# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Philip Mountford' _publ_contact_author_address ; Chemistry Research Laboratory Oxford University Mansfield Road Oxford OX1 3TA UNITED KINGDOM ; _publ_contact_author_email PHILIP.MOUNTFORD@CHEMISTRY.OXFORD.AC.UK _publ_section_title ; New ligand platforms for developing the chemistry of the Ti=N-NR2 functional group and insertion of alkynes into the N-N bond of a Ti=N-NPh2 ligand ; loop_ _publ_author_name 'Philip Mountford' 'Eric Clot' 'Marta Feliz' 'Catherine D. Manley' 'Andrew D. Schwarz' 'Jonathan D. Selby' data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 656394' # Local code adscw19 _chemical_name_systematic ; Ti{MeN(CH2CH2SiMe3)2}(NNNPh2)(py) ; _publ_section_exptl_refinement ; The crystal was small and a weak diffractor. The relections had an average I/s(I) of 6.5. The SiMe3 group of Si(2) was positionally disordered over two sites. However, a satisfactory rational two-site model could not be developed and so this group was refined subject to similarity restraints on the Si(2)-Me distances, N(4)-Si(2)-Me angles and displacement parameters. The pyridine ligand was also disordered and two sets of 0.5 occupancy C atoms for this ligand were positionally and isotropically refined subject to similarity restraints on the displacement parameters. ; _chemical_melting_point ? _cell_length_a 10.1794(5) _cell_length_b 11.1800(7) _cell_length_c 13.8952(8) _cell_angle_alpha 89.726(3) _cell_angle_beta 77.178(2) _cell_angle_gamma 85.912(3) _cell_volume 1537.90(15) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C28 H44 N6 Si2 Ti1' _chemical_formula_moiety 'C28 H44 N6 Si2 Ti1' _chemical_compound_source ? _chemical_formula_weight 568.77 _cell_measurement_reflns_used 4943 _cell_measurement_theta_min 5 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_meas ? _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 9697 _reflns_number_total 5728 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_theta_min 5.145 _diffrn_reflns_theta_max 25.630 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.117 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -11 _reflns_limit_h_max 12 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.84 _refine_diff_density_max 1.05 _refine_ls_number_reflns 3146 _refine_ls_number_restraints 114 _refine_ls_number_parameters 379 _refine_ls_wR_factor_ref 0.0800 _refine_ls_goodness_of_fit_ref 1.2067 _refine_ls_R_factor_all 0.1286 _refine_ls_wR_factor_all 0.1097 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 3146 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_gt 0.0800 _refine_ls_shift/su_max 0.004 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.16 0.913E-01 0.941 -0.622E-01 0.234 ; # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 1.02802(10) 0.26639(10) 0.22363(7) 0.0284 1.0000 Uani . . . . . . N1 N 1.0205(5) 0.1170(4) 0.2566(3) 0.0314 1.0000 Uani . . . . . . N2 N 1.0195(5) -0.0001(5) 0.2834(4) 0.0358 1.0000 Uani . . . . . . N3 N 0.8692(4) 0.3740(4) 0.2977(3) 0.0300 1.0000 Uani . . . . . . N4 N 1.2118(4) 0.3074(4) 0.1455(3) 0.0363 1.0000 Uani D . . . . . N5 N 1.1113(4) 0.3435(4) 0.3428(3) 0.0291 1.0000 Uani . . . . . . N6 N 0.9377(5) 0.2622(6) 0.0927(4) 0.0487 1.0000 Uani . U . . . . Si1 Si 0.69819(16) 0.35603(16) 0.32181(12) 0.0356 1.0000 Uani . . . . . . Si2 Si 1.3111(2) 0.2605(2) 0.03302(12) 0.0546 1.0000 Uani D U . . . . C1 C 0.8947(5) -0.0365(5) 0.3429(4) 0.0342 1.0000 Uani . . . . . . C2 C 0.8398(6) 0.0202(6) 0.4336(5) 0.0399 1.0000 Uani . . . . . . C3 C 0.7175(7) -0.0126(7) 0.4905(5) 0.0495 1.0000 Uani . . . . . . C4 C 0.6509(7) -0.1018(7) 0.4596(6) 0.0519 1.0000 Uani . . . . . . C5 C 0.7055(7) -0.1592(7) 0.3704(7) 0.0565 1.0000 Uani . . . . . . C6 C 0.8274(7) -0.1266(6) 0.3115(5) 0.0458 1.0000 Uani . . . . . . C7 C 1.1400(6) -0.0689(6) 0.2829(4) 0.0342 1.0000 Uani . . . . . . C8 C 1.2648(6) -0.0203(6) 0.2402(4) 0.0405 1.0000 Uani . . . . . . C9 C 1.3839(6) -0.0894(7) 0.2367(5) 0.0491 1.0000 Uani . . . . . . C10 C 1.3864(6) -0.2035(8) 0.2736(5) 0.0529 1.0000 Uani . . . . . . C11 C 1.2646(7) -0.2510(7) 0.3155(5) 0.0476 1.0000 Uani . . . . . . C12 C 1.1427(6) -0.1848(6) 0.3214(5) 0.0400 1.0000 Uani . . . . . . C13 C 0.9027(6) 0.4718(5) 0.3560(5) 0.0367 1.0000 Uani . . . . . . C14 C 1.0554(6) 0.4693(5) 0.3450(4) 0.0328 1.0000 Uani . . . . . . C15 C 1.2596(5) 0.3347(7) 0.3109(4) 0.0429 1.0000 Uani . . . . . . C16 C 1.2997(7) 0.3688(8) 0.2036(5) 0.0522 1.0000 Uani . . . . . . C17 C 1.0699(6) 0.2869(6) 0.4405(4) 0.0356 1.0000 Uani . . . . . . C18 C 0.6249(8) 0.3411(8) 0.4573(6) 0.0617 1.0000 Uani . . . . . . C19 C 0.6568(6) 0.2208(6) 0.2598(6) 0.0486 1.0000 Uani . . . . . . C20 C 0.6068(7) 0.4911(7) 0.2826(7) 0.0623 1.0000 Uani . . . . . . C21 C 1.4298(10) 0.3691(8) -0.0260(6) 0.1157 1.0000 Uani D U . . . . C24 C 0.919(2) 0.386(2) 0.0511(19) 0.0480 0.5000 Uani . U . . . . C241 C 0.900(2) 0.348(2) 0.0513(19) 0.0433 0.5000 Uani . U . . . . C25 C 0.8672(16) 0.407(2) -0.0317(13) 0.0536 0.5000 Uani . U . . . . C251 C 0.8428(17) 0.3466(18) -0.0295(14) 0.0452 0.5000 Uani . U . . . . C26 C 0.8294(16) 0.302(3) -0.0779(14) 0.0557 0.5000 Uani . U . . . . C261 C 0.8138(17) 0.2310(19) -0.0600(15) 0.0441 0.5000 Uani . U . . . . C27 C 0.854(2) 0.189(3) -0.0369(13) 0.0566 0.5000 Uani . U . . . . C271 C 0.8485(19) 0.1287(18) -0.0173(13) 0.0508 0.5000 Uani . U . . . . C28 C 0.897(2) 0.178(2) 0.0455(17) 0.0538 0.5000 Uani . U . . . . C281 C 0.916(2) 0.143(2) 0.0614(16) 0.0488 0.5000 Uani . U . . . . H21 H 0.8892 0.0844 0.4569 0.0483 1.0000 Uiso R . . . . . H31 H 0.6781 0.0298 0.5547 0.0588 1.0000 Uiso R . . . . . H41 H 0.5632 -0.1256 0.5007 0.0648 1.0000 Uiso R . . . . . H51 H 0.6575 -0.2248 0.3475 0.0713 1.0000 Uiso R . . . . . H61 H 0.8662 -0.1678 0.2467 0.0597 1.0000 Uiso R . . . . . H81 H 1.2650 0.0629 0.2134 0.0503 1.0000 Uiso R . . . . . H91 H 1.4716 -0.0549 0.2071 0.0592 1.0000 Uiso R . . . . . H101 H 1.4740 -0.2516 0.2702 0.0677 1.0000 Uiso R . . . . . H111 H 1.2656 -0.3342 0.3420 0.0596 1.0000 Uiso R . . . . . H121 H 1.0559 -0.2195 0.3532 0.0484 1.0000 Uiso R . . . . . H131 H 0.8597 0.4597 0.4271 0.0496 1.0000 Uiso R . . . . . H132 H 0.8676 0.5506 0.3339 0.0496 1.0000 Uiso R . . . . . H141 H 1.0776 0.5134 0.4011 0.0442 1.0000 Uiso R . . . . . H142 H 1.0955 0.5084 0.2814 0.0442 1.0000 Uiso R . . . . . H151 H 1.2986 0.3890 0.3525 0.0534 1.0000 Uiso R . . . . . H152 H 1.2950 0.2501 0.3179 0.0534 1.0000 Uiso R . . . . . H161 H 1.3972 0.3448 0.1755 0.0674 1.0000 Uiso R . . . . . H162 H 1.2834 0.4576 0.1984 0.0674 1.0000 Uiso R . . . . . H171 H 1.1089 0.2019 0.4370 0.0452 1.0000 Uiso R . . . . . H172 H 1.1034 0.3321 0.4911 0.0452 1.0000 Uiso R . . . . . H173 H 0.9691 0.2884 0.4594 0.0452 1.0000 Uiso R . . . . . H181 H 0.5258 0.3311 0.4682 0.0706 1.0000 Uiso R . . . . . H182 H 0.6396 0.4145 0.4932 0.0706 1.0000 Uiso R . . . . . H183 H 0.6704 0.2693 0.4825 0.0706 1.0000 Uiso R . . . . . H191 H 0.5569 0.2140 0.2762 0.0610 1.0000 Uiso R . . . . . H192 H 0.7027 0.1480 0.2833 0.0610 1.0000 Uiso R . . . . . H193 H 0.6892 0.2275 0.1867 0.0610 1.0000 Uiso R . . . . . H201 H 0.5076 0.4805 0.2973 0.0746 1.0000 Uiso R . . . . . H202 H 0.6239 0.5634 0.3189 0.0746 1.0000 Uiso R . . . . . H203 H 0.6403 0.5020 0.2101 0.0746 1.0000 Uiso R . . . . . H241 H 0.9444 0.4553 0.0862 0.0609 0.5000 Uiso R . . . . . H251 H 0.8552 0.4883 -0.0595 0.0672 0.5000 Uiso R . . . . . H261 H 0.7873 0.3100 -0.1363 0.0691 0.5000 Uiso R . . . . . H271 H 0.8362 0.1156 -0.0716 0.0698 0.5000 Uiso R . . . . . H281 H 0.9041 0.0961 0.0735 0.0601 0.5000 Uiso R . . . . . H2411 H 0.9182 0.4280 0.0755 0.0484 0.5000 Uiso R . . . . . H2511 H 0.8196 0.4221 -0.0629 0.0528 0.5000 Uiso R . . . . . H2611 H 0.7674 0.2267 -0.1161 0.0535 0.5000 Uiso R . . . . . H2711 H 0.8299 0.0489 -0.0415 0.0609 0.5000 Uiso R . . . . . H2811 H 0.9421 0.0707 0.0978 0.0614 0.5000 Uiso R . . . . . C23 C 1.4467(10) 0.1483(11) 0.0406(4) 0.1089 1.0000 Uani D U . . . . C22 C 1.2191(7) 0.2314(14) -0.0598(5) 0.1160 1.0000 Uani D U . . . . H211 H 1.4837 0.3361 -0.0907 0.1301 1.0000 Uiso R . . . . . H212 H 1.4921 0.3852 0.0182 0.1301 1.0000 Uiso R . . . . . H213 H 1.3783 0.4455 -0.0372 0.1301 1.0000 Uiso R . . . . . H221 H 1.2835 0.2048 -0.1226 