# 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 'Prasenjit Ghosh' _publ_contact_author_email PGHOSH@CHEM.IITB.AC.IN _publ_section_title ; Controlled Oxidation of Organic Sulfides to Sulfoxides Under Ambient Conditions by a Series of Titanium Isopropoxide Complexes Using Environmentally Benign H2O2 as an Oxidant ; loop_ _publ_author_name 'Prasenjit Ghosh' 'Manas K. Panda' 'Mobin M Shaikh' #===END data_pg146 _database_code_depnum_ccdc_archive 'CCDC 654513' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Cl4 N2 O4 Ti' _chemical_formula_weight 754.40 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.1277(4) _cell_length_b 15.5670(7) _cell_length_c 21.1098(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3656.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4923 _cell_measurement_theta_min 3.1677 _cell_measurement_theta_max 32.4962 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_T_min 0.8395 _exptl_absorpt_correction_T_max 0.8903 _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 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 21722 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.1140 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6330 _reflns_number_gt 4297 _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^)+(0.0281P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_number_reflns 6330 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _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 0.75023(8) 0.31600(5) 0.75786(3) 0.02299(19) Uani 1 1 d . . . Cl1 Cl 0.35268(10) 0.40830(7) 0.76418(6) 0.0369(3) Uani 1 1 d . . . Cl2 Cl 0.21881(11) 0.20845(9) 0.95979(5) 0.0450(4) Uani 1 1 d . . . Cl3 Cl 1.07878(11) 0.10869(8) 0.49351(5) 0.0377(3) Uani 1 1 d . . . Cl4 Cl 1.15210(11) 0.22892(9) 0.73014(6) 0.0457(4) Uani 1 1 d . . . O1 O 0.8312(3) 0.36903(19) 0.82034(13) 0.0277(8) Uani 1 1 d . . . O2 O 0.7415(3) 0.39266(18) 0.69536(12) 0.0300(7) Uani 1 1 d . . . O3 O 0.5929(3) 0.34053(17) 0.79049(12) 0.0251(8) Uani 1 1 d . . . O4 O 0.8930(2) 0.25954(17) 0.72892(12) 0.0245(7) Uani 1 1 d . . . N1 N 0.7251(3) 0.1931(2) 0.82334(13) 0.0196(8) Uani 1 1 d . . . N2 N 0.6641(3) 0.2156(2) 0.68968(14) 0.0188(8) Uani 1 1 d . . . C1 C 0.9532(4) 0.3869(3) 0.8380(2) 0.0334(13) Uani 1 1 d . . . H1 H 1.0044 0.3369 0.8254 0.040 Uiso 1 1 calc R . . C2 C 0.9577(5) 0.3963(4) 0.90977(19) 0.0480(15) Uani 1 1 d . . . H2A H 0.9068 0.4445 0.9228 0.072 Uiso 1 1 calc R . . H2B H 1.0407 0.4070 0.9231 0.072 Uiso 1 1 calc R . . H2C H 0.9286 0.3433 0.9296 0.072 Uiso 1 1 calc R . . C3 C 0.9974(5) 0.4649(3) 0.8042(2) 0.0521(16) Uani 1 1 d . . . H3A H 0.9954 0.4547 0.7584 0.078 Uiso 1 1 calc R . . H3B H 1.0801 0.4772 0.8174 0.078 Uiso 1 1 calc R . . H3C H 0.9458 0.5139 0.8146 0.078 Uiso 1 1 calc R . . C4 C 0.7441(5) 0.4813(3) 0.6827(2) 0.0403(13) Uani 1 1 d . . . H4 H 0.7690 0.5118 0.7223 0.048 Uiso 1 1 calc R . . C5 C 0.8346(5) 0.5008(4) 0.6319(3) 0.075(2) Uani 1 1 d . . . H5A H 0.9137 0.4793 0.6449 0.113 Uiso 1 1 calc R . . H5B H 0.8389 0.5630 0.6254 0.113 Uiso 1 1 calc R . . H5C H 0.8104 0.4728 0.5924 0.113 Uiso 1 1 calc R . . C6 C 0.6197(5) 0.5109(4) 0.6652(2) 0.0472(16) Uani 1 1 d . . . H6A H 0.5961 0.4848 0.6248 0.071 Uiso 1 1 calc R . . H6B H 0.6192 0.5736 0.6610 0.071 Uiso 1 1 calc R . . H6C H 0.5629 0.4937 0.6983 0.071 Uiso 1 1 calc R . . C7 C 0.5105(4) 0.3105(3) 0.82920(19) 0.0219(11) Uani 1 1 d . . . C8 C 0.3896(4) 0.3366(3) 0.82430(19) 0.0230(11) Uani 1 1 d . . . C9 C 0.3012(4) 0.3075(3) 0.86399(19) 0.0270(11) Uani 1 1 d . . . H9 H 0.2211 0.3279 0.8602 0.032 Uiso 1 1 calc R . . C10 C 0.3316(4) 0.2478(3) 0.9096(2) 0.0325(13) Uani 1 1 d . . . C11 C 0.4475(4) 0.2199(3) 0.91646(19) 0.0255(12) Uani 1 1 d . . . H11 H 0.4667 0.1795 0.9486 0.031 Uiso 1 1 calc R . . C12 C 0.5368(4) 0.2502(3) 0.87673(18) 0.0212(11) Uani 1 1 d . . . C13 C 0.6654(4) 0.2191(3) 0.88379(17) 0.0272(12) Uani 1 1 d . . . H13A H 0.7134 0.2653 0.9036 0.033 Uiso 1 1 calc R . . H13B H 0.6660 0.1693 0.9130 0.033 Uiso 1 1 calc R . . C14 C 0.8463(4) 0.1564(3) 0.83984(19) 0.0257(12) Uani 1 1 d . . . H14A H 0.8949 0.2023 0.8598 0.031 Uiso 1 1 calc R . . H14B H 0.8871 0.1398 0.8000 0.031 Uiso 1 1 calc R . . C15 C 0.8460(4) 0.0792(3) 0.8837(2) 0.0305(12) Uani 1 1 d . . . C16 C 0.8621(5) 0.0898(4) 0.9488(2) 0.0608(18) Uani 1 1 d . . . H16 H 0.8738 0.1454 0.9662 0.073 Uiso 1 1 calc R . . C17 C 0.8607(6) 0.0172(6) 0.9881(3) 0.090(3) Uani 1 1 d . . . H17 H 0.8711 0.0230 1.0325 0.108 Uiso 1 1 calc R . . C18 C 0.8438(7) -0.0633(6) 0.9609(5) 0.104(4) Uani 1 1 d . . . H18 H 0.8407 -0.1125 0.9876 0.125 Uiso 1 1 calc R . . C19 C 0.8318(5) -0.0733(4) 0.8981(4) 0.075(2) Uani 1 1 d . . . H19 H 0.8226 -0.1291 0.8805 0.090 Uiso 1 1 calc R . . C20 C 0.8327(4) -0.0032(3) 0.8597(3) 0.0407(14) Uani 1 1 d . . . H20 H 0.8241 -0.0108 0.8153 0.049 Uiso 1 1 calc R . . C21 C 0.6512(4) 0.1297(3) 0.78809(16) 0.0221(11) Uani 1 1 d . . . H21A H 0.5650 0.1444 0.7924 0.026 Uiso 1 1 calc R . . H21B H 0.6637 0.0717 0.8061 0.026 Uiso 1 1 calc R . . C22 C 0.6861(4) 0.1297(3) 0.71845(16) 0.0218(11) Uani 1 1 d . . . H22A H 0.7721 0.1147 0.7142 0.026 Uiso 1 1 calc R . . H22B H 0.6385 0.0858 0.6956 0.026 Uiso 1 1 calc R . . C23 C 0.5304(4) 0.2312(3) 0.67964(18) 0.0223(11) Uani 1 1 d . . . H23A H 0.4906 0.2309 0.7216 0.027 Uiso 1 1 calc R . . H23B H 0.5201 0.2893 0.6614 0.027 Uiso 1 1 calc R . . C24 C 0.4657(4) 0.1678(3) 0.63733(18) 0.0182(10) Uani 1 1 d . . . C25 C 0.4211(4) 0.0911(3) 0.6608(2) 0.0277(12) Uani 1 1 d . . . H25 H 0.4269 0.0798 0.7049 0.033 Uiso 1 1 calc R . . C26 C 0.3686(4) 0.0306(3) 0.6218(2) 0.0303(12) Uani 1 1 d . . . H26 H 0.3402 -0.0221 0.6388 0.036 Uiso 1 1 calc R . . C27 C 0.3575(4) 0.0475(3) 0.5578(2) 0.0314(12) Uani 1 1 d . . . H27 H 0.3232 0.0059 0.5303 0.038 Uiso 1 1 calc R . . C28 C 0.3967(4) 0.1251(3) 0.53414(19) 0.0313(12) Uani 1 1 d . . . H28 H 0.3862 0.1378 0.4905 0.038 Uiso 1 1 calc R . . C29 C 0.4512(4) 0.1846(3) 0.57322(18) 0.0249(11) Uani 1 1 d . . . H29 H 0.4789 0.2374 0.5561 0.030 Uiso 1 1 calc R . . C30 C 0.7235(4) 0.2213(3) 0.62664(17) 0.0244(11) Uani 1 1 d . . . H30A H 0.7093 0.2796 0.6094 0.029 Uiso 1 1 calc R . . H30B H 0.6837 0.1800 0.5978 0.029 Uiso 1 1 calc R . . C31 C 0.8565(4) 0.2042(3) 0.62492(19) 0.0222(11) Uani 1 1 d . . . C32 C 0.9030(4) 0.1680(3) 0.57000(19) 0.0269(12) Uani 1 1 d . . . H32 H 0.8500 0.1523 0.5367 0.032 Uiso 1 1 calc R . . C33 C 1.0241(4) 0.1546(3) 0.56295(19) 0.0247(12) Uani 1 1 d . . . C34 C 1.1018(4) 0.1743(3) 0.6121(2) 0.0275(11) Uani 1 1 d . . . H34 H 1.1857 0.1648 0.6078 0.033 Uiso 1 1 calc R . . C35 C 1.0557(4) 0.2078(3) 0.66724(18) 0.0224(11) Uani 1 1 d . . . C36 C 0.9325(4) 0.2252(3) 0.6752(2) 0.0222(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0194(4) 0.0194(4) 0.0302(4) -0.0026(4) -0.0019(4) 0.0009(4) Cl1 0.0260(6) 0.0295(7) 0.0553(7) 0.0046(6) -0.0076(7) 0.0048(6) Cl2 0.0385(8) 0.0619(10) 0.0346(6) -0.0074(6) 0.0159(6) -0.0053(7) Cl3 0.0390(7) 0.0505(9) 0.0237(6) -0.0005(6) 0.0055(6) 0.0128(7) Cl4 0.0229(7) 0.0649(10) 0.0494(7) -0.0245(7) -0.0085(7) 0.0063(7) O1 0.0192(18) 0.025(2) 0.0391(18) -0.0155(14) -0.0023(16) 0.0004(15) O2 0.0307(18) 0.0166(18) 0.0428(16) 0.0073(14) 0.0039(17) 0.0055(17) O3 0.0210(16) 0.024(2) 0.0301(16) -0.0044(14) -0.0008(15) -0.0034(15) O4 0.0196(16) 0.0285(19) 0.0252(15) -0.0102(14) 0.0011(15) 0.0001(14) N1 0.017(2) 0.019(2) 0.0226(17) -0.0043(17) -0.0001(17) 0.0051(18) N2 0.016(2) 0.020(2) 0.0203(18) -0.0004(16) -0.0008(17) -0.0009(17) C1 0.022(3) 0.042(4) 0.036(3) -0.016(3) -0.003(2) 0.004(3) C2 0.038(3) 0.066(4) 0.040(3) -0.012(3) -0.006(3) -0.014(3) C3 0.046(4) 0.051(4) 0.059(3) 0.007(3) 0.002(3) -0.023(3) C4 0.040(3) 0.038(3) 0.044(3) 0.010(2) 0.001(3) -0.002(3) C5 0.058(4) 0.073(5) 0.095(5) 0.043(4) 0.022(4) 0.009(4) C6 0.049(4) 0.051(4) 0.042(3) 0.012(3) 0.000(3) 0.012(3) C7 0.022(3) 0.016(3) 0.028(2) -0.010(2) -0.005(2) 0.002(2) C8 0.027(3) 0.017(3) 0.025(2) -0.011(2) -0.004(2) 0.001(2) C9 0.018(2) 0.030(3) 0.034(2) -0.017(2) 0.005(2) -0.001(2) C10 0.032(3) 0.040(4) 0.026(2) -0.012(2) 0.014(2) -0.004(3) C11 0.028(3) 0.029(3) 0.019(2) -0.006(2) 0.003(2) 0.001(3) C12 0.020(3) 0.025(3) 0.019(2) -0.008(2) -0.001(2) 0.006(2) C13 0.032(3) 0.030(3) 0.020(2) -0.001(2) -0.007(2) 0.011(3) C14 0.022(3) 0.033(3) 0.023(2) -0.008(2) -0.004(2) 0.005(2) C15 0.023(3) 0.039(4) 0.029(3) -0.001(2) -0.002(2) 0.011(3) C16 0.048(4) 0.105(5) 0.030(3) 0.003(3) -0.001(3) 0.035(4) C17 0.064(5) 0.166(8) 0.040(4) 0.048(5) 0.012(4) 0.060(6) C18 0.043(4) 0.141(9) 0.128(8) 0.100(7) 0.023(6) 0.024(6) C19 0.043(4) 0.050(5) 0.131(6) 0.050(5) -0.001(5) 0.009(3) C20 0.029(3) 0.029(3) 0.064(4) 0.016(3) -0.006(3) 0.004(3) C21 0.017(2) 0.024(3) 0.026(2) 0.003(2) -0.003(2) 0.001(2) C22 0.029(3) 0.016(3) 0.021(2) -0.0014(19) -0.004(2) -0.003(2) C23 0.020(3) 0.027(3) 0.019(2) -0.001(2) -0.001(2) 0.003(2) C24 0.013(2) 0.020(3) 0.022(2) -0.001(2) 0.005(2) 0.003(2) C25 0.023(3) 0.034(3) 0.026(2) 0.010(2) -0.006(2) 0.002(3) C26 0.027(3) 0.023(3) 0.041(3) 0.006(2) -0.005(3) -0.004(2) C27 0.025(3) 0.029(3) 0.040(3) -0.013(2) -0.003(3) 0.003(3) C28 0.030(3) 0.047(4) 0.017(2) -0.007(2) -0.003(2) -0.003(3) C29 0.022(3) 0.028(3) 0.025(2) 0.006(2) 0.003(2) -0.004(2) C30 0.026(3) 0.026(3) 0.021(2) -0.002(2) -0.008(2) 0.000(2) C31 0.019(3) 0.023(3) 0.024(2) 0.006(2) -0.001(2) -0.001(2) C32 0.026(3) 0.032(3) 0.023(2) 0.007(2) -0.003(2) -0.001(2) C33 0.032(3) 0.024(3) 0.018(2) -0.002(2) -0.003(2) 0.003(2) C34 0.022(3) 0.020(3) 0.041(3) 0.000(2) 0.006(2) 0.004(2) C35 0.014(2) 0.025(3) 0.029(2) -0.005(2) 0.002(2) 0.003(2) C36 0.021(3) 0.015(3) 0.030(3) 0.000(2) -0.001(2) -0.006(2) _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 1.782(3) . ? Ti1 O1 1.798(3) . ? Ti1 O4 1.916(3) . ? Ti1 O3 1.919(3) . ? Ti1 N2 2.331(3) . ? Ti1 N1 2.376(3) . ? Cl1 C8 1.739(4) . ? Cl2 C10 1.753(5) . ? Cl3 C33 1.741(4) . ? Cl4 C35 1.738(4) . ? O1 C1 1.435(5) . ? O2 C4 1.405(5) . ? O3 C7 1.315(5) . ? O4 C36 1.329(5) . ? N1 C21 1.486(5) . ? N1 C13 1.495(4) . ? N1 C14 1.505(5) . ? N2 C30 1.489(5) . ? N2 C22 1.489(5) . ? N2 C23 1.522(5) . ? C1 C3 1.491(6) . ? C1 C2 1.524(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 1.502(6) . ? C4 C6 1.506(7) . ? 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 C12 1.405(6) . ? C7 C8 1.409(6) . ? C8 C9 1.369(6) . ? C9 C10 1.381(6) . ? C9 H9 0.9500 . ? C10 C11 1.368(6) . ? C11 C12 1.384(5) . ? C11 H11 0.9500 . ? C12 C13 1.518(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.517(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.388(6) . ? C15 C16 1.395(6) . ? C16 C17 1.401(9) . ? C16 H16 0.9500 . ? C17 C18 1.392(10) . ? C17 H17 0.9500 . ? C18 C19 1.343(9) . ? C18 H18 0.9500 . ? C19 C20 1.359(7) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.521(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.513(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.384(6) . ? C24 C29 1.388(5) . ? C25 C26 1.381(6) . ? C25 H25 0.9500 . ? C26 C27 1.382(6) . ? C26 H26 0.9500 . ? C27 C28 1.378(6) . ? C27 H27 0.9500 . ? C28 C29 1.380(6) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.504(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.389(5) . ? C31 C36 1.396(5) . ? C32 C33 1.372(6) . ? C32 H32 0.9500 . ? C33 C34 1.386(6) . ? C34 C35 1.374(5) . ? C34 H34 0.9500 . ? C35 C36 1.407(6) . ? 