# 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, 2007 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Helgard G. Raubenheimer' 'Jocelyn Bruce' 'Stefan Nogai' 'Oliver Schuster' _publ_contact_author_name 'Helgard G. Raubenheimer' _publ_contact_author_address ; Department of Chemistry and Polymer Science University of Stellenbosch Stellenbosch 7602 SOUTH AFRICA ; _publ_contact_author_email HGR@SUN.AC.ZA _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Synthesis and Structure of potential Single-Source Titanoxy Carbene Complex Precursors for nano-sized MTiOx and MTiNyOz (M = Cr, W) ; #============================================================================== data_[{(OC)5Cr=C(Me)OTi(OiPr)2}(OiPr)]2 _database_code_depnum_ccdc_archive 'CCDC 670773' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H48 Cr2 O18 Ti2' _chemical_formula_sum 'C32 H48 Cr2 O18 Ti2' _chemical_formula_weight 920.50 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' Cr Cr 0.3209 0.6236 '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 10.4677(6) _cell_length_b 10.9006(6) _cell_length_c 11.5402(7) _cell_angle_alpha 87.7710(10) _cell_angle_beta 67.0230(10) _cell_angle_gamma 70.1630(10) _cell_volume 1133.70(11) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4538 _cell_measurement_theta_min 26.08 _cell_measurement_theta_max 2.26 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7163 _exptl_absorpt_correction_T_max 0.8452 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8280 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.11 _reflns_number_total 4401 _reflns_number_gt 3895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 terminal isopropoxide groups are disordered. PART instructions and similarity restraints (SAME-instruction in Shelxl) were applied to model the disorder as best as possible. ; _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^)+(0.0583P)^2^+0.1961P] 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 4401 _refine_ls_number_parameters 320 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.043 _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 Cr1 Cr 0.16610(3) 0.34833(3) 0.64353(3) 0.04465(11) Uani 1 1 d . B . Ti1 Ti -0.10638(3) 0.10500(3) 0.94424(3) 0.03597(11) Uani 1 1 d D . . O2 O 0.2410(3) 0.5718(2) 0.5041(2) 0.1046(8) Uani 1 1 d . . . O3 O -0.1641(2) 0.5028(2) 0.7523(2) 0.0952(6) Uani 1 1 d . . . O4 O 0.1519(3) 0.2334(2) 0.41647(18) 0.0949(6) Uani 1 1 d . . . O5 O 0.4935(2) 0.1911(2) 0.5428(2) 0.1030(7) Uani 1 1 d . . . O6 O 0.1682(3) 0.44809(19) 0.88438(18) 0.0902(6) Uani 1 1 d . . . O11 O 0.00266(15) 0.20988(13) 0.83495(12) 0.0457(3) Uani 1 1 d . B . O21 O 0.04503(13) 0.07715(11) 1.02859(11) 0.0387(3) Uani 1 1 d . . . O31 O -0.25340(14) 0.20709(14) 1.07862(13) 0.0551(4) Uani 1 1 d D A . C2 C 0.2119(3) 0.4888(2) 0.5574(2) 0.0664(6) Uani 1 1 d . . . C3 C -0.0412(3) 0.4451(2) 0.7102(2) 0.0610(5) Uani 1 1 d . . . C4 C 0.1561(3) 0.2791(2) 0.5018(2) 0.0599(5) Uani 1 1 d . . . C5 C 0.3699(3) 0.2502(3) 0.5818(2) 0.0628(6) Uani 1 1 d . . . C6 C 0.1698(3) 0.4097(2) 0.7928(2) 0.0576(5) Uani 1 1 d . . . C11 C 0.1166(2) 0.19481(18) 0.73313(17) 0.0435(4) Uani 1 1 d . . . C12 C 0.2067(3) 0.0525(2) 0.6843(2) 0.0725(7) Uani 1 1 d . B . H12A H 0.1411 0.0062 0.6873 0.109 Uiso 1 1 calc R . . H12B H 0.2602 0.0136 0.7366 0.109 Uiso 1 1 calc R . . H12C H 0.2767 0.0461 0.5976 0.109 Uiso 1 1 calc R . . C22 C 0.0667(3) 0.19027(19) 1.0707(2) 0.0540(5) Uani 1 1 d . . . H22 H 0.0200 0.2671 1.0337 0.065 Uiso 1 1 calc R B . C23 C 0.2301(3) 0.1674(3) 1.0199(3) 0.0795(8) Uani 1 1 d . B . H23A H 0.2773 0.0967 1.0598 0.119 Uiso 1 1 calc R . . H23B H 0.2441 0.2468 1.0381 0.119 Uiso 1 1 calc R . . H23C H 0.2739 0.1438 0.9290 0.119 Uiso 1 1 calc R . . C24 C -0.0116(4) 0.2185(2) 1.2130(2) 0.0744(7) Uani 1 1 d . B . H24A H -0.1150 0.2288 1.2389 0.112 Uiso 1 1 calc R . . H24B H -0.0049 0.2986 1.2397 0.112 Uiso 1 1 calc R . . H24C H 0.0350 0.1462 1.2518 0.112 Uiso 1 1 calc R . . C32A C -0.4083(4) 0.2875(6) 1.1296(6) 0.065(2) Uani 0.662(8) 1 d PD A 1 H32A H -0.4327 0.3349 1.0617 0.078 Uiso 0.662(8) 1 calc PR A 1 C33A C -0.4342(7) 0.3842(8) 1.2308(9) 0.149(5) Uani 0.662(8) 1 d PD A 1 H33A H -0.3922 0.3389 1.2887 0.223 Uiso 0.662(8) 1 calc PR A 1 H33B H -0.5399 0.4295 1.2765 0.223 Uiso 0.662(8) 1 calc PR A 1 H33C H -0.3873 0.4472 1.1932 0.223 Uiso 0.662(8) 1 calc PR A 1 C34A C -0.4992(5) 0.2062(5) 1.1785(6) 0.0862(17) Uani 0.662(8) 1 d PD A 1 H34A H -0.4737 0.1391 1.1123 0.129 Uiso 0.662(8) 1 calc PR A 1 H34B H -0.6031 0.2604 1.2064 0.129 Uiso 0.662(8) 1 calc PR A 1 H34C H -0.4813 0.1649 1.2494 0.129 Uiso 0.662(8) 1 calc PR A 1 C32B C -0.4062(10) 0.2867(17) 1.119(2) 0.140(11) Uani 0.338(8) 1 d PD A 2 H32B H -0.4485 0.2418 1.0781 0.168 Uiso 0.338(8) 1 calc PR A 2 C33B C -0.4232(11) 0.4136(10) 1.0700(17) 0.138(7) Uani 0.338(8) 1 d PD A 2 H33D H -0.4250 0.4079 0.9870 0.207 Uiso 0.338(8) 1 calc PR A 2 H33E H -0.3406 0.4392 1.0633 0.207 Uiso 0.338(8) 1 calc PR A 2 H33F H -0.5152 0.4784 1.1271 0.207 Uiso 0.338(8) 1 calc PR A 2 C34B C -0.4810(19) 0.290(3) 1.2466(13) 0.26(2) Uani 0.338(8) 1 d PD A 2 H34D H -0.5583 0.2532 1.2625 0.397 Uiso 0.338(8) 1 calc PR A 2 H34E H -0.5251 0.3795 1.2855 0.397 Uiso 0.338(8) 1 calc PR A 2 H34F H -0.4125 0.2379 1.2824 0.397 Uiso 0.338(8) 1 calc PR A 2 O41A O -0.199(2) 0.1002(19) 0.8467(18) 0.049(3) Uani 0.526(14) 1 d PD B 1 C42A C -0.2608(12) 0.1466(19) 0.7551(9) 0.138(6) Uani 0.526(14) 1 d PD B 1 H42A H -0.2986 0.0749 0.7544 0.166 Uiso 0.526(14) 1 calc PR B 1 C43A C -0.3960(10) 0.2479(13) 0.7987(8) 0.130(5) Uani 0.526(14) 1 d PD B 1 H43A H -0.3805 0.3310 0.7862 0.195 Uiso 0.526(14) 1 calc PR B 1 H43B H -0.4498 0.2447 0.8882 0.195 Uiso 0.526(14) 1 calc PR B 1 H43C H -0.4530 0.2391 0.7525 0.195 Uiso 0.526(14) 1 calc PR B 1 C44A C -0.1556(13) 0.1189(14) 0.6285(7) 0.107(4) Uani 0.526(14) 1 d PD B 1 H44A H -0.2064 0.1343 0.5719 0.161 Uiso 0.526(14) 1 calc PR B 1 H44B H -0.0904 0.0279 0.6136 0.161 Uiso 0.526(14) 1 calc PR B 1 H44C H -0.0976 0.1754 0.6129 0.161 Uiso 0.526(14) 1 calc PR B 1 O41B O -0.184(3) 0.098(2) 0.836(2) 0.059(4) Uani 0.474(14) 1 d PD B 2 C42B C -0.2489(11) 0.1004(10) 0.7474(9) 0.066(3) Uani 0.474(14) 1 d PD B 2 H42B H -0.2027 0.0089 0.7068 0.079 Uiso 0.474(14) 1 calc PR B 2 C43B C -0.3996(10) 0.120(2) 0.7996(10) 0.154(7) Uani 0.474(14) 1 d PD B 2 H43D H -0.4391 0.1419 0.8905 0.231 Uiso 0.474(14) 1 calc PR B 2 H43E H -0.4140 0.0407 0.7819 0.231 Uiso 0.474(14) 1 calc PR B 2 H43F H -0.4507 0.1916 0.7629 0.231 Uiso 0.474(14) 1 calc PR B 2 C44B C -0.1942(18) 0.173(2) 0.6463(16) 0.154(8) Uani 0.474(14) 1 d PD B 2 H44D H -0.2487 0.1844 0.5928 0.231 Uiso 0.474(14) 1 calc PR B 2 H44E H -0.0898 0.1256 0.5966 0.231 Uiso 0.474(14) 1 calc PR B 2 H44F H -0.2070 0.2582 0.6805 0.231 Uiso 0.474(14) 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 Cr1 0.04760(19) 0.04348(19) 0.04087(19) 0.00952(13) -0.01471(14) -0.01779(14) Ti1 0.03466(17) 0.03505(18) 0.03786(18) 0.00687(13) -0.01589(14) -0.01064(13) O2 0.138(2) 0.0770(13) 0.0825(13) 0.0307(11) -0.0136(13) -0.0571(14) O3 0.0575(11) 0.0777(13) 0.1239(17) 0.0173(12) -0.0267(11) -0.0044(10) O4 0.1243(18) 0.1225(17) 0.0644(11) 0.0105(11) -0.0491(12) -0.0617(15) O5 0.0518(11) 0.1324(19) 0.0985(15) -0.0101(13) -0.0218(10) -0.0088(11) O6 0.1435(19) 0.0801(12) 0.0665(11) 0.0063(9) -0.0480(12) -0.0556(13) O11 0.0508(7) 0.0476(7) 0.0421(7) 0.0137(6) -0.0183(6) -0.0228(6) O21 0.0449(6) 0.0325(6) 0.0446(7) 0.0054(5) -0.0230(6) -0.0148(5) O31 0.0394(7) 0.0517(8) 0.0545(8) 0.0011(6) -0.0087(6) -0.0042(6) C2 0.0819(16) 0.0588(13) 0.0538(13) 0.0136(11) -0.0173(12) -0.0318(12) C3 0.0585(13) 0.0485(12) 0.0692(14) 0.0154(10) -0.0222(11) -0.0160(10) C4 0.0671(14) 0.0662(14) 0.0513(12) 0.0158(10) -0.0250(11) -0.0288(11) C5 0.0541(13) 0.0763(15) 0.0529(12) 0.0028(11) -0.0175(10) -0.0210(12) C6 0.0723(14) 0.0493(12) 0.0543(12) 0.0110(10) -0.0227(11) -0.0288(11) C11 0.0489(10) 0.0415(10) 0.0419(10) 0.0076(8) -0.0214(8) -0.0146(8) C12 0.0831(17) 0.0435(12) 0.0655(15) 0.0052(10) -0.0124(13) -0.0124(11) C22 0.0781(14) 0.0396(10) 0.0655(13) 0.0104(9) -0.0444(12) -0.0283(10) C23 0.0858(17) 0.0806(17) 0.111(2) 0.0318(16) -0.0576(17) -0.0563(15) C24 0.118(2) 0.0516(13) 0.0657(15) -0.0017(11) -0.0498(15) -0.0280(13) C32A 0.040(4) 0.056(5) 0.071(4) 0.008(3) -0.012(3) 0.004(4) C33A 0.066(3) 0.112(5) 0.197(11) -0.089(6) 0.011(4) -0.010(3) C34A 0.0391(19) 0.098(3) 0.104(4) 0.012(3) -0.012(2) -0.023(2) C32B 0.053(12) 0.088(18) 0.19(2) 0.024(14) 0.026(11) -0.003(11) C33B 0.066(6) 0.078(7) 0.211(17) 0.034(8) -0.019(7) 0.001(5) C34B 0.094(12) 0.42(5) 0.069(10) 0.082(18) 0.024(8) 0.083(19) O41A 0.048(3) 0.054(5) 0.062(6) 0.021(4) -0.035(3) -0.024(3) C42A 0.102(7) 0.215(14) 0.075(6) 0.034(8) -0.059(5) -0.004(7) C43A 0.088(5) 0.177(10) 0.106(5) 0.019(6) -0.068(5) 0.010(5) C44A 0.121(7) 0.141(8) 0.052(4) 0.017(4) -0.054(4) -0.015(5) O41B 0.069(9) 0.076(8) 0.054(5) 0.021(4) -0.040(5) -0.034(6) C42B 0.090(6) 0.079(4) 0.085(6) 0.041(3) -0.072(5) -0.057(4) C43B 0.108(7) 0.31(2) 0.138(7) 0.130(10) -0.102(6) -0.134(10) C44B 0.145(12) 0.26(2) 0.167(13) 0.148(14) -0.120(11) -0.143(15) _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 Cr1 C5 1.878(2) . ? Cr1 C4 1.881(2) . ? Cr1 C2 1.889(2) . ? Cr1 C6 1.892(2) . ? Cr1 C3 1.903(2) . ? Cr1 C11 2.0432(19) . ? Ti1 O41B 1.751(5) . ? Ti1 O41A 1.757(5) . ? Ti1 O31 1.7665(13) . ? Ti1 O21 1.9227(12) 2_557 ? Ti1 O11 1.9621(13) . ? Ti1 O21 2.0992(12) . ? Ti1 Ti1 3.2258(6) 2_557 ? O2 C2 1.135(3) . ? O3 C3 1.128(3) . ? O4 C4 1.144(3) . ? O5 C5 1.138(3) . ? O6 C6 1.143(3) . ? O11 C11 1.272(2) . ? O21 C22 1.459(2) . ? O21 Ti1 1.9227(12) 2_557 ? O31 C32B 1.427(8) . ? O31 C32A 1.440(4) . ? C11 C12 1.508(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C22 C23 1.507(4) . ? C22 C24 1.511(3) . ? C22 H22 0.9900 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C32A C34A 1.458(8) . ? C32A C33A 1.484(9) . ? C32A H32A 0.9900 . ? C33A H33A 0.9700 . ? C33A H33B 0.9700 . ? C33A H33C 0.9700 . ? C34A H34A 0.9700 . ? C34A H34B 0.9700 . ? C34A H34C 0.9700 . ? C32B C34B 1.372(17) . ? C32B C33B 1.453(15) . ? C32B H32B 0.9900 . ? C33B H33D 0.9700 . ? C33B H33E 0.9700 . ? C33B H33F 0.9700 . ? C34B H34D 0.9700 . ? C34B H34E 0.9700 . ? C34B H34F 0.9700 . ? O41A C42A 1.439(10) . ? C42A C43A 1.379(11) . ? C42A C44A 1.411(11) . ? C42A H42A 0.9900 . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C43A H43C 0.9700 . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C44A H44C 0.9700 . ? O41B C42B 1.428(8) . ? C42B C43B 1.391(11) . ? C42B C44B 1.424(11) . ? C42B H42B 0.9900 . ? C43B H43D 0.9700 . ? C43B H43E 0.9700 . ? C43B H43F 0.9700 . ? C44B H44D 0.9700 . ? C44B H44E 0.9700 . ? C44B H44F 0.9700 . ? 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 C5 Cr1 C4 90.02(10) . . ? C5 Cr1 C2 88.96(12) . . ? C4 Cr1 C2 91.49(10) . . ? C5 Cr1 C6 90.92(10) . . ? C4 Cr1 C6 175.92(9) . . ? C2 Cr1 C6 92.50(10) . . ? C5 Cr1 C3 178.37(10) . . ? C4 Cr1 C3 90.73(11) . . ? C2 Cr1 C3 92.47(11) . . ? C6 Cr1 C3 88.23(11) . . ? C5 Cr1 C11 91.00(9) . . ? C4 Cr1 C11 87.26(9) . . ? C2 Cr1 C11 178.75(9) . . ? C6 Cr1 C11 88.75(8) . . ? C3 Cr1 C11 87.59(9) . . ? O41B Ti1 O41A 4.8(16) . . ? O41B Ti1 O31 105.8(9) . . ? O41A Ti1 O31 101.5(8) . . ? O41B Ti1 O21 99.2(8) . 2_557 ? O41A Ti1 O21 99.3(6) . 2_557 ? O31 Ti1 O21 113.20(6) . 2_557 ? O41B Ti1 O11 90.0(8) . . ? O41A Ti1 O11 93.5(7) . . ? O31 Ti1 O11 109.26(6) . . ? O21 Ti1 O11 131.86(6) 2_557 . ? O41B Ti1 O21 162.5(9) . . ? O41A Ti1 O21 166.7(7) . . ? O31 Ti1 O21 91.72(6) . . ? O21 Ti1 O21 73.43(5) 2_557 . ? O11 Ti1 O21 83.82(5) . . ? O41B Ti1 Ti1 135.8(8) . 2_557 ? O41A Ti1 Ti1 136.8(6) . 2_557 ? O31 Ti1 Ti1 104.74(5) . 2_557 ? O21 Ti1 Ti1 38.59(3) 2_557 2_557 ? O11 Ti1 Ti1 109.13(4) . 2_557 ? O21 Ti1 Ti1 34.84(3) . 2_557 ? C11 O11 Ti1 139.56(13) . . ? C22 O21 Ti1 132.83(11) . 2_557 ? C22 O21 Ti1 119.85(10) . . ? Ti1 O21 Ti1 106.57(5) 2_557 . ? C32B O31 C32A 4.8(11) . . ? C32B O31 Ti1 139.3(10) . . ? C32A O31 Ti1 143.9(3) . . ? O2 C2 Cr1 178.9(2) . . ? O3 C3 Cr1 178.5(2) . . ? O4 C4 Cr1 178.0(2) . . ? O5 C5 Cr1 179.1(2) . . ? O6 C6 Cr1 178.2(2) . . ? O11 C11 C12 112.73(18) . . ? O11 C11 Cr1 123.06(14) . . ? C12 C11 Cr1 124.18(15) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O21 C22 C23 109.41(18) . . ? O21 C22 C24 109.82(17) . . ? C23 C22 C24 114.1(2) . . ? O21 C22 H22 107.7 . . ? C23 C22 H22 107.7 . . ? C24 C22 H22 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O31 C32A C34A 110.2(4) . . ? O31 C32A C33A 107.8(5) . . ? C34A C32A C33A 111.3(5) . . ? O31 C32A H32A 109.2 . . ? C34A C32A H32A 109.2 . . ? C33A C32A H32A 109.2 . . ? C34B C32B O31 111.0(14) . . ? C34B C32B C33B 115.8(19) . . ? O31 C32B C33B 111.1(10) . . ? C34B C32B H32B 106.1 . . ? O31 C32B H32B 106.1 . . ? C33B C32B H32B 106.1 . . ? C32B C33B H33D 109.5 . . ? C32B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C32B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C32B C34B H34D 109.5 . . ? C32B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C32B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C42A O41A Ti1 155.6(17) . . ? C43A C42A C44A 125.0(10) . . ? C43A C42A O41A 116.4(11) . . ? C44A C42A O41A 114.2(12) . . ? C43A C42A H42A 97.1 . . ? C44A C42A H42A 97.1 . . ? O41A C42A H42A 97.1 . . ? C42B O41B Ti1 176.3(18) . . ? C43B C42B C44B 118.9(10) . . ? C43B C42B O41B 115.6(12) . . ? C44B C42B O41B 110.2(12) . . ? C43B C42B H42B 103.3 . . ? C44B C42B H42B 103.3 . . ? O41B C42B H42B 103.3 . . ? C42B C43B H43D 109.5 . . ? C42B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C42B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C42B C44B H44D 109.5 . . ? C42B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C42B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O41B Ti1 O11 C11 -76.9(9) . . . . ? O41A Ti1 O11 C11 -80.2(7) . . . . ? O31 Ti1 O11 C11 176.35(18) . . . . ? O21 Ti1 O11 C11 25.5(2) 2_557 . . . ? O21 Ti1 O11 C11 86.68(19) . . . . ? Ti1 Ti1 O11 C11 62.37(19) 2_557 . . . ? O41B Ti1 O21 C22 121(3) . . . . ? O41A Ti1 O21 C22 130(3) . . . . ? O31 Ti1 O21 C22 -57.59(14) . . . . ? O21 Ti1 O21 C22 -171.31(16) 2_557 . . . ? O11 Ti1 O21 C22 51.60(13) . . . . ? Ti1 Ti1 O21 C22 -171.31(16) 2_557 . . . ? O41B Ti1 O21 Ti1 -67(3) . . . 