# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Bluemel, Janet' _publ_contact_author_email bluemel@tamu.edu _publ_section_title ; New Linker Systems for Superior Immobilized Catalysts ; _publ_author_name J.Bluemel # Attachment '- bbe1_bbe2.cif' data_bbe1 _database_code_depnum_ccdc_archive 'CCDC 742605' #TrackingRef '- bbe1_bbe2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silane (1) ; _chemical_name_common 'Silane (1)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Br4 Si' _chemical_formula_weight 652.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 13.6296(1) _cell_length_b 13.6296(1) _cell_length_c 18.9768(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3525.24(5) _cell_formula_units_Z 6 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 6.909 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3387 _exptl_absorpt_correction_T_max 0.5450 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 13920 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_sigmaI/netI 0.045 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.11 _reflns_number_total 2791 _reflns_number_gt 2482 _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^)+(0.0536P)^2^+5.2188P] 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 constr _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 0.037(16) _refine_ls_number_reflns 2791 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Br1 Br 0.39842(6) 0.39323(6) 0.39210(4) 0.0562(2) Uani 1 1 d . . . Br2 Br 0.11710(5) -0.11095(6) 0.77413(4) 0.0508(2) Uani 1 1 d . . . Si1 Si 0.5000 0.0000 0.57905(12) 0.0257(5) Uani 1 2 d S . . C11 C 0.4643(4) 0.1082(4) 0.5238(3) 0.0288(13) Uani 1 1 d . . . C12 C 0.3899(5) 0.1713(5) 0.5425(4) 0.0430(17) Uani 1 1 d . . . H12 H 0.3513 0.1563 0.5828 0.052 Uiso 1 1 calc R . . C13 C 0.3687(5) 0.2577(5) 0.5039(4) 0.0501(19) Uani 1 1 d . . . H13 H 0.3183 0.3012 0.5186 0.060 Uiso 1 1 calc R . . C14 C 0.4241(4) 0.2769(5) 0.4439(4) 0.0365(15) Uani 1 1 d . . . C15 C 0.4974(5) 0.2157(5) 0.4225(4) 0.0468(19) Uani 1 1 d . . . H15 H 0.5340 0.2297 0.3811 0.056 Uiso 1 1 calc R . . C16 C 0.5178(5) 0.1319(5) 0.4625(4) 0.0423(17) Uani 1 1 d . . . H16 H 0.5693 0.0896 0.4479 0.051 Uiso 1 1 calc R . . C21 C 0.3927(4) -0.0353(4) 0.6352(3) 0.0232(12) Uani 1 1 d . . . C22 C 0.3593(4) 0.0265(4) 0.6900(3) 0.0291(14) Uani 1 1 d . . . H22 H 0.3940 0.0855 0.6992 0.035 Uiso 1 1 calc R . . C23 C 0.2791(4) 0.0047(4) 0.7302(3) 0.0296(13) Uani 1 1 d . . . H23 H 0.2577 0.0487 0.7659 0.036 Uiso 1 1 calc R . . C24 C 0.2298(4) -0.0818(4) 0.7183(3) 0.0284(13) Uani 1 1 d . . . C25 C 0.2594(5) -0.1460(5) 