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 105.25(14) . . ? O2 Ti1 O4 96.68(13) . . ? O1 Ti1 O4 91.65(12) . . ? O2 Ti1 O3 94.74(13) . . ? O1 Ti1 O3 95.89(13) . . ? O4 Ti1 O3 164.16(12) . . ? O2 Ti1 N2 88.24(13) . . ? O1 Ti1 N2 165.21(13) . . ? O4 Ti1 N2 80.58(11) . . ? O3 Ti1 N2 88.86(12) . . ? O2 Ti1 N1 164.46(13) . . ? O1 Ti1 N1 90.10(13) . . ? O4 Ti1 N1 85.05(11) . . ? O3 Ti1 N1 81.04(12) . . ? N2 Ti1 N1 76.78(11) . . ? C1 O1 Ti1 138.9(3) . . ? C4 O2 Ti1 142.8(3) . . ? C7 O3 Ti1 142.1(3) . . ? C36 O4 Ti1 137.0(3) . . ? C21 N1 C13 111.1(3) . . ? C21 N1 C14 111.1(3) . . ? C13 N1 C14 107.7(3) . . ? C21 N1 Ti1 108.0(2) . . ? C13 N1 Ti1 109.4(3) . . ? C14 N1 Ti1 109.6(2) . . ? C30 N2 C22 110.2(3) . . ? C30 N2 C23 107.5(3) . . ? C22 N2 C23 111.1(3) . . ? C30 N2 Ti1 109.2(2) . . ? C22 N2 Ti1 106.4(2) . . ? C23 N2 Ti1 112.4(2) . . ? O1 C1 C3 110.2(4) . . ? O1 C1 C2 107.9(4) . . ? C3 C1 C2 112.8(4) . . ? O1 C1 H1 108.6 . . ? C3 C1 H1 108.6 . . ? C2 C1 H1 108.6 . . ? 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 110.4(4) . . ? O2 C4 C6 109.2(4) . . ? C5 C4 C6 112.2(4) . . ? O2 C4 H4 108.3 . . ? C5 C4 H4 108.3 . . ? C6 C4 H4 108.3 . . ? 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 C12 122.4(4) . . ? O3 C7 C8 121.2(4) . . ? C12 C7 C8 116.4(4) . . ? C9 C8 C7 123.1(4) . . ? C9 C8 Cl1 119.3(4) . . ? C7 C8 Cl1 117.6(4) . . ? C8 C9 C10 118.3(4) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? C11 C10 C9 121.2(4) . . ? C11 C10 Cl2 120.0(4) . . ? C9 C10 Cl2 118.8(4) . . ? C10 C11 C12 120.3(4) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 120.7(4) . . ? C11 C12 C13 120.6(4) . . ? C7 C12 C13 118.7(4) . . ? N1 C13 C12 114.9(3) . . ? N1 C13 H13A 108.5 . . ? C12 C13 H13A 108.5 . . ? N1 C13 H13B 108.5 . . ? C12 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? N1 C14 C15 116.1(4) . . ? N1 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? N1 C14 H14B 108.3 . . ? C15 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C20 C15 C16 118.9(5) . . ? C20 C15 C14 120.6(4) . . ? C16 C15 C14 120.5(5) . . ? C15 C16 C17 119.1(6) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 C16 119.0(7) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C17 121.6(8) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C18 C19 C20 119.7(7) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C19 C20 C15 121.7(6) . . ? C19 C20 H20 119.1 . . ? C15 C20 H20 119.1 . . ? N1 C21 C22 110.0(3) . . ? N1 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? N1 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? N2 C22 C21 110.7(3) . . ? N2 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 N2 116.3(3) . . ? C24 C23 H23A 108.2 . . ? N2 C23 H23A 108.2 . . ? C24 C23 H23B 108.2 . . ? N2 C23 H23B 108.2 . . ? H23A C23 H23B 107.4 . . ? C25 C24 C29 118.0(4) . . ? C25 C24 C23 121.5(4) . . ? C29 C24 C23 120.5(4) . . ? C26 C25 C24 121.8(4) . . ? C26 C25 H25 119.1 . . ? C24 C25 H25 119.1 . . ? C25 C26 C27 119.4(4) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C28 C27 C26 119.5(4) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C29 C28 C27 120.7(4) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C24 120.5(4) . . ? C28 C29 H29 119.7 . . ? C24 C29 H29 119.7 . . ? N2 C30 C31 116.6(3) . . ? N2 C30 H30A 108.1 . . ? C31 C30 H30A 108.1 . . ? N2 C30 H30B 108.1 . . ? C31 C30 H30B 108.1 . . ? H30A C30 H30B 107.3 . . ? C32 C31 C36 120.2(4) . . ? C32 C31 C30 117.3(4) . . ? C36 C31 C30 122.5(4) . . ? C33 C32 C31 121.2(4) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 119.8(4) . . ? C32 C33 Cl3 119.8(4) . . ? C34 C33 Cl3 120.3(4) . . ? C35 C34 C33 119.1(4) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C34 C35 C36 122.5(4) . . ? C34 C35 Cl4 119.2(3) . . ? C36 C35 Cl4 118.3(3) . . ? O4 C36 C31 122.8(4) . . ? O4 C36 C35 120.1(4) . . ? C31 C36 C35 117.1(4) . . ? 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 -82.4(5) . . . . ? O4 Ti1 O1 C1 15.0(5) . . . . ? O3 Ti1 O1 C1 -178.9(5) . . . . ? N2 Ti1 O1 C1 72.9(7) . . . . ? N1 Ti1 O1 C1 100.1(5) . . . . ? O1 Ti1 O2 C4 -24.2(5) . . . . ? O4 Ti1 O2 C4 -117.8(5) . . . . ? O3 Ti1 O2 C4 73.2(5) . . . . ? N2 Ti1 O2 C4 161.9(5) . . . . ? N1 Ti1 O2 C4 146.7(5) . . . . ? O2 Ti1 O3 C7 166.3(4) . . . . ? O1 Ti1 O3 C7 -87.8(4) . . . . ? O4 Ti1 O3 C7 30.3(7) . . . . ? N2 Ti1 O3 C7 78.2(4) . . . . ? N1 Ti1 O3 C7 1.4(4) . . . . ? O2 Ti1 O4 C36 -50.6(4) . . . . ? O1 Ti1 O4 C36 -156.2(4) . . . . ? O3 Ti1 O4 C36 85.3(6) . . . . ? N2 Ti1 O4 C36 36.5(4) . . . . ? N1 Ti1 O4 C36 113.9(4) . . . . ? O2 Ti1 N1 C21 5.8(6) . . . . ? O1 Ti1 N1 C21 177.1(2) . . . . ? O4 Ti1 N1 C21 -91.3(2) . . . . ? O3 Ti1 N1 C21 81.1(2) . . . . ? N2 Ti1 N1 C21 -9.8(2) . . . . ? O2 Ti1 N1 C13 -115.2(5) . . . . ? O1 Ti1 N1 C13 56.0(3) . . . . ? O4 Ti1 N1 C13 147.6(3) . . . . ? O3 Ti1 N1 C13 -40.0(2) . . . . ? N2 Ti1 N1 C13 -130.9(3) . . . . ? O2 Ti1 N1 C14 127.0(5) . . . . ? O1 Ti1 N1 C14 -61.8(3) . . . . ? O4 Ti1 N1 C14 29.8(2) . . . . ? O3 Ti1 N1 C14 -157.8(3) . . . . ? N2 Ti1 N1 C14 111.3(3) . . . . ? O2 Ti1 N2 C30 45.0(3) . . . . ? O1 Ti1 N2 C30 -111.2(5) . . . . ? O4 Ti1 N2 C30 -52.1(3) . . . . ? O3 Ti1 N2 C30 139.8(3) . . . . ? N1 Ti1 N2 C30 -139.2(3) . . . . ? O2 Ti1 N2 C22 163.9(2) . . . . ? O1 Ti1 N2 C22 7.8(6) . . . . ? O4 Ti1 N2 C22 66.9(2) . . . . ? O3 Ti1 N2 C22 -101.3(2) . . . . ? N1 Ti1 N2 C22 -20.2(2) . . . . ? O2 Ti1 N2 C23 -74.2(3) . . . . ? O1 Ti1 N2 C23 129.6(5) . . . . ? O4 Ti1 N2 C23 -171.3(3) . . . . ? O3 Ti1 N2 C23 20.6(3) . . . . ? N1 Ti1 N2 C23 101.6(3) . . . . ? Ti1 O1 C1 C3 83.3(6) . . . . ? Ti1 O1 C1 C2 -153.2(3) . . . . ? Ti1 O2 C4 C5 128.2(5) . . . . ? Ti1 O2 C4 C6 -108.0(5) . . . . ? Ti1 O3 C7 C12 19.3(6) . . . . ? Ti1 O3 C7 C8 -159.7(3) . . . . ? O3 C7 C8 C9 -179.4(4) . . . . ? C12 C7 C8 C9 1.6(6) . . . . ? O3 C7 C8 Cl1 1.3(5) . . . . ? C12 C7 C8 Cl1 -177.8(3) . . . . ? C7 C8 C9 C10 -2.1(6) . . . . ? Cl1 C8 C9 C10 177.2(3) . . . . ? C8 C9 C10 C11 1.8(6) . . . . ? C8 C9 C10 Cl2 -178.8(3) . . . . ? C9 C10 C11 C12 -1.0(7) . . . . ? Cl2 C10 C11 C12 179.5(3) . . . . ? C10 C11 C12 C7 0.5(7) . . . . ? C10 C11 C12 C13 -179.6(4) . . . . ? O3 C7 C12 C11 -179.8(4) . . . . ? C8 C7 C12 C11 -0.8(6) . . . . ? O3 C7 C12 C13 0.4(6) . . . . ? C8 C7 C12 C13 179.4(4) . . . . ? C21 N1 C13 C12 -52.8(5) . . . . ? C14 N1 C13 C12 -174.7(4) . . . . ? Ti1 N1 C13 C12 66.3(4) . . . . ? C11 C12 C13 N1 132.8(4) . . . . ? C7 C12 C13 N1 -47.3(6) . . . . ? C21 N1 C14 C15 -63.0(4) . . . . ? C13 N1 C14 C15 58.9(5) . . . . ? Ti1 N1 C14 C15 177.7(3) . . . . ? N1 C14 C15 C20 86.1(5) . . . . ? N1 C14 C15 C16 -95.5(5) . . . . ? C20 C15 C16 C17 -1.9(8) . . . . ? C14 C15 C16 C17 179.7(5) . . . . ? C15 C16 C17 C18 0.3(10) . . . . ? C16 C17 C18 C19 1.6(13) . . . . ? C17 C18 C19 C20 -1.8(12) . . . . ? C18 C19 C20 C15 0.0(10) . . . . ? C16 C15 C20 C19 1.8(8) . . . . ? C14 C15 C20 C19 -179.8(5) . . . . ? C13 N1 C21 C22 158.5(3) . . . . ? C14 N1 C21 C22 -81.6(4) . . . . ? Ti1 N1 C21 C22 38.6(4) . . . . ? C30 N2 C22 C21 167.1(3) . . . . ? C23 N2 C22 C21 -73.9(4) . . . . ? Ti1 N2 C22 C21 48.7(4) . . . . ? N1 C21 C22 N2 -61.2(4) . . . . ? C30 N2 C23 C24 61.3(5) . . . . ? C22 N2 C23 C24 -59.3(4) . . . . ? Ti1 N2 C23 C24 -178.5(3) . . . . ? N2 C23 C24 C25 84.9(5) . . . . ? N2 C23 C24 C29 -94.1(5) . . . . ? C29 C24 C25 C26 3.0(7) . . . . ? C23 C24 C25 C26 -176.0(4) . . . . ? C24 C25 C26 C27 -1.4(7) . . . . ? C25 C26 C27 C28 -1.4(7) . . . . ? C26 C27 C28 C29 2.6(7) . . . . ? C27 C28 C29 C24 -1.0(7) . . . . ? C25 C24 C29 C28 -1.8(6) . . . . ? C23 C24 C29 C28 177.2(4) . . . . ? C22 N2 C30 C31 -56.3(5) . . . . ? C23 N2 C30 C31 -177.5(4) . . . . ? Ti1 N2 C30 C31 60.3(4) . . . . ? N2 C30 C31 C32 149.2(4) . . . . ? N2 C30 C31 C36 -32.4(6) . . . . ? C36 C31 C32 C33 -2.0(7) . . . . ? C30 C31 C32 C33 176.4(4) . . . . ? C31 C32 C33 C34 2.4(7) . . . . ? C31 C32 C33 Cl3 179.7(3) . . . . ? C32 C33 C34 C35 -0.5(7) . . . . ? Cl3 C33 C34 C35 -177.8(3) . . . . ? C33 C34 C35 C36 -1.8(7) . . . . ? C33 C34 C35 Cl4 177.6(3) . . . . ? Ti1 O4 C36 C31 -16.5(7) . . . . ? Ti1 O4 C36 C35 164.0(3) . . . . ? C32 C31 C36 O4 -179.7(4) . . . . ? C30 C31 C36 O4 2.0(7) . . . . ? C32 C31 C36 C35 -0.2(6) . . . . ? C30 C31 C36 C35 -178.5(4) . . . . ? C34 C35 C36 O4 -178.4(4) . . . . ? Cl4 C35 C36 O4 2.2(6) . . . . ? C34 C35 C36 C31 2.1(7) . . . . ? Cl4 C35 C36 C31 -177.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.331 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.064 #===END # Attachment 'MP-Ti-sulfox_CombinedCIF.cif' data_pg194 _database_code_depnum_ccdc_archive 'CCDC 679212' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H80 N2 O8 Ti' _chemical_formula_weight 1029.18 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 11.8560(3) _cell_length_b 16.7553(6) _cell_length_c 16.9088(6) _cell_angle_alpha 62.844(4) _cell_angle_beta 86.881(3) _cell_angle_gamma 70.612(3) _cell_volume 2800.27(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10244 _cell_measurement_theta_min 3.0571 _cell_measurement_theta_max 32.5405 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.209 _exptl_absorpt_correction_T_min 0.9343 _exptl_absorpt_correction_T_max 0.9555 _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 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 25227 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9773 _reflns_number_gt 6751 _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^)+(0.0811P)^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 9773 _refine_ls_number_parameters 672 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 0.60337(4) 0.35061(3) 0.32895(3) 0.01825(13) Uani 1 1 d . . . O1 O 0.68701(13) 0.42248(11) 0.34391(10) 0.0204(4) Uani 1 1 d . . . O2 O 0.50864(14) 0.35009(12) 0.41705(11) 0.0248(4) Uani 1 1 d . . . O3 O 0.08503(17) 0.80998(14) -0.03083(13) 0.0442(5) Uani 1 1 d . . . O4 O -0.02687(18) 0.86753(15) 0.06114(17) 0.0562(6) Uani 1 1 d . . . O5 O 0.51489(14) 0.29439(12) 0.29253(10) 0.0208(4) Uani 1 1 d . . . O6 O 0.73595(14) 0.24365(12) 0.37809(11) 0.0264(4) Uani 1 1 d . . . O7 O 1.07788(15) 0.32059(13) -0.01463(12) 0.0335(4) Uani 1 1 d . . . O8 O 1.00122(16) 0.46889(14) -0.13948(12) 0.0362(5) Uani 1 1 d . . . N1 N 0.47023(16) 0.51182(14) 0.23090(12) 0.0191(4) Uani 1 1 d . . . N2 N 0.65873(16) 0.38733(14) 0.18127(12) 0.0192(4) Uani 1 1 d . . . C1 C 0.6941(2) 0.50933(17) 0.31693(15) 0.0201(5) Uani 1 1 d . . . C2 C 0.8031(2) 0.52012(18) 0.33262(15) 0.0209(5) Uani 1 1 d . . . C3 C 0.8032(2) 0.61364(19) 0.29588(16) 0.0242(6) Uani 1 1 d . . . H3 H 0.8753 0.6228 0.3051 0.029 Uiso 1 1 calc R . . C4 C 0.7033(2) 0.69423(18) 0.24651(16) 0.0250(6) Uani 1 1 d . . . C5 C 0.5965(2) 0.68050(18) 0.23788(16) 0.0237(6) Uani 1 1 d . . . H5 H 0.5261 0.7345 0.2071 0.028 Uiso 1 1 calc R . . C6 C 0.5903(2) 0.58944(17) 0.27332(15) 0.0202(5) Uani 1 1 d . . . C7 C 0.9118(2) 0.43365(19) 0.39507(17) 0.0255(6) Uani 1 1 d . . . C8 C 0.8746(2) 0.3941(2) 0.49003(17) 0.0349(7) Uani 1 1 d . . . H8A H 0.8515 0.4440 0.5089 0.052 Uiso 1 1 calc R . . H8B H 0.9424 0.3394 0.5313 0.052 Uiso 1 1 calc R . . H8C H 0.8061 0.3735 0.4905 0.052 Uiso 1 1 calc R . . C9 C 0.9514(2) 0.3549(2) 0.36643(19) 0.0313(6) Uani 1 1 d . . . H9A H 0.8866 0.3291 0.3717 0.047 Uiso 1 1 calc R . . H9B H 1.0237 0.3036 0.4051 0.047 Uiso 1 1 calc R . . H9C H 0.9691 0.3815 0.3042 0.047 Uiso 1 1 calc R . . C10 C 1.0213(2) 0.4626(2) 0.3969(2) 0.0375(7) Uani 1 1 d . . . H10A H 1.0450 0.4896 0.3365 0.056 Uiso 1 1 calc R . . H10B H 1.0883 0.4063 0.4372 0.056 Uiso 1 1 calc R . . H10C H 1.0003 0.5105 0.4184 0.056 Uiso 1 1 calc R . . C11 C 0.7119(3) 0.7928(2) 0.2029(2) 0.0386(7) Uani 1 1 d . . . H11A H 0.7532 0.8023 0.1492 0.058 Uiso 1 1 calc R . . H11B H 