0.1354 1.0000 Uiso R . . . . . H222 H 1.1648 0.3058 -0.0717 0.1354 1.0000 Uiso R . . . . . H223 H 1.1573 0.1666 -0.0360 0.1354 1.0000 Uiso R . . . . . H231 H 1.4996 0.1258 -0.0273 0.1237 1.0000 Uiso R . . . . . H232 H 1.5078 0.1812 0.0796 0.1237 1.0000 Uiso R . . . . . H233 H 1.4066 0.0758 0.0740 0.1237 1.0000 Uiso 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 0.0226(5) 0.0387(7) 0.0235(5) -0.0070(4) -0.0036(4) -0.0042(4) N1 0.029(2) 0.032(3) 0.033(2) -0.007(2) -0.0049(19) -0.003(2) N2 0.023(2) 0.037(3) 0.044(3) -0.005(2) 0.000(2) 0.003(2) N3 0.026(2) 0.036(3) 0.030(2) -0.007(2) -0.0095(19) -0.002(2) N4 0.033(3) 0.052(3) 0.023(2) -0.001(2) -0.0045(19) -0.004(2) N5 0.023(2) 0.038(3) 0.026(2) -0.006(2) -0.0054(18) -0.007(2) N6 0.029(2) 0.081(4) 0.036(3) -0.018(3) -0.008(2) 0.001(3) Si1 0.0251(8) 0.0410(11) 0.0392(9) -0.0123(8) -0.0043(7) -0.0012(7) Si2 0.0477(11) 0.0830(16) 0.0249(9) 0.0011(9) 0.0019(7) 0.0196(10) C1 0.023(3) 0.034(3) 0.045(3) -0.004(3) -0.008(2) 0.003(2) C2 0.033(3) 0.037(4) 0.048(4) -0.010(3) -0.005(3) -0.004(3) C3 0.034(3) 0.053(4) 0.055(4) 0.002(3) 0.002(3) 0.002(3) C4 0.027(3) 0.045(4) 0.080(5) 0.010(4) -0.006(3) 0.001(3) C5 0.043(4) 0.038(4) 0.099(6) 0.003(4) -0.033(4) -0.014(3) C6 0.044(4) 0.041(4) 0.056(4) -0.008(3) -0.017(3) -0.004(3) C7 0.029(3) 0.041(4) 0.034(3) -0.014(3) -0.010(2) 0.002(3) C8 0.032(3) 0.054(4) 0.033(3) -0.016(3) -0.004(3) 0.002(3) C9 0.030(3) 0.070(5) 0.046(4) -0.017(4) -0.008(3) 0.008(3) C10 0.031(4) 0.070(6) 0.057(4) -0.023(4) -0.015(3) 0.015(3) C11 0.039(4) 0.051(4) 0.055(4) -0.016(3) -0.019(3) 0.009(3) C12 0.039(3) 0.035(4) 0.046(4) -0.015(3) -0.012(3) 0.002(3) C13 0.034(3) 0.030(3) 0.048(4) -0.009(3) -0.012(3) 0.000(3) C14 0.038(3) 0.028(3) 0.035(3) -0.002(2) -0.011(2) -0.007(3) C15 0.021(3) 0.074(5) 0.034(3) -0.016(3) -0.007(2) -0.001(3) C16 0.034(3) 0.077(5) 0.044(4) -0.016(4) -0.001(3) -0.019(3) C17 0.043(3) 0.040(4) 0.027(3) -0.004(2) -0.014(2) -0.008(3) C18 0.059(5) 0.064(5) 0.053(4) -0.016(4) 0.011(4) -0.019(4) C19 0.028(3) 0.053(4) 0.066(4) -0.023(4) -0.014(3) 0.000(3) C20 0.035(4) 0.056(5) 0.098(6) -0.013(4) -0.023(4) 0.007(3) C21 0.079(5) 0.180(8) 0.075(5) 0.012(6) 0.002(5) 0.022(6) C24 0.024(6) 0.083(8) 0.040(6) -0.006(7) -0.014(5) 0.000(6) C241 0.027(6) 0.064(8) 0.040(6) -0.028(6) -0.016(5) 0.012(6) C25 0.034(6) 0.090(9) 0.040(6) -0.002(7) -0.014(5) -0.007(7) C251 0.037(6) 0.059(7) 0.043(6) -0.029(6) -0.022(5) 0.017(6) C26 0.042(6) 0.093(9) 0.040(6) -0.003(7) -0.020(5) -0.021(7) C261 0.039(6) 0.051(7) 0.046(7) -0.027(6) -0.025(5) 0.018(6) C27 0.048(7) 0.088(10) 0.040(7) -0.007(7) -0.019(5) -0.022(7) C271 0.053(6) 0.058(7) 0.045(7) -0.023(6) -0.024(5) 0.015(6) C28 0.039(6) 0.082(9) 0.043(7) -0.012(7) -0.014(6) -0.012(6) C281 0.043(6) 0.068(8) 0.039(6) -0.020(6) -0.022(5) 0.009(6) C23 0.069(5) 0.192(8) 0.052(4) -0.022(5) 0.000(4) 0.047(6) C22 0.091(6) 0.188(8) 0.059(5) -0.017(6) -0.008(5) 0.031(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3650(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . N1 . 1.733(5) yes Ti1 . N3 . 2.029(5) yes Ti1 . N4 . 2.026(5) yes Ti1 . N5 . 2.224(4) yes Ti1 . N6 . 2.215(5) yes N1 . N2 . 1.359(7) yes N2 . C1 . 1.438(7) yes N2 . C7 . 1.399(7) yes N3 . Si1 . 1.724(5) yes N3 . C13 . 1.467(7) yes N4 . Si2 . 1.723(5) yes N4 . C16 . 1.529(8) yes N5 . C14 . 1.477(7) yes N5 . C15 . 1.471(7) yes N5 . C17 . 1.483(7) yes N6 . C24 . 1.51(3) yes N6 . C241 . 1.20(3) yes N6 . C28 . 1.29(3) yes N6 . C281 . 1.45(2) yes Si1 . C18 . 1.876(8) yes Si1 . C19 . 1.863(7) yes Si1 . C20 . 1.860(8) yes Si2 . C21 . 1.835(8) yes Si2 . C23 . 1.819(7) yes Si2 . C22 . 1.797(8) yes C1 . C2 . 1.395(8) yes C1 . C6 . 1.383(9) yes C2 . C3 . 1.391(9) yes C2 . H21 . 1.000 no C3 . C4 . 1.367(10) yes C3 . H31 . 1.000 no C4 . C5 . 1.382(11) yes C4 . H41 . 1.000 no C5 . C6 . 1.397(10) yes C5 . H51 . 1.000 no C6 . H61 . 1.000 no C7 . C8 . 1.422(9) yes C7 . C12 . 1.401(9) yes C8 . C9 . 1.382(9) yes C8 . H81 . 1.000 no C9 . C10 . 1.373(11) yes C9 . H91 . 1.000 no C10 . C11 . 1.388(10) yes C10 . H101 . 1.000 no C11 . C12 . 1.385(9) yes C11 . H111 . 1.000 no C12 . H121 . 1.000 no C13 . C14 . 1.525(8) yes C13 . H131 . 1.000 no C13 . H132 . 1.000 no C14 . H141 . 1.000 no C14 . H142 . 1.000 no C15 . C16 . 1.511(9) yes C15 . H151 . 1.000 no C15 . H152 . 1.000 no C16 . H161 . 1.000 no C16 . H162 . 1.000 no C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no C18 . H181 . 1.000 no C18 . H182 . 1.000 no C18 . H183 . 1.000 no C19 . H191 . 1.000 no C19 . H192 . 1.000 no C19 . H193 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C24 . C25 . 1.38(3) yes C24 . H241 . 1.000 no C241 . C251 . 1.38(3) yes C241 . H2411 . 1.000 no C25 . C26 . 1.45(3) yes C25 . H251 . 1.000 no C251 . C261 . 1.43(3) yes C251 . H2511 . 1.000 no C26 . C27 . 1.41(3) yes C26 . H261 . 1.000 no C261 . C271 . 1.35(3) yes C261 . H2611 . 1.000 no C27 . C28 . 1.32(3) yes C27 . H271 . 1.000 no C271 . C281 . 1.43(3) yes C271 . H2711 . 1.000 no C28 . H281 . 1.000 no C281 . H2811 . 1.000 no H241 . H2411 . 0.464 no C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C22 . H221 . 1.000 no C22 . H222 . 1.000 no C22 . H223 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ti1 . N3 . 113.8(2) yes N1 . Ti1 . N4 . 113.7(2) yes N3 . Ti1 . N4 . 130.5(2) yes N1 . Ti1 . N5 . 102.1(2) yes N3 . Ti1 . N5 . 77.75(17) yes N4 . Ti1 . N5 . 79.64(17) yes N1 . Ti1 . N6 . 99.3(2) yes N3 . Ti1 . N6 . 91.07(19) yes N4 . Ti1 . N6 . 94.38(19) yes N5 . Ti1 . N6 . 158.4(2) yes Ti1 . N1 . N2 . 177.7(4) yes N1 . N2 . C1 . 116.1(4) yes N1 . N2 . C7 . 120.9(5) yes C1 . N2 . C7 . 119.5(5) yes Ti1 . N3 . Si1 . 130.5(3) yes Ti1 . N3 . C13 . 115.8(3) yes Si1 . N3 . C13 . 112.6(4) yes Ti1 . N4 . Si2 . 133.8(3) yes Ti1 . N4 . C16 . 115.9(3) yes Si2 . N4 . C16 . 108.5(4) yes Ti1 . N5 . C14 . 101.2(3) yes Ti1 . N5 . C15 . 108.1(3) yes C14 . N5 . C15 . 111.4(5) yes Ti1 . N5 . C17 . 114.8(3) yes C14 . N5 . C17 . 111.2(4) yes C15 . N5 . C17 . 109.9(5) yes Ti1 . N6 . C24 . 112.1(10) yes Ti1 . N6 . C241 . 125.8(10) yes C24 . N6 . C241 . 15.1(16) yes Ti1 . N6 . C28 . 134.1(10) yes C24 . N6 . C28 . 113.8(14) yes C241 . N6 . C28 . 99.8(14) yes Ti1 . N6 . C281 . 114.5(9) yes C24 . N6 . C281 . 133.3(13) yes C241 . N6 . C281 . 119.6(13) yes C28 . N6 . C281 . 19.9(12) yes N3 . Si1 . C18 . 112.0(3) yes N3 . Si1 . C19 . 112.8(3) yes C18 . Si1 . C19 . 106.9(4) yes N3 . Si1 . C20 . 110.1(3) yes C18 . Si1 . C20 . 105.6(4) yes C19 . Si1 . C20 . 109.2(3) yes N4 . Si2 . C21 . 114.28(10) yes N4 . Si2 . C23 . 114.50(10) yes C21 . Si2 . C23 . 92.5(6) yes N4 . Si2 . C22 . 114.70(10) yes C21 . Si2 . C22 . 103.3(5) yes C23 . Si2 . C22 . 114.9(5) yes N2 . C1 . C2 . 119.8(5) yes N2 . C1 . C6 . 121.0(5) yes C2 . C1 . C6 . 119.2(6) yes C1 . C2 . C3 . 120.1(6) yes C1 . C2 . H21 . 119.2 no C3 . C2 . H21 . 120.7 no C2 . C3 . C4 . 120.7(7) yes C2 . C3 . H31 . 119.4 no C4 . C3 . H31 . 119.8 no C3 . C4 . C5 . 119.5(6) yes C3 . C4 . H41 . 120.7 no C5 . C4 . H41 . 119.8 no C4 . C5 . C6 . 120.6(7) yes C4 . C5 . H51 . 119.8 no C6 . C5 . H51 . 119.5 no C5 . C6 . C1 . 119.9(6) yes C5 . C6 . H61 . 120.5 no C1 . C6 . H61 . 119.7 no N2 . C7 . C8 . 118.9(6) yes N2 . C7 . C12 . 122.6(5) yes C8 . C7 . C12 . 118.5(5) yes C7 . C8 . C9 . 119.1(7) yes C7 . C8 . H81 . 119.7 no C9 . C8 . H81 . 121.2 no C8 . C9 . C10 . 122.4(7) yes C8 . C9 . H91 . 119.0 no C10 . C9 . H91 . 118.6 no C9 . C10 . C11 . 118.6(6) yes C9 . C10 . H101 . 120.8 no C11 . C10 . H101 . 120.6 no C10 . C11 . C12 . 121.1(7) yes C10 . C11 . H111 . 119.1 no C12 . C11 . H111 . 119.8 no C7 . C12 . C11 . 120.3(6) yes C7 . C12 . H121 . 119.5 no C11 . C12 . H121 . 120.2 no N3 . C13 . C14 . 110.0(5) yes N3 . C13 . H131 . 108.5 no C14 . C13 . H131 . 108.6 no N3 . C13 . H132 . 109.9 no C14 . C13 . H132 . 110.3 no H131 . C13 . H132 . 109.5 no C13 . C14 . N5 . 109.3(5) yes C13 . C14 . H141 . 110.4 no N5 . C14 . H141 . 109.8 no C13 . C14 . H142 . 108.6 no N5 . C14 . H142 . 109.3 no H141 . C14 . H142 . 109.5 no N5 . C15 . C16 . 109.4(5) yes N5 . C15 . H151 . 109.8 no C16 . C15 . H151 . 110.2 no N5 . C15 . H152 . 109.4 no C16 . C15 . H152 . 108.5 no H151 . C15 . H152 . 109.5 no N4 . C16 . C15 . 109.1(5) yes N4 . C16 . H161 . 109.8 no C15 . C16 . H161 . 