# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ArNH2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H33 N' _chemical_formula_weight 467.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 5.7642(3) _cell_length_b 18.6519(9) _cell_length_c 24.6623(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.236(5) _cell_angle_gamma 90.00 _cell_volume 2650.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.989 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details 'Sortav, Blessing 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex X8' _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 11908 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4914 _reflns_number_gt 3732 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The two amino protons were located from difference maps and their positional and atomic displacement parameters refined isotropically. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+1.0947P] 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 4914 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 N1 N 0.0401(3) 0.66717(9) 0.23279(7) 0.0282(4) Uani 1 1 d . . . C1 C -0.1020(3) 0.72852(9) 0.23527(7) 0.0221(4) Uani 1 1 d . . . C2 C -0.1681(3) 0.76439(9) 0.18754(7) 0.0223(4) Uani 1 1 d . . . C3 C -0.3040(3) 0.82572(9) 0.19115(7) 0.0220(4) Uani 1 1 d . . . H3 H -0.3484 0.8502 0.1588 0.026 Uiso 1 1 calc R . . C4 C -0.3769(3) 0.85227(9) 0.24051(7) 0.0214(4) Uani 1 1 d . . . C5 C -0.3071(3) 0.81597(9) 0.28735(7) 0.0220(4) Uani 1 1 d . . . H5 H -0.3542 0.8337 0.3215 0.026 Uiso 1 1 calc R . . C6 C -0.1710(3) 0.75464(9) 0.28584(7) 0.0215(4) Uani 1 1 d . . . C7 C -0.0960(3) 0.73312(10) 0.13330(7) 0.0243(4) Uani 1 1 d . . . H7 H 0.0723 0.7209 0.1376 0.029 Uiso 1 1 calc R . . C8 C -0.1134(3) 0.78618(9) 0.08649(7) 0.0247(4) Uani 1 1 d . . . C9 C -0.3061(3) 0.78985(10) 0.05216(7) 0.0292(4) Uani 1 1 d . . . H9 H -0.4335 0.7587 0.0579 0.035 Uiso 1 1 calc R . . C10 C -0.3161(4) 0.83841(11) 0.00944(8) 0.0360(5) Uani 1 1 d . . . H10 H -0.4496 0.8401 -0.0138 0.043 Uiso 1 1 calc R . . C11 C -0.1329(4) 0.88403(11) 0.00071(8) 0.0386(5) Uani 1 1 d . . . H11 H -0.1395 0.9172 -0.0285 0.046 Uiso 1 1 calc R . . C12 C 0.0608(4) 0.88136(11) 0.03473(8) 0.0378(5) Uani 1 1 d . . . H12 H 0.1876 0.9127 0.0288 0.045 Uiso 1 1 calc R . . C13 C 0.0703(3) 0.83289(10) 0.07751(8) 0.0316(5) Uani 1 1 d . . . H13 H 0.2035 0.8316 0.1009 0.038 Uiso 1 1 calc R . . C14 C -0.2213(3) 0.66248(10) 0.12104(7) 0.0253(4) Uani 1 1 d . . . C15 C -0.4301(3) 0.64423(10) 0.14424(8) 0.0308(5) Uani 1 1 d . . . H15 H -0.5026 0.6772 0.1679 0.037 Uiso 1 1 calc R . . C16 C -0.5346(4) 0.57882(11) 0.13350(9) 0.0380(5) Uani 1 1 d . . . H16 H -0.6769 0.5672 0.1501 0.046 Uiso 1 1 calc R . . C17 C -0.4340(4) 0.53049(11) 0.09894(9) 0.0427(6) Uani 1 1 d . . . H17 H -0.5065 0.4857 0.0915 0.051 Uiso 1 1 calc R . . C18 C -0.2269(4) 0.54784(11) 0.07527(8) 0.0401(5) Uani 1 1 d . . . H18 H -0.1560 0.5148 0.0515 0.048 Uiso 1 1 calc R . . C19 C -0.1216(4) 0.61324(10) 0.08601(8) 0.0332(5) Uani 1 1 d . . . H19 H 0.0205 0.6247 0.0692 0.040 Uiso 1 1 calc R . . C20 C -0.0971(3) 0.71394(10) 0.33695(7) 0.0239(4) Uani 1 1 d . . . H20 H 0.0707 0.7020 0.3328 0.029 Uiso 1 1 calc R . . C21 C -0.2239(3) 0.64227(10) 0.34252(7) 0.0249(4) Uani 1 1 d . . . C22 C -0.1274(4) 0.58894(10) 0.37526(8) 0.0310(5) Uani 1 1 d . . . H22 H 0.0179 0.5971 0.3931 0.037 Uiso 1 1 calc R . . C23 C -0.2404(4) 0.52395(11) 0.38217(8) 0.0384(5) Uani 1 1 d . . . H23 H -0.1735 0.4882 0.4051 0.046 Uiso 1 1 calc R . . C24 C -0.4499(4) 0.51123(11) 0.35572(9) 0.0392(5) Uani 1 1 d . . . H24 H -0.5264 0.4665 0.3599 0.047 Uiso 1 1 calc R . . C25 C -0.5472(4) 0.56353(11) 0.32327(9) 0.0357(5) Uani 1 1 d . . . H25 H -0.6920 0.5549 0.3053 0.043 Uiso 1 1 calc R . . C26 C -0.4359(3) 0.62882(10) 0.31653(8) 0.0297(4) Uani 1 1 d . . . H26 H -0.5050 0.6646 0.2940 0.036 Uiso 1 1 calc R . . C27 C -0.1119(3) 0.75888(10) 0.38824(7) 0.0235(4) Uani 1 1 d . . . C28 C 0.0710(3) 0.80396(10) 0.40274(8) 0.0285(4) Uani 1 1 d . . . H28 H 0.2046 0.8056 0.3809 0.034 Uiso 1 1 calc R . . C29 C 0.0611(3) 0.84665(10) 0.44867(8) 0.0318(5) Uani 1 1 d . . . H29 H 0.1876 0.8771 0.4582 0.038 Uiso 1 1 calc R . . C30 C -0.1322(4) 0.84486(11) 0.48051(8) 0.0334(5) Uani 1 1 d . . . H30 H -0.1399 0.8745 0.5117 0.040 Uiso 1 1 calc R . . C31 C -0.3141(3) 0.80006(11) 0.46698(8) 0.0322(5) Uani 1 1 d . . . H31 H -0.4467 0.7985 0.4891 0.039 Uiso 1 1 calc R . . C32 C -0.3045(3) 0.75710(10) 0.42107(7) 0.0279(4) Uani 1 1 d . . . H32 H -0.4308 0.7263 0.4121 0.033 Uiso 1 1 calc R . . C33 C -0.5288(3) 0.91851(9) 0.24311(7) 0.0250(4) Uani 1 1 d . . . H33 H -0.5505 0.9369 0.2052 0.030 Uiso 1 1 calc R . . C34 C -0.7670(3) 0.90119(11) 0.26439(10) 0.0412(5) Uani 1 1 d . . . H34A H -0.8389 0.8635 0.2420 0.062 Uiso 1 1 calc R . . H34B H -0.8642 0.9443 0.2629 0.062 Uiso 1 1 calc R . . H34C H -0.7521 0.8846 0.3020 0.062 Uiso 1 1 calc R . . C35 C -0.4172(4) 0.97793(11) 0.27650(10) 0.0433(6) Uani 1 1 d . . . H35A H -0.3847 0.9606 0.3134 0.065 Uiso 1 1 calc R . . H35B H -0.5229 1.0190 0.2778 0.065 Uiso 1 1 calc R . . H35C H -0.2718 0.9926 0.2599 0.065 Uiso 1 1 calc R . . H1 H 0.020(3) 0.6366(11) 0.2606(9) 0.033(6) Uiso 1 1 d . . . H2 H 0.013(4) 0.6423(12) 0.2005(10) 0.046(6) Uiso 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 N1 0.0375(10) 0.0253(9) 0.0219(9) 0.0017(8) -0.0001(7) 0.0071(8) C1 0.0232(9) 0.0182(9) 0.0250(10) -0.0010(8) 0.0003(7) -0.0010(8) C2 0.0257(9) 0.0210(9) 0.0202(9) -0.0008(8) -0.0003(7) -0.0030(8) C3 0.0255(9) 0.0208(9) 0.0196(9) 0.0014(7) -0.0027(7) -0.0035(8) C4 0.0240(9) 0.0168(9) 0.0235(9) 0.0001(7) -0.0008(7) -0.0038(8) C5 0.0241(9) 0.0225(10) 0.0195(9) -0.0027(8) 0.0031(7) -0.0026(8) C6 0.0218(9) 0.0210(9) 0.0215(9) -0.0005(7) -0.0005(7) -0.0039(8) C7 0.0273(9) 0.0257(10) 0.0198(9) -0.0016(8) 0.0010(7) 0.0042(8) C8 0.0337(10) 0.0210(9) 0.0196(9) -0.0048(8) 0.0053(8) 0.0015(8) C9 0.0363(11) 0.0281(10) 0.0231(10) -0.0026(8) 0.0011(8) 0.0004(9) C10 0.0511(13) 0.0343(12) 0.0225(10) 0.0008(9) -0.0022(9) 0.0041(10) C11 0.0619(14) 0.0290(11) 0.0252(11) 0.0034(9) 0.0083(10) 0.0029(11) C12 0.0487(13) 0.0282(11) 0.0370(12) 0.0001(9) 0.0131(10) -0.0065(10) C13 0.0361(11) 0.0288(11) 0.0299(11) -0.0035(9) 0.0043(9) 0.0006(9) C14 0.0334(10) 0.0220(10) 0.0202(9) 0.0007(8) -0.0034(8) 0.0032(8) C15 0.0349(11) 0.0275(11) 0.0298(11) -0.0019(9) -0.0012(9) -0.0007(9) C16 0.0414(12) 0.0329(12) 0.0394(12) 0.0024(10) -0.0064(10) -0.0067(10) C17 0.0616(15) 0.0248(11) 0.0411(13) 0.0005(10) -0.0139(11) -0.0063(11) C18 0.0667(15) 0.0241(11) 0.0293(11) -0.0057(9) -0.0033(11) 0.0077(11) C19 0.0490(12) 0.0278(11) 0.0228(10) 0.0016(8) 0.0012(9) 0.0055(10) C20 0.0246(9) 0.0243(10) 0.0227(9) 0.0013(8) -0.0002(7) 0.0020(8) C21 0.0319(10) 0.0216(10) 0.0213(9) 0.0003(8) 0.0045(8) 0.0039(8) C22 0.0397(11) 0.0280(11) 0.0253(10) -0.0003(8) -0.0004(8) 0.0042(9) C23 0.0601(14) 0.0247(11) 0.0305(11) 0.0072(9) 0.0051(10) 0.0067(10) C24 0.0535(14) 0.0243(11) 0.0400(12) -0.0001(9) 0.0097(11) -0.0060(10) C25 0.0354(11) 0.0291(11) 0.0427(12) 0.0002(10) 0.0033(9) -0.0039(9) C26 0.0316(11) 0.0247(10) 0.0329(11) 0.0031(9) 0.0023(9) 0.0024(9) C27 0.0291(10) 0.0222(10) 0.0191(9) 0.0056(8) -0.0027(7) 0.0026(8) C28 0.0308(10) 0.0288(11) 0.0258(10) 0.0059(8) -0.0026(8) -0.0012(9) C29 0.0393(12) 0.0270(11) 0.0288(11) 0.0019(9) -0.0093(9) -0.0043(9) C30 0.0484(13) 0.0290(11) 0.0226(10) -0.0017(8) -0.0035(9) 0.0034(10) C31 0.0399(11) 0.0352(12) 0.0217(10) 0.0011(9) 0.0036(8) 0.0030(10) C32 0.0316(10) 0.0288(10) 0.0233(10) 0.0013(8) -0.0010(8) -0.0017(9) C33 0.0299(10) 0.0223(10) 0.0229(9) 0.0015(8) 0.0019(8) 0.0039(8) C34 0.0290(11) 0.0309(12) 0.0637(15) 0.0056(11) 0.0016(10) 0.0018(9) C35 0.0409(12) 0.0250(11) 0.0638(16) -0.0104(11) -0.0021(11) 0.0031(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 N1 C1 1.409(2) . ? C1 C2 1.400(2) . ? C1 C6 1.404(2) . ? C2 C3 1.391(2) . ? C2 C7 1.525(2) . ? C3 C4 1.388(2) . ? C4 C5 1.391(2) . ? C4 C33 1.516(2) . ? C5 C6 1.388(2) . ? C6 C20 1.524(2) . ? C7 C8 1.522(2) . ? C7 C14 1.530(3) . ? C8 C9 1.384(3) . ? C8 C13 1.392(3) . ? C9 C10 1.390(3) . ? C10 C11 1.377(3) . ? C11 C12 1.383(3) . ? C12 C13 1.390(3) . ? C14 C15 1.386(3) . ? C14 C19 1.394(3) . ? C15 C16 1.384(3) . ? C16 C17 1.377(3) . ? C17 C18 1.379(3) . ? C18 C19 1.385(3) . ? C20 C27 1.521(2) . ? C20 C21 1.531(3) . ? C21 C22 1.390(3) . ? C21 C26 1.390(3) . ? C22 C23 1.388(3) . ? C23 C24 1.381(3) . ? C24 C25 1.374(3) . ? C25 C26 1.388(3) . ? C27 C32 1.389(3) . ? C27 C28 1.389(3) . ? C28 C29 1.387(3) . ? C29 C30 1.377(3) . ? C30 C31 1.376(3) . ? C31 C32 1.389(3) . ? C33 C35 1.516(3) . ? C33 C34 1.516(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.26(16) . . ? C2 C1 N1 119.97(16) . . ? C6 C1 N1 119.75(16) . . ? C3 C2 C1 118.87(16) . . ? C3 C2 C7 122.36(15) . . ? C1 C2 C7 118.72(15) . . ? C4 C3 C2 122.10(16) . . ? C3 C4 C5 117.86(16) . . ? C3 C4 C33 120.91(16) . . ? C5 C4 C33 121.23(16) . . ? C6 C5 C4 122.16(16) . . ? C5 C6 C1 118.73(16) . . ? C5 C6 C20 122.42(16) . . ? C1 C6 C20 118.83(15) . . ? C8 C7 C2 113.70(14) . . ? C8 C7 C14 112.78(14) . . ? C2 C7 C14 111.48(15) . . ? C9 C8 C13 118.35(17) . . ? C9 C8 C7 122.34(17) . . ? C13 C8 C7 119.31(16) . . ? C8 C9 C10 121.06(19) . . ? C11 C10 C9 120.11(19) . . ? C10 C11 C12 119.66(19) . . ? C11 C12 C13 120.15(19) . . ? C12 C13 C8 120.66(19) . . ? C15 C14 C19 117.86(18) . . ? C15 C14 C7 122.72(16) . . ? C19 C14 C7 119.41(17) . . ? C16 C15 C14 121.05(19) . . ? C17 C16 C15 120.6(2) . . ? C16 C17 C18 119.2(2) . . ? C17 C18 C19 120.4(2) . . ? C18 C19 C14 120.9(2) . . ? C27 C20 C6 113.17(14) . . ? C27 C20 C21 111.78(14) . . ? C6 C20 C21 112.57(14) . . ? C22 C21 C26 118.40(17) . . ? C22 C21 C20 119.40(16) . . ? C26 C21 C20 122.19(16) . . ? C23 C22 C21 120.87(19) . . ? C24 C23 C22 120.00(19) . . ? C25 C24 C23 119.68(19) . . ? C24 C25 C26 120.57(19) . . ? C25 C26 C21 120.47(18) . . ? C32 C27 C28 118.44(17) . . ? C32 C27 C20 122.10(16) . . ? C28 C27 C20 119.46(16) . . ? C29 C28 C27 120.90(18) . . ? C30 C29 C28 119.98(18) . . ? C31 C30 C29 119.86(19) . . ? C30 C31 C32 120.31(19) . . ? C27 C32 C31 120.50(18) . . ? C35 C33 C34 110.17(17) . . ? C35 C33 C4 112.36(15) . . ? C34 C33 C4 111.66(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.229 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.038 _database_code_depnum_ccdc_archive 'CCDC 977193' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H119 N2 Si2 Sn2' _chemical_formula_weight 1618.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 15.2590(7) _cell_length_b 15.4261(8) _cell_length_c 20.5749(9) _cell_angle_alpha 88.697(2) _cell_angle_beta 83.069(2) _cell_angle_gamma 64.915(2) _cell_volume 4352.