# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Philip Mountford' 'Eric Clot' 'Cameron Jones' 'Christian Schulten' 'Andrew D Schwarz' 'Jonathan D Selby' 'Andreas Stasch' _publ_contact_author_name 'Philip Mountford' _publ_contact_author_email PHILIP.MOUNTFORD@CHEMISTRY.OXFORD.AC.UK _publ_section_title ; Cycloaddition reactions of transition metal hydrazides with alkynes and heteroalkynes: coupling of Ti=NNPh2 with PhCCMe, PhCCH, MeCN and tBuCP ; # Attachment 'B813911C_Xray_ESI.cif' data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 698353' _audit_creation_method CRYSTALS_ver_12.84 _chemical_name_systematic ; Ti(N2Npy)(py)(NC(Ph)C(Me)NPh2) . 0.5(Et2O) ; _publ_section_exptl_refinement ; No special details ; _chemical_melting_point ? _cell_length_a 39.2342(10) _cell_length_b 10.6636(3) _cell_length_c 20.7574(6) _cell_angle_alpha 90 _cell_angle_beta 102.0841(15) _cell_angle_gamma 90 _cell_volume 8492.0(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 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 -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -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' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C43 H57 N6 O0.50 Si2 Ti1' _chemical_formula_moiety 'C41 H52 N6 Si2 Ti1 . 0.5 (C4 H10 O)' _chemical_compound_source ? _chemical_formula_weight 770.04 _cell_measurement_reflns_used 7729 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.60 _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_meas ? _exptl_crystal_F_000 3288 _exptl_absorpt_coefficient_mu 0.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.99 _exptl_absorpt_correction_T_max 0.99 _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 13456 _reflns_number_total 7683 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_theta_min 5.113 _diffrn_reflns_theta_max 25.356 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.356 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -47 _reflns_limit_h_max 46 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 2.27 _oxford_diffrn_Wilson_scale 49.45 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.32 _refine_diff_density_max 0.42 _refine_ls_number_reflns 4782 _refine_ls_number_restraints 0 _refine_ls_number_parameters 474 _refine_ls_wR_factor_ref 0.0431 _refine_ls_goodness_of_fit_ref 1.1169 _refine_ls_R_factor_all 0.0847 _refine_ls_wR_factor_all 0.0555 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 4782 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_gt 0.0431 _refine_ls_shift/su_max 0.001771 _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: 1.21 -0.163 1.18 -0.592E-01 0.321 ; 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 0.630031(12) 0.63402(5) 0.56333(2) 0.0230 1.0000 Uani . . . . . . N1 N 0.63919(6) 0.7819(2) 0.53272(11) 0.0272 1.0000 Uani . . . . . . N2 N 0.63013(6) 0.8997(2) 0.40440(11) 0.0279 1.0000 Uani . . . . . . N3 N 0.58598(6) 0.5931(2) 0.59045(11) 0.0270 1.0000 Uani . . . . . . N4 N 0.66292(6) 0.4964(2) 0.56637(11) 0.0251 1.0000 Uani . . . . . . N5 N 0.60341(6) 0.5413(2) 0.47242(11) 0.0257 1.0000 Uani . . . . . . N6 N 0.65380(6) 0.6760(2) 0.67040(11) 0.0273 1.0000 Uani . . . . . . Si1 Si 0.54987(2) 0.68236(8) 0.59122(5) 0.0349 1.0000 Uani . . . . . . Si2 Si 0.70012(2) 0.48048(8) 0.53561(4) 0.0315 1.0000 Uani . . . . . . O1 O 0.5000 0.6612(4) 0.2500 0.0856 1.0000 Uani S T . . . . C1 C 0.65340(7) 0.8959(2) 0.52245(13) 0.0249 1.0000 Uani . . . . . . C2 C 0.65033(7) 0.9550(3) 0.46389(14) 0.0277 1.0000 Uani . . . . . . C3 C 0.67424(7) 0.9559(2) 0.58413(13) 0.0248 1.0000 Uani . . . . . . C4 C 0.65793(8) 0.9919(3) 0.63474(14) 0.0306 1.0000 Uani . . . . . . C5 C 0.67668(8) 1.0433(3) 0.69254(16) 0.0380 1.0000 Uani . . . . . . C6 C 0.71269(8) 1.0573(3) 0.70153(15) 0.0381 1.0000 Uani . . . . . . C7 C 0.72929(8) 1.0201(3) 0.65224(16) 0.0361 1.0000 Uani . . . . . . C8 C 0.71026(7) 0.9702(3) 0.59391(15) 0.0311 1.0000 Uani . . . . . . C9 C 0.66460(8) 1.0827(3) 0.45374(16) 0.0370 1.0000 Uani . . . . . . C10 C 0.64644(7) 0.8283(3) 0.36292(13) 0.0280 1.0000 Uani . . . . . . C11 C 0.62684(8) 0.7668(3) 0.30738(14) 0.0339 1.0000 Uani . . . . . . C12 C 0.64284(9) 0.6870(3) 0.27010(15) 0.0388 1.0000 Uani . . . . . . C13 C 0.67845(9) 0.6654(3) 0.28638(16) 0.0415 1.0000 Uani . . . . . . C14 C 0.69788(9) 0.7269(3) 0.34054(16) 0.0396 1.0000 Uani . . . . . . C15 C 0.68241(8) 0.8073(3) 0.37856(15) 0.0332 1.0000 Uani . . . . . . C16 C 0.59704(7) 0.9564(3) 0.38192(14) 0.0302 1.0000 Uani . . . . . . C17 C 0.58740(8) 1.0148(3) 0.32086(16) 0.0375 1.0000 Uani . . . . . . C18 C 0.55488(9) 1.0705(3) 0.30208(18) 0.0461 1.0000 Uani . . . . . . C19 C 0.53194(9) 1.0711(3) 0.34387(19) 0.0485 1.0000 Uani . . . . . . C20 C 0.54152(8) 1.0155(3) 0.40553(18) 0.0442 1.0000 Uani . . . . . . C21 C 0.57361(8) 0.9578(3) 0.42430(16) 0.0358 1.0000 Uani . . . . . . C22 C 0.58244(7) 0.4556(3) 0.59165(14) 0.0270 1.0000 Uani . . . . . . C23 C 0.64459(7) 0.3811(3) 0.57849(14) 0.0297 1.0000 Uani . . . . . . C24 C 0.60404(7) 0.3757(3) 0.55076(14) 0.0265 1.0000 Uani . . . . . . C25 C 0.59361(8) 0.2388(3) 0.55854(16) 0.0335 1.0000 Uani . . . . . . C26 C 0.59557(7) 0.4193(3) 0.48013(14) 0.0264 1.0000 Uani . . . . . . C27 C 0.58003(8) 0.3461(3) 0.42640(14) 0.0338 1.0000 Uani . . . . . . C28 C 0.57191(9) 0.3999(3) 0.36461(15) 0.0396 1.0000 Uani . . . . . . C29 C 0.57935(9) 0.5248(3) 0.35696(15) 0.0385 1.0000 Uani . . . . . . C30 C 0.59536(7) 0.5929(3) 0.41215(14) 0.0318 1.0000 Uani . . . . . . C31 C 0.51890(10) 0.6818(4) 0.5097(2) 0.0683 1.0000 Uani . . . . . . C32 C 0.52694(11) 0.6232(4) 0.6556(2) 0.0649 1.0000 Uani . . . . . . C33 C 0.56355(9) 0.8482(3) 0.61030(17) 0.0433 1.0000 Uani . . . . . . C34 C 0.72183(8) 0.6353(3) 0.53505(17) 0.0402 1.0000 Uani . . . . . . C35 C 0.73103(9) 0.3673(4) 0.5860(2) 0.0655 1.0000 Uani . . . . . . C36 C 0.68945(11) 0.4219(4) 0.44870(18) 0.0552 1.0000 Uani . . . . . . C37 C 0.63662(8) 0.6725(3) 0.71935(15) 0.0398 1.0000 Uani . . . . . . C38 C 0.65185(10) 0.7026(4) 0.78367(17) 0.0523 1.0000 Uani . . . . . . C39 C 0.68631(9) 0.7381(3) 0.79817(16) 0.0461 1.0000 Uani . . . . . . C40 C 0.70478(8) 0.7421(3) 0.74828(16) 0.0386 1.0000 Uani . . . . . . C41 C 0.68768(8) 0.7093(3) 0.68547(15) 0.0358 1.0000 Uani . . . . . . C42 C 0.50351(12) 0.7300(5) 0.3091(2) 0.0699 1.0000 Uani . . . . . . C43 C 0.47051(12) 0.7835(5) 0.3211(2) 0.0757 1.0000 Uani . . . . . . H41 H 0.6322 0.9804 0.6289 0.0388 1.0000 Uiso R . . . . . H51 H 0.6645 1.0711 0.7278 0.0474 1.0000 Uiso R . . . . . H61 H 0.7265 1.0933 0.7435 0.0464 1.0000 Uiso R . . . . . H71 H 0.7551 1.0297 0.6587 0.0446 1.0000 Uiso R . . . . . H81 H 0.7226 0.9442 0.5585 0.0382 1.0000 Uiso R . . . . . H91 H 0.6781 1.1152 0.4968 0.0479 1.0000 Uiso R . . . . . H92 H 0.6804 1.0762 0.4218 0.0479 1.0000 Uiso R . . . . . H93 H 0.6450 1.1415 0.4360 0.0479 1.0000 Uiso R . . . . . H111 H 0.6011 0.7811 0.2945 0.0420 1.0000 Uiso R . . . . . H121 H 0.6285 0.6434 0.2309 0.0495 1.0000 Uiso R . . . . . H131 H 0.6899 0.6071 0.2596 0.0527 1.0000 Uiso R . . . . . H141 H 0.7236 0.7131 0.3523 0.0484 1.0000 Uiso R . . . . . H151 H 0.6970 0.8500 0.4177 0.0427 1.0000 Uiso R . . . . . H171 H 0.6041 1.0159 0.2905 0.0458 1.0000 Uiso R . . . . . H181 H 0.5481 1.1115 0.2579 0.0543 1.0000 Uiso R . . . . . H191 H 0.5084 1.1105 0.3297 0.0574 1.0000 Uiso R . . . . . H201 H 0.5252 1.0169 0.4366 0.0534 1.0000 Uiso R . . . . . H211 H 0.5805 0.9174 0.4686 0.0471 1.0000 Uiso R . . . . . H221 H 0.5897 0.4284 0.6386 0.0346 1.0000 Uiso R . . . . . H222 H 0.5572 0.4356 0.5750 0.0346 1.0000 Uiso R . . . . . H231 H 0.6486 0.3687 0.6273 0.0380 1.0000 Uiso R . . . . . H232 H 0.6554 0.3102 0.5583 0.0380 1.0000 Uiso R . . . . . H251 H 0.6066 0.1833 0.5331 0.0449 1.0000 Uiso R . . . . . H252 H 0.5996 0.2149 0.6062 0.0449 1.0000 Uiso R . . . . . H253 H 0.5680 0.2288 0.5414 0.0449 1.0000 Uiso R . . . . . H271 H 0.5747 0.2558 0.4328 0.0428 1.0000 Uiso R . . . . . H281 H 0.5608 0.3486 0.3255 0.0482 1.0000 Uiso R . . . . . H291 H 0.5733 0.5657 0.3127 0.0483 1.0000 Uiso R . . . . . H301 H 0.6014 0.6829 0.4069 0.0382 1.0000 Uiso R . . . . . H311 H 0.4982 0.7347 0.5122 0.0781 1.0000 Uiso R . . . . . H312 H 0.5308 0.7165 0.4754 0.0781 1.0000 Uiso R . . . . . H313 H 0.5111 0.5939 0.4977 0.0781 1.0000 Uiso R . . . . . H321 H 0.5058 0.6756 0.6559 0.0836 1.0000 Uiso R . . . . . H322 H 0.5432 0.6284 0.6996 0.0836 1.0000 Uiso R . . . . . H323 H 0.5198 0.5340 0.6460 0.0836 1.0000 Uiso R . . . . . H331 H 0.5426 0.9012 0.6109 0.0584 1.0000 Uiso R . . . . . H332 H 0.5798 0.8518 0.6544 0.0584 1.0000 Uiso R . . . . . H333 H 0.5757 0.8803 0.5759 0.0584 1.0000 Uiso R . . . . . H341 H 0.7434 0.6256 0.5171 0.0526 1.0000 Uiso R . . . . . H342 H 0.7281 0.6681 0.5811 0.0526 1.0000 Uiso R . . . . . H343 H 0.7056 0.6953 0.5069 0.0526 1.0000 Uiso R . . . . . H351 H 0.7525 0.3591 0.5674 0.0795 1.0000 Uiso R . . . . . H352 H 0.7376 0.3989 0.6323 0.0795 1.0000 Uiso R . . . . . H353 H 0.7195 0.2836 0.5856 0.0795 1.0000 Uiso R . . . . . H361 H 0.7114 0.4132 0.4317 0.0750 1.0000 Uiso R . . . . . H362 H 0.6736 0.4835 0.4209 0.0750 1.0000 Uiso R . . . . . H363 H 0.6776 0.3386 0.4469 0.0750 1.0000 Uiso R . . . . . H371 H 0.6115 0.6473 0.7091 0.0507 1.0000 Uiso R . . . . . H381 H 0.6383 0.6985 0.8195 0.0647 1.0000 Uiso R . . . . . H391 H 0.6979 0.7617 0.8442 0.0566 1.0000 Uiso R . . . . . H401 H 0.7299 0.7672 0.7578 0.0468 1.0000 Uiso R . . . . . H411 H 0.7010 0.7106 0.6493 0.0437 1.0000 Uiso R . . . . . H421 H 0.5203 0.8004 0.3085 0.0887 1.0000 Uiso R . . . . . H422 H 0.5130 0.6722 0.3465 0.0887 1.0000 Uiso R . . . . . H431 H 0.4747 0.8301 0.3638 0.0923 1.0000 Uiso R . . . . . H432 H 0.4608 0.8422 0.2843 0.0923 1.0000 Uiso R . . . . . H433 H 0.4536 0.7140 0.3223 0.0923 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 0.0213(2) 0.0234(3) 0.0242(2) -0.0001(2) 0.00440(18) -0.0007(2) N1 0.0255(12) 0.0279(13) 0.0271(13) -0.0023(10) 0.0029(10) -0.0025(10) N2 0.0263(12) 0.0312(13) 0.0253(12) -0.0005(10) 0.0033(10) -0.0007(10) N3 0.0239(12) 0.0276(13) 0.0300(13) -0.0015(10) 0.0064(10) -0.0031(10) N4 0.0252(12) 0.0214(12) 0.0291(13) -0.0016(10) 0.0066(10) -0.0023(9) N5 0.0257(12) 0.0241(12) 0.0275(13) -0.0001(10) 0.0061(9) -0.0032(10) N6 0.0263(12) 0.0270(12) 0.0281(12) 0.0001(10) 0.0045(10) 0.0017(10) Si1 0.0239(4) 0.0315(4) 0.0504(5) 0.0018(4) 0.0106(4) 0.0012(3) Si2 0.0279(4) 0.0276(4) 0.0415(5) 0.0008(4) 0.0131(4) 0.0017(3) O1 0.126(4) 0.061(3) 0.064(3) 0.0000 0.008(3) 0.0000 C1 0.0234(13) 0.0228(14) 0.0291(15) -0.0012(11) 0.0067(11) 0.0000(11) C2 0.0273(14) 0.0254(15) 0.0284(15) -0.0023(12) 0.0011(11) -0.0021(12) C3 0.0270(14) 0.0179(13) 0.0289(14) -0.0018(11) 0.0042(11) -0.0003(11) C4 0.0285(15) 0.0303(15) 0.0331(16) -0.0018(13) 0.0070(13) -0.0004(12) C5 0.0429(18) 0.0359(17) 0.0376(17) -0.0126(14) 0.0144(14) -0.0039(15) C6 0.0415(18) 0.0365(18) 0.0328(17) -0.0083(14) 0.0000(14) -0.0049(14) C7 0.0304(16) 0.0341(17) 0.0425(18) -0.0055(14) 0.0046(13) -0.0036(13) C8 0.0283(15) 0.0284(16) 0.0368(17) -0.0043(13) 0.0071(12) -0.0015(12) C9 0.0410(17) 0.0283(16) 0.0400(18) 0.0019(14) 0.0045(14) -0.0071(14) C10 0.0319(15) 0.0274(15) 0.0258(14) 0.0018(12) 0.0083(12) -0.0035(12) C11 0.0356(16) 0.0379(17) 0.0280(16) 0.0006(13) 0.0061(13) -0.0048(14) C12 0.0480(19) 0.0425(18) 0.0265(16) -0.0034(14) 0.0091(14) -0.0094(16) C13 0.051(2) 0.0387(19) 0.0383(18) -0.0054(15) 0.0162(15) 0.0031(16) C14 0.0384(17) 0.0385(18) 0.0435(19) 0.0002(15) 0.0124(15) 0.0060(15) C15 0.0313(16) 0.0363(17) 0.0315(16) 0.0008(13) 0.0050(12) -0.0009(13) C16 0.0308(15) 0.0243(14) 0.0336(16) -0.0012(12) 0.0026(12) -0.0049(12) C17 0.0415(18) 0.0310(17) 0.0380(18) 0.0035(14) 0.0034(14) -0.0014(14) C18 0.045(2) 0.0376(19) 0.047(2) 0.0058(16) -0.0097(16) 0.0042(16) C19 0.0350(18) 0.0340(18) 0.069(3) -0.0101(17) -0.0063(17) 0.0040(15) C20 0.0339(17) 0.0421(19) 0.056(2) -0.0132(17) 0.0088(16) -0.0035(15) C21 0.0325(16) 0.0342(17) 0.0411(18) -0.0021(14) 0.0089(13) -0.0018(14) C22 0.0231(14) 0.0292(15) 0.0286(15) 0.0043(12) 0.0054(11) -0.0024(12) C23 0.0265(14) 0.0306(16) 0.0322(15) 0.0048(13) 0.0068(11) 0.0022(13) C24 0.0245(14) 0.0241(14) 0.0308(15) 0.0021(12) 0.0056(11) 0.0001(12) C25 0.0344(16) 0.0241(15) 0.0426(18) 0.0046(13) 0.0091(13) -0.0038(13) C26 0.0232(14) 0.0247(14) 0.0313(15) 0.0010(12) 0.0058(12) -0.0008(11) C27 0.0342(16) 0.0312(17) 0.0349(17) -0.0036(13) 0.0049(13) -0.0077(13) C28 0.0442(18) 0.0424(19) 0.0300(16) -0.0070(14) 0.0027(14) -0.0103(15) C29 0.0477(19) 0.0390(19) 0.0270(16) 0.0018(14) 0.0035(14) -0.0079(15) C30 0.0310(15) 0.0344(16) 0.0290(16) 0.0024(13) 0.0040(12) -0.0033(13) C31 0.038(2) 0.057(2) 0.095(3) 0.010(2) -0.020(2) 0.0023(19) C32 0.056(2) 0.047(2) 0.108(3) 0.011(2) 0.054(2) 0.0082(19) C33 0.0402(18) 0.0388(19) 0.055(2) -0.0005(16) 0.0196(15) 0.0034(15) C34 0.0334(16) 0.0395(18) 0.0510(19) -0.0066(16) 0.0160(14) -0.0070(15) C35 0.0340(19) 0.059(2) 0.106(3) 0.030(2) 0.020(2) 0.0188(18) C36 0.072(3) 0.046(2) 0.059(2) -0.0193(18) 0.039(2) -0.0216(19) C37 0.0347(16) 0.053(2) 0.0305(16) -0.0048(15) 0.0049(13) -0.0029(15) C38 0.051(2) 0.074(3) 0.0329(18) -0.0044(18) 0.0114(16) -0.007(2) C39 0.052(2) 0.052(2) 0.0307(18) -0.0070(15) 0.0004(15) -0.0038(17) C40 0.0363(17) 0.0370(18) 0.0388(18) 0.0010(14) -0.0006(14) 0.0026(14) C41 0.0315(16) 0.0398(18) 0.0346(17) -0.0015(14) 0.0037(13) -0.0017(14) C42 0.072(3) 0.071(3) 0.061(3) -0.006(2) -0.001(2) 0.001(2) C43 0.063(3) 0.087(3) 0.075(3) 0.019(3) 0.011(2) -0.012(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1432(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 . 