Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'An, Jin' ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; 'van Niekerk, Lizette' ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; 'Esterhuysen, Catharine' ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; 'Raubenheimer, Helgard G.' ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; _publ_contact_author_name 'Prof Helgard G. Raubenheimer' _publ_contact_author_address ; Department of Chemistry Stellenbosch University Private Bag X1 Matieland 7602 SOUTH AFRICA ; _publ_contact_author_email hgr@sun.ac.za _publ_requested_journal ; Journal of the Chemical Society, Dalton Transactions ; _publ_section_title ; Mono- and bidentate group 6-coordinated and titanium-containing isocyanide ligands prepared from benzoxazole ; _publ_section_references ; Farrugia, L.J. (1997). J. Appl. Cryst. 30, 565. Nonius BV (1998) COLLECT. Data collection software. Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997) Methods Enzymol., 276, 307. Sheldrick, G.M. (1997). SHELX-97. Program for crystal structure analysis. Univ. of Gottingen, Germany. ; data_1 _database_code_CSD 178238 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2-{\h^5^-Dicyclopentadienyl(chloro)titanium(IV))oxyphenyl}isocyanide pentacarbonylchromium(0) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H14 Cl Cr N O6 Ti' _chemical_formula_sum 'C22 H14 Cl1 Cr1 N1 O6 Ti1' _chemical_formula_weight 523.69 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' 'Cl' 'Cl' 0.1484 0.1585 '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 25.700(1) _cell_length_b 10.426(1) _cell_length_c 16.804(2) _cell_angle_alpha 90.000 _cell_angle_beta 99.044(2) _cell_angle_gamma 90.000 _cell_volume 4446.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 176(2) _cell_measurement_reflns_used 3351 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 26.00 _exptl_crystal_description prism _exptl_crystal_colour 'orange-red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 176(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_reflns_number 10123 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4163 _reflns_number_gt 3356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material 'SHELX-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. ; _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^)+(0.0536P)^2^+3.4078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 4163 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.003 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 Ti Ti 0.314762(15) 0.26190(3) 0.16796(2) 0.02185(12) Uani 1 1 d . . . Cr Cr 0.455726(14) 0.24566(3) -0.09132(2) 0.03048(12) Uani 1 1 d . . . Cl Cl 0.22647(2) 0.29739(7) 0.18836(4) 0.04512(19) Uani 1 1 d . . . O6 O 0.31251(6) 0.37814(13) 0.08006(8) 0.0288(4) Uani 1 1 d . . . N N 0.38422(7) 0.44276(18) -0.01629(11) 0.0301(4) Uani 1 1 d . . . C7 C 0.35658(8) 0.5385(2) 0.01756(12) 0.0252(5) Uani 1 1 d . . . C8 C 0.31952(8) 0.50189(19) 0.06573(12) 0.0241(5) Uani 1 1 d . . . O2 O 0.39895(9) 0.2773(2) -0.26347(12) 0.0601(6) Uani 1 1 d . . . C4 C 0.49189(10) 0.2202(3) 0.01533(17) 0.0448(7) Uani 1 1 d . . . O3 O 0.38617(9) 0.01472(19) -0.07677(13) 0.0636(6) Uani 1 1 d . . . C2 C 0.41883(10) 0.2672(2) -0.19853(17) 0.0374(6) Uani 1 1 d . . . C12 C 0.36610(9) 0.6667(2) 0.00248(13) 0.0309(5) Uani 1 1 d . . . H9 H 0.3921 0.6893 -0.0294 0.037 Uiso 1 1 calc R . . C6 C 0.40805(9) 0.3668(2) -0.04564(14) 0.0306(5) Uani 1 1 d . . . C17 C 0.29491(12) 0.0407(2) 0.16952(16) 0.0441(7) Uani 1 1 d . . . H17 H 0.2787 0.0092 0.2127 0.053 Uiso 1 1 calc R . . C3 C 0.41167(10) 0.1033(2) -0.08103(15) 0.0395(6) Uani 1 1 