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'orange green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1698 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.821 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details 'Sortav, Blessing 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex X8' _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 40836 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.20 _reflns_number_total 15466 _reflns_number_gt 12854 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. A molecule of toluene of crystallisation was located in the crystal lattice and its carbon atoms were refined anisotropically. A molecule of hexane of crystallisation was located in the crystal lattice and its carbon atoms were refined isotropically at 50% occupancy. The C-C distances and C-C-C angles of the hexane molecule were restrained to reasonable values using the DFIX (1.52 ang.) and DANG (2.50 ang.) commands of SHELXL. The largest residual electron density peak in the final difference map (1.66 e-/ang.3) lies close (ca. 1.0 ang.) to Sn(1). ; _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^)+(0.0262P)^2^+28.8242P] 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 15466 _refine_ls_number_parameters 953 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1521 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.71763(2) 0.23059(2) 0.203179(16) 0.02058(8) Uani 1 1 d . . . Si1 Si 0.78679(9) 0.07660(10) 0.33610(7) 0.0218(3) Uani 1 1 d . . . N1 N 0.8116(3) 0.1286(3) 0.26397(19) 0.0182(9) Uani 1 1 d . . . C1 C 0.9111(3) 0.1009(3) 0.2363(2) 0.0179(11) Uani 1 1 d . . . Sn2 Sn 0.50706(2) 0.25849(2) 0.261836(17) 0.02074(8) Uani 1 1 d . . . Si2 Si 0.44690(9) 0.48850(10) 0.19895(7) 0.0227(3) Uani 1 1 d . . . N2 N 0.4185(3) 0.4029(3) 0.24242(19) 0.0194(9) Uani 1 1 d . . . C2 C 0.9540(3) 0.0285(3) 0.1864(2) 0.0190(11) Uani 1 1 d . . . C3 C 1.0517(3) -0.0012(3) 0.1614(2) 0.0223(12) Uani 1 1 d . . . H3 H 1.0795 -0.0499 0.1278 0.027 Uiso 1 1 calc R . . C4 C 1.1097(3) 0.0377(3) 0.1838(2) 0.0218(11) Uani 1 1 d . . . C5 C 1.0655(3) 0.1105(3) 0.2314(2) 0.0208(11) Uani 1 1 d . . . H5 H 1.1040 0.1383 0.2474 0.025 Uiso 1 1 calc R . . C6 C 0.9687(3) 0.1446(3) 0.2567(2) 0.0214(11) Uani 1 1 d . . . C7 C 1.2159(4) 0.0065(4) 0.1560(3) 0.0302(13) Uani 1 1 d . . . H7 H 1.2472 0.0287 0.1878 0.036 Uiso 1 1 calc R . . C8 C 1.2244(4) 0.0534(5) 0.0921(3) 0.0468(18) Uani 1 1 d . . . H8A H 1.1946 0.0327 0.0596 0.070 Uiso 1 1 calc R . . H8B H 1.2934 0.0348 0.0764 0.070 Uiso 1 1 calc R . . H8C H 1.1908 0.1231 0.0985 0.070 Uiso 1 1 calc R . . C9 C 1.2706(4) -0.1008(4) 0.1485(3) 0.0420(17) Uani 1 1 d . . . H9A H 1.2453 -0.1243 0.1146 0.063 Uiso 1 1 calc R . . H9B H 1.2620 -0.1299 0.1902 0.063 Uiso 1 1 calc R . . H9C H 1.3401 -0.1181 0.1357 0.063 Uiso 1 1 calc R . . C10 C 0.8920(3) -0.0133(3) 0.1575(3) 0.0231(12) Uani 1 1 d . . . H10 H 0.8443 -0.0159 0.1945 0.028 Uiso 1 1 calc R . . C11 C 0.8319(4) 0.0556(4) 0.1084(3) 0.0264(12) Uani 1 1 d . . . C12 C 0.7364(4) 0.0712(4) 0.1070(3) 0.0339(14) Uani 1 1 d . . . H12 H 0.7086 0.0390 0.1367 0.041 Uiso 1 1 calc R . . C13 C 0.6797(4) 0.1332(4) 0.0628(3) 0.0380(16) Uani 1 1 d . . . H13 H 0.6136 0.1440 0.0630 0.046 Uiso 1 1 calc R . . C14 C 0.7195(5) 0.1784(4) 0.0194(3) 0.0426(18) Uani 1 1 d . . . H14 H 0.6806 0.2222 -0.0100 0.051 Uiso 1 1 calc R . . C15 C 0.8164(4) 0.1607(4) 0.0181(3) 0.0358(15) Uani 1 1 d . . . H15 H 0.8446 0.1903 -0.0135 0.043 Uiso 1 1 calc R . . C16 C 0.8724(4) 0.1002(4) 0.0624(3) 0.0322(14) Uani 1 1 d . . . H16 H 0.9388 0.0889 0.0615 0.039 Uiso 1 1 calc R . . C17 C 0.9477(4) -0.1143(4) 0.1293(3) 0.0322(14) Uani 1 1 d . . . C18 C 0.9487(5) -0.1380(5) 0.0651(4) 0.0501(18) Uani 1 1 d . . . H18 H 0.9160 -0.0892 0.0361 0.060 Uiso 1 1 calc R . . C19 C 0.9971(6) -0.2330(5) 0.0421(4) 0.069(2) Uani 1 1 d . . . H19 H 0.9969 -0.2480 -0.0023 0.083 Uiso 1 1 calc R . . C20 C 1.0448(5) -0.3046(5) 0.0824(5) 0.069(3) Uani 1 1 d . . . H20 H 1.0775 -0.3691 0.0663 0.083 Uiso 1 1 calc R . . C21 C 1.0450(4) -0.2824(4) 0.1470(4) 0.053(2) Uani 1 1 d . . . H21 H 1.0775 -0.3315 0.1758 0.064 Uiso 1 1 calc R . . C22 C 0.9972(4) -0.1872(4) 0.1698(3) 0.0396(16) Uani 1 1 d . . . H22 H 0.9986 -0.1720 0.2140 0.047 Uiso 1 1 calc R . . C23 C 0.9222(3) 0.2357(3) 0.3005(2) 0.0181(11) Uani 1 1 d . . . H23 H 0.8608 0.2364 0.3244 0.022 Uiso 1 1 calc R . . C24 C 0.9831(3) 0.2418(3) 0.3529(2) 0.0219(11) Uani 1 1 d . . . C25 C 1.0596(4) 0.2668(4) 0.3387(3) 0.0310(14) Uani 1 1 d . . . H25 H 1.0766 0.2793 0.2947 0.037 Uiso 1 1 calc R . . C26 C 1.1125(4) 0.2741(4) 0.3867(3) 0.0309(13) Uani 1 1 d . . . H26 H 1.1653 0.2910 0.3754 0.037 Uiso 1 1 calc R . . C27 C 1.0891(4) 0.2571(4) 0.4503(3) 0.0353(14) Uani 1 1 d . . . H27 H 1.1257 0.2614 0.4833 0.042 Uiso 1 1 calc R . . C28 C 1.0108(4) 0.2335(4) 0.4662(3) 0.0354(14) Uani 1 1 d . . . H28 H 0.9932 0.2223 0.5104 0.042 Uiso 1 1 calc R . . C29 C 0.9586(4) 0.2263(4) 0.4176(3) 0.0282(13) Uani 1 1 d . . . H29 H 0.9050 0.2105 0.4289 0.034 Uiso 1 1 calc R . . C30 C 0.8916(3) 0.3259(4) 0.2592(2) 0.0239(12) Uani 1 1 d . . . C31 C 0.8492(4) 0.4153(4) 0.2902(3) 0.0309(13) Uani 1 1 d . . . H31 H 0.8409 0.4194 0.3367 0.037 Uiso 1 1 calc R . . C32 C 0.8186(4) 0.4986(4) 0.2559(3) 0.0345(14) Uani 1 1 d . . . H32 H 0.7900 0.5592 0.2784 0.041 Uiso 1 1 calc R . . C33 C 0.8299(4) 0.4931(4) 0.1882(3) 0.0396(15) Uani 1 1 d . . . H33 H 0.8099 0.5499 0.1639 0.047 Uiso 1 1 calc R . . C34 C 0.8704(5) 0.4051(4) 0.1564(3) 0.0423(16) Uani 1 1 d . . . H34 H 0.8770 0.4014 0.1099 0.051 Uiso 1 1 calc R . . C35 C 0.9017(4) 0.3214(4) 0.1914(3) 0.0338(14) Uani 1 1 d . . . H35 H 0.9302 0.2609 0.1688 0.041 Uiso 1 1 calc R . . C36 C 0.7599(4) -0.0298(4) 0.3188(3) 0.0292(13) Uani 1 1 d . . . H36 H 0.8145 -0.0719 0.2858 0.035 Uiso 1 1 calc R . . C37 C 0.7563(4) -0.0929(4) 0.3760(3) 0.0430(16) Uani 1 1 d . . . H37A H 0.7031 -0.0552 0.4097 0.064 Uiso 1 1 calc R . . H37B H 0.8183 -0.1175 0.3945 0.064 Uiso 1 1 calc R . . H37C H 0.7451 -0.1466 0.3607 0.064 Uiso 1 1 calc R . . C38 C 0.6666(4) 0.0012(4) 0.2859(3) 0.0327(13) Uani 1 1 d . . . H38A H 0.6622 -0.0556 0.2691 0.049 Uiso 1 1 calc R . . H38B H 0.6684 0.0428 0.2495 0.049 Uiso 1 1 calc R . . H38C H 0.6098 0.0361 0.3180 0.049 Uiso 1 1 calc R . . C39 C 0.8975(3) 0.0320(4) 0.3822(3) 0.0267(12) Uani 1 1 d . . . H39 H 0.9243 0.0810 0.3761 0.032 Uiso 1 1 calc R . . C40 C 0.9802(4) -0.0620(4) 0.3552(3) 0.0383(15) Uani 1 1 d . . . H40A H 1.0362 -0.0774 0.3795 0.058 Uiso 1 1 calc R . . H40B H 0.9994 -0.0558 0.3087 0.058 Uiso 1 1 calc R . . H40C H 0.9584 -0.1134 0.3600 0.058 Uiso 1 1 calc R . . C41 C 0.8726(4) 0.0284(4) 0.4568(3) 0.0358(14) Uani 1 1 d . . . H41A H 0.8452 -0.0183 0.4659 0.054 Uiso 1 1 calc R . . H41B H 0.8249 0.0918 0.4738 0.054 Uiso 1 1 calc R . . H41C H 0.9320 0.0094 0.4779 0.054 Uiso 1 1 calc R . . C42 C 0.6731(3) 0.1738(4) 0.3817(2) 0.0267(13) Uani 1 1 d . . . H42 H 0.6259 0.1971 0.3486 0.032 Uiso 1 1 calc R . . C43 C 0.6850(4) 0.2625(4) 0.4020(3) 0.0341(15) Uani 1 1 d . . . H43A H 0.6215 0.3118 0.4204 0.051 Uiso 1 1 calc R . . H43B H 0.7108 0.2871 0.3636 0.051 Uiso 1 1 calc R . . H43C H 0.7303 0.2455 0.4350 0.051 Uiso 1 1 calc R . . C44 C 0.6200(4) 0.1417(4) 0.4387(3) 0.0323(14) Uani 1 1 d . . . H44A H 0.6645 0.1113 0.4715 0.048 Uiso 1 1 calc R . . H44B H 0.5984 0.0958 0.4222 0.048 Uiso 1 1 calc R . . H44C H 0.5633 0.1976 0.4588 0.048 Uiso 1 1 calc R . . C45 C 0.3201(3) 0.4289(3) 0.2706(2) 0.0184(11) Uani 1 1 d . . . C46 C 0.2524(3) 0.4220(3) 0.2308(2) 0.0221(11) Uani 1 1 d . . . C47 C 0.1533(3) 0.4595(4) 0.2542(2) 0.0236(12) Uani 1 1 d . . . H47 H 0.1084 0.4599 0.2258 0.028 Uiso 1 1 calc R . . C48 C 0.1183(3) 0.4962(4) 0.3180(3) 0.0253(12) Uani 1 1 d . . . C49 C 0.1865(3) 0.4902(3) 0.3588(2) 0.0215(11) Uani 1 1 d . . . H49 H 0.1650 0.5083 0.4038 0.026 Uiso 1 1 calc R . . C50 C 0.2856(3) 0.4586(3) 0.3364(2) 0.0183(11) Uani 1 1 d . . . C51 C 0.0090(4) 0.5401(4) 0.3406(3) 0.0337(14) Uani 1 1 d . . . H51 H -0.0185 0.5016 0.3188 0.040 Uiso 1 1 calc R . . C52 C -0.0176(4) 0.5370(5) 0.4133(3) 0.051(2) Uani 1 1 d . . . H52A H 0.0069 0.5752 0.4366 0.077 Uiso 1 1 calc R . . H52B H 0.0117 0.4706 0.4271 0.077 Uiso 1 1 calc R . . H52C H -0.0887 0.5632 0.4234 0.077 Uiso 1 1 calc R . . C53 C -0.0375(6) 0.6389(6) 0.3173(5) 0.110(4) Uani 1 1 d . . . H53A H -0.1082 0.6650 0.3298 0.164 Uiso 1 1 calc R . . H53B H -0.0236 0.6382 0.2696 0.164 Uiso 1 1 calc R . . H53C H -0.0117 0.6789 0.3372 0.164 Uiso 1 1 calc R . . C54 C 0.2945(3) 0.3633(3) 0.1669(2) 0.0210(11) Uani 1 1 d . . . H54 H 0.3491 0.3789 0.1473 0.025 Uiso 1 1 calc R . . C55 C 0.3401(3) 0.2574(3) 0.1820(2) 0.0207(11) Uani 1 1 d . . . C56 C 0.4233(4) 0.1957(4) 0.1431(3) 0.0312(13) Uani 1 1 d . . . H56 H 0.4505 0.2199 0.1072 0.037 Uiso 1 1 calc R . . C57 C 0.4672(4) 0.0989(4) 0.1561(3) 0.0389(16) Uani 1 1 d . . . H57 H 0.5250 0.0578 0.1295 0.047 Uiso 1 1 calc R . . C58 C 0.4280(4) 0.0619(4) 0.2070(3) 0.0330(13) Uani 1 1 d . . . H58 H 0.4578 -0.0046 0.2153 0.040 Uiso 1 1 calc R . . C59 C 0.3455(4) 0.1219(4) 0.2455(3) 0.0327(13) Uani 1 1 d . . . H59 H 0.3180 0.0968 0.2806 0.039 Uiso 1 1 calc R . . C60 C 0.3016(4) 0.2189(4) 0.2337(3) 0.0293(13) Uani 1 1 d . . . H60 H 0.2448 0.2596 0.2612 0.035 Uiso 1 1 calc R . . C61 C 0.2262(4) 0.3820(4) 0.1146(3) 0.0306(14) Uani 1 1 d . . . C62 C 0.1577(4) 0.3459(5) 0.1167(3) 0.0454(17) Uani 1 1 d . . . H62 H 0.1479 0.3114 0.1535 0.054 Uiso 1 1 calc R . . C63 C 0.1027(5) 0.3599(6) 0.0649(4) 0.067(2) Uani 1 1 d . . . H63 H 0.0546 0.3357 0.0671 0.081 Uiso 1 1 calc R . . C64 C 0.1168(5) 0.4077(6) 0.0107(3) 0.064(2) Uani 1 1 d . . . H64 H 0.0808 0.4145 -0.0252 0.077 Uiso 1 1 calc R . . C65 C 0.1833(5) 0.4455(5) 0.0091(3) 0.054(2) Uani 1 1 d . . . H65 H 0.1921 0.4806 -0.0277 0.065 Uiso 1 1 calc R . . C66 C 0.2381(4) 0.4332(4) 0.0605(3) 0.0397(16) Uani 1 1 d . . . H66 H 0.2841 0.4599 0.0587 0.048 Uiso 1 1 calc R . . C67 C 0.3519(3) 0.4572(4) 0.3868(2) 0.0212(11) Uani 1 1 d . . . H67 H 0.4201 0.4171 0.3666 0.025 Uiso 1 1 calc R . . C68 C 0.3477(4) 0.5550(4) 0.4022(2) 0.0250(12) Uani 1 1 d . . . C69 C 0.2670(4) 0.6412(4) 0.3970(2) 0.0293(13) Uani 1 1 d . . . H69 H 0.2090 0.6405 0.3850 0.035 Uiso 1 1 calc R . . C70 C 0.2693(5) 0.7263(4) 0.4086(3) 0.0382(15) Uani 1 1 d . . . H70 H 0.2130 0.7840 0.4046 0.046 Uiso 1 1 calc R . . C71 C 0.3516(5) 0.7305(5) 0.4261(3) 0.0452(16) Uani 1 1 d . . . H71 H 0.3529 0.7906 0.4328 0.054 Uiso 1 1 calc R . . C72 C 0.4321(4) 0.6466(4) 0.4337(3) 0.0383(14) Uani 1 1 d . . . H72 H 0.4889 0.6486 0.4467 0.046 Uiso 1 1 calc R . . C73 C 0.4301(4) 0.5593(4) 0.4225(2) 0.0311(13) Uani 1 1 d . . . H73 H 0.4854 0.5016 0.4285 0.037 Uiso 1 1 calc R . . C74 C 0.3350(3) 0.4062(3) 0.4489(2) 0.0211(11) Uani 1 1 d . . . C75 C 0.3121(4) 0.4488(4) 0.5104(3) 0.0337(14) Uani 1 1 d . . . H75 H 0.3043 0.5129 0.5152 0.040 Uiso 1 1 calc R . . C76 C 0.3002(4) 0.3995(4) 0.5654(3) 0.0411(16) Uani 1 1 d . . . H76 H 0.2848 0.4299 0.6076 0.049 Uiso 1 1 calc R . . C77 C 0.3102(4) 0.3082(4) 0.5596(3) 0.0402(16) Uani 1 1 d . . . H77 H 0.3020 0.2746 0.5974 0.048 Uiso 1 1 calc R . . C78 C 0.3322(4) 0.2651(4) 0.4988(3) 0.0380(15) Uani 1 1 d . . . H78 H 0.3398 0.2011 0.4946 0.046 Uiso 1 1 calc R . . C79 C 0.3438(4) 0.3136(4) 0.4429(3) 0.0319(14) Uani 1 1 d . . . H79 H 0.3576 0.2833 0.4009 0.038 