# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Chuluo Yang' _publ_contact_author_email CLYANG@WHU.EDU.CN _publ_section_title ; Bridged Triphenylamine as Novel Host Material for Highly Efficient Blue and Green Phosphorescent OLEDs ; loop_ _publ_author_name 'Chuluo Yang' 'Yonghua Chen' 'Cong Fan' 'Zuoquan Jiang' 'Dongge Ma' ; Jingui Qin ; 'Youtian Tao' 'Qi Wang' 'Zhiqiang Zhang' # Attachment '080521dm.cif' data_h:\080521e\work\080521dm _database_code_depnum_ccdc_archive 'CCDC 714843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H83 N O2 Si2' _chemical_formula_weight 1290.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6954(5) _cell_length_b 19.5226(5) _cell_length_c 26.3298(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.2890(10) _cell_angle_gamma 90.00 _cell_volume 7492.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7992 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 19.92 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59952 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.05 _reflns_number_total 13230 _reflns_number_gt 6801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13230 _refine_ls_number_parameters 914 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.924 _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 C1 C 0.4151(2) 0.30851(17) 0.26236(13) 0.0708(9) Uani 1 1 d . . . C2 C 0.3598(3) 0.2689(2) 0.22834(13) 0.0914(11) Uani 1 1 d . . . H2 H 0.2971 0.2774 0.2237 0.110 Uiso 1 1 calc R . . C3 C 0.3944(4) 0.2164(2) 0.20044(17) 0.1233(16) Uani 1 1 d . . . H3 H 0.3555 0.1901 0.1776 0.148 Uiso 1 1 calc R . . C4 C 0.4867(5) 0.2045(3) 0.2074(3) 0.143(2) Uani 1 1 d . . . H4 H 0.5103 0.1685 0.1899 0.171 Uiso 1 1 calc R . . C5 C 0.5449(4) 0.2441(3) 0.2392(3) 0.144(2) Uani 1 1 d . . . H5 H 0.6080 0.2371 0.2426 0.173 Uiso 1 1 calc R . . C6 C 0.5075(3) 0.2949(2) 0.26632(17) 0.1044(13) Uani 1 1 d . . . H6 H 0.5470 0.3216 0.2886 0.125 Uiso 1 1 calc R . . C7 C 0.34247(19) 0.45663(16) 0.26627(11) 0.0610(8) Uani 1 1 d . . . C8 C 0.3597(2) 0.46312(19) 0.21564(12) 0.0748(9) Uani 1 1 d . . . H8 H 0.3805 0.4251 0.1993 0.090 Uiso 1 1 calc R . . C9 C 0.3470(3) 0.5233(2) 0.18910(14) 0.0915(11) Uani 1 1 d . . . H9 H 0.3602 0.5258 0.1555 0.110 Uiso 1 1 calc R . . C10 C 0.3153(3) 0.5791(2) 0.21169(18) 0.1016(13) Uani 1 1 d . . . H10 H 0.3061 0.6200 0.1936 0.122 Uiso 1 1 calc R . . C11 C 0.2969(3) 0.57521(19) 0.26131(18) 0.1018(13) Uani 1 1 d . . . H11 H 0.2751 0.6135 0.2770 0.122 Uiso 1 1 calc R . . C12 C 0.3105(2) 0.51475(18) 0.28784(14) 0.0817(10) Uani 1 1 d . . . H12 H 0.2977 0.5130 0.3215 0.098 Uiso 1 1 calc R . . C13 C 0.4521(2) 0.3916(2) 0.35984(12) 0.0763(10) Uani 1 1 d . . . C14 C 0.4850(3) 0.4565(3) 0.37258(16) 0.1243(17) Uani 1 1 d . . . H14 H 0.4665 0.4934 0.3515 0.149 Uiso 1 1 calc R . . C15 C 0.5458(5) 0.4665(5) 0.4168(3) 0.206(3) Uani 1 1 d . . . H15 H 0.5663 0.5103 0.4260 0.247 Uiso 1 1 calc R . . C16 C 0.5758(5) 0.4110(5) 0.4470(2) 0.203(4) Uani 1 1 d . . . H16 H 0.6191 0.4177 0.4755 0.243 Uiso 1 1 calc R . . C17 C 0.5436(4) 0.3475(4) 0.43609(19) 0.152(2) Uani 1 1 d . . . H17 H 0.5621 0.3108 0.4574 0.183 Uiso 1 1 calc R . . C18 C 0.4827(3) 0.3384(3) 0.39251(15) 0.1049(13) Uani 1 1 d . . . H18 H 0.4610 0.2945 0.3846 0.126 Uiso 1 1 calc R . . C19 C 0.26228(19) 0.33884(14) 0.32614(10) 0.0505(7) Uani 1 1 d . . . C20 C 0.26190(18) 0.26986(14) 0.34065(10) 0.0503(7) Uani 1 1 d . . . H20 H 0.3096 0.2421 0.3327 0.060 Uiso 1 1 calc R . . C21 C 0.19452(17) 0.24038(13) 0.36616(9) 0.0473(7) Uani 1 1 d . . . C22 C 0.12353(18) 0.28300(14) 0.37774(10) 0.0483(7) Uani 1 1 d . . . C23 C 0.11841(19) 0.35035(14) 0.36134(11) 0.0556(7) Uani 1 1 d . . . H23 H 0.0686 0.3772 0.3673 0.067 Uiso 1 1 calc R . . C24 C 0.18640(19) 0.37802(14) 0.33628(10) 0.0558(7) Uani 1 1 d . . . H24 H 0.1821 0.4235 0.3258 0.067 Uiso 1 1 calc R . . C25 C 0.19799(17) 0.16581(13) 0.38346(10) 0.0490(7) Uani 1 1 d . . . C26 C 0.25148(19) 0.12328(14) 0.34750(11) 0.0538(7) Uani 1 1 d . . . C27 C 0.3348(2) 0.09426(18) 0.36149(13) 0.0788(10) Uani 1 1 d . . . H27 H 0.3605 0.0960 0.3956 0.095 Uiso 1 1 calc R . . C28 C 0.3827(2) 0.0619(2) 0.32578(17) 0.0994(13) Uani 1 1 d . . . H28 H 0.4401 0.0432 0.3367 0.119 Uiso 1 1 calc R . . C29 C 0.3482(3) 0.05687(19) 0.27567(15) 0.0831(10) Uani 1 1 d . . . C30 C 0.2627(2) 0.08423(18) 0.26137(13) 0.0784(10) Uani 1 1 d . . . H30 H 0.2362 0.0807 0.2275 0.094 Uiso 1 1 calc R . . C31 C 0.2155(2) 0.11679(16) 0.29643(12) 0.0657(8) Uani 1 1 d . . . H31 H 0.1578 0.1350 0.2855 0.079 Uiso 1 1 calc R . . C32 C 0.4018(3) 0.0225(2) 0.23689(16) 0.1235(16) Uani 1 1 d . . . H32A H 0.4603 0.0444 0.2374 0.185 Uiso 1 1 calc R . . H32B H 0.3681 0.0264 0.2033 0.185 Uiso 1 1 calc R . . H32C H 0.4106 -0.0251 0.2455 0.185 Uiso 1 1 calc R . . C33 C 0.24609(19) 0.16062(15) 0.43966(11) 0.0556(7) Uani 1 1 d . . . C34 C 0.2330(3) 0.10503(19) 0.46963(14) 0.0845(10) Uani 1 1 d . . . H34 H 0.1911 0.0715 0.4572 0.101 Uiso 1 1 calc R . . C35 C 0.2811(3) 0.0980(2) 0.51790(15) 0.0952(12) Uani 1 1 d . . . H35 H 0.2716 0.0591 0.5369 0.114 Uiso 1 1 calc R . . C36 C 0.3419(3) 0.1461(2) 0.53881(13) 0.0815(10) Uani 1 1 d . . . C37 C 0.3548(3) 0.2010(2) 0.50888(14) 0.0947(12) Uani 1 1 d . . . H37 H 0.3967 0.2345 0.5214 0.114 Uiso 1 1 calc R . . C38 C 0.3074(2) 0.20853(18) 0.46029(13) 0.0779(10) Uani 1 1 d . . . H38 H 0.3177 0.2473 0.4413 0.094 Uiso 1 1 calc R . . C39 C 0.3917(3) 0.1370(3) 0.59180(14) 0.1286(17) Uani 1 1 d . . . H39A H 0.3482 0.1364 0.6161 0.193 Uiso 1 1 calc R . . H39B H 0.4339 0.1742 0.5996 0.193 Uiso 1 1 calc R . . H39C H 0.4249 0.0945 0.5936 0.193 Uiso 1 1 calc R . . C40 C 0.09898(18) 0.13972(14) 0.38201(10) 0.0535(7) Uani 1 1 d . . . C41 C 0.0759(2) 0.07149(14) 0.37383(11) 0.0609(8) Uani 1 1 d . . . H41 H 0.1201 0.0415 0.3647 0.073 Uiso 1 1 calc R . . C42 C -0.0113(2) 0.04608(15) 0.37883(12) 0.0628(8) Uani 1 1 d . A . C43 C -0.0765(2) 0.09319(15) 0.39015(11) 0.0623(8) Uani 1 1 d . . . H43 H -0.1355 0.0777 0.3928 0.075 Uiso 1 1 calc R . . C44 C -0.05795(18) 0.16187(14) 0.39759(10) 0.0528(7) Uani 1 1 d . . . C45 C 0.03153(18) 0.18464(14) 0.39418(10) 0.0507(7) Uani 1 1 d . . . C46 C -0.0319(2) -0.03081(17) 0.37480(16) 0.0855(11) Uani 1 1 d D . . C47 C 0.0474(5) -0.0731(4) 0.3622(5) 0.111(4) Uani 0.645(12) 1 d PD A 1 H47A H 0.1022 -0.0590 0.3833 0.167 Uiso 0.645(12) 1 calc PR A 1 H47B H 0.0549 -0.0669 0.3268 0.167 Uiso 0.645(12) 1 calc PR A 1 H47C H 0.0357 -0.1206 0.3684 0.167 Uiso 0.645(12) 1 calc PR A 1 C48 C -0.1161(6) -0.0467(4) 0.3417(5) 0.144(6) Uani 0.645(12) 1 d PD A 1 H48A H -0.1057 -0.0427 0.3066 0.216 Uiso 0.645(12) 1 calc PR A 1 H48B H -0.1633 -0.0153 0.3484 0.216 Uiso 0.645(12) 1 calc PR A 1 H48C H -0.1348 -0.0926 0.3483 0.216 Uiso 0.645(12) 1 calc PR A 1 C49 C -0.0438(9) -0.0537(4) 0.4315(3) 0.144(5) Uani 0.645(12) 1 d PD A 1 H49A H -0.0549 -0.1021 0.4321 0.217 Uiso 0.645(12) 1 calc PR A 1 H49B H -0.0947 -0.0297 0.4426 0.217 Uiso 0.645(12) 1 calc PR A 1 H49C H 0.0111 -0.0430 0.4539 0.217 Uiso 0.645(12) 1 calc PR A 1 C47' C -0.1228(9) -0.0490(7) 0.3893(8) 0.120(7) Uani 0.355(12) 1 d PD A 2 H47D H -0.1305 -0.0978 0.3879 0.180 Uiso 0.355(12) 1 calc PR A 2 H47E H -0.1700 -0.0277 0.3660 0.180 Uiso 0.355(12) 1 calc PR A 2 H47F H -0.1270 -0.0332 0.4235 0.180 Uiso 0.355(12) 1 calc PR A 2 C48' C -0.0389(18) -0.0459(8) 0.3152(4) 0.168(12) Uani 0.355(12) 1 d PD A 2 H48D H 0.0177 -0.0336 0.3030 0.252 Uiso 0.355(12) 1 calc PR A 2 H48E H -0.0881 -0.0195 0.2974 0.252 Uiso 0.355(12) 1 calc PR A 2 H48F H -0.0507 -0.0938 0.3091 0.252 Uiso 0.355(12) 1 calc PR A 2 C49' C 0.0420(10) -0.0733(9) 0.4007(8) 0.124(8) Uani 0.355(12) 1 d PD A 2 H49D H 0.0613 -0.1058 0.3769 0.187 Uiso 0.355(12) 1 calc PR A 2 H49E H 0.0202 -0.0972 0.4286 0.187 Uiso 0.355(12) 1 calc PR A 2 H49F H 0.0929 -0.0447 0.4135 0.187 Uiso 0.355(12) 1 calc PR A 2 C50 C -0.13018(18) 0.21612(14) 0.40694(10) 0.0517(7) Uani 1 1 d . . . C51 C -0.16323(19) 0.25416(15) 0.35634(11) 0.0549(7) Uani 1 1 d . . . C52 C -0.1524(2) 0.22875(18) 0.30914(13) 0.0761(9) Uani 1 1 d . . . H52 H -0.1254 0.1860 0.3065 0.091 Uiso 1 1 calc R . . C53 C -0.1811(3) 0.2658(2) 0.26500(14) 0.0969(12) Uani 1 1 d . . . H53 H -0.1718 0.2474 0.2335 0.116 Uiso 1 1 calc R . . C54 C -0.2230(3) 0.3291(2) 0.26618(16) 0.0911(11) Uani 1 1 d . . . C55 C -0.2352(3) 0.35262(19) 0.31365(16) 0.0956(12) Uani 1 1 d . . . H55 H -0.2643 0.3945 0.3164 0.115 Uiso 1 1 calc R . . C56 C -0.2062(2) 0.31682(18) 0.35717(13) 0.0794(10) Uani 1 1 d . . . H56 H -0.2158 0.3354 0.3886 0.095 Uiso 1 1 calc R . . C57 C -0.2519(4) 0.3683(3) 0.21719(16) 0.1396(18) Uani 1 1 d . . . H57A H -0.3156 0.3597 0.2059 0.209 Uiso 1 1 calc R . . H57B H -0.2158 0.3535 0.1913 0.209 Uiso 1 1 calc R . . H57C H -0.2427 0.4164 0.2233 0.209 Uiso 1 1 calc R . . C58 C -0.2110(2) 0.18152(14) 0.42924(12) 0.0564(8) Uani 1 1 d . . . C59 C -0.2997(2) 0.18387(17) 0.40638(13) 0.0710(9) Uani 1 1 d . . . H59 H -0.3144 0.2084 0.3762 0.085 Uiso 1 1 calc R . . C60 C -0.3684(2) 0.1496(2) 0.42822(18) 0.0953(12) Uani 1 1 d . . . H60 H -0.4283 0.1517 0.4119 0.114 Uiso 1 1 calc R . . C61 C -0.3514(3) 0.1134(2) 0.4722(2) 0.0962(13) Uani 1 1 d . . . C62 C -0.2622(3) 0.11130(18) 0.49552(16) 0.0902(11) Uani 1 1 d . . . H62 H -0.2482 0.0865 0.5257 0.108 Uiso 1 1 calc R . . C63 C -0.1930(2) 0.14546(16) 0.47485(14) 0.0739(9) Uani 1 1 d . . . H63 H -0.1335 0.1442 0.4918 0.089 Uiso 1 1 calc R . . C64 C -0.4270(3) 0.0750(3) 0.4949(2) 0.162(2) Uani 1 1 d . . . H64A H -0.4820 0.1021 0.4910 0.243 Uiso 1 1 calc R . . H64B H -0.4081 0.0667 0.5307 0.243 Uiso 1 1 calc R . . H64C H -0.4386 0.0321 0.4775 0.243 Uiso 1 1 calc R . . C65 C -0.08328(18) 0.26959(13) 0.44390(10) 0.0496(7) Uani 1 1 d . . . C66 C 0.00510(18) 0.29068(13) 0.43745(10) 0.0498(7) Uani 1 1 d . . . C67 C 0.04653(19) 0.34354(15) 0.46677(11) 0.0588(8) Uani 1 1 d . . . H67 H 0.1059 0.3571 0.4627 0.071 Uiso 1 1 calc R . . C68 C -0.0003(2) 0.37628(15) 0.50209(11) 0.0625(8) Uani 1 1 d . . . H68 H 0.0282 0.4121 0.5212 0.075 Uiso 1 1 calc R . . C69 C -0.08885(19) 0.35746(14) 0.51012(10) 0.0547(7) Uani 1 1 d . . . C70 C -0.12794(18) 0.30379(14) 0.48032(10) 0.0518(7) Uani 1 1 d . . . H70 H -0.1869 0.2899 0.4848 0.062 Uiso 1 1 calc R . . C71 C -0.2477(2) 0.35017(19) 0.57353(11) 0.0709(9) Uani 1 1 d . . . C72 C -0.2303(3) 0.2817(2) 0.58471(14) 0.1047(13) Uani 1 1 d . . . H72 H -0.1717 0.2642 0.5838 0.126 Uiso 1 1 calc R . . C73 C -0.3008(5) 0.2383(3) 0.59740(18) 0.150(2) Uani 1 1 d . . . H73 H -0.2894 0.1919 0.6035 0.179 Uiso 1 1 calc R . . C74 C -0.3848(5) 0.2644(5) 0.6006(2) 0.161(3) Uani 1 1 d . . . H74 H -0.4305 0.2363 0.6105 0.193 Uiso 1 1 calc R . . C75 C -0.4031(4) 0.3305(4) 0.5899(2) 0.148(2) Uani 1 1 d . . . H75 H -0.4617 0.3475 0.5916 0.178 Uiso 1 1 calc R . . C76 C -0.3363(3) 0.3727(2) 0.57648(13) 0.0978(13) Uani 1 1 d . . . H76 H -0.3507 0.4183 0.5690 0.117 Uiso 1 1 calc R . . C77 C -0.20597(19) 0.48428(16) 0.51948(11) 0.0610(8) Uani 1 1 d . . . C78 C -0.2543(2) 0.53316(19) 0.54393(14) 0.0774(9) Uani 1 1 d . . . H78 H -0.2601 0.5273 0.5784 0.093 Uiso 1 1 calc R . . C79 C -0.2934(3) 0.5892(2) 0.5192(2) 0.0997(12) Uani 1 1 d . . . H79 H -0.3256 0.6204 0.5368 0.120 Uiso 1 1 calc R . . C80 C -0.2856(3) 0.5999(2) 0.4683(2) 0.1092(14) Uani 1 1 d . . . H80 H -0.3133 0.6376 0.4511 0.131 Uiso 1 1 calc R . . C81 C -0.2360(3) 0.5537(3) 0.44305(17) 0.1011(12) Uani 1 1 d . . . H81 H -0.2278 0.5613 0.4091 0.121 Uiso 1 1 calc R . . C82 C -0.1987(2) 0.49654(19) 0.46816(13) 0.0787(10) Uani 1 1 d . . . H82 H -0.1677 0.4650 0.4502 0.094 Uiso 1 1 calc R . . C83 C -0.0804(2) 0.43632(16) 0.61268(11) 0.0640(8) Uani 1 1 d . . . C84 C -0.0878(3) 0.4109(2) 0.66105(13) 0.0896(11) Uani 1 1 d . . . H84 H -0.1321 0.3779 0.6649 0.108 Uiso 1 1 calc R . . C85 C -0.0313(4) 0.4332(3) 0.70392(16) 0.1214(16) Uani 1 1 d . . . H85 H -0.0385 0.4157 0.7360 0.146 Uiso 1 1 calc R . . C86 C 0.0355(4) 0.4811(3) 0.6992(2) 0.1167(16) Uani 1 1 d . . . H86 H 0.0741 0.4958 0.7279 