# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1475 loop_ _publ_author_name 'Ying Shu.' 'Yee-Fun Lim.' 'Zhong Li.' 'Purushothaman, Balaji' 'Hallani, Rawad' 'Jo Kim.' 'Parkin, Sean' 'Malliaras, George' 'Anthony, John E.' _publ_contact_author_name 'Anthony, John E.' _publ_contact_author_email anthony@uky.edu _publ_section_title ; A Survey of Electron-Deficient Pentacenes as Acceptors in Polymer Bulk Heterojunction Solar Cells ; # Attachment 'CF3_TCPS.cif' data_x09043 _database_code_depnum_ccdc_archive 'CCDC 796836' #TrackingRef 'CF3_TCPS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H65 F3 Si2' _chemical_formula_sum 'C57 H65 F3 Si2' _chemical_formula_weight 863.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7922(3) _cell_length_b 17.7744(4) _cell_length_c 18.0925(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.265(1) _cell_angle_gamma 90.00 _cell_volume 4707.52(18) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 9992 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 68.51 _exptl_crystal_description slab _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details 'Sadabs in APEX2 (BrukerAXS, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator 'graded multilayer optics' _diffrn_measurement_device_type 'Bruker X8 Proteum diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 63671 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 68.57 _reflns_number_total 8531 _reflns_number_gt 6588 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 2008)' _computing_publication_material ; SHELX-97 (Sheldrick, 2008) and local procedures ; _publ_section_exptl_refinement ; H atoms were found in difference Fourier maps and subsequently placed in idealized positions with constrained distances of 0.99 \%A (R~2~CH~2~), 0.95 \%A (C~Ar~H), and with U~iso~(H) values set to 1.2U~eq~ of the attached atom. ; _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^ > 2\s(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. To ensure similarity of the major and minor components of disorder, the following restraints (all of which are SHELXL97 commands) were employed. SAME - restrains similar groups to be approximately the same. DELU - a "rigid bond" restraint that ensures that the components of displacement parameters of connected atoms do not change appreciably along a bonded chain. ; _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^)+(0.0803P)^2^+12.0540P] 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 8531 _refine_ls_number_parameters 583 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.1048 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2250 _refine_ls_wR_factor_gt 0.2001 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.059 _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 0.25055(7) 1.03686(6) 0.74792(6) 0.0381(3) Uani 1 1 d . C . C1 C 0.2291(2) 0.7885(2) 0.70766(19) 0.0324(7) Uani 1 1 d . . . C2 C 0.2590(2) 0.7552(2) 0.64428(19) 0.0327(7) Uani 1 1 d . . . C3 C 0.2924(2) 0.7991(2) 0.5894(2) 0.0342(8) Uani 1 1 d . . . H3 H 0.2937 0.8523 0.5944 0.041 Uiso 1 1 calc R . . C4 C 0.3236(2) 0.7663(2) 0.5282(2) 0.0360(8) Uani 1 1 d . . . C5 C 0.3620(3) 0.8111(2) 0.4740(2) 0.0400(8) Uani 1 1 d . . . H5 H 0.3646 0.8643 0.4790 0.048 Uiso 1 1 calc R . . C6 C 0.3943(3) 0.7771(2) 0.4159(2) 0.0401(9) Uani 1 1 d . . . C7 C 0.3893(3) 0.6977(2) 0.4059(2) 0.0417(9) Uani 1 1 d . . . H7 H 0.4117 0.6752 0.3645 0.050 Uiso 1 1 calc R . . C8 C 0.3527(2) 0.6541(2) 0.4553(2) 0.0380(8) Uani 1 1 d . . . H8 H 0.3488 0.6012 0.4478 0.046 Uiso 1 1 calc R . . C9 C 0.3197(2) 0.6866(2) 0.5187(2) 0.0354(8) Uani 1 1 d . . . C10 C 0.2861(2) 0.6427(2) 0.57185(19) 0.0337(8) Uani 1 1 d . . . H10 H 0.2825 0.5897 0.5651 0.040 Uiso 1 1 calc R . . C11 C 0.2571(2) 0.6748(2) 0.63574(19) 0.0318(7) Uani 1 1 d . . . C12 C 0.2291(2) 0.6292(2) 0.6926(2) 0.0333(8) Uani 1 1 d . . . C13 C 0.1982(2) 0.6629(2) 0.75561(19) 0.0332(8) Uani 1 1 d . . . C14 C 0.1710(3) 0.6186(2) 0.8131(2) 0.0373(8) Uani 1 1 d . . . H14 H 0.1733 0.5653 0.8093 0.045 Uiso 1 1 calc R . . C15 C 0.1410(3) 0.6507(2) 0.8753(2) 0.0383(8) Uani 1 1 d . . . C16 C 0.1168(3) 0.6059(2) 0.9355(2) 0.0469(10) Uani 1 1 d . . . H16 H 0.1206 0.5527 0.9330 0.056 Uiso 1 1 calc R . . C17 C 0.0884(3) 0.6388(3) 0.9960(2) 0.0477(10) Uani 1 1 d . . . H17 H 0.0748 0.6084 1.0361 0.057 Uiso 1 1 calc R . . C18 C 0.0790(3) 0.7177(3) 0.9999(2) 0.0467(10) Uani 1 1 d . . . H18 H 0.0568 0.7397 1.0417 0.056 Uiso 1 1 calc R . . C19 C 0.1014(3) 0.7626(2) 0.9445(2) 0.0406(9) Uani 1 1 d . . . H19 H 0.0946 0.8156 0.9479 0.049 Uiso 1 1 calc R . . C20 C 0.1353(2) 0.7307(2) 0.88101(19) 0.0357(8) Uani 1 1 d . . . C21 C 0.1639(2) 0.7747(2) 0.82565(19) 0.0338(8) Uani 1 1 d . . . H21 H 0.1616 0.8279 0.8300 0.041 Uiso 1 1 calc R . . C22 C 0.1963(2) 0.7432(2) 0.76302(18) 0.0308(7) Uani 1 1 d . . . C23 C 0.2340(2) 0.8681(2) 0.71812(19) 0.0323(7) Uani 1 1 d . . . C24 C 0.2401(2) 0.9343(2) 0.7290(2) 0.0380(8) Uani 1 1 d . . . C25 C 0.1699(3) 1.0589(2) 0.8162(2) 0.0423(9) Uani 1 1 d . . . H25 H 0.1823 1.1118 0.8336 0.051 Uiso 1 1 calc R . . C26 C 0.1801(3) 1.0080(2) 0.8867(2) 0.0464(9) Uani 1 1 d . . . H26A H 0.2108 0.9602 0.8772 0.056 Uiso 1 1 calc R . . H26B H 0.2165 1.0338 0.9295 0.056 Uiso 1 1 calc R . . C27 C 0.0819(3) 0.9927(3) 0.9033(3) 0.0687(14) Uani 1 1 d . . . H27A H 0.0640 0.9400 0.8911 0.082 Uiso 1 1 calc R . . H27B H 0.0779 1.0018 0.9567 0.082 Uiso 1 1 calc R . . C28 C 0.0209(3) 1.0462(3) 0.8549(3) 0.0602(12) Uani 1 1 d . . . H28A H 0.0175 1.0955 0.8799 0.072 Uiso 1 1 calc R . . H28B H -0.0415 1.0255 0.8424 0.072 Uiso 1 1 calc R . . C29 C 0.0676(3) 1.0536(3) 0.7852(3) 0.0517(10) Uani 1 1 d . . . H29A H 0.0466 1.0993 0.7565 0.062 Uiso 1 1 calc R . . H29B H 0.0550 1.0091 0.7524 0.062 Uiso 1 1 calc R . . C30 C 0.2236(3) 1.0853(2) 0.6554(2) 0.0478(9) Uani 1 1 d DU . . H30 H 0.2333 1.1407 0.6627 0.057 Uiso 1 1 calc R A 1 C31 C 0.1283(3) 1.0718(3) 0.6112(2) 0.0553(11) Uani 1 1 d DU C . H31A H 0.1098 1.0185 0.6144 0.066 Uiso 1 1 calc R B 1 H31B H 0.0820 1.1041 0.6298 0.066 Uiso 1 1 calc R B 1 C32 C 0.1404(6) 1.0929(5) 0.5310(4) 0.0540(12) Uani 0.674(9) 1 d PDU C 1 H32A H 0.1021 1.0601 0.4949 0.065 Uiso 0.674(9) 1 calc PR C 1 H32B H 0.1220 1.1458 0.5206 0.065 Uiso 0.674(9) 1 calc PR C 1 C33 C 0.2410(5) 1.0823(4) 0.5241(4) 0.0540(12) Uani 0.674(9) 1 d PDU C 1 H33A H 0.2681 1.1304 0.5103 0.065 Uiso 0.674(9) 1 calc PR C 1 H33B H 0.2484 1.0444 0.4854 0.065 Uiso 0.674(9) 1 calc PR C 1 C34 C 0.2874(5) 1.0558(6) 0.6004(4) 0.0540(12) Uani 0.674(9) 1 d PDU C 1 H34A H 0.3494 1.0775 0.6122 0.065 Uiso 0.674(9) 1 calc PR C 1 H34B H 0.2919 1.0003 0.6022 0.065 Uiso 0.674(9) 1 calc PR C 1 C32' C 0.1371(11) 1.0757(11) 0.5298(7) 0.0540(12) Uani 0.326(9) 1 d PDU C 2 H32C H 0.1391 1.1283 0.5121 0.065 Uiso 0.326(9) 1 calc PR C 2 H32D H 0.0871 1.0483 0.4987 0.065 Uiso 0.326(9) 1 calc PR C 2 C33' C 0.2301(9) 1.0355(9) 0.5311(7) 0.0540(12) Uani 0.326(9) 1 d PDU C 2 H33C H 0.2239 0.9805 0.5370 0.065 Uiso 0.326(9) 1 calc PR C 2 H33D H 0.2566 1.0457 0.4848 0.065 Uiso 0.326(9) 1 calc PR C 2 C34' C 0.2880(10) 1.0699(14) 0.5985(8) 0.0540(12) Uani 0.326(9) 1 d PDU C 2 H34C H 0.3165 1.1173 0.5846 0.065 Uiso 0.326(9) 1 calc PR C 2 H34D H 0.3369 1.0347 0.6194 0.065 Uiso 0.326(9) 1 calc PR C 2 C35 C 0.3732(3) 1.0587(2) 0.7858(2) 0.0418(9) Uani 1 1 d . . . H35 H 0.4110 1.0432 0.7468 0.050 Uiso 1 1 calc R C . C36 C 0.3923(3) 1.1423(2) 0.8015(2) 0.0426(9) Uani 1 1 d . C . H36A H 0.3412 1.1657 0.8230 0.051 Uiso 1 1 calc R . . H36B H 0.4001 1.1691 0.7549 0.051 Uiso 1 1 calc R . . C37 C 0.4809(3) 1.1456(2) 0.8576(2) 0.0488(10) Uani 1 1 d . . . H37A H 0.5312 1.1676 0.8339 0.059 Uiso 1 1 calc R C . H37B H 0.4721 1.1768 0.9014 0.059 Uiso 1 1 calc R . . C38 C 0.5030(3) 1.0642(2) 0.8814(3) 0.0499(10) Uani 1 1 d . C . H38A H 0.5525 1.0440 0.8557 0.060 Uiso 1 1 calc R . . H38B H 0.5223 1.0611 0.9361 0.060 Uiso 1 1 calc R . . C39 C 0.4148(3) 1.0209(2) 0.8588(2) 0.0451(9) Uani 1 1 d . C . H39A H 0.3737 1.0254 0.8972 0.054 Uiso 1 1 calc R . . H39B H 0.4272 0.9670 0.8509 0.054 Uiso 1 1 calc R . . C40 C 0.2353(2) 0.5489(2) 0.6885(2) 0.0353(8) Uani 1 1 d . . . C41 C 0.2409(2) 0.4815(2) 0.6895(2) 0.0373(8) Uani 1 1 d . F . Si2 Si 0.24814(7) 0.37868(6) 0.70580(6) 0.0373(3) Uani 1 1 d . . . C42 C 0.1370(3) 0.3496(2) 0.7364(2) 0.0408(9) Uani 1 1 d . F . H42 H 0.0885 0.3560 0.6923 0.049 Uiso 1 1 calc R . . C43 C 0.1054(3) 0.3929(2) 0.8012(2) 0.0434(9) Uani 1 1 d . . . H43A H 0.1561 0.3989 0.8429 0.052 Uiso 1 1 calc R F . H43B H 0.0822 0.4433 0.7848 0.052 Uiso 1 1 calc R . . C44 C 0.0293(3) 0.3443(2) 0.8247(3) 0.0489(10) Uani 1 1 d . F . H44A H 0.0281 0.3488 0.8791 0.059 Uiso 1 1 calc R . . H44B H -0.0308 0.3600 0.7979 0.059 Uiso 1 1 calc R . . C45 C 0.0508(3) 0.2636(2) 0.8042(2) 0.0470(10) Uani 1 1 d . . . H45A H 0.0655 0.2326 0.8499 0.056 Uiso 1 1 calc R F . H45B H -0.0022 0.2409 0.7724 0.056 Uiso 1 1 calc R . . C46 C 0.1323(3) 0.2675(2) 0.7623(3) 0.0571(12) Uani 1 1 d . F . H46A H 0.1239 0.2331 0.7188 0.068 Uiso 1 1 calc R . . H46B H 0.1890 0.2535 0.7953 0.068 Uiso 1 1 calc R . . C47 C 0.3492(3) 0.3604(3) 0.7785(2) 0.0501(10) Uani 1 1 d DU E . H47 H 0.3555 0.3044 0.7816 0.060 Uiso 1 1 calc R D 1 C48 C 0.3435(9) 0.3869(9) 0.8581(6) 0.066(3) Uani 0.591(14) 1 d PDU E 1 H48A H 0.3055 0.3524 0.8836 0.079 Uiso 0.591(14) 1 calc PR E 1 H48B H 0.3176 0.4383 0.8581 0.079 Uiso 0.591(14) 1 calc PR E 1 C49 C 0.4447(9) 0.3857(12) 0.8961(7) 0.083(3) Uani 0.591(14) 1 d PDU E 1 H49A H 0.4540 0.4204 0.9394 0.099 Uiso 0.591(14) 1 calc PR E 1 H49B H 0.4632 0.3344 0.9133 0.099 Uiso 0.591(14) 1 calc PR E 1 C50 C 0.4975(7) 0.4112(9) 0.8360(8) 0.077(3) Uani 0.591(14) 1 d PDU E 1 H50A H 0.5580 0.3864 0.8416 0.092 Uiso 0.591(14) 1 calc PR E 1 H50B H 0.5069 0.4664 0.8387 0.092 Uiso 0.591(14) 1 calc PR E 1 C51 C 0.4419(10) 0.390(2) 0.7624(7) 0.074(4) Uani 0.591(14) 1 d PDU E 1 H51A H 0.4739 0.3504 0.7375 0.088 Uiso 0.591(14) 1 calc PR E 1 H51B H 0.4330 0.4342 0.7291 0.088 Uiso 0.591(14) 1 calc PR E 1 C48' C 0.3579(13) 0.4079(13) 0.8493(10) 0.066(3) Uani 0.409(14) 1 d PDU E 2 H48C H 0.3205 0.3867 0.8855 0.079 Uiso 0.409(14) 1 calc PR E 2 H48D H 0.3383 0.4604 0.8377 0.079 Uiso 0.409(14) 1 calc PR E 2 C49' C 0.4611(15) 0.4045(17) 0.8807(10) 0.083(3) Uani 0.409(14) 1 d PDU E 2 H49C H 0.4851 0.4555 0.8936 0.099 Uiso 0.409(14) 1 calc PR E 2 H49D H 0.4713 0.3728 0.9261 0.099 Uiso 0.409(14) 1 calc PR E 2 C50' C 0.5075(9) 0.3712(12) 0.8205(11) 0.077(3) Uani 0.409(14) 1 d PDU E 2 H50C H 0.5239 0.3180 0.8320 0.092 Uiso 0.409(14) 1 calc PR E 2 H50D H 0.5639 0.3995 0.8154 0.092 Uiso 0.409(14) 1 calc PR E 2 C51' C 0.4399(13) 0.376(3) 0.7488(10) 0.074(4) Uani 0.409(14) 1 d PDU E 2 H51C H 0.4526 0.3381 0.7119 0.088 Uiso 0.409(14) 1 calc PR E 2 H51D H 0.4402 0.4270 0.7260 0.088 Uiso 0.409(14) 1 calc PR E 2 C52 C 0.2610(3) 0.3281(2) 0.6173(2) 0.0493(10) Uani 0.849(19) 1 d PD F 1 H52 H 0.2809 0.2755 0.6309 0.059 Uiso 0.849(19) 1 calc PR F 1 C53 C 0.3275(6) 0.3603(4) 0.5674(4) 0.0568(18) Uani 0.849(19) 1 d PD F 1 H53A H 0.3186 0.4151 0.5602 0.068 Uiso 0.849(19) 1 calc PR F 1 H53B H 0.3917 0.3506 0.5893 0.068 Uiso 0.849(19) 1 calc PR F 1 C54 C 0.3030(8) 0.3181(5) 0.4931(4) 0.074(3) Uani 0.849(19) 1 d PD F 1 H54A H 0.3169 0.3494 0.4509 0.089 Uiso 0.849(19) 1 calc PR F 1 H54B H 0.3381 0.2706 0.4937 0.089 Uiso 0.849(19) 1 calc PR F 1 C55 C 0.2021(8) 0.3021(4) 0.4859(3) 0.072(3) Uani 0.849(19) 1 d PD F 1 H55A H 0.1898 0.2482 0.4746 0.086 Uiso 0.849(19) 1 calc PR F 1 H55B H 0.1682 0.3327 0.4453 0.086 Uiso 0.849(19) 1 calc PR F 1 C56 C 0.1732(5) 0.3232(5) 0.5621(4) 0.0632(17) Uani 0.849(19) 1 d PD F 1 H56A H 0.1409 0.3721 0.5587 0.076 Uiso 0.849(19) 1 calc PR F 1 H56B H 0.1322 0.2844 0.5780 0.076 Uiso 0.849(19) 1 calc PR F 1 C52' C 0.2610(3) 0.3281(2) 0.6173(2) 0.0493(10) Uani 0.151(19) 1 d PD F 2 H52' H 0.2731 0.2749 0.6339 0.059 Uiso 0.151(19) 1 calc PR F 2 C53' C 0.3505(19) 0.352(3) 0.590(2) 0.0568(18) Uani 0.151(19) 1 d PD F 2 H53C H 0.3555 0.4077 0.5888 0.068 Uiso 0.151(19) 1 calc PR F 2 H53D H 0.4041 0.3317 0.6229 0.068 Uiso 0.151(19) 1 calc PR F 2 C54' C 0.345(3) 0.320(3) 0.512(2) 0.074(3) Uani 0.151(19) 1 d PD F 2 H54C H 0.3498 0.3602 0.4750 0.089 Uiso 0.151(19) 1 calc PR F 2 H54D H 0.3948 0.2831 0.5093 0.089 Uiso 0.151(19) 1 calc PR F 2 C55' C 0.254(4) 0.281(3) 0.4944(18) 0.072(3) Uani 0.151(19) 1 d PD F 2 H55C H 0.2592 0.2264 0.5053 0.086 Uiso 0.151(19) 1 calc PR F 2 H55D H 0.2274 0.2878 0.4413 0.086 Uiso 0.151(19) 1 calc PR F 2 C56' C 0.194(2) 0.320(3) 0.5468(16) 0.0632(17) Uani 0.151(19) 1 d PD F 2 H56C H 0.1716 0.3700 0.5270 0.076 Uiso 0.151(19) 1 calc PR F 2 H56D H 0.1407 0.2888 0.5549 0.076 Uiso 0.151(19) 1 calc PR F 2 C57 C 0.4418(3) 0.8227(3) 0.3631(2) 0.0495(10) Uani 1 1 d . . . F1 F 0.41547(18) 0.80228(17) 0.29160(13) 0.0640(7) Uani 1 1 d . . . F2 F 0.4284(3) 0.89568(17) 0.36792(19) 0.0866(11) Uani 1 1 d . . . F3 F 0.53224(18) 0.81079(19) 0.37507(15) 0.0704(8) 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 0.0379(6) 0.0303(5) 0.0452(6) -0.0023(4) 0.0025(4) -0.0018(4) C1 0.0278(17) 0.0354(19) 0.0333(18) -0.0022(14) 0.0015(13) 0.0004(14) C2 0.0285(17) 0.0360(19) 0.0322(17) 0.0014(14) -0.0002(13) 0.0000(14) C3 0.0308(18) 0.0342(19) 0.0362(18) -0.0006(15) -0.0003(14) -0.0028(14) C4 0.0299(18) 0.044(2) 0.0332(18) 0.0041(15) 0.0022(14) -0.0003(15) C5 0.039(2) 0.039(2) 0.042(2) 0.0013(16) 0.0054(16) -0.0031(16) C6 0.0342(19) 0.051(2) 0.0354(19) 0.0071(16) 0.0065(15) -0.0025(16) C7 0.039(2) 0.052(2) 0.0342(19) -0.0036(17) 0.0071(15) 0.0004(17) C8 0.0340(19) 0.040(2) 0.040(2) -0.0007(16) 0.0051(15) -0.0003(15) C9 0.0295(18) 0.040(2) 0.0353(18) -0.0018(15) 0.0019(14) 0.0018(15) C10 0.0323(18) 0.0322(18) 0.0352(18) -0.0010(14) 0.0003(14) 0.0010(14) C11 0.0295(17) 0.0323(18) 0.0324(17) -0.0031(14) 0.0008(13) 0.0015(14) C12 0.0306(18) 0.0315(18) 0.0368(18) -0.0016(14) 0.0012(14) -0.0009(14) C13 0.0292(18) 0.0353(19) 0.0343(18) -0.0025(14) 0.0013(14) -0.0011(14) C14 0.041(2) 0.0340(19) 0.0366(19) -0.0016(15) 0.0050(15) -0.0036(15) C15 0.036(2) 0.043(2) 0.0352(19) -0.0026(16) 0.0050(15) -0.0050(16) C16 0.050(2) 0.046(2) 0.047(2) 0.0013(18) 0.0142(18) -0.0093(18) C17 0.052(2) 0.055(3) 0.039(2) 0.0007(18) 0.0154(18) -0.0092(19) C18 0.039(2) 0.067(3) 0.035(2) -0.0043(19) 0.0097(16) -0.0019(19) C19 0.036(2) 0.047(2) 0.038(2) -0.0069(17) 0.0031(15) 0.0042(16) C20 0.0317(18) 0.044(2) 0.0309(18) -0.0028(15) 0.0032(14) -0.0001(15) C21 0.0303(18) 0.0345(19) 0.0358(18) -0.0051(15) 0.0021(14) 0.0018(14) C22 0.0286(17) 0.0345(19) 0.0287(17) 0.0007(14) 0.0017(13) 0.0009(14) C23 0.0316(18) 0.034(2) 0.0316(17) -0.0006(14) 0.0038(14) 0.0018(14) C24 0.0324(19) 0.041(2) 0.041(2) -0.0017(16) 0.0041(15) 0.0009(15) C25 0.043(2) 0.0297(19) 0.054(2) -0.0037(17) 0.0060(17) 0.0014(16) C26 0.046(2) 0.041(2) 0.053(2) -0.0017(18) 0.0102(18) 0.0023(17) C27 0.052(3) 0.070(3) 0.089(4) 0.024(3) 0.025(3) 0.006(2) C28 0.044(2) 0.062(3) 0.076(3) 0.000(2) 0.014(2) 0.005(2) C29 0.041(2) 0.049(3) 0.063(3) -0.002(2) 0.0032(19) 0.0025(18) C30 0.056(2) 0.034(2) 0.052(2) 0.0003(17) 0.0005(18) -0.0005(18) C31 0.053(2) 0.060(3) 0.050(2) -0.001(2) -0.0035(19) 0.006(2) C32 0.0611(17) 0.048(3) 0.0517(15) 0.0063(15) 0.0033(13) 0.0000(17) C33 0.0611(17) 0.048(3) 0.0517(15) 0.0063(15) 0.0033(13) 0.0000(17) C34 0.0611(17) 0.048(3) 0.0517(15) 0.0063(15) 0.0033(13) 0.0000(17) C32' 0.0611(17) 0.048(3) 0.0517(15) 0.0063(15) 0.0033(13) 0.0000(17) C33' 0.0611(17) 0.048(3) 0.0517(15) 0.0063(15) 0.0033(13) 0.0000(17) C34' 0.0611(17) 0.048(3) 0.0517(15) 0.0063(15) 0.0033(13) 0.0000(17) C35 0.041(2) 0.040(2) 0.044(2) -0.0031(17) 0.0054(17) -0.0017(16) C36 0.048(2) 0.040(2) 