1.765(2) yes Ti1 . N3 . 1.975(2) yes Ti1 . N4 . 1.946(2) yes Ti1 . N5 . 2.192(2) yes Ti1 . N6 . 2.268(2) yes N1 . C1 . 1.372(3) yes N2 . C2 . 1.446(4) yes N2 . C10 . 1.400(4) yes N2 . C16 . 1.420(4) yes N3 . Si1 . 1.709(2) yes N3 . C22 . 1.474(4) yes N4 . Si2 . 1.720(2) yes N4 . C23 . 1.473(4) yes N5 . C26 . 1.354(4) yes N5 . C30 . 1.342(4) yes N6 . C37 . 1.332(4) yes N6 . C41 . 1.348(4) yes Si1 . C31 . 1.865(4) yes Si1 . C32 . 1.870(4) yes Si1 . C33 . 1.866(3) yes Si2 . C34 . 1.859(3) yes Si2 . C35 . 1.868(4) yes Si2 . C36 . 1.872(4) yes O1 . C42 5_655 1.411(5) yes O1 . C42 . 1.411(5) yes C1 . C2 . 1.352(4) yes C1 . C3 . 1.510(4) yes C2 . C9 . 1.504(4) yes C3 . C4 . 1.394(4) yes C3 . C8 . 1.393(4) yes C4 . C5 . 1.383(4) yes C4 . H41 . 1.000 no C5 . C6 . 1.394(4) yes C5 . H51 . 1.000 no C6 . C7 . 1.381(4) yes C6 . H61 . 1.000 no C7 . C8 . 1.389(4) 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 . 1.407(4) yes C10 . C15 . 1.398(4) yes C11 . C12 . 1.386(4) yes C11 . H111 . 1.000 no C12 . C13 . 1.386(5) yes C12 . H121 . 1.000 no C13 . C14 . 1.384(5) yes C13 . H131 . 1.000 no C14 . C15 . 1.389(4) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C16 . C17 . 1.392(4) yes C16 . C21 . 1.399(4) yes C17 . C18 . 1.387(5) yes C17 . H171 . 1.000 no C18 . C19 . 1.375(5) yes C18 . H181 . 1.000 no C19 . C20 . 1.389(5) yes C19 . H191 . 1.000 no C20 . C21 . 1.382(5) yes C20 . H201 . 1.000 no C21 . H211 . 1.000 no C22 . C24 . 1.571(4) yes C22 . H221 . 1.000 no C22 . H222 . 1.000 no C23 . C24 . 1.576(4) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C24 . C25 . 1.533(4) yes C24 . C26 . 1.507(4) yes C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no C26 . C27 . 1.393(4) yes C27 . C28 . 1.380(4) yes C27 . H271 . 1.000 no C28 . C29 . 1.380(4) yes C28 . H281 . 1.000 no C29 . C30 . 1.390(4) yes C29 . H291 . 1.000 no C30 . H301 . 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 . H331 . 1.000 no C33 . H332 . 1.000 no C33 . H333 . 1.000 no C34 . H341 . 1.000 no C34 . H342 . 1.000 no C34 . H343 . 1.000 no C35 . H351 . 1.000 no C35 . H352 . 1.000 no C35 . H353 . 1.000 no C36 . H361 . 1.000 no C36 . H362 . 1.000 no C36 . H363 . 1.000 no C37 . C38 . 1.382(5) yes C37 . H371 . 1.000 no C38 . C39 . 1.376(5) yes C38 . H381 . 1.000 no C39 . C40 . 1.383(5) yes C39 . H391 . 1.000 no C40 . C41 . 1.381(4) yes C40 . H401 . 1.000 no C41 . H411 . 1.000 no C42 . C43 . 1.483(6) yes C42 . H421 . 1.000 no C42 . H422 . 1.000 no C43 . H431 . 1.000 no C43 . H432 . 1.000 no C43 . H433 . 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 . 123.78(10) yes N1 . Ti1 . N4 . 120.11(10) yes N3 . Ti1 . N4 . 115.98(10) yes N1 . Ti1 . N5 . 100.92(10) yes N3 . Ti1 . N5 . 81.85(9) yes N4 . Ti1 . N5 . 83.16(9) yes N1 . Ti1 . N6 . 95.95(10) yes N3 . Ti1 . N6 . 88.22(9) yes N4 . Ti1 . N6 . 89.04(9) yes N5 . Ti1 . N6 . 163.12(9) yes Ti1 . N1 . C1 . 165.3(2) yes C2 . N2 . C10 . 120.5(2) yes C2 . N2 . C16 . 114.0(2) yes C10 . N2 . C16 . 122.3(2) yes Ti1 . N3 . Si1 . 131.01(14) yes Ti1 . N3 . C22 . 108.40(17) yes Si1 . N3 . C22 . 118.19(17) yes Ti1 . N4 . Si2 . 132.15(13) yes Ti1 . N4 . C23 . 106.92(16) yes Si2 . N4 . C23 . 117.61(18) yes Ti1 . N5 . C26 . 114.26(18) yes Ti1 . N5 . C30 . 126.45(19) yes C26 . N5 . C30 . 119.3(2) yes Ti1 . N6 . C37 . 124.91(19) yes Ti1 . N6 . C41 . 117.55(19) yes C37 . N6 . C41 . 117.5(3) yes N3 . Si1 . C31 . 111.94(17) yes N3 . Si1 . C32 . 110.04(15) yes C31 . Si1 . C32 . 109.1(2) yes N3 . Si1 . C33 . 109.11(13) yes C31 . Si1 . C33 . 107.42(18) yes C32 . Si1 . C33 . 109.14(18) yes N4 . Si2 . C34 . 109.89(13) yes N4 . Si2 . C35 . 110.98(15) yes C34 . Si2 . C35 . 109.41(18) yes N4 . Si2 . C36 . 110.80(15) yes C34 . Si2 . C36 . 107.50(16) yes C35 . Si2 . C36 . 108.2(2) yes C42 5_655 O1 . C42 . 117.4(5) yes N1 . C1 . C2 . 126.2(3) yes N1 . C1 . C3 . 114.2(2) yes C2 . C1 . C3 . 119.7(2) yes N2 . C2 . C1 . 120.5(2) yes N2 . C2 . C9 . 113.8(2) yes C1 . C2 . C9 . 125.6(3) yes C1 . C3 . C4 . 120.2(2) yes C1 . C3 . C8 . 121.5(2) yes C4 . C3 . C8 . 118.1(3) yes C3 . C4 . C5 . 121.3(3) yes C3 . C4 . H41 . 119.1 no C5 . C4 . H41 . 119.6 no C4 . C5 . C6 . 119.9(3) yes C4 . C5 . H51 . 120.3 no C6 . C5 . H51 . 119.8 no C5 . C6 . C7 . 119.5(3) yes C5 . C6 . H61 . 120.4 no C7 . C6 . H61 . 120.1 no C6 . C7 . C8 . 120.3(3) yes C6 . C7 . H71 . 119.6 no C8 . C7 . H71 . 120.0 no C3 . C8 . C7 . 120.9(3) yes C3 . C8 . H81 . 119.6 no C7 . C8 . H81 . 119.6 no C2 . C9 . H91 . 109.3 no C2 . C9 . H92 . 109.3 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 . 121.0(3) yes N2 . C10 . C15 . 120.9(3) yes C11 . C10 . C15 . 117.9(3) yes C10 . C11 . C12 . 120.7(3) yes C10 . C11 . H111 . 119.7 no C12 . C11 . H111 . 119.6 no C11 . C12 . C13 . 121.1(3) yes C11 . C12 . H121 . 119.8 no C13 . C12 . H121 . 119.1 no C12 . C13 . C14 . 118.3(3) yes C12 . C13 . H131 . 120.9 no C14 . C13 . H131 . 120.7 no C13 . C14 . C15 . 121.5(3) yes C13 . C14 . H141 . 119.0 no C15 . C14 . H141 . 119.5 no C10 . C15 . C14 . 120.5(3) yes C10 . C15 . H151 . 119.7 no C14 . C15 . H151 . 119.9 no N2 . C16 . C17 . 123.1(3) yes N2 . C16 . C21 . 118.3(3) yes C17 . C16 . C21 . 118.6(3) yes C16 . C17 . C18 . 120.4(3) yes C16 . C17 . H171 . 119.3 no C18 . C17 . H171 . 120.3 no C17 . C18 . C19 . 120.6(3) yes C17 . C18 . H181 . 119.7 no C19 . C18 . H181 . 119.6 no C18 . C19 . C20 . 119.5(3) yes C18 . C19 . H191 . 120.2 no C20 . C19 . H191 . 120.3 no C19 . C20 . C21 . 120.3(3) yes C19 . C20 . H201 . 120.0 no C21 . C20 . H201 . 119.7 no C16 . C21 . C20 . 120.5(3) yes C16 . C21 . H211 . 119.2 no C20 . C21 . H211 . 120.3 no N3 . C22 . C24 . 117.9(2) yes N3 . C22 . H221 . 107.3 no C24 . C22 . H221 . 107.1 no N3 . C22 . H222 . 107.2 no C24 . C22 . H222 . 107.7 no H221 . C22 . H222 . 109.5 no N4 . C23 . C24 . 117.4(2) yes N4 . C23 . H231 . 107.7 no C24 . C23 . H231 . 107.4 no N4 . C23 . H232 . 107.2 no C24 . C23 . H232 . 107.6 no H231 . C23 . H232 . 109.5 no C22 . C24 . C23 . 113.6(2) yes C22 . C24 . C25 . 105.9(2) yes C23 . C24 . C25 . 105.5(2) yes C22 . C24 . C26 . 108.9(2) yes C23 . C24 . C26 . 110.1(2) yes C25 . C24 . C26 . 112.8(2) yes C24 . C25 . H251 . 109.3 no C24 . C25 . H252 . 109.5 no H251 . C25 . H252 . 109.5 no C24 . C25 . H253 . 109.5 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no C24 . C26 . N5 . 113.7(2) yes C24 . C26 . C27 . 