Uiso 1 1 calc R . . C80 C 0.3309(4) 0.5860(4) 0.1728(3) 0.0267(13) Uani 1 1 d . . . H80 H 0.2928 0.5529 0.1576 0.032 Uiso 1 1 calc R . . C81 C 0.2652(4) 0.6553(4) 0.2290(3) 0.0322(14) Uani 1 1 d . . . H81A H 0.3029 0.6823 0.2500 0.048 Uiso 1 1 calc R . . H81B H 0.2406 0.6208 0.2613 0.048 Uiso 1 1 calc R . . H81C H 0.2103 0.7071 0.2117 0.048 Uiso 1 1 calc R . . C82 C 0.3477(4) 0.6443(4) 0.1157(3) 0.0382(16) Uani 1 1 d . . . H82A H 0.2848 0.6885 0.1025 0.057 Uiso 1 1 calc R . . H82B H 0.3871 0.6009 0.0787 0.057 Uiso 1 1 calc R . . H82C H 0.3820 0.6808 0.1292 0.057 Uiso 1 1 calc R . . C83 C 0.5000(4) 0.5412(4) 0.2560(3) 0.0303(13) Uani 1 1 d . . . H83 H 0.4501 0.5644 0.2954 0.036 Uiso 1 1 calc R . . C84 C 0.5181(4) 0.6289(4) 0.2342(3) 0.0430(16) Uani 1 1 d . . . H84A H 0.5325 0.6566 0.2716 0.065 Uiso 1 1 calc R . . H84B H 0.4598 0.6768 0.2174 0.065 Uiso 1 1 calc R . . H84C H 0.5735 0.6092 0.1996 0.065 Uiso 1 1 calc R . . C85 C 0.5914(4) 0.4669(4) 0.2817(3) 0.0320(14) Uani 1 1 d . . . H85A H 0.6445 0.4417 0.2455 0.048 Uiso 1 1 calc R . . H85B H 0.5778 0.4143 0.3006 0.048 Uiso 1 1 calc R . . H85C H 0.6106 0.4969 0.3154 0.048 Uiso 1 1 calc R . . C86 C 0.5389(4) 0.4271(4) 0.1247(3) 0.0325(15) Uani 1 1 d . . . H86 H 0.5847 0.3645 0.1407 0.039 Uiso 1 1 calc R . . C87 C 0.4984(4) 0.4007(4) 0.0673(3) 0.0376(15) Uani 1 1 d . . . H87A H 0.4474 0.4587 0.0520 0.056 Uiso 1 1 calc R . . H87B H 0.4709 0.3555 0.0818 0.056 Uiso 1 1 calc R . . H87C H 0.5511 0.3711 0.0315 0.056 Uiso 1 1 calc R . . C88 C 0.6033(4) 0.4770(5) 0.0985(3) 0.0487(18) Uani 1 1 d . . . H88A H 0.6476 0.4406 0.0603 0.073 Uiso 1 1 calc R . . H88B H 0.6414 0.4803 0.1327 0.073 Uiso 1 1 calc R . . H88C H 0.5622 0.5419 0.0858 0.073 Uiso 1 1 calc R . . C89 C 1.3895(4) -0.0305(5) 0.3923(3) 0.0472(17) Uani 1 1 d . . . C90 C 1.2922(5) 0.0211(5) 0.4099(3) 0.0463(17) Uani 1 1 d . . . H90 H 1.2709 0.0664 0.4454 0.056 Uiso 1 1 calc R . . C91 C 1.2222(5) 0.0092(5) 0.3770(3) 0.0502(19) Uani 1 1 d . . . H91 H 1.1546 0.0462 0.3898 0.060 Uiso 1 1 calc R . . C92 C 1.2533(5) -0.0560(5) 0.3266(3) 0.0514(18) Uani 1 1 d . . . H92 H 1.2073 -0.0655 0.3038 0.062 Uiso 1 1 calc R . . C93 C 1.3518(5) -0.1086(5) 0.3084(4) 0.053(2) Uani 1 1 d . . . H93 H 1.3728 -0.1538 0.2728 0.063 Uiso 1 1 calc R . . C94 C 1.4205(5) -0.0970(5) 0.3407(3) 0.0496(18) Uani 1 1 d . . . H94 H 1.4881 -0.1341 0.3278 0.060 Uiso 1 1 calc R . . C95 C 1.4616(6) -0.0196(7) 0.4248(5) 0.091(3) Uani 1 1 d . . . H95A H 1.4576 0.0451 0.4184 0.136 Uiso 1 1 calc R . . H95B H 1.5264 -0.0668 0.4067 0.136 Uiso 1 1 calc R . . H95C H 1.4504 -0.0295 0.4717 0.136 Uiso 1 1 calc R . . C96 C 0.4581(5) 0.2341(5) -0.0479(8) 0.066(4) Uiso 0.50 1 d PD A 1 H96A H 0.4472 0.2601 -0.0916 0.099 Uiso 0.50 1 calc PR A 1 H96B H 0.5245 0.2210 -0.0398 0.099 Uiso 0.50 1 calc PR A 1 H96C H 0.4111 0.2807 -0.0149 0.099 Uiso 0.50 1 calc PR A 1 C97 C 0.4451(4) 0.1429(5) -0.0439(5) 0.041(3) Uiso 0.50 1 d PD A 1 H97A H 0.4597 0.1149 -0.0006 0.049 Uiso 0.50 1 calc PR A 1 H97B H 0.4918 0.0964 -0.0779 0.049 Uiso 0.50 1 calc PR A 1 C98 C 0.3412(5) 0.1604(7) -0.0537(4) 0.084(5) Uiso 0.50 1 d PD A 1 H98A H 0.3384 0.0985 -0.0615 0.101 Uiso 0.50 1 calc PR A 1 H98B H 0.2961 0.1918 -0.0138 0.101 Uiso 0.50 1 calc PR A 1 C99 C 0.3105(5) 0.2232(8) -0.1114(4) 0.158(12) Uiso 0.50 1 d PD A 1 H99A H 0.2853 0.2909 -0.0965 0.190 Uiso 0.50 1 calc PR A 1 H99B H 0.3686 0.2092 -0.1439 0.190 Uiso 0.50 1 calc PR A 1 C100 C 0.2342(7) 0.2106(11) -0.1443(4) 0.117(8) Uiso 0.50 1 d PD A 1 H10A H 0.1692 0.2483 -0.1198 0.140 Uiso 0.50 1 calc PR A 1 H10B H 0.2461 0.1423 -0.1441 0.140 Uiso 0.50 1 calc PR A 1 C101 C 0.2357(10) 0.2431(12) -0.2143(4) 0.091(6) Uiso 0.50 1 d PD A 1 H10C H 0.1832 0.3074 -0.2167 0.136 Uiso 0.50 1 calc PR A 1 H10D H 0.2262 0.1985 -0.2427 0.136 Uiso 0.50 1 calc PR A 1 H10E H 0.2986 0.2446 -0.2288 0.136 Uiso 0.50 1 calc PR A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01738(15) 0.02082(16) 0.02138(17) 0.00544(13) -0.00412(13) -0.00579(13) Si1 0.0170(6) 0.0275(7) 0.0239(7) 0.0099(6) -0.0074(5) -0.0114(5) N1 0.0132(17) 0.023(2) 0.019(2) 0.0051(16) -0.0067(15) -0.0078(15) C1 0.0104(19) 0.018(2) 0.022(2) 0.0084(19) -0.0060(18) -0.0020(17) Sn2 0.01612(14) 0.02182(17) 0.02401(17) 0.00582(14) -0.00660(13) -0.00696(13) Si2 0.0179(6) 0.0233(7) 0.0249(7) 0.0085(6) -0.0032(5) -0.0069(5) N2 0.0148(17) 0.0207(19) 0.023(2) 0.0115(16) -0.0077(16) -0.0066(15) C2 0.016(2) 0.018(2) 0.024(2) 0.0073(19) -0.0063(19) -0.0072(18) C3 0.022(2) 0.017(2) 0.022(3) 0.000(2) -0.002(2) -0.0026(19) C4 0.020(2) 0.021(2) 0.027(3) 0.004(2) -0.008(2) -0.0100(19) C5 0.023(2) 0.025(2) 0.021(2) 0.003(2) -0.0081(19) -0.0152(19) C6 0.026(2) 0.022(2) 0.019(2) 0.005(2) -0.0068(19) -0.0115(19) C7 0.020(2) 0.035(3) 0.035(3) -0.003(2) -0.002(2) -0.012(2) C8 0.036(3) 0.045(4) 0.054(4) 0.006(3) 0.007(3) -0.016(3) C9 0.024(3) 0.048(4) 0.042(3) -0.013(3) 0.002(3) -0.003(3) C10 0.021(2) 0.021(2) 0.029(3) -0.001(2) -0.009(2) -0.0085(19) C11 0.029(2) 0.022(2) 0.026(3) -0.002(2) -0.005(2) -0.008(2) C12 0.026(3) 0.038(3) 0.032(3) 0.004(3) -0.005(2) -0.008(2) C13 0.027(3) 0.050(4) 0.030(3) 0.002(3) -0.011(2) -0.007(3) C14 0.045(3) 0.041(3) 0.021(3) 0.003(3) -0.012(3) 0.004(3) C15 0.047(3) 0.031(3) 0.022(3) 0.001(2) -0.003(2) -0.009(3) C16 0.031(3) 0.034(3) 0.026(3) -0.003(2) -0.001(2) -0.008(2) C17 0.024(2) 0.024(3) 0.052(4) -0.001(2) -0.012(2) -0.010(2) C18 0.057(4) 0.033(3) 0.062(4) -0.010(3) -0.021(3) -0.016(3) C19 0.070(5) 0.045(4) 0.090(6) -0.032(4) -0.023(4) -0.017(4) C20 0.048(4) 0.025(3) 0.134(7) -0.026(4) -0.022(4) -0.010(3) C21 0.038(3) 0.028(3) 0.097(6) 0.007(3) -0.024(4) -0.013(3) C22 0.033(3) 0.025(3) 0.063(4) -0.003(3) -0.017(3) -0.011(2) C23 0.016(2) 0.019(2) 0.021(2) -0.0037(19) -0.0006(18) -0.0082(18) C24 0.022(2) 0.018(2) 0.024(3) -0.003(2) 0.001(2) -0.0081(19) C25 0.036(3) 0.028(3) 0.024(3) 0.004(2) 0.001(2) -0.011(2) C26 0.026(2) 0.038(3) 0.032(3) -0.001(2) -0.010(2) -0.015(2) C27 0.043(3) 0.039(3) 0.031(3) -0.004(2) -0.018(2) -0.019(2) C28 0.050(3) 0.042(3) 0.018(3) 0.005(2) -0.006(2) -0.022(3) C29 0.030(2) 0.033(3) 0.025(3) 0.004(2) -0.004(2) -0.016(2) C30 0.020(2) 0.029(3) 0.027(3) 0.005(2) -0.007(2) -0.013(2) C31 0.034(3) 0.030(3) 0.032(3) -0.001(2) -0.005(2) -0.016(2) C32 0.037(3) 0.021(3) 0.046(3) 0.000(2) -0.009(3) -0.011(2) C33 0.037(3) 0.033(3) 0.052(4) 0.014(3) -0.013(3) -0.017(2) C34 0.057(4) 0.041(3) 0.029(3) 0.006(3) -0.006(3) -0.021(3) C35 0.039(3) 0.025(3) 0.034(3) 0.005(2) -0.001(2) -0.011(2) C36 0.026(2) 0.026(3) 0.039(3) 0.015(2) -0.010(2) -0.013(2) C37 0.040(3) 0.044(3) 0.057(4) 0.028(3) -0.018(3) -0.027(2) C38 0.029(2) 0.037(3) 0.045(3) 0.013(2) -0.015(2) -0.024(2) C39 0.020(2) 0.034(3) 0.028(3) 0.011(2) -0.005(2) -0.014(2) C40 0.023(3) 0.037(3) 0.050(3) 0.023(3) -0.013(2) -0.007(2) C41 0.031(2) 0.054(3) 0.031(3) 0.018(3) -0.019(2) -0.023(2) C42 0.019(2) 0.042(3) 0.019(2) 0.009(2) -0.0089(19) -0.011(2) C43 0.024(3) 0.035(3) 0.032(3) 0.009(2) 0.002(2) -0.004(2) C44 0.020(2) 0.054(3) 0.026(3) 0.003(2) 0.000(2) -0.020(2) C45 0.0102(19) 0.018(2) 0.022(2) 0.0064(19) -0.0015(18) -0.0018(18) C46 0.023(2) 0.022(2) 0.022(2) 0.008(2) -0.0093(19) -0.0080(19) C47 0.017(2) 0.029(3) 0.024(3) 0.002(2) -0.005(2) -0.008(2) C48 0.020(2) 0.024(3) 0.030(3) 0.002(2) -0.005(2) -0.006(2) C49 0.020(2) 0.019(2) 0.023(3) -0.002(2) -0.003(2) -0.0056(19) C50 0.015(2) 0.016(2) 0.023(2) 0.0014(19) -0.0016(19) -0.0057(18) C51 0.013(2) 0.045(3) 0.040(3) -0.009(3) -0.002(2) -0.009(2) C52 0.027(3) 0.057(4) 0.050(4) -0.005(3) 0.009(3) -0.002(3) C53 0.030(4) 0.087(6) 0.151(9) 0.066(6) 0.025(5) 0.021(4) C54 0.017(2) 0.024(2) 0.021(2) 0.000(2) -0.0039(19) -0.0078(19) C55 0.020(2) 0.025(2) 0.022(2) 0.002(2) -0.0078(19) -0.0126(19) C56 0.033(3) 0.031(3) 0.032(3) 0.006(2) 0.005(2) -0.017(2) C57 0.032(3) 0.031(3) 0.047(4) -0.002(3) 0.004(3) -0.009(2) C58 0.038(3) 0.028(3) 0.041(3) 0.007(2) -0.014(2) -0.020(2) C59 0.043(3) 0.042(3) 0.028(3) 0.010(2) -0.010(2) -0.032(2) C60 0.025(2) 0.037(3) 0.033(3) 0.005(2) -0.008(2) -0.019(2) C61 0.023(3) 0.035(3) 0.024(3) -0.007(2) -0.003(2) -0.003(2) C62 0.036(3) 0.072(4) 0.034(3) -0.006(3) -0.011(3) -0.026(3) C63 0.041(3) 0.105(6) 0.057(4) -0.025(4) -0.019(3) -0.027(4) C64 0.048(4) 0.069(5) 0.040(4) -0.020(3) -0.034(3) 0.019(4) C65 0.063(4) 0.042(4) 0.034(3) -0.002(3) -0.024(3) 0.004(3) C66 0.044(3) 0.028(3) 0.038(3) 0.005(3) -0.021(3) -0.002(3) C67 0.017(2) 0.027(3) 0.018(2) 0.004(2) -0.0082(19) -0.0060(19) C68 0.030(2) 0.036(3) 0.015(2) 0.002(2) -0.004(2) -0.019(2) C69 0.038(3) 0.031(3) 0.025(3) 0.005(2) -0.016(2) -0.017(2) C70 0.056(3) 0.028(3) 0.032(3) 0.005(2) -0.012(3) -0.018(3) C71 0.079(4) 0.045(3) 0.028(3) 0.006(3) -0.011(3) -0.041(3) C72 0.048(3) 0.054(3) 0.033(3) 0.002(3) -0.008(3) -0.040(3) C73 0.034(3) 0.045(3) 0.020(3) 0.002(2) -0.005(2) -0.023(2) C74 0.017(2) 0.025(2) 0.023(2) 0.006(2) -0.0081(19) -0.0090(19) C75 0.039(3) 0.034(3) 0.032(3) 0.002(2) -0.003(2) -0.020(2) C76 0.051(3) 0.048(3) 0.028(3) 0.002(3) 0.003(3) -0.027(3) C77 0.035(3) 0.045(3) 0.040(3) 0.022(3) -0.008(3) -0.017(3) C78 0.039(3) 0.028(3) 0.047(4) 0.007(3) -0.006(3) -0.014(2) C79 0.031(3) 0.030(3) 0.034(3) 0.004(2) -0.008(2) -0.012(2) C80 0.027(2) 0.019(2) 0.030(3) 0.004(2) -0.007(2) -0.006(2) C81 0.024(3) 0.029(3) 0.032(3) 0.009(2) 0.000(2) -0.002(2) C82 0.041(3) 0.029(3) 0.035(3) 0.014(3) -0.008(3) -0.005(3) C83 0.031(2) 0.033(3) 0.032(3) 0.005(2) -0.006(2) -0.019(2) C84 0.047(3) 0.043(3) 0.048(4) 0.005(3) -0.009(3) -0.027(3) C85 0.026(2) 0.037(3) 0.036(3) -0.002(2) -0.007(2) -0.015(2) C86 0.022(3) 0.032(3) 0.029(3) 0.017(2) 0.001(2) 0.001(2) C87 0.037(3) 0.038(3) 0.033(3) -0.003(3) 0.016(3) -0.016(3) C88 0.042(3) 0.085(5) 0.029(3) 0.011(3) -0.006(3) -0.036(3) C89 0.042(3) 0.053(4) 0.052(4) 0.031(3) -0.015(3) -0.024(3) C90 0.058(4) 0.053(4) 0.027(3) 0.016(3) -0.001(3) -0.025(3) C91 0.040(3) 0.058(4) 0.042(4) 0.018(3) -0.003(3) -0.013(3) C92 0.052(4) 0.055(4) 0.049(4) 0.021(3) -0.014(3) -0.023(3) C93 0.042(4) 0.036(3) 0.066(5) 0.015(3) -0.002(3) -0.006(3) C94 0.048(4) 0.042(3) 0.055(4) 0.020(3) -0.004(3) -0.016(3) C95 0.080(5) 0.115(7) 0.092(7) 0.032(5) -0.010(5) -0.057(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N1 2.128(4) . ? Sn1 Sn2 3.1434(5) . ? Si1 N1 1.748(4) . ? Si1 C42 1.897(5) . ? Si1 C39 1.898(5) . ? Si1 C36 1.903(6) . ? N1 C1 1.436(6) . ? C1 C2 1.415(7) . ? C1 C6 1.417(7) . ? Sn2 N2 2.118(4) . ? Si2 N2 1.751(4) . ? Si2 C83 1.878(6) . ? Si2 C86 1.902(5) . ? Si2 C80 1.903(5) . ? N2 C45 1.429(6) . ? C2 C3 1.395(6) . ? C2 C10 1.526(7) . ? C3 C4 1.384(7) . ? C4 C5 1.387(7) . ? C4 C7 1.521(7) . ? C5 C6 1.378(6) . ? C6 C23 1.531(7) . ? C7 C8 1.504(8) . ? C7 C9 1.508(8) . ? C10 C17 1.513(7) . ? C10 C11 1.530(7) . ? C11 C12 1.377(8) . ? C11 C16 1.393(8) . ? C12 C13 1.391(8) . ? C13 C14 1.361(9) . ? C14 C15 1.382(9) . ? C15 C16 1.380(8) . ? C17 C18 1.376(9) . ? C17 C22 1.384(8) . ? C18 C19 1.394(9) . ? C19 C20 1.364(11) . ? C20 C21 1.380(11) . ? C21 C22 1.396(8) . ? C23 C24 1.535(7) . ? C23 C30 1.538(7) . ? C24 