2_557 ? O41A Ti1 O21 Ti1 -58(3) . . . 2_557 ? O31 Ti1 O21 Ti1 113.72(7) . . . 2_557 ? O21 Ti1 O21 Ti1 0.0 2_557 . . 2_557 ? O11 Ti1 O21 Ti1 -137.10(7) . . . 2_557 ? O41B Ti1 O31 C32B -4.7(14) . . . . ? O41A Ti1 O31 C32B -6.9(13) . . . . ? O21 Ti1 O31 C32B -112.3(11) 2_557 . . . ? O11 Ti1 O31 C32B 91.0(11) . . . . ? O21 Ti1 O31 C32B 175.0(11) . . . . ? Ti1 Ti1 O31 C32B -152.3(11) 2_557 . . . ? O41B Ti1 O31 C32A -2.6(10) . . . . ? O41A Ti1 O31 C32A -4.8(8) . . . . ? O21 Ti1 O31 C32A -110.3(5) 2_557 . . . ? O11 Ti1 O31 C32A 93.0(5) . . . . ? O21 Ti1 O31 C32A 177.1(5) . . . . ? Ti1 Ti1 O31 C32A -150.2(5) 2_557 . . . ? C5 Cr1 C2 O2 45(14) . . . . ? C4 Cr1 C2 O2 -45(14) . . . . ? C6 Cr1 C2 O2 136(14) . . . . ? C3 Cr1 C2 O2 -136(14) . . . . ? C11 Cr1 C2 O2 -43(17) . . . . ? C5 Cr1 C3 O3 45(10) . . . . ? C4 Cr1 C3 O3 163(8) . . . . ? C2 Cr1 C3 O3 -106(8) . . . . ? C6 Cr1 C3 O3 -13(8) . . . . ? C11 Cr1 C3 O3 76(8) . . . . ? C5 Cr1 C4 O4 55(6) . . . . ? C2 Cr1 C4 O4 144(6) . . . . ? C6 Cr1 C4 O4 -48(7) . . . . ? C3 Cr1 C4 O4 -124(6) . . . . ? C11 Cr1 C4 O4 -36(6) . . . . ? C4 Cr1 C5 O5 42(17) . . . . ? C2 Cr1 C5 O5 -49(17) . . . . ? C6 Cr1 C5 O5 -142(17) . . . . ? C3 Cr1 C5 O5 160(16) . . . . ? C11 Cr1 C5 O5 130(17) . . . . ? C5 Cr1 C6 O6 -170(6) . . . . ? C4 Cr1 C6 O6 -67(7) . . . . ? C2 Cr1 C6 O6 101(6) . . . . ? C3 Cr1 C6 O6 8(6) . . . . ? C11 Cr1 C6 O6 -79(6) . . . . ? Ti1 O11 C11 C12 -7.4(3) . . . . ? Ti1 O11 C11 Cr1 170.57(9) . . . . ? C5 Cr1 C11 O11 149.56(16) . . . . ? C4 Cr1 C11 O11 -120.47(17) . . . . ? C2 Cr1 C11 O11 -122(5) . . . . ? C6 Cr1 C11 O11 58.66(16) . . . . ? C3 Cr1 C11 O11 -29.63(17) . . . . ? C5 Cr1 C11 C12 -32.7(2) . . . . ? C4 Cr1 C11 C12 57.27(19) . . . . ? C2 Cr1 C11 C12 55(5) . . . . ? C6 Cr1 C11 C12 -123.60(19) . . . . ? C3 Cr1 C11 C12 148.12(19) . . . . ? Ti1 O21 C22 C23 61.3(2) 2_557 . . . ? Ti1 O21 C22 C23 -130.12(16) . . . . ? Ti1 O21 C22 C24 -64.7(2) 2_557 . . . ? Ti1 O21 C22 C24 103.87(18) . . . . ? C32B O31 C32A C34A 98(13) . . . . ? Ti1 O31 C32A C34A 81.7(6) . . . . ? C32B O31 C32A C33A -140(13) . . . . ? Ti1 O31 C32A C33A -156.7(5) . . . . ? C32A O31 C32B C34B -16(12) . . . . ? Ti1 O31 C32B C34B 149.1(19) . . . . ? C32A O31 C32B C33B 114(14) . . . . ? Ti1 O31 C32B C33B -80(2) . . . . ? O41B Ti1 O41A C42A -70(16) . . . . ? O31 Ti1 O41A C42A 84(4) . . . . ? O21 Ti1 O41A C42A -160(4) 2_557 . . . ? O11 Ti1 O41A C42A -26(4) . . . . ? O21 Ti1 O41A C42A -104(4) . . . . ? Ti1 Ti1 O41A C42A -149(3) 2_557 . . . ? Ti1 O41A C42A C43A -78(4) . . . . ? Ti1 O41A C42A C44A 80(4) . . . . ? O41A Ti1 O41B C42B 93(36) . . . . ? O31 Ti1 O41B C42B 66(31) . . . . ? O21 Ti1 O41B C42B -176(31) 2_557 . . . ? O11 Ti1 O41B C42B -44(31) . . . . ? O21 Ti1 O41B C42B -113(30) . . . . ? Ti1 Ti1 O41B C42B -162(30) 2_557 . . . ? Ti1 O41B C42B C43B -94(31) . . . . ? Ti1 O41B C42B C44B 44(31) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.352 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.049 #===END data_[{(OC)5W=C(Me)OTi(OiPr)2}(OiPr)]2 _database_code_depnum_ccdc_archive 'CCDC 670774' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H48 O18 Ti2 W2' _chemical_formula_sum 'C32 H48 O18 Ti2 W2' _chemical_formula_weight 1184.20 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 9.6870(5) _cell_length_b 10.6893(6) _cell_length_c 11.7611(6) _cell_angle_alpha 108.787(1) _cell_angle_beta 107.558(1) _cell_angle_gamma 91.644(1) _cell_volume 1088.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4962 _cell_measurement_theta_min 26.77 _cell_measurement_theta_max 2.23 _exptl_crystal_description block _exptl_crystal_colour red _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 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 5.687 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4248 _exptl_absorpt_correction_T_max 0.6001 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6461 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.77 _reflns_number_total 4503 _reflns_number_gt 4311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXS-97 (Sheldrick, 1997)' _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. Although PLATON geometry checks suggest that HFIX 33 was used to generate hydrogen atoms at C12 we used HFIX 137. They refined to their current position and difference map checks did not show any ambiguities. ; _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^)+(0.0326P)^2^+2.5027P] 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 4503 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0627 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 W1 W 0.274353(15) 0.265491(14) 0.543583(13) 0.01866(6) Uani 1 1 d . . . C3 C 0.0625(4) 0.3043(4) 0.4921(4) 0.0264(8) Uani 1 1 d . . . O3 O -0.0551(3) 0.3257(4) 0.4614(3) 0.0403(8) Uani 1 1 d . . . Ti1 Ti 0.00769(7) 0.15392(6) 0.08043(6) 0.01521(13) Uani 1 1 d . . . O4 O 0.1704(4) -0.0197(3) 0.5447(3) 0.0373(7) Uani 1 1 d . . . C4 C 0.2059(4) 0.0822(4) 0.5427(4) 0.0239(8) Uani 1 1 d . . . C5 C 0.4813(4) 0.2182(4) 0.5827(4) 0.0248(8) Uani 1 1 d . . . O5 O 0.5962(3) 0.1886(3) 0.6049(3) 0.0376(7) Uani 1 1 d . . . C6 C 0.3432(4) 0.4496(4) 0.5461(4) 0.0238(8) Uani 1 1 d . . . O6 O 0.3797(4) 0.5537(3) 0.5494(3) 0.0345(7) Uani 1 1 d . . . C2 C 0.2996(4) 0.3512(4) 0.7306(4) 0.0230(8) Uani 1 1 d . . . O2 O 0.3137(3) 0.4031(3) 0.8358(3) 0.0309(6) Uani 1 1 d . . . O11 O 0.1234(3) 0.1888(3) 0.2566(3) 0.0259(6) Uani 1 1 d . . . C11 C 0.2407(4) 0.1829(4) 0.3394(4) 0.0208(7) Uani 1 1 d . . . C12 C 0.3534(5) 0.1188(5) 0.2822(4) 0.0312(9) Uani 1 1 d . . . H12A H 0.3128 0.0892 0.1893 0.047 Uiso 1 1 calc R . . H12B H 0.3789 0.0419 0.3084 0.047 Uiso 1 1 calc R . . H12C H 0.4412 0.1839 0.3121 0.047 Uiso 1 1 calc R . . O41 O 0.0803(3) 0.3113(3) 0.0902(3) 0.0264(6) Uani 1 1 d . . . C41 C 0.1530(6) 0.4454(5) 0.1498(6) 0.0508(15) Uani 1 1 d . . . H41 H 0.1193 0.4902 0.0856 0.061 Uiso 1 1 calc R . . C42 C 0.3075(6) 0.4494(6) 0.1776(6) 0.0583(16) Uani 1 1 d . . . H42A H 0.3455 0.4035 0.2381 0.088 Uiso 1 1 calc R . . H42B H 0.3542 0.5425 0.2146 0.088 Uiso 1 1 calc R . . H42C H 0.3288 0.4049 0.0990 0.088 Uiso 1 1 calc R . . C43 C 0.0995(5) 0.5165(4) 0.2586(4) 0.0334(10) Uani 1 1 d . . . H43A H -0.0044 0.5242 0.2251 0.050 Uiso 1 1 calc R . . H43B H 0.1556 0.6058 0.3050 0.050 Uiso 1 1 calc R . . H43C H 0.1124 0.4656 0.3162 0.050 Uiso 1 1 calc R . . O31 O -0.1766(3) 0.1726(3) 0.0685(3) 0.0222(5) Uani 1 1 d . . . C31 C -0.2743(4) 0.2711(4) 0.0718(4) 0.0285(9) Uani 1 1 d . . . H31 H -0.2154 0.3617 0.1091 0.034 Uiso 1 1 calc R . . C32 C -0.3602(6) 0.2598(6) 0.1554(5) 0.0485(13) Uani 1 1 d . . . H32A H -0.4159 0.1702 0.1210 0.073 Uiso 1 1 calc R . . H32B H -0.4277 0.3264 0.1586 0.073 Uiso 1 1 calc R . . H32C H -0.2932 0.2753 0.2414 0.073 Uiso 1 1 calc R . . C33 C -0.3682(7) 0.2502(8) -0.0612(6) 0.067(2) Uani 1 1 d . . . H33A H -0.3062 0.2503 -0.1133 0.100 Uiso 1 1 calc R . . H33B H -0.4285 0.3223 -0.0611 0.100 Uiso 1 1 calc R . . H33C H -0.4316 0.1644 -0.0964 0.100 Uiso 1 1 calc R . . O21 O -0.0250(3) -0.0419(2) 0.0774(2) 0.0165(5) Uani 1 1 d . . . C21 C -0.0780(4) -0.0700(4) 0.1721(4) 0.0206(7) Uani 1 1 d . . . H21 H -0.0601 0.0150 0.2458 0.025 Uiso 1 1 calc R . . C22 C 0.0079(5) -0.1693(4) 0.2194(4) 0.0263(8) Uani 1 1 d . . . H22A H 0.1126 -0.1356 0.2515 0.039 Uiso 1 1 calc R . . H22B H -0.0112 -0.2547 0.1494 0.039 Uiso 1 1 calc R . . H22C H -0.0217 -0.1819 0.2880 0.039 Uiso 1 1 calc R . . C23 C -0.2409(4) -0.1145(4) 0.1153(4) 0.0256(8) Uani 1 1 d . . . H23A H -0.2610 -0.1995 0.0445 0.038 Uiso 1 1 calc R . . H23B H -0.2890 -0.0469 0.0840 0.038 Uiso 1 1 calc R . . H23C H -0.2785 -0.1260 0.1804 0.038 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 W1 0.01809(9) 0.02014(9) 0.01531(9) 0.00432(6) 0.00409(6) 0.00220(6) C3 0.027(2) 0.029(2) 0.0200(19) 0.0047(16) 0.0066(16) 0.0015(16) O3 0.0249(16) 0.051(2) 0.0417(19) 0.0119(16) 0.0097(14) 0.0125(14) Ti1 0.0161(3) 0.0145(3) 0.0143(3) 0.0036(2) 0.0053(2) 0.0028(2) O4 0.049(2) 0.0304(17) 0.0325(17) 0.0094(14) 0.0163(15) -0.0006(14) C4 0.0264(19) 0.027(2) 0.0170(18) 0.0049(15) 0.0078(15) 0.0033(16) C5 0.025(2) 0.025(2) 0.0180(18) 0.0030(15) 0.0038(15) 0.0027(16) O5 0.0266(16) 0.0425(19) 0.0358(18) 0.0084(15) 0.0044(13) 0.0097(14) C6 0.0241(18) 0.027(2) 0.0180(18) 0.0046(15) 0.0070(15) 0.0041(16) O6 0.0378(17) 0.0288(17) 0.0387(18) 0.0111(13) 0.0160(14) 0.0028(13) C2 0.0235(18) 0.0221(19) 0.019(2) 0.0058(15) 0.0029(15) 0.0049(15) O2 0.0446(18) 0.0263(15) 0.0206(15) 0.0055(12) 0.0111(13) 0.0111(13) O11 0.0281(14) 0.0241(14) 0.0197(14) 0.0054(11) 0.0021(11) 0.0025(11) C11 0.0229(18) 0.0148(17) 0.0213(18) 0.0055(14) 0.0036(15) -0.0014(14) C12 0.032(2) 0.040(2) 0.023(2) 0.0091(18) 0.0125(17) 0.0113(18) O41 0.0348(15) 0.0174(13) 0.0245(14) 0.0005(11) 0.0140(12) -0.0025(11) C41 0.055(3) 0.024(2) 0.067(4) -0.008(2) 0.037(3) -0.013(2) C42 0.044(3) 0.045(3) 0.065(4) -0.007(3) 0.018(3) -0.008(2) C43 0.036(2) 0.020(2) 0.037(2) -0.0008(17) 0.0130(19) 0.0017(17) O31 0.0191(12) 0.0208(13) 0.0272(14) 0.0075(11) 0.0086(11) 0.0081(10) C31 0.0226(19) 0.025(2) 0.038(2) 0.0090(17) 0.0119(17) 0.0118(16) C32 0.047(3) 0.066(4) 0.047(3) 0.021(3) 0.031(2) 0.032(3) C33 0.059(4) 0.104(5) 0.047(3) 0.035(4) 0.019(3) 0.058(4) O21 0.0216(12) 0.0153(12) 0.0155(12) 0.0062(10) 0.0094(10) 0.0044(10) C21 0.0247(18) 0.0237(18) 0.0192(18) 0.0107(15) 0.0120(15) 0.0034(15) C22 0.032(2) 0.028(2) 0.023(2) 0.0146(16) 0.0098(16) 0.0076(17) C23 0.0259(19) 0.026(2) 0.029(2) 0.0106(16) 0.0133(16) 0.0031(16) _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 W1 C2 2.025(4) . ? W1 C5 2.034(4) . ? W1 C4 2.046(4) . ? W1 C6 2.047(4) . ? W1 C3 2.052(4) . ? W1 C11 2.190(4) . ? C3 O3 1.140(5) . ? Ti1 O41 1.760(3) . ? Ti1 O31 1.770(3) . ? Ti1 O21 1.917(2) 2 ? Ti1 O11 1.941(3) . ? Ti1 O21 2.095(2) . ? Ti1 Ti1 3.1971(12) 2 ? O4 C4 1.142(5) . ? C5 O5 1.142(5) . ? C6 O6 1.144(5) . ? C2 O2 1.145(5) . ? O11 C11 1.273(5) . ? C11 C12 1.518(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O41 C41 1.427(5) . ? C41 C42 1.429(8) . ? C41 C43 1.509(6) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? O31 C31 1.435(4) . ? C31 C33 1.493(7) . ? C31 C32 1.496(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 . ? O21 C21 1.465(4) . ? O21 Ti1 1.917(2) 2 ? C21 C23 1.510(5) . ? C21 C22 1.510(5) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 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 C2 W1 C5 92.10(15) . . ? C2 W1 C4 91.62(15) . . ? C5 W1 C4 88.00(16) . . ? C2 W1 C6 87.88(15) . . ? C5 W1 C6 91.99(16) . . ? C4 W1 C6 179.50(14) . . ? C2 W1 C3 91.55(16) . . ? C5 W1 C3 176.20(15) . . ? C4 W1 C3 90.85(16) . . ? C6 W1 C3 89.19(16) . . ? C2 W1 C11 176.58(14) . . ? C5 W1 C11 90.37(15) . . ? C4 W1 C11 90.82(14) . . ? C6 W1 C11 89.68(14) . . ? C3 W1 C11 86.02(15) . . ? O3 C3 W1 178.8(4) . . ? O41 Ti1 O31 102.87(13) . . ? O41 Ti1 O21 101.20(11) . 2 ? O31 Ti1 O21 111.92(12) . 2 ? O41 Ti1 O11 90.37(13) . . ? O31 Ti1 O11 109.71(13) . . ? O21 Ti1 O11 132.71(12) 2 . ? O41 Ti1 O21 165.84(12) . . ? O31 Ti1 O21 91.20(11) . . ? O21 Ti1 O21 74.43(11) 2 . ? O11 Ti1 O21 83.33(11) . . ? O41 Ti1 Ti1 138.75(10) . 2 ? O31 Ti1 Ti1 103.75(9) . 2 ? O21 Ti1 Ti1 39.14(7) 2 2 ? O11 Ti1 Ti1 109.31(9) . 2 ? O21 Ti1 Ti1 35.29(6) . 2 ? O4 C4 W1 178.4(4) . . ? O5 C5 W1 178.2(4) . . ? O6 C6 W1 178.4(3) . . ? O2 C2 W1 178.1(3) . . ? C11 O11 Ti1 150.2(3) . . ? O11 C11 C12 113.3(3) . . ? O11 C11 W1 122.0(3) . . ? C12 C11 W1 124.6(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C41 O41 Ti1 157.3(3) . . ? O41 C41 C42 111.1(5) . . ? O41 C41 C43 109.1(4) . . ? C42 C41 C43 117.1(5) . . ? O41 C41 H41 106.3 . . ? C42 C41 H41 106.3 . . ? C43 C41 H41 106.3 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C31 O31 Ti1 141.2(3) . . ? O31 C31 C33 108.6(4) . . ? O31 C31 C32 108.4(4) . . ? C33 C31 C32 113.1(4) . . ? O31 C31 H31 108.9 . . ? C33 C31 H31 108.9 . . ? C32 C31 H31 108.9 . . ? 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 . . ? C21 O21 Ti1 132.7(2) . 2 ? C21 O21 Ti1 120.7(2) . . ? Ti1 O21 Ti1 105.57(11) 2 . ? O21 C21 C23 109.0(3) . . ? O21 C21 C22 109.6(3) . . ? C23 C21 C22 114.0(3) . . ? O21 C21 H21 108.0 . . ? C23 C21 H21 108.0 . . ? C22 C21 H21 108.0 . . ? 