# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ghosh, Prasenjit' _publ_contact_author_email pghosh@chem.iitb.ac.in _publ_section_title ; Titanium Isopropoxide Complexes of a Series of Sterically Demanding Aryloxo Based [N2O2]2- Ligands as Precatalysts for Ethylene Polymerization ; _publ_author_name P.Ghosh data_pg117 _database_code_depnum_ccdc_archive 'CCDC 643954' #TrackingRef '- Combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H72 N2 O4 Ti' _chemical_formula_weight 849.03 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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.660(3) _cell_length_b 14.159(10) _cell_length_c 15.4004(16) _cell_angle_alpha 83.58(2) _cell_angle_beta 74.622(14) _cell_angle_gamma 64.80(5) _cell_volume 2408.4(19) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11736 _cell_measurement_theta_min 2.9788 _cell_measurement_theta_max 32.9945 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_T_min 0.9064 _exptl_absorpt_correction_T_max 0.9261 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20221 _diffrn_reflns_av_R_equivalents 0.0951 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8412 _reflns_number_gt 6370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0854P)^2^+2.2394P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8412 _refine_ls_number_parameters 554 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1717 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.28525(4) 0.19392(4) 0.28297(3) 0.02018(16) Uani 1 1 d . . . O1 O 0.20826(18) 0.18070(17) 0.39791(13) 0.0289(5) Uani 1 1 d . . . O2 O 0.42652(17) 0.08190(15) 0.26435(14) 0.0288(5) Uani 1 1 d . . . O3 O 0.35361(16) 0.27947(15) 0.31127(13) 0.0225(4) Uani 1 1 d . . . O4 O 0.20006(17) 0.13640(15) 0.23697(13) 0.0238(4) Uani 1 1 d . . . N1 N 0.12663(19) 0.35993(18) 0.27388(15) 0.0209(5) Uani 1 1 d . . . N2 N 0.32704(19) 0.24275(17) 0.12904(15) 0.0194(5) Uani 1 1 d . . . C1 C 0.2452(3) 0.1531(3) 0.4795(2) 0.0380(8) Uani 1 1 d . . . H1 H 0.3347 0.1279 0.4645 0.046 Uiso 1 1 calc R . . C2 C 0.2155(5) 0.0642(4) 0.5214(3) 0.0651(12) Uani 1 1 d . . . H2A H 0.1288 0.0846 0.5314 0.098 Uiso 1 1 calc R . . H2B H 0.2383 0.0462 0.5790 0.098 Uiso 1 1 calc R . . H2C H 0.2597 0.0037 0.4810 0.098 Uiso 1 1 calc R . . C3 C 0.1930(4) 0.2471(3) 0.5378(3) 0.0631(13) Uani 1 1 d . . . H3A H 0.2155 0.3017 0.5048 0.095 Uiso 1 1 calc R . . H3B H 0.2239 0.2287 0.5922 0.095 Uiso 1 1 calc R . . H3C H 0.1051 0.2728 0.5549 0.095 Uiso 1 1 calc R . . C4 C 0.5163(4) -0.0178(3) 0.2536(4) 0.0684(14) Uani 1 1 d . . . H4 H 0.5841 -0.0122 0.2056 0.082 Uiso 1 1 calc R . . C5 C 0.5640(6) -0.0530(4) 0.3346(4) 0.105(2) Uani 1 1 d . . . H5A H 0.5807 0.0016 0.3542 0.158 Uiso 1 1 calc R . . H5B H 0.6384 -0.1167 0.3206 0.158 Uiso 1 1 calc R . . H5C H 0.5045 -0.0674 0.3829 0.158 Uiso 1 1 calc R . . C6 C 0.4848(3) -0.0931(3) 0.2185(3) 0.0473(9) Uani 1 1 d . . . H6A H 0.4258 -0.1092 0.2657 0.071 Uiso 1 1 calc R . . H6B H 0.5574 -0.1573 0.1999 0.071 Uiso 1 1 calc R . . H6C H 0.4505 -0.0626 0.1667 0.071 Uiso 1 1 calc R . . C7 C 0.3301(2) 0.3746(2) 0.33836(18) 0.0203(6) Uani 1 1 d . . . C8 C 0.4214(2) 0.3972(2) 0.35511(18) 0.0225(6) Uani 1 1 d . . . C9 C 0.5483(2) 0.3116(2) 0.3507(2) 0.0241(6) Uani 1 1 d . . . C10 C 0.6044(3) 0.2558(3) 0.2588(2) 0.0362(8) Uani 1 1 d . . . H10A H 0.6889 0.2088 0.2552 0.054 Uiso 1 1 calc R . . H10B H 0.5995 0.3077 0.2106 0.054 Uiso 1 1 calc R . . H10C H 0.5605 0.2153 0.2523 0.054 Uiso 1 1 calc R . . C11 C 0.5424(3) 0.2306(2) 0.4239(2) 0.0321(7) Uani 1 1 d . . . H11A H 0.6229 0.1744 0.4193 0.048 Uiso 1 1 calc R . . H11B H 0.4877 0.2015 0.4161 0.048 Uiso 1 1 calc R . . H11C H 0.5128 0.2637 0.4832 0.048 Uiso 1 1 calc R . . C12 C 0.6342(3) 0.3561(3) 0.3644(2) 0.0380(8) Uani 1 1 d . . . H12A H 0.6018 0.3921 0.4226 0.057 Uiso 1 1 calc R . . H12B H 0.6424 0.4055 0.3160 0.057 Uiso 1 1 calc R . . H12C H 0.7132 0.2990 0.3635 0.057 Uiso 1 1 calc R . . C13 C 0.3902(3) 0.4989(2) 0.38007(19) 0.0264(6) Uani 1 1 d . . . H13 H 0.4512 0.5153 0.3906 0.032 Uiso 1 1 calc R . . C14 C 0.2747(3) 0.5783(2) 0.3905(2) 0.0285(7) Uani 1 1 d . . . C15 C 0.2461(3) 0.6876(3) 0.4165(3) 0.0432(9) Uani 1 1 d . . . H15A H 0.1875 0.7379 0.3847 0.065 Uiso 1 1 calc R . . H15B H 0.3199 0.6993 0.4000 0.065 Uiso 1 1 calc R . . H15C H 0.2122 0.6968 0.4816 0.065 Uiso 1 1 calc R . . C16 C 0.1866(3) 0.5524(2) 0.37648(19) 0.0252(6) Uani 1 1 d . . . H16 H 0.1068 0.6047 0.3841 0.030 Uiso 1 1 calc R . . C17 C 0.2114(2) 0.4524(2) 0.35160(18) 0.0218(6) Uani 1 1 d . . . C18 C 0.1078(2) 0.4272(2) 0.34929(19) 0.0236(6) Uani 1 1 d . . . H18A H 0.0871 0.3925 0.4067 0.028 Uiso 1 1 calc R . . H18B H 0.0373 0.4938 0.3469 0.028 Uiso 1 1 calc R . . C19 C 0.0137(2) 0.3437(2) 0.2851(2) 0.0235(6) Uani 1 1 d . . . H19A H 0.0020 0.3053 0.3420 0.028 Uiso 1 1 calc R . . H19B H 0.0267 0.2983 0.2354 0.028 Uiso 1 1 calc R . . C20 C -0.1019(2) 0.4405(2) 0.28660(19) 0.0231(6) Uani 1 1 d . . . C21 C -0.1757(3) 0.4889(3) 0.3679(2) 0.0323(7) Uani 1 1 d . . . H21 H -0.1510 0.4636 0.4223 0.039 Uiso 1 1 calc R . . C22 C -0.2844(3) 0.5734(3) 0.3704(3) 0.0446(9) Uani 1 1 d . . . H22 H -0.3338 0.6058 0.4263 0.054 Uiso 1 1 calc R . . C23 C -0.3217(3) 0.6110(3) 0.2927(3) 0.0475(10) Uani 1 1 d . . . H23 H -0.3965 0.6692 0.2947 0.057 Uiso 1 1 calc R . . C24 C -0.2503(3) 0.5638(3) 0.2119(3) 0.0451(9) Uani 1 1 d . . . H24 H -0.2758 0.5894 0.1579 0.054 Uiso 1 1 calc R . . C25 C -0.1407(3) 0.4788(3) 0.2091(2) 0.0318(7) Uani 1 1 d . . . H25 H -0.0920 0.4466 0.1529 0.038 Uiso 1 1 calc R . . C26 C 0.1581(2) 0.4087(2) 0.18562(18) 0.0211(6) Uani 1 1 d . . . H26A H 0.2139 0.4398 0.1884 0.025 Uiso 1 1 calc R . . H26B H 0.0844 0.4652 0.1724 0.025 Uiso 1 1 calc R . . C27 C 0.2164(2) 0.3281(2) 0.11191(18) 0.0206(6) Uani 1 1 d . . . H27A H 0.1592 0.2990 0.1078 0.025 Uiso 1 1 calc R . . H27B H 0.2362 0.3615 0.0536 0.025 Uiso 1 1 calc R . . C28 C 0.4300(2) 0.2751(2) 0.10985(19) 0.0224(6) Uani 1 1 d . . . H28A H 0.5003 0.2155 0.1246 0.027 Uiso 1 1 calc R . . H28B H 0.4075 0.3328 0.1514 0.027 Uiso 1 1 calc R . . C29 C 0.4689(2) 0.3099(2) 0.01527(19) 0.0222(6) Uani 1 1 d . . . C30 C 0.4218(3) 0.4149(2) -0.0084(2) 0.0291(7) Uani 1 1 d . . . H30 H 0.3617 0.4647 0.0351 0.035 Uiso 1 1 calc R . . C31 C 0.4607(3) 0.4481(3) -0.0936(2) 0.0380(8) Uani 1 1 d . . . H31 H 0.4272 0.5202 -0.1083 0.046 Uiso 1 1 calc R . . C32 C 0.5477(3) 0.3773(3) -0.1572(2) 0.0388(8) Uani 1 1 d . . . H32 H 0.5744 0.4000 -0.2161 0.047 Uiso 1 1 calc R . . C33 C 0.5960(3) 0.2728(3) -0.1348(2) 0.0364(8) Uani 1 1 d . . . H33 H 0.6567 0.2235 -0.1785 0.044 Uiso 1 1 calc R . . C34 C 0.5572(3) 0.2393(3) -0.0499(2) 0.0288(7) Uani 1 1 d . . . H34 H 0.5910 0.1671 -0.0357 0.035 Uiso 1 1 calc R . . C35 C 0.3651(2) 0.1511(2) 0.07088(19) 0.0241(6) Uani 1 1 d . . . H35A H 0.4407 0.0966 0.0829 0.029 Uiso 1 1 calc R . . H35B H 0.3837 0.1728 0.0073 0.029 Uiso 1 1 calc R . . C36 C 0.2771(2) 0.1019(2) 0.08086(19) 0.0224(6) Uani 1 1 d . . . C37 C 0.2757(3) 0.0605(2) 0.0038(2) 0.0264(6) Uani 1 1 d . . . H37 H 0.3228 0.0706 -0.0527 0.032 Uiso 1 1 calc R . . C38 C 0.2074(3) 0.0050(2) 0.0072(2) 0.0297(7) Uani 1 1 d . . . C39 C 0.2037(3) -0.0373(3) -0.0772(2) 0.0445(9) Uani 1 1 d . . . H39A H 0.1824 0.0192 -0.1210 0.067 Uiso 1 1 calc R . . H39B H 0.1434 -0.0664 -0.0623 0.067 Uiso 1 1 calc R . . H39C H 0.2829 -0.0921 -0.1030 0.067 Uiso 1 1 calc R . . C40 C 0.1427(3) -0.0116(2) 0.0913(2) 0.0311(7) Uani 1 1 d . . . H40 H 0.0985 -0.0524 0.0945 0.037 Uiso 1 1 calc R . . C41 C 0.1395(2) 0.0287(2) 0.1709(2) 0.0253(6) Uani 1 1 d . . . C42 C 0.0654(3) 0.0084(2) 0.2616(2) 0.0289(7) Uani 1 1 d . . . C43 C 0.0232(3) -0.0767(3) 0.2535(3) 0.0441(9) Uani 1 1 d . . . H43A H -0.0151 -0.0938 0.3135 0.066 Uiso 1 1 calc R . . H43B H 0.0926 -0.1393 0.2260 0.066 Uiso 1 1 calc R . . H43C H -0.0348 -0.0511 0.2158 0.066 Uiso 1 1 calc R . . C44 C 0.1392(3) -0.0305(3) 0.3326(2) 0.0369(8) Uani 1 1 d . . . H44A H 0.1656 0.0225 0.3422 0.055 Uiso 1 1 calc R . . H44B H 0.2097 -0.0954 0.3117 0.055 Uiso 1 1 calc R . . H44C H 0.0896 -0.0433 0.3892 0.055 Uiso 1 1 calc R . . C45 C -0.0458(3) 0.1084(3) 0.2949(3) 0.0510(10) Uani 1 1 d . . . H45A H -0.0211 0.1592 0.3120 0.077 Uiso 1 1 calc R . . H45B H -0.0993 0.0926 0.3473 0.077 Uiso 1 1 calc R . . H45C H -0.0882 0.1376 0.2468 0.077 Uiso 1 1 calc R . . C46 C 0.2055(2) 0.0899(2) 0.16426(19) 0.0216(6) Uani 1 1 d . . . C47 C -0.0515(4) 0.7071(3) 0.2230(3) 0.0514(10) Uani 1 1 d . . . H47A H -0.1083 0.7789 0.2406 0.077 Uiso 1 1 calc R . . H47B H 0.0029 0.6791 0.2635 0.077 Uiso 1 1 calc R . . H47C H -0.0959 0.6639 0.2269 0.077 Uiso 1 1 calc R . . C48 C 0.0190(3) 0.7060(3) 0.1298(2) 0.0381(8) Uani 1 1 d . . . C49 C -0.0352(3) 0.7337(3) 0.0586(2) 0.0401(8) Uani 1 1 d . . . H49 H -0.1187 0.7505 0.0700 0.048 Uiso 1 1 calc R . . C50 C 0.0280(3) 0.7377(3) -0.0280(3) 0.0495(9) Uani 1 1 d . . . H50 H -0.0122 0.7578 -0.0755 0.059 Uiso 1 1 calc R . . C51 C 0.1502(3) 0.7124(3) -0.0467(3) 0.0451(9) Uani 1 1 d . . . H51 H 0.1946 0.7153 -0.1065 0.054 Uiso 1 1 calc R . . C52 C 0.2061(3) 0.6828(3) 0.0243(3) 0.0436(9) Uani 1 1 d . . . H52 H 0.2902 0.6638 0.0127 0.052 Uiso 1 1 calc R . . C53 C 0.1423(3) 0.6806(3) 0.1104(3) 0.0389(8) Uani 1 1 d . . . H53 H 0.1822 0.6616 0.1580 0.047 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 0.0187(3) 0.0180(3) 0.0229(3) -0.00003(19) -0.0040(2) -0.0072(2) O1 0.0319(11) 0.0352(12) 0.0214(10) 0.0019(9) -0.0042(9) -0.0172(10) O2 0.0254(10) 0.0204(11) 0.0352(12) -0.0024(9) -0.0074(9) -0.0039(9) O3 0.0172(9) 0.0216(11) 0.0280(11) -0.0047(8) -0.0048(8) -0.0067(8) O4 0.0239(10) 0.0236(11) 0.0256(10) -0.0006(8) -0.0010(8) -0.0143(8) N1 0.0178(11) 0.0222(13) 0.0227(12) 0.0003(9) -0.0049(9) -0.0084(10) N2 0.0168(11) 0.0175(12) 0.0242(12) -0.0025(9) -0.0028(9) -0.0080(9) C1 0.0398(18) 0.046(2) 0.0273(17) 0.0037(14) -0.0085(14) -0.0174(16) C2 0.090(3) 0.080(3) 0.050(2) 0.032(2) -0.034(2) -0.055(3) C3 0.071(3) 0.059(3) 0.034(2) -0.0099(18) -0.023(2) 0.005(2) C4 0.065(3) 0.034(2) 0.096(4) -0.021(2) -0.045(3) 0.008(2) C5 0.129(5) 0.047(3) 0.129(5) -0.021(3) -0.101(4) 0.020(3) C6 0.050(2) 0.0282(19) 0.060(2) -0.0026(16) -0.0172(19) -0.0097(16) C7 0.0229(14) 0.0195(15) 0.0182(14) 0.0010(11) -0.0040(11) -0.0093(11) C8 0.0212(14) 0.0254(16) 0.0208(14) 0.0001(11) -0.0042(11) -0.0101(12) C9 0.0174(13) 0.0262(16) 