C25 1.375(8) . ? C24 C29 1.382(7) . ? C25 C26 1.385(8) . ? C26 C27 1.362(8) . ? C27 C28 1.391(9) . ? C28 C29 1.386(8) . ? C30 C31 1.383(7) . ? C30 C35 1.385(8) . ? C31 C32 1.379(8) . ? C32 C33 1.381(9) . ? C33 C34 1.373(9) . ? C34 C35 1.390(8) . ? C36 C37 1.522(8) . ? C36 C38 1.534(7) . ? C39 C40 1.524(7) . ? C39 C41 1.540(7) . ? C42 C43 1.528(8) . ? C42 C44 1.538(7) . ? C45 C50 1.404(7) . ? C45 C46 1.432(7) . ? C46 C47 1.396(7) . ? C46 C54 1.522(7) . ? C47 C48 1.391(7) . ? C48 C49 1.386(7) . ? C48 C51 1.526(7) . ? C49 C50 1.397(6) . ? C50 C67 1.527(7) . ? C51 C53 1.479(10) . ? C51 C52 1.505(9) . ? C54 C55 1.521(7) . ? C54 C61 1.527(7) . ? C55 C56 1.387(7) . ? C55 C60 1.395(7) . ? C56 C57 1.388(8) . ? C57 C58 1.377(8) . ? C58 C59 1.369(7) . ? C59 C60 1.385(8) . ? C61 C62 1.372(9) . ? C61 C66 1.389(8) . ? C62 C63 1.394(9) . ? C63 C64 1.367(11) . ? C64 C65 1.366(12) . ? C65 C66 1.388(9) . ? C67 C68 1.522(7) . ? C67 C74 1.538(7) . ? C68 C69 1.391(7) . ? C68 C73 1.400(7) . ? C69 C70 1.355(8) . ? C70 C71 1.374(9) . ? C71 C72 1.378(8) . ? C72 C73 1.385(8) . ? C74 C75 1.375(7) . ? C74 C79 1.384(8) . ? C75 C76 1.386(8) . ? C76 C77 1.357(9) . ? C77 C78 1.366(9) . ? C78 C79 1.391(8) . ? C80 C82 1.526(8) . ? C80 C81 1.534(7) . ? C83 C85 1.528(7) . ? C83 C84 1.539(8) . ? C86 C88 1.531(9) . ? C86 C87 1.534(9) . ? C89 C90 1.361(9) . ? C89 C94 1.385(10) . ? C89 C95 1.423(12) . ? C90 C91 1.405(10) . ? C91 C92 1.356(10) . ? C92 C93 1.379(9) . ? C93 C94 1.381(11) . ? C96 C97 1.500(7) . ? C97 C98 1.530(6) . ? C98 C99 1.505(7) . ? C99 C100 1.496(7) . ? C100 C101 1.515(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 Sn2 104.53(10) . . ? N1 Si1 C42 105.3(2) . . ? N1 Si1 C39 108.9(2) . . ? C42 Si1 C39 114.3(2) . . ? N1 Si1 C36 111.9(2) . . ? C42 Si1 C36 108.7(2) . . ? C39 Si1 C36 107.9(2) . . ? C1 N1 Si1 119.4(3) . . ? C1 N1 Sn1 109.2(3) . . ? Si1 N1 Sn1 131.5(2) . . ? C2 C1 C6 118.0(4) . . ? C2 C1 N1 119.7(4) . . ? C6 C1 N1 122.3(4) . . ? N2 Sn2 Sn1 103.48(11) . . ? N2 Si2 C83 107.2(2) . . ? N2 Si2 C86 108.9(2) . . ? C83 Si2 C86 110.8(3) . . ? N2 Si2 C80 109.3(2) . . ? C83 Si2 C80 109.8(2) . . ? C86 Si2 C80 110.8(2) . . ? C45 N2 Si2 118.8(3) . . ? C45 N2 Sn2 110.2(3) . . ? Si2 N2 Sn2 131.0(2) . . ? C3 C2 C1 119.8(5) . . ? C3 C2 C10 120.1(4) . . ? C1 C2 C10 120.1(4) . . ? C4 C3 C2 122.3(5) . . ? C3 C4 C5 117.0(4) . . ? C3 C4 C7 122.5(4) . . ? C5 C4 C7 120.5(5) . . ? C6 C5 C4 123.3(5) . . ? C5 C6 C1 119.4(4) . . ? C5 C6 C23 119.5(5) . . ? C1 C6 C23 120.7(4) . . ? C8 C7 C9 110.9(5) . . ? C8 C7 C4 111.1(4) . . ? C9 C7 C4 112.1(5) . . ? C17 C10 C2 114.9(4) . . ? C17 C10 C11 112.3(4) . . ? C2 C10 C11 109.8(4) . . ? C12 C11 C16 118.4(5) . . ? C12 C11 C10 119.8(5) . . ? C16 C11 C10 121.8(5) . . ? C11 C12 C13 121.2(6) . . ? C14 C13 C12 119.7(6) . . ? C13 C14 C15 120.1(5) . . ? C16 C15 C14 120.4(6) . . ? C15 C16 C11 120.2(6) . . ? C18 C17 C22 118.0(5) . . ? C18 C17 C10 122.6(5) . . ? C22 C17 C10 119.3(5) . . ? C17 C18 C19 120.6(7) . . ? C20 C19 C18 121.2(8) . . ? C19 C20 C21 119.2(6) . . ? C20 C21 C22 119.6(7) . . ? C17 C22 C21 121.5(6) . . ? C6 C23 C24 115.6(4) . . ? C6 C23 C30 111.2(4) . . ? C24 C23 C30 110.1(4) . . ? C25 C24 C29 117.7(5) . . ? C25 C24 C23 122.4(5) . . ? C29 C24 C23 119.8(5) . . ? C24 C25 C26 121.8(5) . . ? C27 C26 C25 120.3(5) . . ? C26 C27 C28 119.1(5) . . ? C29 C28 C27 120.0(5) . . ? C24 C29 C28 121.1(5) . . ? C31 C30 C35 118.0(5) . . ? C31 C30 C23 119.6(5) . . ? C35 C30 C23 122.4(5) . . ? C32 C31 C30 122.2(5) . . ? C31 C32 C33 119.2(5) . . ? C34 C33 C32 119.7(6) . . ? C33 C34 C35 120.7(6) . . ? C30 C35 C34 120.2(5) . . ? C37 C36 C38 109.4(5) . . ? C37 C36 Si1 117.0(4) . . ? C38 C36 Si1 111.4(4) . . ? C40 C39 C41 111.0(4) . . ? C40 C39 Si1 114.6(4) . . ? C41 C39 Si1 113.5(3) . . ? C43 C42 C44 110.5(4) . . ? C43 C42 Si1 114.8(4) . . ? C44 C42 Si1 116.6(4) . . ? C50 C45 N2 123.8(4) . . ? C50 C45 C46 117.2(4) . . ? N2 C45 C46 119.0(4) . . ? C47 C46 C45 120.0(4) . . ? C47 C46 C54 122.4(5) . . ? C45 C46 C54 117.2(4) . . ? C48 C47 C46 121.8(5) . . ? C49 C48 C47 117.3(4) . . ? C49 C48 C51 122.6(5) . . ? C47 C48 C51 120.1(5) . . ? C48 C49 C50 122.6(5) . . ? C49 C50 C45 120.1(4) . . ? C49 C50 C67 116.8(4) . . ? C45 C50 C67 123.1(4) . . ? C53 C51 C52 111.1(6) . . ? C53 C51 C48 110.1(5) . . ? C52 C51 C48 114.7(5) . . ? C55 C54 C46 109.3(4) . . ? C55 C54 C61 110.4(4) . . ? C46 C54 C61 117.0(4) . . ? C56 C55 C60 118.0(5) . . ? C56 C55 C54 119.3(4) . . ? C60 C55 C54 122.7(4) . . ? C55 C56 C57 120.6(5) . . ? C58 C57 C56 120.7(5) . . ? C59 C58 C57 119.2(5) . . ? C58 C59 C60 120.8(5) . . ? C59 C60 C55 120.7(5) . . ? C62 C61 C66 118.7(5) . . ? C62 C61 C54 123.1(5) . . ? C66 C61 C54 118.1(5) . . ? C61 C62 C63 120.0(7) . . ? C64 C63 C62 121.2(8) . . ? C65 C64 C63 118.9(6) . . ? C64 C65 C66 120.7(7) . . ? C65 C66 C61 120.4(7) . . ? C68 C67 C50 114.0(4) . . ? C68 C67 C74 112.3(4) . . ? C50 C67 C74 111.3(4) . . ? C69 C68 C73 117.4(5) . . ? C69 C68 C67 124.1(5) . . ? C73 C68 C67 118.4(4) . . ? C70 C69 C68 121.3(5) . . ? C69 C70 C71 121.2(6) . . ? C70 C71 C72 119.3(6) . . ? C71 C72 C73 119.9(6) . . ? C72 C73 C68 120.8(5) . . ? C75 C74 C79 118.6(5) . . ? C75 C74 C67 122.6(5) . . ? C79 C74 C67 118.8(5) . . ? C74 C75 C76 120.8(6) . . ? C77 C76 C75 120.5(6) . . ? C76 C77 C78 119.4(6) . . ? C77 C78 C79 121.0(6) . . ? C74 C79 C78 119.6(5) . . ? C82 C80 C81 108.6(4) . . ? C82 C80 Si2 114.4(4) . . ? C81 C80 Si2 113.5(4) . . ? C85 C83 C84 109.0(5) . . ? C85 C83 Si2 113.3(4) . . ? C84 C83 Si2 118.5(4) . . ? C88 C86 C87 109.1(5) . . ? C88 C86 Si2 115.4(4) . . ? C87 C86 Si2 116.1(4) . . ? C90 C89 C94 119.0(7) . . ? C90 C89 C95 122.8(7) . . ? C94 C89 C95 118.2(7) . . ? C89 C90 C91 121.9(6) . . ? C92 C91 C90 118.6(6) . . ? C91 C92 C93 119.9(7) . . ? C92 C93 C94 121.5(7) . . ? C93 C94 C89 119.1(6) . . ? C96 C97 C98 111.4(5) . . ? C99 C98 C97 109.4(5) . . ? C100 C99 C98 114.0(7) . . ? C99 C100 C101 110.7(7) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.657 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.117 _database_code_depnum_ccdc_archive 'CCDC 977194' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound2S _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H78 N2 Sn2' _chemical_formula_weight 1352.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.8594(7) _cell_length_b 12.3800(7) _cell_length_c 12.8382(7) _cell_angle_alpha 103.735(3) _cell_angle_beta 101.423(3) _cell_angle_gamma 94.545(3) _cell_volume 1628.88(17) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details 'Sortav, Blessing 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex X8' _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 10506 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5282 _reflns_number_gt 4187 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. A molecule of toluene of crystallisation was located in the crystal lattice and its carbon atoms were refined isotropically. The C-C distances of that molecule were restrained to reasonable values using the DFIX (1.52 ang. saturated, 1.40 ang. unsaturated) command of SHELXL.The methyl groups of the para-isopropyl substituent were found to be disordered over two sites. This disorder was modelled and the carbon atoms of the both disordered sets refined anisotropically. The DFIX (1.52 ang.) command of SHELXL was used to restrain the distances between the methine carbon, C7, and both disordered sets of bonded methyl carbons, C8, C8A and C9 (coincidental site). The DANG (2.50 ang.) command was used to restrain the distances between the methyl carbons, C8 and C9, and C8A and C9 to a reasonable value. A mild ISOR (0.008) restraint was used on the disordered methyl carbons, C8 and C8A, as their thermal ellipsoids were significantly elongated along one axis in prior refinements. During the course of the data collection for the crystal structure a power outage resulted in an incomplete dataset being collected, and decomposition of the crystal due to failure of the the cryostream unit. As no other suitable crystals of the compound were available for a recollection of the data, and the compound was not subsequently able to be prepared, a low data completeness (92.2%) was obtained for the crystal structure. Despite this, the gross molecular connectivity for the structure is unambiguous. The Level A alert resulting from the short H8A..H39 intermolecular contact (1.76 ang.) is a result of the fact that H8a is associated with one of the disordered isopropyl methyl groups, and that the calculated position for that hydrogen cannot be considered accurate. ; _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^)+(0.0749P)^2^+5.5822P] 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 5282 _refine_ls_number_parameters 376 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1660 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.071 _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 Sn1 Sn 0.64156(5) 0.97641(4) 0.96293(4) 0.02296(19) Uani 1 1 d . . . N1 N 0.4688(5) 0.8817(5) 0.9880(5) 0.0225(13) Uani 1 1 d . . . H1 H 0.4932 0.8522 1.0480 0.027 Uiso 1 1 calc R . . C1 C 0.4221(6) 0.7899(5) 0.8912(6) 0.0203(16) Uani 1 1 d . . . C2 C 0.4517(7) 0.7997(6) 0.7920(6) 0.0235(16) Uani 1 1 d . . . C3 C 0.4115(7) 0.7092(6) 0.6991(6) 0.0318(19) Uani 1 1 d . . . H3 H 0.4302 0.7157 0.6314 0.038 Uiso 1 1 calc R . . C4 C 0.3452(8) 0.6099(7) 0.7026(7) 0.036(2) Uani 1 1 d . B . C5 C 0.3151(7) 0.6036(6) 0.8004(7) 0.0329(19) Uani 1 1 d . . . H5 H 0.2672 0.5369 0.8027 0.040 Uiso 1 1 calc R . . C6 C 0.3518(7) 0.6906(5) 0.8959(6) 0.0234(16) Uani 1 1 d . . . C7 C 0.3035(8) 0.5138(7) 0.6039(7) 0.066(3) Uani 1 1 d D . . H7 H 0.3437 0.5357 0.5469 0.079 Uiso 1 1 calc R A 1 C8 C 0.3529(15) 0.4062(13) 0.6159(17) 0.085(7) Uani 0.618(19) 1 d PDU B 1 H8A H 0.4455 0.4198 0.6405 0.127 Uiso 0.618(19) 1 calc PR B 1 H8B H 0.3291 0.3500 0.5448 0.127 Uiso 0.618(19) 1 calc PR B 1 H8C H 0.3163 0.3787 0.6701 0.127 Uiso 0.618(19) 1 calc PR B 1 C9 C 0.1644(8) 0.4977(11) 0.5555(9) 0.102(5) Uani 1 1 d D B . H9A H 0.1183 0.4748 0.6067 0.153 Uiso 1 1 calc R . . H9B H 0.1449 0.4394 0.4858 0.153 Uiso 1 1 calc R . . H9C H 0.1388 0.5682 0.5422 0.153 Uiso 1 1 calc R . . C10 C 0.5164(7) 0.9114(6) 0.7843(6) 0.0249(17) Uani 1 1 d . . . C11 C 0.4228(7) 0.9890(6) 0.7624(6) 0.0282(18) Uani 1 1 d . . . C12 C 0.4607(9) 1.0988(7) 0.7580(7) 0.039(2) Uani 1 1 d . . . H12 H 0.5479 1.1218 0.7635 0.047 Uiso 1 1 calc R . . C13 C 0.3770(10) 1.1731(8) 0.7463(8) 0.052(3) Uani 1 1 d . . . H13 H 0.4074 1.2470 0.7457 0.062 Uiso 1 1 calc R . . C14 C 0.2493(11) 1.1445(8) 0.7352(7) 0.053(3) Uani 1 1 d . . . H14 H 0.1913 1.1972 0.7280 0.063 Uiso 1 1 calc R . . C15 C 0.2090(10) 1.0359(8) 0.7350(7) 0.048(2) Uani 1 1 d . . . H15 H 0.1210 1.0129 0.7252 0.058 Uiso 1 1 calc R . . C16 C 0.2921(8) 0.9606(7) 0.7486(7) 0.037(2) Uani 1 1 d . . . H16 H 0.2604 0.8868 0.7486 0.044 Uiso 1 1 calc R . . C17 C 0.6098(8) 0.8918(7) 0.7107(7) 0.036(2) Uani 1 1 d . . . C18 C 0.6075(9) 0.9397(8) 0.6212(7) 0.047(2) Uani 