# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' #TrackingRef '- cif-DT-ART-11-2010-001542' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Matthew D. Jones' _publ_contact_author_email mj205@bath.ac.uk _publ_section_title ; Crystallographic Characterisation of Ti(IV) piperazine complexes and their exploitation for the ring opening polymerisation of rac-lactide ; loop_ _publ_author_name S.Hancock M.Mahon M.Jones data_Ti2(1)2OiPr)4 _database_code_depnum_ccdc_archive 'CCDC 800217' #TrackingRef '- cif-DT-ART-11-2010-001542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H91 N4 O8 Ti2' _chemical_formula_weight 1080.16 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 P21/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 23.224(6) _cell_length_b 16.478(5) _cell_length_c 31.844(9) _cell_angle_alpha 90 _cell_angle_beta 96.782(3) _cell_angle_gamma 90 _cell_volume 12101(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 102329 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 25.17 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4648 _exptl_absorpt_coefficient_mu 0.317 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9739 _exptl_absorpt_correction_T_max 0.9934 _exptl_absorpt_process_details ? _exptl_special_details ; 'Jacobson, R. (1998) Private communication' ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type Synchrotron _diffrn_source Synchrotron _diffrn_radiation_monochromator Synchrotron _diffrn_measurement_device_type Synchrotron _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 102329 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 25.17 _reflns_number_total 23430 _reflns_number_gt 17178 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0916P)^2^+8.8799P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23430 _refine_ls_number_parameters 1365 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2005 _refine_ls_wR_factor_gt 0.1800 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.006 _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 -0.03655(2) 0.23271(3) 0.193594(17) 0.03500(14) Uani 1 1 d . . . Ti2 Ti 0.16667(3) 0.24801(4) 0.436238(19) 0.04643(17) Uani 1 1 d . . . Ti3 Ti 0.45151(3) 0.29148(4) 0.697331(19) 0.04437(16) Uani 1 1 d . . . Ti4 Ti 0.65776(3) 0.22560(4) 0.931514(19) 0.04759(17) Uani 1 1 d . . . O1 O -0.03995(9) 0.18678(12) 0.24655(6) 0.0383(5) Uani 1 1 d . . . O2 O -0.01077(9) 0.16745(13) 0.15209(7) 0.0409(5) Uani 1 1 d . . . O3 O -0.02566(9) 0.34153(12) 0.18966(7) 0.0416(5) Uani 1 1 d . . . O4 O -0.11176(10) 0.22870(14) 0.17548(7) 0.0445(5) Uani 1 1 d . . . O5 O 0.15904(10) 0.17769(14) 0.39013(7) 0.0458(5) Uani 1 1 d . . . O6 O 0.13844(11) 0.22288(15) 0.48661(7) 0.0525(6) Uani 1 1 d . . . O7 O 0.17210(11) 0.35455(16) 0.42563(9) 0.0646(7) Uani 1 1 d . . . O8 O 0.24034(11) 0.22603(19) 0.45346(9) 0.0667(8) Uani 1 1 d . . . O9 O 0.45512(10) 0.21649(13) 0.74116(7) 0.0439(5) Uani 1 1 d . . . O10 O 0.47802(11) 0.26771(17) 0.64623(7) 0.0585(7) Uani 1 1 d . . . O11 O 0.45274(10) 0.39674(15) 0.71304(8) 0.0569(6) Uani 1 1 d . . . O12 O 0.37655(10) 0.28145(16) 0.67941(8) 0.0553(6) Uani 1 1 d . . . O13 O 0.63240(10) 0.16923(18) 0.97612(7) 0.0577(7) Uani 1 1 d . . . O14 O 0.65326(9) 0.17741(14) 0.87836(7) 0.0459(5) Uani 1 1 d . . . O15 O 0.73297(10) 0.20948(18) 0.94517(8) 0.0607(7) Uani 1 1 d . . . O16 O 0.65681(11) 0.33562(17) 0.93327(8) 0.0605(7) Uani 1 1 d . . . N1 N -0.02403(11) 0.25239(15) 0.34104(7) 0.0371(6) Uani 1 1 d . . . N2 N 0.06768(11) 0.27033(15) 0.41273(8) 0.0374(6) Uani 1 1 d . . . N3 N 0.06327(11) 0.23454(14) 0.21740(7) 0.0321(5) Uani 1 1 d . . . N4 N 0.15097(11) 0.21603(14) 0.29150(7) 0.0343(5) Uani 1 1 d . . . N5 N 0.46532(12) 0.24348(18) 0.83945(8) 0.0453(6) Uani 1 1 d . . . N6 N 0.55713(12) 0.24018(18) 0.91143(8) 0.0449(6) Uani 1 1 d . . . N7 N 0.55153(11) 0.29797(15) 0.72027(8) 0.0392(6) Uani 1 1 d . . . N8 N 0.64262(11) 0.25926(15) 0.79034(8) 0.0378(6) Uani 1 1 d . . . C1 C -0.08190(14) 0.25969(19) 0.31702(10) 0.0400(7) Uani 1 1 d . . . H1A H -0.0802 0.2978 0.2932 0.048 Uiso 1 1 calc R . . H1B H -0.1094 0.2820 0.3356 0.048 Uiso 1 1 calc R . . C2 C -0.10318(13) 0.1788(2) 0.30033(9) 0.0387(7) Uani 1 1 d . . . C3 C -0.07938(12) 0.14410(18) 0.26586(9) 0.0348(6) Uani 1 1 d . . . C4 C -0.09524(14) 0.06546(19) 0.25198(10) 0.0425(7) Uani 1 1 d . . . C5 C -0.13590(14) 0.0239(2) 0.27254(11) 0.0489(8) Uani 1 1 d . . . H5 H -0.1468 -0.0294 0.2634 0.059 Uiso 1 1 calc R . . C6 C -0.16115(15) 0.0574(2) 0.30602(11) 0.0509(9) Uani 1 1 d . . . C7 C -0.14408(14) 0.1346(2) 0.31917(10) 0.0472(8) Uani 1 1 d . . . H7 H -0.1610 0.1583 0.3420 0.057 Uiso 1 1 calc R . . C8 C -0.06853(16) 0.0266(2) 0.21622(11) 0.0505(8) Uani 1 1 d . . . H8A H -0.0839 -0.0285 0.2116 0.076 Uiso 1 1 calc R . . H8B H -0.0263 0.0241 0.2233 0.076 Uiso 1 1 calc R . . H8C H -0.0779 0.0587 0.1904 0.076 Uiso 1 1 calc R . . C9 C -0.20526(18) 0.0100(3) 0.32800(14) 0.0748(13) Uani 1 1 d . . . H9A H -0.1906 0.0029 0.3579 0.112 Uiso 1 1 calc R . . H9B H -0.2116 -0.0433 0.3146 0.112 Uiso 1 1 calc R . . H9C H -0.2420 0.0400 0.3257 0.112 Uiso 1 1 calc R . . C10 C -0.02483(13) 0.20474(19) 0.37984(9) 0.0379(7) Uani 1 1 d . . . H10A H -0.0428 0.1512 0.3729 0.045 Uiso 1 1 calc R . . H10B H -0.0483 0.2332 0.3993 0.045 Uiso 1 1 calc R . . C11 C 0.03657(13) 0.19309(18) 0.40125(9) 0.0358(6) Uani 1 1 d . . . H11A H 0.0352 0.1605 0.4272 0.043 Uiso 1 1 calc R . . H11B H 0.0589 0.1618 0.3821 0.043 Uiso 1 1 calc R . . C12 C 0.06307(14) 0.3216(2) 0.37371(9) 0.0410(7) Uani 1 1 d . . . H12A H 0.0872 0.2971 0.3534 0.049 Uiso 1 1 calc R . . H12B H 0.0792 0.3760 0.3813 0.049 Uiso 1 1 calc R . . C13 C 0.00181(14) 0.33164(18) 0.35198(10) 0.0402(7) Uani 1 1 d . . . H13A H -0.0220 0.3607 0.3710 0.048 Uiso 1 1 calc R . . H13B H 0.0025 0.3645 0.3260 0.048 Uiso 1 1 calc R . . C14 C 0.04298(15) 0.31490(19) 0.44747(9) 0.0415(7) Uani 1 1 d . . . H14A H 0.0034 0.3337 0.4369 0.050 Uiso 1 1 calc R . . H14B H 0.0670 0.3635 0.4551 0.050 Uiso 1 1 calc R . . C15 C 0.04007(15) 0.26455(19) 0.48665(9) 0.0414(7) Uani 1 1 d . . . C16 C 0.08912(15) 0.2233(2) 0.50517(10) 0.0445(8) Uani 1 1 d . . . C17 C 0.08890(18) 0.1823(2) 0.54384(10) 0.0519(9) Uani 1 1 d . . . C18 C 0.03786(18) 0.1818(2) 0.56231(11) 0.0559(10) Uani 1 1 d . . . H18 H 0.0372 0.1539 0.5884 0.067 Uiso 1 1 calc R . . C19 C -0.01214(18) 0.2197(2) 0.54467(10) 0.0533(9) Uani 1 1 d . . . C20 C -0.01013(16) 0.2619(2) 0.50648(10) 0.0483(8) Uani 1 1 d . . . H20 H -0.0439 0.2893 0.4939 0.058 Uiso 1 1 calc R . . C21 C 0.14345(19) 0.1422(2) 0.56392(12) 0.0649(11) Uani 1 1 d . . . H21A H 0.1355 0.1139 0.5897 0.097 Uiso 1 1 calc R . . H21B H 0.1734 0.1835 0.5711 0.097 Uiso 1 1 calc R . . H21C H 0.1570 0.1031 0.5441 0.097 Uiso 1 1 calc R . . C22 C -0.06680(19) 0.2170(3) 0.56567(12) 0.0689(12) Uani 1 1 d . . . H22A H -0.0717 0.1625 0.5771 0.103 Uiso 1 1 calc R . . H22B H -0.1001 0.2301 0.5449 0.103 Uiso 1 1 calc R . . H22C H -0.0642 0.2567 0.5888 0.103 Uiso 1 1 calc R . . C23 C 0.09315(14) 0.25695(18) 0.18001(9) 0.0358(6) Uani 1 1 d . . . H23A H 0.1346 0.2670 0.1897 0.043 Uiso 1 1 calc R . . H23B H 0.0763 0.3083 0.1680 0.043 Uiso 1 1 calc R . . C24 C 0.08881(13) 0.19358(18) 0.14555(9) 0.0367(7) Uani 1 1 d . . . C25 C 0.03719(14) 0.15354(18) 0.13276(9) 0.0387(7) Uani 1 1 d . . . C26 C 0.03303(15) 0.0975(2) 0.09918(10) 0.0454(8) Uani 1 1 d . . . C27 C 0.08132(17) 0.0864(2) 0.07817(10) 0.0536(9) Uani 1 1 d . . . H27 H 0.0788 0.0491 0.0553 0.064 Uiso 1 1 calc R . . C28 C 0.13312(16) 0.1270(2) 0.08888(10) 0.0501(9) Uani 1 1 d . . . C29 C 0.13637(15) 0.1790(2) 0.12369(10) 0.0440(8) Uani 1 1 d . . . H29 H 0.1721 0.2053 0.1328 0.053 Uiso 1 1 calc R . . C30 C -0.02310(18) 0.0548(2) 0.08631(12) 0.0615(10) Uani 1 1 d . . . H30A H -0.0526 0.0945 0.0755 0.092 Uiso 1 1 calc R . . H30B H -0.0356 0.0268 0.1108 0.092 Uiso 1 1 calc R . . H30C H -0.0179 0.0151 0.0642 0.092 Uiso 1 1 calc R . . C31 C 0.18355(18) 0.1176(3) 0.06325(12) 0.0681(12) Uani 1 1 d . . . H31A H 0.1894 0.0599 0.0576 0.102 Uiso 1 1 calc R . . H31B H 0.2187 0.1399 0.0792 0.102 Uiso 1 1 calc R . . H31C H 0.1752 0.1469 0.0364 0.102 Uiso 1 1 calc R . . C32 C 0.08331(13) 0.15443(17) 0.23600(9) 0.0337(6) Uani 1 1 d . . . H32A H 0.0803 0.1132 0.2132 0.040 Uiso 1 1 calc R . . H32B H 0.0571 0.1377 0.2568 0.040 Uiso 1 1 calc R . . C33 C 0.14502(13) 0.15583(17) 0.25759(9) 0.0358(6) Uani 1 1 d . . . H33A H 0.1555 0.1015 0.2694 0.043 Uiso 1 1 calc R . . H33B H 0.1719 0.1692 0.2366 0.043 Uiso 1 1 calc R . . C34 C 0.07480(13) 0.29649(17) 0.25149(9) 0.0346(6) Uani 1 1 d . . . H34A H 0.0479 0.2870 0.2729 0.042 Uiso 1 1 calc R . . H34B H 0.0662 0.3509 0.2391 0.042 Uiso 1 1 calc R . . C35 C 0.13675(13) 0.29625(18) 0.27348(9) 0.0370(7) Uani 1 1 d . . . H35A H 0.1640 0.3102 0.2529 0.044 Uiso 1 1 calc R . . H35B H 0.1408 0.3376 0.2962 0.044 Uiso 1 1 calc R . . C36 C 0.20898(13) 0.21453(19) 0.31555(10) 0.0390(7) Uani 1 1 d . . . H36A H 0.2126 0.2600 0.3360 0.047 Uiso 1 1 calc R . . H36B H 0.2386 0.2221 0.2959 0.047 Uiso 1 1 calc R . . C37 C 0.21984(13) 0.13570(19) 0.33891(10) 0.0391(7) Uani 1 1 d . . . C38 C 0.19242(13) 0.1198(2) 0.37501(10) 0.0408(7) Uani 1 1 d . . . C39 C 0.19816(15) 0.0443(2) 0.39543(11) 0.0483(8) Uani 1 1 d . . . C40 C 0.23292(17) -0.0138(2) 0.37920(12) 0.0568(9) Uani 1 1 d . . . H40 H 0.2370 -0.0652 0.3928 0.068 Uiso 1 1 calc R . . C41 C 0.26181(17) -0.0005(2) 0.34423(12) 0.0556(9) Uani 1 1 d . . . C42 C 0.25422(15) 0.0748(2) 0.32452(11) 0.0478(8) Uani 1 1 d . . . H42 H 0.2733 0.0851 0.3002 0.057 Uiso 1 1 calc R . . C43 C 0.16795(18) 0.0275(3) 0.43371(12) 0.0611(10) Uani 1 1 d . . . H43A H 0.1841 0.0625 0.4571 0.092 Uiso 1 1 calc R . . H43B H 0.1736 -0.0295 0.4419 0.092 Uiso 1 1 calc R . . H43C H 0.1264 0.0386 0.4271 0.092 Uiso 1 1 calc R . . C44 C 0.2983(2) -0.0659(3) 0.32703(15) 0.0814(14) Uani 1 1 d . . . H44A H 0.2998 -0.1135 0.3456 0.122 Uiso 1 1 calc R . . H44B H 0.3377 -0.0453 0.3258 0.122 Uiso 1 1 calc R . . H44C H 0.2811 -0.0812 0.2986 0.122 Uiso 1 1 calc R . . C45 C -0.06224(16) 0.4073(2) 0.17484(11) 0.0491(8) Uani 1 1 d . . . H45 H -0.0904 0.3878 0.1508 0.059 Uiso 1 1 calc R . . C46 C -0.0954(2) 0.4360(3) 0.20953(15) 0.0730(12) Uani 1 1 d . . . H46A H -0.1187 0.3912 0.2187 0.110 Uiso 1 1 calc R . . H46B H -0.1209 0.4808 0.1992 0.110 Uiso 1 1 calc R . . H46C H -0.0682 0.4548 0.2334 0.110 Uiso 1 1 calc R . . C47 C -0.0251(2) 0.4739(2) 0.15883(14) 0.0676(11) Uani 1 1 d . . . H47A H 0.0040 0.4916 0.1818 0.101 Uiso 1 1 calc R . . H47B H -0.0498 0.5200 0.1490 0.101 Uiso 1 1 calc R . . H47C H -0.0057 0.4531 0.1354 0.101 Uiso 1 1 calc R . . C48 C -0.17194(16) 0.2223(3) 0.16298(13) 0.0587(10) Uani 1 1 d . . . H48 H -0.1837 0.2688 0.1437 0.070 Uiso 1 1 calc R . . C49 C -0.20454(19) 0.2289(4) 0.20008(15) 0.0906(17) Uani 1 1 d . . . H49A H -0.1944 0.1833 0.2193 0.136 Uiso 1 1 calc R . . H49B H -0.2462 0.2278 0.1906 0.136 Uiso 1 1 calc R . . H49C H -0.1946 0.2800 0.2149 0.136 Uiso 1 1 calc R . . C50 C -0.1840(2) 0.1466(3) 0.1387(2) 0.103(2) Uani 1 1 d . . . H50A H -0.1608 0.1456 0.1149 0.154 Uiso 1 1 calc R . . H50B H -0.2253 0.1442 0.1280 0.154 Uiso 1 1 calc R . . H50C H -0.1738 0.0999 0.1571 0.154 Uiso 1 1 calc R . . C51 C 0.21601(18) 0.4160(3) 0.43088(15) 0.0682(11) Uani 1 1 d . . . H51 H 0.2486 0.3955 0.4514 0.082 Uiso 1 1 calc R . . C52 C 0.1928(2) 0.4902(3) 0.44876(17) 0.0885(15) Uani 1 1 d . . . H52A H 0.1615 0.5123 0.4287 0.133 Uiso 1 1 calc R . . H52B H 0.2238 0.5305 0.4541 0.133 Uiso 1 1 calc R . . H52C H 0.1776 0.4769 0.4754 0.133 Uiso 1 1 calc R . . C53 C 0.2379(3) 0.4283(4) 0.39037(19) 0.113(2) Uani 1 1 d . . . H53A H 0.2561 0.3782 0.3819 0.169 Uiso 1 1 calc R . . H53B H 0.2666 0.4722 0.3929 0.169 Uiso 1 1 calc R . . H53C H 0.2057 0.4428 0.3690 0.169 Uiso 1 1 calc R . . C54 C 0.29474(19) 0.1884(4) 0.46299(16) 0.0896(16) Uani 1 1 d . . . H54 H 0.2890 0.1302 0.4547 0.107 Uiso 1 1 calc R . . C55 C 0.3127(3) 0.1883(5) 0.50790(19) 0.138(3) Uani 1 1 d . . . H55A H 0.3150 0.2443 0.5183 0.207 Uiso 1 1 calc R . . H55B H 0.3508 0.1626 0.5136 0.207 Uiso 1 1 calc R . . H55C H 0.2844 0.1581 0.5223 0.207 Uiso 1 1 calc R . . C56 C 0.3355(2) 0.2224(5) 0.4349(2) 0.124(2) Uani 1 1 d . . . H56A H 0.3190 0.2160 0.4053 0.185 Uiso 1 1 calc R . . H56B H 0.3726 0.1933 0.4397 0.185 Uiso 1 1 calc R . . H56C H 0.3419 0.2801 0.4413 0.185 Uiso 1 1 calc R . . C57 C 0.40712(15) 0.2541(2) 0.81647(11) 0.0479(8) Uani 1 1 d . . . H57A H 0.4070 0.3027 0.7982 0.058 Uiso 1 1 calc R . . H57B H 0.3790 0.2635 0.8370 0.058 Uiso 1 1 calc R . . C58 C 0.38824(14) 0.1815(2) 0.78963(10) 0.0452(8) Uani 1 1 d . . . C59 C 0.41439(14) 0.1653(2) 0.75326(10) 0.0426(7) Uani 1 1 d . . . C60 C 0.39908(15) 0.0961(2) 0.72847(11) 0.0481(8) Uani 1 1 d . . . C61 C 0.35529(15) 0.0470(2) 0.74034(12) 0.0539(9) Uani 1 1 d . . . H61 H 0.3436 0.0013 0.7233 0.065 Uiso 1 1 calc R . . C62 C 0.32790(16) 0.0615(2) 0.77574(13) 0.0562(9) Uani 1 1 d . . . C63 C 0.34546(15) 0.1292(2) 0.80050(11) 0.0535(9) Uani 1 1 d . . . H63 H 0.3277 0.1398 0.8253 0.064 Uiso 1 1 calc R . . C64 C 0.42940(17) 0.0769(2) 0.69041(12) 0.0588(10) Uani 1 1 d . . . H64A H 0.4166 0.0237 0.6791 0.088 Uiso 1 1 calc R . . H64B H 0.4714 0.0759 0.6987 0.088 Uiso 1 1 calc R . . H64C H 0.4200 0.1185 0.6687 0.088 Uiso 1 1 calc R . . C65 C 0.28112(18) 0.0048(3) 0.78811(15) 0.0729(12) Uani 1 1 d . . . H65A H 0.2686 -0.0317 0.7645 0.109 Uiso 1 1 calc R . . H65B H 0.2479 0.0367 0.7950 0.109 Uiso 1 1 calc R . . H65C H 0.2966 -0.0273 0.8128 0.109 Uiso 1 1 calc R . . C66 C 0.46766(14) 0.1784(2) 0.87081(10) 0.0475(8) Uani 1 1 d . . . H66A H 0.4528 0.1274 0.8571 0.057 Uiso 1 1 calc R . . H66B H 0.4430 0.1925 0.8931 0.057 Uiso 1 1 calc R . . C67 C 0.53028(14) 0.1669(2) 0.89037(10) 0.0461(8) Uani 1 1 d . . . H67A H 0.5316 0.1224 0.9114 0.055 Uiso 1 1 calc R . . H67B H 0.5538 0.1499 0.8679 0.055 Uiso 1 1 calc R . . C68 C 0.48576(15) 0.3185(2) 0.86017(11) 0.0506(8) Uani 1 1 d . . . H68A H 0.4608 0.3327 0.8822 0.061 Uiso 1 1 calc R . . H68B H 0.4835 0.3631 0.8392 0.061 Uiso 1 1 calc R . . C69 C 0.54817(14) 0.3083(2) 0.88025(10) 0.0466(8) Uani 1 1 d . . . H69A H 0.5731 0.2990 0.8576 0.056 Uiso 1 1 calc R . . H69B H 0.5609 0.3596 0.8947 0.056 Uiso 1 1 calc R . . C70 C 0.53121(16) 0.2612(2) 0.95092(10) 0.0501(8) Uani 1 1 d . . . H70A H 0.4905 0.2785 0.9433 0.060 Uiso 1 1 calc R . . H70B H 0.5527 0.3076 0.9649 0.060 Uiso 1 1 calc R . . C71 C 0.53266(16) 0.1913(2) 0.98160(10) 0.0515(9) Uani 1 1 d . . . C72 C 0.58377(16) 0.1498(2) 0.99350(11) 0.0535(9) Uani 1 1 d . . . C73 C 0.58622(18) 0.0874(3) 1.02397(12) 0.0614(10) Uani 1 1 d . . . C74 C 0.5361(2) 0.0693(3) 1.04166(13) 0.0692(11) Uani 1 1 d . . . H74 H 0.5373 0.0272 1.0621 0.083 Uiso 1 1 calc R . . C75 C 0.48463(19) 0.1095(3) 1.03087(13) 0.0687(11) Uani 1 1 d . . . C76 C 0.48299(17) 0.1701(3) 1.00011(11) 0.0615(10) Uani 1 1 d . . . H76 H 0.4475 0.1975 0.9916 0.074 Uiso 1 1 calc R . . C77 C 0.6420(2) 0.0435(3) 1.03696(15) 0.0833(14) Uani 1 1 d . . . H77A H 0.6342 -0.0056 1.0527 0.125 Uiso 1 1 calc R . . H77B H 0.6684 0.0789 1.0549 0.125 Uiso 1 1 calc R . . H77C H 0.6600 0.0285 1.0117 0.125 Uiso 1 1 calc R . . C78 C 0.4315(2) 0.0897(4) 1.05206(16) 0.0879(15) Uani 1 1 d . . . H78A H 0.4258 0.0307 1.0522 0.132 Uiso 1 1 calc R . . H78B H 0.3974 0.1156 1.0365 0.132 Uiso 1 1 calc R . . H78C H 0.4367 0.1097 1.0812 0.132 Uiso 1 1 calc R . . C79 C 0.57781(15) 0.3452(2) 0.68727(10) 0.0477(8) Uani 1 1 d . . . H79A H 0.6180 0.3606 0.6983 0.057 Uiso 1 1 calc R . . H79B H 0.5553 0.3957 0.6810 0.057 Uiso 1 1 calc R . . C80 C 0.57869(15) 0.2973(2) 0.64708(10) 0.0479(8) Uani 1 1 d . . . C81 C 0.52786(17) 0.2614(2) 0.62876(10) 0.0528(9) Uani 1 1 d . . . C82 C 0.52716(19) 0.2168(3) 0.59111(12) 0.0647(11) Uani 1 1 d . . . C83 C 0.57870(19) 0.2097(3) 0.57339(12) 0.0658(11) Uani 1 1 d . . . H83 H 0.5786 0.1794 0.5480 0.079 Uiso 1 1 calc R . . C84 C 0.63040(18) 0.2447(3) 0.59102(11) 0.0623(10) Uani 1 1 d . . . C85 C 0.62926(17) 0.2883(2) 0.62809(11) 0.0550(9) Uani 1 1 d . . . H85 H 0.6640 0.3128 0.6409 0.066 Uiso 1 1 calc R . . C86 C 0.4710(2) 0.1785(3) 0.57179(13) 0.0825(14) Uani 1 1 d . . . H86A H 0.4734 0.1664 0.5419 0.124 Uiso 1 1 calc R . . H86B H 0.4388 0.2161 0.5741 0.124 Uiso 1 1 calc R . . H86C H 0.4643 0.1281 0.5868 0.124 Uiso 1 1 calc R . . C87 C 0.6850(2) 0.2345(4) 0.57052(14) 0.0844(15) Uani 1 1 d . . . H87A H 0.6895 0.1774 0.5630 0.127 Uiso 1 1 calc R . . H87B H 0.7184 0.2516 0.5903 0.127 Uiso 1 1 calc R . . H87C H 0.6827 0.2679 0.5449 0.127 Uiso 1 1 calc R . . C88 C 0.57840(14) 0.21597(19) 0.72810(10) 0.0418(7) Uani 1 1 d . . . H88A H 0.5778 0.1874 0.7007 0.050 Uiso 1 1 calc R . . H88B H 0.5544 0.1842 0.7459 0.050 Uiso 1 1 calc R . . C89 C 0.64039(13) 0.21784(19) 0.74954(10) 0.0387(7) Uani 1 1 d . . . H89A H 0.6551 0.1617 0.7539 0.046 Uiso 1 1 calc R . . H89B H 0.6654 0.2466 0.7313 0.046 Uiso 1 1 calc R . . C90 C 0.55956(14) 0.34254(19) 0.76141(10) 0.0415(7) Uani 1 1 d . . . H90A H 0.5343 0.3178 0.7808 0.050 Uiso 1 1 calc R . . H90B H 0.5470 0.3995 0.7565 0.050 Uiso 1 1 calc R . . C91 C 0.62179(14) 0.34172(19) 0.78246(10) 0.0412(7) Uani 1 1 d . . . H91A H 0.6469 0.3698 0.7640 0.049 Uiso 1 1 calc R . . H91B H 0.6241 0.3716 0.8096 0.049 Uiso 1 1 calc R . . C92 C 0.70111(14) 0.26008(19) 0.81297(10) 0.0400(7) Uani 1 1 d . . . H92A H 0.7019 0.2961 0.8379 0.048 Uiso 1 1 calc R . . H92B H 0.7284 0.2824 0.7943 0.048 Uiso 1 1 calc R . . C93 C 0.72072(13) 0.17626(19) 0.82725(10) 0.0389(7) Uani 1 1 d . . . C94 C 0.69405(13) 0.1369(2) 0.85898(10) 0.0404(7) Uani 1 1 d . . . C95 C 0.70877(14) 0.0571(2) 0.87073(10) 0.0455(8) Uani 1 1 d . . . C96 C 0.75265(15) 0.0197(2) 0.85190(11) 0.0481(8) Uani 1 1 d . . . H96 H 0.7630 -0.0345 0.8598 0.058 Uiso 1 1 calc R . . C97 C 0.78207(15) 0.0584(2) 0.82195(11) 0.0459(8) Uani 1 1 d . . . C98 C 0.76426(14) 0.1361(2) 0.80950(10) 0.0419(7) Uani 1 1 d . . . H98 H 0.7826 0.1625 0.7881 0.050 Uiso 1 1 calc R . . C99 C 0.67795(16) 0.0144(2) 0.90325(12) 0.0568(9) Uani 1 1 d . . . H99A H 0.6885 0.0396 0.9310 0.085 Uiso 1 1 calc R . . H99B H 0.6893 -0.0429 0.9045 0.085 Uiso 1 1 calc R . . H99C H 0.6360 0.0187 0.8955 0.085 Uiso 1 1 calc R . . C100 C 0.83127(18) 0.0170(2) 0.80393(14) 0.0663(11) Uani 1 1 d . . . H10C H 0.8669 0.0486 0.8108 0.099 Uiso 1 1 calc R . . H10D H 0.8223 0.0128 0.7731 0.099 Uiso 1 1 calc R . . H10E H 0.8367 -0.0375 0.8161 0.099 Uiso 1 1 calc R . . C101 C 0.41238(17) 0.4625(2) 0.70614(14) 0.0608(10) Uani 1 1 d . . . H101 H 0.3844 0.4496 0.6807 0.073 Uiso 1 1 calc R . . C102 C 0.3795(3) 0.4711(3) 0.7428(2) 0.121(2) Uani 1 1 d . . . H10F H 0.3618 0.4189 0.7486 0.181 Uiso 1 1 calc R . . H10G H 0.3490 0.5120 0.7365 0.181 Uiso 1 1 calc R . . H10H H 0.4057 0.4881 0.7676 0.181 Uiso 1 1 calc R . . C103 C 0.4454(2) 0.5367(3) 0.69691(16) 0.0746(12) Uani 1 1 d . . . H10I H 0.4738 0.5495 0.7213 0.112 Uiso 1 1 calc R . . H10J H 0.4185 0.5823 0.6913 0.112 Uiso 1 1 calc R . . H10K H 0.4656 0.5271 0.6720 0.112 Uiso 1 1 calc R . . C104 C 0.31740(18) 0.2737(3) 0.66440(14) 0.0736(13) Uani 1 1 d . . . H104 H 0.3043 0.3276 0.6524 0.088 Uiso 1 1 calc R . . C105 C 0.3092(3) 0.2161(5) 0.6303(2) 0.160(4) Uani 1 1 d . . . H10L H 0.3287 0.2357 0.6066 0.240 Uiso 1 1 calc R . . H10M H 0.2677 0.2097 0.6212 0.240 Uiso 1 1 calc R . . H10N H 0.3257 0.1637 0.6400 0.240 Uiso 1 1 calc R . . C106 C 0.2838(2) 0.2575(5) 0.69995(19) 0.124(3) Uani 1 1 d . . . H10O H 0.3000 0.2102 0.7158 0.187 Uiso 1 1 calc R . . H10P H 0.2433 0.2467 0.6890 0.187 Uiso 1 1 calc R . . H10Q H 0.2856 0.3049 0.7187 0.187 Uiso 1 1 calc R . . C107 C 0.7872(2) 0.1711(4) 0.95896(15) 0.0977(19) Uani 1 1 d . . . H107 H 0.7787 0.1116 0.9578 0.117 Uiso 1 1 calc R . . C108 C 0.8069(2) 0.1862(5) 1.00018(18) 0.131(3) Uani 1 1 d . . . H10R H 0.8207 0.2424 1.0031 0.196 Uiso 1 1 calc R . . H10S H 0.8388 0.1491 1.0095 0.196 Uiso 1 1 calc R . . H10T H 0.7753 0.1780 1.0176 0.196 Uiso 1 1 calc R . . C109 C 0.82792(19) 0.1848(4) 0.92626(16) 0.0952(18) Uani 1 1 d . . . H10U H 0.8315 0.2432 0.9212 0.143 Uiso 1 1 calc R . . H10V H 0.8127 0.1578 0.8999 0.143 Uiso 1 1 calc R . . H10W H 0.8661 0.1625 0.9365 0.143 Uiso 1 1 calc R . . C110 C 0.69967(19) 0.3993(3) 0.93648(14) 0.0706(12) Uani 1 1 d . . . H110 H 0.7358 0.3782 0.9261 0.085 Uiso 1 1 calc R . . C111 C 0.7130(3) 0.4224(4) 0.98163(16) 0.1042(19) Uani 1 1 d . . . H11C H 0.6781 0.4448 0.9919 0.156 Uiso 1 1 calc R . . H11D H 0.7438 0.4633 0.9845 0.156 Uiso 1 1 calc R . . H11E H 0.7258 0.3743 0.9983 0.156 Uiso 1 1 calc R . . C112 C 0.6770(3) 0.4702(3) 0.90890(18) 0.0980(17) Uani 1 1 d . . . H11F H 0.6668 0.4514 0.8798 0.147 Uiso 1 1 calc R . . H11G H 0.7071 0.5120 0.9095 0.147 Uiso 1 1 calc R . . H11H H 0.6426 0.4928 0.9196 0.147 Uiso 1 1 calc R . . C113 C 0.5310(3) 0.0045(4) 0.5101(2) 0.119(2) Uani 1 1 d . . . H11I H 0.5564 -0.0251 0.4924 0.142 Uiso 1 1 calc R . . H11J H 0.5416 0.0626 0.5094 0.142 Uiso 1 1 calc R . . C114 C 0.5439(4) -0.0245(5) 0.5538(3) 0.156(3) Uani 1 1 d . . . H4 H 0.5354 -0.0833 0.5544 0.188 Uiso 1 1 calc R . . H6 H 0.5177 0.0033 0.5715 0.188 Uiso 1 1 calc R . . C115 C 0.6075(3) -0.0106(4) 0.5738(3) 0.161(4) Uani 1 1 d . . . H11K H 0.6120 -0.0298 0.6031 0.242 Uiso 1 1 calc R . . H11L H 0.6166 0.0474 0.5732 0.242 Uiso 1 1 calc R . . H11M H 0.6338 -0.0408 0.5576 0.242 Uiso 1 1 calc R . . C116 C 0.0168(6) -0.0247(5) 0.5169(4) 0.056(3) Uani 0.55 1 d P . 1 H11N H -0.0024 -0.0782 0.5183 0.068 Uiso 0.55 1 calc PR . 1 H11O H 0.0152 0.0026 0.5444 0.068 Uiso 0.55 1 calc PR . 1 C117 C 0.0793(5) -0.0385(5) 0.5109(3) 0.072(2) Uani 0.55 1 d P A 1 H11P H 0.0799 -0.0665 0.4834 0.086 Uiso 0.55 1 calc PR A 1 H11Q H 0.0972 0.0155 0.5081 0.086 Uiso 0.55 1 calc PR A 1 C118 C 0.1171(3) -0.0838(3) 0.5421(2) 0.1044(18) Uani 1 1 d . . . H1 H 0.1565 -0.0844 0.5340 0.157 Uiso 1 1 calc R A 1 H2 H 0.1028 -0.1395 0.5435 0.157 Uiso 1 1 calc R A 1 H3 H 0.1175 -0.0578 0.5698 0.157 Uiso 1 1 calc R A 1 C217 C 0.0590(6) -0.0541(6) 0.5394(4) 0.077(3) Uani 0.45 1 d P A 2 H21D H 0.0570 -0.0169 0.5636 0.092 Uiso 0.45 1 calc PR A 2 H21E H 0.0337 -0.1010 0.5438 0.092 Uiso 0.45 1 calc PR A 2 C216 C 0.0322(7) -0.0101(8) 0.4996(6) 0.067(4) Uani 0.45 1 d P . 2 H21F H 0.0364 -0.0444 0.4747 0.080 Uiso 0.45 1 calc PR . 