# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Simon Aldridge' _publ_contact_author_address ; Department of Chemistry Cardiff University of Wales Main Building Park Place Cardiff CF10 3AT UNITED KINGDOM ; _publ_contact_author_email ALDRIDGES@CARDIFF.AC.UK _publ_section_title ; Influence of ligand backbone flexibility in group 4 metal complexes of tetradentate mixed tertiary amine / alkoxide ligands ; loop_ _publ_author_name 'S. Aldridge' 'Rebecca E. Baghurst' 'Joanne K. Day' 'Ian Fallis' 'M. Hursthouse' ; M.E.Light ; 'Bruno Stengel' 'Robert R. Strevens' # Attachment '_L1_2Ti2_OEt_2O.cif' data_s92_3 _database_code_depnum_ccdc_archive 'CCDC 286913' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H78 N4 O7 Ti2' _chemical_formula_weight 798.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 19.7850(10) _cell_length_b 11.7253(4) _cell_length_c 19.6134(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4550.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.397 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9149 _exptl_absorpt_correction_T_max 0.9804 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean '9.091 pixels mm^1^' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22572 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7502 _reflns_number_gt 5240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski and MInor, 1997)' _computing_data_reduction 'DENZO, COLLECT, MAXUS (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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. The OEt groups are disordered over 2 positions ( 70:30, 50:50) and were refined isotropically The crystal was refined as a racemic twin (40:60) ; _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^)+(0.0710P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.40(3) _refine_ls_number_reflns 7502 _refine_ls_number_parameters 471 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1410 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 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 0.13567(5) 0.14544(7) 0.19975(5) 0.0240(2) Uani 1 1 d . A . Ti2 Ti 0.11442(5) 0.36253(7) 0.06939(4) 0.0230(2) Uani 1 1 d . A . N1 N 0.1668(2) 0.3061(3) 0.2780(2) 0.0218(10) Uani 1 1 d . . . N2 N 0.2255(2) 0.0608(3) 0.1049(2) 0.0269(11) Uani 1 1 d . . . N3 N 0.1636(2) 0.2218(3) -0.0080(2) 0.0236(10) Uani 1 1 d . . . N4 N 0.2039(2) 0.4857(3) 0.1655(2) 0.0270(10) Uani 1 1 d . . . O1 O 0.06807(18) 0.1549(3) 0.26541(16) 0.0287(9) Uani 1 1 d . . . O2 O 0.21209(18) 0.0848(3) 0.24148(17) 0.0288(9) Uani 1 1 d . . . O3 O 0.09167(18) 0.0248(3) 0.16000(18) 0.0355(10) Uani 1 1 d D . . O4 O 0.04710(18) 0.3263(3) 0.00748(17) 0.0288(9) Uani 1 1 d . . . O5 O 0.17813(18) 0.4529(3) 0.02754(17) 0.0284(9) Uani 1 1 d . . . O6 O 0.05891(19) 0.4633(3) 0.11309(19) 0.0330(9) Uani 1 1 d D . . O7 O 0.13222(17) 0.2572(3) 0.1350(2) 0.0231(8) Uani 1 1 d . . . C1 C 0.0665(3) 0.2180(5) 0.3270(3) 0.0281(13) Uani 1 1 d . . . H1 H 0.0374 0.2868 0.3200 0.034 Uiso 1 1 calc R . . C2 C 0.1381(3) 0.2574(5) 0.3409(3) 0.0261(13) Uani 1 1 d . . . H2A H 0.1381 0.3156 0.3774 0.031 Uiso 1 1 calc R . . H2B H 0.1660 0.1921 0.3562 0.031 Uiso 1 1 calc R . . C3 C 0.0359(3) 0.1464(5) 0.3861(3) 0.0299(13) Uani 1 1 d . . . C4 C 0.0322(3) 0.2197(5) 0.4500(3) 0.0416(16) Uani 1 1 d . . . H4A H 0.0060 0.1798 0.4851 0.062 Uiso 1 1 calc R . . H4B H 0.0102 0.2924 0.4392 0.062 Uiso 1 1 calc R . . H4C H 0.0780 0.2341 0.4670 0.062 Uiso 1 1 calc R . . C5 C 0.0766(3) 0.0382(5) 0.4008(3) 0.0402(15) Uani 1 1 d . . . H5A H 0.0547 -0.0049 0.4375 0.060 Uiso 1 1 calc R . . H5B H 0.1225 0.0591 0.4149 0.060 Uiso 1 1 calc R . . H5C H 0.0788 -0.0088 0.3596 0.060 Uiso 1 1 calc R . . C6 C -0.0358(3) 0.1132(5) 0.3650(3) 0.0427(16) Uani 1 1 d . . . H6A H -0.0341 0.0685 0.3228 0.064 Uiso 1 1 calc R . . H6B H -0.0627 0.1822 0.3575 0.064 Uiso 1 1 calc R . . H6C H -0.0566 0.0674 0.4011 0.064 Uiso 1 1 calc R . . C7 C 0.2597(3) 0.0032(4) 0.2207(3) 0.0295(13) Uani 1 1 d . . . H7 H 0.3052 0.0404 0.2203 0.035 Uiso 1 1 calc R . . C8 C 0.2444(3) -0.0366(4) 0.1486(3) 0.0322(14) Uani 1 1 d . . . H8A H 0.2846 -0.0751 0.1294 0.039 Uiso 1 1 calc R . . H8B H 0.2068 -0.0924 0.1497 0.039 Uiso 1 1 calc R . . C9 C 0.2619(3) -0.0964(4) 0.2732(3) 0.0298(13) Uani 1 1 d . . . C10 C 0.2806(3) -0.0466(4) 0.3427(3) 0.0369(15) Uani 1 1 d . . . H10A H 0.2857 -0.1086 0.3758 0.055 Uiso 1 1 calc R . . H10B H 0.2448 0.0052 0.3580 0.055 Uiso 1 1 calc R . . H10C H 0.3233 -0.0046 0.3390 0.055 Uiso 1 1 calc R . . C11 C 0.1936(3) -0.1571(4) 0.2787(3) 0.0394(16) Uani 1 1 d . . . H11A H 0.1950 -0.2117 0.3165 0.059 Uiso 1 1 calc R . . H11B H 0.1841 -0.1976 0.2361 0.059 Uiso 1 1 calc R . . H11C H 0.1580 -0.1008 0.2872 0.059 Uiso 1 1 calc R . . C12 C 0.3169(3) -0.1823(5) 0.2519(3) 0.0391(15) Uani 1 1 d . . . H12A H 0.3603 -0.1426 0.2472 0.059 Uiso 1 1 calc R . . H12B H 0.3046 -0.2170 0.2081 0.059 Uiso 1 1 calc R . . H12C H 0.3209 -0.2419 0.2867 0.059 Uiso 1 1 calc R . . C15 C 0.1280(3) 0.4123(4) 0.2612(3) 0.0259(12) Uani 1 1 d . . . H15A H 0.1078 0.4408 0.3041 0.031 Uiso 1 1 calc R . . H15B H 0.0903 0.3903 0.2309 0.031 Uiso 1 1 calc R . . C16 C 0.1651(3) 0.5124(4) 0.2276(3) 0.0268(13) Uani 1 1 d . . . H16A H 0.1313 0.5716 0.2160 0.032 Uiso 1 1 calc R . . H16B H 0.1964 0.5458 0.2615 0.032 Uiso 1 1 calc R . . C17 C 0.2399(3) 0.3269(4) 0.2883(3) 0.0268(12) Uani 1 1 d . . . H17A H 0.2592 0.2625 0.3145 0.032 Uiso 1 1 calc R . . H17B H 0.2456 0.3969 0.3160 0.032 Uiso 1 1 calc R . . C18 C 0.2796(3) 0.3405(5) 0.2217(3) 0.0301(13) Uani 1 1 d . . . H18A H 0.3280 0.3276 0.2318 0.036 Uiso 1 1 calc R . . H18B H 0.2650 0.2795 0.1901 0.036 Uiso 1 1 calc R . . C19 C 0.2730(3) 0.4547(4) 0.1849(3) 0.0300(13) Uani 1 1 d . . . H19A H 0.2913 0.5153 0.2148 0.036 Uiso 1 1 calc R . . H19B H 0.3012 0.4524 0.1432 0.036 Uiso 1 1 calc R . . C20 C 0.1910(3) 0.0219(4) 0.0427(3) 0.0253(12) Uani 1 1 d . . . H20A H 0.1670 -0.0500 0.0535 0.030 Uiso 1 1 calc R . . H20B H 0.2259 0.0038 0.0082 0.030 Uiso 1 1 calc R . . C21 C 0.1405(3) 0.1038(4) 0.0107(3) 0.0264(13) Uani 1 1 d . . . H21A H 0.1229 0.0674 -0.0313 0.032 Uiso 1 1 calc R . . H21B H 0.1020 0.1115 0.0426 0.032 Uiso 1 1 calc R . . C22 C 0.2882(3) 0.1235(4) 0.0862(3) 0.0283(13) Uani 1 1 d . . . H22A H 0.3165 0.0733 0.0573 0.034 Uiso 1 1 calc R . . H22B H 0.3140 0.1396 0.1284 0.034 Uiso 1 1 calc R . . C23 C 0.2769(3) 0.2341(4) 0.0490(3) 0.0298(13) Uani 1 1 d . . . H23A H 0.3216 0.2679 0.0391 0.036 Uiso 1 1 calc R . . H23B H 0.2532 0.2868 0.0804 0.036 Uiso 1 1 calc R . . C24 C 0.2372(3) 0.2300(4) -0.0172(3) 0.0271(13) Uani 1 1 d . . . H24A H 0.2474 0.2996 -0.0439 0.033 Uiso 1 1 calc R . . H24B H 0.2527 0.1636 -0.0442 0.033 Uiso 1 1 calc R . . C25 C 0.0533(3) 0.2680(5) -0.0556(3) 0.0282(13) Uani 1 1 d . . . H25 H 0.0342 0.1895 -0.0500 0.034 Uiso 1 1 calc R . . C26 C 0.1281(3) 0.2574(4) -0.0709(3) 0.0266(13) Uani 1 1 d . . . H26A H 0.1354 0.2002 -0.1073 0.032 Uiso 1 1 calc R . . H26B H 0.1461 0.3315 -0.0868 0.032 Uiso 1 1 calc R . . C27 C 0.0127(3) 0.3300(5) -0.1121(3) 0.0300(13) Uani 1 1 d . . . C28 C 0.0181(3) 0.2619(5) -0.1791(3) 0.0451(17) Uani 1 1 d . . . H28A H 0.0039 0.1830 -0.1711 0.068 Uiso 1 1 calc R . . H28B H 0.0650 0.2629 -0.1951 0.068 Uiso 1 1 calc R . . H28C H -0.0112 0.2966 -0.2136 0.068 Uiso 1 1 calc R . . C29 C -0.0614(3) 0.3338(5) -0.0912(3) 0.0413(16) Uani 1 1 d . . . H29A H -0.0664 0.3809 -0.0502 0.062 Uiso 1 1 calc R . . H29B H -0.0773 0.2563 -0.0816 0.062 Uiso 1 1 calc R . . H29C H -0.0883 0.3667 -0.1283 0.062 Uiso 1 1 calc R . . C30 C 0.0380(3) 0.4514(5) -0.1232(3) 0.0440(16) Uani 1 1 d . . . H30A H 0.0077 0.4912 -0.1548 0.066 