# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Bezuidenhout, Daniela' _publ_contact_author_email daniela.bezuidenhout@up.ac.za loop_ _publ_author_name D.Bezuidenhout W.Barnard 'B.van der Westhuizen' 'E.van der Watt' ; D.Liles ; data_EvdW12_Complex_1b _database_code_depnum_ccdc_archive 'CCDC 810995' #TrackingRef '- Bezuidenhout_Barnard_vdWesthuizen_vdWatt_Liles_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Ethoxy-(benzo[b]thien-2-yl)-methylidene)-(pentacarbonyl)-tungsten ; _chemical_name_common ;(Ethoxy-(benzo(b)thien-2-yl)-methylidene)-(pentacarbonyl)- tungsten ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H10 O6 S W' _chemical_formula_sum 'C16 H10 O6 S W' _chemical_formula_weight 514.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.3964(6) _cell_length_b 7.7430(5) _cell_length_c 12.5316(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.757(1) _cell_angle_gamma 90.00 _cell_volume 881.68(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4432 _cell_measurement_theta_min 2.435 _cell_measurement_theta_max 26.536 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 6.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.285 _exptl_absorpt_correction_T_max 0.479 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _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 'Bruker (Siemens) P4' _diffrn_measurement_method '\f and \w scans' _diffrn_detector 'SMART 1000 CCD' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 4807 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 26.54 _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 1805 _reflns_number_gt 1750 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement ;SHELXTL and SHELXL-97 (Sheldrick, 1997) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 1997), POV-Ray (Cason, 2004) ; _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^)+(0.0415P)^2^+0.3160P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0067(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1805 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.931 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.108 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.723094(18) 0.2500 0.654898(14) 0.04146(12) Uani 1 2 d S . . C1 C 0.5372(6) 0.2500 0.5312(5) 0.0525(13) Uani 1 2 d S . . O1 O 0.4337(5) 0.2500 0.4603(4) 0.0836(14) Uani 1 2 d S . . C2 C 0.8021(4) 0.4311(5) 0.5674(3) 0.0493(8) Uani 1 1 d . . . O2 O 0.8373(4) 0.5278(5) 0.5104(3) 0.0727(9) Uani 1 1 d . . . C3 C 0.6339(4) 0.4413(5) 0.7290(3) 0.0516(8) Uani 1 1 d . . . O3 O 0.5832(5) 0.5485(5) 0.7695(3) 0.0824(10) Uani 1 1 d . . . C6 C 0.9135(6) 0.2500 0.7998(4) 0.0444(10) Uani 1 2 d S . . O6 O 1.0552(4) 0.2500 0.8056(3) 0.0519(8) Uani 1 2 d S . . S1 S 1.06352(14) 0.2500 1.02260(11) 0.0534(3) Uani 1 2 d S . . C7 C 0.9022(5) 0.2500 0.9146(4) 0.0446(10) Uani 1 2 d S . . C8 C 0.7809(6) 0.2500 0.9545(4) 0.0519(11) Uani 1 2 d S . . H8 H 0.6857 0.2500 0.9090 0.062 Uiso 1 2 calc SR . . C9 C 0.8114(6) 0.2500 1.0719(4) 0.0490(11) Uani 1 2 d S . . C10 C 0.7109(7) 0.2500 1.1386(5) 0.0629(16) Uani 1 2 d S . . H10 H 0.6100 0.2500 1.1071 0.075 Uiso 1 2 calc SR . . C11 C 0.7656(8) 0.2500 1.2500(5) 0.0664(15) Uani 1 2 d S . . H11 H 0.7008 0.2500 1.2951 0.080 Uiso 1 2 calc SR . . C12 C 0.9161(8) 0.2500 1.2980(5) 0.0656(15) Uani 1 2 d S . . H12 H 0.9500 0.2500 1.3745 0.079 Uiso 1 2 calc SR . . C13 C 1.0153(7) 