Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_mk61 _database_code_CSD 166843 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Goldberg, I.' 'Goldschmidt, Zeev' 'Kol, Moshe' 'Tshuva, Edit Y.' _publ_contact_author_name 'Dr Moshe Kol' _publ_contact_author_address ; School of Chemistry Tel Aviv University Ramat Aviv Tel Aviv 69978 ISRAEL ; _publ_contact_author_email 'MOSHEKOL@POST.TAU.AC.IL' _publ_section_title ; Exceptional manifestations of living alpha-olefin polymerization by an amine bis(phenolate) titanium catalyst ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C47 H65 N O3 Ti).(C4 H10 O)' _chemical_formula_sum 'C51 H75 N O4 Ti' _chemical_formula_weight 814.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pbca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.2070(2) _cell_length_b 18.3170(2) _cell_length_c 27.2650(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9592.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8757 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 25.36 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'dark red-brown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 0.220 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8757 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.36 _reflns_number_total 8757 _reflns_number_gt 5741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo' _computing_structure_solution 'SIR-92' _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. One t-butyl residue is rotationally disordered between two sites. There is one molecule of diethyl ether solvent in the asymmetric unit. ; _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^)+(0.0466P)^2^+6.0591P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8757 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1107 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.005 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 0.00138(3) 0.43383(2) 0.265661(17) 0.02059(13) Uani 1 1 d . . . O2 O 0.04674(9) 0.41950(8) 0.32538(6) 0.0226(4) Uani 1 1 d . . . O3 O -0.03248(10) 0.42304(8) 0.20198(6) 0.0249(4) Uani 1 1 d . . . O4 O 0.10956(10) 0.48049(8) 0.23138(6) 0.0268(4) Uani 1 1 d . . . N5 N 0.07044(11) 0.33280(10) 0.24207(7) 0.0205(5) Uani 1 1 d . . . C6 C 0.09672(14) 0.38139(13) 0.34959(9) 0.0212(6) Uani 1 1 d . . . C7 C 0.12502(14) 0.40537(13) 0.39431(10) 0.0237(6) Uani 1 1 d . . . C8 C 0.17853(14) 0.36345(13) 0.41462(9) 0.0240(6) Uani 1 1 d . . . H8 H 0.1985 0.3794 0.4446 0.029 Uiso 1 1 calc R . . C9 C 0.20448(14) 0.29950(13) 0.39349(9) 0.0231(6) Uani 1 1 d . . . C10 C 0.17285(15) 0.27684(13) 0.35018(9) 0.0255(6) Uani 1 1 d . . . H10 H 0.1885 0.2330 0.3351 0.031 Uiso 1 1 calc R . . C11 C 0.11961(14) 0.31559(12) 0.32829(9) 0.0220(6) Uani 1 1 d . . . C12 C 0.08142(15) 0.28370(12) 0.28546(9) 