0.7573 0.7994 0.2450 0.058 Uiso 1 1 calc R . . H11C H 0.6308 0.8409 0.1861 0.058 Uiso 1 1 calc R . . C12 C 0.5052(3) 0.3672(3) 0.4917(2) 0.0562(10) Uani 1 1 d . . . H12 H 0.5324 0.4232 0.4726 0.067 Uiso 1 1 calc R . . C13 C 0.3758(3) 0.4004(3) 0.5082(2) 0.0684(11) Uani 1 1 d . . . H13A H 0.3289 0.4566 0.4538 0.103 Uiso 1 1 calc R . . H13B H 0.3712 0.4171 0.5571 0.103 Uiso 1 1 calc R . . H13C H 0.3430 0.3491 0.5245 0.103 Uiso 1 1 calc R . . C14 C 0.5863(3) 0.2910(3) 0.5690(2) 0.0687(11) Uani 1 1 d . . . H14A H 0.5600 0.2354 0.5935 0.103 Uiso 1 1 calc R . . H14B H 0.5866 0.3120 0.6143 0.103 Uiso 1 1 calc R . . H14C H 0.6677 0.2733 0.5518 0.103 Uiso 1 1 calc R . . C15 C 0.4711(2) 0.57604(18) 0.26966(16) 0.0219(5) Uani 1 1 d . . . H15A H 0.4480 0.5496 0.3311 0.026 Uiso 1 1 calc R . . H15B H 0.4090 0.6395 0.2337 0.026 Uiso 1 1 calc R . . C16 C 0.34464(19) 0.50889(17) 0.22761(16) 0.0207(5) Uani 1 1 d . . . H16A H 0.3291 0.4717 0.2896 0.025 Uiso 1 1 calc R . . H16B H 0.3424 0.4735 0.1945 0.025 Uiso 1 1 calc R . . C17 C 0.2429(2) 0.60430(18) 0.18512(17) 0.0226(5) Uani 1 1 d . . . C18 C 0.2148(2) 0.65743(18) 0.09185(16) 0.0238(6) Uani 1 1 d . . . H18 H 0.2576 0.6337 0.0534 0.029 Uiso 1 1 calc R . . C19 C 0.1238(2) 0.74472(19) 0.05773(18) 0.0294(6) Uani 1 1 d . . . C20 C 0.0578(2) 0.77905(19) 0.1124(2) 0.0353(7) Uani 1 1 d . . . C21 C 0.0809(2) 0.7285(2) 0.2035(2) 0.0355(7) Uani 1 1 d . . . H21 H 0.0348 0.7521 0.2410 0.043 Uiso 1 1 calc R . . C22 C 0.1749(2) 0.64074(19) 0.23910(18) 0.0272(6) Uani 1 1 d . . . H22 H 0.1935 0.6044 0.3022 0.033 Uiso 1 1 calc R . . C23 C -0.0191(3) 0.8841(2) -0.0297(3) 0.0604(10) Uani 1 1 d . . . H23A H -0.0926 0.8829 -0.0536 0.072 Uiso 1 1 calc R . . H23B H -0.0116 0.9474 -0.0674 0.072 Uiso 1 1 calc R . . C24 C 0.5117(2) 0.54723(17) 0.14110(15) 0.0209(5) Uani 1 1 d . . . H24A H 0.5768 0.5719 0.1413 0.025 Uiso 1 1 calc R . . H24B H 0.4442 0.6005 0.0966 0.025 Uiso 1 1 calc R . . C25 C 0.5574(2) 0.46833(17) 0.11502(15) 0.0201(5) Uani 1 1 d . . . H25A H 0.4914 0.4456 0.1121 0.024 Uiso 1 1 calc R . . H25B H 0.5851 0.4931 0.0550 0.024 Uiso 1 1 calc R . . C26 C 0.7736(2) 0.40903(18) 0.17369(15) 0.0204(5) Uani 1 1 d . . . H26A H 0.8343 0.3542 0.2228 0.024 Uiso 1 1 calc R . . H26B H 0.7580 0.4652 0.1839 0.024 Uiso 1 1 calc R . . C27 C 0.8287(2) 0.42894(18) 0.08690(16) 0.0213(5) Uani 1 1 d . . . C28 C 0.9293(2) 0.35668(18) 0.08318(16) 0.0232(6) Uani 1 1 d . . . H28 H 0.9607 0.2951 0.1333 0.028 Uiso 1 1 calc R . . C29 C 0.9798(2) 0.37886(18) 0.00435(16) 0.0235(6) Uani 1 1 d . . . C30 C 0.9348(2) 0.46695(19) -0.06983(16) 0.0250(6) Uani 1 1 d . . . C31 C 0.8382(2) 0.53869(19) -0.06835(17) 0.0274(6) Uani 1 1 d . . . H31 H 0.8078 0.5997 -0.1194 0.033 Uiso 1 1 calc R . . C32 C 0.7861(2) 0.51832(18) 0.01144(16) 0.0248(6) Uani 1 1 d . . . H32 H 0.7193 0.5670 0.0145 0.030 Uiso 1 1 calc R . . C33 C 1.0887(2) 0.3754(2) -0.10698(18) 0.0356(7) Uani 1 1 d . . . H33A H 1.1705 0.3792 -0.1137 0.043 Uiso 1 1 calc R . . H33B H 1.0755 0.3445 -0.1417 0.043 Uiso 1 1 calc R . . C34 C 0.6820(2) 0.30169(17) 0.16788(16) 0.0212(5) Uani 1 1 d . . . H34A H 0.7416 0.2463 0.2173 0.025 Uiso 1 1 calc R . . H34B H 0.7184 0.3127 0.1114 0.025 Uiso 1 1 calc R . . C35 C 0.5719(2) 0.27663(17) 0.16420(15) 0.0196(5) Uani 1 1 d . . . C36 C 0.5465(2) 0.25993(17) 0.09474(16) 0.0226(5) Uani 1 1 d . . . H36 H 0.5985 0.2657 0.0491 0.027 Uiso 1 1 calc R . . C37 C 0.4473(2) 0.23498(17) 0.09054(16) 0.0239(6) Uani 1 1 d . . . C38 C 0.3772(2) 0.22166(18) 0.16132(16) 0.0252(6) Uani 1 1 d . . . H38 H 0.3110 0.2021 0.1603 0.030 Uiso 1 1 calc R . . C39 C 0.3993(2) 0.23560(17) 0.23389(16) 0.0226(5) Uani 1 1 d . . . C40 C 0.4951(2) 0.26943(17) 0.23141(16) 0.0208(5) Uani 1 1 d . . . C41 C 0.4146(2) 0.2236(2) 0.01203(18) 0.0333(6) Uani 1 1 d . . . H41A H 0.3384 0.2115 0.0189 0.050 Uiso 1 1 calc R . . H41B H 0.4782 0.1697 0.0099 0.050 Uiso 1 1 calc R . . H41C H 0.4061 0.2822 -0.0436 0.050 Uiso 1 1 calc R . . C42 C 0.3281(2) 0.20956(19) 0.31525(17) 0.0283(6) Uani 1 1 d . . . C43 C 0.2242(3) 0.1811(2) 0.3004(2) 0.0440(8) Uani 1 1 d . . . H43A H 0.1676 0.2350 0.2494 0.066 Uiso 1 1 calc R . . H43B H 0.1825 0.1636 0.3542 0.066 Uiso 1 1 calc R . . H43C H 0.2559 0.1263 0.2882 0.066 Uiso 1 1 calc R . . C44 C 0.2744(2) 0.2921(2) 0.33842(19) 0.0334(7) Uani 1 1 d . . . H44A H 0.3395 0.3082 0.3538 0.050 Uiso 1 1 calc R . . H44B H 0.2284 0.2727 0.3895 0.050 Uiso 1 1 calc R . . H44C H 0.2210 0.3480 0.2868 0.050 Uiso 1 1 calc R . . C45 C 0.4154(3) 0.1241(2) 0.39637(18) 0.0404(7) Uani 1 1 d . . . H45A H 0.4492 0.0700 0.3834 0.061 Uiso 1 1 calc R . . H45B H 0.3719 0.1057 0.4490 0.061 Uiso 1 1 calc R . . H45C H 0.4807 0.1423 0.4081 0.061 Uiso 1 1 calc R . . C46 C 0.7754(3) 0.14463(19) 0.40640(19) 0.0355(7) Uani 1 1 d . . . H46 H 0.7305 0.1329 0.3668 0.043 Uiso 1 1 calc R . . C47 C 0.9094(3) 0.1116(2) 0.3958(2) 0.0552(9) Uani 1 1 d . . . H47A H 0.9219 0.1495 0.3339 0.083 Uiso 1 1 calc R . . H47B H 0.9374 0.0439 0.4105 0.083 Uiso 1 1 calc R . . H47C H 0.9548 0.1202 0.4363 0.083 Uiso 1 1 calc R . . C48 C 0.7508(3) 0.0921(2) 0.5015(2) 0.0575(9) Uani 1 1 d . . . H48A H 0.7980 0.1002 0.5414 0.086 Uiso 1 1 calc R . . H48B H 0.7735 0.0240 0.5189 0.086 Uiso 1 1 calc R . . H48C H 0.6649 0.1181 0.5061 0.086 Uiso 1 1 calc R . . C49 C 0.6202(5) -0.1059(4) 0.3631(3) 0.1146(18) Uani 1 1 d . . . H49A H 0.5481 -0.0486 0.3451 0.172 Uiso 1 1 calc R . . H49B H 0.6292 -0.1455 0.4281 0.172 Uiso 1 1 calc R . . H49C H 0.6121 -0.1425 0.3334 0.172 Uiso 1 1 calc R . . C50 C 0.7249(5) -0.0781(3) 0.3376(3) 0.0789(12) Uani 1 1 d . . . C51 C 0.8405(5) -0.1426(3) 0.3803(3) 0.0948(16) Uani 1 1 d . . . H51 H 0.8494 -0.2043 0.4276 0.114 Uiso 1 1 calc R . . C52 C 0.9397(6) -0.1177(4) 0.3548(4) 0.1055(17) Uani 1 1 d . . . H52 H 1.0161 -0.1606 0.3875 0.127 Uiso 1 1 calc R . . C53 C 0.9314(6) -0.0303(3) 0.2812(3) 0.1043(17) Uani 1 1 d . . . H53 H 1.0008 -0.0146 0.2598 0.125 Uiso 1 1 calc R . . C54 C 0.8158(5) 0.0325(3) 0.2413(3) 0.0784(12) Uani 1 1 d . . . H54 H 0.8061 0.0942 0.1935 0.094 Uiso 1 1 calc R . . C55 C 0.7143(5) 0.0084(3) 0.2685(3) 0.0774(13) Uani 1 1 d . . . H55 H 0.6370 0.0527 0.2387 0.093 Uiso 1 1 calc R . . C56 C 0.2887(3) 0.9557(3) -0.0407(3) 0.0765(13) Uani 1 1 d . . . H56A H 0.2844 0.8960 -0.0351 0.115 Uiso 1 1 calc R . . H56B H 0.3572 0.9686 -0.0727 0.115 Uiso 1 1 calc R . . H56C H 0.2141 1.0084 -0.0740 0.115 Uiso 1 1 calc R . . C57 C 0.3047(3) 0.9468(2) 0.0508(3) 0.0567(10) Uani 1 1 d . . . C58 C 0.2653(3) 0.8854(3) 0.1214(4) 0.0773(13) Uani 1 1 d . . . H58 H 0.2306 0.8459 0.1129 0.093 Uiso 1 1 calc R . . C59 C 0.2742(4) 0.8790(3) 0.2045(4) 0.0831(14) Uani 1 1 d . . . H59 H 0.2445 0.8360 0.2523 0.100 Uiso 1 1 calc R . . C60 C 0.3263(4) 0.9348(3) 0.2200(3) 0.0751(12) Uani 1 1 d . . . H60 H 0.3317 0.9314 0.2774 0.090 Uiso 1 1 calc R . . C61 C 0.3698(3) 0.9952(3) 0.1483(3) 0.0644(10) Uani 1 1 d . . . H61 H 0.4078 1.0331 0.1566 0.077 Uiso 1 1 calc R . . C62 C 0.3585(3) 1.0008(2) 0.0660(3) 0.0545(9) Uani 1 1 d . . . H62 H 0.3885 1.0431 0.0177 0.065 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(2) 0.0193(2) 0.0157(2) -0.00805(19) 0.00198(17) -0.00546(18) O1 0.0192(8) 0.0221(9) 0.0191(9) -0.0090(7) 0.0016(7) -0.0070(7) O2 0.0264(9) 0.0308(10) 0.0192(9) -0.0126(8) 0.0067(7) -0.0114(8) O3 0.0371(11) 0.0301(12) 0.0392(12) -0.0007(10) -0.0103(9) -0.0009(9) O4 0.0397(12) 0.0331(13) 0.0708(17) -0.0179(12) -0.0068(11) 0.0098(10) O5 0.0234(8) 0.0249(9) 0.0192(9) -0.0121(8) 0.0063(7) -0.0125(7) O6 0.0257(9) 0.0213(10) 0.0280(10) -0.0110(8) -0.0023(8) -0.0031(8) O7 0.0264(10) 0.0406(12) 0.0319(11) -0.0195(9) 0.0118(8) -0.0074(9) O8 0.0350(10) 0.0468(13) 0.0250(10) -0.0150(9) 0.0125(8) -0.0160(10) N1 0.0174(10) 0.0222(11) 0.0189(10) -0.0102(9) 0.0018(8) -0.0073(9) N2 0.0182(10) 0.0208(11) 0.0182(10) -0.0094(9) 0.0029(8) -0.0060(9) C1 0.0233(12) 0.0237(14) 0.0180(12) -0.0130(11) 0.0054(10) -0.0092(11) C2 0.0192(12) 0.0286(15) 0.0189(12) -0.0153(11) 0.0048(10) -0.0071(11) C3 0.0229(13) 0.0354(16) 0.0241(13) -0.0194(12) 0.0072(11) -0.0140(12) C4 0.0331(14) 0.0259(15) 0.0228(13) -0.0152(12) 0.0091(11) -0.0132(12) C5 0.0259(13) 0.0261(15) 0.0201(13) -0.0134(12) 0.0033(11) -0.0065(11) C6 0.0222(12) 0.0242(14) 0.0174(12) -0.0130(11) 0.0039(10) -0.0073(11) C7 0.0202(12) 0.0307(15) 0.0268(14) -0.0151(12) -0.0005(11) -0.0073(11) C8 0.0308(15) 0.0390(17) 0.0252(15) -0.0120(13) -0.0050(12) -0.0038(13) C9 0.0188(13) 0.0376(17) 0.0393(16) -0.0233(14) -0.0024(12) -0.0029(12) C10 0.0240(14) 0.0415(18) 0.0501(18) -0.0240(15) -0.0044(13) -0.0097(13) C11 0.0413(17) 0.0317(17) 0.0473(18) -0.0183(14) 0.0091(14) -0.0184(14) C12 0.0462(19) 0.086(3) 0.0303(18) -0.0331(19) 0.0032(15) -0.0063(18) C13 0.056(2) 0.092(3) 0.041(2) -0.037(2) 0.0090(17) 0.002(2) C14 0.061(2) 0.097(3) 0.036(2) -0.031(2) -0.0001(17) -0.011(2) C15 0.0199(12) 0.0216(14) 0.0227(13) -0.0111(11) 0.0017(10) -0.0042(10) C16 0.0199(12) 0.0223(14) 0.0205(13) -0.0095(11) 0.0023(10) -0.0089(11) C17 0.0158(12) 0.0238(14) 0.0295(14) -0.0121(12) 0.0006(10) -0.0083(10) C18 0.0172(12) 0.0260(14) 0.0278(14) -0.0121(12) 0.0011(11) -0.0073(11) C19 0.0246(13) 0.0244(15) 0.0330(16) -0.0075(13) -0.0047(12) -0.0082(12) C20 0.0219(14) 0.0198(15) 0.054(2) -0.0132(14) -0.0037(13) 0.0005(12) C21 0.0227(14) 0.0419(18) 0.0488(19) -0.0292(16) 0.0089(13) -0.0081(13) C22 0.0209(13) 0.0336(16) 0.0319(15) -0.0173(13) 0.0058(11) -0.0127(12) C23 0.048(2) 0.039(2) 0.062(2) -0.0096(18) -0.0138(18) 0.0059(16) C24 0.0182(12) 0.0232(14) 0.0198(13) -0.0084(11) 0.0017(10) -0.0079(10) C25 0.0195(12) 0.0230(14) 0.0155(12) -0.0061(11) 0.0002(10) -0.0086(10) C26 0.0184(12) 0.0257(14) 0.0194(13) -0.0117(11) 0.0020(10) -0.0085(11) C27 0.0190(12) 0.0262(14) 0.0228(13) -0.0130(11) 0.0023(10) -0.0103(11) C28 0.0202(12) 0.0256(14) 0.0237(13) -0.0097(11) 0.0026(10) -0.0103(11) C29 0.0192(12) 0.0296(15) 0.0260(14) -0.0155(12) 0.0044(11) -0.0103(11) C30 0.0233(13) 0.0382(16) 0.0236(14) -0.0178(13) 0.0085(11) -0.0183(12) C31 0.0291(14) 0.0294(15) 0.0204(13) -0.0058(12) 0.0007(11) -0.0144(12) C32 0.0228(13) 0.0251(14) 0.0285(14) -0.0131(12) 0.0060(11) -0.0100(11) C33 0.0347(15) 0.0478(19) 0.0346(16) -0.0249(15) 0.0162(13) -0.0198(14) C34 0.0226(12) 0.0212(13) 0.0188(13) -0.0102(11) 0.0056(10) -0.0058(10) C35 0.0204(12) 0.0156(13) 0.0210(13) -0.0088(11) -0.0007(10) -0.0030(10) C36 0.0292(13) 0.0178(13) 0.0182(13) -0.0069(11) 0.0045(11) -0.0075(11) C37 0.0300(14) 0.0169(13) 0.0232(13) -0.0088(11) -0.0022(11) -0.0061(11) C38 0.0231(13) 0.0241(14) 0.0293(14) -0.0115(12) -0.0009(11) -0.0102(11) C39 0.0204(12) 0.0182(13) 0.0260(14) -0.0082(11) 0.0007(10) -0.0058(10) C40 0.0225(12) 0.0169(13) 0.0204(13) -0.0086(11) -0.0012(10) -0.0032(10) C41 0.0403(16) 0.0351(17) 0.0308(15) -0.0181(13) -0.0007(13) -0.0155(13) C42 0.0269(13) 0.0299(15) 0.0317(15) -0.0144(13) 0.0078(12) -0.0145(12) C43 0.0428(17) 0.054(2) 0.052(2) -0.0278(17) 0.0192(15) -0.0332(16) C44 0.0284(14) 0.0375(17) 0.0379(16) -0.0193(14) 0.0165(12) -0.0149(13) C45 0.0430(17) 0.0340(17) 0.0288(16) -0.0046(14) 0.0082(13) -0.0103(14) C46 0.0417(16) 0.0193(15) 0.0369(16) -0.0106(13) -0.0052(13) -0.0027(12) C47 0.0426(18) 0.042(2) 0.060(2) -0.0230(18) -0.0042(16) 0.0107(15) C48 0.075(2) 0.0315(19) 0.046(2) -0.0033(16) 0.0001(18) -0.0153(17) C49 0.123(4) 0.129(5) 0.087(4) -0.060(4) 0.024(3) -0.026(4) C50 0.109(4) 0.070(3) 0.065(3) -0.034(2) -0.006(3) -0.031(3) C51 0.113(4) 0.053(3) 0.075(3) -0.012(2) -0.042(3) 0.005(3) C52 0.117(4) 0.071(4) 0.108(4) -0.034(3) -0.035(4) -0.012(3) C53 0.158(5) 0.054(3) 0.085(4) -0.038(3) -0.025(3) -0.005(3) C54 0.118(4) 0.041(2) 0.061(3) -0.021(2) -0.008(3) -0.011(3) C55 0.126(4) 0.037(2) 0.052(2) -0.017(2) -0.020(2) -0.008(2) C56 0.059(2) 0.059(3) 0.113(4) -0.057(3) -0.024(2) 0.007(2) C57 0.0409(18) 0.0316(19) 0.092(3) -0.031(2) -0.0136(19) -0.0002(15) C58 0.061(2) 0.048(2) 0.107(4) -0.018(3) -0.020(3) -0.022(2) C59 0.067(3) 0.052(3) 0.101(4) -0.006(3) 0.001(3) -0.029(2) C60 0.082(3) 0.053(3) 0.065(3) -0.013(2) -0.005(2) -0.013(2) C61 0.081(3) 0.042(2) 0.071(3) -0.023(2) -0.001(2) -0.025(2) C62 0.056(2) 0.040(2) 0.075(3) -0.0311(19) 0.0037(18) -0.0188(17) _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 O6 1.8127(17) . ? Ti1 O2 1.8147(16) . ? Ti1 O1 1.8961(16) . ? Ti1 O5 1.9036(16) . ? Ti1 N2 2.3942(19) . ? Ti1 N1 2.430(2) . ? O1 C1 1.343(3) . ? O2 C12 1.412(3) . ? O3 C19 1.377(3) . ? O3 C23 1.438(4) . ? O4 C20 1.375(3) . ? O4 C23 1.434(4) . ? O5 C40 1.336(3) . ? O6 C46 1.409(3) . ? O7 C29 1.378(3) . ? O7 C33 1.430(3) . ? O8 C30 1.374(3) . ? O8 C33 1.425(3) . ? N1 C24 1.480(3) . ? N1 C15 1.496(3) . ? N1 C16 1.511(3) . ? N2 C25 1.489(3) . ? N2 C34 1.488(3) . ? N2 C26 1.507(3) . ? C1 C6 1.400(3) . ? C1 C2 1.418(3) . ? C2 C3 1.398(3) . ? C2 C7 1.544(3) . ? C3 C4 1.393(3) . ? C3 H3 0.9500 . ? C4 C5 1.386(3) . ? C4 C11 1.509(4) . ? C5 C6 1.389(3) . ? C5 H5 0.9500 . ? C6 C15 1.512(3) . ? C7 C9 1.531(4) . ? C7 C10 1.536(3) . ? C7 C8 1.535(3) . ? 