0.140 Uiso 1 1 calc R . . C87 C 0.0444(3) 0.5068(2) 0.65201(19) 0.0973(12) Uani 1 1 d . . . H87 H 0.0894 0.5393 0.6484 0.117 Uiso 1 1 calc R . . C88 C -0.0126(2) 0.48510(18) 0.60966(13) 0.0760(9) Uani 1 1 d . . . H88 H -0.0055 0.5037 0.5779 0.091 Uiso 1 1 calc R . . N1 N 0.05285(14) 0.25411(11) 0.40267(8) 0.0524(6) Uani 1 1 d . . . Si1 Si 0.36677(6) 0.37466(4) 0.30239(3) 0.0572(3) Uani 1 1 d . . . Si2 Si -0.15552(6) 0.40671(4) 0.55406(3) 0.0581(3) Uani 1 1 d . . . C89 C -0.0461(5) 0.2547(4) 0.1615(3) 0.228(4) Uani 1 1 d D . . H89A H -0.0367 0.2591 0.1263 0.342 Uiso 1 1 calc R . . H89B H -0.0795 0.2938 0.1714 0.342 Uiso 1 1 calc R . . H89C H -0.0806 0.2138 0.1659 0.342 Uiso 1 1 calc R . . C90 C 0.0435(6) 0.2508(3) 0.1938(3) 0.183(3) Uani 1 1 d D . . C91 C 0.1225(7) 0.2135(5) 0.1192(3) 0.296(6) Uani 1 1 d D . . H91A H 0.0661 0.1922 0.1037 0.356 Uiso 1 1 calc R . . H91B H 0.1668 0.1769 0.1266 0.356 Uiso 1 1 calc R . . C92 C 0.1542(6) 0.2540(3) 0.0811(3) 0.229(4) Uani 1 1 d D . . H92A H 0.1038 0.2790 0.0632 0.344 Uiso 1 1 calc R . . H92B H 0.1809 0.2251 0.0575 0.344 Uiso 1 1 calc R . . H92C H 0.1995 0.2856 0.0966 0.344 Uiso 1 1 calc R . . O2 O 0.1052(4) 0.2386(3) 0.1655(3) 0.258(4) Uani 1 1 d D . . O1 O 0.0560(5) 0.2758(4) 0.2381(2) 0.294(4) Uani 1 1 d 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 C1 0.063(2) 0.079(2) 0.076(2) 0.0121(18) 0.0313(18) -0.0030(19) C2 0.095(3) 0.105(3) 0.079(2) -0.019(2) 0.031(2) -0.005(2) C3 0.158(5) 0.114(4) 0.109(3) -0.026(3) 0.062(3) -0.008(3) C4 0.169(6) 0.097(4) 0.188(6) -0.011(4) 0.123(5) 0.008(4) C5 0.114(4) 0.116(4) 0.217(6) 0.008(4) 0.085(5) 0.022(4) C6 0.076(3) 0.103(3) 0.142(4) -0.005(3) 0.047(3) 0.007(2) C7 0.0522(19) 0.071(2) 0.0614(19) 0.0011(16) 0.0137(15) -0.0169(16) C8 0.075(2) 0.088(3) 0.061(2) 0.0093(18) 0.0095(17) -0.0109(19) C9 0.103(3) 0.102(3) 0.070(2) 0.027(2) 0.010(2) -0.010(3) C10 0.102(3) 0.085(3) 0.120(4) 0.034(3) 0.019(3) -0.009(2) C11 0.115(3) 0.063(2) 0.136(4) 0.007(2) 0.050(3) -0.006(2) C12 0.094(3) 0.069(2) 0.090(2) 0.003(2) 0.040(2) -0.017(2) C13 0.059(2) 0.107(3) 0.063(2) 0.013(2) 0.0113(16) -0.023(2) C14 0.120(4) 0.148(4) 0.096(3) 0.013(3) -0.021(3) -0.074(3) C15 0.198(7) 0.250(9) 0.149(5) 0.015(6) -0.056(5) -0.133(6) C16 0.167(6) 0.304(11) 0.117(4) 0.049(6) -0.064(4) -0.112(7) C17 0.104(4) 0.232(7) 0.108(4) 0.052(4) -0.033(3) -0.040(4) C18 0.071(3) 0.145(4) 0.093(3) 0.026(3) -0.012(2) -0.016(3) C19 0.0477(17) 0.0530(18) 0.0515(16) -0.0034(13) 0.0092(13) -0.0059(14) C20 0.0400(16) 0.0550(18) 0.0582(16) -0.0055(14) 0.0152(13) -0.0015(13) C21 0.0376(16) 0.0502(17) 0.0553(16) -0.0045(13) 0.0111(13) -0.0053(13) C22 0.0413(16) 0.0470(17) 0.0591(16) -0.0065(13) 0.0156(13) -0.0082(13) C23 0.0452(17) 0.0498(18) 0.0751(19) -0.0070(15) 0.0206(15) -0.0026(14) C24 0.0559(19) 0.0483(17) 0.0654(18) -0.0014(14) 0.0160(15) -0.0060(15) C25 0.0371(16) 0.0502(17) 0.0621(17) -0.0028(13) 0.0153(13) -0.0023(13) C26 0.0391(17) 0.0540(18) 0.070(2) -0.0040(14) 0.0147(15) -0.0018(14) C27 0.053(2) 0.098(3) 0.085(2) -0.0158(19) 0.0082(18) 0.0150(19) C28 0.058(2) 0.125(3) 0.117(3) -0.028(3) 0.016(2) 0.032(2) C29 0.065(2) 0.089(3) 0.100(3) -0.029(2) 0.028(2) 0.002(2) C30 0.067(2) 0.088(3) 0.083(2) -0.0216(19) 0.0202(19) -0.009(2) C31 0.0508(19) 0.071(2) 0.077(2) -0.0100(17) 0.0137(17) 0.0045(16) C32 0.098(3) 0.139(4) 0.143(4) -0.055(3) 0.053(3) 0.010(3) C33 0.0465(18) 0.0536(18) 0.0707(19) 0.0003(15) 0.0229(15) -0.0007(15) C34 0.083(3) 0.085(3) 0.084(2) 0.021(2) 0.008(2) -0.022(2) C35 0.093(3) 0.103(3) 0.093(3) 0.035(2) 0.023(2) -0.009(2) C36 0.085(3) 0.097(3) 0.064(2) 0.006(2) 0.0168(19) 0.001(2) C37 0.113(3) 0.088(3) 0.077(2) 0.004(2) -0.009(2) -0.023(2) C38 0.091(3) 0.069(2) 0.072(2) 0.0076(17) 0.0031(19) -0.019(2) C39 0.154(4) 0.158(4) 0.070(2) 0.019(3) 0.000(3) -0.010(3) C40 0.0436(17) 0.0500(18) 0.0696(18) -0.0035(14) 0.0180(14) -0.0027(14) C41 0.0500(19) 0.0472(18) 0.089(2) -0.0036(15) 0.0215(16) 0.0032(15) C42 0.0525(19) 0.0483(18) 