0.0240(6) Uani 1 1 d . . . H12A H 0.0352 0.2670 0.2970 0.029 Uiso 1 1 calc R . . H12B H 0.1073 0.2400 0.2742 0.029 Uiso 1 1 calc R . . C13 C 0.03093(15) 0.28669(13) 0.20630(9) 0.0239(6) Uani 1 1 d . . . H13A H -0.0124 0.2700 0.2224 0.029 Uiso 1 1 calc R . . H13B H 0.0591 0.2428 0.1991 0.029 Uiso 1 1 calc R . . C14 C 0.01160(14) 0.32188(12) 0.15843(9) 0.0224(6) Uani 1 1 d . . . C15 C 0.02548(14) 0.28634(13) 0.11466(9) 0.0233(6) Uani 1 1 d . . . H15 H 0.0510 0.2419 0.1153 0.028 Uiso 1 1 calc R . . C16 C 0.00307(15) 0.31385(13) 0.06996(9) 0.0244(6) Uani 1 1 d . A . C17 C -0.03513(15) 0.37849(13) 0.07115(10) 0.0266(7) Uani 1 1 d . . . H17 H -0.0517 0.3976 0.0409 0.032 Uiso 1 1 calc R . . C18 C -0.05058(14) 0.41701(13) 0.11407(10) 0.0256(6) Uani 1 1 d . . . C19 C -0.02451(14) 0.38817(13) 0.15824(9) 0.0239(6) Uani 1 1 d . . . C20 C 0.13918(15) 0.35366(13) 0.22125(9) 0.0251(6) Uani 1 1 d . . . H20A H 0.1540 0.3165 0.1970 0.030 Uiso 1 1 calc R . . H20B H 0.1743 0.3551 0.2478 0.030 Uiso 1 1 calc R . . C21 C 0.13547(15) 0.42756(13) 0.19663(9) 0.0268(6) Uani 1 1 d . . . H21A H 0.1823 0.4422 0.1851 0.032 Uiso 1 1 calc R . . H21B H 0.1041 0.4251 0.1679 0.032 Uiso 1 1 calc R . . C22 C 0.16415(16) 0.50790(14) 0.26270(11) 0.0351(7) Uani 1 1 d . . . H22A H 0.1788 0.4695 0.2855 0.053 Uiso 1 1 calc R . . H22B H 0.1468 0.5499 0.2813 0.053 Uiso 1 1 calc R . . H22C H 0.2039 0.5230 0.2426 0.053 Uiso 1 1 calc R . . C23 C -0.09860(14) 0.41587(13) 0.29824(10) 0.0259(6) Uani 1 1 d . . . H23A H -0.1011 0.4384 0.3312 0.031 Uiso 1 1 calc R . . H23B H -0.1360 0.4366 0.2775 0.031 Uiso 1 1 calc R . . C24 C -0.10521(14) 0.33552(13) 0.30161(10) 0.0258(6) Uani 1 1 d . . . C25 C -0.08085(15) 0.29698(14) 0.34257(10) 0.0296(7) Uani 1 1 d . . . H25 H -0.0621 0.3234 0.3695 0.035 Uiso 1 1 calc R . . C26 C -0.08337(16) 0.22136(14) 0.34485(11) 0.0352(7) Uani 1 1 d . . . H26 H -0.0668 0.1966 0.3731 0.042 Uiso 1 1 calc R . . C27 C -0.11031(16) 0.18179(14) 0.30556(11) 0.0364(8) Uani 1 1 d . . . H27 H -0.1116 0.1300 0.3067 0.044 Uiso 1 1 calc R . . C28 C -0.13498(16) 0.21834(14) 0.26506(11) 0.0354(7) Uani 1 1 d . . . H28 H -0.1535 0.1916 0.2382 0.042 Uiso 1 1 calc R . . C29 C -0.13305(15) 0.29407(14) 0.26316(10) 0.0305(7) Uani 1 1 d . . . H29 H -0.1510 0.3183 0.2351 0.037 Uiso 1 1 calc R . . C30 C -0.00901(15) 0.55205(12) 0.27141(10) 0.0266(7) Uani 1 1 d . . . H30A H 0.0293 0.5701 0.2925 0.032 Uiso 1 1 calc R . . H30B H -0.0017 0.5729 0.2383 0.032 Uiso 1 1 calc R . . C31 C -0.07541(15) 0.58228(12) 0.29098(10) 0.0259(7) Uani 1 1 d . . . C32 C -0.13053(15) 0.60095(13) 0.25967(12) 0.0334(7) Uani 1 1 d . . . H32 H -0.1256 0.5933 0.2254 0.040 Uiso 1 1 calc R . . C33 C -0.19169(17) 0.63010(14) 0.27741(13) 0.0410(8) Uani 1 1 d . . . H33 H -0.2278 0.6429 0.2553 0.049 Uiso 1 1 calc R . . C34 C -0.20085(18) 