0.041(2) 0.0020(16) 0.0099(17) -0.0064(17) C37 0.049(2) 0.049(2) 0.047(2) 0.0014(19) 0.0037(18) -0.0131(19) C38 0.038(2) 0.052(3) 0.057(3) -0.001(2) -0.0008(18) -0.0047(18) C39 0.046(2) 0.033(2) 0.055(2) 0.0033(17) 0.0031(18) 0.0004(17) C40 0.0336(19) 0.036(2) 0.0364(19) -0.0002(15) 0.0052(14) -0.0004(15) C41 0.0355(19) 0.038(2) 0.040(2) 0.0008(16) 0.0101(15) -0.0003(15) Si2 0.0421(6) 0.0319(5) 0.0392(5) 0.0003(4) 0.0102(4) 0.0017(4) C42 0.044(2) 0.036(2) 0.042(2) 0.0001(16) 0.0060(16) 0.0001(16) C43 0.040(2) 0.040(2) 0.052(2) -0.0045(17) 0.0131(17) -0.0007(17) C44 0.047(2) 0.050(2) 0.053(2) -0.0056(19) 0.0165(19) -0.0061(19) C45 0.042(2) 0.044(2) 0.055(2) 0.0115(18) 0.0056(18) -0.0017(17) C46 0.064(3) 0.032(2) 0.079(3) -0.005(2) 0.027(2) -0.003(2) C47 0.048(2) 0.045(2) 0.057(2) 0.0101(19) 0.0060(19) -0.0004(18) C48 0.051(4) 0.085(9) 0.061(4) 0.008(5) 0.002(3) -0.016(4) C49 0.064(6) 0.106(11) 0.071(5) 0.023(6) -0.014(4) -0.011(5) C50 0.044(3) 0.082(9) 0.101(6) 0.004(6) -0.002(3) -0.011(5) C51 0.045(3) 0.097(13) 0.078(5) 0.024(7) 0.009(3) 0.002(3) C48' 0.051(4) 0.085(9) 0.061(4) 0.008(5) 0.002(3) -0.016(4) C49' 0.064(6) 0.106(11) 0.071(5) 0.023(6) -0.014(4) -0.011(5) C50' 0.044(3) 0.082(9) 0.101(6) 0.004(6) -0.002(3) -0.011(5) C51' 0.045(3) 0.097(13) 0.078(5) 0.024(7) 0.009(3) 0.002(3) C52 0.073(3) 0.031(2) 0.049(2) 0.0017(17) 0.023(2) 0.0027(19) C53 0.081(4) 0.049(3) 0.045(4) 0.011(3) 0.025(3) 0.007(3) C54 0.131(8) 0.049(3) 0.051(4) -0.001(3) 0.043(5) 0.008(6) C55 0.134(8) 0.043(4) 0.039(3) -0.004(2) 0.016(4) -0.008(4) C56 0.092(5) 0.060(3) 0.039(3) -0.008(3) 0.015(3) -0.014(4) C52' 0.073(3) 0.031(2) 0.049(2) 0.0017(17) 0.023(2) 0.0027(19) C53' 0.081(4) 0.049(3) 0.045(4) 0.011(3) 0.025(3) 0.007(3) C54' 0.131(8) 0.049(3) 0.051(4) -0.001(3) 0.043(5) 0.008(6) C55' 0.134(8) 0.043(4) 0.039(3) -0.004(2) 0.016(4) -0.008(4) C56' 0.092(5) 0.060(3) 0.039(3) -0.008(3) 0.015(3) -0.014(4) C57 0.050(2) 0.057(3) 0.045(2) 0.0035(19) 0.0145(18) -0.007(2) F1 0.0573(16) 0.096(2) 0.0396(13) 0.0117(13) 0.0109(11) -0.0138(14) F2 0.132(3) 0.0508(17) 0.092(2) 0.0130(15) 0.066(2) -0.0047(17) F3 0.0456(15) 0.106(2) 0.0602(16) 0.0170(15) 0.0107(12) -0.0175(14) _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 C24 1.857(4) . ? Si1 C30 1.873(4) . ? Si1 C25 1.878(4) . ? Si1 C35 1.886(4) . ? C1 C2 1.416(5) . ? C1 C22 1.424(5) . ? C1 C23 1.428(5) . ? C2 C3 1.406(5) . ? C2 C11 1.437(5) . ? C3 C4 1.388(5) . ? C3 H3 0.9500 . ? C4 C9 1.426(5) . ? C4 C5 1.442(5) . ? C5 C6 1.359(5) . ? C5 H5 0.9500 . ? C6 C7 1.423(6) . ? C6 C57 1.502(5) . ? C7 C8 1.354(5) . ? C7 H7 0.9500 . ? C8 C9 1.431(5) . ? C8 H8 0.9500 . ? C9 C10 1.386(5) . ? C10 C11 1.411(5) . ? C10 H10 0.9500 . ? C11 C12 1.418(5) . ? C12 C13 1.420(5) . ? C12 C40 1.433(5) . ? C13 C14 1.409(5) . ? C13 C22 1.434(5) . ? C14 C15 1.390(5) . ? C14 H14 0.9500 . ? C15 C20 1.429(5) . ? C15 C16 1.434(5) . ? C16 C17 1.359(6) . ? C16 H16 0.9500 . ? C17 C18 1.412(6) . ? C17 H17 0.9500 . ? C18 C19 1.358(6) . ? C18 H18 0.9500 . ? C19 C20 1.436(5) . ? C19 H19 0.9500 . ? C20 C21 1.385(5) . ? C21 C22 1.408(5) . ? C21 H21 0.9500 . ? C23 C24 1.194(5) . ? C25 C29 1.540(6) . ? C25 C26 1.552(6) . ? C25 H25 1.0000 . ? C26 C27 1.549(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.503(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.529(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C34' 1.525(14) . ? C30 C31 1.537(6) . ? C30 C34 1.559(9) . ? C30 H30 1.0000 . ? C31 C32' 1.500(14) . ? C31 C32 1.534(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.523(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.524(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C32' C33' 1.547(15) . ? C32' H32C 0.9900 . ? C32' H32D 0.9900 . ? C33' C34' 1.515(16) . ? C33' H33C 0.9900 . ? C33' H33D 0.9900 . ? C34' H34C 0.9900 . ? C34' H34D 0.9900 . ? C35 C36 1.531(5) . ? C35 C39 1.530(6) . ? C35 H35 1.0000 . ? C36 C37 1.540(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.532(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.520(6) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.200(5) . ? C41 Si2 1.852(4) . ? Si2 C52 1.869(4) . ? Si2 C47 1.873(4) . ? Si2 C42 1.881(4) . ? C42 C43 1.529(5) . ? C42 C46 1.537(6) . ? C42 H42 1.0000 . ? C43 C44 1.528(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.527(6) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.515(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48' 1.524(14) . ? C47 C48 1.528(10) . ? C47 C51 1.534(12) . ? C47 C51' 1.542(13) . ? C47 H47 1.0000 . ? C48 C49 1.556(11) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.499(14) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.509(13) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C48' C49' 1.552(14) . ? C48' H48C 0.9900 . ? C48' H48D 0.9900 . ? C49' C50' 1.491(18) . ? C49' H49C 0.9900 . ? C49' H49D 0.9900 . ? C50' C51' 1.522(18) . ? C50' H50C 0.9900 . ? C50' H50D 0.9900 . ? C51' H51C 0.9900 . ? C51' H51D 0.9900 . ? C52 C56 1.522(7) . ? C52 C53 1.539(6) . ? C52 H52 1.0000 . ? C53 C54 1.535(8) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.506(11) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.548(8) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C53' C54' 1.522(19) . ? C53' H53C 0.9900 . ? C53' H53D 0.9900 . ? C54' C55' 1.50(2) . ? C54' H54C 0.9900 . ? C54' H54D 0.9900 . ? C55' C56' 1.56(2) . ? C55' H55C 0.9900 . ? C55' H55D 0.9900 . ? C56' H56C 0.9900 . ? C56' H56D 0.9900 . ? C57 F2 1.318(5) . ? C57 F3 1.341(5) . ? C57 F1 1.345(5) . ? 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 C24 Si1 C30 106.58(18) . . ? C24 Si1 C25 106.36(18) . . ? C30 Si1 C25 114.73(19) . . ? C24 Si1 C35 108.62(17) . . ? C30 Si1 C35 107.45(19) . . ? C25 Si1 C35 112.79(18) . . ? C2 C1 C22 120.7(3) . . ? C2 C1 C23 120.3(3) . . ? C22 C1 C23 118.9(3) . . ? C3 C2 C1 121.5(3) . . ? C3 C2 C11 118.6(3) . . ? C1 C2 C11 119.9(3) . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C9 120.1(3) . . ? C3 C4 C5 121.2(4) . . ? C9 C4 C5 118.6(3) . . ? C6 C5 C4 119.8(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 121.5(3) . . ? C5 C6 C57 120.1(4) . . ? C7 C6 C57 118.3(4) . . ? C8 C7 C6 120.1(4) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 120.8(4) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C4 119.1(3) . . ? C10 C9 C8 121.7(3) . . ? C4 C9 C8 119.1(3) . . ? C9 C10 C11 121.5(3) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C12 121.2(3) . . ? C10 C11 C2 119.2(3) . . ? C12 C11 C2 119.6(3) . . ? C11 C12 C13 120.2(3) . . ? C11 C12 C40 120.3(3) . . ? C13 C12 C40 119.4(3) . . ? C14 C13 C12 121.1(3) . . ? C14 C13 C22 118.4(3) . . ? C12 C13 C22 120.5(3) . . ? C15 C14 C13 121.8(3) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C20 119.7(3) . . ? C14 C15 C16 122.0(4) . . ? C20 C15 C16 118.2(3) . . ? C17 C16 C15 120.8(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 120.7(4) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 120.7(4) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 120.6(4) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C15 118.9(3) . . ? C21 C20 C19 122.2(4) . . ? C15 C20 C19 118.8(3) . . ? C20 C21 C22 122.1(3) . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C21 C22 C1 122.0(3) . . ? C21 C22 C13 119.0(3) . . ? C1 C22 C13 119.0(3) . . ? C24 C23 C1 177.8(4) . . ? C23 C24 Si1 178.9(4) . . ? C29 C25 C26 103.8(3) . . ? C29 C25 Si1 115.5(3) . . ? C26 C25 Si1 115.1(3) . . ? C29 C25 H25 107.3 . . ? C26 C25 H25 107.3 . . ? Si1 C25 H25 107.3 . . ? C27 C26 C25 106.2(4) . . ? C27 C26 H26A 110.5 . . ? C25 C26 H26A 110.5 . . ? C27 C26 H26B 110.5 . . ? C25 C26 H26B 110.5 . . ? H26A C26 H26B 108.7 . . ? C28 C27 C26 106.0(4) . . ? C28 C27 H27A 110.5 . . ? C26 C27 H27A 110.5 . . ? C28 C27 H27B 110.5 . . ? C26 C27 H27B 110.5 . . ? H27A C27 H27B 108.7 . . ? C27 C28 C29 103.3(4) . . ? C27 C28 H28A 111.1 . . ? C29 C28 H28A 111.1 . . ? C27 C28 H28B 111.1 . . ? C29 C28 H28B 111.1 . . ? H28A C28 H28B 109.1 . . ? C28 C29 C25 103.9(4) . . ? C28 C29 H29A 111.0 . . ? C25 C29 H29A 111.0 . . ? C28 C29 H29B 111.0 . . ? C25 C29 H29B 111.0 . . ? H29A C29 H29B 109.0 . . ? C34' C30 C31 103.6(7) . . ? C31 C30 C34 102.1(4) . . ? C34' C30 Si1 116.6(8) . . ? C31 C30 Si1 117.0(3) . . ? C34 C30 Si1 110.2(4) . . ? C34' C30 H30 100.0 . . ? C31 C30 H30 109.1 . . ? C34 C30 H30 109.1 . . ? Si1 C30 H30 109.1 . . ? C32' C31 C30 107.5(7) . . ? C32 C31 C30 103.3(5) . . ? C32' C31 H31A 99.5 . . ? C32 C31 H31A 111.1 . . ? C30 C31 H31A 111.1 . . ? C32' C31 H31B 118.0 . . ? C32 C31 H31B 111.1 . . ? C30 C31 H31B 111.1 . . ? H31A C31 H31B 109.1 . . ? C33 C32 C31 107.2(5) . . ? C33 C32 H32A 110.3 . . ? C31 C32 H32A 110.3 . . ? C33 C32 H32B 110.3 . . ? C31 C32 H32B 110.3 . . ? H32A C32 H32B 108.5 . . ? C32 C33 C34 106.4(6) . . ? C32 C33 H33A 110.5 . . ? C34 C33 H33A 110.5 . . ? C32 C33 H33B 110.5 . . ? C34 C33 H33B 110.5 . . ? H33A C33 H33B 108.6 . . ? C33 C34 C30 103.8(6) . . ? C33 C34 H34A 111.0 . . ? C30 C34 H34A 111.0 . . ? C33 C34 H34B 111.0 . . ? C30 C34 H34B 111.0 . . ? H34A C34 H34B 109.0 . . ? C31 C32' C33' 99.6(9) . . ? C31 C32' H32C 111.9 . . ? C33' C32' H32C 111.9 . . ? C31 C32' H32D 111.9 . . ? C33' C32' H32D 111.9 . . ? H32C C32' H32D 109.6 . . ? C34' C33' C32' 103.0(11) . . ? C34' C33' H33C 111.2 . . ? C32' C33' H33C 111.2 . . ? C34' C33' H33D 111.2 . . ? C32' C33' H33D 111.2 . . ? H33C C33' H33D 109.1 . . ? C33' C34' C30 106.3(10) . . ? C33' C34' H34C 110.5 . . ? C30 C34' H34C 110.5 . . ? C33' C34' H34D 110.5 . . ? C30 C34' H34D 110.5 . . ? H34C C34' H34D 108.7 . . ? C36 C35 C39 103.0(3) . . ? C36 C35 Si1 114.2(3) . . ? C39 C35 Si1 118.0(3) . . ? C36 C35 H35 107.0 . . ? C39 C35 H35 107.0 . . ? Si1 C35 H35 107.0 . . ? C35 C36 C37 106.1(3) . . ? C35 C36 H36A 110.5 . . ? C37 C36 H36A 110.5 . . ? C35 C36 H36B 110.5 . . ? C37 C36 H36B 110.5 . . ? H36A C36 H36B 108.7 . . ? C38 C37 C36 106.0(3) . . ? C38 C37 H37A 110.5 . . ? C36 C37 H37A 110.5 . . ? C38 C37 H37B 110.5 . . ? C36 C37 H37B 110.5 . . ? H37A C37 H37B 108.7 . . ? C39 C38 C37 105.3(3) . . ? C39 C38 H38A 110.7 . . ? C37 C38 H38A 110.7 . . ? C39 C38 H38B 110.7 . . ? C37 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? C38 C39 C35 103.4(3) . . ? C38 C39 H39A 111.1 . . ? C35 C39 H39A 111.1 . . ? C38 C39 H39B 111.1 . . ? C35 C39 H39B 111.1 . . ? H39A C39 H39B 109.0 . . ? C41 C40 C12 176.2(4) . . ? C40 C41 Si2 171.6(3) . . ? C41 Si2 C52 110.42(18) . . ? C41 Si2 C47 107.80(19) . . ? C52 Si2 C47 110.4(2) . . ? C41 Si2 C42 106.54(17) . . ? C52 Si2 C42 108.72(19) . . ? C47 Si2 C42 112.86(19) . . ? C43 C42 C46 102.3(3) . . ? C43 C42 Si2 117.6(3) . . ? C46 C42 Si2 115.5(3) . . ? C43 C42 H42 106.9 . . ? C46 C42 H42 106.9 . . ? Si2 C42 H42 106.9 . . ? C44 C43 C42 104.3(3) . . ? C44 C43 H43A 110.9 . . ? C42 C43 H43A 110.9 . . ? C44 C43 H43B 110.9 . . ? C42 C43 H43B 110.9 . . ? H43A C43 H43B 108.9 . . ? C45 C44 C43 106.0(3) . . ? C45 C44 H44A 110.5 . . ? C43 C44 H44A 110.5 . . ? C45 C44 H44B 110.5 . . ? C43 C44 H44B 110.5 . . ? H44A C44 H44B 108.7 . . ? C46 C45 C44 106.6(3) . . ? C46 C45 H45A 110.4 . . ? C44 C45 H45A 110.4 . . ? C46 C45 H45B 110.4 . . ? C44 C45 H45B 110.4 . . ? H45A C45 H45B 108.6 . . ? C45 C46 C42 105.7(3) . . ? C45 C46 H46A 110.6 . . ? C42 C46 H46A 110.6 . . ? C45 C46 H46B 110.6 . . ? C42 C46 H46B 110.6 . . ? H46A C46 H46B 108.7 . . ? C48' C47 C51 90.0(12) . . ? C48 C47 C51 104.2(8) . . ? C48' C47 C51' 102.6(14) . . ? C48 C47 C51' 116.2(11) . . ? C48' C47 Si2 117.1(9) . . ? C48 C47 Si2 117.5(6) . . ? C51 C47 Si2 116.9(9) . . ? C51' C47 Si2 111.7(11) . . ? C48' C47 H47 120.6 . . ? C48 C47 H47 105.7 . . ? C51 C47 H47 105.7 . . ? C51' C47 H47 97.1 . . ? Si2 C47 H47 105.7 . . ? C47 C48 C49 103.4(8) . . ? C47 C48 H48A 111.1 . . ? C49 C48 H48A 111.1 . . ? C47 C48 H48B 111.1 . . ? C49 C48 H48B 111.1 . . ? H48A C48 H48B 109.0 . . ? C50 C49 C48 104.1(8) . . ? C50 C49 H49A 110.9 . . ? C48 C49 H49A 110.9 . . ? C50 C49 H49B 110.9 . . ? C48 C49 H49B 110.9 . . ? H49A C49 H49B 109.0 . . ? C49 C50 C51 106.8(9) . . ? C49 C50 H50A 110.4 . . ? C51 C50 H50A 110.4 . . ? C49 C50 H50B 110.4 . . ? C51 C50 H50B 110.4 . . ? H50A C50 H50B 108.6 . . ? C50 C51 C47 107.9(8) . . ? C50 C51 H51A 110.1 . . ? C47 C51 H51A 110.1 . . ? C50 C51 H51B 110.1 . . ? C47 C51 H51B 110.1 . . ? H51A C51 H51B 108.4 . . ? C47 C48' C49' 104.2(12) . . ? C47 C48' H48C 110.9 . . ? C49' C48' H48C 110.9 . . ? C47 C48' H48D 110.9 . . ? C49' C48' H48D 110.9 . . ? H48C C48' H48D 108.9 . . ? C50' C49' C48' 106.3(11) . . ? C50' C49' H49C 110.5 . . ? C48' C49' H49C 110.5 . . ? C50' C49' H49D 110.5 . . ? C48' C49' H49D 110.5 . . ? H49C C49' H49D 108.7 . . ? C49' C50' C51' 106.5(16) . . ? C49' C50' H50C 110.4 . . ? C51' C50' H50C 110.4 . . ? C49' C50' H50D 110.4 . . ? C51' C50' H50D 110.4 . . ? H50C C50' H50D 108.6 . . ? C50' C51' C47 100.9(12) . . ? C50' C51' H51C 111.6 . . ? C47 C51' H51C 111.6 . . ? C50' C51' H51D 111.6 . . ? C47 C51' H51D 111.6 . . ? H51C C51' H51D 109.4 . . ? C56 C52 C53 101.1(4) . . ? C56 C52 Si2 114.0(4) . . ? C53 C52 Si2 118.5(4) . . ? C56 C52 H52 107.5 . . ? C53 C52 H52 107.5 . . ? Si2 C52 H52 107.5 . . ? C54 C53 C52 104.0(5) . . ? C54 C53 H53A 111.0 . . ? C52 C53 H53A 111.0 . . ? C54 C53 H53B 111.0 . . ? C52 C53 H53B 111.0 . . ? H53A C53 H53B 109.0 . . ? C55 C54 C53 106.0(5) . . ? C55 C54 H54A 110.5 . . ? C53 C54 H54A 110.5 . . ? C55 C54 H54B 110.5 . . ? C53 C54 H54B 110.5 . . ? H54A C54 H54B 108.7 . . ? C54 C55 C56 105.9(5) . . ? C54 C55 H55A 110.6 . . ? C56 C55 H55A 110.6 . . ? C54 C55 H55B 110.6 . . ? C56 C55 H55B 110.6 . . ? H55A C55 H55B 108.7 . . ? C52 C56 C55 106.3(5) . . ? C52 C56 H56A 110.5 . . ? C55 C56 H56A 110.5 . . ? C52 C56 H56B 110.5 . . ? C55 C56 H56B 110.5 . . ? H56A C56 H56B 108.7 . . ? C54' C53' H53C 110.8 . . ? C54' C53' H53D 110.8 . . ? H53C C53' H53D 108.8 . . ? C55' C54' C53' 107.2(16) . . ? C55' C54' H54C 110.3 . . ? C53' C54' H54C 110.3 . . ? C53' C54' H54D 110.3 . . ? H54C C54' H54D 108.5 . . ? C54' C55' C56' 103.9(19) . . ? C54' C55' H55C 111.0 . . ? C56' C55' H55C 111.0 . . ? C54' C55' H55D 111.0 . . ? C56' C55' H55D 111.0 . . ? H55C C55' H55D 109.0 . . ? C55' C56' H56C 111.6 . . ? C55' C56' H56D 111.6 . . ? H56C C56' H56D 109.4 . . ? F2 C57 F3 107.5(4) . . ? F2 C57 F1 107.7(4) . . ? F3 C57 F1 104.9(3) . . ? F2 C57 C6 113.6(4) . . ? F3 C57 C6 111.1(4) . . ? F1 C57 C6 111.6(3) . . ? 