0.2500 1.2350(5) 0.0586(13) Uani 1 2 d S . . H13 H 1.1159 0.2500 1.2679 0.070 Uiso 1 2 calc SR . . C14 C 0.9631(6) 0.2500 1.1211(4) 0.0493(11) Uani 1 2 d S . . C18 C 1.1112(6) 0.2500 0.7083(4) 0.0597(13) Uani 1 2 d S . . H18A H 1.0770 0.3517 0.6639 0.072 Uiso 0.50 1 calc PR . . H18B H 1.0770 0.1483 0.6639 0.072 Uiso 0.50 1 calc PR . . C19 C 1.2745(6) 0.2500 0.7457(6) 0.0681(15) Uani 1 2 d S . . H19A H 1.3149 0.2500 0.6826 0.102 Uiso 1 2 calc SR . . H19B H 1.3071 0.1488 0.7893 0.102 Uiso 0.50 1 calc PR . . H19C H 1.3071 0.3512 0.7893 0.102 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.03923(16) 0.04543(15) 0.04398(16) 0.000 0.01845(10) 0.000 C1 0.043(3) 0.064(3) 0.050(3) 0.000 0.010(2) 0.000 O1 0.060(3) 0.103(4) 0.078(3) 0.000 0.000(2) 0.000 C2 0.0482(19) 0.0539(19) 0.0507(18) 0.0052(16) 0.0216(16) -0.0004(16) O2 0.078(2) 0.078(2) 0.0715(18) 0.0188(17) 0.0368(16) -0.0011(17) C3 0.0505(19) 0.0520(19) 0.058(2) -0.0006(17) 0.0253(16) 0.0045(16) O3 0.099(3) 0.0672(18) 0.096(2) -0.0028(18) 0.052(2) 0.0178(18) C6 0.043(2) 0.044(2) 0.049(3) 0.000 0.018(2) 0.000 O6 0.0396(17) 0.072(2) 0.0491(19) 0.000 0.0209(15) 0.000 S1 0.0461(6) 0.0671(7) 0.0495(6) 0.000 0.0167(5) 0.000 C7 0.046(2) 0.047(2) 0.045(2) 0.000 0.019(2) 0.000 C8 0.051(3) 0.059(3) 0.049(3) 0.000 0.019(2) 0.000 C9 0.045(3) 0.056(3) 0.050(3) 0.000 0.020(2) 0.000 C10 0.065(4) 0.073(4) 0.060(3) 0.000 0.035(3) 0.000 C11 0.077(4) 0.079(4) 0.055(3) 0.000 0.040(3) 0.000 C12 0.086(4) 0.067(3) 0.047(3) 0.000 0.023(3) 0.000 C13 0.060(3) 0.067(3) 0.049(3) 0.000 0.014(2) 0.000 C14 0.054(3) 0.052(2) 0.047(3) 0.000 0.023(2) 0.000 C18 0.045(3) 0.089(4) 0.052(3) 0.000 0.025(2) 0.000 C19 0.048(3) 0.089(4) 0.077(4) 0.000 0.034(3) 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 W1 C1 2.018(6) . ? W1 C2 2.033(4) . ? W1 C3 2.039(4) . ? W1 C6 2.201(5) . ? C1 O1 1.138(7) . ? C2 O2 1.140(5) . ? C3 O3 1.139(5) . ? C6 O6 1.315(6) . ? C6 C7 1.469(7) . ? O6 C18 1.447(6) . ? S1 C14 1.734(5) . ? S1 C7 1.756(5) . ? C7 C8 1.356(7) . ? C8 C9 1.426(7) . ? C8 H8 0.9300 . ? C9 C14 1.402(7) . ? C9 C10 1.411(7) . ? C10 C11 1.359(8) . ? C10 H10 0.9300 . ? C11 C12 1.389(10) . ? C11 H11 0.9300 . ? C12 C13 1.367(8) . ? C12 H12 0.9300 . ? C13 C14 1.386(8) . ? C13 H13 0.9300 . ? C18 C19 1.487(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 W1 C2 87.08(17) . . ? C1 W1 C2 87.08(17) . 4_565 ? C2 W1 C2 87.2(2) . 4_565 ? C1 W1 C3 88.52(17) . 4_565 ? C2 W1 C3 174.70(13) . 4_565 ? C2 W1 C3 89.61(19) 4_565 4_565 ? C1 W1 C3 88.52(17) . . ? C2 W1 C3 89.62(19) . . ? C2 W1 C3 174.70(13) 4_565 . ? C3 W1 C3 93.2(2) 4_565 . ? C1 W1 C6 175.01(19) . . ? C2 W1 C6 96.52(15) . . ? C2 W1 C6 96.52(15) 4_565 . ? C3 W1 C6 88.05(15) 4_565 . ? C3 W1 C6 88.05(15) . . ? O1 C1 W1 179.0(6) . . ? O2 C2 W1 174.0(4) . . ? O3 C3 W1 179.4(4) . . ? O6 C6 C7 105.7(4) . . ? O6 C6 W1 130.1(4) . . ? C7 C6 W1 124.2(4) . . ? C6 O6 C18 122.3(4) . . ? C14 S1 C7 91.7(2) . . ? C8 C7 C6 129.6(5) . . ? C8 C7 S1 110.9(4) . . ? C6 C7 S1 119.4(4) . . ? C7 C8 C9 114.5(5) . . ? C7 C8 H8 122.8 . . ? C9 C8 H8 122.8 . . ? C14 C9 C10 119.9(5) . . ? C14 C9 C8 111.6(5) . . ? C10 C9 C8 128.5(5) . . ? C11 C10 C9 118.3(6) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C10 C11 C12 121.4(6) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 121.3(5) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C14 