0.64078(15) 0.32695(15) 0.0471(9) Uani 1 1 d . . . H34 H -0.2431 0.6609 0.3391 0.057 Uiso 1 1 calc R . . C35 C -0.14781(18) 0.62188(15) 0.35887(13) 0.0441(9) Uani 1 1 d . . . H35 H -0.1539 0.6283 0.3932 0.053 Uiso 1 1 calc R . . C36 C -0.08575(16) 0.59353(13) 0.34108(11) 0.0332(7) Uani 1 1 d . . . H36 H -0.0496 0.5815 0.3634 0.040 Uiso 1 1 calc R . . C37 C 0.09796(15) 0.47452(13) 0.42061(10) 0.0258(6) Uani 1 1 d . . . C38 C 0.11252(16) 0.54178(13) 0.38894(10) 0.0317(7) Uani 1 1 d . . . H38A H 0.0959 0.5856 0.4059 0.048 Uiso 1 1 calc R . . H38B H 0.0882 0.5369 0.3575 0.048 Uiso 1 1 calc R . . H38C H 0.1627 0.5459 0.3831 0.048 Uiso 1 1 calc R . . C39 C 0.01955(16) 0.46823(14) 0.42978(10) 0.0328(7) Uani 1 1 d . . . H39A H 0.0025 0.5134 0.4449 0.049 Uiso 1 1 calc R . . H39B H 0.0105 0.4270 0.4518 0.049 Uiso 1 1 calc R . . H39C H -0.0045 0.4602 0.3986 0.049 Uiso 1 1 calc R . . C40 C 0.13348(17) 0.48659(15) 0.47033(10) 0.0375(8) Uani 1 1 d . . . H40A H 0.1837 0.4929 0.4654 0.056 Uiso 1 1 calc R . . H40B H 0.1252 0.4442 0.4915 0.056 Uiso 1 1 calc R . . H40C H 0.1143 0.5304 0.4859 0.056 Uiso 1 1 calc R . . C41 C 0.26412(15) 0.25477(13) 0.41570(9) 0.0262(6) Uani 1 1 d . . . C42 C 0.28817(17) 0.28563(15) 0.46494(10) 0.0377(8) Uani 1 1 d . . . H42A H 0.3071 0.3348 0.4601 0.057 Uiso 1 1 calc R . . H42B H 0.3243 0.2539 0.4788 0.057 Uiso 1 1 calc R . . H42C H 0.2485 0.2880 0.4875 0.057 Uiso 1 1 calc R . . C43 C 0.32588(15) 0.25395(15) 0.38015(11) 0.0338(7) Uani 1 1 d . . . H43A H 0.3419 0.3040 0.3745 0.051 Uiso 1 1 calc R . . H43B H 0.3114 0.2322 0.3489 0.051 Uiso 1 1 calc R . . H43C H 0.3639 0.2251 0.3943 0.051 Uiso 1 1 calc R . . C44 C 0.23972(16) 0.17576(13) 0.42418(10) 0.0326(7) Uani 1 1 d . . . H44A H 0.2773 0.1477 0.4395 0.049 Uiso 1 1 calc R . . H44B H 0.2274 0.1535 0.3927 0.049 Uiso 1 1 calc R . . H44C H 0.1989 0.1758 0.4458 0.049 Uiso 1 1 calc R . . C45 C 0.02147(16) 0.27457(14) 0.02203(10) 0.0291(7) Uani 1 1 d . . . C46 C -0.0106(3) 0.3112(2) -0.02248(14) 0.0399(12) Uani 0.72 1 d P A 1 H46A H 0.0063 0.3615 -0.0248 0.060 Uiso 0.72 1 calc PR A 1 H46B H -0.0614 0.3113 -0.0193 0.060 Uiso 0.72 1 calc PR A 1 H46C H 0.0027 0.2843 -0.0521 0.060 Uiso 0.72 1 calc PR A 1 C47 C 0.0993(2) 0.2705(3) 0.01776(15) 0.0445(12) Uani 0.72 1 d P A 1 H47A H 0.1119 0.2465 -0.0131 0.067 Uiso 0.72 1 calc PR A 1 H47B H 0.1182 0.2425 0.0453 0.067 Uiso 0.72 1 calc PR A 1 H47C H 0.1188 0.3200 0.0183 0.067 Uiso 0.72 1 calc PR A 1 C48 C -0.0084(2) 0.19619(19) 0.02576(14) 0.0351(10) Uani 0.72 1 d P A 1 H48A H 0.0034 0.1688 -0.0040 0.053 Uiso 0.72 1 calc PR A 1 H48B H -0.0592 0.1986 0.0292 0.053 Uiso 0.72 1 calc PR A 1 H48C H 0.0116 0.1716 0.0544 0.053 Uiso 0.72 1 calc PR A 1 C46' C -0.0403(6) 0.2470(6) -0.0074(4) 0.040(3) Uani 0.28 1 d P A 2 H46D H -0.0708 0.2880 -0.0157 0.060 Uiso 0.28 1 