2 H21G H 0.0538 0.0409 0.4965 0.080 Uiso 0.45 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0326(3) 0.0374(3) 0.0341(3) 0.0005(2) 0.0003(2) 0.0013(2) Ti2 0.0364(4) 0.0565(4) 0.0442(3) -0.0019(3) -0.0041(3) -0.0029(3) Ti3 0.0397(4) 0.0498(3) 0.0418(3) 0.0034(3) -0.0031(2) 0.0009(3) Ti4 0.0350(4) 0.0677(4) 0.0390(3) -0.0019(3) -0.0001(2) 0.0004(3) O1 0.0327(12) 0.0434(11) 0.0384(11) 0.0014(9) 0.0028(9) -0.0020(9) O2 0.0371(13) 0.0464(12) 0.0384(11) -0.0055(9) 0.0011(9) -0.0016(10) O3 0.0410(13) 0.0366(11) 0.0451(12) 0.0047(9) -0.0038(10) 0.0065(9) O4 0.0353(13) 0.0511(13) 0.0459(13) -0.0028(10) -0.0005(10) -0.0001(10) O5 0.0403(13) 0.0563(14) 0.0400(12) 0.0037(10) 0.0018(10) 0.0101(11) O6 0.0467(15) 0.0691(16) 0.0388(12) -0.0010(11) -0.0074(11) 0.0043(12) O7 0.0469(15) 0.0592(16) 0.0835(19) 0.0000(14) -0.0098(13) -0.0136(12) O8 0.0378(15) 0.095(2) 0.0643(17) 0.0024(15) -0.0053(12) 0.0012(14) O9 0.0392(13) 0.0490(13) 0.0425(12) 0.0010(10) 0.0002(10) -0.0030(10) O10 0.0453(15) 0.0890(19) 0.0399(13) -0.0009(12) -0.0011(11) -0.0099(13) O11 0.0481(15) 0.0477(14) 0.0717(17) 0.0045(12) -0.0064(12) 0.0079(11) O12 0.0389(14) 0.0680(16) 0.0559(15) 0.0033(12) -0.0072(11) 0.0020(12) O13 0.0400(14) 0.0914(19) 0.0404(13) 0.0078(12) -0.0007(10) 0.0026(13) O14 0.0351(13) 0.0615(14) 0.0407(12) 0.0019(10) 0.0022(9) 0.0067(11) O15 0.0354(14) 0.088(2) 0.0572(16) 0.0037(13) 0.0001(11) 0.0019(13) O16 0.0460(15) 0.0691(17) 0.0645(17) -0.0139(13) -0.0015(12) -0.0063(13) N1 0.0354(15) 0.0438(14) 0.0307(13) 0.0012(10) -0.0018(10) 0.0003(11) N2 0.0371(15) 0.0417(14) 0.0326(13) -0.0021(10) 0.0009(10) -0.0022(11) N3 0.0343(14) 0.0339(12) 0.0278(12) 0.0026(9) 0.0020(10) 0.0013(10) N4 0.0316(14) 0.0357(12) 0.0340(13) -0.0005(10) -0.0026(10) 0.0006(10) N5 0.0370(16) 0.0602(17) 0.0372(14) 0.0002(12) -0.0022(11) -0.0011(13) N6 0.0371(16) 0.0657(18) 0.0316(13) -0.0005(12) 0.0033(11) 0.0019(13) N7 0.0420(16) 0.0413(14) 0.0329(13) 0.0049(10) -0.0010(11) 0.0008(12) N8 0.0351(15) 0.0416(14) 0.0350(13) -0.0024(10) -0.0037(11) 0.0040(11) C1 0.0343(18) 0.0492(18) 0.0356(16) 0.0001(13) -0.0002(13) 0.0041(14) C2 0.0286(17) 0.0522(18) 0.0330(15) 0.0034(13) -0.0049(12) -0.0017(13) C3 0.0264(16) 0.0435(16) 0.0335(15) 0.0068(12) -0.0005(12) 0.0007(12) C4 0.0380(19) 0.0450(17) 0.0422(17) 0.0043(13) -0.0049(14) 0.0004(14) C5 0.040(2) 0.0471(18) 0.055(2) 0.0088(15) -0.0097(15) -0.0108(15) C6 0.038(2) 0.069(2) 0.0447(19) 0.0131(16) -0.0027(15) -0.0133(17) C7 0.0301(18) 0.075(2) 0.0362(17) 0.0039(15) 0.0008(13) -0.0026(16) C8 0.052(2) 0.0448(18) 0.054(2) -0.0014(15) 0.0055(16) -0.0009(16) C9 0.058(3) 0.100(3) 0.066(3) 0.020(2) 0.005(2) -0.036(2) C10 0.0382(18) 0.0419(16) 0.0329(15) -0.0015(12) 0.0017(12) -0.0008(13) C11 0.0353(17) 0.0384(15) 0.0325(15) -0.0041(12) -0.0016(12) -0.0032(13) C12 0.0399(19) 0.0474(17) 0.0345(16) 0.0040(13) -0.0008(13) -0.0029(14) C13 0.0443(19) 0.0388(16) 0.0369(16) 0.0020(12) 0.0032(13) -0.0004(14) C14 0.047(2) 0.0420(17) 0.0351(16) -0.0072(13) 0.0028(13) -0.0013(14) C15 0.047(2) 0.0449(17) 0.0305(15) -0.0076(13) -0.0036(13) -0.0044(14) C16 0.047(2) 0.0497(19) 0.0353(16) -0.0081(13) -0.0035(14) -0.0048(15) C17 0.072(3) 0.0469(19) 0.0332(17) -0.0073(14) -0.0067(16) -0.0064(17) C18 0.081(3) 0.055(2) 0.0307(17) -0.0045(15) -0.0009(17) -0.016(2) C19 0.069(3) 0.058(2) 0.0335(17) -0.0091(15) 0.0077(16) -0.0137(19) C20 0.052(2) 0.056(2) 0.0352(17) -0.0126(14) -0.0011(15) -0.0044(16) C21 0.086(3) 0.061(2) 0.043(2) -0.0010(17) -0.0152(19) 0.002(2) C22 0.080(3) 0.087(3) 0.043(2) -0.0094(19) 0.016(2) -0.020(2) C23 0.0344(17) 0.0394(15) 0.0336(15) 0.0057(12) 0.0032(12) -0.0004(13) C24 0.0396(18) 0.0404(16) 0.0291(14) 0.0060(12) -0.0003(12) 0.0047(13) C25 0.0452(19) 0.0398(16) 0.0308(15) 0.0036(12) 0.0029(13) 0.0074(14) C26 0.054(2) 0.0430(17) 0.0385(17) -0.0002(13) 0.0022(15) 0.0072(15) C27 0.074(3) 0.052(2) 0.0342(17) -0.0041(14) 0.0024(16) 0.0172(19) C28 0.055(2) 0.059(2) 0.0381(17) 0.0058(15) 0.0109(15) 0.0182(18) C29 0.0415(19) 0.0523(19) 0.0379(17) 0.0101(14) 0.0039(14) 0.0085(15) C30 0.072(3) 0.056(2) 0.055(2) -0.0169(17) 0.0012(19) -0.0061(19) C31 0.070(3) 0.093(3) 0.044(2) 0.004(2) 0.0201(19) 0.025(2) C32 0.0342(17) 0.0331(14) 0.0323(15) 0.0014(11) -0.0018(12) 0.0038(12) C33 0.0358(17) 0.0343(15) 0.0359(15) 0.0018(12) -0.0010(12) 0.0021(12) C34 0.0345(17) 0.0318(14) 0.0370(15) -0.0017(12) 0.0012(12) 0.0010(12) C35 0.0378(18) 0.0376(15) 0.0343(15) 0.0020(12) -0.0018(12) -0.0027(13) C36 0.0338(18) 0.0444(17) 0.0370(16) 0.0019(13) -0.0031(13) -0.0028(13) C37 0.0304(17) 0.0458(17) 0.0391(16) 0.0028(13) -0.0047(13) 0.0021(13) C38 0.0326(18) 0.0483(18) 0.0395(17) 0.0025(13) -0.0036(13) 0.0053(14) C39 0.044(2) 0.053(2) 0.0460(19) 0.0069(15) -0.0039(15) 0.0030(16) C40 0.061(2) 0.049(2) 0.057(2) 0.0117(16) -0.0046(18) 0.0090(18) C41 0.056(2) 0.056(2) 0.054(2) 0.0002(17) 0.0011(17) 0.0193(18) C42 0.044(2) 0.058(2) 0.0404(18) 0.0019(15) 0.0016(14) 0.0102(16) C43 0.061(3) 0.067(2) 0.056(2) 0.0208(18) 0.0088(18) 0.007(2) C44 0.099(4) 0.067(3) 0.078(3) 0.005(2) 0.013(3) 0.036(3) C45 0.053(2) 0.0440(18) 0.0470(19) 0.0033(14) -0.0054(15) 0.0133(16) C46 0.076(3) 0.063(3) 0.081(3) -0.011(2) 0.009(2) 0.023(2) C47 0.089(3) 0.044(2) 0.068(3) 0.0170(18) 0.000(2) 0.005(2) C48 0.036(2) 0.079(3) 0.059(2) -0.0115(19) -0.0050(16) 0.0039(18) C49 0.041(3) 0.158(5) 0.074(3) -0.023(3) 0.008(2) 0.003(3) C50 0.062(3) 0.104(4) 0.138(5) -0.056(4) -0.006(3) -0.011(3) C51 0.053(3) 0.068(3) 0.082(3) -0.003(2) 0.002(2) -0.022(2) C52 0.101(4) 0.070(3) 0.094(4) -0.003(3) 0.012(3) -0.027(3) C53 0.126(5) 0.119(5) 0.098(4) -0.031(4) 0.034(4) -0.065(4) C54 0.044(3) 0.135(5) 0.086(3) 0.008(3) -0.009(2) 0.014(3) C55 0.101(5) 0.211(8) 0.090(4) 0.022(5) -0.040(4) 0.017(5) C56 0.056(4) 0.185(7) 0.132(6) 0.002(5) 0.022(3) -0.007(4) C57 0.0353(19) 0.065(2) 0.0418(18) -0.0007(15) -0.0031(14) 0.0082(16) C58 0.0329(18) 0.058(2) 0.0426(18) 0.0064(15) -0.0033(14) 0.0033(15) C59 0.0312(18) 0.0487(18) 0.0459(18) 0.0042(14) -0.0033(13) 0.0003(14) C60 0.039(2) 0.0463(18) 0.057(2) 0.0035(15) -0.0026(15) 0.0004(15) C61 0.045(2) 0.052(2) 0.063(2) -0.0002(17) -0.0012(17) -0.0032(16) C62 0.039(2) 0.064(2) 0.063(2) 0.0131(18) -0.0037(17) -0.0049(17) C63 0.036(2) 0.076(3) 0.047(2) 0.0101(18) -0.0013(15) 0.0043(18) C64 0.060(2) 0.053(2) 0.062(2) -0.0114(17) 0.0022(18) -0.0003(18) C65 0.056(3) 0.082(3) 0.080(3) 0.011(2) 0.008(2) -0.020(2) C66 0.0366(19) 0.063(2) 0.0415(18) 0.0008(15) -0.0007(14) 0.0013(16) C67 0.0376(19) 0.060(2) 0.0395(17) -0.0012(15) -0.0006(14) 0.0010(16) C68 0.046(2) 0.063(2) 0.0408(18) 0.0013(16) -0.0009(15) 0.0032(17) C69 0.040(2) 0.061(2) 0.0377(17) -0.0002(15) 0.0013(14) 0.0001(16) C70 0.041(2) 0.074(2) 0.0351(17) -0.0040(16) 0.0029(14) 0.0037(17) C71 0.045(2) 0.076(2) 0.0339(17) 0.0001(16) 0.0049(14) -0.0034(18) C72 0.045(2) 0.078(3) 0.0362(18) -0.0007(16) -0.0001(15) 0.0005(18) C73 0.061(3) 0.080(3) 0.042(2) 0.0062(18) -0.0013(17) -0.004(2) C74 0.075(3) 0.079(3) 0.052(2) 0.011(2) 0.002(2) -0.009(2) C75 0.065(3) 0.089(3) 0.053(2) 0.003(2) 0.014(2) -0.017(2) C76 0.047(2) 0.095(3) 0.043(2) -0.0032(19) 0.0050(16) -0.007(2) C77 0.078(3) 0.105(4) 0.065(3) 0.025(3) -0.002(2) 0.017(3) C78 0.073(3) 0.119(4) 0.075(3) 0.011(3) 0.025(2) -0.024(3) C79 0.046(2) 0.055(2) 0.0412(18) 0.0077(15) -0.0010(14) -0.0017(16) C80 0.045(2) 0.064(2) 0.0333(16) 0.0093(15) -0.0024(14) -0.0005(16) C81 0.051(2) 0.072(2) 0.0346(17) 0.0047(16) 0.0012(15) -0.0013(18) C82 0.063(3) 0.092(3) 0.0369(19) -0.0027(19) -0.0021(17) -0.011(2) C83 0.072(3) 0.086(3) 0.0386(19) -0.0049(19) 0.0038(19) 0.005(2) C84 0.055(3) 0.091(3) 0.0388(19) 0.0063(19) 0.0007(17) 0.010(2) C85 0.050(2) 0.078(3) 0.0352(18) 0.0109(17) -0.0001(15) 0.0023(19) C86 0.083(3) 0.116(4) 0.047(2) -0.016(2) 0.001(2) -0.023(3) C87 0.071(3) 0.137(5) 0.047(2) -0.001(3) 0.009(2) 0.022(3) C88 0.044(2) 0.0428(17) 0.0367(16) -0.0015(13) -0.0019(14) 0.0023(14) C89 0.0337(18) 0.0429(16) 0.0388(16) -0.0014(13) 0.0009(13) -0.0002(13) C90 0.0437(19) 0.0415(16) 0.0380(16) -0.0038(13) -0.0011(13) 0.0042(14) C91 0.0437(19) 0.0399(16) 0.0388(17) -0.0028(13) 0.0001(14) 0.0018(14) C92 0.0378(19) 0.0425(17) 0.0386(16) -0.0013(13) -0.0005(13) 0.0012(14) C93 0.0336(17) 0.0450(17) 0.0369(16) -0.0011(13) -0.0007(13) 0.0003(13) C94 0.0298(17) 0.0532(19) 0.0375(16) -0.0017(13) 0.0017(13) 0.0035(14) C95 0.0375(19) 0.0539(19) 0.0446(18) 0.0051(15) 0.0034(14) -0.0026(15) C96 0.044(2) 0.0454(18) 0.054(2) 0.0054(15) 0.0038(16) 0.0059(15) C97 0.046(2) 0.0469(18) 0.0460(19) -0.0009(14) 0.0084(15) 0.0035(15) C98 0.0406(19) 0.0501(18) 0.0346(16) 0.0019(13) 0.0035(13) 0.0011(14) C99 0.051(2) 0.060(2) 0.061(2) 0.0114(18) 0.0125(18) -0.0048(18) C100 0.073(3) 0.057(2) 0.075(3) 0.0007(19) 0.034(2) 0.017(2) C101 0.053(2) 0.052(2) 0.075(3) 0.0097(19) -0.0024(19) 0.0092(18) C102 0.147(6) 0.086(4) 0.145(6) 0.035(4) 0.082(5) 0.046(4) C103 0.075(3) 0.056(2) 0.092(3) 0.012(2) 0.007(2) 0.009(2) C104 0.043(2) 0.111(4) 0.063(3) 0.002(2) -0.0076(19) 0.000(2) C105 0.072(4) 0.240(9) 0.156(6) -0.125(7) -0.040(4) 0.022(5) C106 0.043(3) 0.236(8) 0.095(4) 0.044(5) 0.007(3) 0.016(4) C107 0.048(3) 0.178(6) 0.065(3) 0.006(3) -0.003(2) 0.020(3) C108 0.076(4) 0.235(9) 0.078(4) 0.051(5) -0.002(3) 0.034(5) C109 0.041(3) 0.170(6) 0.075(3) -0.024(3) 0.007(2) -0.014(3) C110 0.060(3) 0.072(3) 0.077(3) -0.014(2) -0.004(2) -0.010(2) C111 0.138(5) 0.098(4) 0.071(3) -0.009(3) -0.012(3) -0.035(4) C112 0.119(5) 0.090(4) 0.083(4) 0.009(3) -0.002(3) -0.017(3) C113 0.142(6) 0.086(4) 0.119(5) -0.003(4) -0.021(4) 0.000(4) C114 0.191(8) 0.113(6) 0.149(7) 0.022(5) -0.046(6) -0.013(5) C115 0.148(7) 0.103(5) 0.211(9) 0.015(5) -0.072(6) -0.009(5) C116 0.065(8) 0.047(5) 0.060(6) -0.006(4) 0.020(6) -0.013(5) C117 0.086(7) 0.053(4) 0.077(6) -0.001(4) 0.014(5) -0.017(5) C118 0.099(4) 0.072(3) 0.142(6) 0.000(3) 0.013(4) -0.006(3) C217 0.101(10) 0.055(6) 0.080(8) -0.005(5) 0.036(8) -0.014(6) C216 0.077(14) 0.054(7) 0.075(9) -0.018(6) 0.036(9) -0.018(8) _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(2) . ? Ti1 O3 1.817(2) . ? Ti1 O2 1.857(2) . ? Ti1 O1 1.859(2) . ? Ti1 N3 2.353(3) . ? Ti2 O8 1.772(3) . ? Ti2 O7 1.795(3) . ? Ti2 O6 1.850(3) . ? Ti2 O5 1.862(2) . ? Ti2 N2 2.361(3) . ? Ti3 O12 1.774(2) . ? Ti3 O11 1.804(3) . ? Ti3 O10 1.848(3) . ? Ti3 O9 1.859(2) . ? Ti3 N7 2.354(3) . ? Ti4 O15 1.769(3) . ? Ti4 O16 1.814(3) . ? Ti4 O13 1.851(3) . ? Ti4 O14 1.862(2) . ? Ti4 N6 2.361(3) . ? O1 C3 1.358(3) . ? O2 C25 1.354(4) . ? O3 C45 1.423(4) . ? O4 C48 1.411(4) . ? O5 C38 1.353(4) . ? O6 C16 1.350(4) . ? O7 C51 1.433(4) . ? O8 C54 1.408(5) . ? O9 C59 1.357(4) . ? O10 C81 1.346(4) . ? O11 C101 1.432(4) . ? O12 C104 1.406(5) . ? O13 C72 1.353(4) . ? O14 C94 1.364(4) . ? O15 C107 1.431(5) . ? O16 C110 1.442(5) . ? N1 C13 1.462(4) . ? N1 C10 1.466(4) . ? N1 C1 1.471(4) . ? N2 C11 1.488(4) . ? N2 C12 1.496(4) . ? N2 C14 1.498(4) . ? N3 C34 1.491(4) . ? N3 C23 1.494(4) . ? N3 C32 1.498(3) . ? N4 C33 1.461(4) . ? N4 C35 1.463(4) . ? N4 C36 1.469(4) . ? N5 C68 1.454(5) . ? N5 C66 1.462(4) . ? N5 C57 1.470(4) . ? N6 C67 1.482(4) . ? N6 C69 1.497(4) . ? N6 C70 1.498(4) . ? N7 C90 1.494(4) . ? N7 C79 1.494(4) . ? N7 C88 1.497(4) . ? N8 C91 1.454(4) . ? N8 C92 1.461(4) . ? N8 C89 1.463(4) . ? C1 C2 1.496(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.388(4) . ? C2 C3 1.408(4) . ? C3 C4 1.404(4) . ? C4 C5 1.391(5) . ? C4 C8 1.503(5) . ? C5 C6 1.391(5) . ? C5 H5 0.9500 . ? C6 C7 1.383(5) . ? C6 C9 1.523(5) . ? C7 H7 0.9500 . ? 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 C11 1.518(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.516(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.506(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.391(5) . ? C15 C16 1.396(5) . ? C16 C17 1.405(5) . ? C17 C18 1.384(5) . ? C17 C21 1.503(5) . ? C18 C19 1.379(5) . ? C18 H18 0.9500 . ? C19 C20 1.406(5) . ? C19 C22 1.504(5) . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.509(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.387(4) . ? C24 C29 1.394(4) . ? C25 C26 1.407(4) . ? C26 C27 1.384(5) . ? C26 C30 1.496(5) . ? C27 C28 1.384(5) . ? C27 H27 0.9500 . ? C28 C29 1.396(5) . ? C28 C31 1.513(5) . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.515(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.524(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.503(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C42 1.393(5) . ? C37 C38 1.403(4) . ? C38 C39 1.403(5) . ? C39 C40 1.391(5) . ? C39 C43 1.502(5) . ? C40 C41 1.384(5) . ? C40 H40 0.9500 . ? C41 C42 1.392(5) . ? C41 C44 1.514(5) . ? C42 H42 0.9500 . ? 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 C46 1.496(5) . ? C45 C47 1.521(5) . ? C45 H45 1.0000 . ? 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 C50 1.476(6) . ? C48 C49 1.481(6) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C53 1.455(7) . ? C51 C52 1.477(7) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.442(7) . ? C54 C56 1.486(7) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.506(5) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C63 1.389(5) . ? C58 C59 1.396(5) . ? C59 C60 1.408(5) . ? C60 C61 1.386(5) . ? C60 C64 1.505(5) . ? C61 C62 1.379(5) . ? C61 H61 0.9500 . ? C62 C63 1.400(5) . ? C62 C65 1.520(5) . ? C63 H63 0.9500 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.525(4) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.523(5) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.509(5) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.383(5) . ? C71 C76 1.400(5) . ? C72 C73 1.410(5) . ? C73 C74 1.384(6) . ? C73 C77 1.499(6) . ? C74 C75 1.374(6) . ? C74 H74 0.9500 . ? C75 C76 1.396(6) . ? C75 C78 1.511(6) . ? C76 H76 0.9500 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 C80 1.506(5) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.386(5) . ? C80 C85 1.391(5) . ? C81 C82 1.405(5) . ? C82 C83 1.387(6) . ? C82 C86 1.513(6) . ? C83 C84 1.390(6) . ? C83 H83 0.9500 . ? C84 C85 1.385(5) . ? C84 C87 1.503(6) . ? C85 H85 0.9500 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 C89 1.519(4) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 C91 1.520(4) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 C93 1.508(4) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C98 1.384(4) . ? C93 C94 1.404(4) . ? C94 C95 1.398(5) . ? C95 C96 1.387(5) . ? C95 C99 1.502(5) . ? C96 C97 1.392(5) . ? C96 H96 0.9500 . ? C97 C98 1.389(5) . ? C97 C100 1.502(5) . ? C98 H98 0.9500 . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 H10C 0.9800 . ? C100 H10D 0.9800 . ? C100 H10E 0.9800 . ? C101 C102 1.475(6) . ? C101 C103 1.491(6) . ? C101 H101 1.0000 . ? C102 H10F 0.9800 . ? C102 H10G 0.9800 . ? C102 H10H 0.9800 . ? C103 H10I 0.9800 . ? C103 H10J 0.9800 . ? C103 H10K 0.9800 . ? C104 C105 1.436(7) . ? C104 C106 1.474(7) . ? C104 H104 1.0000 . ? C105 H10L 0.9800 . ? C105 H10M 0.9800 . ? C105 H10N 0.9800 . ? C106 H10O 0.9800 . ? C106 H10P 0.9800 . ? C106 H10Q 0.9800 . ? C107 C108 1.361(7) . ? C107 C109 1.504(6) . ? C107 H107 1.0000 . ? C108 H10R 0.9800 . ? C108 H10S 0.9800 . ? C108 H10T 0.9800 . ? C109 H10U 0.9800 . ? C109 H10V 0.9800 . ? C109 H10W 0.9800 . ? C110 C111 1.484(6) . ? C110 C112 1.517(7) . ? C110 H110 1.0000 . ? C111 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C113 C114 1.468(9) . ? C113 C113 1.513(12) 3_656 ? C113 H11I 0.9900 . ? C113 H11J 0.9900 . ? C114 C115 1.553(9) . ? C114 H4 0.9900 . ? C114 H6 0.9900 . ? C115 H11K 0.9800 . ? C115 H11L 0.9800 . ? C115 H11M 0.9800 . ? C116 C116 1.49(2) 3_556 ? C116 C117 1.504(17) . ? C116 H11N 0.9900 . ? C116 H11O 0.9900 . ? C117 C118 1.451(12) . ? C117 H11P 0.9900 . ? C117 H11Q 0.9900 . ? C118 C217 1.427(14) . ? C118 H1 0.9800 . ? C118 H2 0.9800 . ? C118 H3 0.9800 . ? C217 C216 1.53(2) . ? C217 H21D 0.9900 . ? C217 H21E 0.9900 . ? C216 C216 1.53(3) 3_556 ? C216 H21F 0.9900 . ? C216 H21G 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ti1 O3 98.86(10) . . ? O4 Ti1 O2 97.75(10) . . ? O3 Ti1 O2 117.59(10) . . ? O4 Ti1 O1 97.70(10) . . ? O3 Ti1 O1 119.05(10) . . ? O2 Ti1 O1 117.50(10) . . ? O4 Ti1 N3 178.59(10) . . ? O3 Ti1 N3 82.51(9) . . ? O2 Ti1 N3 81.29(9) . . ? O1 Ti1 N3 81.87(9) . . ? O8 Ti2 O7 99.88(13) . . ? O8 Ti2 O6 96.54(12) . . ? O7 Ti2 O6 114.97(13) . . ? O8 Ti2 O5 96.62(12) . . ? O7 Ti2 O5 117.55(12) . . ? O6 Ti2 O5 122.26(11) . . ? O8 Ti2 N2 177.15(12) . . ? O7 Ti2 N2 82.84(10) . . ? O6 Ti2 N2 83.02(10) . . ? O5 Ti2 N2 81.29(9) . . ? O12 Ti3 O11 99.30(12) . . ? O12 Ti3 O10 96.50(12) . . ? O11 Ti3 O10 116.85(13) . . ? O12 Ti3 O9 97.77(11) . . ? O11 Ti3 O9 115.66(11) . . ? O10 Ti3 O9 122.01(12) . . ? O12 Ti3 N7 177.16(11) . . ? O11 Ti3 N7 83.54(10) . . ? O10 Ti3 N7 82.16(10) . . ? O9 Ti3 N7 80.90(9) . . ? O15 Ti4 O16 99.07(13) . . ? O15 Ti4 O13 97.50(12) . . ? O16 Ti4 O13 118.15(13) . . ? O15 Ti4 O14 96.15(11) . . ? O16 Ti4 O14 117.06(12) . . ? O13 Ti4 O14 119.67(12) . . ? O15 Ti4 N6 176.88(12) . . ? O16 Ti4 N6 83.77(11) . . ? O13 Ti4 N6 82.21(10) . . ? O14 Ti4 N6 81.35(9) . . ? C3 O1 Ti1 136.46(18) . . ? C25 O2 Ti1 140.6(2) . . ? C45 O3 Ti1 133.8(2) . . ? C48 O4 Ti1 176.7(2) . . ? C38 O5 Ti2 135.6(2) . . ? C16 O6 Ti2 141.7(2) . . ? C51 O7 Ti2 137.2(3) . . ? C54 O8 Ti2 165.1(3) . . ? C59 O9 Ti3 131.0(2) . . ? C81 O10 Ti3 140.6(2) . . ? C101 O11 Ti3 134.1(2) . . ? C104 O12 Ti3 178.9(3) . . ? C72 O13 Ti4 142.1(2) . . ? C94 O14 Ti4 130.73(19) . . ? C107 O15 Ti4 161.6(4) . . ? C110 O16 Ti4 136.0(3) . . ? C13 N1 C10 108.9(2) . . ? C13 N1 C1 112.0(2) . . ? C10 N1 C1 112.4(2) . . ? C11 N2 C12 107.1(2) . . ? C11 N2 C14 112.6(2) . . ? C12 N2 C14 109.9(2) . . ? C11 N2 Ti2 111.78(18) . . ? C12 N2 Ti2 108.84(18) . . ? C14 N2 Ti2 106.60(18) . . ? C34 N3 C23 110.5(2) . . ? C34 N3 C32 107.1(2) . . ? C23 N3 C32 112.4(2) . . ? C34 N3 Ti1 109.19(17) . . ? C23 N3 Ti1 106.21(17) . . ? C32 N3 Ti1 111.37(17) . . ? C33 N4 C35 109.0(2) . . ? C33 N4 C36 112.0(2) . . ? C35 N4 C36 111.7(2) . . ? C68 N5 C66 109.2(3) . . ? C68 N5 C57 110.9(3) . . ? C66 N5 C57 112.7(3) . . ? C67 N6 C69 107.0(2) . . ? C67 N6 C70 112.3(3) . . ? C69 N6 C70 110.2(3) . . ? C67 N6 Ti4 112.9(2) . . ? C69 N6 Ti4 108.15(19) . . ? C70 N6 Ti4 106.21(19) . . ? C90 N7 C79 110.0(3) . . ? C90 N7 C88 106.9(2) . . ? C79 N7 C88 113.0(3) . . ? C90 N7 Ti3 108.11(19) . . ? C79 N7 Ti3 105.99(18) . . ? C88 N7 Ti3 112.79(19) . . ? C91 N8 C92 110.3(2) . . ? C91 N8 C89 107.8(2) . . ? C92 N8 C89 112.1(2) . . ? N1 C1 C2 110.8(3) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C7 C2 C3 118.4(3) . . ? C7 C2 C1 121.9(3) . . ? C3 C2 C1 119.7(3) . . ? O1 C3 C4 120.1(3) . . ? O1 C3 C2 119.4(3) . . ? C4 C3 C2 120.6(3) . . ? C5 C4 C3 118.3(3) . . ? C5 C4 C8 120.7(3) . . ? C3 C4 C8 121.0(3) . . ? C6 C5 C4 122.4(3) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C7 C6 C5 117.8(3) . . ? C7 C6 C9 121.1(4) . . ? C5 C6 C9 121.1(4) . . ? C6 C7 C2 122.6(3) . . ? C6 C7 H7 118.7 . . ? C2 C7 H7 118.7 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 110.0(2) . . ? N1 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? N1 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C10 113.9(2) . . ? N2 C11 H11A 108.8 . . ? C10 C11 H11A 108.8 . . ? N2 C11 H11B 108.8 . . ? C10 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N2 C12 C13 114.3(3) . . ? N2 C12 H12A 108.7 . . ? C13 C12 H12A 108.7 . . ? N2 C12 H12B 108.7 . . ? C13 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? N1 C13 C12 110.4(3) . . ? N1 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? N1 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N2 C14 C15 113.6(3) . . ? N2 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? N2 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C20 C15 C16 118.6(3) . . ? C20 C15 C14 121.0(3) . . ? C16 C15 C14 120.3(3) . . ? O6 C16 C15 120.6(3) . . ? O6 C16 C17 118.2(3) . . ? C15 C16 C17 121.2(3) . . ? C18 C17 C16 117.9(3) . . ? C18 C17 C21 122.5(3) . . ? C16 C17 C21 119.6(4) . . ? C19 C18 C17 123.1(3) . . ? C19 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? C18 C19 C20 117.7(3) . . ? C18 C19 C22 121.3(3) . . ? C20 C19 C22 121.0(4) . . ? C15 C20 C19 121.5(3) . . ? C15 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 C24 114.3(2) . . ? N3 C23 H23A 108.7 . . ? C24 C23 H23A 108.7 . . ? N3 C23 H23B 108.7 . . ? C24 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C25 C24 C29 118.7(3) . . ? C25 C24 C23 121.6(3) . . ? C29 C24 C23 119.5(3) . . ? O2 C25 C24 121.0(3) . . ? O2 C25 C26 118.0(3) . . ? C24 C25 C26 121.0(3) . . ? C27 C26 C25 117.8(3) . . ? C27 C26 C30 122.3(3) . . ? C25 C26 C30 119.8(3) . . ? C28 C27 C26 123.2(3) . . ? C28 C27 H27 118.4 . . ? C26 C27 H27 118.4 . . ? C27 C28 C29 117.2(3) . . ? C27 C28 C31 121.6(3) . . ? C29 C28 C31 121.2(4) . . ? C24 C29 C28 122.0(3) . . ? C24 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C33 113.5(2) . . ? N3 C32 H32A 108.9 . . ? C33 C32 H32A 108.9 . . ? N3 C32 H32B 108.9 . . ? C33 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? N4 C33 C32 110.3(2) . . ? N4 C33 H33A 109.6 . . ? C32 C33 H33A 109.6 . . ? N4 C33 H33B 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? N3 C34 C35 114.3(2) . . ? N3 C34 H34A 108.7 . . ? C35 C34 H34A 108.7 . . ? N3 C34 H34B 108.7 . . ? C35 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? N4 C35 C34 109.9(2) . . ? N4 C35 H35A 109.7 . . ? C34 C35 H35A 109.7 . . ? N4 C35 H35B 109.7 . . ? C34 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? N4 C36 C37 111.2(2) . . ? N4 C36 H36A 109.4 . . ? C37 C36 H36A 109.4 . . ? N4 C36 H36B 109.4 . . ? C37 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C42 C37 C38 117.9(3) . . ? C42 C37 C36 121.9(3) . . ? C38 C37 C36 120.0(3) . . ? O5 C38 C37 119.7(3) . . ? O5 C38 C39 119.1(3) . . ? C37 C38 C39 121.2(3) . . ? C40 C39 C38 117.8(3) . . ? C40 C39 C43 121.5(3) . . ? C38 C39 C43 120.8(3) . . ? C41 C40 C39 123.2(3) . . ? C41 C40 H40 118.4 . . ? C39 C40 H40 118.4 . . ? C40 C41 C42 117.2(3) . . ? C40 C41 C44 121.6(4) . . ? C42 C41 C44 121.2(4) . . ? C41 C42 C37 122.7(3) . . ? C41 C42 H42 118.6 . . ? C37 C42 H42 118.6 . . ? C39 C43 H43A 109.5 . . ? C39 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C39 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 . . ? O3 C45 C46 109.6(3) . . ? O3 C45 C47 108.7(3) . . ? C46 C45 C47 112.4(3) . . ? O3 C45 H45 108.7 . . ? C46 C45 H45 108.7 . . ? C47 C45 H45 108.7 . . ? 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 . . ? O4 C48 C50 109.3(3) . . ? O4 C48 C49 110.6(3) . . ? C50 C48 C49 113.4(4) . . ? O4 C48 H48 107.8 . . ? C50 C48 H48 107.8 . . ? C49 C48 H48 107.8 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O7 C51 C53 108.2(4) . . ? O7 C51 C52 110.0(4) . . ? C53 C51 C52 114.1(5) . . ? O7 C51 H51 108.1 . . ? C53 C51 H51 108.1 . . ? C52 C51 H51 108.1 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O8 C54 C55 111.1(5) . . ? O8 C54 C56 108.9(5) . . ? C55 C54 C56 117.8(5) . . ? O8 C54 H54 106.0 . . ? C55 C54 H54 106.0 . . ? C56 C54 H54 106.0 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N5 C57 C58 112.1(3) . . ? N5 C57 H57A 109.2 . . ? C58 C57 H57A 109.2 . . ? N5 C57 H57B 109.2 . . ? C58 C57 H57B 109.2 . . ? H57A C57 H57B 107.9 . . ? C63 C58 C59 118.9(3) . . ? C63 C58 C57 121.3(3) . . ? C59 C58 C57 119.8(3) . . ? O9 C59 C58 120.2(3) . . ? O9 C59 C60 118.9(3) . . ? C58 C59 C60 120.9(3) . . ? C61 C60 C59 117.6(3) . . ? C61 C60 C64 121.7(3) . . ? C59 C60 C64 120.7(3) . . ? C62 C61 C60 123.1(4) . . ? C62 C61 H61 118.4 . . ? C60 C61 H61 118.4 . . ? C61 C62 C63 117.8(3) . . ? C61 C62 C65 121.2(4) . . ? C63 C62 C65 121.0(4) . . ? C58 C63 C62 121.6(4) . . ? C58 C63 H63 119.2 . . ? C62 C63 H63 119.2 . . ? C60 C64 H64A 109.5 . . ? C60 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C60 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 C65 H65A 109.5 . . ? C62 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C62 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N5 C66 C67 109.1(3) . . ? N5 C66 H66A 109.9 . . ? C67 C66 H66A 109.9 . . ? N5 C66 H66B 109.9 . . ? C67 C66 H66B 109.9 . . ? H66A C66 H66B 108.3 . . ? N6 C67 C66 114.4(3) . . ? N6 C67 H67A 108.7 . . ? C66 C67 H67A 108.7 . . ? N6 C67 H67B 108.7 . . ? C66 C67 H67B 108.7 . . ? H67A C67 H67B 107.6 . . ? N5 C68 C69 110.0(3) . . ? N5 C68 H68A 109.7 . . ? C69 C68 H68A 109.7 . . ? N5 C68 H68B 109.7 . . ? C69 C68 H68B 109.7 . . ? H68A C68 H68B 108.2 . . ? N6 C69 C68 114.3(3) . . ? N6 C69 H69A 108.7 . . ? C68 C69 H69A 108.7 . . ? N6 C69 H69B 108.7 . . ? C68 C69 H69B 108.7 . . ? H69A C69 H69B 107.6 . . ? N6 C70 C71 112.7(3) . . ? N6 C70 H70A 109.0 . . ? C71 C70 H70A 109.0 . . ? N6 C70 H70B 109.0 . . ? C71 C70 H70B 109.0 . . ? H70A C70 H70B 107.8 . . ? C72 C71 C76 119.0(4) . . ? C72 C71 C70 120.5(3) . . ? C76 C71 C70 120.4(3) . . ? O13 C72 C71 120.1(3) . . ? O13 C72 C73 119.1(3) . . ? C71 C72 C73 120.8(4) . . ? C74 C73 C72 118.0(4) . . ? C74 C73 C77 121.6(4) . . ? C72 C73 C77 120.3(4) . . ? C75 C74 C73 122.9(4) . . ? C75 C74 H74 118.6 . . ? C73 C74 H74 118.6 . . ? C74 C75 C76 118.1(4) . . ? C74 C75 C78 121.1(4) . . ? C76 C75 C78 120.8(4) . . ? C75 C76 C71 121.2(4) . . ? C75 C76 H76 119.4 . . ? C71 C76 H76 119.4 . . ? C73 C77 H77A 109.5 . . ? C73 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C73 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C75 C78 H78A 109.5 . . ? C75 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C75 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N7 C79 C80 111.9(3) . . ? N7 C79 H79A 109.2 . . ? C80 C79 H79A 109.2 . . ? N7 C79 H79B 109.2 . . ? C80 C79 H79B 109.2 . . ? H79A C79 H79B 107.9 . . ? C81 C80 C85 119.5(3) . . ? C81 C80 C79 119.0(3) . . ? C85 C80 C79 121.5(3) . . ? O10 C81 C80 121.6(3) . . ? O10 C81 C82 118.0(3) . . ? C80 C81 C82 120.4(4) . . ? C83 C82 C81 117.9(4) . . ? C83 C82 C86 122.9(4) . . ? C81 C82 C86 119.2(4) . . ? C82 C83 C84 123.1(4) . . ? C82 C83 H83 118.4 . . ? C84 C83 H83 118.4 . . ? C85 C84 C83 117.2(4) . . ? C85 C84 C87 122.0(4) . . ? C83 C84 C87 120.7(4) . . ? C84 C85 C80 121.8(4) . . ? C84 C85 H85 119.1 . . ? C80 C85 H85 119.1 . . ? C82 C86 H86A 109.5 . . ? C82 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C82 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C84 C87 H87A 109.5 . . ? C84 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C84 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N7 C88 C89 114.3(3) . . ? N7 C88 H88A 108.7 . . ? C89 C88 H88A 108.7 . . ? N7 C88 H88B 108.7 . . ? C89 C88 H88B 108.7 . . ? H88A C88 H88B 107.6 . . ? N8 C89 C88 109.9(3) . . ? N8 C89 H89A 109.7 . . ? C88 C89 H89A 109.7 . . ? N8 C89 H89B 109.7 . . ? C88 C89 H89B 109.7 . . ? H89A C89 H89B 108.2 . . ? N7 C90 C91 113.3(3) . . ? N7 C90 H90A 108.9 . . ? C91 C90 H90A 108.9 . . ? N7 C90 H90B 108.9 . . ? C91 C90 H90B 108.9 . . ? H90A C90 H90B 107.7 . . ? N8 C91 C90 111.3(3) . . ? N8 C91 H91A 109.4 . . ? C90 C91 H91A 109.4 . . ? N8 C91 H91B 109.4 . . ? C90 C91 H91B 109.4 . . ? H91A C91 H91B 108.0 . . ? N8 C92 C93 111.7(3) . . ? N8 C92 H92A 109.3 . . ? C93 C92 H92A 109.3 . . ? N8 C92 H92B 109.3 . . ? C93 C92 H92B 109.3 . . ? H92A C92 H92B 107.9 . . ? C98 C93 C94 118.6(3) . . ? C98 C93 C92 121.6(3) . . ? C94 C93 C92 119.8(3) . . ? O14 C94 C95 120.0(3) . . ? O14 C94 C93 119.3(3) . . ? C95 C94 C93 120.8(3) . . ? C96 C95 C94 118.2(3) . . ? C96 C95 C99 121.6(3) . . ? C94 C95 C99 120.3(3) . . ? C95 C96 C97 122.5(3) . . ? C95 C96 H96 118.7 . . ? C97 C96 H96 118.7 . . ? C98 C97 C96 117.7(3) . . ? C98 C97 C100 121.6(3) . . ? C96 C97 C100 120.7(3) . . ? C93 C98 C97 122.1(3) . . ? C93 C98 H98 118.9 . . ? C97 C98 H98 118.9 . . ? C95 C99 H99A 109.5 . . ? C95 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C95 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C97 C100 H10C 109.5 . . ? C97 C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? C97 C100 H10E 109.5 . . ? H10C C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? O11 C101 C102 110.0(4) . . ? O11 C101 C103 107.9(3) . . ? C102 C101 C103 113.8(4) . . ? O11 C101 H101 108.3 . . ? C102 C101 H101 108.3 . . ? C103 C101 H101 108.3 . . ? C101 C102 H10F 109.5 . . ? C101 C102 H10G 109.5 . . ? H10F C102 H10G 109.5 . . ? C101 C102 H10H 109.5 . . ? H10F C102 H10H 109.5 . . ? H10G C102 H10H 109.5 . . ? C101 C103 H10I 109.5 . . ? C101 C103 H10J 109.5 . . ? H10I C103 H10J 109.5 . . ? C101 C103 H10K 109.5 . . ? H10I C103 H10K 109.5 . . ? H10J C103 H10K 109.5 . . ? O12 C104 C105 110.7(4) . . ? O12 C104 C106 109.9(4) . . ? C105 C104 C106 115.2(6) . . ? O12 C104 H104 106.9 . . ? C105 C104 H104 106.9 . . ? C106 C104 H104 106.9 . . ? C104 C105 H10L 109.5 . . ? C104 C105 H10M 109.5 . . ? H10L C105 H10M 109.5 . . ? C104 C105 H10N 109.5 . . ? H10L C105 H10N 109.5 . . ? H10M C105 H10N 109.5 . . ? C104 C106 H10O 109.5 . . ? C104 C106 H10P 109.5 . . ? H10O C106 H10P 109.5 . . ? C104 C106 H10Q 109.5 . . ? H10O C106 H10Q 109.5 . . ? H10P C106 H10Q 109.5 . . ? C108 C107 O15 113.5(5) . . ? C108 C107 C109 118.2(5) . . ? O15 C107 C109 108.9(4) . . ? C108 C107 H107 105.0 . . ? O15 C107 H107 105.0 . . ? C109 C107 H107 105.0 . . ? C107 C108 H10R 109.5 . . ? C107 C108 H10S 109.5 . . ? H10R C108 H10S 109.5 . . ? C107 C108 H10T 109.5 . . ? H10R C108 H10T 109.5 . . ? H10S C108 H10T 109.5 . . ? C107 C109 H10U 109.5 . . ? C107 C109 H10V 109.5 . . ? H10U C109 H10V 109.5 . . ? C107 C109 H10W 109.5 . . ? H10U C109 H10W 109.5 . . ? H10V C109 H10W 109.5 . . ? O16 C110 C111 108.6(4) . . ? O16 C110 C112 109.3(4) . . ? C111 C110 C112 112.5(4) . . ? O16 C110 H110 108.8 . . ? C111 C110 H110 108.8 . . ? C112 C110 H110 108.8 . . ? C110 C111 H11C 109.5 . . ? C110 C111 H11D 109.5 . . ? H11C C111 H11D 109.5 . . ? C110 C111 H11E 109.5 . . ? H11C C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? C110 C112 H11F 109.5 . . ? C110 C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? C110 C112 H11H 109.5 . . ? H11F C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? C114 C113 C113 116.7(8) . 