# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Philippe Gerbier' _publ_contact_author_address ; CMOS - UMR 5637 Universite Montpellier 2 Place E. Bataillon CC007 Montpellier 34095 cedex 5 FRANCE ; _publ_contact_author_email GERBIER@UNIV-MONTP2.FR _publ_section_title ; Towards a Better Understanding of Photo-excited Spin Alignment Processes Using Silole Diradicals ; loop_ _publ_author_name 'Gerbier Philippe' 'Sylvie Choua' 'Christian Guerin' 'Philippe Guionneau' 'Petra Lesniakova' 'Nans Roques' ; J.-P.Sutter ; 'Yoshio Teki' data_nr376 _database_code_depnum_ccdc_archive 'CCDC 603216' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H48 N4 O2 Si' _chemical_formula_weight 692.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9846(3) _cell_length_b 11.4743(4) _cell_length_c 17.4918(8) _cell_angle_alpha 81.1010(10) _cell_angle_beta 89.0170(10) _cell_angle_gamma 65.707(2) _cell_volume 1982.62(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6168 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 26.8 _exptl_crystal_description spearhead _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12809 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0870 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 26.58 _reflns_number_total 8110 _reflns_number_gt 4117 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury (CCDC)' _computing_publication_material 'shelxl-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^)+(0.0564P)^2^+1.1981P] 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 SHELXL _refine_ls_extinction_coef 0.0056(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8110 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1490 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1823 _refine_ls_wR_factor_gt 0.1477 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.010 _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 0.69626(9) 0.64208(9) 0.48256(5) 0.0580(3) Uani 1 1 d . . . N4 N 0.1840(3) 0.8393(3) 0.80736(15) 0.0659(7) Uani 1 1 d . . . C1 C 1.0183(3) 0.4971(3) 0.23170(17) 0.0540(8) Uani 1 1 d . . . C27 C 0.3826(3) 0.9245(3) 0.56322(18) 0.0606(8) Uani 1 1 d . . . C29 C 0.2987(3) 0.8704(3) 0.68491(16) 0.0528(7) Uani 1 1 d . . . N3 N 0.1722(3) 1.0346(3) 0.76248(15) 0.0703(8) Uani 1 1 d . . . C19 C 0.6912(3) 0.6706(3) 0.37422(16) 0.0528(7) Uani 1 1 d . . . C18 C 0.5160(3) 0.7540(3) 0.48360(17) 0.0558(8) Uani 1 1 d . . . C16 C 0.5640(3) 0.7500(3) 0.34793(16) 0.0504(7) Uani 1 1 d . . . C32 C 0.2188(3) 0.9169(3) 0.75110(16) 0.0525(7) Uani 1 1 