Uiso 1 1 calc R . . H30B H 0.0837 0.4492 -0.1424 0.066 Uiso 1 1 calc R . . H30C H 0.0388 0.4920 -0.0795 0.066 Uiso 1 1 calc R . . C31 C 0.2222(3) 0.5417(4) 0.0464(3) 0.0238(12) Uani 1 1 d . . . H31 H 0.2688 0.5084 0.0481 0.029 Uiso 1 1 calc R . . C32 C 0.2054(3) 0.5813(4) 0.1181(3) 0.0301(13) Uani 1 1 d . . . H32A H 0.2396 0.6374 0.1334 0.036 Uiso 1 1 calc R . . H32B H 0.1608 0.6195 0.1180 0.036 Uiso 1 1 calc R . . C33 C 0.2234(3) 0.6364(4) -0.0080(3) 0.0291(13) Uani 1 1 d . . . C34 C 0.2400(3) 0.5819(5) -0.0773(3) 0.0398(15) Uani 1 1 d . . . H34A H 0.2839 0.5432 -0.0746 0.060 Uiso 1 1 calc R . . H34B H 0.2419 0.6413 -0.1124 0.060 Uiso 1 1 calc R . . H34C H 0.2049 0.5264 -0.0891 0.060 Uiso 1 1 calc R . . C35 C 0.1540(3) 0.6934(5) -0.0133(3) 0.0406(15) Uani 1 1 d . . . H35A H 0.1190 0.6347 -0.0181 0.061 Uiso 1 1 calc R . . H35B H 0.1531 0.7438 -0.0532 0.061 Uiso 1 1 calc R . . H35C H 0.1454 0.7382 0.0280 0.061 Uiso 1 1 calc R . . C36 C 0.2782(3) 0.7248(4) 0.0086(3) 0.0342(14) Uani 1 1 d . . . H36A H 0.2655 0.7666 0.0500 0.051 Uiso 1 1 calc R . . H36B H 0.2826 0.7783 -0.0295 0.051 Uiso 1 1 calc R . . H36C H 0.3214 0.6859 0.0161 0.051 Uiso 1 1 calc R . . C13A C 0.0317(3) -0.0417(7) 0.1749(5) 0.046(2) Uiso 0.70 1 d PD A 1 H13A H 0.0214 -0.0413 0.2243 0.055 Uiso 0.70 1 calc PR A 1 H13B H 0.0368 -0.1215 0.1592 0.055 Uiso 0.70 1 calc PR A 1 C14A C -0.0232(4) 0.0215(8) 0.1339(5) 0.061(3) Uiso 0.70 1 d PD A 1 H14A H -0.0289 0.0987 0.1522 0.092 Uiso 0.70 1 calc PR A 1 H14B H -0.0660 -0.0200 0.1374 0.092 Uiso 0.70 1 calc PR A 1 H14C H -0.0095 0.0261 0.0859 0.092 Uiso 0.70 1 calc PR A 1 C13B C 0.0237(5) -0.0199(15) 0.1677(15) 0.046(2) Uiso 0.30 1 d PD A 2 H13C H -0.0083 0.0215 0.1379 0.055 Uiso 0.30 1 calc PR A 2 H13D H 0.0083 -0.0130 0.2156 0.055 Uiso 0.30 1 calc PR A 2 C14B C 0.0291(12) -0.1461(16) 0.1466(12) 0.061(3) Uiso 0.30 1 d PD A 2 H14D H 0.0485 -0.1512 0.1007 0.092 Uiso 0.30 1 calc PR A 2 H14E H -0.0160 -0.1806 0.1467 0.092 Uiso 0.30 1 calc PR A 2 H14F H 0.0583 -0.1867 0.1788 0.092 Uiso 0.30 1 calc PR A 2 C37A C -0.0114(4) 0.4951(14) 0.1219(13) 0.102(4) Uiso 0.48 1 d PD B 3 H37A H -0.0318 0.5115 0.0768 0.122 Uiso 0.48 1 calc PR B 3 H37B H -0.0143 0.5652 0.1499 0.122 Uiso 0.48 1 calc PR B 3 C38A C -0.0511(8) 0.3985(13) 0.1569(8) 0.067(3) Uiso 0.48 1 d PD B 3 H38A H -0.0411 0.3259 0.1344 0.101 Uiso 0.48 1 calc PR B 3 H38B H -0.0997 0.4142 0.1538 0.101 Uiso 0.48 1 calc PR B 3 H38C H -0.0379 0.3939 0.2050 0.101 Uiso 0.48 1 calc PR B 3 C37B C -0.0124(3) 0.4849(12) 0.1020(12) 0.102(4) Uiso 0.52 1 d PD B 4 H37C H -0.0394 0.4304 0.1293 0.122 Uiso 0.52 1 calc PR B 4 H37D H -0.0234 0.4729 0.0533 0.122 Uiso 0.52 1 calc PR B 4 C38B C -0.0308(7) 0.6076(11) 0.1226(8) 0.067(3) Uiso 0.52 1 d PD B 4 H38D H -0.0517 0.6072 0.1679 0.101 Uiso 0.52 1 calc PR B 4 H38E H -0.0627 0.6393 0.0894 0.101 Uiso 0.52 1 calc PR B 4 H38F H 0.0102 0.6544 0.1236 0.101 Uiso 0.52 1 calc PR B 4 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 0.0311(6) 0.0207(5) 0.0202(5) 0.0010(4) -0.0021(4) -0.0023(4) Ti2 0.0283(5) 0.0203(5) 0.0204(5) -0.0006(4) 0.0002(4) 0.0020(4) N1 0.025(3) 0.020(2) 0.020(2) 0.0017(17) -0.0020(19) 0.0011(19) N2 0.034(3) 0.022(2) 0.025(2) -0.0006(18) -0.004(2) 0.003(2) N3 0.027(3) 0.021(2) 0.023(3) 0.0031(18) -0.0015(19) -0.0039(19) N4 0.030(3) 0.022(2) 0.029(3) 0.0013(19) 0.002(2) 0.001(2) O1 0.033(2) 0.035(2) 0.018(2) 0.0000(16) -0.0015(16) -0.0062(18) O2 0.042(2) 0.0189(18) 0.025(2) -0.0002(15) -0.0041(17) 0.0058(17) O3 0.045(3) 0.031(2) 0.030(2) -0.0017(16) -0.0038(18) -0.0125(19) O4 0.028(2) 0.034(2) 0.025(2) -0.0039(16) -0.0018(15) 0.0050(17) O5 0.039(2) 0.0202(19) 0.026(2) 0.0001(14) 0.0018(17) -0.0032(16) O6 0.036(2) 0.036(2) 0.028(2) -0.0036(17) -0.0018(17) 0.0131(19) O7 0.027(2) 0.0252(18) 0.0173(15) -0.0016(12) 0.0023(15) -0.0015(16) C1 0.031(4) 0.031(3) 0.023(3) 0.002(2) 0.000(2) 0.008(3) C2 0.034(3) 0.029(3) 0.015(3) 0.003(2) -0.001(2) 0.006(3) C3 0.021(3) 0.039(3) 0.029(3) 0.002(3) 0.002(2) -0.003(3) C4 0.040(4) 0.061(4) 0.023(3) 0.008(3) 0.008(3) -0.006(3) C5 0.040(4) 0.043(4) 0.037(4) 0.010(3) 0.004(3) -0.004(3) C6 0.036(4) 0.062(4) 0.030(4) 0.009(3) 0.001(3) -0.017(3) C7 0.033(3) 0.027(3) 0.029(3) -0.004(2) -0.003(2) 0.008(3) C8 0.038(4) 0.021(3) 0.038(4) 0.001(2) 0.001(3) 0.009(3) C9 0.037(4) 0.025(3) 0.028(3) -0.001(2) -0.004(2) 0.003(3) C10 0.057(4) 0.022(3) 0.032(3) 0.004(2) -0.013(3) 0.008(3) C11 0.060(5) 0.023(3) 0.035(4) 0.004(2) -0.001(3) 0.008(3) C12 0.056(4) 0.028(3) 0.033(3) 0.001(2) -0.011(3) 0.012(3) C15 0.034(3) 0.020(3) 0.023(3) 0.001(2) 0.000(2) -0.002(2) C16 0.035(3) 0.021(3) 0.025(3) -0.004(2) -0.001(2) 0.002(2) C17 0.029(3) 0.029(3) 0.022(3) 0.000(2) -0.006(2) -0.001(2) C18 0.025(3) 0.043(3) 0.023(3) -0.004(2) -0.002(2) 0.004(3) C19 0.022(3) 0.035(3) 0.032(3) 0.002(2) 0.003(2) -0.008(2) C20 0.032(3) 0.015(3) 0.028(3) -0.005(2) 0.002(2) -0.005(2) C21 0.042(4) 0.021(3) 0.016(3) -0.003(2) -0.009(2) -0.001(2) C22 0.021(3) 0.037(3) 0.026(3) 0.001(2) 0.001(2) -0.002(2) C23 0.028(3) 0.033(3) 0.028(3) -0.003(2) 0.001(2) -0.003(2) C24 0.034(4) 0.025(3) 0.022(3) 0.002(2) 0.002(2) 0.004(2) C25 0.034(4) 0.028(3) 0.022(3) 0.000(2) -0.007(2) 0.000(3) C26 0.043(4) 0.019(3) 0.018(3) -0.001(2) -0.004(2) 0.005(2) C27 0.034(4) 0.035(3) 0.022(3) 0.004(2) -0.005(2) 0.002(3) C28 0.051(4) 0.056(4) 0.028(4) 0.001(3) -0.010(3) -0.004(3) C29 0.029(4) 0.058(4) 0.037(4) 0.006(3) -0.007(3) 0.002(3) C30 0.045(4) 0.039(4) 0.048(4) 0.019(3) -0.014(3) -0.002(3) C31 0.026(3) 0.019(3) 0.027(3) -0.001(2) -0.001(2) -0.006(2) C32 0.042(4) 0.021(3) 0.027(3) 0.000(2) 0.000(3) -0.001(3) C33 0.035(4) 0.025(3) 0.028(3) 0.000(2) 0.003(2) -0.004(3) C34 0.058(4) 0.032(4) 0.029(3) 0.000(2) 0.005(3) -0.009(3) C35 0.043(4) 0.035(3) 0.044(4) 0.013(3) 0.001(3) -0.001(3) C36 0.042(4) 0.027(3) 0.033(3) 0.004(2) 0.003(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 O7 1.826(4) . ? Ti1 O3 1.835(3) . ? Ti1 O1 1.860(4) . ? Ti1 O2 1.860(4) . ? Ti1 N1 2.506(4) . ? Ti2 O7 1.818(4) . ? Ti2 O6 1.827(4) . ? Ti2 O5 1.840(4) . ? Ti2 O4 1.852(3) . ? Ti2 N3 2.443(4) . ? N1 C2 1.474(6) . ? N1 C17 1.480(6) . ? N1 C15 1.499(6) . ? N2 C20 1.470(6) . ? N2 C8 1.477(6) . ? N2 C22 1.488(6) . ? N3 C24 1.472(6) . ? N3 C26 1.479(6) . ? N3 C21 1.502(6) . ? N4 C32 1.456(6) . ? N4 C19 1.463(6) . ? N4 C16 1.474(6) . ? O1 C1 1.418(6) . ? O2 C7 1.404(6) . ? O3 C13A 1.449(2) . ? O3 C13B 1.450(2) . ? O4 C25 1.419(6) . ? O5 C31 1.408(6) . ? O6 C37B 1.449(2) . ? O6 C37A 1.451(2) . ? C1 C2 1.516(8) . ? C1 C3 1.553(7) . ? C3 C4 1.522(8) . ? C3 C6 1.529(8) . ? C3 C5 1.531(8) . ? C7 C8 1.519(8) . ? C7 C9 1.556(7) . ? C9 C10 1.530(7) . ? C9 C11 1.531(8) . ? C9 C12 1.542(8) . ? C15 C16 1.533(7) . ? C17 C18 1.532(7) . ? C18 C19 1.528(7) . ? C20 C21 1.522(7) . ? C22 C23 1.505(7) . ? C23 C24 1.518(7) . ? C25 C26 1.515(7) . ? C25 C27 1.549(7) . ? C27 C29 1.523(8) . ? C27 C30 1.525(7) . ? C27 C28 1.541(8) . ? C31 C32 1.519(7) . ? C31 C33 1.541(7) . ? C33 C35 1.531(8) . ? C33 C36 1.535(7) . ? C33 C34 1.536(8) . ? C13A C14A 1.542(2) . ? C13B C14B 1.541(2) . ? C37A C38A 1.541(2) . ? C37B C38B 1.538(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Ti1 O3 103.87(16) . . ? O7 Ti1 O1 114.34(16) . . ? O3 Ti1 O1 89.93(16) . . ? O7 Ti1 O2 127.63(16) . . ? O3 Ti1 O2 106.15(16) . . ? O1 Ti1 O2 107.61(15) . . ? O7 Ti1 N1 84.01(15) . . ? O3 Ti1 N1 162.97(16) . . ? O1 Ti1 N1 73.04(14) . . ? O2 Ti1 N1 79.52(14) . . ? O7 Ti2 O6 102.94(17) . . ? O7 Ti2 O5 125.04(16) . . ? O6 Ti2 O5 104.41(16) . . ? O7 Ti2 O4 116.57(16) . . ? O6 Ti2 O4 91.36(16) . . ? O5 Ti2 O4 109.42(16) . . ? O7 Ti2 N3 84.45(15) . . ? O6 Ti2 N3 