# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 152446, 152447, 152448 data_global _publ_creation_date 1997-11-19 _publ_creation_method 'SHELXL-97 (Sheldrick, 1997)' _publ_contact_author 'Prof D Jurgen Martens' _publ_contact_author_address ; Prof D Jurgen Martens Department of Chemistry University of Oldenburg Oldenburg 26111 GERMANY ; _publ_contact_author_email ? _publ_requested_journal 'Perkin Transactions 1' _journal_coden_Cambridge 207 _publ_section_title ; Silylene and Disilene Additions to an Octa-1,3,5,7-tetrayne: Formation of a C-C-linked Quatersilirene ; loop_ _publ_author_name _publ_author_adress 'Martens, Juergen' ; Fachbereich Chemie der Universitaet Oldenburg Carl-von-Ossietzky-Strasse 9-11 D-26111 Oldenburg Germany ; 'Ostendorf, Detlev' ; Fachbereich Chemie der Universitaet Oldenburg Carl-von-Ossietzky-Strasse 9-11 D-26111 Oldenburg Germany ; 'Saak, Wolfgang' ; Fachbereich Chemie der Universitaet Oldenburg Carl-von-Ossietzky-Strasse 9-11 D-26111 Oldenburg Germany ; 'von Keyserlingk, Nikolai Graf' ; Fachbereich Chemie der Universitaet Oldenburg Carl-von-Ossietzky-Strasse 9-11 D-26111 Oldenburg Germany ; 'Weidenbruch, Manfred' ; Fachbereich Chemie der Universitaet Oldenburg Carl-von-Ossietzky-Strasse 9-11 D-26111 Oldenburg Germany ; _publ_section_abstract ; ? ; data_messima _database_code_CSD 152446 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 N2 Si' _chemical_formula_weight 452.70 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 orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 7.5318(2) _cell_length_b 13.3032(5) _cell_length_c 25.6712(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2572.18(13) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9261 _exptl_absorpt_correction_T_max 0.9464 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'imaging plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18649 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.97 _reflns_number_total 4806 _reflns_number_gt 4434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1997)' _computing_cell_refinement 'IPDS (Stoe, 1997)' _computing_data_reduction 'XRED (Stoe, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _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^)+(0.0853P)^2^+0.2342P] 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 -0.01(12) _refine_ls_number_reflns 4806 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 0.79438(6) 0.49230(3) 0.882672(19) 0.02374(13) Uani 1 1 d . . . N1 N 0.6383(2) 0.39512(11) 0.87593(7) 0.0293(4) Uani 1 1 d . . . N2 N 0.9145(2) 0.44425(12) 0.83039(7) 0.0301(4) Uani 1 1 d . . . C1 C 0.4722(3) 0.38467(15) 0.89799(8) 0.0337(4) Uani 1 1 d . . . H1 H 0.4277 0.4375 0.9192 0.040 Uiso 1 1 calc R . . C2 C 0.3715(3) 0.30286(17) 0.89062(10) 0.0416(5) Uani 1 1 d . . . H2 H 0.2570 0.2985 0.9060 0.050 Uiso 1 1 calc R . . C3 C 0.4389(3) 0.22109(16) 0.85887(10) 0.0426(5) Uani 1 1 d . . . H3 H 0.3720 0.1609 0.8555 0.051 Uiso 1 1 calc R . . C4 C 0.5954(3) 0.23019(16) 0.83432(9) 0.0398(5) Uani 1 1 d . . . H4 H 0.6381 0.1764 0.8135 0.048 Uiso 1 1 calc R . . C5 C 0.6994(3) 0.32054(14) 0.83918(8) 0.0329(4) Uani 1 1 d . . . C6 C 0.8493(3) 0.34986(15) 0.81491(8) 0.0340(5) Uani 1 1 d . . . C7 C 0.9730(4) 0.30276(18) 0.77642(11) 0.0509(6) Uani 1 1 d . . . H7A H 0.9134 0.2939 0.7424 0.061 Uiso 1 1 calc R . . H7B H 1.0134 0.2362 0.7890 0.061 Uiso 1 1 calc R . . C8 C 1.1300(3) 0.37477(18) 0.77137(9) 0.0420(5) Uani 1 1 d . . . H8 H 1.2413 0.3411 0.7834 0.050 Uiso 1 1 calc R . . C9 C 1.1576(4) 0.4191(2) 0.71708(11) 0.0527(6) Uani 1 1 d . . . H9A H 1.2843 0.4355 0.7112 0.063 Uiso 1 1 calc R . . H9B H 1.1180 0.3715 0.6898 0.063 Uiso 1 1 calc R . . C10 C 1.0452(4) 0.51328(19) 0.71656(9) 0.0462(6) Uani 1 1 d . . . H10A H 0.9178 0.4971 0.7123 0.055 Uiso 1 1 calc R . . H10B H 1.0825 0.5596 0.6885 0.055 Uiso 1 1 calc R . . C11 C 1.0825(3) 0.55788(16) 0.77027(9) 0.0353(5) Uani 1 1 d . . . H11A H 0.9875 0.6053 0.7806 0.042 Uiso 1 1 calc R . . H11B H 1.1977 0.5937 0.7706 0.042 Uiso 1 1 calc R . . C12 C 1.0870(3) 0.46594(15) 0.80710(8) 0.0319(4) Uani 1 1 d . . . H12 H 1.1800 0.4744 0.8345 0.038 Uiso 1 1 calc R . . C13 C 0.9524(2) 0.49197(14) 0.93977(7) 0.0276(4) Uani 1 1 d . . . C14 C 0.9522(3) 0.41537(16) 0.97814(9) 0.0372(5) Uani 1 1 d . . . C15 C 1.0786(3) 0.41691(18) 1.01756(9) 0.0430(5) Uani 1 1 d . . . H15 H 1.0751 0.3662 1.0436 0.052 Uiso 1 1 calc R . . C16 C 1.2100(3) 0.49008(19) 1.02019(9) 0.0423(5) Uani 1 1 d . . . C17 C 1.2127(3) 0.56293(17) 0.98204(9) 0.0371(5) Uani 1 1 d . . . H17 H 1.3027 0.6129 0.9829 0.044 Uiso 1 1 calc R . . C18 C 1.0860(3) 0.56536(15) 0.94180(8) 0.0300(4) Uani 1 1 d . . . C19 C 0.8196(5) 0.3300(2) 0.97848(12) 0.0646(9) Uani 1 1 d . . . H19A H 0.8437 0.2857 1.0082 0.097 Uiso 1 1 calc R . . H19B H 0.8300 0.2916 0.9460 0.097 Uiso 1 1 calc R . . H19C H 0.6992 0.3573 0.9815 0.097 Uiso 1 1 calc R . . C20 C 1.3448(4) 0.4903(3) 1.06422(12) 0.0653(8) Uani 1 1 d . . . H20A H 1.4261 0.5471 1.0598 0.098 Uiso 1 1 calc R . . H20B H 1.4123 0.4273 1.0636 0.098 Uiso 1 1 calc R . . H20C H 1.2828 0.4965 1.0976 0.098 Uiso 1 1 calc R . . C21 C 1.1012(3) 0.64982(17) 0.90243(9) 0.0383(5) Uani 1 1 d . . . H21A H 1.0068 0.6432 0.8764 0.057 Uiso 1 1 calc R . . H21B H 1.2171 0.6462 0.8851 0.057 Uiso 1 1 calc R . . H21C H 1.0897 0.7146 0.9203 0.057 Uiso 1 1 calc R . . C22 C 0.6671(2) 0.61392(13) 0.87619(8) 0.0247(4) Uani 1 1 d . . . C23 C 0.6371(3) 0.68079(14) 0.91849(8) 0.0290(4) Uani 1 1 d . . . C24 C 0.5499(3) 0.77210(15) 0.91015(10) 0.0360(5) Uani 1 1 d . . . H24 H 0.5333 0.8165 0.9387 0.043 Uiso 1 1 calc R . . C25 C 0.4870(3) 0.79971(15) 0.86166(10) 0.0380(5) Uani 1 1 d . . . C26 C 0.5089(3) 0.73296(16) 0.82066(9) 0.0356(5) Uani 1 1 d . . . H26 H 0.4653 0.7507 0.7872 0.043 Uiso 1 1 calc R . . C27 C 0.5935(3) 0.64023(15) 0.82724(8) 0.0295(4) Uani 1 1 d . . . C28 C 0.6895(3) 0.65777(17) 0.97401(9) 0.0404(5) Uani 1 1 d . . . H28A H 0.7496 0.5925 0.9753 0.061 Uiso 1 1 calc R . . H28B H 0.5830 0.6557 0.9959 0.061 Uiso 1 1 calc R . . H28C H 0.7700 0.7102 0.9868 0.061 Uiso 1 1 calc R . . C29 C 0.3903(4) 0.89876(19) 0.85434(14) 0.0611(8) Uani 1 1 d . . . H29A H 0.3885 0.9356 0.8874 0.092 Uiso 1 1 calc R . . H29B H 0.2682 0.8857 0.8430 0.092 Uiso 1 1 calc R . . H29C H 0.4517 0.9390 0.8279 0.092 Uiso 1 1 calc R . . C30 C 0.5954(3) 0.57012(19) 0.78102(9) 0.0412(5) Uani 1 1 d . . . H30A H 0.6579 0.5081 0.7903 0.062 Uiso 1 1 calc R . . H30B H 0.6562 0.6026 0.7518 0.062 Uiso 1 1 calc R . . H30C H 0.4731 0.5541 0.7709 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0331(2) 0.0205(2) 0.0176(3) -0.00027(18) -0.00019(18) -0.0003(2) N1 0.0405(8) 0.0232(7) 0.0243(10) -0.0013(6) 0.0012(7) -0.0027(6) N2 0.0418(9) 0.0237(7) 0.0248(9) -0.0014(6) 0.0038(7) 0.0011(7) C1 0.0435(11) 0.0318(9) 0.0256(12) 0.0035(8) 0.0018(8) -0.0031(8) C2 0.0437(11) 0.0424(11) 0.0388(14) 0.0100(10) -0.0033(9) -0.0095(9) C3 0.0585(14) 0.0281(10) 0.0412(14) 0.0061(9) -0.0120(11) -0.0144(9) C4 0.0617(14) 0.0247(9) 0.0330(13) -0.0020(8) -0.0107(10) -0.0048(9) C5 0.0486(11) 0.0228(9) 0.0274(11) -0.0030(7) -0.0030(9) -0.0029(9) C6 0.0517(12) 0.0249(9) 0.0255(12) -0.0045(8) -0.0001(9) 0.0026(8) C7 0.0787(18) 0.0349(11) 0.0393(15) -0.0095(9) 0.0139(13) 0.0035(11) C8 0.0461(12) 0.0479(13) 0.0319(13) -0.0047(10) 0.0007(9) 0.0173(10) C9 0.0611(15) 0.0578(15) 0.0391(16) -0.0094(11) 0.0137(11) 0.0015(12) C10 0.0631(15) 0.0464(13) 0.0290(13) 0.0030(10) 0.0059(10) -0.0030(11) C11 0.0367(10) 0.0380(11) 0.0312(12) 0.0001(8) 0.0067(9) -0.0068(9) C12 0.0317(9) 0.0391(10) 0.0250(11) 0.0001(8) -0.0020(8) 0.0065(8) C13 0.0356(9) 0.0272(9) 0.0199(9) -0.0015(7) -0.0011(7) 0.0057(8) C14 0.0475(12) 0.0330(10) 0.0312(13) 0.0046(8) -0.0029(9) 0.0027(9) C15 0.0555(13) 0.0437(12) 0.0297(13) 0.0058(9) -0.0073(10) 0.0121(10) C16 