d . . . C20 C 0.3283(3) 0.9025(3) 0.38662(16) 0.0527(7) Uani 1 1 d . . . C26 C 0.4421(3) 0.7958(3) 0.55303(16) 0.0542(8) Uani 1 1 d . . . C11 C 0.5186(3) 0.7824(3) 0.26465(17) 0.0525(8) Uani 1 1 d . . . C17 C 0.4664(3) 0.8015(3) 0.40908(16) 0.0512(7) Uani 1 1 d . . . C28 C 0.3124(3) 0.9610(3) 0.62769(18) 0.0598(8) Uani 1 1 d . . . C6 C 1.0314(3) 0.5591(4) 0.2906(2) 0.0683(9) Uani 1 1 d . . . C4 C 0.8035(3) 0.6069(3) 0.32529(16) 0.0528(7) Uani 1 1 d . . . C12 C 0.5693(4) 0.8517(3) 0.21177(18) 0.0647(9) Uani 1 1 d . . . O2 O 0.2167(3) 0.7185(3) 0.81315(17) 0.1116(11) Uani 1 1 d . . . C2 C 0.8989(3) 0.4862(3) 0.2215(2) 0.0646(9) Uani 1 1 d . . . C21 C 0.3071(4) 1.0179(3) 0.33808(18) 0.0618(9) Uani 1 1 d . . . C33 C 0.0819(3) 1.0520(4) 0.82768(19) 0.0683(9) Uani 1 1 d . . . C30 C 0.3600(4) 0.7411(4) 0.6765(2) 0.0741(11) Uani 1 1 d . . . C5 C 0.9254(3) 0.6117(4) 0.3369(2) 0.0674(9) Uani 1 1 d . . . C3 C 0.7931(3) 0.5399(3) 0.2677(2) 0.0647(9) Uani 1 1 d . . . C34 C 0.1105(3) 0.9132(4) 0.86845(18) 0.0649(9) Uani 1 1 d . . . C25 C 0.2174(3) 0.8872(4) 0.4169(2) 0.0680(9) Uani 1 1 d . . . C7 C 0.5339(4) 0.8749(5) 0.1336(2) 0.0869(12) Uani 1 1 d . . . C31 C 0.4319(4) 0.7052(4) 0.61186(19) 0.0745(11) Uani 1 1 d . . . C22 C 0.1799(4) 1.1147(4) 0.3218(2) 0.0759(11) Uani 1 1 d . . . C23 C 0.0726(4) 1.0984(5) 0.3531(3) 0.0839(13) Uani 1 1 d . . . C24 C 0.0891(4) 0.9857(5) 0.4000(2) 0.0824(12) Uani 1 1 d . . . C10 C 0.4308(4) 0.7377(4) 0.2376(2) 0.0783(11) Uani 1 1 d . . . C8 C 0.4499(4) 0.8279(6) 0.1078(3) 0.1028(17) Uani 1 1 d . . . C9 C 0.3985(4) 0.7598(6) 0.1584(3) 0.1017(17) Uani 1 1 d . . . C35 C 0.7372(6) 0.4691(4) 0.5206(3) 0.0828(12) Uani 1 1 d . . . C36 C 0.8071(5) 0.6964(5) 0.5318(3) 0.0813(12) Uani 1 1 d . . . C37 C 0.1043(6) 1.1408(6) 0.8757(3) 0.1045(16) Uani 1 1 d . . . C40 C -0.0090(6) 0.8807(8) 0.8872(4) 0.1094(18) Uani 1 1 d . . . C39 C 0.2103(6) 0.8666(7) 0.9380(3) 0.1101(18) Uani 1 1 d . . . C38 C -0.0614(5) 1.1252(7) 0.7878(4) 0.1135(17) Uani 1 1 d . . . C41 C 1.1231(3) 0.4462(3) 0.17660(19) 0.0569(8) Uani 1 1 d . . . N1 N 1.1097(3) 0.3978(4) 0.1202(2) 0.1198(15) Uani 1 1 d . . . N2 N 1.2458(3) 0.4502(4) 0.1786(2) 0.1011(12) Uani 1 1 d . . . C43 C 1.3294(4) 0.3791(5) 0.1197(3) 0.1104(17) Uani 1 1 d . . . O1 O 1.2916(4) 0.4910(6) 0.2298(3) 0.228(3) Uani 1 1 d . . . C44 C 1.2311(5) 0.3681(7) 0.0727(3) 0.133(2) Uani 1 1 d . . . C46 C 1.4371(5) 0.4166(5) 0.0976(3) 0.133(2) Uani 1 1 d . . . H46A H 1.4860 0.4139 0.1433 0.199 Uiso 1 1 calc R . . H46B H 1.4010 0.5030 0.0689 0.199 