# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_mje1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '5 in manuscript' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 Cl2 N2 Si2' _chemical_formula_weight 609.81 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.5958(11) _cell_length_b 14.9387(10) _cell_length_c 16.2175(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.656(2) _cell_angle_gamma 90.00 _cell_volume 3495.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 2134 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9516 _exptl_absorpt_correction_T_max 0.9673 _exptl_absorpt_process_details ; Sheldrick, G. M. (2008). SADABS. University of G\"ottingen, Germany. ; _exptl_special_details ; THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.5161 RESPONSE: We have cut the dataset at a mean I/sigma of 1.32 at a resolution of 0.97 \%A. Despite of trying several crystals and long irradiation times this was the best achievable resolution. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10721 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 21.52 _reflns_number_total 4033 _reflns_number_gt 2372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4033 _refine_ls_number_parameters 388 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.995 _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 Si1 Si 0.95661(9) 0.12903(9) 0.29322(8) 0.0494(4) Uani 1 1 d . . . Si2 Si 1.58058(8) -0.32738(8) 0.17013(8) 0.0394(4) Uani 1 1 d . . . Cl1 Cl 1.16611(10) 0.08974(9) -0.03118(8) 0.0736(5) Uani 1 1 d . A . Cl2 Cl 1.33978(9) -0.02614(9) -0.06187(7) 0.0621(4) Uani 1 1 d . . . C1 C 1.1177(3) 0.0099(3) 0.2657(3) 0.0393(12) Uani 1 1 d . . . C2 C 1.0549(3) 0.0556(3) 0.2797(3) 0.0488(13) Uani 1 1 d . A . C3 C 1.4177(3) -0.2120(3) 0.2029(2) 0.0345(11) Uani 1 1 d . A . C4 C 1.4826(3) -0.2569(3) 0.1902(3) 0.0377(12) Uani 1 1 d . . . C11 C 1.1929(3) -0.0463(3) 0.2515(3) 0.0321(11) Uani 1 1 d . A . C12 C 1.2244(3) -0.0444(3) 0.1738(3) 0.0312(11) Uani 1 1 d . . . N13 N 1.1828(2) 0.0128(2) 0.1125(2) 0.0402(10) Uani 1 1 d . A . C14 C 1.2168(3) 0.0156(3) 0.0440(3) 0.0432(13) Uani 1 1 d . . . C15 C 1.2941(3) -0.0379(3) 0.0296(3) 0.0395(12) Uani 1 1 d . A . N16 N 1.3331(2) -0.0946(2) 0.0837(2) 0.0347(9) Uani 1 1 d . . . C17 C 1.2990(3) -0.0992(3) 0.1585(3) 0.0304(11) Uani 1 1 d . A . C18 C 1.3418(3) -0.1583(3) 0.2200(3) 0.0290(11) Uani 1 1 d . . . C19 C 1.3112(3) -0.1611(3) 0.2987(3) 0.0318(11) Uani 1 1 d . A . C20 C 1.3535(3) -0.2180(3) 0.3634(3) 0.0408(12) Uani 1 1 d . . . H20 H 1.4022 -0.2568 0.3534 0.049 Uiso 1 1 calc R A . C21 C 1.3253(3) -0.2177(3) 0.4396(3) 0.0497(13) Uani 1 1 d . A . H21 H 1.3543 -0.2562 0.4823 0.060 Uiso 1 1 calc R . . C22 C 1.2534(3) -0.1606(3) 0.4551(3) 0.0522(14) Uani 1 1 d . . . H22 H 1.2347 -0.1607 0.5087 0.063 Uiso 1 1 calc R A . C23 C 1.2105(3) -0.1056(3) 0.3954(3) 0.0451(13) Uani 1 1 d . A . H23 H 1.1618 -0.0678 0.4074 0.054 Uiso 1 1 calc R . . C24 C 1.2378(3) -0.1039(3) 0.3141(3) 0.0331(11) Uani 1 1 d . . . C31 C 1.0089(9) 0.2140(7) 0.3782(5) 0.052(3) Uani 0.662(17) 1 d PDU A 1 H31 H 1.0616 0.2442 0.3567 0.063 Uiso 0.662(17) 1 calc PR A 1 C32 C 0.9388(11) 0.2864(10) 0.3894(15) 0.069(4) Uani 0.662(17) 1 d PDU A 1 H32A H 0.8798 0.2587 0.3968 0.103 Uiso 0.662(17) 1 calc PR A 1 H32B H 0.9296 0.3250 0.3399 0.103 Uiso 0.662(17) 1 calc PR A 1 H32C H 0.9619 0.3224 0.4387 0.103 Uiso 0.662(17) 1 calc PR A 1 C33 C 1.0489(10) 0.1693(8) 0.4604(6) 0.084(4) Uani 0.662(17) 1 d PDU A 1 H33A H 1.0773 0.2148 0.4997 0.126 Uiso 0.662(17) 1 calc PR A 1 H33B H 1.0959 0.1254 0.4504 0.126 Uiso 0.662(17) 1 calc PR A 1 H33C H 0.9992 0.1390 0.4839 0.126 Uiso 0.662(17) 1 calc PR A 1 C34 C 0.9298(3) 0.1951(3) 0.1955(3) 0.0533(14) Uani 1 1 d D A . H34 H 0.8741 0.2325 0.2005 0.064 Uiso 1 1 calc R . . C35 C 1.0082(4) 0.2592(4) 0.1817(4) 0.094(2) Uani 1 1 d D . . H35A H 1.0648 0.2249 0.1789 0.142 Uiso 1 1 calc R A . H35B H 1.0192 0.3018 0.2281 0.142 Uiso 1 1 calc R . . H35C H 0.9905 0.2919 0.1293 0.142 Uiso 1 1 calc R . . C36 C 0.9050(4) 0.1355(4) 0.1190(3) 0.0833(18) Uani 1 1 d D . . H36A H 0.8892 0.1730 0.0693 0.125 Uiso 1 1 calc R A . H36B H 0.8519 0.0978 0.1262 0.125 Uiso 1 1 calc R . . H36C H 0.9581 0.0975 0.1123 0.125 Uiso 1 1 calc R . . C37 C 0.8576(3) 0.0509(4) 0.3049(4) 0.0823(19) Uani 1 1 d . A . H37 H 0.8529 0.0108 0.2550 0.099 Uiso 1 1 calc R . . C38 C 0.7644(3) 0.0981(4) 0.2961(3) 0.090(2) Uani 1 1 d . . . H38A H 0.7152 0.0538 0.2981 0.134 Uiso 1 1 calc R A . H38B H 0.7533 0.1299 0.2426 0.134 Uiso 1 1 calc R . . H38C H 0.7644 0.1410 0.3418 0.134 Uiso 1 1 calc R . . C39 C 0.8720(4) -0.0105(5) 0.3766(4) 0.117(2) Uani 1 1 d . . . H39A H 0.8754 0.0240 0.4284 0.175 Uiso 1 1 calc R A . H39B H 0.9300 -0.0435 0.3765 0.175 Uiso 1 1 calc R . . H39C H 0.8202 -0.0528 0.3727 0.175 Uiso 1 1 calc R . . C41 C 1.6908(3) -0.2810(3) 0.2305(3) 0.0542(14) Uani 1 1 d . . . H41 H 1.7423 -0.3205 0.2179 0.065 Uiso 1 1 calc R . . C42 C 1.6940(4) -0.2824(4) 0.3230(3) 0.091(2) Uani 1 1 d . . . H42A H 1.7546 -0.2608 0.3500 0.136 Uiso 1 1 calc R . . H42B H 1.6843 -0.3437 0.3414 0.136 Uiso 1 1 calc R . . H42C H 1.6452 -0.2435 0.3384 0.136 Uiso 1 1 calc R . . C43 C 1.7130(5) -0.1879(5) 0.2041(4) 0.128(3) Uani 1 1 d . . . H43A H 1.6637 -0.1469 0.2147 0.191 Uiso 1 1 calc R . . H43B H 1.7176 -0.1878 0.1444 0.191 Uiso 1 1 calc R . . H43C H 1.7721 -0.1685 0.2359 0.191 Uiso 1 1 calc R . . C44 C 1.5811(3) -0.3247(3) 0.0553(3) 0.0474(13) Uani 1 1 d . . . H44 H 1.5248 -0.3584 0.0295 0.057 Uiso 1 1 calc R . . C45 C 1.6649(4) -0.3751(4) 0.0304(3) 0.0784(18) Uani 1 1 d . . . H45A H 1.6614 -0.3742 -0.0304 0.118 Uiso 1 1 calc R . . H45B H 1.6643 -0.4372 0.0498 0.118 Uiso 1 1 calc R . . H45C H 1.7223 -0.3459 0.0561 0.118 Uiso 1 1 calc R . . C46 C 1.5730(3) -0.2307(3) 0.0160(3) 0.0646(16) Uani 1 1 d . . . H46A H 1.6308 -0.1977 0.0329 0.097 Uiso 1 1 calc R . . H46B H 1.5215 -0.1984 0.0350 0.097 Uiso 1 1 calc R . . H46C H 1.5614 -0.2360 -0.0449 0.097 Uiso 1 1 calc R . . C47 C 1.5564(3) -0.4438(3) 0.2060(3) 0.0466(13) Uani 1 1 d . . . H47 H 1.6174 -0.4754 0.2176 0.056 Uiso 1 1 calc R . . C48 C 1.4949(4) -0.4986(3) 0.1392(3) 0.0731(17) Uani 1 1 d . . . H48A H 1.4821 -0.5572 0.1622 0.110 Uiso 1 1 calc R . . H48B H 1.5270 -0.5069 0.0909 0.110 Uiso 1 1 calc R . . H48C H 1.4365 -0.4668 0.1220 0.110 Uiso 1 1 calc R . . C49 C 1.5140(3) -0.4457(3) 0.2876(3) 0.0638(16) Uani 1 1 d . . . H49A H 1.4533 -0.4162 0.2786 0.096 Uiso 1 1 calc R . . H49B H 1.5551 -0.4141 0.3315 0.096 Uiso 1 1 calc R . . H49C H 1.5067 -0.5079 0.3046 0.096 Uiso 1 1 calc R . . C31B C 0.9699(11) 0.1814(12) 0.3945(10) 0.032(5) Uiso 0.338(17) 1 d PDU A 2 H31B H 0.9439 0.1386 0.4325 0.039 Uiso 0.338(17) 1 calc PR A 2 C32B C 0.9174(19) 0.2697(17) 0.399(3) 0.078(13) Uiso 0.338(17) 1 d PDU A 2 H32D H 0.8986 0.2760 0.4539 0.117 Uiso 0.338(17) 1 calc PR A 2 H32E H 0.8623 0.2698 0.3559 0.117 Uiso 0.338(17) 1 calc PR A 2 H32F H 0.9578 0.3197 0.3889 0.117 Uiso 0.338(17) 1 calc PR A 2 C33B C 1.0730(10) 0.1927(14) 0.4294(15) 0.052(7) Uiso 0.338(17) 1 d PDU A 2 H33D H 1.1040 0.2254 0.3890 0.078 Uiso 0.338(17) 1 calc PR A 2 H33E H 1.1017 0.1337 0.4397 0.078 Uiso 0.338(17) 1 calc PR A 2 H33F H 1.0792 0.2264 0.4819 0.078 Uiso 0.338(17) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0445(9) 0.0608(10) 0.0442(9) -0.0008(7) 0.0105(7) 0.0251(8) Si2 0.0350(8) 0.0407(9) 0.0440(8) 0.0036(7) 0.0108(6) 0.0122(7) Cl1 0.0914(11) 0.0654(10) 0.0624(9) 0.0228(8) 0.0068(8) 0.0298(8) Cl2 0.0827(10) 0.0609(9) 0.0469(8) 0.0097(7) 0.0238(7) 0.0072(8) C1 0.035(3) 0.041(3) 0.043(3) -0.005(2) 0.010(2) 0.002(3) C2 0.043(3) 0.048(3) 0.057(3) -0.007(3) 0.010(3) 0.010(3) C3 0.038(3) 0.032(3) 0.036(3) 0.004(2) 0.010(2) 0.006(3) C4 0.042(3) 0.034(3) 0.040(3) 0.006(2) 0.013(2) 0.008(3) C11 0.027(3) 0.024(3) 0.046(3) -0.005(2) 0.010(2) -0.003(2) C12 0.030(3) 0.022(3) 0.041(3) -0.006(2) 0.006(2) 0.001(2) N13 0.039(2) 0.032(3) 0.049(3) 0.002(2) 0.004(2) 0.0061(19) C14 0.049(3) 0.033(3) 0.046(3) 0.006(3) 0.002(3) 0.005(3) C15 0.047(3) 0.039(3) 0.033(3) 0.000(3) 0.010(2) -0.002(3) N16 0.038(2) 0.031(2) 0.035(2) -0.002(2) 0.008(2) -0.0006(18) C17 0.032(3) 0.024(3) 0.037(3) -0.006(2) 0.010(2) -0.007(2) C18 0.029(3) 0.019(3) 0.040(3) -0.004(2) 0.009(2) -0.001(2) C19 0.032(3) 0.026(3) 0.039(3) -0.003(2) 0.011(2) -0.002(2) C20 0.045(3) 0.031(3) 0.048(3) 0.003(3) 0.012(3) 0.002(2) C21 0.061(4) 0.042(3) 0.048(3) 0.009(3) 0.016(3) 0.003(3) C22 0.063(4) 0.055(4) 0.042(3) 0.001(3) 0.019(3) -0.006(3) C23 0.043(3) 0.042(3) 0.053(3) -0.011(3) 0.016(3) 0.004(3) C24 0.031(3) 0.029(3) 0.041(3) -0.007(2) 0.010(2) -0.003(2) C31 0.053(7) 0.049(7) 0.055(5) -0.001(4) 0.010(5) 0.010(5) C32 0.074(8) 0.058(7) 0.078(9) -0.013(6) 0.024(8) 0.019(7) C33 0.109(9) 0.086(9) 0.053(7) -0.004(6) -0.003(6) 0.014(7) C34 0.047(3) 0.062(4) 0.053(3) 0.004(3) 0.015(3) 0.013(3) C35 0.089(5) 0.093(5) 0.107(5) 0.025(4) 0.034(4) -0.008(4) C36 0.089(4) 0.115(5) 0.047(4) 0.005(4) 0.014(3) 0.016(4) C37 0.052(4) 0.113(5) 0.088(4) 0.051(4) 0.031(3) 0.032(4) C38 0.050(4) 0.132(6) 0.091(5) 0.025(4) 0.025(3) 0.009(4) C39 0.090(5) 0.121(6) 0.143(6) 0.053(5) 0.033(5) 0.022(4) C41 0.050(3) 0.063(4) 0.050(3) -0.003(3) 0.011(3) 0.004(3) C42 0.107(5) 0.100(5) 0.058(4) 0.002(3) -0.010(4) -0.017(4) C43 0.131(6) 0.132(7) 0.105(5) 0.040(5) -0.030(5) -0.077(5) C44 0.046(3) 0.051(3) 0.047(3) -0.003(3) 0.013(2) 0.006(3) C45 0.078(4) 0.098(5) 0.066(4) -0.003(3) 0.033(3) 0.025(4) C46 0.060(4) 0.080(4) 0.055(3) 0.019(3) 0.012(3) -0.005(3) C47 0.040(3) 0.040(3) 0.061(3) 0.006(3) 0.011(3) 0.009(2) C48 0.081(4) 0.050(4) 0.090(4) 0.002(3) 0.015(3) -0.008(3) C49 0.073(4) 0.051(4) 0.074(4) 0.018(3) 0.030(3) 0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C31B 1.804(14) . ? Si1 C2 1.846(5) . ? Si1 C34 1.859(5) . ? Si1 C37 1.889(6) . ? Si1 C31 1.943(10) . ? Si2 C4 1.844(5) . ? Si2 C44 1.865(4) . ? Si2 C47 1.884(5) . ? Si2 C41 1.885(5) . ? Cl1 C14 1.729(4) . ? Cl2 C15 1.725(5) . ? C1 C2 1.191(6) . ? C1 C11 1.428(6) . ? C3 C4 1.203(5) . ? C3 C18 1.428(6) . ? C11 C12 1.405(6) . ? C11 C24 1.415(5) . ? C12 N13 1.380(5) . ? C12 C17 1.415(5) . ? N13 C14 1.284(5) . ? C14 C15 1.430(6) . ? C15 N16 1.289(5) . ? N16 C17 1.380(5) . ? C17 C18 1.406(5) . ? C18 C19 1.415(5) . ? C19 C20 1.419(5) . ? C19 C24 1.422(5) . ? C20 C21 1.359(6) . ? C20 H20 0.9500 . ? C21 C22 1.404(6) . ? C21 H21 0.9500 . ? C22 C23 1.351(6) . ? C22 H22 0.9500 . ? C23 C24 1.434(6) . ? C23 H23 0.9500 . ? C31 C32 1.518(9) . ? C31 C33 1.527(10) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.525(6) . ? C34 C35 1.533(6) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.471(7) . ? C37 C38 1.521(6) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C41 C42 1.495(6) . ? C41 C43 1.504(7) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C46 1.540(6) . ? C44 C45 1.540(6) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.535(6) . ? C47 C49 1.543(6) . ? C47 H47 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C31B C32B 1.531(14) . ? C31B C33B 1.536(13) . ? C31B H31B 1.0000 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C33B H33D 0.9800 . ? C33B H33E 0.9800 . ? C33B H33F 0.9800 . ? 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 C31B Si1 C2 112.8(5) . . ? C31B Si1 C34 121.8(6) . . ? C2 Si1 C34 106.4(2) . . ? C31B Si1 C37 99.0(7) . . ? C2 Si1 C37 105.3(2) . . ? C34 Si1 C37 110.4(2) . . ? C31B Si1 C31 25.0(5) . . ? C2 Si1 C31 104.1(3) . . ? C34 Si1 C31 105.5(3) . . ? C37 Si1 C31 123.9(5) . . ? C4 Si2 C44 106.48(19) . . ? C4 Si2 C47 106.6(2) . . ? C44 Si2 C47 110.9(2) . . ? C4 Si2 C41 108.8(2) . . ? C44 Si2 C41 112.3(2) . . ? C47 Si2 C41 111.3(2) . . ? C2 C1 C11 178.1(5) . . ? C1 C2 Si1 175.7(4) . . ? C4 C3 C18 178.6(5) . . ? C3 C4 Si2 179.0(4) . . ? C12 C11 C24 118.6(4) . . ? C12 C11 C1 119.7(4) . . ? C24 C11 C1 121.7(4) . . ? N13 C12 C11 119.4(4) . . ? N13 C12 C17 119.9(4) . . ? C11 C12 C17 120.7(4) . . ? C14 N13 C12 117.3(4) . . ? N13 C14 C15 122.7(4) . . ? N13 C14 Cl1 116.8(4) . . ? C15 C14 Cl1 120.5(4) . . ? N16 C15 C14 122.3(4) . . ? N16 C15 Cl2 117.6(4) . . ? C14 C15 Cl2 120.0(4) . . ? C15 N16 C17 116.8(4) . . ? N16 C17 C18 118.3(4) . . ? N16 C17 C12 120.9(4) . . ? C18 C17 C12 120.7(4) . . ? C17 C18 C19 119.4(4) . . ? C17 C18 C3 119.3(4) . . ? C19 C18 C3 121.2(4) . . ? C18 C19 C20 121.6(4) . . ? C18 C19 C24 119.4(4) . . ? C20 C19 C24 119.0(4) . . ? C21 C20 C19 120.9(5) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 120.1(5) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 121.3(5) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 120.5(5) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C11 C24 C19 121.2(4) . . ? C11 C24 C23 120.6(4) . . ? C19 C24 C23 118.2(4) . . ? C32 C31 C33 112.5(11) . . ? C32 C31 Si1 110.6(9) . . ? C33 C31 Si1 113.1(9) . . ? C32 C31 H31 106.7 . . ? C33 C31 H31 106.7 . . ? Si1 C31 H31 106.7 . . ? C36 C34 C35 109.7(4) . . ? C36 C34 Si1 112.2(3) . . ? C35 C34 Si1 113.0(3) . . ? C36 C34 H34 107.2 . . ? C35 C34 H34 107.2 . . ? Si1 C34 H34 107.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C38 112.5(5) . . ? C39 C37 Si1 116.4(4) . . ? C38 C37 Si1 113.0(4) . . ? C39 C37 H37 104.5 . . ? C38 C37 H37 104.5 . . ? Si1 C37 H37 104.