# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ; Department of Polymer Chemistry, Graduate School of Engineering, Kyoto University, ; _publ_contact_author_email chujo_at_chujo.synchem.kyoto-u.ac.jp _publ_contact_author_fax ' +81-75-383-2607 ' _publ_contact_author_phone ' +81-75-383-2604 ' #TrackingRef '- 1C.cif' _publ_contact_author_name 'Yoshiki Chujo' loop_ _publ_author_name 'Yuichiro Tokoro' 'Hyeonuk Yeo' 'Kazuo Tanaka' 'Yoshiki Chujo' data_1 _database_code_depnum_ccdc_archive 'CCDC 888302' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H17 N Si' _chemical_formula_weight 251.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_21/m _symmetry_space_group_name_Hall -p_2yb _space_group_IT_number 11:b loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.2798(6) _cell_length_b 6.9773(5) _cell_length_c 10.5690(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.586(3) _cell_angle_gamma 90.00 _cell_volume 682.13(8) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 268 _exptl_absorpt_coefficient_mu 0.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9553 _exptl_absorpt_correction_T_max 0.9553 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5341 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1302 _reflns_number_gt 1105 _reflns_threshold_expression >2\s(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'Yadokari-XG (Wakita, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG (Wakita, 2000)' _computing_publication_material 'Yadokari-XG (Wakita, 2000)' _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^)+(0.0812P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1302 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.60491(19) 0.0233(3) 0.7595(2) 0.0305(4) Uani 1 1 d . . . H1 H 0.548(3) 0.044(4) 0.688(3) 0.086(9) Uiso 1 1 d . . . H2 H 0.547(3) -0.021(4) 0.820(3) 0.088(9) Uiso 1 1 d . . . H3 H 0.667(3) -0.071(4) 0.745(3) 0.080(8) Uiso 1 1 d . . . C2 C 0.6628(3) 0.2500 0.9927(3) 0.0356(6) Uani 1 2 d S . . H4 H 0.563(3) 0.2500 1.004(3) 0.041(7) Uiso 1 2 d S . . H5 H 0.7022(19) 0.141(3) 1.0395(19) 0.041(5) Uiso 1 1 d . . . C3 C 0.9000(2) 0.2500 0.8141(2) 0.0242(5) Uani 1 2 d S . . C4 C 0.9746(2) 0.2500 0.6999(2) 0.0231(5) Uani 1 2 d S . . C5 C 0.8976(2) 0.2500 0.5765(2) 0.0225(5) Uani 1 2 d S . . C6 C 0.6768(3) 0.2500 0.4608(2) 0.0281(6) Uani 1 2 d S . . H6 H 0.575(3) 0.2500 0.459(3) 0.040(7) Uiso 1 2 d S . . C7 C 0.7396(3) 0.2500 0.3447(2) 0.0346(6) Uani 1 2 d S . . H7 H 0.681(3) 0.2500 0.270(3) 0.039(7) Uiso 1 2 d S . . C8 C 0.8880(3) 0.2500 0.3480(3) 0.0355(6) Uani 1 2 d S . . H8 H 0.934(3) 0.2500 0.280(3) 0.061(10) Uiso 1 2 d S . . C9 C 0.9717(2) 0.2500 0.4638(2) 0.0288(6) Uani 1 2 d S . . C10 C 1.1266(3) 0.2500 0.4759(3) 0.0380(7) Uani 1 2 d S . . H9 H 1.174(3) 0.2500 0.395(3) 0.066(10) Uiso 1 2 d S . . C11 C 1.1996(3) 0.2500 0.5898(3) 0.0361(7) Uani 1 2 d S . . H10 H 1.301(3) 0.2500 0.598(3) 0.043(8) Uiso 1 2 d S . . C12 C 1.1285(2) 0.2500 0.7065(3) 0.0304(6) Uani 1 2 d S . . C13 C 1.2069(2) 0.2500 0.8252(3) 0.0379(7) Uani 1 2 d S . . H11 H 1.312(3) 0.2500 0.828(2) 0.038(7) Uiso 1 2 d S . . C14 C 1.1372(3) 0.2500 0.9342(3) 0.0429(7) Uani 1 2 d S . . H12 H 1.190(3) 0.2500 1.016(3) 0.049(8) Uiso 1 2 d S . . C15 C 0.9855(3) 0.2500 0.9274(3) 0.0349(6) Uani 1 2 d S . . H13 H 0.942(3) 0.2500 1.008(3) 0.056(9) Uiso 1 2 d S . . Si1 Si 0.69532(6) 0.2500 0.81908(6) 0.0232(3) Uani 1 2 d S . . N1 N 0.75089(19) 0.2500 0.57206(18) 0.0238(5) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0303(9) 0.0269(9) 0.0352(11) -0.0015(8) 0.0086(8) -0.0034(8) C2 0.0461(16) 0.0345(14) 0.0278(15) 0.000 0.0132(12) 0.000 C3 0.0287(11) 0.0222(11) 0.0215(13) 0.000 0.0006(9) 0.000 C4 0.0234(11) 0.0165(10) 0.0296(14) 0.000 0.0038(9) 0.000 C5 0.0256(11) 0.0159(10) 0.0266(13) 0.000 0.0060(9) 0.000 C6 0.0313(12) 0.0270(11) 0.0254(14) 0.000 -0.0016(10) 0.000 C7 0.0527(15) 0.0281(12) 0.0225(14) 0.000 -0.0002(12) 0.000 C8 0.0589(17) 0.0260(12) 0.0235(15) 0.000 0.0165(12) 0.000 C9 0.0394(13) 0.0193(10) 0.0296(15) 0.000 0.0139(10) 0.000 C10 0.0400(14) 0.0297(13) 0.0475(18) 0.000 0.0243(13) 0.000 C11 0.0221(12) 0.0258(12) 0.062(2) 0.000 0.0150(12) 0.000 C12 0.0239(11) 0.0195(11) 0.0479(17) 0.000 0.0034(11) 0.000 C13 0.0228(12) 0.0308(13) 0.058(2) 0.000 -0.0066(12) 0.000 C14 0.0396(14) 0.0442(15) 0.0413(18) 0.000 -0.0187(13) 0.000 C15 0.0380(13) 0.0380(14) 0.0277(15) 0.000 -0.0041(11) 0.000 Si1 0.0262(4) 0.0224(4) 0.0217(4) 0.000 0.0069(3) 0.000 N1 0.0262(9) 0.0224(9) 0.0230(11) 0.000 0.0039(8) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 Si1 1.8755(17) . ? C2 Si1 1.884(3) . ? C3 C15 1.382(3) . ? C3 C4 1.439(3) . ? C3 Si1 1.904(2) . ? C4 C12 1.424(3) . ? C4 C5 1.436(3) . ? C5 N1 1.359(3) . ? C5 C9 1.422(3) . ? C6 N1 1.314(3) . ? C6 C7 1.400(4) . ? C7 C8 1.375(4) . ? C8 C9 1.397(4) . ? C9 C10 1.433(3) . ? C10 C11 1.333(4) . ? C11 C12 1.445(4) . ? C12 C13 1.399(4) . ? C13 C14 1.365(4) . ? C14 C15 1.404(4) . ? Si1 C1 1.8755(17) 4_565 ? 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 C15 C3 C4 116.4(2) . . ? C15 C3 Si1 118.76(18) . . ? C4 C3 Si1 124.83(17) . . ? C12 C4 C5 117.9(2) . . ? C12 C4 C3 120.5(2) . . ? C5 C4 C3 121.59(19) . . ? N1 C5 C9 121.4(2) . . ? N1 C5 C4 117.14(19) . . ? C9 C5 C4 121.45(19) . . ? N1 C6 C7 124.0(2) . . ? C8 C7 C6 117.7(2) . . ? C7 C8 C9 120.5(2) . . ? C8 C9 C5 117.5(2) . . ? C8 C9 C10 124.2(2) . . ? C5 C9 C10 118.3(2) . . ? C11 C10 C9 120.9(2) . . ? C10 C11 C12 122.5(2) . . ? C13 C12 C4 119.4(2) . . ? C13 C12 C11 121.7(2) . . ? C4 C12 C11 118.9(2) . . ? C14 C13 C12 120.6(2) . . ? C13 C14 C15 119.8(3) . . ? C3 C15 C14 123.3(3) . . ? C1 Si1 C1 115.00(13) 4_565 . ? C1 Si1 C2 102.98(8) 4_565 . ? C1 Si1 C2 102.98(8) . . ? C1 Si1 C3 114.28(6) 4_565 . ? C1 Si1 C3 114.28(6) . . ? C2 Si1 C3 105.35(12) . . ? C6 N1 C5 118.85(19) . . ? 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 C15 C3 C4 C12 0.0 . . . . ? Si1 C3 C4 C12 180.0 . . . . ? C15 C3 C4 C5 180.0 . . . . ? Si1 C3 C4 C5 0.0 . . . . ? C12 C4 C5 N1 180.0 . . . . ? C3 C4 C5 N1 0.0 . . . . ? C12 C4 C5 C9 0.0 . . . . ? C3 C4 C5 C9 180.0 . . . . ? N1 C6 C7 C8 0.0 . . . . ? C6 C7 C8 C9 0.0 . . . . ? C7 C8 C9 C5 0.0 . . . . ? C7 C8 C9 C10 180.0 . . . . ? N1 C5 C9 C8 0.0 . . . . ? C4 C5 C9 C8 180.0 . . . . ? N1 C5 C9 C10 180.0 . . . . ? C4 C5 C9 C10 0.0 . . . . ? C8 C9 C10 C11 180.0 . . . . ? C5 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C5 C4 C12 C13 180.0 . . . . ? C3 C4 C12 C13 0.0 . . . . ? C5 C4 C12 C11 0.0 . . . . ? C3 C4 C12 C11 180.0 . . . . ? C10 C11 C12 C13 180.0 . . . . ? C10 C11 C12 C4 0.0 . . . . ? C4 C12 C13 C14 0.0 . . . . ? C11 C12 C13 C14 180.0 . . . . ? C12 C13 C14 C15 0.000(1) . . . . ? C4 C3 C15 C14 0.000(1) . . . . ? Si1 C3 C15 C14 180.0 . . . . ? C13 C14 C15 C3 0.000(1) . . . . ? C15 C3 Si1 C1 112.30(8) . . . 4_565 ? C4 C3 Si1 C1 -67.70(8) . . . 4_565 ? C15 C3 Si1 C1 -112.30(8) . . . . ? C4 C3 Si1 C1 67.70(8) . . . . ? C15 C3 Si1 C2 0.0 . . . . ? C4 C3 Si1 C2 180.0 . . . . ? C7 C6 N1 C5 0.0 . . . . ? C9 C5 N1 C6 0.0 . . . . ? C4 C5 N1 C6 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.512 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.057 # Attachment '- 1E.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 888303' #TrackingRef '- 1E.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C18H13NSi _chemical_formula_sum 'C18 H13 N Si' _chemical_formula_weight 271.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5359(18) _cell_length_b 14.647(2) _cell_length_c 16.586(2) _cell_angle_alpha 90.159(4) _cell_angle_beta 109.894(4) _cell_angle_gamma 98.672(4) _cell_volume 2826.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 95(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9847 _exptl_absorpt_correction_T_max 0.9847 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 95(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20858 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.1014 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9619 _reflns_number_gt 6204 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1336P)^2^+11.2724P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9619 _refine_ls_number_parameters 817 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1422 _refine_ls_R_factor_gt 0.1052 _refine_ls_wR_factor_ref 0.3138 _refine_ls_wR_factor_gt 0.2756 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.79296(14) 0.42196(12) 0.60515(11) 0.0387(4) Uani 1 1 d . . . Si2 Si 0.80200(14) 0.13647(12) 0.10969(11) 0.0389(4) Uani 1 1 d . . . Si3 Si 0.21458(14) 0.11629(12) 0.46148(11) 0.0399(4) Uani 1 1 d . . . Si4 Si 0.21168(14) 0.32598(12) -0.04713(11) 0.0396(4) Uani 1 1 d . . . C95 C 0.6417(5) 0.1317(4) 0.0568(4) 0.0350(12) Uani 1 1 d . . . C94 C 0.3724(5) 0.3534(4) -0.0187(4) 0.0340(12) Uani 1 1 d . . . C97 C 0.4464(5) 0.3348(4) 0.0599(4) 0.0344(13) Uani 1 1 d . . . C96 C 0.5937(5) 0.1605(4) -0.0269(4) 0.0370(13) Uani 1 1 d . . . C9 C 0.6319(5) 0.3939(4) 0.5438(4) 0.0361(13) Uani 1 1 d . . . N10 N 0.7832(4) 0.2156(3) -0.0236(3) 0.0376(11) Uani 1 1 d . . . C11 C 0.3710(5) 0.1205(4) 0.4785(4) 0.0336(12) Uani 1 1 d . . . C12 C 0.4094(5) 0.0857(4) 0.4154(3) 0.0345(12) Uani 1 1 d . . . C13 C 0.4237(5) 0.3931(4) -0.0776(3) 0.0318(12) Uani 1 1 d . . . C14 C 0.3991(5) 0.1124(4) -0.0271(4) 0.0397(14) Uani 1 1 d . . . H74 H 0.3181 0.1042 -0.0550 0.048 Uiso 1 1 calc R . . C15 C 0.3228(5) 0.0445(4) 0.3359(4) 0.0366(13) Uani 1 1 d . . . C16 C 0.5883(5) 0.3554(4) 0.4589(4) 0.0355(13) Uani 1 1 d . . . C17 C 0.4459(5) 0.0871(4) 0.0560(4) 0.0399(14) Uani 1 1 d . . . H75 H 0.3966 0.0634 0.0863 0.048 Uiso 1 1 calc R . . C18 C 0.5661(5) 0.3531(4) 0.0813(4) 0.0363(13) Uani 1 1 d . . . H76 H 0.6142 0.3403 0.1367 0.044 Uiso 1 1 calc R . . C19 C 0.8574(6) 0.3145(4) 0.4440(4) 0.0456(15) Uani 1 1 d . . . N11 N 0.2122(4) 0.0427(4) 0.3294(3) 0.0405(12) Uani 1 1 d . . . C21 C 0.5035(5) 0.2191(4) -0.1965(4) 0.0375(13) Uani 1 1 d . . . H77 H 0.4727 0.2377 -0.2535 0.045 Uiso 1 1 calc R . . C22 C 0.5558(5) 0.0495(4) 0.3594(4) 0.0402(14) Uani 1 1 d . . . C23 C 0.3504(5) 0.4177(4) -0.1590(4) 0.0363(13) Uani 1 1 d . . . C24 C 0.4575(5) 0.1567(4) 0.5555(4) 0.0359(13) Uani 1 1 d . . . C25 C 0.5251(5) 0.0879(4) 0.4276(4) 0.0366(13) Uani 1 1 d . . . C26 C 0.6696(5) 0.3267(4) 0.4229(4) 0.0390(13) Uani 1 1 d . . . C27 C 0.7966(5) 0.4813(5) 0.7064(4) 0.0446(15) Uani 1 1 d . . . C28 C 0.8718(5) 0.0612(5) 0.0595(4) 0.0444(15) Uani 1 1 d . . . H53 H 0.9462 0.0948 0.0608 0.067 Uiso 1 1 calc R . . H54 H 0.8225 0.0440 -0.0001 0.067 Uiso 1 1 calc R . . H55 H 0.8835 0.0053 0.0915 0.067 Uiso 1 1 calc R . . C29 C 0.4740(5) 0.1508(4) -0.0705(4) 0.0388(13) Uani 1 1 d . . . C30 C 0.1289(6) 0.0055(5) 0.2586(4) 0.0467(15) Uani 1 1 d . . . N9 N 0.2360(4) 0.4022(3) -0.1735(3) 0.0426(12) Uani 1 1 d . . . C32 C 0.4314(5) 0.1792(4) -0.1576(4) 0.0423(14) Uani 1 1 d . . . H72 H 0.3509 0.1695 -0.1880 0.051 Uiso 1 1 calc R . . N12 N 0.7814(4) 0.3437(3) 0.4727(3) 0.0374(11) Uani 1 1 d . . . C34 C 0.5531(5) 0.4118(4) 