d . . . O5 O 0.52048(8) 0.4806(2) -0.11938(13) 0.0651(6) Uani 1 1 d . . . C20 C 0.39821(11) 0.2798(3) 0.24881(17) 0.0473(7) Uani 1 1 d . . . H20 H 0.4268 0.2321 0.2342 0.057 Uiso 1 1 calc R . . C9 C 0.29001(9) 0.5984(2) 0.09494(14) 0.0334(5) Uani 1 1 d . . . H6 H 0.2634 0.5769 0.1259 0.040 Uiso 1 1 calc R . . O1 O 0.53266(9) 0.0669(2) -0.15304(14) 0.0715(7) Uani 1 1 d . . . C13 C 0.34884(11) 0.0489(2) 0.16850(16) 0.0438(7) Uani 1 1 d . . . H13 H 0.3760 0.0203 0.2097 0.053 Uiso 1 1 calc R . . O4 O 0.51322(9) 0.2029(2) 0.07860(14) 0.0733(7) Uani 1 1 d . . . C10 C 0.29964(11) 0.7261(2) 0.07859(15) 0.0371(6) Uani 1 1 d . . . H11 H 0.2794 0.7911 0.0989 0.045 Uiso 1 1 calc R . . C16 C 0.26878(10) 0.0871(2) 0.09584(16) 0.0416(6) Uani 1 1 d . . . H16 H 0.2317 0.0911 0.0799 0.050 Uiso 1 1 calc R . . C1 C 0.50392(11) 0.1354(3) -0.12979(17) 0.0454(7) Uani 1 1 d . . . C18 C 0.33963(10) 0.4394(2) 0.25867(14) 0.0394(6) Uani 1 1 d . . . H18 H 0.3214 0.5188 0.2514 0.047 Uiso 1 1 calc R . . C5 C 0.49714(10) 0.3910(3) -0.10789(16) 0.0415(6) Uani 1 1 d . . . C14 C 0.35592(10) 0.1067(2) 0.09609(15) 0.0392(6) Uani 1 1 d . . . H14 H 0.3887 0.1289 0.0806 0.047 Uiso 1 1 calc R . . C22 C 0.32710(11) 0.3369(3) 0.30511(14) 0.0422(6) Uani 1 1 d . . . H22 H 0.2991 0.3347 0.3359 0.051 Uiso 1 1 calc R . . C19 C 0.38363(10) 0.4052(3) 0.22469(15) 0.0446(7) Uani 1 1 d . . . H19 H 0.4009 0.4580 0.1908 0.054 Uiso 1 1 calc R . . C15 C 0.30618(11) 0.1261(2) 0.05034(15) 0.0377(6) Uani 1 1 d . . . H15 H 0.2993 0.1602 -0.0027 0.045 Uiso 1 1 calc R . . C21 C 0.36250(13) 0.2382(3) 0.29869(16) 0.0487(8) Uani 1 1 d . . . H21 H 0.3626 0.1566 0.3237 0.058 Uiso 1 1 calc R . . C11 C 0.33772(11) 0.7607(2) 0.03382(16) 0.0379(6) Uani 1 1 d . . . H10 H 0.3444 0.8486 0.0246 0.046 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 Ti 0.0251(2) 0.0190(2) 0.0218(2) 0.00109(14) 0.00474(16) -0.00062(15) Cr 0.02532(19) 0.0301(2) 0.0372(2) -0.00109(16) 0.00881(17) 0.00164(15) Cl 0.0315(3) 0.0528(4) 0.0542(4) -0.0162(3) 0.0164(3) -0.0011(3) O6 0.0384(9) 0.0193(8) 0.0281(8) 0.0027(6) 0.0038(7) -0.0034(6) N 0.0311(10) 0.0298(11) 0.0298(10) -0.0036(8) 0.0053(8) -0.0007(8) C7 0.0291(11) 0.0216(11) 0.0240(11) -0.0030(9) 0.0015(9) 0.0004(9) C8 0.0296(11) 0.0175(10) 0.0241(11) 0.0005(8) 0.0011(9) -0.0027(8) O2 0.0711(15) 0.0599(13) 0.0448(12) -0.0072(10) -0.0047(11) 0.0184(11) C4 0.0342(14) 0.0496(16) 0.0497(17) 0.0076(13) 0.0037(12) -0.0029(12) O3 0.0840(16) 0.0426(12) 0.0729(14) -0.0220(10) 0.0391(12) -0.0236(11) C2 0.0349(13) 0.0309(13) 0.0471(16) -0.0053(11) 0.0084(12) 0.0089(10) C12 0.0356(12) 0.0293(12) 0.0265(12) 0.0054(10) 0.0011(10) -0.0079(10) C6 0.0291(11) 0.0297(12) 0.0332(13) -0.0005(10) 0.0056(10) -0.0044(10) C17 0.0711(19) 0.0196(12) 0.0466(16) 0.0023(11) 0.0248(14) -0.0064(12) C3 0.0460(15) 0.0331(13) 0.0436(15) -0.0126(12) 0.0196(12) -0.0010(12) O5 0.0513(12) 0.0600(14) 0.0847(16) 0.0083(12) 0.0127(11) -0.0222(11) C20 0.0322(13) 0.0607(18) 0.0439(16) -0.0076(14) -0.0096(12) 0.0061(13) C9 0.0387(13) 0.0308(12) 0.0320(12) -0.0002(10) 0.0098(10) 0.0022(11) O1 0.0613(14) 0.0644(14) 0.0981(18) 0.0083(13) 0.0413(13) 0.0296(12) C13 0.0607(17) 0.0248(12) 0.0432(15) -0.0009(11) -0.0001(13) 0.0183(12) O4 0.0653(14) 0.0883(17) 0.0590(14) 0.0180(13) -0.0127(12) -0.0043(13) C10 0.0491(15) 0.0226(12) 0.0399(15) -0.0041(10) 0.0076(12) 0.0104(11) C16 0.0405(14) 0.0261(12) 0.0566(16) -0.0159(12) 0.0029(12) -0.0059(11) C1 0.0406(14) 0.0434(16) 0.0564(17) 0.0083(13) 0.0203(13) 0.0109(13) C18 0.0511(15) 0.0325(13) 0.0315(13) -0.0058(11) -0.0025(11) -0.0053(12) C5 0.0323(12) 0.0437(15) 0.0497(16) -0.0025(12) 0.0095(11) -0.0027(12) C14 0.0454(14) 