Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name _publ_author_address R.Fandos ; Departamento de Quimica Inorganica, Organica y Bioquimica Universidad de Castilla-La Mancha Facultad de Ciencias del Medio Ambiente Avda Carlos III s/n 45071-Toledo Spain ; B.Gallego ; Departamento de Quimica Inorganica, Organica y Bioquimica Universidad de Castilla-La Mancha Facultad de Ciencias del Medio Ambiente Avda Carlos III s/n 45071-Toledo Spain ; A.Otero ; Departamento de Quimica Inorganica, Organica y Bioquimica Universidad de Castilla-La Mancha Facultad de Quimicas Campus de Ciudad Real Avda. Camilo Jose Cela s/n 13071-Ciudad Real Spain ; A.M.Rodriguez ; Departamento de Quimica Inorganica, Organica y Bioquimica Universidad de Castilla-La Mancha ETS Ingenieros Industriales Campus de Ciudad Real Avda. Camilo Jose Cela 3 13071-Ciudad Real Spain ; M.J.Ruiz ; ? ; _publ_contact_author_name 'Antonio Otero' _publ_contact_author_address ; Dept de Quimica Inorg. Organica y B Facultad de Ciencias Quimicas Univ. de Castilla-La-Mancha CIUDAD REAL CIUDAD REAL 13017 SPAIN ; _publ_contact_author_email AnaMaria.RFdez@uclm.es _publ_requested_journal 'Dalton Transactions' _publ_section_title ; A New Building Block for Early-Late Heterometallic Complexes; Preparation of a New Tetrameric Metallomacrocycle by Self Assembly ; #============================================================================ data_3 _database_code_depnum_ccdc_archive 'CCDC 296373' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H36 N2 O9 Ti2, H2 O' _chemical_formula_sum 'C34 H38 N2 O10 Ti2' _chemical_formula_weight 730.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.210(2) _cell_length_b 14.420(3) _cell_length_c 14.711(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.87(3) _cell_angle_gamma 90.00 _cell_volume 3323.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(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 'four circle diffractometer Nonius-Mach3' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 4141 _diffrn_reflns_av_R_equivalents 0.0077 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.98 _reflns_number_total 3988 _reflns_number_gt 3361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (control program)' _computing_cell_refinement 'Nonius (control program)' _computing_data_reduction 'XCAD4 (Harms, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0851P)^2^+1.7950P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3988 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.233 _refine_ls_shift/su_mean 0.010 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 0.41196(2) 0.31360(2) 0.28457(2) 0.03211(13) Uani 1 1 d . . . O1 O 0.5000 0.36691(15) 0.2500 0.0486(5) Uani 1 2 d S . . O2 O 0.40124(11) 0.21668(11) 0.18108(10) 0.0456(4) Uani 1 1 d . . . O3 O 0.45919(11) 0.32744(11) 0.42510(11) 0.0490(4) Uani 1 1 d . . . O4 O 0.37900(15) 0.07021(13) 0.13032(13) 0.0702(6) Uani 1 1 d . . . O5 O 0.47735(18) 0.2725(2) 0.57160(13) 0.0880(8) Uani 1 1 d . . . N1 N 0.40688(11) 0.17983(11) 0.34631(12) 0.0368(4) Uani 1 1 d . . . C1 C 0.39086(13) 0.10484(15) 0.29153(16) 0.0418(4) Uani 1 1 d . . . C2 C 0.38403(16) 0.01841(17) 0.3293(2) 0.0585(7) Uani 1 1 d . . . H2 H 0.3726 -0.0340 0.2913 0.070 Uiso 1 1 calc . . . C3 C 0.39478(17) 0.0123(2) 0.4254(2) 0.0638(8) Uani 1 1 d . . . H3 H 0.3872 -0.0445 0.4520 0.077 Uiso 1 1 calc . . . C4 C 0.41646(16) 0.0888(2) 0.48210(18) 0.0577(7) Uani 1 1 d . . . H4 H 0.4260 0.0841 0.5470 0.069 Uiso 1 1 calc . . . C5 C 0.42379(14) 0.17314(17) 0.43993(16) 0.0442(5) Uani 1 1 d . . . C6 C 0.38862(15) 0.12900(15) 0.19127(16) 0.0451(5) Uani 1 1 d . . . C7 C 0.45577(16) 0.26404(19) 0.48614(15) 0.0523(6) Uani 1 1 d . . . C10 C 0.26069(15) 0.32289(17) 0.22664(19) 0.0500(5) Uani 1 1 d . . . C11 C 0.28226(16) 0.3641(2) 0.31671(17) 0.0545(6) Uani 1 1 d . . . C12 C 0.33284(16) 0.44340(17) 0.31334(15) 0.0488(5) Uani 1 1 d . . . C13 C 0.34057(14) 0.45214(15) 0.22011(15) 0.0429(5) Uani 1 1 d . . . C14 C 0.29752(14) 0.37696(16) 0.16769(14) 0.0433(5) Uani 1 1 d . . . C15 C 0.20520(19) 0.2395(2) 0.1963(3) 0.0830(10) Uani 1 1 d . . . H15A H 0.1464 0.2582 0.1783 0.125 Uiso 1 1 calc R . . H15B H 0.2138 0.1962 0.2474 0.125 Uiso 1 1 calc R . . H15C H 0.2199 0.2107 0.1437 0.125 Uiso 1 1 calc R . . C16 C 0.2523(3) 0.3321(3) 0.3995(3) 0.0980(14) Uani 1 1 d . . . H16A H 0.2956 0.3443 0.4563 0.147 Uiso 1 1 calc R . . H16B H 0.2409 0.2667 0.3943 0.147 Uiso 1 1 calc R . . H16C H 0.2010 0.3647 0.4011 0.147 Uiso 1 1 calc R . . C17 C 0.3678(3) 0.5092(2) 0.3930(2) 0.0878(12) Uani 1 1 d . . . H17A H 0.3247 0.5537 0.3968 0.132 Uiso 1 1 calc R . . H17B H 0.4165 0.5408 0.3823 0.132 Uiso 1 1 calc R . . H17C H 0.3844 0.4751 0.4509 0.132 Uiso 1 1 calc R . . C18 C 0.3840(2) 0.52898(19) 0.1822(2) 0.0683(8) Uani 1 1 d . . . H18A H 0.4230 0.5033 0.1496 0.103 Uiso 1 1 calc R . . H18B H 0.4149 0.5671 0.2331 0.103 Uiso 1 1 calc R . . H18C H 0.3421 0.5659 0.1394 0.103 Uiso 1 1 calc R . . C19 C 0.2907(2) 0.3617(2) 0.06511(17) 0.0696(8) Uani 1 1 d . . . H19A H 0.2524 0.4065 0.0286 0.104 Uiso 1 1 calc R . . H19B H 0.2694 0.3004 0.0476 0.104 Uiso 1 1 calc R . . H19C H 0.3461 0.3683 0.0535 0.104 Uiso 1 1 calc R . . O6 O 0.0000 0.6731(4) 0.7500 0.1302(19) Uani 1 2 d S . . H1 H 0.017(8) 0.721(9) 0.814(7) 0.39(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0371(2) 0.0311(2) 0.02957(19) 0.00135(12) 0.01121(14) 0.00293(12) O1 0.0463(12) 0.0363(11) 0.0700(15) 0.000 0.0272(11) 0.000 O2 0.0662(10) 0.0398(8) 0.0331(7) -0.0014(6) 0.0167(7) 0.0057(7) O3 0.0573(10) 0.0476(9) 0.0360(8) -0.0060(6) 0.0010(7) 0.0049(7) O4 0.0946(15) 0.0520(10) 0.0547(10) -0.0195(9) 0.0024(10) 0.0085(10) O5 0.119(2) 0.1052(18) 0.0294(9) -0.0002(10) 0.0012(10) 0.0149(15) N1 0.0356(8) 0.0390(9) 0.0354(8) 0.0055(6) 0.0086(6) 0.0013(6) C1 0.0365(10) 0.0381(10) 0.0470(11) 0.0027(8) 0.0042(8) -0.0020(8) C2 0.0472(13) 0.0416(12) 0.0800(18) 0.0106(12) 0.0038(12) -0.0045(9) C3 0.0493(13) 0.0575(15) 0.083(2) 0.0361(15) 0.0144(13) 0.0006(11) C4 0.0483(12) 0.0732(17) 0.0545(14) 0.0323(13) 0.0186(10) 0.0143(12) C5 0.0390(10) 0.0566(13) 0.0369(10) 0.0129(9) 0.0093(8) 0.0089(9) C6 0.0476(11) 0.0403(11) 0.0431(11) -0.0056(9) 0.0036(9) 0.0063(9) C7 0.0552(13) 0.0665(15) 0.0310(10) 0.0008(10) 0.0032(9) 0.0135(11) C10 0.0383(11) 0.0537(13) 0.0567(14) 0.0093(10) 0.0098(10) 0.0077(9) C11 0.0510(13) 0.0727(16) 0.0472(12) 0.0205(11) 0.0259(10) 0.0271(12) C12 0.0618(14) 0.0493(12) 0.0346(10) -0.0031(9) 0.0108(9) 0.0227(10) C13 0.0518(12) 0.0384(10) 0.0379(10) 0.0050(8) 0.0102(9) 0.0117(9) C14 0.0475(11) 0.0472(11) 0.0329(10) 0.0019(8) 0.0060(8) 0.0114(9) C15 0.0465(15) 0.074(2) 0.119(3) 0.013(2) 0.0044(16) -0.0130(14) C16 0.084(2) 0.150(4) 0.081(2) 0.053(2) 0.059(2) 0.048(2) C17 0.131(3) 0.0696(19) 0.0496(15) -0.0232(14) -0.0020(17) 0.041(2) C18 0.0800(19) 0.0453(13) 0.080(2) 0.0219(13) 0.0202(16) 0.0055(13) C19 0.094(2) 0.0747(19) 0.0325(11) -0.0013(11) 0.0032(12) 0.0148(16) O6 0.190(6) 0.115(4) 0.090(3) 0.000 0.045(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.8051(10) . ? Ti1 