0.5810(4) 0.0373(13) Uani 1 1 d . . . C35 C 0.2205(5) 0.1749(5) 0.5657(4) 0.0465(15) Uani 1 1 d . . . C36 C 0.8211(6) 0.2910(5) -0.1409(4) 0.0468(15) Uani 1 1 d . . . H61 H 0.8763 0.3202 -0.1641 0.056 Uiso 1 1 calc R . . C37 C 0.8563(6) 0.2593(5) -0.0581(4) 0.0460(15) Uani 1 1 d . . . C38 C 0.6694(5) 0.2051(4) -0.0694(4) 0.0371(13) Uani 1 1 d . . . C39 C 0.8267(6) 0.2696(5) 0.3624(4) 0.0488(16) Uani 1 1 d . . . C40 C 0.6251(5) 0.2342(4) -0.1540(4) 0.0375(13) Uani 1 1 d . . . C41 C 0.5649(5) 0.0958(4) 0.0963(4) 0.0395(14) Uani 1 1 d . . . C42 C 0.8604(5) 0.3207(5) 0.6464(4) 0.0436(15) Uani 1 1 d . . . C43 C 0.5736(5) 0.1598(4) 0.5690(4) 0.0390(14) Uani 1 1 d . . . C44 C 0.1378(5) 0.0011(5) 0.4679(4) 0.0436(14) Uani 1 1 d . . . C45 C 0.8824(5) 0.5156(4) 0.5678(4) 0.0454(15) Uani 1 1 d . . . H62 H 0.9286 0.5592 0.6163 0.068 Uiso 1 1 calc R . . H63 H 0.8318 0.5483 0.5228 0.068 Uiso 1 1 calc R . . H64 H 0.9333 0.4879 0.5448 0.068 Uiso 1 1 calc R . . C46 C 0.6290(6) 0.2836(4) 0.3391(4) 0.0440(15) Uani 1 1 d . . . C47 C 0.5441(5) 0.4106(4) -0.0575(4) 0.0352(13) Uani 1 1 d . . . C48 C 0.4751(5) 0.0113(4) 0.2854(4) 0.0422(14) Uani 1 1 d . . . C49 C 0.5201(6) 0.4740(4) -0.1970(4) 0.0460(15) Uani 1 1 d . . . C50 C 0.1286(5) 0.1911(5) 0.3824(4) 0.0504(16) Uani 1 1 d . . . H65 H 0.0559 0.1542 0.3463 0.076 Uiso 1 1 calc R . . H66 H 0.1721 0.2168 0.3462 0.076 Uiso 1 1 calc R . . H67 H 0.1127 0.2417 0.4131 0.076 Uiso 1 1 calc R . . C51 C 0.8115(5) 0.0736(4) 0.2108(4) 0.0438(15) Uani 1 1 d . . . C52 C 0.1332(5) 0.4230(5) -0.0491(5) 0.0495(16) Uani 1 1 d . . . C53 C 0.3198(7) 0.4834(5) -0.2961(4) 0.0535(18) Uani 1 1 d . . . C54 C 0.3972(6) 0.4577(4) -0.2190(4) 0.0424(14) Uani 1 1 d . . . C55 C 0.3549(5) 0.0072(4) 0.2704(4) 0.0379(13) Uani 1 1 d . . . C56 C 0.2655(5) -0.0325(4) 0.1967(4) 0.0415(14) Uani 1 1 d . . . H56 H 0.2830 -0.0585 0.1510 0.050 Uiso 1 1 calc R . . C57 C 0.4344(5) 0.3940(4) 0.5356(4) 0.0436(15) Uani 1 1 d . . . C58 C 0.6082(5) 0.1257(4) 0.5057(4) 0.0402(14) Uani 1 1 d . . . C59 C 0.8871(6) 0.2492(5) 0.1556(4) 0.0538(17) Uani 1 1 d . . . C60 C 0.3931(5) 0.3604(4) 0.4503(5) 0.0468(16) Uani 1 1 d . . . C61 C 0.6142(5) 0.3889(4) 0.0236(4) 0.0387(14) Uani 1 1 d . . . H71 H 0.6954 0.3993 0.0383 0.046 Uiso 1 1 calc R . . C62 C 0.4345(6) 0.2969(4) 0.3251(4) 0.0472(16) Uani 1 1 d . . . C63 C 0.4716(5) 0.3389(4) 0.4118(4) 0.0415(14) Uani 1 1 d . . . C64 C 0.5885(6) 0.4499(5) -0.1206(5) 0.0467(16) Uani 1 1 d . . . C65 C 0.5084(6) 0.2713(4) 0.2919(4) 0.0435(15) Uani 1 1 d . . . H70 H 0.4805 0.2441 0.2350 0.052 Uiso 1 1 calc R . . C66 C 0.7065(5) 0.2795(4) -0.1884(4) 0.0424(14) Uani 1 1 d . . . C67 C 0.1664(6) 0.4283(5) -0.2462(4) 0.0561(18) Uani 1 1 d . . . H57 H 0.0861 0.4183 -0.2563 0.067 Uiso 1 1 calc R . . C69 C 0.1315(5) 0.2296(4) -0.1292(4) 0.0462(15) Uani 1 1 d . . . H47 H 0.1184 0.1729 -0.1003 0.069 Uiso 1 1 calc R . . H48 H 0.1767 0.2196 -0.1655 0.069 Uiso 1 1 calc R . . H49 H 0.0575 0.2457 -0.1649 0.069 Uiso 1 1 calc R . . C70 C 0.8050(6) 0.5254(5) 0.7706(5) 0.0537(17) Uani 1 1 d . . . C71 C 0.7138(6) 0.2550(4) 0.3111(4) 0.0490(16) Uani 1 1 d . . . H58 H 0.6920 0.2250 0.2556 0.059 Uiso 1 1 calc R . . C72 C 0.1967(5) 0.2716(5) 0.0521(4) 0.0503(17) Uani 1 1 d . . . C73 C 0.8941(6) 0.2504(5) 0.6695(4) 0.0538(17) Uani 1 1 d . . . H39 H 0.9211 0.1942 0.6881 0.065 Uiso 1 1 calc R . . C74 C 0.8206(6) 0.0327(5) 0.2733(5) 0.0526(17) Uani 1 1 d . . . H59 H 0.8279 -0.0003 0.3236 0.063 Uiso 1 1 calc R . . C75 C 0.1526(6) -0.0342(5) 0.1894(4) 0.0473(16) Uani 1 1 d . . . C76 C 0.2051(7) 0.4695(5) -0.3081(4) 0.0555(19) Uani 1 1 d . . . C77 C 0.0854(7) -0.0712(6) 0.4728(5) 0.066(2) Uani 1 1 d . . . H68 H 0.0431 -0.1295 0.4768 0.080 Uiso 1 1 calc R . . C78 C 0.0857(8) 0.4866(7) -0.0513(6) 0.082(3) Uani 1 1 d . . . H40 H 0.0472 0.5381 -0.0531 0.098 Uiso 1 1 calc R . . C79 C 0.1795(7) 0.2338(7) 0.1106(5) 0.073(2) Uani 1 1 d . . . C80 C 0.9353(11) 0.3216(9) 0.1877(7) 0.111(4) Uani 1 1 d . . . H73 H 0.9746 0.3806 0.2139 0.134 Uiso 1 1 calc R . . C98 C 0.2158(6) 0.2151(5) 0.6260(5) 0.0553(18) Uani 1 1 d . . . H41 H 0.2120 0.2474 0.6744 0.066 Uiso 1 1 calc R . . H9 H 0.638(6) 0.063(4) 0.371(4) 0.045(17) Uiso 1 1 d . . . H8 H 0.675(6) 0.125(4) 0.509(4) 0.045(18) Uiso 1 1 d . . . H6 H 0.585(6) 0.437(5) 0.650(4) 0.057(19) Uiso 1 1 d . . . H19 H 0.637(5) 0.186(4) 0.617(4) 0.043(17) Uiso 1 1 d . . . H20 H 0.439(6) 0.181(5) 0.601(4) 0.054(19) Uiso 1 1 d . . . H22 H 0.552(5) 0.503(4) -0.242(4) 0.047(17) Uiso 1 1 d . . . H18 H 0.491(7) -0.004(6) 0.230(5) 0.09(3) Uiso 1 1 d . . . H16 H 0.311(5) 0.359(4) 0.418(4) 0.040(16) Uiso 1 1 d . . . H15 H 0.383(6) 0.405(5) 0.559(5) 0.06(2) Uiso 1 1 d . . . H25 H 0.601(6) 0.076(5) 0.157(4) 0.053(19) Uiso 1 1 d . . . H23 H 0.686(5) 0.313(5) -0.243(4) 0.048(18) Uiso 1 1 d . . . H27 H 0.660(6) 0.467(5) -0.111(5) 0.06(2) Uiso 1 1 d . . . H26 H 0.417(5) 0.306(4) 0.093(4) 0.032(16) Uiso 1 1 d . . . H30 H 0.159(8) 0.482(6) -0.358(6) 0.09(3) Uiso 1 1 d . . . H32 H 0.354(5) 0.287(4) 0.291(4) 0.041(16) Uiso 1 1 d . . . H29 H 0.085(5) -0.063(4) 0.144(4) 0.036(15) Uiso 1 1 d . . . H35 H 0.881(5) 0.250(4) 0.346(4) 0.043(18) Uiso 1 1 d . . . H34 H 0.168(7) 0.201(6) 0.163(5) 0.08(3) Uiso 1 1 d . . . H42 H 0.930(6) 0.267(5) -0.022(5) 0.06(2) Uiso 1 1 d . . . H44 H 0.359(5) 0.522(4) -0.335(4) 0.043(17) Uiso 1 1 d . . . H46 H 0.941(6) 0.323(5) 0.491(4) 0.053(19) Uiso 1 1 d . . . H52 H 0.802(6) 0.554(5) 0.816(4) 0.05(2) Uiso 1 1 d . . . H50 H 0.047(6) 0.012(5) 0.256(4) 0.06(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0391(8) 0.0399(9) 0.0416(9) 0.0068(7) 0.0180(7) 0.0098(7) Si2 0.0400(8) 0.0400(9) 0.0412(9) 0.0035(7) 0.0185(7) 0.0092(7) Si3 0.0381(8) 0.0428(10) 0.0438(9) 0.0038(7) 0.0179(7) 0.0124(7) Si4 0.0367(8) 0.0409(9) 0.0455(9) 0.0020(7) 0.0183(7) 0.0090(7) C95 0.040(3) 0.029(3) 0.045(3) 0.004(2) 0.023(3) 0.011(2) C94 0.034(3) 0.031(3) 0.041(3) 0.000(2) 0.015(2) 0.013(2) C97 0.042(3) 0.030(3) 0.035(3) 0.006(2) 0.019(3) 0.008(2) C96 0.045(3) 0.028(3) 0.048(3) 0.002(2) 0.029(3) 0.009(2) C9 0.035(3) 0.036(3) 0.045(3) 0.008(3) 0.021(2) 0.012(2) N10 0.033(2) 0.043(3) 0.040(3) 0.001(2) 0.015(2) 0.010(2) C11 0.039(3) 0.028(3) 0.039(3) 0.007(2) 0.018(2) 0.009(2) C12 0.045(3) 0.032(3) 0.031(3) 0.010(2) 0.016(2) 0.015(2) C13 0.038(3) 0.028(3) 0.034(3) 0.003(2) 0.016(2) 0.010(2) C14 0.037(3) 0.038(3) 0.050(3) 0.007(3) 0.018(3) 0.015(2) C15 0.045(3) 0.030(3) 0.039(3) 0.007(2) 0.019(3) 0.011(2) C16 0.047(3) 0.027(3) 0.037(3) 0.011(2) 0.016(3) 0.014(2) C17 0.048(3) 0.032(3) 0.050(3) 0.006(3) 0.028(3) 0.009(2) C18 0.041(3) 0.028(3) 0.040(3) 0.004(2) 0.011(3) 0.013(2) C19 0.053(4) 0.041(4) 0.050(4) 0.011(3) 0.024(3) 0.018(3) N11 0.039(3) 0.045(3) 0.041(3) 0.005(2) 0.015(2) 0.014(2) C21 0.046(3) 0.038(3) 0.031(3) 0.001(2) 0.011(2) 0.019(3) C22 0.038(3) 0.042(3) 0.051(3) 0.016(3) 0.023(3) 0.016(3) C23 0.045(3) 0.030(3) 0.037(3) 0.002(2) 0.017(3) 0.011(2) C24 0.046(3) 0.032(3) 0.039(3) 0.006(2) 0.023(3) 0.016(2) C25 0.038(3) 0.030(3) 0.047(3) 0.011(2) 0.019(3) 0.012(2) C26 0.051(3) 0.034(3) 0.036(3) 0.005(2) 0.018(3) 0.012(3) C27 0.046(3) 0.048(4) 0.042(3) 0.005(3) 0.018(3) 0.006(3) C28 0.042(3) 0.054(4) 0.043(3) 0.010(3) 0.018(3) 0.016(3) C29 0.048(3) 0.031(3) 0.043(3) 0.005(2) 0.020(3) 0.014(3) C30 0.044(3) 0.046(4) 0.051(4) 0.001(3) 0.013(3) 0.016(3) N9 0.044(3) 0.037(3) 0.047(3) 0.005(2) 0.015(2) 0.011(2) C32 0.042(3) 0.039(3) 0.048(3) -0.004(3) 0.015(3) 0.011(3) N12 0.038(2) 0.038(3) 0.041(3) 0.008(2) 0.019(2) 0.008(2) C34 0.043(3) 0.034(3) 0.044(3) 0.008(3) 0.022(3) 0.015(2) C35 0.038(3) 0.051(4) 0.057(4) 0.008(3) 0.020(3) 0.015(3) C36 0.049(3) 0.050(4) 0.048(3) 0.006(3) 0.025(3) 0.010(3) C37 0.042(3) 0.057(4) 0.043(3) 0.005(3) 0.019(3) 0.012(3) C38 0.047(3) 0.025(3) 0.045(3) 0.003(2) 0.021(3) 0.011(2) C39 0.059(4) 0.042(4) 0.058(4) 0.010(3) 0.032(3) 0.017(3) C40 0.043(3) 0.033(3) 0.040(3) 0.004(2) 0.015(3) 0.013(2) C41 0.043(3) 0.034(3) 0.046(3) -0.001(3) 0.020(3) 0.009(3) C42 0.041(3) 0.052(4) 0.043(3) 0.008(3) 0.018(3) 0.014(3) C43 0.042(3) 0.028(3) 0.043(3) 0.004(3) 0.008(3) 0.007(2) C44 0.042(3) 0.043(4) 0.050(3) 0.008(3) 0.018(3) 0.015(3) C45 0.046(3) 0.041(3) 0.056(4) 0.002(3) 0.025(3) 0.008(3) C46 0.059(4) 0.039(3) 0.043(3) 0.013(3) 0.025(3) 0.015(3) C47 0.041(3) 0.031(3) 0.041(3) 0.001(2) 0.022(3) 0.008(2) C48 0.054(4) 0.036(3) 0.047(3) 0.012(3) 0.026(3) 0.017(3) C49 0.061(4) 0.036(3) 0.051(4) 0.001(3) 0.034(3) 0.003(3) C50 0.044(3) 0.047(4) 0.061(4) -0.008(3) 0.018(3) 0.010(3) C51 0.043(3) 0.041(4) 0.054(4) 0.002(3) 0.024(3) 0.009(3) C52 0.043(3) 0.046(4) 0.068(4) 0.004(3) 0.026(3) 0.015(3) C53 0.085(5) 0.035(4) 0.046(4) 0.007(3) 0.024(4) 0.020(3) C54 0.060(4) 0.028(3) 0.046(3) 0.002(3) 0.027(3) 0.008(3) C55 0.048(3) 0.035(3) 0.033(3) 0.006(2) 0.015(3) 0.012(3) C56 0.059(4) 0.033(3) 0.037(3) 0.006(3) 0.020(3) 0.015(3) C57 0.042(3) 0.038(3) 0.063(4) 0.008(3) 0.029(3) 0.016(3) C58 0.031(3) 0.035(3) 0.062(4) 0.017(3) 0.022(3) 0.014(2) C59 0.067(4) 0.045(4) 0.053(4) -0.006(3) 0.031(3) -0.004(3) C60 0.037(3) 0.039(4) 0.061(4) 0.007(3) 0.011(3) 0.009(3) C61 0.033(3) 0.034(3) 0.054(4) 0.000(3) 0.018(3) 0.013(2) C62 0.045(3) 0.040(4) 0.047(4) 0.013(3) 0.003(3) 0.011(3) C63 0.052(3) 0.027(3) 0.046(3) 0.007(3) 0.014(3) 0.016(3) C64 0.044(3) 0.043(4) 0.061(4) -0.002(3) 0.029(3) 0.006(3) C65 0.060(4) 0.034(3) 0.036(3) 0.008(3) 0.013(3) 0.013(3) C66 0.051(3) 0.043(4) 0.043(3) 0.010(3) 0.023(3) 0.021(3) C67 0.054(4) 0.054(4) 0.053(4) 0.004(3) 0.005(3) 0.019(3) C69 0.045(3) 0.039(3) 0.052(4) 0.008(3) 0.013(3) 0.008(3) C70 0.053(4) 0.057(4) 0.056(4) 0.002(4) 0.024(3) 0.010(3) C71 0.078(5) 0.037(3) 0.042(3) 0.009(3) 0.030(3) 0.020(3) C72 0.042(3) 0.057(4) 0.052(4) 0.004(3) 0.019(3) 0.002(3) C73 0.055(4) 0.050(4) 0.057(4) 0.011(3) 0.016(3) 0.019(3) C74 0.052(4) 0.054(4) 0.059(4) 0.011(3) 0.025(3) 0.016(3) C75 0.044(3) 0.047(4) 0.046(4) 0.000(3) 0.011(3) 0.004(3) C76 0.074(5) 0.046(4) 0.039(4) 0.012(3) 0.006(3) 0.020(4) C77 0.064(5) 0.070(5) 0.075(5) 0.008(4) 0.034(4) 0.013(4) C78 0.073(5) 0.072(6) 0.103(7) -0.005(5) 0.028(5) 0.024(5) C79 0.061(5) 0.094(6) 0.061(5) 0.016(5) 0.027(4) -0.013(4) C80 0.148(10) 0.108(9) 0.082(7) -0.018(6) 0.061(7) -0.018(8) C98 0.056(4) 0.061(4) 0.053(4) -0.010(3) 0.022(3) 0.015(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 C42 1.837(7) . ? Si1 C27 1.872(7) . ? Si1 C45 1.880(6) . ? Si1 C9 1.905(6) . ? Si2 C59 1.831(7) . ? Si2 C28 1.858(6) . ? Si2 C95 1.890(6) . ? Si2 C51 1.892(7) . ? Si3 C44 1.835(7) . ? Si3 C50 1.867(7) . ? Si3 C11 1.875(6) . ? Si3 C35 1.902(7) . ? Si4 C52 1.841(7) . ? Si4 C69 1.868(6) . ? Si4 C94 1.884(6) . ? Si4 C72 1.885(7) . ? C95 C41 1.382(8) . ? C95 C96 1.408(8) . ? C94 C97 1.375(8) . ? C94 C13 1.422(8) . ? C97 C18 1.402(8) . ? C96 C29 1.412(8) . ? C96 C38 1.447(8) . ? C9 C34 1.385(8) . ? C9 C16 1.407(8) . ? N10 C37 1.327(8) . ? N10 C38 1.353(7) . ? C11 C24 1.403(8) . ? C11 C12 1.415(8) . ? C12 C25 1.390(8) . ? C12 C15 1.451(8) . ? C13 C47 1.412(8) . ? C13 C23 1.435(8) . ? C14 C17 1.379(8) . ? C14 C29 1.421(8) . ? C15 N11 1.350(8) . ? C15 C55 1.414(8) . ? C16 C63 1.386(8) . ? C16 C26 1.454(8) . ? C17 C41 1.397(8) . ? C18 C61 1.363(9) . ? C19 N12 1.323(8) . ? C19 C39 1.405(9) . ? N11 C30 1.326(8) . ? C21 C32 1.347(9) . ? C21 C40 1.427(8) . ? C22 C48 1.351(9) . ? C22 C25 1.449(9) . ? C23 N9 1.353(8) . ? C23 C54 1.406(8) . ? C24 C43 1.389(8) . ? C25 C58 1.404(9) . ? C26 N12 1.347(7) . ? C26 C46 1.416(8) . ? C27 C70 1.210(10) . ? C29 C32 1.445(8) . ? C30 C75 1.423(9) . ? N9 C67 1.323(8) . ? C34 C57 1.404(8) . ? C35 C98 1.181(9) . ? C36 C66 1.367(9) . ? C36 C37 1.396(9) . ? C38 C40 1.416(8) . ? C39 C71 1.365(10) . ? C40 C66 1.415(9) . ? C42 C73 1.186(9) . ? C43 C58 1.384(9) . ? C44 C77 1.178(10) . ? C46 C71 1.411(9) . ? C46 C65 1.429(9) . ? C47 C61 1.401(8) . ? C47 C64 1.428(9) . ? C48 C55 1.434(9) . ? C49 C64 1.350(10) . ? C49 C54 1.438(9) . ? C51 C74 1.179(9) . ? C52 C78 1.173(11) . ? C53 C76 1.364(11) . ? C53 C54 1.410(9) . ? C55 C56 1.399(8) . ? C56 C75 1.376(9) . ? C57 C60 1.390(9) . ? C59 C80 1.166(13) . ? C60 C63 1.412(9) . ? C62 C65 1.324(10) . ? C62 C63 1.455(9) . ? C67 C76 1.381(11) . ? C72 C79 1.185(10) . ? 