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 C22 C1 C2 C3 -179.4(3) . . . . ? C23 C1 C2 C3 -1.3(5) . . . . ? C22 C1 C2 C11 -0.5(5) . . . . ? C23 C1 C2 C11 177.6(3) . . . . ? C1 C2 C3 C4 178.5(3) . . . . ? C11 C2 C3 C4 -0.3(5) . . . . ? C2 C3 C4 C9 1.9(5) . . . . ? C2 C3 C4 C5 -176.9(3) . . . . ? C3 C4 C5 C6 178.1(3) . . . . ? C9 C4 C5 C6 -0.7(5) . . . . ? C4 C5 C6 C7 1.5(6) . . . . ? C4 C5 C6 C57 -174.6(3) . . . . ? C5 C6 C7 C8 -0.7(6) . . . . ? C57 C6 C7 C8 175.4(4) . . . . ? C6 C7 C8 C9 -0.9(6) . . . . ? C3 C4 C9 C10 -1.2(5) . . . . ? C5 C4 C9 C10 177.7(3) . . . . ? C3 C4 C9 C8 -179.7(3) . . . . ? C5 C4 C9 C8 -0.9(5) . . . . ? C7 C8 C9 C10 -176.8(3) . . . . ? C7 C8 C9 C4 1.7(5) . . . . ? C4 C9 C10 C11 -1.1(5) . . . . ? C8 C9 C10 C11 177.4(3) . . . . ? C9 C10 C11 C12 -175.3(3) . . . . ? C9 C10 C11 C2 2.6(5) . . . . ? C3 C2 C11 C10 -1.9(5) . . . . ? C1 C2 C11 C10 179.3(3) . . . . ? C3 C2 C11 C12 176.1(3) . . . . ? C1 C2 C11 C12 -2.8(5) . . . . ? C10 C11 C12 C13 -178.6(3) . . . . ? C2 C11 C12 C13 3.5(5) . . . . ? C10 C11 C12 C40 4.0(5) . . . . ? C2 C11 C12 C40 -173.9(3) . . . . ? C11 C12 C13 C14 -179.2(3) . . . . ? C40 C12 C13 C14 -1.8(5) . . . . ? C11 C12 C13 C22 -1.0(5) . . . . ? C40 C12 C13 C22 176.5(3) . . . . ? C12 C13 C14 C15 179.7(3) . . . . ? C22 C13 C14 C15 1.4(5) . . . . ? C13 C14 C15 C20 1.4(6) . . . . ? C13 C14 C15 C16 -177.4(4) . . . . ? C14 C15 C16 C17 179.4(4) . . . . ? C20 C15 C16 C17 0.6(6) . . . . ? C15 C16 C17 C18 2.2(7) . . . . ? C16 C17 C18 C19 -2.5(7) . . . . ? C17 C18 C19 C20 -0.2(6) . . . . ? C14 C15 C20 C21 -2.9(5) . . . . ? C16 C15 C20 C21 176.0(3) . . . . ? C14 C15 C20 C19 178.0(3) . . . . ? C16 C15 C20 C19 -3.1(5) . . . . ? C18 C19 C20 C21 -176.1(4) . . . . ? C18 C19 C20 C15 2.9(5) . . . . ? C15 C20 C21 C22 1.6(5) . . . . ? C19 C20 C21 C22 -179.3(3) . . . . ? C20 C21 C22 C1 -177.4(3) . . . . ? C20 C21 C22 C13 1.2(5) . . . . ? C2 C1 C22 C21 -178.3(3) . . . . ? C23 C1 C22 C21 3.5(5) . . . . ? C2 C1 C22 C13 3.1(5) . . . . ? C23 C1 C22 C13 -175.1(3) . . . . ? C14 C13 C22 C21 -2.6(5) . . . . ? C12 C13 C22 C21 179.0(3) . . . . ? C14 C13 C22 C1 176.0(3) . . . . ? C12 C13 C22 C1 -2.3(5) . . . . ? C24 Si1 C25 C29 -69.7(3) . . . . ? C30 Si1 C25 C29 47.8(4) . . . . ? C35 Si1 C25 C29 171.3(3) . . . . ? C24 Si1 C25 C26 51.3(3) . . . . ? C30 Si1 C25 C26 168.8(3) . . . . ? C35 Si1 C25 C26 -67.7(3) . . . . ? C29 C25 C26 C27 -13.7(5) . . . . ? Si1 C25 C26 C27 -140.9(3) . . . . ? C25 C26 C27 C28 -11.7(5) . . . . ? C26 C27 C28 C29 32.7(6) . . . . ? C27 C28 C29 C25 -41.6(5) . . . . ? C26 C25 C29 C28 33.8(4) . . . . ? Si1 C25 C29 C28 160.7(3) . . . . ? C24 Si1 C30 C34' -63.3(9) . . . . ? C25 Si1 C30 C34' 179.2(9) . . . . ? C35 Si1 C30 C34' 53.0(9) . . . . ? C24 Si1 C30 C31 60.1(4) . . . . ? C25 Si1 C30 C31 -57.3(4) . . . . ? C35 Si1 C30 C31 176.4(3) . . . . ? C24 Si1 C30 C34 -55.8(5) . . . . ? C25 Si1 C30 C34 -173.3(5) . . . . ? C35 Si1 C30 C34 60.4(5) . . . . ? C34' C30 C31 C32' -18.7(15) . . . . ? C34 C30 C31 C32' -28.2(8) . . . . ? Si1 C30 C31 C32' -148.6(8) . . . . ? C34' C30 C31 C32 -30.0(10) . . . . ? C34 C30 C31 C32 -39.5(7) . . . . ? Si1 C30 C31 C32 -159.9(4) . . . . ? C32' C31 C32 C33 -87(4) . . . . ? C30 C31 C32 C33 25.2(7) . . . . ? C31 C32 C33 C34 -0.5(8) . . . . ? C32 C33 C34 C30 -24.2(8) . . . . ? C34' C30 C34 C33 -61(4) . . . . ? C31 C30 C34 C33 39.5(8) . . . . ? Si1 C30 C34 C33 164.5(6) . . . . ? C32 C31 C32' C33' 109(4) . . . . ? C30 C31 C32' C33' 38.7(14) . . . . ? C31 C32' C33' C34' -44.0(14) . . . . ? C32' C33' C34' C30 33.9(15) . . . . ? C31 C30 C34' C33' -9.9(15) . . . . ? C34 C30 C34' C33' 71(5) . . . . ? Si1 C30 C34' C33' 120.2(11) . . . . ? C24 Si1 C35 C36 178.1(3) . . . . ? C30 Si1 C35 C36 63.2(3) . . . . ? C25 Si1 C35 C36 -64.3(3) . . . . ? C24 Si1 C35 C39 -60.7(3) . . . . ? C30 Si1 C35 C39 -175.7(3) . . . . ? C25 Si1 C35 C39 56.9(4) . . . . ? C39 C35 C36 C37 29.8(4) . . . . ? Si1 C35 C36 C37 158.9(3) . . . . ? C35 C36 C37 C38 -8.0(4) . . . . ? C36 C37 C38 C39 -17.1(5) . . . . ? C37 C38 C39 C35 35.7(4) . . . . ? C36 C35 C39 C38 -40.3(4) . . . . ? Si1 C35 C39 C38 -167.1(3) . . . . ? C41 Si2 C42 C43 -52.0(3) . . . . ? C52 Si2 C42 C43 -171.0(3) . . . . ? C47 Si2 C42 C43 66.1(4) . . . . ? C41 Si2 C42 C46 -173.0(3) . . . . ? C52 Si2 C42 C46 68.0(4) . . . . ? C47 Si2 C42 C46 -54.8(4) . . . . ? C46 C42 C43 C44 -38.4(4) . . . . ? Si2 C42 C43 C44 -166.1(3) . . . . ? C42 C43 C44 C45 27.8(4) . . . . ? C43 C44 C45 C46 -5.9(5) . . . . ? C44 C45 C46 C42 -18.2(5) . . . . ? C43 C42 C46 C45 35.1(5) . . . . ? Si2 C42 C46 C45 164.0(3) . . . . ? C41 Si2 C47 C48' 48.9(10) . . . . ? C52 Si2 C47 C48' 169.6(10) . . . . ? C42 Si2 C47 C48' -68.5(10) . . . . ? C41 Si2 C47 C48 68.8(7) . . . . ? C52 Si2 C47 C48 -170.5(7) . . . . ? C42 Si2 C47 C48 -48.6(7) . . . . ? C41 Si2 C47 C51 -56.2(15) . . . . ? C52 Si2 C47 C51 64.5(15) . . . . ? C42 Si2 C47 C51 -173.6(15) . . . . ? C41 Si2 C47 C51' -69(2) . . . . ? C52 Si2 C47 C51' 52(2) . . . . ? C42 Si2 C47 C51' 174(2) . . . . ? C48' C47 C48 C49 -70(4) . . . . ? C51 C47 C48 C49 -32.2(18) . . . . ? C51' C47 C48 C49 -27(3) . . . . ? Si2 C47 C48 C49 -163.3(8) . . . . ? C47 C48 C49 C50 37.1(15) . . . . ? C48 C49 C50 C51 -27(2) . . . . ? C49 C50 C51 C47 7(3) . . . . ? C48' C47 C51 C50 27(2) . . . . ? C48 C47 C51 C50 16(3) . . . . ? C51' C47 C51 C50 -144(16) . . . . ? Si2 C47 C51 C50 147.5(16) . . . . ? C48 C47 C48' C49' 107(5) . . . . ? C51 C47 C48' C49' -37(2) . . . . ? C51' C47 C48' C49' -35(3) . . . . ? Si2 C47 C48' C49' -157.4(12) . . . . ? C47 C48' C49' C50' 12(2) . . . . ? C48' C49' C50' C51' 16(3) . . . . ? C49' C50' C51' C47 -37(4) . . . . ? C48' C47 C51' C50' 44(3) . . . . ? C48 C47 C51' C50' 32(4) . . . . ? C51 C47 C51' C50' 54(11) . . . . ? Si2 C47 C51' C50' 170(2) . . . . ? C41 Si2 C52 C56 -75.4(5) . . . . ? C47 Si2 C52 C56 165.4(4) . . . . ? C42 Si2 C52 C56 41.1(5) . . . . ? C41 Si2 C52 C53 43.3(5) . . . . ? C47 Si2 C52 C53 -75.8(5) . . . . ? C42 Si2 C52 C53 159.9(5) . . . . ? C56 C52 C53 C54 -40.9(6) . . . . ? Si2 C52 C53 C54 -166.2(4) . . . . ? C52 C53 C54 C55 31.6(8) . . . . ? C53 C54 C55 C56 -9.4(9) . . . . ? C53 C52 C56 C55 35.3(7) . . . . ? Si2 C52 C56 C55 163.5(5) . . . . ? C54 C55 C56 C52 -16.5(9) . . . . ? C53' C54' C55' C56' 24(5) . . . . ? C5 C6 C57 F2 -15.6(6) . . . . ? C7 C6 C57 F2 168.2(4) . . . . ? C5 C6 C57 F3 105.7(4) . . . . ? C7 C6 C57 F3 -70.5(5) . . . . ? C5 C6 C57 F1 -137.6(4) . . . . ? C7 C6 C57 F1 46.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 68.57 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.612 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.072 # Attachment 'CF3_TIPS.cif' data_k05285 _database_code_depnum_ccdc_archive 'CCDC 796837' #TrackingRef 'CF3_TIPS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H53 F3 Si2' _chemical_formula_sum 'C45 H53 F3 Si2' _chemical_formula_weight 707.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si .0817 .0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0009(2) _cell_length_b 12.9917(3) _cell_length_c 33.9922(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.2183(11) _cell_angle_gamma 90.00 _cell_volume 3951.56(17) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 7455 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.942 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_detector_area_resol_mean 18 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 13454 _diffrn_reflns_av_R_equivalents 0.0924 _diffrn_reflns_av_sigmaI/netI 0.1306 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6976 _reflns_number_gt 3511 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 1994)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures ; _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^)+(0.0733P)^2^] 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 6976 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1525 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1550 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.85885(11) 0.34931(7) -0.06865(3) 0.0254(3) Uani 1 1 d . . . Si2 Si 0.80198(11) -0.08704(8) 0.23318(3) 0.0286(3) Uani 1 1 d . . . C1 C 0.8693(4) 0.1902(2) 0.04845(9) 0.0220(8) Uani 1 1 d . . . C2 C 0.9927(4) 0.1850(2) 0.07717(9) 0.0232(8) Uani 1 1 d . . . C3 C 1.1271(4) 0.2376(2) 0.07292(9) 0.0234(8) Uani 1 1 d . . . H3 H 1.1345 0.2766 0.0496 0.028 Uiso 1 1 calc R . . C4 C 1.2479(4) 0.2345(2) 0.10141(10) 0.0246(9) Uani 1 1 d . . . C5 C 1.3840(4) 0.2919(3) 0.09798(10) 0.0283(9) Uani 1 1 d . . . H5 H 1.3920 0.3327 0.0751 0.034 Uiso 1 1 calc R . . C6 C 1.4997(4) 0.2885(3) 0.12678(10) 0.0255(9) Uani 1 1 d . . . C7 C 1.4929(4) 0.2259(3) 0.16101(10) 0.0308(9) Uani 1 1 d . . . H7 H 1.5761 0.2230 0.1807 0.037 Uiso 1 1 calc R . . C8 C 1.3691(4) 0.1711(3) 0.16547(9) 0.0281(9) Uani 1 1 d . . . H8 H 1.3662 0.1299 0.1885 0.034 Uiso 1 1 calc R . . C9 C 1.2414(4) 0.1732(3) 0.13637(9) 0.0243(8) Uani 1 1 d . . . C10 C 1.1111(4) 0.1205(2) 0.14089(9) 0.0241(8) Uani 1 1 d . . . H10 H 1.1070 0.0792 0.1638 0.029 Uiso 1 1 calc R . . C11 C 0.9841(4) 0.1256(2) 0.11287(9) 0.0213(8) Uani 1 1 d . . . C12 C 0.8483(4) 0.0754(2) 0.11864(9) 0.0211(8) Uani 1 1 d . . . C13 C 0.7234(4) 0.0812(2) 0.08982(8) 0.0205(8) Uani 1 1 d . . . C14 C 0.5880(4) 0.0312(2) 0.09469(9) 0.0241(9) Uani 1 1 d . . . H14 H 0.5814 -0.0087 0.1178 0.029 Uiso 1 1 calc R . . C15 C 0.4643(4) 0.0382(2) 0.06698(9) 0.0218(8) Uani 1 1 d . . . C16 C 0.3252(4) -0.0125(3) 0.07157(9) 0.0269(9) Uani 1 1 d . . . H16 H 0.3171 -0.0532 0.0945 0.032 Uiso 1 1 calc R . . C17 C 0.2065(4) -0.0038(3) 0.04426(10) 0.0287(9) Uani 1 1 d . . . H17 H 0.1164 -0.0387 0.0480 0.034 Uiso 1 1 calc R . . C18 C 0.2139(4) 0.0573(3) 0.00965(9) 0.0278(9) Uani 1 1 d . . . H18 H 0.1289 0.0629 -0.0094 0.033 Uiso 1 1 calc R . . C19 C 0.3421(4) 0.1074(3) 0.00379(9) 0.0271(9) Uani 1 1 d . . . H19 H 0.3456 0.1480 -0.0193 0.033 Uiso 1 1 calc R . . C20 C 0.4716(4) 0.1001(2) 0.03184(9) 0.0213(8) Uani 1 1 d . . . C21 C 0.6052(4) 0.1481(2) 0.02673(9) 0.0239(8) Uani 1 1 d . . . H21 H 0.6111 0.1877 0.0035 0.029 Uiso 1 1 calc R . . C22 C 0.7323(4) 0.1410(2) 0.05427(9) 0.0214(8) Uani 1 1 d . . . C23 C 0.8769(3) 0.2452(2) 0.01198(10) 0.0222(8) Uani 1 1 d . . . C24 C 0.8779(4) 0.2887(3) -0.01956(10) 0.0250(9) Uani 1 1 d . . . C25 C 0.6550(4) 0.3832(3) -0.07950(10) 0.0306(9) Uani 1 1 d . . . H25 H 0.6451 0.4310 -0.1027 0.037 Uiso 1 1 calc R . . C26 C 0.5966(4) 0.4401(3) -0.04462(9) 0.0365(10) Uani 1 1 d . . . H26A H 0.4927 0.4609 -0.0519 0.055 Uiso 1 1 calc R . . H26B H 0.6581 0.5013 -0.0381 0.055 Uiso 1 1 calc R . . H26C H 0.6020 0.3943 -0.0216 0.055 Uiso 1 1 calc R . . C27 C 0.5543(4) 0.2891(3) -0.09050(10) 0.0404(10) Uani 1 1 d . . . H27A H 0.5668 0.2385 -0.0690 0.061 Uiso 1 1 calc R . . H27B H 0.5826 0.2578 -0.1149 0.061 Uiso 1 1 calc R . . H27C H 0.4497 0.3111 -0.0946 0.061 Uiso 1 1 calc R . . C28 C 0.9179(4) 0.2481(3) -0.10316(9) 0.0288(9) Uani 1 1 d . . . H28 H 0.8567 0.1859 -0.0985 0.035 Uiso 1 1 calc R . . C29 C 0.8842(4) 0.2724(3) -0.14735(9) 0.0397(10) Uani 1 1 d . . . H29A H 0.9519 0.3266 -0.1546 0.059 Uiso 1 1 calc R . . H29B H 0.7805 0.2959 -0.1528 0.059 Uiso 1 1 calc R . . H29C H 0.8985 0.2103 -0.1629 0.059 Uiso 1 1 calc R . . C30 C 1.0813(4) 0.2145(3) -0.09365(10) 0.0420(11) Uani 1 1 d . . . H30A H 1.0983 0.1509 -0.1080 0.063 Uiso 1 1 calc R . . H30B H 1.1025 0.2025 -0.0651 0.063 Uiso 1 1 calc R . . H30C H 1.1473 0.2687 -0.1018 0.063 Uiso 1 1 calc R . . C31 C 0.9749(4) 0.4700(3) -0.06584(9) 0.0268(9) Uani 1 1 d . . . H31 H 0.9201 0.5209 -0.0507 0.032 Uiso 1 1 calc R . . C32 C 0.9874(4) 0.5194(3) -0.10642(9) 0.0368(10) Uani 1 1 d . . . H32A H 1.0298 0.5886 -0.1027 0.055 Uiso 1 1 calc R . . H32B H 0.8879 0.5238 -0.1212 0.055 Uiso 1 1 calc R . . H32C H 1.0524 0.4771 -0.1212 0.055 Uiso 1 1 calc R . . C33 C 1.1290(4) 0.4578(3) -0.04276(10) 0.0391(10) Uani 1 1 d . . . H33A H 1.1920 0.4152 -0.0580 0.059 Uiso 1 1 calc R . . H33B H 1.1188 0.4247 -0.0173 0.059 Uiso 1 1 calc R . . H33C H 1.1750 0.5257 -0.0382 0.059 Uiso 1 1 calc R . . C34 C 0.8367(4) 0.0215(3) 0.15509(10) 0.0232(8) Uani 1 1 d . . . C35 C 0.8258(4) -0.0213(3) 0.18616(9) 0.0268(9) Uani 1 1 d . . . C36 C 0.6439(4) -0.1810(3) 0.22198(10) 0.0360(10) Uani 1 1 d . . . H36 H 0.6221 -0.2118 0.2477 0.043 Uiso 1 1 calc R . . C37 C 0.6839(5) -0.2695(3) 0.19532(10) 0.0493(12) Uani 1 1 d . . . H37A H 0.5996 -0.3174 0.1912 0.074 Uiso 1 1 calc R . . H37B H 0.7719 -0.3058 0.2079 0.074 Uiso 1 1 calc R . . H37C H 0.7058 -0.2419 0.1697 0.074 Uiso 1 1 calc R . . C38 C 0.5009(4) -0.1270(3) 0.20390(10) 0.0449(11) Uani 1 1 d . . . H38A H 0.5183 -0.0958 0.1786 0.067 Uiso 1 1 calc R . . H38B H 0.4732 -0.0733 0.2220 0.067 Uiso 1 1 calc R . . H38C H 0.4197 -0.1774 0.1996 0.067 Uiso 1 1 calc R . . C39 C 0.7593(4) 0.0112(3) 0.27123(9) 0.0320(9) Uani 1 1 d . . . H39 H 0.8575 0.0311 0.2858 0.038 Uiso 1 1 calc R . . C40 C 0.6879(4) 0.1114(3) 0.25387(10) 0.0420(11) Uani 1 1 d . . . H40A H 0.5894 0.0962 0.2399 0.063 Uiso 1 1 calc R . . H40B H 0.7520 0.1415 0.2353 0.063 Uiso 1 1 calc R . . H40C H 0.6770 0.1602 0.2753 0.063 Uiso 1 1 calc R . . C41 C 0.6640(4) -0.0315(3) 0.30232(9) 0.0396(10) Uani 1 1 d . . . H41A H 0.6558 0.0204 0.3229 0.059 Uiso 1 1 calc R . . H41B H 0.7113 -0.0936 0.3143 0.059 Uiso 1 1 calc R . . H41C H 0.5641 -0.0486 0.2896 0.059 Uiso 1 1 calc R . . C42 C 0.9817(4) -0.1555(3) 0.24953(10) 0.0362(10) Uani 1 1 d . . . H42 H 0.9991 -0.2052 0.2280 0.043 Uiso 1 1 calc R . . C43 C 0.9691(4) -0.2195(3) 0.28696(10) 0.0478(11) Uani 1 1 d . . . H43A H 1.0607 -0.2597 0.2932 0.072 Uiso 1 1 calc R . . H43B H 0.8834 -0.2662 0.2824 0.072 Uiso 1 1 calc R . . H43C H 0.9550 -0.1735 0.3091 0.072 Uiso 1 1 calc R . . C44 C 1.1176(4) -0.0849(3) 0.25482(11) 0.0518(12) Uani 1 1 d . . . H44A H 1.1042 -0.0338 0.2753 0.078 Uiso 1 1 calc R . . H44B H 1.1286 -0.0498 0.2298 0.078 Uiso 1 1 calc R . . H44C H 1.2073 -0.1259 0.2627 0.078 Uiso 1 1 calc R . . C45 C 1.6344(4) 0.3517(3) 0.12400(10) 0.0341(9) Uani 1 1 d . . . F1 F 1.6523(2) 0.37976(17) 0.08672(6) 0.0485(6) Uani 1 1 d . . . F2 F 1.7613(2) 0.30512(16) 0.13817(6) 0.0438(6) Uani 1 1 d . . . F3 F 1.6312(2) 0.44061(16) 0.14448(7) 0.0552(7) 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 0.0251(6) 0.0300(6) 0.0222(5) 0.0021(4) 0.0067(4) -0.0029(5) Si2 0.0286(6) 0.0350(7) 0.0233(5) 0.0026(5) 0.0084(4) -0.0025(5) C1 0.023(2) 0.024(2) 0.0197(18) 0.0005(15) 0.0070(16) 0.0020(17) C2 0.021(2) 0.023(2) 0.0270(19) -0.0054(16) 0.0092(17) -0.0031(17) C3 0.023(2) 0.026(2) 0.0215(18) 0.0030(15) 0.0074(16) 0.0026(18) C4 0.020(2) 0.022(2) 0.033(2) -0.0069(16) 0.0098(17) 0.0008(17) C5 0.028(2) 0.023(2) 0.035(2) -0.0013(16) 0.0106(19) 0.0013(18) C6 0.012(2) 0.032(2) 0.034(2) -0.0037(17) 0.0081(17) -0.0045(17) C7 0.023(2) 0.039(2) 0.031(2) -0.0010(18) 0.0028(17) -0.0003(19) C8 0.023(2) 0.041(2) 0.0205(18) -0.0016(16) 0.0061(17) 0.0000(19) C9 0.023(2) 0.025(2) 0.0256(19) -0.0034(16) 0.0080(17) 0.0015(18) C10 0.024(2) 0.027(2) 0.0230(19) -0.0015(15) 0.0102(16) -0.0012(18) C11 0.019(2) 0.027(2) 0.0195(18) -0.0025(15) 0.0074(16) 0.0008(17) C12 0.021(2) 0.024(2) 0.0200(17) -0.0003(15) 0.0113(15) 0.0015(17) C13 0.020(2) 0.022(2) 0.0205(18) -0.0010(15) 0.0054(15) 0.0000(17) C14 0.029(2) 0.025(2) 0.0198(18) 0.0005(15) 0.0078(17) -0.0009(18) C15 0.021(2) 0.025(2) 0.0198(18) -0.0035(15) 0.0065(16) -0.0029(17) C16 0.031(2) 0.028(2) 0.0232(19) 0.0002(16) 0.0074(17) -0.0030(18) C17 0.020(2) 0.033(2) 0.035(2) -0.0033(18) 0.0098(18) -0.0020(18) C18 0.022(2) 0.034(2) 0.0266(19) -0.0040(17) -0.0018(16) 0.0033(19) C19 0.025(2) 0.031(2) 0.0263(19) -0.0036(16) 0.0062(17) 0.0015(19) C20 0.019(2) 0.022(2) 0.0247(18) -0.0014(15) 0.0084(16) 0.0029(17) C21 0.026(2) 0.025(2) 0.0223(18) 0.0012(15) 0.0099(16) -0.0003(18) C22 0.020(2) 0.025(2) 0.0198(18) -0.0021(15) 0.0045(16) 0.0008(17) C23 0.010(2) 0.029(2) 0.028(2) -0.0065(17) 0.0045(15) 0.0002(16) C24 0.017(2) 0.032(2) 0.028(2) -0.0017(17) 0.0075(16) -0.0018(17) C25 0.031(2) 0.034(2) 0.029(2) 0.0038(17) 0.0084(17) 0.0006(19) C26 0.028(2) 0.045(3) 0.038(2) 0.0029(19) 0.0058(17) 0.010(2) C27 0.028(2) 0.054(3) 0.040(2) -0.003(2) 0.0027(18) -0.001(2) C28 0.030(2) 0.032(2) 0.0258(19) -0.0007(16) 0.0063(17) -0.0070(18) C29 0.053(3) 0.041(3) 0.027(2) -0.0053(18) 0.0113(19) -0.006(2) C30 0.040(3) 0.045(3) 0.043(2) -0.0055(19) 0.010(2) 0.006(2) C31 0.026(2) 0.029(2) 0.0269(19) -0.0019(16) 0.0077(16) 0.0016(18) C32 0.040(3) 0.037(2) 0.035(2) 0.0078(18) 0.0096(18) -0.005(2) C33 0.042(3) 0.043(3) 0.033(2) -0.0013(19) 0.0091(19) -0.014(2) C34 0.017(2) 0.025(2) 0.028(2) -0.0029(17) 0.0014(16) -0.0036(16) C35 0.020(2) 0.035(2) 0.026(2) -0.0016(17) 0.0051(16) -0.0007(18) C36 0.039(3) 0.041(2) 0.028(2) 0.0029(18) 0.0079(18) -0.011(2) C37 0.062(3) 0.045(3) 0.043(2) -0.014(2) 0.015(2) -0.017(2) C38 0.041(3) 0.060(3) 0.033(2) 0.007(2) 0.0054(19) -0.018(2) C39 0.029(2) 0.040(2) 0.027(2) 0.0012(17) 0.0056(17) -0.0043(19) C40 0.046(3) 0.049(3) 0.032(2) 0.0012(19) 0.0060(19) 0.007(2) C41 0.045(3) 0.050(3) 0.027(2) 0.0036(18) 0.0167(18) 0.001(2) C42 0.039(3) 0.045(3) 0.0272(19) 0.0043(18) 0.0124(18) 0.006(2) C43 0.042(3) 0.063(3) 0.039(2) 0.010(2) 0.008(2) 0.009(2) C44 0.027(2) 0.071(3) 0.058(3) 0.016(2) 0.005(2) -0.003(2) C45 0.030(3) 0.037(3) 0.035(2) -0.0041(19) 0.0054(19) 0.001(2) F1 0.0365(14) 0.0661(16) 0.0436(13) 0.0165(11) 0.0071(11) -0.0130(12) F2 0.0239(13) 0.0492(14) 0.0578(14) 0.0070(11) 0.0020(11) 0.0005(11) F3 0.0399(15) 0.0442(15) 0.0850(17) -0.0229(13) 0.0229(12) -0.0126(12) _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 C24 1.836(3) . ? Si1 C28 1.877(3) . ? Si1 C31 1.881(3) . ? Si1 C25 1.884(3) . ? Si2 C35 1.845(3) . ? Si2 C42 1.877(4) . ? Si2 C36 1.883(4) . ? Si2 C39 1.886(3) . ? C1 C2 1.399(4) . ? C1 C22 1.422(4) . ? C1 C23 1.439(4) . ? C2 C3 1.411(4) . ? C2 C11 1.448(4) . ? C3 C4 1.376(4) . ? C3 H3 0.9500 . ? C4 C9 1.437(4) . ? C4 C5 1.450(4) . ? C5 C6 1.350(4) . ? C5 H5 0.9500 . ? C6 C7 1.426(4) . ? C6 C45 1.475(5) . ? C7 C8 1.346(4) . ? C7 H7 0.9500 . ? C8 C9 1.433(4) . ? C8 H8 0.9500 . ? C9 C10 1.381(4) . ? C10 C11 1.408(4) . ? C10 H10 0.9500 . ? C11 C12 1.418(4) . ? C12 C13 1.411(4) . ? C12 C34 1.436(4) . ? C13 C14 1.406(4) . ? C13 C22 1.446(4) . ? C14 C15 1.382(4) . ? C14 H14 0.9500 . ? C15 C16 1.439(4) . ? C15 C20 1.447(4) . ? C16 C17 1.342(4) . ? C16 H16 0.9500 . ? C17 C18 1.427(4) . ? C17 H17 0.9500 . ? C18 C19 1.358(4) . ? C18 H18 0.9500 . ? C19 C20 1.427(4) . ? C19 H19 0.9500 . ? C20 C21 1.382(4) . ? C21 C22 1.401(4) . ? C21 H21 0.9500 . ? C23 C24 1.213(4) . ? C25 C26 1.537(4) . ? C25 C27 1.544(5) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.533(4) . ? C28 C30 1.534(5) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.526(4) . ? C31 C32 1.536(4) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.207(4) . ? C36 C37 1.531(5) . ? C36 C38 1.535(5) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.535(4) . ? C39 C40 1.541(5) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C44 1.523(5) . ? C42 C43 1.535(4) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 F2 1.336(4) . ? C45 F1 1.345(4) . ? C45 F3 1.351(4) . ? 