0.0291(16) -0.0026(12) -0.0060(12) -0.0084(12) C10 0.0187(14) 0.051(2) 0.0329(18) -0.0073(15) -0.0029(13) -0.0087(14) C11 0.0244(15) 0.0286(17) 0.0348(18) 0.0037(13) -0.0083(13) -0.0034(13) C12 0.0283(16) 0.038(2) 0.053(2) -0.0030(16) -0.0141(15) -0.0157(15) C13 0.0313(16) 0.0273(17) 0.0271(16) 0.0038(12) -0.0113(13) -0.0167(13) C14 0.0370(17) 0.0223(16) 0.0285(16) 0.0020(12) -0.0120(13) -0.0124(13) C15 0.049(2) 0.0235(18) 0.064(2) -0.0005(16) -0.0277(19) -0.0135(15) C16 0.0262(15) 0.0187(15) 0.0279(16) 0.0019(11) -0.0083(12) -0.0061(12) C17 0.0218(14) 0.0235(15) 0.0195(14) 0.0003(11) -0.0053(11) -0.0086(12) C18 0.0181(13) 0.0244(15) 0.0256(15) -0.0047(12) -0.0046(11) -0.0055(11) C19 0.0192(13) 0.0223(15) 0.0293(16) -0.0005(12) -0.0031(12) -0.0103(12) C20 0.0170(13) 0.0239(15) 0.0302(16) -0.0027(12) -0.0043(12) -0.0103(12) C21 0.0241(15) 0.0354(18) 0.0382(18) -0.0072(14) -0.0016(13) -0.0148(14) C22 0.0228(16) 0.039(2) 0.068(3) -0.0211(18) 0.0031(17) -0.0130(15) C23 0.0225(16) 0.0297(19) 0.086(3) -0.0009(19) -0.0129(19) -0.0064(14) C24 0.0365(19) 0.043(2) 0.064(3) 0.0190(18) -0.0275(18) -0.0196(17) C25 0.0258(15) 0.0354(18) 0.0380(18) 0.0005(14) -0.0110(14) -0.0144(14) C26 0.0206(13) 0.0187(14) 0.0248(15) 0.0031(11) -0.0056(11) -0.0095(11) C27 0.0186(13) 0.0199(15) 0.0249(15) 0.0031(11) -0.0071(11) -0.0090(11) C28 0.0166(13) 0.0265(16) 0.0270(15) -0.0014(12) -0.0045(11) -0.0116(12) C29 0.0195(13) 0.0244(15) 0.0266(15) -0.0001(12) -0.0073(11) -0.0117(12) C30 0.0266(15) 0.0293(17) 0.0324(17) 0.0011(13) -0.0047(13) -0.0141(13) C31 0.0383(18) 0.040(2) 0.0415(19) 0.0118(15) -0.0118(15) -0.0235(16) C32 0.0389(18) 0.058(2) 0.0281(17) 0.0093(16) -0.0071(15) -0.0309(18) C33 0.0296(16) 0.055(2) 0.0279(17) -0.0074(15) 0.0027(13) -0.0247(16) C34 0.0244(15) 0.0306(17) 0.0329(17) -0.0013(13) -0.0022(13) -0.0152(13) C35 0.0196(13) 0.0254(16) 0.0262(15) -0.0017(12) -0.0021(12) -0.0100(12) C36 0.0195(13) 0.0197(15) 0.0282(15) -0.0003(11) -0.0059(12) -0.0082(11) C37 0.0251(15) 0.0247(16) 0.0285(16) -0.0010(12) -0.0048(12) -0.0101(12) C38 0.0290(16) 0.0303(17) 0.0339(17) -0.0029(13) -0.0110(13) -0.0135(13) C39 0.050(2) 0.056(2) 0.040(2) -0.0095(17) -0.0112(17) -0.0318(19) C40 0.0286(16) 0.0313(17) 0.0415(19) -0.0016(14) -0.0123(14) -0.0174(13) C41 0.0196(14) 0.0242(16) 0.0328(16) 0.0013(12) -0.0064(12) -0.0100(12) C42 0.0251(15) 0.0249(16) 0.0367(17) -0.0007(13) -0.0033(13) -0.0125(13) C43 0.052(2) 0.051(2) 0.044(2) 0.0017(17) -0.0066(17) -0.0382(19) C44 0.0428(19) 0.040(2) 0.0325(18) 0.0037(14) -0.0040(15) -0.0249(16) C45 0.0275(17) 0.038(2) 0.068(3) 0.0025(18) 0.0130(17) -0.0103(16) C46 0.0198(13) 0.0190(14) 0.0274(15) 0.0000(11) -0.0091(11) -0.0074(11) C47 0.060(2) 0.045(2) 0.053(2) 0.0021(18) -0.010(2) -0.028(2) C48 0.0412(19) 0.0267(18) 0.045(2) -0.0063(14) -0.0050(16) -0.0142(15) C49 0.0264(16) 0.038(2) 0.054(2) -0.0017(16) -0.0159(16) -0.0083(14) C50 0.046(2) 0.053(2) 0.052(2) 0.0031(18) -0.0179(19) -0.0211(19) C51 0.044(2) 0.044(2) 0.051(2) -0.0035(17) -0.0028(17) -0.0261(17) C52 0.0302(17) 0.037(2) 0.065(3) -0.0075(17) -0.0094(17) -0.0146(15) C53 0.0338(18) 0.0264(18) 0.060(2) -0.0050(15) -0.0177(17) -0.0112(14) _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 O2 1.792(2) . ? Ti1 O1 1.812(2) . ? Ti1 O4 1.900(2) . ? Ti1 O3 1.902(2) . ? Ti1 N1 2.373(3) . ? Ti1 N2 2.378(2) . ? O1 C1 1.413(4) . ? O2 C4 1.377(4) . ? O3 C7 1.340(3) . ? O4 C46 1.334(3) . ? N1 C18 1.490(3) . ? N1 C26 1.490(4) . ? N1 C19 1.505(3) . ? N2 C27 1.475(3) . ? N2 C35 1.489(4) . ? N2 C28 1.506(3) . ? C1 C3 1.489(5) . ? C1 C2 1.495(6) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.474(6) . ? C4 C6 1.481(6) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C17 1.411(4) . ? C7 C8 1.413(4) . ? C8 C13 1.393(4) . ? C8 C9 1.534(4) . ? C9 C11 1.527(4) . ? C9 C12 1.537(4) . ? C9 C10 1.539(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.394(4) . ? C13 H13 0.9500 . ? C14 C16 1.384(4) . ? C14 C15 1.507(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.389(4) . ? C16 H16 0.9500 . ? C17 C18 1.509(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.517(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.379(4) . ? C20 C21 1.392(4) . ? C21 C22 1.382(5) . ? C21 H21 0.9500 . ? C22 C23 1.371(6) . ? C22 H22 0.9500 . ? C23 C24 1.373(6) . ? C23 H23 0.9500 . ? C24 C25 1.391(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.505(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.508(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.390(4) . ? C29 C30 1.392(4) . ? C30 C31 1.379(5) . ? C30 H30 0.9500 . ? C31 C32 1.373(5) . ? C31 H31 0.9500 . ? C32 C33 1.383(5) . ? C32 H32 0.9500 . ? C33 C34 1.377(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.515(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.388(4) . ? C36 C46 1.402(4) . ? C37 C38 1.382(4) . ? C37 H37 0.9500 . ? C38 C40 1.392(4) . ? C38 C39 1.511(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.393(4) . ? C40 H40 0.9500 . ? C41 C46 1.418(4) . ? C41 C42 1.535(4) . ? C42 C45 1.528(5) . ? C42 C44 1.530(5) . ? C42 C43 1.539(4) . ? 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 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 C48 1.473(5) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.377(5) . ? C48 C53 1.398(5) . ? C49 C50 1.371(5) . ? C49 H49 0.9500 . ? C50 C51 1.386(5) . ? C50 H50 0.9500 . ? C51 C52 1.389(5) . ? C51 H51 0.9500 . ? C52 C53 1.362(5) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? 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 O2 Ti1 O1 104.86(10) . . ? O2 Ti1 O4 97.23(10) . . ? O1 Ti1 O4 91.59(9) . . ? O2 Ti1 O3 92.28(10) . . ? O1 Ti1 O3 95.76(9) . . ? O4 Ti1 O3 166.09(9) . . ? O2 Ti1 N1 164.48(9) . . ? O1 Ti1 N1 89.78(9) . . ? O4 Ti1 N1 87.31(9) . . ? O3 Ti1 N1 80.95(9) . . ? O2 Ti1 N2 90.91(9) . . ? O1 Ti1 N2 163.02(9) . . ? O4 Ti1 N2 80.01(8) . . ? O3 Ti1 N2 89.75(9) . . ? N1 Ti1 N2 75.20(8) . . ? C1 O1 Ti1 133.3(2) . . ? C4 O2 Ti1 165.2(3) . . ? C7 O3 Ti1 144.80(17) . . ? C46 O4 Ti1 141.98(18) . . ? C18 N1 C26 110.3(2) . . ? C18 N1 C19 108.1(2) . . ? C26 N1 C19 112.0(2) . . ? C18 N1 Ti1 109.56(16) . . ? C26 N1 Ti1 109.21(16) . . ? C19 N1 Ti1 107.65(17) . . ? C27 N2 C35 110.5(2) . . ? C27 N2 C28 112.0(2) . . ? C35 N2 C28 107.6(2) . . ? C27 N2 Ti1 107.97(16) . . ? C35 N2 Ti1 109.41(17) . . ? C28 N2 Ti1 109.37(16) . . ? O1 C1 C3 109.8(3) . . ? O1 C1 C2 108.9(3) . . ? C3 C1 C2 115.0(4) . . ? O1 C1 H1 107.6 . . ? C3 C1 H1 107.6 . . ? C2 C1 H1 107.6 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 C5 111.4(4) . . ? O2 C4 C6 113.8(3) . . ? C5 C4 C6 114.6(4) . . ? O2 C4 H4 105.3 . . ? C5 C4 H4 105.3 . . ? C6 C4 H4 105.3 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C17 118.9(2) . . ? O3 C7 C8 121.1(2) . . ? C17 C7 C8 120.0(3) . . ? C13 C8 C7 117.3(3) . . ? C13 C8 C9 121.3(3) . . ? C7 C8 C9 121.3(3) . . ? C11 C9 C8 109.6(2) . . ? C11 C9 C12 108.4(3) . . ? C8 C9 C12 111.8(2) . . ? C11 C9 C10 108.4(3) . . ? C8 C9 C10 111.6(2) . . ? C12 C9 C10 106.8(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 C14 123.8(3) . . ? C8 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? C16 C14 C13 117.2(3) . . ? C16 C14 C15 121.2(3) . . ? C13 C14 C15 121.7(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 C17 122.0(3) . . ? C14 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C16 C17 C7 119.5(3) . . ? C16 C17 C18 118.5(2) . . ? C7 C17 C18 121.6(3) . . ? N1 C18 C17 116.9(2) . . ? N1 C18 H18A 108.1 . . ? C17 C18 H18A 108.1 . . ? N1 C18 H18B 108.1 . . ? C17 C18 H18B 108.1 . . ? H18A C18 H18B 107.3 . . ? N1 C19 C20 117.1(2) . . ? N1 C19 H19A 108.0 . . ? C20 C19 H19A 108.0 . . ? N1 C19 H19B 108.0 . . ? C20 C19 H19B 108.0 . . ? H19A C19 H19B 107.3 . . ? C25 C20 C21 118.2(3) . . ? C25 C20 C19 121.4(3) . . ? C21 C20 C19 120.3(3) . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 C21 120.6(3) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 119.6(3) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C20 C25 C24 120.9(3) . . ? C20 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? N1 C26 C27 110.1(2) . . ? N1 C26 H26A 109.6 . . ? C27 C26 H26A 109.6 . . ? N1 C26 H26B 109.6 . . ? C27 C26 H26B 109.6 . . ? H26A C26 H26B 108.2 . . ? N2 C27 C26 111.2(2) . . ? N2 C27 H27A 109.4 . . ? C26 C27 H27A 109.4 . . ? N2 C27 H27B 109.4 . . ? C26 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? N2 C28 C29 117.1(2) . . ? N2 C28 H28A 108.0 . . ? C29 C28 H28A 108.0 . . ? N2 C28 H28B 108.0 . . ? C29 C28 H28B 108.0 . . ? H28A C28 H28B 107.3 . . ? C34 C29 C30 117.7(3) . . ? C34 C29 C28 121.3(3) . . ? C30 C29 C28 120.9(3) . . ? C31 C30 C29 121.3(3) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C32 C31 C30 120.2(3) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 119.3(3) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C34 C33 C32 120.7(3) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C29 120.8(3) . . ? C33 C34 H34 119.6 . . ? C29 C34 H34 119.6 . . ? N2 C35 C36 117.3(2) . . ? N2 C35 H35A 108.0 . . ? C36 C35 H35A 108.0 . . ? N2 C35 H35B 108.0 . . ? C36 C35 H35B 108.0 . . ? H35A C35 H35B 107.2 . . ? C37 C36 C46 119.6(3) . . ? C37 C36 C35 117.2(3) . . ? C46 C36 C35 123.0(2) . . ? C38 C37 C36 121.7(3) . . ? C38 C37 H37 119.2 . . ? C36 C37 H37 119.2 . . ? C37 C38 C40 117.9(3) . . ? C37 C38 C39 121.4(3) . . ? C40 C38 C39 120.7(3) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 C41 123.2(3) . . ? C38 C40 H40 118.4 . . ? C41 C40 H40 118.4 . . ? C40 C41 C46 117.3(3) . . ? C40 C41 C42 120.7(3) . . ? C46 C41 C42 121.9(3) . . ? C45 C42 C44 109.5(3) . . ? C45 C42 C41 109.7(3) . . ? C44 C42 C41 111.7(2) . . ? C45 C42 C43 108.2(3) . . ? C44 C42 C43 106.1(3) . . ? C41 C42 C43 111.6(3) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O4 C46 C36 119.4(2) . . ? O4 C46 C41 120.5(3) . . ? C36 C46 C41 120.1(3) . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C48 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C53 117.4(3) . . ? C49 C48 C47 121.1(3) . . ? C53 C48 C47 121.4(3) . . ? C50 C49 C48 121.9(3) . . ? C50 C49 H49 119.1 . . ? C48 C49 H49 119.1 . . ? C49 C50 C51 120.4(4) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C50 C51 C52 118.2(4) . . ? C50 C51 H51 120.9 . . ? C52 C51 H51 120.9 . . ? C53 C52 C51 121.0(3) . . ? C53 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? C52 C53 C48 121.1(3) . . ? C52 C53 H53 119.5 . . ? C48 C53 H53 119.5 . . ? 