# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_f101025b _database_code_depnum_ccdc_archive 'CCDC 875347' #TrackingRef 'web_deposit_cif_file_0_WeifengChen_1351068190.f101025b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H50 F3 N Si5' _chemical_formula_weight 622.16 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' F F 0.0171 0.0103 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6872(8) _cell_length_b 23.8106(16) _cell_length_c 14.0462(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.988(2) _cell_angle_gamma 90.00 _cell_volume 3598.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.27 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.233 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26379 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6332 _reflns_number_gt 5128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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. Due to the disorder of the CF3 group, PART instructions have been applied. A number of DELU, SIMU, ISOR instructions have been used in order to refine respective atomsrefine respective atoms anisotropically. They were used as following: DFIX 1.30 0.01 C21 F2' C21 F1' C21 F3' DELU C21 F1 F2 F3 F1' F2' F3' SIMU C21 F1 F2 F3 F1' F2' F3' ISOR 0.01 F2' ISOR 0.01 F3' ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5000P] 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 6332 _refine_ls_number_parameters 392 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si -0.07028(5) 0.12596(2) 0.20865(4) 0.03463(16) Uani 1 1 d . . . Si2 Si 0.17133(7) 0.17669(3) 0.14746(6) 0.0640(2) Uani 1 1 d . . . Si3 Si -0.18264(6) 0.23996(3) 0.25385(6) 0.0589(2) Uani 1 1 d . . . Si4 Si -0.18819(6) 0.13212(3) 0.38175(5) 0.05053(19) Uani 1 1 d . . . Si5 Si -0.21880(6) 0.10447(3) 0.03901(5) 0.0520(2) Uani 1 1 d . . . N1 N 0.01556(14) 0.06486(6) 0.26498(12) 0.0352(4) Uani 1 1 d . . . C1 C -0.10508(18) 0.16966(8) 0.30687(15) 0.0396(4) Uani 1 1 d . . . C2 C 0.03310(19) 0.18066(9) 0.38506(16) 0.0432(5) Uani 1 1 d . . . H2A H 0.0347 0.2125 0.4286 0.052 Uiso 1 1 calc R . . H2B H 0.0633 0.1481 0.4293 0.052 Uiso 1 1 calc R . . C3 C 0.1189(2) 0.19235(9) 0.32861(17) 0.0465(5) Uani 1 1 d . . . H3A H 0.2046 0.1900 0.3775 0.056 Uiso 1 1 calc R . . H3B H 0.1044 0.2303 0.3012 0.056 Uiso 1 1 calc R . . C4 C 0.09835(19) 0.15056(8) 0.23900(16) 0.0400(5) Uani 1 1 d . . . C5 C -0.0961(3) 0.07331(11) 0.4624(2) 0.0610(6) Uani 1 1 d . . . H5A H -0.0174 0.0872 0.5099 0.091 Uiso 1 1 calc R . . H5B H -0.0828 0.0453 0.4186 0.091 Uiso 1 1 calc R . . H5C H -0.1406 0.0570 0.5003 0.091 Uiso 1 1 calc R . . C6 C -0.3433(2) 0.10227(14) 0.2989(3) 0.0764(8) Uani 1 1 d . . . H6A H -0.3343 0.0777 0.2481 0.115 Uiso 1 1 calc R . . H6B H -0.3992 0.1322 0.2647 0.115 Uiso 1 1 calc R . . H6C H -0.3761 0.0816 0.3413 0.115 Uiso 1 1 calc R . . C7 C -0.2150(3) 0.17998(15) 0.4769(3) 0.0925(10) Uani 1 1 d . . . H7A H -0.2558 0.1596 0.5136 0.139 Uiso 1 1 calc R . . H7B H -0.2662 0.2109 0.4407 0.139 Uiso 1 1 calc R . . H7C H -0.1366 0.1939 0.5250 0.139 Uiso 1 1 calc R . . C8 C -0.3558(3) 0.23394(14) 0.1900(3) 0.0873(10) Uani 1 1 d . . . H8A H -0.3889 0.2257 0.2412 0.131 Uiso 1 1 calc R . . H8B H -0.3775 0.2043 0.1398 0.131 Uiso 1 1 calc R . . H8C H -0.3900 0.2687 0.1563 0.131 Uiso 1 1 calc R . . C9 C -0.1432(3) 0.29386(12) 0.3592(3) 0.0905(11) Uani 1 1 d . . . H9A H -0.1777 0.3295 0.3298 0.136 Uiso 1 1 calc R . . H9B H -0.0545 0.2971 0.3932 0.136 Uiso 1 1 calc R . . H9C H -0.1771 0.2826 0.4084 0.136 Uiso 1 1 calc R . . C10 C -0.1326(3) 0.27193(12) 0.1540(3) 0.0906(10) Uani 1 1 d . . . H10A H -0.1321 0.2436 0.1056 0.136 Uiso 1 1 calc R . . H10B H -0.0507 0.2874 0.1874 0.136 Uiso 1 1 calc R . . H10C H -0.1896 0.3012 0.1181 0.136 Uiso 1 1 calc R . . C11 C 0.0634(4) 0.2127(2) 0.0297(3) 0.1268(17) Uani 1 1 d . . . H11A H 0.0364 0.2474 0.0488 0.190 Uiso 1 1 calc R . . H11B H -0.0073 0.1891 -0.0049 0.190 Uiso 1 1 calc R . . H11C H 0.1052 0.2201 -0.0157 0.190 Uiso 1 1 calc R . . C12 C 0.3007(3) 0.22644(18) 0.2169(3) 0.1119(14) Uani 1 1 d . . . H12A H 0.3505 0.2319 0.1771 0.168 Uiso 1 1 calc R . . H12B H 0.3513 0.2112 0.2833 0.168 Uiso 1 1 calc R . . H12C H 0.2668 0.2618 0.2259 0.168 Uiso 1 1 calc R . . C13 C 0.2408(4) 0.11793(18) 0.0983(3) 0.1160(14) Uani 1 1 d . . . H13A H 0.1760 0.0931 0.0563 0.174 Uiso 1 1 calc R . . H13B H 0.2988 0.0975 0.1558 0.174 Uiso 1 1 calc R . . H13C H 0.2832 0.1332 0.0577 0.174 Uiso 1 1 calc R . . C14 C 0.13780(18) 0.08762(8) 0.27619(15) 0.0372(4) Uani 1 1 d . . . H14 H 0.1636 0.0691 0.2255 0.045 Uiso 1 1 calc R . . C15 C 0.24090(18) 0.08082(8) 0.38275(16) 0.0403(5) Uani 1 1 d . . . C16 C 0.3614(2) 0.09717(12) 0.3997(2) 0.0636(7) Uani 1 1 d . . . H16 H 0.3788 0.1115 0.3453 0.076 Uiso 1 1 calc R . . C17 C 0.4560(2) 0.09234(14) 0.4970(2) 0.0733(8) Uani 1 1 d . . . H17 H 0.5362 0.1036 0.5071 0.088 Uiso 1 1 calc R . . C18 C 0.4326(2) 0.07134(11) 0.5777(2) 0.0585(6) Uani 1 1 d . A . C19 C 0.3134(2) 0.05411(11) 0.56154(18) 0.0570(6) Uani 1 1 d . . . H19 H 0.2963 0.0394 0.6159 0.068 Uiso 1 1 calc R . . C20 C 0.2198(2) 0.05889(10) 0.46429(17) 0.0480(5) Uani 1 1 d . . . H20 H 0.1401 0.0468 0.4541 0.058 Uiso 1 1 calc R . . C21 C 0.5332(3) 0.06609(15) 0.6833(3) 0.0833(9) Uani 1 1 d DU . . C22 C -0.00915(18) 0.00723(8) 0.25514(14) 0.0373(4) Uani 1 1 d . . . C23 C 0.0821(2) -0.03245(9) 0.26409(17) 0.0473(5) Uani 1 1 d . . . H23 H 0.1634 -0.0209 0.2791 0.057 Uiso 1 1 calc R . . C24 C 0.0521(3) -0.08898(10) 0.2508(2) 0.0625(7) Uani 1 1 d . . . H24 H 0.1134 -0.1150 0.2555 0.075 Uiso 1 1 calc R . . C25 C -0.0660(3) -0.10712(11) 0.2307(2) 0.0718(8) Uani 1 1 d . . . H25 H -0.0851 -0.1452 0.2222 0.086 Uiso 1 1 calc R . . C26 C -0.1564(3) -0.06817(11) 0.2232(2) 0.0702(8) Uani 1 1 d . . . H26 H -0.2372 -0.0801 0.2090 0.084 Uiso 1 1 calc R . . C27 C -0.1284(2) -0.01178(9) 0.23659(18) 0.0503(5) Uani 1 1 d . . . H27 H -0.1900 0.0138 0.2332 0.060 Uiso 1 1 calc R . . C28 C -0.1366(3) 0.05382(14) -0.0126(2) 0.0880(10) Uani 1 1 d . . . H28A H -0.1255 0.0189 0.0242 0.132 Uiso 1 1 calc R . . H28B H -0.0569 0.0688 -0.0040 0.132 Uiso 1 1 calc R . . H28C H -0.1849 0.0475 -0.0848 0.132 Uiso 1 1 calc R . . C29 C -0.3659(3) 0.07111(17) 0.0335(2) 0.0939(11) Uani 1 1 d . . . H29A H -0.4162 0.0611 -0.0366 0.141 Uiso 1 1 calc R . . H29B H -0.4105 0.0971 0.0585 0.141 Uiso 1 1 calc R . . H29C H -0.3465 0.0380 0.0759 0.141 Uiso 1 1 calc R . . C30 C -0.2691(3) 0.16675(14) -0.0486(2) 0.0863(10) Uani 1 1 d . . . H30A H -0.1974 0.1853 -0.0511 0.129 Uiso 1 1 calc R . . H30B H -0.3138 0.1923 -0.0229 0.129 Uiso 1 1 calc R . . H30C H -0.3221 0.1546 -0.1168 0.129 Uiso 1 1 calc R . . F1 F 0.6193(10) 0.1076(6) 0.7011(8) 0.133(3) Uani 0.60(2) 1 d PU A 1 F2 F 0.5965(11) 0.0208(5) 0.6952(10) 0.149(4) Uani 0.60(2) 1 d PU A 1 F3 F 0.4912(8) 0.0696(8) 0.7576(5) 0.142(4) Uani 0.60(2) 1 d PU A 1 F1' F 0.558(2) 0.0143(4) 0.7153(13) 0.140(6) Uani 0.40(2) 1 d PDU A 2 F2' F 0.5076(16) 0.0917(7) 0.7535(10) 0.125(4) Uani 0.40(2) 1 d PDU A 2 F3' F 0.6380(10) 0.0877(8) 0.6908(15) 0.130(4) Uani 0.40(2) 1 d PDU 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 0.0375(3) 0.0319(3) 0.0325(3) 0.0006(2) 0.0114(2) -0.0017(2) Si2 0.0660(5) 0.0717(5) 0.0630(4) 0.0133(4) 0.0347(4) -0.0160(4) Si3 0.0563(4) 0.0382(3) 0.0682(5) -0.0025(3) 0.0089(3) 0.0106(3) Si4 0.0501(4) 0.0562(4) 0.0533(4) -0.0048(3) 0.0289(3) 0.0036(3) Si5 0.0567(4) 0.0533(4) 0.0345(3) -0.0009(3) 0.0051(3) -0.0017(3) N1 0.0361(8) 0.0309(8) 0.0389(9) -0.0008(7) 0.0150(7) -0.0025(6) C1 0.0383(10) 0.0370(10) 0.0417(11) -0.0039(8) 0.0137(9) 0.0025(8) C2 0.0440(11) 0.0395(11) 0.0403(11) -0.0075(9) 0.0102(9) 0.0017(9) C3 0.0456(12) 0.0364(11) 0.0512(12) -0.0043(9) 0.0120(10) -0.0063(9) C4 0.0437(11) 0.0358(10) 0.0428(11) 0.0031(9) 0.0192(9) -0.0062(8) C5 0.0728(16) 0.0655(15) 0.0559(14) 0.0100(12) 0.0373(13) 0.0014(13) C6 0.0543(16) 0.086(2) 0.095(2) -0.0012(17) 0.0355(15) -0.0069(14) C7 0.116(3) 0.096(2) 0.091(2) -0.0163(19) 0.067(2) 0.019(2) C8 0.0606(17) 0.076(2) 0.098(2) 0.0006(17) 0.0013(16) 0.0177(15) C9 0.089(2) 0.0505(16) 0.112(3) -0.0231(16) 0.0175(19) 0.0179(15) C10 0.107(3) 0.0532(16) 0.097(2) 0.0257(16) 0.023(2) 0.0054(16) C11 0.105(3) 0.178(4) 0.103(3) 0.078(3) 0.047(2) -0.010(3) C12 0.100(3) 0.130(3) 0.116(3) 0.006(2) 0.053(2) -0.060(2) C13 0.158(4) 0.130(3) 0.112(3) 0.006(2) 0.109(3) 0.001(3) C14 0.0379(10) 0.0370(10) 0.0391(10) -0.0007(8) 0.0176(9) -0.0036(8) C15 0.0347(10) 0.0403(11) 0.0444(11) -0.0050(9) 0.0139(9) 0.0017(8) C16 0.0413(13) 0.0887(19) 0.0630(16) 0.0006(14) 0.0228(12) -0.0056(12) C17 0.0330(12) 0.101(2) 0.0779(19) -0.0096(16) 0.0131(13) -0.0069(13) C18 0.0414(12) 0.0647(15) 0.0566(15) -0.0124(12) 0.0051(11) 0.0103(11) C19 0.0548(14) 0.0645(15) 0.0453(13) 0.0024(11) 0.0127(11) 0.0082(11) C20 0.0395(11) 0.0537(13) 0.0482(13) 0.0040(10) 0.0143(10) 0.0014(9) C21 0.0547(17) 0.093(2) 0.075(2) -0.0206(18) -0.0042(14) 0.0156(16) C22 0.0468(11) 0.0328(10) 0.0324(10) 0.0000(8) 0.0155(8) -0.0028(8) C23 0.0542(13) 0.0398(11) 0.0499(12) -0.0021(9) 0.0224(10) 0.0001(9) C24 0.0856(19) 0.0356(12) 0.0711(17) -0.0037(11) 0.0357(15) 0.0069(12) C25 0.097(2) 0.0370(13) 0.0827(19) -0.0079(12) 0.0364(17) -0.0148(13) C26 0.0742(18) 0.0480(14) 0.094(2) -0.0101(14) 0.0387(16) -0.0226(13) C27 0.0533(13) 0.0394(11) 0.0607(14) -0.0026(10) 0.0251(11) -0.0065(10) C28 0.118(3) 0.085(2) 0.0539(16) -0.0153(15) 0.0264(17) 0.0162(19) C29 0.074(2) 0.122(3) 0.0652(19) -0.0016(19) 0.0050(15) -0.0343(19) C30 0.099(2) 0.0749(19) 0.0559(17) 0.0118(14) -0.0010(16) 0.0023(17) F1 0.092(5) 0.166(7) 0.090(3) -0.035(4) -0.023(3) -0.034(4) F2 0.101(5) 0.163(6) 0.119(6) -0.020(5) -0.026(3) 0.082(5) F3 0.083(3) 0.278(13) 0.040(3) -0.010(4) -0.004(2) 0.022(5) F1' 0.174(13) 0.082(5) 0.079(6) 0.015(4) -0.042(7) 0.014(5) F2' 0.117(7) 0.144(7) 0.086(6) -0.050(5) 0.007(4) 0.019(5) F3' 0.060(4) 0.165(9) 0.131(7) 0.005(6) 0.000(4) -0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.7689(16) . ? Si1 C1 1.895(2) . ? Si1 C4 1.937(2) . ? Si1 Si5 2.3920(8) . ? Si2 C11 1.852(4) . ? Si2 C12 1.868(3) . ? Si2 C13 1.880(4) . ? Si2 C4 1.904(2) . ? Si3 C8 1.872(3) . ? Si3 C9 1.875(3) . ? Si3 C10 1.878(3) . ? Si3 C1 1.911(2) . ? Si4 C5 1.857(3) . ? Si4 C6 1.871(3) . ? Si4 C7 1.873(3) . ? Si4 C1 1.910(2) . ? Si5 C28 1.857(3) . ? Si5 C29 1.868(3) . ? Si5 C30 1.869(3) . ? N1 C22 1.398(2) . ? N1 C14 1.478(2) . ? C1 C2 1.580(3) . ? C2 C3 1.527(3) . ? C3 C4 1.548(3) . ? C4 C14 1.595(3) . ? C14 C15 1.520(3) . ? C15 C20 1.366(3) . ? C15 C16 1.389(3) . ? C16 C17 1.386(4) . ? C17 C18 1.362(4) . ? C18 C19 1.383(3) . ? C18 C21 1.495(4) . ? C19 C20 1.382(3) . ? C21 F2 1.282(9) . ? C21 F2' 1.290(9) . ? C21 F3' 1.295(9) . ? C21 F1' 1.305(8) . ? C21 F3 1.317(8) . ? C21 F1 1.362(9) . ? C22 C27 1.390(3) . ? C22 C23 1.393(3) . ? C23 C24 1.385(3) . ? C24 C25 1.366(4) . ? C25 C26 1.379(4) . ? C26 C27 1.377(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C1 111.81(8) . . ? N1 Si1 C4 78.44(8) . . ? C1 Si1 C4 99.38(9) . . ? N1 Si1 Si5 109.50(6) . . ? C1 Si1 Si5 124.35(7) . . ? C4 Si1 Si5 124.33(7) . . ? C11 Si2 C12 107.63(19) . . ? C11 Si2 C13 104.9(2) . . ? C12 Si2 C13 106.6(2) . . ? C11 Si2 C4 115.19(14) . . ? C12 Si2 C4 109.86(13) . . ? C13 Si2 C4 112.13(13) . . ? C8 Si3 C9 108.50(16) . . ? C8 Si3 C10 105.49(16) . . ? C9 Si3 C10 105.01(16) . . ? C8 Si3 C1 112.28(12) . . ? C9 Si3 C1 111.05(12) . . ? C10 Si3 C1 114.05(12) . . ? C5 Si4 C6 106.43(14) . . ? C5 Si4 C7 104.02(14) . . ? C6 Si4 C7 106.47(16) . . ? C5 Si4 C1 112.99(10) . . ? C6 Si4 C1 114.40(12) . . ? C7 Si4 C1 111.76(13) . . ? C28 Si5 C29 108.42(18) . . ? C28 Si5 C30 109.64(16) . . ? C29 Si5 C30 105.21(17) . . ? C28 Si5 Si1 104.07(11) . . ? C29 Si5 Si1 115.47(11) . . ? C30 Si5 Si1 113.92(10) . . ? C22 N1 C14 121.62(16) . . ? C22 N1 Si1 134.74(14) . . ? C14 N1 Si1 95.85(11) . . ? C2 C1 Si1 98.36(12) . . ? C2 C1 Si4 107.24(13) . . ? Si1 C1 Si4 116.36(10) . . ? C2 C1 Si3 109.03(13) . . ? Si1 C1 Si3 113.66(10) . . ? Si4 C1 Si3 111.03(10) . . ? C3 C2 C1 111.67(17) . . ? C2 C3 C4 112.35(16) . . ? C3 C4 C14 113.87(16) . . ? C3 C4 Si2 111.78(13) . . ? C14 C4 Si2 112.32(13) . . ? C3 C4 Si1 101.23(13) . . ? C14 C4 Si1 85.82(11) . . ? Si2 C4 Si1 129.48(11) . . ? N1 C14 C15 115.31(16) . . ? N1 C14 C4 99.55(14) . . ? C15 C14 C4 116.06(16) . . ? C20 C15 C16 117.8(2) . . ? C20 C15 C14 122.21(18) . . ? C16 C15 C14 120.0(2) . . ? C17 C16 C15 120.7(2) . . ? C18 C17 C16 120.6(2) . . ? C17 C18 C19 119.3(2) . . ? C17 C18 C21 121.4(3) . . ? C19 C18 C21 119.3(3) . . ? C20 C19 C18 119.8(2) . . ? C15 C20 C19 121.8(2) . . ? F2 C21 F2' 126.4(9) . . ? F2 C21 F3' 81.1(9) . . ? F2' C21 F3' 104.2(10) . . ? F2 C21 F1' 28.6(11) . . ? F2' C21 F1' 105.7(11) . . ? F3' C21 F1' 105.9(10) . . ? F2 C21 F3 109.0(8) . . ? F2' C21 F3 25.3(11) . . ? F3' C21 F3 122.9(9) . . ? F1' C21 F3 83.6(10) . . ? F2 C21 F1 103.8(7) . . ? F2' C21 F1 83.8(9) . . ? F3' C21 F1 24.3(10) . . ? F1' C21 F1 125.0(9) . . ? F3 C21 F1 106.6(7) . . ? F2 C21 C18 112.9(6) . . ? F2' C21 C18 113.0(8) . . ? F3' C21 C18 113.5(9) . . ? F1' C21 C18 113.7(7) . . ? F3 C21 C18 112.9(4) . . ? F1 C21 C18 111.1(6) . . ? C27 C22 C23 118.20(19) . . ? C27 C22 N1 119.44(18) . . ? C23 C22 N1 122.36(18) . . ? C24 C23 C22 120.1(2) . . ? C25 C24 C23 121.1(2) . . ? C24 C25 C26 119.0(2) . . ? C27 C26 C25 120.7(2) . . ? C26 C27 C22 120.7(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.314 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.050 data_mo_20101104b_0m _database_code_depnum_ccdc_archive 'CCDC 875348' #TrackingRef 'mo_20101104b_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H55 N Si5' _chemical_formula_weight 570.20 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 11.4647(8) _cell_length_b 11.7712(9) _cell_length_c 14.2938(11) _cell_angle_alpha 74.1470(10) _cell_angle_beta 82.1350(10) _cell_angle_gamma 69.5230(10) _cell_volume 1736.