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 C24 Si1 C28 105.23(15) . . ? C24 Si1 C31 108.34(14) . . ? C28 Si1 C31 115.01(15) . . ? C24 Si1 C25 105.73(15) . . ? C28 Si1 C25 112.15(15) . . ? C31 Si1 C25 109.80(15) . . ? C35 Si2 C42 107.36(15) . . ? C35 Si2 C36 106.33(15) . . ? C42 Si2 C36 111.17(17) . . ? C35 Si2 C39 109.42(15) . . ? C42 Si2 C39 110.52(16) . . ? C36 Si2 C39 111.84(16) . . ? C2 C1 C22 121.1(3) . . ? C2 C1 C23 121.1(3) . . ? C22 C1 C23 117.8(3) . . ? C1 C2 C3 122.0(3) . . ? C1 C2 C11 120.0(3) . . ? C3 C2 C11 117.9(3) . . ? C4 C3 C2 122.3(3) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C9 119.9(3) . . ? C3 C4 C5 122.6(3) . . ? C9 C4 C5 117.5(3) . . ? C6 C5 C4 121.1(3) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 120.8(3) . . ? C5 C6 C45 120.6(3) . . ? C7 C6 C45 118.5(3) . . ? C8 C7 C6 120.2(3) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 121.6(3) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C10 C9 C8 122.7(3) . . ? C10 C9 C4 118.6(3) . . ? C8 C9 C4 118.7(3) . . ? C9 C10 C11 122.6(3) . . ? C9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C10 C11 C12 122.3(3) . . ? C10 C11 C2 118.7(3) . . ? C12 C11 C2 119.1(3) . . ? C13 C12 C11 120.9(3) . . ? C13 C12 C34 119.9(3) . . ? C11 C12 C34 119.2(3) . . ? C14 C13 C12 121.9(3) . . ? C14 C13 C22 118.3(3) . . ? C12 C13 C22 119.8(3) . . ? C15 C14 C13 122.3(3) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 C15 C16 122.9(3) . . ? C14 C15 C20 119.6(3) . . ? C16 C15 C20 117.5(3) . . ? C17 C16 C15 121.5(3) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 120.8(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 120.3(3) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 121.0(3) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 123.0(3) . . ? C21 C20 C15 118.2(3) . . ? C19 C20 C15 118.8(3) . . ? C20 C21 C22 123.0(3) . . ? C20 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C21 C22 C1 122.4(3) . . ? C21 C22 C13 118.6(3) . . ? C1 C22 C13 119.0(3) . . ? C24 C23 C1 176.9(4) . . ? C23 C24 Si1 173.8(3) . . ? C26 C25 C27 109.1(3) . . ? C26 C25 Si1 111.6(2) . . ? C27 C25 Si1 113.3(2) . . ? C26 C25 H25 107.5 . . ? C27 C25 H25 107.5 . . ? Si1 C25 H25 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 110.4(3) . . ? C29 C28 Si1 115.4(2) . . ? C30 C28 Si1 113.4(2) . . ? C29 C28 H28 105.6 . . ? C30 C28 H28 105.6 . . ? Si1 C28 H28 105.6 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C32 110.7(3) . . ? C33 C31 Si1 114.1(2) . . ? C32 C31 Si1 113.4(2) . . ? C33 C31 H31 106.0 . . ? C32 C31 H31 106.0 . . ? Si1 C31 H31 106.0 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C12 178.3(4) . . ? C34 C35 Si2 178.0(3) . . ? C37 C36 C38 110.3(3) . . ? C37 C36 Si2 112.7(3) . . ? C38 C36 Si2 111.5(3) . . ? C37 C36 H36 107.3 . . ? C38 C36 H36 107.3 . . ? Si2 C36 H36 107.3 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 C39 C40 109.1(3) . . ? C41 C39 Si2 113.4(2) . . ? C40 C39 Si2 114.6(2) . . ? C41 C39 H39 106.3 . . ? C40 C39 H39 106.3 . . ? Si2 C39 H39 106.3 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C44 C42 C43 111.0(3) . . ? C44 C42 Si2 113.9(3) . . ? C43 C42 Si2 111.3(2) . . ? C44 C42 H42 106.7 . . ? C43 C42 H42 106.7 . . ? Si2 C42 H42 106.7 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? F2 C45 F1 106.1(3) . . ? F2 C45 F3 105.4(3) . . ? F1 C45 F3 105.4(3) . . ? F2 C45 C6 113.6(3) . . ? F1 C45 C6 113.2(3) . . ? F3 C45 C6 112.3(3) . . ? 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 C22 C1 C2 C3 -176.7(3) . . . . ? C23 C1 C2 C3 3.5(5) . . . . ? C22 C1 C2 C11 2.4(5) . . . . ? C23 C1 C2 C11 -177.4(3) . . . . ? C1 C2 C3 C4 178.7(3) . . . . ? C11 C2 C3 C4 -0.4(5) . . . . ? C2 C3 C4 C9 2.2(5) . . . . ? C2 C3 C4 C5 -177.3(3) . . . . ? C3 C4 C5 C6 179.0(3) . . . . ? C9 C4 C5 C6 -0.6(5) . . . . ? C4 C5 C6 C7 1.7(5) . . . . ? C4 C5 C6 C45 -176.6(3) . . . . ? C5 C6 C7 C8 -1.5(5) . . . . ? C45 C6 C7 C8 176.8(3) . . . . ? C6 C7 C8 C9 0.1(5) . . . . ? C7 C8 C9 C10 -177.7(3) . . . . ? C7 C8 C9 C4 1.0(5) . . . . ? C3 C4 C9 C10 -1.6(5) . . . . ? C5 C4 C9 C10 178.0(3) . . . . ? C3 C4 C9 C8 179.7(3) . . . . ? C5 C4 C9 C8 -0.7(4) . . . . ? C8 C9 C10 C11 177.8(3) . . . . ? C4 C9 C10 C11 -0.8(5) . . . . ? C9 C10 C11 C12 -176.8(3) . . . . ? C9 C10 C11 C2 2.6(5) . . . . ? C1 C2 C11 C10 178.9(3) . . . . ? C3 C2 C11 C10 -1.9(4) . . . . ? C1 C2 C11 C12 -1.7(5) . . . . ? C3 C2 C11 C12 177.4(3) . . . . ? C10 C11 C12 C13 -179.4(3) . . . . ? C2 C11 C12 C13 1.2(5) . . . . ? C10 C11 C12 C34 3.1(5) . . . . ? C2 C11 C12 C34 -176.3(3) . . . . ? C11 C12 C13 C14 179.3(3) . . . . ? C34 C12 C13 C14 -3.2(5) . . . . ? C11 C12 C13 C22 -1.5(5) . . . . ? C34 C12 C13 C22 176.0(3) . . . . ? C12 C13 C14 C15 178.7(3) . . . . ? C22 C13 C14 C15 -0.6(5) . . . . ? C13 C14 C15 C16 179.9(3) . . . . ? C13 C14 C15 C20 -1.0(5) . . . . ? C14 C15 C16 C17 179.6(3) . . . . ? C20 C15 C16 C17 0.4(5) . . . . ? C15 C16 C17 C18 -0.5(5) . . . . ? C16 C17 C18 C19 0.2(5) . . . . ? C17 C18 C19 C20 0.1(5) . . . . ? C18 C19 C20 C21 178.7(3) . . . . ? C18 C19 C20 C15 -0.2(5) . . . . ? C14 C15 C20 C21 1.8(4) . . . . ? C16 C15 C20 C21 -179.1(3) . . . . ? C14 C15 C20 C19 -179.2(3) . . . . ? C16 C15 C20 C19 -0.1(4) . . . . ? C19 C20 C21 C22 179.9(3) . . . . ? C15 C20 C21 C22 -1.1(5) . . . . ? C20 C21 C22 C1 179.5(3) . . . . ? C20 C21 C22 C13 -0.4(5) . . . . ? C2 C1 C22 C21 177.5(3) . . . . ? C23 C1 C22 C21 -2.7(5) . . . . ? C2 C1 C22 C13 -2.6(5) . . . . ? C23 C1 C22 C13 177.2(3) . . . . ? C14 C13 C22 C21 1.2(4) . . . . ? C12 C13 C22 C21 -178.0(3) . . . . ? C14 C13 C22 C1 -178.7(3) . . . . ? C12 C13 C22 C1 2.1(4) . . . . ? C2 C1 C23 C24 155(7) . . . . ? C22 C1 C23 C24 -24(7) . . . . ? C1 C23 C24 Si1 21(9) . . . . ? C28 Si1 C24 C23 -87(3) . . . . ? C31 Si1 C24 C23 149(3) . . . . ? C25 Si1 C24 C23 32(3) . . . . ? C24 Si1 C25 C26 48.9(3) . . . . ? C28 Si1 C25 C26 163.0(2) . . . . ? C31 Si1 C25 C26 -67.8(3) . . . . ? C24 Si1 C25 C27 -74.8(3) . . . . ? C28 Si1 C25 C27 39.4(3) . . . . ? C31 Si1 C25 C27 168.6(2) . . . . ? C24 Si1 C28 C29 168.9(3) . . . . ? C31 Si1 C28 C29 -72.0(3) . . . . ? C25 Si1 C28 C29 54.4(3) . . . . ? C24 Si1 C28 C30 -62.4(3) . . . . ? C31 Si1 C28 C30 56.8(3) . . . . ? C25 Si1 C28 C30 -176.8(2) . . . . ? C24 Si1 C31 C33 43.3(3) . . . . ? C28 Si1 C31 C33 -74.1(3) . . . . ? C25 Si1 C31 C33 158.3(2) . . . . ? C24 Si1 C31 C32 171.3(2) . . . . ? C28 Si1 C31 C32 53.9(3) . . . . ? C25 Si1 C31 C32 -73.7(3) . . . . ? C13 C12 C34 C35 -91(12) . . . . ? C11 C12 C34 C35 87(12) . . . . ? C12 C34 C35 Si2 79(16) . . . . ? C42 Si2 C35 C34 155(9) . . . . ? C36 Si2 C35 C34 36(9) . . . . ? C39 Si2 C35 C34 -85(9) . . . . ? C35 Si2 C36 C37 68.1(3) . . . . ? C42 Si2 C36 C37 -48.5(3) . . . . ? C39 Si2 C36 C37 -172.6(2) . . . . ? C35 Si2 C36 C38 -56.7(3) . . . . ? C42 Si2 C36 C38 -173.2(2) . . . . ? C39 Si2 C36 C38 62.7(3) . . . . ? C35 Si2 C39 C41 151.1(2) . . . . ? C42 Si2 C39 C41 -90.9(3) . . . . ? C36 Si2 C39 C41 33.5(3) . . . . ? C35 Si2 C39 C40 24.8(3) . . . . ? C42 Si2 C39 C40 142.8(3) . . . . ? C36 Si2 C39 C40 -92.8(3) . . . . ? C35 Si2 C42 C44 57.9(3) . . . . ? C36 Si2 C42 C44 173.8(2) . . . . ? C39 Si2 C42 C44 -61.4(3) . . . . ? C35 Si2 C42 C43 -175.7(3) . . . . ? C36 Si2 C42 C43 -59.8(3) . . . . ? C39 Si2 C42 C43 65.1(3) . . . . ? C5 C6 C45 F2 -143.6(3) . . . . ? C7 C6 C45 F2 38.1(4) . . . . ? C5 C6 C45 F1 -22.4(5) . . . . ? C7 C6 C45 F1 159.3(3) . . . . ? C5 C6 C45 F3 96.8(4) . . . . ? C7 C6 C45 F3 -81.5(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max .341 _refine_diff_density_min -.264 _refine_diff_density_rms .063 # Attachment 'Nitro_TIPS.cif' data_x09015 _database_code_depnum_ccdc_archive 'CCDC 796838' #TrackingRef 'Nitro_TIPS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H53 N O2 Si2' _chemical_formula_sum 'C44 H53 N O2 Si2' _chemical_formula_weight 684.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3935(2) _cell_length_b 7.7475(2) _cell_length_c 17.3713(4) _cell_angle_alpha 96.230(1) _cell_angle_beta 100.619(1) _cell_angle_gamma 94.648(1) _cell_volume 967.02(4) _cell_formula_units_Z 1 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 6169 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 68.48 _exptl_crystal_description lath _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 1.108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.594 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details 'Sadabs in APEX2 (BrukerAXS, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator 'graded multilayer optics' _diffrn_measurement_device_type 'Bruker X8 Proteum diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 13133 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 68.48 _reflns_number_total 3491 _reflns_number_gt 3049 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 2008)' _computing_publication_material ; SHELX-97 (Sheldrick, 2008) and local procedures ; _publ_section_exptl_refinement ; H atoms were found in difference Fourier maps and subsequently placed in idealized positions with constrained distances of 0.98 \%A (RCH~3~), 1.00 \%A (R~3~CH), 0.95 \%A (C~Ar~H), and with U~iso~(H) values set to either 1.2U~eq~ or 1.5U~eq~ (RCH~3~) of the attached atom. ; _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^ > 2\s(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^)+(0.0646P)^2^+2.1061P] 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 3491 _refine_ls_number_parameters 255 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.1962 _refine_ls_wR_factor_gt 0.1900 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.073 _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 0.23629(12) 0.67094(13) 0.17917(5) 0.0319(3) Uani 1 1 d . . . C1 C 0.4420(4) 0.5326(4) 0.42046(18) 0.0276(7) Uani 1 1 d . . . C2 C 0.3398(4) 0.5882(4) 0.47851(18) 0.0267(6) Uani 1 1 d . . . C3 C 0.1795(4) 0.6718(4) 0.45902(19) 0.0293(7) Uani 1 1 d . . . H3 H 0.1403 0.6930 0.4060 0.035 Uiso 1 1 calc R . . C4 C 0.0755(4) 0.7249(4) 0.5149(2) 0.0311(7) Uani 1 1 d . . . C5 C -0.0904(5) 0.8046(4) 0.4940(2) 0.0353(8) Uani 1 1 d U A . H5 H -0.1325 0.8240 0.4409 0.042 Uiso 1 1 calc R . . C6 C -0.1888(5) 0.8531(4) 0.5504(2) 0.0382(8) Uani 1 1 d DU . . H6 H -0.3010 0.9035 0.5355 0.046 Uiso 0.564(3) 1 calc PR A 2 N1 N -0.3529(8) 0.9336(8) 0.5257(4) 0.0310(13) Uani 0.436(3) 1 d PDU A 1 O1 O -0.4050(7) 0.9488(7) 0.4551(3) 0.0369(13) Uani 0.436(3) 1 d PDU . 1 O2 O -0.4374(7) 0.9842(7) 0.5783(4) 0.0380(13) Uani 0.436(3) 1 d PDU . 1 C7 C -0.1284(5) 0.8306(5) 0.6302(2) 0.0405(8) Uani 1 1 d DU A . H7 H -0.1984 0.8679 0.6685 0.049 Uiso 0.936(3) 1 calc PR B 1 N1' N -0.285(4) 0.872(6) 0.6620(19) 0.049(5) Uiso 0.064(3) 1 d PDU A 2 O1' O -0.389(4) 0.974(5) 0.631(2) 0.053(8) Uiso 0.064(3) 1 d PDU A 2 O2' O -0.277(7) 0.837(8) 0.731(2) 0.087(14) Uiso 0.064(3) 1 d PDU A 2 C8 C 0.0293(5) 0.7556(5) 0.6524(2) 0.0385(8) Uani 1 1 d U . . H8 H 0.0686 0.7403 0.7062 0.046 Uiso 1 1 calc R A . C9 C 0.1378(5) 0.6989(4) 0.5955(2) 0.0320(7) Uani 1 1 d . A . C10 C 0.2967(4) 0.6176(4) 0.61583(19) 0.0313(7) Uani 1 1 d . . . H10 H 0.3377 0.6008 0.6694 0.038 Uiso 1 1 calc R A . C11 C 0.3992(4) 0.5591(4) 0.55912(18) 0.0271(7) Uani 1 1 d . . . C12 C 0.3834(4) 0.5665(4) 0.34152(19) 0.0295(7) Uani 1 1 d . . . C13 C 0.3293(4) 0.6003(5) 0.27515(19) 0.0334(7) Uani 1 1 d . . . C14 C 0.1953(5) 0.4727(5) 0.1027(2) 0.0392(8) Uani 1 1 d . . . H14 H 0.1424 0.5110 0.0508 0.047 Uiso 1 1 calc R . . C15 C 0.0558(6) 0.3309(6) 0.1194(3) 0.0524(10) Uani 1 1 d . . . H15A H 0.0402 0.2306 0.0784 0.079 Uiso 1 1 calc R . . H15B H -0.0635 0.3776 0.1194 0.079 Uiso 1 1 calc R . . H15C H 0.1014 0.2940 0.1710 0.079 Uiso 1 1 calc R . . C16 C 0.3769(6) 0.3985(5) 0.0945(2) 0.0451(9) Uani 1 1 d . . . H16A H 0.4374 0.3683 0.1457 0.068 Uiso 1 1 calc R . . H16B H 0.4583 0.4859 0.0769 0.068 Uiso 1 1 calc R . . H16C H 0.3516 0.2936 0.0557 0.068 Uiso 1 1 calc R . . C17 C 0.4207(5) 0.8303(5) 0.1573(2) 0.0369(8) Uani 1 1 d . . . H17 H 0.5345 0.7677 0.1607 0.044 Uiso 1 1 calc R . . C18 C 0.3815(5) 0.8821(6) 0.0738(2) 0.0444(9) Uani 1 1 d . . . H18A H 0.2799 0.9565 0.0690 0.067 Uiso 1 1 calc R . . H18B H 0.3467 0.7769 0.0354 0.067 Uiso 1 1 calc R . . H18C H 0.4926 0.9463 0.0636 0.067 Uiso 1 1 calc R . . C19 C 0.4717(6) 0.9907(5) 0.2191(2) 0.0476(9) Uani 1 1 d . . . H19A H 0.5831 1.0572 0.2105 0.071 Uiso 1 1 calc R . . H19B H 0.4954 0.9537 0.2719 0.071 Uiso 1 1 calc R . . H19C H 0.3694 1.0642 0.2147 0.071 Uiso 1 1 calc R . . C20 C 0.0201(5) 0.7782(6) 0.1904(2) 0.0471(9) Uani 1 1 d . . . H20 H 0.0624 0.8958 0.2211 0.056 Uiso 1 1 calc R . . C21 C -0.0933(5) 0.8099(6) 0.1110(3) 0.0522(11) Uani 1 1 d . . . H21A H -0.1440 0.6976 0.0799 0.078 Uiso 1 1 calc R . . H21B H -0.0136 0.8741 0.0822 0.078 Uiso 1 1 calc R . . H21C H -0.1949 0.8783 0.1202 0.078 Uiso 1 1 calc R . . C22 C -0.1048(6) 0.6821(8) 0.2374(3) 0.0709(16) Uani 1 1 d . . . H22A H -0.1858 0.7629 0.2574 0.106 Uiso 1 1 calc R . . H22B H -0.0278 0.6385 0.2818 0.106 Uiso 1 1 calc R . . H22C H -0.1804 0.5838 0.2028 0.106 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 0.0230(5) 0.0413(5) 0.0331(5) 0.0097(4) 0.0054(3) 0.0067(4) C1 0.0206(15) 0.0279(16) 0.0341(16) 0.0052(12) 0.0054(12) 0.0001(12) C2 0.0213(15) 0.0237(16) 0.0354(16) 0.0053(12) 0.0066(12) 0.0003(12) C3 0.0235(16) 0.0275(16) 0.0375(17) 0.0083(12) 0.0056(13) 0.0014(13) C4 0.0214(16) 0.0249(16) 0.0474(19) 0.0033(13) 0.0097(13) -0.0003(12) C5 0.0244(16) 0.0272(17) 0.055(2) 0.0081(14) 0.0081(14) 0.0011(13) C6 0.0243(16) 0.0272(17) 