0.090(2) -0.0067(15) 0.0192(16) -0.0074(15) C43 0.0441(18) 0.0535(19) 0.093(2) -0.0112(16) 0.0223(16) -0.0132(15) C44 0.0413(17) 0.0482(18) 0.0719(18) -0.0091(14) 0.0191(14) -0.0068(13) C45 0.0424(17) 0.0450(17) 0.0674(17) -0.0057(13) 0.0175(14) -0.0038(13) C46 0.073(3) 0.049(2) 0.139(3) -0.003(2) 0.033(3) -0.0022(19) C47 0.087(5) 0.047(4) 0.201(11) -0.017(7) 0.027(7) 0.006(4) C48 0.083(7) 0.071(5) 0.263(16) -0.050(9) -0.041(9) -0.013(5) C49 0.190(13) 0.068(5) 0.186(9) 0.007(5) 0.062(9) -0.022(6) C47' 0.096(12) 0.065(8) 0.20(2) -0.004(12) 0.035(15) -0.037(7) C48' 0.27(3) 0.087(11) 0.150(14) -0.047(10) 0.042(17) -0.071(17) C49' 0.127(15) 0.072(9) 0.166(18) 0.023(13) -0.018(14) -0.006(9) C50 0.0416(16) 0.0483(16) 0.0676(18) -0.0112(14) 0.0161(14) -0.0072(13) C51 0.0433(17) 0.0542(18) 0.0693(19) -0.0124(15) 0.0149(14) -0.0117(14) C52 0.074(2) 0.083(2) 0.075(2) -0.011(2) 0.0226(18) 0.0063(19) C53 0.101(3) 0.128(4) 0.064(2) -0.008(2) 0.020(2) -0.002(3) C54 0.090(3) 0.085(3) 0.095(3) 0.009(2) 0.000(2) -0.008(2) C55 0.114(3) 0.070(2) 0.095(3) -0.013(2) -0.016(2) 0.008(2) C56 0.093(3) 0.069(2) 0.072(2) -0.0170(19) -0.0068(19) 0.012(2) C57 0.173(5) 0.142(4) 0.097(3) 0.035(3) -0.006(3) -0.004(4) C58 0.0435(19) 0.0494(17) 0.081(2) -0.0155(16) 0.0252(16) -0.0087(14) C59 0.044(2) 0.079(2) 0.092(2) -0.0231(18) 0.0197(18) -0.0142(17) C60 0.047(2) 0.109(3) 0.135(3) -0.027(3) 0.030(2) -0.020(2) C61 0.078(3) 0.075(3) 0.148(4) -0.018(3) 0.060(3) -0.027(2) C62 0.084(3) 0.077(2) 0.118(3) 0.009(2) 0.046(2) -0.015(2) C63 0.060(2) 0.064(2) 0.100(3) 0.0074(19) 0.0226(19) -0.0124(17) C64 0.114(4) 0.135(4) 0.262(6) -0.004(4) 0.115(4) -0.047(3) C65 0.0418(17) 0.0509(17) 0.0575(16) -0.0030(13) 0.0111(13) -0.0058(13) C66 0.0431(17) 0.0452(16) 0.0642(17) -0.0067(13) 0.0193(14) -0.0070(13) C67 0.0430(17) 0.0625(19) 0.0734(19) -0.0132(16) 0.0170(15) -0.0148(15) C68 0.0582(19) 0.0640(19) 0.0678(18) -0.0180(15) 0.0186(15) -0.0201(16) C69 0.0514(18) 0.0589(18) 0.0553(16) -0.0083(14) 0.0128(14) -0.0136(15) C70 0.0403(16) 0.0557(18) 0.0619(17) -0.0068(14) 0.0166(14) -0.0079(14) C71 0.075(3) 0.088(3) 0.0521(18) -0.0102(17) 0.0193(17) -0.020(2) C72 0.138(4) 0.093(3) 0.094(3) 0.002(2) 0.053(3) -0.031(3) C73 0.229(7) 0.120(4) 0.118(4) -0.011(3) 0.093(4) -0.074(5) C74 0.169(6) 0.207(7) 0.120(4) -0.018(4) 0.074(4) -0.113(6) C75 0.101(4) 0.216(7) 0.138(4) 0.016(5) 0.053(3) -0.059(5) C76 0.074(3) 0.140(4) 0.085(2) 0.001(2) 0.031(2) -0.028(3) C77 0.0487(18) 0.073(2) 0.0626(19) -0.0144(16) 0.0124(14) -0.0155(16) C78 0.067(2) 0.079(2) 0.085(2) -0.019(2) 0.0063(19) -0.006(2) C79 0.074(3) 0.082(3) 0.142(4) -0.010(3) 0.009(3) 0.001(2) C80 0.074(3) 0.086(3) 0.159(5) 0.023(3) -0.018(3) -0.005(2) C81 0.086(3) 0.108(3) 0.106(3) 0.031(3) 0.003(2) -0.009(3) C82 0.071(2) 0.086(3) 0.080(2) -0.001(2) 0.0119(18) -0.012(2) C83 0.062(2) 0.064(2) 0.067(2) -0.0121(16) 0.0106(16) 0.0032(17) C84 0.097(3) 0.107(3) 0.064(2) -0.004(2) 0.008(2) -0.006(2) C85 0.153(5) 0.136(4) 0.068(3) -0.005(3) -0.014(3) 0.001(4) C86 0.108(4) 0.121(4) 0.108(4) -0.037(3) -0.037(3) 0.021(3) C87 0.074(3) 0.093(3) 0.121(3) -0.038(3) -0.004(3) 0.003(2) C88 0.072(2) 0.077(2) 0.077(2) -0.0205(18) 0.0041(19) -0.005(2) N1 0.0434(14) 0.0441(14) 0.0745(15) -0.0113(11) 0.0265(12) -0.0105(11) Si1 0.0488(5) 0.0691(6) 0.0555(5) 0.0040(4) 0.0141(4) -0.0092(4) Si2 0.0538(5) 0.0673(6) 0.0555(5) -0.0107(4) 0.0162(4) -0.0105(4) C89 0.314(11) 0.159(6) 0.184(6) -0.022(5) -0.070(7) -0.014(7) C90 0.228(10) 0.126(5) 0.199(8) -0.004(6) 0.045(9) -0.033(6) C91 0.369(16) 0.302(14) 0.226(10) -0.139(10) 0.069(10) -0.066(11) C92 0.268(9) 0.144(6) 0.305(11) -0.096(6) 0.148(9) -0.056(6) O2 0.202(5) 0.268(6) 0.330(8) -0.162(6) 0.129(5) -0.104(4) O1 0.325(9) 0.347(10) 0.196(5) 0.005(6) -0.025(6) -0.016(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 C1 C2 1.369(5) . ? C1 C6 1.374(5) . ? C1 Si1 1.864(3) . ? C2 C3 1.394(5) . ? C2 H2 0.9300 . ? C3 C4 1.365(7) . ? C3 H3 0.9300 . ? C4 C5 1.361(7) . ? C4 