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 C42 Si1 C27 101.6(3) . . ? C42 Si1 C45 116.2(3) . . ? C27 Si1 C45 99.6(3) . . ? C42 Si1 C9 114.2(3) . . ? C27 Si1 C9 101.6(3) . . ? C45 Si1 C9 119.1(3) . . ? C59 Si2 C28 115.8(3) . . ? C59 Si2 C95 117.0(3) . . ? C28 Si2 C95 116.9(3) . . ? C59 Si2 C51 100.7(3) . . ? C28 Si2 C51 99.8(3) . . ? C95 Si2 C51 102.0(3) . . ? C44 Si3 C50 115.3(3) . . ? C44 Si3 C11 114.5(3) . . ? C50 Si3 C11 120.0(3) . . ? C44 Si3 C35 100.3(3) . . ? C50 Si3 C35 100.0(3) . . ? C11 Si3 C35 101.8(3) . . ? C52 Si4 C69 114.6(3) . . ? C52 Si4 C94 117.9(3) . . ? C69 Si4 C94 117.9(3) . . ? C52 Si4 C72 98.9(3) . . ? C69 Si4 C72 100.0(3) . . ? C94 Si4 C72 102.5(3) . . ? C41 C95 C96 116.3(5) . . ? C41 C95 Si2 122.1(5) . . ? C96 C95 Si2 121.5(4) . . ? C97 C94 C13 116.4(5) . . ? C97 C94 Si4 121.6(5) . . ? C13 C94 Si4 122.0(4) . . ? C94 C97 C18 122.2(6) . . ? C95 C96 C29 122.7(5) . . ? C95 C96 C38 119.1(5) . . ? C29 C96 C38 118.2(5) . . ? C34 C9 C16 117.4(5) . . ? C34 C9 Si1 121.0(4) . . ? C16 C9 Si1 121.6(4) . . ? C37 N10 C38 118.3(5) . . ? C24 C11 C12 115.7(5) . . ? C24 C11 Si3 122.0(4) . . ? C12 C11 Si3 122.3(4) . . ? C25 C12 C11 122.7(5) . . ? C25 C12 C15 119.7(5) . . ? C11 C12 C15 117.6(5) . . ? C47 C13 C94 122.1(5) . . ? C47 C13 C23 119.3(5) . . ? C94 C13 C23 118.6(5) . . ? C17 C14 C29 118.9(5) . . ? N11 C15 C55 123.0(5) . . ? N11 C15 C12 116.4(5) . . ? C55 C15 C12 120.6(5) . . ? C63 C16 C9 122.3(6) . . ? C63 C16 C26 120.0(5) . . ? C9 C16 C26 117.5(5) . . ? C14 C17 C41 120.9(6) . . ? C61 C18 C97 120.9(5) . . ? N12 C19 C39 122.6(6) . . ? C30 N11 C15 119.3(5) . . ? C32 C21 C40 121.6(5) . . ? C48 C22 C25 121.7(6) . . ? N9 C23 C54 122.7(5) . . ? N9 C23 C13 116.7(5) . . ? C54 C23 C13 120.6(5) . . ? C43 C24 C11 122.6(5) . . ? C12 C25 C58 119.3(5) . . ? C12 C25 C22 118.6(5) . . ? C58 C25 C22 122.2(5) . . ? N12 C26 C46 123.7(6) . . ? N12 C26 C16 116.7(5) . . ? C46 C26 C16 119.6(5) . . ? C70 C27 Si1 174.7(6) . . ? C96 C29 C14 118.5(5) . . ? C96 C29 C32 119.4(5) . . ? C14 C29 C32 122.1(5) . . ? N11 C30 C75 121.9(6) . . ? C67 N9 C23 118.3(6) . . ? C21 C32 C29 121.3(5) . . ? C19 N12 C26 118.5(5) . . ? C9 C34 C57 121.5(6) . . ? C98 C35 Si3 173.9(6) . . ? C66 C36 C37 119.4(6) . . ? N10 C37 C36 122.8(6) . . ? N10 C38 C40 123.2(5) . . ? N10 C38 C96 115.8(5) . . ? C40 C38 C96 121.0(5) . . ? C71 C39 C19 118.7(6) . . ? C66 C40 C38 116.4(5) . . ? C66 C40 C21 125.2(5) . . ? C38 C40 C21 118.4(5) . . ? C95 C41 C17 122.7(6) . . ? C73 C42 Si1 173.9(6) . . ? C58 C43 C24 120.2(6) . . ? C77 C44 Si3 177.3(7) . . ? C71 C46 C26 115.4(6) . . ? C71 C46 C65 126.2(6) . . ? C26 C46 C65 118.3(6) . . ? C61 C47 C13 118.4(5) . . ? C61 C47 C64 123.1(5) . . ? C13 C47 C64 118.5(5) . . ? C22 C48 C55 121.5(6) . . ? C64 C49 C54 120.3(6) . . ? C74 C51 Si2 177.4(6) . . ? C78 C52 Si4 177.8(7) . . ? C76 C53 C54 119.1(7) . . ? C23 C54 C53 117.1(6) . . ? C23 C54 C49 118.7(6) . . ? C53 C54 C49 124.1(6) . . ? C56 C55 C15 116.7(6) . . ? C56 C55 C48 125.4(6) . . ? C15 C55 C48 117.9(5) . . ? C75 C56 C55 120.8(6) . . ? C60 C57 C34 120.2(6) . . ? C43 C58 C25 119.6(5) . . ? C80 C59 Si2 174.9(8) . . ? C57 C60 C63 119.2(6) . . ? C18 C61 C47 120.0(5) . . ? C65 C62 C63 121.8(6) . . ? C16 C63 C60 119.2(6) . . ? C16 C63 C62 118.3(6) . . ? C60 C63 C62 122.4(6) . . ? C49 C64 C47 122.5(6) . . ? C62 C65 C46 121.9(6) . . ? C36 C66 C40 119.8(6) . . ? N9 C67 C76 122.9(7) . . ? C39 C71 C46 121.0(6) . . ? C79 C72 Si4 175.1(6) . . ? C56 C75 C30 118.4(6) . . ? C53 C76 C67 119.9(7) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.205 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.112 # Attachment '- 1F.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 888304' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H8 F3 N Si' _chemical_formula_weight 263.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_21/n _symmetry_space_group_name_Hall -p_2yn _space_group_IT_number 14:b2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.1120(13) _cell_length_b 14.615(3) _cell_length_c 9.2149(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.739(4) _cell_angle_gamma 90.00 _cell_volume 1082.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9115 _exptl_absorpt_correction_T_max 0.9768 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8029 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1894 _reflns_number_gt 1615 _reflns_threshold_expression >2\s(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'Yadokari-XG (Wakita, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG (Wakita, 2000)' _computing_publication_material 'Yadokari-XG (Wakita, 2000)' _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^)+(0.0485P)^2^+0.4403P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1894 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.14419(7) 0.21768(3) 0.45284(6) 0.02440(19) Uani 1 1 d . . . F1 F 0.01707(14) 0.23137(8) 0.30570(12) 0.0327(3) Uani 1 1 d . . . F2 F 0.31481(15) 0.27132(7) 0.44525(13) 0.0330(3) Uani 1 1 d . . . F3 F 0.06097(16) 0.29855(8) 0.54165(13) 0.0378(3) Uani 1 1 d . . . N1 N 0.24338(19) 0.11398(10) 0.34135(16) 0.0226(4) Uani 1 1 d . . . C1 C 0.2941(2) 0.11572(14) 0.2097(2) 0.0270(4) Uani 1 1 d . . . C2 C 0.3669(3) 0.03922(14) 0.1540(2) 0.0292(5) Uani 1 1 d . . . C3 C 0.3901(3) -0.03990(14) 0.2350(2) 0.0293(5) Uani 1 1 d . . . C4 C 0.3369(2) -0.04349(13) 0.3741(2) 0.0257(4) Uani 1 1 d . . . C5 C 0.3512(3) -0.12067(14) 0.4724(2) 0.0295(5) Uani 1 1 d . . . C6 C 0.2933(3) -0.11692(14) 0.6034(2) 0.0290(5) Uani 1 1 d . . . C7 C 0.2156(2) -0.03558(13) 0.6517(2) 0.0254(4) Uani 1 1 d . . . C8 C 0.1519(3) -0.02587(14) 0.7859(2) 0.0298(5) Uani 1 1 d . . . C9 C 0.0815(3) 0.05518(15) 0.8206(2) 0.0308(5) Uani 1 1 d . . . C10 C 0.0721(3) 0.13127(14) 0.7261(2) 0.0275(5) Uani 1 1 d . . . C11 C 0.1338(2) 0.12534(13) 0.5933(2) 0.0238(4) Uani 1 1 d . . . C12 C 0.2031(2) 0.04130(13) 0.5592(2) 0.0228(4) Uani 1 1 d . . . C13 C 0.2635(2) 0.03586(12) 0.4210(2) 0.0222(4) Uani 1 1 d . . . H8 H 0.027(3) 0.1862(15) 0.752(2) 0.027(5) Uiso 1 1 d . . . H4 H 0.400(3) -0.1719(15) 0.445(2) 0.028(5) Uiso 1 1 d . . . H7 H 0.039(3) 0.0645(15) 0.911(2) 0.036(6) Uiso 1 1 d . . . H1 H 0.274(2) 0.1712(14) 0.156(2) 0.020(5) Uiso 1 1 d . . . H2 H 0.401(3) 0.0456(15) 0.062(2) 0.039(6) Uiso 1 1 d . . . H6 H 0.159(3) -0.0731(15) 0.853(2) 0.035(6) Uiso 1 1 d . . . H3 H 0.441(3) -0.0898(16) 0.200(2) 0.032(6) Uiso 1 1 d . . . H5 H 0.308(3) -0.1668(16) 0.666(2) 0.038(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0275(3) 0.0180(3) 0.0290(3) 0.0016(2) 0.0090(2) 0.0016(2) F1 0.0321(7) 0.0287(7) 0.0370(7) 0.0065(5) 0.0042(5) 0.0052(5) F2 0.0344(7) 0.0247(6) 0.0418(7) -0.0019(5) 0.0117(5) -0.0047(5) F3 0.0482(8) 0.0252(6) 0.0436(7) 0.0008(5) 0.0197(6) 0.0076(5) N1 0.0209(9) 0.0217(8) 0.0255(8) 0.0004(6) 0.0041(6) 0.0004(6) C1 0.0264(11) 0.0275(11) 0.0275(10) 0.0024(8) 0.0053(8) -0.0015(9) C2 0.0275(11) 0.0328(11) 0.0284(11) -0.0064(9) 0.0080(8) -0.0030(9) C3 0.0245(11) 0.0256(11) 0.0382(12) -0.0112(9) 0.0062(9) -0.0012(9) C4 0.0198(10) 0.0212(10) 0.0351(11) -0.0044(8) 0.0003(8) -0.0018(8) C5 0.0235(11) 0.0190(10) 0.0448(13) -0.0037(9) -0.0003(9) 0.0013(9) C6 0.0256(11) 0.0219(11) 0.0378(12) 0.0058(8) -0.0025(9) -0.0013(8) C7 0.0192(10) 0.0254(10) 0.0300(10) 0.0029(8) -0.0019(8) -0.0032(8) C8 0.0269(11) 0.0315(11) 0.0300(11) 0.0087(9) -0.0003(8) -0.0052(9) C9 0.0293(11) 0.0373(12) 0.0264(11) 0.0019(9) 0.0057(8) -0.0052(10) C10 0.0258(11) 0.0270(11) 0.0305(11) -0.0025(8) 0.0068(8) -0.0010(9) C11 0.0206(10) 0.0228(10) 0.0284(10) -0.0011(7) 0.0045(8) -0.0026(8) C12 0.0175(10) 0.0221(10) 0.0279(10) 0.0003(7) -0.0002(7) -0.0024(8) C13 0.0179(10) 0.0204(9) 0.0277(10) 0.0000(7) 0.0006(7) -0.0021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 F2 1.6004(13) . ? Si1 F1 1.6016(13) . ? Si1 F3 1.6343(12) . ? Si1 C11 1.8799(19) . ? Si1 N1 2.0548(16) . ? N1 C1 1.333(2) . ? N1 C13 1.355(2) . ? C1 C2 1.394(3) . ? C2 C3 1.375(3) . ? C3 C4 1.408(3) . ? C4 C13 1.398(3) . ? C4 C5 1.441(3) . ? C5 C6 1.354(3) . ? C6 C7 1.443(3) . ? C7 C12 1.406(3) . ? C7 C8 1.411(3) . ? C8 C9 1.371(3) . ? C9 C10 1.409(3) . ? C10 C11 1.385(3) . ? C11 C12 1.404(3) . ? C12 C13 1.427(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 Si1 F1 111.33(7) . . ? F2 Si1 F3 94.91(7) . . ? F1 Si1 F3 94.09(7) . . ? F2 Si1 C11 120.07(8) . . ? F1 Si1 C11 126.10(8) . . ? F3 Si1 C11 96.56(7) . . ? F2 Si1 N1 86.58(6) . . ? F1 Si1 N1 85.40(6) . . ? F3 Si1 N1 178.52(7) . . ? C11 Si1 N1 82.64(7) . . ? C1 N1 C13 118.65(16) . . ? C1 N1 Si1 129.11(13) . . ? C13 N1 Si1 112.17(12) . . ? N1 C1 C2 121.17(18) . . ? C3 C2 C1 120.59(18) . . ? C2 C3 C4 119.26(18) . . ? C13 C4 C3 116.48(18) . . ? C13 C4 C5 117.17(18) . . ? C3 C4 C5 126.35(18) . . ? C6 C5 C4 121.36(19) . . ? C5 C6 C7 121.75(19) . . ? C12 C7 C8 116.48(18) . . ? C12 C7 C6 118.07(18) . . ? C8 C7 C6 125.45(18) . . ? C9 C8 C7 120.33(19) . . ? C8 C9 C10 121.82(19) . . ? C11 C10 C9 120.05(19) . . ? C10 C11 C12 117.12(17) . . ? C10 C11 Si1 128.19(15) . . ? C12 C11 Si1 114.65(13) . . ? C11 C12 C7 124.20(17) . . ? C11 C12 C13 116.41(16) . . ? C7 C12 C13 119.40(17) . . ? N1 C13 C4 123.84(17) . . ? N1 C13 C12 113.92(16) . . ? C4 C13 C12 122.24(17) . . ? 