125.2(3) yes N5 . C26 . C27 . 121.1(3) yes C26 . C27 . C28 . 119.2(3) yes C26 . C27 . H271 . 120.1 no C28 . C27 . H271 . 120.6 no C27 . C28 . C29 . 119.7(3) yes C27 . C28 . H281 . 120.3 no C29 . C28 . H281 . 120.1 no C28 . C29 . C30 . 118.6(3) yes C28 . C29 . H291 . 120.8 no C30 . C29 . H291 . 120.6 no C29 . C30 . N5 . 122.1(3) yes C29 . C30 . H301 . 119.3 no N5 . C30 . H301 . 118.6 no Si1 . C31 . H311 . 109.4 no Si1 . C31 . H312 . 109.4 no H311 . C31 . H312 . 109.5 no Si1 . C31 . H313 . 109.6 no H311 . C31 . H313 . 109.5 no H312 . C31 . H313 . 109.5 no Si1 . C32 . H321 . 109.8 no Si1 . C32 . H322 . 108.9 no H321 . C32 . H322 . 109.5 no Si1 . C32 . H323 . 109.6 no H321 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no Si1 . C33 . H331 . 109.8 no Si1 . C33 . H332 . 109.3 no H331 . C33 . H332 . 109.5 no Si1 . C33 . H333 . 109.4 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.5 no Si2 . C34 . H341 . 109.6 no Si2 . C34 . H342 . 109.1 no H341 . C34 . H342 . 109.5 no Si2 . C34 . H343 . 109.7 no H341 . C34 . H343 . 109.5 no H342 . C34 . H343 . 109.5 no Si2 . C35 . H351 . 109.9 no Si2 . C35 . H352 . 109.1 no H351 . C35 . H352 . 109.5 no Si2 . C35 . H353 . 109.4 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no Si2 . C36 . H361 . 109.6 no Si2 . C36 . H362 . 108.9 no H361 . C36 . H362 . 109.5 no Si2 . C36 . H363 . 109.9 no H361 . C36 . H363 . 109.5 no H362 . C36 . H363 . 109.5 no N6 . C37 . C38 . 123.0(3) yes N6 . C37 . H371 . 118.5 no C38 . C37 . H371 . 118.4 no C37 . C38 . C39 . 118.8(3) yes C37 . C38 . H381 . 121.3 no C39 . C38 . H381 . 119.9 no C38 . C39 . C40 . 119.3(3) yes C38 . C39 . H391 . 120.5 no C40 . C39 . H391 . 120.2 no C39 . C40 . C41 . 118.2(3) yes C39 . C40 . H401 . 120.6 no C41 . C40 . H401 . 121.2 no C40 . C41 . N6 . 123.1(3) yes C40 . C41 . H411 . 118.6 no N6 . C41 . H411 . 118.3 no O1 . C42 . C43 . 114.6(4) yes O1 . C42 . H421 . 108.9 no C43 . C42 . H421 . 108.2 no O1 . C42 . H422 . 107.9 no C43 . C42 . H422 . 107.7 no H421 . C42 . H422 . 109.5 no C42 . C43 . H431 . 110.6 no C42 . C43 . H432 . 108.6 no H431 . C43 . H432 . 109.5 no C42 . C43 . H433 . 109.1 no H431 . C43 . H433 . 109.5 no H432 . C43 . H433 . 109.5 no #===end data_Compound_5 _database_code_depnum_ccdc_archive 'CCDC 698354' _audit_creation_method CRYSTALS_ver_12.84 _chemical_name_systematic ; Ti2(N2Npy)2{u-N(NPh2)C(Me)N}2 . 0.8 C6H6 ; _publ_section_exptl_refinement ; N(5) and N(21) of the pyridyl substituent were positionally disordered and modelled as such. The C6H6 molecule of crystallisation has partial chemical occupancy and is disordered around a special position. ; _chemical_melting_point ? _cell_length_a 40.0450(3) _cell_length_b 40.0450(3) _cell_length_c 11.26710(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 15647.3(2) _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/3,y+2/3,z+2/3 -x+1/3,-y+2/3,-z+2/3 x+2/3,y+1/3,z+1/3 -x+2/3,-y+1/3,-z+1/3 -y,x-y,z y,-x+y,-z -y+1/3,x-y+2/3,z+2/3 y+1/3,-x+y+2/3,-z+2/3 -y+2/3,x-y+1/3,z+1/3 y+2/3,-x+y+1/3,-z+1/3 -x+y,-x,z x-y,x,-z -x+y+1/3,-x+2/3,z+2/3 x-y+1/3,x+2/3,-z+2/3 -x+y+2/3,-x+1/3,z+1/3 x-y+2/3,x+1/3,-z+1/3 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 9 _chemical_formula_sum 'C62.80 H88.8 N12 Si4 Ti2' _chemical_formula_moiety 'C58 H84 N12 Si4 Ti2, 0.8 C6H6' _chemical_compound_source ? _chemical_formula_weight 1220.02 _cell_measurement_reflns_used 7932 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_meas ? _exptl_crystal_F_000 5846.398 _exptl_absorpt_coefficient_mu 0.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.97 _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 'USER DEFINED STRUCTURE SOLUTION' _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 15799 _reflns_number_total 7952 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_min 5.141 _diffrn_reflns_theta_max 27.524 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.974 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -51 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 52 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 2.09 _oxford_diffrn_Wilson_scale 53.30 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.32 _refine_diff_density_max 0.57 _refine_ls_number_reflns 5552 _refine_ls_number_restraints 0 _refine_ls_number_parameters 415 _refine_ls_wR_factor_ref 0.0453 _refine_ls_goodness_of_fit_ref 1.0697 _refine_ls_R_factor_all 0.0603 _refine_ls_wR_factor_all 0.0586 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 5552 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_gt 0.0453 _refine_ls_shift/su_max 0.003 _refine_ls_extinction_method None _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: 0.953 0.589 0.672 ; 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 0.291101(8) 0.155790(8) 0.15214(2) 0.0230 1.0000 Uani . . . . . . N1 N 0.29411(4) 0.16627(4) -0.05003(12) 0.0263 1.0000 Uani . . . . . . N2 N 0.27884(4) 0.17227(4) -0.15579(13) 0.0314 1.0000 Uani . . . . . . N3 N 0.24828(4) 0.10507(4) 0.15166(12) 0.0269 1.0000 Uani . . . . . . N4 N 0.26770(4) 0.18620(4) 0.18893(12) 0.0246 1.0000 Uani . . . . . . N5 N 0.1393(3) 0.1285(3) 0.1456(12) 0.0626 0.5000 Uani . . . . . . N51 N 0.1315(3) 0.1136(2) 0.1547(13) 0.0532 0.5000 Uani . . . . . . N6 N 0.34376(4) 0.17297(4) 0.05355(13) 0.0306 1.0000 Uani . . . . . . Si1 Si 0.241148(14) 0.060200(13) 0.19814(4) 0.0311 1.0000 Uani . . . . . . Si2 Si 0.280210(14) 0.224691(13) 0.28572(4) 0.0271 1.0000 Uani . . . . . . C1 C 0.25217(5) 0.13958(5) -0.21812(15) 0.0321 1.0000 Uani . . . . . . C2 C 0.25165(7) 0.10486(6) -0.20263(19) 0.0478 1.0000 Uani . . . . . . C3 C 0.22478(11) 0.07222(7) -0.2618(3) 0.0800 1.0000 Uani . . . . . . C4 C 0.19886(11) 0.07361(8) -0.3389(3) 0.0876 1.0000 Uani . . . . . . C5 C 0.19918(8) 0.10790(8) -0.3553(2) 0.0661 1.0000 Uani . . . . . . C6 C 0.22544(6) 0.14099(6) -0.29499(18) 0.0432 1.0000 Uani . . . . . . C7 C 0.29024(5) 0.21085(5) -0.18576(14) 0.0278 1.0000 Uani . . . . . . C8 C 0.29819(5) 0.23761(5) -0.09576(15) 0.0289 1.0000 Uani . . . . . . C9 C 0.31178(5) 0.27603(5) -0.12379(16) 0.0323 1.0000 Uani . . . . . . C10 C 0.31776(6) 0.28835(5) -0.23996(17) 0.0352 1.0000 Uani . . . . . . C11 C 0.30956(6) 0.26172(6) -0.32976(17) 0.0411 1.0000 Uani . . . . . . C12 C 0.29610(6) 0.22317(6) -0.30354(16) 0.0372 1.0000 Uani . . . . . . C13 C 0.21343(5) 0.10245(5) 0.09493(16) 0.0303 1.0000 Uani . . . . . . C14 C 0.23001(5) 0.17205(5) 0.12822(15) 0.0279 1.0000 Uani . . . . . . C15 C 0.19988(5) 0.12910(5) 0.15017(16) 0.0294 1.0000 Uani . . . . . . C16 C 0.19194(6) 0.12071(6) 0.28296(17) 0.0369 1.0000 Uani . . . . . . C17 C 0.16340(5) 