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 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 W1 C3 O3 160(19) . . . . ? C5 W1 C3 O3 -36(20) . . . . ? C4 W1 C3 O3 -109(19) . . . . ? C6 W1 C3 O3 72(19) . . . . ? C11 W1 C3 O3 -18(19) . . . . ? C2 W1 C4 O4 -49(13) . . . . ? C5 W1 C4 O4 43(13) . . . . ? C6 W1 C4 O4 -45(25) . . . . ? C3 W1 C4 O4 -140(13) . . . . ? C11 W1 C4 O4 134(13) . . . . ? C2 W1 C5 O5 88(12) . . . . ? C4 W1 C5 O5 -4(12) . . . . ? C6 W1 C5 O5 176(100) . . . . ? C3 W1 C5 O5 -76(12) . . . . ? C11 W1 C5 O5 -94(12) . . . . ? C2 W1 C6 O6 -41(13) . . . . ? C5 W1 C6 O6 -133(13) . . . . ? C4 W1 C6 O6 -44(25) . . . . ? C3 W1 C6 O6 51(13) . . . . ? C11 W1 C6 O6 137(13) . . . . ? C5 W1 C2 O2 113(10) . . . . ? C4 W1 C2 O2 -159(10) . . . . ? C6 W1 C2 O2 21(10) . . . . ? C3 W1 C2 O2 -68(10) . . . . ? C11 W1 C2 O2 -23(12) . . . . ? O41 Ti1 O11 C11 -90.4(5) . . . . ? O31 Ti1 O11 C11 165.8(5) . . . . ? O21 Ti1 O11 C11 15.3(6) 2 . . . ? O21 Ti1 O11 C11 76.9(5) . . . . ? Ti1 Ti1 O11 C11 52.6(5) 2 . . . ? Ti1 O11 C11 C12 0.2(7) . . . . ? Ti1 O11 C11 W1 178.0(3) . . . . ? C2 W1 C11 O11 -40(2) . . . . ? C5 W1 C11 O11 -176.4(3) . . . . ? C4 W1 C11 O11 95.6(3) . . . . ? C6 W1 C11 O11 -84.4(3) . . . . ? C3 W1 C11 O11 4.8(3) . . . . ? C2 W1 C11 C12 137(2) . . . . ? C5 W1 C11 C12 1.2(3) . . . . ? C4 W1 C11 C12 -86.8(3) . . . . ? C6 W1 C11 C12 93.2(3) . . . . ? C3 W1 C11 C12 -177.6(3) . . . . ? O31 Ti1 O41 C41 93.2(8) . . . . ? O21 Ti1 O41 C41 -151.0(8) 2 . . . ? O11 Ti1 O41 C41 -17.2(8) . . . . ? O21 Ti1 O41 C41 -80.5(9) . . . . ? Ti1 Ti1 O41 C41 -137.7(8) 2 . . . ? Ti1 O41 C41 C42 87.1(8) . . . . ? Ti1 O41 C41 C43 -43.4(11) . . . . ? O41 Ti1 O31 C31 -4.8(4) . . . . ? O21 Ti1 O31 C31 -112.7(4) 2 . . . ? O11 Ti1 O31 C31 90.3(4) . . . . ? O21 Ti1 O31 C31 173.6(4) . . . . ? Ti1 Ti1 O31 C31 -153.0(4) 2 . . . ? Ti1 O31 C31 C33 102.7(5) . . . . ? Ti1 O31 C31 C32 -134.1(4) . . . . ? O41 Ti1 O21 C21 116.6(5) . . . . ? O31 Ti1 O21 C21 -57.2(2) . . . . ? O21 Ti1 O21 C21 -169.6(3) 2 . . . ? O11 Ti1 O21 C21 52.5(2) . . . . ? Ti1 Ti1 O21 C21 -169.6(3) 2 . . . ? O41 Ti1 O21 Ti1 -73.7(5) . . . 2 ? O31 Ti1 O21 Ti1 112.44(13) . . . 2 ? O21 Ti1 O21 Ti1 0.0 2 . . 2 ? O11 Ti1 O21 Ti1 -137.86(14) . . . 2 ? Ti1 O21 C21 C23 -68.4(4) 2 . . . ? Ti1 O21 C21 C23 98.0(3) . . . . ? Ti1 O21 C21 C22 57.1(4) 2 . . . ? Ti1 O21 C21 C22 -136.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.77 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.352 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.126 #===END data_(OC)5Cr=C(Me)OTi(OiPr)3(C5H5N)2 _database_code_depnum_ccdc_archive 'CCDC 670775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 Cr2 N2 O14 Ti' _chemical_formula_sum 'C30 H30 Cr2 N2 O14 Ti' _chemical_formula_weight 794.46 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 23.5279(14) _cell_length_b 15.4230(10) _cell_length_c 14.9208(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.695(2) _cell_angle_gamma 90.00 _cell_volume 5320.3(5) _cell_formula_units_Z 6 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 9446 _cell_measurement_theta_min 26.75 _cell_measurement_theta_max 2.20 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2436 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7401 _exptl_absorpt_correction_T_max 0.9164 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29084 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.68 _reflns_number_total 10099 _reflns_number_gt 8276 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One isopropoxide group (on O241) of the complete formula unit is disordered. PART instructions and similarity restraints (SAME-instruction in Shelxl) were applied to model the disorder as best as possible. ; _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^)+(0.0560P)^2^+1.9762P] 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 10099 _refine_ls_number_parameters 702 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Cr1 Cr 0.295364(16) 0.25387(2) 0.64891(3) 0.02274(10) Uani 1 1 d . . . Ti1 Ti 0.5000 0.20965(3) 0.7500 0.01676(13) Uani 1 2 d S . . Cr2 Cr 0.369765(15) 0.26283(2) 0.26795(2) 0.01941(10) Uani 1 1 d . . . Ti2 Ti 0.170961(17) 0.28976(3) 0.08337(3) 0.02021(11) Uani 1 1 d . A . Cr3 Cr -0.031104(17) 0.22388(4) -0.04691(3) 0.04274(14) Uani 1 1 d . . . O11 O 0.26210(7) 0.06374(12) 0.65401(12) 0.0329(4) Uani 1 1 d . . . C11 C 0.27332(9) 0.13577(16) 0.65204(15) 0.0242(5) Uani 1 1 d . . . O12 O 0.34563(8) 0.24557(12) 0.85249(13) 0.0364(4) Uani 1 1 d . . . C12 C 0.32672(10) 0.24958(16) 0.77673(18) 0.0263(5) Uani 1 1 d . . . O13 O 0.34652(8) 0.43265(12) 0.63182(12) 0.0366(4) Uani 1 1 d . . . C13 C 0.32631(10) 0.36638(16) 0.63899(16) 0.0275(5) Uani 1 1 d . . . O14 O 0.24336(8) 0.26067(13) 0.44703(13) 0.0402(5) Uani 1 1 d . . . C14 C 0.26407(11) 0.25735(16) 0.52276(18) 0.0282(5) Uani 1 1 d . . . O15 O 0.18289(8) 0.32247(14) 0.69222(14) 0.0464(5) Uani 1 1 d . . . C15 C 0.22540(11) 0.29643(17) 0.67477(18) 0.0320(6) Uani 1 1 d . . . O16 O 0.42132(6) 0.23443(10) 0.68142(10) 0.0205(3) Uani 1 1 d . . . C16 C 0.37474(10) 0.21057(14) 0.62963(15) 0.0215(5) Uani 1 1 d . . . C17 C 0.38351(10) 0.14767(16) 0.55575(16) 0.0273(5) Uani 1 1 d . . . H17A H 0.3789 0.1782 0.4973 0.041 Uiso 1 1 calc R . . H17B H 0.3548 0.1010 0.5515 0.041 Uiso 1 1 calc R . . H17C H 0.4225 0.1230 0.5706 0.041 Uiso 1 1 calc R . . O21 O 0.29869(7) 0.11766(11) 0.32929(13) 0.0345(4) Uani 1 1 d . . . C21 C 0.32584(10) 0.17196(15) 0.30723(16) 0.0243(5) Uani 1 1 d . . . O22 O 0.37135(8) 0.16326(16) 0.09270(14) 0.0536(6) Uani 1 1 d . . . C22 C 0.37048(10) 0.20133(18) 0.15714(18) 0.0321(6) Uani 1 1 d . . . O23 O 0.43136(8) 0.41108(12) 0.19115(12) 0.0348(4) Uani 1 1 d . . . C23 C 0.40788(10) 0.35577(16) 0.22013(15) 0.0245(5) Uani 1 1 d . . . O24 O 0.36791(8) 0.36426(12) 0.44172(12) 0.0344(4) Uani 1 1 d . . . C24 C 0.36796(10) 0.32621(15) 0.37606(16) 0.0231(5) Uani 1 1 d . . . O25 O 0.48367(7) 0.18257(12) 0.35743(13) 0.0384(4) Uani 1 1 d . . . C25 C 0.44071(10) 0.21281(16) 0.32301(16) 0.0262(5) Uani 1 1 d . . . O26 O 0.25131(6) 0.27169(10) 0.15875(10) 0.0211(3) Uani 1 1 d . . . C26 C 0.29043(9) 0.31546(15) 0.20961(15) 0.0201(5) Uani 1 1 d . . . C27 C 0.27347(10) 0.40669(16) 0.22780(17) 0.0283(5) Uani 1 1 d . . . H27A H 0.2490 0.4304 0.1729 0.042 Uiso 1 1 calc R . . H27B H 0.3083 0.4424 0.2442 0.042 Uiso 1 1 calc R . . H27C H 0.2520 0.4069 0.2782 0.042 Uiso 1 1 calc R . . O31 O -0.08455(13) 0.3907(2) 0.00517(18) 0.0907(10) Uani 1 1 d . . . C31 C -0.06497(13) 0.3279(3) -0.0152(2) 0.0557(9) Uani 1 1 d . . . O32 O -0.06589(9) 0.2705(2) -0.24772(16) 0.0868(10) Uani 1 1 d . . . C32 C -0.05190(12) 0.2534(3) -0.1725(2) 0.0611(11) Uani 1 1 d . . . O33 O 0.03761(10) 0.06952(19) -0.0939(2) 0.0894(11) Uani 1 1 d . . . C33 C 0.01070(12) 0.1273(3) -0.0773(2) 0.0598(10) Uani 1 1 d . . . O34 O 0.00044(10) 0.17661(19) 0.15358(17) 0.0708(8) Uani 1 1 d . . . C34 C -0.01090(12) 0.1945(2) 0.0788(2) 0.0449(8) Uani 1 1 d . . . O35 O -0.14361(9) 0.1276(2) -0.05425(18) 0.0823(9) Uani 1 1 d . . . C35 C -0.10080(13) 0.1641(3) -0.0530(2) 0.0618(11) Uani 1 1 d . . . O36 O 0.09347(7) 0.25876(11) 0.00988(12) 0.0305(4) Uani 1 1 d . . . C36 C 0.04634(11) 0.29076(19) -0.03275(18) 0.0362(6) Uani 1 1 d . . . C37 C 0.05219(13) 0.3815(2) -0.0673(2) 0.0588(9) Uani 1 1 d . . . H37A H 0.0880 0.3861 -0.0916 0.088 Uiso 1 1 calc R . . H37B H 0.0533 0.4228 -0.0171 0.088 Uiso 1 1 calc R . . H37C H 0.0191 0.3946 -0.1157 0.088 Uiso 1 1 calc R . . N111 N 0.47887(8) 0.31895(12) 0.84353(12) 0.0190(4) Uani 1 1 d . . . C112 C 0.48960(10) 0.30499(15) 0.93384(16) 0.0257(5) Uani 1 1 d . . . H112 H 0.5105 0.2544 0.9563 0.031 Uiso 1 1 calc R . . C113 C 0.47181(10) 0.36045(16) 0.99578(16) 0.0281(5) Uani 1 1 d . . . H113 H 0.4806 0.3482 1.0593 0.034 Uiso 1 1 calc R . . C114 C 0.44101(10) 0.43407(16) 0.96401(16) 0.0279(5) Uani 1 1 d . . . H114 H 0.4279 0.4731 1.0050 0.034 Uiso 1 1 calc R . . C115 C 0.42985(10) 0.44937(15) 0.87135(16) 0.0267(5) Uani 1 1 d . . . H115 H 0.4091 0.4997 0.8475 0.032 Uiso 1 1 calc R . . C116 C 0.44908(9) 0.39102(14) 0.81343(16) 0.0218(5) Uani 1 1 d . . . H116 H 0.4410 0.4022 0.7497 0.026 Uiso 1 1 calc R . . O121 O 0.47624(7) 0.13531(10) 0.82544(11) 0.0246(4) Uani 1 1 d . . . C122 C 0.45680(10) 0.05307(15) 0.85061(17) 0.0283(5) Uani 1 1 d . . . H122 H 0.4904 0.0122 0.8606 0.034 Uiso 1 1 calc R . . C123 C 0.43450(13) 0.0617(2) 0.9385(2) 0.0474(8) Uani 1 1 d . . . H12D H 0.4650 0.0856 0.9857 0.071 Uiso 1 1 calc R . . H12E H 0.4231 0.0045 0.9576 0.071 Uiso 1 1 calc R . . H12F H 0.4010 0.1005 0.9292 0.071 Uiso 1 1 calc R . . C124 C 0.41151(12) 0.01882(18) 0.7732(2) 0.0418(7) Uani 1 1 d . . . H12A H 0.3787 0.0590 0.7616 0.063 Uiso 1 1 calc R . . H12B H 0.3982 -0.0382 0.7897 0.063 Uiso 1 1 calc R . . H12C H 0.4283 0.0134 0.7181 0.063 Uiso 1 1 calc R . . N212 N 0.15434(8) 0.17197(13) 0.16610(15) 0.0280(5) Uani 1 1 d . . . C213 C 0.16656(11) 0.17836(18) 0.25741(19) 0.0334(6) Uani 1 1 d . . . H213 H 0.1884 0.2269 0.2836 0.040 Uiso 1 1 calc R . . C214 C 0.14909(12) 0.1182(2) 0.3152(2) 0.0469(8) Uani 1 1 d . . . H214 H 0.1588 0.1254 0.3795 0.056 Uiso 1 1 calc R . . C215 C 0.11751(13) 0.0480(2) 0.2784(3) 0.0573(10) Uani 1 1 d . . . H215 H 0.1039 0.0065 0.3164 0.069 Uiso 1 1 calc R . . C216 C 0.10598(12) 0.03881(18) 0.1855(3) 0.0544(9) Uani 1 1 d . . . H216 H 0.0852 -0.0104 0.1586 0.065 Uiso 1 1 calc R . . C217 C 0.12471(11) 0.10140(17) 0.1304(2) 0.0402(7) Uani 1 1 d . . . H217 H 0.1164 0.0942 0.0660 0.048 Uiso 1 1 calc R . . N221 N 0.19899(8) 0.18700(12) -0.00780(13) 0.0232(4) Uani 1 1 d . . . C222 C 0.23599(10) 0.12258(15) 0.02216(17) 0.0255(5) Uani 1 1 d . . . H222 H 0.2492 0.1164 0.0860 0.031 Uiso 1 1 calc R . . C223 C 0.25559(11) 0.06499(16) -0.03573(18) 0.0310(6) Uani 1 1 d . . . H223 H 0.2819 0.0204 -0.0119 0.037 Uiso 1 1 calc R . . C224 C 0.23675(11) 0.07255(16) -0.12851(17) 0.0306(6) Uani 1 1 d . . . H224 H 0.2496 0.0333 -0.1696 0.037 Uiso 1 1 calc R . . C225 C 0.19860(10) 0.13878(16) -0.16038(17) 0.0279(5) Uani 1 1 d . . . H225 H 0.1848 0.1459 -0.2239 0.033 Uiso 1 1 calc R . . C226 C 0.18088(10) 0.19426(15) -0.09853(16) 0.0257(5) Uani 1 1 d . . . H226 H 0.1548 0.2396 -0.1209 0.031 Uiso 1 1 calc R . . O231 O 0.19406(7) 0.36794(10) 0.01175(10) 0.0246(4) Uani 1 1 d . . . C232 C 0.22364(11) 0.41518(17) -0.04754(18) 0.0335(6) Uani 1 1 d D . . H232 H 0.2073 0.3983 -0.1119 0.040 Uiso 1 1 calc R . . C233 C 0.28697(12) 0.3920(2) -0.0274(2) 0.0498(8) Uani 1 1 d D . . H23A H 0.3040 0.4109 0.0344 0.075 Uiso 1 1 calc R . . H23B H 0.3068 0.4209 -0.0714 0.075 Uiso 1 1 calc R . . H23C H 0.2913 0.3290 -0.0322 0.075 Uiso 1 1 calc R . . C234 C 0.21286(13) 0.51078(17) -0.0362(2) 0.0405(7) Uani 1 1 d D . . H23D H 0.1713 0.5226 -0.0526 0.061 Uiso 1 1 calc R . . H23E H 0.2335 0.5442 -0.0760 0.061 Uiso 1 1 calc R . . H23F H 0.2268 0.5276 0.0275 0.061 Uiso 1 1 calc R . . O241 O 0.14002(7) 0.35348(10) 0.16002(11) 0.0258(4) Uani 1 1 d . . . C24A C 0.0952(3) 0.3992(3) 0.1919(4) 0.0314(13) Uani 0.646(10) 1 d PD A 1 H24H H 0.0579 0.3913 0.1479 0.038 Uiso 0.646(10) 1 calc PR A 1 C24B C 0.0892(3) 0.3635(3) 0.2836(4) 0.0445(16) Uani 0.646(10) 1 d PD A 1 H24D H 0.0769 0.3027 0.2770 0.067 Uiso 0.646(10) 1 calc PR A 1 H24C H 0.0603 0.3972 0.3082 0.067 Uiso 0.646(10) 1 calc PR A 1 H24B H 0.1265 0.3672 0.3255 0.067 Uiso 0.646(10) 1 calc PR A 1 C24C C 0.1110(6) 0.4933(5) 0.1976(12) 0.074(5) Uani 0.646(10) 1 d PD A 1 H24E H 0.1464 0.5014 0.2432 0.111 Uiso 0.646(10) 1 calc PR A 1 H24G H 0.0795 0.5268 0.2152 0.111 Uiso 0.646(10) 1 calc PR A 1 H24F H 0.1176 0.5133 0.1380 0.111 Uiso 0.646(10) 1 calc PR A 1 C24D C 0.1176(4) 0.3951(6) 0.2357(8) 0.037(3) Uani 0.354(10) 1 d PD A 2 H24A H 0.1440 0.3846 0.2954 0.045 Uiso 0.354(10) 1 calc PR A 2 C24E C 0.0591(4) 0.3544(7) 0.2340(8) 0.053(3) Uani 0.354(10) 1 d PD A 2 H24I H 0.0356 0.3600 0.1728 0.080 Uiso 0.354(10) 1 calc PR A 2 H24K H 0.0397 0.3840 0.2781 0.080 Uiso 0.354(10) 1 calc PR A 2 H24J H 0.0639 0.2929 0.2501 0.080 Uiso 0.354(10) 1 calc PR A 2 C24F C 0.1110(10) 0.4917(8) 0.215(2) 0.057(6) Uani 0.354(10) 1 d PD A 2 H24N H 0.1459 0.5135 0.1957 0.086 Uiso 0.354(10) 1 calc PR A 2 H24M H 0.1052 0.5227 0.2701 0.086 Uiso 0.354(10) 1 calc PR A 2 H24L H 0.0774 0.5011 0.1663 0.086 Uiso 0.354(10) 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 Cr1 0.0187(2) 0.0234(2) 0.0249(2) -0.00169(15) 0.00102(15) 0.00229(14) Ti1 0.0173(3) 0.0134(3) 0.0189(3) 0.000 0.0018(2) 0.000 Cr2 0.01667(19) 0.0216(2) 0.0192(2) -0.00160(14) 0.00112(14) -0.00008(14) Ti2 0.0169(2) 0.0193(2) 0.0229(2) -0.00229(16) -0.00048(16) 0.00052(15) Cr3 0.0152(2) 0.0768(4) 0.0345(3) -0.0271(2) 0.00020(17) 0.0045(2) O11 0.0341(10) 0.0275(10) 0.0369(10) -0.0035(8) 0.0058(8) -0.0029(8) C11 0.0193(12) 0.0299(14) 0.0222(12) -0.0033(10) 0.0010(9) 0.0014(10) O12 0.0366(11) 0.0440(12) 0.0276(11) -0.0036(8) 0.0036(8) 0.0002(8) C12 0.0228(13) 0.0273(13) 0.0298(15) -0.0052(10) 0.0075(11) 0.0018(10) O13 0.0404(11) 0.0223(10) 0.0427(11) 0.0017(8) -0.0039(8) -0.0007(8) C13 0.0246(13) 0.0276(14) 0.0271(13) -0.0023(10) -0.0034(10) 0.0078(10) O14 0.0417(11) 0.0437(12) 0.0309(11) -0.0021(8) -0.0048(9) 0.0038(9) C14 0.0260(13) 0.0272(13) 0.0306(15) -0.0027(10) 0.0031(11) 0.0023(10) O15 0.0306(11) 0.0490(13) 0.0615(14) -0.0051(10) 0.0137(9) 0.0106(9) C15 0.0295(14) 0.0300(14) 0.0347(15) -0.0008(11) 0.0015(11) 0.0019(11) O16 0.0179(8) 0.0184(8) 0.0234(8) -0.0006(6) -0.0004(6) -0.0006(6) C16 0.0244(12) 0.0193(12) 0.0205(12) 0.0035(9) 0.0037(9) -0.0010(9) C17 0.0251(12) 0.0277(13) 0.0285(13) -0.0069(10) 0.0032(10) -0.0015(10) O21 0.0323(10) 0.0236(10) 0.0472(11) 0.0026(8) 0.0060(8) -0.0032(8) C21 0.0222(12) 0.0210(12) 0.0278(13) -0.0038(10) 0.0002(10) 0.0043(10) O22 0.0345(11) 0.0841(17) 0.0416(12) -0.0331(12) 0.0050(9) 0.0004(10) C22 0.0172(12) 0.0443(16) 