# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _publ_contact_author_name 'Klaus Harms' _publ_contact_author_email harms@chemie.uni-marburg.de loop_ _publ_author_name W.Darwish E.Seikel R.Kaesmarker K.Harms J.Sundermeyer #===END # Attachment '- 3a_dalton_transactions_K11.cif' #data_3a #TrackingRef '- 3a_dalton_transactions_K11.cif' data_k11 _database_code_depnum_ccdc_archive 'CCDC 269282' #TrackingRef '- 3a_dalton_transactions_K11.cif' _audit_creation_date 2005-04-18T15:59:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '(C47 H30 N10 O Ti), 1.5(C6 H5 Cl)' _chemical_formula_sum 'C56 H37.50 Cl1.50 N10 O Ti' _chemical_formula_weight 967.53 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3080(17) _cell_length_b 12.5821(14) _cell_length_c 16.717(2) _cell_angle_alpha 70.981(10) _cell_angle_beta 78.757(11) _cell_angle_gamma 68.628(10) _cell_volume 2270.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8506 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 26 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 998 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.332 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.1148 _diffrn_reflns_av_unetI/netI 0.1667 _diffrn_reflns_number 15399 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 23 _diffrn_reflns_theta_full 23 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 6330 _reflns_number_gt 3220 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0388P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_number_reflns 6330 _refine_ls_number_parameters 648 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1528 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1321 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.922 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.844 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.062 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2 C 0.2309(5) 0.6136(5) 0.0311(4) 0.0253(14) Uani 1 1 d . . . C3 C 0.3267(5) 0.6322(5) -0.0326(4) 0.0252(14) Uani 1 1 d . . . C4 C 0.3832(5) 0.7178(5) -0.0555(4) 0.0307(15) Uani 1 1 d . . . H4 H 0.3622 0.7775 -0.027 0.037 Uiso 1 1 calc R . . C5 C 0.4702(6) 0.7118(5) -0.1208(4) 0.0368(17) Uani 1 1 d . . . H5 H 0.5102 0.7685 -0.1375 0.044 Uiso 1 1 calc R . . C6 C 0.5019(5) 0.6244(5) -0.1637(4) 0.0355(16) Uani 1 1 d . . . H6 H 0.5618 0.6239 -0.2092 0.043 Uiso 1 1 calc R . . C7 C 0.4471(5) 0.5385(5) -0.1408(4) 0.0318(16) Uani 1 1 d . . . H7 H 0.4689 0.4785 -0.169 0.038 Uiso 1 1 calc R . . C8 C 0.3587(5) 0.5443(5) -0.0744(4) 0.0246(14) Uani 1 1 d . . . C9 C 0.2834(5) 0.4704(5) -0.0355(4) 0.0262(14) Uani 1 1 d . . . C11 C 0.2103(5) 0.3219(5) -0.0301(4) 0.0277(15) Uani 1 1 d . . . C13 C 0.0731(5) 0.2492(5) 0.0512(4) 0.0243(14) Uani 1 1 d . . . C14 C 0.1280(5) 0.1758(5) -0.0063(4) 0.0273(15) Uani 1 1 d . . . C15 C 0.1133(5) 0.0749(5) -0.0122(4) 0.0312(15) Uani 1 1 d . . . H15 H 0.0558 0.0435 0.0238 0.037 Uiso 1 1 calc R . . C16 C 0.1856(5) 0.0215(5) -0.0725(4) 0.0331(16) Uani 1 1 d . . . H16 H 0.1778 -0.0482 -0.0778 0.04 Uiso 1 1 calc R . . C17 C 0.2706(6) 0.0684(5) -0.1261(4) 0.0348(16) Uani 1 1 d . . . H17 H 0.3187 0.03 -0.1671 0.042 Uiso 1 1 calc R . . C18 C 0.2854(5) 0.1696(5) -0.1200(4) 0.0304(15) Uani 1 1 d . . . H18 H 0.3422 0.2016 -0.1566 0.036 Uiso 1 1 calc R . . C19 C 0.2140(5) 0.2227(5) -0.0587(4) 0.0270(14) Uani 1 1 d . . . C21 C -0.0614(5) 0.2956(5) 0.1645(4) 0.0273(15) Uani 1 1 d . . . C23 C -0.1110(5) 0.4364(5) 0.2319(4) 0.0284(15) Uani 1 1 d . . . C24 C -0.1941(5) 0.3697(5) 0.2670(4) 0.0288(15) Uani 1 1 d . . . C25 C -0.2877(6) 0.3823(6) 0.3279(4) 0.0392(17) Uani 1 1 d . . . H25 H -0.3103 0.4434 0.3553 0.047 Uiso 1 1 calc R . . C26 C -0.3472(6) 0.3006(6) 0.3471(4) 0.0460(18) Uani 1 1 d . . . H26 H -0.411 0.305 0.3897 0.055 Uiso 1 1 calc R . . C27 C -0.3160(6) 0.2126(6) 0.3056(4) 0.0436(18) Uani 1 1 d . . . H27 H -0.3589 0.1586 0.3203 0.052 Uiso 1 1 calc R . . C28 C -0.2232(6) 0.2027(6) 0.2434(4) 0.0364(17) Uani 1 1 d . . . H28 H -0.2035 0.1444 0.2138 0.044 Uiso 1 1 calc R . . C29 C -0.1598(5) 0.2809(5) 0.2254(4) 0.0293(15) Uani 1 1 d . . . C31 C -0.0489(5) 0.5945(5) 0.2203(4) 0.0272(14) Uani 1 1 d . . . C33 C 0.0858(5) 0.6687(5) 0.1360(4) 0.0257(14) Uani 1 1 d . . . C34 C 0.0281(5) 0.7464(5) 0.1912(4) 0.0285(15) Uani 1 1 d . . . C35 C 0.0450(5) 0.8447(5) 0.1992(4) 0.0299(15) Uani 1 1 d . . . H35 H 0.1006 0.8779 0.162 0.036 Uiso 1 1 calc R . . C36 C -0.0221(6) 0.8935(5) 0.2636(4) 0.0368(17) Uani 1 1 d . . . H36 H -0.0111 0.9604 0.2712 0.044 Uiso 1 1 calc R . . C37 C -0.1063(6) 0.8453(6) 0.3179(4) 0.0407(17) Uani 1 1 d . . . H37 H -0.1503 0.8799 0.3618 0.049 Uiso 1 1 calc R . . C38 C -0.1257(6) 0.7490(5) 0.3083(4) 0.0328(16) Uani 1 1 d . . . H38 H -0.1841 0.7181 0.3434 0.039 Uiso 1 1 calc R . . C39 C -0.0556(5) 0.6986(5) 0.2445(4) 0.0288(15) Uani 1 1 d . . . C41 C 0.2648(5) 0.2676(5) 0.2465(4) 0.0247(14) Uani 1 1 d . . . C43 C 0.2823(5) 0.1295(5) 0.1684(3) 0.0230(13) Uani 1 1 d . . . C44 C 0.2333(5) 0.0477(5) 0.2273(4) 0.0274(14) Uani 1 1 d . . . H44 H 0.1741 0.0721 0.2697 0.033 Uiso 1 1 calc R . . C45 C 0.2709(5) -0.0689(5) 0.2240(4) 0.0277(14) Uani 1 1 d . . . H45 H 0.2382 -0.1241 0.2651 0.033 Uiso 1 1 calc R . . C46 C 0.3559(5) -0.1071(5) 0.1614(4) 0.0286(15) Uani 1 1 d . . . C47 C 0.4021(5) -0.0245(5) 0.1026(4) 0.0279(14) Uani 1 1 d . . . H47 H 0.4589 -0.0482 0.0588 0.033 Uiso 1 1 calc R . . C48 C 0.3672(5) 0.0939(5) 0.1058(4) 0.0279(14) Uani 1 1 d . . . H48 H 0.4013 0.1487 0.0657 0.034 Uiso 1 1 calc R . . C49 C 0.3964(6) -0.2358(5) 0.1574(4) 0.0366(16) Uani 1 1 d . . . H49A H 0.334 -0.2498 0.1379 0.055 Uiso 1 1 calc R . . H49B H 0.4143 -0.2899 0.2141 0.055 Uiso 1 1 calc R . . H49C H 0.4667 -0.25 0.1178 0.055 Uiso 1 1 calc R . . C51 C 0.1945(5) 0.4418(5) 0.3011(4) 0.0267(14) Uani 1 1 d . . . C52 C 0.2433(5) 0.5314(5) 0.2851(4) 0.0266(14) Uani 1 1 d . . . H52 H 0.2841 0.5558 0.2316 0.032 Uiso 1 1 calc R . . C53 C 0.2311(6) 0.5849(6) 0.3493(4) 0.0360(16) Uani 1 1 d . . . H53 H 0.2618 0.648 0.338 0.043 Uiso 1 1 calc R . . C54 C 0.1755(6) 0.5485(6) 0.4287(4) 0.0363(16) Uani 1 1 d . . . C55 C 0.1314(6) 0.4558(6) 0.4437(4) 0.0371(16) Uani 1 1 d . . . H55 H 0.0948 0.4279 0.4982 0.045 Uiso 1 1 calc R . . C56 C 0.1398(5) 0.4032(5) 0.3802(4) 0.0312(15) Uani 1 1 d . . . H56 H 0.1081 0.3408 0.3913 0.037 Uiso 1 1 calc R . . C57 C 0.1621(7) 0.6115(7) 0.4958(5) 0.058(2) Uani 1 1 d . . . H57A H 0.2299 0.6378 0.4891 0.086 Uiso 1 1 calc R . . H57B H 0.1572 0.5566 0.5525 0.086 Uiso 1 1 calc R . . H57C H 0.0905 0.6805 0.489 0.086 Uiso 1 1 calc R . . C101 C 0.4662(7) 0.2457(7) 0.5912(6) 0.058(2) Uani 1 1 d . . . C102 C 0.4953(7) 0.1323(9) 0.6460(5) 0.067(2) Uani 1 1 d . . . H102 H 0.5374 0.1122 0.6937 0.081 Uiso 1 1 