0.0442(11) 0.0552(13) 0.0276(12) -0.0046(10) -0.0064(9) 0.0152(12) C17 0.0354(10) 0.0453(11) 0.0306(12) -0.0084(9) -0.0038(9) 0.0033(9) C18 0.0331(9) 0.0336(10) 0.0234(11) -0.0058(7) 0.0011(8) 0.0046(8) C19 0.086(2) 0.0529(15) 0.0549(19) 0.0337(13) -0.0273(16) -0.0230(15) C20 0.0587(15) 0.093(2) 0.0440(17) 0.0051(15) -0.0198(12) 0.0058(16) C21 0.0429(11) 0.0401(11) 0.0319(12) 0.0019(9) -0.0017(9) -0.0138(9) C22 0.0275(8) 0.0236(8) 0.0232(11) -0.0014(7) 0.0005(7) -0.0024(6) C23 0.0296(9) 0.0258(9) 0.0316(12) -0.0049(8) -0.0001(7) -0.0039(7) C24 0.0317(10) 0.0266(9) 0.0498(14) -0.0104(9) 0.0023(9) -0.0008(8) C25 0.0318(10) 0.0249(9) 0.0572(15) 0.0068(9) 0.0026(9) 0.0012(8) C26 0.0322(10) 0.0381(11) 0.0363(13) 0.0117(9) -0.0027(8) 0.0019(8) C27 0.0275(9) 0.0331(10) 0.0279(11) 0.0034(8) -0.0011(7) -0.0017(8) C28 0.0497(12) 0.0450(12) 0.0265(12) -0.0124(9) -0.0010(9) 0.0100(10) C29 0.0613(16) 0.0367(13) 0.085(2) 0.0131(13) 0.0024(15) 0.0162(12) C30 0.0414(11) 0.0557(13) 0.0264(12) -0.0049(10) -0.0075(9) 0.0084(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N2 1.7404(17) . ? Si1 N1 1.7559(16) . ? Si1 C13 1.8880(19) . ? Si1 C22 1.8880(19) . ? N1 C1 1.380(3) . ? N1 C5 1.445(2) . ? N2 C6 1.406(3) . ? N2 C12 1.459(3) . ? C1 C2 1.340(3) . ? C2 C3 1.451(4) . ? C3 C4 1.342(4) . ? C4 C5 1.440(3) . ? C5 C6 1.347(3) . ? C6 C7 1.496(3) . ? C7 C8 1.527(4) . ? C8 C9 1.528(4) . ? C8 C12 1.555(3) . ? C9 C10 1.512(4) . ? C10 C11 1.527(3) . ? C11 C12 1.546(3) . ? C13 C18 1.403(3) . ? C13 C14 1.417(3) . ? C14 C15 1.390(3) . ? C14 C19 1.512(3) . ? C15 C16 1.389(4) . ? C16 C17 1.378(3) . ? C16 C20 1.519(3) . ? C17 C18 1.407(3) . ? C18 C21 1.516(3) . ? C22 C27 1.417(3) . ? C22 C23 1.422(3) . ? C23 C24 1.398(3) . ? C23 C28 1.510(3) . ? C24 C25 1.381(3) . ? C25 C26 1.387(3) . ? C25 C29 1.518(3) . ? C26 C27 1.399(3) . ? C27 C30 1.509(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 N2 Si1 N1 90.09(8) . . ? N2 Si1 C13 105.67(8) . . ? N1 Si1 C13 119.78(9) . . ? N2 Si1 C22 120.72(8) . . ? N1 Si1 C22 106.39(8) . . ? C13 Si1 C22 112.99(8) . . ? C1 N1 C5 119.19(17) . . ? C1 N1 Si1 129.83(15) . . ? C5 N1 Si1 110.90(14) . . ? C6 N2 C12 111.85(17) . . ? C6 N2 Si1 111.36(14) . . ? C12 N2 Si1 134.94(14) . . ? C2 C1 N1 122.5(2) . . ? C1 C2 C3 119.3(2) . . ? C4 C3 C2 120.2(2) . . ? C3 C4 C5 120.8(2) . . ? C6 C5 C4 131.1(2) . . ? C6 C5 N1 111.73(17) . . ? C4 C5 N1 117.16(19) . . ? C5 C6 N2 114.89(19) . . ? C5 C6 C7 134.9(2) . . ? N2 C6 C7 110.1(2) . . ? C6 C7 C8 106.01(19) . . ? C7 C8 C9 115.2(2) . . ? C7 C8 C12 106.15(18) . . ? C9 C8 C12 105.37(19) . . ? C10 C9 C8 104.59(19) . . ? C9 C10 C11 102.2(2) . . ? C10 C11 C12 104.40(17) . . ? N2 C12 C11 112.80(16) . . ? N2 C12 C8 105.83(17) . . ? C11 C12 C8 105.12(17) . . ? C18 C13 C14 118.38(18) . . ? C18 C13 Si1 118.64(14) . . ? C14 C13 Si1 122.72(15) . . ? C15 C14 C13 119.6(2) . . ? C15 C14 C19 117.3(2) . . ? C13 C14 C19 123.0(2) . . ? C14 C15 C16 122.3(2) . . ? C17 C16 C15 117.9(2) . . ? C17 C16 C20 121.2(2) . . ? C15 C16 C20 120.9(2) . . ? C16 C17 C18 121.9(2) . . ? C13 C18 C17 119.86(19) . . ? C13 C18 C21 123.05(17) . . ? C17 C18 C21 117.09(19) . . ? C27 C22 C23 117.43(17) . . ? C27 C22 Si1 119.23(14) . . ? C23 C22 Si1 123.33(15) . . ? C24 C23 C22 120.10(19) . . ? C24 C23 C28 116.34(19) . . ? C22 C23 C28 123.53(18) . . ? C25 C24 C23 122.0(2) . . ? C24 C25 C26 118.22(18) . . ? C24 C25 C29 120.5(2) . . ? C26 C25 C29 121.3(2) . . ? C25 C26 C27 121.8(2) . . ? C26 C27 C22 120.19(19) . . ? C26 C27 C30 117.03(19) . . ? C22 C27 C30 122.74(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 N2 Si1 N1 C1 -167.47(19) . . . . ? C13 Si1 N1 C1 84.33(19) . . . . ? C22 Si1 N1 C1 -45.3(2) . . . . ? N2 Si1 N1 C5 9.15(14) . . . . ? C13 Si1 N1 C5 -99.05(15) . . . . ? C22 Si1 N1 C5 131.36(14) . . . . ? N1 Si1 N2 C6 -8.85(15) . . . . ? C13 Si1 N2 C6 112.24(15) . . . . ? C22 Si1 N2 C6 -118.08(14) . . . . ? N1 Si1 N2 C12 -171.60(19) . . . . ? C13 Si1 N2 C12 -50.5(2) . . . . ? C22 Si1 N2 C12 79.2(2) . . . . ? C5 N1 C1 C2 6.6(3) . . . . ? Si1 N1 C1 C2 -176.98(17) . . . . ? N1 C1 C2 C3 0.8(3) . . . . ? C1 C2 C3 C4 -4.5(4) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C3 C4 C5 C6 -173.1(2) . . . . ? C3 C4 C5 N1 6.9(3) . . . . ? C1 N1 C5 C6 169.70(19) . . . . ? Si1 N1 C5 C6 -7.3(2) . . . . ? C1 N1 C5 C4 -10.3(3) . . . . ? Si1 N1 C5 C4 172.66(15) . . . . ? C4 C5 C6 N2 -179.4(2) . . . . ? N1 C5 C6 N2 0.6(3) . . . . ? C4 C5 C6 C7 -3.7(5) . . . . ? N1 C5 C6 C7 176.3(3) . . . . ? C12 N2 C6 C5 173.41(18) . . . . ? Si1 N2 C6 C5 6.5(2) . . . . ? C12 N2 C6 C7 -3.4(3) . . . . ? Si1 N2 C6 C7 -170.29(16) . . . . ? C5 C6 C7 C8 -172.7(2) . . . . ? N2 C6 C7 C8 3.2(3) . . . . ? C6 C7 C8 C9 -118.0(2) . . . . ? C6 C7 C8 C12 -1.8(3) . . . . ? C7 C8 C9 C10 88.7(2) . . . . ? C12 C8 C9 C10 -27.9(3) . . . . ? C8 C9 C10 C11 42.1(2) . . . . ? C9 C10 C11 C12 -40.0(2) . . . . ? C6 N2 C12 C11 116.50(19) . . . . ? Si1 N2 C12 C11 -80.8(2) . . . . ? C6 N2 C12 C8 2.1(2) . . . . ? Si1 N2 C12 C8 164.77(16) . . . . ? C10 C11 C12 N2 -92.1(2) . . . . ? C10 C11 C12 C8 22.7(2) . . . . ? C7 C8 C12 N2 -0.1(2) . . . . ? C9 C8 C12 N2 122.6(2) . . . . ? C7 C8 C12 C11 -119.6(2) . . . . ? C9 C8 C12 C11 3.0(2) . . . . ? N2 Si1 C13 C18 75.03(16) . . . . ? N1 Si1 C13 C18 174.38(14) . . . . ? C22 Si1 C13 C18 -59.03(16) . . . . ? N2 Si1 C13 C14 -98.97(17) . . . . ? N1 Si1 C13 C14 0.4(2) . . . . ? C22 Si1 C13 C14 126.97(16) . . . . ? C18 C13 C14 C15 2.5(3) . . . . ? Si1 C13 C14 C15 176.47(17) . . . . ? C18 C13 C14 C19 -177.3(2) . . . . ? Si1 C13 C14 C19 -3.3(3) . . . . ? C13 C14 C15 C16 -1.7(3) . . . . ? C19 C14 C15 C16 178.1(2) . . . . ? C14 C15 C16 C17 0.0(3) . . . . ? C14 C15 C16 C20 179.2(2) . . . . ? C15 C16 C17 C18 1.0(3) . . . . ? C20 C16 C17 C18 -178.3(2) . . . . ? C14 C13 C18 C17 -1.6(3) . . . . ? Si1 C13 C18 C17 -175.82(15) . . . . ? C14 C13 C18 C21 179.03(19) . . . . ? Si1 C13 C18 C21 4.8(2) . . . . ? C16 C17 C18 C13 -0.2(3) . . . . ? C16 C17 C18 C21 179.3(2) . . . . ? N2 Si1 C22 C27 31.56(18) . . . . ? N1 Si1 C22 C27 -68.62(16) . . . . ? C13 Si1 C22 C27 157.96(14) . . . . ? N2 Si1 C22 C23 -149.77(15) . . . . ? N1 Si1 C22 C23 110.04(16) . . . . ? C13 Si1 C22 C23 -23.37(18) . . . . ? C27 C22 C23 C24 -4.8(3) . . . . ? Si1 C22 C23 C24 176.56(15) . . . . ? C27 C22 C23 C28 173.11(19) . . . . ? Si1 C22 C23 C28 -5.6(3) . . . . ? C22 C23 C24 C25 1.4(3) . . . . ? C28 C23 C24 C25 -176.7(2) . . . . ? C23 C24 C25 C26 1.4(3) . . . . ? C23 C24 C25 C29 179.0(2) . . . . ? C24 C25 C26 C27 -0.6(3) . . . . ? C29 C25 C26 C27 -178.2(2) . . . . ? C25 C26 C27 C22 -2.9(3) . . . . ? C25 C26 C27 C30 174.8(2) . . . . ? C23 C22 C27 C26 5.5(3) . . . . ? Si1 C22 C27 C26 -175.75(15) . . . . ? C23 C22 C27 C30 -172.07(19) . . . . ? Si1 C22 C27 C30 6.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.310 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.050 #===END data_sitbuma _database_code_CSD 152447 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H66 N2 Si3' _chemical_formula_weight 611.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 26.2381(15) _cell_length_b 9.2920(3) _cell_length_c 16.1808(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.905(7) _cell_angle_gamma 90.00 _cell_volume 3793.