . ? C1 B2 B9 114.1(2) . . ? C6 B2 B9 57.49(19) . . ? C1 B2 B5 57.74(18) . . ? C6 B2 B5 97.8(2) . . ? B9 B2 B5 57.15(19) . . ? C1 B2 Sn4 63.91(14) . . ? C6 B2 Sn4 75.53(14) . . ? B9 B2 Sn4 120.46(17) . . ? B5 B2 Sn4 100.80(15) . . ? C1 B2 H2 118.7(17) . . ? C6 B2 H2 114.2(17) . . ? B9 B2 H2 110.7(17) . . ? B5 B2 H2 131.4(17) . . ? Sn4 B2 H2 121.4(17) . . ? C1 B3 B8 118.4(2) . . ? C1 B3 B7 115.8(2) . . ? B8 B3 B7 57.77(16) . . ? C1 B3 B5 60.72(18) . . ? B8 B3 B5 61.38(17) . . ? B7 B3 B5 100.5(2) . . ? C1 B3 Sn4 72.75(14) . . ? B8 B3 Sn4 115.56(17) . . ? B7 B3 Sn4 61.09(12) . . ? B5 B3 Sn4 114.54(17) . . ? C1 B3 H3 116.2(16) . . ? B8 B3 H3 111.8(17) . . ? B7 B3 H3 123.4(16) . . ? B5 B3 H3 123.5(16) . . ? Sn4 B3 H3 117.2(17) . . ? C1 B5 B11 133.5(2) . . ? C1 B5 B9 100.5(2) . . ? B11 B5 B9 55.82(19) . . ? C1 B5 B8 100.82(19) . . ? B11 B5 B8 56.59(17) . . ? B9 B5 B8 103.5(2) . . ? C1 B5 B3 48.64(15) . . ? B11 B5 B3 106.6(2) . . ? B9 B5 B3 122.5(2) . . ? B8 B5 B3 54.83(15) . . ? C1 B5 B2 45.71(16) . . ? B11 B5 B2 103.5(2) . . ? B9 B5 B2 55.48(17) . . ? B8 B5 B2 115.6(2) . . ? B3 B5 B2 84.80(17) . . ? C1 B5 H5 107.2(19) . . ? B11 B5 H5 119.3(19) . . ? B9 B5 H5 119.7(17) . . ? B8 B5 H5 121.6(18) . . ? B3 B5 H5 116.1(17) . . ? B2 B5 H5 120.8(19) . . ? C61 C6 B2 112.1(2) . . ? C61 C6 B10 118.5(3) . . ? B2 C6 B10 116.6(2) . . ? C61 C6 B12 114.4(2) . . ? B2 C6 B12 122.9(2) . . ? B10 C6 B12 65.27(18) . . ? C61 C6 B9 119.5(2) . . ? B2 C6 B9 66.9(2) . . ? B10 C6 B9 112.8(2) . . ? B12 C6 B9 62.2(2) . . ? C61 C6 Sn4 109.27(18) . . ? B2 C6 Sn4 73.09(14) . . ? B10 C6 Sn4 56.24(13) . . ? B12 C6 Sn4 118.34(16) . . ? B9 C6 Sn4 125.27(19) . . ? B8 B7 B13 60.62(17) . . ? B8 B7 B10 106.0(2) . . ? B13 B7 B10 60.68(16) . . ? B8 B7 B3 58.63(16) . . ? B13 B7 B3 112.8(2) . . ? B10 B7 B3 113.4(2) . . ? B8 B7 Sn4 131.81(17) . . ? B13 B7 Sn4 131.43(17) . . ? B10 B7 Sn4 71.52(13) . . ? B3 B7 Sn4 77.79(13) . . ? B8 B7 H7 120.3(15) . . ? B13 B7 H7 115.1(15) . . ? B10 B7 H7 122.9(15) . . ? B3 B7 H7 118.3(15) . . ? Sn4 B7 H7 97.0(15) . . ? B7 B8 B11 109.3(2) . . ? B7 B8 B3 63.60(16) . . ? B11 B8 B3 117.3(2) . . ? B7 B8 B13 59.77(17) . . ? B11 B8 B13 61.62(18) . . ? B3 B8 B13 116.4(2) . . ? B7 B8 B5 106.1(2) . . ? B11 B8 B5 59.43(18) . . ? B3 B8 B5 63.79(17) . . ? B13 B8 B5 107.1(2) . . ? B7 B8 H8 119.2(17) . . ? B11 B8 H8 123.0(17) . . ? B3 B8 H8 110.2(17) . . ? B13 B8 H8 121.0(17) . . ? B5 B8 H8 125.4(17) . . ? C6 B9 B11 106.6(2) . . ? C6 B9 B12 58.56(19) . . ? B11 B9 B12 62.1(2) . . ? C6 B9 B2 55.56(18) . . ? B11 B9 B2 117.3(2) . . ? B12 B9 B2 109.4(2) . . ? C6 B9 B5 104.0(2) . . ? B11 B9 B5 60.4(2) . . ? B12 B9 B5 108.8(2) . . ? B2 B9 B5 67.4(2) . . ? C6 B9 H9 118.9(19) . . ? B11 B9 H9 126.2(19) . . ? B12 B9 H9 120.1(19) . . ? B2 B9 H9 111.5(19) . . ? B5 B9 H9 126.4(19) . . ? C6 B10 B13 107.2(2) . . ? C6 B10 B7 118.3(2) . . ? B13 B10 B7 58.42(16) . . ? C6 B10 B12 57.46(17) . . ? B13 B10 B12 58.94(17) . . ? B7 B10 B12 109.3(2) . . ? C6 B10 Sn4 90.76(15) . . ? B13 B10 Sn4 124.29(17) . . ? B7 B10 Sn4 66.52(13) . . ? B12 B10 Sn4 142.8(2) . . ? C6 B10 H10 120.3(16) . . ? B13 B10 H10 117.5(16) . . ? B7 B10 H10 118.2(16) . . ? B12 B10 H10 117.2(16) . . ? Sn4 B10 H10 94.6(16) . . ? B9 B11 B8 116.1(2) . . ? B9 B11 B12 59.1(2) . . ? B8 B11 B12 109.4(2) . . ? B9 B11 B13 108.4(2) . . ? B8 B11 B13 59.35(17) . . ? B12 B11 B13 58.99(18) . . ? B9 B11 B5 63.8(2) . . ? B8 B11 B5 63.98(19) . . ? B12 B11 B5 109.2(2) . . ? B13 B11 B5 108.8(2) . . ? B9 B11 H11 118.3(18) . . ? B8 B11 H11 117.3(18) . . ? B12 B11 H11 123.7(18) . . ? B13 B11 H11 123.9(18) . . ? B5 B11 H11 118.3(18) . . ? C6 B12 B9 59.26(19) . . ? C6 B12 B13 108.2(2) . . ? B9 B12 B13 109.9(3) . . ? C6 B12 B11 104.6(2) . . ? B9 B12 B11 58.8(2) . . ? B13 B12 B11 61.10(18) . . ? C6 B12 B10 57.26(17) . . ? B9 B12 B10 104.4(2) . . ? B13 B12 B10 60.26(17) . . ? B11 B12 B10 104.2(2) . . ? C6 B12 H12 113.5(19) . . ? B9 B12 H12 122.1(18) . . ? B13 B12 H12 124.6(18) . . ? B11 B12 H12 133.9(18) . . ? B10 B12 H12 117.7(18) . . ? B7 B13 B8 59.61(16) . . ? B7 B13 B12 113.1(2) . . ? B8 B13 B12 109.9(2) . . ? B7 B13 B10 60.90(16) . . ? B8 B13 B10 105.5(2) . . ? B12 B13 B10 60.81(17) . . ? B7 B13 B11 107.1(2) . . ? B8 B13 B11 59.03(18) . . ? B12 B13 B11 59.91(19) . . ? B10 B13 B11 103.7(2) . . ? B7 B13 H13 122.5(16) . . ? B8 B13 H13 119.4(17) . . ? B12 B13 H13 118.4(16) . . ? B10 B13 H13 128.7(17) . . ? B11 B13 H13 119.6(17) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C61 H61A 109.5 . . ? C6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C40 N41 C51 118.3(2) . . ? C40 N41 Sn4 123.92(17) . . ? C51 N41 Sn4 117.62(15) . . ? C49 N42 C50 118.6(2) . . ? C49 N42 Sn4 123.13(17) . . ? C50 N42 Sn4 118.25(16) . . ? N41 C40 C41 122.8(2) . . ? N41 C40 H40 118.6 . . ? C41 C40 H40 118.6 . . ? C42 C41 C40 119.4(2) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C41 C42 C43 119.7(2) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C51 C43 C42 117.3(2) . . ? C51 C43 C44 118.7(2) . . ? C42 C43 C44 124.0(2) . . ? C45 C44 C43 121.5(2) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C44 C45 C46 121.1(2) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C47 C46 C50 117.4(2) . . ? C47 C46 C45 123.4(2) . . ? C50 C46 C45 119.3(2) . . ? C48 C47 C46 119.7(2) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C47 C48 C49 119.3(2) . . ? C47 C48 H48 120.3 . . ? C49 C48 H48 120.3 . . ? N42 C49 C48 122.7(2) . . ? N42 C49 H49 118.7 . . ? C48 C49 H49 118.7 . . ? N42 C50 C46 122.4(2) . . ? N42 C50 C51 118.1(2) . . ? C46 C50 C51 119.5(2) . . ? N41 C51 C43 122.5(2) . . ? N41 C51 C50 117.5(2) . . ? C43 C51 C50 120.0(2) . . ? O1S C1S C5S 108.1(6) . . ? O1S C1S H1S1 110.1 . . ? C5S C1S H1S1 110.1 . . ? O1S C1S H1S2 110.1 . . ? C5S C1S H1S2 110.1 . . ? H1S1 C1S H1S2 108.4 . . ? O1S C3S C4S 106.5(8) . . ? O1S C3S H3S1 110.4 . . ? C4S C3S H3S1 110.4 . . ? O1S C3S H3S2 110.4 . . ? C4S C3S H3S2 110.4 . . ? H3S1 C3S H3S2 108.6 . . ? C3S C4S C5S 102.7(7) . . ? C3S C4S H4S1 111.2 . . ? C5S C4S H4S1 111.2 . . ? C3S C4S H4S2 111.2 . . ? C5S C4S H4S2 111.2 . . ? H4S1 C4S H4S2 109.1 . . ? C1S C5S C4S 100.7(5) . . ? C1S C5S H5S1 111.6 . . ? C4S C5S H5S1 111.6 . . ? C1S C5S H5S2 111.6 . . ? C4S C5S H5S2 111.6 . . ? H5S1 C5S H5S2 109.4 . . ? O1T C1T C4T 105.6(7) . . ? O1T C1T H1T1 110.6 . . ? C4T C1T H1T1 110.6 . . ? O1T C1T H1T2 110.6 . . ? C4T C1T H1T2 110.6 . . ? H1T1 C1T H1T2 108.7 . . ? O1T C2T C3T 107.3(9) . . ? O1T C2T H2T1 110.3 . . ? C3T C2T H2T1 110.3 . . ? O1T C2T H2T2 110.3 . . ? C3T C2T H2T2 110.3 . . ? H2T1 C2T H2T2 108.5 . . ? C4T C3T C2T 101.8(6) . . ? C4T C3T H3T1 111.4 . . ? C2T C3T H3T1 111.4 . . ? C4T C3T H3T2 111.4 . . ? C2T C3T H3T2 111.4 . . ? H3T1 C3T H3T2 109.3 . . ? C3T C4T C1T 101.6(6) . . ? C3T C4T H4T1 111.4 . . ? C1T C4T H4T1 111.4 . . ? C3T C4T H4T2 111.4 . . ? C1T C4T H4T2 111.4 . . ? H4T1 C4T H4T2 109.3 . . ? C1S O1S C3S 107.7(9) . . ? C2T O1T C1T 109.4(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.62 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.038 _refine_diff_density_min -1.114 _refine_diff_density_rms 0.106 # Attachment 'Compound_3_revised.cif' data_x3 _database_code_depnum_ccdc_archive 'CCDC 697457' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H28 B10 Cl2 D2 N2 Sn' _chemical_formula_weight 562.