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C41 C43 108.8(5) . . ? C42 C41 Si2 114.3(4) . . ? C43 C41 Si2 113.3(4) . . ? C42 C41 H41 106.6 . . ? C43 C41 H41 106.6 . . ? Si2 C41 H41 106.6 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46 C44 C45 110.6(4) . . ? C46 C44 Si2 114.9(3) . . ? C45 C44 Si2 111.9(3) . . ? C46 C44 H44 106.2 . . ? C45 C44 H44 106.2 . . ? Si2 C44 H44 106.2 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C49 109.2(4) . . ? C48 C47 Si2 113.0(3) . . ? C49 C47 Si2 113.6(3) . . ? C48 C47 H47 106.9 . . ? C49 C47 H47 106.9 . . ? Si2 C47 H47 106.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C32B C31B C33B 110.9(16) . . ? C32B C31B Si1 115(2) . . ? C33B C31B Si1 110.4(15) . . ? C32B C31B H31B 106.6 . . ? C33B C31B H31B 106.6 . . ? Si1 C31B H31B 106.6 . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C31B C33B H33D 109.5 . . ? C31B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C31B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C1 C2 Si1 -167(11) . . . . ? C31B Si1 C2 C1 -144(6) . . . . ? C34 Si1 C2 C1 -8(6) . . . . ? C37 Si1 C2 C1 109(6) . . . . ? C31 Si1 C2 C1 -120(6) . . . . ? C18 C3 C4 Si2 125(22) . . . . ? C44 Si2 C4 C3 81(23) . . . . ? C47 Si2 C4 C3 -38(23) . . . . ? C41 Si2 C4 C3 -158(23) . . . . ? C2 C1 C11 C12 172(15) . . . . ? C2 C1 C11 C24 -9(15) . . . . ? C24 C11 C12 N13 -178.6(3) . . . . ? C1 C11 C12 N13 0.8(6) . . . . ? C24 C11 C12 C17 0.3(6) . . . . ? C1 C11 C12 C17 179.7(4) . . . . ? C11 C12 N13 C14 176.5(4) . . . . ? C17 C12 N13 C14 -2.4(6) . . . . ? C12 N13 C14 C15 0.5(6) . . . . ? C12 N13 C14 Cl1 -178.3(3) . . . . ? N13 C14 C15 N16 2.0(7) . . . . ? Cl1 C14 C15 N16 -179.2(3) . . . . ? N13 C14 C15 Cl2 -176.6(4) . . . . ? Cl1 C14 C15 Cl2 2.1(5) . . . . ? C14 C15 N16 C17 -2.3(6) . . . . ? Cl2 C15 N16 C17 176.3(3) . . . . ? C15 N16 C17 C18 -178.1(4) . . . . ? C15 N16 C17 C12 0.4(6) . . . . ? N13 C12 C17 N16 2.1(6) . . . . ? C11 C12 C17 N16 -176.9(4) . . . . ? N13 C12 C17 C18 -179.6(4) . . . . ? C11 C12 C17 C18 1.5(6) . . . . ? N16 C17 C18 C19 176.8(4) . . . . ? C12 C17 C18 C19 -1.6(6) . . . . ? N16 C17 C18 C3 -0.9(6) . . . . ? C12 C17 C18 C3 -179.3(4) . . . . ? C4 C3 C18 C17 139(20) . . . . ? C4 C3 C18 C19 -39(21) . . . . ? C17 C18 C19 C20 -178.5(4) . . . . ? C3 C18 C19 C20 -0.9(6) . . . . ? C17 C18 C19 C24 -0.1(6) . . . . ? C3 C18 C19 C24 177.5(4) . . . . ? C18 C19 C20 C21 177.8(4) . . . . ? C24 C19 C20 C21 -0.6(6) . . . . ? C19 C20 C21 C22 0.0(7) . . . . ? C20 C21 C22 C23 0.5(7) . . . . ? C21 C22 C23 C24 -0.3(7) . . . . ? C12 C11 C24 C19 -2.0(6) . . . . ? C1 C11 C24 C19 178.6(4) . . . . ? C12 C11 C24 C23 177.6(4) . . . . ? C1 C11 C24 C23 -1.9(6) . . . . ? C18 C19 C24 C11 1.9(6) . . . . ? C20 C19 C24 C11 -179.6(4) . . . . ? C18 C19 C24 C23 -177.7(4) . . . . ? C20 C19 C24 C23 0.8(6) . . . . ? C22 C23 C24 C11 -179.9(4) . . . . ? C22 C23 C24 C19 -0.4(6) . . . . ? C31B Si1 C31 C32 -72.6(17) . . . . ? C2 Si1 C31 C32 173.4(10) . . . . ? C34 Si1 C31 C32 61.6(11) . . . . ? C37 Si1 C31 C32 -66.8(11) . . . . ? C31B Si1 C31 C33 54.6(15) . . . . ? C2 Si1 C31 C33 -59.4(13) . . . . ? C34 Si1 C31 C33 -171.2(12) . . . . ? C37 Si1 C31 C33 60.4(13) . . . . ? C31B Si1 C34 C36 -169.8(7) . . . . ? C2 Si1 C34 C36 59.1(4) . . . . ? C37 Si1 C34 C36 -54.7(4) . . . . ? C31 Si1 C34 C36 169.3(5) . . . . ? C31B Si1 C34 C35 65.6(8) . . . . ? C2 Si1 C34 C35 -65.5(4) . . . . ? C37 Si1 C34 C35 -179.3(4) . . . . ? C31 Si1 C34 C35 44.7(6) . . . . ? C31B Si1 C37 C39 -55.4(7) . . . . ? C2 Si1 C37 C39 61.3(5) . . . . ? C34 Si1 C37 C39 175.7(5) . . . . ? C31 Si1 C37 C39 -57.9(6) . . . . ? C31B Si1 C37 C38 77.0(6) . . . . ? C2 Si1 C37 C38 -166.3(4) . . . . ? C34 Si1 C37 C38 -51.9(5) . . . . ? C31 Si1 C37 C38 74.5(5) . . . . ? C4 Si2 C41 C42 62.8(4) . . . . ? C44 Si2 C41 C42 -179.6(4) . . . . ? C47 Si2 C41 C42 -54.5(5) . . . . ? C4 Si2 C41 C43 -62.6(5) . . . . ? C44 Si2 C41 C43 55.0(5) . . . . ? C47 Si2 C41 C43 -179.9(4) . . . . ? C4 Si2 C44 C46 48.1(4) . . . . ? C47 Si2 C44 C46 163.7(3) . . . . ? C41 Si2 C44 C46 -71.0(4) . . . . ? C4 Si2 C44 C45 175.4(3) . . . . ? C47 Si2 C44 C45 -69.0(4) . . . . ? C41 Si2 C44 C45 56.3(4) . . . . ? C4 Si2 C47 C48 85.5(4) . . . . ? C44 Si2 C47 C48 -30.1(4) . . . . ? C41 Si2 C47 C48 -155.9(3) . . . . ? C4 Si2 C47 C49 -39.6(4) . . . . ? C44 Si2 C47 C49 -155.2(3) . . . . ? C41 Si2 C47 C49 79.0(4) . . . . ? C2 Si1 C31B C32B 154.8(17) . . . . ? C34 Si1 C31B C32B 27(2) . . . . ? C37 Si1 C31B C32B -94.3(19) . . . . ? C31 Si1 C31B C32B 81(2) . . . . ? C2 Si1 C31B C33B 28.1(19) . . . . ? C34 Si1 C31B C33B -100.2(15) . . . . ? C37 Si1 C31B C33B 139.0(16) . . . . ? C31 Si1 C31B C33B -45.8(15) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 21.52 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.284 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.048 _database_code_depnum_ccdc_archive 'CCDC 936729' ####################################################################### # # 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_nb_1s _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4d in manuscript' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H54 N2 Si2' _chemical_formula_weight 691.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 '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 14.8061(10) _cell_length_b 16.0206(11) _cell_length_c 17.5296(11) _cell_angle_alpha 97.524(4) _cell_angle_beta 98.064(4) _cell_angle_gamma 90.635(4) _cell_volume 4079.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2349 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 64.08 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6845 _exptl_absorpt_correction_T_max 0.9098 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28246 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0949 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 66.22 _reflns_number_total 10899 _reflns_number_gt 5421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10899 _refine_ls_number_parameters 892 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1516 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.2080 _refine_ls_wR_factor_gt 0.1721 _refine_ls_goodness_of_fit_ref 1.042 _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 C1 C 0.1519(3) 0.9371(3) 0.6315(3) 0.0523(12) Uani 1 1 d . . . C2 C 0.1056(3) 1.0106(3) 0.6643(3) 0.0548(13) Uani 1 1 d . . . C3 C 0.0896(4) 1.0185(3) 0.7415(3) 0.0664(15) Uani 1 1 d . . . H3A H 0.1083 0.9764 0.7716 0.080 Uiso 1 1 calc R . . C4 C 0.0467(4) 1.0876(3) 0.7742(3) 0.0782(17) Uani 1 1 d . . . H4A H 0.0361 1.0920 0.8256 0.094 Uiso 1 1 calc R . . C5 C 0.0194(4) 1.1505(3) 0.7287(4) 0.0843(18) Uani 1 1 d . . . H5A H -0.0094 1.1975 0.7499 0.101 Uiso 1 1 calc R . . C6 C 0.0349(4) 1.1433(3) 0.6531(3) 0.0693(16) Uani 1 1 d . . . H6A H 0.0161 1.1859 0.6237 0.083 Uiso 1 1 calc R . . C7 C 0.0781(3) 1.0740(3) 0.6184(3) 0.0604(14) Uani 1 1 d . . . C8 C 0.0944(3) 1.0650(3) 0.5368(3) 0.0563(13) Uani 1 1 d . . . C9 C 0.0708(3) 1.1273(3) 0.4874(3) 0.0697(16) Uani 1 1 d . . . H9A H 0.0436 1.1759 0.5071 0.084 Uiso 1 1 calc R . . C10 C 0.0866(4) 1.1182(3) 0.4123(3) 0.0697(16) Uani 1 1 d . . . H10A H 0.0697 1.1603 0.3818 0.084 Uiso 1 1 calc R . . C11 C 0.1276(4) 1.0472(3) 0.3807(3) 0.0666(15) Uani 1 1 d . . . H11A H 0.1393 1.0414 0.3295 0.080 Uiso 1 1 calc R . . C12 C 0.1508(3) 0.9849(3) 0.4274(3) 0.0632(14) Uani 1 1 d . . . H12A H 0.1766 0.9360 0.4064 0.076 Uiso 1 1 calc R . . C13 C 0.1365(3) 0.9938(3) 0.5044(3) 0.0516(12) Uani 1 1 d . . . C14 C 0.1649(3) 0.9270(3) 0.5519(3) 0.0501(12) Uani 1 1 d . . . C15 C 0.2343(3) 0.8013(3) 0.5660(2) 0.0484(12) Uani 1 1 d . . . C16 C 0.2782(3) 0.7304(3) 0.5339(2) 0.0474(12) Uani 1 1 d . . . C17 C 0.3055(3) 0.6669(3) 0.5805(2) 0.0452(11) Uani 1 1 d . . . C18 C 0.3455(3) 0.5919(3) 0.5487(3) 0.0523(13) Uani 1 1 d . . . H18A H 0.3539 0.5848 0.4967 0.063 Uiso 1 1 calc R . . C19 C 0.3713(3) 0.5310(3) 0.5933(3) 0.0578(13) Uani 1 1 d . . . H19A H 0.3959 0.4818 0.5716 0.069 Uiso 1 1 calc R . . C20 C 0.3610(3) 0.5421(3) 0.6728(3) 0.0558(13) Uani 1 1 d . . . H20A H 0.3794 0.5001 0.7031 0.067 Uiso 1 1 calc R . . C21 C 0.3246(3) 0.6129(3) 0.7058(2) 0.0535(13) Uani 1 1 d . . . H21A H 0.3187 0.6191 0.7583 0.064 Uiso 1 1 calc R . . C22 C 0.2953(3) 0.6781(3) 0.6603(2) 0.0489(12) Uani 1 1 d . . . C23 C 0.2566(3) 0.7511(3) 0.6934(2) 0.0478(12) Uani 1 1 d . . . C24 C 0.2237(3) 0.8118(3) 0.6456(2) 0.0481(12) Uani 1 1 d . . . C25 C 0.2508(3) 0.7698(3) 0.7751(3) 0.0516(12) Uani 1 1 d . . . C26 C 0.2476(3) 0.7928(3) 0.8427(3) 0.0564(13) Uani 1 1 d . . . C27 C 0.3465(4) 0.9278(3) 0.9507(3) 0.0640(14) Uani 1 1 d . . . H27A H 0.4011 0.8971 0.9397 0.077 Uiso 1 1 calc R . . C28 C 0.3713(4) 0.9789(3) 1.0319(3) 0.0893(19) Uani 1 1 d . . . H28A H 0.4209 1.0177 1.0312 0.134 Uiso 1 1 calc R . . H28B H 0.3891 0.9413 1.0693 0.134 Uiso 1 1 calc R . . H28C H 0.3193 1.0095 1.0457 0.134 Uiso 1 1 calc R . . C29 C 0.3285(4) 0.9883(3) 0.8891(3) 0.0786(17) Uani 1 1 d . . . H29A H 0.3791 1.0278 0.8947 0.118 Uiso 1 1 calc R . . H29B H 0.2738 1.0182 0.8960 0.118 Uiso 1 1 calc R . . H29C H 0.3215 0.9566 0.8381 0.118 Uiso 1 1 calc R . . C30 C 0.1404(4) 0.8973(3) 0.9537(3) 0.0691(15) Uani 1 1 d . . . H30A H 0.1444 0.9525 0.9358 0.083 Uiso 1 1 calc R . . C31 C 0.1226(4) 0.9152(4) 1.0390(3) 0.102(2) Uani 1 1 d . . . H31A H 0.0642 0.9401 1.0407 0.153 Uiso 1 1 calc R . . H31B H 0.1694 0.9531 1.0683 0.153 Uiso 1 1 calc R . . H31C H 0.1233 0.8633 1.0610 0.153 Uiso 1 1 calc R . . C32 C 0.0574(4) 0.8519(4) 0.9039(3) 0.102(2) Uani 1 1 d . . . H32A H 0.0035 0.8821 0.9131 0.152 Uiso 1 1 calc R . . H32B H 0.0519 0.7959 0.9171 0.152 Uiso 1 1 calc R . . H32C H 0.0644 0.8488 0.8500 0.152 Uiso 1 1 calc R . . C33 C 0.2805(4) 0.7658(3) 1.0091(3) 0.0668(15) Uani 1 1 d . . . H33A H 0.2796 0.7933 1.0623 0.080 Uiso 1 1 calc R . . C34 C 0.3758(4) 0.7326(3) 1.0046(3) 0.092(2) Uani 1 1 d . . . H34A H 0.3885 0.6922 1.0403 0.138 Uiso 1 1 calc R . . H34B H 0.4198 0.7786 1.0180 0.138 Uiso 1 1 calc R . . H34C H 0.3792 0.7062 0.9527 0.138 Uiso 1 1 calc R . . C35 C 0.2090(4) 0.6927(3) 0.9938(3) 0.0856(18) Uani 1 1 d . . . H35A H 0.2254 0.6528 1.0294 0.128 Uiso 1 1 calc R . . H35B H 0.2068 0.6653 0.9414 0.128 Uiso 1 1 calc R . . H35C H 0.1501 0.7143 1.0010 0.128 Uiso 1 1 calc R . . C36 C 0.2979(3) 0.7267(3) 0.4556(3) 0.0501(12) Uani 1 1 d . . . C37 C 0.3181(3) 0.7298(3) 0.3915(3) 0.0533(13) Uani 1 1 d . . . C38 C 0.3379(4) 0.8706(3) 0.3004(3) 0.0641(15) Uani 1 1 d . . . H38A H 0.2719 0.8783 0.2948 0.077 Uiso 1 1 calc R . . C39 C 0.3721(4) 0.9007(3) 0.2302(3) 0.101(2) Uani 1 1 d . . . H39A H 0.3603 0.9595 0.2299 0.151 Uiso 1 1 calc R . . H39B H 0.3410 0.8692 0.1833 0.151 Uiso 1 1 calc R . . H39C H 0.4366 0.8924 0.2331 0.151 Uiso 1 1 calc R . . C40 C 0.3799(4) 0.9246(3) 0.3749(3) 0.0723(16) Uani 1 1 d . . . H40A H 0.3671 0.9826 0.3712 0.109 Uiso 1 1 calc R . . H40B H 0.4448 0.9179 0.3825 0.109 Uiso 1 1 calc R . . H40C H 0.3545 0.9075 0.4181 0.109 Uiso 1 1 calc R . . C41 C 0.4817(3) 0.7314(3) 0.3050(3) 0.0579(13) Uani 1 1 d . . . H41A H 0.5151 0.7838 0.3284 0.069 Uiso 1 1 calc R . . C42 C 0.5092(4) 0.7100(3) 0.2238(3) 0.0873(18) Uani 1 1 d . . . H42A H 0.5736 0.7004 0.2284 0.131 Uiso 1 1 calc R . . H42B H 0.4953 0.7560 0.1945 0.131 Uiso 1 1 calc R . . H42C H 0.4762 0.6601 0.1975 0.131 Uiso 1 1 calc R . . C43 C 0.5148(3) 0.6641(3) 0.3568(3) 0.0760(16) Uani 1 1 d . . . H43A H 0.5790 0.6567 0.3565 0.114 Uiso 1 1 calc R . . H43B H 0.4825 0.6117 0.3372 0.114 Uiso 1 1 calc R . . H43C H 0.5036 0.6818 0.4090 0.114 Uiso 1 1 calc R . . C44 C 0.2848(3) 0.6909(3) 0.2178(3) 0.0545(13) Uani 1 1 d . . . H44A H 0.3090 0.7009 0.1704 0.065 Uiso 1 1 calc R . . C45 C 0.2884(4) 0.5954(3) 0.2228(3) 0.0737(16) Uani 1 1 d . . . H45A H 0.2509 0.5653 0.1784 0.111 Uiso 1 1 calc R . . H45B H 0.2663 0.5839 0.2694 0.111 Uiso 1 1 calc R . . H45C H 0.3502 0.5777 0.2236 0.111 Uiso 1 1 calc R . . C46 C 0.1849(3) 0.7183(3) 0.2098(3) 0.0769(16) Uani 1 1 d . . . H46A H 0.1501 0.6848 0.1659 0.115 Uiso 1 1 calc R . . H46B H 0.1825 0.7766 0.2025 0.115 Uiso 1 1 calc R . . H46C H 0.1598 0.7106 0.2561 0.115 Uiso 1 1 calc R . . C1B C 0.1474(3) 0.4604(3) 0.6050(3) 0.0506(12) Uani 1 1 d . . . C2B C 0.1075(3) 0.5391(3) 0.6351(3) 0.0506(12) Uani 1 1 d . . . C3B C 0.1002(3) 0.5562(3) 0.7139(3) 0.0564(13) Uani 1 1 d . . . H3BA H 0.1212 0.5178 0.7472 0.068 Uiso 1 1 calc R . . C4B C 0.0619(3) 0.6296(3) 0.7432(3) 0.0633(14) Uani 1 1 d . . . H4BA H 0.0562 0.6402 0.7957 0.076 Uiso 1 1 calc R . . C5B C 0.0323(3) 0.6872(3) 0.6937(3) 0.0646(14) Uani 1 1 d . . . H5BA H 0.0073 0.7371 0.7133 0.078 Uiso 1 1 calc R . . C6B C 0.0392(4) 0.6715(3) 0.6164(3) 0.0636(15) Uani 1 1 d . . . H6BA H 0.0180 0.7108 0.5840 0.076 Uiso 1 1 calc R . . C7B C 0.0778(3) 0.5974(3) 0.5843(3) 0.0516(12) Uani 1 1 d . . . C8B C 0.0870(3) 0.5801(3) 0.5017(3) 0.0523(12) Uani 1 1 d . . . C9B C 0.0569(3) 0.6362(3) 0.4487(3) 0.0616(14) Uani 1 1 d . . . H9BA H 0.0308 0.6862 0.4666 0.074 Uiso 1 1 calc R . . C10B C 0.0650(4) 0.6188(3) 0.3713(3) 0.0632(14) Uani 1 1 d . . . H10B H 0.0436 0.6568 0.3376 0.076 Uiso 1 1 calc R . . C11B C 0.1045(3) 0.5456(3) 0.3426(3) 0.0606(14) Uani 1 1 d . . . H11B H 0.1105 0.5344 0.2902 0.073 Uiso 1 1 calc R . . C12B C 0.1349(3) 0.4894(3) 0.3935(3) 0.0569(13) Uani 1 1 d . . . H12B H 0.1611 0.4397 0.3750 0.068 Uiso 1 1 calc R . . C13B C 0.1268(3) 0.5065(3) 0.4720(3) 0.0487(12) Uani 1 1 d . . . C14B C 0.1581(3) 0.4445(3) 0.5245(3) 0.0487(12) Uani 1 1 d . . . C15B C 0.2253(3) 0.3192(3) 