O3 2.0217(17) . ? Ti1 O2 2.0410(16) . ? Ti1 N1 2.1427(17) . ? Ti1 C14 2.366(2) . ? Ti1 C12 2.368(2) . ? Ti1 C13 2.380(2) . ? Ti1 C11 2.384(2) . ? Ti1 C10 2.384(2) . ? Ti1 Ti1 3.2666(9) 2_655 ? O1 Ti1 1.8051(10) 2_655 ? O2 C6 1.296(3) . ? O3 C7 1.293(3) . ? O4 C6 1.215(3) . ? O5 C7 1.222(3) . ? N1 C1 1.334(3) . ? N1 C5 1.337(3) . ? C1 C2 1.380(3) . ? C1 C6 1.507(3) . ? C2 C3 1.382(4) . ? C3 C4 1.374(4) . ? C4 C5 1.384(3) . ? C5 C7 1.506(4) . ? C10 C14 1.408(3) . ? C10 C11 1.412(4) . ? C10 C15 1.500(4) . ? C11 C12 1.415(4) . ? C11 C16 1.496(4) . ? C12 C13 1.414(3) . ? C12 C17 1.501(4) . ? C13 C14 1.407(3) . ? C13 C18 1.496(3) . ? C14 C19 1.501(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O3 97.28(6) . . ? O1 Ti1 O2 90.20(7) . . ? O3 Ti1 O2 140.15(7) . . ? O1 Ti1 N1 128.46(8) . . ? O3 Ti1 N1 72.61(7) . . ? O2 Ti1 N1 72.21(7) . . ? O1 Ti1 C14 99.21(7) . . ? O3 Ti1 C14 136.53(7) . . ? O2 Ti1 C14 79.72(7) . . ? N1 Ti1 C14 123.20(8) . . ? O1 Ti1 C12 102.56(9) . . ? O3 Ti1 C12 79.61(7) . . ? O2 Ti1 C12 136.75(8) . . ? N1 Ti1 C12 123.67(8) . . ? C14 Ti1 C12 57.64(8) . . ? O1 Ti1 C13 82.48(8) . . ? O3 Ti1 C13 110.02(7) . . ? O2 Ti1 C13 109.75(7) . . ? N1 Ti1 C13 148.95(7) . . ? C14 Ti1 C13 34.50(8) . . ? C12 Ti1 C13 34.66(7) . . ? O1 Ti1 C11 136.63(10) . . ? O3 Ti1 C11 83.62(9) . . ? O2 Ti1 C11 116.52(9) . . ? N1 Ti1 C11 93.39(8) . . ? C14 Ti1 C11 57.26(8) . . ? C12 Ti1 C11 34.65(10) . . ? C13 Ti1 C11 57.27(8) . . ? O1 Ti1 C10 133.65(7) . . ? O3 Ti1 C10 116.41(9) . . ? O2 Ti1 C10 83.62(8) . . ? N1 Ti1 C10 93.11(8) . . ? C14 Ti1 C10 34.48(8) . . ? C12 Ti1 C10 57.65(9) . . ? C13 Ti1 C10 57.33(8) . . ? C11 Ti1 C10 34.45(9) . . ? O1 Ti1 Ti1 25.20(6) . 2_655 ? O3 Ti1 Ti1 100.75(6) . 2_655 ? O2 Ti1 Ti1 71.44(5) . 2_655 ? N1 Ti1 Ti1 105.29(5) . 2_655 ? C14 Ti1 Ti1 111.01(6) . 2_655 ? C12 Ti1 Ti1 127.76(7) . 2_655 ? C13 Ti1 Ti1 104.49(6) . 2_655 ? C11 Ti1 Ti1 161.29(7) . 2_655 ? C10 Ti1 Ti1 142.12(7) . 2_655 ? Ti1 O1 Ti1 129.60(13) . 2_655 ? C6 O2 Ti1 124.59(14) . . ? C7 O3 Ti1 124.62(15) . . ? C1 N1 C5 121.37(19) . . ? C1 N1 Ti1 119.77(14) . . ? C5 N1 Ti1 118.79(15) . . ? N1 C1 C2 120.8(2) . . ? N1 C1 C6 110.85(18) . . ? C2 C1 C6 128.2(2) . . ? C1 C2 C3 117.9(3) . . ? C4 C3 C2 121.0(2) . . ? C3 C4 C5 118.1(2) . . ? N1 C5 C4 120.4(2) . . ? N1 C5 C7 110.98(19) . . ? C4 C5 C7 128.4(2) . . ? O4 C6 O2 126.1(2) . . ? O4 C6 C1 121.8(2) . . ? O2 C6 C1 111.97(18) . . ? O5 C7 O3 126.3(3) . . ? O5 C7 C5 121.8(3) . . ? O3 C7 C5 111.91(19) . . ? C14 C10 C11 107.6(2) . . ? C14 C10 C15 125.3(3) . . ? C11 C10 C15 127.0(3) . . ? C14 C10 Ti1 72.03(13) . . ? C11 C10 Ti1 72.78(14) . . ? C15 C10 Ti1 123.00(19) . . ? C10 C11 C12 108.3(2) . . ? C10 C11 C16 125.5(3) . . ? C12 C11 C16 126.2(3) . . ? C10 C11 Ti1 72.78(13) . . ? C12 C11 Ti1 72.03(13) . . ? C16 C11 Ti1 123.69(19) . . ? C13 C12 C11 107.6(2) . . ? C13 C12 C17 126.3(3) . . ? C11 C12 C17 126.1(3) . . ? C13 C12 Ti1 73.16(12) . . ? C11 C12 Ti1 73.31(13) . . ? C17 C12 Ti1 121.73(18) . . ? C14 C13 C12 107.9(2) . . ? C14 C13 C18 125.5(2) . . ? C12 C13 C18 126.5(2) . . ? C14 C13 Ti1 72.17(12) . . ? C12 C13 Ti1 72.18(12) . . ? C18 C13 Ti1 122.88(17) . . ? C13 C14 C10 108.5(2) . . ? C13 C14 C19 124.2(2) . . ? C10 C14 C19 127.2(2) . . ? C13 C14 Ti1 73.33(12) . . ? C10 C14 Ti1 73.49(13) . . ? C19 C14 Ti1 121.02(17) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.381 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.067 #=====================END data_4 _database_code_depnum_ccdc_archive 'CCDC 296374' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H30 N2 O5 Ti' _chemical_formula_weight 486.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.1811(5) _cell_length_b 24.4114(6) _cell_length_c 11.8199(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.955(2) _cell_angle_gamma 90.00 _cell_volume 4789.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 3.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16438 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 70.55 _reflns_number_total 4422 _reflns_number_gt 3371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+1.3488P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4422 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.74543(3) 0.620716(17) 0.87116(4) 0.01633(14) Uani 1 1 d . . . C1 C 0.77394(16) 0.71056(10) 0.7158(2) 0.0207(5) Uani 1 1 d . . . C2 C 0.78025(16) 0.65965(10) 0.6453(2) 0.0199(5) Uani 1 1 d . . . C3 C 0.78690(17) 0.65657(11) 0.5312(2) 0.0248(6) Uani 1 1 d . . . H3 H 0.7858 0.6887 0.4854 0.030 Uiso 1 1 calc R . . C4 C 0.79530(17) 0.60501(12) 0.4856(2) 0.0274(6) Uani 1 1 d . . . H4 H 0.7982 0.6016 0.4067 0.033 Uiso 1 1 calc R . . C5 C 0.79951(17) 0.55823(11) 0.5550(2) 0.0243(6) Uani 1 1 d . . . H5 H 0.8081 0.5230 0.5262 0.029 Uiso 1 1 calc R . . C6 C 0.79063(16) 0.56510(10) 0.6677(2) 0.0206(5) Uani 1 1 d . . . C7 C 0.79381(17) 0.52105(10) 0.7587(2) 0.0217(5) Uani 1 1 d . . . C8 C 0.81759(16) 0.63630(9) 1.0375(2) 0.0196(5) Uani 1 1 d . . . C9 C 0.83402(18) 0.64922(10) 1.1653(2) 0.0233(6) Uani 1 1 d . . . H9A H 0.8260 0.6162 1.2082 0.035 Uiso 1 1 calc R . . H9B H 0.7971 0.6780 1.1770 0.035 Uiso 1 1 calc R . . H9C H 0.8897 0.6619 1.1944 0.035 Uiso 1 1 calc R . . C10 C 0.95059(17) 0.61368(10) 0.9955(2) 0.0228(6) Uani 1 1 d . . . C11 C 0.97245(19) 0.56625(12) 1.0813(3) 0.0335(7) Uani 1 1 d . . . H11A H 0.9575 0.5754 1.1536 0.050 Uiso 1 1 calc R . . H11B H 1.0306 0.5595 1.0992 0.050 Uiso 1 1 calc R . . H11C H 0.9434 0.5333 1.0465 0.050 Uiso 1 1 calc R . . C12 C 0.99658(19) 0.66562(12) 1.0426(3) 0.0341(7) Uani 1 1 d . . . H12A H 0.9784 0.6957 0.9872 0.051 Uiso 1 1 calc R . . H12B H 1.0544 0.6596 1.0529 0.051 Uiso 1 1 calc R . . H12C H 0.9866 0.6750 1.1183 0.051 Uiso 1 1 calc R . . C13 C 0.96841(19) 0.59875(14) 0.8793(2) 0.0337(7) Uani 1 1 d . . . H13A H 0.9397 0.5650 0.8488 0.051 Uiso 1 1 calc R . . H13B H 1.0265 0.5932 0.8916 0.051 Uiso 1 1 calc R . . H13C H 0.9505 0.6285 0.8230 0.051 Uiso 1 1 calc R . . C14 C 0.62980(16) 0.66017(10) 0.9110(2) 0.0210(5) Uani 1 1 d . . . C15 C 0.63697(16) 0.60649(11) 0.9589(2) 0.0230(5) Uani 1 1 d . . . C16 C 0.62380(17) 0.56891(10) 0.8649(2) 0.0234(6) Uani 1 1 d . . . C17 C 0.60960(16) 0.59882(11) 0.7595(2) 0.0219(5) Uani 1 1 d . . . C18 C 0.61092(16) 0.65513(10) 0.7868(2) 0.0208(5) Uani 1 1 d . . . C19 C 0.63810(18) 0.71331(11) 0.9778(2) 0.0287(6) Uani 1 1 d . . . H19A H 0.5846 0.7289 0.9713 0.043 Uiso 1 1 calc R . . H19B H 0.6702 0.7391 0.9451 0.043 Uiso 1 1 calc R . . H19C H 0.6649 0.7065 1.0604 0.043 Uiso 1 1 calc R . . C20 C 0.64534(19) 0.59204(13) 1.0854(2) 0.0331(7) Uani 1 1 d . . . H20A H 0.5929 0.5805 1.0955 0.050 Uiso 1 1 calc R . . H20B H 0.6643 0.6241 1.1346 0.050 Uiso 1 1 calc R . . H20C H 0.6842 0.5621 1.1084 0.050 Uiso 1 1 calc R . . C21 C 0.61850(19) 0.50761(11) 0.8748(3) 0.0327(7) Uani 1 1 d . . . H21A H 0.6503 0.4959 0.9522 0.049 Uiso 1 1 calc R . . H21B H 0.6396 0.4902 0.8142 0.049 Uiso 1 1 calc R . . H21C H 0.5621 0.4969 0.8646 0.049 Uiso 1 1 calc R . . C22 C 0.58963(19) 0.57523(12) 0.6375(2) 