0.0294(13) 0.0465(15) -0.0057(11) 0.0186(12) 0.0087(11) C22 0.0550(16) 0.0482(16) 0.0225(12) -0.0041(11) 0.0030(11) -0.0005(14) C19 0.0380(14) 0.0513(17) 0.0406(15) -0.0001(13) -0.0062(11) -0.0191(13) C15 0.0654(17) 0.0192(11) 0.0283(12) -0.0063(9) 0.0069(12) 0.0065(11) C21 0.069(2) 0.0421(16) 0.0284(14) 0.0055(11) -0.0124(14) 0.0012(14) C11 0.0521(15) 0.0193(12) 0.0397(15) 0.0010(10) -0.0012(12) -0.0020(11) _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 Ti O6 1.9046(14) . ? Ti C21 2.355(2) . ? Ti C20 2.359(2) . ? Ti C17 2.363(2) . ? Ti C14 2.366(2) . ? Ti Cl 2.3766(7) . ? Ti C13 2.386(2) . ? Ti C16 2.395(2) . ? Ti C19 2.397(2) . ? Ti C22 2.407(2) . ? Ti C15 2.413(2) . ? Ti C18 2.419(2) . ? Cr C1 1.878(3) . ? Cr C3 1.892(3) . ? Cr C5 1.897(3) . ? Cr C4 1.903(3) . ? Cr C2 1.913(3) . ? Cr C6 1.995(2) . ? O6 C8 1.330(2) . ? N C6 1.158(3) . ? N C7 1.397(3) . ? C7 C12 1.389(3) . ? C7 C8 1.397(3) . ? C8 C9 1.395(3) . ? O2 C2 1.135(3) . ? C4 O4 1.132(3) . ? O3 C3 1.141(3) . ? C12 C11 1.375(3) . ? C12 H9 0.9500 . ? C17 C13 1.391(4) . ? C17 C16 1.399(4) . ? C17 H17 0.9500 . ? O5 C5 1.143(3) . ? C20 C21 1.405(4) . ? C20 C19 1.402(4) . ? C20 H20 0.9500 . ? C9 C10 1.390(3) . ? C9 H6 0.9500 . ? O1 C1 1.140(3) . ? C13 C14 1.395(4) . ? C13 H13 0.9500 . ? C10 C11 1.373(4) . ? C10 H11 0.9500 . ? C16 C15 1.380(4) . ? C16 H16 0.9500 . ? C18 C19 1.391(4) . ? C18 C22 1.391(4) . ? C18 H18 0.9500 . ? C14 C15 1.399(4) . ? C14 H14 0.9500 . ? C22 C21 1.388(4) . ? C22 H22 0.9500 . ? C19 H19 0.9500 . ? C15 H15 0.9500 . ? C21 H21 0.9500 . ? C11 H10 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ti C21 137.57(9) . . ? O6 Ti C20 108.08(9) . . ? C21 Ti C20 34.69(11) . . ? O6 Ti C17 130.49(8) . . ? C21 Ti C17 88.23(10) . . ? C20 Ti C17 104.44(10) . . ? O6 Ti C14 90.05(8) . . ? C21 Ti C14 101.27(10) . . ? C20 Ti C14 84.79(10) . . ? C17 Ti C14 56.83(9) . . ? O6 Ti Cl 95.71(5) . . ? C21 Ti Cl 104.54(9) . . ? C20 Ti Cl 134.98(8) . . ? C17 Ti Cl 86.43(8) . . ? C14 Ti Cl 133.93(7) . . ? O6 Ti C13 124.16(8) . . ? C21 Ti C13 76.23(9) . . ? C20 Ti C13 76.80(10) . . ? C17 Ti C13 34.07(9) . . ? C14 Ti C13 34.14(9) . . ? Cl Ti C13 120.16(8) . . ? O6 Ti C16 98.00(8) . . ? C21 Ti C16 122.39(9) . . ? C20 Ti C16 133.11(10) . . ? C17 Ti C16 34.19(9) . . ? C14 Ti C16 56.35(9) . . ? Cl Ti C16 77.59(7) . . ? C13 Ti C16 56.33(9) . . ? O6 Ti C19 80.92(8) . . ? C21 Ti C19 56.66(10) . . ? C20 Ti C19 34.29(9) . . ? C17 Ti C19 138.71(10) . . ? C14 Ti C19 105.55(10) . . ? Cl Ti C19 120.51(8) . . ? C13 Ti C19 109.34(10) . . ? C16 Ti C19 161.90(10) . . ? O6 Ti C22 121.28(8) . . ? C21 Ti C22 33.88(9) . . ? C20 Ti C22 56.75(10) . . ? C17 Ti C22 107.61(9) . . ? C14 Ti C22 135.14(9) . . ? Cl Ti C22 78.25(7) . . ? C13 Ti C22 107.79(9) . . ? C16 Ti C22 135.40(10) . . ? C19 Ti C22 55.86(10) . . ? O6 Ti C15 75.54(7) . . ? C21 Ti C15 132.06(9) . . ? C20 Ti C15 118.43(10) . . ? C17 Ti C15 56.25(9) . . ? C14 Ti C15 34.03(9) . . ? Cl Ti C15 104.07(7) . . ? C13 Ti C15 56.19(8) . . ? C16 Ti C15 33.36(9) . . ? C19 Ti C15 131.17(10) . . ? C22 Ti C15 162.99(9) . . ? O6 Ti C18 88.54(8) . . ? C21 Ti C18 56.29(9) . . ? C20 Ti C18 56.65(9) . . ? C17 Ti C18 140.89(9) . . ? C14 Ti C18 138.58(9) . . ? Cl Ti C18 87.35(7) . . ? C13 Ti C18 130.48(9) . . ? C16 Ti C18 164.06(10) . . ? C19 Ti C18 33.57(9) . . ? C22 Ti C18 33.50(9) . . ? C15 Ti C18 161.10(9) . . ? C1 Cr C3 89.28(11) . . ? C1 Cr C5 91.32(12) . . ? C3 Cr C5 176.37(11) . . ? C1 Cr C4 89.31(12) . . ? C3 Cr C4 90.87(11) . . ? C5 Cr C4 92.71(12) . . ? C1 Cr C2 90.23(11) . . ? C3 Cr C2 87.88(11) . . ? C5 Cr C2 88.53(11) . . ? C4 Cr C2 178.68(11) . . ? C1 Cr C6 176.58(11) . . ? C3 Cr C6 92.81(10) . . ? C5 