111.0 no N4 . C16 . H162 . 108.7 no C15 . C16 . H162 . 108.7 no H161 . C16 . H162 . 109.5 no N5 . C17 . H171 . 109.6 no N5 . C17 . H172 . 109.6 no H171 . C17 . H172 . 109.5 no N5 . C17 . H173 . 109.2 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no Si1 . C18 . H181 . 109.6 no Si1 . C18 . H182 . 109.7 no H181 . C18 . H182 . 109.5 no Si1 . C18 . H183 . 109.1 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no Si1 . C19 . H191 . 109.8 no Si1 . C19 . H192 . 109.0 no H191 . C19 . H192 . 109.5 no Si1 . C19 . H193 . 109.6 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no Si1 . C20 . H201 . 109.8 no Si1 . C20 . H202 . 109.6 no H201 . C20 . H202 . 109.5 no Si1 . C20 . H203 . 108.9 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no Si2 . C21 . H211 . 109.9 no Si2 . C21 . H212 . 109.2 no H211 . C21 . H212 . 109.5 no Si2 . C21 . H213 . 109.3 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no N6 . C24 . C25 . 123.2(18) yes N6 . C24 . H241 . 117.7 no C25 . C24 . H241 . 119.0 no N6 . C241 . C251 . 126.4(17) yes N6 . C241 . H2411 . 116.4 no C251 . C241 . H2411 . 117.1 no C24 . C25 . C26 . 116.3(19) yes C24 . C25 . H251 . 123.3 no C26 . C25 . H251 . 120.4 no C241 . C251 . C261 . 115.8(17) yes C241 . C251 . H2511 . 121.9 no C261 . C251 . H2511 . 122.3 no C25 . C26 . C27 . 117.5(16) yes C25 . C26 . H261 . 121.4 no C27 . C26 . H261 . 121.1 no C251 . C261 . C271 . 122.7(17) yes C251 . C261 . H2611 . 118.2 no C271 . C261 . H2611 . 119.1 no C26 . C27 . C28 . 122(2) yes C26 . C27 . H271 . 118.5 no C28 . C27 . H271 . 119.8 no C261 . C271 . C281 . 115.5(17) yes C261 . C271 . H2711 . 121.1 no C281 . C271 . H2711 . 123.4 no C27 . C28 . N6 . 127(2) yes C27 . C28 . H281 . 117.4 no N6 . C28 . H281 . 115.6 no N6 . C281 . C271 . 119.8(16) yes N6 . C281 . H2811 . 120.3 no C271 . C281 . H2811 . 119.8 no C24 . H241 . H2411 . 19.3 no C241 . H2411 . H241 . 154.5 no Si2 . C23 . H231 . 109.8 no Si2 . C23 . H232 . 109.7 no H231 . C23 . H232 . 109.5 no Si2 . C23 . H233 . 108.9 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no Si2 . C22 . H221 . 109.9 no Si2 . C22 . H222 . 109.7 no H221 . C22 . H222 . 109.5 no Si2 . C22 . H223 . 108.8 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no _chemical_name_common Ti(MeN(CH2CH2SiMe3)2)(NNNPh2)(py) ##end data_Compound_7 _database_code_depnum_ccdc_archive 'CCDC 656395' # Local code adscw57 _chemical_name_systematic ; Ti{MeN(CH2CH2SiMe3)2}{NC(Ph)C(Me)NPh2}(py) ; _publ_section_exptl_refinement ; Comments: Examination of the ADPs for C(123) suggested some evidence of positional disorder. Attempts to refine a model in which this atom is "split", even with appropriate restraints, were unsuccessful. There are two crystallographically independent molecules in the asymmetric unit. ; _chemical_melting_point ? _cell_length_a 10.19100(10) _cell_length_b 19.6879(2) _cell_length_c 38.0089(4) _cell_angle_alpha 90 _cell_angle_beta 92.0565(4) _cell_angle_gamma 90 _cell_volume 7621.17(13) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C37 H52 N6 Si2 Ti1' _chemical_formula_moiety 'C37 H52 N6 Si2 Ti1' _chemical_compound_source ? _chemical_formula_weight 684.93 _cell_measurement_reflns_used 26230 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_meas ? _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.321 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 54098 _reflns_number_total 17133 _diffrn_reflns_av_R_equivalents 0.087 _diffrn_reflns_theta_min 5.107 _diffrn_reflns_theta_max 27.483 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.933 _diffrn_measured_fraction_theta_full 0.980 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 49 _oxford_diffrn_Wilson_B_factor 2.12 _oxford_diffrn_Wilson_scale 78.10 _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.32 _refine_diff_density_max 0.52 _refine_ls_number_reflns 6837 _refine_ls_number_restraints 0 _refine_ls_number_parameters 829 _refine_ls_wR_factor_ref 0.0443 _refine_ls_goodness_of_fit_ref 1.1400 _refine_ls_R_factor_all 0.1262 _refine_ls_wR_factor_all 0.1081 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 6837 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_gt 0.0443 _refine_ls_shift/su_max 0.006168 _chemical_absolute_configuration . _refine_ls_extinction_method None _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.370 0.120 0.160 ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.30593(6) 0.36476(3) 0.391024(15) 0.0232 1.0000 Uani . . . . . . N1 N 0.3307(3) 0.45279(13) 0.39491(7) 0.0243 1.0000 Uani . . . . . . N2 N 0.4390(3) 0.56662(14) 0.35797(7) 0.0277 1.0000 Uani . . . . . . N3 N 0.3500(3) 0.31157(14) 0.43541(8) 0.0323 1.0000 Uani . . . . . . N4 N 0.1976(3) 0.34010(14) 0.34784(8) 0.0302 1.0000 Uani . . . . . . N5 N 0.1069(3) 0.34646(14) 0.41185(8) 0.0308 1.0000 Uani . . . . . . N6 N 0.4843(3) 0.33348(13) 0.36449(7) 0.0246 1.0000 Uani . . . . . . Si1 Si 0.49688(11) 0.29196(6) 0.45718(3) 0.0365 1.0000 Uani . . . . . . Si2 Si 0.20051(10) 0.37389(5) 0.30609(3) 0.0332 1.0000 Uani . . . . . . C1 C 0.3295(3) 0.51817(16) 0.40760(8) 0.0240 1.0000 Uani . . . . . . C2 C 0.3768(3) 0.57336(17) 0.39128(9) 0.0271 1.0000 Uani . . . . . . C3 C 0.2704(3) 0.52609(16) 0.44290(9) 0.0281 1.0000 Uani . . . . . . C4 C 0.1589(4) 0.5656(2) 0.44745(11) 0.0398 1.0000 Uani . . . . . . C5 C 0.1059(5) 0.5719(2) 0.48028(13) 0.0560 1.0000 Uani . . . . . . C6 C 0.1641(5) 0.5392(3) 0.50878(12) 0.0616 1.0000 Uani . . . . . . C7 C 0.2737(5) 0.4995(2) 0.50477(11) 0.0544 1.0000 Uani . . . . . . C8 C 0.3254(4) 0.4928(2) 0.47177(10) 0.0398 1.0000 Uani . . . . . . C9 C 0.3738(4) 0.64542(17) 0.40460(10) 0.0364 1.0000 Uani . . . . . . C10 C 0.5753(3) 0.55596(17) 0.35863(9) 0.0282 1.0000 Uani . . . . . . C11 C 0.6480(4) 0.55820(18) 0.39061(10) 0.0353 1.0000 Uani . . . . . . C12 C 0.7822(4) 0.5485(2) 0.39190(12) 0.0431 1.0000 Uani . . . . . . C13 C 0.8491(4) 0.5360(2) 0.36164(13) 0.0483 1.0000 Uani . . . . . . C14 C 0.7777(4) 0.5312(2) 0.32987(12) 0.0454 1.0000 Uani . . . . . . C15 C 0.6426(4) 0.53975(18) 0.32828(10) 0.0362 1.0000 Uani . . . . . . C16 C 0.3662(4) 0.59258(17) 0.32852(9) 0.0298 1.0000 Uani . . . . . . C17 C 0.2298(4) 0.5869(2) 0.32847(10) 0.0371 1.0000 Uani . . . . . . C18 C 0.1514(4) 0.6115(2) 0.30095(11) 0.0470 1.0000 Uani . . . . . . C19 C 0.2072(4) 0.6416(2) 0.27223(10) 0.0480 1.0000 Uani . . . . . . C20 C 0.3418(5) 0.6481(2) 0.27217(10) 0.0466 1.0000 Uani . . . . . . C21 C 0.4209(4) 0.62550(19) 0.29994(10) 0.0374 1.0000 Uani . . . . . . C22 C 0.2396(4) 0.2866(2) 0.45610(12) 0.0482 1.0000 Uani . . . . . . C23 C 0.1232(4) 0.3328(2) 0.45006(11) 0.0450 1.0000 Uani . . . . . . C24 C 0.0683(4) 0.2847(2) 0.39220(12) 0.0450 1.0000 Uani . . . . . . C25 C 0.0823(4) 0.2969(2) 0.35322(11) 0.0442 1.0000 Uani . . . . . . C26 C 0.0108(4) 0.4013(2) 0.40496(11) 0.0403 1.0000 Uani . . . . . . C27 C 0.6478(4) 0.3263(3) 0.43687(13) 0.0727 1.0000 Uani . . . . . . C28 C 0.5011(6) 0.3248(3) 0.50354(11) 0.0619 1.0000 Uani . . . . . . C29 C 0.5169(5) 0.1975(2) 0.45890(13) 0.0555 1.0000 Uani . . . . . . C30 C 0.1853(5) 0.3036(2) 0.27310(12) 0.0574 1.0000 Uani . . . . . . C31 C 0.0568(4) 0.4314(2) 0.29731(12) 0.0488 1.0000 Uani . . . . . . C32 C 0.3523(4) 0.42299(19) 0.29915(9) 0.0334 1.0000 Uani . . . . . . C33 C 0.5853(3) 0.37477(18) 0.35853(9) 0.0292 1.0000 Uani . . . . . . C34 C 0.6941(4) 0.3543(2) 0.34052(10) 0.0361 1.0000 Uani . . . . . . C35 C 0.6992(4) 0.2886(2) 0.32832(10) 0.0379 1.0000 Uani . . . . . . C36 C 0.5961(4) 0.24552(19) 0.33407(10) 0.0345 1.0000 Uani . . . . . . C37 C 0.4911(3) 0.26927(18) 0.35200(9) 0.0303 1.0000 Uani . . . . . . H41 H 0.1173 0.5894 0.4267 0.0520 1.0000 Uiso R . . . . . H51 H 0.0256 0.6003 0.4832 0.0712 1.0000 Uiso R . . . . . H61 H 0.1262 0.5442 0.5325 0.0743 1.0000 Uiso R . . . . . H71 H 0.3151 0.4755 0.5255 0.0681 1.0000 Uiso R . . . . . H81 H 0.4047 0.4637 0.4687 0.0508 1.0000 Uiso R . . . . . H91 H 0.3300 0.6464 0.4277 0.0480 1.0000 Uiso R . . . . . H92 H 0.4657 0.6628 0.4078 0.0480 1.0000 Uiso R . . . . . H93 H 0.3239 0.6748 0.3873 0.0480 1.0000 Uiso R . . . . . H111 H 0.6012 0.5669 0.4128 0.0444 1.0000 Uiso R . . . . . H121 H 0.8318 0.5504 0.4151 0.0541 1.0000 Uiso R . . . . . H131 H 0.9467 0.5308 0.3626 0.0609 1.0000 Uiso R . . . . . H141 H 0.8251 