calc PR A 2 H46E H -0.0663 0.2113 0.0122 0.060 Uiso 0.28 1 calc PR A 2 H46F H -0.0237 0.2238 -0.0376 0.060 Uiso 0.28 1 calc PR A 2 C47' C 0.0604(7) 0.3318(6) -0.0145(4) 0.045(3) Uani 0.28 1 d P A 2 H47D H 0.0706 0.3077 -0.0457 0.068 Uiso 0.28 1 calc PR A 2 H47E H 0.1039 0.3483 0.0006 0.068 Uiso 0.28 1 calc PR A 2 H47F H 0.0300 0.3740 -0.0203 0.068 Uiso 0.28 1 calc PR A 2 C48' C 0.0760(6) 0.2098(6) 0.0253(4) 0.037(3) Uani 0.28 1 d P A 2 H48D H 0.0844 0.1901 -0.0076 0.056 Uiso 0.28 1 calc PR A 2 H48E H 0.0575 0.1712 0.0465 0.056 Uiso 0.28 1 calc PR A 2 H48F H 0.1198 0.2281 0.0390 0.056 Uiso 0.28 1 calc PR A 2 C49 C -0.09449(17) 0.48767(14) 0.11270(11) 0.0348(7) Uani 1 1 d . . . C50 C -0.04902(18) 0.55240(13) 0.12873(11) 0.0378(8) Uani 1 1 d . . . H50A H -0.0773 0.5969 0.1295 0.057 Uiso 1 1 calc R . . H50B H -0.0107 0.5587 0.1054 0.057 Uiso 1 1 calc R . . H50C H -0.0300 0.5429 0.1615 0.057 Uiso 1 1 calc R . . C51 C -0.15780(16) 0.47963(15) 0.14669(12) 0.0400(8) Uani 1 1 d . . . H51A H -0.1419 0.4691 0.1801 0.060 Uiso 1 1 calc R . . H51B H -0.1872 0.4395 0.1351 0.060 Uiso 1 1 calc R . . H51C H -0.1847 0.5251 0.1466 0.060 Uiso 1 1 calc R . . C52 C -0.1218(2) 0.50393(16) 0.06090(11) 0.0518(10) Uani 1 1 d . . . H52A H -0.1507 0.5480 0.0617 0.078 Uiso 1 1 calc R . . H52B H -0.1497 0.4626 0.0493 0.078 Uiso 1 1 calc R . . H52C H -0.0824 0.5116 0.0387 0.078 Uiso 1 1 calc R . . O53 O 0.21360(13) 0.42899(13) 0.08932(8) 0.0544(6) Uani 1 1 d . . . C54 C 0.2656(2) 0.3777(2) 0.07655(13) 0.0596(10) Uani 1 1 d . . . H54A H 0.3120 0.3974 0.0852 0.072 Uiso 1 1 calc R . . H54B H 0.2646 0.3691 0.0407 0.072 Uiso 1 1 calc R . . C55 C 0.2539(2) 0.3078(2) 0.10283(15) 0.0692(11) Uani 1 1 d . . . H55A H 0.2609 0.3153 0.1381 0.104 Uiso 1 1 calc R . . H55B H 0.2869 0.2711 0.0909 0.104 Uiso 1 1 calc R . . H55C H 0.2062 0.2910 0.0969 0.104 Uiso 1 1 calc R . . C56 C 0.2188(2) 0.4956(2) 0.06521(14) 0.0698(12) Uani 1 1 d . . . H56A H 0.2186 0.4875 0.0293 0.084 Uiso 1 1 calc R . . H56B H 0.2632 0.5196 0.0741 0.084 Uiso 1 1 calc R . . C57 C 0.1593(3) 0.5442(2) 0.07895(15) 0.0925(16) Uani 1 1 d . . . H57A H 0.1153 0.5205 0.0700 0.139 Uiso 1 1 calc R . . H57B H 0.1634 0.5907 0.0615 0.139 Uiso 1 1 calc R . . H57C H 0.1601 0.5531 0.1144 0.139 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 0.0228(3) 0.0162(2) 0.0228(3) -0.00011(19) 0.0004(2) 0.0015(2) O2 0.0252(11) 0.0188(8) 0.0237(10) -0.0007(7) 0.0001(9) 0.0019(8) O3 0.0306(11) 0.0206(9) 0.0235(10) -0.0019(7) -0.0010(9) 0.0040(8) O4 0.0304(12) 0.0204(9) 0.0296(11) 0.0005(8) 0.0031(9) -0.0002(8) N5 0.0244(13) 0.0186(10) 0.0184(12) 0.0008(8) -0.0014(10) -0.0010(9) C6 0.0228(16) 0.0192(13) 0.0215(15) 0.0033(11) 0.0014(12) 0.0000(11) C7 0.0249(17) 0.0216(13) 0.0246(16) -0.0018(11) 0.0049(13) -0.0034(12) C8 0.0274(17) 0.0247(14) 