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 O2 Ti1 O1 C1 44.1(3) . . . . ? O4 Ti1 O1 C1 142.0(3) . . . . ? O3 Ti1 O1 C1 -49.8(3) . . . . ? N1 Ti1 O1 C1 -130.7(3) . . . . ? N2 Ti1 O1 C1 -158.2(3) . . . . ? O1 Ti1 O2 C4 63.2(10) . . . . ? O4 Ti1 O2 C4 -30.4(10) . . . . ? O3 Ti1 O2 C4 159.8(10) . . . . ? N1 Ti1 O2 C4 -136.6(10) . . . . ? N2 Ti1 O2 C4 -110.4(10) . . . . ? O2 Ti1 O3 C7 -176.3(3) . . . . ? O1 Ti1 O3 C7 -71.1(3) . . . . ? O4 Ti1 O3 C7 50.5(5) . . . . ? N1 Ti1 O3 C7 17.7(3) . . . . ? N2 Ti1 O3 C7 92.8(3) . . . . ? O2 Ti1 O4 C46 -53.9(3) . . . . ? O1 Ti1 O4 C46 -159.1(3) . . . . ? O3 Ti1 O4 C46 78.9(5) . . . . ? N1 Ti1 O4 C46 111.2(3) . . . . ? N2 Ti1 O4 C46 35.8(3) . . . . ? O2 Ti1 N1 C18 -106.5(3) . . . . ? O1 Ti1 N1 C18 54.37(18) . . . . ? O4 Ti1 N1 C18 145.98(18) . . . . ? O3 Ti1 N1 C18 -41.50(17) . . . . ? N2 Ti1 N1 C18 -133.65(18) . . . . ? O2 Ti1 N1 C26 14.4(4) . . . . ? O1 Ti1 N1 C26 175.28(17) . . . . ? O4 Ti1 N1 C26 -93.11(17) . . . . ? O3 Ti1 N1 C26 79.41(17) . . . . ? N2 Ti1 N1 C26 -12.74(16) . . . . ? O2 Ti1 N1 C19 136.2(3) . . . . ? O1 Ti1 N1 C19 -62.92(17) . . . . ? O4 Ti1 N1 C19 28.69(17) . . . . ? O3 Ti1 N1 C19 -158.79(17) . . . . ? N2 Ti1 N1 C19 109.05(17) . . . . ? O2 Ti1 N2 C27 170.31(17) . . . . ? O1 Ti1 N2 C27 11.8(4) . . . . ? O4 Ti1 N2 C27 73.12(17) . . . . ? O3 Ti1 N2 C27 -97.42(17) . . . . ? N1 Ti1 N2 C27 -16.72(16) . . . . ? O2 Ti1 N2 C35 50.05(17) . . . . ? O1 Ti1 N2 C35 -108.4(3) . . . . ? O4 Ti1 N2 C35 -47.13(16) . . . . ? O3 Ti1 N2 C35 142.32(16) . . . . ? N1 Ti1 N2 C35 -136.97(17) . . . . ? O2 Ti1 N2 C28 -67.57(18) . . . . ? O1 Ti1 N2 C28 134.0(3) . . . . ? O4 Ti1 N2 C28 -164.75(17) . . . . ? O3 Ti1 N2 C28 24.70(17) . . . . ? N1 Ti1 N2 C28 105.41(18) . . . . ? Ti1 O1 C1 C3 107.7(3) . . . . ? Ti1 O1 C1 C2 -125.6(3) . . . . ? Ti1 O2 C4 C5 -102.2(9) . . . . ? Ti1 O2 C4 C6 29.3(13) . . . . ? Ti1 O3 C7 C17 -2.9(5) . . . . ? Ti1 O3 C7 C8 176.0(2) . . . . ? O3 C7 C8 C13 177.9(2) . . . . ? C17 C7 C8 C13 -3.2(4) . . . . ? O3 C7 C8 C9 -5.2(4) . . . . ? C17 C7 C8 C9 173.7(2) . . . . ? C13 C8 C9 C11 112.9(3) . . . . ? C7 C8 C9 C11 -63.9(3) . . . . ? C13 C8 C9 C12 -7.4(4) . . . . ? C7 C8 C9 C12 175.8(3) . . . . ? C13 C8 C9 C10 -127.0(3) . . . . ? C7 C8 C9 C10 56.2(4) . . . . ? C7 C8 C13 C14 0.9(4) . . . . ? C9 C8 C13 C14 -176.0(3) . . . . ? C8 C13 C14 C16 1.2(5) . . . . ? C8 C13 C14 C15 -179.2(3) . . . . ? C13 C14 C16 C17 -1.0(4) . . . . ? C15 C14 C16 C17 179.3(3) . . . . ? C14 C16 C17 C7 -1.2(4) . . . . ? C14 C16 C17 C18 172.3(3) . . . . ? O3 C7 C17 C16 -177.7(3) . . . . ? C8 C7 C17 C16 3.4(4) . . . . ? O3 C7 C17 C18 9.1(4) . . . . ? C8 C7 C17 C18 -169.9(3) . . . . ? C26 N1 C18 C17 -57.9(3) . . . . ? C19 N1 C18 C17 179.3(2) . . . . ? Ti1 N1 C18 C17 62.3(3) . . . . ? C16 C17 C18 N1 140.7(3) . . . . ? C7 C17 C18 N1 -46.0(4) . . . . ? C18 N1 C19 C20 58.6(3) . . . . ? C26 N1 C19 C20 -63.1(3) . . . . ? Ti1 N1 C19 C20 176.84(19) . . . . ? N1 C19 C20 C25 92.5(3) . . . . ? N1 C19 C20 C21 -91.8(3) . . . . ? C25 C20 C21 C22 -0.4(5) . . . . ? C19 C20 C21 C22 -176.3(3) . . . . ? C20 C21 C22 C23 0.2(5) . . . . ? C21 C22 C23 C24 0.1(5) . . . . ? C22 C23 C24 C25 -0.2(5) . . . . ? C21 C20 C25 C24 0.4(5) . . . . ? C19 C20 C25 C24 176.2(3) . . . . ? C23 C24 C25 C20 -0.1(5) . . . . ? C18 N1 C26 C27 161.2(2) . . . . ? C19 N1 C26 C27 -78.4(3) . . . . ? Ti1 N1 C26 C27 40.7(2) . . . . ? C35 N2 C27 C26 164.6(2) . . . . ? C28 N2 C27 C26 -75.4(3) . . . . ? Ti1 N2 C27 C26 45.0(2) . . . . ? N1 C26 C27 N2 -59.5(3) . . . . ? C27 N2 C28 C29 -59.8(3) . . . . ? C35 N2 C28 C29 61.8(3) . . . . ? Ti1 N2 C28 C29 -179.43(18) . . . . ? N2 C28 C29 C34 -90.3(3) . . . . ? N2 C28 C29 C30 92.9(3) . . . . ? C34 C29 C30 C31 0.3(4) . . . . ? C28 C29 C30 C31 177.1(3) . . . . ? C29 C30 C31 C32 -0.1(5) . . . . ? C30 C31 C32 C33 -0.2(5) . . . . ? C31 C32 C33 C34 0.4(5) . . . . ? C32 C33 C34 C29 -0.3(5) . . . . ? C30 C29 C34 C33 -0.1(4) . . . . ? C28 C29 C34 C33 -176.9(3) . . . . ? C27 N2 C35 C36 -59.6(3) . . . . ? C28 N2 C35 C36 177.8(2) . . . . ? Ti1 N2 C35 C36 59.1(3) . . . . ? N2 C35 C36 C37 146.0(3) . . . . ? N2 C35 C36 C46 -38.9(4) . . . . ? C46 C36 C37 C38 -1.7(4) . . . . ? C35 C36 C37 C38 173.6(3) . . . . ? C36 C37 C38 C40 -2.2(4) . . . . ? C36 C37 C38 C39 178.3(3) . . . . ? C37 C38 C40 C41 2.8(5) . . . . ? C39 C38 C40 C41 -177.7(3) . . . . ? C38 C40 C41 C46 0.4(4) . . . . ? C38 C40 C41 C42 179.5(3) . . . . ? C40 C41 C42 C45 -107.7(3) . . . . ? C46 C41 C42 C45 71.2(4) . . . . ? C40 C41 C42 C44 130.7(3) . . . . ? C46 C41 C42 C44 -50.3(4) . . . . ? C40 C41 C42 C43 12.2(4) . . . . ? C46 C41 C42 C43 -168.9(3) . . . . ? Ti1 O4 C46 C36 -21.3(4) . . . . ? Ti1 O4 C46 C41 158.7(2) . . . . ? C37 C36 C46 O4 -175.0(3) . . . . ? C35 C36 C46 O4 10.0(4) . . . . ? C37 C36 C46 C41 5.1(4) . . . . ? C35 C36 C46 C41 -169.9(3) . . . . ? C40 C41 C46 O4 175.6(3) . . . . ? C42 C41 C46 O4 -3.4(4) . . . . ? C40 C41 C46 C36 -4.4(4) . . . . ? C42 C41 C46 C36 176.6(3) . . . . ? C53 C48 C49 C50 -0.7(5) . . . . ? C47 C48 C49 C50 177.0(3) . . . . ? C48 C49 C50 C51 0.7(6) . . . . ? C49 C50 C51 C52 0.3(6) . . . . ? C50 C51 C52 C53 -1.3(5) . . . . ? C51 C52 C53 C48 1.4(5) . . . . ? C49 C48 C53 C52 -0.3(5) . . . . ? C47 C48 C53 C52 -178.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.199 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.078 #===END data_pg232 _database_code_depnum_ccdc_archive 'CCDC 709171' #TrackingRef '- Combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H71 Cl2 N2 O4 Ti' _chemical_formula_weight 942.94 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' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.046(4) _cell_length_b 13.411(5) _cell_length_c 17.802(6) _cell_angle_alpha 95.17(3) _cell_angle_beta 102.22(3) _cell_angle_gamma 110.10(3) _cell_volume 2597.8(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1498 _cell_measurement_theta_min 2.9483 _cell_measurement_theta_max 29.0113 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1006 _exptl_absorpt_coefficient_mu 0.313 _exptl_absorpt_correction_T_min 0.9315 _exptl_absorpt_correction_T_max 0.9546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18346 _diffrn_reflns_av_R_equivalents 0.1056 _diffrn_reflns_av_sigmaI/netI 0.2319 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9114 _reflns_number_gt 4175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0508P)^2^+0.0000P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9114 _refine_ls_number_parameters 589 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2158 _refine_ls_R_factor_gt 0.0918 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1424 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.79104(9) 0.18710(9) 0.77824(6) 0.0236(3) Uani 1 1 d . . . Cl1 Cl 0.67273(16) 0.80376(15) 0.93246(13) 0.0714(7) Uani 1 1 d . . . Cl2 Cl 0.7369(2) 0.40117(17) 0.30472(10) 0.0685(7) Uani 1 1 d . . . O1 O 0.9545(3) 0.2701(3) 0.7776(2) 0.0251(10) Uani 1 1 d . . . O2 O 0.6231(3) 0.1385(3) 0.7745(2) 0.0222(10) Uani 1 1 d . . . O3 O 0.8336(3) 0.1724(3) 0.8793(2) 0.0311(11) Uani 1 1 d . . . O4 O 0.7874(3) 0.0683(3) 0.7208(2) 0.0316(11) Uani 1 1 d . . . N1 N 0.7967(4) 0.3639(4) 0.8139(3) 0.0216(12) Uani 1 1 d . . . N2 N 0.7151(4) 0.2359(4) 0.6573(2) 0.0237(12) Uani 1 1 d . . . C1 C 1.0489(5) 0.3614(5) 0.8107(3) 0.0224(15) Uani 1 1 d . . . C2 C 1.1680(5) 0.3788(5) 0.8030(3) 0.0229(15) Uani 1 1 d . . . C3 C 1.2595(5) 0.4771(5) 0.8382(3) 0.0246(15) Uani 1 1 d . . . H3 H 1.3403 0.4875 0.8351 0.029 Uiso 1 1 calc R . . C4 C 1.2416(5) 0.5623(5) 0.8781(3) 0.0264(16) Uani 1 1 d . . . C5 C 1.1255(5) 0.5425(5) 0.8849(3) 0.0272(16) Uani 1 1 d . . . H5 H 1.1094 0.5989 0.9111 0.033 Uiso 1 1 calc R . . C6 C 1.0294(5) 0.4432(5) 0.8552(3) 0.0203(14) Uani 1 1 d . . . C7 C 1.1952(5) 0.2897(5) 0.7583(4) 0.0298(16) Uani 1 1 d . . . C8 C 1.1193(5) 0.2576(5) 0.6719(3) 0.0402(18) Uani 1 1 d . . . H8A H 1.1307 0.3226 0.6484 0.060 Uiso 1 1 calc R . . H8B H 1.0325 0.2212 0.6694 0.060 Uiso 1 1 calc R . . H8C H 1.1469 0.2088 0.6431 0.060 Uiso 1 1 calc R . . C9 C 1.1596(5) 0.1885(5) 0.7951(4) 0.0372(18) Uani 1 1 d . . . H9A H 1.1750 0.1314 0.7657 0.056 Uiso 1 1 calc R . . H9B H 1.0725 0.1643 0.7938 0.056 Uiso 1 1 calc R . . H9C H 1.2085 0.2050 0.8494 0.056 Uiso 1 1 calc R . . C10 C 1.3280(5) 0.3222(5) 0.7590(4) 0.0402(18) Uani 1 1 d . . . H10A H 1.3780 0.3414 0.8131 0.060 Uiso 1 1 calc R . . H10B H 1.3519 0.3845 0.7328 0.060 Uiso 1 1 calc R . . H10C H 1.3406 0.2619 0.7316 0.060 Uiso 1 1 calc R . . C11 C 1.3454(5) 0.6698(5) 0.9128(4) 0.0427(19) Uani 1 1 d . . . H11A H 1.4047 0.6604 0.9557 0.064 Uiso 1 1 calc R . . H11B H 1.3127 0.7214 0.9325 0.064 Uiso 1 1 calc R . . H11C H 1.3858 0.6971 0.8724 0.064 Uiso 1 1 calc R . . C12 C 0.9108(5) 0.4265(5) 0.8762(3) 0.0255(15) Uani 1 1 d . . . H12A H 0.9099 0.3892 0.9217 0.031 Uiso 1 1 calc R . . H12B H 0.9089 0.4982 0.8930 0.031 Uiso 1 1 calc R . . C13 C 0.6918(5) 0.3663(5) 0.8465(3) 0.0294(16) Uani 1 1 d . . . H13A H 0.6148 0.3193 0.8079 0.035 Uiso 1 1 calc R . . H13B H 0.6964 0.3333 0.8941 0.035 Uiso 1 1 calc R . . C14 C 0.6824(5) 0.4737(5) 0.8673(3) 0.0257(15) Uani 1 1 d . . . C15 C 0.7346(5) 0.5321(5) 0.9433(3) 0.0354(18) Uani 1 1 d . . . H15 H 0.7745 0.5027 0.9820 0.042 Uiso 1 1 calc R . . C16 C 0.7291(5) 0.6324(6) 0.9632(4) 0.042(2) Uani 1 1 d . . . H16 H 0.7647 0.6711 1.0152 0.051 Uiso 1 1 calc R . . C17 C 0.6720(6) 0.6751(6) 0.9073(4) 0.0418(19) Uani 1 1 d . . . C18 C 0.6189(5) 0.6185(6) 0.8330(4) 0.0400(19) Uani 1 1 d . . . H18 H 0.5786 0.6484 0.7948 0.048 Uiso 1 1 calc R . . C19 C 0.6232(5) 0.5181(5) 0.8127(3) 0.0314(17) Uani 1 1 d . . . H19 H 0.5851 0.4794 0.7608 0.038 Uiso 1 1 calc R . . C20 C 0.7963(5) 0.4133(5) 0.7431(3) 0.0292(16) Uani 1 1 d . . . H20A H 0.8765 0.4297 0.7310 0.035 Uiso 1 1 calc R . . H20B H 0.7834 0.4819 0.7526 0.035 Uiso 1 1 calc R . . C21 C 0.6951(5) 0.3372(5) 0.6740(3) 0.0238(15) Uani 1 1 d . . . H21A H 0.6148 0.3212 0.6860 0.029 Uiso 1 1 calc R . . H21B H 0.6941 0.3724 0.6275 0.029 Uiso 1 1 calc R . . C22 C 0.8098(5) 0.2487(5) 0.6122(3) 0.0263(16) Uani 1 1 d . . . H22A H 0.8888 0.3010 0.6458 0.032 Uiso 1 1 calc R . . H22B H 0.8192 0.1785 0.6031 0.032 Uiso 1 1 calc R . . C23 C 0.7880(5) 0.2851(5) 0.5351(3) 0.0224(15) Uani 1 1 d . . . C24 C 0.8415(5) 0.3932(5) 0.5315(4) 