# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Reinhard Tacke' _publ_contact_author_name 'Reinhard Tacke' _publ_contact_author_email r.tacke@uni-wuerzburg.de _publ_section_title ; Novel Neutral Hexacoordinate Silicon (IV) Complexes with Two Bidentate Monoanionic Benzamidinato Ligands and Two Monodentate (Pseudo)halogeno Ligands or One Bidentate Dianionic S,S, S,Se or Se,Se Ligand ; # Attachment '- bisamidinato_si_complexes_dalton_final_28_04_10.txt' data_jun08fc _database_code_depnum_ccdc_archive 'CCDC 775531' #TrackingRef '- bisamidinato_si_complexes_dalton_final_28_04_10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H38 Cl2 N4 Si' _chemical_formula_sum 'C26 H38 Cl2 N4 Si' _chemical_formula_weight 505.59 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5369(5) _cell_length_b 17.8631(9) _cell_length_c 16.0043(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.067(2) _cell_angle_gamma 90.00 _cell_volume 2719.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7661 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 29.39 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .2 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .5740 _exptl_absorpt_correction_T_max .7459 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source rotating_anode _diffrn_radiation_monochromator MONTEL_multi_layer_optics _diffrn_measurement_device_type Bruker-Nonius-Kappa_Apex2_CCD _diffrn_measurement_method omega_and_phi_scans _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20988 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 29.45 _reflns_number_total 7501 _reflns_number_gt 5830 _reflns_threshold_expression >2sigma(I) _computing_data_collection Bruker-SAINT _computing_cell_refinement Bruker-SAINT _computing_data_reduction Bruker-SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/POvray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+2.9547P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7501 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.77507(19) 0.07350(11) 0.30428(12) 0.0167(4) Uani 1 1 d . . . C2 C 0.7298(2) -0.00052(11) 0.33549(11) 0.0178(4) Uani 1 1 d . . . C3 C 0.8274(2) -0.05628(11) 0.35444(13) 0.0216(4) Uani 1 1 d . . . H3 H 0.9236 -0.0481 0.3456 0.026 Uiso 1 1 calc R . . C4 C 0.7848(2) -0.12456(12) 0.38653(13) 0.0250(4) Uani 1 1 d . . . H4 H 0.8521 -0.1626 0.4003 0.030 Uiso 1 1 calc R . . C5 C 0.6441(2) -0.13686(12) 0.39830(13) 0.0271(5) Uani 1 1 d . . . H5 H 0.6151 -0.1833 0.4204 0.032 Uiso 1 1 calc R . . C6 C 0.5459(2) -0.08172(13) 0.37804(14) 0.0285(5) Uani 1 1 d . . . H6 H 0.4494 -0.0906 0.3855 0.034 Uiso 1 1 calc R . . C7 C 0.5878(2) -0.01317(12) 0.34671(13) 0.0244(4) Uani 1 1 d . . . H7 H 0.5203 0.0248 0.3330 0.029 Uiso 1 1 calc R . . C8 C 0.7833(2) 0.15276(11) 0.43585(12) 0.0193(4) Uani 1 1 d . . . H8 H 0.8444 0.1974 0.4485 0.023 Uiso 1 1 calc R . . C10 C 0.8378(2) 0.09096(12) 0.49467(13) 0.0273(5) Uani 1 1 d . . . H10A H 0.7724 0.0486 0.4907 0.041 Uiso 1 1 calc R . . H10B H 0.8458 0.1099 0.5523 0.041 Uiso 1 1 calc R . . H10C H 0.9303 0.0745 0.4789 0.041 Uiso 1 1 calc R . . C11 C 0.7795(2) 0.03605(11) 0.15486(12) 0.0199(4) Uani 1 1 d . . . H11 H 0.7563 -0.0140 0.1784 0.024 Uiso 1 1 calc R . . C12 C 0.6524(2) 0.06200(13) 0.09916(14) 0.0279(5) Uani 1 1 d . . . H12A H 0.5697 0.0640 0.1321 0.042 Uiso 1 1 calc R . . H12B H 0.6351 0.0268 0.0526 0.042 Uiso 1 1 calc R . . H12C H 0.6708 0.1119 0.0770 0.042 Uiso 1 1 calc R . . C13 C 0.9087(2) 0.02638(12) 0.10490(13) 0.0252(4) Uani 1 1 d . . . H13A H 0.9291 0.0737 0.0772 0.038 Uiso 1 1 calc R . . H13B H 0.8905 -0.0128 0.0626 0.038 Uiso 1 1 calc R . . H13C H 0.9894 0.0120 0.1428 0.038 Uiso 1 1 calc R . . C14 C 1.0432(2) 0.24274(11) 0.32053(11) 0.0170(4) Uani 1 1 d . . . C15 C 1.1672(2) 0.28082(11) 0.36361(12) 0.0185(4) Uani 1 1 d . . . C16 C 1.1716(2) 0.29720(12) 0.44863(13) 0.0243(4) Uani 1 1 d . . . H16 H 1.0953 0.2839 0.4807 0.029 Uiso 1 1 calc R . . C17 C 1.2894(2) 0.33339(13) 0.48638(14) 0.0301(5) Uani 1 1 d . . . H17 H 1.2946 0.3434 0.5448 0.036 Uiso 1 1 calc R . . C18 C 1.3989(2) 0.35474(13) 0.43895(15) 0.0294(5) Uani 1 1 d . . . H18 H 1.4782 0.3800 0.4649 0.035 Uiso 1 1 calc R . . C19 C 1.3934(2) 0.33946(12) 0.35396(14) 0.0258(4) Uani 1 1 d . . . H19 H 1.4682 0.3545 0.3215 0.031 Uiso 1 1 calc R . . C20 C 1.2778(2) 0.30195(11) 0.31637(13) 0.0210(4) Uani 1 1 d . . . H20 H 1.2742 0.2907 0.2582 0.025 Uiso 1 1 calc R . . C21 C 0.8861(2) 0.35290(11) 0.32200(12) 0.0203(4) Uani 1 1 d . . . H21 H 0.9776 0.3778 0.3389 0.024 Uiso 1 1 calc R . . C22 C 0.7915(2) 0.36216(12) 0.39400(14) 0.0270(5) Uani 1 1 d . . . H22A H 0.7013 0.3373 0.3799 0.041 Uiso 1 1 calc R . . H22B H 0.7755 0.4156 0.4037 0.041 Uiso 1 1 calc R . . H22C H 0.8368 0.3396 0.4448 0.041 Uiso 1 1 calc R . . C23 C 0.8246(2) 0.39148(12) 0.24270(13) 0.0269(4) Uani 1 1 d . . . H23A H 0.8865 0.3831 0.1972 0.040 Uiso 1 1 calc R . . H23B H 0.8166 0.4453 0.2530 0.040 Uiso 1 1 calc R . . H23C H 0.7314 0.3708 0.2268 0.040 Uiso 1 1 calc R . . C24 C 1.2361(2) 0.11658(13) 0.22125(14) 0.0278(5) Uani 1 1 d . . . H24A H 1.1805 0.1242 0.1681 0.042 Uiso 1 1 calc R . . H24B H 1.2882 0.0694 0.2191 0.042 Uiso 1 1 calc R . . H24C H 1.3024 0.1581 0.2308 0.042 Uiso 1 1 calc R . . C25 C 1.1380(2) 0.11342(11) 0.29286(12) 0.0191(4) Uani 1 1 d . . . H25 H 1.0817 0.0664 0.2845 0.023 Uiso 1 1 calc R . . C26 C 1.2199(2) 0.10590(13) 0.37779(14) 0.0278(5) Uani 1 1 d . . . H26A H 1.2891 0.1464 0.3847 0.042 Uiso 1 1 calc R . . H26B H 1.2685 0.0575 0.3809 0.042 Uiso 1 1 calc R . . H26C H 1.1549 0.1089 0.4224 0.042 Uiso 1 1 calc R . . Cl1 Cl 0.90283(5) 0.22330(3) 0.12545(3) 0.02033(10) Uani 1 1 d . . . Cl2 Cl 0.62828(5) 0.22784(3) 0.22384(3) 0.02234(11) Uani 1 1 d . . . N1 N 0.80759(17) 0.08765(9) 0.22558(10) 0.0173(3) Uani 1 1 d . . . N2 N 0.79123(17) 0.13645(9) 0.34658(10) 0.0172(3) Uani 1 1 d . . . N3 N 0.91586(17) 0.27336(9) 0.30656(10) 0.0178(3) Uani 1 1 d . . . N4 N 1.03681(17) 0.17549(9) 0.28696(10) 0.0172(3) Uani 1 1 d . . . C9 C 0.6333(2) 0.17589(13) 0.45388(14) 0.0282(5) Uani 1 1 d . . . H9A H 0.5978 0.2126 0.4121 0.042 Uiso 1 1 calc R . . H9B H 0.6342 0.1981 0.5099 0.042 Uiso 1 1 calc R . . H9C H 0.5723 0.1317 0.4512 0.042 Uiso 1 1 calc R . . Si Si 0.84381(5) 0.18858(3) 0.25027(3) 0.01546(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0137(8) 0.0170(9) 0.0189(8) 0.0016(7) -0.0023(6) -0.0014(7) C2 0.0188(9) 0.0183(9) 0.0163(8) 0.0011(7) 0.0000(7) -0.0040(7) C3 0.0212(10) 0.0192(9) 0.0245(10) 0.0010(8) 0.0022(7) -0.0014(8) C4 0.0336(12) 0.0182(9) 0.0228(10) 0.0029(8) 0.0002(8) 0.0013(8) C5 0.0377(12) 0.0208(10) 0.0226(10) 0.0028(8) 0.0016(8) -0.0094(9) C6 0.0234(11) 0.0327(12) 0.0293(11) 0.0065(9) 0.0013(8) -0.0089(9) C7 0.0177(10) 0.0265(10) 0.0285(10) 0.0058(9) -0.0008(8) -0.0023(8) C8 0.0228(10) 0.0189(9) 0.0160(8) 0.0004(7) 0.0009(7) -0.0017(8) C10 0.0356(12) 0.0264(11) 0.0194(9) 0.0015(8) -0.0014(8) 0.0015(9) C11 0.0245(10) 0.0166(9) 0.0182(9) -0.0005(7) -0.0018(7) -0.0036(8) C12 0.0299(12) 0.0279(11) 0.0245(10) -0.0009(9) -0.0072(8) -0.0024(9) C13 0.0320(12) 0.0217(10) 0.0221(10) -0.0025(8) 0.0027(8) 0.0016(9) C14 0.0182(9) 0.0181(9) 0.0148(8) 0.0029(7) 0.0016(7) -0.0008(7) C15 0.0190(9) 0.0151(8) 0.0209(9) 0.0003(7) -0.0020(7) 0.0009(7) C16 0.0241(10) 0.0263(10) 0.0224(10) -0.0020(8) 0.0002(8) 0.0008(8) C17 0.0307(12) 0.0339(12) 0.0246(10) -0.0101(9) -0.0053(9) 0.0042(10) C18 0.0225(11) 0.0254(11) 0.0389(12) -0.0097(9) -0.0064(9) 0.0007(9) C19 0.0184(10) 0.0227(10) 0.0361(11) -0.0011(9) 0.0012(8) -0.0026(8) C20 0.0203(10) 0.0204(9) 0.0222(9) 0.0002(8) 0.0004(7) -0.0023(8) C21 0.0218(10) 0.0151(9) 0.0235(9) -0.0018(7) -0.0008(7) 0.0006(7) C22 0.0314(12) 0.0224(10) 0.0277(11) -0.0014(9) 0.0052(9) 0.0076(9) C23 0.0359(12) 0.0165(9) 0.0277(11) 0.0043(8) -0.0009(9) 0.0018(9) C24 0.0253(11) 0.0258(11) 0.0335(11) 0.0004(9) 0.0094(9) 0.0036(9) C25 0.0173(9) 0.0157(9) 0.0242(9) 0.0003(7) 0.0011(7) 0.0017(7) C26 0.0254(11) 0.0273(11) 0.0299(11) 0.0018(9) -0.0035(8) 0.0071(9) Cl1 0.0259(2) 0.0179(2) 0.0172(2) 0.00252(17) 0.00192(16) -0.00208(18) Cl2 0.0169(2) 0.0217(2) 0.0280(2) 0.00203(19) -0.00159(17) 0.00167(18) N1 0.0201(8) 0.0150(7) 0.0167(7) 0.0009(6) 0.0003(6) -0.0019(6) N2 0.0188(8) 0.0157(7) 0.0173(7) 0.0022(6) 0.0027(6) -0.0005(6) N3 0.0187(8) 0.0150(7) 0.0195(7) 0.0003(6) 0.0004(6) 0.0004(6) N4 0.0164(8) 0.0163(8) 0.0187(7) -0.0003(6) 0.0002(6) 0.0001(6) C9 0.0282(11) 0.0299(11) 0.0275(10) 0.0018(9) 0.0092(9) 0.0048(9) Si 0.0160(2) 0.0138(2) 0.0164(2) 0.00122(19) 0.00001(18) -0.00049(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.316(2) . ? C1 N1 1.342(2) . ? C1 C2 1.488(3) . ? C1 Si 2.3415(19) . ? C2 C3 1.382(3) . ? C2 C7 1.397(3) . ? C3 C4 1.395(3) . ? C4 C5 1.385(3) . ? C5 C6 1.382(3) . ? C6 C7 1.392(3) . ? C8 N2 1.465(2) . ? C8 C10 1.518(3) . ? C8 C9 1.535(3) . ? C11 N1 1.469(2) . ? C11 C12 1.525(3) . ? C11 C13 1.525(3) . ? C14 N4 1.316(2) . ? C14 N3 1.337(2) . ? C14 C15 1.490(3) . ? C14 Si 2.348(2) . ? C15 C16 1.389(3) . ? C15 C20 1.393(3) . ? C16 C17 1.396(3) . ? C17 C18 1.388(3) . ? C18 C19 1.385(3) . ? C19 C20 1.390(3) . ? C21 N3 1.473(2) . ? C21 C22 1.522(3) . ? C21 C23 1.524(3) . ? C24 C25 1.531(3) . ? C25 N4 1.468(2) . ? C25 C26 1.525(3) . ? Cl1 Si 2.2026(7) . ? Cl2 Si 2.1846(7) . ? N1 Si 1.8726(17) . ? N2 Si 1.8984(16) . ? N3 Si 1.8680(17) . ? N4 Si 1.9063(17) . ? 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 C1 N1 107.19(16) . . ? N2 C1 C2 127.78(17) . . ? N1 C1 C2 125.03(17) . . ? N2 C1 Si 54.14(9) . . ? N1 C1 Si 53.06(9) . . ? C2 C1 Si 177.95(14) . . ? C3 C2 C7 119.93(18) . . ? C3 C2 C1 120.47(18) . . ? C7 C2 C1 119.59(18) . . ? C2 C3 C4 120.11(19) . . ? C5 C4 C3 119.9(2) . . ? C6 C5 C4 120.1(2) . . ? C5 C6 C7 120.3(2) . . ? C6 C7 C2 119.6(2) . . ? N2 C8 C10 114.88(16) . . ? N2 C8 C9 110.50(16) . . ? C10 C8 C9 111.20(17) . . ? N1 C11 C12 110.71(17) . . ? N1 C11 C13 111.40(16) . . ? C12 C11 C13 111.46(17) . . ? N4 C14 N3 106.85(16) . . ? N4 C14 C15 128.19(17) . . ? N3 C14 C15 124.92(17) . . ? N4 C14 Si 54.24(10) . . ? N3 C14 Si 52.61(10) . . ? C15 C14 Si 177.15(14) . . ? C16 C15 C20 120.20(18) . . ? C16 C15 C14 121.14(18) . . ? C20 C15 C14 118.62(17) . . ? C15 C16 C17 119.3(2) . . ? C18 C17 C16 120.3(2) . . ? C19 C18 C17 120.4(2) . . ? C18 C19 C20 119.6(2) . . ? C19 C20 C15 120.25(19) . . ? N3 C21 C22 111.32(16) . . ? N3 C21 C23 111.33(16) . . ? C22 C21 C23 111.59(17) . . ? N4 C25 C26 114.63(16) . . ? N4 C25 C24 110.96(16) . . ? C26 C25 C24 111.62(17) . . ? C1 N1 C11 124.26(16) . . ? C1 N1 Si 91.99(12) . . ? C11 N1 Si 141.93(13) . . ? C1 N2 C8 131.25(16) . . ? C1 N2 Si 91.69(12) . . ? C8 N2 Si 136.80(13) . . ? C14 N3 C21 123.39(16) . . ? C14 N3 Si 92.74(12) . . ? C21 N3 Si 142.57(13) . . ? C14 N4 C25 130.69(16) . . ? C14 N4 Si 91.71(12) . . ? C25 N4 Si 136.72(13) . . ? N3 Si N1 159.78(7) . . ? N3 Si N2 96.63(7) . . ? N1 Si N2 69.13(7) . . ? N3 Si N4 68.70(7) . . ? N1 Si N4 96.12(7) . . ? N2 Si N4 89.69(7) . . ? N3 Si Cl2 98.16(6) . . ? N1 Si Cl2 96.39(6) . . ? N2 Si Cl2 90.90(5) . . ? N4 Si Cl2 166.82(6) . . ? N3 Si Cl1 95.75(5) . . ? N1 Si Cl1 97.75(5) . . ? N2 Si Cl1 166.82(6) . . ? N4 Si Cl1 90.61(5) . . ? Cl2 Si Cl1 91.80(3) . . ? N3 Si C1 129.55(7) . . ? N1 Si C1 34.95(7) . . ? N2 Si C1 34.18(7) . . ? N4 Si C1 93.91(7) . . ? Cl2 Si C1 93.96(5) . . ? Cl1 Si C1 132.70(5) . . ? N3 Si C14 34.64(7) . . ? N1 Si C14 128.96(7) . . ? N2 Si C14 93.72(7) . . ? N4 Si C14 34.05(7) . . ? Cl2 Si C14 132.80(5) . . ? Cl1 Si C14 93.89(5) . . ? C1 Si C14 115.05(7) . . ? 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 C1 C2 C3 -101.8(2) . . . . ? N1 C1 C2 C3 78.0(3) . . . . ? Si C1 C2 C3 100(4) . . . . ? N2 C1 C2 C7 77.3(3) . . . . ? N1 C1 C2 C7 -102.8(2) . . . . ? Si C1 C2 C7 -81(4) . . . . ? C7 C2 C3 C4 -1.4(3) . . . . ? C1 C2 C3 C4 177.69(18) . . . . ? C2 C3 C4 C5 0.9(3) . . . . ? C3 C4 C5 C6 0.2(3) . . . . ? C4 C5 C6 C7 -0.8(3) . . . . ? C5 C6 C7 C2 0.3(3) . . . . ? C3 C2 C7 C6 0.9(3) . . . . ? C1 C2 C7 C6 -178.28(19) . . . . ? N4 C14 C15 C16 -113.6(2) . . . . ? N3 C14 C15 C16 68.7(3) . . . . ? Si C14 C15 C16 98(3) . . . . ? N4 C14 C15 C20 68.3(3) . . . . ? N3 C14 C15 C20 -109.3(2) . . . . ? Si C14 C15 C20 -80(3) . . . . ? C20 C15 C16 C17 -1.5(3) . . . . ? C14 C15 C16 C17 -179.57(19) . . . . ? C15 C16 C17 C18 1.9(3) . . . . ? C16 C17 C18 C19 -0.9(3) . . . . ? C17 C18 C19 C20 -0.5(3) . . . . ? C18 C19 C20 C15 0.9(3) . . . . ? C16 C15 C20 C19 0.1(3) . . . . ? C14 C15 C20 C19 178.20(18) . . . . ? N2 C1 N1 C11 -168.68(17) . . . . ? C2 C1 N1 C11 11.4(3) . . . . ? Si C1 N1 C11 -167.6(2) . . . . ? N2 C1 N1 Si -1.05(15) . . . . ? C2 C1 N1 Si 179.06(17) . . . . ? C12 C11 N1 C1 103.4(2) . . . . ? C13 C11 N1 C1 -131.92(19) . . . . ? C12 C11 N1 Si -56.2(3) . . . . ? C13 C11 N1 Si 68.4(3) . . . . ? N1 C1 N2 C8 -173.71(18) . . . . ? C2 C1 N2 C8 6.2(3) . . . . ? Si C1 N2 C8 -174.7(2) . . . . ? N1 C1 N2 Si 1.04(15) . . . . ? C2 C1 N2 Si -179.08(18) . . . . ? C10 C8 N2 C1 35.2(3) . . . . ? C9 C8 N2 C1 -91.6(2) . . . . ? C10 C8 N2 Si -137.08(18) . . . . ? C9 C8 N2 Si 96.1(2) . . . . ? N4 C14 N3 C21 -169.47(16) . . . . ? C15 C14 N3 C21 8.6(3) . . . . ? Si C14 N3 C21 -169.6(2) . . . . ? N4 C14 N3 Si 0.17(15) . . . . ? C15 C14 N3 Si 178.22(16) . . . . ? C22 C21 N3 C14 -112.5(2) . . . . ? C23 C21 N3 C14 122.3(2) . . . . ? C22 C21 N3 Si 84.6(2) . . . . ? C23 C21 N3 Si -40.5(3) . . . . ? N3 C14 N4 C25 -170.60(18) . . . . ? C15 C14 N4 C25 11.4(3) . . . . ? Si C14 N4 C25 -170.4(2) . . . . ? N3 C14 N4 Si -0.17(15) . . . . ? C15 C14 N4 Si -178.13(17) . . . . ? C26 C25 N4 C14 35.5(3) . . . . ? C24 C25 N4 C14 -92.1(2) . . . . ? C26 C25 N4 Si -130.48(18) . . . . ? C24 C25 N4 Si 102.0(2) . . . . ? C14 N3 Si N1 43.2(3) . . . . ? C21 N3 Si N1 -151.1(2) . . . . ? C14 N3 Si N2 86.95(12) . . . . ? C21 N3 Si N2 -107.3(2) . . . . ? C14 N3 Si N4 -0.12(11) . . . . ? C21 N3 Si N4 165.6(2) . . . . ? C14 N3 Si Cl2 178.82(10) . . . . ? C21 N3 Si Cl2 -15.5(2) . . . . ? C14 N3 Si Cl1 -88.53(11) . . . . ? C21 N3 Si Cl1 77.2(2) . . . . ? C14 N3 Si C1 76.75(14) . . . . ? C21 N3 Si C1 -117.5(2) . . . . ? C21 N3 Si C14 165.7(3) . . . . ? C1 N1 Si N3 48.1(3) . . . . ? C11 N1 Si N3 -148.6(2) . . . . ? C1 N1 Si N2 0.74(11) . . . . ? C11 N1 Si N2 164.1(2) . . . . ? C1 N1 Si N4 88.07(12) . . . . ? C11 N1 Si N4 -108.6(2) . . . . ? C1 N1 Si Cl2 -87.78(11) . . . . ? C11 N1 Si Cl2 75.5(2) . . . . ? C1 N1 Si Cl1 179.52(10) . . . . ? C11 N1 Si Cl1 -17.2(2) . . . . ? C11 N1 Si C1 163.3(3) . . . . ? C1 N1 Si C14 78.10(14) . . . . ? C11 N1 Si C14 -118.6(2) . . . . ? C1 N2 Si N3 -165.94(12) . . . . ? C8 N2 Si N3 8.3(2) . . . . ? C1 N2 Si N1 -0.76(11) . . . . ? C8 N2 Si N1 173.5(2) . . . . ? C1 N2 Si N4 -97.43(12) . . . . ? C8 N2 Si N4 76.80(19) . . . . ? C1 N2 Si Cl2 95.74(11) . . . . ? C8 N2 Si Cl2 -90.04(19) . . . . ? C1 N2 Si Cl1 -6.1(3) . . . . ? C8 N2 Si Cl1 168.15(18) . . . . ? C8 N2 Si C1 174.2(3) . . . . ? C1 N2 Si C14 -131.26(12) . . . . ? C8 N2 Si C14 42.96(19) . . . . ? C14 N4 Si N3 0.12(11) . . . . ? C25 N4 Si N3 169.5(2) . . . . ? C14 N4 Si N1 -166.08(11) . . . . ? C25 N4 Si N1 3.32(19) . . . . ? C14 N4 Si N2 -97.12(12) . . . . ? C25 N4 Si N2 72.29(19) . . . . ? C14 N4 Si Cl2 -4.5(3) . . . . ? C25 N4 Si Cl2 164.92(18) . . . . ? C14 N4 Si Cl1 96.06(11) . . . . ? C25 N4 Si Cl1 -94.54(18) . . . . ? C14 N4 Si C1 -131.06(11) . . . . ? C25 N4 Si C1 38.35(19) . . . . ? C25 N4 Si C14 169.4(2) . . . . ? N2 C1 Si N3 18.24(15) . . . . ? N1 C1 Si N3 -160.52(12) . . . . ? C2 C1 Si N3 177(100) . . . . ? N2 C1 Si N1 178.76(18) . . . . ? C2 C1 Si N1 -22(4) . . . . ? N1 C1 Si N2 -178.76(18) . . . . ? C2 C1 Si N2 159(4) . . . . ? N2 C1 Si N4 83.67(12) . . . . ? N1 C1 Si N4 -95.09(12) . . . . ? C2 C1 Si N4 -117(4) . . . . ? N2 C1 Si Cl2 -85.75(11) . . . . ? N1 C1 Si Cl2 95.49(11) . . . . ? C2 C1 Si Cl2 73(4) . . . . ? N2 C1 Si Cl1 178.12(10) . . . . ? N1 C1 Si Cl1 -0.64(14) . . . . ? C2 C1 Si Cl1 -23(4) . . . . ? N2 C1 Si C14 55.89(13) . . . . ? N1 C1 Si C14 -122.87(12) . . . . ? C2 C1 Si C14 -145(4) . . . . ? N4 C14 Si N3 -179.80(18) . . . . ? C15 C14 Si N3 -31(3) . . . . ? N4 C14 Si N1 17.91(14) . . . . ? N3 C14 Si N1 -162.29(12) . . . . ? C15 C14 Si N1 167(3) . . . . ? N4 C14 Si N2 83.92(12) . . . . ? N3 C14 Si N2 -96.28(12) . . . . ? C15 C14 Si N2 -127(3) . . . . ? N3 C14 Si N4 179.80(18) . . . . ? C15 C14 Si N4 149(3) . . . . ? N4 C14 Si Cl2 178.61(10) . . . . ? N3 C14 Si Cl2 -1.60(14) . . . . ? C15 C14 Si Cl2 -32(3) . . . . ? N4 C14 Si Cl1 -85.31(11) . . . . ? N3 C14 Si Cl1 94.48(11) . . . . ? C15 C14 Si Cl1 64(3) . . . . ? N4 C14 Si C1 56.14(13) . . . . ? N3 C14 Si C1 -124.06(12) . . . . ? C15 C14 Si C1 -155(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.453 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.065 # *******************Data Compound 3 ******************* data_jun10u5 _database_code_depnum_ccdc_archive 'CCDC 775532' #TrackingRef '- bisamidinato_si_complexes_dalton_final_28_04_10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H38 F2 N4 Si' _chemical_formula_sum 'C26 H38 F2 N4 Si' _chemical_formula_weight 472.