0.6664(3) 0.0374(16) Uani 1 1 d . . . H25 H 0.2248 -0.2055 0.6586 0.045 Uiso 1 1 calc R . . C26 C 0.3416(5) -0.1223(5) 0.6255(3) 0.0340(15) Uani 1 1 d . . . H26 H 0.3628 -0.1668 0.5901 0.041 Uiso 1 1 calc R . . Br3 Br 0.91019(7) 0.64027(6) 0.71867(5) 0.0661(3) Uani 1 1 d . . . Si2 Si 1.0000 1.0000 0.5000 0.0429(9) Uani 1 4 d S . . C31 C 0.9739(5) 0.8928(5) 0.5588(4) 0.0409(15) Uani 1 1 d . . . C32 C 1.0331(5) 0.8077(5) 0.5626(4) 0.0489(18) Uani 1 1 d . . . H32 H 1.0863 0.8020 0.5305 0.059 Uiso 1 1 calc R . . C33 C 1.0186(5) 0.7346(5) 0.6086(4) 0.0402(17) Uani 1 1 d . . . H33 H 1.0612 0.6795 0.6107 0.048 Uiso 1 1 calc R . . C34 C 0.9372(5) 0.7435(5) 0.6540(4) 0.0440(18) Uani 1 1 d . . . C35 C 0.8768(6) 0.8229(6) 0.6532(4) 0.057(2) Uani 1 1 d . . . H35 H 0.8229 0.8271 0.6848 0.069 Uiso 1 1 calc R . . C36 C 0.8954(6) 0.8982(6) 0.6049(4) 0.0532(18) Uani 1 1 d . . . H36 H 0.8535 0.9538 0.6037 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0416(5) 0.0475(5) 0.0795(6) 0.0330(4) -0.0018(4) 0.0013(4) Br2 0.0414(4) 0.0507(5) 0.0601(5) -0.0048(4) 0.0218(4) -0.0105(4) Si1 0.0246(12) 0.0241(12) 0.0284(13) 0.000 0.000 -0.0026(10) C11 0.024(3) 0.029(3) 0.033(3) -0.001(3) -0.005(3) -0.003(2) C12 0.041(4) 0.049(4) 0.040(4) 0.014(3) 0.010(3) 0.010(3) C13 0.052(4) 0.041(4) 0.057(5) 0.014(4) 0.010(4) 0.018(3) C14 0.027(3) 0.035(3) 0.047(4) 0.017(3) -0.004(3) -0.003(3) C15 0.047(4) 0.050(5) 0.043(5) 0.007(3) 0.016(3) 0.000(4) C16 0.046(4) 0.039(4) 0.042(4) 0.008(3) 0.011(3) 0.016(3) C21 0.024(3) 0.021(3) 0.025(3) 0.006(2) -0.009(2) -0.005(2) C22 0.030(3) 0.025(3) 0.032(3) -0.005(3) -0.010(3) -0.005(3) C23 0.028(3) 0.032(3) 0.029(3) -0.002(3) -0.001(3) 0.001(3) C24 0.020(3) 0.030(3) 0.036(3) 0.000(3) -0.001(3) 0.001(2) C25 0.037(4) 0.030(3) 0.045(4) -0.004(3) 0.009(3) -0.007(3) C26 0.037(4) 0.031(3) 0.034(4) -0.006(3) -0.003(3) 0.005(3) Br3 0.0671(5) 0.0602(5) 0.0709(6) 0.0206(5) -0.0092(5) -0.0071(4) Si2 0.0408(13) 0.0408(13) 0.047(2) 0.000 0.000 0.000 C31 0.038(4) 0.041(4) 0.044(4) -0.005(3) -0.002(3) 0.005(3) C32 0.039(4) 0.052(4) 0.056(5) -0.009(4) -0.007(4) 0.008(3) C33 0.032(4) 0.025(3) 0.064(5) -0.004(3) -0.010(3) 0.000(3) C34 0.048(4) 0.036(4) 0.049(4) -0.003(3) -0.010(3) -0.010(3) C35 0.067(5) 0.052(5) 0.053(5) 0.005(4) 0.011(4) 0.002(4) C36 0.058(5) 0.045(5) 0.057(5) 0.005(4) 0.015(4) 0.015(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 Br1 C14 1.897(6) . ? Br2 C24 1.907(6) . ? Si1 C21 1.873(6) . ? Si1 C21 1.873(6) 2_655 ? Si1 C11 1.874(6) 2_655 ? Si1 C11 1.874(6) . ? C11 C12 1.376(9) . ? C11 C16 1.410(9) . ? C12 C13 1.417(9) . ? C12 