0.0338(17) Uani 1 1 d . . . H24 H 0.8900 0.4434 0.5779 0.041 Uiso 1 1 calc R . . C25 C 0.8252(6) 0.4291(6) 0.4609(4) 0.0406(18) Uani 1 1 d . . . H25 H 0.8617 0.5037 0.4593 0.049 Uiso 1 1 calc R . . C26 C 0.7563(6) 0.3570(6) 0.3930(4) 0.0390(18) Uani 1 1 d . . . C27 C 0.7031(6) 0.2493(6) 0.3951(4) 0.0394(19) Uani 1 1 d . . . H27 H 0.6550 0.1994 0.3485 0.047 Uiso 1 1 calc R . . C28 C 0.7204(5) 0.2142(5) 0.4659(3) 0.0296(16) Uani 1 1 d . . . H28 H 0.6848 0.1393 0.4670 0.035 Uiso 1 1 calc R . . C29 C 0.5992(5) 0.1494(5) 0.6097(3) 0.0280(16) Uani 1 1 d . . . H29A H 0.6181 0.0856 0.5941 0.034 Uiso 1 1 calc R . . H29B H 0.5713 0.1748 0.5612 0.034 Uiso 1 1 calc R . . C30 C 0.4931(5) 0.1130(4) 0.6472(3) 0.0232(15) Uani 1 1 d . . . C31 C 0.3762(5) 0.0807(5) 0.5992(3) 0.0262(16) Uani 1 1 d . . . H31 H 0.3661 0.0938 0.5471 0.031 Uiso 1 1 calc R . . C32 C 0.2729(5) 0.0295(5) 0.6245(3) 0.0276(16) Uani 1 1 d . . . C33 C 0.2947(5) 0.0134(4) 0.7005(3) 0.0222(15) Uani 1 1 d . . . H33 H 0.2256 -0.0246 0.7182 0.027 Uiso 1 1 calc R . . C34 C 0.4090(5) 0.0478(4) 0.7538(3) 0.0224(15) Uani 1 1 d . . . C35 C 0.5116(5) 0.1017(4) 0.7259(3) 0.0221(15) Uani 1 1 d . . . C36 C 0.4267(5) 0.0250(5) 0.8386(3) 0.0249(15) Uani 1 1 d . . . C37 C 0.3043(5) -0.0382(5) 0.8549(3) 0.0381(17) Uani 1 1 d . . . H37A H 0.2552 0.0069 0.8537 0.057 Uiso 1 1 calc R . . H37B H 0.3193 -0.0586 0.9065 0.057 Uiso 1 1 calc R . . H37C H 0.2601 -0.1033 0.8150 0.057 Uiso 1 1 calc R . . C38 C 0.5052(6) -0.0440(5) 0.8513(4) 0.0392(18) Uani 1 1 d . . . H38A H 0.5047 -0.0682 0.9016 0.059 Uiso 1 1 calc R . . H38B H 0.5895 -0.0011 0.8512 0.059 Uiso 1 1 calc R . . H38C H 0.4718 -0.1070 0.8092 0.059 Uiso 1 1 calc R . . C39 C 0.4891(5) 0.1295(5) 0.8991(3) 0.0373(18) Uani 1 1 d . . . H39A H 0.4452 0.1781 0.8879 0.056 Uiso 1 1 calc R . . H39B H 0.5740 0.1645 0.8967 0.056 Uiso 1 1 calc R . . H39C H 0.4880 0.1126 0.9515 0.056 Uiso 1 1 calc R . . C40 C 0.1465(5) -0.0103(5) 0.5701(3) 0.0401(19) Uani 1 1 d . . . H40A H 0.1344 -0.0741 0.5331 0.060 Uiso 1 1 calc R . . H40B H 0.1371 0.0466 0.5413 0.060 Uiso 1 1 calc R . . H40C H 0.0855 -0.0291 0.6005 0.060 Uiso 1 1 calc R . . C41 C 0.9385(6) 0.1681(5) 0.9308(3) 0.0349(17) Uani 1 1 d . . . H41 H 1.0125 0.2256 0.9236 0.042 Uiso 1 1 calc R . . C42 C 0.9494(6) 0.0596(5) 0.9115(4) 0.0465(19) Uani 1 1 d . . . H42A H 0.8778 0.0021 0.9185 0.070 Uiso 1 1 calc R . . H42B H 1.0238 0.0589 0.9464 0.070 Uiso 1 1 calc R . . H42C H 0.9535 0.0480 0.8572 0.070 Uiso 1 1 calc R . . C43 C 0.9335(7) 0.1904(6) 1.0144(4) 0.062(2) Uani 1 1 d . . . H43A H 0.9327 0.2629 1.0261 0.093 Uiso 1 1 calc R . . H43B H 1.0055 0.1857 1.0494 0.093 Uiso 1 1 calc R . . H43C H 0.8591 0.1370 1.0219 0.093 Uiso 1 1 calc R . . C48 C 0.4488(9) 0.5092(12) 0.5614(6) 0.105(5) Uani 1 1 d . . . H48 H 0.4132 0.5152 0.6036 0.127 Uiso 1 1 calc R . . C47 C 0.4676(9) 0.4181(10) 0.5399(6) 0.109(4) Uani 1 1 d . . . H47 H 0.4455 0.3604 0.5680 0.131 Uiso 1 1 calc R . . C49 C 0.4823(9) 0.5933(9) 0.5210(7) 0.099(5) Uani 1 1 d . . . H49 H 0.4707 0.6583 0.5353 0.119 Uiso 1 1 calc R . . C44 C 0.7670(6) -0.0414(5) 0.6995(4) 0.047(2) Uani 1 1 d . . . H44 H 0.7980 -0.0652 0.7486 0.056 Uiso 1 1 calc R . . C45 C 0.8435(8) -0.0534(6) 0.6470(5) 0.089(3) Uani 1 1 d . . . H45A H 0.8186 -0.0287 0.5984 0.134 Uiso 1 1 calc R . . H45B H 0.8329 -0.1294 0.6354 0.134 Uiso 1 1 calc R . . H45C H 0.9297 -0.0100 0.6726 0.134 Uiso 1 1 calc R . . C46 C 0.6385(6) -0.1101(6) 0.6705(5) 0.083(3) Uani 1 1 d . . . H46A H 0.5943 -0.0989 0.7088 0.125 Uiso 1 1 calc R . . H46B H 0.6304 -0.1858 0.6621 0.125 Uiso 1 1 calc R . . H46C H 0.6042 -0.0919 0.6210 0.125 Uiso 1 1 calc R . . C111 C 0.8708(8) 0.7129(6) 0.7488(5) 0.065(2) Uani 1 1 d . . . H111 H 0.8397 0.7216 0.7928 0.078 Uiso 1 1 calc R . . C222 C 0.9929(7) 0.7461(6) 0.7578(5) 0.064(2) Uani 1 1 d . . . H222 H 1.0483 0.7778 0.8078 0.076 Uiso 1 1 calc R . . C333 C 1.0353(7) 0.7333(6) 0.6936(5) 0.069(3) Uani 1 1 d . . . H333 H 1.1209 0.7553 0.6993 0.082 Uiso 1 1 calc R . . C444 C 0.9574(8) 0.6900(6) 0.6225(5) 0.072(3) Uani 1 1 d . . . H444 H 0.9888 0.6849 0.5782 0.086 Uiso 1 1 calc R . . C555 C 0.8328(8) 0.6529(6) 0.6131(5) 0.063(3) Uani 1 1 d . . . H555 H 0.7773 0.6186 0.5636 0.076 Uiso 1 1 calc R . . C666 C 0.7920(7) 0.6672(6) 0.6771(5) 0.064(2) Uani 1 1 d . . . H666 H 0.7064 0.6446 0.6718 0.077 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 0.0202(6) 0.0284(7) 0.0240(6) 0.0072(5) 0.0050(5) 0.0109(5) Cl1 0.0474(13) 0.0396(13) 0.136(2) 0.0041(12) 0.0378(12) 0.0218(10) Cl2 0.1081(18) 0.0856(17) 0.0342(11) 0.0348(11) 0.0252(11) 0.0535(14) O1 0.016(2) 0.032(3) 0.030(2) 0.005(2) 0.0025(18) 0.015(2) O2 0.018(2) 0.020(2) 0.024(2) 0.0061(18) 0.0033(18) 0.0032(18) O3 0.018(2) 0.037(3) 0.034(3) 0.008(2) -0.0026(19) 0.010(2) O4 0.025(2) 0.040(3) 0.033(3) 0.011(2) 0.0072(19) 0.014(2) N1 0.020(3) 0.031(3) 0.021(3) 0.014(2) 0.008(2) 0.015(2) N2 0.020(3) 0.034(3) 0.021(3) 0.003(2) 0.010(2) 0.012(2) C1 0.017(4) 0.032(4) 0.016(3) 0.005(3) 0.001(3) 0.008(3) C2 0.020(4) 0.031(4) 0.019(3) 0.014(3) 0.005(3) 0.010(3) C3 0.013(3) 0.036(4) 0.023(3) 0.012(3) 0.006(3) 0.004(3) C4 0.016(4) 0.035(4) 0.022(4) 0.004(3) 0.001(3) 0.004(3) C5 0.035(4) 0.041(4) 0.012(3) 0.009(3) 0.007(3) 0.021(3) C6 0.018(3) 0.030(4) 0.011(3) 0.009(3) 0.001(3) 0.007(3) C7 0.016(4) 0.030(4) 0.043(4) 0.011(3) 0.010(3) 0.005(3) C8 0.031(4) 0.040(5) 0.052(5) 0.001(4) 0.011(3) 0.018(3) C9 0.039(4) 0.030(4) 0.052(4) 0.002(4) 0.019(3) 0.021(3) C10 0.029(4) 0.038(5) 0.056(5) 0.008(4) 0.018(3) 0.011(3) C11 0.028(4) 0.039(5) 0.048(4) -0.003(4) 0.011(3) -0.001(3) C12 0.033(4) 0.026(4) 0.020(3) 0.002(3) 0.011(3) 0.012(3) C13 0.029(4) 0.041(4) 0.026(4) 0.012(3) 0.013(3) 0.018(3) C14 0.015(3) 0.038(4) 0.027(4) 0.009(3) 0.014(3) 0.008(3) C15 0.039(4) 0.048(5) 0.031(4) 0.010(4) 0.014(3) 0.027(4) C16 0.027(4) 0.059(5) 0.040(4) -0.010(4) 0.008(3) 0.019(4) C17 0.030(4) 0.051(5) 0.059(5) 0.015(4) 0.024(4) 0.023(4) C18 0.032(4) 0.066(5) 0.041(5) 0.025(4) 0.015(3) 0.034(4) C19 0.024(4) 0.055(5) 0.027(4) 0.013(3) 0.011(3) 0.026(4) C20 0.027(4) 0.036(4) 0.039(4) 0.015(3) 0.023(3) 0.018(3) C21 0.024(4) 0.042(4) 0.019(3) 0.018(3) 0.017(3) 0.019(3) C22 0.029(4) 0.033(4) 0.022(4) 0.003(3) 0.009(3) 0.017(3) C23 0.024(4) 0.029(4) 0.019(3) 0.005(3) 0.011(3) 0.013(3) C24 0.037(4) 0.039(5) 0.030(4) 0.004(3) 0.018(3) 0.013(3) C25 0.052(5) 0.040(5) 0.038(4) 0.011(4) 0.023(4) 0.019(4) C26 0.057(5) 0.052(5) 0.024(4) 0.015(4) 0.021(3) 0.032(4) C27 0.035(4) 0.065(6) 0.020(4) -0.003(4) 0.004(3) 0.027(4) C28 0.031(4) 0.035(4) 0.028(4) 0.010(3) 0.014(3) 0.013(3) C29 0.029(4) 0.046(4) 0.018(3) 0.006(3) 0.010(3) 0.021(3) C30 0.020(4) 0.025(4) 0.025(4) 0.003(3) 0.005(3) 0.009(3) C31 0.033(4) 0.030(4) 0.020(3) 0.005(3) 0.004(3) 0.018(3) C32 0.023(4) 0.036(4) 0.025(4) 0.003(3) 0.006(3) 0.012(3) C33 0.020(4) 0.018(4) 0.031(4) -0.001(3) 0.014(3) 0.006(3) C34 0.021(4) 0.022(4) 0.026(4) 0.003(3) 0.005(3) 0.011(3) C35 0.018(4) 0.014(4) 0.029(4) -0.005(3) 0.001(3) 0.005(3) C36 0.022(4) 0.029(4) 0.021(3) 0.002(3) 0.011(3) 0.003(3) C37 0.036(4) 0.048(5) 0.039(4) 0.028(3) 0.020(3) 0.016(4) C38 0.046(4) 0.044(5) 0.042(4) 0.024(3) 0.023(3) 0.023(4) C39 0.043(4) 0.054(5) 0.025(4) 0.017(3) 0.019(3) 0.022(4) C40 0.031(4) 0.057(5) 0.032(4) -0.001(4) 0.007(3) 0.019(4) C41 0.034(4) 0.035(4) 0.033(4) 0.007(3) 0.006(3) 0.010(3) C42 0.052(5) 0.059(5) 0.039(4) 0.024(4) 0.012(3) 0.030(4) C43 0.083(6) 0.081(6) 0.035(5) 0.016(4) 0.009(4) 0.049(5) C48 0.097(9) 0.167(13) 0.073(8) -0.014(8) -0.019(6) 0.107(10) C47 0.084(8) 0.165(12) 0.085(8) -0.018(7) -0.021(6) 0.089(8) C49 0.081(8) 0.102(10) 0.098(9) -0.042(8) -0.049(7) 0.071(8) C44 0.045(5) 0.035(5) 0.059(5) -0.003(4) 0.016(4) 0.015(4) C45 0.108(7) 0.048(6) 0.117(8) -0.009(5) 0.071(6) 0.015(5) C46 0.051(6) 0.043(6) 0.144(8) -0.014(5) 0.035(5) 0.004(4) C111 0.060(6) 0.058(6) 0.081(7) 0.030(5) 0.035(5) 0.013(5) C222 0.036(5) 0.076(7) 0.059(6) 0.004(5) 0.013(4) -0.002(4) C333 0.047(5) 0.075(7) 0.068(6) -0.019(5) 0.017(5) 0.010(4) C444 0.076(7) 0.070(7) 0.064(6) -0.017(5) 0.020(5) 0.026(5) C555 0.070(7) 0.041(5) 0.063(6) -0.012(4) -0.012(5) 0.025(5) C666 0.053(6) 0.061(6) 0.078(7) 0.013(5) 0.007(5) 0.026(5) _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 O4 1.796(4) . ? Ti1 O3 1.811(4) . ? Ti1 O2 1.884(4) . ? Ti1 O1 1.903(4) . ? Ti1 N1 2.372(5) . ? Ti1 N2 2.395(5) . ? Cl1 C17 1.739(7) . ? Cl2 C26 1.728(7) . ? O1 C1 1.331(6) . ? O2 C35 1.330(6) . ? O3 C41 1.418(6) . ? O4 C44 1.407(7) . ? N1 C20 1.476(7) . ? N1 C12 1.489(6) . ? N1 C13 1.506(6) . ? N2 C21 1.475(6) . ? N2 C29 1.490(6) . ? N2 C22 1.501(6) . ? C1 C6 1.409(7) . ? C1 C2 1.411(7) . ? C2 C3 1.380(7) . ? C2 C7 1.543(7) . ? C3 C4 1.393(7) . ? C3 H3 0.9500 . ? C4 C5 1.366(7) . ? C4 C11 1.515(7) . ? C5 C6 1.396(7) . ? C5 H5 0.9500 . ? C6 C12 1.502(7) . ? C7 C10 1.503(7) . ? C7 C9 1.527(8) . ? C7 C8 1.550(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.503(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.382(8) . ? C14 C15 1.397(7) . ? C15 C16 1.386(8) . ? C15 H15 0.9500 . ? C16 C17 1.370(9) . ? C16 H16 0.9500 . ? C17 C18 1.364(8) . ? C18 C19 1.384(8) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.524(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.499(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.384(8) . ? C23 C28 1.385(7) . ? C24 C25 1.385(8) . ? C24 H24 0.9500 . ? C25 C26 1.377(8) . ? C25 H25 0.9500 . ? C26 C27 1.371(9) . ? C27 C28 1.384(8) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.520(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.381(7) . ? C30 C35 1.402(8) . ? C31 C32 1.389(8) . ? C31 H31 0.9500 . ? C32 C33 1.374(7) . ? C32 C40 1.505(7) . ? C33 C34 1.394(7) . ? C33 H33 0.9500 . ? C34 C35 1.417(8) . ? C34 C36 1.551(8) . ? C36 C37 1.531(8) . ? C36 C39 1.534(7) . ? C36 C38 1.534(8) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? 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 C43 1.509(8) . ? C41 C42 1.520(8) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C48 C47 1.354(12) . ? C48 C49 1.382(15) . ? C48 H48 0.9500 . ? C47 C49 1.369(13) 2_666 ? C47 H47 0.9500 . ? C49 C47 1.369(13) 2_666 ? C49 H49 0.9500 . ? C44 C46 1.451(8) . ? C44 C45 1.480(9) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C111 C222 1.351(9) . ? C111 C666 1.361(9) . ? C111 H111 0.9500 . ? C222 C333 1.367(9) . ? C222 H222 0.9500 . ? C333 C444 1.346(9) . ? C333 H333 0.9500 . ? C444 C555 1.377(10) . ? C444 H444 0.9500 . ? C555 C666 1.356(10) . ? C555 H555 0.9500 . ? C666 H666 0.9500 . ? 