0.0333(15) -0.0127(12) 0.0006(10) 0.0021(11) O23 0.0376(10) 0.0358(11) 0.0341(10) 0.0021(8) 0.0149(8) -0.0047(8) C23 0.0218(12) 0.0315(14) 0.0202(12) -0.0029(10) 0.0036(9) 0.0020(10) O24 0.0470(11) 0.0322(10) 0.0251(9) -0.0073(8) 0.0095(8) -0.0112(8) C24 0.0213(12) 0.0223(12) 0.0250(13) 0.0030(10) 0.0024(9) -0.0046(9) O25 0.0254(10) 0.0435(12) 0.0414(11) -0.0027(9) -0.0064(8) 0.0079(8) C25 0.0252(13) 0.0275(13) 0.0247(13) -0.0041(10) 0.0017(10) -0.0026(10) O26 0.0174(8) 0.0219(8) 0.0228(8) -0.0002(6) 0.0006(6) -0.0023(6) C26 0.0204(11) 0.0238(12) 0.0169(11) 0.0029(9) 0.0053(9) 0.0002(9) C27 0.0239(12) 0.0256(13) 0.0331(14) -0.0042(10) -0.0005(10) -0.0009(10) O31 0.100(2) 0.109(2) 0.0661(17) 0.0027(16) 0.0225(15) 0.0740(19) C31 0.0429(18) 0.091(3) 0.0304(16) -0.0031(16) -0.0006(13) 0.0292(18) O32 0.0278(12) 0.198(3) 0.0335(14) -0.0244(16) 0.0023(10) -0.0061(15) C32 0.0149(14) 0.132(4) 0.0352(19) -0.0303(19) 0.0008(12) -0.0027(16) O33 0.0395(13) 0.098(2) 0.132(3) -0.084(2) 0.0209(14) -0.0076(13) C33 0.0219(15) 0.083(3) 0.074(2) -0.054(2) 0.0082(14) -0.0122(15) O34 0.0615(16) 0.102(2) 0.0490(15) 0.0021(14) 0.0112(12) 0.0392(15) C34 0.0244(14) 0.063(2) 0.0464(19) -0.0190(15) 0.0051(13) 0.0119(13) O35 0.0231(12) 0.140(3) 0.0832(19) -0.0388(18) 0.0090(11) -0.0174(14) C35 0.0235(16) 0.111(3) 0.050(2) -0.035(2) 0.0041(13) 0.0017(17) O36 0.0171(8) 0.0355(10) 0.0351(10) -0.0108(8) -0.0052(7) 0.0031(7) C36 0.0248(13) 0.0476(17) 0.0327(15) -0.0187(12) -0.0043(11) 0.0095(12) C37 0.0412(18) 0.054(2) 0.070(2) 0.0020(17) -0.0184(16) 0.0147(15) N111 0.0191(9) 0.0164(9) 0.0206(10) -0.0013(7) 0.0014(7) 0.0001(7) C112 0.0269(13) 0.0240(12) 0.0246(13) -0.0002(10) 0.0010(10) 0.0049(10) C113 0.0322(13) 0.0320(14) 0.0192(12) -0.0014(10) 0.0025(10) 0.0031(10) C114 0.0303(13) 0.0263(13) 0.0287(13) -0.0084(10) 0.0092(10) -0.0001(10) C115 0.0281(13) 0.0201(12) 0.0317(14) 0.0001(10) 0.0049(10) 0.0042(9) C116 0.0228(12) 0.0189(12) 0.0230(12) 0.0022(9) 0.0024(9) 0.0006(9) O121 0.0275(9) 0.0194(8) 0.0261(9) 0.0028(7) 0.0030(7) -0.0043(7) C122 0.0289(13) 0.0202(12) 0.0358(14) 0.0086(10) 0.0058(11) -0.0013(10) C123 0.0479(18) 0.055(2) 0.0432(17) 0.0209(14) 0.0199(14) 0.0029(15) C124 0.0413(16) 0.0272(15) 0.0526(18) 0.0063(12) -0.0022(13) -0.0126(12) N212 0.0163(10) 0.0226(11) 0.0446(13) 0.0005(9) 0.0046(9) 0.0006(8) C213 0.0254(13) 0.0330(15) 0.0430(16) 0.0097(12) 0.0093(11) 0.0045(11) C214 0.0374(16) 0.0455(19) 0.062(2) 0.0283(15) 0.0190(14) 0.0109(13) C215 0.0370(17) 0.0428(19) 0.098(3) 0.0345(19) 0.0290(18) 0.0091(14) C216 0.0246(15) 0.0227(15) 0.117(3) 0.0039(17) 0.0165(17) -0.0039(11) C217 0.0224(13) 0.0252(14) 0.073(2) -0.0075(13) 0.0082(13) -0.0021(10) N221 0.0189(10) 0.0210(10) 0.0277(11) -0.0034(8) -0.0012(8) -0.0001(8) C222 0.0217(12) 0.0247(13) 0.0285(13) -0.0003(10) 0.0007(10) 0.0012(9) C223 0.0306(14) 0.0235(13) 0.0389(15) 0.0013(11) 0.0064(11) 0.0072(10) C224 0.0345(14) 0.0241(13) 0.0352(15) -0.0055(10) 0.0119(11) 0.0001(10) C225 0.0290(13) 0.0270(13) 0.0268(13) -0.0024(10) 0.0033(10) -0.0039(10) C226 0.0222(12) 0.0225(12) 0.0308(14) -0.0009(10) 0.0004(10) 0.0010(9) O231 0.0246(8) 0.0235(9) 0.0247(9) 0.0003(7) 0.0025(7) 0.0028(7) C232 0.0407(15) 0.0345(15) 0.0271(14) -0.0006(11) 0.0108(11) -0.0027(12) C233 0.0433(18) 0.0500(19) 0.063(2) -0.0038(15) 0.0268(15) 0.0010(14) C234 0.0468(17) 0.0290(15) 0.0456(17) 0.0122(12) 0.0081(13) -0.0011(12) O241 0.0248(9) 0.0239(9) 0.0296(9) -0.0005(7) 0.0075(7) 0.0020(7) C24A 0.029(3) 0.039(3) 0.026(3) -0.005(2) 0.006(2) 0.010(2) C24B 0.055(4) 0.053(3) 0.029(3) -0.004(2) 0.017(3) 0.006(3) C24C 0.083(8) 0.038(6) 0.111(9) 0.001(5) 0.048(8) 0.030(5) C24D 0.032(5) 0.052(6) 0.025(5) -0.009(4) -0.002(4) 0.015(4) C24E 0.041(6) 0.079(7) 0.041(7) -0.017(5) 0.013(5) -0.003(5) C24F 0.060(12) 0.028(9) 0.079(11) -0.020(7) -0.001(8) -0.014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C15 1.877(3) . ? Cr1 C14 1.890(3) . ? Cr1 C11 1.897(3) . ? Cr1 C13 1.898(3) . ? Cr1 C12 1.914(3) . ? Cr1 C16 2.053(2) . ? Ti1 O121 1.7685(15) 2_656 ? Ti1 O121 1.7685(16) . ? Ti1 O16 1.9791(15) 2_656 ? Ti1 O16 1.9791(15) . ? Ti1 N111 2.3009(18) 2_656 ? Ti1 N111 2.3009(18) . ? Cr2 C25 1.883(2) . ? Cr2 C24 1.893(2) . ? Cr2 C21 1.898(3) . ? Cr2 C23 1.899(3) . ? Cr2 C22 1.909(3) . ? Cr2 C26 2.073(2) . ? Ti2 O231 1.7626(16) . ? Ti2 O241 1.7643(16) . ? Ti2 O36 2.0033(16) . ? Ti2 O26 2.0315(15) . ? Ti2 N221 2.2650(19) . ? Ti2 N212 2.271(2) . ? Cr3 C35 1.869(3) . ? Cr3 C33 1.886(3) . ? Cr3 C31 1.890(4) . ? Cr3 C32 1.902(4) . ? Cr3 C34 1.902(3) . ? Cr3 C36 2.070(3) . ? O11 C11 1.144(3) . ? O12 C12 1.137(3) . ? O13 C13 1.141(3) . ? O14 C14 1.146(3) . ? O15 C15 1.152(3) . ? O16 C16 1.273(3) . ? C16 C17 1.511(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O21 C21 1.138(3) . ? O22 C22 1.130(3) . ? O23 C23 1.144(3) . ? O24 C24 1.142(3) . ? O25 C25 1.145(3) . ? O26 C26 1.273(3) . ? C26 C27 1.501(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O31 C31 1.137(4) . ? O32 C32 1.141(4) . ? O33 C33 1.147(4) . ? O34 C34 1.132(4) . ? O35 C35 1.151(4) . ? O36 C36 1.271(3) . ? C36 C37 1.507(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? N111 C112 1.342(3) . ? N111 C116 1.346(3) . ? C112 C113 1.380(3) . ? C112 H112 0.9500 . ? C113 C114 1.383(3) . ? C113 H113 0.9500 . ? C114 C115 1.379(3) . ? C114 H114 0.9500 . ? C115 C116 1.381(3) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? O121 C122 1.422(3) . ? C122 C123 1.506(4) . ? C122 C124 1.514(4) . ? C122 H122 1.0000 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C124 H12A 0.9800 . ? C124 H12B 0.9800 . ? C124 H12C 0.9800 . ? N212 C213 1.343(3) . ? N212 C217 1.348(3) . ? C213 C214 1.380(4) . ? C213 H213 0.9500 . ? C214 C215 1.370(5) . ? C214 H214 0.9500 . ? C215 C216 1.369(5) . ? C215 H215 0.9500 . ? C216 C217 1.392(4) . ? C216 H216 0.9500 . ? C217 H217 0.9500 . ? N221 C222 1.342(3) . ? N221 C226 1.346(3) . ? C222 C223 1.377(3) . ? C222 H222 0.9500 . ? C223 C224 1.378(4) . ? C223 H223 0.9500 . ? C224 C225 1.385(3) . ? C224 H224 0.9500 . ? C225 C226 1.379(3) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? O231 C232 1.423(3) . ? C232 C233 1.508(4) . ? C232 C234 1.511(4) . ? C232 H232 1.0000 . ? C233 H23A 0.9800 . ? C233 H23B 0.9800 . ? C233 H23C 0.9800 . ? C234 H23D 0.9800 . ? C234 H23E 0.9800 . ? C234 H23F 0.9800 . ? O241 C24A 1.422(5) . ? O241 C24D 1.478(9) . ? C24A C24C 1.498(9) . ? C24A C24B 1.506(7) . ? C24A H24H 1.0000 . ? C24B H24D 0.9800 . ? C24B H24C 0.9800 . ? C24B H24B 0.9800 . ? C24C H24E 0.9800 . ? C24C H24G 0.9800 . ? C24C H24F 0.9800 . ? C24D C24E 1.510(12) . ? C24D C24F 1.524(13) . ? C24D H24A 1.0000 . ? C24E H24I 0.9800 . ? C24E H24K 0.9800 . ? C24E H24J 0.9800 . ? C24F H24N 0.9800 . ? C24F H24M 0.9800 . ? C24F H24L 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 C15 Cr1 C14 90.02(11) . . ? C15 Cr1 C11 94.39(11) . . ? C14 Cr1 C11 89.66(10) . . ? C15 Cr1 C13 93.44(11) . . ? C14 Cr1 C13 88.89(10) . . ? C11 Cr1 C13 172.04(10) . . ? C15 Cr1 C12 89.87(11) . . ? C14 Cr1 C12 179.57(12) . . ? C11 Cr1 C12 89.94(10) . . ? C13 Cr1 C12 91.54(10) . . ? C15 Cr1 C16 175.89(10) . . ? C14 Cr1 C16 93.79(10) . . ? C11 Cr1 C16 87.20(9) . . ? C13 Cr1 C16 85.09(9) . . ? C12 Cr1 C16 86.33(9) . . ? O121 Ti1 O121 99.18(11) 2_656 . ? O121 Ti1 O16 94.50(7) 2_656 2_656 ? O121 Ti1 O16 99.90(7) . 2_656 ? O121 Ti1 O16 99.90(7) 2_656 . ? O121 Ti1 O16 94.50(7) . . ? O16 Ti1 O16 157.73(9) 2_656 . ? O121 Ti1 N111 87.68(7) 2_656 2_656 ? O121 Ti1 N111 172.07(7) . 2_656 ? O16 Ti1 N111 83.42(6) 2_656 2_656 ? O16 Ti1 N111 80.31(6) . 2_656 ? O121 Ti1 N111 172.07(7) 2_656 . ? O121 Ti1 N111 87.68(7) . . ? O16 Ti1 N111 80.31(6) 2_656 . ? O16 Ti1 N111 83.42(6) . . ? N111 Ti1 N111 85.78(9) 2_656 . ? C25 Cr2 C24 89.89(10) . . ? C25 Cr2 C21 92.99(10) . . ? C24 Cr2 C21 91.06(10) . . ? C25 Cr2 C23 91.78(10) . . ? C24 Cr2 C23 90.98(10) . . ? C21 Cr2 C23 174.82(10) . . ? C25 Cr2 C22 91.42(10) . . ? C24 Cr2 C22 178.49(11) . . ? C21 Cr2 C22 89.62(11) . . ? C23 Cr2 C22 88.22(11) . . ? C25 Cr2 C26 178.30(10) . . ? C24 Cr2 C26 89.70(9) . . ? C21 Cr2 C26 85.37(9) . . ? C23 Cr2 C26 89.88(9) . . ? C22 Cr2 C26 89.01(10) . . ? O231 Ti2 O241 102.87(8) . . ? O231 Ti2 O36 100.55(8) . . ? O241 Ti2 O36 92.56(7) . . ? O231 Ti2 O26 93.99(7) . . ? O241 Ti2 O26 99.85(7) . . ? O36 Ti2 O26 158.30(7) . . ? O231 Ti2 N221 87.58(7) . . ? O241 Ti2 N221 168.59(7) . . ? O36 Ti2 N221 80.86(7) . . ? O26 Ti2 N221 83.78(6) . . ? O231 Ti2 N212 168.65(7) . . ? O241 Ti2 N212 87.70(8) . . ? O36 Ti2 N212 82.85(7) . . ? O26 Ti2 N212 79.96(7) . . ? N221 Ti2 N212 82.26(7) . . ? C35 Cr3 C33 95.21(15) . . ? C35 Cr3 C31 91.38(16) . . ? C33 Cr3 C31 173.41(14) . . ? C35 Cr3 C32 90.39(15) . . ? C33 Cr3 C32 90.12(16) . . ? C31 Cr3 C32 90.03(15) . . ? C35 Cr3 C34 89.27(14) . . ? C33 Cr3 C34 90.16(15) . . ? C31 Cr3 C34 89.72(13) . . ? C32 Cr3 C34 179.57(12) . . ? C35 Cr3 C36 176.96(12) . . ? C33 Cr3 C36 85.96(11) . . ? C31 Cr3 C36 87.45(13) . . ? C32 Cr3 C36 92.41(13) . . ? C34 Cr3 C36 87.93(12) . . ? O11 C11 Cr1 177.5(2) . . ? O12 C12 Cr1 178.8(2) . . ? O13 C13 Cr1 177.5(2) . . ? O14 C14 Cr1 177.6(2) . . ? O15 C15 Cr1 178.8(2) . . ? C16 O16 Ti1 151.12(15) . . ? O16 C16 C17 114.20(19) . . ? O16 C16 Cr1 121.60(16) . . ? C17 C16 Cr1 124.19(16) . . ? 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 . . ? O21 C21 Cr2 178.7(2) . . ? O22 C22 Cr2 178.4(3) . . ? O23 C23 Cr2 179.2(2) . . ? O24 C24 Cr2 178.8(2) . . ? O25 C25 Cr2 179.2(2) . . ? C26 O26 Ti2 138.86(15) . . ? O26 C26 C27 114.71(19) . . ? O26 C26 Cr2 122.54(16) . . ? C27 C26 Cr2 122.68(16) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O31 C31 Cr3 178.8(3) . . ? O32 C32 Cr3 178.1(3) . . ? O33 C33 Cr3 177.9(3) . . ? O34 C34 Cr3 179.1(3) . . ? O35 C35 Cr3 178.1(3) . . ? C36 O36 Ti2 143.32(18) . . ? O36 C36 C37 113.9(2) . . ? O36 C36 Cr3 121.8(2) . . ? C37 C36 Cr3 124.23(19) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C112 N111 C116 117.20(19) . . ? C112 N111 Ti1 118.04(14) . . ? C116 N111 Ti1 124.08(15) . . ? N111 C112 C113 123.3(2) . . ? N111 C112 H112 118.3 . . ? C113 C112 H112 118.3 . . ? C112 C113 C114 119.0(2) . . ? C112 C113 H113 120.5 . . ? C114 C113 H113 120.5 . . ? C115 C114 C113 118.3(2) . . ? C115 C114 H114 120.8 . . ? C113 C114 H114 120.8 . . ? C114 C115 C116 119.5(2) . . ? C114 C115 H115 120.2 . . ? C116 C115 H115 120.2 . . ? N111 C116 C115 122.7(2) . . ? N111 C116 H116 118.7 . . ? C115 C116 H116 118.7 . . ? C122 O121 Ti1 154.33(15) . . ? O121 C122 C123 109.4(2) . . ? O121 C122 C124 108.96(19) . . ? C123 C122 C124 112.7(2) . . ? O121 C122 H122 108.6 . . ? C123 C122 H122 108.6 . . ? C124 C122 H122 108.6 . . ? C122 C123 H12D 109.5 . . ? C122 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C122 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C122 C124 H12A 109.5 . . ? C122 C124 H12B 109.5 . . ? H12A C124 H12B 109.5 . . ? C122 C124 H12C 109.5 . . ? H12A C124 H12C 109.5 . . ? H12B C124 H12C 109.5 . . ? C213 N212 C217 117.3(2) . . ? C213 N212 Ti2 117.82(16) . . ? C217 N212 Ti2 124.03(19) . . ? N212 C213 C214 123.5(3) . . ? N212 C213 H213 118.2 . . ? C214 C213 H213 118.2 . . ? C215 C214 C213 118.8(3) . . ? C215 C214 H214 120.6 . . ? C213 C214 H214 120.6 . . ? C216 C215 C214 118.6(3) . . ? C216 C215 H215 120.7 . . ? C214 C215 H215 120.7 . . ? C215 C216 C217 120.1(3) . . ? C215 C216 H216 120.0 . . ? C217 C216 H216 120.0 . . ? N212 C217 C216 121.6(3) . . ? N212 C217 H217 119.2 . . ? C216 C217 H217 119.2 . . ? C222 N221 C226 117.5(2) . . ? C222 N221 Ti2 124.15(16) . . ? C226 N221 Ti2 118.20(15) . . ? N221 C222 C223 122.7(2) . . ? N221 C222 H222 118.6 . . ? C223 C222 H222 118.6 . . ? C222 C223 C224 119.5(2) . . ? C222 C223 H223 120.2 . . ? C224 C223 H223 120.2 . . ? C223 C224 C225 118.3(2) . . ? C223 C224 H224 120.8 . . ? C225 C224 H224 120.8 . . ? C226 C225 C224 119.0(2) . . ? C226 C225 H225 120.5 . . ? C224 C225 H225 120.5 . . ? N221 C226 C225 122.9(2) . . ? N221 C226 H226 118.6 . . ? C225 C226 H226 118.6 . . ? C232 O231 Ti2 165.52(15) . . ? O231 C232 C233 109.5(2) . . ? O231 C232 C234 108.5(2) . . ? C233 C232 C234 112.9(2) . . ? O231 C232 H232 108.6 . . ? C233 C232 H232 108.6 . . ? C234 C232 H232 108.6 . . ? C232 C233 H23A 109.5 . . ? C232 C233 H23B 109.5 . . ? H23A C233 H23B 109.5 . . ? C232 C233 H23C 109.5 . . ? H23A C233 H23C 109.5 . . ? H23B C233 H23C 109.5 . . ? C232 C234 H23D 109.5 . . ? C232 C234 H23E 109.5 . . ? H23D C234 H23E 109.5 . . ? C232 C234 H23F 109.5 . . ? H23D C234 H23F 109.5 . . ? H23E C234 H23F 109.5 . . ? C24A O241 C24D 30.4(3) . . ? C24A O241 Ti2 156.0(3) . . ? C24D O241 Ti2 170.2(5) . . ? O241 C24A C24C 107.9(6) . . ? O241 C24A C24B 108.8(4) . . ? C24C C24A C24B 111.6(8) . . ? O241 C24A H24H 109.5 . . ? C24C C24A H24H 109.5 . . ? C24B C24A H24H 109.5 . . ? O241 C24D C24E 105.1(8) . . ? O241 C24D C24F 108.0(13) . . ? C24E C24D C24F 110.1(11) . . ? O241 C24D H24A 111.2 . . ? C24E C24D H24A 111.2 . . ? C24F C24D H24A 111.2 . . ? C24D C24E H24I 109.5 . . ? C24D C24E H24K 109.5 . . ? H24I C24E H24K 109.5 . . ? C24D C24E H24J 109.5 . . ? H24I C24E H24J 109.5 . . ? H24K C24E H24J 109.5 . . ? C24D C24F H24N 109.5 . . ? C24D C24F H24M 109.5 . . ? H24N C24F H24M 109.5 . . ? C24D C24F H24L 109.5 . . ? H24N C24F H24L 109.5 . . ? H24M C24F H24L 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 Cr1 C11 O11 -167(5) . . . . ? C14 Cr1 C11 O11 103(5) . . . . ? C13 Cr1 C11 O11 24(5) . . . . ? C12 Cr1 C11 O11 -77(5) . . . . ? C16 Cr1 C11 