118.7(6) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C13 C14 C9 120.4(5) . . ? C13 C14 S1 128.2(5) . . ? C9 C14 S1 111.4(4) . . ? O6 C18 C19 107.6(5) . . ? O6 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? O6 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 W1 C6 O6 -43.96(11) . . . . ? C3 W1 C6 O6 -133.35(11) . . . . ? C2 W1 C6 C7 136.04(11) . . . . ? C3 W1 C6 C7 46.65(11) . . . . ? C7 C6 O6 C18 180.0 . . . . ? W1 C6 O6 C18 0.0 . . . . ? O6 C6 C7 C8 180.0 . . . . ? W1 C6 C7 C8 0.0 . . . . ? O6 C6 C7 S1 0.0 . . . . ? W1 C6 C7 S1 180.0 . . . . ? C14 S1 C7 C8 0.0 . . . . ? C14 S1 C7 C6 180.0 . . . . ? C6 C7 C8 C9 180.0 . . . . ? S1 C7 C8 C9 0.0 . . . . ? C7 C8 C9 C14 0.0 . . . . ? C7 C8 C9 C10 180.0 . . . . ? C14 C9 C10 C11 0.0 . . . . ? C8 C9 C10 C11 180.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C9 0.0 . . . . ? C12 C13 C14 S1 180.0 . . . . ? C10 C9 C14 C13 0.0 . . . . ? C8 C9 C14 C13 180.0 . . . . ? C10 C9 C14 S1 180.0 . . . . ? C8 C9 C14 S1 0.0 . . . . ? C7 S1 C14 C13 180.0 . . . . ? C7 S1 C14 C9 0.0 . . . . ? C6 O6 C18 C19 180.0 . . . . ? #END data_EvdW09_Complex_2b _database_code_depnum_ccdc_archive 'CCDC 810996' #TrackingRef '- Bezuidenhout_Barnard_vdWesthuizen_vdWatt_Liles_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ((Chloro-bis(\h^5^-pentadienyl)-titanium-oxy)-(benzo[b]thien-2-yl)-methylidene) -(pentacarbonyl)-tungsten dichloromethane solvate ; _chemical_name_common ; ((Chloro-bis(eta$5!-pentadienyl)-titanium-oxy)-(benzo(b)thien- 2-yl)-methylidene) -(pentacarbonyl)-tungsten dichloromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C24 H15 Cl O6 S Ti W, C H2 Cl2' _chemical_formula_sum 'C25 H17 Cl3 O6 S Ti W' _chemical_formula_weight 783.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3533(6) _cell_length_b 11.6696(6) _cell_length_c 12.3627(7) _cell_angle_alpha 66.392(1) _cell_angle_beta 88.689(1) _cell_angle_gamma 66.317(1) _cell_volume 1355.73(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6906 _cell_measurement_theta_min 2.908 _cell_measurement_theta_max 26.570 _exptl_crystal_description rectangular-prism _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 4.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.212 _exptl_absorpt_correction_T_max 0.276 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _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 'Bruker (Siemens) P4' _diffrn_measurement_method '\f and \w scans' _diffrn_detector 'SMART 1000 CCD' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 7350 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 26.57 _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _reflns_number_total 4908 _reflns_number_gt 4739 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement ;SHELXTL and SHELXL-97 (Sheldrick, 1997) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 1997), POV-Ray (Cason, 2004) ; _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^)+(0.0472P)^2^+1.0141P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4908 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.311 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.103 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.578583(12) 0.890836(13) 0.288402(11) 0.03433(7) Uani 1 1 d . . . C1 C 0.6784(4) 0.9824(4) 0.3257(4) 0.0421(8) Uani 1 1 d . . . O1 O 0.7385(3) 1.0313(4) 0.3483(3) 0.0613(8) Uani 1 1 d . . . C2 C 0.4160(4) 1.0763(5) 