0.0198(15) -0.0004(11) -0.0016(13) -0.0017(12) C9 0.0263(17) 0.0220(13) 0.0212(15) 0.0026(11) 0.0022(13) -0.0013(12) C10 0.0322(18) 0.0184(13) 0.0260(16) -0.0006(11) 0.0034(13) 0.0027(12) C11 0.0298(17) 0.0176(13) 0.0185(14) 0.0024(10) 0.0012(13) -0.0002(11) C12 0.0320(18) 0.0172(13) 0.0229(15) 0.0039(10) -0.0008(13) 0.0035(12) C13 0.0315(17) 0.0183(13) 0.0218(15) -0.0022(11) 0.0003(13) 0.0013(11) C14 0.0234(17) 0.0195(13) 0.0242(15) 0.0023(10) -0.0005(12) -0.0009(11) C15 0.0220(16) 0.0202(13) 0.0278(16) 0.0007(11) 0.0001(13) 0.0005(11) C16 0.0249(16) 0.0249(14) 0.0234(15) 0.0030(11) -0.0006(13) -0.0046(12) C17 0.0317(18) 0.0245(14) 0.0235(16) 0.0052(11) -0.0067(13) -0.0050(12) C18 0.0245(17) 0.0230(14) 0.0295(16) 0.0009(11) -0.0033(13) -0.0002(12) C19 0.0264(17) 0.0221(13) 0.0232(16) 0.0018(11) -0.0013(13) -0.0030(11) C20 0.0274(17) 0.0244(14) 0.0235(15) -0.0029(11) 0.0013(13) 0.0024(12) C21 0.0277(17) 0.0289(14) 0.0237(15) 0.0018(12) 0.0066(13) -0.0013(12) C22 0.0336(19) 0.0305(15) 0.0412(18) -0.0028(13) 0.0044(16) -0.0110(13) C23 0.0246(17) 0.0232(14) 0.0300(16) 0.0002(11) 0.0020(13) -0.0004(11) C24 0.0216(16) 0.0247(14) 0.0310(16) -0.0011(12) 0.0057(13) -0.0028(12) C25 0.0300(18) 0.0296(15) 0.0291(16) -0.0018(12) 0.0050(14) -0.0055(13) C26 0.034(2) 0.0331(16) 0.0384(18) 0.0063(13) 0.0055(15) -0.0021(14) C27 0.040(2) 0.0233(14) 0.0460(19) -0.0007(14) 0.0127(16) -0.0060(13) C28 0.037(2) 0.0320(16) 0.0368(18) -0.0070(13) 0.0057(16) -0.0132(14) C29 0.0286(18) 0.0325(15) 0.0305(17) 0.0013(12) 0.0013(14) -0.0052(13) C30 0.0328(18) 0.0175(13) 0.0295(16) 0.0007(10) -0.0022(14) 0.0009(12) C31 0.0317(18) 0.0094(12) 0.0365(17) -0.0011(11) -0.0019(14) -0.0007(11) C32 0.0329(19) 0.0189(14) 0.049(2) 0.0012(13) -0.0031(16) -0.0023(13) C33 0.031(2) 0.0244(15) 0.067(3) 0.0007(15) -0.0055(17) -0.0027(13) C34 0.027(2) 0.0312(17) 0.083(3) -0.0087(17) 0.012(2) -0.0010(14) C35 0.046(2) 0.0314(16) 0.055(2) -0.0124(15) 0.0158(19) -0.0029(15) C36 0.037(2) 0.0228(14) 0.0402(19) -0.0045(12) 0.0007(15) -0.0018(13) C37 0.0324(18) 0.0207(13) 0.0244(15) -0.0042(11) -0.0002(13) 0.0037(12) C38 0.0365(19) 0.0212(14) 0.0374(18) -0.0062(12) -0.0010(15) -0.0018(13) C39 0.040(2) 0.0270(15) 0.0312(17) -0.0057(12) 0.0067(14) 0.0041(13) C40 0.049(2) 0.0337(16) 0.0301(17) -0.0115(13) -0.0052(16) 0.0074(14) C41 0.0269(17) 0.0272(14) 0.0246(15) 0.0019(11) 0.0003(13) 0.0034(12) C42 0.039(2) 0.0432(17) 0.0307(17) -0.0016(13) -0.0078(15) 0.0114(15) C43 0.0276(19) 0.0347(16) 0.0391(18) 0.0008(13) 0.0020(14) 0.0022(13) C44 0.036(2) 0.0288(15) 0.0334(17) 0.0061(12) 0.0058(15) 0.0071(13) C45 0.0334(19) 0.0327(15) 0.0211(16) -0.0023(12) 0.0003(13) 0.0035(13) C46 0.058(4) 0.041(2) 0.021(2) -0.0036(18) 0.000(2) 0.002(2) C47 0.040(3) 0.066(3) 0.028(2) -0.005(2) 0.010(2) -0.003(2) C48 0.047(3) 0.028(2) 