0.5455(2) 0.0470(12) Uani 1 1 d . . . C16B C 0.2707(3) 0.2473(3) 0.5172(2) 0.0474(12) Uani 1 1 d . . . C17B C 0.2958(3) 0.1859(3) 0.5666(2) 0.0452(11) Uani 1 1 d . . . C18B C 0.3394(3) 0.1109(3) 0.5399(3) 0.0524(13) Uani 1 1 d . . . H18B H 0.3525 0.1023 0.4892 0.063 Uiso 1 1 calc R . . C19B C 0.3620(3) 0.0516(3) 0.5876(3) 0.0571(13) Uani 1 1 d . . . H19B H 0.3892 0.0025 0.5688 0.068 Uiso 1 1 calc R . . C20B C 0.3447(3) 0.0636(3) 0.6649(3) 0.0545(13) Uani 1 1 d . . . H20B H 0.3617 0.0230 0.6971 0.065 Uiso 1 1 calc R . . C21B C 0.3033(3) 0.1343(3) 0.6932(3) 0.0547(13) Uani 1 1 d . . . H21B H 0.2908 0.1408 0.7442 0.066 Uiso 1 1 calc R . . C22B C 0.2787(3) 0.1988(3) 0.6453(2) 0.0463(12) Uani 1 1 d . . . C23B C 0.2370(3) 0.2728(3) 0.6747(2) 0.0482(12) Uani 1 1 d . . . C24B C 0.2112(3) 0.3337(3) 0.6247(2) 0.0473(12) Uani 1 1 d . . . C25B C 0.2271(3) 0.2916(3) 0.7549(3) 0.0539(13) Uani 1 1 d . . . C26B C 0.2231(4) 0.3094(3) 0.8230(3) 0.0615(14) Uani 1 1 d . A . C27B C 0.1375(6) 0.4231(7) 0.9448(5) 0.093(2) Uiso 0.50 1 d PD A 1 H27B H 0.1488 0.4787 0.9297 0.111 Uiso 0.50 1 calc PR A 1 C27C C 0.0958(6) 0.3675(8) 0.9311(6) 0.093(2) Uiso 0.50 1 d PD A 2 H27C H 0.0684 0.3109 0.9147 0.111 Uiso 0.50 1 calc PR A 2 C28B C 0.0515(8) 0.3797(8) 0.8960(7) 0.093(2) Uiso 0.50 1 d PD A 1 H28D H 0.0009 0.4164 0.8993 0.139 Uiso 0.50 1 calc PR A 1 H28E H 0.0384 0.3283 0.9155 0.139 Uiso 0.50 1 calc PR A 1 H28F H 0.0613 0.3674 0.8428 0.139 Uiso 0.50 1 calc PR A 1 C29B C 0.1237(8) 0.4301(8) 1.0303(6) 0.093(2) Uiso 0.50 1 d PD A 1 H29D H 0.1222 0.4884 1.0513 0.139 Uiso 0.50 1 calc PR A 1 H29E H 0.1730 0.4039 1.0589 0.139 Uiso 0.50 1 calc PR A 1 H29F H 0.0670 0.4023 1.0342 0.139 Uiso 0.50 1 calc PR A 1 C28C C 0.0476(8) 0.4223(7) 0.8703(6) 0.0927(8) Uiso 0.50 1 d PD A 2 H28G H -0.0168 0.4221 0.8725 0.139 Uiso 0.50 1 calc PR A 2 H28H H 0.0583 0.3993 0.8191 0.139 Uiso 0.50 1 calc PR A 2 H28I H 0.0719 0.4791 0.8822 0.139 Uiso 0.50 1 calc PR A 2 C29C C 0.0667(8) 0.3942(8) 1.0111(6) 0.093(4) Uiso 0.50 1 d PD A 2 H29G H 0.0696 0.4546 1.0223 0.140 Uiso 0.50 1 calc PR A 2 H29H H 0.1070 0.3708 1.0501 0.140 Uiso 0.50 1 calc PR A 2 H29I H 0.0054 0.3742 1.0110 0.140 Uiso 0.50 1 calc PR A 2 C30B C 0.3404(7) 0.4285(6) 0.9401(6) 0.067(2) Uiso 0.50 1 d PD A 1 H30B H 0.3924 0.3917 0.9360 0.081 Uiso 0.50 1 calc PR A 1 C30C C 0.2778(8) 0.4556(5) 0.9471(5) 0.067(2) Uiso 0.50 1 d PD A 2 H30C H 0.2291 0.4963 0.9503 0.081 Uiso 0.50 1 calc PR A 2 C31B C 0.3414(5) 0.4810(5) 0.8858(4) 0.146(3) Uani 1 1 d . . . H31D H 0.3337 0.4487 0.8350 0.218 Uiso 1 1 calc R A 1 H31E H 0.3987 0.5118 0.8945 0.218 Uiso 1 1 calc R A 1 H31F H 0.2926 0.5196 0.8893 0.218 Uiso 1 1 calc R A 1 C32B C 0.3515(6) 0.4736(4) 1.0269(3) 0.164(4) Uani 1 1 d . . . H32D H 0.3497 0.4321 1.0615 0.246 Uiso 1 1 calc R A 1 H32E H 0.3026 0.5117 1.0328 0.246 Uiso 1 1 calc R A 1 H32F H 0.4088 0.5044 1.0390 0.246 Uiso 1 1 calc R A 1 C33B C 0.2608(4) 0.2697(3) 0.9874(3) 0.0750(17) Uani 1 1 d . A . H33B H 0.2639 0.2953 1.0416 0.090 Uiso 1 1 calc R . . C34B C 0.3547(4) 0.2367(3) 0.9766(3) 0.100(2) Uani 1 1 d . . . H34D H 0.3702 0.1950 1.0106 0.150 Uiso 1 1 calc R . . H34E H 0.3991 0.2823 0.9888 0.150 Uiso 1 1 calc R . . H34F H 0.3541 0.2118 0.9237 0.150 Uiso 1 1 calc R . . C35B C 0.1915(4) 0.1966(4) 0.9740(3) 0.097(2) Uani 1 1 d . . . H35D H 0.2111 0.1560 1.0080 0.146 Uiso 1 1 calc R . . H35E H 0.1863 0.1706 0.9210 0.146 Uiso 1 1 calc R . . H35F H 0.1332 0.2171 0.9845 0.146 Uiso 1 1 calc R . . C36B C 0.2926(3) 0.2388(3) 0.4397(3) 0.0507(12) Uani 1 1 d . . . C37B C 0.3156(3) 0.2354(2) 0.3758(3) 0.0518(13) Uani 1 1 d . . . C38B C 0.2613(3) 0.2242(3) 0.2039(3) 0.0635(14) Uani 1 1 d . . . H38B H 0.2847 0.2302 0.1553 0.076 Uiso 1 1 calc R . . C39B C 0.1896(4) 0.2901(3) 0.2145(3) 0.0905(19) Uani 1 1 d . . . H39D H 0.1405 0.2800 0.1721 0.136 Uiso 1 1 calc R . . H39E H 0.2165 0.3451 0.2154 0.136 Uiso 1 1 calc R . . H39F H 0.1666 0.2868 0.2626 0.136 Uiso 1 1 calc R . . C40B C 0.2182(4) 0.1351(3) 0.1955(3) 0.0874(19) Uani 1 1 d . . . H40D H 0.1684 0.1287 0.1535 0.131 Uiso 1 1 calc R . . H40E H 0.1961 0.1267 0.2429 0.131 Uiso 1 1 calc R . . H40F H 0.2633 0.0942 0.1847 0.131 Uiso 1 1 calc R . . C41B C 0.4199(4) 0.3459(3) 0.2920(3) 0.0610(14) Uani 1 1 d . . . H41B H 0.4828 0.3395 0.3162 0.073 Uiso 1 1 calc R . . C42B C 0.4259(4) 0.3737(3) 0.2124(3) 0.0816(17) Uani 1 1 d . . . H42D H 0.4580 0.4271 0.2194 0.122 Uiso 1 1 calc R . . H42E H 0.3655 0.3787 0.1856 0.122 Uiso 1 1 calc R . . H42F H 0.4580 0.3326 0.1824 0.122 Uiso 1 1 calc R . . C43B C 0.3800(4) 0.4169(3) 0.3443(3) 0.0819(18) Uani 1 1 d . . . H43D H 0.4147 0.4682 0.3460 0.123 Uiso 1 1 calc R . . H43E H 0.3830 0.4020 0.3959 0.123 Uiso 1 1 calc R . . H43F H 0.3176 0.4246 0.3235 0.123 Uiso 1 1 calc R . . C44B C 0.4424(3) 0.1532(3) 0.2758(3) 0.0618(14) Uani 1 1 d . . . H44B H 0.4069 0.1002 0.2711 0.074 Uiso 1 1 calc R . . C45B C 0.4899(4) 0.1499(4) 0.2033(3) 0.098(2) Uani 1 1 d . . . H45D H 0.5298 0.1031 0.2013 0.148 Uiso 1 1 calc R . . H45E H 0.5249 0.2013 0.2056 0.148 Uiso 1 1 calc R . . H45F H 0.4449 0.1434 0.1577 0.148 Uiso 1 1 calc R . . C46B C 0.5143(3) 0.1556(3) 0.3484(3) 0.0734(16) Uani 1 1 d . . . H46D H 0.5543 0.1093 0.3415 0.110 Uiso 1 1 calc R . . H46E H 0.4845 0.1515 0.3930 0.110 Uiso 1 1 calc R . . H46F H 0.5492 0.2077 0.3560 0.110 Uiso 1 1 calc R . . N1 N 0.1808(3) 0.8806(2) 0.6777(2) 0.0521(10) Uani 1 1 d . . . N2 N 0.2060(3) 0.8616(2) 0.5200(2) 0.0524(10) Uani 1 1 d . . . N1B N 0.1716(3) 0.4054(2) 0.65387(19) 0.0489(10) Uani 1 1 d . . . N2B N 0.1971(3) 0.3765(2) 0.49560(19) 0.0490(10) Uani 1 1 d . . . Si1 Si 0.25272(11) 0.84690(8) 0.94223(7) 0.0587(4) Uani 1 1 d . . . Si2 Si 0.35727(10) 0.75419(8) 0.30206(7) 0.0522(4) Uani 1 1 d . . . Si1B Si 0.22775(15) 0.35320(9) 0.92523(8) 0.0900(7) Uani 1 1 d D . . Si2B Si 0.36069(9) 0.24040(8) 0.28481(7) 0.0522(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.053(4) 0.045(3) 0.058(3) 0.002(2) 0.009(3) 0.008(3) C2 0.051(4) 0.044(3) 0.069(3) 0.000(3) 0.009(3) 0.016(3) C3 0.065(4) 0.057(3) 0.076(4) 0.000(3) 0.012(3) 0.023(3) C4 0.075(5) 0.071(4) 0.085(4) -0.007(3) 0.013(3) 0.025(4) C5 0.081(5) 0.066(4) 0.101(5) -0.012(3) 0.015(4) 0.031(4) C6 0.061(4) 0.049(3) 0.098(4) 0.006(3) 0.013(3) 0.023(3) C7 0.049(4) 0.052(3) 0.079(4) 0.003(3) 0.007(3) 0.012(3) C8 0.047(4) 0.041(3) 0.080(4) 0.006(3) 0.007(3) 0.011(3) C9 0.063(4) 0.046(3) 0.102(4) 0.019(3) 0.007(3) 0.018(3) C10 0.064(4) 0.059(4) 0.090(4) 0.030(3) 0.008(3) 0.020(3) C11 0.059(4) 0.065(4) 0.082(4) 0.028(3) 0.012(3) 0.018(3) C12 0.062(4) 0.056(3) 0.076(4) 0.023(3) 0.011(3) 0.017(3) C13 0.044(3) 0.046(3) 0.066(3) 0.011(3) 0.007(3) 0.010(3) C14 0.046(3) 0.044(3) 0.060(3) 0.007(2) 0.006(2) 0.011(3) C15 0.051(3) 0.046(3) 0.050(3) 0.008(2) 0.007(2) 0.009(3) C16 0.048(3) 0.043(3) 0.051(3) 0.004(2) 0.005(2) 0.008(3) C17 0.047(3) 0.039(3) 0.049(3) 0.004(2) 0.005(2) 0.007(3) C18 0.055(4) 0.041(3) 0.060(3) 0.003(2) 0.009(3) 0.009(3) C19 0.067(4) 0.041(3) 0.065(3) 0.005(2) 0.009(3) 0.016(3) C20 0.056(4) 0.050(3) 0.064(3) 0.013(3) 0.010(3) 0.014(3) C21 0.062(4) 0.049(3) 0.050(3) 0.009(2) 0.010(3) 0.010(3) C22 0.052(3) 0.046(3) 0.048(3) 0.006(2) 0.006(2) 0.005(3) C23 0.052(3) 0.046(3) 0.046(3) 0.004(2) 0.009(2) 0.009(3) C24 0.052(3) 0.042(3) 0.051(3) 0.004(2) 0.009(2) 0.010(3) C25 0.052(3) 0.046(3) 0.058(3) 0.011(3) 0.007(3) 0.015(3) C26 0.069(4) 0.041(3) 0.057(3) 0.005(3) 0.004(3) 0.012(3) C27 0.075(4) 0.053(3) 0.061(3) -0.001(3) 0.009(3) 0.015(3) C28 0.105(5) 0.084(4) 0.076(4) -0.004(3) 0.018(4) -0.007(4) C29 0.103(5) 0.054(3) 0.082(4) 0.010(3) 0.023(4) 0.010(3) C30 0.068(4) 0.070(4) 0.068(3) 0.001(3) 0.014(3) 0.022(3) C31 0.099(5) 0.110(5) 0.097(5) -0.010(4) 0.029(4) 0.038(4) C32 0.076(5) 0.112(6) 0.112(5) -0.003(4) 0.010(4) 0.030(5) C33 0.087(4) 0.058(4) 0.054(3) 0.006(3) 0.006(3) 0.013(3) C34 0.109(5) 0.082(4) 0.087(4) 0.028(3) 0.005(4) 0.026(4) C35 0.112(5) 0.065(4) 0.079(4) 0.013(3) 0.007(4) -0.002(4) C36 0.049(3) 0.040(3) 0.059(3) 0.000(2) 0.003(3) 0.016(3) C37 0.052(3) 0.048(3) 0.060(3) 0.004(2) 0.010(3) 0.022(3) C38 0.075(4) 0.052(3) 0.065(3) 0.006(3) 0.007(3) 0.015(3) C39 0.178(7) 0.057(4) 0.071(4) 0.012(3) 0.026(4) 0.007(4) C40 0.079(4) 0.054(3) 0.083(4) 0.000(3) 0.012(3) 0.013(3) C41 0.057(3) 0.056(3) 0.062(3) 0.005(3) 0.014(3) 0.019(3) C42 0.072(4) 0.102(5) 0.085(4) -0.002(3) 0.014(3) 0.007(4) C43 0.067(4) 0.059(3) 0.104(4) 0.024(3) 0.006(3) 0.019(3) C44 0.056(3) 0.053(3) 0.054(3) 0.004(2) 0.012(2) 0.008(3) C45 0.083(4) 0.060(4) 0.079(4) -0.001(3) 0.021(3) 0.005(3) C46 0.065(4) 0.086(4) 0.078(4) 0.012(3) 0.005(3) 0.018(4) C1B 0.053(3) 0.043(3) 0.055(3) 0.005(2) 0.005(2) 0.008(3) C2B 0.048(3) 0.047(3) 0.055(3) 0.002(2) 0.006(2) 0.010(3) C3B 0.048(3) 0.049(3) 0.071(3) 0.005(3) 0.006(3) 0.017(3) C4B 0.060(4) 0.058(3) 0.068(3) -0.003(3) 0.007(3) 0.019(3) C5B 0.070(4) 0.045(3) 0.075(4) -0.004(3) 0.007(3) 0.015(3) C6B 0.064(4) 0.047(3) 0.078(4) 0.007(3) 0.003(3) 0.017(3) C7B 0.044(3) 0.039(3) 0.069(3) 0.001(2) 0.004(3) 0.010(3) C8B 0.045(3) 0.046(3) 0.064(3) 0.007(3) 0.005(3) 0.007(3) C9B 0.062(4) 0.046(3) 0.077(4) 0.012(3) 0.005(3) 0.012(3) C10B 0.061(4) 0.055(3) 0.078(4) 0.022(3) 0.012(3) 0.018(3) C11B 0.060(4) 0.060(3) 0.063(3) 0.012(3) 0.009(3) 0.013(3) C12B 0.058(3) 0.055(3) 0.061(3) 0.016(3) 0.010(3) 0.021(3) C13B 0.047(3) 0.042(3) 0.057(3) 0.007(2) 0.003(2) 0.010(3) C14B 0.046(3) 0.046(3) 0.054(3) 0.008(2) 0.004(2) 0.005(3) C15B 0.048(3) 0.044(3) 0.049(3) 0.006(2) 0.006(2) 0.011(3) C16B 0.049(3) 0.046(3) 0.047(3) 0.003(2) 0.008(2) 0.011(3) C17B 0.046(3) 0.043(3) 0.047(3) 0.006(2) 0.008(2) 0.010(3) C18B 0.058(4) 0.043(3) 0.055(3) -0.001(2) 0.011(3) 0.011(3) C19B 0.062(4) 0.042(3) 0.066(3) 0.004(2) 0.005(3) 0.013(3) C20B 0.059(4) 0.049(3) 0.057(3) 0.013(2) 0.006(3) 0.017(3) C21B 0.058(4) 0.050(3) 0.057(3) 0.011(2) 0.010(3) 0.013(3) C22B 0.047(3) 0.041(3) 0.050(3) 0.005(2) 0.006(2) 0.008(3) C23B 0.048(3) 0.046(3) 0.050(3) 0.005(2) 0.008(2) 0.013(3) C24B 0.050(3) 0.042(3) 0.050(3) 0.003(2) 0.009(2) 0.012(3) C25B 0.057(3) 0.049(3) 0.058(3) 0.012(3) 0.011(3) 0.023(3) C26B 0.078(4) 0.051(3) 0.061(3) 0.017(3) 0.017(3) 0.026(3) C31B 0.173(8) 0.159(8) 0.103(5) -0.032(5) 0.062(5) -0.038(6) C32B 0.296(12) 0.086(5) 0.084(5) 0.006(4) -0.054(6) 0.018(6) C33B 0.114(5) 0.061(4) 0.052(3) 0.008(3) 0.017(3) 0.020(4) C34B 0.112(6) 0.078(4) 0.110(5) 0.014(4) 0.009(4) 0.038(4) C35B 0.128(6) 0.079(5) 0.085(4) 0.011(4) 0.020(4) 0.008(5) C36B 0.053(3) 0.038(3) 0.060(3) 0.004(2) 0.002(3) 0.013(3) C37B 0.059(3) 0.037(3) 0.057(3) 0.003(2) 0.003(3) 0.011(3) C38B 0.065(4) 0.070(4) 0.057(3) 0.010(3) 0.009(3) 0.006(3) C39B 0.069(4) 0.097(5) 0.103(4) 0.024(4) -0.005(4) 0.025(4) C40B 0.084(4) 0.093(5) 0.078(4) 0.007(3) -0.005(3) -0.011(4) C41B 0.061(4) 0.053(3) 0.070(3) 0.015(3) 0.008(3) 0.012(3) C42B 0.083(4) 0.080(4) 0.086(4) 0.032(3) 0.008(3) 0.000(4) C43B 0.089(5) 0.051(4) 0.106(4) 0.005(3) 0.019(4) 0.015(4) C44B 0.064(4) 0.050(3) 0.072(3) 0.001(3) 0.018(3) 0.014(3) C45B 0.092(5) 0.113(5) 0.093(4) 0.005(4) 0.026(4) 0.051(4) C46B 0.068(4) 0.061(3) 0.093(4) 0.018(3) 0.007(3) 0.029(3) N1 0.054(3) 0.045(2) 0.056(2) 0.0036(19) 0.008(2) 0.015(2) N2 0.053(3) 0.047(2) 0.059(2) 0.013(2) 0.010(2) 0.016(2) N1B 0.049(3) 0.042(2) 0.055(2) 0.0030(19) 0.006(2) 0.012(2) N2B 0.048(3) 0.042(2) 0.056(2) 0.0052(19) 0.004(2) 0.011(2) Si1 0.0695(10) 0.0539(9) 0.0523(8) 0.0033(7) 0.0102(7) 0.0176(8) Si2 0.0581(10) 0.0449(8) 0.0534(8) 0.0054(6) 0.0079(7) 0.0145(8) Si1B 0.159(2) 0.0622(10) 0.0544(9) 0.0119(8) 0.0255(10) 0.0522(12) Si2B 0.0571(9) 0.0458(8) 0.0538(8) 0.0067(6) 0.0078(7) 0.0127(8) _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 N1 1.327(5) . ? C1 C14 1.425(6) . ? C1 C2 1.461(6) . ? C2 C3 1.396(6) . ? C2 C7 1.406(6) . ? C3 C4 1.382(6) . ? C3 H3A 0.9300 . ? C4 C5 1.394(7) . ? C4 H4A 0.9300 . ? C5 C6 1.368(7) . ? C5 H5A 0.9300 . ? C6 C7 1.401(6) . ? C6 H6A 0.9300 . ? C7 C8 1.471(6) . ? C8 C13 1.401(6) . ? C8 C9 1.419(6) . ? C9 C10 1.359(6) . ? C9 H9A 0.9300 . ? C10 C11 1.384(6) . ? C10 H10A 0.9300 . ? C11 C12 1.388(5) . ? C11 H11A 0.9300 . ? C12 C13 1.385(6) . ? C12 H12A 0.9300 . ? C13 C14 1.470(5) . ? C14 N2 1.317(5) . ? C15 N2 1.371(5) . ? C15 C16 1.408(5) . ? C15 C24 1.414(6) . ? C16 C17 1.414(5) . ? C16 C36 1.436(6) . ? C17 C22 1.418(6) . ? C17 C18 1.428(5) . ? C18 C19 1.355(5) . ? C18 H18A 0.9300 . ? C19 C20 1.412(6) . ? C19 H19A 0.9300 . ? C20 C21 1.357(6) . ? C20 H20A 0.9300 . ? C21 C22 1.430(5) . ? C21 H21A 0.9300 . ? C22 C23 1.400(6) . ? C23 C24 1.412(5) . ? C23 C25 1.440(6) . ? C24 N1 1.374(5) . ? C25 C26 1.201(6) . ? C26 Si1 1.835(5) . ? C27 C28 1.540(6) . ? C27 C29 1.542(6) . ? C27 Si1 1.866(5) . ? C27 H27A 0.9800 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C32 1.522(7) . ? C30 C31 1.546(6) . ? C30 Si1 1.881(5) . ? C30 H30A 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.522(7) . ? C33 C35 1.541(6) . ? C33 Si1 1.873(4) . ? C33 H33A 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.210(6) . ? C37 Si2 1.832(5) . ? C38 C40 1.518(6) . ? C38 C39 1.527(6) . ? C38 Si2 1.893(4) . ? C38 H38A 0.9800 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.533(6) . ? C41 C43 1.540(5) . ? C41 Si2 1.877(5) . ? C41 H41A 0.9800 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C46 1.540(6) . ? C44 C45 1.545(6) . ? C44 Si2 1.871(4) . ? C44 H44A 0.9800 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C1B N1B 1.327(5) . ? C1B C14B 1.432(6) . ? C1B C2B 1.465(6) . ? C2B C3B 1.392(6) . ? C2B C7B 1.406(5) . ? C3B C4B 1.379(6) . ? C3B H3BA 0.9300 . ? C4B C5B 1.380(6) . ? C4B H4BA 0.9300 . ? C5B C6B 1.365(6) . ? C5B H5BA 0.9300 . ? C6B C7B 1.407(6) . ? C6B H6BA 0.9300 . ? C7B C8B 1.465(6) . ? C8B C13B 1.395(6) . ? C8B C9B 1.408(5) . ? C9B C10B 1.370(6) . ? C9B H9BA 0.9300 . ? C10B C11B 1.383(6) . ? C10B H10B 0.9300 . ? C11B C12B 1.385(5) . ? C11B H11B 0.9300 . ? C12B C13B 1.390(6) . ? C12B H12B 0.9300 . ? C13B C14B 1.475(5) . ? C14B N2B 1.315(5) . ? C15B N2B 1.377(5) . ? C15B C16B 1.409(5) . ? C15B C24B 1.422(5) . ? C16B C17B 1.413(5) . ? C16B C36B 1.429(6) . ? C17B C22B 1.426(5) . ? C17B C18B 1.427(5) . ? C18B C19B 1.360(5) . ? C18B H18B 0.9300 . ? C19B C20B 1.403(6) . ? C19B H19B 0.9300 . ? C20B C21B 1.364(5) . ? C20B H20B 0.9300 . ? C21B C22B 1.433(5) . ? C21B H21B 0.9300 . ? C22B C23B 1.414(5) . ? C23B C24B 1.416(5) . ? C23B C25B 1.427(6) . ? C24B N1B 1.367(5) . ? C25B C26B 1.201(6) . ? C26B Si1B 1.828(5) . ? C27B C29B 1.531(8) . ? C27B C28B 1.534(9) . ? C27B Si1B 1.794(8) . ? C27B H27B 0.9800 . ? C27C C29C 1.534(9) . ? C27C C28C 1.569(8) . ? C27C Si1B 1.985(8) . ? C27C H27C 0.9800 . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? C28C H28G 0.9600 . ? C28C H28H 0.9600 . ? C28C H28I 0.9600 . ? C29C H29G 0.9600 . ? C29C H29H 0.9600 . ? C29C H29I 0.9600 . ? C30B C31B 1.351(10) . ? C30B C32B 1.582(11) . ? C30B Si1B 2.014(8) . ? C30B H30B 0.9800 . ? C30C C31B 1.611(11) . ? C30C C32B 1.640(10) . ? C30C Si1B 1.765(7) . ? C30C H30C 0.9800 . ? C31B H31D 0.9600 . ? C31B H31E 0.9600 . ? C31B H31F 0.9600 . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? C33B C34B 1.520(7) . ? C33B C35B 1.522(7) . ? C33B Si1B 1.860(5) . ? C33B H33B 0.9800 . ? C34B H34D 0.9600 . ? C34B H34E 0.9600 . ? C34B H34F 0.9600 . ? C35B H35D 0.9600 . ? C35B H35E 0.9600 . ? C35B H35F 0.9600 . ? C36B C37B 1.211(6) . ? C37B Si2B 1.824(5) . ? C38B C39B 1.517(6) . ? C38B C40B 1.538(6) . ? C38B Si2B 1.885(5) . ? C38B H38B 0.9800 . ? C39B H39D 0.9600 . ? C39B H39E 0.9600 . ? C39B H39F 0.9600 . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C41B C42B 1.533(6) . ? C41B C43B 1.541(6) . ? C41B Si2B 1.876(5) . ? C41B H41B 0.9800 . ? C42B H42D 0.9600 . ? C42B H42E 0.9600 . ? C42B H42F 0.9600 . ? C43B H43D 0.9600 . ? C43B H43E 0.9600 . ? C43B H43F 0.9600 . ? C44B C45B 1.532(6) . ? C44B C46B 1.536(6) . ? C44B Si2B 1.864(5) . ? C44B H44B 0.9800 . ? C45B H45D 0.9600 . ? C45B H45E 0.9600 . ? C45B H45F 0.9600 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? C46B H46F 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 N1 C1 C14 121.3(4) . . ? N1 C1 C2 118.3(4) . . ? C14 C1 C2 120.3(4) . . ? C3 C2 C7 119.9(4) . . ? C3 C2 C1 120.1(4) . . ? C7 C2 C1 120.0(5) . . ? C4 C3 C2 121.3(5) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 118.9(5) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C6 C5 C4 120.2(5) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 C7 122.2(5) . . ? C5 C6 H6A 118.9 . . ? C7 C6 H6A 118.9 . . ? C6 C7 C2 117.5(5) . . ? C6 C7 C8 122.8(4) . . ? C2 C7 C8 119.7(4) . . ? C13 C8 C9 116.3(5) . . ? C13 C8 C7 120.6(4) . . ? C9 C8 C7 123.0(5) . . ? C10 C9 C8 122.3(5) . . ? C10 C9 H9A 118.8 . . ? C8 C9 H9A 118.8 . . ? C9 C10 C11 120.9(5) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C10 C11 C12 118.1(5) . . ? C10 C11 H11A 120.9 . . ? C12 C11 H11A 120.9 . . ? C13 C12 C11 121.7(5) . . ? C13 C12 H12A 119.2 . . ? C11 C12 H12A 119.2 . . ? C12 C13 C8 120.6(4) . . ? C12 C13 C14 119.4(4) . . ? C8 C13 C14 120.0(4) . . ? N2 C14 C1 122.3(4) . . ? N2 C14 C13 118.4(4) . . ? C1 C14 C13 119.2(4) . . ? N2 C15 C16 119.0(4) . . ? N2 C15 C24 120.7(4) . . ? C16 C15 C24 120.2(4) . . ? C15 C16 C17 119.3(4) . . ? C15 C16 C36 118.8(4) . . ? C17 C16 C36 121.9(4) . . ? C16 C17 C22 120.1(4) . . ? C16 C17 C18 120.9(4) . . ? C22 C17 C18 119.0(4) . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C20 120.1(4) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C21 C20 C19 121.1(4) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C20 C21 C22 120.5(4) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C23 C22 C17 120.5(4) . . ? C23 C22 C21 121.1(4) . . ? C17 C22 C21 118.4(4) . . ? C22 C23 C24 119.4(4) . . ? C22 C23 C25 123.5(4) . . ? C24 C23 C25 117.1(4) . . ? N1 C24 C23 118.8(4) . . ? N1 C24 C15 120.8(4) . . ? C23 C24 C15 120.3(4) . . ? C26 C25 C23 174.2(5) . . ? C25 C26 Si1 168.9(5) . . ? C28 C27 C29 109.7(4) . . ? C28 C27 Si1 115.2(4) . . ? C29 C27 Si1 112.4(3) . . ? C28 C27 H27A 106.3 . . ? C29 C27 H27A 106.3 . . ? Si1 C27 H27A 106.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C30 C31 109.5(5) . . ? C32 C30 Si1 115.3(4) . . ? C31 C30 Si1 113.7(4) . . ? C32 C30 H30A 105.9 . . ? C31 C30 H30A 105.9 . . ? Si1 C30 H30A 105.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C35 110.7(4) . . ? C34 C33 Si1 111.5(4) . . ? C35 C33 Si1 112.1(3) . . ? C34 C33 H33A 107.4 . . ? C35 C33 H33A 107.4 . . ? Si1 C33 H33A 107.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C16 174.7(5) . . ? C36 C37 Si2 169.3(4) . . ? C40 C38 C39 110.5(4) . . ? C40 C38 Si2 113.1(3) . . ? C39 C38 Si2 111.0(3) . . ? C40 C38 H38A 107.3 . . ? C39 C38 H38A 107.3 . . ? Si2 C38 H38A 107.3 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C43 110.6(4) . . ? C42 C41 Si2 112.7(3) . . ? C43 C41 Si2 114.1(3) . . ? C42 C41 H41A 106.3 . . ? C43 C41 H41A 106.3 . . ? Si2 C41 H41A 106.3 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46 C44 C45 109.7(4) . . ? C46 C44 Si2 111.9(3) . . ? C45 C44 Si2 112.1(3) . . ? C46 C44 H44A 107.6 . . ? C45 C44 H44A 107.6 . . ? Si2 C44 H44A 107.6 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N1B C1B C14B 122.0(4) . . ? N1B C1B C2B 118.2(4) . . ? C14B C1B C2B 119.8(4) . . ? C3B C2B C7B 120.3(4) . . ? C3B C2B C1B 120.0(4) . . ? C7B C2B C1B 119.7(4) . . ? C4B C3B C2B 120.7(4) . . ? C4B C3B H3BA 119.6 . . ? C2B C3B H3BA 119.6 . . ? C3B C4B C5B 119.4(5) . . ? C3B C4B H4BA 120.3 . . ? C5B C4B H4BA 120.3 . . ? C6B C5B C4B 120.6(5) . . ? C6B C5B H5BA 119.7 . . ? C4B C5B H5BA 119.7 . . ? C5B C6B C7B 121.7(4) . . ? C5B C6B H6BA 119.2 . . ? C7B C6B H6BA 119.2 . . ? C2B C7B C6B 117.2(4) . . ? C2B C7B C8B 120.3(4) . . ? C6B C7B C8B 122.5(4) . . ? C13B C8B C9B 116.9(4) . . ? C13B C8B C7B 121.0(4) . . ? C9B C8B C7B 122.1(4) . . ? C10B C9B C8B 121.6(5) . . ? C10B C9B H9BA 119.2 . . ? C8B C9B H9BA 119.2 . . ? C9B C10B C11B 121.0(4) . . ? C9B C10B H10B 119.5 . . ? C11B C10B H10B 119.5 . . ? C10B C11B C12B 118.7(5) . . ? C10B C11B H11B 120.7 . . ? C12B C11B H11B 120.7 . . ? C11B C12B C13B 120.7(4) . . ? C11B C12B H12B 119.6 . . ? C13B C12B H12B 119.6 . . ? C12B C13B C8B 121.2(4) . . ? C12B C13B C14B 119.4(4) . . ? C8B C13B C14B 119.4(4) . . ? N2B C14B C1B 121.9(4) . . ? N2B C14B C13B 118.4(4) . . ? C1B C14B C13B 119.7(4) . . ? N2B C15B C16B 118.7(4) . . ? N2B C15B C24B 120.5(4) . . ? C16B C15B C24B 120.7(4) . . ? C15B C16B C17B 119.3(4) . . ? C15B C16B C36B 119.5(4) . . ? C17B C16B C36B 121.1(4) . . ? C16B C17B C22B 120.0(4) . . ? C16B C17B C18B 121.4(4) . . ? C22B C17B C18B 118.5(4) . . ? C19B C18B C17B 121.0(4) . . ? C19B C18B H18B 119.5 . . ? C17B C18B H18B 119.5 . . ? C18B C19B C20B 120.7(4) . . ? C18B C19B H19B 119.7 . . ? C20B C19B H19B 119.7 . . ? C21B C20B C19B 120.6(4) . . ? C21B C20B H20B 119.7 . . ? C19B C20B H20B 119.7 . . ? C20B C21B C22B 120.7(4) . . ? C20B C21B H21B 119.6 . . ? C22B C21B H21B 119.6 . . ? C23B C22B C17B 120.5(4) . . ? C23B C22B C21B 121.0(4) . . ? C17B C22B C21B 118.5(4) . . ? C22B C23B C24B 119.1(4) . . ? C22B C23B C25B 122.0(4) . . ? C24B C23B C25B 118.7(4) . . ? N1B C24B C23B 118.6(4) . . ? N1B C24B C15B 121.3(4) . . ? C23B C24B C15B 120.1(4) . . ? C26B C25B C23B 176.6(6) . . ? C25B C26B Si1B 170.1(5) . . ? C29B C27B C28B 107.5(9) . . ? C29B C27B Si1B 111.0(7) . . ? C28B C27B Si1B 104.6(8) . . ? C29B C27B H27B 111.2 . . ? C28B C27B H27B 111.2 . . ? Si1B C27B H27B 111.2 . . ? C29C C27C C28C 110.1(8) . . ? C29C C27C Si1B 118.2(8) . . ? C28C C27C Si1B 113.5(7) . . ? C29C C27C H27C 104.5 . . ? C28C C27C H27C 104.5 . . ? Si1B C27C H27C 104.5 . . ? C27B C28B H28D 109.5 . . ? C27B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C27B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C27C C28C H28G 109.5 . . ? C27C C28C H28H 109.5 . . ? H28G C28C H28H 109.5 . . ? C27C C28C H28I 109.5 . . ? H28G C28C H28I 109.5 . . ? H28H C28C H28I 109.5 . . ? C27C C29C H29G 109.5 . . ? C27C C29C H29H 109.5 . . ? H29G C29C H29H 109.5 . . ? C27C C29C H29I 109.5 . . ? H29G C29C H29I 109.5 . . ? H29H C29C H29I 109.5 . . ? C31B C30B C32B 114.9(8) . . ? C31B C30B Si1B 114.3(6) . . ? C32B C30B Si1B 106.4(6) . . ? C31B C30B H30B 106.9 . . ? C32B C30B H30B 106.9 . . ? Si1B C30B H30B 106.9 . . ? C31B C30C C32B 99.2(7) . . ? C31B C30C Si1B 115.1(6) . . ? C32B C30C Si1B 116.2(6) . . ? C31B C30C H30C 108.6 . . ? C32B C30C H30C 108.6 . . ? Si1B C30C H30C 108.6 . . ? C30B C31B C30C 40.0(5) . . ? C30B C31B H31D 109.5 . . ? C30C C31B H31D 117.7 . . ? C30B C31B H31E 109.5 . . ? C30C C31B H31E 130.1 . . ? H31D C31B H31E 109.5 . . ? C30B C31B H31F 109.5 . . ? C30C C31B H31F 70.0 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C30B C32B C30C 37.7(5) . . ? C30B C32B H32D 109.5 . . ? C30C C32B H32D 114.3 . . ? C30B C32B H32E 109.5 . . ? C30C C32B H32E 73.0 . . ? H32D C32B H32E 109.5 . . ? C30B C32B H32F 109.5 . . ? C30C C32B H32F 132.3 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C34B C33B C35B 109.6(4) . . ? C34B C33B Si1B 111.8(4) . . ? C35B C33B Si1B 112.8(4) . . ? C34B C33B H33B 107.4 . . ? C35B C33B H33B 107.4 . . ? Si1B C33B H33B 107.4 . . ? C33B C34B H34D 109.5 . . ? C33B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C33B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C33B C35B H35D 109.5 . . ? C33B C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C33B C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? C37B C36B C16B 175.8(5) . . ? C36B C37B Si2B 173.0(4) . . ? C39B C38B C40B 110.5(4) . . ? C39B C38B Si2B 111.9(3) . . ? C40B C38B Si2B 111.6(3) . . ? C39B C38B H38B 107.5 . . ? C40B C38B H38B 107.5 . . ? Si2B C38B H38B 107.5 . . ? C38B C39B H39D 109.5 . . ? C38B C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? C38B C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C38B C40B H40D 109.5 . . ? C38B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C38B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C42B C41B C43B 109.7(4) . . ? C42B C41B Si2B 112.9(3) . . ? C43B C41B Si2B 114.5(4) . . ? C42B C41B H41B 106.4 . . ? C43B C41B H41B 106.4 . . ? Si2B C41B H41B 106.4 . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C41B C43B H43D 109.5 . . ? C41B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C41B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C45B C44B C46B 109.6(4) . . ? C45B C44B Si2B 113.4(3) . . ? C46B C44B Si2B 112.4(3) . . ? C45B C44B H44B 107.0 . . ? C46B C44B H44B 107.0 . . ? Si2B C44B H44B 107.0 . . ? C44B C45B H45D 109.5 . . ? C44B C45B H45E 109.5 . . ? H45D C45B H45E 109.5 . . ? C44B C45B H45F 109.5 . . ? H45D C45B H45F 109.5 . . ? H45E C45B H45F 109.5 . . ? C44B C46B H46D 109.5 . . ? C44B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C44B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? C1 N1 C24 117.4(4) . . ? C14 N2 C15 117.4(4) . . ? C1B N1B C24B 116.8(4) . . ? C14B N2B C15B 117.3(4) . . ? C26 Si1 C27 103.8(2) . . ? C26 Si1 C33 106.8(2) . . ? C27 Si1 C33 112.5(2) . . ? C26 Si1 C30 109.3(2) . . ? C27 Si1 C30 111.3(2) . . ? C33 Si1 C30 112.6(3) . . ? C37 Si2 C44 108.0(2) . . ? C37 Si2 C41 109.7(2) . . ? C44 Si2 C41 112.5(2) . . ? C37 Si2 C38 105.4(2) . . ? C44 Si2 C38 110.3(2) . . ? C41 Si2 C38 110.6(2) . . ? C30C Si1B C27B 73.5(5) . . ? C30C Si1B C26B 113.2(4) . . ? C27B Si1B C26B 114.4(3) . . ? C30C Si1B C33B 121.5(4) . . ? C27B Si1B C33B 121.1(4) . . ? C26B Si1B C33B 109.3(2) . . ? C30C Si1B C27C 105.6(5) . . ? C27B Si1B C27C 32.1(4) . . ? C26B Si1B C27C 100.4(4) . . ? C33B Si1B C27C 104.2(4) . . ? C30C Si1B C30B 31.2(4) . . ? C27B Si1B C30B 104.7(5) . . ? C26B Si1B C30B 100.7(4) . . ? C33B Si1B C30B 103.8(4) . . ? C27C Si1B C30B 136.7(5) . . ? C37B Si2B C44B 106.2(2) . . ? C37B Si2B C41B 107.7(2) . . ? C44B Si2B C41B 111.4(2) . . ? C37B Si2B C38B 107.4(2) . . ? C44B Si2B C38B 111.2(2) . . ? C41B Si2B C38B 112.6(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -2.5(7) . . . . ? C14 C1 C2 C3 177.3(5) . . . . ? N1 C1 C2 C7 176.7(4) . . . . ? C14 C1 C2 C7 -3.4(7) . . . . ? C7 C2 C3 C4 0.3(8) . . . . ? C1 C2 C3 C4 179.5(5) . . . . ? C2 C3 C4 C5 -0.3(9) . . . . ? C3 C4 C5 C6 0.2(9) . . . . ? C4 C5 C6 C7 -0.1(9) . . . . ? C5 C6 C7 C2 0.1(8) . . . . ? C5 C6 C7 C8 179.4(5) . . . . ? C3 C2 C7 C6 -0.1(8) . . . . ? C1 C2 C7 C6 -179.4(5) . . . . ? C3 C2 C7 C8 -179.5(5) . . . . ? C1 C2 C7 C8 1.3(7) . . . . ? C6 C7 C8 C13 -178.9(5) . . . . ? C2 C7 C8 C13 0.4(8) . . . . ? C6 C7 C8 C9 2.5(8) . . . . ? C2 C7 C8 C9 -178.3(5) . . . . ? C13 C8 C9 C10 1.0(8) . . . . ? C7 C8 C9 C10 179.7(5) . . . . ? C8 C9 C10 C11 -0.6(9) . . . . ? C9 C10 C11 C12 1.0(9) . . . . ? C10 C11 C12 C13 -2.1(8) . . . . ? C11 C12 C13 C8 2.6(8) . . . . ? C11 C12 C13 C14 -178.1(4) . . . . ? C9 C8 C13 C12 -2.0(7) . . . . ? C7 C8 C13 C12 179.3(4) . . . . ? C9 C8 C13 C14 