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 C14 1.437(4) . ? C12 C13 1.506(4) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.514(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.399(3) . ? C17 C18 1.403(3) . ? C18 C19 1.373(3) . ? C18 H18 0.9500 . ? C19 C20 1.380(4) . ? C20 C21 1.366(4) . ? C21 C22 1.394(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.506(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.512(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.396(3) . ? C27 C28 1.412(3) . ? C28 C29 1.372(3) . ? C28 H28 0.9500 . ? C29 C30 1.377(4) . ? C30 C31 1.367(4) . ? C31 C32 1.395(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.510(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.394(3) . ? C35 C40 1.404(3) . ? C36 C37 1.388(3) . ? C36 H36 0.9500 . ? C37 C38 1.394(3) . ? C37 C41 1.511(3) . ? C38 C39 1.402(3) . ? C38 H38 0.9500 . ? C39 C40 1.419(3) . ? C39 C42 1.538(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.530(4) . ? C42 C44 1.534(4) . ? C42 C45 1.543(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 . ? C46 C48 1.508(4) . ? C46 C47 1.529(4) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.445(6) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C55 1.352(6) . ? C50 C51 1.407(6) . ? C51 C52 1.359(7) . ? C51 H51 0.9500 . ? C52 C53 1.399(7) . ? C52 H52 0.9500 . ? C53 C54 1.392(6) . ? C53 H53 0.9500 . ? C54 C55 1.384(6) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.502(5) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.356(5) . ? C57 C62 1.381(4) . ? C58 C59 1.366(6) . ? C58 H58 0.9500 . ? C59 C60 1.396(6) . ? C59 H59 0.9500 . ? C60 C61 1.386(5) . ? C60 H60 0.9500 . ? C61 C62 1.363(5) . ? C61 H61 0.9500 . ? C62 H62 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 O6 Ti1 O2 107.58(8) . . ? O6 Ti1 O1 90.58(7) . . ? O2 Ti1 O1 95.28(7) . . ? O6 Ti1 O5 94.88(7) . . ? O2 Ti1 O5 91.03(7) . . ? O1 Ti1 O5 170.03(7) . . ? O6 Ti1 N2 91.62(7) . . ? O2 Ti1 N2 159.13(7) . . ? O1 Ti1 N2 92.55(7) . . ? O5 Ti1 N2 78.97(6) . . ? O6 Ti1 N1 161.81(7) . . ? O2 Ti1 N1 88.79(7) . . ? O1 Ti1 N1 79.80(6) . . ? O5 Ti1 N1 92.65(7) . . ? N2 Ti1 N1 73.59(6) . . ? C1 O1 Ti1 146.63(15) . . ? C12 O2 Ti1 138.74(18) . . ? C19 O3 C23 105.2(2) . . ? C20 O4 C23 105.7(2) . . ? C40 O5 Ti1 146.67(15) . . ? C46 O6 Ti1 141.71(16) . . ? C29 O7 C33 105.5(2) . . ? C30 O8 C33 105.64(19) . . ? C24 N1 C15 109.14(18) . . ? C24 N1 C16 112.00(17) . . ? C15 N1 C16 108.86(17) . . ? C24 N1 Ti1 110.16(13) . . ? C15 N1 Ti1 109.04(13) . . ? C16 N1 Ti1 107.57(13) . . ? C25 N2 C34 109.45(17) . . ? C25 N2 C26 112.82(17) . . ? C34 N2 C26 108.34(17) . . ? C25 N2 Ti1 108.93(13) . . ? C34 N2 Ti1 108.56(13) . . ? C26 N2 Ti1 108.67(13) . . ? O1 C1 C6 118.1(2) . . ? O1 C1 C2 121.2(2) . . ? C6 C1 C2 120.6(2) . . ? C3 C2 C1 116.6(2) . . ? C3 C2 C7 121.7(2) . . ? C1 C2 C7 121.5(2) . . ? C2 C3 C4 123.6(2) . . ? C2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C5 C4 C3 117.7(2) . . ? C5 C4 C11 121.3(2) . . ? C3 C4 C11 120.9(2) . . ? C4 C5 C6 121.4(2) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.8(2) . . ? C5 C6 C15 120.6(2) . . ? C1 C6 C15 119.6(2) . . ? C9 C7 C10 107.3(2) . . ? C9 C7 C8 109.6(2) . . ? C10 C7 C8 108.3(2) . . ? C9 C7 C2 112.17(19) . . ? C10 C7 C2 111.6(2) . . ? C8 C7 C2 107.76(19) . . ? 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 . . ? O2 C12 C14 114.8(3) . . ? O2 C12 C13 108.4(3) . . ? C14 C12 C13 115.1(3) . . ? O2 C12 H12 105.9 . . ? C14 C12 H12 105.9 . . ? C13 C12 H12 105.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C6 114.82(19) . . ? N1 C15 H15A 108.6 . . ? C6 C15 H15A 108.6 . . ? N1 C15 H15B 108.6 . . ? C6 C15 H15B 108.6 . . ? H15A C15 H15B 107.5 . . ? N1 C16 C17 116.63(19) . . ? N1 C16 H16A 108.1 . . ? C17 C16 H16A 108.1 . . ? N1 C16 H16B 108.1 . . ? C17 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C22 C17 C18 118.9(2) . . ? C22 C17 C16 120.0(2) . . ? C18 C17 C16 121.1(2) . . ? C19 C18 C17 118.0(2) . . ? C19 C18 H18 121.0 . . ? C17 C18 H18 121.0 . . ? C18 C19 C20 121.9(2) . . ? C18 C19 O3 127.8(3) . . ? C20 C19 O3 110.3(2) . . ? C21 C20 C19 121.7(2) . . ? C21 C20 O4 128.5(3) . . ? C19 C20 O4 109.8(3) . . ? C20 C21 C22 117.0(3) . . ? C20 C21 H21 121.5 . . ? C22 C21 H21 121.5 . . ? C21 C22 C17 122.4(2) . . ? C21 C22 H22 118.8 . . ? C17 C22 H22 118.8 . . ? O3 C23 O4 108.1(2) . . ? O3 C23 H23A 110.1 . . ? O4 C23 H23A 110.1 . . ? O3 C23 H23B 110.1 . . ? O4 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? N1 C24 C25 110.58(19) . . ? N1 C24 H24A 109.5 . . ? C25 C24 H24A 109.5 . . ? N1 C24 H24B 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? N2 C25 C24 110.41(18) . . ? N2 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? N2 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? N2 C26 C27 117.51(18) . . ? N2 C26 H26A 107.9 . . ? C27 C26 H26A 107.9 . . ? N2 C26 H26B 107.9 . . ? C27 C26 H26B 107.9 . . ? H26A C26 H26B 107.2 . . ? C32 C27 C28 119.1(2) . . ? C32 C27 C26 121.7(2) . . ? C28 C27 C26 119.2(2) . . ? C29 C28 C27 117.4(2) . . ? C29 C28 H28 121.3 . . ? C27 C28 H28 121.3 . . ? C28 C29 C30 122.5(2) . . ? C28 C29 O7 127.7(2) . . ? C30 C29 O7 109.8(2) . . ? C31 C30 O8 128.2(2) . . ? C31 C30 C29 121.6(2) . . ? O8 C30 C29 110.2(2) . . ? C30 C31 C32 117.0(2) . . ? C30 C31 H31 121.5 . . ? C32 C31 H31 121.5 . . ? C27 C32 C31 122.4(2) . . ? C27 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? O8 C33 O7 108.6(2) . . ? O8 C33 H33A 110.0 . . ? O7 C33 H33A 110.0 . . ? O8 C33 H33B 110.0 . . ? O7 C33 H33B 110.0 . . ? H33A C33 H33B 108.3 . . ? N2 C34 C35 114.72(19) . . ? N2 C34 H34A 108.6 . . ? C35 C34 H34A 108.6 . . ? N2 C34 H34B 108.6 . . ? C35 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? C36 C35 C40 119.8(2) . . ? C36 C35 C34 120.4(2) . . ? C40 C35 C34 119.9(2) . . ? C37 C36 C35 121.6(2) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C36 C37 C38 117.5(2) . . ? C36 C37 C41 121.7(2) . . ? C38 C37 C41 120.8(2) . . ? C37 C38 C39 123.5(2) . . ? C37 C38 H38 118.2 . . ? C39 C38 H38 118.2 . . ? C38 C39 C40 117.0(2) . . ? C38 C39 C42 121.5(2) . . ? C40 C39 C42 121.4(2) . . ? O5 C40 C35 118.6(2) . . ? O5 C40 C39 121.3(2) . . ? C35 C40 C39 120.1(2) . . ? C37 C41 H41A 109.5 . . ? C37 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C37 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C44 107.3(2) . . ? C43 C42 C39 112.1(2) . . ? C44 C42 C39 112.5(2) . . ? C43 C42 C45 108.7(2) . . ? C44 C42 C45 108.2(2) . . ? C39 C42 C45 108.0(2) . . ? 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 . . ? O6 C46 C48 110.4(2) . . ? O6 C46 C47 108.0(2) . . ? C48 C46 C47 112.1(3) . . ? O6 C46 H46 108.7 . . ? C48 C46 H46 108.7 . . ? C47 C46 H46 108.7 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C55 C50 C51 118.7(5) . . ? C55 C50 C49 120.5(5) . . ? C51 C50 C49 120.7(5) . . ? C52 C51 C50 120.9(5) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C51 C52 C53 121.3(5) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? C54 C53 C52 116.3(6) . . ? C54 C53 H53 121.9 . . ? C52 C53 H53 121.9 . . ? C55 C54 C53 122.4(4) . . ? C55 C54 H54 118.8 . . ? C53 C54 H54 118.8 . . ? C50 C55 C54 120.2(5) . . ? C50 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C57 C56 H56A 109.5 . . ? C57 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C57 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C62 117.8(4) . . ? C58 C57 C56 120.6(4) . . ? C62 C57 C56 121.6(4) . . ? C57 C58 C59 121.7(4) . . ? C57 C58 H58 119.2 . . ? C59 C58 H58 119.2 . . ? C58 C59 C60 120.9(4) . . ? C58 C59 H59 119.6 . . ? C60 C59 H59 119.6 . . ? C61 C60 C59 117.2(4) . . ? C61 C60 H60 121.4 . . ? C59 C60 H60 121.4 . . ? C62 C61 C60 120.5(4) . . ? C62 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? C61 C62 C57 121.9(4) . . ? C61 C62 H62 119.1 . . ? C57 C62 H62 119.1 . . ? 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 O6 Ti1 O1 C1 157.3(3) . . . . ? O2 Ti1 O1 C1 -95.0(3) . . . . ? O5 Ti1 O1 C1 34.1(6) . . . . ? N2 Ti1 O1 C1 65.6(3) . . . . ? N1 Ti1 O1 C1 -7.2(3) . . . . ? O6 Ti1 O2 C12 75.4(3) . . . . ? O1 Ti1 O2 C12 -16.9(3) . . . . ? O5 Ti1 O2 C12 170.8(3) . . . . ? N2 Ti1 O2 C12 -128.5(3) . . . . ? N1 Ti1 O2 C12 -96.6(3) . . . . ? O6 Ti1 O5 C40 -81.2(3) . . . . ? O2 Ti1 O5 C40 171.1(3) . . . . ? O1 Ti1 O5 C40 41.7(6) . . . . ? N2 Ti1 O5 C40 9.5(3) . . . . ? N1 Ti1 O5 C40 82.2(3) . . . . ? O2 Ti1 O6 C46 78.4(3) . . . . ? O1 Ti1 O6 C46 174.1(3) . . . . ? O5 Ti1 O6 C46 -14.2(3) . . . . ? N2 Ti1 O6 C46 -93.3(3) . . . . ? N1 Ti1 O6 C46 -128.3(3) . . . . ? O6 Ti1 N1 C24 26.6(3) . . . . ? O2 Ti1 N1 C24 -178.78(14) . . . . ? O1 Ti1 N1 C24 85.64(14) . . . . ? O5 Ti1 N1 C24 -87.80(14) . . . . ? N2 Ti1 N1 C24 -10.11(13) . . . . ? O6 Ti1 N1 C15 -93.1(3) . . . . ? O2 Ti1 N1 C15 61.47(14) . . . . ? O1 Ti1 N1 C15 -34.12(14) . . . . ? O5 Ti1 N1 C15 152.45(14) . . . . ? N2 Ti1 N1 C15 -129.86(14) . . . . ? O6 Ti1 N1 C16 148.9(2) . . . . ? O2 Ti1 N1 C16 -56.44(14) . . . . ? O1 Ti1 N1 C16 -152.03(15) . . . . ? O5 Ti1 N1 C16 34.54(14) . . . . ? N2 Ti1 N1 C16 112.22(14) . . . . ? O6 Ti1 N2 C25 171.41(14) . . . . ? O2 Ti1 N2 C25 14.1(3) . . . . ? O1 Ti1 N2 C25 -97.94(14) . . . . ? O5 Ti1 N2 C25 76.75(14) . . . . ? N1 Ti1 N2 C25 -19.35(13) . . . . ? O6 Ti1 N2 C34 52.31(14) . . . . ? O2 Ti1 N2 C34 -105.0(2) . . . . ? O1 Ti1 N2 C34 142.96(14) . . . . ? O5 Ti1 N2 C34 -42.35(14) . . . . ? N1 Ti1 N2 C34 -138.46(14) . . . . ? O6 Ti1 N2 C26 -65.32(15) . . . . ? O2 Ti1 N2 C26 137.4(2) . . . . ? O1 Ti1 N2 C26 25.33(15) . . . . ? O5 Ti1 N2 C26 -159.97(15) . . . . ? N1 Ti1 N2 C26 103.92(15) . . . . ? Ti1 O1 C1 C6 21.9(4) . . . . ? Ti1 O1 C1 C2 -158.56(19) . . . . ? O1 C1 C2 C3 175.3(2) . . . . ? C6 C1 C2 C3 -5.2(3) . . . . ? O1 C1 C2 C7 -10.8(3) . . . . ? C6 C1 C2 C7 168.7(2) . . . . ? C1 C2 C3 C4 0.4(3) . . . . ? C7 C2 C3 C4 -173.5(2) . . . . ? C2 C3 C4 C5 3.7(4) . . . . ? C2 C3 C4 C11 -175.4(2) . . . . ? C3 C4 C5 C6 -3.1(3) . . . . ? C11 C4 C5 C6 176.0(2) . . . . ? C4 C5 C6 C1 -1.5(4) . . . . ? C4 C5 C6 C15 175.1(2) . . . . ? O1 C1 C6 C5 -174.6(2) . . . . ? C2 