H4 0.9300 . ? C5 C6 1.376(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.378(4) . ? C7 C8 1.394(4) . ? C7 Si1 1.873(3) . ? C8 C9 1.367(5) . ? C8 H8 0.9300 . ? C9 C10 1.352(5) . ? C9 H9 0.9300 . ? C10 C11 1.370(5) . ? C10 H10 0.9300 . ? C11 C12 1.373(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.382(5) . ? C13 C18 1.386(5) . ? C13 Si1 1.867(3) . ? C14 C15 1.387(7) . ? C14 H14 0.9300 . ? C15 C16 1.384(9) . ? C15 H15 0.9300 . ? C16 C17 1.343(9) . ? C16 H16 0.9300 . ? C17 C18 1.375(6) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.400(4) . ? C19 C24 1.405(4) . ? C19 Si1 1.866(3) . ? C20 C21 1.390(3) . ? C20 H20 0.9300 . ? C21 C22 1.398(3) . ? C21 C25 1.524(4) . ? C22 C23 1.383(4) . ? C22 N1 1.415(3) . ? C23 C24 1.376(3) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C40 1.537(4) . ? C25 C26 1.547(4) . ? C25 C33 1.560(4) . ? C26 C27 1.357(4) . ? C26 C31 1.387(4) . ? C27 C28 1.396(4) . ? C27 H27 0.9300 . ? C28 C29 1.356(5) . ? C28 H28 0.9300 . ? C29 C30 1.373(5) . ? C29 C32 1.522(4) . ? C30 C31 1.378(4) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C38 1.363(4) . ? C33 C34 1.369(4) . ? C34 C35 1.380(5) . ? C34 H34 0.9300 . ? C35 C36 1.364(5) . ? C35 H35 0.9300 . ? C36 C37 1.357(5) . ? C36 C39 1.502(5) . ? C37 C38 1.385(5) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.385(4) . ? C40 C45 1.391(3) . ? C41 C42 1.395(4) . ? C41 H41 0.9300 . ? C42 C43 1.387(4) . ? C42 C46 1.532(4) . ? C43 C44 1.377(4) . ? C43 H43 0.9300 . ? C44 C45 1.402(3) . ? C44 C50 1.541(4) . ? C45 N1 1.403(3) . ? C46 C48 1.453(7) . ? C46 C49' 1.464(11) . ? C46 C47' 1.478(9) . ? C46 C47 1.499(7) . ? C46 C49 1.588(8) . ? C46 C48' 1.588(10) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C47' H47D 0.9600 . ? C47' H47E 0.9600 . ? C47' H47F 0.9600 . ? C48' H48D 0.9600 . ? C48' H48E 0.9600 . ? C48' H48F 0.9600 . ? C49' H49D 0.9600 . ? C49' H49E 0.9600 . ? C49' H49F 0.9600 . ? C50 C65 1.530(4) . ? C50 C58 1.545(4) . ? C50 C51 1.549(4) . ? C51 C52 1.366(4) . ? C51 C56 1.378(4) . ? C52 C53 1.389(5) . ? C52 H52 0.9300 . ? C53 C54 1.383(5) . ? C53 H53 0.9300 . ? C54 C55 1.364(5) . ? C54 C57 1.513(5) . ? C55 C56 1.364(5) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 C59 1.367(4) . ? C58 C63 1.388(4) . ? C59 C60 1.394(5) . ? C59 H59 0.9300 . ? C60 C61 1.352(5) . ? C60 H60 0.9300 . ? C61 C62 1.375(6) . ? C61 C64 1.526(5) . ? C62 C63 1.384(4) . ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.393(3) . ? C65 C70 1.399(3) . ? C66 C67 1.383(4) . ? C66 N1 1.416(3) . ? C67 C68 1.382(4) . ? C67 H67 0.9300 . ? C68 C69 1.393(4) . ? C68 H68 0.9300 . ? C69 C70 1.389(4) . ? C69 Si2 1.874(3) . ? C70 H70 0.9300 . ? C71 C72 1.385(5) . ? C71 C76 1.387(5) . ? C71 Si2 1.868(3) . ? C72 C73 1.411(6) . ? C72 H72 0.9300 . ? C73 C74 1.349(9) . ? C73 H73 0.9300 . ? C74 C75 1.340(9) . ? C74 H74 0.9300 . ? C75 C76 1.362(6) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C77 C82 1.390(4) . ? C77 C78 1.395(4) . ? C77 Si2 1.871(3) . ? C78 C79 1.363(5) . ? C78 H78 0.9300 . ? C79 C80 1.375(6) . ? C79 H79 0.9300 . ? C80 C81 1.382(6) . ? C80 H80 0.9300 . ? C81 C82 1.375(5) . ? C81 H81 0.9300 . ? C82 H82 0.9300 . ? C83 C84 1.384(4) . ? C83 C88 1.388(4) . ? C83 Si2 1.871(3) . ? C84 C85 1.384(6) . ? C84 H84 0.9300 . ? C85 C86 1.372(6) . ? C85 H85 0.9300 . ? C86 C87 1.362(6) . ? C86 H86 0.9300 . ? C87 C88 1.374(5) . ? C87 H87 0.9300 . ? C88 H88 0.9300 . ? C89 C90 1.477(7) . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 O1 1.255(6) . ? C90 O2 1.267(6) . ? C91 O2 1.367(6) . ? C91 C92 1.403(8) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? 