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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 10.7196(7) _cell_length_b 16.3778(11) _cell_length_c 15.0928(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.260(3) _cell_angle_gamma 90.00 _cell_volume 2543.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9727 _cell_measurement_theta_min 2.425 _cell_measurement_theta_max 37.444 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.697 _exptl_absorpt_correction_T_max 0.812 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95280 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 37.85 _reflns_number_total 13000 _reflns_number_gt 10989 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 (Bruker, 2006)' _computing_data_reduction 'APEX2 (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2003)' _computing_publication_material 'SHELXTL (Bruker, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.3273P] 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 13000 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.1260 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 Sn4 Sn 0.672302(8) 0.543927(5) 0.101254(6) 0.01134(4) Uani 1 1 d . . . C1 C 0.59658(14) 0.42477(9) 0.20375(10) 0.0142(2) Uani 1 1 d . . . B2 B 0.56987(17) 0.49346(11) 0.26348(12) 0.0159(3) Uani 1 1 d . . . H2 H 0.468(2) 0.5081(16) 0.2680(18) 0.027(6) Uiso 1 1 d . . . B3 B 0.73311(16) 0.40188(10) 0.19723(11) 0.0147(3) Uani 1 1 d . . . H3 H 0.835(2) 0.6336(16) 0.2555(17) 0.024(6) Uiso 1 1 d . . . B5 B 0.69757(17) 0.39753(10) 0.31495(12) 0.0164(3) Uani 1 1 d . . . H5 H 0.844(2) 0.5996(14) 0.4375(17) 0.016(5) Uiso 1 1 d . . . C6 C 0.67243(14) 0.56859(9) 0.30614(10) 0.0147(2) Uani 1 1 d . . . B7 B 0.85289(16) 0.48547(11) 0.21708(12) 0.0154(3) Uani 1 1 d . . . H7 H 0.920(3) 0.4852(17) 0.1740(19) 0.029(7) Uiso 1 1 d . . . B8 B 0.86495(17) 0.40701(11) 0.29829(12) 0.0176(3) Uani 1 1 d . . . H8 H 1.031(3) 0.523(2) 0.367(2) 0.037(8) Uiso 1 1 d . . . B9 B 0.68159(18) 0.49232(11) 0.38188(12) 0.0170(3) Uani 1 1 d . . . H9 H 0.636(3) 0.4954(18) 0.433(2) 0.030(7) Uiso 1 1 d . . . B10 B 0.80248(16) 0.57487(10) 0.26741(11) 0.0149(3) Uani 1 1 d . . . H10 H 0.740(2) 0.3477(16) 0.1516(17) 0.026(6) Uiso 1 1 d . . . B11 B 0.83318(18) 0.44686(13) 0.39731(12) 0.0181(3) Uani 1 1 d . . . H11 H 0.875(2) 0.4177(15) 0.4623(16) 0.018(5) Uiso 1 1 d . . . B12 B 0.81396(19) 0.55490(12) 0.38693(13) 0.0176(3) Uani 1 1 d . . . H12 H 0.669(2) 0.3415(17) 0.3419(17) 0.024(6) Uiso 1 1 d . . . B13 B 0.92207(17) 0.50586(12) 0.33484(13) 0.0182(3) Uani 1 1 d . . . H13 H 0.938(2) 0.3550(14) 0.3084(15) 0.013(5) Uiso 1 1 d . . . C11 C 0.48529(16) 0.36801(10) 0.15805(12) 0.0208(3) Uani 1 1 d . . . H11A H 0.4464 0.3854 0.0941 0.031 Uiso 1 1 calc R . . H11B H 0.4195 0.3699 0.1918 0.031 Uiso 1 1 calc R . . H11C H 0.5181 0.3121 0.1587 0.031 Uiso 1 1 calc R . . C61 C 0.60220(18) 0.64776(11) 0.31665(13) 0.0230(3) Uani 1 1 d . . . H61A H 0.5367 0.6364 0.3491 0.035 Uiso 1 1 calc R . . H61B H 0.5597 0.6702 0.2555 0.035 Uiso 1 1 calc R . . H61C H 0.6652 0.6873 0.3521 0.035 Uiso 1 1 calc R . . N41 N 0.82594(12) 0.61558(7) 0.04259(9) 0.0132(2) Uani 1 1 d . . . N42 N 0.73363(13) 0.46722(8) -0.01223(9) 0.0129(2) Uani 1 1 d . . . C40 C 0.87011(15) 0.68987(9) 0.07345(10) 0.0150(2) Uani 1 1 d . . . H40 H 0.8491 0.7108 0.1262 0.018 Uiso 1 1 calc R . . C41 C 0.94471(15) 0.73752(9) 0.03230(11) 0.0157(2) Uani 1 1 d . . . H41 H 0.9737 0.7899 0.0564 0.019 Uiso 1 1 calc R . . C42 C 0.97681(14) 0.70757(9) -0.04510(10) 0.0140(2) Uani 1 1 d . . . C43 C 0.93182(14) 0.63002(9) -0.07628(10) 0.0135(2) Uani 1 1 d . . . H43 H 0.9526 0.6074 -0.1284 0.016 Uiso 1 1 calc R . . C44 C 0.85675(13) 0.58552(8) -0.03170(10) 0.0119(2) Uani 1 1 d . . . C45 C 0.80489(13) 0.50321(9) -0.06255(10) 0.0123(2) Uani 1 1 d . . . C46 C 0.82645(15) 0.46466(9) -0.13914(11) 0.0148(2) Uani 1 1 d . . . H46 H 0.8751 0.4916 -0.1743 0.018 Uiso 1 1 calc R . . C47 C 0.77718(15) 0.38694(9) -0.16455(11) 0.0156(2) Uani 1 1 d . . . C48 C 0.70495(15) 0.35050(9) -0.11159(11) 0.0165(2) Uani 1 1 d . . . H48 H 0.6700 0.2973 -0.1263 0.020 Uiso 1 1 calc R . . C49 C 0.68464(14) 0.39262(9) -0.03744(10) 0.0148(2) Uani 1 1 d . . . H49 H 0.6336 0.3676 -0.0027 0.018 Uiso 1 1 calc R . . C50 C 1.05589(16) 0.75729(9) -0.09281(12) 0.0189(3) Uani 1 1 d . . . H50A H 1.1396 0.7708 -0.0490 0.028 Uiso 1 1 calc R . . H50B H 1.0092 0.8077 -0.1165 0.028 Uiso 1 1 calc R . . H50C H 1.0706 0.7259 -0.1442 0.028 Uiso 1 1 calc R . . C51 C 0.79940(19) 0.34489(11) -0.24715(12) 0.0240(3) Uani 1 1 d . . . H51A H 0.8789 0.3661 -0.2587 0.036 Uiso 1 1 calc R . . H51B H 0.7253 0.3551 -0.3012 0.036 Uiso 1 1 calc R . . H51C H 0.8085 0.2860 -0.2355 0.036 Uiso 1 1 calc R . . C53 C 0.6205(3) 0.87105(13) 0.09124(16) 0.0364(5) Uani 1 1 d . . . H53A H 0.6403 0.8997 0.0390 0.044 Uiso 1 1 calc R . . H53B H 0.5550 0.9037 0.1106 0.044 Uiso 1 1 calc R . . Cl1 Cl 0.55525(6) 0.77422(4) 0.05429(5) 0.04244(14) Uani 1 1 d . . . Cl2 Cl 0.76073(7) 0.86439(6) 0.18230(8) 0.0825(4) 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 Sn4 0.01133(5) 0.01101(6) 0.01247(6) 0.00064(3) 0.00461(4) 0.00092(2) C1 0.0152(5) 0.0124(6) 0.0141(6) 0.0013(4) 0.0029(4) -0.0022(4) B2 0.0157(6) 0.0176(7) 0.0160(7) 0.0004(5) 0.0069(5) -0.0004(5) B3 0.0175(6) 0.0128(6) 0.0137(6) -0.0002(5) 0.0043(5) 0.0011(5) B5 0.0210(7) 0.0127(6) 0.0153(7) 0.0009(5) 0.0046(5) -0.0011(5) C6 0.0173(6) 0.0128(6) 0.0148(6) -0.0002(4) 0.0060(5) 0.0013(4) B7 0.0131(6) 0.0169(7) 0.0170(7) 0.0007(5) 0.0055(5) 0.0008(5) B8 0.0175(7) 0.0171(7) 0.0168(7) 0.0023(6) 0.0023(5) 0.0053(5) B9 0.0219(7) 0.0171(7) 0.0131(6) 0.0003(5) 0.0069(6) -0.0001(6) B10 0.0153(6) 0.0146(7) 0.0143(6) -0.0004(5) 0.0034(5) -0.0013(5) B11 0.0219(9) 0.0173(8) 0.0138(8) 0.0012(5) 0.0029(7) 0.0010(5) B12 0.0211(8) 0.0162(7) 0.0144(7) -0.0012(5) 0.0034(6) -0.0010(6) B13 0.0147(6) 0.0203(8) 0.0177(7) -0.0003(6) 0.0013(5) 0.0000(5) C11 0.0200(7) 0.0185(7) 0.0226(7) -0.0003(6) 0.0039(5) -0.0061(5) C61 0.0282(8) 0.0186(7) 0.0240(7) -0.0022(6) 0.0101(6) 0.0058(6) N41 0.0152(5) 0.0118(5) 0.0142(5) -0.0011(4) 0.0064(4) -0.0010(4) N42 0.0133(5) 0.0122(5) 0.0141(5) -0.0005(4) 0.0054(4) -0.0008(4) C40 0.0201(6) 0.0126(5) 0.0134(6) -0.0008(4) 0.0068(5) -0.0026(5) C41 0.0193(6) 0.0119(5) 0.0172(6) -0.0005(4) 0.0073(5) -0.0020(4) C42 0.0143(5) 0.0119(5) 0.0168(6) 0.0005(4) 0.0062(4) -0.0004(4) C43 0.0149(5) 0.0129(5) 0.0148(6) -0.0006(4) 0.0076(4) -0.0003(4) C44 0.0111(5) 0.0107(5) 0.0145(5) -0.0006(4) 0.0048(4) 0.0004(4) C45 0.0118(5) 0.0120(5) 0.0139(5) -0.0002(4) 0.0047(4) 0.0002(4) C46 0.0147(6) 0.0144(6) 0.0167(6) -0.0021(4) 0.0065(5) -0.0006(4) C47 