H12 0.9500 . ? C13 C14 1.392(10) . ? C13 H13 0.9500 . ? C14 C15 1.363(10) . ? C15 C16 1.400(10) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.387(8) . ? C21 C22 1.412(9) . ? C22 C23 1.366(9) . ? C22 H22 0.9500 . ? C23 C24 1.377(8) . ? C23 H23 0.9500 . ? C24 C25 1.378(9) . ? C25 C26 1.401(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? Br3 C34 1.903(7) . ? Si2 C31 1.873(7) 3_576 ? Si2 C31 1.873(7) 4_756 ? Si2 C31 1.873(7) 2_775 ? Si2 C31 1.873(7) . ? C31 C36 1.384(10) . ? C31 C32 1.415(10) . ? C32 C33 1.339(11) . ? C32 H32 0.9500 . ? C33 C34 1.410(10) . ? C33 H33 0.9500 . ? C34 C35 1.360(11) . ? C35 C36 1.399(11) . ? C35 H35 0.9500 . ? C36 H36 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 C21 Si1 C21 110.6(4) . 2_655 ? C21 Si1 C11 108.6(3) . 2_655 ? C21 Si1 C11 108.5(2) 2_655 2_655 ? C21 Si1 C11 108.5(2) . . ? C21 Si1 C11 108.6(3) 2_655 . ? C11 Si1 C11 112.0(4) 2_655 . ? C12 C11 C16 116.8(6) . . ? C12 C11 Si1 122.6(5) . . ? C16 C11 Si1 120.5(5) . . ? C11 C12 C13 122.4(6) . . ? C11 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C14 C13 C12 118.0(6) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? C15 C14 C13 121.7(6) . . ? C15 C14 Br1 119.5(5) . . ? C13 C14 Br1 118.8(5) . . ? C14 C15 C16 119.0(6) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C15 C16 C11 122.1(6) . . ? C15 C16 H16 118.9 . . ? C11 C16 H16 118.9 . . ? C26 C21 C22 116.5(5) . . ? C26 C21 Si1 122.4(5) . . ? C22 C21 Si1 121.2(4) . . ? C23 C22 C21 122.7(5) . . ? C23 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? C22 C23 C24 119.0(6) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C25 121.2(6) . . ? C23 C24 Br2 118.7(5) . . ? C25 C24 Br2 120.1(4) . . ? C24 C25 C26 119.0(6) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C21 C26 C25 121.7(6) . . ? C21 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C31 Si2 C31 106.8(4) 3_576 4_756 ? C31 Si2 C31 110.8(2) 3_576 2_775 ? C31 Si2 C31 110.8(2) 4_756 2_775 ? C31 Si2 C31 110.8(2) 3_576 . ? C31 Si2 C31 110.8(2) 4_756 . ? C31 Si2 C31 106.8(4) 2_775 . ? C36 C31 C32 116.9(7) . . ? C36 C31 Si2 118.8(5) . . ? C32 C31 Si2 124.2(6) . . ? C33 C32 C31 124.0(7) . . ? C33 C32 H32 118.0 . . ? C31 C32 H32 118.0 . . ? C32 C33 C34 116.8(6) . . ? C32 C33 H33 121.6 . . ? C34 C33 H33 121.6 . . ? C35 C34 C33 122.5(7) . . ? C35 C34 Br3 118.6(6) . . ? C33 C34 Br3 118.9(5) . . ? C34 C35 C36 118.8(8) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C31 C36 C35 121.0(7) . . ? C31 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? 