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 O4 Ti1 O3 106.09(18) . . ? O4 Ti1 O2 97.30(16) . . ? O3 Ti1 O2 92.86(17) . . ? O4 Ti1 O1 93.79(17) . . ? O3 Ti1 O1 93.72(17) . . ? O2 Ti1 O1 165.01(16) . . ? O4 Ti1 N1 160.92(18) . . ? O3 Ti1 N1 92.29(16) . . ? O2 Ti1 N1 86.62(15) . . ? O1 Ti1 N1 79.68(16) . . ? O4 Ti1 N2 86.79(17) . . ? O3 Ti1 N2 166.17(16) . . ? O2 Ti1 N2 80.26(16) . . ? O1 Ti1 N2 90.35(17) . . ? N1 Ti1 N2 75.43(15) . . ? C1 O1 Ti1 143.3(3) . . ? C35 O2 Ti1 143.3(4) . . ? C41 O3 Ti1 136.1(4) . . ? C44 O4 Ti1 157.7(4) . . ? C20 N1 C12 110.3(4) . . ? C20 N1 C13 110.6(4) . . ? C12 N1 C13 106.5(4) . . ? C20 N1 Ti1 106.8(3) . . ? C12 N1 Ti1 109.2(3) . . ? C13 N1 Ti1 113.5(3) . . ? C21 N2 C29 110.2(4) . . ? C21 N2 C22 111.7(5) . . ? C29 N2 C22 107.6(4) . . ? C21 N2 Ti1 108.9(3) . . ? C29 N2 Ti1 111.7(4) . . ? C22 N2 Ti1 106.8(3) . . ? O1 C1 C6 118.9(5) . . ? O1 C1 C2 122.2(5) . . ? C6 C1 C2 118.9(5) . . ? C3 C2 C1 117.8(5) . . ? C3 C2 C7 121.3(5) . . ? C1 C2 C7 120.8(5) . . ? C2 C3 C4 124.6(5) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? C5 C4 C3 116.0(5) . . ? C5 C4 C11 122.1(5) . . ? C3 C4 C11 121.9(5) . . ? C4 C5 C6 122.9(5) . . ? C4 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C5 C6 C1 119.4(5) . . ? C5 C6 C12 117.8(5) . . ? C1 C6 C12 122.7(5) . . ? C10 C7 C9 107.8(5) . . ? C10 C7 C2 112.9(5) . . ? C9 C7 C2 109.6(5) . . ? C10 C7 C8 107.8(5) . . ? C9 C7 C8 107.2(5) . . ? C2 C7 C8 111.3(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C11 H11A 109.5 . . ? C4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C6 116.5(4) . . ? N1 C12 H12A 108.2 . . ? C6 C12 H12A 108.2 . . ? N1 C12 H12B 108.2 . . ? C6 C12 H12B 108.2 . . ? H12A C12 H12B 107.3 . . ? C14 C13 N1 118.1(5) . . ? C14 C13 H13A 107.8 . . ? N1 C13 H13A 107.8 . . ? C14 C13 H13B 107.8 . . ? N1 C13 H13B 107.8 . . ? H13A C13 H13B 107.1 . . ? C19 C14 C15 117.9(6) . . ? C19 C14 C13 121.8(5) . . ? C15 C14 C13 120.3(6) . . ? C16 C15 C14 121.2(6) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C17 C16 C15 119.4(6) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C18 C17 C16 120.2(6) . . ? C18 C17 Cl1 121.1(6) . . ? C16 C17 Cl1 118.6(5) . . ? C17 C18 C19 120.8(6) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C14 C19 C18 120.5(6) . . ? C14 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? N1 C20 C21 110.5(5) . . ? N1 C20 H20A 109.6 . . ? C21 C20 H20A 109.6 . . ? N1 C20 H20B 109.6 . . ? C21 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? N2 C21 C20 110.4(4) . . ? N2 C21 H21A 109.6 . . ? C20 C21 H21A 109.6 . . ? N2 C21 H21B 109.6 . . ? C20 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 N2 117.9(4) . . ? C23 C22 H22A 107.8 . . ? N2 C22 H22A 107.8 . . ? C23 C22 H22B 107.8 . . ? N2 C22 H22B 107.8 . . ? H22A C22 H22B 107.2 . . ? C24 C23 C28 117.8(6) . . ? C24 C23 C22 119.3(5) . . ? C28 C23 C22 122.8(6) . . ? C23 C24 C25 120.8(6) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 120.2(7) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 120.1(7) . . ? C27 C26 Cl2 119.5(5) . . ? C25 C26 Cl2 120.4(6) . . ? C26 C27 C28 119.3(6) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? C27 C28 C23 121.8(6) . . ? C27 C28 H28 119.1 . . ? C23 C28 H28 119.1 . . ? N2 C29 C30 117.3(4) . . ? N2 C29 H29A 108.0 . . ? C30 C29 H29A 108.0 . . ? N2 C29 H29B 108.0 . . ? C30 C29 H29B 108.0 . . ? H29A C29 H29B 107.2 . . ? C31 C30 C35 120.6(6) . . ? C31 C30 C29 117.5(5) . . ? C35 C30 C29 121.5(5) . . ? C30 C31 C32 122.2(6) . . ? C30 C31 H31 118.9 . . ? C32 C31 H31 118.9 . . ? C33 C32 C31 115.6(5) . . ? C33 C32 C40 122.8(6) . . ? C31 C32 C40 121.5(6) . . ? C32 C33 C34 125.9(6) . . ? C32 C33 H33 117.1 . . ? C34 C33 H33 117.1 . . ? C33 C34 C35 116.5(5) . . ? C33 C34 C36 123.0(5) . . ? C35 C34 C36 120.5(5) . . ? O2 C35 C30 121.6(5) . . ? O2 C35 C34 119.4(5) . . ? C30 C35 C34 119.0(5) . . ? C37 C36 C39 107.8(5) . . ? C37 C36 C38 106.9(5) . . ? C39 C36 C38 108.5(5) . . ? C37 C36 C34 111.6(4) . . ? C39 C36 C34 111.8(5) . . ? C38 C36 C34 110.0(5) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C32 C40 H40A 109.5 . . ? C32 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C32 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O3 C41 C43 110.2(5) . . ? O3 C41 C42 110.5(4) . . ? C43 C41 C42 111.4(6) . . ? O3 C41 H41 108.2 . . ? C43 C41 H41 108.2 . . ? C42 C41 H41 108.2 . . ? 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 . . ? C47 C48 C49 118.8(11) . . ? C47 C48 H48 120.6 . . ? C49 C48 H48 120.6 . . ? C48 C47 C49 121.9(12) . 2_666 ? C48 C47 H47 119.0 . . ? C49 C47 H47 119.0 2_666 . ? C47 C49 C48 119.2(10) 2_666 . ? C47 C49 H49 120.4 2_666 . ? C48 C49 H49 120.4 . . ? O4 C44 C46 113.7(5) . . ? O4 C44 C45 110.0(6) . . ? C46 C44 C45 114.2(6) . . ? O4 C44 H44 106.1 . . ? C46 C44 H44 106.1 . . ? C45 C44 H44 106.1 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C222 C111 C666 120.3(8) . . ? C222 C111 H111 119.8 . . ? C666 C111 H111 119.8 . . ? C111 C222 C333 118.7(7) . . ? C111 C222 H222 120.7 . . ? C333 C222 H222 120.7 . . ? C444 C333 C222 120.9(8) . . ? C444 C333 H333 119.5 . . ? C222 C333 H333 119.5 . . ? C333 C444 C555 120.7(8) . . ? C333 C444 H444 119.6 . . ? C555 C444 H444 119.6 . . ? C666 C555 C444 117.7(7) . . ? C666 C555 H555 121.2 . . ? C444 C555 H555 121.2 . . ? C555 C666 C111 121.6(8) . . ? C555 C666 H666 119.2 . . ? C111 C666 H666 119.2 . . ? 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 O4 Ti1 O1 C1 -167.0(6) . . . . ? O3 Ti1 O1 C1 -60.6(6) . . . . ? O2 Ti1 O1 C1 55.2(10) . . . . ? N1 Ti1 O1 C1 31.0(6) . . . . ? N2 Ti1 O1 C1 106.1(6) . . . . ? O4 Ti1 O2 C35 -57.4(6) . . . . ? O3 Ti1 O2 C35 -164.0(6) . . . . ? O1 Ti1 O2 C35 80.0(8) . . . . ? N1 Ti1 O2 C35 103.8(6) . . . . ? N2 Ti1 O2 C35 28.0(6) . . . . ? O4 Ti1 O3 C41 65.4(5) . . . . ? O2 Ti1 O3 C41 163.9(5) . . . . ? O1 Ti1 O3 C41 -29.6(5) . . . . ? N1 Ti1 O3 C41 -109.4(5) . . . . ? N2 Ti1 O3 C41 -136.5(7) . . . . ? O3 Ti1 O4 C44 36.5(10) . . . . ? O2 Ti1 O4 C44 -58.6(10) . . . . ? O1 Ti1 O4 C44 131.5(10) . . . . ? N1 Ti1 O4 C44 -159.5(9) . . . . ? N2 Ti1 O4 C44 -138.4(10) . . . . ? O4 Ti1 N1 C20 1.0(7) . . . . ? O3 Ti1 N1 C20 165.7(3) . . . . ? O2 Ti1 N1 C20 -101.6(3) . . . . ? O1 Ti1 N1 C20 72.3(3) . . . . ? N2 Ti1 N1 C20 -20.8(3) . . . . ? O4 Ti1 N1 C12 -118.2(5) . . . . ? O3 Ti1 N1 C12 46.4(4) . . . . ? O2 Ti1 N1 C12 139.1(4) . . . . ? O1 Ti1 N1 C12 -47.0(3) . . . . ? N2 Ti1 N1 C12 -140.0(4) . . . . ? O4 Ti1 N1 C13 123.2(5) . . . . ? O3 Ti1 N1 C13 -72.2(4) . . . . ? O2 Ti1 N1 C13 20.6(3) . . . . ? O1 Ti1 N1 C13 -165.5(4) . . . . ? N2 Ti1 N1 C13 101.4(4) . . . . ? O4 Ti1 N2 C21 177.5(4) . . . . ? O3 Ti1 N2 C21 18.6(9) . . . . ? O2 Ti1 N2 C21 79.5(3) . . . . ? O1 Ti1 N2 C21 -88.7(3) . . . . ? N1 Ti1 N2 C21 -9.5(3) . . . . ? O4 Ti1 N2 C29 55.7(3) . . . . ? O3 Ti1 N2 C29 -103.3(7) . . . . ? O2 Ti1 N2 C29 -42.3(3) . . . . ? O1 Ti1 N2 C29 149.5(3) . . . . ? N1 Ti1 N2 C29 -131.3(3) . . . . ? O4 Ti1 N2 C22 -61.7(3) . . . . ? O3 Ti1 N2 C22 139.3(7) . . . . ? O2 Ti1 N2 C22 -159.7(3) . . . . ? O1 Ti1 N2 C22 32.0(3) . . . . ? N1 Ti1 N2 C22 111.3(3) . . . . ? Ti1 O1 C1 C6 -15.2(9) . . . . ? Ti1 O1 C1 C2 164.5(4) . . . . ? O1 C1 C2 C3 178.7(5) . . . . ? C6 C1 C2 C3 -1.6(8) . . . . ? O1 C1 C2 C7 -2.7(8) . . . . ? C6 C1 C2 C7 177.1(5) . . . . ? C1 C2 C3 C4 -2.8(8) . . . . ? C7 C2 C3 C4 178.5(6) . . . . ? C2 C3 C4 C5 3.2(9) . . . . ? C2 C3 C4 C11 -177.5(6) . . . . ? C3 C4 C5 C6 0.9(8) . . . . ? C11 C4 C5 C6 -178.4(5) . . . . ? C4 C5 C6 C1 -5.1(8) . . . . ? C4 C5 C6 C12 171.4(5) . . . . ? O1 C1 C6 C5 -174.9(5) . . . . ? C2 C1 C6 C5 5.4(8) . . . . ? O1 C1 C6 C12 8.8(8) . . . . ? C2 C1 C6 C12 -171.0(5) . . . . ? C3 C2 C7 C10 0.7(8) . . . . ? C1 C2 C7 C10 -177.9(5) . . . . ? C3 C2 C7 C9 120.9(6) . . . . ? C1 C2 C7 C9 -57.7(7) . . . . ? C3 C2 C7 C8 -120.7(6) . . . . ? C1 C2 C7 C8 60.7(7) . . . . ? C20 N1 C12 C6 -55.2(6) . . . . ? C13 N1 C12 C6 -175.3(5) . . . . ? Ti1 N1 C12 C6 61.9(6) . . . . ? C5 C6 C12 N1 142.3(5) . . . . ? C1 C6 C12 N1 -41.3(8) . . . . ? C20 N1 C13 C14 -56.9(6) . . . . ? C12 N1 C13 C14 62.9(6) . . . . ? Ti1 N1 C13 C14 -176.9(4) . . . . ? N1 C13 C14 C19 86.5(7) . . . . ? N1 C13 C14 C15 -93.2(7) . . . . ? C19 C14 C15 C16 -1.1(9) . . . . ? C13 C14 C15 C16 178.6(6) . . . . ? C14 C15 C16 C17 -0.3(10) . . . . ? C15 C16 C17 C18 1.3(10) . . . . ? C15 C16 C17 Cl1 -176.9(5) . . . . ? C16 C17 C18 C19 -0.9(10) . . . . ? Cl1 C17 C18 C19 177.3(5) . . . . ? C15 C14 C19 C18 1.5(9) . . . . ? C13 C14 C19 C18 -178.2(6) . . . . ? C17 C18 C19 C14 -0.6(10) . . . . ? C12 N1 C20 C21 167.5(4) . . . . ? C13 N1 C20 C21 -74.9(5) . . . . ? Ti1 N1 C20 C21 49.0(5) . . . . ? C29 N2 C21 C20 161.0(4) . . . . ? C22 N2 C21 C20 -79.4(5) . . . . ? Ti1 N2 C21 C20 38.3(5) . . . . ? N1 C20 C21 N2 -61.2(6) . . . . ? C21 N2 C22 C23 -58.0(6) . . . . ? C29 N2 C22 C23 63.1(6) . . . . ? Ti1 N2 C22 C23 -176.9(4) . . . . ? N2 C22 C23 C24 96.6(6) . . . . ? N2 C22 C23 C28 -86.3(7) . . . . ? C28 C23 C24 C25 1.5(8) . . . . ? C22 C23 C24 C25 178.7(5) . . . . ? C23 C24 C25 C26 -0.7(9) . . . . ? C24 C25 C26 C27 0.2(9) . . . . ? C24 C25 C26 Cl2 -179.4(4) . . . . ? C25 C26 C27 C28 -0.5(9) . . . . ? Cl2 C26 C27 C28 179.1(4) . . . . ? C26 C27 C28 C23 1.3(9) . . . . ? C24 C23 C28 C27 -1.7(8) . . . . ? C22 C23 C28 C27 -178.9(5) . . . . ? C21 N2 C29 C30 -64.6(7) . . . . ? C22 N2 C29 C30 173.4(5) . . . . ? Ti1 N2 C29 C30 56.5(6) . . . . ? N2 C29 C30 C31 147.0(5) . . . . ? N2 C29 C30 C35 -39.6(8) . . . . ? C35 C30 C31 C32 -4.3(8) . . . . ? C29 C30 C31 C32 169.2(5) . . . . ? C30 C31 C32 C33 0.1(8) . . . . ? C30 C31 C32 C40 -176.8(5) . . . . ? C31 C32 C33 C34 3.0(8) . . . . ? C40 C32 C33 C34 179.9(5) . . . . ? C32 C33 C34 C35 -1.8(8) . . . . ? C32 C33 C34 C36 -179.0(5) . . . . ? Ti1 O2 C35 C30 -16.1(9) . . . . ? Ti1 O2 C35 C34 162.8(4) . . . . ? C31 C30 C35 O2 -175.6(5) . . . . ? C29 C30 C35 O2 11.2(8) . . . . ? C31 C30 C35 C34 5.5(8) . . . . ? C29 C30 C35 C34 -167.7(5) . . . . ? C33 C34 C35 O2 178.6(4) . . . . ? C36 C34 C35 O2 -4.1(8) . . . . ? C33 C34 C35 C30 -2.5(8) . . . . ? C36 C34 C35 C30 174.8(5) . . . . ? C33 C34 C36 C37 -0.3(7) . . . . ? C35 C34 C36 C37 -177.4(5) . . . . ? C33 C34 C36 C39 -121.2(5) . . . . ? C35 C34 C36 C39 61.7(7) . . . . ? C33 C34 C36 C38 118.2(6) . . . . ? C35 C34 C36 C38 -59.0(7) . . . . ? Ti1 O3 C41 C43 161.8(4) . . . . ? Ti1 O3 C41 C42 -74.6(7) . . . . ? C49 C48 C47 C49 -0.6(16) . . . 