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9867 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.920 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23579 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6067 _reflns_number_gt 5449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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^)+(0.0836P)^2^+0.4035P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6067 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.1298 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 0.20305(4) 0.72773(4) 0.21688(3) 0.03003(14) Uani 1 1 d . . . Si4 Si 0.32074(5) 0.41749(4) 0.24985(4) 0.04171(15) Uani 1 1 d . . . Si5 Si 0.19205(5) 0.59188(5) 0.06128(3) 0.03924(15) Uani 1 1 d . . . Si3 Si 0.44673(5) 0.78216(5) 0.27788(4) 0.04714(16) Uani 1 1 d . . . Si2 Si 0.25142(6) 0.98161(5) 0.13222(4) 0.05041(17) Uani 1 1 d . . . C25 C -0.10232(17) 0.79555(18) 0.35290(13) 0.0433(4) Uani 1 1 d . . . C18 C 0.15193(17) 0.7143(2) 0.50738(13) 0.0485(5) Uani 1 1 d . . . C30 C -0.1651(2) 0.8010(2) 0.44186(16) 0.0626(6) Uani 1 1 d . . . H30 H -0.1377 0.7351 0.4959 0.075 Uiso 1 1 calc R . . C26 C -0.14603(19) 0.8946(2) 0.27392(15) 0.0564(5) Uani 1 1 d . . . H26 H -0.1056 0.8928 0.2131 0.068 Uiso 1 1 calc R . . C27 C -0.2491(2) 0.9963(2) 0.28437(19) 0.0694(6) Uani 1 1 d . . . H27 H -0.2776 1.0621 0.2305 0.083 Uiso 1 1 calc R . . C29 C -0.2683(2) 0.9032(3) 0.4520(2) 0.0768(7) Uani 1 1 d . . . H29 H -0.3095 0.9051 0.5126 0.092 Uiso 1 1 calc R . . C19 C 0.1672(2) 0.5891(2) 0.54329(15) 0.0592(5) Uani 1 1 d . . . H19 H 0.1709 0.5407 0.5006 0.071 Uiso 1 1 calc R . . C28 C -0.3098(2) 1.0010(2) 0.3737(2) 0.0719(7) Uani 1 1 d . . . H28 H -0.3784 1.0700 0.3808 0.086 Uiso 1 1 calc R . . C23 C 0.1469(3) 0.7844(3) 0.57240(17) 0.0779(7) Uani 1 1 d . . . H23 H 0.1352 0.8694 0.5500 0.093 Uiso 1 1 calc R . . C20 C 0.1774(2) 0.5338(3) 0.64274(18) 0.0762(7) Uani 1 1 d . . . H20 H 0.1865 0.4495 0.6661 0.091 Uiso 1 1 calc R . . C21 C 0.1740(3) 0.6038(4) 0.70563(17) 0.0923(10) Uani 1 1 d . . . H21 H 0.1817 0.5671 0.7719 0.111 Uiso 1 1 calc R . . C22 C 0.1594(4) 0.7277(4) 0.6709(2) 0.1024(11) Uani 1 1 d . . . H22 H 0.1578 0.7749 0.7139 0.123 Uiso 1 1 calc R . . C17 C 0.14197(18) 0.78096(18) 0.40016(12) 0.0430(4) Uani 1 1 d . . . H17A H 0.0696 0.8560 0.3936 0.052 Uiso 1 1 calc R . . H17B H 0.2147 0.8073 0.3795 0.052 Uiso 1 1 calc R . . C12 C 0.2581(2) 0.4508(2) 0.00911(17) 0.0615(6) Uani 1 1 d . . . H12A H 0.2113 0.4622 -0.0455 0.092 Uiso 1 1 calc R . . H12B H 0.2530 0.3780 0.0579 0.092 Uiso 1 1 calc R . . H12C H 0.3436 0.4401 -0.0118 0.092 Uiso 1 1 calc R . . C11 C 0.1934(2) 0.7237(2) -0.04747(14) 0.0607(6) Uani 1 1 d . . . H11A H 0.1490 0.7204 -0.0984 0.091 Uiso 1 1 calc R . . H11B H 0.2780 0.7163 -0.0700 0.091 Uiso 1 1 calc R . . H11C H 0.1540 0.8019 -0.0297 0.091 Uiso 1 1 calc R . . C14 C 0.4588(2) 0.30859(19) 0.19490(19) 0.0650(6) Uani 1 1 d . . . H14A H 0.4696 0.2238 0.2302 0.097 Uiso 1 1 calc R . . H14B H 0.5325 0.3281 0.1985 0.097 Uiso 1 1 calc R . . H14C H 0.4448 0.3184 0.1280 0.097 Uiso 1 1 calc R . . C15 C 0.1878(2) 0.3547(2) 0.27095(19) 0.0683(6) Uani 1 1 d . . . H15A H 0.2126 0.2719 0.3127 0.102 Uiso 1 1 calc R . . H15B H 0.1645 0.3519 0.2098 0.102 Uiso 1 1 calc R . . H15C H 0.1181 0.4080 0.3011 0.102 Uiso 1 1 calc R . . C16 C 0.3721(3) 0.3956(2) 0.37380(16) 0.0734(7) Uani 1 1 d . . . H16A H 0.3193 0.4630 0.4014 0.110 Uiso 1 1 calc R . . H16B H 0.4567 0.3946 0.3692 0.110 Uiso 1 1 calc R . . H16C H 0.3666 0.3177 0.4146 0.110 Uiso 1 1 calc R . . C10 C 0.4810(2) 0.6321(2) 0.37369(17) 0.0680(6) Uani 1 1 d . . . H10A H 0.5162 0.5631 0.3435 0.102 Uiso 1 1 calc R . . H10B H 0.4053 0.6265 0.4096 0.102 Uiso 1 1 calc R . . H10C H 0.5392 0.6295 0.4172 0.102 Uiso 1 1 calc R . . C9 C 0.4033(3) 0.9068(3) 0.34828(19) 0.0741(7) Uani 1 1 d . . . H9A H 0.3355 0.8986 0.3941 0.111 Uiso 1 1 calc R . . H9B H 0.3785 0.9879 0.3040 0.111 Uiso 1 1 calc R . . H9C H 0.4738 0.8974 0.3825 0.111 Uiso 1 1 calc R . . C8 C 0.6002(2) 0.7808(3) 0.21185(19) 0.0692(6) Uani 1 1 d . . . H8A H 0.6566 0.7801 0.2561 0.104 Uiso 1 1 calc R . . H8B H 0.5879 0.8542 0.1591 0.104 Uiso 1 1 calc R . . H8C H 0.6345 0.7076 0.1866 0.104 Uiso 1 1 calc R . . C7 C 0.3675(3) 1.0671(2) 0.1015(2) 0.0830(8) Uani 1 1 d . . . H7A H 0.3269 1.1529 0.0695 0.125 Uiso 1 1 calc R . . H7B H 0.4330 1.0289 0.0590 0.125 Uiso 1 1 calc R . . H7C H 0.4022 1.0634 0.1601 0.125 Uiso 1 1 calc R . . C6 C 0.1228(3) 1.0575(2) 0.2133(2) 0.0738(7) Uani 1 1 d . . . H6A H 0.1560 1.0514 0.2733 0.111 Uiso 1 1 calc R . . H6B H 0.0614 1.0161 0.2267 0.111 Uiso 1 1 calc R . . H6C H 0.0848 1.1439 0.1817 0.111 Uiso 1 1 calc R . . C5 C 0.1798(3) 1.0165(2) 0.0131(2) 0.0859(9) Uani 1 1 d . . . H5A H 0.1146 0.9804 0.0225 0.129 Uiso 1 1 calc R . . H5B H 0.2423 0.9817 -0.0326 0.129 Uiso 1 1 calc R . . H5C H 0.1457 1.1054 -0.0116 0.129 Uiso 1 1 calc R . . C4 C 0.28317(15) 0.58202(14) 0.16763(11) 0.0316(3) Uani 1 1 d . . . C1 C 0.32683(16) 0.80693(15) 0.18642(12) 0.0355(4) Uani 1 1 d . . . C2 C 0.39646(17) 0.74363(16) 0.10067(12) 0.0396(4) Uani 1 1 d . . . H2A H 0.3495 0.7851 0.0423 0.048 Uiso 1 1 calc R . . H2B H 0.4781 0.7534 0.0870 0.048 Uiso 1 1 calc R . . C3 C 0.41097(16) 0.60426(16) 0.12749(13) 0.0381(4) Uani 1 1 d . . . H3A H 0.4725 0.5598 0.1766 0.046 Uiso 1 1 calc R . . H3B H 0.4407 0.5709 0.0704 0.046 Uiso 1 1 calc R . . N1 N 0.13196(13) 0.71188(13) 0.33309(10) 0.0377(3) Uani 1 1 d . . . C24 C 0.01319(17) 0.68520(17) 0.34405(13) 0.0425(4) Uani 1 1 d . . . H24A H 0.0157 0.6177 0.4015 0.051 Uiso 1 1 calc R . . H24B H 0.0064 0.6563 0.2883 0.051 Uiso 1 1 calc R . . C13 C 0.02321(19) 0.6112(2) 0.09433(16) 0.0557(5) Uani 1 1 d . . . H13A H -0.0173 0.6898 0.1113 0.084 Uiso 1 1 calc R . . H13B H 0.0165 0.5445 0.1488 0.084 Uiso 1 1 calc R . . H13C H -0.0159 0.6092 0.0398 0.084 Uiso 1 1 calc R . . H1 H 0.1044(17) 0.8049(17) 0.1530(13) 0.040(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0317(2) 0.0305(2) 0.0285(2) -0.00843(17) -0.00168(17) -0.00984(18) Si4 0.0472(3) 0.0308(2) 0.0448(3) -0.0063(2) -0.0041(2) -0.0115(2) Si5 0.0427(3) 0.0441(3) 0.0360(3) -0.0153(2) -0.0038(2) -0.0154(2) Si3 0.0455(3) 0.0566(3) 0.0493(3) -0.0161(2) -0.0048(2) -0.0255(2) Si2 0.0628(4) 0.0317(3) 0.0563(3) -0.0083(2) -0.0024(3) -0.0169(2) C25 0.0396(9) 0.0538(10) 0.0426(9) -0.0132(8) 0.0019(7) -0.0231(8) C18 0.0402(10) 0.0746(13) 0.0360(9) -0.0225(9) 0.0032(7) -0.0200(9) C30 0.0617(13) 0.0667(13) 0.0486(11) -0.0112(10) 0.0102(10) -0.0147(11) C26 0.0474(11) 0.0710(13) 0.0464(10) -0.0068(10) -0.0011(8) -0.0199(10) C27 0.0529(13) 0.0661(14) 0.0758(15) -0.0026(12) -0.0088(11) -0.0120(11) C29 0.0674(15) 0.0885(18) 0.0680(15) -0.0305(14) 0.0217(12) -0.0179(14) C19 0.0536(12) 0.0754(14) 0.0422(10) -0.0136(10) -0.0018(9) -0.0142(11) C28 0.0512(13) 0.0671(14) 0.0931(18) -0.0266(13) 0.0013(12) -0.0106(11) C23 0.104(2) 0.0970(19) 0.0502(13) -0.0354(13) 0.0064(12) -0.0443(16) C20 0.0648(15) 0.0961(19) 0.0518(13) 0.0031(12) -0.0066(11) -0.0218(14) C21 0.090(2) 0.153(3) 0.0343(12) -0.0135(15) -0.0017(12) -0.048(2) C22 0.133(3) 0.157(3) 0.0440(14) -0.0457(18) 0.0040(15) -0.067(3) C17 0.0458(10) 0.0516(10) 0.0385(9) -0.0183(8) 0.0017(7) -0.0200(8) C12 0.0678(14) 0.0668(13) 0.0617(13) -0.0374(11) -0.0045(10) -0.0194(11) C11 0.0799(15) 0.0703(13) 0.0361(10) -0.0076(9) -0.0122(10) -0.0301(12) C14 0.0631(14) 0.0408(10) 0.0813(15) -0.0196(10) -0.0055(11) -0.0007(10) C15 0.0706(15) 0.0516(12) 0.0795(16) 0.0041(11) -0.0042(12) -0.0310(11) C16 0.107(2) 0.0534(12) 0.0507(12) 0.0006(10) -0.0196(12) -0.0188(13) C10 0.0610(14) 0.0807(16) 0.0596(13) -0.0006(11) -0.0194(11) -0.0265(12) C9 0.0834(17) 0.0934(18) 0.0755(16) -0.0456(14) -0.0020(13) -0.0469(15) C8 0.0484(12) 0.0896(17) 0.0791(16) -0.0186(13) -0.0031(11) -0.0357(12) C7 0.103(2) 0.0498(13) 0.101(2) -0.0112(13) 0.0109(16) -0.0431(14) C6 0.0740(16) 0.0450(11) 0.0918(18) -0.0207(12) 0.0040(13) -0.0065(11) C5 0.123(2) 0.0447(12) 0.0755(16) 0.0074(11) -0.0370(16) -0.0153(14) C4 0.0335(8) 0.0304(7) 0.0324(8) -0.0096(6) -0.0009(6) -0.0110(6) C1 0.0394(9) 0.0334(8) 0.0379(8) -0.0105(7) -0.0008(7) -0.0159(7) C2 0.0424(9) 0.0427(9) 0.0373(8) -0.0110(7) 0.0049(7) -0.0197(7) C3 0.0348(8) 0.0409(9) 0.0403(9) -0.0146(7) 0.0038(7) -0.0132(7) N1 0.0403(8) 0.0458(8) 0.0322(7) -0.0146(6) 0.0035(6) -0.0186(6) C24 0.0457(10) 0.0482(10) 0.0394(9) -0.0138(7) 0.0040(7) -0.0222(8) C13 0.0454(11) 0.0678(13) 0.0605(12) -0.0215(10) -0.0078(9) -0.0201(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.7392(14) . ? Si1 C1 1.8994(17) . ? Si1 C4 1.9135(15) . ? Si1 H1 1.432(18) . ? Si4 C16 1.866(2) . ? Si4 C15 1.871(2) . ? Si4 C14 1.886(2) . ? Si4 C4 1.9049(16) . ? Si5 C11 1.875(2) . ? Si5 C13 1.877(2) . ? Si5 C12 1.879(2) . ? Si5 C4 1.9155(16) . ? Si3 C10 1.869(2) . ? Si3 C8 1.876(2) . ? Si3 C9 1.890(2) . ? Si3 C1 1.9201(17) . ? Si2 C6 1.869(3) . ? Si2 C5 1.872(3) . ? Si2 C7 1.875(3) . ? Si2 C1 1.9091(17) . ? C25 C30 1.378(3) . ? C25 C26 1.383(3) . ? C25 C24 1.516(3) . ? C18 C19 1.377(3) . ? C18 C23 1.385(3) . ? C18 C17 1.519(3) . ? C30 C29 1.386(3) . ? C30 H30 0.9300 . ? C26 C27 1.383(3) . ? C26 H26 0.9300 . ? C27 C28 1.374(4) . ? C27 H27 0.9300 . ? C29 C28 1.365(4) . ? C29 H29 0.9300 . ? C19 C20 1.395(3) . ? C19 H19 0.9300 . ? C28 H28 0.9300 . ? C23 C22 1.387(4) . ? C23 H23 0.9300 . ? C20 C21 1.364(4) . ? C20 H20 0.9300 . ? C21 C22 1.363(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C17 N1 1.454(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C4 C3 1.581(2) . ? C1 C2 1.584(2) . ? C2 C3 1.533(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C24 1.480(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 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 Si1 C1 118.89(7) . . ? N1 Si1 C4 119.21(7) . . ? C1 Si1 C4 101.23(7) . . ? N1 Si1 H1 105.0(7) . . ? C1 Si1 H1 105.6(7) . . ? C4 Si1 H1 105.6(7) . . ? C16 Si4 C15 105.12(13) . . ? C16 Si4 C14 102.81(12) . . ? C15 Si4 C14 108.95(12) . . ? C16 Si4 C4 116.34(9) . . ? C15 Si4 C4 113.60(9) . . ? C14 Si4 C4 109.31(9) . . ? C11 Si5 C13 105.57(11) . . ? C11 Si5 C12 102.75(11) . . ? C13 Si5 C12 106.89(11) . . ? C11 Si5 C4 114.43(9) . . ? C13 Si5 C4 113.34(8) . . ? C12 Si5 C4 112.95(9) . . ? C10 Si3 C8 105.46(12) . . ? C10 Si3 C9 104.38(13) . . ? C8 Si3 C9 106.70(12) . . ? C10 Si3 C1 115.49(9) . . ? C8 Si3 C1 109.60(10) . . ? C9 Si3 C1 114.48(10) . . ? C6 Si2 C5 105.51(14) . . ? C6 Si2 C7 109.45(13) . . ? C5 Si2 C7 103.30(14) . . ? C6 Si2 C1 112.46(10) . . ? C5 Si2 C1 113.12(9) . . ? C7 Si2 C1 112.40(11) . . ? C30 C25 C26 118.04(19) . . ? C30 C25 C24 120.18(18) . . ? C26 C25 C24 121.76(17) . . ? C19 C18 C23 118.4(2) . . ? C19 C18 C17 124.16(18) . . ? C23 C18 C17 117.4(2) . . ? C25 C30 C29 121.0(2) . . ? C25 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C25 C26 C27 120.8(2) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C28 C27 C26 120.5(2) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C28 C29 C30 120.5(2) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C18 C19 C20 120.9(2) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C29 C28 C27 119.2(2) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C18 C23 C22 120.0(3) . . ? C18 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 119.7(2) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 121.0(3) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? N1 C17 C18 117.48(16) . . ? N1 C17 H17A 107.9 . . ? C18 C17 H17A 107.9 . . ? N1 C17 H17B 107.9 . . ? C18 C17 H17B 107.9 . . ? H17A C17 H17B 107.2 . . ? Si5 C12 H12A 109.5 . . ? Si5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si5 C11 H11A 109.5 . . ? Si5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si4 C14 H14A 109.5 . . ? Si4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si4 C15 H15A 109.5 . . ? Si4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si4 C16 H16A 109.5 . . ? Si4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si3 C10 H10A 109.5 . . ? Si3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C4 Si4 107.66(10) . . ? C3 C4 Si1 99.72(10) . . ? Si4 C4 Si1 122.11(8) . . ? C3 C4 Si5 109.55(11) . . ? Si4 C4 Si5 108.41(8) . . ? Si1 C4 Si5 108.70(8) . . ? C2 C1 Si1 96.74(10) . . ? C2 C1 Si2 108.18(11) . . ? Si1 C1 Si2 109.75(9) . . ? C2 C1 Si3 108.87(11) . . ? Si1 C1 Si3 122.38(9) . . ? Si2 C1 Si3 109.57(8) . . ? C3 C2 C1 110.97(13) . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 111.37(13) . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C17 N1 C24 114.27(13) . . ? C17 N1 Si1 122.19(12) . . ? C24 N1 Si1 116.02(11) . . ? N1 C24 C25 114.62(15) . . ? N1 C24 H24A 108.6 . . ? C25 C24 H24A 108.6 . . ? N1 C24 H24B 108.6 . . ? C25 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? Si5 C13 H13A 109.5 . . ? Si5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 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 C26 C25 C30 C29 -0.5(4) . . . . ? C24 C25 C30 C29 177.7(2) . . . . ? C30 C25 C26 C27 0.5(3) . . . . ? C24 C25 C26 C27 -177.8(2) . . . . ? C25 C26 C27 C28 0.3(4) . . . . ? C25 C30 C29 C28 -0.1(4) . . . . ? C23 C18 C19 C20 0.1(3) . . . . ? C17 C18 C19 C20 179.1(2) . . . . ? C30 C29 C28 C27 0.9(4) . . . . ? C26 C27 C28 C29 -0.9(4) . . . . ? C19 C18 C23 C22 1.1(4) . . . . ? C17 C18 C23 C22 -178.0(3) . . . . ? C18 C19 C20 C21 -1.0(4) . . . . ? C19 C20 C21 C22 0.7(5) . . . . ? C20 C21 C22 C23 0.5(5) . . . . ? C18 C23 C22 C21 -1.4(5) . . . . ? C19 C18 C17 N1 8.2(3) . . . . ? C23 C18 C17 N1 -172.7(2) . . . . ? C16 Si4 C4 C3 76.85(15) . . . . ? C15 Si4 C4 C3 -160.88(13) . . . . ? C14 Si4 C4 C3 -38.97(14) . . . . ? C16 Si4 C4 Si1 -37.29(16) . . . . ? C15 Si4 C4 Si1 84.98(14) . . . . ? C14 Si4 C4 Si1 -153.12(11) . . . . ? C16 Si4 C4 Si5 -164.72(12) . . . . ? C15 Si4 C4 Si5 -42.45(13) . . . . ? C14 Si4 C4 Si5 79.46(11) . . . . ? N1 Si1 C4 C3 -132.37(10) . . . . ? C1 Si1 C4 C3 0.10(11) . . . . ? N1 Si1 C4 Si4 -14.27(13) . . . . ? C1 Si1 C4 Si4 118.20(10) . . . . ? N1 Si1 C4 Si5 113.02(8) . . . . ? C1 Si1 C4 Si5 -114.51(8) . . . . ? C11 Si5 C4 C3 -42.99(14) . . . . ? C13 Si5 C4 C3 -164.13(12) . . . . ? C12 Si5 C4 C3 74.11(14) . . . . ? C11 Si5 C4 Si4 -160.22(10) . . . . ? C13 Si5 C4 Si4 78.64(11) . . . . ? C12 Si5 C4 Si4 -43.12(12) . . . . ? C11 Si5 C4 Si1 65.03(12) . . . . ? C13 Si5 C4 Si1 -56.11(11) . . . . ? C12 Si5 C4 Si1 -177.87(10) . . . . ? N1 Si1 C1 C2 155.99(10) . . . . ? C4 Si1 C1 C2 23.33(11) . . . . ? N1 Si1 C1 Si2 -91.91(10) . . . . ? C4 Si1 C1 Si2 135.43(8) . . . . ? N1 Si1 C1 Si3 38.57(13) . . . . ? C4 Si1 C1 Si3 -94.10(10) . . . . ? C6 Si2 C1 C2 159.68(14) . . . . ? C5 Si2 C1 C2 40.27(18) . . . . ? C7 Si2 C1 C2 -76.25(16) . . . . ? C6 Si2 C1 Si1 55.25(13) . . . . ? C5 Si2 C1 Si1 -64.16(15) . . . . ? C7 Si2 C1 Si1 179.32(12) . . . . ? C6 Si2 C1 Si3 -81.76(13) . . . . ? C5 Si2 C1 Si3 158.83(14) . . . . ? C7 Si2 C1 Si3 42.30(14) . . . . ? C10 Si3 C1 C2 -86.27(15) . . . . ? C8 Si3 C1 C2 32.63(15) . . . . ? C9 Si3 C1 C2 152.45(13) . . . . ? C10 Si3 C1 Si1 25.05(15) . . . . ? C8 Si3 C1 Si1 143.95(12) . . . . ? C9 Si3 C1 Si1 -96.23(13) . . . . ? C10 Si3 C1 Si2 155.60(11) . . . . ? C8 Si3 C1 Si2 -85.50(12) . . . . ? C9 Si3 C1 Si2 34.32(13) . . . . ? Si1 C1 C2 C3 -42.65(15) . . . . ? Si2 C1 C2 C3 -156.04(12) . . . . ? Si3 C1 C2 C3 84.96(15) . . . . ? C1 C2 C3 C4 49.44(19) . . . . ? Si4 C4 C3 C2 -154.41(12) . . . . ? Si1 C4 C3 C2 -26.06(15) . . . . ? Si5 C4 C3 C2 87.89(14) . . . . ? C18 C17 N1 C24 68.4(2) . . . . ? C18 C17 N1 Si1 -143.16(14) . . . . ? C1 Si1 N1 C17 14.43(17) . . . . ? C4 Si1 N1 C17 138.71(13) . . . . ? C1 Si1 N1 C24 162.41(11) . . . . ? C4 Si1 N1 C24 -73.32(14) . . . . ? C17 N1 C24 C25 45.7(2) . . . . ? Si1 N1 C24 C25 -104.77(15) . . . . ? C30 C25 C24 N1 -105.2(2) . . . . ? C26 C25 C24 N1 73.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.365 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.057 data_mo_20101106a_0m _database_code_depnum_ccdc_archive 'CCDC 875349' #TrackingRef 'mo_20101106a_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H53 N O Si5' _chemical_formula_weight 584.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1986(8) _cell_length_b 11.4219(9) _cell_length_c 16.3207(12) _cell_angle_alpha 77.5760(10) _cell_angle_beta 78.1960(10) _cell_angle_gamma 71.5880(10) _cell_volume 1742.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9894 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 0.227 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.902 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24536 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6091 _reflns_number_gt 5171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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^)+(0.1012P)^2^+0.4546P] 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 6091 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 0.33263(5) 0.80983(5) 0.27300(3) 0.02985(17) Uani 1 1 d . . . Si2 Si 0.18712(7) 0.72277(7) 0.45840(4) 0.0474(2) Uani 1 1 d . . . Si3 Si 0.46679(7) 1.00361(6) 0.31635(4) 0.0458(2) Uani 1 1 d . . . Si4 Si 0.28945(8) 0.53895(6) 0.32531(4) 0.0500(2) Uani 1 1 d . . . Si5 Si 0.64680(7) 0.80916(7) 0.19994(4) 0.0506(2) Uani 1 1 d . . . C14 C 0.4942(2) 0.84200(19) 0.28953(13) 0.0345(4) Uani 1 1 d . . . C17 C 0.3207(2) 0.67407(19) 0.36171(13) 0.0359(5) Uani 1 1 d . . . C1 C 0.2758(2) 0.8019(2) 0.09823(13) 0.0387(5) Uani 1 1 d . . . C13 C 0.1745(2) 0.9132(2) 0.22578(13) 0.0366(5) Uani 1 1 d . . . H13 H 0.0924 0.8819 0.2455 0.044 Uiso 1 1 calc R . . C7 C 0.1374(2) 1.0506(2) 0.19583(13) 0.0389(5) Uani 1 1 d . . . C15 C 0.5319(2) 0.7442(2) 0.37186(15) 0.0452(5) Uani 1 1 d . . . H15A H 0.6328 0.7142 0.3688 0.054 Uiso 1 1 calc R . . H15B H 0.4948 0.7856 0.4212 0.054 Uiso 1 1 calc R . . C16 C 0.4736(2) 0.6316(2) 0.38300(15) 0.0460(5) Uani 1 1 d . . . H16A H 0.4744 0.5884 0.4411 0.055 Uiso 1 1 calc R . . H16B H 0.5332 0.5736 0.3460 0.055 Uiso 1 1 calc R . . C8 C 0.2174(3) 1.1055(2) 0.12918(15) 0.0469(6) Uani 1 1 d . . . H8 H 0.2947 1.0549 0.0997 0.056 Uiso 1 1 calc R . . C6 C 0.1512(3) 0.8502(2) 0.06402(16) 0.0484(6) Uani 1 1 d . . . H6 H 0.0740 0.9023 0.0927 0.058 Uiso 1 1 calc R . . C2 C 0.3901(3) 0.7262(2) 0.05132(15) 0.0505(6) Uani 1 1 d . . . H2 H 0.4755 0.6947 0.0714 0.061 Uiso 1 1 calc R . . C10 C 0.0715(3) 1.3106(2) 0.14736(17) 0.0538(6) Uani 1 1 d . . . C9 C 0.1853(3) 1.2347(2) 0.10511(16) 0.0548(6) Uani 1 1 d . . . H9 H 0.2412 1.2694 0.0603 0.066 Uiso 1 1 calc R . . C12 C 0.0181(3) 1.1300(2) 0.23499(17) 0.0532(6) Uani 1 1 d . . . H12 H -0.0413 1.0962 0.2779 0.064 Uiso 1 1 calc R . . C5 C 0.1414(3) 0.8212(3) -0.01233(18) 0.0634(8) Uani 1 1 d . . . H5 H 0.0576 0.8539 -0.0344 0.076 Uiso 1 1 calc R . . C11 C -0.0130(3) 1.2591(2) 0.21057(18) 0.0606(7) Uani 1 1 d . . . H11 H -0.0925 1.3107 0.2378 0.073 Uiso 1 1 calc R . . C23 C 0.4944(4) 1.1260(3) 0.2243(2) 0.0781(9) Uani 1 1 d . . . H23A H 0.4328 1.1348 0.1846 0.117 Uiso 1 1 calc R . . H23B H 0.5895 1.1022 0.1970 0.117 Uiso 1 1 calc R . . H23C H 0.4751 1.2042 0.2436 0.117 Uiso 1 1 calc R . . C20 C 0.3259(4) 0.3931(3) 0.4060(2) 0.0807(10) Uani 1 1 d . . . H20A H 0.2453 0.3948 0.4486 0.121 Uiso 1 1 calc R . . H20B H 0.4042 0.3883 0.4321 0.121 Uiso 1 1 calc R . . H20C H 0.3470 0.3214 0.3788 0.121 Uiso 1 1 calc R . . C4 C 0.2540(4) 0.7448(3) -0.05569(17) 0.0712(9) Uani 1 1 d . . . H4 H 0.2462 0.7252 -0.1066 0.085 Uiso 1 1 calc R . . C24 C 0.6077(3) 0.9016(3) 0.09383(16) 0.0665(8) Uani 1 1 d . . . H24A H 0.6920 0.8892 0.0537 0.100 Uiso 1 1 calc R . . H24B H 0.5702 0.9887 0.0983 0.100 Uiso 1 1 calc R . . H24C H 0.5406 0.8741 0.0751 0.100 Uiso 1 1 calc R . . C3 C 0.3771(4) 0.6979(3) -0.02415(18) 0.0670(8) Uani 1 1 d . . . H3 H 0.4533 0.6462 -0.0537 0.080 Uiso 1 1 calc R . . C22 C 0.5934(4) 0.9948(3) 0.3875(2) 0.0786(9) Uani 1 1 d . . . H22A H 0.5665 1.0711 0.4104 0.118 Uiso 1 1 calc R . . H22B H 0.6855 0.9830 0.3556 0.118 Uiso 1 1 calc R . . H22C H 0.5931 0.9258 0.4330 0.118 Uiso 1 1 calc R . . C21 C 0.2873(3) 1.0657(3) 0.3732(2) 0.0691(8) Uani 1 1 d . . . H21A H 0.2866 1.1297 0.4031 0.104 Uiso 1 1 calc R . . H21B H 0.2602 0.9991 0.4128 0.104 Uiso 1 1 calc R . . H21C H 0.2229 1.1002 0.3329 0.104 Uiso 1 1 calc R . . C19 C 0.1087(4) 0.5810(3) 0.3001(2) 0.0787(10) Uani 1 1 d . . . H19A H 0.0937 0.5100 0.2850 0.118 Uiso 1 1 calc R . . H19B H 0.0964 0.6490 0.2535 0.118 Uiso 1 1 calc R . . H19C H 0.0428 0.6056 0.3489 0.118 Uiso 1 1 calc R . . C18 C 0.4110(4) 0.4918(3) 0.2282(2) 0.0835(10) Uani 1 1 d . . . H18A H 0.3828 0.4317 0.2080 0.125 Uiso 1 1 calc R . . H18B H 0.5043 0.4553 0.2416 0.125 Uiso 1 1 calc R . . H18C H 0.4085 0.5640 0.1851 0.125 Uiso 1 1 calc R . . C26 C 0.1306(5) 0.5899(4) 0.5297(2) 0.0983(13) Uani 1 1 d . . . H26A H 0.0624 0.6208 0.5759 0.147 Uiso 1 1 calc R . . H26B H 0.2100 0.5292 0.5515 0.147 Uiso 1 1 calc R . . H26C H 0.0903 0.5517 0.4981 0.147 Uiso 1 1 calc R . . C25 C 0.8014(3) 0.8455(4) 0.2229(2) 0.0838(10) Uani 1 1 d . . . H25A H 0.8814 0.8162 0.1822 0.126 Uiso 1 1 calc R . . H25B H 0.8203 0.8048 0.2789 0.126 Uiso 1 1 calc R . . H25C H 0.7815 0.9343 0.2194 0.126 Uiso 1 1 calc R . . C28 C 0.2613(4) 0.7777(4) 0.5346(2) 0.0880(11) Uani 1 1 d . . . H28A H 0.3088 0.8380 0.5040 0.132 Uiso 1 1 calc R . . H28B H 0.3261 0.7078 0.5629 0.132 Uiso 1 1 calc R . . H28C H 0.1870 0.8155 0.5757 0.132 Uiso 1 1 calc R . . C27 C 0.0264(3) 0.8457(4) 0.4317(2) 0.0878(11) Uani 1 1 d . . . H27A H -0.0152 0.8189 0.3940 0.132 Uiso 1 1 calc R . . H27B H 0.0495 0.9215 0.4045 0.132 Uiso 1 1 calc R . . H27C H -0.0384 0.8604 0.4826 0.132 Uiso 1 1 calc R . . C29 C 0.1242(4) 1.4980(3) 0.0701(3) 0.0889(11) Uani 1 1 d . . . H29A H 0.2142 1.4712 0.0884 0.133 Uiso 1 1 calc R . . H29B H 0.0874 1.5871 0.0664 0.133 Uiso 1 1 calc R . . H29C H 0.1332 1.4754 0.0154 0.133 Uiso 1 1 calc R . . O1 O 0.0327(2) 1.43961(17) 0.12894(15) 0.0778(6) Uani 1 1 d . . . N1 N 0.28817(18) 0.83065(16) 0.17407(11) 0.0382(4) Uani 1 1 d . . . C30 C 0.7070(4) 0.6394(3) 0.1905(2) 0.0866(11) Uani 1 1 d . . . H30A H 0.6303 0.6142 0.1818 0.130 Uiso 1 1 calc R . . H30B H 0.7412 0.5911 0.2416 0.130 Uiso 1 1 calc R . . H30C H 0.7805 0.6258 0.1433 0.130 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0309(3) 0.0285(3) 0.0295(3) -0.0038(2) -0.0049(2) -0.0078(2) Si2 0.0544(4) 0.0556(4) 0.0365(4) -0.0046(3) 0.0015(3) -0.0286(3) Si3 0.0528(4) 0.0472(4) 0.0463(4) -0.0105(3) -0.0043(3) -0.0268(3) Si4 0.0726(5) 0.0340(3) 0.0498(4) -0.0016(3) -0.0192(3) -0.0210(3) Si5 0.0332(3) 0.0655(5) 0.0468(4) -0.0101(3) 0.0029(3) -0.0102(3) C14 0.0335(10) 0.0389(11) 0.0320(10) -0.0019(8) -0.0065(8) -0.0129(9) C17 0.0421(11) 0.0315(10) 0.0361(11) 0.0000(8) -0.0094(9) -0.0147(9) C1 0.0504(12) 0.0365(11) 0.0322(11) -0.0010(9) -0.0102(9) -0.0168(9) C13 0.0343(10) 0.0393(11) 0.0336(11) -0.0056(9) -0.0039(8) -0.0077(9) C7 0.0363(11) 0.0411(12) 0.0354(11) -0.0064(9) -0.0089(9) -0.0032(9) C15 0.0457(12) 0.0527(13) 0.0389(12) 