0.065(2) 0.0034(15) 0.0142(15) 0.0044(13) N1 0.023(3) 0.023(3) 0.051(3) 0.006(2) 0.013(2) 0.004(2) O1 0.024(3) 0.040(3) 0.046(3) 0.004(2) 0.008(2) 0.003(2) O2 0.028(3) 0.039(3) 0.054(3) 0.005(2) 0.022(2) 0.011(2) C7 0.0323(18) 0.0354(19) 0.056(2) -0.0017(15) 0.0184(15) 0.0017(15) C8 0.0300(18) 0.040(2) 0.047(2) 0.0015(15) 0.0155(15) 0.0020(15) C9 0.0261(17) 0.0280(17) 0.0434(18) 0.0021(13) 0.0126(14) 0.0014(13) C10 0.0243(16) 0.0355(18) 0.0353(17) 0.0055(13) 0.0090(13) 0.0026(13) C11 0.0213(15) 0.0272(16) 0.0332(16) 0.0044(12) 0.0074(12) -0.0013(12) C12 0.0219(16) 0.0308(17) 0.0369(18) 0.0063(13) 0.0081(13) 0.0007(13) C13 0.0207(16) 0.043(2) 0.0374(18) 0.0082(14) 0.0083(13) 0.0008(14) C14 0.0363(19) 0.043(2) 0.0392(19) 0.0108(15) 0.0050(15) 0.0083(16) C15 0.046(2) 0.046(2) 0.062(3) 0.0059(18) 0.0051(19) -0.0002(18) C16 0.045(2) 0.045(2) 0.046(2) 0.0055(16) 0.0085(17) 0.0134(18) C17 0.0272(17) 0.046(2) 0.0412(19) 0.0127(15) 0.0091(14) 0.0093(15) C18 0.0334(19) 0.058(2) 0.049(2) 0.0211(18) 0.0143(16) 0.0113(17) C19 0.047(2) 0.044(2) 0.054(2) 0.0097(17) 0.0135(18) 0.0025(18) C20 0.0293(19) 0.061(3) 0.049(2) 0.0005(18) 0.0051(16) 0.0100(17) C21 0.0287(19) 0.068(3) 0.068(3) 0.032(2) 0.0133(18) 0.0136(19) C22 0.032(2) 0.146(5) 0.046(2) 0.035(3) 0.0126(18) 0.030(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C13 1.841(3) . ? Si1 C17 1.884(4) . ? Si1 C14 1.884(4) . ? Si1 C20 1.891(4) . ? C1 C2 1.419(4) . ? C1 C12 1.420(4) . ? C1 C11 1.430(4) 2_666 ? C2 C3 1.401(4) . ? C2 C11 1.436(4) . ? C3 C4 1.394(5) . ? C3 H3 0.9500 . ? C4 C5 1.424(5) . ? C4 C9 1.432(5) . ? C5 C6 1.362(5) . ? C5 H5 0.9500 . ? C6 C7 1.410(5) . ? C6 N1 1.426(7) . ? C6 H6 0.9500 . ? N1 O1 1.237(8) . ? N1 O2 1.246(8) . ? O1 O2 1.371(8) 2_476 ? O2 O1 1.371(8) 2_476 ? C7 C8 1.356(5) . ? C7 N1' 1.419(12) . ? C7 H7 0.9500 . ? N1' O1' 1.238(13) . ? N1' O2' 1.246(12) . ? C8 C9 1.438(5) . ? C8 H8 0.9500 . ? C9 C10 1.385(5) . ? C10 C11 1.408(4) . ? C10 H10 0.9500 . ? C11 C1 1.430(4) 2_666 ? C12 C13 1.212(5) . ? C14 C16 1.527(5) . ? C14 C15 1.533(6) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.525(5) . ? C17 C18 1.528(5) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.532(5) . ? C20 C22 1.540(6) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 C13 Si1 C17 106.72(15) . . ? C13 Si1 C14 107.62(16) . . ? C17 Si1 C14 109.35(16) . . ? C13 Si1 C20 107.01(16) . . ? C17 Si1 C20 111.61(18) . . ? C14 Si1 C20 114.15(17) . . ? C2 C1 C12 119.3(3) . . ? C2 C1 C11 120.4(3) . 2_666 ? C12 C1 C11 120.3(3) . 2_666 ? C3 C2 C1 121.3(3) . . ? C3 C2 C11 118.5(3) . . ? C1 C2 C11 120.2(3) . . ? C4 C3 C2 122.1(3) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 121.7(3) . . ? C3 C4 C9 119.1(3) . . ? C5 C4 C9 119.2(3) . . ? C6 C5 C4 119.8(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 121.7(3) . . ? C5 C6 N1 117.1(4) . . ? C7 C6 N1 121.1(4) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? N1 C6 H6 2.8 . . ? O1 N1 O2 123.6(6) . . ? O1 N1 C6 119.9(5) . . ? O2 N1 C6 116.5(6) . . ? N1 O1 O2 127.1(5) . 2_476 ? N1 O2 O1 109.3(6) . 2_476 ? C8 C7 C6 120.1(3) . . ? C8 C7 N1' 137.9(12) . . ? C6 C7 N1' 100.9(13) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? N1' C7 H7 21.3 . . ? O1' N1' O2' 124.4(19) . . ? O1' N1' C7 119.7(17) . . ? O2' N1' C7 113.3(16) . . ? C7 C8 C9 120.9(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C4 119.4(3) . . ? C10 C9 C8 122.3(3) . . ? C4 C9 C8 118.2(3) . . ? C9 C10 C11 121.7(3) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C1 121.5(3) . 2_666 ? C10 C11 C2 119.2(3) . . ? C1 C11 C2 119.3(3) 2_666 . ? C13 C12 C1 177.5(4) . . ? C12 C13 Si1 173.9(3) . . ? C16 C14 C15 110.5(3) . . ? C16 C14 Si1 111.0(3) . . ? C15 C14 Si1 112.6(3) . . ? C16 C14 H14 107.5 . . ? C15 C14 H14 107.5 . . ? Si1 C14 H14 107.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 111.2(3) . . ? C19 C17 Si1 113.1(2) . . ? C18 C17 Si1 114.4(3) . . ? C19 C17 H17 105.7 . . ? C18 C17 H17 105.7 . . ? Si1 C17 H17 105.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 110.0(3) . . ? C21 C20 Si1 112.5(3) . . ? C22 C20 Si1 114.3(3) . . ? C21 C20 H20 106.5 . . ? C22 C20 H20 106.5 . . ? Si1 C20 H20 106.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 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 C12 C1 C2 C3 1.8(5) . . . . ? C11 C1 C2 C3 -177.3(3) 2_666 . . . ? C12 C1 C2 C11 -178.4(3) . . . . ? C11 C1 C2 C11 2.5(5) 2_666 . . . ? C1 C2 C3 C4 178.9(3) . . . . ? C11 C2 C3 C4 -0.9(5) . . . . ? C2 C3 C4 C5 -177.9(3) . . . . ? C2 C3 C4 C9 2.2(5) . . . . ? C3 C4 C5 C6 179.4(3) . . . . ? C9 C4 C5 C6 -0.8(5) . . . . ? C4 C5 C6 C7 1.6(5) . . . . ? C4 C5 C6 N1 179.5(4) . . . . ? C5 C6 N1 O1 3.5(7) . . . . ? C7 C6 N1 O1 -178.6(5) . . . . ? C5 C6 N1 O2 -177.0(5) . . . . ? C7 C6 N1 O2 0.9(7) . . . . ? O2 N1 O1 O2 -2.4(11) . . . 2_476 ? C6 N1 O1 O2 177.1(5) . . . 2_476 ? O1 N1 O2 O1 2.0(10) . . . 2_476 ? C6 N1 O2 O1 -177.5(5) . . . 2_476 ? C5 C6 C7 C8 -1.4(5) . . . . ? N1 C6 C7 C8 -179.2(4) . . . . ? C5 C6 C7 N1' -171(2) . . . . ? N1 C6 C7 N1' 11(2) . . . . ? C8 C7 N1' O1' 166(3) . . . . ? C6 C7 N1' O1' -27(5) . . . . ? C8 C7 N1' O2' 3(6) . . . . ? C6 C7 N1' O2' 170(4) . . . . ? C6 C7 C8 C9 0.3(5) . . . . ? N1' C7 C8 C9 165(3) . . . . ? C3 C4 C9 C10 -1.7(5) . . . . ? C5 C4 C9 C10 178.4(3) . . . . ? C3 C4 C9 C8 179.6(3) . . . . ? C5 C4 C9 C8 -0.2(5) . . . . ? C7 C8 C9 C10 -178.2(3) . . . . ? C7 C8 C9 C4 0.4(5) . . . . ? C4 C9 C10 C11 -0.1(5) . . . . ? C8 C9 C10 C11 178.5(3) . . . . ? C9 C10 C11 C1 -176.8(3) . . . 2_666 ? C9 C10 C11 C2 1.5(5) . . . . ? C3 C2 C11 C10 -1.0(4) . . . . ? C1 C2 C11 C10 179.2(3) . . . . ? C3 C2 C11 C1 177.4(3) . . . 2_666 ? C1 C2 C11 C1 -2.4(5) . . . 2_666 ? C2 C1 C12 C13 17(8) . . . . ? C11 C1 C12 C13 -163(8) 2_666 . . . ? C1 C12 C13 Si1 8(10) . . . . ? C17 Si1 C13 C12 90(3) . . . . ? C14 Si1 C13 C12 -152(3) . . . . ? C20 Si1 C13 C12 -29(3) . . . . ? C13 Si1 C14 C16 -63.9(3) . . . . ? C17 Si1 C14 C16 51.7(3) . . . . ? C20 Si1 C14 C16 177.5(3) . . . . ? C13 Si1 C14 C15 60.7(3) . . . . ? C17 Si1 C14 C15 176.2(3) . . . . ? C20 Si1 C14 C15 -57.9(3) . . . . ? C13 Si1 C17 C19 -60.4(3) . . . . ? C14 Si1 C17 C19 -176.5(3) . . . . ? C20 Si1 C17 C19 56.2(3) . . . . ? C13 Si1 C17 C18 170.8(3) . . . . ? C14 Si1 C17 C18 54.7(3) . . . . ? C20 Si1 C17 C18 -72.6(3) . . . . ? C13 Si1 C20 C21 -168.3(3) . . . . ? C17 Si1 C20 C21 75.3(3) . . . . ? C14 Si1 C20 C21 -49.4(4) . . . . ? C13 Si1 C20 C22 -41.9(4) . . . . ? C17 Si1 C20 C22 -158.3(3) . . . . ? C14 Si1 C20 C22 77.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 68.48 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.422 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.064 # Attachment 'Offset_TIPSCF3.cif' data_x09109 _database_code_depnum_ccdc_archive 'CCDC 796839' #TrackingRef 'Offset_TIPSCF3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H53 F3 Si2' _chemical_formula_sum 'C45 H53 F3 Si2' _chemical_formula_weight 707.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7521(2) _cell_length_b 15.8341(4) _cell_length_c 17.6273(5) _cell_angle_alpha 70.9410(10) _cell_angle_beta 80.2570(10) _cell_angle_gamma 81.9880(10) _cell_volume 2007.37(9) _cell_formula_units_Z 2 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 9880 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 68.50 _exptl_crystal_description lath _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.637 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details 'Sadabs in APEX2 (BrukerAXS, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator 'graded multilayer optics' _diffrn_measurement_device_type 'Bruker X8 Proteum diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 28041 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 68.50 _reflns_number_total 7275 _reflns_number_gt 6200 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 2008)' _computing_publication_material ; SHELX-97 (Sheldrick, 2008) and local procedures ; _publ_section_exptl_refinement ; H atoms were found in difference Fourier maps and subsequently placed in idealized positions with constrained distances of 0.98 \%A (RCH~3~), 1.00 \%A (R~3~CH), 0.95 \%A (C~Ar~H), and with U~iso~(H) values set to either 1.2U~eq~ or 1.5U~eq~ (RCH~3~) of the attached atom. ; _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^ > 2\s(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. In order to maintain a chemically sensible geometry and similarity between the disordered groups, a number of constraints (EXYZ, EADP) and restraints (SAME, SIMU) were applied. ; _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^)+(0.0400P)^2^+2.9034P] 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 7275 _refine_ls_number_parameters 525 _refine_ls_number_restraints 160 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1606 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.003 _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 0.01807(10) 0.30308(5) 0.92360(5) 0.0360(2) Uani 1 1 d . . . C1 C 0.3444(3) 0.30842(18) 0.68904(16) 0.0328(6) Uani 1 1 d . . . C2 C 0.3191(3) 0.37640(18) 0.61423(16) 0.0309(6) Uani 1 1 d . . . C3 C 0.2096(3) 0.45487(18) 0.61187(16) 0.0326(6) Uani 1 1 d . . . H3 H 0.1512 0.4629 0.6613 0.039 Uiso 1 1 calc R . . C4 C 0.1834(3) 0.52184(18) 0.53919(17) 0.0330(6) Uani 1 1 d . . . C5 C 0.0725(3) 0.60072(18) 0.53669(17) 0.0341(6) Uani 1 1 d . . . H5 H 0.0127 0.6084 0.5860 0.041 Uiso 1 1 calc R . . C6 C 0.0478(4) 0.66719(18) 0.46507(17) 0.0345(6) Uani 1 1 d . . . C7 C -0.0653(4) 0.74770(19) 0.46246(19) 0.0380(6) Uani 1 1 d . . . H7 H -0.1273 0.7555 0.5114 0.046 Uiso 1 1 calc R . . C8 C -0.0850(4) 0.8125(2) 0.3915(2) 0.0436(7) Uani 1 1 d . . . H8 H -0.1605 0.8653 0.3911 0.052 Uiso 1 1 calc R . . C9 C 0.0063(4) 0.8026(2) 0.31710(19) 0.0431(7) Uani 1 1 d . . . H9 H -0.0078 0.8492 0.2678 0.052 Uiso 1 1 calc R . . C10 C 0.1133(4) 0.7273(2) 0.31622(18) 0.0398(7) Uani 1 1 d . . . H10 H 0.1722 0.7215 0.2661 0.048 Uiso 1 1 calc R . . C11 C 0.1389(4) 0.65648(19) 0.38958(17) 0.0354(6) Uani 1 1 d . . . C12 C 0.2475(4) 0.57824(19) 0.39084(17) 0.0351(6) Uani 1 1 d . . . H12 H 0.3065 0.5710 0.3412 0.042 Uiso 1 1 calc R . . C13 C 0.2721(3) 0.50961(18) 0.46392(16) 0.0322(6) Uani 1 1 d . . . C14 C 0.3811(3) 0.43041(19) 0.46638(16) 0.0331(6) Uani 1 1 d . . . H14 H 0.4402 0.4224 0.4171 0.040 Uiso 1 1 calc R . . C15 C 0.4052(3) 0.36315(18) 0.53912(16) 0.0324(6) Uani 1 1 d . . . C16 C 0.5117(3) 0.28142(19) 0.54128(17) 0.0325(6) Uani 1 1 d . . . C17 C 0.5354(3) 0.21463(19) 0.61537(17) 0.0334(6) Uani 1 1 d . B . C18 C 0.6399(4) 0.13219(19) 0.61872(18) 0.0364(6) Uani 1 1 d . . . H18 H 0.6954 0.1218 0.5698 0.044 Uiso 1 1 calc R A 1 C19 C 0.6615(4) 0.0685(2) 0.69027(19) 0.0399(7) Uani 0.858(2) 1 d PD B 1 C45 C 0.6108(5) 0.0108(3) 0.8406(2) 0.0491(9) Uani 0.858(2) 1 d PD B 1 F1 F 0.5383(4) 0.03227(18) 0.90646(14) 0.0800(9) Uani 0.858(2) 1 d PD B 1 F2 F 0.7818(3) -0.01250(15) 0.84719(13) 0.0544(6) Uani 0.858(2) 1 d PD B 1 F3 F 0.5434(3) -0.06538(16) 0.84487(15) 0.0642(7) Uani 0.858(2) 1 d PD B 1 C20 C 0.5819(4) 0.0836(2) 0.76474(19) 0.0422(7) Uani 0.858(2) 1 d PD B 1 H20A H 0.5999 0.0391 0.8148 0.051 Uiso 0.142(2) 1 calc PR B 2 C19' C 0.6615(4) 0.0685(2) 0.69027(19) 0.0399(7) Uani 0.142(2) 1 d PD B 2 H19A H 0.7297 0.0135 0.6911 0.048 Uiso 0.858(2) 1 calc PR B 1 F3' F 0.840(2) -0.0283(11) 0.6342(9) 0.083(5) Uiso 0.142(2) 1 d PD B 2 F2' F 0.6865(19) -0.0879(10) 0.7483(9) 0.066(4) Uiso 0.142(2) 1 d PD B 2 F1' F 0.908(2) -0.0203(12) 0.7440(10) 0.077(5) Uiso 0.142(2) 1 d PD B 2 C45' C 0.771(3) -0.0154(14) 0.7062(11) 0.058(6) Uiso 0.142(2) 1 d PD B 2 C20' C 0.5819(4) 0.0836(2) 0.76474(19) 0.0422(7) Uani 0.142(2) 1 d PD B 2 C21 C 0.4808(4) 0.1609(2) 0.76427(18) 0.0383(6) Uani 1 1 d . . . H21 H 0.4276 0.1697 0.8141 0.046 Uiso 1 1 calc R B 1 C22 C 0.4535(3) 0.22920(19) 0.69018(17) 0.0340(6) Uani 1 1 d . B . C23 C 0.2506(4) 0.31781(18) 0.76356(17) 0.0345(6) Uani 1 1 d . . . C24 C 0.1662(4) 0.31907(19) 0.82717(17) 0.0362(6) Uani 1 1 d . . . C25 C -0.0871(4) 0.1957(2) 0.94354(19) 0.0451(7) Uani 1 1 d . . . H25 H -0.1888 0.2116 0.9118 0.054 Uiso 1 1 calc R . . C26 C -0.1621(5) 0.1559(3) 1.0330(2) 0.0612(10) Uani 1 1 d . . . H26A H -0.2301 0.1058 1.0389 0.092 Uiso 1 1 calc R . . H26B H -0.2386 0.2022 1.0511 0.092 Uiso 1 1 calc R . . H26C H -0.0653 0.1343 1.0658 0.092 Uiso 1 1 calc R . . C27 C 0.0334(5) 0.1227(2) 0.9155(2) 0.0526(8) Uani 1 1 d . . . H27A H 0.1299 0.1014 0.9485 0.079 Uiso 1 1 calc R . . H27B H 0.0813 0.1478 0.8585 0.079 Uiso 1 1 calc R . . H27C H -0.0344 0.0725 0.9218 0.079 Uiso 1 1 calc R . . C28 C 0.1520(4) 0.2961(2) 1.00545(19) 0.0469(8) Uani 1 1 d . . . H28 H 0.0765 0.2735 1.0585 0.056 Uiso 1 1 calc R . . C29 C 0.3147(5) 0.2296(3) 1.0061(2) 0.0604(9) Uani 1 1 d . . . H29A H 0.3926 0.2501 0.9551 0.091 Uiso 1 1 calc R . . H29B H 0.2792 0.1704 1.0124 0.091 Uiso 1 1 calc R . . H29C H 0.3768 0.2256 1.0514 0.091 Uiso 1 1 calc R . . C30 C 0.2058(5) 0.3868(3) 1.0007(3) 0.0601(9) Uani 1 1 d . . . H30A H 0.2733 0.3793 1.0451 0.090 Uiso 1 1 calc R . . H30B H 0.1004 0.4279 1.0052 0.090 Uiso 1 1 calc R . . H30C H 0.2784 0.4116 0.9488 0.090 Uiso 1 1 calc R . . C31 C -0.1493(4) 0.4037(2) 0.90832(18) 0.0409(7) Uani 1 1 d . . . H31 H -0.0839 0.4575 0.8974 0.049 Uiso 1 1 calc R . . C32 C -0.2844(4) 0.3993(2) 0.9841(2) 0.0498(8) Uani 1 1 d . . . H32A H -0.3645 0.4543 0.9738 0.075 Uiso 1 1 calc R . . H32B H -0.2229 0.3936 1.0300 0.075 Uiso 1 1 calc R . . H32C H -0.3516 0.3473 0.9967 0.075 Uiso 1 1 calc R . . C33 C -0.2441(5) 0.4190(3) 0.8346(2) 0.0592(9) Uani 1 1 d . . . H33A H -0.1574 0.4253 0.7861 0.089 Uiso 0.858(2) 1 calc PR . . H33B H -0.3246 0.4737 0.8273 0.089 Uiso 0.858(2) 1 calc PR . . H33C H -0.3109 0.3677 0.8433 0.089 Uiso 0.858(2) 1 calc PR . . H33D H -0.3712 0.4191 0.8517 0.089 Uiso 0.142(2) 1 calc PR . . H33E H -0.2040 0.3708 0.8105 0.089 Uiso 0.142(2) 1 calc PR . . H33F H -0.2177 0.4768 0.7945 0.089 Uiso 0.142(2) 1 calc PR . . C34 C 0.5914(3) 0.26556(19) 0.46733(17) 0.0341(6) Uani 1 1 d . B . C35 C 0.6594(4) 0.2496(2) 0.40562(18) 0.0386(6) Uani 1 1 d . . . Si2 Si 0.77825(12) 0.21319(6) 0.31881(5) 0.0329(2) Uani 0.858(2) 1 d PDU B 1 C36 C 0.6761(5) 0.1093(3) 0.3218(2) 0.0395(9) Uani 0.858(2) 1 d PDU B 1 H36 H 0.5613 0.1308 0.3000 0.047 Uiso 0.858(2) 1 calc PR B 1 C37 C 0.6341(7) 0.0459(3) 0.4077(3) 0.0478(11) Uani 0.858(2) 1 d PDU B 1 H37A H 0.5737 -0.0037 0.4060 0.072 Uiso 0.858(2) 1 calc PR B 1 H37B H 0.5583 0.0788 0.4410 0.072 Uiso 0.858(2) 1 calc PR B 1 H37C H 0.7436 0.0220 0.4311 0.072 Uiso 0.858(2) 1 calc PR B 1 C38 C 0.7873(6) 0.0584(3) 0.2662(2) 0.0468(9) Uani 0.858(2) 1 d PDU B 1 H38A H 0.8976 0.0317 0.2879 0.070 Uiso 0.858(2) 1 calc PR B 1 H38B H 0.8132 0.1003 0.2116 0.070 Uiso 0.858(2) 1 calc PR B 1 H38C H 0.7216 0.0110 0.2638 0.070 Uiso 0.858(2) 1 calc PR B 1 C39 C 1.0195(4) 0.1935(2) 0.3322(2) 0.0403(8) Uani 0.858(2) 1 d PDU B 1 H39 H 1.0480 0.2469 0.3446 0.048 Uiso 0.858(2) 1 calc PR B 1 C40 C 1.0619(5) 0.1115(3) 0.4042(2) 0.0466(9) Uani 0.858(2) 1 d PDU B 1 H40A H 1.0360 0.0571 0.3949 0.070 Uiso 0.858(2) 1 calc PR B 1 H40B H 0.9901 0.1179 0.4537 0.070 Uiso 0.858(2) 1 calc PR B 1 H40C H 1.1866 0.1071 0.4100 0.070 Uiso 0.858(2) 1 calc PR B 1 C41 C 1.1398(5) 0.1901(3) 0.2541(2) 0.0530(10) Uani 0.858(2) 1 d PDU B 1 H41A H 1.2624 0.1776 0.2646 0.079 Uiso 0.858(2) 1 calc PR B 1 H41B H 1.1256 0.2480 0.2119 0.079 Uiso 0.858(2) 1 calc PR B 1 H41C H 1.1080 0.1427 0.2360 0.079 Uiso 0.858(2) 1 calc PR B 1 C42 C 0.7443(5) 0.3091(2) 0.2236(2) 0.0391(8) Uani 0.858(2) 1 d PDU B 1 H42 H 0.8127 0.2913 0.1770 0.047 Uiso 0.858(2) 1 calc PR B 1 C43 C 0.5530(5) 0.3291(3) 0.2089(2) 0.0538(10) Uani 