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description quader _exptl_crystal_colour colorless _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.150 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8996 _exptl_absorpt_correction_T_max 0.9822 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _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 14144 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.95 _reflns_number_total 6894 _reflns_number_gt 5698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1997)' _computing_cell_refinement 'IPDS (Stoe, 1997)' _computing_data_reduction 'XRED (Stoe, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _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^)+(0.0459P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(9) _refine_ls_number_reflns 6894 _refine_ls_number_parameters 370 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 Si2 Si 0.61153(2) 0.18658(7) 0.77980(4) 0.02349(15) Uani 1 1 d . . . Si1 Si 0.84955(2) 0.14152(7) 0.75868(4) 0.02224(15) Uani 1 1 d . . . Si3 Si 0.65968(2) 0.39529(7) 0.75367(4) 0.02246(15) Uani 1 1 d . . . C4 C 0.69248(8) 0.2320(3) 0.71226(14) 0.0205(5) Uani 1 1 d . . . N1 N 0.78813(6) 0.1562(2) 0.78311(11) 0.0217(4) Uani 1 1 d . . . C3 C 0.67479(8) 0.1011(3) 0.76134(15) 0.0217(5) Uani 1 1 d . . . C1 C 0.76970(9) 0.0749(3) 0.84185(15) 0.0270(6) Uani 1 1 d . . . H1 H 0.7954 0.0330 0.8888 0.032 Uiso 1 1 calc R . . C5 C 0.74965(8) 0.2232(3) 0.71320(14) 0.0202(5) Uani 1 1 d . . . C6 C 0.77142(8) 0.2716(3) 0.65243(14) 0.0214(5) Uani 1 1 d . . . N2 N 0.82663(7) 0.2466(2) 0.66633(12) 0.0242(4) Uani 1 1 d . . . C13 C 0.90558(10) 0.2288(3) 0.84477(16) 0.0341(7) Uani 1 1 d . . . C12 C 0.84129(10) 0.2673(3) 0.58519(16) 0.0333(6) Uani 1 1 d . . . H12 H 0.8493 0.1727 0.5621 0.040 Uiso 1 1 calc R . . C2 C 0.71899(9) 0.0522(3) 0.83671(16) 0.0264(6) Uani 1 1 d . . . H2 H 0.7102 0.0030 0.8825 0.032 Uiso 1 1 calc R . . C33 C 0.71064(11) 0.5034(3) 0.84241(19) 0.0371(7) Uani 1 1 d . . . C25 C 0.55423(10) 0.1086(3) 0.6854(2) 0.0390(7) Uani 1 1 d . . . C29 C 0.61883(11) 0.5279(3) 0.66661(19) 0.0387(7) Uani 1 1 d . . . C11 C 0.88665(10) 0.3718(4) 0.59207(19) 0.0472(8) Uani 1 1 d . . . H11A H 0.9110 0.3713 0.6508 0.057 Uiso 1 1 calc R . . H11B H 0.9069 0.3468 0.5506 0.057 Uiso 1 1 calc R . . C18 C 0.80847(11) -0.1083(4) 0.6739(2) 0.0482(8) Uani 1 1 d . . . H18A H 0.7964 -0.0468 0.6231 0.072 Uiso 1 1 calc R . . H18B H 0.7821 -0.1069 0.7067 0.072 Uiso 1 1 calc R . . H18C H 0.8130 -0.2071 0.6559 0.072 Uiso 1 1 calc R . . C8 C 0.79263(9) 0.3388(3) 0.52212(15) 0.0267(5) Uani 1 1 d . . . H8 H 0.7790 0.2759 0.4706 0.032 Uiso 1 1 calc R . . C10 C 0.86025(12) 0.5166(4) 0.5712(2) 0.0550(9) Uani 1 1 d . . . H10A H 0.8841 0.5867 0.5545 0.066 Uiso 1 1 calc R . . H10B H 0.8490 0.5553 0.6204 0.066 Uiso 1 1 calc R . . C7 C 0.75021(9) 0.3544(3) 0.57109(15) 0.0269(6) Uani 1 1 d . . . H7A H 0.7450 0.4568 0.5835 0.032 Uiso 1 1 calc R . . H7B H 0.7159 0.3139 0.5372 0.032 Uiso 1 1 calc R . . C30 C 0.59837(12) 0.4537(4) 0.57935(19) 0.0511(8) Uani 1 1 d . . . H30A H 0.6285 0.4241 0.5584 0.077 Uiso 1 1 calc R . . H30B H 0.5760 0.5207 0.5383 0.077 Uiso 1 1 calc R . . H30C H 0.5776 0.3688 0.5855 0.077 Uiso 1 1 calc R . . C21 C 0.59556(11) 0.1572(4) 0.88852(19) 0.0447(8) Uani 1 1 d . . . C15 C 0.96053(9) 0.1931(4) 0.8326(2) 0.0496(8) Uani 1 1 d . . . H15A H 0.9660 0.0887 0.8361 0.074 Uiso 1 1 calc R . . H15B H 0.9881 0.2403 0.8778 0.074 Uiso 1 1 calc R . . H15C H 0.9623 0.2275 0.7763 0.074 Uiso 1 1 calc R . . C20 C 0.87933(13) -0.1519(4) 0.8099(2) 0.0501(8) Uani 1 1 d . . . H20A H 0.9132 -0.1181 0.8475 0.075 Uiso 1 1 calc R . . H20B H 0.8835 -0.2502 0.7908 0.075 Uiso 1 1 calc R . . H20C H 0.8524 -0.1509 0.8415 0.075 Uiso 1 1 calc R . . C9 C 0.81229(10) 0.4813(3) 0.49522(19) 0.0396(7) Uani 1 1 d . . . H9A H 0.7848 0.5570 0.4873 0.047 Uiso 1 1 calc R . . H9B H 0.8228 0.4706 0.4413 0.047 Uiso 1 1 calc R . . C26 C 0.57212(11) 0.0746(4) 0.6035(2) 0.0488(8) Uani 1 1 d . . . H26A H 0.5836 0.1635 0.5815 0.073 Uiso 1 1 calc R . . H26B H 0.5424 0.0328 0.5596 0.073 Uiso 1 1 calc R . . H26C H 0.6016 0.0059 0.6179 0.073 Uiso 1 1 calc R . . C34 C 0.68396(13) 0.6225(4) 0.8826(2) 0.0542(9) Uani 1 1 d . . . H34A H 0.6628 0.6845 0.8370 0.081 Uiso 1 1 calc R . . H34B H 0.7113 0.6801 0.9223 0.081 Uiso 1 1 calc R . . H34C H 0.6609 0.5783 0.9140 0.081 Uiso 1 1 calc R . . C36 C 0.74337(13) 0.4087(4) 0.9158(2) 0.0545(9) Uani 1 1 d . . . H36A H 0.7611 0.3327 0.8920 0.082 Uiso 1 1 calc R . . H36B H 0.7199 0.3650 0.9466 0.082 Uiso 1 1 calc R . . H36C H 0.7700 0.4679 0.9556 0.082 Uiso 1 1 calc R . . C14 C 0.89777(12) 0.3911(4) 0.8401(2) 0.0497(8) Uani 1 1 d . . . H14A H 0.8989 0.4257 0.7834 0.075 Uiso 1 1 calc R . . H14B H 0.9260 0.4374 0.8846 0.075 Uiso 1 1 calc R . . H14C H 0.8633 0.4149 0.8492 0.075 Uiso 1 1 calc R . . C23 C 0.63779(16) 0.2338(5) 0.9595(2) 0.0675(11) Uani 1 1 d . . . H23A H 0.6729 0.1957 0.9611 0.101 Uiso 1 1 calc R . . H23B H 0.6306 0.2174 1.0150 0.101 Uiso 1 1 calc R . . H23C H 0.6368 0.3373 0.9475 0.101 Uiso 1 1 calc R . . C35 C 0.75156(12) 0.5728(4) 0.8014(2) 0.0541(9) Uani 1 1 d . . . H35A H 0.7331 0.6350 0.7536 0.081 Uiso 1 1 calc R . . H35B H 0.7706 0.4971 0.7799 0.081 Uiso 1 1 calc R . . H35C H 0.7768 0.6302 0.8447 0.081 Uiso 1 1 calc R . . C17 C 0.86187(9) -0.0517(3) 0.73085(16) 0.0309(6) Uani 1 1 d . . . C27 C 0.50490(10) 0.2068(4) 0.6593(2) 0.0552(9) Uani 1 1 d . . . H27A H 0.5149 0.3005 0.6407 0.083 Uiso 1 1 calc R . . H27B H 0.4905 0.2202 0.7086 0.083 Uiso 1 1 calc R . . H27C H 0.4780 0.1621 0.6120 0.083 Uiso 1 1 calc R . . C16 C 0.90353(12) 0.1775(5) 0.93449(17) 0.0562(9) Uani 1 1 d . . . H16A H 0.9086 0.0730 0.9388 0.084 Uiso 1 1 calc R . . H16B H 0.8690 0.2021 0.9431 0.084 Uiso 1 1 calc R . . H16C H 0.9317 0.2249 0.9786 0.084 Uiso 1 1 calc R . . C31 C 0.57041(12) 0.5742(4) 0.6974(2) 0.0529(9) Uani 1 1 d . . . H31A H 0.5827 0.6216 0.7535 0.079 Uiso 1 1 calc R . . H31B H 0.5494 0.4891 0.7026 0.079 Uiso 1 1 calc R . . H31C H 0.5485 0.6411 0.6557 0.079 Uiso 1 1 calc R . . C28 C 0.53714(14) -0.0376(4) 0.7136(3) 0.0634(10) Uani 1 1 d . . . H28A H 0.5251 -0.0246 0.7653 0.095 Uiso 1 1 calc R . . H28B H 0.5673 -0.1041 0.7261 0.095 Uiso 1 1 calc R . . H28C H 0.5082 -0.0772 0.6674 0.095 Uiso 1 1 calc R . . C24 C 0.59899(15) -0.0044(5) 0.9172(3) 0.0701(11) Uani 1 1 d . . . H24A H 0.6342 -0.0423 0.9197 0.105 Uiso 1 1 calc R . . H24B H 0.5720 -0.0603 0.8757 0.105 Uiso 1 1 calc R . . H24C H 0.5928 -0.0116 0.9741 0.105 Uiso 1 1 calc R . . C32 C 0.64703(14) 0.6657(4) 0.6503(2) 0.0596(9) Uani 1 1 d . . . H32A H 0.6609 0.7175 0.7045 0.089 Uiso 1 1 calc R . . H32B H 0.6218 0.7272 0.6095 0.089 Uiso 1 1 calc R . . H32C H 0.6763 0.6402 0.6263 0.089 Uiso 1 1 calc R . . C19 C 0.90305(13) -0.0632(4) 0.6792(2) 0.0540(9) Uani 1 1 d . . . H19A H 0.9373 -0.0271 0.7141 0.081 Uiso 1 1 calc R . . H19B H 0.8913 -0.0056 0.6267 0.081 Uiso 1 1 calc R . . H19C H 0.9067 -0.1640 0.6641 0.081 Uiso 1 1 calc R . . C22 C 0.54061(15) 0.2157(6) 0.8854(3) 0.0849(15) Uani 1 1 d . . . H22A H 0.5138 0.1656 0.8403 0.127 Uiso 1 1 calc R . . H22B H 0.5393 0.3190 0.8728 0.127 Uiso 1 1 calc R . . H22C H 0.5334 0.1998 0.9410 0.127 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si2 0.0206(3) 0.0218(4) 0.0309(3) 0.0029(3) 0.0120(2) 0.0017(2) Si1 0.0157(3) 0.0277(4) 0.0225(3) 0.0011(3) 0.0038(2) 0.0010(2) Si3 0.0259(3) 0.0167(4) 0.0278(3) 0.0008(3) 0.0124(3) 0.0016(3) C4 0.0187(11) 0.0214(15) 0.0220(11) 0.0004(9) 0.0069(9) 0.0014(8) N1 0.0151(8) 0.0284(14) 0.0203(9) 0.0032(8) 0.0026(7) 0.0017(8) C3 0.0193(10) 0.0192(16) 0.0273(12) 0.0030(9) 0.0073(9) 0.0024(8) C1 0.0239(12) 0.0332(17) 0.0233(12) 0.0091(10) 0.0052(9) 0.0062(10) C5 0.0191(10) 0.0190(15) 0.0221(11) -0.0003(9) 0.0051(8) 0.0027(8) C6 0.0184(11) 0.0208(15) 0.0248(12) 0.0004(9) 0.0058(9) 0.0020(9) N2 0.0203(9) 0.0289(13) 0.0265(10) 0.0023(9) 0.0120(8) 0.0034(8) C13 0.0253(12) 0.046(2) 0.0270(13) -0.0045(11) 0.0009(10) -0.0080(11) C12 0.0310(13) 0.0407(18) 0.0316(13) 0.0097(12) 0.0145(11) 0.0087(11) C2 0.0276(12) 0.0243(16) 0.0288(13) 0.0082(10) 0.0105(10) 0.0036(10) C33 0.0410(15) 0.0274(19) 0.0435(16) -0.0139(12) 0.0127(12) -0.0081(11) C25 0.0198(12) 0.0316(19) 0.0634(19) -0.0098(13) 0.0077(12) -0.0001(10) C29 0.0431(15) 0.0287(19) 0.0499(18) 0.0153(13) 0.0224(13) 0.0148(12) C11 0.0269(13) 0.076(3) 0.0393(15) 0.0083(16) 