0.0063(10) -0.0166(10) -0.0190(10) C16 0.0464(13) 0.0439(13) 0.0451(13) 0.0055(10) -0.0162(10) -0.0119(10) C8 0.0505(13) 0.0374(12) 0.0412(12) -0.0043(10) 0.0006(10) -0.0023(10) C6 0.0530(14) 0.0458(13) 0.0502(14) -0.0013(11) -0.0184(11) -0.0171(11) C2 0.0558(15) 0.0560(14) 0.0386(12) -0.0113(11) -0.0054(11) -0.0131(12) C10 0.0610(15) 0.0364(12) 0.0582(16) -0.0081(11) -0.0159(12) -0.0010(11) C9 0.0639(16) 0.0431(13) 0.0471(14) -0.0004(11) -0.0014(12) -0.0096(12) C12 0.0458(13) 0.0451(13) 0.0539(15) -0.0049(11) 0.0013(11) 0.0001(11) C5 0.082(2) 0.0703(18) 0.0523(16) 0.0029(14) -0.0339(15) -0.0350(16) C11 0.0563(15) 0.0446(14) 0.0634(17) -0.0126(12) -0.0037(13) 0.0095(12) C23 0.111(3) 0.0554(17) 0.077(2) 0.0018(15) -0.0102(18) -0.0470(18) C20 0.126(3) 0.0433(15) 0.081(2) 0.0085(14) -0.034(2) -0.0349(17) C4 0.110(3) 0.083(2) 0.0369(14) -0.0084(14) -0.0184(15) -0.046(2) C24 0.0640(17) 0.091(2) 0.0414(14) -0.0123(14) 0.0108(12) -0.0280(16) C3 0.084(2) 0.076(2) 0.0476(15) -0.0259(14) 0.0025(14) -0.0297(16) C22 0.083(2) 0.108(3) 0.074(2) -0.0321(19) -0.0161(17) -0.052(2) C21 0.0690(18) 0.0622(17) 0.084(2) -0.0372(16) 0.0040(15) -0.0232(14) C19 0.090(2) 0.075(2) 0.092(2) -0.0078(18) -0.0401(19) -0.0405(18) C18 0.124(3) 0.0476(16) 0.076(2) -0.0243(15) -0.001(2) -0.0208(18) C26 0.131(3) 0.101(3) 0.072(2) -0.0052(19) 0.022(2) -0.074(3) C25 0.0395(15) 0.130(3) 0.081(2) -0.011(2) -0.0015(14) -0.0311(17) C28 0.100(3) 0.129(3) 0.0586(19) -0.037(2) 0.0065(17) -0.063(2) C27 0.0608(19) 0.116(3) 0.064(2) -0.0174(19) 0.0114(15) -0.0048(19) C29 0.119(3) 0.0401(16) 0.103(3) 0.0062(16) -0.025(2) -0.0233(18) O1 0.0927(16) 0.0343(10) 0.0907(16) -0.0076(10) -0.0112(12) 0.0009(10) N1 0.0394(9) 0.0356(9) 0.0365(10) -0.0088(7) -0.0096(7) -0.0018(7) C30 0.0637(19) 0.078(2) 0.096(3) -0.0298(19) 0.0082(17) 0.0087(16) _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 N1 1.7134(18) . ? Si1 C13 1.872(2) . ? Si1 C14 1.878(2) . ? Si1 C17 1.896(2) . ? Si2 C27 1.850(3) . ? Si2 C26 1.873(3) . ? Si2 C28 1.879(3) . ? Si2 C17 1.917(2) . ? Si3 C23 1.861(3) . ? Si3 C21 1.866(3) . ? Si3 C22 1.873(3) . ? Si3 C14 1.910(2) . ? Si4 C19 1.861(3) . ? Si4 C18 1.866(3) . ? Si4 C20 1.875(3) . ? Si4 C17 1.902(2) . ? Si5 C30 1.870(3) . ? Si5 C24 1.872(3) . ? Si5 C25 1.876(3) . ? Si5 C14 1.907(2) . ? C14 C15 1.580(3) . ? C17 C16 1.568(3) . ? C1 N1 1.386(3) . ? C1 C6 1.396(3) . ? C1 C2 1.406(3) . ? C13 N1 1.482(3) . ? C13 C7 1.489(3) . ? C13 H13 0.9800 . ? C7 C8 1.382(3) . ? C7 C12 1.395(3) . ? C15 C16 1.543(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C8 C9 1.392(3) . ? C8 H8 0.9300 . ? C6 C5 1.386(4) . ? C6 H6 0.9300 . ? C2 C3 1.380(4) . ? C2 H2 0.9300 . ? C10 C11 1.360(4) . ? C10 C9 1.367(4) . ? C10 O1 1.381(3) . ? C9 H9 0.9300 . ? C12 C11 1.392(4) . ? C12 H12 0.9300 . ? C5 C4 1.372(5) . ? C5 H5 0.9300 . ? C11 H11 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C4 C3 1.359(5) . ? C4 H4 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C3 H3 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C29 O1 1.410(4) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 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 Si1 C13 48.59(9) . . ? N1 Si1 C14 122.03(9) . . ? C13 Si1 C14 131.85(10) . . ? N1 Si1 C17 126.22(9) . . ? C13 Si1 C17 121.20(9) . . ? C14 Si1 C17 101.25(9) . . ? C27 Si2 C26 106.9(2) . . ? C27 Si2 C28 107.72(19) . . ? C26 Si2 C28 100.41(18) . . ? C27 Si2 C17 114.13(12) . . ? C26 Si2 C17 113.69(15) . . ? C28 Si2 C17 112.90(13) . . ? C23 Si3 C21 106.69(16) . . ? C23 Si3 C22 105.13(16) . . ? C21 Si3 C22 107.37(15) . . ? C23 Si3 C14 115.51(13) . . ? C21 Si3 C14 111.64(11) . . ? C22 Si3 C14 110.02(13) . . ? C19 Si4 C18 106.98(18) . . ? C19 Si4 C20 110.91(17) . . ? C18 Si4 C20 103.49(16) . . ? C19 Si4 C17 110.97(13) . . ? C18 Si4 C17 112.80(13) . . ? C20 Si4 C17 111.39(13) . . ? C30 Si5 C24 108.20(16) . . ? C30 Si5 C25 105.74(18) . . ? C24 Si5 C25 106.97(15) . . ? C30 Si5 C14 110.89(13) . . ? C24 Si5 C14 114.09(11) . . ? C25 Si5 C14 110.53(13) . . ? C15 C14 Si1 100.99(13) . . ? C15 C14 Si5 109.08(15) . . ? Si1 C14 Si5 114.29(11) . . ? C15 C14 Si3 106.80(15) . . ? Si1 C14 Si3 115.39(11) . . ? Si5 C14 Si3 109.55(10) . . ? C16 C17 Si1 99.82(13) . . ? C16 C17 Si4 108.20(15) . . ? Si1 C17 Si4 113.27(11) . . ? C16 C17 Si2 111.05(15) . . ? Si1 C17 Si2 113.30(11) . . ? Si4 C17 Si2 110.64(10) . . ? N1 C1 C6 121.4(2) . . ? N1 C1 C2 121.2(2) . . ? C6 C1 C2 117.4(2) . . ? N1 C13 C7 118.54(18) . . ? N1 C13 Si1 60.11(10) . . ? C7 C13 Si1 128.51(16) . . ? N1 C13 H13 113.0 . . ? C7 C13 H13 113.0 . . ? Si1 C13 H13 113.0 . . ? C8 C7 C12 117.0(2) . . ? C8 C7 C13 122.6(2) . . ? C12 C7 C13 120.4(2) . . ? C16 C15 C14 112.70(18) . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 C17 111.39(18) . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C7 C8 C9 121.7(2) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C5 C6 C1 120.5(3) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C3 C2 C1 120.9(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C11 C10 C9 119.7(2) . . ? C11 C10 O1 116.2(2) . . ? C9 C10 O1 124.1(3) . . ? C10 C9 C8 120.0(2) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C12 C7 120.8(2) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? C4 C5 C6 120.6(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C10 C11 C12 120.7(2) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C20 H20A 109.5 . . ? Si4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? Si5 C24 H24A 109.5 . . ? Si5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si4 C19 H19A 109.5 . . ? Si4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si4 C18 H18A 109.5 . . ? Si4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si5 C25 H25A 109.5 . . ? Si5 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si5 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O1 C29 H29A 109.5 . . ? O1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C10 O1 C29 118.4(2) . . ? C1 N1 C13 124.52(18) . . ? C1 N1 Si1 159.39(15) . . ? C13 N1 Si1 71.30(11) . . ? Si5 C30 H30A 109.5 . . ? Si5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 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 N1 Si1 C14 C15 -149.58(14) . . . . ? C13 Si1 C14 C15 149.57(14) . . . . ? C17 Si1 C14 C15 -2.96(16) . . . . ? N1 Si1 C14 Si5 -32.65(15) . . . . ? C13 Si1 C14 Si5 -93.50(15) . . . . ? C17 Si1 C14 Si5 113.97(12) . . . . ? N1 Si1 C14 Si3 95.71(12) . . . . ? C13 Si1 C14 Si3 34.86(17) . . . . ? C17 Si1 C14 Si3 -117.67(12) . . . . ? C30 Si5 C14 C15 48.7(2) . . . . ? C24 Si5 C14 C15 171.20(16) . . . . ? C25 Si5 C14 C15 -68.2(2) . . . . ? C30 Si5 C14 Si1 -63.44(17) . . . . ? C24 Si5 C14 Si1 59.03(17) . . . . ? C25 Si5 C14 Si1 179.62(15) . . . . ? C30 Si5 C14 Si3 165.30(15) . . . . ? C24 Si5 C14 Si3 -72.23(15) . . . . ? C25 Si5 C14 Si3 48.36(17) . . . . ? C23 Si3 C14 C15 155.49(18) . . . . ? C21 Si3 C14 C15 -82.40(18) . . . . ? C22 Si3 C14 C15 36.70(18) . . . . ? C23 Si3 C14 Si1 -93.18(17) . . . . ? C21 Si3 C14 Si1 28.93(17) . . . . ? C22 Si3 C14 Si1 148.03(14) . . . . ? C23 Si3 C14 Si5 37.48(17) . . . . ? C21 Si3 C14 Si5 159.60(14) . . . . ? C22 Si3 C14 Si5 -81.30(15) . . . . ? N1 Si1 C17 C16 127.07(14) . . . . ? C13 Si1 C17 C16 -173.93(13) . . . . ? C14 Si1 C17 C16 -17.62(15) . . . . ? N1 Si1 C17 Si4 12.27(17) . . . . ? C13 Si1 C17 Si4 71.28(15) . . . . ? C14 Si1 C17 Si4 -132.41(12) . . . . ? N1 Si1 C17 Si2 -114.81(12) . . . . ? C13 Si1 C17 Si2 -55.80(15) . . . . ? C14 Si1 C17 Si2 100.51(12) . . . . ? C19 Si4 C17 C16 179.19(17) . . . . ? C18 Si4 C17 C16 -60.8(2) . . . . ? C20 Si4 C17 C16 55.1(2) . . . . ? C19 Si4 C17 Si1 -71.13(17) . . . . ? C18 Si4 C17 Si1 48.89(18) . . . . ? C20 Si4 C17 Si1 164.76(16) . . . . ? C19 Si4 C17 Si2 57.33(17) . . . . ? C18 Si4 C17 Si2 177.35(15) . . . . ? C20 Si4 C17 Si2 -66.78(18) . . . . ? C27 Si2 C17 C16 149.3(2) . . . . ? C26 Si2 C17 C16 -87.7(2) . . . . ? C28 Si2 C17 C16 25.9(2) . . . . ? C27 Si2 C17 Si1 37.9(2) . . . . ? C26 Si2 C17 Si1 160.92(18) . . . . ? C28 Si2 C17 Si1 -85.53(18) . . . . ? C27 Si2 C17 Si4 -90.51(18) . . . . ? C26 Si2 C17 Si4 32.5(2) . . . . ? C28 Si2 C17 Si4 146.03(16) . . . . ? C14 Si1 C13 N1 99.18(15) . . . . ? C17 Si1 C13 N1 -112.76(13) . . . . ? N1 Si1 C13 C7 -104.3(2) . . . . ? C14 Si1 C13 C7 -5.1(3) . . . . ? C17 Si1 C13 C7 142.95(18) . . . . ? N1 C13 C7 C8 -9.8(3) . . . . ? Si1 C13 C7 C8 63.2(3) . . . . ? N1 C13 C7 C12 170.2(2) . . . . ? Si1 C13 C7 C12 -116.8(2) . . . . ? Si1 C14 C15 C16 24.5(2) . . . . ? Si5 C14 C15 C16 -96.1(2) . . . . ? Si3 C14 C15 C16 145.54(17) . . . . ? C14 C15 C16 C17 -42.0(3) . . . . ? Si1 C17 C16 C15 34.5(2) . . . . ? Si4 C17 C16 C15 153.16(17) . . . . ? Si2 C17 C16 C15 -85.2(2) . . . . ? C12 C7 C8 C9 3.6(4) . . . . ? C13 C7 C8 C9 -176.4(2) . . . . ? N1 C1 C6 C5 179.4(2) . . . . ? C2 C1 C6 C5 1.5(3) . . . . ? N1 C1 C2 C3 180.0(2) . . . . ? C6 C1 C2 C3 -2.1(4) . . . . ? C11 C10 C9 C8 -2.7(4) . . . . ? O1 C10 C9 C8 178.9(3) . . . . ? C7 C8 C9 C10 -0.5(4) . . . . ? C8 C7 C12 C11 -3.7(4) . . . . ? C13 C7 C12 C11 176.3(2) . . . . ? C1 C6 C5 C4 -0.2(4) . . . . ? C9 C10 C11 C12 2.5(4) . . . . ? O1 C10 C11 C12 -178.9(3) . . . . ? C7 C12 C11 C10 0.7(4) . . . . ? C6 C5 C4 C3 -0.7(4) . . . . ? C5 C4 C3 C2 0.1(5) . . . . ? C1 C2 C3 C4 1.3(4) . . . . ? C11 C10 O1 C29 173.6(3) . . . . ? C9 C10 O1 C29 -8.0(4) . . . . ? C6 C1 N1 C13 0.0(3) . . . . ? C2 C1 N1 C13 177.8(2) . . . . ? C6 C1 N1 Si1 136.3(4) . . . . ? C2 C1 N1 Si1 -45.9(6) . . . . ? C7 C13 N1 C1 -74.6(3) . . . . ? Si1 C13 N1 C1 165.1(2) . . . . ? C7 C13 N1 Si1 120.32(19) . . . . ? C13 Si1 N1 C1 -143.1(5) . . . . ? C14 Si1 N1 C1 97.1(5) . . . . ? C17 Si1 N1 C1 -40.9(5) . . . . ? C14 Si1 N1 C13 -119.84(13) . . . . ? C17 Si1 N1 C13 102.14(14) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.431 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.072 data_f101110d _database_code_depnum_ccdc_archive 'CCDC 875350' #TrackingRef 'web_deposit_cif_file_0_WeifengChen_1351067981.f101110d.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H51 N Si5' _chemical_formula_weight 554.16 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 9.9889(8) _cell_length_b 10.8412(8) _cell_length_c 16.4060(13) _cell_angle_alpha 81.7450(10) _cell_angle_beta 78.7950(10) _cell_angle_gamma 78.6920(10) _cell_volume 1698.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9976 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23618 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5936 _reflns_number_gt 5294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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. PART instructions for C19 C20 C21 have been applied to the trimethylsilyl group which has disorders. ISOR instruction for C15 has been used to restrain its displacement parameters and refine the atom's anisotropically. ; _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^)+(0.1214P)^2^+1.1312P] 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 5936 _refine_ls_number_parameters 359 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1554 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 0.854 _refine_ls_restrained_S_all 0.866 _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 0.28046(5) 0.86373(5) 0.25282(3) 0.03487(17) Uani 1 1 d . A . Si2 Si 0.15804(8) 1.10053(7) 0.13270(4) 0.0601(2) Uani 1 1 d . . . Si3 Si 0.37447(8) 1.12905(7) 0.24077(5) 0.0598(2) Uani 1 1 d . . . Si4 Si 0.31413(7) 0.75172(7) 0.44366(4) 0.0546(2) Uani 1 1 d . A . Si5 Si 0.04264(6) 0.74338(6) 0.37746(4) 0.04618(19) Uani 1 1 d . A . N1 N 0.29735(17) 0.75918(17) 0.18110(11) 0.0426(4) Uani 1 1 d . A . C1 C 0.2668(2) 0.70440(19) 0.11632(13) 0.0430(5) Uani 1 1 d . . . C2 C 0.3709(3) 0.6627(2) 0.05156(16) 0.0569(6) Uani 1 1 d . . . H2 H 0.4615 0.6733 0.0502 0.068 Uiso 1 1 calc R . . C3 C 0.3394(3) 0.6052(3) -0.01081(17) 0.0707(8) Uani 1 1 d . . . H3 H 0.4094 0.5786 -0.0542 0.085 Uiso 1 1 calc R . . C4 C 0.2078(4) 0.5869(3) -0.00995(19) 0.0752(8) Uani 1 1 d . . . H4 H 0.1884 0.5471 -0.0518 0.090 Uiso 1 1 calc R . . C5 C 0.1041(3) 0.6280(3) 0.05380(19) 0.0704(7) Uani 1 1 d . . . H5 H 0.0139 0.6169 0.0547 0.085 Uiso 1 1 calc R . . C6 C 0.1336(3) 0.6860(2) 0.11663(15) 0.0552(6) Uani 1 1 d . . . H6 H 0.0628 0.7128 0.1596 0.066 