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 F2 Si1 N1 C1 -60.08(17) . . . . ? F1 Si1 N1 C1 51.66(17) . . . . ? F3 Si1 N1 C1 121(3) . . . . ? C11 Si1 N1 C1 178.99(18) . . . . ? F2 Si1 N1 C13 116.83(13) . . . . ? F1 Si1 N1 C13 -131.43(13) . . . . ? F3 Si1 N1 C13 -62(3) . . . . ? C11 Si1 N1 C13 -4.09(13) . . . . ? C13 N1 C1 C2 -0.1(3) . . . . ? Si1 N1 C1 C2 176.60(14) . . . . ? N1 C1 C2 C3 -0.9(3) . . . . ? C1 C2 C3 C4 1.1(3) . . . . ? C2 C3 C4 C13 -0.4(3) . . . . ? C2 C3 C4 C5 179.8(2) . . . . ? C13 C4 C5 C6 1.1(3) . . . . ? C3 C4 C5 C6 -179.0(2) . . . . ? C4 C5 C6 C7 -0.4(3) . . . . ? C5 C6 C7 C12 -0.8(3) . . . . ? C5 C6 C7 C8 179.88(19) . . . . ? C12 C7 C8 C9 0.2(3) . . . . ? C6 C7 C8 C9 179.5(2) . . . . ? C7 C8 C9 C10 -0.8(3) . . . . ? C8 C9 C10 C11 0.4(3) . . . . ? C9 C10 C11 C12 0.5(3) . . . . ? C9 C10 C11 Si1 -177.16(16) . . . . ? F2 Si1 C11 C10 99.79(19) . . . . ? F1 Si1 C11 C10 -99.72(19) . . . . ? F3 Si1 C11 C10 0.23(19) . . . . ? N1 Si1 C11 C10 -178.51(19) . . . . ? F2 Si1 C11 C12 -77.90(16) . . . . ? F1 Si1 C11 C12 82.59(16) . . . . ? F3 Si1 C11 C12 -177.46(14) . . . . ? N1 Si1 C11 C12 3.80(14) . . . . ? C10 C11 C12 C7 -1.1(3) . . . . ? Si1 C11 C12 C7 176.89(15) . . . . ? C10 C11 C12 C13 178.97(17) . . . . ? Si1 C11 C12 C13 -3.1(2) . . . . ? C8 C7 C12 C11 0.7(3) . . . . ? C6 C7 C12 C11 -178.64(17) . . . . ? C8 C7 C12 C13 -179.32(17) . . . . ? C6 C7 C12 C13 1.3(3) . . . . ? C1 N1 C13 C4 0.9(3) . . . . ? Si1 N1 C13 C4 -176.35(15) . . . . ? C1 N1 C13 C12 -179.27(17) . . . . ? Si1 N1 C13 C12 3.5(2) . . . . ? C3 C4 C13 N1 -0.7(3) . . . . ? C5 C4 C13 N1 179.22(17) . . . . ? C3 C4 C13 C12 179.55(17) . . . . ? C5 C4 C13 C12 -0.6(3) . . . . ? C11 C12 C13 N1 -0.5(2) . . . . ? C7 C12 C13 N1 179.55(17) . . . . ? C11 C12 C13 C4 179.32(17) . . . . ? C7 C12 C13 C4 -0.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.337 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.057 # Attachment '- 2C.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 888305' #TrackingRef '- 2C.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H21 N Si' _chemical_formula_weight 423.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1959(11) _cell_length_b 19.4826(15) _cell_length_c 35.670(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.882(3) _cell_angle_gamma 90.00 _cell_volume 9158.8(12) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9881 _exptl_absorpt_correction_T_max 0.9881 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61046 _diffrn_reflns_av_R_equivalents 0.1032 _diffrn_reflns_av_sigmaI/netI 0.1139 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15829 _reflns_number_gt 8260 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0781P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15829 _refine_ls_number_parameters 1467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1627 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.0859(2) 0.97486(14) 0.06959(7) 0.0280(7) Uani 1 1 d . . . C1 C 0.0026(3) 1.0123(2) 0.07220(9) 0.0329(9) Uani 1 1 d . . . H1 H -0.058(2) 0.9874(16) 0.0713(8) 0.023(9) Uiso 1 1 d . . . C2 C 0.0048(3) 1.0839(2) 0.07402(10) 0.0354(10) Uani 1 1 d . . . H2 H -0.056(2) 1.1059(16) 0.0760(8) 0.023(9) Uiso 1 1 d . . . C3 C 0.0951(3) 1.1177(2) 0.07375(9) 0.0352(10) Uani 1 1 d . . . H3 H 0.102(2) 1.1674(18) 0.0758(8) 0.031(9) Uiso 1 1 d . . . C4 C 0.1854(3) 1.08009(18) 0.07171(9) 0.0303(9) Uani 1 1 d . . . C5 C 0.2844(3) 1.1095(2) 0.07247(10) 0.0347(10) Uani 1 1 d . . . H4 H 0.290(3) 1.160(2) 0.0759(10) 0.054(12) Uiso 1 1 d . . . C6 C 0.3683(3) 1.0697(2) 0.07023(10) 0.0352(10) Uani 1 1 d . . . H5 H 0.439(2) 1.0889(16) 0.0713(8) 0.023(9) Uiso 1 1 d . . . C7 C 0.3613(3) 0.99616(18) 0.06718(9) 0.0301(9) Uani 1 1 d . . . C8 C 0.4462(3) 0.9538(2) 0.06457(10) 0.0383(10) Uani 1 1 d . . . H6 H 0.515(3) 0.9752(18) 0.0642(9) 0.043(11) Uiso 1 1 d . . . C9 C 0.4348(3) 0.8838(2) 0.06244(11) 0.0426(11) Uani 1 1 d . . . H7 H 0.493(3) 0.8545(17) 0.0618(8) 0.033(10) Uiso 1 1 d . . . C10 C 0.3378(3) 0.8537(2) 0.06262(10) 0.0335(9) Uani 1 1 d . . . H8 H 0.329(2) 0.8052(16) 0.0603(7) 0.014(8) Uiso 1 1 d . . . C11 C 0.2504(3) 0.89283(17) 0.06437(9) 0.0277(9) Uani 1 1 d . . . C12 C 0.2646(3) 0.96512(17) 0.06698(8) 0.0262(8) Uani 1 1 d . . . C13 C 0.1760(3) 1.00819(18) 0.06944(8) 0.0273(8) Uani 1 1 d . . . Si1 Si 0.11916(8) 0.85387(5) 0.06083(3) 0.0274(3) Uani 1 1 d . . . C14 C 0.0397(4) 0.8685(2) 0.01711(11) 0.0366(10) Uani 1 1 d . . . H9 H -0.022(4) 0.888(2) 0.0222(12) 0.085(17) Uiso 1 1 d . . . H10 H 0.069(4) 0.900(2) 0.0030(13) 0.085(17) Uiso 1 1 d . . . H11 H 0.023(3) 0.824(3) 0.0041(12) 0.089(16) Uiso 1 1 d . . . C15 C 0.1520(3) 0.76110(19) 0.05584(9) 0.0303(9) Uani 1 1 d . . . C16 C 0.1688(3) 0.70004(19) 0.05323(9) 0.0293(9) Uani 1 1 d . . . C17 C 0.1814(3) 0.62629(17) 0.05145(9) 0.0286(9) Uani 1 1 d . . . C18 C 0.1860(3) 0.5930(2) 0.01744(11) 0.0468(12) Uani 1 1 d . . . H12 H 0.186(3) 0.621(2) -0.0050(10) 0.058(12) Uiso 1 1 d . . . C19 C 0.1906(4) 0.5222(2) 0.01600(11) 0.0553(13) Uani 1 1 d . . . H13 H 0.192(3) 0.4970(19) -0.0080(10) 0.054(12) Uiso 1 1 d . . . C20 C 0.1902(3) 0.48358(19) 0.04855(10) 0.0359(10) Uani 1 1 d . . . H14 H 0.190(3) 0.4301(19) 0.0464(9) 0.043(10) Uiso 1 1 d . . . C21 C 0.1882(3) 0.51669(19) 0.08255(10) 0.0326(9) Uani 1 1 d . . . H15 H 0.184(3) 0.4899(18) 0.1051(10) 0.045(11) Uiso 1 1 d . . . C22 C 0.1844(3) 0.58771(18) 0.08418(9) 0.0295(9) Uani 1 1 d . . . H16 H 0.182(2) 0.6124(15) 0.1088(8) 0.019(8) Uiso 1 1 d . . . C23 C 0.0471(3) 0.84568(17) 0.10313(9) 0.0276(8) Uani 1 1 d . . . C24 C -0.0045(3) 0.83712(17) 0.13016(9) 0.0269(8) Uani 1 1 d . . . C25 C -0.0661(3) 0.82835(17) 0.16220(9) 0.0283(9) Uani 1 1 d . . . C26 C -0.0234(3) 0.83620(19) 0.19875(10) 0.0332(9) Uani 1 1 d . . . H17 H 0.044(2) 0.8486(16) 0.2016(8) 0.026(10) Uiso 1 1 d . . . C27 C -0.0821(3) 0.82826(19) 0.22933(10) 0.0384(10) Uani 1 1 d . . . H18 H -0.050(3) 0.8356(17) 0.2551(9) 0.041(10) Uiso 1 1 d . . . C28 C -0.1841(3) 0.81241(19) 0.22419(11) 0.0400(10) Uani 1 1 d . . . H19 H -0.226(3) 0.8063(19) 0.2458(10) 0.057(12) Uiso 1 1 d . . . C29 C -0.2279(3) 0.80413(19) 0.18815(11) 0.0358(10) Uani 1 1 d . . . H20 H -0.302(3) 0.7935(16) 0.1832(8) 0.032(10) Uiso 1 1 d . . . C30 C -0.1681(3) 0.81136(18) 0.15733(10) 0.0320(9) Uani 1 1 d . . . H21 H -0.199(3) 0.8029(19) 0.1332(10) 0.053(12) Uiso 1 1 d . . . N2 N -0.0362(2) 0.48608(15) 0.18106(7) 0.0288(7) Uani 1 1 d . . . C31 C 0.0480(3) 0.5229(2) 0.18092(9) 0.0320(9) Uani 1 1 d . . . H22 H 0.113(3) 0.4995(16) 0.1838(8) 0.028(10) Uiso 1 1 d . . . C32 C 0.0480(3) 0.5946(2) 0.17858(10) 0.0364(10) Uani 1 1 d . . . H23 H 0.111(3) 0.6209(19) 0.1795(9) 0.044(11) Uiso 1 1 d . . . C33 C -0.0432(3) 0.6286(2) 0.17566(10) 0.0373(10) Uani 1 1 d . . . H24 H -0.046(3) 0.677(2) 0.1749(9) 0.046(11) Uiso 1 1 d . . . C34 C -0.1349(3) 0.59118(17) 0.17479(9) 0.0306(9) Uani 1 1 d . . . C35 C -0.2341(3) 0.6203(2) 0.16989(10) 0.0359(10) Uani 1 1 d . . . H25 H -0.239(2) 0.6686(18) 0.1682(8) 0.032(10) Uiso 1 1 d . . . C36 C -0.3175(4) 0.5805(2) 0.16762(10) 0.0364(10) Uani 1 1 d . . . H26 H -0.385(3) 0.600(2) 0.1618(10) 0.054(12) Uiso 1 1 d . . . C37 C -0.3107(3) 0.50748(18) 0.17059(9) 0.0289(9) Uani 1 1 d . . . C38 C -0.3964(3) 0.4651(2) 0.16756(10) 0.0335(9) Uani 1 1 d . . . H27 H -0.462(3) 0.4842(17) 0.1628(9) 0.034(10) Uiso 1 1 d . . . C39 C -0.3873(3) 0.3950(2) 0.17161(9) 0.0321(9) Uani 1 1 d . . . H28 H -0.451(3) 0.3648(17) 0.1694(8) 0.033(10) Uiso 1 1 d . . . C40 C -0.2915(3) 0.36535(19) 0.17982(9) 0.0286(9) Uani 1 1 d . . . H29 H -0.287(2) 0.3152(16) 0.1833(7) 0.021(8) Uiso 1 1 d . . . C41 C -0.2030(3) 0.40427(17) 0.18262(8) 0.0253(8) Uani 1 1 d . . . C42 C -0.2148(3) 0.47667(17) 0.17731(8) 0.0260(8) Uani 1 1 d . . . C43 C -0.1258(3) 0.51924(18) 0.17798(9) 0.0279(9) Uani 1 1 d . . . Si2 Si -0.07449(8) 0.36764(5) 0.19565(3) 0.0280(3) Uani 1 1 d . . . C44 C -0.0117(4) 0.3942(2) 0.24121(11) 0.0396(10) Uani 1 1 d . . . H30 H 0.056(3) 0.403(2) 0.2374(11) 0.059(14) Uiso 1 1 d . . . H31 H -0.020(3) 0.359(2) 0.2609(12) 0.079(15) Uiso 1 1 d . . . H32 H -0.042(3) 0.437(2) 0.2508(11) 0.067(14) Uiso 1 1 d . . . C45 C -0.1082(3) 0.27690(18) 0.20665(9) 0.0302(9) Uani 1 1 d . . . C46 C -0.1284(3) 0.21829(19) 0.21543(9) 0.0303(9) Uani 1 1 d . . . C47 C -0.1502(3) 0.14742(18) 0.22405(9) 0.0304(9) Uani 1 1 d . . . C48 C -0.0718(3) 0.10335(19) 0.23645(10) 0.0344(10) Uani 1 1 d . . . H33 H -0.005(3) 0.1202(17) 0.2396(8) 0.031(10) Uiso 1 1 d . . . C49 C -0.0910(4) 0.0340(2) 0.24250(10) 0.0396(10) Uani 1 1 d . . . H34 H -0.024(3) 0.002(2) 0.2508(10) 0.061(12) Uiso 1 1 d . . . C50 C -0.1891(4) 0.0094(2) 0.23728(10) 0.0447(11) Uani 1 1 d . . . H35 H -0.206(3) -0.043(2) 0.2418(10) 0.067(13) Uiso 1 1 d . . . C51 C -0.2676(4) 0.0531(2) 0.22695(11) 0.0497(12) Uani 1 1 d . . . H36 H -0.339(3) 0.037(2) 0.2222(10) 0.061(13) Uiso 1 1 d . . . C52 C -0.2482(3) 0.1224(2) 0.21978(11) 0.0443(11) Uani 1 1 d . . . H37 H -0.312(3) 0.155(2) 0.2114(10) 0.055(12) Uiso 1 1 d . . . C53 C 0.0065(3) 0.35316(17) 0.15600(9) 0.0280(8) Uani 1 1 d . . . C54 C 0.0539(3) 0.34160(17) 0.12838(9) 0.0287(8) Uani 1 1 d . . . C55 C 0.1066(3) 0.32640(17) 0.09482(9) 0.0268(8) Uani 1 1 d . . . C56 C 0.0524(3) 0.32203(19) 0.06000(10) 0.0333(9) Uani 1 1 d . . . H38 H -0.014(2) 0.3308(16) 0.0588(8) 0.020(9) Uiso 1 1 d . . . C57 C 0.1005(3) 0.30531(19) 0.02775(10) 0.0348(10) Uani 1 1 d . . . H39 H 0.061(3) 0.3023(18) 0.0039(10) 0.042(11) Uiso 1 1 d . . . C58 C 0.2037(3) 0.29244(19) 0.02939(11) 0.0393(10) Uani 1 1 d . . . H40 H 0.236(3) 0.2793(19) 0.0066(10) 0.053(12) Uiso 1 1 d . . . C59 C 0.2589(3) 0.29774(19) 0.06353(11) 0.0346(10) Uani 1 1 d . . . H41 H 0.327(2) 0.2895(15) 0.0651(7) 0.013(8) Uiso 1 1 d . . . C60 C 0.2108(3) 0.31410(18) 0.09591(10) 0.0298(9) Uani 1 1 d . . . H42 H 0.247(2) 0.3155(17) 0.1187(9) 0.031(10) Uiso 1 1 d . . . N3 N 0.5562(2) 1.56990(15) 0.06708(8) 0.0313(7) Uani 1 1 d . . . C61 C 0.4675(3) 1.5380(2) 0.06378(11) 0.0425(11) Uani 1 1 d . . . H43 H 0.407(3) 1.5663(19) 0.0592(9) 0.043(11) Uiso 1 1 d . . . C62 C 0.4569(4) 1.4668(2) 0.06513(11) 0.0441(11) Uani 1 1 d . . . H44 H 0.389(3) 1.446(2) 0.0626(10) 0.057(13) Uiso 1 1 d . . . C63 C 0.5425(3) 1.4274(2) 0.07059(11) 0.0403(11) Uani 1 1 d . . . H45 H 0.536(3) 1.380(2) 0.0725(9) 0.042(11) Uiso 1 1 d . . . C64 C 0.6375(3) 1.45822(18) 0.07450(9) 0.0326(9) Uani 1 1 d . . . C65 C 0.7313(3) 1.4220(2) 0.08159(10) 0.0335(10) Uani 1 1 d . . . H46 H 0.729(2) 1.3741(18) 0.0840(9) 0.034(10) Uiso 1 1 d . . . C66 C 0.8201(3) 1.4557(2) 0.08507(9) 0.0341(10) Uani 1 1 d . . . H47 H 0.885(3) 1.4308(19) 0.0911(9) 0.043(11) Uiso 1 1 d . . . C67 C 0.8261(3) 1.52886(18) 0.08138(9) 0.0303(9) Uani 1 1 d . . . C68 C 0.9188(3) 1.5646(2) 0.08360(10) 0.0349(10) Uani 1 1 d . . . H48 H 0.978(3) 1.5380(18) 0.0866(9) 0.038(11) Uiso 1 1 d . . . C69 C 0.9217(3) 1.6344(2) 0.08009(10) 0.0356(10) Uani 1 1 d . . . H49 H 0.988(3) 1.6573(18) 0.0807(9) 0.040(11) Uiso 1 1 d . . . C70 C 0.8310(3) 1.6717(2) 0.07448(9) 0.0309(9) Uani 1 1 d . . . H50 H 0.835(2) 1.7211(17) 0.0726(8) 0.022(9) Uiso 1 1 d . . . C71 C 0.7367(3) 1.64001(17) 0.07180(8) 0.0263(8) Uani 1 1 d . . . C72 C 0.7358(3) 1.56740(17) 0.07515(9) 0.0265(8) Uani 1 1 d . . . C73 C 0.6409(3) 1.53063(17) 0.07203(9) 0.0274(9) Uani 1 1 d . . . Si3 Si 0.61757(8) 1.69132(5) 0.06424(3) 0.0281(3) Uani 1 1 d . . . C74 C 0.5462(3) 1.68679(19) 0.01789(9) 0.0380(10) Uani 1 1 d . . . H51 H 0.4766 1.6756 0.0216 0.057 Uiso 1 1 calc R . . H52 H 0.5756 1.6521 0.0027 0.057 Uiso 1 1 calc R . . H53 H 0.5497 1.7304 0.0055 0.057 Uiso 1 1 calc R . . C75 C 