178.7(4) . . . . ? C7 C8 C13 C14 0.0(7) . . . . ? N1 C1 C14 N2 0.0(8) . . . . ? C2 C1 C14 N2 -179.8(5) . . . . ? N1 C1 C14 C13 -176.4(4) . . . . ? C2 C1 C14 C13 3.8(7) . . . . ? C12 C13 C14 N2 2.1(7) . . . . ? C8 C13 C14 N2 -178.6(5) . . . . ? C12 C13 C14 C1 178.7(4) . . . . ? C8 C13 C14 C1 -2.1(7) . . . . ? N2 C15 C16 C17 -178.5(4) . . . . ? C24 C15 C16 C17 4.6(7) . . . . ? N2 C15 C16 C36 4.5(7) . . . . ? C24 C15 C16 C36 -172.4(4) . . . . ? C15 C16 C17 C22 -5.0(7) . . . . ? C36 C16 C17 C22 171.9(4) . . . . ? C15 C16 C17 C18 176.4(5) . . . . ? C36 C16 C17 C18 -6.7(7) . . . . ? C16 C17 C18 C19 -179.7(4) . . . . ? C22 C17 C18 C19 1.7(7) . . . . ? C17 C18 C19 C20 -1.6(7) . . . . ? C18 C19 C20 C21 0.6(8) . . . . ? C19 C20 C21 C22 0.4(8) . . . . ? C16 C17 C22 C23 1.2(7) . . . . ? C18 C17 C22 C23 179.8(5) . . . . ? C16 C17 C22 C21 -179.3(4) . . . . ? C18 C17 C22 C21 -0.7(7) . . . . ? C20 C21 C22 C23 179.2(5) . . . . ? C20 C21 C22 C17 -0.3(7) . . . . ? C17 C22 C23 C24 3.1(7) . . . . ? C21 C22 C23 C24 -176.4(4) . . . . ? C17 C22 C23 C25 -174.8(4) . . . . ? C21 C22 C23 C25 5.7(8) . . . . ? C22 C23 C24 N1 176.0(5) . . . . ? C25 C23 C24 N1 -6.0(7) . . . . ? C22 C23 C24 C15 -3.5(7) . . . . ? C25 C23 C24 C15 174.5(4) . . . . ? N2 C15 C24 N1 3.2(7) . . . . ? C16 C15 C24 N1 -179.9(5) . . . . ? N2 C15 C24 C23 -177.2(4) . . . . ? C16 C15 C24 C23 -0.3(7) . . . . ? C22 C23 C25 C26 142(5) . . . . ? C24 C23 C25 C26 -36(5) . . . . ? C23 C25 C26 Si1 -12(7) . . . . ? C15 C16 C36 C37 56(5) . . . . ? C17 C16 C36 C37 -121(5) . . . . ? C16 C36 C37 Si2 -6(7) . . . . ? N1B C1B C2B C3B 3.2(7) . . . . ? C14B C1B C2B C3B -177.6(4) . . . . ? N1B C1B C2B C7B -177.5(4) . . . . ? C14B C1B C2B C7B 1.6(7) . . . . ? C7B C2B C3B C4B 1.4(8) . . . . ? C1B C2B C3B C4B -179.3(5) . . . . ? C2B C3B C4B C5B -1.2(8) . . . . ? C3B C4B C5B C6B 0.9(8) . . . . ? C4B C5B C6B C7B -0.9(9) . . . . ? C3B C2B C7B C6B -1.3(7) . . . . ? C1B C2B C7B C6B 179.4(5) . . . . ? C3B C2B C7B C8B 178.9(4) . . . . ? C1B C2B C7B C8B -0.4(7) . . . . ? C5B C6B C7B C2B 1.1(8) . . . . ? C5B C6B C7B C8B -179.1(5) . . . . ? C2B C7B C8B C13B -1.1(7) . . . . ? C6B C7B C8B C13B 179.1(5) . . . . ? C2B C7B C8B C9B 179.0(4) . . . . ? C6B C7B C8B C9B -0.8(8) . . . . ? C13B C8B C9B C10B 0.9(7) . . . . ? C7B C8B C9B C10B -179.3(5) . . . . ? C8B C9B C10B C11B -0.9(8) . . . . ? C9B C10B C11B C12B 0.8(8) . . . . ? C10B C11B C12B C13B -0.6(8) . . . . ? C11B C12B C13B C8B 0.7(8) . . . . ? C11B C12B C13B C14B 178.7(4) . . . . ? C9B C8B C13B C12B -0.8(7) . . . . ? C7B C8B C13B C12B 179.4(4) . . . . ? C9B C8B C13B C14B -178.8(4) . . . . ? C7B C8B C13B C14B 1.3(7) . . . . ? N1B C1B C14B N2B -3.9(8) . . . . ? C2B C1B C14B N2B 177.0(5) . . . . ? N1B C1B C14B C13B 177.7(4) . . . . ? C2B C1B C14B C13B -1.4(7) . . . . ? C12B C13B C14B N2B 3.4(7) . . . . ? C8B C13B C14B N2B -178.5(5) . . . . ? C12B C13B C14B C1B -178.1(4) . . . . ? C8B C13B C14B C1B 0.0(7) . . . . ? N2B C15B C16B C17B -176.8(4) . . . . ? C24B C15B C16B C17B 5.1(7) . . . . ? N2B C15B C16B C36B 4.8(7) . . . . ? C24B C15B C16B C36B -173.3(4) . . . . ? C15B C16B C17B C22B -2.7(7) . . . . ? C36B C16B C17B C22B 175.7(4) . . . . ? C15B C16B C17B C18B 178.0(5) . . . . ? C36B C16B C17B C18B -3.6(7) . . . . ? C16B C17B C18B C19B -179.0(4) . . . . ? C22B C17B C18B C19B 1.7(7) . . . . ? C17B C18B C19B C20B -1.3(7) . . . . ? C18B C19B C20B C21B 1.3(8) . . . . ? C19B C20B C21B C22B -1.7(8) . . . . ? C16B C17B C22B C23B -0.3(7) . . . . ? C18B C17B C22B C23B 179.0(5) . . . . ? C16B C17B C22B C21B 178.7(4) . . . . ? C18B C17B C22B C21B -2.0(7) . . . . ? C20B C21B C22B C23B -179.0(5) . . . . ? C20B C21B C22B C17B 2.1(7) . . . . ? C17B C22B C23B C24B 0.9(7) . . . . ? C21B C22B C23B C24B -178.0(4) . . . . ? C17B C22B C23B C25B -173.7(4) . . . . ? C21B C22B C23B C25B 7.4(7) . . . . ? C22B C23B C24B N1B -179.5(5) . . . . ? C25B C23B C24B N1B -4.7(7) . . . . ? C22B C23B C24B C15B 1.4(7) . . . . ? C25B C23B C24B C15B 176.2(4) . . . . ? N2B C15B C24B N1B -1.6(7) . . . . ? C16B C15B C24B N1B 176.5(5) . . . . ? N2B C15B C24B C23B 177.4(4) . . . . ? C16B C15B C24B C23B -4.5(7) . . . . ? C22B C23B C25B C26B 89(8) . . . . ? C24B C23B C25B C26B -86(8) . . . . ? C23B C25B C26B Si1B 35(10) . . . . ? C32B C30B C31B C30C -69.2(10) . . . . ? Si1B C30B C31B C30C 54.2(6) . . . . ? C32B C30C C31B C30B 56.0(8) . . . . ? Si1B C30C C31B C30B -68.7(8) . . . . ? C31B C30B C32B C30C 74.9(10) . . . . ? Si1B C30B C32B C30C -52.6(6) . . . . ? C31B C30C C32B C30B -48.0(7) . . . . ? Si1B C30C C32B C30B 75.9(8) . . . . ? C15B C16B C36B C37B 75(6) . . . . ? C17B C16B C36B C37B -104(6) . . . . ? C16B C36B C37B Si2B -2(9) . . . . ? C14 C1 N1 C24 -0.2(7) . . . . ? C2 C1 N1 C24 179.7(5) . . . . ? C23 C24 N1 C1 179.1(4) . . . . ? C15 C24 N1 C1 -1.4(7) . . . . ? C1 C14 N2 C15 1.8(7) . . . . ? C13 C14 N2 C15 178.2(4) . . . . ? C16 C15 N2 C14 179.8(5) . . . . ? C24 C15 N2 C14 -3.3(7) . . . . ? C14B C1B N1B C24B 2.8(7) . . . . ? C2B C1B N1B C24B -178.1(5) . . . . ? C23B C24B N1B C1B -179.3(4) . . . . ? C15B C24B N1B C1B -0.2(7) . . . . ? C1B C14B N2B C15B 1.9(7) . . . . ? C13B C14B N2B C15B -179.6(4) . . . . ? C16B C15B N2B C14B -177.4(5) . . . . ? C24B C15B N2B C14B 0.7(7) . . . . ? C25 C26 Si1 C27 -24(2) . . . . ? C25 C26 Si1 C33 -144(2) . . . . ? C25 C26 Si1 C30 94(2) . . . . ? C28 C27 Si1 C26 -175.3(3) . . . . ? C29 C27 Si1 C26 58.1(4) . . . . ? C28 C27 Si1 C33 -60.2(4) . . . . ? C29 C27 Si1 C33 173.2(3) . . . . ? C28 C27 Si1 C30 67.2(4) . . . . ? C29 C27 Si1 C30 -59.3(4) . . . . ? C34 C33 Si1 C26 66.0(4) . . . . ? C35 C33 Si1 C26 -58.8(4) . . . . ? C34 C33 Si1 C27 -47.3(4) . . . . ? C35 C33 Si1 C27 -172.1(4) . . . . ? C34 C33 Si1 C30 -174.1(4) . . . . ? C35 C33 Si1 C30 61.2(4) . . . . ? C32 C30 Si1 C26 30.7(5) . . . . ? C31 C30 Si1 C26 158.3(4) . . . . ? C32 C30 Si1 C27 144.7(4) . . . . ? C31 C30 Si1 C27 -87.6(4) . . . . ? C32 C30 Si1 C33 -87.9(4) . . . . ? C31 C30 Si1 C33 39.7(5) . . . . ? C36 C37 Si2 C44 -153(2) . . . . ? C36 C37 Si2 C41 84(2) . . . . ? C36 C37 Si2 C38 -35(2) . . . . ? C46 C44 Si2 C37 66.2(4) . . . . ? C45 C44 Si2 C37 -57.6(4) . . . . ? C46 C44 Si2 C41 -172.6(3) . . . . ? C45 C44 Si2 C41 63.7(4) . . . . ? C46 C44 Si2 C38 -48.5(4) . . . . ? C45 C44 Si2 C38 -172.3(3) . . . . ? C42 C41 Si2 C37 153.2(3) . . . . ? C43 C41 Si2 C37 26.0(4) . . . . ? C42 C41 Si2 C44 32.9(4) . . . . ? C43 C41 Si2 C44 -94.3(4) . . . . ? C42 C41 Si2 C38 -90.9(4) . . . . ? C43 C41 Si2 C38 141.9(3) . . . . ? C40 C38 Si2 C37 52.4(4) . . . . ? C39 C38 Si2 C37 177.3(4) . . . . ? C40 C38 Si2 C44 168.8(4) . . . . ? C39 C38 Si2 C44 -66.4(4) . . . . ? C40 C38 Si2 C41 -66.1(4) . . . . ? C39 C38 Si2 C41 58.7(4) . . . . ? C31B C30C Si1B C27B -130.5(8) . . . . ? C32B C30C Si1B C27B 114.3(8) . . . . ? C31B C30C Si1B C26B -20.5(8) . . . . ? C32B C30C Si1B C26B -135.7(7) . . . . ? C31B C30C Si1B C33B 112.7(7) . . . . ? C32B C30C Si1B C33B -2.5(10) . . . . ? C31B C30C Si1B C27C -129.3(7) . . . . ? C32B C30C Si1B C27C 115.4(8) . . . . ? C31B C30C Si1B C30B 51.0(8) . . . . ? C32B C30C Si1B C30B -64.3(9) . . . . ? C29B C27B Si1B C30C -93.3(8) . . . . ? C28B C27B Si1B C30C 151.1(9) . . . . ? C29B C27B Si1B C26B 158.3(7) . . . . ? C28B C27B Si1B C26B 42.7(9) . . . . ? C29B C27B Si1B C33B 24.0(10) . . . . ? C28B C27B Si1B C33B -91.6(7) . . . . ? C29B C27B Si1B C27C 88.9(12) . . . . ? C28B C27B Si1B C27C -26.7(7) . . . . ? C29B C27B Si1B C30B -92.5(9) . . . . ? C28B C27B Si1B C30B 151.9(7) . . . . ? C25B C26B Si1B C30C 4(3) . . . . ? C25B C26B Si1B C27B 85(3) . . . . ? C25B C26B Si1B C33B -135(3) . . . . ? C25B C26B Si1B C27C 116(3) . . . . ? C25B C26B Si1B C30B -26(3) . . . . ? C34B C33B Si1B C30C -73.5(6) . . . . ? C35B C33B Si1B C30C 162.3(5) . . . . ? C34B C33B Si1B C27B -162.5(5) . . . . ? C35B C33B Si1B C27B 73.4(6) . . . . ? C34B C33B Si1B C26B 61.3(5) . . . . ? C35B C33B Si1B C26B -62.9(5) . . . . ? C34B C33B Si1B C27C 167.8(5) . . . . ? C35B C33B Si1B C27C 43.7(6) . . . . ? C34B C33B Si1B C30B -45.5(5) . . . . ? C35B C33B Si1B C30B -169.7(5) . . . . ? C29C C27C Si1B C30C -69.0(9) . . . . ? C28C C27C Si1B C30C 62.2(10) . . . . ? C29C C27C Si1B C27B -66.9(11) . . . . ? C28C C27C Si1B C27B 64.3(10) . . . . ? C29C C27C Si1B C26B 173.2(8) . . . . ? C28C C27C Si1B C26B -55.6(9) . . . . ? C29C C27C Si1B C33B 60.0(9) . . . . ? C28C C27C Si1B C33B -168.7(8) . . . . ? C29C C27C Si1B C30B -68.8(10) . . . . ? C28C C27C Si1B C30B 62.4(11) . . . . ? C31B C30B Si1B C30C -67.1(9) . . . . ? C32B C30B Si1B C30C 60.8(9) . . . . ? C31B C30B Si1B C27B -68.5(9) . . . . ? C32B C30B Si1B C27B 59.3(7) . . . . ? C31B C30B Si1B C26B 50.5(9) . . . . ? C32B C30B Si1B C26B 178.3(5) . . . . ? C31B C30B Si1B C33B 163.6(8) . . . . ? C32B C30B Si1B C33B -68.6(6) . . . . ? C31B C30B Si1B C27C -67.5(11) . . . . ? C32B C30B Si1B C27C 60.4(8) . . . . ? C36B C37B Si2B C44B 98(3) . . . . ? C36B C37B Si2B C41B -22(3) . . . . ? C36B C37B Si2B C38B -143(3) . . . . ? C45B C44B Si2B C37B -177.8(4) . . . . ? C46B C44B Si2B C37B -52.9(4) . . . . ? C45B C44B Si2B C41B -60.8(4) . . . . ? C46B C44B Si2B C41B 64.1(4) . . . . ? C45B C44B Si2B C38B 65.6(4) . . . . ? C46B C44B Si2B C38B -169.4(3) . . . . ? C42B C41B Si2B C37B -156.2(3) . . . . ? C43B C41B Si2B C37B -29.8(4) . . . . ? C42B C41B Si2B C44B 87.7(4) . . . . ? C43B C41B Si2B C44B -145.9(3) . . . . ? C42B C41B Si2B C38B -38.0(4) . . . . ? C43B C41B Si2B C38B 88.4(4) . . . . ? C39B C38B Si2B C37B 58.8(4) . . . . ? C40B C38B Si2B C37B -65.7(4) . . . . ? C39B C38B Si2B C44B 174.6(4) . . . . ? C40B C38B Si2B C44B 50.1(4) . . . . ? C39B C38B Si2B C41B -59.6(4) . . . . ? C40B C38B Si2B C41B 175.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.764 _diffrn_reflns_theta_full 66.22 _diffrn_measured_fraction_theta_full 0.764 _refine_diff_density_max 0.434 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.058 _database_code_depnum_ccdc_archive 'CCDC 936730' ####################################################################### # # 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_nb_03s _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4b in manuscript' _chemical_melting_point ? _chemical_formula_moiety 'C54 H74 N2 Si2' _chemical_formula_sum 'C54 H74 N2 Si2' _chemical_formula_weight 807.33 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1333(12) _cell_length_b 13.6022(15) _cell_length_c 17.6452(19) _cell_angle_alpha 80.944(2) _cell_angle_beta 81.277(2) _cell_angle_gamma 72.615(2) _cell_volume 2502.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5298 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 30.64 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.106 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9709 _exptl_absorpt_correction_T_max 0.9750 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 51136 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0747 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 30.51 _reflns_number_total 15173 _reflns_number_gt 8602 _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^)+(0.0958P)^2^+0.2111P] 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 15173 _refine_ls_number_parameters 517 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1222 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.2064 _refine_ls_wR_factor_gt 0.1716 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.070 _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 C1 C 0.75656(17) 0.61031(13) 0.78738(9) 0.0200(4) Uani 1 1 d . . . C2 C 0.75633(17) 0.51249(13) 0.82775(10) 0.0215(4) Uani 1 1 d . . . C3 C 0.75240(17) 0.43214(14) 0.78694(10) 0.0226(4) Uani 1 1 d . . . C4 C 0.7496(2) 0.33228(15) 0.82528(11) 0.0299(4) Uani 1 1 d . . . H4A H 0.7515 0.3185 0.8796 0.036 Uiso 1 1 calc R . . C5 C 0.7443(2) 0.25639(16) 0.78510(12) 0.0360(5) Uani 1 1 d . . . H5A H 0.7428 0.1903 0.8116 0.043 Uiso 1 1 calc R . . C6 C 0.7411(2) 0.27498(16) 0.70454(12) 0.0363(5) Uani 1 1 d . . . H6A H 0.7372 0.2213 0.6773 0.044 Uiso 1 1 calc R . . C7 C 0.7436(2) 0.36881(15) 0.66530(11) 0.0303(4) Uani 1 1 d . . . H7A H 0.7414 0.3800 0.6110 0.036 Uiso 1 1 calc R . . C8 C 0.74941(18) 0.45086(14) 0.70483(10) 0.0231(4) Uani 1 1 d . . . C9 C 0.75367(18) 0.54839(14) 0.66443(10) 0.0226(4) Uani 1 1 d . . . C10 C 0.75944(17) 0.62710(13) 0.70568(10) 0.0209(4) Uani 1 1 d . . . C11 C 0.76685(18) 0.79478(14) 0.70535(10) 0.0236(4) Uani 1 1 d . . . C12 C 0.74336(18) 0.78279(14) 0.78921(10) 0.0224(4) Uani 1 1 d . . . C13 C 0.71195(18) 0.86922(14) 0.83748(10) 0.0241(4) Uani 1 1 d . . . C14 C 0.7527(2) 0.84921(15) 0.91075(11) 0.0291(4) Uani 1 1 d . . . H14A H 0.8030 0.7818 0.9279 0.035 Uiso 1 1 calc R . . C15 C 0.7205(2) 0.92677(16) 0.95887(12) 0.0331(5) Uani 1 1 d . . . H15A H 0.7503 0.9119 1.0083 0.040 Uiso 1 1 calc R . . C16 C 0.6454(2) 1.02568(15) 0.93614(12) 0.0315(4) Uani 1 1 d . . . C17 C 0.6019(2) 1.04462(15) 0.86390(12) 0.0319(4) Uani 1 1 d . . . H17A H 0.5480 1.1110 0.8479 0.038 Uiso 1 1 calc R . . C18 C 0.6357(2) 0.96818(15) 0.81480(11) 0.0299(4) Uani 1 1 d . . . H18A H 0.6066 0.9834 0.7652 0.036 Uiso 1 1 calc R . . C19 C 0.6124(2) 1.10983(18) 0.98845(13) 0.0442(6) Uani 1 1 d . . . H19A H 0.6513 1.0822 1.0364 0.066 Uiso 1 1 calc R . . H19B H 0.5202 1.1342 1.0003 0.066 Uiso 1 1 calc R . . H19C H 0.6442 1.1678 0.9626 0.066 Uiso 1 1 calc R . . C20 C 0.79268(19) 0.88820(14) 0.65741(10) 0.0259(4) Uani 