165.34(16) . . ? O5 Ti2 N3 80.75(14) . . ? O4 Ti2 N3 73.98(15) . . ? C2 N1 C17 109.0(4) . . ? C2 N1 C15 108.0(4) . . ? C17 N1 C15 113.1(4) . . ? C2 N1 Ti1 97.3(3) . . ? C17 N1 Ti1 116.6(3) . . ? C15 N1 Ti1 111.4(3) . . ? C20 N2 C8 111.0(4) . . ? C20 N2 C22 109.6(4) . . ? C8 N2 C22 108.3(4) . . ? C24 N3 C26 110.3(4) . . ? C24 N3 C21 113.0(4) . . ? C26 N3 C21 108.6(4) . . ? C24 N3 Ti2 115.3(3) . . ? C26 N3 Ti2 98.0(3) . . ? C21 N3 Ti2 110.5(3) . . ? C32 N4 C19 109.8(4) . . ? C32 N4 C16 111.9(4) . . ? C19 N4 C16 108.9(4) . . ? C1 O1 Ti1 129.6(3) . . ? C7 O2 Ti1 132.7(3) . . ? C13A O3 Ti1 135.8(5) . . ? C13B O3 Ti1 132.3(9) . . ? C25 O4 Ti2 128.4(3) . . ? C31 O5 Ti2 137.1(3) . . ? C37B O6 Ti2 128.9(7) . . ? C37A O6 Ti2 143.0(11) . . ? Ti2 O7 Ti1 170.7(2) . . ? O1 C1 C2 106.9(4) . . ? O1 C1 C3 111.3(4) . . ? C2 C1 C3 113.3(4) . . ? N1 C2 C1 109.2(4) . . ? C4 C3 C6 108.8(5) . . ? C4 C3 C5 109.7(5) . . ? C6 C3 C5 109.2(5) . . ? C4 C3 C1 109.2(4) . . ? C6 C3 C1 107.3(4) . . ? C5 C3 C1 112.6(4) . . ? O2 C7 C8 110.2(4) . . ? O2 C7 C9 109.7(4) . . ? C8 C7 C9 113.0(4) . . ? N2 C8 C7 110.7(4) . . ? C10 C9 C11 109.1(5) . . ? C10 C9 C12 108.6(5) . . ? C11 C9 C12 109.8(4) . . ? C10 C9 C7 108.1(4) . . ? C11 C9 C7 111.8(4) . . ? C12 C9 C7 109.3(4) . . ? N1 C15 C16 119.1(4) . . ? N4 C16 C15 116.3(4) . . ? N1 C17 C18 113.6(4) . . ? C19 C18 C17 116.8(5) . . ? N4 C19 C18 114.9(4) . . ? N2 C20 C21 116.8(4) . . ? N3 C21 C20 118.9(4) . . ? N2 C22 C23 114.8(4) . . ? C22 C23 C24 117.8(5) . . ? N3 C24 C23 114.0(4) . . ? O4 C25 C26 107.2(4) . . ? O4 C25 C27 110.6(4) . . ? C26 C25 C27 113.8(4) . . ? N3 C26 C25 108.8(4) . . ? C29 C27 C30 109.1(5) . . ? C29 C27 C28 108.1(5) . . ? C30 C27 C28 109.8(5) . . ? C29 C27 C25 108.7(4) . . ? C30 C27 C25 111.8(5) . . ? C28 C27 C25 109.3(4) . . ? O5 C31 C32 109.5(4) . . ? O5 C31 C33 111.1(4) . . ? C32 C31 C33 115.1(4) . . ? N4 C32 C31 111.0(4) . . ? C35 C33 C36 110.7(4) . . ? C35 C33 C34 108.3(5) . . ? C36 C33 C34 108.5(5) . . ? C35 C33 C31 110.4(4) . . ? C36 C33 C31 110.5(4) . . ? C34 C33 C31 108.4(4) . . ? O3 C13A C14A 102.3(6) . . ? O3 C13B C14B 104.7(13) . . ? O6 C37A C38A 110.7(10) . . ? O6 C37B C38B 110.8(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.618 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.069 # Attachment '_L2_2Zr.cif' data_c:\bono\solv\s92 _database_code_depnum_ccdc_archive 'CCDC 286914' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H68 N4 O4 Zr' _chemical_formula_weight 664.12 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' 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' Zr Zr -2.9673 0.5597 '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 10.762(2) _cell_length_b 12.115(2) _cell_length_c 15.963(3) _cell_angle_alpha 76.68(3) _cell_angle_beta 72.59(3) _cell_angle_gamma 68.58(3) _cell_volume 1831.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.337 _exptl_absorpt_correction_type Sortav _exptl_absorpt_correction_T_min 0.8956 _exptl_absorpt_correction_T_max 0.9356 _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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36431 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.45 _reflns_number_total 8322 _reflns_number_gt 7352 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0335P)^2^+1.5704P] 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 SHELXL _refine_ls_extinction_coef 0.0057(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8322 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Zr1 Zr 0.235125(19) 0.788660(15) 0.245899(12) 0.01666(7) Uani 1 1 d . B . O1 O 0.37624(14) 0.63958(12) 0.29519(9) 0.0228(3) Uani 1 1 d . B . O2 O 0.20090(15) 0.68223(12) 0.17737(9) 0.0249(3) Uani 1 1 d . B . O3 O 0.27439(14) 0.94839(11) 0.23016(9) 0.0211(3) Uani 1 1 d . B . O4 O 0.02929(14) 0.88501(12) 0.27232(10) 0.0242(3) Uani 1 1 d . . . N1 N 0.48146(18) 0.75247(15) 0.14076(11) 0.0245(4) Uani 1 1 d . . . N2 N 0.2298(2) 0.88623(15) 0.08191(12) 0.0281(4) Uani 1 1 d . . . N3 N 0.23097(17) 0.83814(14) 0.39668(11) 0.0210(3) Uani 1 1 d . . . N4 N 0.09467(18) 0.67980(15) 0.38044(12) 0.0259(4) Uani 1 1 d . . . C1 C 0.5164(2) 0.58593(19) 0.26050(14) 0.0267(4) Uani 1 1 d . . . H1 H 0.5680 0.6201 0.2848 0.032 Uiso 1 1 calc R B . C2 C 0.5464(2) 0.62221(19) 0.16042(14) 0.0283(5) Uani 1 1 d . B . H2A H 0.6469 0.6007 0.1355 0.034 Uiso 1 1 calc R . . H2B H 0.5096 0.5792 0.1330 0.034 Uiso 1 1 calc R . . C3 C 0.4807(3) 0.7868(2) 0.04597(14) 0.0333(5) Uani 1 1 d . B . H3A H 0.4705 0.7216 0.0236 0.040 Uiso 1 1 calc R . . H3B H 0.5691 0.7991 0.0118 0.040 Uiso 1 1 calc R . . C4 C 0.3640(3) 0.9004(2) 0.03295(14) 0.0333(5) Uani 1 1 d . B . H4A H 0.3765 0.9659 0.0535 0.040 Uiso 1 1 calc R . . H4B H 0.3658 0.9229 -0.0310 0.040 Uiso 1 1 calc R . . C5 C 0.1972(3) 0.8052(2) 0.04016(16) 0.0403(6) Uani 1 1 d . B . H5A H 0.2828 0.7567 0.0033 0.048 Uiso 1 1 calc R . . H5B H 0.1346 0.8536 0.0011 0.048 Uiso 1 1 calc R . . C6 C 0.1307(3) 0.7238(2) 0.10974(16) 0.0377(6) Uani 1 1 d . . . H6 H 0.0354 0.7740 0.1359 0.045 Uiso 1 1 calc R B . C7 C 0.5655(2) 0.4482(2) 0.28696(16) 0.0343(5) Uani 1 1 d . B . C8 C 0.5034(3) 0.3867(2) 0.24384(18) 0.0415(6) Uani 1 1 d . . . H8A H 0.5143 0.3046 0.2737 0.062 Uiso 1 1 calc R B . H8B H 0.5507 0.3852 0.1810 0.062 Uiso 1 1 calc R . . H8C H 0.4055 0.4311 0.2492 0.062 Uiso 1 1 calc R . . C9 C 0.5210(3) 0.4207(2) 0.38760(18) 0.0516(7) Uani 1 1 d . . . H9A H 0.5507 0.3339 0.4053 0.077 Uiso 1 1 calc R B . H9B H 0.4207 0.4530 0.4067 0.077 Uiso 1 1 calc R . . H9C H 0.5630 0.4577 0.4154 0.077 Uiso 1 1 calc R . . C10 C 0.7230(3) 0.4000(2) 0.2591(2) 0.0557(8) Uani 1 1 d . . . H10A H 0.7620 0.4405 0.2861 0.084 Uiso 1 1 calc R B . H10B H 0.7532 0.4150 0.1944 0.084 Uiso 1 1 calc R . . H10C H 0.7542 0.3137 0.2789 0.084 Uiso 1 1 calc R . . C11 C 0.5588(2) 0.8170(2) 0.16168(16) 0.0336(5) Uani 1 1 d . B . H11A H 0.6539 0.7930 0.1266 0.050 Uiso 1 1 calc R . . H11B H 0.5580 0.7973 0.2249 0.050 Uiso 1 1 calc R . . H11C H 0.5160 0.9034 0.1475 0.050 Uiso 1 1 calc R . . C12 C 0.1245(3) 1.0041(2) 0.07874(17) 0.0393(6) Uani 1 1 d . B . H12A H 0.1452 1.0572 0.1068 0.059 Uiso 1 1 calc R . . H12B H 0.0343 0.9960 0.1104 0.059 Uiso 1 1 calc R . . H12C H 0.1236 1.0381 0.0169 0.059 Uiso 1 1 calc R . . C13 C 0.1170(3) 0.6215(2) 0.07377(16) 0.0362(6) Uani 1 1 d . B . C14 C 0.0467(5) 0.6706(3) -0.0030(2) 0.0768(12) Uani 1 1 d . . . H14A H 0.1054 0.7057 -0.0533 0.115 Uiso 1 1 calc R B . H14B H -0.0415 0.7322 0.0156 0.115 Uiso 1 1 calc R . . H14C H 0.0308 0.6055 -0.0207 0.115 Uiso 1 1 calc R . . C15 C 0.2557(4) 0.5304(3) 0.0446(2) 0.0636(9) Uani 1 1 d . . . H15A H 0.2431 0.4594 0.0333 0.095 Uiso 1 1 calc R B . H15B H 0.3059 0.5076 0.0912 0.095 Uiso 1 1 calc R . . H15C H 0.3080 0.5651 -0.0099 0.095 Uiso 1 1 calc R . . C16 C 0.0304(4) 0.5565(3) 0.1490(2) 0.0642(9) Uani 1 1 d . . . H16A H 0.0147 0.4956 0.1261 0.096 Uiso 1 1 calc R B . H16B H -0.0580 0.6144 0.1728 0.096 Uiso 1 1 calc R . . H16C H 0.0794 0.5180 0.1963 0.096 Uiso 1 1 calc R . . C17 C 0.2721(2) 1.01147(18) 0.29414(13) 0.0230(4) Uani 1 1 d . . . H17 H 0.3684 0.9879 0.3005 0.028 Uiso 1 1 calc R B . C18 C 0.1863(2) 0.97022(17) 0.38270(13) 0.0225(4) Uani 1 1 d . B . H18A H 0.1992 0.9998 0.4314 0.027 Uiso 1 1 calc R . . H18B H 0.0877 1.0026 0.3822 0.027 Uiso 1 1 calc R . . C19 C 0.1359(2) 0.79406(19) 0.47361(13) 0.0279(5) Uani 1 1 d . B . H19A H 0.0420 0.8522 0.4792 0.034 Uiso 1 1 calc R . . H19B H 0.1651 0.7864 0.5285 0.034 Uiso 1 1 calc R . . C20 C 0.1350(2) 0.67390(19) 0.46232(13) 0.0270(4) Uani 1 1 d . B . H20A H 0.2277 0.6148 0.4606 0.032 Uiso 1 1 calc R . . H20B H 0.0700 0.6462 0.5139 0.032 Uiso 1 1 calc R . . C21 C -0.0529(2) 0.7483(2) 0.38707(17) 0.0391(6) Uani 1 1 d . B . H21A H -0.0885 0.7932 0.4384 0.047 Uiso 1 1 calc R A 1 H21B H -0.1049 0.6918 0.3975 0.047 Uiso 1 1 calc R A 1 C22 C -0.0763(3) 0.8352(3) 0.3039(2) 0.0268(7) Uani 0.719(4) 1 d P B 1 H22 H -0.0712 0.7886 0.2581 0.032 Uiso 0.719(4) 1 calc PR B 1 C23 C 0.2227(2) 1.14914(18) 0.26785(14) 0.0280(5) Uani 1 1 d . B . C24 C 0.2390(3) 1.2105(2) 0.33623(17) 0.0424(6) Uani 1 1 d . . . H24A H 0.3335 1.1763 0.3435 0.064 Uiso 1 1 calc R B . H24B H 0.1752 1.1978 0.3932 0.064 Uiso 1 1 calc R . . H24C H 0.2187 1.2965 0.3156 0.064 Uiso 1 1 calc R . . C25 C 0.0722(3) 1.1958(2) 0.26188(17) 0.0376(6) Uani 1 1 d . . . H25A H 0.0124 1.1937 0.3217 0.056 Uiso 1 1 calc R B . H25B H 0.0573 1.1453 0.2283 0.056 Uiso 1 1 calc R . . H25C H 0.0508 1.2784 0.2318 0.056 Uiso 1 1 calc R . . C26 C 0.3138(3) 1.1789(2) 0.17732(16) 0.0394(6) Uani 1 1 d . . . H26A H 0.2872 1.2659 0.1604 0.059 Uiso 1 1 calc R B . H26B H 0.3022 1.1419 0.1329 0.059 Uiso 1 1 calc R . . H26C H 0.4102 1.1479 0.1808 0.059 Uiso 1 1 calc R . . C27 C 0.3698(2) 0.78953(19) 0.41376(15) 0.0281(5) Uani 1 1 d . B . H27A H 0.3700 0.8225 0.4643 0.042 Uiso 1 1 calc R . . H27B H 0.4358 0.8117 0.3612 0.042 Uiso 1 1 calc R . . H27C H 0.3956 0.7021 0.4272 0.042 Uiso 1 1 calc R . . C28 C 0.1213(3) 0.5565(2) 0.36597(16) 0.0366(5) Uani 1 1 d . B . H28A H 0.2197 0.5126 0.3580 0.055 Uiso 1 1 calc R . . H28B H 0.0922 0.5586 0.3129 0.055 Uiso 1 1 calc R . . H28C H 0.0696 0.5164 0.4174 0.055 Uiso 1 1 calc R . . C29 C -0.2206(2) 0.9338(2) 0.31892(18) 0.0365(5) Uani 1 1 d . . . C30 C -0.2305(4) 1.0274(3) 0.3679(3) 0.0436(10) Uani 0.719(4) 1 d P B 1 H30A H -0.1546 1.0598 0.3392 0.065 Uiso 0.719(4) 1 calc PR B 1 H30B H -0.2254 0.9927 0.4291 0.065 Uiso 0.719(4) 1 calc PR B 1 H30C H -0.3182 1.0917 0.3678 0.065 Uiso 0.719(4) 1 calc PR B 1 C31 C -0.3326(4) 0.8764(4) 0.3605(3) 0.0543(12) Uani 0.719(4) 1 d P B 1 H31A H -0.4224 0.9371 0.3596 0.081 Uiso 0.719(4) 1 calc PR B 1 H31B H -0.3285 0.8420 0.4219 0.081 Uiso 0.719(4) 1 calc PR B 1 H31C H -0.3191 0.8130 0.3269 0.081 Uiso 0.719(4) 1 calc PR B 1 C32 C -0.2404(4) 0.9961(4) 0.2229(3) 0.0526(11) Uani 0.719(4) 1 d P B 1 H32A H -0.2290 0.9354 0.1875 0.079 Uiso 0.719(4) 1 calc PR B 1 H32B H -0.1717 1.0369 0.1943 0.079 Uiso 0.719(4) 1 calc PR B 1 H32C H -0.3327 1.0546 0.2275 0.079 Uiso 0.719(4) 1 calc PR B 1 C32A C -0.2392(10) 0.8947(8) 0.2524(6) 0.039(2) Uiso 0.281(4) 1 d P B 2 H32D H -0.3330 0.9365 0.2451 0.059 Uiso 0.281(4) 1 calc PR B 2 H32E H -0.2244 0.8084 0.2665 0.059 Uiso 0.281(4) 1 calc PR B 2 H32F H -0.1735 0.9108 0.1973 0.059 Uiso 0.281(4) 1 calc PR B 2 C30A C -0.2398(10) 1.0679(8) 0.3097(7) 0.039(2) Uiso 0.281(4) 1 d P B 2 H30D H -0.1710 1.0888 0.2585 0.058 Uiso 0.281(4) 1 calc PR B 2 H30E H -0.2286 1.0853 0.3635 0.058 Uiso 0.281(4) 1 calc PR B 2 H30F H -0.3321 1.1151 0.3012 0.058 Uiso 0.281(4) 1 calc PR B 2 C31A C -0.3339(10) 0.9099(9) 0.4153(7) 0.042(2) Uiso 0.281(4) 1 d P B 2 H31D H -0.4273 0.9591 0.4102 0.063 Uiso 0.281(4) 1 calc PR B 2 H31E H -0.3125 0.9316 0.4635 0.063 Uiso 0.281(4) 1 calc PR B 2 H31F H -0.3276 0.8252 0.4279 0.063 Uiso 0.281(4) 1 calc PR B 2 C22A C -0.0777(7) 0.8663(6) 0.3515(5) 0.0228(17) Uiso 0.281(4) 1 d P B 2 H22A H -0.0783 0.9108 0.3972 0.027 Uiso 0.281(4) 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 Zr1 0.01697(11) 0.01661(10) 0.01504(10) -0.00205(6) -0.00335(7) -0.00423(7) O1 0.0194(7) 0.0218(7) 0.0207(7) -0.0019(5) -0.0040(6) -0.0005(5) O2 0.0348(9) 0.0213(7) 0.0199(7) -0.0026(5) -0.0098(6) -0.0080(6) O3 0.0251(7) 0.0194(7) 0.0177(7) -0.0034(5) -0.0019(6) -0.0080(6) O4 0.0169(7) 0.0241(7) 0.0299(8) -0.0031(6) -0.0053(6) -0.0053(6) N1 0.0241(9) 0.0262(9) 0.0205(9) -0.0044(7) -0.0007(7) -0.0078(7) N2 0.0387(11) 0.0234(9) 0.0244(9) 0.0009(7) -0.0133(8) -0.0103(8) N3 0.0217(9) 0.0218(8) 0.0175(8) -0.0025(6) -0.0018(7) -0.0070(7) N4 0.0253(9) 0.0259(9) 0.0250(9) -0.0018(7) -0.0025(7) -0.0102(7) C1 0.0202(10) 0.0287(11) 0.0270(11) -0.0056(8) -0.0051(9) -0.0026(8) C2 0.0208(11) 0.0278(11) 0.0281(11) -0.0083(9) 0.0002(9) -0.0005(8) C3 0.0395(14) 0.0358(12) 0.0170(10) -0.0018(9) 0.0034(9) -0.0124(10) C4 0.0476(15) 0.0305(12) 0.0195(10) 0.0022(8) -0.0035(10) -0.0169(10) C5 0.0678(18) 0.0390(13) 0.0273(12) 0.0048(10) -0.0250(12) -0.0268(13) C6 0.0574(17) 0.0291(12) 0.0344(13) -0.0061(10) -0.0222(12) -0.0126(11) C7 0.0273(12) 0.0285(12) 0.0379(13) -0.0032(9) -0.0101(10) 0.0025(9) C8 0.0431(15) 0.0278(12) 0.0468(15) -0.0037(10) -0.0074(12) -0.0070(10) C9 0.0608(19) 0.0356(14) 0.0407(15) 0.0070(11) -0.0204(14) 0.0040(12) C10 0.0318(15) 0.0397(15) 0.080(2) -0.0078(14) -0.0177(15) 0.0095(11) C11 0.0255(12) 0.0384(13) 0.0364(13) -0.0079(10) 0.0020(10) -0.0154(10) C12 0.0474(15) 0.0322(12) 0.0352(13) 0.0042(10) -0.0212(12) -0.0055(11) C13 0.0579(16) 0.0268(11) 0.0325(12) -0.0079(9) -0.0202(12) -0.0134(11) C14 0.146(4) 0.0434(17) 0.078(2) 0.0005(15) -0.077(3) -0.037(2) C15 0.087(3) 0.0390(16) 0.063(2) -0.0271(14) -0.0242(18) 0.0000(15) C16 0.097(3) 0.0596(19) 0.059(2) -0.0124(15) -0.0214(19) -0.0456(19) C17 0.0235(11) 0.0242(10) 0.0217(10) -0.0055(8) -0.0025(8) -0.0090(8) C18 0.0266(11) 0.0215(10) 0.0192(10) -0.0053(7) -0.0031(8) -0.0078(8) C19 0.0342(12) 0.0280(11) 0.0175(10) -0.0027(8) 0.0005(9) -0.0108(9) C20 0.0316(12) 0.0269(11) 0.0185(10) 0.0006(8) -0.0003(9) -0.0113(9) C21 0.0237(12) 0.0486(15) 0.0387(14) 0.0032(11) -0.0019(10) -0.0142(11) C22 0.0202(15) 0.0333(16) 0.0283(16) -0.0091(13) -0.0035(12) -0.0089(12) C23 0.0332(12) 0.0208(10) 0.0265(11) -0.0045(8) 0.0010(9) -0.0104(9) C24 0.0570(17) 0.0305(12) 0.0418(14) -0.0119(10) -0.0003(12) -0.0213(12) C25 0.0404(14) 0.0238(11) 0.0372(13) 0.0008(9) -0.0065(11) -0.0024(10) C26 0.0485(15) 0.0274(12) 0.0356(13) -0.0025(10) 0.0062(11) -0.0186(11) C27 0.0303(12) 0.0288(11) 0.0263(11) -0.0048(8) -0.0112(9) -0.0065(9) C28 0.0494(15) 0.0340(12) 0.0316(12) -0.0025(10) -0.0017(11) -0.0268(11) C29 0.0190(11) 0.0403(13) 0.0503(15) -0.0131(11) -0.0085(10) -0.0052(9) C30 0.0287(19) 0.045(2) 0.056(3) -0.0275(19) -0.0077(17) -0.0002(15) C31 0.0222(19) 0.072(3) 0.069(3) -0.011(2) -0.0079(18) -0.0170(18) C32 0.033(2) 0.073(3) 0.044(2) -0.008(2) -0.0164(18) -0.0024(19) _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 Zr1 O4 2.0559(16) . ? Zr1 O2 2.0574(14) . ? Zr1 O1 2.0602(15) . ? Zr1 O3 2.0727(14) . ? Zr1 N3 2.5953(17) . ? Zr1 N4 2.616(2) . ? Zr1 N1 2.620(2) . ? Zr1 N2 2.6207(19) . ? O1 C1 1.398(3) . ? O2 C6 1.397(3) . ? O3 C17 1.399(2) . ? O4 C22 1.388(3) . ? O4 C22A 1.470(8) . ? N1 C2 1.475(3) . ? N1 C11 1.476(3) . ? N1 C3 1.476(3) . ? N2 C12 1.465(3) . ? N2 C4 1.474(3) . ? N2 C5 1.491(3) . ? N3 C27 1.476(3) . ? N3 C18 1.476(2) . ? N3 C19 1.478(3) . ? N4 C28 1.474(3) . ? N4 C20 1.475(3) . ? N4 C21 1.483(3) . ? C1 C2 1.524(3) . ? C1 C7 1.551(3) . ? C3 C4 1.509(3) . ? C5 C6 1.501(3) . ? C6 C13 1.549(3) . ? C7 C9 1.527(4) . ? C7 C8 1.534(4) . ? C7 C10 1.535(4) . ? C13 C15 1.510(4) . ? C13 C14 1.523(4) . ? C13 C16 1.537(4) . ? C17 C18 1.527(3) . ? C17 C23 1.551(3) . ? C19 C20 1.511(3) . ? C21 C22A 1.369(7) . ? C21 C22 1.516(4) . ? C22 C29 1.566(4) . ? C23 C25 1.533(3) . ? C23 C26 1.533(3) . ? C23 C24 1.536(3) . ? C29 C32A 1.348(9) . ? C29 C30 1.476(4) . ? C29 C31 1.515(4) . ? C29 C30A 1.539(9) . ? C29 C32 1.584(5) . ? C29 C22A 1.634(8) . ? C29 C31A 1.693(10) . ? 