Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Rita Boaretto' 'V. Bertolasi' 'Michele Chierotti' 'Roberto Gobetto' 'Silvana Sostero' _publ_contact_author_name 'Rita Boaretto' _publ_contact_author_address ; Department of Chemistry University of Ferrara Via Borsai 46 Ferrara 44100 ITALY ; _publ_contact_author_email BAR@UNIFE.IT _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, characterization and reactivity of new complexes of Titanium and Zirconium containing a potential tridentate amidinatocyclopentadienyl ligand. ; data_(2a) _database_code_depnum_ccdc_archive 'CCDC 652429' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H34 N4 Si Ti' _chemical_formula_sum 'C20 H34 N4 Si Ti' _chemical_formula_weight 406.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0461(2) _cell_length_b 17.0028(3) _cell_length_c 12.8224(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.286(1) _cell_angle_gamma 90.00 _cell_volume 2177.05(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 18403 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 30.0 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.459 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.908 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_process_details ; SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22995 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.7 _diffrn_reflns_theta_max 30.0 _reflns_number_total 6343 _reflns_number_gt 4706 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997)' _computing_cell_refinement 'Denzo SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III (Burnett & Johnson, 1996)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995) ; _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^)+(0.0396P)^2^+0.7314P] 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 6343 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _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 Ti1 Ti 0.68303(3) 0.197866(16) 0.74754(2) 0.01661(8) Uani 1 1 d . . . Si1 Si 0.92222(4) 0.09435(2) 0.73939(4) 0.01898(11) Uani 1 1 d . . . N1 N 0.88462(13) 0.19318(7) 0.75802(11) 0.0197(3) Uani 1 1 d . . . N2 N 1.10804(13) 0.23062(8) 0.75898(12) 0.0251(3) Uani 1 1 d . . . N3 N 0.64857(14) 0.25936(9) 0.62343(12) 0.0261(3) Uani 1 1 d . . . N4 N 0.63249(14) 0.27052(8) 0.85184(12) 0.0254(3) Uani 1 1 d . . . C1 C 0.74252(15) 0.06528(9) 0.74348(13) 0.0199(3) Uani 1 1 d . . . C2 C 0.63799(16) 0.07667(9) 0.65902(14) 0.0223(3) Uani 1 1 d . . . C3 C 0.51817(16) 0.09530(9) 0.70232(15) 0.0233(4) Uani 1 1 d . . . C4 C 0.54428(15) 0.09200(9) 0.81370(14) 0.0222(3) Uani 1 1 d . . . C5 C 0.68031(16) 0.07291(9) 0.83946(14) 0.0206(3) Uani 1 1 d . . . C6 C 0.6513(2) 0.07100(12) 0.54388(15) 0.0366(5) Uani 1 1 d . . . H61 H 0.7088 0.1122 0.5242 0.044 Uiso 1 1 calc R . . H62 H 0.5645 0.0762 0.5049 0.044 Uiso 1 1 calc R . . H63 H 0.6889 0.0209 0.5289 0.044 Uiso 1 1 calc R . . C7 C 0.38065(17) 0.10450(11) 0.64429(17) 0.0341(4) Uani 1 1 d . . . H71 H 0.3355 0.0547 0.6412 0.041 Uiso 1 1 calc R . . H72 H 0.3882 0.1228 0.5744 0.041 Uiso 1 1 calc R . . H73 H 0.3305 0.1419 0.6803 0.041 Uiso 1 1 calc R . . C8 C 0.43725(17) 0.09865(11) 0.88658(16) 0.0331(4) Uani 1 1 d . . . H81 H 0.3835 0.0518 0.8818 0.040 Uiso 1 1 calc R . . H82 H 0.3817 0.1434 0.8672 0.040 Uiso 1 1 calc R . . H83 H 0.4783 0.1050 0.9573 0.040 Uiso 1 1 calc R . . C9 C 0.74791(18) 0.05835(12) 0.94844(15) 0.0318(4) Uani 1 1 d . . . H91 H 0.6845 0.0657 0.9984 0.038 Uiso 1 1 calc R . . H92 H 0.8208 0.0946 0.9631 0.038 Uiso 1 1 calc R . . H93 H 0.7815 0.0055 0.9532 0.038 Uiso 1 1 calc R . . C10 C 0.98874(18) 0.07282(11) 0.61233(15) 0.0310(4) Uani 1 1 d . . . H101 H 0.9392 0.1024 0.5573 0.037 Uiso 1 1 calc R . . H102 H 0.9797 0.0177 0.5972 0.037 Uiso 1 1 calc R . . H103 H 1.0816 0.0873 0.6170 0.037 Uiso 1 1 calc R . . C11 C 1.04045(17) 0.04797(11) 0.84389(16) 0.0304(4) Uani 1 1 d . . . H111 H 1.1309 0.0590 0.8309 0.036 Uiso 1 1 calc R . . H112 H 1.0264 -0.0079 0.8435 0.036 Uiso 1 1 calc R . . H113 H 1.0249 0.0689 0.9110 0.036 Uiso 1 1 calc R . . C12 C 0.97906(15) 0.25229(9) 0.76250(13) 0.0206(3) Uani 1 1 d . . . C13 C 0.94393(17) 0.33222(10) 0.76857(16) 0.0301(4) Uani 1 1 d . . . H13 H 0.8553 0.3464 0.7730 0.036 Uiso 1 1 calc R . . C14 C 1.04065(19) 0.38915(11) 0.76786(17) 0.0357(5) Uani 1 1 d . . . H14 H 1.0180 0.4421 0.7709 0.043 Uiso 1 1 calc R . . C15 C 1.17232(18) 0.36694(11) 0.76258(16) 0.0340(4) Uani 1 1 d . . . H15 H 1.2397 0.4043 0.7610 0.041 Uiso 1 1 calc R . . C16 C 1.20021(17) 0.28806(11) 0.75977(16) 0.0308(4) Uani 1 1 d . . . H16 H 1.2891 0.2732 0.7583 0.037 Uiso 1 1 calc R . . C17 C 0.73976(19) 0.28052(13) 0.54747(17) 0.0378(5) Uani 1 1 d . . . H171 H 0.7130 0.2544 0.4821 0.045 Uiso 1 1 calc R . . H172 H 0.8291 0.2647 0.5733 0.045 Uiso 1 1 calc R . . H173 H 0.7375 0.3364 0.5368 0.045 Uiso 1 1 calc R . . C18 C 0.5123(2) 0.28291(14) 0.58458(19) 0.0468(6) Uani 1 1 d . . . H181 H 0.5096 0.3387 0.5731 0.056 Uiso 1 1 calc R . . H182 H 0.4527 0.2693 0.6354 0.056 Uiso 1 1 calc R . . H183 H 0.4851 0.2562 0.5198 0.056 Uiso 1 1 calc R . . C19 C 0.6291(2) 0.25444(12) 0.96303(16) 0.0377(5) Uani 1 1 d . . . H191 H 0.6862 0.2910 1.0037 0.045 Uiso 1 1 calc R . . H192 H 0.6599 0.2018 0.9783 0.045 Uiso 1 1 calc R . . H193 H 0.5391 0.2599 0.9805 0.045 Uiso 1 1 calc R . . C20 C 0.5971(2) 0.35309(11) 0.83269(19) 0.0406(5) Uani 1 1 d . . . H201 H 0.5067 0.3619 0.8478 0.049 Uiso 1 1 calc R . . H202 H 0.6043 0.3657 0.7606 0.049 Uiso 1 1 calc R . . H203 H 0.6568 0.3859 0.8771 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.01764(13) 0.01389(14) 0.01851(15) -0.00005(11) 0.00296(10) 0.00078(10) Si1 0.0176(2) 0.0154(2) 0.0241(3) -0.00100(17) 0.00283(17) 0.00044(16) N1 0.0196(6) 0.0149(6) 0.0242(8) -0.0013(5) 0.0009(5) -0.0010(5) N2 0.0214(7) 0.0226(7) 0.0320(9) -0.0029(6) 0.0054(6) -0.0036(6) N3 0.0262(7) 0.0274(8) 0.0252(8) 0.0080(6) 0.0049(6) 0.0030(6) N4 0.0269(7) 0.0206(7) 0.0299(9) -0.0050(6) 0.0079(6) -0.0001(6) C1 0.0198(7) 0.0138(7) 0.0258(9) -0.0014(6) 0.0017(6) -0.0014(6) C2 0.0240(8) 0.0166(8) 0.0255(9) -0.0048(6) -0.0005(7) -0.0006(6) C3 0.0197(7) 0.0162(7) 0.0327(10) -0.0046(7) -0.0023(7) -0.0008(6) C4 0.0190(7) 0.0154(7) 0.0327(10) 0.0010(7) 0.0055(7) -0.0039(6) C5 0.0218(7) 0.0156(7) 0.0247(9) 0.0026(6) 0.0033(6) -0.0012(6) C6 0.0365(10) 0.0443(11) 0.0275(11) -0.0133(9) -0.0026(8) 0.0049(9) C7 0.0226(8) 0.0306(10) 0.0466(13) -0.0105(9) -0.0072(8) 0.0037(7) C8 0.0245(8) 0.0337(10) 0.0432(13) 0.0040(9) 0.0125(8) -0.0010(8) C9 0.0324(9) 0.0382(11) 0.0249(10) 0.0118(8) 0.0037(8) 0.0021(8) C10 0.0315(9) 0.0293(9) 0.0340(11) -0.0063(8) 0.0124(8) -0.0044(7) C11 0.0221(8) 0.0276(9) 0.0405(12) 0.0028(8) -0.0015(7) 0.0026(7) C12 0.0227(7) 0.0195(8) 0.0193(9) -0.0001(6) 0.0011(6) -0.0015(6) C13 0.0255(8) 0.0182(8) 0.0462(12) -0.0018(8) 0.0023(8) 0.0011(7) C14 0.0394(10) 0.0168(8) 0.0500(14) -0.0003(8) 0.0012(9) -0.0043(8) C15 0.0341(9) 0.0257(9) 0.0429(13) -0.0024(8) 0.0080(9) -0.0136(8) C16 0.0242(8) 0.0311(10) 0.0385(12) -0.0039(8) 0.0100(8) -0.0060(7) C17 0.0361(10) 0.0495(12) 0.0287(11) 0.0134(9) 0.0074(8) -0.0001(9) C18 0.0316(10) 0.0606(14) 0.0482(15) 0.0271(11) 0.0042(9) 0.0094(10) C19 0.0449(11) 0.0407(11) 0.0282(11) -0.0122(9) 0.0075(9) -0.0002(9) C20 0.0449(11) 0.0224(9) 0.0572(15) -0.0091(9) 0.0180(10) 0.0040(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N3 1.9039(15) . ? Ti1 N4 1.9291(14) . ? Ti1 N1 2.0164(13) . ? Ti1 C1 2.3343(16) . ? Ti1 C2 2.3721(16) . ? Ti1 C3 2.4310(16) . ? Ti1 C5 2.4312(16) . ? Ti1 C4 2.4823(15) . ? Ti1 Si1 2.9897(5) . ? Si1 N1 1.7446(13) . ? Si1 C10 1.8636(18) . ? Si1 C11 1.8653(18) . ? Si1 C1 1.8780(16) . ? N1 C12 1.379(2) . ? N2 C16 1.345(2) . ? N2 C12 1.353(2) . ? N3 C17 1.454(2) . ? N3 C18 1.460(2) . ? N4 C19 1.456(2) . ? N4 C20 1.462(2) . ? C1 C2 1.437(2) . ? C1 C5 1.446(2) . ? C2 C3 1.416(2) . ? C2 C6 1.500(3) . ? C3 C4 1.425(3) . ? C3 C7 1.504(2) . ? C4 C5 1.408(2) . ? C4 C8 1.504(2) . ? C5 C9 1.506(2) . ? C6 H61 0.9600 . ? C6 H62 0.9600 . ? C6 H63 0.9600 . ? C7 H71 0.9600 . ? C7 H72 0.9600 . ? C7 H73 0.9600 . ? C8 H81 0.9600 . ? C8 H82 0.9600 . ? C8 H83 0.9600 . ? C9 H91 0.9600 . ? C9 H92 0.9600 . ? C9 H93 0.9600 . ? C10 H101 0.9600 . ? C10 H102 0.9600 . ? C10 H103 0.9600 . ? C11 H111 0.9600 . ? C11 H112 0.9600 . ? C11 H113 0.9600 . ? C12 C13 1.408(2) . ? C13 C14 1.372(2) . ? C13 H13 0.9300 . ? C14 C15 1.384(3) . ? C14 H14 0.9300 . ? C15 C16 1.371(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 H171 0.9600 . ? C17 H172 0.9600 . ? C17 H173 0.9600 . ? C18 H181 0.9600 . ? C18 H182 0.9600 . ? C18 H183 0.9600 . ? C19 H191 0.9600 . ? C19 H192 0.9600 . ? C19 H193 0.9600 . ? C20 H201 0.9600 . ? C20 H202 0.9600 . ? C20 H203 0.9600 . ? 