calc R . . C103 C 0.4618(7) 0.0492(8) 0.6293(6) 0.066(2) Uani 1 1 d . . . H103 H 0.4808 -0.0294 0.6661 0.08 Uiso 1 1 calc R . . C106 C 0.4059(6) 0.2748(7) 0.5201(5) 0.056(2) Uani 1 1 d . . . H106 H 0.3871 0.3525 0.4821 0.068 Uiso 1 1 calc R . . C105 C 0.3745(7) 0.1872(8) 0.5066(5) 0.060(2) Uani 1 1 d . . . H105 H 0.3335 0.2039 0.459 0.073 Uiso 1 1 calc R . . C104 C 0.4031(8) 0.0774(8) 0.5624(6) 0.067(2) Uani 1 1 d . . . H104 H 0.3802 0.018 0.5533 0.081 Uiso 1 1 calc R . . N1 N 0.2106(4) 0.5117(4) 0.0303(3) 0.0254(12) Uani 1 1 d . . . N10 N 0.2839(4) 0.3840(4) -0.0632(3) 0.0261(12) Uani 1 1 d . . . N12 N 0.1255(4) 0.3359(4) 0.0368(3) 0.0243(12) Uani 1 1 d . . . N20 N -0.0123(4) 0.2298(4) 0.1112(3) 0.0292(12) Uani 1 1 d . . . N22 N -0.0309(4) 0.3881(4) 0.1715(3) 0.0261(12) Uani 1 1 d . . . N30 N -0.1171(4) 0.5288(4) 0.2566(3) 0.0292(12) Uani 1 1 d . . . N32 N 0.0398(4) 0.5779(4) 0.1549(3) 0.0243(12) Uani 1 1 d . . . N40 N 0.1762(4) 0.6855(4) 0.0795(3) 0.0273(12) Uani 1 1 d . . . N42 N 0.2422(4) 0.2511(4) 0.1735(3) 0.0242(11) Uani 1 1 d . . . N50 N 0.2013(4) 0.3886(4) 0.2351(3) 0.0236(11) Uani 1 1 d . . . Ti1 Ti 0.13026(10) 0.41230(9) 0.13076(7) 0.0226(3) Uani 1 1 d . . . O41 O 0.3245(4) 0.1981(3) 0.3042(3) 0.0326(10) Uani 1 1 d . . . Cl1 Cl 0.5101(3) 0.3558(3) 0.6044(3) 0.1338(13) Uani 1 1 d . . . Cl2 Cl -0.1530(6) -0.0756(6) 0.5512(4) 0.074(2) Uani 0.5 1 d P A -1 C201 C -0.0380(10) -0.0216(11) 0.5106(8) 0.050(4) Uani 0.5 1 d PGU A -1 C202 C 0.0729(13) -0.0885(9) 0.5378(7) 0.066(8) Uani 0.5 1 d PGU A -1 H202 H 0.0842 -0.1623 0.5804 0.079 Uiso 0.5 1 calc PR A -1 C203 C 0.1672(9) -0.0475(11) 0.5025(9) 0.071(5) Uani 0.5 1 d PGU A -1 H203 H 0.243 -0.0933 0.5211 0.086 Uiso 0.5 1 calc PR A -1 C204 C 0.1506(8) 0.0604(12) 0.4402(9) 0.075(10) Uani 0.5 1 d PGU A -1 H204 H 0.2151 0.0885 0.4161 0.09 Uiso 0.5 1 calc PR A -1 C205 C 0.0398(10) 0.1274(8) 0.4130(6) 0.041(3) Uani 0.5 1 d PGU A -1 H205 H 0.0284 0.2012 0.3704 0.05 Uiso 0.5 1 calc PR A -1 C206 C -0.0545(8) 0.0864(10) 0.4483(7) 0.041(7) Uani 0.5 1 d PGU A -1 H206 H -0.1303 0.1322 0.4298 0.05 Uiso 0.5 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.030(4) 0.023(3) 0.027(3) -0.011(3) -0.006(3) -0.008(3) C3 0.027(4) 0.021(3) 0.028(4) -0.005(3) -0.007(3) -0.008(3) C4 0.033(4) 0.030(3) 0.034(4) -0.014(3) -0.005(3) -0.010(3) C5 0.034(4) 0.034(4) 0.054(5) -0.019(3) -0.007(4) -0.017(3) C6 0.021(4) 0.037(4) 0.046(4) -0.017(3) 0.009(3) -0.008(3) C7 0.033(4) 0.027(3) 0.038(4) -0.012(3) -0.002(3) -0.010(3) C8 0.019(3) 0.025(3) 0.029(4) -0.009(3) -0.003(3) -0.005(3) C9 0.026(4) 0.023(3) 0.029(4) -0.008(3) -0.006(3) -0.005(3) C11 0.033(4) 0.020(3) 0.030(4) -0.010(3) -0.011(3) -0.002(3) C13 0.025(3) 0.017(3) 0.029(3) -0.005(3) -0.013(3) 0.000(3) C14 0.034(4) 0.020(3) 0.029(4) -0.008(3) -0.009(3) -0.007(3) C15 0.032(4) 0.028(4) 0.040(4) -0.010(3) -0.013(3) -0.011(3) C16 0.031(4) 0.027(3) 0.044(4) -0.023(3) -0.008(3) 0.002(3) C17 0.032(4) 0.028(4) 0.045(4) -0.021(3) -0.009(3) 0.001(3) C18 0.035(4) 0.027(3) 0.029(4) -0.007(3) -0.002(3) -0.011(3) C19 0.027(4) 0.022(3) 0.030(4) -0.009(3) -0.011(3) -0.001(3) C21 0.022(4) 0.028(3) 0.029(4) -0.006(3) -0.008(3) -0.004(3) C23 0.025(4) 0.028(3) 0.029(4) -0.007(3) -0.008(3) -0.003(3) C24 0.031(4) 0.033(4) 0.026(4) -0.009(3) -0.006(3) -0.011(3) C25 0.032(4) 0.051(4) 0.038(4) -0.015(3) 0.004(3) -0.019(4) C26 0.043(5) 0.059(5) 0.042(4) -0.012(4) 0.001(4) -0.026(4) C27 0.047(5) 0.051(4) 0.038(4) -0.005(4) -0.002(4) -0.029(4) C28 0.037(4) 0.038(4) 0.038(4) -0.012(3) -0.004(3) -0.016(3) C29 0.026(4) 0.029(3) 0.033(4) -0.010(3) -0.010(3) -0.005(3) C31 0.029(4) 0.028(3) 0.026(4) -0.011(3) -0.003(3) -0.006(3) C33 0.027(4) 0.024(3) 0.028(4) -0.010(3) -0.007(3) -0.005(3) C34 0.033(4) 0.021(3) 0.029(4) -0.007(3) -0.014(3) -0.001(3) C35 0.030(4) 0.027(3) 0.036(4) -0.016(3) -0.005(3) -0.005(3) C36 0.044(4) 0.027(4) 0.048(4) -0.018(3) -0.008(4) -0.013(3) C37 0.044(4) 0.044(4) 0.039(4) -0.025(3) -0.004(3) -0.008(3) C38 0.033(4) 0.037(4) 0.028(4) -0.015(3) -0.003(3) -0.005(3) C39 0.030(4) 0.023(3) 0.028(4) -0.005(3) -0.007(3) -0.002(3) C41 0.021(3) 0.025(3) 0.030(4) -0.008(3) -0.006(3) -0.007(3) C43 0.024(3) 0.020(3) 0.023(3) -0.003(3) -0.009(3) -0.004(3) C44 0.022(3) 0.024(3) 0.036(4) -0.013(3) -0.002(3) -0.003(3) C45 0.033(4) 0.024(3) 0.029(4) -0.008(3) -0.003(3) -0.012(3) C46 0.035(4) 0.020(3) 0.036(4) -0.010(3) -0.009(3) -0.011(3) C47 0.025(4) 0.027(3) 0.026(4) -0.008(3) -0.007(3) 0.002(3) C48 0.027(4) 0.024(3) 0.031(4) -0.009(3) -0.004(3) -0.005(3) C49 0.040(4) 0.025(3) 0.045(4) -0.014(3) 0.000(3) -0.010(3) C51 0.019(3) 0.028(3) 0.029(4) -0.012(3) -0.007(3) 0.002(3) C52 0.027(4) 0.028(3) 0.028(3) -0.011(3) -0.004(3) -0.007(3) C53 0.040(4) 0.037(4) 0.037(4) -0.015(3) -0.006(3) -0.014(3) C54 0.042(4) 0.043(4) 0.029(4) -0.018(3) -0.011(3) -0.007(3) C55 0.042(4) 0.045(4) 0.026(4) -0.017(3) 0.001(3) -0.012(3) C56 0.033(4) 0.028(3) 0.034(4) -0.011(3) -0.001(3) -0.010(3) C57 0.066(6) 0.071(5) 0.050(5) -0.043(4) 0.003(4) -0.020(4) C101 0.035(5) 0.062(5) 0.090(7) -0.036(5) -0.009(5) -0.016(4) C102 0.038(5) 0.101(7) 0.048(5) -0.018(5) -0.015(4) -0.004(5) C103 0.051(6) 0.058(5) 0.083(7) -0.007(5) -0.014(5) -0.016(4) C106 0.027(4) 0.052(5) 0.065(6) 0.000(4) -0.001(4) 0.000(4) C105 0.058(6) 0.072(6) 0.051(5) -0.015(5) -0.010(4) -0.020(5) C104 0.069(6) 0.074(6) 0.066(6) -0.022(5) -0.015(5) -0.023(5) N1 0.029(3) 0.025(3) 0.028(3) -0.012(2) -0.003(2) -0.010(2) N10 0.031(3) 0.021(3) 0.030(3) -0.008(2) -0.005(2) -0.009(2) N12 0.027(3) 0.018(3) 0.027(3) -0.006(2) -0.003(2) -0.007(2) N20 0.031(3) 0.030(3) 0.030(3) -0.007(2) -0.006(3) -0.012(2) N22 0.023(3) 0.022(3) 0.033(3) -0.014(2) -0.002(2) -0.002(2) N30 0.025(3) 0.031(3) 0.031(3) -0.013(2) 0.000(2) -0.005(2) N32 0.027(3) 0.023(3) 0.024(3) -0.009(2) -0.006(2) -0.007(2) N40 0.029(3) 0.023(3) 0.033(3) -0.012(2) -0.005(3) -0.007(2) N42 0.023(3) 0.022(3) 0.029(3) -0.005(2) -0.008(2) -0.007(2) N50 0.028(3) 0.019(3) 0.025(3) -0.007(2) -0.004(2) -0.006(2) Ti1 0.0247(6) 0.0199(6) 0.0238(6) -0.0075(5) -0.0051(5) -0.0052(5) O41 0.035(3) 0.026(2) 0.037(3) -0.013(2) -0.014(2) 0.000(2) Cl1 0.089(2) 0.119(2) 0.235(4) -0.097(3) -0.031(2) -0.0302(18) Cl2 0.098(6) 0.085(4) 0.056(4) -0.018(3) 0.006(4) -0.060(4) C201 0.071(12) 0.051(9) 0.032(8) -0.009(7) -0.005(8) -0.028(8) C202 0.077(15) 0.063(16) 0.064(15) -0.005(13) -0.024(13) -0.033(13) C203 0.063(12) 0.076(12) 0.067(12) -0.006(9) -0.033(9) -0.012(10) C204 0.084(18) 0.14(2) 0.053(16) -0.044(14) 0.011(14) -0.088(16) C205 0.037(8) 0.051(8) 0.039(8) -0.010(7) -0.005(7) -0.018(7) C206 0.048(12) 0.024(11) 0.035(10) -0.001(8) -0.006(10) 0.003(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C2 N40 1.322(7) . ? C2 N1 1.397(7) . ? C2 C3 1.459(8) . ? C3 