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 C21 Si1 C11 C12 23.3(7) . . . . ? C21 Si1 C11 C12 -97.0(6) 2_655 . . . ? C11 Si1 C11 C12 143.2(7) 2_655 . . . ? C21 Si1 C11 C16 -160.6(5) . . . . ? C21 Si1 C11 C16 79.1(6) 2_655 . . . ? C11 Si1 C11 C16 -40.7(5) 2_655 . . . ? C16 C11 C12 C13 -1.8(11) . . . . ? Si1 C11 C12 C13 174.4(6) . . . . ? C11 C12 C13 C14 1.9(11) . . . . ? C12 C13 C14 C15 -0.7(11) . . . . ? C12 C13 C14 Br1 -179.1(6) . . . . ? C13 C14 C15 C16 -0.5(11) . . . . ? Br1 C14 C15 C16 177.8(6) . . . . ? C14 C15 C16 C11 0.6(11) . . . . ? C12 C11 C16 C15 0.6(10) . . . . ? Si1 C11 C16 C15 -175.8(6) . . . . ? C21 Si1 C21 C26 -129.2(6) 2_655 . . . ? C11 Si1 C21 C26 -10.2(6) 2_655 . . . ? C11 Si1 C21 C26 111.8(5) . . . . ? C21 Si1 C21 C22 51.2(4) 2_655 . . . ? C11 Si1 C21 C22 170.2(5) 2_655 . . . ? C11 Si1 C21 C22 -67.8(5) . . . . ? C26 C21 C22 C23 -2.2(9) . . . . ? Si1 C21 C22 C23 177.5(4) . . . . ? C21 C22 C23 C24 1.5(9) . . . . ? C22 C23 C24 C25 -0.5(9) . . . . ? C22 C23 C24 Br2 -179.4(4) . . . . ? C23 C24 C25 C26 0.2(9) . . . . ? Br2 C24 C25 C26 179.0(5) . . . . ? C22 C21 C26 C25 1.8(9) . . . . ? Si1 C21 C26 C25 -177.9(5) . . . . ? C24 C25 C26 C21 -0.9(10) . . . . ? C31 Si2 C31 C36 -60.1(5) 3_576 . . . ? C31 Si2 C31 C36 -178.5(6) 4_756 . . . ? C31 Si2 C31 C36 60.7(6) 2_775 . . . ? C31 Si2 C31 C32 123.9(8) 3_576 . . . ? C31 Si2 C31 C32 5.5(6) 4_756 . . . ? C31 Si2 C31 C32 -115.3(7) 2_775 . . . ? C36 C31 C32 C33 -1.6(11) . . . . ? Si2 C31 C32 C33 174.5(6) . . . . ? C31 C32 C33 C34 2.1(11) . . . . ? C32 C33 C34 C35 -1.7(11) . . . . ? C32 C33 C34 Br3 178.1(5) . . . . ? C33 C34 C35 C36 0.9(12) . . . . ? Br3 C34 C35 C36 -179.0(6) . . . . ? C32 C31 C36 C35 0.6(11) . . . . ? Si2 C31 C36 C35 -175.7(6) . . . . ? C34 C35 C36 C31 -0.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.11 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.494 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.091 ###END data_bbe2 _database_code_depnum_ccdc_archive 'CCDC 742606' #TrackingRef '- bbe1_bbe2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Stannane (2) ; _chemical_name_common 'Stannane (2)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Br4 Sn' _chemical_formula_weight 742.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7752(6) _cell_length_b 11.2894(6) _cell_length_c 11.8628(7) _cell_angle_alpha 70.695(1) _cell_angle_beta 74.850(1) _cell_angle_gamma 79.261(2) _cell_volume 1185.4(1) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 7.828 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2552 _exptl_absorpt_correction_T_max 0.7448 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 8197 