0.2093(4) 0.0495(10) Uani 1 1 d . . . O2 O 0.3328(4) 1.1819(4) 0.1570(4) 0.0804(12) Uani 1 1 d . . . C3 C 0.6292(4) 0.9346(5) 0.1244(4) 0.0472(9) Uani 1 1 d . . . O3 O 0.6598(5) 0.9604(5) 0.0320(3) 0.0829(12) Uani 1 1 d . . . C4 C 0.7472(4) 0.7171(4) 0.3497(4) 0.0436(9) Uani 1 1 d . . . O4 O 0.8470(3) 0.6248(4) 0.3779(4) 0.0710(10) Uani 1 1 d . . . C5 C 0.5299(4) 0.8486(5) 0.4559(4) 0.0498(10) Uani 1 1 d . . . O5 O 0.5073(4) 0.8246(5) 0.5503(3) 0.0821(12) Uani 1 1 d . . . C6 C 0.4682(3) 0.7801(4) 0.2676(3) 0.0336(7) Uani 1 1 d . . . O6 O 0.3566(2) 0.8009(3) 0.3003(2) 0.0389(5) Uani 1 1 d . . . S1 S 0.43424(9) 0.56443(10) 0.24504(9) 0.0419(2) Uani 1 1 d . . . C7 C 0.5152(3) 0.6699(4) 0.2258(3) 0.0359(7) Uani 1 1 d . . . C8 C 0.6200(4) 0.6355(4) 0.1692(4) 0.0439(8) Uani 1 1 d . . . H8 H 0.6747 0.6799 0.1519 0.053 Uiso 1 1 calc R . . C9 C 0.6368(4) 0.5236(4) 0.1391(4) 0.0418(8) Uani 1 1 d . . . C10 C 0.7305(4) 0.4647(5) 0.0768(4) 0.0518(10) Uani 1 1 d . . . H10 H 0.7936 0.4968 0.0506 0.062 Uiso 1 1 calc R . . C11 C 0.7269(5) 0.3601(4) 0.0560(4) 0.0544(11) Uani 1 1 d . . . H11 H 0.7874 0.3217 0.0140 0.065 Uiso 1 1 calc R . . C12 C 0.6356(5) 0.3101(4) 0.0958(4) 0.0556(11) Uani 1 1 d . . . H12 H 0.6366 0.2376 0.0809 0.067 Uiso 1 1 calc R . . C13 C 0.5424(4) 0.3646(4) 0.1571(4) 0.0490(9) Uani 1 1 d . . . H13 H 0.4813 0.3299 0.1842 0.059 Uiso 1 1 calc R . . C14 C 0.5436(4) 0.4733(4) 0.1769(3) 0.0394(8) Uani 1 1 d . . . Ti1 Ti 0.17781(6) 0.85315(6) 0.32641(6) 0.03333(14) Uani 1 1 d . . . Cl1 Cl 0.15870(12) 1.04861(11) 0.35376(11) 0.0606(3) Uani 1 1 d . . . C18 C -0.0116(4) 0.8930(6) 0.2127(4) 0.0608(12) Uani 1 1 d . . . H18 H -0.0730 0.8641 0.2503 0.073 Uiso 1 1 calc R . . C19 C 0.0962(4) 0.8152(5) 0.1761(4) 0.0561(10) Uani 1 1 d . . . H19 H 0.1214 0.7241 0.1880 0.067 Uiso 1 1 calc R . . C20 C 0.1598(4) 0.8977(5) 0.1185(4) 0.0519(10) Uani 1 1 d . . . H20 H 0.2328 0.8722 0.0825 0.062 Uiso 1 1 calc R . . C21 C 0.0970(5) 1.0229(5) 0.1238(4) 0.0610(12) Uani 1 1 d . . . H21 H 0.1207 1.0961 0.0939 0.073 Uiso 1 1 calc R . . C22 C -0.0120(4) 1.0199(5) 0.1839(4) 0.0668(13) Uani 1 1 d . . . H22 H -0.0720 1.0908 0.2004 0.080 Uiso 1 1 calc R . . C23 C 0.0698(6) 0.7682(7) 0.4827(6) 0.0811(19) Uani 1 1 d . . . H23 H -0.0206 0.8147 0.4708 0.097 Uiso 1 1 calc R . . C24 C 0.1366(8) 0.6647(7) 0.4498(5) 0.088(2) Uani 1 1 d . . . H24 H 0.1016 0.6262 0.4139 0.106 Uiso 1 1 calc R . . C25 C 0.2713(7) 0.6271(5) 0.4815(5) 0.102(3) Uani 1 1 d . . . H25 H 0.3438 0.5603 0.4707 0.122 Uiso 1 1 calc R . . C26 C 0.2675(7) 0.7158(8) 0.5331(4) 0.083(2) Uani 1 1 d . . . H26 H 0.3397 0.7190 0.5635 0.100 Uiso 1 1 calc R . . C27 C 0.1470(8) 0.7925(7) 0.5313(5) 0.0851(19) Uani 1 1 d . . . H27 H 0.1209 0.8578 0.5625 0.102 Uiso 1 1 calc R . . Cl2 Cl 0.97758(18) 0.59039(18) 0.11178(17) 0.0922(5) Uani 1 1 d . . . Cl3 Cl 1.1768(3) 0.3928(3) 0.3169(3) 0.1424(10) Uani 1 1 d . . . C28 C 1.0456(8) 0.4249(7) 0.2270(7) 0.101(2) Uani 1 1 d . . . H28A H 0.9797 0.4114 0.2753 0.122 Uiso 1 1 calc R . . H28B H 1.0719 0.3583 0.1929 0.122 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.03372(10) 0.03882(10) 0.03766(10) -0.01956(7) 0.00886(6) -0.01921(7) C1 0.041(2) 0.047(2) 0.045(2) -0.0222(17) 0.0081(16) -0.0234(17) O1 0.0561(19) 0.072(2) 0.075(2) -0.0390(18) 0.0071(16) -0.0374(17) C2 0.048(2) 0.046(2) 0.060(3) -0.024(2) 0.013(2) -0.024(2) O2 0.064(2) 0.0463(19) 