C8 1.395(8) . ? C3 C4 1.401(8) . ? C4 C5 1.372(8) . ? C4 H4 0.95 . ? C5 C6 1.403(8) . ? C5 H5 0.95 . ? C6 C7 1.388(8) . ? C6 H6 0.95 . ? C7 C8 1.394(8) . ? C7 H7 0.95 . ? C8 C9 1.465(8) . ? C9 N10 1.310(7) . ? C9 N1 1.390(7) . ? C11 N10 1.332(7) . ? C11 N12 1.382(7) . ? C11 C19 1.457(8) . ? C13 N20 1.336(7) . ? C13 N12 1.395(7) . ? C13 C14 1.450(8) . ? C14 C15 1.382(8) . ? C14 C19 1.412(8) . ? C15 C16 1.384(8) . ? C15 H15 0.95 . ? C16 C17 1.409(9) . ? C16 H16 0.95 . ? C17 C18 1.387(8) . ? C17 H17 0.95 . ? C18 C19 1.392(8) . ? C18 H18 0.95 . ? C21 N20 1.324(7) . ? C21 N22 1.390(7) . ? C21 C29 1.448(8) . ? C23 N30 1.328(7) . ? C23 N22 1.392(7) . ? C23 C24 1.471(8) . ? C24 C25 1.379(8) . ? C24 C29 1.401(8) . ? C25 C26 1.393(9) . ? C25 H25 0.95 . ? C26 C27 1.393(9) . ? C26 H26 0.95 . ? C27 C28 1.386(9) . ? C27 H27 0.95 . ? C28 C29 1.394(8) . ? C28 H28 0.95 . ? C31 N30 1.318(7) . ? C31 N32 1.395(7) . ? C31 C39 1.462(8) . ? C33 N40 1.344(7) . ? C33 N32 1.376(7) . ? C33 C34 1.462(8) . ? C34 C35 1.377(8) . ? C34 C39 1.401(8) . ? C35 C36 1.390(8) . ? C35 H35 0.95 . ? C36 C37 1.414(9) . ? C36 H36 0.95 . ? C37 C38 1.380(8) . ? C37 H37 0.95 . ? C38 C39 1.402(8) . ? C38 H38 0.95 . ? C41 O41 1.221(7) . ? C41 N42 1.396(7) . ? C41 N50 1.402(7) . ? C41 Ti1 2.561(6) . ? C43 C48 1.387(8) . ? C43 C44 1.398(7) . ? C43 N42 1.452(7) . ? C44 C45 1.385(7) . ? C44 H44 0.95 . ? C45 C46 1.399(8) . ? C45 H45 0.95 . ? C46 C47 1.385(8) . ? C46 C49 1.531(7) . ? C47 C48 1.408(8) . ? C47 H47 0.95 . ? C48 H48 0.95 . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? C51 C56 1.383(8) . ? C51 C52 1.392(8) . ? C51 N50 1.441(7) . ? C52 C53 1.401(8) . ? C52 H52 0.95 . ? C53 C54 1.385(8) . ? C53 H53 0.95 . ? C54 C55 1.392(9) . ? C54 C57 1.524(8) . ? C55 C56 1.393(8) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C57 H57A 0.98 . ? C57 H57B 0.98 . ? C57 H57C 0.98 . ? C101 C102 1.381(11) . ? C101 C106 1.400(11) . ? C101 Cl1 1.746(8) . ? C102 C103 1.374(11) . ? C102 H102 0.95 . ? C103 C104 1.331(11) . ? C103 H103 0.95 . ? C106 C105 1.387(11) . ? C106 H106 0.95 . ? C105 C104 1.355(11) . ? C105 H105 0.95 . ? C104 H104 0.95 . ? N1 Ti1 2.060(5) . ? N12 Ti1 2.111(5) . ? N22 Ti1 2.066(5) . ? N32 Ti1 2.104(5) . ? N42 Ti1 1.982(4) . ? N50 Ti1 1.990(5) . ? Cl2 C201 1.718(9) . ? C201 C202 1.39 . ? C201 C206 1.39 . ? C202 C203 1.39 . ? C202 H202 0.95 . ? C203 C204 1.39 . ? C203 H203 0.95 . ? C204 C205 1.39 . ? C204 H204 0.95 . ? C205 C206 1.39 . ? C205 H205 0.95 . ? C206 H206 0.95 . ? 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 N40 C2 N1 128.6(5) . . ? N40 C2 C3 122.5(5) . . ? N1 C2 C3 108.9(5) . . ? C8 C3 C4 121.0(5) . . ? C8 C3 C2 107.0(5) . . ? C4 C3 C2 132.0(5) . . ? C5 C4 C3 117.3(5) . . ? C5 C4 H4 121.4 . . ? C3 C4 H4 121.4 . . ? C4 C5 C6 122.0(6) . . ? C4 C5 H5 119 . . ? C6 C5 H5 119 . . ? C7 C6 C5 121.1(6) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 117.1(5) . . ? C6 C7 H7 121.4 . . ? C8 C7 H7 121.4 . . ? C7 C8 C3 121.5(5) . . ? C7 C8 C9 131.3(5) . . ? C3 C8 C9 107.2(5) . . ? N10 C9 N1 127.5(5) . . ? N10 C9 C8 123.6(5) . . ? N1 C9 C8 108.8(5) . . ? N10 C11 N12 126.8(5) . . ? N10 C11 C19 122.9(5) . . ? N12 C11 C19 110.3(5) . . ? N20 C13 N12 126.5(5) . . ? N20 C13 C14 122.9(5) . . ? N12 C13 C14 110.5(5) . . ? C15 C14 C19 121.9(6) . . ? C15 C14 C13 132.0(6) . . ? C19 C14 C13 106.0(5) . . ? C14 C15 C16 117.4(6) . . ? C14 C15 H15 121.3 . . ? C16 C15 H15 121.3 . . ? C15 C16 C17 121.4(6) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C18 C17 C16 121.1(6) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 117.8(6) . . ? C17 C18 H18 121.1 . . ? C19 C18 H18 121.1 . . ? C18 C19 C14 120.4(5) . . ? C18 C19 C11 133.0(6) . . ? C14 C19 C11 106.5(5) . . ? N20 C21 N22 127.4(5) . . ? N20 C21 C29 123.2(5) . . ? N22 C21 C29 109.3(5) . . ? N30 C23 N22 127.8(5) . . ? N30 C23 C24 122.4(5) . . ? N22 C23 C24 109.8(5) . . ? C25 C24 C29 122.7(6) . . ? C25 C24 C23 131.9(6) . . ? C29 C24 C23 105.4(5) . . ? C24 C25 C26 116.5(6) . . ? C24 C25 H25 121.7 . . ? C26 C25 H25 121.7 . . ? C27 C26 C25 121.9(7) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C28 C27 C26 120.9(6) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 118.1(6) . . ? C27 C28 H28 120.9 . . ? C29 C28 H28 120.9 . . ? C28 C29 C24 119.8(6) . . ? C28 C29 C21 132.1(6) . . ? C24 C29 C21 108.0(5) . . ? N30 C31 N32 127.1(5) . . ? N30 C31 C39 123.7(5) . . ? N32 C31 C39 109.1(5) . . ? N40 C33 N32 127.7(5) . . ? N40 C33 C34 121.3(5) . . ? N32 C33 C34 110.9(5) . . ? C35 C34 C39 121.4(6) . . ? C35 C34 C33 132.9(6) . . ? C39 C34 C33 105.6(5) . . ? C34 C35 C36 117.7(6) . . ? C34 C35 H35 121.1 . . ? C36 C35 H35 121.1 . . ? C35 C36 C37 121.1(6) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C38 C37 C36 121.2(6) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 117.2(6) . . ? C37 C38 H38 121.4 . . ? C39 C38 H38 121.4 . . ? C34 C39 C38 121.3(6) . . ? C34 C39 C31 107.3(5) . . ? C38 C39 C31 131.4(6) . . ? O41 C41 N42 130.6(5) . . ? O41 C41 N50 128.9(5) . . ? N42 C41 N50 100.5(5) . . ? O41 C41 Ti1 177.1(4) . . ? N42 C41 Ti1 50.2(3) . . ? N50 C41 Ti1 50.5(3) . . ? C48 C43 C44 119.7(5) . . ? C48 C43 N42 121.2(5) . . ? C44 C43 N42 119.0(5) . . ? C45 C44 C43 120.0(5) . . ? C45 C44 H44 120 . . ? C43 C44 H44 120 . . ? C44 C45 C46 121.5(5) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C47 C46 C45 117.8(5) . . ? C47 C46 C49 120.9(5) . . ? C45 C46 C49 121.3(5) . . ? C46 C47 C48 121.7(5) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C43 C48 C47 119.3(5) . . ? C43 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C56 C51 C52 120.3(5) . . ? C56 C51 N50 119.7(5) . . ? C52 C51 N50 120.0(5) . . ? C51 C52 C53 118.7(6) . . ? C51 C52 H52 120.7 . . ? C53 C52 H52 120.7 . . ? C54 C53 C52 122.0(6) . . ? C54 C53 H53 119 . . ? C52 C53 H53 119 . . ? C53 C54 C55 117.9(6) . . ? C53 C54 C57 119.9(6) . . ? C55 C54 C57 122.1(6) . . ? C54 C55 C56 121.2(6) . . ? C54 C55 H55 119.4 . . ? C56 C55 H55 119.4 . . ? C51 C56 C55 119.9(6) . . ? C51 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C102 C101 C106 121.0(8) . . ? C102 C101 Cl1 121.5(7) . . ? C106 C101 Cl1 117.4(7) . . ? C103 C102 C101 118.0(8) . . ? C103 C102 H102 121 . . ? C101 C102 H102 121 . . ? C104 C103 C102 120.9(9) . . ? C104 C103 H103 119.5 . . ? C102 C103 H103 119.5 . . ? C105 C106 C101 118.4(8) . . ? C105 C106 H106 120.8 . . ? C101 C106 H106 120.8 . . ? C104 C105 C106 119.0(8) . . ? C104 C105 H105 120.5 . . ? C106 C105 H105 120.5 . . ? C103 C104 C105 122.7(9) . . ? C103 C104 H104 118.6 . . ? C105 C104 H104 118.6 . . ? C9 N1 C2 107.9(4) . . ? C9 N1 Ti1 124.8(4) . . ? C2 N1 Ti1 124.4(4) . . ? C9 N10 C11 122.9(5) . . ? C11 N12 C13 106.6(4) . . ? C11 N12 Ti1 124.1(4) . . ? C13 N12 Ti1 123.7(4) . . ? C21 N20 C13 