0.031(2) -0.0099(17) 0.003(2) 0.0024(19) C46' 0.039(7) 0.053(7) 0.027(6) -0.011(5) 0.004(5) 0.017(6) C47' 0.058(9) 0.051(7) 0.026(6) 0.019(5) 0.025(6) 0.011(6) C48' 0.041(8) 0.043(6) 0.028(6) -0.009(5) 0.000(5) 0.016(6) C49 0.044(2) 0.0244(14) 0.0357(18) -0.0012(12) -0.0106(16) 0.0090(13) C50 0.057(2) 0.0234(15) 0.0333(18) 0.0021(12) -0.0032(16) 0.0012(14) C51 0.033(2) 0.0292(16) 0.058(2) -0.0078(14) -0.0121(17) 0.0101(14) C52 0.077(3) 0.0316(16) 0.047(2) -0.0006(14) -0.028(2) 0.0237(17) O53 0.0519(16) 0.0679(15) 0.0432(14) 0.0003(12) 0.0117(12) 0.0058(13) C54 0.048(3) 0.086(3) 0.045(2) -0.0003(19) 0.003(2) 0.002(2) C55 0.056(3) 0.075(3) 0.077(3) -0.006(2) -0.009(2) -0.001(2) C56 0.081(3) 0.082(3) 0.046(2) 0.013(2) 0.015(2) 0.001(2) C57 0.132(5) 0.091(3) 0.054(3) 0.006(2) 0.019(3) 0.044(3) _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 O3 1.8645(18) . ? Ti1 O2 1.8652(17) . ? Ti1 C23 2.141(3) . ? Ti1 C30 2.180(2) . ? Ti1 N5 2.366(2) . ? Ti1 O4 2.4334(18) . ? O2 C6 1.358(3) . ? O3 C19 1.361(3) . ? O4 C22 1.442(3) . ? O4 C21 1.444(3) . ? N5 C20 1.487(3) . ? N5 C13 1.497(3) . ? N5 C12 1.501(3) . ? C6 C7 1.405(4) . ? C6 C11 1.408(3) . ? C7 C8 1.397(4) . ? C7 C37 1.546(3) . ? C8 C9 1.397(3) . ? C8 H8 0.9500 . ? C9 C10 1.391(4) . ? C9 C41 1.533(4) . ? C10 C11 1.381(4) . ? C10 H10 0.9500 . ? C11 C12 1.497(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.502(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.385(3) . ? C14 C19 1.398(3) . ? C15 C16 1.387(3) . ? C15 H15 0.9500 . ? C16 C17 1.393(4) . ? C16 C45 1.533(4) . ? C17 C18 1.398(4) . ? C17 H17 0.9500 . ? C18 C19 1.407(4) . ? C18 C49 1.545(4) . ? C20 C21 1.512(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.480(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.401(4) . ? C24 C25 1.402(4) . ? C25 C26 1.387(4) . ? C25 H25 0.9500 . ? C26 C27 1.393(4) . ? C26 H26 0.9500 . ? C27 C28 1.376(4) . ? C27 H27 0.9500 . ? C28 C29 1.389(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.489(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C36 1.396(4) . ? C31 C32 1.402(4) . ? C32 C33 1.378(4) . ? C32 H32 0.9500 . ? C33 C34 1.376(4) . ? C33 H33 0.9500 . ? C34 C35 1.384(5) . ? C34 H34 0.9500 . ? C35 C36 1.388(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.530(4) . ? C37 C39 1.531(4) . ? C37 C40 1.533(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.528(4) . ? C41 C43 1.532(4) . ? C41 C44 1.539(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C47 1.502(5) . ? C45 C46' 1.519(11) . ? C45 C46 1.516(5) . ? C45 C48 1.550(4) . ? C45 C48' 1.585(10) . ? C45 C47' 1.628(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C46' H46D 0.9800 . ? C46' H46E 0.9800 . ? C46' H46F 0.9800 . ? C47' H47D 0.9800 . ? C47' H47E 0.9800 . ? C47' H47F 0.9800 . ? C48' H48D 0.9800 . ? C48' H48E 0.9800 . ? C48' H48F 0.9800 . ? C49 C51 1.536(4) . ? C49 C50 1.536(4) . ? C49 C52 1.536(4) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? O53 C56 1.390(4) . ? O53 C54 1.414(4) . ? C54 C55 1.484(5) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.495(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? 