0.0165(6) 0.0145(6) 0.0164(6) -0.0033(5) 0.0056(5) 0.0009(4) C48 0.0188(6) 0.0126(6) 0.0185(6) -0.0041(5) 0.0061(5) -0.0020(5) C49 0.0158(6) 0.0126(5) 0.0168(6) -0.0007(4) 0.0058(5) -0.0015(4) C50 0.0228(7) 0.0133(6) 0.0253(7) 0.0025(5) 0.0145(6) -0.0004(5) C51 0.0316(8) 0.0217(7) 0.0226(7) -0.0102(6) 0.0142(6) -0.0039(6) C53 0.0515(14) 0.0236(9) 0.0320(10) 0.0017(8) 0.0083(9) 0.0013(9) Cl1 0.0324(2) 0.0416(3) 0.0563(4) -0.0197(3) 0.0172(2) -0.0123(2) Cl2 0.0318(3) 0.0866(6) 0.1113(7) -0.0761(6) -0.0094(4) 0.0142(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 Sn4 N42 2.3611(13) . ? Sn4 N41 2.3854(12) . ? Sn4 B7 2.4135(17) . ? Sn4 B10 2.5561(17) . ? Sn4 B3 2.7215(17) . ? Sn4 C1 2.7502(14) . ? Sn4 B2 3.0642(17) . ? Sn4 C6 3.1182(15) . ? C1 C11 1.517(2) . ? C1 B2 1.518(2) . ? C1 B3 1.540(2) . ? C1 B5 1.780(2) . ? B2 C6 1.655(2) . ? B2 B9 1.852(2) . ? B2 B5 2.086(3) . ? B2 H2 1.14(3) . ? B3 B8 1.767(2) . ? B3 B7 1.843(2) . ? B3 B5 1.920(2) . ? B3 H10 1.14(3) . ? B5 B11 1.816(3) . ? B5 B9 1.886(2) . ? B5 B8 1.887(3) . ? B5 H12 1.08(3) . ? C6 C61 1.530(2) . ? C6 B10 1.659(2) . ? C6 B12 1.674(3) . ? C6 B9 1.677(2) . ? B7 B8 1.755(2) . ? B7 B13 1.756(3) . ? B7 B10 1.801(2) . ? B7 H7 1.09(3) . ? B8 B11 1.749(3) . ? B8 B13 1.764(3) . ? B8 H13 1.14(2) . ? B9 B12 1.735(3) . ? B9 B11 1.743(3) . ? B9 H9 1.02(3) . ? B10 B13 1.796(2) . ? B10 B12 1.803(3) . ? B10 H3 1.06(3) . ? B11 B12 1.783(3) . ? B11 B13 1.798(3) . ? B11 H11 1.07(2) . ? B12 B13 1.765(3) . ? B12 H5 1.04(2) . ? B13 H8 1.17(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? N41 C40 1.3410(19) . ? N41 C44 1.3475(18) . ? N42 C49 1.3420(19) . ? N42 C45 1.3538(19) . ? C40 C41 1.383(2) . ? C40 H40 0.9500 . ? C41 C42 1.396(2) . ? C41 H41 0.9500 . ? C42 C43 1.393(2) . ? C42 C50 1.497(2) . ? C43 C44 1.3910(19) . ? C43 H43 0.9500 . ? C44 C45 1.483(2) . ? C45 C46 1.392(2) . ? C46 C47 1.390(2) . ? C46 H46 0.9500 . ? C47 C48 1.393(2) . ? C47 C51 1.500(2) . ? C48 C49 1.383(2) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C53 Cl2 1.733(3) . ? C53 Cl1 1.760(2) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? 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 N42 Sn4 N41 68.35(4) . . ? N42 Sn4 B7 89.12(5) . . ? N41 Sn4 B7 88.10(5) . . ? N42 Sn4 B10 129.11(5) . . ? N41 Sn4 B10 91.30(5) . . ? B7 Sn4 B10 42.37(6) . . ? N42 Sn4 B3 81.80(5) . . ? N41 Sn4 B3 122.05(5) . . ? B7 Sn4 B3 41.53(5) . . ? B10 Sn4 B3 70.35(5) . . ? N42 Sn4 C1 102.50(4) . . ? N41 Sn4 C1 154.30(4) . . ? B7 Sn4 C1 67.31(5) . . ? B10 Sn4 C1 75.81(5) . . ? B3 Sn4 C1 32.70(5) . . ? N42 Sn4 B2 132.14(5) . . ? N41 Sn4 B2 150.27(5) . . ? B7 Sn4 B2 73.05(5) . . ? B10 Sn4 B2 59.26(5) . . ? B3 Sn4 B2 55.26(5) . . ? C1 Sn4 B2 29.65(5) . . ? N42 Sn4 C6 149.93(4) . . ? N41 Sn4 C6 119.72(4) . . ? B7 Sn4 C6 63.61(5) . . ? B10 Sn4 C6 32.09(5) . . ? B3 Sn4 C6 69.47(4) . . ? C1 Sn4 C6 56.79(4) . . ? B2 Sn4 C6 31.05(4) . . ? C11 C1 B2 117.97(13) . . ? C11 C1 B3 117.51(13) . . ? B2 C1 B3 123.98(13) . . ? C11 C1 B5 117.91(12) . . ? B2 C1 B5 77.99(11) . . ? B3 C1 B5 70.21(10) . . ? C11 C1 Sn4 119.82(10) . . ? B2 C1 Sn4 86.71(9) . . ? B3 C1 Sn4 72.63(8) . . ? B5 C1 Sn4 120.71(9) . . ? C1 B2 C6 124.51(13) . . ? C1 B2 B9 112.77(13) . . ? C6 B2 B9 56.81(9) . . ? C1 B2 B5 56.61(9) . . ? C6 B2 B5 96.89(11) . . ? B9 B2 B5 56.87(9) . . ? C1 B2 Sn4 63.64(8) . . ? C6 B2 Sn4 76.28(8) . . ? B9 B2 Sn4 119.62(9) . . ? B5 B2 Sn4 98.98(8) . . ? C1 B2 H2 122.4(14) . . ? C6 B2 H2 111.3(14) . . ? B9 B2 H2 108.4(13) . . ? B5 B2 H2 132.6(13) . . ? Sn4 B2 H2 123.7(13) . . ? C1 B3 B8 118.53(13) . . ? C1 B3 B7 116.10(12) . . ? B8 B3 B7 58.14(10) . . ? C1 B3 B5 60.77(10) . . ? B8 B3 B5 61.38(10) . . ? B7 B3 B5 100.77(11) . . ? C1 B3 Sn4 74.68(8) . . ? B8 B3 Sn4 115.67(10) . . ? B7 B3 Sn4 60.25(7) . . ? B5 B3 Sn4 116.38(9) . . ? C1 B3 H10 116.8(12) . . ? B8 B3 H10 112.8(13) . . ? B7 B3 H10 121.2(13) . . ? B5 B3 H10 126.4(13) . . ? Sn4 B3 H10 113.0(13) . . ? C1 B5 B11 133.83(12) . . ? C1 B5 B9 100.14(11) . . ? B11 B5 B9 56.12(10) . . ? C1 B5 B8 101.75(11) . . ? B11 B5 B8 56.35(10) . . ? B9 B5 B8 103.65(11) . . ? C1 B5 B3 49.02(8) . . ? B11 B5 B3 106.78(12) . . ? B9 B5 B3 122.44(11) . . ? B8 B5 B3 55.32(9) . . ? C1 B5 B2 45.39(8) . . ? B11 B5 B2 103.64(11) . . ? B9 B5 B2 55.31(9) . . ? B8 B5 B2 115.97(11) . . ? B3 B5 B2 84.66(9) . . ? C1 B5 H12 113.8(13) . . ? B11 B5 H12 112.3(13) . . ? B9 B5 H12 114.7(14) . . ? B8 B5 H12 120.2(14) . . ? B3 B5 H12 122.0(14) . . ? B2 B5 H12 123.4(13) . . ? C61 C6 B2 112.20(13) . . ? C61 C6 B10 118.06(13) . . ? B2 C6 B10 116.18(12) . . ? C61 C6 B12 114.20(13) . . ? B2 C6 B12 123.46(13) . . ? B10 C6 B12 65.50(10) . . ? C61 C6 B9 119.81(13) . . ? B2 C6 B9 67.50(10) . . ? B10 C6 B9 113.06(12) . . ? B12 C6 B9 62.34(10) . . ? C61 C6 Sn4 110.43(10) . . ? B2 C6 Sn4 72.67(8) . . ? B10 C6 Sn4 54.95(7) . . ? B12 C6 Sn4 116.97(9) . . ? B9 C6 Sn4 124.27(9) . . ? B8 B7 B13 60.31(10) . . ? B8 B7 B10 105.83(12) . . ? B13 B7 B10 60.65(10) . . ? B8 B7 B3 58.77(10) . . ? B13 B7 B3 112.54(12) . . ? B10 B7 B3 113.25(11) . . ? B8 B7 Sn4 133.11(10) . . ? B13 B7 Sn4 133.12(11) . . ? B10 B7 Sn4 73.05(8) . . ? B3 B7 Sn4 78.22(8) . . ? B8 B7 H7 118.7(15) . . ? B13 B7 H7 116.2(14) . . ? B10 B7 H7 125.3(15) . . ? B3 B7 H7 116.2(14) . . ? Sn4 B7 H7 95.5(14) . . ? B11 B8 B7 109.24(13) . . ? B11 B8 B13 61.57(11) . . ? B7 B8 B13 59.85(10) . . ? B11 B8 B3 117.07(12) . . ? B7 B8 B3 63.09(10) . . ? B13 B8 B3 115.93(13) . . ? B11 B8 B5 59.80(10) . . ? B7 B8 B5 105.45(11) . . ? B13 B8 B5 107.08(12) . . ? B3 B8 B5 63.29(10) . . ? B11 B8 H13 117.2(11) . . ? B7 B8 H13 123.6(11) . . ? B13 B8 H13 118.6(11) . . ? B3 B8 H13 115.8(11) . . ? B5 B8 H13 124.5(11) . . ? C6 B9 B12 58.74(10) . . ? C6 B9 B11 106.48(12) . . ? B12 B9 B11 61.70(11) . . ? C6 B9 B2 55.69(9) . . ? B12 B9 B2 109.66(12) . . ? B11 B9 B2 117.39(12) . . ? C6 B9 B5 104.16(11) . . ? B12 B9 B5 108.30(12) . . ? B11 B9 B5 59.92(10) . . ? B2 B9 B5 67.83(10) . . ? C6 B9 H9 121.8(16) . . ? B12 B9 H9 119.8(16) . . ? B11 B9 H9 123.1(16) . . ? B2 B9 H9 114.1(16) . . ? B5 B9 H9 125.3(17) . . ? C6 B10 B13 107.35(12) . . ? C6 B10 B7 118.64(12) . . ? B13 B10 B7 58.43(10) . . ? C6 B10 B12 57.66(10) . . ? B13 B10 B12 58.74(10) . . ? B7 B10 B12 109.27(12) . . ? C6 B10 Sn4 92.96(9) . . ? B13 B10 Sn4 122.55(10) . . ? B7 B10 Sn4 64.58(7) . . ? B12 B10 Sn4 144.20(10) . . ? C6 B10 H3 117.9(13) . . ? B13 B10 H3 116.9(14) . . ? B7 B10 H3 121.0(13) . . ? B12 B10 H3 113.8(14) . . ? Sn4 B10 H3 97.4(13) . . ? B9 B11 B8 116.26(12) . . ? B9 B11 B12 58.93(11) . . ? B8 B11 B12 109.90(13) . . ? B9 B11 B13 108.15(13) . . ? B8 B11 B13 59.60(10) . . ? B12 B11 B13 59.06(11) . . ? B9 B11 B5 63.96(10) . . ? B8 B11 B5 63.85(10) . . ? B12 B11 B5 109.31(13) . . ? B13 B11 B5 108.67(12) . . ? B9 B11 H11 116.8(12) . . ? B8 B11 H11 118.9(13) . . ? B12 B11 H11 122.1(13) . . ? B13 B11 H11 124.8(13) . . ? B5 B11 H11 118.7(13) . . ? C6 B12 B9 58.92(10) . . ? C6 B12 B13 108.10(13) . . ? B9 B12 B13 110.04(13) . . ? C6 