123.0(5) . . ? C21 N22 C23 107.4(5) . . ? C21 N22 Ti1 125.1(4) . . ? C23 N22 Ti1 124.8(4) . . ? C31 N30 C23 122.4(5) . . ? C33 N32 C31 107.1(4) . . ? C33 N32 Ti1 124.4(4) . . ? C31 N32 Ti1 123.6(4) . . ? C2 N40 C33 121.5(5) . . ? C41 N42 C43 116.5(4) . . ? C41 N42 Ti1 97.1(3) . . ? C43 N42 Ti1 144.2(4) . . ? C41 N50 C51 118.9(5) . . ? C41 N50 Ti1 96.5(3) . . ? C51 N50 Ti1 143.5(4) . . ? N42 Ti1 N50 65.59(18) . . ? N42 Ti1 N1 109.90(19) . . ? N50 Ti1 N1 107.35(19) . . ? N42 Ti1 N22 103.12(18) . . ? N50 Ti1 N22 106.04(19) . . ? N1 Ti1 N22 140.26(19) . . ? N42 Ti1 N32 145.39(19) . . ? N50 Ti1 N32 79.99(18) . . ? N1 Ti1 N32 82.89(18) . . ? N22 Ti1 N32 82.27(18) . . ? N42 Ti1 N12 80.50(19) . . ? N50 Ti1 N12 146.06(18) . . ? N1 Ti1 N12 81.97(18) . . ? N22 Ti1 N12 82.30(18) . . ? N32 Ti1 N12 133.94(19) . . ? N42 Ti1 C41 32.75(18) . . ? N50 Ti1 C41 32.95(17) . . ? N1 Ti1 C41 114.35(19) . . ? N22 Ti1 C41 105.39(18) . . ? N32 Ti1 C41 112.67(18) . . ? N12 Ti1 C41 113.23(18) . . ? C202 C201 C206 120 . . ? C202 C201 Cl2 119.8(8) . . ? C206 C201 Cl2 120.2(8) . . ? C203 C202 C201 120 . . ? C203 C202 H202 120 . . ? C201 C202 H202 120 . . ? C204 C203 C202 120 . . ? C204 C203 H203 120 . . ? C202 C203 H203 120 . . ? C203 C204 C205 120 . . ? C203 C204 H204 120 . . ? C205 C204 H204 120 . . ? C204 C205 C206 120 . . ? C204 C205 H205 120 . . ? C206 C205 H205 120 . . ? C205 C206 C201 120 . . ? C205 C206 H206 120 . . ? C201 C206 H206 120 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N40 C2 C3 C8 -176.8(6) . . . . ? N1 C2 C3 C8 3.2(7) . . . . ? N40 C2 C3 C4 2.3(10) . . . . ? N1 C2 C3 C4 -177.7(6) . . . . ? C8 C3 C4 C5 0.5(9) . . . . ? C2 C3 C4 C5 -178.5(6) . . . . ? C3 C4 C5 C6 0.2(10) . . . . ? C4 C5 C6 C7 -0.9(10) . . . . ? C5 C6 C7 C8 0.9(10) . . . . ? C6 C7 C8 C3 -0.2(9) . . . . ? C6 C7 C8 C9 179.2(6) . . . . ? C4 C3 C8 C7 -0.5(9) . . . . ? C2 C3 C8 C7 178.7(6) . . . . ? C4 C3 C8 C9 -180.0(5) . . . . ? C2 C3 C8 C9 -0.8(6) . . . . ? C7 C8 C9 N10 -4.4(10) . . . . ? C3 C8 C9 N10 175.0(6) . . . . ? C7 C8 C9 N1 178.7(6) . . . . ? C3 C8 C9 N1 -2.0(7) . . . . ? N20 C13 C14 C15 -3.0(10) . . . . ? N12 C13 C14 C15 174.3(6) . . . . ? N20 C13 C14 C19 -179.1(6) . . . . ? N12 C13 C14 C19 -1.8(7) . . . . ? C19 C14 C15 C16 -0.8(9) . . . . ? C13 C14 C15 C16 -176.3(6) . . . . ? C14 C15 C16 C17 -0.3(9) . . . . ? C15 C16 C17 C18 0.4(10) . . . . ? C16 C17 C18 C19 0.6(9) . . . . ? C17 C18 C19 C14 -1.6(9) . . . . ? C17 C18 C19 C11 174.7(6) . . . . ? C15 C14 C19 C18 1.8(9) . . . . ? C13 C14 C19 C18 178.3(6) . . . . ? C15 C14 C19 C11 -175.4(6) . . . . ? C13 C14 C19 C11 1.1(6) . . . . ? N10 C11 C19 C18 0.3(10) . . . . ? N12 C11 C19 C18 -176.9(6) . . . . ? N10 C11 C19 C14 177.0(6) . . . . ? N12 C11 C19 C14 -0.2(7) . . . . ? N30 C23 C24 C25 -0.9(10) . . . . ? N22 C23 C24 C25 179.6(7) . . . . ? N30 C23 C24 C29 179.6(6) . . . . ? N22 C23 C24 C29 0.2(7) . . . . ? C29 C24 C25 C26 0.5(10) . . . . ? C23 C24 C25 C26 -178.9(7) . . . . ? C24 C25 C26 C27 -1.6(10) . . . . ? C25 C26 C27 C28 0.3(11) . . . . ? C26 C27 C28 C29 2.0(10) . . . . ? C27 C28 C29 C24 -3.0(9) . . . . ? C27 C28 C29 C21 -178.8(6) . . . . ? C25 C24 C29 C28 1.8(10) . . . . ? C23 C24 C29 C28 -178.7(6) . . . . ? C25 C24 C29 C21 178.5(6) . . . . ? C23 C24 C29 C21 -2.0(7) . . . . ? N20 C21 C29 C28 0.2(11) . . . . ? N22 C21 C29 C28 179.4(6) . . . . ? N20 C21 C29 C24 -176.0(6) . . . . ? N22 C21 C29 C24 3.2(7) . . . . ? N40 C33 C34 C35 1.1(10) . . . . ? N32 C33 C34 C35 177.4(6) . . . . ? N40 C33 C34 C39 -176.4(5) . . . . ? N32 C33 C34 C39 -0.1(7) . . . . ? C39 C34 C35 C36 1.5(9) . . . . ? C33 C34 C35 C36 -175.7(6) . . . . ? C34 C35 C36 C37 -1.2(10) . . . . ? C35 C36 C37 C38 -0.7(10) . . . . ? C36 C37 C38 C39 2.2(10) . . . . ? C35 C34 C39 C38 0.0(9) . . . . ? C33 C34 C39 C38 177.9(6) . . . . ? C35 C34 C39 C31 -178.7(6) . . . . ? C33 C34 C39 C31 -0.9(6) . . . . ? C37 C38 C39 C34 -1.9(9) . . . . ? C37 C38 C39 C31 176.6(6) . . . . ? N30 C31 C39 C34 -178.8(6) . . . . ? N32 C31 C39 C34 1.6(7) . . . . ? N30 C31 C39 C38 2.6(11) . . . . ? N32 C31 C39 C38 -177.0(6) . . . . ? C48 C43 C44 C45 1.1(9) . . . . ? N42 C43 C44 C45 -179.5(5) . . . . ? C43 C44 C45 C46 -1.4(9) . . . . ? C44 C45 C46 C47 0.2(9) . . . . ? C44 C45 C46 C49 -179.4(6) . . . . ? C45 C46 C47 C48 1.2(9) . . . . ? C49 C46 C47 C48 -179.2(6) . . . . ? C44 C43 C48 C47 0.3(9) . . . . ? N42 C43 C48 C47 -179.1(5) . . . . ? C46 C47 C48 C43 -1.5(9) . . . . ? C56 C51 C52 C53 -2.9(9) . . . . ? N50 C51 C52 C53 177.4(5) . . . . ? C51 C52 C53 C54 2.2(9) . . . . ? C52 C53 C54 C55 0.1(10) . . . . ? C52 C53 C54 C57 -178.6(6) . . . . ? C53 C54 C55 C56 -1.7(10) . . . . ? C57 C54 C55 C56 177.0(6) . . . . ? C52 C51 C56 C55 1.3(9) . . . . ? N50 C51 C56 C55 -178.9(5) . . . . ? C54 C55 C56 C51 1.0(10) . . . . ? C106 C101 C102 C103 -1.1(12) . . . . ? Cl1 C101 C102 C103 -177.3(6) . . . . ? C101 C102 C103 C104 0.1(12) . . . . ? C102 C101 C106 C105 1.0(11) . . . . ? Cl1 C101 C106 C105 177.4(6) . . . . ? C101 C106 C105 C104 0.0(11) . . . . ? C102 C103 C104 C105 0.9(14) . . . . ? C106 C105 C104 C103 -1.0(13) . . . . ? N10 C9 N1 C2 -172.8(6) . . . . ? C8 C9 N1 C2 4.0(6) . . . . ? N10 C9 N1 Ti1 25.5(9) . . . . ? C8 C9 N1 Ti1 -157.7(4) . . . . ? N40 C2 N1 C9 175.6(6) . . . . ? C3 C2 N1 C9 -4.4(6) . . . . ? N40 C2 N1 Ti1 -22.6(9) . . . . ? C3 C2 N1 Ti1 157.4(4) . . . . ? N1 C9 N10 C11 0.2(9) . . . . ? C8 C9 N10 C11 -176.1(6) . . . . ? N12 C11 N10 C9 -0.8(9) . . . . ? C19 C11 N10 C9 -177.4(6) . . . . ? N10 C11 N12 C13 -177.9(6) . . . . ? C19 C11 N12 C13 -0.9(6) . . . . ? N10 C11 N12 Ti1 -23.5(8) . . . . ? C19 C11 N12 Ti1 153.5(4) . . . . ? N20 C13 N12 C11 178.8(6) . . . . ? C14 C13 N12 C11 1.6(6) . . . . ? N20 C13 N12 Ti1 24.3(8) . . . . ? C14 C13 N12 Ti1 -152.9(4) . . . . ? N22 C21 N20 C13 -3.9(10) . . . . ? C29 C21 N20 C13 175.1(6) . . . . ? N12 C13 N20 C21 2.2(9) . . . . ? C14 C13 N20 C21 179.0(6) . . . . ? N20 C21 N22 C23 176.1(6) . . . . ? C29 C21 N22 C23 -3.0(6) . . . . ? N20 C21 N22 Ti1 -22.0(8) . . . . ? C29 C21 N22 Ti1 158.9(4) . . . . ? N30 C23 N22 C21 -177.6(6) . . . . ? C24 C23 N22 C21 1.8(6) . . . . ? N30 C23 N22 Ti1 20.4(9) . . . . ? C24 C23 N22 Ti1 -160.2(4) . . . . ? N32 C31 N30 C23 -2.1(10) . . . . ? C39 C31 N30 C23 178.3(6) . . . . ? N22 C23 N30 C31 5.1(10) . . . . ? C24 C23 N30 C31 -174.3(6) . . . . ? N40 C33 N32 C31 177.1(6) . . . . ? C34 C33 N32 C31 1.1(6) . . . . ? N40 C33 N32 Ti1 21.2(8) . . . . ? C34 C33 N32 Ti1 -154.7(4) . . . . ? N30 C31 N32 C33 178.7(6) . . . . ? C39 C31 N32 C33 -1.6(6) . . . . ? N30 C31 N32 Ti1 -25.2(8) . . . . ? C39 C31 N32 Ti1 154.4(4) . . . . ? N1 C2 N40 C33 -2.1(10) . . . . ? C3 C2 N40 C33 178.0(6) . . . . ? N32 C33 N40 C2 2.5(9) . . . . ? C34 C33 N40 C2 178.1(6) . . . . ? O41 C41 N42 C43 