C1 C6 C5 5.9(3) . . . . ? O1 C1 C6 C15 8.7(3) . . . . ? C2 C1 C6 C15 -170.8(2) . . . . ? C3 C2 C7 C9 -130.1(2) . . . . ? C1 C2 C7 C9 56.2(3) . . . . ? C3 C2 C7 C10 -9.7(3) . . . . ? C1 C2 C7 C10 176.7(2) . . . . ? C3 C2 C7 C8 109.2(3) . . . . ? C1 C2 C7 C8 -64.4(3) . . . . ? Ti1 O2 C12 C14 -77.2(4) . . . . ? Ti1 O2 C12 C13 152.5(2) . . . . ? C24 N1 C15 C6 -54.9(2) . . . . ? C16 N1 C15 C6 -177.42(19) . . . . ? Ti1 N1 C15 C6 65.5(2) . . . . ? C5 C6 C15 N1 128.1(2) . . . . ? C1 C6 C15 N1 -55.2(3) . . . . ? C24 N1 C16 C17 -70.4(3) . . . . ? C15 N1 C16 C17 50.4(3) . . . . ? Ti1 N1 C16 C17 168.42(16) . . . . ? N1 C16 C17 C22 -98.8(3) . . . . ? N1 C16 C17 C18 81.3(3) . . . . ? C22 C17 C18 C19 2.0(3) . . . . ? C16 C17 C18 C19 -178.0(2) . . . . ? C17 C18 C19 C20 -2.3(4) . . . . ? C17 C18 C19 O3 177.0(2) . . . . ? C23 O3 C19 C18 174.5(3) . . . . ? C23 O3 C19 C20 -6.1(3) . . . . ? C18 C19 C20 C21 1.0(4) . . . . ? O3 C19 C20 C21 -178.4(2) . . . . ? C18 C19 C20 O4 179.9(2) . . . . ? O3 C19 C20 O4 0.5(3) . . . . ? C23 O4 C20 C21 -175.8(3) . . . . ? C23 O4 C20 C19 5.4(3) . . . . ? C19 C20 C21 C22 0.5(4) . . . . ? O4 C20 C21 C22 -178.2(3) . . . . ? C20 C21 C22 C17 -0.7(4) . . . . ? C18 C17 C22 C21 -0.6(4) . . . . ? C16 C17 C22 C21 179.5(2) . . . . ? C19 O3 C23 O4 9.4(3) . . . . ? C20 O4 C23 O3 -9.1(3) . . . . ? C15 N1 C24 C25 158.23(18) . . . . ? C16 N1 C24 C25 -81.2(2) . . . . ? Ti1 N1 C24 C25 38.5(2) . . . . ? C34 N2 C25 C24 165.82(18) . . . . ? C26 N2 C25 C24 -73.5(2) . . . . ? Ti1 N2 C25 C24 47.3(2) . . . . ? N1 C24 C25 N2 -59.0(2) . . . . ? C25 N2 C26 C27 -62.4(3) . . . . ? C34 N2 C26 C27 59.0(3) . . . . ? Ti1 N2 C26 C27 176.72(17) . . . . ? N2 C26 C27 C32 80.4(3) . . . . ? N2 C26 C27 C28 -102.5(2) . . . . ? C32 C27 C28 C29 -0.1(3) . . . . ? C26 C27 C28 C29 -177.3(2) . . . . ? C27 C28 C29 C30 -1.2(3) . . . . ? C27 C28 C29 O7 179.6(2) . . . . ? C33 O7 C29 C28 176.3(2) . . . . ? C33 O7 C29 C30 -3.0(3) . . . . ? C33 O8 C30 C31 -178.3(2) . . . . ? C33 O8 C30 C29 2.4(3) . . . . ? C28 C29 C30 C31 1.6(4) . . . . ? O7 C29 C30 C31 -179.0(2) . . . . ? C28 C29 C30 O8 -178.9(2) . . . . ? O7 C29 C30 O8 0.4(3) . . . . ? O8 C30 C31 C32 179.9(2) . . . . ? C29 C30 C31 C32 -0.7(4) . . . . ? C28 C27 C32 C31 1.0(4) . . . . ? C26 C27 C32 C31 178.1(2) . . . . ? C30 C31 C32 C27 -0.5(4) . . . . ? C30 O8 C33 O7 -4.2(3) . . . . ? C29 O7 C33 O8 4.4(3) . . . . ? C25 N2 C34 C35 -50.7(2) . . . . ? C26 N2 C34 C35 -174.09(19) . . . . ? Ti1 N2 C34 C35 68.1(2) . . . . ? N2 C34 C35 C36 130.2(2) . . . . ? N2 C34 C35 C40 -50.3(3) . . . . ? C40 C35 C36 C37 -0.8(4) . . . . ? C34 C35 C36 C37 178.8(2) . . . . ? C35 C36 C37 C38 -3.7(4) . . . . ? C35 C36 C37 C41 175.6(2) . . . . ? C36 C37 C38 C39 2.5(4) . . . . ? C41 C37 C38 C39 -176.8(2) . . . . ? C37 C38 C39 C40 3.1(4) . . . . ? C37 C38 C39 C42 -173.3(2) . . . . ? Ti1 O5 C40 C35 8.1(4) . . . . ? Ti1 O5 C40 C39 -172.32(19) . . . . ? C36 C35 C40 O5 -173.8(2) . . . . ? C34 C35 C40 O5 6.6(3) . . . . ? C36 C35 C40 C39 6.6(4) . . . . ? C34 C35 C40 C39 -173.0(2) . . . . ? C38 C39 C40 O5 172.9(2) . . . . ? C42 C39 C40 O5 -10.8(4) . . . . ? C38 C39 C40 C35 -7.6(3) . . . . ? C42 C39 C40 C35 168.8(2) . . . . ? C38 C39 C42 C43 -7.5(3) . . . . ? C40 C39 C42 C43 176.3(2) . . . . ? C38 C39 C42 C44 -128.6(3) . . . . ? C40 C39 C42 C44 55.2(3) . . . . ? C38 C39 C42 C45 112.1(3) . . . . ? C40 C39 C42 C45 -64.1(3) . . . . ? Ti1 O6 C46 C48 -86.3(3) . . . . ? Ti1 O6 C46 C47 150.8(2) . . . . ? C55 C50 C51 C52 2.0(7) . . . . ? C49 C50 C51 C52 178.1(5) . . . . ? C50 C51 C52 C53 -4.7(8) . . . . ? C51 C52 C53 C54 5.5(8) . . . . ? C52 C53 C54 C55 -3.9(7) . . . . ? C51 C50 C55 C54 -0.4(7) . . . . ? C49 C50 C55 C54 -176.4(4) . . . . ? C53 C54 C55 C50 1.4(7) . . . . ? C62 C57 C58 C59 2.2(6) . . . . ? C56 C57 C58 C59 -177.1(4) . . . . ? C57 C58 C59 C60 -1.0(7) . . . . ? C58 C59 C60 C61 -1.0(6) . . . . ? C59 C60 C61 C62 1.6(6) . . . . ? C60 C61 C62 C57 -0.4(6) . . . . ? C58 C57 C62 C61 -1.5(5) . . . . ? C56 C57 C62 C61 177.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.671 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.049 #===END data_pg212 _database_code_depnum_ccdc_archive 'CCDC 690057' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H84 N2 O8 Ti' _chemical_formula_weight 1021.20 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.743(4) _cell_length_b 18.552(4) _cell_length_c 16.993(4) _cell_angle_alpha 90.000(17) _cell_angle_beta 113.19(2) _cell_angle_gamma 90.000(17) _cell_volume 5721(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1859 _cell_measurement_theta_min 2.9812 _cell_measurement_theta_max 32.7854 _exptl_crystal_description block _exptl_crystal_colour yello _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 0.204 _exptl_absorpt_correction_T_min 0.9377 _exptl_absorpt_correction_T_max 0.9527 _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 28748 _diffrn_reflns_av_R_equivalents 0.0997 _diffrn_reflns_av_sigmaI/netI 0.1350 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9986 _reflns_number_gt 5157 _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^)+(0.0572P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9986 _refine_ls_number_parameters 666 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1315 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1324 _refine_ls_wR_factor_gt 0.1112 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _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 0.25645(3) 0.04972(3) 0.74670(4) 0.02106(16) Uani 1 1 d . . . O1 O 0.18250(11) 0.03296(11) 0.79080(12) 0.0238(5) Uani 1 1 d . . . O2 O 0.33174(11) 0.04304(11) 0.70312(13) 0.0246(5) Uani 1 1 d . . . O3 O 0.30700(12) 0.10657(11) 0.83656(13) 0.0303(6) Uani 1 1 d . . . O4 O 0.20192(12) 0.10902(11) 0.66039(13) 0.0288(5) Uani 1 1 d . . . O5 O 0.06024(15) -0.22837(15) 0.30202(16) 0.0573(8) Uani 1 1 d . . . O6 O 0.16230(15) -0.27668(14) 0.41181(19) 0.0648(9) Uani 1 1 d . . . O7 O 0.37126(14) -0.30746(13) 1.03507(16) 0.0500(7) Uani 1 1 d . . . O8 O 0.46360(14) -0.26200(14) 1.15709(15) 0.0481(7) Uani 1 1 d . . . N1 N 0.19526(13) -0.05043(13) 0.66035(15) 0.0202(6) Uani 1 1 d . . . N2 N 0.32110(13) -0.05400(13) 0.82301(15) 0.0208(6) Uani 1 1 d . . . C1 C 0.11672(17) 0.00241(17) 0.77341(19) 0.0219(8) Uani 1 1 d . . . C2 C 0.07968(17) 0.01340(17) 0.82962(19) 0.0240(8) Uani 1 1 d . . . C3 C 0.01263(19) -0.02236(17) 0.8100(2) 0.0285(8) Uani 1 1 d . . . H3 H -0.0117 -0.0163 0.8479 0.034 Uiso 1 1 calc R . . C4 C -0.02121(18) -0.06666(17) 0.7379(2) 0.0272(8) Uani 1 1 d . . . C5 C 0.01559(18) -0.07321(16) 0.6838(2) 0.0244(8) Uani 1 1 d . . . H5 H -0.0057 -0.1022 0.6340 0.029 Uiso 1 1 calc R . . C6 C 0.08241(17) -0.03926(16) 0.69900(19) 0.0206(7) Uani 1 1 d . . . C7 C 0.10925(18) 0.06718(18) 0.9053(2) 0.0270(8) Uani 1 1 d . . . C8 C 0.1880(2) 0.0486(2) 0.9670(2) 0.0490(11) Uani 1 1 d . . . H8A H 0.1897 -0.0014 0.9863 0.073 Uiso 1 1 calc R . . H8B H 0.2032 0.0810 1.0165 0.073 Uiso 1 1 calc R . . H8C H 0.2215 0.0543 0.9375 0.073 Uiso 1 1 calc R . . C9 C 0.1088(2) 0.14347(18) 0.8685(2) 0.0444(10) Uani 1 1 d . . . H9A H 0.1390 0.1436 0.8345 0.067 Uiso 1 1 calc R . . H9B H 0.1291 0.1780 0.9157 0.067 Uiso 1 1 calc R . . H9C H 0.0581 0.1571 0.8322 0.067 Uiso 1 1 calc R . . C10 C 0.0611(2) 0.0687(2) 0.9569(2) 0.0544(12) Uani 1 1 d . . . H10A H 0.0111 0.0837 0.9198 0.082 Uiso 1 1 calc R . . H10B H 0.0818 0.1029 1.0044 0.082 Uiso 1 1 calc R . . H10C H 0.0595 0.0205 0.9797 0.082 Uiso 1 1 calc R . . C11 C -0.0949(2) -0.1032(2) 0.7222(2) 0.0406(10) Uani 1 1 d . . . C12 C -0.1529(2) -0.0457(2) 0.7183(3) 0.0583(12) Uani 1 1 d . . . H12A H -0.1376 -0.0214 0.7738 0.087 Uiso 1 1 calc R . . H12B H -0.2007 -0.0691 0.7048 0.087 Uiso 1 1 calc R . . H12C H -0.1573 -0.0103 0.6738 0.087 Uiso 1 1 calc R . . C13 C -0.0859(3) -0.1546(2) 0.7968(3) 0.0649(14) Uani 1 1 d . . . H13A H -0.0531 -0.1944 0.7971 0.097 Uiso 1 1 calc R . . H13B H -0.1341 -0.1740 0.7896 0.097 Uiso 1 1 calc R . . H13C H -0.0647 -0.1283 0.8511 0.097 Uiso 1 1 calc R . . C14 C -0.1256(2) -0.1452(2) 0.6386(3) 0.0602(13) Uani 1 1 d . . . H14A H -0.1335 -0.1123 0.5906 0.090 Uiso 1 1 calc R . . H14B H -0.1725 -0.1675 0.6321 0.090 Uiso 1 1 calc R . . H14C H -0.0904 -0.1827 0.6393 0.090 Uiso 1 1 calc R . . C15 C 0.11374(16) -0.04215(17) 0.63073(18) 0.0219(7) Uani 1 1 d . . . H15A H 0.0901 -0.0828 0.5919 0.026 Uiso 1 1 calc R . . H15B H 0.0992 0.0026 0.5965 0.026 Uiso 1 1 calc R . . C16 C 0.21927(18) -0.11805(16) 0.7105(2) 0.0243(8) Uani 1 1 d . . . H16A H 0.2074 -0.1597 0.6709 0.029 Uiso 1 1 calc R . . H16B H 0.1921 -0.1239 0.7481 0.029 Uiso 1 1 calc R . . C17 C 0.30112(17) -0.11713(17) 0.7644(2) 0.0247(8) Uani 1 1 d . . . H17A H 0.3153 -0.1621 0.7983 0.030 Uiso 1 1 calc R . . H17B H 0.3285 -0.1150 0.7266 0.030 Uiso 1 1 calc R . . C18 C 0.21435(17) -0.04874(17) 0.58318(19) 0.0253(8) Uani 1 1 d . . . H18A H 0.2670 -0.0618 0.6019 0.030 Uiso 1 1 calc R . . H18B H 0.2090 0.0016 0.5622 0.030 Uiso 1 1 calc R . . C19 C 0.17041(18) -0.09674(17) 0.5084(2) 0.0250(8) Uani 1 1 d . . . C20 C 0.19182(18) -0.16770(19) 0.5034(2) 0.0344(9) Uani 1 1 d . . . H20 H 0.2332 -0.1883 0.5481 0.041 Uiso 1 1 calc R . . C21 C 0.1512(2) -0.2066(2) 0.4319(2) 0.0412(10) Uani 1 1 d . . . C22 C 0.1086(3) -0.2876(3) 0.3280(4) 0.113(2) Uani 1 1 d . . . H22A H 0.1332 -0.2941 0.2878 0.135 Uiso 1 1 calc R . . H22B H 0.0803 -0.3319 0.3267 0.135 Uiso 1 1 calc R . . C23 C 0.0910(2) -0.1779(2) 0.3666(2) 0.0392(10) Uani 1 1 d . . . C24 C 0.0686(2) -0.1085(2) 0.3679(2) 0.0369(9) Uani 1 1 d . . . H24 H 0.0274 -0.0886 0.3222 0.044 Uiso 1 1 calc R . . C25 C 0.1101(2) -0.06867(18) 0.4407(2) 0.0307(9) Uani 1 1 d . . . H25 H 0.0964 -0.0201 0.4442 0.037 Uiso 1 1 calc R . . C26 C 0.30184(18) -0.06392(17) 0.8996(2) 0.0268(8) Uani 1 1 d . . . H26A H 0.2499 -0.0801 0.8787 0.032 Uiso 1 1 calc R . . H26B H 0.3044 -0.0161 0.9265 0.032 Uiso 1 1 calc R . . C27 C 0.34800(18) -0.11600(18) 0.9690(2) 0.0253(8) Uani 1 1 d . . . C28 C 0.40212(19) -0.08975(19) 1.0428(2) 0.0320(9) Uani 1 1 d . . . H28 H 0.4107 -0.0392 1.0478 0.038 Uiso 1 1 calc R . . C29 C 0.4451(2) -0.1341(2) 1.1107(2) 0.0376(9) Uani 1 1 d . . . H29 H 0.4816 -0.1151 1.1616 0.045 Uiso 1 1 calc R . . C30 C 0.43136(19) -0.20644(19) 1.0994(2) 0.0321(9) Uani 1 1 d . . . C31 C 0.4314(2) -0.3258(2) 1.1113(2) 0.0543(12) Uani 1 1 d . . . H31A H 0.4685 -0.3529 1.0975 0.065 Uiso 1 1 calc R . . H31B H 0.4143 -0.3570 1.1471 0.065 Uiso 1 1 calc R . . C32 C 0.37629(19) -0.23368(19) 1.0266(2) 0.0320(9) Uani 1 1 d . . . C33 C 0.33349(18) -0.18991(18) 0.9610(2) 0.0291(8) Uani 1 1 d . . . H33 H 0.2952 -0.2092 0.9117 0.035 Uiso 1 1 calc R . . C34 C 0.40279(16) -0.04091(17) 0.85549(19) 0.0232(7) Uani 1 1 d . . . H34A H 0.4281 -0.0831 0.8902 0.028 Uiso 1 1 calc R . . H34B H 0.4146 0.0012 0.8944 0.028 Uiso 1 1 calc R . . C35 C 0.43516(17) -0.02764(16) 0.78980(18) 0.0199(7) Uani 1 1 d . . . C36 C 0.40006(17) 0.01858(16) 0.71977(19) 0.0211(7) Uani 1 1 d . . . C37 C 0.43823(17) 0.03914(17) 0.66789(19) 0.0227(7) Uani 1 1 d . . . C38 C 0.50827(17) 0.00950(17) 0.6871(2) 0.0258(8) Uani 1 1 d . . . H38 H 0.5341 0.0233 0.6527 0.031 Uiso 1 1 calc R . . C39 C 0.54243(17) -0.03929(17) 0.7540(2) 0.0255(8) Uani 1 1 d . . . C40 C 0.50394(17) -0.05657(16) 0.8042(2) 0.0238(8) Uani 1 1 d . . . H40 H 0.5254 -0.0894 0.8503 0.029 Uiso 1 1 calc R . . C41 C 0.40602(19) 0.09635(19) 0.5965(2) 0.0317(9) Uani 1 1 d . . . C42 C 0.3323(2) 0.0722(2) 0.5287(2) 0.0471(11) Uani 1 1 d . . . H42A H 0.3378 0.0245 0.5071 