0.0296(6) Uani 1 1 d . . . H22A H 0.5313 0.5769 0.6034 0.044 Uiso 1 1 calc R . . H22B H 0.6075 0.5370 0.6409 0.044 Uiso 1 1 calc R . . H22C H 0.6171 0.5964 0.5890 0.044 Uiso 1 1 calc R . . C23 C 0.59193(17) 0.70085(11) 0.6994(2) 0.0270(6) Uani 1 1 d . . . H23A H 0.6148 0.6926 0.6335 0.040 Uiso 1 1 calc R . . H23B H 0.6152 0.7350 0.7368 0.040 Uiso 1 1 calc R . . H23C H 0.5334 0.7048 0.6708 0.040 Uiso 1 1 calc R . . C24 C -0.0584(6) 0.8522(4) 0.6754(5) 0.120(3) Uani 1 1 d . . . C25 C -0.0375(4) 0.8081(3) 0.6460(6) 0.097(2) Uani 1 1 d . . . N1 N 0.77931(13) 0.61453(8) 0.70867(17) 0.0184(4) Uani 1 1 d . . . N2 N 0.86245(13) 0.62368(8) 0.97288(17) 0.0191(4) Uani 1 1 d . . . O1 O 0.76225(11) 0.69889(7) 0.81656(14) 0.0199(4) Uani 1 1 d . . . O2 O 0.77984(13) 0.75651(7) 0.67761(16) 0.0293(5) Uani 1 1 d . . . O3 O 0.77396(11) 0.53959(7) 0.85011(15) 0.0206(4) Uani 1 1 d . . . O4 O 0.81482(13) 0.47427(7) 0.74479(17) 0.0302(5) Uani 1 1 d . . . O5 O 0.0000 0.8763(2) 0.7500 0.0919(17) Uani 1 2 d S . . O5A O 0.0000 0.7764(3) 0.7500 0.154(3) Uani 1 2 d S . . 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 0.0186(3) 0.0146(2) 0.0157(2) 0.00074(15) 0.00408(16) 0.00123(16) C1 0.0178(14) 0.0200(13) 0.0229(12) 0.0017(10) 0.0029(10) -0.0010(9) C2 0.0156(14) 0.0215(12) 0.0213(12) 0.0023(9) 0.0024(10) -0.0008(9) C3 0.0226(15) 0.0305(14) 0.0208(12) 0.0046(10) 0.0046(11) -0.0008(10) C4 0.0226(16) 0.0415(16) 0.0190(12) -0.0019(11) 0.0070(11) -0.0011(11) C5 0.0209(15) 0.0283(14) 0.0235(13) -0.0076(10) 0.0058(11) -0.0006(10) C6 0.0189(14) 0.0201(12) 0.0220(12) -0.0030(9) 0.0040(10) -0.0003(9) C7 0.0210(15) 0.0179(12) 0.0260(13) -0.0013(10) 0.0059(11) -0.0013(9) C8 0.0234(15) 0.0146(11) 0.0202(12) 0.0028(9) 0.0045(10) -0.0009(9) C9 0.0298(16) 0.0206(12) 0.0194(12) -0.0009(9) 0.0064(11) -0.0019(10) C10 0.0198(15) 0.0245(13) 0.0222(12) -0.0027(10) 0.0020(10) 0.0024(10) C11 0.0276(17) 0.0334(15) 0.0373(16) 0.0058(12) 0.0044(13) 0.0112(12) C12 0.0227(17) 0.0322(15) 0.0481(18) -0.0096(13) 0.0106(14) -0.0011(11) C13 0.0195(16) 0.0538(18) 0.0281(14) -0.0065(13) 0.0065(12) 0.0050(13) C14 0.0167(14) 0.0246(13) 0.0229(12) -0.0002(10) 0.0073(10) 0.0021(9) C15 0.0158(14) 0.0290(13) 0.0250(13) 0.0036(10) 0.0069(11) 0.0022(10) C16 0.0171(14) 0.0215(13) 0.0324(14) 0.0015(10) 0.0079(11) -0.0003(9) C17 0.0151(14) 0.0245(12) 0.0245(12) -0.0015(10) 0.0023(10) -0.0001(9) C18 0.0145(14) 0.0232(12) 0.0240(12) 0.0018(10) 0.0038(10) 0.0029(9) C19 0.0260(16) 0.0288(14) 0.0316(14) -0.0079(11) 0.0079(12) 0.0042(11) C20 0.0270(17) 0.0451(17) 0.0287(14) 0.0104(12) 0.0100(12) 0.0009(13) C21 0.0261(17) 0.0224(14) 0.0503(18) 0.0050(12) 0.0109(13) -0.0042(11) C22 0.0254(16) 0.0338(15) 0.0281(14) -0.0096(11) 0.0046(12) -0.0031(11) C23 0.0218(15) 0.0286(14) 0.0285(13) 0.0070(11) 0.0029(11) 0.0036(10) C24 0.176(9) 0.117(6) 0.060(3) -0.001(4) 0.015(4) -0.028(6) C25 0.069(4) 0.132(6) 0.088(4) 0.024(4) 0.015(3) 0.004(4) N1 0.0185(12) 0.0196(10) 0.0166(9) -0.0005(8) 0.0039(8) -0.0012(8) N2 0.0201(12) 0.0175(10) 0.0195(10) 0.0009(8) 0.0045(8) 0.0020(8) O1 0.0240(10) 0.0157(8) 0.0198(8) 0.0008(6) 0.0054(7) -0.0003(6) O2 0.0372(13) 0.0195(9) 0.0308(10) 0.0054(7) 0.0082(9) -0.0016(8) O3 0.0230(10) 0.0166(8) 0.0221(8) 0.0005(7) 0.0055(7) 0.0024(7) O4 0.0366(13) 0.0183(9) 0.0380(11) -0.0050(8) 0.0140(9) 0.0015(8) O5 0.059(3) 0.069(3) 0.138(5) 0.000 0.007(3) 0.000 O5A 0.145(8) 0.117(6) 0.177(8) 0.000 -0.002(6) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 2.0586(17) . ? Ti1 N2 2.060(2) . ? Ti1 O3 2.0704(17) . ? Ti1 C8 2.071(2) . ? Ti1 N1 2.151(2) . ? Ti1 C14 2.362(3) . ? Ti1 C15 2.381(3) . ? Ti1 C18 2.419(3) . ? Ti1 C17 2.426(3) . ? Ti1 C16 2.427(3) . ? C1 O2 1.223(3) . ? C1 O1 1.289(3) . ? C1 C2 1.516(4) . ? C2 N1 1.334(3) . ? C2 C3 1.385(4) . ? C3 C4 1.391(4) . ? C3 H3 0.9500 . ? C4 C5 1.397(4) . ? C4 H4 0.9500 . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 N1 1.333(3) . ? C6 C7 1.512(4) . ? C7 O4 1.222(3) . ? C7 O3 1.296(3) . ? C8 N2 1.255(3) . ? C8 C9 1.497(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N2 1.488(4) . ? C10 C11 1.522(4) . ? C10 C12 1.522(4) . ? C10 C13 1.526(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.420(4) . ? C14 C18 1.425(4) . ? C14 C19 1.506(4) . ? C15 C16 1.413(4) . ? C15 C20 1.506(4) . ? C16 C17 1.410(4) . ? C16 C21 1.506(4) . ? C17 C18 1.411(4) . ? C17 C22 1.508(4) . ? C18 C23 1.498(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.215(10) . ? C24 O5 1.294(8) . ? C25 O5A 1.454(7) . ? O5 C24 1.294(8) 2_556 ? O5A C25 1.454(7) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 N2 87.46(8) . . ? O1 Ti1 O3 142.39(8) . . ? N2 Ti1 O3 83.00(8) . . ? O1 Ti1 C8 91.68(8) . . ? N2 Ti1 C8 35.38(10) . . ? O3 Ti1 C8 100.81(8) . . ? O1 Ti1 N1 72.12(7) . . ? N2 Ti1 N1 94.32(8) . . ? O3 Ti1 N1 72.46(7) . . ? C8 Ti1 N1 128.82(10) . . ? O1 Ti1 C14 82.99(8) . . ? N2 Ti1 C14 127.85(9) . . ? O3 Ti1 C14 130.64(9) . . ? C8 Ti1 C14 93.67(10) . . ? N1 Ti1 C14 129.94(8) . . ? O1 Ti1 C15 117.44(8) . . ? N2 Ti1 C15 120.43(9) . . ? O3 Ti1 C15 98.57(8) . . ? C8 Ti1 C15 87.54(10) . . ? N1 Ti1 C15 143.27(9) . . ? C14 Ti1 C15 34.85(9) . . ? O1 Ti1 C18 75.24(8) . . ? N2 Ti1 C18 155.92(8) . . ? O3 Ti1 C18 120.88(8) . . ? C8 Ti1 C18 127.00(10) . . ? N1 Ti1 C18 96.09(8) . . ? C14 Ti1 C18 34.66(9) . . ? C15 Ti1 C18 57.21(9) . . ? O1 Ti1 C17 103.12(8) . . ? N2 Ti1 C17 169.14(8) . . ? O3 Ti1 C17 87.03(8) . . ? C8 Ti1 C17 144.40(10) . . ? N1 Ti1 C17 86.73(9) . . ? C14 Ti1 C17 57.16(9) . . ? C15 Ti1 C17 56.87(9) . . ? C18 Ti1 C17 33.86(9) . . ? O1 Ti1 C16 131.51(8) . . ? N2 Ti1 C16 137.62(9) . . ? O3 Ti1 C16 74.14(8) . . ? C8 Ti1 C16 115.10(10) . . ? N1 Ti1 C16 111.44(9) . . ? C14 Ti1 C16 57.09(9) . . ? C15 Ti1 C16 34.17(9) . . ? C18 Ti1 C16 56.29(9) . . ? C17 Ti1 C16 33.78(9) . . ? O2 C1 O1 126.2(2) . . ? O2 C1 C2 121.6(2) . . ? O1 C1 C2 112.1(2) . . ? N1 C2 C3 121.2(2) . . ? N1 C2 C1 110.8(2) . . ? C3 C2 C1 128.0(2) . . ? C2 C3 C4 118.0(2) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C3 C4 C5 120.5(2) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 117.5(2) . . ? C6 C5 H5 121.2 . . ? C4 C5 H5 121.2 . . ? N1 C6 C5 121.3(2) . . ? N1 C6 C7 111.5(2) . . ? C5 C6 C7 127.1(2) . . ? O4 C7 O3 126.1(2) . . ? O4 C7 C6 121.8(2) . . ? O3 C7 C6 112.1(2) . . ? N2 C8 C9 132.9(3) . . ? N2 C8 Ti1 71.85(14) . . ? C9 C8 Ti1 155.2(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 108.0(2) . . ? N2 C10 C12 109.7(2) . . ? C11 C10 C12 112.0(2) . . ? N2 C10 C13 108.0(2) . . ? C11 C10 C13 110.2(2) . . ? C12 C10 C13 108.9(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C18 107.7(2) . . ? C15 C14 C19 126.8(2) . . ? C18 C14 C19 125.5(2) . . ? C15 C14 Ti1 73.28(15) . . ? C18 C14 Ti1 74.85(15) . . ? C19 C14 Ti1 119.01(19) . . ? C16 C15 C14 107.8(2) . . ? C16 C15 C20 125.7(2) . . ? C14 C15 C20 126.0(3) . . ? C16 C15 Ti1 74.73(16) . . ? C14 C15 Ti1 71.87(15) . . ? C20 C15 Ti1 125.6(2) . . ? C17 C16 C15 108.3(2) . . ? C17 C16 C21 125.7(3) . . ? C15 C16 C21 125.8(3) . . ? C17 C16 Ti1 73.04(15) . . ? C15 C16 Ti1 71.10(15) . . ? C21 C16 Ti1 125.75(19) . . ? C16 C17 C18 108.3(2) . . ? C16 C17 C22 126.3(2) . . ? C18 C17 C22 125.2(2) . . ? C16 C17 Ti1 73.19(15) . . ? C18 C17 Ti1 72.82(15) . . ? C22 C17 Ti1 123.64(19) . . ? C17 C18 C14 107.8(2) . . ? C17 C18 C23 125.5(2) . . ? C14 C18 C23 126.7(2) . . ? C17 C18 Ti1 73.32(15) . . ? C14 C18 Ti1 70.48(15) . . ? C23 C18 Ti1 123.91(19) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 O5 111.2(9) . . ? C24 C25 O5A 109.2(7) . . ? C6 N1 C2 121.3(2) . . ? C6 N1 Ti1 119.10(17) . . ? C2 N1 Ti1 119.23(17) . . ? C8 N2 C10 133.4(2) . . ? C8 N2 Ti1 72.77(15) . . ? C10 N2 Ti1 153.29(16) . . ? C1 O1 Ti1 124.21(15) . . ? C7 O3 Ti1 123.76(15) . . ? C24 O5 C24 126.0(9) . 