Uiso 1 1 calc R . . H46C H 1.4959 0.3579 0.0661 0.199 Uiso 1 1 calc R . . C47 C 1.4043(6) 0.2233(6) 0.1659(4) 0.214(4) Uani 1 1 d . . . H47A H 1.4746 0.2147 0.2011 0.321 Uiso 1 1 calc R . . H47B H 1.4410 0.1666 0.1285 0.321 Uiso 1 1 calc R . . H47C H 1.3394 0.2006 0.1942 0.321 Uiso 1 1 calc R . . C42 C 1.2434(7) 0.2745(9) 0.0285(5) 0.243(5) Uani 1 1 d . . . H42A H 1.1586 0.2955 0.0029 0.364 Uiso 1 1 calc R . . H42B H 1.2719 0.1918 0.0614 0.364 Uiso 1 1 calc R . . H42C H 1.3084 0.2709 -0.0095 0.364 Uiso 1 1 calc R . . C45 C 1.1966(7) 0.5150(8) 0.0094(4) 0.235(5) Uani 1 1 d . . . H45A H 1.1871 0.5816 0.0391 0.352 Uiso 1 1 calc R . . H45B H 1.1152 0.5393 -0.0207 0.352 Uiso 1 1 calc R . . H45C H 1.2688 0.5037 -0.0245 0.352 Uiso 1 1 calc R . . H3 H 0.714(3) 0.529(3) 0.2592(17) 0.064(9) Uiso 1 1 d . . . H27 H 0.390(3) 0.990(3) 0.5217(19) 0.078(10) Uiso 1 1 d . . . H28 H 0.274(3) 1.048(3) 0.6334(18) 0.068(10) Uiso 1 1 d . . . H2 H 0.886(3) 0.441(3) 0.185(2) 0.084(12) Uiso 1 1 d . . . H10 H 0.400(3) 0.688(3) 0.2737(19) 0.071(11) Uiso 1 1 d . . . H30 H 0.359(3) 0.677(3) 0.713(2) 0.078(11) Uiso 1 1 d . . . H5 H 0.935(3) 0.660(3) 0.378(2) 0.084(11) Uiso 1 1 d . . . H21 H 0.378(3) 1.034(3) 0.3196(18) 0.067(10) Uiso 1 1 d . . . H6 H 1.117(4) 0.562(3) 0.299(2) 0.087(11) Uiso 1 1 d . . . H25 H 0.236(3) 0.811(4) 0.451(2) 0.083(12) Uiso 1 1 d . . . H36A H 0.778(4) 0.698(4) 0.578(3) 0.108(16) Uiso 1 1 d . . . H31 H 0.478(3) 0.615(4) 0.6102(19) 0.080(11) Uiso 1 1 d . . . H12 H 0.638(4) 0.882(4) 0.230(2) 0.094(12) Uiso 1 1 d . . . H23 H -0.014(5) 1.162(4) 0.343(2) 0.117(15) Uiso 1 1 d . . . H35C H 0.676(5) 0.447(4) 0.501(3) 0.114(18) Uiso 1 1 d . . . H36B H 0.909(5) 0.631(5) 0.527(3) 0.138(17) Uiso 1 1 d . . . H35B H 0.718(4) 0.461(4) 0.574(3) 0.113(16) Uiso 1 1 d . . . H24 H 0.011(4) 0.973(4) 0.425(2) 0.101(12) Uiso 1 1 d . . . H22 H 0.175(4) 1.193(4) 0.291(2) 0.096(13) Uiso 1 1 d . . . H36C H 0.803(4) 0.783(5) 0.505(3) 0.128(17) Uiso 1 1 d . . . H35A H 0.827(5) 0.415(5) 0.505(3) 0.126(17) Uiso 1 1 d . . . H9 H 0.350(4) 0.719(4) 0.148(2) 0.108(15) Uiso 1 1 d . . . H37A H 0.212(3) 1.064(3) 0.9050(18) 0.067(9) Uiso 1 1 d . . . H38A H -0.114(5) 1.151(5) 0.836(3) 0.146(19) Uiso 1 1 d . . . H37B H 0.040(5) 1.156(4) 0.917(3) 0.128(16) Uiso 1 1 d . . . H39A H 0.223(5) 0.781(5) 0.953(3) 0.14(2) Uiso 1 1 d . . . H7 H 0.577(4) 0.923(4) 0.094(3) 0.123(15) Uiso 1 1 d . . . H40C H -0.063(5) 0.923(5) 0.837(3) 0.14(2) Uiso 1 1 d . . . H8 H 0.428(4) 0.845(4) 0.054(3) 0.126(16) Uiso 1 1 d . . . H300C H 0.088(5) 1.227(5) 