0.071 Uiso 1 1 calc R . . H42B H 0.3160 0.1069 0.4814 0.071 Uiso 1 1 calc R . . H42C H 0.2955 0.0696 0.5541 0.071 Uiso 1 1 calc R . . C43 C 0.3965(2) 0.16732(19) 0.6364(2) 0.0445(10) Uani 1 1 d . . . H43A H 0.3649 0.1596 0.6680 0.067 Uiso 1 1 calc R . . H43B H 0.3736 0.2030 0.5911 0.067 Uiso 1 1 calc R . . H43C H 0.4448 0.1850 0.6757 0.067 Uiso 1 1 calc R . . C44 C 0.4585(2) 0.1113(2) 0.5515(2) 0.0432(10) Uani 1 1 d . . . H44A H 0.5060 0.1281 0.5936 0.065 Uiso 1 1 calc R . . H44B H 0.4371 0.1485 0.5077 0.065 Uiso 1 1 calc R . . H44C H 0.4658 0.0670 0.5245 0.065 Uiso 1 1 calc R . . C45 C 0.61966(18) -0.06863(18) 0.7717(2) 0.0295(8) Uani 1 1 d . . . C46 C 0.67619(19) -0.0093(2) 0.8100(3) 0.0525(11) Uani 1 1 d . . . H46A H 0.6733 0.0082 0.8630 0.079 Uiso 1 1 calc R . . H46B H 0.6661 0.0306 0.7690 0.079 Uiso 1 1 calc R . . H46C H 0.7257 -0.0283 0.8225 0.079 Uiso 1 1 calc R . . C47 C 0.6269(2) -0.0926(3) 0.6897(3) 0.103(2) Uani 1 1 d . . . H47A H 0.6761 -0.1128 0.7035 0.154 Uiso 1 1 calc R . . H47B H 0.6195 -0.0511 0.6515 0.154 Uiso 1 1 calc R . . H47C H 0.5897 -0.1294 0.6612 0.154 Uiso 1 1 calc R . . C48 C 0.6400(2) -0.1307(2) 0.8335(4) 0.101(2) Uani 1 1 d . . . H48A H 0.6908 -0.1455 0.8459 0.152 Uiso 1 1 calc R . . H48B H 0.6066 -0.1712 0.8083 0.152 Uiso 1 1 calc R . . H48C H 0.6357 -0.1158 0.8868 0.152 Uiso 1 1 calc R . . C49 C 0.3534(2) 0.1667(2) 0.8697(3) 0.0532(12) Uani 1 1 d . . . H49 H 0.3822 0.1759 0.8337 0.064 Uiso 1 1 calc R . . C50 C 0.4061(2) 0.1531(2) 0.9605(2) 0.0569(12) Uani 1 1 d . . . H50A H 0.3784 0.1486 0.9971 0.085 Uiso 1 1 calc R . . H50B H 0.4407 0.1934 0.9804 0.085 Uiso 1 1 calc R . . H50C H 0.4333 0.1084 0.9630 0.085 Uiso 1 1 calc R . . C51 C 0.3052(4) 0.2313(2) 0.8646(3) 0.132(3) Uani 1 1 d . . . H51A H 0.2712 0.2389 0.8050 0.198 Uiso 1 1 calc R . . H51B H 0.3361 0.2741 0.8855 0.198 Uiso 1 1 calc R . . H51C H 0.2769 0.2227 0.8999 0.198 Uiso 1 1 calc R . . C52 C 0.15978(18) 0.17352(17) 0.6412(2) 0.0299(8) Uani 1 1 d . . . H52 H 0.1586 0.1933 0.6954 0.036 Uiso 1 1 calc R . . C53 C 0.1967(2) 0.22771(19) 0.6049(3) 0.0520(11) Uani 1 1 d . . . H53A H 0.2463 0.2381 0.6474 0.078 Uiso 1 1 calc R . . H53B H 0.1677 0.2722 0.5906 0.078 Uiso 1 1 calc R . . H53C H 0.2002 0.2080 0.5531 0.078 Uiso 1 1 calc R . . C54 C 0.0822(2) 0.1578(2) 0.5800(3) 0.0663(13) Uani 1 1 d . . . H54A H 0.0827 0.1386 0.5265 0.099 Uiso 1 1 calc R . . H54B H 0.0532 0.2024 0.5681 0.099 Uiso 1 1 calc R . . H54C H 0.0602 0.1223 0.6056 0.099 Uiso 1 1 calc R . . C55 C 0.1409(3) 0.6485(4) 0.5839(4) 0.121(2) Uani 1 1 d . . . H55A H 0.1056 0.6869 0.5798 0.182 Uiso 1 1 calc R . . H55B H 0.1181 0.6015 0.5835 0.182 Uiso 1 1 calc R . . H55C H 0.1553 0.6517 0.5350 0.182 Uiso 1 1 calc R . . C56 C 0.2080(3) 0.6569(2) 0.6657(4) 0.0661(13) Uani 1 1 d . . . C57 C 0.2020(3) 0.6430(3) 0.7428(4) 0.0797(17) Uani 1 1 d . . . H57 H 0.1560 0.6288 0.7435 0.096 Uiso 1 1 calc R . . C58 C 0.2615(4) 0.6496(3) 0.8169(4) 0.0874(19) Uani 1 1 d . . . H58 H 0.2571 0.6393 0.8694 0.105 Uiso 1 1 calc R . . C59 C 0.3282(3) 0.6709(3) 0.8178(4) 0.0775(16) Uani 1 1 d . . . H59 H 0.3698 0.6752 0.8704 0.093 Uiso 1 1 calc R . . C60 C 0.3340(3) 0.6860(2) 0.7417(4) 0.0646(14) Uani 1 1 d . . . H60 H 0.3796 0.7018 0.7411 0.078 Uiso 1 1 calc R . . C61 C 0.2737(3) 0.6783(2) 0.6667(3) 0.0547(12) Uani 1 1 d . . . H61 H 0.2781 0.6881 0.6141 0.066 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 0.0160(3) 0.0200(3) 0.0213(3) 0.0003(3) 0.0010(2) 0.0011(3) O1 0.0196(12) 0.0300(14) 0.0203(12) -0.0057(10) 0.0061(10) -0.0029(11) O2 0.0166(12) 0.0278(13) 0.0247(12) 0.0070(10) 0.0030(10) 0.0019(11) O3 0.0294(14) 0.0271(14) 0.0277(13) -0.0091(11) 0.0042(11) -0.0074(12) O4 0.0243(13) 0.0238(13) 0.0311(13) 0.0065(11) 0.0032(11) 0.0066(11) O5 0.0396(17) 0.065(2) 0.0564(18) -0.0380(16) 0.0068(14) -0.0033(16) O6 0.0442(18) 0.0500(19) 0.079(2) -0.0406(16) 0.0013(16) 0.0123(15) O7 0.0451(18) 0.0336(16) 0.0500(17) 0.0175(13) -0.0041(14) 0.0036(13) O8 0.0460(18) 0.0439(17) 0.0379(16) 0.0146(14) -0.0013(13) 0.0081(14) N1 0.0181(14) 0.0204(15) 0.0171(14) 0.0001(12) 0.0017(11) 0.0004(13) N2 0.0166(14) 0.0229(16) 0.0219(15) 0.0015(12) 0.0067(12) 0.0012(13) C1 0.0167(18) 0.0239(19) 0.0211(19) 0.0076(15) 0.0032(15) 0.0068(15) C2 0.0234(19) 0.0259(19) 0.0200(18) 0.0043(15) 0.0055(15) 0.0035(16) C3 0.031(2) 0.032(2) 0.031(2) 0.0031(17) 0.0216(17) 0.0019(17) C4 0.026(2) 0.022(2) 0.034(2) 0.0026(16) 0.0127(17) 0.0022(16) C5 0.0256(19) 0.0177(18) 0.0257(19) 0.0004(15) 0.0055(16) 0.0000(15) C6 0.0205(17) 0.0214(18) 0.0182(17) 0.0039(15) 0.0057(14) 0.0040(15) C7 0.0258(19) 0.035(2) 0.0196(18) -0.0070(16) 0.0083(15) -0.0004(16) C8 0.045(2) 0.060(3) 0.027(2) -0.016(2) -0.0015(18) 0.010(2) C9 0.051(3) 0.034(2) 0.040(2) -0.0111(19) 0.009(2) 0.000(2) C10 0.055(3) 0.075(3) 0.046(3) -0.026(2) 0.034(2) -0.016(2) C11 0.038(2) 0.035(2) 0.057(3) -0.009(2) 0.027(2) -0.0131(19) C12 0.036(2) 0.061(3) 0.091(3) -0.013(3) 0.038(2) -0.016(2) C13 0.079(4) 0.053(3) 0.082(3) 0.007(3) 0.052(3) -0.024(3) C14 0.052(3) 0.059(3) 0.076(3) -0.030(2) 0.033(3) -0.037(2) C15 0.0164(17) 0.0286(19) 0.0176(18) -0.0007(15) 0.0033(14) -0.0022(16) C16 0.0251(19) 0.0203(18) 0.0238(18) -0.0034(15) 0.0058(15) -0.0058(16) C17 0.0229(19) 0.0212(19) 0.0280(19) 0.0006(16) 0.0080(15) 0.0033(16) C18 0.0230(18) 0.0286(19) 0.0239(18) -0.0018(16) 0.0091(15) -0.0025(17) C19 0.0253(19) 0.026(2) 0.029(2) -0.0072(16) 0.0161(16) -0.0046(16) C20 0.021(2) 0.038(2) 0.039(2) -0.0093(18) 0.0076(17) 0.0031(18) C21 0.029(2) 0.038(2) 0.050(3) -0.020(2) 0.008(2) 0.0034(19) C22 0.058(4) 0.087(4) 0.134(5) -0.081(4) -0.025(3) 0.023(3) C23 0.029(2) 0.051(3) 0.036(2) -0.024(2) 0.0104(18) -0.006(2) C24 0.034(2) 0.047(3) 0.029(2) -0.0032(19) 0.0112(17) 0.002(2) C25 0.040(2) 0.026(2) 0.0232(19) -0.0022(16) 0.0096(17) 0.0001(17) C26 0.0266(19) 0.027(2) 0.0278(19) 0.0018(16) 0.0112(16) 0.0027(16) C27 0.0231(19) 0.031(2) 0.0230(19) 0.0043(16) 0.0099(15) 0.0062(16) C28 0.042(2) 0.031(2) 0.025(2) 0.0032(17) 0.0147(18) 0.0021(18) C29 0.036(2) 0.049(3) 0.020(2) 0.0013(18) 0.0029(17) -0.002(2) C30 0.029(2) 0.034(2) 0.030(2) 0.0156(18) 0.0092(17) 0.0082(18) C31 0.045(3) 0.044(3) 0.054(3) 0.021(2) -0.003(2) 0.008(2) C32 0.027(2) 0.028(2) 0.040(2) 0.0110(18) 0.0116(18) 0.0013(17) C33 0.0238(19) 0.031(2) 0.028(2) 0.0029(16) 0.0050(16) -0.0005(17) C34 0.0198(17) 0.0255(19) 0.0200(18) 0.0033(15) 0.0033(14) 0.0035(16) C35 0.0180(17) 0.0244(19) 0.0142(17) -0.0016(14) 0.0030(14) 0.0021(15) C36 0.0156(17) 0.0220(19) 0.0214(19) -0.0058(15) 0.0026(14) -0.0029(15) C37 0.0234(18) 0.0271(19) 0.0168(17) -0.0046(15) 0.0071(14) -0.0048(16) C38 0.0214(19) 0.034(2) 0.0224(19) -0.0062(16) 0.0087(15) -0.0047(17) C39 0.0188(17) 0.0230(19) 0.0288(19) -0.0110(16) 0.0029(15) -0.0062(16) C40 0.0180(17) 0.0227(19) 0.0225(18) -0.0041(15) -0.0010(14) 0.0004(16) C41 0.026(2) 0.040(2) 0.025(2) 0.0069(17) 0.0064(16) -0.0042(18) C42 0.034(2) 0.064(3) 0.031(2) 0.017(2) 0.0001(18) -0.012(2) C43 0.057(3) 0.040(2) 0.044(2) 0.012(2) 0.027(2) 0.007(2) C44 0.035(2) 0.057(3) 0.039(2) 0.012(2) 0.0156(19) -0.002(2) C45 0.0211(19) 0.036(2) 0.032(2) -0.0050(17) 0.0108(16) 0.0019(16) C46 0.018(2) 0.052(3) 0.075(3) -0.006(2) 0.005(2) 0.000(2) C47 0.034(3) 0.204(6) 0.060(3) -0.062(4) 0.009(2) 0.032(3) C48 0.049(3) 0.057(3) 0.222(7) 0.075(4) 0.079(4) 0.039(3) C49 0.052(3) 0.057(3) 0.043(3) -0.012(2) 0.011(2) -0.028(2) C50 0.045(3) 0.059(3) 0.044(3) -0.019(2) -0.007(2) -0.003(2) C51 0.142(6) 0.035(3) 0.110(5) -0.019(3) -0.068(4) 0.015(4) C52 0.027(2) 0.026(2) 0.032(2) 0.0055(16) 0.0064(16) 0.0101(17) C53 0.054(3) 0.030(2) 0.073(3) 0.017(2) 0.026(2) 0.006(2) C54 0.026(2) 0.054(3) 0.098(4) 0.013(3) 0.001(2) 0.018(2) C55 0.084(5) 0.138(6) 0.140(6) -0.020(5) 0.044(5) -0.031(4) C56 0.071(4) 0.048(3) 0.091(4) -0.008(3) 0.044(3) -0.011(3) C57 0.095(5) 0.065(4) 0.113(5) -0.012(4) 0.078(4) -0.016(3) C58 0.128(6) 0.068(4) 0.102(5) -0.001(4) 0.084(5) 0.012(4) C59 0.089(4) 0.066(4) 0.082(4) -0.012(3) 0.039(3) 0.034(3) C60 0.069(4) 0.045(3) 0.094(4) -0.007(3) 0.048(3) 0.007(3) C61 0.070(3) 0.032(2) 0.079(4) 0.004(2) 0.049(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O3 1.800(2) . ? Ti1 O4 1.810(2) . ? Ti1 O2 1.908(2) . ? Ti1 O1 1.911(2) . ? Ti1 N1 2.381(3) . ? Ti1 N2 2.390(3) . ? O1 C1 1.339(4) . ? O2 C36 1.343(3) . ? O3 C49 1.412(4) . ? O4 C52 1.420(4) . ? O5 C23 1.388(4) . ? O5 C22 1.408(5) . ? O6 C21 1.384(4) . ? O6 C22 1.415(5) . ? O7 C32 1.384(4) . ? O7 C31 1.411(4) . ? O8 C30 1.392(4) . ? O8 C31 1.422(4) . ? N1 C16 1.485(4) . ? N1 C15 1.493(4) . ? N1 C18 1.501(4) . ? N2 C17 1.487(4) . ? N2 C26 1.504(4) . ? N2 C34 1.505(4) . ? C1 C6 1.407(4) . ? C1 C2 1.428(4) . ? C2 C3 1.399(4) . ? C2 C7 1.549(4) . ? C3 C4 1.406(4) . ? C3 H3 0.9500 . ? C4 C5 1.383(4) . ? C4 C11 1.529(5) . ? C5 C6 1.391(4) . ? C5 H5 0.9500 . ? C6 C15 1.515(4) . ? C7 C10 1.527(5) . ? C7 C8 1.534(5) . ? C7 C9 1.546(5) . ? 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 C14 1.522(5) . ? C11 C13 1.540(5) . ? C11 C12 1.548(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.512(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.514(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C25 1.391(4) . ? C19 C20 1.395(4) . ? C20 C21 1.367(5) . ? C20 H20 0.9500 . ? C21 C23 1.374(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.364(5) . ? C24 C25 1.397(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.520(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.376(4) . ? C27 C33 1.397(4) . ? C28 C29 1.399(5) . ? C28 H28 0.9500 . ? C29 C30 1.367(5) . ? C29 H29 0.9500 . ? C30 C32 1.381(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.369(4) . ? C33 H33 0.9500 . ? C34 C35 1.509(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C40 1.389(4) . ? C35 C36 1.408(4) . ? C36 C37 1.419(4) . ? C37 C38 1.402(4) . ? C37 C41 1.547(4) . ? C38 C39 1.401(4) . ? C38 H38 0.9500 . ? C39 C40 1.385(4) . ? C39 C45 1.533(4) . ? C40 H40 0.9500 . ? C41 C42 1.526(5) . ? C41 C43 1.526(5) . ? C41 C44 1.535(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C48 1.502(5) . ? C45 C46 1.520(5) . ? C45 C47 1.524(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.503(5) . ? C49 C51 1.512(6) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C54 1.502(5) . ? C52 C53 1.509(5) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.504(7) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C61 1.350(6) . ? C56 C57 1.386(6) . ? C57 C58 1.346(7) . ? C57 H57 0.9500 . ? C58 C59 1.368(7) . ? C58 H58 0.9500 . ? C59 C60 1.373(6) . ? C59 H59 0.9500 . ? C60 C61 1.366(6) . ? C60 H60 0.9500 . ? C61 H61 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 O3 Ti1 O4 106.58(10) . . ? O3 Ti1 O2 96.37(10) . . ? O4 Ti1 O2 91.76(9) . . ? O3 Ti1 O1 90.96(9) . . ? O4 Ti1 O1 96.55(10) . . ? O2 Ti1 O1 166.90(9) . . ? O3 Ti1 N1 163.21(9) . . ? O4 Ti1 N1 88.82(9) . . ? O2 Ti1 N1 89.65(9) . . ? O1 Ti1 N1 80.45(9) . . ? O3 Ti1 N2 90.70(10) . . ? O4 Ti1 N2 161.66(9) . . ? O2 Ti1 N2 80.04(8) . . ? O1 Ti1 N2 89.05(9) . . ? N1 Ti1 N2 74.87(8) . . ? C1 O1 Ti1 143.8(2) . . ? C36 O2 Ti1 144.2(2) . . ? C49 O3 Ti1 149.0(2) . . ? C52 O4 Ti1 143.7(2) . . ? C23 O5 C22 104.3(3) . . ? C21 O6 C22 104.7(3) . . ? C32 O7 C31 105.4(3) . . ? C30 O8 C31 104.4(3) . . ? C16 N1 C15 109.8(2) . . ? C16 N1 C18 112.7(2) . . ? C15 N1 C18 108.2(2) . . ? C16 N1 Ti1 109.62(17) . . ? C15 N1 Ti1 110.21(18) . . ? C18 N1 Ti1 106.33(17) . . ? C17 N2 C26 113.1(2) . . ? C17 N2 C34 109.6(2) . . ? C26 N2 C34 107.6(2) . . ? C17 N2 Ti1 109.07(17) . . ? C26 N2 Ti1 107.76(17) . . ? C34 N2 Ti1 109.60(17) . . ? O1 C1 C6 120.8(3) . . ? O1 C1 C2 120.0(3) . . ? C6 C1 C2 119.2(3) . . ? C3 C2 C1 117.3(3) . . ? C3 C2 C7 121.0(3) . . ? C1 C2 C7 121.5(3) . . ? C2 C3 C4 124.4(3) . . ? C2 C3 H3 117.8 . . ? C4 C3 H3 117.8 . . ? C5 C4 C3 115.9(3) . . ? C5 C4 C11 123.9(3) . . ? C3 C4 C11 120.2(3) . . ? C4 C5 C6 123.0(3) . . ? C4 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C5 C6 C1 120.1(3) . . ? C5 C6 C15 119.0(3) . . ? C1 C6 C15 120.7(3) . . ? C10 C7 C8 107.8(3) . . ? C10 C7 C9 108.0(3) . . ? C8 C7 C9 108.9(3) . . ? C10 C7 C2 111.9(3) . . ? C8 C7 C2 111.8(3) . . ? C9 C7 C2 108.3(3) . . ? 