2_556 ? C25 O5A C25 115.7(9) 2_556 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 N1 174.4(2) . . . . ? O1 C1 C2 N1 -5.5(3) . . . . ? O2 C1 C2 C3 -5.2(5) . . . . ? O1 C1 C2 C3 175.0(3) . . . . ? N1 C2 C3 C4 -2.1(4) . . . . ? C1 C2 C3 C4 177.4(3) . . . . ? C2 C3 C4 C5 -2.1(4) . . . . ? C3 C4 C5 C6 3.4(4) . . . . ? C4 C5 C6 N1 -0.7(4) . . . . ? C4 C5 C6 C7 -179.3(3) . . . . ? N1 C6 C7 O4 -169.6(2) . . . . ? C5 C6 C7 O4 9.1(4) . . . . ? N1 C6 C7 O3 8.9(3) . . . . ? C5 C6 C7 O3 -172.4(3) . . . . ? O1 Ti1 C8 N2 -83.23(14) . . . . ? O3 Ti1 C8 N2 61.11(15) . . . . ? N1 Ti1 C8 N2 -14.99(18) . . . . ? C14 Ti1 C8 N2 -166.31(14) . . . . ? C15 Ti1 C8 N2 159.37(15) . . . . ? C18 Ti1 C8 N2 -155.95(13) . . . . ? C17 Ti1 C8 N2 161.24(15) . . . . ? C16 Ti1 C8 N2 138.53(14) . . . . ? O1 Ti1 C8 C9 102.3(4) . . . . ? N2 Ti1 C8 C9 -174.5(5) . . . . ? O3 Ti1 C8 C9 -113.4(4) . . . . ? N1 Ti1 C8 C9 170.5(4) . . . . ? C14 Ti1 C8 C9 19.2(4) . . . . ? C15 Ti1 C8 C9 -15.1(4) . . . . ? C18 Ti1 C8 C9 29.5(5) . . . . ? C17 Ti1 C8 C9 -13.3(5) . . . . ? C16 Ti1 C8 C9 -36.0(4) . . . . ? O1 Ti1 C14 C15 -171.62(16) . . . . ? N2 Ti1 C14 C15 -90.37(17) . . . . ? O3 Ti1 C14 C15 27.24(19) . . . . ? C8 Ti1 C14 C15 -80.37(16) . . . . ? N1 Ti1 C14 C15 128.82(15) . . . . ? C18 Ti1 C14 C15 114.2(2) . . . . ? C17 Ti1 C14 C15 77.80(16) . . . . ? C16 Ti1 C14 C15 37.33(15) . . . . ? O1 Ti1 C14 C18 74.14(15) . . . . ? N2 Ti1 C14 C18 155.39(14) . . . . ? O3 Ti1 C14 C18 -87.00(16) . . . . ? C8 Ti1 C14 C18 165.38(15) . . . . ? N1 Ti1 C14 C18 14.57(19) . . . . ? C15 Ti1 C14 C18 -114.2(2) . . . . ? C17 Ti1 C14 C18 -36.44(15) . . . . ? C16 Ti1 C14 C18 -76.91(16) . . . . ? O1 Ti1 C14 C19 -48.3(2) . . . . ? N2 Ti1 C14 C19 32.9(2) . . . . ? O3 Ti1 C14 C19 150.52(18) . . . . ? C8 Ti1 C14 C19 42.9(2) . . . . ? N1 Ti1 C14 C19 -107.9(2) . . . . ? C15 Ti1 C14 C19 123.3(3) . . . . ? C18 Ti1 C14 C19 -122.5(3) . . . . ? C17 Ti1 C14 C19 -158.9(2) . . . . ? C16 Ti1 C14 C19 160.6(2) . . . . ? C18 C14 C15 C16 0.9(3) . . . . ? C19 C14 C15 C16 179.3(3) . . . . ? Ti1 C14 C15 C16 -66.66(19) . . . . ? C18 C14 C15 C20 -171.2(3) . . . . ? C19 C14 C15 C20 7.2(5) . . . . ? Ti1 C14 C15 C20 121.3(3) . . . . ? C18 C14 C15 Ti1 67.52(19) . . . . ? C19 C14 C15 Ti1 -114.1(3) . . . . ? O1 Ti1 C15 C16 124.38(15) . . . . ? N2 Ti1 C15 C16 -131.31(15) . . . . ? O3 Ti1 C15 C16 -44.44(16) . . . . ? C8 Ti1 C15 C16 -145.00(16) . . . . ? N1 Ti1 C15 C16 27.6(2) . . . . ? C14 Ti1 C15 C16 115.0(2) . . . . ? C18 Ti1 C15 C16 76.91(16) . . . . ? C17 Ti1 C15 C16 36.30(15) . . . . ? O1 Ti1 C15 C14 9.38(17) . . . . ? N2 Ti1 C15 C14 113.69(15) . . . . ? O3 Ti1 C15 C14 -159.44(15) . . . . ? C8 Ti1 C15 C14 100.00(16) . . . . ? N1 Ti1 C15 C14 -87.36(19) . . . . ? C18 Ti1 C15 C14 -38.09(15) . . . . ? C17 Ti1 C15 C14 -78.70(16) . . . . ? C16 Ti1 C15 C14 -115.0(2) . . . . ? O1 Ti1 C15 C20 -112.4(2) . . . . ? N2 Ti1 C15 C20 -8.1(3) . . . . ? O3 Ti1 C15 C20 78.8(2) . . . . ? C8 Ti1 C15 C20 -21.8(2) . . . . ? N1 Ti1 C15 C20 150.9(2) . . . . ? C14 Ti1 C15 C20 -121.8(3) . . . . ? C18 Ti1 C15 C20 -159.9(3) . . . . ? C17 Ti1 C15 C20 159.5(3) . . . . ? C16 Ti1 C15 C20 123.2(3) . . . . ? C14 C15 C16 C17 0.8(3) . . . . ? C20 C15 C16 C17 172.9(3) . . . . ? Ti1 C15 C16 C17 -64.0(2) . . . . ? C14 C15 C16 C21 -174.3(3) . . . . ? C20 C15 C16 C21 -2.2(5) . . . . ? Ti1 C15 C16 C21 121.0(3) . . . . ? C14 C15 C16 Ti1 64.76(19) . . . . ? C20 C15 C16 Ti1 -123.1(3) . . . . ? O1 Ti1 C16 C17 38.89(19) . . . . ? N2 Ti1 C16 C17 -169.18(14) . . . . ? O3 Ti1 C16 C17 -109.14(16) . . . . ? C8 Ti1 C16 C17 156.15(15) . . . . ? N1 Ti1 C16 C17 -45.77(17) . . . . ? C14 Ti1 C16 C17 78.80(16) . . . . ? C15 Ti1 C16 C17 116.9(2) . . . . ? C18 Ti1 C16 C17 37.04(15) . . . . ? O1 Ti1 C16 C15 -77.99(18) . . . . ? N2 Ti1 C16 C15 73.94(19) . . . . ? O3 Ti1 C16 C15 133.97(16) . . . . ? C8 Ti1 C16 C15 39.26(18) . . . . ? N1 Ti1 C16 C15 -162.66(14) . . . . ? C14 Ti1 C16 C15 -38.09(15) . . . . ? C18 Ti1 C16 C15 -79.84(16) . . . . ? C17 Ti1 C16 C15 -116.9(2) . . . . ? O1 Ti1 C16 C21 161.0(2) . . . . ? N2 Ti1 C16 C21 -47.0(3) . . . . ? O3 Ti1 C16 C21 13.0(2) . . . . ? C8 Ti1 C16 C21 -81.7(3) . . . . ? N1 Ti1 C16 C21 76.4(3) . . . . ? C14 Ti1 C16 C21 -159.1(3) . . . . ? C15 Ti1 C16 C21 -121.0(3) . . . . ? C18 Ti1 C16 C21 159.2(3) . . . . ? C17 Ti1 C16 C21 122.1(3) . . . . ? C15 C16 C17 C18 -2.1(3) . . . . ? C21 C16 C17 C18 172.9(3) . . . . ? Ti1 C16 C17 C18 -64.85(19) . . . . ? C15 C16 C17 C22 -177.5(3) . . . . ? C21 C16 C17 C22 -2.5(5) . . . . ? Ti1 C16 C17 C22 119.7(3) . . . . ? C15 C16 C17 Ti1 62.75(19) . . . . ? C21 C16 C17 Ti1 -122.2(3) . . . . ? O1 Ti1 C17 C16 -151.13(15) . . . . ? N2 Ti1 C17 C16 42.2(5) . . . . ? O3 Ti1 C17 C16 65.50(15) . . . . ? C8 Ti1 C17 C16 -39.0(2) . . . . ? N1 Ti1 C17 C16 138.08(16) . . . . ? C14 Ti1 C17 C16 -78.57(16) . . . . ? C15 Ti1 C17 C16 -36.74(15) . . . . ? C18 Ti1 C17 C16 -115.9(2) . . . . ? O1 Ti1 C17 C18 -35.23(16) . . . . ? N2 Ti1 C17 C18 158.1(4) . . . . ? O3 Ti1 C17 C18 -178.60(15) . . . . ? C8 Ti1 C17 C18 76.9(2) . . . . ? N1 Ti1 C17 C18 -106.02(15) . . . . ? C14 Ti1 C17 C18 37.33(15) . . . . ? C15 Ti1 C17 C18 79.16(16) . . . . ? C16 Ti1 C17 C18 115.9(2) . . . . ? O1 Ti1 C17 C22 86.0(2) . . . . ? N2 Ti1 C17 C22 -80.6(5) . . . . ? O3 Ti1 C17 C22 -57.3(2) . . . . ? C8 Ti1 C17 C22 -161.8(2) . . . . ? N1 Ti1 C17 C22 15.3(2) . . . . ? C14 Ti1 C17 C22 158.6(3) . . . . ? C15 Ti1 C17 C22 -159.6(3) . . . . ? C18 Ti1 C17 C22 121.3(3) . . . . ? C16 Ti1 C17 C22 -122.8(3) . . . . ? C16 C17 C18 C14 2.6(3) . . . . ? C22 C17 C18 C14 178.1(3) . . . . ? Ti1 C17 C18 C14 -62.47(19) . . . . ? C16 C17 C18 C23 -174.8(3) . . . . ? C22 C17 C18 C23 0.7(4) . . . . ? Ti1 C17 C18 C23 120.1(3) . . . . ? C16 C17 C18 Ti1 65.09(19) . . . . ? C22 C17 C18 Ti1 -119.4(3) . . . . ? C15 C14 C18 C17 -2.1(3) . . . . ? C19 C14 C18 C17 179.4(3) . . . . ? Ti1 C14 C18 C17 64.32(19) . . . . ? C15 C14 C18 C23 175.2(3) . . . . ? C19 C14 C18 C23 -3.2(5) . . . . ? Ti1 C14 C18 C23 -118.3(3) . . . . ? C15 C14 C18 Ti1 -66.46(19) . . . . ? C19 C14 C18 Ti1 115.1(3) . . . . ? O1 Ti1 C18 C17 144.48(16) . . . . ? N2 Ti1 C18 C17 -170.1(2) . . . . ? O3 Ti1 C18 C17 1.63(18) . . . . ? C8 Ti1 C18 C17 -134.76(16) . . . . ? N1 Ti1 C18 C17 74.81(16) . . . . ? C14 Ti1 C18 C17 -116.4(2) . . . . ? C15 Ti1 C18 C17 -78.08(16) . . . . ? C16 Ti1 C18 C17 -36.95(15) . . . . ? O1 Ti1 C18 C14 -99.14(15) . . . . ? N2 Ti1 C18 C14 -53.7(3) . . . . ? O3 Ti1 C18 C14 118.01(15) . . . . ? C8 Ti1 C18 C14 -18.38(19) . . . . ? N1 Ti1 C18 C14 -168.81(15) . . . . ? C15 Ti1 C18 C14 38.30(15) . . . . ? C17 Ti1 C18 C14 116.4(2) . . . . ? C16 Ti1 C18 C14 79.42(16) . . . . ? O1 Ti1 C18 C23 22.5(2) . . . . ? N2 Ti1 C18 C23 68.0(3) . . . . ? O3 Ti1 C18 C23 -120.3(2) . . . . ? C8 Ti1 C18 C23 103.3(2) . . . . ? N1 Ti1 C18 C23 -47.2(2) . . . . ? C14 Ti1 C18 C23 121.7(3) . . . . ? C15 Ti1 C18 C23 160.0(2) . . . . ? C17 Ti1 C18 C23 -122.0(3) . . . . ? C16 Ti1 C18 C23 -158.9(3) . . . . ? O5 C24 C25 O5A 51.3(9) . . . . ? C5 C6 N1 C2 -3.5(4) . . . . ? C7 C6 N1 C2 175.3(2) . . . . ? C5 C6 N1 Ti1 169.3(2) . . . . ? C7 C6 N1 Ti1 -11.8(3) . . . . ? C3 C2 N1 C6 5.0(4) . . . . ? C1 C2 N1 C6 -174.6(2) . . . . ? C3 C2 N1 Ti1 -167.9(2) . . . . ? C1 C2 N1 Ti1 12.5(3) . . . . ? O1 Ti1 N1 C6 175.6(2) . . . . ? N2 Ti1 N1 C6 89.7(2) . . . . ? O3 Ti1 N1 C6 8.44(18) . . . . ? C8 Ti1 N1 C6 98.3(2) . . . . ? C14 Ti1 N1 C6 -120.34(19) . . . . ? C15 Ti1 N1 C6 -72.2(2) . . . . ? C18 Ti1 N1 C6 -112.1(2) . . . . ? C17 Ti1 N1 C6 -79.5(2) . . . . ? C16 Ti1 N1 C6 -56.0(2) . . . . ? O1 Ti1 N1 C2 -11.37(18) . . . . ? N2 Ti1 N1 C2 -97.29(19) . . . . ? O3 Ti1 N1 C2 -178.5(2) . . . . ? C8 Ti1 N1 C2 -88.7(2) . . . . ? C14 Ti1 N1 C2 52.7(2) . . . . ? C15 Ti1 N1 C2 100.8(2) . . . . ? C18 Ti1 N1 C2 61.0(2) . . . . ? C17 Ti1 N1 C2 93.5(2) . . . . ? C16 Ti1 N1 C2 117.06(19) . . . . ? C9 C8 N2 C10 3.2(5) . . . . ? Ti1 C8 N2 C10 -173.7(3) . . . . ? C9 C8 N2 Ti1 176.9(3) . . . . ? C11 C10 N2 C8 59.9(3) . . . . ? C12 C10 N2 C8 -62.4(4) . . . . ? C13 C10 N2 C8 179.1(3) . . . . ? C11 C10 N2 Ti1 -106.6(4) . . . . ? C12 C10 N2 Ti1 131.1(3) . . . . ? C13 C10 N2 Ti1 12.6(5) . . . . ? O1 Ti1 N2 C8 96.50(14) . . . . ? O3 Ti1 N2 C8 -119.95(15) . . . . ? N1 Ti1 N2 C8 168.34(14) . . . . ? C14 Ti1 N2 C8 17.41(18) . . . . ? C15 Ti1 N2 C8 -24.09(17) . . . . ? C18 Ti1 N2 C8 52.9(3) . . . . ? C17 Ti1 N2 C8 -96.5(5) . . . . ? C16 Ti1 N2 C8 -62.85(19) . . . . ? O1 Ti1 N2 C10 -93.7(4) . . . . ? O3 Ti1 N2 C10 49.8(4) . . . . ? C8 Ti1 N2 C10 169.8(4) . . . . ? N1 Ti1 N2 C10 -21.9(4) . . . . ? C14 Ti1 N2 C10 -172.8(3) . . . . ? C15 Ti1 N2 C10 145.7(4) . . . . ? C18 Ti1 N2 C10 -137.3(3) . . . . ? C17 Ti1 N2 C10 73.3(6) . . . . ? C16 Ti1 N2 C10 106.9(4) . . . . ? O2 C1 O1 Ti1 175.8(2) . . . . ? C2 C1 O1 Ti1 -4.4(3) . . . . ? N2 Ti1 O1 C1 103.7(2) . . . . ? O3 Ti1 O1 C1 28.6(3) . . . . ? C8 Ti1 O1 C1 138.8(2) . . . . ? N1 Ti1 O1 C1 8.28(19) . . . . ? C14 Ti1 O1 C1 -127.7(2) . . . . ? C15 Ti1 O1 C1 -133.1(2) . . . . ? C18 Ti1 O1 C1 -93.3(2) . . . . ? C17 Ti1 O1 C1 -73.9(2) . . . . ? C16 Ti1 O1 C1 -94.9(2) . . . . ? O4 C7 O3 Ti1 176.2(2) . . . . ? C6 C7 O3 Ti1 -2.1(3) . . . . ? O1 Ti1 O3 C7 -23.2(3) . . . . ? N2 Ti1 O3 C7 -99.7(2) . . . . ? C8 Ti1 O3 C7 -130.4(2) . . . . ? N1 Ti1 O3 C7 -2.9(2) . . . . ? C14 Ti1 O3 C7 125.1(2) . . . . ? C15 Ti1 O3 C7 140.4(2) . . . . ? C18 Ti1 O3 C7 83.7(2) . . . . ? C17 Ti1 O3 C7 84.6(2) . . . . ? C16 Ti1 O3 C7 116.3(2) . . . . ? C25 C24 O5 C24 -29.6(5) . . . 2_556 ? C24 C25 O5A C25 -27.1(6) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 70.55 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.596 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.067 #===============END data_6 _database_code_depnum_ccdc_archive 'CCDC 296375' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H60 N2 O10 Rh2 Ti2, 2(C H2 Cl2)' _chemical_formula_sum 'C52 H64 Cl4 N2 O10 Rh2 Ti2' _chemical_formula_weight 1320.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6793(2) _cell_length_b 19.0548(6) _cell_length_c 13.1973(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.460(2) _cell_angle_gamma 90.00 _cell_volume 2622.29(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 9.874 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22196 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 70.54 _reflns_number_total 4924 _reflns_number_gt 4625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.8864P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4924 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0548 _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 Rh1 Rh 0.726307(12) 0.116006(6) 0.623851(10) 0.01071(6) Uani 1 1 d . . . Ti1 Ti 0.41304(3) 0.067154(16) 0.67957(2) 0.01007(8) Uani 1 1 d . . . C1 C 0.25980(17) 0.02471(9) 0.46989(14) 0.0121(3) Uani 1 1 d . . . C2 C 0.21629(17) 0.09930(10) 0.47700(14) 0.0128(3) Uani 1 1 d . . . C3 C 0.13212(17) 0.13714(10) 0.40176(14) 0.0147(4) Uani 1 1 d . . . C4 C 0.10590(17) 0.20640(10) 0.42406(15) 0.0156(4) Uani 1 1 d . . . C5 C 0.16626(18) 0.23598(10) 0.51851(15) 0.0146(4) Uani 1 1 d . . . C6 C 0.25135(17) 0.19460(10) 0.58883(14) 0.0133(3) Uani 1 1 d . . . C7 C 0.33269(17) 0.21822(9) 0.69154(14) 0.0134(3) Uani 1 1 d . . . C8 C 0.30931(18) 0.04197(10) 0.82367(14) 0.0137(3) Uani 1 1 d . . . C9 C 0.44528(17) 0.04501(9) 0.85988(13) 0.0129(3) Uani 1 1 d . . . C10 C 0.50036(18) -0.01190(9) 0.81539(14) 0.0141(4) Uani 1 1 d . . . C11 C 0.39946(18) -0.04831(9) 0.74876(14) 0.0130(3) Uani 1 1 d . . . C12 C 0.28109(17) -0.01491(9) 0.75450(14) 0.0132(3) Uani 1 1 d . . . C13 C 0.21496(19) 0.09104(11) 0.85589(16) 0.0180(4) Uani 1 1 d . . . C14 C 0.51799(19) 0.09612(10) 0.93759(15) 0.0164(4) Uani 1 1 d . . . C15 C 0.63990(19) -0.02995(11) 0.83585(16) 0.0191(4) Uani 1 1 d . . . C16 C 0.4117(2) -0.11404(10) 0.68954(16) 0.0168(4) Uani 1 1 d . . . C17 C 0.15113(18) -0.03839(10) 0.69589(16) 0.0170(4) Uani 1 1 d . . . C18 C 0.63445(18) 0.21366(9) 0.59381(15) 0.0155(4) Uani 1 1 d . . . C19 C 0.6739(2) 0.25107(10) 0.50461(16) 0.0190(4) Uani 1 1 d . . . C20 C 0.8119(2) 0.23349(10) 0.49587(16) 0.0194(4) Uani 1 1 d . . . C21 C 0.85329(18) 0.16084(10) 0.53907(15) 0.0155(4) Uani 1 1 d . . . C22 C 0.91746(17) 0.14976(10) 0.64251(15) 0.0154(4) Uani 1 1 d . . . C23 C 0.94936(19) 0.20765(11) 0.72242(16) 0.0190(4) Uani 1 1 d . . . C24 C 0.8320(2) 0.25269(10) 0.72987(16) 0.0189(4) Uani 1 1 d . . . C25 C 0.70614(18) 0.21256(9) 0.69642(15) 0.0154(4) Uani 1 1 d . . . C26 C 0.1102(2) 0.90628(12) 0.93501(17) 0.0245(4) Uani 1 1 d . . . N1 N 0.27294(14) 0.12779(8) 0.56803(12) 0.0117(3) Uani 1 1 d . . . O1 O 0.34382(12) 0.00463(6) 0.54753(10) 0.0143(3) Uani 1 1 d . . . O2 O 0.40338(12) 0.16854(6) 0.73910(10) 0.0143(3) Uani 1 1 d . . . O3 O 0.32936(13) 0.27928(7) 0.72067(10) 0.0187(3) Uani 1 1 d . . . O4 O 0.56134(12) 0.07792(7) 0.65634(10) 0.0154(3) Uani 1 1 d . . . O5 O 0.78879(12) 0.01109(6) 0.60802(10) 0.0140(3) Uani 1 1 d . . . Cl1 Cl -0.05002(5) 0.93320(3) 0.88590(4) 0.03219(13) Uani 1 1 d . . . Cl2 Cl 0.12756(5) 0.86718(3) 1.05853(4) 0.03133(12) Uani 1 1 d . . . H3 H 0.093(2) 0.1157(11) 0.3359(19) 0.012(5) Uiso 1 1 d . . . H4 H 0.047(2) 0.2327(13) 0.374(2) 0.022(6) Uiso 1 1 d . . . H5 H 0.153(2) 0.2830(13) 0.5380(19) 0.017(6) Uiso 1 1 d . . . H13A H 0.214(3) 0.0880(18) 0.931(3) 0.053(9) Uiso 1 1 d . . . H13B H 0.228(3) 0.1391(18) 0.847(2) 0.041(8) Uiso 1 1 d . . . H13C H 0.137(3) 0.0810(17) 0.821(3) 0.047(9) Uiso 