Uiso 1 1 calc R . . C7 C 0.5412(2) 0.6687(2) 0.21121(13) 0.0431(5) Uani 1 1 d . A . C8 C 0.5040(2) 0.5553(2) 0.24826(18) 0.0585(6) Uani 1 1 d . . . H8 H 0.4116 0.5458 0.2566 0.070 Uiso 1 1 calc R . . C9 C 0.6020(3) 0.4550(3) 0.2734(2) 0.0745(8) Uani 1 1 d . . . H9 H 0.5744 0.3799 0.2996 0.089 Uiso 1 1 calc R . . C10 C 0.7394(3) 0.4657(3) 0.2599(2) 0.0731(8) Uani 1 1 d . . . H10 H 0.8050 0.3984 0.2769 0.088 Uiso 1 1 calc R . . C11 C 0.7788(3) 0.5760(3) 0.2213(2) 0.0699(8) Uani 1 1 d . . . H11 H 0.8719 0.5834 0.2114 0.084 Uiso 1 1 calc R . . C12 C 0.6815(2) 0.6774(3) 0.19654(17) 0.0590(6) Uani 1 1 d . . . H12 H 0.7101 0.7519 0.1700 0.071 Uiso 1 1 calc R . . C13 C 0.0783(6) 1.2712(3) 0.1333(3) 0.1280(19) Uani 1 1 d . . . H13A H 0.1432 1.3223 0.1020 0.192 Uiso 1 1 calc R . . H13B H 0.0542 1.2920 0.1899 0.192 Uiso 1 1 calc R . . H13C H -0.0037 1.2872 0.1083 0.192 Uiso 1 1 calc R . . C14 C 0.0154(5) 1.0245(4) 0.1209(3) 0.1106(14) Uani 1 1 d . . . H14A H -0.0165 1.0593 0.0695 0.166 Uiso 1 1 calc R . . H14B H -0.0593 1.0393 0.1670 0.166 Uiso 1 1 calc R . . H14C H 0.0473 0.9351 0.1202 0.166 Uiso 1 1 calc R . . C15 C 0.2921(5) 1.0704(6) 0.0382(2) 0.139(2) Uani 1 1 d U . . H15A H 0.3274 0.9813 0.0393 0.209 Uiso 1 1 calc R . . H15B H 0.3664 1.1149 0.0376 0.209 Uiso 1 1 calc R . . H15C H 0.2515 1.0994 -0.0111 0.209 Uiso 1 1 calc R . . C16 C 0.3194(4) 0.5777(3) 0.4707(2) 0.0849(10) Uani 1 1 d . . . H16A H 0.3566 0.5354 0.4215 0.127 Uiso 1 1 calc R . . H16B H 0.2273 0.5613 0.4921 0.127 Uiso 1 1 calc R . . H16C H 0.3771 0.5468 0.5123 0.127 Uiso 1 1 calc R . . C17 C 0.4996(3) 0.7723(4) 0.4103(2) 0.0898(11) Uani 1 1 d . . . H17A H 0.5494 0.7404 0.4557 0.135 Uiso 1 1 calc R . . H17B H 0.5038 0.8605 0.3951 0.135 Uiso 1 1 calc R . . H17C H 0.5405 0.7264 0.3632 0.135 Uiso 1 1 calc R . . C18 C 0.2510(3) 0.8232(4) 0.54501(17) 0.0796(9) Uani 1 1 d . . . H18A H 0.1570 0.8119 0.5658 0.119 Uiso 1 1 calc R . . H18B H 0.2553 0.9119 0.5359 0.119 Uiso 1 1 calc R . . H18C H 0.3085 0.7822 0.5851 0.119 Uiso 1 1 calc R . . C19 C 0.5529(5) 1.0561(6) 0.1928(5) 0.096(2) Uani 0.672(6) 1 d P A 1 H19A H 0.6165 1.1119 0.1930 0.145 Uiso 0.672(6) 1 calc PR A 1 H19B H 0.5530 1.0423 0.1363 0.145 Uiso 0.672(6) 1 calc PR A 1 H19C H 0.5807 0.9767 0.2244 0.145 Uiso 0.672(6) 1 calc PR A 1 C20 C 0.3886(7) 1.1478(7) 0.3520(3) 0.101(2) Uani 0.672(6) 1 d P A 1 H20A H 0.4082 1.0658 0.3825 0.151 Uiso 0.672(6) 1 calc PR A 1 H20B H 0.3028 1.1934 0.3786 0.151 Uiso 0.672(6) 1 calc PR A 1 H20C H 0.4620 1.1937 0.3510 0.151 Uiso 0.672(6) 1 calc PR A 1 C21 C 0.3523(8) 1.2977(5) 0.1908(5) 0.104(2) Uani 0.672(6) 1 d P A 1 H21A H 0.2787 1.3485 0.2245 0.156 Uiso 0.672(6) 1 calc PR A 1 H21B H 0.3300 1.3009 0.1361 0.156 Uiso 0.672(6) 1 calc PR A 1 H21C H 0.4369 1.3296 0.1862 0.156 Uiso 0.672(6) 1 calc PR A 1 C19' C 0.4843(16) 1.1484(17) 0.1364(10) 0.121(6) Uani 0.328(6) 1 d P A 2 H19D H 0.5691 1.1728 0.1421 0.181 Uiso 0.328(6) 1 calc PR A 2 H19E H 0.4358 1.2126 0.1008 0.181 Uiso 0.328(6) 1 calc PR A 2 H19F H 0.5049 1.0698 0.1124 0.181 Uiso 0.328(6) 1 calc PR A 2 C20' C 0.4848(14) 1.0524(13) 0.3151(10) 0.104(5) Uani 0.328(6) 1 d P A 2 H20D H 0.5585 1.0988 0.3121 0.155 Uiso 0.328(6) 1 calc PR A 2 H20E H 0.5232 0.9676 0.3022 0.155 Uiso 0.328(6) 1 calc PR A 2 H20F H 0.4313 1.0499 0.3705 0.155 Uiso 0.328(6) 1 calc PR A 2 C21' C 0.2916(13) 1.2846(10) 0.2752(12) 0.108(5) Uani 0.328(6) 1 d P A 2 H21D H 0.2654 1.2762 0.3350 0.162 Uiso 0.328(6) 1 calc PR A 2 H21E H 0.2106 1.3158 0.2500 0.162 Uiso 0.328(6) 1 calc PR A 2 H21F H 0.3556 1.3428 0.2586 0.162 Uiso 0.328(6) 1 calc PR A 2 C22 C -0.0997(3) 0.8348(3) 0.3225(2) 0.0658(7) Uani 1 1 d . . . H22A H -0.1738 0.7874 0.3307 0.099 Uiso 1 1 calc R . . H22B H -0.0647 0.8496 0.2639 0.099 Uiso 1 1 calc R . . H22C H -0.1336 0.9144 0.3449 0.099 Uiso 1 1 calc R . . C23 C 0.0910(3) 0.5834(2) 0.33912(17) 0.0591(6) Uani 1 1 d . . . H23A H 0.0087 0.5488 0.3416 0.089 Uiso 1 1 calc R . . H23B H 0.1503 0.5285 0.3737 0.089 Uiso 1 1 calc R . . H23C H 0.1389 0.5909 0.2824 0.089 Uiso 1 1 calc R . . C24 C -0.0429(3) 0.7244(3) 0.48995(18) 0.0733(8) Uani 1 1 d . . . H24A H -0.0710 0.8060 0.5101 0.110 Uiso 1 1 calc R . . H24B H 0.0214 0.6724 0.5226 0.110 Uiso 1 1 calc R . . H24C H -0.1226 0.6852 0.4947 0.110 Uiso 1 1 calc R . . C25 C 0.2292(2) 1.04033(19) 0.23371(13) 0.0429(5) Uani 1 1 d . A . C26 C 0.1071(2) 1.0639(2) 0.30973(13) 0.0462(5) Uani 1 1 d . . . H26A H 0.0965 1.1500 0.3231 0.055 Uiso 1 1 calc R A . H26B H 0.0212 1.0537 0.2944 0.055 Uiso 1 1 calc R . . C27 C 0.1357(2) 0.9710(2) 0.38670(13) 0.0435(5) Uani 1 1 d . A . H27A H 0.0502 0.9710 0.4266 0.052 Uiso 1 1 calc R . . H27B H 0.2011 0.9999 0.4130 0.052 Uiso 1 1 calc R . . C28 C 0.1957(2) 0.83132(19) 0.36502(12) 0.0384(4) Uani 1 1 d . . . C31 C 0.4376(2) 0.78021(19) 0.18735(13) 0.0410(4) Uani 1 1 d . . . H31 H 0.4763 0.8358 0.1398 0.049 Uiso 1 1 calc R A . 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 0.0355(3) 0.0365(3) 0.0320(3) -0.0061(2) -0.0020(2) -0.0068(2) Si2 0.0758(5) 0.0551(4) 0.0400(4) 0.0036(3) -0.0077(3) 0.0022(3) Si3 0.0658(4) 0.0489(4) 0.0642(5) -0.0099(3) 0.0046(3) -0.0218(3) Si4 0.0518(4) 0.0678(4) 0.0420(4) -0.0055(3) -0.0135(3) 0.0003(3) Si5 0.0449(3) 0.0474(3) 0.0446(3) -0.0031(3) 0.0008(3) -0.0139(3) N1 0.0377(9) 0.0501(10) 0.0419(9) -0.0157(8) -0.0039(7) -0.0075(7) C1 0.0529(12) 0.0395(10) 0.0371(10) -0.0079(8) -0.0078(9) -0.0066(9) C2 0.0584(14) 0.0623(14) 0.0494(13) -0.0190(11) -0.0048(11) -0.0044(11) C3 0.084(2) 0.0795(18) 0.0479(14) -0.0284(13) -0.0063(13) -0.0009(15) C4 0.100(2) 0.0788(19) 0.0583(16) -0.0250(14) -0.0274(16) -0.0177(16) C5 0.0778(18) 0.0837(19) 0.0615(16) -0.0166(14) -0.0201(14) -0.0275(15) C6 0.0577(14) 0.0655(15) 0.0471(13) -0.0139(11) -0.0074(10) -0.0175(11) C7 0.0389(10) 0.0485(11) 0.0428(11) -0.0148(9) -0.0014(8) -0.0080(9) C8 0.0442(12) 0.0496(13) 0.0834(18) -0.0074(12) -0.0112(12) -0.0116(10) C9 0.0702(18) 0.0509(14) 0.101(2) 0.0000(14) -0.0201(16) -0.0075(12) C10 0.0563(15) 0.0755(19) 0.080(2) -0.0086(15) -0.0168(14) 0.0106(13) C11 0.0367(12) 0.097(2) 0.0745(18) -0.0144(16) -0.0084(11) -0.0046(13) C12 0.0445(12) 0.0697(16) 0.0624(15) -0.0087(12) -0.0013(11) -0.0157(11) C13 0.196(5) 0.062(2) 0.125(4) 0.006(2) -0.077(4) 0.019(3) C14 0.150(4) 0.113(3) 0.089(3) 0.016(2) -0.073(3) -0.038(3) C15 0.138(4) 0.197(5) 0.0442(18) 0.003(2) 0.007(2) 0.029(3) C16 0.094(2) 0.076(2) 0.076(2) 0.0084(16) -0.0314(17) 0.0108(17) C17 0.0556(16) 0.139(3) 0.081(2) -0.027(2) -0.0219(15) -0.0123(18) C18 0.083(2) 0.108(2) 0.0444(14) -0.0129(15) -0.0209(13) 0.0059(17) C19 0.061(3) 0.101(4) 0.132(5) -0.046(4) 0.021(3) -0.039(3) C20 0.107(4) 0.145(6) 0.074(3) -0.027(3) -0.004(3) -0.079(5) C21 0.131(5) 0.057(3) 0.135(6) 0.001(3) -0.031(5) -0.039(3) C19' 0.098(9) 0.147(13) 0.113(11) -0.003(9) 0.023(8) -0.064(10) C20' 0.098(9) 0.100(9) 0.132(12) 0.005(8) -0.050(8) -0.048(7) C21' 0.094(8) 0.063(6) 0.171(15) -0.041(8) 0.005(8) -0.032(6) C22 0.0484(13) 0.0702(17) 0.0818(19) -0.0097(14) -0.0141(13) -0.0141(12) C23 0.0673(15) 0.0479(13) 0.0636(15) -0.0047(11) -0.0064(12) -0.0196(11) C24 0.0779(19) 0.0825(19) 0.0540(15) -0.0047(14) 0.0149(13) -0.0287(15) C25 0.0498(12) 0.0373(10) 0.0371(10) -0.0033(8) 0.0003(9) -0.0048(9) C26 0.0507(12) 0.0433(11) 0.0392(11) -0.0075(9) 0.0010(9) -0.0017(9) C27 0.0478(11) 0.0465(11) 0.0337(10) -0.0088(8) 0.0010(8) -0.0069(9) C28 0.0411(10) 0.0413(10) 0.0317(9) -0.0040(8) -0.0035(8) -0.0073(8) C31 0.0383(10) 0.0436(11) 0.0420(11) -0.0107(8) -0.0001(8) -0.0117(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 Si1 N1 1.7113(17) . ? Si1 C31 1.872(2) . ? Si1 C25 1.879(2) . ? Si1 C28 1.885(2) . ? Si2 C14 1.833(4) . ? Si2 C15 1.863(4) . ? Si2 C13 1.866(4) . ? Si2 C25 1.908(2) . ? Si3 C20' 1.807(12) . ? Si3 C21' 1.842(11) . ? Si3 C19' 1.853(13) . ? Si3 C19 1.871(5) . ? Si3 C21 1.883(5) . ? Si3 C20 1.899(5) . ? Si3 C25 1.921(2) . ? Si4 C16 1.868(3) . ? Si4 C17 1.874(3) . ? Si4 C18 1.880(3) . ? Si4 C28 1.919(2) . ? Si5 C23 1.872(3) . ? Si5 C22 1.872(3) . ? Si5 C24 1.878(3) . ? Si5 C28 1.919(2) . ? N1 C1 1.398(3) . ? N1 C31 1.488(3) . ? C1 C6 1.382(3) . ? C1 C2 1.393(3) . ? C2 C3 1.385(4) . ? C2 H2 0.9300 . ? C3 C4 1.364(5) . ? C3 H3 0.9300 . ? C4 C5 1.378(4) . ? C4 H4 0.9300 . ? C5 C6 1.385(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.376(3) . ? C7 C12 1.395(3) . ? C7 C31 1.489(3) . ? C8 C9 1.386(4) . ? C8 H8 0.9300 . ? C9 C10 1.373(4) . ? C9 H9 0.9300 . ? C10 C11 1.362(4) . ? C10 H10 0.9300 . ? C11 C12 1.387(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C19' H19F 0.9600 . ? C20' H20D 0.9600 . ? C20' H20E 0.9600 . ? C20' H20F 0.9600 . ? C21' H21D 0.9600 . ? C21' H21E 0.9600 . ? C21' H21F 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.577(3) . ? C26 C27 1.534(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.579(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C31 H31 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 Si1 C31 48.80(8) . . ? N1 Si1 C25 125.69(10) . . ? C31 Si1 C25 120.10(9) . . ? N1 Si1 C28 122.22(9) . . ? C31 Si1 C28 132.70(9) . . ? C25 Si1 C28 101.53(9) . . ? C14 Si2 C15 105.1(3) . . ? C14 Si2 C13 103.6(2) . . ? C15 Si2 C13 112.3(3) . . ? C14 Si2 C25 113.42(14) . . ? C15 Si2 C25 112.10(16) . . ? C13 Si2 C25 109.92(16) . . ? C20' Si3 C21' 107.0(8) . . ? C20' Si3 C19' 108.3(8) . . ? C21' Si3 C19' 110.5(8) . . ? C20' Si3 C19 65.4(6) . . ? C21' Si3 C19 135.7(4) . . ? C19' Si3 C19 45.1(6) . . ? C20' Si3 C21 129.1(4) . . ? C21' Si3 C21 44.1(5) . . ? C19' Si3 C21 67.2(6) . . ? C19 Si3 C21 104.5(3) . . ? C20' Si3 C20 43.9(5) . . ? C21' Si3 C20 65.5(6) . . ? C19' Si3 C20 135.9(5) . . ? C19 Si3 C20 104.9(3) . . ? C21 Si3 C20 102.3(3) . . ? C20' Si3 C25 114.4(4) . . ? C21' Si3 C25 107.4(4) . . ? C19' Si3 C25 109.2(5) . . ? C19 Si3 C25 115.41(17) . . ? C21 Si3 C25 114.5(2) . . ? C20 Si3 C25 113.76(17) . . ? C16 Si4 C17 105.43(18) . . ? C16 Si4 C18 105.77(17) . . ? C17 Si4 C18 106.36(16) . . ? C16 Si4 C28 115.21(13) . . ? C17 Si4 C28 114.30(14) . . ? C18 Si4 C28 109.08(11) . . ? C23 Si5 C22 107.24(13) . . ? C23 Si5 C24 108.41(13) . . ? C22 Si5 C24 103.69(15) . . ? C23 Si5 C28 113.93(11) . . ? C22 Si5 C28 112.53(11) . . ? C24 Si5 C28 110.45(12) . . ? C1 N1 C31 124.85(17) . . ? C1 N1 Si1 158.69(16) . . ? C31 N1 Si1 71.24(10) . . ? C6 C1 C2 118.4(2) . . ? C6 C1 N1 120.9(2) . . ? C2 C1 N1 120.7(2) . . ? C3 C2 C1 119.9(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.1(2) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 120.9(2) . . ? C1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C12 117.7(2) . . ? C8 C7 C31 122.41(19) . . ? C12 C7 C31 119.8(2) . . ? C7 C8 C9 121.1(2) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 120.5(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 119.3(3) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 120.8(2) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C7 120.6(2) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si4 C16 H16A 109.5 . . ? Si4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si4 C17 H17A 109.5 . . ? Si4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si4 C18 H18A 109.5 . . ? Si4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? Si3 C19' H19D 109.5 . . ? Si3 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? Si3 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? Si3 C20' H20D 109.5 . . ? Si3 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? Si3 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? Si3 C21' H21D 109.5 . . ? Si3 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? Si3 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? Si5 C22 H22A 109.5 . . ? Si5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si5 C23 H23A 109.5 . . ? Si5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si5 C24 H24A 109.5 . . ? Si5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 Si1 100.13(13) . . ? C26 C25 Si2 108.37(15) . . ? Si1 C25 Si2 115.15(11) . . ? C26 C25 Si3 110.01(15) . . ? Si1 C25 Si3 112.79(11) . . ? Si2 C25 Si3 109.86(10) . . ? C27 C26 C25 110.83(17) . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C26 C27 C28 113.05(16) . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27B 109.0 . . ? C28 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 Si1 100.24(13) . . ? C27 C28 Si5 107.88(13) . . ? Si1 C28 Si5 113.22(10) . . ? C27 C28 Si4 107.99(13) . . ? Si1 C28 Si4 117.23(11) . . ? Si5 C28 Si4 109.41(10) . . ? N1 C31 C7 118.30(17) . . ? N1 C31 Si1 59.95(10) . . ? C7 C31 Si1 129.73(16) . . ? N1 C31 H31 112.6 . . ? C7 C31 H31 112.6 . . ? Si1 C31 H31 112.6 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.343 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.060 data_f120112a _database_code_depnum_ccdc_archive 'CCDC 875352' #TrackingRef 'web_deposit_cif_file_0_WeifengChen_1351068294.f120112a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H49 F6 N Si5' _chemical_formula_weight 690.16 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' F F 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 22.667(4) _cell_length_b 14.110(2) _cell_length_c 23.682(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7574(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4193 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 23.58 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6557 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25486 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7395 _reflns_number_gt 4486 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. Due to the disorder of the CF3 group, PART instructions have been applied. A number of DELU, SIMU, ISOR instructions have been used in order to refine respective atoms anisotropically. They were used as following: DELU C31 F2' F1' F1 F2 F3 ISOR 0.1 F6' ; _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^)+(0.0627P)^2^+5.0045P] 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 7395 _refine_ls_number_parameters 447 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1012 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1509 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.11430(4) 0.25266(6) 0.12049(3) 0.0438(2) Uani 1 1 d . . . Si2 Si 0.12465(5) 0.37963(7) 0.00750(4) 0.0609(3) Uani 1 1 d . . . Si3 Si 0.22379(5) 0.23517(7) 0.03765(4) 0.0642(3) Uani 1 1 d . . . Si4 Si 0.18032(5) 0.21033(7) 0.25027(4) 0.0612(3) Uani 1 1 d . . . Si5 Si 0.06847(5) 0.10253(7) 0.10801(5) 0.0700(3) Uani 1 1 d . . . N1 N 0.06354(10) 0.33317(16) 0.15101(9) 0.0416(6) Uani 1 1 d . . . C1 C 0.16319(14) 0.3140(2) 0.06743(12) 0.0479(7) Uani 1 1 d . . . C2 C 0.19094(14) 0.3900(2) 0.10810(12) 0.0474(7) Uani 1 1 d . . . H2A H 0.2271 0.4142 0.0915 0.057 Uiso 1 1 calc R . . H2B H 0.1638 0.4427 0.1121 0.057 Uiso 1 1 calc R . . C3 C 0.20444(14) 0.3494(2) 0.16607(13) 0.0506(8) Uani 1 1 d . . . H3A H 0.2115 0.4011 0.1922 0.061 Uiso 1 1 calc R . . H3B H 0.2403 0.3120 0.1639 0.061 Uiso 1 1 calc R . . C4 C 0.15406(13) 0.28678(19) 0.18916(12) 0.0438(7) Uani 1 1 d . . . C5 C 0.08184(17) 0.4837(3) 0.03339(15) 0.0692(10) Uani 1 1 d . . . H5A H 0.0617 0.5129 0.0023 0.104 Uiso 1 1 calc R . . H5B H 0.1083 0.5287 0.0503 0.104 Uiso 1 1 calc R . . H5C H 0.0535 0.4631 0.0609 0.104 Uiso 1 1 calc R . . C6 C 0.0725(2) 0.3048(3) -0.03378(16) 0.0891(13) Uani 1 1 d . . . H6A H 0.0428 0.2797 -0.0090 0.134 Uiso 1 1 calc R . . H6B H 0.0937 0.2535 -0.0511 0.134 Uiso 1 1 calc R . . H6C H 0.0541 0.3426 -0.0625 0.134 Uiso 1 1 calc R . . F3 F 0.12168(16) 0.76747(19) 0.18502(14) 0.1380(12) Uani 1 1 d U A . C7 C 0.1791(2) 0.4307(3) -0.04310(16) 0.0890(13) Uani 1 1 d . . . H7A H 0.1589 0.4694 -0.0702 0.134 Uiso 1 1 calc R . . H7B H 0.1994 0.3803 -0.0622 0.134 Uiso 1 1 calc R . . H7C H 0.2071 0.4687 -0.0229 0.134 Uiso 1 1 calc R . . C8 C 0.1993(2) 0.1695(3) -0.0265(2) 0.1131(17) Uani 1 1 d . . . H8A H 0.1934 0.2134 -0.0570 0.170 Uiso 1 1 calc R . . H8B H 0.1629 0.1372 -0.0186 0.170 Uiso 1 1 calc R . . H8C H 0.2289 0.1242 -0.0370 0.170 Uiso 1 1 calc R . . C9 C 0.29147(19) 0.3049(3) 0.0199(2) 0.0963(14) Uani 1 1 d . . . H9A H 0.3184 0.2656 -0.0009 0.144 Uiso 1 1 calc R . . H9B H 0.3100 0.3262 0.0540 0.144 Uiso 1 1 calc R . . H9C H 0.2807 0.3587 -0.0027 0.144 Uiso 1 1 calc R . . C10 C 0.2504(2) 0.1449(3) 0.08882(19) 0.0902(13) Uani 1 1 d . . . H10A H 0.2173 0.1117 0.1045 0.135 Uiso 1 1 calc R . . H10B H 0.2719 0.1757 0.1186 0.135 Uiso 1 1 calc R . . H10C H 0.2758 0.1008 0.0698 0.135 Uiso 1 1 calc R . . C11 C 0.12084(19) 0.1829(3) 0.30121(16) 0.0861(13) Uani 1 1 d . . . H11A H 0.0885 0.1534 0.2818 0.129 Uiso 1 1 calc R . . H11B H 0.1075 0.2404 0.3187 0.129 Uiso 1 1 calc R . . H11C H 0.1356 0.1406 0.3297 0.129 Uiso 1 1 calc R . . C12 C 0.2121(2) 0.0931(3) 0.22921(19) 0.0945(14) Uani 1 1 d . . . H12A H 0.2201 0.0562 0.2624 0.142 Uiso 1 1 calc R . . H12B H 0.2481 0.1029 0.2087 0.142 Uiso 1 1 calc R . . H12C H 0.1844 0.0599 0.2057 0.142 Uiso 1 1 calc R . . C13 C 0.23925(19) 0.2756(3) 0.28949(18) 0.0922(14) Uani 1 1 d . . . H13A H 0.2242 0.3357 0.3019 0.138 Uiso 1 1 calc R . . H13B H 0.2725 0.2857 0.2650 0.138 Uiso 1 1 calc R . . H13C H 0.2514 0.2390 0.3216 0.138 Uiso 1 1 calc R . . C14 C 0.0290(2) 0.0824(3) 0.1747(2) 0.1016(15) Uani 1 1 d . . . H14A H 0.0065 0.0248 0.1721 0.152 Uiso 1 1 calc R . . H14B H 0.0028 0.1346 0.1819 0.152 Uiso 1 1 calc R . . H14C H 0.0569 0.0772 0.2050 0.152 Uiso 1 1 calc R . . C15 C 0.0129(3) 0.1002(4) 0.0501(2) 0.125(2) Uani 1 1 d . . . H15A H -0.0057 0.0391 0.0490 0.187 Uiso 1 1 calc R . . H15B H 0.0321 0.1121 0.0147 0.187 Uiso 1 1 calc R . . H15C H -0.0163 0.1482 0.0568 0.187 Uiso 1 1 calc R . . C16 C 0.1186(2) 0.0001(3) 0.0954(3) 0.138(2) Uani 1 1 d . . . H16A H 0.1491 -0.0004 0.1235 0.207 Uiso 1 1 calc R . . H16B H 0.1361 0.0057 0.0586 0.207 Uiso 1 1 calc R . . H16C H 0.0965 -0.0578 0.0975 0.207 Uiso 1 1 calc R . . C17 C 0.00292(13) 0.3485(2) 0.14863(13) 0.0455(7) Uani 1 1 d . . . C18 C -0.02952(14) 0.3817(2) 0.19406(14) 0.0534(8) Uani 1 1 d . . . H18 H -0.0106 0.3956 0.2279 0.064 Uiso 1 1 calc R . . C19 C -0.08935(17) 0.3943(3) 0.18963(18) 0.0708(11) Uani 1 1 d . . . H19 H -0.1102 0.4166 0.2208 0.085 Uiso 1 1 calc R . . C20 C -0.11906(18) 0.3752(3) 0.1412(2) 0.0777(12) Uani 1 1 d . . . H20 H -0.1597 0.3836 0.1391 0.093 Uiso 1 1 calc R . . C21 C -0.08771(18) 0.3433(3) 0.09568(19) 0.0779(12) Uani 1 1 d . . . H21 H -0.1074 0.3300 0.0621 0.094 Uiso 1 1 calc R . . C22 C -0.02743(16) 0.3305(3) 0.09859(15) 0.0636(9) Uani 1 1 d . . . H22 H -0.0069 0.3098 0.0669 0.076 Uiso 1 1 calc R . . C23 C 0.09580(13) 0.34360(19) 0.20411(12) 0.0426(7) Uani 1 1 d . . . H23 H 0.0745 0.3080 0.2332 0.051 Uiso 1 1 calc R . . C24 C 0.10396(13) 0.4441(2) 0.22518(12) 0.0433(7) Uani 1 1 d . . . C25 C 0.12370(13) 0.4586(2) 0.27963(12) 0.0467(7) Uani 1 1 d . . . H25 H 0.1317 0.4065 0.3024 0.056 Uiso 1 1 calc R . . C26 C 0.13179(14) 0.5489(2) 0.30098(12) 0.0488(7) Uani 1 1 d . B . C27 C 0.11980(14) 0.6273(2) 0.26847(13) 0.0501(7) Uani 1 1 d . . . H27 H 0.1254 0.6880 0.2827 0.060 Uiso 1 1 calc R . . C28 C 0.09923(14) 0.6135(2) 0.21402(13) 0.0470(7) Uani 1 1 d . A . C29 C 0.09153(13) 0.5229(2) 0.19241(12) 0.0452(7) Uani 1 1 d . . . H29 H 0.0779 0.5150 0.1557 0.054 Uiso 1 1 calc R . . C30 C 0.1547(2) 0.5597(3) 0.35994(15) 0.0695(10) Uani 1 1 d . . . C31 C 0.08425(19) 0.6973(2) 0.17837(16) 0.0631(9) Uani 1 1 d U . . F1 F 0.0990(13) 0.6848(15) 0.1265(7) 0.118(5) Uani 0.41(3) 1 d PU A 1 F2 F 0.0304(6) 0.720(2) 0.1793(15) 0.137(8) Uani 0.41(3) 1 d PU A 1 F1' F 0.0748(10) 0.6783(8) 0.1262(5) 0.120(5) Uani 0.59(3) 1 d PU A 2 F2' F 0.0383(7) 0.7428(10) 0.1974(6) 0.116(3) Uani 0.59(3) 1 d PU A 2 F4 F 0.1494(8) 0.6451(7) 0.3795(4) 0.133(5) Uani 0.79(3) 1 d P B 1 F5 F 0.1256(4) 0.5034(7) 0.3947(3) 0.101(2) Uani 0.79(3) 1 d P B 1 F6 F 0.2093(3) 0.5330(11) 0.3638(5) 0.128(4) Uani 0.79(3) 1 d P B 1 F4' F 0.180(2) 0.635(2) 0.3706(13) 0.099(13) Uani 0.21(3) 1 d P B 2 F5' F 0.1144(14) 0.557(6) 0.3989(10) 0.134(17) Uani 0.21(3) 1 d P B 2 F6' F 0.190(3) 0.496(3) 0.3757(18) 0.14(2) Uani 0.21(3) 1 d PU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0514(5) 0.0351(4) 0.0450(4) -0.0061(3) 0.0062(4) -0.0036(4) Si2 0.0732(7) 0.0654(6) 0.0442(5) 0.0024(4) 0.0056(5) -0.0043(5) Si3 0.0694(6) 0.0556(6) 0.0676(6) -0.0135(5) 0.0217(5) 0.0012(5) Si4 0.0716(7) 0.0553(6) 0.0568(5) 0.0066(4) -0.0056(5) 0.0151(5) Si5 0.0805(7) 0.0470(6) 0.0827(7) -0.0172(5) 0.0154(6) -0.0200(5) N1 0.0416(14) 0.0434(14) 0.0399(12) -0.0060(10) -0.0028(11) -0.0006(11) C1 0.0553(19) 0.0424(17) 0.0459(16) -0.0067(13) 0.0085(14) -0.0031(14) C2 0.0497(18) 0.0393(16) 0.0531(17) -0.0024(13) 0.0081(15) -0.0063(14) C3 0.0504(18) 0.0427(17) 0.0586(19) -0.0065(14) -0.0005(15) 0.0016(14) C4 0.0483(17) 0.0350(15) 0.0480(16) -0.0022(13) 0.0029(14) 0.0038(13) C5 0.079(3) 0.071(2) 0.057(2) 0.0108(18) -0.0018(19) 0.007(2) C6 0.099(3) 0.112(4) 0.056(2) -0.014(2) -0.005(2) -0.008(3) F3 0.185(3) 0.0732(18) 0.156(3) 0.0423(17) -0.045(2) -0.0426(19) C7 0.106(3) 0.094(3) 0.067(2) 0.021(2) 0.023(2) 0.000(3) C8 0.149(5) 0.097(4) 0.093(3) -0.047(3) 0.012(3) 0.014(3) C9 0.077(3) 0.098(3) 0.114(4) 0.000(3) 0.042(3) 0.001(2) C10 0.090(3) 0.064(3) 0.116(3) 0.003(2) 0.024(3) 0.020(2) C11 0.102(3) 0.093(3) 0.063(2) 0.026(2) 0.008(2) 0.014(3) C12 0.121(4) 0.066(3) 0.097(3) 0.011(2) -0.008(3) 0.039(3) C13 0.087(3) 0.102(3) 0.088(3) -0.008(2) -0.033(3) 0.026(2) C14 0.096(3) 0.100(3) 0.109(4) 0.004(3) 0.020(3) -0.043(3) C15 0.163(5) 0.102(4) 0.109(4) -0.031(3) -0.021(4) -0.063(4) C16 0.127(4) 0.049(3) 0.239(7) -0.034(4) 0.048(5) -0.012(3) C17 0.0482(18) 0.0361(16) 0.0521(17) 0.0055(13) -0.0026(15) -0.0030(13) C18 0.0492(19) 0.0510(19) 0.0600(19) 0.0034(15) 0.0048(16) 0.0034(15) C19 0.061(2) 0.060(2) 0.091(3) 0.020(2) 0.017(2) 0.0088(18) C20 0.050(2) 0.077(3) 0.106(3) 0.036(2) 0.001(2) 0.0007(19) C21 0.062(3) 0.088(3) 0.085(3) 0.022(2) -0.024(2) -0.018(2) C22 0.060(2) 0.071(2) 0.059(2) 0.0039(17) -0.0025(18) -0.0129(18) C23 0.0512(17) 0.0366(16) 0.0399(15) 0.0001(12) 0.0010(13) 0.0023(13) C24 0.0450(17) 0.0432(17) 0.0416(15) -0.0044(13) 0.0009(13) 0.0031(13) C25 0.0519(18) 0.0441(17) 0.0443(16) -0.0018(13) -0.0020(14) 0.0085(14) C26 0.0517(19) 0.0484(19) 0.0463(16) -0.0078(14) -0.0030(14) 0.0007(14) C27 0.0539(19) 0.0429(18) 0.0536(17) -0.0112(14) 0.0019(15) -0.0021(14) C28 0.0514(18) 0.0396(17) 0.0498(17) -0.0041(14) 0.0051(14) 0.0048(14) C29 0.0497(18) 0.0432(17) 0.0427(16) -0.0058(13) -0.0002(14) 0.0044(14) C30 0.088(3) 0.069(3) 0.052(2) -0.011(2) -0.009(2) 0.003(2) C31 0.084(3) 0.041(2) 0.065(2) -0.0046(17) 0.002(2) 0.0021(18) F1 0.200(15) 0.089(7) 0.065(6) 0.035(5) 0.054(8) 0.042(7) F2 0.074(5) 0.158(16) 0.178(19) 0.089(12) 0.019(7) 0.047(6) F1' 0.242(14) 0.054(4) 0.064(5) -0.005(4) -0.058(6) 0.029(6) F2' 0.163(7) 0.083(4) 0.103(5) 0.008(4) 0.013(5) 0.077(4) F4 0.245(12) 0.080(4) 0.075(4) -0.040(3) -0.049(6) 0.032(7) F5 0.147(6) 0.111(5) 0.046(3) 0.000(3) -0.010(3) -0.014(4) F6 0.082(4) 0.212(13) 0.090(4) -0.034(6) -0.040(3) 0.017(5) F4' 0.17(3) 0.07(2) 0.055(11) 0.004(12) -0.047(14) -0.07(2) F5' 0.087(14) 0.25(5) 0.066(10) -0.054(19) 0.032(9) -0.06(2) F6' 0.23(5) 0.098(19) 0.09(2) -0.020(13) -0.09(3) 0.08(2) _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 N1 1.771(2) . ? Si1 C1 1.886(3) . ? Si1 C4 1.921(3) . ? Si1 Si5 2.3778(13) . ? Si2 C6 1.862(4) . ? Si2 C5 1.864(4) . ? Si2 C7 1.865(4) . ? Si2 C1 1.907(3) . ? Si3 C10 1.859(4) . ? Si3 C8 1.864(4) . ? Si3 C9 1.871(4) . ? Si3 C1 1.903(3) . ? Si4 C11 1.850(4) . ? Si4 C13 1.870(4) . ? Si4 C12 1.872(4) . ? Si4 C4 1.901(3) . ? Si5 C14 1.838(4) . ? Si5 C15 1.862(5) . ? Si5 C16 1.863(5) . ? N1 C17 1.392(4) . ? N1 C23 1.462(3) . ? C1 C2 1.573(4) . ? C2 C3 1.519(4) . ? C3 C4 1.544(4) . ? C4 C23 1.585(4) . ? F3 C31 1.313(4) . ? C17 C18 1.385(4) . ? C17 C22 1.393(4) . ? C18 C19 1.372(5) . ? C19 C20 1.356(5) . ? C20 C21 1.368(6) . ? C21 C22 1.380(5) . ? C23 C24 1.515(4) . ? C24 C25 1.380(4) . ? C24 C29 1.385(4) . ? C25 C26 1.383(4) . ? C26 C27 1.375(4) . ? C26 C30 1.497(5) . ? C27 C28 1.385(4) . ? C28 C29 1.388(4) . ? C28 C31 1.492(4) . ? C30 F4' 1.23(2) . ? C30 F6' 1.25(3) . ? C30 F4 1.297(9) . ? C30 F5' 1.30(2) . ? C30 F6 1.298(9) . ? C30 F5 1.320(8) . ? C31 F2 1.262(15) . ? C31 F1' 1.281(10) . ? C31 F1 1.284(14) . ? C31 F2' 1.304(12) . ? 