Cr C6 86.76(10) . . ? C4 Cr C6 87.96(11) . . ? C2 Cr C6 92.55(10) . . ? C8 O6 Ti 140.29(13) . . ? C6 N C7 177.6(2) . . ? C12 C7 C8 121.6(2) . . ? C12 C7 N 119.8(2) . . ? C8 C7 N 118.53(19) . . ? O6 C8 C7 119.61(19) . . ? O6 C8 C9 122.7(2) . . ? C7 C8 C9 117.71(19) . . ? O4 C4 Cr 178.8(3) . . ? O2 C2 Cr 176.7(2) . . ? C11 C12 C7 119.8(2) . . ? C11 C12 H9 120.1 . . ? C7 C12 H9 120.1 . . ? N C6 Cr 174.14(19) . . ? C13 C17 C16 108.0(2) . . ? C13 C17 Ti 73.90(14) . . ? C16 C17 Ti 74.17(13) . . ? C13 C17 H17 126.0 . . ? C16 C17 H17 126.0 . . ? Ti C17 H17 117.9 . . ? O3 C3 Cr 177.3(2) . . ? C21 C20 C19 106.9(3) . . ? C21 C20 Ti 72.49(15) . . ? C19 C20 Ti 74.34(14) . . ? C21 C20 H20 126.6 . . ? C19 C20 H20 126.6 . . ? Ti C20 H20 118.6 . . ? C10 C9 C8 119.9(2) . . ? C10 C9 H6 120.1 . . ? C8 C9 H6 120.1 . . ? C17 C13 C14 107.7(2) . . ? C17 C13 Ti 72.03(14) . . ? C14 C13 Ti 72.13(13) . . ? C17 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? Ti C13 H13 121.4 . . ? C11 C10 C9 121.6(2) . . ? C11 C10 H11 119.2 . . ? C9 C10 H11 119.2 . . ? C15 C16 C17 108.2(2) . . ? C15 C16 Ti 74.03(14) . . ? C17 C16 Ti 71.64(14) . . ? C15 C16 H16 125.9 . . ? C17 C16 H16 125.9 . . ? Ti C16 H16 120.2 . . ? O1 C1 Cr 178.9(3) . . ? C19 C18 C22 108.0(2) . . ? C19 C18 Ti 72.33(14) . . ? C22 C18 Ti 72.77(14) . . ? C19 C18 H18 126.0 . . ? C22 C18 H18 126.0 . . ? Ti C18 H18 120.7 . . ? O5 C5 Cr 177.5(2) . . ? C13 C14 C15 108.0(2) . . ? C13 C14 Ti 73.73(14) . . ? C15 C14 Ti 74.81(14) . . ? C13 C14 H14 126.0 . . ? C15 C14 H14 126.0 . . ? Ti C14 H14 117.4 . . ? C21 C22 C18 108.3(3) . . ? C21 C22 Ti 70.99(14) . . ? C18 C22 Ti 73.72(14) . . ? C21 C22 H22 125.9 . . ? C18 C22 H22 125.9 . . ? Ti C22 H22 121.1 . . ? C18 C19 C20 108.5(3) . . ? C18 C19 Ti 74.10(14) . . ? C20 C19 Ti 71.37(14) . . ? C18 C19 H19 125.7 . . ? C20 C19 H19 125.7 . . ? Ti C19 H19 120.5 . . ? C16 C15 C14 108.0(2) . . ? C16 C15 Ti 72.61(13) . . ? C14 C15 Ti 71.16(13) . . ? C16 C15 H15 126.0 . . ? C14 C15 H15 126.0 . . ? Ti C15 H15 121.9 . . ? C22 C21 C20 108.4(2) . . ? C22 C21 Ti 75.13(14) . . ? C20 C21 Ti 72.82(14) . . ? C22 C21 H21 125.8 . . ? C20 C21 H21 125.8 . . ? Ti C21 H21 118.1 . . ? C10 C11 C12 119.3(2) . . ? C10 C11 H10 120.3 . . ? C12 C11 H10 120.3 . . ? _refine_diff_density_max 0.260 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.058 #===END data_2 _database_code_CSD 178239 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-2-(\h^5^-Dicyclopentadienylchlorotitanium(IV))bis(oxyphenylisocyanide) tetracarbonylchromium(0) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H18 Cr N2 O6 Ti' _chemical_formula_sum 'C28 H18 Cr1 N2 O6 Ti1' _chemical_formula_weight 578.34 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9512(1) _cell_length_b 14.8432(2) _cell_length_c 15.7525(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.6435(7) _cell_angle_gamma 90.00 _cell_volume 2597.39(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5895 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.89 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_reflns_number 17312 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.43 _reflns_number_total 5900 _reflns_number_gt 4499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material 'WINGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+1.1551P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 5900 _refine_ls_number_parameters 389 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C35A C 0.1082(19) 0.373(2) -0.3174(11) 0.086(8) Uani 0.370(19) 1 d PD A 1 H35A H 0.1730 0.3336 -0.3020 0.103 Uiso 0.370(19) 1 calc PR A 1 C34A C 0.1029(12) 0.462(2) -0.3489(10) 0.066(5) Uani 