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 22.46 _reflns_number_total 3093 _reflns_number_gt 2361 _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^)+(0.0628P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3093 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Sn1 Sn 0.25200(6) 0.89698(5) 0.84794(5) 0.0354(2) Uani 1 1 d . . . Br1 Br 0.73039(11) 0.59555(9) 0.47164(8) 0.0589(3) Uani 1 1 d . . . Br2 Br -0.28166(10) 1.19121(10) 0.54565(9) 0.0566(3) Uani 1 1 d . . . Br3 Br 0.37513(10) 1.37739(9) 1.01908(9) 0.0574(3) Uani 1 1 d . . . Br4 Br -0.01243(12) 0.40033(9) 1.31789(9) 0.0640(3) Uani 1 1 d . . . C11 C 0.4124(8) 0.8060(7) 0.7331(7) 0.035(2) Uani 1 1 d . . . C12 C 0.3978(9) 0.6853(8) 0.7374(8) 0.047(2) Uani 1 1 d . . . H12 H 0.3210 0.6437 0.7950 0.057 Uiso 1 1 calc R . . C13 C 0.4920(10) 0.6223(8) 0.6602(8) 0.048(2) Uani 1 1 d . . . H13 H 0.4790 0.5394 0.6650 0.058 Uiso 1 1 calc R . . C14 C 0.6045(8) 0.6817(8) 0.5765(7) 0.040(2) Uani 1 1 d . . . C15 C 0.6223(9) 0.8014(9) 0.5690(8) 0.047(2) Uani 1 1 d . . . H15 H 0.6999 0.8420 0.5116 0.057 Uiso 1 1 calc R . . C16 C 0.5255(9) 0.8645(8) 0.6465(8) 0.044(2) Uani 1 1 d . . . H16 H 0.5373 0.9483 0.6398 0.052 Uiso 1 1 calc R . . C21 C 0.0881(8) 0.9932(7) 0.7495(7) 0.035(2) Uani 1 1 d . . . C22 C 0.0203(9) 0.9266(8) 0.7030(7) 0.043(2) Uani 1 1 d . . . H22 H 0.0506 0.8394 0.7131 0.052 Uiso 1 1 calc R . . C23 C -0.0881(8) 0.9830(8) 0.6436(7) 0.036(2) Uani 1 1 d . . . H23 H -0.1346 0.9355 0.6150 0.043 Uiso 1 1 calc R . . C24 C -0.1284(8) 1.1101(8) 0.6263(7) 0.038(2) Uani 1 1 d . . . C25 C -0.0631(8) 1.1809(8) 0.6657(7) 0.037(2) Uani 1 1 d . . . H25 H -0.0904 1.2691 0.6498 0.045 Uiso 1 1 calc R . . C26 C 0.0445(8) 1.1218(8) 0.7298(7) 0.037(2) Uani 1 1 d . . . H26 H 0.0882 1.1696 0.7603 0.044 Uiso 1 1 calc R . . C31 C 0.3192(8) 1.0343(8) 0.9031(7) 0.036(2) Uani 1 1 d . . . C32 C 0.3720(8) 1.1417(8) 0.8188(7) 0.038(2) Uani 1 1 d . . . H32 H 0.3923 1.1463 0.7347 0.045 Uiso 1 1 calc R . . C33 C 0.3972(9) 1.2414(8) 0.8478(8) 0.045(2) Uani 1 1 d . . . H33 H 0.4357 1.3129 0.7867 0.054 Uiso 1 1 calc R . . C34 C 0.3637(8) 1.2336(8) 0.9711(8) 0.038(2) Uani 1 1 d . . . C35 C 0.3181(8) 1.1266(9) 1.0603(8) 0.043(2) Uani 1 1 d . . . H35 H 0.3027 1.1205 1.1444 0.052 Uiso 1 1 calc R . . C36 C 0.2950(8) 1.0281(8) 1.0253(7) 0.040(2) Uani 1 1 d . . . H36 H 0.2617 0.9544 1.0864 0.048 Uiso 1 1 calc R . . C41 C 0.1640(8) 0.7468(7) 1.0012(7) 0.0341(19) Uani 1 1 d . . . C42 C 0.0362(9) 0.7084(8) 1.0060(8) 0.048(2) Uani 1 1 d . . . H42 H -0.0158 0.7523 0.9442 0.057 Uiso 1 1 calc R . . C43 C -0.0171(9) 