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 Si1 C1 111.07(12) . . ? N1 Si1 C4 78.38(11) . . ? C1 Si1 C4 99.99(13) . . ? N1 Si1 Si5 109.78(9) . . ? C1 Si1 Si5 125.63(10) . . ? C4 Si1 Si5 122.25(10) . . ? C6 Si2 C5 106.8(2) . . ? C6 Si2 C7 107.6(2) . . ? C5 Si2 C7 104.57(18) . . ? C6 Si2 C1 113.96(17) . . ? C5 Si2 C1 112.11(14) . . ? C7 Si2 C1 111.26(18) . . ? C10 Si3 C8 106.7(2) . . ? C10 Si3 C9 103.9(2) . . ? C8 Si3 C9 108.8(2) . . ? C10 Si3 C1 113.16(16) . . ? C8 Si3 C1 112.2(2) . . ? C9 Si3 C1 111.60(17) . . ? C11 Si4 C13 107.4(2) . . ? C11 Si4 C12 105.6(2) . . ? C13 Si4 C12 107.0(2) . . ? C11 Si4 C4 112.78(16) . . ? C13 Si4 C4 108.80(17) . . ? C12 Si4 C4 114.79(17) . . ? C14 Si5 C15 107.5(2) . . ? C14 Si5 C16 108.4(3) . . ? C15 Si5 C16 106.3(3) . . ? C14 Si5 Si1 104.12(15) . . ? C15 Si5 Si1 113.75(16) . . ? C16 Si5 Si1 116.40(17) . . ? C17 N1 C23 120.9(2) . . ? C17 N1 Si1 136.4(2) . . ? C23 N1 Si1 95.20(16) . . ? C2 C1 Si1 98.05(18) . . ? C2 C1 Si3 109.7(2) . . ? Si1 C1 Si3 113.79(16) . . ? C2 C1 Si2 107.89(19) . . ? Si1 C1 Si2 116.72(17) . . ? Si3 C1 Si2 109.80(15) . . ? C3 C2 C1 112.1(2) . . ? C2 C3 C4 112.8(2) . . ? C3 C4 C23 113.9(2) . . ? C3 C4 Si4 111.3(2) . . ? C23 C4 Si4 112.21(19) . . ? C3 C4 Si1 101.00(19) . . ? C23 C4 Si1 85.69(17) . . ? Si4 C4 Si1 130.49(16) . . ? C18 C17 N1 123.0(3) . . ? C18 C17 C22 117.4(3) . . ? N1 C17 C22 119.6(3) . . ? C19 C18 C17 120.6(3) . . ? C20 C19 C18 122.0(4) . . ? C19 C20 C21 118.3(4) . . ? C20 C21 C22 121.2(4) . . ? C21 C22 C17 120.5(4) . . ? N1 C23 C24 116.0(2) . . ? N1 C23 C4 100.0(2) . . ? C24 C23 C4 116.5(2) . . ? C25 C24 C29 118.1(3) . . ? C25 C24 C23 119.1(3) . . ? C29 C24 C23 122.8(3) . . ? C24 C25 C26 121.4(3) . . ? C27 C26 C25 120.7(3) . . ? C27 C26 C30 120.6(3) . . ? C25 C26 C30 118.7(3) . . ? C26 C27 C28 118.4(3) . . ? C27 C28 C29 121.0(3) . . ? C27 C28 C31 119.5(3) . . ? C29 C28 C31 119.5(3) . . ? C24 C29 C28 120.5(3) . . ? F4' C30 F6' 105(2) . . ? F4' C30 F4 34(2) . . ? F6' C30 F4 127.9(19) . . ? F4' C30 F5' 102.0(18) . . ? F6' C30 F5' 102(2) . . ? F4 C30 F5' 73(3) . . ? F4' C30 F6 78(2) . . ? F6' C30 F6 33(3) . . ? F4 C30 F6 109.4(7) . . ? F5' C30 F6 128(2) . . ? F4' C30 F5 128.4(15) . . ? F6' C30 F5 73(3) . . ? F4 C30 F5 106.9(6) . . ? F5' C30 F5 36(3) . . ? F6 C30 F5 105.0(7) . . ? F4' C30 C26 116.1(13) . . ? F6' C30 C26 115.2(18) . . ? F4 C30 C26 113.3(6) . . ? F5' C30 C26 114.6(12) . . ? F6 C30 C26 111.5(6) . . ? F5 C30 C26 110.3(5) . . ? F2 C31 F1' 84.6(14) . . ? F2 C31 F1 107.7(14) . . ? F1' C31 F1 25.1(13) . . ? F2 C31 F2' 25.4(17) . . ? F1' C31 F2' 107.6(10) . . ? F1 C31 F2' 127.3(12) . . ? F2 C31 F3 115.7(15) . . ? F1' C31 F3 112.4(9) . . ? F1 C31 F3 92.9(13) . . ? F2' C31 F3 96.0(8) . . ? F2 C31 C28 114.2(10) . . ? F1' C31 C28 114.7(6) . . ? F1 C31 C28 111.9(10) . . ? F2' C31 C28 112.1(7) . . ? F3 C31 C28 112.5(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.277 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.045 data_f120301a _database_code_depnum_ccdc_archive 'CCDC 875388' #TrackingRef 'f120301a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H50 Cl N Si5' _chemical_formula_weight 588.60 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1571(11) _cell_length_b 15.9991(13) _cell_length_c 17.0546(14) _cell_angle_alpha 72.259(2) _cell_angle_beta 84.025(2) _cell_angle_gamma 89.806(2) _cell_volume 3399.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8775 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 26.23 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9134 _exptl_absorpt_correction_T_max 0.9411 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36538 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.50 _reflns_number_total 12553 _reflns_number_gt 8283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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^)+(0.1000P)^2^+0.6555P] 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 12553 _refine_ls_number_parameters 673 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.006 _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 0.28072(6) 0.03035(5) 0.29155(4) 0.03103(18) Uani 1 1 d . . . Si2 Si 0.26148(7) 0.24337(5) 0.23700(5) 0.0474(2) Uani 1 1 d . . . Si3 Si 0.45541(7) 0.15949(6) 0.17620(5) 0.0507(2) Uani 1 1 d . . . Si4 Si 0.38010(7) -0.14232(5) 0.40372(5) 0.0449(2) Uani 1 1 d . . . Si5 Si 0.22843(6) -0.03638(6) 0.48551(5) 0.0428(2) Uani 1 1 d . . . Cl1 Cl -0.16414(8) 0.21642(7) 0.08521(6) 0.0781(3) Uani 1 1 d . . . N1 N 0.25673(17) -0.01831(15) 0.21895(14) 0.0385(6) Uani 1 1 d . . . C1 C 0.3292(2) -0.02815(18) 0.39388(16) 0.0341(6) Uani 1 1 d . . . C2 C 0.4175(2) 0.03836(19) 0.39216(17) 0.0396(7) Uani 1 1 d . . . H2A H 0.4301 0.0332 0.4485 0.047 Uiso 1 1 calc R . . H2B H 0.4797 0.0237 0.3640 0.047 Uiso 1 1 calc R . . C3 C 0.3910(2) 0.13302(19) 0.34803(17) 0.0425(7) Uani 1 1 d . . . H3A H 0.4521 0.1704 0.3368 0.051 Uiso 1 1 calc R . . H3B H 0.3416 0.1533 0.3840 0.051 Uiso 1 1 calc R . . C4 C 0.3456(2) 0.14113(18) 0.26410(16) 0.0375(6) Uani 1 1 d . . . C5 C 0.1575(2) -0.00766(18) 0.26504(16) 0.0360(6) Uani 1 1 d . . . H5 H 0.1304 -0.0629 0.3053 0.043 Uiso 1 1 calc R . . C6 C 0.0776(2) 0.04388(18) 0.21787(16) 0.0359(6) Uani 1 1 d . . . C7 C 0.0969(2) 0.0945(2) 0.13530(18) 0.0439(7) Uani 1 1 d . . . H7 H 0.1610 0.0932 0.1071 0.053 Uiso 1 1 calc R . . C8 C 0.0234(2) 0.1465(2) 0.09441(19) 0.0496(8) Uani 1 1 d . . . H8 H 0.0381 0.1802 0.0393 0.060 Uiso 1 1 calc R . . C9 C -0.0718(2) 0.1484(2) 0.13521(19) 0.0502(8) Uani 1 1 d . . . C10 C -0.0954(3) 0.0960(3) 0.2155(2) 0.0605(9) Uani 1 1 d . . . H10 H -0.1607 0.0952 0.2424 0.073 Uiso 1 1 calc R . . C11 C -0.0198(2) 0.0439(2) 0.25614(19) 0.0534(8) Uani 1 1 d . . . H11 H -0.0356 0.0084 0.3105 0.064 Uiso 1 1 calc R . . C12 C 0.2735(2) -0.07700(18) 0.17328(16) 0.0387(7) Uani 1 1 d . . . C13 C 0.3719(3) -0.0921(2) 0.1443(2) 0.0567(9) Uani 1 1 d . . . H13 H 0.4270 -0.0628 0.1553 0.068 Uiso 1 1 calc R . . C14 C 0.3891(3) -0.1500(3) 0.0995(2) 0.0770(12) Uani 1 1 d . . . H14 H 0.4556 -0.1601 0.0808 0.092 Uiso 1 1 calc R . . C15 C 0.3085(4) -0.1930(3) 0.0821(2) 0.0822(13) Uani 1 1 d . . . H15 H 0.3201 -0.2320 0.0516 0.099 Uiso 1 1 calc R . . C16 C 0.2111(3) -0.1781(2) 0.1098(2) 0.0656(10) Uani 1 1 d . . . H16 H 0.1565 -0.2069 0.0976 0.079 Uiso 1 1 calc R . . C17 C 0.1928(3) -0.1205(2) 0.15575(18) 0.0491(8) Uani 1 1 d . . . H17 H 0.1261 -0.1113 0.1747 0.059 Uiso 1 1 calc R . . C18 C 0.5016(3) -0.1398(3) 0.3360(2) 0.0705(11) Uani 1 1 d . . . H18A H 0.5529 -0.1059 0.3500 0.106 Uiso 1 1 calc R . . H18B H 0.4902 -0.1136 0.2791 0.106 Uiso 1 1 calc R . . H18C H 0.5243 -0.1986 0.3440 0.106 Uiso 1 1 calc R . . C19 C 0.2891(3) -0.2156(2) 0.3757(2) 0.0651(10) Uani 1 1 d . . . H19A H 0.2831 -0.1942 0.3174 0.098 Uiso 1 1 calc R . . H19B H 0.2233 -0.2162 0.4060 0.098 Uiso 1 1 calc R . . H19C H 0.3143 -0.2742 0.3894 0.098 Uiso 1 1 calc R . . C20 C 0.4142(3) -0.1977(2) 0.5107(2) 0.0639(10) Uani 1 1 d . . . H20A H 0.4465 -0.2520 0.5123 0.096 Uiso 1 1 calc R . . H20B H 0.3533 -0.2093 0.5491 0.096 Uiso 1 1 calc R . . H20C H 0.4603 -0.1602 0.5257 0.096 Uiso 1 1 calc R . . C21 C 0.1400(3) 0.0575(2) 0.4699(2) 0.0650(10) Uani 1 1 d . . . H21A H 0.1034 0.0612 0.4232 0.097 Uiso 1 1 calc R . . H21B H 0.1788 0.1111 0.4600 0.097 Uiso 1 1 calc R . . H21C H 0.0923 0.0484 0.5186 0.097 Uiso 1 1 calc R . . C22 C 0.1410(3) -0.1347(2) 0.5116(2) 0.0678(10) Uani 1 1 d . . . H22A H 0.1803 -0.1869 0.5240 0.102 Uiso 1 1 calc R . . H22B H 0.1038 -0.1318 0.4654 0.102 Uiso 1 1 calc R . . H22C H 0.0938 -0.1361 0.5589 0.102 Uiso 1 1 calc R . . C23 C 0.2913(3) -0.0371(3) 0.5791(2) 0.0723(11) Uani 1 1 d . . . H23A H 0.2399 -0.0408 0.6244 0.108 Uiso 1 1 calc R . . H23B H 0.3319 0.0159 0.5673 0.108 Uiso 1 1 calc R . . H23C H 0.3344 -0.0869 0.5936 0.108 Uiso 1 1 calc R . . C24 C 0.3167(3) 0.3301(2) 0.2749(2) 0.0754(11) Uani 1 1 d . . . H24A H 0.2768 0.3819 0.2598 0.113 Uiso 1 1 calc R . . H24B H 0.3859 0.3441 0.2502 0.113 Uiso 1 1 calc R . . H24C H 0.3155 0.3088 0.3341 0.113 Uiso 1 1 calc R . . C25 C 0.2494(3) 0.2924(2) 0.1241(2) 0.0709(11) Uani 1 1 d . . . H25A H 0.2220 0.2489 0.1032 0.106 Uiso 1 1 calc R . . H25B H 0.3156 0.3125 0.0950 0.106 Uiso 1 1 calc R . . H25C H 0.2046 0.3410 0.1160 0.106 Uiso 1 1 calc R . . C26 C 0.1274(3) 0.2244(2) 0.2872(2) 0.0663(10) Uani 1 1 d . . . H26A H 0.0870 0.2731 0.2612 0.099 Uiso 1 1 calc R . . H26B H 0.1265 0.2190 0.3449 0.099 Uiso 1 1 calc R . . H26C H 0.0996 0.1715 0.2815 0.099 Uiso 1 1 calc R . . C27 C 0.5164(3) 0.2718(3) 0.1513(3) 0.0808(13) Uani 1 1 d . . . H27A H 0.5475 0.2763 0.1983 0.121 Uiso 1 1 calc R . . H27B H 0.4652 0.3153 0.1380 0.121 Uiso 1 1 calc R . . H27C H 0.5676 0.2811 0.1048 0.121 Uiso 1 1 calc R . . C28 C 0.4126(3) 0.1458(3) 0.0798(2) 0.0659(10) Uani 1 1 d . . . H28A H 0.4665 0.1213 0.0522 0.099 Uiso 1 1 calc R . . H28B H 0.3959 0.2019 0.0439 0.099 Uiso 1 1 calc R . . H28C H 0.3534 0.1071 0.0939 0.099 Uiso 1 1 calc R . . C29 C 0.5649(3) 0.0852(3) 0.2040(3) 0.0798(12) Uani 1 1 d . . . H29A H 0.6176 0.0989 0.1583 0.120 Uiso 1 1 calc R . . H29B H 0.5417 0.0253 0.2165 0.120 Uiso 1 1 calc R . . H29C H 0.5915 0.0934 0.2516 0.120 Uiso 1 1 calc R . . C30 C 0.1506(2) 0.48827(17) 0.74132(16) 0.0366(6) Uani 1 1 d . . . C31 C 0.1072(2) 0.53436(18) 0.65625(17) 0.0413(7) Uani 1 1 d . . . H31A H 0.0459 0.5650 0.6663 0.050 Uiso 1 1 calc R . . H31B H 0.1573 0.5775 0.6208 0.050 Uiso 1 1 calc R . . C32 C 0.0820(2) 0.46825(19) 0.61181(18) 0.0401(7) Uani 1 1 d . . . H32A H 0.0710 0.4996 0.5551 0.048 Uiso 1 1 calc R . . H32B H 0.0192 0.4360 0.6390 0.048 Uiso 1 1 calc R . . C33 C 0.17022(19) 0.40208(17) 0.61211(16) 0.0321(6) Uani 1 1 d . . . C34 C 0.3384(2) 0.33793(18) 0.74450(17) 0.0391(7) Uani 1 1 d . . . H34 H 0.3671 0.3085 0.7048 0.047 Uiso 1 1 calc R . . C35 C 0.4170(2) 0.36032(18) 0.79190(18) 0.0407(7) Uani 1 1 d . . . C36 C 0.5163(2) 0.3812(2) 0.7557(2) 0.0540(8) Uani 1 1 d . . . H36 H 0.5342 0.3774 0.7027 0.065 Uiso 1 1 calc R . . C37 C 0.5904(3) 0.4076(3) 0.7965(2) 0.0635(10) Uani 1 1 d . . . H37 H 0.6566 0.4222 0.7710 0.076 Uiso 1 1 calc R . . C38 C 0.5636(3) 0.4119(2) 0.8753(2) 0.0572(9) Uani 1 1 d . . . C39 C 0.4671(3) 0.3897(2) 0.91354(19) 0.0558(9) Uani 1 1 d . . . H39 H 0.4503 0.3921 0.9671 0.067 Uiso 1 1 calc R . . C40 C 0.3940(2) 0.3634(2) 0.87225(18) 0.0477(8) Uani 1 1 d . . . H40 H 0.3285 0.3475 0.8989 0.057 Uiso 1 1 calc R . . C41 C 0.2229(2) 0.20993(18) 0.83600(17) 0.0413(7) Uani 1 1 d . . . C42 C 0.3049(3) 0.1566(2) 0.8586(2) 0.0595(9) Uani 1 1 d . . . H42 H 0.3716 0.1788 0.8418 0.071 Uiso 1 1 calc R . . C43 C 0.2864(4) 0.0694(2) 0.9067(2) 0.0779(12) Uani 1 1 d . . . H43 H 0.3414 0.0339 0.9228 0.093 Uiso 1 1 calc R . . C44 C 0.1893(4) 0.0350(2) 0.9306(2) 0.0842(14) Uani 1 1 d . . . H44 H 0.1787 -0.0237 0.9617 0.101 Uiso 1 1 calc R . . C45 C 0.1082(4) 0.0865(2) 0.9091(2) 0.0745(12) Uani 1 1 d . . . H45 H 0.0419 0.0633 0.9254 0.089 Uiso 1 1 calc R . . C46 C 0.1247(3) 0.1748(2) 0.8621(2) 0.0558(9) Uani 1 1 d . . . H46 H 0.0691 0.2103 0.8482 0.067 Uiso 1 1 calc R . . C47 C 0.3688(3) 0.5839(2) 0.7198(2) 0.0675(10) Uani 1 1 d . . . H47A H 0.4088 0.6154 0.7461 0.101 Uiso 1 1 calc R . . H47B H 0.3710 0.6155 0.6619 0.101 Uiso 1 1 calc R . . H47C H 0.3961 0.5267 0.7264 0.101 Uiso 1 1 calc R . . C48 C 0.2434(3) 0.5506(3) 0.8814(2) 0.0714(11) Uani 1 1 d . . . H48A H 0.2701 0.4934 0.9040 0.107 Uiso 1 1 calc R . . H48B H 0.1768 0.5533 0.9092 0.107 Uiso 1 1 calc R . . H48C H 0.2882 0.5941 0.8891 0.107 Uiso 1 1 calc R . . C49 C 0.1805(3) 0.6842(2) 0.7281(2) 0.0750(12) Uani 1 1 d . . . H49A H 0.2210 0.7262 0.7423 0.112 Uiso 1 1 calc R . . H49B H 0.1113 0.6837 0.7525 0.112 Uiso 1 1 calc R . . H49C H 0.1818 0.7001 0.6690 0.112 Uiso 1 1 calc R . . C50 C -0.0710(3) 0.4003(3) 0.7968(3) 0.0833(13) Uani 1 1 d . . . H50A H -0.0489 0.3485 0.7836 0.125 Uiso 1 1 calc R . . H50B H -0.0958 0.4410 0.7492 0.125 Uiso 1 1 calc R . . H50C H -0.1248 0.3848 0.8418 0.125 Uiso 1 1 calc R . . C51 C 0.0767(3) 0.3730(2) 0.9251(2) 0.0687(11) Uani 1 1 d . . . H51A H 0.0173 0.3533 0.9642 0.103 Uiso 1 1 calc R . . H51B H 0.1243 0.4017 0.9482 0.103 Uiso 1 1 calc R . . H51C H 0.1083 0.3235 0.9129 0.103 Uiso 1 1 calc R . . C52 C -0.0215(3) 0.5479(3) 0.8535(3) 0.0830(13) Uani 1 1 d . . . H52A H -0.0408 0.5896 0.8040 0.124 Uiso 1 1 calc R . . H52B H 0.0266 0.5753 0.8774 0.124 Uiso 1 1 calc R . . H52C H -0.0811 0.5281 0.8925 0.124 Uiso 1 1 calc R . . C53 C -0.0046(3) 0.2562(2) 0.6673(2) 0.0677(10) Uani 1 1 