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 N3 Ti1 N4 100.96(7) . . ? N3 Ti1 N1 99.60(6) . . ? N4 Ti1 N1 108.53(6) . . ? N3 Ti1 C1 122.37(6) . . ? N4 Ti1 C1 136.17(6) . . ? N1 Ti1 C1 72.88(5) . . ? N3 Ti1 C2 93.98(6) . . ? N4 Ti1 C2 146.84(6) . . ? N1 Ti1 C2 97.77(5) . . ? C1 Ti1 C2 35.54(6) . . ? N3 Ti1 C3 97.92(6) . . ? N4 Ti1 C3 113.61(6) . . ? N1 Ti1 C3 129.83(5) . . ? C1 Ti1 C3 58.08(5) . . ? C2 Ti1 C3 34.25(5) . . ? N3 Ti1 C5 150.98(6) . . ? N4 Ti1 C5 101.87(6) . . ? N1 Ti1 C5 89.87(5) . . ? C1 Ti1 C5 35.25(6) . . ? C2 Ti1 C5 57.39(6) . . ? C3 Ti1 C5 56.31(6) . . ? N3 Ti1 C4 128.78(6) . . ? N4 Ti1 C4 91.56(6) . . ? N1 Ti1 C4 123.10(5) . . ? C1 Ti1 C4 57.45(5) . . ? C2 Ti1 C4 56.55(6) . . ? C3 Ti1 C4 33.69(6) . . ? C5 Ti1 C4 33.29(5) . . ? N3 Ti1 Si1 111.56(4) . . ? N4 Ti1 Si1 132.44(5) . . ? N1 Ti1 Si1 34.30(4) . . ? C1 Ti1 Si1 38.91(4) . . ? C2 Ti1 Si1 65.40(4) . . ? C3 Ti1 Si1 95.66(4) . . ? C5 Ti1 Si1 63.53(4) . . ? C4 Ti1 Si1 93.93(4) . . ? N1 Si1 C10 114.37(8) . . ? N1 Si1 C11 116.06(8) . . ? C10 Si1 C11 106.49(9) . . ? N1 Si1 C1 91.51(6) . . ? C10 Si1 C1 114.24(8) . . ? C11 Si1 C1 114.02(8) . . ? N1 Si1 Ti1 40.64(4) . . ? C10 Si1 Ti1 120.84(7) . . ? C11 Si1 Ti1 132.43(6) . . ? C1 Si1 Ti1 51.33(5) . . ? C12 N1 Si1 123.33(11) . . ? C12 N1 Ti1 130.95(10) . . ? Si1 N1 Ti1 105.07(6) . . ? C16 N2 C12 117.59(15) . . ? C17 N3 C18 109.85(15) . . ? C17 N3 Ti1 128.73(12) . . ? C18 N3 Ti1 120.90(12) . . ? C19 N4 C20 108.27(15) . . ? C19 N4 Ti1 126.49(12) . . ? C20 N4 Ti1 125.17(13) . . ? C2 C1 C5 106.33(14) . . ? C2 C1 Si1 124.68(13) . . ? C5 C1 Si1 120.44(12) . . ? C2 C1 Ti1 73.67(9) . . ? C5 C1 Ti1 76.04(9) . . ? Si1 C1 Ti1 89.75(6) . . ? C3 C2 C1 108.50(15) . . ? C3 C2 C6 124.85(16) . . ? C1 C2 C6 126.65(15) . . ? C3 C2 Ti1 75.15(9) . . ? C1 C2 Ti1 70.80(9) . . ? C6 C2 Ti1 119.60(12) . . ? C2 C3 C4 108.25(14) . . ? C2 C3 C7 127.14(17) . . ? C4 C3 C7 123.95(16) . . ? C2 C3 Ti1 70.59(9) . . ? C4 C3 Ti1 75.13(9) . . ? C7 C3 Ti1 127.48(12) . . ? C5 C4 C3 108.16(14) . . ? C5 C4 C8 127.80(17) . . ? C3 C4 C8 123.66(15) . . ? C5 C4 Ti1 71.36(9) . . ? C3 C4 Ti1 71.18(9) . . ? C8 C4 Ti1 128.62(12) . . ? C4 C5 C1 108.65(15) . . ? C4 C5 C9 125.67(15) . . ? C1 C5 C9 125.60(14) . . ? C4 C5 Ti1 75.35(9) . . ? C1 C5 Ti1 68.71(9) . . ? C9 C5 Ti1 124.45(12) . . ? C2 C6 H61 109.5 . . ? C2 C6 H62 109.5 . . ? H61 C6 H62 109.5 . . ? C2 C6 H63 109.5 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 109.5 . . ? C3 C7 H71 109.5 . . ? C3 C7 H72 109.5 . . ? H71 C7 H72 109.5 . . ? C3 C7 H73 109.5 . . ? H71 C7 H73 109.5 . . ? H72 C7 H73 109.5 . . ? C4 C8 H81 109.5 . . ? C4 C8 H82 109.5 . . ? H81 C8 H82 109.5 . . ? C4 C8 H83 109.5 . . ? H81 C8 H83 109.5 . . ? H82 C8 H83 109.5 . . ? C5 C9 H91 109.5 . . ? C5 C9 H92 109.5 . . ? H91 C9 H92 109.5 . . ? C5 C9 H93 109.5 . . ? H91 C9 H93 109.5 . . ? H92 C9 H93 109.5 . . ? Si1 C10 H101 109.5 . . ? Si1 C10 H102 109.5 . . ? H101 C10 H102 109.5 . . ? Si1 C10 H103 109.5 . . ? H101 C10 H103 109.5 . . ? H102 C10 H103 109.5 . . ? Si1 C11 H111 109.5 . . ? Si1 C11 H112 109.5 . . ? H111 C11 H112 109.5 . . ? Si1 C11 H113 109.5 . . ? H111 C11 H113 109.5 . . ? H112 C11 H113 109.5 . . ? N2 C12 N1 117.21(14) . . ? N2 C12 C13 120.76(15) . . ? N1 C12 C13 122.02(14) . . ? C14 C13 C12 119.89(16) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 119.28(17) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 117.84(16) . . ? C16 C15 H15 121.1 . . ? C14 C15 H15 121.1 . . ? N2 C16 C15 124.60(16) . . ? N2 C16 H16 117.7 . . ? C15 C16 H16 117.7 . . ? N3 C17 H171 109.5 . . ? N3 C17 H172 109.5 . . ? H171 C17 H172 109.5 . . ? N3 C17 H173 109.5 . . ? H171 C17 H173 109.5 . . ? H172 C17 H173 109.5 . . ? N3 C18 H181 109.5 . . ? N3 C18 H182 109.5 . . ? H181 C18 H182 109.5 . . ? N3 C18 H183 109.5 . . ? H181 C18 H183 109.5 . . ? H182 C18 H183 109.5 . . ? N4 C19 H191 109.5 . . ? N4 C19 H192 109.5 . . ? H191 C19 H192 109.5 . . ? N4 C19 H193 109.5 . . ? H191 C19 H193 109.5 . . ? H192 C19 H193 109.5 . . ? N4 C20 H201 109.5 . . ? N4 C20 H202 109.5 . . ? H201 C20 H202 109.5 . . ? N4 C20 H203 109.5 . . ? H201 C20 H203 109.5 . . ? H202 C20 H203 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.389 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.059 #===END data_(2b) _database_code_depnum_ccdc_archive 'CCDC 652430' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H33 N5 Si1 Ti1' _chemical_formula_sum 'C19 H33 N5 Si1 Ti1' _chemical_formula_weight 407.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6755(2) _cell_length_b 12.9384(3) _cell_length_c 38.3224(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.049(2) _cell_angle_gamma 90.00 _cell_volume 4295.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150 _cell_measurement_reflns_used 53434 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.0 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.467 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_process_details ; SORTAV (R. H: Blessing, Acta Crystallogr., 1995, A51, 33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41164 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.4 _diffrn_reflns_theta_max 27.0 _reflns_number_total 9361 _reflns_number_gt 6581 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997)' _computing_cell_refinement 'Denzo SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III (Burnett & Johnson, 1996)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995) ; _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^)+(0.0553P)^2^+1.8625P] 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 9361 _refine_ls_number_parameters 484 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _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 Ti1A Ti 0.17453(5) 0.23631(3) 0.696018(11) 0.02178(12) Uani 1 1 d . . . Si1A Si -0.08198(8) 0.21201(5) 0.745157(17) 0.02279(16) Uani 1 1 d . . . N1A N 0.1188(2) 0.22041(16) 0.74669(5) 0.0232(5) Uani 1 1 d . . . N2A N 0.1363(3) 0.22080(18) 0.80725(5) 0.0309(5) Uani 1 1 d . . . N3A N 0.3636(3) 0.23187(18) 0.77454(6) 0.0330(5) Uani 1 1 d . . . N4A N 0.3511(3) 0.1519(2) 0.68829(6) 0.0425(7) Uani 1 1 d . . . N5A N 0.2578(3) 0.37269(19) 0.69740(6) 0.0415(6) Uani 1 1 d . . . C1A C -0.0906(3) 0.20473(19) 0.69614(6) 0.0230(5) Uani 1 1 d . . . C2A C -0.0312(3) 0.1161(2) 0.67859(6) 0.0254(6) Uani 1 1 d . . . C3A C 0.0279(3) 0.1483(2) 0.64677(6) 0.0258(6) Uani 1 1 d . . . C4A C 0.0068(3) 0.2568(2) 0.64380(7) 0.0267(6) Uani 1 1 d . . . C5A C -0.0704(3) 0.2912(2) 0.67315(7) 0.0274(6) Uani 1 1 d . . . C6A C -0.0386(4) 0.0058(2) 0.69111(7) 0.0390(7) Uani 1 1 d . . . H61 H -0.0090 -0.0398 0.6729 0.047 Uiso 1 1 calc R . . H62 H -0.1421 -0.0099 