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 Zr1 O2 90.08(6) . . ? O4 Zr1 O1 141.74(6) . . ? O2 Zr1 O1 88.99(6) . . ? O4 Zr1 O3 87.69(6) . . ? O2 Zr1 O3 141.97(6) . . ? O1 Zr1 O3 115.17(6) . . ? O4 Zr1 N3 85.54(6) . . ? O2 Zr1 N3 148.77(6) . . ? O1 Zr1 N3 75.98(6) . . ? O3 Zr1 N3 68.82(6) . . ? O4 Zr1 N4 68.49(6) . . ? O2 Zr1 N4 82.00(6) . . ? O1 Zr1 N4 73.52(6) . . ? O3 Zr1 N4 131.36(6) . . ? N3 Zr1 N4 67.62(6) . . ? O4 Zr1 N1 149.78(6) . . ? O2 Zr1 N1 88.28(6) . . ? O1 Zr1 N1 68.41(6) . . ? O3 Zr1 N1 75.44(6) . . ? N3 Zr1 N1 110.46(6) . . ? N4 Zr1 N1 140.81(6) . . ? O4 Zr1 N2 84.02(7) . . ? O2 Zr1 N2 68.05(6) . . ? O1 Zr1 N2 130.24(6) . . ? O3 Zr1 N2 73.97(6) . . ? N3 Zr1 N2 141.65(5) . . ? N4 Zr1 N2 139.22(6) . . ? N1 Zr1 N2 67.43(6) . . ? C1 O1 Zr1 131.01(12) . . ? C6 O2 Zr1 125.24(13) . . ? C17 O3 Zr1 129.74(12) . . ? C22 O4 C22A 37.2(3) . . ? C22 O4 Zr1 124.79(15) . . ? C22A O4 Zr1 127.6(3) . . ? C2 N1 C11 109.98(17) . . ? C2 N1 C3 110.53(17) . . ? C11 N1 C3 108.21(18) . . ? C2 N1 Zr1 102.78(12) . . ? C11 N1 Zr1 111.85(13) . . ? C3 N1 Zr1 113.41(14) . . ? C12 N2 C4 108.52(18) . . ? C12 N2 C5 109.40(19) . . ? C4 N2 C5 109.94(19) . . ? C12 N2 Zr1 111.07(14) . . ? C4 N2 Zr1 110.48(13) . . ? C5 N2 Zr1 107.43(12) . . ? C27 N3 C18 110.21(16) . . ? C27 N3 C19 108.29(16) . . ? C18 N3 C19 110.64(16) . . ? C27 N3 Zr1 110.73(12) . . ? C18 N3 Zr1 102.44(11) . . ? C19 N3 Zr1 114.43(12) . . ? C28 N4 C20 108.20(17) . . ? C28 N4 C21 109.45(19) . . ? C20 N4 C21 111.35(18) . . ? C28 N4 Zr1 110.44(13) . . ? C20 N4 Zr1 110.18(12) . . ? C21 N4 Zr1 107.23(13) . . ? O1 C1 C2 108.04(17) . . ? O1 C1 C7 113.24(18) . . ? C2 C1 C7 112.50(18) . . ? N1 C2 C1 109.08(17) . . ? N1 C3 C4 110.28(18) . . ? N2 C4 C3 111.68(18) . . ? N2 C5 C6 110.61(19) . . ? O2 C6 C5 108.3(2) . . ? O2 C6 C13 112.86(18) . . ? C5 C6 C13 114.2(2) . . ? C9 C7 C8 109.2(2) . . ? C9 C7 C10 108.4(2) . . ? C8 C7 C10 109.9(2) . . ? C9 C7 C1 108.53(19) . . ? C8 C7 C1 111.22(18) . . ? C10 C7 C1 109.5(2) . . ? C15 C13 C14 109.8(3) . . ? C15 C13 C16 107.3(2) . . ? C14 C13 C16 109.0(3) . . ? C15 C13 C6 111.1(2) . . ? C14 C13 C6 110.9(2) . . ? C16 C13 C6 108.5(2) . . ? O3 C17 C18 108.29(16) . . ? O3 C17 C23 113.20(16) . . ? C18 C17 C23 112.84(17) . . ? N3 C18 C17 108.58(16) . . ? N3 C19 C20 110.27(17) . . ? N4 C20 C19 111.83(17) . . ? C22A C21 N4 114.1(4) . . ? C22A C21 C22 36.6(3) . . ? N4 C21 C22 112.0(2) . . ? O4 C22 C21 108.8(2) . . ? O4 C22 C29 111.7(2) . . ? C21 C22 C29 112.7(2) . . ? C25 C23 C26 109.4(2) . . ? C25 C23 C24 109.3(2) . . ? C26 C23 C24 108.85(19) . . ? C25 C23 C17 111.61(18) . . ? C26 C23 C17 107.89(18) . . ? C24 C23 C17 109.70(18) . . ? C32A C29 C30 153.7(5) . . ? C32A C29 C31 74.0(5) . . ? C30 C29 C31 112.8(3) . . ? C32A C29 C30A 117.6(6) . . ? C30 C29 C30A 37.1(4) . . ? C31 C29 C30A 125.6(4) . . ? C32A C29 C22 85.4(4) . . ? C30 C29 C22 113.6(2) . . ? C31 C29 C22 110.2(3) . . ? C30A C29 C22 123.1(4) . . ? C32A C29 C32 47.8(4) . . ? C30 C29 C32 107.5(3) . . ? C31 C29 C32 106.8(3) . . ? C30A C29 C32 70.4(4) . . ? C22 C29 C32 105.4(2) . . ? C32A C29 C22A 118.6(5) . . ? C30 C29 C22A 82.5(3) . . ? C31 C29 C22A 115.4(3) . . ? C30A C29 C22A 104.4(5) . . ? C22 C29 C22A 33.2(3) . . ? C32 C29 C22A 128.5(3) . . ? C32A C29 C31A 111.1(6) . . ? C30 C29 C31A 77.8(4) . . ? C31 C29 C31A 37.3(4) . . ? C30A C29 C31A 103.3(5) . . ? C22 C29 C31A 115.9(4) . . ? C32 C29 C31A 132.1(4) . . ? C22A C29 C31A 99.3(5) . . ? C21 C22A O4 112.6(5) . . ? C21 C22A C29 117.0(5) . . ? O4 C22A C29 103.9(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.117 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.085 # Attachment 'L1Ti2_OiPr_6.cif' data_s92 _database_code_depnum_ccdc_archive 'CCDC 286915' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H76 N2 O8 Ti2' _chemical_formula_weight 748.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0190(5) _cell_length_b 14.3144(6) _cell_length_c 15.7604(8) _cell_angle_alpha 70.240(3) _cell_angle_beta 88.145(2) _cell_angle_gamma 71.787(2) _cell_volume 2214.83(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9236 _exptl_absorpt_correction_T_max 0.9419 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _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 'Bruker Nonius kappa CCD area detector' _diffrn_measurement_method 'phi & omega scan to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31559 _diffrn_reflns_av_R_equivalents 0.1319 _diffrn_reflns_av_sigmaI/netI 0.1503 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.39 _reflns_number_total 8020 _reflns_number_gt 4406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0662P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'calculated positions, riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8020 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1451 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1758 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 0.28057(7) 0.25664(6) 0.21396(5) 0.0357(2) Uani 1 1 d . . . Ti2 Ti 0.04472(7) 0.24403(7) 0.63038(5) 0.0383(3) Uani 1 1 d . . . O1 O 0.1414(3) 0.3251(2) 0.12839(18) 0.0404(8) Uani 1 1 d . . . O2 O 0.3924(3) 0.2183(2) 0.13792(19) 0.0452(8) Uani 1 1 d . . . O3 O 0.3576(3) 0.3334(2) 0.2510(2) 0.0442(8) Uani 1 1 d . . . O4 O 0.2905(3) 0.1290(2) 0.2961(2) 0.0461(8) Uani 1 1 d . . . O5 O 0.1252(3) 0.3184(2) 0.67147(19) 0.0413(8) Uani 1 1 d . . . O6 O -0.0359(3) 0.2060(3) 0.7306(2) 0.0504(9) Uani 1 1 d . . . O7 O -0.0935(3) 0.3162(3) 0.5466(2) 0.0489(9) Uani 1 1 d . . . O8 O 0.1389(3) 0.1150(2) 0.6291(2) 0.0476(8) Uani 1 1 d . . . N1 N 0.1064(3) 0.3117(3) 0.2980(2) 0.0326(8) Uani 1 1 d . . . N2 N 0.1724(3) 0.3038(3) 0.5115(2) 0.0341(8) Uani 1 1 d . . . C1 C 0.0752(4) 0.4246(3) 0.2885(3) 0.0398(11) Uani 1 1 d . . . H1A H -0.0182 0.4530 0.2928 0.048 Uiso 1 1 calc R . . H1B H 0.0937 0.4629 0.2270 0.048 Uiso 1 1 calc R . . C2 C 0.1063(4) 0.4147(3) 0.4523(3) 0.0394(11) Uani 1 1 d . . . H2A H 0.1216 0.4613 0.4820 0.047 Uiso 1 1 calc R . . H2B H 0.0129 0.4260 0.4496 0.047 Uiso 1 1 calc R . . C3 C 0.1442(5) 0.4492(4) 0.3560(3) 0.0464(12) Uani 1 1 d . . . H3A H 0.1280 0.5258 0.3348 0.056 Uiso 1 1 calc R . . H3B H 0.2375 0.4152 0.3563 0.056 Uiso 1 1 calc R . . C4 C 0.2168(4) 0.2343(3) 0.4561(3) 0.0359(11) Uani 1 1 d . . . H4A H 0.2530 0.1607 0.4971 0.043 Uiso 1 1 calc R . . H4B H 0.2858 0.2536 0.4196 0.043 Uiso 1 1 calc R . . C5 C 0.1092(4) 0.2428(3) 0.3936(3) 0.0365(11) Uani 1 1 d . . . H5A H 0.1170 0.1717 0.3944 0.044 Uiso 1 1 calc R . . H5B H 0.0265 0.2699 0.4175 0.044 Uiso 1 1 calc R . . C6 C 0.0100(4) 0.3530(4) 0.1453(3) 0.0365(11) Uani 1 1 d . . . H6 H -0.0227 0.4307 0.1303 0.044 Uiso 1 1 calc R . . C7 C 0.0025(4) 0.3023(4) 0.2464(3) 0.0393(11) Uani 1 1 d . . . H7A H -0.0819 0.3372 0.2640 0.047 Uiso 1 1 calc R . . H7B H 0.0116 0.2275 0.2608 0.047 Uiso 1 1 calc R . . C8 C -0.0705(4) 0.3250(4) 0.0847(3) 0.0448(12) Uani 1 1 d . . . C9 C -0.0215(6) 0.2074(4) 0.1000(4) 0.0667(16) Uani 1 1 d . . . H9A H -0.0315 0.1679 0.1626 0.100 Uiso 1 1 calc R . . H9B H 0.0693 0.1868 0.0885 0.100 Uiso 1 1 calc R . . H9C H -0.0709 0.1923 0.0586 0.100 Uiso 1 1 calc R . . C10 C -0.0577(5) 0.3861(4) -0.0153(3) 0.0577(14) Uani 1 1 d . . . H10A H -0.1052 0.3675 -0.0551 0.087 Uiso 1 1 calc R . . H10B H 0.0330 0.3680 -0.0274 0.087 Uiso 1 1 calc R . . H10C H -0.0927 0.4616 -0.0267 0.087 Uiso 1 1 calc R . . C11 C -0.2100(5) 0.3580(5) 0.1050(4) 0.0700(17) Uani 1 1 d . . . H11A H -0.2622 0.3446 0.0640 0.105 Uiso 1 1 calc R . . H11B H -0.2394 0.4329 0.0964 0.105 Uiso 1 1 calc R . . H11C H -0.2185 0.3177 0.1677 0.105 Uiso 1 1 calc R . . C12 C 0.4099(5) 0.2144(4) 0.0485(3) 0.0545(14) Uani 1 1 d . . . H12 H 0.3324 0.2656 0.0082 0.065 Uiso 1 1 calc R . . C13 C 0.4175(10) 0.1065(6) 0.0527(5) 0.145(4) Uani 1 1 d . . . H13A H 0.4905 0.0548 0.0944 0.217 Uiso 1 1 calc R . . H13B H 0.4287 0.1015 -0.0077 0.217 Uiso 1 1 calc R . . H13C H 0.3382 0.0927 0.0741 0.217 