0.370(19) 1 d PD A 1 H34A H 0.1678 0.4929 -0.3541 0.079 Uiso 0.370(19) 1 calc PR A 1 C33A C -0.0117(16) 0.4980(12) -0.3712(13) 0.047(3) Uani 0.370(19) 1 d PD A 1 H33A H -0.0381 0.5541 -0.3970 0.057 Uiso 0.370(19) 1 calc PR A 1 C32A C -0.0795(16) 0.4327(15) -0.3472(15) 0.058(6) Uani 0.370(19) 1 d PD A 1 H32A H -0.1591 0.4384 -0.3521 0.069 Uiso 0.370(19) 1 calc PR A 1 C31A C -0.005(3) 0.3570(9) -0.3145(14) 0.062(6) Uani 0.370(19) 1 d PD A 1 H31A H -0.0286 0.3041 -0.2940 0.075 Uiso 0.370(19) 1 calc PR A 1 C31B C 0.0672(9) 0.3497(5) -0.3110(6) 0.051(2) Uani 0.630(19) 1 d PD A 2 H31B H 0.1046 0.2959 -0.2856 0.062 Uiso 0.630(19) 1 calc PR A 2 C32B C -0.0525(9) 0.3695(10) -0.3265(10) 0.056(2) Uani 0.630(19) 1 d PD A 2 H32B H -0.1086 0.3331 -0.3151 0.067 Uiso 0.630(19) 1 calc PR A 2 C33B C -0.0697(11) 0.4565(9) -0.3632(9) 0.065(4) Uani 0.630(19) 1 d PD A 2 H33B H -0.1413 0.4889 -0.3812 0.078 Uiso 0.630(19) 1 calc PR A 2 C34B C 0.0380(16) 0.4866(6) -0.3684(7) 0.063(3) Uani 0.630(19) 1 d PD A 2 H34B H 0.0501 0.5431 -0.3892 0.075 Uiso 0.630(19) 1 calc PR A 2 C35B C 0.1247(11) 0.4195(7) -0.3379(9) 0.069(3) Uani 0.630(19) 1 d PD A 2 H35B H 0.2035 0.4209 -0.3358 0.083 Uiso 0.630(19) 1 calc PR A 2 C1 C 0.3619(2) 0.12955(19) -0.08687(18) 0.0584(6) Uani 1 1 d . . . C2 C 0.5425(2) 0.1487(2) 0.07411(19) 0.0675(7) Uani 1 1 d . . . C3 C 0.3435(2) 0.05636(17) 0.05548(16) 0.0547(6) Uani 1 1 d . . . C4 C 0.3933(2) 0.20916(17) 0.14933(18) 0.0574(6) Uani 1 1 d . . . C5 C 0.2068(2) 0.21162(14) -0.01178(14) 0.0437(5) Uani 1 1 d . . . C6 C 0.4112(2) 0.29343(16) -0.01288(16) 0.0485(5) Uani 1 1 d . . . C11 C -0.01321(18) 0.25937(14) -0.06798(13) 0.0380(4) Uani 1 1 d . . . C12 C -0.04885(18) 0.33569(14) -0.12462(13) 0.0385(4) Uani 1 1 d . . . C13 C -0.1716(2) 0.35234(16) -0.16543(15) 0.0481(5) Uani 1 1 d . . . H13 H -0.1984 0.4014 -0.2044 0.058 Uiso 1 1 calc R . . C14 C -0.2546(2) 0.29704(17) -0.14888(17) 0.0538(6) Uani 1 1 d . . . H14 H -0.3364 0.3085 -0.1782 0.065 Uiso 1 1 calc R . . C15 C -0.2176(2) 0.22552(17) -0.08970(17) 0.0549(6) Uani 1 1 d . . . H15 H -0.2740 0.1905 -0.0769 0.066 Uiso 1 1 calc R . . C16 C -0.0973(2) 0.20604(15) -0.04952(15) 0.0474(5) Uani 1 1 d . . . H16 H -0.0719 0.1573 -0.0100 0.057 Uiso 1 1 calc R . . C21 C 0.45095(19) 0.42936(14) -0.09572(14) 0.0432(5) Uani 1 1 d . . . C22 C 0.3513(2) 0.47749(14) -0.15292(15) 0.0443(5) Uani 1 1 d . . . C23 C 0.3729(2) 0.54593(17) -0.20578(17) 0.0574(6) Uani 1 1 d . . . H23 H 0.3085 0.5793 -0.2447 0.069 Uiso 1 1 calc R . . C24 C 0.4871(3) 0.56475(19) -0.20145(19) 0.0652(7) Uani 1 1 d . . . H24 H 0.4990 0.6095 -0.2386 0.078 Uiso 1 1 calc R . . C25 C 0.5833(3) 0.5186(2) -0.1432(2) 0.0728(8) Uani 1 1 d . . . H25 H 0.6607 0.5331 -0.1393 0.087 Uiso 1 1 calc R . . C26 C 0.5659(2) 0.45033(19) -0.09018(19) 0.0620(7) Uani 1 1 d . . . H26 H 0.6315 0.4185 -0.0507 0.074 Uiso 1 1 calc R . . C41 C 0.0867(3) 0.5806(2) -0.0889(2) 0.0794(9) Uani 1 1 d . . . H41 H 0.1209 0.5631 -0.0280 0.095 Uiso 1 1 calc R . . C42 C 0.1449(3) 0.6189(2) -0.1364(2) 0.0858(10) Uani 1 1 d . . . H42 H 0.2262 0.6337 -0.1132 0.103 Uiso 1 1 calc R . . C43 C 0.0714(5) 0.6329(2) -0.2213(2) 0.1006(13) Uani 1 1 d . A . H43 H 0.0937 0.6572 -0.2671 0.121 Uiso 1 1 calc R . . C44 C -0.0410(4) 0.6069(3) -0.2319(3) 0.123(2) Uani 1 1 d . A . H44 H -0.1096 0.6113 -0.2847 0.147 Uiso 1 1 calc R . . C45 C -0.0338(4) 0.5709(3) -0.1445(4) 0.1196(17) Uani 1 1 d . A . H45 H -0.0956 0.5468 -0.1291 0.143 Uiso 1 1 calc R . . N5 N 0.10782(17) 0.23543(12) -0.03323(11) 0.0447(4) Uani 1 1 d . . . N6 N 0.43195(17) 0.35729(13) -0.04609(13) 0.0502(4) Uani 1 1 d . . . O1 O 0.3544(2) 0.10030(18) -0.15557(15) 0.0976(7) Uani 