1 1 d . . . H14A H 0.468(3) 0.1353(15) 0.948(2) 0.028(7) Uiso 1 1 d . . . H14B H 0.543(3) 0.0776(16) 1.002(3) 0.038(8) Uiso 1 1 d . . . H14C H 0.592(3) 0.1127(13) 0.918(2) 0.022(6) Uiso 1 1 d . . . H15A H 0.659(4) -0.062(2) 0.886(3) 0.059(10) Uiso 1 1 d . . . H15B H 0.668(3) -0.0519(18) 0.783(3) 0.051(9) Uiso 1 1 d . . . H15C H 0.693(3) 0.0103(18) 0.852(2) 0.045(8) Uiso 1 1 d . . . H16A H 0.369(3) -0.1113(17) 0.621(3) 0.047(9) Uiso 1 1 d . . . H16B H 0.378(3) -0.149(2) 0.719(3) 0.054(10) Uiso 1 1 d . . . H16C H 0.495(3) -0.1244(15) 0.690(2) 0.035(8) Uiso 1 1 d . . . H17A H 0.136(2) -0.0882(14) 0.7054(19) 0.019(6) Uiso 1 1 d . . . H17B H 0.085(3) -0.0172(14) 0.720(2) 0.027(7) Uiso 1 1 d . . . H17C H 0.137(2) -0.0270(14) 0.626(2) 0.024(6) Uiso 1 1 d . . . H18 H 0.547(2) 0.2053(12) 0.5861(17) 0.012(5) Uiso 1 1 d . . . H19A H 0.615(2) 0.2377(13) 0.437(2) 0.021(6) Uiso 1 1 d . . . H19B H 0.662(2) 0.2999(14) 0.5137(18) 0.018(6) Uiso 1 1 d . . . H20A H 0.872(2) 0.2665(13) 0.5338(19) 0.019(6) Uiso 1 1 d . . . H20B H 0.820(2) 0.2345(12) 0.423(2) 0.018(6) Uiso 1 1 d . . . H21 H 0.861(2) 0.1258(13) 0.490(2) 0.021(6) Uiso 1 1 d . . . H22 H 0.966(2) 0.1093(11) 0.6583(17) 0.007(5) Uiso 1 1 d . . . H23A H 1.017(2) 0.2384(13) 0.7076(19) 0.022(6) Uiso 1 1 d . . . H23B H 0.982(2) 0.1849(13) 0.789(2) 0.018(6) Uiso 1 1 d . . . H24A H 0.842(2) 0.2687(13) 0.800(2) 0.023(6) Uiso 1 1 d . . . H24B H 0.827(3) 0.2962(14) 0.685(2) 0.027(6) Uiso 1 1 d . . . H25 H 0.664(2) 0.1999(12) 0.7512(18) 0.011(5) Uiso 1 1 d . . . H26A H 0.166(3) 0.9466(14) 0.945(2) 0.025(6) Uiso 1 1 d . . . H26B H 0.135(3) 0.8732(14) 0.887(2) 0.026(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01161(8) 0.00902(8) 0.01160(8) -0.00065(4) 0.00274(5) -0.00105(4) Ti1 0.01147(16) 0.00813(15) 0.01022(15) 0.00051(11) 0.00149(11) -0.00007(11) C1 0.0121(8) 0.0123(8) 0.0128(8) 0.0015(7) 0.0048(6) -0.0017(7) C2 0.0117(8) 0.0135(8) 0.0131(8) 0.0004(7) 0.0025(6) -0.0018(7) C3 0.0124(8) 0.0170(9) 0.0142(9) 0.0012(7) 0.0020(7) -0.0014(7) C4 0.0125(8) 0.0168(9) 0.0172(9) 0.0052(8) 0.0028(7) 0.0012(7) C5 0.0153(9) 0.0113(8) 0.0178(9) 0.0008(7) 0.0050(7) 0.0020(7) C6 0.0137(9) 0.0126(8) 0.0143(8) -0.0001(7) 0.0045(7) -0.0008(7) C7 0.0149(9) 0.0133(8) 0.0128(8) 0.0008(7) 0.0048(7) -0.0009(7) C8 0.0164(9) 0.0136(8) 0.0119(8) 0.0017(7) 0.0049(7) -0.0015(7) C9 0.0162(9) 0.0124(8) 0.0095(8) 0.0033(7) 0.0017(6) 0.0001(7) C10 0.0157(9) 0.0133(8) 0.0129(8) 0.0042(7) 0.0022(7) 0.0010(7) C11 0.0161(9) 0.0109(8) 0.0121(8) 0.0029(7) 0.0027(6) -0.0010(7) C12 0.0147(9) 0.0119(8) 0.0136(8) 0.0032(7) 0.0046(7) -0.0011(7) C13 0.0153(10) 0.0185(10) 0.0203(10) -0.0036(8) 0.0037(7) 0.0014(8) C14 0.0187(10) 0.0157(9) 0.0137(9) -0.0007(8) 0.0007(7) -0.0010(8) C15 0.0160(10) 0.0201(10) 0.0197(10) 0.0020(9) 0.0004(7) 0.0037(8) C16 0.0198(11) 0.0118(9) 0.0183(10) 0.0003(7) 0.0031(8) 0.0014(7) C17 0.0145(9) 0.0169(9) 0.0200(10) -0.0010(8) 0.0047(7) -0.0023(7) C18 0.0145(9) 0.0102(8) 0.0225(10) 0.0009(7) 0.0058(7) 0.0015(7) C19 0.0222(10) 0.0139(9) 0.0216(10) 0.0036(8) 0.0063(8) 0.0019(7) C20 0.0235(10) 0.0170(9) 0.0195(10) 0.0016(8) 0.0084(8) -0.0030(8) C21 0.0159(9) 0.0140(8) 0.0188(9) -0.0026(8) 0.0084(7) -0.0038(7) C22 0.0113(8) 0.0131(8) 0.0223(10) -0.0014(8) 0.0046(7) -0.0023(7) C23 0.0168(9) 0.0191(9) 0.0208(10) -0.0040(8) 0.0028(7) -0.0051(8) C24 0.0247(10) 0.0134(9) 0.0188(10) -0.0050(8) 0.0049(7) -0.0034(8) C25 0.0194(9) 0.0107(8) 0.0181(9) -0.0034(7) 0.0085(7) 0.0000(7) C26 0.0213(10) 0.0287(11) 0.0238(11) 0.0034(9) 0.0051(8) 0.0026(9) N1 0.0122(7) 0.0107(7) 0.0124(7) 0.0005(6) 0.0034(6) -0.0003(6) O1 0.0181(6) 0.0113(6) 0.0125(6) -0.0007(5) 0.0010(5) 0.0012(5) O2 0.0187(6) 0.0099(6) 0.0133(6) 0.0001(5) 0.0010(5) 0.0005(5) O3 0.0260(7) 0.0117(6) 0.0172(7) -0.0023(5) 0.0020(5) 0.0017(5) O4 0.0165(7) 0.0135(6) 0.0164(6) 0.0001(5) 0.0041(5) -0.0018(5) O5 0.0170(6) 0.0114(6) 0.0130(6) -0.0025(5) 0.0021(5) -0.0008(5) Cl1 0.0221(3) 0.0482(3) 0.0260(3) 0.0053(2) 0.00442(19) 0.0089(2) Cl2 0.0251(3) 0.0400(3) 0.0289(3) 0.0130(2) 0.0058(2) 0.0020(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O4 2.0348(13) . ? Rh1 C18 2.1009(18) . ? Rh1 C22 2.1035(18) . ? Rh1 C25 2.1065(18) . ? Rh1 C21 2.1155(18) . ? Rh1 O5 2.1321(13) . ? Ti1 O4 1.6893(13) . ? Ti1 O2 2.0964(13) . ? Ti1 O1 2.1086(13) . ? Ti1 N1 2.1885(15) . ? Ti1 C9 2.3677(17) . ? Ti1 C10 2.3729(18) . ? Ti1 C11 2.3985(17) . ? Ti1 C8 2.4461(18) . ? Ti1 C12 2.4515(18) . ? C1 O5 1.250(2) 3_656 ? C1 O1 1.267(2) . ? C1 C2 1.504(2) . ? C2 N1 1.338(2) . ? C2 C3 1.389(3) . ? C3 C4 1.394(3) . ? C3 H3 0.97(2) . ? C4 C5 1.393(3) . ? C4 H4 0.95(3) . ? C5 C6 1.394(3) . ? C5 H5 0.95(3) . ? C6 N1 1.333(2) . ? C6 C7 1.512(3) . ? C7 O3 1.228(2) . ? C7 O2 1.287(2) . ? C8 C12 1.407(3) . ? C8 C9 1.429(3) . ? C8 C13 1.502(3) . ? C9 C10 1.420(3) . ? C9 C14 1.503(3) . ? C10 C11 1.417(3) . ? C10 C15 1.496(3) . ? C11 C12 1.432(3) . ? C11 C16 1.497(3) . ? C12 C17 1.504(3) . ? C13 H13A 1.00(4) . ? C13 H13B 0.94(3) . ? C13 H13C 0.88(4) . ? C14 H14A 0.95(3) . ? C14 H14B 0.91(3) . ? C14 H14C 0.94(3) . ? C15 H15A 0.89(4) . ? C15 H15B 0.92(4) . ? C15 H15C 0.95(3) . ? C16 H16A 0.92(4) . ? C16 H16B 0.89(4) . ? C16 H16C 0.91(3) . ? C17 H17A 0.98(3) . ? C17 H17B 0.93(3) . ? C17 H17C 0.92(3) . ? C18 C25 1.405(3) . ? C18 C19 1.512(3) . ? C18 H18 0.94(2) . ? C19 C20 1.540(3) . ? C19 H19A 1.01(3) . ? C19 H19B 0.95(3) . ? C20 C21 1.526(3) . ? C20 H20A 0.96(3) . ? C20 H20B 0.98(3) . ? C21 C22 1.405(3) . ? C21 H21 0.94(3) . ? C22 C23 1.513(3) . ? C22 H22 0.93(2) . ? C23 C24 1.539(3) . ? C23 H23A 0.98(3) . ? C23 H23B 0.98(3) . ? C24 C25 1.527(3) . ? C24 H24A 0.95(3) . ? C24 H24B 1.01(3) . ? C25 H25 0.96(2) . ? C26 Cl2 1.765(2) . ? C26 Cl1 1.770(2) . ? C26 H26A 0.96(3) . ? C26 H26B 0.97(3) . ? O5 C1 1.250(2) 3_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Rh1 C18 88.02(6) . . ? O4 Rh1 C22 161.25(6) . . ? C18 Rh1 C22 98.81(7) . . ? O4 Rh1 C25 92.15(6) . . ? C18 Rh1 C25 39.00(8) . . ? C22 Rh1 C25 82.62(7) . . ? O4 Rh1 C21 159.79(6) . . ? C18 Rh1 C21 82.47(7) . . ? C22 Rh1 C21 38.90(7) . . ? C25 Rh1 C21 91.59(7) . . ? O4 Rh1 O5 89.41(5) . . ? C18 Rh1 O5 162.79(6) . . ? C22 Rh1 O5 88.96(6) . . ? C25 Rh1 O5 158.18(6) . . ? C21 Rh1 O5 94.42(6) . . ? O4 Ti1 O2 94.59(6) . . ? O4 Ti1 O1 95.39(6) . . ? O2 Ti1 O1 142.52(5) . . ? O4 Ti1 N1 110.21(6) . . ? O2 Ti1 N1 71.57(5) . . ? O1 Ti1 N1 71.07(5) . . ? O4 Ti1 C9 105.38(6) . . ? O2 Ti1 C9 78.22(6) . . ? O1 Ti1 C9 132.76(6) . . ? N1 Ti1 C9 134.44(6) . . ? O4 Ti1 C10 89.03(6) . . ? O2 Ti1 C10 110.18(6) . . ? O1 Ti1 C10 106.03(6) . . ? N1 Ti1 C10 160.64(6) . . ? C9 Ti1 C10 34.85(6) . . ? O4 Ti1 C11 108.45(6) . . ? O2 Ti1 C11 133.69(6) . . ? O1 Ti1 C11 75.95(6) . . ? N1 Ti1 C11 130.67(6) . . ? C9 Ti1 C11 57.41(6) . . ? C10 Ti1 C11 34.54(6) . . ? O4 Ti1 C8 139.86(6) . . ? O2 Ti1 C8 79.76(6) . . ? O1 Ti1 C8 113.26(6) . . ? N1 Ti1 C8 105.54(6) . . ? C9 Ti1 C8 34.48(6) . . ? C10 Ti1 C8 57.20(6) . . ? C11 Ti1 C8 56.58(6) . . ? O4 Ti1 C12 142.52(6) . . ? O2 Ti1 C12 110.95(6) . . ? O1 Ti1 C12 80.99(6) . . ? N1 Ti1 C12 