0.6971 0.047 Uiso 1 1 calc R . . H63 H 0.0304 -0.0030 0.7113 0.047 Uiso 1 1 calc R . . C7A C 0.0856(4) 0.0812(2) 0.61845(7) 0.0414(8) Uani 1 1 d . . . H71 H 0.1017 0.0123 0.6272 0.050 Uiso 1 1 calc R . . H72 H 0.1812 0.1084 0.6109 0.050 Uiso 1 1 calc R . . H73 H 0.0108 0.0798 0.5991 0.050 Uiso 1 1 calc R . . C8A C 0.0439(3) 0.3220(2) 0.61272(7) 0.0338(7) Uani 1 1 d . . . H81 H 0.1264 0.2904 0.6008 0.041 Uiso 1 1 calc R . . H82 H 0.0749 0.3898 0.6205 0.041 Uiso 1 1 calc R . . H83 H -0.0458 0.3272 0.5971 0.041 Uiso 1 1 calc R . . C9A C -0.1271(4) 0.4001(2) 0.67784(8) 0.0472(8) Uani 1 1 d . . . H91 H -0.0642 0.4469 0.6653 0.057 Uiso 1 1 calc R . . H92 H -0.1208 0.4175 0.7022 0.057 Uiso 1 1 calc R . . H93 H -0.2323 0.4053 0.6689 0.057 Uiso 1 1 calc R . . C10A C -0.1620(3) 0.0963(2) 0.76695(7) 0.0300(6) Uani 1 1 d . . . H101 H -0.1163 0.0349 0.7580 0.036 Uiso 1 1 calc R . . H102 H -0.2718 0.0939 0.7624 0.036 Uiso 1 1 calc R . . H103 H -0.1391 0.1006 0.7917 0.036 Uiso 1 1 calc R . . C11A C -0.1768(3) 0.3277(2) 0.76366(7) 0.0346(7) Uani 1 1 d . . . H111 H -0.1712 0.3234 0.7887 0.041 Uiso 1 1 calc R . . H112 H -0.2830 0.3301 0.7553 0.041 Uiso 1 1 calc R . . H113 H -0.1249 0.3891 0.7565 0.041 Uiso 1 1 calc R . . C12A C 0.2088(3) 0.22434(19) 0.77688(6) 0.0245(5) Uiso 1 1 d . . . C13A C 0.2263(3) 0.2223(2) 0.83647(7) 0.0380(7) Uani 1 1 d . . . H13A H 0.1794 0.2193 0.8577 0.046 Uiso 1 1 calc R . . C14A C 0.3845(3) 0.2281(2) 0.83698(7) 0.0411(7) Uani 1 1 d . . . H14A H 0.4452 0.2286 0.8577 0.049 Uiso 1 1 calc R . . C15A C 0.4474(3) 0.2332(2) 0.80481(7) 0.0388(7) Uani 1 1 d . . . H15A H 0.5542 0.2377 0.8041 0.047 Uiso 1 1 calc R . . C16A C 0.3604(4) 0.0424(3) 0.68000(9) 0.0661(12) Uani 1 1 d . . . H161 H 0.4108 0.0339 0.6585 0.079 Uiso 1 1 calc R . . H162 H 0.2582 0.0139 0.6776 0.079 Uiso 1 1 calc R . . H163 H 0.4183 0.0073 0.6985 0.079 Uiso 1 1 calc R . . C17A C 0.5072(4) 0.1925(4) 0.69616(9) 0.0790(14) Uani 1 1 d . . . H171 H 0.5543 0.1559 0.7157 0.095 Uiso 1 1 calc R . . H172 H 0.5013 0.2647 0.7017 0.095 Uiso 1 1 calc R . . H173 H 0.5681 0.1834 0.6762 0.095 Uiso 1 1 calc R . . C18A C 0.2305(5) 0.4520(2) 0.72311(9) 0.0585(10) Uani 1 1 d . . . H181 H 0.3270 0.4828 0.7309 0.070 Uiso 1 1 calc R . . H182 H 0.1828 0.4216 0.7427 0.070 Uiso 1 1 calc R . . H183 H 0.1637 0.5041 0.7128 0.070 Uiso 1 1 calc R . . C19A C 0.3395(5) 0.4182(3) 0.66858(9) 0.0827(15) Uani 1 1 d . . . H191 H 0.2775 0.4720 0.6578 0.099 Uiso 1 1 calc R . . H192 H 0.3584 0.3658 0.6516 0.099 Uiso 1 1 calc R . . H193 H 0.4360 0.4466 0.6775 0.099 Uiso 1 1 calc R . . Ti1B Ti -0.06509(5) 0.23693(3) 0.949781(11) 0.02088(12) Uani 1 1 d . . . Si1B Si -0.32973(8) 0.25104(5) 0.997204(17) 0.02129(16) Uani 1 1 d . . . N1B N -0.1286(2) 0.25717(15) 1.00063(5) 0.0223(4) Uani 1 1 d . . . N2B N -0.1241(2) 0.27083(17) 1.06131(5) 0.0272(5) Uani 1 1 d . . . N3B N 0.1112(3) 0.27323(18) 1.03102(6) 0.0326(5) Uani 1 1 d . . . N4B N 0.0200(3) 0.10272(18) 0.94502(6) 0.0374(6) Uani 1 1 d . . . N5B N 0.1118(2) 0.32253(19) 0.94508(5) 0.0332(6) Uani 1 1 d . . . C1B C -0.3326(3) 0.2572(2) 0.94823(6) 0.0245(5) Uani 1 1 d . . . C2B C -0.3109(3) 0.1732(2) 0.92473(6) 0.0284(6) Uani 1 1 d . . . C3B C -0.2288(3) 0.2103(2) 0.89618(7) 0.0293(6) Uani 1 1 d . . . C4B C -0.2040(3) 0.3180(2) 0.90079(6) 0.0278(6) Uani 1 1 d . . . C5B C -0.2687(3) 0.3475(2) 0.93220(6) 0.0253(6) Uani 1 1 d . . . C6B C -0.3723(4) 0.0648(2) 0.92863(8) 0.0497(9) Uani 1 1 d . . . H64 H -0.3676 0.0288 0.9068 0.060 Uiso 1 1 calc R . . H65 H -0.4774 0.0678 0.9352 0.060 Uiso 1 1 calc R . . H66 H -0.3108 0.0290 0.9463 0.060 Uiso 1 1 calc R . . C7B C -0.1939(3) 0.1531(2) 0.86313(7) 0.0399(7) Uani 1 1 d . . . H74 H -0.2323 0.1921 0.8432 0.048 Uiso 1 1 calc R . . H75 H -0.2430 0.0866 0.8630 0.048 Uiso 1 1 calc R . . H76 H -0.0844 0.1443 0.8622 0.048 Uiso 1 1 calc R . . C8B C -0.1310(4) 0.3880(2) 0.87516(7) 0.0409(7) Uani 1 1 d . . . H84 H -0.2076 0.4100 0.8577 0.049 Uiso 1 1 calc R . . H85 H -0.0504 0.3514 0.8641 0.049 Uiso 1 1 calc R . . H86 H -0.0882 0.4473 0.8872 0.049 Uiso 1 1 calc R . . C9B C -0.2766(4) 0.4565(2) 0.94589(8) 0.0405(7) Uani 1 1 d . . . H94 H -0.2206 0.5017 0.9313 0.049 Uiso 1 1 calc R . . H95 H -0.2318 0.4590 0.9693 0.049 Uiso 1 1 calc R . . H96 H -0.3825 0.4782 0.9458 0.049 Uiso 1 1 calc R . . C10B C -0.4127(3) 0.1300(2) 1.01451(7) 0.0316(6) Uani 1 1 d . . . H104 H -0.3698 0.0715 1.0030 0.038 Uiso 1 1 calc R . . H105 H -0.5227 0.1305 1.0102 0.038 Uiso 1 1 calc R . . H106 H -0.3883 0.1255 1.0392 0.038 Uiso 1 1 calc R . . C11B C -0.4353(3) 0.3591(2) 1.01732(7) 0.0281(6) Uani 1 1 d . . . H114 H -0.4291 0.3516 1.0423 0.034 Uiso 1 1 calc R . . H115 H -0.5415 0.3579 1.0089 0.034 Uiso 1 1 calc R . . H116 H -0.3897 0.4237 1.0111 0.034 Uiso 1 1 calc R . . C12B C -0.0448(3) 0.26680(19) 1.03175(6) 0.0237(5) Uani 1 1 d . . . C13B C -0.0391(3) 0.2796(2) 1.09113(7) 0.0321(6) Uani 1 1 d . . . H13B H -0.0902 0.2831 1.1118 0.038 Uiso 1 1 calc R . . C14B C 0.1190(3) 0.2839(2) 1.09326(7) 0.0382(7) Uani 1 1 d . . . H14B H 0.1755 0.2887 1.1145 0.046 Uiso 1 1 calc R . . C15B C 0.1884(3) 0.2807(2) 1.06190(7) 0.0378(7) Uani 1 1 d . . . H15B H 0.2956 0.2840 1.0622 0.045 Uiso 1 1 calc R . . C16B C 0.0032(4) 0.0078(2) 0.92501(9) 0.0583(10) Uani 1 1 d . . . H164 H 0.0989 -0.0080 0.9147 0.070 Uiso 1 1 calc R . . H165 H -0.0766 0.0162 0.9069 0.070 Uiso 1 1 calc R . . H166 H -0.0237 -0.0477 0.9402 0.070 Uiso 1 1 calc R . . C17B C 0.1431(4) 0.0896(3) 0.97251(8) 0.0565(10) Uani 1 1 d . . . H174 H 0.1165 0.0342 0.9877 0.068 Uiso 1 1 calc R . . H175 H 0.1550 0.1524 0.9857 0.068 Uiso 1 1 calc R . . H176 H 0.2383 0.0735 0.9620 0.068 Uiso 1 1 calc R . . C18B C 0.1160(4) 0.4305(3) 0.95564(9) 0.0548(9) Uani 1 1 d . . . H184 H 0.2058 0.4427 0.9708 0.066 Uiso 1 1 calc R . . H185 H 0.0250 0.4466 0.9677 0.066 Uiso 1 1 calc R . . H186 H 0.1201 0.4736 0.9353 0.066 Uiso 1 1 calc R . . C19B C 0.2565(4) 0.2946(3) 0.93029(8) 0.0573(10) Uani 1 1 d . . . H194 H 0.2724 0.3373 0.9103 0.069 Uiso 1 1 calc R . . H195 H 0.2530 0.2234 0.9233 0.069 Uiso 1 1 calc R . . H196 H 0.3398 0.3048 0.9475 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1A 0.0186(2) 0.0276(3) 0.0193(2) -0.00202(18) 0.00258(17) -0.00180(19) Si1A 0.0224(4) 0.0248(4) 0.0217(4) -0.0002(3) 0.0050(3) 0.0006(3) N1A 0.0238(11) 0.0252(12) 0.0206(11) 0.0001(8) 0.0018(8) 0.0008(9) N2A 0.0277(13) 0.0442(14) 0.0210(12) 0.0009(10) 0.0020(9) 0.0008(10) N3A 0.0257(13) 0.0456(15) 0.0277(13) 0.0037(10) 0.0009(10) -0.0026(10) N4A 0.0269(14) 0.074(2) 0.0268(13) -0.0011(12) 0.0039(10) 0.0193(13) N5A 0.0530(17) 0.0431(15) 0.0283(13) 0.0008(11) 0.0012(11) -0.0245(13) C1A 0.0181(13) 0.0261(13) 0.0246(13) 0.0012(10) 0.0006(10) -0.0014(10) C2A 0.0264(14) 0.0276(14) 0.0218(13) -0.0022(10) -0.0014(10) -0.0068(11) C3A 0.0264(14) 0.0307(15) 0.0202(13) -0.0018(10) 0.0006(10) -0.0040(11) C4A 0.0205(14) 0.0346(15) 0.0246(14) 0.0062(11) -0.0017(10) -0.0010(11) C5A 0.0253(14) 0.0288(14) 0.0283(14) 0.0039(11) 0.0028(11) 0.0050(11) C6A 0.061(2) 0.0300(16) 0.0264(15) -0.0013(11) 0.0079(14) -0.0074(14) C7A 0.064(2) 0.0351(17) 0.0255(15) -0.0057(12) 0.0104(14) -0.0102(15) C8A 0.0322(16) 0.0403(17) 0.0292(15) 0.0091(12) 0.0036(12) 0.0008(13) C9A 0.050(2) 0.0406(19) 0.053(2) 0.0154(15) 0.0187(16) 0.0221(15) C10A 0.0298(15) 0.0357(16) 0.0249(14) -0.0011(11) 0.0043(11) -0.0056(12) C11A 0.0349(17) 0.0354(16) 0.0340(16) -0.0022(12) 0.0079(12) 0.0064(13) C13A 0.0332(17) 0.058(2) 0.0226(15) 0.0013(13) 0.0024(12) -0.0018(14) C14A 0.0364(18) 0.060(2) 0.0260(15) 0.0018(13) -0.0052(12) -0.0015(15) C15A 0.0240(15) 0.056(2) 0.0358(17) 0.0043(14) -0.0033(12) -0.0022(13) C16A 0.066(3) 0.073(3) 0.062(2) 0.0169(19) 0.0258(19) 0.044(2) C17A 