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.1810(7) _cell_length_b 16.4410(13) _cell_length_c 9.7818(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.801(4) _cell_angle_gamma 90.00 _cell_volume 1282.99(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4182 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 30.56 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .30 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .601258 _exptl_absorpt_correction_T_max .717735 _exptl_absorpt_process_details Bruker-TWINABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source rotating_anode _diffrn_radiation_monochromator MONTEL_multi_layer_optics _diffrn_measurement_device_type Bruker-Nonius-Kappa_Apex2_CCD _diffrn_measurement_method omega_and_phi_scans _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4629 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 32.27 _reflns_number_total 4629 _reflns_number_gt 4490 _reflns_threshold_expression >2sigma(I) _computing_data_collection Bruker-SAINT _computing_cell_refinement Bruker-SAINT _computing_data_reduction Bruker-SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/POvray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+0.1416P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.15(9) _refine_ls_number_reflns 4629 _refine_ls_number_parameters 307 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.69403(17) 0.41096(9) 0.96430(15) 0.0116(2) Uani 1 1 d . . . C2 C 0.76766(18) 0.46066(9) 1.08979(16) 0.0121(2) Uani 1 1 d . . . C7 C 0.7034(2) 0.53809(10) 1.10434(18) 0.0182(3) Uani 1 1 d . . . H7 H 0.6158 0.5592 1.0327 0.022 Uiso 1 1 calc R . . C6 C 0.7671(2) 0.58442(10) 1.22306(19) 0.0200(3) Uani 1 1 d . . . H6 H 0.7227 0.6370 1.2326 0.024 Uiso 1 1 calc R . . C5 C 0.8954(2) 0.55389(10) 1.32760(17) 0.0177(3) Uani 1 1 d . . . H5 H 0.9385 0.5854 1.4090 0.021 Uiso 1 1 calc R . . C4 C 0.9607(2) 0.47735(11) 1.31336(18) 0.0204(3) Uani 1 1 d . . . H4 H 1.0495 0.4569 1.3845 0.024 Uiso 1 1 calc R . . C3 C 0.8966(2) 0.43037(10) 1.19527(17) 0.0172(3) Uani 1 1 d . . . H3 H 0.9407 0.3776 1.1866 0.021 Uiso 1 1 calc R . . C8 C 0.84248(19) 0.47448(9) 0.79823(17) 0.0143(3) Uani 1 1 d . . . H8 H 0.9254 0.4908 0.8852 0.017 Uiso 1 1 calc R . . C10 C 0.7527(2) 0.55077(10) 0.7303(2) 0.0208(3) Uani 1 1 d . . . H10A H 0.6639 0.5351 0.6499 0.031 Uiso 1 1 calc R . . H10B H 0.8333 0.5862 0.6987 0.031 Uiso 1 1 calc R . . H10C H 0.7035 0.5798 0.7989 0.031 Uiso 1 1 calc R . . C9 C 0.9362(2) 0.43252(10) 0.69934(18) 0.0170(3) Uani 1 1 d . . . H9A H 0.9809 0.3804 0.7399 0.026 Uiso 1 1 calc R . . H9B H 1.0287 0.4672 0.6859 0.026 Uiso 1 1 calc R . . H9C H 0.8591 0.4229 0.6087 0.026 Uiso 1 1 calc R . . C11 C 0.47960(17) 0.34151(10) 1.06548(15) 0.0129(2) Uani 1 1 d . . . H11 H 0.5440 0.3640 1.1566 0.015 Uiso 1 1 calc R . . C12 C 0.3155(2) 0.38917(11) 1.02215(19) 0.0195(3) Uani 1 1 d . . . H12A H 0.3406 0.4470 1.0140 0.029 Uiso 1 1 calc R . . H12B H 0.2489 0.3820 1.0931 0.029 Uiso 1 1 calc R . . H12C H 0.2521 0.3690 0.9316 0.029 Uiso 1 1 calc R . . C13 C 0.4474(2) 0.25146(10) 1.08596(18) 0.0181(3) Uani 1 1 d . . . H13A H 0.3872 0.2280 0.9969 0.027 Uiso 1 1 calc R . . H13B H 0.3796 0.2453 1.1563 0.027 Uiso 1 1 calc R . . H13C H 0.5545 0.2232 1.1178 0.027 Uiso 1 1 calc R . . C14 C 0.67601(17) 0.26656(9) 0.61600(15) 0.0112(2) Uani 1 1 d . . . C15 C 0.73752(18) 0.21818(9) 0.50974(16) 0.0117(2) Uani 1 1 d . . . C16 C 0.8584(2) 0.24952(10) 0.44348(18) 0.0163(3) Uani 1 1 d . . . H16 H 0.9096 0.3005 0.4718 0.020 Uiso 1 1 calc R . . C17 C 0.9037(2) 0.20585(10) 0.33565(18) 0.0172(3) Uani 1 1 d . . . H17 H 0.9864 0.2269 0.2907 0.021 Uiso 1 1 calc R . . C18 C 0.82818(19) 0.13151(10) 0.29366(17) 0.0150(3) Uani 1 1 d . . . H18 H 0.8580 0.1024 0.2189 0.018 Uiso 1 1 calc R . . C19 C 0.7098(2) 0.09963(10) 0.36017(18) 0.0171(3) Uani 1 1 d . . . H19 H 0.6594 0.0485 0.3320 0.020 Uiso 1 1 calc R . . C20 C 0.66499(19) 0.14298(9) 0.46864(17) 0.0157(3) Uani 1 1 d . . . H20 H 0.5843 0.1210 0.5149 0.019 Uiso 1 1 calc R . . C21 C 0.47154(17) 0.34616(10) 0.44457(15) 0.0122(2) Uani 1 1 d . . . H21 H 0.5261 0.3184 0.3754 0.015 Uiso 1 1 calc R . . C22 C 0.2952(2) 0.31138(11) 0.42818(18) 0.0199(3) Uani 1 1 d . . . H22A H 0.3018 0.2522 0.4404 0.030 Uiso 1 1 calc R . . H22B H 0.2286 0.3243 0.3345 0.030 Uiso 1 1 calc R . . H22C H 0.2419 0.3353 0.4991 0.030 Uiso 1 1 calc R . . C23 C 0.4666(2) 0.43746(10) 0.41359(18) 0.0182(3) Uani 1 1 d . . . H23A H 0.4204 0.4663 0.4842 0.027 Uiso 1 1 calc R . . H23B H 0.3957 0.4475 0.3204 0.027 Uiso 1 1 calc R . . H23C H 0.5804 0.4570 0.4164 0.027 Uiso 1 1 calc R . . C24 C 0.8238(2) 0.19498(9) 0.82721(17) 0.0151(3) Uani 1 1 d . . . H24 H 0.8950 0.1754 0.7629 0.018 Uiso 1 1 calc R . . C25 C 0.7298(3) 0.12244(11) 0.8691(2) 0.0256(4) Uani 1 1 d . . . H25A H 0.6605 0.1405 0.9331 0.038 Uiso 1 1 calc R . . H25B H 0.8105 0.0817 0.9159 0.038 Uiso 1 1 calc R . . H25C H 0.6581 0.0985 0.7851 0.038 Uiso 1 1 calc R . . C26 C 0.9379(2) 0.23273(11) 0.95606(19) 0.0219(3) Uani 1 1 d . . . H26A H 0.9967 0.2795 0.9275 0.033 Uiso 1 1 calc R . . H26B H 1.0200 0.1923 1.0018 0.033 Uiso 1 1 calc R . . H26C H 0.8705 0.2506 1.0217 0.033 Uiso 1 1 calc R . . F1 F 0.39370(12) 0.27087(6) 0.75523(10) 0.01430(18) Uani 1 1 d . . . F2 F 0.40437(12) 0.41566(6) 0.72907(10) 0.01422(18) Uani 1 1 d . . . N2 N 0.72140(16) 0.41853(8) 0.83708(14) 0.0127(2) Uani 1 1 d . . . N1 N 0.58158(15) 0.35143(7) 0.96045(13) 0.0112(2) Uani 1 1 d . . . N3 N 0.57162(15) 0.32978(7) 0.58486(13) 0.0111(2) Uani 1 1 d . . . N4 N 0.70638(16) 0.25543(8) 0.75283(14) 0.0122(2) Uani 1 1 d . . . Si Si 0.54080(4) 0.34034(2) 0.76649(4) 0.00986(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0124(5) 0.0097(5) 0.0125(6) -0.0013(5) 0.0027(5) 0.0009(4) C2 0.0139(5) 0.0108(6) 0.0118(6) -0.0023(5) 0.0033(5) -0.0013(4) C7 0.0203(6) 0.0149(6) 0.0175(7) -0.0028(6) 0.0001(6) 0.0038(5) C6 0.0264(8) 0.0140(7) 0.0190(7) -0.0046(6) 0.0036(6) 0.0009(6) C5 0.0213(7) 0.0166(6) 0.0149(7) -0.0050(6) 0.0036(6) -0.0050(5) C4 0.0214(7) 0.0205(7) 0.0164(7) -0.0031(6) -0.0021(6) 0.0018(6) C3 0.0202(7) 0.0144(7) 0.0155(7) -0.0015(5) 0.0009(5) 0.0030(5) C8 0.0147(6) 0.0124(6) 0.0162(7) -0.0015(5) 0.0044(5) -0.0030(5) C10 0.0215(7) 0.0133(7) 0.0288(9) 0.0028(6) 0.0083(6) -0.0016(6) C9 0.0161(6) 0.0172(7) 0.0197(7) -0.0012(6) 0.0079(5) -0.0033(5) C11 0.0155(5) 0.0128(5) 0.0112(5) -0.0006(5) 0.0051(5) -0.0023(5) C12 0.0169(6) 0.0229(7) 0.0204(7) 0.0000(6) 0.0078(6) 0.0029(6) C13 0.0239(7) 0.0152(6) 0.0168(7) 0.0005(5) 0.0080(6) -0.0037(6) C14 0.0116(5) 0.0095(5) 0.0127(6) -0.0012(5) 0.0031(5) -0.0011(4) C15 0.0124(5) 0.0107(6) 0.0121(6) -0.0009(5) 0.0028(5) 0.0003(4) C16 0.0179(6) 0.0145(6) 0.0177(7) -0.0034(5) 0.0066(5) -0.0040(5) C17 0.0175(6) 0.0174(6) 0.0183(7) -0.0011(6) 0.0076(6) -0.0003(5) C18 0.0160(6) 0.0152(6) 0.0137(6) -0.0021(5) 0.0031(5) 0.0039(5) C19 0.0221(7) 0.0127(6) 0.0172(7) -0.0039(5) 0.0063(6) -0.0013(5) C20 0.0192(6) 0.0121(6) 0.0176(7) -0.0018(5) 0.0078(6) -0.0026(5) C21 0.0148(5) 0.0129(6) 0.0088(5) 0.0001(5) 0.0022(5) 0.0013(5) C22 0.0158(6) 0.0242(7) 0.0172(7) 0.0030(6) -0.0016(5) -0.0039(6) C23 0.0257(7) 0.0135(6) 0.0147(7) 0.0033(5) 0.0030(6) 0.0004(5) C24 0.0176(6) 0.0132(6) 0.0144(7) 0.0021(5) 0.0030(5) 0.0038(5) C25 0.0342(9) 0.0142(7) 0.0247(8) 0.0051(6) -0.0013(7) -0.0033(6) C26 0.0205(7) 0.0212(7) 0.0199(7) 0.0044(6) -0.0041(6) -0.0012(6) F1 0.0150(4) 0.0143(4) 0.0138(4) -0.0010(3) 0.0036(3) -0.0044(3) F2 0.0156(4) 0.0129(4) 0.0142(4) 0.0009(3) 0.0035(3) 0.0041(3) N2 0.0149(5) 0.0114(5) 0.0122(5) -0.0014(4) 0.0043(4) -0.0032(4) N1 0.0131(5) 0.0108(5) 0.0102(5) -0.0010(4) 0.0036(4) -0.0011(4) N3 0.0136(5) 0.0092(5) 0.0102(5) -0.0006(4) 0.0020(4) 0.0009(4) N4 0.0146(5) 0.0109(5) 0.0109(5) -0.0005(4) 0.0025(4) 0.0008(4) Si 0.01128(14) 0.00892(14) 0.00953(15) -0.00022(13) 0.00260(13) -0.00051(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.318(2) . ? C1 N1 1.3380(18) . ? C1 C2 1.487(2) . ? C1 Si 2.3640(15) . ? C2 C3 1.394(2) . ? C2 C7 1.396(2) . ? C7 C6 1.390(2) . ? C6 C5 1.387(2) . ? C5 C4 1.386(2) . ? C4 C3 1.392(2) . ? C8 N2 1.462(2) . ? C8 C9 1.526(2) . ? C8 C10 1.529(2) . ? C11 N1 1.4690(18) . ? C11 C13 1.525(2) . ? C11 C12 1.531(2) . ? C14 N4 1.3189(19) . ? C14 N3 1.3369(18) . ? C14 C15 1.482(2) . ? C14 Si 2.3630(15) . ? C15 C20 1.392(2) . ? C15 C16 1.396(2) . ? C16 C17 1.392(2) . ? C17 C18 1.390(2) . ? C18 C19 1.384(2) . ? C19 C20 1.393(2) . ? C21 N3 1.4588(18) . ? C21 C22 1.527(2) . ? C21 C23 1.530(2) . ? C24 N4 1.4597(19) . ? C24 C25 1.523(2) . ? C24 C26 1.524(2) . ? F1 Si 1.6451(10) . ? F2 Si 1.6529(10) . ? N2 Si 1.9647(13) . ? N1 Si 1.8611(13) . ? N3 Si 1.8571(14) . ? N4 Si 1.9703(13) . ? 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 C1 N1 107.58(13) . . ? N2 C1 C2 127.23(13) . . ? N1 C1 C2 125.15(13) . . ? N2 C1 Si 56.21(8) . . ? N1 C1 Si 51.77(7) . . ? C2 C1 Si 171.99(11) . . ? C3 C2 C7 119.37(14) . . ? C3 C2 C1 121.10(13) . . ? C7 C2 C1 119.50(13) . . ? C6 C7 C2 120.33(15) . . ? C5 C6 C7 119.98(15) . . ? C4 C5 C6 120.00(15) . . ? C5 C4 C3 120.30(15) . . ? C4 C3 C2 120.01(15) . . ? N2 C8 C9 110.16(13) . . ? N2 C8 C10 109.95(13) . . ? C9 C8 C10 110.85(14) . . ? N1 C11 C13 109.95(13) . . ? N1 C11 C12 110.40(13) . . ? C13 C11 C12 111.52(13) . . ? N4 C14 N3 107.83(13) . . ? N4 C14 C15 128.33(13) . . ? N3 C14 C15 123.80(13) . . ? N4 C14 Si 56.49(8) . . ? N3 C14 Si 51.62(7) . . ? C15 C14 Si 172.15(10) . . ? C20 C15 C16 119.63(14) . . ? C20 C15 C14 119.34(13) . . ? C16 C15 C14 120.87(13) . . ? C17 C16 C15 119.76(15) . . ? C18 C17 C16 120.12(16) . . ? C19 C18 C17 120.38(15) . . ? C18 C19 C20 119.60(15) . . ? C15 C20 C19 120.48(15) . . ? N3 C21 C22 110.48(12) . . ? N3 C21 C23 110.62(12) . . ? C22 C21 C23 111.31(13) . . ? N4 C24 C25 110.56(13) . . ? N4 C24 C26 110.47(13) . . ? C25 C24 C26 110.47(15) . . ? C1 N2 C8 124.84(13) . . ? C1 N2 Si 89.90(9) . . ? C8 N2 Si 145.10(11) . . ? C1 N1 C11 123.71(12) . . ? C1 N1 Si 93.85(9) . . ? C11 N1 Si 134.49(9) . . ? C14 N3 C21 123.70(12) . . ? C14 N3 Si 94.02(9) . . ? C21 N3 Si 135.71(10) . . ? C14 N4 C24 123.74(13) . . ? C14 N4 Si 89.59(9) . . ? C24 N4 Si 146.64(11) . . ? F1 Si F2 93.28(5) . . ? F1 Si N3 97.09(5) . . ? F2 Si N3 94.95(5) . . ? F1 Si N1 95.71(5) . . ? F2 Si N1 96.44(6) . . ? N3 Si N1 162.32(5) . . ? F1 Si N2 163.70(6) . . ? F2 Si N2 90.34(6) . . ? N3 Si N2 98.43(6) . . ? N1 Si N2 68.08(6) . . ? F1 Si N4 90.41(6) . . ? F2 Si N4 163.04(6) . . ? N3 Si N4 68.15(5) . . ? N1 Si N4 99.66(6) . . ? N2 Si N4 90.73(5) . . ? F1 Si C14 92.20(5) . . ? F2 Si C14 129.27(5) . . ? N3 Si C14 34.36(5) . . ? N1 Si C14 133.03(5) . . ? N2 Si C14 97.79(5) . . ? N4 Si C14 33.93(5) . . ? F1 Si C1 130.03(6) . . ? F2 Si C1 91.31(5) . . ? N3 Si C1 132.01(6) . . ? N1 Si C1 34.38(5) . . ? N2 Si C1 33.89(5) . . ? N4 Si C1 98.95(5) . . ? C14 Si C1 121.70(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 C3 -103.67(19) . . . . ? N1 C1 C2 C3 78.9(2) . . . . ? Si C1 C2 C3 143.5(7) . . . . ? N2 C1 C2 C7 78.2(2) . . . . ? N1 C1 C2 C7 -99.24(19) . . . . ? Si C1 C2 C7 -34.6(9) . . . . ? C3 C2 C7 C6 -0.2(3) . . . . ? C1 C2 C7 C6 177.95(16) . . . . ? C2 C7 C6 C5 0.2(3) . . . . ? C7 C6 C5 C4 0.3(3) . . . . ? C6 C5 C4 C3 -0.8(3) . . . . ? C5 C4 C3 C2 0.9(3) . . . . ? C7 C2 C3 C4 -0.3(2) . . . . ? C1 C2 C3 C4 -178.44(16) . . . . ? N4 C14 C15 C20 76.3(2) . . . . ? N3 C14 C15 C20 -101.34(18) . . . . ? Si C14 C15 C20 -49.2(8) . . . . ? N4 C14 C15 C16 -108.24(19) . . . . ? N3 C14 C15 C16 74.08(19) . . . . ? Si C14 C15 C16 126.2(7) . . . . ? C20 C15 C16 C17 0.9(2) . . . . ? C14 C15 C16 C17 -174.53(15) . . . . ? C15 C16 C17 C18 0.3(2) . . . . ? C16 C17 C18 C19 -1.2(2) . . . . ? C17 C18 C19 C20 0.8(2) . . . . ? C16 C15 C20 C19 -1.3(2) . . . . ? C14 C15 C20 C19 174.21(14) . . . . ? C18 C19 C20 C15 0.4(2) . . . . ? N1 C1 N2 C8 -176.94(13) . . . . ? C2 C1 N2 C8 5.2(2) . . . . ? Si C1 N2 C8 176.34(17) . . . . ? N1 C1 N2 Si 6.72(12) . . . . ? C2 C1 N2 Si -171.11(13) . . . . ? C9 C8 N2 C1 138.07(16) . . . . ? C10 C8 N2 C1 -99.48(18) . . . . ? C9 C8 N2 Si -48.3(2) . . . . ? C10 C8 N2 Si 74.1(2) . . . . ? N2 C1 N1 C11 -159.89(13) . . . . ? C2 C1 N1 C11 18.0(2) . . . . ? Si C1 N1 C11 -152.78(15) . . . . ? N2 C1 N1 Si -7.11(12) . . . . ? C2 C1 N1 Si 170.77(12) . . . . ? C13 C11 N1 C1 -146.90(14) . . . . ? C12 C11 N1 C1 89.64(16) . . . . ? C13 C11 N1 Si 72.88(17) . . . . ? C12 C11 N1 Si -50.6(2) . . . . ? N4 C14 N3 C21 -161.41(13) . . . . ? C15 C14 N3 C21 16.7(2) . . . . ? Si C14 N3 C21 -155.42(15) . . . . ? N4 C14 N3 Si -5.99(12) . . . . ? C15 C14 N3 Si 172.10(12) . . . . ? C22 C21 N3 C14 95.87(17) . . . . ? C23 C21 N3 C14 -140.42(14) . . . . ? C22 C21 N3 Si -47.7(2) . . . . ? C23 C21 N3 Si 76.04(17) . . . . ? N3 C14 N4 C24 -175.93(13) . . . . ? C15 C14 N4 C24 6.1(2) . . . . ? Si C14 N4 C24 178.44(16) . . . . ? N3 C14 N4 Si 5.63(11) . . . . ? C15 C14 N4 Si -172.34(14) . . . . ? C25 C24 N4 C14 -104.39(18) . . . . ? C26 C24 N4 C14 133.02(16) . . . . ? C25 C24 N4 Si 72.8(2) . . . . ? C26 C24 N4 Si -49.8(2) . . . . ? C14 N3 Si F1 -83.49(9) . . . . ? C21 N3 Si F1 66.81(15) . . . . ? C14 N3 Si F2 -177.43(9) . . . . ? C21 N3 Si F2 -27.13(15) . . . . ? C14 N3 Si N1 52.6(2) . . . . ? C21 N3 Si N1 -157.11(18) . . . . ? C14 N3 Si N2 91.49(9) . . . . ? C21 N3 Si N2 -118.21(14) . . . . ? C14 N3 Si N4 4.11(8) . . . . ? C21 N3 Si N4 154.40(15) . . . . ? C21 N3 Si C14 150.30(19) . . . . ? C14 N3 Si C1 86.31(10) . . . . ? C21 N3 Si C1 -123.39(14) . . . . ? C1 N1 Si F1 -176.84(9) . . . . ? C11 N1 Si F1 -29.08(15) . . . . ? C1 N1 Si F2 -82.88(9) . . . . ? C11 N1 Si F2 64.89(15) . . . . ? C1 N1 Si N3 46.9(2) . . . . ? C11 N1 Si N3 -165.30(17) . . . . ? C1 N1 Si N2 4.89(9) . . . . ? C11 N1 Si N2 152.66(16) . . . . ? C1 N1 Si N4 91.76(9) . . . . ? C11 N1 Si N4 -120.48(15) . . . . ? C1 N1 Si C14 84.76(10) . . . . ? C11 N1 Si C14 -127.48(14) . . . . ? C11 N1 Si C1 147.76(19) . . . . ? C1 N2 Si F1 -11.1(3) . . . . ? C8 N2 Si F1 174.12(17) . . . . ? C1 N2 Si F2 91.85(10) . . . . ? C8 N2 Si F2 -82.91(19) . . . . ? C1 N2 Si N3 -173.09(9) . . . . ? C8 N2 Si N3 12.15(19) . . . . ? C1 N2 Si N1 -4.96(9) . . . . ? C8 N2 Si N1 -179.7(2) . . . . ? C1 N2 Si N4 -105.08(10) . . . . ? C8 N2 Si N4 80.16(19) . . . . ? C1 N2 Si C14 -138.38(9) . . . . ? C8 N2 Si C14 46.86(19) . . . . ? C8 N2 Si C1 -174.8(2) . . . . ? C14 N4 Si F1 93.32(9) . . . . ? C24 N4 Si F1 -84.32(19) . . . . ? C14 N4 Si F2 -9.4(2) . . . . ? C24 N4 Si F2 172.97(17) . . . . ? C14 N4 Si N3 -4.15(8) . . . . ? C24 N4 Si N3 178.2(2) . . . . ? C14 N4 Si N1 -170.82(9) . . . . ? C24 N4 Si N1 11.54(19) . . . . ? C14 N4 Si N2 -102.94(9) . . . . ? C24 N4 Si N2 79.42(19) . . . . ? C24 N4 Si C14 -177.6(2) . . . . ? C14 N4 Si C1 -135.97(9) . . . . ? C24 N4 Si C1 46.39(19) . . . . ? N4 C14 Si F1 -87.48(9) . . . . ? N3 C14 Si F1 99.36(9) . . . . ? C15 C14 Si F1 42.6(8) . . . . ? N4 C14 Si F2 176.48(9) . . . . ? N3 C14 Si F2 3.31(11) . . . . ? C15 C14 Si F2 -53.4(8) . . . . ? N4 C14 Si N3 173.16(14) . . . . ? C15 C14 Si N3 -56.8(8) . . . . ? N4 C14 Si N1 12.43(12) . . . . ? N3 C14 Si N1 -160.73(9) . . . . ? C15 C14 Si N1 142.5(8) . . . . ? N4 C14 Si N2 79.61(10) . . . . ? N3 C14 Si N2 -93.56(9) . . . . ? C15 C14 Si N2 -150.3(8) . . . . ? N3 C14 Si N4 -173.16(14) . . . . ? C15 C14 Si N4 130.1(8) . . . . ? N4 C14 Si C1 53.80(11) . . . . ? N3 C14 Si C1 -119.36(9) . . . . ? C15 C14 Si C1 -176.1(8) . . . . ? N2 C1 Si F1 175.94(9) . . . . ? N1 C1 Si F1 4.10(11) . . . . ? C2 C1 Si F1 -66.1(8) . . . . ? N2 C1 Si F2 -88.66(10) . . . . ? N1 C1 Si F2 99.50(9) . . . . ? C2 C1 Si F2 29.3(8) . . . . ? N2 C1 Si N3 9.21(12) . . . . ? N1 C1 Si N3 -162.63(9) . . . . ? C2 C1 Si N3 127.2(8) . . . . ? N2 C1 Si N1 171.84(14) . . . . ? C2 C1 Si N1 -70.2(8) . . . . ? N1 C1 Si N2 -171.84(14) . . . . ? C2 C1 Si N2 118.0(8) . . . . ? N2 C1 Si N4 77.79(10) . . . . ? N1 C1 Si N4 -94.05(9) . . . . ? C2 C1 Si N4 -164.2(8) . . . . ? N2 C1 Si C14 50.66(11) . . . . ? N1 C1 Si C14 -121.18(9) . . . . ? C2 C1 Si C14 168.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 32.27 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.328 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.051 # *******************Data Compound 4 ******************* data_jun06u _database_code_depnum_ccdc_archive 'CCDC 775533' #TrackingRef '- bisamidinato_si_complexes_dalton_final_28_04_10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H38 N6 Si' _chemical_formula_sum 'C28 H38 N6 Si' _chemical_formula_weight 486.73 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6880(19) _cell_length_b 18.094(4) _cell_length_c 16.310(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.40(3) _cell_angle_gamma 90.00 _cell_volume 2846.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 3884 _cell_measurement_theta_min 5.05 _cell_measurement_theta_max 25.7 _exptl_crystal_description long_prism _exptl_crystal_colour colorless _exptl_crystal_size_max .4 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9121 _exptl_absorpt_correction_T_max 1.0069 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37540 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 29.15 _reflns_number_total 7599 _reflns_number_gt 5301 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.1377P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7599 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 C30 C 0.90648(13) 0.21237(7) 0.64674(8) 0.0271(3) Uani 1 1 d . . . C29 C 0.66607(13) 0.21414(7) 0.72536(8) 0.0279(3) Uani 1 1 d . . . C1 C 1.05337(12) 0.23696(7) 0.82199(7) 0.0237(2) Uani 1 1 d . . . C2 C 1.17638(12) 0.27646(7) 0.86284(8) 0.0258(3) Uani 1 1 d . . . C7 C 1.28374(13) 0.29657(8) 0.81620(9) 0.0305(3) Uani 1 1 d . . . H7 H 1.2790 0.2842 0.7594 0.037 Uiso 1 1 calc R . . C6 C 1.39775(14) 0.33477(9) 0.85294(11) 0.0399(3) Uani 1 1 d . . . H6 H 1.4699 0.3496 0.8209 0.048 Uiso 1 1 calc R . . C5 C 1.40640(15) 0.35127(10) 0.93585(11) 0.0460(4) Uani 1 1 d . . . H5 H 1.4853 0.3766 0.9609 0.055 Uiso 1 1 calc R . . C4 C 1.30049(17) 0.33099(10) 0.98276(10) 0.0470(4) Uani 1 1 d . . . H4 H 1.3074 0.3421 1.0399 0.056 Uiso 1 1 calc R . . C3 C 1.18376(15) 0.29436(9) 0.94637(9) 0.0369(3) Uani 1 1 d . . . H3 H 1.1099 0.2817 0.9781 0.044 Uiso 1 1 calc R . . C12 C 0.83061(18) 0.37936(8) 0.73852(10) 0.0421(4) Uani 1 1 d . . . H12A H 0.8924 0.3706 0.6953 0.063 Uiso 1 1 calc R . . H12B H 0.8190 0.4327 0.7459 0.063 Uiso 1 1 calc R . . H12C H 0.7401 0.3567 0.7226 0.063 Uiso 1 1 calc R . . C11 C 0.89351(13) 0.34510(7) 0.81935(8) 0.0280(3) Uani 1 1 d . . . H11 H 0.9825 0.3714 0.8361 0.034 Uiso 1 1 calc R . . C13 C 0.79935(18) 0.35502(9) 0.88779(10) 0.0438(4) Uani 1 1 d . . . H13A H 0.7125 0.3281 0.8739 0.066 Uiso 1 1 calc R . . H13B H 0.7792 0.4077 0.8942 0.066 Uiso 1 1 calc R . . H13C H 0.8455 0.3357 0.9394 0.066 Uiso 1 1 calc R . . C10 C 1.23996(16) 0.11062(9) 0.72702(11) 0.0429(4) Uani 1 1 d . . . H10A H 1.1826 0.1163 0.6746 0.064 Uiso 1 1 calc R . . H10B H 1.2930 0.0646 0.7263 0.064 Uiso 1 1 calc R . . H10C H 1.3040 0.1525 0.7349 0.064 Uiso 1 1 calc R . . C8 C 1.14704(13) 0.10834(8) 0.79754(9) 0.0307(3) Uani 1 1 d . . . H8 H 1.0918 0.0617 0.7902 0.037 Uiso 1 1 calc R . . C9 C 1.23037(17) 0.10236(10) 0.88141(11) 0.0464(4) Uani 1 1 d . . . H9A H 1.2968 0.1432 0.8881 0.070 Uiso 1 1 calc R . . H9B H 1.2805 0.0552 0.8850 0.070 Uiso 1 1 calc R . . H9C H 1.1674 0.1048 0.9249 0.070 Uiso 1 1 calc R . . C14 C 0.78097(12) 0.06870(7) 0.80504(8) 0.0240(2) Uani 1 1 d . . . C15 C 0.73024(13) -0.00299(7) 0.83495(8) 0.0262(3) Uani 1 1 d . . . C20 C 0.59039(14) -0.01248(9) 0.84585(10) 0.0395(3) Uani 1 1 d . . . H20 H 0.5261 0.0263 0.8324 0.047 Uiso 1 1 calc R . . C19 C 0.54570(17) -0.07908(10) 0.87653(11) 0.0491(4) Uani 1 1 d . . . H19 H 0.4502 -0.0859 0.8833 0.059 Uiso 1 1 calc R . . C18 C 0.63841(19) -0.13551(9) 0.89727(10) 0.0450(4) Uani 1 1 d . . . H18 H 0.6069 -0.1805 0.9191 0.054 Uiso 1 1 calc R . . C17 C 0.77686(18) -0.12647(8) 0.88629(9) 0.0401(3) Uani 1 1 d . . . H17 H 0.8407 -0.1653 0.9004 0.048 Uiso 1 1 calc R . . C16 C 0.82293(14) -0.06051(8) 0.85460(9) 0.0334(3) Uani 1 1 d . . . H16 H 0.9181 -0.0547 0.8463 0.040 Uiso 1 1 calc R . . C22 C 0.91148(17) 0.02285(9) 0.60955(10) 0.0423(4) Uani 1 1 d . . . H22A H 0.9336 0.0704 0.5851 0.064 Uiso 1 1 calc R . . H22B H 0.8912 -0.0137 0.5658 0.064 Uiso 1 1 calc R . . H22C H 0.9908 0.0061 0.6467 0.064 Uiso 1 1 calc R . . C21 C 0.78526(14) 0.03181(8) 0.65788(8) 0.0311(3) Uani 1 1 d . . . H21 H 0.7617 -0.0178 0.6797 0.037 Uiso 1 1 calc R . . C23 C 0.65979(18) 0.05934(11) 0.60194(11) 0.0493(4) Uani 1 1 d . . . H23A H 0.5780 0.0605 0.6330 0.074 Uiso 1 1 calc R . . H23B H 0.6426 0.0259 0.5548 0.074 Uiso 1 1 calc R . . H23C H 0.6785 0.1092 0.5823 0.074 Uiso 1 1 calc R . . C25 C 0.64484(17) 0.16919(11) 0.95148(11) 0.0478(4) Uani 1 1 d . . . H25A H 0.6088 0.2060 0.9109 0.072 Uiso 1 1 calc R . . H25B H 0.6461 0.1901 1.0070 0.072 Uiso 1 1 calc R . . H25C H 0.5853 0.1253 0.9473 0.072 Uiso 1 1 calc R . . C24 C 0.79181(14) 0.14759(8) 0.93478(8) 0.0296(3) Uani 1 1 d . . . H24 H 0.8510 0.1922 0.9474 0.036 Uiso 1 1 calc R . . C26 C 0.84929(19) 0.08686(9) 0.99342(9) 0.0435(4) Uani 1 1 d . . . H26A H 0.7859 0.0446 0.9897 0.065 Uiso 1 1 calc R . . H26B H 0.8585 0.1058 1.0500 0.065 Uiso 1 1 calc R . . H26C H 0.9404 0.0713 0.9783 0.065 Uiso 1 1 calc R . . N6 N 0.93935(14) 0.23329(8) 0.58496(8) 0.0398(3) Uani 1 1 d . . . N5 N 0.55310(12) 0.23081(8) 0.70729(9) 0.0441(3) Uani 1 1 d . . . N1 N 0.92598(10) 0.26670(6) 0.80768(6) 0.0231(2) Uani 1 1 d . . . N2 N 1.04641(10) 0.16918(6) 0.79120(7) 0.0248(2) Uani 1 1 d . . . N4 N 0.79994(10) 0.13095(6) 0.84719(6) 0.0241(2) Uani 1 1 d . . . N3 N 0.81601(10) 0.08170(6) 0.72851(6) 0.0247(2) Uani 1 1 d . . . Si Si 0.85546(3) 0.181147(19) 0.75390(2) 0.02148(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C30 0.0294(6) 0.0260(6) 0.0263(6) 0.0022(5) 0.0040(5) -0.0004(5) C29 0.0261(6) 0.0264(7) 0.0311(6) 0.0043(5) 0.0022(5) -0.0006(5) C1 0.0226(5) 0.0264(6) 0.0225(6) 0.0038(5) 0.0040(4) -0.0001(4) C2 0.0224(5) 0.0270(6) 0.0276(6) 0.0020(5) 0.0009(4) 0.0007(5) C7 0.0260(6) 0.0345(7) 0.0311(7) 0.0024(6) 0.0031(5) -0.0021(5) C6 0.0255(6) 0.0416(9) 0.0526(9) 0.0007(7) 0.0038(6) -0.0057(6) C5 0.0303(7) 0.0460(9) 0.0592(10) -0.0133(8) -0.0091(7) -0.0045(6) C4 0.0468(9) 0.0568(11) 0.0355(8) -0.0138(8) -0.0055(7) 0.0002(7) C3 0.0351(7) 0.0454(9) 0.0306(7) -0.0032(6) 0.0047(5) -0.0011(6) C12 0.0566(9) 0.0268(7) 0.0419(8) 0.0076(6) -0.0004(7) 0.0020(6) C11 0.0266(6) 0.0220(6) 0.0352(7) -0.0014(5) 0.0018(5) 0.0002(5) C13 0.0533(9) 0.0369(9) 0.0434(9) -0.0012(7) 0.0153(7) 0.0132(7) C10 0.0389(7) 0.0423(9) 0.0496(9) -0.0016(7) 0.0154(6) 0.0081(6) C8 0.0271(6) 