9.1(9) . . . . ? N50 C41 N42 C43 -172.2(4) . . . . ? Ti1 C41 N42 C43 -167.2(5) . . . . ? O41 C41 N42 Ti1 176.3(6) . . . . ? N50 C41 N42 Ti1 -4.9(4) . . . . ? C48 C43 N42 C41 -116.2(6) . . . . ? C44 C43 N42 C41 64.4(7) . . . . ? C48 C43 N42 Ti1 85.8(8) . . . . ? C44 C43 N42 Ti1 -93.6(7) . . . . ? O41 C41 N50 C51 -5.4(9) . . . . ? N42 C41 N50 C51 175.8(4) . . . . ? Ti1 C41 N50 C51 170.9(5) . . . . ? O41 C41 N50 Ti1 -176.3(6) . . . . ? N42 C41 N50 Ti1 4.9(4) . . . . ? C56 C51 N50 C41 -63.5(7) . . . . ? C52 C51 N50 C41 116.2(6) . . . . ? C56 C51 N50 Ti1 101.2(7) . . . . ? C52 C51 N50 Ti1 -79.0(8) . . . . ? C41 N42 Ti1 N50 3.7(3) . . . . ? C43 N42 Ti1 N50 164.0(7) . . . . ? C41 N42 Ti1 N1 104.3(3) . . . . ? C43 N42 Ti1 N1 -95.4(6) . . . . ? C41 N42 Ti1 N22 -98.1(3) . . . . ? C43 N42 Ti1 N22 62.1(6) . . . . ? C41 N42 Ti1 N32 -2.7(5) . . . . ? C43 N42 Ti1 N32 157.6(5) . . . . ? C41 N42 Ti1 N12 -177.8(3) . . . . ? C43 N42 Ti1 N12 -17.6(6) . . . . ? C43 N42 Ti1 C41 160.2(8) . . . . ? C41 N50 Ti1 N42 -3.7(3) . . . . ? C51 N50 Ti1 N42 -170.3(7) . . . . ? C41 N50 Ti1 N1 -108.2(3) . . . . ? C51 N50 Ti1 N1 85.2(6) . . . . ? C41 N50 Ti1 N22 93.7(3) . . . . ? C51 N50 Ti1 N22 -72.9(6) . . . . ? C41 N50 Ti1 N32 172.6(3) . . . . ? C51 N50 Ti1 N32 6.0(6) . . . . ? C41 N50 Ti1 N12 -6.5(5) . . . . ? C51 N50 Ti1 N12 -173.1(5) . . . . ? C51 N50 Ti1 C41 -166.6(8) . . . . ? C9 N1 Ti1 N42 43.2(5) . . . . ? C2 N1 Ti1 N42 -115.6(5) . . . . ? C9 N1 Ti1 N50 112.9(5) . . . . ? C2 N1 Ti1 N50 -45.9(5) . . . . ? C9 N1 Ti1 N22 -101.2(5) . . . . ? C2 N1 Ti1 N22 100.0(5) . . . . ? C9 N1 Ti1 N32 -170.0(5) . . . . ? C2 N1 Ti1 N32 31.2(5) . . . . ? C9 N1 Ti1 N12 -33.6(5) . . . . ? C2 N1 Ti1 N12 167.6(5) . . . . ? C9 N1 Ti1 C41 78.3(5) . . . . ? C2 N1 Ti1 C41 -80.5(5) . . . . ? C21 N22 Ti1 N42 -45.6(5) . . . . ? C23 N22 Ti1 N42 113.2(5) . . . . ? C21 N22 Ti1 N50 -113.6(5) . . . . ? C23 N22 Ti1 N50 45.2(5) . . . . ? C21 N22 Ti1 N1 100.2(5) . . . . ? C23 N22 Ti1 N1 -101.0(5) . . . . ? C21 N22 Ti1 N32 169.2(5) . . . . ? C23 N22 Ti1 N32 -32.0(4) . . . . ? C21 N22 Ti1 N12 32.7(5) . . . . ? C23 N22 Ti1 N12 -168.5(5) . . . . ? C21 N22 Ti1 C41 -79.4(5) . . . . ? C23 N22 Ti1 C41 79.5(5) . . . . ? C33 N32 Ti1 N42 84.1(5) . . . . ? C31 N32 Ti1 N42 -67.8(6) . . . . ? C33 N32 Ti1 N50 78.2(5) . . . . ? C31 N32 Ti1 N50 -73.8(5) . . . . ? C33 N32 Ti1 N1 -30.9(4) . . . . ? C31 N32 Ti1 N1 177.1(5) . . . . ? C33 N32 Ti1 N22 -174.0(5) . . . . ? C31 N32 Ti1 N22 34.1(5) . . . . ? C33 N32 Ti1 N12 -102.5(5) . . . . ? C31 N32 Ti1 N12 105.5(5) . . . . ? C33 N32 Ti1 C41 82.5(5) . . . . ? C31 N32 Ti1 C41 -69.4(5) . . . . ? C11 N12 Ti1 N42 -79.0(4) . . . . ? C13 N12 Ti1 N42 71.1(4) . . . . ? C11 N12 Ti1 N50 -76.4(5) . . . . ? C13 N12 Ti1 N50 73.7(6) . . . . ? C11 N12 Ti1 N1 32.8(4) . . . . ? C13 N12 Ti1 N1 -177.0(5) . . . . ? C11 N12 Ti1 N22 176.2(5) . . . . ? C13 N12 Ti1 N22 -33.6(4) . . . . ? C11 N12 Ti1 N32 104.8(5) . . . . ? C13 N12 Ti1 N32 -105.1(5) . . . . ? C11 N12 Ti1 C41 -80.3(4) . . . . ? C13 N12 Ti1 C41 69.8(5) . . . . ? O41 C41 Ti1 N42 -107(9) . . . . ? N50 C41 Ti1 N42 173.7(5) . . . . ? O41 C41 Ti1 N50 79(9) . . . . ? N42 C41 Ti1 N50 -173.7(5) . . . . ? O41 C41 Ti1 N1 164(9) . . . . ? N42 C41 Ti1 N1 -89.3(3) . . . . ? N50 C41 Ti1 N1 84.5(3) . . . . ? O41 C41 Ti1 N22 -17(9) . . . . ? N42 C41 Ti1 N22 90.4(3) . . . . ? N50 C41 Ti1 N22 -95.9(3) . . . . ? O41 C41 Ti1 N32 71(9) . . . . ? N42 C41 Ti1 N32 178.3(3) . . . . ? N50 C41 Ti1 N32 -7.9(4) . . . . ? O41 C41 Ti1 N12 -105(9) . . . . ? N42 C41 Ti1 N12 2.3(4) . . . . ? N50 C41 Ti1 N12 176.0(3) . . . . ? C206 C201 C202 C203 0 . . . . ? Cl2 C201 C202 C203 177.2(12) . . . . ? C201 C202 C203 C204 0 . . . . ? C202 C203 C204 C205 0 . . . . ? C203 C204 C205 C206 0 . . . . ? C204 C205 C206 C201 0 . . . . ? C202 C201 C206 C205 0 . . . . ? Cl2 C201 C206 C205 -177.2(12) . . . . ? #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 269283' #TrackingRef '- 2a_dalton_transactions_z17.cif' _audit_creation_date 2005-04-18T16:02:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C44 H33 N8 Ti1' _chemical_formula_sum 'C44 H33 N9 Ti' _chemical_formula_weight 735.69 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9544(9) _cell_length_b 17.0865(9) _cell_length_c 19.5582(15) _cell_angle_alpha 90 _cell_angle_beta 104.568(6) _cell_angle_gamma 90 _cell_volume 3543.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 11975 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 26 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -2 8 11 0.062 0 -11 7 0.031 1 -3 -6 0.049 0 10 4 0.021 0 -13 -5 0.035 9 -4 -2 0.161 0 1 7 0.042 2 7 -8 0.058 -2 -7 7 0.067 -10 2 11 0.147 0 0 -1 0.033 0 7 -4 0.012 4 11 -9 0.08 -3 -6 -11 0.083 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.289 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; a grid of 8 x 8 x 8 = 512 sampling points was used ; _exptl_absorpt_correction_T_min 0.9484 _exptl_absorpt_correction_T_max 0.9885 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0926 _diffrn_reflns_av_unetI/netI 0.0885 _diffrn_reflns_number 29449 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 6229 _reflns_number_gt 3550 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0342P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_number_reflns 6229 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.866 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.21 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.043 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2 C 0.3357(3) 0.19479(16) 0.44585(14) 0.0328(7) Uani 1 1 d . . . C3 C 0.2798(3) 0.26090(16) 0.47342(14) 0.0345(7) Uani 1 1 d . . . C4 C 0.1704(3) 0.30393(17) 0.44628(16) 0.0411(8) Uani 1 1 d . . . H4 H 0.1143 0.2911 0.4022 0.049 Uiso 1 1 calc R . . C5 C 0.1470(3) 0.36597(19) 0.48617(17) 0.0506(9) Uani 1 1 d . . . H5 H 0.0743 0.3974 0.4685 0.061 Uiso 1 1 calc R . . C6 C 0.2278(3) 0.3839(2) 0.55212(16) 0.0499(8) Uani 1 1 d . . . H6 H 0.2082 0.4266 0.5786 0.06 Uiso 1 1 calc R . . C7 C 0.3344(3) 0.34078(18) 0.57894(16) 0.0417(8) Uani 1 1 d . . . H7 H 0.3888 0.3527 0.6238 0.05 Uiso 1 1 calc R . . C8 C 0.3604(3) 0.27943(16) 0.53892(14) 0.0328(7) Uani 1 1 d . . . C9 C 0.4653(3) 0.22437(17) 0.55065(14) 0.0337(7) Uani 1 1 d . . . C11 C 0.6588(3) 0.17654(17) 0.61780(13) 0.0328(7) Uani 1 1 d . . . C13 C 0.7901(3) 0.08151(17) 0.60228(13) 0.0319(7) Uani 1 1 d . . . C14 C 0.8477(3) 0.11881(17) 0.66951(12) 0.0319(6) Uani 1 1 d . . . C15 C 0.9635(3) 0.10585(17) 0.71725(13) 0.0371(7) Uani 1 1 d . . . H15 H 1.019 0.0658 0.7099 0.045 Uiso 1 1 calc R . . C16 C 0.9940(3) 0.15395(18) 0.77591(14) 0.0428(8) Uani 1 1 d . . . H16 H 1.073 0.1474 0.8093 0.051 Uiso 1 1 calc R . . C17 C 0.9119(3) 0.21162(19) 0.78711(14) 0.0439(8) Uani 