0.102(3) -0.017(2) 0.012(2) -0.0108(18) C3 0.051(2) 0.055(2) 0.041(2) -0.0201(18) 0.0130(18) -0.030(2) O3 0.097(3) 0.112(3) 0.057(2) -0.034(2) 0.035(2) -0.064(3) C4 0.041(2) 0.044(2) 0.049(2) -0.0171(17) 0.0087(17) -0.0238(19) O4 0.049(2) 0.0545(19) 0.090(3) -0.0199(18) 0.0076(18) -0.0148(17) C5 0.050(2) 0.065(3) 0.047(2) -0.029(2) 0.0167(19) -0.031(2) O5 0.084(3) 0.126(4) 0.052(2) -0.043(2) 0.0269(19) -0.056(3) C6 0.0281(17) 0.0351(16) 0.0337(17) -0.0142(14) 0.0033(13) -0.0101(14) O6 0.0283(12) 0.0448(13) 0.0484(14) -0.0241(12) 0.0108(11) -0.0163(11) S1 0.0395(5) 0.0415(4) 0.0515(5) -0.0237(4) 0.0099(4) -0.0201(4) C7 0.0311(17) 0.0371(17) 0.0422(19) -0.0196(15) 0.0038(14) -0.0145(14) C8 0.037(2) 0.049(2) 0.056(2) -0.0329(18) 0.0109(17) -0.0180(17) C9 0.0335(18) 0.0441(19) 0.050(2) -0.0272(17) 0.0034(16) -0.0116(15) C10 0.043(2) 0.063(2) 0.058(2) -0.037(2) 0.0108(19) -0.0190(19) C11 0.054(3) 0.049(2) 0.049(2) -0.0273(19) 0.0021(19) -0.0047(19) C12 0.069(3) 0.0368(19) 0.054(2) -0.0255(18) -0.001(2) -0.0094(19) C13 0.058(3) 0.0355(18) 0.049(2) -0.0160(17) 0.0022(19) -0.0183(18) C14 0.0397(19) 0.0355(17) 0.0363(18) -0.0143(14) -0.0014(15) -0.0104(15) Ti1 0.0271(3) 0.0348(3) 0.0347(3) -0.0127(3) 0.0064(2) -0.0124(2) Cl1 0.0734(7) 0.0493(5) 0.0709(7) -0.0361(5) 0.0294(6) -0.0277(5) C18 0.038(2) 0.083(3) 0.054(3) -0.020(2) 0.0015(19) -0.027(2) C19 0.053(3) 0.069(3) 0.050(2) -0.027(2) -0.0006(19) -0.029(2) C20 0.044(2) 0.067(3) 0.0351(19) -0.0154(19) 0.0036(16) -0.021(2) C21 0.063(3) 0.052(2) 0.041(2) 0.0007(19) -0.003(2) -0.020(2) C22 0.037(2) 0.065(3) 0.062(3) -0.018(2) -0.005(2) 0.003(2) C23 0.062(3) 0.075(4) 0.070(4) -0.004(3) 0.031(3) -0.024(3) C24 0.157(7) 0.081(4) 0.046(3) -0.003(3) -0.001(3) -0.091(5) C25 0.104(5) 0.044(3) 0.067(3) 0.014(3) 0.052(4) 0.014(3) C26 0.084(4) 0.111(5) 0.040(3) 0.006(3) -0.010(3) -0.065(4) C27 0.126(6) 0.081(4) 0.052(3) -0.025(3) 0.032(4) -0.051(4) Cl2 0.0966(11) 0.0854(10) 0.1028(12) -0.0331(9) 0.0070(9) -0.0530(9) Cl3 0.1361(19) 0.1105(15) 0.159(2) -0.0679(15) -0.0536(16) -0.0191(13) C28 0.104(5) 0.075(4) 0.123(6) -0.032(4) -0.006(4) -0.046(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C1 2.007(4) . ? W1 C3 2.013(4) . ? W1 C4 2.017(4) . ? W1 C5 2.046(4) . ? W1 C2 2.056(4) . ? W1 C6 2.211(4) . ? C1 O1 1.149(5) . ? C2 O2 1.133(5) . ? C3 O3 1.143(6) . ? C4 O4 1.141(5) . ? C5 O5 1.135(6) . ? C6 O6 1.279(4) . ? C6 C7 1.474(5) . ? O6 Ti1 1.931(2) . ? S1 C14 1.730(4) . ? S1 C7 1.755(4) . ? C7 C8 1.368(5) . ? C8 C9 1.436(5) . ? C8 H8 0.9300 . ? C9 C14 1.394(6) . ? C9 C10 1.413(5) . ? C10 C11 1.360(6) . ? C10 H10 0.9300 . ? C11 C12 1.374(7) . ? C11 H11 0.9300 . ? C12 C13 1.382(6) . ? C12 H12 0.9300 . ? C13 C14 1.389(5) . ? C13 H13 0.9300 . ? Ti1 C24 2.343(5) . ? Ti1 C25 2.357(4) . ? Ti1 C23 2.356(5) . ? Ti1 Cl1 2.3623(12) . ? Ti1 C19 2.361(4) . ? Ti1 C22 2.365(4) . ? Ti1 C18 2.372(4) . ? Ti1 C26 2.379(5) . ? Ti1 C21 2.390(4) . ? Ti1 C27 2.401(5) . ? Ti1 C20 2.405(4) . ? C18 C22 1.376(8) . ? C18 C19 1.393(7) . ? C18 H18 0.9300 . ? C19 C20 1.393(6) . ? C19 H19 0.9300 . ? C20 C21 1.373(7) . ? C20 H20 0.9300 . ? C21 C22 1.434(7) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C27 1.252(10) . ? C23 C24 1.358(10) . ? C23 H23 0.9300 . ? C24 C25 1.428(10) . ? C24 H24 0.9300 . ? C25 C26 1.404(10) . ? C25 H25 0.9300 . ? C26 C27 1.294(10) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? Cl2 