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 116.0(4) . . ? C2 C1 Si1 121.6(3) . . ? C6 C1 Si1 122.3(3) . . ? C1 C2 C3 122.3(4) . . ? C1 C2 H2 118.8 . . ? C3 C2 H2 118.8 . . ? C4 C3 C2 118.5(5) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C5 C4 C3 121.4(5) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 117.9(5) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 121.0 . . ? C1 C6 C5 123.8(5) . . ? C1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? C12 C7 C8 115.6(3) . . ? C12 C7 Si1 123.2(2) . . ? C8 C7 Si1 121.2(3) . . ? C9 C8 C7 122.5(4) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 119.7(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 122.3(3) . . ? C11 C12 H12 118.9 . . ? C7 C12 H12 118.9 . . ? C14 C13 C18 117.3(4) . . ? C14 C13 Si1 122.5(3) . . ? C18 C13 Si1 120.1(3) . . ? C13 C14 C15 120.1(5) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 119.8(6) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 121.4(6) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 118.2(6) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? C17 C18 C13 123.2(5) . . ? C17 C18 H18 118.4 . . ? C13 C18 H18 118.4 . . ? C20 C19 C24 116.2(2) . . ? C20 C19 Si1 118.9(2) . . ? C24 C19 Si1 124.5(2) . . ? C21 C20 C19 123.9(2) . . ? C21 C20 H20 118.0 . . ? C19 C20 H20 118.0 . . ? C20 C21 C22 117.1(2) . . ? C20 C21 C25 122.8(2) . . ? C22 C21 C25 120.1(2) . . ? C23 C22 C21 120.7(2) . . ? C23 C22 N1 120.7(2) . . ? C21 C22 N1 118.4(2) . . ? C24 C23 C22 120.6(3) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C19 121.3(3) . . ? C23 C24 H24 119.4 . . ? C19 C24 H24 119.4 . . ? C21 C25 C40 108.3(2) . . ? C21 C25 C26 109.3(2) . . ? C40 C25 C26 111.1(2) . . ? C21 C25 C33 109.8(2) . . ? C40 C25 C33 108.4(2) . . ? C26 C25 C33 110.0(2) . . ? C27 C26 C31 116.4(3) . . ? C27 C26 C25 124.7(3) . . ? C31 C26 C25 118.8(3) . . ? C26 C27 C28 121.4(3) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C29 C28 C27 122.0(3) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C30 117.1(3) . . ? C28 C29 C32 121.5(4) . . ? C30 C29 C32 121.4(4) . . ? C29 C30 C31 121.1(3) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C30 C31 C26 122.0(3) . . ? C30 C31 H31 119.0 . . ? C26 C31 H31 119.0 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C38 C33 C34 116.6(3) . . ? C38 C33 C25 122.0(3) . . ? C34 C33 C25 121.2(3) . . ? C33 C34 C35 121.1(3) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C36 C35 C34 122.4(3) . . ? C36 C35 H35 118.8 . . ? C34 C35 H35 118.8 . . ? C37 C36 C35 116.2(3) . . ? C37 C36 C39 123.1(4) . . ? C35 C36 C39 120.7(4) . . ? C36 C37 C38 122.0(4) . . ? C36 C37 H37 119.0 . . ? C38 C37 H37 119.0 . . ? C33 C38 C37 121.6(3) . . ? C33 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C45 118.3(2) . . ? C41 C40 C25 122.4(2) . . ? C45 C40 C25 119.0(2) . . ? C40 C41 C42 122.5(3) . . ? C40 C41 H41 118.7 . . ? C42 C41 H41 118.7 . . ? C43 C42 C41 116.8(3) . . ? C43 C42 C46 121.9(3) . . ? C41 C42 C46 121.2(3) . . ? C44 C43 C42 123.2(3) . . ? C44 C43 H43 118.4 . . ? C42 C43 H43 118.4 . . ? C43 C44 C45 118.0(2) . . ? C43 C44 C50 124.3(2) . . ? C45 C44 C50 117.6(2) . . ? C40 C45 C44 121.1(2) . . ? C40 C45 N1 119.7(2) . . ? C44 C45 N1 119.2(2) . . ? C48 C46 C49' 133.1(9) . . ? C48 C46 C47' 51.4(6) . . ? C49' C46 C47' 112.6(8) . . ? C48 C46 C47 112.1(5) . . ? C49' C46 C47 40.5(7) . . ? C47' C46 C47 132.7(7) . . ? C48 C46 C42 113.3(4) . . ? C49' C46 C42 113.2(8) . . ? C47' C46 C42 113.2(6) . . ? C47 C46 C42 113.8(4) . . ? C48 C46 C49 108.5(6) . . ? C49' C46 C49 64.3(8) . . ? C47' C46 C49 58.6(7) . . ? C47 C46 C49 103.5(5) . . ? C42 C46 C49 104.8(4) . . ? C48 C46 C48' 54.8(7) . . ? C49' C46 C48' 107.9(8) . . ? C47' C46 C48' 105.3(8) . . ? C47 C46 C48' 68.5(8) . . ? C42 C46 C48' 103.8(6) . . ? C49 C46 C48' 151.1(6) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? C46 C47' H47D 109.5 . . ? C46 C47' H47E 109.5 . . ? H47D C47' H47E 109.5 . . ? C46 C47' H47F 109.5 . . ? H47D C47' H47F 109.5 . . ? H47E C47' H47F 109.5 . . ? C46 C48' H48D 109.5 . . ? C46 C48' H48E 109.5 . . ? H48D C48' H48E 109.5 . . ? C46 C48' H48F 109.5 . . ? H48D C48' H48F 109.5 . . ? H48E C48' H48F 109.5 . . ? C46 C49' H49D 109.5 . . ? C46 C49' H49E 109.5 . . ? H49D C49' H49E 109.5 . . ? C46 C49' H49F 109.5 . . ? H49D C49' H49F 109.5 . . ? H49E C49' H49F 109.5 . . ? C65 C50 