B12 B11 104.82(13) . . ? B9 B12 B11 59.37(10) . . ? B13 B12 B11 60.90(11) . . ? C6 B12 B10 56.84(10) . . ? B9 B12 B10 103.73(12) . . ? B13 B12 B10 60.43(10) . . ? B11 B12 B10 103.99(12) . . ? C6 B12 H5 118.0(13) . . ? B9 B12 H5 121.8(13) . . ? B13 B12 H5 122.8(12) . . ? B11 B12 H5 129.0(13) . . ? B10 B12 H5 121.8(13) . . ? B7 B13 B8 59.84(10) . . ? B7 B13 B12 113.17(13) . . ? B8 B13 B12 110.07(13) . . ? B7 B13 B10 60.92(10) . . ? B8 B13 B10 105.67(12) . . ? B12 B13 B10 60.83(10) . . ? B7 B13 B11 107.04(12) . . ? B8 B13 B11 58.82(10) . . ? B12 B13 B11 60.04(11) . . ? B10 B13 B11 103.66(12) . . ? B7 B13 H8 124.0(16) . . ? B8 B13 H8 125.0(16) . . ? B12 B13 H8 114.0(16) . . ? B10 B13 H8 123.7(16) . . ? B11 B13 H8 121.8(16) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C61 H61A 109.5 . . ? C6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C40 N41 C44 118.40(12) . . ? C40 N41 Sn4 122.06(9) . . ? C44 N41 Sn4 118.99(9) . . ? C49 N42 C45 118.34(13) . . ? C49 N42 Sn4 121.59(10) . . ? C45 N42 Sn4 119.39(9) . . ? N41 C40 C41 123.25(13) . . ? N41 C40 H40 118.4 . . ? C41 C40 H40 118.4 . . ? C40 C41 C42 119.12(13) . . ? C40 C41 H41 120.4 . . ? C42 C41 H41 120.4 . . ? C43 C42 C41 117.39(13) . . ? C43 C42 C50 121.50(13) . . ? C41 C42 C50 121.11(13) . . ? C44 C43 C42 120.45(13) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? N41 C44 C43 121.39(13) . . ? N41 C44 C45 115.84(12) . . ? C43 C44 C45 122.77(12) . . ? N42 C45 C46 121.29(13) . . ? N42 C45 C44 116.14(12) . . ? C46 C45 C44 122.57(12) . . ? C47 C46 C45 120.38(14) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 117.59(13) . . ? C46 C47 C51 120.86(14) . . ? C48 C47 C51 121.54(14) . . ? C49 C48 C47 119.30(14) . . ? C49 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? N42 C49 C48 123.09(13) . . ? N42 C49 H49 118.5 . . ? C48 C49 H49 118.5 . . ? C42 C50 H50A 109.5 . . ? C42 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C42 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C47 C51 H51A 109.5 . . ? C47 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C47 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Cl2 C53 Cl1 111.97(13) . . ? Cl2 C53 H53A 109.2 . . ? Cl1 C53 H53A 109.2 . . ? Cl2 C53 H53B 109.2 . . ? Cl1 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.141 _refine_diff_density_min -3.045 _refine_diff_density_rms 0.201 # Attachment 'Compound_4_revised.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 697458' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H32 B10 Cl2 D2 N2 Sn' _chemical_formula_weight 686.26 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 11.4342(11) _cell_length_b 16.0203(16) _cell_length_c 17.1455(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3140.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 106 _cell_measurement_theta_min 3.23 _cell_measurement_theta_max 17.24 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6889 _exptl_absorpt_correction_T_max 0.8241 _exptl_absorpt_process_details TWINABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12491 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1347 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.63 _reflns_number_total 12491 _reflns_number_gt 7773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 (Bruker, 2006)' _computing_data_reduction 'APEX2 (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2003)' _computing_publication_material 'SHELXTL (Bruker, 2003)' _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. refined as three domains domain 2 is Rotated from first domain by 118.9 degrees about reciprocal axis -0.437 0.134 1.000 and real axis -0.985 0.162 1.000 Twin law to convert hkl from first to -0.050 0.447 -0.518 domain 2 (SHELXL TWIN matrix): -1.153 -0.455 -0.309 -0.848 0.675 0.539 domain 3 is Rotated from first domain by 108.1 degrees about reciprocal axis -0.136 1.000 -0.326 and real axis -0.280 1.000 -0.282 Twin law to convert hkl from first to -0.269 -0.352 -0.551 domain 3 (SHELXL TWIN matrix): 0.053 0.847 -0.492 1.449 -0.193 -0.200 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0186P] 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 0.12(3) _refine_ls_number_reflns 12491 _refine_ls_number_parameters 398 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1339 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1887 _refine_ls_wR_factor_gt 0.1588 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn4 Sn 0.51842(3) 0.34308(2) 0.28757(4) 0.02169(13) Uani 1 1 d . . . C1 C 0.4640(6) 0.5004(5) 0.3293(4) 0.0247(16) Uani 1 1 d . . . B2 B 0.5665(8) 0.4931(5) 0.3871(5) 0.0261(18) Uani 1 1 d . . . H2 H 0.6465 0.5073 0.3517 0.031 Uiso 1 1 calc R . . B3 B 0.3485(7) 0.4530(5) 0.3368(4) 0.0215(17) Uani 1 1 d . . . H3 H 0.3098 0.4526 0.2768 0.026 Uiso 1 1 calc R . . B5 B 0.3995(7) 0.5238(5) 0.4216(5) 0.0204(16) Uani 1 1 d D . . H5 H 0.362(8) 0.587(3) 0.429(6) 0.07(3) Uiso 1 1 d D . . C6 C 0.5860(6) 0.4118(4) 0.4456(4) 0.0236(15) Uani 1 1 d . . . B7 B 0.3579(10) 0.3483(5) 0.3841(6) 0.023(2) Uani 1 1 d . . . H7 H 0.3035 0.2969 0.3587 0.028 Uiso 1 1 calc R . . B8 B 0.2941(7) 0.4342(5) 0.4314(5) 0.0232(17) Uani 1 1 d . . . H8 H 0.1970 0.4420 0.4357 0.028 Uiso 1 1 calc R . . B9 B 0.5233(7) 0.4950(5) 0.4896(5) 0.0231(17) Uani 1 1 d . . . H9 H 0.581(6) 0.545(4) 0.521(4) 0.013(16) Uiso 1 1 d . . . B10 B 0.4967(7) 0.3315(5) 0.4340(5) 0.0258(18) Uani 1 1 d . . . H10 H 0.5440 0.2703 0.4342 0.031 Uiso 1 1 calc R . . B11 B 0.3799(7) 0.4654(5) 0.5098(5) 0.0240(18) Uani 1 1 d . . . H11 H 0.3343 0.4962 0.5599 0.029 Uiso 1 1 calc R . . B12 B 0.5003(8) 0.3938(6) 0.5222(5) 0.027(2) Uani 1 1 d . . . H12 H 0.521(8) 0.368(7) 0.576(7) 0.06(3) Uiso 1 1 d . . . B13 B 0.3639(7) 0.3555(5) 0.4871(5) 0.0240(18) Uani 1 1 d . . . H13 H 0.317(6) 0.315(4) 0.531(4) 0.016(17) Uiso 1 1 d . . . C11 C 0.4731(6) 0.5694(5) 0.2681(4) 0.030(2) Uani 1 1 d . . . H11A H 0.5021 0.6206 0.2927 0.046 Uiso 1 1 calc R . . H11B H 0.3958 0.5797 0.2455 0.046 Uiso 1 1 calc R . . H11C H 0.5274 0.5521 0.2269 0.046 Uiso 1 1 calc R . . C61 C 0.7176(6) 0.3943(5) 0.4583(5) 0.036(2) Uani 1 1 d . . . H61A H 0.7553 0.3842 0.4078 0.054 Uiso 1 1 calc R . . H61B H 0.7269 0.3451 0.4916 0.054 Uiso 1 1 calc R . . H61C H 0.7541 0.4427 0.4835 0.054 Uiso 1 1 calc R . . N41 N 0.4690(4) 0.2000(4) 0.2728(4) 0.0254(18) Uani 1 1 d . . . N42 N 0.3684(6) 0.3229(4) 0.1961(4) 0.0238(16) Uani 1 1 d . . . C42 C 0.5301(6) 0.1403(5) 0.3091(4) 0.029(2) Uani 1 1 d . . . H42 H 0.5980 0.1558 0.3374 0.035 Uiso 1 1 calc R . . C43 C 0.4992(5) 0.0580(4) 0.3071(4) 0.026(2) Uani 1 1 d . . . H43 H 0.5456 0.0178 0.3337 0.032 Uiso 1 1 calc R . . C44 C 0.4001(6) 0.0329(4) 0.2663(4) 0.0218(16) Uani 1 1 d . . . C45 C 0.3618(6) -0.0555(4) 0.2670(4) 0.0224(17) Uani 1 1 d . . . C46 C 0.3946(7) -0.1093(5) 0.3278(5) 0.0327(18) Uani 1 1 d . . . H46 H 0.4422 -0.0891 0.3691 0.039 Uiso 1 1 calc R . . C47 C 0.3583(7) -0.1910(5) 0.3277(5) 0.0368(19) Uani 1 1 d . . . H47 H 0.3807 -0.2265 