1 1 d . . . O2 O 0.64335(19) 0.1344(2) 0.10217(18) 0.1183(10) Uani 1 1 d . . . O3 O 0.3244(2) -0.01645(13) 0.06890(15) 0.0855(6) Uani 1 1 d . . . O4 O 0.4023(2) 0.22521(16) 0.22219(14) 0.0901(7) Uani 1 1 d . . . O6 O 0.24276(14) 0.45639(12) -0.15466(12) 0.0591(4) Uani 1 1 d . A . O5 O 0.03450(13) 0.38711(11) -0.13677(10) 0.0519(4) Uani 1 1 d . A . Cr Cr 0.37755(3) 0.17357(2) 0.02958(2) 0.04453(11) Uani 1 1 d . . . Ti Ti 0.07476(3) 0.47377(2) -0.20975(2) 0.03984(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C35A 0.057(12) 0.15(2) 0.068(7) -0.003(14) 0.040(8) 0.037(13) C34A 0.046(7) 0.107(16) 0.045(6) -0.001(9) 0.017(5) 0.000(9) C33A 0.043(8) 0.047(6) 0.042(5) 0.002(4) 0.004(5) -0.006(5) C32A 0.058(9) 0.072(11) 0.045(10) -0.008(7) 0.022(8) -0.042(9) C31A 0.11(2) 0.029(5) 0.061(10) -0.008(4) 0.045(15) -0.017(10) C31B 0.050(6) 0.045(3) 0.068(4) -0.005(2) 0.032(4) 0.005(3) C32B 0.049(4) 0.064(6) 0.053(3) -0.007(4) 0.017(4) -0.014(4) C33B 0.070(9) 0.072(7) 0.039(4) -0.001(5) 0.004(4) 0.020(7) C34B 0.101(11) 0.045(4) 0.047(5) 0.007(3) 0.033(9) -0.003(6) C35B 0.081(6) 0.068(6) 0.084(7) -0.028(5) 0.059(6) -0.025(5) C1 0.0490(14) 0.0664(16) 0.0619(15) 0.0096(13) 0.0228(12) 0.0078(12) C2 0.0502(16) 0.0787(19) 0.0669(16) 0.0067(14) 0.0138(13) 0.0145(14) C3 0.0609(15) 0.0516(14) 0.0539(13) 0.0062(11) 0.0238(12) 0.0095(12) C4 0.0622(16) 0.0493(14) 0.0587(15) 0.0053(11) 0.0198(12) -0.0040(12) C5 0.0478(13) 0.0415(11) 0.0420(11) 0.0068(9) 0.0167(10) 0.0059(10) C6 0.0391(12) 0.0547(14) 0.0505(12) 0.0059(11) 0.0151(10) 0.0094(10) C11 0.0384(11) 0.0420(11) 0.0352(10) -0.0015(8) 0.0154(8) 0.0055(9) C12 0.0372(11) 0.0439(11) 0.0363(10) 0.0026(8) 0.0157(8) 0.0019(9) C13 0.0414(12) 0.0511(13) 0.0491(12) 0.0069(10) 0.0134(10) 0.0067(10) C14 0.0335(11) 0.0610(15) 0.0652(15) -0.0069(12) 0.0162(11) -0.0009(10) C15 0.0511(14) 0.0526(14) 0.0698(15) -0.0048(12) 0.0325(12) -0.0098(11) C16 0.0583(14) 0.0402(11) 0.0502(12) 0.0018(9) 0.0275(11) 0.0010(10) C21 0.0461(12) 0.0423(11) 0.0440(11) -0.0038(9) 0.0202(10) -0.0016(10) C22 0.0428(12) 0.0443(12) 0.0460(11) 0.0020(9) 0.0165(10) -0.0068(10) C23 0.0575(15) 0.0557(14) 0.0596(14) 0.0123(11) 0.0222(12) -0.0069(12) C24 0.0746(19) 0.0592(16) 0.0746(17) 0.0001(13) 0.0424(16) -0.0209(14) C25 0.0561(17) 0.081(2) 0.095(2) -0.0074(17) 0.0439(16) -0.0171(15) C26 0.0447(14) 0.0705(17) 0.0749(17) 0.0001(14) 0.0271(13) 0.0020(12) C41 0.103(3) 0.078(2) 0.0616(17) -0.0120(15) 0.0352(18) -0.0003(18) C42 0.111(3) 0.0642(19) 0.085(2) -0.0231(17) 0.039(2) -0.0212(18) C43 0.176(4) 0.0410(16) 0.070(2) 0.0015(14) 0.028(3) 0.014(2) C44 0.100(3) 0.084(3) 0.120(3) -0.048(2) -0.034(3) 0.058(2) C45 0.109(3) 0.073(2) 0.221(5) -0.054(3) 0.114(4) -0.010(2) N5 0.0448(11) 0.0478(10) 0.0409(9) 0.0050(8) 0.0152(8) 0.0093(8) N6 0.0499(11) 0.0475(11) 0.0547(11) 0.0061(9) 0.0212(9) 0.0070(9) O1 0.1043(18) 0.127(2) 0.0720(14) -0.0176(14) 0.0452(13) 0.0012(15) O2 0.0485(13) 0.177(3) 0.1127(19) -0.0012(19) 0.0103(12) 0.0335(16) O3 0.127(2) 0.0498(12) 0.0884(15) 0.0109(10) 0.0497(14) -0.0011(11) O4 0.126(2) 0.0861(16) 0.0630(12) -0.0098(11) 0.0405(13) -0.0205(14) O6 0.0391(9) 0.0663(11) 0.0678(11) 0.0278(9) 0.0149(8) -0.0029(8) O5 0.0390(8) 0.0643(10) 0.0510(9) 0.0198(8) 0.0150(7) -0.0014(7) Cr 0.0393(2) 0.0451(2) 0.0474(2) 0.00962(15) 0.01383(16) 0.00953(15) Ti 0.0407(2) 0.0365(2) 0.0403(2) 0.00809(15) 0.01257(16) 0.00272(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 C35A C31A 1.395(9) . ? C35A C34A 1.403(9) . ? C35A Ti 2.402(16) . ? C35A H35A 0.9300 . ? C34A C33A 1.389(9) . ? C34A Ti 2.343(15) . ? C34A H34A 0.9300 . ? C33A C32A 1.402(9) . ? C33A Ti 2.393(18) . ? C33A H33A 0.9300 . ? C32A