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 . . ? C14 C11 C4 113.0(3) . . ? C14 C11 C13 109.0(3) . . ? C4 C11 C13 109.7(3) . . ? C14 C11 C12 107.3(3) . . ? C4 C11 C12 109.9(3) . . ? C13 C11 C12 107.8(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C6 117.1(2) . . ? N1 C15 H15A 108.0 . . ? C6 C15 H15A 108.0 . . ? N1 C15 H15B 108.0 . . ? C6 C15 H15B 108.0 . . ? H15A C15 H15B 107.3 . . ? N1 C16 C17 111.2(2) . . ? N1 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? N1 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N2 C17 C16 110.7(2) . . ? N2 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? N1 C18 C19 117.6(3) . . ? N1 C18 H18A 107.9 . . ? C19 C18 H18A 107.9 . . ? N1 C18 H18B 107.9 . . ? C19 C18 H18B 107.9 . . ? H18A C18 H18B 107.2 . . ? C25 C19 C20 119.0(3) . . ? C25 C19 C18 119.7(3) . . ? C20 C19 C18 121.3(3) . . ? C21 C20 C19 117.8(3) . . ? C21 C20 H20 121.1 . . ? C19 C20 H20 121.1 . . ? C20 C21 C23 122.1(3) . . ? C20 C21 O6 128.3(4) . . ? C23 C21 O6 109.6(3) . . ? O5 C22 O6 110.6(3) . . ? O5 C22 H22A 109.5 . . ? O6 C22 H22A 109.5 . . ? O5 C22 H22B 109.5 . . ? O6 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C21 122.4(3) . . ? C24 C23 O5 127.3(4) . . ? C21 C23 O5 110.3(3) . . ? C23 C24 C25 115.7(3) . . ? C23 C24 H24 122.2 . . ? C25 C24 H24 122.2 . . ? C19 C25 C24 123.1(3) . . ? C19 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? N2 C26 C27 118.1(3) . . ? N2 C26 H26A 107.8 . . ? C27 C26 H26A 107.8 . . ? N2 C26 H26B 107.8 . . ? C27 C26 H26B 107.8 . . ? H26A C26 H26B 107.1 . . ? C28 C27 C33 119.5(3) . . ? C28 C27 C26 119.7(3) . . ? C33 C27 C26 120.7(3) . . ? C27 C28 C29 122.9(3) . . ? C27 C28 H28 118.5 . . ? C29 C28 H28 118.5 . . ? C30 C29 C28 116.1(3) . . ? C30 C29 H29 122.0 . . ? C28 C29 H29 122.0 . . ? C29 C30 C32 121.8(3) . . ? C29 C30 O8 128.1(3) . . ? C32 C30 O8 109.9(3) . . ? O7 C31 O8 109.6(3) . . ? O7 C31 H31A 109.8 . . ? O8 C31 H31A 109.8 . . ? O7 C31 H31B 109.8 . . ? O8 C31 H31B 109.8 . . ? H31A C31 H31B 108.2 . . ? C33 C32 C30 121.9(3) . . ? C33 C32 O7 128.7(3) . . ? C30 C32 O7 109.4(3) . . ? C32 C33 C27 117.8(3) . . ? C32 C33 H33 121.1 . . ? C27 C33 H33 121.1 . . ? N2 C34 C35 117.4(2) . . ? N2 C34 H34A 108.0 . . ? C35 C34 H34A 108.0 . . ? N2 C34 H34B 108.0 . . ? C35 C34 H34B 108.0 . . ? H34A C34 H34B 107.2 . . ? C40 C35 C36 120.4(3) . . ? C40 C35 C34 118.4(3) . . ? C36 C35 C34 120.9(3) . . ? O2 C36 C35 120.2(3) . . ? O2 C36 C37 120.9(3) . . ? C35 C36 C37 118.9(3) . . ? C38 C37 C36 117.8(3) . . ? C38 C37 C41 121.0(3) . . ? C36 C37 C41 121.1(3) . . ? C39 C38 C37 123.9(3) . . ? C39 C38 H38 118.1 . . ? C37 C38 H38 118.1 . . ? C40 C39 C38 116.3(3) . . ? C40 C39 C45 122.8(3) . . ? C38 C39 C45 120.8(3) . . ? C39 C40 C35 122.5(3) . . ? C39 C40 H40 118.8 . . ? C35 C40 H40 118.8 . . ? C42 C41 C43 109.9(3) . . ? C42 C41 C44 107.9(3) . . ? C43 C41 C44 106.9(3) . . ? C42 C41 C37 111.5(3) . . ? C43 C41 C37 109.2(3) . . ? C44 C41 C37 111.4(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C48 C45 C46 107.9(3) . . ? C48 C45 C47 108.7(4) . . ? C46 C45 C47 106.6(3) . . ? C48 C45 C39 112.4(3) . . ? C46 C45 C39 109.4(3) . . ? C47 C45 C39 111.6(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O3 C49 C50 110.8(3) . . ? O3 C49 C51 107.9(4) . . ? C50 C49 C51 111.0(4) . . ? O3 C49 H49 109.0 . . ? C50 C49 H49 109.0 . . ? C51 C49 H49 109.0 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O4 C52 C54 109.9(3) . . ? O4 C52 C53 108.8(3) . . ? C54 C52 C53 111.8(3) . . ? O4 C52 H52 108.8 . . ? C54 C52 H52 108.8 . . ? C53 C52 H52 108.8 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C61 C56 C57 118.8(5) . . ? C61 C56 C55 122.3(5) . . ? C57 C56 C55 118.9(5) . . ? C58 C57 C56 119.9(5) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 121.2(6) . . ? C57 C58 H58 119.4 . . ? C59 C58 H58 119.4 . . ? C58 C59 C60 119.0(6) . . ? C58 C59 H59 120.5 . . ? C60 C59 H59 120.5 . . ? C61 C60 C59 119.5(5) . . ? C61 C60 H60 120.3 . . ? C59 C60 H60 120.3 . . ? C56 C61 C60 121.5(5) . . ? C56 C61 H61 119.2 . . ? C60 C61 H61 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 O3 Ti1 O1 C1 173.8(3) . . . . ? O4 Ti1 O1 C1 67.0(3) . . . . ? O2 Ti1 O1 C1 -62.0(6) . . . . ? N1 Ti1 O1 C1 -20.7(3) . . . . ? N2 Ti1 O1 C1 -95.5(3) . . . . ? O3 Ti1 O2 C36 64.9(3) . . . . ? O4 Ti1 O2 C36 171.8(3) . . . . ? O1 Ti1 O2 C36 -58.7(6) . . . . ? N1 Ti1 O2 C36 -99.3(3) . . . . ? N2 Ti1 O2 C36 -24.6(3) . . . . ? O4 Ti1 O3 C49 -50.2(5) . . . . ? O2 Ti1 O3 C49 43.6(5) . . . . ? O1 Ti1 O3 C49 -147.3(5) . . . . ? N1 Ti1 O3 C49 153.9(4) . . . . ? N2 Ti1 O3 C49 123.6(5) . . . . ? O3 Ti1 O4 C52 -37.5(3) . . . . ? O2 Ti1 O4 C52 -134.7(3) . . . . ? O1 Ti1 O4 C52 55.4(3) . . . . ? N1 Ti1 O4 C52 135.7(3) . . . . ? N2 Ti1 O4 C52 162.5(3) . . . . ? O3 Ti1 N1 C16 -18.4(4) . . . . ? O4 Ti1 N1 C16 -175.29(19) . . . . ? O2 Ti1 N1 C16 92.94(19) . . . . ? O1 Ti1 N1 C16 -78.44(19) . . . . ? N2 Ti1 N1 C16 13.17(18) . . . . ? O3 Ti1 N1 C15 102.6(4) . . . . ? O4 Ti1 N1 C15 -54.36(19) . . . . ? O2 Ti1 N1 C15 -146.12(18) . . . . ? O1 Ti1 N1 C15 42.49(18) . . . . ? N2 Ti1 N1 C15 134.11(19) . . . . ? O3 Ti1 N1 C18 -140.5(3) . . . . ? O4 Ti1 N1 C18 62.64(19) . . . . ? O2 Ti1 N1 C18 -29.13(18) . . . . ? O1 Ti1 N1 C18 159.48(19) . . . . ? N2 Ti1 N1 C18 -108.90(19) . . . . ? O3 Ti1 N2 C17 -173.11(18) . . . . ? O4 Ti1 N2 C17 -12.3(4) . . . . ? O2 Ti1 N2 C17 -76.77(18) . . . . ? O1 Ti1 N2 C17 95.94(18) . . . . ? N1 Ti1 N2 C17 15.58(18) . . . . ? O3 Ti1 N2 C26 63.73(19) . . . . ? O4 Ti1 N2 C26 -135.5(3) . . . . ? O2 Ti1 N2 C26 160.1(2) . . . . ? O1 Ti1 N2 C26 -27.21(19) . . . . ? N1 Ti1 N2 C26 -107.57(19) . . . . ? O3 Ti1 N2 C34 -53.06(19) . . . . ? O4 Ti1 N2 C34 107.8(3) . . . . ? O2 Ti1 N2 C34 43.28(18) . . . . ? O1 Ti1 N2 C34 -144.01(18) . . . . ? N1 Ti1 N2 C34 135.63(19) . . . . ? Ti1 O1 C1 C6 5.8(5) . . . . ? Ti1 O1 C1 C2 -172.7(2) . . . . ? O1 C1 C2 C3 -177.4(3) . . . . ? C6 C1 C2 C3 4.2(4) . . . . ? O1 C1 C2 C7 7.2(4) . . . . ? C6 C1 C2 C7 -171.3(3) . . . . ? C1 C2 C3 C4 -1.6(5) . . . . ? C7 C2 C3 C4 173.8(3) . . . . ? C2 C3 C4 C5 -0.8(5) . . . . ? C2 C3 C4 C11 -179.8(3) . . . . ? C3 C4 C5 C6 0.7(5) . . . . ? C11 C4 C5 C6 179.7(3) . . . . ? C4 C5 C6 C1 1.9(5) . . . . ? C4 C5 C6 C15 -172.5(3) . . . . ? O1 C1 C6 C5 177.2(3) . . . . ? C2 C1 C6 C5 -4.4(4) . . . . ? O1 C1 C6 C15 -8.5(4) . . . . ? C2 C1 C6 C15 169.9(3) . . . . ? C3 C2 C7 C10 5.6(4) . . . . ? C1 C2 C7 C10 -179.1(3) . . . . ? C3 C2 C7 C8 126.6(3) . . . . ? C1 C2 C7 C8 -58.1(4) . . . . ? C3 C2 C7 C9 -113.3(3) . . . . ? C1 C2 C7 C9 61.9(4) . . . . ? C5 C4 C11 C14 -2.5(5) . . . . ? C3 C4 C11 C14 176.4(3) . . . . ? C5 C4 C11 C13 119.4(4) . . . . ? C3 C4 C11 C13 -61.7(4) . . . . ? C5 C4 C11 C12 -122.3(4) . . . . ? C3 C4 C11 C12 56.7(4) . . . . ? C16 N1 C15 C6 59.2(3) . . . . ? C18 N1 C15 C6 -177.5(3) . . . . ? Ti1 N1 C15 C6 -61.7(3) . . . . ? C5 C6 C15 N1 -141.9(3) . . . . ? C1 C6 C15 N1 43.8(4) . . . . ? C15 N1 C16 C17 -161.9(2) . . . . ? C18 N1 C16 C17 77.5(3) . . . . ? Ti1 N1 C16 C17 -40.7(3) . . . . ? C26 N2 C17 C16 77.3(3) . . . . ? C34 N2 C17 C16 -162.7(2) . . . . ? Ti1 N2 C17 C16 -42.6(3) . . . . ? N1 C16 C17 N2 57.5(3) . . . . ? C16 N1 C18 C19 72.5(3) . . . . ? C15 N1 C18 C19 -49.0(4) . . . . ? Ti1 N1 C18 C19 -167.4(2) . . . . ? N1 C18 C19 C25 95.4(4) . . . . ? N1 C18 C19 C20 -88.4(4) . . . . ? C25 C19 C20 C21 -0.9(5) . . . . ? C18 C19 C20 C21 -177.1(3) . . . . ? C19 C20 C21 C23 -0.2(6) . . . . ? C19 C20 C21 O6 178.7(3) . . . . ? C22 O6 C21 C20 -175.2(5) . . . . ? C22 O6 C21 C23 3.9(5) . . . . ? C23 O5 C22 O6 7.3(6) . . . . ? C21 O6 C22 O5 -7.0(6) . . . . ? C20 C21 C23 C24 1.2(6) . . . . ? O6 C21 C23 C24 -177.9(3) . . . . ? C20 C21 C23 O5 179.7(3) . . . . ? O6 C21 C23 O5 0.6(4) . . . . ? C22 O5 C23 C24 173.6(4) . . . . ? C22 O5 C23 C21 -4.8(5) . . . . ? C21 C23 C24 C25 -1.0(5) . . . . ? O5 C23 C24 C25 -179.2(3) . . . . ? C20 C19 C25 C24 1.1(5) . . . . ? C18 C19 C25 C24 177.3(3) . . . . ? C23 C24 C25 C19 -0.1(5) . . . . ? C17 N2 C26 C27 72.4(3) . . . . ? C34 N2 C26 C27 -48.9(3) . . . . ? Ti1 N2 C26 C27 -167.0(2) . . . . ? N2 C26 C27 C28 100.6(3) . . . . ? N2 C26 C27 C33 -83.0(4) . . . . ? C33 C27 C28 C29 1.3(5) . . . . ? C26 C27 C28 C29 177.7(3) . . . . ? C27 C28 C29 C30 1.2(5) . . . . ? C28 C29 C30 C32 -2.5(5) . . . . ? C28 C29 C30 O8 -177.4(3) . . . . ? C31 O8 C30 C29 -177.8(4) . . . . ? C31 O8 C30 C32 6.9(4) . . . . ? C32 O7 C31 O8 11.5(4) . . . . ? C30 O8 C31 O7 -11.4(4) . . . . ? C29 C30 C32 C33 1.4(5) . . . . ? O8 C30 C32 C33 177.1(3) . . . . ? C29 C30 C32 O7 -175.6(3) . . . . ? O8 C30 C32 O7 0.0(4) . . . . ? C31 O7 C32 C33 176.2(4) . . . . ? C31 O7 C32 C30 -7.0(4) . . . . ? C30 C32 C33 C27 1.1(5) . . . . ? O7 C32 C33 C27 177.6(3) . . . . ? C28 C27 C33 C32 -2.4(5) . . . . ? C26 C27 C33 C32 -178.8(3) . . . . ? C17 N2 C34 C35 57.9(3) . . . . ? C26 N2 C34 C35 -178.7(3) . . . . ? Ti1 N2 C34 C35 -61.8(3) . . . . ? N2 C34 C35 C40 -142.0(3) . . . . ? N2 C34 C35 C36 44.0(4) . . . . ? Ti1 O2 C36 C35 10.4(5) . . . . ? Ti1 O2 C36 C37 -169.1(2) . . . . ? C40 C35 C36 O2 176.1(3) . . . . ? C34 C35 C36 O2 -10.1(4) . . . . ? C40 C35 C36 C37 -4.4(4) . . . . ? C34 C35 C36 C37 169.4(3) . . . . ? O2 C36 C37 C38 -177.7(3) . . . . ? C35 C36 C37 C38 2.8(4) . . . . ? O2 C36 C37 C41 6.4(4) . . . . ? C35 C36 C37 C41 -173.1(3) . . . . ? C36 C37 C38 C39 0.3(5) . . . . ? C41 C37 C38 C39 176.2(3) . . . . ? C37 C38 C39 C40 -1.7(5) . . . . ? C37 C38 C39 C45 -179.2(3) . . . . ? C38 C39 C40 C35 0.1(5) . . . . ? C45 C39 C40 C35 177.5(3) . . . . ? C36 C35 C40 C39 3.0(5) . . . . ? C34 C35 C40 C39 -171.0(3) . . . . ? C38 C37 C41 C42 122.8(3) . . . . ? C36 C37 C41 C42 -61.4(4) . . . . ? C38 C37 C41 C43 -115.5(3) . . . . ? C36 C37 C41 C43 60.2(4) . . . . ? C38 C37 C41 C44 2.3(4) . . . . ? C36 C37 C41 C44 178.0(3) . . . . ? C40 C39 C45 C48 14.3(5) . . . . ? C38 C39 C45 C48 -168.4(4) . . . . ? C40 C39 C45 C46 -105.6(4) . . . . ? C38 C39 C45 C46 71.7(4) . . . . ? C40 C39 C45 C47 136.7(4) . . . . ? C38 C39 C45 C47 -46.0(5) . . . . ? Ti1 O3 C49 C50 -145.4(3) . . . . ? Ti1 O3 C49 C51 92.9(5) . . . . ? Ti1 O4 C52 C54 -121.0(3) . . . . ? Ti1 O4 C52 C53 116.2(3) . . . . ? C61 C56 C57 C58 -1.2(7) . . . . ? C55 C56 C57 C58 179.5(5) . . . . ? C56 C57 C58 C59 0.9(8) . . . . ? C57 C58 C59 C60 0.3(8) . . . . ? C58 C59 C60 C61 -1.2(7) . . . . ? C57 C56 C61 C60 0.3(7) . . . . ? C55 C56 C61 C60 179.5(5) . . . . ? C59 C60 C61 C56 0.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.497 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.056 # Attachment 'pg237.cif' data_pg237 _database_code_depnum_ccdc_archive 'CCDC 711908' #TrackingRef 'pg237.