0.0106(11) -0.0047(14) C18 0.0442(16) 0.0328(19) 0.0586(18) -0.0144(16) -0.0011(13) 0.0034(14) C8 0.0294(12) 0.0301(16) 0.0229(12) 0.0027(10) 0.0112(10) 0.0022(10) C10 0.0500(18) 0.043(2) 0.074(2) -0.0112(17) 0.0200(17) -0.0160(15) C7 0.0265(11) 0.0307(17) 0.0253(12) 0.0051(10) 0.0102(9) 0.0058(9) C30 0.0504(17) 0.059(2) 0.0421(17) 0.0203(15) 0.0089(14) 0.0235(15) C21 0.0475(15) 0.049(2) 0.0490(16) 0.0167(15) 0.0317(13) 0.0042(14) C15 0.0179(12) 0.067(2) 0.0571(18) 0.0000(17) -0.0018(11) -0.0050(13) C20 0.0537(18) 0.034(2) 0.0552(19) 0.0121(14) 0.0016(15) 0.0068(13) C9 0.0335(14) 0.039(2) 0.0476(17) 0.0161(13) 0.0139(12) -0.0007(12) C26 0.0336(15) 0.058(2) 0.0478(18) -0.0179(16) -0.0013(13) 0.0020(13) C34 0.0626(19) 0.041(2) 0.062(2) -0.0270(16) 0.0207(16) -0.0077(15) C36 0.0537(18) 0.053(2) 0.0471(17) -0.0185(17) -0.0024(14) -0.0056(16) C14 0.0442(16) 0.049(2) 0.0516(18) -0.0186(16) 0.0057(13) -0.0117(15) C23 0.094(3) 0.082(3) 0.0372(17) 0.0028(17) 0.0355(18) 0.006(2) C35 0.0460(17) 0.048(2) 0.071(2) -0.0141(17) 0.0207(16) -0.0196(15) C17 0.0277(12) 0.0283(17) 0.0355(14) 0.0010(11) 0.0070(11) 0.0083(10) C27 0.0249(13) 0.060(3) 0.073(2) -0.0184(18) 0.0003(13) 0.0109(14) C16 0.0527(17) 0.079(3) 0.0267(14) -0.0035(16) -0.0063(12) -0.0210(18) C31 0.0471(17) 0.045(2) 0.072(2) 0.0141(17) 0.0238(16) 0.0265(15) C28 0.0473(18) 0.040(2) 0.102(3) -0.011(2) 0.0184(19) -0.0155(15) C24 0.073(2) 0.073(3) 0.073(2) 0.032(2) 0.034(2) -0.006(2) C32 0.074(2) 0.037(2) 0.076(2) 0.0303(17) 0.0352(18) 0.0150(16) C19 0.0548(18) 0.049(3) 0.066(2) -0.0013(16) 0.0298(16) 0.0218(15) C22 0.074(2) 0.125(4) 0.079(3) 0.019(3) 0.060(2) 0.026(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 Si2 C3 1.936(2) . ? Si2 C21 1.936(3) . ? Si2 C25 1.965(3) . ? Si2 Si3 2.4142(9) . ? Si1 N2 1.748(2) . ? Si1 N1 1.7666(17) . ? Si1 C17 1.900(3) . ? Si1 C13 1.907(2) . ? Si3 C33 1.951(3) . ? Si3 C4 1.952(2) . ? Si3 C29 1.956(3) . ? C4 C5 1.498(3) . ? C4 C3 1.590(3) . ? N1 C1 1.400(3) . ? N1 C5 1.435(3) . ? C3 C2 1.505(3) . ? C1 C2 1.327(3) . ? C5 C6 1.343(3) . ? C6 N2 1.423(3) . ? C6 C7 1.494(3) . ? N2 C12 1.478(3) . ? C13 C14 1.521(5) . ? C13 C15 1.543(4) . ? C13 C16 1.543(4) . ? C12 C11 1.516(4) . ? C12 C8 1.549(3) . ? C33 C36 1.537(5) . ? C33 C34 1.544(4) . ? C33 C35 1.549(4) . ? C25 C28 1.538(5) . ? C25 C27 1.545(4) . ? C25 C26 1.554(4) . ? C29 C30 1.530(5) . ? C29 C32 1.538(4) . ? C29 C31 1.547(4) . ? C11 C10 1.509(5) . ? C18 C17 1.543(4) . ? C8 C9 1.527(4) . ? C8 C7 1.540(3) . ? C10 C9 1.534(4) . ? C21 C22 1.529(4) . ? C21 C23 1.534(5) . ? C21 C24 1.567(5) . ? C20 C17 1.546(4) . ? C17 C19 1.540(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Si2 C21 119.37(12) . . ? C3 Si2 C25 103.56(11) . . ? C21 Si2 C25 110.14(13) . . ? C3 Si2 Si3 77.92(8) . . ? C21 Si2 Si3 121.75(11) . . ? C25 Si2 Si3 119.07(10) . . ? N2 Si1 N1 91.54(9) . . ? N2 Si1 C17 111.47(11) . . ? N1 Si1 C17 110.54(11) . . ? N2 Si1 C13 113.74(12) . . ? N1 Si1 C13 111.81(11) . . ? C17 Si1 C13 115.33(12) . . ? C33 Si3 C4 112.05(11) . . ? C33 Si3 C29 109.60(14) . . ? C4 Si3 C29 116.68(11) . . ? C33 Si3 Si2 124.80(10) . . ? C4 Si3 Si2 74.73(7) . . ? C29 Si3 Si2 115.00(9) . . ? C5 C4 C3 112.45(18) . . ? C5 C4 Si3 124.99(17) . . ? C3 C4 Si3 101.94(14) . . ? C1 N1 C5 118.02(17) . . ? C1 N1 Si1 128.04(16) . . ? C5 N1 Si1 110.18(14) . . ? C2 C3 C4 111.74(18) . . ? C2 C3 Si2 120.13(17) . . ? C4 C3 Si2 98.23(14) . . ? C2 C1 N1 124.8(2) . . ? C6 C5 N1 111.95(18) . . ? C6 C5 C4 126.9(2) . . ? N1 C5 C4 121.18(19) . . ? C5 C6 N2 116.6(2) . . ? C5 C6 C7 133.4(2) . . ? N2 C6 C7 109.92(18) . . ? C6 N2 C12 109.86(18) . . ? C6 N2 Si1 108.86(14) . . ? C12 N2 Si1 136.03(16) . . ? C14 C13 C15 109.0(2) . . ? C14 C13 C16 108.3(3) . . ? C15 C13 C16 109.1(2) . . ? C14 C13 Si1 108.58(18) . . ? C15 C13 Si1 112.05(19) . . ? C16 C13 Si1 109.71(19) . . ? N2 C12 C11 114.1(2) . . ? N2 C12 C8 105.83(18) . . ? C11 C12 C8 105.2(2) . . ? C1 C2 C3 122.6(2) . . ? C36 C33 C34 107.9(3) . . ? C36 C33 C35 105.3(3) . . ? C34 C33 C35 109.2(3) . . ? C36 C33 Si3 113.5(2) . . ? C34 C33 Si3 112.4(2) . . ? C35 C33 Si3 108.3(2) . . ? C28 C25 C27 108.2(3) . . ? C28 C25 C26 104.7(3) . . ? C27 C25 C26 108.2(3) . . ? C28 C25 Si2 108.6(2) . . ? C27 C25 Si2 113.6(2) . . ? C26 C25 Si2 113.09(17) . . ? C30 C29 C32 106.3(3) . . ? C30 C29 C31 108.1(3) . . ? C32 C29 C31 107.5(3) . . ? C30 C29 Si3 111.4(2) . . ? C32 C29 Si3 117.0(2) . . ? C31 C29 Si3 106.21(19) . . ? C10 C11 C12 104.6(2) . . ? C9 C8 C7 114.4(2) . . ? C9 C8 C12 106.1(2) . . ? C7 C8 C12 106.43(19) . . ? C11 C10 C9 102.4(3) . . ? C6 C7 C8 104.93(19) . . ? C22 C21 C23 110.0(3) . . ? C22 C21 C24 109.1(3) . . ? C23 C21 C24 104.6(3) . . ? C22 C21 Si2 110.9(2) . . ? C23 C21 Si2 108.82(19) . . ? C24 C21 Si2 113.3(2) . . ? C8 C9 C10 102.9(2) . . ? C19 C17 C18 108.1(2) . . ? C19 C17 C20 108.3(2) . . ? C18 C17 C20 107.7(3) . . ? C19 C17 Si1 112.6(2) . . ? C18 C17 Si1 106.12(18) . . ? C20 C17 Si1 113.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Si2 Si3 C33 -90.05(13) . . . . ? C21 Si2 Si3 C33 27.17(16) . . . . ? C25 Si2 Si3 C33 171.01(14) . . . . ? C3 Si2 Si3 C4 16.45(10) . . . . ? C21 Si2 Si3 C4 133.68(13) . . . . ? C25 Si2 Si3 C4 -82.48(12) . . . . ? C3 Si2 Si3 C29 129.17(12) . . . . ? C21 Si2 Si3 C29 -113.61(15) . . . . ? C25 Si2 Si3 C29 30.23(14) . . . . ? C33 Si3 C4 C5 -26.9(2) . . . . ? C29 Si3 C4 C5 100.5(2) . . . . ? Si2 Si3 C4 C5 -148.80(19) . . . . ? C33 Si3 C4 C3 101.68(16) . . . . ? C29 Si3 C4 C3 -130.84(15) . . . . ? Si2 Si3 C4 C3 -20.17(12) . . . . ? N2 Si1 N1 C1 165.8(2) . . . . ? C17 Si1 N1 C1 52.2(2) . . . . ? C13 Si1 N1 C1 -77.8(2) . . . . ? N2 Si1 N1 C5 8.45(17) . . . . ? C17 Si1 N1 C5 -105.20(18) . . . . ? C13 Si1 N1 C5 124.85(18) . . . . ? C5 C4 C3 C2 33.8(3) . . . . ? Si3 C4 C3 C2 -102.35(18) . . . . ? C5 C4 C3 Si2 160.95(15) . . . . ? Si3 C4 C3 Si2 24.78(14) . . . . ? C21 Si2 C3 C2 -18.5(2) . . . . ? C25 Si2 C3 C2 -141.4(2) . . . . ? Si3 Si2 C3 C2 101.29(19) . . . . ? C21 Si2 C3 C4 -139.62(16) . . . . ? C25 Si2 C3 C4 97.54(16) . . . . ? Si3 Si2 C3 C4 -19.82(12) . . . . ? C5 N1 C1 C2 1.6(4) . . . . ? Si1 N1 C1 C2 -154.2(2) . . . . ? C1 N1 C5 C6 -167.0(2) . . . . ? Si1 N1 C5 C6 -7.0(3) . . . . ? C1 N1 C5 C4 12.2(3) . . . . ? Si1 N1 C5 C4 172.17(17) . . . . ? C3 C4 C5 C6 149.0(2) . . . . ? Si3 C4 C5 C6 -86.8(3) . . . . ? C3 C4 C5 N1 -30.1(3) . . . . ? Si3 C4 C5 N1 94.2(3) . . . . ? N1 C5 C6 N2 1.2(3) . . . . ? C4 C5 C6 N2 -177.9(2) . . . . ? N1 C5 C6 C7 -176.1(3) . . . . ? C4 C5 C6 C7 4.8(5) . . . . ? C5 C6 N2 C12 164.0(2) . . . . ? C7 C6 N2 C12 -18.1(3) . . . . ? C5 C6 N2 Si1 5.2(3) . . . . ? C7 C6 N2 Si1 -176.87(18) . . . . ? N1 Si1 N2 C6 -7.64(17) . . . . ? C17 Si1 N2 C6 105.18(17) . . . . ? C13 Si1 N2 C6 -122.35(17) . . . . ? N1 Si1 N2 C12 -158.2(3) . . . . ? C17 Si1 N2 C12 -45.4(3) . . . . ? C13 Si1 N2 C12 87.0(3) . . . . ? N2 Si1 C13 C14 32.1(2) . . . . ? N1 Si1 C13 C14 -69.9(2) . . . . ? C17 Si1 C13 C14 162.68(19) . . . . ? N2 Si1 C13 C15 -88.3(2) . . . . ? N1 Si1 C13 C15 169.7(2) . . . . ? C17 Si1 C13 C15 42.3(3) . . . . ? N2 Si1 C13 C16 150.3(2) . . . . ? N1 Si1 C13 C16 48.3(3) . . . . ? C17 Si1 C13 C16 -79.1(2) . . . . ? C6 N2 C12 C11 126.7(2) . . . . ? Si1 N2 C12 C11 -82.9(3) . . . . ? C6 N2 C12 C8 11.5(3) . . . . ? Si1 N2 C12 C8 161.9(2) . . . . ? N1 C1 C2 C3 5.8(4) . . . . ? C4 C3 C2 C1 -23.9(3) . . . . ? Si2 C3 C2 C1 -138.0(2) . . . . ? C4 Si3 C33 C36 -51.0(2) . . . . ? C29 Si3 C33 C36 177.9(2) . . . . ? Si2 Si3 C33 C36 35.3(2) . . . . ? C4 Si3 C33 C34 -173.7(2) . . . . ? C29 Si3 C33 C34 55.1(3) . . . . ? Si2 Si3 C33 C34 -87.4(2) . . . . ? C4 Si3 C33 C35 65.5(2) . . . . ? C29 Si3 C33 C35 -65.6(2) . . . . ? Si2 Si3 C33 C35 151.85(19) . . . . ? C3 Si2 C25 C28 86.3(2) . . . . ? C21 Si2 C25 C28 -42.4(2) . . . . ? Si3 Si2 C25 C28 169.87(18) . . . . ? C3 Si2 C25 C27 -153.3(2) . . . . ? C21 Si2 C25 C27 78.0(3) . . . . ? Si3 Si2 C25 C27 -69.7(2) . . . . ? C3 Si2 C25 C26 -29.4(2) . . . . ? C21 Si2 C25 C26 -158.2(2) . . . . ? Si3 Si2 C25 C26 54.1(2) . . . . ? C33 Si3 C29 C30 153.5(2) . . . . ? C4 Si3 C29 C30 24.9(2) . . . . ? Si2 Si3 C29 C30 -59.9(2) . . . . ? C33 Si3 C29 C32 31.0(3) . . . . ? C4 Si3 C29 C32 -97.7(2) . . . . ? Si2 Si3 C29 C32 177.5(2) . . . . ? C33 Si3 C29 C31 -89.0(2) . . . . ? C4 Si3 C29 C31 142.4(2) . . . . ? Si2 Si3 C29 C31 57.6(2) . . . . ? N2 C12 C11 C10 -89.8(3) . . . . ? C8 C12 C11 C10 25.7(3) . . . . ? N2 C12 C8 C9 121.3(2) . . . . ? C11 C12 C8 C9 0.2(3) . . . . ? N2 C12 C8 C7 -0.9(3) . . . . ? C11 C12 C8 C7 -122.1(2) . . . . ? C12 C11 C10 C9 -41.8(3) . . . . ? C5 C6 C7 C8 -165.8(3) . . . . ? N2 C6 C7 C8 16.7(3) . . . . ? C9 C8 C7 C6 -126.0(2) . . . . ? C12 C8 C7 C6 -9.2(3) . . . . ? C3 Si2 C21 C22 -172.2(3) . . . . ? C25 Si2 C21 C22 -52.7(3) . . . . ? Si3 Si2 C21 C22 94.0(3) . . . . ? C3 Si2 C21 C23 66.7(3) . . . . ? C25 Si2 C21 C23 -173.8(2) . . . . ? Si3 Si2 C21 C23 -27.1(3) . . . . ? C3 Si2 C21 C24 -49.2(3) . . . . ? C25 Si2 C21 C24 70.4(3) . . . . ? Si3 Si2 C21 C24 -142.9(2) . . . . ? C7 C8 C9 C10 91.6(3) . . . . ? C12 C8 C9 C10 -25.4(3) . . . . ? C11 C10 C9 C8 41.3(3) . . . . ? N2 Si1 C17 C19 59.4(2) . . . . ? N1 Si1 C17 C19 159.65(19) . . . . ? C13 Si1 C17 C19 -72.3(2) . . . . ? N2 Si1 C17 C18 -58.7(2) . . . . ? N1 Si1 C17 C18 41.6(2) . . . . ? C13 Si1 C17 C18 169.67(19) . . . . ? N2 Si1 C17 C20 -176.86(18) . . . . ? N1 Si1 C17 C20 -76.6(2) . . . . ? C13 Si1 C17 C20 51.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.439 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.044 #===END data_sitimema _database_code_CSD 152448 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 N2 Si' _chemical_formula_weight 536.85 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.7011(5) _cell_length_b 11.7040(8) _cell_length_c 14.5936(10) _cell_angle_alpha 96.862(8) _cell_angle_beta 100.249(7) _cell_angle_gamma 100.163(7) _cell_volume 1585.37(17) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description quader _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9424 _exptl_absorpt_correction_T_max 0.9832 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _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 19376 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.1461 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.91 _reflns_number_total 11412 _reflns_number_gt 5634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1999)' _computing_cell_refinement 'IPDS (Stoe, 1999)' _computing_data_reduction 'XRED (Stoe, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _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^)+(0.0330P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(2) _refine_ls_number_reflns 11412 _refine_ls_number_parameters 703 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 0.792 _refine_ls_restrained_S_all 0.792 _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 -0.08429(17) -0.27580(13) -0.87670(10) 0.0302(4) Uani 1 1 d . . . N1 N -0.0337(6) -0.4121(5) -0.8832(3) 0.0331(14) Uani 1 1 d . . . N2 N -0.2150(6) -0.3270(5) -0.8159(4) 0.0362(14) Uani 1 1 d . . . C1 C 0.0765(8) -0.4500(6) -0.9205(5) 0.0417(17) Uani 1 1 d . . . H1 H 0.1400 -0.3943 -0.9436 0.050 Uiso 1 1 calc R . . C2 C 0.0983(9) -0.5625(6) -0.9256(5) 0.046(2) Uani 1 1 d . . . H2 H 0.1713 -0.5850 -0.9550 0.056 Uiso 1 1 calc R . . C3 C 0.0096(8) -0.6461(6) -0.8860(4) 0.0439(19) Uani 1 1 d . . . H3 H 0.0246 -0.7244 -0.8883 0.053 Uiso 1 1 calc R . . C4 C -0.0959(8) -0.6140(6) -0.8452(5) 0.044(2) Uani 1 1 d . . . H4 H -0.1521 -0.6697 -0.8174 0.053 Uiso 1 1 calc R . . C5 C -0.1241(8) -0.4972(6) -0.8431(4) 0.0338(16) Uani 1 1 d . . . C6 C -0.2205(7) -0.4466(6) -0.8076(4) 0.0372(17) Uani 1 1 d . . . C7 C -0.3467(8) -0.4918(6) -0.7661(5) 0.0535(19) Uani 1 1 d . . . H7A H -0.3202 -0.4821 -0.6965 0.064 Uiso 1 1 calc R . . H7B H -0.3870 -0.5757 -0.7913 0.064 Uiso 1 1 calc R . . C8 C -0.4542(5) -0.4129(4) -0.7985(3) 0.0534(13) Uani 1 1 d . . . H8 H -0.5199 -0.4506 -0.8595 0.064 Uiso 1 1 calc R . . C9 C -0.5380(8) -0.3738(6) -0.7265(5) 0.062(2) Uani 1 1 d . . . H9A H -0.6414 -0.4071 -0.7490 0.074 Uiso 1 1 calc R . . H9B H -0.5056 -0.4003 -0.6658 0.074 Uiso 1 1 calc R . . C10 C -0.5110(7) -0.2437(6) -0.7146(5) 0.0808(19) Uani 1 1 d . . . H10A H -0.5203 -0.2102 -0.6510 0.097 Uiso 1 1 calc R . . H10B H -0.5787 -0.2167 -0.7623 0.097 Uiso 1 1 calc R . . C11 C -0.3620(7) -0.2093(5) -0.7279(5) 0.088(2) Uani 1 1 d . . . H11A H -0.2923 -0.2153 -0.6711 0.106 Uiso 1 1 calc R . . H11B H -0.3428 -0.1281 -0.7420 0.106 Uiso 1 1 calc R . . C12 C -0.3555(7) -0.2970(5) -0.8109(4) 0.0555(16) Uani 1 1 d . . . H12 H -0.3956 -0.2708 -0.8709 0.067 Uiso 1 1 calc R . . C13 C -0.1865(7) -0.2265(5) -0.9808(4) 0.0333(16) Uani 1 1 d . . . C14 C -0.2192(8) -0.1092(6) -0.9719(5) 0.0400(17) Uani 1 1 d . . . C15 C -0.3107(8) -0.0831(6) -1.0485(5) 0.0454(18) Uani 1 1 d . . . H15 H -0.3299 -0.0060 -1.0430 0.054 Uiso 1 1 calc R . . C16 C -0.3741(8) -0.1553(7) -1.1286(5) 0.0442(19) Uani 1 1 d . . . C17 C -0.3412(8) -0.2691(6) -1.1384(5) 0.0413(18) Uani 1 1 d . . . H17 H -0.3795 -0.3221 -1.1955 0.050 Uiso 1 1 calc R . . C18 C -0.2534(7) -0.3036(6) -1.0652(4) 0.0345(17) Uani 1 1 d . . . C19 C -0.1615(8) -0.0195(5) -0.8851(4) 0.049(2) Uani 1 1 d . . . H19A H -0.1009 -0.0524 -0.8384 0.074 Uiso 1 1 calc R . . H19B H -0.2411 0.0025 -0.8589 0.074 Uiso 1 1 calc R . . H19C H -0.1047 0.0503 -0.9014 0.074 Uiso 1 1 calc R . . C20 C -0.4728(8) -0.1250(7) -1.2090(5) 0.0573(19) Uani 1 1 d . . . H20A H -0.4823 -0.0432 -1.1945 0.086 Uiso 1 1 calc R . . H20B H -0.5669 -0.1770 -1.2189 0.086 Uiso 1 1 calc R . . H20C H -0.4338 -0.1351 -1.2663 0.086 Uiso 1 1 calc R . . C21 C -0.2271(9) -0.4271(6) -1.0811(5) 0.055(2) Uani 1 1 d . . . H21A H -0.1609 -0.4401 -1.0261 0.083 Uiso 1 1 calc R . . H21B H -0.1854 -0.4378 -1.1372 0.083 Uiso 1 1 calc R . . H21C H -0.3179 -0.4834 -1.0903 0.083 Uiso 1 1 calc R . . C22 C 0.0787(7) -0.1610(5) -0.8199(4) 0.0260(15) Uani 1 1 d . . . C23 C 0.1633(7) -0.1011(5) -0.8787(4) 0.0271(15) Uani 1 1 d . . . C24 C 0.2675(8) -0.0046(6) -0.8404(4) 0.0378(17) Uani 1 1 d . . . H24 H 0.3229 0.0320 -0.8804 0.045 Uiso 1 1 calc R . . C25 C 0.2966(8) 0.0427(6) -0.7452(5) 0.0434(18) Uani 1 1 d . . . C26 C 0.2237(8) -0.0177(6) -0.6874(4) 0.0394(16) Uani 1 1 d . . . H26 H 0.2463 0.0106 -0.6216 0.047 Uiso 1 1 calc R . . C27 C 0.1162(7) -0.1205(5) -0.7219(4) 0.0322(16) Uani 1 1 d . . . C28 C 0.1536(7) -0.1478(6) -0.9828(4) 0.0321(15) Uani 1 1 d . . . H28 H 0.0762 -0.2201 -1.0005 0.039 Uiso 1 1 calc R . . C29 C 0.1133(8) -0.0601(7) -1.0474(4) 0.051(2) Uani 1 1 d . . . H29A H 0.1064 -0.0942 -1.1131 0.076 Uiso 1 1 calc R . . H29B H 0.1867 0.0123 -1.0311 0.076 Uiso 1 1 calc R . . H29C H 0.0208 -0.0421 -1.0393 0.076 Uiso 1 1 calc R . . C30 C 0.2926(8) -0.1830(6) -0.9995(5) 0.054(2) Uani 1 1 d . . . H30A H 0.3172 -0.2397 -0.9582 0.080 Uiso 1 1 calc R . . H30B H 0.3697 -0.1131 -0.9855 0.080 Uiso 1 1 calc R . . H30C H 0.2801 -0.2187 -1.0655 0.080 Uiso 1 1 calc R . . C31 C 0.4019(9) 0.1568(7) -0.7063(5) 0.060(2) Uani 1 1 d . . . H31 H 0.4073 0.1730 -0.6368 0.072 Uiso 1 1 calc R . . C32 C 0.3585(10) 0.2606(6) -0.7492(6) 0.076(3) Uani 1 1 d . . . H32A H 0.4302 0.3321 -0.7217 0.114 Uiso 1 1 calc R . . H32B H 0.2653 0.2704 -0.7362 0.114 Uiso 1 1 calc R . . H32C H 0.3522 0.2462 -0.8176 0.114 Uiso 1 1 calc R . . C33 C 0.5520(10) 0.1459(8) -0.7230(6) 0.089(3) Uani 1 1 d . . . H33A H 0.5816 0.0803 -0.6942 0.133 Uiso 1 1 calc R . . H33B H 0.6204 0.2190 -0.6945 0.133 Uiso 1 1 calc R . . H33C H 0.5494 0.1317 -0.7909 0.133 Uiso 1 1 calc R . . C34 C 0.0522(7) -0.1855(6) -0.6524(4) 0.0371(16) Uani 1 1 d . . . H34 H -0.0481 -0.2241 -0.6843 