0.5215 0.3078 0.0539 1.0000 Uiso R . . . . . H151 H 0.5924 0.5343 0.3054 0.0460 1.0000 Uiso R . . . . . H171 H 0.1886 0.5652 0.3491 0.0462 1.0000 Uiso R . . . . . H181 H 0.0538 0.6071 0.3017 0.0586 1.0000 Uiso R . . . . . H191 H 0.1512 0.6582 0.2518 0.0599 1.0000 Uiso R . . . . . H201 H 0.3832 0.6697 0.2515 0.0573 1.0000 Uiso R . . . . . H211 H 0.5180 0.6328 0.2999 0.0473 1.0000 Uiso R . . . . . H221 H 0.2668 0.2863 0.4816 0.0611 1.0000 Uiso R . . . . . H222 H 0.2154 0.2395 0.4484 0.0611 1.0000 Uiso R . . . . . H231 H 0.1391 0.3764 0.4630 0.0563 1.0000 Uiso R . . . . . H232 H 0.0420 0.3107 0.4587 0.0563 1.0000 Uiso R . . . . . H241 H -0.0248 0.2731 0.3970 0.0592 1.0000 Uiso R . . . . . H242 H 0.1269 0.2464 0.3999 0.0592 1.0000 Uiso R . . . . . H251 H 0.0019 0.3203 0.3434 0.0544 1.0000 Uiso R . . . . . H252 H 0.0939 0.2527 0.3408 0.0544 1.0000 Uiso R . . . . . H261 H 0.0019 0.4095 0.3790 0.0509 1.0000 Uiso R . . . . . H262 H 0.0420 0.4437 0.4170 0.0509 1.0000 Uiso R . . . . . H263 H -0.0764 0.3879 0.4141 0.0509 1.0000 Uiso R . . . . . H271 H 0.7274 0.3125 0.4513 0.0914 1.0000 Uiso R . . . . . H272 H 0.6422 0.3770 0.4360 0.0914 1.0000 Uiso R . . . . . H273 H 0.6540 0.3080 0.4124 0.0914 1.0000 Uiso R . . . . . H281 H 0.5869 0.3126 0.5155 0.0770 1.0000 Uiso R . . . . . H282 H 0.4906 0.3753 0.5033 0.0770 1.0000 Uiso R . . . . . H283 H 0.4278 0.3038 0.5166 0.0770 1.0000 Uiso R . . . . . H291 H 0.6017 0.1862 0.4716 0.0673 1.0000 Uiso R . . . . . H292 H 0.4425 0.1769 0.4716 0.0673 1.0000 Uiso R . . . . . H293 H 0.5177 0.1791 0.4344 0.0673 1.0000 Uiso R . . . . . H301 H 0.1868 0.3231 0.2488 0.0740 1.0000 Uiso R . . . . . H302 H 0.2602 0.2712 0.2767 0.0740 1.0000 Uiso R . . . . . H303 H 0.1006 0.2790 0.2761 0.0740 1.0000 Uiso R . . . . . H311 H 0.0611 0.4501 0.2729 0.0603 1.0000 Uiso R . . . . . H312 H 0.0591 0.4696 0.3146 0.0603 1.0000 Uiso R . . . . . H313 H -0.0266 0.4052 0.2995 0.0603 1.0000 Uiso R . . . . . H321 H 0.3503 0.4417 0.2747 0.0406 1.0000 Uiso R . . . . . H322 H 0.3585 0.4612 0.3165 0.0406 1.0000 Uiso R . . . . . H323 H 0.4303 0.3926 0.3026 0.0406 1.0000 Uiso R . . . . . H331 H 0.5820 0.4223 0.3678 0.0366 1.0000 Uiso R . . . . . H341 H 0.7672 0.3868 0.3363 0.0457 1.0000 Uiso R . . . . . H351 H 0.7773 0.2724 0.3155 0.0470 1.0000 Uiso R . . . . . H361 H 0.5975 0.1978 0.3251 0.0437 1.0000 Uiso R . . . . . H371 H 0.4166 0.2376 0.3562 0.0375 1.0000 Uiso R . . . . . Ti101 Ti 0.92917(6) 0.85310(3) 0.379456(16) 0.0258 1.0000 Uani . . . . . . N101 N 0.8849(3) 0.93861(14) 0.38311(7) 0.0272 1.0000 Uani . . . . . . N102 N 0.9214(3) 1.07222(14) 0.35243(7) 0.0298 1.0000 Uani . . . . . . N103 N 0.9944(3) 0.81662(15) 0.42613(8) 0.0368 1.0000 Uani . . . . . . N104 N 0.8672(3) 0.81478(14) 0.33288(8) 0.0328 1.0000 Uani . . . . . . N105 N 0.7642(3) 0.78215(15) 0.39428(8) 0.0374 1.0000 Uani . . . . . . N106 N 1.1314(3) 0.85865(14) 0.36065(7) 0.0300 1.0000 Uani . . . . . . Si101 Si 1.11261(12) 0.85035(6) 0.45470(3) 0.0421 1.0000 Uani . . . . . . Si102 Si 0.88031(10) 0.84909(5) 0.29134(3) 0.0302 1.0000 Uani . . . . . . C101 C 0.8256(3) 0.99632(17) 0.39503(9) 0.0272 1.0000 Uani . . . . . . C102 C 0.8427(3) 1.06030(17) 0.38280(9) 0.0299 1.0000 Uani . . . . . . C103 C 0.7266(3) 0.98304(18) 0.42227(9) 0.0311 1.0000 Uani . . . . . . C104 C 0.5940(4) 0.9945(2) 0.41397(12) 0.0477 1.0000 Uani . . . . . . C105 C 0.4986(4) 0.9759(3) 0.43716(15) 0.0618 1.0000 Uani . . . . . . C106 C 0.5340(5) 0.9467(2) 0.46894(14) 0.0587 1.0000 Uani . . . . . . C107 C 0.6650(5) 0.9363(3) 0.47779(12) 0.0569 1.0000 Uani . . . . . . C108 C 0.7600(4) 0.9538(2) 0.45435(10) 0.0438 1.0000 Uani . . . . . . C109 C 0.7820(4) 1.12323(19) 0.39754(11) 0.0427 1.0000 Uani . . . . . . C110 C 1.0572(3) 1.08517(17) 0.35665(10) 0.0309 1.0000 Uani . . . . . . C111 C 1.1125(4) 1.09473(18) 0.39087(10) 0.0371 1.0000 Uani . . . . . . C112 C 1.2466(4) 1.10489(19) 0.39524(13) 0.0501 1.0000 Uani . . . . . . C113 C 1.3275(4) 1.1061(2) 0.36716(14) 0.0533 1.0000 Uani . . . . . . C114 C 1.2740(4) 1.0959(2) 0.33347(13) 0.0500 1.0000 Uani . . . . . . C115 C 1.1399(4) 1.08488(18) 0.32830(10) 0.0376 1.0000 Uani . . . . . . C116 C 0.8488(4) 1.08691(17) 0.32087(9) 0.0300 1.0000 Uani . . . . . . C117 C 0.7358(4) 1.0493(2) 0.31296(11) 0.0411 1.0000 Uani . . . . . . C118 C 0.6599(4) 1.0630(2) 0.28253(12) 0.0511 1.0000 Uani . . . . . . C119 C 0.6976(5) 1.1142(2) 0.25949(11) 0.0510 1.0000 Uani . . . . . . C120 C 0.8074(4) 1.1517(2) 0.26780(10) 0.0429 1.0000 Uani . . . . . . C121 C 0.8827(4) 1.13938(18) 0.29828(9) 0.0338 1.0000 Uani . . . . . . C122 C 0.9342(5) 0.7531(2) 0.43791(13) 0.0610 1.0000 Uani . . . . . . C123 C 0.7945(6) 0.7556(3) 0.42913(17) 0.1041 1.0000 Uani . . . . . . C124 C 0.7676(8) 0.7300(3) 0.36811(14) 0.1025 1.0000 Uani . . . . . . C125 C 0.7870(5) 0.7532(2) 0.33283(12) 0.0602 1.0000 Uani . . . . . . C126 C 0.6351(5) 0.8146(3) 0.3938(2) 0.1009 1.0000 Uani . . . . . . C127 C 1.1346(4) 0.94288(19) 0.44855(11) 0.0397 1.0000 Uani . . . . . . C128 C 1.0672(7) 0.8384(3) 0.50161(12) 0.0873 1.0000 Uani . . . . . . C129 C 1.2749(5) 0.8086(3) 0.44809(16) 0.0794 1.0000 Uani . . . . . . C130 C 0.9624(4) 0.7870(2) 0.26219(11) 0.0431 1.0000 Uani . . . . . . C131 C 0.7143(4) 0.8673(2) 0.27076(11) 0.0495 1.0000 Uani . . . . . . C132 C 0.9785(4) 0.92924(18) 0.29179(9) 0.0340 1.0000 Uani . . . . . . C133 C 1.2035(4) 0.91497(19) 0.35758(10) 0.0349 1.0000 Uani . . . . . . C134 C 1.3253(4) 0.9145(2) 0.34302(11) 0.0459 1.0000 Uani . . . . . . C135 C 1.3754(4) 0.8544(2) 0.33080(11) 0.0491 1.0000 Uani . . . . . . C136 C 1.3023(4) 0.7960(2) 0.33413(11) 0.0450 1.0000 Uani . . . . . . C137 C 1.1822(4) 0.80014(19) 0.34908(10) 0.0388 1.0000 Uani . . . . . . H1041 H 0.5679 1.0165 0.3911 0.0593 1.0000 Uiso R . . . . . H1051 H 0.4037 0.9834 0.4307 0.0761 1.0000 Uiso R . . . . . H1061 H 0.4651 0.9331 0.4857 0.0725 1.0000 Uiso R . . . . . H1071 H 0.6914 0.9162 0.5011 0.0725 1.0000 Uiso R . . . . . H1081 H 0.8548 0.9451 0.4605 0.0551 1.0000 Uiso R . . . . . H1091 H 0.7294 1.1109 0.4183 0.0540 1.0000 Uiso R . . . . . H1092 H 0.8525 1.1561 0.4050 0.0540 1.0000 Uiso R . . . . . H1093 H 0.7232 1.1445 0.3790 0.0540 1.0000 Uiso R . . . . . H1111 H 1.0549 1.0943 0.4116 0.0460 1.0000 Uiso R . . . . . H1121 H 1.2859 1.1110 0.4195 0.0594 1.0000 Uiso R . . . . . H1131 H 1.4236 1.1150 0.3710 0.0662 1.0000 Uiso R . . . . . H1141 H 1.3325 1.0959 0.3129 0.0640 1.0000 Uiso R . . . . . H1151 H 1.1017 1.0765 0.3041 0.0482 1.0000 Uiso R . . . . . H1171 H 0.7103 1.0121 0.3293 0.0491 1.0000 Uiso R . . . . . H1181 H 0.5775 1.0366 0.2775 0.0611 1.0000 Uiso R . . . . . H1191 H 0.6453 1.1226 0.2372 0.0642 1.0000 Uiso R . . . . . H1201 H 0.8335 1.1888 0.2514 0.0518 1.0000 Uiso R . . . . . H1211 H 0.9611 1.1681 0.3044 0.0448 1.0000 Uiso R . . . . . H1221 H 0.9503 0.7477 0.4639 0.0791 1.0000 Uiso R . . . . . H1222 H 0.9736 0.7137 0.4254 0.0791 1.0000 Uiso R . . . . . H1231 H 0.7529 0.7859 0.4466 0.1474 1.0000 Uiso R . . . . . H1232 H 0.7563 0.7089 0.4307 0.1474 1.0000 Uiso R . . . . . H1241 H 0.8416 0.6986 0.3747 0.1385 1.0000 Uiso R . . . . . H1242 H 0.6827 0.7046 0.3685 0.1385 1.0000 Uiso R . . . . . H1251 H 0.6995 0.7633 0.3212 0.0753 1.0000 Uiso R . . . . . H1252 H 0.8323 0.7173 0.3192 0.0753 1.0000 Uiso R . . . . . H1261 H 0.6135 0.8335 0.3698 0.1343 1.0000 Uiso R . . . . . H1262 H 0.6368 0.8523 0.4114 0.1343 1.0000 Uiso R . . . . . H1263 H 0.5670 0.7806 0.4001 0.1343 1.0000 Uiso R . . . . . H1271 H 1.2038 0.9598 0.4657 0.0487 1.0000 Uiso R . . . . . H1272 H 1.0500 0.9668 0.4527 0.0487 1.0000 Uiso R . . . . . H1273 H 1.1621 0.9520 0.4240 0.0487 1.0000 Uiso R . . . . . H1281 H 1.1368 0.8583 0.5177 0.1083 1.0000 Uiso R . . . . . H1282 H 0.9819 0.8620 0.5053 0.1083 1.0000 Uiso R . . . . . H1283 H 1.0577 0.7889 0.5067 0.1083 1.0000 Uiso R . . . . . H1291 H 1.3430 0.8283 0.4647 0.0963 1.0000 Uiso R . . . . . H1292 H 1.3013 0.8162 0.4233 0.0963 1.0000 Uiso R . . . . . H1293 H 1.2669 0.7587 0.4525 0.0963 1.0000 Uiso R . . . . . H1301 H 0.9699 0.8070 0.2382 0.0569 1.0000 Uiso R . . . . . H1302 H 1.0521 0.7765 0.2723 0.0569 1.0000 Uiso R . . . . . H1303 H 0.9095 0.7443 0.2605 0.0569 1.0000 Uiso R . . . . . H1311 H 0.7244 0.8870 0.2468 0.0619 1.0000 Uiso R . . . . . H1312 H 0.6672 