0.6696(3) 1.78042(19) 0.06412(9) 0.0311(9) Uani 1 1 d . . . C76 C 0.6945(3) 1.8403(2) 0.06434(9) 0.0316(9) Uani 1 1 d . . . C77 C 0.7150(3) 1.91370(17) 0.06539(9) 0.0296(9) Uani 1 1 d . . . C78 C 0.7297(3) 1.94751(19) 0.09975(10) 0.0334(9) Uani 1 1 d . . . H54 H 0.730(3) 1.9186(18) 0.1235(9) 0.043(10) Uiso 1 1 d . . . C79 C 0.7390(3) 2.0184(2) 0.10087(11) 0.0384(10) Uani 1 1 d . . . H55 H 0.749(3) 2.0423(19) 0.1264(10) 0.051(11) Uiso 1 1 d . . . C80 C 0.7325(3) 2.0559(2) 0.06786(11) 0.0358(10) Uani 1 1 d . . . H56 H 0.737(3) 2.1083(19) 0.0700(9) 0.045(11) Uiso 1 1 d . . . C81 C 0.7198(3) 2.0225(2) 0.03376(11) 0.0385(10) Uani 1 1 d . . . H57 H 0.716(2) 2.0473(17) 0.0097(9) 0.037(10) Uiso 1 1 d . . . C82 C 0.7115(3) 1.95182(19) 0.03229(11) 0.0359(10) Uani 1 1 d . . . H58 H 0.697(3) 1.9245(19) 0.0084(10) 0.048(11) Uiso 1 1 d . . . C83 C 0.5349(3) 1.69918(17) 0.10363(9) 0.0295(9) Uani 1 1 d . . . C84 C 0.4774(3) 1.70996(17) 0.12890(9) 0.0296(9) Uani 1 1 d . . . C85 C 0.4085(3) 1.72337(17) 0.15811(9) 0.0274(8) Uani 1 1 d . . . C86 C 0.3049(3) 1.73287(17) 0.14931(10) 0.0294(9) Uani 1 1 d . . . H59 H 0.276(2) 1.7291(16) 0.1233(9) 0.033(10) Uiso 1 1 d . . . C87 C 0.2387(3) 1.74707(18) 0.17713(11) 0.0331(9) Uani 1 1 d . . . H60 H 0.170(2) 1.7563(16) 0.1715(8) 0.024(9) Uiso 1 1 d . . . C88 C 0.2748(3) 1.75255(18) 0.21432(11) 0.0357(10) Uani 1 1 d . . . H61 H 0.230(3) 1.7644(17) 0.2329(9) 0.035(10) Uiso 1 1 d . . . C89 C 0.3765(3) 1.74301(19) 0.22341(10) 0.0363(10) Uani 1 1 d . . . H62 H 0.406(2) 1.7464(16) 0.2500(9) 0.028(9) Uiso 1 1 d . . . C90 C 0.4438(3) 1.72850(18) 0.19553(10) 0.0316(9) Uani 1 1 d . . . H63 H 0.517(2) 1.7189(15) 0.2025(8) 0.018(8) Uiso 1 1 d . . . N4 N 0.4288(2) 1.06902(15) 0.16684(7) 0.0308(7) Uani 1 1 d . . . C91 C 0.5108(3) 1.0302(2) 0.16380(10) 0.0369(10) Uani 1 1 d . . . H64 H 0.578(3) 1.0556(17) 0.1646(9) 0.034(10) Uiso 1 1 d . . . C92 C 0.5064(4) 0.9584(2) 0.16133(10) 0.0405(10) Uani 1 1 d . . . H65 H 0.573(3) 0.9326(19) 0.1592(9) 0.046(11) Uiso 1 1 d . . . C93 C 0.4138(3) 0.9266(2) 0.16138(10) 0.0390(10) Uani 1 1 d . . . H66 H 0.409(2) 0.8793(18) 0.1591(8) 0.027(9) Uiso 1 1 d . . . C94 C 0.3251(3) 0.96585(18) 0.16336(9) 0.0316(9) Uani 1 1 d . . . C95 C 0.2241(3) 0.9382(2) 0.16179(10) 0.0353(10) Uani 1 1 d . . . H67 H 0.219(3) 0.8864(19) 0.1589(9) 0.043(10) Uiso 1 1 d . . . C96 C 0.1423(3) 0.9803(2) 0.16226(9) 0.0346(10) Uani 1 1 d . . . H68 H 0.077(2) 0.9636(15) 0.1618(8) 0.016(9) Uiso 1 1 d . . . C97 C 0.1528(3) 1.05354(18) 0.16479(9) 0.0296(9) Uani 1 1 d . . . C98 C 0.0691(3) 1.0977(2) 0.16418(10) 0.0341(10) Uani 1 1 d . . . H69 H 0.004(2) 1.0789(15) 0.1612(8) 0.017(8) Uiso 1 1 d . . . C99 C 0.0820(3) 1.1676(2) 0.16658(10) 0.0330(9) Uani 1 1 d . . . H70 H 0.020(3) 1.1990(18) 0.1658(9) 0.038(10) Uiso 1 1 d . . . C100 C 0.1793(3) 1.1952(2) 0.17088(9) 0.0290(9) Uani 1 1 d . . . H71 H 0.188(3) 1.2427(19) 0.1725(9) 0.044(11) Uiso 1 1 d . . . C101 C 0.2666(3) 1.15457(17) 0.17143(8) 0.0275(8) Uani 1 1 d . . . C102 C 0.2510(3) 1.08246(17) 0.16754(8) 0.0277(9) Uani 1 1 d . . . C103 C 0.3375(3) 1.03753(18) 0.16619(8) 0.0289(9) Uani 1 1 d . . . Si4 Si 0.39694(8) 1.19058(5) 0.18258(3) 0.0281(3) Uani 1 1 d . . . C104 C 0.4532(3) 1.16499(18) 0.22931(9) 0.0365(9) Uani 1 1 d . . . H72 H 0.4999 1.1278 0.2263 0.055 Uiso 1 1 calc R . . H73 H 0.4002 1.1505 0.2450 0.055 Uiso 1 1 calc R . . H74 H 0.4885 1.2034 0.2407 0.055 Uiso 1 1 calc R . . C105 C 0.3666(3) 1.28295(19) 0.18991(9) 0.0293(9) Uani 1 1 d . . . C106 C 0.3473(3) 1.34328(19) 0.19416(9) 0.0292(9) Uani 1 1 d . . . C107 C 0.3300(3) 1.41632(18) 0.19835(9) 0.0279(8) Uani 1 1 d . . . C108 C 0.3054(3) 1.4445(2) 0.23262(11) 0.0389(10) Uani 1 1 d . . . H75 H 0.298(2) 1.4119(18) 0.2525(9) 0.039(10) Uiso 1 1 d . . . C109 C 0.2955(3) 1.5150(2) 0.23649(11) 0.0437(11) Uani 1 1 d . . . H76 H 0.279(3) 1.5356(19) 0.2612(10) 0.052(11) Uiso 1 1 d . . . C110 C 0.3105(3) 1.5579(2) 0.20616(12) 0.0412(11) Uani 1 1 d . . . H77 H 0.301(3) 1.606(2) 0.2106(10) 0.058(12) Uiso 1 1 d . . . C111 C 0.3319(3) 1.5300(2) 0.17182(12) 0.0370(10) Uani 1 1 d . . . H78 H 0.342(3) 1.5607(19) 0.1525(10) 0.047(12) Uiso 1 1 d . . . C112 C 0.3413(3) 1.46004(19) 0.16772(11) 0.0339(9) Uani 1 1 d . . . H79 H 0.354(2) 1.4395(17) 0.1438(9) 0.039(10) Uiso 1 1 d . . . C113 C 0.4900(3) 1.20151(17) 0.14648(9) 0.0301(9) Uani 1 1 d . . . C114 C 0.5580(3) 1.21104(17) 0.12501(9) 0.0302(9) Uani 1 1 d . . . C115 C 0.6383(3) 1.22169(17) 0.09992(9) 0.0277(9) Uani 1 1 d . . . C116 C 0.6175(3) 1.22840(18) 0.06148(10) 0.0309(9) Uani 1 1 d . . . H80 H 0.547(3) 1.2224(16) 0.0517(8) 0.025(9) Uiso 1 1 d . . . C117 C 0.6955(3) 1.23799(18) 0.03724(11) 0.0342(10) Uani 1 1 d . . . H81 H 0.676(3) 1.2408(18) 0.0106(10) 0.050(11) Uiso 1 1 d . . . C118 C 0.7952(3) 1.24108(18) 0.05114(10) 0.0327(9) Uani 1 1 d . . . H82 H 0.849(3) 1.2468(18) 0.0330(10) 0.049(11) Uiso 1 1 d . . . C119 C 0.8173(3) 1.23538(18) 0.08931(10) 0.0323(9) Uani 1 1 d . . . H83 H 0.884(3) 1.2356(17) 0.0985(9) 0.035(11) Uiso 1 1 d . . . C120 C 0.7398(3) 1.22559(18) 0.11373(10) 0.0304(9) Uani 1 1 d . . . H84 H 0.759(2) 1.2201(17) 0.1402(9) 0.035(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.032(2) 0.0259(18) 0.0257(15) 0.0013(13) 0.0025(14) 0.0029(15) C1 0.036(3) 0.031(2) 0.031(2) -0.0017(17) 0.0027(19) 0.004(2) C2 0.049(3) 0.029(2) 0.028(2) 0.0008(17) 0.004(2) 0.014(2) C3 0.059(3) 0.023(2) 0.0242(19) 0.0010(16) 0.0036(19) 0.001(2) C4 0.045(3) 0.021(2) 0.0249(19) 0.0026(15) 0.0028(18) 0.0018(18) C5 0.047(3) 0.024(2) 0.033(2) 0.0002(17) 0.0019(19) -0.004(2) C6 0.039(3) 0.033(2) 0.033(2) 0.0035(17) -0.0004(19) -0.012(2) C7 0.031(2) 0.032(2) 0.0268(19) 0.0015(16) 0.0016(16) -0.0028(18) C8 0.034(3) 0.038(3) 0.043(2) 0.0027(19) 0.004(2) 0.000(2) C9 0.033(3) 0.041(3) 0.054(3) 0.004(2) 0.006(2) 0.010(2) C10 0.036(3) 0.023(2) 0.042(2) 0.0022(18) 0.0051(18) 0.0038(19) C11 0.035(2) 0.026(2) 0.0226(17) 0.0043(15) 0.0072(16) 0.0004(17) C12 0.032(2) 0.027(2) 0.0193(17) 0.0028(15) 0.0003(16) 0.0011(17) C13 0.036(2) 0.026(2) 0.0200(17) 0.0017(15) -0.0007(16) 0.0026(17) Si1 0.0331(6) 0.0231(6) 0.0262(5) 0.0001(4) 0.0037(4) 0.0010(5) C14 0.044(3) 0.031(3) 0.034(2) 0.000(2) 0.003(2) 0.002(2) C15 0.040(3) 0.025(2) 0.0253(19) 0.0031(16) 0.0013(17) -0.0010(18) C16 0.033(2) 0.033(2) 0.0220(18) 0.0033(16) 0.0015(16) -0.0044(18) C17 0.033(2) 0.023(2) 0.0294(19) -0.0008(16) 0.0051(16) 0.0022(16) C18 0.080(4) 0.029(3) 0.031(2) 0.0026(19) 0.001(2) 0.008(2) C19 0.106(4) 0.028(3) 0.032(2) -0.0049(19) 0.000(2) 0.010(2) C20 0.046(3) 0.020(2) 0.041(2) 0.0011(18) -0.0007(19) -0.0002(18) C21 0.030(2) 0.030(2) 0.037(2) 0.0070(18) 0.0005(18) 0.0001(17) C22 0.035(2) 0.027(2) 0.0264(19) -0.0013(17) -0.0002(17) 0.0001(17) C23 0.030(2) 0.019(2) 0.034(2) -0.0017(16) -0.0026(17) -0.0007(16) C24 0.030(2) 0.021(2) 0.0289(19) 0.0023(15) -0.0014(17) -0.0029(16) C25 0.040(3) 0.018(2) 0.0277(19) 0.0016(15) 0.0083(17) 0.0013(17) C26 0.036(3) 0.029(2) 0.035(2) 0.0002(17) 0.006(2) 0.0011(19) C27 0.055(3) 0.033(2) 0.027(2) -0.0006(17) 0.004(2) -0.001(2) C28 0.056(3) 0.027(2) 0.039(2) -0.0007(18) 0.017(2) 0.001(2) C29 0.034(3) 0.028(2) 0.046(2) -0.0017(18) 0.011(2) -0.0033(19) C30 0.037(3) 0.024(2) 0.036(2) -0.0004(17) 0.0009(19) -0.0007(18) N2 0.032(2) 0.0266(18) 0.0285(16) -0.0026(13) 0.0062(14) -0.0002(15) C31 0.033(3) 0.034(2) 0.029(2) -0.0025(17) 0.0017(18) -0.002(2) C32 0.047(3) 0.033(3) 0.030(2) -0.0011(17) 0.0011(19) -0.007(2) C33 0.058(3) 0.024(2) 0.030(2) -0.0014(17) 0.0020(19) -0.005(2) C34 0.045(3) 0.021(2) 0.0263(19) -0.0017(15) 0.0027(17) 0.0012(18) C35 0.053(3) 0.021(2) 0.034(2) 0.0014(17) 0.0036(19) 0.011(2) C36 0.046(3) 0.031(2) 0.033(2) 0.0011(17) 0.002(2) 0.010(2) C37 0.031(2) 0.029(2) 0.0264(18) -0.0008(16) 0.0044(16) 0.0032(18) C38 0.028(3) 0.039(3) 0.034(2) 0.0040(18) 0.0017(18) 0.010(2) C39 0.028(2) 0.038(3) 0.031(2) 0.0002(17) 0.0020(17) -0.0013(19) C40 0.034(2) 0.025(2) 0.0275(19) 0.0003(16) 0.0068(17) -0.0008(18) C41 0.034(2) 0.023(2) 0.0198(17) -0.0016(14) 0.0043(16) 0.0008(17) C42 0.033(2) 0.025(2) 0.0202(17) 0.0010(15) 0.0088(16) 0.0012(17) C43 0.037(3) 0.024(2) 0.0226(18) 0.0003(15) 0.0053(16) 0.0014(18) Si2 0.0317(6) 0.0236(6) 0.0292(5) 0.0018(4) 0.0046(5) 0.0024(5) C44 0.046(3) 0.037(3) 0.036(2) 0.000(2) 0.004(2) 0.005(2) C45 0.035(2) 0.025(2) 0.0308(19) 0.0021(16) 0.0071(17) 0.0057(17) C46 0.031(2) 0.031(2) 0.0292(19) 0.0003(17) 0.0026(17) 0.0067(17) C47 0.035(2) 0.027(2) 0.0293(19) 0.0063(16) 0.0042(17) 0.0030(18) C48 0.041(3) 0.030(2) 0.033(2) 0.0027(17) 0.0069(19) -0.003(2) C49 0.052(3) 0.033(3) 0.035(2) 0.0048(18) 0.011(2) 0.007(2) C50 0.064(4) 0.034(3) 0.036(2) 0.0041(19) 0.001(2) -0.007(2) C51 0.049(3) 0.050(3) 0.049(3) 0.010(2) -0.008(2) -0.018(3) C52 0.044(3) 0.040(3) 0.049(2) 0.012(2) -0.003(2) -0.004(2) C53 0.031(2) 0.023(2) 0.0292(19) 0.0017(16) -0.0024(17) -0.0008(16) C54 0.031(2) 0.021(2) 0.034(2) -0.0010(16) -0.0026(17) 0.0017(16) C55 0.032(2) 0.020(2) 0.0286(19) -0.0016(15) 0.0057(17) -0.0008(16) C56 0.032(3) 0.028(2) 0.040(2) -0.0002(17) 0.005(2) -0.0050(19) C57 0.044(3) 0.030(2) 0.030(2) -0.0007(17) 0.003(2) -0.0052(19) C58 0.053(3) 0.028(2) 0.038(2) -0.0018(18) 0.014(2) -0.002(2) C59 0.031(3) 0.029(2) 0.045(2) 0.0050(18) 0.012(2) 0.0041(18) C60 0.034(3) 0.026(2) 0.029(2) 0.0046(17) 0.0069(19) 0.0017(17) N3 0.028(2) 0.0282(18) 0.0384(17) -0.0031(14) 0.0059(14) 0.0002(15) C61 0.033(3) 0.038(3) 0.056(3) -0.007(2) 0.005(2) 0.004(2) C62 0.038(3) 0.036(3) 0.059(3) -0.010(2) 0.008(2) -0.006(2) C63 0.050(3) 0.023(2) 0.049(2) -0.0021(19) 0.008(2) -0.006(2) C64 0.041(3) 0.026(2) 0.031(2) -0.0045(16) 0.0070(18) 0.0000(19) C65 0.045(3) 0.021(2) 0.035(2) 0.0028(17) 0.0078(19) 0.006(2) C66 0.041(3) 0.033(2) 0.029(2) -0.0024(17) 0.0049(19) 0.013(2) C67 0.034(2) 0.029(2) 0.0280(19) -0.0027(16) 0.0033(17) 0.0073(18) C68 0.029(3) 0.044(3) 0.033(2) -0.0008(18) 0.0057(18) 0.011(2) C69 0.033(3) 0.036(3) 0.039(2) -0.0010(18) 0.0078(19) -0.001(2) C70 0.033(3) 0.027(2) 0.033(2) 0.0000(17) 0.0039(17) 0.0052(19) C71 0.030(2) 0.027(2) 0.0227(18) -0.0019(15) 0.0045(16) -0.0004(17) C72 0.035(2) 0.021(2) 0.0234(18) -0.0018(15) 0.0077(16) 0.0034(17) C73 0.034(2) 0.024(2) 0.0248(18) 0.0000(15) 0.0076(16) 0.0020(17) Si3 0.0288(6) 0.0246(6) 0.0310(5) 0.0010(4) 0.0028(4) 0.0034(5) C74 0.038(3) 0.040(2) 0.036(2) 0.0032(18) -0.0001(18) -0.0003(19) C75 0.036(2) 0.025(2) 0.031(2) 0.0040(16) 0.0010(17) 0.0054(18) C76 0.029(2) 0.035(3) 0.030(2) 0.0023(17) 0.0016(16) 0.0079(18) C77 0.031(2) 0.020(2) 0.039(2) 0.0019(16) 0.0064(17) 0.0028(16) C78 0.034(2) 0.031(2) 0.036(2) 0.0017(18) 0.0062(18) 0.0028(18) C79 0.043(3) 0.032(2) 0.041(2) -0.0048(19) 0.0043(19) 0.0027(19) C80 0.037(3) 0.023(2) 0.049(2) -0.0015(19) 0.0088(19) 0.0016(18) C81 0.043(3) 0.032(3) 0.041(2) 0.0085(19) 0.006(2) 0.0001(19) C82 0.043(3) 0.027(2) 0.038(2) 0.0015(18) 0.0045(19) -0.0013(18) C83 0.035(2) 0.017(2) 0.036(2) 0.0019(16) -0.0009(18) 0.0029(16) C84 0.034(2) 0.021(2) 0.034(2) 0.0003(16) 0.0024(18) 0.0044(16) C85 