0.0255(18) 0.165(5) 0.046(2) -0.018(2) -0.0043(15) 0.022(2) C18A 0.087(3) 0.040(2) 0.048(2) -0.0068(15) -0.0027(18) -0.0259(19) C19A 0.126(4) 0.085(3) 0.039(2) -0.0072(19) 0.018(2) -0.072(3) Ti1B 0.0191(2) 0.0232(2) 0.0205(2) -0.00026(17) 0.00320(17) 0.00116(18) Si1B 0.0200(4) 0.0237(4) 0.0204(3) -0.0006(3) 0.0037(3) 0.0008(3) N1B 0.0205(11) 0.0266(12) 0.0199(11) 0.0012(8) 0.0016(8) -0.0016(9) N2B 0.0267(12) 0.0358(13) 0.0192(11) -0.0002(9) 0.0012(9) -0.0022(10) N3B 0.0238(12) 0.0471(15) 0.0265(12) 0.0057(10) -0.0012(9) -0.0043(10) N4B 0.0459(16) 0.0338(14) 0.0330(13) -0.0003(10) 0.0068(11) 0.0157(11) N5B 0.0226(12) 0.0519(16) 0.0251(12) 0.0007(10) 0.0011(9) -0.0075(11) C1B 0.0175(13) 0.0329(15) 0.0232(13) 0.0003(10) 0.0013(10) 0.0015(10) C2B 0.0232(14) 0.0351(16) 0.0270(14) -0.0067(11) 0.0034(11) -0.0061(11) C3B 0.0217(14) 0.0438(17) 0.0226(14) -0.0061(11) 0.0026(10) -0.0027(12) C4B 0.0250(14) 0.0364(16) 0.0217(14) 0.0060(11) -0.0001(10) 0.0026(12) C5B 0.0253(14) 0.0290(14) 0.0215(13) 0.0039(10) -0.0001(10) 0.0058(11) C6B 0.050(2) 0.053(2) 0.048(2) -0.0236(16) 0.0221(16) -0.0278(16) C7B 0.0355(17) 0.058(2) 0.0271(15) -0.0130(13) 0.0088(12) -0.0101(14) C8B 0.048(2) 0.0477(19) 0.0278(16) 0.0081(13) 0.0116(13) 0.0036(15) C9B 0.055(2) 0.0316(16) 0.0358(17) 0.0079(12) 0.0151(14) 0.0116(14) C10B 0.0295(16) 0.0310(15) 0.0346(16) -0.0006(12) 0.0056(12) -0.0038(12) C11B 0.0264(15) 0.0321(15) 0.0265(14) -0.0009(11) 0.0069(11) 0.0050(11) C12B 0.0246(14) 0.0221(13) 0.0246(13) 0.0020(10) 0.0022(10) -0.0015(10) C13B 0.0354(16) 0.0392(17) 0.0216(14) 0.0025(11) 0.0019(11) -0.0025(13) C14B 0.0380(17) 0.0513(19) 0.0242(15) 0.0034(12) -0.0078(12) -0.0071(14) C15B 0.0249(15) 0.055(2) 0.0333(16) 0.0073(13) -0.0026(12) -0.0078(13) C16B 0.085(3) 0.0356(19) 0.056(2) -0.0040(15) 0.0215(19) 0.0205(18) C17B 0.063(2) 0.065(2) 0.042(2) 0.0077(16) 0.0055(16) 0.0375(19) C18B 0.050(2) 0.053(2) 0.061(2) -0.0060(17) 0.0024(17) -0.0292(17) C19B 0.0306(18) 0.099(3) 0.0434(19) -0.0121(19) 0.0108(14) -0.0177(18) _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 Ti1A N5A 1.906(2) . ? Ti1A N4A 1.917(2) . ? Ti1A N1A 2.036(2) . ? Ti1A C1A 2.337(2) . ? Ti1A C5A 2.365(3) . ? Ti1A C4A 2.425(3) . ? Ti1A C2A 2.434(3) . ? Ti1A C3A 2.494(2) . ? Ti1A Si1A 3.0072(8) . ? Si1A N1A 1.743(2) . ? Si1A C11A 1.866(3) . ? Si1A C10A 1.866(3) . ? Si1A C1A 1.878(2) . ? N1A C12A 1.362(3) . ? N2A C13A 1.331(3) . ? N2A C12A 1.353(3) . ? N3A C15A 1.336(3) . ? N3A C12A 1.354(3) . ? N4A C16A 1.455(4) . ? N4A C17A 1.469(4) . ? N5A C18A 1.451(4) . ? N5A C19A 1.467(4) . ? C1A C2A 1.438(3) . ? C1A C5A 1.441(3) . ? C2A C3A 1.410(3) . ? C2A C6A 1.508(4) . ? C3A C4A 1.420(4) . ? C3A C7A 1.497(3) . ? C4A C5A 1.411(4) . ? C4A C8A 1.508(3) . ? C5A C9A 1.506(4) . ? C6A H61 0.9600 . ? C6A H62 0.9600 . ? C6A H63 0.9600 . ? C7A H71 0.9600 . ? C7A H72 0.9600 . ? C7A H73 0.9600 . ? C8A H81 0.9600 . ? C8A H82 0.9600 . ? C8A H83 0.9600 . ? C9A H91 0.9600 . ? C9A H92 0.9600 . ? C9A H93 0.9600 . ? C10A H101 0.9600 . ? C10A H102 0.9600 . ? C10A H103 0.9600 . ? C11A H111 0.9600 . ? C11A H112 0.9600 . ? C11A H113 0.9600 . ? C13A C14A 1.374(4) . ? C13A H13A 0.9300 . ? C14A C15A 1.376(4) . ? C14A H14A 0.9300 . ? C15A H15A 0.9300 . ? C16A H161 0.9600 . ? C16A H162 0.9600 . ? C16A H163 0.9600 . ? C17A H171 0.9600 . ? C17A H172 0.9600 . ? C17A H173 0.9600 . ? C18A H181 0.9600 . ? C18A H182 0.9600 . ? C18A H183 0.9600 . ? C19A H191 0.9600 . ? C19A H192 0.9600 . ? C19A H193 0.9600 . ? Ti1B N4B 1.899(2) . ? Ti1B N5B 1.909(2) . ? Ti1B N1B 2.070(2) . ? Ti1B C1B 2.333(2) . ? Ti1B C5B 2.344(2) . ? Ti1B C4B 2.416(2) . ? Ti1B C2B 2.435(3) . ? Ti1B C3B 2.459(3) . ? Ti1B Si1B 3.0085(8) . ? Si1B N1B 1.745(2) . ? Si1B C10B 1.860(3) . ? Si1B C11B 1.861(3) . ? Si1B C1B 1.877(2) . ? N1B C12B 1.369(3) . ? N2B C13B 1.332(3) . ? N2B C12B 1.358(3) . ? N3B C15B 1.332(3) . ? N3B C12B 1.357(3) . ? N4B C16B 1.451(4) . ? N4B C17B 1.470(4) . ? N5B C19B 1.450(4) . ? N5B C18B 1.455(4) . ? C1B C2B 1.430(3) . ? C1B C5B 1.445(3) . ? C2B C3B 1.420(3) . ? C2B C6B 1.511(4) . ? C3B C4B 1.420(4) . ? C3B C7B 1.511(3) . ? C4B C5B 1.408(3) . ? C4B C8B 1.501(4) . ? C5B C9B 1.507(4) . ? C6B H64 0.9600 . ? C6B H65 0.9600 . ? C6B H66 0.9600 . ? C7B H74 0.9600 . ? C7B H75 0.9600 . ? C7B H76 0.9600 . ? C8B H84 0.9600 . ? C8B H85 0.9600 . ? C8B H86 0.9600 . ? C9B H94 0.9600 . ? C9B H95 0.9600 . ? C9B H96 0.9600 . ? C10B H104 0.9600 . ? C10B H105 0.9600 . ? C10B H106 0.9600 . ? C11B H114 0.9600 . ? C11B H115 0.9600 . ? C11B H116 0.9600 . ? C13B C14B 1.371(4) . ? C13B H13B 0.9300 . ? C14B C15B 1.373(4) . ? C14B H14B 0.9300 . ? C15B H15B 0.9300 . ? C16B H164 0.9600 . ? C16B H165 0.9600 . ? C16B H166 0.9600 . ? C17B H174 0.9600 . ? C17B H175 0.9600 . ? C17B H176 0.9600 . ? C18B H184 0.9600 . ? C18B H185 0.9600 . ? C18B H186 0.9600 . ? C19B H194 0.9600 . ? C19B H195 0.9600 . ? C19B H196 0.9600 . ? 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 N5A Ti1A N4A 103.11(12) . . ? N5A Ti1A N1A 100.13(9) . . ? N4A Ti1A N1A 108.78(9) . . ? N5A Ti1A C1A 122.23(10) . . ? N4A Ti1A C1A 134.08(11) . . ? N1A Ti1A C1A 72.34(8) . . ? N5A Ti1A C5A 93.66(11) . . ? N4A Ti1A C5A 145.47(10) . . ? N1A Ti1A C5A 97.44(8) . . ? C1A Ti1A C5A 35.69(9) . . ? N5A Ti1A C4A 97.54(10) . . ? N4A Ti1A C4A 112.60(9) . . ? N1A Ti1A C4A 129.44(9) . . ? C1A Ti1A C4A 58.21(8) . . ? C5A Ti1A C4A 34.24(9) . . ? N5A Ti1A C2A 150.48(10) . . ? N4A Ti1A C2A 100.04(11) . . ? N1A Ti1A C2A 89.39(8) . . ? C1A Ti1A C2A 35.02(8) . . ? C5A Ti1A C2A 57.23(9) . . ? C4A Ti1A C2A 56.25(9) . . ? N5A Ti1A C3A 128.38(9) . . ? N4A Ti1A C3A 90.16(10) . . ? N1A Ti1A C3A 122.54(8) . . ? C1A Ti1A C3A 57.26(8) . . ? C5A Ti1A C3A 56.26(9) . . ? C4A Ti1A C3A 33.52(8) . . ? C2A Ti1A C3A 33.23(8) . . ? N5A Ti1A Si1A 111.80(8) . . ? N4A Ti1A Si1A 131.40(8) . . ? N1A Ti1A Si1A 34.01(6) . . ? C1A Ti1A Si1A 38.65(6) . . ? C5A Ti1A Si1A 65.36(6) . . ? C4A Ti1A Si1A 95.54(6) . . ? C2A Ti1A Si1A 63.17(6) . . ? C3A Ti1A Si1A 93.52(6) . . ? N1A Si1A C11A 113.38(12) . . ? N1A Si1A C10A 115.46(11) . . ? C11A Si1A C10A 106.95(12) . . ? N1A Si1A C1A 91.35(10) . . ? C11A Si1A C1A 115.17(12) . . ? C10A Si1A C1A 114.29(12) . . ? N1A Si1A Ti1A 40.81(7) . . ? C11A Si1A Ti1A 120.65(9) . . ? C10A Si1A Ti1A 132.03(9) . . ? C1A Si1A Ti1A 50.99(8) . . ? C12A N1A Si1A 123.88(17) . . ? C12A N1A Ti1A 130.69(17) . . ? Si1A N1A Ti1A 105.18(10) . . ? C13A N2A C12A 116.4(2) . . ? C15A N3A C12A 116.1(2) . . ? C16A N4A C17A 109.3(3) . . ? C16A N4A Ti1A 130.0(2) . . ? C17A N4A Ti1A 120.0(2) . . ? C18A N5A C19A 109.3(3) . . ? C18A N5A Ti1A 126.8(2) . . ? C19A N5A Ti1A 123.2(2) . . ? C2A C1A C5A 105.9(2) . . ? C2A C1A Si1A 120.76(18) . . ? C5A C1A Si1A 124.95(19) . . ? C2A C1A Ti1A 76.17(14) . . ? C5A C1A Ti1A 73.21(14) . . ? Si1A C1A Ti1A 90.36(10) . . ? C3A C2A C1A 109.0(2) . . ? C3A C2A C6A 125.3(2) . . ? C1A C2A C6A 125.6(2) . . ? C3A C2A Ti1A 75.75(15) . . ? C1A C2A Ti1A 68.81(14) . . ? C6A C2A Ti1A 124.09(19) . . ? C2A C3A C4A 108.0(2) . . ? C2A C3A C7A 127.4(2) . . ? C4A C3A C7A 124.2(2) . . ? C2A C3A Ti1A 71.02(14) . . ? C4A C3A Ti1A 70.58(14) . . ? C7A C3A Ti1A 129.55(19) . . ? C5A C4A C3A 108.2(2) . . ? C5A C4A C8A 125.7(2) . . ? C3A C4A C8A 125.7(2) . . ? C5A C4A Ti1A 70.52(14) . . ? C3A C4A Ti1A 75.90(14) . . ? C8A C4A Ti1A 124.66(18) . . ? C4A C5A C1A 108.7(2) . . ? C4A C5A C9A 124.2(2) . . ? C1A C5A C9A 127.1(2) . . ? C4A C5A Ti1A 75.24(15) . . ? C1A C5A Ti1A 71.10(14) . . ? C9A C5A Ti1A 122.0(2) . . ? C2A C6A H61 109.5 . . ? C2A C6A H62 109.5 . . ? H61 C6A H62 109.5 . . ? C2A C6A H63 109.5 . . ? H61 C6A H63 109.5 . . ? H62 C6A H63 109.5 . . ? C3A C7A H71 109.5 . . ? C3A C7A H72 109.5 . . ? H71 C7A H72 109.5 . . ? C3A C7A H73 