0.12192(5) 0.08465(19) 0.0364 1.0000 Uani . . . . . . C18 C 0.16011(7) 0.11817(7) -0.0365(2) 0.0487 1.0000 Uani . . . . . . C19 C 0.12616(7) 0.11153(7) -0.0918(2) 0.0559 1.0000 Uani . . . . . . C20 C 0.09762(8) 0.11056(10) -0.0255(3) 0.0728 1.0000 Uani . . . . . . C21 C 0.1069(4) 0.1233(4) 0.0954(13) 0.0794 0.5000 Uani . . . . . . C211 C 0.0992(5) 0.1065(4) 0.091(2) 0.0850 0.5000 Uani . . . . . . C22 C 0.20202(7) 0.03742(6) 0.3118(2) 0.0497 1.0000 Uani . . . . . . C23 C 0.22731(6) 0.02792(6) 0.0654(2) 0.0436 1.0000 Uani . . . . . . C24 C 0.28520(6) 0.06464(6) 0.26784(19) 0.0410 1.0000 Uani . . . . . . C25 C 0.24304(6) 0.21263(7) 0.40469(17) 0.0415 1.0000 Uani . . . . . . C26 C 0.28440(7) 0.26675(6) 0.20010(18) 0.0416 1.0000 Uani . . . . . . C27 C 0.32729(6) 0.24011(6) 0.36026(16) 0.0361 1.0000 Uani . . . . . . C28 C 0.33085(5) 0.17629(5) -0.05243(14) 0.0269 1.0000 Uani . . . . . . C29 C 0.35592(6) 0.18954(6) -0.16048(18) 0.0411 1.0000 Uani . . . . . . C101 C 0.3941(3) 0.6249(3) 0.1797(10) 0.0936 0.4000 Uani . . . . . . C102 C 0.3732(3) 0.6205(4) 0.0778(12) 0.1072 0.4000 Uani . . . . . . C103 C 0.3845(3) 0.6518(4) 0.0037(9) 0.0946 0.4000 Uani . . . . . . C104 C 0.4169(2) 0.6863(3) 0.0299(7) 0.0724 0.4000 Uani . . . . . . C105 C 0.4378(3) 0.6895(3) 0.1262(7) 0.0727 0.4000 Uani . . . . . . C106 C 0.4260(3) 0.6587(3) 0.2030(8) 0.0808 0.4000 Uani . . . . . . H21 H 0.2707 0.1036 -0.1481 0.0572 1.0000 Uiso R . . . . . H31 H 0.2243 0.0473 -0.2498 0.0866 1.0000 Uiso R . . . . . H41 H 0.1795 0.0498 -0.3816 0.0881 1.0000 Uiso R . . . . . H51 H 0.1803 0.1090 -0.4113 0.0684 1.0000 Uiso R . . . . . H61 H 0.2254 0.1657 -0.3064 0.0502 1.0000 Uiso R . . . . . H81 H 0.2940 0.2291 -0.0110 0.0362 1.0000 Uiso R . . . . . H91 H 0.3173 0.2951 -0.0586 0.0405 1.0000 Uiso R . . . . . H101 H 0.3278 0.3162 -0.2591 0.0437 1.0000 Uiso R . . . . . H111 H 0.3134 0.2703 -0.4145 0.0496 1.0000 Uiso R . . . . . H121 H 0.2906 0.2042 -0.3689 0.0462 1.0000 Uiso R . . . . . H131 H 0.2194 0.1096 0.0093 0.0397 1.0000 Uiso R . . . . . H132 H 0.1919 0.0752 0.1013 0.0397 1.0000 Uiso R . . . . . H141 H 0.2351 0.1755 0.0409 0.0356 1.0000 Uiso R . . . . . H142 H 0.2188 0.1881 0.1550 0.0356 1.0000 Uiso R . . . . . H161 H 0.1833 0.1382 0.3174 0.0469 1.0000 Uiso R . . . . . H162 H 0.2161 0.1253 0.3237 0.0469 1.0000 Uiso R . . . . . H163 H 0.1713 0.0933 0.2944 0.0469 1.0000 Uiso R . . . . . H181 H 0.1821 0.1203 -0.0845 0.0624 1.0000 Uiso R . . . . . H191 H 0.1231 0.1076 -0.1797 0.0720 1.0000 Uiso R . . . . . H201 H 0.0744 0.1092 -0.0636 0.0848 1.0000 Uiso R . . . . . H211 H 0.0887 0.1279 0.1438 0.0943 0.5000 Uiso R . . . . . H2111 H 0.0746 0.0971 0.1361 0.1087 0.5000 Uiso R . . . . . H221 H 0.1987 0.0119 0.3362 0.0598 1.0000 Uiso R . . . . . H222 H 0.2091 0.0547 0.3827 0.0598 1.0000 Uiso R . . . . . H223 H 0.1773 0.0336 0.2772 0.0598 1.0000 Uiso R . . . . . H231 H 0.2230 0.0021 0.0899 0.0561 1.0000 Uiso R . . . . . H232 H 0.2484 0.0395 0.0051 0.0561 1.0000 Uiso R . . . . . H233 H 0.2030 0.0250 0.0303 0.0561 1.0000 Uiso R . . . . . H241 H 0.2802 0.0386 0.2934 0.0550 1.0000 Uiso R . . . . . H242 H 0.3068 0.0758 0.2090 0.0550 1.0000 Uiso R . . . . . H243 H 0.2924 0.0820 0.3385 0.0550 1.0000 Uiso R . . . . . H251 H 0.2513 0.2354 0.4578 0.0540 1.0000 Uiso R . . . . . H252 H 0.2402 0.1903 0.4524 0.0540 1.0000 Uiso R . . . . . H253 H 0.2178 0.2057 0.3670 0.0540 1.0000 Uiso R . . . . . H261 H 0.2915 0.2888 0.2555 0.0553 1.0000 Uiso R . . . . . H262 H 0.3047 0.2746 0.1377 0.0553 1.0000 Uiso R . . . . . H263 H 0.2591 0.2592 0.1617 0.0553 1.0000 Uiso R . . . . . H271 H 0.3336 0.2622 0.4148 0.0445 1.0000 Uiso R . . . . . H272 H 0.3479 0.2483 0.2988 0.0445 1.0000 Uiso R . . . . . H273 H 0.3256 0.2181 0.4068 0.0445 1.0000 Uiso R . . . . . H291 H 0.3825 0.1953 -0.1388 0.0535 1.0000 Uiso R . . . . . H292 H 0.3570 0.2134 -0.1922 0.0535 1.0000 Uiso R . . . . . H293 H 0.3451 0.1689 -0.2224 0.0535 1.0000 Uiso R . . . . . H1011 H 0.3849 0.6032 0.2378 0.1135 0.4000 Uiso R . . . . . H1021 H 0.3507 0.5952 0.0536 0.1128 0.4000 Uiso R . . . . . H1031 H 0.3688 0.6500 -0.0677 0.1036 0.4000 Uiso R . . . . . H1041 H 0.4250 0.7087 -0.0249 0.0726 0.4000 Uiso R . . . . . H1051 H 0.4620 0.7143 0.1425 0.0757 0.4000 Uiso R . . . . . H1061 H 0.4417 0.6619 0.2757 0.0811 0.4000 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 0.02352(15) 0.02240(14) 0.02624(15) -0.00386(10) -0.00481(10) 0.01377(12) N1 0.0325(7) 0.0295(7) 0.0213(6) -0.0009(5) -0.0055(5) 0.0189(6) N2 0.0403(8) 0.0275(7) 0.0264(7) -0.0025(5) -0.0144(6) 0.0169(6) N3 0.0270(7) 0.0244(6) 0.0327(7) -0.0021(5) -0.0049(5) 0.0154(6) N4 0.0273(7) 0.0254(6) 0.0245(6) -0.0028(5) -0.0029(5) 0.0157(5) N5 0.048(6) 0.106(8) 0.056(3) -0.001(6) -0.002(4) 0.055(6) N51 0.032(3) 0.066(5) 0.065(4) -0.002(4) 0.003(2) 0.026(4) N6 0.0349(7) 0.0307(7) 0.0319(7) -0.0049(6) -0.0082(6) 0.0206(6) Si1 0.0335(2) 0.0233(2) 0.0386(3) -0.00127(18) -0.00542(19) 0.01584(19) Si2 0.0348(2) 0.0288(2) 0.0232(2) -0.00476(16) -0.00268(17) 0.02000(19) C1 0.0385(9) 0.0332(9) 0.0249(8) -0.0042(6) -0.0059(7) 0.0181(8) C2 0.0690(14) 0.0363(10) 0.0391(10) -0.0082(8) -0.0151(10) 0.0270(10) C3 0.128(3) 0.0358(12) 0.0608(16) -0.0179(11) -0.0381(17) 0.0296(15) C4 0.111(3) 0.0449(14) 0.0637(17) -0.0151(12) -0.0456(18) 0.0060(15) C5 0.0643(16) 0.0591(15) 0.0509(14) -0.0048(11) -0.0296(12) 0.0130(12) C6 0.0437(11) 0.0435(11) 0.0383(10) -0.0039(8) -0.0141(8) 0.0188(9) C7 0.0301(8) 0.0303(8) 0.0249(7) -0.0001(6) -0.0045(6) 0.0166(7) C8 0.0330(8) 0.0322(8) 0.0232(7) 0.0005(6) -0.0024(6) 0.0175(7) C9 0.0368(9) 0.0317(9) 0.0299(8) -0.0019(7) -0.0031(7) 0.0182(7) C10 0.0377(9) 0.0312(9) 0.0367(9) 0.0059(7) 0.0009(7) 0.0173(7) C11 0.0540(12) 0.0429(11) 0.0260(8) 0.0065(7) 0.0040(8) 0.0239(9) C12 0.0509(11) 0.0365(9) 0.0259(8) -0.0021(7) -0.0027(7) 0.0230(8) C13 0.0264(8) 0.0283(8) 0.0376(9) -0.0045(7) -0.0081(7) 0.0148(7) C14 0.0293(8) 0.0279(8) 0.0307(8) -0.0012(6) -0.0042(6) 0.0175(7) C15 0.0258(8) 0.0294(8) 0.0358(9) 0.0008(6) -0.0021(6) 0.0160(7) C16 0.0368(9) 0.0369(9) 0.0388(10) 0.0052(7) 0.0066(7) 0.0197(8) C17 0.0286(8) 0.0305(9) 0.0535(11) -0.0016(8) -0.0057(8) 0.0173(7) C18 0.0482(12) 0.0601(13) 0.0497(12) -0.0002(10) -0.0097(9) 0.0359(11) C19 0.0578(14) 0.0521(13) 0.0679(15) -0.0088(11) -0.0266(12) 0.0350(12) C20 0.0433(13) 0.088(2) 0.094(2) -0.0060(17) -0.0237(14) 0.0382(14) C21 0.046(6) 0.146(13) 0.070(5) -0.014(7) -0.006(4) 0.066(8) C211 0.043(5) 0.108(9) 0.112(8) -0.026(8) -0.012(4) 0.044(6) C22 0.0504(12) 0.0354(10) 0.0607(13) 0.0132(9) 0.0075(10) 0.0195(9) C23 0.0472(11) 0.0298(9) 0.0582(13) -0.0138(8) -0.0149(9) 0.0225(8) C24 0.0482(11) 0.0363(9) 0.0476(11) -0.0029(8) -0.0129(9) 0.0279(9) C25 0.0440(10) 0.0533(12) 0.0327(9) -0.0092(8) 0.0009(8) 0.0284(9) C26 0.0643(13) 0.0319(9) 0.0363(10) -0.0082(7) -0.0082(9) 0.0298(9) C27 0.0390(9) 0.0383(9) 0.0325(9) -0.0119(7) -0.0077(7) 0.0204(8) C28 0.0323(8) 0.0258(7) 0.0254(8) -0.0055(6) -0.0036(6) 0.0167(7) C29 0.0414(10) 0.0521(11) 0.0353(10) 0.0004(8) 0.0053(8) 0.0275(9) C101 0.072(5) 0.111(7) 0.118(8) 0.027(6) 0.009(5) 0.061(6) C102 0.063(5) 0.113(8) 0.142(10) 0.007(7) -0.012(6) 0.041(5) C103 0.080(6) 0.145(10) 0.085(6) -0.013(6) -0.014(5) 0.076(7) C104 0.078(5) 0.085(5) 0.067(5) -0.010(4) 0.008(4) 0.051(4) C105 0.078(5) 0.081(5) 0.064(4) -0.009(4) -0.005(4) 0.044(4) C106 0.075(5) 0.106(7) 0.082(5) -0.002(5) -0.001(4) 0.061(5) 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 . N6 6_555 1.8684(14) yes Ti1 . N1 . 