0.045 Uiso 1 1 calc R . . C35 C 0.1302(9) -0.2820(6) -0.6308(5) 0.059(2) Uani 1 1 d . . . H35A H 0.1360 -0.3287 -0.6898 0.089 Uiso 1 1 calc R . . H35B H 0.0787 -0.3325 -0.5937 0.089 Uiso 1 1 calc R . . H35C H 0.2270 -0.2477 -0.5946 0.089 Uiso 1 1 calc R . . C36 C 0.0433(9) -0.1123(7) -0.5610(5) 0.065(2) Uani 1 1 d . . . H36A H -0.0034 -0.1634 -0.5221 0.097 Uiso 1 1 calc R . . H36B H -0.0125 -0.0522 -0.5754 0.097 Uiso 1 1 calc R . . H36C H 0.1399 -0.0743 -0.5267 0.097 Uiso 1 1 calc R . . Si2 Si -0.83672(17) -0.61269(13) -0.31575(10) 0.0286(4) Uani 1 1 d . . . N3 N -0.8804(6) -0.4713(4) -0.3033(3) 0.0314(13) Uani 1 1 d . . . N4 N -0.7137(6) -0.5649(4) -0.3827(3) 0.0336(14) Uani 1 1 d . . . C37 C -0.9824(8) -0.4316(6) -0.2609(5) 0.0438(18) Uani 1 1 d . . . H37 H -1.0361 -0.4836 -0.2289 0.053 Uiso 1 1 calc R . . C38 C -1.0096(9) -0.3262(7) -0.2622(5) 0.049(2) Uani 1 1 d . . . H38 H -1.0842 -0.3039 -0.2343 0.058 Uiso 1 1 calc R . . C39 C -0.9234(9) -0.2431(6) -0.3071(5) 0.048(2) Uani 1 1 d . . . H39 H -0.9394 -0.1654 -0.3072 0.058 Uiso 1 1 calc R . . C40 C -0.8233(7) -0.2775(5) -0.3475(4) 0.0387(17) Uani 1 1 d . . . H40 H -0.7659 -0.2222 -0.3749 0.046 Uiso 1 1 calc R . . C41 C -0.7972(7) -0.3945(5) -0.3518(4) 0.0322(16) Uani 1 1 d . . . C42 C -0.7071(7) -0.4452(5) -0.3940(4) 0.0329(16) Uani 1 1 d . . . C43 C -0.5982(8) -0.4087(6) -0.4498(5) 0.0499(19) Uani 1 1 d . . . H43A H -0.5116 -0.3575 -0.4089 0.060 Uiso 1 1 calc R . . H43B H -0.6365 -0.3656 -0.4997 0.060 Uiso 1 1 calc R . . C44 C -0.5637(5) -0.5230(4) -0.4929(3) 0.0410(11) Uani 1 1 d . . . H44 H -0.6179 -0.5470 -0.5595 0.049 Uiso 1 1 calc R . . C45 C -0.4073(9) -0.5244(8) -0.4878(6) 0.082(3) Uani 1 1 d . . . H45A H -0.3937 -0.5684 -0.5467 0.098 Uiso 1 1 calc R . . H45B H -0.3513 -0.4432 -0.4794 0.098 Uiso 1 1 calc R . . C46 C -0.3600(7) -0.5815(9) -0.4073(6) 0.127(4) Uani 1 1 d . . . H46A H -0.3094 -0.6434 -0.4276 0.153 Uiso 1 1 calc R . . H46B H -0.2918 -0.5229 -0.3580 0.153 Uiso 1 1 calc R . . C47 C -0.4770(6) -0.6328(5) -0.3686(3) 0.0566(14) Uani 1 1 d . . . H47A H -0.4678 -0.5941 -0.3031 0.068 Uiso 1 1 calc R . . H47B H -0.4788 -0.7176 -0.3681 0.068 Uiso 1 1 calc R . . C48 C -0.6143(5) -0.6156(4) -0.4308(3) 0.0350(12) Uani 1 1 d . . . H48 H -0.6648 -0.6913 -0.4718 0.042 Uiso 1 1 calc R . . C49 C -0.7288(7) -0.6686(6) -0.2139(4) 0.0290(15) Uani 1 1 d . . . C50 C -0.6997(7) -0.7800(5) -0.2270(4) 0.0359(17) Uani 1 1 d . . . C51 C -0.6136(8) -0.8212(6) -0.1557(4) 0.0409(17) Uani 1 1 d . . . H51 H -0.5964 -0.8987 -0.1650 0.049 Uiso 1 1 calc R . . C52 C -0.5526(8) -0.7452(7) -0.0697(5) 0.0434(19) Uani 1 1 d . . . C53 C -0.5747(7) -0.6356(6) -0.0594(4) 0.0404(18) Uani 1 1 d . . . H53 H -0.5289 -0.5844 -0.0025 0.048 Uiso 1 1 calc R . . C54 C -0.6632(7) -0.5919(6) -0.1291(4) 0.0356(17) Uani 1 1 d . . . C55 C -0.7615(8) -0.8686(6) -0.3185(5) 0.051(2) Uani 1 1 d . . . H55A H -0.7316 -0.9433 -0.3111 0.077 Uiso 1 1 calc R . . H55B H -0.7260 -0.8373 -0.3712 0.077 Uiso 1 1 calc R . . H55C H -0.8662 -0.8815 -0.3313 0.077 Uiso 1 1 calc R . . C56 C -0.4526(9) -0.7908(7) 0.0056(4) 0.064(2) Uani 1 1 d . . . H56A H -0.4479 -0.8720 -0.0174 0.095 Uiso 1 1 calc R . . H56B H -0.4897 -0.7883 0.0638 0.095 Uiso 1 1 calc R . . H56C H -0.3566 -0.7413 0.0180 0.095 Uiso 1 1 calc R . . C57 C -0.6807(7) -0.4649(6) -0.1098(5) 0.0455(18) Uani 1 1 d . . . H57A H -0.6272 -0.4289 -0.0465 0.068 Uiso 1 1 calc R . . H57B H -0.7823 -0.4631 -0.1141 0.068 Uiso 1 1 calc R . . H57C H -0.6440 -0.4211 -0.1566 0.068 Uiso 1 1 calc R . . C58 C -1.0067(7) -0.7266(5) -0.3672(4) 0.0283(15) Uani 1 1 d . . . C59 C -1.0536(7) -0.7631(6) -0.4667(4) 0.0333(16) Uani 1 1 d . . . C60 C -1.1623(8) -0.8586(6) -0.4998(4) 0.0409(18) Uani 1 1 d . . . H60 H -1.1910 -0.8836 -0.5659 0.049 Uiso 1 1 calc R . . C61 C -1.2327(8) -0.9205(6) -0.4399(5) 0.0396(17) Uani 1 1 d . . . C62 C -1.1963(7) -0.8798(5) -0.3450(4) 0.0347(16) Uani 1 1 d . . . H62 H -1.2467 -0.9190 -0.3038 0.042 Uiso 1 1 calc R . . C63 C -1.0864(7) -0.7814(5) -0.3073(4) 0.0303(16) Uani 1 1 d . . . C64 C -0.9912(8) -0.6939(7) -0.5395(5) 0.0444(19) Uani 1 1 d . . . H64 H -0.8894 -0.6562 -0.5109 0.053 Uiso 1 1 calc R . . C65 C -1.0738(9) -0.5956(6) -0.5595(5) 0.056(2) Uani 1 1 d . . . H65A H -1.0334 -0.5513 -0.6048 0.084 Uiso 1 1 calc R . . H65B H -1.0657 -0.5425 -0.5007 0.084 Uiso 1 1 calc R . . H65C H -1.1748 -0.6303 -0.5858 0.084 Uiso 1 1 calc R . . C66 C -0.9938(9) -0.7698(7) -0.6322(5) 0.065(2) Uani 1 1 d . . . H66A H -0.9375 -0.8302 -0.6203 0.098 Uiso 1 1 calc R . . H66B H -0.9528 -0.7206 -0.6744 0.098 Uiso 1 1 calc R . . H66C H -1.0928 -0.8075 -0.6617 0.098 Uiso 1 1 calc R . . C67 C -1.3494(9) -1.0309(7) -0.4804(5) 0.053(2) Uani 1 1 d . . . H67 H -1.3602 -1.0423 -0.5505 0.064 Uiso 1 1 calc R . . C68 C -1.3016(9) -1.1376(7) -0.4462(6) 0.078(3) Uani 1 1 d . . . H68A H -1.3762 -1.2077 -0.4723 0.118 Uiso 1 1 calc R . . H68B H -1.2844 -1.1269 -0.3772 0.118 Uiso 1 1 calc R . . H68C H -1.2131 -1.1471 -0.4671 0.118 Uiso 1 1 calc R . . C69 C -1.4926(8) -1.0172(7) -0.4586(5) 0.063(2) Uani 1 1 d . . . H69A H -1.5642 -1.0886 -0.4867 0.095 Uiso 1 1 calc R . . H69B H -1.5213 -0.9497 -0.4849 0.095 Uiso 1 1 calc R . . H69C H -1.4851 -1.0044 -0.3902 0.095 Uiso 1 1 calc R . . C70 C -1.0578(7) -0.7407(6) -0.2010(4) 0.0321(15) Uani 1 1 d . . . H70 H -0.9789 -0.6695 -0.1845 0.038 Uiso 1 1 calc R . . C71 C -1.0137(7) -0.8349(6) -0.1436(4) 0.0428(17) Uani 1 1 d . . . H71A H -0.9266 -0.8559 -0.1597 0.064 Uiso 1 1 calc R . . H71B H -1.0908 -0.9049 -0.1582 0.064 Uiso 1 1 calc R . . H71C H -0.9957 -0.8042 -0.0761 0.064 Uiso 1 1 calc R . . C72 C -1.1944(7) -0.7066(6) -0.1743(4) 0.0388(15) Uani 1 1 d . . . H72A H -1.2217 -0.6456 -0.2102 0.058 Uiso 1 1 calc R . . H72B H -1.1754 -0.6766 -0.1067 0.058 Uiso 1 1 calc R . . H72C H -1.2723 -0.7759 -0.1893 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0322(13) 0.0274(10) 0.0321(10) 0.0055(8) 0.0119(8) 0.0030(9) N1 0.031(4) 0.033(3) 0.038(3) 0.012(2) 0.013(2) 0.005(3) N2 0.032(4) 0.035(3) 0.047(3) 0.005(3) 0.021(3) 0.005(3) C1 0.042(4) 0.032(4) 0.053(4) 0.007(3) 0.014(3) 0.008(3) C2 0.053(5) 0.031(4) 0.060(5) 0.008(3) 0.014(4) 0.016(4) C3 0.056(6) 0.039(4) 0.038(4) 0.004(3) 0.009(4) 0.016(4) C4 0.063(6) 0.033(4) 0.044(4) 0.021(3) 0.012(4) 0.018(4) C5 0.038(5) 0.037(4) 0.029(3) 0.010(3) 0.012(3) 0.004(3) C6 0.038(5) 0.039(4) 0.033(3) 0.013(3) 0.011(3) -0.005(3) C7 0.057(5) 0.042(4) 0.065(4) 0.019(3) 0.025(3) -0.001(3) C8 0.047(4) 0.049(3) 0.058(3) -0.009(2) 0.016(3) -0.003(2) C9 0.050(5) 0.054(4) 0.089(5) 0.017(4) 0.041(4) -0.001(3) C10 0.043(5) 0.096(5) 0.106(5) 0.004(4) 0.039(4) 0.003(3) C11 0.064(5) 0.061(4) 0.132(6) -0.028(4) 0.044(4) -0.003(3) C12 0.062(5) 0.045(3) 0.064(4) 0.014(3) 0.030(3) 0.001(3) C13 0.034(4) 0.021(3) 0.049(4) 0.004(3) 0.018(3) 0.008(3) C14 0.041(5) 0.042(4) 0.044(4) 0.012(3) 0.025(3) 0.009(3) C15 0.045(5) 0.035(4) 0.064(5) 0.015(3) 0.017(3) 0.019(3) C16 0.035(5) 0.060(5) 0.042(4) 0.015(4) 0.013(3) 0.010(4) C17 0.045(5) 0.043(4) 0.039(4) 0.005(3) 0.011(3) 0.015(3) C18 0.034(4) 0.040(4) 0.027(3) 0.008(3) 0.010(3) -0.002(3) C19 0.065(6) 0.028(4) 0.054(4) 0.005(3) 0.002(4) 0.017(4) C20 0.046(5) 0.075(5) 0.062(4) 0.021(3) 0.018(3) 0.025(3) C21 0.084(6) 0.034(4) 0.042(4) -0.003(3) 0.003(4) 0.010(4) C22 0.026(4) 0.029(3) 0.028(3) 0.013(3) 0.012(3) 0.008(3) C23 0.027(4) 0.029(3) 0.028(3) 0.003(3) 0.008(3) 0.007(3) C24 0.047(5) 0.040(4) 0.033(4) 0.015(3) 0.021(3) 0.007(4) C25 0.045(5) 0.047(4) 0.037(4) 0.010(3) 0.006(3) 0.003(3) C26 0.043(4) 0.036(3) 0.034(3) 0.009(3) 0.010(3) -0.010(3) C27 0.030(4) 0.030(3) 0.037(3) 0.002(3) 0.005(3) 0.009(3) C28 0.032(4) 0.026(3) 0.033(3) -0.003(3) 0.011(3) -0.005(3) C29 0.067(5) 0.055(4) 0.035(4) 0.015(3) 0.013(3) 0.016(4) C30 0.058(5) 0.053(4) 0.054(4) 0.001(3) 0.036(3) 0.004(3) C31 0.061(6) 