0.0279(7) 0.0373(7) 0.0019(6) 0.0043(5) 0.0051(5) C9 0.0424(8) 0.0464(10) 0.0485(9) 0.0076(8) -0.0053(7) 0.0134(7) C14 0.0213(5) 0.0252(6) 0.0251(6) 0.0039(5) -0.0008(4) -0.0006(4) C15 0.0285(6) 0.0255(6) 0.0238(6) 0.0023(5) -0.0008(5) -0.0047(5) C20 0.0293(6) 0.0416(8) 0.0467(9) 0.0115(7) -0.0015(6) -0.0066(6) C19 0.0393(8) 0.0539(10) 0.0534(10) 0.0120(8) 0.0010(7) -0.0211(7) C18 0.0664(10) 0.0333(8) 0.0348(8) 0.0061(6) 0.0013(7) -0.0217(7) C17 0.0607(9) 0.0254(7) 0.0338(7) 0.0042(6) 0.0026(7) 0.0016(6) C16 0.0359(7) 0.0294(7) 0.0349(7) 0.0033(6) 0.0042(5) 0.0016(5) C22 0.0572(9) 0.0351(8) 0.0356(8) -0.0070(6) 0.0086(7) 0.0040(7) C21 0.0400(7) 0.0262(7) 0.0259(6) -0.0010(5) -0.0025(5) -0.0036(5) C23 0.0515(9) 0.0512(10) 0.0409(9) -0.0076(8) -0.0170(7) 0.0011(7) C25 0.0473(9) 0.0532(11) 0.0461(9) 0.0013(8) 0.0213(7) 0.0056(7) C24 0.0357(6) 0.0296(7) 0.0242(6) 0.0006(5) 0.0068(5) -0.0028(5) C26 0.0621(10) 0.0424(9) 0.0252(7) 0.0034(6) -0.0014(7) 0.0017(7) N6 0.0496(7) 0.0381(7) 0.0332(6) 0.0064(5) 0.0116(5) -0.0012(6) N5 0.0294(6) 0.0442(8) 0.0578(8) 0.0068(7) -0.0005(5) 0.0050(5) N1 0.0205(4) 0.0219(5) 0.0272(5) 0.0012(4) 0.0032(4) -0.0005(4) N2 0.0217(5) 0.0247(5) 0.0281(5) 0.0013(4) 0.0022(4) 0.0014(4) N4 0.0259(5) 0.0238(5) 0.0228(5) 0.0027(4) 0.0033(4) -0.0026(4) N3 0.0280(5) 0.0224(5) 0.0234(5) 0.0015(4) 0.0008(4) -0.0026(4) Si 0.02075(15) 0.02147(16) 0.02236(16) 0.00268(13) 0.00267(11) -0.00028(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C30 N6 1.1491(18) . ? C30 Si 1.9444(14) . ? C29 N5 1.1467(17) . ? C29 Si 1.9440(13) . ? C1 N2 1.3245(17) . ? C1 N1 1.3465(15) . ? C1 C2 1.4919(17) . ? C1 Si 2.3514(13) . ? C2 C7 1.3935(18) . ? C2 C3 1.3956(19) . ? C7 C6 1.3901(19) . ? C6 C5 1.380(2) . ? C5 C4 1.386(3) . ? C4 C3 1.394(2) . ? C12 C11 1.531(2) . ? C11 N1 1.4692(17) . ? C11 C13 1.517(2) . ? C10 C8 1.526(2) . ? C8 N2 1.4676(16) . ? C8 C9 1.525(2) . ? C14 N4 1.3234(17) . ? C14 N3 1.3446(16) . ? C14 C15 1.4856(18) . ? C14 Si 2.3386(13) . ? C15 C16 1.3922(19) . ? C15 C20 1.3936(19) . ? C20 C19 1.390(2) . ? C19 C18 1.381(3) . ? C18 C17 1.380(2) . ? C17 C16 1.391(2) . ? C22 C21 1.525(2) . ? C21 N3 1.4719(17) . ? C21 C23 1.533(2) . ? C25 C24 1.526(2) . ? C24 N4 1.4694(16) . ? C24 C26 1.527(2) . ? N1 Si 1.8761(11) . ? N2 Si 1.9046(11) . ? N4 Si 1.8930(11) . ? N3 Si 1.8776(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 C30 Si 177.18(13) . . ? N5 C29 Si 177.23(13) . . ? N2 C1 N1 106.93(10) . . ? N2 C1 C2 128.54(11) . . ? N1 C1 C2 124.51(11) . . ? N2 C1 Si 54.06(6) . . ? N1 C1 Si 52.87(6) . . ? C2 C1 Si 176.70(9) . . ? C7 C2 C3 120.00(12) . . ? C7 C2 C1 119.15(12) . . ? C3 C2 C1 120.84(12) . . ? C6 C7 C2 119.88(13) . . ? C5 C6 C7 120.17(14) . . ? C6 C5 C4 120.26(14) . . ? C5 C4 C3 120.25(15) . . ? C4 C3 C2 119.40(14) . . ? N1 C11 C13 111.13(11) . . ? N1 C11 C12 110.62(11) . . ? C13 C11 C12 111.56(12) . . ? N2 C8 C9 114.11(12) . . ? N2 C8 C10 111.20(12) . . ? C9 C8 C10 112.19(12) . . ? N4 C14 N3 107.36(11) . . ? N4 C14 C15 127.34(11) . . ? N3 C14 C15 125.30(12) . . ? N4 C14 Si 54.01(6) . . ? N3 C14 Si 53.38(6) . . ? C15 C14 Si 178.03(9) . . ? C16 C15 C20 119.49(13) . . ? C16 C15 C14 120.14(11) . . ? C20 C15 C14 120.34(12) . . ? C19 C20 C15 119.50(15) . . ? C18 C19 C20 120.80(15) . . ? C17 C18 C19 119.90(14) . . ? C18 C17 C16 120.00(15) . . ? C17 C16 C15 120.30(14) . . ? N3 C21 C22 110.90(11) . . ? N3 C21 C23 110.93(12) . . ? C22 C21 C23 110.88(13) . . ? N4 C24 C25 111.24(12) . . ? N4 C24 C26 114.32(12) . . ? C25 C24 C26 111.35(13) . . ? C1 N1 C11 124.57(10) . . ? C1 N1 Si 92.22(8) . . ? C11 N1 Si 141.65(8) . . ? C1 N2 C8 131.14(10) . . ? C1 N2 Si 91.67(7) . . ? C8 N2 Si 136.60(9) . . ? C14 N4 C24 131.45(11) . . ? C14 N4 Si 91.54(8) . . ? C24 N4 Si 136.76(9) . . ? C14 N3 C21 124.68(11) . . ? C14 N3 Si 91.54(8) . . ? C21 N3 Si 141.48(9) . . ? N1 Si N3 162.07(5) . . ? N1 Si N4 97.97(5) . . ? N3 Si N4 69.52(5) . . ? N1 Si N2 69.17(5) . . ? N3 Si N2 97.64(5) . . ? N4 Si N2 91.69(5) . . ? N1 Si C29 98.77(5) . . ? N3 Si C29 94.22(5) . . ? N4 Si C29 90.38(6) . . ? N2 Si C29 167.94(6) . . ? N1 Si C30 93.92(5) . . ? N3 Si C30 98.28(5) . . ? N4 Si C30 167.79(5) . . ? N2 Si C30 89.93(6) . . ? C29 Si C30 90.54(6) . . ? N1 Si C14 131.46(5) . . ? N3 Si C14 35.08(5) . . ? N4 Si C14 34.45(5) . . ? N2 Si C14 96.33(5) . . ? C29 Si C14 92.10(5) . . ? C30 Si C14 133.35(5) . . ? N1 Si C1 34.91(4) . . ? N3 Si C1 130.98(5) . . ? N4 Si C1 96.15(5) . . ? N2 Si C1 34.27(5) . . ? C29 Si C1 133.67(5) . . ? C30 Si C1 91.99(5) . . ? C14 Si C1 118.07(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 C7 68.11(18) . . . . ? N1 C1 C2 C7 -109.83(15) . . . . ? Si C1 C2 C7 -73.1(16) . . . . ? N2 C1 C2 C3 -112.93(16) . . . . ? N1 C1 C2 C3 69.13(18) . . . . ? Si C1 C2 C3 105.9(16) . . . . ? C3 C2 C7 C6 -0.3(2) . . . . ? C1 C2 C7 C6 178.65(13) . . . . ? C2 C7 C6 C5 1.6(2) . . . . ? C7 C6 C5 C4 -1.1(3) . . . . ? C6 C5 C4 C3 -0.6(3) . . . . ? C5 C4 C3 C2 1.8(3) . . . . ? C7 C2 C3 C4 -1.4(2) . . . . ? C1 C2 C3 C4 179.70(14) . . . . ? N4 C14 C15 C16 -103.21(16) . . . . ? N3 C14 C15 C16 76.95(17) . . . . ? Si C14 C15 C16 124(3) . . . . ? N4 C14 C15 C20 74.91(18) . . . . ? N3 C14 C15 C20 -104.93(16) . . . . ? Si C14 C15 C20 -58(3) . . . . ? C16 C15 C20 C19 0.3(2) . . . . ? C14 C15 C20 C19 -177.83(14) . . . . ? C15 C20 C19 C18 0.8(3) . . . . ? C20 C19 C18 C17 -1.1(3) . . . . ? C19 C18 C17 C16 0.2(2) . . . . ? C18 C17 C16 C15 0.9(2) . . . . ? C20 C15 C16 C17 -1.2(2) . . . . ? C14 C15 C16 C17 176.96(13) . . . . ? N2 C1 N1 C11 -169.26(11) . . . . ? C2 C1 N1 C11 9.06(19) . . . . ? Si C1 N1 C11 -168.47(14) . . . . ? N2 C1 N1 Si -0.79(10) . . . . ? C2 C1 N1 Si 177.52(11) . . . . ? C13 C11 N1 C1 -114.62(14) . . . . ? C12 C11 N1 C1 120.88(14) . . . . ? C13 C11 N1 Si 84.17(17) . . . . ? C12 C11 N1 Si -40.34(19) . . . . ? N1 C1 N2 C8 -171.42(12) . . . . ? C2 C1 N2 C8 10.4(2) . . . . ? Si C1 N2 C8 -172.20(16) . . . . ? N1 C1 N2 Si 0.78(10) . . . . ? C2 C1 N2 Si -177.45(12) . . . . ? C9 C8 N2 C1 37.3(2) . . . . ? C10 C8 N2 C1 -90.82(17) . . . . ? C9 C8 N2 Si -131.31(13) . . . . ? C10 C8 N2 Si 100.56(14) . . . . ? N3 C14 N4 C24 -173.22(12) . . . . ? C15 C14 N4 C24 6.9(2) . . . . ? Si C14 N4 C24 -174.87(15) . . . . ? N3 C14 N4 Si 1.65(9) . . . . ? C15 C14 N4 Si -178.21(11) . . . . ? C25 C24 N4 C14 -88.74(17) . . . . ? C26 C24 N4 C14 38.43(18) . . . . ? C25 C24 N4 Si 98.75(14) . . . . ? C26 C24 N4 Si -134.07(12) . . . . ? N4 C14 N3 C21 -167.70(11) . . . . ? C15 C14 N3 C21 12.17(18) . . . . ? Si C14 N3 C21 -166.03(13) . . . . ? N4 C14 N3 Si -1.67(9) . . . . ? C15 C14 N3 Si 178.20(10) . . . . ? C22 C21 N3 C14 -134.99(13) . . . . ? C23 C21 N3 C14 101.32(15) . . . . ? C22 C21 N3 Si 67.80(17) . . . . ? C23 C21 N3 Si -55.88(19) . . . . ? C1 N1 Si N3 45.00(18) . . . . ? C11 N1 Si N3 -150.39(15) . . . . ? C1 N1 Si N4 89.34(8) . . . . ? C11 N1 Si N4 -106.04(14) . . . . ? C1 N1 Si N2 0.56(7) . . . . ? C11 N1 Si N2 165.18(15) . . . . ? C1 N1 Si C29 -179.03(8) . . . . ? C11 N1 Si C29 -14.42(15) . . . . ? C1 N1 Si C30 -87.87(8) . . . . ? C11 N1 Si C30 76.74(14) . . . . ? C1 N1 Si C14 80.26(9) . . . . ? C11 N1 Si C14 -115.13(14) . . . . ? C11 N1 Si C1 164.61(18) . . . . ? C14 N3 Si N1 48.83(18) . . . . ? C21 N3 Si N1 -149.76(15) . . . . ? C14 N3 Si N4 1.19(7) . . . . ? C21 N3 Si N4 162.60(15) . . . . ? C14 N3 Si N2 90.14(8) . . . . ? C21 N3 Si N2 -108.44(14) . . . . ? C14 N3 Si C29 -87.64(8) . . . . ? C21 N3 Si C29 73.77(14) . . . . ? C14 N3 Si C30 -178.81(7) . . . . ? C21 N3 Si C30 -17.40(14) . . . . ? C21 N3 Si C14 161.41(18) . . . . ? C14 N3 Si C1 81.23(9) . . . . ? C21 N3 Si C1 -117.35(13) . . . . ? C14 N4 Si N1 -167.93(7) . . . . ? C24 N4 Si N1 6.46(12) . . . . ? C14 N4 Si N3 -1.21(7) . . . . ? C24 N4 Si N3 173.18(13) . . . . ? C14 N4 Si N2 -98.73(7) . . . . ? C24 N4 Si N2 75.66(12) . . . . ? C14 N4 Si C29 93.16(8) . . . . ? C24 N4 Si C29 -92.46(13) . . . . ? C14 N4 Si C30 -1.2(3) . . . . ? C24 N4 Si C30 173.2(2) . . . . ? C24 N4 Si C14 174.39(16) . . . . ? C14 N4 Si C1 -132.79(7) . . . . ? C24 N4 Si C1 41.59(12) . . . . ? C1 N2 Si N1 -0.57(7) . . . . ? C8 N2 Si N1 170.87(14) . . . . ? C1 N2 Si N3 -168.02(7) . . . . ? C8 N2 Si N3 3.43(13) . . . . ? C1 N2 Si N4 -98.46(8) . . . . ? C8 N2 Si N4 72.99(13) . . . . ? C1 N2 Si C29 1.4(3) . . . . ? C8 N2 Si C29 172.8(2) . . . . ? C1 N2 Si C30 93.64(8) . . . . ? C8 N2 Si C30 -94.91(13) . . . . ? C1 N2 Si C14 -132.69(8) . . . . ? C8 N2 Si C14 38.76(13) . . . . ? C8 N2 Si C1 171.45(17) . . . . ? N5 C29 Si N1 -176(100) . . . . ? N5 C29 Si N3 -8(3) . . . . ? N5 C29 Si N4 -78(3) . . . . ? N5 C29 Si N2 -178(100) . . . . ? N5 C29 Si C30 90(3) . . . . ? N5 C29 Si C14 -43(3) . . . . ? N5 C29 Si C1 -176(100) . . . . ? N6 C30 Si N1 6(3) . . . . ? N6 C30 Si N3 -161(3) . . . . ? N6 C30 Si N4 -161(2) . . . . ? N6 C30 Si N2 -63(3) . . . . ? N6 C30 Si C29 105(3) . . . . ? N6 C30 Si C14 -162(3) . . . . ? N6 C30 Si C1 -29(3) . . . . ? N4 C14 Si N1 16.04(9) . . . . ? N3 C14 Si N1 -161.99(7) . . . . ? C15 C14 Si N1 150(3) . . . . ? N4 C14 Si N3 178.03(11) . . . . ? C15 C14 Si N3 -48(3) . . . . ? N3 C14 Si N4 -178.03(11) . . . . ? C15 C14 Si N4 134(3) . . . . ? N4 C14 Si N2 83.74(8) . . . . ? N3 C14 Si N2 -94.29(8) . . . . ? C15 C14 Si N2 -142(3) . . . . ? N4 C14 Si C29 -87.61(8) . . . . ? N3 C14 Si C29 94.35(8) . . . . ? C15 C14 Si C29 46(3) . . . . ? N4 C14 Si C30 179.65(8) . . . . ? N3 C14 Si C30 1.62(10) . . . . ? C15 C14 Si C30 -47(3) . . . . ? N4 C14 Si C1 55.77(8) . . . . ? N3 C14 Si C1 -122.26(8) . . . . ? C15 C14 Si C1 -170(3) . . . . ? N2 C1 Si N1 179.06(12) . . . . ? C2 C1 Si N1 -38.2(16) . . . . ? N2 C1 Si N3 15.82(10) . . . . ? N1 C1 Si N3 -163.25(8) . . . . ? C2 C1 Si N3 158.6(16) . . . . ? N2 C1 Si N4 83.95(8) . . . . ? N1 C1 Si N4 -95.12(8) . . . . ? C2 C1 Si N4 -133.3(16) . . . . ? N1 C1 Si N2 -179.06(12) . . . . ? C2 C1 Si N2 142.7(16) . . . . ? N2 C1 Si C29 -179.61(8) . . . . ? N1 C1 Si C29 1.33(10) . . . . ? C2 C1 Si C29 -36.9(16) . . . . ? N2 C1 Si C30 -86.95(8) . . . . ? N1 C1 Si C30 93.99(8) . . . . ? C2 C1 Si C30 55.8(16) . . . . ? N2 C1 Si C14 55.89(9) . . . . ? N1 C1 Si C14 -123.18(8) . . . . ? C2 C1 Si C14 -161.4(16) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.15 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.298 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.044 # *******************Data Compound 5 ******************* data_jun03u _database_code_depnum_ccdc_archive 'CCDC 775534' #TrackingRef '- bisamidinato_si_complexes_dalton_final_28_04_10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H38 N10 Si' _chemical_formula_sum 'C26 H38 N10 Si' _chemical_formula_weight 518.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3457(13) _cell_length_b 10.0135(16) _cell_length_c 17.620(3) _cell_angle_alpha 97.257(18) _cell_angle_beta 95.735(17) _cell_angle_gamma 115.332(16) _cell_volume 1456.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 7.85 _cell_measurement_theta_max 25.25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; data result from a twinned crystal with three domains, only one domain integrated, R-value due to overlaps ; _diffrn_ambient_temperature 183(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 image_plate_Stoe_IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16780 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 29.08 _reflns_number_total 7508 _reflns_number_gt 5729 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+0.6435P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7508 _refine_ls_number_parameters 351 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1453 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1108(2) 0.26874(17) 0.30994(9) 0.0262(3) Uani 1 1 d . A . C2 C 1.1963(2) 0.42798(18) 0.35300(9) 0.0294(3) Uani 1 1 d . . . C3 C 1.1860(3) 0.5435(2) 0.32069(11) 0.0436(5) Uani 1 1 d . . . H3 H 1.1249 0.5219 0.2704 0.052 Uiso 1 1 calc R . . C4 C 1.2655(3) 0.6918(2) 0.36192(13) 0.0489(5) Uani 1 1 d . . . H4 H 1.2562 0.7702 0.3399 0.059 Uiso 1 1 calc R . . C5 C 1.3566(3) 0.7247(2) 0.43391(13) 0.0456(5) Uani 1 1 d . . . H5 H 1.4115 0.8257 0.4613 0.055 Uiso 1 1 calc R . . C6 C 1.3686(3) 0.6106(2) 0.46640(13) 0.0518(6) Uani 1 1 d . . . H6 H 1.4321 0.6335 0.5162 0.062 Uiso 1 1 calc R . . C7 C 1.2877(3) 0.4616(2) 0.42650(12) 0.0444(5) Uani 1 1 d . . . H7 H 1.2950 0.3834 0.4495 0.053 Uiso 1 1 calc R . . C10 C 0.934(2) 0.148(2) 0.4601(7) 0.0555(16) Uani 0.673(4) 1 d PD A 1 H10A H 0.8554 0.1436 0.4937 0.083 Uiso 0.673(4) 1 calc PR A 1 H10B H 1.0397 0.2290 0.4842 0.083 Uiso 0.673(4) 1 calc PR A 1 H10C H 0.9400 0.0516 0.4529 0.083 Uiso 0.673(4) 1 calc PR A 1 C8 C 0.8832(3) 0.1762(3) 0.38258(12) 0.0449(5) Uani 0.50 1 d PD A 1 H8 H 0.9174 0.2870 0.3929 0.054 Uiso 0.673(4) 1 calc PR A 1 C9 C 0.7103(4) 0.1126(4) 0.35511(18) 0.0483(7) Uani 0.673(4) 1 d PD A 1 H9A H 0.6909 0.1520 0.3090 0.072 Uiso 0.673(4) 1 calc PR A 1 H9B H 0.6591 0.1403 0.3961 0.072 Uiso 0.673(4) 1 calc PR A 1 H9C H 0.6650 0.0027 0.3418 0.072 Uiso 0.673(4) 1 calc PR A 1 C9B C 0.8065(9) 0.2671(9) 0.3658(4) 0.0483(7) Uani 0.327(4) 1 d PD A 2 H9D H 0.8790 0.3727 0.3881 0.072 Uiso 0.327(4) 1 calc PR A 2 H9E H 0.7080 0.2358 0.3883 0.072 Uiso 0.327(4) 1 calc PR A 2 H9F H 0.7796 0.2556 0.3094 0.072 Uiso 0.327(4) 1 calc PR A 2 C8B C 0.8832(3) 0.1762(3) 0.38258(12) 0.0449(5) Uani 0.50 1 d PD A 2 H8B H 0.7868 0.0782 0.3608 0.054 Uiso 0.327(4) 1 calc PR A 2 C10B C 0.919(5) 0.133(5) 0.4566(15) 0.0555(16) Uani 0.327(4) 1 d PD A 2 H10D H 1.0351 0.1687 0.4704 0.083 Uiso 0.327(4) 1 calc PR A 2 H10E H 0.8641 0.0236 0.4511 0.083 Uiso 0.327(4) 1 calc PR A 2 H10F H 0.8813 0.1792 0.4976 0.083 Uiso 0.327(4) 1 calc PR A 2 C12 C 1.4191(3) 0.2150(3) 0.24116(19) 0.0626(7) Uani 1 1 d . . . H12A H 1.4417 0.2233 0.2975 0.094 Uiso 1 1 calc R . . H12B H 1.5201 0.2660 0.2220 0.094 Uiso 1 1 calc R . . H12C H 1.3656 0.1087 0.2161 0.094 Uiso 1 1 calc R . . C11 C 1.3106(2) 0.2880(2) 0.22224(11) 0.0354(4) Uani 1 1 d . A . H11 H 1.3649 0.3944 0.2510 0.042 Uiso 1 1 calc R . . C13 C 1.2873(3) 0.2911(3) 0.13609(13) 0.0570(6) Uani 1 1 d . . . H13A H 1.2352 0.1879 0.1064 0.086 Uiso 1 1 calc R . . H13B H 1.3920 0.3462 0.1210 0.086 Uiso 1 1 calc R . . H13C H 1.2196 0.3412 0.1252 0.086 Uiso 1 1 calc R . . C14 C 0.7142(2) -0.11008(17) 0.18798(9) 0.0262(3) Uani 1 1 d . A . C15 C 0.5421(2) -0.19932(19) 0.15127(10) 0.0322(4) Uani 1 1 d . . . C16 C 0.4222(3) -0.1859(3) 0.18706(13) 0.0451(5) Uani 1 1 d . . . H16 H 0.4491 -0.1192 0.2353 0.054 Uiso 1 1 calc R . . C17 C 0.2610(3) -0.2711(3) 0.15177(17) 0.0588(6) Uani 1 1 d . . . H17 H 0.1787 -0.2621 0.1763 0.071 Uiso 1 1 calc R . . C18 C 0.2213(3) -0.3674(3) 0.08204(17) 0.0623(8) Uani 1 1 d . . . H18 H 0.1116 -0.4250 0.0586 0.075 Uiso 1 1 calc R . . C19 C 0.3397(3) -0.3810(3) 0.04582(16) 0.0623(7) Uani 1 1 d . . . H19 H 0.3114 -0.4476 -0.0026 0.075 Uiso 1 1 calc R . . C20 C 0.5008(3) -0.2976(2) 0.07995(13) 0.0469(5) Uani 1 1 d . . . H20 H 0.5822 -0.3074 0.0550 0.056 Uiso 1 1 calc R . . C25 C 0.8494(3) 0.2686(2) 0.14884(13) 0.0476(5) Uani 1 1 d . . . H25A H 0.8218 0.2884 0.1999 0.071 Uiso 1 1 calc R . . H25B H 0.8106 0.3176 0.1128 0.071 Uiso 1 1 calc R . . H25C H 0.9663 0.3085 0.1535 0.071 Uiso 1 1 calc R . . C24 C 0.7710(3) 0.1003(2) 0.11831(10) 0.0355(4) Uani 1 1 d . A . H24 H 0.6520 0.0637 0.1122 0.043 Uiso 1 1 calc R . . C26 C 0.8098(4) 0.0609(3) 0.03907(12) 0.0537(6) Uani 1 1 d . . . H26A H 0.9262 0.0969 0.0431 0.081 Uiso 1 1 calc R . . H26B H 0.7729 0.1091 0.0018 0.081 Uiso 1 1 calc R . . H26C H 0.7553 -0.0484 0.0214 0.081 Uiso 1 1 calc R . . C22 C 0.7369(4) -0.2785(3) 0.35255(14) 0.0616(7) Uani 1 1 d . . . H22A H 0.8498 -0.2260 0.3779 0.092 Uiso 1 1 calc R . . H22B H 0.6863 -0.3778 0.3668 0.092 Uiso 1 1 calc R . . H22C H 0.6808 -0.2197 0.3695 0.092 Uiso 1 1 calc R . . C21 C 0.7274(2) -0.2968(2) 0.26522(11) 0.0351(4) Uani 1 1 d . A . H21 H 0.6112 -0.3517 0.2410 0.042 Uiso 1 1 calc R . . C23 C 0.8092(3) -0.3919(2) 0.23661(16) 0.0560(6) Uani 1 1 d . . . H23A H 0.7915 -0.4115 0.1797 0.084 Uiso 1 1 calc R . . H23B H 0.7638 -0.4876 0.2550 0.084 Uiso 1 1 calc R . . H23C H 0.9248 -0.3378 0.2567 0.084 Uiso 1 1 calc R . . N2 N 0.98077(18) 0.15884(15) 0.32485(8) 0.0277(3) Uani 1 1 d . . . N1 N 1.15550(18) 0.21166(15) 0.24856(8) 0.0278(3) Uani 1 1 d . . . N4 N 0.81610(17) 0.02191(15) 0.17476(8) 0.0268(3) Uani 1 1 d . . . N3 N 0.79480(18) -0.15062(15) 0.24014(8) 0.0287(3) Uani 1 1 d . . . N6 N 1.1035(2) -0.04595(17) 0.30986(11) 0.0434(4) Uani 1 1 d . . . N5 N 1.0536(2) -0.06217(18) 0.15916(10) 0.0408(4) Uani 1 1 d . . . N9 N 1.2033(2) 0.03250(17) 0.36572(10) 0.0375(4) Uani 1 1 d . A . N10 N 1.3005(3) 0.1009(2) 0.41904(12) 0.0584(6) Uani 1 1 d . . . N7 N 0.9649(2) -0.16763(17) 0.10908(9) 0.0364(3) Uani 1 1 d . A . N8 N 0.8877(3) -0.2670(2) 0.05998(11) 0.0539(5) Uani 1 1 d . . . Si Si 0.99042(6) 0.01721(5) 0.24265(3) 0.02577(12) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0279(8) 0.0243(7) 0.0232(7) 0.0019(5) -0.0023(6) 0.0109(6) C2 0.0308(9) 0.0246(7) 0.0288(7) -0.0003(6) 0.0008(6) 0.0109(6) C3 0.0605(14) 0.0291(8) 0.0349(9) 0.0001(7) -0.0062(9) 0.0188(9) C4 0.0659(15) 0.0278(9) 0.0497(11) 0.0024(8) 0.0031(10) 0.0206(9) C5 0.0480(12) 0.0280(9) 0.0476(11) -0.0105(8) 0.0045(9) 0.0103(8) C6 0.0568(14) 0.0406(11) 0.0415(11) -0.0124(8) -0.0140(10) 0.0167(10) C7 0.0518(13) 0.0343(9) 0.0377(10) -0.0027(7) -0.0114(9) 0.0170(9) C10 0.057(4) 0.086(4) 0.0285(14) 0.015(2) 0.0115(16) 0.034(3) C8 0.0448(12) 0.0673(14) 0.0358(9) 0.0206(9) 0.0147(9) 0.0326(11) C9 0.0455(17) 0.0715(19) 0.0378(13) 0.0083(13) 0.0102(12) 0.0351(15) C9B 0.0455(17) 0.0715(19) 0.0378(13) 0.0083(13) 0.0102(12) 0.0351(15) C8B 0.0448(12) 0.0673(14) 0.0358(9) 0.0206(9) 0.0147(9) 0.0326(11) C10B 0.057(4) 0.086(4) 0.0285(14) 0.015(2) 0.0115(16) 0.034(3) C12 0.0321(12) 0.0724(16) 0.0911(19) 0.0339(15) 0.0207(12) 0.0234(11) C11 0.0307(10) 0.0302(8) 0.0367(9) 0.0025(7) 0.0071(7) 0.0064(7) C13 0.0512(14) 0.0729(16) 0.0444(12) 0.0187(11) 0.0206(10) 0.0206(12) C14 0.0269(8) 0.0246(7) 0.0242(7) 0.0013(5) 0.0027(6) 0.0100(6) C15 0.0291(9) 0.0273(8) 0.0344(8) 0.0074(6) -0.0025(7) 0.0085(7) C16 0.0321(11) 0.0536(12) 0.0479(11) 0.0123(9) 0.0029(8) 0.0177(9) C17 0.0282(11) 0.0691(16) 0.0808(17) 0.0351(14) 0.0057(11) 0.0183(11) C18 0.0319(12) 0.0453(12) 0.0868(19) 0.0223(12) -0.0237(12) 0.0008(9) C19 0.0538(16) 0.0408(11) 0.0672(15) -0.0051(10) -0.0258(12) 0.0097(11) C20 0.0424(12) 0.0353(9) 0.0489(11) -0.0065(8) -0.0102(9) 0.0122(9) C25 0.0606(14) 0.0346(10) 0.0480(11) 0.0085(8) -0.0002(10) 0.0235(10) C24 0.0438(11) 0.0315(8) 0.0291(8) 0.0066(6) -0.0009(7) 0.0162(8) C26 0.0828(18) 0.0524(12) 0.0289(9) 0.0119(8) 0.0095(10) 0.0317(12) C22 0.086(2) 0.0576(14) 0.0477(12) 0.0264(11) 0.0223(13) 0.0313(14) C21 0.0318(10) 0.0294(8) 0.0387(9) 0.0112(7) 0.0016(7) 0.0084(7) C23 0.0696(17) 0.0300(9) 0.0745(16) 0.0174(10) 0.0230(13) 0.0237(10) N2 0.0299(8) 0.0264(6) 0.0227(6) 0.0031(5) 0.0020(5) 0.0097(5) N1 0.0272(7) 0.0237(6) 0.0277(6) -0.0003(5) 0.0024(5) 0.0087(5) N4 0.0280(7) 0.0251(6) 0.0231(6) 0.0034(5) 0.0006(5) 0.0089(5) N3 0.0282(8) 0.0238(6) 0.0297(7) 0.0038(5) -0.0011(5) 0.0091(5) N6 0.0399(10) 0.0253(7) 0.0546(10) 0.0029(7) -0.0167(8) 0.0116(7) N5 0.0305(8) 0.0323(8) 0.0479(9) -0.0124(7) 0.0053(7) 0.0090(6) N9 0.0331(9) 0.0287(7) 0.0446(9) 0.0097(6) -0.0055(7) 0.0099(6) N10 0.0537(13) 0.0479(10) 0.0525(11) 0.0072(8) -0.0208(9) 0.0102(9) N7 0.0365(9) 0.0314(7) 0.0364(8) -0.0018(6) 0.0098(6) 0.0120(6) N8 0.0514(12) 0.0462(10) 0.0435(10) -0.0142(8) 0.0073(8) 0.0092(9) Si 0.0250(2) 0.0214(2) 0.0270(2) 0.00035(15) -0.00042(16) 0.00882(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.322(2) . ? C1 N1 1.345(2) . ? C1 C2 1.497(2) . ? C1 Si 2.3600(17) . ? C2 C3 1.386(3) . ? C2 C7 1.394(2) . ? C3 C4 1.401(3) . ? C4 C5 1.372(3) . ? C5 C6 1.381(3) . ? C6 C7 1.398(3) . ? C10 C8 1.503(7) . ? C8 C9 1.461(4) . ? C8 N2 