3_656 ? C114 C113 H11I 108.1 . . ? C113 C113 H11I 108.1 3_656 . ? C114 C113 H11J 108.1 . . ? C113 C113 H11J 108.1 3_656 . ? H11I C113 H11J 107.3 . . ? C113 C114 C115 114.8(7) . . ? C113 C114 H4 108.6 . . ? C115 C114 H4 108.6 . . ? C113 C114 H6 108.6 . . ? C115 C114 H6 108.6 . . ? H4 C114 H6 107.5 . . ? C114 C115 H11K 109.5 . . ? C114 C115 H11L 109.5 . . ? H11K C115 H11L 109.5 . . ? C114 C115 H11M 109.5 . . ? H11K C115 H11M 109.5 . . ? H11L C115 H11M 109.5 . . ? C116 C116 C117 114.9(16) 3_556 . ? C116 C116 H11N 108.6 3_556 . ? C117 C116 H11N 108.6 . . ? C116 C116 H11O 108.6 3_556 . ? C117 C116 H11O 108.6 . . ? H11N C116 H11O 107.5 . . ? C118 C117 C116 120.4(9) . . ? C118 C117 H11P 107.2 . . ? C116 C117 H11P 107.2 . . ? C118 C117 H11Q 107.2 . . ? C116 C117 H11Q 107.2 . . ? H11P C117 H11Q 106.9 . . ? C217 C118 C117 45.0(5) . . ? C217 C118 H1 153.3 . . ? C117 C118 H1 109.5 . . ? C217 C118 H2 90.1 . . ? C117 C118 H2 109.5 . . ? H1 C118 H2 109.5 . . ? C217 C118 H3 79.2 . . ? C117 C118 H3 109.5 . . ? H1 C118 H3 109.5 . . ? H2 C118 H3 109.5 . . ? C118 C217 C216 120.2(11) . . ? C118 C217 H21D 107.3 . . ? C216 C217 H21D 107.3 . . ? C118 C217 H21E 107.3 . . ? C216 C217 H21E 107.3 . . ? H21D C217 H21E 106.9 . . ? C217 C216 C216 113(2) . 3_556 ? C217 C216 H21F 108.9 . . ? C216 C216 H21F 108.9 3_556 . ? C217 C216 H21G 108.9 . . ? C216 C216 H21G 108.9 3_556 . ? H21F C216 H21G 107.7 . . ? 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 C3 14.9(3) . . . . ? O3 Ti1 O1 C3 119.6(3) . . . . ? O2 Ti1 O1 C3 -88.0(3) . . . . ? N3 Ti1 O1 C3 -163.7(3) . . . . ? O4 Ti1 O2 C25 155.6(3) . . . . ? O3 Ti1 O2 C25 51.4(3) . . . . ? O1 Ti1 O2 C25 -101.5(3) . . . . ? N3 Ti1 O2 C25 -25.4(3) . . . . ? O4 Ti1 O3 C45 -3.3(3) . . . . ? O2 Ti1 O3 C45 100.3(3) . . . . ? O1 Ti1 O3 C45 -107.3(3) . . . . ? N3 Ti1 O3 C45 176.4(3) . . . . ? O3 Ti1 O4 C48 -137(4) . . . . ? O2 Ti1 O4 C48 103(4) . . . . ? O1 Ti1 O4 C48 -16(4) . . . . ? N3 Ti1 O4 C48 56(7) . . . . ? O8 Ti2 O5 C38 7.6(3) . . . . ? O7 Ti2 O5 C38 112.3(3) . . . . ? O6 Ti2 O5 C38 -94.5(3) . . . . ? N2 Ti2 O5 C38 -170.5(3) . . . . ? O8 Ti2 O6 C16 176.4(4) . . . . ? O7 Ti2 O6 C16 72.3(4) . . . . ? O5 Ti2 O6 C16 -81.5(4) . . . . ? N2 Ti2 O6 C16 -6.5(3) . . . . ? O8 Ti2 O7 C51 -5.8(4) . . . . ? O6 Ti2 O7 C51 96.3(4) . . . . ? O5 Ti2 O7 C51 -108.6(4) . . . . ? N2 Ti2 O7 C51 175.1(4) . . . . ? O7 Ti2 O8 C54 -152.0(12) . . . . ? O6 Ti2 O8 C54 91.2(12) . . . . ? O5 Ti2 O8 C54 -32.4(12) . . . . ? N2 Ti2 O8 C54 10(3) . . . . ? O12 Ti3 O9 C59 4.9(3) . . . . ? O11 Ti3 O9 C59 109.2(3) . . . . ? O10 Ti3 O9 C59 -97.8(3) . . . . ? N7 Ti3 O9 C59 -172.5(3) . . . . ? O12 Ti3 O10 C81 179.0(4) . . . . ? O11 Ti3 O10 C81 75.1(4) . . . . ? O9 Ti3 O10 C81 -77.6(4) . . . . ? N7 Ti3 O10 C81 -3.6(4) . . . . ? O12 Ti3 O11 C101 -13.0(4) . . . . ? O10 Ti3 O11 C101 89.2(4) . . . . ? O9 Ti3 O11 C101 -116.3(3) . . . . ? N7 Ti3 O11 C101 167.0(3) . . . . ? O11 Ti3 O12 C104 99(15) . . . . ? O10 Ti3 O12 C104 -19(15) . . . . ? O9 Ti3 O12 C104 -143(15) . . . . ? N7 Ti3 O12 C104 -81(15) . . . . ? O15 Ti4 O13 C72 177.1(4) . . . . ? O16 Ti4 O13 C72 72.6(4) . . . . ? O14 Ti4 O13 C72 -81.4(4) . . . . ? N6 Ti4 O13 C72 -6.0(4) . . . . ? O15 Ti4 O14 C94 5.3(3) . . . . ? O16 Ti4 O14 C94 108.8(3) . . . . ? O13 Ti4 O14 C94 -97.0(3) . . . . ? N6 Ti4 O14 C94 -172.8(3) . . . . ? O16 Ti4 O15 C107 162.0(9) . . . . ? O13 Ti4 O15 C107 41.8(9) . . . . ? O14 Ti4 O15 C107 -79.3(9) . . . . ? N6 Ti4 O15 C107 -43(3) . . . . ? O15 Ti4 O16 C110 10.6(4) . . . . ? O13 Ti4 O16 C110 114.2(4) . . . . ? O14 Ti4 O16 C110 -91.1(4) . . . . ? N6 Ti4 O16 C110 -168.1(4) . . . . ? O8 Ti2 N2 C11 0(2) . . . . ? O7 Ti2 N2 C11 162.7(2) . . . . ? O6 Ti2 N2 C11 -80.95(19) . . . . ? O5 Ti2 N2 C11 43.31(19) . . . . ? O8 Ti2 N2 C12 -118(2) . . . . ? O7 Ti2 N2 C12 44.6(2) . . . . ? O6 Ti2 N2 C12 160.9(2) . . . . ? O5 Ti2 N2 C12 -74.8(2) . . . . ? O8 Ti2 N2 C14 124(2) . . . . ? O7 Ti2 N2 C14 -73.9(2) . . . . ? O6 Ti2 N2 C14 42.44(19) . . . . ? O5 Ti2 N2 C14 166.7(2) . . . . ? O4 Ti1 N3 C34 -143(4) . . . . ? O3 Ti1 N3 C34 50.39(18) . . . . ? O2 Ti1 N3 C34 169.91(18) . . . . ? O1 Ti1 N3 C34 -70.50(18) . . . . ? O4 Ti1 N3 C23 98(4) . . . . ? O3 Ti1 N3 C23 -68.82(17) . . . . ? O2 Ti1 N3 C23 50.70(17) . . . . ? O1 Ti1 N3 C23 170.29(18) . . . . ? O4 Ti1 N3 C32 -25(4) . . . . ? O3 Ti1 N3 C32 168.51(19) . . . . ? O2 Ti1 N3 C32 -71.96(18) . . . . ? O1 Ti1 N3 C32 47.62(18) . . . . ? O15 Ti4 N6 C67 5(2) . . . . ? O16 Ti4 N6 C67 160.7(2) . . . . ? O13 Ti4 N6 C67 -79.7(2) . . . . ? O14 Ti4 N6 C67 42.1(2) . . . . ? O15 Ti4 N6 C69 -113(2) . . . . ? O16 Ti4 N6 C69 42.5(2) . . . . ? O13 Ti4 N6 C69 162.1(2) . . . . ? O14 Ti4 N6 C69 -76.2(2) . . . . ? O15 Ti4 N6 C70 129(2) . . . . ? O16 Ti4 N6 C70 -75.8(2) . . . . ? O13 Ti4 N6 C70 43.8(2) . . . . ? O14 Ti4 N6 C70 165.6(2) . . . . ? O12 Ti3 N7 C90 -135(2) . . . . ? O11 Ti3 N7 C90 44.2(2) . . . . ? O10 Ti3 N7 C90 162.5(2) . . . . ? O9 Ti3 N7 C90 -73.13(19) . . . . ? O12 Ti3 N7 C79 107(2) . . . . ? O11 Ti3 N7 C79 -73.7(2) . . . . ? O10 Ti3 N7 C79 44.7(2) . . . . ? O9 Ti3 N7 C79 169.0(2) . . . . ? O12 Ti3 N7 C88 -17(2) . . . . ? O11 Ti3 N7 C88 162.2(2) . . . . ? O10 Ti3 N7 C88 -79.4(2) . . . . ? O9 Ti3 N7 C88 44.9(2) . . . . ? C13 N1 C1 C2 170.9(2) . . . . ? C10 N1 C1 C2 -66.2(3) . . . . ? N1 C1 C2 C7 102.7(3) . . . . ? N1 C1 C2 C3 -74.1(3) . . . . ? Ti1 O1 C3 C4 66.7(4) . . . . ? Ti1 O1 C3 C2 -114.5(3) . . . . ? C7 C2 C3 O1 179.0(3) . . . . ? C1 C2 C3 O1 -4.0(4) . . . . ? C7 C2 C3 C4 -2.2(4) . . . . ? C1 C2 C3 C4 174.7(3) . . . . ? O1 C3 C4 C5 -179.8(3) . . . . ? C2 C3 C4 C5 1.4(4) . . . . ? O1 C3 C4 C8 1.0(4) . . . . ? C2 C3 C4 C8 -177.8(3) . . . . ? C3 C4 C5 C6 0.1(5) . . . . ? C8 C4 C5 C6 179.3(3) . . . . ? C4 C5 C6 C7 -0.8(5) . . . . ? C4 C5 C6 C9 -179.6(3) . . . . ? C5 C6 C7 C2 -0.1(5) . . . . ? C9 C6 C7 C2 178.8(3) . . . . ? C3 C2 C7 C6 1.6(5) . . . . ? C1 C2 C7 C6 -175.3(3) . . . . ? C13 N1 C10 C11 -60.2(3) . . . . ? C1 N1 C10 C11 175.1(2) . . . . ? C12 N2 C11 C10 -52.2(3) . . . . ? C14 N2 C11 C10 68.7(3) . . . . ? Ti2 N2 C11 C10 -171.38(19) . . . . ? N1 C10 C11 N2 58.9(3) . . . . ? C11 N2 C12 C13 51.4(3) . . . . ? C14 N2 C12 C13 -71.1(3) . . . . ? Ti2 N2 C12 C13 172.5(2) . . . . ? C10 N1 C13 C12 59.4(3) . . . . ? C1 N1 C13 C12 -175.7(2) . . . . ? N2 C12 C13 N1 -57.2(3) . . . . ? C11 N2 C14 C15 54.7(3) . . . . ? C12 N2 C14 C15 174.0(3) . . . . ? Ti2 N2 C14 C15 -68.2(3) . . . . ? N2 C14 C15 C20 -132.4(3) . . . . ? N2 C14 C15 C16 51.5(4) . . . . ? Ti2 O6 C16 C15 -12.7(5) . . . . ? Ti2 O6 C16 C17 168.3(3) . . . . ? C20 C15 C16 O6 178.7(3) . . . . ? C14 C15 C16 O6 -5.0(4) . . . . ? C20 C15 C16 C17 -2.3(5) . . . . ? C14 C15 C16 C17 173.9(3) . . . . ? O6 C16 C17 C18 -178.9(3) . . . . ? C15 C16 C17 C18 2.2(5) . . . . ? O6 C16 C17 C21 2.1(5) . . . . ? C15 C16 C17 C21 -176.8(3) . . . . ? C16 C17 C18 C19 -0.4(5) . . . . ? C21 C17 C18 C19 178.6(3) . . . . ? C17 C18 C19 C20 -1.2(5) . . . . ? C17 C18 C19 C22 179.5(3) . . . . ? C16 C15 C20 C19 0.7(5) . . . . ? C14 C15 C20 C19 -175.5(3) . . . . ? C18 C19 C20 C15 1.0(5) . . . . ? C22 C19 C20 C15 -179.7(3) . . . . ? C34 N3 C23 C24 174.3(2) . . . . ? C32 N3 C23 C24 54.6(3) . . . . ? Ti1 N3 C23 C24 -67.4(3) . . . . ? N3 C23 C24 C25 43.2(4) . . . . ? N3 C23 C24 C29 -141.8(3) . . . . ? Ti1 O2 C25 C24 4.0(5) . . . . ? Ti1 O2 C25 C26 -175.7(2) . . . . ? C29 C24 C25 O2 -177.9(3) . . . . ? C23 C24 C25 O2 -2.9(4) . . . . ? C29 C24 C25 C26 1.8(4) . . . . ? C23 C24 C25 C26 176.8(3) . . . . ? O2 C25 C26 C27 176.9(3) . . . . ? C24 C25 C26 C27 -2.8(5) . . . . ? O2 C25 C26 C30 -0.8(5) . . . . ? C24 C25 C26 C30 179.5(3) . . . . ? C25 C26 C27 C28 0.6(5) . . . . ? C30 C26 C27 C28 178.2(3) . . . . ? C26 C27 C28 C29 2.5(5) . . . . ? C26 C27 C28 C31 -175.7(3) . . . . ? C25 C24 C29 C28 1.5(5) . . . . ? C23 C24 C29 C28 -173.7(3) . . . . ? C27 C28 C29 C24 -3.6(5) . . . . ? C31 C28 C29 C24 174.6(3) . . . . ? C34 N3 C32 C33 -52.2(3) . . . . ? C23 N3 C32 C33 69.4(3) . . . . ? Ti1 N3 C32 C33 -171.52(19) . . . . ? C35 N4 C33 C32 -60.6(3) . . . . ? C36 N4 C33 C32 175.2(2) . . . . ? N3 C32 C33 N4 58.7(3) . . . . ? C23 N3 C34 C35 -70.9(3) . . . . ? C32 N3 C34 C35 51.9(3) . . . . ? Ti1 N3 C34 C35 172.64(19) . . . . ? C33 N4 C35 C34 59.6(3) . . . . ? C36 N4 C35 C34 -176.1(2) . . . . ? N3 C34 C35 N4 -57.6(3) . . . . ? C33 N4 C36 C37 -65.3(3) . . . . ? C35 N4 C36 C37 172.0(3) . . . . ? N4 C36 C37 C42 102.8(3) . . . . ? N4 C36 C37 C38 -73.6(4) . . . . ? Ti2 O5 C38 C37 -105.9(3) . . . . ? Ti2 O5 C38 C39 75.2(4) . . . . ? C42 C37 C38 O5 179.5(3) . . . . ? C36 C37 C38 O5 -4.0(4) . . . . ? C42 C37 C38 C39 -1.6(5) . . . . ? C36 C37 C38 C39 174.9(3) . . . . ? O5 C38 C39 C40 -179.8(3) . . . . ? C37 C38 C39 C40 1.3(5) . . . . ? O5 C38 C39 C43 -0.2(5) . . . . ? C37 C38 C39 C43 -179.1(3) . . . . ? C38 C39 C40 C41 0.1(6) . . . . ? C43 C39 C40 C41 -179.5(4) . . . . ? C39 C40 C41 C42 -1.1(6) . . . . ? C39 C40 C41 C44 -178.8(4) . . . . ? C40 C41 C42 C37 0.7(6) . . . . ? C44 C41 C42 C37 178.5(4) . . . . ? C38 C37 C42 C41 0.6(5) . . . . ? C36 C37 C42 C41 -175.9(3) . . . . ? Ti1 O3 C45 C46 85.1(4) . . . . ? Ti1 O3 C45 C47 -151.8(3) . . . . ? Ti1 O4 C48 C50 -79(4) . . . . ? Ti1 O4 C48 C49 47(4) . . . . ? Ti2 O7 C51 C53 100.1(5) . . . . ? Ti2 O7 C51 C52 -134.6(4) . . . . ? Ti2 O8 C54 C55 -118.3(11) . . . . ? Ti2 O8 C54 C56 110.3(12) . . . . ? C68 N5 C57 C58 171.8(3) . . . . ? C66 N5 C57 C58 -65.4(4) . . . . ? N5 C57 C58 C63 108.3(4) . . . . ? N5 C57 C58 C59 -71.0(4) . . . . ? Ti3 O9 C59 C58 -106.1(3) . . . . ? Ti3 O9 C59 C60 73.7(4) . . . . ? C63 C58 C59 O9 178.1(3) . . . . ? C57 C58 C59 O9 -2.5(5) . . . . ? C63 C58 C59 C60 -1.8(5) . . . . ? C57 C58 C59 C60 177.6(3) . . . . ? O9 C59 C60 C61 -176.8(3) . . . . ? C58 C59 C60 C61 3.0(5) . . . . ? O9 C59 C60 C64 3.0(5) . . . . ? C58 C59 C60 C64 -177.1(3) . . . . ? C59 C60 C61 C62 -2.3(5) . . . . ? C64 C60 C61 C62 177.9(3) . . . . ? C60 C61 C62 C63 0.2(5) . . . . ? C60 C61 C62 C65 -178.5(4) . . . . ? C59 C58 C63 C62 -0.4(5) . . . . ? C57 C58 C63 C62 -179.8(3) . . . . ? C61 C62 C63 C58 1.2(5) . . . . ? C65 C62 C63 C58 179.9(3) . . . . ? C68 N5 C66 C67 -61.0(4) . . . . ? C57 N5 C66 C67 175.3(3) . . . . ? C69 N6 C67 C66 -52.0(3) . . . . ? C70 N6 C67 C66 69.1(4) . . . . ? Ti4 N6 C67 C66 -170.9(2) . . . . ? N5 C66 C67 N6 59.0(4) . . . . ? C66 N5 C68 C69 60.6(3) . . . . ? C57 N5 C68 C69 -174.7(3) . . . . ? C67 N6 C69 C68 50.9(4) . . . . ? C70 N6 C69 C68 -71.5(4) . . . . ? Ti4 N6 C69 C68 172.8(2) . . . . ? N5 C68 C69 N6 -57.2(4) . . . . ? C67 N6 C70 C71 54.2(4) . . . . ? C69 N6 C70 C71 173.4(3) . . . . ? Ti4 N6 C70 C71 -69.7(3) . . . . ? N6 C70 C71 C72 51.2(4) . . . . ? N6 C70 C71 C76 -132.1(4) . . . . ? Ti4 O13 C72 C71 -14.9(6) . . . . ? Ti4 O13 C72 C73 165.6(3) . . . . ? C76 C71 C72 O13 -179.9(3) . . . . ? C70 C71 C72 O13 -3.1(5) . . . . ? C76 C71 C72 C73 -0.4(6) . . . . ? C70 C71 C72 C73 176.3(3) . . . . ? O13 C72 C73 C74 179.3(4) . . . . ? C71 C72 C73 C74 -0.2(6) . . . . ? O13 C72 C73 C77 0.2(6) . . . . ? C71 C72 C73 C77 -179.3(4) . . . . ? C72 C73 C74 C75 -0.2(7) . . . . ? C77 C73 C74 C75 178.9(4) . . . . ? C73 C74 C75 C76 1.3(7) . . . . ? C73 C74 C75 C78 -177.9(4) . . . . ? C74 C75 C76 C71 -1.9(6) . . . . ? C78 C75 C76 C71 177.3(4) . . . . ? C72 C71 C76 C75 1.5(6) . . . . ? C70 C71 C76 C75 -175.2(4) . . . . ? C90 N7 C79 C80 171.5(3) . . . . ? C88 N7 C79 C80 52.2(4) . . . . ? Ti3 N7 C79 C80 -71.8(3) . . . . ? N7 C79 C80 C81 51.5(4) . . . . ? N7 C79 C80 C85 -128.4(3) . . . . ? Ti3 O10 C81 C80 -19.5(6) . . . . ? Ti3 O10 C81 C82 160.3(3) . . . . ? C85 C80 C81 O10 179.3(3) . . . . ? C79 C80 C81 O10 -0.6(5) . . . . ? C85 C80 C81 C82 -0.5(6) . . . . ? C79 C80 C81 C82 179.6(3) . . . . ? O10 C81 C82 C83 -179.4(4) . . . . ? C80 C81 C82 C83 0.4(6) . . . . ? O10 C81 C82 C86 0.3(6) . . . . ? C80 C81 C82 C86 -179.8(4) . . . . ? C81 C82 C83 C84 -0.2(7) . . . . ? C86 C82 C83 C84 -180.0(4) . . . . ? C82 C83 C84 C85 0.1(7) . . . . ? C82 C83 C84 C87 179.6(4) . . . . ? C83 C84 C85 C80 -0.2(6) . . . . ? C87 C84 C85 C80 -179.6(4) . . . . ? C81 C80 C85 C84 0.4(6) . . . . ? C79 C80 C85 C84 -179.7(3) . . . . ? C90 N7 C88 C89 -52.0(3) . . . . ? C79 N7 C88 C89 69.2(3) . . . . ? Ti3 N7 C88 C89 -170.7(2) . . . . ? C91 N8 C89 C88 -60.4(3) . . . . ? C92 N8 C89 C88 177.9(2) . . . . ? N7 C88 C89 N8 58.9(3) . . . . ? C79 N7 C90 C91 -72.0(3) . . . . ? C88 N7 C90 C91 51.0(3) . . . . ? Ti3 N7 C90 C91 172.7(2) . . . . ? C92 N8 C91 C90 -176.4(3) . . . . ? C89 N8 C91 C90 60.9(3) . . . . ? N7 C90 C91 N8 -58.4(3) . . . . ? C91 N8 C92 C93 171.7(3) . . . . ? C89 N8 C92 C93 -68.1(3) . . . . ? N8 C92 C93 C98 110.8(3) . . . . ? N8 C92 C93 C94 -68.4(4) . . . . ? Ti4 O14 C94 C95 76.5(4) . . . . ? Ti4 O14 C94 C93 -103.7(3) . . . . ? C98 C93 C94 O14 176.5(3) . . . . ? C92 C93 C94 O14 -4.2(4) . . . . ? C98 C93 C94 C95 -3.6(5) . . . . ? C92 C93 C94 C95 175.6(3) . . . . ? O14 C94 C95 C96 -176.6(3) . . . . ? C93 C94 C95 C96 3.6(5) . . . . ? O14 C94 C95 C99 2.7(5) . . . . ? C93 C94 C95 C99 -177.1(3) . . . . ? C94 C95 C96 C97 -0.2(5) . . . . ? C99 C95 C96 C97 -179.5(3) . . . . ? C95 C96 C97 C98 -3.0(5) . . . . ? C95 C96 C97 C100 177.0(4) . . . . ? C94 C93 C98 C97 0.3(5) . . . . ? C92 C93 C98 C97 -179.0(3) . . . . ? C96 C97 C98 C93 3.0(5) . . . . ? C100 C97 C98 C93 -177.0(3) . . . . ? Ti3 O11 C101 C102 96.9(5) . . . . ? Ti3 O11 C101 C103 -138.4(3) . . . . ? Ti3 O12 C104 C105 49(15) . . . . ? Ti3 O12 C104 C106 177(100) . . . . ? Ti4 O15 C107 C108 -98.1(11) . . . . ? Ti4 O15 C107 C109 128.0(8) . . . . ? Ti4 O16 C110 C111 -94.8(5) . . . . ? Ti4 O16 C110 C112 142.2(4) . . . . ? C113 C113 C114 C115 -177.5(7) 3_656 . . . ? C116 C116 C117 C118 178.3(8) 3_556 . . . ? C116 C117 C118 C217 -6.4(8) . . . . ? C117 C118 C217 C216 2.2(8) . . . . ? C118 C217 C216 C216 174.3(10) . . . 3_556 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.644 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.056 #===END data_Ti2(2)(OiPr)6 _database_code_depnum_ccdc_archive 'CCDC 800218' #TrackingRef '- cif-DT-ART-11-2010-001542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H82 N2 O8 Ti2' _chemical_formula_weight 886.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.5960(5) _cell_length_b 23.1890(14) _cell_length_c 11.4210(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.398(3) _cell_angle_gamma 90.00 _cell_volume 2540.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 58823 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.362 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9311 _exptl_absorpt_correction_T_max 0.9647 _exptl_absorpt_process_details 'Sortav (Blessing 1995)' _exptl_special_details ; the tBu group C17-c18 was disordered over two poisitions in a 60:40 ratio ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27064 _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5764 _reflns_number_gt 4253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0694P)^2^+1.4482P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5764 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1525 _refine_ls_wR_factor_gt 0.1373 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.23800(4) 0.117329(18) 0.50175(4) 0.03170(14) Uani 1 1 d . . . O1 O 0.0845(2) 0.16041(10) 0.49216(18) 0.0507(5) Uani 1 1 d . . . N1 N 0.43231(18) 0.05667(8) 0.52872(16) 0.0273(4) Uani 1 1 d . . . C1 C -0.0318(5) 0.1960(3) 0.5066(5) 0.131(3) Uani 1 1 d . . . H1 H 0.0184 0.2330 0.5235 0.158 Uiso 1 1 calc R . . O2 O 0.35704(19) 0.16233(8) 0.42223(17) 0.0423(4) Uani 1 1 d . . . C2 C -0.0983(6) 0.1906(4) 0.6099(5) 0.139(3) Uani 1 1 d . . . H2A H -0.1378 0.1517 0.6156 0.208 Uiso 1 1 calc R . . H2B H -0.1733 0.2192 0.6134 0.208 Uiso 1 1 calc R . . H2C H -0.0317 0.1969 0.6750 0.208 Uiso 1 1 calc R . . O3 O 0.17455(16) 0.05434(8) 0.41892(15) 0.0365(4) Uani 1 1 d . . . C3 C -0.0976(5) 0.2120(3) 0.3962(5) 0.117(2) Uani 1 1 d . . . H3A H -0.0262 0.2242 0.3415 0.176 Uiso 1 1 calc R . . H3B H -0.1628 0.2438 0.4086 0.176 Uiso 1 1 calc R . . H3C H -0.1483 0.1787 0.3635 0.176 Uiso 1 1 calc R . . O4 O 0.25555(16) 0.11812(8) 0.66678(15) 0.0353(4) Uani 1 1 d . . . C4 C 0.3610(3) 0.22022(11) 0.3788(3) 0.0433(6) Uani 1 1 d . . . H4 H 0.3069 0.2455 0.4321 0.052 Uiso 1 1 calc R . . C5 C 0.2950(4) 0.22310(15) 0.2570(3) 0.0602(8) Uani 1 1 d . . . H5A H 0.3500 0.2000 0.2031 0.090 Uiso 1 1 calc R . . H5B H 0.2926 0.2633 0.2303 0.090 Uiso 1 1 calc R . . H5C H 0.1998 0.2079 0.2588 0.090 Uiso 1 1 calc R . . C6 C 0.5107(3) 0.23978(14) 0.3811(4) 0.0606(8) Uani 1 1 d . . . H6A H 0.5482 0.2382 0.4616 0.091 Uiso 1 1 calc R . . H6B H 0.5159 0.2795 0.3520 0.091 Uiso 1 1 calc R . . H6C H 0.5654 0.2144 0.3312 0.091 Uiso 1 1 calc R . . C7 C 0.0703(3) 0.04608(14) 0.3302(3) 0.0506(7) Uani 1 1 d . . . H7 H -0.0128 0.0703 0.3479 0.061 Uiso 1 1 calc R . . C8 C 0.0283(3) -0.01642(16) 0.3273(3) 0.0578(8) Uani 1 1 d . . . H8A H 0.1077 -0.0400 0.3038 0.087 Uiso 1 1 calc R . . H8B H -0.0492 -0.0217 0.2708 0.087 Uiso 1 1 calc R . . H8C H -0.0009 -0.0283 0.4053 0.087 Uiso 1 1 calc R . . C9 C 0.1277(6) 0.0643(2) 0.2127(3) 0.0991(17) Uani 1 1 d . . . H9A H 0.1504 0.1055 0.2149 0.149 Uiso 1 1 calc R . . H9B H 0.0576 0.0571 0.1506 0.149 Uiso 1 1 calc R . . H9C H 0.2120 0.0420 0.1971 0.149 Uiso 1 1 calc R . . C10 C 0.3524(2) 0.11160(10) 0.7526(2) 0.0305(5) Uani 1 1 d . . . C11 C 0.3144(2) 0.11864(11) 0.8697(2) 0.0342(5) Uani 1 1 d . . . C12 C 0.4164(3) 0.11310(11) 0.9580(2) 0.0368(5) Uani 1 1 d . . . H12 H 0.3903 0.1185 1.0369 0.044 Uiso 1 1 calc R . . C13 C 0.5555(3) 0.09995(11) 0.9355(2) 0.0344(5) Uani 1 1 d . A . C14 C 0.5883(2) 0.09142(10) 0.8187(2) 0.0322(5) Uani 1 1 d . . . H14 H 0.6811 0.0812 0.8005 0.039 Uiso 1 1 calc R . . C15 C 0.4906(2) 0.09730(10) 0.7276(2) 0.0297(5) Uani 1 1 d . . . C16 C 0.1657(3) 0.13227(13) 0.8971(2) 0.0440(6) Uani 1 1 d . . . H16A H 0.1591 0.1416 0.9805 0.066 Uiso 1 1 calc R . . H16B H 0.1069 0.0988 0.8787 0.066 Uiso 1 1 calc R . . H16C H 0.1340 0.1653 0.8501 0.066 Uiso 1 1 calc R . . C17 C 0.6672(3) 0.09450(12) 1.0328(2) 0.0402(6) Uani 1 1 d . . . C18 C 0.6315(7) 0.1356(4) 1.1393(5) 0.076(2) Uani 0.60 1 d P A 1 H18A H 0.5437 0.1232 1.1734 0.113 Uiso 0.60 1 calc PR A 1 H18B H 0.6223 0.1754 1.1111 0.113 Uiso 0.60 1 calc PR A 1 H18C H 0.7066 0.1335 1.1989 0.113 Uiso 0.60 1 calc PR A 1 C19 C 0.6699(7) 0.0349(3) 1.0786(6) 0.0690(17) Uani 0.60 1 d P A 1 H19A H 0.7468 0.0308 1.1360 0.104 Uiso 0.60 1 calc PR A 1 H19B H 0.6831 0.0078 1.0139 0.104 Uiso 0.60 1 calc PR A 1 H19C H 0.5815 0.0265 1.1163 0.104 Uiso 0.60 1 calc PR A 1 C20 C 0.8080(8) 0.1132(5) 0.9937(7) 0.087(3) Uani 0.60 1 d P A 1 H20D H 0.8743 0.1119 1.0603 0.130 Uiso 0.60 1 calc PR A 1 H20E H 0.8022 0.1527 0.9633 0.130 Uiso 0.60 1 calc PR A 1 H20F H 0.8395 0.0873 0.9320 0.130 Uiso 0.60 1 calc PR A 1 C21 C 0.5355(2) 0.08922(10) 0.6029(2) 0.0300(5) Uani 1 1 d . . . H21A H 0.5506 0.1276 0.5673 0.036 Uiso 1 1 calc R . . H21B H 0.6255 0.0684 0.6034 0.036 Uiso 1 1 calc R . . C22 C 0.4936(2) 0.04393(10) 0.41258(19) 0.0294(5) Uani 1 1 d . . . H22A H 0.5309 0.0801 0.3797 0.035 Uiso 1 1 calc R . . H22B H 0.4188 0.0300 0.3585 0.035 Uiso 1 1 calc R . . C23 C 0.6097(2) -0.00080(10) 0.41814(19) 0.0282(4) Uani 1 1 d . . . H23A H 0.6418 -0.0081 0.3378 0.034 Uiso 1 1 calc R . . H23B H 0.6894 0.0152 0.4643 0.034 Uiso 1 1 calc R . . C18A C 0.6099(10) 0.0791(7) 1.1469(7) 0.083(4) Uani 0.40 1 d P A 2 H18D H 0.5436 0.0472 1.1367 0.125 Uiso 0.40 1 calc PR A 2 H18E H 0.5621 0.1126 1.1796 0.125 Uiso 0.40 1 calc PR A 2 H18F H 0.6859 0.0672 1.2005 0.125 Uiso 0.40 1 calc PR A 2 C19A C 0.7633(10) 0.0370(4) 1.0052(8) 0.063(2) Uani 0.40 1 d P A 2 H19D H 0.8305 0.0309 1.0700 0.095 Uiso 0.40 1 calc PR A 2 H19E H 0.8134 0.0431 0.9325 0.095 Uiso 0.40 1 calc PR A 2 H19F H 0.7029 0.0031 0.9968 0.095 Uiso 0.40 1 calc PR A 2 C20A C 0.7672(15) 0.1418(5) 1.0249(12) 0.075(4) Uani 0.40 1 d P A 2 H20A H 0.8473 0.1342 1.0775 0.113 Uiso 0.40 1 calc PR A 2 H20B H 0.7224 0.1780 1.0477 0.113 Uiso 0.40 1 calc PR A 2 H20C H 0.7989 0.1450 0.9442 0.113 Uiso 0.40 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0288(2) 0.0280(2) 0.0381(2) 0.00108(18) -0.00279(16) 0.00370(16) O1 0.0376(10) 0.0554(13) 0.0589(12) 0.0021(10) -0.0050(9) 0.0201(9) N1 0.0287(9) 0.0252(9) 0.0279(9) -0.0019(7) 0.0001(7) 0.0017(7) C1 0.090(3) 0.191(7) 0.115(4) 0.032(4) 0.033(3) 0.099(4) O2 0.0415(10) 0.0273(9) 0.0582(11) 0.0099(8) 0.0016(8) 0.0032(7) C2 0.115(4) 0.193(7) 0.109(4) 0.018(4) 0.036(3) 0.091(5) O3 0.0319(8) 0.0382(9) 0.0391(9) 0.0007(7) -0.0085(7) -0.0020(7) C3 0.084(3) 0.135(5) 0.131(5) 0.010(4) -0.024(3) 0.059(3) O4 0.0296(8) 0.0376(9) 0.0385(9) -0.0067(7) -0.0011(7) 0.0064(7) C4 0.0447(14) 0.0265(12) 0.0590(16) 0.0043(11) 0.0057(12) 0.0024(10) C5 0.071(2) 0.0428(17) 0.067(2) 0.0125(15) -0.0029(16) 0.0021(15) C6 0.0553(18) 0.0363(16) 0.090(2) 0.0010(16) 0.0018(17) -0.0073(13) C7 0.0377(14) 0.0514(17) 0.0615(18) -0.0083(14) -0.0208(12) 0.0023(12) C8 0.0546(17) 0.065(2) 0.0541(18) -0.0125(15) 0.0025(14) -0.0227(15) C9 0.135(4) 0.101(4) 0.059(2) 0.034(2) -0.048(2) -0.052(3) C10 0.0307(11) 0.0260(11) 0.0348(11) -0.0045(9) -0.0008(9) -0.0012(9) C11 0.0348(12) 0.0302(12) 0.0377(12) -0.0040(10) 0.0035(9) -0.0018(9) C12 0.0420(13) 0.0353(13) 0.0333(12) -0.0014(10) 0.0056(10) -0.0049(10) C13 0.0386(13) 0.0337(12) 0.0308(12) 0.0026(9) -0.0006(9) -0.0042(10) C14 0.0304(11) 0.0297(12) 0.0366(12) -0.0009(9) 0.0002(9) -0.0004(9) C15 0.0323(11) 0.0245(10) 0.0324(11) -0.0042(9) 0.0008(9) -0.0007(9) C16 0.0363(13) 0.0518(17) 0.0441(14) -0.0101(12) 0.0062(11) -0.0007(11) C17 0.0421(14) 0.0444(14) 0.0337(13) 0.0029(11) -0.0044(10) -0.0036(11) C18 0.074(4) 0.099(5) 0.052(3) -0.034(3) -0.028(3) 0.028(4) C19 0.077(4) 0.057(3) 0.071(4) 0.019(3) -0.036(3) -0.008(3) C20 0.045(4) 0.166(11) 0.047(4) 0.019(5) -0.011(3) -0.033(5) C21 0.0264(10) 0.0310(12) 0.0326(11) -0.0040(9) -0.0012(8) 0.0007(9) C22 0.0323(11) 0.0275(11) 0.0284(11) 0.0020(8) -0.0002(9) 0.0024(9) C23 0.0295(11) 0.0269(11) 0.0281(10) 0.0012(9) 0.0006(8) 0.0015(9) C18A 0.066(6) 0.150(12) 0.034(4) 0.018(5) 0.000(4) 0.024(7) C19A 0.067(5) 0.060(5) 0.063(5) -0.002(4) -0.024(4) 0.015(4) C20A 0.088(10) 0.058(7) 0.078(9) 0.024(6) -0.045(7) -0.028(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 O1 1.7813(18) . ? Ti1 O2 1.8080(18) . ? Ti1 O3 1.8360(18) . ? Ti1 O4 1.8883(17) . ? Ti1 N1 2.3499(18) . ? O1 C1 1.400(4) . ? N1 C23 1.490(3) 3_656 ? N1 C21 1.492(3) . ? N1 C22 1.494(3) . ? C1 C2 1.360(7) . ? C1 C3 1.445(7) . ? C1 H1 1.0000 . ? O2 C4 1.432(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C7 1.420(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C10 1.343(3) . ? C4 C6 1.506(4) . ? C4 C5 1.516(4) . ? 