1 1 d . . . H17 H 0.9355 0.2431 0.8284 0.053 Uiso 1 1 calc R . . C18 C 0.7960(3) 0.22452(17) 0.73962(14) 0.0411(8) Uani 1 1 d . . . H18 H 0.7398 0.2637 0.7478 0.049 Uiso 1 1 calc R . . C19 C 0.7656(3) 0.17762(16) 0.67954(13) 0.0325(7) Uani 1 1 d . . . C21 C 0.7928(3) -0.01112(16) 0.51413(13) 0.0314(7) Uani 1 1 d . . . C23 C 0.6650(3) -0.04106(16) 0.40947(13) 0.0320(7) Uani 1 1 d . . . C24 C 0.7709(3) -0.09427(16) 0.42073(13) 0.0318(7) Uani 1 1 d . . . C25 C 0.8014(3) -0.15391(17) 0.37960(14) 0.0371(7) Uani 1 1 d . . . H25 H 0.747 -0.167 0.3351 0.045 Uiso 1 1 calc R . . C26 C 0.9132(3) -0.19345(18) 0.40545(14) 0.0404(8) Uani 1 1 d . . . H26 H 0.9366 -0.234 0.3781 0.049 Uiso 1 1 calc R . . C27 C 0.9926(3) -0.17491(18) 0.47111(14) 0.0395(7) Uani 1 1 d . . . H27 H 1.0688 -0.2033 0.4877 0.047 Uiso 1 1 calc R . . C28 C 0.9626(3) -0.11602(18) 0.51245(13) 0.0367(7) Uani 1 1 d . . . H28 H 1.0166 -0.1037 0.5573 0.044 Uiso 1 1 calc R . . C29 C 0.8516(3) -0.07583(16) 0.48638(13) 0.0323(7) Uani 1 1 d . . . C31 C 0.4706(3) 0.00659(17) 0.34297(13) 0.0321(7) Uani 1 1 d . . . C33 C 0.3366(3) 0.10106(17) 0.35766(13) 0.0327(7) Uani 1 1 d . . . C34 C 0.2799(3) 0.06333(17) 0.29015(13) 0.0322(7) Uani 1 1 d . . . C35 C 0.1673(3) 0.07610(18) 0.23957(14) 0.0381(7) Uani 1 1 d . . . H35 H 0.1097 0.1155 0.2457 0.046 Uiso 1 1 calc R . . C36 C 0.1426(3) 0.02941(19) 0.18029(15) 0.0456(8) Uani 1 1 d . . . H36 H 0.0669 0.0376 0.1446 0.055 Uiso 1 1 calc R . . C37 C 0.2249(3) -0.02935(19) 0.17115(14) 0.0435(8) Uani 1 1 d . . . H37 H 0.2042 -0.0607 0.1297 0.052 Uiso 1 1 calc R . . C38 C 0.3363(3) -0.04269(18) 0.22141(14) 0.0395(8) Uani 1 1 d . . . H38 H 0.3929 -0.0827 0.2154 0.047 Uiso 1 1 calc R . . C39 C 0.3628(3) 0.00476(17) 0.28127(13) 0.0339(7) Uani 1 1 d . . . C42 C 0.7345(3) 0.23622(18) 0.39597(13) 0.0364(7) Uani 1 1 d . . . C43 C 0.7590(3) 0.3129(2) 0.42427(15) 0.0449(8) Uani 1 1 d . . . C44 C 0.8183(3) 0.3654(2) 0.38864(18) 0.0584(10) Uani 1 1 d . . . H44 H 0.8342 0.4173 0.406 0.07 Uiso 1 1 calc R . . C45 C 0.8546(3) 0.3437(3) 0.32835(19) 0.0663(12) Uani 1 1 d . . . H45 H 0.8931 0.3808 0.3043 0.08 Uiso 1 1 calc R . . C46 C 0.8350(3) 0.2683(3) 0.30352(18) 0.0622(11) Uani 1 1 d . . . H46 H 0.8638 0.2535 0.2635 0.075 Uiso 1 1 calc R . . C47 C 0.7743(3) 0.2135(2) 0.33521(15) 0.0474(9) Uani 1 1 d . . . C48 C 0.7192(4) 0.3364(2) 0.49030(16) 0.0541(10) Uani 1 1 d . . . H48 H 0.6979 0.2873 0.5125 0.065 Uiso 1 1 calc R . . C49 C 0.6029(4) 0.3869(3) 0.4739(2) 0.0816(12) Uani 1 1 d . . . H49A H 0.6209 0.4362 0.4528 0.122 Uiso 1 1 calc R . . H49B H 0.5775 0.3978 0.5175 0.122 Uiso 1 1 calc R . . H49C H 0.5345 0.3595 0.4405 0.122 Uiso 1 1 calc R . . C50 C 0.8267(4) 0.3770(3) 0.5451(2) 0.0835(13) Uani 1 1 d . . . H50A H 0.8414 0.4291 0.528 0.125 Uiso 1 1 calc R . . H50B H 0.9039 0.3457 0.5521 0.125 Uiso 1 1 calc R . . H50C H 0.8031 0.3818 0.59 0.125 Uiso 1 1 calc R . . C51 C 0.7487(4) 0.1320(2) 0.30593(16) 0.0607(11) Uani 1 1 d . . . H51 H 0.7353 0.098 0.345 0.073 Uiso 1 1 calc R . . C52 C 0.6265(4) 0.1305(2) 0.2473(2) 0.0722(12) Uani 1 1 d . . . H52A H 0.5572 0.1507 0.2655 0.108 Uiso 1 1 calc R . . H52B H 0.6078 0.0766 0.2308 0.108 Uiso 1 1 calc R . . H52C H 0.6363 0.1632 0.2079 0.108 Uiso 1 1 calc R . . C53 C 0.8542(4) 0.0953(3) 0.27897(19) 0.0977(18) Uani 1 1 d . . . H53A H 0.8311 0.0415 0.2635 0.147 Uiso 1 1 calc R . . H53B H 0.932 0.0948 0.3169 0.147 Uiso 1 1 calc R . . H53C H 0.8674 0.1259 0.2391 0.147 Uiso 1 1 calc R . . N1 N 0.4482(2) 0.17538(13) 0.49268(11) 0.0332(6) Uani 1 1 d . . . N10 N 0.5616(2) 0.22523(14) 0.60796(11) 0.0356(6) Uani 1 1 d . . . N12 N 0.6782(2) 0.11840(14) 0.57211(10) 0.0309(5) Uani 1 1 d . . . N20 N 0.8431(2) 0.02239(13) 0.57663(11) 0.0320(6) Uani 1 1 d . . . N22 N 0.6817(2) 0.00951(13) 0.46649(10) 0.0312(6) Uani 1 1 d . . . N30 N 0.5682(2) -0.04172(14) 0.35229(11) 0.0343(6) Uani 1 1 d . . . N32 N 0.4519(2) 0.06620(13) 0.38702(10) 0.0314(6) Uani 1 1 d . . . N40 N 0.2835(2) 0.16048(14) 0.38369(11) 0.0337(6) Uani 1 1 d . . . N41 N 0.6698(2) 0.18258(14) 0.42742(11) 0.0327(6) Uani 1 1 d . . . Ti1 Ti 0.59215(5) 0.11540(3) 0.46591(2) 0.03033(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.0298(18) 0.0343(17) 0.0358(15) 0.0028(13) 0.0109(13) -0.0011(14) C3 0.0359(19) 0.0312(16) 0.0378(15) 0.0009(13) 0.0118(14) 0.0006(15) C4 0.0368(19) 0.0402(19) 0.0459(17) -0.0008(14) 0.0098(15) 0.0011(16) C5 0.039(2) 0.045(2) 0.065(2) 0.0016(16) 0.0089(16) 0.0125(17) C6 0.053(2) 0.0415(18) 0.0572(19) -0.0053(17) 0.0175(16) 0.008(2) C7 0.040(2) 0.0418(19) 0.0450(17) -0.0042(15) 0.0134(15) 0.0030(17) C8 0.0325(18) 0.0299(16) 0.0389(15) -0.0006(13) 0.0145(13) 0.0005(14) C9 0.0384(19) 0.0318(16) 0.0331(15) -0.0023(13) 0.0132(13) 0.0000(15) C11 0.0385(19) 0.0308(16) 0.0288(14) -0.0002(12) 0.0079(13) 0.0026(15) C13 0.0370(19) 0.0307(16) 0.0278(13) 0.0027(12) 0.0077(13) -0.0007(15) C14 0.0368(17) 0.0319(15) 0.0262(12) 0.0005(13) 0.0068(11) -0.0018(16) C15 0.0412(19) 0.0352(17) 0.0343(14) -0.0012(13) 0.0082(13) 0.0038(16) C16 0.042(2) 0.0467(19) 0.0352(15) -0.0059(14) 0.0016(14) 0.0012(17) C17 0.047(2) 0.047(2) 0.0325(15) -0.0119(14) 0.0003(15) -0.0014(17) C18 0.050(2) 0.0359(18) 0.0348(15) -0.0074(13) 0.0064(14) 0.0048(16) C19 0.0374(19) 0.0309(16) 0.0283(14) -0.0013(12) 0.0068(12) 0.0018(15) C21 0.0364(19) 0.0305(16) 0.0270(13) 0.0049(12) 0.0072(12) 0.0011(14) C23 0.0378(19) 0.0308(16) 0.0289(14) -0.0016(12) 0.0115(13) -0.0032(15) C24 0.0364(18) 0.0303(17) 0.0296(14) 0.0003(12) 0.0097(12) 0.0009(14) C25 0.042(2) 0.0364(17) 0.0318(15) -0.0057(13) 0.0081(14) 0.0005(16) C26 0.048(2) 0.0374(18) 0.0386(16) -0.0072(13) 0.0162(15) 0.0061(16) C27 0.0382(19) 0.0393(18) 0.0412(16) 0.0030(14) 0.0107(14) 0.0076(16) C28 0.0392(19) 0.0378(16) 0.0319(14) 0.0011(14) 0.0068(12) 0.0053(17) C29 0.0397(19) 0.0291(15) 0.0294(14) 0.0019(12) 0.0110(13) -0.0002(15) C31 0.0324(18) 0.0340(17) 0.0298(14) 0.0005(12) 0.0080(12) -0.0011(15) C33 0.0322(17) 0.0319(17) 0.0337(13) 0.0027(12) 0.0076(12) -0.0035(14) C34 0.0296(17) 0.0355(17) 0.0313(14) -0.0009(12) 0.0072(12) -0.0057(15) C35 0.0342(19) 0.0402(17) 0.0377(15) 0.0004(14) 0.0051(14) -0.0028(15) C36 0.037(2) 0.055(2) 0.0386(16) -0.0018(15) -0.0018(14) -0.0055(18) C37 0.044(2) 0.050(2) 0.0325(15) -0.0071(14) 0.0019(14) -0.0062(18) C38 0.040(2) 0.0430(19) 0.0362(15) -0.0074(13) 0.0102(14) -0.0053(16) C39 0.0327(18) 0.0374(17) 0.0316(14) -0.0013(12) 0.0078(12) -0.0061(15) C42 0.0286(18) 0.0462(19) 0.0309(14) 0.0127(13) 0.0009(13) 0.0052(15) C43 0.039(2) 0.051(2) 0.0383(16) 0.0130(15) -0.0015(14) -0.0065(17) C44 0.041(2) 0.062(3) 0.062(2) 0.0226(18) -0.0075(17) -0.0154(19) C45 0.040(2) 0.098(3) 0.057(2) 0.039(2) 0.0052(18) -0.010(2) C46 0.045(2) 0.092(3) 0.052(2) 0.032(2) 0.0187(17) 