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 O3 Ti1 O2 163.92(7) . . ? O3 Ti1 C23 93.28(10) . . ? O2 Ti1 C23 92.01(9) . . ? O3 Ti1 C30 98.07(9) . . ? O2 Ti1 C30 96.88(9) . . ? C23 Ti1 C30 92.33(10) . . ? O3 Ti1 N5 81.92(7) . . ? O2 Ti1 N5 82.26(7) . . ? C23 Ti1 N5 119.69(8) . . ? C30 Ti1 N5 147.96(9) . . ? O3 Ti1 O4 88.71(7) . . ? O2 Ti1 O4 89.19(7) . . ? C23 Ti1 O4 168.26(7) . . ? C30 Ti1 O4 75.93(8) . . ? N5 Ti1 O4 72.03(6) . . ? C6 O2 Ti1 145.77(15) . . ? C19 O3 Ti1 145.71(16) . . ? C22 O4 C21 111.8(2) . . ? C22 O4 Ti1 121.04(15) . . ? C21 O4 Ti1 108.08(14) . . ? C20 N5 C13 110.26(19) . . ? C20 N5 C12 109.3(2) . . ? C13 N5 C12 104.28(17) . . ? C20 N5 Ti1 113.61(13) . . ? C13 N5 Ti1 109.53(15) . . ? C12 N5 Ti1 109.46(14) . . ? O2 C6 C7 122.3(2) . . ? O2 C6 C11 117.4(2) . . ? C7 C6 C11 120.3(2) . . ? C8 C7 C6 117.2(2) . . ? C8 C7 C37 120.9(2) . . ? C6 C7 C37 121.9(2) . . ? C7 C8 C9 124.0(2) . . ? C7 C8 H8 118.0 . . ? C9 C8 H8 118.0 . . ? C10 C9 C8 116.4(2) . . ? C10 C9 C41 120.1(2) . . ? C8 C9 C41 123.5(2) . . ? C11 C10 C9 122.5(2) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 C6 119.5(2) . . ? C10 C11 C12 120.0(2) . . ? C6 C11 C12 120.2(2) . . ? C11 C12 N5 116.72(19) . . ? C11 C12 H12A 108.1 . . ? N5 C12 H12A 108.1 . . ? C11 C12 H12B 108.1 . . ? N5 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? N5 C13 C14 116.7(2) . . ? N5 C13 H13A 108.1 . . ? C14 C13 H13A 108.1 . . ? N5 C13 H13B 108.1 . . ? C14 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C15 C14 C19 120.0(2) . . ? C15 C14 C13 119.9(2) . . ? C19 C14 C13 119.9(2) . . ? C14 C15 C16 121.8(2) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C15 C16 C17 116.8(2) . . ? C15 C16 C45 120.5(2) . . ? C17 C16 C45 122.7(2) . . ? C16 C17 C18 124.1(2) . . ? C16 C17 H17 118.0 . . ? C18 C17 H17 118.0 . . ? C17 C18 C19 116.8(2) . . ? C17 C18 C49 121.2(2) . . ? C19 C18 C49 122.0(2) . . ? O3 C19 C14 117.4(2) . . ? O3 C19 C18 122.3(2) . . ? C14 C19 C18 120.4(2) . . ? N5 C20 C21 110.9(2) . . ? N5 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? N5 C20 H20B 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 108.0 . . ? O4 C21 C20 109.0(2) . . ? O4 C21 H21A 109.9 . . ? C20 C21 H21A 109.9 . . ? O4 C21 H21B 109.9 . . ? C20 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 Ti1 104.81(17) . . ? C24 C23 H23A 110.8 . . ? Ti1 C23 H23A 110.8 . . ? C24 C23 H23B 110.8 . . ? Ti1 C23 H23B 110.8 . . ? H23A C23 H23B 108.9 . . ? C29 C24 C25 116.8(2) . . ? C29 C24 C23 121.7(2) . . ? C25 C24 C23 