1.474(2) . ? C12 C11 1.517(3) . ? C11 N1 1.475(2) . ? C11 C13 1.518(3) . ? C14 N4 1.324(2) . ? C14 N3 1.339(2) . ? C14 C15 1.490(2) . ? C14 Si 2.3647(18) . ? C15 C16 1.386(3) . ? C15 C20 1.401(3) . ? C16 C17 1.401(3) . ? C17 C18 1.371(4) . ? C18 C19 1.378(4) . ? C19 C20 1.393(3) . ? C25 C24 1.517(3) . ? C24 N4 1.476(2) . ? C24 C26 1.523(3) . ? C22 C21 1.516(3) . ? C21 N3 1.471(2) . ? C21 C23 1.525(3) . ? N2 Si 1.9324(15) . ? N1 Si 1.8784(15) . ? N4 Si 1.9436(15) . ? N3 Si 1.8720(16) . ? N6 N9 1.204(2) . ? N6 Si 1.8521(17) . ? N5 N7 1.204(2) . ? N5 Si 1.8507(16) . ? N9 N10 1.145(2) . ? N7 N8 1.141(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 107.57(13) . . ? N2 C1 C2 127.24(15) . . ? N1 C1 C2 125.18(15) . . ? N2 C1 Si 54.95(8) . . ? N1 C1 Si 52.66(8) . . ? C2 C1 Si 176.66(13) . . ? C3 C2 C7 119.21(16) . . ? C3 C2 C1 120.77(15) . . ? C7 C2 C1 120.02(16) . . ? C2 C3 C4 120.21(18) . . ? C5 C4 C3 120.39(19) . . ? C4 C5 C6 119.85(18) . . ? C5 C6 C7 120.4(2) . . ? C2 C7 C6 119.93(19) . . ? C9 C8 N2 116.3(2) . . ? C9 C8 C10 116.5(8) . . ? N2 C8 C10 112.4(8) . . ? N1 C11 C12 110.99(16) . . ? N1 C11 C13 111.54(17) . . ? C12 C11 C13 110.6(2) . . ? N4 C14 N3 107.38(15) . . ? N4 C14 C15 126.82(15) . . ? N3 C14 C15 125.80(15) . . ? N4 C14 Si 55.27(9) . . ? N3 C14 Si 52.21(8) . . ? C15 C14 Si 176.02(12) . . ? C16 C15 C20 119.56(19) . . ? C16 C15 C14 120.56(17) . . ? C20 C15 C14 119.88(18) . . ? C15 C16 C17 119.7(2) . . ? C18 C17 C16 120.4(3) . . ? C17 C18 C19 120.3(2) . . ? C18 C19 C20 120.3(2) . . ? C19 C20 C15 119.7(2) . . ? N4 C24 C25 110.67(15) . . ? N4 C24 C26 110.85(16) . . ? C25 C24 C26 112.39(18) . . ? N3 C21 C22 111.79(16) . . ? N3 C21 C23 111.07(16) . . ? C22 C21 C23 110.8(2) . . ? C1 N2 C8 125.37(16) . . ? C1 N2 Si 90.97(10) . . ? C8 N2 Si 143.47(14) . . ? C1 N1 C11 124.89(14) . . ? C1 N1 Si 92.62(11) . . ? C11 N1 Si 140.07(12) . . ? C14 N4 C24 122.86(15) . . ? C14 N4 Si 90.69(10) . . ? C24 N4 Si 146.09(12) . . ? C14 N3 C21 124.11(15) . . ? C14 N3 Si 93.36(10) . . ? C21 N3 Si 141.58(12) . . ? N9 N6 Si 125.60(13) . . ? N7 N5 Si 124.99(14) . . ? N10 N9 N6 176.3(2) . . ? N8 N7 N5 176.4(2) . . ? N5 Si N6 90.15(9) . . ? N5 Si N3 97.62(7) . . ? N6 Si N3 93.10(7) . . ? N5 Si N1 92.70(7) . . ? N6 Si N1 96.89(7) . . ? N3 Si N1 165.61(7) . . ? N5 Si N2 161.44(7) . . ? N6 Si N2 92.90(7) . . ? N3 Si N2 100.49(7) . . ? N1 Si N2 68.76(6) . . ? N5 Si N4 91.38(7) . . ? N6 Si N4 161.49(7) . . ? N3 Si N4 68.42(6) . . ? N1 Si N4 101.46(7) . . ? N2 Si N4 91.49(6) . . ? N5 Si C1 127.41(7) . . ? N6 Si C1 94.92(7) . . ? N3 Si C1 134.11(7) . . ? N1 Si C1 34.71(6) . . ? N2 Si C1 34.08(6) . . ? N4 Si C1 98.75(6) . . ? N5 Si C14 94.02(7) . . ? N6 Si C14 127.45(7) . . ? N3 Si C14 34.43(6) . . ? N1 Si C14 135.05(6) . . ? N2 Si C14 98.59(6) . . ? N4 Si C14 34.04(6) . . ? C1 Si C14 121.90(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 C1 C2 C3 -107.0(2) . . . . ? N1 C1 C2 C3 73.9(3) . . . . ? Si C1 C2 C3 123(2) . . . . ? N2 C1 C2 C7 73.0(3) . . . . ? N1 C1 C2 C7 -106.2(2) . . . . ? Si C1 C2 C7 -57(2) . . . . ? C7 C2 C3 C4 -0.6(3) . . . . ? C1 C2 C3 C4 179.4(2) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C4 C5 C6 C7 -0.3(4) . . . . ? C3 C2 C7 C6 -0.5(3) . . . . ? C1 C2 C7 C6 179.5(2) . . . . ? C5 C6 C7 C2 0.9(4) . . . . ? N4 C14 C15 C16 -93.9(2) . . . . ? N3 C14 C15 C16 87.0(2) . . . . ? Si C14 C15 C16 145.8(17) . . . . ? N4 C14 C15 C20 86.1(2) . . . . ? N3 C14 C15 C20 -93.0(2) . . . . ? Si C14 C15 C20 -34.3(18) . . . . ? C20 C15 C16 C17 0.3(3) . . . . ? C14 C15 C16 C17 -179.80(19) . . . . ? C15 C16 C17 C18 -0.1(3) . . . . ? C16 C17 C18 C19 -0.2(4) . . . . ? C17 C18 C19 C20 0.3(4) . . . . ? C18 C19 C20 C15 -0.2(4) . . . . ? C16 C15 C20 C19 -0.1(3) . . . . ? C14 C15 C20 C19 179.9(2) . . . . ? N1 C1 N2 C8 -173.60(15) . . . . ? C2 C1 N2 C8 7.1(3) . . . . ? Si C1 N2 C8 -176.02(19) . . . . ? N1 C1 N2 Si 2.42(13) . . . . ? C2 C1 N2 Si -176.88(15) . . . . ? C9 C8 N2 C1 128.9(2) . . . . ? C10 C8 N2 C1 -93.3(9) . . . . ? C9 C8 N2 Si -44.4(3) . . . . ? C10 C8 N2 Si 93.4(9) . . . . ? N2 C1 N1 C11 -167.90(16) . . . . ? C2 C1 N1 C11 11.4(3) . . . . ? Si C1 N1 C11 -165.42(19) . . . . ? N2 C1 N1 Si -2.49(13) . . . . ? C2 C1 N1 Si 176.83(14) . . . . ? C12 C11 N1 C1 107.2(2) . . . . ? C13 C11 N1 C1 -129.0(2) . . . . ? C12 C11 N1 Si -49.8(3) . . . . ? C13 C11 N1 Si 74.1(3) . . . . ? N3 C14 N4 C24 178.12(14) . . . . ? C15 C14 N4 C24 -1.1(3) . . . . ? Si C14 N4 C24 174.70(17) . . . . ? N3 C14 N4 Si 3.41(12) . . . . ? C15 C14 N4 Si -175.82(15) . . . . ? C25 C24 N4 C14 141.75(18) . . . . ? C26 C24 N4 C14 -92.8(2) . . . . ? C25 C24 N4 Si -47.8(3) . . . . ? C26 C24 N4 Si 77.6(2) . . . . ? N4 C14 N3 C21 -174.57(15) . . . . ? C15 C14 N3 C21 4.7(3) . . . . ? Si C14 N3 C21 -171.02(19) . . . . ? N4 C14 N3 Si -3.55(13) . . . . ? C15 C14 N3 Si 175.69(15) . . . . ? C22 C21 N3 C14 -124.1(2) . . . . ? C23 C21 N3 C14 111.5(2) . . . . ? C22 C21 N3 Si 70.5(3) . . . . ? C23 C21 N3 Si -53.9(3) . . . . ? Si N6 N9 N10 -168(4) . . . . ? Si N5 N7 N8 -178(100) . . . . ? N7 N5 Si N6 113.13(19) . . . . ? N7 N5 Si N3 20.0(2) . . . . ? N7 N5 Si N1 -149.97(19) . . . . ? N7 N5 Si N2 -147.3(2) . . . . ? N7 N5 Si N4 -48.43(19) . . . . ? N7 N5 Si C1 -150.55(16) . . . . ? N7 N5 Si C14 -14.45(19) . . . . ? N9 N6 Si N5 126.4(2) . . . . ? N9 N6 Si N3 -135.9(2) . . . . ? N9 N6 Si N1 33.7(2) . . . . ? N9 N6 Si N2 -35.3(2) . . . . ? N9 N6 Si N4 -138.8(2) . . . . ? N9 N6 Si C1 -1.2(2) . . . . ? N9 N6 Si C14 -138.40(18) . . . . ? C14 N3 Si N5 -85.98(11) . . . . ? C21 N3 Si N5 82.0(2) . . . . ? C14 N3 Si N6 -176.55(11) . . . . ? C21 N3 Si N6 -8.6(2) . . . . ? C14 N3 Si N1 49.5(3) . . . . ? C21 N3 Si N1 -142.5(2) . . . . ? C14 N3 Si N2 89.92(10) . . . . ? C21 N3 Si N2 -102.09(19) . . . . ? C14 N3 Si N4 2.48(9) . . . . ? C21 N3 Si N4 170.5(2) . . . . ? C14 N3 Si C1 83.53(12) . . . . ? C21 N3 Si C1 -108.47(19) . . . . ? C21 N3 Si C14 168.0(2) . . . . ? C1 N1 Si N5 -179.18(11) . . . . ? C11 N1 Si N5 -18.0(2) . . . . ? C1 N1 Si N6 -88.70(11) . . . . ? C11 N1 Si N6 72.5(2) . . . . ? C1 N1 Si N3 44.9(3) . . . . ? C11 N1 Si N3 -153.8(2) . . . . ? C1 N1 Si N2 1.74(9) . . . . ? C11 N1 Si N2 163.0(2) . . . . ? C1 N1 Si N4 88.86(10) . . . . ? C11 N1 Si N4 -109.91(19) . . . . ? C11 N1 Si C1 161.2(2) . . . . ? C1 N1 Si C14 82.39(12) . . . . ? C11 N1 Si C14 -116.38(18) . . . . ? C1 N2 Si N5 -4.7(3) . . . . ? C8 N2 Si N5 169.9(2) . . . . ? C1 N2 Si N6 94.50(11) . . . . ? C8 N2 Si N6 -91.0(2) . . . . ? C1 N2 Si N3 -171.81(10) . . . . ? C8 N2 Si N3 2.7(2) . . . . ? C1 N2 Si N1 -1.77(9) . . . . ? C8 N2 Si N1 172.8(2) . . . . ? C1 N2 Si N4 -103.49(10) . . . . ? C8 N2 Si N4 71.1(2) . . . . ? C8 N2 Si C1 174.5(3) . . . . ? C1 N2 Si C14 -136.94(10) . . . . ? C8 N2 Si C14 37.6(2) . . . . ? C14 N4 Si N5 95.14(11) . . . . ? C24 N4 Si N5 -76.9(2) . . . . ? C14 N4 Si N6 0.5(3) . . . . ? C24 N4 Si N6 -171.5(2) . . . . ? C14 N4 Si N3 -2.51(9) . . . . ? C24 N4 Si N3 -174.5(2) . . . . ? C14 N4 Si N1 -171.82(9) . . . . ? C24 N4 Si N1 16.2(2) . . . . ? C14 N4 Si N2 -103.20(10) . . . . ? C24 N4 Si N2 84.8(2) . . . . ? C14 N4 Si C1 -136.65(10) . . . . ? C24 N4 Si C1 51.3(2) . . . . ? C24 N4 Si C14 -172.0(3) . . . . ? N2 C1 Si N5 178.13(11) . . . . ? N1 C1 Si N5 1.03(14) . . . . ? C2 C1 Si N5 -50(2) . . . . ? N2 C1 Si N6 -87.90(12) . . . . ? N1 C1 Si N6 95.00(12) . . . . ? C2 C1 Si N6 44(2) . . . . ? N2 C1 Si N3 11.25(13) . . . . ? N1 C1 Si N3 -165.85(11) . . . . ? C2 C1 Si N3 143(2) . . . . ? N2 C1 Si N1 177.10(15) . . . . ? C2 C1 Si N1 -51(2) . . . . ? N1 C1 Si N2 -177.10(15) . . . . ? C2 C1 Si N2 132(2) . . . . ? N2 C1 Si N4 79.59(10) . . . . ? N1 C1 Si N4 -97.51(11) . . . . ? C2 C1 Si N4 -148(2) . . . . ? N2 C1 Si C14 52.68(11) . . . . ? N1 C1 Si C14 -124.42(11) . . . . ? C2 C1 Si C14 -175(2) . . . . ? N4 C14 Si N5 -86.51(11) . . . . ? N3 C14 Si N5 97.62(11) . . . . ? C15 C14 Si N5 36.3(18) . . . . ? N4 C14 Si N6 -179.78(11) . . . . ? N3 C14 Si N6 4.34(14) . . . . ? C15 C14 Si N6 -57.0(18) . . . . ? N4 C14 Si N3 175.88(15) . . . . ? C15 C14 Si N3 -61.3(17) . . . . ? N4 C14 Si N1 11.38(13) . . . . ? N3 C14 Si N1 -164.49(10) . . . . ? C15 C14 Si N1 134.2(17) . . . . ? N4 C14 Si N2 79.83(10) . . . . ? N3 C14 Si N2 -96.04(10) . . . . ? C15 C14 Si N2 -157.3(18) . . . . ? N3 C14 Si N4 -175.88(15) . . . . ? C15 C14 Si N4 122.8(18) . . . . ? N4 C14 Si C1 53.05(11) . . . . ? N3 C14 Si C1 -122.83(10) . . . . ? C15 C14 Si C1 175.9(17) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 29.08 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.465 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.049 # *******************Data Compound 6 ******************* data_jun17iau _database_code_depnum_ccdc_archive 'CCDC 775535' #TrackingRef '- bisamidinato_si_complexes_dalton_final_28_04_10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H38 N6 O2 Si' _chemical_formula_sum 'C28 H38 N6 O2 Si' _chemical_formula_weight 518.73 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 monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 10.2220(18) _cell_length_b 8.1615(10) _cell_length_c 18.248(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.75(2) _cell_angle_gamma 90.00 _cell_volume 1465.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5.65 _cell_measurement_theta_max 26.6 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9001 _exptl_absorpt_correction_T_max 0.9798 _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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_image_plate _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20168 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 29.10 _reflns_number_total 3869 _reflns_number_gt 2880 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.2053P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3869 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.20123(13) 0.31537(17) 0.31093(7) 0.0402(3) Uani 1 1 d . . . C2 C 0.33408(14) 0.24331(18) 0.35376(8) 0.0451(3) Uani 1 1 d . . . C3 C 0.3923(2) 0.1159(3) 0.32540(12) 0.0820(7) Uani 1 1 d . . . H3 H 0.3480 0.0711 0.2777 0.098 Uiso 1 1 calc R . . C4 C 0.5166(2) 0.0521(3) 0.36678(14) 0.0910(7) Uani 1 1 d . . . H4 H 0.5552 -0.0359 0.3467 0.109 Uiso 1 1 calc R . . C5 C 0.58256(17) 0.1146(2) 0.43526(11) 0.0682(5) Uani 1 1 d . . . H5 H 0.6667 0.0710 0.4628 0.082 Uiso 1 1 calc R . . C6 C 0.5257(2) 0.2418(3) 0.46401(11) 0.0771(6) Uani 1 1 d . . . H6 H 0.5714 0.2866 0.5115 0.092 Uiso 1 1 calc R . . C7 C 0.40110(19) 0.3061(3) 0.42386(10) 0.0679(5) Uani 1 1 d . . . H7 H 0.3624 0.3928 0.4447 0.081 Uiso 1 1 calc R . . C11 C 0.05933(16) 0.1719(2) 0.38071(8) 0.0562(4) Uani 1 1 d . . . H11 H 0.1372 0.0950 0.3937 0.067 Uiso 1 1 calc R . . C12 C 0.0540(3) 0.2601(4) 0.45350(10) 0.0901(7) Uani 1 1 d . . . H12A H 0.1385 0.3187 0.4742 0.135 Uiso 1 1 calc R . . H12B H 0.0411 0.1807 0.4905 0.135 Uiso 1 1 calc R . . H12C H -0.0211 0.3372 0.4421 0.135 Uiso 1 1 calc R . . C13 C -0.06939(19) 0.0721(3) 0.34760(11) 0.0714(5) Uani 1 1 d . . . H13A H -0.1476 0.1444 0.3359 0.107 Uiso 1 1 calc R . . H13B H -0.0794 -0.0093 0.3844 0.107 Uiso 1 1 calc R . . H13C H -0.0629 0.0178 0.3014 0.107 Uiso 1 1 calc R . . C8 C 0.29483(14) 0.5114(2) 0.23364(9) 0.0533(4) Uani 1 1 d . . . H8 H 0.3802 0.4521 0.2577 0.064 Uiso 1 1 calc R . . C9 C 0.2763(2) 0.5096(3) 0.14829(11) 0.0808(6) Uani 1 1 d . . . H9A H 0.2683 0.3973 0.1302 0.121 Uiso 1 1 calc R . . H9B H 0.3542 0.5608 0.1370 0.121 Uiso 1 1 calc R . . H9C H 0.1946 0.5696 0.1231 0.121 Uiso 1 1 calc R . . C10 C 0.30996(19) 0.6854(3) 0.26541(13) 0.0749(5) Uani 1 1 d . . . H10A H 0.2258 0.7450 0.2451 0.112 Uiso 1 1 calc R . . H10B H 0.3832 0.7404 0.2509 0.112 Uiso 1 1 calc R . . H10C H 0.3305 0.6813 0.3205 0.112 Uiso 1 1 calc R . . C14 C 0.09599(15) 0.6810(2) 0.37526(10) 0.0584(4) Uani 1 1 d . . . N2 N 0.08246(11) 0.28915(15) 0.32420(6) 0.0417(3) Uani 1 1 d . . . N1 N 0.18332(11) 0.42401(15) 0.25435(6) 0.0421(3) Uani 1 1 d . . . N3 N 0.02818(13) 0.61062(17) 0.32424(8) 0.0557(3) Uani 1 1 d . . . O O 0.16178(16) 0.7570(3) 0.42763(10) 0.1103(6) Uani 1 1 d . . . Si Si 0.0000 0.45639(6) 0.2500 0.03821(15) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0396(6) 0.0399(7) 0.0392(6) -0.0022(5) 0.0073(5) 0.0006(5) C2 0.0399(6) 0.0445(8) 0.0470(7) 0.0041(6) 0.0049(5) 0.0008(5) C3 0.0625(10) 0.0852(14) 0.0792(12) -0.0310(11) -0.0133(9) 0.0265(10) C4 0.0670(12) 0.0839(15) 0.1030(16) -0.0246(12) -0.0098(11) 0.0329(11) C5 0.0466(8) 0.0663(12) 0.0789(11) 0.0142(9) -0.0050(8) 0.0063(8) C6 0.0622(10) 0.0863(14) 0.0646(10) -0.0029(10) -0.0138(8) 0.0061(10) C7 0.0614(9) 0.0694(11) 0.0604(9) -0.0104(8) -0.0048(7) 0.0112(8) C11 0.0527(8) 0.0645(10) 0.0480(7) 0.0167(7) 0.0078(6) -0.0067(7) C12 0.1038(16) 0.124(2) 0.0461(9) 0.0081(11) 0.0268(10) -0.0220(14) C13 0.0608(10) 0.0702(12) 0.0778(11) 0.0267(9) 0.0094(8) -0.0158(8) C8 0.0384(6) 0.0599(9) 0.0646(9) 0.0146(7) 0.0191(6) 0.0028(6) C9 0.0721(11) 0.1106(17) 0.0709(12) 0.0164(11) 0.0383(10) -0.0037(11) C10 0.0560(9) 0.0648(12) 0.1085(15) 0.0043(11) 0.0303(10) -0.0169(8) C14 0.0396(7) 0.0645(10) 0.0678(9) -0.0195(8) 0.0092(6) 0.0006(7) N2 0.0401(5) 0.0469(6) 0.0363(5) 0.0032(4) 0.0073(4) -0.0027(5) N1 0.0351(5) 0.0455(6) 0.0457(6) 0.0057(5) 0.0113(4) 0.0016(4) N3 0.0432(6) 0.0525(8) 0.0697(8) -0.0190(6) 0.0123(6) -0.0031(5) O 0.0707(9) 0.1458(16) 0.1003(11) -0.0655(12) -0.0007(8) -0.0132(10) Si 0.0336(2) 0.0390(3) 0.0415(3) 0.000 0.00922(18) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.3183(17) . ? C1 N1 1.3353(17) . ? C1 C2 1.4916(18) . ? C1 Si 2.3560(14) . ? C2 C3 1.368(2) . ? C2 C7 1.376(2) . ? C3 C4 1.391(3) . ? C4 C5 1.349(3) . ? C5 C6 1.362(3) . ? C6 C7 1.389(2) . ? C11 N2 1.4724(18) . ? C11 C12 1.525(3) . ? C11 C13 1.526(2) . ? C8 N1 1.4779(17) . ? C8 C9 1.517(2) . ? C8 C10 1.526(3) . ? C14 N3 1.152(2) . ? C14 O 1.184(2) . ? N2 Si 1.9461(12) . ? N1 Si 1.8727(11) . ? N3 Si 1.8141(13) . ? Si N3 1.8141(13) 2 ? Si N1 1.8727(11) 2 ? Si N2 1.9461(12) 2 ? Si C1 2.3560(14) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 108.05(11) . . ? N2 C1 C2 126.34(12) . . ? N1 C1 C2 125.54(12) . . ? N2 C1 Si 55.69(7) . . ? N1 C1 Si 52.54(6) . . ? C2 C1 Si 173.74(10) . . ? C3 C2 C7 118.50(15) . . ? C3 C2 C1 121.95(13) . . ? C7 C2 C1 119.56(14) . . ? C2 C3 C4 120.42(17) . . ? C5 C4 C3 120.96(19) . . ? C4 C5 C6 119.15(16) . . ? C5 C6 C7 120.70(18) . . ? C2 C7 C6 120.27(18) . . ? N2 C11 C12 110.70(15) . . ? N2 C11 C13 110.77(12) . . ? C12 C11 C13 111.48(16) . . ? N1 C8 C9 111.59(14) . . ? N1 C8 C10 110.94(13) . . ? C9 C8 C10 111.73(17) . . ? N3 C14 O 177.60(19) . . ? C1 N2 C11 124.41(12) . . ? C1 N2 Si 90.29(8) . . ? C11 N2 Si 145.25(10) . . ? C1 N1 C8 124.38(11) . . ? C1 N1 Si 92.99(8) . . ? C8 N1 Si 138.89(10) . . ? C14 N3 Si 152.66(13) . . ? N3 Si N3 92.13(10) . 2 ? N3 Si N1 94.81(5) . 2 ? N3 Si N1 96.43(6) 2 2 ? N3 Si N1 96.43(6) . . ? N3 Si N1 94.81(5) 2 . ? N1 Si N1 163.78(8) 2 . ? N3 Si N2 90.92(6) . . ? N3 Si N2 163.18(5) 2 . ? N1 Si N2 99.79(5) 2 . ? N1 Si N2 68.41(5) . . ? N3 Si N2 163.18(5) . 2 ? N3 Si N2 90.92(6) 2 2 ? N1 Si N2 68.41(5) 2 2 ? N1 Si N2 99.79(5) . 2 ? N2 Si N2 90.93(7) . 2 ? N3 Si C1 92.59(6) . . ? N3 Si C1 129.25(5) 2 . ? N1 Si C1 133.36(5) 2 . ? N1 Si C1 34.47(5) . . ? N2 Si C1 34.02(5) . . ? N2 Si C1 98.25(5) 2 . ? N3 Si C1 129.25(5) . 2 ? N3 Si C1 92.59(6) 2 2 ? N1 Si C1 34.47(5) 2 2 ? N1 Si C1 133.36(5) . 2 ? N2 Si C1 98.25(5) . 2 ? N2 Si C1 34.03(5) 2 2 ? C1 Si C1 121.51(7) . 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 N2 C1 C2 C3 102.6(2) . . . . ? N1 C1 C2 C3 -80.6(2) . . . . ? Si C1 C2 C3 -150.6(8) . . . . ? N2 C1 C2 C7 -77.5(2) . . . . ? N1 C1 C2 C7 99.27(19) . . . . ? Si C1 C2 C7 29.3(10) . . . . ? C7 C2 C3 C4 -0.1(4) . . . . ? C1 C2 C3 C4 179.8(2) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? C4 C5 C6 C7 0.4(4) . . . . ? C3 C2 C7 C6 0.7(3) . . . . ? C1 C2 C7 C6 -179.14(18) . . . . ? C5 C6 C7 C2 -0.9(3) . . . . ? N1 C1 N2 C11 177.55(13) . . . . ? C2 C1 N2 C11 -5.2(2) . . . . ? Si C1 N2 C11 -177.94(15) . . . . ? N1 C1 N2 Si -4.50(11) . . . . ? C2 C1 N2 Si 172.73(12) . . . . ? C12 C11 N2 C1 100.16(18) . . . . ? C13 C11 N2 C1 -135.66(16) . . . . ? C12 C11 N2 Si -76.2(2) . . . . ? C13 C11 N2 Si 48.0(3) . . . . ? N2 C1 N1 C8 166.47(13) . . . . ? C2 C1 N1 C8 -10.8(2) . . . . ? Si C1 N1 C8 161.78(16) . . . . ? N2 C1 N1 Si 4.69(11) . . . . ? C2 C1 N1 Si -172.58(12) . . . . ? C9 C8 N1 C1 133.93(16) . . . . ? C10 C8 N1 C1 -100.77(17) . . . . ? C9 C8 N1 Si -74.4(2) . . . . ? C10 C8 N1 Si 50.9(2) . . . . ? O C14 N3 Si 174(100) . . . . ? C14 N3 Si N3 -110.9(3) . . . 2 ? C14 N3 Si N1 152.5(3) . . . 2 ? C14 N3 Si N1 -15.8(3) . . . . ? C14 N3 Si N2 52.6(3) . . . . ? C14 N3 Si N2 148.9(3) . . . 2 ? C14 N3 Si C1 18.6(3) . . . . ? C14 N3 Si C1 154.0(3) . . . 2 ? C1 N1 Si N3 85.20(9) . . . . ? C8 N1 Si N3 -71.69(16) . . . . ? C1 N1 Si N3 177.89(9) . . . 2 ? C8 N1 Si N3 21.00(16) . . . 2 ? C1 N1 Si N1 -48.37(7) . . . 2 ? C8 N1 Si N1 154.74(15) . . . 2 ? C1 N1 Si N2 -3.25(8) . . . . ? C8 N1 Si N2 -160.13(16) . . . . ? C1 N1 Si N2 -90.35(9) . . . 2 ? C8 N1 Si N2 112.77(15) . . . 2 ? C8 N1 Si C1 -156.89(19) . . . . ? C1 N1 Si C1 -83.96(12) . . . 2 ? C8 N1 Si C1 119.15(15) . . . 2 ? C1 N2 Si N3 -93.27(9) . . . . ? C11 N2 Si N3 83.75(18) . . . . ? C1 N2 Si N3 7.2(2) . . . 2 ? C11 N2 Si N3 -175.8(2) . . . 2 ? C1 N2 Si N1 171.69(8) . . . 2 ? C11 N2 Si N1 -11.29(18) . . . 2 ? C1 N2 Si N1 3.28(8) . . . . ? C11 N2 Si N1 -179.70(19) . . . . ? C1 N2 Si N2 103.45(9) . . . 2 ? C11 N2 Si N2 -79.53(17) . . . 2 ? C11 N2 Si C1 177.0(2) . . . . ? C1 N2 Si C1 136.81(8) . . . 2 ? C11 N2 Si C1 -46.17(18) . . . 2 ? N2 C1 Si N3 87.81(9) . . . . ? N1 C1 Si N3 -97.59(9) . . . . ? C2 C1 Si N3 -23.2(9) . . . . ? N2 C1 Si N3 -177.32(9) . . . 2 ? N1 C1 Si N3 -2.72(11) . . . 2 ? C2 C1 Si N3 71.7(9) . . . 2 ? N2 C1 Si N1 -11.29(11) . . . 2 ? N1 C1 Si N1 163.31(8) . . . 2 ? C2 C1 Si N1 -122.3(9) . . . 2 ? N2 C1 Si N1 -174.60(13) . . . . ? C2 C1 Si N1 74.4(9) . . . . ? N1 C1 Si N2 174.60(13) . . . . ? C2 C1 Si N2 -111.0(9) . . . . ? N2 C1 Si N2 -79.31(10) . . . 2 ? N1 C1 Si N2 95.30(9) . . . 2 ? C2 C1 Si N2 169.7(9) . . . 2 ? N2 C1 Si C1 -52.61(7) . . . 2 ? N1 C1 Si C1 121.99(8) . . . 2 ? C2 C1 Si C1 -163.6(9) . . . 2 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 29.10 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.295 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.034 # *******************Data Compound 7 ******************* data_jun16u _database_code_depnum_ccdc_archive 'CCDC 775536' #TrackingRef '- bisamidinato_si_complexes_dalton_final_28_04_10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H38 N6 S2 Si' _chemical_formula_sum 'C28 H38 N6 S2 Si' _chemical_formula_weight 550.85 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6263(11) _cell_length_b 15.6704(17) _cell_length_c 15.3420(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.051(11) _cell_angle_gamma 90.00 _cell_volume 3035.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4584 _cell_measurement_theta_min 6.25 _cell_measurement_theta_max 26.