109.5 . . ? H71 C7A H73 109.5 . . ? H72 C7A H73 109.5 . . ? C4A C8A H81 109.5 . . ? C4A C8A H82 109.5 . . ? H81 C8A H82 109.5 . . ? C4A C8A H83 109.5 . . ? H81 C8A H83 109.5 . . ? H82 C8A H83 109.5 . . ? C5A C9A H91 109.5 . . ? C5A C9A H92 109.5 . . ? H91 C9A H92 109.5 . . ? C5A C9A H93 109.5 . . ? H91 C9A H93 109.5 . . ? H92 C9A H93 109.5 . . ? Si1A C10A H101 109.5 . . ? Si1A C10A H102 109.5 . . ? H101 C10A H102 109.5 . . ? Si1A C10A H103 109.5 . . ? H101 C10A H103 109.5 . . ? H102 C10A H103 109.5 . . ? Si1A C11A H111 109.5 . . ? Si1A C11A H112 109.5 . . ? H111 C11A H112 109.5 . . ? Si1A C11A H113 109.5 . . ? H111 C11A H113 109.5 . . ? H112 C11A H113 109.5 . . ? N2A C12A N3A 124.6(2) . . ? N2A C12A N1A 117.3(2) . . ? N3A C12A N1A 118.2(2) . . ? N2A C13A C14A 123.6(3) . . ? N2A C13A H13A 118.2 . . ? C14A C13A H13A 118.2 . . ? C13A C14A C15A 115.7(3) . . ? C13A C14A H14A 122.2 . . ? C15A C14A H14A 122.2 . . ? N3A C15A C14A 123.6(3) . . ? N3A C15A H15A 118.2 . . ? C14A C15A H15A 118.2 . . ? N4A C16A H161 109.5 . . ? N4A C16A H162 109.5 . . ? H161 C16A H162 109.5 . . ? N4A C16A H163 109.5 . . ? H161 C16A H163 109.5 . . ? H162 C16A H163 109.5 . . ? N4A C17A H171 109.5 . . ? N4A C17A H172 109.5 . . ? H171 C17A H172 109.5 . . ? N4A C17A H173 109.5 . . ? H171 C17A H173 109.5 . . ? H172 C17A H173 109.5 . . ? N5A C18A H181 109.5 . . ? N5A C18A H182 109.5 . . ? H181 C18A H182 109.5 . . ? N5A C18A H183 109.5 . . ? H181 C18A H183 109.5 . . ? H182 C18A H183 109.5 . . ? N5A C19A H191 109.5 . . ? N5A C19A H192 109.5 . . ? H191 C19A H192 109.5 . . ? N5A C19A H193 109.5 . . ? H191 C19A H193 109.5 . . ? H192 C19A H193 109.5 . . ? N4B Ti1B N5B 101.70(11) . . ? N4B Ti1B N1B 109.29(9) . . ? N5B Ti1B N1B 105.72(9) . . ? N4B Ti1B C1B 119.43(10) . . ? N5B Ti1B C1B 137.40(10) . . ? N1B Ti1B C1B 72.28(8) . . ? N4B Ti1B C5B 145.21(10) . . ? N5B Ti1B C5B 102.47(10) . . ? N1B Ti1B C5B 87.66(8) . . ? C1B Ti1B C5B 35.99(9) . . ? N4B Ti1B C4B 120.18(10) . . ? N5B Ti1B C4B 92.59(9) . . ? N1B Ti1B C4B 122.00(8) . . ? C1B Ti1B C4B 58.46(8) . . ? C5B Ti1B C4B 34.36(8) . . ? N4B Ti1B C2B 89.39(10) . . ? N5B Ti1B C2B 148.29(9) . . ? N1B Ti1B C2B 98.21(8) . . ? C1B Ti1B C2B 34.82(8) . . ? C5B Ti1B C2B 57.50(10) . . ? C4B Ti1B C2B 56.66(9) . . ? N4B Ti1B C3B 90.10(10) . . ? N5B Ti1B C3B 115.72(9) . . ? N1B Ti1B C3B 129.32(9) . . ? C1B Ti1B C3B 57.65(8) . . ? C5B Ti1B C3B 56.81(9) . . ? C4B Ti1B C3B 33.85(9) . . ? C2B Ti1B C3B 33.74(8) . . ? N4B Ti1B Si1B 115.24(7) . . ? N5B Ti1B Si1B 131.68(7) . . ? N1B Ti1B Si1B 34.28(6) . . ? C1B Ti1B Si1B 38.61(6) . . ? C5B Ti1B Si1B 63.19(6) . . ? C4B Ti1B Si1B 94.46(6) . . ? C2B Ti1B Si1B 65.06(6) . . ? C3B Ti1B Si1B 95.04(6) . . ? N1B Si1B C10B 114.56(11) . . ? N1B Si1B C11B 116.54(11) . . ? C10B Si1B C11B 106.07(12) . . ? N1B Si1B C1B 91.92(10) . . ? C10B Si1B C1B 114.03(12) . . ? C11B Si1B C1B 113.68(12) . . ? N1B Si1B Ti1B 41.92(7) . . ? C10B Si1B Ti1B 119.10(9) . . ? C11B Si1B Ti1B 134.74(9) . . ? C1B Si1B Ti1B 50.86(8) . . ? C12B N1B Si1B 123.54(17) . . ? C12B N1B Ti1B 132.53(17) . . ? Si1B N1B Ti1B 103.80(10) . . ? C13B N2B C12B 115.9(2) . . ? C15B N3B C12B 116.2(2) . . ? C16B N4B C17B 109.2(2) . . ? C16B N4B Ti1B 142.8(2) . . ? C17B N4B Ti1B 107.97(19) . . ? C19B N5B C18B 109.8(3) . . ? C19B N5B Ti1B 127.5(2) . . ? C18B N5B Ti1B 122.64(19) . . ? C2B C1B C5B 106.3(2) . . ? C2B C1B Si1B 127.0(2) . . ? C5B C1B Si1B 118.30(18) . . ? C2B C1B Ti1B 76.49(15) . . ? C5B C1B Ti1B 72.42(14) . . ? Si1B C1B Ti1B 90.53(10) . . ? C3B C2B C1B 108.5(2) . . ? C3B C2B C6B 125.7(2) . . ? C1B C2B C6B 125.7(2) . . ? C3B C2B Ti1B 74.03(15) . . ? C1B C2B Ti1B 68.70(14) . . ? C6B C2B Ti1B 125.5(2) . . ? C4B C3B C2B 108.3(2) . . ? C4B C3B C7B 123.3(2) . . ? C2B C3B C7B 127.7(3) . . ? C4B C3B Ti1B 71.44(14) . . ? C2B C3B Ti1B 72.23(14) . . ? C7B C3B Ti1B 129.53(19) . . ? C5B C4B C3B 108.0(2) . . ? C5B C4B C8B 126.7(3) . . ? C3B C4B C8B 125.2(2) . . ? C5B C4B Ti1B 70.03(14) . . ? C3B C4B Ti1B 74.71(15) . . ? C8B C4B Ti1B 124.04(19) . . ? C4B C5B C1B 108.9(2) . . ? C4B C5B C9B 125.4(2) . . ? C1B C5B C9B 125.7(2) . . ? C4B C5B Ti1B 75.61(15) . . ? C1B C5B Ti1B 71.60(14) . . ? C9B C5B Ti1B 121.25(19) . . ? C2B C6B H64 109.5 . . ? C2B C6B H65 109.5 . . ? H64 C6B H65 109.5 . . ? C2B C6B H66 109.5 . . ? H64 C6B H66 109.5 . . ? H65 C6B H66 109.5 . . ? C3B C7B H74 109.5 . . ? C3B C7B H75 109.5 . . ? H74 C7B H75 109.5 . . ? C3B C7B H76 109.5 . . ? H74 C7B H76 109.5 . . ? H75 C7B H76 109.5 . . ? C4B C8B H84 109.5 . . ? C4B C8B H85 109.5 . . ? H84 C8B H85 109.5 . . ? C4B C8B H86 109.5 . . ? H84 C8B H86 109.5 . . ? H85 C8B H86 109.5 . . ? C5B C9B H94 109.5 . . ? C5B C9B H95 109.5 . . ? H94 C9B H95 109.5 . . ? C5B C9B H96 109.5 . . ? H94 C9B H96 109.5 . . ? H95 C9B H96 109.5 . . ? Si1B C10B H104 109.5 . . ? Si1B C10B H105 109.5 . . ? H104 C10B H105 109.5 . . ? Si1B C10B H106 109.5 . . ? H104 C10B H106 109.5 . . ? H105 C10B H106 109.5 . . ? Si1B C11B H114 109.5 . . ? Si1B C11B H115 109.5 . . ? H114 C11B H115 109.5 . . ? Si1B C11B H116 109.5 . . ? H114 C11B H116 109.5 . . ? H115 C11B H116 109.5 . . ? N3B C12B N2B 124.4(2) . . ? N3B C12B N1B 118.2(2) . . ? N2B C12B N1B 117.4(2) . . ? N2B C13B C14B 124.2(2) . . ? N2B C13B H13B 117.9 . . ? C14B C13B H13B 117.9 . . ? C13B C14B C15B 115.5(3) . . ? C13B C14B H14B 122.2 . . ? C15B C14B H14B 122.2 . . ? N3B C15B C14B 123.8(3) . . ? N3B C15B H15B 118.1 . . ? C14B C15B H15B 118.1 . . ? N4B C16B H164 109.5 . . ? N4B C16B H165 109.5 . . ? H164 C16B H165 109.5 . . ? N4B C16B H166 109.5 . . ? H164 C16B H166 109.5 . . ? H165 C16B H166 109.5 . . ? N4B C17B H174 109.5 . . ? N4B C17B H175 109.5 . . ? H174 C17B H175 109.5 . . ? N4B C17B H176 109.5 . . ? H174 C17B H176 109.5 . . ? H175 C17B H176 109.5 . . ? N5B C18B H184 109.5 . . ? N5B C18B H185 109.5 . . ? H184 C18B H185 109.5 . . ? N5B C18B H186 109.5 . . ? H184 C18B H186 109.5 . . ? H185 C18B H186 109.5 . . ? N5B C19B H194 109.5 . . ? N5B C19B H195 109.5 . . ? H194 C19B H195 109.5 . . ? N5B C19B H196 109.5 . . ? H194 C19B H196 109.5 . . ? H195 C19B H196 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.07 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.455 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.072 #===END data_(2c) _database_code_depnum_ccdc_archive 'CCDC 652431' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H33 N5 Si Ti' _chemical_formula_sum 'C19 H33 N5 Si Ti' _chemical_formula_weight 407.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6330(2) _cell_length_b 12.8584(2) _cell_length_c 19.4243(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.036(1) _cell_angle_gamma 90.00 _cell_volume 2123.23(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 21119 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 30.0 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.472 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details ; SORTAV (R. H. Blessing, Acta Crystallogr., 1995, A51,33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22056 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.0 _reflns_number_total 6186 _reflns_number_gt 4300 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997)' _computing_cell_refinement 'Denzo SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III (Burnett & Johnson, 1996)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995) ; _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^)+(0.0548P)^2^+0.4340P] 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 6186 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1153 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _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 Ti1 Ti 0.26849(3) 0.24321(2) 0.141274(15) 