O11 9(5) . . . . ? C15 Cr1 C12 O12 129(11) . . . . ? C14 Cr1 C12 O12 53(23) . . . . ? C11 Cr1 C12 O12 35(11) . . . . ? C13 Cr1 C12 O12 -138(11) . . . . ? C16 Cr1 C12 O12 -53(11) . . . . ? C15 Cr1 C13 O13 -170(5) . . . . ? C14 Cr1 C13 O13 -80(5) . . . . ? C11 Cr1 C13 O13 -1(6) . . . . ? C12 Cr1 C13 O13 100(5) . . . . ? C16 Cr1 C13 O13 14(5) . . . . ? C15 Cr1 C14 O14 2(6) . . . . ? C11 Cr1 C14 O14 97(6) . . . . ? C13 Cr1 C14 O14 -91(6) . . . . ? C12 Cr1 C14 O14 78(18) . . . . ? C16 Cr1 C14 O14 -176(100) . . . . ? C14 Cr1 C15 O15 179(100) . . . . ? C11 Cr1 C15 O15 90(11) . . . . ? C13 Cr1 C15 O15 -92(11) . . . . ? C12 Cr1 C15 O15 0(11) . . . . ? C16 Cr1 C15 O15 -23(12) . . . . ? O121 Ti1 O16 C16 35.7(3) 2_656 . . . ? O121 Ti1 O16 C16 -64.4(3) . . . . ? O16 Ti1 O16 C16 165.2(3) 2_656 . . . ? N111 Ti1 O16 C16 121.6(3) 2_656 . . . ? N111 Ti1 O16 C16 -151.6(3) . . . . ? Ti1 O16 C16 C17 -38.0(4) . . . . ? Ti1 O16 C16 Cr1 140.9(2) . . . . ? C15 Cr1 C16 O16 -13.0(15) . . . . ? C14 Cr1 C16 O16 144.78(19) . . . . ? C11 Cr1 C16 O16 -125.75(19) . . . . ? C13 Cr1 C16 O16 56.23(19) . . . . ? C12 Cr1 C16 O16 -35.63(19) . . . . ? C15 Cr1 C16 C17 165.9(14) . . . . ? C14 Cr1 C16 C17 -36.4(2) . . . . ? C11 Cr1 C16 C17 53.1(2) . . . . ? C13 Cr1 C16 C17 -124.9(2) . . . . ? C12 Cr1 C16 C17 143.2(2) . . . . ? C25 Cr2 C21 O21 -148(10) . . . . ? C24 Cr2 C21 O21 122(10) . . . . ? C23 Cr2 C21 O21 9(10) . . . . ? C22 Cr2 C21 O21 -56(10) . . . . ? C26 Cr2 C21 O21 33(10) . . . . ? C25 Cr2 C22 O22 41(8) . . . . ? C24 Cr2 C22 O22 -169(6) . . . . ? C21 Cr2 C22 O22 -52(8) . . . . ? C23 Cr2 C22 O22 133(8) . . . . ? C26 Cr2 C22 O22 -137(8) . . . . ? C25 Cr2 C23 O23 36(16) . . . . ? C24 Cr2 C23 O23 126(16) . . . . ? C21 Cr2 C23 O23 -121(16) . . . . ? C22 Cr2 C23 O23 -55(16) . . . . ? C26 Cr2 C23 O23 -144(16) . . . . ? C25 Cr2 C24 O24 21(10) . . . . ? C21 Cr2 C24 O24 114(10) . . . . ? C23 Cr2 C24 O24 -71(10) . . . . ? C22 Cr2 C24 O24 -129(9) . . . . ? C26 Cr2 C24 O24 -161(10) . . . . ? C24 Cr2 C25 O25 25(17) . . . . ? C21 Cr2 C25 O25 -66(17) . . . . ? C23 Cr2 C25 O25 116(17) . . . . ? C22 Cr2 C25 O25 -156(17) . . . . ? C26 Cr2 C25 O25 -51(19) . . . . ? O231 Ti2 O26 C26 60.4(2) . . . . ? O241 Ti2 O26 C26 -43.4(2) . . . . ? O36 Ti2 O26 C26 -167.4(2) . . . . ? N221 Ti2 O26 C26 147.5(2) . . . . ? N212 Ti2 O26 C26 -129.3(2) . . . . ? Ti2 O26 C26 C27 5.9(3) . . . . ? Ti2 O26 C26 Cr2 -177.09(10) . . . . ? C25 Cr2 C26 O26 -65(3) . . . . ? C24 Cr2 C26 O26 -141.16(18) . . . . ? C21 Cr2 C26 O26 -50.07(18) . . . . ? C23 Cr2 C26 O26 127.85(18) . . . . ? C22 Cr2 C26 O26 39.63(19) . . . . ? C25 Cr2 C26 C27 112(3) . . . . ? C24 Cr2 C26 C27 35.64(19) . . . . ? C21 Cr2 C26 C27 126.73(19) . . . . ? C23 Cr2 C26 C27 -55.34(19) . . . . ? C22 Cr2 C26 C27 -143.6(2) . . . . ? C35 Cr3 C31 O31 131(18) . . . . ? C33 Cr3 C31 O31 -48(19) . . . . ? C32 Cr3 C31 O31 -139(18) . . . . ? C34 Cr3 C31 O31 41(18) . . . . ? C36 Cr3 C31 O31 -47(18) . . . . ? C35 Cr3 C32 O32 18(12) . . . . ? C33 Cr3 C32 O32 113(12) . . . . ? C31 Cr3 C32 O32 -74(12) . . . . ? C34 Cr3 C32 O32 -19(31) . . . . ? C36 Cr3 C32 O32 -161(12) . . . . ? C35 Cr3 C33 O33 -144(11) . . . . ? C31 Cr3 C33 O33 34(12) . . . . ? C32 Cr3 C33 O33 126(11) . . . . ? C34 Cr3 C33 O33 -55(11) . . . . ? C36 Cr3 C33 O33 33(11) . . . . ? C35 Cr3 C34 O34 -9(21) . . . . ? C33 Cr3 C34 O34 -104(21) . . . . ? C31 Cr3 C34 O34 82(21) . . . . ? C32 Cr3 C34 O34 27(36) . . . . ? C36 Cr3 C34 O34 170(100) . . . . ? C33 Cr3 C35 O35 112(11) . . . . ? C31 Cr3 C35 O35 -67(11) . . . . ? C32 Cr3 C35 O35 -158(11) . . . . ? C34 Cr3 C35 O35 22(11) . . . . ? C36 Cr3 C35 O35 0(14) . . . . ? O231 Ti2 O36 C36 -50.0(3) . . . . ? O241 Ti2 O36 C36 53.6(3) . . . . ? O26 Ti2 O36 C36 178.7(3) . . . . ? N221 Ti2 O36 C36 -135.8(3) . . . . ? N212 Ti2 O36 C36 140.9(3) . . . . ? Ti2 O36 C36 C37 25.9(4) . . . . ? Ti2 O36 C36 Cr3 -151.59(18) . . . . ? C35 Cr3 C36 O36 67(3) . . . . ? C33 Cr3 C36 O36 -45.5(2) . . . . ? C31 Cr3 C36 O36 134.7(2) . . . . ? C32 Cr3 C36 O36 -135.4(2) . . . . ? C34 Cr3 C36 O36 44.9(2) . . . . ? C35 Cr3 C36 C37 -110(3) . . . . ? C33 Cr3 C36 C37 137.3(3) . . . . ? C31 Cr3 C36 C37 -42.6(3) . . . . ? C32 Cr3 C36 C37 47.3(3) . . . . ? C34 Cr3 C36 C37 -132.4(3) . . . . ? O121 Ti1 N111 C112 -112.7(5) 2_656 . . . ? O121 Ti1 N111 C112 37.30(17) . . . . ? O16 Ti1 N111 C112 -63.16(16) 2_656 . . . ? O16 Ti1 N111 C112 132.10(17) . . . . ? N111 Ti1 N111 C112 -147.19(19) 2_656 . . . ? O121 Ti1 N111 C116 77.1(5) 2_656 . . . ? O121 Ti1 N111 C116 -132.95(17) . . . . ? O16 Ti1 N111 C116 126.59(18) 2_656 . . . ? O16 Ti1 N111 C116 -38.16(17) . . . . ? N111 Ti1 N111 C116 42.55(15) 2_656 . . . ? C116 N111 C112 C113 -0.1(3) . . . . ? Ti1 N111 C112 C113 -171.06(19) . . . . ? N111 C112 C113 C114 0.4(4) . . . . ? C112 C113 C114 C115 -0.6(4) . . . . ? C113 C114 C115 C116 0.6(3) . . . . ? C112 N111 C116 C115 0.1(3) . . . . ? Ti1 N111 C116 C115 170.38(17) . . . . ? C114 C115 C116 N111 -0.3(3) . . . . ? O121 Ti1 O121 C122 -21.2(3) 2_656 . . . ? O16 Ti1 O121 C122 -117.4(3) 2_656 . . . ? O16 Ti1 O121 C122 79.6(3) . . . . ? N111 Ti1 O121 C122 128.4(5) 2_656 . . . ? N111 Ti1 O121 C122 162.8(3) . . . . ? Ti1 O121 C122 C123 -168.2(3) . . . . ? Ti1 O121 C122 C124 -44.6(4) . . . . ? O231 Ti2 N212 C213 115.6(4) . . . . ? O241 Ti2 N212 C213 -43.27(17) . . . . ? O36 Ti2 N212 C213 -136.14(17) . . . . ? O26 Ti2 N212 C213 57.15(16) . . . . ? N221 Ti2 N212 C213 142.17(17) . . . . ? O231 Ti2 N212 C217 -75.4(4) . . . . ? O241 Ti2 N212 C217 125.71(19) . . . . ? O36 Ti2 N212 C217 32.84(19) . . . . ? O26 Ti2 N212 C217 -133.87(19) . . . . ? N221 Ti2 N212 C217 -48.85(19) . . . . ? C217 N212 C213 C214 -1.8(3) . . . . ? Ti2 N212 C213 C214 167.9(2) . . . . ? N212 C213 C214 C215 -0.1(4) . . . . ? C213 C214 C215 C216 1.9(4) . . . . ? C214 C215 C216 C217 -1.9(4) . . . . ? C213 N212 C217 C216 1.8(3) . . . . ? Ti2 N212 C217 C216 -167.20(19) . . . . ? C215 C216 C217 N212 0.0(4) . . . . ? O231 Ti2 N221 C222 125.34(18) . . . . ? O241 Ti2 N221 C222 -78.2(4) . . . . ? O36 Ti2 N221 C222 -133.56(19) . . . . ? O26 Ti2 N221 C222 31.06(18) . . . . ? N212 Ti2 N221 C222 -49.61(18) . . . . ? O231 Ti2 N221 C226 -49.58(17) . . . . ? O241 Ti2 N221 C226 106.9(4) . . . . ? O36 Ti2 N221 C226 51.52(17) . . . . ? O26 Ti2 N221 C226 -143.86(17) . . . . ? N212 Ti2 N221 C226 135.47(17) . . . . ? C226 N221 C222 C223 0.0(3) . . . . ? Ti2 N221 C222 C223 -174.92(18) . . . . ? N221 C222 C223 C224 -0.3(4) . . . . ? C222 C223 C224 C225 0.3(4) . . . . ? C223 C224 C225 C226 -0.1(4) . . . . ? C222 N221 C226 C225 0.1(3) . . . . ? Ti2 N221 C226 C225 175.41(18) . . . . ? C224 C225 C226 N221 -0.1(4) . . . . ? O241 Ti2 O231 C232 149.6(6) . . . . ? O36 Ti2 O231 C232 -115.3(6) . . . . ? O26 Ti2 O231 C232 48.6(6) . . . . ? N221 Ti2 O231 C232 -35.0(6) . . . . ? N212 Ti2 O231 C232 -8.7(9) . . . . ? Ti2 O231 C232 C233 -31.1(7) . . . . ? Ti2 O231 C232 C234 -154.8(5) . . . . ? O231 Ti2 O241 C24A 88.8(5) . . . . ? O36 Ti2 O241 C24A -12.7(5) . . . . ? O26 Ti2 O241 C24A -174.8(5) . . . . ? N221 Ti2 O241 C24A -67.1(7) . . . . ? N212 Ti2 O241 C24A -95.4(5) . . . . ? O231 Ti2 O241 C24D -148(2) . . . . ? O36 Ti2 O241 C24D 111(2) . . . . ? O26 Ti2 O241 C24D -51(2) . . . . ? N221 Ti2 O241 C24D 56(2) . . . . ? N212 Ti2 O241 C24D 28(2) . . . . ? C24D O241 C24A C24C 80.6(12) . . . . ? Ti2 O241 C24A C24C -115.7(9) . . . . ? C24D O241 C24A C24B -40.6(8) . . . . ? Ti2 O241 C24A C24B 123.1(6) . . . . ? C24A O241 C24D C24E 52.9(9) . . . . ? Ti2 O241 C24D C24E -85(3) . . . . ? C24A O241 C24D C24F -64.6(12) . . . . ? Ti2 O241 C24D C24F 157.4(19) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.360 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.081 #===END data_(OC)5W=C(Me)OTi(OiPr)3(C5H5N)2 _database_code_depnum_ccdc_archive 'CCDC 670776' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 N2 O14 Ti W2' _chemical_formula_sum 'C30 H30 N2 O14 Ti W2' _chemical_formula_weight 1058.16 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 23.5197(15) _cell_length_b 15.4154(10) _cell_length_c 14.9223(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.7040(10) _cell_angle_gamma 90.00 _cell_volume 5316.2(6) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5006 _cell_measurement_theta_min 26.36 _cell_measurement_theta_max 2.41 _exptl_crystal_description block _exptl_crystal_colour red _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 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3036 _exptl_absorpt_coefficient_mu 6.763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3755 _exptl_absorpt_correction_T_max 0.5512 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31409 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.86 _reflns_number_total 11164 _reflns_number_gt 9184 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One isopropoxide group (on O241) of the complete formula unit is disordered. PART instructions and similarity restraints (SAME-instruction in Shelxl) were applied to model the disorder as best as possible. ; _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^)+(0.0436P)^2^+16.2353P] 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 11164 _refine_ls_number_parameters 702 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.050 _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 W1 W 0.293352(11) 0.255487(15) 0.654567(16) 0.03053(7) Uani 1 1 d . . . Ti1 Ti 0.5000 0.20762(8) 0.7500 0.0229(3) Uani 1 2 d S . . W2 W 0.370534(9) 0.263913(14) 0.271649(14) 0.02141(7) Uani 1 1 d . . . Ti2 Ti 0.16976(4) 0.29278(6) 0.08543(7) 0.0243(2) Uani 1 1 d . A . W3 W -0.033125(11) 0.21465(3) -0.04695(2) 0.06141(12) Uani 1 1 d . . . O11 O 0.2589(2) 0.0562(3) 0.6609(3) 0.0435(11) Uani 1 1 d . . . C11 C 0.2692(3) 0.1284(4) 0.6576(4) 0.0366(14) Uani 1 1 d . . . O12 O 0.3471(2) 0.2448(3) 0.8638(3) 0.0436(11) Uani 1 1 d . . . C12 C 0.3281(3) 0.2497(4) 0.7883(4) 0.0340(14) Uani 1 1 d . . . O13 O 0.3471(2) 0.4414(3) 0.6375(3) 0.0449(11) Uani 1 1 d . . . C13 C 0.3262(3) 0.3758(4) 0.6443(4) 0.0347(14) Uani 1 1 d . . . O14 O 0.2393(2) 0.2633(3) 0.4460(3) 0.0485(12) Uani 1 1 d . . . C14 C 0.2594(3) 0.2601(4) 0.5209(5) 0.0416(16) Uani 1 1 d . . . O15 O 0.1791(2) 0.3294(4) 0.7061(4) 0.0613(14) Uani 1 1 d . . . C15 C 0.2196(3) 0.3014(4) 0.6846(5) 0.0431(16) Uani 1 1 d . . . O16 O 0.42281(17) 0.2325(2) 0.6821(3) 0.0266(8) Uani 1 1 d . . . C16 C 0.3766(3) 0.2086(3) 0.6320(4) 0.0266(12) Uani 1 1 d . . . C17 C 0.3853(3) 0.1459(4) 0.5586(4) 0.0368(14) Uani 1 1 d . . . H17A H 0.3823 0.1769 0.5006 0.055 Uiso 1 1 calc R . . H17B H 0.3556 0.1006 0.5526 0.055 Uiso 1 1 calc R . . H17C H 0.4237 0.1193 0.5748 0.055 Uiso 1 1 calc R . . O21 O 0.29843(19) 0.1128(3) 0.3417(3) 0.0396(10) Uani 1 1 d . . . C21 C 0.3247(2) 0.1670(4) 0.3173(4) 0.0289(12) Uani 1 1 d . . . O22 O 0.3721(2) 0.1551(4) 0.0921(3) 0.0594(15) Uani 1 1 d . . . C22 C 0.3715(2) 0.1948(4) 0.1554(4) 0.0346(14) Uani 1 1 d . . . O23 O 0.43696(18) 0.4148(3) 0.1899(3) 0.0369(10) Uani 1 1 d . . . C23 C 0.4125(2) 0.3612(4) 0.2188(4) 0.0274(12) Uani 1 1 d . . . O24 O 0.36805(19) 0.3719(3) 0.4494(3) 0.0380(10) Uani 1 1 d . . . C24 C 0.3685(2) 0.3333(4) 0.3849(4) 0.0272(12) Uani 1 1 d . . . O25 O 0.48777(18) 0.1791(3) 0.3622(3) 0.0401(10) Uani 1 1 d . . . C25 C 0.4456(2) 0.2097(4) 0.3293(4) 0.0275(12) Uani 1 1 d . . . O26 O 0.24898(16) 0.2756(2) 0.1595(3) 0.0245(8) Uani 1 1 d . . . C26 C 0.2872(2) 0.3194(3) 0.2105(3) 0.0222(11) Uani 1 1 d . . . C27 C 0.2692(2) 0.4097(4) 0.2307(4) 0.0303(13) Uani 1 1 d . . . H27A H 0.2443 0.4339 0.1765 0.045 Uiso 1 1 calc R . . H27B H 0.3037 0.4462 0.2476 0.045 Uiso 1 1 calc R . . H27C H 0.2480 0.4081 0.2813 0.045 Uiso 1 1 calc R . . O31 O -0.0961(3) 0.3850(6) -0.0019(6) 0.115(3) Uani 1 1 d . . . C31 C -0.0738(4) 0.3241(7) -0.0190(6) 0.073(3) Uani 1 1 d . . . O32 O -0.0669(3) 0.2548(9) -0.2555(5) 0.204(8) Uani 1 1 d . . . C32 C -0.0549(4) 0.2414(11) -0.1815(7) 0.138(7) Uani 1 1 d . . . O33 O 0.0411(3) 0.0536(6) -0.0881(7) 0.148(4) Uani 1 1 d . . . C33 C 0.0130(3) 0.1111(7) -0.0731(8) 0.099(4) Uani 1 1 d . . . O34 O -0.0015(4) 0.1691(6) 0.1600(6) 0.120(3) Uani 1 1 d . . . C34 C -0.0125(3) 0.1861(7) 0.0857(7) 0.069(2) Uani 1 1 d . . . O35 O -0.1465(3) 0.1058(6) -0.0461(6) 0.136(4) Uani 1 1 d . . . C35 C -0.1057(3) 0.1467(8) -0.0496(8) 0.103(5) Uani 1 1 d . . . O36 O 0.09370(17) 0.2609(3) 0.0127(3) 0.0348(10) Uani 1 1 d . . . C36 C 0.0470(3) 0.2889(5) -0.0320(5) 0.0472(18) Uani 1 1 d . . . C37 C 0.0522(4) 0.3795(7) -0.0664(8) 0.102(4) Uani 1 1 d . . . H37A H 0.0931 0.3943 -0.0617 0.153 Uiso 1 1 calc R . . H37B H 0.0342 0.4202 -0.0296 0.153 Uiso 1 1 calc R . . H37C H 0.0326 0.3832 -0.1302 0.153 Uiso 1 1 calc R . . N111 N 0.4785(2) 0.3168(3) 0.8421(3) 0.0247(10) Uani 1 1 d . . . C112 C 0.4900(3) 0.3043(4) 0.9319(4) 0.0301(13) Uani 1 1 d . . . H112 H 0.5114 0.2543 0.9549 0.036 Uiso 1 1 calc R . . C113 C 0.4724(3) 0.3597(4) 0.9925(4) 0.0318(13) Uani 1 1 d . . . H113 H 0.4815 0.3481 1.0561 0.038 Uiso 1 1 calc R . . C114 C 0.4414(3) 0.4323(4) 0.9610(4) 0.0305(13) Uani 1 1 d . . . H114 H 0.4283 0.4714 1.0021 0.037 Uiso 1 1 calc R . . C115 C 0.4297(3) 0.4470(4) 0.8694(4) 0.0304(13) Uani 1 1 d . . . H115 H 0.4087 0.4970 0.8452 0.036 Uiso 1 1 calc R . . C116 C 0.4489(3) 0.3881(3) 0.8128(4) 0.0280(12) Uani 1 1 d . . . H116 H 0.4406 0.3988 0.7491 0.034 Uiso 1 1 calc R . . O121 O 0.47549(18) 0.1340(2) 0.8239(3) 0.0310(9) Uani 1 1 d . . . C122 C 0.4561(3) 0.0514(4) 0.8477(4) 