2.3084(13) yes Ti1 . N3 . 1.8929(14) yes Ti1 . N4 . 1.9170(13) yes Ti1 . N6 . 2.1687(16) yes N1 . N2 . 1.4137(18) yes N1 . C28 . 1.318(2) yes N2 . C1 . 1.396(2) yes N2 . C7 . 1.415(2) yes N3 . Si1 . 1.7523(14) yes N3 . C13 . 1.490(2) yes N4 . Si2 . 1.7446(13) yes N4 . C14 . 1.487(2) yes N5 . C17 . 1.313(13) yes N5 . C21 . 1.333(18) yes N51 . C17 . 1.391(13) yes N51 . C211 . 1.38(2) yes N6 . C28 . 1.334(2) yes Si1 . C22 . 1.871(2) yes Si1 . C23 . 1.871(2) yes Si1 . C24 . 1.857(2) yes Si2 . C25 . 1.878(2) yes Si2 . C26 . 1.874(2) yes Si2 . C27 . 1.8645(19) yes C1 . C2 . 1.391(3) yes C1 . C6 . 1.400(3) yes C2 . C3 . 1.380(3) yes C2 . H21 . 1.000 no C3 . C4 . 1.376(5) yes C3 . H31 . 1.000 no C4 . C5 . 1.379(5) yes C4 . H41 . 1.000 no C5 . C6 . 1.389(3) yes C5 . H51 . 1.000 no C6 . H61 . 1.000 no C7 . C8 . 1.392(2) yes C7 . C12 . 1.394(2) yes C8 . C9 . 1.388(2) yes C8 . H81 . 1.000 no C9 . C10 . 1.377(3) yes C9 . H91 . 1.000 no C10 . C11 . 1.385(3) yes C10 . H101 . 1.000 no C11 . C12 . 1.389(3) yes C11 . H111 . 1.000 no C12 . H121 . 1.000 no C13 . C15 . 1.549(2) yes C13 . H131 . 1.000 no C13 . H132 . 1.000 no C14 . C15 . 1.549(2) yes C14 . H141 . 1.000 no C14 . H142 . 1.000 no C15 . C16 . 1.531(3) yes C15 . C17 . 1.530(2) yes C16 . H161 . 1.000 no C16 . H162 . 1.000 no C16 . H163 . 1.000 no C17 . C18 . 1.373(3) yes C18 . C19 . 1.395(3) yes C18 . H181 . 1.000 no C19 . C20 . 1.350(4) yes C19 . H191 . 1.000 no C20 . C21 . 1.437(15) yes C20 . C211 . 1.33(2) yes C20 . H201 . 1.000 no C21 . H211 . 1.000 no C211 . H2111 . 1.000 no C22 . H221 . 1.000 no C22 . H222 . 1.000 no C22 . H223 . 1.000 no C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 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 . C29 . 1.496(3) yes C29 . H291 . 1.000 no C29 . H292 . 1.000 no C29 . H293 . 1.000 no C101 . C102 . 1.377(16) yes C101 . C106 . 1.341(14) yes C101 . H1011 . 1.000 no C102 . C103 . 1.380(16) yes C102 . H1021 . 1.000 no C103 . C104 . 1.375(14) yes C103 . H1031 . 1.000 no C104 . C105 . 1.337(11) yes C104 . H1041 . 1.000 no C105 . C106 . 1.383(12) yes C105 . H1051 . 1.000 no C106 . H1061 . 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 N6 6_555 Ti1 . N1 . 140.42(6) yes N6 6_555 Ti1 . N3 . 108.34(6) yes N1 . Ti1 . N3 . 97.43(6) yes N6 6_555 Ti1 . N4 . 107.29(6) yes N1 . Ti1 . N4 . 95.48(5) yes N3 . Ti1 . N4 . 102.36(6) yes N6 6_555 Ti1 . N6 . 81.73(7) yes N1 . Ti1 . N6 . 58.86(5) yes N3 . Ti1 . N6 . 123.66(6) yes N4 . Ti1 . N6 . 128.02(6) yes Ti1 . N1 . N2 . 151.04(11) yes Ti1 . N1 . C28 . 91.40(10) yes N2 . N1 . C28 . 116.30(14) yes N1 . N2 . C1 . 117.24(13) yes N1 . N2 . C7 . 117.10(13) yes C1 . N2 . C7 . 125.55(14) yes Ti1 . N3 . Si1 . 134.05(8) yes Ti1 . N3 . C13 . 112.99(10) yes Si1 . N3 . C13 . 112.91(11) yes Ti1 . N4 . Si2 . 132.90(8) yes Ti1 . N4 . C14 . 112.57(10) yes Si2 . N4 . C14 . 114.37(10) yes C17 . N5 . C21 . 120.1(12) yes C17 . N51 . C211 . 114.0(13) yes Ti1 . N6 . Ti1 6_555 98.27(7) yes Ti1 . N6 . C28 . 97.26(11) yes Ti1 6_555 N6 . C28 . 163.42(14) yes N3 . Si1 . C22 . 111.84(9) yes N3 . Si1 . C23 . 108.04(8) yes C22 . Si1 . C23 . 108.91(11) yes N3 . Si1 . C24 . 111.61(8) yes C22 . Si1 . C24 . 106.34(11) yes C23 . Si1 . C24 . 110.08(9) yes N4 . Si2 . C25 . 112.23(8) yes N4 . Si2 . C26 . 109.23(8) yes C25 . Si2 . C26 . 107.57(10) yes N4 . Si2 . C27 . 111.74(7) yes C25 . Si2 . C27 . 107.68(9) yes C26 . Si2 . C27 . 108.23(10) yes N2 . C1 . C2 . 119.76(17) yes N2 . C1 . C6 . 121.02(17) yes C2 . C1 . C6 . 119.22(18) yes C1 . C2 . C3 . 120.1(2) yes C1 . C2 . H21 . 119.8 no C3 . C2 . H21 . 120.1 no C2 . C3 . C4 . 120.9(3) yes C2 . C3 . H31 . 119.8 no C4 . C3 . H31 . 119.3 no C3 . C4 . C5 . 119.6(2) yes C3 . C4 . H41 . 120.3 no C5 . C4 . H41 . 120.1 no C4 . C5 . C6 . 120.6(2) yes C4 . C5 . H51 . 119.7 no C6 . C5 . H51 . 119.7 no C1 . C6 . C5 . 119.6(2) yes C1 . C6 . H61 . 120.0 no C5 . C6 . H61 . 120.4 no N2 . C7 . C8 . 119.43(15) yes N2 . C7 . C12 . 121.24(15) yes C8 . C7 . C12 . 119.20(16) yes C7 . C8 . C9 . 119.99(16) yes C7 . C8 . H81 . 119.9 no C9 . C8 . H81 . 120.1 no C8 . C9 . C10 . 121.00(17) yes C8 . C9 . H91 . 119.5 no C10 . C9 . H91 . 119.5 no C9 . C10 . C11 . 119.12(17) yes C9 . C10 . H101 . 120.3 no C11 . C10 . H101 . 120.5 no C10 . C11 . C12 . 120.75(17) yes C10 . C11 . H111 . 119.7 no C12 . C11 . H111 . 119.5 no C7 . C12 . C11 . 119.93(17) yes C7 . C12 . H121 . 119.8 no C11 . C12 . H121 . 120.2 no N3 . C13 . C15 . 114.69(14) yes N3 . C13 . H131 . 108.1 no C15 . C13 . H131 . 108.0 no N3 . C13 . H132 . 108.1 no C15 . C13 . H132 . 108.4 no H131 . C13 . H132 . 109.5 no N4 . C14 . C15 . 115.35(13) yes N4 . C14 . H141 . 107.6 no C15 . C14 . H141 . 107.7 no N4 . C14 . H142 . 108.3 no C15 . C14 . H142 . 108.4 no H141 . C14 . H142 . 109.5 no C13 . C15 . C14 . 110.73(14) yes C13 . C15 . C16 . 110.32(14) yes C14 . C15 . C16 . 111.12(14) yes C13 . C15 . C17 . 107.89(14) yes C14 . C15 . C17 . 105.78(13) yes C16 . C15 . C17 . 110.87(15) yes C15 . C16 . H161 . 109.4 no C15 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 109.5 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no C15 . C17 . N51 . 116.5(6) yes C15 . C17 . N5 . 115.9(6) yes N51 . C17 . N5 . 22.3(6) yes C15 . C17 . C18 . 122.04(18) yes N51 . C17 . C18 . 120.8(6) yes N5 . C17 . C18 . 120.2(6) yes C17 . C18 . C19 . 119.7(2) yes C17 . C18 . H181 . 119.7 no C19 . C18 . H181 . 120.5 no C18 . C19 . C20 . 119.2(3) yes C18 . C19 . H191 . 120.2 no C20 . C19 . H191 . 120.5 no C19 . C20 . C21 . 116.7(6) yes C19 . C20 . C211 . 117.3(8) yes C21 . C20 . C211 . 24.1(9) yes C19 . C20 . H201 . 120.9 no C21 . C20 . H201 . 119.8 no C211 . C20 . H201 . 121.3 no C20 . C21 . N5 . 121.1(12) yes C20 . C21 . H211 . 119.9 no N5 . C21 . H211 . 118.9 no N51 . C211 . C20 . 126.0(15) yes N51 . C211 . H2111 . 