C28 1.733(7) . ? Cl3 C28 1.700(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 W1 C3 91.11(17) . . ? C1 W1 C4 86.56(16) . . ? C3 W1 C4 87.52(18) . . ? C1 W1 C5 87.41(17) . . ? C3 W1 C5 178.52(15) . . ? C4 W1 C5 92.33(18) . . ? C1 W1 C2 91.40(17) . . ? C3 W1 C2 86.38(18) . . ? C4 W1 C2 173.53(15) . . ? C5 W1 C2 93.71(18) . . ? C1 W1 C6 174.00(13) . . ? C3 W1 C6 94.68(15) . . ? C4 W1 C6 92.12(14) . . ? C5 W1 C6 86.79(16) . . ? C2 W1 C6 90.53(15) . . ? O1 C1 W1 178.1(4) . . ? O2 C2 W1 173.3(4) . . ? O3 C3 W1 178.5(4) . . ? O4 C4 W1 174.5(4) . . ? O5 C5 W1 177.5(4) . . ? O6 C6 C7 112.7(3) . . ? O6 C6 W1 121.2(3) . . ? C7 C6 W1 125.9(2) . . ? C6 O6 Ti1 171.7(3) . . ? C14 S1 C7 91.62(18) . . ? C8 C7 C6 127.7(3) . . ? C8 C7 S1 111.4(3) . . ? C6 C7 S1 120.9(3) . . ? C7 C8 C9 113.1(3) . . ? C7 C8 H8 123.5 . . ? C9 C8 H8 123.5 . . ? C14 C9 C10 119.1(4) . . ? C14 C9 C8 112.2(3) . . ? C10 C9 C8 128.7(4) . . ? C11 C10 C9 118.8(4) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 121.3(4) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 121.7(4) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C12 C13 C14 117.4(4) . . ? C12 C13 H13 121.3 . . ? C14 C13 H13 121.3 . . ? C13 C14 C9 121.6(4) . . ? C13 C14 S1 126.7(3) . . ? C9 C14 S1 111.7(3) . . ? O6 Ti1 C24 113.4(2) . . ? O6 Ti1 C25 81.32(18) . . ? C24 Ti1 C25 35.4(2) . . ? O6 Ti1 C23 135.78(18) . . ? C24 Ti1 C23 33.6(2) . . ? C25 Ti1 C23 56.3(2) . . ? O6 Ti1 Cl1 94.87(8) . . ? C24 Ti1 Cl1 129.93(18) . . ? C25 Ti1 Cl1 122.7(2) . . ? C23 Ti1 Cl1 97.9(2) . . ? O6 Ti1 C19 98.98(14) . . ? C24 Ti1 C19 81.37(18) . . ? C25 Ti1 C19 100.8(3) . . ? C23 Ti1 C19 100.6(2) . . ? Cl1 Ti1 C19 135.87(13) . . ? O6 Ti1 C22 127.24(15) . . ? C24 Ti1 C22 108.2(2) . . ? C25 Ti1 C22 143.3(3) . . ? C23 Ti1 C22 96.5(2) . . ? Cl1 Ti1 C22 81.64(15) . . ? C19 Ti1 C22 56.77(19) . . ? O6 Ti1 C18 131.83(15) . . ? C24 Ti1 C18 78.4(2) . . ? C25 Ti1 C18 111.1(3) . . ? C23 Ti1 C18 80.2(2) . . ? Cl1 Ti1 C18 112.99(14) . . ? C19 Ti1 C18 34.23(17) . . ? C22 Ti1 C18 33.76(19) . . ? O6 Ti1 C26 85.55(19) . . ? C24 Ti1 C26 55.9(2) . . ? C25 Ti1 C26 34.5(3) . . ? C23 Ti1 C26 52.9(2) . . ? Cl1 Ti1 C26 88.2(2) . . ? C19 Ti1 C26 134.3(2) . . ? C22 Ti1 C26 146.2(2) . . ? C18 Ti1 C26 131.38(19) . . ? O6 Ti1 C21 92.18(15) . . ? C24 Ti1 C21 134.1(2) . . ? C25 Ti1 C21 155.4(2) . . ? C23 Ti1 C21 131.5(2) . . ? Cl1 Ti1 C21 81.41(14) . . ? C19 Ti1 C21 56.49(18) . . ? C22 Ti1 C21 35.09(18) . . ? C18 Ti1 C21 56.81(18) . . ? C26 Ti1 C21 169.2(2) . . ? O6 Ti1 C27 115.5(2) . . ? C24 Ti1 C27 53.8(2) . . ? C25 Ti1 C27 55.0(2) . . ? C23 Ti1 C27 30.5(2) . . ? Cl1 Ti1 C27 77.14(17) . . ? C19 Ti1 C27 130.8(2) . . ? C22 Ti1 C27 114.8(2) . . ? C18 Ti1 C27 108.8(2) . . ? C26 Ti1 C27 31.4(2) . . ? C21 Ti1 C27 146.0(2) . . ? O6 Ti1 C20 77.38(13) . . ? C24 Ti1 C20 113.90(18) . . ? C25 Ti1 C20 122.4(2) . . ? C23 Ti1 C20 133.8(2) . . ? Cl1 Ti1 C20 112.09(12) . . ? C19 Ti1 C20 33.98(16) . . ? C22 Ti1 C20 56.55(17) . . ? C18 Ti1 C20 56.28(16) . . ? C26 Ti1 C20 154.2(2) . . ? C21 Ti1 C20 33.27(17) . . ? C27 Ti1 C20 164.2(2) . . ? C22 C18 C19 108.5(4) . . ? C22 C18 Ti1 72.8(3) . . ? C19 C18 Ti1 72.5(2) . . ? C22 C18 H18 125.8 . . ? C19 C18 H18 125.8 . . ? Ti1 C18 H18 120.7 . . ? C18 C19 C20 107.9(5) . . ? C18 C19 Ti1 73.3(3) . . ? C20 C19 Ti1 74.7(3) . . ? C18 C19 H19 126.0 . . ? C20 C19 H19 126.0 . . ? Ti1 C19 H19 117.9 . . ? C21 