d . . . H53A H -0.0256 0.2010 0.6619 0.102 Uiso 1 1 calc R . . H53B H -0.0558 0.2988 0.6494 0.102 Uiso 1 1 calc R . . H53C H 0.0039 0.2492 0.7241 0.102 Uiso 1 1 calc R . . C54 C 0.0870(3) 0.3086(2) 0.4942(2) 0.0637(10) Uani 1 1 d . . . H54A H 0.1487 0.3209 0.4568 0.096 Uiso 1 1 calc R . . H54B H 0.0415 0.3564 0.4782 0.096 Uiso 1 1 calc R . . H54C H 0.0546 0.2556 0.4925 0.096 Uiso 1 1 calc R . . C55 C 0.2077(3) 0.2019(2) 0.6319(2) 0.0641(10) Uani 1 1 d . . . H55A H 0.2143 0.1869 0.6901 0.096 Uiso 1 1 calc R . . H55B H 0.2736 0.2191 0.6011 0.096 Uiso 1 1 calc R . . H55C H 0.1811 0.1518 0.6199 0.096 Uiso 1 1 calc R . . C56 C 0.2120(3) 0.5111(3) 0.4261(2) 0.0701(11) Uani 1 1 d . . . H56A H 0.2640 0.5303 0.3800 0.105 Uiso 1 1 calc R . . H56B H 0.1774 0.5611 0.4345 0.105 Uiso 1 1 calc R . . H56C H 0.1638 0.4725 0.4148 0.105 Uiso 1 1 calc R . . C57 C 0.3586(3) 0.3682(3) 0.4971(2) 0.0657(10) Uani 1 1 d . . . H57A H 0.3197 0.3271 0.4805 0.099 Uiso 1 1 calc R . . H57B H 0.3908 0.3377 0.5453 0.099 Uiso 1 1 calc R . . H57C H 0.4101 0.3970 0.4529 0.099 Uiso 1 1 calc R . . C58 C 0.3603(3) 0.5342(3) 0.5366(2) 0.0689(10) Uani 1 1 d . . . H58A H 0.4045 0.5598 0.4864 0.103 Uiso 1 1 calc R . . H58B H 0.4008 0.5063 0.5805 0.103 Uiso 1 1 calc R . . H58C H 0.3213 0.5794 0.5507 0.103 Uiso 1 1 calc R . . Cl2 Cl 0.65571(9) 0.44506(9) 0.92722(7) 0.0944(4) Uani 1 1 d . . . N2 N 0.23918(17) 0.29790(14) 0.78883(14) 0.0388(5) Uani 1 1 d . . . Si6 Si 0.21574(6) 0.39348(5) 0.71544(4) 0.03084(18) Uani 1 1 d . . . Si7 Si 0.23413(8) 0.57229(5) 0.76818(5) 0.0488(2) Uani 1 1 d . . . Si8 Si 0.03849(7) 0.45196(6) 0.82765(5) 0.0499(2) Uani 1 1 d . . . Si9 Si 0.11872(6) 0.29458(5) 0.60213(5) 0.0428(2) Uani 1 1 d . . . Si10 Si 0.27222(6) 0.45145(6) 0.52117(5) 0.0410(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 Si1 0.0325(4) 0.0323(4) 0.0293(4) -0.0110(3) -0.0035(3) -0.0005(3) Si2 0.0658(6) 0.0332(4) 0.0427(5) -0.0096(4) -0.0093(4) 0.0009(4) Si3 0.0515(5) 0.0561(6) 0.0406(5) -0.0127(4) 0.0064(4) -0.0163(4) Si4 0.0471(5) 0.0382(5) 0.0494(5) -0.0111(4) -0.0133(4) 0.0109(4) Si5 0.0374(5) 0.0523(5) 0.0342(4) -0.0074(4) -0.0014(3) 0.0036(4) Cl1 0.0730(6) 0.0973(8) 0.0682(6) -0.0246(6) -0.0298(5) 0.0349(6) N1 0.0354(13) 0.0442(14) 0.0419(14) -0.0221(11) -0.0033(11) -0.0003(10) C1 0.0323(14) 0.0375(15) 0.0323(14) -0.0092(12) -0.0070(11) 0.0022(12) C2 0.0354(15) 0.0477(17) 0.0351(15) -0.0101(13) -0.0092(12) -0.0019(13) C3 0.0479(17) 0.0417(17) 0.0400(16) -0.0142(13) -0.0081(14) -0.0070(13) C4 0.0439(16) 0.0372(15) 0.0321(15) -0.0122(12) -0.0019(12) -0.0050(13) C5 0.0361(15) 0.0411(16) 0.0313(14) -0.0125(12) -0.0011(12) -0.0030(12) C6 0.0375(15) 0.0397(16) 0.0334(15) -0.0148(13) -0.0057(12) -0.0025(12) C7 0.0418(17) 0.0493(18) 0.0394(17) -0.0136(14) 0.0011(13) 0.0018(14) C8 0.058(2) 0.0532(19) 0.0344(16) -0.0085(14) -0.0035(15) 0.0041(16) C9 0.054(2) 0.058(2) 0.0452(18) -0.0210(16) -0.0180(16) 0.0111(16) C10 0.0427(19) 0.089(3) 0.046(2) -0.0154(19) -0.0047(15) 0.0110(18) C11 0.0426(18) 0.076(2) 0.0352(17) -0.0083(16) -0.0010(14) -0.0016(16) C12 0.0517(18) 0.0373(16) 0.0303(14) -0.0144(12) -0.0067(13) 0.0028(13) C13 0.055(2) 0.076(2) 0.0486(19) -0.0329(18) -0.0065(16) 0.0132(18) C14 0.089(3) 0.099(3) 0.059(2) -0.045(2) -0.016(2) 0.043(3) C15 0.127(4) 0.077(3) 0.068(3) -0.052(2) -0.033(3) 0.039(3) C16 0.104(3) 0.048(2) 0.055(2) -0.0255(17) -0.023(2) -0.001(2) C17 0.064(2) 0.0443(18) 0.0424(17) -0.0178(14) -0.0061(15) -0.0032(15) C18 0.067(2) 0.068(2) 0.075(3) -0.021(2) -0.005(2) 0.028(2) C19 0.085(3) 0.044(2) 0.069(2) -0.0165(18) -0.023(2) 0.0013(18) C20 0.076(2) 0.053(2) 0.059(2) -0.0080(17) -0.0237(19) 0.0223(18) C21 0.059(2) 0.075(3) 0.058(2) -0.0216(19) 0.0060(18) 0.0117(19) C22 0.053(2) 0.071(2) 0.062(2) 0.0014(19) 0.0062(18) -0.0083(18) C23 0.066(2) 0.114(3) 0.0385(19) -0.024(2) -0.0117(17) 0.012(2) C24 0.106(3) 0.049(2) 0.079(3) -0.029(2) -0.018(2) -0.003(2) C25 0.097(3) 0.057(2) 0.049(2) -0.0022(17) -0.009(2) 0.007(2) C26 0.070(2) 0.054(2) 0.071(2) -0.0136(19) -0.007(2) 0.0196(18) C27 0.083(3) 0.083(3) 0.071(3) -0.019(2) 0.008(2) -0.042(2) C28 0.076(3) 0.078(3) 0.0417(19) -0.0215(18) 0.0106(18) -0.016(2) C29 0.053(2) 0.104(3) 0.077(3) -0.028(2) 0.016(2) -0.002(2) C30 0.0468(17) 0.0287(14) 0.0334(15) -0.0078(12) -0.0053(12) 0.0045(12) C31 0.0494(18) 0.0334(15) 0.0400(16) -0.0081(13) -0.0095(14) 0.0129(13) C32 0.0389(16) 0.0461(17) 0.0363(15) -0.0118(13) -0.0113(12) 0.0082(13) C33 0.0306(14) 0.0373(15) 0.0321(14) -0.0142(12) -0.0080(11) 0.0015(11) C34 0.0425(16) 0.0382(16) 0.0363(16) -0.0096(13) -0.0088(13) 0.0045(13) C35 0.0427(17) 0.0370(16) 0.0399(16) -0.0068(13) -0.0088(13) 0.0031(13) C36 0.0455(19) 0.071(2) 0.0467(19) -0.0194(17) -0.0049(15) 0.0021(16) C37 0.046(2) 0.085(3) 0.056(2) -0.0155(19) -0.0088(17) -0.0094(18) C38 0.058(2) 0.060(2) 0.054(2) -0.0116(17) -0.0227(17) -0.0073(17) C39 0.066(2) 0.067(2) 0.0350(17) -0.0133(16) -0.0124(16) -0.0056(18) C40 0.0450(18) 0.0539(19) 0.0416(17) -0.0089(15) -0.0093(14) -0.0012(15) C41 0.062(2) 0.0276(14) 0.0349(15) -0.0090(12) -0.0101(14) 0.0040(14) C42 0.083(3) 0.0393(18) 0.056(2) -0.0111(16) -0.0186(19) 0.0148(17) C43 0.122(4) 0.039(2) 0.072(3) -0.0099(19) -0.030(3) 0.028(2) C44 0.150(5) 0.033(2) 0.060(2) 0.0003(18) -0.012(3) -0.001(3) C45 0.109(3) 0.049(2) 0.056(2) -0.0059(18) 0.006(2) -0.022(2) C46 0.070(2) 0.0418(18) 0.0492(19) -0.0059(15) -0.0029(17) -0.0045(16) C47 0.076(3) 0.063(2) 0.072(2) -0.030(2) -0.017(2) -0.0181(19) C48 0.106(3) 0.066(2) 0.051(2) -0.0255(19) -0.024(2) 0.002(2) C49 0.120(3) 0.0361(19) 0.070(3) -0.0157(18) -0.020(2) 0.007(2) C50 0.062(2) 0.102(3) 0.083(3) -0.033(3) 0.022(2) -0.013(2) C51 0.095(3) 0.052(2) 0.046(2) -0.0017(16) 0.0109(19) 0.0098(19) C52 0.094(3) 0.069(3) 0.082(3) -0.025(2) 0.015(2) 0.032(2) C53 0.067(2) 0.062(2) 0.075(3) -0.023(2) -0.004(2) -0.0211(19) C54 0.070(2) 0.071(2) 0.061(2) -0.0315(19) -0.0227(19) -0.0081(19) C55 0.082(3) 0.046(2) 0.075(2) -0.0293(18) -0.024(2) 0.0097(18) C56 0.072(3) 0.082(3) 0.044(2) 0.0010(18) -0.0096(18) -0.002(2) C57 0.052(2) 0.078(3) 0.068(2) -0.027(2) 0.0051(18) 0.0027(18) C58 0.055(2) 0.076(3) 0.075(3) -0.025(2) 0.0068(19) -0.0229(19) Cl2 0.0865(8) 0.1218(10) 0.0823(7) -0.0334(7) -0.0346(6) -0.0288(7) N2 0.0406(13) 0.0307(12) 0.0429(14) -0.0059(11) -0.0117(11) 0.0022(10) Si6 0.0352(4) 0.0264(4) 0.0310(4) -0.0075(3) -0.0077(3) 0.0020(3) Si7 0.0758(6) 0.0315(4) 0.0430(5) -0.0144(4) -0.0144(4) 0.0011(4) Si8 0.0603(6) 0.0430(5) 0.0431(5) -0.0117(4) 0.0053(4) 0.0094(4) Si9 0.0450(5) 0.0410(5) 0.0477(5) -0.0195(4) -0.0112(4) -0.0038(4) Si10 0.0394(5) 0.0476(5) 0.0358(4) -0.0122(4) -0.0044(3) -0.0026(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.705(2) . ? Si1 C4 1.874(3) . ? Si1 C5 1.878(3) . ? Si1 C1 1.887(3) . ? Si2 C26 1.862(4) . ? Si2 C25 1.869(4) . ? Si2 C24 1.877(3) . ? Si2 C4 1.936(3) . ? Si3 C28 1.865(3) . ? Si3 C29 1.871(4) . ? Si3 C27 1.878(4) . ? Si3 C4 1.925(3) . ? Si4 C18 1.866(4) . ? Si4 C20 1.871(3) . ? Si4 C19 1.873(3) . ? Si4 C1 1.908(3) . ? Si5 C22 1.865(3) . ? Si5 C21 1.868(4) . ? Si5 C23 1.869(3) . ? Si5 C1 1.913(3) . ? Cl1 C9 1.741(3) . ? N1 C12 1.395(3) . ? N1 C5 1.489(3) . ? C1 C2 1.571(4) . ? C2 C3 1.529(4) . ? C3 C4 1.577(4) . ? C5 C6 1.483(4) . ? C6 C11 1.376(4) . ? C6 C7 1.391(4) . ? C7 C8 1.377(4) . ? C8 C9 1.372(4) . ? C9 C10 1.374(4) . ? C10 C11 1.396(5) . ? C12 C17 1.379(4) . ? C12 C13 1.385(4) . ? C13 C14 1.375(5) . ? C14 C15 1.371(6) . ? C15 C16 1.363(6) . ? C16 C17 1.386(4) . ? C30 C31 1.579(4) . ? C30 Si6 1.884(3) . ? C30 Si7 1.927(3) . ? C30 Si8 1.927(3) . ? C31 C32 1.532(4) . ? C32 C33 1.568(4) . ? C33 Si6 1.885(3) . ? C33 Si9 1.912(3) . ? C33 Si10 1.912(3) . ? C34 N2 1.480(4) . ? C34 C35 1.484(4) . ? C34 Si6 1.879(3) . ? C35 C36 1.382(4) . ? C35 C40 1.388(4) . ? C36 C37 1.391(4) . ? C37 C38 1.375(5) . ? C38 C39 1.362(5) . ? C38 Cl2 1.746(3) . ? C39 C40 1.386(4) . ? C41 C46 1.384(4) . ? C41 C42 1.386(4) . ? C41 N2 1.396(3) . ? C42 C43 1.394(5) . ? C43 C44 1.364(6) . ? C44 C45 1.359(6) . ? C45 C46 1.400(5) . ? C47 Si7 1.860(4) . ? C48 Si7 1.872(3) . ? C49 Si7 1.876(4) . ? C50 Si8 1.862(4) . ? C51 Si8 1.871(4) . ? C52 Si8 1.873(3) . ? C53 Si9 1.860(3) . ? C54 Si9 1.875(3) . ? C55 Si9 1.866(3) . ? C56 Si10 1.867(4) . ? C57 Si10 1.860(4) . ? C58 Si10 1.858(3) . ? N2 Si6 1.706(2) . ? 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 Si1 C4 122.69(12) . . ? N1 Si1 C5 48.80(11) . . ? C4 Si1 C5 132.55(13) . . ? N1 Si1 C1 124.75(12) . . ? C4 Si1 C1 101.92(12) . . ? C5 Si1 C1 119.93(12) . . ? C26 Si2 C25 104.84(18) . . ? C26 Si2 C24 105.06(18) . . ? C25 Si2 C24 108.05(18) . . ? C26 Si2 C4 114.72(14) . . ? C25 Si2 C4 114.56(15) . . ? C24 Si2 C4 109.02(16) . . ? C28 Si3 C29 107.35(19) . . ? C28 Si3 C27 108.92(18) . . ? C29 Si3 C27 102.9(2) . . ? C28 Si3 C4 112.56(14) . . ? C29 Si3 C4 113.72(15) . . ? C27 Si3 C4 110.84(16) . . ? C18 Si4 C20 104.05(17) . . ? C18 Si4 C19 105.68(18) . . ? C20 Si4 C19 109.01(17) . . ? C18 Si4 C1 112.92(15) . . ? C20 Si4 C1 111.26(14) . . ? C19 Si4 C1 113.36(14) . . ? C22 Si5 C21 103.83(17) . . ? C22 Si5 C23 109.19(18) . . ? C21 Si5 C23 104.69(18) . . ? C22 Si5 C1 113.46(15) . . ? C21 Si5 C1 114.76(14) . . ? C23 Si5 C1 110.34(14) . . ? C12 N1 C5 125.2(2) . . ? C12 N1 Si1 155.4(2) . . ? C5 N1 Si1 71.66(14) . . ? C2 C1 Si1 99.25(17) . . ? C2 C1 Si4 111.24(18) . . ? Si1 C1 Si4 115.27(14) . . ? C2 C1 Si5 110.07(18) . . ? Si1 C1 Si5 112.06(13) . . ? Si4 C1 Si5 108.66(13) . . ? C3 C2 C1 111.6(2) . . ? C2 C3 C4 111.6(2) . . ? C3 C4 Si1 99.80(17) . . ? C3 C4 Si3 109.45(19) . . ? Si1 C4 Si3 113.01(14) . . ? C3 C4 Si2 108.99(18) . . ? Si1 C4 Si2 117.94(15) . . ? Si3 C4 Si2 107.23(14) . . ? C6 C5 N1 118.6(2) . . ? C6 C5 Si1 129.9(2) . . ? N1 C5 Si1 59.54(12) . . ? C11 C6 C7 117.5(3) . . ? C11 C6 C5 120.0(3) . . ? C7 C6 C5 122.6(3) . . ? C8 C7 C6 121.5(3) . . ? C9 C8 C7 119.8(3) . . ? C8 C9 C10 120.4(3) . . ? C8 C9 Cl1 120.2(3) . . ? C10 C9 Cl1 119.4(3) . . ? C9 C10 C11 119.0(3) . . ? C6 C11 C10 121.7(3) . . ? C17 C12 C13 118.8(3) . . ? C17 C12 N1 120.8(3) . . ? C13 C12 N1 120.3(3) . . ? C14 C13 C12 120.7(3) . . ? C15 C14 C13 120.2(4) . . ? C16 C15 C14 119.7(3) . . ? C15 C16 C17 120.8(4) . . ? C12 C17 C16 119.9(3) . . ? C31 C30 Si6 99.57(17) . . ? C31 C30 Si7 108.90(18) . . ? Si6 C30 Si7 117.99(15) . . ? C31 C30 Si8 109.20(19) . . ? Si6 C30 Si8 113.19(14) . . ? Si7 C30 Si8 107.49(13) . . ? C32 C31 C30 111.9(2) . . ? C31 C32 C33 111.4(2) . . ? C32 C33 Si6 99.58(17) . . ? C32 C33 Si9 110.70(17) . . ? Si6 C33 Si9 115.00(14) . . ? C32 C33 Si10 110.04(19) . . ? Si6 C33 Si10 112.82(13) . . ? Si9 C33 Si10 108.43(13) . . ? N2 C34 C35 119.3(2) . . ? N2 C34 Si6 59.65(13) . . ? C35 C34 Si6 129.5(2) . . ? C36 C35 C40 117.6(3) . . ? C36 C35 C34 120.3(3) . . ? C40 C35 C34 122.2(3) . . ? C35 C36 C37 121.8(3) . . ? C38 C37 C36 118.7(3) . . ? C39 C38 C37 121.1(3) . . ? C39 C38 Cl2 119.7(3) . . ? C37 C38 Cl2 119.2(3) . . ? C38 C39 C40 119.7(3) . . ? C39 C40 C35 121.2(3) . . ? C46 C41 C42 118.9(3) . . ? C46 C41 N2 120.7(3) . . ? C42 C41 N2 120.5(3) . . ? C41 C42 C43 119.3(4) . . ? C44 C43 C42 121.4(4) . . ? C45 C44 C43 120.0(4) . . ? C44 C45 C46 119.7(4) . . ? C41 C46 C45 120.8(4) . . ? C41 N2 C34 125.1(2) . . ? C41 N2 Si6 156.1(2) . . ? C34 N2 Si6 71.86(14) . . ? N2 Si6 C34 48.49(11) . . ? N2 Si6 C30 122.98(12) . . ? C34 Si6 C30 131.85(13) . . ? N2 Si6 C33 125.30(12) . . ? C34 Si6 C33 120.34(12) . . ? C30 Si6 C33 101.79(12) . . ? C47 Si7 C48 105.00(18) . . ? C47 Si7 C49 104.92(19) . . ? C48 Si7 C49 107.39(17) . . ? C47 Si7 C30 114.82(14) . . ? C48 Si7 C30 114.95(15) . . ? C49 Si7 C30 109.07(16) . . ? C50 Si8 C51 107.4(2) . . ? C50 Si8 C52 102.4(2) . . ? C51 Si8 C52 108.35(18) . . ? C50 Si8 C30 113.33(15) . . ? C51 Si8 C30 112.92(15) . . ? C52 Si8 C30 111.77(16) . . ? C53 Si9 C55 106.19(17) . . ? C53 Si9 C54 103.63(17) . . ? C55 Si9 C54 108.88(17) . . ? C53 Si9 C33 112.76(14) . . ? C55 Si9 C33 113.48(14) . . ? C54 Si9 C33 111.29(14) . . ? C58 Si10 C57 104.14(18) . . ? C58 Si10 C56 104.61(18) . . ? C57 Si10 C56 108.73(18) . . ? C58 Si10 C33 114.81(14) . . ? C57 Si10 C33 113.15(15) . . ? C56 Si10 C33 110.80(14) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.434 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.050