0.01679(9) Uani 1 1 d . . . Si1 Si 0.57348(5) 0.26469(3) 0.24025(2) 0.01800(11) Uani 1 1 d . . . N1 N 0.37215(16) 0.25773(9) 0.24304(7) 0.0180(3) Uani 1 1 d . . . N2 N 0.41755(18) 0.24466(11) 0.36480(8) 0.0260(3) Uani 1 1 d . . . N3 N 0.09255(19) 0.24711(12) 0.36440(9) 0.0309(4) Uani 1 1 d . . . N4 N 0.07619(17) 0.32274(14) 0.12646(8) 0.0345(4) Uani 1 1 d . . . N5 N 0.1924(2) 0.10441(12) 0.14379(8) 0.0354(4) Uani 1 1 d . . . C1 C 0.53276(19) 0.27615(12) 0.14263(9) 0.0189(3) Uani 1 1 d . . . C2 C 0.4542(2) 0.36705(13) 0.10961(9) 0.0220(4) Uani 1 1 d . . . C3 C 0.3635(2) 0.33771(13) 0.04528(9) 0.0234(4) Uani 1 1 d . . . C4 C 0.3843(2) 0.22904(14) 0.03623(9) 0.0233(4) Uani 1 1 d . . . C5 C 0.49147(19) 0.19224(14) 0.09393(9) 0.0233(4) Uani 1 1 d . . . C6 C 0.4720(3) 0.47659(13) 0.13771(11) 0.0361(5) Uani 1 1 d . . . H61 H 0.4174 0.5238 0.1035 0.043 Uiso 1 1 calc R . . H62 H 0.5816 0.4947 0.1476 0.043 Uiso 1 1 calc R . . H63 H 0.4285 0.4810 0.1798 0.043 Uiso 1 1 calc R . . C7 C 0.2741(3) 0.40662(16) -0.00999(11) 0.0399(5) Uani 1 1 d . . . H71 H 0.2658 0.4751 0.0088 0.048 Uiso 1 1 calc R . . H72 H 0.1707 0.3786 -0.0251 0.048 Uiso 1 1 calc R . . H73 H 0.3285 0.4103 -0.0490 0.048 Uiso 1 1 calc R . . C8 C 0.3171(2) 0.16989(17) -0.02872(10) 0.0342(5) Uani 1 1 d . . . H81 H 0.3793 0.1829 -0.0642 0.041 Uiso 1 1 calc R . . H82 H 0.2109 0.1921 -0.0450 0.041 Uiso 1 1 calc R . . H83 H 0.3182 0.0968 -0.0185 0.041 Uiso 1 1 calc R . . C9 C 0.5549(3) 0.08279(16) 0.10090(12) 0.0425(5) Uani 1 1 d . . . H91 H 0.4759 0.0354 0.0786 0.051 Uiso 1 1 calc R . . H92 H 0.5830 0.0652 0.1495 0.051 Uiso 1 1 calc R . . H93 H 0.6462 0.0780 0.0791 0.051 Uiso 1 1 calc R . . C10 C 0.6782(2) 0.37881(14) 0.28569(10) 0.0295(4) Uani 1 1 d . . . H101 H 0.6288 0.4418 0.2664 0.035 Uiso 1 1 calc R . . H102 H 0.7861 0.3781 0.2794 0.035 Uiso 1 1 calc R . . H103 H 0.6737 0.3754 0.3347 0.035 Uiso 1 1 calc R . . C11 C 0.6860(2) 0.14677(15) 0.27503(10) 0.0317(4) Uani 1 1 d . . . H111 H 0.7097 0.1504 0.3251 0.038 Uiso 1 1 calc R . . H112 H 0.7822 0.1433 0.2567 0.038 Uiso 1 1 calc R . . H113 H 0.6242 0.0858 0.2612 0.038 Uiso 1 1 calc R . . C12 C 0.3146(2) 0.25098(11) 0.30425(9) 0.0184(3) Uani 1 1 d . . . C13 C 0.3563(2) 0.24000(15) 0.42347(10) 0.0309(4) Uani 1 1 d . . . H13 H 0.4249 0.2354 0.4660 0.037 Uiso 1 1 calc R . . C14 C 0.1970(2) 0.24165(15) 0.42418(11) 0.0313(4) Uani 1 1 d . . . H14 H 0.1614 0.2389 0.4667 0.038 Uiso 1 1 calc R . . C15 C 0.1510(2) 0.25082(13) 0.30595(10) 0.0252(4) Uani 1 1 d . . . H15 H 0.0813 0.2535 0.2637 0.030 Uiso 1 1 calc R . . C16 C 0.0599(3) 0.4348(2) 0.11479(14) 0.0603(8) Uani 1 1 d . . . H161 H -0.0019 0.4475 0.0695 0.072 Uiso 1 1 calc R . . H162 H 0.1621 0.4654 0.1171 0.072 Uiso 1 1 calc R . . H163 H 0.0087 0.4651 0.1500 0.072 Uiso 1 1 calc R . . C17 C -0.0790(2) 0.2787(2) 0.12945(13) 0.0599(8) Uani 1 1 d . . . H171 H -0.1210 0.3106 0.1669 0.072 Uiso 1 1 calc R . . H172 H -0.0694 0.2051 0.1374 0.072 Uiso 1 1 calc R . . H173 H -0.1483 0.2914 0.0860 0.072 Uiso 1 1 calc R . . C18 C 0.2460(3) 0.02449(16) 0.19555(12) 0.0512(6) Uani 1 1 d . . . H181 H 0.1569 -0.0129 0.2063 0.061 Uiso 1 1 calc R . . H182 H 0.3017 0.0564 0.2373 0.061 Uiso 1 1 calc R . . H183 H 0.3146 -0.0228 0.1772 0.061 Uiso 1 1 calc R . . C19 C 0.0962(4) 0.0577(2) 0.08216(13) 0.0658(8) Uani 1 1 d . . . H191 H 0.1570 0.0066 0.0626 0.079 Uiso 1 1 calc R . . H192 H 0.0625 0.1108 0.0481 0.079 Uiso 1 1 calc R . . H193 H 0.0058 0.0250 0.0954 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.01390(15) 0.02179(15) 0.01471(16) -0.00046(10) 0.00261(11) -0.00113(10) Si1 0.0150(2) 0.0219(2) 0.0165(2) 0.00157(16) 0.00083(17) 0.00045(16) N1 0.0165(6) 0.0209(6) 0.0166(7) -0.0004(5) 0.0033(5) 0.0004(5) N2 0.0219(7) 0.0391(9) 0.0170(8) 0.0009(6) 0.0031(6) -0.0013(6) N3 0.0258(8) 0.0450(9) 0.0237(9) -0.0019(7) 0.0096(7) 0.0000(7) N4 0.0183(7) 0.0605(11) 0.0240(9) -0.0022(7) 0.0016(7) 0.0114(7) N5 0.0469(10) 0.0331(8) 0.0270(9) -0.0049(7) 0.0087(8) -0.0202(7) C1 0.0131(7) 0.0262(8) 0.0176(9) 0.0002(6) 0.0038(6) -0.0006(6) C2 0.0232(8) 0.0240(8) 0.0181(9) 0.0039(6) 0.0019(7) -0.0055(6) C3 0.0208(8) 0.0314(9) 0.0182(9) 0.0055(7) 0.0042(7) -0.0039(7) C4 0.0185(8) 0.0368(9) 0.0161(9) -0.0049(7) 0.0070(7) -0.0028(7) C5 0.0173(8) 0.0303(9) 0.0234(9) -0.0062(7) 0.0061(7) 0.0028(7) C6 0.0508(13) 0.0229(9) 0.0298(11) 0.0057(7) -0.0062(10) -0.0079(8) C7 0.0439(12) 0.0441(11) 0.0267(11) 0.0127(9) -0.0077(9) -0.0074(9) C8 0.0255(10) 0.0538(12) 0.0238(10) -0.0135(8) 0.0056(8) -0.0020(8) C9 0.0378(12) 0.0390(11) 0.0472(14) -0.0171(9) -0.0021(10) 0.0158(9) C10 0.0302(10) 0.0352(10) 0.0209(10) 0.0006(7) -0.0012(8) -0.0103(8) C11 0.0289(10) 0.0364(10) 0.0291(11) 0.0060(8) 0.0031(8) 0.0119(8) C12 0.0208(8) 0.0187(7) 0.0162(8) -0.0010(6) 0.0048(6) -0.0006(6) C13 0.0271(10) 0.0498(12) 0.0154(9) 0.0004(8) 0.0022(8) -0.0007(8) C14 0.0315(10) 0.0451(11) 0.0196(9) -0.0020(8) 0.0109(8) -0.0017(8) C15 0.0204(8) 0.0361(9) 0.0194(9) -0.0017(7) 0.0038(7) 0.0000(7) C16 0.0496(15) 0.0646(16) 0.0617(18) -0.0088(13) -0.0042(13) 0.0374(12) C17 0.0184(10) 0.134(2) 0.0282(13) -0.0010(14) 0.0050(9) 0.0069(12) C18 0.0819(18) 0.0286(11) 0.0459(15) 0.0010(9) 0.0190(13) -0.0196(11) C19 0.093(2) 0.0650(16) 0.0365(14) -0.0067(12) 0.0041(14) -0.0524(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 Ti1 N5 1.9053(15) . ? Ti1 N4 1.9283(15) . ? Ti1 N1 2.0314(14) . ? Ti1 C1 2.3160(16) . ? Ti1 C5 2.3660(16) . ? Ti1 C2 2.4143(16) . ? Ti1 C4 2.4304(17) . ? Ti1 C3 2.4816(17) . ? Ti1 Si1 2.9901(5) . ? Si1 N1 1.7506(14) . ? Si1 C10 1.8632(18) . ? Si1 C11 1.8631(18) . ? Si1 C1 1.8731(17) . ? N1 C12 1.369(2) . ? N2 C13 1.339(2) . ? N2 C12 1.347(2) . ? N3 C15 1.321(2) . ? N3 C14 1.342(3) . ? N4 C16 1.462(3) . ? N4 C17 1.465(3) . ? N5 C18 1.455(3) . ? N5 C19 1.462(3) . ? C1 C5 1.438(2) . ? C1 C2 1.444(2) . ? C2 C3 1.406(2) . ? C2 C6 1.509(2) . ? C3 C4 1.424(2) . ? C3 C7 1.498(2) . ? C4 C5 1.405(2) . ? C4 C8 1.501(2) . ? C5 C9 1.508(2) . ? C6 H61 0.9600 . ? C6 H62 0.9600 . ? C6 H63 0.9600 . ? C7 H71 0.9600 . ? C7 H72 0.9600 . ? C7 H73 0.9600 . ? C8 H81 0.9600 . ? C8 H82 0.9600 . ? C8 H83 0.9600 . ? C9 H91 0.9600 . ? C9 H92 0.9600 . ? C9 H93 0.9600 . ? C10 H101 0.9600 . ? C10 H102 0.9600 . ? C10 H103 0.9600 . ? C11 H111 0.9600 . ? C11 H112 0.9600 . ? C11 H113 0.9600 . ? C12 C15 1.418(2) . ? C13 C14 1.378(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H161 0.9600 . ? C16 H162 0.9600 . ? C16 H163 0.9600 . ? C17 H171 0.9600 . ? C17 H172 0.9600 . ? C17 H173 0.9600 . ? C18 H181 0.9600 . ? C18 H182 0.9600 . ? C18 H183 0.9600 . ? C19 H191 0.9600 . ? C19 H192 0.9600 . ? C19 H193 0.9600 . ? 