0.3694 0.044 Uiso 1 1 calc R . . C48 C 0.2899(7) -0.2227(5) 0.2684(5) 0.038(2) Uani 1 1 d . . . H48 H 0.2678 -0.2798 0.2683 0.045 Uiso 1 1 calc R . . C49 C 0.2541(7) -0.1704(4) 0.2093(5) 0.0313(18) Uani 1 1 d . . . H49 H 0.2042 -0.1908 0.1692 0.038 Uiso 1 1 calc R . . C50 C 0.2909(6) -0.0880(5) 0.2083(5) 0.0286(17) Uani 1 1 d . . . H50 H 0.2672 -0.0528 0.1666 0.034 Uiso 1 1 calc R . . C51 C 0.3383(6) 0.0942(4) 0.2266(4) 0.0220(15) Uani 1 1 d . . . H51 H 0.2708 0.0798 0.1973 0.026 Uiso 1 1 calc R . . C52 C 0.3759(6) 0.1781(4) 0.2300(4) 0.0198(15) Uani 1 1 d . . . C53 C 0.3164(6) 0.2473(4) 0.1878(4) 0.0228(15) Uani 1 1 d . . . C54 C 0.2167(6) 0.2383(4) 0.1415(4) 0.0227(15) Uani 1 1 d . . . H54 H 0.1820 0.1848 0.1355 0.027 Uiso 1 1 calc R . . C55 C 0.1672(6) 0.3076(4) 0.1038(4) 0.0210(15) Uani 1 1 d . . . C56 C 0.0614(6) 0.3020(4) 0.0570(4) 0.0217(15) Uani 1 1 d . . . C57 C 0.0227(6) 0.2278(4) 0.0223(4) 0.0199(14) Uani 1 1 d . . . H57 H 0.0654 0.1778 0.0311 0.024 Uiso 1 1 calc R . . C58 C -0.0765(6) 0.2254(4) -0.0247(4) 0.0254(16) Uani 1 1 d . . . H58 H -0.0991 0.1750 -0.0496 0.031 Uiso 1 1 calc R . . C59 C -0.1428(6) 0.2985(5) -0.0349(4) 0.0309(17) Uani 1 1 d . . . H59 H -0.2104 0.2975 -0.0671 0.037 Uiso 1 1 calc R . . C71 C -0.0118(7) 0.3749(5) 0.0464(6) 0.031(2) Uani 1 1 d . . . H71 H 0.0091 0.4258 0.0710 0.037 Uiso 1 1 calc R . . C72 C -0.1106(7) 0.3716(5) 0.0014(5) 0.0287(17) Uani 1 1 d . . . H72 H -0.1573 0.4202 -0.0048 0.034 Uiso 1 1 calc R . . C73 C 0.2281(6) 0.3823(4) 0.1110(4) 0.0237(16) Uani 1 1 d . . . H73 H 0.2017 0.4302 0.0836 0.028 Uiso 1 1 calc R . . C74 C 0.3257(6) 0.3879(4) 0.1571(4) 0.0236(16) Uani 1 1 d . . . H74 H 0.3643 0.4402 0.1614 0.028 Uiso 1 1 calc R . . C021 C 0.4485(7) 0.1605(5) 0.6159(6) 0.037(2) Uani 1 1 d . . . H02A H 0.5046 0.1876 0.6519 0.044 Uiso 1 1 calc R . . H02B H 0.4013 0.2050 0.5910 0.044 Uiso 1 1 calc R . . Cl1 Cl 0.35555(18) 0.09449(14) 0.66960(13) 0.0408(5) Uani 1 1 d . . . Cl2 Cl 0.5270(2) 0.10537(15) 0.54277(14) 0.0390(6) 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 Sn4 0.01716(19) 0.02085(19) 0.0271(2) -0.0037(3) 0.0031(4) -0.00174(17) C1 0.018(4) 0.024(4) 0.032(4) 0.002(3) 0.002(3) 0.005(3) B2 0.029(4) 0.023(4) 0.026(5) -0.005(4) 0.005(3) 0.000(3) B3 0.026(4) 0.025(4) 0.014(4) 0.002(3) 0.002(3) 0.004(3) B5 0.020(4) 0.016(4) 0.026(4) -0.002(3) 0.002(3) -0.002(3) C6 0.020(4) 0.025(4) 0.026(4) -0.002(3) -0.002(3) 0.002(3) B7 0.021(5) 0.022(5) 0.027(5) 0.005(4) -0.002(4) -0.001(4) B8 0.020(4) 0.023(4) 0.026(5) 0.001(4) 0.002(3) -0.003(3) B9 0.023(4) 0.020(4) 0.026(4) -0.001(3) -0.001(4) 0.000(3) B10 0.024(5) 0.022(4) 0.031(5) -0.002(3) -0.003(3) 0.002(3) B11 0.028(4) 0.016(4) 0.028(5) -0.006(3) 0.007(3) -0.004(3) B12 0.037(5) 0.027(4) 0.018(4) -0.002(4) -0.007(4) -0.002(4) B13 0.026(4) 0.021(4) 0.025(4) 0.002(3) 0.000(3) 0.004(3) C11 0.027(4) 0.024(4) 0.040(6) 0.005(3) 0.002(3) -0.006(3) C61 0.024(4) 0.038(5) 0.047(5) -0.009(4) -0.019(4) 0.009(3) N41 0.011(2) 0.028(3) 0.038(5) -0.006(3) -0.002(3) 0.003(2) N42 0.022(4) 0.033(4) 0.016(3) -0.008(3) 0.002(3) -0.003(3) C42 0.018(3) 0.031(4) 0.038(6) -0.008(3) 0.000(3) 0.002(3) C43 0.012(4) 0.027(3) 0.040(6) -0.005(3) -0.005(3) 0.007(2) C44 0.018(3) 0.022(3) 0.026(4) -0.006(3) -0.001(2) -0.001(3) C45 0.021(3) 0.020(3) 0.026(5) 0.003(3) 0.004(2) 0.003(3) C46 0.025(4) 0.035(5) 0.037(4) 0.010(4) -0.007(3) -0.002(3) C47 0.035(5) 0.037(5) 0.038(5) 0.011(4) -0.007(4) -0.010(4) C48 0.034(4) 0.021(4) 0.058(7) 0.006(4) -0.007(4) -0.002(3) C49 0.038(5) 0.021(4) 0.035(4) 0.000(3) -0.006(3) 0.001(3) C50 0.030(4) 0.026(4) 0.030(4) 0.001(3) -0.003(3) 0.002(3) C51 0.022(4) 0.017(3) 0.028(4) -0.004(3) 0.003(3) 0.004(3) C52 0.016(3) 0.023(4) 0.020(4) -0.006(3) 0.005(3) 0.002(3) C53 0.023(3) 0.021(4) 0.025(4) -0.002(3) 0.008(3) 0.000(3) C54 0.026(4) 0.018(4) 0.024(4) -0.004(3) 0.006(3) 0.001(3) C55 0.024(4) 0.016(3) 0.023(4) -0.001(3) 0.007(3) -0.002(3) C56 0.025(4) 0.014(3) 0.026(4) 0.004(3) 0.007(3) 0.001(3) C57 0.020(3) 0.017(3) 0.023(4) -0.005(3) 0.004(3) 0.003(3) C58 0.028(4) 0.022(4) 0.026(4) -0.004(3) -0.001(3) -0.004(3) C59 0.022(4) 0.044(5) 0.027(4) 0.003(4) 0.002(3) -0.003(3) C71 0.033(5) 0.022(4) 0.038(5) -0.003(4) 0.002(4) 0.003(3) C72 0.028(4) 0.024(4) 0.033(4) 0.011(3) 0.004(3) 0.014(3) C73 0.036(4) 0.017(4) 0.018(4) -0.002(3) 0.000(3) 0.008(3) C74 0.027(4) 0.011(4) 0.032(4) -0.001(3) 0.005(3) 0.001(3) C021 0.036(5) 0.014(3) 0.061(6) -0.004(4) 0.007(4) 0.002(3) Cl1 0.0338(11) 0.0434(12) 0.0451(13) -0.0029(10) 0.0053(9) -0.0026(9) Cl2 0.0379(12) 0.0350(12) 0.0441(14) 0.0004(10) 0.0078(10) 0.0063(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 Sn4 N42 2.347(7) . ? Sn4 N41 2.374(6) . ? Sn4 B7 2.473(11) . ? Sn4 B10 2.530(9) . ? C1 C11 1.526(10) . ? C1 B3 1.529(11) . ? C1 B2 1.539(11) . ? C1 B5 1.786(11) . ? B2 C6 1.660(11) . ? B2 B9 1.826(12) . ? B2 B5 2.059(11) . ? B2 H2 1.1200 . ? B3 B8 1.763(11) . ? B3 B7 1.866(12) . ? B3 B5 1.933(11) . ? B3 H3 1.1200 . ? B5 B11 1.792(12) . ? B5 B8 1.882(11) . ? B5 B9 1.891(11) . ? B5 H5 1.10(2) . ? C6 C61 1.546(10) . ? C6 B10 1.654(10) . ? C6 B12 1.663(12) . ? C6 B9 1.692(11) . ? B7 B8 1.755(13) . ? B7 B13 1.771(13) . ? B7 B10 1.824(13) . ? B7 H7 1.1200 . ? B8 B11 1.738(12) . ? B8 B13 1.771(12) . ? B8 H8 1.1200 . ? B9 B12 1.735(12) . ? B9 B11 1.742(12) . ? B9 H9 1.17(6) . ? B10 B13 1.812(12) . ? B10 B12 1.812(12) . ? B10 H10 1.1200 . ? B11 B12 1.804(12) . ? B11 B13 1.813(11) . ? B11 H11 1.1200 . ? B12 B13 1.781(12) . ? B12 H12 1.04(11) . ? B13 H13 1.13(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? N41 C42 1.337(10) . ? N41 C52 1.340(9) . ? N42 C74 1.330(10) . ? N42 C53 1.356(10) . ? C42 C43 1.364(10) . ? C42 H42 0.9500 . ? C43 C44 1.391(9) . ? C43 H43 0.9500 . ? C44 C51 1.388(9) . ? C44 C45 1.483(9) . ? C45 C50 1.394(10) . ? C45 C46 1.403(10) . ? C46 C47 1.373(11) . ? C46 H46 0.9500 . ? C47 C48 1.379(11) . ? C47 H47 0.9500 . ? C48 C49 1.377(11) . ? C48 H48 0.9500 . ? C49 C50 1.385(10) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.412(9) . ? C51 H51 0.9500 . ? C52 C53 1.488(10) . ? C53 C54 1.396(10) . ? C54 C55 1.404(10) . ? C54 H54 0.9500 . ? C55 C73 1.389(10) . ? C55 C56 1.455(10) . ? C56 C57 1.400(10) . ? C56 C71 1.448(11) . ? C57 C58 1.392(10) . ? C57 H57 0.9500 . ? C58 C59 1.406(11) . ? C58 H58 0.9500 . ? C59 C72 1.376(11) . ? C59 H59 0.9500 . ? C71 C72 1.368(12) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.370(10) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C021 Cl1 1.759(8) . ? C021 Cl2 1.778(8) . ? C021 H02A 0.9900 . ? C021 H02B 0.9900 . ? 