0.9005 0.2857 0.0619 1.0000 Uiso R . . . . . H1313 H 0.6627 0.8242 0.2688 0.0619 1.0000 Uiso R . . . . . H1321 H 0.9837 0.9471 0.2673 0.0436 1.0000 Uiso R . . . . . H1322 H 0.9354 0.9637 0.3068 0.0436 1.0000 Uiso R . . . . . H1323 H 1.0690 0.9197 0.3016 0.0436 1.0000 Uiso R . . . . . H1331 H 1.1672 0.9588 0.3663 0.0445 1.0000 Uiso R . . . . . H1341 H 1.3771 0.9575 0.3415 0.0559 1.0000 Uiso R . . . . . H1351 H 1.4626 0.8536 0.3195 0.0625 1.0000 Uiso R . . . . . H1361 H 1.3368 0.7515 0.3258 0.0568 1.0000 Uiso R . . . . . H1371 H 1.1295 0.7577 0.3516 0.0469 1.0000 Uiso 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 0.0245(3) 0.0216(3) 0.0237(3) -0.0009(3) 0.0033(2) -0.0004(3) N1 0.0255(15) 0.0244(15) 0.0233(15) -0.0015(11) 0.0069(12) -0.0022(12) N2 0.0293(16) 0.0284(15) 0.0256(15) 0.0027(12) 0.0038(13) -0.0020(13) N3 0.0345(17) 0.0302(16) 0.0322(17) 0.0103(13) 0.0035(14) 0.0000(13) N4 0.0259(15) 0.0308(16) 0.0339(16) -0.0067(13) 0.0018(13) -0.0041(13) N5 0.0296(16) 0.0269(16) 0.0364(17) 0.0032(13) 0.0073(13) -0.0003(13) N6 0.0276(15) 0.0212(15) 0.0252(15) 0.0015(11) 0.0005(12) 0.0027(12) Si1 0.0414(6) 0.0412(6) 0.0267(5) 0.0035(5) -0.0018(5) -0.0012(5) Si2 0.0306(5) 0.0412(6) 0.0275(5) -0.0108(4) -0.0027(4) 0.0026(5) C1 0.0229(17) 0.0256(18) 0.0232(17) -0.0003(14) -0.0015(14) 0.0008(14) C2 0.0330(19) 0.0271(19) 0.0216(17) 0.0004(14) 0.0047(15) -0.0009(15) C3 0.034(2) 0.0227(18) 0.0281(19) -0.0027(14) 0.0053(16) -0.0063(15) C4 0.041(2) 0.040(2) 0.039(2) -0.0036(18) 0.0111(19) 0.0020(18) C5 0.051(3) 0.057(3) 0.061(3) -0.013(2) 0.024(2) 0.001(2) C6 0.087(4) 0.062(3) 0.038(3) -0.013(2) 0.033(3) -0.011(3) C7 0.083(4) 0.051(3) 0.030(2) 0.005(2) 0.013(2) -0.010(3) C8 0.053(3) 0.038(2) 0.029(2) -0.0007(17) 0.0092(18) -0.0014(19) C9 0.052(2) 0.0244(19) 0.0330(19) 0.0026(16) 0.0077(17) -0.0052(17) C10 0.0301(19) 0.0226(18) 0.032(2) 0.0071(15) 0.0052(16) -0.0014(15) C11 0.041(2) 0.0275(19) 0.038(2) 0.0020(16) 0.0025(18) -0.0063(16) C12 0.039(2) 0.038(2) 0.053(3) 0.0088(19) -0.007(2) -0.0023(18) C13 0.033(2) 0.041(2) 0.071(3) 0.017(2) 0.007(2) 0.0078(19) C14 0.045(3) 0.037(2) 0.056(3) 0.017(2) 0.025(2) 0.0125(19) C15 0.039(2) 0.028(2) 0.042(2) 0.0093(17) 0.0092(19) 0.0072(17) C16 0.039(2) 0.0254(18) 0.0254(18) -0.0006(15) 0.0038(16) 0.0048(16) C17 0.039(2) 0.042(2) 0.030(2) 0.0064(17) -0.0008(17) -0.0028(18) C18 0.043(2) 0.052(3) 0.046(3) 0.002(2) -0.004(2) 0.002(2) C19 0.060(3) 0.048(2) 0.035(2) 0.001(2) -0.004(2) 0.020(2) C20 0.070(3) 0.042(2) 0.029(2) 0.0092(18) 0.014(2) 0.021(2) C21 0.044(2) 0.034(2) 0.034(2) 0.0068(16) 0.0119(18) 0.0086(17) C22 0.042(2) 0.055(3) 0.049(3) 0.021(2) 0.010(2) 0.000(2) C23 0.043(2) 0.051(3) 0.043(2) 0.0107(19) 0.013(2) -0.0008(19) C24 0.037(2) 0.035(2) 0.064(3) -0.003(2) 0.014(2) -0.0116(18) C25 0.038(2) 0.045(2) 0.050(3) -0.015(2) 0.0018(19) -0.0121(19) C26 0.028(2) 0.041(2) 0.053(3) 0.0033(19) 0.0077(19) 0.0045(17) C27 0.045(3) 0.122(5) 0.049(3) 0.025(3) -0.021(2) -0.029(3) C28 0.089(4) 0.062(3) 0.034(2) -0.004(2) -0.010(2) 0.008(3) C29 0.055(3) 0.052(3) 0.058(3) -0.001(2) -0.012(2) 0.018(2) C30 0.058(3) 0.069(3) 0.045(3) -0.032(2) 0.004(2) -0.008(2) C31 0.036(2) 0.058(3) 0.051(3) -0.001(2) -0.007(2) 0.006(2) C32 0.035(2) 0.041(2) 0.0250(18) -0.0002(16) 0.0025(16) 0.0055(17) C33 0.0279(19) 0.0266(19) 0.0332(19) 0.0000(15) 0.0023(16) 0.0007(15) C34 0.0287(19) 0.042(2) 0.038(2) 0.0032(18) 0.0056(16) 0.0030(18) C35 0.032(2) 0.046(2) 0.036(2) -0.0030(18) 0.0040(17) 0.0104(18) C36 0.039(2) 0.032(2) 0.033(2) -0.0062(16) 0.0012(17) 0.0106(17) C37 0.031(2) 0.0275(19) 0.032(2) 0.0039(15) -0.0015(16) 0.0021(15) Ti101 0.0303(3) 0.0223(3) 0.0247(3) 0.0013(3) -0.0006(3) -0.0014(3) N101 0.0303(16) 0.0244(15) 0.0270(15) 0.0013(12) 0.0029(13) 0.0001(12) N102 0.0339(17) 0.0274(16) 0.0278(16) 0.0037(13) -0.0014(13) -0.0032(13) N103 0.048(2) 0.0311(17) 0.0305(17) 0.0081(13) -0.0060(15) -0.0024(14) N104 0.0418(18) 0.0290(16) 0.0273(16) -0.0038(13) -0.0018(14) -0.0109(14) N105 0.0421(19) 0.0316(17) 0.0389(19) 0.0041(14) 0.0060(15) -0.0059(14) N106 0.0325(16) 0.0261(16) 0.0314(16) 0.0002(13) 0.0005(13) 0.0037(13) Si101 0.0533(7) 0.0387(6) 0.0331(6) 0.0034(5) -0.0130(5) 0.0026(5) Si102 0.0327(5) 0.0316(5) 0.0260(5) -0.0023(4) -0.0018(4) -0.0012(4) C101 0.0257(19) 0.0292(19) 0.0265(18) -0.0022(15) -0.0017(15) 0.0003(15) C102 0.035(2) 0.0271(19) 0.0274(19) -0.0021(15) 0.0005(16) 0.0021(15) C103 0.031(2) 0.0298(19) 0.033(2) -0.0022(15) 0.0085(16) 0.0005(16) C104 0.033(2) 0.053(3) 0.058(3) 0.008(2) 0.005(2) 0.0046(19) C105 0.032(2) 0.071(3) 0.084(4) 0.012(3) 0.016(2) 0.003(2) C106 0.046(3) 0.062(3) 0.070(3) -0.006(3) 0.032(3) -0.010(2) C107 0.056(3) 0.077(3) 0.039(3) 0.008(2) 0.017(2) -0.008(3) C108 0.034(2) 0.060(3) 0.038(2) 0.004(2) 0.0074(18) -0.0022(19) C109 0.055(3) 0.029(2) 0.044(2) -0.0005(17) 0.008(2) 0.0084(18) C110 0.034(2) 0.0196(17) 0.039(2) 0.0065(15) -0.0005(17) -0.0015(15) C111 0.042(2) 0.027(2) 0.042(2) 0.0012(17) -0.0066(18) -0.0026(17) C112 0.053(3) 0.029(2) 0.067(3) 0.007(2) -0.019(2) -0.0055(19) C113 0.037(2) 0.037(2) 0.085(4) 0.015(2) -0.012(3) -0.0071(18) C114 0.044(3) 0.037(2) 0.070(3) 0.017(2) 0.009(2) 0.0033(19) C115 0.041(2) 0.029(2) 0.043(2) 0.0101(17) -0.0003(19) 0.0028(17) C116 0.036(2) 0.0260(18) 0.0275(19) -0.0041(15) -0.0018(16) 0.0050(16) C117 0.043(2) 0.035(2) 0.046(2) -0.0014(18) -0.0058(19) -0.0003(18) C118 0.049(3) 0.043(2) 0.060(3) -0.018(2) -0.023(2) 0.007(2) C119 0.069(3) 0.046(3) 0.037(2) -0.009(2) -0.016(2) 0.022(2) C120 0.057(3) 0.042(2) 0.030(2) 0.0022(18) 0.0001(19) 0.016(2) C121 0.042(2) 0.0281(19) 0.0315(19) -0.0005(16) 0.0007(16) 0.0076(17) C122 0.087(4) 0.039(3) 0.056(3) 0.018(2) -0.021(3) -0.018(2) C123 0.107(5) 0.108(5) 0.095(5) 0.061(4) -0.029(4) -0.065(4) C124 0.181(7) 0.070(4) 0.060(4) -0.026(3) 0.049(4) -0.080(4) C125 0.091(4) 0.049(3) 0.040(3) -0.006(2) 0.000(2) -0.034(3) C126 0.048(3) 0.064(4) 0.192(8) 0.000(4) 0.022(4) -0.022(3) C127 0.034(2) 0.042(2) 0.043(2) -0.0037(18) -0.0040(18) -0.0009(18) C128 0.140(5) 0.090(4) 0.031(2) 0.013(3) -0.014(3) -0.045(4) C129 0.071(3) 0.064(3) 0.100(4) -0.028(3) -0.042(3) 0.031(3) C130 0.050(3) 0.039(2) 0.041(2) -0.0119(18) 0.006(2) -0.0066(19) C131 0.041(2) 0.056(3) 0.051(3) 0.006(2) -0.010(2) -0.001(2) C132 0.042(2) 0.031(2) 0.030(2) 0.0000(15) 0.0055(17) -0.0032(17) C133 0.034(2) 0.031(2) 0.039(2) 0.0024(16) -0.0020(17) 0.0028(16) C134 0.030(2) 0.051(3) 0.057(3) 0.008(2) 0.006(2) -0.0051(19) C135 0.033(2) 0.070(3) 0.045(2) 0.007(2) 0.0049(18) 0.015(2) C136 0.043(2) 0.049(3) 0.043(2) -0.005(2) 0.004(2) 0.018(2) C137 0.042(2) 0.031(2) 0.043(2) -0.0026(17) -0.0048(19) 0.0074(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . N1 . 1.757(3) yes Ti1 . N3 . 2.022(3) yes Ti1 . N4 . 2.005(3) yes Ti1 . N5 . 2.232(3) yes Ti1 . N6 . 2.199(3) yes N1 . C1 . 1.375(4) yes N2 . C2 . 1.442(4) yes N2 . C10 . 1.405(4) yes N2 . C16 . 1.416(4) yes N3 . Si1 . 1.728(3) yes N3 . C22 . 1.479(5) yes N4 . Si2 . 1.722(3) yes N4 . C25 . 1.471(5) yes N5 . C23 . 1.481(5) yes N5 . C24 . 1.473(5) yes N5 . C26 . 1.475(4) yes N6 . C33 . 1.337(4) yes N6 . C37 . 1.353(4) yes Si1 . C27 . 1.871(5) yes Si1 . C28 . 1.876(4) yes Si1 . C29 . 1.871(4) yes Si2 . C30 . 1.870(4) yes Si2 . C31 . 1.872(4) yes Si2 . C32 . 1.851(4) yes C1 . C2 . 1.349(5) yes C1 . C3 . 1.499(5) yes C2 . C9 . 1.507(5) yes C3 . C4 . 1.393(5) yes C3 . C8 . 1.380(5) yes C4 . C5 . 1.383(6) yes C4 . H41 . 1.000 no C5 . C6 . 1.376(7) yes C5 . H51 . 1.000 no C6 . C7 . 1.377(7) yes C6 . H61 . 1.000 no C7 . C8 . 1.384(5) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . C11 . 1.401(5) yes C10 . C15 . 1.400(5) yes C11 . C12 . 1.380(5) yes C11 . H111 . 1.000 no C12 . C13 . 1.380(6) yes C12 . H121 . 1.000 no C13 . C14 . 1.390(6) yes C13 . H131 . 1.000 no C14 . C15 . 1.386(5) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C16 . C17 . 1.394(5) yes C16 . C21 . 1.398(5) yes C17 . C18 . 1.380(5) yes C17 . H171 . 1.000 no C18 . C19 . 1.383(6) yes C18 . H181 . 1.000 no C19 . C20 . 1.378(6) yes C19 . H191 . 1.000 no C20 . C21 . 1.379(5) yes C20 . H201 . 1.000 no C21 . H211 . 1.000 no C22 . C23 . 1.504(6) yes C22 . H221 . 1.000 no C22 . H222 . 1.000 no C23 . H231 . 1.000 no C23 . H232 . 1.000 no C24 . C25 . 1.513(6) yes C24 . H241 . 