1 1 d . . . C21 C 0.7493(2) 0.91703(16) 0.58496(11) 0.0331(5) Uani 1 1 d . . . H21A H 0.7012 0.8791 0.5682 0.040 Uiso 1 1 calc R . . C22 C 0.7760(2) 1.00096(17) 0.53690(12) 0.0384(5) Uani 1 1 d . . . H22A H 0.7445 1.0202 0.4880 0.046 Uiso 1 1 calc R . . C23 C 0.8474(2) 1.05719(15) 0.55879(12) 0.0340(5) Uani 1 1 d . . . C24 C 0.8936(2) 1.02610(15) 0.63038(12) 0.0338(5) Uani 1 1 d . . . H24A H 0.9453 1.0620 0.6459 0.041 Uiso 1 1 calc R . . C25 C 0.8654(2) 0.94354(15) 0.67959(11) 0.0302(4) Uani 1 1 d . . . H25A H 0.8962 0.9248 0.7287 0.036 Uiso 1 1 calc R . . C26 C 0.8739(3) 1.14964(17) 0.50678(13) 0.0467(6) Uani 1 1 d . . . H26A H 0.8343 1.1595 0.4592 0.070 Uiso 1 1 calc R . . H26B H 0.9656 1.1375 0.4941 0.070 Uiso 1 1 calc R . . H26C H 0.8390 1.2119 0.5333 0.070 Uiso 1 1 calc R . . C27 C 0.75515(18) 0.49588(13) 0.91016(10) 0.0230(4) Uani 1 1 d . . . C28 C 0.75397(19) 0.47864(14) 0.97908(10) 0.0258(4) Uani 1 1 d . . . C29 C 0.7590(2) 0.57520(16) 1.11908(11) 0.0309(4) Uani 1 1 d . . . H29A H 0.7560 0.5634 1.1766 0.037 Uiso 1 1 calc R . . C30 C 0.6463(2) 0.66769(17) 1.09801(14) 0.0457(6) Uani 1 1 d . . . H30A H 0.6536 0.7297 1.1166 0.068 Uiso 1 1 calc R . . H30B H 0.5674 0.6529 1.1222 0.068 Uiso 1 1 calc R . . H30C H 0.6459 0.6797 1.0418 0.068 Uiso 1 1 calc R . . C31 C 0.8835(3) 0.6003(2) 1.08639(14) 0.0477(6) Uani 1 1 d . . . H31A H 0.8855 0.6637 1.1053 0.072 Uiso 1 1 calc R . . H31B H 0.8896 0.6106 1.0299 0.072 Uiso 1 1 calc R . . H31C H 0.9549 0.5427 1.1031 0.072 Uiso 1 1 calc R . . C32 C 0.59360(18) 0.42649(15) 1.12299(10) 0.0271(4) Uani 1 1 d . . . H32A H 0.5265 0.4905 1.1063 0.033 Uiso 1 1 calc R . . C33 C 0.5736(2) 0.4116(2) 1.21132(12) 0.0484(6) Uani 1 1 d . . . H33A H 0.4914 0.3982 1.2285 0.073 Uiso 1 1 calc R . . H33B H 0.5755 0.4744 1.2311 0.073 Uiso 1 1 calc R . . H33C H 0.6411 0.3525 1.2309 0.073 Uiso 1 1 calc R . . C34 C 0.5710(2) 0.33788(19) 1.08846(16) 0.0486(6) Uani 1 1 d . . . H34A H 0.4886 0.3281 1.1106 0.073 Uiso 1 1 calc R . . H34B H 0.6380 0.2738 1.1003 0.073 Uiso 1 1 calc R . . H34C H 0.5721 0.3550 1.0323 0.073 Uiso 1 1 calc R . . C35 C 0.89421(19) 0.34225(16) 1.10555(11) 0.0323(5) Uani 1 1 d . . . H35A H 0.9682 0.3664 1.0792 0.039 Uiso 1 1 calc R . . C36 C 0.9144(2) 0.3173(2) 1.19148(14) 0.0630(9) Uani 1 1 d . . . H36A H 0.9911 0.2595 1.1981 0.094 Uiso 1 1 calc R . . H36B H 0.8413 0.2981 1.2211 0.094 Uiso 1 1 calc R . . H36C H 0.9239 0.3785 1.2101 0.094 Uiso 1 1 calc R . . C37 C 0.9010(3) 0.2453(2) 1.0698(2) 0.0674(9) Uani 1 1 d . . . H37A H 0.9781 0.1908 1.0823 0.101 Uiso 1 1 calc R . . H37B H 0.9028 0.2618 1.0136 0.101 Uiso 1 1 calc R . . H37C H 0.8267 0.2212 1.0906 0.101 Uiso 1 1 calc R . . C38 C 0.75096(19) 0.56851(14) 0.58262(10) 0.0271(4) Uani 1 1 d . . . C39 C 0.7469(2) 0.58396(16) 0.51404(11) 0.0325(5) Uani 1 1 d . . . C40 C 0.5908(3) 0.7089(2) 0.38957(14) 0.0549(7) Uani 1 1 d . . . H40A H 0.5277 0.6684 0.4061 0.066 Uiso 1 1 calc R . . C41 C 0.5471(5) 0.7919(4) 0.4375(3) 0.174(3) Uani 1 1 d . . . H41A H 0.4649 0.8371 0.4235 0.262 Uiso 1 1 calc R . . H41B H 0.6085 0.8322 0.4299 0.262 Uiso 1 1 calc R . . H41C H 0.5380 0.7628 0.4918 0.262 Uiso 1 1 calc R . . C42 C 0.5756(3) 0.7431(3) 0.30425(15) 0.0707(9) Uani 1 1 d . . . H42A H 0.4924 0.7933 0.2989 0.106 Uiso 1 1 calc R . . H42B H 0.5824 0.6826 0.2785 0.106 Uiso 1 1 calc R . . H42C H 0.6421 0.7754 0.2805 0.106 Uiso 1 1 calc R . . C43 C 0.8902(2) 0.65409(18) 0.36955(12) 0.0381(5) Uani 1 1 d . . . H43A H 0.9635 0.5979 0.3892 0.046 Uiso 1 1 calc R . . C44 C 0.8921(3) 0.7517(2) 0.40045(18) 0.0737(9) Uani 1 1 d . . . H44A H 0.9697 0.7703 0.3783 0.111 Uiso 1 1 calc R . . H44B H 0.8896 0.7392 0.4568 0.111 Uiso 1 1 calc R . . H44C H 0.8183 0.8087 0.3861 0.111 Uiso 1 1 calc R . . C45 C 0.9167(3) 0.6636(2) 0.28148(13) 0.0541(7) Uani 1 1 d . . . H45A H 0.9932 0.6865 0.2654 0.081 Uiso 1 1 calc R . . H45B H 0.8447 0.7145 0.2588 0.081 Uiso 1 1 calc R . . H45C H 0.9291 0.5961 0.2639 0.081 Uiso 1 1 calc R . . C46 C 0.7579(3) 0.48288(18) 0.37393(12) 0.0422(6) Uani 1 1 d . . . H46A H 0.7554 0.4958 0.3167 0.051 Uiso 1 1 calc R . . C47 C 0.6466(3) 0.4397(2) 0.40943(15) 0.0674(9) Uani 1 1 d . . . H47A H 0.6567 0.3738 0.3898 0.101 Uiso 1 1 calc R . . H47B H 0.5670 0.4894 0.3953 0.101 Uiso 1 1 calc R . . H47C H 0.6449 0.4282 0.4658 0.101 Uiso 1 1 calc R . . C48 C 0.8841(3) 0.40235(19) 0.38957(15) 0.0592(8) Uani 1 1 d . . . H48A H 0.8877 0.3373 0.3709 0.089 Uiso 1 1 calc R . . H48B H 0.8908 0.3900 0.4452 0.089 Uiso 1 1 calc R . . H48C H 0.9542 0.4283 0.3626 0.089 Uiso 1 1 calc R . . C1A C 0.4213(13) 0.8767(12) 0.6646(9) 0.093(4) Uiso 0.31 1 d PD A 2 H1AA H 0.4234 0.8465 0.6174 0.140 Uiso 0.31 1 calc PR A 2 H1AB H 0.4647 0.8226 0.7029 0.140 Uiso 0.31 1 calc PR A 2 H1AC H 0.4639 0.9316 0.6528 0.140 Uiso 0.31 1 calc PR A 2 C2A C 0.2840(15) 0.9222(12) 0.6970(8) 0.103(5) Uiso 0.31 1 d PD A 2 H2A1 H 0.2414 0.9739 0.6563 0.124 Uiso 0.31 1 calc PR A 2 H2A2 H 0.2425 0.8657 0.7065 0.124 Uiso 0.31 1 calc PR A 2 C3A C 0.2595(13) 0.9713(12) 0.7667(9) 0.099(4) Uiso 0.31 1 d PD A 2 H3A1 H 0.3004 1.0281 0.7578 0.119 Uiso 0.31 1 calc PR A 2 H3A2 H 0.3002 0.9198 0.8081 0.119 Uiso 0.31 1 calc PR A 2 C4A C 0.1262(14) 1.0137(10) 0.7937(7) 0.077(3) Uiso 0.31 1 d PD A 2 H4A1 H 0.0846 1.0732 0.7575 0.093 Uiso 0.31 1 calc PR A 2 H4A2 H 0.0802 0.9603 0.8005 0.093 Uiso 0.31 1 calc PR A 2 C5A C 0.1319(14) 1.0446(13) 0.8632(8) 0.117(5) Uiso 0.31 1 d PD A 2 H5AA H 0.1679 1.1042 0.8555 0.141 Uiso 0.31 1 calc PR A 2 H5AB H 0.1840 0.9871 0.8964 0.141 Uiso 0.31 1 calc PR A 2 C6A C -0.0088(13) 1.0762(12) 0.8995(8) 0.082(4) Uiso 0.31 1 d PD A 2 H6AA H -0.0136 1.1000 0.9498 0.124 Uiso 0.31 1 calc PR A 2 H6AB H -0.0425 1.0162 0.9063 0.124 Uiso 0.31 1 calc PR A 2 H6AC H -0.0588 1.1323 0.8653 0.124 Uiso 0.31 1 calc PR A 2 C1S C 0.4263(5) 0.8399(5) 0.6413(3) 0.0773(15) Uiso 0.69 1 d P B 1 H1SA H 0.5188 0.8129 0.6344 0.116 Uiso 0.69 1 calc PR B 1 H1SB H 0.3975 0.8859 0.5949 0.116 Uiso 0.69 1 calc PR B 1 H1SC H 0.3884 0.7821 0.6497 0.116 Uiso 0.69 1 calc PR B 1 C2S C 0.3851(5) 0.9019(4) 0.7125(3) 0.0678(12) Uiso 0.69 1 d P B 1 H2SA H 0.4165 0.8551 0.7586 0.081 Uiso 0.69 1 calc PR B 1 H2SB H 0.4261 0.9587 0.7040 0.081 Uiso 0.69 1 calc PR B 1 C3S C 0.2421(4) 0.9485(4) 0.7289(3) 0.0616(11) Uiso 0.69 1 d P B 1 H3SA H 0.2115 0.9987 0.6840 0.074 Uiso 0.69 1 calc PR B 1 H3SB H 0.2006 0.8924 0.7340 0.074 Uiso 0.69 1 calc PR B 1 C4S C 0.2022(5) 1.0022(4) 0.7997(3) 0.0588(11) Uiso 0.69 1 d P B 1 H4SA H 0.2383 1.0617 0.7931 0.071 Uiso 0.69 1 calc PR B 1 H4SB H 0.2376 0.9536 0.8441 0.071 Uiso 0.69 1 calc PR B 1 C5S C 0.0562(5) 1.0423(4) 0.8183(3) 0.0650(12) Uiso 0.69 1 d P B 1 H5SA H 0.0196 1.0927 0.7751 0.078 Uiso 0.69 1 calc PR B 1 H5SB H 0.0185 0.9836 0.8251 0.078 Uiso 0.69 1 calc PR B 1 C6S C 0.0269(7) 1.0930(5) 0.8907(4) 0.087(2) Uiso 0.69 1 d P B 1 H6SA H -0.0651 1.1187 0.9028 0.130 Uiso 0.69 1 calc PR B 1 H6SB H 0.0640 1.1512 0.8834 0.130 Uiso 0.69 1 calc PR B 1 H6SC H 0.0626 1.0425 0.9333 0.130 Uiso 0.69 1 calc PR B 1 N1 N 0.74480(15) 0.69147(11) 0.82802(8) 0.0218(3) Uani 1 1 d . . . N2 N 0.76962(15) 0.71972(12) 0.66599(8) 0.0236(3) Uani 1 1 d . . . Si1 Si 0.74959(5) 0.45319(4) 1.08506(3) 0.02348(13) Uani 1 1 d . . . Si2 Si 0.74552(6) 0.60983(4) 0.40837(3) 0.02954(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0234(9) 0.0216(8) 0.0158(8) -0.0040(6) -0.0013(7) -0.0071(7) C2 0.0245(9) 0.0227(8) 0.0162(8) -0.0010(6) -0.0009(7) -0.0062(7) C3 0.0252(10) 0.0224(8) 0.0191(8) -0.0026(7) 0.0008(7) -0.0067(7) C4 0.0414(12) 0.0263(9) 0.0219(9) -0.0012(7) 0.0024(8) -0.0131(9) C5 0.0509(14) 0.0260(10) 0.0328(11) -0.0014(8) 0.0005(10) -0.0169(10) C6 0.0513(14) 0.0294(10) 0.0335(11) -0.0118(9) 0.0005(10) -0.0179(10) C7 0.0419(12) 0.0300(10) 0.0213(9) -0.0066(8) -0.0012(8) -0.0130(9) C8 0.0284(10) 0.0236(9) 0.0175(8) -0.0049(7) 0.0004(7) -0.0074(7) C9 0.0274(10) 0.0252(9) 0.0148(8) -0.0032(7) -0.0013(7) -0.0070(7) C10 0.0250(9) 0.0219(8) 0.0152(8) -0.0028(6) -0.0010(7) -0.0061(7) C11 0.0269(10) 0.0238(9) 0.0201(8) -0.0020(7) -0.0035(7) -0.0072(7) C12 0.0255(9) 0.0234(9) 0.0197(8) -0.0036(7) -0.0035(7) -0.0078(7) C13 0.0288(10) 0.0231(9) 0.0220(9) -0.0031(7) -0.0027(7) -0.0096(8) C14 0.0372(11) 0.0242(9) 0.0265(10) -0.0052(7) -0.0076(8) -0.0065(8) C15 0.0447(13) 0.0315(10) 0.0249(10) -0.0077(8) -0.0098(9) -0.0086(9) C16 0.0363(12) 0.0294(10) 0.0313(10) -0.0108(8) -0.0010(9) -0.0108(9) C17 0.0368(12) 0.0222(9) 0.0349(11) -0.0048(8) -0.0042(9) -0.0048(8) C18 0.0362(11) 0.0287(10) 0.0249(9) -0.0035(8) -0.0078(8) -0.0073(8) C19 0.0564(15) 0.0359(12) 0.0425(13) -0.0195(10) -0.0047(11) -0.0092(11) C20 0.0319(11) 0.0226(9) 0.0216(9) -0.0011(7) -0.0005(8) -0.0070(8) C21 0.0440(13) 0.0298(10) 0.0273(10) 0.0005(8) -0.0076(9) -0.0134(9) C22 0.0540(14) 0.0344(11) 0.0247(10) 0.0047(8) -0.0081(10) -0.0114(10) C23 0.0430(13) 0.0224(9) 0.0320(11) 0.0007(8) 0.0037(9) -0.0084(9) C24 0.0434(13) 0.0258(10) 0.0346(11) -0.0031(8) -0.0016(9) -0.0148(9) C25 0.0394(12) 0.0272(10) 0.0252(10) -0.0009(8) -0.0052(8) -0.0116(9) C26 0.0663(17) 0.0292(11) 0.0400(13) 0.0058(9) 0.0035(12) -0.0160(11) C27 0.0288(10) 0.0188(8) 0.0203(8) -0.0021(7) -0.0003(7) -0.0064(7) C28 0.0300(10) 0.0263(9) 0.0195(8) -0.0030(7) -0.0018(7) -0.0060(8) C29 0.0403(12) 0.0358(11) 0.0185(9) -0.0050(8) -0.0002(8) -0.0142(9) C30 0.0583(16) 0.0320(11) 0.0434(13) -0.0103(10) -0.0058(12) -0.0047(11) C31 0.0579(16) 0.0555(15) 0.0396(13) -0.0115(11) 0.0062(11) -0.0334(13) C32 0.0272(10) 0.0322(10) 0.0208(9) -0.0029(7) -0.0023(7) -0.0071(8) C33 0.0343(13) 0.0830(19) 0.0245(11) 0.0035(11) 0.0025(9) -0.0194(12) C34 0.0394(13) 0.0491(14) 0.0629(16) -0.0219(12) 0.0082(12) -0.0200(11) C35 0.0270(10) 0.0359(11) 0.0275(10) 0.0030(8) -0.0024(8) -0.0027(9) C36 0.0371(14) 0.090(2) 0.0361(13) 0.0203(13) -0.0071(11) 0.0075(14) C37 0.0443(16) 0.0386(14) 0.112(3) -0.0192(15) -0.0195(16) 0.0095(12) C38 0.0365(11) 0.0252(9) 0.0205(9) -0.0050(7) 0.0001(8) -0.0105(8) C39 0.0450(13) 0.0327(10) 0.0217(9) -0.0032(8) -0.0044(9) -0.0133(9) C40 0.0494(16) 0.0693(18) 0.0330(12) -0.0021(12) -0.0057(11) 0.0014(13) C41 0.156(5) 0.179(5) 0.108(4) -0.069(4) -0.046(3) 0.115(4) C42 0.0460(17) 0.106(3) 0.0427(15) 0.0186(16) -0.0129(13) -0.0050(16) C43 0.0439(13) 0.0444(12) 0.0272(10) -0.0005(9) -0.0024(9) -0.0167(10) C44 0.091(2) 0.074(2) 0.073(2) -0.0225(17) 0.0151(18) -0.054(2) C45 0.0465(15) 0.0796(19) 0.0324(12) 0.0043(12) 0.0026(11) -0.0208(14) C46 0.0680(17) 0.0459(13) 0.0187(9) -0.0059(9) -0.0025(10) -0.0253(12) C47 0.104(3) 0.082(2) 0.0397(14) -0.0106(14) -0.0017(15) -0.064(2) C48 0.093(2) 0.0368(13) 0.0423(14) -0.0066(11) -0.0050(14) -0.0097(14) N1 0.0272(8) 0.0220(7) 0.0171(7) -0.0032(6) -0.0025(6) -0.0080(6) N2 0.0300(9) 0.0242(8) 0.0171(7) 0.0002(6) -0.0028(6) -0.0098(6) Si1 0.0272(3) 0.0273(3) 0.0136(2) -0.00088(19) -0.00134(19) -0.0055(2) Si2 0.0386(3) 0.0359(3) 0.0144(2) -0.0033(2) -0.0024(2) -0.0110(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.373(2) . ? C1 C2 1.407(2) . ? C1 C10 1.421(2) . ? C2 C3 1.414(2) . ? C2 C27 1.435(2) . ? C3 C4 1.426(2) . ? C3 C8 1.435(2) . ? C4 C5 1.361(3) . ? C4 H4A 0.9500 . ? C5 C6 1.408(3) . ? C5 H5A 0.9500 . ? C6 C7 1.359(3) . ? C6 H6A 0.9500 . ? C7 C8 1.428(3) . ? C7 H7A 0.9500 . ? C8 C9 1.414(2) . ? C9 C10 1.407(2) . ? C9 C38 1.430(2) . ? C10 N2 1.369(2) . ? C11 N2 1.313(2) . ? C11 C12 1.455(2) . ? C11 C20 1.490(2) . ? C12 N1 1.317(2) . ? C12 C13 1.486(2) . ? C13 C18 1.394(3) . ? C13 C14 1.395(3) . ? C14 C15 1.388(3) . ? C14 H14A 0.9500 . ? C15 C16 1.389(3) . ? C15 H15A 0.9500 . ? C16 C17 1.391(3) . ? C16 C19 1.508(3) . ? C17 C18 1.387(3) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.389(3) . ? C20 C21 1.392(3) . ? C21 C22 1.390(3) . ? C21 H21A 0.9500 . ? C22 C23 1.385(3) . ? C22 H22A 0.9500 . ? C23 C24 1.392(3) . ? C23 C26 1.512(3) . ? C24 C25 1.391(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.201(2) . ? C28 Si1 1.8432(18) . ? C29 C30 1.531(3) . ? C29 C31 1.533(3) . ? C29 Si1 1.887(2) . ? C29 H29A 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.531(3) . ? C32 C34 1.532(3) . ? C32 Si1 1.883(2) . ? C32 H32A 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C37 1.526(3) . ? C35 C36 1.536(3) . ? C35 Si1 1.885(2) . ? C35 H35A 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.200(3) . ? C39 Si2 1.844(2) . ? C40 C41 1.440(5) . ? C40 C42 1.524(3) . ? C40 Si2 1.881(3) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.520(3) . ? C43 C45 1.529(3) . ? C43 Si2 1.881(2) . ? C43 H43A 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C48 1.534(4) . ? C46 C47 1.536(4) . ? C46 Si2 1.880(2) . ? C46 H46A 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C1A C2A 1.525(17) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C2A C3A 1.442(15) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A C4A 1.457(14) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A C5A 1.374(14) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5A C6A 1.558(18) . ? C5A H5AA 0.9900 . ? C5A H5AB 0.9900 . ? C6A H6AA 0.9800 . ? C6A H6AB 0.9800 . ? C6A H6AC 0.9800 . ? C1S C2S 1.558(7) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S C3S 1.529(7) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S C4S 1.489(7) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S C5S 1.554(7) . ? C4S H4SA 0.9900 . ? C4S H4SB 0.9900 . ? C5S C6S 1.493(8) . ? C5S H5SA 0.9900 . ? C5S H5SB 0.9900 . ? C6S H6SA 0.9800 . ? C6S H6SB 0.9800 . ? C6S H6SC 0.9800 . ? 