2_666 ? C47 C48 C49 C47 0.6(16) . . . 2_666 ? Ti1 O4 C44 C46 72.9(12) . . . . ? Ti1 O4 C44 C45 -157.6(8) . . . . ? C666 C111 C222 C333 0.4(13) . . . . ? C111 C222 C333 C444 1.0(13) . . . . ? C222 C333 C444 C555 -3.0(13) . . . . ? C333 C444 C555 C666 3.6(13) . . . . ? C444 C555 C666 C111 -2.3(12) . . . . ? C222 C111 C666 C555 0.3(13) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.694 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.071 #===END data_pg241a _database_code_depnum_ccdc_archive 'CCDC 715915' #TrackingRef '- Combined_5aug,10.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H38 Cl6 N2 O4 Ti' _chemical_formula_sum 'C36 H38 Cl6 N2 O4 Ti' _chemical_formula_weight 823.28 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' Cl Cl 0.1484 0.1585 '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 Trigonal _symmetry_space_group_name_H-M 'R -3C' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 25.591(4) _cell_length_b 25.591(4) _cell_length_c 29.747(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 16871(5) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3374 _cell_measurement_theta_min 3.1294 _cell_measurement_theta_max 32.5192 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7632 _exptl_absorpt_coefficient_mu 0.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8561 _exptl_absorpt_correction_T_max 0.9087 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36190 _diffrn_reflns_av_R_equivalents 0.2525 _diffrn_reflns_av_sigmaI/netI 0.1038 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.18 _reflns_number_total 3371 _reflns_number_gt 1710 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep3 _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.1064P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3371 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1305 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2108 _refine_ls_wR_factor_gt 0.1939 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.75580(5) 0.08914(5) 0.4167 0.0693(5) Uani 1 2 d S . . Cl1 Cl 0.72996(6) 0.08747(6) 0.26176(6) 0.0780(5) Uani 1 1 d . . . Cl2 Cl 0.72531(6) 0.29495(6) 0.25727(6) 0.0764(5) Uani 1 1 d . . . Cl3 Cl 0.84201(13) 0.44280(10) 0.54952(8) 0.1428(10) Uani 1 1 d . . . O1 O 0.75315(15) 0.11396(14) 0.35659(13) 0.0682(10) Uani 1 1 d . . . O2 O 0.68480(14) 0.07797(17) 0.43382(16) 0.0890(13) Uani 1 1 d . . . N1 N 0.79599(16) 0.19304(16) 0.42959(16) 0.0601(12) Uani 1 1 d . . . C1 C 0.7469(2) 0.1555(2) 0.3350(2) 0.0617(14) Uani 1 1 d . . . C2 C 0.7352(2) 0.1500(2) 0.2889(2) 0.0607(14) Uani 1 1 d . . . C3 C 0.7280(2) 0.1909(2) 0.2652(2) 0.0617(14) Uani 1 1 d . . . H3 H 0.7192 0.1853 0.2340 0.074 Uiso 1 1 calc R . . C4 C 0.73376(19) 0.2415(2) 0.2872(2) 0.0599(14) Uani 1 1 d . . . C5 C 0.74578(19) 0.2491(2) 0.3319(2) 0.0606(14) Uani 1 1 d . . . H5 H 0.7502 0.2841 0.3465 0.073 Uiso 1 1 calc R . . C6 C 0.75175(19) 0.2061(2) 0.3568(2) 0.0578(13) Uani 1 1 d . . . C7 C 0.7582(2) 0.2138(2) 0.4072(2) 0.0656(15) Uani 1 1 d . . . H7A H 0.7751 0.2571 0.4141 0.079 Uiso 1 1 calc R . . H7B H 0.7173 0.1918 0.4206 0.079 Uiso 1 1 calc R . . C8 C 0.7946(2) 0.2025(2) 0.4793(2) 0.0713(15) Uani 1 1 d . . . H8A H 0.8246 0.1943 0.4937 0.086 Uiso 1 1 calc R . . H8B H 0.7543 0.1720 0.4906 0.086 Uiso 1 1 calc R . . C9 C 0.8069(3) 0.2642(2) 0.4949(2) 0.0674(15) Uani 1 1 d . . . C10 C 0.7619(3) 0.2765(3) 0.5018(2) 0.0844(18) Uani 1 1 d . . . H10 H 0.7218 0.2467 0.4942 0.101 Uiso 1 1 calc R . . C11 C 0.7718(4) 0.3311(4) 0.5196(3) 0.108(2) Uani 1 1 d . . . H11 H 0.7392 0.3379 0.5250 0.129 Uiso 1 1 calc R . . C12 C 0.8284(4) 0.3735(3) 0.5288(3) 0.094(2) Uani 1 1 d . . . C13 C 0.8754(3) 0.3647(3) 0.5223(2) 0.091(2) Uani 1 1 d . . . H13 H 0.9153 0.3957 0.5291 0.109 Uiso 1 1 calc R . . C14 C 0.8648(3) 0.3092(2) 0.5054(2) 0.0787(18) Uani 1 1 d . . . H14 H 0.8977 0.3024 0.5010 0.094 Uiso 1 1 calc R . . C15 C 0.8588(2) 0.2246(2) 0.4116(2) 0.0631(14) Uani 1 1 d . . . H15A H 0.8574 0.2288 0.3786 0.076 Uiso 1 1 calc R . . H15B H 0.8811 0.2656 0.4246 0.076 Uiso 1 1 calc R . . C16 C 0.6234(3) 0.0533(5) 0.4353(4) 0.164(5) Uani 1 1 d . . . H16 H 0.6178 0.0119 0.4391 0.197 Uiso 1 1 calc R . . C17 C 0.5966(4) 0.0382(4) 0.3917(4) 0.185(6) Uani 1 1 d . . . H17A H 0.5526 0.0150 0.3947 0.278 Uiso 1 1 calc R . . H17B H 0.6106 0.0140 0.3758 0.278 Uiso 1 1 calc R . . H17C H 0.6083 0.0753 0.3748 0.278 Uiso 1 1 calc R . . C18 C 0.5984(4) 0.0494(5) 0.4737(5) 0.217(7) Uani 1 1 d . . . H18A H 0.6143 0.0327 0.4960 0.325 Uiso 1 1 calc R . . H18B H 0.5547 0.0230 0.4710 0.325 Uiso 1 1 calc R . . H18C H 0.6073 0.0897 0.4833 0.325 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 0.0575(6) 0.0575(6) 0.0762(12) 0.0037(4) -0.0037(4) 0.0164(6) Cl1 0.0842(9) 0.0771(9) 0.0733(12) -0.0141(8) -0.0085(8) 0.0408(7) Cl2 0.0716(8) 0.0690(8) 0.0808(12) 0.0054(8) -0.0085(8) 0.0294(6) Cl3 0.259(3) 0.1385(16) 0.0899(17) -0.0141(13) -0.0049(17) 0.1435(19) O1 0.075(2) 0.0566(19) 0.064(3) -0.0038(19) -0.0145(19) 0.0269(17) O2 0.049(2) 0.093(2) 0.098(4) 0.009(2) -0.004(2) 0.0142(18) N1 0.052(2) 0.055(2) 0.066(4) 0.000(2) -0.004(2) 0.0213(18) C1 0.046(3) 0.058(3) 0.070(5) -0.001(3) 0.002(3) 0.018(2) C2 0.049(3) 0.058(3) 0.066(4) -0.010(3) 0.001(3) 0.020(2) C3 0.054(3) 0.066(3) 0.055(4) 0.004(3) -0.001(3) 0.022(2) C4 0.047(3) 0.062(3) 0.061(4) 0.003(3) 0.002(3) 0.020(2) C5 0.049(3) 0.061(3) 0.067(5) 0.003(3) 0.007(3) 0.024(2) C6 0.047(2) 0.059(3) 0.058(4) -0.003(3) 0.000(2) 0.019(2) C7 0.058(3) 0.069(3) 0.074(5) -0.006(3) -0.007(3) 0.034(2) C8 0.068(3) 0.078(3) 0.064(5) 0.000(3) -0.002(3) 0.034(3) C9 0.079(4) 0.073(3) 0.054(4) 0.005(3) 0.004(3) 0.041(3) C10 0.087(4) 0.098(4) 0.075(5) 0.003(4) 0.008(4) 0.051(4) C11 0.142(6) 0.173(7) 0.067(5) 0.008(5) 0.015(5) 0.124(6) C12 0.137(6) 0.115(5) 0.066(5) -0.007(4) -0.013(5) 0.090(5) C13 0.123(5) 0.086(4) 0.071(5) -0.014(4) -0.027(4) 0.058(4) C14 0.101(4) 0.078(4) 0.074(5) -0.012(3) -0.020(4) 0.058(4) C15 0.056(3) 0.052(3) 0.066(4) 0.000(3) 0.001(3) 0.017(2) C16 0.060(4) 0.243(11) 0.139(9) 0.106(9) 0.001(5) 0.039(6) C17 0.162(7) 0.159(7) 0.294(15) -0.140(9) -0.154(9) 0.124(7) C18 0.137(8) 0.161(9) 0.258(17) -0.074(10) 0.083(10) 0.004(7) _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 O2 1.767(4) 12_545 ? Ti1 O2 1.768(4) . ? Ti1 O1 1.909(4) . ? Ti1 O1 1.909(4) 12_545 ? Ti1 N1 2.354(4) 12_545 ? Ti1 N1 2.354(4) . ? Cl1 C2 1.736(5) . ? Cl2 C4 1.734(5) . ? Cl3 C12 1.740(7) . ? O1 C1 1.319(6) . ? O2 C16 1.370(8) . ? N1 C7 1.475(6) . ? N1 C15 1.491(6) . ? N1 C8 1.501(7) . ? C1 C6 1.397(7) . ? C1 C2 1.398(8) . ? C2 C3 1.347(7) . ? C3 C4 1.389(7) . ? C3 H3 0.9500 . ? C4 C5 1.359(8) . ? C5 C6 1.395(7) . ? C5 H5 0.9500 . ? C6 C7 1.510(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.519(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.354(8) . ? C9 C14 1.382(7) . ? C10 C11 1.392(10) . ? C10 H10 0.9500 . ? C11 C12 1.333(10) . ? C11 H11 0.9500 . ? C12 C13 1.344(9) . ? C13 C14 1.399(7) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C15 1.472(9) 12_545 ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.288(13) . ? C16 C17 1.428(14) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 O2 Ti1 O2 107.0(3) 12_545 . ? O2 Ti1 O1 93.29(18) 12_545 . ? O2 Ti1 O1 96.86(18) . . ? O2 Ti1 O1 96.86(18) 12_545 12_545 ? O2 Ti1 O1 93.28(18) . 12_545 ? O1 Ti1 O1 162.9(2) . 12_545 ? O2 Ti1 N1 88.21(17) 12_545 12_545 ? O2 Ti1 N1 164.38(17) . 12_545 ? O1 Ti1 N1 85.53(16) . 12_545 ? O1 Ti1 N1 81.09(16) 12_545 12_545 ? O2 Ti1 N1 164.39(17) 12_545 . ? O2 Ti1 N1 88.20(17) . . ? O1 Ti1 N1 81.09(16) . . ? O1 Ti1 N1 85.53(16) 12_545 . ? N1 Ti1 N1 76.89(19) 12_545 . ? C1 O1 Ti1 139.7(4) . . ? C16 O2 Ti1 158.9(7) . . ? C7 N1 C15 111.5(4) . . ? C7 N1 C8 108.3(4) . . ? C15 N1 C8 111.9(4) . . ? C7 N1 Ti1 109.7(3) . . ? C15 N1 Ti1 107.3(3) . . ? C8 N1 Ti1 108.1(3) . . ? O1 C1 C6 122.2(6) . . ? O1 C1 C2 120.2(5) . . ? C6 C1 C2 117.7(5) . . ? C3 C2 C1 122.6(5) . . ? C3 C2 Cl1 119.8(5) . . ? C1 C2 Cl1 117.6(4) . . ? C2 C3 C4 119.1(5) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 120.3(5) . . ? C5 C4 Cl2 119.8(4) . . ? C3 C4 Cl2 119.8(5) . . ? C4 C5 C6 120.8(5) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 119.4(5) . . ? C5 C6 C7 118.1(5) . . ? C1 C6 C7 122.3(5) . . ? N1 C7 C6 116.8(4) . . ? N1 C7 H7A 108.1 . . ? C6 C7 H7A 108.1 . . ? N1 C7 H7B 108.1 . . ? C6 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? N1 C8 C9 117.3(5) . . ? N1 C8 H8A 108.0 . . ? C9 C8 H8A 108.0 . . ? N1 C8 H8B 108.0 . . ? C9 C8 H8B 108.0 . . ? H8A C8 H8B 107.2 . . ? C10 C9 C14 117.0(5) . . ? C10 C9 C8 122.0(5) . . ? C14 C9 C8 120.9(5) . . ? C9 C10 C11 122.7(6) . . ? C9 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C12 C11 C10 118.3(6) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? C11 C12 C13 122.1(7) . . ? C11 C12 Cl3 119.0(6) . . ? C13 C12 Cl3 118.8(6) . . ? C12 C13 C14 119.1(6) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C9 C14 C13 120.7(6) . . ? C9 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C15 C15 N1 112.3(4) 12_545 . ? C15 C15 H15A 109.1 12_545 . ? N1 C15 H15A 109.1 . . ? C15 C15 H15B 109.1 12_545 . ? N1 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? C18 C16 O2 118.4(10) . . ? C18 C16 C17 129.2(9) . . ? O2 C16 C17 112.3(9) . . ? C18 C16 H16 91.0 . . ? O2 C16 H16 91.0 . . ? C17 C16 H16 91.0 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? 