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 N42 Sn4 N41 67.8(2) . . ? N42 Sn4 B7 84.8(2) . . ? N41 Sn4 B7 85.8(3) . . ? N42 Sn4 B10 125.6(2) . . ? N41 Sn4 B10 90.7(2) . . ? B7 Sn4 B10 42.7(3) . . ? C11 C1 B3 118.5(6) . . ? C11 C1 B2 116.4(6) . . ? B3 C1 B2 124.4(7) . . ? C11 C1 B5 119.0(6) . . ? B3 C1 B5 70.9(5) . . ? B2 C1 B5 76.1(5) . . ? C1 B2 C6 123.4(6) . . ? C1 B2 B9 114.4(6) . . ? C6 B2 B9 57.8(4) . . ? C1 B2 B5 57.4(5) . . ? C6 B2 B5 97.9(5) . . ? B9 B2 B5 57.9(4) . . ? C1 B2 H2 104.9 . . ? C6 B2 H2 112.2 . . ? B9 B2 H2 137.6 . . ? B5 B2 H2 149.8 . . ? C1 B3 B8 117.9(6) . . ? C1 B3 B7 115.7(6) . . ? B8 B3 B7 57.8(5) . . ? C1 B3 B5 60.8(5) . . ? B8 B3 B5 61.0(4) . . ? B7 B3 B5 100.6(5) . . ? C1 B3 H3 105.4 . . ? B8 B3 H3 134.8 . . ? B7 B3 H3 114.6 . . ? B5 B3 H3 144.4 . . ? C1 B5 B11 133.6(6) . . ? C1 B5 B8 100.6(5) . . ? B11 B5 B8 56.4(4) . . ? C1 B5 B9 100.7(5) . . ? B11 B5 B9 56.4(4) . . ? B8 B5 B9 103.8(5) . . ? C1 B5 B3 48.3(4) . . ? B11 B5 B3 106.9(5) . . ? B8 B5 B3 55.0(4) . . ? B9 B5 B3 123.1(5) . . ? C1 B5 B2 46.5(4) . . ? B11 B5 B2 103.5(5) . . ? B8 B5 B2 115.9(5) . . ? B9 B5 B2 54.9(4) . . ? B3 B5 B2 85.6(5) . . ? C1 B5 H5 117(5) . . ? B11 B5 H5 110(5) . . ? B8 B5 H5 116(5) . . ? B9 B5 H5 117(5) . . ? B3 B5 H5 120(5) . . ? B2 B5 H5 127(5) . . ? C61 C6 B10 118.5(6) . . ? C61 C6 B2 110.9(6) . . ? B10 C6 B2 117.1(6) . . ? C61 C6 B12 115.5(6) . . ? B10 C6 B12 66.2(5) . . ? B2 C6 B12 122.3(6) . . ? C61 C6 B9 119.5(6) . . ? B10 C6 B9 113.9(6) . . ? B2 C6 B9 66.0(5) . . ? B12 C6 B9 62.3(5) . . ? B8 B7 B13 60.3(5) . . ? B8 B7 B10 105.1(6) . . ? B13 B7 B10 60.5(5) . . ? B8 B7 B3 58.2(4) . . ? B13 B7 B3 112.1(6) . . ? B10 B7 B3 112.7(6) . . ? B8 B7 Sn4 130.1(5) . . ? B13 B7 Sn4 129.8(6) . . ? B10 B7 Sn4 70.3(5) . . ? B3 B7 Sn4 77.5(4) . . ? B8 B7 H7 121.7 . . ? B13 B7 H7 117.2 . . ? B10 B7 H7 123.8 . . ? B3 B7 H7 117.5 . . ? Sn4 B7 H7 97.3 . . ? B11 B8 B7 110.4(6) . . ? B11 B8 B3 117.5(6) . . ? B7 B8 B3 64.0(5) . . ? B11 B8 B13 62.2(5) . . ? B7 B8 B13 60.3(5) . . ? B3 B8 B13 117.3(6) . . ? B11 B8 B5 59.2(4) . . ? B7 B8 B5 106.9(6) . . ? B3 B8 B5 64.0(5) . . ? B13 B8 B5 107.6(5) . . ? B11 B8 H8 118.5 . . ? B7 B8 H8 122.0 . . ? B3 B8 H8 113.0 . . ? B13 B8 H8 119.4 . . ? B5 B8 H8 123.8 . . ? C6 B9 B12 58.0(5) . . ? C6 B9 B11 105.8(5) . . ? B12 B9 B11 62.5(5) . . ? C6 B9 B2 56.2(4) . . ? B12 B9 B2 109.6(6) . . ? B11 B9 B2 116.2(6) . . ? C6 B9 B5 103.6(5) . . ? B12 B9 B5 108.2(6) . . ? B11 B9 B5 59.0(5) . . ? B2 B9 B5 67.3(5) . . ? C6 B9 H9 121(3) . . ? B12 B9 H9 125(3) . . ? B11 B9 H9 129(3) . . ? B2 B9 H9 108(3) . . ? B5 B9 H9 123(3) . . ? C6 B10 B13 107.0(6) . . ? C6 B10 B12 57.1(5) . . ? B13 B10 B12 58.9(5) . . ? C6 B10 B7 118.6(6) . . ? B13 B10 B7 58.3(5) . . ? B12 B10 B7 109.3(6) . . ? C6 B10 Sn4 90.1(4) . . ? B13 B10 Sn4 124.4(5) . . ? B12 B10 Sn4 141.8(5) . . ? B7 B10 Sn4 67.0(4) . . ? C6 B10 H10 112.5 . . ? B13 B10 H10 126.1 . . ? B12 B10 H10 118.0 . . ? B7 B10 H10 123.4 . . ? Sn4 B10 H10 91.1 . . ? B8 B11 B9 117.1(6) . . ? B8 B11 B5 64.4(5) . . ? B9 B11 B5 64.7(5) . . ? B8 B11 B12 109.8(6) . . ? B9 B11 B12 58.6(5) . . ? B5 B11 B12 109.6(6) . . ? B8 B11 B13 59.8(5) . . ? B9 B11 B13 108.5(6) . . ? B5 B11 B13 109.8(6) . . ? B12 B11 B13 59.0(4) . . ? B8 B11 H11 117.2 . . ? B9 B11 H11 118.1 . . ? B5 B11 H11 118.4 . . ? B12 B11 H11 123.1 . . ? B13 B11 H11 123.1 . . ? C6 B12 B9 59.7(5) . . ? C6 B12 B13 108.0(6) . . ? B9 B12 B13 110.2(6) . . ? C6 B12 B11 104.3(6) . . ? B9 B12 B11 58.9(5) . . ? B13 B12 B11 60.7(5) . . ? C6 B12 B10 56.6(4) . . ? B9 B12 B10 104.4(6) . . ? B13 B12 B10 60.5(5) . . ? B11 B12 B10 103.6(6) . . ? C6 B12 H12 130(5) . . ? B9 B12 H12 129(6) . . ? B13 B12 H12 111(5) . . ? B11 B12 H12 122(5) . . ? B10 B12 H12 122(6) . . ? B8 B13 B7 59.4(5) . . ? B8 B13 B12 109.4(6) . . ? B7 B13 B12 113.2(7) . . ? B8 B13 B10 105.0(6) . . ? B7 B13 B10 61.2(5) . . ? B12 B13 B10 60.6(5) . . ? B8 B13 B11 58.0(5) . . ? B7 B13 B11 106.3(6) . . ? B12 B13 B11 60.3(5) . . ? B10 B13 B11 103.2(6) . . ? B8 B13 H13 124(3) . . ? B7 B13 H13 127(3) . . ? B12 B13 H13 113(3) . . ? B10 B13 H13 128(3) . . ? B11 B13 H13 118(3) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C61 H61A 109.5 . . ? C6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C42 N41 C52 118.9(6) . . ? C42 N41 Sn4 121.1(5) . . ? C52 N41 Sn4 120.0(5) . . ? C74 N42 C53 119.0(7) . . ? C74 N42 Sn4 119.7(5) . . ? C53 N42 Sn4 120.9(5) . . ? N41 C42 C43 123.0(7) . . ? N41 C42 H42 118.5 . . ? C43 C42 H42 118.5 . . ? C42 C43 C44 120.1(7) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C51 C44 C43 117.1(6) . . ? C51 C44 C45 122.0(6) . . ? C43 C44 C45 120.9(6) . . ? C50 C45 C46 117.6(7) . . ? C50 C45 C44 121.5(6) . . ? C46 C45 C44 120.9(6) . . ? C47 C46 C45 120.2(7) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C46 C47 C48 121.6(8) . . ? C46 C47 H47 119.2 . . ? C48 C47 H47 119.2 . . ? C49 C48 C47 119.2(7) . . ? C49 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? C48 C49 C50 119.9(7) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C49 C50 C45 121.6(7) . . ? C49 C50 H50 119.2 . . ? C45 C50 H50 119.2 . . ? C44 C51 C52 119.9(6) . . ? C44 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? N41 C52 C51 120.8(6) . . ? N41 C52 C53 115.8(6) . . ? C51 C52 C53 123.4(6) . . ? N42 C53 C54 120.6(7) . . ? N42 C53 C52 114.4(6) . . ? C54 C53 C52 124.9(6) . . ? C53 C54 C55 120.6(6) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C73 C55 C54 116.0(6) . . ? C73 C55 C56 121.3(6) . . ? C54 C55 C56 122.6(6) . . ? C57 C56 C71 116.6(7) . . ? C57 C56 C55 123.3(6) . . ? C71 C56 C55 120.0(7) . . ? C58 C57 C56 121.8(6) . . ? C58 C57 H57 119.1 . . ? C56 C57 H57 119.1 . . ? C57 C58 C59 119.3(7) . . ? C57 C58 H58 120.4 . . ? C59 C58 H58 120.4 . . ? C72 C59 C58 120.5(7) . . ? C72 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C72 C71 C56 121.1(8) . . ? C72 C71 H71 119.4 . . ? C56 C71 H71 119.4 . . ? C71 C72 C59 120.6(7) . . ? C71 C72 H72 119.7 . . ? C59 C72 H72 119.7 . . ? C74 C73 C55 121.0(7) . . ? C74 C73 H73 119.5 . . ? C55 C73 H73 119.5 . . ? N42 C74 C73 122.5(7) . . ? N42 C74 H74 118.7 . . ? C73 C74 H74 118.7 . . ? Cl1 C021 Cl2 112.0(4) . . ? Cl1 C021 H02A 109.2 . . ? Cl2 C021 H02A 109.2 . . ? Cl1 C021 H02B 109.2 . . ? Cl2 C021 H02B 109.2 . . ? H02A C021 H02B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C1 B2 C6 -167.3(7) . . . . ? B3 C1 B2 C6 22.3(11) . . . . ? B5 C1 B2 C6 76.9(7) . . . . ? C11 C1 B2 B9 126.4(7) . . . . ? B3 C1 B2 B9 -44.0(10) . . . . ? B5 C1 B2 B9 10.6(6) . . . . ? C11 C1 B2 B5 115.8(7) . . . . ? B3 C1 B2 B5 -54.6(7) . . . . ? C11 C1 B3 B8 -135.8(7) . . . . ? B2 C1 B3 B8 34.4(10) . . . . ? B5 C1 B3 B8 -22.5(6) . . . . ? C11 C1 B3 B7 158.7(6) . . . . ? B2 C1 B3 B7 -31.1(10) . . . . ? B5 C1 B3 B7 -88.0(6) . . . . ? C11 C1 B3 B5 -113.3(7) . . . . ? B2 C1 B3 B5 56.9(7) . . . . ? C11 C1 B5 B11 -175.5(7) . . . . ? B3 C1 B5 B11 71.9(8) . . . . ? B2 C1 B5 B11 -62.7(8) . . . . ? C11 C1 B5 B8 131.4(6) . . . . ? B3 C1 B5 B8 18.8(5) . . . . ? B2 C1 B5 B8 -115.9(6) . . . . ? C11 C1 B5 B9 -122.2(6) . . . . ? B3 C1 B5 B9 125.2(6) . . . . ? B2 C1 B5 B9 -9.5(5) . . . . ? C11 C1 B5 B3 112.6(7) . . . . ? B2 C1 B5 B3 -134.6(6) . . . . ? C11 C1 B5 B2 -112.8(7) . . . . ? B3 C1 B5 B2 134.6(6) . . . . ? B8 B3 B5 C1 157.3(6) . . . . ? B7 B3 B5 C1 113.6(6) . . . . ? C1 B3 B5 B11 -134.0(6) . . . . ? B8 B3 B5 B11 