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 C1 C2 119.37(15) . . ? N1 C1 C10 120.06(15) . . ? C2 C1 C10 120.41(15) . . ? C1 C2 C3 119.61(15) . . ? C1 C2 C27 120.01(16) . . ? C3 C2 C27 120.34(15) . . ? C2 C3 C4 121.81(16) . . ? C2 C3 C8 119.76(15) . . ? C4 C3 C8 118.42(16) . . ? C5 C4 C3 120.91(18) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 120.59(18) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C7 C6 C5 120.78(19) . . ? C7 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C6 C7 C8 120.75(18) . . ? C6 C7 H7A 119.6 . . ? C8 C7 H7A 119.6 . . ? C9 C8 C7 121.21(16) . . ? C9 C8 C3 120.24(16) . . ? C7 C8 C3 118.55(16) . . ? C10 C9 C8 119.34(15) . . ? C10 C9 C38 119.59(15) . . ? C8 C9 C38 121.08(16) . . ? N2 C10 C9 119.16(15) . . ? N2 C10 C1 120.32(15) . . ? C9 C10 C1 120.52(15) . . ? N2 C11 C12 120.74(15) . . ? N2 C11 C20 114.61(15) . . ? C12 C11 C20 124.63(16) . . ? N1 C12 C11 120.67(16) . . ? N1 C12 C13 114.79(15) . . ? C11 C12 C13 124.51(15) . . ? C18 C13 C14 118.26(17) . . ? C18 C13 C12 122.65(17) . . ? C14 C13 C12 118.94(16) . . ? C15 C14 C13 120.64(18) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C16 121.18(18) . . ? C14 C15 H15A 119.4 . . ? C16 C15 H15A 119.4 . . ? C15 C16 C17 118.06(18) . . ? C15 C16 C19 120.76(19) . . ? C17 C16 C19 121.18(19) . . ? C18 C17 C16 121.12(18) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C13 120.70(18) . . ? C17 C18 H18A 119.7 . . ? C13 C18 H18A 119.7 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 118.51(17) . . ? C25 C20 C11 122.84(17) . . ? C21 C20 C11 118.50(17) . . ? C22 C21 C20 120.5(2) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C23 C22 C21 121.42(19) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C22 C23 C24 117.80(18) . . ? C22 C23 C26 121.1(2) . . ? C24 C23 C26 121.1(2) . . ? C25 C24 C23 121.27(19) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C20 C25 C24 120.48(18) . . ? C20 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C2 177.80(19) . . ? C27 C28 Si1 179.14(19) . . ? C30 C29 C31 110.03(18) . . ? C30 C29 Si1 111.37(15) . . ? C31 C29 Si1 111.54(15) . . ? C30 C29 H29A 107.9 . . ? C31 C29 H29A 107.9 . . ? Si1 C29 H29A 107.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C34 111.75(19) . . ? C33 C32 Si1 112.22(14) . . ? C34 C32 Si1 113.76(14) . . ? C33 C32 H32A 106.2 . . ? C34 C32 H32A 106.2 . . ? Si1 C32 H32A 106.2 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 C35 C36 111.9(2) . . ? C37 C35 Si1 113.36(16) . . ? C36 C35 Si1 113.64(16) . . ? C37 C35 H35A 105.7 . . ? C36 C35 H35A 105.7 . . ? Si1 C35 H35A 105.7 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C9 178.5(2) . . ? C38 C39 Si2 177.91(19) . . ? C41 C40 C42 114.4(3) . . ? C41 C40 Si2 116.9(2) . . ? C42 C40 Si2 114.08(19) . . ? C41 C40 H40A 102.9 . . ? C42 C40 H40A 102.9 . . ? Si2 C40 H40A 102.9 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C45 111.3(2) . . ? C44 C43 Si2 113.57(18) . . ? C45 C43 Si2 113.83(16) . . ? C44 C43 H43A 105.8 . . ? C45 C43 H43A 105.8 . . ? Si2 C43 H43A 105.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C48 C46 C47 110.3(2) . . ? C48 C46 Si2 111.44(17) . . ? C47 C46 Si2 112.23(18) . . ? C48 C46 H46A 107.5 . . ? C47 C46 H46A 107.5 . . ? Si2 C46 H46A 107.5 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C2A C1A H1AA 109.5 . . ? C2A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C3A C2A C1A 118.4(14) . . ? C3A C2A H2A1 107.7 . . ? C1A C2A H2A1 107.7 . . ? C3A C2A H2A2 107.7 . . ? C1A C2A H2A2 107.7 . . ? H2A1 C2A H2A2 107.1 . . ? C2A C3A C4A 115.3(15) . . ? C2A C3A H3A1 108.5 . . ? C4A C3A H3A1 108.5 . . ? C2A C3A H3A2 108.5 . . ? C4A C3A H3A2 108.5 . . ? H3A1 C3A H3A2 107.5 . . ? C5A C4A C3A 102.4(14) . . ? C5A C4A H4A1 111.3 . . ? C3A C4A H4A1 111.3 . . ? C5A C4A H4A2 111.3 . . ? C3A C4A H4A2 111.3 . . ? H4A1 C4A H4A2 109.2 . . ? C4A C5A C6A 104.0(13) . . ? C4A C5A H5AA 111.0 . . ? C6A C5A H5AA 111.0 . . ? C4A C5A H5AB 111.0 . . ? C6A C5A H5AB 111.0 . . ? H5AA C5A H5AB 109.0 . . ? C5A C6A H6AA 109.5 . . ? C5A C6A H6AB 109.5 . . ? H6AA C6A H6AB 109.5 . . ? C5A C6A H6AC 109.5 . . ? H6AA C6A H6AC 109.5 . . ? H6AB C6A H6AC 109.5 . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C3S C2S C1S 114.3(4) . . ? C3S C2S H2SA 108.7 . . ? C1S C2S H2SA 108.7 . . ? C3S C2S H2SB 108.7 . . ? C1S C2S H2SB 108.7 . . ? H2SA C2S H2SB 107.6 . . ? C4S C3S C2S 114.3(5) . . ? C4S C3S H3SA 108.7 . . ? C2S C3S H3SA 108.7 . . ? C4S C3S H3SB 108.7 . . ? C2S C3S H3SB 108.7 . . ? H3SA C3S H3SB 107.6 . . ? C3S C4S C5S 113.4(5) . . ? C3S C4S H4SA 108.9 . . ? C5S C4S H4SA 108.9 . . ? C3S C4S H4SB 108.9 . . ? C5S C4S H4SB 108.9 . . ? H4SA C4S H4SB 107.7 . . ? C6S C5S C4S 108.9(4) . . ? C6S C5S H5SA 109.9 . . ? C4S C5S H5SA 109.9 . . ? C6S C5S H5SB 109.9 . . ? C4S C5S H5SB 109.9 . . ? H5SA C5S H5SB 108.3 . . ? C5S C6S H6SA 109.5 . . ? C5S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? C5S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? C12 N1 C1 118.44(15) . . ? C11 N2 C10 118.58(15) . . ? C28 Si1 C32 106.85(9) . . ? C28 Si1 C35 106.14(9) . . ? C32 Si1 C35 115.17(9) . . ? C28 Si1 C29 106.52(9) . . ? C32 Si1 C29 110.80(9) . . ? C35 Si1 C29 110.81(10) . . ? C39 Si2 C46 106.45(9) . . ? C39 Si2 C43 106.10(10) . . ? C46 Si2 C43 110.55(11) . . ? C39 Si2 C40 106.87(11) . . ? C46 Si2 C40 111.67(13) . . ? C43 Si2 C40 114.63(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 172.10(16) . . . . ? C10 C1 C2 C3 -3.2(3) . . . . ? N1 C1 C2 C27 -5.5(3) . . . . ? C10 C1 C2 C27 179.15(16) . . . . ? C1 C2 C3 C4 -178.83(18) . . . . ? C27 C2 C3 C4 -1.2(3) . . . . ? C1 C2 C3 C8 0.4(3) . . . . ? C27 C2 C3 C8 177.95(17) . . . . ? C2 C3 C4 C5 179.20(19) . . . . ? C8 C3 C4 C5 0.0(3) . . . . ? C3 C4 C5 C6 -0.1(3) . . . . ? C4 C5 C6 C7 0.1(4) . . . . ? C5 C6 C7 C8 0.0(3) . . . . ? C6 C7 C8 C9 179.2(2) . . . . ? C6 C7 C8 C3 -0.1(3) . . . . ? C2 C3 C8 C9 1.6(3) . . . . ? C4 C3 C8 C9 -179.17(18) . . . . ? C2 C3 C8 C7 -179.09(17) . . . . ? C4 C3 C8 C7 0.1(3) . . . . ? C7 C8 C9 C10 -179.96(18) . . . . ? C3 C8 C9 C10 -0.7(3) . . . . ? C7 C8 C9 C38 0.7(3) . . . . ? C3 C8 C9 C38 179.92(18) . . . . ? C8 C9 C10 N2 176.92(17) . . . . ? C38 C9 C10 N2 -3.7(3) . . . . ? C8 C9 C10 C1 -2.2(3) . . . . ? C38 C9 C10 C1 177.20(17) . . . . ? N1 C1 C10 N2 9.8(3) . . . . ? C2 C1 C10 N2 -174.90(17) . . . . ? N1 C1 C10 C9 -171.10(16) . . . . ? C2 C1 C10 C9 4.2(3) . . . . ? N2 C11 C12 N1 11.1(3) . . . . ? C20 C11 C12 N1 -167.23(18) . . . . ? N2 C11 C12 C13 -166.63(18) . . . . ? C20 C11 C12 C13 15.1(3) . . . . ? N1 C12 C13 C18 -140.83(19) . . . . ? C11 C12 C13 C18 37.0(3) . . . . ? N1 C12 C13 C14 34.6(3) . . . . ? C11 C12 C13 C14 -147.61(19) . . . . ? C18 C13 C14 C15 -1.5(3) . . . . ? C12 C13 C14 C15 -177.12(18) . . . . ? C13 C14 C15 C16 1.0(3) . . . . ? C14 C15 C16 C17 0.8(3) . . . . ? C14 C15 C16 C19 -179.2(2) . . . . ? C15 C16 C17 C18 -2.1(3) . . . . ? C19 C16 C17 C18 177.8(2) . . . . ? C16 C17 C18 C13 1.6(3) . . . . ? C14 C13 C18 C17 0.2(3) . . . . ? C12 C13 C18 C17 175.64(18) . . . . ? N2 C11 C20 C25 -140.3(2) . . . . ? C12 C11 C20 C25 38.0(3) . . . . ? N2 C11 C20 C21 35.1(3) . . . . ? C12 C11 C20 C21 -146.5(2) . . . . ? C25 C20 C21 C22 -1.5(3) . . . . ? C11 C20 C21 C22 -177.21(19) . . . . ? C20 C21 C22 C23 1.0(4) . . . . ? C21 C22 C23 C24 0.9(3) . . . . ? C21 C22 C23 C26 -178.8(2) . . . . ? C22 C23 C24 C25 -2.2(3) . . . . ? C26 C23 C24 C25 177.6(2) . . . . ? C21 C20 C25 C24 0.3(3) . . . . ? C11 C20 C25 C24 175.74(19) . . . . ? C23 C24 C25 C20 1.6(3) . . . . ? C1 C2 C27 C28 177(100) . . . . ? C3 C2 C27 C28 0(5) . . . . ? C2 C27 C28 Si1 -99(12) . . . . ? C10 C9 C38 C39 -146(9) . . . . ? C8 C9 C38 C39 34(9) . . . . ? C9 C38 C39 Si2 -168(6) . . . . ? C1A C2A C3A C4A 179.5(13) . . . . ? C2A C3A C4A C5A 174.0(13) . . . . ? C3A C4A C5A C6A -172.3(12) . . . . ? C1S C2S C3S C4S 176.4(4) . . . . ? C2S C3S C4S C5S -176.0(4) . . . . ? C3S C4S C5S C6S 179.1(5) . . . . ? C11 C12 N1 C1 -6.3(3) . . . . ? C13 C12 N1 C1 171.63(15) . . . . ? C2 C1 N1 C12 -179.02(17) . . . . ? C10 C1 N1 C12 -3.7(3) . . . . ? C12 C11 N2 C10 -4.8(3) . . . . ? C20 C11 N2 C10 173.61(16) . . . . ? C9 C10 N2 C11 175.75(17) . . . . ? C1 C10 N2 C11 -5.1(3) . . . . ? C27 C28 Si1 C32 37(12) . . . . ? C27 C28 Si1 C35 160(12) . . . . ? C27 C28 Si1 C29 -82(12) . . . . ? C33 C32 Si1 C28 -175.94(16) . . . . ? C34 C32 Si1 C28 55.96(17) . . . . ? C33 C32 Si1 C35 66.46(18) . . . . ? C34 C32 Si1 C35 -61.64(18) . . . . ? C33 C32 Si1 C29 -60.29(18) . . . . ? C34 C32 Si1 C29 171.60(15) . . . . ? C37 C35 Si1 C28 -57.0(2) . . . . ? C36 C35 Si1 C28 173.86(18) . . . . ? C37 C35 Si1 C32 61.0(2) . . . . ? C36 C35 Si1 C32 -68.1(2) . . . . ? C37 C35 Si1 C29 -172.21(18) . . . . ? C36 C35 Si1 C29 58.6(2) . . . . ? C30 C29 Si1 C28 61.23(17) . . . . ? C31 C29 Si1 C28 -62.12(17) . . . . ? C30 C29 Si1 C32 -54.63(17) . . . . ? C31 C29 Si1 C32 -177.98(15) . . . . ? C30 C29 Si1 C35 176.25(14) . . . . ? C31 C29 Si1 C35 52.89(17) . . . . ? C38 C39 Si2 C46 127(6) . . . . ? C38 C39 Si2 C43 9(6) . . . . ? C38 C39 Si2 C40 -114(6) . . . . ? C48 C46 Si2 C39 -63.59(19) . . . . ? C47 C46 Si2 C39 60.7(2) . . . . ? C48 C46 Si2 C43 51.22(19) . . . . ? C47 C46 Si2 C43 175.51(17) . . . . ? C48 C46 Si2 C40 -179.87(16) . . . . ? C47 C46 Si2 C40 -55.6(2) . . . . ? C44 C43 Si2 C39 -60.1(2) . . . . ? C45 C43 Si2 C39 171.17(18) . . . . ? C44 C43 Si2 C46 -175.11(19) . . . . ? C45 C43 Si2 C46 56.1(2) . . . . ? C44 C43 Si2 C40 57.6(2) . . . . ? C45 C43 Si2 C40 -71.1(2) . . . . ? C41 C40 Si2 C39 40.3(4) . . . . ? C42 C40 Si2 C39 177.6(2) . . . . ? C41 C40 Si2 C46 156.4(4) . . . . ? C42 C40 Si2 C46 -66.3(3) . . . . ? C41 C40 Si2 C43 -76.9(4) . . . . ? C42 C40 Si2 C43 60.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.689 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.060 _database_code_depnum_ccdc_archive 'CCDC 936731' ####################################################################### # # 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_nb_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4a in manuscript' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H52 N2 Si2' _chemical_formula_weight 568.98 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' _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 14.5474(8) _cell_length_b 14.9254(9) _cell_length_c 16.2869(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.065(4) _cell_angle_gamma 90.00 _cell_volume 3509.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1960 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 62.02 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.077 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9656 _exptl_absorpt_correction_T_max 0.9912 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18087 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 24.55 _reflns_number_total 5539 _reflns_number_gt 4101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5539 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1667 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.007 _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 0.7167(2) 1.01444(19) 0.04875(18) 0.0397(7) Uani 1 1 d . . . C2 C 0.7966(2) 0.96316(19) 0.03302(17) 0.0367(7) Uani 1 1 d . . . C3 C 0.80037(19) 0.89817(17) 0.16134(16) 0.0293(6) Uani 1 1 d . . . C4 C 0.84295(19) 0.83870(17) 0.22154(16) 0.0302(6) Uani 1 1 d . . . C5 C 0.81119(19) 0.83485(17) 0.30038(17) 0.0313(6) Uani 1 1 d . . . C6 C 0.8531(2) 0.77751(19) 0.36386(18) 0.0383(7) Uani 1 1 d . . . H6A H 0.9023 0.7392 0.3528 0.046 Uiso 1 1 calc R . . C7 C 0.8242(2) 0.7764(2) 0.44027(19) 0.0454(8) Uani 1 1 d . . . H7A H 0.8540 0.7385 0.4823 0.055 Uiso 1 1 calc R . . C8 C 0.7498(2) 0.8316(2) 0.45693(19) 0.0464(8) Uani 1 1 d . . . H8A H 0.7296 0.8301 0.5102 0.056 Uiso 1 1 calc R . . C9 C 0.7069(2) 0.8865(2) 0.39824(18) 0.0407(7) Uani 1 1 d . . . H9A H 0.6569 0.9229 0.4108 0.049 Uiso 1 1 calc R . . C10 C 0.73560(19) 0.89054(17) 0.31768(17) 0.0323(6) Uani 1 1 d . . . C11 C 0.69220(19) 0.94808(18) 0.25617(17) 0.0322(6) Uani 1 1 d . . . C12 C 0.72457(19) 0.95148(17) 0.17790(17) 0.0308(6) Uani 1 1 d . . . C13 C 0.6164(2) 1.00351(19) 0.27214(18) 0.0382(7) Uani 1 1 d . . . C14 C 0.5523(2) 1.0499(2) 0.28779(19) 0.0440(8) Uani 1 1 d . . . C15 C 0.4337(2) 1.1921(2) 0.2033(2) 0.0517(9) Uani 1 1 d . . . H15A H 0.3792 1.2319 0.2078 0.062 Uiso 1 1 calc R . . C16 C 0.4106(3) 1.1324(3) 0.1269(2) 0.0806(13) Uani 1 1 d . . . H16A H 0.3999 1.1700 0.0773 0.121 Uiso 1 1 calc R . . H16B H 0.3547 1.0975 0.1327 0.121 Uiso 1 1 calc R . . H16C H 0.4624 1.0916 0.1220 0.121 Uiso 1 1 calc R . . C17 C 0.5163(3) 1.2517(3) 0.1917(3) 0.0909(15) Uani 1 1 d . . . H17A H 0.5025 1.2867 0.1408 0.136 Uiso 1 1 calc R . . H17B H 0.5709 1.2142 0.1878 0.136 Uiso 1 1 calc R . . H17C H 0.5286 1.2923 0.2391 0.136 Uiso 1 1 calc R . . C18 C 0.4821(5) 1.1928(4) 0.3934(3) 0.138(3) Uani 1 1 d . . . H18 H 0.4446 1.1576 0.4297 0.166 Uiso 1 1 calc R . . C19 C 0.5624(4) 1.1874(4) 0.4434(4) 0.120(2) Uani 1 1 d . . . H19A H 0.5605 1.2277 0.4907 0.181 Uiso 1 1 calc R . . H19B H 0.6135 1.2049 0.4128 0.181 Uiso 1 1 calc R . . H19C H 0.5719 1.1257 0.4633 0.181 Uiso 1 1 calc R . . C20 C 0.4255(4) 1.2786(3) 0.3935(3) 0.0901(16) Uani 1 1 d . . . H20A H 0.4419 1.3104 