0.033(2) 0.018(2) 0.031(2) -0.0019(15) 0.0026(17) -0.0011(16) C86 0.034(3) 0.021(2) 0.033(2) -0.0013(16) 0.0037(19) 0.0007(17) C87 0.030(3) 0.025(2) 0.046(2) 0.0001(17) 0.008(2) 0.0045(18) C88 0.044(3) 0.028(2) 0.037(2) -0.0048(17) 0.018(2) -0.0038(19) C89 0.044(3) 0.032(2) 0.032(2) -0.0035(18) -0.001(2) -0.0082(19) C90 0.029(3) 0.031(2) 0.035(2) 0.0031(17) 0.0003(18) 0.0025(18) N4 0.031(2) 0.0333(19) 0.0284(16) 0.0004(13) 0.0018(14) -0.0016(15) C91 0.038(3) 0.037(3) 0.036(2) 0.0007(18) -0.0010(19) -0.001(2) C92 0.048(3) 0.037(3) 0.036(2) 0.0007(18) 0.003(2) 0.009(2) C93 0.060(3) 0.024(2) 0.033(2) 0.0022(18) 0.002(2) 0.004(2) C94 0.046(3) 0.025(2) 0.0241(19) 0.0031(16) 0.0028(18) 0.0004(19) C95 0.049(3) 0.027(2) 0.030(2) -0.0007(17) 0.0044(19) -0.009(2) C96 0.043(3) 0.033(2) 0.028(2) -0.0004(17) 0.0070(19) -0.013(2) C97 0.039(3) 0.027(2) 0.0237(18) 0.0013(15) 0.0080(17) -0.0070(18) C98 0.026(3) 0.044(3) 0.033(2) -0.0019(18) 0.0050(18) -0.009(2) C99 0.031(3) 0.034(3) 0.034(2) -0.0045(17) 0.0067(18) 0.0013(19) C100 0.031(2) 0.027(2) 0.0295(19) 0.0016(17) 0.0041(17) -0.0002(19) C101 0.035(2) 0.025(2) 0.0227(18) 0.0016(15) 0.0043(16) -0.0019(17) C102 0.044(3) 0.024(2) 0.0160(16) 0.0002(15) 0.0072(16) -0.0011(18) C103 0.046(3) 0.025(2) 0.0159(17) 0.0022(15) 0.0032(16) 0.0034(18) Si4 0.0323(6) 0.0236(6) 0.0287(5) -0.0002(4) 0.0042(4) -0.0005(5) C104 0.042(3) 0.031(2) 0.037(2) -0.0035(17) 0.0036(18) 0.0016(18) C105 0.031(2) 0.028(2) 0.0297(19) 0.0038(16) 0.0063(17) -0.0013(17) C106 0.026(2) 0.034(2) 0.0278(19) 0.0010(17) -0.0003(16) -0.0049(17) C107 0.030(2) 0.023(2) 0.0301(19) -0.0007(16) -0.0037(16) 0.0009(16) C108 0.048(3) 0.034(3) 0.034(2) 0.0014(19) -0.0049(19) 0.005(2) C109 0.054(3) 0.038(3) 0.038(2) -0.011(2) -0.010(2) 0.009(2) C110 0.034(3) 0.026(2) 0.061(3) -0.010(2) -0.013(2) 0.0022(19) C111 0.033(3) 0.025(2) 0.053(3) 0.004(2) -0.004(2) -0.0009(18) C112 0.032(2) 0.031(2) 0.039(2) 0.0011(18) 0.0017(18) 0.0035(18) C113 0.040(3) 0.019(2) 0.0307(19) -0.0026(15) -0.0031(18) -0.0015(17) C114 0.036(2) 0.020(2) 0.034(2) 0.0001(16) 0.0041(18) -0.0009(16) C115 0.030(2) 0.022(2) 0.031(2) -0.0014(15) 0.0066(17) 0.0022(16) C116 0.028(3) 0.032(2) 0.032(2) 0.0034(17) 0.0010(18) 0.0018(18) C117 0.046(3) 0.028(2) 0.029(2) 0.0029(17) 0.005(2) 0.0019(19) C118 0.038(3) 0.025(2) 0.036(2) -0.0019(17) 0.009(2) 0.0018(18) C119 0.030(3) 0.024(2) 0.043(2) -0.0016(17) 0.006(2) -0.0022(18) C120 0.038(3) 0.022(2) 0.031(2) -0.0015(16) 0.0057(19) -0.0005(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.326(4) . ? N1 C13 1.355(4) . ? C1 C2 1.395(5) . ? C2 C3 1.362(5) . ? C3 C4 1.403(5) . ? C4 C13 1.408(5) . ? C4 C5 1.426(5) . ? C5 C6 1.358(5) . ? C6 C7 1.440(5) . ? C7 C8 1.398(5) . ? C7 C12 1.412(5) . ? C8 C9 1.373(5) . ? C9 C10 1.408(5) . ? C10 C11 1.385(5) . ? C11 C12 1.423(5) . ? C11 Si1 1.890(4) . ? C12 C13 1.446(5) . ? Si1 C23 1.831(3) . ? Si1 C14 1.857(4) . ? Si1 C15 1.869(4) . ? C15 C16 1.215(5) . ? C16 C17 1.448(5) . ? C17 C18 1.380(5) . ? C17 C22 1.388(4) . ? C18 C19 1.381(6) . ? C19 C20 1.384(5) . ? C20 C21 1.375(5) . ? C21 C22 1.386(5) . ? C23 C24 1.219(4) . ? C24 C25 1.446(4) . ? C25 C30 1.389(5) . ? C25 C26 1.403(5) . ? C26 C27 1.378(5) . ? C27 C28 1.384(5) . ? C28 C29 1.392(5) . ? C29 C30 1.392(5) . ? N2 C31 1.323(4) . ? N2 C43 1.347(4) . ? C31 C32 1.399(5) . ? C32 C33 1.372(5) . ? C33 C34 1.411(5) . ? C34 C43 1.411(5) . ? C34 C35 1.429(5) . ? C35 C36 1.345(5) . ? C36 C37 1.429(5) . ? C37 C38 1.401(5) . ? C37 C42 1.411(5) . ? C38 C39 1.378(5) . ? C39 C40 1.407(5) . ? C40 C41 1.392(5) . ? C41 C42 1.431(5) . ? C41 Si2 1.877(4) . ? C42 C43 1.437(5) . ? Si2 C53 1.837(3) . ? Si2 C44 1.860(4) . ? Si2 C45 1.869(4) . ? C45 C46 1.217(5) . ? C46 C47 1.447(5) . ? C47 C52 1.383(5) . ? C47 C48 1.399(5) . ? C48 C49 1.393(5) . ? C49 C50 1.385(6) . ? C50 C51 1.377(6) . ? C51 C52 1.400(6) . ? C53 C54 1.214(4) . ? C54 C55 1.445(4) . ? C55 C60 1.395(5) . ? C55 C56 1.404(5) . ? C56 C57 1.381(5) . ? C57 C58 1.383(5) . ? C58 C59 1.391(5) . ? C59 C60 1.382(5) . ? N3 C61 1.324(5) . ? N3 C73 1.359(4) . ? C61 C62 1.395(6) . ? C62 C63 1.372(6) . ? C63 C64 1.391(5) . ? C64 C73 1.414(5) . ? C64 C65 1.435(5) . ? C65 C66 1.343(5) . ? C66 C67 1.434(5) . ? C67 C68 1.407(5) . ? C67 C72 1.416(5) . ? C68 C69 1.366(5) . ? C69 C70 1.407(5) . ? C70 C71 1.388(5) . ? C71 C72 1.420(5) . ? C71 Si3 1.871(4) . ? C72 C73 1.442(5) . ? Si3 C83 1.828(3) . ? Si3 C74 1.863(3) . ? Si3 C75 1.867(4) . ? C75 C76 1.211(5) . ? C76 C77 1.456(5) . ? C77 C82 1.394(5) . ? C77 C78 1.396(5) . ? C78 C79 1.387(5) . ? C79 C80 1.385(5) . ? C80 C81 1.382(5) . ? C81 C82 1.383(5) . ? C83 C84 1.226(4) . ? C84 C85 1.440(4) . ? C85 C90 1.395(5) . ? C85 C86 1.400(5) . ? C86 C87 1.383(5) . ? C87 C88 1.391(5) . ? C88 C89 1.378(5) . ? C89 C90 1.395(5) . ? N4 C91 1.329(5) . ? N4 C103 1.351(4) . ? C91 C92 1.403(5) . ? C92 C93 1.369(6) . ? C93 C94 1.402(5) . ? C94 C103 1.409(5) . ? C94 C95 1.436(5) . ? C95 C96 1.356(5) . ? C96 C97 1.437(5) . ? C97 C98 1.399(5) . ? C97 C102 1.413(5) . ? C98 C99 1.376(5) . ? C99 C100 1.394(5) . ? C100 C101 1.396(5) . ? C101 C102 1.426(5) . ? C101 Si4 1.882(4) . ? C102 C103 1.441(5) . ? Si4 C113 1.836(4) . ? Si4 C104 1.858(3) . ? Si4 C105 1.865(4) . ? C105 C106 1.214(5) . ? C106 C107 1.450(5) . ? C107 C108 1.394(5) . ? C107 C112 1.399(5) . ? C108 C109 1.387(5) . ? C109 C110 1.389(6) . ? C110 C111 1.382(5) . ? C111 C112 1.378(5) . ? C113 C114 1.222(4) . ? C114 C115 1.437(4) . ? C115 C116 1.391(5) . ? C115 C120 1.406(5) . ? C116 C117 1.390(5) . ? C117 C118 1.383(5) . ? C118 C119 1.382(5) . ? C119 C120 1.389(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 C1 N1 C13 117.8(3) . . ? N1 C1 C2 122.5(4) . . ? C3 C2 C1 119.9(4) . . ? C2 C3 C4 119.6(4) . . ? C3 C4 C13 116.7(4) . . ? C3 C4 C5 124.6(4) . . ? C13 C4 C5 118.6(3) . . ? C6 C5 C4 121.2(4) . . ? C5 C6 C7 121.6(4) . . ? C8 C7 C12 118.3(3) . . ? C8 C7 C6 122.9(4) . . ? C12 C7 C6 118.8(3) . . ? C9 C8 C7 120.2(4) . . ? C8 C9 C10 120.7(4) . . ? C11 C10 C9 122.0(4) . . ? C10 C11 C12 116.1(3) . . ? C10 C11 Si1 122.6(3) . . ? C12 C11 Si1 121.3(3) . . ? C7 C12 C11 122.7(3) . . ? C7 C12 C13 119.0(3) . . ? C11 C12 C13 118.3(3) . . ? N1 C13 C4 123.5(3) . . ? N1 C13 C12 115.8(3) . . ? C4 C13 C12 120.8(3) . . ? C23 Si1 C14 114.24(19) . . ? C23 Si1 C15 97.28(15) . . ? C14 Si1 C15 101.06(18) . . ? C23 Si1 C11 119.50(15) . . ? C14 Si1 C11 118.15(18) . . ? C15 Si1 C11 100.30(16) . . ? C16 C15 Si1 176.9(3) . . ? C15 C16 C17 175.5(4) . . ? C18 C17 C22 119.0(3) . . ? C18 C17 C16 121.0(3) . . ? C22 C17 C16 119.9(3) . . ? C17 C18 C19 120.4(4) . . ? C18 C19 C20 120.6(4) . . ? C21 C20 C19 119.1(4) . . ? C20 C21 C22 120.5(3) . . ? C21 C22 C17 120.3(3) . . ? C24 C23 Si1 176.0(3) . . ? C23 C24 C25 178.9(4) . . ? C30 C25 C26 118.9(3) . . ? C30 C25 C24 120.6(3) . . ? C26 C25 C24 120.4(3) . . ? C27 C26 C25 120.5(4) . . ? C26 C27 C28 120.1(4) . . ? C27 C28 C29 120.3(4) . . ? C30 C29 C28 119.5(4) . . ? C25 C30 C29 120.6(4) . . ? C31 N2 C43 118.3(3) . . ? N2 C31 C32 122.9(4) . . ? C33 C32 C31 118.9(4) . . ? C32 C33 C34 120.0(4) . . ? C43 C34 C33 116.2(4) . . ? C43 C34 C35 118.5(4) . . ? C33 C34 C35 125.2(4) . . ? C36 C35 C34 121.4(4) . . ? C35 C36 C37 121.4(4) . . ? C38 C37 C42 118.4(3) . . ? C38 C37 C36 122.3(4) . . ? C42 C37 C36 119.3(4) . . ? C39 C38 C37 120.7(4) . . ? C38 C39 C40 120.1(4) . . ? C41 C40 C39 122.2(4) . . ? C40 C41 C42 116.3(3) . . ? C40 C41 Si2 123.7(3) . . ? C42 C41 Si2 119.9(3) . . ? C37 C42 C41 122.2(3) . . ? C37 C42 C43 118.9(3) . . ? C41 C42 C43 118.9(3) . . ? N2 C43 C34 123.6(3) . . ? N2 C43 C42 116.0(3) . . ? C34 C43 C42 120.4(3) . . ? C53 Si2 C44 117.67(19) . . ? C53 Si2 C45 99.80(15) . . ? C44 Si2 C45 100.38(18) . . ? C53 Si2 C41 114.91(15) . . ? C44 Si2 C41 117.91(18) . . ? C45 Si2 C41 100.95(16) . . ? C46 C45 Si2 177.1(3) . . ? C45 C46 C47 177.0(3) . . ? C52 C47 C48 119.4(4) . . ? C52 C47 C46 120.5(3) . . ? C48 C47 C46 120.1(3) . . ? C49 C48 C47 120.5(4) . . ? C50 C49 C48 119.4(4) . . ? C51 C50 C49 120.4(4) . . ? C50 C51 C52 120.3(4) . . ? C47 C52 C51 119.8(4) . . ? C54 C53 Si2 175.2(3) . . ? C53 C54 C55 177.6(4) . . ? C60 C55 C56 118.2(3) . . ? C60 C55 C54 121.8(3) . . ? C56 C55 C54 120.0(3) . . ? C57 C56 C55 121.1(4) . . ? C56 C57 C58 120.1(4) . . ? C57 C58 C59 119.6(4) . . ? C60 C59 C58 120.4(4) . . ? C59 C60 C55 120.6(4) . . ? C61 N3 C73 117.7(3) . . ? N3 C61 C62 123.6(4) . . ? C63 C62 C61 118.6(4) . . ? C62 C63 C64 120.2(4) . . ? C63 C64 C73 117.1(4) . . ? C63 C64 C65 124.7(4) . . ? C73 C64 C65 118.1(4) . . ? C66 C65 C64 121.1(4) . . ? C65 C66 C67 122.0(4) . . ? C68 C67 C72 118.0(3) . . ? C68 C67 C66 122.6(3) . . ? C72 C67 C66 119.4(3) . . ? C69 C68 C67 121.0(4) . . ? C68 C69 C70 120.0(4) . . ? C71 C70 C69 122.2(4) . . ? C70 C71 C72 116.7(3) . . ? C70 C71 Si3 121.1(3) . . ? C72 C71 Si3 122.3(3) . . ? C67 C72 C71 122.1(3) . . ? C67 C72 C73 118.0(3) . . ? C71 C72 C73 120.0(3) . . ? N3 C73 C64 122.8(3) . . ? N3 C73 C72 115.9(3) . . ? C64 C73 C72 121.4(3) . . ? C83 Si3 C74 113.05(17) . . ? C83 Si3 C75 99.05(15) . . ? C74 Si3 C75 102.20(16) . . ? C83 Si3 C71 117.61(15) . . ? C74 Si3 C71 119.09(16) . . ? C75 Si3 C71 101.00(16) . . ? C76 C75 Si3 174.2(3) . . ? C75 C76 C77 174.7(4) . . ? C82 C77 C78 119.3(3) . . ? C82 C77 C76 120.2(3) . . ? C78 C77 C76 120.2(3) . . ? C79 C78 C77 120.2(4) . . ? C80 C79 C78 120.0(4) . . ? C81 C80 C79 120.0(4) . . ? C80 C81 C82 120.5(4) . . ? C81 C82 C77 120.0(4) . . ? C84 C83 Si3 174.5(3) . . ? C83 C84 C85 178.9(4) . . ? C90 C85 C86 118.7(3) . . ? C90 C85 C84 120.8(3) . . ? C86 C85 C84 120.4(3) . . ? C87 C86 C85 120.7(4) . . ? C86 C87 C88 120.1(4) . . ? C89 C88 C87 119.8(4) . . ? C88 C89 C90 120.5(4) . . ? C85 C90 C89 120.2(4) . . ? C91 N4 C103 118.0(3) . . ? N4 C91 C92 122.8(4) . . ? C93 C92 C91 119.0(4) . . ? C92 C93 C94 120.1(4) . . ? C93 C94 C103 116.7(4) . . ? C93 C94 C95 124.6(4) . . ? C103 C94 C95 118.6(3) . . ? C96 C95 C94 120.6(4) . . ? C95 C96 C97 121.9(4) . . ? C98 C97 C102 118.5(3) . . ? C98 C97 C96 122.5(4) . . ? C102 C97 C96 119.0(3) . . ? C99 C98 C97 120.9(4) . . ? C98 C99 C100 119.9(4) . . ? C99 C100 C101 122.5(4) . . ? C100 C101 C102 116.3(3) . . ? C100 C101 Si4 122.4(3) . . ? C102 C101 Si4 120.9(3) . . ? C97 C102 C101 121.8(3) . . ? C97 C102 C103 118.7(3) . . ? C101 C102 C103 119.5(3) . . ? N4 C103 C94 123.4(3) . . ? N4 C103 C102 115.5(3) . . ? C94 C103 C102 121.0(3) . . ? C113 Si4 C104 114.15(16) . . ? C113 Si4 C105 98.20(15) . . ? C104 Si4 C105 102.24(16) . . ? C113 Si4 C101 122.12(15) . . ? C104 Si4 C101 114.15(16) . . ? C105 Si4 C101 100.87(16) . . ? C106 C105 Si4 179.0(3) . . ? C105 C106 C107 176.6(4) . . ? C108 C107 C112 118.9(3) . . ? C108 C107 C106 121.5(3) . . ? C112 C107 C106 119.6(3) . . ? C109 C108 C107 120.3(4) . . ? C108 C109 C110 120.0(4) . . ? C111 C110 C109 119.8(4) . . ? C112 C111 C110 120.4(4) . . ? C111 C112 C107 120.4(4) . . ? C114 C113 Si4 174.1(3) . . ? C113 C114 C115 179.5(4) . . ? C116 C115 C120 118.6(3) . . ? C116 C115 C114 120.8(3) . . ? C120 C115 