C31A 1.406(10) . ? C32A Ti 2.35(2) . ? C32A H32A 0.9300 . ? C31A Ti 2.341(19) . ? C31A H31A 0.9300 . ? C31B C32B 1.392(7) . ? C31B C35B 1.393(7) . ? C31B Ti 2.416(8) . ? C31B H31B 0.9300 . ? C32B C33B 1.397(8) . ? C32B Ti 2.455(14) . ? C32B H32B 0.9300 . ? C33B C34B 1.394(7) . ? C33B Ti 2.411(12) . ? C33B H33B 0.9300 . ? C34B C35B 1.389(8) . ? C34B Ti 2.381(9) . ? C34B H34B 0.9300 . ? C35B Ti 2.443(10) . ? C35B H35B 0.9300 . ? C1 O1 1.139(3) . ? C1 Cr 1.890(3) . ? C2 O2 1.140(3) . ? C2 Cr 1.869(3) . ? C3 O3 1.140(3) . ? C3 Cr 1.866(3) . ? C4 O4 1.138(3) . ? C4 Cr 1.900(3) . ? C5 N5 1.160(3) . ? C5 Cr 1.981(2) . ? C6 N6 1.153(3) . ? C6 Cr 1.993(2) . ? C11 N5 1.391(3) . ? C11 C16 1.392(3) . ? C11 C12 1.407(3) . ? C12 O5 1.324(2) . ? C12 C13 1.389(3) . ? C13 C14 1.384(3) . ? C13 H13 0.9300 . ? C14 C15 1.374(3) . ? C14 H14 0.9300 . ? C15 C16 1.371(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C26 1.380(3) . ? C21 N6 1.392(3) . ? C21 C22 1.396(3) . ? C22 O6 1.325(3) . ? C22 C23 1.397(3) . ? C23 C24 1.370(4) . ? C23 H23 0.9300 . ? C24 C25 1.362(4) . ? C24 H24 0.9300 . ? C25 C26 1.377(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C41 C42 1.323(4) . ? C41 C45 1.389(6) . ? C41 Ti 2.442(3) . ? C41 H41 0.9300 . ? C42 C43 1.318(5) . ? C42 Ti 2.441(3) . ? C42 H42 0.9300 . ? C43 C44 1.348(6) . ? C43 Ti 2.369(3) . ? C43 H43 0.9300 . ? C44 C45 1.449(6) . ? C44 Ti 2.364(3) . ? C44 H44 0.9300 . ? C45 Ti 2.409(3) . ? C45 H45 0.9300 . ? O6 Ti 1.8883(17) . ? O5 Ti 1.9015(15) . ? 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 C31A C35A C34A 104.8(13) . . ? C31A C35A Ti 70.5(8) . . ? C34A C35A Ti 70.5(8) . . ? C31A C35A H35A 127.6 . . ? C34A C35A H35A 127.6 . . ? Ti C35A H35A 123.1 . . ? C33A C34A C35A 111.3(15) . . ? C33A C34A Ti 75.0(11) . . ? C35A C34A Ti 75.1(8) . . ? C33A C34A H34A 124.4 . . ? C35A C34A H34A 124.3 . . ? Ti C34A H34A 117.2 . . ? C34A C33A C32A 106.3(16) . . ? C34A C33A Ti 71.0(10) . . ? C32A C33A Ti 71.1(12) . . ? C34A C33A H33A 126.8 . . ? C32A C33A H33A 126.9 . . ? Ti C33A H33A 122.8 . . ? C33A C32A C31A 107.6(14) . . ? C33A C32A Ti 74.6(12) . . ? C31A C32A Ti 72.2(11) . . ? C33A C32A H32A 126.2 . . ? C31A C32A H32A 126.2 . . ? Ti C32A H32A 118.9 . . ? C35A C31A C32A 109.9(12) . . ? C35A C31A Ti 75.3(9) . . ? C32A C31A Ti 72.9(11) . . ? C35A C31A H31A 125.1 . . ? C32A C31A H31A 125.0 . . ? Ti C31A H31A 118.5 . . ? C32B C31B C35B 112.3(10) . . ? C32B C31B Ti 74.9(7) . . ? C35B C31B Ti 74.4(6) . . ? C32B C31B H31B 123.8 . . ? C35B C31B H31B 123.9 . . ? Ti C31B H31B 118.3 . . ? C31B C32B C33B 104.7(9) . . ? C31B C32B Ti 71.9(6) . . ? C33B C32B Ti 71.6(8) . . ? C31B C32B H32B 127.7 . . ? C33B C32B H32B 127.7 . . ? Ti C32B H32B 120.9 . . ? C34B C33B C32B 108.8(8) . . ? C34B C33B Ti 71.9(6) . . ? C32B C33B Ti 75.1(8) . . ? C34B C33B H33B 125.6 . . ? C32B C33B H33B 125.6 . . ? Ti C33B H33B 119.2 . . ? C35B C34B C33B 109.7(7) . . ? C35B C34B Ti 75.7(5) . . ? C33B C34B Ti 74.3(6) . . ? C35B C34B H34B 125.2 . . ? C33B C34B H34B 125.2 . . ? Ti C34B H34B 116.7 . . ? C34B C35B C31B 104.5(8) . . ? C34B C35B Ti 70.8(5) . . ? C31B C35B Ti 72.3(5) . . ? C34B C35B H35B 127.8 . . ? C31B C35B H35B 127.7 . . ? Ti C35B H35B 121.1 . . ? O1 C1 Cr 177.6(3) . . ? O2 C2 Cr 179.1(3) . . ? O3 C3 Cr 177.4(2) . . ? O4 C4 Cr 175.9(2) . . ? N5 C5 Cr 177.70(19) . . ? N6 C6 Cr 171.8(2) . . ? N5 C11 C16 119.93(19) . . ? N5 C11 C12 118.88(18) . . ? C16 C11 C12 121.15(19) . . ? O5 C12 C13 123.57(19) . . ? O5 C12 C11 119.20(18) . . ? C13 C12 C11 117.22(19) . . ? C14 C13 C12 121.0(2) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C15 C14 C13 120.8(2) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 