0.4459 0.135 Uiso 1 1 calc R . . H20B H 0.3594 1.2638 0.3870 0.135 Uiso 1 1 calc R . . H20C H 0.4389 1.3170 0.3475 0.135 Uiso 1 1 calc R . . C21 C 0.3518(3) 1.0430(4) 0.3044(3) 0.0912(16) Uani 1 1 d . . . H21A H 0.3500 1.0057 0.2532 0.109 Uiso 1 1 calc R . . C22 C 0.3612(4) 0.9779(3) 0.3726(3) 0.0990(16) Uani 1 1 d . . . H22A H 0.3060 0.9397 0.3685 0.148 Uiso 1 1 calc R . . H22B H 0.3677 1.0099 0.4256 0.148 Uiso 1 1 calc R . . H22C H 0.4161 0.9406 0.3693 0.148 Uiso 1 1 calc R . . C23 C 0.2584(3) 1.0924(4) 0.2953(3) 0.0978(17) Uani 1 1 d . . . H23A H 0.2081 1.0489 0.2972 0.147 Uiso 1 1 calc R . . H23B H 0.2497 1.1243 0.2423 0.147 Uiso 1 1 calc R . . H23C H 0.2576 1.1354 0.3407 0.147 Uiso 1 1 calc R . . C24 C 0.9197(2) 0.78567(17) 0.20404(16) 0.0318(6) Uani 1 1 d . . . C25 C 0.9846(2) 0.73949(19) 0.19117(17) 0.0365(7) Uani 1 1 d . . . C26 C 1.0820(2) 0.6665(2) 0.05425(18) 0.0445(8) Uani 1 1 d . . . H26A H 1.0261 0.6317 0.0308 0.053 Uiso 1 1 calc R . . C27 C 1.1656(3) 0.6163(3) 0.0285(2) 0.0676(11) Uani 1 1 d . . . H27A H 1.1631 0.6176 -0.0319 0.101 Uiso 1 1 calc R . . H27B H 1.1644 0.5540 0.0473 0.101 Uiso 1 1 calc R . . H27C H 1.2228 0.6451 0.0535 0.101 Uiso 1 1 calc R . . C28 C 1.0719(3) 0.7598(3) 0.0139(2) 0.0571(9) Uani 1 1 d . . . H28A H 1.0726 0.7541 -0.0460 0.086 Uiso 1 1 calc R . . H28B H 1.1235 0.7980 0.0371 0.086 Uiso 1 1 calc R . . H28C H 1.0132 0.7868 0.0248 0.086 Uiso 1 1 calc R . . C29 C 1.1920(2) 0.7125(2) 0.22690(18) 0.0428(8) Uani 1 1 d . . . H29A H 1.2429 0.6710 0.2155 0.051 Uiso 1 1 calc R . . C30 C 1.1925(3) 0.7153(3) 0.3201(2) 0.0648(11) Uani 1 1 d . . . H30A H 1.2519 0.7393 0.3458 0.097 Uiso 1 1 calc R . . H30B H 1.1840 0.6546 0.3408 0.097 Uiso 1 1 calc R . . H30C H 1.1421 0.7539 0.3338 0.097 Uiso 1 1 calc R . . C31 C 1.2169(3) 0.8048(3) 0.1969(2) 0.0761(13) Uani 1 1 d . . . H31A H 1.2751 0.8248 0.2283 0.114 Uiso 1 1 calc R . . H31B H 1.1675 0.8473 0.2053 0.114 Uiso 1 1 calc R . . H31C H 1.2242 0.8020 0.1380 0.114 Uiso 1 1 calc R . . C32 C 1.0557(2) 0.5502(2) 0.20772(19) 0.0429(8) Uani 1 1 d . . . H32A H 1.1165 0.5186 0.2194 0.051 Uiso 1 1 calc R . . C33 C 1.0117(3) 0.5505(2) 0.2887(2) 0.0549(9) Uani 1 1 d . . . H33A H 1.0006 0.4887 0.3052 0.082 Uiso 1 1 calc R . . H33B H 0.9528 0.5831 0.2805 0.082 Uiso 1 1 calc R . . H33C H 1.0537 0.5799 0.3322 0.082 Uiso 1 1 calc R . . C34 C 0.9957(3) 0.4941(2) 0.1433(2) 0.0619(10) Uani 1 1 d . . . H34A H 0.9854 0.4348 0.1664 0.093 Uiso 1 1 calc R . . H34B H 1.0273 0.4874 0.0939 0.093 Uiso 1 1 calc R . . H34C H 0.9360 0.5240 0.1284 0.093 Uiso 1 1 calc R . . C35 C 0.6710(3) 1.0796(2) -0.0137(2) 0.0597(10) Uani 1 1 d . . . H35A H 0.6181 1.1076 0.0080 0.090 Uiso 1 1 calc R . . H35B H 0.6496 1.0479 -0.0651 0.090 Uiso 1 1 calc R . . H35C H 0.7157 1.1260 -0.0246 0.090 Uiso 1 1 calc R . . C36 C 0.8397(3) 0.9749(2) -0.04542(19) 0.0503(9) Uani 1 1 d . . . H36A H 0.8930 0.9347 -0.0449 0.075 Uiso 1 1 calc R . . H36B H 0.8602 1.0371 -0.0497 0.075 Uiso 1 1 calc R . . H36C H 0.7940 0.9606 -0.0930 0.075 Uiso 1 1 calc R . . N1 N 0.68187(17) 1.00871(15) 0.11890(15) 0.0378(6) Uani 1 1 d . . . N2 N 0.83568(16) 0.90527(15) 0.08665(14) 0.0332(6) Uani 1 1 d . . . Si1 Si 0.45354(6) 1.12275(6) 0.29964(5) 0.0449(3) Uani 1 1 d . . . Si2 Si 1.08117(5) 0.66641(5) 0.16994(5) 0.0326(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0434(19) 0.0334(15) 0.0411(17) 0.0026(13) 0.0007(14) 0.0025(14) C2 0.0422(18) 0.0316(15) 0.0363(16) -0.0021(13) 0.0044(13) -0.0004(14) C3 0.0296(15) 0.0239(13) 0.0351(15) -0.0038(11) 0.0065(12) -0.0019(12) C4 0.0315(16) 0.0234(13) 0.0362(15) -0.0035(11) 0.0059(12) -0.0007(12) C5 0.0343(16) 0.0242(13) 0.0358(15) -0.0021(11) 0.0059(12) -0.0020(12) C6 0.0418(18) 0.0306(15) 0.0433(17) 0.0027(13) 0.0087(14) 0.0041(13) C7 0.053(2) 0.0423(18) 0.0414(18) 0.0084(14) 0.0087(15) 0.0020(16) C8 0.056(2) 0.0458(18) 0.0407(18) 0.0024(15) 0.0197(15) 0.0014(16) C9 0.0395(18) 0.0378(16) 0.0476(18) -0.0049(14) 0.0166(14) 0.0002(14) C10 0.0313(16) 0.0258(14) 0.0410(16) -0.0039(12) 0.0093(13) -0.0030(12) C11 0.0288(16) 0.0256(13) 0.0430(16) -0.0059(12) 0.0073(13) -0.0003(12) C12 0.0294(15) 0.0243(13) 0.0381(15) -0.0025(12) 0.0014(12) -0.0012(12) C13 0.0377(18) 0.0316(15) 0.0460(17) -0.0032(13) 0.0073(14) 0.0014(14) C14 0.0431(19) 0.0427(18) 0.0468(18) -0.0029(14) 0.0085(15) 0.0069(16) C15 0.049(2) 0.058(2) 0.0486(19) 0.0084(16) 0.0107(15) 0.0139(17) C16 0.084(3) 0.110(4) 0.047(2) -0.006(2) 0.003(2) 0.016(3) C17 0.091(3) 0.084(3) 0.105(4) 0.016(3) 0.041(3) -0.011(3) C18 0.179(6) 0.145(5) 0.072(3) -0.061(3) -0.056(3) 0.130(5) C19 0.091(4) 0.102(4) 0.151(5) -0.067(4) -0.052(4) 0.028(3) C20 0.120(4) 0.084(3) 0.066(3) -0.013(2) 0.012(3) 0.059(3) C21 0.052(3) 0.119(4) 0.109(4) 0.049(3) 0.035(2) 0.024(3) C22 0.088(4) 0.077(3) 0.136(4) 0.022(3) 0.030(3) 0.004(3) C23 0.050(3) 0.139(5) 0.109(4) 0.040(3) 0.027(3) 0.023(3) C24 0.0376(17) 0.0242(14) 0.0345(15) 0.0010(11) 0.0075(12) 0.0019(13) C25 0.0422(18) 0.0308(15) 0.0375(16) 0.0032(12) 0.0082(13) 0.0029(14) C26 0.0383(18) 0.054(2) 0.0412(17) -0.0060(15) 0.0055(14) 0.0044(15) C27 0.061(2) 0.092(3) 0.053(2) -0.016(2) 0.0202(18) 0.017(2) C28 0.054(2) 0.075(2) 0.0413(18) 0.0137(17) 0.0032(16) -0.0014(19) C29 0.0394(18) 0.0487(18) 0.0403(17) -0.0052(14) 0.0049(14) 0.0061(15) C30 0.074(3) 0.070(2) 0.048(2) 0.0026(18) -0.0023(18) -0.010(2) C31 0.080(3) 0.081(3) 0.063(2) 0.013(2) -0.007(2) -0.036(2) C32 0.0406(18) 0.0329(16) 0.0551(19) 0.0040(14) 0.0056(15) 0.0108(14) C33 0.058(2) 0.0465(19) 0.062(2) 0.0162(17) 0.0157(18) 0.0090(17) C34 0.063(2) 0.0442(19) 0.078(3) -0.0031(18) 0.006(2) -0.0006(18) C35 0.070(3) 0.055(2) 0.053(2) 0.0152(17) 0.0046(18) 0.0197(19) C36 0.064(2) 0.0475(19) 0.0410(18) 0.0052(15) 0.0132(16) 0.0057(17) N1 0.0377(15) 0.0288(12) 0.0464(15) 0.0020(11) 0.0034(12) 0.0048(11) N2 0.0368(14) 0.0278(12) 0.0353(13) -0.0017(10) 0.0062(11) -0.0019(11) Si1 0.0415(6) 0.0545(6) 0.0398(5) 0.0025(4) 0.0094(4) 0.0236(4) Si2 0.0319(5) 0.0322(4) 0.0344(4) 0.0004(3) 0.0067(3) 0.0085(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.308(4) . ? C1 C2 1.441(4) . ? C1 C35 1.502(4) . ? C2 N2 1.308(4) . ? C2 C36 1.501(4) . ? C3 N2 1.382(4) . ? C3 C4 1.408(4) . ? C3 C12 1.412(4) . ? C4 C5 1.418(4) . ? C4 C24 1.426(4) . ? C5 C6 1.421(4) . ? C5 C10 1.434(4) . ? C6 C7 1.362(4) . ? C6 H6A 0.9500 . ? C7 C8 1.413(4) . ? C7 H7A 0.9500 . ? C8 C9 1.353(4) . ? C8 H8A 0.9500 . ? C9 C10 1.426(4) . ? C9 H9A 0.9500 . ? C10 C11 1.409(4) . ? C11 C12 1.413(4) . ? C11 C13 1.428(4) . ? C12 N1 1.375(4) . ? C13 C14 1.213(4) . ? C14 Si1 1.831(3) . ? C15 C17 1.524(6) . ? C15 C16 1.533(5) . ? C15 Si1 1.873(3) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.342(6) . ? C18 C20 1.523(6) . ? C18 Si1 1.855(4) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.470(6) . ? C21 C23 1.538(6) . ? C21 Si1 1.908(5) . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.208(4) . ? C25 Si2 1.844(3) . ? C26 C27 1.531(5) . ? C26 C28 1.539(5) . ? C26 Si2 1.886(3) . ? C26 H26A 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.517(5) . ? C29 C31 1.521(5) . ? C29 Si2 1.888(3) . ? C29 H29A 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C34 1.529(5) . ? C32 C33 1.535(5) . ? C32 Si2 1.893(3) . ? C32 H32A 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 C1 C2 121.9(3) . . ? N1 C1 C35 116.6(3) . . ? C2 C1 C35 121.5(3) . . ? N2 C2 C1 121.7(3) . . ? N2 C2 C36 116.9(3) . . ? C1 C2 C36 121.3(3) . . ? N2 C3 C4 118.8(2) . . ? N2 C3 C12 120.6(2) . . ? C4 C3 C12 120.6(2) . . ? C3 C4 C5 119.4(3) . . ? C3 C4 C24 119.9(2) . . ? C5 C4 C24 120.6(2) . . ? C4 C5 C6 121.6(3) . . ? C4 C5 C10 119.8(2) . . ? C6 C5 C10 118.5(3) . . ? C7 C6 C5 121.3(3) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C6 C7 C8 119.9(3) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C9 C8 C7 121.1(3) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C8 C9 C10 120.9(3) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 121.6(3) . . ? C11 C10 C5 120.1(2) . . ? C9 C10 C5 118.4(3) . . ? C10 C11 C12 119.6(3) . . ? C10 C11 C13 120.8(3) . . ? C12 C11 C13 119.6(3) . . ? N1 C12 C3 120.8(3) . . ? N1 C12 C11 118.7(3) . . ? C3 C12 C11 120.4(2) . . ? C14 C13 C11 178.3(3) . . ? C13 C14 Si1 173.9(3) . . ? C17 C15 C16 109.7(3) . . ? C17 C15 Si1 112.5(3) . . ? C16 C15 Si1 110.7(3) . . ? C17 C15 H15A 107.9 . . ? C16 C15 H15A 107.9 . . ? Si1 C15 H15A 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 118.7(5) . . ? C19 C18 Si1 123.8(4) . . ? C20 C18 Si1 114.1(3) . . ? C19 C18 H18 96.2 . . ? C20 C18 H18 96.2 . . ? Si1 C18 H18 96.2 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 112.9(4) . . ? C22 C21 Si1 116.3(4) . . ? C23 C21 Si1 112.2(4) . . ? C22 C21 H21A 104.7 . . ? C23 C21 H21A 104.7 . . ? Si1 C21 H21A 104.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C4 178.2(3) . . ? C24 C25 Si2 178.2(3) . . ? C27 C26 C28 111.3(3) . . ? C27 C26 Si2 112.1(2) . . ? C28 C26 Si2 114.6(2) . . ? C27 C26 H26A 106.1 . . ? C28 C26 H26A 106.1 . . ? Si2 C26 H26A 106.1 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C31 108.8(3) . . ? C30 C29 Si2 113.6(2) . . ? C31 C29 Si2 113.3(2) . . ? C30 C29 H29A 106.9 . . ? C31 C29 H29A 106.9 . . ? Si2 C29 H29A 106.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C33 109.2(3) . . ? C34 C32 Si2 113.4(2) . . ? C33 C32 Si2 113.3(2) . . ? C34 C32 H32A 106.8 . . ? C33 C32 H32A 106.8 . . ? Si2 C32 H32A 106.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C1 C35 H35A 109.5 . . ? C1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C2 C36 H36A 109.5 . . ? C2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C1 N1 C12 117.4(3) . . ? C2 N2 C3 117.4(2) . . ? C14 Si1 C18 108.79(18) . . ? C14 Si1 C15 106.38(15) . . ? C18 Si1 C15 112.0(2) . . ? C14 Si1 C21 104.83(18) . . ? C18 Si1 C21 114.5(3) . . ? C15 Si1 C21 109.80(18) . . ? C25 Si2 C26 106.56(13) . . ? C25 Si2 C29 108.45(14) . . ? C26 Si2 C29 112.39(14) . . ? C25 Si2 C32 107.27(14) . . ? C26 Si2 C32 110.57(14) . . ? C29 Si2 C32 111.32(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 3.2(4) . . . . ? C35 C1 C2 N2 -178.9(3) . . . . ? N1 C1 C2 C36 -175.8(3) . . . . ? C35 C1 C2 C36 2.0(4) . . . . ? N2 C3 C4 C5 176.0(2) . . . . ? C12 C3 C4 C5 -2.2(4) . . . . ? N2 C3 C4 C24 -1.5(4) . . . . ? C12 C3 C4 C24 -179.7(2) . . . . ? C3 C4 C5 C6 -178.5(2) . . . . ? C24 C4 C5 C6 -1.1(4) . . . . ? C3 C4 C5 C10 0.7(4) . . . . ? C24 C4 C5 C10 178.2(2) . . . . ? C4 C5 C6 C7 177.8(3) . . . . ? C10 C5 C6 C7 -1.5(4) . . . . ? C5 C6 C7 C8 1.4(5) . . . . ? C6 C7 C8 C9 -0.5(5) . . . . ? C7 C8 C9 C10 -0.2(5) . . . . ? C8 C9 C10 C11 -179.3(3) . . . . ? C8 C9 C10 C5 0.0(4) . . . . ? C4 C5 C10 C11 0.8(4) . . . . ? C6 C5 C10 C11 -179.9(3) . . . . ? C4 C5 C10 C9 -178.5(3) . . . . ? C6 C5 C10 C9 0.8(4) . . . . ? C9 C10 C11 C12 178.4(3) . . . . ? C5 C10 C11 C12 -1.0(4) . . . . ? C9 C10 C11 C13 -1.1(4) . . . . ? C5 C10 C11 C13 179.5(2) . . . . ? N2 C3 C12 N1 2.8(4) . . . . ? C4 C3 C12 N1 -179.0(2) . . . . ? N2 C3 C12 C11 -176.1(3) . . . . ? C4 C3 C12 C11 2.1(4) . . . . ? C10 C11 C12 N1 -179.4(2) . . . . ? C13 C11 C12 N1 0.1(4) . . . . ? C10 C11 C12 C3 -0.5(4) . . . . ? C13 C11 C12 C3 179.0(2) . . . . ? C10 C11 C13 C14 6(11) . . . . ? C12 C11 C13 C14 -174(100) . . . . ? C11 C13 C14 Si1 -176(100) . . . . ? C3 C4 C24 C25 -172(10) . . . . ? C5 C4 C24 C25 10(10) . . . . ? C4 C24 C25 Si2 88(14) . . . . ? C2 C1 N1 C12 0.0(4) . . . . ? C35 C1 N1 C12 -177.9(3) . . . . ? C3 C12 N1 C1 -2.9(4) . . . . ? C11 C12 N1 C1 176.1(3) . . . . ? C1 C2 N2 C3 -3.3(4) . . . . ? C36 C2 N2 C3 175.8(3) . . . . ? C4 C3 N2 C2 -177.8(2) . . . . ? C12 C3 N2 C2 0.4(4) . . . . ? C13 C14 Si1 C18 -137(3) . . . . ? C13 C14 Si1 C15 -16(3) . . . . ? C13 C14 Si1 C21 100(3) . . . . ? C19 C18 Si1 C14 -1.1(8) . . . . ? C20 C18 Si1 C14 157.7(5) . . . . ? C19 C18 Si1 C15 -118.4(7) . . . . ? C20 C18 Si1 C15 40.4(6) . . . . ? C19 C18 Si1 C21 115.8(7) . . . . ? C20 C18 Si1 C21 -85.5(6) . . . . ? C17 C15 Si1 C14 -62.0(3) . . . . ? C16 C15 Si1 C14 61.1(3) . . . . ? C17 C15 Si1 C18 56.7(4) . . . . ? C16 C15 Si1 C18 179.8(3) . . . . ? C17 C15 Si1 C21 -175.0(3) . . . . ? C16 C15 Si1 C21 -51.8(3) . . . . ? C22 C21 Si1 C14 60.5(4) . . . . ? C23 C21 Si1 C14 -167.5(3) . . . . ? C22 C21 Si1 C18 -58.7(5) . . . . ? C23 C21 Si1 C18 73.3(4) . . . . ? C22 C21 Si1 C15 174.4(4) . . . . ? C23 C21 Si1 C15 -53.6(4) . . . . ? C24 C25 Si2 C26 68(8) . . . . ? C24 C25 Si2 C29 -171(8) . . . . ? C24 C25 Si2 C32 -50(8) . . . . ? C27 C26 Si2 C25 173.8(3) . . . . ? C28 C26 Si2 C25 45.8(3) . . . . ? C27 C26 Si2 C29 55.2(3) . . . . ? C28 C26 Si2 C29 -72.9(3) . . . . ? C27 C26 Si2 C32 -69.9(3) . . . . ? C28 C26 Si2 C32 162.0(2) . . . . ? C30 C29 Si2 C25 61.0(3) . . . . ? C31 C29 Si2 C25 -63.9(3) . . . . ? C30 C29 Si2 C26 178.6(2) . . . . ? C31 C29 Si2 C26 53.7(3) . . . . ? C30 C29 Si2 C32 -56.7(3) . . . . ? C31 C29 Si2 C32 178.4(3) . . . . ? C34 C32 Si2 C25 86.8(3) . . . . ? C33 C32 Si2 C25 -38.4(3) . . . . ? C34 C32 Si2 C26 -29.0(3) . . . . ? C33 C32 Si2 C26 -154.2(2) . . . . ? C34 C32 Si2 C29 -154.7(2) . . . . ? C33 C32 Si2 C29 80.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 24.55 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.762 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.054 #================================================================== _database_code_depnum_ccdc_archive 'CCDC 936732'