0.6057(9) 1.1009(8) 0.050(2) Uani 1 1 d . . . H43 H -0.1057 0.5796 1.1050 0.060 Uiso 1 1 calc R . . C44 C 0.0606(9) 0.5427(7) 1.1884(7) 0.038(2) Uani 1 1 d . . . C45 C 0.1842(9) 0.5792(8) 1.1884(7) 0.040(2) Uani 1 1 d . . . H45 H 0.2343 0.5354 1.2515 0.048 Uiso 1 1 calc R . . C46 C 0.2368(9) 0.6821(8) 1.0939(7) 0.041(2) Uani 1 1 d . . . H46 H 0.3240 0.7087 1.0927 0.049 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 Sn1 0.0291(3) 0.0361(4) 0.0351(4) -0.0070(3) -0.0022(2) -0.0029(3) Br1 0.0623(7) 0.0586(7) 0.0461(6) -0.0199(5) 0.0007(5) 0.0071(5) Br2 0.0400(6) 0.0685(7) 0.0499(6) 0.0000(5) -0.0140(5) -0.0047(5) Br3 0.0530(6) 0.0552(7) 0.0732(7) -0.0316(6) -0.0165(5) -0.0006(5) Br4 0.0810(8) 0.0410(6) 0.0527(6) -0.0058(5) 0.0117(5) -0.0172(5) C11 0.033(5) 0.029(5) 0.036(5) -0.004(4) -0.012(4) 0.006(4) C12 0.038(5) 0.042(6) 0.052(6) -0.010(5) 0.003(4) -0.005(4) C13 0.064(7) 0.036(5) 0.045(6) -0.011(4) -0.014(5) -0.005(5) C14 0.027(5) 0.044(6) 0.037(5) -0.003(4) -0.003(4) 0.004(4) C15 0.031(5) 0.052(6) 0.045(6) -0.005(5) 0.004(4) -0.003(4) C16 0.048(6) 0.032(5) 0.051(6) -0.013(4) -0.006(5) -0.010(4) C21 0.030(5) 0.039(5) 0.034(5) -0.014(4) 0.000(4) 0.002(4) C22 0.051(6) 0.032(5) 0.046(5) -0.014(4) -0.006(5) -0.005(4) C23 0.038(5) 0.039(5) 0.030(5) -0.004(4) -0.008(4) -0.012(4) C24 0.025(5) 0.050(6) 0.029(5) -0.002(4) 0.001(4) -0.007(4) C25 0.035(5) 0.032(5) 0.044(5) -0.013(4) -0.009(4) 0.006(4) C26 0.036(5) 0.040(5) 0.034(5) -0.015(4) -0.002(4) -0.004(4) C31 0.023(4) 0.041(5) 0.036(5) -0.002(4) -0.008(4) -0.001(4) C32 0.037(5) 0.046(6) 0.027(5) -0.010(4) -0.004(4) -0.004(4) C33 0.043(5) 0.043(6) 0.043(6) -0.007(5) -0.004(4) -0.011(4) C34 0.022(4) 0.043(5) 0.043(6) -0.006(4) -0.007(4) -0.003(4) C35 0.032(5) 0.063(6) 0.031(5) -0.018(5) -0.001(4) 0.002(4) C36 0.029(5) 0.041(5) 0.041(6) -0.004(4) 0.002(4) -0.010(4) C41 0.024(5) 0.039(5) 0.037(5) -0.013(4) 0.000(4) -0.004(4) C42 0.045(6) 0.050(6) 0.038(5) -0.001(5) -0.010(4) -0.003(5) C43 0.030(5) 0.061(6) 0.057(6) -0.015(5) -0.003(5) -0.010(5) C44 0.041(5) 0.029(5) 0.035(5) -0.011(4) 0.009(4) -0.006(4) C45 0.044(5) 0.038(5) 0.032(5) -0.004(4) -0.008(4) -0.001(4) C46 0.033(5) 0.047(6) 0.039(5) -0.014(5) -0.007(4) 0.002(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 Sn1 C31 2.130(8) . ? Sn1 C11 2.140(8) . ? Sn1 C21 2.145(8) . ? Sn1 C41 2.146(8) . ? Br1 C14 1.888(8) . ? Br2 C24 1.913(8) . ? Br3 C34 1.919(8) . ? Br4 C44 1.917(8) . ? C11 C12 1.380(11) . ? C11 C16 1.393(11) . ? C12 C13 1.391(12) . ? C12 H12 0.9500 . ? C13 C14 1.382(11) . ? C13 H13 0.9500 . ? C14 C15 1.365(12) . ? C15 C16 