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 C8 1.504(5) . ? C7 C9 1.522(5) . ? C7 H7 1.0000 . ? 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 C15 1.403(3) . ? C10 C11 1.404(3) . ? C11 C12 1.394(4) . ? C11 C16 1.503(3) . ? C12 C13 1.399(3) . ? C12 H12 0.9500 . ? C13 C14 1.392(3) . ? C13 C17 1.531(3) . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 C21 1.511(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20A 1.462(12) . ? C17 C18A 1.471(9) . ? C17 C19 1.478(6) . ? C17 C20 1.497(8) . ? C17 C18 1.588(6) . ? C17 C19A 1.655(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20D 0.9800 . ? C20 H20E 0.9800 . ? C20 H20F 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.522(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N1 1.491(3) 3_656 ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 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 O1 Ti1 O2 100.21(9) . . ? O1 Ti1 O3 98.69(9) . . ? O2 Ti1 O3 113.95(9) . . ? O1 Ti1 O4 96.28(9) . . ? O2 Ti1 O4 116.98(9) . . ? O3 Ti1 O4 122.85(8) . . ? O1 Ti1 N1 175.03(9) . . ? O2 Ti1 N1 84.39(7) . . ? O3 Ti1 N1 80.99(7) . . ? O4 Ti1 N1 79.86(7) . . ? C1 O1 Ti1 169.5(3) . . ? C23 N1 C21 113.02(17) 3_656 . ? C23 N1 C22 107.83(17) 3_656 . ? C21 N1 C22 109.50(17) . . ? C23 N1 Ti1 110.60(12) 3_656 . ? C21 N1 Ti1 106.55(13) . . ? C22 N1 Ti1 109.30(13) . . ? C2 C1 O1 116.1(5) . . ? C2 C1 C3 125.2(5) . . ? O1 C1 C3 112.3(4) . . ? C2 C1 H1 98.4 . . ? O1 C1 H1 98.4 . . ? C3 C1 H1 98.4 . . ? C4 O2 Ti1 137.50(16) . . ? 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 . . ? C7 O3 Ti1 133.97(17) . . ? 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 . . ? C10 O4 Ti1 140.43(15) . . ? O2 C4 C6 108.0(2) . . ? O2 C4 C5 110.2(2) . . ? C6 C4 C5 112.3(3) . . ? O2 C4 H4 108.7 . . ? C6 C4 H4 108.7 . . ? C5 C4 H4 108.7 . . ? 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 C8 109.2(2) . . ? O3 C7 C9 109.1(3) . . ? C8 C7 C9 110.5(3) . . ? O3 C7 H7 109.3 . . ? C8 C7 H7 109.3 . . ? C9 C7 H7 109.3 . . ? 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 . . ? O4 C10 C15 121.3(2) . . ? O4 C10 C11 119.4(2) . . ? C15 C10 C11 119.3(2) . . ? C12 C11 C10 119.0(2) . . ? C12 C11 C16 121.5(2) . . ? C10 C11 C16 119.5(2) . . ? C11 C12 C13 122.9(2) . . ? C11 C12 H12 118.6 . . ? C13 C12 H12 118.6 . . ? C14 C13 C12 116.5(2) . . ? C14 C13 C17 120.9(2) . . ? C12 C13 C17 122.6(2) . . ? C15 C14 C13 122.6(2) . . ? C15 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? C14 C15 C10 119.7(2) . . ? C14 C15 C21 119.4(2) . . ? C10 C15 C21 120.9(2) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20A C17 C18A 119.8(8) . . ? C20A C17 C19 135.9(6) . . ? C18A C17 C19 57.5(6) . . ? C20A C17 C20 33.5(6) . . ? C18A C17 C20 134.0(6) . . ? C19 C17 C20 111.7(6) . . ? C20A C17 C13 110.0(5) . . ? C18A C17 C13 113.2(4) . . ? C19 C17 C13 109.9(3) . . ? C20 C17 C13 112.3(4) . . ? C20A C17 C18 75.6(7) . . ? C18A C17 C18 51.3(6) . . ? C19 C17 C18 107.0(5) . . ? C20 C17 C18 105.5(5) . . ? C13 C17 C18 110.2(3) . . ? C20A C17 C19A 102.9(7) . . ? C18A C17 C19A 101.3(7) . . ? C19 C17 C19A 46.3(4) . . ? C20 C17 C19A 70.5(6) . . ? C13 C17 C19A 108.1(3) . . ? C18 C17 C19A 139.5(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? C17 C20 H20D 109.5 . . ? C17 C20 H20E 109.5 . . ? C17 C20 H20F 109.5 . . ? N1 C21 C15 113.43(18) . . ? N1 C21 H21A 108.9 . . ? C15 C21 H21A 108.9 . . ? N1 C21 H21B 108.9 . . ? C15 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? N1 C22 C23 113.67(18) . . ? N1 C22 H22A 108.8 . . ? C23 C22 H22A 108.8 . . ? N1 C22 H22B 108.8 . . ? C23 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? N1 C23 C22 113.84(17) 3_656 . ? N1 C23 H23A 108.8 3_656 . ? C22 C23 H23A 108.8 . . ? N1 C23 H23B 108.8 3_656 . ? C22 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C17 C18A H18D 109.5 . . ? C17 C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C17 C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C17 C19A H19D 109.5 . . ? C17 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C17 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C17 C20A H20A 109.5 . . ? C17 C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C17 C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.575 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.059 #===END data_Ti2(3)(OiPr)6 _database_code_depnum_ccdc_archive 'CCDC 800219' #TrackingRef '- cif-DT-ART-11-2010-001542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H94 N2 O8 Ti2' _chemical_formula_weight 971.09 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8260(6) _cell_length_b 18.8930(9) _cell_length_c 14.5330(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.050(2) _cell_angle_gamma 90.00 _cell_volume 2883.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25539 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.324 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42193 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 24.00 _reflns_number_total 4506 _reflns_number_gt 3430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0266P)^2^+2.2256P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4506 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.19932(4) 0.15791(2) 1.08768(3) 0.02695(14) Uani 1 1 d . . . O1 O 0.30224(17) 0.22310(9) 1.15337(13) 0.0372(5) Uani 1 1 d . . . N1 N 0.07170(18) 0.06831(10) 0.99994(14) 0.0235(5) Uani 1 1 d . . . C1 C 0.3892(3) 0.27525(15) 1.2008(2) 0.0505(8) Uani 1 1 d . . . H1 H 0.3631 0.2881 1.2601 0.061 Uiso 1 1 calc R . . O2 O 0.05082(16) 0.20684(8) 1.06163(12) 0.0331(4) Uani 1 1 d . . . C2 C 0.5199(3) 0.24536(18) 1.2301(3) 0.0603(10) Uani 1 1 d . . . H2A H 0.5188 0.2025 1.2679 0.090 Uiso 1 1 calc R . . H2B H 0.5772 0.2804 1.2681 0.090 Uiso 1 1 calc R . . H2C H 0.5500 0.2335 1.1736 0.090 Uiso 1 1 calc R . . O3 O 0.21173(16) 0.09205(9) 1.18198(12) 0.0320(4) Uani 1 1 d . . . C3 C 0.3782(3) 0.34028(16) 1.1420(3) 0.0705(11) Uani 1 1 d . . . H3A H 0.4002 0.3293 1.0821 0.106 Uiso 1 1 calc R . . H3B H 0.4365 0.3764 1.1763 0.106 Uiso 1 1 calc R . . H3C H 0.2906 0.3580 1.1290 0.106 Uiso 1 1 calc R . . O4 O 0.28212(15) 0.14853(9) 0.98912(12) 0.0311(4) Uani 1 1 d . . . C4 C -0.0043(4) 0.32263(18) 1.0035(3) 0.0800(12) Uani 1 1 d . . . H4A H 0.0770 0.3250 0.9853 0.120 Uiso 1 1 calc R . . H4B H -0.0279 0.3700 1.0206 0.120 Uiso 1 1 calc R . . H4C H -0.0704 0.3046 0.9500 0.120 Uiso 1 1 calc R . . C5 C 0.0085(3) 0.27370(13) 1.0872(2) 0.0385(7) Uani 1 1 d . . . H5 H 0.0748 0.2932 1.1415 0.046 Uiso 1 1 calc R . . C6 C -0.1127(3) 0.26436(18) 1.1183(3) 0.0602(9) Uani 1 1 d . . . H6A H -0.1800 0.2479 1.0646 0.090 Uiso 1 1 calc R . . H6B H -0.1378 0.3097 1.1410 0.090 Uiso 1 1 calc R . . H6C H -0.0997 0.2294 1.1696 0.090 Uiso 1 1 calc R . . C7 C 0.1702(3) 0.14212(17) 1.3233(2) 0.0518(8) Uani 1 1 d . . . H7A H 0.1734 0.1905 1.2996 0.078 Uiso 1 1 calc R . . H7B H 0.1987 0.1421 1.3926 0.078 Uiso 1 1 calc R . . H7C H 0.0826 0.1244 1.3042 0.078 Uiso 1 1 calc R . . C8 C 0.2561(3) 0.09506(13) 1.28241(18) 0.0321(6) Uani 1 1 d . . . H8 H 0.3439 0.1155 1.2986 0.038 Uiso 1 1 calc R . . C9 C 0.2618(3) 0.02076(15) 1.3206(2) 0.0440(7) Uani 1 1 d . . . H9A H 0.1753 0.0018 1.3104 0.066 Uiso 1 1 calc R . . H9B H 0.3024 0.0211 1.3887 0.066 Uiso 1 1 calc R . . H9C H 0.3114 -0.0090 1.2876 0.066 Uiso 1 1 calc R . . C10 C 0.2792(2) 0.11236(12) 0.90792(18) 0.0271(6) Uani 1 1 d . . . C11 C 0.3890(2) 0.10594(12) 0.87296(18) 0.0276(6) Uani 1 1 d . . . C12 C 0.3782(2) 0.06493(13) 0.79126(18) 0.0307(6) Uani 1 1 d . . . H12 H 0.4515 0.0599 0.7668 0.037 Uiso 1 1 calc R . . C13 C 0.2671(2) 0.03113(13) 0.74363(18) 0.0309(6) Uani 1 1 d . . . C14 C 0.1602(2) 0.04069(13) 0.77972(18) 0.0278(6) Uani 1 1 d . . . H14 H 0.0822 0.0190 0.7483 0.033 Uiso 1 1 calc R . . C15 C 0.1645(2) 0.08107(12) 0.86024(17) 0.0258(6) Uani 1 1 d . . . C16 C 0.5146(2) 0.14207(14) 0.92324(19) 0.0335(6) Uani 1 1 d . . . C17 C 0.4933(3) 0.22216(14) 0.9310(2) 0.0423(7) Uani 1 1 d . . . H17A H 0.4633 0.2423 0.8673 0.063 Uiso 1 1 calc R . . H17B H 0.5736 0.2448 0.9631 0.063 Uiso 1 1 calc R . . H17C H 0.4295 0.2304 0.9674 0.063 Uiso 1 1 calc R . . C18 C 0.5643(3) 0.10965(15) 1.02243(19) 0.0403(7) Uani 1 1 d . . . H18A H 0.5016 0.1171 1.0600 0.060 Uiso 1 1 calc R . . H18B H 0.6448 0.1324 1.0540 0.060 Uiso 1 1 calc R . . H18C H 0.5784 0.0588 1.0164 0.060 Uiso 1 1 calc R . . C19 C 0.6187(2) 0.13217(16) 0.8686(2) 0.0413(7) Uani 1 1 d . . . H19A H 0.6369 0.0816 0.8644 0.062 Uiso 1 1 calc R . . H19B H 0.6962 0.1569 0.9019 0.062 Uiso 1 1 calc R . . H19C H 0.5891 0.1517 0.8045 0.062 Uiso 1 1 calc R . . C20 C 0.2588(3) -0.01534(15) 0.6559(2) 0.0410(7) Uani 1 1 d . . . C21 C 0.1611(4) 0.0163(3) 0.5725(2) 0.0870(15) Uani 1 1 d . . . H21A H 0.0780 0.0187 0.5880 0.130 Uiso 1 1 calc R . . H21B H 0.1545 -0.0135 0.5163 0.130 Uiso 1 1 calc R . . H21C H 0.1879 0.0641 0.5596 0.130 Uiso 1 1 calc R . . C22 C 0.3846(3) -0.02045(19) 0.6274(2) 0.0573(9) Uani 1 1 d . . . H22A H 0.4118 0.0270 0.6133 0.086 Uiso 1 1 calc R . . H22B H 0.3739 -0.0504 0.5709 0.086 Uiso 1 1 calc R . . H22C H 0.4492 -0.0412 0.6795 0.086 Uiso 1 1 calc R . . C23 C 0.2197(4) -0.09034(19) 0.6768(3) 0.0840(14) Uani 1 1 d . . . H23A H 0.2837 -0.1100 0.7303 0.126 Uiso 1 1 calc R . . H23B H 0.2136 -0.1202 0.6208 0.126 Uiso 1 1 calc R . . H23C H 0.1369 -0.0888 0.6929 0.126 Uiso 1 1 calc R . . C24 C 0.0481(2) 0.09001(12) 0.89798(17) 0.0254(5) Uani 1 1 d . . . H24A H 0.0211 0.1402 0.8917 0.031 Uiso 1 1 calc R . . H24B H -0.0220 0.0611 0.8596 0.031 Uiso 1 1 calc R . . C25 C 0.1349(2) -0.00264(12) 1.01715(17) 0.0242(5) Uani 1 1 d . . . H25A H 0.1616 -0.0110 1.0864 0.029 Uiso 1 1 calc R . . H25B H 0.2126 -0.0020 0.9926 0.029 Uiso 1 1 calc R . . C26 C 0.0508(2) -0.06347(12) 0.97118(17) 0.0238(5) Uani 1 1 d . . . H26A H 0.0323 -0.0580 0.9014 0.029 Uiso 1 1 calc R . . H26B H 0.0981 -0.1084 0.9878 0.029 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 0.0282(3) 0.0241(2) 0.0278(3) -0.0028(2) 0.00517(19) -0.0022(2) O1 0.0386(11) 0.0316(10) 0.0395(11) -0.0093(8) 0.0059(9) -0.0102(8) N1 0.0228(11) 0.0226(10) 0.0250(11) 0.0010(8) 0.0058(9) 0.0018(8) C1 0.0444(19) 0.0423(18) 0.060(2) -0.0151(15) 0.0030(16) -0.0125(14) O2 0.0358(10) 0.0240(9) 0.0378(11) -0.0051(8) 0.0057(8) 0.0037(8) C2 0.044(2) 0.056(2) 0.073(2) -0.0193(18) -0.0007(17) -0.0079(15) O3 0.0373(11) 0.0302(10) 0.0259(10) -0.0024(8) 0.0027(8) -0.0020(8) C3 0.069(2) 0.0340(18) 0.098(3) -0.0061(19) 0.002(2) -0.0148(17) O4 0.0289(9) 0.0341(10) 0.0315(10) -0.0059(8) 0.0097(8) -0.0064(8) C4 0.113(3) 0.041(2) 0.090(3) 0.0214(19) 0.032(3) 0.026(2) C5 0.0411(17) 0.0256(14) 0.0468(18) -0.0086(12) 0.0071(14) 0.0054(12) C6 0.049(2) 0.060(2) 0.076(3) -0.0205(18) 0.0232(18) 0.0060(16) C7 0.056(2) 0.061(2) 0.0404(19) -0.0078(15) 0.0160(16) 0.0065(16) C8 0.0319(15) 0.0373(15) 0.0250(14) -0.0031(12) 0.0032(12) -0.0021(12) C9 0.0512(19) 0.0480(18) 0.0309(16) 0.0071(13) 0.0062(14) -0.0013(14) C10 0.0304(15) 0.0243(13) 0.0262(14) 0.0038(11) 0.0061(12) -0.0002(10) C11 0.0270(14) 0.0262(13) 0.0296(15) 0.0050(11) 0.0065(11) 0.0012(10) C12 0.0277(14) 0.0344(14) 0.0321(15) 0.0060(12) 0.0110(12) 0.0050(11) C13 0.0323(15) 0.0328(14) 0.0278(15) 0.0025(11) 0.0079(12) 0.0004(11) C14 0.0253(14) 0.0300(14) 0.0267(14) 0.0033(11) 0.0039(11) 0.0007(10) C15 0.0257(14) 0.0248(13) 0.0266(14) 0.0035(11) 0.0063(11) 0.0010(10) C16 0.0265(14) 0.0398(16) 0.0340(16) 0.0011(12) 0.0067(12) -0.0048(11) C17 0.0371(16) 0.0370(16) 0.0539(19) 0.0010(14) 0.0133(14) -0.0086(13) C18 0.0319(16) 0.0512(18) 0.0354(16) 0.0002(13) 0.0035(13) -0.0024(13) C19 0.0263(15) 0.0567(18) 0.0407(17) 0.0025(14) 0.0079(13) -0.0047(13) C20 0.0370(16) 0.0509(18) 0.0376(17) -0.0143(14) 0.0139(13) -0.0031(13) C21 0.063(3) 0.154(4) 0.038(2) -0.032(2) 0.0004(18) 0.028(3) C22 0.051(2) 0.071(2) 0.055(2) -0.0235(18) 0.0231(17) -0.0015(17) C23 0.108(3) 0.061(2) 0.102(3) -0.040(2) 0.063(3) -0.030(2) C24 0.0256(13) 0.0239(13) 0.0254(14) 0.0012(10) 0.0036(11) 0.0018(10) C25 0.0221(13) 0.0232(12) 0.0269(14) 0.0002(10) 0.0053(11) 0.0018(10) C26 0.0226(13) 0.0239(12) 0.0253(13) -0.0018(10) 0.0067(10) 0.0017(10) _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 O1 1.7758(17) . ? Ti1 O2 1.8131(17) . ? Ti1 O3 1.8317(17) . ? Ti1 O4 1.8735(17) . ? Ti1 N1 2.3547(19) . ? O1 C1 1.420(3) . ? N1 C26 1.488(3) 3_557 ? N1 C24 1.498(3) . ? N1 C25 1.498(3) . ? C1 C3 1.485(5) . ? C1 C2 1.487(4) . ? C1 H1 1.0000 . ? O2 C5 1.423(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C8 1.423(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C10 1.357(3) . ? C4 C5 1.507(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.499(4) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.509(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.505(4) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.398(3) . ? C10 C11 1.406(3) . ? C11 C12 1.399(4) . ? C11 C16 1.539(3) . ? C12 C13 1.389(4) . ? C12 H12 0.9500 . ? C13 C14 1.393(4) . ? C13 C20 1.533(4) . ? C14 C15 1.388(3) . ? C14 H14 0.9500 . ? C15 C24 1.501(3) . ? C16 C17 1.539(4) . ? C16 C19 1.540(4) . ? C16 C18 1.538(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.520(4) . ? C20 C21 1.524(5) . ? C20 C23 1.530(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.517(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 N1 1.488(3) 3_557 ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? 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 O1 Ti1 O2 99.64(8) . . ? O1 Ti1 O3 98.42(8) . . ? O2 Ti1 O3 113.76(8) . . ? O1 Ti1 O4 97.03(8) . . ? O2 Ti1 O4 116.95(8) . . ? O3 Ti1 O4 123.09(8) . . ? O1 Ti1 N1 177.20(8) . . ? O2 Ti1 N1 83.08(7) . . ? O3 Ti1 N1 81.00(7) . . ? O4 Ti1 N1 81.07(7) . . ? C1 O1 Ti1 176.0(2) . . ? C26 N1 C24 110.25(18) 3_557 . ? C26 N1 C25 107.47(17) 3_557 . ? C24 N1 C25 111.79(18) . . ? C26 N1 Ti1 109.72(13) 3_557 . ? C24 N1 Ti1 105.99(13) . . ? C25 N1 Ti1 111.64(13) . . ? O1 C1 C3 110.1(3) . . ? O1 C1 C2 110.4(2) . . ? C3 C1 C2 114.6(3) . . ? O1 C1 H1 107.1 . . ? C3 C1 H1 107.1 . . ? C2 C1 H1 107.1 . . ? C5 O2 Ti1 136.34(16) . . ? 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 . . ? C8 O3 Ti1 133.29(15) . . ? 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 . . ? C10 O4 Ti1 142.92(15) . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 C6 109.6(2) . . ? O2 C5 C4 107.8(2) . . ? C6 C5 C4 113.6(3) . . ? O2 C5 H5 108.6 . . ? C6 C5 H5 108.6 . . ? C4 C5 H5 108.6 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 108.3(2) . . ? O3 C8 C7 109.9(2) . . ? C9 C8 C7 112.2(2) . . ? O3 C8 H8 108.8 . . ? C9 C8 H8 108.8 . . ? C7 C8 H8 108.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 C15 118.3(2) . . ? O4 C10 C11 120.9(2) . . ? C15 C10 C11 120.7(2) . . ? C12 C11 C10 116.8(2) . . ? C12 C11 C16 122.1(2) . . ? C10 C11 C16 121.1(2) . . ? C13 C12 C11 124.2(2) . . ? C13 C12 H12 117.9 . . ? C11 C12 H12 117.9 . . ? C12 C13 C14 116.8(2) . . ? C12 C13 C20 123.2(2) . . ? C14 C13 C20 120.1(2) . . ? C15 C14 C13 121.9(2) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C10 119.6(2) . . ? C14 C15 C24 120.7(2) . . ? C10 C15 C24 119.6(2) . . ? C11 C16 C17 109.9(2) . . ? C11 C16 C19 112.0(2) . . ? C17 C16 C19 107.4(2) . . ? C11 C16 C18 109.7(2) . . ? C17 C16 C18 110.3(2) . . ? C19 C16 C18 107.6(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C21 107.7(3) . . ? C22 C20 C23 107.7(3) . . ? C21 C20 C23 110.5(3) . . ? C22 C20 C13 112.8(2) . . ? C21 C20 C13 109.0(2) . . ? C23 C20 C13 109.1(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 C15 111.96(19) . . ? N1 C24 H24A 109.2 . . ? C15 C24 H24A 109.2 . . ? N1 C24 H24B 109.2 . . ? C15 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N1 C25 C26 113.81(19) . . ? N1 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? N1 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? N1 C26 C25 113.76(19) 3_557 . ? N1 C26 H26A 108.8 3_557 . ? C25 C26 H26A 108.8 . . ? N1 C26 H26B 108.8 3_557 . ? C25 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.233 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.067 #===END data_Ti2(4)(OiPr)6 _database_code_depnum_ccdc_archive 'CCDC 800220' #TrackingRef '- cif-DT-ART-11-2010-001542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H96 N2 O8 Ti2' _chemical_formula_weight 973.11 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.4410(3) _cell_length_b 10.0110(3) _cell_length_c 15.1580(5) _cell_angle_alpha 79.5090(10) _cell_angle_beta 84.6760(10) _cell_angle_gamma 87.7970(10) _cell_volume 1402.28(8) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16969 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 530 _exptl_absorpt_coefficient_mu 0.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9363 _exptl_absorpt_correction_T_max 0.9517 _exptl_absorpt_process_details 'Sortav (Blessing 1995)' _exptl_special_details ; The isopropoxide group adorning O1 is disordered in a 60:40 ratio The methyl groups of the isoproxide group of O3 are diordered in a 50:50 ratio ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19702 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 27.53 _reflns_number_total 6423 _reflns_number_gt 5071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0821P)^2^+1.4868P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6423 _refine_ls_number_parameters 350 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1701 _refine_ls_wR_factor_gt 0.1525 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.077 _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 0.24189(5) 0.15474(4) 0.15444(3) 0.02616(15) Uani 1 1 d . A . O1 O 0.0868(2) 0.2192(2) 0.21059(15) 0.0400(5) Uani 1 1 d . . . N1 N 0.4333(2) 0.04371(19) 0.08499(13) 0.0224(4) Uani 1 1 d . . . C1 C -0.0309(7) 0.2120(8) 0.2765(5) 0.0602(17) Uani 0.60 1 d PU A 1 H1 H -0.0053 0.1499 0.3325 0.072 Uiso 0.60 1 calc PR A 1 O2 O 0.3698(2) 0.28258(19) 0.15684(14) 0.0361(5) Uani 1 1 d . . . C2 C -0.0600(13) 0.3516(11) 0.2969(7) 0.091(3) Uani 0.60 1 d PU A 1 H2A H 0.0251 0.3841 0.3181 0.136 Uiso 0.60 1 calc PR A 1 H2B H -0.1391 0.3490 0.3438 0.136 Uiso 0.60 1 calc PR A 1 H2C H -0.0850 0.4131 0.2423 0.136 Uiso 0.60 1 calc PR A 1 O3 O 0.1740(2) 0.1667(2) 0.04368(13) 0.0342(4) Uani 1 1 d . . . C3 C -0.1524(8) 0.1455(9) 0.2350(6) 0.0631(19) Uani 0.60 1 d PU A 1 H3A H -0.1555 0.1872 0.1715 0.095 Uiso 0.60 1 calc PR A 1 H3B H -0.2443 0.1603 0.2680 0.095 Uiso 0.60 1 calc PR A 1 H3C H -0.1328 0.0477 0.2398 0.095 Uiso 0.60 1 calc PR A 1 O4 O 0.25174(19) -0.00952(18) 0.23695(12) 0.0296(4) Uani 1 1 d . . . C4 C 0.3916(3) 0.4086(3) 0.1837(2) 0.0373(6) Uani 1 1 d . A . H4 H 0.3783 0.3949 0.2510 0.045 Uiso 1 1 calc R . . C5 C 0.5419(5) 0.4495(5) 0.1543(4) 0.0789(15) Uani 1 1 d . . . H5A H 0.6072 0.3793 0.1823 0.118 Uiso 1 1 calc R A . H5B H 0.5590 0.5359 0.1727 0.118 Uiso 1 1 calc R . . H5C H 0.5578 0.4599 0.0886 0.118 Uiso 1 1 calc R . . C6 C 0.2885(5) 0.5158(4) 0.1468(4) 0.0747(13) Uani 1 1 d . . . H6A H 0.3028 0.5334 0.0809 0.112 Uiso 1 1 calc R A . H6B H 0.3037 0.5994 0.1694 0.112 Uiso 1 1 calc R . . H6C H 0.1913 0.4853 0.1659 0.112 Uiso 1 1 calc R . . C7 C 0.0681(3) 0.2561(3) 0.0020(2) 0.0512(9) Uani 1 1 d D A . H7 H -0.0064 0.2782 0.0488 0.061 Uiso 1 1 calc R B 1 C8 C 0.0043(11) 0.1795(9) -0.0590(7) 0.075(2) Uani 0.50 1 d PDU A 1 H8A H -0.0225 0.0893 -0.0259 0.113 Uiso 0.50 1 calc PR A 1 H8B H 0.0737 0.1698 -0.1098 0.113 Uiso 0.50 1 calc PR A 1 H8C H -0.0805 0.2288 -0.0816 0.113 Uiso 0.50 1 calc PR A 1 C9 C 0.1262(14) 0.3815(8) -0.0518(7) 0.070(3) Uani 0.50 1 d PDU A 1 H9A H 0.1952 0.3594 -0.0997 0.105 Uiso 0.50 1 calc PR A 1 H9B H 0.1734 0.4310 -0.0131 0.105 Uiso 0.50 1 calc PR A 1 H9C H 0.0488 0.4383 -0.0786 0.105 Uiso 0.50 1 calc PR A 1 C10 C 0.5345(3) 0.0016(3) 0.15567(17) 0.0255(5) Uani 1 1 d . A . H10A H 0.5522 0.0810 0.1834 0.031 Uiso 1 1 calc R . . H10B H 0.6263 -0.0266 0.1267 0.031 Uiso 1 1 calc R . . C11 C 0.4819(3) -0.1130(3) 0.22876(16) 0.0259(5) Uani 1 1 d . . . C12 C 0.3403(3) -0.1142(2) 0.26617(16) 0.0256(5) Uani 1 1 d . A . C13 C 0.2905(3) -0.2239(3) 0.33339(17) 0.0288(5) Uani 1 1 d . . . C14 C 0.3898(3) -0.3252(3) 0.36278(18) 0.0345(6) Uani 1 1 d . A . H14 H 0.3585 -0.3993 0.4081 0.041 Uiso 1 1 calc R . . C15 C 0.5318(3) -0.3236(3) 0.3294(2) 0.0372(6) Uani 1 1 d . . . C16 C 0.5759(3) -0.2174(3) 0.26094(18) 0.0323(6) Uani 1 1 d . A . H16 H 0.6719 -0.2159 0.2357 0.039 Uiso 1 1 calc R . . C17 C 0.1350(3) -0.2295(3) 0.3733(2) 0.0367(6) Uani 1 1 d . A . C18 C 0.1043(4) -0.1109(3) 0.4246(2) 0.0497(8) Uani 1 1 d . . . H18A H 0.1662 -0.1199 0.4739 0.075 Uiso 1 1 calc R A . H18B H 0.0045 -0.1125 0.4492 0.075 Uiso 1 1 calc R . . H18C H 0.1225 -0.0247 0.3833 0.075 Uiso 1 1 calc R . . C19 C 0.1041(4) -0.3617(3) 0.4407(3) 0.0536(9) Uani 1 1 d . . . H19A H 0.1263 -0.4397 0.4106 0.080 Uiso 1 1 calc R A . H19B H 0.0034 -0.3626 0.4631 0.080 Uiso 1 1 calc R . . H19C H 0.1630 -0.3672 0.4912 0.080 Uiso 1 1 calc R . . C20 C 0.0342(3) -0.2229(4) 0.2986(3) 0.0493(8) Uani 1 1 d . . . H20A H 0.0514 -0.1400 0.2539 0.074 Uiso 1 1 calc R A . H20B H -0.0646 -0.2221 0.3248 0.074 Uiso 1 1 calc R . . H20C H 0.0516 -0.3024 0.2695 0.074 Uiso 1 1 calc R . . C21 C 0.6359(4) -0.4351(4) 0.3655(3) 0.0577(10) Uani 1 1 d . A . H21A H 0.7280 -0.4217 0.3299 0.087 Uiso 1 1 calc R . . H21B H 0.5991 -0.5237 0.3612 0.087 Uiso 1 1 calc R . . H21C H 0.6479 -0.4319 0.4286 0.087 Uiso 1 1 calc R . . C22 C 0.3821(2) -0.0724(2) 0.04839(16) 0.0232(5) Uani 1 1 d . A . H22A H 0.3034 -0.0396 0.0106 0.028 Uiso 1 1 calc R . . H22B H 0.3435 -0.1416 0.0993 0.028 Uiso 1 1 calc R . . C23 C 0.4968(3) -0.1397(2) -0.00779(16) 0.0237(5) Uani 1 1 d . . . H23A H 0.5703 -0.1819 0.0317 0.028 Uiso 1 1 calc R A . H23B H 0.4534 -0.2131 -0.0313 0.028 Uiso 1 1 calc R . . C24 C 0.5048(7) 0.0352(5) 0.4569(4) 0.108(2) Uani 1 1 d DU . . H24A H 0.4510 -0.0180 0.4227 0.130 Uiso 1 1 calc R . . H24B H 0.6059 0.0270 0.4343 0.130 Uiso 1 1 calc R . . C25 C 0.4642(6) 0.1750(5) 0.4267(4) 0.1032(18) Uani 1 1 d DU . . H25A H 0.4936 0.1951 0.3613 0.124 Uiso 1 1 calc R . . H25B H 0.5252 0.2298 0.4554 0.124 Uiso 1 1 calc R . . C26 C 0.3220(5) 0.2310(6) 0.4376(4) 0.0955(17) Uani 1 1 d DU . . H26A H 0.2639 0.2030 0.3940 0.143 Uiso 1 1 calc R . . H26B H 0.3254 0.3304 0.4273 0.143 Uiso 1 1 calc R . . H26C H 0.2799 0.1975 0.4988 0.143 Uiso 1 1 calc R . . C1' C -0.0551(9) 0.2665(9) 0.2353(6) 0.0438(18) Uani 0.40 1 d PDU A 2 H1' H -0.0973 0.3363 0.1885 0.053 Uiso 0.40 1 calc PR A 2 C2' C -0.1501(16) 0.1466(14) 0.2756(10) 0.080(4) Uani 0.40 1 d PDU A 2 H2'1 H -0.0993 0.0827 0.3194 0.120 Uiso 0.40 1 calc PR A 2 H2'2 H -0.1745 0.1004 0.2275 0.120 Uiso 0.40 1 calc PR A 2 H2'3 H -0.2374 0.1796 0.3057 0.120 Uiso 0.40 1 calc PR A 2 C3' C -0.0503(19) 0.3080(16) 0.3273(7) 0.082(4) Uani 0.40 1 d PDU A 2 H3'1 H -0.1474 0.3245 0.3526 0.123 Uiso 0.40 1 calc PR A 2 H3'2 H 0.0043 0.3912 0.3203 0.123 Uiso 0.40 1 calc PR A 2 H3'3 H -0.0048 0.2350 0.3680 0.123 Uiso 0.40 1 calc PR A 2 C8' C -0.0630(7) 0.1896(8) -0.0044(7) 0.062(2) Uani 0.50 1 d PDU A 2 H8'1 H -0.0497 0.1369 -0.0531 0.093 Uiso 0.50 1 calc PR A 2 H8'2 H -0.1388 0.2582 -0.0170 0.093 Uiso 0.50 1 calc PR A 2 H8'3 H -0.0892 0.1288 0.0527 0.093 Uiso 0.50 1 calc PR A 2 C9' C 0.1333(11) 0.3489(10) -0.0770(6) 0.058(3) Uani 0.50 1 d PDU A 2 H9'1 H 0.1663 0.2970 -0.1242 0.087 Uiso 0.50 1 calc PR A 2 H9'2 H 0.2143 0.3934 -0.0595 0.087 Uiso 0.50 1 calc PR A 2 H9'3 H 0.0628 0.4179 -0.0998 0.087 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0253(2) 0.0221(2) 0.0296(3) -0.00327(17) 0.00143(17) 0.00171(16) O1 0.0348(10) 0.0366(11) 0.0454(12) -0.0069(9) 0.0089(9) 0.0068(8) N1 0.0221(9) 0.0218(9) 0.0223(10) -0.0009(8) -0.0012(8) -0.0027(7) C1 0.051(3) 0.066(3) 0.054(3) 0.000(3) 0.018(3) 0.020(3) O2 0.0364(10) 0.0251(9) 0.0478(12) -0.0113(8) 0.0014(9) -0.0032(8) C2 0.103(5) 0.095(5) 0.074(4) -0.034(4) 0.011(4) 0.037(4) O3 0.0281(9) 0.0376(10) 0.0348(10) -0.0018(8) -0.0054(8) 0.0073(8) C3 0.035(3) 0.079(4) 0.071(4) -0.007(3) 0.007(3) -0.008(3) O4 0.0281(9) 0.0274(9) 0.0296(9) 0.0006(7) 0.0049(7) 0.0017(7) C4 0.0489(17) 0.0260(13) 0.0384(15) -0.0097(11) -0.0033(12) -0.0012(11) C5 0.056(2) 0.063(3) 0.131(4) -0.051(3) -0.001(2) -0.0168(19) C6 0.079(3) 0.0315(17) 0.117(4) -0.015(2) -0.025(3) 0.0105(18) C7 0.0320(15) 0.062(2) 0.0509(19) 0.0118(16) -0.0076(13) 0.0121(14) C8 0.072(4) 0.063(4) 0.091(5) 0.004(4) -0.039(4) -0.006(3) C9 0.081(5) 0.050(4) 0.082(5) -0.010(4) -0.027(4) -0.001(4) C10 0.0235(11) 0.0275(12) 0.0247(12) -0.0023(9) -0.0027(9) -0.0010(9) C11 0.0289(12) 0.0273(12) 0.0214(12) -0.0032(9) -0.0029(9) -0.0015(9) C12 0.0293(12) 0.0247(11) 0.0226(12) -0.0040(9) -0.0014(9) -0.0010(9) C13 0.0347(13) 0.0283(12) 0.0227(12) -0.0035(10) -0.0008(10) -0.0037(10) C14 0.0450(16) 0.0295(13) 0.0267(13) 0.0016(10) -0.0038(11) -0.0019(11) C15 0.0414(15) 0.0334(14) 0.0346(15) 0.0017(11) -0.0092(12) 0.0051(12) C16 0.0305(13) 0.0361(14) 0.0292(13) -0.0030(11) -0.0038(10) 0.0027(11) C17 0.0381(15) 0.0317(14) 0.0359(15) 0.0015(11) 0.0067(12) -0.0066(11) C18 0.0536(19) 0.0437(17) 0.0473(19) -0.0080(14) 0.0202(15) -0.0034(14) C19 0.054(2) 0.0407(17) 0.056(2) 0.0106(15) 0.0163(16) -0.0079(14) C20 0.0373(16) 0.0491(18) 0.058(2) 0.0008(15) -0.0050(14) -0.0119(14) C21 0.054(2) 0.051(2) 0.057(2) 0.0181(17) -0.0078(17) 0.0137(16) C22 0.0232(11) 0.0200(10) 0.0258(12) -0.0021(9) -0.0013(9) -0.0042(8) C23 0.0243(11) 0.0199(10) 0.0256(12) -0.0012(9) 0.0008(9) -0.0039(9) C24 0.123(4) 0.097(3) 0.106(4) -0.002(3) -0.037(3) -0.034(3) C25 0.133(4) 0.086(3) 0.083(3) -0.001(3) -0.006(3) 0.023(3) C26 0.095(3) 0.098(3) 0.088(3) -0.002(3) -0.001(3) -0.020(3) C1' 0.041(3) 0.044(3) 0.041(4) 0.000(3) 0.001(3) 0.015(3) C2' 0.063(5) 0.097(6) 0.074(6) -0.002(5) 0.002(4) 0.001(4) C3' 0.090(6) 0.081(6) 0.071(6) -0.015(4) 0.010(4) 0.014(4) C8' 0.042(3) 0.063(4) 0.078(4) 0.007(3) -0.023(3) -0.007(3) C9' 0.052(4) 0.061(4) 0.052(4) 0.013(3) -0.001(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.7835(19) . ? Ti1 O2 1.8001(19) . ? Ti1 O3 1.834(2) . ? Ti1 O4 1.8809(18) . ? Ti1 N1 2.351(2) . ? O1 C1 1.419(6) . ? O1 C1' 1.443(8) . ? N1 C22 1.490(3) . ? N1 C23 1.491(3) 2_655 ? N1 C10 1.495(3) . ? C1 C2 1.496(11) . ? C1 C3 1.581(11) . ? C1 H1 1.0000 . ? O2 C4 1.422(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C7 1.430(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C12 1.351(3) . ? C4 C6 1.488(5) . ? C4 C5 1.497(5) . ? 