C44 107.8(2) . . ? C65 C50 C58 111.2(2) . . ? C44 C50 C58 109.8(2) . . ? C65 C50 C51 106.7(2) . . ? C44 C50 C51 109.8(2) . . ? C58 C50 C51 111.4(2) . . ? C52 C51 C56 116.3(3) . . ? C52 C51 C50 123.3(3) . . ? C56 C51 C50 120.4(3) . . ? C51 C52 C53 120.9(3) . . ? C51 C52 H52 119.5 . . ? C53 C52 H52 119.5 . . ? C54 C53 C52 122.4(3) . . ? C54 C53 H53 118.8 . . ? C52 C53 H53 118.8 . . ? C55 C54 C53 115.6(4) . . ? C55 C54 C57 123.8(4) . . ? C53 C54 C57 120.6(4) . . ? C56 C55 C54 122.3(4) . . ? C56 C55 H55 118.9 . . ? C54 C55 H55 118.9 . . ? C55 C56 C51 122.5(3) . . ? C55 C56 H56 118.8 . . ? C51 C56 H56 118.8 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 C63 117.6(3) . . ? C59 C58 C50 123.7(3) . . ? C63 C58 C50 118.7(3) . . ? C58 C59 C60 120.2(4) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C61 C60 C59 122.6(4) . . ? C61 C60 H60 118.7 . . ? C59 C60 H60 118.7 . . ? C60 C61 C62 117.4(3) . . ? C60 C61 C64 121.9(5) . . ? C62 C61 C64 120.7(5) . . ? C61 C62 C63 121.0(4) . . ? C61 C62 H62 119.5 . . ? C63 C62 H62 119.5 . . ? C62 C63 C58 121.1(3) . . ? C62 C63 H63 119.5 . . ? C58 C63 H63 119.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 C70 117.9(2) . . ? C66 C65 C50 118.4(2) . . ? C70 C65 C50 123.3(2) . . ? C67 C66 C65 120.3(2) . . ? C67 C66 N1 121.2(2) . . ? C65 C66 N1 118.4(2) . . ? C68 C67 C66 119.9(3) . . ? C68 C67 H67 120.0 . . ? C66 C67 H67 120.0 . . ? C67 C68 C69 122.3(3) . . ? C67 C68 H68 118.8 . . ? C69 C68 H68 118.8 . . ? C70 C69 C68 116.1(2) . . ? C70 C69 Si2 121.7(2) . . ? C68 C69 Si2 122.0(2) . . ? C69 C70 C65 123.4(2) . . ? C69 C70 H70 118.3 . . ? C65 C70 H70 118.3 . . ? C72 C71 C76 116.3(4) . . ? C72 C71 Si2 120.6(3) . . ? C76 C71 Si2 123.2(3) . . ? C71 C72 C73 120.7(5) . . ? C71 C72 H72 119.7 . . ? C73 C72 H72 119.7 . . ? C74 C73 C72 119.5(6) . . ? C74 C73 H73 120.2 . . ? C72 C73 H73 120.2 . . ? C75 C74 C73 120.8(6) . . ? C75 C74 H74 119.6 . . ? C73 C74 H74 119.6 . . ? C74 C75 C76 120.3(6) . . ? C74 C75 H75 119.8 . . ? C76 C75 H75 119.8 . . ? C75 C76 C71 122.4(5) . . ? C75 C76 H76 118.8 . . ? C71 C76 H76 118.8 . . ? C82 C77 C78 115.9(3) . . ? C82 C77 Si2 122.6(3) . . ? C78 C77 Si2 121.5(2) . . ? C79 C78 C77 122.5(4) . . ? C79 C78 H78 118.7 . . ? C77 C78 H78 118.7 . . ? C78 C79 C80 120.3(4) . . ? C78 C79 H79 119.8 . . ? C80 C79 H79 119.8 . . ? C79 C80 C81 119.0(4) . . ? C79 C80 H80 120.5 . . ? C81 C80 H80 120.5 . . ? C82 C81 C80 120.0(4) . . ? C82 C81 H81 120.0 . . ? C80 C81 H81 120.0 . . ? C81 C82 C77 122.2(4) . . ? C81 C82 H82 118.9 . . ? C77 C82 H82 118.9 . . ? C84 C83 C88 116.1(3) . . ? C84 C83 Si2 122.8(3) . . ? C88 C83 Si2 121.1(2) . . ? C83 C84 C85 121.9(4) . . ? C83 C84 H84 119.1 . . ? C85 C84 H84 119.1 . . ? C86 C85 C84 120.2(4) . . ? C86 C85 H85 119.9 . . ? C84 C85 H85 119.9 . . ? C87 C86 C85 119.1(4) . . ? C87 C86 H86 120.4 . . ? C85 C86 H86 120.4 . . ? C86 C87 C88 120.5(4) . . ? C86 C87 H87 119.8 . . ? C88 C87 H87 119.8 . . ? C87 C88 C83 122.3(4) . . ? C87 C88 H88 118.9 . . ? C83 C88 H88 118.9 . . ? C45 N1 C22 118.3(2) . . ? C45 N1 C66 118.1(2) . . ? C22 N1 C66 123.5(2) . . ? C1 Si1 C19 108.58(14) . . ? C1 Si1 C13 108.42(17) . . ? C19 Si1 C13 106.93(12) . . ? C1 Si1 C7 111.51(14) . . ? C19 Si1 C7 112.24(13) . . ? C13 Si1 C7 108.99(16) . . ? C71 Si2 C77 110.82(15) . . ? C71 Si2 C83 109.15(14) . . ? C77 Si2 C83 107.89(14) . . ? C71 Si2 C69 108.67(14) . . ? C77 Si2 C69 108.72(13) . . ? C83 Si2 C69 111.60(13) . . ? C90 C89 H89A 109.5 . . ? C90 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C90 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? O1 C90 O2 126.0(8) . . ? O1 C90 C89 122.0(7) . . ? O2 C90 C89 108.8(7) . . ? O2 C91 C92 123.5(8) . . ? O2 C91 H91A 106.4 . . ? C92 C91 H91A 106.4 . . ? O2 C91 H91B 106.4 . . ? C92 C91 H91B 106.4 . . ? H91A C91 H91B 106.5 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C90 O2 C91 145.1(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.617 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.049