23.3(5) . . . . ? B7 B3 B5 B11 -20.4(7) . . . . ? C1 B3 B5 B8 -157.3(6) . . . . ? B7 B3 B5 B8 -43.7(5) . . . . ? C1 B3 B5 B9 -73.6(7) . . . . ? B8 B3 B5 B9 83.7(7) . . . . ? B7 B3 B5 B9 40.1(8) . . . . ? C1 B3 B5 B2 -31.2(4) . . . . ? B8 B3 B5 B2 126.1(5) . . . . ? B7 B3 B5 B2 82.4(6) . . . . ? C6 B2 B5 C1 -124.9(6) . . . . ? B9 B2 B5 C1 -168.6(6) . . . . ? C1 B2 B5 B11 138.6(6) . . . . ? C6 B2 B5 B11 13.7(6) . . . . ? B9 B2 B5 B11 -30.0(5) . . . . ? C1 B2 B5 B8 79.6(6) . . . . ? C6 B2 B5 B8 -45.2(7) . . . . ? B9 B2 B5 B8 -89.0(6) . . . . ? C1 B2 B5 B9 168.6(6) . . . . ? C6 B2 B5 B9 43.8(5) . . . . ? C1 B2 B5 B3 32.2(5) . . . . ? C6 B2 B5 B3 -92.6(5) . . . . ? B9 B2 B5 B3 -136.4(5) . . . . ? C1 B2 C6 C61 146.3(7) . . . . ? B9 B2 C6 C61 -114.0(7) . . . . ? B5 B2 C6 C61 -157.8(5) . . . . ? C1 B2 C6 B10 6.0(10) . . . . ? B9 B2 C6 B10 105.7(7) . . . . ? B5 B2 C6 B10 61.9(7) . . . . ? C1 B2 C6 B12 -71.7(10) . . . . ? B9 B2 C6 B12 28.0(6) . . . . ? B5 B2 C6 B12 -15.8(8) . . . . ? C1 B2 C6 B9 -99.7(8) . . . . ? B5 B2 C6 B9 -43.8(5) . . . . ? C1 B3 B7 B8 108.1(7) . . . . ? B5 B3 B7 B8 45.6(5) . . . . ? C1 B3 B7 B13 80.0(9) . . . . ? B8 B3 B7 B13 -28.1(6) . . . . ? B5 B3 B7 B13 17.5(8) . . . . ? C1 B3 B7 B10 14.0(9) . . . . ? B8 B3 B7 B10 -94.1(7) . . . . ? B5 B3 B7 B10 -48.6(7) . . . . ? C1 B3 B7 Sn4 -48.1(6) . . . . ? B8 B3 B7 Sn4 -156.2(5) . . . . ? B5 B3 B7 Sn4 -110.7(4) . . . . ? N42 Sn4 B7 B8 -103.0(8) . . . . ? N41 Sn4 B7 B8 -171.1(8) . . . . ? B10 Sn4 B7 B8 93.4(9) . . . . ? N42 Sn4 B7 B13 175.0(6) . . . . ? N41 Sn4 B7 B13 107.0(6) . . . . ? B10 Sn4 B7 B13 11.5(5) . . . . ? N42 Sn4 B7 B10 163.5(4) . . . . ? N41 Sn4 B7 B10 95.5(4) . . . . ? N42 Sn4 B7 B3 -76.5(4) . . . . ? N41 Sn4 B7 B3 -144.5(4) . . . . ? B10 Sn4 B7 B3 120.0(6) . . . . ? B13 B7 B8 B11 38.3(6) . . . . ? B10 B7 B8 B11 -3.9(8) . . . . ? B3 B7 B8 B11 -111.6(6) . . . . ? Sn4 B7 B8 B11 -80.6(8) . . . . ? B13 B7 B8 B3 149.9(6) . . . . ? B10 B7 B8 B3 107.7(7) . . . . ? Sn4 B7 B8 B3 30.9(7) . . . . ? B10 B7 B8 B13 -42.2(5) . . . . ? B3 B7 B8 B13 -149.9(6) . . . . ? Sn4 B7 B8 B13 -118.9(8) . . . . ? B13 B7 B8 B5 101.0(6) . . . . ? B10 B7 B8 B5 58.8(7) . . . . ? B3 B7 B8 B5 -48.9(5) . . . . ? Sn4 B7 B8 B5 -17.9(9) . . . . ? C1 B3 B8 B11 -3.7(10) . . . . ? B7 B3 B8 B11 100.6(7) . . . . ? B5 B3 B8 B11 -26.1(6) . . . . ? C1 B3 B8 B7 -104.2(7) . . . . ? B5 B3 B8 B7 -126.7(6) . . . . ? C1 B3 B8 B13 -74.9(8) . . . . ? B7 B3 B8 B13 29.4(6) . . . . ? B5 B3 B8 B13 -97.3(6) . . . . ? C1 B3 B8 B5 22.4(6) . . . . ? B7 B3 B8 B5 126.7(6) . . . . ? C1 B5 B8 B11 135.9(6) . . . . ? B9 B5 B8 B11 32.0(5) . . . . ? B3 B5 B8 B11 153.0(6) . . . . ? B2 B5 B8 B11 89.4(6) . . . . ? C1 B5 B8 B7 31.9(7) . . . . ? B11 B5 B8 B7 -104.1(7) . . . . ? B9 B5 B8 B7 -72.1(7) . . . . ? B3 B5 B8 B7 48.9(6) . . . . ? B2 B5 B8 B7 -14.7(8) . . . . ? C1 B5 B8 B3 -17.1(5) . . . . ? B11 B5 B8 B3 -153.0(6) . . . . ? B9 B5 B8 B3 -121.0(6) . . . . ? B2 B5 B8 B3 -63.6(6) . . . . ? C1 B5 B8 B13 95.3(6) . . . . ? B11 B5 B8 B13 -40.6(5) . . . . ? B9 B5 B8 B13 -8.6(7) . . . . ? B3 B5 B8 B13 112.4(6) . . . . ? B2 B5 B8 B13 48.7(8) . . . . ? C61 C6 B9 B12 -105.2(7) . . . . ? B10 C6 B9 B12 43.0(6) . . . . ? B2 C6 B9 B12 153.4(6) . . . . ? C61 C6 B9 B11 -147.3(7) . . . . ? B10 C6 B9 B11 0.9(8) . . . . ? B2 C6 B9 B11 111.3(6) . . . . ? B12 C6 B9 B11 -42.1(6) . . . . ? C61 C6 B9 B2 101.4(7) . . . . ? B10 C6 B9 B2 -110.4(7) . . . . ? B12 C6 B9 B2 -153.4(6) . . . . ? C61 C6 B9 B5 151.6(6) . . . . ? B10 C6 B9 B5 -60.2(7) . . . . ? B2 C6 B9 B5 50.2(5) . . . . ? B12 C6 B9 B5 -103.2(6) . . . . ? C1 B2 B9 C6 115.5(7) . . . . ? B5 B2 B9 C6 126.0(5) . . . . ? C1 B2 B9 B12 91.7(7) . . . . ? C6 B2 B9 B12 -23.8(5) . . . . ? B5 B2 B9 B12 102.2(6) . . . . ? C1 B2 B9 B11 23.4(9) . . . . ? C6 B2 B9 B11 -92.0(6) . . . . ? B5 B2 B9 B11 33.9(5) . . . . ? C1 B2 B9 B5 -10.5(6) . . . . ? C6 B2 B9 B5 -126.0(5) . . . . ? C1 B5 B9 C6 -35.4(6) . . . . ? B11 B5 B9 C6 100.5(6) . . . . ? B8 B5 B9 C6 68.5(6) . . . . ? B3 B5 B9 C6 11.5(8) . . . . ? B2 B5 B9 C6 -43.7(5) . . . . ? C1 B5 B9 B12 -95.8(6) . . . . ? B11 B5 B9 B12 40.1(6) . . . . ? B8 B5 B9 B12 8.0(7) . . . . ? B3 B5 B9 B12 -48.9(8) . . . . ? B2 B5 B9 B12 -104.2(6) . . . . ? C1 B5 B9 B11 -135.8(6) . . . . ? B8 B5 B9 B11 -32.0(5) . . . . ? B3 B5 B9 B11 -89.0(6) . . . . ? B2 B5 B9 B11 -144.2(5) . . . . ? C1 B5 B9 B2 8.4(5) . . . . ? B11 B5 B9 B2 144.2(5) . . . . ? B8 B5 B9 B2 112.2(5) . . . . ? B3 B5 B9 B2 55.2(6) . . . . ? C61 C6 B10 B13 140.0(7) . . . . ? B2 C6 B10 B13 -82.7(7) . . . . ? B12 C6 B10 B13 32.8(6) . . . . ? B9 C6 B10 B13 -8.5(8) . . . . ? C61 C6 B10 B12 107.2(7) . . . . ? B2 C6 B10 B12 -115.5(7) . . . . ? B9 C6 B10 B12 -41.3(6) . . . . ? C61 C6 B10 B7 -157.3(7) . . . . ? B2 C6 B10 B7 -20.0(10) . . . . ? B12 C6 B10 B7 95.5(7) . . . . ? B9 C6 B10 B7 54.1(9) . . . . ? C61 C6 B10 Sn4 -93.7(6) . . . . ? B2 C6 B10 Sn4 43.6(6) . . . . ? B12 C6 B10 Sn4 159.1(5) . . . . ? B9 C6 B10 Sn4 117.7(5) . . . . ? B8 B7 B10 C6 -51.1(9) . . . . ? B13 B7 B10 C6 -93.1(7) . . . . ? B3 B7 B10 C6 10.3(10) . . . . ? Sn4 B7 B10 C6 76.7(6) . . . . ? B8 B7 B10 B13 42.1(6) . . . . ? B3 B7 B10 B13 103.4(7) . . . . ? Sn4 B7 B10 B13 169.8(5) . . . . ? B8 B7 B10 B12 11.3(8) . . . . ? B13 B7 B10 B12 -30.8(6) . . . . ? B3 B7 B10 B12 72.7(8) . . . . ? Sn4 B7 B10 B12 139.1(5) . . . . ? B8 B7 B10 Sn4 -127.8(6) . . . . ? B13 B7 B10 Sn4 -169.8(5) . . . . ? B3 B7 B10 Sn4 -66.4(5) . . . . ? N42 Sn4 B10 C6 -141.6(4) . . . . ? N41 Sn4 B10 C6 155.6(4) . . . . ? B7 Sn4 B10 C6 -121.3(5) . . . . ? N42 Sn4 B10 B13 -30.8(7) . . . . ? N41 Sn4 B10 B13 -93.6(5) . . . . ? B7 Sn4 B10 B13 -10.5(5) . . . . ? N42 Sn4 B10 B12 -112.6(8) . . . . ? N41 Sn4 B10 B12 -175.4(8) . . . . ? B7 Sn4 B10 B12 -92.3(8) . . . . ? N42 Sn4 B10 B7 -20.3(5) . . . . ? N41 Sn4 B10 B7 -83.1(4) . . . . ? B7 B8 B11 B9 59.1(8) . . . . ? B3 B8 B11 B9 -11.5(9) . . . . ? B13 B8 B11 B9 96.5(7) . . . . ? B5 B8 B11 B9 -38.9(6) . . . . ? B7 B8 B11 B5 98.0(6) . . . . ? B3 B8 B11 B5 27.4(6) . . . . ? B13 B8 B11 B5 135.4(6) . . . . ? B7 B8 B11 B12 -4.9(8) . . . . ? B3 B8 B11 B12 -75.5(8) . . . . ? B13 B8 B11 B12 32.5(6) . . . . ? B5 B8 B11 B12 -102.9(6) . . . . ? B7 B8 B11 B13 -37.5(6) . . . . ? B3 B8 B11 B13 -108.0(7) . . . . ? B5 B8 B11 B13 -135.4(6) . . . . ? C6 B9 B11 B8 -57.7(8) . . . . ? B12 B9 B11 B8 -97.6(7) . . . . ? B2 B9 B11 B8 1.9(9) . . . . ? B5 B9 B11 B8 38.8(6) . . . . ? C6 B9 B11 B5 -96.5(6) . . . . ? B12 B9 B11 B5 -136.4(6) . . . . ? B2 B9 B11 B5 -36.9(6) . . . . ? C6 B9 B11 B12 39.9(5) . . . . ? B2 B9 B11 B12 99.5(7) . . . . ? B5 B9 B11 B12 136.4(6) . . . . ? C6 B9 B11 B13 7.1(8) . . . . ? B12 B9 B11 B13 -32.8(6) . . . . ? B2 B9 B11 B13 66.7(8) . . . . ? B5 B9 B11 B13 103.7(6) . . . . ? C1 B5 B11 B8 -70.8(8) . . . . ? B9 B5 B11 B8 -141.8(6) . . . . ? B3 B5 B11 B8 -22.9(5) . . . . ? B2 B5 B11 B8 -112.4(5) . . . . ? C1 B5 B11 B9 71.0(8) . . . . ? B8 B5 B11 B9 141.8(6) . . . . ? B3 B5 B11 B9 118.9(6) . . . . ? B2 B5 B11 B9 29.5(5) . . . . ? C1 