0.841(3) 0.135(19) Uiso 1 1 d . . . H40A H -0.055(5) 0.930(5) 0.922(3) 0.121(17) Uiso 1 1 d . . . H39C H 0.159(5) 0.916(5) 0.979(3) 0.135(17) Uiso 1 1 d . . . H39B H 0.303(6) 0.909(6) 0.920(3) 0.17(2) Uiso 1 1 d . . . H400B H 0.033(8) 0.785(8) 0.908(4) 0.23(4) Uiso 1 1 d . . . H38C H -0.058(8) 1.220(9) 0.764(5) 0.27(4) Uiso 1 1 d . . . H38B H -0.086(6) 1.059(7) 0.761(4) 0.19(3) 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 0.0603(5) 0.0533(5) 0.0454(5) -0.0119(4) 0.0063(4) -0.0075(4) N4 0.0791(19) 0.0689(19) 0.0591(17) -0.0254(15) 0.0285(14) -0.0357(16) C1 0.0476(17) 0.0487(18) 0.0548(19) -0.0094(15) 0.0123(14) -0.0090(14) C27 0.073(2) 0.056(2) 0.0484(19) -0.0113(16) 0.0226(16) -0.0217(18) C29 0.0574(18) 0.059(2) 0.0401(16) -0.0140(15) 0.0096(13) -0.0207(16) N3 0.084(2) 0.072(2) 0.0555(17) -0.0268(15) 0.0288(14) -0.0283(16) C19 0.0517(18) 0.0528(18) 0.0453(17) -0.0162(14) 0.0103(14) -0.0105(15) C18 0.0582(18) 0.0544(18) 0.0440(18) -0.0129(15) 0.0139(14) -0.0112(15) C16 0.0520(17) 0.0519(18) 0.0435(17) -0.0149(14) 0.0125(13) -0.0155(15) C32 0.0522(17) 0.068(2) 0.0413(17) -0.0188(15) 0.0126(13) -0.0261(16) C20 0.0513(17) 0.0571(19) 0.0416(17) -0.0181(15) 0.0103(13) -0.0111(15) C26 0.0564(18) 0.0558(19) 0.0405(17) -0.0133(15) 0.0113(13) -0.0119(15) C11 0.0452(16) 0.0592(19) 0.0467(17) -0.0213(15) 0.0090(13) -0.0109(15) C17 0.0510(17) 0.0505(18) 0.0446(18) -0.0144(14) 0.0122(13) -0.0117(14) C28 0.069(2) 0.052(2) 0.057(2) -0.0211(17) 0.0236(16) -0.0191(17) C6 0.0465(19) 0.081(2) 0.067(2) -0.0224(19) 0.0057(16) -0.0130(18) C4 0.0495(17) 0.0510(18) 0.0454(17) -0.0109(14) 0.0083(13) -0.0077(14) C12 0.069(2) 0.074(2) 0.0448(19) -0.0167(17) 0.0096(16) -0.0218(19) O2 0.162(3) 0.091(2) 0.103(2) -0.0351(17) 0.071(2) -0.069(2) C2 0.062(2) 0.065(2) 0.073(2) -0.0324(19) 0.0249(17) -0.0249(18) C21 0.062(2) 0.059(2) 0.051(2) -0.0112(16) 0.0082(16) -0.0115(19) C33 0.069(2) 0.082(2) 0.059(2) -0.0329(19) 0.0250(17) -0.0296(19) C30 0.105(3) 0.059(2) 0.048(2) -0.0084(18) 0.0238(19) -0.025(2) C5 0.052(2) 0.080(2) 0.059(2) -0.0294(19) 0.0037(16) -0.0103(18) C3 0.056(2) 0.070(2) 0.075(2) -0.0339(19) 0.0251(17) -0.0258(18) C34 0.064(2) 0.087(3) 0.0480(19) -0.0246(18) 0.0206(16) -0.0310(19) C25 0.058(2) 0.076(3) 0.063(2) -0.014(2) 0.0083(17) -0.021(2) C7 0.082(3) 0.114(3) 0.046(2) -0.015(2) 0.010(2) -0.023(3) C31 0.103(3) 0.054(2) 0.051(2) -0.0131(18) 0.0238(19) -0.016(2) C22 0.083(3) 0.063(3) 0.060(2) -0.012(2) -0.005(2) -0.008(2) C23 0.060(3) 0.093(3) 0.074(3) -0.031(3) -0.008(2) -0.001(2) C24 