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 C8' 1.446(4) . ? C7 C9 1.463(5) . ? C7 C9' 1.476(5) . ? C7 C8 1.485(5) . ? C7 H7 1.0000 . ? 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 C11 1.507(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.393(4) . ? C11 C12 1.402(3) . ? C12 C13 1.417(3) . ? C13 C14 1.394(4) . ? C13 C17 1.534(4) . ? C14 C15 1.388(4) . ? C14 H14 0.9500 . ? C15 C16 1.391(4) . ? C15 C21 1.518(4) . ? C16 H16 0.9500 . ? C17 C20 1.536(5) . ? C17 C19 1.537(4) . ? C17 C18 1.538(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.527(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N1 1.491(3) 2_655 ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C24 1.363(11) 2_656 ? C24 C25 1.4408(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.4415(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C1' C2' 1.527(5) . ? C1' C3' 1.531(5) . ? C1' H1' 1.0000 . ? C2' H2'1 0.9800 . ? C2' H2'2 0.9800 . ? C2' H2'3 0.9800 . ? C3' H3'1 0.9800 . ? C3' H3'2 0.9800 . ? C3' H3'3 0.9800 . ? C8' H8'1 0.9800 . ? C8' H8'2 0.9800 . ? C8' H8'3 0.9800 . ? C9' H9'1 0.9800 . ? C9' H9'2 0.9800 . ? C9' H9'3 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 O1 Ti1 O2 101.85(10) . . ? O1 Ti1 O3 97.69(10) . . ? O2 Ti1 O3 112.96(10) . . ? O1 Ti1 O4 95.28(9) . . ? O2 Ti1 O4 118.15(9) . . ? O3 Ti1 O4 122.91(9) . . ? O1 Ti1 N1 173.01(8) . . ? O2 Ti1 N1 84.67(8) . . ? O3 Ti1 N1 81.86(8) . . ? O4 Ti1 N1 79.27(7) . . ? C1 O1 C1' 32.3(4) . . ? C1 O1 Ti1 154.8(3) . . ? C1' O1 Ti1 165.1(4) . . ? C22 N1 C23 107.41(18) . 2_655 ? C22 N1 C10 113.34(18) . . ? C23 N1 C10 110.05(18) 2_655 . ? C22 N1 Ti1 110.61(13) . . ? C23 N1 Ti1 109.78(14) 2_655 . ? C10 N1 Ti1 105.64(14) . . ? O1 C1 C2 107.7(7) . . ? O1 C1 C3 104.8(6) . . ? C2 C1 C3 117.2(8) . . ? O1 C1 H1 109.0 . . ? C2 C1 H1 109.0 . . ? C3 C1 H1 109.0 . . ? C4 O2 Ti1 144.97(18) . . ? C7 O3 Ti1 130.1(2) . . ? C12 O4 Ti1 142.93(16) . . ? O2 C4 C6 111.9(3) . . ? O2 C4 C5 108.4(3) . . ? C6 C4 C5 111.3(3) . . ? O2 C4 H4 108.4 . . ? C6 C4 H4 108.4 . . ? C5 C4 H4 108.4 . . ? 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 C8' 113.6(4) . . ? O3 C7 C9 113.3(6) . . ? C8' C7 C9 129.5(7) . . ? O3 C7 C9' 110.2(5) . . ? C8' C7 C9' 119.9(6) . . ? C9 C7 C9' 21.4(6) . . ? O3 C7 C8 105.5(4) . . ? C8' C7 C8 40.5(5) . . ? C9 C7 C8 108.4(7) . . ? C9' C7 C8 89.7(7) . . ? O3 C7 H7 109.8 . . ? C8' C7 H7 69.9 . . ? C9 C7 H7 109.8 . . ? C9' C7 H7 127.9 . . ? C8 C7 H7 109.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? N1 C10 C11 113.6(2) . . ? N1 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? N1 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C16 C11 C12 119.7(2) . . ? C16 C11 C10 119.5(2) . . ? C12 C11 C10 120.8(2) . . ? O4 C12 C11 119.1(2) . . ? O4 C12 C13 120.4(2) . . ? C11 C12 C13 120.5(2) . . ? C14 C13 C12 117.0(2) . . ? C14 C13 C17 121.5(2) . . ? C12 C13 C17 121.4(2) . . ? C15 C14 C13 123.5(3) . . ? C15 C14 H14 118.2 . . ? C13 C14 H14 118.2 . . ? C14 C15 C16 118.0(3) . . ? C14 C15 C21 121.3(3) . . ? C16 C15 C21 120.8(3) . . ? C15 C16 C11 121.2(3) . . ? C15 C16 H16 119.4 . . ? C11 C16 H16 119.4 . . ? C13 C17 C20 110.5(2) . . ? C13 C17 C19 112.0(3) . . ? C20 C17 C19 107.1(3) . . ? C13 C17 C18 108.9(2) . . ? C20 C17 C18 110.9(3) . . ? C19 C17 C18 107.4(3) . . ? 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 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C15 C21 H21A 109.5 . . ? C15 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C15 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C23 114.06(19) . . ? N1 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? N1 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? N1 C23 C22 113.58(19) 2_655 . ? N1 C23 H23A 108.8 2_655 . ? C22 C23 H23A 108.8 . . ? N1 C23 H23B 108.8 2_655 . ? C22 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C24 C24 C25 127.5(8) 2_656 . ? C24 C24 H24A 105.4 2_656 . ? C25 C24 H24A 105.4 . . ? C24 C24 H24B 105.4 2_656 . ? C25 C24 H24B 105.4 . . ? H24A C24 H24B 106.0 . . ? C24 C25 C26 124.9(6) . . ? C24 C25 H25A 106.1 . . ? C26 C25 H25A 106.1 . . ? C24 C25 H25B 106.1 . . ? C26 C25 H25B 106.1 . . ? H25A C25 H25B 106.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 C1' C2' 110.5(8) . . ? O1 C1' C3' 106.1(9) . . ? C2' C1' C3' 91.9(10) . . ? O1 C1' H1' 115.3 . . ? C2' C1' H1' 115.3 . . ? C3' C1' H1' 115.3 . . ? C1' C2' H2'1 109.5 . . ? C1' C2' H2'2 109.5 . . ? H2'1 C2' H2'2 109.5 . . ? C1' C2' H2'3 109.5 . . ? H2'1 C2' H2'3 109.5 . . ? H2'2 C2' H2'3 109.5 . . ? C1' C3' H3'1 109.5 . . ? C1' C3' H3'2 109.5 . . ? H3'1 C3' H3'2 109.5 . . ? C1' C3' H3'3 109.5 . . ? H3'1 C3' H3'3 109.5 . . ? H3'2 C3' H3'3 109.5 . . ? C7 C8' H8'1 109.5 . . ? C7 C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? C7 C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C7 C9' H9'1 109.5 . . ? C7 C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C7 C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.352 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.072 #===END data_Ti2(5)(OiPr)6 _database_code_depnum_ccdc_archive 'CCDC 800221' #TrackingRef '- cif-DT-ART-11-2010-001542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H116 N2 O8 Ti2' _chemical_formula_weight 1113.37 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.0450(10) _cell_length_b 13.2550(11) _cell_length_c 13.9140(14) _cell_angle_alpha 115.990(5) _cell_angle_beta 109.683(5) _cell_angle_gamma 91.805(5) _cell_volume 1685.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26403 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 610 _exptl_absorpt_coefficient_mu 0.285 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33515 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7641 _reflns_number_gt 5497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0875P)^2^+0.9724P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7641 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.02161(4) 0.29689(4) 0.72115(3) 0.03219(14) Uani 1 1 d . . . O1 O 0.03355(18) 0.22676(16) 0.58345(14) 0.0455(4) Uani 1 1 d . . . N1 N 0.01965(17) 0.39386(15) 0.90856(15) 0.0292(4) Uani 1 1 d . . . C1 C 0.0731(4) 0.1658(4) 0.4918(3) 0.0876(14) Uani 1 1 d . . . H1 H 0.1336 0.1225 0.5221 0.105 Uiso 1 1 calc R . . O2 O -0.13497(16) 0.21554(15) 0.68861(14) 0.0429(4) Uani 1 1 d . . . C2 C -0.0300(4) 0.0748(4) 0.3913(3) 0.0920(14) Uani 1 1 d . . . H2A H -0.0660 0.0242 0.4140 0.138 Uiso 1 1 calc R . . H2B H 0.0057 0.0305 0.3335 0.138 Uiso 1 1 calc R . . H2C H -0.1000 0.1077 0.3578 0.138 Uiso 1 1 calc R . . O3 O 0.01970(18) 0.44062(15) 0.73493(14) 0.0421(4) Uani 1 1 d . . . C3 C 0.1608(4) 0.2392(3) 0.4793(4) 0.0801(11) Uani 1 1 d . . . H3A H 0.1909 0.1917 0.4184 0.120 Uiso 1 1 calc R . . H3B H 0.2368 0.2827 0.5530 0.120 Uiso 1 1 calc R . . H3C H 0.1137 0.2925 0.4582 0.120 Uiso 1 1 calc R . . O4 O 0.17263(16) 0.26430(15) 0.80370(13) 0.0389(4) Uani 1 1 d . . . C4 C -0.2447(3) 0.1323(2) 0.5923(2) 0.0503(7) Uani 1 1 d . . . H4 H -0.2163 0.0878 0.5273 0.060 Uiso 1 1 calc R . . C5 C -0.3492(3) 0.1918(4) 0.5532(3) 0.0766(10) Uani 1 1 d . . . H5A H -0.3771 0.2363 0.6167 0.115 Uiso 1 1 calc R . . H5B H -0.4249 0.1345 0.4861 0.115 Uiso 1 1 calc R . . H5C H -0.3138 0.2435 0.5313 0.115 Uiso 1 1 calc R . . C6 C -0.2938(4) 0.0514(3) 0.6266(4) 0.0748(10) Uani 1 1 d . . . H6A H -0.2218 0.0178 0.6558 0.112 Uiso 1 1 calc R . . H6B H -0.3654 -0.0099 0.5588 0.112 Uiso 1 1 calc R . . H6C H -0.3263 0.0935 0.6874 0.112 Uiso 1 1 calc R . . C7 C 0.0206(3) 0.4931(2) 0.6654(2) 0.0438(6) Uani 1 1 d . . . H7 H 0.0775 0.4585 0.6220 0.053 Uiso 1 1 calc R . . C8 C -0.1147(4) 0.4713(4) 0.5802(3) 0.0829(12) Uani 1 1 d . . . H8A H -0.1491 0.3883 0.5312 0.124 Uiso 1 1 calc R . . H8B H -0.1130 0.5063 0.5314 0.124 Uiso 1 1 calc R . . H8C H -0.1715 0.5049 0.6216 0.124 Uiso 1 1 calc R . . C9 C 0.0785(5) 0.6190(3) 0.7430(3) 0.0886(13) Uani 1 1 d . . . H9A H 0.0226 0.6543 0.7849 0.133 Uiso 1 1 calc R . . H9B H 0.0839 0.6552 0.6961 0.133 Uiso 1 1 calc R . . H9C H 0.1669 0.6298 0.7989 0.133 Uiso 1 1 calc R . . C10 C 0.2443(2) 0.27637(19) 0.91031(19) 0.0331(5) Uani 1 1 d . . . C11 C 0.3785(2) 0.2726(2) 0.9433(2) 0.0374(5) Uani 1 1 d . . . C12 C 0.4434(2) 0.2835(2) 1.0533(2) 0.0422(6) Uani 1 1 d . . . H12 H 0.5341 0.2810 1.0769 0.051 Uiso 1 1 calc R . . C13 C 0.3841(3) 0.2980(2) 1.1310(2) 0.0416(6) Uani 1 1 d . . . C14 C 0.2526(2) 0.3055(2) 1.0963(2) 0.0379(5) Uani 1 1 d . . . H14 H 0.2098 0.3180 1.1481 0.046 Uiso 1 1 calc R . . C15 C 0.1823(2) 0.29506(19) 0.98747(19) 0.0330(5) Uani 1 1 d . . . C16 C 0.4504(3) 0.2592(3) 0.8619(2) 0.0497(7) Uani 1 1 d . . . C17 C 0.4394(4) 0.3606(4) 0.8307(4) 0.0786(11) Uani 1 1 d . . . H17A H 0.3467 0.3568 0.7885 0.118 Uiso 1 1 calc R . . H17B H 0.4885 0.3536 0.7818 0.118 Uiso 1 1 calc R . . H17C H 0.4762 0.4342 0.9023 0.118 Uiso 1 1 calc R . . C18 C 0.5989(3) 0.2667(3) 0.9212(3) 0.0628(8) Uani 1 1 d . . . H18A H 0.6376 0.3400 0.9930 0.094 Uiso 1 1 calc R . . H18B H 0.6423 0.2617 0.8687 0.094 Uiso 1 1 calc R . . H18C H 0.6112 0.2033 0.9394 0.094 Uiso 1 1 calc R . . C19 C 0.3917(3) 0.1457(3) 0.7508(2) 0.0585(8) Uani 1 1 d . . . H19A H 0.2971 0.1421 0.7123 0.070 Uiso 1 1 calc R . . H19B H 0.4346 0.1433 0.6980 0.070 Uiso 1 1 calc R . . C20 C 0.4053(4) 0.0442(3) 0.7672(3) 0.0759(10) Uani 1 1 d . . . H20A H 0.4987 0.0423 0.7976 0.114 Uiso 1 1 calc R . . H20B H 0.3591 -0.0252 0.6926 0.114 Uiso 1 1 calc R . . H20C H 0.3671 0.0474 0.8225 0.114 Uiso 1 1 calc R . . C21 C 0.4641(3) 0.3127(3) 1.2526(2) 0.0552(7) Uani 1 1 d . . . C22 C 0.5643(4) 0.2353(4) 1.2471(3) 0.0888(13) Uani 1 1 d . . . H22A H 0.5182 0.1550 1.1948 0.133 Uiso 1 1 calc R . . H22B H 0.6138 0.2454 1.3249 0.133 Uiso 1 1 calc R . . H22C H 0.6251 0.2561 1.2180 0.133 Uiso 1 1 calc R . . C23 C 0.5461(3) 0.4398(3) 1.3317(3) 0.0716(10) Uani 1 1 d . . . H23A H 0.6033 0.4477 1.4079 0.086 Uiso 1 1 calc R . . H23B H 0.6043 0.4530 1.2958 0.086 Uiso 1 1 calc R . . C24 C 0.4705(4) 0.5303(3) 1.3524(3) 0.0737(10) Uani 1 1 d . . . H24A H 0.4107 0.5223 1.2779 0.111 Uiso 1 1 calc R . . H24B H 0.5308 0.6056 1.3977 0.111 Uiso 1 1 calc R . . H24C H 0.4192 0.5237 1.3956 0.111 Uiso 1 1 calc R . . C25 C 0.3756(4) 0.2848(4) 1.3058(3) 0.0733(10) Uani 1 1 d . . . H25A H 0.3143 0.3368 1.3138 0.110 Uiso 1 1 calc R . . H25B H 0.4301 0.2943 1.3825 0.110 Uiso 1 1 calc R . . H25C H 0.3259 0.2053 1.2553 0.110 Uiso 1 1 calc R . . C26 C 0.0419(2) 0.3097(2) 0.9546(2) 0.0327(5) Uani 1 1 d . . . H26A H -0.0172 0.2343 0.8948 0.039 Uiso 1 1 calc R . . H26B H 0.0192 0.3365 1.0236 0.039 Uiso 1 1 calc R . . C27 C 0.1204(2) 0.50355(19) 0.98455(19) 0.0311(5) Uani 1 1 d . . . H27A H 0.1106 0.5492 0.9430 0.037 Uiso 1 1 calc R . . H27B H 0.2090 0.4855 0.9985 0.037 Uiso 1 1 calc R . . C28 C -0.1113(2) 0.4238(2) 0.89920(19) 0.0316(5) Uani 1 1 d . . . H28A H -0.1793 0.3520 0.8557 0.038 Uiso 1 1 calc R . . H28B H -0.1312 0.4659 0.8539 0.038 Uiso 1 1 calc R . . C29 C 0.7494(5) 0.0450(4) 0.0567(5) 0.1032(15) Uani 1 1 d . . . H29A H 0.7251 -0.0335 0.0423 0.155 Uiso 1 1 calc R . . H29B H 0.6697 0.0723 0.0304 0.155 Uiso 1 1 calc R . . H29C H 0.7991 0.0953 0.1400 0.155 Uiso 1 1 calc R . . C30 C 0.8325(5) 0.0466(4) -0.0082(5) 0.1014(14) Uani 1 1 d . . . H30A H 0.8556 0.1256 0.0047 0.122 Uiso 1 1 calc R . . H30B H 0.7826 -0.0040 -0.0925 0.122 Uiso 1 1 calc R . . C31 C 0.9581(5) 0.0053(4) 0.0331(5) 0.1001(14) Uani 1 1 d . . . H31A H 1.0100 0.0598 0.1160 0.120 Uiso 1 1 calc R . . H31B H 0.9335 -0.0703 0.0270 0.120 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 0.0330(2) 0.0392(2) 0.0231(2) 0.01447(17) 0.01003(16) 0.00719(17) O1 0.0498(10) 0.0597(11) 0.0259(8) 0.0177(8) 0.0169(8) 0.0163(9) N1 0.0279(9) 0.0342(10) 0.0258(9) 0.0147(8) 0.0103(7) 0.0061(8) C1 0.097(3) 0.091(3) 0.0474(19) -0.0020(18) 0.048(2) -0.014(2) O2 0.0383(9) 0.0467(10) 0.0288(8) 0.0089(7) 0.0098(7) -0.0022(8) C2 0.078(2) 0.111(3) 0.0436(19) 0.000(2) 0.0271(18) -0.004(2) O3 0.0539(10) 0.0473(10) 0.0321(9) 0.0243(8) 0.0173(8) 0.0125(8) C3 0.107(3) 0.071(2) 0.089(3) 0.036(2) 0.072(3) 0.020(2) O4 0.0391(9) 0.0550(10) 0.0264(8) 0.0207(8) 0.0146(7) 0.0183(8) C4 0.0405(14) 0.0503(15) 0.0354(13) 0.0004(12) 0.0154(11) -0.0041(12) C5 0.0531(19) 0.095(3) 0.061(2) 0.035(2) 0.0033(16) 0.0045(18) C6 0.065(2) 0.0537(19) 0.099(3) 0.0239(19) 0.043(2) 0.0028(16) C7 0.0531(15) 0.0538(15) 0.0392(13) 0.0303(12) 0.0228(12) 0.0173(12) C8 0.066(2) 0.122(3) 0.075(2) 0.075(3) 0.0072(18) 0.006(2) C9 0.113(3) 0.073(2) 0.073(2) 0.048(2) 0.012(2) -0.011(2) C10 0.0377(12) 0.0372(12) 0.0256(11) 0.0163(9) 0.0117(9) 0.0108(10) C11 0.0378(12) 0.0441(13) 0.0299(11) 0.0169(10) 0.0134(10) 0.0107(10) C12 0.0353(12) 0.0528(15) 0.0318(12) 0.0174(11) 0.0091(10) 0.0128(11) C13 0.0465(14) 0.0473(14) 0.0291(12) 0.0186(11) 0.0114(11) 0.0162(11) C14 0.0467(14) 0.0437(13) 0.0286(11) 0.0190(10) 0.0178(10) 0.0154(11) C15 0.0367(12) 0.0353(12) 0.0289(11) 0.0166(10) 0.0129(9) 0.0101(9) C16 0.0359(13) 0.0750(19) 0.0410(14) 0.0289(14) 0.0163(11) 0.0138(13) C17 0.063(2) 0.129(3) 0.084(3) 0.079(3) 0.0368(19) 0.018(2) C18 0.0388(14) 0.097(2) 0.0526(17) 0.0344(17) 0.0194(13) 0.0100(15) C19 0.0481(16) 0.085(2) 0.0371(14) 0.0216(15) 0.0202(13) 0.0222(15) C20 0.082(2) 0.075(2) 0.055(2) 0.0207(18) 0.0230(18) 0.0119(19) C21 0.0597(17) 0.077(2) 0.0317(13) 0.0292(14) 0.0151(13) 0.0306(15) C22 0.105(3) 0.126(3) 0.057(2) 0.060(2) 0.029(2) 0.072(3) C23 0.0570(19) 0.104(3) 0.0384(16) 0.0300(18) 0.0080(14) 0.0101(19) C24 0.085(2) 0.076(2) 0.0437(17) 0.0195(16) 0.0191(17) 0.0021(19) C25 0.084(2) 0.100(3) 0.0421(17) 0.0451(18) 0.0162(16) 0.019(2) C26 0.0375(12) 0.0365(12) 0.0292(11) 0.0182(10) 0.0152(9) 0.0089(10) C27 0.0271(10) 0.0358(12) 0.0273(11) 0.0137(9) 0.0091(9) 0.0045(9) C28 0.0284(11) 0.0369(12) 0.0267(11) 0.0133(9) 0.0104(9) 0.0058(9) C29 0.122(4) 0.097(3) 0.112(4) 0.056(3) 0.061(3) 0.035(3) C30 0.103(3) 0.096(3) 0.108(4) 0.042(3) 0.051(3) 0.033(3) C31 0.122(4) 0.082(3) 0.106(4) 0.043(3) 0.057(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.7803(17) . ? Ti1 O2 1.8127(17) . ? Ti1 O3 1.8308(17) . ? Ti1 O4 1.8649(16) . ? Ti1 N1 2.3567(18) . ? O1 C1 1.401(3) . ? N1 C28 1.491(3) . ? N1 C27 1.493(3) . ? N1 C26 1.501(3) . ? C1 C2 1.439(5) . ? C1 C3 1.454(5) . ? C1 H1 1.0000 . ? O2 C4 1.417(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C7 1.421(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C10 1.358(3) . ? C4 C6 1.502(5) . ? C4 C5 1.504(5) . ? 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 C8 1.484(4) . ? C7 C9 1.499(5) . ? C7 H7 1.0000 . ? 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 C15 1.398(3) . ? C10 C11 1.406(3) . ? C11 C12 1.392(3) . ? C11 C16 1.544(3) . ? C12 C13 1.392(4) . ? C12 H12 0.9500 . ? C13 C14 1.389(4) . ? C13 C21 1.541(3) . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 C26 1.507(3) . ? C16 C19 1.515(4) . ? C16 C18 1.546(4) . ? C16 C17 1.580(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.464(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C25 1.531(5) . ? C21 C22 1.530(4) . ? C21 C23 1.575(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.464(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.518(3) 2_567 ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C27 1.518(3) 2_567 ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.494(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.530(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C31 1.481(9) 2_755 ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? 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 O1 Ti1 O2 100.54(8) . . ? O1 Ti1 O3 98.72(8) . . ? O2 Ti1 O3 115.42(9) . . ? O1 Ti1 O4 96.88(8) . . ? O2 Ti1 O4 116.82(8) . . ? O3 Ti1 O4 121.04(8) . . ? O1 Ti1 N1 176.55(7) . . ? O2 Ti1 N1 82.70(7) . . ? O3 Ti1 N1 80.85(7) . . ? O4 Ti1 N1 80.49(6) . . ? C1 O1 Ti1 164.9(2) . . ? C28 N1 C27 107.10(16) . . ? C28 N1 C26 110.64(17) . . ? C27 N1 C26 112.64(17) . . ? C28 N1 Ti1 109.11(12) . . ? C27 N1 Ti1 112.24(13) . . ? C26 N1 Ti1 105.11(13) . . ? O1 C1 C2 113.3(3) . . ? O1 C1 C3 112.9(3) . . ? C2 C1 C3 120.7(4) . . ? O1 C1 H1 102.2 . . ? C2 C1 H1 102.2 . . ? C3 C1 H1 102.2 . . ? C4 O2 Ti1 140.23(16) . . ? 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 . . ? C7 O3 Ti1 136.36(16) . . ? 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 . . ? C10 O4 Ti1 142.79(15) . . ? O2 C4 C6 109.0(3) . . ? O2 C4 C5 109.3(2) . . ? C6 C4 C5 111.8(3) . . ? O2 C4 H4 108.9 . . ? C6 C4 H4 108.9 . . ? C5 C4 H4 108.9 . . ? 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 C8 110.0(2) . . ? O3 C7 C9 108.9(2) . . ? C8 C7 C9 112.0(3) . . ? O3 C7 H7 108.6 . . ? C8 C7 H7 108.6 . . ? C9 C7 H7 108.6 . . ? 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 . . ? O4 C10 C15 118.5(2) . . ? O4 C10 C11 120.8(2) . . ? C15 C10 C11 120.7(2) . . ? C12 C11 C10 116.8(2) . . ? C12 C11 C16 121.9(2) . . ? C10 C11 C16 121.3(2) . . ? C11 C12 C13 124.2(2) . . ? C11 C12 H12 117.9 . . ? C13 C12 H12 117.9 . . ? C14 C13 C12 116.9(2) . . ? C14 C13 C21 122.1(2) . . ? C12 C13 C21 120.9(2) . . ? C13 C14 C15 121.6(2) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C10 119.7(2) . . ? C14 C15 C26 120.4(2) . . ? C10 C15 C26 119.8(2) . . ? C19 C16 C11 111.0(2) . . ? C19 C16 C18 109.0(2) . . ? C11 C16 C18 111.5(2) . . ? C19 C16 C17 109.1(3) . . ? C11 C16 C17 109.8(2) . . ? C18 C16 C17 106.3(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C16 114.5(3) . . ? C20 C19 H19A 108.6 . . ? C16 C19 H19A 108.6 . . ? C20 C19 H19B 108.6 . . ? C16 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C25 C21 C22 108.9(3) . . ? C25 C21 C13 112.0(3) . . ? C22 C21 C13 110.6(2) . . ? C25 C21 C23 111.0(3) . . ? C22 C21 C23 106.3(3) . . ? C13 C21 C23 108.0(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C21 116.4(3) . . ? C24 C23 H23A 108.2 . . ? C21 C23 H23A 108.2 . . ? C24 C23 H23B 108.2 . . ? C21 C23 H23B 108.2 . . ? H23A C23 H23B 107.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 C15 112.13(18) . . ? N1 C26 H26A 109.2 . . ? C15 C26 H26A 109.2 . . ? N1 C26 H26B 109.2 . . ? C15 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? N1 C27 C28 114.03(18) . 2_567 ? N1 C27 H27A 108.7 . . ? C28 C27 H27A 108.7 2_567 . ? N1 C27 H27B 108.7 . . ? C28 C27 H27B 108.7 2_567 . ? H27A C27 H27B 107.6 . . ? N1 C28 C27 113.95(17) . 2_567 ? N1 C28 H28A 108.8 . . ? C27 C28 H28A 108.8 2_567 . ? N1 C28 H28B 108.8 . . ? C27 C28 H28B 108.8 2_567 . ? H28A C28 H28B 107.7 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C29 C30 C31 109.9(4) . . ? C29 C30 H30A 109.7 . . ? C31 C30 H30A 109.7 . . ? C29 C30 H30B 109.7 . . ? C31 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C31 C31 C30 114.0(6) 2_755 . ? C31 C31 H31A 108.8 2_755 . ? C30 C31 H31A 108.8 . . ? C31 C31 H31B 108.8 2_755 . ? C30 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.761 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.062 #===END data_Ti2(6)(OiPr)6 _database_code_depnum_ccdc_archive 'CCDC 800222' #TrackingRef '- cif-DT-ART-11-2010-001542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H96 N2 O8 Ti2' _chemical_formula_weight 985.12 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.24600(10) _cell_length_b 24.3060(3) _cell_length_c 26.2840(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.5990(10) _cell_angle_gamma 90.00 _cell_volume 5904.59(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 92915 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 0.318 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; the isopropoxide groups adorning Ti2 are disordered over two positions in a 55:45 ratio. The methyl groups of two tBu (C20, C50) functionalities are disordered over two positions again in a 55:45 ratio. In addition the methyl group of the piperazine ring is disordered on three (C26-28) of the ring carbons in a 60:20:20 ratio ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67951 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 24.99 _reflns_number_total 10306 _reflns_number_gt 8005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1126P)^2^+10.5855P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10306 _refine_ls_number_parameters 589 _refine_ls_number_restraints 123 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0851 _refine_ls_wR_factor_ref 0.2403 _refine_ls_wR_factor_gt 0.2225 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.004 _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 0.15711(8) 0.10008(3) 0.16138(3) 0.0421(2) Uani 1 1 d . . . Ti2 Ti -0.22025(9) 0.26452(3) 0.35967(3) 0.0483(2) Uani 1 1 d D . . O1 O 0.2521(4) 0.07468(14) 0.10783(11) 0.0594(8) Uani 1 1 d . . . O2 O -0.0269(3) 0.08551(14) 0.13925(11) 0.0559(8) Uani 1 1 d . . . O3 O 0.2135(4) 0.17153(13) 0.15787(12) 0.0580(8) Uani 1 1 d . . . O4 O 0.2426(3) 0.05163(11) 0.20855(10) 0.0431(6) Uani 1 1 d . . . O5 O -0.3258(8) 0.2937(3) 0.4065(3) 0.062(2) Uiso 0.55 1 d PD A 2 O6 O -0.0403(8) 0.2904(3) 0.3808(3) 0.069(2) Uiso 0.55 1 d PD A 1 O7 O -0.2605(8) 0.1928(3) 0.3648(3) 0.055(2) Uiso 0.55 1 d PD A 1 O8 O -0.2916(3) 0.30784(13) 0.30551(11) 0.0512(7) Uani 1 1 d . A . N1 N 0.0390(3) 0.13070(13) 0.23448(12) 0.0383(7) Uani 1 1 d . . . N2 N -0.0775(4) 0.22837(14) 0.29298(14) 0.0455(8) Uani 1 1 d . A . C1 C 0.3334(8) 0.0355(3) 0.0807(2) 0.0879(19) Uani 1 1 d . . . H1 H 0.4102 0.0199 0.1041 0.105 Uiso 1 1 calc R . . C2 C 0.2402(10) -0.0090(4) 0.0629(4) 0.122(3) Uani 1 1 d U . . H2A H 0.1944 -0.0263 0.0920 0.183 Uiso 1 1 calc R . . H2B H 0.2979 -0.0364 0.0451 0.183 Uiso 1 1 calc R . . H2C H 0.1654 0.0057 0.0395 0.183 Uiso 1 1 calc R . . C3 C 0.4038(11) 0.0640(4) 0.0379(4) 0.147(4) Uani 1 1 d . . . H3A H 0.3294 0.0777 0.0138 0.220 Uiso 1 1 calc R . . H3B H 0.4670 0.0382 0.0204 0.220 Uiso 1 1 calc R . . H3C H 0.4613 0.0950 0.0511 0.220 Uiso 1 1 calc R . . C4 C -0.0994(6) 0.0730(2) 0.09266(17) 0.0639(13) Uani 1 1 d . . . H4 H -0.0252 0.0687 0.0660 0.077 Uiso 1 1 calc R . . C5 C -0.1959(8) 0.1209(3) 0.0778(2) 0.104(2) Uani 1 1 d . . . H5A H -0.2732 0.1243 0.1024 0.156 Uiso 1 1 calc R . . H5B H -0.2385 0.1145 0.0438 0.156 Uiso 1 1 calc R . . H5C H -0.1387 0.1548 0.0777 0.156 Uiso 1 1 calc R . . C6 C -0.1767(9) 0.0185(3) 0.0984(3) 0.105(2) Uani 1 1 d . . . H6A H -0.1071 -0.0096 0.1097 0.157 Uiso 1 1 calc R . . H6B H -0.2206 0.0077 0.0655 0.157 Uiso 1 1 calc R . . H6C H -0.2523 0.0222 0.1235 0.157 Uiso 1 1 calc R . . C7 C 0.3141(8) 0.2012(3) 0.1283(3) 0.092(2) Uani 1 1 d . . . H7 H 0.3259 0.1801 0.0960 0.111 Uiso 1 1 calc R . . C8 C 0.2578(11) 0.2543(4) 0.1144(4) 0.150(4) Uani 1 1 d . . . H8A H 0.1681 0.2498 0.0941 0.225 Uiso 1 1 calc R . . H8B H 0.3290 0.2741 0.0943 0.225 Uiso 1 1 calc R . . H8C H 0.2380 0.2754 0.1452 0.225 Uiso 1 1 calc R . . C9 C 0.4629(8) 0.2019(3) 0.1561(3) 0.101(2) Uani 1 1 d U . . H9A H 0.4513 0.2139 0.1914 0.151 Uiso 1 1 calc R . . H9B H 0.5273 0.2275 0.1389 0.151 Uiso 1 1 calc R . . H9C H 0.5048 0.1649 0.1558 0.151 Uiso 1 1 calc R . . C10 C 0.2441(4) 0.03820(15) 0.25848(14) 0.0379(8) Uani 1 1 d . . . C11 C 0.3665(4) 0.01383(16) 0.28222(15) 0.0400(9) Uani 1 1 d . . . C12 C 0.3581(4) 0.00255(17) 0.33375(15) 0.0443(9) Uani 1 1 d . . . H12 H 0.4398 -0.0139 0.3503 0.053 Uiso 1 1 calc R . . C13 C 0.2373(5) 0.01374(18) 0.36313(16) 0.0471(10) Uani 1 1 d . B . C14 C 0.1201(4) 0.03809(17) 0.33802(14) 0.0418(9) Uani 1 1 d . . . H14 H 0.0362 0.0465 0.3565 0.050 Uiso 1 1 calc R . . C15 C 0.1222(4) 0.05057(16) 0.28647(14) 0.0389(9) Uani 1 1 d . . . C16 C 0.5038(5) 0.00137(18) 0.25225(16) 0.0475(10) Uani 1 1 d . . . C17 C 0.5643(5) 0.0549(2) 0.22994(19) 0.0574(12) Uani 1 1 d . . . H17A H 0.6533 0.0468 0.2119 0.086 Uiso 1 1 calc R . . H17B H 0.5857 0.0810 0.2576 0.086 Uiso 1 1 calc R . . H17C H 0.4926 0.0710 0.2061 0.086 Uiso 1 1 calc R . . C18 C 0.4702(5) -0.0397(2) 0.20952(18) 0.0579(12) Uani 1 1 d . . . H18A H 0.3897 -0.0258 0.1881 0.087 Uiso 1 1 calc R . . H18B H 0.4434 -0.0752 0.2242 0.087 Uiso 1 1 calc R . . H18C H 0.5558 -0.0444 0.1888 0.087 Uiso 1 1 calc R . . C19 C 0.6254(5) -0.0235(2) 0.2864(2) 0.0638(13) Uani 1 1 d . . . H19A H 0.5920 -0.0582 0.3010 0.096 Uiso 1 1 calc R . . H19B H 0.6510 0.0023 0.3138 0.096 Uiso 1 1 calc R . . H19C H 0.7106 -0.0305 0.2660 0.096 Uiso 1 1 calc R . . C20 C 0.2348(4) -0.0018(2) 0.41943(16) 0.0642(13) Uani 1 1 d D . . C21 C 0.2482(12) -0.0654(3) 0.4222(4) 0.082(3) Uiso 0.55 1 d PD B 3 H21A H 0.3357 -0.0771 0.4051 0.123 Uiso 0.55 1 calc PR B 3 H21B H 0.1632 -0.0822 0.4055 0.123 Uiso 0.55 1 calc PR B 3 H21C H 0.2540 -0.0769 0.4580 0.123 Uiso 0.55 1 calc PR B 3 C22 C 0.0986(7) 0.0142(4) 0.4469(3) 0.065(2) Uiso 0.55 1 d PD B 3 H22A H 0.1076 0.0027 0.4826 0.097 Uiso 0.55 1 calc PR B 3 H22B H 0.0148 -0.0040 0.4307 0.097 Uiso 0.55 1 calc PR B 3 H22C H 0.0857 0.0542 0.4453 0.097 Uiso 0.55 1 calc PR B 3 C23 C 0.3685(7) 0.0225(4) 0.4473(3) 0.060(2) Uiso 0.55 1 d PD B 3 H23A H 0.4558 0.0119 0.4293 0.090 Uiso 0.55 1 calc PR B 3 H23B H 0.3743 0.0083 0.4822 0.090 Uiso 0.55 1 calc PR B 3 H23C H 0.3607 0.0627 0.4480 0.090 Uiso 0.55 1 calc PR B 3 C24 C -0.0057(4) 0.07897(16) 0.26105(15) 0.0402(9) Uani 1 1 d . . . H24A H -0.0522 0.0537 0.2360 0.048 Uiso 1 1 calc R . . H24B H -0.0776 0.0881 0.2870 0.048 Uiso 1 1 calc R . . C25 C -0.0915(4) 0.16277(17) 0.21820(15) 0.0413(9) Uani 1 1 d . A . H25A H -0.1599 0.1377 0.2001 0.050 Uiso 1 1 calc R . . H25B H -0.0620 0.1913 0.1937 0.050 Uiso 1 1 calc R . . C26 C -0.1702(4) 0.19060(16) 0.26121(16) 0.0420(9) Uani 1 1 d . . . H26 H -0.1923 0.1597 0.2849 0.050 Uiso 1 1 calc R A . C27 C 0.0502(4) 0.1946(2) 0.31090(17) 0.0515(11) Uani 1 1 d . . . H27 H 0.0076 0.1634 0.3303 0.062 Uiso 1 1 calc R A . C28 C 0.1302(4) 0.16736(19) 0.26745(16) 0.0475(10) Uani 1 1 d . A . H28 H 0.1436 0.1994 0.2442 0.057 Uiso 1 1 calc R . . C29 C 0.1641(7) 0.2194(3) 0.3471(3) 0.0439(15) Uiso 0.60 1 d P A . H29A H 0.1164 0.2373 0.3755 0.066 Uiso 0.60 1 calc PR . . H29B H 0.2213 0.2466 0.3289 0.066 Uiso 0.60 1 calc PR . . H29C H 0.2280 0.1902 0.3603 0.066 Uiso 0.60 1 calc PR . . C39 C -0.0297(5) 0.27787(18) 0.26362(18) 0.0504(11) Uani 1 1 d . . . H39A H 0.0114 0.3053 0.2878 0.061 Uiso 1 1 calc R A . H39B H 0.0482 0.2667 0.2407 0.061 Uiso 1 1 calc R . . C40 C -0.1485(5) 0.30446(17) 0.23260(17) 0.0464(10) Uani 1 1 d . A . C41 C -0.1340(5) 0.31378(18) 0.18059(19) 0.0560(12) Uani 1 1 d . . . H41 H -0.0469 0.3031 0.1650 0.067 Uiso 1 1 calc R A . C42 C -0.2419(6) 0.33796(19) 0.15119(18) 0.0590(12) Uani 1 1 d . A . C43 C -0.3676(5) 0.35386(18) 0.17569(17) 0.0525(11) Uani 1 1 d . . . H43 H -0.4422 0.3713 0.1560 0.063 Uiso 1 1 calc R A . C44 C -0.3894(5) 0.34543(16) 0.22745(16) 0.0456(10) Uani 1 1 d . A . C45 C -0.2774(5) 0.31935(17) 0.25607(15) 0.0436(9) Uani 1 1 d . . . C46 C -0.5284(5) 0.36480(18) 0.25280(18) 0.0517(11) Uani 1 1 d . . . C47 C -0.6371(6) 0.3905(2) 0.2145(2) 0.0713(15) Uani 1 1 d . A . H47A H -0.5921 0.4219 0.1977 0.107 Uiso 1 1 calc R . . H47B H -0.7226 0.4030 0.2325 0.107 Uiso 1 1 calc R . . H47C H -0.6659 0.3630 0.1889 0.107 Uiso 1 1 calc R . . C48 C -0.4886(6) 0.4094(2) 0.2928(2) 0.0692(14) Uani 1 1 d . A . H48A H -0.4175 0.3945 0.3175 0.104 Uiso 1 1 calc R . . H48B H -0.5758 0.4205 0.3105 0.104 Uiso 1 1 calc R . . H48C H -0.4473 0.4414 0.2758 0.104 Uiso 1 1 calc R . . C49 C -0.6054(5) 0.3168(2) 0.27807(19) 0.0576(12) Uani 1 1 d . A . H49A H -0.6296 0.2887 0.2525 0.086 Uiso 1 1 calc R . . H49B H -0.6943 0.3301 0.2934 0.086 Uiso 1 1 calc R . . H49C H -0.5416 0.3008 0.3046 0.086 Uiso 1 1 calc R . . C50 C -0.2299(6) 0.3504(2) 0.0943(2) 0.0768(15) Uani 1 1 d DU . . C51 C -0.3408(12) 0.3177(5) 0.0630(5) 0.098(4) Uiso 0.55 1 d PD A 3 H51A H -0.3301 0.3259 0.0268 0.148 Uiso 0.55 1 calc PR A 3 H51B H -0.4384 0.3278 0.0732 0.148 Uiso 0.55 1 calc PR A 3 H51C H -0.3253 0.2783 0.0689 0.148 Uiso 0.55 1 calc PR A 3 C52 C -0.2494(13) 0.4130(2) 0.0854(4) 0.070(3) Uiso 0.55 1 d PD A 3 H52A H -0.1753 0.4331 0.1053 0.105 Uiso 0.55 1 calc PR A 3 H52B H -0.3456 0.4242 0.0963 0.105 Uiso 0.55 1 calc PR A 3 H52C H -0.2397 0.4213 0.0492 0.105 Uiso 0.55 1 calc PR A 3 C53 C -0.0759(9) 0.3376(5) 0.0769(5) 0.101(4) Uiso 0.55 1 d PD A 3 H53A H -0.0057 0.3591 0.0972 0.152 Uiso 0.55 1 calc PR A 3 H53B H -0.0679 0.3473 0.0409 0.152 Uiso 0.55 1 calc PR A 3 H53C H -0.0560 0.2983 0.0814 0.152 Uiso 0.55 1 calc PR A 3 C54 C -0.4851(15) 0.3067(4) 0.4259(4) 0.082(3) Uiso 0.55 1 d PD A 1 H54 H -0.5642 0.3131 0.3999 0.099 Uiso 0.55 1 calc PR A 1 C55 C -0.4332(19) 0.3616(4) 0.4469(6) 0.117(5) Uiso 0.55 1 d PD A 1 H55A H -0.3988 0.3845 0.4190 0.176 Uiso 0.55 1 calc PR A 1 H55B H -0.3539 0.3555 0.4718 0.176 Uiso 0.55 1 calc PR A 1 H55C H -0.5132 0.3803 0.4634 0.176 Uiso 0.55 1 calc PR A 1 C56 C -0.5368(15) 0.2673(5) 0.4656(5) 0.107(4) Uiso 0.55 1 d PD A 1 H56A H -0.5631 0.2322 0.4494 0.160 Uiso 0.55 1 calc PR A 1 H56B H -0.6215 0.2828 0.4820 0.160 Uiso 0.55 1 calc PR A 1 H56C H -0.4595 0.2611 0.4912 0.160 Uiso 0.55 1 calc PR A 1 C57 C 0.0125(17) 0.3117(6) 0.4245(5) 0.118(5) Uiso 0.55 1 d PD A 1 H57 H -0.0770 0.3330 0.4320 0.141 Uiso 0.55 1 calc PR A 1 C58 C 0.1054(16) 0.3613(5) 0.4178(5) 0.114(4) Uiso 0.55 1 d PD A 1 H58A H 0.0823 0.3784 0.3848 0.171 Uiso 0.55 1 calc PR A 1 H58B H 0.2075 0.3504 0.4192 0.171 Uiso 0.55 1 calc PR A 1 H58C H 0.0874 0.3878 0.4450 0.171 Uiso 0.55 1 calc PR A 1 C59 C 0.0235(17) 0.2842(6) 0.4757(5) 0.122(5) Uiso 0.55 1 d PD A 1 H59A H -0.0475 0.2543 0.4770 0.182 Uiso 0.55 1 calc PR A 1 H59B H 0.0041 0.3111 0.5023 0.182 Uiso 0.55 1 calc PR A 1 H59C H 0.1210 0.2691 0.4810 0.182 Uiso 0.55 1 calc PR A 1 C60 C -0.3331(11) 0.1584(3) 0.3995(4) 0.071(3) Uiso 0.55 1 d PD A 1 H60 H -0.3550 0.1805 0.4305 0.085 Uiso 0.55 1 calc PR A 1 C61 C -0.4735(14) 0.1464(7) 0.3711(7) 0.146(6) Uiso 0.55 1 d PD A 1 H61A H -0.5208 0.1811 0.3615 0.220 Uiso 0.55 1 calc PR A 1 H61B H -0.5371 0.1252 0.3930 0.220 Uiso 0.55 1 calc PR A 1 H61C H -0.4539 0.1251 0.3404 0.220 Uiso 0.55 1 calc PR A 1 C62 C -0.2497(14) 0.1074(5) 0.4162(6) 0.108(4) Uiso 0.55 1 d PD A 1 H62A H -0.1595 0.1184 0.4338 0.161 Uiso 0.55 1 calc PR A 1 H62B H -0.2272 0.0853 0.3862 0.161 Uiso 0.55 1 calc PR A 1 H62C H -0.3084 0.0856 0.4392 0.161 Uiso 0.55 1 calc PR A 1 O5A O -0.3671(8) 0.2810(3) 0.4028(2) 0.0379(17) Uiso 0.45 1 d PD A 1 O6A O -0.0727(8) 0.2928(3) 0.3942(3) 0.0379(18) Uiso 0.45 1 d PD A 2 O7A O -0.2247(9) 0.1886(3) 0.3749(3) 0.042(2) Uiso 0.45 1 d PD A 2 C21A C 0.1501(17) -0.0552(5) 0.4278(8) 0.132(7) Uiso 0.45 1 d PD B 4 H21D H 0.0583 -0.0538 0.4083 0.198 Uiso 0.45 1 calc PR B 4 H21E H 0.1306 -0.0593 0.4641 0.198 Uiso 0.45 1 calc PR B 4 H21F H 0.2072 -0.0866 0.4164 0.198 Uiso 0.45 1 calc PR B 4 C22A C 0.1444(15) 0.0433(5) 0.4458(6) 0.110(5) Uiso 0.45 1 d PD B 4 H22D H 0.0485 0.0456 0.4290 0.165 Uiso 0.45 1 calc PR B 4 H22E H 0.1937 0.0788 0.4432 0.165 Uiso 0.45 1 calc PR B 4 H22F H 0.1338 0.0338 0.4817 0.165 Uiso 0.45 1 calc PR B 4 C23A C 0.3798(8) -0.0041(5) 0.4485(4) 0.069(3) Uiso 0.45 1 d PD B 4 H23D H 0.3640 -0.0145 0.4840 0.103 Uiso 0.45 1 calc PR B 4 H23E H 0.4263 0.0321 0.4475 0.103 Uiso 0.45 1 calc PR B 4 H23F H 0.4423 -0.0314 0.4327 0.103 Uiso 0.45 1 calc PR B 4 C29A C 0.275(2) 0.1586(8) 0.2856(7) 0.045(5) Uani 0.20 1 d P . . H29D H 0.3309 0.1410 0.2588 0.067 Uiso 0.20 1 calc PR A . H29E H 0.2749 0.1347 0.3156 0.067 Uiso 0.20 1 calc PR . . H29F H 0.3195 0.1940 0.2947 0.067 Uiso 0.20 1 calc PR . . C51A C -0.3771(10) 0.3421(6) 0.0653(5) 0.082(4) Uiso 0.45 1 d PD A 4 H51D H -0.3655 0.3500 0.0290 0.123 Uiso 0.45 1 calc PR A 4 H51E H -0.4492 0.3672 0.0791 0.123 Uiso 0.45 1 calc PR A 4 H51F H -0.4093 0.3040 0.0694 0.123 Uiso 0.45 1 calc PR A 4 C52A C -0.1902(18) 0.4112(3) 0.0856(7) 0.103(6) Uiso 0.45 1 d PD A 4 H52D H -0.1819 0.4180 0.0490 0.154 Uiso 0.45 1 calc PR A 4 H52E H -0.0976 0.4193 0.1030 0.154 Uiso 0.45 1 calc PR A 4 H52F H -0.2658 0.4348 0.0992 0.154 Uiso 0.45 1 calc PR A 4 C53A C -0.1183(15) 0.3154(7) 0.0667(7) 0.133(8) Uiso 0.45 1 d PD A 4 H53D H -0.1180 0.3258 0.0307 0.199 Uiso 0.45 1 calc PR A 4 H53E H -0.1437 0.2764 0.0696 0.199 Uiso 0.45 1 calc PR A 4 H53F H -0.0220 0.3217 0.0821 0.199 Uiso 0.45 1 calc PR A 4 C54A C -0.436(2) 0.3070(5) 0.4403(5) 0.106(6) Uiso 0.45 1 d PD A 2 H54A H -0.5184 0.2821 0.4305 0.127 Uiso 0.45 1 calc PR A 2 C55A C -0.4954(19) 0.3644(5) 0.4336(6) 0.091(5) Uiso 0.45 1 d PD A 2 H55D H -0.5055 0.3728 0.3972 0.137 Uiso 0.45 1 calc PR A 2 H55E H -0.4290 0.3908 0.4500 0.137 Uiso 0.45 1 calc PR A 2 H55F H -0.5902 0.3668 0.4492 0.137 Uiso 0.45 1 calc PR A 2 C56A C -0.396(2) 0.2914(7) 0.4943(6) 0.132(7) Uiso 0.45 1 d PD A 2 H56D H -0.3509 0.2549 0.4947 0.197 Uiso 0.45 1 calc PR A 2 H56E H -0.4833 0.2906 0.5146 0.197 Uiso 0.45 1 calc PR A 2 H56F H -0.3278 0.3185 0.5086 0.197 Uiso 0.45 1 calc PR A 2 C57A C -0.0434(12) 0.3308(4) 0.4337(4) 0.052(2) Uiso 0.45 1 d PD A 2 H57A H -0.1250 0.3274 0.4577 0.063 Uiso 0.45 1 calc PR A 2 C58A C -0.057(2) 0.3873(5) 0.4102(7) 0.130(6) Uiso 0.45 1 d PD A 2 H58D H -0.1503 0.3902 0.3916 0.194 Uiso 0.45 1 calc PR A 2 H58E H 0.0216 0.3932 0.3867 0.194 Uiso 0.45 1 calc PR A 2 H58F H -0.0524 0.4152 0.4371 0.194 Uiso 0.45 1 calc PR A 2 C59A C 0.093(2) 0.3213(9) 0.4650(10) 0.188(11) Uiso 0.45 1 d PD A 2 H59D H 0.0901 0.2845 0.4802 0.282 Uiso 0.45 1 calc PR A 2 H59E H 0.1003 0.3490 0.4920 0.282 Uiso 0.45 1 calc PR A 2 H59F H 0.1767 0.3242 0.4432 0.282 Uiso 0.45 1 calc PR A 2 C60A C -0.2843(14) 0.1557(5) 0.4157(4) 0.066(3) Uiso 0.45 1 d PD A 2 H60A H -0.3831 0.1698 0.4232 0.079 Uiso 0.45 1 calc PR A 2 C61A C -0.2976(18) 0.0976(4) 0.3956(6) 0.099(5) Uiso 0.45 1 d PD A 2 H61D H -0.3641 0.0971 0.3659 0.148 Uiso 0.45 1 calc PR A 2 H61E H -0.3350 0.0737 0.4222 0.148 Uiso 0.45 1 calc PR A 2 H61F H -0.2022 0.0844 0.3857 0.148 Uiso 0.45 1 calc PR A 2 C62A C -0.189(2) 0.1617(8) 0.4629(6) 0.147(8) Uiso 0.45 1 d PD A 2 H62D H -0.1872 0.2003 0.4735 0.221 Uiso 0.45 1 calc PR A 2 H62E H -0.0910 0.1495 0.4556 0.221 Uiso 0.45 1 calc PR A 2 H62F H -0.2280 0.1390 0.4902 0.221 Uiso 0.45 1 calc PR A 2 C29B C -0.314(3) 0.2050(11) 0.2378(10) 0.064(6) Uiso 0.20 1 d P A . H29G H -0.3727 0.2234 0.2631 0.095 Uiso 0.20 1 calc PR . . H29H H -0.3627 0.1713 0.2261 0.095 Uiso 0.20 1 calc PR . . H29I H -0.3002 0.2296 0.2088 0.095 Uiso 0.20 1 calc PR . . 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 0.0512(5) 0.0421(4) 0.0333(4) 0.0002(3) 0.0052(3) 0.0033(3) Ti2 0.0485(5) 0.0500(5) 0.0463(5) -0.0101(3) 0.0004(3) 0.0052(3) O1 0.081(2) 0.0590(19) 0.0391(16) -0.0005(14) 0.0155(15) 0.0113(17) O2 0.0595(19) 0.070(2) 0.0381(15) -0.0074(14) -0.0047(14) 0.0009(16) O3 0.071(2) 0.0490(18) 0.0546(18) 0.0038(14) 0.0216(15) -0.0049(15) O4 0.0493(16) 0.0452(16) 0.0349(14) 0.0009(12) 0.0062(12) 0.0095(13) O8 0.0497(17) 0.0633(19) 0.0409(16) -0.0065(14) 0.0070(13) 0.0092(14) N1 0.0392(17) 0.0371(17) 0.0387(17) -0.0019(13) 0.0009(14) 0.0045(14) N2 0.0374(18) 0.0415(19) 0.058(2) -0.0120(16) 0.0073(15) -0.0030(15) C1 0.119(5) 0.083(4) 0.062(3) -0.017(3) 0.014(3) 0.034(4) C2 0.125(4) 0.108(4) 0.135(5) -0.032(4) 0.018(4) -0.003(4) C3 0.147(8) 0.166(9) 0.131(7) -0.035(7) 0.080(6) 0.022(7) C4 0.069(3) 0.085(4) 0.037(2) -0.009(2) -0.007(2) 0.004(3) C5 0.104(5) 0.137(6) 0.070(4) 0.010(4) -0.020(4) 0.035(5) C6 0.132(6) 0.109(5) 0.072(4) -0.021(4) -0.015(4) -0.036(5) C7 0.105(5) 0.070(4) 0.103(5) 0.026(3) 0.041(4) -0.008(4) C8 0.139(8) 0.127(7) 0.186(10) 0.089(7) 0.052(7) -0.005(6) C9 0.089(4) 0.089(4) 0.127(4) 0.009(3) 0.025(3) -0.002(3) C10 0.045(2) 0.0331(19) 0.036(2) -0.0030(15) 0.0039(16) 0.0011(16) C11 0.041(2) 0.037(2) 0.042(2) 0.0006(16) 0.0014(17) -0.0005(17) C12 0.043(2) 0.047(2) 0.043(2) 0.0007(18) -0.0039(18) 0.0013(18) C13 0.046(2) 0.052(3) 0.043(2) -0.0019(19) -0.0024(18) -0.0045(19) C14 0.044(2) 0.046(2) 0.036(2) -0.0017(17) 0.0035(17) -0.0003(18) C15 0.042(2) 0.035(2) 0.040(2) 0.0004(16) 0.0036(16) 0.0010(16) C16 0.043(2) 0.050(2) 0.050(2) 0.0032(19) 0.0070(18) 0.0089(19) C17 0.047(3) 0.062(3) 0.064(3) 0.008(2) 0.013(2) -0.002(2) C18 0.058(3) 0.060(3) 0.057(3) -0.006(2) 0.015(2) 0.013(2) C19 0.046(3) 0.078(4) 0.067(3) 0.006(3) 0.006(2) 0.015(2) C20 0.059(3) 0.097(4) 0.036(2) 0.002(2) -0.002(2) -0.001(3) C24 0.041(2) 0.042(2) 0.038(2) 0.0007(17) 0.0046(16) 0.0022(17) C25 0.041(2) 0.041(2) 0.041(2) -0.0012(17) -0.0022(17) 0.0019(17) C26 0.037(2) 0.038(2) 0.051(2) -0.0031(17) 0.0009(17) -0.0010(17) C27 0.039(2) 0.060(3) 0.055(3) -0.020(2) 0.0033(19) -0.002(2) C28 0.038(2) 0.057(3) 0.048(2) -0.010(2) 0.0010(18) 0.0033(19) C39 0.043(2) 0.044(2) 0.064(3) -0.010(2) 0.016(2) -0.0067(19) C40 0.049(2) 0.037(2) 0.054(2) -0.0122(18) 0.0150(19) -0.0093(18) C41 0.062(3) 0.043(2) 0.064(3) -0.009(2) 0.028(2) -0.011(2) C42 0.082(3) 0.045(3) 0.051(3) -0.003(2) 0.020(2) -0.017(2) C43 0.066(3) 0.043(2) 0.049(2) 0.0025(19) 0.008(2) -0.008(2) C44 0.054(2) 0.036(2) 0.047(2) -0.0034(17) 0.0090(19) -0.0062(18) C45 0.049(2) 0.039(2) 0.043(2) -0.0087(17) 0.0071(18) -0.0054(18) C46 0.053(3) 0.046(2) 0.057(3) 0.002(2) 0.006(2) 0.008(2) C47 0.075(4) 0.064(3) 0.075(3) 0.008(3) 0.003(3) 0.023(3) C48 0.072(3) 0.062(3) 0.075(3) -0.017(3) 0.017(3) 0.010(3) C49 0.045(2) 0.063(3) 0.065(3) 0.006(2) 0.009(2) 0.003(2) C50 0.093(3) 0.076(3) 0.062(3) 0.001(2) 0.021(3) -0.019(3) C29A 0.067(14) 0.039(11) 0.029(9) -0.004(8) 0.013(9) 0.020(10) _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 O1 1.790(3) . ? Ti1 O2 1.817(3) . ? Ti1 O3 1.817(3) . ? Ti1 O4 1.869(3) . ? Ti1 N1 2.357(3) . ? Ti2 O5 1.743(7) . ? Ti2 O6A 1.757(6) . ? Ti2 O7 1.789(6) . ? Ti2 O5A 1.837(6) . ? Ti2 O6 1.850(7) . ? Ti2 O8 1.876(3) . ? Ti2 O7A 1.888(7) . ? Ti2 N2 2.391(3) . ? O1 C1 1.418(6) . ? O2 C4 1.413(5) . ? O3 C7 1.425(6) . ? O4 C10 1.352(4) . ? O5 C54A 1.409(17) . ? O6 C57 1.339(13) . ? O7 C60 1.420(12) . ? O8 C45 1.339(5) . ? N1 C28 1.488(5) . ? N1 C25 1.489(5) . ? N1 C24 1.502(5) . ? N2 C26 1.495(5) . ? N2 C27 1.503(6) . ? N2 C39 1.502(6) . ? C1 C2 1.452(10) . ? C1 C3 1.489(11) . ? 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 1.510(8) . ? C4 C6 1.515(9) . ? 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 C8 1.437(10) . ? C7 C9 1.540(10) . ? C7 H7 1.0000 . ? 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 C15 1.396(5) . ? C10 C11 1.408(5) . ? C11 C12 1.386(6) . ? C11 C16 1.543(6) . ? C12 C13 1.402(6) . ? C12 H12 0.9500 . ? C13 C14 1.386(6) . ? C13 C20 1.528(6) . ? C14 C15 1.389(5) . ? C14 H14 0.9500 . ? C15 C24 1.509(5) . ? C16 C18 1.528(6) . ? C16 C17 1.539(6) . ? C16 C19 1.542(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.520(4) . ? C20 C23A 1.526(5) . ? C20 C21A 1.536(5) . ? C20 C23 1.536(4) . ? C20 C22A 1.552(5) . ? C20 C21 1.553(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.521(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C29B 1.49(2) . ? C26 H26 1.0000 . ? C27 C29 1.524(8) . ? C27 C28 1.529(6) . ? C27 H27 1.0000 . ? C28 C29A 1.43(2) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C39 C40 1.496(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.396(6) . ? C40 C45 1.405(6) . ? C41 C42 1.377(7) . ? C41 H41 0.9500 . ? C42 C43 1.398(7) . ? C42 C50 1.534(7) . ? C43 C44 1.396(6) . ? C43 H43 0.9500 . ? C44 C45 1.413(6) . ? C44 C46 1.538(6) . ? C46 C49 1.528(6) . ? C46 C47 1.534(7) . ? C46 C48 1.548(7) . ? 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 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.521(5) . ? C50 C53A 1.535(5) . ? C50 C53 1.540(5) . ? C50 C52A 1.540(5) . ? C50 C52 1.548(5) . ? C50 C51A 1.555(5) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 O5A 1.410(13) . ? C54 C56 1.504(5) . ? C54 C55 1.515(5) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.494(5) . ? C57 C59 1.504(5) . ? C57 H57 1.0000 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.507(5) . ? C60 C62 1.518(5) . ? C60 H60 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? O6A C57A 1.410(12) . ? O7A C60A 1.459(14) . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C29A H29D 0.9800 . ? C29A H29E 0.9800 . ? C29A H29F 0.9800 . ? C51A H51D 0.9800 . ? C51A H51E 0.9800 . ? C51A H51F 0.9800 . ? C52A H52D 0.9800 . ? C52A H52E 0.9800 . ? C52A H52F 0.9800 . ? C53A H53D 0.9800 . ? C53A H53E 0.9800 . ? C53A H53F 0.9800 . ? C54A C56A 1.503(5) . ? C54A C55A 1.507(5) . ? C54A H54A 1.0000 . ? C55A H55D 0.9800 . ? C55A H55E 0.9800 . ? C55A H55F 0.9800 . ? C56A H56D 0.9800 . ? C56A H56E 0.9800 . ? C56A H56F 0.9800 . ? C57A C59A 1.503(5) . ? C57A C58A 1.508(5) . ? C57A H57A 1.0000 . ? C58A H58D 0.9800 . ? C58A H58E 0.9800 . ? C58A H58F 0.9800 . ? C59A H59D 0.9800 . ? C59A H59E 0.9800 . ? C59A H59F 0.9800 . ? C60A C62A 1.505(5) . ? C60A C61A 1.512(15) . ? C60A H60A 1.0000 . ? C61A H61D 0.9800 . ? C61A H61E 0.9800 . ? C61A H61F 0.9800 . ? C62A H62D 0.9800 . ? C62A H62E 0.9800 . ? C62A H62F 0.9800 . ? C29B H29G 0.9800 . ? C29B H29H 0.9800 . ? C29B H29I 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 O1 Ti1 O2 99.02(15) . . ? O1 Ti1 O3 98.16(15) . . ? O2 Ti1 O3 115.96(16) . . ? O1 Ti1 O4 95.53(13) . . ? O2 Ti1 O4 117.67(14) . . ? O3 Ti1 O4 121.27(14) . . ? O1 Ti1 N1 177.19(13) . . ? O2 Ti1 N1 82.63(12) . . ? O3 Ti1 N1 83.09(13) . . ? O4 Ti1 N1 81.68(11) . . ? O5 Ti2 O6A 85.3(4) . . ? O5 Ti2 O7 102.7(4) . . ? O6A Ti2 O7 120.2(3) . . ? O5 Ti2 O5A 15.7(3) . . ? O6A Ti2 O5A 100.0(4) . . ? O7 Ti2 O5A 90.4(3) . . ? O5 Ti2 O6 99.6(4) . . ? O6A Ti2 O6 14.8(3) . . ? O7 Ti2 O6 119.8(4) . . ? O5A Ti2 O6 114.5(4) . . ? O5 Ti2 O8 96.7(3) . . ? O6A Ti2 O8 115.0(3) . . ? O7 Ti2 O8 122.4(3) . . ? O5A Ti2 O8 95.5(2) . . ? O6 Ti2 O8 109.3(3) . . ? O5 Ti2 O7A 103.4(3) . . ? O6A Ti2 O7A 107.1(3) . . ? O7 Ti2 O7A 13.1(3) . . ? O5A Ti2 O7A 93.5(3) . . ? O6 Ti2 O7A 107.1(4) . . ? O8 Ti2 O7A 134.4(3) . . ? O5 Ti2 N2 177.3(3) . . ? O6A Ti2 N2 94.9(3) . . ? O7 Ti2 N2 79.5(2) . . ? O5A Ti2 N2 164.8(3) . . ? O6 Ti2 N2 80.5(3) . . ? O8 Ti2 N2 80.77(13) . . ? O7A Ti2 N2 79.2(2) . . ? C1 O1 Ti1 154.9(4) . . ? C4 O2 Ti1 137.5(3) . . ? C7 O3 Ti1 134.7(4) . . ? C10 O4 Ti1 142.0(2) . . ? C54A O5 Ti2 165.6(9) . . ? C57 O6 Ti2 133.8(9) . . ? C60 O7 Ti2 136.6(6) . . ? C45 O8 Ti2 144.2(3) . . ? C28 N1 C25 107.2(3) . . ? C28 N1 C24 112.9(3) . . ? C25 N1 C24 109.9(3) . . ? C28 N1 Ti1 113.3(2) . . ? C25 N1 Ti1 108.7(2) . . ? C24 N1 Ti1 104.7(2) . . ? C26 N2 C27 105.9(3) . . ? C26 N2 C39 112.2(3) . . ? C27 N2 C39 111.0(3) . . ? C26 N2 Ti2 108.4(2) . . ? C27 N2 Ti2 114.6(3) . . ? C39 N2 Ti2 105.0(2) . . ? O1 C1 C2 110.2(6) . . ? O1 C1 C3 108.4(6) . . ? C2 C1 C3 111.8(7) . . ? O1 C1 H1 108.8 . . ? C2 C1 H1 108.8 . . ? C3 C1 H1 108.8 . . ? 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 108.7(5) . . ? O2 C4 C6 108.4(4) . . ? C5 C4 C6 114.9(6) . . ? O2 C4 H4 108.2 . . ? C5 C4 H4 108.2 . . ? C6 C4 H4 108.2 . . ? 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 C8 110.9(6) . . ? O3 C7 C9 109.5(5) . . ? C8 C7 C9 115.0(7) . . ? O3 C7 H7 107.0 . . ? C8 C7 H7 107.0 . . ? C9 C7 H7 107.0 . . ? 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 . . ? O4 C10 C15 118.3(3) . . ? O4 C10 C11 121.2(3) . . ? C15 C10 C11 120.5(4) . . ? C12 C11 C10 116.7(4) . . ? C12 C11 C16 122.0(4) . . ? C10 C11 C16 121.3(3) . . ? C11 C12 C13 124.5(4) . . ? C11 C12 H12 117.7 . . ? C13 C12 H12 117.7 . . ? C14 C13 C12 116.4(4) . . ? C14 C13 C20 122.3(4) . . ? C12 C13 C20 121.3(4) . . ? C13 C14 C15 121.7(4) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C14 C15 C10 120.0(4) . . ? C14 C15 C24 120.0(4) . . ? C10 C15 C24 120.0(3) . . ? C18 C16 C17 109.9(4) . . ? C18 C16 C19 107.6(4) . . ? C17 C16 C19 106.6(4) . . ? C18 C16 C11 110.5(4) . . ? C17 C16 C11 110.0(4) . . ? C19 C16 C11 112.2(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C23A 119.9(7) . . ? C22 C20 C13 115.7(5) . . ? C23A C20 C13 117.2(6) . . ? C22 C20 C21A 73.4(7) . . ? C23A C20 C21A 110.0(7) . . ? C13 C20 C21A 111.6(8) . . ? C22 C20 C23 110.0(5) . . ? C23A C20 C23 24.7(5) . . ? C13 C20 C23 109.4(5) . . ? C21A C20 C23 131.5(8) . . ? C22 C20 C22A 31.1(6) . . ? C23A C20 C22A 106.2(7) . . ? C13 C20 C22A 106.3(7) . . ? C21A C20 C22A 104.4(8) . . ? C23 C20 C22A 87.3(7) . . ? C22 C20 C21 107.3(6) . . ? C23A C20 C21 82.6(6) . . ? C13 C20 C21 106.8(5) . . ? C21A C20 C21 36.0(7) . . ? C23 C20 C21 107.3(6) . . ? C22A C20 C21 136.4(8) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 C15 111.5(3) . . ? N1 C24 H24A 109.3 . . ? C15 C24 H24A 109.3 . . ? N1 C24 H24B 109.3 . . ? C15 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? N1 C25 C26 114.9(3) . . ? N1 C25 H25A 108.6 . . ? C26 C25 H25A 108.6 . . ? N1 C25 H25B 108.6 . . ? C26 C25 H25B 108.6 . . ? H25A C25 H25B 107.5 . . ? C29B C26 N2 125.3(11) . . ? C29B C26 C25 103.7(11) . . ? N2 C26 C25 114.2(3) . . ? C29B C26 H26 103.8 . . ? N2 C26 H26 103.8 . . ? C25 C26 H26 103.8 . . ? N2 C27 C29 120.2(4) . . ? N2 C27 C28 113.3(4) . . ? C29 C27 C28 107.3(4) . . ? N2 C27 H27 104.9 . . ? C29 C27 H27 104.9 . . ? C28 C27 H27 104.9 . . ? C29A C28 N1 128.1(8) . . ? C29A C28 C27 106.6(8) . . ? N1 C28 C27 114.6(3) . . ? C29A C28 H28 100.9 . . ? N1 C28 H28 100.9 . . ? C27 C28 H28 100.9 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C40 C39 N2 113.8(3) . . ? C40 C39 H39A 108.8 . . ? N2 C39 H39A 108.8 . . ? C40 C39 H39B 108.8 . . ? N2 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C41 C40 C45 119.6(4) . . ? C41 C40 C39 121.0(4) . . ? C45 C40 C39 119.4(4) . . ? C42 C41 C40 122.1(4) . . ? C42 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? C41 C42 C43 117.3(4) . . ? C41 C42 C50 124.1(5) . . ? C43 C42 C50 118.6(5) . . ? C44 C43 C42 123.5(5) . . ? C44 C43 H43 118.2 . . ? C42 C43 H43 118.2 . . ? C43 C44 C45 117.4(4) . . ? C43 C44 C46 121.5(4) . . ? C45 C44 C46 121.0(4) . . ? O8 C45 C40 118.7(4) . . ? O8 C45 C44 121.3(4) . . ? C40 C45 C44 120.0(4) . . ? C49 C46 C47 106.9(4) . . ? C49 C46 C44 111.1(4) . . ? C47 C46 C44 112.4(4) . . ? C49 C46 C48 110.1(4) . . ? C47 C46 C48 107.5(4) . . ? C44 C46 C48 108.9(4) . . ? 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 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 C42 110.9(6) . . ? C51 C50 C53A 84.6(8) . . ? C42 C50 C53A 114.8(9) . . ? C51 C50 C53 110.4(7) . . ? C42 C50 C53 110.0(7) . . ? C53A C50 C53 26.9(8) . . ? C51 C50 C52A 125.6(9) . . ? C42 C50 C52A 111.0(8) . . ? C53A C50 C52A 107.2(8) . . ? C53 C50 C52A 85.7(8) . . ? C51 C50 C52 111.0(7) . . ? C42 C50 C52 109.2(6) . . ? C53A C50 C52 123.4(10) . . ? C53 C50 C52 105.0(6) . . ? C52A C50 C52 20.5(7) . . ? C51 C50 C51A 25.7(6) . . ? C42 C50 C51A 111.5(7) . . ? C53A C50 C51A 106.7(8) . . ? C53 C50 C51A 129.2(8) . . ? C52A C50 C51A 105.1(7) . . ? C52 C50 C51A 87.6(7) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O5A C54 C56 106.3(10) . . ? O5A C54 C55 107.8(11) . . ? C56 C54 C55 114.4(5) . . ? O5A C54 H54 109.4 . . ? C56 C54 H54 109.4 . . ? C55 C54 H54 109.4 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O6 C57 C58 114.1(10) . . ? O6 C57 C59 127.5(10) . . ? C58 C57 C59 116.1(6) . . ? O6 C57 H57 95.0 . . ? C58 C57 H57 95.0 . . ? C59 C57 H57 95.0 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O7 C60 C61 102.3(10) . . ? O7 C60 C62 114.9(9) . . ? C61 C60 C62 114.1(5) . . ? O7 C60 H60 108.4 . . ? C61 C60 H60 108.4 . . ? C62 C60 H60 108.4 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C54 O5A Ti2 163.2(6) . . ? C57A O6A Ti2 140.1(7) . . ? C60A O7A Ti2 134.6(7) . . ? C20 C21A H21D 109.5 . . ? C20 C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C20 C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C20 C22A H22D 109.5 . . ? C20 C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C20 C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C20 C23A H23D 109.5 . . ? C20 C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C20 C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C28 C29A H29D 109.5 . . ? C28 C29A H29E 109.5 . . ? H29D C29A H29E 109.5 . . ? C28 C29A H29F 109.5 . . ? H29D C29A H29F 109.5 . . ? H29E C29A H29F 109.5 . . ? C50 C51A H51D 109.5 . . ? C50 C51A H51E 109.5 . . ? H51D C51A H51E 109.5 . . ? C50 C51A H51F 109.5 . . ? H51D C51A H51F 109.5 . . ? H51E C51A H51F 109.5 . . ? C50 C52A H52D 109.5 . . ? C50 C52A H52E 109.5 . . ? H52D C52A H52E 109.5 . . ? C50 C52A H52F 109.5 . . ? H52D C52A H52F 109.5 . . ? H52E C52A H52F 109.5 . . ? C50 C53A H53D 109.5 . . ? C50 C53A H53E 109.5 . . ? H53D C53A H53E 109.5 . . ? C50 C53A H53F 109.5 . . ? H53D C53A H53F 109.5 . . ? H53E C53A H53F 109.5 . . ? O5 C54A C56A 111.9(14) . . ? O5 C54A C55A 113.9(13) . . ? C56A C54A C55A 115.1(6) . . ? O5 C54A H54A 104.9 . . ? C56A C54A H54A 104.9 . . ? C55A C54A H54A 104.9 . . ? C54A C55A H55D 109.5 . . ? C54A C55A H55E 109.5 . . ? H55D C55A H55E 109.5 . . ? C54A C55A H55F 109.5 . . ? H55D C55A H55F 109.5 . . ? H55E C55A H55F 109.5 . . ? C54A C56A H56D 109.5 . . ? C54A C56A H56E 109.5 . . ? H56D C56A H56E 109.5 . . ? C54A C56A H56F 109.5 . . ? H56D C56A H56F 109.5 . . ? H56E C56A H56F 109.5 . . ? O6A C57A C59A 116.3(14) . . ? O6A C57A C58A 106.4(10) . . ? C59A C57A C58A 115.1(6) . . ? O6A C57A H57A 106.1 . . ? C59A C57A H57A 106.1 . . ? C58A C57A H57A 106.1 . . ? C57A C58A H58D 109.5 . . ? C57A C58A H58E 109.5 . . ? H58D C58A H58E 109.5 . . ? C57A C58A H58F 109.5 . . ? H58D C58A H58F 109.5 . . ? H58E C58A H58F 109.5 . . ? C57A C59A H59D 109.5 . . ? C57A C59A H59E 109.5 . . ? H59D C59A H59E 109.5 . . ? C57A C59A H59F 109.5 . . ? H59D C59A H59F 109.5 . . ? H59E C59A H59F 109.5 . . ? O7A C60A C62A 109.2(13) . . ? O7A C60A C61A 106.5(10) . . ? C62A C60A C61A 114.6(9) . . ? O7A C60A H60A 108.8 . . ? C62A C60A H60A 108.8 . . ? C61A C60A H60A 108.8 . . ? C60A C61A H61D 109.5 . . ? C60A C61A H61E 109.5 . . ? H61D C61A H61E 109.5 . . ? C60A C61A H61F 109.5 . . ? H61D C61A H61F 109.5 . . ? H61E C61A H61F 109.5 . . ? C60A C62A H62D 109.5 . . ? C60A C62A H62E 109.5 . . ? H62D C62A H62E 109.5 . . ? C60A C62A H62F 109.5 . . ? H62D C62A H62F 109.5 . . ? H62E C62A H62F 109.5 . . ? C26 C29B H29G 109.5 . . ? C26 C29B H29H 109.5 . . ? H29G C29B H29H 109.5 . . ? C26 C29B H29I 109.5 . . ? H29G C29B H29I 109.5 . . ? H29H C29B H29I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.887 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.069 #===END data_Ti2(7)(OiPr)6 _database_code_depnum_ccdc_archive 'CCDC 800223' #TrackingRef '- cif-DT-ART-11-2010-001542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H83 N2 O8 Ti2' _chemical_formula_weight 899.95 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 9.4140(4) _cell_length_b 9.9250(4) _cell_length_c 13.9710(12) _cell_angle_alpha 92.550(2) _cell_angle_beta 94.4870(10) _cell_angle_gamma 92.879(3) _cell_volume 1298.18(13) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12787 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 487 _exptl_absorpt_coefficient_mu 0.355 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9323 _exptl_absorpt_correction_T_max 0.9653 _exptl_absorpt_process_details 'Sortav (Blessing 1995)' _exptl_special_details ; two isopropoxide groups were disordered in ratios of 70:30 and 80:20, these were refined isotropically. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18880 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5909 _reflns_number_gt 5199 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication (Farrugia, 1999)' _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^)+(0.0873P)^2^+0.8868P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5909 _refine_ls_number_parameters 284 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1747 _refine_ls_wR_factor_gt 0.1663 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.144 _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 0.72566(4) 0.69267(4) 0.34091(3) 0.03141(15) Uani 1 1 d D . . O1 O 0.876(3) 0.745(2) 0.277(2) 0.039(3) Uani 0.30 1 d PD A 1 N1 N 0.54442(19) 0.56895(19) 0.41163(12) 0.0311(4) Uani 1 1 d . A . C1 C 0.9705(7) 0.7731(6) 0.2120(5) 0.0180(12) Uiso 0.30 1 d PD A 1 H1 H 0.9587 0.6995 0.1603 0.022 Uiso 0.30 1 calc PR A 1 O2 O 0.6047(4) 0.8286(3) 0.3377(3) 0.0513(8) Uani 0.80 1 d P A 1 C2 C 0.9591(10) 0.9062(7) 0.1639(6) 0.0350(16) Uiso 0.30 1 d PD A 1 H2A H 0.8632 0.9108 0.1318 0.052 Uiso 0.30 1 calc PR A 1 H2B H 1.0298 0.9132 0.1162 0.052 Uiso 0.30 1 calc PR A 1 H2C H 0.9769 0.9808 0.2123 0.052 Uiso 0.30 1 calc PR A 1 O3 O 0.81389(19) 0.68185(19) 0.46184(12) 0.0437(4) Uani 1 1 d . A . C3 C 1.1141(8) 0.7655(10) 0.2619(6) 0.0441(18) Uiso 0.30 1 d PD A 1 H3A H 1.1178 0.6827 0.2974 0.066 Uiso 0.30 1 calc PR A 1 H3B H 1.1342 0.8441 0.3068 0.066 Uiso 0.30 1 calc PR A 1 H3C H 1.1855 0.7649 0.2145 0.066 Uiso 0.30 1 calc PR A 1 O4 O 0.68667(17) 0.55097(18) 0.24848(11) 0.0371(4) Uani 1 1 d . A . C4 C 0.5923(5) 0.9469(5) 0.2865(4) 0.0661(12) Uiso 0.80 1 d PD A 1 H4 H 0.6910 0.9891 0.2861 0.079 Uiso 0.80 1 calc PR A 1 C6 C 0.5412(6) 0.9141(6) 0.1850(4) 0.0826(14) Uiso 0.80 1 d PD A 1 H6A H 0.6067 0.8537 0.1558 0.124 Uiso 0.80 1 calc PR A 1 H6B H 0.5375 0.9975 0.1501 0.124 Uiso 0.80 1 calc PR A 1 H6C H 0.4457 0.8694 0.1820 0.124 Uiso 0.80 1 calc PR A 1 C7 C 0.9295(3) 0.7609(3) 0.5107(2) 0.0547(7) Uani 1 1 d . . . H7 H 0.9960 0.7928 0.4630 0.066 Uiso 1 1 calc R A . C8 C 0.8739(6) 0.8811(4) 0.5624(4) 0.0949(14) Uani 1 1 d . A . H8A H 0.8242 0.9368 0.5157 0.142 Uiso 1 1 calc R . . H8B H 0.9538 0.9347 0.5968 0.142 Uiso 1 1 calc R . . H8C H 0.8075 0.8501 0.6084 0.142 Uiso 1 1 calc R . . C9 C 1.0080(4) 0.6732(5) 0.5812(3) 0.0836(12) Uani 1 1 d . A . H9A H 1.0440 0.5960 0.5462 0.125 Uiso 1 1 calc R . . H9B H 0.9427 0.6407 0.6274 0.125 Uiso 1 1 calc R . . H9C H 1.0883 0.7264 0.6155 0.125 Uiso 1 1 calc R . . C10 C 0.5856(2) 0.4567(2) 0.21287(15) 0.0317(4) Uani 1 1 d . . . C11 C 0.6115(3) 0.3683(2) 0.13432(15) 0.0358(5) Uani 1 1 d . A . C12 C 0.5009(3) 0.2760(3) 0.10076(17) 0.0418(5) Uani 1 1 d . . . H12 H 0.5159 0.2164 0.0478 0.050 Uiso 1 1 calc R A . C13 C 0.3699(3) 0.2657(3) 0.13998(18) 0.0437(6) Uani 1 1 d . A . C14 C 0.3491(3) 0.3519(2) 0.21780(17) 0.0385(5) Uani 1 1 d . . . H14 H 0.2611 0.3456 0.2467 0.046 Uiso 1 1 calc R A . C15 C 0.4552(2) 0.4476(2) 0.25441(15) 0.0314(4) Uani 1 1 d . A . C16 C 0.7534(3) 0.3787(3) 0.08694(18) 0.0451(6) Uani 1 1 d . . . C17 C 0.8802(3) 0.3632(4) 0.1608(2) 0.0645(9) Uani 1 1 d . A . H17A H 0.9695 0.3757 0.1299 0.097 Uiso 1 1 calc R . . H17B H 0.8739 0.2727 0.1861 0.097 Uiso 1 1 calc R . . H17C H 0.8782 0.4312 0.2137 0.097 Uiso 1 1 calc R . . C18 C 0.7666(3) 0.5143(4) 0.0406(2) 0.0583(7) Uani 1 1 d . A . H18A H 0.6893 0.5192 -0.0101 0.087 Uiso 1 1 calc R . . H18B H 0.8588 0.5236 0.0128 0.087 Uiso 1 1 calc R . . H18C H 0.7601 0.5874 0.0894 0.087 Uiso 1 1 calc R . . C19 C 0.7616(4) 0.2669(4) 0.0079(3) 0.0772(11) Uani 1 1 d . A . H19A H 0.6896 0.2795 -0.0450 0.116 Uiso 1 1 calc R . . H19B H 0.7436 0.1785 0.0345 0.116 Uiso 1 1 calc R . . H19C H 0.8567 0.2714 -0.0160 0.116 Uiso 1 1 calc R . . C20 C 0.2523(4) 0.1650(3) 0.0985(2) 0.0630(8) Uani 1 1 d . . . H20A H 0.1864 0.1457 0.1478 0.095 Uiso 1 1 calc R A . H20B H 0.2942 0.0812 0.0777 0.095 Uiso 1 1 calc R . . H20C H 0.2003 0.2028 0.0434 0.095 Uiso 1 1 calc R . . C21 C 0.4247(2) 0.5444(2) 0.33547(15) 0.0334(4) Uani 1 1 d . . . H21A H 0.4011 0.6318 0.3085 0.040 Uiso 1 1 calc R A . H21B H 0.3396 0.5085 0.3654 0.040 Uiso 1 1 calc R . . C22 C 0.6037(2) 0.4423(2) 0.44612(15) 0.0318(4) Uani 1 1 d . . . H22A H 0.6926 0.4660 0.4874 0.038 Uiso 1 1 calc R A . H22B H 0.6297 0.3874 0.3898 0.038 Uiso 1 1 calc R . . C23 C 0.4957(2) 0.6447(2) 0.49738(15) 0.0337(5) Uani 1 1 d . . . H23 H 0.5821 0.6735 0.5411 0.040 Uiso 1 1 calc R A . C24 C 0.4099(7) 0.7773(6) 0.4742(4) 0.0487(12) Uani 0.50 1 d P A . H24A H 0.4662 0.8363 0.4353 0.073 Uiso 0.50 1 calc PR . . H24B H 0.3931 0.8259 0.5345 0.073 Uiso 0.50 1 calc PR . . H24C H 0.3182 0.7505 0.4386 0.073 Uiso 0.50 1 calc PR . . C3A C 1.1065(8) 0.6903(9) 0.2558(6) 0.104(2) Uiso 0.70 1 d PD A 2 H3A1 H 1.0709 0.6101 0.2869 0.157 Uiso 0.70 1 calc PR A 2 H3A2 H 1.1794 0.7402 0.2993 0.157 Uiso 0.70 1 calc PR A 2 H3A3 H 1.1484 0.6623 0.1965 0.157 Uiso 0.70 1 calc PR A 2 O1A O 0.8736(10) 0.7748(9) 0.2897(8) 0.0385(15) Uani 0.70 1 d PD A 2 C1A C 0.9932(9) 0.7735(8) 0.2339(7) 0.102(3) Uiso 0.70 1 d PD A 2 H1A H 0.9464 0.7157 0.1787 0.122 Uiso 0.70 1 calc PR A 2 C2A C 1.0085(9) 0.8946(8) 0.1830(6) 0.095(2) Uiso 0.70 1 d PD A 2 H2A1 H 0.9144 0.9300 0.1683 0.143 Uiso 0.70 1 calc PR A 2 H2A2 H 1.0525 0.8748 0.1230 0.143 Uiso 0.70 1 calc PR A 2 H2A3 H 1.0691 0.9619 0.2228 0.143 Uiso 0.70 1 calc PR A 2 C5A C 0.6979(14) 1.0565(12) 0.2843(10) 0.047(3) Uiso 0.20 1 d PD A 2 H5A1 H 0.6922 1.0757 0.3533 0.071 Uiso 0.20 1 calc PR A 2 H5A2 H 0.6722 1.1361 0.2491 0.071 Uiso 0.20 1 calc PR A 2 H5A3 H 0.7954 1.0343 0.2724 0.071 Uiso 0.20 1 calc PR A 2 O2A O 0.6087(16) 0.8194(15) 0.3053(9) 0.039(3) Uiso 0.20 1 d P A 2 C6A C 0.5888(17) 0.9048(15) 0.1513(9) 0.049(3) Uiso 0.20 1 d PD A 2 H6A1 H 0.5186 0.8285 0.1386 0.073 Uiso 0.20 1 calc PR A 2 H6A2 H 0.6818 0.8782 0.1323 0.073 Uiso 0.20 1 calc PR A 2 H6A3 H 0.5582 0.9812 0.1143 0.073 Uiso 0.20 1 calc PR A 2 C4A C 0.6003(13) 0.9435(12) 0.2521(9) 0.038(3) Uiso 0.20 1 d PD A 2 H4A H 0.5041 0.9762 0.2639 0.046 Uiso 0.20 1 calc PR A 2 C5 C 0.5106(11) 1.0427(10) 0.3372(8) 0.166(4) Uiso 0.80 1 d PD A 1 H5A H 0.5529 1.0585 0.4034 0.249 Uiso 0.80 1 calc PR A 1 H5B H 0.4120 1.0064 0.3381 0.249 Uiso 0.80 1 calc PR A 1 H5C H 0.5115 1.1281 0.3046 0.249 Uiso 0.80 1 calc PR A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0289(2) 0.0357(2) 0.0303(2) 0.00311(15) 0.00621(15) 0.00067(15) O1 0.044(5) 0.038(8) 0.033(6) -0.012(5) 0.017(4) -0.013(5) N1 0.0306(9) 0.0393(10) 0.0234(8) 0.0005(7) 0.0046(7) 0.0002(7) O2 0.0482(16) 0.0446(15) 0.062(2) 0.0012(16) 0.0061(16) 0.0140(10) O3 0.0391(9) 0.0568(11) 0.0332(8) 0.0014(7) 0.0008(7) -0.0136(8) O4 0.0318(8) 0.0500(9) 0.0293(8) -0.0050(6) 0.0079(6) -0.0013(7) C7 0.0469(15) 0.0764(19) 0.0371(13) -0.0051(12) 0.0033(11) -0.0256(14) C8 0.111(4) 0.069(2) 0.097(3) -0.027(2) -0.010(3) -0.015(2) C9 0.057(2) 0.108(3) 0.079(3) -0.004(2) -0.0251(19) -0.002(2) C10 0.0346(10) 0.0370(11) 0.0237(9) 0.0037(8) 0.0007(8) 0.0046(8) C11 0.0430(12) 0.0407(12) 0.0243(10) 0.0016(8) 0.0024(8) 0.0086(9) C12 0.0563(15) 0.0399(12) 0.0288(11) -0.0020(9) 0.0008(10) 0.0051(10) C13 0.0525(14) 0.0413(13) 0.0354(12) 0.0018(9) -0.0028(10) -0.0066(11) C14 0.0386(12) 0.0449(13) 0.0315(11) 0.0056(9) 0.0019(9) -0.0033(10) C15 0.0332(10) 0.0370(11) 0.0241(9) 0.0045(8) 0.0011(8) 0.0027(8) C16 0.0451(13) 0.0593(16) 0.0314(11) -0.0084(10) 0.0078(10) 0.0104(11) C17 0.0487(16) 0.094(2) 0.0533(17) -0.0060(16) 0.0048(13) 0.0309(16) C18 0.0531(16) 0.078(2) 0.0457(15) 0.0093(14) 0.0171(12) -0.0020(14) C19 0.077(2) 0.092(3) 0.063(2) -0.0344(19) 0.0288(18) 0.001(2) C20 0.068(2) 0.0589(18) 0.0579(18) -0.0110(14) 0.0007(15) -0.0180(15) C21 0.0287(10) 0.0444(12) 0.0276(10) 0.0013(8) 0.0043(8) 0.0025(8) C22 0.0298(10) 0.0402(11) 0.0257(9) 0.0006(8) 0.0054(8) 0.0014(8) C23 0.0359(11) 0.0383(11) 0.0272(10) 0.0000(8) 0.0074(8) -0.0017(9) C24 0.064(3) 0.044(3) 0.041(3) 0.002(2) 0.016(2) 0.013(2) O1A 0.0405(19) 0.041(4) 0.034(3) -0.007(3) 0.0090(16) -0.008(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 O2A 1.775(15) . ? Ti1 O1A 1.791(3) . ? Ti1 O1 1.796(5) . ? Ti1 O2 1.809(3) . ? Ti1 O3 1.8334(18) . ? Ti1 O4 1.8689(16) . ? Ti1 N1 2.3572(18) . ? O1 C1 1.350(10) . ? N1 C22 1.486(3) . ? N1 C21 1.491(3) . ? N1 C23 1.500(3) . ? C1 C3 1.479(8) . ? C1 C2 1.513(7) . ? C1 H1 1.0000 . ? O2 C4 1.406(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C7 1.419(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C10 1.350(3) . ? C4 C5 1.448(8) . ? C4 C6 1.478(6) . ? C4 H4 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.505(6) . ? C7 C9 1.517(5) . ? C7 H7 1.0000 . ? 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 C15 1.399(3) . ? C10 C11 1.418(3) . ? C11 C12 1.390(4) . ? C11 C16 1.538(3) . ? C12 C13 1.389(4) . ? C12 H12 0.9500 . ? C13 C14 1.385(4) . ? C13 C20 1.516(4) . ? C14 C15 1.394(3) . ? C14 H14 0.9500 . ? C15 C21 1.506(3) . ? C16 C18 1.523(4) . ? C16 C17 1.534(4) . ? C16 C19 1.539(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.529(3) 2_666 ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C22 1.529(3) 2_666 ? C23 C24 1.611(6) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C3A C1A 1.406(8) . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? O1A C1A 1.419(10) . ? C1A C2A 1.430(8) . ? C1A H1A 1.0000 . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? C5A C4A 1.447(9) . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? O2A C4A 1.47(2) . ? C6A C4A 1.438(9) . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C4A H4A 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 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 O2A Ti1 O1A 92.6(6) . . ? O2A Ti1 O1 98.6(12) . . ? O1A Ti1 O1 10.9(8) . . ? O2A Ti1 O2 14.8(4) . . ? O1A Ti1 O2 99.2(4) . . ? O1 Ti1 O2 107.0(10) . . ? O2A Ti1 O3 125.0(4) . . ? O1A Ti1 O3 96.4(5) . . ? O1 Ti1 O3 100.1(11) . . ? O2 Ti1 O3 110.79(14) . . ? O2A Ti1 O4 105.0(4) . . ? O1A Ti1 O4 98.6(3) . . ? O1 Ti1 O4 88.2(6) . . ? O2 Ti1 O4 116.71(14) . . ? O3 Ti1 O4 126.68(8) . . ? O2A Ti1 N1 92.5(5) . . ? O1A Ti1 N1 174.9(4) . . ? O1 Ti1 N1 165.4(7) . . ? O2 Ti1 N1 85.86(13) . . ? O3 Ti1 N1 80.89(7) . . ? O4 Ti1 N1 79.78(7) . . ? C1 O1 Ti1 168(2) . . ? C22 N1 C21 112.99(17) . . ? C22 N1 C23 107.17(16) . . ? C21 N1 C23 110.62(17) . . ? C22 N1 Ti1 108.25(12) . . ? C21 N1 Ti1 106.17(13) . . ? C23 N1 Ti1 111.69(13) . . ? O1 C1 C3 106.7(17) . . ? O1 C1 C2 117.0(14) . . ? C3 C1 C2 110.1(6) . . ? O1 C1 H1 107.6 . . ? C3 C1 H1 107.6 . . ? C2 C1 H1 107.6 . . ? C4 O2 Ti1 135.2(3) . . ? 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 . . ? C7 O3 Ti1 130.82(17) . . ? 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 . . ? C10 O4 Ti1 143.47(14) . . ? O2 C4 C5 110.3(6) . . ? O2 C4 C6 110.8(4) . . ? C5 C4 C6 115.5(6) . . ? O2 C4 H4 106.6 . . ? C5 C4 H4 106.6 . . ? C6 C4 H4 106.6 . . ? 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 C8 109.7(3) . . ? O3 C7 C9 108.5(3) . . ? C8 C7 C9 110.6(3) . . ? O3 C7 H7 109.3 . . ? C8 C7 H7 109.3 . . ? C9 C7 H7 109.3 . . ? 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 . . ? O4 C10 C15 119.10(19) . . ? O4 C10 C11 120.3(2) . . ? C15 C10 C11 120.6(2) . . ? C12 C11 C10 116.7(2) . . ? C12 C11 C16 122.2(2) . . ? C10 C11 C16 121.1(2) . . ? C11 C12 C13 123.9(2) . . ? C11 C12 H12 118.0 . . ? C13 C12 H12 118.0 . . ? C14 C13 C12 117.9(2) . . ? C14 C13 C20 120.8(3) . . ? C12 C13 C20 121.4(2) . . ? C13 C14 C15 121.1(2) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C10 119.8(2) . . ? C14 C15 C21 119.2(2) . . ? C10 C15 C21 120.94(19) . . ? C18 C16 C17 110.6(3) . . ? C18 C16 C11 108.9(2) . . ? C17 C16 C11 111.0(2) . . ? C18 C16 C19 107.9(3) . . ? C17 C16 C19 106.5(3) . . ? C11 C16 C19 111.9(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C13 C20 H20A 109.5 . . ? C13 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C13 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 C15 114.48(18) . . ? N1 C21 H21A 108.6 . . ? C15 C21 H21A 108.6 . . ? N1 C21 H21B 108.6 . . ? C15 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? N1 C22 C23 115.30(18) . 2_666 ? N1 C22 H22A 108.4 . . ? C23 C22 H22A 108.4 2_666 . ? N1 C22 H22B 108.4 . . ? C23 C22 H22B 108.4 2_666 . ? H22A C22 H22B 107.5 . . ? N1 C23 C22 112.49(17) . 2_666 ? N1 C23 C24 115.4(2) . . ? C22 C23 C24 105.1(3) 2_666 . ? N1 C23 H23 107.8 . . ? C22 C23 H23 107.8 2_666 . ? C24 C23 H23 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C1A C3A H3A1 109.5 . . ? C1A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C1A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C1A O1A Ti1 152.1(7) . . ? C3A C1A O1A 121.1(9) . . ? C3A C1A C2A 123.3(8) . . ? O1A C1A C2A 111.6(8) . . ? C3A C1A H1A 96.7 . . ? O1A C1A H1A 96.7 . . ? C2A C1A H1A 96.7 . . ? C1A C2A H2A1 109.5 . . ? C1A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? C1A C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? C4A C5A H5A1 109.5 . . ? C4A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C4A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? C4A O2A Ti1 143.0(11) . . ? C4A C6A H6A1 109.5 . . ? C4A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C4A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C6A C4A C5A 117.4(12) . . ? C6A C4A O2A 107.5(11) . . ? C5A C4A O2A 117.8(11) . . ? C6A C4A H4A 104.1 . . ? C5A C4A H4A 104.1 . . ? O2A C4A H4A 104.1 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.942 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.066 #===END data_Ti2(8)(OiPr)6 _database_code_depnum_ccdc_archive 'CCDC 800224' #TrackingRef '- cif-DT-ART-11-2010-001542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H103 N2 O8 Ti2' _chemical_formula_weight 1028.20 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14.2220(3) _cell_length_b 15.3740(4) _cell_length_c 17.4080(4) _cell_angle_alpha 69.6250(10) _cell_angle_beta 89.943(2) _cell_angle_gamma 62.8660(10) _cell_volume 3118.09(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 41364 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1122 _exptl_absorpt_coefficient_mu 0.303 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; 'two isopropoxide groups were disordered in a 60:40 ratio.' ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53805 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14135 _reflns_number_gt 9735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0913P)^2^+2.5340P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14135 _refine_ls_number_parameters 717 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1847 _refine_ls_wR_factor_gt 0.1579 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.007 _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 0.23928(4) 0.36431(4) 0.33002(3) 0.03396(14) Uani 1 1 d . A . O1 O 0.13096(16) 0.35859(18) 0.37869(13) 0.0487(5) Uani 1 1 d . . . N1 N 0.39379(16) 0.35149(16) 0.27131(12) 0.0278(4) Uani 1 1 d . . . C1 C 0.1267(3) 0.5798(3) 0.3303(3) 0.0631(10) Uani 1 1 d . A . H1 H 0.1244 0.5379 0.3882 0.076 Uiso 1 1 calc R . . Ti2 Ti 0.71970(4) 0.22038(4) 0.10337(3) 0.03302(13) Uani 1 1 d . . . O2 O 0.19867(16) 0.50386(16) 0.29905(13) 0.0458(5) Uani 1 1 d . . . N2 N 0.55448(16) 0.24481(16) 0.14401(12) 0.0284(4) Uani 1 1 d . A . C2 C 0.1695(3) 0.6477(3) 0.3382(3) 0.0696(11) Uani 1 1 d . . . H2A H 0.2410 0.6032 0.3739 0.104 Uiso 1 1 calc R A . H2B H 0.1212 0.6956 0.3630 0.104 Uiso 1 1 calc R . . H2C H 0.1748 0.6896 0.2828 0.104 Uiso 1 1 calc R . . O3 O 0.22073(16) 0.32432(18) 0.24608(13) 0.0449(5) Uani 1 1 d . . . C3 C 0.0174(3) 0.6359(4) 0.2830(4) 0.0911(15) Uani 1 1 d . . . H3A H 0.0153 0.6779 0.2252 0.137 Uiso 1 1 calc R A . H3B H -0.0312 0.6831 0.3082 0.137 Uiso 1 1 calc R . . H3C H -0.0054 0.5844 0.2837 0.137 Uiso 1 1 calc R . . O4 O 0.34511(14) 0.27774(16) 0.42626(11) 0.0369(4) Uani 1 1 d . . . C4 C 0.0806(7) 0.3167(8) 0.4416(6) 0.096(3) Uani 0.60 1 d PD A 1 H4 H 0.1378 0.2455 0.4812 0.115 Uiso 0.60 1 calc PR A 1 O5 O 0.77735(15) 0.09773(16) 0.19494(13) 0.0445(5) Uani 1 1 d . B . C5 C 0.0023(8) 0.3002(9) 0.4039(7) 0.132(5) Uani 0.60 1 d PD A 1 H5A H -0.0437 0.3640 0.3544 0.198 Uiso 0.60 1 calc PR A 1 H5B H -0.0422 0.2858 0.4443 0.198 Uiso 0.60 1 calc PR A 1 H5C H 0.0398 0.2396 0.3878 0.198 Uiso 0.60 1 calc PR A 1 O6 O 0.83890(16) 0.21046(18) 0.06396(14) 0.0484(5) Uani 1 1 d . B . C6 C 0.0378(8) 0.3837(8) 0.4891(6) 0.107(3) Uani 0.60 1 d PD A 1 H6A H -0.0094 0.4574 0.4506 0.161 Uiso 0.60 1 calc PR A 1 H6B H 0.0974 0.3799 0.5209 0.161 Uiso 0.60 1 calc PR A 1 H6C H -0.0032 0.3589 0.5276 0.161 Uiso 0.60 1 calc PR A 1 O7 O 0.68517(15) 0.33722(16) 0.12800(13) 0.0417(5) Uani 1 1 d . B 1 C7 C 0.1415(3) 0.3120(3) 0.2094(2) 0.0579(9) Uani 1 1 d U A . H7 H 0.0998 0.2947 0.2530 0.069 Uiso 1 1 calc R . . O8 O 0.65455(15) 0.21899(15) 0.01008(11) 0.0362(4) Uani 1 1 d . A . C8 C 0.0656(5) 0.4138(5) 0.1408(4) 0.134(2) Uani 1 1 d U . . H8A H 0.0385 0.4710 0.1614 0.201 Uiso 1 1 calc R A . H8B H 0.0051 0.4081 0.1207 0.201 Uiso 1 1 calc R . . H8C H 0.1029 0.4296 0.0949 0.201 Uiso 1 1 calc R . . C9 C 0.1951(4) 0.2201(5) 0.1841(4) 0.115(2) Uani 1 1 d . . . H9A H 0.2328 0.2367 0.1388 0.173 Uiso 1 1 calc R A . H9B H 0.1408 0.2059 0.1650 0.173 Uiso 1 1 calc R . . H9C H 0.2468 0.1573 0.2320 0.173 Uiso 1 1 calc R . . C10 C 0.4501(2) 0.2365(2) 0.45807(16) 0.0314(5) Uani 1 1 d . A . C11 C 0.4958(2) 0.1556(2) 0.53801(16) 0.0343(6) Uani 1 1 d . . . C12 C 0.6062(2) 0.1141(2) 0.56535(17) 0.0373(6) Uani 1 1 d . A . H12 H 0.6392 0.0584 0.6190 0.045 Uiso 1 1 calc R . . C13 C 0.6701(2) 0.1500(2) 0.51815(17) 0.0370(6) Uani 1 1 d . . . C14 C 0.6202(2) 0.2321(2) 0.44046(17) 0.0343(6) Uani 1 1 d . A . H14 H 0.6617 0.2586 0.4072 0.041 Uiso 1 1 calc R . . C15 C 0.5112(2) 0.2769(2) 0.40975(15) 0.0304(5) Uani 1 1 d . . . C16 C 0.4284(2) 0.1153(2) 0.59340(17) 0.0388(6) Uani 1 1 d . A . C17 C 0.3805(3) 0.0667(3) 0.55184(19) 0.0456(7) Uani 1 1 d . . . H17A H 0.3350 0.1205 0.4978 0.068 Uiso 1 1 calc R A . H17B H 0.3372 0.0422 0.5879 0.068 Uiso 1 1 calc R . . H17C H 0.4390 0.0065 0.5435 0.068 Uiso 1 1 calc R . . C18 C 0.3363(3) 0.2097(3) 0.60748(19) 0.0489(7) Uani 1 1 d . . . H18A H 0.3669 0.2368 0.6379 0.073 Uiso 1 1 calc R A . H18B H 0.2902 0.1859 0.6401 0.073 Uiso 1 1 calc R . . H18C H 0.2936 0.2663 0.5534 0.073 Uiso 1 1 calc R . . C19 C 0.4942(3) 0.0303(3) 0.67927(19) 0.0519(8) Uani 1 1 d . . . H19A H 0.5544 -0.0300 0.6724 0.078 Uiso 1 1 calc R A . H19B H 0.4482 0.0061 0.7118 0.078 Uiso 1 1 calc R . . H19C H 0.5219 0.0603 0.7086 0.078 Uiso 1 1 calc R . . C20 C 0.7907(2) 0.0975(3) 0.5529(2) 0.0471(7) Uani 1 1 d . A . C21 C 0.8066(3) 0.1052(5) 0.6363(3) 0.0855(15) Uani 1 1 d . . . H21A H 0.7786 0.1798 0.6277 0.128 Uiso 1 1 calc R A . H21B H 0.8834 0.0650 0.6608 0.128 Uiso 1 1 calc R . . H21C H 0.7679 0.0756 0.6741 0.128 Uiso 1 1 calc R . . C22 C 0.8443(3) -0.0207(3) 0.5667(3) 0.0800(12) Uani 1 1 d . . . H22A H 0.8084 -0.0546 0.6040 0.120 Uiso 1 1 calc R A . H22B H 0.9205 -0.0557 0.5920 0.120 Uiso 1 1 calc R . . H22C H 0.8382 -0.0269 0.5130 0.120 Uiso 1 1 calc R . . C23 C 0.8473(3) 0.1478(4) 0.4936(3) 0.0822(13) Uani 1 1 d . . . H23A H 0.8360 0.1447 0.4393 0.123 Uiso 1 1 calc R A . H23B H 0.9246 0.1089 0.5167 0.123 Uiso 1 1 calc R . . H23C H 0.8178 0.2220 0.4867 0.123 Uiso 1 1 calc R . . C24 C 0.4576(2) 0.3690(2) 0.32645(15) 0.0310(5) Uani 1 1 d . A . H24A H 0.4095 0.4339 0.3358 0.037 Uiso 1 1 calc R . . H24B H 0.5134 0.3809 0.2979 0.037 Uiso 1 1 calc R . . C25 C 0.4552(2) 0.24617(19) 0.26663(15) 0.0291(5) Uani 1 1 d . A . H25A H 0.4084 0.2393 0.2298 0.035 Uiso 1 1 calc R . . H25B H 0.4711 0.1911 0.3230 0.035 Uiso 1 1 calc R . . C26 C 0.5617(2) 0.2221(2) 0.23489(15) 0.0297(5) Uani 1 1 d . . . H26A H 0.5905 0.2641 0.2478 0.036 Uiso 1 1 calc R A . H26B H 0.6141 0.1461 0.2662 0.036 Uiso 1 1 calc R . . C27 C 0.3537(2) 0.4387(2) 0.18666(15) 0.0303(5) Uani 1 1 d . A . H27A H 0.3234 0.5069 0.1938 0.036 Uiso 1 1 calc R . . H27B H 0.2937 0.4380 0.1586 0.036 Uiso 1 1 calc R . . C28 C 0.4339(2) 0.4375(2) 0.12780(16) 0.0324(5) Uani 1 1 d . . . H28A H 0.4024 0.5081 0.0813 0.039 Uiso 1 1 calc R A . H28B H 0.4999 0.4257 0.1585 0.039 Uiso 1 1 calc R . . C29 C 0.4649(2) 0.3530(2) 0.09140(15) 0.0307(5) Uani 1 1 d . A . H29A H 0.4005 0.3467 0.0804 0.037 Uiso 1 1 calc R . . H29B H 0.4856 0.3782 0.0370 0.037 Uiso 1 1 calc R . . C30 C 0.5371(2) 0.1627(2) 0.12911(15) 0.0308(5) Uani 1 1 d . . . H30A H 0.4786 0.1569 0.1573 0.037 Uiso 1 1 calc R A . H30B H 0.6034 0.0933 0.1551 0.037 Uiso 1 1 calc R . . C31 C 0.8819(2) 0.0133(3) 0.2371(2) 0.0527(8) Uani 1 1 d . . . H31 H 0.9306 0.0430 0.2406 0.063 Uiso 1 1 calc R B . C32 C 0.8759(4) -0.0474(4) 0.3225(3) 0.0998(18) Uani 1 1 d . B . H32A H 0.8456 0.0002 0.3521 0.150 Uiso 1 1 calc R . . H32B H 0.9482 -0.1044 0.3527 0.150 Uiso 1 1 calc R . . H32C H 0.8297 -0.0782 0.3192 0.150 Uiso 1 1 calc R . . C33 C 0.9247(4) -0.0577(3) 0.1874(3) 0.0864(13) Uani 1 1 d U B . H33A H 0.8814 -0.0927 0.1887 0.130 Uiso 1 1 calc R . . H33B H 0.9998 -0.1116 0.2122 0.130 Uiso 1 1 calc R . . H33C H 0.9200 -0.0141 0.1294 0.130 Uiso 1 1 calc R . . C34 C 0.8950(7) 0.2262(6) -0.0055(6) 0.118(5) Uani 0.60 1 d PD B 1 H34 H 0.8515 0.2352 -0.0556 0.142 Uiso 0.60 1 calc PR B 1 C35 C 0.9001(6) 0.3254(5) -0.0245(5) 0.074(2) Uani 0.60 1 d PD B 1 H35A H 0.9431 0.3185 0.0234 0.111 Uiso 0.60 1 calc PR B 1 H35B H 0.8272 0.3849 -0.0360 0.111 Uiso 0.60 1 calc PR B 1 H35C H 0.9335 0.3385 -0.0735 0.111 Uiso 0.60 1 calc PR B 1 C36 C 0.9986(7) 0.1319(6) 0.0133(8) 0.117(4) Uani 0.60 1 d PD B 1 H36A H 1.0460 0.1258 0.0580 0.176 Uiso 0.60 1 calc PR B 1 H36B H 1.0310 0.1371 -0.0367 0.176 Uiso 0.60 1 calc PR B 1 H36C H 0.9889 0.0691 0.0314 0.176 Uiso 0.60 1 calc PR B 1 C37 C 0.7510(3) 0.3748(3) 0.1516(2) 0.0553(8) Uani 1 1 d D . . H37 H 0.7907 0.3873 0.1052 0.066 Uiso 1 1 calc R B 1 C38 C 0.8322(6) 0.2986(6) 0.2263(5) 0.105(3) Uani 0.60 1 d PD B 1 H38A H 0.8805 0.3254 0.2344 0.158 Uiso 0.60 1 calc PR B 1 H38B H 0.8737 0.2308 0.2203 0.158 Uiso 0.60 1 calc PR B 1 H38C H 0.7972 0.2881 0.2747 0.158 Uiso 0.60 1 calc PR B 1 C39 C 0.6796(5) 0.4804(4) 0.1540(5) 0.0677(18) Uani 0.60 1 d PD B 1 H39A H 0.7217 0.5159 0.1551 0.102 Uiso 0.60 1 calc PR B 1 H39B H 0.6477 0.4711 0.2042 0.102 Uiso 0.60 1 calc PR B 1 H39C H 0.6222 0.5239 0.1044 0.102 Uiso 0.60 1 calc PR B 1 C40 C 0.5731(2) 0.2075(2) -0.01724(16) 0.0301(5) Uani 1 1 d . . . C41 C 0.5091(2) 0.1848(2) 0.03902(15) 0.0300(5) Uani 1 1 d . A . C42 C 0.4224(2) 0.1770(2) 0.01265(16) 0.0330(5) Uani 1 1 d . . . H42 H 0.3788 0.1631 0.0513 0.040 Uiso 1 1 calc R A . C43 C 0.3975(2) 0.1890(2) -0.06863(16) 