121.4(2) . . ? C26 C25 C24 121.8(3) . . ? C26 C25 H25 119.1 . . ? C24 C25 H25 119.1 . . ? C25 C26 C27 119.9(3) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 119.5(3) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C24 121.6(3) . . ? C28 C29 H29 119.2 . . ? C24 C29 H29 119.2 . . ? C31 C30 Ti1 118.26(17) . . ? C31 C30 H30A 107.7 . . ? Ti1 C30 H30A 107.7 . . ? C31 C30 H30B 107.7 . . ? Ti1 C30 H30B 107.7 . . ? H30A C30 H30B 107.1 . . ? C36 C31 C32 116.9(3) . . ? C36 C31 C30 121.8(3) . . ? C32 C31 C30 121.3(3) . . ? C33 C32 C31 121.6(3) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C34 C33 C32 120.6(3) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 119.2(3) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C34 C35 C36 120.4(3) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 121.3(3) . . ? C35 C36 H36 119.3 . . ? C31 C36 H36 119.3 . . ? C38 C37 C39 109.4(2) . . ? C38 C37 C40 107.5(2) . . ? C39 C37 C40 107.7(2) . . ? C38 C37 C7 109.7(2) . . ? C39 C37 C7 110.2(2) . . ? C40 C37 C7 112.3(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C43 109.0(2) . . ? C42 C41 C9 112.0(2) . . ? C43 C41 C9 109.5(2) . . ? C42 C41 C44 107.9(2) . . ? C43 C41 C44 108.8(2) . . ? C9 C41 C44 109.5(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 C45 C46' 136.1(5) . . ? C47 C45 C46 111.3(3) . . ? C46' C45 C46 53.7(5) . . ? C47 C45 C16 108.6(3) . . ? C46' C45 C16 115.2(4) . . ? C46 C45 C16 112.4(2) . . ? C47 C45 C48 109.2(3) . . ? C46' C45 C48 55.7(5) . . ? C46 C45 C48 108.2(3) . . ? C16 C45 C48 107.1(2) . . ? C47 C45 C48' 46.3(5) . . ? C46' C45 C48' 107.3(6) . . ? C46 C45 C48' 130.1(5) . . ? C16 C45 C48' 117.1(4) . . ? C48 C45 C48' 63.1(5) . . ? C47 C45 C47' 61.8(5) . . ? C46' C45 C47' 104.5(7) . . ? C46 C45 C47' 54.0(5) . . ? C16 C45 C47' 108.9(4) . . ? C48 C45 C47' 143.8(5) . . ? C48' C45 C47' 102.3(6) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? C45 C46' H46D 109.5 . . ? C45 C46' H46E 109.5 . . ? C45 C46' H46F 109.5 . . ? C45 C47' H47D 109.5 . . ? C45 C47' H47E 109.5 . . ? C45 C47' H47F 109.5 . . ? C45 C48' H48D 109.5 . . ? C45 C48' H48E 109.5 . . ? C51 C49 C50 110.6(2) . . ? C51 C49 C52 107.6(3) . . ? C50 C49 C52 107.8(2) . . ? C51 C49 C18 109.7(2) . . ? C50 C49 C18 109.2(2) . . ? C52 C49 C18 111.8(2) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C56 O53 C54 114.6(3) . . ? O53 C54 C55 110.3(3) . . ? O53 C54 H54A 109.6 . . ? C55 C54 H54A 109.6 . . ? O53 C54 H54B 109.6 . . ? C55 C54 H54B 109.6 . . ? H54A C54 H54B 108.1 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O53 C56 C57 110.4(3) . . ? O53 C56 H56A 109.6 . . ? C57 C56 H56A 109.6 . . ? O53 C56 H56B 109.6 . . ? C57 C56 H56B 109.6 . . ? H56A C56 H56B 108.1 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.260 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.051