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H20 Cl2 N O4 Ti0.50' _chemical_formula_weight 421.21 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 25.514(4) _cell_length_b 25.514(2) _cell_length_c 30.429(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 17154(3) _cell_formula_units_Z 36 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8490 _cell_measurement_theta_min 3.1622 _cell_measurement_theta_max 32.5836 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7848 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_T_min 0.8590 _exptl_absorpt_correction_T_max 0.8868 _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 44655 _diffrn_reflns_av_R_equivalents 0.2281 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3359 _reflns_number_gt 2857 _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^)+(0.0807P)^2^+98.3064P] 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 3359 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.2152 _refine_ls_wR_factor_gt 0.2020 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _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 0.41584(5) 0.0000 0.2500 0.0469(4) Uani 1 2 d S . . Cl1 Cl 0.39071(7) -0.02230(7) 0.09799(4) 0.0635(5) Uani 1 1 d . . . Cl2 Cl 0.38733(7) -0.23359(7) 0.09125(4) 0.0616(4) Uani 1 1 d . . . O1 O 0.41324(16) -0.02681(16) 0.19092(10) 0.0502(9) Uani 1 1 d . . . O2 O 0.5682(3) -0.1721(3) 0.36479(17) 0.1084(18) Uani 1 1 d . . . O3 O 0.4838(4) -0.2642(3) 0.37651(17) 0.111(2) Uani 1 1 d . . . O4 O 0.4042(2) 0.0603(2) 0.23408(12) 0.0687(12) Uani 1 1 d . . . N1 N 0.45653(18) -0.06379(19) 0.26151(11) 0.0439(10) Uani 1 1 d . . . C1 C 0.4071(2) -0.0745(2) 0.16995(14) 0.0424(11) Uani 1 1 d . . . C2 C 0.3960(2) -0.0798(2) 0.12422(14) 0.0447(12) Uani 1 1 d . . . C3 C 0.3898(2) -0.1276(2) 0.10004(14) 0.0479(13) Uani 1 1 d . . . H3 H 0.3819 -0.1301 0.0694 0.057 Uiso 1 1 calc R . . C4 C 0.3951(2) -0.1719(2) 0.12130(14) 0.0443(12) Uani 1 1 d . . . C5 C 0.4066(2) -0.1687(2) 0.16570(14) 0.0428(11) Uani 1 1 d . . . H5 H 0.4109 -0.1997 0.1796 0.051 Uiso 1 1 calc R . . C6 C 0.4119(2) -0.1208(2) 0.19018(14) 0.0420(11) Uani 1 1 d . . . C7 C 0.4186(2) -0.1230(2) 0.23942(13) 0.0478(12) Uani 1 1 d . . . H7A H 0.3777 -0.1426 0.2527 0.057 Uiso 1 1 calc R . . H7B H 0.4361 -0.1492 0.2457 0.057 Uiso 1 1 calc R . . C8 C 0.5190(2) -0.0329(2) 0.24433(13) 0.0455(12) Uani 1 1 d . . . H8A H 0.5180 -0.0376 0.2120 0.055 Uiso 1 1 calc R . . H8B H 0.5411 -0.0522 0.2568 0.055 Uiso 1 1 calc R . . C9 C 0.4538(3) -0.0756(3) 0.31017(14) 0.0518(13) Uani 1 1 d . . . H9A H 0.4139 -0.0835 0.3210 0.062 Uiso 1 1 calc R . . H9B H 0.4849 -0.0380 0.3246 0.062 Uiso 1 1 calc R . . C10 C 0.4627(3) -0.1269(3) 0.32549(15) 0.0663(17) Uani 1 1 d . . . C11 C 0.4121(4) -0.1838(4) 0.3328(2) 0.097(3) Uani 1 1 d . . . H11 H 0.3734 -0.1896 0.3253 0.117 Uiso 1 1 calc R . . C12 C 0.4155(5) -0.2329(5) 0.3506(3) 0.122(4) Uani 1 1 d . . . H12 H 0.3804 -0.2710 0.3558 0.147 Uiso 1 1 calc R . . C13 C 0.4701(5) -0.2230(5) 0.3599(2) 0.091(2) Uani 1 1 d . . . C14 C 0.5194(4) -0.1688(4) 0.35351(18) 0.079(2) Uani 1 1 d . . . C15 C 0.5187(3) -0.1175(4) 0.33578(16) 0.0732(19) Uani 1 1 d . . . H15 H 0.5545 -0.0797 0.3315 0.088 Uiso 1 1 calc R . . C16 C 0.5431(5) -0.2278(5) 0.3870(2) 0.103(3) Uani 1 1 d . . . H16A H 0.5660 -0.2485 0.3792 0.124 Uiso 1 1 calc R . . H16B H 0.5469 -0.2205 0.4191 0.124 Uiso 1 1 calc R . . C17 C 0.3741(5) 0.0920(5) 0.2372(3) 0.130(4) Uani 1 1 d . . . H17 H 0.3315 0.0607 0.2297 0.156 Uiso 1 1 calc R . . C18 C 0.3895(5) 0.1339(5) 0.2029(3) 0.126(3) Uani 1 1 d . . . H18A H 0.3695 0.1578 0.2075 0.189 Uiso 1 1 calc R . . H18B H 0.3762 0.1123 0.1748 0.189 Uiso 1 1 calc R . . H18C H 0.4334 0.1609 0.2024 0.189 Uiso 1 1 calc R . . C19 C 0.3684(5) 0.1094(4) 0.2794(3) 0.125(4) Uani 1 1 d . . . H19A H 0.3493 0.0737 0.2985 0.187 Uiso 1 1 calc R . . H19B H 0.3433 0.1285 0.2785 0.187 Uiso 1 1 calc R . . H19C H 0.4086 0.1383 0.2909 0.187 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 0.0438(6) 0.0622(9) 0.0410(6) -0.0193(6) -0.0097(3) 0.0311(4) Cl1 0.0819(11) 0.0713(10) 0.0456(7) -0.0053(6) -0.0219(7) 0.0445(8) Cl2 0.0640(9) 0.0652(9) 0.0539(7) -0.0285(6) -0.0089(6) 0.0312(7) O1 0.062(2) 0.063(2) 0.0372(16) -0.0183(16) -0.0211(15) 0.0401(19) O2 0.121(5) 0.128(5) 0.076(3) -0.009(3) 0.001(3) 0.062(4) O3 0.171(7) 0.097(4) 0.071(3) 0.001(3) -0.020(4) 0.071(5) O4 0.089(3) 0.090(3) 0.061(2) -0.022(2) -0.014(2) 0.070(3) N1 0.047(2) 0.062(3) 0.0284(17) -0.0115(17) -0.0064(16) 0.032(2) C1 0.041(3) 0.055(3) 0.034(2) -0.012(2) -0.010(2) 0.026(2) C2 0.041(3) 0.059(3) 0.034(2) -0.001(2) -0.0080(19) 0.026(2) C3 0.048(3) 0.065(3) 0.028(2) -0.015(2) -0.009(2) 0.026(3) C4 0.040(3) 0.054(3) 0.038(2) -0.017(2) -0.007(2) 0.023(2) C5 0.039(3) 0.049(3) 0.039(2) -0.007(2) -0.005(2) 0.022(2) C6 0.038(3) 0.054(3) 0.034(2) -0.007(2) -0.0056(19) 0.023(2) C7 0.061(3) 0.059(3) 0.028(2) -0.006(2) -0.007(2) 0.034(3) C8 0.054(3) 0.064(3) 0.030(2) -0.014(2) -0.009(2) 0.038(3) C9 0.059(3) 0.071(4) 0.028(2) -0.005(2) -0.003(2) 0.035(3) C10 0.083(4) 0.096(5) 0.023(2) -0.013(3) -0.010(3) 0.048(4) C11 0.130(7) 0.083(5) 0.054(3) 0.017(4) -0.021(4) 0.035(5) C12 0.121(8) 0.121(8) 0.073(5) 0.007(5) -0.017(5) 0.021(6) C13 0.107(7) 0.112(7) 0.044(3) -0.007(4) -0.012(4) 0.047(6) C14 0.114(6) 0.126(7) 0.032(3) -0.009(3) -0.005(3) 0.086(6) C15 0.101(5) 0.103(5) 0.035(3) -0.011(3) -0.006(3) 0.066(5) C16 0.171(10) 0.135(8) 0.051(4) 0.009(5) 0.006(5) 0.112(8) C17 0.179(10) 0.166(10) 0.129(7) 0.035(7) 0.031(7) 0.149(9) C18 0.131(8) 0.139(8) 0.136(8) 0.049(7) 0.033(6) 0.089(7) C19 0.170(9) 0.087(6) 0.137(7) 0.011(5) 0.083(7) 0.078(6) _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 1.775(4) 4 ? Ti1 O4 1.775(4) . ? Ti1 O1 1.913(3) 4 ? Ti1 O1 1.913(3) . ? Ti1 N1 2.353(4) 4 ? Ti1 N1 2.353(4) . ? Cl1 C2 1.733(5) . ? Cl2 C4 1.743(5) . ? O1 C1 1.311(6) . ? O2 C14 1.333(8) . ? O2 C16 1.408(10) . ? O3 C13 1.359(10) . ? O3 C16 1.360(11) . ? O4 C17 1.369(8) . ? N1 C8 1.477(6) . ? N1 C7 1.487(6) . ? N1 C9 1.506(5) . ? C1 C6 1.392(7) . ? C1 C2 1.413(6) . ? C2 C3 1.365(7) . ? C3 C4 1.366(7) . ? C3 H3 0.9500 . ? C4 C5 1.377(6) . ? C5 C6 1.378(6) . ? C5 H5 0.9500 . ? C6 C7 1.512(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C8 1.495(10) 4 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.513(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.360(9) . ? C10 C11 1.395(10) . ? C11 C12 1.407(13) . ? C11 H11 0.9500 . ? C12 C13 1.317(12) . ? C12 H12 0.9500 . ? C13 C14 1.340(11) . ? C14 C15 1.423(10) . ? C15 H15 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C19 1.390(12) . ? C17 C18 1.402(12) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 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 O4 Ti1 O4 106.1(3) 4 . ? O4 Ti1 O1 93.60(15) 4 4 ? O4 Ti1 O1 96.34(16) . 4 ? O4 Ti1 O1 96.34(16) 4 . ? O4 Ti1 O1 93.60(15) . . ? O1 Ti1 O1 163.4(2) 4 . ? O4 Ti1 N1 164.46(18) 4 4 ? O4 Ti1 N1 88.99(18) . 4 ? O1 Ti1 N1 80.85(13) 4 4 ? O1 Ti1 N1 86.12(14) . 4 ? O4 Ti1 N1 88.99(18) 4 . ? O4 Ti1 N1 164.46(18) . . ? O1 Ti1 N1 86.12(14) 4 . ? O1 Ti1 N1 80.85(13) . . ? N1 Ti1 N1 76.2(2) 4 . ? C1 O1 Ti1 139.1(3) . . ? C14 O2 C16 102.7(7) . . ? C13 O3 C16 100.9(7) . . ? C17 O4 Ti1 151.7(6) . . ? C8 N1 C7 111.3(3) . . ? C8 N1 C9 112.6(4) . . ? C7 N1 C9 107.5(4) . . ? C8 N1 Ti1 108.1(3) . . ? C7 N1 Ti1 110.3(3) . . ? C9 N1 Ti1 106.9(3) . . ? O1 C1 C6 123.5(4) . . ? O1 C1 C2 119.6(4) . . ? C6 C1 C2 116.9(4) . . ? C3 C2 C1 123.0(5) . . ? C3 C2 Cl1 119.0(3) . . ? C1 C2 Cl1 118.0(4) . . ? C2 C3 C4 118.0(4) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C3 C4 C5 121.4(4) . . ? C3 C4 Cl2 119.0(3) . . ? C5 C4 Cl2 119.5(4) . . ? C4 C5 C6 120.5(5) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.2(4) . . ? C5 C6 C7 117.7(4) . . ? C1 C6 C7 121.9(4) . . ? N1 C7 C6 116.0(4) . . ? N1 C7 H7A 108.3 . . ? C6 C7 H7A 108.3 . . ? N1 C7 H7B 108.3 . . ? C6 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N1 C8 C8 111.6(3) . 4 ? N1 C8 H8A 109.3 . . ? C8 C8 H8A 109.3 4 . ? N1 C8 H8B 109.3 . . ? C8 C8 H8B 109.3 4 . ? H8A C8 H8B 108.0 . . ? N1 C9 C10 117.6(4) . . ? N1 C9 H9A 107.9 . . ? C10 C9 H9A 107.9 . . ? N1 C9 H9B 107.9 . . ? C10 C9 H9B 107.9 . . ? H9A C9 H9B 107.2 . . ? C15 C10 C11 119.4(7) . . ? C15 C10 C9 121.2(6) . . ? C11 C10 C9 119.1(6) . . ? C10 C11 C12 123.3(8) . . ? C10 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C13 C12 C11 116.3(9) . . ? C13 C12 H12 121.8 . . ? C11 C12 H12 121.8 . . ? C12 C13 C14 121.5(9) . . ? C12 C13 O3 126.1(10) . . ? C14 C13 O3 112.4(8) . . ? O2 C14 C13 108.7(8) . . ? O2 C14 C15 126.7(9) . . ? C13 C14 C15 124.5(8) . . ? C10 C15 C14 114.8(7) . . ? C10 C15 H15 122.6 . . ? C14 C15 H15 122.6 . . ? O3 C16 O2 111.4(7) . . ? O3 C16 H16A 109.3 . . ? O2 C16 H16A 109.3 . . ? O3 C16 H16B 109.3 . . ? O2 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? O4 C17 C19 115.5(8) . . ? O4 C17 C18 111.9(8) . . ? C19 C17 C18 118.5(9) . . ? O4 C17 H17 102.6 . . ? C19 C17 H17 102.6 . . ? C18 C17 H17 102.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 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 O4 Ti1 O1 C1 -57.9(5) 4 . . . ? O4 Ti1 O1 C1 -164.5(5) . . . . ? O1 Ti1 O1 C1 68.7(5) 4 . . . ? N1 Ti1 O1 C1 106.7(5) 4 . . . ? N1 Ti1 O1 C1 30.1(5) . . . . ? O4 Ti1 O4 C17 30.2(12) 4 . . . ? O1 Ti1 O4 C17 -65.4(13) 4 . . . ? O1 Ti1 O4 C17 127.9(13) . . . . ? N1 Ti1 O4 C17 -146.1(13) 4 . . . ? N1 Ti1 O4 C17 -163.7(12) . . . . ? O4 Ti1 N1 C8 170.7(3) 4 . . . ? O4 Ti1 N1 C8 4.1(7) . . . . ? O1 Ti1 N1 C8 -95.7(3) 4 . . . ? O1 Ti1 N1 C8 74.1(3) . . . . ? N1 Ti1 N1 C8 -14.13(18) 4 . . . ? O4 Ti1 N1 C7 48.8(3) 4 . . . ? O4 Ti1 N1 C7 -117.8(6) . . . . ? O1 Ti1 N1 C7 142.5(3) 4 . . . ? O1 Ti1 N1 C7 -47.8(3) . . . . ? N1 Ti1 N1 C7 -136.0(3) 4 . . . ? O4 Ti1 N1 C9 -67.8(3) 4 . . . ? O4 Ti1 N1 C9 125.6(6) . . . . ? O1 Ti1 N1 C9 25.9(3) 4 . . . ? O1 Ti1 N1 C9 -164.4(3) . . . . ? N1 Ti1 N1 C9 107.4(3) 4 . . . ? Ti1 O1 C1 C6 -13.4(8) . . . . ? Ti1 O1 C1 C2 167.7(4) . . . . ? O1 C1 C2 C3 179.4(5) . . . . ? C6 C1 C2 C3 0.3(7) . . . . ? O1 C1 C2 Cl1 -0.3(6) . . . . ? C6 C1 C2 Cl1 -179.3(4) . . . . ? C1 C2 C3 C4 -0.6(8) . . . . ? Cl1 C2 C3 C4 179.0(4) . . . . ? C2 C3 C4 C5 -0.2(8) . . . . ? C2 C3 C4 Cl2 -179.9(4) . . . . ? C3 C4 C5 C6 1.3(7) . . . . ? Cl2 C4 C5 C6 -179.0(4) . . . . ? C4 C5 C6 C1 -1.6(7) . . . . ? C4 C5 C6 C7 174.2(4) . . . . ? O1 C1 C6 C5 -178.2(5) . . . . ? C2 C1 C6 C5 0.8(7) . . . . ? O1 C1 C6 C7 6.1(7) . . . . ? C2 C1 C6 C7 -174.9(5) . . . . ? C8 N1 C7 C6 -60.1(5) . . . . ? C9 N1 C7 C6 176.2(4) . . . . ? Ti1 N1 C7 C6 59.9(5) . . . . ? C5 C6 C7 N1 146.9(4) . . . . ? C1 C6 C7 N1 -37.3(7) . . . . ? C7 N1 C8 C8 162.7(4) . . . 4 ? C9 N1 C8 C8 -76.5(5) . . . 4 ? Ti1 N1 C8 C8 41.4(4) . . . 4 ? C8 N1 C9 C10 -76.0(6) . . . . ? C7 N1 C9 C10 46.9(6) . . . . ? Ti1 N1 C9 C10 165.4(4) . . . . ? N1 C9 C10 C15 90.8(6) . . . . ? N1 C9 C10 C11 -94.8(6) . . . . ? C15 C10 C11 C12 0.2(10) . . . . ? C9 C10 C11 C12 -174.3(6) . . . . ? C10 C11 C12 C13 -1.0(12) . . . . ? C11 C12 C13 C14 1.5(12) . . . . ? C11 C12 C13 O3 -178.8(7) . . . . ? C16 O3 C13 C12 -169.2(8) . . . . ? C16 O3 C13 C14 10.6(8) . . . . ? C16 O2 C14 C13 -12.3(7) . . . . ? C16 O2 C14 C15 170.2(6) . . . . ? C12 C13 C14 O2 -178.9(7) . . . . ? O3 C13 C14 O2 1.4(8) . . . . ? C12 C13 C14 C15 -1.3(11) . . . . ? O3 C13 C14 C15 178.9(5) . . . . ? C11 C10 C15 C14 0.1(8) . . . . ? C9 C10 C15 C14 174.5(4) . . . . ? O2 C14 C15 C10 177.6(5) . . . . ? C13 C14 C15 C10 0.4(8) . . . . ? C13 O3 C16 O2 -18.6(8) . . . . ? C14 O2 C16 O3 19.9(8) . . . . ? Ti1 O4 C17 C19 51.8(19) . . . . ? Ti1 O4 C17 C18 -168.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.693 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.087