0.061(5) 0.042(4) 0.007(3) 0.007(3) -0.023(4) C32 0.102(7) 0.029(4) 0.100(6) 0.007(4) 0.051(5) -0.010(4) C33 0.059(6) 0.087(6) 0.098(7) 0.025(5) -0.030(5) -0.006(5) C34 0.033(4) 0.048(4) 0.029(3) 0.015(3) 0.010(3) -0.006(3) C35 0.088(6) 0.046(4) 0.046(4) 0.018(3) 0.015(4) 0.013(4) C36 0.082(6) 0.069(5) 0.058(4) 0.015(4) 0.039(4) 0.026(4) Si2 0.0279(12) 0.0253(10) 0.0371(11) 0.0092(8) 0.0129(8) 0.0082(9) N3 0.039(4) 0.023(3) 0.038(3) 0.007(2) 0.018(3) 0.009(3) N4 0.034(4) 0.026(3) 0.045(3) 0.012(2) 0.015(3) 0.007(3) C37 0.039(5) 0.051(4) 0.053(4) 0.022(3) 0.021(3) 0.017(3) C38 0.041(5) 0.052(5) 0.066(5) 0.012(4) 0.026(4) 0.026(4) C39 0.053(6) 0.028(4) 0.069(5) 0.017(4) 0.008(4) 0.020(4) C40 0.037(5) 0.026(4) 0.048(4) 0.010(3) 0.005(3) -0.006(3) C41 0.026(4) 0.022(3) 0.046(4) 0.012(3) 0.002(3) -0.001(3) C42 0.037(5) 0.025(3) 0.040(4) 0.014(3) 0.011(3) 0.005(3) C43 0.040(4) 0.056(4) 0.066(4) 0.026(3) 0.028(3) 0.013(3) C44 0.023(3) 0.071(3) 0.037(2) 0.023(2) 0.0159(19) 0.013(2) C45 0.084(7) 0.118(7) 0.077(5) 0.056(5) 0.042(4) 0.060(5) C46 0.052(5) 0.222(10) 0.131(6) 0.129(7) 0.019(4) 0.019(5) C47 0.042(4) 0.083(4) 0.059(3) 0.034(3) 0.014(3) 0.031(3) C48 0.027(3) 0.044(3) 0.040(3) 0.009(2) 0.017(2) 0.011(2) C49 0.020(4) 0.040(4) 0.027(3) 0.011(3) 0.008(3) 0.001(3) C50 0.034(4) 0.027(4) 0.048(4) 0.008(3) 0.005(3) 0.012(3) C51 0.050(5) 0.042(4) 0.039(3) 0.010(3) 0.014(3) 0.023(3) C52 0.035(5) 0.054(4) 0.049(4) 0.022(4) 0.011(3) 0.018(4) C53 0.037(5) 0.052(4) 0.029(3) 0.001(3) 0.003(3) 0.008(3) C54 0.033(4) 0.033(4) 0.046(4) 0.006(3) 0.015(3) 0.013(3) C55 0.043(5) 0.054(5) 0.058(4) -0.010(3) 0.012(3) 0.023(4) C56 0.094(6) 0.065(4) 0.032(3) 0.002(3) -0.008(3) 0.042(4) C57 0.037(4) 0.039(4) 0.052(4) -0.005(3) -0.004(3) 0.005(3) C58 0.026(4) 0.018(3) 0.043(4) 0.005(3) 0.009(3) 0.007(3) C59 0.019(4) 0.052(4) 0.039(3) 0.026(3) 0.017(3) 0.009(3) C60 0.045(5) 0.047(4) 0.027(3) 0.001(3) 0.003(3) 0.007(3) C61 0.035(4) 0.036(4) 0.045(4) 0.007(3) 0.015(3) -0.009(3) C62 0.032(4) 0.027(3) 0.042(4) 0.005(3) 0.014(3) -0.009(3) C63 0.036(4) 0.020(3) 0.038(4) 0.008(3) 0.013(3) 0.007(3) C64 0.027(4) 0.065(5) 0.041(4) 0.020(3) 0.002(3) 0.005(3) C65 0.078(6) 0.036(4) 0.059(5) 0.026(3) 0.024(4) 0.006(4) C66 0.076(6) 0.091(6) 0.063(5) 0.049(4) 0.054(4) 0.040(4) C67 0.050(5) 0.052(4) 0.047(4) -0.001(3) 0.021(3) -0.021(3) C68 0.049(6) 0.052(5) 0.125(7) -0.009(5) 0.035(5) -0.017(4) C69 0.043(5) 0.067(5) 0.067(4) 0.025(4) -0.004(3) -0.017(3) C70 0.035(4) 0.033(4) 0.030(3) 0.005(3) 0.013(3) 0.007(3) C71 0.034(4) 0.048(4) 0.048(4) 0.018(3) 0.013(3) 0.003(3) C72 0.036(4) 0.037(3) 0.045(3) 0.004(2) 0.014(3) 0.006(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 N2 1.736(6) . ? Si1 N1 1.747(5) . ? Si1 C13 1.870(6) . ? Si1 C22 1.874(7) . ? N1 C1 1.398(8) . ? N1 C5 1.455(9) . ? N2 C6 1.412(8) . ? N2 C12 1.478(8) . ? C1 C2 1.366(9) . ? C2 C3 1.430(11) . ? C3 C4 1.358(10) . ? C4 C5 1.440(9) . ? C5 C6 1.337(9) . ? C6 C7 1.502(10) . ? C7 C8 1.560(8) . ? C8 C9 1.514(8) . ? C8 C12 1.565(7) . ? C9 C10 1.482(9) . ? C10 C11 1.483(8) . ? C11 C12 1.509(7) . ? C13 C18 1.413(8) . ? C13 C14 1.459(8) . ? C14 C15 1.398(9) . ? C14 C19 1.498(9) . ? C15 C16 1.335(9) . ? C16 C17 1.420(9) . ? C16 C20 1.496(9) . ? C17 C18 1.390(8) . ? C18 C21 1.510(9) . ? C22 C27 1.413(7) . ? C22 C23 1.446(9) . ? C23 C24 1.362(9) . ? C23 C28 1.533(8) . ? C24 C25 1.392(8) . ? C25 C26 1.375(10) . ? C25 C31 1.510(10) . ? C26 C27 1.419(9) . ? C27 C34 1.494(9) . ? C28 C29 1.529(8) . ? C28 C30 1.529(9) . ? C31 C32 1.522(10) . ? C31 C33 1.542(12) . ? C34 C35 1.500(8) . ? C34 C36 1.521(9) . ? Si2 N4 1.732(6) . ? Si2 N3 1.776(5) . ? Si2 C58 1.899(7) . ? Si2 C49 1.912(6) . ? N3 C37 1.374(8) . ? N3 C41 1.435(8) . ? N4 C42 1.422(7) . ? N4 C48 1.455(7) . ? C37 C38 1.308(9) . ? C38 C39 1.461(11) . ? C39 C40 1.318(10) . ? C40 C41 1.432(8) . ? C41 C42 1.335(9) . ? C42 C43 1.481(9) . ? C43 C44 1.526(7) . ? C44 C45 1.509(9) . ? C44 C48 1.563(6) . ? C45 C46 1.464(8) . ? C46 C47 1.426(8) . ? C47 C48 1.532(6) . ? C49 C50 1.380(8) . ? C49 C54 1.413(8) . ? C50 C51 1.402(8) . ? C50 C55 1.544(8) . ? C51 C52 1.414(9) . ? C52 C53 1.332(9) . ? C52 C56 1.542(8) . ? C53 C54 1.415(8) . ? C54 C57 1.524(8) . ? C58 C63 1.404(9) . ? C58 C59 1.431(8) . ? C59 C60 1.367(10) . ? C59 C64 1.553(10) . ? C60 C61 1.395(10) . ? C61 C62 1.370(8) . ? C61 C67 1.538(10) . ? C62 C63 1.405(9) . ? C63 C70 1.528(8) . ? C64 C66 1.521(9) . ? C64 C65 1.540(9) . ? C67 C69 1.509(11) . ? C67 C68 1.514(10) . ? C70 C71 1.537(8) . ? C70 C72 1.549(9) . ? 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 N2 Si1 N1 89.8(3) . . ? N2 Si1 C13 103.7(3) . . ? N1 Si1 C13 122.6(3) . . ? N2 Si1 C22 122.6(3) . . ? N1 Si1 C22 107.6(3) . . ? C13 Si1 C22 110.3(3) . . ? C1 N1 C5 117.1(5) . . ? C1 N1 Si1 130.3(5) . . ? C5 N1 Si1 112.6(4) . . ? C6 N2 C12 109.8(5) . . ? C6 N2 Si1 111.3(4) . . ? C12 N2 Si1 132.0(4) . . ? C2 C1 N1 123.7(7) . . ? C1 C2 C3 119.1(7) . . ? C4 C3 C2 120.2(7) . . ? C3 C4 C5 121.2(7) . . ? C6 C5 C4 131.6(7) . . ? C6 C5 N1 109.9(6) . . ? C4 C5 N1 118.5(6) . . ? C5 C6 N2 116.3(6) . . ? C5 C6 C7 133.8(7) . . ? N2 C6 C7 109.6(5) . . ? C6 C7 C8 102.8(5) . . ? C9 C8 C7 115.8(5) . . ? C9 C8 C12 104.6(4) . . ? C7 C8 C12 103.6(5) . . ? C10 C9 C8 106.5(5) . . ? C9 C10 C11 104.3(5) . . ? C10 C11 C12 103.4(5) . . ? N2 C12 C11 117.2(6) . . ? N2 C12 C8 106.0(4) . . ? C11 C12 C8 104.0(4) . . ? C18 C13 C14 116.6(6) . . ? C18 C13 Si1 122.8(4) . . ? C14 C13 Si1 119.9(5) . . ? C15 C14 C13 117.0(6) . . ? C15 C14 C19 120.1(6) . . ? C13 C14 C19 122.9(6) . . ? C16 C15 C14 126.8(7) . . ? C15 C16 C17 116.6(6) . . ? C15 C16 C20 125.5(7) . . ? C17 C16 C20 117.9(7) . . ? C18 C17 C16 120.6(7) . . ? C17 C18 C13 122.3(6) . . ? C17 C18 C21 116.9(6) . . ? C13 C18 C21 120.8(5) . . ? C27 C22 C23 117.2(6) . . ? C27 C22 Si1 123.1(5) . . ? C23 C22 Si1 119.3(4) . . ? C24 C23 C22 120.4(5) . . ? C24 C23 C28 116.2(6) . . ? C22 C23 C28 123.1(6) . . ? C23 C24 C25 122.9(7) . . ? C26 C25 C24 117.4(7) . . ? C26 C25 C31 120.7(6) . . ? C24 C25 C31 121.9(7) . . ? C25 C26 C27 122.8(6) . . ? C22 C27 C26 119.0(6) . . ? C22 C27 C34 122.3(6) . . ? C26 C27 C34 118.6(5) . . ? C29 C28 C30 110.0(6) . . ? C29 C28 C23 112.3(5) . . ? C30 C28 C23 111.6(5) . . ? C25 C31 C32 112.8(6) . . ? C25 C31 C33 110.2(7) . . ? C32 C31 C33 109.0(7) . . ? C27 C34 C35 109.6(6) . . ? C27 C34 C36 116.6(6) . . ? C35 C34 C36 109.7(5) . . ? N4 Si2 N3 89.9(3) . . ? N4 Si2 C58 122.5(3) . . ? N3 Si2 C58 108.8(3) . . ? N4 Si2 C49 104.8(3) . . ? N3 Si2 C49 122.3(3) . . ? C58 Si2 C49 108.7(3) . . ? C37 N3 C41 119.4(5) . . ? C37 N3 Si2 130.0(5) . . ? C41 N3 Si2 110.4(4) . . ? C42 N4 C48 111.0(5) . . ? C42 N4 Si2 112.4(4) . . ? C48 N4 Si2 136.5(4) . . ? C38 C37 N3 123.6(7) . . ? C37 C38 C39 119.0(7) . . ? C40 C39 C38 119.1(6) . . ? C39 C40 C41 122.9(7) . . ? C42 C41 C40 130.5(7) . . ? C42 C41 N3 113.7(5) . . ? C40 C41 N3 115.8(6) . . ? C41 C42 N4 113.6(6) . . ? C41 C42 C43 136.5(6) . . ? N4 C42 C43 110.0(5) . . ? C42 C43 C44 105.1(5) . . ? C45 C44 C43 116.2(6) . . ? C45 C44 C48 104.7(4) . . ? C43 C44 C48 105.0(4) . . ? C46 C45 C44 107.4(6) . . ? C47 C46 C45 111.9(6) . . ? C46 C47 C48 107.3(4) . . ? N4 C48 C47 116.6(4) . . ? N4 C48 C44 104.7(4) . . ? C47 C48 C44 105.2(4) . . ? C50 C49 C54 119.3(5) . . ? C50 C49 Si2 119.9(5) . . ? C54 C49 Si2 120.4(5) . . ? C49 C50 C51 121.4(6) . . ? C49 C50 C55 123.2(5) . . ? C51 C50 C55 115.3(6) . . ? C50 C51 C52 118.8(6) . . ? C53 C52 C51 119.4(6) . . ? C53 C52 C56 122.8(7) . . ? C51 C52 C56 117.6(6) . . ? C52 C53 C54 123.2(6) . . ? C49 C54 C53 117.7(6) . . ? C49 C54 C57 123.5(5) . . ? C53 C54 C57 118.7(6) . . ? C63 C58 C59 118.2(6) . . ? C63 C58 Si2 120.2(5) . . ? C59 C58 Si2 121.6(5) . . ? C60 C59 C58 119.4(6) . . ? C60 C59 C64 118.2(6) . . ? C58 C59 C64 122.3(6) . . ? C59 C60 C61 122.3(6) . . ? C62 C61 C60 118.5(6) . . ? C62 C61 C67 121.3(6) . . ? C60 C61 C67 120.2(6) . . ? C61 C62 C63 121.5(6) . . ? C62 C63 C58 119.6(6) . . ? C62 C63 C70 117.3(6) . . ? C58 C63 C70 123.1(6) . . ? C66 C64 C65 109.1(5) . . ? C66 C64 C59 113.9(6) . . ? C65 C64 C59 109.7(6) . . ? C69 C67 C68 112.4(7) . . ? C69 C67 C61 112.1(6) . . ? C68 C67 C61 109.7(6) . . ? C63 C70 C71 112.8(5) . . ? C63 C70 C72 108.9(5) . . ? C71 C70 C72 109.4(6) . . ? 