C20 C19 108.8(4) . . ? C21 C20 Ti1 72.8(3) . . ? C19 C20 Ti1 71.3(2) . . ? C21 C20 H20 125.6 . . ? C19 C20 H20 125.6 . . ? Ti1 C20 H20 122.0 . . ? C20 C21 C22 107.2(5) . . ? C20 C21 Ti1 74.0(2) . . ? C22 C21 Ti1 71.5(3) . . ? C20 C21 H21 126.4 . . ? C22 C21 H21 126.4 . . ? Ti1 C21 H21 120.0 . . ? C18 C22 C21 107.5(5) . . ? C18 C22 Ti1 73.4(3) . . ? C21 C22 Ti1 73.4(2) . . ? C18 C22 H22 126.3 . . ? C21 C22 H22 126.3 . . ? Ti1 C22 H22 118.9 . . ? C27 C23 C24 110.6(6) . . ? C27 C23 Ti1 76.7(4) . . ? C24 C23 Ti1 72.7(3) . . ? C27 C23 H23 124.7 . . ? C24 C23 H23 124.7 . . ? Ti1 C23 H23 117.6 . . ? C23 C24 C25 105.8(6) . . ? C23 C24 Ti1 73.7(3) . . ? C25 C24 Ti1 72.8(3) . . ? C23 C24 H24 127.1 . . ? C25 C24 H24 127.1 . . ? Ti1 C24 H24 118.5 . . ? C26 C25 C24 102.8(5) . . ? C26 C25 Ti1 73.6(3) . . ? C24 C25 Ti1 71.8(3) . . ? C26 C25 H25 128.6 . . ? C24 C25 H25 128.6 . . ? Ti1 C25 H25 118.5 . . ? C27 C26 C25 108.9(6) . . ? C27 C26 Ti1 75.2(3) . . ? C25 C26 Ti1 71.9(3) . . ? C27 C26 H26 125.6 . . ? C25 C26 H26 125.6 . . ? Ti1 C26 H26 119.1 . . ? C23 C27 C26 111.9(7) . . ? C23 C27 Ti1 72.8(4) . . ? C26 C27 Ti1 73.4(3) . . ? C23 C27 H27 124.0 . . ? C26 C27 H27 124.0 . . ? Ti1 C27 H27 121.3 . . ? Cl3 C28 Cl2 113.6(4) . . ? Cl3 C28 H28A 108.8 . . ? Cl2 C28 H28A 108.8 . . ? Cl3 C28 H28B 108.8 . . ? Cl2 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 W1 C6 O6 -135.6(3) . . . . ? C4 W1 C6 O6 136.7(3) . . . . ? C5 W1 C6 O6 44.5(3) . . . . ? C2 W1 C6 O6 -49.2(3) . . . . ? C3 W1 C6 C7 49.5(3) . . . . ? C4 W1 C6 C7 -38.2(3) . . . . ? C5 W1 C6 C7 -130.4(3) . . . . ? C2 W1 C6 C7 135.9(3) . . . . ? O6 C6 C7 C8 169.7(4) . . . . ? W1 C6 C7 C8 -15.0(5) . . . . ? O6 C6 C7 S1 -9.8(4) . . . . ? W1 C6 C7 S1 165.53(18) . . . . ? C14 S1 C7 C8 0.3(3) . . . . ? C14 S1 C7 C6 179.9(3) . . . . ? C6 C7 C8 C9 -179.1(3) . . . . ? S1 C7 C8 C9 0.4(4) . . . . ? C7 C8 C9 C14 -1.2(5) . . . . ? C7 C8 C9 C10 177.3(4) . . . . ? C14 C9 C10 C11 -0.2(6) . . . . ? C8 C9 C10 C11 -178.7(4) . . . . ? C9 C10 C11 C12 -1.0(7) . . . . ? C10 C11 C12 C13 0.9(7) . . . . ? C11 C12 C13 C14 0.4(6) . . . . ? C12 C13 C14 C9 -1.6(6) . . . . ? C12 C13 C14 S1 177.0(3) . . . . ? C10 C9 C14 C13 1.5(6) . . . . ? C8 C9 C14 C13 -179.8(4) . . . . ? C10 C9 C14 S1 -177.3(3) . . . . ? C8 C9 C14 S1 1.5(4) . . . . ? C7 S1 C14 C13 -179.7(4) . . . . ? C7 S1 C14 C9 -1.0(3) . . . . ? O6 Ti1 C18 C22 -97.0(3) . . . . ? C24 Ti1 C18 C22 151.9(4) . . . . ? C25 Ti1 C18 C22 165.6(3) . . . . ? C23 Ti1 C18 C22 117.7(4) . . . . ? Cl1 Ti1 C18 C22 23.2(3) . . . . ? C19 Ti1 C18 C22 -116.5(4) . . . . ? C26 Ti1 C18 C22 132.4(4) . . . . ? C21 Ti1 C18 C22 -38.7(3) . . . . ? C27 Ti1 C18 C22 106.8(3) . . . . ? C20 Ti1 C18 C22 -78.8(3) . . . . ? O6 Ti1 C18 C19 19.4(4) . . . . ? C24 Ti1 C18 C19 -91.7(4) . . . . ? C25 Ti1 C18 C19 -77.9(3) . . . . ? C23 Ti1 C18 C19 -125.8(3) . . . . ? Cl1 Ti1 C18 C19 139.7(3) . . . . ? C22 Ti1 C18 C19 116.5(4) . . . . ? C26 Ti1 C18 C19 -111.1(4) . . . . ? C21 Ti1 C18 C19 77.8(3) . . . . ? C27 Ti1 C18 C19 -136.7(3) . . . . ? C20 Ti1 C18 C19 37.7(3) . . . . ? C22 C18 C19 C20 -2.9(5) . . . . ? Ti1 C18 C19 C20 -67.3(3) . . . . ? C22 C18 C19 Ti1 64.4(3) . . . . ? O6 Ti1 C19 C18 -165.5(3) . . . . ? C24 Ti1 C19 C18 82.1(4) . . . . ? C25 Ti1 C19 C18 111.7(3) . . . . ? C23 Ti1 C19 C18 54.4(3) . . . . ? Cl1 Ti1 C19 C18 -58.8(3) . . . . ? C22 Ti1 C19 C18 -36.5(3) . . . . ? C26 Ti1 