0.858(2) 1 d PDU B 1 H43A H 0.4812 0.3433 0.2552 0.081 Uiso 0.858(2) 1 calc PR B 1 H43B H 0.5123 0.2764 0.2020 0.081 Uiso 0.858(2) 1 calc PR B 1 H43C H 0.5422 0.3803 0.1598 0.081 Uiso 0.858(2) 1 calc PR B 1 C44 C 0.8170(7) 0.3934(3) 0.2252(3) 0.0553(11) Uani 0.858(2) 1 d PDU B 1 H44A H 0.7981 0.4422 0.1754 0.083 Uiso 0.858(2) 1 calc PR B 1 H44B H 0.9431 0.3810 0.2292 0.083 Uiso 0.858(2) 1 calc PR B 1 H44C H 0.7563 0.4108 0.2720 0.083 Uiso 0.858(2) 1 calc PR B 1 Si2' Si 0.6629(9) 0.2492(5) 0.3070(4) 0.0521(17) Uani 0.142(2) 1 d PDU B 2 C36' C 0.721(3) 0.1265(11) 0.3211(14) 0.039(3) Uiso 0.142(2) 1 d PDU B 2 H36' H 0.8444 0.1116 0.3339 0.046 Uiso 0.142(2) 1 calc PR B 2 C37' C 0.606(5) 0.065(2) 0.3892(18) 0.055(7) Uiso 0.142(2) 1 d PDU B 2 H37D H 0.5328 0.1000 0.4216 0.083 Uiso 0.142(2) 1 calc PR B 2 H37E H 0.6799 0.0179 0.4236 0.083 Uiso 0.142(2) 1 calc PR B 2 H37F H 0.5297 0.0378 0.3664 0.083 Uiso 0.142(2) 1 calc PR B 2 C38' C 0.714(4) 0.1035(19) 0.2425(15) 0.062(5) Uiso 0.142(2) 1 d PDU B 2 H38D H 0.6946 0.1591 0.1982 0.093 Uiso 0.142(2) 1 calc PR B 2 H38E H 0.6185 0.0657 0.2512 0.093 Uiso 0.142(2) 1 calc PR B 2 H38F H 0.8263 0.0713 0.2283 0.093 Uiso 0.142(2) 1 calc PR B 2 C39' C 0.836(2) 0.3217(13) 0.2368(14) 0.054(4) Uiso 0.142(2) 1 d PDU B 2 H39' H 0.8381 0.3192 0.1807 0.065 Uiso 0.142(2) 1 calc PR B 2 C40' C 0.786(5) 0.4191(15) 0.237(2) 0.060(7) Uiso 0.142(2) 1 d PDU B 2 H40D H 0.6860 0.4208 0.2789 0.089 Uiso 0.142(2) 1 calc PR B 2 H40E H 0.7527 0.4558 0.1839 0.089 Uiso 0.142(2) 1 calc PR B 2 H40F H 0.8860 0.4427 0.2478 0.089 Uiso 0.142(2) 1 calc PR B 2 C41' C 1.020(3) 0.286(2) 0.2636(19) 0.077(6) Uiso 0.142(2) 1 d PDU B 2 H41D H 1.1072 0.2891 0.2157 0.115 Uiso 0.142(2) 1 calc PR B 2 H41E H 1.0175 0.2238 0.2987 0.115 Uiso 0.142(2) 1 calc PR B 2 H41F H 1.0519 0.3230 0.2934 0.115 Uiso 0.142(2) 1 calc PR B 2 C42' C 0.442(2) 0.2902(15) 0.2699(12) 0.060(5) Uiso 0.142(2) 1 d PDU B 2 H42' H 0.3718 0.2372 0.2923 0.072 Uiso 0.142(2) 1 calc PR B 2 C43' C 0.340(3) 0.3613(16) 0.3035(15) 0.061(6) Uiso 0.142(2) 1 d PDU B 2 H43D H 0.4048 0.3720 0.3420 0.092 Uiso 0.142(2) 1 calc PR B 2 H43E H 0.2251 0.3411 0.3311 0.092 Uiso 0.142(2) 1 calc PR B 2 H43F H 0.3225 0.4171 0.2591 0.092 Uiso 0.142(2) 1 calc PR B 2 C44' C 0.449(4) 0.316(2) 0.1796(13) 0.074(6) Uiso 0.142(2) 1 d PDU B 2 H44D H 0.5660 0.2977 0.1558 0.111 Uiso 0.142(2) 1 calc PR B 2 H44E H 0.4232 0.3807 0.1573 0.111 Uiso 0.142(2) 1 calc PR B 2 H44F H 0.3611 0.2851 0.1669 0.111 Uiso 0.142(2) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0308(4) 0.0454(4) 0.0292(4) -0.0110(3) 0.0049(3) -0.0073(3) C1 0.0231(13) 0.0392(15) 0.0335(14) -0.0106(12) 0.0051(11) -0.0072(11) C2 0.0217(12) 0.0362(14) 0.0330(14) -0.0101(11) 0.0045(10) -0.0082(10) C3 0.0259(13) 0.0381(14) 0.0320(14) -0.0121(11) 0.0071(11) -0.0075(11) C4 0.0238(13) 0.0371(14) 0.0372(15) -0.0109(12) 0.0024(11) -0.0095(11) C5 0.0266(13) 0.0385(15) 0.0374(15) -0.0130(12) 0.0030(11) -0.0093(11) C6 0.0296(14) 0.0353(14) 0.0405(15) -0.0126(12) -0.0015(12) -0.0111(11) C7 0.0341(15) 0.0373(15) 0.0450(17) -0.0148(13) -0.0045(13) -0.0068(12) C8 0.0411(17) 0.0354(15) 0.0542(19) -0.0124(14) -0.0069(14) -0.0064(13) C9 0.0470(18) 0.0376(15) 0.0433(17) -0.0064(13) -0.0103(14) -0.0095(13) C10 0.0404(16) 0.0427(16) 0.0376(16) -0.0115(13) -0.0033(13) -0.0123(13) C11 0.0310(14) 0.0361(14) 0.0394(15) -0.0096(12) -0.0029(12) -0.0109(11) C12 0.0308(14) 0.0407(15) 0.0327(14) -0.0102(12) 0.0030(11) -0.0114(12) C13 0.0251(13) 0.0365(14) 0.0341(14) -0.0100(11) 0.0026(11) -0.0104(11) C14 0.0258(13) 0.0419(15) 0.0313(14) -0.0128(12) 0.0042(11) -0.0082(11) C15 0.0220(12) 0.0385(14) 0.0350(14) -0.0104(11) 0.0037(11) -0.0090(11) C16 0.0202(12) 0.0409(15) 0.0347(14) -0.0122(12) 0.0048(10) -0.0065(11) C17 0.0215(13) 0.0419(15) 0.0359(15) -0.0132(12) 0.0045(11) -0.0073(11) C18 0.0275(14) 0.0415(15) 0.0388(15) -0.0141(12) 0.0041(12) -0.0047(11) C19 0.0307(15) 0.0414(16) 0.0440(17) -0.0134(13) 0.0029(12) -0.0010(12) C45 0.040(2) 0.057(2) 0.039(2) -0.0101(17) 0.0060(16) 0.0070(17) F1 0.098(2) 0.0794(18) 0.0330(12) -0.0050(11) 0.0077(12) 0.0389(15) F2 0.0470(13) 0.0605(14) 0.0473(12) -0.0091(10) -0.0092(10) 0.0074(10) F3 0.0545(14) 0.0528(14) 0.0652(15) 0.0090(11) -0.0039(12) -0.0097(11) C20 0.0341(15) 0.0430(16) 0.0409(16) -0.0060(13) 0.0012(13) 0.0001(12) C19' 0.0307(15) 0.0414(16) 0.0440(17) -0.0134(13) 0.0029(12) -0.0010(12) C20' 0.0341(15) 0.0430(16) 0.0409(16) -0.0060(13) 0.0012(13) 0.0001(12) C21 0.0307(14) 0.0461(16) 0.0339(15) -0.0109(12) 0.0038(12) -0.0033(12) C22 0.0254(13) 0.0404(15) 0.0338(14) -0.0102(12) 0.0026(11) -0.0062(11) C23 0.0300(14) 0.0346(14) 0.0335(15) -0.0064(11) 0.0026(12) -0.0036(11) C24 0.0339(15) 0.0366(15) 0.0355(15) -0.0098(12) 0.0020(12) -0.0056(11) C25 0.0406(17) 0.0521(18) 0.0388(16) -0.0066(14) -0.0019(13) -0.0139(14) C26 0.053(2) 0.061(2) 0.053(2) -0.0028(17) 0.0136(17) -0.0132(17) C27 0.066(2) 0.0471(18) 0.0430(18) -0.0114(15) 0.0052(16) -0.0209(16) C28 0.0415(17) 0.062(2) 0.0361(16) -0.0139(14) 0.0028(13) -0.0127(15) C29 0.057(2) 0.059(2) 0.067(2) -0.0161(18) -0.0242(19) 0.0006(17) C30 0.047(2) 0.068(2) 0.077(3) -0.036(2) -0.0154(18) -0.0023(17) C31 0.0337(15) 0.0507(17) 0.0395(16) -0.0185(14) 0.0032(12) -0.0062(13) C32 0.0358(16) 0.063(2) 0.055(2) -0.0293(17) 0.0069(14) -0.0060(14) C33 0.058(2) 0.068(2) 0.054(2) -0.0276(18) -0.0160(17) 0.0182(18) C34 0.0265(13) 0.0380(15) 0.0357(15) -0.0101(12) 0.0008(11) -0.0054(11) C35 0.0320(15) 0.0449(16) 0.0375(16) -0.0114(13) -0.0005(12) -0.0081(12) Si2 0.0292(5) 0.0377(5) 0.0291(4) -0.0114(4) 0.0056(4) -0.0032(4) C36 0.039(2) 0.0422(19) 0.0415(19) -0.0174(16) -0.0007(16) -0.0112(15) C37 0.057(3) 0.047(2) 0.040(2) -0.0116(18) 0.001(2) -0.017(2) C38 0.060(2) 0.045(2) 0.0380(19) -0.0159(16) -0.0028(17) -0.0106(18) C39 0.0304(17) 0.0456(19) 0.0429(19) -0.0147(15) 0.0030(14) -0.0033(14) C40 0.0388(19) 0.055(2) 0.041(2) -0.0135(17) -0.0010(15) 0.0051(16) C41 0.0342(19) 0.063(2) 0.049(2) -0.0102(18) 0.0122(16) 0.0005(17) C42 0.0382(18) 0.0424(18) 0.0336(17) -0.0116(14) 0.0032(14) -0.0031(14) C43 0.042(2) 0.060(2) 0.046(2) -0.0035(18) 0.0004(17) 0.0018(18) C44 0.061(3) 0.040(2) 0.055(3) -0.005(2) 0.000(2) -0.006(2) Si2' 0.049(4) 0.057(3) 0.049(3) -0.022(3) 0.000(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C24 1.847(3) . ? Si1 C28 1.882(3) . ? Si1 C31 1.886(3) . ? Si1 C25 1.892(3) . ? C1 C22 1.408(4) . ? C1 C2 1.427(4) . ? C1 C23 1.432(4) . ? C2 C3 1.397(4) . ? C2 C15 1.444(4) . ? C3 C4 1.396(4) . ? C3 H3 0.9500 . ? C4 C5 1.406(4) . ? C4 C13 1.447(4) . ? C5 C6 1.377(4) . ? C5 H5 0.9500 . ? C6 C7 1.435(4) . ? C6 C11 1.447(4) . ? C7 C8 1.351(4) . ? C7 H7 0.9500 . ? C8 C9 1.426(5) . ? C8 H8 0.9500 . ? C9 C10 1.358(4) . ? C9 H9 0.9500 . ? C10 C11 1.431(4) . ? C10 H10 0.9500 . ? C11 C12 1.394(4) . ? C12 C13 1.410(4) . ? C12 H12 0.9500 . ? C13 C14 1.404(4) . ? C14 C15 1.395(4) . ? C14 H14 0.9500 . ? C15 C16 1.428(4) . ? C16 C17 1.408(4) . ? C16 C34 1.429(4) . ? C17 C18 1.426(4) . ? C17 C22 1.439(4) . ? C18 C19 1.353(4) . ? C18 H18 0.9500 . ? C19 C20 1.432(4) . ? C45 F1 1.328(4) . ? C45 F2 1.340(4) . ? C45 F3 1.355(5) . ? C20 C21 1.357(4) . ? C20 H20A 0.9500 . ? F3' C45' 1.359(18) . ? F2' C45' 1.338(17) . ? F1' C45' 1.324(17) . ? C21 C22 1.424(4) . ? C21 H21 0.9500 . ? C23 C24 1.203(4) . ? C25 C26 1.537(4) . ? C25 C27 1.538(5) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.524(5) . ? C28 C29 1.525(5) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.535(5) . ? C31 C32 1.540(4) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C33 H33D 0.9800 . ? C33 H33E 0.9800 . ? C33 H33F 0.9800 . ? C34 C35 1.214(4) . ? C35 Si2' 1.737(7) . ? C35 Si2 1.864(3) . ? Si2 C42 1.888(3) . ? Si2 C39 1.894(4) . ? Si2 C36 1.905(4) . ? C36 C37 1.529(5) . ? C36 C38 1.545(5) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.533(5) . ? C39 C41 1.538(5) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.521(5) . ? C42 C44 1.529(6) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? Si2' C36' 1.876(15) . ? Si2' C42' 1.887(15) . ? Si2' C39' 1.896(16) . ? C36' C37' 1.517(18) . ? C36' C38' 1.553(18) . ? C36' H36' 1.0000 . ? C37' H37D 0.9800 . ? C37' H37E 0.9800 . ? C37' H37F 0.9800 . ? C38' H38D 0.9800 . ? C38' H38E 0.9800 . ? C38' H38F 0.9800 . ? C39' C40' 1.538(18) . ? C39' C41' 1.549(18) . ? C39' H39' 1.0000 . ? C40' H40D 0.9800 . ? C40' H40E 0.9800 . ? C40' H40F 0.9800 . ? C41' H41D 0.9800 . ? C41' H41E 0.9800 . ? C41' H41F 0.9800 . ? C42' C44' 1.503(18) . ? C42' C43' 1.509(18) . ? C42' H42' 1.0000 . ? C43' H43D 0.9800 . ? C43' H43E 0.9800 . ? C43' H43F 0.9800 . ? C44' H44D 0.9800 . ? C44' H44E 0.9800 . ? C44' H44F 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 C24 Si1 C28 108.55(14) . . ? C24 Si1 C31 106.79(13) . . ? C28 Si1 C31 110.90(15) . . ? C24 Si1 C25 106.45(14) . . ? C28 Si1 C25 112.03(15) . . ? C31 Si1 C25 111.83(14) . . ? C22 C1 C2 120.6(2) . . ? C22 C1 C23 119.1(2) . . ? C2 C1 C23 120.2(2) . . ? C3 C2 C1 121.4(2) . . ? C3 C2 C15 119.1(2) . . ? C1 C2 C15 119.5(2) . . ? C4 C3 C2 122.0(2) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 122.1(3) . . ? C3 C4 C13 119.0(2) . . ? C5 C4 C13 118.9(3) . . ? C6 C5 C4 122.1(3) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 122.2(3) . . ? C5 C6 C11 119.4(3) . . ? C7 C6 C11 118.4(3) . . ? C8 C7 C6 121.0(3) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.8(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 120.5(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 121.1(3) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 122.5(3) . . ? C12 C11 C6 119.2(3) . . ? C10 C11 C6 118.3(3) . . ? C11 C12 C13 121.6(3) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C14 C13 C12 122.4(3) . . ? C14 C13 C4 118.8(2) . . ? C12 C13 C4 118.7(2) . . ? C15 C14 C13 121.9(3) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 C16 121.8(2) . . ? C14 C15 C2 119.1(2) . . ? C16 C15 C2 119.1(2) . . ? C17 C16 C15 121.0(2) . . ? C17 C16 C34 119.2(2) . . ? C15 C16 C34 119.8(2) . . ? C16 C17 C18 121.8(3) . . ? C16 C17 C22 119.7(2) . . ? C18 C17 C22 118.5(3) . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 120.2(3) . . ? F1 C45 F2 107.0(3) . . ? F1 C45 F3 106.7(3) . . ? F2 C45 F3 105.4(3) . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? F1' C45' F2' 105.9(17) . . ? F1' C45' F3' 105.6(17) . . ? F2' C45' F3' 105.5(16) . . ? C20 C21 C22 121.0(3) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C1 C22 C21 121.3(3) . . ? C1 C22 C17 120.0(2) . . ? C21 C22 C17 118.6(3) . . ? C24 C23 C1 174.5(3) . . ? C23 C24 Si1 169.3(3) . . ? C26 C25 C27 109.2(3) . . ? C26 C25 Si1 112.4(2) . . ? C27 C25 Si1 114.5(2) . . ? C26 C25 H25 106.8 . . ? C27 C25 H25 106.8 . . ? Si1 C25 H25 106.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 109.6(3) . . ? C30 C28 Si1 113.0(2) . . ? C29 C28 Si1 112.2(2) . . ? C30 C28 H28 107.2 . . ? C29 C28 H28 107.2 . . ? Si1 C28 H28 107.2 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C32 110.1(3) . . ? C33 C31 Si1 112.4(2) . . ? C32 C31 Si1 112.8(2) . . ? C33 C31 H31 107.1 . . ? C32 C31 H31 107.1 . . ? Si1 C31 H31 107.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C33 H33D 109.5 . . ? H33A C33 H33D 141.1 . . ? H33B C33 H33D 56.3 . . ? H33C C33 H33D 56.3 . . ? C31 C33 H33E 109.5 . . ? H33A C33 H33E 56.3 . . ? H33B C33 H33E 141.1 . . ? H33C C33 H33E 56.3 . . ? H33D C33 H33E 109.5 . . ? C31 C33 H33F 109.5 . . ? H33A C33 H33F 56.3 . . ? H33B C33 H33F 56.3 . . ? H33C C33 H33F 141.1 . . ? H33D C33 H33F 109.5 . . ? H33E C33 H33F 109.5 . . ? C35 C34 C16 178.2(3) . . ? C34 C35 Si2' 153.8(4) . . ? C34 C35 Si2 173.1(3) . . ? C35 Si2 C42 106.99(15) . . ? C35 Si2 C39 106.71(15) . . ? C42 Si2 C39 109.74(16) . . ? C35 Si2 C36 106.66(15) . . ? C42 Si2 C36 111.77(17) . . ? C39 Si2 C36 114.52(17) . . ? C37 C36 C38 110.9(3) . . ? C37 C36 Si2 112.9(3) . . ? C38 C36 Si2 112.7(3) . . ? C37 C36 H36 106.6 . . ? C38 C36 H36 106.6 . . ? Si2 C36 H36 106.6 . . ? C40 C39 C41 111.3(3) . . ? C40 C39 Si2 113.4(2) . . ? C41 C39 Si2 112.6(3) . . ? C40 C39 H39 106.3 . . ? C41 C39 H39 106.3 . . ? Si2 C39 H39 106.3 . . ? C43 C42 C44 110.5(3) . . ? C43 C42 Si2 112.8(2) . . ? C44 C42 Si2 110.8(3) . . ? C43 C42 H42 107.5 . . ? C44 C42 H42 107.5 . . ? Si2 C42 H42 107.5 . . ? C35 Si2' C36' 99.8(8) . . ? C35 Si2' C42' 111.9(7) . . ? C36' Si2' C42' 112.3(10) . . ? C35 Si2' C39' 110.1(8) . . ? C36' Si2' C39' 112.9(10) . . ? C42' Si2' C39' 109.5(10) . . ? C37' C36' C38' 107.8(19) . . ? C37' C36' Si2' 114.5(17) . . ? C38' C36' Si2' 111.6(15) . . ? C37' C36' H36' 107.6 . . ? C38' C36' H36' 107.6 . . ? Si2' C36' H36' 107.6 . . ? C36' C37' H37D 109.5 . . ? C36' C37' H37E 109.5 . . ? H37D C37' H37E 109.5 . . ? C36' C37' H37F 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? C36' C38' H38D 109.5 . . ? C36' C38' H38E 109.5 . . ? H38D C38' H38E 109.5 . . ? C36' C38' H38F 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? C40' C39' C41' 112(2) . . ? C40' C39' Si2' 108.5(17) . . ? C41' C39' Si2' 110.4(15) . . ? C40' C39' H39' 108.7 . . ? C41' C39' H39' 108.7 . . ? Si2' C39' H39' 108.7 . . ? C39' C40' H40D 109.5 . . ? C39' C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C39' C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? C39' C41' H41D 109.5 . . ? C39' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? C39' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? C44' C42' C43' 112.1(18) . . ? C44' C42' Si2' 114.1(16) . . ? C43' C42' Si2' 114.2(15) . . ? C44' C42' H42' 105.1 . . ? C43' C42' H42' 105.1 . . ? Si2' C42' H42' 105.1 . . ? C42' C43' H43D 109.5 . . ? C42' C43' H43E 109.5 . . ? H43D C43' H43E 109.5 . . ? C42' C43' H43F 109.5 . . ? H43D C43' H43F 109.5 . . ? H43E C43' H43F 109.5 . . ? C42' C44' H44D 109.5 . . ? C42' C44' H44E 109.5 . . ? H44D C44' H44E 109.5 . . ? C42' C44' H44F 109.5 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 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 C22 C1 C2 C3 179.2(2) . . . . ? C23 C1 C2 C3 2.8(4) . . . . ? C22 C1 C2 C15 0.6(4) . . . . ? C23 C1 C2 C15 -175.7(2) . . . . ? C1 C2 C3 C4 -179.8(2) . . . . ? C15 C2 C3 C4 -1.3(4) . . . . ? C2 C3 C4 C5 179.7(3) . . . . ? C2 C3 C4 C13 0.1(4) . . . . ? C3 C4 C5 C6 179.4(3) . . . . ? C13 C4 C5 C6 -1.0(4) . . . . ? C4 C5 C6 C7 -180.0(3) . . . . ? C4 C5 C6 C11 -0.4(4) . . . . ? C5 C6 C7 C8 178.9(3) . . . . ? C11 C6 C7 C8 -0.7(4) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C7 C8 C9 C10 0.8(5) . . . . ? C8 C9 C10 C11 -0.7(4) . . . . ? C9 C10 C11 C12 179.9(3) . . . . ? C9 C10 C11 C6 -0.1(4) . . . . ? C5 C6 C11 C12 1.2(4) . . . . ? C7 C6 C11 C12 -179.2(2) . . . . ? C5 C6 C11 C10 -178.9(2) . . . . ? C7 C6 C11 C10 0.8(4) . . . . ? C10 C11 C12 C13 179.4(3) . . . . ? C6 C11 C12 C13 -0.6(4) . . . . ? C11 C12 C13 C14 -179.9(3) . . . . ? C11 C12 C13 C4 -0.7(4) . . . . ? C3 C4 C13 C14 0.4(4) . . . . ? C5 C4 C13 C14 -179.3(2) . . . . ? C3 C4 C13 C12 -178.8(2) . . . . ? C5 C4 C13 C12 1.5(4) . . . . ? C12 C13 C14 C15 179.6(3) . . . . ? C4 C13 C14 C15 0.5(4) . . . . ? C13 C14 C15 C16 178.0(2) . . . . ? C13 C14 C15 C2 -1.7(4) . . . . ? C3 C2 C15 C14 2.1(4) . . . . ? C1 C2 C15 C14 -179.3(2) . . . . ? C3 C2 C15 C16 -177.6(2) . . . . ? C1 C2 C15 C16 1.0(4) . . . . ? C14 C15 C16 C17 179.5(2) . . . . ? C2 C15 C16 C17 -0.8(4) . . . . ? C14 C15 C16 C34 -2.4(4) . . . . ? C2 C15 C16 C34 177.3(2) . . . . ? C15 C16 C17 C18 179.4(2) . . . . ? C34 C16 C17 C18 1.3(4) . . . . ? C15 C16 C17 C22 -0.9(4) . . . . ? C34 C16 C17 C22 -179.0(2) . . . . ? C16 C17 C18 C19 -179.9(3) . . . . ? C22 C17 C18 C19 0.4(4) . . . . ? C17 C18 C19 C20 -1.3(4) . . . . ? C18 C19 C20 C21 1.5(5) . . . . ? C19 C20 C21 C22 -0.8(5) . . . . ? C2 C1 C22 C21 179.6(3) . . . . ? C23 C1 C22 C21 -4.0(4) . . . . ? C2 C1 C22 C17 -2.4(4) . . . . ? C23 C1 C22 C17 174.0(2) . . . . ? C20 C21 C22 C1 178.0(3) . . . . ? C20 C21 C22 C17 0.0(4) . . . . ? C16 C17 C22 C1 2.5(4) . . . . ? C18 C17 C22 C1 -177.7(2) . . . . ? C16 C17 C22 C21 -179.5(3) . . . . ? C18 C17 C22 C21 0.3(4) . . . . ? C28 Si1 C24 C23 128.4(14) . . . . ? C31 Si1 C24 C23 -112.0(14) . . . . ? C25 Si1 C24 C23 7.6(14) . . . . ? C24 Si1 C25 C26 160.1(2) . . . . ? C28 Si1 C25 C26 41.6(3) . . . . ? C31 Si1 C25 C26 -83.6(3) . . . . ? C24 Si1 C25 C27 34.8(3) . . . . ? C28 Si1 C25 C27 -83.7(3) . . . . ? C31 Si1 C25 C27 151.1(2) . . . . ? C24 Si1 C28 C30 74.9(3) . . . . ? C31 Si1 C28 C30 -42.1(3) . . . . ? C25 Si1 C28 C30 -167.8(2) . . . . ? C24 Si1 C28 C29 -49.6(3) . . . . ? C31 Si1 C28 C29 -166.6(2) . . . . ? C25 Si1 C28 C29 67.6(3) . . . . ? C24 Si1 C31 C33 54.2(3) . . . . ? C28 Si1 C31 C33 172.3(2) . . . . ? C25 Si1 C31 C33 -61.9(3) . . . . ? C24 Si1 C31 C32 179.4(2) . . . . ? C28 Si1 C31 C32 -62.5(3) . . . . ? C25 Si1 C31 C32 63.3(3) . . . . ? Si2' C35 Si2 C42 38.6(5) . . . . ? Si2' C35 Si2 C39 156.0(5) . . . . ? Si2' C35 Si2 C36 -81.2(5) . . . . ? C35 Si2 C36 C37 -40.1(3) . . . . ? C42 Si2 C36 C37 -156.7(3) . . . . ? C39 Si2 C36 C37 77.7(3) . . . . ? C35 Si2 C36 C38 -166.7(3) . . . . ? C42 Si2 C36 C38 76.7(3) . . . . ? C39 Si2 C36 C38 -48.9(3) . . . . ? C35 Si2 C39 C40 69.3(3) . . . . ? C42 Si2 C39 C40 -175.1(3) . . . . ? C36 Si2 C39 C40 -48.4(3) . . . . ? C35 Si2 C39 C41 -163.2(3) . . . . ? C42 Si2 C39 C41 -47.6(3) . . . . ? C36 Si2 C39 C41 79.1(3) . . . . ? C35 Si2 C42 C43 -64.5(3) . . . . ? C39 Si2 C42 C43 -179.9(3) . . . . ? C36 Si2 C42 C43 51.9(3) . . . . ? C35 Si2 C42 C44 60.0(3) . . . . ? C39 Si2 C42 C44 -55.4(3) . . . . ? C36 Si2 C42 C44 176.4(3) . . . . ? C34 C35 Si2' C36' -124.3(10) . . . . ? Si2 C35 Si2' C36' 48.8(8) . . . . ? C34 C35 Si2' C42' -5.3(13) . . . . ? Si2 C35 Si2' C42' 167.7(10) . . . . ? C34 C35 Si2' C39' 116.7(10) . . . . ? Si2 C35 Si2' C39' -70.2(8) . . . . ? C35 Si2' C36' C37' 51(2) . . . . ? C42' Si2' C36' C37' -67(2) . . . . ? C39' Si2' C36' C37' 168(2) . . . . ? C35 Si2' C36' C38' 174.0(16) . . . . ? C42' Si2' C36' C38' 55(2) . . . . ? C39' Si2' C36' C38' -69(2) . . . . ? C35 Si2' C39' C40' -63(2) . . . . ? C36' Si2' C39' C40' -174.0(19) . . . . ? C42' Si2' C39' C40' 60(2) . . . . ? C35 Si2' C39' C41' 59.5(18) . . . . ? C36' Si2' C39' C41' -51(2) . . . . ? C42' Si2' C39' C41' -177.1(17) . . . . ? C35 Si2' C42' C44' 163.9(17) . . . . ? C36' Si2' C42' C44' -85(2) . . . . ? C39' Si2' C42' C44' 41(2) . . . . ? C35 Si2' C42' C43' 33.1(19) . . . . ? C36' Si2' C42' C43' 144.5(17) . . . . ? C39' Si2' C42' C43' -89.2(19) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 68.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.530 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.055 # Attachment 'TNPS_CF3.cif' data_x09057s _database_code_depnum_ccdc_archive 'CCDC 796840' #TrackingRef 'TNPS_CF3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H53 F3 Si2' _chemical_formula_sum 'C45 H53 F3 Si2' _chemical_formula_weight 707.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6256(4) _cell_length_b 28.5329(7) _cell_length_c 10.5392(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.9740(10) _cell_angle_gamma 90.00 _cell_volume 4008.26(19) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 9996 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 68.35 _exptl_crystal_description lath _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_correction_T_max 0.994 _exptl_absorpt_process_details 'Sadabs in APEX2 (BrukerAXS, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator 'graded multilayer optics' _diffrn_measurement_device_type 'Bruker X8 Proteum diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 52027 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 68.00 _reflns_number_total 7186 _reflns_number_gt 5161 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 2008)' _computing_publication_material ; SHELX-97 (Sheldrick, 2008) and local procedures ; _publ_section_exptl_refinement ; H atoms were found in difference Fourier maps and subsequently placed in idealized positions with constrained distances of 0.98 \%A (RCH~3~), 0.99 \%A (R~2~CH~2~), 0.95 \%A (C~Ar~H), and with U~iso~(H) values set to either 1.2U~eq~ or 1.5U~eq~ (RCH~3~) of the attached atom. ; _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^ > 2\s(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 extensive disorder in this structure, a number of restraints were included in the refinement so as to ensure chemically reasonable geometry and physically sensible displacement parameters. The particular restraints used were (all are SHELXL97 commands): SAME - makes chemically identical groups of atoms have similar geometry. SADI - restrains chemically similar distances to be the same. SIMU - similar displacement parameters for a group of atoms. ; _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^)+(0.0760P)^2^+9.6991P] 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 7186 _refine_ls_number_parameters 510 _refine_ls_number_restraints 264 _refine_ls_R_factor_all 0.1192 _refine_ls_R_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.2273 _refine_ls_wR_factor_gt 0.2056 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.047 _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 0.64782(9) 0.13032(4) 0.08660(10) 0.0372(3) Uani 1 1 d . . . C1 C 0.4442(3) 0.22923(13) 0.2400(4) 0.0357(9) Uani 1 1 d . A . C2 C 0.3763(3) 0.21288(14) 0.3149(3) 0.0363(9) Uani 1 1 d . . . C3 C 0.3630(3) 0.16495(14) 0.3366(4) 0.0380(9) Uani 1 1 d . . . H3 H 0.3999 0.1426 0.2986 0.046 Uiso 1 1 calc R . . C4 C 0.2971(3) 0.14925(14) 0.4123(4) 0.0387(9) Uani 1 1 d . . . C5 C 0.2848(3) 0.10062(15) 0.4376(4) 0.0417(10) Uani 1 1 d . . . H5 H 0.3221 0.0779 0.4015 0.050 Uiso 1 1 calc R . . C6 C 0.2205(3) 0.08651(15) 0.5129(4) 0.0431(10) Uani 1 1 d . . . C7 C 0.1637(3) 0.11962(15) 0.5685(4) 0.0457(10) Uani 1 1 d . . . H7 H 0.1190 0.1092 0.6207 0.055 Uiso 1 1 calc R . . C8 C 0.1734(3) 0.16605(15) 0.5471(4) 0.0437(10) Uani 1 1 d . . . H8 H 0.1349 0.1879 0.5843 0.052 Uiso 1 1 calc R . . C9 C 0.2405(3) 0.18278(14) 0.4697(4) 0.0382(9) Uani 1 1 d . . . C10 C 0.2526(3) 0.22996(14) 0.4482(4) 0.0409(9) Uani 1 1 d . . . H10 H 0.2151 0.2520 0.4862 0.049 Uiso 1 1 calc R . . C11 C 0.3187(3) 0.24646(14) 0.3719(3) 0.0365(9) Uani 1 1 d . . . C12 C 0.3300(3) 0.29487(14) 0.3500(4) 0.0379(9) Uani 1 1 d . . . C13 C 0.3986(3) 0.31127(14) 0.2759(3) 0.0363(9) Uani 1 1 d . . . C14 C 0.4120(3) 0.35902(14) 0.2543(4) 0.0394(9) Uani 1 1 d . . . H14 H 0.3740 0.3812 0.2912 0.047 Uiso 1 1 calc R . . C15 C 0.4784(3) 0.37532(14) 0.1812(4) 0.0392(9) Uani 1 1 d . . . C16 C 0.4923(3) 0.42407(15) 0.1602(4) 0.0444(10) Uani 1 1 d . . . H16 H 0.4538 0.4464 0.1956 0.053 Uiso 1 1 calc R . . C17 C 0.5593(3) 0.43894(15) 0.0908(4) 0.0468(10) Uani 1 1 d . . . H17 H 0.5686 0.4716 0.0797 0.056 Uiso 1 1 calc R . . C18 C 0.6160(3) 0.40596(15) 0.0343(4) 0.0470(10) Uani 1 1 d . . . H18 H 0.6627 0.4169 -0.0145 0.056 Uiso 1 1 calc R . . C19 C 0.6043(3) 0.35916(15) 0.0492(4) 0.0444(10) Uani 1 1 d . . . H19 H 0.6423 0.3377 0.0100 0.053 Uiso 1 1 calc R . . C20 C 0.5352(3) 0.34184(14) 0.1234(3) 0.0372(9) Uani 1 1 d . . . C21 C 0.5222(3) 0.29450(14) 0.1430(3) 0.0371(9) Uani 1 1 d . . . H21 H 0.5594 0.2726 0.1041 0.045 Uiso 1 1 calc R . . C22 C 0.4557(3) 0.27765(13) 0.2187(3) 0.0355(9) Uani 1 1 d . . . C23 C 0.5049(3) 0.19625(14) 0.1872(4) 0.0380(9) Uani 1 1 d . . . C24 C 0.5590(3) 0.16943(14) 0.1454(4) 0.0406(9) Uani 1 1 d . A . C25 C 0.6944(4) 0.16276(15) -0.0427(4) 0.0458(10) Uani 1 1 d . A . H25A H 0.7490 0.1442 -0.0671 0.055 Uiso 1 1 calc R . . H25B H 0.6391 0.1646 -0.1201 0.055 Uiso 1 1 calc R . . C26 C 0.7327(5) 0.21145(19) -0.0096(5) 0.0673(15) Uani 1 1 d . . . H26A H 0.6790 0.2296 0.0184 0.081 Uiso 1 1 calc R A . H26B H 0.7897 0.2094 0.0658 0.081 Uiso 1 1 calc R . . C27 C 0.7667(4) 0.23854(17) -0.1142(5) 0.0565(12) Uani 1 1 d . A . H27A H 0.8212 0.2216 -0.1418 0.085 Uiso 1 1 calc R . . H27B H 0.7906 0.2695 -0.0811 0.085 Uiso 1 1 calc R . . H27C H 0.7104 0.2423 -0.1883 0.085 Uiso 1 1 calc R . . C28 C 0.7540(3) 0.11911(17) 0.2280(4) 0.0527(12) Uani 1 1 d . A . H28A H 0.7886 0.1492 0.2543 0.063 Uiso 1 1 calc R . . H28B H 0.7258 0.1078 0.3017 0.063 Uiso 1 1 calc R . . C29 C 0.8312(4) 0.0838(2) 0.2024(6) 0.0728(16) Uani 1 1 d . . . H29A H 0.8579 0.0942 0.1266 0.087 Uiso 1 1 calc R A . H29B H 0.7980 0.0531 0.1807 0.087 Uiso 1 1 calc R . . C30 C 0.9187(4) 0.0777(3) 0.3192(7) 0.103(3) Uani 1 1 d . A . H30A H 0.9534 0.1077 0.3392 0.155 Uiso 1 1 calc R . . H30B H 0.9657 0.0543 0.2985 0.155 Uiso 1 1 calc R . . H30C H 0.8928 0.0671 0.3944 0.155 Uiso 1 1 calc R . . C31 C 0.5786(8) 0.0752(5) 0.0197(11) 0.0465(17) Uani 0.836(8) 1 d PDU A 1 H31A H 0.5611 0.0779 -0.0759 0.056 Uiso 0.836(8) 1 calc PR A 1 H31B H 0.6253 0.0484 0.0408 0.056 Uiso 0.836(8) 1 calc PR A 1 C32 C 0.4826(4) 0.06336(18) 0.0672(5) 0.0501(14) Uani 0.836(8) 1 d PDU A 1 H32A H 0.4359 0.0903 0.0503 0.060 Uiso 0.836(8) 1 calc PR A 1 H32B H 0.4494 0.0361 0.0181 0.060 Uiso 0.836(8) 1 calc PR A 1 C33 C 0.5048(6) 0.0521(3) 0.2119(6) 0.0584(18) Uani 0.836(8) 1 d PDU A 1 H33A H 0.5543 0.0267 0.2297 0.088 Uiso 0.836(8) 1 calc PR A 1 H33B H 0.4429 0.0422 0.2376 0.088 Uiso 0.836(8) 1 calc PR A 1 H33C H 0.5316 0.0800 0.2613 0.088 Uiso 0.836(8) 1 calc PR A 1 C31' C 0.591(5) 0.073(3) 0.033(7) 0.047(4) Uiso 0.164(8) 1 d PDU A 2 H31C H 0.5281 0.0787 -0.0312 0.056 Uiso 0.164(8) 1 calc PR A 2 H31D H 0.6371 0.0562 -0.0129 0.056 Uiso 0.164(8) 1 calc PR A 2 C32' C 0.5664(19) 0.0395(9) 0.137(3) 0.050(3) Uiso 0.164(8) 1 d PDU A 2 H32C H 0.5602 0.0071 0.1020 0.059 Uiso 0.164(8) 1 calc PR A 2 H32D H 0.6225 0.0399 0.2134 0.059 Uiso 0.164(8) 1 calc PR A 2 C33' C 0.470(2) 0.0526(14) 0.179(4) 0.051(7) Uiso 0.164(8) 1 d PDU A 2 H33D H 0.4595 0.0313 0.2483 0.077 Uiso 0.164(8) 1 calc PR A 2 H33E H 0.4133 0.0500 0.1051 0.077 Uiso 0.164(8) 1 calc PR A 2 H33F H 0.4748 0.0849 0.2115 0.077 Uiso 0.164(8) 1 calc PR A 2 C34 C 0.2689(3) 0.32717(14) 0.4022(4) 0.0412(9) Uani 1 1 d . B . C35 C 0.2121(4) 0.35234(16) 0.4449(4) 0.0497(11) Uani 1 1 d D . . Si2 Si 0.1238(2) 0.38423(9) 0.5195(2) 0.0546(6) Uani 0.710(5) 1 d PDU B 1 C36 C 0.1834(7) 0.4374(3) 0.6003(9) 0.084(2) Uani 0.710(5) 1 d PDU B 1 H36A H 0.1539 0.4425 0.6774 0.100 Uiso 0.710(5) 1 calc PR B 1 H36B H 0.2550 0.4296 0.6332 0.100 Uiso 0.710(5) 1 calc PR B 1 C37 C 0.1813(6) 0.4769(3) 0.5426(7) 0.0632(18) Uani 0.710(5) 1 d PDU B 1 H37A H 0.1111 0.4839 0.4996 0.076 Uiso 0.710(5) 1 calc PR B 1 H37B H 0.2211 0.4744 0.4743 0.076 Uiso 0.710(5) 1 calc PR B 1 C38 C 0.2225(7) 0.5180(3) 0.6341(9) 0.079(2) Uani 0.710(5) 1 d PDU B 1 H38A H 0.1737 0.5262 0.6869 0.118 Uiso 0.710(5) 1 calc PR B 1 H38B H 0.2342 0.5452 0.5824 0.118 Uiso 0.710(5) 1 calc PR B 1 H38C H 0.2858 0.5085 0.6909 0.118 Uiso 0.710(5) 1 calc PR B 1 C39 C 0.0163(6) 0.3975(3) 0.3828(8) 0.0698(19) Uani 0.710(5) 1 d PDU B 1 H39A H -0.0385 0.4112 0.4194 0.084 Uiso 0.710(5) 1 calc PR B 1 H39B H 0.0381 0.4216 0.3271 0.084 Uiso 0.710(5) 1 calc PR B 1 C40 C -0.0253(6) 0.3568(3) 0.2992(8) 0.0699(19) Uani 0.710(5) 1 d PDU B 1 H40A H -0.0505 0.3333 0.3537 0.084 Uiso 0.710(5) 1 calc PR B 1 H40B H 0.0299 0.3421 0.2654 0.084 Uiso 0.710(5) 1 calc PR B 1 C41 C -0.1107(7) 0.3693(4) 0.1836(8) 0.088(3) Uani 0.710(5) 1 d PDU B 1 H41A H -0.1669 0.3829 0.2159 0.132 Uiso 0.710(5) 1 calc PR B 1 H41B H -0.1332 0.3409 0.1338 0.132 Uiso 0.710(5) 1 calc PR B 1 H41C H -0.0864 0.3921 0.1278 0.132 Uiso 0.710(5) 1 calc PR B 1 C42 C 0.0791(7) 0.3478(3) 0.6443(8) 0.082(2) Uani 0.710(5) 1 d PDU B 1 H42A H 0.1209 0.3571 0.7291 0.098 Uiso 0.710(5) 1 calc PR B 1 H42B H 0.0102 0.3587 0.6447 0.098 Uiso 0.710(5) 1 calc PR B 1 C43 C 0.0760(8) 0.3077(4) 0.6448(11) 0.096(3) Uani 0.710(5) 1 d PDU B 1 H43A H 0.1466 0.2980 0.6767 0.116 Uiso 0.710(5) 1 calc PR B 1 H43B H 0.0597 0.2990 0.5519 0.116 Uiso 0.710(5) 1 calc PR B 1 C44 C 0.0106(8) 0.2708(3) 0.7142(9) 0.068(2) Uani 0.710(5) 1 d PDU B 1 H44A H 0.0501 0.2614 0.7991 0.102 Uiso 0.710(5) 1 calc PR B 1 H44B H -0.0057 0.2429 0.6593 0.102 Uiso 0.710(5) 1 calc PR B 1 H44C H -0.0516 0.2859 0.7255 0.102 Uiso 0.710(5) 1 calc PR B 1 Si2' Si 0.0912(5) 0.3818(3) 0.4806(6) 0.0546(6) Uani 0.290(5) 1 d PDU B 2 C36' C 0.1350(15) 0.4307(5) 0.6023(17) 0.059(3) Uiso 0.290(5) 1 d PDU B 2 H36C H 0.1063 0.4191 0.6754 0.070 Uiso 0.290(5) 1 calc PR B 2 H36D H 0.2070 0.4225 0.6274 0.070 Uiso 0.290(5) 1 calc PR B 2 C37' C 0.1407(14) 0.4764(5) 0.6313(19) 0.065(3) Uiso 0.290(5) 1 d PDU B 2 H37C H 0.0844 0.4791 0.6771 0.078 Uiso 0.290(5) 1 calc PR B 2 H37D H 0.1139 0.4898 0.5445 0.078 Uiso 0.290(5) 1 calc PR B 2 C38' C 0.2054(17) 0.5165(7) 0.693(2) 0.068(5) Uiso 0.290(5) 1 d PDU B 2 H38D H 0.1658 0.5454 0.6826 0.102 Uiso 0.290(5) 1 calc PR B 2 H38E H 0.2626 0.5201 0.6505 0.102 Uiso 0.290(5) 1 calc PR B 2 H38F H 0.2298 0.5100 0.7853 0.102 Uiso 0.290(5) 1 calc PR B 2 C39' C 0.0155(15) 0.4096(6) 0.3334(15) 0.060(3) Uiso 0.290(5) 1 d PDU B 2 H39C H -0.0322 0.4323 0.3581 0.073 Uiso 0.290(5) 1 calc PR B 2 H39D H 0.0598 0.4266 0.2856 0.073 Uiso 0.290(5) 1 calc PR B 2 C40' C -0.0413(16) 0.3714(7) 0.2487(19) 0.066(3) Uiso 0.290(5) 1 d PDU B 2 H40C H -0.0848 0.3544 0.2978 0.080 Uiso 0.290(5) 1 calc PR B 2 H40D H 0.0071 0.3486 0.2260 0.080 Uiso 0.290(5) 1 calc PR B 2 C41' C -0.1060(16) 0.3913(8) 0.124(2) 0.076(5) Uiso 0.290(5) 1 d PDU B 2 H41D H -0.1435 0.3658 0.0734 0.114 Uiso 0.290(5) 1 calc PR B 2 H41E H -0.0627 0.4064 0.0725 0.114 Uiso 0.290(5) 1 calc PR B 2 H41F H -0.1531 0.4143 0.1460 0.114 Uiso 0.290(5) 1 calc PR B 2 C42' C 0.0210(15) 0.3357(6) 0.549(2) 0.080(4) Uiso 0.290(5) 1 d PDU B 2 H42C H -0.0063 0.3551 0.6110 0.096 Uiso 0.290(5) 1 calc PR B 2 H42D H -0.0363 0.3320 0.4744 0.096 Uiso 0.290(5) 1 calc PR B 2 C43' C 0.0178(19) 0.3004(6) 0.595(2) 0.077(3) Uiso 0.290(5) 1 d PDU B 2 H43C H 0.0804 0.2846 0.5851 0.093 Uiso 0.290(5) 1 calc PR B 2 H43D H -0.0371 0.2838 0.5363 0.093 Uiso 0.290(5) 1 calc PR B 2 C44' C 0.005(3) 0.2852(10) 0.742(2) 0.086(7) Uiso 0.290(5) 1 d PDU B 2 H44D H 0.0128 0.2512 0.7521 0.129 Uiso 0.290(5) 1 calc PR B 2 H44E H -0.0625 0.2941 0.7532 0.129 Uiso 0.290(5) 1 calc PR B 2 H44F H 0.0553 0.3011 0.8067 0.129 Uiso 0.290(5) 1 calc PR B 2 C45 C 0.2096(4) 0.03630(17) 0.5438(5) 0.0536(11) Uani 1 1 d . . . F1 F 0.2680(3) 0.00773(10) 0.4925(4) 0.0827(10) Uani 1 1 d . . . F2 F 0.2332(3) 0.02832(10) 0.6715(3) 0.0754(9) Uani 1 1 d . . . F3 F 0.1156(2) 0.02111(10) 0.5045(4) 0.0822(10) 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 0.0424(6) 0.0408(6) 0.0272(5) 0.0023(4) 0.0049(4) 0.0037(5) C1 0.036(2) 0.042(2) 0.0260(18) -0.0036(15) -0.0006(15) 0.0023(16) C2 0.041(2) 0.041(2) 0.0233(18) -0.0013(15) -0.0006(16) 0.0023(16) C3 0.038(2) 0.042(2) 0.032(2) -0.0011(16) 0.0012(17) 0.0036(16) C4 0.042(2) 0.043(2) 0.0277(19) 0.0011(16) -0.0020(16) -0.0011(17) C5 0.042(2) 0.045(2) 0.035(2) -0.0024(17) -0.0006(18) 0.0034(18) C6 0.046(3) 0.045(2) 0.036(2) 0.0032(17) 0.0041(18) 0.0002(18) C7 0.045(3) 0.054(3) 0.037(2) 0.0041(19) 0.0057(18) 0.0002(19) C8 0.045(3) 0.051(3) 0.035(2) 0.0001(18) 0.0076(18) 0.0037(19) C9 0.037(2) 0.048(2) 0.0271(19) -0.0002(16) -0.0007(16) -0.0001(17) C10 0.044(2) 0.045(2) 0.030(2) -0.0011(17) 0.0017(17) 0.0018(18) C11 0.035(2) 0.046(2) 0.0258(19) -0.0018(16) -0.0006(15) 0.0021(16) C12 0.042(2) 0.042(2) 0.0272(19) -0.0021(16) 0.0000(16) 0.0021(17) C13 0.037(2) 0.044(2) 0.0239(18) -0.0005(15) -0.0020(16) 0.0021(16) C14 0.042(2) 0.041(2) 0.032(2) -0.0030(16) 