0.0364(14) Uani 1 1 d . . . H122 H 0.4895 0.0101 0.8562 0.044 Uiso 1 1 calc R . . C123 C 0.4345(3) 0.0584(5) 0.9356(5) 0.056(2) Uani 1 1 d . . . H12D H 0.4662 0.0763 0.9843 0.085 Uiso 1 1 calc R . . H12E H 0.4196 0.0019 0.9509 0.085 Uiso 1 1 calc R . . H12F H 0.4034 0.1015 0.9293 0.085 Uiso 1 1 calc R . . C124 C 0.4106(3) 0.0191(4) 0.7723(5) 0.0506(19) Uani 1 1 d . . . H12A H 0.3768 0.0575 0.7653 0.076 Uiso 1 1 calc R . . H12B H 0.3992 -0.0398 0.7865 0.076 Uiso 1 1 calc R . . H12C H 0.4258 0.0183 0.7154 0.076 Uiso 1 1 calc R . . N212 N 0.1540(2) 0.1757(3) 0.1681(4) 0.0333(11) Uani 1 1 d . . . C213 C 0.1672(3) 0.1802(5) 0.2579(5) 0.0422(16) Uani 1 1 d . . . H213 H 0.1892 0.2288 0.2839 0.051 Uiso 1 1 calc R . . C214 C 0.1516(3) 0.1203(5) 0.3160(6) 0.057(2) Uani 1 1 d . . . H214 H 0.1623 0.1274 0.3802 0.068 Uiso 1 1 calc R . . C215 C 0.1206(3) 0.0508(5) 0.2802(7) 0.063(2) Uani 1 1 d . . . H215 H 0.1080 0.0091 0.3192 0.075 Uiso 1 1 calc R . . C216 C 0.1073(3) 0.0407(5) 0.1888(7) 0.064(2) Uani 1 1 d . . . H216 H 0.0868 -0.0089 0.1625 0.076 Uiso 1 1 calc R . . C217 C 0.1247(3) 0.1053(4) 0.1342(6) 0.0479(18) Uani 1 1 d . . . H217 H 0.1152 0.0988 0.0698 0.057 Uiso 1 1 calc R . . N221 N 0.19832(19) 0.1897(3) -0.0035(3) 0.0275(10) Uani 1 1 d . . . C222 C 0.2356(2) 0.1267(4) 0.0262(4) 0.0316(13) Uani 1 1 d . . . H222 H 0.2493 0.1218 0.0900 0.038 Uiso 1 1 calc R . . C223 C 0.2553(3) 0.0680(4) -0.0305(4) 0.0345(14) Uani 1 1 d . . . H223 H 0.2818 0.0238 -0.0061 0.041 Uiso 1 1 calc R . . C224 C 0.2362(3) 0.0744(4) -0.1219(4) 0.0366(14) Uani 1 1 d . . . H224 H 0.2489 0.0347 -0.1628 0.044 Uiso 1 1 calc R . . C225 C 0.1982(3) 0.1396(4) -0.1535(4) 0.0341(14) Uani 1 1 d . . . H225 H 0.1845 0.1460 -0.2171 0.041 Uiso 1 1 calc R . . C226 C 0.1800(2) 0.1953(4) -0.0938(4) 0.0302(13) Uani 1 1 d . . . H226 H 0.1534 0.2398 -0.1171 0.036 Uiso 1 1 calc R . . O231 O 0.19299(16) 0.3708(2) 0.0146(3) 0.0276(8) Uani 1 1 d . . . C232 C 0.2244(3) 0.4134(4) -0.0445(5) 0.0428(16) Uani 1 1 d D . . H232 H 0.2085 0.3957 -0.1087 0.051 Uiso 1 1 calc R . . C233 C 0.2859(3) 0.3896(5) -0.0226(6) 0.060(2) Uani 1 1 d D . . H23A H 0.3024 0.4091 0.0393 0.091 Uiso 1 1 calc R . . H23B H 0.3066 0.4175 -0.0661 0.091 Uiso 1 1 calc R . . H23C H 0.2898 0.3265 -0.0264 0.091 Uiso 1 1 calc R . . C234 C 0.2154(3) 0.5110(4) -0.0350(6) 0.058(2) Uani 1 1 d D . . H23D H 0.1742 0.5248 -0.0539 0.086 Uiso 1 1 calc R . . H23E H 0.2378 0.5425 -0.0737 0.086 Uiso 1 1 calc R . . H23F H 0.2284 0.5282 0.0288 0.086 Uiso 1 1 calc R . . O241 O 0.13895(17) 0.3566(3) 0.1608(3) 0.0311(9) Uani 1 1 d D . . C24A C 0.0929(6) 0.3918(9) 0.1978(10) 0.047(5) Uani 0.513(17) 1 d PD A 1 H24H H 0.0542 0.3834 0.1578 0.057 Uiso 0.513(17) 1 calc PR A 1 C24B C 0.0940(13) 0.3665(16) 0.2932(10) 0.076(7) Uani 0.513(17) 1 d PD A 1 H24D H 0.0724 0.3123 0.2948 0.114 Uiso 0.513(17) 1 calc PR A 1 H24C H 0.0762 0.4123 0.3242 0.114 Uiso 0.513(17) 1 calc PR A 1 H24B H 0.1341 0.3580 0.3241 0.114 Uiso 0.513(17) 1 calc PR A 1 C24C C 0.1089(9) 0.4891(9) 0.2168(16) 0.077(7) Uani 0.513(17) 1 d PDU A 1 H24E H 0.1445 0.4931 0.2627 0.115 Uiso 0.513(17) 1 calc PR A 1 H24G H 0.0774 0.5184 0.2395 0.115 Uiso 0.513(17) 1 calc PR A 1 H24F H 0.1149 0.5169 0.1603 0.115 Uiso 0.513(17) 1 calc PR A 1 C24D C 0.1145(7) 0.4060(14) 0.2244(12) 0.093(12) Uani 0.487(17) 1 d PD A 2 H24A H 0.1414 0.4325 0.2771 0.111 Uiso 0.487(17) 1 calc PR A 2 C24E C 0.0681(13) 0.3469(16) 0.245(2) 0.133(16) Uani 0.487(17) 1 d PD A 2 H24I H 0.0350 0.3484 0.1937 0.200 Uiso 0.487(17) 1 calc PR A 2 H24K H 0.0556 0.3659 0.3005 0.200 Uiso 0.487(17) 1 calc PR A 2 H24J H 0.0831 0.2875 0.2526 0.200 Uiso 0.487(17) 1 calc PR A 2 C24F C 0.0720(13) 0.4684(18) 0.159(2) 0.138(12) Uani 0.487(17) 1 d PDU A 2 H24N H 0.0937 0.4998 0.1193 0.206 Uiso 0.487(17) 1 calc PR A 2 H24M H 0.0548 0.5101 0.1960 0.206 Uiso 0.487(17) 1 calc PR A 2 H24L H 0.0414 0.4341 0.1221 0.206 Uiso 0.487(17) 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 W1 0.03857(15) 0.02624(13) 0.02570(13) -0.00219(9) 0.00320(10) 0.00376(10) Ti1 0.0372(8) 0.0141(6) 0.0172(7) 0.000 0.0044(6) 0.000 W2 0.02065(11) 0.02311(11) 0.01932(12) -0.00249(8) 0.00075(8) -0.00082(8) Ti2 0.0197(5) 0.0224(5) 0.0292(5) -0.0025(4) 0.0000(4) 0.0010(4) W3 0.01832(14) 0.1013(3) 0.0628(2) -0.04732(19) 0.00292(13) 0.00016(14) O11 0.054(3) 0.033(3) 0.041(3) -0.0038(19) 0.004(2) -0.002(2) C11 0.043(4) 0.033(4) 0.033(3) -0.003(3) 0.004(3) 0.002(3) O12 0.053(3) 0.046(3) 0.030(3) -0.0024(19) 0.005(2) 0.000(2) C12 0.040(4) 0.029(3) 0.033(4) -0.007(2) 0.009(3) -0.001(3) O13 0.058(3) 0.029(2) 0.040(3) -0.0023(19) -0.010(2) 0.006(2) C13 0.052(4) 0.019(3) 0.029(3) -0.002(2) -0.002(3) 0.007(3) O14 0.063(3) 0.047(3) 0.030(3) -0.002(2) -0.007(2) 0.007(2) C14 0.045(4) 0.030(3) 0.048(4) -0.006(3) 0.005(3) 0.002(3) O15 0.050(3) 0.070(4) 0.065(4) -0.009(3) 0.012(3) 0.011(3) C15 0.052(4) 0.041(4) 0.035(4) -0.007(3) 0.003(3) 0.003(3) O16 0.036(2) 0.0195(18) 0.023(2) 0.0004(15) 0.0025(17) -0.0005(16) C16 0.043(3) 0.015(2) 0.022(3) 0.002(2) 0.007(3) -0.002(2) C17 0.046(4) 0.031(3) 0.032(3) -0.006(3) 0.006(3) -0.003(3) O21 0.043(3) 0.025(2) 0.050(3) 0.0012(19) 0.007(2) -0.0046(19) C21 0.028(3) 0.022(3) 0.034(3) -0.002(2) 0.000(2) 0.000(2) O22 0.039(3) 0.094(4) 0.044(3) -0.037(3) 0.003(2) 0.004(3) C22 0.021(3) 0.048(4) 0.035(3) -0.014(3) 0.003(2) -0.002(3) O23 0.039(2) 0.040(2) 0.034(2) 0.0014(19) 0.011(2) -0.003(2) C23 0.028(3) 0.027(3) 0.026(3) -0.001(2) 0.002(2) 0.000(2) O24 0.055(3) 0.032(2) 0.029(2) -0.0058(18) 0.011(2) -0.013(2) C24 0.028(3) 0.027(3) 0.027(3) 0.002(2) 0.006(2) -0.007(2) O25 0.028(2) 0.042(3) 0.045(3) -0.001(2) -0.006(2) 0.0051(19) C25 0.024(3) 0.031(3) 0.024(3) -0.007(2) -0.003(2) -0.001(2) O26 0.0233(19) 0.0228(19) 0.026(2) -0.0024(15) 0.0015(16) -0.0014(15) C26 0.026(3) 0.022(3) 0.020(3) 0.002(2) 0.006(2) -0.003(2) C27 0.030(3) 0.025(3) 0.035(3) -0.004(2) 0.002(3) 0.002(2) O31 0.102(6) 0.134(7) 0.115(6) 0.008(5) 0.037(5) 0.070(5) C31 0.056(5) 0.107(8) 0.052(5) -0.010(5) 0.003(4) 0.034(5) O32 0.033(4) 0.53(2) 0.048(5) -0.050(8) -0.006(3) -0.003(7) C32 0.019(4) 0.34(2) 0.051(6) -0.069(9) 0.000(4) 0.010(7) O33 0.053(4) 0.150(8) 0.245(10) -0.152(8) 0.038(5) -0.012(4) C33 0.028(4) 0.123(9) 0.147(10) -0.100(8) 0.022(5) -0.021(5) O34 0.102(6) 0.169(9) 0.098(6) 0.036(6) 0.039(5) 0.075(6) C34 0.037(4) 0.087(7) 0.083(7) -0.005(5) 0.014(5) 0.014(4) O35 0.042(4) 0.190(9) 0.181(8) -0.106(7) 0.038(5) -0.043(5) C35 0.022(4) 0.160(11) 0.130(9) -0.095(8) 0.023(5) -0.021(5) O36 0.021(2) 0.038(2) 0.041(3) -0.0130(18) -0.0042(18) 0.0026(17) C36 0.028(3) 0.064(5) 0.045(4) -0.012(3) -0.005(3) 0.010(3) C37 0.055(6) 0.096(8) 0.135(10) 0.043(7) -0.030(6) 0.013(5) N111 0.038(3) 0.017(2) 0.019(2) -0.0024(17) 0.004(2) -0.0003(19) C112 0.044(3) 0.023(3) 0.021(3) 0.000(2) 0.002(2) 0.008(2) C113 0.041(3) 0.034(3) 0.019(3) -0.005(2) 0.001(2) 0.006(3) C114 0.037(3) 0.024(3) 0.030(3) -0.008(2) 0.005(3) 0.004(2) C115 0.039(3) 0.020(3) 0.030(3) 0.000(2) 0.003(3) 0.006(2) C116 0.041(3) 0.021(3) 0.022(3) 0.002(2) 0.003(2) 0.003(2) O121 0.047(2) 0.0187(19) 0.026(2) 0.0036(15) 0.0044(18) -0.0061(17) C122 0.051(4) 0.021(3) 0.037(4) 0.008(2) 0.008(3) 0.000(3) C123 0.064(5) 0.062(5) 0.049(5) 0.028(4) 0.024(4) 0.006(4) C124 0.052(4) 0.033(4) 0.062(5) 0.011(3) -0.003(4) -0.015(3) N212 0.021(2) 0.028(3) 0.051(3) 0.002(2) 0.010(2) 0.001(2) C213 0.032(3) 0.044(4) 0.052(4) 0.010(3) 0.010(3) 0.001(3) C214 0.045(4) 0.063(5) 0.065(5) 0.032(4) 0.018(4) 0.004(4) C215 0.037(4) 0.053(5) 0.101(7) 0.036(5) 0.021(5) 0.009(4) C216 0.040(4) 0.034(4) 0.119(8) 0.003(4) 0.021(5) -0.009(3) C217 0.029(3) 0.033(4) 0.083(6) -0.006(3) 0.011(3) -0.006(3) N221 0.022(2) 0.025(2) 0.034(3) 0.000(2) 0.001(2) 0.0010(19) C222 0.027(3) 0.027(3) 0.038(3) -0.002(2) 0.001(3) -0.002(2) C223 0.031(3) 0.026(3) 0.045(4) -0.001(3) 0.003(3) 0.007(2) C224 0.040(4) 0.028(3) 0.044(4) -0.012(3) 0.013(3) -0.003(3) C225 0.032(3) 0.035(3) 0.034(3) -0.008(3) 0.004(3) -0.002(3) C226 0.027(3) 0.025(3) 0.036(3) -0.006(2) 0.001(2) 0.001(2) O231 0.027(2) 0.024(2) 0.030(2) -0.0004(16) 0.0027(17) 0.0010(16) C232 0.047(4) 0.046(4) 0.037(4) 0.003(3) 0.012(3) -0.003(3) C233 0.052(5) 0.055(5) 0.084(6) -0.008(4) 0.038(4) -0.002(4) C234 0.064(5) 0.038(4) 0.072(5) 0.019(4) 0.016(4) 0.006(4) O241 0.029(2) 0.030(2) 0.035(2) -0.0012(17) 0.0097(18) 0.0034(17) C24A 0.048(10) 0.046(9) 0.052(10) -0.018(8) 0.022(9) -0.004(8) C24B 0.104(17) 0.104(16) 0.023(9) -0.001(10) 0.021(10) 0.022(13) C24C 0.077(14) 0.019(7) 0.14(2) -0.033(9) 0.033(12) 0.006(8) C24D 0.024(9) 0.15(3) 0.10(2) -0.099(18) -0.007(10) -0.009(11) C24E 0.18(4) 0.12(3) 0.14(3) 0.06(2) 0.13(3) 0.09(2) C24F 0.18(3) 0.100(19) 0.16(3) 0.061(17) 0.10(2) 0.097(18) _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 W1 C15 2.000(7) . ? W1 C14 2.008(8) . ? W1 C12 2.013(7) . ? W1 C13 2.026(6) . ? W1 C11 2.042(6) . ? W1 C16 2.171(6) . ? Ti1 O121 1.753(4) . ? Ti1 O121 1.753(4) 2_656 ? Ti1 O16 1.946(4) 2_656 ? Ti1 O16 1.946(4) . ? Ti1 N111 2.288(4) . ? Ti1 N111 2.288(4) 2_656 ? W2 C25 1.997(6) . ? W2 C24 2.008(6) . ? W2 C21 2.033(6) . ? W2 C23 2.034(6) . ? W2 C22 2.040(6) . ? W2 C26 2.177(5) . ? Ti2 O241 1.749(4) . ? Ti2 O231 1.755(4) . ? Ti2 O36 1.975(4) . ? Ti2 O26 1.999(4) . ? Ti2 N221 2.251(5) . ? Ti2 N212 2.255(5) . ? W3 C35 1.997(9) . ? W3 C34 1.997(11) . ? W3 C33 2.009(10) . ? W3 C32 2.020(12) . ? W3 C31 2.021(9) . ? W3 C36 2.181(7) . ? O11 C11 1.142(7) . ? O12 C12 1.136(7) . ? O13 C13 1.137(7) . ? O14 C14 1.131(8) . ? O15 C15 1.143(8) . ? O16 C16 1.255(7) . ? C16 C17 1.503(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O21 C21 1.138(7) . ? O22 C22 1.128(7) . ? O23 C23 1.136(7) . ? O24 C24 1.134(7) . ? O25 C25 1.126(7) . ? O26 C26 1.260(6) . ? C26 C27 1.503(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O31 C31 1.128(11) . ? O32 C32 1.108(13) . ? O33 C33 1.151(11) . ? O34 C34 1.123(11) . ? O35 C35 1.157(11) . ? O36 C36 1.251(8) . ? C36 C37 1.500(12) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? N111 C116 1.331(7) . ? N111 C112 1.331(7) . ? C112 C113 1.363(8) . ? C112 H112 0.9500 . ? C113 C114 1.370(8) . ? C113 H113 0.9500 . ? C114 C115 1.362(8) . ? C114 H114 0.9500 . ? C115 C116 1.372(8) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? O121 C122 1.419(7) . ? C122 C124 1.488(9) . ? C122 C123 1.497(9) . ? C122 H122 1.0000 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C124 H12A 0.9800 . ? C124 H12B 0.9800 . ? C124 H12C 0.9800 . ? N212 C213 1.320(8) . ? N212 C217 1.334(8) . ? C213 C214 1.363(9) . ? C213 H213 0.9500 . ? C214 C215 1.351(12) . ? C214 H214 0.9500 . ? C215 C216 1.351(12) . ? C215 H215 0.9500 . ? C216 C217 1.394(11) . ? C216 H216 0.9500 . ? C217 H217 0.9500 . ? N221 C222 1.328(7) . ? N221 C226 1.338(7) . ? C222 C223 1.376(8) . ? C222 H222 0.9500 . ? C223 C224 1.357(9) . ? C223 H223 0.9500 . ? C224 C225 1.370(9) . ? C224 H224 0.9500 . ? C225 C226 1.362(8) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? O231 C232 1.413(7) . ? C232 C233 1.468(9) . ? C232 C234 1.529(9) . ? C232 H232 1.0000 . ? C233 H23A 0.9800 . ? C233 H23B 0.9800 . ? C233 H23C 0.9800 . ? C234 H23D 0.9800 . ? C234 H23E 0.9800 . ? C234 H23F 0.9800 . ? O241 C24A 1.413(11) . ? O241 C24D 1.420(11) . ? C24A C24B 1.471(15) . ? C24A C24C 1.560(14) . ? C24A H24H 1.0000 . ? C24B H24D 0.9800 . ? C24B H24C 0.9800 . ? C24B H24B 0.9800 . ? C24C H24E 0.9800 . ? C24C H24G 0.9800 . ? C24C H24F 0.9800 . ? C24D C24E 1.495(17) . ? C24D C24F 1.584(17) . ? C24D H24A 1.0000 . ? C24E H24I 0.9800 . ? C24E H24K 0.9800 . ? C24E H24J 0.9800 . ? C24F H24N 0.9800 . ? C24F H24M 0.9800 . ? C24F H24L 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 C15 W1 C14 90.5(3) . . ? C15 W1 C12 90.1(3) . . ? C14 W1 C12 179.3(3) . . ? C15 W1 C13 93.0(3) . . ? C14 W1 C13 88.8(2) . . ? C12 W1 C13 91.5(2) . . ? C15 W1 C11 94.5(3) . . ? C14 W1 C11 89.7(3) . . ? C12 W1 C11 89.9(2) . . ? C13 W1 C11 172.4(3) . . ? C15 W1 C16 175.7(2) . . ? C14 W1 C16 93.5(2) . . ? C12 W1 C16 85.9(2) . . ? C13 W1 C16 85.7(2) . . ? C11 W1 C16 86.9(2) . . ? O121 Ti1 O121 99.3(3) . 2_656 ? O121 Ti1 O16 100.61(17) . 2_656 ? O121 Ti1 O16 94.10(17) 2_656 2_656 ? O121 Ti1 O16 94.10(17) . . ? O121 Ti1 O16 100.61(17) 2_656 . ? O16 Ti1 O16 157.2(2) 2_656 . ? O121 Ti1 N111 87.89(17) . . ? O121 Ti1 N111 171.64(18) 2_656 . ? O16 Ti1 N111 80.25(16) 2_656 . ? O16 Ti1 N111 83.05(16) . . ? O121 Ti1 N111 171.64(18) . 2_656 ? O121 Ti1 N111 87.89(17) 2_656 2_656 ? O16 Ti1 N111 83.05(16) 2_656 2_656 ? O16 Ti1 N111 80.25(16) . 2_656 ? N111 Ti1 N111 85.3(2) . 