119.7(2) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C11 119.9(2) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C26 C21 N6 120.2(2) . . ? C26 C21 C22 121.2(2) . . ? N6 C21 C22 118.59(19) . . ? O6 C22 C21 119.22(19) . . ? O6 C22 C23 123.7(2) . . ? C21 C22 C23 117.1(2) . . ? C24 C23 C22 121.2(2) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C23 120.6(2) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.0(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C21 119.8(3) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? C42 C41 C45 109.1(4) . . ? C42 C41 Ti 74.27(18) . . ? C45 C41 Ti 72.06(18) . . ? C42 C41 H41 125.5 . . ? C45 C41 H41 125.5 . . ? Ti C41 H41 119.9 . . ? C43 C42 C41 110.4(4) . . ? C43 C42 Ti 71.07(19) . . ? C41 C42 Ti 74.29(19) . . ? C43 C42 H42 124.8 . . ? C41 C42 H42 124.8 . . ? Ti C42 H42 121.4 . . ? C42 C43 C44 109.9(4) . . ? C42 C43 Ti 77.17(19) . . ? C44 C43 Ti 73.3(2) . . ? C42 C43 H43 125.0 . . ? C44 C43 H43 125.0 . . ? Ti C43 H43 116.4 . . ? C43 C44 C45 106.3(3) . . ? C43 C44 Ti 73.65(19) . . ? C45 C44 Ti 74.0(2) . . ? C43 C44 H44 126.8 . . ? C45 C44 H44 126.9 . . ? Ti C44 H44 117.7 . . ? C41 C45 C44 104.2(3) . . ? C41 C45 Ti 74.66(18) . . ? C44 C45 Ti 70.64(18) . . ? C41 C45 H45 127.9 . . ? C44 C45 H45 127.9 . . ? Ti C45 H45 119.0 . . ? C5 N5 C11 173.8(2) . . ? C6 N6 C21 173.4(2) . . ? C22 O6 Ti 147.59(15) . . ? C12 O5 Ti 148.12(14) . . ? C3 Cr C2 91.06(12) . . ? C3 Cr C1 86.46(11) . . ? C2 Cr C1 90.53(12) . . ? C3 Cr C4 89.54(11) . . ? C2 Cr C4 88.71(12) . . ? C1 Cr C4 175.92(11) . . ? C3 Cr C5 93.24(10) . . ? C2 Cr C5 174.40(11) . . ? C1 Cr C5 93.33(10) . . ? C4 Cr C5 87.73(10) . . ? C3 Cr C6 173.19(10) . . ? C2 Cr C6 89.26(11) . . ? C1 Cr C6 86.73(11) . . ? C4 Cr C6 97.27(10) . . ? C5 Cr C6 86.90(9) . . ? O6 Ti O5 95.33(7) . . ? O6 Ti C34A 85.7(3) . . ? O5 Ti C34A 132.1(7) . . ? O6 Ti C31A 108.2(7) . . ? O5 Ti C31A 78.3(4) . . ? C34A Ti C31A 56.5(6) . . ? O6 Ti C32A 136.7(5) . . ? O5 Ti C32A 95.4(5) . . ? C34A Ti C32A 56.8(6) . . ? C31A Ti C32A 34.9(3) . . ? O6 Ti C44 130.34(14) . . ? O5 Ti C44 112.95(18) . . ? C34A Ti C44 101.7(7) . . ? C31A Ti C44 116.8(6) . . ? C32A Ti C44 82.1(5) . . ? O6 Ti C43 99.02(14) . . ? O5 Ti C43 136.07(12) . . ? C34A Ti C43 90.4(7) . . ? C31A Ti C43 133.9(5) . . ? C32A Ti C43 101.7(5) . . ? C44 Ti C43 33.09(15) . . ? O6 Ti C34B 104.3(4) . . ? O5 Ti C34B 134.4(2) . . ? C34A Ti C34B 19.7(3) . . ? C31A Ti C34B 56.6(4) . . ? C32A Ti C34B 43.5(4) . . ? C44 Ti C34B 84.7(3) . . ? C43 Ti C34B 81.3(2) . . ? O6 Ti C33A 118.5(5) . . ? O5 Ti C33A 129.6(4) . . ? C34A Ti C33A 34.1(2) . . ? C31A Ti C33A 57.2(6) . . ? C32A Ti C33A 34.4(3) . . ? C44 Ti C33A 73.6(4) . . ? C43 Ti C33A 77.3(4) . . ? C34B Ti C33A 14.5(3) . . ? O6 Ti C35A 79.3(5) . . ? O5 Ti C35A 98.7(7) . . ? C34A Ti C35A 34.4(3) . . ? C31A Ti C35A 34.2(3) . . ? C32A Ti C35A 57.7(5) . . ? C44 Ti C35A 131.1(5) . . ? C43 Ti C35A 124.7(7) . . ? C34B Ti C35A 47.4(4) . . ? C33A Ti C35A 57.4(5) . . ? O6 Ti C45 122.29(15) . . ? O5 Ti C45 81.41(13) . . ? C34A Ti C45 136.9(7) . . ? C31A Ti C45 126.8(7) . . ? C32A Ti C45 100.7(5) . . ? C44 Ti C45 35.34(16) . . ? C43 Ti C45 55.89(15) . . ? C34B Ti C45 118.7(4) . . ? C33A Ti C45 105.9(5) . . ? C35A Ti C45 158.4(5) . . ? O6 Ti C33B 133.9(3) . . ? O5 Ti C33B 106.7(4) . . ? C34A Ti C33B 49.5(4) . . ? C31A Ti C33B 42.1(5) . . ? C32A Ti C33B 11.3(4) . . ? C44 Ti C33B 77.2(3) . . ? C43 Ti C33B 92.5(3) . . ? C34B Ti C33B 33.8(2) . . ? C33A Ti C33B 23.3(4) . . ? C35A Ti C33B 58.0(5) . . ? C45 Ti C33B 101.1(3) . . ? _refine_diff_density_max 0.568 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.047 #===END