0.0000(17) 0.0030(17) C15 0.045(2) 0.043(2) 0.0279(19) -0.0008(16) 0.0021(17) -0.0004(17) C16 0.054(3) 0.041(2) 0.036(2) 0.0002(17) 0.0043(19) -0.0012(19) C17 0.057(3) 0.041(2) 0.040(2) 0.0011(18) 0.005(2) -0.0037(19) C18 0.054(3) 0.050(3) 0.037(2) 0.0009(18) 0.0092(19) -0.007(2) C19 0.049(3) 0.052(3) 0.032(2) -0.0023(18) 0.0068(18) -0.0011(19) C20 0.041(2) 0.042(2) 0.0251(18) -0.0017(15) -0.0017(16) -0.0008(17) C21 0.040(2) 0.045(2) 0.0251(19) -0.0031(16) 0.0035(16) 0.0015(17) C22 0.040(2) 0.040(2) 0.0225(18) -0.0023(15) -0.0018(15) 0.0016(16) C23 0.039(2) 0.041(2) 0.032(2) -0.0009(16) 0.0016(17) -0.0027(17) C24 0.045(2) 0.043(2) 0.032(2) -0.0007(17) 0.0040(18) -0.0035(18) C25 0.060(3) 0.045(2) 0.030(2) 0.0028(17) 0.0031(19) 0.002(2) C26 0.082(4) 0.068(3) 0.058(3) -0.005(3) 0.032(3) -0.021(3) C27 0.057(3) 0.057(3) 0.052(3) 0.015(2) 0.006(2) -0.002(2) C28 0.049(3) 0.069(3) 0.038(2) 0.018(2) 0.003(2) -0.005(2) C29 0.048(3) 0.090(4) 0.079(4) 0.040(3) 0.011(3) 0.013(3) C30 0.054(4) 0.138(6) 0.113(5) 0.080(5) 0.005(4) 0.011(4) C31 0.055(4) 0.039(3) 0.044(3) -0.001(2) 0.007(3) 0.006(3) C32 0.052(3) 0.042(3) 0.054(3) -0.004(2) 0.004(2) -0.003(2) C33 0.056(4) 0.055(3) 0.064(4) 0.019(3) 0.012(3) -0.005(3) C34 0.047(3) 0.043(2) 0.032(2) -0.0009(17) 0.0060(18) 0.0007(18) C35 0.057(3) 0.047(2) 0.047(3) 0.003(2) 0.014(2) 0.003(2) Si2 0.0448(16) 0.0781(11) 0.0353(14) -0.0102(10) -0.0048(10) 0.0195(11) C36 0.078(5) 0.081(4) 0.076(4) -0.020(4) -0.021(4) 0.035(4) C37 0.062(4) 0.073(4) 0.053(3) 0.000(3) 0.010(3) -0.004(3) C38 0.076(5) 0.088(6) 0.070(5) 0.001(4) 0.013(5) 0.017(4) C39 0.063(4) 0.087(4) 0.058(4) -0.005(3) 0.008(3) 0.019(3) C40 0.059(4) 0.096(4) 0.053(4) 0.004(3) 0.007(3) 0.001(3) C41 0.074(6) 0.138(7) 0.050(4) 0.013(5) 0.006(4) 0.000(5) C42 0.068(4) 0.106(5) 0.067(4) -0.021(4) 0.003(3) 0.001(4) C43 0.083(5) 0.108(5) 0.092(4) 0.005(4) 0.004(4) 0.011(4) C44 0.057(5) 0.091(6) 0.057(5) 0.004(4) 0.012(4) 0.004(5) Si2' 0.0448(16) 0.0781(11) 0.0353(14) -0.0102(10) -0.0048(10) 0.0195(11) C45 0.051(3) 0.051(3) 0.058(3) 0.005(2) 0.009(2) 0.000(2) F1 0.104(3) 0.0432(16) 0.115(3) 0.0049(16) 0.056(2) 0.0081(16) F2 0.101(2) 0.0670(19) 0.0546(17) 0.0235(14) 0.0089(16) 0.0011(16) F3 0.062(2) 0.0615(18) 0.113(3) 0.0246(18) -0.0057(18) -0.0143(15) _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 C24 1.845(4) . ? Si1 C31' 1.85(8) . ? Si1 C25 1.864(4) . ? Si1 C28 1.877(4) . ? Si1 C31 1.893(15) . ? C1 C22 1.414(5) . ? C1 C2 1.414(6) . ? C1 C23 1.438(6) . ? C2 C3 1.405(5) . ? C2 C11 1.446(5) . ? C3 C4 1.393(6) . ? C3 H3 0.9500 . ? C4 C5 1.429(6) . ? C4 C9 1.438(6) . ? C5 C6 1.359(6) . ? C5 H5 0.9500 . ? C6 C7 1.423(6) . ? C6 C45 1.484(6) . ? C7 C8 1.355(6) . ? C7 H7 0.9500 . ? C8 C9 1.427(6) . ? C8 H8 0.9500 . ? C9 C10 1.381(6) . ? C10 C11 1.407(6) . ? C10 H10 0.9500 . ? C11 C12 1.414(6) . ? C12 C13 1.415(6) . ? C12 C34 1.427(6) . ? C13 C14 1.400(5) . ? C13 C22 1.444(5) . ? C14 C15 1.385(6) . ? C14 H14 0.9500 . ? C15 C16 1.427(6) . ? C15 C20 1.441(6) . ? C16 C17 1.350(6) . ? C16 H16 0.9500 . ? C17 C18 1.425(6) . ? C17 H17 0.9500 . ? C18 C19 1.358(6) . ? C18 H18 0.9500 . ? C19 C20 1.431(6) . ? C19 H19 0.9500 . ? C20 C21 1.384(5) . ? C21 C22 1.409(6) . ? C21 H21 0.9500 . ? C23 C24 1.208(6) . ? C25 C26 1.500(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.497(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.521(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.535(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.531(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.526(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C31' C32' 1.54(2) . ? C31' H31C 0.9900 . ? C31' H31D 0.9900 . ? C32' C33' 1.520(19) . ? C32' H32C 0.9900 . ? C32' H32D 0.9900 . ? C33' H33D 0.9800 . ? C33' H33E 0.9800 . ? C33' H33F 0.9800 . ? C34 C35 1.209(6) . ? C35 Si2 1.812(5) . ? C35 Si2' 1.953(8) . ? Si2 C36 1.843(8) . ? Si2 C39 1.868(7) . ? Si2 C42 1.874(9) . ? C36 C37 1.278(10) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.548(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.494(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.542(11) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.146(11) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.647(12) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? Si2' C39' 1.854(13) . ? Si2' C42' 1.854(13) . ? Si2' C36' 1.906(12) . ? C36' C37' 1.337(15) . ? C36' H36C 0.9900 . ? C36' H36D 0.9900 . ? C37' C38' 1.506(16) . ? C37' H37C 0.9900 . ? C37' H37D 0.9900 . ? C38' H38D 0.9800 . ? C38' H38E 0.9800 . ? C38' H38F 0.9800 . ? C39' C40' 1.517(16) . ? C39' H39C 0.9900 . ? C39' H39D 0.9900 . ? C40' C41' 1.532(19) . ? C40' H40C 0.9900 . ? C40' H40D 0.9900 . ? C41' H41D 0.9800 . ? C41' H41E 0.9800 . ? C41' H41F 0.9800 . ? C42' C43' 1.126(16) . ? C42' H42C 0.9900 . ? C42' H42D 0.9900 . ? C43' C44' 1.648(19) . ? C43' H43C 0.9900 . ? C43' H43D 0.9900 . ? C44' H44D 0.9800 . ? C44' H44E 0.9800 . ? C44' H44F 0.9800 . ? C45 F1 1.330(6) . ? C45 F3 1.334(5) . ? C45 F2 1.337(5) . ? 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 C24 Si1 C31' 112.1(18) . . ? C24 Si1 C25 106.94(19) . . ? C31' Si1 C25 113.6(14) . . ? C24 Si1 C28 106.7(2) . . ? C31' Si1 C28 107(2) . . ? C25 Si1 C28 110.0(2) . . ? C24 Si1 C31 108.5(4) . . ? C25 Si1 C31 111.0(3) . . ? C28 Si1 C31 113.4(3) . . ? C22 C1 C2 121.2(4) . . ? C22 C1 C23 119.1(4) . . ? C2 C1 C23 119.7(4) . . ? C3 C2 C1 122.3(4) . . ? C3 C2 C11 118.5(4) . . ? C1 C2 C11 119.2(4) . . ? C4 C3 C2 121.8(4) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 122.2(4) . . ? C3 C4 C9 119.5(4) . . ? C5 C4 C9 118.3(4) . . ? C6 C5 C4 120.7(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 121.0(4) . . ? C5 C6 C45 121.4(4) . . ? C7 C6 C45 117.6(4) . . ? C8 C7 C6 120.0(4) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 121.2(4) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 122.2(4) . . ? C10 C9 C4 119.1(4) . . ? C8 C9 C4 118.7(4) . . ? C9 C10 C11 122.2(4) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C10 C11 C12 121.7(4) . . ? C10 C11 C2 118.9(4) . . ? C12 C11 C2 119.5(4) . . ? C11 C12 C13 121.3(4) . . ? C11 C12 C34 118.4(4) . . ? C13 C12 C34 120.3(4) . . ? C14 C13 C12 122.3(4) . . ? C14 C13 C22 118.6(4) . . ? C12 C13 C22 119.1(4) . . ? C15 C14 C13 122.7(4) . . ? C15 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? C14 C15 C16 122.4(4) . . ? C14 C15 C20 118.9(4) . . ? C16 C15 C20 118.7(4) . . ? C17 C16 C15 121.1(4) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 120.3(4) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.6(4) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 122.5(4) . . ? C21 C20 C15 119.2(4) . . ? C19 C20 C15 118.3(4) . . ? C20 C21 C22 122.3(4) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C21 C22 C1 121.9(4) . . ? C21 C22 C13 118.4(3) . . ? C1 C22 C13 119.7(4) . . ? C24 C23 C1 177.5(4) . . ? C23 C24 Si1 176.8(4) . . ? C26 C25 Si1 116.4(3) . . ? C26 C25 H25A 108.2 . . ? Si1 C25 H25A 108.2 . . ? C26 C25 H25B 108.2 . . ? Si1 C25 H25B 108.2 . . ? H25A C25 H25B 107.3 . . ? C27 C26 C25 116.9(4) . . ? C27 C26 H26A 108.1 . . ? C25 C26 H26A 108.1 . . ? C27 C26 H26B 108.1 . . ? C25 C26 H26B 108.1 . . ? H26A C26 H26B 107.3 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 Si1 114.9(4) . . ? C29 C28 H28A 108.6 . . ? Si1 C28 H28A 108.6 . . ? C29 C28 H28B 108.6 . . ? Si1 C28 H28B 108.6 . . ? H28A C28 H28B 107.5 . . ? C28 C29 C30 112.6(6) . . ? C28 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? C28 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 Si1 117.1(8) . . ? C32 C31 H31A 108.0 . . ? Si1 C31 H31A 108.0 . . ? C32 C31 H31B 108.0 . . ? Si1 C31 H31B 108.0 . . ? H31A C31 H31B 107.3 . . ? C33 C32 C31 111.6(6) . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C32' C31' Si1 118(5) . . ? C32' C31' H31C 107.8 . . ? Si1 C31' H31C 107.8 . . ? C32' C31' H31D 107.8 . . ? Si1 C31' H31D 107.8 . . ? H31C C31' H31D 107.1 . . ? C33' C32' C31' 113(3) . . ? C33' C32' H32C 109.1 . . ? C31' C32' H32C 109.1 . . ? C33' C32' H32D 109.1 . . ? C31' C32' H32D 109.1 . . ? H32C C32' H32D 107.8 . . ? C32' C33' H33D 109.5 . . ? C32' C33' H33E 109.5 . . ? H33D C33' H33E 109.5 . . ? C32' C33' H33F 109.5 . . ? H33D C33' H33F 109.5 . . ? H33E C33' H33F 109.5 . . ? C35 C34 C12 175.6(5) . . ? C34 C35 Si2 173.4(4) . . ? C34 C35 Si2' 163.2(5) . . ? C35 Si2 C36 110.2(4) . . ? C35 Si2 C39 104.6(3) . . ? C36 Si2 C39 113.0(4) . . ? C35 Si2 C42 111.6(3) . . ? C36 Si2 C42 107.9(5) . . ? C39 Si2 C42 109.6(4) . . ? C37 C36 Si2 122.8(6) . . ? C37 C36 H36A 106.6 . . ? Si2 C36 H36A 106.6 . . ? C37 C36 H36B 106.6 . . ? Si2 C36 H36B 106.6 . . ? H36A C36 H36B 106.6 . . ? C36 C37 C38 113.7(7) . . ? C36 C37 H37A 108.8 . . ? C38 C37 H37A 108.8 . . ? C36 C37 H37B 108.8 . . ? C38 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? C40 C39 Si2 116.0(6) . . ? C40 C39 H39A 108.3 . . ? Si2 C39 H39A 108.3 . . ? C40 C39 H39B 108.3 . . ? Si2 C39 H39B 108.3 . . ? H39A C39 H39B 107.4 . . ? C39 C40 C41 114.7(8) . . ? C39 C40 H40A 108.6 . . ? C41 C40 H40A 108.6 . . ? C39 C40 H40B 108.6 . . ? C41 C40 H40B 108.6 . . ? H40A C40 H40B 107.6 . . ? C43 C42 Si2 125.1(8) . . ? C43 C42 H42A 106.0 . . ? Si2 C42 H42A 106.0 . . ? C43 C42 H42B 106.0 . . ? Si2 C42 H42B 106.0 . . ? H42A C42 H42B 106.3 . . ? C42 C43 C44 131.7(10) . . ? C42 C43 H43A 104.3 . . ? C44 C43 H43A 104.3 . . ? C42 C43 H43B 104.3 . . ? C44 C43 H43B 104.3 . . ? H43A C43 H43B 105.6 . . ? C39' Si2' C42' 112.6(9) . . ? C39' Si2' C36' 106.9(8) . . ? C42' Si2' C36' 111.9(9) . . ? C39' Si2' C35 111.6(8) . . ? C42' Si2' C35 107.0(8) . . ? C36' Si2' C35 106.6(7) . . ? C37' C36' Si2' 149.7(16) . . ? C37' C36' H36C 99.3 . . ? Si2' C36' H36C 99.3 . . ? C37' C36' H36D 99.3 . . ? Si2' C36' H36D 99.3 . . ? H36C C36' H36D 104.0 . . ? C36' C37' C38' 147.2(19) . . ? C36' C37' H37C 100.0 . . ? C38' C37' H37C 100.0 . . ? C36' C37' H37D 100.0 . . ? C38' C37' H37D 100.0 . . ? H37C C37' H37D 104.2 . . ? C37' C38' H38D 109.5 . . ? C37' C38' H38E 109.5 . . ? H38D C38' H38E 109.5 . . ? C37' C38' H38F 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? C40' C39' Si2' 108.2(12) . . ? C40' C39' H39C 110.1 . . ? Si2' C39' H39C 110.1 . . ? C40' C39' H39D 110.1 . . ? Si2' C39' H39D 110.1 . . ? H39C C39' H39D 108.4 . . ? C39' C40' C41' 111.8(15) . . ? C39' C40' H40C 109.3 . . ? C41' C40' H40C 109.3 . . ? C39' C40' H40D 109.3 . . ? C41' C40' H40D 109.3 . . ? H40C C40' H40D 107.9 . . ? C40' C41' H41D 109.5 . . ? C40' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? C40' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? C43' C42' Si2' 151(2) . . ? C43' C42' H42C 98.9 . . ? Si2' C42' H42C 98.9 . . ? C43' C42' H42D 98.9 . . ? Si2' C42' H42D 98.9 . . ? H42C C42' H42D 103.9 . . ? C42' C43' C44' 132(2) . . ? C42' C43' H43C 104.3 . . ? C44' C43' H43C 104.3 . . ? C42' C43' H43D 104.3 . . ? C44' C43' H43D 104.3 . . ? H43C C43' H43D 105.6 . . ? C43' C44' H44D 109.5 . . ? C43' C44' H44E 109.5 . . ? H44D C44' H44E 109.5 . . ? C43' C44' H44F 109.5 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 109.5 . . ? F1 C45 F3 107.0(4) . . ? F1 C45 F2 105.4(4) . . ? F3 C45 F2 105.8(4) . . ? F1 C45 C6 114.0(4) . . ? F3 C45 C6 112.3(4) . . ? F2 C45 C6 111.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C22 C1 C2 C3 179.5(3) . . . . ? C23 C1 C2 C3 -2.2(5) . . . . ? C22 C1 C2 C11 -0.8(5) . . . . ? C23 C1 C2 C11 177.5(3) . . . . ? C1 C2 C3 C4 178.9(4) . . . . ? C11 C2 C3 C4 -0.8(5) . . . . ? C2 C3 C4 C5 -178.4(3) . . . . ? C2 C3 C4 C9 0.3(6) . . . . ? C3 C4 C5 C6 179.4(4) . . . . ? C9 C4 C5 C6 0.7(6) . . . . ? C4 C5 C6 C7 0.0(6) . . . . ? C4 C5 C6 C45 -177.9(4) . . . . ? C5 C6 C7 C8 -0.2(6) . . . . ? C45 C6 C7 C8 177.7(4) . . . . ? C6 C7 C8 C9 -0.3(6) . . . . ? C7 C8 C9 C10 -179.0(4) . . . . ? C7 C8 C9 C4 1.0(6) . . . . ? C3 C4 C9 C10 0.1(5) . . . . ? C5 C4 C9 C10 178.9(3) . . . . ? C3 C4 C9 C8 -179.9(4) . . . . ? C5 C4 C9 C8 -1.1(5) . . . . ? C8 C9 C10 C11 180.0(4) . . . . ? C4 C9 C10 C11 0.0(6) . . . . ? C9 C10 C11 C12 179.6(4) . . . . ? C9 C10 C11 C2 -0.5(6) . . . . ? C3 C2 C11 C10 0.9(5) . . . . ? C1 C2 C11 C10 -178.9(3) . . . . ? C3 C2 C11 C12 -179.2(3) . . . . ? C1 C2 C11 C12 1.1(5) . . . . ? C10 C11 C12 C13 178.3(3) . . . . ? C2 C11 C12 C13 -1.6(5) . . . . ? C10 C11 C12 C34 -3.0(5) . . . . ? C2 C11 C12 C34 177.1(3) . . . . ? C11 C12 C13 C14 -179.2(3) . . . . ? C34 C12 C13 C14 2.1(6) . . . . ? C11 C12 C13 C22 1.8(5) . . . . ? C34 C12 C13 C22 -176.9(3) . . . . ? C12 C13 C14 C15 -179.6(4) . . . . ? C22 C13 C14 C15 -0.6(5) . . . . ? C13 C14 C15 C16 -179.5(4) . . . . ? C13 C14 C15 C20 0.9(6) . . . . ? C14 C15 C16 C17 178.5(4) . . . . ? C20 C15 C16 C17 -1.9(6) . . . . ? C15 C16 C17 C18 1.5(6) . . . . ? C16 C17 C18 C19 -0.2(7) . . . . ? C17 C18 C19 C20 -0.6(6) . . . . ? C18 C19 C20 C21 -178.8(4) . . . . ? C18 C19 C20 C15 0.2(6) . . . . ? C14 C15 C20 C21 -0.3(5) . . . . ? C16 C15 C20 C21 -179.9(4) . . . . ? C14 C15 C20 C19 -179.4(4) . . . . ? C16 C15 C20 C19 1.0(5) . . . . ? C19 C20 C21 C22 178.5(4) . . . . ? C15 C20 C21 C22 -0.5(5) . . . . ? C20 C21 C22 C1 -178.9(3) . . . . ? C20 C21 C22 C13 0.8(5) . . . . ? C2 C1 C22 C21 -179.2(3) . . . . ? C23 C1 C22 C21 2.4(5) . . . . ? C2 C1 C22 C13 1.1(5) . . . . ? C23 C1 C22 C13 -177.3(3) . . . . ? C14 C13 C22 C21 -0.3(5) . . . . ? C12 C13 C22 C21 178.7(3) . . . . ? C14 C13 C22 C1 179.4(3) . . . . ? C12 C13 C22 C1 -1.6(5) . . . . ? C24 Si1 C25 C26 50.3(4) . . . . ? C31' Si1 C25 C26 175(2) . . . . ? C28 Si1 C25 C26 -65.2(4) . . . . ? C31 Si1 C25 C26 168.5(5) . . . . ? Si1 C25 C26 C27 -177.7(4) . . . . ? C24 Si1 C28 C29 174.7(3) . . . . ? C31' Si1 C28 C29 54.4(16) . . . . ? C25 Si1 C28 C29 -69.6(4) . . . . ? C31 Si1 C28 C29 55.3(5) . . . . ? Si1 C28 C29 C30 177.4(4) . . . . ? C24 Si1 C31 C32 -21.9(7) . . . . ? C31' Si1 C31 C32 105(16) . . . . ? C25 Si1 C31 C32 -139.1(5) . . . . ? C28 Si1 C31 C32 96.5(6) . . . . ? Si1 C31 C32 C33 -65.5(7) . . . . ? C24 Si1 C31' C32' -69(4) . . . . ? C25 Si1 C31' C32' 170(3) . . . . ? C28 Si1 C31' C32' 48(4) . . . . ? C31 Si1 C31' C32' -124(18) . . . . ? Si1 C31' C32' C33' 79(5) . . . . ? Si2' C35 Si2 C36 -139.6(11) . . . . ? Si2' C35 Si2 C39 -18.0(10) . . . . ? Si2' C35 Si2 C42 100.5(11) . . . . ? C35 Si2 C36 C37 90.1(9) . . . . ? C39 Si2 C36 C37 -26.5(11) . . . . ? C42 Si2 C36 C37 -147.8(9) . . . . ? Si2 C36 C37 C38 171.7(7) . . . . ? C35 Si2 C39 C40 50.7(7) . . . . ? C36 Si2 C39 C40 170.5(7) . . . . ? C42 Si2 C39 C40 -69.1(8) . . . . ? Si2 C39 C40 C41 -177.3(6) . . . . ? C35 Si2 C42 C43 -26.2(12) . . . . ? C36 Si2 C42 C43 -147.4(10) . . . . ? C39 Si2 C42 C43 89.2(11) . . . . ? Si2 C42 C43 C44 -158.6(9) . . . . ? C34 C35 Si2' C39' -63.1(17) . . . . ? Si2 C35 Si2' C39' 140.3(14) . . . . ? C34 C35 Si2' C42' 60.5(17) . . . . ? Si2 C35 Si2' C42' -96.1(13) . . . . ? Si2 C35 Si2' C36' 23.9(10) . . . . ? C39' Si2' C36' C37' -5(4) . . . . ? C42' Si2' C36' C37' -128(3) . . . . ? C35 Si2' C36' C37' 115(3) . . . . ? Si2' C36' C37' C38' -135(3) . . . . ? C42' Si2' C39' C40' -42.8(19) . . . . ? C36' Si2' C39' C40' -166.2(15) . . . . ? C35 Si2' C39' C40' 77.6(16) . . . . ? Si2' C39' C40' C41' -179.8(16) . . . . ? C39' Si2' C42' C43' 141(4) . . . . ? C36' Si2' C42' C43' -99(4) . . . . ? C35 Si2' C42' C43' 18(4) . . . . ? Si2' C42' C43' C44' 111(4) . . . . ? C5 C6 C45 F1 0.5(6) . . . . ? C7 C6 C45 F1 -177.4(4) . . . . ? C5 C6 C45 F3 -121.4(5) . . . . ? C7 C6 C45 F3 60.7(6) . . . . ? C5 C6 C45 F2 119.9(5) . . . . ? C7 C6 C45 F2 -58.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 68.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.613 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.064