2_656 ? C25 W2 C24 91.0(2) . . ? C25 W2 C21 91.7(2) . . ? C24 W2 C21 90.7(2) . . ? C25 W2 C23 91.2(2) . . ? C24 W2 C23 91.3(2) . . ? C21 W2 C23 176.4(2) . . ? C25 W2 C22 90.0(2) . . ? C24 W2 C22 179.0(3) . . ? C21 W2 C22 89.5(2) . . ? C23 W2 C22 88.4(2) . . ? C25 W2 C26 178.1(2) . . ? C24 W2 C26 89.0(2) . . ? C21 W2 C26 86.4(2) . . ? C23 W2 C26 90.7(2) . . ? C22 W2 C26 90.0(2) . . ? O241 Ti2 O231 102.38(18) . . ? O241 Ti2 O36 92.99(18) . . ? O231 Ti2 O36 101.04(19) . . ? O241 Ti2 O26 100.00(17) . . ? O231 Ti2 O26 93.50(17) . . ? O36 Ti2 O26 157.97(16) . . ? O241 Ti2 N221 168.65(18) . . ? O231 Ti2 N221 88.18(17) . . ? O36 Ti2 N221 80.75(17) . . ? O26 Ti2 N221 83.29(16) . . ? O241 Ti2 N212 88.21(19) . . ? O231 Ti2 N212 168.38(18) . . ? O36 Ti2 N212 82.94(19) . . ? O26 Ti2 N212 79.80(17) . . ? N221 Ti2 N212 81.66(18) . . ? C35 W3 C34 87.4(4) . . ? C35 W3 C33 94.0(4) . . ? C34 W3 C33 88.7(4) . . ? C35 W3 C32 91.7(5) . . ? C34 W3 C32 178.9(5) . . ? C33 W3 C32 90.9(5) . . ? C35 W3 C31 90.4(4) . . ? C34 W3 C31 90.9(4) . . ? C33 W3 C31 175.6(4) . . ? C32 W3 C31 89.6(5) . . ? C35 W3 C36 175.4(4) . . ? C34 W3 C36 88.2(3) . . ? C33 W3 C36 87.1(3) . . ? C32 W3 C36 92.8(4) . . ? C31 W3 C36 88.5(3) . . ? O11 C11 W1 176.1(6) . . ? O12 C12 W1 178.6(6) . . ? O13 C13 W1 176.6(6) . . ? O14 C14 W1 178.6(6) . . ? O15 C15 W1 176.3(6) . . ? C16 O16 Ti1 150.8(4) . . ? O16 C16 C17 113.8(5) . . ? O16 C16 W1 121.1(4) . . ? C17 C16 W1 125.2(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 . . ? O21 C21 W2 179.1(5) . . ? O22 C22 W2 178.6(6) . . ? O23 C23 W2 178.7(5) . . ? O24 C24 W2 179.0(6) . . ? O25 C25 W2 179.7(6) . . ? C26 O26 Ti2 138.6(4) . . ? O26 C26 C27 114.9(5) . . ? O26 C26 W2 122.0(4) . . ? C27 C26 W2 123.0(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O31 C31 W3 178.9(9) . . ? O32 C32 W3 179.0(16) . . ? O33 C33 W3 177.7(9) . . ? O34 C34 W3 178.9(11) . . ? O35 C35 W3 176.0(12) . . ? C36 O36 Ti2 145.3(5) . . ? O36 C36 C37 112.7(7) . . ? O36 C36 W3 121.9(6) . . ? C37 C36 W3 125.2(5) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C116 N111 C112 116.5(5) . . ? C116 N111 Ti1 124.8(4) . . ? C112 N111 Ti1 118.2(4) . . ? N111 C112 C113 123.2(5) . . ? N111 C112 H112 118.4 . . ? C113 C112 H112 118.4 . . ? C112 C113 C114 119.5(5) . . ? C112 C113 H113 120.2 . . ? C114 C113 H113 120.2 . . ? C115 C114 C113 118.3(5) . . ? C115 C114 H114 120.9 . . ? C113 C114 H114 120.9 . . ? C114 C115 C116 118.7(5) . . ? C114 C115 H115 120.7 . . ? C116 C115 H115 120.7 . . ? N111 C116 C115 123.8(5) . . ? N111 C116 H116 118.1 . . ? C115 C116 H116 118.1 . . ? C122 O121 Ti1 153.7(4) . . ? O121 C122 C124 109.3(5) . . ? O121 C122 C123 109.4(5) . . ? C124 C122 C123 111.9(6) . . ? O121 C122 H122 108.7 . . ? C124 C122 H122 108.7 . . ? C123 C122 H122 108.7 . . ? C122 C123 H12D 109.5 . . ? C122 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C122 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C122 C124 H12A 109.5 . . ? C122 C124 H12B 109.5 . . ? H12A C124 H12B 109.5 . . ? C122 C124 H12C 109.5 . . ? H12A C124 H12C 109.5 . . ? H12B C124 H12C 109.5 . . ? C213 N212 C217 115.8(6) . . ? C213 N212 Ti2 118.7(4) . . ? C217 N212 Ti2 124.7(5) . . ? N212 C213 C214 124.7(7) . . ? N212 C213 H213 117.6 . . ? C214 C213 H213 117.6 . . ? C215 C214 C213 118.4(8) . . ? C215 C214 H214 120.8 . . ? C213 C214 H214 120.8 . . ? C216 C215 C214 119.8(7) . . ? C216 C215 H215 120.1 . . ? C214 C215 H215 120.1 . . ? C215 C216 C217 118.1(8) . . ? C215 C216 H216 120.9 . . ? C217 C216 H216 120.9 . . ? N212 C217 C216 123.1(8) . . ? N212 C217 H217 118.5 . . ? C216 C217 H217 118.5 . . ? C222 N221 C226 116.8(5) . . ? C222 N221 Ti2 124.8(4) . . ? C226 N221 Ti2 118.2(4) . . ? N221 C222 C223 123.5(6) . . ? N221 C222 H222 118.2 . . ? C223 C222 H222 118.2 . . ? C224 C223 C222 118.9(6) . . ? C224 C223 H223 120.5 . . ? C222 C223 H223 120.5 . . ? C223 C224 C225 118.1(6) . . ? C223 C224 H224 120.9 . . ? C225 C224 H224 120.9 . . ? C226 C225 C224 120.1(6) . . ? C226 C225 H225 119.9 . . ? C224 C225 H225 119.9 . . ? N221 C226 C225 122.5(5) . . ? N221 C226 H226 118.8 . . ? C225 C226 H226 118.8 . . ? C232 O231 Ti2 162.2(4) . . ? O231 C232 C233 110.7(6) . . ? O231 C232 C234 107.5(5) . . ? C233 C232 C234 111.9(6) . . ? O231 C232 H232 108.9 . . ? C233 C232 H232 108.9 . . ? C234 C232 H232 108.9 . . ? C232 C233 H23A 109.5 . . ? C232 C233 H23B 109.5 . . ? H23A C233 H23B 109.5 . . ? C232 C233 H23C 109.5 . . ? H23A C233 H23C 109.5 . . ? H23B C233 H23C 109.5 . . ? C232 C234 H23D 109.5 . . ? C232 C234 H23E 109.5 . . ? H23D C234 H23E 109.5 . . ? C232 C234 H23F 109.5 . . ? H23D C234 H23F 109.5 . . ? H23E C234 H23F 109.5 . . ? C24A O241 C24D 25.5(7) . . ? C24A O241 Ti2 155.1(7) . . ? C24D O241 Ti2 177.9(11) . . ? O241 C24A C24B 113.5(16) . . ? O241 C24A C24C 105.3(12) . . ? C24B C24A C24C 96.8(14) . . ? O241 C24A H24H 113.3 . . ? C24B C24A H24H 113.3 . . ? C24C C24A H24H 113.3 . . ? O241 C24D C24E 102.0(15) . . ? O241 C24D C24F 101.7(15) . . ? C24E C24D C24F 95.3(15) . . ? O241 C24D H24A 118.0 . . ? C24E C24D H24A 118.0 . . ? C24F C24D H24A 118.0 . . ? C24D C24E H24I 109.5 . . ? C24D C24E H24K 109.5 . . ? H24I C24E H24K 109.5 . . ? C24D C24E H24J 109.5 . . ? H24I C24E H24J 109.5 . . ? H24K C24E H24J 109.5 . . ? C24D C24F H24N 109.5 . . ? C24D C24F H24M 109.5 . . ? H24N C24F H24M 109.5 . . ? C24D C24F H24L 109.5 . . ? H24N C24F H24L 109.5 . . ? H24M C24F H24L 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 W1 C11 O11 -149(8) . . . . ? C14 W1 C11 O11 120(8) . . . . ? C12 W1 C11 O11 -59(8) . . . . ? C13 W1 C11 O11 41(9) . . . . ? C16 W1 C11 O11 26(8) . . . . ? C15 W1 C12 O12 85(27) . . . . ? C14 W1 C12 O12 -69(39) . . . . ? C13 W1 C12 O12 178(100) . . . . ? C11 W1 C12 O12 -10(27) . . . . ? C16 W1 C12 O12 -97(27) . . . . ? C15 W1 C13 O13 -179(100) . . . . ? C14 W1 C13 O13 -89(9) . . . . ? C12 W1 C13 O13 91(9) . . . . ? C11 W1 C13 O13 -10(10) . . . . ? C16 W1 C13 O13 5(9) . . . . ? C15 W1 C14 O14 -1(25) . . . . ? C12 W1 C14 O14 152(21) . . . . ? C13 W1 C14 O14 -94(25) . . . . ? C11 W1 C14 O14 93(25) . . . . ? C16 W1 C14 O14 -180(100) . . . . ? C14 W1 C15 O15 -155(10) . . . . ? C12 W1 C15 O15 26(10) . . . . ? C13 W1 C15 O15 -66(10) . . . . ? C11 W1 C15 O15 116(10) . . . . ? C16 W1 C15 O15 6(13) . . . . ? O121 Ti1 O16 C16 -62.0(8) . . . . ? O121 Ti1 O16 C16 38.3(8) 2_656 . . . ? O16 Ti1 O16 C16 167.6(8) 2_656 . . . ? N111 Ti1 O16 C16 -149.3(8) . . . . ? N111 Ti1 O16 C16 124.2(8) 2_656 . . . ? Ti1 O16 C16 C17 -40.5(10) . . . . ? Ti1 O16 C16 W1 139.0(6) . . . . ? C15 W1 C16 O16 -17(3) . . . . ? C14 W1 C16 O16 143.8(4) . . . . ? C12 W1 C16 O16 -36.5(4) . . . . ? C13 W1 C16 O16 55.3(4) . . . . ? C11 W1 C16 O16 -126.7(4) . . . . ? C15 W1 C16 C17 162(3) . . . . ? C14 W1 C16 C17 -36.7(5) . . . . ? C12 W1 C16 C17 142.9(5) . . . . ? C13 W1 C16 C17 -125.3(5) . . . . ? C11 W1 C16 C17 52.8(5) . . . . ? C25 W2 C21 O21 -143(35) . . . . ? C24 W2 C21 O21 126(35) . . . . ? C23 W2 C21 O21 2(37) . . . . ? C22 W2 C21 O21 -53(35) . . . . ? C26 W2 C21 O21 37(35) . . . . ? C25 W2 C22 O22 58(21) . . . . ? C24 W2 C22 O22 -137(20) . . . . ? C21 W2 C22 O22 -33(21) . . . . ? C23 W2 C22 O22 150(21) . . . . ? C26 W2 C22 O22 -120(21) . . . . ? C25 W2 C23 O23 7(22) . . . . ? C24 W2 C23 O23 98(22) . . . . ? C21 W2 C23 O23 -138(21) . . . . ? C22 W2 C23 O23 -83(22) . . . . ? C26 W2 C23 O23 -173(100) . . . . ? C25 W2 C24 O24 -2(32) . . . . ? C21 W2 C24 O24 89(32) . . . . ? C23 W2 C24 O24 -94(32) . . . . ? C22 W2 C24 O24 -167(100) . . . . ? C26 W2 C24 O24 176(100) . . . . ? C24 W2 C25 O25 47(100) . . . . ? C21 W2 C25 O25 -44(100) . . . . ? C23 W2 C25 O25 138(100) . . . . ? C22 W2 C25 O25 -134(100) . . . . ? C26 W2 C25 O25 -45(100) . . . . ? O241 Ti2 O26 C26 -41.8(6) . . . . ? O231 Ti2 O26 C26 61.4(5) . . . . ? O36 Ti2 O26 C26 -167.1(5) . . . . ? N221 Ti2 O26 C26 149.1(5) . . . . ? N212 Ti2 O26 C26 -128.2(5) . . . . ? Ti2 O26 C26 C27 6.5(8) . . . . ? Ti2 O26 C26 W2 -177.7(3) . . . . ? C25 W2 C26 O26 -52(6) . . . . ? C24 W2 C26 O26 -142.8(4) . . . . ? C21 W2 C26 O26 -52.0(4) . . . . ? C23 W2 C26 O26 125.9(4) . . . . ? C22 W2 C26 O26 37.5(4) . . . . ? C25 W2 C26 C27 124(6) . . . . ? C24 W2 C26 C27 32.7(4) . . . . ? C21 W2 C26 C27 123.5(5) . . . . ? C23 W2 C26 C27 -58.6(4) . . . . ? C22 W2 C26 C27 -147.0(5) . . . . ? C35 W3 C31 O31 99(54) . . . . ? C34 W3 C31 O31 11(54) . . . . ? C33 W3 C31 O31 -74(56) . . . . ? C32 W3 C31 O31 -170(100) . . . . ? C36 W3 C31 O31 -77(54) . . . . ? C35 W3 C32 O32 -57(43) . . . . ? C34 W3 C32 O32 -29(55) . . . . ? C33 W3 C32 O32 37(43) . . . . ? C31 W3 C32 O32 -148(43) . . . . ? C36 W3 C32 O32 124(43) . . . . ? C35 W3 C33 O33 178(100) . . . . ? C34 W3 C33 O33 -95(29) . . . . ? C32 W3 C33 O33 86(29) . . . . ? C31 W3 C33 O33 -10(34) . . . . ? C36 W3 C33 O33 -7(29) . . . . ? C35 W3 C34 O34 16(52) . . . . ? C33 W3 C34 O34 -78(52) . . . . ? C32 W3 C34 O34 -12(64) . . . . ? C31 W3 C34 O34 106(52) . . . . ? C36 W3 C34 O34 -166(52) . . . . ? C34 W3 C35 O35 -8(13) . . . . ? C33 W3 C35 O35 81(13) . . . . ? C32 W3 C35 O35 172(13) . . . . ? C31 W3 C35 O35 -99(13) . . . . ? C36 W3 C35 O35 -23(17) . . . . ? O241 Ti2 O36 C36 55.5(8) . . . . ? O231 Ti2 O36 C36 -47.7(9) . . . . ? O26 Ti2 O36 C36 -178.1(7) . . . . ? N221 Ti2 O36 C36 -134.0(9) . . . . ? N212 Ti2 O36 C36 143.3(9) . . . . ? Ti2 O36 C36 C37 22.8(13) . . . . ? Ti2 O36 C36 W3 -152.8(5) . . . . ? C35 W3 C36 O36 59(5) . . . . ? C34 W3 C36 O36 43.5(6) . . . . ? C33 W3 C36 O36 -45.3(7) . . . . ? C32 W3 C36 O36 -136.0(7) . . . . ? C31 W3 C36 O36 134.5(6) . . . . ? C35 W3 C36 C37 -117(5) . . . . ? C34 W3 C36 C37 -131.6(8) . . . . ? C33 W3 C36 C37 139.6(9) . . . . ? C32 W3 C36 C37 48.9(9) . . . . ? C31 W3 C36 C37 -40.6(8) . . . . ? O121 Ti1 N111 C116 -132.0(5) . . . . ? O121 Ti1 N111 C116 78.9(13) 2_656 . . . ? O16 Ti1 N111 C116 126.8(5) 2_656 . . . ? O16 Ti1 N111 C116 -37.6(5) . . . . ? N111 Ti1 N111 C116 43.1(4) 2_656 . . . ? O121 Ti1 N111 C112 39.4(4) . . . . ? O121 Ti1 N111 C112 -109.7(12) 2_656 . . . ? O16 Ti1 N111 C112 -61.8(4) 2_656 . . . ? O16 Ti1 N111 C112 133.7(4) . . . . ? N111 Ti1 N111 C112 -145.5(5) 2_656 . . . ? C116 N111 C112 C113 0.7(9) . . . . ? Ti1 N111 C112 C113 -171.4(5) . . . . ? N111 C112 C113 C114 0.0(10) . . . . ? C112 C113 C114 C115 -0.7(9) . . . . ? C113 C114 C115 C116 0.7(9) . . . . ? C112 N111 C116 C115 -0.7(9) . . . . ? Ti1 N111 C116 C115 170.8(4) . . . . ? C114 C115 C116 N111 0.0(9) . . . . ? O121 Ti1 O121 C122 -20.3(8) 2_656 . . . ? O16 Ti1 O121 C122 -116.3(9) 2_656 . . . ? O16 Ti1 O121 C122 81.1(9) . . . . ? N111 Ti1 O121 C122 164.0(9) . . . . ? N111 Ti1 O121 C122 128.3(12) 2_656 . . . ? Ti1 O121 C122 C124 -47.9(11) . . . . ? Ti1 O121 C122 C123 -170.7(7) . . . . ? O241 Ti2 N212 C213 -45.0(5) . . . . ? O231 Ti2 N212 C213 111.0(10) . . . . ? O36 Ti2 N212 C213 -138.2(5) . . . . ? O26 Ti2 N212 C213 55.5(4) . . . . ? N221 Ti2 N212 C213 140.1(5) . . . . ? O241 Ti2 N212 C217 125.1(5) . . . . ? O231 Ti2 N212 C217 -79.0(11) . . . . ? O36 Ti2 N212 C217 31.8(5) . . . . ? O26 Ti2 N212 C217 -134.4(5) . . . . ? N221 Ti2 N212 C217 -49.8(5) . . . . ? C217 N212 C213 C214 -2.0(9) . . . . ? Ti2 N212 C213 C214 168.9(5) . . . . ? N212 C213 C214 C215 0.3(11) . . . . ? C213 C214 C215 C216 2.1(11) . . . . ? C214 C215 C216 C217 -2.4(11) . . . . ? C213 N212 C217 C216 1.5(9) . . . . ? Ti2 N212 C217 C216 -168.8(5) . . . . ? C215 C216 C217 N212 0.6(11) . . . . ? O241 Ti2 N221 C222 -77.2(10) . . . . ? O231 Ti2 N221 C222 124.2(5) . . . . ? O36 Ti2 N221 C222 -134.3(5) . . . . ? O26 Ti2 N221 C222 30.4(4) . . . . ? N212 Ti2 N221 C222 -50.2(5) . . . . ? O241 Ti2 N221 C226 107.9(10) . . . . ? O231 Ti2 N221 C226 -50.7(4) . . . . ? O36 Ti2 N221 C226 50.8(4) . . . . ? O26 Ti2 N221 C226 -144.5(4) . . . . ? N212 Ti2 N221 C226 134.9(4) . . . . ? C226 N221 C222 C223 -0.4(8) . . . . ? Ti2 N221 C222 C223 -175.4(4) . . . . ? N221 C222 C223 C224 0.2(9) . . . . ? C222 C223 C224 C225 0.3(9) . . . . ? C223 C224 C225 C226 -0.7(9) . . . . ? C222 N221 C226 C225 0.0(8) . . . . ? Ti2 N221 C226 C225 175.3(4) . . . . ? C224 C225 C226 N221 0.5(9) . . . . ? O241 Ti2 O231 C232 151.6(13) . . . . ? O36 Ti2 O231 C232 -112.8(13) . . . . ? O26 Ti2 O231 C232 50.6(13) . . . . ? N221 Ti2 O231 C232 -32.6(13) . . . . ? N212 Ti2 O231 C232 -3.7(19) . . . . ? Ti2 O231 C232 C233 -34.0(16) . . . . ? Ti2 O231 C232 C234 -156.5(11) . . . . ? O231 Ti2 O241 C24A 107.7(16) . . . . ? O36 Ti2 O241 C24A 5.7(16) . . . . ? O26 Ti2 O241 C24A -156.4(16) . . . . ? N221 Ti2 O241 C24A -50(2) . . . . ? N212 Ti2 O241 C24A -77.1(16) . . . . ? O231 Ti2 O241 C24D -150(21) . . . . ? O36 Ti2 O241 C24D 108(21) . . . . ? O26 Ti2 O241 C24D -54(21) . . . . ? N221 Ti2 O241 C24D 52(21) . . . . ? N212 Ti2 O241 C24D 25(21) . . . . ? C24D O241 C24A C24B -58(3) . . . . ? Ti2 O241 C24A C24B 117(2) . . . . ? C24D O241 C24A C24C 46(3) . . . . ? Ti2 O241 C24A C24C -138.3(14) . . . . ? C24A O241 C24D C24E 45(2) . . . . ? Ti2 O241 C24D C24E -62(21) . . . . ? C24A O241 C24D C24F -53(2) . . . . ? Ti2 O241 C24D C24F -160(21) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.86 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 3.152 _refine_diff_density_min -4.027 _refine_diff_density_rms 0.165 #===END data_Cl2Ti(OiPr)2(C5H5N)2 _database_code_depnum_ccdc_archive 'CCDC 670777' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H24 Cl2 N2 O2 Ti' _chemical_formula_sum 'C16 H24 Cl2 N2 O2 Ti' _chemical_formula_weight 395.