1.405(12) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.393(11) . ? C21 C22 1.400(11) . ? C22 C23 1.366(11) . ? C22 H22 0.9500 . ? C23 C24 1.376(11) . ? C23 H23 0.9500 . ? C24 C25 1.362(11) . ? C25 C26 1.397(11) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C32 1.377(11) . ? C31 C36 1.386(11) . ? C32 C33 1.361(11) . ? C32 H32 0.9500 . ? C33 C34 1.389(11) . ? C33 H33 0.9500 . ? C34 C35 1.374(11) . ? C35 C36 1.382(11) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C42 1.379(11) . ? C41 C46 1.390(11) . ? C42 C43 1.393(12) . ? C42 H42 0.9500 . ? C43 C44 1.372(11) . ? C43 H43 0.9500 . ? C44 C45 1.346(11) . ? C45 C46 1.390(11) . ? C45 H45 0.9500 . ? C46 H46 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 C31 Sn1 C11 116.2(3) . . ? C31 Sn1 C21 106.5(3) . . ? C11 Sn1 C21 107.9(3) . . ? C31 Sn1 C41 112.2(3) . . ? C11 Sn1 C41 105.4(3) . . ? C21 Sn1 C41 108.3(3) . . ? C12 C11 C16 117.3(7) . . ? C12 C11 Sn1 118.4(6) . . ? C16 C11 Sn1 124.2(6) . . ? C11 C12 C13 122.2(8) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C14 C13 C12 119.4(8) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C15 C14 C13 120.2(8) . . ? C15 C14 Br1 120.9(6) . . ? C13 C14 Br1 118.8(7) . . ? C14 C15 C16 119.8(8) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 121.1(8) . . ? C11 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C26 C21 C22 117.6(7) . . ? C26 C21 Sn1 122.3(6) . . ? C22 C21 Sn1 120.1(6) . . ? C23 C22 C21 122.1(8) . . ? C23 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C22 C23 C24 118.5(7) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C25 C24 C23 122.1(7) . . ? C25 C24 Br2 118.4(6) . . ? C23 C24 Br2 119.5(6) . . ? C24 C25 C26 119.0(7) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C21 C26 C25 120.6(7) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C32 C31 C36 116.6(8) . . ? C32 C31 Sn1 121.4(6) . . ? C36 C31 Sn1 121.5(6) . . ? C33 C32 C31 124.4(8) . . ? C33 C32 H32 117.8 . . ? C31 C32 H32 117.8 . . ? C32 C33 C34 116.7(8) . . ? C32 C33 H33 121.6 . . ? C34 C33 H33 121.6 . . ? C35 C34 C33 121.8(8) . . ? C35 C34 Br3 118.6(6) . . ? C33 C34 Br3 119.5(6) . . ? C34 C35 C36 118.7(8) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C35 C36 C31 121.5(8) . . ? C35 C36 H36 119.2 . . ? C31 C36 H36 119.2 . . ? C42 C41 C46 118.6(8) . . ? C42 C41 Sn1 120.0(6) . . ? C46 C41 Sn1 121.4(6) . . ? C41 C42 C43 120.4(8) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 118.9(8) . . ? C44 C43 H43 120.6 . . ? C42 C43 H43 120.6 . . ? C45 C44 C43 122.5(8) . . ? C45 C44 Br4 118.9(6) . . ? C43 C44 Br4 118.6(7) . . ? C44 C45 C46 118.6(8) . . ? C44 C45 H45 120.7 . . ? C46 C45 H45 120.7 . . ? C45 C46 C41 121.1(8) . . ? C45 C46 H46 119.4 . . ? C41 C46 H46 119.4 . . ? 