B5 B11 B12 32.4(10) . . . . ? B8 B5 B11 B12 103.2(6) . . . . ? B9 B5 B11 B12 -38.6(5) . . . . ? B3 B5 B11 B12 80.3(6) . . . . ? B2 B5 B11 B12 -9.2(7) . . . . ? C1 B5 B11 B13 -30.7(10) . . . . ? B8 B5 B11 B13 40.1(5) . . . . ? B9 B5 B11 B13 -101.7(6) . . . . ? B3 B5 B11 B13 17.2(7) . . . . ? B2 B5 B11 B13 -72.2(6) . . . . ? C61 C6 B12 B9 111.4(7) . . . . ? B10 C6 B12 B9 -137.0(6) . . . . ? B2 C6 B12 B9 -29.0(7) . . . . ? C61 C6 B12 B13 -145.2(6) . . . . ? B10 C6 B12 B13 -33.6(6) . . . . ? B2 C6 B12 B13 74.4(8) . . . . ? B9 C6 B12 B13 103.4(7) . . . . ? C61 C6 B12 B11 151.4(6) . . . . ? B10 C6 B12 B11 -97.0(6) . . . . ? B2 C6 B12 B11 11.0(8) . . . . ? B9 C6 B12 B11 40.0(5) . . . . ? C61 C6 B12 B10 -111.6(7) . . . . ? B2 C6 B12 B10 108.1(7) . . . . ? B9 C6 B12 B10 137.0(6) . . . . ? B11 B9 B12 C6 133.3(6) . . . . ? B2 B9 B12 C6 23.3(5) . . . . ? B5 B9 B12 C6 94.9(6) . . . . ? C6 B9 B12 B13 -99.5(6) . . . . ? B11 B9 B12 B13 33.8(6) . . . . ? B2 B9 B12 B13 -76.3(7) . . . . ? B5 B9 B12 B13 -4.6(8) . . . . ? C6 B9 B12 B11 -133.3(6) . . . . ? B2 B9 B12 B11 -110.1(7) . . . . ? B5 B9 B12 B11 -38.4(5) . . . . ? C6 B9 B12 B10 -36.0(5) . . . . ? B11 B9 B12 B10 97.3(6) . . . . ? B2 B9 B12 B10 -12.8(8) . . . . ? B5 B9 B12 B10 58.9(7) . . . . ? B8 B11 B12 C6 70.0(7) . . . . ? B9 B11 B12 C6 -40.4(5) . . . . ? B5 B11 B12 C6 1.0(7) . . . . ? B13 B11 B12 C6 102.8(6) . . . . ? B8 B11 B12 B9 110.4(6) . . . . ? B5 B11 B12 B9 41.4(6) . . . . ? B13 B11 B12 B9 143.2(6) . . . . ? B8 B11 B12 B13 -32.8(6) . . . . ? B9 B11 B12 B13 -143.2(6) . . . . ? B5 B11 B12 B13 -101.8(6) . . . . ? B8 B11 B12 B10 11.5(7) . . . . ? B9 B11 B12 B10 -98.9(6) . . . . ? B5 B11 B12 B10 -57.5(7) . . . . ? B13 B11 B12 B10 44.3(5) . . . . ? B13 B10 B12 C6 -142.8(6) . . . . ? B7 B10 B12 C6 -112.2(7) . . . . ? Sn4 B10 B12 C6 -35.3(7) . . . . ? C6 B10 B12 B9 37.4(5) . . . . ? B13 B10 B12 B9 -105.3(6) . . . . ? B7 B10 B12 B9 -74.8(7) . . . . ? Sn4 B10 B12 B9 2.1(10) . . . . ? C6 B10 B12 B13 142.8(6) . . . . ? B7 B10 B12 B13 30.6(6) . . . . ? Sn4 B10 B12 B13 107.5(8) . . . . ? C6 B10 B12 B11 98.3(6) . . . . ? B13 B10 B12 B11 -44.4(5) . . . . ? B7 B10 B12 B11 -13.9(8) . . . . ? Sn4 B10 B12 B11 63.0(9) . . . . ? B11 B8 B13 B7 -139.0(7) . . . . ? B3 B8 B13 B7 -30.5(7) . . . . ? B5 B8 B13 B7 -99.8(7) . . . . ? B11 B8 B13 B12 -32.9(6) . . . . ? B7 B8 B13 B12 106.1(7) . . . . ? B3 B8 B13 B12 75.5(8) . . . . ? B5 B8 B13 B12 6.3(8) . . . . ? B11 B8 B13 B10 -96.5(6) . . . . ? B7 B8 B13 B10 42.5(6) . . . . ? B3 B8 B13 B10 12.0(8) . . . . ? B5 B8 B13 B10 -57.3(7) . . . . ? B7 B8 B13 B11 139.0(7) . . . . ? B3 B8 B13 B11 108.4(7) . . . . ? B5 B8 B13 B11 39.2(5) . . . . ? B10 B7 B13 B8 131.9(6) . . . . ? B3 B7 B13 B8 27.4(6) . . . . ? Sn4 B7 B13 B8 119.4(7) . . . . ? B8 B7 B13 B12 -99.6(7) . . . . ? B10 B7 B13 B12 32.3(6) . . . . ? B3 B7 B13 B12 -72.1(8) . . . . ? Sn4 B7 B13 B12 19.8(9) . . . . ? B8 B7 B13 B10 -131.9(6) . . . . ? B3 B7 B13 B10 -104.4(7) . . . . ? Sn4 B7 B13 B10 -12.5(6) . . . . ? B8 B7 B13 B11 -35.5(6) . . . . ? B10 B7 B13 B11 96.4(6) . . . . ? B3 B7 B13 B11 -8.0(9) . . . . ? Sn4 B7 B13 B11 83.9(7) . . . . ? C6 B12 B13 B8 -64.6(8) . . . . ? B9 B12 B13 B8 -1.1(8) . . . . ? B11 B12 B13 B8 32.1(6) . . . . ? B10 B12 B13 B8 -96.7(6) . . . . ? C6 B12 B13 B7 -0.4(8) . . . . ? B9 B12 B13 B7 63.1(8) . . . . ? B11 B12 B13 B7 96.2(7) . . . . ? B10 B12 B13 B7 -32.5(6) . . . . ? C6 B12 B13 B10 32.1(5) . . . . ? B9 B12 B13 B10 95.6(7) . . . . ? B11 B12 B13 B10 128.7(6) . . . . ? C6 B12 B13 B11 -96.6(6) . . . . ? B9 B12 B13 B11 -33.1(6) . . . . ? B10 B12 B13 B11 -128.7(6) . . . . ? C6 B10 B13 B8 72.0(7) . . . . ? B12 B10 B13 B8 104.1(6) . . . . ? B7 B10 B13 B8 -41.6(5) . . . . ? Sn4 B10 B13 B8 -30.2(7) . . . . ? C6 B10 B13 B7 113.6(6) . . . . ? B12 B10 B13 B7 145.7(6) . . . . ? Sn4 B10 B13 B7 11.3(5) . . . . ? C6 B10 B13 B12 -32.1(6) . . . . ? B7 B10 B13 B12 -145.7(6) . . . . ? Sn4 B10 B13 B12 -134.3(6) . . . . ? C6 B10 B13 B11 12.0(7) . . . . ? B12 B10 B13 B11 44.1(5) . . . . ? B7 B10 B13 B11 -101.5(6) . . . . ? Sn4 B10 B13 B11 -90.2(6) . . . . ? B9 B11 B13 B8 -111.2(7) . . . . ? B5 B11 B13 B8 -42.3(6) . . . . ? B12 B11 B13 B8 -143.8(6) . . . . ? B8 B11 B13 B7 36.1(6) . . . . ? B9 B11 B13 B7 -75.1(8) . . . . ? B5 B11 B13 B7 -6.2(8) . . . . ? B12 B11 B13 B7 -107.7(7) . . . . ? B8 B11 B13 B12 143.8(6) . . . . ? B9 B11 B13 B12 32.6(6) . . . . ? B5 B11 B13 B12 101.6(6) . . . . ? B8 B11 B13 B10 99.5(6) . . . . ? B9 B11 B13 B10 -11.7(8) . . . . ? B5 B11 B13 B10 57.3(7) . . . . ? B12 B11 B13 B10 -44.3(5) . . . . ? N42 Sn4 N41 C42 174.6(6) . . . . ? B7 Sn4 N41 C42 -99.4(6) . . . . ? B10 Sn4 N41 C42 -56.9(6) . . . . ? N42 Sn4 N41 C52 -7.9(5) . . . . ? B7 Sn4 N41 C52 78.1(6) . . . . ? B10 Sn4 N41 C52 120.7(6) . . . . ? N41 Sn4 N42 C74 -177.0(6) . . . . ? B7 Sn4 N42 C74 95.4(6) . . . . ? B10 Sn4 N42 C74 109.1(6) . . . . ? N41 Sn4 N42 C53 9.7(5) . . . . ? B7 Sn4 N42 C53 -77.9(6) . . . . ? B10 Sn4 N42 C53 -64.2(6) . . . . ? C52 N41 C42 C43 -2.8(11) . . . . ? Sn4 N41 C42 C43 174.7(5) . . . . ? N41 C42 C43 C44 -0.2(11) . . . . ? C42 C43 C44 C51 2.1(10) . . . . ? C42 C43 C44 C45 -176.8(6) . . . . ? C51 C44 C45 C50 23.5(10) . . . . ? C43 C44 C45 C50 -157.7(7) . . . . ? C51 C44 C45 C46 -155.6(7) . . . . ? C43 C44 C45 C46 23.2(10) . . . . ? C50 C45 C46 C47 0.7(11) . . . . ? C44 C45 C46 C47 179.9(7) . . . . ? C45 C46 C47 C48 0.5(12) . . . . ? C46 C47 C48 C49 -2.2(12) . . . . ? C47 C48 C49 C50 2.7(12) . . . . ? C48 C49 C50 C45 -1.5(12) . . . . ? C46 C45 C50 C49 -0.2(11) . . . . ? C44 C45 C50 C49 -179.3(7) . . . . ? C43 C44 C51 C52 -1.1(10) . . . . ? C45 C44 C51 C52 177.8(6) . . . . ? C42 N41 C52 C51 3.8(10) . . . . ? Sn4 N41 C52 C51 -173.8(5) . . . . ? C42 N41 C52 C53 -176.7(6) . . . . ? Sn4 N41 C52 C53 5.8(8) . . . . ? C44 C51 C52 N41 -1.8(10) . . . . ? C44 C51 C52 C53 178.6(6) . . . . ? C74 N42 C53 C54 -2.4(11) . . . . ? Sn4 N42 C53 C54 170.9(5) . . . . ? C74 N42 C53 C52 176.3(6) . . . . ? Sn4 N42 C53 C52 -10.4(8) . . . . ? N41 C52 C53 N42 2.8(9) . . . . ? C51 C52 C53 N42 -177.6(6) . . . . ? N41 C52 C53 C54 -178.5(7) . . . . ? C51 C52 C53 C54 1.0(11) . . . . ? N42 C53 C54 C55 -1.2(11) . . . . ? C52 C53 C54 C55 -179.7(6) . . . . ? C53 C54 C55 C73 4.5(10) . . . . ? C53 C54 C55 C56 -178.0(7) . . . . ? C73 C55 C56 C57 153.8(7) . . . . ? C54 C55 C56 C57 -23.5(11) . . . . ? C73 C55 C56 C71 -28.1(10) . . . . ? C54 C55 C56 C71 154.6(7) . . . . ? C71 C56 C57 C58 4.5(10) . . . . ? C55 C56 C57 C58 -177.4(7) . . . . ? C56 C57 C58 C59 -2.9(11) . . . . ? C57 C58 C59 C72 -0.3(11) . . . . ? C57 C56 C71 C72 -3.1(11) . . . . ? C55 C56 C71 C72 178.7(8) . . . . ? C56 C71 C72 C59 0.0(13) . . . . ? C58 C59 C72 C71 1.7(12) . . . . ? C54 C55 C73 C74 -4.5(10) . . . . ? C56 C55 C73 C74 178.0(7) . . . . ? C53 N42 C74 C73 2.5(11) . . . . ? Sn4 N42 C74 C73 -170.9(5) . . . . ? C55 C73 C74 N42 1.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.739 _refine_diff_density_min -1.667 _refine_diff_density_rms 0.198