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8390 _exptl_absorpt_correction_T_max 0.9063 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '_image_plate_Stoe-IPDS' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48274 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 29.11 _reflns_number_total 7622 _reflns_number_gt 5519 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+0.9262P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7622 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 C1 C 0.64748(13) 0.12184(9) 0.15796(10) 0.0210(3) Uani 1 1 d . . . C2 C 0.72832(12) 0.06718(9) 0.11554(10) 0.0213(3) Uani 1 1 d . . . C3 C 0.76138(13) -0.00765(10) 0.15805(11) 0.0242(3) Uani 1 1 d . . . H3 H 0.7340 -0.0215 0.2136 0.029 Uiso 1 1 calc R . . C4 C 0.83426(14) -0.06188(10) 0.11917(12) 0.0265(3) Uani 1 1 d . . . H4 H 0.8563 -0.1126 0.1481 0.032 Uiso 1 1 calc R . . C5 C 0.87454(14) -0.04173(11) 0.03824(12) 0.0284(4) Uani 1 1 d . . . H5 H 0.9234 -0.0791 0.0113 0.034 Uiso 1 1 calc R . . C6 C 0.84339(14) 0.03318(12) -0.00350(12) 0.0301(4) Uani 1 1 d . . . H6 H 0.8718 0.0473 -0.0586 0.036 Uiso 1 1 calc R . . C7 C 0.77059(14) 0.08775(10) 0.03511(11) 0.0264(3) Uani 1 1 d . . . H7 H 0.7499 0.1390 0.0064 0.032 Uiso 1 1 calc R . . C11 C 0.75801(13) 0.15884(11) 0.28722(11) 0.0275(4) Uani 1 1 d . . . H11 H 0.8012 0.1074 0.2728 0.033 Uiso 1 1 calc R . . C13 C 0.74981(17) 0.16178(15) 0.38589(13) 0.0419(5) Uani 1 1 d . . . H13A H 0.7195 0.2166 0.4034 0.063 Uiso 1 1 calc R . . H13B H 0.8205 0.1553 0.4125 0.063 Uiso 1 1 calc R . . H13C H 0.7041 0.1153 0.4054 0.063 Uiso 1 1 calc R . . C12 C 0.81820(16) 0.23662(14) 0.25390(16) 0.0432(5) Uani 1 1 d . . . H12A H 0.8220 0.2340 0.1902 0.065 Uiso 1 1 calc R . . H12B H 0.8900 0.2369 0.2792 0.065 Uiso 1 1 calc R . . H12C H 0.7811 0.2888 0.2709 0.065 Uiso 1 1 calc R . . C8 C 0.51645(14) 0.13368(11) 0.03474(11) 0.0265(4) Uani 1 1 d . . . H8 H 0.5589 0.0862 0.0092 0.032 Uiso 1 1 calc R . . C9 C 0.39970(15) 0.10712(13) 0.03273(13) 0.0371(4) Uani 1 1 d . . . H9A H 0.3900 0.0577 0.0709 0.056 Uiso 1 1 calc R . . H9B H 0.3783 0.0920 -0.0270 0.056 Uiso 1 1 calc R . . H9C H 0.3561 0.1546 0.0530 0.056 Uiso 1 1 calc R . . C10 C 0.53298(18) 0.21380(13) -0.02072(13) 0.0390(5) Uani 1 1 d . . . H10A H 0.4910 0.2609 0.0027 0.059 Uiso 1 1 calc R . . H10B H 0.5103 0.2023 -0.0810 0.059 Uiso 1 1 calc R . . H10C H 0.6081 0.2294 -0.0192 0.059 Uiso 1 1 calc R . . C14 C 0.34602(13) 0.15124(10) 0.24751(10) 0.0225(3) Uani 1 1 d . . . C15 C 0.23454(13) 0.12455(10) 0.26207(11) 0.0246(3) Uani 1 1 d . . . C20 C 0.20167(15) 0.10493(12) 0.34614(13) 0.0324(4) Uani 1 1 d . . . H20 H 0.2497 0.1107 0.3942 0.039 Uiso 1 1 calc R . . C19 C 0.09834(16) 0.07681(13) 0.35966(14) 0.0381(4) Uani 1 1 d . . . H19 H 0.0758 0.0639 0.4169 0.046 Uiso 1 1 calc R . . C18 C 0.02819(15) 0.06773(12) 0.28898(15) 0.0376(4) Uani 1 1 d . . . H18 H -0.0413 0.0466 0.2979 0.045 Uiso 1 1 calc R . . C17 C 0.05941(15) 0.08941(12) 0.20576(14) 0.0359(4) Uani 1 1 d . . . H17 H 0.0107 0.0848 0.1581 0.043 Uiso 1 1 calc R . . C16 C 0.16207(14) 0.11797(11) 0.19189(12) 0.0297(4) Uani 1 1 d . . . H16 H 0.1832 0.1331 0.1348 0.036 Uiso 1 1 calc R . . C24 C 0.43373(15) 0.01710(10) 0.29633(12) 0.0292(4) Uani 1 1 d . . . H24 H 0.3594 0.0009 0.3104 0.035 Uiso 1 1 calc R . . C26 C 0.5002(3) 0.00916(15) 0.3792(2) 0.0818(12) Uani 1 1 d . . . H26A H 0.5724 0.0290 0.3683 0.123 Uiso 1 1 calc R . . H26B H 0.5022 -0.0507 0.3977 0.123 Uiso 1 1 calc R . . H26C H 0.4690 0.0440 0.4251 0.123 Uiso 1 1 calc R . . C25 C 0.4722(2) -0.04389(13) 0.22628(19) 0.0556(7) Uani 1 1 d . . . H25A H 0.4274 -0.0379 0.1738 0.083 Uiso 1 1 calc R . . H25B H 0.4681 -0.1027 0.2477 0.083 Uiso 1 1 calc R . . H25C H 0.5457 -0.0303 0.2123 0.083 Uiso 1 1 calc R . . C21 C 0.30792(14) 0.30193(10) 0.20735(12) 0.0284(4) Uani 1 1 d . . . H21 H 0.2334 0.2811 0.2122 0.034 Uiso 1 1 calc R . . C23 C 0.32741(18) 0.36353(12) 0.28226(14) 0.0406(5) Uani 1 1 d . . . H23A H 0.3151 0.3343 0.3376 0.061 Uiso 1 1 calc R . . H23B H 0.2789 0.4121 0.2765 0.061 Uiso 1 1 calc R . . H23C H 0.4007 0.3839 0.2811 0.061 Uiso 1 1 calc R . . C22 C 0.31655(19) 0.34410(13) 0.11869(13) 0.0417(5) Uani 1 1 d . . . H22A H 0.3889 0.3651 0.1112 0.063 Uiso 1 1 calc R . . H22B H 0.2668 0.3920 0.1147 0.063 Uiso 1 1 calc R . . H22C H 0.2995 0.3024 0.0729 0.063 Uiso 1 1 calc R . . C27 C 0.50589(14) 0.23973(10) 0.42233(11) 0.0266(3) Uani 1 1 d . . . C28 C 0.61744(14) 0.35539(10) 0.15504(11) 0.0271(4) Uani 1 1 d . . . N1 N 0.65361(11) 0.14863(8) 0.24168(9) 0.0223(3) Uani 1 1 d . . . N2 N 0.55596(11) 0.14902(8) 0.12458(9) 0.0214(3) Uani 1 1 d . . . N4 N 0.43252(11) 0.10624(8) 0.26635(9) 0.0222(3) Uani 1 1 d . . . N3 N 0.37752(11) 0.22629(8) 0.21456(9) 0.0220(3) Uani 1 1 d . . . N5 N 0.52198(11) 0.23882(9) 0.34738(9) 0.0247(3) Uani 1 1 d . . . N6 N 0.57087(12) 0.30436(9) 0.19524(10) 0.0256(3) Uani 1 1 d . . . Si Si 0.52118(3) 0.20131(3) 0.23414(3) 0.01987(10) Uani 1 1 d . . . S1 S 0.48704(6) 0.24226(4) 0.52529(3) 0.05387(18) Uani 1 1 d . . . S2 S 0.68133(5) 0.42606(4) 0.10141(4) 0.04645(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0229(7) 0.0203(7) 0.0198(7) -0.0008(5) -0.0024(6) -0.0003(5) C2 0.0212(7) 0.0234(7) 0.0193(7) -0.0030(5) -0.0025(6) -0.0001(5) C3 0.0249(8) 0.0283(7) 0.0192(8) -0.0001(6) -0.0014(7) 0.0009(6) C4 0.0271(8) 0.0250(7) 0.0271(9) -0.0012(6) -0.0033(7) 0.0042(6) C5 0.0231(8) 0.0349(9) 0.0273(9) -0.0063(7) 0.0017(7) 0.0050(6) C6 0.0287(9) 0.0395(9) 0.0222(8) 0.0005(7) 0.0050(7) 0.0026(7) C7 0.0263(8) 0.0285(8) 0.0245(8) 0.0030(6) -0.0009(7) 0.0025(6) C11 0.0241(8) 0.0338(8) 0.0244(8) -0.0090(6) -0.0060(7) 0.0048(6) C13 0.0364(10) 0.0640(13) 0.0249(9) -0.0095(9) -0.0111(9) 0.0049(9) C12 0.0309(10) 0.0496(12) 0.0487(13) -0.0026(9) -0.0090(9) -0.0075(8) C8 0.0288(8) 0.0311(8) 0.0192(8) -0.0075(6) -0.0066(7) 0.0063(6) C9 0.0306(9) 0.0473(11) 0.0329(10) -0.0164(8) -0.0106(8) 0.0035(8) C10 0.0483(12) 0.0445(10) 0.0241(9) 0.0026(7) -0.0069(9) 0.0105(9) C14 0.0251(8) 0.0243(7) 0.0179(7) -0.0043(5) -0.0025(6) 0.0002(6) C15 0.0248(8) 0.0234(7) 0.0254(8) -0.0027(6) -0.0009(7) 0.0018(6) C20 0.0303(9) 0.0399(9) 0.0271(9) 0.0000(7) 0.0007(8) 0.0029(7) C19 0.0322(10) 0.0472(11) 0.0352(11) 0.0067(8) 0.0093(9) 0.0046(8) C18 0.0231(8) 0.0384(10) 0.0514(13) 0.0049(8) 0.0049(9) 0.0016(7) C17 0.0261(9) 0.0411(10) 0.0403(11) -0.0023(8) -0.0057(8) -0.0005(7) C16 0.0281(9) 0.0342(8) 0.0268(9) -0.0022(7) -0.0029(8) -0.0006(7) C24 0.0314(9) 0.0224(7) 0.0336(9) 0.0028(6) -0.0021(8) -0.0002(6) C26 0.138(3) 0.0338(11) 0.0711(18) 0.0211(11) -0.062(2) -0.0114(14) C25 0.0667(16) 0.0248(9) 0.0763(18) -0.0027(10) 0.0285(14) 0.0013(9) C21 0.0306(9) 0.0268(8) 0.0278(9) -0.0012(6) -0.0012(7) 0.0081(6) C23 0.0511(12) 0.0340(9) 0.0365(11) -0.0095(8) -0.0031(10) 0.0154(8) C22 0.0570(13) 0.0355(9) 0.0323(10) 0.0024(8) -0.0059(10) 0.0162(9) C27 0.0324(9) 0.0216(7) 0.0259(9) -0.0032(6) 0.0015(7) 0.0015(6) C28 0.0301(8) 0.0283(8) 0.0229(8) -0.0069(6) -0.0011(7) 0.0007(6) N1 0.0222(6) 0.0262(6) 0.0183(7) -0.0045(5) -0.0030(6) 0.0019(5) N2 0.0222(6) 0.0237(6) 0.0183(6) -0.0044(5) -0.0030(6) 0.0023(5) N4 0.0231(7) 0.0212(6) 0.0223(7) -0.0013(5) -0.0012(6) 0.0000(5) N3 0.0231(6) 0.0217(6) 0.0212(7) -0.0028(5) -0.0015(6) 0.0023(5) N5 0.0264(7) 0.0272(6) 0.0205(7) -0.0047(5) -0.0015(6) 0.0007(5) N6 0.0276(7) 0.0245(6) 0.0246(7) -0.0036(5) 0.0000(6) -0.0005(5) Si 0.0213(2) 0.02043(19) 0.0178(2) -0.00326(15) -0.00199(17) 0.00104(15) S1 0.0942(5) 0.0445(3) 0.0235(2) 0.0009(2) 0.0163(3) 0.0068(3) S2 0.0599(4) 0.0462(3) 0.0336(3) 0.0017(2) 0.0118(3) -0.0192(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.326(2) . ? C1 N1 1.352(2) . ? C1 C2 1.491(2) . ? C1 Si 2.3512(17) . ? C2 C7 1.391(2) . ? C2 C3 1.402(2) . ? C3 C4 1.395(2) . ? C4 C5 1.387(3) . ? C5 C6 1.390(2) . ? C6 C7 1.395(2) . ? C11 N1 1.489(2) . ? C11 C13 1.520(3) . ? C11 C12 1.529(3) . ? C8 N2 1.4768(19) . ? C8 C9 1.531(3) . ? C8 C10 1.533(3) . ? C14 N4 1.327(2) . ? C14 N3 1.343(2) . ? C14 C15 1.489(2) . ? C14 Si 2.3592(17) . ? C15 C20 1.396(3) . ? C15 C16 1.404(2) . ? C20 C19 1.396(3) . ? C19 C18 1.395(3) . ? C18 C17 1.385(3) . ? C17 C16 1.391(3) . ? C24 N4 1.471(2) . ? C24 C26 1.515(3) . ? C24 C25 1.524(3) . ? C21 N3 1.479(2) . ? C21 C23 1.518(2) . ? C21 C22 1.518(3) . ? C27 N5 1.171(2) . ? C27 S1 1.6023(19) . ? C28 N6 1.174(2) . ? C28 S2 1.6058(19) . ? N1 Si 1.8664(14) . ? N2 Si 1.9279(14) . ? N4 Si 1.9330(14) . ? N3 Si 1.8746(14) . ? N5 Si 1.8338(15) . ? N6 Si 1.8361(15) . ? 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 C1 N1 107.55(14) . . ? N2 C1 C2 127.94(14) . . ? N1 C1 C2 124.41(13) . . ? N2 C1 Si 55.08(8) . . ? N1 C1 Si 52.48(8) . . ? C2 C1 Si 175.66(11) . . ? C7 C2 C3 119.39(15) . . ? C7 C2 C1 122.06(14) . . ? C3 C2 C1 118.55(15) . . ? C4 C3 C2 120.26(16) . . ? C5 C4 C3 120.00(15) . . ? C4 C5 C6 119.95(16) . . ? C5 C6 C7 120.32(17) . . ? C2 C7 C6 120.06(15) . . ? N1 C11 C13 113.25(15) . . ? N1 C11 C12 111.70(14) . . ? C13 C11 C12 110.62(16) . . ? N2 C8 C9 111.81(15) . . ? N2 C8 C10 109.73(14) . . ? C9 C8 C10 110.62(15) . . ? N4 C14 N3 107.39(14) . . ? N4 C14 C15 126.47(15) . . ? N3 C14 C15 126.12(14) . . ? N4 C14 Si 55.02(8) . . ? N3 C14 Si 52.53(8) . . ? C15 C14 Si 175.29(12) . . ? C20 C15 C16 119.45(17) . . ? C20 C15 C14 119.88(15) . . ? C16 C15 C14 120.67(16) . . ? C19 C20 C15 120.07(17) . . ? C18 C19 C20 119.91(19) . . ? C17 C18 C19 120.27(18) . . ? C18 C17 C16 120.09(18) . . ? C17 C16 C15 120.15(18) . . ? N4 C24 C26 110.05(15) . . ? N4 C24 C25 112.12(16) . . ? C26 C24 C25 111.2(2) . . ? N3 C21 C23 111.43(14) . . ? N3 C21 C22 111.33(15) . . ? C23 C21 C22 112.86(16) . . ? N5 C27 S1 178.39(17) . . ? N6 C28 S2 179.11(16) . . ? C1 N1 C11 120.92(14) . . ? C1 N1 Si 92.45(10) . . ? C11 N1 Si 139.98(11) . . ? C1 N2 C8 125.83(14) . . ? C1 N2 Si 90.60(10) . . ? C8 N2 Si 143.56(11) . . ? C14 N4 C24 125.20(14) . . ? C14 N4 Si 90.75(10) . . ? C24 N4 Si 144.02(12) . . ? C14 N3 C21 123.40(15) . . ? C14 N3 Si 92.82(10) . . ? C21 N3 Si 138.72(11) . . ? C27 N5 Si 159.35(14) . . ? C28 N6 Si 161.27(14) . . ? N5 Si N6 91.72(7) . . ? N5 Si N1 95.38(6) . . ? N6 Si N1 95.63(7) . . ? N5 Si N3 94.21(7) . . ? N6 Si N3 95.72(6) . . ? N1 Si N3 164.90(6) . . ? N5 Si N2 164.76(6) . . ? N6 Si N2 90.33(6) . . ? N1 Si N2 69.39(6) . . ? N3 Si N2 100.61(6) . . ? N5 Si N4 89.89(6) . . ? N6 Si N4 164.53(6) . . ? N1 Si N4 99.54(6) . . ? N3 Si N4 68.82(6) . . ? N2 Si N4 92.15(6) . . ? N5 Si C1 130.45(6) . . ? N6 Si C1 93.74(6) . . ? N1 Si C1 35.07(5) . . ? N3 Si C1 133.95(6) . . ? N2 Si C1 34.32(5) . . ? N4 Si C1 96.90(6) . . ? N5 Si C14 90.75(6) . . ? N6 Si C14 130.33(6) . . ? N1 Si C14 133.45(6) . . ? N3 Si C14 34.66(6) . . ? N2 Si C14 99.40(6) . . ? N4 Si C14 34.24(5) . . ? C1 Si C14 120.83(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 C1 C2 C7 53.5(2) . . . . ? N1 C1 C2 C7 -130.53(17) . . . . ? Si C1 C2 C7 -173.6(14) . . . . ? N2 C1 C2 C3 -125.75(18) . . . . ? N1 C1 C2 C3 50.2(2) . . . . ? Si C1 C2 C3 7.1(15) . . . . ? C7 C2 C3 C4 -1.4(2) . . . . ? C1 C2 C3 C4 177.90(14) . . . . ? C2 C3 C4 C5 0.2(2) . . . . ? C3 C4 C5 C6 0.9(2) . . . . ? C4 C5 C6 C7 -0.9(3) . . . . ? C3 C2 C7 C6 1.4(2) . . . . ? C1 C2 C7 C6 -177.81(15) . . . . ? C5 C6 C7 C2 -0.3(3) . . . . ? N4 C14 C15 C20 59.2(2) . . . . ? N3 C14 C15 C20 -119.21(19) . . . . ? Si C14 C15 C20 -47.6(15) . . . . ? N4 C14 C15 C16 -120.10(19) . . . . ? N3 C14 C15 C16 61.5(2) . . . . ? Si C14 C15 C16 133.1(14) . . . . ? C16 C15 C20 C19 1.7(3) . . . . ? C14 C15 C20 C19 -177.60(16) . . . . ? C15 C20 C19 C18 0.5(3) . . . . ? C20 C19 C18 C17 -2.3(3) . . . . ? C19 C18 C17 C16 1.9(3) . . . . ? C18 C17 C16 C15 0.3(3) . . . . ? C20 C15 C16 C17 -2.1(3) . . . . ? C14 C15 C16 C17 177.19(16) . . . . ? N2 C1 N1 C11 -156.42(14) . . . . ? C2 C1 N1 C11 26.9(2) . . . . ? Si C1 N1 C11 -156.81(16) . . . . ? N2 C1 N1 Si 0.39(13) . . . . ? C2 C1 N1 Si -176.27(14) . . . . ? C13 C11 N1 C1 -161.83(15) . . . . ? C12 C11 N1 C1 72.5(2) . . . . ? C13 C11 N1 Si 55.9(2) . . . . ? C12 C11 N1 Si -69.8(2) . . . . ? N1 C1 N2 C8 -179.62(14) . . . . ? C2 C1 N2 C8 -3.1(3) . . . . ? Si C1 N2 C8 -179.25(18) . . . . ? N1 C1 N2 Si -0.38(12) . . . . ? C2 C1 N2 Si 176.13(15) . . . . ? C9 C8 N2 C1 135.29(17) . . . . ? C10 C8 N2 C1 -101.59(19) . . . . ? C9 C8 N2 Si -43.4(2) . . . . ? C10 C8 N2 Si 79.7(2) . . . . ? N3 C14 N4 C24 -174.06(14) . . . . ? C15 C14 N4 C24 7.3(3) . . . . ? Si C14 N4 C24 -178.23(18) . . . . ? N3 C14 N4 Si 4.17(13) . . . . ? C15 C14 N4 Si -174.50(15) . . . . ? C26 C24 N4 C14 -127.7(2) . . . . ? C25 C24 N4 C14 108.0(2) . . . . ? C26 C24 N4 Si 55.3(3) . . . . ? C25 C24 N4 Si -69.0(3) . . . . ? N4 C14 N3 C21 -163.32(14) . . . . ? C15 C14 N3 C21 15.4(2) . . . . ? Si C14 N3 C21 -159.02(17) . . . . ? N4 C14 N3 Si -4.30(13) . . . . ? C15 C14 N3 Si 174.37(14) . . . . ? C23 C21 N3 C14 98.6(2) . . . . ? C22 C21 N3 C14 -134.47(17) . . . . ? C23 C21 N3 Si -48.6(3) . . . . ? C22 C21 N3 Si 78.4(2) . . . . ? S1 C27 N5 Si 145(6) . . . . ? S2 C28 N6 Si -145(11) . . . . ? C27 N5 Si N6 169.6(4) . . . . ? C27 N5 Si N1 -94.6(4) . . . . ? C27 N5 Si N3 73.7(4) . . . . ? C27 N5 Si N2 -92.8(5) . . . . ? C27 N5 Si N4 5.0(4) . . . . ? C27 N5 Si C1 -94.0(4) . . . . ? C27 N5 Si C14 39.2(4) . . . . ? C28 N6 Si N5 143.1(4) . . . . ? C28 N6 Si N1 47.5(4) . . . . ? C28 N6 Si N3 -122.5(4) . . . . ? C28 N6 Si N2 -21.8(4) . . . . ? C28 N6 Si N4 -121.1(4) . . . . ? C28 N6 Si C1 12.4(4) . . . . ? C28 N6 Si C14 -124.5(4) . . . . ? C1 N1 Si N5 179.23(10) . . . . ? C11 N1 Si N5 -32.46(19) . . . . ? C1 N1 Si N6 -88.50(10) . . . . ? C11 N1 Si N6 59.81(19) . . . . ? C1 N1 Si N3 50.0(3) . . . . ? C11 N1 Si N3 -161.7(2) . . . . ? C1 N1 Si N2 -0.27(9) . . . . ? C11 N1 Si N2 148.04(19) . . . . ? C1 N1 Si N4 88.44(10) . . . . ? C11 N1 Si N4 -123.25(18) . . . . ? C11 N1 Si C1 148.3(2) . . . . ? C1 N1 Si C14 83.06(12) . . . . ? C11 N1 Si C14 -128.63(17) . . . . ? C14 N3 Si N5 -85.23(10) . . . . ? C21 N3 Si N5 67.83(18) . . . . ? C14 N3 Si N6 -177.38(10) . . . . ? C21 N3 Si N6 -24.33(18) . . . . ? C14 N3 Si N1 44.1(3) . . . . ? C21 N3 Si N1 -162.9(2) . . . . ? C14 N3 Si N2 91.21(10) . . . . ? C21 N3 Si N2 -115.74(17) . . . . ? C14 N3 Si N4 3.02(9) . . . . ? C21 N3 Si N4 156.07(19) . . . . ? C14 N3 Si C1 81.80(12) . . . . ? C21 N3 Si C1 -125.14(16) . . . . ? C21 N3 Si C14 153.1(2) . . . . ? C1 N2 Si N5 -1.6(3) . . . . ? C8 N2 Si N5 177.4(2) . . . . ? C1 N2 Si N6 96.17(10) . . . . ? C8 N2 Si N6 -84.86(19) . . . . ? C1 N2 Si N1 0.28(9) . . . . ? C8 N2 Si N1 179.2(2) . . . . ? C1 N2 Si N3 -167.95(9) . . . . ? C8 N2 Si N3 11.0(2) . . . . ? C1 N2 Si N4 -99.10(10) . . . . ? C8 N2 Si N4 79.87(19) . . . . ? C8 N2 Si C1 179.0(2) . . . . ? C1 N2 Si C14 -132.76(10) . . . . ? C8 N2 Si C14 46.2(2) . . . . ? C14 N4 Si N5 91.50(10) . . . . ? C24 N4 Si N5 -91.0(2) . . . . ? C14 N4 Si N6 -4.6(3) . . . . ? C24 N4 Si N6 173.0(2) . . . . ? C14 N4 Si N1 -173.06(10) . . . . ? C24 N4 Si N1 4.5(2) . . . . ? C14 N4 Si N3 -3.05(9) . . . . ? C24 N4 Si N3 174.5(2) . . . . ? C14 N4 Si N2 -103.60(10) . . . . ? C24 N4 Si N2 73.9(2) . . . . ? C14 N4 Si C1 -137.71(10) . . . . ? C24 N4 Si C1 39.8(2) . . . . ? C24 N4 Si C14 177.5(3) . . . . ? N2 C1 Si N5 179.45(10) . . . . ? N1 C1 Si N5 -1.01(13) . . . . ? C2 C1 Si N5 44.3(15) . . . . ? N2 C1 Si N6 -85.08(10) . . . . ? N1 C1 Si N6 94.46(10) . . . . ? C2 C1 Si N6 139.7(15) . . . . ? N2 C1 Si N1 -179.55(15) . . . . ? C2 C1 Si N1 45.3(14) . . . . ? N2 C1 Si N3 16.56(13) . . . . ? N1 C1 Si N3 -163.90(10) . . . . ? C2 C1 Si N3 -118.6(14) . . . . ? N1 C1 Si N2 179.55(15) . . . . ? C2 C1 Si N2 -135.2(15) . . . . ? N2 C1 Si N4 83.67(10) . . . . ? N1 C1 Si N4 -96.78(10) . . . . ? C2 C1 Si N4 -51.5(15) . . . . ? N2 C1 Si C14 57.51(11) . . . . ? N1 C1 Si C14 -122.94(10) . . . . ? C2 C1 Si C14 -77.7(15) . . . . ? N4 C14 Si N5 -88.70(10) . . . . ? N3 C14 Si N5 96.32(10) . . . . ? C15 C14 Si N5 21.3(15) . . . . ? N4 C14 Si N6 178.41(10) . . . . ? N3 C14 Si N6 3.42(13) . . . . ? C15 C14 Si N6 -71.6(15) . . . . ? N4 C14 Si N1 9.45(13) . . . . ? N3 C14 Si N1 -165.54(10) . . . . ? C15 C14 Si N1 119.4(15) . . . . ? N4 C14 Si N3 174.99(15) . . . . ? C15 C14 Si N3 -75.0(15) . . . . ? N4 C14 Si N2 79.89(10) . . . . ? N3 C14 Si N2 -95.10(10) . . . . ? C15 C14 Si N2 -170.1(15) . . . . ? N3 C14 Si N4 -174.99(15) . . . . ? C15 C14 Si N4 110.0(15) . . . . ? N4 C14 Si C1 51.07(11) . . . . ? N3 C14 Si C1 -123.92(10) . . . . ? C15 C14 Si C1 161.1(14) . . . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.397 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.057 # *******************Data Compound 8 . 0.5 C7H8 ******************* data_jun11u _database_code_depnum_ccdc_archive 'CCDC 775537' #TrackingRef '- bisamidinato_si_complexes_dalton_final_28_04_10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H42 N4 S2 Si, 1/2 (C7H8) ' _chemical_formula_sum 'C35.50 H46 N4 S2 Si' _chemical_formula_weight 620.97 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2763(13) _cell_length_b 20.044(2) _cell_length_c 14.0228(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.261(15) _cell_angle_gamma 90.00 _cell_volume 3450.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 6.9 _cell_measurement_theta_max 27.65 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.219 _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 173(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 image_plate_Stoe_IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27226 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 29.20 _reflns_number_total 9053 _reflns_number_gt 6456 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.3140P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9053 _refine_ls_number_parameters 412 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 C1 C 1.11993(12) 0.21964(7) 0.58487(10) 0.0194(3) Uani 1 1 d . A 2 C2 C 1.23975(12) 0.20883(7) 0.58876(10) 0.0215(3) Uani 1 1 d . A 2 C7 C 1.30294(14) 0.24240(8) 0.65647(12) 0.0311(3) Uani 1 1 d . A 2 H7 H 1.2699 0.2734 0.6987 0.037 Uiso 1 1 calc R A 2 C6 C 1.41407(15) 0.23040(10) 0.66197(13) 0.0374(4) Uani 1 1 d . A 2 H6 H 1.4568 0.2530 0.7084 0.045 Uiso 1 1 calc R A 2 C5 C 1.46358(14) 0.18548(9) 0.59999(13) 0.0336(4) Uani 1 1 d . A 2 H5 H 1.5397 0.1774 0.6044 0.040 Uiso 1 1 calc R A 2 C4 C 1.40138(14) 0.15266(8) 0.53183(12) 0.0296(3) Uani 1 1 d . A 2 H4 H 1.4350 0.1222 0.4892 0.035 Uiso 1 1 calc R A 2 C3 C 1.29012(13) 0.16428(8) 0.52576(11) 0.0252(3) Uani 1 1 d . A 2 H3 H 1.2479 0.1419 0.4787 0.030 Uiso 1 1 calc R A 2 C8 C 1.04978(12) 0.11069(7) 0.65579(10) 0.0205(3) Uani 1 1 d . A 2 H8 H 0.9802 0.1028 0.6908 0.025 Uiso 1 1 calc R A 2 C9 C 1.14128(14) 0.10198(8) 0.72875(11) 0.0282(3) Uani 1 1 d . A 2 H9A H 1.2115 0.1010 0.6959 0.042 Uiso 1 1 calc R A 2 H9B H 1.1308 0.0600 0.7635 0.042 Uiso 1 1 calc R A 2 H9C H 1.1403 0.1394 0.7738 0.042 Uiso 1 1 calc R A 2 C10 C 1.05532(15) 0.05733(7) 0.57770(11) 0.0272(3) Uani 1 1 d . A 2 H10A H 0.9955 0.0641 0.5322 0.041 Uiso 1 1 calc R A 2 H10B H 1.0489 0.0130 0.6066 0.041 Uiso 1 1 calc R A 2 H10C H 1.1251 0.0608 0.5443 0.041 Uiso 1 1 calc R A 2 C11 C 1.12543(13) 0.33016(7) 0.50352(11) 0.0260(3) Uani 1 1 d . A 2 H11 H 1.2056 0.3214 0.5053 0.031 Uiso 1 1 calc R A 2 C12 C 1.10378(16) 0.39444(8) 0.55943(14) 0.0370(4) Uani 1 1 d . A 2 H12A H 1.0253 0.4034 0.5602 0.055 Uiso 1 1 calc R A 2 H12B H 1.1417 0.4317 0.5288 0.055 Uiso 1 1 calc R A 2 H12C H 1.1305 0.3893 0.6250 0.055 Uiso 1 1 calc R A 2 C13 C 1.09096(17) 0.33705(9) 0.39942(13) 0.0382(4) Uani 1 1 d . A 2 H13A H 1.1084 0.2958 0.3651 0.057 Uiso 1 1 calc R A 2 H13B H 1.1300 0.3745 0.3704 0.057 Uiso 1 1 calc R A 2 H13C H 1.0124 0.3453 0.3958 0.057 Uiso 1 1 calc R A 2 C14 C 0.84649(12) 0.32703(7) 0.64886(10) 0.0196(3) Uani 1 1 d . A 2 C15 C 0.79004(12) 0.38194(7) 0.70192(10) 0.0209(3) Uani 1 1 d . A 2 C16 C 0.83467(15) 0.44625(8) 0.70564(11) 0.0291(3) Uani 1 1 d . A 2 H16 H 0.8983 0.4565 0.6702 0.035 Uiso 1 1 calc R A 2 C17 C 0.78532(16) 0.49532(8) 0.76166(12) 0.0327(4) Uani 1 1 d . A 2 H17 H 0.8153 0.5390 0.7636 0.039 Uiso 1 1 calc R A 2 C18 C 0.69290(15) 0.48068(8) 0.81443(11) 0.0304(4) Uani 1 1 d . A 2 H18 H 0.6605 0.5141 0.8532 0.037 Uiso 1 1 calc R A 2 C19 C 0.64774(14) 0.41690(8) 0.81046(11) 0.0279(3) Uani 1 1 d . A 2 H19 H 0.5838 0.4070 0.8457 0.034 Uiso 1 1 calc R A 2 C20 C 0.69654(13) 0.36760(7) 0.75465(11) 0.0247(3) Uani 1 1 d . A 2 H20 H 0.6660 0.3241 0.7525 0.030 Uiso 1 1 calc R A 2 C21 C 0.93271(13) 0.27935(7) 0.79342(10) 0.0223(3) Uani 1 1 d . A 2 H21 H 0.8913 0.3164 0.8243 0.027 Uiso 1 1 calc R A 2 C22 C 1.05303(14) 0.29294(9) 0.80873(11) 0.0304(3) Uani 1 1 d . A 2 H22A H 1.0958 0.2567 0.7806 0.046 Uiso 1 1 calc R A 2 H22B H 1.0685 0.2956 