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 C31 Sn1 C11 C12 152.0(6) . . . . ? C21 Sn1 C11 C12 -88.5(7) . . . . ? C41 Sn1 C11 C12 27.1(7) . . . . ? C31 Sn1 C11 C16 -33.3(8) . . . . ? C21 Sn1 C11 C16 86.2(7) . . . . ? C41 Sn1 C11 C16 -158.3(7) . . . . ? C16 C11 C12 C13 0.7(13) . . . . ? Sn1 C11 C12 C13 175.7(6) . . . . ? C11 C12 C13 C14 0.3(13) . . . . ? C12 C13 C14 C15 -0.6(13) . . . . ? C12 C13 C14 Br1 -179.5(6) . . . . ? C13 C14 C15 C16 -0.2(13) . . . . ? Br1 C14 C15 C16 178.7(6) . . . . ? C12 C11 C16 C15 -1.4(12) . . . . ? Sn1 C11 C16 C15 -176.2(6) . . . . ? C14 C15 C16 C11 1.2(13) . . . . ? C31 Sn1 C21 C26 0.8(7) . . . . ? C11 Sn1 C21 C26 -124.7(6) . . . . ? C41 Sn1 C21 C26 121.7(6) . . . . ? C31 Sn1 C21 C22 -178.8(6) . . . . ? C11 Sn1 C21 C22 55.7(7) . . . . ? C41 Sn1 C21 C22 -57.9(7) . . . . ? C26 C21 C22 C23 -2.0(12) . . . . ? Sn1 C21 C22 C23 177.6(6) . . . . ? C21 C22 C23 C24 1.9(12) . . . . ? C22 C23 C24 C25 0.4(12) . . . . ? C22 C23 C24 Br2 -179.1(6) . . . . ? C23 C24 C25 C26 -2.5(12) . . . . ? Br2 C24 C25 C26 177.0(6) . . . . ? C22 C21 C26 C25 -0.1(11) . . . . ? Sn1 C21 C26 C25 -179.7(6) . . . . ? C24 C25 C26 C21 2.3(12) . . . . ? C11 Sn1 C31 C32 62.0(7) . . . . ? C21 Sn1 C31 C32 -58.3(7) . . . . ? C41 Sn1 C31 C32 -176.7(6) . . . . ? C11 Sn1 C31 C36 -126.4(6) . . . . ? C21 Sn1 C31 C36 113.3(6) . . . . ? C41 Sn1 C31 C36 -5.1(7) . . . . ? C36 C31 C32 C33 -2.1(12) . . . . ? Sn1 C31 C32 C33 169.9(6) . . . . ? C31 C32 C33 C34 -1.4(12) . . . . ? C32 C33 C34 C35 5.0(12) . . . . ? C32 C33 C34 Br3 -173.0(6) . . . . ? C33 C34 C35 C36 -4.9(12) . . . . ? Br3 C34 C35 C36 173.1(6) . . . . ? C34 C35 C36 C31 1.1(12) . . . . ? C32 C31 C36 C35 2.2(11) . . . . ? Sn1 C31 C36 C35 -169.8(6) . . . . ? C31 Sn1 C41 C42 132.3(6) . . . . ? C11 Sn1 C41 C42 -100.4(7) . . . . ? C21 Sn1 C41 C42 14.9(7) . . . . ? C31 Sn1 C41 C46 -51.1(7) . . . . ? C11 Sn1 C41 C46 76.3(7) . . . . ? C21 Sn1 C41 C46 -168.5(6) . . . . ? C46 C41 C42 C43 -1.0(12) . . . . ? Sn1 C41 C42 C43 175.7(7) . . . . ? C41 C42 C43 C44 -0.8(13) . . . . ? C42 C43 C44 C45 2.3(13) . . . . ? C42 C43 C44 Br4 -179.4(7) . . . . ? C43 C44 C45 C46 -2.0(13) . . . . ? Br4 C44 C45 C46 179.7(6) . . . . ? C44 C45 C46 C41 0.1(12) . . . . ? C42 C41 C46 C45 1.3(12) . . . . ? Sn1 C41 C46 C45 -175.3(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.46 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.456 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.149 ###END