103.83(6) . . ? C9 Ti1 C12 56.80(6) . . ? C10 Ti1 C12 57.10(6) . . ? C11 Ti1 C12 34.32(6) . . ? C8 Ti1 C12 33.39(6) . . ? O5 C1 O1 126.63(16) 3_656 . ? O5 C1 C2 119.21(16) 3_656 . ? O1 C1 C2 114.16(15) . . ? N1 C2 C3 121.92(17) . . ? N1 C2 C1 110.69(15) . . ? C3 C2 C1 127.36(17) . . ? C2 C3 C4 117.98(17) . . ? C2 C3 H3 120.7(13) . . ? C4 C3 H3 121.4(13) . . ? C5 C4 C3 119.79(17) . . ? C5 C4 H4 120.9(15) . . ? C3 C4 H4 119.3(15) . . ? C4 C5 C6 118.43(17) . . ? C4 C5 H5 123.8(15) . . ? C6 C5 H5 117.7(15) . . ? N1 C6 C5 121.32(17) . . ? N1 C6 C7 112.17(16) . . ? C5 C6 C7 126.45(17) . . ? O3 C7 O2 126.71(17) . . ? O3 C7 C6 120.85(16) . . ? O2 C7 C6 112.42(15) . . ? C12 C8 C9 107.95(16) . . ? C12 C8 C13 126.90(17) . . ? C9 C8 C13 125.15(17) . . ? C12 C8 Ti1 73.51(10) . . ? C9 C8 Ti1 69.76(10) . . ? C13 C8 Ti1 122.82(13) . . ? C10 C9 C8 108.22(16) . . ? C10 C9 C14 125.30(17) . . ? C8 C9 C14 126.35(17) . . ? C10 C9 Ti1 72.77(10) . . ? C8 C9 Ti1 75.77(10) . . ? C14 C9 Ti1 120.79(12) . . ? C11 C10 C9 107.65(16) . . ? C11 C10 C15 126.45(17) . . ? C9 C10 C15 125.90(17) . . ? C11 C10 Ti1 73.72(10) . . ? C9 C10 Ti1 72.37(10) . . ? C15 C10 Ti1 119.75(13) . . ? C10 C11 C12 108.16(16) . . ? C10 C11 C16 126.40(17) . . ? C12 C11 C16 125.24(17) . . ? C10 C11 Ti1 71.74(10) . . ? C12 C11 Ti1 74.87(10) . . ? C16 C11 Ti1 123.33(13) . . ? C8 C12 C11 107.98(16) . . ? C8 C12 C17 127.41(17) . . ? C11 C12 C17 124.61(17) . . ? C8 C12 Ti1 73.09(10) . . ? C11 C12 Ti1 70.81(10) . . ? C17 C12 Ti1 121.96(12) . . ? C8 C13 H13A 114(2) . . ? C8 C13 H13B 116.0(19) . . ? H13A C13 H13B 103(3) . . ? C8 C13 H13C 110(2) . . ? H13A C13 H13C 107(3) . . ? H13B C13 H13C 107(3) . . ? C9 C14 H14A 112.4(17) . . ? C9 C14 H14B 113.2(19) . . ? H14A C14 H14B 104(3) . . ? C9 C14 H14C 111.7(16) . . ? H14A C14 H14C 108(2) . . ? H14B C14 H14C 107(2) . . ? C10 C15 H15A 110(2) . . ? C10 C15 H15B 116(2) . . ? H15A C15 H15B 102(3) . . ? C10 C15 H15C 112(2) . . ? H15A C15 H15C 111(3) . . ? H15B C15 H15C 105(3) . . ? C11 C16 H16A 113(2) . . ? C11 C16 H16B 108(2) . . ? H16A C16 H16B 108(3) . . ? C11 C16 H16C 112.1(19) . . ? H16A C16 H16C 107(3) . . ? H16B C16 H16C 109(3) . . ? C12 C17 H17A 112.5(15) . . ? C12 C17 H17B 112.2(16) . . ? H17A C17 H17B 103(2) . . ? C12 C17 H17C 112.1(16) . . ? H17A C17 H17C 111(2) . . ? H17B C17 H17C 106(2) . . ? C25 C18 C19 124.90(17) . . ? C25 C18 Rh1 70.71(10) . . ? C19 C18 Rh1 111.55(13) . . ? C25 C18 H18 115.3(14) . . ? C19 C18 H18 116.0(13) . . ? Rh1 C18 H18 106.6(14) . . ? C18 C19 C20 112.82(16) . . ? C18 C19 H19A 109.8(14) . . ? C20 C19 H19A 108.1(14) . . ? C18 C19 H19B 107.1(15) . . ? C20 C19 H19B 112.5(15) . . ? H19A C19 H19B 106(2) . . ? C21 C20 C19 111.96(16) . . ? C21 C20 H20A 107.1(14) . . ? C19 C20 H20A 111.1(15) . . ? C21 C20 H20B 107.7(14) . . ? C19 C20 H20B 110.9(14) . . ? H20A C20 H20B 108(2) . . ? C22 C21 C20 122.73(17) . . ? C22 C21 Rh1 70.08(10) . . ? C20 C21 Rh1 113.40(13) . . ? C22 C21 H21 117.5(15) . . ? C20 C21 H21 116.7(15) . . ? Rh1 C21 H21 103.3(15) . . ? C21 C22 C23 123.84(17) . . ? C21 C22 Rh1 71.01(10) . . ? C23 C22 Rh1 111.80(13) . . ? C21 C22 H22 118.3(14) . . ? C23 C22 H22 114.8(14) . . ? Rh1 C22 H22 104.7(13) . . ? C22 C23 C24 112.77(16) . . ? C22 C23 H23A 111.2(15) . . ? C24 C23 H23A 108.8(15) . . ? C22 C23 H23B 106.7(14) . . ? C24 C23 H23B 109.3(14) . . ? H23A C23 H23B 108(2) . . ? C25 C24 C23 112.36(15) . . ? C25 C24 H24A 110.3(15) . . ? C23 C24 H24A 108.6(15) . . ? C25 C24 H24B 107.9(15) . . ? C23 C24 H24B 111.3(15) . . ? H24A C24 H24B 106(2) . . ? C18 C25 C24 122.28(17) . . ? C18 C25 Rh1 70.28(10) . . ? C24 C25 Rh1 113.50(13) . . ? C18 C25 H25 119.1(13) . . ? C24 C25 H25 115.5(13) . . ? Rh1 C25 H25 103.5(13) . . ? Cl2 C26 Cl1 111.16(12) . . ? Cl2 C26 H26A 105.9(16) . . ? Cl1 C26 H26A 109.9(16) . . ? Cl2 C26 H26B 109.8(16) . . ? Cl1 C26 H26B 109.2(16) . . ? H26A C26 H26B 111(2) . . ? C6 N1 C2 120.50(16) . . ? C6 N1 Ti1 119.29(12) . . ? C2 N1 Ti1 120.05(12) . . ? C1 O1 Ti1 123.96(11) . . ? C7 O2 Ti1 124.49(11) . . ? Ti1 O4 Rh1 165.88(8) . . ? C1 O5 Rh1 120.61(11) 3_656 . ? 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 O5 C1 C2 N1 176.30(15) 3_656 . . . ? O1 C1 C2 N1 -2.9(2) . . . . ? O5 C1 C2 C3 -5.3(3) 3_656 . . . ? O1 C1 C2 C3 175.55(17) . . . . ? N1 C2 C3 C4 -1.0(3) . . . . ? C1 C2 C3 C4 -179.21(17) . . . . ? C2 C3 C4 C5 1.6(3) . . . . ? C3 C4 C5 C6 -0.4(3) . . . . ? C4 C5 C6 N1 -1.5(3) . . . . ? C4 C5 C6 C7 175.54(17) . . . . ? N1 C6 C7 O3 176.62(16) . . . . ? C5 C6 C7 O3 -0.7(3) . . . . ? N1 C6 C7 O2 -1.8(2) . . . . ? C5 C6 C7 O2 -179.09(17) . . . . ? O4 Ti1 C8 C12 -115.96(12) . . . . ? O2 Ti1 C8 C12 159.09(11) . . . . ? O1 Ti1 C8 C12 15.95(12) . . . . ? N1 Ti1 C8 C12 91.66(11) . . . . ? C9 Ti1 C8 C12 -116.85(15) . . . . ? C10 Ti1 C8 C12 -78.67(11) . . . . ? C11 Ti1 C8 C12 -37.16(10) . . . . ? O4 Ti1 C8 C9 0.89(16) . . . . ? O2 Ti1 C8 C9 -84.06(11) . . . . ? O1 Ti1 C8 C9 132.80(10) . . . . ? N1 Ti1 C8 C9 -151.49(10) . . . . ? C10 Ti1 C8 C9 38.18(10) . . . . ? C11 Ti1 C8 C9 79.69(11) . . . . ? C12 Ti1 C8 C9 116.85(15) . . . . ? O4 Ti1 C8 C13 120.38(15) . . . . ? O2 Ti1 C8 C13 35.43(15) . . . . ? O1 Ti1 C8 C13 -107.71(15) . . . . ? N1 Ti1 C8 C13 -32.00(16) . . . . ? C9 Ti1 C8 C13 119.5(2) . . . . ? C10 Ti1 C8 C13 157.68(17) . . . . ? C11 Ti1 C8 C13 -160.82(18) . . . . ? C12 Ti1 C8 C13 -123.7(2) . . . . ? C12 C8 C9 C10 -2.0(2) . . . . ? C13 C8 C9 C10 177.36(17) . . . . ? Ti1 C8 C9 C10 -66.10(12) . . . . ? C12 C8 C9 C14 -177.97(17) . . . . ? C13 C8 C9 C14 1.4(3) . . . . ? Ti1 C8 C9 C14 117.97(18) . . . . ? C12 C8 C9 Ti1 64.06(12) . . . . ? C13 C8 C9 Ti1 -116.54(18) . . . . ? O4 Ti1 C9 C10 -64.80(11) . . . . ? O2 Ti1 C9 C10 -156.37(11) . . . . ? O1 Ti1 C9 C10 47.96(13) . . . . ? N1 Ti1 C9 C10 154.69(10) . . . . ? C11 Ti1 C9 C10 37.54(10) . . . . ? C8 Ti1 C9 C10 114.60(15) . . . . ? C12 Ti1 C9 C10 78.67(11) . . . . ? O4 Ti1 C9 C8 -179.41(10) . . . . ? O2 Ti1 C9 C8 89.02(11) . . . . ? O1 Ti1 C9 C8 -66.64(13) . . . . ? N1 Ti1 C9 C8 40.09(14) . . . . ? C10 Ti1 C9 C8 -114.60(15) . . . . ? C11 Ti1 C9 C8 -77.07(11) . . . . ? C12 Ti1 C9 C8 -35.93(10) . . . . ? O4 Ti1 C9 C14 56.50(15) . . . . ? O2 Ti1 C9 C14 -35.07(14) . . . . ? O1 Ti1 C9 C14 169.26(12) . . . . ? N1 Ti1 C9 C14 -84.01(16) . . . . ? C10 Ti1 C9 C14 121.30(19) . . . . ? C11 Ti1 C9 C14 158.84(17) . . . . ? C8 Ti1 C9 C14 -124.1(2) . . . . ? C12 Ti1 C9 C14 -160.03(17) . . . . ? C8 C9 C10 C11 2.3(2) . . . . ? C14 C9 C10 C11 178.27(17) . . . . ? Ti1 C9 C10 C11 -65.81(12) . . . . ? C8 C9 C10 C15 -177.53(18) . . . . ? C14 C9 C10 C15 -1.5(3) . . . . ? Ti1 C9 C10 C15 114.37(19) . . . . ? C8 C9 C10 Ti1 68.09(12) . . . . ? C14 C9 C10 Ti1 -115.92(18) . . . . ? O4 Ti1 C10 C11 -125.66(11) . . . . ? O2 Ti1 C10 C11 139.81(10) . . . . ? O1 Ti1 C10 C11 -30.33(12) . . . . ? N1 Ti1 C10 C11 48.1(2) . . . . ? C9 Ti1 C10 C11 115.10(15) . . . . ? C8 Ti1 C10 C11 77.34(11) . . . . ? C12 Ti1 C10 C11 37.34(10) . . . . ? O4 Ti1 C10 C9 119.24(11) . . . . ? O2 Ti1 C10 C9 24.71(12) . . . . ? O1 Ti1 C10 C9 -145.43(10) . . . . ? N1 Ti1 