1 1 d . . . H18 H 0.5440 0.9854 0.6042 0.056 Uiso 1 1 calc R . . C19 C 0.6961(11) 0.9211(10) 0.5583(9) 0.062(3) Uani 1 1 d . . . H19 H 0.6918 0.9526 0.4973 0.075 Uiso 1 1 calc R . . C20 C 0.7860(10) 0.8609(9) 0.5811(8) 0.057(3) Uani 1 1 d . . . H20 H 0.8484 0.8530 0.5384 0.068 Uiso 1 1 calc R . . C21 C 0.7937(10) 0.8078(8) 0.6658(8) 0.055(3) Uani 1 1 d . . . H21 H 0.8572 0.7612 0.6796 0.066 Uiso 1 1 calc R . . C22 C 0.7017(8) 0.8268(7) 0.7304(7) 0.042(2) Uani 1 1 d . . . H22 H 0.7047 0.7926 0.7896 0.051 Uiso 1 1 calc R . . C23 C 0.3118(6) 0.6834(5) 1.0012(6) 0.0209(16) Uani 1 1 d . . . H23 H 0.3873 0.7164 1.0626 0.025 Uiso 1 1 calc R . . C24 C 0.2776(7) 0.5629(6) 1.0066(6) 0.0269(17) Uani 1 1 d . . . C25 C 0.1574(7) 0.5051(6) 0.9624(6) 0.0288(18) Uani 1 1 d . . . H25 H 0.0915 0.5419 0.9313 0.035 Uiso 1 1 calc R . . C26 C 0.1322(8) 0.3934(6) 0.9631(8) 0.040(2) Uani 1 1 d . . . H26 H 0.0497 0.3535 0.9310 0.048 Uiso 1 1 calc R . . C27 C 0.2259(9) 0.3412(7) 1.0098(9) 0.055(3) Uani 1 1 d . . . H27 H 0.2089 0.2646 1.0093 0.066 Uiso 1 1 calc R . . C28 C 0.3427(9) 0.3982(8) 1.0568(10) 0.066(3) Uani 1 1 d . . . H28 H 0.4069 0.3626 1.0919 0.079 Uiso 1 1 calc R . . C29 C 0.3689(8) 0.5094(7) 1.0535(9) 0.052(3) Uani 1 1 d . . . H29 H 0.4519 0.5483 1.0846 0.063 Uiso 1 1 calc R . . C30 C 0.2082(7) 0.7553(5) 1.0226(6) 0.0219(16) Uani 1 1 d . . . C31 C 0.1197(7) 0.7767(6) 0.9378(7) 0.0270(18) Uani 1 1 d . . . H31 H 0.1240 0.7454 0.8637 0.032 Uiso 1 1 calc R . . C32 C 0.0265(8) 0.8419(6) 0.9585(7) 0.034(2) Uani 1 1 d . . . H32 H -0.0330 0.8548 0.8992 0.041 Uiso 1 1 calc R . . C33 C 0.0192(8) 0.8892(6) 1.0669(8) 0.037(2) Uani 1 1 d . . . H33 H -0.0448 0.9348 1.0819 0.044 Uiso 1 1 calc R . . C34 C 0.1055(8) 0.8691(6) 1.1515(7) 0.034(2) Uani 1 1 d . . . H34 H 0.1018 0.9021 1.2254 0.041 Uiso 1 1 calc R . . C35 C 0.1967(7) 0.8020(6) 1.1307(6) 0.0275(18) Uani 1 1 d . . . H35 H 0.2533 0.7867 1.1904 0.033 Uiso 1 1 calc R . . C36 C 0.1609(11) 0.7315(10) 1.3940(10) 0.092(4) Uiso 1 1 d D . . C37 C 0.2896(10) 0.7751(10) 1.4342(10) 0.076(3) Uiso 1 1 d D . . H37 H 0.3178 0.8448 1.4876 0.091 Uiso 1 1 calc R . . C38 C 0.3711(13) 0.7083(10) 1.3896(11) 0.094(4) Uiso 1 1 d D . . H38 H 0.4593 0.7339 1.4145 0.113 Uiso 1 1 calc R . . C39 C 0.3346(14) 0.6060(11) 1.3108(12) 0.115(5) Uiso 1 1 d D . . H39 H 0.3972 0.5646 1.2844 0.138 Uiso 1 1 calc R . . C40 C 0.2062(13) 0.5642(13) 1.2703(14) 0.125(6) Uiso 1 1 d D . . H40 H 0.1776 0.4948 1.2166 0.150 Uiso 1 1 calc R . . C41 C 0.1244(12) 0.6313(9) 1.3144(9) 0.078(4) Uiso 1 1 d D . . H41 H 0.0362 0.6067 1.2880 0.094 Uiso 1 1 calc R . . C42 C 0.0756(17) 0.8078(15) 1.4420(15) 0.147(7) Uiso 1 1 d D . . H42A H -0.0118 0.7830 1.3998 0.221 Uiso 1 1 calc R . . H42B H 0.1018 0.8844 1.4391 0.221 Uiso 1 1 calc R . . H42C H 0.0808 0.8062 1.5187 0.221 Uiso 1 1 calc R . . C8A C 0.3855(14) 0.479(2) 0.5249(16) 0.065(9) Uani 0.382(19) 1 d PDU B 2 H8A1 H 0.3890 0.5333 0.4807 0.097 Uiso 0.382(19) 1 calc PR B 2 H8A2 H 0.3503 0.4046 0.4765 0.097 Uiso 0.382(19) 1 calc PR B 2 H8A3 H 0.4712 0.4764 0.5657 0.097 Uiso 0.382(19) 1 calc PR B 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 Sn1 0.0215(3) 0.0167(3) 0.0289(3) 0.00381(19) 0.0074(2) -0.00619(18) N1 0.023(3) 0.020(3) 0.023(4) 0.007(2) 0.004(3) -0.003(2) C1 0.021(4) 0.013(3) 0.025(4) 0.000(3) 0.005(3) -0.001(3) C2 0.024(4) 0.019(4) 0.024(4) 0.004(3) 0.005(3) -0.005(3) C3 0.033(4) 0.028(4) 0.029(5) -0.001(3) 0.011(4) -0.008(3) C4 0.031(5) 0.029(4) 0.041(5) -0.006(4) 0.012(4) -0.010(4) C5 0.027(4) 0.021(4) 0.047(5) -0.002(3) 0.016(4) -0.011(3) C6 0.020(4) 0.014(3) 0.037(5) 0.004(3) 0.011(3) 0.002(3) C7 0.057(7) 0.052(6) 0.066(7) -0.029(5) 0.033(6) -0.033(5) C8 0.096(9) 0.071(9) 0.079(9) 0.013(6) 0.007(6) 0.012(6) C9 0.083(9) 0.138(13) 0.045(8) -0.028(7) 0.007(6) -0.042(9) C10 0.032(4) 0.023(4) 0.017(4) 0.002(3) 0.009(3) -0.010(3) C11 0.036(5) 0.029(4) 0.017(4) 0.007(3) 0.005(3) -0.008(3) C12 0.044(5) 0.039(5) 0.035(5) 0.019(4) 0.002(4) -0.009(4) C13 0.066(7) 0.039(5) 0.045(6) 0.023(4) -0.011(5) -0.005(5) C14 0.079(8) 0.045(6) 0.038(6) 0.020(4) 0.007(5) 0.021(5) C15 0.053(6) 0.062(6) 0.035(6) 0.018(4) 0.011(4) 0.012(5) C16 0.044(5) 0.033(5) 0.035(5) 0.010(4) 0.013(4) -0.001(4) C17 0.027(5) 0.030(4) 0.039(5) -0.009(4) 0.006(4) -0.016(4) C18 0.042(5) 0.050(6) 0.042(6) 0.008(4) 0.011(4) -0.017(4) C19 0.067(8) 0.074(8) 0.051(7) 0.018(5) 0.032(6) -0.011(6) C20 0.052(7) 0.073(7) 0.043(7) 0.004(5) 0.025(5) -0.010(6) C21 0.051(6) 0.052(6) 0.042(7) -0.012(5) -0.002(5) 0.004(5) C22 0.032(5) 0.049(6) 0.033(5) -0.011(4) 0.009(4) -0.018(4) C23 0.018(4) 0.018(4) 0.027(4) 0.009(3) 0.002(3) -0.001(3) C24 0.023(4) 0.019(4) 0.041(5) 0.007(3) 0.014(4) -0.001(3) C25 0.026(4) 0.018(4) 0.046(5) 0.010(3) 0.015(4) -0.001(3) C26 0.032(5) 0.019(4) 0.071(7) 0.011(4) 0.024(4) -0.007(4) C27 0.041(6) 0.023(4) 0.120(9) 0.031(5) 0.042(6) 0.008(4) C28 0.028(5) 0.040(5) 0.148(11) 0.062(6) 0.017(6) 0.004(4) C29 0.026(5) 0.036(5) 0.108(9) 0.045(5) 0.014(5) -0.001(4) C30 0.022(4) 0.010(3) 0.031(5) 0.003(3) 0.007(3) -0.009(3) C31 0.027(4) 0.014(3) 0.039(5) 0.009(3) 0.007(4) -0.010(3) C32 0.029(5) 0.022(4) 0.052(6) 0.018(4) 0.008(4) -0.004(3) C33 0.033(5) 0.019(4) 0.069(7) 0.021(4) 0.025(5) 0.006(3) C34 0.045(5) 0.025(4) 0.038(5) 0.008(4) 0.023(4) 0.000(4) C35 0.026(4) 0.026(4) 0.031(5) 0.016(3) 0.003(3) -0.008(3) C8A 0.062(11) 0.063(11) 0.067(11) 0.010(7) 0.018(7) 0.009(7) _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 N1 2.242(6) 2_677 ? Sn1 N1 2.251(6) . ? Sn1 C10 2.338(7) . ? N1 C1 1.444(8) . ? N1 Sn1 2.242(6) 2_677 ? C1 C2 1.402(10) . ? C1 C6 1.415(9) . ? C2 C3 1.397(10) . ? C2 C10 1.534(9) . ? C3 C4 1.389(10) . ? C4 C5 1.376(11) . ? C4 C7 1.483(11) . ? C5 C6 1.391(10) . ? C6 C23 1.519(10) . ? C7 C8A 1.488(8) . ? C7 C9 1.493(7) . ? C7 C8 1.504(7) . ? C10 C11 1.485(11) . ? C10 C17 1.514(11) . ? C11 C16 1.400(11) . ? C11 C12 1.407(10) . ? C12 C13 1.356(13) . ? C13 C14 1.374(14) . ? C14 C15 1.380(13) . ? C15 C16 1.365(12) . ? C17 C22 1.353(12) . ? C17 C18 1.410(12) . ? C18 C19 1.372(13) . ? C19 C20 1.304(15) . ? C20 C21 1.390(14) . ? C21 C22 1.421(13) . ? C23 C30 1.516(10) . ? C23 C24 1.530(9) . ? C24 C29 1.356(11) . ? C24 C25 1.380(10) . ? C25 C26 1.391(10) . ? C26 C27 1.364(12) . ? C27 C28 1.351(13) . ? C28 C29 1.396(11) . ? C30 C31 1.394(10) . ? C30 C35 1.405(10) . ? C31 C32 1.370(11) . ? C32 C33 1.396(12) . ? C33 C34 1.372(12) . ? C34 C35 1.368(11) . ? C36 C41 1.379(8) . ? C36 C37 1.404(8) . ? C36 C42 1.489(8) . ? C37 C38 1.374(7) . ? C38 C39 1.392(8) . ? C39 C40 1.398(8) . ? C40 C41 1.375(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 N1 79.8(2) 2_677 . ? N1 Sn1 C10 94.5(2) 2_677 . ? N1 Sn1 C10 77.2(2) . . ? C1 N1 Sn1 122.8(4) . 2_677 ? C1 N1 Sn1 107.6(4) . . ? Sn1 N1 Sn1 100.2(2) 2_677 . ? C2 C1 C6 120.4(6) . . ? C2 C1 N1 118.3(6) . . ? C6 C1 N1 121.4(6) . . ? C3 C2 C1 118.6(6) . . ? C3 C2 C10 121.0(6) . . ? C1 C2 C10 120.2(6) . . ? C4 C3 C2 122.0(7) . . ? C5 C4 C3 118.1(7) . . ? C5 C4 C7 120.1(7) . . ? C3 C4 C7 121.8(8) . . ? C4 C5 C6 122.8(7) . . ? C5 C6 C1 118.1(6) . . ? C5 C6 C23 121.6(6) . . ? C1 C6 C23 120.2(6) . . ? C4 C7 C8A 122.3(11) . . ? C4 C7 C9 113.7(7) . . ? C8A C7 C9 115.9(8) . . ? C4 C7 C8 114.9(11) . . ? C8A C7 C8 69.6(14) . . ? C9 C7 C8 112.7(7) . . ? C11 C10 C17 117.2(7) . . ? C11 C10 C2 111.4(6) . . ? C17 C10 C2 111.0(6) . . ? C11 C10 Sn1 110.6(5) . . ? C17 C10 Sn1 105.0(5) . . ? C2 C10 Sn1 100.0(4) . . ? C16 C11 C12 115.2(8) . . ? C16 C11 C10 123.2(7) . . ? C12 C11 C10 121.6(7) . . ? C13 C12 C11 122.1(8) . . ? C12 C13 C14 121.9(9) . . ? C13 C14 C15 117.1(9) . . ? C16 C15 C14 121.8(10) . . ? C15 C16 C11 121.8(8) . . ? C22 C17 C18 117.1(8) . . ? C22 C17 C10 119.9(8) . . ? C18 C17 C10 123.0(8) . . ? C19 C18 C17 120.6(10) . . ? C20 C19 C18 121.0(11) . . ? C19 C20 C21 122.3(10) . . ? C20 C21 C22 116.5(10) . . ? C17 C22 C21 122.3(10) . . ? C30 C23 C6 111.6(6) . . ? C30 C23 C24 112.3(6) . . ? C6 C23 C24 113.3(6) . . ? C29 C24 C25 118.5(7) . . ? C29 C24 C23 119.3(7) . . ? C25 C24 C23 122.1(7) . . ? C24 C25 C26 120.3(8) . . ? C27 C26 C25 120.0(8) . . ? C28 C27 C26 120.1(8) . . ? C27 C28 C29 119.9(9) . . ? C24 C29 C28 121.1(8) . . ? C31 C30 C35 117.0(7) . . ? C31 C30 C23 122.4(6) . . ? C35 C30 C23 120.5(6) . . ? C32 C31 C30 121.7(7) . . ? C31 C32 C33 119.9(8) . . ? C34 C33 C32 119.3(8) . . ? C35 C34 C33 120.8(7) . . ? C34 C35 C30 121.3(7) . . ? C41 C36 C37 120.7(12) . . ? C41 C36 C42 126.6(12) . . ? C37 C36 C42 112.6(12) . . ? C38 C37 C36 114.3(12) . . ? C37 C38 C39 125.1(14) . . ? C38 C39 C40 120.1(15) . . ? C41 C40 C39 114.8(15) . . ? C40 C41 C36 124.9(13) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 1.209 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.137 _database_code_depnum_ccdc_archive 'CCDC 977195' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H164 N4 Si2 Sn2' _chemical_formula_weight 1908.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Sn Sn -0.6537 1.4246 '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' 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' _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 17.5664(8) _cell_length_b 13.8316(5) _cell_length_c 21.8305(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.274(5) _cell_angle_gamma 90.00 _cell_volume 5302.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'orange green' _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 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details 'Sortav, Blessing 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex X8' _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 72060 _diffrn_reflns_av_R_equivalents 0.0961 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12152 _reflns_number_gt 8304 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. A molecule of hexane of crystallisation was located in the crystal lattice and its carbon atoms were refined isotropically. A half molecule of hexane of crystallisation (sitting on an inversion centre) was located in the crystal lattice and its carbon atoms were refined isotropically. the DFIX command of SHELXL was used to restrain the C-C bonds in both hexane molecules to a reasonable distance (1.52 ang.) for such interactions. The methyl groups of the para-isopropyl substituent were found to be disordered over two sites. This disorder was modelled and the carbon atoms of the major disordered set refined anisotropically, while the carbons of the minor set were refined isotropically. The DFIX (1.52 ang.) command of SHELXL was used to restrain the distances between the methine carbon, C7, and both disordered sets of bonded methyl carbons, C8, C9 and C8A, C9A.In addition, the DFIX command of SHELXL was used to restrain the distances between the quaternary carbon, C46, and the three attached methyl carbons, C47, C48, C49, to a reasonable distance (1.52 ang.) for such interactions. A mild ISOR (0.008) restraint was used on C9, C48 and C49, as they displayed elongated thermal displacement ellipsoids in prior