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 O2 Ti1 O1 C1 164.6(5) 12_545 . . . ? O2 Ti1 O1 C1 57.1(5) . . . . ? O1 Ti1 O1 C1 -68.9(5) 12_545 . . . ? N1 Ti1 O1 C1 -107.4(5) 12_545 . . . ? N1 Ti1 O1 C1 -30.0(5) . . . . ? O2 Ti1 O2 C16 -30.5(13) 12_545 . . . ? O1 Ti1 O2 C16 65.1(13) . . . . ? O1 Ti1 O2 C16 -128.7(13) 12_545 . . . ? N1 Ti1 O2 C16 163.1(11) 12_545 . . . ? N1 Ti1 O2 C16 145.9(13) . . . . ? O2 Ti1 N1 C7 117.2(7) 12_545 . . . ? O2 Ti1 N1 C7 -49.8(4) . . . . ? O1 Ti1 N1 C7 47.4(3) . . . . ? O1 Ti1 N1 C7 -143.3(4) 12_545 . . . ? N1 Ti1 N1 C7 134.9(4) 12_545 . . . ? O2 Ti1 N1 C15 -4.0(9) 12_545 . . . ? O2 Ti1 N1 C15 -171.0(4) . . . . ? O1 Ti1 N1 C15 -73.8(3) . . . . ? O1 Ti1 N1 C15 95.5(3) 12_545 . . . ? N1 Ti1 N1 C15 13.6(2) 12_545 . . . ? O2 Ti1 N1 C8 -124.9(7) 12_545 . . . ? O2 Ti1 N1 C8 68.1(3) . . . . ? O1 Ti1 N1 C8 165.3(3) . . . . ? O1 Ti1 N1 C8 -25.3(3) 12_545 . . . ? N1 Ti1 N1 C8 -107.2(3) 12_545 . . . ? Ti1 O1 C1 C6 13.4(7) . . . . ? Ti1 O1 C1 C2 -166.7(4) . . . . ? O1 C1 C2 C3 179.5(4) . . . . ? C6 C1 C2 C3 -0.6(7) . . . . ? O1 C1 C2 Cl1 -0.5(6) . . . . ? C6 C1 C2 Cl1 179.4(3) . . . . ? C1 C2 C3 C4 1.5(7) . . . . ? Cl1 C2 C3 C4 -178.5(3) . . . . ? C2 C3 C4 C5 -0.7(7) . . . . ? C2 C3 C4 Cl2 179.5(4) . . . . ? C3 C4 C5 C6 -0.9(7) . . . . ? Cl2 C4 C5 C6 178.9(3) . . . . ? C4 C5 C6 C1 1.8(7) . . . . ? C4 C5 C6 C7 -173.3(4) . . . . ? O1 C1 C6 C5 178.9(4) . . . . ? C2 C1 C6 C5 -1.0(6) . . . . ? O1 C1 C6 C7 -6.3(7) . . . . ? C2 C1 C6 C7 173.9(4) . . . . ? C15 N1 C7 C6 58.5(5) . . . . ? C8 N1 C7 C6 -177.9(4) . . . . ? Ti1 N1 C7 C6 -60.1(5) . . . . ? C5 C6 C7 N1 -147.0(4) . . . . ? C1 C6 C7 N1 38.0(6) . . . . ? C7 N1 C8 C9 -49.6(5) . . . . ? C15 N1 C8 C9 73.7(5) . . . . ? Ti1 N1 C8 C9 -168.4(4) . . . . ? N1 C8 C9 C10 92.7(7) . . . . ? N1 C8 C9 C14 -91.4(7) . . . . ? C14 C9 C10 C11 -1.5(10) . . . . ? C8 C9 C10 C11 174.6(6) . . . . ? C9 C10 C11 C12 2.2(11) . . . . ? C10 C11 C12 C13 -1.4(12) . . . . ? C10 C11 C12 Cl3 178.2(5) . . . . ? C11 C12 C13 C14 -0.1(11) . . . . ? Cl3 C12 C13 C14 -179.6(5) . . . . ? C10 C9 C14 C13 0.0(9) . . . . ? C8 C9 C14 C13 -176.1(6) . . . . ? C12 C13 C14 C9 0.8(10) . . . . ? C7 N1 C15 C15 -161.2(5) . . . 12_545 ? C8 N1 C15 C15 77.4(6) . . . 12_545 ? Ti1 N1 C15 C15 -41.1(6) . . . 12_545 ? Ti1 O2 C16 C18 143.9(13) . . . . ? Ti1 O2 C16 C17 -39.4(18) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.599 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.078 #===END #===END data_pg250 _database_code_depnum_ccdc_archive 'CCDC 722297' #TrackingRef '- Combined_5aug,10.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C52 H70 Cl2 N2 O4 Ti, 1.17(C7 H8), 0.83(C6 H6) ; _chemical_formula_sum 'C65.17 H84.35 Cl2 N2 O4 Ti' _chemical_formula_weight 1078.56 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.794(5) _cell_length_b 20.558(3) _cell_length_c 15.600(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.09(3) _cell_angle_gamma 90.00 _cell_volume 6223(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2857 _cell_measurement_theta_min 2.9653 _cell_measurement_theta_max 32.6133 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2310 _exptl_absorpt_coefficient_mu 0.269 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9407 _exptl_absorpt_correction_T_max 0.9607 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30359 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.1619 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 32.64 _reflns_number_total 10357 _reflns_number_gt 4430 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep3 _computing_publication_material 'SHELXLTL (Sheldrick, 2008)' _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^)+(0.0629P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10357 _refine_ls_number_parameters 378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1501 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 0.840 _refine_ls_restrained_S_all 0.840 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.5000 0.18945(2) 0.7500 0.02030(11) Uani 1 2 d S . . Cl1 Cl 0.16740(3) 0.49191(3) 0.65146(5) 0.0611(2) Uani 1 1 d . . . O1 O 0.49527(5) 0.19843(6) 0.62684(8) 0.0228(3) Uani 1 1 d . . . O2 O 0.42395(5) 0.13781(6) 0.70985(8) 0.0264(3) Uani 1 1 d . . . N1 N 0.42627(6) 0.28312(7) 0.69306(10) 0.0213(3) Uani 1 1 d . . . C1 C 0.46082(8) 0.22460(8) 0.53852(12) 0.0224(4) Uani 1 1 d . . . C2 C 0.47938(8) 0.20984(9) 0.46459(13) 0.0266(4) Uani 1 1 d . . . C3 C 0.44235(9) 0.24140(10) 0.37628(14) 0.0342(5) Uani 1 1 d . . . H3A H 0.4547 0.2326 0.3263 0.041 Uiso 1 1 calc R . . C4 C 0.38860(9) 0.28485(10) 0.35681(13) 0.0315(5) Uani 1 1 d . . . C5 C 0.37103(8) 0.29652(9) 0.43012(13) 0.0260(4) Uani 1 1 d . . . H5A H 0.3347 0.3261 0.4191 0.031 Uiso 1 1 calc R . . C6 C 0.40488(8) 0.26628(8) 0.51974(12) 0.0223(4) Uani 1 1 d . . . C7 C 0.37527(8) 0.27364(9) 0.59002(12) 0.0250(4) Uani 1 1 d . . . H7A H 0.3271 0.2723 0.5698 0.030 Uiso 1 1 calc R . . C8 C 0.46808(8) 0.34193(8) 0.70190(13) 0.0252(4) Uani 1 1 d . . . H8A H 0.4404 0.3814 0.6962 0.030 Uiso 1 1 calc R . . H8B H 0.4816 0.3426 0.6493 0.030 Uiso 1 1 calc R . . C9 C 0.53473(8) 0.15840(9) 0.47867(13) 0.0286(4) Uani 1 1 d . . . C10 C 0.51162(10) 0.09243(10) 0.49963(17) 0.0426(6) Uani 1 1 d . . . H10A H 0.5449 0.0589 0.5041 0.064 Uiso 1 1 calc R . . H10B H 0.4661 0.0814 0.4475 0.064 Uiso 1 1 calc R . . H10C H 0.5090 0.0948 0.5607 0.064 Uiso 1 1 calc R . . C11 C 0.60445(9) 0.17540(11) 0.56301(17) 0.0481(7) Uani 1 1 d . . . H11A H 0.6389 0.1433 0.5671 0.072 Uiso 1 1 calc R . . H11B H 0.6004 0.1751 0.6230 0.072 Uiso 1 1 calc R . . H11C H 0.6187 0.2187 0.5529 0.072 Uiso 1 1 calc R . . C12 C 0.54478(11) 0.15086(13) 0.38869(16) 0.0585(7) Uani 1 1 d . . . H12A H 0.5785 0.1163 0.3990 0.088 Uiso 1 1 calc R . . H12B H 0.5616 0.1919 0.3753 0.088 Uiso 1 1 calc R . . H12C H 0.5007 0.1395 0.3339 0.088 Uiso 1 1 calc R . . C13 C 0.35224(10) 0.31746(11) 0.25706(14) 0.0421(6) Uani 1 1 d . . . C14 C 0.31971(14) 0.26376(15) 0.17965(17) 0.0830(10) Uani 1 1 d . . . H14A H 0.2929 0.2840 0.1165 0.125 Uiso 1 1 calc R . . H14B H 0.2894 0.2365 0.1954 0.125 Uiso 1 1 calc R . . H14C H 0.3563 0.2368 0.1781 0.125 Uiso 1 1 calc R . . C15 C 0.40264(12) 0.35821(19) 0.2396(2) 0.1125(13) Uani 1 1 d . . . H15A H 0.4223 0.3915 0.2899 0.169 Uiso 1 1 calc R . . H15B H 0.3789 0.3793 0.1766 0.169 Uiso 1 1 calc R . . H15C H 0.4396 0.3304 0.2410 0.169 Uiso 1 1 calc R . . C16 C 0.29303(10) 0.36050(11) 0.24816(15) 0.0448(6) Uani 1 1 d . . . H16A H 0.3104 0.3941 0.2981 0.067 Uiso 1 1 calc R . . H16B H 0.2585 0.3340 0.2560 0.067 Uiso 1 1 calc R . . H16C H 0.2719 0.3811 0.1846 0.067 Uiso 1 1 calc R . . C17 C 0.38765(8) 0.28730(9) 0.75173(13) 0.0262(4) Uani 1 1 d . . . H17A H 0.3971 0.2584 0.8038 0.031 Uiso 1 1 calc R . . C18 C 0.33299(8) 0.33959(9) 0.72409(12) 0.0240(4) Uani 1 1 d . . . C19 C 0.26415(8) 0.32395(9) 0.66951(13) 0.0276(5) Uani 1 1 d . . . H19A H 0.2519 0.2806 0.6470 0.033 Uiso 1 1 calc R . . C20 C 0.21251(9) 0.37026(10) 0.64691(14) 0.0336(5) Uani 1 1 d . . . H20A H 0.1654 0.3588 0.6101 0.040 Uiso 1 1 calc R . . C21 C 0.23093(9) 0.43288(10) 0.67882(14) 0.0350(5) Uani 1 1 d . . . C22 C 0.29862(9) 0.44993(10) 0.73329(15) 0.0399(6) Uani 1 1 d . . . H22A H 0.3105 0.4935 0.7549 0.048 Uiso 1 1 calc R . . C23 C 0.34947(9) 0.40333(9) 0.75655(14) 0.0340(5) Uani 1 1 d . . . H23A H 0.3963 0.4150 0.7952 0.041 Uiso 1 1 calc R . . C24 C 0.38371(8) 0.09961(9) 0.62715(14) 0.0323(5) Uani 1 1 d . . . H24A H 0.3869 0.1188 0.5704 0.039 Uiso 1 1 calc R . . C25 C 0.30870(9) 0.10158(11) 0.60867(16) 0.0469(6) Uani 1 1 d . . . H25A H 0.2928 0.1468 0.6004 0.070 Uiso 1 1 calc R . . H25B H 0.3049 0.0823 0.6635 0.070 Uiso 1 1 calc R . . H25C H 0.2802 0.0768 0.5502 0.070 Uiso 1 1 calc R . . C26 C 0.41097(10) 0.03104(10) 0.64202(18) 0.0494(6) Uani 1 1 d . . . H26A H 0.4590 0.0315 0.6531 0.074 Uiso 1 1 calc R . . H26B H 0.3831 0.0050 0.5847 0.074 Uiso 1 1 calc R . . H26C H 0.4086 0.0120 0.6980 0.074 Uiso 1 1 calc R . . C1S C 0.33500(18) 0.4289(2) 0.9776(2) 0.091(2) Uani 0.584(3) 1 d PG A 1 C2S C 0.3635(2) 0.49095(19) 0.9941(3) 0.103(3) Uani 0.584(3) 1 d PG A 1 H2SA H 0.3354 0.5278 0.9876 0.124 Uiso 0.584(3) 1 calc PR A 1 C3S C 0.4331(2) 0.4991(2) 1.0199(3) 0.138(3) Uani 0.584(3) 1 d PG A 1 H3SA H 0.4525 0.5414 1.0312 0.165 Uiso 0.584(3) 1 calc PR A 1 C4S C 0.47414(19) 0.4451(3) 1.0294(3) 0.121(3) Uani 0.584(3) 1 d PG A 1 H4SA H 0.5217 0.4507 1.0471 0.145 Uiso 0.584(3) 1 calc PR A 1 C5S C 0.4457(2) 0.3831(2) 1.0130(3) 0.140(3) Uani 0.584(3) 1 d PG A 1 H5SA H 0.4737 0.3463 1.0194 0.168 Uiso 0.584(3) 1 calc PR A 1 C6S C 0.3761(2) 0.37501(18) 0.9871(3) 0.114(3) Uani 0.584(3) 1 d PG A 1 H6SA H 0.3566 0.3326 0.9759 0.137 Uiso 0.584(3) 1 calc PR A 1 C7S C 0.2606(5) 0.4146(4) 0.9475(6) 0.151(4) Uani 0.584(3) 1 d P A 1 H7SA H 0.2319 0.4483 0.9027 0.227 Uiso 0.584(3) 1 calc PR A 1 H7SB H 0.2525 0.4142 1.0044 0.227 Uiso 0.584(3) 1 calc PR A 1 H7SC H 0.2487 0.3721 0.9158 0.227 Uiso 0.584(3) 1 calc PR A 1 C1SB C 0.3532(3) 0.4826(3) 1.0336(4) 0.091(3) Uani 0.416(3) 1 d PG A 2 H1SB H 0.3553 0.5256 1.0571 0.110 Uiso 0.416(3) 1 calc PR A 2 C2SB C 0.4130(3) 0.4520(4) 1.0438(5) 0.144(5) Uani 0.416(3) 1 d PG A 2 H2SB H 0.4560 0.4741 1.0742 0.173 Uiso 0.416(3) 1 calc PR A 2 C3SB C 0.4100(5) 0.3891(4) 1.0095(6) 0.126(4) Uani 0.416(3) 1 d PG A 2 H3SB H 0.4509 0.3682 1.0164 0.152 Uiso 0.416(3) 1 calc PR A 2 C4SB C 0.3472(6) 0.3568(3) 0.9650(5) 0.189(6) Uani 0.416(3) 1 d PG A 2 H4SB H 0.3451 0.3138 0.9415 0.227 Uiso 0.416(3) 1 calc PR A 2 C5SB C 0.2874(4) 0.3874(3) 0.9548(5) 0.161(8) Uani 0.416(3) 1 d PG A 2 H5SB H 0.2444 0.3653 0.9244 0.194 Uiso 0.416(3) 1 calc PR A 2 C6SB C 0.2904(3) 0.4503(3) 0.9891(5) 0.132(5) Uani 0.416(3) 1 d PG A 2 H6SB H 0.2495 0.4712 0.9822 0.158 Uiso 0.416(3) 1 calc PR A 2 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 0.01916(18) 0.0186(2) 0.0211(2) 0.000 0.00742(16) 0.000 Cl1 0.0385(3) 0.0435(3) 0.0856(5) -0.0080(3) 0.0147(3) 0.0188(2) O1 0.0221(5) 0.0242(7) 0.0195(6) 0.0005(5) 0.0071(5) 0.0039(5) O2 0.0263(5) 0.0271(7) 0.0257(6) -0.0069(5) 0.0117(5) -0.0060(5) N1 0.0212(6) 0.0232(7) 0.0197(7) 0.0007(6) 0.0096(5) 0.0017(5) C1 0.0203(7) 0.0242(9) 0.0199(8) 0.0011(7) 0.0067(7) -0.0007(6) C2 0.0240(7) 0.0311(10) 0.0248(9) 0.0014(8) 0.0113(7) 0.0032(7) C3 0.0351(9) 0.0458(12) 0.0261(10) 0.0057(9) 0.0178(8) 0.0108(9) C4 0.0293(8) 0.0389(11) 0.0249(9) 0.0071(8) 0.0110(8) 0.0059(8) C5 0.0216(7) 0.0274(10) 0.0280(9) 0.0018(8) 0.0106(7) 0.0045(7) C6 0.0196(7) 0.0259(9) 0.0209(9) -0.0007(7) 0.0088(6) 0.0006(6) C7 0.0151(7) 0.0363(10) 0.0199(9) -0.0012(8) 0.0047(6) 0.0041(7) C8 0.0262(8) 0.0203(9) 0.0286(9) 0.0020(7) 0.0120(7) 0.0013(7) C9 0.0285(8) 0.0329(10) 0.0281(9) 0.0006(8) 0.0160(7) 0.0080(7) C10 0.0421(10) 0.0318(12) 0.0593(14) -0.0017(10) 0.0278(10) 0.0065(9) C11 0.0245(9) 0.0481(14) 0.0648(15) -0.0125(11) 0.0144(9) 0.0051(9) C12 0.0702(12) 0.0752(17) 0.0452(12) 0.0159(12) 0.0395(11) 0.0397(12) C13 0.0382(9) 0.0615(14) 0.0263(10) 0.0174(10) 0.0144(8) 0.0204(10) C14 0.115(2) 0.095(2) 0.0269(13) 0.0095(13) 0.0215(14) 