0.0341(6) Uani 1 1 d . A . C44 C 0.4646(2) 0.2072(2) -0.12230(17) 0.0357(6) Uani 1 1 d . . . H44 H 0.4497 0.2137 -0.1778 0.043 Uiso 1 1 calc R A . C45 C 0.5530(2) 0.2166(2) -0.09973(16) 0.0324(5) Uani 1 1 d . A . C46 C 0.6258(2) 0.2336(2) -0.16202(18) 0.0391(6) Uani 1 1 d . . . C47 C 0.6239(3) 0.3385(3) -0.1760(2) 0.0508(8) Uani 1 1 d . A . H47A H 0.6488 0.3365 -0.1226 0.076 Uiso 1 1 calc R . . H47B H 0.5503 0.3973 -0.1993 0.076 Uiso 1 1 calc R . . H47C H 0.6714 0.3487 -0.2148 0.076 Uiso 1 1 calc R . . C48 C 0.7405(3) 0.1417(3) -0.1278(2) 0.0518(8) Uani 1 1 d . A . H48A H 0.7666 0.1370 -0.0737 0.078 Uiso 1 1 calc R . . H48B H 0.7871 0.1536 -0.1669 0.078 Uiso 1 1 calc R . . H48C H 0.7414 0.0752 -0.1209 0.078 Uiso 1 1 calc R . . C49 C 0.5881(3) 0.2405(3) -0.2472(2) 0.0595(9) Uani 1 1 d . A . H49A H 0.6339 0.2558 -0.2859 0.089 Uiso 1 1 calc R . . H49B H 0.5133 0.2974 -0.2691 0.089 Uiso 1 1 calc R . . H49C H 0.5928 0.1728 -0.2413 0.089 Uiso 1 1 calc R . . C50 C 0.2987(2) 0.1828(3) -0.09566(19) 0.0438(7) Uani 1 1 d . . . C51 C 0.3002(3) 0.0824(3) -0.0327(3) 0.0661(10) Uani 1 1 d . A . H51A H 0.2402 0.0759 -0.0525 0.099 Uiso 1 1 calc R . . H51B H 0.2931 0.0878 0.0217 0.099 Uiso 1 1 calc R . . H51C H 0.3683 0.0197 -0.0272 0.099 Uiso 1 1 calc R . . C52 C 0.2937(4) 0.1799(4) -0.1809(3) 0.0812(12) Uani 1 1 d U A . H52A H 0.2888 0.2451 -0.2222 0.122 Uiso 1 1 calc R . . H52B H 0.2303 0.1745 -0.1946 0.122 Uiso 1 1 calc R . . H52C H 0.3587 0.1183 -0.1815 0.122 Uiso 1 1 calc R . . C53 C 0.1972(3) 0.2787(4) -0.0931(3) 0.0727(11) Uani 1 1 d . A . H53A H 0.1910 0.3443 -0.1347 0.109 Uiso 1 1 calc R . . H53B H 0.2023 0.2801 -0.0374 0.109 Uiso 1 1 calc R . . H53C H 0.1336 0.2728 -0.1054 0.109 Uiso 1 1 calc R . . C54 C 0.5458(4) 0.4845(4) 0.4765(3) 0.0923(16) Uani 1 1 d . . . H54A H 0.5993 0.4091 0.5081 0.111 Uiso 1 1 calc R . . H54B H 0.5172 0.4909 0.4218 0.111 Uiso 1 1 calc R . . C55 C 0.6020(4) 0.5497(3) 0.4616(3) 0.0903(15) Uani 1 1 d . . . H55A H 0.5493 0.6253 0.4292 0.108 Uiso 1 1 calc R . . H55B H 0.6310 0.5438 0.5160 0.108 Uiso 1 1 calc R . . C56 C 0.6918(5) 0.5149(5) 0.4157(4) 0.123(2) Uani 1 1 d . . . H56A H 0.7464 0.4415 0.4491 0.185 Uiso 1 1 calc R . . H56B H 0.7243 0.5611 0.4054 0.185 Uiso 1 1 calc R . . H56C H 0.6638 0.5194 0.3623 0.185 Uiso 1 1 calc R . . C4A C 0.0360(8) 0.3587(11) 0.3997(6) 0.077(3) Uani 0.40 1 d PDU A 2 H4A H 0.0484 0.2989 0.3830 0.092 Uiso 0.40 1 calc PR A 2 C5A C -0.0644(8) 0.4336(11) 0.3404(8) 0.100(4) Uani 0.40 1 d PDU A 2 H5A1 H -0.1037 0.4951 0.3553 0.150 Uiso 0.40 1 calc PR A 2 H5A2 H -0.1082 0.3992 0.3418 0.150 Uiso 0.40 1 calc PR A 2 H5A3 H -0.0492 0.4571 0.2842 0.150 Uiso 0.40 1 calc PR A 2 C6A C 0.0490(11) 0.2980(12) 0.4880(7) 0.095(4) Uani 0.40 1 d PDU A 2 H6A1 H 0.0564 0.3362 0.5204 0.143 Uiso 0.40 1 calc PR A 2 H6A2 H 0.1135 0.2284 0.5050 0.143 Uiso 0.40 1 calc PR A 2 H6A3 H -0.0143 0.2887 0.4981 0.143 Uiso 0.40 1 calc PR A 2 C34A C 0.9231(8) 0.2183(8) 0.0308(7) 0.065(3) Uani 0.40 1 d PDU B 2 H34A H 0.9224 0.2692 0.0545 0.078 Uiso 0.40 1 calc PR B 2 C35A C 0.8994(18) 0.2899(16) -0.0565(8) 0.142(8) Uani 0.40 1 d PDU B 2 H35D H 0.9589 0.2586 -0.0838 0.213 Uiso 0.40 1 calc PR B 2 H35E H 0.8904 0.3582 -0.0596 0.213 Uiso 0.40 1 calc PR B 2 H35F H 0.8330 0.3010 -0.0848 0.213 Uiso 0.40 1 calc PR B 2 C36A C 1.0295(9) 0.1336(12) 0.0755(10) 0.111(5) Uani 0.40 1 d PDU B 2 H36D H 1.0336 0.0650 0.0858 0.167 Uiso 0.40 1 calc PR B 2 H36E H 1.0439 0.1374 0.1290 0.167 Uiso 0.40 1 calc PR B 2 H36F H 1.0830 0.1409 0.0422 0.167 Uiso 0.40 1 calc PR B 2 C38A C 0.7627(12) 0.3426(12) 0.2430(4) 0.087(3) Uani 0.40 1 d PDU B 2 H38D H 0.8215 0.3498 0.2639 0.131 Uiso 0.40 1 calc PR B 2 H38E H 0.7786 0.2684 0.2693 0.131 Uiso 0.40 1 calc PR B 2 H38F H 0.6955 0.3881 0.2565 0.131 Uiso 0.40 1 calc PR B 2 C39A C 0.7109(10) 0.4881(5) 0.1094(8) 0.077(3) Uani 0.40 1 d PDU B 2 H39D H 0.7121 0.5059 0.0497 0.116 Uiso 0.40 1 calc PR B 2 H39E H 0.7565 0.5084 0.1329 0.116 Uiso 0.40 1 calc PR B 2 H39F H 0.6369 0.5265 0.1170 0.116 Uiso 0.40 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0306(2) 0.0430(3) 0.0338(3) -0.0169(2) 0.01114(19) -0.0208(2) O1 0.0396(11) 0.0671(14) 0.0502(12) -0.0241(11) 0.0205(9) -0.0335(11) N1 0.0301(10) 0.0298(10) 0.0259(10) -0.0116(8) 0.0077(8) -0.0159(9) C1 0.0441(18) 0.056(2) 0.092(3) -0.038(2) 0.0286(19) -0.0202(16) Ti2 0.0279(2) 0.0389(3) 0.0364(3) -0.0163(2) 0.00933(19) -0.0183(2) O2 0.0403(11) 0.0422(11) 0.0536(12) -0.0214(10) 0.0200(9) -0.0171(9) N2 0.0312(11) 0.0322(11) 0.0250(10) -0.0116(9) 0.0076(8) -0.0175(9) C2 0.058(2) 0.065(2) 0.087(3) -0.045(2) 0.012(2) -0.0193(19) O3 0.0408(11) 0.0667(14) 0.0436(11) -0.0272(10) 0.0113(9) -0.0350(11) C3 0.052(2) 0.080(3) 0.126(4) -0.052(3) -0.002(3) -0.012(2) O4 0.0347(10) 0.0510(11) 0.0304(9) -0.0145(8) 0.0115(8) -0.0261(9) C4 0.085(6) 0.109(7) 0.094(7) -0.025(6) 0.059(6) -0.059(6) O5 0.0326(10) 0.0429(11) 0.0462(11) -0.0122(9) 0.0043(9) -0.0129(9) C5 0.127(8) 0.163(10) 0.218(13) -0.121(10) 0.116(9) -0.124(8) O6 0.0346(10) 0.0650(14) 0.0588(13) -0.0310(11) 0.0193(9) -0.0295(10) C6 0.098(7) 0.156(9) 0.091(6) -0.063(6) 0.068(5) -0.069(7) O7 0.0362(10) 0.0480(11) 0.0542(12) -0.0256(10) 0.0119(9) -0.0269(9) C7 0.0481(17) 0.081(2) 0.0595(19) -0.0326(17) 0.0053(15) -0.0395(17) O8 0.0363(10) 0.0474(11) 0.0358(10) -0.0200(9) 0.0153(8) -0.0263(9) C8 0.113(4) 0.134(4) 0.145(4) -0.045(3) -0.044(3) -0.059(3) C9 0.097(4) 0.129(5) 0.165(6) -0.099(5) 0.002(4) -0.059(4) C10 0.0347(13) 0.0388(14) 0.0303(12) -0.0184(11) 0.0105(10) -0.0217(12) C11 0.0455(15) 0.0401(14) 0.0299(13) -0.0177(11) 0.0125(11) -0.0276(13) C12 0.0456(15) 0.0384(14) 0.0300(13) -0.0137(11) 0.0055(11) -0.0218(13) C13 0.0370(14) 0.0418(15) 0.0363(14) -0.0187(12) 0.0061(11) -0.0199(13) C14 0.0358(13) 0.0415(14) 0.0363(14) -0.0201(12) 0.0120(11) -0.0237(12) C15 0.0366(13) 0.0355(13) 0.0290(12) -0.0178(11) 0.0105(10) -0.0215(11) C16 0.0540(17) 0.0458(16) 0.0308(13) -0.0174(12) 0.0158(12) -0.0336(14) C17 0.0590(19) 0.0581(19) 0.0428(16) -0.0240(14) 0.0206(14) -0.0435(16) C18 0.065(2) 0.0571(19) 0.0382(16) -0.0234(14) 0.0265(15) -0.0365(17) C19 0.072(2) 0.0537(19) 0.0359(16) -0.0111(14) 0.0119(15) -0.0403(18) C20 0.0347(15) 0.0571(19) 0.0453(17) -0.0205(15) 0.0041(13) -0.0186(14) C21 0.049(2) 0.138(4) 0.074(3) -0.059(3) 0.0054(19) -0.037(3) C22 0.057(2) 0.072(3) 0.088(3) -0.027(2) 0.007(2) -0.016(2) C23 0.045(2) 0.107(4) 0.078(3) -0.016(3) 0.0042(19) -0.038(2) C24 0.0342(13) 0.0362(13) 0.0296(12) -0.0148(11) 0.0107(10) -0.0212(11) C25 0.0339(13) 0.0298(12) 0.0265(12) -0.0114(10) 0.0072(10) -0.0175(11) C26 0.0323(13) 0.0325(13) 0.0239(11) -0.0101(10) 0.0056(10) -0.0161(11) C27 0.0304(12) 0.0297(12) 0.0290(12) -0.0098(10) 0.0078(10) -0.0143(11) C28 0.0348(13) 0.0320(13) 0.0274(12) -0.0082(10) 0.0074(10) -0.0164(11) C29 0.0305(12) 0.0330(13) 0.0266(12) -0.0105(10) 0.0058(10) -0.0148(11) C30 0.0340(13) 0.0348(13) 0.0302(12) -0.0141(11) 0.0102(10) -0.0209(11) C31 0.0324(15) 0.0487(18) 0.060(2) -0.0088(15) -0.0028(14) -0.0152(14) C32 0.065(3) 0.107(4) 0.060(3) 0.013(2) -0.002(2) -0.022(3) C33 0.080(3) 0.060(2) 0.099(3) -0.028(2) 0.022(2) -0.021(2) C34 0.121(9) 0.244(15) 0.120(9) -0.138(10) 0.088(7) -0.141(10) C35 0.073(4) 0.060(4) 0.083(5) -0.016(4) 0.049(4) -0.037(4) C36 0.092(6) 0.079(5) 0.208(12) -0.080(7) 0.113(7) -0.047(5) C37 0.059(2) 0.075(2) 0.067(2) -0.0404(19) 0.0264(17) -0.0514(19) C38 0.059(4) 0.071(5) 0.164(9) -0.049(6) -0.052(5) -0.013(4) C39 0.087(5) 0.057(4) 0.079(5) -0.029(3) 0.008(4) -0.049(4) C40 0.0305(12) 0.0304(12) 0.0347(13) -0.0152(11) 0.0107(10) -0.0171(11) C41 0.0345(13) 0.0311(12) 0.0299(12) -0.0151(10) 0.0123(10) -0.0179(11) C42 0.0355(13) 0.0389(14) 0.0345(13) -0.0193(11) 0.0146(11) -0.0222(12) C43 0.0367(14) 0.0393(14) 0.0342(13) -0.0199(12) 0.0107(11) -0.0208(12) C44 0.0438(15) 0.0399(14) 0.0309(13) -0.0187(11) 0.0131(11) -0.0228(13) C45 0.0374(14) 0.0329(13) 0.0327(13) -0.0163(11) 0.0144(11) -0.0192(11) C46 0.0508(16) 0.0450(15) 0.0380(14) -0.0233(13) 0.0243(13) -0.0309(14) C47 0.073(2) 0.0494(18) 0.0477(17) -0.0227(15) 0.0330(16) -0.0406(17) C48 0.0517(18) 0.0511(18) 0.063(2) -0.0295(16) 0.0343(16) -0.0281(16) C49 0.080(2) 0.089(3) 0.0443(18) -0.0386(18) 0.0363(17) -0.059(2) C50 0.0418(15) 0.0610(19) 0.0462(16) -0.0312(15) 0.0138(13) -0.0314(15) C51 0.067(2) 0.078(3) 0.075(2) -0.031(2) 0.0134(19) -0.052(2) C52 0.082(2) 0.141(3) 0.066(2) -0.059(2) 0.0249(18) -0.076(2) C53 0.048(2) 0.086(3) 0.082(3) -0.038(2) 0.0008(19) -0.027(2) C54 0.112(4) 0.058(3) 0.088(3) -0.035(2) -0.010(3) -0.022(3) C55 0.110(4) 0.052(2) 0.088(3) -0.029(2) -0.006(3) -0.021(2) C56 0.131(5) 0.078(4) 0.141(5) -0.050(4) 0.031(4) -0.030(3) C4A 0.050(4) 0.095(6) 0.068(5) -0.001(4) 0.021(4) -0.044(4) C5A 0.082(5) 0.111(6) 0.103(6) -0.033(4) 0.024(4) -0.050(4) C6A 0.085(5) 0.100(5) 0.093(6) -0.020(4) 0.030(4) -0.051(4) C34A 0.044(4) 0.070(4) 0.062(5) -0.009(3) 0.032(4) -0.025(3) C35A 0.135(9) 0.147(9) 0.135(9) -0.041(5) 0.042(5) -0.071(6) C36A 0.110(5) 0.112(5) 0.112(5) -0.043(2) 0.0217(14) -0.054(3) C38A 0.088(5) 0.100(5) 0.087(5) -0.034(4) 0.004(4) -0.056(4) C39A 0.081(5) 0.066(5) 0.088(5) -0.017(4) 0.007(4) -0.048(4) _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 O1 1.7798(19) . ? Ti1 O2 1.814(2) . ? Ti1 O3 1.832(2) . ? Ti1 O4 1.8624(19) . ? Ti1 N1 2.378(2) . ? O1 C4A 1.398(10) . ? O1 C4 1.433(8) . ? N1 C25 1.481(3) . ? N1 C27 1.491(3) . ? N1 C24 1.491(3) . ? C1 O2 1.434(4) . ? C1 C3 1.457(5) . ? C1 C2 1.469(5) . ? C1 H1 1.0000 . ? Ti2 O6 1.789(2) . ? Ti2 O5 1.808(2) . ? Ti2 O7 1.839(2) . ? Ti2 O8 1.8819(19) . ? Ti2 N2 2.354(2) . ? N2 C26 1.489(3) . ? N2 C30 1.494(3) . ? N2 C29 1.496(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C7 1.412(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C10 1.354(3) . ? C4 C5 1.452(5) . ? C4 C6 1.462(5) . ? C4 H4 1.0000 . ? O5 C31 1.419(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? O6 C34A 1.365(10) . ? O6 C34 1.459(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O7 C37 1.428(3) . ? C7 C8 1.484(7) . ? C7 C9 1.490(6) . ? C7 H7 1.0000 . ? O8 C40 1.359(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 C11 1.402(4) . ? C10 C15 1.406(4) . ? C11 C12 1.405(4) . ? C11 C16 1.536(4) . ? C12 C13 1.395(4) . ? C12 H12 0.9500 . ? C13 C14 1.386(4) . ? C13 C20 1.536(4) . ? C14 C15 1.391(4) . ? C14 H14 0.9500 . ? C15 C24 1.509(4) . ? C16 C19 1.531(4) . ? C16 C17 1.544(4) . ? C16 C18 1.548(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.522(5) . ? C20 C23 1.523(5) . ? C20 C22 1.541(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.538(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.530(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.527(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C41 1.497(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.481(5) . ? C31 C33 1.537(6) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.450(5) . ? C34 C35 1.480(5) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39A 1.449(5) . ? C37 C38 1.450(4) . ? C37 C38A 1.477(5) . ? C37 C39 1.488(4) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.399(3) . ? C40 C45 1.410(4) . ? C41 C42 1.386(4) . ? C42 C43 1.386(4) . ? C42 H42 0.9500 . ? C43 C44 1.386(4) . ? C43 C50 1.537(4) . ? C44 C45 1.400(4) . ? C44 H44 0.9500 . ? C45 C46 1.538(4) . ? C46 C48 1.525(4) . ? C46 C47 1.532(4) . ? C46 C49 1.530(4) . ? 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 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C52 1.502(5) . ? C50 C53 1.538(5) . ? C50 C51 1.541(5) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.504(7) . ? C54 C54 1.515(10) 2_666 ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.494(8) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C4A C5A 1.451(5) . ? C4A C6A 1.453(5) . ? C4A H4A 1.0000 . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C34A C36A 1.446(5) . ? C34A C35A 1.461(5) . ? C34A H34A 1.0000 . ? C35A H35D 0.9800 . ? C35A H35E 0.9800 . ? C35A H35F 0.9800 . ? C36A H36D 0.9800 . ? C36A H36E 0.9800 . ? C36A H36F 0.9800 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 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 O1 Ti1 O2 100.53(10) . . ? O1 Ti1 O3 98.27(10) . . ? O2 Ti1 O3 115.86(10) . . ? O1 Ti1 O4 96.11(9) . . ? O2 Ti1 O4 112.72(10) . . ? O3 Ti1 O4 125.32(10) . . ? O1 Ti1 N1 173.78(9) . . ? O2 Ti1 N1 85.56(8) . . ? O3 Ti1 N1 79.97(8) . . ? O4 Ti1 N1 80.26(7) . . ? C4A O1 C4 33.1(4) . . ? C4A O1 Ti1 167.6(5) . . ? C4 O1 Ti1 156.7(4) . . ? C25 N1 C27 111.30(19) . . ? C25 N1 C24 112.13(19) . . ? C27 N1 C24 110.49(19) . . ? C25 N1 Ti1 109.97(14) . . ? C27 N1 Ti1 106.48(14) . . ? C24 N1 Ti1 106.19(14) . . ? O2 C1 C3 111.0(4) . . ? O2 C1 C2 111.2(3) . . ? C3 C1 C2 115.4(4) . . ? O2 C1 H1 106.2 . . ? C3 C1 H1 106.2 . . ? C2 C1 H1 106.2 . . ? O6 Ti2 O5 100.03(10) . . ? O6 Ti2 O7 97.48(9) . . ? O5 Ti2 O7 112.96(10) . . ? O6 Ti2 O8 95.39(9) . . ? O5 Ti2 O8 115.56(9) . . ? O7 Ti2 O8 126.37(9) . . ? O6 Ti2 N2 175.12(9) . . ? O5 Ti2 N2 84.67(8) . . ? O7 Ti2 N2 81.76(8) . . ? O8 Ti2 N2 81.30(7) . . ? C1 O2 Ti1 130.3(2) . . ? C26 N2 C30 107.75(18) . . ? C26 N2 C29 112.57(19) . . ? C30 N2 C29 109.59(19) . . ? C26 N2 Ti2 110.98(14) . . ? C30 N2 Ti2 104.62(14) . . ? C29 N2 Ti2 110.97(14) . . ? 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 . . ? C7 O3 Ti1 137.9(2) . . ? 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 . . ? C10 O4 Ti1 144.59(16) . . ? O1 C4 C5 109.8(7) . . ? O1 C4 C6 110.3(6) . . ? C5 C4 C6 114.7(8) . . ? O1 C4 H4 107.2 . . ? C5 C4 H4 107.2 . . ? C6 C4 H4 107.2 . . ? C31 O5 Ti2 136.9(2) . . ? C34A O6 C34 28.1(5) . . ? C34A O6 Ti2 171.7(5) . . ? C34 O6 Ti2 150.9(4) . . ? C37 O7 Ti2 131.36(18) . . ? O3 C7 C8 109.6(3) . . ? O3 C7 C9 109.2(3) . . ? C8 C7 C9 114.6(5) . . ? O3 C7 H7 107.7 . . ? C8 C7 H7 107.7 . . ? C9 C7 H7 107.7 . . ? C40 O8 Ti2 142.97(16) . . ? 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 . . ? O4 C10 C11 120.1(2) . . ? O4 C10 C15 118.7(2) . . ? C11 C10 C15 121.2(2) . . ? C10 C11 C12 116.7(2) . . ? C10 C11 C16 121.7(2) . . ? C12 C11 C16 121.6(2) . . ? C13 C12 C11 123.7(3) . . ? C13 C12 H12 118.2 . . ? C11 C12 H12 118.2 . . ? C14 C13 C12 117.3(2) . . ? C14 C13 C20 123.1(3) . . ? C12 C13 C20 119.7(3) . . ? C13 C14 C15 121.9(2) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C14 C15 C10 119.1(2) . . ? C14 C15 C24 121.1(2) . . ? C10 C15 C24 119.8(2) . . ? C19 C16 C11 112.5(2) . . ? C19 C16 C17 107.6(2) . . ? C11 C16 C17 110.8(2) . . ? C19 C16 C18 107.5(2) . . ? C11 C16 C18 108.7(2) . . ? C17 C16 C18 109.7(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C23 109.0(3) . . ? C21 C20 C13 110.0(3) . . ? C23 C20 C13 112.5(3) . . ? C21 C20 C22 108.5(3) . . ? C23 C20 C22 107.9(3) . . ? C13 C20 C22 109.0(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 C15 112.9(2) . . ? N1 C24 H24A 109.0 . . ? C15 C24 H24A 109.0 . . ? N1 C24 H24B 109.0 . . ? C15 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? N1 C25 C26 116.7(2) . . ? N1 C25 H25A 108.1 . . ? C26 C25 H25A 108.1 . . ? N1 C25 H25B 108.1 . . ? C26 C25 H25B 108.1 . . ? H25A C25 H25B 107.3 . . ? N2 C26 C25 115.4(2) . . ? N2 C26 H26A 108.4 . . ? C25 C26 H26A 108.4 . . ? N2 C26 H26B 108.4 . . ? C25 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? N1 C27 C28 117.9(2) . . ? N1 C27 H27A 107.8 . . ? C28 C27 H27A 107.8 . . ? N1 C27 H27B 107.8 . . ? C28 C27 H27B 107.8 . . ? H27A C27 H27B 107.2 . . ? C29 C28 C27 114.4(2) . . ? C29 C28 H28A 108.7 . . ? C27 C28 H28A 108.7 . . ? C29 C28 H28B 108.7 . . ? C27 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? N2 C29 C28 116.1(2) . . ? N2 C29 H29A 108.3 . . ? C28 C29 H29A 108.3 . . ? N2 C29 H29B 108.3 . . ? C28 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? N2 C30 C41 114.5(2) . . ? N2 C30 H30A 108.6 . . ? C41 C30 H30A 108.6 . . ? N2 C30 H30B 108.6 . . ? C41 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? O5 C31 C32 109.0(3) . . ? O5 C31 C33 108.6(3) . . ? C32 C31 C33 111.1(4) . . ? O5 C31 H31 109.4 . . ? C32 C31 H31 109.4 . . ? C33 C31 H31 109.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C34 O6 109.3(7) . . ? C36 C34 C35 114.7(7) . . ? O6 C34 C35 109.5(6) . . ? C36 C34 H34 107.7 . . ? O6 C34 H34 107.7 . . ? C35 C34 H34 107.7 . . ? O7 C37 C39A 114.6(6) . . ? O7 C37 C38 113.9(4) . . ? C39A C37 C38 129.8(6) . . ? O7 C37 C38A 106.7(5) . . ? C39A C37 C38A 111.3(8) . . ? C38 C37 C38A 40.9(6) . . ? O7 C37 C39 108.4(3) . . ? C39A C37 C39 35.4(5) . . ? C38 C37 C39 114.8(5) . . ? C38A C37 C39 81.2(7) . . ? O7 C37 H37 106.4 . . ? C39A C37 H37 71.2 . . ? C38 C37 H37 106.4 . . ? C38A C37 H37 141.5 . . ? C39 C37 H37 106.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? O8 C40 C41 118.4(2) . . ? O8 C40 C45 121.7(2) . . ? C41 C40 C45 119.9(2) . . ? C42 C41 C40 120.2(2) . . ? C42 C41 C30 119.3(2) . . ? C40 C41 C30 120.5(2) . . ? C43 C42 C41 121.7(2) . . ? C43 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C44 C43 C42 117.0(2) . . ? C44 C43 C50 123.1(2) . . ? C42 C43 C50 119.9(2) . . ? C43 C44 C45 124.0(2) . . ? C43 C44 H44 118.0 . . ? C45 C44 H44 118.0 . . ? C44 C45 C40 117.0(2) . . ? C44 C45 C46 121.1(2) . . ? C40 C45 C46 121.8(2) . . ? C48 C46 C47 110.0(3) . . ? C48 C46 C49 108.3(3) . . ? C47 C46 C49 107.2(3) . . ? C48 C46 C45 109.6(2) . . ? C47 C46 C45 109.4(2) . . ? C49 C46 C45 112.2(2) . . ? 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 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 C50 C43 112.8(3) . . ? C52 C50 C53 110.5(3) . . ? C43 C50 C53 108.3(3) . . ? C52 C50 C51 108.4(3) . . ? C43 C50 C51 109.9(3) . . ? C53 C50 C51 106.9(3) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C54 114.8(5) . 2_666 ? C55 C54 H54A 108.6 . . ? C54 C54 H54A 108.6 2_666 . ? C55 C54 H54B 108.6 . . ? C54 C54 H54B 108.6 2_666 . ? H54A C54 H54B 107.6 . . ? C56 C55 C54 112.2(4) . . ? C56 C55 H55A 109.2 . . ? C54 C55 H55A 109.2 . . ? C56 C55 H55B 109.2 . . ? C54 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O1 C4A C5A 119.2(8) . . ? O1 C4A C6A 112.1(9) . . ? C5A C4A C6A 127.0(11) . . ? O1 C4A H4A 94.2 . . ? C5A C4A H4A 94.2 . . ? C6A C4A H4A 94.2 . . ? C4A C5A H5A1 109.5 . . ? C4A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C4A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? C4A C6A H6A1 109.5 . . ? C4A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C4A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? O6 C34A C36A 116.2(10) . . ? O6 C34A C35A 116.9(12) . . ? C36A C34A C35A 124.0(13) . . ? O6 C34A H34A 95.6 . . ? C36A C34A H34A 95.6 . . ? C35A C34A H34A 95.6 . . ? C34A C35A H35D 109.5 . . ? C34A C35A H35E 109.5 . . ? H35D C35A H35E 109.5 . . ? C34A C35A H35F 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? C34A C36A H36D 109.5 . . ? C34A C36A H36E 109.5 . . ? H36D C36A H36E 109.5 . . ? C34A C36A H36F 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 109.5 . . ? C37 C38A H38D 109.5 . . ? C37 C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C37 C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C37 C39A H39D 109.5 . . ? C37 C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C37 C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.680 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.096 #===END data_1H2 _database_code_depnum_ccdc_archive 'CCDC 800225' #TrackingRef '- cif-DT-ART-11-2010-001542' _audit_creation_method shelxl-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H30 N2 O2 ' _chemical_formula_sum 'C22 H30 N2 O2' _chemical_formula_weight 354.48 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' o o 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4960(3) _cell_length_b 12.8830(3) _cell_length_c 8.9960(3) _cell_angle_alpha 90 _cell_angle_beta 102.393(2) _cell_angle_gamma 90 _cell_volume 961.70(5) _cell_formula_units_z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11978 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 384 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type none _exptl_absorpt_correction_t_min ? _exptl_absorpt_correction_t_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17655 _diffrn_reflns_av_r_equivalents 0.0443 _diffrn_reflns_av_sigmai/neti 0.0276 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 27.53 _reflns_number_total 2199 _reflns_number_gt 1733 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'collect (nonius bv, 1997-2000)' _computing_cell_refinement 'hkl scalepack (otwinski & minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0718P)^2^+0.2546P] 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 2199 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 O1 O 0.35844(10) 0.17239(8) 0.68125(11) 0.0278(3) Uani 1 1 d . . . N1 N 0.37005(13) 0.06980(8) 0.94180(11) 0.0229(3) Uani 1 1 d . . . C1 C 0.19592(14) 0.15239(9) 0.64969(14) 0.0216(3) Uani 1 1 d . . . H1 H 0.396(2) 0.1472(17) 0.780(3) 0.061(6) Uiso 1 1 d . . . C2 C 0.11187(15) 0.16300(10) 0.49874(14) 0.0227(3) Uani 1 1 d . . . C3 C -0.05310(15) 0.14411(10) 0.46528(14) 0.0239(3) Uani 1 1 d . . . H3 H -0.1112 0.1523 0.3633 0.029 Uiso 1 1 calc R . . C4 C -0.13649(15) 0.11360(10) 0.57549(15) 0.0241(3) Uani 1 1 d . . . C5 C -0.04825(15) 0.10226(10) 0.72388(15) 0.0238(3) Uani 1 1 d . . . H5 H -0.1024 0.0805 0.8005 0.029 Uiso 1 1 calc R . . C6 C 0.11675(15) 0.12168(10) 0.76401(14) 0.0223(3) Uani 1 1 d . . . C7 C 0.19982(16) 0.19321(12) 0.37629(15) 0.0300(3) Uani 1 1 d . . . H7A H 0.1219 0.2029 0.2798 0.045 Uiso 1 1 calc R . . H7B H 0.2760 0.1382 0.3646 0.045 Uiso 1 1 calc R . . H7C H 0.2587 0.2581 0.4049 0.045 Uiso 1 1 calc R . . C8 C -0.31518(16) 0.09167(11) 0.53461(17) 0.0308(3) Uani 1 1 d . . . H8A H -0.3331 0.0204 0.4966 0.046 Uiso 1 1 calc R . . H8B H -0.3676 0.1403 0.4556 0.046 Uiso 1 1 calc R . . H8C H -0.3608 0.1001 0.6251 0.046 Uiso 1 1 calc R . . C9 C 0.20698(15) 0.11330(11) 0.92823(14) 0.0254(3) Uani 1 1 d . . . H9A H 0.2155 0.1831 0.9754 0.031 Uiso 1 1 calc R . . H9B H 0.1452 0.0686 0.9847 0.031 Uiso 1 1 calc R . . C10 C 0.46726(15) 0.08066(10) 1.09696(14) 0.0248(3) Uani 1 1 d . . . H10A H 0.4165 0.0414 1.1688 0.030 Uiso 1 1 calc R . . H10B H 0.4726 0.1547 1.1273 0.030 Uiso 1 1 calc R . . C11 C 0.63597(15) 0.03970(11) 1.10364(15) 0.0251(3) Uani 1 1 d . . . H11A H 0.6882 0.0809 1.0348 0.030 Uiso 1 1 calc R . . H11B H 0.7011 0.0470 1.2085 0.030 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 O1 0.0191(5) 0.0372(6) 0.0267(5) 0.0022(4) 0.0043(4) -0.0029(4) N1 0.0231(5) 0.0237(6) 0.0203(5) -0.0012(4) 0.0013(4) 0.0013(4) C1 0.0182(6) 0.0210(6) 0.0255(7) -0.0006(5) 0.0046(5) 0.0012(5) C2 0.0240(6) 0.0212(6) 0.0235(7) 0.0003(5) 0.0061(5) 0.0020(5) C3 0.0235(6) 0.0240(7) 0.0225(6) -0.0013(5) 0.0010(5) 0.0028(5) C4 0.0202(6) 0.0218(6) 0.0298(7) -0.0020(5) 0.0046(5) 0.0018(5) C5 0.0223(6) 0.0241(7) 0.0268(7) 0.0012(5) 0.0093(5) 0.0013(5) C6 0.0220(6) 0.0221(6) 0.0226(6) -0.0001(5) 0.0045(5) 0.0027(5) C7 0.0299(7) 0.0352(8) 0.0259(7) 0.0042(6) 0.0084(5) 0.0028(6) C8 0.0216(7) 0.0334(7) 0.0361(8) -0.0019(6) 0.0036(6) 0.0000(5) C9 0.0241(7) 0.0298(7) 0.0228(6) 0.0012(5) 0.0057(5) 0.0034(5) C10 0.0278(7) 0.0248(6) 0.0198(6) -0.0012(5) 0.0008(5) 0.0017(5) C11 0.0260(7) 0.0246(7) 0.0225(6) -0.0014(5) 0.0002(5) -0.0011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.3730(14) . ? O1 H1 0.93(2) . ? N1 C11 1.4665(17) 3_657 ? N1 C10 1.4681(15) . ? N1 C9 1.4750(16) . ? C1 C2 1.3987(18) . ? C1 C6 1.4013(18) . ? C2 C3 1.3903(17) . ? C2 C7 1.5089(18) . ? C3 C4 1.3931(19) . ? C3 H3 0.9500 . ? C4 C5 1.3913(18) . ? C4 C8 1.5100(17) . ? C5 C6 1.3931(17) . ? C5 H5 0.9500 . ? C6 C9 1.5152(17) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.5164(18) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N1 1.4665(17) 3_657 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? 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 C1 O1 H1 105.0(13) . . ? C11 N1 C10 109.60(10) 3_657 . ? C11 N1 C9 111.49(10) 3_657 . ? C10 N1 C9 111.67(10) . . ? O1 C1 C2 117.62(11) . . ? O1 C1 C6 121.40(11) . . ? C2 C1 C6 120.97(11) . . ? C3 C2 C1 118.30(11) . . ? C3 C2 C7 121.41(11) . . ? C1 C2 C7 120.29(11) . . ? C2 C3 C4 122.57(12) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C5 C4 C3 117.44(11) . . ? C5 C4 C8 121.37(12) . . ? C3 C4 C8 121.18(12) . . ? C4 C5 C6 122.33(12) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 118.38(11) . . ? C5 C6 C9 120.69(11) . . ? C1 C6 C9 120.90(11) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C6 112.18(10) . . ? N1 C9 H9A 109.2 . . ? C6 C9 H9A 109.2 . . ? N1 C9 H9B 109.2 . . ? C6 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? N1 C10 C11 109.79(10) . . ? N1 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? N1 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N1 C11 C10 110.34(11) 3_657 . ? N1 C11 H11A 109.6 3_657 . ? C10 C11 H11A 109.6 . . ? N1 C11 H11B 109.6 3_657 . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.234 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.045 #===END