0.053(2) 0.111(4) 0.078(3) -0.030(3) 0.008(2) -0.024(2) C10 0.060(2) 0.108(3) 0.077(3) -0.041(2) 0.0190(19) -0.036(2) C8 0.066(3) 0.162(5) 0.057(3) -0.041(3) 0.000(2) -0.017(3) C9 0.058(2) 0.161(5) 0.096(4) -0.075(4) 0.007(2) -0.037(3) C35 0.090(3) 0.064(3) 0.079(3) -0.011(2) 0.001(3) -0.017(2) C36 0.090(3) 0.081(3) 0.066(3) -0.017(2) -0.002(2) -0.026(3) C37 0.140(5) 0.112(4) 0.081(3) -0.051(3) 0.041(3) -0.060(4) C40 0.102(4) 0.144(5) 0.103(4) -0.036(4) 0.056(4) -0.067(4) C39 0.121(4) 0.123(5) 0.063(3) -0.027(3) -0.002(3) -0.021(4) C38 0.077(3) 0.121(5) 0.120(4) -0.033(4) 0.006(3) -0.013(3) C41 0.0503(18) 0.0534(19) 0.059(2) -0.0108(16) 0.0168(15) -0.0133(15) N1 0.083(2) 0.201(4) 0.116(3) -0.102(3) 0.060(2) -0.075(3) N2 0.074(2) 0.134(3) 0.122(3) -0.074(3) 0.046(2) -0.052(2) C43 0.079(3) 0.139(4) 0.144(4) -0.082(3) 0.069(3) -0.057(3) O1 0.134(3) 0.395(8) 0.272(6) -0.246(6) 0.116(4) -0.161(5) C44 0.082(3) 0.228(6) 0.121(4) -0.100(4) 0.067(3) -0.074(4) C46 0.095(3) 0.156(5) 0.167(5) -0.058(4) 0.066(3) -0.064(3) C47 0.154(5) 0.128(5) 0.204(7) 0.046(5) 0.081(5) 0.068(4) C42 0.194(6) 0.413(12) 0.296(9) -0.313(10) 0.192(7) -0.217(8) C45 0.179(6) 0.260(9) 0.126(5) 0.088(6) 0.060(5) 0.005(6) _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 C36 1.855(4) . ? Si1 C35 1.858(4) . ? Si1 C18 1.866(3) . ? Si1 C19 1.870(3) . ? N4 O2 1.268(3) . ? N4 C32 1.379(4) . ? N4 C34 1.483(4) . ? C1 C6 1.380(5) . ? C1 C2 1.385(4) . ? C1 C41 1.475(4) . ? C27 C28 1.376(4) . ? C27 C26 1.386(4) . ? C29 C28 1.381(4) . ? C29 C30 1.384(4) . ? C29 C32 1.472(4) . ? N3 C32 1.280(4) . ? N3 C33 1.481(4) . ? C19 C16 1.356(4) . ? C19 C4 1.485(4) . ? C18 C17 1.362(4) . ? C18 C26 1.480(4) . ? C16 C11 1.488(4) . ? C16 C17 1.509(4) . ? C20 C25 1.387(4) . ? C20 C21 1.390(4) . ? C20 C17 1.494(4) . ? C26 C31 1.383(4) . ? C11 C12 1.385(4) . ? C11 C10 1.383(5) . ? C6 C5 1.384(4) . ? C4 C5 1.382(4) . ? C4 C3 1.391(4) . ? C12 C7 1.382(5) . ? C2 C3 1.384(4) . ? C21 C22 1.381(5) . ? C33 C37 1.510(5) . ? C33 C34 1.545(5) . ? C33 C38 1.562(6) . ? C30 C31 1.386(4) . ? C34 C40 1.523(5) . ? C34 C39 1.526(6) . ? C25 C24 1.397(5) . ? C7 C8 1.359(6) . ? C22 C23 1.361(6) . ? C23 C24 1.364(6) . ? C10 C9 1.394(6) . ? C8 C9 1.357(7) . ? C41 N1 1.244(4) . ? C41 N2 1.369(4) . ? N1 C44 1.503(5) . ? N2 O1 1.271(5) . ? N2 C43 1.477(5) . ? C43 C44 1.425(6) . ? C43 C46 1.444(5) . ? C43 C47 1.701(7) . ? C44 C42 1.380(7) . ? C44 C45 1.767(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 C36 Si1 C35 110.0(2) . . ? C36 Si1 C18 112.31(19) . . ? C35 