117.2 no C20 . C211 . H2111 . 116.8 no Si1 . C22 . H221 . 109.7 no Si1 . C22 . H222 . 109.4 no H221 . C22 . H222 . 109.5 no Si1 . C22 . H223 . 109.3 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no Si1 . C23 . H231 . 109.5 no Si1 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.5 no Si1 . C23 . H233 . 109.4 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no Si1 . C24 . H241 . 109.6 no Si1 . C24 . H242 . 109.3 no H241 . C24 . H242 . 109.5 no Si1 . C24 . H243 . 109.5 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no Si2 . C25 . H251 . 109.6 no Si2 . C25 . H252 . 109.6 no H251 . C25 . H252 . 109.5 no Si2 . C25 . H253 . 109.3 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no Si2 . C26 . H261 . 109.3 no Si2 . C26 . H262 . 109.7 no H261 . C26 . H262 . 109.5 no Si2 . C26 . H263 . 109.3 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no Si2 . C27 . H271 . 109.6 no Si2 . C27 . H272 . 109.3 no H271 . C27 . H272 . 109.5 no Si2 . C27 . H273 . 109.5 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no N6 . C28 . N1 . 112.37(15) yes N6 . C28 . C29 . 122.62(16) yes N1 . C28 . C29 . 125.01(15) yes C28 . C29 . H291 . 109.4 no C28 . C29 . H292 . 109.3 no H291 . C29 . H292 . 109.5 no C28 . C29 . H293 . 109.7 no H291 . C29 . H293 . 109.5 no H292 . C29 . H293 . 109.5 no C102 . C101 . C106 . 120.3(10) yes C102 . C101 . H1011 . 119.9 no C106 . C101 . H1011 . 119.8 no C101 . C102 . C103 . 119.0(11) yes C101 . C102 . H1021 . 122.6 no C103 . C102 . H1021 . 118.3 no C102 . C103 . C104 . 119.9(9) yes C102 . C103 . H1031 . 120.9 no C104 . C103 . H1031 . 119.1 no C103 . C104 . C105 . 120.0(9) yes C103 . C104 . H1041 . 119.3 no C105 . C104 . H1041 . 120.7 no C104 . C105 . C106 . 120.4(9) yes C104 . C105 . H1051 . 119.5 no C106 . C105 . H1051 . 120.1 no C105 . C106 . C101 . 120.3(9) yes C105 . C106 . H1061 . 118.9 no C101 . C106 . H1061 . 120.8 no #===end data_Compound_7 _database_code_depnum_ccdc_archive 'CCDC 698355' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Cp2Ti{N(NPh2)PCtBu} ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H29 N2 P Ti' _chemical_formula_weight 460.39 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' P P 0.1023 0.0942 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.654(3) _cell_length_b 9.4448(19) _cell_length_c 16.641(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.60(3) _cell_angle_gamma 90.00 _cell_volume 2303.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.919 _exptl_absorpt_correction_T_max 0.967 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9086 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4906 _reflns_number_gt 3892 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0491P)^2^+1.2132P] 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 4906 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.27106(2) 0.18615(4) -0.00085(2) 0.01766(11) Uani 1 1 d . . . P1 P 0.30465(3) 0.24674(5) 0.16544(3) 0.02014(13) Uani 1 1 d . . . N1 N 0.21731(10) 0.15564(16) 0.08894(11) 0.0197(4) Uani 1 1 d . . . C1 C 0.36252(13) 0.3007(2) 0.10320(13) 0.0203(4) Uani 1 1 d . . . N2 N 0.15298(11) 0.08464(16) 0.11492(12) 0.0228(4) Uani 1 1 d . . . C2 C 0.44484(14) 0.3997(2) 0.13470(15) 0.0293(5) Uani 1 1 d . . . C3 C 0.4929(2) 0.3916(4) 0.23184(17) 0.0604(9) Uani 1 1 d . . . H3A H 0.4501 0.4182 0.2603 0.091 Uiso 1 1 calc R . . H3B H 0.5449 0.4568 0.2494 0.091 Uiso 1 1 calc R . . H3C H 0.5145 0.2948 0.2482 0.091 Uiso 1 1 calc R . . C4 C 0.51357(15) 0.3617(3) 0.09119(19) 0.0426(6) Uani 1 1 d . . . H4A H 0.5370 0.2659 0.1082 0.064 Uiso 1 1 calc R . . H4B H 0.5643 0.4293 0.1089 0.064 Uiso 1 1 calc R . . H4C H 0.4833 0.3657 0.0287 0.064 Uiso 1 1 calc R . . C5 C 0.41369(16) 0.5533(2) 0.11099(18) 0.0403(6) Uani 1 1 d . . . H5A H 0.3828 0.5608 0.0487 0.060 Uiso 1 1 calc R . . H5B H 0.4669 0.6161 0.1292 0.060 Uiso 1 1 calc R . . H5C H 0.3715 0.5810 0.1399 0.060 Uiso 1 1 calc R . . C6 C 0.16854(12) -0.06226(19) 0.13540(13) 0.0198(4) Uani 1 1 d . . . C7 C 0.11783(13) -0.1624(2) 0.07723(14) 0.0224(4) Uani 1 1 d . . . H7 H 0.0733 -0.1334 0.0244 0.027 Uiso 1 1 calc R . . C8 C 0.13256(14) -0.3055(2) 0.09659(15) 0.0253(5) Uani 1 1 d . . . H8 H 0.0975 -0.3744 0.0571 0.030 Uiso 1 1 calc R . . C9 C 0.19771(13) -0.3481(2) 0.17283(14) 0.0245(5) Uani 1 1 d . . . H9 H 0.2078 -0.4461 0.1855 0.029 Uiso 1 1 calc R . . C10 C 0.24875(14) -0.2477(2) 0.23121(14) 0.0259(5) Uani 1 1 d . . . H10 H 0.2936 -0.2771 0.2837 0.031 Uiso 1 1 calc R . . C11 C 0.23398(13) -0.1044(2) 0.21257(14) 0.0228(4) Uani 1 1 d . . . H11 H 0.2685 -0.0355 0.2524 0.027 Uiso 1 1 calc R . . C12 C 0.08612(12) 0.15931(19) 0.13430(13) 0.0182(4) Uani 1 1 d . . . C13 C 0.02625(12) 0.0880(2) 0.16656(13) 0.0205(4) Uani 1 1 d . . . H13 H 0.0323 -0.0112 0.1764 0.025 Uiso 1 1 calc R . . C14 C -0.04174(13) 0.1621(2) 0.18415(14) 0.0234(4) Uani 1 1 d . . . H14 H -0.0815 0.1127 0.2063 0.028 Uiso 1 1 calc R . . C15 C -0.05286(13) 0.3068(2) 0.17000(14) 0.0246(4) Uani 1 1 d . . . H15 H -0.1003 0.3563 0.1811 0.030 Uiso 1 1 calc R . . C16 C 0.00700(13) 0.3774(2) 0.13923(14) 0.0235(4) Uani 1 1 d . . . H16 H 0.0007 0.4767 0.1300 0.028 Uiso 1 1 calc R . . C17 C 0.07586(13) 0.30615(19) 0.12173(13) 0.0194(4) Uani 1 1 d . . . H17 H 0.1163 0.3570 0.1011 0.023 Uiso 1 1 calc R . . C18 C 0.29646(17) 0.0099(3) -0.09531(16) 0.0368(6) Uani 1 1 d . . . H18 H 0.2648 0.0154 -0.1555 0.044 Uiso 1 1 calc R . . C19 C 0.26720(15) -0.0627(2) -0.03669(16) 0.0318(5) Uani 1 1 d . . . H19 H 0.2114 -0.1132 -0.0498 0.038 Uiso 1 1 calc R . . C20 C 0.33441(14) -0.0482(2) 0.04503(15) 0.0269(5) Uani 1 1 d . . . H20 H 0.3328 -0.0889 0.0967 0.032 Uiso 1 1 calc R . . C21 C 0.40426(14) 0.0365(2) 0.03717(15) 0.0297(5) Uani 1 1 d . . . H21 H 0.4581 0.0644 0.0826 0.036 Uiso 1 1 calc R . . C22 C 0.38091(16) 0.0734(2) -0.04982(17) 0.0359(6) Uani 1 1 d . . . H22 H 0.4159 0.1308 -0.0736 0.043 Uiso 1 1 calc R . . C23 C 0.14851(14) 0.2347(2) -0.13252(14) 0.0281(5) Uani 1 1 d . . . H23 H 0.1151 0.1572 -0.1650 0.034 Uiso 1 1 calc R . . C24 C 0.12896(14) 0.3075(2) -0.06720(15) 0.0272(5) Uani 1 1 d . . . H24 H 0.0791 0.2893 -0.0487 0.033 Uiso 1 1 calc R . . C25 C 0.19628(14) 0.4118(2) -0.03421(14) 0.0266(5) Uani 1 1 d . . . H25 H 0.2005 0.4755 0.0112 0.032 Uiso 1 1 calc R . . C26 C 0.25624(15) 0.4054(2) -0.08025(14) 0.0278(5) Uani 1 1 d . . . H26 H 0.3080 0.4642 -0.0715 0.033 Uiso 1 1 calc R . . C27 C 0.22647(15) 0.2975(2) -0.14093(14) 0.0288(5) Uani 1 1 d . . . H27 H 0.2541 0.2709 -0.1811 0.035 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 0.01525(18) 0.01898(18) 0.0198(2) -0.00040(14) 0.00748(14) 0.00175(12) P1 