1.000 no C24 . H242 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C26 . H261 . 1.000 no C26 . H262 . 1.000 no C26 . H263 . 1.000 no C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C28 . H281 . 1.000 no C28 . H282 . 1.000 no C28 . H283 . 1.000 no C29 . H291 . 1.000 no C29 . H292 . 1.000 no C29 . H293 . 1.000 no C30 . H301 . 1.000 no C30 . H302 . 1.000 no C30 . H303 . 1.000 no C31 . H311 . 1.000 no C31 . H312 . 1.000 no C31 . H313 . 1.000 no C32 . H321 . 1.000 no C32 . H322 . 1.000 no C32 . H323 . 1.000 no C33 . C34 . 1.383(5) yes C33 . H331 . 1.000 no C34 . C35 . 1.376(5) yes C34 . H341 . 1.000 no C35 . C36 . 1.374(5) yes C35 . H351 . 1.000 no C36 . C37 . 1.371(5) yes C36 . H361 . 1.000 no C37 . H371 . 1.000 no Ti101 . N101 . 1.750(3) yes Ti101 . N103 . 2.005(3) yes Ti101 . N104 . 2.006(3) yes Ti101 . N105 . 2.272(3) yes Ti101 . N106 . 2.208(3) yes N101 . C101 . 1.371(4) yes N102 . C102 . 1.448(5) yes N102 . C110 . 1.411(4) yes N102 . C116 . 1.417(4) yes N103 . Si101 . 1.726(3) yes N103 . C122 . 1.470(5) yes N104 . Si102 . 1.727(3) yes N104 . C125 . 1.462(5) yes N105 . C123 . 1.447(6) yes N105 . C124 . 1.431(6) yes N105 . C126 . 1.463(6) yes N106 . C133 . 1.338(5) yes N106 . C137 . 1.344(4) yes Si101 . C127 . 1.851(4) yes Si101 . C128 . 1.873(5) yes Si101 . C129 . 1.872(5) yes Si102 . C130 . 1.868(4) yes Si102 . C131 . 1.873(4) yes Si102 . C132 . 1.868(4) yes C101 . C102 . 1.356(5) yes C101 . C103 . 1.494(5) yes C102 . C109 . 1.502(5) yes C103 . C104 . 1.396(5) yes C103 . C108 . 1.380(5) yes C104 . C105 . 1.384(6) yes C104 . H1041 . 1.000 no C105 . C106 . 1.375(7) yes C105 . H1051 . 1.000 no C106 . C107 . 1.380(7) yes C106 . H1061 . 1.000 no C107 . C108 . 1.383(6) yes C107 . H1071 . 1.000 no C108 . H1081 . 1.000 no C109 . H1091 . 1.000 no C109 . H1092 . 1.000 no C109 . H1093 . 1.000 no C110 . C111 . 1.411(5) yes C110 . C115 . 1.392(5) yes C111 . C112 . 1.385(6) yes C111 . H1111 . 1.000 no C112 . C113 . 1.373(7) yes C112 . H1121 . 1.000 no C113 . C114 . 1.389(6) yes C113 . H1131 . 1.000 no C114 . C115 . 1.390(6) yes C114 . H1141 . 1.000 no C115 . H1151 . 1.000 no C116 . C117 . 1.393(5) yes C116 . C121 . 1.395(5) yes C117 . C118 . 1.395(5) yes C117 . H1171 . 1.000 no C118 . C119 . 1.397(6) yes C118 . H1181 . 1.000 no C119 . C120 . 1.369(6) yes C119 . H1191 . 1.000 no C120 . C121 . 1.388(5) yes C120 . H1201 . 1.000 no C121 . H1211 . 1.000 no C122 . C123 . 1.451(7) yes C122 . H1221 . 1.000 no C122 . H1222 . 1.000 no C123 . H1231 . 1.000 no C123 . H1232 . 1.000 no C124 . C125 . 1.437(7) yes C124 . H1241 . 1.000 no C124 . H1242 . 1.000 no C125 . H1251 . 1.000 no C125 . H1252 . 1.000 no C126 . H1261 . 1.000 no C126 . H1262 . 1.000 no C126 . H1263 . 1.000 no C127 . H1271 . 1.000 no C127 . H1272 . 1.000 no C127 . H1273 . 1.000 no C128 . H1281 . 1.000 no C128 . H1282 . 1.000 no C128 . H1283 . 1.000 no C129 . H1291 . 1.000 no C129 . H1292 . 1.000 no C129 . H1293 . 1.000 no C130 . H1301 . 1.000 no C130 . H1302 . 1.000 no C130 . H1303 . 1.000 no C131 . H1311 . 1.000 no C131 . H1312 . 1.000 no C131 . H1313 . 1.000 no C132 . H1321 . 1.000 no C132 . H1322 . 1.000 no C132 . H1323 . 1.000 no C133 . C134 . 1.377(5) yes C133 . H1331 . 1.000 no C134 . C135 . 1.375(6) yes C134 . H1341 . 1.000 no C135 . C136 . 1.379(6) yes C135 . H1351 . 1.000 no C136 . C137 . 1.370(6) yes C136 . H1361 . 1.000 no C137 . H1371 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ti1 . N3 . 114.44(12) yes N1 . Ti1 . N4 . 112.40(12) yes N3 . Ti1 . N4 . 131.06(12) yes N1 . Ti1 . N5 . 105.02(12) yes N3 . Ti1 . N5 . 78.34(11) yes N4 . Ti1 . N5 . 76.74(11) yes N1 . Ti1 . N6 . 101.31(11) yes N3 . Ti1 . N6 . 94.31(11) yes N4 . Ti1 . N6 . 89.81(11) yes N5 . Ti1 . N6 . 153.39(10) yes Ti1 . N1 . C1 . 161.8(2) yes C2 . N2 . C10 . 117.6(3) yes C2 . N2 . C16 . 115.2(3) yes C10 . N2 . C16 . 123.9(3) yes Ti1 . N3 . Si1 . 132.66(17) yes Ti1 . N3 . C22 . 117.7(2) yes Si1 . N3 . C22 . 109.5(2) yes Ti1 . N4 . Si2 . 129.34(16) yes Ti1 . N4 . C25 . 116.5(2) yes Si2 . N4 . C25 . 113.1(2) yes Ti1 . N5 . C23 . 107.8(2) yes Ti1 . N5 . C24 . 100.5(2) yes C23 . N5 . C24 . 111.4(3) yes Ti1 . N5 . C26 . 115.2(2) yes C23 . N5 . C26 . 111.0(3) yes C24 . N5 . C26 . 110.5(3) yes Ti1 . N6 . C33 . 124.2(2) yes Ti1 . N6 . C37 . 118.4(2) yes C33 . N6 . C37 . 117.4(3) yes N3 . Si1 . C27 . 115.61(18) yes N3 . Si1 . C28 . 111.3(2) yes C27 . Si1 . C28 . 105.8(2) yes N3 . Si1 . C29 . 109.29(18) yes C27 . Si1 . C29 . 106.4(3) yes C28 . Si1 . C29 . 108.1(2) yes N4 . Si2 . C30 . 109.2(2) yes N4 . Si2 . C31 . 111.03(18) yes C30 . Si2 . C31 . 106.4(2) yes N4 . Si2 . C32 . 112.03(15) yes C30 . Si2 . C32 . 109.90(19) yes C31 . Si2 . C32 . 108.15(19) yes N1 . C1 . C2 . 125.8(3) yes N1 . C1 . C3 . 114.9(3) yes C2 . C1 . C3 . 119.3(3) yes N2 . C2 . C1 . 120.3(3) yes N2 . C2 . C9 . 113.3(3) yes C1 . C2 . C9 . 126.3(3) yes C1 . C3 . C4 . 121.7(3) yes C1 . C3 . C8 . 119.8(3) yes C4 . C3 . C8 . 118.5(3) yes C3 . C4 . C5 . 120.6(4) yes C3 . C4 . H41 . 119.2 no C5 . C4 . H41 . 120.2 no C4 . C5 . C6 . 119.8(4) yes C4 . C5 . H51 . 119.8 no C6 . C5 . H51 . 120.4 no C5 . C6 . C7 . 120.5(4) yes C5 . C6 . H61 . 119.7 no C7 . C6 . H61 . 119.8 no C6 . C7 . C8 . 119.4(4) yes C6 . C7 . H71 . 120.1 no C8 . C7 . H71 . 120.4 no C7 . C8 . C3 . 121.2(4) yes C7 . C8 . H81 . 119.7 no C3 . C8 . H81 . 119.1 no C2 . C9 . H91 . 109.2 no C2 . C9 . H92 . 109.4 no H91 . C9 . H92 . 109.5 no C2 . C9 . H93 . 109.8 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N2 . C10 . C11 . 120.2(3) yes N2 . C10 . C15 . 122.2(3) yes C11 . C10 . C15 . 117.6(3) yes C10 . C11 . C12 . 121.3(4) yes C10 . C11 . H111 . 119.0 no C12 . C11 . H111 . 119.8 no C11 . C12 . C13 . 120.9(4) yes C11 . C12 . H121 . 119.7 no C13 . C12 . H121 . 119.4 no C12 . C13 . C14 . 118.5(4) yes C12 . C13 . H131 . 120.6 no C14 . C13 . H131 . 120.9 no C13 . C14 . C15 . 121.2(4) yes C13 . C14 . H141 . 119.1 no C15 . C14 . H141 . 119.7 no C10 . C15 . C14 . 120.4(4) yes C10 . C15 . H151 . 119.5 no C14 . C15 . H151 . 120.1 no N2 . C16 . C17 . 117.8(3) yes N2 . C16 . C21 . 124.7(3) yes C17 . C16 . C21 . 117.5(3) yes C16 . C17 . C18 . 121.5(4) yes C16 . C17 . H171 . 118.7 no C18 . C17 . H171 . 119.8 no C17 . C18 . C19 . 120.4(4) yes C17 . C18 . H181 . 119.9 no C19 . C18 . H181 . 119.7 no C18 . C19 . C20 . 118.6(4) yes C18 . C19 . H191 . 120.8 no C20 . C19 . H191 . 120.6 no C19 . C20 . C21 . 121.5(4) yes C19 . C20 . H201 . 119.3 no C21 . C20 . H201 . 119.2 no C16 . C21 . C20 . 120.4(4) yes C16 . C21 . H211 . 119.3 no C20 . C21 . H211 . 120.3 no N3 . C22 . C23 . 109.2(3) yes N3 . C22 . H221 . 109.2 no C23 . C22 . H221 . 110.0 no N3 . C22 . H222 . 109.7 no C23 . C22 . H222 . 109.3 no H221 . C22 . H222 . 109.5 no C22 . C23 . N5 . 108.6(3) yes C22 . C23 . H231 . 109.4 no N5 . C23 . H231 . 109.6 no C22 . C23 . H232 . 110.2 no N5 . C23 . H232 . 109.6 no H231 . C23 . H232 . 109.5 no N5 . C24 . C25 . 109.5(3) yes N5 . C24 . H241 . 109.6 no C25 . C24 . H241 . 109.8 no N5 . C24 . H242 . 109.2 no C25 . C24 . H242 . 109.3 no H241 . C24 . H242 . 109.5 no C24 . C25 . N4 . 109.4(3) yes C24 . C25 . H251 . 109.4 no N4 . C25 . H251 . 109.2 no C24 . C25 . H252 . 110.1 no N4 . C25 . H252 . 109.2 no H251 . C25 . H252 . 109.5 no N5 . C26 . H261 . 109.2 no N5 . C26 . H262 . 109.4 no H261 . C26 . H262 . 109.5 no N5 . C26 . H263 . 109.8 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no Si1 . C27 . H271 . 109.8 no Si1 . C27 . H272 . 109.1 no H271 . C27 . H272 . 109.5 no Si1 . C27 . H273 . 109.5 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no Si1 . C28 . H281 . 109.5 no Si1 . C28 . H282 . 109.6 no H281 . C28 . H282 . 109.5 no Si1 . C28 . H283 . 109.3 no H281 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no Si1 . C29 . H291 . 109.3 no Si1 . C29 . H292 . 109.7 no H291 . C29 . H292 . 109.5 no Si1 . C29 . H293 . 109.5 no H291 . C29 . H293 . 109.5 no H292 . C29 . H293 . 109.5 no Si2 . C30 . H301 . 109.4 no Si2 . C30 . H302 . 109.6 no H301 . C30 . H302 . 109.5 no Si2 . C30 . H303 . 109.4 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no Si2 . C31 . H311 . 109.1 no Si2 . C31 . H312 . 109.7 no H311 . C31 . H312 . 109.5 no Si2 . C31 . H313 . 109.6 no H311 . C31 . H313 . 109.5 no H312 . C31 . H313 . 109.5 no Si2 . C32 . H321 . 