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 N2 Si1 N1 C1 -177.0(6) . . . . ? C13 Si1 N1 C1 76.8(7) . . . . ? C22 Si1 N1 C1 -52.7(6) . . . . ? N2 Si1 N1 C5 3.4(5) . . . . ? C13 Si1 N1 C5 -102.9(5) . . . . ? C22 Si1 N1 C5 127.7(4) . . . . ? N1 Si1 N2 C6 -3.3(5) . . . . ? C13 Si1 N2 C6 120.3(4) . . . . ? C22 Si1 N2 C6 -114.2(4) . . . . ? N1 Si1 N2 C12 -150.2(6) . . . . ? C13 Si1 N2 C12 -26.6(6) . . . . ? C22 Si1 N2 C12 98.8(6) . . . . ? C5 N1 C1 C2 3.6(9) . . . . ? Si1 N1 C1 C2 -176.0(5) . . . . ? N1 C1 C2 C3 -3.8(11) . . . . ? C1 C2 C3 C4 0.9(11) . . . . ? C2 C3 C4 C5 1.9(11) . . . . ? C3 C4 C5 C6 180.0(7) . . . . ? C3 C4 C5 N1 -2.0(10) . . . . ? C1 N1 C5 C6 177.8(6) . . . . ? Si1 N1 C5 C6 -2.6(7) . . . . ? C1 N1 C5 C4 -0.7(8) . . . . ? Si1 N1 C5 C4 179.0(5) . . . . ? C4 C5 C6 N2 178.2(6) . . . . ? N1 C5 C6 N2 0.0(8) . . . . ? C4 C5 C6 C7 -8.2(13) . . . . ? N1 C5 C6 C7 173.7(7) . . . . ? C12 N2 C6 C5 157.0(6) . . . . ? Si1 N2 C6 C5 2.6(7) . . . . ? C12 N2 C6 C7 -18.1(7) . . . . ? Si1 N2 C6 C7 -172.6(5) . . . . ? C5 C6 C7 C8 -145.7(7) . . . . ? N2 C6 C7 C8 28.3(7) . . . . ? C6 C7 C8 C9 -140.5(5) . . . . ? C6 C7 C8 C12 -26.7(6) . . . . ? C7 C8 C9 C10 124.3(6) . . . . ? C12 C8 C9 C10 10.9(7) . . . . ? C8 C9 C10 C11 -33.1(8) . . . . ? C9 C10 C11 C12 42.4(7) . . . . ? C6 N2 C12 C11 115.3(6) . . . . ? Si1 N2 C12 C11 -97.4(6) . . . . ? C6 N2 C12 C8 -0.2(6) . . . . ? Si1 N2 C12 C8 147.1(5) . . . . ? C10 C11 C12 N2 -151.3(5) . . . . ? C10 C11 C12 C8 -34.8(7) . . . . ? C9 C8 C12 N2 138.8(5) . . . . ? C7 C8 C12 N2 17.1(5) . . . . ? C9 C8 C12 C11 14.6(7) . . . . ? C7 C8 C12 C11 -107.1(5) . . . . ? N2 Si1 C13 C18 -85.8(6) . . . . ? N1 Si1 C13 C18 13.0(7) . . . . ? C22 Si1 C13 C18 141.2(5) . . . . ? N2 Si1 C13 C14 84.4(6) . . . . ? N1 Si1 C13 C14 -176.9(5) . . . . ? C22 Si1 C13 C14 -48.6(6) . . . . ? C18 C13 C14 C15 -1.5(9) . . . . ? Si1 C13 C14 C15 -172.2(6) . . . . ? C18 C13 C14 C19 177.4(6) . . . . ? Si1 C13 C14 C19 6.6(9) . . . . ? C13 C14 C15 C16 1.4(12) . . . . ? C19 C14 C15 C16 -177.4(7) . . . . ? C14 C15 C16 C17 -2.3(12) . . . . ? C14 C15 C16 C20 179.4(8) . . . . ? C15 C16 C17 C18 3.4(11) . . . . ? C20 C16 C17 C18 -178.2(7) . . . . ? C16 C17 C18 C13 -3.8(11) . . . . ? C16 C17 C18 C21 178.6(7) . . . . ? C14 C13 C18 C17 2.8(10) . . . . ? Si1 C13 C18 C17 173.2(6) . . . . ? C14 C13 C18 C21 -179.8(7) . . . . ? Si1 C13 C18 C21 -9.3(9) . . . . ? N2 Si1 C22 C27 9.0(6) . . . . ? N1 Si1 C22 C27 -92.5(5) . . . . ? C13 Si1 C22 C27 131.5(5) . . . . ? N2 Si1 C22 C23 -164.2(4) . . . . ? N1 Si1 C22 C23 94.3(5) . . . . ? C13 Si1 C22 C23 -41.7(5) . . . . ? C27 C22 C23 C24 -4.5(8) . . . . ? Si1 C22 C23 C24 169.1(5) . . . . ? C27 C22 C23 C28 168.7(5) . . . . ? Si1 C22 C23 C28 -17.7(8) . . . . ? C22 C23 C24 C25 -1.4(10) . . . . ? C28 C23 C24 C25 -175.1(6) . . . . ? C23 C24 C25 C26 5.5(10) . . . . ? C23 C24 C25 C31 -173.5(7) . . . . ? C24 C25 C26 C27 -3.8(11) . . . . ? C31 C25 C26 C27 175.2(7) . . . . ? C23 C22 C27 C26 6.1(8) . . . . ? Si1 C22 C27 C26 -167.3(5) . . . . ? C23 C22 C27 C34 -170.7(6) . . . . ? Si1 C22 C27 C34 16.0(8) . . . . ? C25 C26 C27 C22 -2.0(10) . . . . ? C25 C26 C27 C34 174.8(7) . . . . ? C24 C23 C28 C29 -64.4(8) . . . . ? C22 C23 C28 C29 122.1(6) . . . . ? C24 C23 C28 C30 59.7(8) . . . . ? C22 C23 C28 C30 -113.8(7) . . . . ? C26 C25 C31 C32 -117.6(8) . . . . ? C24 C25 C31 C32 61.4(10) . . . . ? C26 C25 C31 C33 120.3(8) . . . . ? C24 C25 C31 C33 -60.8(9) . . . . ? C22 C27 C34 C35 82.6(7) . . . . ? C26 C27 C34 C35 -94.1(7) . . . . ? C22 C27 C34 C36 -152.1(6) . . . . ? C26 C27 C34 C36 31.2(9) . . . . ? N4 Si2 N3 C37 175.9(6) . . . . ? C58 Si2 N3 C37 51.3(6) . . . . ? C49 Si2 N3 C37 -76.6(7) . . . . ? N4 Si2 N3 C41 0.0(4) . . . . ? C58 Si2 N3 C41 -124.5(4) . . . . ? C49 Si2 N3 C41 107.5(4) . . . . ? N3 Si2 N4 C42 0.3(4) . . . . ? C58 Si2 N4 C42 112.7(4) . . . . ? C49 Si2 N4 C42 -123.2(4) . . . . ? N3 Si2 N4 C48 -179.8(6) . . . . ? C58 Si2 N4 C48 -67.4(7) . . . . ? C49 Si2 N4 C48 56.7(7) . . . . ? C41 N3 C37 C38 0.2(10) . . . . ? Si2 N3 C37 C38 -175.3(6) . . . . ? N3 C37 C38 C39 -2.9(12) . . . . ? C37 C38 C39 C40 1.9(11) . . . . ? C38 C39 C40 C41 1.8(11) . . . . ? C39 C40 C41 C42 175.7(7) . . . . ? C39 C40 C41 N3 -4.3(9) . . . . ? C37 N3 C41 C42 -176.7(6) . . . . ? Si2 N3 C41 C42 -0.4(7) . . . . ? C37 N3 C41 C40 3.3(8) . . . . ? Si2 N3 C41 C40 179.6(4) . . . . ? C40 C41 C42 N4 -179.4(6) . . . . ? N3 C41 C42 N4 0.6(8) . . . . ? C40 C41 C42 C43 1.6(13) . . . . ? N3 C41 C42 C43 -178.4(8) . . . . ? C48 N4 C42 C41 179.5(5) . . . . ? Si2 N4 C42 C41 -0.6(7) . . . . ? C48 N4 C42 C43 -1.2(7) . . . . ? Si2 N4 C42 C43 178.7(5) . . . . ? C41 C42 C43 C44 -167.3(7) . . . . ? N4 C42 C43 C44 13.7(7) . . . . ? C42 C43 C44 C45 -135.0(5) . . . . ? C42 C43 C44 C48 -19.9(6) . . . . ? C43 C44 C45 C46 98.4(8) . . . . ? C48 C44 C45 C46 -16.9(8) . . . . ? C44 C45 C46 C47 8.8(11) . . . . ? C45 C46 C47 C48 3.5(10) . . . . ? C42 N4 C48 C47 104.4(5) . . . . ? Si2 N4 C48 C47 -75.5(8) . . . . ? C42 N4 C48 C44 -11.5(6) . . . . ? Si2 N4 C48 C44 168.7(5) . . . . ? C46 C47 C48 N4 -129.4(6) . . . . ? C46 C47 C48 C44 -13.9(7) . . . . ? C45 C44 C48 N4 142.1(5) . . . . ? C43 C44 C48 N4 19.2(6) . . . . ? C45 C44 C48 C47 18.7(6) . . . . ? C43 C44 C48 C47 -104.2(5) . . . . ? N4 Si2 C49 C50 -81.5(6) . . . . ? N3 Si2 C49 C50 179.0(5) . . . . ? C58 Si2 C49 C50 51.0(6) . . . . ? N4 Si2 C49 C54 90.4(5) . . . . ? N3 Si2 C49 C54 -9.1(6) . . . . ? C58 Si2 C49 C54 -137.1(5) . . . . ? C54 C49 C50 C51 4.0(10) . . . . ? Si2 C49 C50 C51 176.0(6) . . . . ? C54 C49 C50 C55 -177.7(6) . . . . ? Si2 C49 C50 C55 -5.6(9) . . . . ? C49 C50 C51 C52 -1.7(11) . . . . ? C55 C50 C51 C52 179.9(6) . . . . ? C50 C51 C52 C53 -2.0(11) . . . . ? C50 C51 C52 C56 -177.1(7) . . . . ? C51 C52 C53 C54 3.3(11) . . . . ? C56 C52 C53 C54 178.2(7) . . . . ? C50 C49 C54 C53 -2.7(9) . . . . ? Si2 C49 C54 C53 -174.7(5) . . . . ? C50 C49 C54 C57 176.2(7) . . . . ? Si2 C49 C54 C57 4.2(9) . . . . ? C52 C53 C54 C49 -1.0(11) . . . . ? C52 C53 C54 C57 -179.9(7) . . . . ? N4 Si2 C58 C63 165.9(4) . . . . ? N3 Si2 C58 C63 -91.7(5) . . . . ? C49 Si2 C58 C63 43.6(5) . . . . ? N4 Si2 C58 C59 -11.1(5) . . . . ? N3 Si2 C58 C59 91.3(5) . . . . ? C49 Si2 C58 C59 -133.4(4) . . . . ? C63 C58 C59 C60 -7.9(8) . . . . ? Si2 C58 C59 C60 169.2(5) . . . . ? C63 C58 C59 C64 168.5(6) . . . . ? Si2 C58 C59 C64 -14.5(8) . . . . ? C58 C59 C60 C61 1.7(10) . . . . ? C64 C59 C60 C61 -174.8(6) . . . . ? C59 C60 C61 C62 3.8(11) . . . . ? C59 C60 C61 C67 -177.0(7) . . . . ? C60 C61 C62 C63 -3.0(10) . . . . ? C67 C61 C62 C63 177.8(7) . . . . ? C61 C62 C63 C58 -3.2(9) . . . . ? C61 C62 C63 C70 178.0(6) . . . . ? C59 C58 C63 C62 8.6(8) . . . . ? Si2 C58 C63 C62 -168.5(5) . . . . ? C59 C58 C63 C70 -172.7(5) . . . . ? Si2 C58 C63 C70 10.2(8) . . . . ? C60 C59 C64 C66 -32.5(9) . . . . ? C58 C59 C64 C66 151.1(6) . . . . ? C60 C59 C64 C65 90.1(8) . . . . ? C58 C59 C64 C65 -86.3(7) . . . . ? C62 C61 C67 C69 60.2(9) . . . . ? C60 C61 C67 C69 -119.0(8) . . . . ? C62 C61 C67 C68 -65.5(9) . . . . ? C60 C61 C67 C68 115.4(8) . . . . ? C62 C63 C70 C71 60.9(8) . . . . ? C58 C63 C70 C71 -117.9(7) . . . . ? C62 C63 C70 C72 -60.8(7) . . . . ? C58 C63 C70 C72 120.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.91 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.204 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.040