C10 C9 -67.0(2) . . . . ? C11 Ti1 C10 C9 -115.10(15) . . . . ? C8 Ti1 C10 C9 -37.76(10) . . . . ? C12 Ti1 C10 C9 -77.76(11) . . . . ? O4 Ti1 C10 C15 -2.56(15) . . . . ? O2 Ti1 C10 C15 -97.09(15) . . . . ? O1 Ti1 C10 C15 92.76(15) . . . . ? N1 Ti1 C10 C15 171.19(16) . . . . ? C9 Ti1 C10 C15 -121.8(2) . . . . ? C11 Ti1 C10 C15 123.1(2) . . . . ? C8 Ti1 C10 C15 -159.56(17) . . . . ? C12 Ti1 C10 C15 160.44(17) . . . . ? C9 C10 C11 C12 -1.7(2) . . . . ? C15 C10 C11 C12 178.15(18) . . . . ? Ti1 C10 C11 C12 -66.58(12) . . . . ? C9 C10 C11 C16 -176.68(17) . . . . ? C15 C10 C11 C16 3.1(3) . . . . ? Ti1 C10 C11 C16 118.40(18) . . . . ? C9 C10 C11 Ti1 64.92(12) . . . . ? C15 C10 C11 Ti1 -115.27(19) . . . . ? O4 Ti1 C11 C10 58.92(12) . . . . ? O2 Ti1 C11 C10 -56.89(13) . . . . ? O1 Ti1 C11 C10 149.97(12) . . . . ? N1 Ti1 C11 C10 -161.02(10) . . . . ? C9 Ti1 C11 C10 -37.90(11) . . . . ? C8 Ti1 C11 C10 -79.27(11) . . . . ? C12 Ti1 C11 C10 -115.41(15) . . . . ? O4 Ti1 C11 C12 174.32(10) . . . . ? O2 Ti1 C11 C12 58.52(13) . . . . ? O1 Ti1 C11 C12 -94.62(11) . . . . ? N1 Ti1 C11 C12 -45.61(13) . . . . ? C9 Ti1 C11 C12 77.51(11) . . . . ? C10 Ti1 C11 C12 115.41(15) . . . . ? C8 Ti1 C11 C12 36.14(10) . . . . ? O4 Ti1 C11 C16 -63.16(16) . . . . ? O2 Ti1 C11 C16 -178.96(13) . . . . ? O1 Ti1 C11 C16 27.90(15) . . . . ? N1 Ti1 C11 C16 76.91(17) . . . . ? C9 Ti1 C11 C16 -159.97(18) . . . . ? C10 Ti1 C11 C16 -122.1(2) . . . . ? C8 Ti1 C11 C16 158.66(18) . . . . ? C12 Ti1 C11 C16 122.5(2) . . . . ? C9 C8 C12 C11 1.0(2) . . . . ? C13 C8 C12 C11 -178.39(17) . . . . ? Ti1 C8 C12 C11 62.62(12) . . . . ? C9 C8 C12 C17 -179.27(17) . . . . ? C13 C8 C12 C17 1.3(3) . . . . ? Ti1 C8 C12 C17 -117.64(18) . . . . ? C9 C8 C12 Ti1 -61.63(12) . . . . ? C13 C8 C12 Ti1 118.99(19) . . . . ? C10 C11 C12 C8 0.4(2) . . . . ? C16 C11 C12 C8 175.50(17) . . . . ? Ti1 C11 C12 C8 -64.11(12) . . . . ? C10 C11 C12 C17 -179.33(17) . . . . ? C16 C11 C12 C17 -4.2(3) . . . . ? Ti1 C11 C12 C17 116.15(17) . . . . ? C10 C11 C12 Ti1 64.52(12) . . . . ? C16 C11 C12 Ti1 -120.39(18) . . . . ? O4 Ti1 C12 C8 107.71(13) . . . . ? O2 Ti1 C12 C8 -22.09(12) . . . . ? O1 Ti1 C12 C8 -165.19(11) . . . . ? N1 Ti1 C12 C8 -97.35(11) . . . . ? C9 Ti1 C12 C8 37.13(10) . . . . ? C10 Ti1 C12 C8 79.00(11) . . . . ? C11 Ti1 C12 C8 116.58(15) . . . . ? O4 Ti1 C12 C11 -8.87(16) . . . . ? O2 Ti1 C12 C11 -138.67(10) . . . . ? O1 Ti1 C12 C11 78.23(11) . . . . ? N1 Ti1 C12 C11 146.07(10) . . . . ? C9 Ti1 C12 C11 -79.45(11) . . . . ? C10 Ti1 C12 C11 -37.58(10) . . . . ? C8 Ti1 C12 C11 -116.58(15) . . . . ? O4 Ti1 C12 C17 -128.32(15) . . . . ? O2 Ti1 C12 C17 101.87(15) . . . . ? O1 Ti1 C12 C17 -41.22(14) . . . . ? N1 Ti1 C12 C17 26.61(16) . . . . ? C9 Ti1 C12 C17 161.09(17) . . . . ? C10 Ti1 C12 C17 -157.04(17) . . . . ? C11 Ti1 C12 C17 -119.46(19) . . . . ? C8 Ti1 C12 C17 124.0(2) . . . . ? O4 Rh1 C18 C25 95.88(11) . . . . ? C22 Rh1 C18 C25 -66.56(12) . . . . ? C21 Rh1 C18 C25 -101.99(12) . . . . ? O5 Rh1 C18 C25 177.46(18) . . . . ? O4 Rh1 C18 C19 -143.22(14) . . . . ? C22 Rh1 C18 C19 54.34(15) . . . . ? C25 Rh1 C18 C19 120.90(19) . . . . ? C21 Rh1 C18 C19 18.91(14) . . . . ? O5 Rh1 C18 C19 -61.6(3) . . . . ? C25 C18 C19 C20 50.2(3) . . . . ? Rh1 C18 C19 C20 -30.8(2) . . . . ? C18 C19 C20 C21 27.7(2) . . . . ? C19 C20 C21 C22 -92.3(2) . . . . ? C19 C20 C21 Rh1 -11.7(2) . . . . ? O4 Rh1 C21 C22 176.80(15) . . . . ? C18 Rh1 C21 C22 114.19(12) . . . . ? C25 Rh1 C21 C22 76.17(12) . . . . ? O5 Rh1 C21 C22 -82.83(11) . . . . ? O4 Rh1 C21 C20 58.8(2) . . . . ? C18 Rh1 C21 C20 -3.84(14) . . . . ? C22 Rh1 C21 C20 -118.02(19) . . . . ? C25 Rh1 C21 C20 -41.85(14) . . . . ? O5 Rh1 C21 C20 159.14(13) . . . . ? C20 C21 C22 C23 1.6(3) . . . . ? Rh1 C21 C22 C23 -104.01(17) . . . . ? C20 C21 C22 Rh1 105.63(17) . . . . ? O4 Rh1 C22 C21 -176.56(16) . . . . ? C18 Rh1 C22 C21 -66.23(12) . . . . ? C25 Rh1 C22 C21 -101.84(12) . . . . ? O5 Rh1 C22 C21 98.35(11) . . . . ? O4 Rh1 C22 C23 -56.8(3) . . . . ? C18 Rh1 C22 C23 53.55(15) . . . . ? C25 Rh1 C22 C23 17.94(14) . . . . ? C21 Rh1 C22 C23 119.78(19) . . . . ? O5 Rh1 C22 C23 -141.88(14) . . . . ? C21 C22 C23 C24 52.1(2) . . . . ? Rh1 C22 C23 C24 -29.0(2) . . . . ? C22 C23 C24 C25 26.1(2) . . . . ? C19 C18 C25 C24 2.6(3) . . . . ? Rh1 C18 C25 C24 105.94(17) . . . . ? C19 C18 C25 Rh1 -103.32(18) . . . . ? C23 C24 C25 C18 -91.9(2) . . . . ? C23 C24 C25 Rh1 -11.1(2) . . . . ? O4 Rh1 C25 C18 -84.18(11) . . . . ? C22 Rh1 C25 C18 113.90(12) . . . . ? C21 Rh1 C25 C18 75.96(12) . . . . ? O5 Rh1 C25 C18 -177.98(14) . . . . ? O4 Rh1 C25 C24 158.26(14) . . . . ? C18 Rh1 C25 C24 -117.56(18) . . . . ? C22 Rh1 C25 C24 -3.66(14) . . . . ? C21 Rh1 C25 C24 -41.61(14) . . . . ? O5 Rh1 C25 C24 64.5(2) . . . . ? C5 C6 N1 C2 2.3(3) . . . . ? C7 C6 N1 C2 -175.19(15) . . . . ? C5 C6 N1 Ti1 177.77(13) . . . . ? C7 C6 N1 Ti1 0.3(2) . . . . ? C3 C2 N1 C6 -1.0(3) . . . . ? C1 C2 N1 C6 177.52(15) . . . . ? C3 C2 N1 Ti1 -176.47(13) . . . . ? C1 C2 N1 Ti1 2.05(19) . . . . ? O4 Ti1 N1 C6 -87.41(14) . . . . ? O2 Ti1 N1 C6 0.71(13) . . . . ? O1 Ti1 N1 C6 -176.23(14) . . . . ? C9 Ti1 N1 C6 51.79(16) . . . . ? C10 Ti1 N1 C6 99.2(2) . . . . ? C11 Ti1 N1 C6 133.04(13) . . . . ? C8 Ti1 N1 C6 74.02(14) . . . . ? C12 Ti1 N1 C6 108.53(13) . . . . ? O4 Ti1 N1 C2 88.12(14) . . . . ? O2 Ti1 N1 C2 176.23(15) . . . . ? O1 Ti1 N1 C2 -0.71(13) . . . . ? C9 Ti1 N1 C2 -132.69(13) . . . . ? C10 Ti1 N1 C2 -85.2(2) . . . . ? C11 Ti1 N1 C2 -51.43(16) . . . . ? C8 Ti1 N1 C2 -110.45(14) . . . . ? C12 Ti1 N1 C2 -75.94(14) . . . . ? O5 C1 O1 Ti1 -176.49(13) 3_656 . . . ? C2 C1 O1 Ti1 2.6(2) . . . . ? O4 Ti1 O1 C1 -110.73(14) . . . . ? O2 Ti1 O1 C1 -5.96(18) . . . . ? N1 Ti1 O1 C1 -1.19(13) . . . . ? C9 Ti1 O1 C1 132.52(14) . . . . ? C10 Ti1 O1 C1 158.73(14) . . . . ? C11 Ti1 O1 C1 141.56(15) . . . . ? C8 Ti1 O1 C1 98.08(14) . . . . ? C12 Ti1 O1 C1 106.89(14) . . . . ? O3 C7 O2 Ti1 -175.58(14) . . . . ? C6 C7 O2 Ti1 2.7(2) . . . . ? O4 Ti1 O2 C7 107.81(14) . . . . ? O1 Ti1 O2 C7 2.77(18) . . . . ? N1 Ti1 O2 C7 -1.99(13) . . . . ? C9 Ti1 O2 C7 -147.42(15) . . . . ? C10 Ti1 O2 C7 -161.54(13) . . . . ? C11 Ti1 O2 C7 -131.15(14) . . . . ? C8 Ti1 O2 C7 -112.30(14) . . . . ? C12 Ti1 O2 C7 -100.16(14) . . . . ? O2 Ti1 O4 Rh1 -29.2(3) . . . . ? O1 Ti1 O4 Rh1 114.7(3) . . . . ? N1 Ti1 O4 Rh1 42.9(3) . . . . ? C9 Ti1 O4 Rh1 -108.2(3) . . . . ? C10 Ti1 O4 Rh1 -139.3(3) . . . . ? C11 Ti1 O4 Rh1 -168.4(3) . . . . ? C8 Ti1 O4 Rh1 -108.7(3) . . . . ? C12 Ti1 O4 Rh1 -163.1(3) . . . . ? C18 Rh1 O4 Ti1 -5.9(3) . . . . ? C22 Rh1 O4 Ti1 106.1(4) . . . . ? C25 Rh1 O4 Ti1 32.9(3) . . . . ? C21 Rh1 O4 Ti1 -67.6(4) . . . . ? O5 Rh1 O4 Ti1 -168.9(3) . . . . ? O4 Rh1 O5 C1 73.75(13) . . . 3_656 ? C18 Rh1 O5 C1 -7.6(3) . . . 3_656 ? C22 Rh1 O5 C1 -124.93(14) . . . 3_656 ? C25 Rh1 O5 C1 168.08(17) . . . 3_656 ? C21 Rh1 O5 C1 -86.38(14) . . . 3_656 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 70.54 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.556 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.070