C114 120.6(3) . . ? C117 C116 C115 120.6(4) . . ? C118 C117 C116 120.2(4) . . ? C119 C118 C117 120.0(4) . . ? C118 C119 C120 120.2(4) . . ? C119 C120 C115 120.4(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 C13 N1 C1 C2 1.3(5) . . . . ? N1 C1 C2 C3 -1.1(5) . . . . ? C1 C2 C3 C4 -0.1(5) . . . . ? C2 C3 C4 C13 1.0(5) . . . . ? C2 C3 C4 C5 -177.9(3) . . . . ? C3 C4 C5 C6 -179.8(3) . . . . ? C13 C4 C5 C6 1.4(5) . . . . ? C4 C5 C6 C7 -0.3(5) . . . . ? C5 C6 C7 C8 179.6(3) . . . . ? C5 C6 C7 C12 -0.8(5) . . . . ? C12 C7 C8 C9 -0.9(5) . . . . ? C6 C7 C8 C9 178.8(3) . . . . ? C7 C8 C9 C10 0.4(6) . . . . ? C8 C9 C10 C11 1.0(6) . . . . ? C9 C10 C11 C12 -1.6(5) . . . . ? C9 C10 C11 Si1 175.1(3) . . . . ? C8 C7 C12 C11 0.2(5) . . . . ? C6 C7 C12 C11 -179.5(3) . . . . ? C8 C7 C12 C13 -179.6(3) . . . . ? C6 C7 C12 C13 0.7(5) . . . . ? C10 C11 C12 C7 1.0(5) . . . . ? Si1 C11 C12 C7 -175.7(2) . . . . ? C10 C11 C12 C13 -179.1(3) . . . . ? Si1 C11 C12 C13 4.1(4) . . . . ? C1 N1 C13 C4 -0.3(5) . . . . ? C1 N1 C13 C12 179.3(3) . . . . ? C3 C4 C13 N1 -0.8(5) . . . . ? C5 C4 C13 N1 178.1(3) . . . . ? C3 C4 C13 C12 179.6(3) . . . . ? C5 C4 C13 C12 -1.5(5) . . . . ? C7 C12 C13 N1 -179.2(3) . . . . ? C11 C12 C13 N1 1.0(4) . . . . ? C7 C12 C13 C4 0.5(5) . . . . ? C11 C12 C13 C4 -179.4(3) . . . . ? C10 C11 Si1 C23 105.2(3) . . . . ? C12 C11 Si1 C23 -78.3(3) . . . . ? C10 C11 Si1 C14 -107.9(3) . . . . ? C12 C11 Si1 C14 68.6(3) . . . . ? C10 C11 Si1 C15 0.7(3) . . . . ? C12 C11 Si1 C15 177.2(3) . . . . ? C23 Si1 C15 C16 35(6) . . . . ? C14 Si1 C15 C16 -81(6) . . . . ? C11 Si1 C15 C16 157(6) . . . . ? Si1 C15 C16 C17 -4(10) . . . . ? C15 C16 C17 C18 117(5) . . . . ? C15 C16 C17 C22 -60(5) . . . . ? C22 C17 C18 C19 1.7(6) . . . . ? C16 C17 C18 C19 -175.3(4) . . . . ? C17 C18 C19 C20 0.3(7) . . . . ? C18 C19 C20 C21 -1.9(7) . . . . ? C19 C20 C21 C22 1.4(6) . . . . ? C20 C21 C22 C17 0.6(6) . . . . ? C18 C17 C22 C21 -2.2(6) . . . . ? C16 C17 C22 C21 174.8(3) . . . . ? C14 Si1 C23 C24 53(5) . . . . ? C15 Si1 C23 C24 -53(5) . . . . ? C11 Si1 C23 C24 -159(5) . . . . ? Si1 C23 C24 C25 -124(18) . . . . ? C23 C24 C25 C30 91(20) . . . . ? C23 C24 C25 C26 -90(20) . . . . ? C30 C25 C26 C27 -1.0(5) . . . . ? C24 C25 C26 C27 179.6(3) . . . . ? C25 C26 C27 C28 0.0(6) . . . . ? C26 C27 C28 C29 0.3(6) . . . . ? C27 C28 C29 C30 0.5(6) . . . . ? C26 C25 C30 C29 1.8(5) . . . . ? C24 C25 C30 C29 -178.8(3) . . . . ? C28 C29 C30 C25 -1.6(5) . . . . ? C43 N2 C31 C32 1.5(5) . . . . ? N2 C31 C32 C33 -1.1(5) . . . . ? C31 C32 C33 C34 -0.4(5) . . . . ? C32 C33 C34 C43 1.5(5) . . . . ? C32 C33 C34 C35 -176.6(3) . . . . ? C43 C34 C35 C36 -1.2(5) . . . . ? C33 C34 C35 C36 176.8(3) . . . . ? C34 C35 C36 C37 1.0(5) . . . . ? C35 C36 C37 C38 -178.7(3) . . . . ? C35 C36 C37 C42 2.2(5) . . . . ? C42 C37 C38 C39 0.9(5) . . . . ? C36 C37 C38 C39 -178.2(3) . . . . ? C37 C38 C39 C40 1.6(5) . . . . ? C38 C39 C40 C41 -2.7(5) . . . . ? C39 C40 C41 C42 1.1(5) . . . . ? C39 C40 C41 Si2 177.1(2) . . . . ? C38 C37 C42 C41 -2.6(5) . . . . ? C36 C37 C42 C41 176.5(3) . . . . ? C38 C37 C42 C43 175.9(3) . . . . ? C36 C37 C42 C43 -4.9(5) . . . . ? C40 C41 C42 C37 1.6(4) . . . . ? Si2 C41 C42 C37 -174.6(2) . . . . ? C40 C41 C42 C43 -176.9(3) . . . . ? Si2 C41 C42 C43 6.9(4) . . . . ? C31 N2 C43 C34 -0.3(5) . . . . ? C31 N2 C43 C42 178.5(3) . . . . ? C33 C34 C43 N2 -1.1(5) . . . . ? C35 C34 C43 N2 177.1(3) . . . . ? C33 C34 C43 C42 -179.9(3) . . . . ? C35 C34 C43 C42 -1.6(5) . . . . ? C37 C42 C43 N2 -174.1(3) . . . . ? C41 C42 C43 N2 4.5(4) . . . . ? C37 C42 C43 C34 4.7(4) . . . . ? C41 C42 C43 C34 -176.7(3) . . . . ? C40 C41 Si2 C53 101.2(3) . . . . ? C42 C41 Si2 C53 -82.9(3) . . . . ? C40 C41 Si2 C44 -113.2(3) . . . . ? C42 C41 Si2 C44 62.7(3) . . . . ? C40 C41 Si2 C45 -5.2(3) . . . . ? C42 C41 Si2 C45 170.8(2) . . . . ? C53 Si2 C45 C46 124(6) . . . . ? C44 Si2 C45 C46 3(6) . . . . ? C41 Si2 C45 C46 -118(6) . . . . ? Si2 C45 C46 C47 -134(7) . . . . ? C45 C46 C47 C52 -105(8) . . . . ? C45 C46 C47 C48 74(8) . . . . ? C52 C47 C48 C49 3.5(5) . . . . ? C46 C47 C48 C49 -175.8(3) . . . . ? C47 C48 C49 C50 -2.1(5) . . . . ? C48 C49 C50 C51 -1.3(6) . . . . ? C49 C50 C51 C52 3.2(6) . . . . ? C48 C47 C52 C51 -1.6(6) . . . . ? C46 C47 C52 C51 177.7(3) . . . . ? C50 C51 C52 C47 -1.7(6) . . . . ? C44 Si2 C53 C54 170(4) . . . . ? C45 Si2 C53 C54 63(4) . . . . ? C41 Si2 C53 C54 -44(4) . . . . ? Si2 C53 C54 C55 -6(12) . . . . ? C53 C54 C55 C60 -148(9) . . . . ? C53 C54 C55 C56 31(9) . . . . ? C60 C55 C56 C57 0.7(5) . . . . ? C54 C55 C56 C57 -177.8(3) . . . . ? C55 C56 C57 C58 0.1(5) . . . . ? C56 C57 C58 C59 -1.3(6) . . . . ? C57 C58 C59 C60 1.6(6) . . . . ? C58 C59 C60 C55 -0.8(5) . . . . ? C56 C55 C60 C59 -0.3(5) . . . . ? C54 C55 C60 C59 178.1(3) . . . . ? C73 N3 C61 C62 0.0(5) . . . . ? N3 C61 C62 C63 0.8(6) . . . . ? C61 C62 C63 C64 -0.3(6) . . . . ? C62 C63 C64 C73 -0.9(5) . . . . ? C62 C63 C64 C65 177.7(3) . . . . ? C63 C64 C65 C66 -179.9(3) . . . . ? C73 C64 C65 C66 -1.3(5) . . . . ? C64 C65 C66 C67 -0.9(5) . . . . ? C65 C66 C67 C68 -177.7(3) . . . . ? C65 C66 C67 C72 2.2(5) . . . . ? C72 C67 C68 C69 0.4(5) . . . . ? C66 C67 C68 C69 -179.8(3) . . . . ? C67 C68 C69 C70 0.5(5) . . . . ? C68 C69 C70 C71 -0.9(5) . . . . ? C69 C70 C71 C72 0.2(5) . . . . ? C69 C70 C71 Si3 -179.9(3) . . . . ? C68 C67 C72 C71 -1.1(5) . . . . ? C66 C67 C72 C71 179.1(3) . . . . ? C68 C67 C72 C73 178.6(3) . . . . ? C66 C67 C72 C73 -1.2(4) . . . . ? C70 C71 C72 C67 0.7(5) . . . . ? Si3 C71 C72 C67 -179.1(2) . . . . ? C70 C71 C72 C73 -178.9(3) . . . . ? Si3 C71 C72 C73 1.2(4) . . . . ? C61 N3 C73 C64 -1.3(5) . . . . ? C61 N3 C73 C72 179.5(3) . . . . ? C63 C64 C73 N3 1.7(5) . . . . ? C65 C64 C73 N3 -177.0(3) . . . . ? C63 C64 C73 C72 -179.1(3) . . . . ? C65 C64 C73 C72 2.2(5) . . . . ? C67 C72 C73 N3 178.3(3) . . . . ? C71 C72 C73 N3 -2.0(4) . . . . ? C67 C72 C73 C64 -1.0(4) . . . . ? C71 C72 C73 C64 178.7(3) . . . . ? C70 C71 Si3 C83 -108.3(3) . . . . ? C72 C71 Si3 C83 71.6(3) . . . . ? C70 C71 Si3 C74 108.9(3) . . . . ? C72 C71 Si3 C74 -71.2(3) . . . . ? C70 C71 Si3 C75 -1.9(3) . . . . ? C72 C71 Si3 C75 178.0(3) . . . . ? C83 Si3 C75 C76 -46(3) . . . . ? C74 Si3 C75 C76 70(3) . . . . ? C71 Si3 C75 C76 -167(3) . . . . ? Si3 C75 C76 C77 7(7) . . . . ? C75 C76 C77 C82 -96(4) . . . . ? C75 C76 C77 C78 78(4) . . . . ? C82 C77 C78 C79 1.1(6) . . . . ? C76 C77 C78 C79 -173.5(3) . . . . ? C77 C78 C79 C80 0.7(6) . . . . ? C78 C79 C80 C81 -1.9(6) . . . . ? C79 C80 C81 C82 1.2(6) . . . . ? C80 C81 C82 C77 0.6(6) . . . . ? C78 C77 C82 C81 -1.8(6) . . . . ? C76 C77 C82 C81 172.8(3) . . . . ? C74 Si3 C83 C84 -68(4) . . . . ? C75 Si3 C83 C84 40(4) . . . . ? C71 Si3 C83 C84 147(3) . . . . ? Si3 C83 C84 C85 35(25) . . . . ? C83 C84 C85 C90 -150(22) . . . . ? C83 C84 C85 C86 29(22) . . . . ? C90 C85 C86 C87 0.0(5) . . . . ? C84 C85 C86 C87 -178.7(3) . . . . ? C85 C86 C87 C88 0.4(5) . . . . ? C86 C87 C88 C89 -0.7(5) . . . . ? C87 C88 C89 C90 0.6(5) . . . . ? C86 C85 C90 C89 -0.2(5) . . . . ? C84 C85 C90 C89 178.6(3) . . . . ? C88 C89 C90 C85 -0.1(5) . . . . ? C103 N4 C91 C92 -2.3(5) . . . . ? N4 C91 C92 C93 1.2(6) . . . . ? C91 C92 C93 C94 0.9(5) . . . . ? C92 C93 C94 C103 -1.6(5) . . . . ? C92 C93 C94 C95 176.9(3) . . . . ? C93 C94 C95 C96 -177.1(3) . . . . ? C103 C94 C95 C96 1.3(5) . . . . ? C94 C95 C96 C97 -0.8(5) . . . . ? C95 C96 C97 C98 178.1(3) . . . . ? C95 C96 C97 C102 -1.2(5) . . . . ? C102 C97 C98 C99 -0.6(5) . . . . ? C96 C97 C98 C99 -179.9(3) . . . . ? C97 C98 C99 C100 -2.1(5) . . . . ? C98 C99 C100 C101 2.6(5) . . . . ? C99 C100 C101 C102 -0.3(5) . . . . ? C99 C100 C101 Si4 -173.0(3) . . . . ? C98 C97 C102 C101 2.9(5) . . . . ? C96 C97 C102 C101 -177.8(3) . . . . ? C98 C97 C102 C103 -176.8(3) . . . . ? C96 C97 C102 C103 2.5(4) . . . . ? C100 C101 C102 C97 -2.4(4) . . . . ? Si4 C101 C102 C97 170.4(2) . . . . ? C100 C101 C102 C103 177.3(3) . . . . ? Si4 C101 C102 C103 -9.9(4) . . . . ? C91 N4 C103 C94 1.5(5) . . . . ? C91 N4 C103 C102 -176.8(3) . . . . ? C93 C94 C103 N4 0.4(5) . . . . ? C95 C94 C103 N4 -178.1(3) . . . . ? C93 C94 C103 C102 178.6(3) . . . . ? C95 C94 C103 C102 0.1(5) . . . . ? C97 C102 C103 N4 176.4(3) . . . . ? C101 C102 C103 N4 -3.3(4) . . . . ? C97 C102 C103 C94 -2.0(5) . . . . ? C101 C102 C103 C94 178.3(3) . . . . ? C100 C101 Si4 C113 -107.9(3) . . . . ? C102 C101 Si4 C113 79.8(3) . . . . ? C100 C101 Si4 C104 107.9(3) . . . . ? C102 C101 Si4 C104 -64.4(3) . . . . ? C100 C101 Si4 C105 -0.9(3) . . . . ? C102 C101 Si4 C105 -173.2(2) . . . . ? C113 Si4 C105 C106 23(26) . . . . ? C104 Si4 C105 C106 140(26) . . . . ? C101 Si4 C105 C106 -102(26) . . . . ? Si4 C105 C106 C107 -46(30) . . . . ? C105 C106 C107 C108 -126(6) . . . . ? C105 C106 C107 C112 52(7) . . . . ? C112 C107 C108 C109 -2.0(6) . . . . ? C106 C107 C108 C109 176.0(4) . . . . ? C107 C108 C109 C110 -0.3(6) . . . . ? C108 C109 C110 C111 2.2(6) . . . . ? C109 C110 C111 C112 -1.9(6) . . . . ? C110 C111 C112 C107 -0.4(6) . . . . ? C108 C107 C112 C111 2.4(6) . . . . ? C106 C107 C112 C111 -175.7(3) . . . . ? C104 Si4 C113 C114 -35(3) . . . . ? C105 Si4 C113 C114 72(3) . . . . ? C101 Si4 C113 C114 -179(100) . . . . ? Si4 C113 C114 C115 75(56) . . . . ? C113 C114 C115 C116 127(55) . . . . ? C113 C114 C115 C120 -53(55) . . . . ? C120 C115 C116 C117 0.7(5) . . . . ? C114 C115 C116 C117 -179.3(3) . . . . ? C115 C116 C117 C118 -0.1(5) . . . . ? C116 C117 C118 C119 -0.7(5) . . . . ? C117 C118 C119 C120 0.9(5) . . . . ? C118 C119 C120 C115 -0.3(5) . . . . ? C116 C115 C120 C119 -0.5(5) . . . . ? C114 C115 C120 C119 179.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.366 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.067 # Attachment '- 2F.cif' data_m4 _database_code_depnum_ccdc_archive 'CCDC 888306' #TrackingRef '- 2F.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H17 F12 N Si' _chemical_formula_weight 695.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_n_a_21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 7.3912(9) _cell_length_b 19.057(2) _cell_length_c 21.384(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3012.