refinements. In the case of C48 and C49, this command was used after attempts to model disorder of the tert butyl group containing those atoms were not successful. The largest residual electron density peak in the final difference map (1.72 e-/ang.3) was located close (ca. 1.1 ang.) to Sn(1). ; _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^)+(0.0750P)^2^+9.5215P] 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 12152 _refine_ls_number_parameters 539 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1709 _refine_ls_wR_factor_gt 0.1438 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.558294(16) 0.075697(19) 0.979512(13) 0.02161(10) Uani 1 1 d . . . Si1 Si 0.54604(7) 0.24872(8) 1.08846(6) 0.0221(3) Uani 1 1 d . . . N1 N 0.5981(2) 0.1490(2) 1.06386(16) 0.0207(7) Uani 1 1 d . . . C1 C 0.6728(2) 0.1220(3) 1.08579(19) 0.0210(9) Uani 1 1 d . . . N2 N 0.7134(2) -0.0769(3) 0.98302(19) 0.0316(9) Uani 1 1 d . . . C2 C 0.6834(2) 0.0533(3) 1.1340(2) 0.0224(9) Uani 1 1 d . . . C3 C 0.7565(3) 0.0283(3) 1.1545(2) 0.0292(10) Uani 1 1 d . . . H3 H 0.7617 -0.0174 1.1868 0.035 Uiso 1 1 calc R . . C4 C 0.8217(3) 0.0667(3) 1.1300(2) 0.0308(11) Uani 1 1 d . B . C5 C 0.8113(3) 0.1312(3) 1.0814(2) 0.0310(11) Uani 1 1 d . . . H5 H 0.8551 0.1572 1.0626 0.037 Uiso 1 1 calc R . . C6 C 0.7399(2) 0.1592(3) 1.0592(2) 0.0241(9) Uani 1 1 d . . . C7 C 0.9007(3) 0.0390(4) 1.1555(3) 0.0564(17) Uani 1 1 d D . . H7 H 0.8976 0.0583 1.1996 0.068 Uiso 1 1 calc R A 1 C8 C 0.9102(5) -0.0710(5) 1.1598(4) 0.048(3) Uani 0.661(11) 1 d PD B 1 H8A H 0.9156 -0.0979 1.1186 0.072 Uiso 0.661(11) 1 calc PR B 1 H8B H 0.8654 -0.0993 1.1788 0.072 Uiso 0.661(11) 1 calc PR B 1 H8C H 0.9558 -0.0862 1.1847 0.072 Uiso 0.661(11) 1 calc PR B 1 C9 C 0.9666(5) 0.0955(9) 1.1347(6) 0.075(4) Uani 0.661(11) 1 d PDU B 1 H9A H 0.9554 0.1647 1.1380 0.112 Uiso 0.661(11) 1 calc PR B 1 H9B H 0.9766 0.0795 1.0919 0.112 Uiso 0.661(11) 1 calc PR B 1 H9C H 1.0115 0.0798 1.1602 0.112 Uiso 0.661(11) 1 calc PR B 1 C10 C 0.6169(3) 0.0048(3) 1.1661(2) 0.0299(10) Uani 1 1 d . . . H10 H 0.5712 0.0113 1.1382 0.036 Uiso 1 1 calc R . . C11 C 0.6309(3) -0.1039(3) 1.1753(2) 0.0284(10) Uani 1 1 d . . . C12 C 0.6221(3) -0.1667(3) 1.1258(2) 0.0358(12) Uani 1 1 d . . . H12 H 0.6058 -0.1423 1.0871 0.043 Uiso 1 1 calc R . . C13 C 0.6369(3) -0.2647(4) 1.1325(2) 0.0443(14) Uani 1 1 d . . . H13 H 0.6304 -0.3068 1.0984 0.053 Uiso 1 1 calc R . . C14 C 0.6612(3) -0.3017(3) 1.1887(3) 0.0409(13) Uani 1 1 d . . . H14 H 0.6718 -0.3687 1.1932 0.049 Uiso 1 1 calc R . . C15 C 0.6697(3) -0.2402(3) 1.2381(2) 0.0392(13) Uani 1 1 d . . . H15 H 0.6858 -0.2649 1.2768 0.047 Uiso 1 1 calc R . . C16 C 0.6548(3) -0.1421(3) 1.2312(2) 0.0347(12) Uani 1 1 d . . . H16 H 0.6610 -0.1004 1.2655 0.042 Uiso 1 1 calc R . . C17 C 0.5970(3) 0.0521(4) 1.2269(3) 0.0397(13) Uani 1 1 d . . . C18 C 0.5273(4) 0.0317(5) 1.2529(3) 0.0569(17) Uani 1 1 d . . . H18 H 0.4937 -0.0135 1.2339 0.068 Uiso 1 1 calc R . . C19 C 0.5064(5) 0.0780(6) 1.3074(4) 0.076(3) Uani 1 1 d . . . H19 H 0.4584 0.0642 1.3247 0.091 Uiso 1 1 calc R . . C20 C 0.5552(6) 0.1435(6) 1.3360(4) 0.082(3) Uani 1 1 d . . . H20 H 0.5402 0.1763 1.3720 0.098 Uiso 1 1 calc R . . C21 C 0.6246(5) 0.1602(4) 1.3121(3) 0.064(2) Uani 1 1 d . . . H21 H 0.6592 0.2027 1.3326 0.077 Uiso 1 1 calc R . . C22 C 0.6458(4) 0.1155(4) 1.2579(2) 0.0440(14) Uani 1 1 d . . . H22 H 0.6945 0.1286 1.2417 0.053 Uiso 1 1 calc R . . C23 C 0.7374(3) 0.2315(3) 1.0058(2) 0.0286(10) Uani 1 1 d . . . H23 H 0.6829 0.2366 0.9919 0.034 Uiso 1 1 calc R . . C24 C 0.7633(3) 0.3344(3) 1.0233(2) 0.0294(10) Uani 1 1 d . . . C25 C 0.8016(3) 0.3585(3) 1.0778(2) 0.0346(11) Uani 1 1 d . . . H25 H 0.8154 0.3091 1.1061 0.041 Uiso 1 1 calc R . . C26 C 0.8197(3) 0.4546(4) 1.0911(3) 0.0423(13) Uani 1 1 d . . . H26 H 0.8454 0.4702 1.1286 0.051 Uiso 1 1 calc R . . C27 C 0.8004(3) 0.5275(4) 1.0499(3) 0.0472(14) Uani 1 1 d . . . H27 H 0.8123 0.5930 1.0592 0.057 Uiso 1 1 calc R . . C28 C 0.7642(3) 0.5045(4) 0.9956(3) 0.0452(14) Uani 1 1 d . . . H28 H 0.7513 0.5542 0.9671 0.054 Uiso 1 1 calc R . . C29 C 0.7459(3) 0.4088(3) 0.9820(3) 0.0363(12) Uani 1 1 d . . . H29 H 0.7213 0.3938 0.9440 0.044 Uiso 1 1 calc R . . C30 C 0.7821(3) 0.1968(3) 0.9502(2) 0.0333(11) Uani 1 1 d . . . C31 C 0.8595(3) 0.2137(4) 0.9444(3) 0.0449(13) Uani 1 1 d . . . H31 H 0.8862 0.2485 0.9757 0.054 Uiso 1 1 calc R . . C32 C 0.8990(3) 0.1805(4) 0.8935(3) 0.0516(15) Uani 1 1 d . . . H32 H 0.9522 0.1917 0.8908 0.062 Uiso 1 1 calc R . . C33 C 0.8610(4) 0.1321(4) 0.8475(3) 0.0540(16) Uani 1 1 d . . . H33 H 0.8877 0.1089 0.8131 0.065 Uiso 1 1 calc R . . C34 C 0.7831(4) 0.1172(4) 0.8515(3) 0.0505(15) Uani 1 1 d . . . H34 H 0.7561 0.0853 0.8192 0.061 Uiso 1 1 calc R . . C35 C 0.7446(3) 0.1489(4) 0.9025(2) 0.0385(12) Uani 1 1 d . . . H35 H 0.6915 0.1376 0.9049 0.046 Uiso 1 1 calc R . . C36 C 0.4832(3) 0.2143(3) 1.1537(2) 0.0265(10) Uani 1 1 d . . . H36 H 0.5182 0.1821 1.1841 0.032 Uiso 1 1 calc R . . C37 C 0.4433(3) 0.2933(4) 1.1903(2) 0.0383(12) Uani 1 1 d . . . H37A H 0.4074 0.3280 1.1633 0.057 Uiso 1 1 calc R . . H37B H 0.4814 0.3387 1.2069 0.057 Uiso 1 1 calc R . . H37C H 0.4158 0.2637 1.2240 0.057 Uiso 1 1 calc R . . C38 C 0.4252(3) 0.1353(3) 1.1348(2) 0.0330(11) Uani 1 1 d . . . H38A H 0.4003 0.1106 1.1714 0.049 Uiso 1 1 calc R . . H38B H 0.4517 0.0823 1.1144 0.049 Uiso 1 1 calc R . . H38C H 0.3868 0.1629 1.1067 0.049 Uiso 1 1 calc R . . C39 C 0.4851(3) 0.2896(3) 1.0196(2) 0.0257(10) Uani 1 1 d . . . H39 H 0.4627 0.2296 1.0010 0.031 Uiso 1 1 calc R . . C40 C 0.4176(3) 0.3550(4) 1.0358(2) 0.0356(12) Uani 1 1 d . . . H40A H 0.4364 0.4113 1.0589 0.053 Uiso 1 1 calc R . . H40B H 0.3818 0.3187 1.0608 0.053 Uiso 1 1 calc R . . H40C H 0.3917 0.3768 0.9981 0.053 Uiso 1 1 calc R . . C41 C 0.5333(3) 0.3374(3) 0.9692(2) 0.0327(11) Uani 1 1 d . . . H41A H 0.5001 0.3552 0.9343 0.049 Uiso 1 1 calc R . . H41B H 0.5721 0.2917 0.9556 0.049 Uiso 1 1 calc R . . H41C H 0.5582 0.3955 0.9858 0.049 Uiso 1 1 calc R . . C42 C 0.6110(3) 0.3510(3) 1.1144(2) 0.0263(10) Uani 1 1 d . . . H42 H 0.6513 0.3555 1.0829 0.032 Uiso 1 1 calc R . . C43 C 0.6531(3) 0.3291(3) 1.1749(2) 0.0329(11) Uani 1 1 d . . . H43A H 0.6874 0.3828 1.1853 0.049 Uiso 1 1 calc R . . H43B H 0.6828 0.2696 1.1706 0.049 Uiso 1 1 calc R . . H43C H 0.6161 0.3209 1.2074 0.049 Uiso 1 1 calc R . . C44 C 0.5751(3) 0.4527(3) 1.1175(2) 0.0375(12) Uani 1 1 d . . . H44A H 0.5365 0.4536 1.1493 0.056 Uiso 1 1 calc R . . H44B H 0.5511 0.4685 1.0778 0.056 Uiso 1 1 calc R . . H44C H 0.6147 0.5004 1.1274 0.056 Uiso 1 1 calc R . . C45 C 0.6586(3) -0.0331(3) 0.9900(2) 0.0277(10) Uani 1 1 d . . . C46 C 0.7845(3) -0.1309(3) 0.9742(2) 0.0415(14) Uani 1 1 d D . . C47 C 0.8499(3) -0.0607(4) 0.9740(3) 0.0517(16) Uani 1 1 d D . . H47A H 0.8428 -0.0150 0.9401 0.078 Uiso 1 1 calc R . . H47B H 0.8977 -0.0962 0.9689 0.078 Uiso 1 1 calc R . . H47C H 0.8519 -0.0253 1.0129 0.078 Uiso 1 1 calc R . . C48 C 0.7789(5) -0.1789(7) 0.9116(4) 0.104(3) Uani 1 1 d DU . . H48A H 0.7413 -0.2311 0.9126 0.156 Uiso 1 1 calc R . . H48B H 0.8287 -0.2056 0.9012 0.156 Uiso 1 1 calc R . . H48C H 0.7633 -0.1309 0.8808 0.156 Uiso 1 1 calc R . . C49 C 0.7919(5) -0.2028(6) 1.0253(4) 0.093(3) Uani 1 1 d DU . . H49A H 0.7950 -0.1686 1.0646 0.140 Uiso 1 1 calc R . . H49B H 0.8382 -0.2412 1.0201 0.140 Uiso 1 1 calc R . . H49C H 0.7475 -0.2457 1.0246 0.140 Uiso 1 1 calc R . . C50 C 0.5593(7) 0.2339(7) 0.7825(6) 0.127(4) Uiso 1 1 d D . . H50A H 0.5985 0.1992 0.7600 0.191 Uiso 1 1 calc R . . H50B H 0.5111 0.2320 0.7590 0.191 Uiso 1 1 calc R . . H50C H 0.5525 0.2032 0.8224 0.191 Uiso 1 1 calc R . . C51 C 0.5835(7) 0.3373(8) 0.7916(7) 0.164(5) Uiso 1 1 d D . . H51A H 0.5648 0.3595 0.8317 0.197 Uiso 1 1 calc R . . H51B H 0.5582 0.3772 0.7595 0.197 Uiso 1 1 calc R . . C52 C 0.6678(6) 0.3558(7) 0.7900(6) 0.132(4) Uiso 1 1 d D . . H52A H 0.6864 0.3410 0.7486 0.159 Uiso 1 1 calc R . . H52B H 0.6944 0.3126 0.8196 0.159 Uiso 1 1 calc R . . C53 C 0.6863(7) 0.4618(8) 0.8060(6) 0.147(5) Uiso 1 1 d D . . H53A H 0.6639 0.5061 0.7749 0.177 Uiso 1 1 calc R . . H53B H 0.6665 0.4790 0.8466 0.177 Uiso 1 1 calc R . . C54 C 0.7722(7) 0.4672(9) 0.8063(7) 0.157(5) Uiso 1 1 d D . . H54A H 0.7931 0.4499 0.7661 0.189 Uiso 1 1 calc R . . H54B H 0.7956 0.4258 0.8386 0.189 Uiso 1 1 calc R . . C55 C 0.7823(10) 0.5741(9) 0.8205(8) 0.194(7) Uiso 1 1 d D . . H55A H 0.7745 0.6118 0.7829 0.291 Uiso 1 1 calc R . . H55B H 0.8339 0.5854 0.8370 0.291 Uiso 1 1 calc R . . H55C H 0.7451 0.5939 0.8508 0.291 Uiso 1 1 calc R . . C56 C 1.0200(9) 0.3110(9) 1.0788(7) 0.176(6) Uiso 1 1 d D . . H56A H 0.9655 0.2957 1.0795 0.264 Uiso 1 1 calc R . . H56B H 1.0426 0.3017 1.1198 0.264 Uiso 1 1 calc R . . H56C H 1.0450 0.2682 1.0497 0.264 Uiso 1 1 calc R . . C57 C 1.0301(8) 0.4125(9) 1.0597(6) 0.153(5) Uiso 1 1 d D . . H57A H 1.0855 0.4247 1.0575 0.184 Uiso 1 1 calc R . . H57B H 1.0106 0.4540 1.0928 0.184 Uiso 1 1 calc R . . C58 C 0.9945(8) 0.4463(3) 1.0011(6) 0.142(5) Uiso 1 1 d D . . H58A H 0.9396 0.4302 0.9996 0.170 Uiso 1 1 calc R . . H58B H 1.0191 0.4151 0.9659 0.170 Uiso 1 1 calc R . . C8A C 0.9099(11) -0.0285(12) 1.2082(7) 0.057(6) Uiso 0.339(11) 1 d PD B 2 H8A1 H 0.9639 -0.0334 1.2199 0.085 Uiso 0.339(11) 1 calc PR B 2 H8A2 H 0.8906 -0.0925 1.1964 0.085 Uiso 0.339(11) 1 calc PR B 2 H8A3 H 0.8812 -0.0041 1.2429 0.085 Uiso 0.339(11) 1 calc PR B 2 C9A C 0.9556(9) 0.0292(13) 1.1022(6) 0.047(5) Uiso 0.339(11) 1 d PD B 2 H9A1 H 0.9479 0.0833 1.0737 0.071 Uiso 0.339(11) 1 calc PR B 2 H9A2 H 0.9459 -0.0319 1.0807 0.071 Uiso 0.339(11) 1 calc PR B 2 H9A3 H 1.0082 0.0300 1.1182 0.071 Uiso 0.339(11) 1 calc PR B 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 Sn1 0.02405(17) 0.01813(16) 0.02248(16) -0.00062(11) -0.00317(11) 0.00149(12) Si1 0.0238(6) 0.0181(5) 0.0242(6) -0.0012(4) -0.0044(5) 0.0036(5) N1 0.0214(18) 0.0184(17) 0.0223(18) -0.0044(13) -0.0022(14) 0.0010(14) C1 0.026(2) 0.0131(19) 0.024(2) -0.0020(15) -0.0043(18) 0.0022(16) N2 0.032(2) 0.026(2) 0.037(2) -0.0061(16) -0.0048(18) 0.0033(17) C2 0.021(2) 0.018(2) 0.028(2) 0.0004(16) -0.0025(18) 0.0009(16) C3 0.031(3) 0.020(2) 0.035(3) 0.0036(18) -0.009(2) -0.0001(19) C4 0.025(2) 0.025(2) 0.042(3) -0.0007(19) -0.007(2) 0.0022(19) C5 0.023(2) 0.025(2) 0.045(3) -0.001(2) -0.002(2) -0.0051(18) C6 0.025(2) 0.017(2) 0.030(2) 0.0005(17) -0.0025(19) -0.0014(17) C7 0.031(3) 0.059(4) 0.078(5) 0.003(3) -0.017(3) 0.009(3) C8 0.038(5) 0.056(6) 0.050(6) 0.014(4) -0.008(4) 0.021(4) C9 0.049(5) 0.083(6) 0.092(6) 0.021(5) -0.011(5) -0.005(4) C10 0.024(2) 0.027(2) 0.039(3) 0.013(2) -0.004(2) 0.0014(19) C11 0.023(2) 0.026(2) 0.035(3) 0.0071(19) -0.005(2) -0.0037(18) C12 0.041(3) 0.032(3) 0.034(3) 0.009(2) -0.015(2) -0.008(2) C13 0.065(4) 0.030(3) 0.038(3) 0.000(2) -0.020(3) -0.015(3) C14 0.052(3) 0.021(2) 0.049(3) 0.006(2) -0.018(3) -0.008(2) C15 0.049(3) 0.026(2) 0.041(3) 0.007(2) -0.017(3) -0.004(2) C16 0.046(3) 0.023(2) 0.035(3) 0.0046(19) -0.010(2) -0.002(2) C17 0.043(3) 0.032(3) 0.045(3) 0.020(2) 0.009(2) 0.016(2) C18 