0.8772 0.046 Uiso 1 1 calc R A 2 H22C H 1.0725 0.3353 0.7782 0.046 Uiso 1 1 calc R A 2 C23 C 0.89692(14) 0.21426(8) 0.84008(11) 0.0291(3) Uani 1 1 d . A 2 H23A H 0.8189 0.2074 0.8286 0.044 Uiso 1 1 calc R A 2 H23B H 0.9108 0.2165 0.9089 0.044 Uiso 1 1 calc R A 2 H23C H 0.9381 0.1770 0.8127 0.044 Uiso 1 1 calc R A 2 C24 C 0.77464(13) 0.34150(7) 0.48146(10) 0.0235(3) Uani 1 1 d . A 2 H24 H 0.7921 0.3177 0.4208 0.028 Uiso 1 1 calc R A 2 C25 C 0.79290(16) 0.41604(8) 0.46283(13) 0.0342(4) Uani 1 1 d . A 2 H25A H 0.7708 0.4417 0.5190 0.051 Uiso 1 1 calc R A 2 H25B H 0.7494 0.4300 0.4076 0.051 Uiso 1 1 calc R A 2 H25C H 0.8702 0.4240 0.4500 0.051 Uiso 1 1 calc R A 2 C26 C 0.65540(15) 0.32663(9) 0.50351(12) 0.0342(4) Uani 1 1 d . A 2 H26A H 0.6463 0.2787 0.5144 0.051 Uiso 1 1 calc R A 2 H26B H 0.6098 0.3405 0.4495 0.051 Uiso 1 1 calc R A 2 H26C H 0.6336 0.3512 0.5608 0.051 Uiso 1 1 calc R A 2 C27 C 0.76213(13) 0.12447(7) 0.50099(11) 0.0235(3) Uani 1 1 d . A 2 C28 C 0.82340(13) 0.13888(7) 0.41833(11) 0.0238(3) Uani 1 1 d . A 2 C29 C 0.80080(15) 0.10376(8) 0.33374(12) 0.0312(4) Uani 1 1 d . A 2 H29 H 0.8416 0.1132 0.2779 0.037 Uiso 1 1 calc R A 2 C30 C 0.71980(17) 0.05551(8) 0.33052(14) 0.0385(4) Uani 1 1 d . A 2 H30 H 0.7054 0.0322 0.2728 0.046 Uiso 1 1 calc R A 2 C31 C 0.65953(17) 0.04121(8) 0.41207(14) 0.0389(4) Uani 1 1 d . A 2 H31 H 0.6041 0.0082 0.4100 0.047 Uiso 1 1 calc R A 2 C32 C 0.68061(15) 0.07539(8) 0.49654(13) 0.0309(3) Uani 1 1 d . A 2 H32 H 0.6394 0.0654 0.5519 0.037 Uiso 1 1 calc R A 2 C39 C 0.5959(5) 0.5799(4) 0.4309(6) 0.052(3) Uani 0.50 1 d PD B -1 H39A H 0.6519 0.5592 0.3911 0.078 Uiso 0.50 1 calc PR B -1 H39B H 0.6309 0.6065 0.4811 0.078 Uiso 0.50 1 calc PR B -1 H39C H 0.5498 0.6088 0.3914 0.078 Uiso 0.50 1 calc PR B -1 C33 C 0.5372(2) 0.51194(14) 0.57282(18) 0.0341(19) Uani 0.50 1 d PGD B -1 H33 H 0.5878 0.5363 0.6107 0.041 Uiso 0.50 1 calc PR B -1 C34 C 0.4740(3) 0.46229(15) 0.61412(16) 0.0414(9) Uani 0.50 1 d PGD B -1 H34 H 0.4814 0.4527 0.6802 0.050 Uiso 0.50 1 calc PR B -1 C35 C 0.4000(3) 0.42667(14) 0.5588(2) 0.050(3) Uani 0.50 1 d PGD B -1 H35 H 0.3568 0.3927 0.5870 0.060 Uiso 0.50 1 calc PR B -1 C36 C 0.3892(2) 0.44069(14) 0.4621(2) 0.0401(8) Uani 0.50 1 d PGD B -1 H36 H 0.3386 0.4163 0.4243 0.048 Uiso 0.50 1 calc PR B -1 C37 C 0.4524(2) 0.49034(14) 0.42081(16) 0.041(2) Uani 0.50 1 d PGD B -1 H37 H 0.4450 0.4999 0.3547 0.050 Uiso 0.50 1 calc PR B -1 C38 C 0.5264(2) 0.52596(14) 0.47616(19) 0.0344(7) Uani 0.50 1 d PGD B -1 N1 N 1.04202(10) 0.17827(6) 0.61526(8) 0.0192(2) Uani 1 1 d . A 2 N2 N 1.07008(10) 0.27304(6) 0.54883(9) 0.0207(2) Uani 1 1 d . A 2 N4 N 0.90463(10) 0.27969(6) 0.69127(8) 0.0192(2) Uani 1 1 d . A 2 N3 N 0.84801(10) 0.31444(6) 0.55501(8) 0.0194(2) Uani 1 1 d . A 2 S2 S 0.78731(3) 0.166939(17) 0.60930(2) 0.02165(8) Uani 1 1 d . A 2 S1 S 0.92744(3) 0.199375(18) 0.41917(2) 0.02409(9) Uani 1 1 d . A 2 Si Si 0.92903(3) 0.234613(18) 0.57195(3) 0.01720(9) Uani 1 1 d . A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0172(7) 0.0208(6) 0.0202(6) -0.0022(5) -0.0004(5) 0.0012(5) C2 0.0166(8) 0.0227(7) 0.0252(7) 0.0020(5) 0.0001(5) 0.0006(5) C7 0.0211(9) 0.0348(8) 0.0374(9) -0.0098(7) 0.0000(6) -0.0017(6) C6 0.0220(9) 0.0475(10) 0.0427(10) -0.0076(8) -0.0065(7) -0.0045(7) C5 0.0166(9) 0.0415(9) 0.0428(9) 0.0059(7) 0.0009(7) 0.0029(7) C4 0.0234(9) 0.0333(8) 0.0320(8) 0.0026(6) 0.0058(6) 0.0062(6) C3 0.0218(8) 0.0277(7) 0.0262(7) -0.0003(6) 0.0013(6) 0.0010(6) C8 0.0210(8) 0.0185(6) 0.0219(6) 0.0007(5) 0.0007(5) 0.0009(5) C9 0.0324(10) 0.0253(7) 0.0268(7) 0.0015(6) -0.0063(6) 0.0038(6) C10 0.0316(9) 0.0203(7) 0.0296(7) -0.0026(6) -0.0023(6) 0.0007(6) C11 0.0204(8) 0.0231(7) 0.0345(8) 0.0052(6) 0.0040(6) -0.0015(6) C12 0.0353(11) 0.0239(8) 0.0517(10) 0.0003(7) 0.0059(8) -0.0063(7) C13 0.0390(11) 0.0401(9) 0.0357(9) 0.0138(7) 0.0051(7) -0.0049(8) C14 0.0173(7) 0.0190(6) 0.0225(6) -0.0012(5) 0.0001(5) -0.0016(5) C15 0.0215(8) 0.0203(6) 0.0208(6) -0.0009(5) -0.0029(5) 0.0029(5) C16 0.0309(9) 0.0249(7) 0.0315(8) -0.0044(6) 0.0057(6) -0.0030(6) C17 0.0432(11) 0.0208(7) 0.0342(8) -0.0059(6) 0.0027(7) -0.0015(7) C18 0.0340(10) 0.0301(8) 0.0273(8) -0.0072(6) -0.0004(6) 0.0107(7) C19 0.0246(9) 0.0336(8) 0.0257(7) -0.0011(6) 0.0027(6) 0.0055(6) C20 0.0241(8) 0.0233(7) 0.0268(7) -0.0006(5) -0.0001(6) 0.0012(6) C21 0.0234(8) 0.0242(7) 0.0194(6) -0.0019(5) -0.0018(5) 0.0034(6) C22 0.0294(9) 0.0367(8) 0.0252(7) -0.0035(6) -0.0055(6) -0.0061(7) C23 0.0295(9) 0.0349(8) 0.0228(7) 0.0034(6) -0.0011(6) -0.0032(7) C24 0.0235(8) 0.0251(7) 0.0218(7) -0.0003(5) -0.0043(5) 0.0046(6) C25 0.0372(11) 0.0287(8) 0.0367(9) 0.0079(7) -0.0101(7) 0.0027(7) C26 0.0245(9) 0.0438(9) 0.0344(9) 0.0029(7) -0.0080(7) 0.0005(7) C27 0.0212(8) 0.0190(6) 0.0303(7) -0.0009(5) -0.0075(6) 0.0039(5) C28 0.0246(8) 0.0202(6) 0.0264(7) -0.0028(5) -0.0062(6) 0.0072(6) C29 0.0376(10) 0.0266(7) 0.0294(8) -0.0077(6) -0.0114(7) 0.0117(7) C30 0.0466(12) 0.0252(8) 0.0434(10) -0.0121(7) -0.0242(8) 0.0098(7) C31 0.0384(11) 0.0227(8) 0.0554(11) -0.0037(7) -0.0234(8) -0.0008(7) C32 0.0278(9) 0.0225(7) 0.0422(9) 0.0012(6) -0.0098(7) -0.0020(6) C39 0.036(5) 0.049(4) 0.072(5) 0.007(4) 0.024(4) -0.004(3) C33 0.030(4) 0.040(4) 0.032(4) -0.009(3) -0.008(3) 0.001(3) C34 0.036(2) 0.054(2) 0.0340(18) 0.0047(16) 0.0011(15) 0.0116(18) C35 0.049(6) 0.033(4) 0.068(6) 0.011(3) 0.002(4) 0.003(3) C36 0.031(2) 0.0352(18) 0.054(2) -0.0125(16) -0.0074(16) 0.0033(15) C37 0.035(4) 0.052(5) 0.036(4) 0.000(3) 0.004(3) 0.010(4) C38 0.0256(19) 0.0355(17) 0.0422(19) 0.0012(14) 0.0079(14) 0.0039(14) N1 0.0163(6) 0.0178(5) 0.0236(6) 0.0004(4) -0.0007(4) 0.0004(4) N2 0.0167(7) 0.0197(6) 0.0256(6) 0.0027(4) 0.0008(5) -0.0004(4) N4 0.0204(7) 0.0192(5) 0.0180(5) -0.0015(4) -0.0015(4) 0.0021(4) N3 0.0194(7) 0.0197(5) 0.0191(5) -0.0007(4) -0.0015(4) 0.0027(4) S2 0.0183(2) 0.02221(16) 0.02444(17) -0.00121(13) 0.00040(13) -0.00262(13) S1 0.0249(2) 0.02701(18) 0.02032(16) -0.00323(13) 0.00138(13) 0.00165(14) Si 0.0155(2) 0.01742(17) 0.01869(17) -0.00063(13) -0.00029(13) 0.00078(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.3314(18) . ? C1 N1 1.3371(18) . ? C1 C2 1.488(2) . ? C1 Si 2.3688(16) . ? C2 C7 1.396(2) . ? C2 C3 1.402(2) . ? C7 C6 1.387(3) . ? C6 C5 1.393(3) . ? C5 C4 1.387(3) . ? C4 C3 1.388(2) . ? C8 N1 1.4718(17) . ? C8 C9 1.526(2) . ? C8 C10 1.532(2) . ? C11 N2 1.4765(18) . ? C11 C13 1.524(2) . ? C11 C12 1.532(2) . ? C14 N4 1.3266(18) . ? C14 N3 1.3402(18) . ? C14 C15 1.4998(19) . ? C14 Si 2.3731(14) . ? C15 C20 1.398(2) . ? C15 C16 1.402(2) . ? C16 C17 1.398(2) . ? C17 C18 1.389(2) . ? C18 C19 1.394(2) . ? C19 C20 1.397(2) . ? C21 N4 1.4719(18) . ? C21 C22 1.516(2) . ? C21 C23 1.525(2) . ? C24 N3 1.4700(19) . ? C24 C26 1.527(2) . ? C24 C25 1.533(2) . ? C27 C32 1.405(2) . ? C27 C28 1.414(2) . ? C27 S2 1.7671(15) . ? C28 C29 1.406(2) . ? C28 S1 1.7612(17) . ? C29 C30 1.388(3) . ? C30 C31 1.395(3) . ? C31 C32 1.392(2) . ? C39 C38 1.518(6) . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? N1 Si 1.8869(13) . ? N2 Si 1.9239(13) . ? N4 Si 1.9261(12) . ? N3 Si 1.8983(12) . ? S2 Si 2.2693(6) . ? S1 Si 2.2558(6) . ? 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 C1 N1 106.93(13) . . ? N2 C1 C2 125.72(13) . . ? N1 C1 C2 127.35(13) . . ? N2 C1 Si 54.28(8) . . ? N1 C1 Si 52.70(7) . . ? C2 C1 Si 177.47(10) . . ? C7 C2 C3 119.35(14) . . ? C7 C2 C1 120.07(13) . . ? C3 C2 C1 120.57(14) . . ? C6 C7 C2 119.84(15) . . ? C7 C6 C5 120.61(16) . . ? C4 C5 C6 119.75(16) . . ? C5 C4 C3 120.09(15) . . ? C4 C3 C2 120.34(15) . . ? N1 C8 C9 114.22(12) . . ? N1 C8 C10 111.68(11) . . ? C9 C8 C10 111.37(12) . . ? N2 C11 C13 110.86(13) . . ? N2 C11 C12 110.53(13) . . ? C13 C11 C12 111.46(14) . . ? N4 C14 N3 107.19(12) . . ? N4 C14 C15 123.46(12) . . ? N3 C14 C15 129.34(13) . . ? N4 C14 Si 54.22(7) . . ? N3 C14 Si 53.04(7) . . ? C15 C14 Si 175.88(10) . . ? C20 C15 C16 119.41(13) . . ? C20 C15 C14 119.60(13) . . ? C16 C15 C14 120.79(14) . . ? C17 C16 C15 119.84(15) . . ? C18 C17 C16 120.52(15) . . ? C17 C18 C19 119.87(14) . . ? C18 C19 C20 119.96(15) . . ? C19 C20 C15 120.41(14) . . ? N4 C21 C22 111.14(12) . . ? N4 C21 C23 110.78(12) . . ? C22 C21 C23 112.05(13) . . ? N3 C24 C26 111.76(12) . . ? N3 C24 C25 112.92(13) . . ? C26 C24 C25 111.46(14) . . ? C32 C27 C28 119.21(14) . . ? C32 C27 S2 119.82(13) . . ? C28 C27 S2 120.96(12) . . ? C29 C28 C27 119.05(15) . . ? C29 C28 S1 119.39(13) . . ? C27 C28 S1 121.56(11) . . ? C30 C29 C28 121.00(17) . . ? C29 C30 C31 119.95(16) . . ? C32 C31 C30 119.97(17) . . ? C31 C32 C27 120.81(17) . . ? C34 C33 C38 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C37 C36 C35 120.0 . . ? C38 C37 C36 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 C39 120.0(4) . . ? C33 C38 C39 120.0(4) . . ? C1 N1 C8 130.44(13) . . ? C1 N1 Si 92.99(9) . . ? C8 N1 Si 136.16(10) . . ? C1 N2 C11 125.10(13) . . ? C1 N2 Si 91.53(9) . . ? C11 N2 Si 143.05(10) . . ? C14 N4 C21 124.24(11) . . ? C14 N4 Si 91.81(8) . . ? C21 N4 Si 143.77(10) . . ? C14 N3 C24 127.46(12) . . ? C14 N3 Si 92.61(9) . . ? C24 N3 Si 135.87(9) . . ? C27 S2 Si 102.76(6) . . ? C28 S1 Si 103.01(5) . . ? N1 Si N3 158.23(6) . . ? N1 Si N2 68.47(5) . . ? N3 Si N2 96.49(6) . . ? N1 Si N4 96.78(5) . . ? N3 Si N4 68.28(5) . . ? N2 Si N4 95.87(6) . . ? N1 Si S1 96.98(4) . . ? N3 Si S1 98.21(4) . . ? N2 Si S1 88.24(4) . . ? N4 Si S1 166.20(4) . . ? N1 Si S2 97.54(4) . . ? N3 Si S2 97.52(4) . . ? N2 Si S2 165.87(4) . . ? N4 Si S2 87.56(4) . . ? S1 Si S2 91.65(2) . . ? N1 Si C1 34.31(5) . . ? N3 Si C1 129.35(5) . . ? N2 Si C1 34.19(5) . . ? N4 Si C1 98.67(5) . . ? S1 Si C1 92.14(4) . . ? S2 Si C1 131.75(4) . . ? N1 Si C14 129.47(5) . . ? N3 Si C14 34.34(5) . . ? N2 Si C14 98.66(5) . . ? N4 Si C14 33.97(5) . . ? S1 Si C14 132.39(4) . . ? S2 Si C14 91.85(4) . . ? C1 Si C14 119.24(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 C7 76.10(19) . . . . ? N1 C1 C2 C7 -104.67(18) . . . . ? Si C1 C2 C7 165(2) . . . . ? N2 C1 C2 C3 -104.87(17) . . . . ? N1 C1 C2 C3 74.36(19) . . . . ? Si C1 C2 C3 -16(3) . . . . ? C3 C2 C7 C6 -1.3(2) . . . . ? C1 C2 C7 C6 177.77(15) . . . . ? C2 C7 C6 C5 0.5(3) . . . . ? C7 C6 C5 C4 0.3(3) . . . . ? C6 C5 C4 C3 -0.4(3) . . . . ? C5 C4 C3 C2 -0.4(2) . . . . ? C7 C2 C3 C4 1.2(2) . . . . ? C1 C2 C3 C4 -177.79(14) . . . . ? N4 C14 C15 C20 -72.8(2) . . . . ? N3 C14 C15 C20 105.77(18) . . . . ? Si C14 C15 C20 -18.2(16) . . . . ? N4 C14 C15 C16 102.04(18) . . . . ? N3 C14 C15 C16 -79.4(2) . . . . ? Si C14 C15 C16 156.6(15) . . . . ? C20 C15 C16 C17 -0.2(2) . . . . ? C14 C15 C16 C17 -174.96(15) . . . . ? C15 C16 C17 C18 0.6(3) . . . . ? C16 C17 C18 C19 -1.1(3) . . . . ? C17 C18 C19 C20 1.0(2) . . . . ? C18 C19 C20 C15 -0.6(2) . . . . ? C16 C15 C20 C19 0.1(2) . . . . ? C14 C15 C20 C19 175.01(14) . . . . ? C32 C27 C28 C29 0.2(2) . . . . ? S2 C27 C28 C29 179.84(11) . . . . ? C32 C27 C28 S1 -179.53(12) . . . . ? S2 C27 C28 S1 0.13(18) . . . . ? C27 C28 C29 C30 0.0(2) . . . . ? S1 C28 C29 C30 179.67(13) . . . . ? C28 C29 C30 C31 -0.1(3) . . . . ? C29 C30 C31 C32 0.1(3) . . . . ? C30 C31 C32 C27 0.1(3) . . . . ? C28 C27 C32 C31 -0.2(2) . . . . ? S2 C27 C32 C31 -179.86(13) . . . . ? C38 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C33 0.0 . . . . ? C36 C37 C38 C39 179.7(4) . . . . ? C34 C33 C38 C37 0.0 . . . . ? C34 C33 C38 C39 -179.7(4) . . . . ? N2 C1 N1 C8 175.97(13) . . . . ? C2 C1 N1 C8 -3.4(2) . . . . ? Si C1 N1 C8 173.45(16) . . . . ? N2 C1 N1 Si 2.52(11) . . . . ? C2 C1 N1 Si -176.82(13) . . . . ? C9 C8 N1 C1 43.1(2) . . . . ? C10 C8 N1 C1 -84.43(18) . . . . ? C9 C8 N1 Si -146.39(12) . . . . ? C10 C8 N1 Si 86.10(16) . . . . ? N1 C1 N2 C11 -177.33(13) . . . . ? C2 C1 N2 C11 2.0(2) . . . . ? Si C1 N2 C11 -174.87(16) . . . . ? N1 C1 N2 Si -2.47(11) . . . . ? C2 C1 N2 Si 176.89(12) . . . . ? C13 C11 N2 C1 117.81(16) . . . . ? C12 C11 N2 C1 -118.08(16) . . . . ? C13 C11 N2 Si -53.6(2) . . . . ? C12 C11 N2 Si 70.5(2) . . . . ? N3 C14 N4 C21 173.24(13) . . . . ? C15 C14 N4 C21 -8.0(2) . . . . ? Si C14 N4 C21 176.18(16) . . . . ? N3 C14 N4 Si -2.94(11) . . . . ? C15 C14 N4 Si 175.86(13) . . . . ? C22 C21 N4 C14 -109.22(16) . . . . ? C23 C21 N4 C14 125.53(15) . . . . ? C22 C21 N4 Si 64.3(2) . . . . ? C23 C21 N4 Si -60.9(2) . . . . ? N4 C14 N3 C24 163.07(13) . . . . ? C15 C14 N3 C24 -15.6(2) . . . . ? Si C14 N3 C24 160.09(16) . . . . ? N4 C14 N3 Si 2.99(12) . . . . ? C15 C14 N3 Si -175.72(14) . . . . ? C26 C24 N3 C14 -56.65(19) . . . . ? C25 C24 N3 C14 69.97(19) . . . . ? C26 C24 N3 Si 94.10(16) . . . . ? C25 C24 N3 Si -139.28(13) . . . . ? C32 C27 S2 Si 177.78(12) . . . . ? C28 C27 S2 Si -1.88(13) . . . . ? C29 C28 S1 Si -178.00(11) . . . . ? C27 C28 S1 Si 1.71(13) . . . . ? C1 N1 Si N3 -50.45(18) . . . . ? C8 N1 Si N3 136.75(15) . . . . ? C1 N1 Si N2 -1.79(8) . . . . ? C8 N1 Si N2 -174.59(14) . . . . ? C1 N1 Si N4 -95.45(9) . . . . ? C8 N1 Si N4 91.76(13) . . . . ? C1 N1 Si S1 83.53(8) . . . . ? C8 N1 Si S1 -89.27(13) . . . . ? C1 N1 Si S2 176.13(7) . . . . ? C8 N1 Si S2 3.33(13) . . . . ? C8 N1 Si C1 -172.80(18) . . . . ? C1 N1 Si C14 -85.18(10) . . . . ? C8 N1 Si C14 102.03(14) . . . . ? C14 N3 Si N1 -51.21(18) . . . . ? C24 N3 Si N1 151.64(15) . . . . ? C14 N3 Si N2 -95.87(9) . . . . ? C24 N3 Si N2 106.98(14) . . . . ? C14 N3 Si N4 -2.11(8) . . . . ? C24 N3 Si N4 -159.27(15) . . . . ? C14 N3 Si S1 174.98(8) . . . . ? C24 N3 Si S1 17.83(14) . . . . ? C14 N3 Si S2 82.21(8) . . . . ? C24 N3 Si S2 -74.94(14) . . . . ? C14 N3 Si C1 -85.40(10) . . . . ? C24 N3 Si C1 117.45(14) . . . . ? C24 N3 Si C14 -157.15(19) . . . . ? C1 N2 Si N1 1.80(8) . . . . ? C11 N2 Si N1 174.80(18) . . . . ? C1 N2 Si N3 165.52(8) . . . . ? C11 N2 Si N3 -21.47(17) . . . . ? C1 N2 Si N4 96.80(9) . . . . ? C11 N2 Si N4 -90.20(17) . . . . ? C1 N2 Si S1 -96.41(8) . . . . ? C11 N2 Si S1 76.59(16) . . . . ? C1 N2 Si S2 -6.7(2) . . . . ? C11 N2 Si S2 166.34(13) . . . . ? C11 N2 Si C1 173.0(2) . . . . ? C1 N2 Si C14 130.94(8) . . . . ? C11 N2 Si C14 -56.06(17) . . . . ? C14 N4 Si N1 165.74(9) . . . . ? C21 N4 Si N1 -8.92(18) . . . . ? C14 N4 Si N3 2.13(8) . . . . ? C21 N4 Si N3 -172.52(18) . . . . ? C14 N4 Si N2 96.80(9) . . . . ? C21 N4 Si N2 -77.86(17) . . . . ? C14 N4 Si S1 -10.0(2) . . . . ? C21 N4 Si S1 175.35(13) . . . . ? C14 N4 Si S2 -96.95(8) . . . . ? C21 N4 Si S2 88.39(17) . . . . ? C14 N4 Si C1 131.16(9) . . . . ? C21 N4 Si C1 -43.50(17) . . . . ? C21 N4 Si C14 -174.7(2) . . . . ? C28 S1 Si N1 95.62(6) . . . . ? C28 S1 Si N3 -100.02(7) . . . . ? C28 S1 Si N2 163.68(6) . . . . ? C28 S1 Si N4 -88.65(19) . . . . ? C28 S1 Si S2 -2.18(5) . . . . ? C28 S1 Si C1 129.71(6) . . . . ? C28 S1 Si C14 -96.19(7) . . . . ? C27 S2 Si N1 -95.03(6) . . . . ? C27 S2 Si N3 100.73(6) . . . . ? C27 S2 Si N2 -87.10(18) . . . . ? C27 S2 Si N4 168.44(6) . . . . ? C27 S2 Si S1 2.23(5) . . . . ? C27 S2 Si C1 -92.11(7) . . . . ? C27 S2 Si C14 134.74(6) . . . . ? N2 C1 Si N1 -177.03(13) . . . . ? C2 C1 Si N1 92(2) . . . . ? N2 C1 Si N3 -18.73(11) . . . . ? N1 C1 Si N3 158.30(8) . . . . ? C2 C1 Si N3 -110(2) . . . . ? N1 C1 Si N2 177.03(13) . . . . ? C2 C1 Si N2 -91(2) . . . . ? N2 C1 Si N4 -87.68(9) . . . . ? N1 C1 Si N4 89.35(9) . . . . ? C2 C1 Si N4 -179(100) . . . . ? N2 C1 Si S1 83.70(8) . . . . ? N1 C1 Si S1 -99.26(8) . . . . ? C2 C1 Si S1 -7(2) . . . . ? N2 C1 Si S2 177.82(7) . . . . ? N1 C1 Si S2 -5.14(10) . . . . ? C2 C1 Si S2 87(2) . . . . ? N2 C1 Si C14 -58.86(10) . . . . ? N1 C1 Si C14 118.17(9) . . . . ? C2 C1 Si C14 -150(2) . . . . ? N4 C14 Si N1 -18.47(11) . . . . ? N3 C14 Si N1 158.01(9) . . . . ? C15 C14 Si N1 -75.4(16) . . . . ? N4 C14 Si N3 -176.48(14) . . . . ? C15 C14 Si N3 126.6(16) . . . . ? N4 C14 Si N2 -87.65(9) . . . . ? N3 C14 Si N2 88.83(9) . . . . ? C15 C14 Si N2 -144.6(15) . . . . ? N3 C14 Si N4 176.48(14) . . . . ? C15 C14 Si N4 -56.9(15) . . . . ? N4 C14 Si S1 176.79(8) . . . . ? N3 C14 Si S1 -6.73(11) . . . . ? C15 C14 Si S1 119.9(15) . . . . ? N4 C14 Si S2 82.87(8) . . . . ? N3 C14 Si S2 -100.65(8) . . . . ? C15 C14 Si S2 25.9(15) . . . . ? N4 C14 Si C1 -58.54(10) . . . . ? N3 C14 Si C1 117.94(9) . . . . ? C15 C14 Si C1 -115.5(15) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 29.20 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.406 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.055 # *******************Data Compound 9 . 0.5 C7H8 ******************* data_jun13abu _database_code_depnum_ccdc_archive 'CCDC 775538' #TrackingRef '- bisamidinato_si_complexes_dalton_final_28_04_10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H42 N4 S Se Si, 1/2 (C7H8) ' _chemical_formula_sum 'C35.50 H46 N4 S Se Si' _chemical_formula_weight 667.87 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3497(10) _cell_length_b 20.1217(18) _cell_length_c 13.9760(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.054(10) _cell_angle_gamma 90.00 _cell_volume 3473.