Uiso 1 1 calc R . . C14 C 0.5229(6) 0.2460(7) 0.0139(4) 0.102(3) Uani 1 1 d . . . H14A H 0.5097 0.3176 0.0123 0.153 Uiso 1 1 calc R . . H14B H 0.5341 0.2434 -0.0473 0.153 Uiso 1 1 calc R . . H14C H 0.5996 0.1981 0.0538 0.153 Uiso 1 1 calc R . . C15 C 0.4657(4) 0.3677(4) 0.2237(3) 0.0525(14) Uani 1 1 d . . . H15 H 0.5235 0.3197 0.1950 0.063 Uiso 1 1 calc R . . C16 C 0.4212(7) 0.4763(6) 0.1555(6) 0.132(3) Uani 1 1 d . . . H16A H 0.3834 0.4752 0.1005 0.198 Uiso 1 1 calc R . . H16B H 0.4943 0.5025 0.1407 0.198 Uiso 1 1 calc R . . H16C H 0.3567 0.5224 0.1805 0.198 Uiso 1 1 calc R . . C17 C 0.5367(6) 0.3621(7) 0.3047(5) 0.115(3) Uani 1 1 d . . . H17A H 0.4815 0.4101 0.3326 0.173 Uiso 1 1 calc R . . H17B H 0.6134 0.3822 0.2867 0.173 Uiso 1 1 calc R . . H17C H 0.5619 0.2904 0.3483 0.173 Uiso 1 1 calc R . . C18 C 0.3585(4) 0.0228(4) 0.3094(3) 0.0444(12) Uani 1 1 d . . . H18 H 0.4314 0.0196 0.2699 0.053 Uiso 1 1 calc R . . C19 C 0.2693(5) -0.0255(4) 0.2821(4) 0.0678(16) Uani 1 1 d . . . H19A H 0.1960 -0.0206 0.3191 0.102 Uiso 1 1 calc R . . H19B H 0.3153 -0.0993 0.2913 0.102 Uiso 1 1 calc R . . H19C H 0.2388 0.0121 0.2181 0.102 Uiso 1 1 calc R . . C20 C 0.4113(5) -0.0324(4) 0.4064(3) 0.0614(14) Uani 1 1 d . . . H20A H 0.4707 0.0000 0.4203 0.092 Uiso 1 1 calc R . . H20B H 0.4570 -0.1065 0.4163 0.092 Uiso 1 1 calc R . . H20C H 0.3409 -0.0269 0.4459 0.092 Uiso 1 1 calc R . . C21 C 0.2372(4) 0.3434(4) 0.6409(3) 0.0386(11) Uani 1 1 d . . . H21 H 0.2131 0.4213 0.6125 0.046 Uiso 1 1 calc R . . C22 C 0.2839(4) 0.2955(4) 0.5671(3) 0.0391(11) Uani 1 1 d . . . H22A H 0.3383 0.3330 0.5281 0.047 Uiso 1 1 calc R . . H22B H 0.3361 0.2210 0.5956 0.047 Uiso 1 1 calc R . . C23 C 0.3369(4) 0.3075(4) 0.7211(3) 0.0465(12) Uani 1 1 d . . . C24 C 0.4605(4) 0.3305(4) 0.6860(4) 0.0624(15) Uani 1 1 d . . . H24A H 0.5209 0.3135 0.7374 0.094 Uiso 1 1 calc R . . H24B H 0.4397 0.4049 0.6492 0.094 Uiso 1 1 calc R . . H24C H 0.4993 0.2877 0.6490 0.094 Uiso 1 1 calc R . . C25 C 0.3672(5) 0.1914(4) 0.7758(3) 0.0584(14) Uani 1 1 d . . . H25A H 0.4278 0.1722 0.8277 0.088 Uiso 1 1 calc R . . H25B H 0.4053 0.1500 0.7375 0.088 Uiso 1 1 calc R . . H25C H 0.2880 0.1774 0.7972 0.088 Uiso 1 1 calc R . . C26 C 0.2800(5) 0.3723(4) 0.7822(3) 0.0598(15) Uani 1 1 d . . . H26A H 0.1997 0.3602 0.8032 0.090 Uiso 1 1 calc R . . H26B H 0.2631 0.4470 0.7477 0.090 Uiso 1 1 calc R . . H26C H 0.3411 0.3509 0.8344 0.090 Uiso 1 1 calc R . . C27 C -0.0489(5) 0.2035(5) 0.8209(3) 0.0556(14) Uani 1 1 d . . . H27 H -0.0128 0.2563 0.8289 0.067 Uiso 1 1 calc R . . C28 C 0.0283(8) 0.0978(6) 0.8837(4) 0.113(3) Uani 1 1 d . . . H28A H -0.0220 0.0498 0.8947 0.169 Uiso 1 1 calc R . . H28B H 0.0506 0.1032 0.9412 0.169 Uiso 1 1 calc R . . H28C H 0.1069 0.0709 0.8566 0.169 Uiso 1 1 calc R . . C29 C -0.1872(5) 0.2346(6) 0.8369(4) 0.087(2) Uani 1 1 d . . . H29A H -0.2308 0.3059 0.7956 0.131 Uiso 1 1 calc R . . H29B H -0.1963 0.2323 0.8996 0.131 Uiso 1 1 calc R . . H29C H -0.2257 0.1861 0.8260 0.131 Uiso 1 1 calc R . . C30 C -0.2182(5) 0.3077(5) 0.5457(5) 0.0764(19) Uani 1 1 d . . . H30 H -0.2289 0.2728 0.6108 0.092 Uiso 1 1 calc R . . C31 C -0.3142(5) 0.4070(5) 0.5215(6) 0.112(3) Uani 1 1 d . . . H31A H -0.3080 0.4405 0.5653 0.168 Uiso 1 1 calc R . . H31B H -0.3989 0.3981 0.5212 0.168 Uiso 1 1 calc R . . H31C H -0.3023 0.4510 0.4610 0.168 Uiso 1 1 calc R . . C32 C -0.2238(6) 0.2329(5) 0.5035(4) 0.0795(19) Uani 1 1 d . . . H32A H -0.2025 0.2567 0.4406 0.119 Uiso 1 1 calc R . . H32B H -0.3104 0.2276 0.5050 0.119 Uiso 1 1 calc R . . H32C H -0.1621 0.1641 0.5366 0.119 Uiso 1 1 calc R . . C33 C 0.1459(5) 0.0094(4) 0.6795(3) 0.0474(12) Uani 1 1 d . . . H33 H 0.0808 0.0093 0.7252 0.057 Uiso 1 1 calc R . . C34 C 0.1161(6) -0.0394(4) 0.6140(4) 0.0710(17) Uani 1 1 d . . . H34A H 0.0285 -0.0011 0.5859 0.106 Uiso 1 1 calc R . . H34B H 0.1238 -0.1129 0.6469 0.106 Uiso 1 1 calc R . . H34C H 0.1767 -0.0356 0.5670 0.106 Uiso 1 1 calc R . . C35 C 0.2763(6) -0.0486(5) 0.7269(5) 0.093(2) Uani 1 1 d . . . H35A H 0.3399 -0.0517 0.6822 0.139 Uiso 1 1 calc R . . H35B H 0.2801 -0.1199 0.7645 0.139 Uiso 1 1 calc R . . H35C H 0.2947 -0.0124 0.7653 0.139 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0361(5) 0.0387(5) 0.0368(5) -0.0165(4) 0.0056(4) -0.0146(4) Ti2 0.0364(5) 0.0457(6) 0.0382(5) -0.0200(4) 0.0066(4) -0.0147(4) O1 0.0397(19) 0.053(2) 0.0347(17) -0.0187(16) 0.0046(14) -0.0188(16) O2 0.0449(19) 0.057(2) 0.0413(18) -0.0258(17) 0.0111(15) -0.0181(17) O3 0.0400(19) 0.059(2) 0.0493(19) -0.0297(17) 0.0116(15) -0.0255(17) O4 0.051(2) 0.033(2) 0.0503(19) -0.0161(16) 0.0179(15) -0.0084(16) O5 0.0400(19) 0.051(2) 0.0415(18) -0.0272(16) 0.0043(14) -0.0140(16) O6 0.057(2) 0.064(2) 0.0421(19) -0.0264(18) 0.0142(16) -0.0276(18) O7 0.0299(18) 0.069(2) 0.052(2) -0.0248(18) 0.0031(15) -0.0156(17) O8 0.056(2) 0.039(2) 0.0500(19) -0.0178(16) 0.0178(16) -0.0168(17) N1 0.034(2) 0.034(2) 0.032(2) -0.0118(17) 0.0037(16) -0.0127(17) N2 0.036(2) 0.031(2) 0.035(2) -0.0157(18) 0.0045(16) -0.0059(17) C1 0.043(3) 0.036(3) 0.039(3) -0.016(2) 0.008(2) -0.007(2) C2 0.040(3) 0.031(3) 0.046(3) -0.018(2) 0.003(2) -0.005(2) C3 0.056(3) 0.038(3) 0.048(3) -0.019(2) 0.002(2) -0.014(2) C4 0.043(3) 0.030(3) 0.034(2) -0.015(2) 0.006(2) -0.007(2) C5 0.037(3) 0.038(3) 0.038(3) -0.018(2) 0.010(2) -0.011(2) C6 0.035(3) 0.041(3) 0.034(2) -0.012(2) 0.003(2) -0.014(2) C7 0.035(3) 0.040(3) 0.044(3) -0.014(2) 0.002(2) -0.014(2) C8 0.044(3) 0.050(3) 0.044(3) -0.014(2) -0.005(2) -0.021(3) C9 0.096(5) 0.063(4) 0.053(3) -0.020(3) -0.013(3) -0.040(3) C10 0.069(4) 0.061(4) 0.045(3) -0.011(3) -0.010(3) -0.029(3) C11 0.054(4) 0.095(5) 0.065(4) -0.021(3) -0.006(3) -0.035(3) C12 0.055(3) 0.071(4) 0.041(3) -0.025(3) 0.009(3) -0.020(3) C13 0.288(12) 0.111(7) 0.079(5) -0.071(5) 0.075(6) -0.088(7) C14 0.065(4) 0.202(9) 0.057(4) -0.053(5) 0.028(3) -0.060(5) C15 0.036(3) 0.061(4) 0.071(4) -0.028(3) 0.003(3) -0.023(3) C16 0.086(5) 0.076(6) 0.193(9) 0.011(6) 0.025(6) -0.035(5) C17 0.074(5) 0.210(9) 0.122(6) -0.095(6) 0.024(4) -0.087(6) C18 0.042(3) 0.037(3) 0.050(3) -0.015(2) 0.009(2) -0.007(2) C19 0.069(4) 0.049(4) 0.085(4) -0.022(3) -0.008(3) -0.018(3) C20 0.061(4) 0.053(4) 0.059(3) -0.012(3) 0.005(3) -0.010(3) C21 0.032(3) 0.037(3) 0.046(3) -0.019(2) 0.002(2) -0.006(2) C22 0.033(3) 0.042(3) 0.045(3) -0.020(2) 0.005(2) -0.012(2) C23 0.044(3) 0.045(3) 0.049(3) -0.023(3) -0.006(2) -0.004(2) C24 0.037(3) 0.074(4) 0.084(4) -0.037(3) -0.003(3) -0.018(3) C25 0.065(4) 0.050(4) 0.053(3) -0.019(3) -0.016(3) -0.005(3) C26 0.053(3) 0.064(4) 0.062(3) -0.035(3) -0.018(3) -0.001(3) C27 0.062(4) 0.074(4) 0.045(3) -0.030(3) 0.015(3) -0.030(3) C28 0.148(7) 0.113(7) 0.048(4) -0.023(4) 0.028(4) -0.008(6) C29 0.064(4) 0.152(7) 0.080(4) -0.077(5) 0.030(3) -0.042(4) C30 0.037(3) 0.093(5) 0.124(5) -0.070(4) 0.003(3) -0.018(3) C31 0.042(4) 0.052(4) 0.220(9) -0.023(5) 0.007(5) -0.011(3) C32 0.077(4) 0.077(5) 0.097(5) -0.025(4) -0.006(4) -0.047(4) C33 0.059(3) 0.041(3) 0.047(3) -0.017(3) 0.012(2) -0.021(3) C34 0.093(5) 0.064(4) 0.079(4) -0.037(3) 0.026(3) -0.044(4) C35 0.074(5) 0.063(4) 0.116(6) 0.003(4) -0.026(4) -0.022(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 O2 1.784(3) . ? Ti1 O4 1.820(3) . ? Ti1 O3 1.821(3) . ? Ti1 O1 1.853(3) . ? Ti1 N1 2.378(3) . ? Ti2 O6 1.792(3) . ? Ti2 O8 1.820(3) . ? Ti2 O7 1.831(3) . ? Ti2 O5 1.853(3) . ? Ti2 N2 2.391(3) . ? O1 C6 1.418(5) . ? O2 C12 1.433(5) . ? O3 C15 1.426(5) . ? O4 C18 1.413(5) . ? O5 C21 1.415(5) . ? O6 C27 1.415(5) . ? O7 C30 1.418(5) . ? O8 C33 1.429(5) . ? N1 C7 1.489(5) . ? N1 C5 1.491(5) . ? N1 C1 1.499(5) . ? N2 C22 1.484(5) . ? N2 C2 1.496(5) . ? N2 C4 1.498(5) . ? C1 C3 1.518(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.518(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.515(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.522(6) . ? C6 C8 1.549(5) . ? C6 H6 1.0000 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C11 1.518(7) . ? C8 C9 1.533(7) . ? C8 C10 1.550(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.481(7) . ? C12 C13 1.499(8) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.486(7) . ? C15 C16 1.498(8) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.501(6) . ? C18 C19 1.511(6) . ? C18 H18 1.0000 . ? 