0.050(4) 0.056(4) 0.065(4) 0.034(3) 0.019(3) 0.020(3) C19 0.086(5) 0.079(5) 0.066(5) 0.047(4) 0.046(4) 0.054(5) C20 0.140(8) 0.056(4) 0.053(4) 0.023(4) 0.044(5) 0.052(5) C21 0.113(6) 0.035(3) 0.044(4) 0.006(3) 0.018(4) 0.031(4) C22 0.070(4) 0.029(3) 0.033(3) 0.007(2) 0.006(3) 0.018(3) C23 0.022(2) 0.023(2) 0.040(3) 0.0058(19) -0.001(2) -0.0028(18) C24 0.023(2) 0.020(2) 0.046(3) 0.0037(19) 0.004(2) -0.0006(18) C25 0.034(3) 0.023(2) 0.047(3) 0.007(2) 0.002(2) -0.001(2) C26 0.046(3) 0.027(2) 0.054(4) -0.003(2) 0.001(3) -0.006(2) C27 0.047(3) 0.024(3) 0.071(4) 0.002(3) 0.009(3) -0.003(2) C28 0.041(3) 0.030(3) 0.065(4) 0.017(3) 0.008(3) 0.004(2) C29 0.034(3) 0.030(3) 0.045(3) 0.009(2) 0.003(2) 0.004(2) C30 0.037(3) 0.028(2) 0.036(3) 0.007(2) 0.006(2) -0.003(2) C31 0.045(3) 0.032(3) 0.058(4) -0.001(2) 0.016(3) -0.007(2) C32 0.042(3) 0.041(3) 0.072(4) 0.002(3) 0.025(3) -0.009(3) C33 0.067(4) 0.048(3) 0.049(4) 0.004(3) 0.029(3) 0.002(3) C34 0.062(4) 0.055(4) 0.034(3) 0.003(3) 0.005(3) -0.003(3) C35 0.040(3) 0.042(3) 0.034(3) 0.007(2) 0.006(2) -0.005(2) C36 0.031(2) 0.020(2) 0.029(2) -0.0028(17) -0.0036(19) 0.0039(18) C37 0.041(3) 0.037(3) 0.037(3) -0.005(2) 0.003(2) 0.007(2) C38 0.026(2) 0.037(3) 0.037(3) -0.001(2) 0.003(2) -0.002(2) C39 0.027(2) 0.020(2) 0.030(2) -0.0001(17) -0.0046(19) 0.0017(18) C40 0.039(3) 0.031(3) 0.036(3) -0.001(2) -0.011(2) 0.011(2) C41 0.041(3) 0.024(2) 0.032(3) 0.0035(19) -0.009(2) 0.006(2) C42 0.029(2) 0.018(2) 0.031(3) -0.0010(17) -0.005(2) 0.0018(18) C43 0.031(3) 0.028(2) 0.039(3) -0.003(2) -0.011(2) 0.001(2) C44 0.050(3) 0.023(2) 0.039(3) -0.005(2) -0.008(2) 0.004(2) C45 0.024(2) 0.025(2) 0.034(3) -0.0027(19) -0.003(2) 0.0027(19) C46 0.027(3) 0.026(3) 0.071(4) -0.013(2) -0.003(3) 0.004(2) C47 0.035(3) 0.038(3) 0.083(5) 0.007(3) 0.018(3) 0.006(2) C48 0.070(4) 0.118(5) 0.123(6) -0.070(5) -0.003(4) 0.031(4) C49 0.066(4) 0.079(4) 0.137(6) 0.053(4) 0.024(4) 0.019(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 N1 2.202(3) . ? Sn1 C45 2.325(4) . ? Sn1 Sn1 3.0759(6) 3_657 ? Si1 N1 1.746(4) . ? Si1 C36 1.881(5) . ? Si1 C42 1.897(4) . ? Si1 C39 1.911(4) . ? N1 C1 1.436(5) . ? C1 C6 1.422(6) . ? C1 C2 1.427(6) . ? N2 C45 1.149(6) . ? N2 C46 1.472(6) . ? C2 C3 1.394(6) . ? C2 C10 1.529(6) . ? C3 C4 1.380(7) . ? C4 C5 1.395(7) . ? C4 C7 1.532(7) . ? C5 C6 1.390(6) . ? C6 C23 1.538(6) . ? C7 C9 1.478(7) . ? C7 C8A 1.486(8) . ? C7 C8 1.534(6) . ? C7 C9A 1.535(8) . ? C10 C17 1.529(8) . ? C10 C11 1.535(6) . ? C11 C16 1.386(6) . ? C11 C12 1.393(7) . ? C12 C13 1.387(7) . ? C13 C14 1.388(7) . ? C14 C15 1.378(7) . ? C15 C16 1.389(6) . ? C17 C18 1.389(8) . ? C17 C22 1.391(8) . ? C18 C19 1.405(10) . ? C19 C20 1.386(12) . ? C20 C21 1.357(11) . ? C21 C22 1.394(8) . ? C23 C30 1.536(7) . ? C23 C24 1.540(6) . ? C24 C25 1.394(7) . ? C24 C29 1.396(6) . ? C25 C26 1.396(7) . ? C26 C27 1.390(8) . ? C27 C28 1.369(8) . ? C28 C29 1.393(7) . ? C30 C35 1.387(7) . ? C30 C31 1.389(7) . ? C31 C32 1.402(8) . ? C32 C33 1.368(9) . ? C33 C34 1.388(9) . ? C34 C35 1.387(8) . ? C36 C37 1.531(6) . ? C36 C38 1.545(6) . ? C39 C40 1.539(6) . ? C39 C41 1.551(7) . ? C42 C43 1.528(6) . ? C42 C44 1.543(6) . ? C46 C49 1.498(6) . ? C46 C47 1.504(6) . ? C46 C48 1.520(6) . ? C50 C51 1.503(7) . ? C51 C52 1.504(7) . ? C52 C53 1.539(7) . ? C53 C54 1.510(7) . ? C54 C55 1.520(7) . ? C56 C57 1.476(7) . ? C57 C58 1.487(7) . ? C58 C58 1.499(8) 3_767 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 C45 89.39(14) . . ? N1 Sn1 Sn1 105.76(10) . 3_657 ? C45 Sn1 Sn1 92.23(12) . 3_657 ? N1 Si1 C36 110.69(19) . . ? N1 Si1 C42 111.41(19) . . ? C36 Si1 C42 108.7(2) . . ? N1 Si1 C39 106.23(18) . . ? C36 Si1 C39 110.0(2) . . ? C42 Si1 C39 109.71(19) . . ? C1 N1 Si1 125.8(3) . . ? C1 N1 Sn1 115.4(3) . . ? Si1 N1 Sn1 117.51(17) . . ? C6 C1 C2 116.5(4) . . ? C6 C1 N1 122.0(4) . . ? C2 C1 N1 121.5(4) . . ? C45 N2 C46 178.7(4) . . ? C3 C2 C1 120.3(4) . . ? C3 C2 C10 116.9(4) . . ? C1 C2 C10 122.8(4) . . ? C4 C3 C2 123.2(4) . . ? C3 C4 C5 116.4(4) . . ? C3 C4 C7 121.1(4) . . ? C5 C4 C7 122.6(5) . . ? C6 C5 C4 123.0(5) . . ? C5 C6 C1 120.5(4) . . ? C5 C6 C23 117.1(4) . . ? C1 C6 C23 122.4(4) . . ? C9 C7 C8A 119.9(10) . . ? C9 C7 C4 117.7(6) . . ? C8A C7 C4 121.4(9) . . ? C9 C7 C8 117.3(7) . . ? C8A C7 C8 47.2(8) . . ? C4 C7 C8 111.5(5) . . ? C9 C7 C9A 45.7(8) . . ? C8A C7 C9A 118.1(11) . . ? C4 C7 C9A 109.0(8) . . ? C8 C7 C9A 83.6(8) . . ? C2 C10 C17 113.7(4) . . ? C2 C10 C11 111.6(4) . . ? C17 C10 C11 110.1(4) . . ? C16 C11 C12 118.1(4) . . ? C16 C11 C10 122.3(4) . . ? C12 C11 C10 119.6(4) . . ? C13 C12 C11 120.7(4) . . ? C12 C13 C14 120.4(5) . . ? C15 C14 C13 119.3(5) . . ? C14 C15 C16 120.1(5) . . ? C11 C16 C15 121.4(5) . . ? C18 C17 C22 118.0(6) . . ? C18 C17 C10 119.3(6) . . ? C22 C17 C10 122.7(5) . . ? C17 C18 C19 120.2(7) . . ? C20 C19 C18 120.6(7) . . ? C21 C20 C19 119.3(7) . . ? C20 C21 C22 120.7(8) . . ? C17 C22 C21 121.2(7) . . ? C30 C23 C6 113.0(4) . . ? C30 C23 C24 109.3(4) . . ? C6 C23 C24 114.2(4) . . ? C25 C24 C29 118.0(4) . . ? C25 C24 C23 124.5(4) . . ? C29 C24 C23 117.5(4) . . ? C24 C25 C26 120.6(5) . . ? C27 C26 C25 120.3(5) . . ? C28 C27 C26 119.6(5) . . ? C27 C28 C29 120.4(5) . . ? C28 C29 C24 121.1(5) . . ? C35 C30 C31 117.5(5) . . ? C35 C30 C23 120.0(4) . . ? C31 C30 C23 122.5(5) . . ? C30 C31 C32 121.3(6) . . ? C33 C32 C31 120.0(6) . . ? C32 C33 C34 119.5(6) . . ? C35 C34 C33 120.1(6) . . ? C30 C35 C34 121.5(5) . . ? C37 C36 C38 109.7(4) . . ? C37 C36 Si1 119.8(3) . . ? C38 C36 Si1 111.8(3) . . ? C40 C39 C41 110.4(4) . . ? C40 C39 Si1 114.4(3) . . ? C41 C39 Si1 112.3(3) . . ? C43 C42 C44 109.5(4) . . ? C43 C42 Si1 112.7(3) . . ? C44 C42 Si1 116.6(3) . . ? N2 C45 Sn1 164.2(4) . . ? N2 C46 C49 107.4(5) . . ? N2 C46 C47 108.9(4) . . ? C49 C46 C47 112.1(5) . . ? N2 C46 C48 107.6(4) . . ? C49 C46 C48 112.4(7) . . ? C47 C46 C48 108.3(6) . . ? C50 C51 C52 115.8(10) . . ? C51 C52 C53 111.2(9) . . ? C54 C53 C52 104.8(9) . . ? C53 C54 C55 99.3(11) . . ? C56 C57 C58 119.4(11) . . ? C57 C58 C58 106.7(11) . 3_767 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.728 _refine_diff_density_min -0.870 _refine_diff_density_rms 0.118 _database_code_depnum_ccdc_archive 'CCDC 977196' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_LSnBr _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47.50 H56 Br N Si Sn' _chemical_formula_weight 867.62 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' N N 0.0061 0.0033 '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' 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 9.9346(4) _cell_length_b 13.1778(5) _cell_length_c 17.8089(8) _cell_angle_alpha 72.260(2) _cell_angle_beta 74.655(2) _cell_angle_gamma 71.450(2) _cell_volume 2068.62(15) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _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 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 894 _exptl_absorpt_coefficient_mu 1.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.680 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details 'Sortav, Blessing 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex X8' _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 28260 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8954 _reflns_number_gt 8377 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. A molecule of toluene of crystallisation was located in the crystal lattice and its carbon atoms refined, isotropically, at 50% occupancy. The C-C distances of that molecule were restrained to reasonable values using the DFIX (1.52 ang. saturated, 1.40 ang. unsaturated) command of SHELXL. Additionally, the FLAT command was used to restrain the seven carbon atoms of the toluene molecule to a plane. ; _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^)+(0.0330P)^2^+7.8377P] 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 8954 _refine_ls_number_parameters 470 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.183 _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 0.51554(2) 0.900102(15) 0.287382(12) 0.01674(5) Uani 1 1 d . . . Br1 Br 0.48957(4) 1.10775(2) 0.26450(2) 0.03058(8) Uani 1 1 d . . . Si1 Si 0.13291(7) 0.97855(5) 0.27899(4) 0.00942(14) Uani 1 1 d . . . N1 N 0.3077(2) 0.88939(17) 0.28697(12) 0.0093(4) Uani 1 1 d . . . C1 C 0.3386(2) 0.77387(19) 0.29044(14) 0.0066(5) Uani 1 1 d . . . C2 C 0.3955(3) 0.73514(19) 0.21950(14) 0.0080(5) Uani 1 1 d . . . C3 C 0.4273(3) 0.6230(2) 0.22356(15) 0.0113(5) Uani 1 1 d . . . H3 H 0.4637 0.5987 0.1752 0.014 Uiso 1 1 calc R . . C4 C 0.4077(3) 0.5456(2) 0.29541(15) 0.0109(5) Uani 1 1 d . . . C5 C 0.3570(3) 0.5831(2) 0.36552(15) 0.0108(5) Uani 1 1 d . . . H5 H 0.3446 0.5311 0.4155 0.013 Uiso 1 1 calc R . . C6 C 0.3240(3) 0.6944(2) 0.36471(14) 0.0079(5) Uani 1 1 d . . . C7 C 0.4366(3) 0.4249(2) 0.29626(16) 0.0161(6) Uani 1 1 d . . . H7 H 0.4235 0.3819 0.3534 0.019 Uiso 1 1 calc R . . C8 C 0.5894(3) 0.3775(2) 0.25464(18) 0.0187(6) Uani 1 1 d . . . H8A H 0.6049 0.4193 0.1986 0.028 Uiso 1 1 calc R . . H8B H 0.6020 0.3000 0.2565 0.028 Uiso 1 1 calc R . . H8C H 0.6596 0.3827 0.2821 0.028 Uiso 1 1 calc R . . C9 C 0.3271(3) 0.4111(3) 0.2563(2) 0.0298(8) Uani 1 1 d . . . H9A H 0.2290 0.4402 0.2838 0.045 Uiso 1 1 calc R . . H9B H 0.3426 0.3327 0.2597 0.045 Uiso 1 1 calc R . . H9C H 0.3394 0.4517 0.1999 0.045 Uiso 1 1 calc R . . C10 C 0.4286(3) 0.81357(19) 0.13839(14) 0.0084(5) Uani 1 1 d . . . H10 H 0.3577 0.8866 0.1407 0.010 Uiso 1 1 calc R . . C11 C 0.5783(3) 0.8316(2) 0.12397(15) 0.0106(5) Uani 1 1 d . . . C12 C 0.5965(3) 0.9379(2) 0.09283(16) 0.0133(5) Uani 1 1 d . . . H12 H 0.5155 0.9979 0.0805 0.016 Uiso 1 1 calc R . . C13 C 0.7314(3) 0.9576(2) 0.07942(17) 0.0185(6) Uani 1 1 d . . . H13 H 0.7417 1.0308 0.0590 0.022 Uiso 1 1 calc R . . C14 C 0.8500(3) 0.8710(2) 0.09568(18) 0.0199(6) Uani 1 1 d . . . H14 H 0.9423 0.8843 0.0860 0.024 Uiso 1 1 calc R . . C15 C 0.8344(3) 0.7642(3) 0.12624(19) 0.0231(7) Uani 1 1 d . . . H15 H 0.9161 0.7044 0.1374 0.028 Uiso 1 1 calc R . . C16 C 0.6991(3) 0.7449(2) 0.14054(18) 0.0187(6) Uani 1 1 d . . . H16 H 0.6888 0.6718 0.1618 0.022 Uiso 1 1 calc R . . C17 C 0.4031(3) 0.77742(19) 0.07068(14) 0.0097(5) Uani 1 1 d . . . C18 C 0.5092(3) 0.7566(2) 0.00466(16) 0.0162(6) Uani 1 1 d . . . H18 H 0.6032 0.7637 0.0007 0.019 Uiso 1 1 calc R . . C19 C 0.4789(3) 0.7254(3) -0.05595(17) 0.0242(7) Uani 1 1 d . . . H19 H 0.5521 0.7122 -0.1012 0.029 Uiso 1 1 calc R . . C20 C 0.3442(4) 0.7136(3) -0.05061(18) 0.0238(7) Uani 1 1 d . . . H20 H 0.3239 0.6926 -0.0921 0.029 Uiso 1 1 calc R . . C21 C 0.2376(3) 0.7324(2) 0.01571(17) 0.0194(6) Uani 1 1 d . . . H21 H 0.1445 0.7234 0.0200 0.023 Uiso 1 1 calc R . . C22 C 0.2671(3) 0.7642(2) 0.07521(15) 0.0133(5) Uani 1 1 d . . . H22 H 0.1933 0.7774 0.1202 0.016 Uiso 1 1 calc R . . C23 C 0.2823(3) 0.7291(2) 0.44390(14) 0.0086(5) Uani 1 1 d . . . H23 H 0.2100 0.8025 0.4355 0.010 Uiso 1 1 calc R . . C24 C 0.2083(3) 0.6507(2) 0.51285(14) 0.0097(5) Uani 1 1 d . . . C25 C 0.0759(3) 0.6388(2) 0.50921(16) 