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 N5 Ti1 N4 102.07(8) . . ? N5 Ti1 N1 99.00(6) . . ? N4 Ti1 N1 108.56(6) . . ? N5 Ti1 C1 120.94(7) . . ? N4 Ti1 C1 136.51(7) . . ? N1 Ti1 C1 72.91(6) . . ? N5 Ti1 C5 93.32(7) . . ? N4 Ti1 C5 145.75(7) . . ? N1 Ti1 C5 98.82(6) . . ? C1 Ti1 C5 35.76(6) . . ? N5 Ti1 C2 150.63(7) . . ? N4 Ti1 C2 101.83(7) . . ? N1 Ti1 C2 89.30(6) . . ? C1 Ti1 C2 35.47(6) . . ? C5 Ti1 C2 57.46(6) . . ? N5 Ti1 C4 98.36(7) . . ? N4 Ti1 C4 112.58(7) . . ? N1 Ti1 C4 130.39(6) . . ? C1 Ti1 C4 58.32(6) . . ? C5 Ti1 C4 34.04(6) . . ? C2 Ti1 C4 56.42(6) . . ? N5 Ti1 C3 129.67(7) . . ? N4 Ti1 C3 90.97(7) . . ? N1 Ti1 C3 122.61(6) . . ? C1 Ti1 C3 57.67(6) . . ? C5 Ti1 C3 56.35(6) . . ? C2 Ti1 C3 33.34(5) . . ? C4 Ti1 C3 33.67(6) . . ? N5 Ti1 Si1 109.80(6) . . ? N4 Ti1 Si1 133.29(5) . . ? N1 Ti1 Si1 34.58(4) . . ? C1 Ti1 Si1 38.79(4) . . ? C5 Ti1 Si1 65.83(4) . . ? C2 Ti1 Si1 63.47(4) . . ? C4 Ti1 Si1 95.84(4) . . ? C3 Ti1 Si1 93.93(4) . . ? N1 Si1 C10 115.35(8) . . ? N1 Si1 C11 113.89(8) . . ? C10 Si1 C11 106.84(9) . . ? N1 Si1 C1 91.33(7) . . ? C10 Si1 C1 114.06(8) . . ? C11 Si1 C1 115.16(8) . . ? N1 Si1 Ti1 41.19(5) . . ? C10 Si1 Ti1 132.66(6) . . ? C11 Si1 Ti1 120.21(7) . . ? C1 Si1 Ti1 50.76(5) . . ? C12 N1 Si1 122.87(11) . . ? C12 N1 Ti1 132.41(11) . . ? Si1 N1 Ti1 104.24(7) . . ? C13 N2 C12 116.60(15) . . ? C15 N3 C14 116.44(16) . . ? C16 N4 C17 108.87(19) . . ? C16 N4 Ti1 127.09(15) . . ? C17 N4 Ti1 123.95(16) . . ? C18 N5 C19 110.02(17) . . ? C18 N5 Ti1 127.58(13) . . ? C19 N5 Ti1 120.86(14) . . ? C5 C1 C2 105.76(14) . . ? C5 C1 Si1 126.03(13) . . ? C2 C1 Si1 120.26(12) . . ? C5 C1 Ti1 74.02(9) . . ? C2 C1 Ti1 75.98(9) . . ? Si1 C1 Ti1 90.45(7) . . ? C3 C2 C1 108.87(15) . . ? C3 C2 C6 125.30(16) . . ? C1 C2 C6 125.78(15) . . ? C3 C2 Ti1 75.96(10) . . ? C1 C2 Ti1 68.55(9) . . ? C6 C2 Ti1 123.64(13) . . ? C2 C3 C4 108.08(15) . . ? C2 C3 C7 128.02(17) . . ? C4 C3 C7 123.53(17) . . ? C2 C3 Ti1 70.70(10) . . ? C4 C3 Ti1 71.19(9) . . ? C7 C3 Ti1 129.17(13) . . ? C5 C4 C3 108.16(15) . . ? C5 C4 C8 127.17(17) . . ? C3 C4 C8 124.25(17) . . ? C5 C4 Ti1 70.47(10) . . ? C3 C4 Ti1 75.14(10) . . ? C8 C4 Ti1 126.05(12) . . ? C4 C5 C1 108.98(15) . . ? C4 C5 C9 124.35(16) . . ? C1 C5 C9 126.64(16) . . ? C4 C5 Ti1 75.49(10) . . ? C1 C5 Ti1 70.23(9) . . ? C9 C5 Ti1 122.08(14) . . ? C2 C6 H61 109.5 . . ? C2 C6 H62 109.5 . . ? H61 C6 H62 109.5 . . ? C2 C6 H63 109.5 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 109.5 . . ? C3 C7 H71 109.5 . . ? C3 C7 H72 109.5 . . ? H71 C7 H72 109.5 . . ? C3 C7 H73 109.5 . . ? H71 C7 H73 109.5 . . ? H72 C7 H73 109.5 . . ? C4 C8 H81 109.5 . . ? C4 C8 H82 109.5 . . ? H81 C8 H82 109.5 . . ? C4 C8 H83 109.5 . . ? H81 C8 H83 109.5 . . ? H82 C8 H83 109.5 . . ? C5 C9 H91 109.5 . . ? C5 C9 H92 109.5 . . ? H91 C9 H92 109.5 . . ? C5 C9 H93 109.5 . . ? H91 C9 H93 109.5 . . ? H92 C9 H93 109.5 . . ? Si1 C10 H101 109.5 . . ? Si1 C10 H102 109.5 . . ? H101 C10 H102 109.5 . . ? Si1 C10 H103 109.5 . . ? H101 C10 H103 109.5 . . ? H102 C10 H103 109.5 . . ? Si1 C11 H111 109.5 . . ? Si1 C11 H112 109.5 . . ? H111 C11 H112 109.5 . . ? Si1 C11 H113 109.5 . . ? H111 C11 H113 109.5 . . ? H112 C11 H113 109.5 . . ? N2 C12 N1 118.55(15) . . ? N2 C12 C15 119.18(16) . . ? N1 C12 C15 122.27(15) . . ? N2 C13 C14 123.41(18) . . ? N2 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? N3 C14 C13 120.91(18) . . ? N3 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? N3 C15 C12 123.45(17) . . ? N3 C15 H15 118.3 . . ? C12 C15 H15 118.3 . . ? N4 C16 H161 109.5 . . ? N4 C16 H162 109.5 . . ? H161 C16 H162 109.5 . . ? N4 C16 H163 109.5 . . ? H161 C16 H163 109.5 . . ? H162 C16 H163 109.5 . . ? N4 C17 H171 109.5 . . ? N4 C17 H172 109.5 . . ? H171 C17 H172 109.5 . . ? N4 C17 H173 109.5 . . ? H171 C17 H173 109.5 . . ? H172 C17 H173 109.5 . . ? N5 C18 H181 109.5 . . ? N5 C18 H182 109.5 . . ? H181 C18 H182 109.5 . . ? N5 C18 H183 109.5 . . ? H181 C18 H183 109.5 . . ? H182 C18 H183 109.5 . . ? N5 C19 H191 109.5 . . ? N5 C19 H192 109.5 . . ? H191 C19 H192 109.5 . . ? N5 C19 H193 109.5 . . ? H191 C19 H193 109.5 . . ? H192 C19 H193 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.461 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.063 #===END data_(2d) _database_code_depnum_ccdc_archive 'CCDC 652432' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H32 N4 S Si Ti' _chemical_formula_sum 'C18 H32 N4 S Si Ti' _chemical_formula_weight 412.53 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' S S 0.1246 0.1234 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8186(2) _cell_length_b 17.3817(4) _cell_length_c 12.8635(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.870(1) _cell_angle_gamma 90.00 _cell_volume 2155.95(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 36023 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 30.00 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.558 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.879 _exptl_absorpt_process_details ; SORTAV (R. H. Blessing, Acta Crystallogr., 1995, A51, 33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34166 _diffrn_reflns_av_R_equivalents 0.0755 _diffrn_reflns_av_sigmaI/netI 0.0680 _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 -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6260 _reflns_number_gt 4268 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997)' _computing_cell_refinement 'Denzo SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III (Burnett & Johnson, 1996)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995) ; _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^)+(0.0421P)^2^+0.6772P] 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 6260 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _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 Ti1 Ti 0.52352(3) 0.680455(19) 0.74738(2) 0.01866(9) Uani 1 1 d . . . S1 S 0.26217(6) 0.82833(3) 0.75560(4) 0.03032(13) Uani 1 1 d . . . Si1 Si 0.27713(5) 0.57835(3) 0.71509(4) 0.02006(12) Uani 1 1 d . . . N1 N 0.31483(16) 0.67675(9) 0.72456(12) 0.0202(3) Uani 1 1 d . . . N2 N 0.08885(17) 0.71558(10) 0.74316(13) 0.0269(4) Uani 1 1 d . . . N3 N 0.56301(18) 0.70093(10) 0.89522(13) 0.0280(4) Uani 1 1 d . . . N4 N 0.57220(17) 0.77792(10) 0.69214(13) 0.0272(4) Uani 1 1 d . . . C1 C 0.45700(19) 0.55581(10) 0.69420(14) 0.0194(4) Uani 1 1 d . . . C2 C 0.57809(19) 0.54669(11) 0.77606(14) 0.0214(4) Uani 1 1 d . . . C3 C 0.69305(19) 0.57728(11) 0.73973(15) 0.0228(4) Uani 1 1 d . . . C4 C 0.6482(2) 0.60349(11) 0.63304(15) 0.0231(4) Uani 1 1 d . . . C5 C 0.50507(19) 0.58929(11) 0.60449(14) 0.0213(4) Uani 1 1 d . . . C6 C 0.5860(2) 0.50833(12) 0.88202(16) 0.0279(4) Uani 1 1 d . . . H61 H 0.6537 0.4679 0.8897 0.034 Uiso 1 1 calc R . . H62 H 0.4970 0.4871 0.8866 0.034 Uiso 1 1 calc R . . H63 H 0.6122 0.5455 0.9373 0.034 Uiso 1 1 calc R . . C7 C 0.8424(2) 0.57333(13) 0.79519(18) 0.0318(5) Uani 1 1 d . . . H71 H 0.8466 0.5685 0.8701 0.038 Uiso 1 1 calc R . . H72 H 0.8896 0.6194 0.7809 0.038 Uiso 1 1 calc R . . H73 H 0.8861 0.5296 0.7699 0.038 Uiso 1 1 calc R . . C8 C 0.7448(2) 0.63184(14) 0.56440(17) 0.0328(5) Uani 1 1 d . . . H81 H 0.7956 0.5892 0.5433 0.039 Uiso 1 1 calc R . . H82 H 0.8084 0.6682 0.6032 0.039 Uiso 1 1 calc R . . H83 H 0.6923 0.6562 0.5026 0.039 Uiso 1 1 calc R . . C9 C 0.4178(2) 0.60316(12) 0.49656(15) 0.0280(4) Uani 1 1 d . . . H91 H 0.4706 0.6318 0.4541 0.034 Uiso 1 1 calc R . . H92 H 0.3365 0.6318 0.5037 0.034 Uiso 1 1 calc R . . H93 H 0.3908 0.5547 0.4631 0.034 Uiso 1 1 calc R . . C10 C 0.2331(2) 0.54089(12) 0.84032(16) 0.0285(4) Uani 1 1 d . . . H101 H 0.3011 0.5583 0.8993 0.034 Uiso 1 1 calc R . . H102 H 0.2323 0.4857 0.8387 0.034 Uiso 1 1 calc R . . H103 H 0.1432 0.5594 0.8475 0.034 Uiso 1 1 calc R . . C11 C 0.1345(2) 0.55015(13) 0.60506(17) 0.0318(5) Uani 1 1 d . . . H111 H 0.0478 0.5687 0.6194 0.038 Uiso 1 1 calc R . . H112 H 0.1312 0.4951 0.5990 0.038 Uiso 1 1 calc R . . H113 H 0.1508 0.5721 0.5400 0.038 Uiso 1 1 calc R . . C12 C 0.2188(2) 0.73036(11) 0.73878(14) 0.0216(4) Uani 1 1 d . . . C13 C 0.0939(2) 0.84786(13) 0.76864(16) 0.0328(5) Uani 1 1 d . . . H13 H 0.0595 0.8963 0.7803 0.039 Uiso 1 1 calc R . . C14 C 0.0203(2) 0.78228(13) 0.75942(16) 0.0316(5) Uani 1 1 d . . . H14 H -0.0731 0.7820 0.7638 0.038 Uiso 1 1 calc R . . C15 C 0.4703(2) 0.70407(14) 0.97127(16) 0.0373(5) Uani 1 1 d . . . H151 H 0.4888 0.6613 1.0190 0.045 Uiso 1 1 calc R . . H152 H 0.3758 0.7017 0.9343 0.045 Uiso 1 1 calc R . . H153 H 0.4851 0.7513 1.0106 0.045 Uiso 1 1 calc R . . C16 C 0.7071(2) 0.70458(15) 0.94962(18) 0.0416(6) Uani 1 1 d . . . H161 H 0.7201 0.7488 0.9952 0.050 Uiso 1 1 calc R . . H162 H 0.7664 0.7085 0.8984 0.050 Uiso 1 1 calc R . . H163 H 0.7298 