0.0208(3) 0.0200(3) 0.0215(3) -0.0001(2) 0.0098(2) -0.00242(19) N1 0.0178(8) 0.0166(8) 0.0276(10) 0.0010(7) 0.0115(7) -0.0016(6) C1 0.0173(9) 0.0223(10) 0.0223(11) 0.0009(8) 0.0081(8) -0.0009(7) N2 0.0198(8) 0.0139(7) 0.0407(11) 0.0045(7) 0.0179(8) 0.0008(6) C2 0.0231(10) 0.0371(12) 0.0266(12) 0.0020(10) 0.0074(9) -0.0114(9) C3 0.0504(16) 0.086(2) 0.0307(15) 0.0038(15) -0.0025(13) -0.0445(16) C4 0.0240(11) 0.0436(14) 0.0628(19) 0.0048(13) 0.0185(12) -0.0084(10) C5 0.0362(13) 0.0326(12) 0.0542(17) -0.0114(12) 0.0185(12) -0.0160(10) C6 0.0177(9) 0.0158(9) 0.0300(12) 0.0012(8) 0.0136(8) 0.0008(7) C7 0.0208(9) 0.0218(10) 0.0239(11) 0.0018(8) 0.0068(8) 0.0006(7) C8 0.0267(10) 0.0182(9) 0.0308(12) -0.0042(9) 0.0097(9) -0.0040(8) C9 0.0266(10) 0.0157(9) 0.0336(13) 0.0023(9) 0.0137(9) 0.0007(8) C10 0.0255(10) 0.0229(10) 0.0263(12) 0.0041(9) 0.0052(9) -0.0001(8) C11 0.0225(10) 0.0189(9) 0.0274(12) -0.0034(8) 0.0092(9) -0.0044(7) C12 0.0145(8) 0.0174(9) 0.0223(10) -0.0016(8) 0.0058(8) -0.0001(7) C13 0.0196(9) 0.0182(9) 0.0247(11) 0.0009(8) 0.0089(8) -0.0011(7) C14 0.0176(9) 0.0278(10) 0.0256(11) -0.0020(9) 0.0085(8) -0.0035(8) C15 0.0183(9) 0.0293(11) 0.0276(12) -0.0046(9) 0.0097(9) 0.0044(8) C16 0.0241(10) 0.0175(9) 0.0280(12) 0.0000(8) 0.0081(9) 0.0038(8) C17 0.0200(9) 0.0164(9) 0.0230(11) 0.0003(8) 0.0091(8) -0.0010(7) C18 0.0475(14) 0.0348(13) 0.0274(13) -0.0071(10) 0.0122(11) 0.0173(11) C19 0.0318(12) 0.0234(11) 0.0378(14) -0.0082(10) 0.0091(10) 0.0056(9) C20 0.0277(10) 0.0228(10) 0.0303(12) 0.0013(9) 0.0102(9) 0.0115(8) C21 0.0218(10) 0.0311(11) 0.0361(13) -0.0034(10) 0.0101(9) 0.0098(8) C22 0.0377(13) 0.0351(12) 0.0468(15) 0.0023(11) 0.0296(12) 0.0121(10) C23 0.0244(10) 0.0287(11) 0.0248(12) 0.0027(9) 0.0005(9) 0.0022(8) C24 0.0187(10) 0.0333(11) 0.0297(12) 0.0096(10) 0.0086(9) 0.0081(8) C25 0.0316(11) 0.0229(10) 0.0241(12) 0.0042(9) 0.0083(9) 0.0083(9) C26 0.0288(11) 0.0259(10) 0.0290(12) 0.0073(9) 0.0106(10) -0.0012(8) C27 0.0354(12) 0.0328(11) 0.0211(11) 0.0067(9) 0.0135(10) 0.0076(9) _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 N1 1.9770(17) . ? Ti1 C1 2.115(2) . ? Ti1 C23 2.395(2) . ? Ti1 C22 2.396(2) . ? Ti1 C24 2.398(2) . ? Ti1 C25 2.401(2) . ? Ti1 C21 2.412(2) . ? Ti1 C18 2.417(2) . ? Ti1 C19 2.420(2) . ? Ti1 C26 2.423(2) . ? Ti1 C27 2.425(2) . ? Ti1 C20 2.436(2) . ? P1 C1 1.677(2) . ? P1 N1 1.7336(18) . ? N1 N2 1.399(2) . ? C1 C2 1.528(3) . ? N2 C12 1.391(2) . ? N2 C6 1.429(2) . ? C2 C3 1.526(3) . ? C2 C4 1.536(3) . ? C2 C5 1.538(3) . ? C6 C7 1.386(3) . ? C6 C11 1.390(3) . ? C7 C8 1.390(3) . ? C8 C9 1.379(3) . ? C9 C10 1.391(3) . ? C10 C11 1.390(3) . ? C12 C17 1.403(3) . ? C12 C13 1.405(3) . ? C13 C14 1.388(3) . ? C14 C15 1.387(3) . ? C15 C16 1.387(3) . ? C16 C17 1.386(3) . ? C18 C19 1.395(4) . ? C18 C22 1.406(4) . ? C19 C20 1.403(3) . ? C20 C21 1.398(3) . ? C21 C22 1.406(3) . ? C23 C27 1.408(3) . ? C23 C24 1.408(3) . ? C24 C25 1.406(3) . ? C25 C26 1.406(3) . ? C26 C27 1.394(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti1 C1 78.54(7) . . ? N1 Ti1 C23 107.61(8) . . ? C1 Ti1 C23 138.14(8) . . ? N1 Ti1 C22 137.68(8) . . ? C1 Ti1 C22 98.38(8) . . ? C23 Ti1 C22 102.33(9) . . ? N1 Ti1 C24 81.09(7) . . ? C1 Ti1 C24 112.55(8) . . ? C23 Ti1 C24 34.17(8) . . ? C22 Ti1 C24 135.73(9) . . ? N1 Ti1 C25 90.09(7) . . ? C1 Ti1 C25 82.51(8) . . ? C23 Ti1 C25 56.64(7) . . ? C22 Ti1 C25 131.75(8) . . ? C24 Ti1 C25 34.06(7) . . ? N1 Ti1 C21 105.96(8) . . ? C1 Ti1 C21 79.12(8) . . ? C23 Ti1 C21 133.83(8) . . ? C22 Ti1 C21 34.02(8) . . ? C24 Ti1 C21 167.67(8) . . ? C25 Ti1 C21 152.50(8) . . ? N1 Ti1 C18 127.04(8) . . ? C1 Ti1 C18 131.76(8) . . ? C23 Ti1 C18 78.39(8) . . ? C22 Ti1 C18 33.96(8) . . ? C24 Ti1 C18 111.58(9) . . ? C25 Ti1 C18 129.76(8) . . ? C21 Ti1 C18 56.09(8) . . ? N1 Ti1 C19 93.69(8) . . ? C1 Ti1 C19 130.51(8) . . ? C23 Ti1 C19 91.02(8) . . ? C22 Ti1 C19 56.17(8) . . ? C24 Ti1 C19 114.32(8) . . ? C25 Ti1 C19 146.85(8) . . ? C21 Ti1 C19 55.94(8) . . ? C18 Ti1 C19 33.52(8) . . ? N1 Ti1 C26 123.52(7) . . ? C1 Ti1 C26 85.22(8) . . ? C23 Ti1 C26 56.31(7) . . ? C22 Ti1 C26 97.86(8) . . ? C24 Ti1 C26 56.31(7) . . ? C25 Ti1 C26 33.90(7) . . ? C21 Ti1 C26 123.49(8) . . ? C18 Ti1 C26 103.89(8) . . ? C19 Ti1 C26 134.92(8) . . ? N1 Ti1 C27 137.27(7) . . ? C1 Ti1 C27 116.61(8) . . ? C23 Ti1 C27 33.95(8) . . ? C22 Ti1 C27 82.19(8) . . ? C24 Ti1 C27 56.19(8) . . ? C25 Ti1 C27 56.00(8) . . ? C21 Ti1 C27 115.86(8) . . ? C18 Ti1 C27 74.40(8) . . ? C19 Ti1 C27 102.15(8) . . ? C26 Ti1 C27 33.42(7) . . ? N1 Ti1 C20 82.26(7) . . ? C1 Ti1 C20 97.16(8) . . ? C23 Ti1 C20 124.57(8) . . ? C22 Ti1 C20 56.01(8) . . ? C24 Ti1 C20 141.99(7) . . ? C25 Ti1 C20 172.24(8) . . ? C21 Ti1 C20 33.51(7) . . ? C18 Ti1 C20 55.65(8) . . ? C19 Ti1 C20 33.58(8) . . ? C26 Ti1 C20 153.86(8) . . ? C27 Ti1 C20 130.02(8) . . ? C1 P1 N1 98.93(9) . . ? N2 N1 P1 118.59(14) . . ? N2 N1 Ti1 147.94(14) . . ? P1 N1 Ti1 92.70(7) . . ? C2 C1 P1 123.21(16) . . ? C2 C1 Ti1 147.16(16) . . ? P1 C1 Ti1 89.60(8) . . ? C12 N2 N1 120.72(15) . . ? C12 N2 C6 121.07(16) . . ? N1 N2 C6 117.28(15) . . ? C3 C2 C1 112.01(18) . . ? C3 C2 C4 108.8(2) . . ? C1 C2 C4 109.97(19) . . ? C3 C2 C5 108.2(2) . . ? C1 C2 C5 109.66(17) . . ? C4 C2 C5 108.11(19) . . ? C7 C6 C11 120.34(17) . . ? C7 C6 N2 119.22(18) . . ? C11 C6 N2 120.44(17) . . ? C6 C7 C8 119.61(19) . . ? C9 C8 C7 120.38(19) . . ? C8 C9 C10 120.05(18) . . ? C11 C10 C9 119.90(19) . . ? C6 C11 C10 119.72(18) . . ? N2 C12 C17 121.51(17) . . ? N2 C12 C13 120.21(17) . . ? C17 C12 C13 118.28(17) . . ? C14 C13 C12 120.20(18) . . ? C15 C14 C13 121.36(19) . . ? C16 C15 C14 118.40(18) . . ? C17 C16 C15 121.39(18) . . ? C16 C17 C12 120.35(18) . . ? C19 C18 C22 108.1(2) . . ? C19 C18 Ti1 73.38(13) . . ? C22 C18 Ti1 72.21(13) . . ? C18 C19 C20 108.1(2) . . ? C18 C19 Ti1 73.10(13) . . ? C20 C19 Ti1 73.82(12) . . ? C21 C20 C19 108.0(2) . . ? C21 C20 Ti1 72.30(12) . . ? C19 C20 Ti1 72.60(12) . . ? C20 C21 C22 108.0(2) . . ? C20 C21 Ti1 74.19(11) . . ? C22 C21 Ti1 72.38(12) . . ? C18 C22 C21 107.7(2) . . ? C18 C22 Ti1 73.83(12) . . ? C21 C22 Ti1 73.60(12) . . ? C27 C23 C24 107.6(2) . . ? C27 C23 Ti1 74.22(12) . . ? C24 C23 Ti1 73.06(12) . . ? C25 C24 C23 107.90(19) . . ? C25 C24 Ti1 73.07(12) . . ? C23 C24 Ti1 72.77(12) . . ? C24 C25 C26 108.0(2) . . ? C24 C25 Ti1 72.87(12) . . ? C26 C25 Ti1 73.91(12) . . ? C27 C26 C25 108.01(19) . . ? C27 C26 Ti1 73.38(12) . . ? C25 C26 Ti1 72.19(12) . . ? C26 C27 C23 108.5(2) . . ? C26 C27 Ti1 73.20(13) . . ? C23 C27 Ti1 71.83(12) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.341 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.069 #===end