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 C22 1.538(5) . ? C21 C23 1.538(6) . ? C21 H21 1.0000 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C25 1.523(7) . ? C23 C24 1.541(7) . ? C23 C26 1.544(6) . ? 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 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.487(7) . ? C27 C28 1.494(8) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.415(8) . ? C30 C32 1.454(7) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.488(7) . ? C33 C34 1.522(6) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ti1 O4 100.46(14) . . ? O2 Ti1 O3 99.60(13) . . ? O4 Ti1 O3 115.90(14) . . ? O2 Ti1 O1 95.42(13) . . ? O4 Ti1 O1 118.40(14) . . ? O3 Ti1 O1 119.31(14) . . ? O2 Ti1 N1 170.99(12) . . ? O4 Ti1 N1 81.51(13) . . ? O3 Ti1 N1 87.27(12) . . ? O1 Ti1 N1 76.04(12) . . ? O6 Ti2 O8 99.54(15) . . ? O6 Ti2 O7 99.95(14) . . ? O8 Ti2 O7 116.23(14) . . ? O6 Ti2 O5 95.49(13) . . ? O8 Ti2 O5 118.61(14) . . ? O7 Ti2 O5 119.01(14) . . ? O6 Ti2 N2 170.38(12) . . ? O8 Ti2 N2 83.62(13) . . ? O7 Ti2 N2 86.61(13) . . ? O5 Ti2 N2 75.10(12) . . ? C6 O1 Ti1 126.8(2) . . ? C12 O2 Ti1 146.1(3) . . ? C15 O3 Ti1 133.4(3) . . ? C18 O4 Ti1 137.2(3) . . ? C21 O5 Ti2 127.3(2) . . ? C27 O6 Ti2 145.8(3) . . ? C30 O7 Ti2 131.2(4) . . ? C33 O8 Ti2 135.7(3) . . ? C7 N1 C5 106.5(3) . . ? C7 N1 C1 108.0(3) . . ? C5 N1 C1 112.4(3) . . ? C7 N1 Ti1 98.7(2) . . ? C5 N1 Ti1 117.3(2) . . ? C1 N1 Ti1 112.4(2) . . ? C22 N2 C2 111.5(3) . . ? C22 N2 C4 109.1(3) . . ? C2 N2 C4 110.9(3) . . ? C22 N2 Ti2 99.0(2) . . ? C2 N2 Ti2 111.5(2) . . ? C4 N2 Ti2 114.3(2) . . ? N1 C1 C3 117.3(4) . . ? N1 C1 H1A 108.0 . . ? C3 C1 H1A 108.0 . . ? N1 C1 H1B 108.0 . . ? C3 C1 H1B 108.0 . . ? H1A C1 H1B 107.2 . . ? N2 C2 C3 117.4(3) . . ? N2 C2 H2A 108.0 . . ? C3 C2 H2A 108.0 . . ? N2 C2 H2B 108.0 . . ? C3 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? C1 C3 C2 115.3(4) . . ? C1 C3 H3A 108.5 . . ? C2 C3 H3A 108.5 . . ? C1 C3 H3B 108.5 . . ? C2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? N2 C4 C5 112.2(3) . . ? N2 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N1 C5 C4 114.7(3) . . ? N1 C5 H5A 108.6 . . ? C4 C5 H5A 108.6 . . ? N1 C5 H5B 108.6 . . ? C4 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? O1 C6 C7 107.4(3) . . ? O1 C6 C8 111.7(3) . . ? C7 C6 C8 114.3(4) . . ? O1 C6 H6 107.7 . . ? C7 C6 H6 107.7 . . ? C8 C6 H6 107.7 . . ? N1 C7 C6 109.9(3) . . ? N1 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? N1 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C11 C8 C9 110.4(4) . . ? C11 C8 C6 109.2(4) . . ? C9 C8 C6 111.1(4) . . ? C11 C8 C10 109.5(4) . . ? C9 C8 C10 108.7(4) . . ? C6 C8 C10 108.0(4) . . ? 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 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 C12 C14 109.9(4) . . ? O2 C12 C13 107.5(4) . . ? C14 C12 C13 114.6(6) . . ? O2 C12 H12 108.2 . . ? C14 C12 H12 108.2 . . ? C13 C12 H12 108.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C17 109.2(4) . . ? O3 C15 C16 109.3(4) . . ? C17 C15 C16 112.0(6) . . ? O3 C15 H15 108.8 . . ? C17 C15 H15 108.8 . . ? C16 C15 H15 108.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 C20 109.1(4) . . ? O4 C18 C19 108.7(4) . . ? C20 C18 C19 112.4(4) . . ? O4 C18 H18 108.8 . . ? C20 C18 H18 108.8 . . ? C19 C18 H18 108.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 C22 107.6(3) . . ? O5 C21 C23 110.4(4) . . ? C22 C21 C23 114.5(4) . . ? O5 C21 H21 108.1 . . ? C22 C21 H21 108.1 . . ? C23 C21 H21 108.1 . . ? N2 C22 C21 109.9(3) . . ? N2 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? N2 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C25 C23 C21 111.8(4) . . ? C25 C23 C24 110.0(4) . . ? C21 C23 C24 109.6(4) . . ? C25 C23 C26 109.3(4) . . ? C21 C23 C26 107.4(4) . . ? C24 C23 C26 108.7(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 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O6 C27 C29 109.4(4) . . ? O6 C27 C28 109.2(4) . . ? C29 C27 C28 113.9(6) . . ? O6 C27 H27 108.1 . . ? C29 C27 H27 108.1 . . ? C28 C27 H27 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 . . ? C31 C30 O7 111.7(5) . . ? C31 C30 C32 120.1(6) . . ? O7 C30 C32 111.2(5) . . ? C31 C30 H30 103.9 . . ? O7 C30 H30 103.9 . . ? C32 C30 H30 103.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O8 C33 C35 109.1(4) . . ? O8 C33 C34 108.1(4) . . ? C35 C33 C34 111.6(5) . . ? O8 C33 H33 109.3 . . ? C35 C33 H33 109.3 . . ? C34 C33 H33 109.3 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.451 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.061 # Attachment 'L2Ti_OiPr_2.cif' data_s92_2 _database_code_depnum_ccdc_archive 'CCDC 286916' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H48 N2 O4 Ti' _chemical_formula_weight 452.52 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 8.830(5) _cell_length_b 9.726(5) _cell_length_c 17.047(5) _cell_angle_alpha 93.801(5) _cell_angle_beta 98.098(5) _cell_angle_gamma 112.844(5) _cell_volume 1323.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.9025 _exptl_absorpt_correction_T_max 0.9930 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean '9.091 pixels mm^1^' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13694 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4583 _reflns_number_gt 3854 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski and MInor, 1997)' _computing_data_reduction 'DENZO, COLLECT, MAXUS (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0247P)^2^+1.0046P] 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 SHELXL _refine_ls_extinction_coef 0.0073(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4583 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 N1 N 0.6552(2) 0.10074(19) 0.26968(10) 0.0206(4) Uani 1 1 d . . . N2 N 0.8831(2) 0.35876(19) 0.21379(10) 0.0203(4) Uani 1 1 d . . . O1 O 0.51009(17) 0.19092(14) 0.15463(8) 0.0184(3) Uani 1 1 d . . . O2 O 0.79413(16) 0.43342(15) 0.34162(8) 0.0189(3) Uani 1 1 d . . . O3 O 0.46284(17) 0.27679(16) 0.30965(8) 0.0225(3) Uani 1 1 d . . . O4 O 0.62997(17) 0.48719(15) 0.20019(8) 0.0221(3) Uani 1 1 d . . . Ti1 Ti 0.62959(4) 0.32558(4) 0.24996(2) 0.01705(13) Uani 1 1 d . . . C1 C 0.4493(2) 0.0329(2) 0.14554(12) 0.0180(4) Uani 1 1 d . . . H1 H 0.5121 0.0018 0.1085 0.022 Uiso 1 1 calc R . . C2 C 0.4911(3) -0.0130(2) 0.22750(12) 0.0208(5) Uani 1 1 d . . . H2A H 0.4036 -0.0191 0.2593 0.025 Uiso 1 1 calc R . . H2B H 0.4954 -0.1132 0.2206 0.025 Uiso 1 1 calc R . . C3 C 0.7926(3) 0.0914(2) 0.23104(14) 0.0252(5) Uani 1 1 d . . . H3A H 0.7523 0.0597 0.1729 0.030 Uiso 1 1 calc R . . H3B H 0.8291 0.0156 0.2535 0.030 Uiso 1 1 calc R . . C4 C 0.9379(3) 0.2434(2) 0.24553(14) 0.0256(5) Uani 1 1 d . . . H4A H 0.9822 0.2722 0.3036 0.031 Uiso 1 1 calc R . . H4B H 1.0284 0.2380 0.2188 0.031 Uiso 1 1 calc R . . C5 C 0.9948(3) 0.5102(2) 0.25610(12) 0.0212(5) Uani 1 1 d . . . H5A H 0.9722 0.5883 0.2283 0.025 Uiso 1 1 calc R . . H5B H 1.1129 0.5269 0.2565 0.025 Uiso 1 1 calc R . . C6 C 0.9637(2) 0.5213(2) 0.34214(12) 