0.0158(6) Uani 1 1 d . . . H25 H 0.0327 0.6791 0.4636 0.019 Uiso 1 1 calc R . . C26 C 0.0060(3) 0.5692(2) 0.57097(18) 0.0196(6) Uani 1 1 d . . . H26 H -0.0845 0.5627 0.5675 0.024 Uiso 1 1 calc R . . C27 C 0.0678(3) 0.5090(2) 0.63802(17) 0.0189(6) Uani 1 1 d . . . H27 H 0.0202 0.4609 0.6803 0.023 Uiso 1 1 calc R . . C28 C 0.1988(3) 0.5198(2) 0.64236(16) 0.0171(6) Uani 1 1 d . . . H28 H 0.2417 0.4789 0.6880 0.021 Uiso 1 1 calc R . . C29 C 0.2687(3) 0.5901(2) 0.58051(15) 0.0128(5) Uani 1 1 d . . . H29 H 0.3588 0.5968 0.5845 0.015 Uiso 1 1 calc R . . C30 C 0.4106(3) 0.7460(2) 0.46535(14) 0.0100(5) Uani 1 1 d . . . C31 C 0.3889(3) 0.8250(2) 0.50747(16) 0.0173(6) Uani 1 1 d . . . H31 H 0.2941 0.8692 0.5212 0.021 Uiso 1 1 calc R . . C32 C 0.5037(4) 0.8404(2) 0.52970(19) 0.0251(7) Uani 1 1 d . . . H32 H 0.4873 0.8952 0.5578 0.030 Uiso 1 1 calc R . . C33 C 0.6420(3) 0.7755(3) 0.51069(18) 0.0249(7) Uani 1 1 d . . . H33 H 0.7206 0.7855 0.5260 0.030 Uiso 1 1 calc R . . C34 C 0.6655(3) 0.6964(3) 0.46967(17) 0.0215(7) Uani 1 1 d . . . H34 H 0.7603 0.6514 0.4572 0.026 Uiso 1 1 calc R . . C35 C 0.5507(3) 0.6822(2) 0.44634(16) 0.0150(6) Uani 1 1 d . . . H35 H 0.5682 0.6283 0.4172 0.018 Uiso 1 1 calc R . . C36 C 0.1104(3) 1.0347(2) 0.16999(16) 0.0144(6) Uani 1 1 d . . . H36 H 0.1498 0.9702 0.1451 0.017 Uiso 1 1 calc R . . C37 C 0.2046(3) 1.1154(2) 0.12434(18) 0.0205(6) Uani 1 1 d . . . H37A H 0.2164 1.1242 0.0665 0.031 Uiso 1 1 calc R . . H37B H 0.2995 1.0862 0.1401 0.031 Uiso 1 1 calc R . . H37C H 0.1577 1.1871 0.1374 0.031 Uiso 1 1 calc R . . C38 C -0.0437(3) 1.0874(3) 0.15320(19) 0.0232(7) Uani 1 1 d . . . H38A H -0.0880 1.1512 0.1768 0.035 Uiso 1 1 calc R . . H38B H -0.1011 1.0333 0.1769 0.035 Uiso 1 1 calc R . . H38C H -0.0405 1.1113 0.0951 0.035 Uiso 1 1 calc R . . C39 C 0.1160(3) 1.0980(2) 0.32116(19) 0.0204(6) Uani 1 1 d . . . H39 H 0.2022 1.1267 0.2915 0.025 Uiso 1 1 calc R . . C40 C -0.0150(4) 1.1978(2) 0.3070(2) 0.0295(8) Uani 1 1 d . . . H40A H -0.1040 1.1762 0.3363 0.044 Uiso 1 1 calc R . . H40B H -0.0177 1.2233 0.2495 0.044 Uiso 1 1 calc R . . H40C H -0.0067 1.2575 0.3261 0.044 Uiso 1 1 calc R . . C41 C 0.1288(4) 1.0661(3) 0.4076(2) 0.0362(9) Uani 1 1 d . . . H41A H 0.1226 1.1319 0.4246 0.054 Uiso 1 1 calc R . . H41B H 0.2219 1.0127 0.4147 0.054 Uiso 1 1 calc R . . H41C H 0.0502 1.0330 0.4403 0.054 Uiso 1 1 calc R . . C42 C -0.0060(3) 0.8970(2) 0.33520(16) 0.0146(6) Uani 1 1 d . . . H42 H 0.0272 0.8512 0.3864 0.018 Uiso 1 1 calc R . . C43 C -0.0155(3) 0.8158(2) 0.29167(19) 0.0200(6) Uani 1 1 d . . . H43A H -0.0819 0.7719 0.3262 0.030 Uiso 1 1 calc R . . H43B H 0.0806 0.7667 0.2793 0.030 Uiso 1 1 calc R . . H43C H -0.0511 0.8570 0.2418 0.030 Uiso 1 1 calc R . . C44 C -0.1574(3) 0.9698(3) 0.35945(19) 0.0228(7) Uani 1 1 d . . . H44A H -0.1904 1.0225 0.3115 0.034 Uiso 1 1 calc R . . H44B H -0.1539 1.0100 0.3967 0.034 Uiso 1 1 calc R . . H44C H -0.2247 0.9233 0.3856 0.034 Uiso 1 1 calc R . . C45 C 1.0951(13) 0.4532(11) 0.1113(6) 0.105(6) Uiso 0.50 1 d PD A -1 H45A H 1.1690 0.3829 0.1123 0.158 Uiso 0.50 1 calc PR A -1 H45B H 1.0188 0.4448 0.1589 0.158 Uiso 0.50 1 calc PR A -1 H45C H 1.1391 0.5101 0.1112 0.158 Uiso 0.50 1 calc PR A -1 C46 C 1.0309(6) 0.4866(6) 0.0367(4) 0.056(2) Uiso 0.50 1 d PD A -1 C47 C 1.1186(8) 0.5098(8) -0.0376(3) 0.047(3) Uiso 0.50 1 d PD A -1 H47 H 1.2176 0.5022 -0.0391 0.056 Uiso 0.50 1 calc PR A -1 C48 C 1.0705(6) 0.5437(7) -0.1103(4) 0.0437(19) Uiso 0.50 1 d PD A -1 H48 H 1.1348 0.5639 -0.1589 0.052 Uiso 0.50 1 calc PR A -1 C49 C 0.9310(7) 0.5484(8) -0.1131(4) 0.053(3) Uiso 0.50 1 d PD A -1 H49 H 0.8978 0.5645 -0.1619 0.064 Uiso 0.50 1 calc PR A -1 C50 C 0.8429(10) 0.5272(9) -0.0375(4) 0.066(3) Uiso 0.50 1 d PD A -1 H50 H 0.7437 0.5359 -0.0360 0.079 Uiso 0.50 1 calc PR A -1 C51 C 0.8888(8) 0.4945(13) 0.0357(5) 0.073(5) Uiso 0.50 1 d PD A -1 H51 H 0.8233 0.4779 0.0845 0.088 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01686(8) 0.01300(8) 0.02211(9) -0.00398(7) -0.00688(7) -0.00379(7) Br1 0.03228(15) 0.01488(13) 0.05017(19) -0.00728(13) -0.01528(14) -0.00791(12) Si1 0.0099(3) 0.0065(3) 0.0110(3) -0.0032(2) -0.0028(2) 0.0007(2) N1 0.0125(9) 0.0062(9) 0.0101(9) -0.0033(7) -0.0040(8) -0.0010(7) C1 0.0067(10) 0.0050(9) 0.0084(10) -0.0031(8) -0.0017(8) -0.0003(8) C2 0.0104(10) 0.0070(10) 0.0062(10) -0.0015(8) -0.0011(8) -0.0023(8) C3 0.0161(11) 0.0108(11) 0.0073(10) -0.0050(9) 0.0003(9) -0.0033(9) C4 0.0151(11) 0.0065(10) 0.0115(11) -0.0034(9) -0.0024(9) -0.0024(9) C5 0.0158(11) 0.0082(10) 0.0068(10) -0.0002(9) -0.0015(9) -0.0030(9) C6 0.0089(10) 0.0095(10) 0.0061(10) -0.0039(8) -0.0016(8) -0.0012(8) C7 0.0269(13) 0.0074(11) 0.0121(12) -0.0035(9) 0.0011(10) -0.0047(10) C8 0.0238(13) 0.0114(11) 0.0218(13) -0.0100(10) -0.0052(11) 0.0009(10) C9 0.0229(14) 0.0200(13) 0.054(2) -0.0203(13) -0.0016(14) -0.0087(12) C10 0.0114(10) 0.0065(10) 0.0070(10) -0.0027(8) 0.0000(8) -0.0021(8) C11 0.0123(11) 0.0119(11) 0.0079(10) -0.0027(9) -0.0007(9) -0.0041(9) C12 0.0145(11) 0.0115(11) 0.0128(11) -0.0022(9) -0.0033(9) -0.0019(9) C13 0.0204(12) 0.0177(12) 0.0199(13) -0.0039(10) -0.0017(11) -0.0106(10) C14 0.0156(12) 0.0262(14) 0.0208(13) -0.0063(11) -0.0033(10) -0.0090(11) C15 0.0140(12) 0.0215(14) 0.0289(15) -0.0021(12) -0.0069(11) 0.0006(11) C16 0.0160(12) 0.0126(12) 0.0232(14) -0.0004(11) -0.0036(11) -0.0020(10) C17 0.0166(11) 0.0048(10) 0.0062(10) 0.0000(8) -0.0026(9) -0.0015(9) C18 0.0184(12) 0.0187(12) 0.0110(12) -0.0056(10) 0.0010(10) -0.0055(10) C19 0.0292(15) 0.0307(15) 0.0114(12) -0.0109(11) 0.0012(11) -0.0046(13) C20 0.0348(15) 0.0268(14) 0.0149(12) -0.0101(11) -0.0077(12) -0.0072(12) C21 0.0224(13) 0.0191(13) 0.0186(13) -0.0035(11) -0.0073(11) -0.0063(11) C22 0.0156(11) 0.0130(11) 0.0097(11) -0.0019(9) -0.0023(9) -0.0026(10) C23 0.0123(10) 0.0083(10) 0.0050(10) -0.0029(8) -0.0019(8) -0.0012(9) C24 0.0127(11) 0.0094(10) 0.0060(10) -0.0048(8) 0.0004(9) -0.0004(9) C25 0.0171(12) 0.0184(12) 0.0120(12) -0.0019(10) -0.0044(10) -0.0050(10) C26 0.0146(12) 0.0235(13) 0.0220(14) -0.0043(11) -0.0019(11) -0.0087(11) C27 0.0205(13) 0.0168(12) 0.0158(13) -0.0023(10) 0.0042(11) -0.0076(11) C28 0.0223(13) 0.0146(12) 0.0106(12) -0.0002(10) -0.0029(10) -0.0024(10) C29 0.0132(11) 0.0139(11) 0.0096(11) -0.0024(9) -0.0023(9) -0.0015(9) C30 0.0141(11) 0.0099(10) 0.0057(10) -0.0002(8) -0.0019(9) -0.0045(9) C31 0.0255(13) 0.0138(12) 0.0142(12) -0.0050(10) -0.0060(10) -0.0038(10) C32 0.0452(16) 0.0175(13) 0.0223(14) -0.0035(11) -0.0154(13) -0.0149(12) C33 0.0308(14) 0.0292(15) 0.0207(14) 0.0069(12) -0.0132(12) -0.0214(12) C34 0.0173(12) 0.0312(15) 0.0142(13) 0.0026(11) -0.0055(10) -0.0094(11) C35 0.0145(11) 0.0184(12) 0.0126(11) -0.0059(10) -0.0021(10) -0.0030(10) C36 0.0134(11) 0.0132(11) 0.0140(12) -0.0011(10) -0.0041(10) -0.0006(10) C37 0.0198(13) 0.0190(13) 0.0179(13) 0.0000(11) -0.0002(11) -0.0055(11) C38 0.0178(13) 0.0262(15) 0.0216(14) 0.0023(12) -0.0099(11) -0.0030(12) C39 0.0196(13) 0.0139(12) 0.0291(14) -0.0144(11) -0.0039(11) 0.0021(10) C40 0.0285(16) 0.0151(13) 0.0391(18) -0.0149(13) 0.0002(14) 0.0048(12) C41 0.050(2) 0.0309(17) 0.0285(16) -0.0142(14) -0.0100(15) -0.0031(16) C42 0.0128(11) 0.0143(12) 0.0147(12) 0.0006(10) -0.0040(10) -0.0034(10) C43 0.0180(12) 0.0186(13) 0.0269(14) -0.0056(11) -0.0065(11) -0.0075(10) C44 0.0138(12) 0.0249(14) 0.0238(15) -0.0041(12) 0.0022(11) -0.0033(11) _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 N1 2.116(2) . ? Sn1 Br1 2.5782(4) . ? Si1 N1 1.774(2) . ? Si1 C39 1.886(3) . ? Si1 C36 1.901(3) . ? Si1 C42 1.902(3) . ? N1 C1 1.439(3) . ? C1 C2 1.417(3) . ? C1 C6 1.420(3) . ? C2 C3 1.393(3) . ? C2 C10 1.522(3) . ? C3 C4 1.384(3) . ? C4 C5 1.394(4) . ? C4 C7 1.519(4) . ? C5 C6 1.394(3) . ? C6 C23 1.527(3) . ? C7 C8 1.525(4) . ? C7 C9 1.529(5) . ? C10 C11 1.523(4) . ? C10 C17 1.528(4) . ? C11 C12 1.391(4) . ? C11 C16 1.393(4) . ? C12 C13 1.391(4) . ? C13 C14 1.378(4) . ? C14 C15 1.388(4) . ? C15 C16 1.391(4) . ? C17 C18 1.387(3) . ? C17 C22 1.395(4) . ? C18 C19 1.395(4) . ? C19 C20 1.372(5) . ? C20 C21 1.388(4) . ? C21 C22 1.377(4) . ? C23 C30 1.520(4) . ? C23 C24 1.532(3) . ? C24 C29 1.393(4) . ? C24 C25 1.394(4) . ? C25 C26 1.385(4) . ? C26 C27 1.390(4) . ? C27 C28 1.378(4) . ? C28 C29 1.392(4) . ? C30 C35 1.393(4) . ? C30 C31 1.393(4) . ? C31 C32 1.390(5) . ? C32 C33 1.384(5) . ? C33 C34 1.375(5) . ? C34 C35 1.394(4) . ? C36 C38 1.535(4) . ? C36 C37 1.539(4) . ? C39 C41 1.496(5) . ? C39 C40 1.539(4) . ? C42 C44 1.537(4) . ? C42 C43 1.538(4) . ? C45 C46 1.510(7) . ? C46 C47 1.384(6) . ? C46 C51 1.387(7) . ? C47 C48 1.396(7) . ? C48 C49 1.380(7) . ? C49 C50 1.400(7) . ? C50 C51 1.393(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 Br1 104.89(6) . . ? N1 Si1 C39 106.76(12) . . ? N1 Si1 C36 111.10(11) . . ? C39 Si1 C36 108.30(13) . . ? N1 Si1 C42 108.40(11) . . ? C39 Si1 C42 113.45(13) . . ? C36 Si1 C42 108.85(13) . . ? C1 N1 Si1 121.34(17) . . ? C1 N1 Sn1 100.07(14) . . ? Si1 N1 Sn1 138.49(12) . . ? C2 C1 C6 117.8(2) . . ? C2 C1 N1 120.4(2) . . ? C6 C1 N1 121.6(2) . . ? C3 C2 C1 120.0(2) . . ? C3 C2 C10 118.8(2) . . ? C1 C2 C10 121.2(2) . . ? C4 C3 C2 122.4(2) . . ? C3 C4 C5 117.6(2) . . ? C3 C4 C7 120.4(2) . . ? C5 C4 C7 122.0(2) . . ? C6 C5 C4 122.2(2) . . ? C5 C6 C1 119.8(2) . . ? C5 C6 C23 119.6(2) . . ? C1 C6 C23 120.5(2) . . ? C4 C7 C8 112.9(2) . . ? C4 C7 C9 109.7(2) . . ? C8 C7 C9 109.5(2) . . ? C2 C10 C11 111.3(2) . . ? C2 C10 C17 111.6(2) . . ? C11 C10 C17 113.6(2) . . ? C12 C11 C16 118.4(2) . . ? C12 C11 C10 119.4(2) . . ? C16 C11 C10 122.2(2) . . ? C13 C12 C11 121.0(2) . . ? C14 C13 C12 120.0(3) . . ? C13 C14 C15 119.9(3) . . ? C14 C15 C16 119.9(3) . . ? C15 C16 C11 120.8(3) . . ? C18 C17 C22 118.1(3) . . ? C18 C17 C10 123.1(2) . . ? C22 C17 C10 118.7(2) . . ? C17 C18 C19 120.6(3) . . ? C20 C19 C18 120.4(3) . . ? C19 C20 C21 119.7(3) . . ? C22 C21 C20 119.9(3) . . ? C21 C22 C17 121.3(2) . . ? C30 C23 C6 111.5(2) . . ? C30 C23 C24 111.8(2) . . ? C6 C23 C24 112.9(2) . . ? C29 C24 C25 118.0(2) . . ? C29 C24 C23 122.1(2) . . ? C25 C24 C23 119.9(2) . . ? C26 C25 C24 121.1(3) . . ? C25 C26 C27 120.3(3) . . ? C28 C27 C26 119.2(3) . . ? C27 C28 C29 120.6(3) . . ? C28 C29 C24 120.9(3) . . ? C35 C30 C31 118.1(3) . . ? C35 C30 C23 122.0(2) . . ? C31 C30 C23 119.9(2) . . ? C32 C31 C30 121.1(3) . . ? C33 C32 C31 119.8(3) . . ? C34 C33 C32 120.0(3) . . ? C33 C34 C35 120.2(3) . . ? C30 C35 C34 120.7(3) . . ? C38 C36 C37 109.2(2) . . ? C38 C36 Si1 117.61(19) . . ? C37 C36 Si1 111.2(2) . . ? C41 C39 C40 109.5(3) . . ? C41 C39 Si1 114.2(2) . . ? C40 C39 Si1 116.8(2) . . ? C44 C42 C43 109.9(2) . . ? C44 C42 Si1 113.5(2) . . ? C43 C42 Si1 114.06(19) . . ? C47 C46 C51 115.9(7) . . ? C47 C46 C45 119.0(7) . . ? C51 C46 C45 125.1(7) . . ? C46 C47 C48 124.0(7) . . ? C49 C48 C47 121.2(7) . . ? C48 C49 C50 113.9(7) . . ? C51 C50 C49 125.4(9) . . ? C46 C51 C50 119.4(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.752 _refine_diff_density_min -1.309 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 977197'