0.6588 0.9911 0.050 Uiso 1 1 calc R . . C17 C 0.5674(3) 0.79657(14) 0.58071(18) 0.0412(6) Uani 1 1 d . . . H171 H 0.5091 0.8406 0.5618 0.049 Uiso 1 1 calc R . . H172 H 0.5306 0.7536 0.5376 0.049 Uiso 1 1 calc R . . H173 H 0.6593 0.8078 0.5696 0.049 Uiso 1 1 calc R . . C18 C 0.6164(2) 0.84608(13) 0.75578(19) 0.0401(5) Uani 1 1 d . . . H181 H 0.7077 0.8608 0.7467 0.048 Uiso 1 1 calc R . . H182 H 0.6178 0.8349 0.8290 0.048 Uiso 1 1 calc R . . H183 H 0.5529 0.8875 0.7335 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.02082(17) 0.01629(17) 0.01934(16) -0.00060(13) 0.00500(13) -0.00093(13) S1 0.0387(3) 0.0179(3) 0.0358(3) -0.0013(2) 0.0108(2) 0.0027(2) Si1 0.0193(3) 0.0176(3) 0.0234(3) -0.0008(2) 0.0042(2) -0.0005(2) N1 0.0234(8) 0.0166(8) 0.0213(7) -0.0010(6) 0.0060(6) 0.0015(6) N2 0.0251(9) 0.0270(9) 0.0302(9) 0.0006(7) 0.0096(7) 0.0055(7) N3 0.0344(10) 0.0275(9) 0.0222(8) -0.0039(7) 0.0056(7) -0.0060(7) N4 0.0266(9) 0.0220(9) 0.0335(9) 0.0029(7) 0.0069(7) -0.0031(7) C1 0.0220(9) 0.0141(9) 0.0222(9) -0.0005(7) 0.0050(7) 0.0004(7) C2 0.0241(10) 0.0157(9) 0.0243(9) 0.0012(7) 0.0045(8) 0.0006(7) C3 0.0213(9) 0.0202(10) 0.0272(10) 0.0000(8) 0.0049(8) 0.0012(7) C4 0.0258(10) 0.0210(10) 0.0240(9) -0.0012(8) 0.0087(8) 0.0036(8) C5 0.0237(10) 0.0187(10) 0.0213(9) -0.0024(7) 0.0035(8) 0.0028(7) C6 0.0279(11) 0.0271(11) 0.0274(10) 0.0072(8) 0.0017(9) -0.0016(8) C7 0.0245(10) 0.0305(12) 0.0406(12) 0.0031(9) 0.0063(9) 0.0001(9) C8 0.0290(11) 0.0408(14) 0.0313(11) 0.0022(9) 0.0127(9) 0.0018(9) C9 0.0314(11) 0.0304(11) 0.0219(10) -0.0009(8) 0.0048(8) 0.0028(9) C10 0.0263(11) 0.0270(11) 0.0340(11) 0.0041(9) 0.0102(9) -0.0005(8) C11 0.0254(11) 0.0342(12) 0.0344(11) -0.0077(9) 0.0020(9) -0.0013(9) C12 0.0280(10) 0.0201(10) 0.0170(8) 0.0011(7) 0.0048(8) 0.0023(8) C13 0.0455(13) 0.0256(11) 0.0295(11) 0.0015(9) 0.0130(10) 0.0161(10) C14 0.0317(11) 0.0329(13) 0.0321(11) 0.0015(9) 0.0110(9) 0.0122(9) C15 0.0449(14) 0.0436(14) 0.0245(10) -0.0053(9) 0.0094(10) 0.0003(11) C16 0.0400(13) 0.0506(16) 0.0330(12) -0.0085(11) 0.0040(10) -0.0144(11) C17 0.0472(14) 0.0348(13) 0.0410(13) 0.0164(10) 0.0071(11) -0.0035(11) C18 0.0448(13) 0.0221(11) 0.0544(14) 0.0014(10) 0.0119(11) -0.0054(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N3 1.9014(16) . ? Ti1 N4 1.9317(17) . ? Ti1 N1 2.0154(16) . ? Ti1 C1 2.3280(18) . ? Ti1 C2 2.3989(19) . ? Ti1 C5 2.4077(18) . ? Ti1 C3 2.4614(19) . ? Ti1 C4 2.4763(19) . ? Ti1 Si1 2.9657(6) . ? S1 C13 1.725(2) . ? S1 C12 1.759(2) . ? Si1 N1 1.7493(16) . ? Si1 C11 1.860(2) . ? Si1 C10 1.862(2) . ? Si1 C1 1.8771(19) . ? N1 C12 1.362(2) . ? N2 C12 1.314(2) . ? N2 C14 1.376(3) . ? N3 C16 1.457(3) . ? N3 C15 1.458(3) . ? N4 C18 1.459(3) . ? N4 C17 1.462(3) . ? C1 C2 1.441(3) . ? C1 C5 1.449(3) . ? C2 C3 1.405(3) . ? C2 C6 1.506(3) . ? C3 C4 1.434(3) . ? C3 C7 1.506(3) . ? C4 C5 1.406(3) . ? C4 C8 1.495(3) . ? C5 C9 1.507(3) . ? C6 H61 0.9600 . ? C6 H62 0.9600 . ? C6 H63 0.9600 . ? C7 H71 0.9600 . ? C7 H72 0.9600 . ? C7 H73 0.9600 . ? C8 H81 0.9600 . ? C8 H82 0.9600 . ? C8 H83 0.9600 . ? C9 H91 0.9600 . ? C9 H92 0.9600 . ? C9 H93 0.9600 . ? C10 H101 0.9600 . ? C10 H102 0.9600 . ? C10 H103 0.9600 . ? C11 H111 0.9600 . ? C11 H112 0.9600 . ? C11 H113 0.9600 . ? C13 C14 1.343(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H151 0.9600 . ? C15 H152 0.9600 . ? C15 H153 0.9600 . ? C16 H161 0.9600 . ? C16 H162 0.9600 . ? C16 H163 0.9600 . ? C17 H171 0.9600 . ? C17 H172 0.9600 . ? C17 H173 0.9600 . ? C18 H181 0.9600 . ? C18 H182 0.9600 . ? C18 H183 0.9600 . ? 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 N3 Ti1 N4 100.71(7) . . ? N3 Ti1 N1 99.30(7) . . ? N4 Ti1 N1 106.84(7) . . ? N3 Ti1 C1 117.46(7) . . ? N4 Ti1 C1 141.55(7) . . ? N1 Ti1 C1 72.92(6) . . ? N3 Ti1 C2 91.72(7) . . ? N4 Ti1 C2 147.45(7) . . ? N1 Ti1 C2 100.54(6) . . ? C1 Ti1 C2 35.45(6) . . ? N3 Ti1 C5 149.15(7) . . ? N4 Ti1 C5 106.53(7) . . ? N1 Ti1 C5 86.54(6) . . ? C1 Ti1 C5 35.58(6) . . ? C2 Ti1 C5 57.45(6) . . ? N3 Ti1 C3 99.47(7) . . ? N4 Ti1 C3 114.09(7) . . ? N1 Ti1 C3 130.35(6) . . ? C1 Ti1 C3 57.63(6) . . ? C2 Ti1 C3 33.57(6) . . ? C5 Ti1 C3 56.22(6) . . ? N3 Ti1 C4 131.67(7) . . ? N4 Ti1 C4 94.06(7) . . ? N1 Ti1 C4 119.95(6) . . ? C1 Ti1 C4 57.69(6) . . ? C2 Ti1 C4 56.40(6) . . ? C5 Ti1 C4 33.42(6) . . ? C3 Ti1 C4 33.77(6) . . ? N3 Ti1 Si1 105.02(5) . . ? N4 Ti1 Si1 136.48(5) . . ? N1 Ti1 Si1 34.96(4) . . ? C1 Ti1 Si1 39.26(5) . . ? C2 Ti1 Si1 66.06(5) . . ? C5 Ti1 Si1 63.72(5) . . ? C3 Ti1 Si1 95.64(5) . . ? C4 Ti1 Si1 94.31(5) . . ? C13 S1 C12 89.35(10) . . ? N1 Si1 C11 115.46(9) . . ? N1 Si1 C10 111.24(9) . . ? C11 Si1 C10 107.56(10) . . ? N1 Si1 C1 91.24(8) . . ? C11 Si1 C1 115.47(9) . . ? C10 Si1 C1 115.41(9) . . ? N1 Si1 Ti1 41.31(5) . . ? C11 Si1 Ti1 137.89(8) . . ? C10 Si1 Ti1 113.86(7) . . ? C1 Si1 Ti1 51.71(6) . . ? C12 N1 Si1 122.39(13) . . ? C12 N1 Ti1 131.98(13) . . ? Si1 N1 Ti1 103.73(8) . . ? C12 N2 C14 110.41(18) . . ? C16 N3 C15 110.42(16) . . ? C16 N3 Ti1 119.02(14) . . ? C15 N3 Ti1 130.00(14) . . ? C18 N4 C17 108.74(17) . . ? C18 N4 Ti1 125.02(14) . . ? C17 N4 Ti1 126.21(14) . . ? C2 C1 C5 106.17(15) . . ? C2 C1 Si1 125.97(14) . . ? C5 C1 Si1 119.14(13) . . ? C2 C1 Ti1 74.96(10) . . ? C5 C1 Ti1 75.21(10) . . ? Si1 C1 Ti1 89.03(7) . . ? C3 C2 C1 108.62(16) . . ? C3 C2 C6 124.13(17) . . ? C1 C2 C6 127.20(17) . . ? C3 C2 Ti1 75.66(11) . . ? C1 C2 Ti1 69.59(10) . . ? C6 C2 Ti1 122.69(13) . . ? C2 C3 C4 108.53(16) . . ? C2 C3 C7 126.62(17) . . ? C4 C3 C7 124.28(18) . . ? C2 C3 Ti1 70.77(11) . . ? C4 C3 Ti1 73.68(11) . . ? C7 C3 Ti1 128.27(14) . . ? C5 C4 C3 107.78(16) . . ? C5 C4 C8 128.12(17) . . ? C3 C4 C8 123.74(17) . . ? C5 C4 Ti1 70.61(10) . . ? C3 C4 Ti1 72.55(11) . . ? C8 C4 Ti1 127.75(14) . . ? C4 C5 C1 108.80(16) . . ? C4 C5 C9 125.40(17) . . ? C1 C5 C9 125.74(17) . . ? C4 C5 Ti1 75.97(11) . . ? C1 C5 Ti1 69.21(10) . . ? C9 C5 Ti1 123.09(13) . . ? C2 C6 H61 109.5 . . ? C2 C6 H62 109.5 . . ? H61 C6 H62 109.5 . . ? C2 C6 H63 109.5 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 109.5 . . ? C3 C7 H71 109.5 . . ? C3 C7 H72 109.5 . . ? H71 C7 H72 109.5 . . ? C3 C7 H73 109.5 . . ? H71 C7 H73 109.5 . . ? H72 C7 H73 109.5 . . ? C4 C8 H81 109.5 . . ? C4 C8 H82 109.5 . . ? H81 C8 H82 109.5 . . ? C4 C8 H83 109.5 . . ? H81 C8 H83 109.5 . . ? H82 C8 H83 109.5 . . ? C5 C9 H91 109.5 . . ? C5 C9 H92 109.5 . . ? H91 C9 H92 109.5 . . ? C5 C9 H93 109.5 . . ? H91 C9 H93 109.5 . . ? H92 C9 H93 109.5 . . ? Si1 C10 H101 109.5 . . ? Si1 C10 H102 109.5 . . ? H101 C10 H102 109.5 . . ? Si1 C10 H103 109.5 . . ? H101 C10 H103 109.5 . . ? H102 C10 H103 109.5 . . ? Si1 C11 H111 109.5 . . ? Si1 C11 H112 109.5 . . ? H111 C11 H112 109.5 . . ? Si1 C11 H113 109.5 . . ? H111 C11 H113 109.5 . . ? H112 C11 H113 109.5 . . ? N2 C12 N1 125.07(18) . . ? N2 C12 S1 113.49(14) . . ? N1 C12 S1 121.44(14) . . ? C14 C13 S1 109.50(16) . . ? C14 C13 H13 125.3 . . ? S1 C13 H13 125.3 . . ? C13 C14 N2 117.25(19) . . ? C13 C14 H14 121.4 . . ? N2 C14 H14 121.4 . . ? N3 C15 H151 109.5 . . ? N3 C15 H152 109.5 . . ? H151 C15 H152 109.5 . . ? N3 C15 H153 109.5 . . ? H151 C15 H153 109.5 . . ? H152 C15 H153 109.5 . . ? N3 C16 H161 109.5 . . ? N3 C16 H162 109.5 . . ? H161 C16 H162 109.5 . . ? N3 C16 H163 109.5 . . ? H161 C16 H163 109.5 . . ? H162 C16 H163 109.5 . . ? N4 C17 H171 109.5 . . ? N4 C17 H172 109.5 . . ? H171 C17 H172 109.5 . . ? N4 C17 H173 109.5 . . ? H171 C17 H173 109.5 . . ? H172 C17 H173 109.5 . . ? N4 C18 H181 109.5 . . ? N4 C18 H182 109.5 . . ? H181 C18 H182 109.5 . . ? N4 C18 H183 109.5 . . ? H181 C18 H183 109.5 . . ? H182 C18 H183 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.373 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.091