0.0187(4) Uani 1 1 d . . . H6 H 1.0306 0.4751 0.3744 0.022 Uiso 1 1 calc R . . C7 C 0.2622(2) -0.0410(2) 0.10775(12) 0.0190(4) Uani 1 1 d . . . C8 C 0.2419(3) 0.0141(2) 0.02642(13) 0.0254(5) Uani 1 1 d . . . H8A H 0.3169 -0.0058 -0.0056 0.038 Uiso 1 1 calc R . . H8B H 0.2697 0.1225 0.0343 0.038 Uiso 1 1 calc R . . H8C H 0.1260 -0.0392 -0.0015 0.038 Uiso 1 1 calc R . . C9 C 0.1555(3) 0.0033(3) 0.15963(14) 0.0277(5) Uani 1 1 d . . . H9A H 0.0414 -0.0297 0.1297 0.042 Uiso 1 1 calc R . . H9B H 0.2038 0.1128 0.1740 0.042 Uiso 1 1 calc R . . H9C H 0.1530 -0.0450 0.2084 0.042 Uiso 1 1 calc R . . C10 C 0.2043(3) -0.2127(2) 0.09542(14) 0.0290(5) Uani 1 1 d . . . H10A H 0.0885 -0.2592 0.0667 0.043 Uiso 1 1 calc R . . H10B H 0.2111 -0.2491 0.1475 0.043 Uiso 1 1 calc R . . H10C H 0.2762 -0.2396 0.0642 0.043 Uiso 1 1 calc R . . C11 C 0.6811(3) 0.0787(3) 0.35465(13) 0.0292(5) Uani 1 1 d . . . H11A H 0.5924 0.0898 0.3797 0.044 Uiso 1 1 calc R . . H11B H 0.7898 0.1540 0.3822 0.044 Uiso 1 1 calc R . . H11C H 0.6781 -0.0224 0.3585 0.044 Uiso 1 1 calc R . . C12 C 0.8803(3) 0.3556(3) 0.12684(13) 0.0299(5) Uani 1 1 d . . . H12A H 0.8429 0.4319 0.1074 0.045 Uiso 1 1 calc R . . H12B H 0.8032 0.2559 0.0994 0.045 Uiso 1 1 calc R . . H12C H 0.9928 0.3770 0.1160 0.045 Uiso 1 1 calc R . . C13 C 1.0186(3) 0.6848(2) 0.38205(13) 0.0219(5) Uani 1 1 d . . . C14 C 1.2056(3) 0.7717(3) 0.38303(16) 0.0353(6) Uani 1 1 d . . . H14A H 1.2439 0.8714 0.4140 0.053 Uiso 1 1 calc R . . H14B H 1.2248 0.7829 0.3281 0.053 Uiso 1 1 calc R . . H14C H 1.2676 0.7162 0.4076 0.053 Uiso 1 1 calc R . . C15 C 0.9187(3) 0.7647(2) 0.33875(14) 0.0305(5) Uani 1 1 d . . . H15A H 0.7989 0.7042 0.3346 0.046 Uiso 1 1 calc R . . H15B H 0.9451 0.7773 0.2850 0.046 Uiso 1 1 calc R . . H15C H 0.9483 0.8637 0.3689 0.046 Uiso 1 1 calc R . . C16 C 0.9880(3) 0.6798(2) 0.46811(13) 0.0301(5) Uani 1 1 d . . . H16A H 1.0590 0.6375 0.4980 0.045 Uiso 1 1 calc R . . H16B H 0.8704 0.6167 0.4681 0.045 Uiso 1 1 calc R . . H16C H 1.0151 0.7820 0.4934 0.045 Uiso 1 1 calc R . . C17 C 0.5482(3) 0.5058(2) 0.12665(13) 0.0240(5) Uani 1 1 d . . . H17 H 0.5464 0.4293 0.0839 0.029 Uiso 1 1 calc R . . C18 C 0.6458(3) 0.6613(3) 0.10637(15) 0.0360(6) Uani 1 1 d . . . H18A H 0.6537 0.7373 0.1493 0.054 Uiso 1 1 calc R . . H18B H 0.5884 0.6761 0.0561 0.054 Uiso 1 1 calc R . . H18C H 0.7583 0.6714 0.1005 0.054 Uiso 1 1 calc R . . C19 C 0.3701(3) 0.4806(3) 0.13218(17) 0.0389(6) Uani 1 1 d . . . H19A H 0.3107 0.3784 0.1444 0.058 Uiso 1 1 calc R . . H19B H 0.3141 0.4935 0.0811 0.058 Uiso 1 1 calc R . . H19C H 0.3703 0.5537 0.1747 0.058 Uiso 1 1 calc R . . C20 C 0.4551(3) 0.3382(2) 0.38650(13) 0.0238(5) Uani 1 1 d . . . H20 H 0.5663 0.3695 0.4220 0.029 Uiso 1 1 calc R . . C21 C 0.4150(3) 0.4750(3) 0.37860(14) 0.0316(6) Uani 1 1 d . . . H21A H 0.5021 0.5503 0.3559 0.047 Uiso 1 1 calc R . . H21B H 0.4103 0.5178 0.4314 0.047 Uiso 1 1 calc R . . H21C H 0.3068 0.4455 0.3433 0.047 Uiso 1 1 calc R . . C22 C 0.3244(3) 0.2183(3) 0.42187(16) 0.0433(7) Uani 1 1 d . . . H22A H 0.2155 0.1849 0.3866 0.065 Uiso 1 1 calc R . . H22B H 0.3178 0.2600 0.4746 0.065 Uiso 1 1 calc R . . H22C H 0.3554 0.1325 0.4273 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0203(9) 0.0226(9) 0.0188(9) 0.0001(7) 0.0009(7) 0.0101(8) N2 0.0180(9) 0.0216(9) 0.0197(9) -0.0020(7) 0.0039(7) 0.0069(8) O1 0.0186(7) 0.0141(7) 0.0206(8) 0.0010(6) 0.0035(6) 0.0047(6) O2 0.0155(7) 0.0171(7) 0.0202(8) -0.0010(6) 0.0037(6) 0.0030(6) O3 0.0190(8) 0.0222(8) 0.0248(8) -0.0022(6) 0.0081(6) 0.0060(7) O4 0.0229(8) 0.0190(8) 0.0233(8) 0.0017(6) 0.0009(6) 0.0086(7) Ti1 0.0154(2) 0.0156(2) 0.0196(2) 0.00005(15) 0.00421(15) 0.00562(16) C1 0.0180(10) 0.0161(10) 0.0197(11) -0.0004(8) 0.0049(9) 0.0066(9) C2 0.0202(11) 0.0176(11) 0.0238(12) 0.0003(9) 0.0028(9) 0.0075(9) C3 0.0229(12) 0.0255(12) 0.0307(13) -0.0030(10) 0.0012(10) 0.0156(10) C4 0.0207(11) 0.0285(12) 0.0298(13) -0.0031(10) 0.0017(9) 0.0145(10) C5 0.0159(11) 0.0230(11) 0.0223(11) 0.0014(9) 0.0049(9) 0.0048(9) C6 0.0159(10) 0.0184(11) 0.0210(11) 0.0024(9) 0.0028(9) 0.0062(9) C7 0.0178(11) 0.0180(11) 0.0202(11) 0.0010(9) 0.0033(9) 0.0062(9) C8 0.0215(12) 0.0262(12) 0.0243(12) 0.0011(9) 0.0024(9) 0.0060(10) C9 0.0205(12) 0.0319(13) 0.0318(13) 0.0033(10) 0.0087(10) 0.0105(10) C10 0.0239(12) 0.0205(12) 0.0342(14) -0.0002(10) -0.0001(10) 0.0025(10) C11 0.0357(13) 0.0266(12) 0.0243(12) 0.0048(10) -0.0002(10) 0.0132(11) C12 0.0238(12) 0.0404(14) 0.0245(12) -0.0016(10) 0.0083(10) 0.0115(11) C13 0.0201(11) 0.0161(11) 0.0255(12) 0.0023(9) 0.0016(9) 0.0040(9) C14 0.0255(13) 0.0201(12) 0.0514(16) -0.0003(11) 0.0028(11) 0.0020(10) C15 0.0349(13) 0.0208(12) 0.0361(14) 0.0030(10) 0.0037(11) 0.0125(11) C16 0.0390(14) 0.0207(12) 0.0250(13) -0.0065(10) 0.0005(10) 0.0092(11) C17 0.0244(12) 0.0224(11) 0.0249(12) 0.0030(9) 0.0005(9) 0.0104(10) C18 0.0401(15) 0.0292(13) 0.0346(14) 0.0127(11) 0.0064(12) 0.0082(12) C19 0.0249(13) 0.0360(14) 0.0578(18) 0.0172(13) 0.0031(12) 0.0140(12) C20 0.0232(11) 0.0263(12) 0.0222(11) -0.0008(9) 0.0085(9) 0.0094(10) C21 0.0321(13) 0.0321(13) 0.0338(14) -0.0023(11) 0.0081(11) 0.0169(11) C22 0.0508(17) 0.0353(15) 0.0472(17) 0.0075(12) 0.0318(14) 0.0130(13) _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 N1 C11 1.477(3) . ? N1 C2 1.482(3) . ? N1 C3 1.489(3) . ? N1 Ti1 2.325(2) . ? N2 C12 1.477(3) . ? N2 C5 1.481(3) . ? N2 C4 1.488(3) . ? N2 Ti1 2.313(2) . ? O1 C1 1.407(2) . ? O1 Ti1 1.9056(15) . ? O2 C6 1.405(2) . ? O2 Ti1 1.9006(15) . ? O3 C20 1.425(2) . ? O3 Ti1 1.8363(15) . ? O4 C17 1.415(2) . ? O4 Ti1 1.8342(16) . ? C1 C2 1.534(3) . ? C1 C7 1.542(3) . ? C3 C4 1.510(3) . ? C5 C6 1.534(3) . ? C6 C13 1.547(3) . ? C7 C8 1.531(3) . ? C7 C9 1.535(3) . ? C7 C10 1.535(3) . ? C13 C16 1.529(3) . ? C13 C14 1.532(3) . ? C13 C15 1.533(3) . ? C17 C19 1.513(3) . ? C17 C18 1.514(3) . ? C20 C21 1.512(3) . ? C20 C22 1.517(3) . ? 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 C11 N1 C2 109.82(16) . . ? C11 N1 C3 110.64(17) . . ? C2 N1 C3 110.65(16) . . ? C11 N1 Ti1 113.65(12) . . ? C2 N1 Ti1 102.21(12) . . ? C3 N1 Ti1 109.58(12) . . ? C12 N2 C5 110.27(16) . . ? C12 N2 C4 111.10(16) . . ? C5 N2 C4 110.06(17) . . ? C12 N2 Ti1 113.71(13) . . ? C5 N2 Ti1 102.45(11) . . ? C4 N2 Ti1 108.92(12) . . ? C1 O1 Ti1 126.75(12) . . ? C6 O2 Ti1 126.10(12) . . ? C20 O3 Ti1 132.32(13) . . ? C17 O4 Ti1 135.18(13) . . ? O4 Ti1 O3 107.70(7) . . ? O4 Ti1 O2 98.10(7) . . ? O3 Ti1 O2 91.41(7) . . ? O4 Ti1 O1 91.10(7) . . ? O3 Ti1 O1 99.38(7) . . ? O2 Ti1 O1 163.03(6) . . ? O4 Ti1 N2 89.70(6) . . ? O3 Ti1 N2 159.17(7) . . ? O2 Ti1 N2 74.47(7) . . ? O1 Ti1 N2 91.43(6) . . ? O4 Ti1 N1 159.25(6) . . ? O3 Ti1 N1 89.56(6) . . ? O2 Ti1 N1 92.78(7) . . ? O1 Ti1 N1 74.37(6) . . ? N2 Ti1 N1 76.20(6) . . ? O1 C1 C2 107.55(16) . . ? O1 C1 C7 111.60(16) . . ? C2 C1 C7 114.11(16) . . ? N1 C2 C1 108.83(16) . . ? N1 C3 C4 109.50(17) . . ? N2 C4 C3 110.12(17) . . ? N2 C5 C6 108.92(16) . . ? O2 C6 C5 108.10(16) . . ? O2 C6 C13 112.19(16) . . ? C5 C6 C13 113.65(17) . . ? C8 C7 C9 108.72(17) . . ? C8 C7 C10 109.19(17) . . ? C9 C7 C10 110.08(17) . . ? C8 C7 C1 107.66(16) . . ? C9 C7 C1 111.62(17) . . ? C10 C7 C1 109.51(17) . . ? C16 C13 C14 109.06(19) . . ? C16 C13 C15 108.45(18) . . ? C14 C13 C15 110.08(18) . . ? C16 C13 C6 108.20(17) . . ? C14 C13 C6 109.13(17) . . ? C15 C13 C6 111.86(18) . . ? O4 C17 C19 109.80(18) . . ? O4 C17 C18 108.95(18) . . ? C19 C17 C18 111.91(19) . . ? O3 C20 C21 109.33(18) . . ? O3 C20 C22 109.03(18) . . ? C21 C20 C22 111.61(19) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.209 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.054