0.012(2) C47 0.039(2) 0.063(2) 0.0418(17) 0.0214(16) 0.0133(15) 0.0157(18) C48 0.068(3) 0.043(2) 0.0481(18) -0.0005(15) 0.0073(17) -0.0134(19) C49 0.053(3) 0.124(4) 0.068(2) 0.001(3) 0.017(2) 0.004(3) C50 0.084(3) 0.074(3) 0.077(3) -0.031(2) -0.009(2) 0.016(3) C51 0.084(3) 0.063(3) 0.0427(18) 0.0167(17) 0.0299(19) 0.027(2) C52 0.084(3) 0.053(3) 0.083(3) -0.004(2) 0.028(2) 0.007(2) C53 0.104(4) 0.142(5) 0.051(2) 0.009(2) 0.026(2) 0.072(3) N1 0.0338(15) 0.0334(14) 0.0329(12) -0.0026(10) 0.0094(11) 0.0010(12) N10 0.0410(16) 0.0331(14) 0.0328(12) -0.0037(10) 0.0094(11) -0.0003(13) N12 0.0346(14) 0.0297(12) 0.0279(11) -0.0011(10) 0.0069(10) 0.0013(13) N20 0.0389(16) 0.0287(13) 0.0283(11) 0.0001(10) 0.0082(10) 0.0015(12) N22 0.0364(15) 0.0313(13) 0.0238(11) -0.0019(10) 0.0039(10) 0.0014(12) N30 0.0364(16) 0.0371(14) 0.0283(12) -0.0024(10) 0.0061(11) -0.0008(13) N32 0.0321(15) 0.0336(14) 0.0278(11) -0.0022(10) 0.0063(10) 0.0014(12) N40 0.0335(15) 0.0334(14) 0.0341(12) -0.0028(11) 0.0080(11) -0.0028(12) N41 0.0338(15) 0.0360(14) 0.0271(11) 0.0020(10) 0.0051(10) 0.0036(12) Ti1 0.0338(3) 0.0314(3) 0.0250(2) -0.0005(2) 0.00593(19) 0.0019(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C2 N40 1.341(3) . ? C2 N1 1.379(3) . ? C2 C3 1.452(4) . ? C3 C4 1.392(4) . ? C3 C8 1.397(4) . ? C4 C5 1.378(4) . ? C4 H4 0.95 . ? C5 C6 1.402(4) . ? C5 H5 0.95 . ? C6 C7 1.368(4) . ? C6 H6 0.95 . ? C7 C8 1.380(4) . ? C7 H7 0.95 . ? C8 C9 1.458(4) . ? C9 N10 1.332(4) . ? C9 N1 1.384(3) . ? C11 N10 1.327(4) . ? C11 N12 1.388(3) . ? C11 C19 1.455(4) . ? C13 N20 1.325(4) . ? C13 N12 1.373(4) . ? C13 C14 1.455(4) . ? C14 C15 1.391(4) . ? C14 C19 1.395(4) . ? C15 C16 1.382(4) . ? C15 H15 0.95 . ? C16 C17 1.389(4) . ? C16 H16 0.95 . ? C17 C18 1.389(4) . ? C17 H17 0.95 . ? C18 C19 1.392(4) . ? C18 H18 0.95 . ? C21 N20 1.337(3) . ? C21 N22 1.379(3) . ? C21 C29 1.452(4) . ? C23 N30 1.334(3) . ? C23 N22 1.386(3) . ? C23 C24 1.447(4) . ? C24 C25 1.390(4) . ? C24 C29 1.399(4) . ? C25 C26 1.378(4) . ? C25 H25 0.95 . ? C26 C27 1.394(4) . ? C26 H26 0.95 . ? C27 C28 1.381(4) . ? C27 H27 0.95 . ? C28 C29 1.378(4) . ? C28 H28 0.95 . ? C31 N30 1.326(4) . ? C31 N32 1.382(3) . ? C31 C39 1.461(4) . ? C33 N40 1.333(4) . ? C33 N32 1.384(4) . ? C33 C34 1.460(4) . ? C34 C35 1.391(4) . ? C34 C39 1.391(4) . ? C35 C36 1.377(4) . ? C35 H35 0.95 . ? C36 C37 1.391(4) . ? C36 H36 0.95 . ? C37 C38 1.380(4) . ? C37 H37 0.95 . ? C38 C39 1.393(4) . ? C38 H38 0.95 . ? C42 N41 1.393(4) . ? C42 C47 1.419(4) . ? C42 C43 1.421(4) . ? C43 C44 1.393(4) . ? C43 C48 1.518(4) . ? C44 C45 1.387(5) . ? C44 H44 0.95 . ? C45 C46 1.374(5) . ? C45 H45 0.95 . ? C46 C47 1.382(5) . ? C46 H46 0.95 . ? C47 C51 1.505(5) . ? C48 C49 1.504(5) . ? C48 C50 1.543(5) . ? C48 H48 1 . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? C50 H50A 0.98 . ? C50 H50B 0.98 . ? C50 H50C 0.98 . ? C51 C53 1.521(5) . ? C51 C52 1.528(5) . ? C51 H51 1 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C53 H53A 0.98 . ? C53 H53B 0.98 . ? C53 H53C 0.98 . ? N1 Ti1 2.056(2) . ? N12 Ti1 2.054(2) . ? N22 Ti1 2.057(2) . ? N32 Ti1 2.063(2) . ? N41 Ti1 1.712(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N40 C2 N1 127.1(3) . . ? N40 C2 C3 123.6(3) . . ? N1 C2 C3 109.3(2) . . ? C4 C3 C8 121.0(3) . . ? C4 C3 C2 132.2(3) . . ? C8 C3 C2 106.8(2) . . ? C5 C4 C3 117.1(3) . . ? C5 C4 H4 121.5 . . ? C3 C4 H4 121.5 . . ? C4 C5 C6 121.6(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 121.0(3) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 118.0(3) . . ? C6 C7 H7 121 . . ? C8 C7 H7 121 . . ? C7 C8 C3 121.3(3) . . ? C7 C8 C9 131.9(3) . . ? C3 C8 C9 106.8(2) . . ? N10 C9 N1 127.7(3) . . ? N10 C9 C8 123.5(2) . . ? N1 C9 C8 108.8(2) . . ? N10 C11 N12 127.1(2) . . ? N10 C11 C19 124.1(2) . . ? N12 C11 C19 108.8(2) . . ? N20 C13 N12 128.1(2) . . ? N20 C13 C14 123.0(3) . . ? N12 C13 C14 108.9(2) . . ? C15 C14 C19 122.1(2) . . ? C15 C14 C13 130.7(3) . . ? C19 C14 C13 107.1(2) . . ? C16 C15 C14 116.9(3) . . ? C16 C15 H15 121.6 . . ? C14 C15 H15 121.6 . . ? C15 C16 C17 121.4(3) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C18 121.8(3) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 117.2(3) . . ? C17 C18 H18 121.4 . . ? C19 C18 H18 121.4 . . ? C18 C19 C14 120.5(3) . . ? C18 C19 C11 132.8(3) . . ? C14 C19 C11 106.6(2) . . ? N20 C21 N22 126.8(3) . . ? N20 C21 C29 123.2(3) . . ? N22 C21 C29 109.9(2) . . ? N30 C23 N22 126.6(3) . . ? N30 C23 C24 124.1(2) . . ? N22 C23 C24 109.3(2) . . ? C25 C24 C29 120.5(3) . . ? C25 C24 C23 132.3(3) . . ? C29 C24 C23 107.2(2) . . ? C26 C25 C24 117.9(3) . . ? C26 C25 H25 121.1 . . ? C24 C25 H25 121.1 . . ? C25 C26 C27 121.1(3) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 121.3(3) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C29 C28 C27 117.7(3) . . ? C29 C28 H28 121.2 . . ? C27 C28 H28 121.2 . . ? C28 C29 C24 121.5(3) . . ? C28 C29 C21 132.4(3) . . ? C24 C29 C21 106.1(2) . . ? N30 C31 N32 127.9(2) . . ? N30 C31 C39 123.8(2) . . ? N32 C31 C39 108.3(3) . . ? N40 C33 N32 127.5(2) . . ? N40 C33 C34 123.7(3) . . ? N32 C33 C34 108.7(2) . . ? C35 C34 C39 120.9(3) . . ? C35 C34 C33 132.3(3) . . ? C39 C34 C33 106.8(2) . . ? C36 C35 C34 117.4(3) . . ? C36 C35 H35 121.3 . . ? C34 C35 H35 121.3 . . ? C35 C36 C37 122.0(3) . . ? C35 C36 H36 119 . . ? C37 C36 H36 119 . . ? C38 C37 C36 120.9(3) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 117.5(3) . . ? C37 C38 H38 121.2 . . ? C39 C38 H38 121.2 . . ? C34 C39 C38 121.3(3) . . ? C34 C39 C31 107.4(2) . . ? C38 C39 C31 131.3(3) . . ? N41 C42 C47 119.2(3) . . ? N41 C42 C43 120.1(3) . . ? C47 C42 C43 120.7(3) . . ? C44 C43 C42 117.7(3) . . ? C44 C43 C48 121.6(3) . . ? C42 C43 C48 120.6(3) . . ? C45 C44 C43 121.5(4) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C46 C45 C44 119.9(3) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C47 121.8(4) . . ? C45 C46 H46 119.1 . . ? C47 C46 H46 119.1 . . ? C46 C47 C42 118.3(3) . . ? C46 C47 C51 121.4(3) . . ? C42 C47 C51 120.3(3) . . ? C49 C48 C43 112.3(3) . . ? C49 C48 C50 110.4(3) . . ? C43 C48 C50 112.2(3) . . ? C49 C48 H48 107.2 . . ? C43 C48 H48 107.2 . . ? C50 C48 H48 107.2 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C47 C51 C53 115.3(4) . . ? C47 C51 C52 110.2(3) . . ? C53 C51 C52 109.3(3) . . ? C47 C51 H51 107.2 . . ? C53 C51 H51 107.2 . . ? C52 C51 H51 107.2 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C2 N1 C9 108.2(2) . . ? C2 N1 Ti1 124.45(18) . . ? C9 N1 Ti1 123.78(19) . . ? C11 N10 C9 123.5(2) . . ? C13 N12 C11 108.5(2) . . ? C13 N12 Ti1 123.78(17) . . ? C11 N12 Ti1 124.30(18) . . ? C13 N20 C21 123.6(2) . . ? C21 N22 C23 107.4(2) . . ? C21 N22 Ti1 124.54(17) . . ? C23 N22 Ti1 125.30(18) . . ? C31 N30 C23 123.6(2) . . ? C31 