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9823 _exptl_absorpt_correction_T_max 0.9823 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21531 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5248 _reflns_number_gt 4955 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0454P)^2^+0.8592P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.92(11) _refine_ls_number_reflns 5248 _refine_ls_number_parameters 501 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.085 _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 0.75018(8) 0.45683(3) 0.31501(3) 0.02155(13) Uani 1 1 d . . . N1 N 0.7234(2) 0.33424(8) 0.31776(9) 0.0219(4) Uani 1 1 d . . . C1 C 0.6674(3) 0.28730(12) 0.27619(11) 0.0256(5) Uani 1 1 d . . . H1 H 0.633(3) 0.3028(13) 0.2377(13) 0.025(6) Uiso 1 1 d . . . C2 C 0.6649(3) 0.21548(12) 0.28882(12) 0.0288(5) Uani 1 1 d . . . H2 H 0.619(4) 0.1841(14) 0.2624(13) 0.031(7) Uiso 1 1 d . . . C3 C 0.7223(3) 0.19167(11) 0.34631(11) 0.0268(5) Uani 1 1 d . . . H3 H 0.727(3) 0.1421(14) 0.3566(11) 0.020(6) Uiso 1 1 d . . . C4 C 0.7849(3) 0.23985(11) 0.39108(10) 0.0237(4) Uani 1 1 d . . . C5 C 0.8532(3) 0.22151(12) 0.45123(12) 0.0284(5) Uani 1 1 d . . . H4 H 0.855(4) 0.1716(15) 0.4640(13) 0.037(7) Uiso 1 1 d . . . C6 C 0.9150(3) 0.27141(13) 0.49066(12) 0.0293(5) Uani 1 1 d . . . H5 H 0.960(4) 0.2590(17) 0.5290(16) 0.048(9) Uiso 1 1 d . . . C7 C 0.9182(3) 0.34407(12) 0.47380(10) 0.0261(5) Uani 1 1 d . . . C8 C 0.9949(3) 0.39707(13) 0.51154(11) 0.0312(5) Uani 1 1 d . . . H6 H 1.051(4) 0.3838(14) 0.5530(14) 0.036(7) Uiso 1 1 d . . . C9 C 0.9981(3) 0.46503(13) 0.49176(11) 0.0324(5) Uani 1 1 d . . . H7 H 1.054(3) 0.5028(13) 0.5165(11) 0.026(6) Uiso 1 1 d . . . C10 C 0.9261(3) 0.48423(12) 0.43339(11) 0.0280(5) Uani 1 1 d . . . H8 H 0.931(4) 0.5345(15) 0.4177(13) 0.039(7) Uiso 1 1 d . . . C11 C 0.8495(3) 0.43469(11) 0.39405(11) 0.0245(5) Uani 1 1 d . . . C12 C 0.8482(3) 0.36436(11) 0.41507(10) 0.0221(4) Uani 1 1 d . . . C13 C 0.7815(3) 0.31113(11) 0.37376(10) 0.0223(4) Uani 1 1 d . . . C14 C 0.5006(3) 0.45690(13) 0.29997(13) 0.0308(5) Uani 1 1 d . . . H9 H 0.454(3) 0.4140(14) 0.2847(12) 0.027(6) Uiso 1 1 d . . . H10 H 0.447(4) 0.4679(17) 0.3346(17) 0.053(10) Uiso 1 1 d . . . H11 H 0.471(5) 0.4969(18) 0.2726(15) 0.056(9) Uiso 1 1 d . . . C15 C 0.8876(3) 0.43819(11) 0.24510(10) 0.0232(4) Uani 1 1 d . . . C16 C 0.9766(3) 0.43109(10) 0.19848(10) 0.0242(4) Uani 1 1 d . . . C17 C 1.0958(3) 0.42729(11) 0.14539(10) 0.0248(5) Uani 1 1 d . . . C18 C 1.0863(3) 0.37345(11) 0.10039(10) 0.0273(5) Uani 1 1 d . . . C19 C 1.2084(4) 0.37224(13) 0.05111(12) 0.0328(5) Uani 1 1 d . . . H12 H 1.201(4) 0.3377(16) 0.0215(14) 0.040(7) Uiso 1 1 d . . . C20 C 1.3384(4) 0.42369(14) 0.04553(13) 0.0370(6) Uani 1 1 d . . . H13 H 1.416(4) 0.4205(15) 0.0140(15) 0.044(8) Uiso 1 1 d . . . C21 C 1.3465(3) 0.47775(13) 0.08825(12) 0.0329(5) Uani 1 1 d . . . C22 C 1.2265(3) 0.47939(12) 0.13812(12) 0.0291(5) Uani 1 1 d . . . H14 H 1.228(3) 0.5144(14) 0.1680(13) 0.029(6) Uiso 1 1 d . . . C23 C 1.4861(4) 0.53427(16) 0.08154(13) 0.0441(7) Uani 1 1 d . . . C24 C 0.9435(4) 0.31824(12) 0.10447(11) 0.0330(5) Uani 1 1 d . . . C25 C 0.7890(3) 0.55489(10) 0.31436(11) 0.0238(4) Uani 1 1 d . . . C26 C 0.8094(3) 0.61734(11) 0.31081(11) 0.0241(4) Uani 1 1 d . . . C27 C 0.8300(3) 0.69211(10) 0.30657(10) 0.0223(4) Uani 1 1 d . . . C28 C 0.8813(3) 0.72637(11) 0.25112(10) 0.0258(5) Uani 1 1 d . . . C29 C 0.8953(3) 0.79867(12) 0.24914(11) 0.0295(5) Uani 1 1 d . . . H15 H 0.935(3) 0.8230(13) 0.2094(13) 0.034(7) Uiso 1 1 d . . . C30 C 0.8623(3) 0.83854(11) 0.30215(11) 0.0283(5) Uani 1 1 d . . . H16 H 0.871(3) 0.8889(14) 0.3028(12) 0.028(6) Uiso 1 1 d . . . C31 C 0.8155(3) 0.80520(11) 0.35737(11) 0.0237(5) Uani 1 1 d . . . C32 C 0.7974(3) 0.73273(11) 0.35960(11) 0.0230(4) Uani 1 1 d . . . H17 H 0.765(3) 0.7113(13) 0.3974(12) 0.023(6) Uiso 1 1 d . . . C33 C 0.7855(3) 0.84573(12) 0.41651(11) 0.0287(5) Uani 1 1 d . . . C34 C 0.9160(4) 0.68430(13) 0.19274(12) 0.0367(6) Uani 1 1 d . . . F1 F 0.8264(3) 0.91331(7) 0.41114(8) 0.0508(4) Uani 1 1 d . . . F2 F 0.8852(2) 0.82037(9) 0.46329(7) 0.0491(4) Uani 1 1 d . . . F3 F 0.6137(2) 0.84295(8) 0.43603(7) 0.0430(4) Uani 1 1 d . . . F4 F 0.9814(4) 0.72478(10) 0.14691(8) 0.0754(7) Uani 1 1 d . . . F5 F 1.0373(2) 0.63329(9) 0.20084(8) 0.0501(4) Uani 1 1 d . . . F6 F 0.7668(2) 0.65373(9) 0.17109(8) 0.0504(4) Uani 1 1 d . . . F7 F 0.9545(2) 0.27148(7) 0.05808(7) 0.0467(4) Uani 1 1 d . . . F8 F 0.7769(2) 0.34488(8) 0.10293(8) 0.0459(4) Uani 1 1 d . . . F9 F 0.9538(2) 0.28090(7) 0.15791(7) 0.0437(4) Uani 1 1 d . . . F10 F 1.4372(3) 0.59403(10) 0.10775(12) 0.0777(7) Uani 1 1 d . . . F11 F 1.6441(2) 0.51605(12) 0.10412(14) 0.0844(7) Uani 1 1 d . . . F12 F 1.5172(3) 0.55032(13) 0.02168(10) 0.0839(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 0.0250(3) 0.0163(2) 0.0233(3) -0.0011(2) 0.0005(2) -0.0005(2) N1 0.0237(9) 0.0198(8) 0.0223(9) 0.0002(8) 0.0013(8) -0.0015(7) C1 0.0267(11) 0.0285(12) 0.0218(12) -0.0030(9) -0.0015(9) 0.0000(9) C2 0.0257(11) 0.0226(11) 0.0380(14) -0.0088(10) 0.0023(10) -0.0050(9) C3 0.0257(12) 0.0180(11) 0.0368(13) 0.0004(9) 0.0065(10) -0.0010(8) C4 0.0227(10) 0.0225(11) 0.0259(11) 0.0023(9) 0.0057(9) -0.0001(8) C5 0.0265(11) 0.0240(11) 0.0346(13) 0.0082(10) 0.0054(10) 0.0008(9) C6 0.0254(11) 0.0362(13) 0.0264(12) 0.0074(10) 0.0014(10) 0.0003(10) C7 0.0240(11) 0.0320(12) 0.0224(11) 0.0007(9) 0.0040(9) 0.0017(9) C8 0.0322(13) 0.0395(13) 0.0220(12) -0.0032(10) -0.0028(10) 0.0024(10) C9 0.0361(13) 0.0344(13) 0.0267(12) -0.0105(10) 0.0002(10) -0.0024(10) C10 0.0295(12) 0.0251(11) 0.0293(12) -0.0029(9) 0.0011(10) -0.0007(9) C11 0.0230(11) 0.0202(10) 0.0302(12) -0.0007(9) 0.0021(9) 0.0008(8) C12 0.0208(10) 0.0240(10) 0.0215(10) -0.0007(9) 0.0037(8) 0.0009(8) C13 0.0197(10) 0.0220(11) 0.0254(12) 0.0015(9) 0.0058(9) 0.0009(8) C14 0.0279(12) 0.0224(11) 0.0421(16) -0.0002(11) -0.0001(11) 0.0011(9) C15 0.0332(11) 0.0171(10) 0.0194(11) 0.0003(8) -0.0022(10) 0.0004(9) C16 0.0338(11) 0.0169(9) 0.0218(11) 0.0018(8) -0.0038(10) 0.0003(9) C17 0.0289(11) 0.0214(10) 0.0241(11) 0.0022(8) -0.0018(9) 0.0054(9) C18 0.0358(12) 0.0251(11) 0.0210(11) -0.0001(9) -0.0028(10) 0.0082(9) C19 0.0424(14) 0.0265(12) 0.0296(13) -0.0038(10) 0.0028(11) 0.0082(10) C20 0.0349(13) 0.0377(14) 0.0383(14) -0.0007(11) 0.0111(12) 0.0086(11) C21 0.0288(12) 0.0335(12) 0.0363(14) 0.0003(10) 0.0033(10) 0.0041(10) C22 0.0325(13) 0.0240(11) 0.0309(13) -0.0041(10) 0.0002(10) 0.0048(9) C23 0.0344(14) 0.0514(17) 0.0465(16) -0.0039(13) 0.0106(12) -0.0046(12) C24 0.0494(15) 0.0266(12) 0.0229(11) -0.0008(9) -0.0009(11) 0.0006(11) C25 0.0314(12) 0.0213(10) 0.0188(10) -0.0028(10) 0.0011(10) -0.0006(8) C26 0.0260(11) 0.0247(11) 0.0216(11) -0.0008(9) -0.0001(9) -0.0005(8) C27 0.0201(10) 0.0183(9) 0.0285(12) -0.0027(9) -0.0018(9) -0.0009(8) C28 0.0281(11) 0.0290(12) 0.0202(11) 0.0004(9) 0.0014(9) -0.0048(9) C29 0.0347(12) 0.0271(11) 0.0268(12) 0.0037(10) -0.0007(10) -0.0059(10) C30 0.0292(12) 0.0201(10) 0.0357(14) 0.0033(9) -0.0030(10) -0.0037(9) C31 0.0202(10) 0.0204(11) 0.0303(12) -0.0003(9) -0.0050(9) -0.0001(8) C32 0.0224(10) 0.0211(11) 0.0254(11) 0.0021(9) -0.0017(9) -0.0022(8) C33 0.0300(12) 0.0248(11) 0.0312(12) -0.0043(10) -0.0029(10) -0.0016(9) C34 0.0491(15) 0.0332(13) 0.0278(13) -0.0037(10) 0.0058(12) -0.0114(12) F1 0.0761(11) 0.0224(7) 0.0540(10) -0.0129(7) 0.0133(9) -0.0088(7) F2 0.0612(10) 0.0504(9) 0.0356(8) -0.0172(7) -0.0204(8) 0.0160(8) F3 0.0374(8) 0.0505(9) 0.0411(9) -0.0136(7) 0.0084(7) -0.0017(7) F4 0.140(2) 0.0531(11) 0.0330(9) -0.0071(8) 0.0353(11) -0.0279(12) F5 0.0463(9) 0.0551(10) 0.0488(9) -0.0241(8) 0.0097(7) 0.0042(7) F6 0.0516(9) 0.0575(10) 0.0423(9) -0.0217(8) -0.0100(7) -0.0020(8) F7 0.0730(11) 0.0330(8) 0.0340(8) -0.0119(6) 0.0012(8) -0.0113(7) F8 0.0405(8) 0.0405(8) 0.0568(10) -0.0043(7) -0.0077(7) -0.0053(7) F9 0.0672(11) 0.0315(7) 0.0324(8) 0.0061(6) -0.0054(7) -0.0092(7) F10 0.0609(11) 0.0507(11) 0.1215(18) -0.0257(12) 0.0369(13) -0.0227(9) F11 0.0367(10) 0.0833(14) 0.133(2) 0.0211(15) -0.0191(12) -0.0145(9) F12 0.0927(17) 0.0901(16) 0.0688(14) 0.0085(11) 0.0200(12) -0.0465(13) _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 C15 1.842(2) . ? Si1 C14 1.873(3) . ? Si1 C11 1.890(2) . ? Si1 C25 1.891(2) . ? Si1 N1 2.3454(17) . ? N1 C1 1.327(3) . ? N1 C13 1.346(3) . ? C1 C2 1.395(3) . ? C2 C3 1.377(4) . ? C3 C4 1.405(3) . ? C4 C13 1.408(3) . ? C4 C5 1.425(3) . ? C5 C6 1.351(4) . ? C6 C7 1.431(3) . ? C7 C8 1.411(3) . ? C7 C12 1.412(3) . ? C8 C9 1.363(4) . ? C9 C10 1.405(4) . ? C10 C11 1.385(3) . ? C11 C12 1.414(3) . ? C12 C13 1.433(3) . ? C15 C16 1.202(3) . ? C16 C17 1.439(3) . ? C17 C22 1.394(3) . ? C17 C18 1.408(3) . ? C18 C19 1.387(3) . ? C18 C24 1.493(3) . ? C19 C20 1.378(4) . ? C20 C21 1.378(4) . ? C21 C22 1.388(4) . ? C21 C23 1.498(4) . ? C23 F11 1.310(4) . ? C23 F10 1.320(3) . ? C23 F12 1.336(3) . ? C24 F8 1.332(3) . ? C24 F7 1.336(3) . ? C24 F9 1.348(3) . ? C25 C26 1.202(3) . ? C26 C27 1.436(3) . ? C27 C32 1.394(3) . ? C27 C28 1.406(3) . ? C28 C29 1.382(3) . ? C28 C34 1.506(3) . ? C29 C30 1.386(3) . ? C30 C31 1.385(3) . ? C31 C32 1.388(3) . ? C31 C33 1.498(3) . ? C33 F1 1.328(3) . ? C33 F2 1.333(3) . ? C33 F3 1.337(3) . ? C34 F6 1.330(3) . ? C34 F5 1.334(3) . ? C34 F4 1.338(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 Si1 C14 113.82(11) . . ? C15 Si1 C11 117.94(9) . . ? C14 Si1 C11 122.44(11) . . ? C15 Si1 C25 95.80(10) . . ? C14 Si1 C25 98.49(10) . . ? C11 Si1 C25 99.69(10) . . ? C15 Si1 N1 82.80(8) . . ? C14 Si1 N1 85.53(9) . . ? C11 Si1 N1 77.76(8) . . ? C25 Si1 N1 175.97(8) . . ? C1 N1 C13 118.34(18) . . ? C1 N1 Si1 132.91(16) . . ? C13 N1 Si1 108.75(13) . . ? N1 C1 C2 122.4(2) . . ? C3 C2 C1 119.5(2) . . ? C2 C3 C4 119.6(2) . . ? C3 C4 C13 116.5(2) . . ? C3 C4 C5 124.8(2) . . ? C13 C4 C5 118.7(2) . . ? C6 C5 C4 120.7(2) . . ? C5 C6 C7 122.0(2) . . ? C8 C7 C12 117.4(2) . . ? C8 C7 C6 123.7(2) . . ? C12 C7 C6 118.9(2) . . ? C9 C8 C7 120.6(2) . . ? C8 C9 C10 121.1(2) . . ? C11 C10 C9 121.1(2) . . ? C10 C11 C12 117.1(2) . . ? C10 C11 Si1 123.32(17) . . ? C12 C11 Si1 119.55(16) . . ? C7 C12 C11 122.7(2) . . ? C7 C12 C13 118.73(19) . . ? C11 C12 C13 118.5(2) . . ? N1 C13 C4 123.7(2) . . ? N1 C13 C12 115.25(18) . . ? C4 C13 C12 121.0(2) . . ? C16 C15 Si1 175.27(18) . . ? C15 C16 C17 174.3(2) . . ? C22 C17 C18 118.5(2) . . ? C22 C17 C16 118.5(2) . . ? C18 C17 C16 123.0(2) . . ? C19 C18 C17 119.9(2) . . ? C19 C18 C24 119.5(2) . . ? C17 C18 C24 120.6(2) . . ? C20 C19 C18 120.5(2) . . ? C19 C20 C21 120.3(2) . . ? C20 C21 C22 119.9(2) . . ? C20 C21 C23 120.3(2) . . ? C22 C21 C23 119.8(2) . . ? C21 C22 C17 120.9(2) . . ? F11 C23 F10 108.4(3) . . ? F11 C23 F12 105.1(3) . . ? F10 C23 F12 104.9(3) . . ? F11 C23 C21 112.8(2) . . ? F10 C23 C21 113.0(2) . . ? F12 C23 C21 112.0(2) . . ? F8 C24 F7 107.0(2) . . ? F8 C24 F9 105.9(2) . . ? F7 C24 F9 105.89(18) . . ? F8 C24 C18 112.54(19) . . ? F7 C24 C18 112.6(2) . . ? F9 C24 C18 112.5(2) . . ? C26 C25 Si1 176.5(2) . . ? C25 C26 C27 178.9(2) . . ? C32 C27 C28 118.35(19) . . ? C32 C27 C26 118.8(2) . . ? C28 C27 C26 122.9(2) . . ? C29 C28 C27 120.6(2) . . ? C29 C28 C34 119.5(2) . . ? C27 C28 C34 119.87(19) . . ? C28 C29 C30 120.5(2) . . ? C31 C30 C29 119.3(2) . . ? C30 C31 C32 120.6(2) . . ? C30 C31 C33 121.34(19) . . ? C32 C31 C33 118.0(2) . . ? C31 C32 C27 120.5(2) . . ? F1 C33 F2 106.87(19) . . ? F1 C33 F3 106.38(19) . . ? F2 C33 F3 106.0(2) . . ? F1 C33 C31 113.2(2) . . ? F2 C33 C31 111.38(18) . . ? F3 C33 C31 112.55(18) . . ? F6 C34 F5 106.45(19) . . ? F6 C34 F4 107.3(2) . . ? F5 C34 F4 105.8(2) . . ? F6 C34 C28 112.4(2) . . ? F5 C34 C28 113.3(2) . . ? F4 C34 C28 111.23(19) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.300 _refine_diff_density_min -0.185 _refine_diff_density_rms 0.044