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4668 _cell_measurement_theta_min 6.85 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 1.206 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5479 _exptl_absorpt_correction_T_max 0.6263 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49552 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 29.14 _reflns_number_total 9258 _reflns_number_gt 7675 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+0.8953P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9258 _refine_ls_number_parameters 419 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.11864(11) 0.21934(7) 0.58262(11) 0.0205(3) Uani 1 1 d . A 2 C2 C 1.23847(11) 0.20814(8) 0.58534(11) 0.0228(3) Uani 1 1 d . A 2 C7 C 1.30238(13) 0.24204(9) 0.65198(14) 0.0330(4) Uani 1 1 d . A 2 H7 H 1.2703 0.2732 0.6945 0.040 Uiso 1 1 calc R A 2 C6 C 1.41372(14) 0.22978(11) 0.65573(15) 0.0405(4) Uani 1 1 d . A 2 H6 H 1.4573 0.2528 0.7009 0.049 Uiso 1 1 calc R A 2 C5 C 1.46115(13) 0.18424(10) 0.59412(15) 0.0372(4) Uani 1 1 d . A 2 H5 H 1.5368 0.1759 0.5975 0.045 Uiso 1 1 calc R A 2 C4 C 1.39809(13) 0.15087(9) 0.52758(14) 0.0320(4) Uani 1 1 d . A 2 H4 H 1.4306 0.1198 0.4852 0.038 Uiso 1 1 calc R A 2 C3 C 1.28656(12) 0.16288(8) 0.52269(12) 0.0259(3) Uani 1 1 d . A 2 H3 H 1.2436 0.1402 0.4767 0.031 Uiso 1 1 calc R A 2 C8 C 1.04880(11) 0.11142(7) 0.65522(11) 0.0214(3) Uani 1 1 d . A 2 H8 H 0.9799 0.1042 0.6912 0.026 Uiso 1 1 calc R A 2 C9 C 1.14053(13) 0.10305(8) 0.72790(12) 0.0292(3) Uani 1 1 d . A 2 H9A H 1.2100 0.1012 0.6942 0.044 Uiso 1 1 calc R A 2 H9B H 1.1298 0.0618 0.7639 0.044 Uiso 1 1 calc R A 2 H9C H 1.1406 0.1408 0.7722 0.044 Uiso 1 1 calc R A 2 C10 C 1.05280(14) 0.05764(8) 0.57794(13) 0.0287(3) Uani 1 1 d . A 2 H10A H 0.9927 0.0641 0.5331 0.043 Uiso 1 1 calc R A 2 H10B H 1.0467 0.0138 0.6079 0.043 Uiso 1 1 calc R A 2 H10C H 1.1216 0.0606 0.5433 0.043 Uiso 1 1 calc R A 2 C11 C 1.12461(12) 0.32918(8) 0.50085(13) 0.0271(3) Uani 1 1 d . A 2 H11 H 1.2042 0.3202 0.5024 0.033 Uiso 1 1 calc R A 2 C12 C 1.10404(15) 0.39320(9) 0.55636(16) 0.0388(4) Uani 1 1 d . A 2 H12A H 1.0262 0.4028 0.5568 0.058 Uiso 1 1 calc R A 2 H12B H 1.1428 0.4300 0.5257 0.058 Uiso 1 1 calc R A 2 H12C H 1.1299 0.3880 0.6223 0.058 Uiso 1 1 calc R A 2 C13 C 1.09057(16) 0.33566(10) 0.39620(15) 0.0400(4) Uani 1 1 d . A 2 H13A H 1.1084 0.2946 0.3620 0.060 Uiso 1 1 calc R A 2 H13B H 1.1291 0.3730 0.3668 0.060 Uiso 1 1 calc R A 2 H13C H 1.0124 0.3435 0.3926 0.060 Uiso 1 1 calc R A 2 C14 C 0.84789(11) 0.32747(7) 0.64766(11) 0.0204(3) Uani 1 1 d . A 2 C15 C 0.79221(12) 0.38232(7) 0.70101(11) 0.0218(3) Uani 1 1 d . A 2 C16 C 0.83791(14) 0.44581(8) 0.70578(13) 0.0313(3) Uani 1 1 d . A 2 H16 H 0.9021 0.4555 0.6710 0.038 Uiso 1 1 calc R A 2 C17 C 0.78918(16) 0.49479(9) 0.76157(14) 0.0360(4) Uani 1 1 d . A 2 H17 H 0.8201 0.5380 0.7646 0.043 Uiso 1 1 calc R A 2 C18 C 0.69537(14) 0.48079(9) 0.81293(13) 0.0329(4) Uani 1 1 d . A 2 H18 H 0.6628 0.5143 0.8512 0.039 Uiso 1 1 calc R A 2 C19 C 0.64945(13) 0.41792(9) 0.80816(12) 0.0299(3) Uani 1 1 d . A 2 H19 H 0.5851 0.4085 0.8428 0.036 Uiso 1 1 calc R A 2 C20 C 0.69777(12) 0.36842(8) 0.75250(12) 0.0261(3) Uani 1 1 d . A 2 H20 H 0.6665 0.3253 0.7496 0.031 Uiso 1 1 calc R A 2 C21 C 0.93417(12) 0.28020(8) 0.79242(11) 0.0235(3) Uani 1 1 d . A 2 H21 H 0.8934 0.3173 0.8235 0.028 Uiso 1 1 calc R A 2 C22 C 1.05482(14) 0.29338(9) 0.80747(13) 0.0324(4) Uani 1 1 d . A 2 H22A H 1.0969 0.2567 0.7802 0.049 Uiso 1 1 calc R A 2 H22B H 1.0700 0.2969 0.8761 0.049 Uiso 1 1 calc R A 2 H22C H 1.0749 0.3350 0.7757 0.049 Uiso 1 1 calc R A 2 C23 C 0.89848(14) 0.21551(9) 0.84009(12) 0.0312(3) Uani 1 1 d . A 2 H23A H 0.8213 0.2082 0.8278 0.047 Uiso 1 1 calc R A 2 H23B H 0.9109 0.2185 0.9092 0.047 Uiso 1 1 calc R A 2 H23C H 0.9404 0.1784 0.8138 0.047 Uiso 1 1 calc R A 2 C24 C 0.77526(12) 0.34197(8) 0.48023(11) 0.0239(3) Uani 1 1 d . A 2 H24 H 0.7924 0.3183 0.4192 0.029 Uiso 1 1 calc R A 2 C25 C 0.79423(15) 0.41629(9) 0.46178(15) 0.0365(4) Uani 1 1 d . A 2 H25A H 0.7722 0.4418 0.5182 0.055 Uiso 1 1 calc R A 2 H25B H 0.7514 0.4304 0.4063 0.055 Uiso 1 1 calc R A 2 H25C H 0.8712 0.4240 0.4490 0.055 Uiso 1 1 calc R A 2 C26 C 0.65606(13) 0.32781(10) 0.50234(14) 0.0348(4) Uani 1 1 d . A 2 H26A H 0.6458 0.2799 0.5115 0.052 Uiso 1 1 calc R A 2 H26B H 0.6110 0.3430 0.4489 0.052 Uiso 1 1 calc R A 2 H26C H 0.6351 0.3514 0.5608 0.052 Uiso 1 1 calc R A 2 C27 C 0.75747(12) 0.12164(7) 0.49759(12) 0.0251(3) Uani 1 1 d . A 2 C28 C 0.81834(13) 0.13582(8) 0.41557(12) 0.0268(3) Uani 1 1 d . A 2 C29 C 0.79665(17) 0.10088(10) 0.33078(14) 0.0389(4) Uani 1 1 d . A 2 H29 H 0.8376 0.1103 0.2749 0.047 Uiso 1 1 calc R A 2 C30 C 0.7163(2) 0.05272(10) 0.32722(18) 0.0504(6) Uani 1 1 d . A 2 H30 H 0.7025 0.0296 0.2692 0.061 Uiso 1 1 calc R A 2 C31 C 0.65626(19) 0.03841(9) 0.40841(19) 0.0500(6) Uani 1 1 d . A 2 H31 H 0.6015 0.0053 0.4062 0.060 Uiso 1 1 calc R A 2 C32 C 0.67650(14) 0.07284(9) 0.49351(16) 0.0369(4) Uani 1 1 d . A 2 H32 H 0.6351 0.0631 0.5490 0.044 Uiso 1 1 calc R A 2 C39 C 0.5969(4) 0.5808(4) 0.4362(5) 0.053(3) Uani 0.50 1 d PD B -1 H39A H 0.6589 0.5613 0.4028 0.079 Uiso 0.50 1 calc PR B -1 H39B H 0.6229 0.6092 0.4884 0.079 Uiso 0.50 1 calc PR B -1 H39C H 0.5543 0.6075 0.3912 0.079 Uiso 0.50 1 calc PR B -1 C33 C 0.5353(2) 0.51062(16) 0.5737(2) 0.0362(18) Uani 0.50 1 d PGD B -1 H33 H 0.5849 0.5344 0.6129 0.043 Uiso 0.50 1 calc PR B -1 C34 C 0.4716(3) 0.46071(17) 0.61320(19) 0.0460(10) Uani 0.50 1 d PGD B -1 H34 H 0.4777 0.4504 0.6793 0.055 Uiso 0.50 1 calc PR B -1 C35 C 0.3991(3) 0.42590(15) 0.5559(2) 0.058(4) Uani 0.50 1 d PGD B -1 H35 H 0.3556 0.3918 0.5829 0.070 Uiso 0.50 1 calc PR B -1 C36 C 0.3903(2) 0.44099(16) 0.4592(2) 0.0446(10) Uani 0.50 1 d PGD B -1 H36 H 0.3407 0.4172 0.4201 0.054 Uiso 0.50 1 calc PR B -1 C37 C 0.4539(3) 0.49090(16) 0.41971(18) 0.047(2) Uani 0.50 1 d PGD B -1 H37 H 0.4479 0.5012 0.3536 0.056 Uiso 0.50 1 calc PR B -1 C38 C 0.5265(2) 0.52571(15) 0.4770(2) 0.0371(8) Uani 0.50 1 d PGD B -1 N1 N 1.04135(9) 0.17839(6) 0.61357(9) 0.0203(2) Uani 1 1 d . A 2 N2 N 1.06944(9) 0.27258(6) 0.54628(9) 0.0212(2) Uani 1 1 d . A 2 N4 N 0.90585(10) 0.28023(6) 0.69019(9) 0.0205(2) Uani 1 1 d . A 2 N3 N 0.84813(10) 0.31454(6) 0.55390(9) 0.0202(2) Uani 1 1 d . A 2 S1 S 0.7842(7) 0.1703(4) 0.6071(7) 0.02164(19) Uani 0.4068(11) 1 d PD A 2 S2 S 0.9240(8) 0.1994(5) 0.4198(5) 0.0246(4) Uani 0.5932(11) 1 d PD A 2 Se1 Se 0.77985(19) 0.16450(11) 0.61523(18) 0.02164(19) Uani 0.5932(11) 1 d PD A 2 Se2 Se 0.9262(5) 0.1977(3) 0.4064(3) 0.0246(4) Uani 0.4068(11) 1 d PD A 2 Si Si 0.92887(3) 0.235077(19) 0.57088(3) 0.01800(8) Uani 1 1 d D A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0186(6) 0.0211(7) 0.0218(7) -0.0019(6) 0.0003(5) -0.0003(5) C2 0.0183(6) 0.0229(7) 0.0272(7) 0.0026(6) 0.0012(5) -0.0006(5) C7 0.0235(7) 0.0356(9) 0.0399(10) -0.0102(8) -0.0009(6) -0.0017(6) C6 0.0239(8) 0.0498(11) 0.0477(11) -0.0067(9) -0.0063(7) -0.0048(7) C5 0.0189(7) 0.0444(10) 0.0483(11) 0.0084(9) 0.0008(7) 0.0041(7) C4 0.0253(7) 0.0346(9) 0.0361(9) 0.0043(7) 0.0076(6) 0.0076(6) C3 0.0229(7) 0.0280(8) 0.0267(8) 0.0013(6) 0.0034(6) 0.0012(6) C8 0.0221(6) 0.0188(6) 0.0233(7) 0.0016(6) 0.0012(5) 0.0016(5) C9 0.0334(8) 0.0259(8) 0.0285(8) 0.0013(6) -0.0059(6) 0.0046(6) C10 0.0342(8) 0.0206(7) 0.0314(8) -0.0033(6) -0.0015(6) 0.0007(6) C11 0.0219(7) 0.0245(7) 0.0351(9) 0.0065(7) 0.0054(6) -0.0021(5) C12 0.0371(9) 0.0241(8) 0.0551(12) 0.0021(8) 0.0063(8) -0.0052(7) C13 0.0402(10) 0.0414(11) 0.0384(10) 0.0147(8) 0.0048(8) -0.0049(8) C14 0.0197(6) 0.0176(6) 0.0238(7) -0.0020(5) 0.0010(5) -0.0003(5) C15 0.0234(6) 0.0197(7) 0.0225(7) -0.0012(6) -0.0006(5) 0.0041(5) C16 0.0356(8) 0.0237(8) 0.0348(9) -0.0051(7) 0.0070(7) -0.0029(6) C17 0.0465(10) 0.0214(8) 0.0401(10) -0.0076(7) 0.0049(8) -0.0012(7) C18 0.0380(9) 0.0302(8) 0.0304(9) -0.0072(7) 0.0012(7) 0.0104(7) C19 0.0281(7) 0.0335(8) 0.0281(8) -0.0021(7) 0.0030(6) 0.0062(6) C20 0.0258(7) 0.0238(7) 0.0289(8) -0.0006(6) 0.0015(6) 0.0011(6) C21 0.0260(7) 0.0249(7) 0.0196(7) -0.0023(6) -0.0007(5) 0.0034(5) C22 0.0309(8) 0.0374(9) 0.0287(8) -0.0017(7) -0.0053(6) -0.0057(7) C23 0.0333(8) 0.0353(9) 0.0250(8) 0.0055(7) 0.0006(6) -0.0030(7) C24 0.0248(7) 0.0244(7) 0.0226(7) -0.0002(6) -0.0037(5) 0.0040(5) C25 0.0409(9) 0.0267(8) 0.0417(10) 0.0091(7) -0.0111(8) 0.0027(7) C26 0.0244(7) 0.0441(10) 0.0357(9) 0.0037(8) -0.0071(7) 0.0008(7) C27 0.0228(7) 0.0191(7) 0.0333(8) -0.0022(6) -0.0078(6) 0.0023(5) C28 0.0281(7) 0.0228(7) 0.0296(8) -0.0034(6) -0.0069(6) 0.0089(6) C29 0.0503(10) 0.0349(9) 0.0315(9) -0.0104(8) -0.0127(8) 0.0203(8) C30 0.0650(13) 0.0306(9) 0.0557(13) -0.0190(9) -0.0368(12) 0.0171(9) C31 0.0514(11) 0.0225(8) 0.0760(16) -0.0054(9) -0.0352(12) -0.0018(8) C32 0.0310(8) 0.0241(8) 0.0555(12) 0.0030(8) -0.0133(8) -0.0026(6) C39 0.037(4) 0.058(5) 0.063(6) 0.008(4) 0.026(4) -0.007(3) C33 0.030(3) 0.043(4) 0.035(4) -0.005(3) -0.002(3) -0.002(3) C34 0.040(2) 0.061(3) 0.037(2) 0.009(2) 0.0036(16) 0.0102(19) C35 0.049(5) 0.027(3) 0.099(9) 0.013(4) 0.000(5) 0.004(3) C36 0.0364(19) 0.037(2) 0.060(3) -0.013(2) -0.0093(18) 0.0053(16) C37 0.045(3) 0.058(6) 0.037(4) -0.005(4) 0.001(3) 0.019(4) C38 0.0288(16) 0.0369(19) 0.046(2) -0.0009(17) 0.0078(14) 0.0051(14) N1 0.0181(5) 0.0174(5) 0.0252(6) 0.0006(5) 0.0008(4) 0.0005(4) N2 0.0172(5) 0.0197(6) 0.0267(6) 0.0029(5) 0.0012(4) -0.0008(4) N4 0.0221(5) 0.0203(6) 0.0191(6) -0.0010(5) -0.0002(4) 0.0028(4) N3 0.0199(5) 0.0192(6) 0.0214(6) 0.0001(5) -0.0008(4) 0.0023(4) S1 0.0192(2) 0.0190(5) 0.0268(5) 0.0004(3) 0.0008(2) -0.0029(2) S2 0.0262(2) 0.0280(3) 0.0196(10) -0.0045(8) 0.0026(7) 0.00236(19) Se1 0.0192(2) 0.0190(5) 0.0268(5) 0.0004(3) 0.0008(2) -0.0029(2) Se2 0.0262(2) 0.0280(3) 0.0196(10) -0.0045(8) 0.0026(7) 0.00236(19) Si 0.01664(16) 0.01693(18) 0.02044(19) -0.00042(15) 0.00050(13) 0.00122(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.3320(19) . ? C1 N1 1.3334(19) . ? C1 C2 1.4973(19) . ? C1 Si 2.3705(14) . ? C2 C3 1.396(2) . ? C2 C7 1.398(2) . ? C7 C6 1.398(2) . ? C6 C5 1.388(3) . ? C5 C4 1.386(3) . ? C4 C3 1.400(2) . ? C8 N1 1.4706(19) . ? C8 C10 1.530(2) . ? C8 C9 1.530(2) . ? C11 N2 1.4715(19) . ? C11 C12 1.525(3) . ? C11 C13 1.527(3) . ? C14 N4 1.3297(18) . ? C14 N3 1.3359(19) . ? C14 C15 1.499(2) . ? C14 Si 2.3685(15) . ? C15 C16 1.398(2) . ? C15 C20 1.399(2) . ? C16 C17 1.394(2) . ? C17 C18 1.392(3) . ? C18 C19 1.388(3) . ? C19 C20 1.398(2) . ? C21 N4 1.4706(19) . ? C21 C23 1.527(2) . ? C21 C22 1.528(2) . ? C24 N3 1.4742(18) . ? C24 C26 1.531(2) . ? C24 C25 1.536(2) . ? C27 C28 1.401(2) . ? C27 C32 1.403(2) . ? C27 S1 1.846(11) . ? C27 Se1 1.877(3) . ? C28 C29 1.404(2) . ? C28 Se2 1.828(6) . ? C28 S2 1.828(11) . ? C29 C30 1.387(3) . ? C30 C31 1.387(4) . ? C31 C32 1.399(3) . ? C39 C38 1.521(6) . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? N1 Si 1.8935(13) . ? N2 Si 1.9241(12) . ? N4 Si 1.9204(13) . ? N3 Si 1.8991(13) . ? S1 Si 2.269(8) . ? S2 Si 2.231(7) . ? Se1 Si 2.4064(19) . ? Se2 Si 2.419(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 N2 C1 N1 107.11(12) . . ? N2 C1 C2 125.54(13) . . ? N1 C1 C2 127.34(13) . . ? N2 C1 Si 54.23(7) . . ? N1 C1 Si 52.92(7) . . ? C2 C1 Si 177.31(11) . . ? C3 C2 C7 119.72(14) . . ? C3 C2 C1 120.21(14) . . ? C7 C2 C1 120.06(14) . . ? C6 C7 C2 119.58(17) . . ? C5 C6 C7 120.60(17) . . ? C4 C5 C6 119.94(16) . . ? C5 C4 C3 120.09(17) . . ? C2 C3 C4 120.06(15) . . ? N1 C8 C10 111.77(13) . . ? N1 C8 C9 114.18(12) . . ? C10 C8 C9 111.50(13) . . ? N2 C11 C12 110.90(14) . . ? N2 C11 C13 110.62(14) . . ? C12 C11 C13 111.66(15) . . ? N4 C14 N3 107.31(12) . . ? N4 C14 C15 123.42(14) . . ? N3 C14 C15 129.24(13) . . ? N4 C14 Si 54.14(7) . . ? N3 C14 Si 53.23(7) . . ? C15 C14 Si 175.69(11) . . ? C16 C15 C20 119.65(15) . . ? C16 C15 C14 120.73(14) . . ? C20 C15 C14 119.44(14) . . ? C17 C16 C15 119.89(16) . . ? C18 C17 C16 120.36(17) . . ? C19 C18 C17 119.98(16) . . ? C18 C19 C20 120.11(16) . . ? C19 C20 C15 120.02(15) . . ? N4 C21 C23 110.84(13) . . ? N4 C21 C22 111.39(13) . . ? C23 C21 C22 111.70(13) . . ? N3 C24 C26 112.07(13) . . ? N3 C24 C25 112.88(13) . . ? C26 C24 C25 111.22(14) . . ? C28 C27 C32 119.50(16) . . ? C28 C27 S1 118.3(3) . . ? C32 C27 S1 122.1(3) . . ? C28 C27 Se1 123.00(13) . . ? C32 C27 Se1 117.50(15) . . ? S1 C27 Se1 5.2(3) . . ? C27 C28 C29 119.13(17) . . ? C27 C28 Se2 126.02(16) . . ? C29 C28 Se2 114.85(19) . . ? C27 C28 S2 120.0(2) . . ? C29 C28 S2 120.9(3) . . ? Se2 C28 S2 6.1(3) . . ? C30 C29 C28 121.1(2) . . ? C31 C30 C29 119.92(18) . . ? C30 C31 C32 119.84(19) . . ? C31 C32 C27 120.5(2) . . ? C34 C33 C38 120.0 . . ? C35 C34 C33 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C37 120.0 . . ? C38 C37 C36 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 C39 121.4(4) . . ? C33 C38 C39 118.6(4) . . ? C1 N1 C8 130.55(12) . . ? C1 N1 Si 92.90(9) . . ? C8 N1 Si 136.24(10) . . ? C1 N2 C11 125.15(12) . . ? C1 N2 Si 91.59(9) . . ? C11 N2 Si 143.02(10) . . ? C14 N4 C21 124.20(13) . . ? C14 N4 Si 91.72(9) . . ? C21 N4 Si 143.91(10) . . ? C14 N3 C24 127.61(12) . . ? C14 N3 Si 92.47(9) . . ? C24 N3 Si 136.27(10) . . ? C27 S1 Si 105.1(4) . . ? C28 S2 Si 105.9(4) . . ? C27 Se1 Si 99.06(10) . . ? C28 Se2 Si 98.87(19) . . ? N1 Si N3 158.67(6) . . ? N1 Si N4 96.93(6) . . ? N3 Si N4 68.41(5) . . ? N1 Si N2 68.34(5) . . ? N3 Si N2 96.96(6) . . ? N4 Si N2 95.96(6) . . ? N1 Si S2 97.1(3) . . ? N3 Si S2 98.0(3) . . ? N4 Si S2 166.0(3) . . ? N2 Si S2 88.9(3) . . ? N1 Si S1 99.3(2) . . ? N3 Si S1 95.6(2) . . ? N4 Si S1 87.8(3) . . ? N2 Si S1 167.4(2) . . ? S2 Si S1 90.3(4) . . ? N1 Si C14 129.80(6) . . ? N3 Si C14 34.30(5) . . ? N4 Si C14 34.14(5) . . ? N2 Si C14 98.89(5) . . ? S2 Si C14 132.1(3) . . ? S1 Si C14 91.0(3) . . ? N1 Si C1 34.18(5) . . ? N3 Si C1 129.80(5) . . ? N4 Si C1 98.64(5) . . ? N2 Si C1 34.17(5) . . ? S2 Si C1 92.8(3) . . ? S1 Si C1 133.4(2) . . ? C14 Si C1 119.43(5) . . ? N1 Si Se1 97.14(7) . . ? N3 Si Se1 97.32(7) . . ? N4 Si Se1 86.66(8) . . ? N2 Si Se1 165.43(7) . . ? S2 Si Se1 91.9(3) . . ? S1 Si Se1 2.5(3) . . ? C14 Si Se1 91.33(7) . . ? C1 Si Se1 131.27(7) . . ? N1 Si Se2 96.97(14) . . ? N3 Si Se2 97.85(15) . . ? N4 Si Se2 166.04(15) . . ? N2 Si Se2 87.92(14) . . ? S2 Si Se2 1.0(4) . . ? S1 Si Se2 91.3(3) . . ? C14 Si Se2 132.02(15) . . ? C1 Si Se2 92.11(14) . . ? Se1 Si Se2 92.95(15) . . ? 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 C1 C2 C3 -105.44(18) . . . . ? N1 C1 C2 C3 73.1(2) . . . . ? Si C1 C2 C3 -21(3) . . . . ? N2 C1 C2 C7 75.8(2) . . . . ? N1 C1 C2 C7 -105.6(2) . . . . ? Si C1 C2 C7 160(2) . . . . ? C3 C2 C7 C6 -0.6(3) . . . . ? C1 C2 C7 C6 178.16(17) . . . . ? C2 C7 C6 C5 -0.1(3) . . . . ? C7 C6 C5 C4 0.5(3) . . . . ? C6 C5 C4 C3 -0.2(3) . . . . ? C7 C2 C3 C4 0.9(2) . . . . ? C1 C2 C3 C4 -177.85(15) . . . . ? C5 C4 C3 C2 -0.5(3) . . . . ? N4 C14 C15 C16 100.69(19) . . . . ? N3 C14 C15 C16 -81.4(2) . . . . ? Si C14 C15 C16 155.1(13) . . . . ? N4 C14 C15 C20 -74.45(19) . . . . ? N3 C14 C15 C20 103.48(19) . . . . ? Si C14 C15 C20 -20.1(15) . . . . ? C20 C15 C16 C17 -0.1(3) . . . . ? C14 C15 C16 C17 -175.21(16) . . . . ? C15 C16 C17 C18 0.2(3) . . . . ? C16 C17 C18 C19 -0.5(3) . . . . ? C17 C18 C19 C20 0.5(3) . . . . ? C18 C19 C20 C15 -0.4(2) . . . . ? C16 C15 C20 C19 0.2(2) . . . . ? C14 C15 C20 C19 175.35(14) . . . . ? C32 C27 C28 C29 0.2(2) . . . . ? S1 C27 C28 C29 -177.9(4) . . . . ? Se1 C27 C28 C29 179.44(15) . . . . ? C32 C27 C28 Se2 179.6(3) . . . . ? S1 C27 C28 Se2 1.6(4) . . . . ? Se1 C27 C28 Se2 -1.1(3) . . . . ? C32 C27 C28 S2 179.9(4) . . . . ? S1 C27 C28 S2 1.9(5) . . . . ? Se1 C27 C28 S2 -0.8(4) . . . . ? C27 C28 C29 C30 -0.1(2) . . . . ? Se2 C28 C29 C30 -179.6(2) . . . . ? S2 C28 C29 C30 -179.8(4) . . . . ? C28 C29 C30 C31 -0.2(3) . . . . ? C29 C30 C31 C32 0.3(3) . . . . ? C30 C31 C32 C27 -0.2(3) . . . . ? C28 C27 C32 C31 0.0(2) . . . . ? S1 C27 C32 C31 177.9(4) . . . . ? Se1 C27 C32 C31 -179.31(16) . . . . ? C38 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C33 0.0 . . . . ? C36 C37 C38 C39 -179.7(4) . . . . ? C34 C33 C38 C37 0.0 . . . . ? C34 C33 C38 C39 179.7(4) . . . . ? N2 C1 N1 C8 176.48(14) . . . . ? C2 C1 N1 C8 -2.3(3) . . . . ? Si C1 N1 C8 174.37(19) . . . . ? N2 C1 N1 Si 2.11(12) . . . . ? C2 C1 N1 Si -176.63(14) . . . . ? C10 C8 N1 C1 -85.41(19) . . . . ? C9 C8 N1 C1 42.3(2) . . . . ? C10 C8 N1 Si 86.44(17) . . . . ? C9 C8 N1 Si -145.85(13) . . . . ? N1 C1 N2 C11 -177.61(14) . . . . ? C2 C1 N2 C11 1.2(2) . . . . ? Si C1 N2 C11 -175.53(17) . . . . ? N1 C1 N2 Si -2.08(12) . . . . ? C2 C1 N2 Si 176.70(14) . . . . ? C12 C11 N2 C1 -117.79(17) . . . . ? C13 C11 N2 C1 117.74(17) . . . . ? C12 C11 N2 Si 69.6(2) . . . . ? C13 C11 N2 Si -54.8(2) . . . . ? N3 C14 N4 C21 173.68(13) . . . . ? C15 C14 N4 C21 -8.0(2) . . . . ? Si C14 N4 C21 176.33(16) . . . . ? N3 C14 N4 Si -2.64(12) . . . . ? C15 C14 N4 Si 175.68(12) . . . . ? C23 C21 N4 C14 125.48(15) . . . . ? C22 C21 N4 C14 -109.50(16) . . . . ? C23 C21 N4 Si -60.8(2) . . . . ? C22 C21 N4 Si 64.3(2) . . . . ? N4 C14 N3 C24 163.81(14) . . . . ? C15 C14 N3 C24 -14.4(2) . . . . ? Si C14 N3 C24 161.13(17) . . . . ? N4 C14 N3 Si 2.67(12) . . . . ? C15 C14 N3 Si -175.52(14) . . . . ? C26 C24 N3 C14 -57.5(2) . . . . ? C25 C24 N3 C14 69.0(2) . . . . ? C26 C24 N3 Si 94.60(17) . . . . ? C25 C24 N3 Si -138.88(14) . . . . ? C28 C27 S1 Si -5.4(5) . . . . ? C32 C27 S1 Si 176.61(18) . . . . ? Se1 C27 S1 Si 149(4) . . . . ? C27 C28 S2 Si 2.7(6) . . . . ? C29 C28 S2 Si -177.5(2) . . . . ? Se2 C28 S2 Si -180(100) . . . . ? C28 C27 Se1 Si -1.36(18) . . . . ? C32 C27 Se1 Si 177.92(12) . . . . ? S1 C27 Se1 Si -29(4) . . . . ? C27 C28 Se2 Si 2.9(3) . . . . ? C29 C28 Se2 Si -177.69(14) . . . . ? S2 C28 Se2 Si 0(5) . . . . ? C1 N1 Si N3 -50.3(2) . . . . ? C8 N1 Si N3 135.90(17) . . . . ? C1 N1 Si N4 -95.19(10) . . . . ? C8 N1 Si N4 91.00(15) . . . . ? C1 N1 Si N2 -1.50(9) . . . . ? C8 N1 Si N2 -175.31(16) . . . . ? C1 N1 Si S2 84.5(3) . . . . ? C8 N1 Si S2 -89.3(3) . . . . ? C1 N1 Si S1 176.0(3) . . . . ? C8 N1 Si S1 2.2(3) . . . . ? C1 N1 Si C14 -84.93(11) . . . . ? C8 N1 Si C14 101.26(15) . . . . ? C8 N1 Si C1 -173.8(2) . . . . ? C1 N1 Si Se1 177.33(11) . . . . ? C8 N1 Si Se1 3.52(16) . . . . ? C1 N1 Si Se2 83.45(17) . . . . ? C8 N1 Si Se2 -90.4(2) . . . . ? C14 N3 Si N1 -50.8(2) . . . . ? C24 N3 Si N1 150.94(16) . . . . ? C14 N3 Si N4 -1.90(8) . . . . ? C24 N3 Si N4 -160.15(16) . . . . ? C14 N3 Si N2 -95.58(9) . . . . ? C24 N3 Si N2 106.17(15) . . . . ? C14 N3 Si S2 174.6(3) . . . . ? C24 N3 Si S2 16.3(3) . . . . ? C14 N3 Si S1 83.4(3) . . . . ? C24 N3 Si S1 -74.8(3) . . . . ? C24 N3 Si C14 -158.2(2) . . . . ? C14 N3 Si C1 -85.04(10) . . . . ? C24 N3 Si C1 116.71(14) . . . . ? C14 N3 Si Se1 81.55(10) . . . . ? C24 N3 Si Se1 -76.70(16) . . . . ? C14 N3 Si Se2 175.57(16) . . . . ? C24 N3 Si Se2 17.3(2) . . . . ? C14 N4 Si N1 165.88(9) . . . . ? C21 N4 Si N1 -8.96(18) . . . . ? C14 N4 Si N3 1.91(8) . . . . ? C21 N4 Si N3 -172.93(19) . . . . ? C14 N4 Si N2 97.06(9) . . . . ? C21 N4 Si N2 -77.78(18) . . . . ? C14 N4 Si S2 -12.7(11) . . . . ? C21 N4 Si S2 172.4(11) . . . . ? C14 N4 Si S1 -95.0(2) . . . . ? C21 N4 Si S1 90.1(3) . . . . ? C21 N4 Si C14 -174.8(2) . . . . ? C14 N4 Si C1 131.42(9) . . . . ? C21 N4 Si C1 -43.42(18) . . . . ? C14 N4 Si Se1 -97.32(10) . . . . ? C21 N4 Si Se1 87.84(18) . . . . ? C14 N4 Si Se2 -8.5(6) . . . . ? C21 N4 Si Se2 176.6(6) . . . . ? C1 N2 Si N1 1.50(9) . . . . ? C11 N2 Si N1 175.4(2) . . . . ? C1 N2 Si N3 165.51(9) . . . . ? C11 N2 Si N3 -20.57(19) . . . . ? C1 N2 Si N4 96.61(9) . . . . ? C11 N2 Si N4 -89.47(19) . . . . ? C1 N2 Si S2 -96.6(3) . . . . ? C11 N2 Si S2 77.4(3) . . . . ? C1 N2 Si S1 -10.0(12) . . . . ? C11 N2 Si S1 163.9(12) . . . . ? C1 N2 Si C14 130.92(9) . . . . ? C11 N2 Si C14 -55.16(19) . . . . ? C11 N2 Si C1 173.9(2) . . . . ? C1 N2 Si Se1 -3.1(3) . . . . ? C11 N2 Si Se1 170.8(3) . . . . ? C1 N2 Si Se2 -96.84(17) . . . . ? C11 N2 Si Se2 77.1(2) . . . . ? C28 S2 Si N1 94.7(4) . . . . ? C28 S2 Si N3 -100.4(4) . . . . ? C28 S2 Si N4 -86.7(12) . . . . ? C28 S2 Si N2 162.7(4) . . . . ? C28 S2 Si S1 -4.7(5) . . . . ? C28 S2 Si C14 -96.3(5) . . . . ? C28 S2 Si C1 128.8(4) . . . . ? C28 S2 Si Se1 -2.7(4) . . . . ? C28 S2 Si Se2 179(100) . . . . ? C27 S1 Si N1 -91.8(4) . . . . ? C27 S1 Si N3 103.5(4) . . . . ? C27 S1 Si N4 171.6(4) . . . . ? C27 S1 Si N2 -80.9(13) . . . . ? C27 S1 Si S2 5.4(5) . . . . ? C27 S1 Si C14 137.6(4) . . . . ? C27 S1 Si C1 -88.7(4) . . . . ? C27 S1 Si Se1 -124(8) . . . . ? C27 S1 Si Se2 5.5(4) . . . . ? N4 C14 Si N1 -18.37(12) . . . . ? N3 C14 Si N1 158.48(9) . . . . ? C15 C14 Si N1 -75.2(14) . . . . ? N4 C14 Si N3 -176.85(14) . . . . ? C15 C14 Si N3 126.3(14) . . . . ? N3 C14 Si N4 176.85(14) . . . . ? C15 C14 Si N4 -56.8(14) . . . . ? N4 C14 Si N2 -87.51(9) . . . . ? N3 C14 Si N2 89.33(9) . . . . ? C15 C14 Si N2 -144.3(14) . . . . ? N4 C14 Si S2 175.9(4) . . . . ? N3 C14 Si S2 -7.3(4) . . . . ? C15 C14 Si S2 119.1(14) . . . . ? N4 C14 Si S1 84.6(3) . . . . ? N3 C14 Si S1 -98.6(3) . . . . ? C15 C14 Si S1 27.8(14) . . . . ? N4 C14 Si C1 -58.35(10) . . . . ? N3 C14 Si C1 118.50(9) . . . . ? C15 C14 Si C1 -115.2(14) . . . . ? N4 C14 Si Se1 82.06(10) . . . . ? N3 C14 Si Se1 -101.09(10) . . . . ? C15 C14 Si Se1 25.2(14) . . . . ? N4 C14 Si Se2 177.2(2) . . . . ? N3 C14 Si Se2 -5.9(2) . . . . ? C15 C14 Si Se2 120.4(14) . . . . ? N2 C1 Si N1 -177.51(14) . . . . ? C2 C1 Si N1 96(2) . . . . ? N2 C1 Si N3 -18.87(12) . . . . ? N1 C1 Si N3 158.65(10) . . . . ? C2 C1 Si N3 -105(2) . . . . ? N2 C1 Si N4 -87.89(10) . . . . ? N1 C1 Si N4 89.62(10) . . . . ? C2 C1 Si N4 -174(2) . . . . ? N1 C1 Si N2 177.51(14) . . . . ? C2 C1 Si N2 -86(2) . . . . ? N2 C1 Si S2 83.9(3) . . . . ? N1 C1 Si S2 -98.5(3) . . . . ? C2 C1 Si S2 -2(2) . . . . ? N2 C1 Si S1 177.0(4) . . . . ? N1 C1 Si S1 -5.5(4) . . . . ? C2 C1 Si S1 91(2) . . . . ? N2 C1 Si C14 -59.00(11) . . . . ? N1 C1 Si C14 118.51(10) . . . . ? C2 C1 Si C14 -145(2) . . . . ? N2 C1 Si Se1 178.96(12) . . . . ? N1 C1 Si Se1 -3.53(14) . . . . ? C2 C1 Si Se1 93(2) . . . . ? N2 C1 Si Se2 83.17(17) . . . . ? N1 C1 Si Se2 -99.32(17) . . . . ? C2 C1 Si Se2 -3(2) . . . . ? C27 Se1 Si N1 -95.10(10) . . . . ? C27 Se1 Si N3 100.62(10) . . . . ? C27 Se1 Si N4 168.34(11) . . . . ? C27 Se1 Si N2 -90.8(3) . . . . ? C27 Se1 Si S2 2.3(3) . . . . ? C27 Se1 Si S1 53(8) . . . . ? C27 Se1 Si C14 134.50(10) . . . . ? C27 Se1 Si C1 -93.10(12) . . . . ? C27 Se1 Si Se2 2.31(17) . . . . ? C28 Se2 Si N1 94.9(2) . . . . ? C28 Se2 Si N3 -100.5(2) . . . . ? C28 Se2 Si N4 -90.7(6) . . . . ? C28 Se2 Si N2 162.8(2) . . . . ? C28 Se2 Si S2 -1(24) . . . . ? C28 Se2 Si S1 -4.7(3) . . . . ? C28 Se2 Si C14 -97.1(2) . . . . ? C28 Se2 Si C1 128.8(2) . . . . ? C28 Se2 Si Se1 -2.