109.6 no Si2 . C32 . H322 . 109.4 no H321 . C32 . H322 . 109.5 no Si2 . C32 . H323 . 109.4 no H321 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no N6 . C33 . C34 . 122.8(3) yes N6 . C33 . H331 . 118.3 no C34 . C33 . H331 . 118.9 no C33 . C34 . C35 . 118.8(4) yes C33 . C34 . H341 . 120.4 no C35 . C34 . H341 . 120.8 no C34 . C35 . C36 . 119.2(3) yes C34 . C35 . H351 . 120.2 no C36 . C35 . H351 . 120.5 no C35 . C36 . C37 . 118.9(3) yes C35 . C36 . H361 . 120.3 no C37 . C36 . H361 . 120.8 no C36 . C37 . N6 . 122.9(3) yes C36 . C37 . H371 . 118.6 no N6 . C37 . H371 . 118.5 no N101 . Ti101 . N103 . 110.66(13) yes N101 . Ti101 . N104 . 110.97(13) yes N103 . Ti101 . N104 . 136.91(12) yes N101 . Ti101 . N105 . 112.12(12) yes N103 . Ti101 . N105 . 77.59(12) yes N104 . Ti101 . N105 . 77.01(12) yes N101 . Ti101 . N106 . 102.97(12) yes N103 . Ti101 . N106 . 91.18(12) yes N104 . Ti101 . N106 . 90.05(12) yes N105 . Ti101 . N106 . 144.90(11) yes Ti101 . N101 . C101 . 160.3(2) yes C102 . N102 . C110 . 120.5(3) yes C102 . N102 . C116 . 114.9(3) yes C110 . N102 . C116 . 122.7(3) yes Ti101 . N103 . Si101 . 128.36(17) yes Ti101 . N103 . C122 . 116.5(2) yes Si101 . N103 . C122 . 115.2(3) yes Ti101 . N104 . Si102 . 128.88(16) yes Ti101 . N104 . C125 . 118.1(2) yes Si102 . N104 . C125 . 112.6(2) yes Ti101 . N105 . C123 . 108.3(3) yes Ti101 . N105 . C124 . 103.4(3) yes C123 . N105 . C124 . 111.5(5) yes Ti101 . N105 . C126 . 113.7(3) yes C123 . N105 . C126 . 109.4(5) yes C124 . N105 . C126 . 110.4(5) yes Ti101 . N106 . C133 . 126.3(2) yes Ti101 . N106 . C137 . 116.0(2) yes C133 . N106 . C137 . 117.6(3) yes N103 . Si101 . C127 . 112.61(16) yes N103 . Si101 . C128 . 111.1(2) yes C127 . Si101 . C128 . 106.2(2) yes N103 . Si101 . C129 . 110.3(2) yes C127 . Si101 . C129 . 107.7(2) yes C128 . Si101 . C129 . 108.8(3) yes N104 . Si102 . C130 . 109.72(17) yes N104 . Si102 . C131 . 111.00(18) yes C130 . Si102 . C131 . 107.2(2) yes N104 . Si102 . C132 . 112.39(15) yes C130 . Si102 . C132 . 107.88(17) yes C131 . Si102 . C132 . 108.50(19) yes N101 . C101 . C102 . 126.4(3) yes N101 . C101 . C103 . 113.6(3) yes C102 . C101 . C103 . 119.9(3) yes N102 . C102 . C101 . 120.4(3) yes N102 . C102 . C109 . 114.3(3) yes C101 . C102 . C109 . 125.3(3) yes C101 . C103 . C104 . 119.2(3) yes C101 . C103 . C108 . 122.3(3) yes C104 . C103 . C108 . 118.2(4) yes C103 . C104 . C105 . 120.7(4) yes C103 . C104 . H1041 . 119.4 no C105 . C104 . H1041 . 119.9 no C104 . C105 . C106 . 120.1(4) yes C104 . C105 . H1051 . 120.1 no C106 . C105 . H1051 . 119.8 no C105 . C106 . C107 . 119.8(4) yes C105 . C106 . H1061 . 120.2 no C107 . C106 . H1061 . 120.0 no C106 . C107 . C108 . 120.0(4) yes C106 . C107 . H1071 . 120.1 no C108 . C107 . H1071 . 119.9 no C107 . C108 . C103 . 121.1(4) yes C107 . C108 . H1081 . 120.0 no C103 . C108 . H1081 . 118.9 no C102 . C109 . H1091 . 109.5 no C102 . C109 . H1092 . 109.7 no H1091 . C109 . H1092 . 109.5 no C102 . C109 . H1093 . 109.2 no H1091 . C109 . H1093 . 109.5 no H1092 . C109 . H1093 . 109.5 no N102 . C110 . C111 . 119.1(3) yes N102 . C110 . C115 . 122.0(3) yes C111 . C110 . C115 . 118.8(3) yes C110 . C111 . C112 . 119.3(4) yes C110 . C111 . H1111 . 120.0 no C112 . C111 . H1111 . 120.7 no C111 . C112 . C113 . 121.8(4) yes C111 . C112 . H1121 . 119.3 no C113 . C112 . H1121 . 118.9 no C112 . C113 . C114 . 119.1(4) yes C112 . C113 . H1131 . 120.1 no C114 . C113 . H1131 . 120.7 no C113 . C114 . C115 . 120.3(4) yes C113 . C114 . H1141 . 119.7 no C115 . C114 . H1141 . 120.0 no C110 . C115 . C114 . 120.6(4) yes C110 . C115 . H1151 . 119.1 no C114 . C115 . H1151 . 120.3 no N102 . C116 . C117 . 118.5(3) yes N102 . C116 . C121 . 122.6(3) yes C117 . C116 . C121 . 118.9(3) yes C116 . C117 . C118 . 120.4(4) yes C116 . C117 . H1171 . 119.1 no C118 . C117 . H1171 . 120.5 no C117 . C118 . C119 . 120.2(4) yes C117 . C118 . H1181 . 119.8 no C119 . C118 . H1181 . 120.0 no C118 . C119 . C120 . 119.1(4) yes C118 . C119 . H1191 . 120.2 no C120 . C119 . H1191 . 120.8 no C119 . C120 . C121 . 121.4(4) yes C119 . C120 . H1201 . 118.9 no C121 . C120 . H1201 . 119.7 no C116 . C121 . C120 . 120.1(4) yes C116 . C121 . H1211 . 119.3 no C120 . C121 . H1211 . 120.6 no N103 . C122 . C123 . 108.5(4) yes N103 . C122 . H1221 . 109.5 no C123 . C122 . H1221 . 110.8 no N103 . C122 . H1222 . 109.6 no C123 . C122 . H1222 . 108.9 no H1221 . C122 . H1222 . 109.5 no C122 . C123 . N105 . 113.5(5) yes C122 . C123 . H1231 . 107.7 no N105 . C123 . H1231 . 108.0 no C122 . C123 . H1232 . 109.6 no N105 . C123 . H1232 . 108.5 no H1231 . C123 . H1232 . 109.5 no N105 . C124 . C125 . 115.3(4) yes N105 . C124 . H1241 . 107.8 no C125 . C124 . H1241 . 107.6 no N105 . C124 . H1242 . 107.8 no C125 . C124 . H1242 . 108.7 no H1241 . C124 . H1242 . 109.5 no N104 . C125 . C124 . 111.0(4) yes N104 . C125 . H1251 . 109.0 no C124 . C125 . H1251 . 109.0 no N104 . C125 . H1252 . 108.6 no C124 . C125 . H1252 . 109.8 no H1251 . C125 . H1252 . 109.5 no N105 . C126 . H1261 . 110.0 no N105 . C126 . H1262 . 108.8 no H1261 . C126 . H1262 . 109.5 no N105 . C126 . H1263 . 109.6 no H1261 . C126 . H1263 . 109.5 no H1262 . C126 . H1263 . 109.5 no Si101 . C127 . H1271 . 109.3 no Si101 . C127 . H1272 . 109.5 no H1271 . C127 . H1272 . 109.5 no Si101 . C127 . H1273 . 109.5 no H1271 . C127 . H1273 . 109.5 no H1272 . C127 . H1273 . 109.5 no Si101 . C128 . H1281 . 109.9 no Si101 . C128 . H1282 . 108.8 no H1281 . C128 . H1282 . 109.5 no Si101 . C128 . H1283 . 109.7 no H1281 . C128 . H1283 . 109.5 no H1282 . C128 . H1283 . 109.5 no Si101 . C129 . H1291 . 109.9 no Si101 . C129 . H1292 . 109.2 no H1291 . C129 . H1292 . 109.5 no Si101 . C129 . H1293 . 109.3 no H1291 . C129 . H1293 . 109.5 no H1292 . C129 . H1293 . 109.5 no Si102 . C130 . H1301 . 109.5 no Si102 . C130 . H1302 . 109.3 no H1301 . C130 . H1302 . 109.5 no Si102 . C130 . H1303 . 109.6 no H1301 . C130 . H1303 . 109.5 no H1302 . C130 . H1303 . 109.5 no Si102 . C131 . H1311 . 109.5 no Si102 . C131 . H1312 . 109.4 no H1311 . C131 . H1312 . 109.5 no Si102 . C131 . H1313 . 109.4 no H1311 . C131 . H1313 . 109.5 no H1312 . C131 . H1313 . 109.5 no Si102 . C132 . H1321 . 109.6 no Si102 . C132 . H1322 . 109.4 no H1321 . C132 . H1322 . 109.5 no Si102 . C132 . H1323 . 109.4 no H1321 . C132 . H1323 . 109.5 no H1322 . C132 . H1323 . 109.5 no N106 . C133 . C134 . 122.4(4) yes N106 . C133 . H1331 . 118.5 no C134 . C133 . H1331 . 119.2 no C133 . C134 . C135 . 119.5(4) yes C133 . C134 . H1341 . 120.2 no C135 . C134 . H1341 . 120.3 no C134 . C135 . C136 . 118.5(4) yes C134 . C135 . H1351 . 120.3 no C136 . C135 . H1351 . 121.1 no C135 . C136 . C137 . 118.8(4) yes C135 . C136 . H1361 . 120.3 no C137 . C136 . H1361 . 120.9 no C136 . C137 . N106 . 123.2(4) yes C136 . C137 . H1371 . 118.8 no N106 . C137 . H1371 . 118.0 no _chemical_name_common Ti(MeN(CH2CH2SiMe3)2)(NC(Ph)C(Me)NPh2)(py) ##end data_Compound_10 _database_code_depnum_ccdc_archive 'CCDC 656396' # Local code adscw53 _chemical_name_systematic ; Cp*Ti{MeC(NiPr)2}{NNMe2) ; _chemical_melting_point ? _cell_length_a 9.3311(2) _cell_length_b 14.7945(4) _cell_length_c 16.4429(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2269.93(10) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b n m ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 -x,-y,z+1/2 x,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C20 H38 N4 Ti1' _chemical_formula_moiety 'C20 H38 N4 Ti1' _chemical_compound_source ? _chemical_formula_weight 382.45 _cell_measurement_reflns_used 2833 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_meas ? _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.94 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 5047 _reflns_number_total 2663 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_min 5.119 _diffrn_reflns_theta_max 27.477 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.653 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 2.21 _oxford_diffrn_Wilson_scale 1.07 _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.30 _refine_diff_density_max 0.30 _refine_ls_number_reflns 2192 _refine_ls_number_restraints 2 _refine_ls_number_parameters 126 _refine_ls_wR_factor_ref 0.0459 _refine_ls_goodness_of_fit_ref 0.9446 _refine_ls_R_factor_all 