0.0571(18) C15 0.0518(13) 0.199(3) 0.0921(18) 0.110(2) 0.0378(13) 0.0290(18) C16 0.0458(11) 0.0483(13) 0.0338(11) 0.0167(10) 0.0125(9) 0.0155(10) C17 0.0307(8) 0.0284(10) 0.0241(9) 0.0047(8) 0.0164(7) 0.0087(7) C18 0.0253(7) 0.0256(9) 0.0214(8) -0.0010(7) 0.0109(7) 0.0031(7) C19 0.0285(8) 0.0249(10) 0.0307(10) -0.0053(8) 0.0146(7) -0.0022(7) C20 0.0228(8) 0.0366(11) 0.0371(11) -0.0045(9) 0.0098(8) 0.0026(8) C21 0.0303(8) 0.0315(11) 0.0398(11) -0.0014(9) 0.0129(8) 0.0123(8) C22 0.0380(10) 0.0263(10) 0.0494(13) -0.0120(9) 0.0146(9) 0.0013(8) C23 0.0249(8) 0.0335(11) 0.0370(11) -0.0108(9) 0.0083(8) 0.0001(8) C24 0.0288(8) 0.0321(11) 0.0362(10) -0.0126(9) 0.0151(8) -0.0113(8) C25 0.0299(9) 0.0513(14) 0.0539(14) -0.0124(11) 0.0144(9) -0.0120(9) C26 0.0516(11) 0.0337(12) 0.0671(15) -0.0179(11) 0.0306(11) -0.0099(10) C1S 0.126(4) 0.084(4) 0.056(3) 0.017(3) 0.037(3) 0.039(4) C2S 0.129(5) 0.095(5) 0.079(4) 0.007(4) 0.042(4) 0.044(4) C3S 0.142(6) 0.124(6) 0.094(5) -0.027(4) 0.008(5) 0.053(5) C4S 0.131(5) 0.112(5) 0.083(4) -0.008(4) 0.018(4) 0.044(5) C5S 0.189(5) 0.170(6) 0.066(4) 0.041(4) 0.061(4) 0.135(5) C6S 0.226(7) 0.084(5) 0.042(3) 0.008(3) 0.069(4) 0.040(6) C7S 0.225(8) 0.147(8) 0.117(6) 0.037(5) 0.110(6) 0.036(7) C1SB 0.100(6) 0.058(5) 0.094(7) 0.029(5) 0.025(5) 0.024(5) C2SB 0.132(8) 0.224(14) 0.079(6) 0.078(8) 0.051(6) 0.040(9) C3SB 0.172(8) 0.161(11) 0.080(7) 0.065(7) 0.086(6) 0.113(8) C4SB 0.374(16) 0.140(10) 0.098(8) 0.054(6) 0.146(9) 0.159(10) C5SB 0.259(18) 0.092(9) 0.048(6) 0.012(6) -0.004(9) -0.009(10) C6SB 0.134(9) 0.091(7) 0.118(9) 0.031(6) 0.010(7) 0.047(7) _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 O2 1.8224(12) . ? Ti1 O2 1.8224(12) 2_656 ? Ti1 O1 1.8856(13) . ? Ti1 O1 1.8856(13) 2_656 ? Ti1 N1 2.4040(14) 2_656 ? Ti1 N1 2.4040(14) . ? Cl1 C21 1.7418(19) . ? O1 C1 1.345(2) . ? O2 C24 1.421(2) . ? N1 C8 1.482(2) . ? N1 C7 1.493(2) . ? N1 C17 1.502(2) . ? C1 C6 1.408(2) . ? C1 C2 1.418(3) . ? C2 C3 1.399(2) . ? C2 C9 1.543(2) . ? C3 C4 1.392(3) . ? C3 H3A 0.9500 . ? C4 C5 1.382(3) . ? C4 C13 1.541(3) . ? C5 C6 1.395(2) . ? C5 H5A 0.9500 . ? C6 C7 1.512(3) . ? C7 H7A 0.9500 . ? C8 C8 1.512(3) 2_656 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C12 1.524(3) . ? C9 C11 1.530(2) . ? C9 C10 1.533(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.502(3) . ? C13 C16 1.518(3) . ? C13 C14 1.549(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.514(2) . ? C17 H17A 0.9500 . ? C18 C19 1.384(2) . ? C18 C23 1.392(3) . ? C19 C20 1.391(2) . ? C19 H19A 0.9500 . ? C20 C21 1.373(3) . ? C20 H20A 0.9500 . ? C21 C22 1.371(2) . ? C22 C23 1.383(3) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C26 1.506(3) . ? C24 C25 1.526(3) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S C7S 1.498(10) . ? C2S C3S 1.3900 . ? C2S H2SA 0.9500 . ? C3S C4S 1.3900 . ? C3S H3SA 0.9500 . ? C4S C5S 1.3900 . ? C4S H4SA 0.9500 . ? C5S C6S 1.3900 . ? C5S H5SA 0.9500 . ? C6S H6SA 0.9500 . ? C7S H7SA 0.9800 . ? C7S H7SB 0.9800 . ? C7S H7SC 0.9800 . ? C1SB C2SB 1.3900 . ? C1SB C6SB 1.3900 . ? C1SB H1SB 0.9500 . ? C2SB C3SB 1.3900 . ? C2SB H2SB 0.9500 . ? C3SB C4SB 1.3900 . ? C3SB H3SB 0.9500 . ? C4SB C5SB 1.3900 . ? C4SB H4SB 0.9500 . ? C5SB C6SB 1.3900 . ? C5SB H5SB 0.9500 . ? C6SB H6SB 0.9500 . ? 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 O2 Ti1 O2 108.74(8) . 2_656 ? O2 Ti1 O1 95.03(6) . . ? O2 Ti1 O1 91.51(6) 2_656 . ? O2 Ti1 O1 91.51(6) . 2_656 ? O2 Ti1 O1 95.03(6) 2_656 2_656 ? O1 Ti1 O1 168.77(7) . 2_656 ? O2 Ti1 N1 160.72(5) . 2_656 ? O2 Ti1 N1 89.39(5) 2_656 2_656 ? O1 Ti1 N1 90.88(5) . 2_656 ? O1 Ti1 N1 80.09(5) 2_656 2_656 ? O2 Ti1 N1 89.39(5) . . ? O2 Ti1 N1 160.72(5) 2_656 . ? O1 Ti1 N1 80.09(5) . . ? O1 Ti1 N1 90.88(5) 2_656 . ? N1 Ti1 N1 73.55(7) 2_656 . ? C1 O1 Ti1 145.99(11) . . ? C24 O2 Ti1 136.27(12) . . ? C8 N1 C7 109.35(13) . . ? C8 N1 C17 112.84(14) . . ? C7 N1 C17 108.33(12) . . ? C8 N1 Ti1 109.86(9) . . ? C7 N1 Ti1 109.75(10) . . ? C17 N1 Ti1 106.65(10) . . ? O1 C1 C6 118.89(17) . . ? O1 C1 C2 120.98(15) . . ? C6 C1 C2 120.12(15) . . ? C3 C2 C1 116.83(16) . . ? C3 C2 C9 121.41(17) . . ? C1 C2 C9 121.66(15) . . ? C4 C3 C2 124.27(19) . . ? C4 C3 H3A 117.9 . . ? C2 C3 H3A 117.9 . . ? C5 C4 C3 116.97(17) . . ? C5 C4 C13 123.43(17) . . ? C3 C4 C13 119.61(18) . . ? C4 C5 C6 122.17(16) . . ? C4 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C5 C6 C1 119.50(17) . . ? C5 C6 C7 118.46(15) . . ? C1 C6 C7 121.70(15) . . ? N1 C7 C6 116.06(13) . . ? N1 C7 H7A 122.0 . . ? C6 C7 H7A 122.0 . . ? N1 C8 C8 109.95(12) . 2_656 ? N1 C8 H8A 109.7 . . ? C8 C8 H8A 109.7 2_656 . ? N1 C8 H8B 109.7 . . ? C8 C8 H8B 109.7 2_656 . ? H8A C8 H8B 108.2 . . ? C12 C9 C11 108.19(17) . . ? C12 C9 C10 107.78(18) . . ? C11 C9 C10 108.22(16) . . ? C12 C9 C2 111.69(15) . . ? C11 C9 C2 111.83(16) . . ? C10 C9 C2 108.99(15) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C16 108.6(2) . . ? C15 C13 C4 110.08(17) . . ? C16 C13 C4 111.77(18) . . ? C15 C13 C14 111.7(2) . . ? C16 C13 C14 106.02(17) . . ? C4 C13 C14 108.62(19) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 116.98(15) . . ? N1 C17 H17A 121.5 . . ? C18 C17 H17A 121.5 . . ? C19 C18 C23 118.07(16) . . ? C19 C18 C17 120.13(16) . . ? C23 C18 C17 121.71(15) . . ? C18 C19 C20 121.47(17) . . ? C18 C19 H19A 119.3 . . ? C20 C19 H19A 119.3 . . ? C21 C20 C19 118.72(16) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? C22 C21 C20 121.27(17) . . ? C22 C21 Cl1 118.99(15) . . ? C20 C21 Cl1 119.73(14) . . ? C21 C22 C23 119.55(18) . . ? C21 C22 H22A 120.2 . . ? C23 C22 H22A 120.2 . . ? C22 C23 C18 120.91(16) . . ? C22 C23 H23A 119.5 . . ? C18 C23 H23A 119.5 . . ? O2 C24 C26 109.90(15) . . ? O2 C24 C25 108.78(17) . . ? C26 C24 C25 111.57(17) . . ? O2 C24 H24A 108.8 . . ? C26 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C2S C1S C6S 120.0 . . ? C2S C1S C7S 124.5(4) . . ? C6S C1S C7S 115.5(4) . . ? C3S C2S C1S 120.0 . . ? C3S C2S H2SA 120.0 . . ? C1S C2S H2SA 120.0 . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3SA 120.0 . . ? C4S C3S H3SA 120.0 . . ? C3S C4S C5S 120.0 . . ? C3S C4S H4SA 120.0 . . ? C5S C4S H4SA 120.0 . . ? C6S C5S C4S 120.0 . . ? C6S C5S H5SA 120.0 . . ? C4S C5S H5SA 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6SA 120.0 . . ? C1S C6S H6SA 120.0 . . ? C1S C7S H7SA 109.5 . . ? C1S C7S H7SB 109.5 . . ? H7SA C7S H7SB 109.5 . . ? C1S C7S H7SC 109.5 . . ? H7SA C7S H7SC 109.5 . . ? H7SB C7S H7SC 109.5 . . ? C2SB C1SB C6SB 120.0 . . ? C2SB C1SB H1SB 120.0 . . ? C6SB C1SB H1SB 120.0 . . ? C1SB C2SB C3SB 120.0 . . ? C1SB C2SB H2SB 120.0 . . ? C3SB C2SB H2SB 120.0 . . ? C4SB C3SB C2SB 120.0 . . ? C4SB C3SB H3SB 120.0 . . ? C2SB C3SB H3SB 120.0 . . ? C3SB C4SB C5SB 120.0 . . ? C3SB C4SB H4SB 120.0 . . ? C5SB C4SB H4SB 120.0 . . ? C6SB C5SB C4SB 120.0 . . ? C6SB C5SB H5SB 120.0 . . ? C4SB C5SB H5SB 120.0 . . ? C5SB C6SB C1SB 120.0 . . ? C5SB C6SB H6SB 120.0 . . ? C1SB C6SB H6SB 120.0 . . ? 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 O2 Ti1 O1 C1 70.32(19) . . . . ? O2 Ti1 O1 C1 179.29(19) 2_656 . . . ? O1 Ti1 O1 C1 -55.05(18) 2_656 . . . ? N1 Ti1 O1 C1 -91.30(19) 2_656 . . . ? N1 Ti1 O1 C1 -18.17(18) . . . . ? O2 Ti1 O2 C24 -76.44(15) 2_656 . . . ? O1 Ti1 O2 C24 16.87(16) . . . . ? O1 Ti1 O2 C24 -172.27(16) 2_656 . . . ? N1 Ti1 O2 C24 124.21(19) 2_656 . . . ? N1 Ti1 O2 C24 96.87(16) . . . . ? O2 Ti1 N1 C8 -173.98(12) . . . . ? O2 Ti1 N1 C8 -13.5(2) 2_656 . . . ? O1 Ti1 N1 C8 -78.77(11) . . . . ? O1 Ti1 N1 C8 94.52(11) 2_656 . . . ? N1 Ti1 N1 C8 15.12(8) 2_656 . . . ? O2 Ti1 N1 C7 -53.71(11) . . . . ? O2 Ti1 N1 C7 106.77(17) 2_656 . . . ? O1 Ti1 N1 C7 41.50(11) . . . . ? O1 Ti1 N1 C7 -145.22(11) 2_656 . . . ? N1 Ti1 N1 C7 135.38(14) 2_656 . . . ? O2 Ti1 N1 C17 63.42(10) . . . . ? O2 Ti1 N1 C17 -136.09(15) 2_656 . . . ? O1 Ti1 N1 C17 158.63(10) . . . . ? O1 Ti1 N1 C17 -28.08(10) 2_656 . . . ? N1 Ti1 N1 C17 -107.48(11) 2_656 . . . ? Ti1 O1 C1 C6 4.1(3) . . . . ? Ti1 O1 C1 C2 -174.82(13) . . . . ? O1 C1 C2 C3 -177.53(15) . . . . ? C6 C1 C2 C3 3.6(3) . . . . ? O1 C1 C2 C9 6.1(3) . . . . ? C6 C1 C2 C9 -172.82(15) . . . . ? C1 C2 C3 C4 -1.1(3) . . . . ? C9 C2 C3 C4 175.37(17) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? C2 C3 C4 C13 179.11(18) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C13 C4 C5 C6 180.00(18) . . . . ? C4 C5 C6 C1 2.9(3) . . . . ? C4 C5 C6 C7 -170.56(16) . . . . ? O1 C1 C6 C5 176.57(15) . . . . ? C2 C1 C6 C5 -4.5(2) . . . . ? O1 C1 C6 C7 -10.2(2) . . . . ? C2 C1 C6 C7 168.67(15) . . . . ? C8 N1 C7 C6 58.43(19) . . . . ? C17 N1 C7 C6 -178.23(14) . . . . ? Ti1 N1 C7 C6 -62.15(16) . . . . ? C5 C6 C7 N1 -140.12(16) . . . . ? C1 C6 C7 N1 46.6(2) . . . . ? C7 N1 C8 C8 -164.05(17) . . . 2_656 ? C17 N1 C8 C8 75.32(19) . . . 2_656 ? Ti1 N1 C8 C8 -43.5(2) . . . 2_656 ? C3 C2 C9 C12 3.1(3) . . . . ? C1 C2 C9 C12 179.34(18) . . . . ? C3 C2 C9 C11 124.5(2) . . . . ? C1 C2 C9 C11 -59.2(2) . . . . ? C3 C2 C9 C10 -115.9(2) . . . . ? C1 C2 C9 C10 60.4(2) . . . . ? C5 C4 C13 C15 117.8(3) . . . . ? C3 C4 C13 C15 -61.9(3) . . . . ? C5 C4 C13 C16 -3.1(3) . . . . ? C3 C4 C13 C16 177.25(18) . . . . ? C5 C4 C13 C14 -119.7(2) . . . . ? C3 C4 C13 C14 60.6(3) . . . . ? C8 N1 C17 C18 64.15(17) . . . . ? C7 N1 C17 C18 -57.06(19) . . . . ? Ti1 N1 C17 C18 -175.13(11) . . . . ? N1 C17 C18 C19 100.1(2) . . . . ? N1 C17 C18 C23 -83.5(2) . . . . ? C23 C18 C19 C20 0.3(3) . . . . ? C17 C18 C19 C20 176.85(18) . . . . ? C18 C19 C20 C21 0.8(3) . . . . ? C19 C20 C21 C22 -1.1(3) . . . . ? C19 C20 C21 Cl1 179.90(16) . . . . ? C20 C21 C22 C23 0.1(3) . . . . ? Cl1 C21 C22 C23 179.16(18) . . . . ? C21 C22 C23 C18 1.1(3) . . . . ? C19 C18 C23 C22 -1.3(3) . . . . ? C17 C18 C23 C22 -177.76(19) . . . . ? Ti1 O2 C24 C26 91.2(2) . . . . ? Ti1 O2 C24 C25 -146.44(15) . . . . ? C6S C1S C2S C3S 0.0 . . . . ? C7S C1S C2S C3S -178.7(5) . . . . ? C1S C2S C3S C4S 0.0 . . . . ? C2S C3S C4S C5S 0.0 . . . . ? C3S C4S C5S C6S 0.0 . . . . ? C4S C5S C6S C1S 0.0 . . . . ? C2S C1S C6S C5S 0.0 . . . . ? C7S C1S C6S C5S 178.8(4) . . . . ? C6SB C1SB C2SB C3SB 0.0 . . . . ? C1SB C2SB C3SB C4SB 0.0 . . . . ? C2SB C3SB C4SB C5SB 0.0 . . . . ? C3SB C4SB C5SB C6SB 0.0 . . . . ? C4SB C5SB C6SB C1SB 0.0 . . . . ? C2SB C1SB C6SB C5SB 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.709 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.063