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.445 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.059 # *******************Data Compound 10 . 0.5 C7H8 ******************* data_jun12u _database_code_depnum_ccdc_archive 'CCDC 775539' #TrackingRef '- bisamidinato_si_complexes_dalton_final_28_04_10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H42 N4 Se2 Si, 1/2 (C7H8) ' _chemical_formula_sum 'C35.50 H46 N4 Se2 Si' _chemical_formula_weight 714.77 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.370(3) _cell_length_b 20.230(4) _cell_length_c 13.968(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.15(3) _cell_angle_gamma 90.00 _cell_volume 3495.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.3 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 2.179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.3813 _exptl_absorpt_correction_T_max 0.4196 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 image_plate_Stoe_IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41663 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 29.14 _reflns_number_total 9336 _reflns_number_gt 7014 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9336 _refine_ls_number_parameters 371 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 C1 C 1.11742(17) 0.21923(10) 0.58138(15) 0.0189(4) Uani 1 1 d . A 2 C2 C 1.23690(17) 0.20753(10) 0.58312(17) 0.0214(4) Uani 1 1 d . A 2 C7 C 1.30220(19) 0.24157(13) 0.64798(19) 0.0304(5) Uani 1 1 d . A 2 H7 H 1.2713 0.2730 0.6903 0.037 Uiso 1 1 calc R A 2 C6 C 1.4133(2) 0.22912(15) 0.6503(2) 0.0377(6) Uani 1 1 d . A 2 H6 H 1.4580 0.2522 0.6946 0.045 Uiso 1 1 calc R A 2 C5 C 1.45879(19) 0.18330(14) 0.5884(2) 0.0333(6) Uani 1 1 d . A 2 H5 H 1.5343 0.1749 0.5905 0.040 Uiso 1 1 calc R A 2 C4 C 1.39392(19) 0.14986(12) 0.52345(18) 0.0285(5) Uani 1 1 d . A 2 H4 H 1.4251 0.1185 0.4810 0.034 Uiso 1 1 calc R A 2 C3 C 1.28281(18) 0.16209(11) 0.52016(17) 0.0246(4) Uani 1 1 d . A 2 H3 H 1.2386 0.1395 0.4751 0.030 Uiso 1 1 calc R A 2 C8 C 1.04746(17) 0.11189(10) 0.65468(16) 0.0200(4) Uani 1 1 d . A 2 H8 H 0.9790 0.1050 0.6912 0.024 Uiso 1 1 calc R A 2 C9 C 1.1398(2) 0.10372(12) 0.72701(18) 0.0278(5) Uani 1 1 d . A 2 H9A H 1.2088 0.1017 0.6929 0.042 Uiso 1 1 calc R A 2 H9B H 1.1293 0.0628 0.7634 0.042 Uiso 1 1 calc R A 2 H9C H 1.1403 0.1415 0.7710 0.042 Uiso 1 1 calc R A 2 C10 C 1.0503(2) 0.05792(11) 0.57812(18) 0.0276(5) Uani 1 1 d . A 2 H10A H 0.9891 0.0637 0.5342 0.041 Uiso 1 1 calc R A 2 H10B H 1.0456 0.0145 0.6088 0.041 Uiso 1 1 calc R A 2 H10C H 1.1181 0.0610 0.5422 0.041 Uiso 1 1 calc R A 2 C11 C 1.12392(18) 0.32878(11) 0.49984(18) 0.0257(5) Uani 1 1 d . A 2 H11 H 1.2034 0.3197 0.5014 0.031 Uiso 1 1 calc R A 2 C12 C 1.1038(2) 0.39276(12) 0.5554(2) 0.0364(6) Uani 1 1 d . A 2 H12A H 1.0260 0.4020 0.5569 0.055 Uiso 1 1 calc R A 2 H12B H 1.1414 0.4294 0.5238 0.055 Uiso 1 1 calc R A 2 H12C H 1.1310 0.3879 0.6210 0.055 Uiso 1 1 calc R A 2 C13 C 1.0898(2) 0.33538(15) 0.3950(2) 0.0396(6) Uani 1 1 d . A 2 H13A H 1.1073 0.2945 0.3608 0.059 Uiso 1 1 calc R A 2 H13B H 1.1284 0.3725 0.3657 0.059 Uiso 1 1 calc R A 2 H13C H 1.0118 0.3434 0.3914 0.059 Uiso 1 1 calc R A 2 C14 C 0.84841(16) 0.32786(10) 0.64669(16) 0.0184(4) Uani 1 1 d . A 2 C15 C 0.79376(18) 0.38266(10) 0.70004(16) 0.0206(4) Uani 1 1 d . A 2 C16 C 0.8407(2) 0.44585(12) 0.70545(19) 0.0296(5) Uani 1 1 d . A 2 H16 H 0.9052 0.4551 0.6712 0.036 Uiso 1 1 calc R A 2 C17 C 0.7926(2) 0.49477(12) 0.7609(2) 0.0342(6) Uani 1 1 d . A 2 H17 H 0.8246 0.5374 0.7644 0.041 Uiso 1 1 calc R A 2 C18 C 0.6981(2) 0.48182(12) 0.81144(18) 0.0302(5) Uani 1 1 d . A 2 H18 H 0.6657 0.5154 0.8494 0.036 Uiso 1 1 calc R A 2 C19 C 0.65128(19) 0.41927(12) 0.80596(17) 0.0267(5) Uani 1 1 d . A 2 H19 H 0.5865 0.4103 0.8399 0.032 Uiso 1 1 calc R A 2 C20 C 0.69906(18) 0.36984(11) 0.75085(17) 0.0242(4) Uani 1 1 d . A 2 H20 H 0.6670 0.3272 0.7479 0.029 Uiso 1 1 calc R A 2 C21 C 0.93469(18) 0.28067(11) 0.79135(16) 0.0216(4) Uani 1 1 d . A 2 H21 H 0.8942 0.3177 0.8223 0.026 Uiso 1 1 calc R A 2 C22 C 1.0551(2) 0.29369(13) 0.80661(19) 0.0313(5) Uani 1 1 d . A 2 H22A H 1.0971 0.2572 0.7793 0.047 Uiso 1 1 calc R A 2 H22B H 1.0703 0.2971 0.8753 0.047 Uiso 1 1 calc R A 2 H22C H 1.0752 0.3351 0.7749 0.047 Uiso 1 1 calc R A 2 C23 C 0.8989(2) 0.21637(12) 0.83956(18) 0.0292(5) Uani 1 1 d . A 2 H23A H 0.8213 0.2098 0.8289 0.044 Uiso 1 1 calc R A 2 H23B H 0.9134 0.2190 0.9085 0.044 Uiso 1 1 calc R A 2 H23C H 0.9390 0.1792 0.8122 0.044 Uiso 1 1 calc R A 2 C24 C 0.77526(18) 0.34277(11) 0.47956(16) 0.0234(4) Uani 1 1 d . A 2 H24 H 0.7920 0.3193 0.4184 0.028 Uiso 1 1 calc R A 2 C25 C 0.7946(2) 0.41693(12) 0.4614(2) 0.0356(6) Uani 1 1 d . A 2 H25A H 0.7727 0.4423 0.5179 0.053 Uiso 1 1 calc R A 2 H25B H 0.7519 0.4312 0.4059 0.053 Uiso 1 1 calc R A 2 H25C H 0.8715 0.4245 0.4488 0.053 Uiso 1 1 calc R A 2 C26 C 0.65612(19) 0.32904(14) 0.5017(2) 0.0338(6) Uani 1 1 d . A 2 H26A H 0.6453 0.2814 0.5096 0.051 Uiso 1 1 calc R A 2 H26B H 0.6110 0.3451 0.4489 0.051 Uiso 1 1 calc R A 2 H26C H 0.6359 0.3518 0.5610 0.051 Uiso 1 1 calc R A 2 C27 C 0.75143(18) 0.11889(10) 0.49509(17) 0.0239(5) Uani 1 1 d . A 2 C28 C 0.81073(19) 0.13175(11) 0.41242(17) 0.0254(5) Uani 1 1 d . A 2 C29 C 0.7880(2) 0.09611(12) 0.32844(19) 0.0328(6) Uani 1 1 d . A 2 H29 H 0.8281 0.1047 0.2719 0.039 Uiso 1 1 calc R A 2 C30 C 0.7070(2) 0.04817(13) 0.3273(2) 0.0406(7) Uani 1 1 d . A 2 H30 H 0.6922 0.0244 0.2701 0.049 Uiso 1 1 calc R A 2 C31 C 0.6481(2) 0.03517(12) 0.4094(2) 0.0407(7) Uani 1 1 d . A 2 H31 H 0.5929 0.0026 0.4087 0.049 Uiso 1 1 calc R A 2 C32 C 0.6705(2) 0.07022(12) 0.4932(2) 0.0322(6) Uani 1 1 d . A 2 H32 H 0.6305 0.0611 0.5496 0.039 Uiso 1 1 calc R A 2 N1 N 1.04013(14) 0.17859(8) 0.61251(14) 0.0188(3) Uani 1 1 d . A 2 N2 N 1.06859(14) 0.27259(9) 0.54551(14) 0.0201(4) Uani 1 1 d . A 2 N4 N 0.90586(14) 0.28050(8) 0.68929(13) 0.0183(3) Uani 1 1 d . A 2 N3 N 0.84781(14) 0.31499(8) 0.55332(13) 0.0189(3) Uani 1 1 d . A 2 Se2 Se 0.777407(17) 0.165758(10) 0.612529(16) 0.02092(6) Uani 1 1 d . A 2 Se1 Se 0.922820(18) 0.197354(11) 0.407717(16) 0.02415(6) Uani 1 1 d . A 2 Si Si 0.92810(4) 0.23563(3) 0.57022(4) 0.01682(11) Uani 1 1 d . A 2 C57 C 1.4026(6) 0.4220(3) -0.4343(5) 0.0441(4) Uiso 0.50 1 d PD B -1 H57A H 1.3416 0.4427 -0.4012 0.053 Uiso 0.50 1 calc PR B -1 H57B H 1.4456 0.3965 -0.3883 0.053 Uiso 0.50 1 calc PR B -1 H57C H 1.3753 0.3925 -0.4845 0.053 Uiso 0.50 1 calc PR B -1 C51 C 1.5436(4) 0.5087(2) -0.4189(3) 0.0441(4) Uiso 0.50 1 d PGD B -1 H51 H 1.5480 0.4973 -0.3530 0.053 Uiso 0.50 1 calc PR B -1 C52 C 1.6082(3) 0.5589(2) -0.4553(3) 0.0441(4) Uiso 0.50 1 d PGD B -1 H52 H 1.6567 0.5819 -0.4144 0.053 Uiso 0.50 1 calc PR B -1 C53 C 1.6018(4) 0.5755(2) -0.5518(3) 0.0441(4) Uiso 0.50 1 d PGD B -1 H53 H 1.6459 0.6098 -0.5767 0.053 Uiso 0.50 1 calc PR B -1 C54 C 1.5308(4) 0.5418(2) -0.6117(2) 0.0441(4) Uiso 0.50 1 d PGD B -1 H54 H 1.5264 0.5532 -0.6776 0.053 Uiso 0.50 1 calc PR B -1 C55 C 1.4662(3) 0.4916(2) -0.5753(3) 0.0441(4) Uiso 0.50 1 d PGD B -1 H55 H 1.4176 0.4686 -0.6162 0.053 Uiso 0.50 1 calc PR B -1 C56 C 1.4726(4) 0.4750(2) -0.4788(3) 0.0441(4) Uiso 0.50 1 d PGD B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0154(9) 0.0218(9) 0.0195(10) -0.0022(8) -0.0004(8) 0.0004(7) C2 0.0147(9) 0.0223(10) 0.0272(11) 0.0013(8) 0.0003(8) 0.0005(8) C7 0.0206(11) 0.0354(12) 0.0353(13) -0.0100(11) 0.0006(10) -0.0006(9) C6 0.0201(11) 0.0528(16) 0.0402(15) -0.0087(13) -0.0059(11) -0.0075(11) C5 0.0158(10) 0.0448(14) 0.0393(14) 0.0074(12) 0.0016(10) 0.0050(10) C4 0.0228(11) 0.0318(12) 0.0311(12) 0.0031(10) 0.0070(9) 0.0072(9) C3 0.0206(10) 0.0297(11) 0.0236(11) -0.0016(9) 0.0014(8) 0.0007(9) C8 0.0185(10) 0.0190(9) 0.0227(10) 0.0009(8) 0.0001(8) 0.0016(7) C9 0.0302(12) 0.0260(11) 0.0273(12) 0.0019(9) -0.0071(10) 0.0036(9) C10 0.0297(12) 0.0219(10) 0.0311(12) -0.0022(9) -0.0025(10) -0.0003(9) C11 0.0182(10) 0.0257(10) 0.0331(12) 0.0064(9) 0.0054(9) -0.0021(8) C12 0.0337(14) 0.0242(11) 0.0515(17) 0.0004(11) 0.0050(12) -0.0060(10) C13 0.0382(15) 0.0447(15) 0.0360(15) 0.0152(12) 0.0054(12) -0.0064(12) C14 0.0138(9) 0.0182(9) 0.0231(10) -0.0016(8) 0.0001(8) -0.0010(7) C15 0.0219(10) 0.0183(9) 0.0217(10) -0.0009(8) -0.0020(8) 0.0030(8) C16 0.0302(12) 0.0249(11) 0.0337(13) -0.0033(10) 0.0065(10) -0.0037(9) C17 0.0437(15) 0.0208(11) 0.0382(14) -0.0058(10) 0.0049(12) -0.0027(10) C18 0.0359(13) 0.0266(11) 0.0282(12) -0.0064(10) 0.0012(10) 0.0100(10) C19 0.0233(11) 0.0308(11) 0.0261(11) -0.0014(9) 0.0025(9) 0.0046(9) C20 0.0223(10) 0.0231(10) 0.0271(11) -0.0010(9) 0.0006(9) 0.0007(8) C21 0.0214(10) 0.0242(10) 0.0191(10) -0.0024(8) -0.0005(8) 0.0030(8) C22 0.0258(12) 0.0393(13) 0.0288(12) -0.0022(10) -0.0070(10) -0.0052(10) C23 0.0313(12) 0.0338(12) 0.0226(11) 0.0026(9) -0.0005(10) -0.0030(10) C24 0.0231(10) 0.0246(10) 0.0226(11) 0.0002(9) -0.0026(9) 0.0039(8) C25 0.0361(14) 0.0291(12) 0.0416(15) 0.0097(11) -0.0127(12) 0.0041(10) C26 0.0208(11) 0.0467(14) 0.0338(14) 0.0031(11) -0.0074(10) 0.0014(10) C27 0.0219(10) 0.0184(9) 0.0313(12) -0.0037(9) -0.0068(9) 0.0030(8) C28 0.0247(11) 0.0219(10) 0.0295(12) -0.0046(9) -0.0080(9) 0.0068(8) C29 0.0368(14) 0.0300(12) 0.0315(13) -0.0078(10) -0.0116(11) 0.0123(10) C30 0.0487(17) 0.0281(12) 0.0450(16) -0.0145(11) -0.0262(14) 0.0095(11) C31 0.0417(15) 0.0234(11) 0.0569(19) -0.0029(12) -0.0237(14) -0.0047(10) C32 0.0273(12) 0.0244(11) 0.0448(15) 0.0008(10) -0.0115(11) -0.0032(9) N1 0.0153(8) 0.0174(8) 0.0238(9) 0.0005(7) -0.0002(7) 0.0009(6) N2 0.0140(8) 0.0209(8) 0.0253(9) 0.0018(7) 0.0011(7) 0.0002(6) N4 0.0185(8) 0.0181(8) 0.0184(8) -0.0008(7) -0.0011(7) 0.0020(6) N3 0.0169(8) 0.0191(8) 0.0207(9) 0.0001(7) -0.0017(7) 0.0026(6) Se2 0.01613(10) 0.02150(10) 0.02513(11) -0.00111(8) 0.00089(8) -0.00213(8) Se1 0.02316(11) 0.02928(12) 0.02000(11) -0.00324(9) 0.00144(8) 0.00235(9) Si 0.0137(2) 0.0177(2) 0.0191(3) -0.0007(2) -0.0003(2) 0.0012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.334(3) . ? C1 N1 1.335(3) . ? C1 C2 1.497(3) . ? C1 Si 2.370(2) . ? C2 C3 1.394(3) . ? C2 C7 1.394(3) . ? C7 C6 1.398(3) . ? C6 C5 1.388(4) . ? C5 C4 1.386(4) . ? C4 C3 1.397(3) . ? C8 N1 1.475(3) . ? C8 C10 1.529(3) . ? C8 C9 1.532(3) . ? C11 N2 1.473(3) . ? C11 C13 1.528(4) . ? C11 C12 1.530(4) . ? C14 N3 1.330(3) . ? C14 N4 1.332(3) . ? C14 C15 1.498(3) . ? C14 Si 2.366(2) . ? C15 C20 1.396(3) . ? C15 C16 1.406(3) . ? C16 C17 1.391(4) . ? C17 C18 1.392(4) . ? C18 C19 1.394(3) . ? C19 C20 1.394(3) . ? C21 N4 1.469(3) . ? C21 C22 1.527(3) . ? C21 C23 1.531(3) . ? C24 N3 1.476(3) . ? C24 C26 1.532(3) . ? C24 C25 1.540(3) . ? C27 C28 1.394(4) . ? C27 C32 1.405(3) . ? C27 Se2 1.921(2) . ? C28 C29 1.405(3) . ? C28 Se1 1.921(2) . ? C29 C30 1.394(4) . ? C30 C31 1.386(5) . ? C31 C32 1.396(4) . ? N1 Si 1.8965(18) . ? N2 Si 1.9240(19) . ? N4 Si 1.9153(19) . ? N3 Si 1.9022(18) . ? Se2 Si 2.4142(7) . ? Se1 Si 2.3989(8) . ? C57 C56 1.513(6) . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? 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 C1 N1 107.26(18) . . ? N2 C1 C2 125.47(19) . . ? N1 C1 C2 127.25(19) . . ? N2 C1 Si 54.24(11) . . ? N1 C1 Si 53.06(10) . . ? C2 C1 Si 176.97(16) . . ? C3 C2 C7 120.0(2) . . ? C3 C2 C1 119.86(19) . . ? C7 C2 C1 120.2(2) . . ? C2 C7 C6 119.6(2) . . ? C5 C6 C7 120.4(2) . . ? C4 C5 C6 119.9(2) . . ? C5 C4 C3 120.2(2) . . ? C2 C3 C4 119.9(2) . . ? N1 C8 C10 112.06(18) . . ? N1 C8 C9 114.02(18) . . ? C10 C8 C9 111.44(18) . . ? N2 C11 C13 110.8(2) . . ? N2 C11 C12 110.9(2) . . ? C13 C11 C12 111.5(2) . . ? N3 C14 N4 107.38(18) . . ? N3 C14 C15 129.16(19) . . ? N4 C14 C15 123.43(19) . . ? N3 C14 Si 53.43(10) . . ? N4 C14 Si 54.00(11) . . ? C15 C14 Si 175.68(16) . . ? C20 C15 C16 119.2(2) . . ? C20 C15 C14 119.74(19) . . ? C16 C15 C14 120.9(2) . . ? C17 C16 C15 120.0(2) . . ? C16 C17 C18 120.6(2) . . ? C17 C18 C19 119.5(2) . . ? C18 C19 C20 120.3(2) . . ? C19 C20 C15 120.3(2) . . ? N4 C21 C22 111.72(19) . . ? N4 C21 C23 110.82(18) . . ? C22 C21 C23 111.62(19) . . ? N3 C24 C26 111.92(19) . . ? N3 C24 C25 113.05(19) . . ? C26 C24 C25 111.1(2) . . ? C28 C27 C32 119.5(2) . . ? C28 C27 Se2 121.88(16) . . ? C32 C27 Se2 118.7(2) . . ? C27 C28 C29 119.4(2) . . ? C27 C28 Se1 122.59(17) . . ? C29 C28 Se1 118.0(2) . . ? C30 C29 C28 120.6(3) . . ? C31 C30 C29 120.1(2) . . ? C30 C31 C32 119.6(2) . . ? C31 C32 C27 120.8(3) . . ? C1 N1 C8 130.56(18) . . ? C1 N1 Si 92.70(13) . . ? C8 N1 Si 136.48(14) . . ? C1 N2 C11 125.21(18) . . ? C1 N2 Si 91.52(13) . . ? C11 N2 Si 142.99(15) . . ? C14 N4 C21 124.04(18) . . ? C14 N4 Si 91.76(13) . . ? C21 N4 Si 143.99(14) . . ? C14 N3 C24 127.72(18) . . ? C14 N3 Si 92.41(13) . . ? C24 N3 Si 136.43(14) . . ? C27 Se2 Si 101.97(8) . . ? C28 Se1 Si 102.04(8) . . ? N1 Si N3 158.92(8) . . ? N1 Si N4 97.15(8) . . ? N3 Si N4 68.38(8) . . ? N1 Si N2 68.45(8) . . ? N3 Si N2 96.97(8) . . ? N4 Si N2 95.94(9) . . ? N1 Si C14 130.10(8) . . ? N3 Si C14 34.16(8) . . ? N4 Si C14 34.24(7) . . ? N2 Si C14 98.75(8) . . ? N1 Si C1 34.23(8) . . ? N3 Si C1 129.93(8) . . ? N4 Si C1 98.82(8) . . ? N2 Si C1 34.24(7) . . ? C14 Si C1 119.57(7) . . ? N1 Si Se1 96.68(6) . . ? N3 Si Se1 98.17(6) . . ? N4 Si Se1 166.16(6) . . ? N2 Si Se1 88.74(7) . . ? C14 Si Se1 132.16(6) . . ? C1 Si Se1 92.38(6) . . ? N1 Si Se2 97.56(6) . . ? N3 Si Se2 96.96(6) . . ? N4 Si Se2 87.26(6) . . ? N2 Si Se2 165.91(6) . . ? C14 Si Se2 91.62(6) . . ? C1 Si Se2 131.72(6) . . ? Se1 Si Se2 91.35(3) . . ? C52 C51 C56 120.0 . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 C57 122.6(4) . . ? C51 C56 C57 117.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 C3 -105.8(3) . . . . ? N1 C1 C2 C3 72.4(3) . . . . ? Si C1 C2 C3 -22(3) . . . . ? N2 C1 C2 C7 74.7(3) . . . . ? N1 C1 C2 C7 -107.1(3) . . . . ? Si C1 C2 C7 158(3) . . . . ? C3 C2 C7 C6 -0.9(4) . . . . ? C1 C2 C7 C6 178.6(2) . . . . ? C2 C7 C6 C5 0.2(4) . . . . ? C7 C6 C5 C4 0.3(4) . . . . ? C6 C5 C4 C3 0.0(4) . . . . ? C7 C2 C3 C4 1.2(4) . . . . ? C1 C2 C3 C4 -178.3(2) . . . . ? C5 C4 C3 C2 -0.7(4) . . . . ? N3 C14 C15 C20 102.6(3) . . . . ? N4 C14 C15 C20 -75.1(3) . . . . ? Si C14 C15 C20 -23(2) . . . . ? N3 C14 C15 C16 -82.1(3) . . . . ? N4 C14 C15 C16 100.3(3) . . . . ? Si C14 C15 C16 153(2) . . . . ? C20 C15 C16 C17 -0.1(4) . . . . ? C14 C15 C16 C17 -175.4(2) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? C16 C17 C18 C19 -0.2(4) . . . . ? C17 C18 C19 C20 0.4(4) . . . . ? C18 C19 C20 C15 -0.5(4) . . . . ? C16 C15 C20 C19 0.3(3) . . . . ? C14 C15 C20 C19 175.7(2) . . . . ? C32 C27 C28 C29 0.4(3) . . . . ? Se2 C27 C28 C29 -179.78(16) . . . . ? C32 C27 C28 Se1 179.91(16) . . . . ? Se2 C27 C28 Se1 -0.3(3) . . . . ? C27 C28 C29 C30 -0.1(3) . . . . ? Se1 C28 C29 C30 -179.56(18) . . . . ? C28 C29 C30 C31 -0.1(4) . . . . ? C29 C30 C31 C32 -0.1(4) . . . . ? C30 C31 C32 C27 0.5(4) . . . . ? C28 C27 C32 C31 -0.7(3) . . . . ? Se2 C27 C32 C31 179.56(19) . . . . ? N2 C1 N1 C8 177.1(2) . . . . ? C2 C1 N1 C8 -1.3(4) . . . . ? Si C1 N1 C8 174.9(3) . . . . ? N2 C1 N1 Si 2.25(18) . . . . ? C2 C1 N1 Si -176.2(2) . . . . ? C10 C8 N1 C1 -85.9(3) . . . . ? C9 C8 N1 C1 41.9(3) . . . . ? C10 C8 N1 Si 86.7(3) . . . . ? C9 C8 N1 Si -145.58(19) . . . . ? N1 C1 N2 C11 -177.4(2) . . . . ? C2 C1 N2 C11 1.1(3) . . . . ? Si C1 N2 C11 -175.2(2) . . . . ? N1 C1 N2 Si -2.22(17) . . . . ? C2 C1 N2 Si 176.29(19) . . . . ? C13 C11 N2 C1 117.2(2) . . . . ? C12 C11 N2 C1 -118.4(2) . . . . ? C13 C11 N2 Si -54.7(3) . . . . ? C12 C11 N2 Si 69.7(3) . . . . ? N3 C14 N4 C21 173.59(19) . . . . ? C15 C14 N4 C21 -8.3(3) . . . . ? Si C14 N4 C21 175.9(2) . . . . ? N3 C14 N4 Si -2.33(17) . . . . ? C15 C14 N4 Si 175.77(18) . . . . ? C22 C21 N4 C14 -109.0(2) . . . . ? C23 C21 N4 C14 125.9(2) . . . . ? C22 C21 N4 Si 64.1(3) . . . . ? C23 C21 N4 Si -61.1(3) . . . . ? N4 C14 N3 C24 164.01(19) . . . . ? C15 C14 N3 C24 -13.9(4) . . . . ? Si C14 N3 C24 161.7(2) . . . . ? N4 C14 N3 Si 2.35(17) . . . . ? C15 C14 N3 Si -175.6(2) . . . . ? C26 C24 N3 C14 -58.1(3) . . . . ? C25 C24 N3 C14 68.3(3) . . . . ? C26 C24 N3 Si 94.8(3) . . . . ? C25 C24 N3 Si -138.8(2) . . . . ? C28 C27 Se2 Si -2.66(19) . . . . ? C32 C27 Se2 Si 177.12(16) . . . . ? C27 C28 Se1 Si 3.12(19) . . . . ? C29 C28 Se1 Si -177.40(16) . . . . ? C1 N1 Si N3 -50.2(3) . . . . ? C8 N1 Si N3 135.5(2) . . . . ? C1 N1 Si N4 -95.19(14) . . . . ? C8 N1 Si N4 90.5(2) . . . . ? C1 N1 Si N2 -1.60(12) . . . . ? C8 N1 Si N2 -176.0(2) . . . . ? C1 N1 Si C14 -84.79(15) . . . . ? C8 N1 Si C14 100.9(2) . . . . ? C8 N1 Si C1 -174.3(3) . . . . ? C1 N1 Si Se1 84.38(12) . . . . ? C8 N1 Si Se1 -90.0(2) . . . . ? C1 N1 Si Se2 176.64(12) . . . . ? C8 N1 Si Se2 2.3(2) . . . . ? C14 N3 Si N1 -50.7(3) . . . . ? C24 N3 Si N1 150.5(2) . . . . ? C14 N3 Si N4 -1.67(12) . . . . ? C24 N3 Si N4 -160.5(2) . . . . ? C14 N3 Si N2 -95.32(14) . . . . ? C24 N3 Si N2 105.8(2) . . . . ? C24 N3 Si C14 -158.8(3) . . . . ? C14 N3 Si C1 -84.98(15) . . . . ? C24 N3 Si C1 116.2(2) . . . . ? C14 N3 Si Se1 174.95(11) . . . . ? C24 N3 Si Se1 16.1(2) . . . . ? C14 N3 Si Se2 82.57(12) . . . . ? C24 N3 Si Se2 -76.3(2) . . . . ? C14 N4 Si N1 165.79(13) . . . . ? C21 N4 Si N1 -8.5(3) . . . . ? C14 N4 Si N3 1.67(12) . . . . ? C21 N4 Si N3 -172.6(3) . . . . ? C14 N4 Si N2 96.83(13) . . . . ? C21 N4 Si N2 -77.4(3) . . . . ? C21 N4 Si C14 -174.2(3) . . . . ? C14 N4 Si C1 131.25(13) . . . . ? C21 N4 Si C1 -43.0(3) . . . . ? C14 N4 Si Se1 -12.4(3) . . . . ? C21 N4 Si Se1 173.33(19) . . . . ? C14 N4 Si Se2 -96.93(12) . . . . ? C21 N4 Si Se2 88.8(2) . . . . ? C1 N2 Si N1 1.60(13) . . . . ? C11 N2 Si N1 175.1(3) . . . . ? C1 N2 Si N3 165.84(13) . . . . ? C11 N2 Si N3 -20.7(3) . . . . ? C1 N2 Si N4 96.97(14) . . . . ? C11 N2 Si N4 -89.6(3) . . . . ? C1 N2 Si C14 131.39(13) . . . . ? C11 N2 Si C14 -55.2(3) . . . . ? C11 N2 Si C1 173.5(3) . . . . ? C1 N2 Si Se1 -96.09(13) . . . . ? C11 N2 Si Se1 77.4(3) . . . . ? C1 N2 Si Se2 -5.6(3) . . . . ? C11 N2 Si Se2 167.9(2) . . . . ? N3 C14 Si N1 158.66(13) . . . . ? N4 C14 Si N1 -18.57(17) . . . . ? C15 C14 Si N1 -73(2) . . . . ? N4 C14 Si N3 -177.2(2) . . . . ? C15 C14 Si N3 128(2) . . . . ? N3 C14 Si N4 177.2(2) . . . . ? C15 C14 Si N4 -55(2) . . . . ? N3 C14 Si N2 89.53(14) . . . . ? N4 C14 Si N2 -87.70(14) . . . . ? C15 C14 Si N2 -142(2) . . . . ? N3 C14 Si C1 118.56(13) . . . . ? N4 C14 Si C1 -58.67(15) . . . . ? C15 C14 Si C1 -113(2) . . . . ? N3 C14 Si Se1 -6.75(15) . . . . ? N4 C14 Si Se1 176.02(11) . . . . ? C15 C14 Si Se1 121(2) . . . . ? N3 C14 Si Se2 -100.04(12) . . . . ? N4 C14 Si Se2 82.73(12) . . . . ? C15 C14 Si Se2 28(2) . . . . ? N2 C1 Si N1 -177.3(2) . . . . ? C2 C1 Si N1 97(3) . . . . ? N2 C1 Si N3 -18.47(17) . . . . ? N1 C1 Si N3 158.88(14) . . . . ? C2 C1 Si N3 -104(3) . . . . ? N2 C1 Si N4 -87.59(14) . . . . ? N1 C1 Si N4 89.75(14) . . . . ? C2 C1 Si N4 -173(3) . . . . ? N1 C1 Si N2 177.3(2) . . . . ? C2 C1 Si N2 -86(3) . . . . ? N2 C1 Si C14 -58.49(15) . . . . ? N1 C1 Si C14 118.86(14) . . . . ? C2 C1 Si C14 -144(3) . . . . ? N2 C1 Si Se1 84.26(13) . . . . ? N1 C1 Si Se1 -98.40(13) . . . . ? C2 C1 Si Se1 -1(3) . . . . ? N2 C1 Si Se2 178.19(11) . . . . ? N1 C1 Si Se2 -4.46(16) . . . . ? C2 C1 Si Se2 93(3) . . . . ? C28 Se1 Si N1 94.23(9) . . . . ? C28 Se1 Si N3 -100.78(9) . . . . ? C28 Se1 Si N4 -87.6(3) . . . . ? C28 Se1 Si N2 162.36(8) . . . . ? C28 Se1 Si C14 -96.95(10) . . . . ? C28 Se1 Si C1 128.31(8) . . . . ? C28 Se1 Si Se2 -3.54(7) . . . . ? C27 Se2 Si N1 -93.48(9) . . . . ? C27 Se2 Si N3 101.84(9) . . . . ? C27 Se2 Si N4 169.67(8) . . . . ? C27 Se2 Si N2 -86.8(3) . . . . ? C27 Se2 Si C14 135.69(8) . . . . ? C27 Se2 Si C1 -90.95(10) . . . . ? C27 Se2 Si Se1 3.45(7) . . . . ? C56 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C51 0.0 . . . . ? C54 C55 C56 C57 178.5(5) . . . . ? C52 C51 C56 C55 0.0 . . . . ? C52 C51 C56 C57 -178.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.671 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.083