Si1 C18 115.1(2) . . ? C36 Si1 C19 116.1(2) . . ? C35 Si1 C19 110.71(19) . . ? C18 Si1 C19 91.83(13) . . ? O2 N4 C32 127.4(3) . . ? O2 N4 C34 121.5(3) . . ? C32 N4 C34 110.9(3) . . ? C6 C1 C2 118.6(3) . . ? C6 C1 C41 123.4(3) . . ? C2 C1 C41 117.9(3) . . ? C28 C27 C26 121.5(3) . . ? C28 C29 C30 118.2(3) . . ? C28 C29 C32 118.1(3) . . ? C30 C29 C32 123.7(3) . . ? C32 N3 C33 109.8(3) . . ? C16 C19 C4 125.6(3) . . ? C16 C19 Si1 108.2(2) . . ? C4 C19 Si1 125.9(2) . . ? C17 C18 C26 125.0(3) . . ? C17 C18 Si1 108.6(2) . . ? C26 C18 Si1 126.1(2) . . ? C19 C16 C11 123.4(2) . . ? C19 C16 C17 115.9(3) . . ? C11 C16 C17 120.6(2) . . ? N3 C32 N4 112.2(3) . . ? N3 C32 C29 123.7(3) . . ? N4 C32 C29 124.1(3) . . ? C25 C20 C21 117.8(3) . . ? C25 C20 C17 120.9(3) . . ? C21 C20 C17 121.2(3) . . ? C27 C26 C31 117.1(3) . . ? C27 C26 C18 122.7(3) . . ? C31 C26 C18 120.2(3) . . ? C12 C11 C10 118.5(3) . . ? C12 C11 C16 120.6(3) . . ? C10 C11 C16 120.8(3) . . ? C18 C17 C20 124.1(2) . . ? C18 C17 C16 115.2(3) . . ? C20 C17 C16 120.6(2) . . ? C27 C28 C29 121.0(3) . . ? C1 C6 C5 120.1(3) . . ? C5 C4 C3 117.3(3) . . ? C5 C4 C19 119.8(3) . . ? C3 C4 C19 123.0(3) . . ? C11 C12 C7 120.8(4) . . ? C1 C2 C3 120.8(3) . . ? C22 C21 C20 120.9(4) . . ? N3 C33 C37 108.7(3) . . ? N3 C33 C34 105.1(3) . . ? C37 C33 C34 117.1(4) . . ? N3 C33 C38 104.3(3) . . ? C37 C33 C38 107.7(4) . . ? C34 C33 C38 113.1(4) . . ? C29 C30 C31 120.2(3) . . ? C4 C5 C6 122.1(3) . . ? C2 C3 C4 121.0(3) . . ? N4 C34 C40 108.4(3) . . ? N4 C34 C39 105.3(3) . . ? C40 C34 C39 111.1(5) . . ? N4 C34 C33 99.5(2) . . ? C40 C34 C33 117.6(4) . . ? C39 C34 C33 113.4(4) . . ? C20 C25 C24 120.8(4) . . ? C8 C7 C12 119.9(4) . . ? C30 C31 C26 121.8(3) . . ? C23 C22 C21 120.3(4) . . ? C24 C23 C22 120.5(4) . . ? C23 C24 C25 119.7(4) . . ? C11 C10 C9 119.8(4) . . ? C9 C8 C7 120.5(4) . . ? C8 C9 C10 120.4(4) . . ? N1 C41 N2 110.7(3) . . ? N1 C41 C1 124.3(3) . . ? N2 C41 C1 125.0(3) . . ? C41 N1 C44 109.7(3) . . ? O1 N2 C41 126.3(3) . . ? O1 N2 C43 122.9(3) . . ? C41 N2 C43 110.1(3) . . ? C44 C43 C46 130.1(5) . . ? C44 C43 N2 101.0(3) . . ? C46 C43 N2 113.5(4) . . ? C44 C43 C47 99.2(5) . . ? C46 C43 C47 105.6(5) . . ? N2 C43 C47 104.1(4) . . ? C42 C44 C43 129.8(6) . . ? C42 C44 N1 110.9(4) . . ? C43 C44 N1 105.6(4) . . ? C42 C44 C45 108.2(6) . . ? C43 C44 C45 94.8(5) . . ? N1 C44 C45 103.9(4) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.58 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.466 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.042