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.7977(5) _cell_length_b 13.4237(7) _cell_length_c 16.4837(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.9060(10) _cell_angle_gamma 90.00 _cell_volume 1928.18(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5129 _cell_measurement_theta_min 2.337 _cell_measurement_theta_max 26.311 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7122 _exptl_absorpt_correction_T_max 0.8677 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10977 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.35 _reflns_number_total 3908 _reflns_number_gt 3471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 two isopropoxide groups are disordered. PART instructions and similarity restraints (SAME-instruction in Shelxl) were applied to model the disorder as best as possible. ; _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^)+(0.0558P)^2^+1.0083P] 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 3908 _refine_ls_number_parameters 270 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.027 _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 0.73112(4) 0.87167(2) 0.24866(2) 0.02478(12) Uani 1 1 d . A . Cl1 Cl 0.92871(5) 0.82076(4) 0.17129(3) 0.03081(14) Uani 1 1 d . . . Cl2 Cl 0.58746(5) 0.91299(4) 0.35573(3) 0.03414(14) Uani 1 1 d . . . N11 N 0.93631(18) 0.93263(13) 0.33728(10) 0.0283(4) Uani 1 1 d . . . C12 C 1.0704(2) 0.8839(2) 0.35609(13) 0.0412(5) Uani 1 1 d . . . H12 H 1.0805 0.8190 0.3346 0.049 Uiso 1 1 calc R . . C13 C 1.1944(3) 0.9255(3) 0.40584(15) 0.0554(8) Uani 1 1 d . . . H13 H 1.2873 0.8890 0.4181 0.066 Uiso 1 1 calc R . . C14 C 1.1823(3) 1.0191(2) 0.43717(15) 0.0608(9) Uani 1 1 d . . . H14 H 1.2654 1.0482 0.4720 0.073 Uiso 1 1 calc R . . C15 C 1.0474(3) 1.0695(2) 0.41702(14) 0.0520(7) Uani 1 1 d . . . H15 H 1.0364 1.1353 0.4366 0.062 Uiso 1 1 calc R . . C16 C 0.9274(3) 1.02416(16) 0.36800(12) 0.0367(5) Uani 1 1 d . . . H16 H 0.8338 1.0598 0.3555 0.044 Uiso 1 1 calc R . . N21 N 0.79294(19) 0.72845(12) 0.32159(10) 0.0288(4) Uani 1 1 d . . . C22 C 0.8019(3) 0.64245(15) 0.28004(13) 0.0368(5) Uani 1 1 d . . . H22 H 0.7819 0.6442 0.2219 0.044 Uiso 1 1 calc R . . C23 C 0.8380(4) 0.55325(19) 0.31719(15) 0.0581(8) Uani 1 1 d . . . H23 H 0.8446 0.4947 0.2855 0.070 Uiso 1 1 calc R . . C24 C 0.8649(5) 0.5494(2) 0.40189(17) 0.0866(13) Uani 1 1 d . . . H24 H 0.8907 0.4883 0.4293 0.104 Uiso 1 1 calc R . . C25 C 0.8537(5) 0.6362(2) 0.44583(15) 0.0747(11) Uani 1 1 d . . . H25 H 0.8706 0.6357 0.5040 0.090 Uiso 1 1 calc R . . C26 C 0.8177(3) 0.72315(17) 0.40362(13) 0.0420(5) Uani 1 1 d . . . H26 H 0.8099 0.7826 0.4341 0.050 Uiso 1 1 calc R . . O31 O 0.58523(15) 0.80229(11) 0.18840(8) 0.0303(3) Uani 1 1 d D . . C32A C 0.4868(3) 0.8022(3) 0.11421(18) 0.0341(10) Uani 0.695(8) 1 d PD A 1 H32A H 0.4975 0.8673 0.0861 0.041 Uiso 0.695(8) 1 calc PR A 1 C33A C 0.3230(5) 0.7931(10) 0.1331(7) 0.075(4) Uani 0.695(8) 1 d PD A 1 H33A H 0.3067 0.7260 0.1538 0.113 Uiso 0.695(8) 1 calc PR A 1 H33B H 0.2513 0.8048 0.0830 0.113 Uiso 0.695(8) 1 calc PR A 1 H33C H 0.3054 0.8424 0.1746 0.113 Uiso 0.695(8) 1 calc PR A 1 C34A C 0.5254(12) 0.7206(11) 0.0596(6) 0.073(4) Uani 0.695(8) 1 d PD A 1 H34A H 0.6343 0.7247 0.0531 0.109 Uiso 0.695(8) 1 calc PR A 1 H34B H 0.4628 0.7272 0.0059 0.109 Uiso 0.695(8) 1 calc PR A 1 H34C H 0.5046 0.6562 0.0837 0.109 Uiso 0.695(8) 1 calc PR A 1 C32B C 0.4864(8) 0.7393(6) 0.1395(5) 0.045(3) Uani 0.305(8) 1 d PD A 2 H32B H 0.4828 0.6740 0.1685 0.054 Uiso 0.305(8) 1 calc PR A 2 C33B C 0.3250(11) 0.7818(16) 0.1250(9) 0.037(4) Uani 0.305(8) 1 d PD A 2 H33D H 0.2852 0.7879 0.1775 0.056 Uiso 0.305(8) 1 calc PR A 2 H33E H 0.2585 0.7374 0.0887 0.056 Uiso 0.305(8) 1 calc PR A 2 H33F H 0.3273 0.8477 0.0996 0.056 Uiso 0.305(8) 1 calc PR A 2 C34B C 0.548(2) 0.722(2) 0.0612(10) 0.049(6) Uani 0.305(8) 1 d PD A 2 H34D H 0.5393 0.7828 0.0284 0.074 Uiso 0.305(8) 1 calc PR A 2 H34E H 0.4898 0.6682 0.0307 0.074 Uiso 0.305(8) 1 calc PR A 2 H34F H 0.6565 0.7022 0.0729 0.074 Uiso 0.305(8) 1 calc PR A 2 O41 O 0.70967(16) 0.99036(10) 0.20295(8) 0.0327(3) Uani 1 1 d D . . C42A C 0.7219(6) 1.0840(3) 0.1710(3) 0.0409(12) Uani 0.526(5) 1 d PD A 1 H42A H 0.8084 1.1197 0.2046 0.049 Uiso 0.526(5) 1 calc PR A 1 C43A C 0.5772(8) 1.1406(5) 0.1749(4) 0.078(2) Uani 0.526(5) 1 d PD A 1 H43A H 0.4949 1.1127 0.1353 0.118 Uiso 0.526(5) 1 calc PR A 1 H43B H 0.5928 1.2107 0.1617 0.118 Uiso 0.526(5) 1 calc PR A 1 H43C H 0.5488 1.1356 0.2302 0.118 Uiso 0.526(5) 1 calc PR A 1 C44A C 0.7566(6) 1.0755(4) 0.0856(3) 0.0549(15) Uani 0.526(5) 1 d PD A 1 H44A H 0.8530 1.0390 0.0854 0.082 Uiso 0.526(5) 1 calc PR A 1 H44B H 0.7664 1.1422 0.0629 0.082 Uiso 0.526(5) 1 calc PR A 1 H44C H 0.6733 1.0396 0.0523 0.082 Uiso 0.526(5) 1 calc PR A 1 C42B C 0.6298(6) 1.0761(3) 0.1754(4) 0.0472(15) Uani 0.474(5) 1 d PD A 2 H42B H 0.5558 1.0915 0.2147 0.057 Uiso 0.474(5) 1 calc PR A 2 C43B C 0.7263(6) 1.1664(3) 0.1691(3) 0.0446(14) Uani 0.474(5) 1 d PD A 2 H43D H 0.7923 1.1772 0.2213 0.067 Uiso 0.474(5) 1 calc PR A 2 H43E H 0.6599 1.2245 0.1564 0.067 Uiso 0.474(5) 1 calc PR A 2 H43F H 0.7902 1.1568 0.1255 0.067 Uiso 0.474(5) 1 calc PR A 2 C44B C 0.5384(13) 1.0514(7) 0.0944(6) 0.171(7) Uani 0.474(5) 1 d PD A 2 H44D H 0.6083 1.0348 0.0550 0.256 Uiso 0.474(5) 1 calc PR A 2 H44E H 0.4754 1.1089 0.0745 0.256 Uiso 0.474(5) 1 calc PR A 2 H44F H 0.4717 0.9942 0.1009 0.256 Uiso 0.474(5) 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 0.02747(19) 0.0248(2) 0.02136(19) -0.00168(13) 0.00077(14) -0.00035(13) Cl1 0.0322(3) 0.0377(3) 0.0235(2) -0.00189(19) 0.00730(19) -0.00067(19) Cl2 0.0272(2) 0.0434(3) 0.0324(3) -0.0108(2) 0.00627(19) 0.0004(2) N11 0.0276(8) 0.0365(9) 0.0207(8) 0.0013(7) 0.0026(6) -0.0066(7) C12 0.0268(10) 0.0680(16) 0.0288(11) -0.0001(10) 0.0038(9) -0.0030(10) C13 0.0260(11) 0.107(2) 0.0321(13) 0.0070(14) -0.0001(9) -0.0130(13) C14 0.0537(16) 0.094(2) 0.0311(13) 0.0082(14) -0.0065(11) -0.0456(16) C15 0.0728(18) 0.0523(15) 0.0275(12) 0.0040(10) -0.0056(12) -0.0358(13) C16 0.0493(13) 0.0352(11) 0.0242(10) 0.0045(8) 0.0005(9) -0.0121(10) N21 0.0386(9) 0.0281(8) 0.0200(8) -0.0007(6) 0.0053(7) 0.0019(7) C22 0.0562(13) 0.0317(11) 0.0233(10) -0.0016(8) 0.0086(9) 0.0056(10) C23 0.110(2) 0.0324(12) 0.0322(13) -0.0015(10) 0.0103(14) 0.0183(14) C24 0.189(4) 0.0342(14) 0.0341(14) 0.0085(12) 0.0059(19) 0.0274(19) C25 0.158(3) 0.0428(15) 0.0206(12) 0.0045(10) 0.0046(16) 0.0166(18) C26 0.0723(16) 0.0311(11) 0.0227(10) -0.0016(9) 0.0068(10) 0.0020(11) O31 0.0291(7) 0.0360(8) 0.0248(7) -0.0054(6) 0.0001(6) -0.0024(6) C32A 0.0315(16) 0.041(2) 0.0276(16) -0.0004(14) -0.0044(12) -0.0039(13) C33A 0.022(4) 0.101(8) 0.099(8) 0.005(5) -0.002(3) 0.000(3) C34A 0.072(7) 0.086(7) 0.054(6) -0.033(5) -0.014(4) 0.020(6) C32B 0.041(4) 0.030(5) 0.058(6) 0.004(4) -0.015(4) 0.001(3) C33B 0.038(9) 0.055(8) 0.018(5) 0.000(5) 0.001(5) 0.002(6) C34B 0.024(5) 0.098(16) 0.024(8) -0.037(8) -0.002(4) -0.003(6) O41 0.0418(8) 0.0291(7) 0.0269(7) 0.0019(6) 0.0031(6) 0.0051(6) C42A 0.037(3) 0.038(3) 0.044(3) 0.0076(19) -0.006(2) -0.007(2) C43A 0.112(6) 0.065(4) 0.058(4) 0.003(3) 0.011(4) 0.050(4) C44A 0.063(3) 0.058(3) 0.044(3) 0.013(2) 0.013(2) 0.002(2) C42B 0.031(3) 0.040(3) 0.068(4) 0.026(3) 0.000(3) 0.003(3) C43B 0.056(3) 0.024(3) 0.053(3) 0.005(2) 0.006(3) -0.001(2) C44B 0.178(10) 0.133(8) 0.155(9) 0.113(8) -0.141(9) -0.115(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 O41 1.7614(14) . ? Ti1 O31 1.7750(14) . ? Ti1 N21 2.2930(17) . ? Ti1 N11 2.3102(16) . ? Ti1 Cl2 2.3736(6) . ? Ti1 Cl1 2.3927(6) . ? N11 C16 1.335(3) . ? N11 C12 1.347(3) . ? C12 C13 1.388(3) . ? C12 H12 0.9500 . ? C13 C14 1.368(4) . ? C13 H13 0.9500 . ? C14 C15 1.367(4) . ? C14 H14 0.9500 . ? C15 C16 1.380(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 C26 1.341(3) . ? N21 C22 1.350(3) . ? C22 C23 1.362(3) . ? C22 H22 0.9500 . ? C23 C24 1.385(4) . ? C23 H23 0.9500 . ? C24 C25 1.382(4) . ? C24 H24 0.9500 . ? C25 C26 1.373(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? O31 C32B 1.389(5) . ? O31 C32A 1.398(3) . ? C32A C34A 1.487(8) . ? C32A C33A 1.520(6) . ? C32A H32A 1.0000 . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 0.9800 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C32B C34B 1.487(8) . ? C32B C33B 1.518(7) . ? C32B H32B 1.0000 . ? C33B H33D 0.9800 . ? C33B H33E 0.9800 . ? C33B H33F 0.9800 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? O41 C42A 1.372(4) . ? O41 C42B 1.392(4) . ? C42A C44A 1.485(6) . ? C42A C43A 1.492(6) . ? C42A H42A 1.0000 . ? C43A H43A 0.9800 . ? C43A H43B 0.9800 . ? C43A H43C 0.9800 . ? C44A H44A 0.9800 . ? C44A H44B 0.9800 . ? C44A H44C 0.9800 . ? C42B C43B 1.491(6) . ? C42B C44B 1.498(8) . ? C42B H42B 1.0000 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? C44B H44D 0.9800 . ? C44B H44E 0.9800 . ? C44B H44F 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 O41 Ti1 O31 102.04(7) . . ? O41 Ti1 N21 170.55(6) . . ? O31 Ti1 N21 87.40(6) . . ? O41 Ti1 N11 88.77(6) . . ? O31 Ti1 N11 169.03(6) . . ? N21 Ti1 N11 81.79(6) . . ? O41 Ti1 Cl2 94.02(5) . . ? O31 Ti1 Cl2 96.93(5) . . ? N21 Ti1 Cl2 85.31(4) . . ? N11 Ti1 Cl2 84.07(4) . . ? O41 Ti1 Cl1 94.20(5) . . ? O31 Ti1 Cl1 94.27(5) . . ? N21 Ti1 Cl1 84.41(4) . . ? N11 Ti1 Cl1 82.90(4) . . ? Cl2 Ti1 Cl1 164.42(2) . . ? C16 N11 C12 117.04(19) . . ? C16 N11 Ti1 118.95(14) . . ? C12 N11 Ti1 123.86(15) . . ? N11 C12 C13 122.2(3) . . ? N11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C14 C13 C12 119.7(3) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 118.2(2) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? C14 C15 C16 119.5(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? N11 C16 C15 123.2(2) . . ? N11 C16 H16 118.4 . . ? C15 C16 H16 118.4 . . ? C26 N21 C22 116.96(17) . . ? C26 N21 Ti1 124.53(14) . . ? C22 N21 Ti1 118.50(13) . . ? N21 C22 C23 123.3(2) . . ? N21 C22 H22 118.3 . . ? C23 C22 H22 118.3 . . ? C22 C23 C24 118.9(2) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C25 C24 C23 118.9(2) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C26 C25 C24 118.6(2) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? N21 C26 C25 123.4(2) . . ? N21 C26 H26 118.3 . . ? C25 C26 H26 118.3 . . ? C32B O31 C32A 39.5(4) . . ? C32B O31 Ti1 172.4(3) . . ? C32A O31 Ti1 143.44(19) . . ? O31 C32A C34A 111.4(5) . . ? O31 C32A C33A 108.2(5) . . ? C34A C32A C33A 111.5(6) . . ? O31 C32A H32A 108.6 . . ? C34A C32A H32A 108.6 . . ? C33A C32A H32A 108.6 . . ? O31 C32B C34B 109.0(13) . . ? O31 C32B C33B 111.0(9) . . ? C34B C32B C33B 111.7(8) . . ? O31 C32B H32B 108.3 . . ? C34B C32B H32B 108.3 . . ? C33B C32B H32B 108.3 . . ? C32B C33B H33D 109.5 . . ? C32B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C32B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C32B C34B H34D 109.5 . . ? C32B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C32B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C42A O41 C42B 34.9(3) . . ? C42A O41 Ti1 169.4(2) . . ? C42B O41 Ti1 155.1(3) . . ? O41 C42A C44A 109.3(4) . . ? O41 C42A C43A 109.8(4) . . ? C44A C42A C43A 111.6(4) . . ? O41 C42A H42A 108.7 . . ? C44A C42A H42A 108.7 . . ? C43A C42A H42A 108.7 . . ? O41 C42B C43B 115.4(4) . . ? O41 C42B C44B 106.9(5) . . ? C43B C42B C44B 111.0(5) . . ? O41 C42B H42B 107.7 . . ? C43B C42B H42B 107.7 . . ? C44B C42B H42B 107.7 . . ? C42B C43B H43D 109.5 . . ? C42B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C42B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C42B C44B H44D 109.5 . . ? C42B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C42B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O41 Ti1 N11 C16 40.22(15) . . . . ? O31 Ti1 N11 C16 -149.8(3) . . . . ? N21 Ti1 N11 C16 -140.04(15) . . . . ? Cl2 Ti1 N11 C16 -53.95(14) . . . . ? Cl1 Ti1 N11 C16 134.61(14) . . . . ? O41 Ti1 N11 C12 -135.12(16) . . . . ? O31 Ti1 N11 C12 34.9(4) . . . . ? N21 Ti1 N11 C12 44.62(16) . . . . ? Cl2 Ti1 N11 C12 130.72(16) . . . . ? Cl1 Ti1 N11 C12 -40.73(16) . . . . ? C16 N11 C12 C13 0.7(3) . . . . ? Ti1 N11 C12 C13 176.12(16) . . . . ? N11 C12 C13 C14 -0.2(4) . . . . ? C12 C13 C14 C15 -1.0(4) . . . . ? C13 C14 C15 C16 1.7(4) . . . . ? C12 N11 C16 C15 0.0(3) . . . . ? Ti1 N11 C16 C15 -175.63(16) . . . . ? C14 C15 C16 N11 -1.2(3) . . . . ? O41 Ti1 N21 C26 49.9(5) . . . . ? O31 Ti1 N21 C26 -133.51(19) . . . . ? N11 Ti1 N21 C26 48.34(18) . . . . ? Cl2 Ti1 N21 C26 -36.33(18) . . . . ? Cl1 Ti1 N21 C26 131.95(18) . . . . ? O41 Ti1 N21 C22 -131.7(4) . . . . ? O31 Ti1 N21 C22 44.81(16) . . . . ? N11 Ti1 N21 C22 -133.34(16) . . . . ? Cl2 Ti1 N21 C22 141.99(16) . . . . ? Cl1 Ti1 N21 C22 -49.74(15) . . . . ? C26 N21 C22 C23 -1.7(4) . . . . ? Ti1 N21 C22 C23 179.8(2) . . . . ? N21 C22 C23 C24 1.0(5) . . . . ? C22 C23 C24 C25 0.2(6) . . . . ? C23 C24 C25 C26 -0.6(6) . . . . ? C22 N21 C26 C25 1.3(4) . . . . ? Ti1 N21 C26 C25 179.6(3) . . . . ? C24 C25 C26 N21 -0.1(5) . . . . ? O41 Ti1 O31 C32B 125(3) . . . . ? N21 Ti1 O31 C32B -54(3) . . . . ? N11 Ti1 O31 C32B -45(3) . . . . ? Cl2 Ti1 O31 C32B -139(3) . . . . ? Cl1 Ti1 O31 C32B 30(3) . . . . ? O41 Ti1 O31 C32A 16.7(3) . . . . ? N21 Ti1 O31 C32A -162.7(3) . . . . ? N11 Ti1 O31 C32A -153.1(3) . . . . ? Cl2 Ti1 O31 C32A 112.3(3) . . . . ? Cl1 Ti1 O31 C32A -78.5(3) . . . . ? C32B O31 C32A C34A -54.8(9) . . . . ? Ti1 O31 C32A C34A 113.9(7) . . . . ? C32B O31 C32A C33A 68.1(8) . . . . ? Ti1 O31 C32A C33A -123.2(6) . . . . ? C32A O31 C32B C34B 65.4(13) . . . . ? Ti1 O31 C32B C34B -52(4) . . . . ? C32A O31 C32B C33B -58.1(9) . . . . ? Ti1 O31 C32B C33B -176(3) . . . . ? O31 Ti1 O41 C42A -146.1(12) . . . . ? N21 Ti1 O41 C42A 30.4(14) . . . . ? N11 Ti1 O41 C42A 32.0(12) . . . . ? Cl2 Ti1 O41 C42A 115.9(12) . . . . ? Cl1 Ti1 O41 C42A -50.8(12) . . . . ? O31 Ti1 O41 C42B 55.8(6) . . . . ? N21 Ti1 O41 C42B -127.7(7) . . . . ? N11 Ti1 O41 C42B -126.1(6) . . . . ? Cl2 Ti1 O41 C42B -42.1(6) . . . . ? Cl1 Ti1 O41 C42B 151.1(6) . . . . ? C42B O41 C42A C44A -110.2(7) . . . . ? Ti1 O41 C42A C44A 85.8(12) . . . . ? C42B O41 C42A C43A 12.5(5) . . . . ? Ti1 O41 C42A C43A -151.5(10) . . . . ? C42A O41 C42B C43B -16.9(4) . . . . ? Ti1 O41 C42B C43B 156.2(4) . . . . ? C42A O41 C42B C44B 107.1(8) . . . . ? Ti1 O41 C42B C44B -79.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.596 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.068