0.0472 _refine_ls_wR_factor_all 0.0492 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 2192 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_gt 0.0459 _refine_ls_shift/su_max 0.003 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.56 0.679 1.00 0.207E-01 ; _publ_section_exptl_refinement ; No special details ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.10366(3) 0.40557(2) 0.7500 0.0227 1.0000 Uani S T . . . . N1 N -0.01520(17) 0.31642(11) 0.7500 0.0261 1.0000 Uani S T . . . . N2 N -0.14456(18) 0.27032(12) 0.7500 0.0342 1.0000 Uani S T . . . . N3 N 0.28595(13) 0.37078(9) 0.68188(8) 0.0316 1.0000 Uani . . . . . . C1 C -0.1601(2) 0.21667(14) 0.67593(15) 0.0578 1.0000 Uani . . . . . . C2 C -0.06997(17) 0.51075(10) 0.70678(13) 0.0434 1.0000 Uani . . . . . . C3 C 0.06335(19) 0.54617(10) 0.68048(10) 0.0365 1.0000 Uani . . . . . . C4 C 0.1460(2) 0.56734(14) 0.7500 0.0312 1.0000 Uani S T . . . . C5 C -0.1921(3) 0.48068(14) 0.6532(2) 0.0805 1.0000 Uani . . . . . . C6 C 0.1055(3) 0.56387(14) 0.59384(12) 0.0629 1.0000 Uani . . . . . . C7 C 0.2959(3) 0.60446(17) 0.750000(7) 0.0468 1.0000 Uani S T . . . . C8 C 0.3540(2) 0.34740(14) 0.7500 0.0321 1.0000 Uani S T . . . . C9 C 0.4944(2) 0.29618(17) 0.750000(7) 0.0455 1.0000 Uani S T . . . . C10 C 0.3294(2) 0.33425(13) 0.60251(11) 0.0456 1.0000 Uani . . . . . . C11 C 0.4240(3) 0.4018(2) 0.55586(16) 0.0694 1.0000 Uani . . . . . . C12 C 0.1959(2) 0.30977(16) 0.55479(12) 0.0569 1.0000 Uani . . . . . . H11 H -0.2538 0.1838 0.6769 0.0709 1.0000 Uiso R . . . . . H12 H -0.0800 0.1720 0.6722 0.0709 1.0000 Uiso R . . . . . H13 H -0.1570 0.2579 0.6278 0.0709 1.0000 Uiso R . . . . . H51 H -0.1646 0.4875 0.5948 0.1006 1.0000 Uiso R . . . . . H52 H -0.2783 0.5186 0.6648 0.1006 1.0000 Uiso R . . . . . H53 H -0.2145 0.4159 0.6648 0.1006 1.0000 Uiso R . . . . . H61 H 0.2050 0.5889 0.5926 0.0784 1.0000 Uiso R . . . . . H62 H 0.0378 0.6085 0.5690 0.0784 1.0000 Uiso R . . . . . H63 H 0.1023 0.5061 0.5623 0.0784 1.0000 Uiso R . . . . . H101 H 0.3857 0.2778 0.6121 0.0563 1.0000 Uiso R . . . . . H111 H 0.4533 0.3754 0.5024 0.0851 1.0000 Uiso R . . . . . H112 H 0.5113 0.4156 0.5888 0.0851 1.0000 Uiso R . . . . . H113 H 0.3685 0.4587 0.5464 0.0851 1.0000 Uiso R . . . . . H121 H 0.2236 0.2840 0.5008 0.0684 1.0000 Uiso R . . . . . H122 H 0.1375 0.3657 0.5464 0.0684 1.0000 Uiso R . . . . . H123 H 0.1383 0.2643 0.5857 0.0684 1.0000 Uiso R . . . . . H92 H 0.5493 0.3142 0.7997 0.0539 0.5000 Uiso R . . . . . H91 H 0.4765 0.2295 0.7500 0.0539 0.5000 Uiso RS . . . . . H71 H 0.2925 0.6720 0.7500 0.0555 1.0000 Uiso RS . . . . . H72 H 0.3476 0.5830 0.7997 0.0555 0.5000 Uiso 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 0.01976(18) 0.02063(18) 0.02777(18) 0.0000 0.0000 -0.00007(12) N1 0.0210(7) 0.0214(8) 0.0360(8) 0.0000 0.0000 -0.0003(6) N2 0.0214(8) 0.0257(8) 0.0554(11) 0.0000 0.0000 -0.0033(6) N3 0.0260(6) 0.0329(6) 0.0358(7) -0.0007(5) 0.0063(5) -0.0005(5) C1 0.0318(8) 0.0493(11) 0.0924(16) -0.0339(11) -0.0104(9) -0.0033(7) C2 0.0327(7) 0.0221(7) 0.0755(12) 0.0034(7) -0.0168(8) 0.0031(6) C3 0.0455(8) 0.0226(6) 0.0415(9) 0.0034(6) -0.0076(7) 0.0009(6) C4 0.0304(10) 0.0229(9) 0.0403(11) 0.0000 0.0000 -0.0038(7) C5 0.0587(12) 0.0351(9) 0.148(3) 0.0081(13) -0.0627(16) 0.0004(9) C6 0.114(2) 0.0371(9) 0.0378(9) 0.0094(8) -0.0096(11) -0.0045(11) C7 0.0350(12) 0.0341(11) 0.0714(17) 0.0000 0.0000 -0.0129(10) C8 0.0202(8) 0.0242(9) 0.0518(13) 0.0000 0.0000 -0.0019(7) C9 0.0215(9) 0.0363(12) 0.0786(18) 0.0000 0.0000 0.0038(9) C10 0.0404(9) 0.0513(10) 0.0452(9) -0.0074(8) 0.0167(8) 0.0003(8) C11 0.0557(12) 0.0956(19) 0.0568(12) 0.0010(12) 0.0288(10) -0.0151(12) C12 0.0600(12) 0.0691(13) 0.0416(9) -0.0179(9) 0.0099(9) -0.0075(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.002(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . N1 . 1.7233(17) yes Ti1 . N3 . 2.1006(12) yes Ti1 . C2 . 2.3561(15) yes Ti1 . C3 . 2.4031(15) yes Ti1 . C4 . 2.426(2) yes Ti1 . C8 . 2.489(2) yes N1 . N2 . 1.386(2) yes N2 . C1 . 1.461(2) yes N3 . C8 . 1.3331(17) yes N3 . C10 . 1.470(2) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . C2 8_556 1.421(4) yes C2 . C3 . 1.417(3) yes C2 . C5 . 1.507(3) yes C3 . C4 . 1.414(2) yes C3 . C6 . 1.501(3) yes C4 . C7 . 1.502(3) yes C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . H61 . 1.000 no C6 . H62 . 1.000 no C6 . H63 . 1.000 no C7 . H72 8_556 1.000 no C7 . H71 . 1.000 no C7 . H72 . 1.000 no C8 . C9 . 1.514(3) yes C9 . H92 8_556 1.000 no C9 . H92 . 1.000 no C9 . H91 . 1.000 no C10 . C11 . 1.538(3) yes C10 . C12 . 1.516(3) yes C10 . H101 . 1.000 no C11 . H111 . 1.000 no C11 . H112 . 1.000 no C11 . H113 . 1.000 no C12 . H121 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 8_556 Ti1 . C3 8_556 34.64(6) yes C2 8_556 Ti1 . N3 8_556 123.90(6) yes C3 8_556 Ti1 . N3 8_556 94.88(6) yes C2 8_556 Ti1 . N1 . 93.61(6) yes C3 8_556 Ti1 . N1 . 124.18(6) yes N3 8_556 Ti1 . N1 . 109.49(6) yes C2 8_556 Ti1 . N3 . 151.58(6) yes C3 8_556 Ti1 . N3 . 126.33(6) yes N3 8_556 Ti1 . N3 . 64.45(7) yes N1 . Ti1 . N3 . 109.49(6) yes C2 8_556 Ti1 . C2 . 35.11(11) yes C3 8_556 Ti1 . C2 . 57.60(6) yes N3 8_556 Ti1 . C2 . 151.58(6) yes N1 . Ti1 . C2 . 93.61(6) yes N3 . Ti1 . C2 . 123.90(6) yes C2 8_556 Ti1 . C3 . 57.60(6) yes C3 8_556 Ti1 . C3 . 56.81(8) yes N3 8_556 Ti1 . C3 . 126.33(6) yes N1 . Ti1 . C3 . 124.18(6) yes N3 . Ti1 . C3 . 94.88(6) yes C2 8_556 Ti1 . C4 . 57.35(6) yes C3 8_556 Ti1 . C4 . 34.06(5) yes N3 8_556 Ti1 . C4 . 96.30(6) yes N1 . Ti1 . C4 . 149.32(8) yes N3 . Ti1 . C4 . 96.30(6) yes C2 8_556 Ti1 . C8 . 150.88(6) yes C3 8_556 Ti1 . C8 . 116.50(6) yes N3 8_556 Ti1 . C8 . 32.38(4) yes N1 . Ti1 . C8 . 109.83(7) yes N3 . Ti1 . C8 . 32.38(4) yes C2 . Ti1 . C3 . 34.64(6) yes C2 . Ti1 . C4 . 57.35(6) yes C3 . Ti1 . C4 . 34.06(5) yes C2 . Ti1 . C8 . 150.88(6) yes C3 . Ti1 . C8 . 116.50(6) yes C4 . Ti1 . C8 . 100.85(7) yes Ti1 . N1 . N2 . 159.53(14) yes C1 8_556 N2 . N1 . 110.71(12) yes C1 8_556 N2 . C1 . 112.9(2) yes N1 . N2 . C1 . 110.71(12) yes Ti1 . N3 . C8 . 90.06(10) yes Ti1 . N3 . C10 . 141.89(11) yes C8 . N3 . C10 . 121.30(14) yes N2 . C1 . H11 . 109.7 no N2 . C1 . H12 . 109.6 no H11 . C1 . H12 . 109.5 no N2 . C1 . H13 . 109.0 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no Ti1 . C2 . C2 8_556 72.44(5) yes Ti1 . C2 . C3 . 74.49(9) yes C2 8_556 C2 . C3 . 107.76(11) yes Ti1 . C2 . C5 . 120.08(12) yes C2 8_556 C2 . C5 . 125.75(17) yes C3 . C2 . C5 . 126.5(2) yes Ti1 . C3 . C2 . 70.87(9) yes Ti1 . C3 . C4 . 73.85(10) yes C2 . C3 . C4 . 108.30(16) yes Ti1 . C3 . C6 . 124.17(13) yes C2 . C3 . C6 . 125.73(18) yes C4 . C3 . C6 . 125.86(17) yes Ti1 . C4 . C3 8_556 72.10(10) yes Ti1 . C4 . C3 . 72.10(10) yes C3 8_556 C4 . C3 . 107.9(2) yes Ti1 . C4 . C7 . 120.83(15) yes C3 8_556 C4 . C7 . 126.07(10) yes C3 . C4 . C7 . 126.07(10) yes C2 . C5 . H51 . 109.8 no C2 . C5 . H52 . 109.4 no H51 . C5 . H52 . 109.5 no C2 . C5 . H53 . 109.3 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no C3 . C6 . H61 . 109.1 no C3 . C6 . H62 . 109.7 no H61 . C6 . H62 . 109.5 no C3 . C6 . H63 . 109.6 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no C4 . C7 . H72 8_556 109.4 no C4 . C7 . H71 . 109.7 no H72 8_556 C7 . H71 . 109.4 no C4 . C7 . H72 . 109.4 no H72 8_556 C7 . H72 . 109.5 no H71 . C7 . H72 . 109.4 no Ti1 . C8 . N3 8_556 57.56(9) yes Ti1 . C8 . N3 . 57.56(9) yes N3 8_556 C8 . N3 . 114.33(18) yes Ti1 . C8 . C9 . 170.19(16) yes N3 8_556 C8 . C9 . 122.82(9) yes N3 . C8 . C9 . 122.82(9) yes C8 . C9 . H92 8_556 108.1 no C8 . C9 . H92 . 108.1 no H92 8_556 C9 . H92 . 109.5 no C8 . C9 . H91 . 110.4 no H92 8_556 C9 . H91 . 110.4 no H92 . C9 . H91 . 110.4 no N3 . C10 . C11 . 111.24(16) yes N3 . C10 . C12 . 108.74(14) yes C11 . C10 . C12 . 111.63(19) yes N3 . C10 . H101 . 108.2 no C11 . C10 . H101 . 108.6 no C12 . C10 . H101 . 108.3 no C10 . C11 . H111 . 110.0 no C10 . C11 . H112 . 109.3 no H111 . C11 . H112 . 109.5 no C10 . C11 . H113 . 109.1 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no C10 . C12 . H121 . 109.8 no C10 . C12 . H122 . 108.8 no H121 . C12 . H122 . 109.5 no C10 . C12 . H123 . 109.9 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no _chemical_name_common Cp*Ti(MeC(NiPr)2)(NNMe2)