N32 C33 108.8(2) . . ? C31 N32 Ti1 124.53(19) . . ? C33 N32 Ti1 124.44(18) . . ? C33 N40 C2 123.5(2) . . ? C42 N41 Ti1 179.0(2) . . ? N41 Ti1 N12 105.99(10) . . ? N41 Ti1 N1 105.99(10) . . ? N12 Ti1 N1 85.19(9) . . ? N41 Ti1 N22 107.65(11) . . ? N12 Ti1 N22 85.39(9) . . ? N1 Ti1 N22 146.36(10) . . ? N41 Ti1 N32 107.67(10) . . ? N12 Ti1 N32 146.34(10) . . ? N1 Ti1 N32 85.34(9) . . ? N22 Ti1 N32 84.85(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N40 C2 C3 C4 -1.3(5) . . . . ? N1 C2 C3 C4 177.8(3) . . . . ? N40 C2 C3 C8 179.5(3) . . . . ? N1 C2 C3 C8 -1.4(3) . . . . ? C8 C3 C4 C5 1.2(4) . . . . ? C2 C3 C4 C5 -177.9(3) . . . . ? C3 C4 C5 C6 -1.7(5) . . . . ? C4 C5 C6 C7 0.9(5) . . . . ? C5 C6 C7 C8 0.4(5) . . . . ? C6 C7 C8 C3 -0.9(5) . . . . ? C6 C7 C8 C9 178.1(3) . . . . ? C4 C3 C8 C7 0.1(4) . . . . ? C2 C3 C8 C7 179.4(3) . . . . ? C4 C3 C8 C9 -179.1(3) . . . . ? C2 C3 C8 C9 0.2(3) . . . . ? C7 C8 C9 N10 0.2(5) . . . . ? C3 C8 C9 N10 179.3(3) . . . . ? C7 C8 C9 N1 -178.0(3) . . . . ? C3 C8 C9 N1 1.1(3) . . . . ? N20 C13 C14 C15 3.2(5) . . . . ? N12 C13 C14 C15 -175.7(3) . . . . ? N20 C13 C14 C19 -179.5(3) . . . . ? N12 C13 C14 C19 1.5(3) . . . . ? C19 C14 C15 C16 0.3(4) . . . . ? C13 C14 C15 C16 177.2(3) . . . . ? C14 C15 C16 C17 1.1(4) . . . . ? C15 C16 C17 C18 -0.9(5) . . . . ? C16 C17 C18 C19 -0.6(5) . . . . ? C17 C18 C19 C14 2.0(4) . . . . ? C17 C18 C19 C11 -176.3(3) . . . . ? C15 C14 C19 C18 -1.8(4) . . . . ? C13 C14 C19 C18 -179.4(3) . . . . ? C15 C14 C19 C11 176.9(3) . . . . ? C13 C14 C19 C11 -0.7(3) . . . . ? N10 C11 C19 C18 -0.6(5) . . . . ? N12 C11 C19 C18 178.1(3) . . . . ? N10 C11 C19 C14 -179.1(3) . . . . ? N12 C11 C19 C14 -0.3(3) . . . . ? N30 C23 C24 C25 1.4(5) . . . . ? N22 C23 C24 C25 -178.1(3) . . . . ? N30 C23 C24 C29 -179.5(3) . . . . ? N22 C23 C24 C29 0.9(3) . . . . ? C29 C24 C25 C26 -0.4(4) . . . . ? C23 C24 C25 C26 178.6(3) . . . . ? C24 C25 C26 C27 0.7(4) . . . . ? C25 C26 C27 C28 -0.4(5) . . . . ? C26 C27 C28 C29 -0.3(4) . . . . ? C27 C28 C29 C24 0.7(4) . . . . ? C27 C28 C29 C21 -178.7(3) . . . . ? C25 C24 C29 C28 -0.3(4) . . . . ? C23 C24 C29 C28 -179.5(3) . . . . ? C25 C24 C29 C21 179.2(3) . . . . ? C23 C24 C29 C21 0.0(3) . . . . ? N20 C21 C29 C28 -0.7(5) . . . . ? N22 C21 C29 C28 178.6(3) . . . . ? N20 C21 C29 C24 179.9(3) . . . . ? N22 C21 C29 C24 -0.9(3) . . . . ? N40 C33 C34 C35 -0.6(5) . . . . ? N32 C33 C34 C35 -179.1(3) . . . . ? N40 C33 C34 C39 179.7(3) . . . . ? N32 C33 C34 C39 1.2(3) . . . . ? C39 C34 C35 C36 -1.0(4) . . . . ? C33 C34 C35 C36 179.4(3) . . . . ? C34 C35 C36 C37 1.1(5) . . . . ? C35 C36 C37 C38 -0.6(5) . . . . ? C36 C37 C38 C39 0.0(5) . . . . ? C35 C34 C39 C38 0.4(4) . . . . ? C33 C34 C39 C38 -179.9(3) . . . . ? C35 C34 C39 C31 -180.0(3) . . . . ? C33 C34 C39 C31 -0.3(3) . . . . ? C37 C38 C39 C34 0.1(4) . . . . ? C37 C38 C39 C31 -179.4(3) . . . . ? N30 C31 C39 C34 179.8(3) . . . . ? N32 C31 C39 C34 -0.8(3) . . . . ? N30 C31 C39 C38 -0.6(5) . . . . ? N32 C31 C39 C38 178.9(3) . . . . ? N41 C42 C43 C44 -176.8(3) . . . . ? C47 C42 C43 C44 2.7(4) . . . . ? N41 C42 C43 C48 2.1(4) . . . . ? C47 C42 C43 C48 -178.5(3) . . . . ? C42 C43 C44 C45 -1.2(5) . . . . ? C48 C43 C44 C45 179.9(3) . . . . ? C43 C44 C45 C46 -1.5(5) . . . . ? C44 C45 C46 C47 2.9(6) . . . . ? C45 C46 C47 C42 -1.4(5) . . . . ? C45 C46 C47 C51 177.5(3) . . . . ? N41 C42 C47 C46 178.1(3) . . . . ? C43 C42 C47 C46 -1.4(4) . . . . ? N41 C42 C47 C51 -0.9(4) . . . . ? C43 C42 C47 C51 179.6(3) . . . . ? C44 C43 C48 C49 75.4(4) . . . . ? C42 C43 C48 C49 -103.4(4) . . . . ? C44 C43 C48 C50 -49.7(4) . . . . ? C42 C43 C48 C50 131.5(3) . . . . ? C46 C47 C51 C53 39.9(4) . . . . ? C42 C47 C51 C53 -141.2(3) . . . . ? C46 C47 C51 C52 -84.5(4) . . . . ? C42 C47 C51 C52 94.5(3) . . . . ? N40 C2 N1 C9 -178.8(3) . . . . ? C3 C2 N1 C9 2.1(3) . . . . ? N40 C2 N1 Ti1 21.8(4) . . . . ? C3 C2 N1 Ti1 -157.24(19) . . . . ? N10 C9 N1 C2 179.9(3) . . . . ? C8 C9 N1 C2 -2.0(3) . . . . ? N10 C9 N1 Ti1 -20.5(4) . . . . ? C8 C9 N1 Ti1 157.52(18) . . . . ? N12 C11 N10 C9 0.4(5) . . . . ? C19 C11 N10 C9 178.9(3) . . . . ? N1 C9 N10 C11 -0.3(5) . . . . ? C8 C9 N10 C11 -178.1(3) . . . . ? N20 C13 N12 C11 179.4(3) . . . . ? C14 C13 N12 C11 -1.7(3) . . . . ? N20 C13 N12 Ti1 -20.9(4) . . . . ? C14 C13 N12 Ti1 157.97(18) . . . . ? N10 C11 N12 C13 180.0(3) . . . . ? C19 C11 N12 C13 1.3(3) . . . . ? N10 C11 N12 Ti1 20.4(4) . . . . ? C19 C11 N12 Ti1 -158.28(18) . . . . ? N12 C13 N20 C21 0.5(5) . . . . ? C14 C13 N20 C21 -178.3(3) . . . . ? N22 C21 N20 C13 0.8(4) . . . . ? C29 C21 N20 C13 179.9(3) . . . . ? N20 C21 N22 C23 -179.3(3) . . . . ? C29 C21 N22 C23 1.4(3) . . . . ? N20 C21 N22 Ti1 18.6(4) . . . . ? C29 C21 N22 Ti1 -160.59(18) . . . . ? N30 C23 N22 C21 179.0(3) . . . . ? C24 C23 N22 C21 -1.5(3) . . . . ? N30 C23 N22 Ti1 -19.2(4) . . . . ? C24 C23 N22 Ti1 160.41(19) . . . . ? N32 C31 N30 C23 2.3(5) . . . . ? C39 C31 N30 C23 -178.4(3) . . . . ? N22 C23 N30 C31 -1.5(4) . . . . ? C24 C23 N30 C31 179.0(3) . . . . ? N30 C31 N32 C33 -179.0(3) . . . . ? C39 C31 N32 C33 1.6(3) . . . . ? N30 C31 N32 Ti1 17.5(4) . . . . ? C39 C31 N32 Ti1 -161.91(18) . . . . ? N40 C33 N32 C31 179.8(3) . . . . ? C34 C33 N32 C31 -1.7(3) . . . . ? N40 C33 N32 Ti1 -16.7(4) . . . . ? C34 C33 N32 Ti1 161.76(17) . . . . ? N32 C33 N40 C2 -2.0(4) . . . . ? C34 C33 N40 C2 179.7(3) . . . . ? N1 C2 N40 C33 -0.7(4) . . . . ? C3 C2 N40 C33 178.2(3) . . . . ? C47 C42 N41 Ti1 43(12) . . . . ? C43 C42 N41 Ti1 -137(12) . . . . ? C42 N41 Ti1 N12 89(12) . . . . ? C42 N41 Ti1 N1 18E1(10) . . . . ? C42 N41 Ti1 N22 -1(12) . . . . ? C42 N41 Ti1 N32 -91(12) . . . . ? C13 N12 Ti1 N41 -79.5(2) . . . . ? C11 N12 Ti1 N41 77.0(2) . . . . ? C13 N12 Ti1 N1 175.2(2) . . . . ? C11 N12 Ti1 N1 -28.3(2) . . . . ? C13 N12 Ti1 N22 27.5(2) . . . . ? C11 N12 Ti1 N22 -175.9(2) . . . . ? C13 N12 Ti1 N32 101.1(3) . . . . ? C11 N12 Ti1 N32 -102.4(3) . . . . ? C2 N1 Ti1 N41 79.2(2) . . . . ? C9 N1 Ti1 N41 -77.1(2) . . . . ? C2 N1 Ti1 N12 -175.5(2) . . . . ? C9 N1 Ti1 N12 28.2(2) . . . . ? C2 N1 Ti1 N22 -101.3(2) . . . . ? C9 N1 Ti1 N22 102.4(2) . . . . ? C2 N1 Ti1 N32 -27.9(2) . . . . ? C9 N1 Ti1 N32 175.8(2) . . . . ? C21 N22 Ti1 N41 78.6(2) . . . . ? C23 N22 Ti1 N41 -80.3(2) . . . . ? C21 N22 Ti1 N12 -26.7(2) . . . . ? C23 N22 Ti1 N12 174.4(2) . . . . ? C21 N22 Ti1 N1 -100.9(3) . . . . ? C23 N22 Ti1 N1 100.2(2) . . . . ? C21 N22 Ti1 N32 -174.5(2) . . . . ? C23 N22 Ti1 N32 26.7(2) . . . . ? C31 N32 Ti1 N41 81.2(2) . . . . ? C33 N32 Ti1 N41 -79.7(2) . . . . ? C31 N32 Ti1 N12 -99.4(3) . . . . ? C33 N32 Ti1 N12 99.7(3) . . . . ? C31 N32 Ti1 N1 -173.5(2) . . . . ? C33 N32 Ti1 N1 25.6(2) . . . . ? C31 N32 Ti1 N22 -25.7(2) . . . . ? C33 N32 Ti1 N22 173.4(2) . . . . ?