C19 C18 102.0(4) . . . . ? C21 Ti1 C19 C18 -78.8(3) . . . . ? C27 Ti1 C19 C18 59.1(4) . . . . ? C20 Ti1 C19 C18 -114.5(4) . . . . ? O6 Ti1 C19 C20 -50.9(3) . . . . ? C24 Ti1 C19 C20 -163.4(4) . . . . ? C25 Ti1 C19 C20 -133.7(3) . . . . ? C23 Ti1 C19 C20 168.9(3) . . . . ? Cl1 Ti1 C19 C20 55.7(3) . . . . ? C22 Ti1 C19 C20 78.0(3) . . . . ? C18 Ti1 C19 C20 114.5(4) . . . . ? C26 Ti1 C19 C20 -143.5(3) . . . . ? C21 Ti1 C19 C20 35.7(3) . . . . ? C27 Ti1 C19 C20 173.6(3) . . . . ? C18 C19 C20 C21 2.8(5) . . . . ? Ti1 C19 C20 C21 -63.5(3) . . . . ? C18 C19 C20 Ti1 66.3(3) . . . . ? O6 Ti1 C20 C21 -114.4(3) . . . . ? C24 Ti1 C20 C21 135.4(4) . . . . ? C25 Ti1 C20 C21 174.6(4) . . . . ? C23 Ti1 C20 C21 102.3(4) . . . . ? Cl1 Ti1 C20 C21 -24.2(3) . . . . ? C19 Ti1 C20 C21 117.4(4) . . . . ? C22 Ti1 C20 C21 38.7(3) . . . . ? C18 Ti1 C20 C21 79.5(3) . . . . ? C26 Ti1 C20 C21 -164.1(4) . . . . ? C27 Ti1 C20 C21 99.5(8) . . . . ? O6 Ti1 C20 C19 128.2(3) . . . . ? C24 Ti1 C20 C19 18.0(4) . . . . ? C25 Ti1 C20 C19 57.2(4) . . . . ? C23 Ti1 C20 C19 -15.2(4) . . . . ? Cl1 Ti1 C20 C19 -141.6(3) . . . . ? C22 Ti1 C20 C19 -78.8(3) . . . . ? C18 Ti1 C20 C19 -38.0(3) . . . . ? C26 Ti1 C20 C19 78.5(5) . . . . ? C21 Ti1 C20 C19 -117.4(4) . . . . ? C27 Ti1 C20 C19 -18.0(9) . . . . ? C19 C20 C21 C22 -1.6(5) . . . . ? Ti1 C20 C21 C22 -64.2(3) . . . . ? C19 C20 C21 Ti1 62.6(3) . . . . ? O6 Ti1 C21 C20 62.8(3) . . . . ? C24 Ti1 C21 C20 -63.3(5) . . . . ? C25 Ti1 C21 C20 -11.0(7) . . . . ? C23 Ti1 C21 C20 -109.6(4) . . . . ? Cl1 Ti1 C21 C20 157.4(3) . . . . ? C19 Ti1 C21 C20 -36.5(3) . . . . ? C22 Ti1 C21 C20 -114.9(5) . . . . ? C18 Ti1 C21 C20 -77.8(3) . . . . ? C26 Ti1 C21 C20 140.5(12) . . . . ? C27 Ti1 C21 C20 -151.4(4) . . . . ? O6 Ti1 C21 C22 177.7(3) . . . . ? C24 Ti1 C21 C22 51.6(5) . . . . ? C25 Ti1 C21 C22 104.0(6) . . . . ? C23 Ti1 C21 C22 5.3(5) . . . . ? Cl1 Ti1 C21 C22 -87.7(3) . . . . ? C19 Ti1 C21 C22 78.4(4) . . . . ? C18 Ti1 C21 C22 37.2(3) . . . . ? C26 Ti1 C21 C22 -104.6(12) . . . . ? C27 Ti1 C21 C22 -36.5(6) . . . . ? C20 Ti1 C21 C22 114.9(5) . . . . ? C19 C18 C22 C21 1.9(5) . . . . ? Ti1 C18 C22 C21 66.0(3) . . . . ? C19 C18 C22 Ti1 -64.1(3) . . . . ? C20 C21 C22 C18 -0.2(5) . . . . ? Ti1 C21 C22 C18 -66.0(3) . . . . ? C20 C21 C22 Ti1 65.9(3) . . . . ? O6 Ti1 C22 C18 111.7(3) . . . . ? C24 Ti1 C22 C18 -29.1(4) . . . . ? C25 Ti1 C22 C18 -22.9(5) . . . . ? C23 Ti1 C22 C18 -61.4(4) . . . . ? Cl1 Ti1 C22 C18 -158.5(3) . . . . ? C19 Ti1 C22 C18 37.0(3) . . . . ? C26 Ti1 C22 C18 -84.5(5) . . . . ? C21 Ti1 C22 C18 114.6(5) . . . . ? C27 Ti1 C22 C18 -86.9(4) . . . . ? C20 Ti1 C22 C18 78.0(3) . . . . ? O6 Ti1 C22 C21 -2.8(4) . . . . ? C24 Ti1 C22 C21 -143.7(4) . . . . ? C25 Ti1 C22 C21 -137.4(4) . . . . ? C23 Ti1 C22 C21 -176.0(4) . . . . ? Cl1 Ti1 C22 C21 86.9(3) . . . . ? C19 Ti1 C22 C21 -77.6(3) . . . . ? C18 Ti1 C22 C21 -114.6(5) . . . . ? C26 Ti1 C22 C21 161.0(4) . . . . ? C27 Ti1 C22 C21 158.5(3) . . . . ? C20 Ti1 C22 C21 -36.6(3) . . . . ? O6 Ti1 C23 C27 58.1(6) . . . . ? C24 Ti1 C23 C27 116.8(6) . . . . ? C25 Ti1 C23 C27 76.9(5) . . . . ? Cl1 Ti1 C23 C27 -47.3(5) . . . . ? C19 Ti1 C23 C27 173.0(5) . . . . ? C22 Ti1 C23 C27 -129.7(5) . . . . ? C18 Ti1 C23 C27 -159.4(5) . . . . ? C26 Ti1 C23 C27 34.4(4) . . . . ? C21 Ti1 C23 C27 -132.8(4) . . . . ? C20 Ti1 C23 C27 -178.5(4) . . . . ? O6 Ti1 C23 C24 -58.7(6) . . . . ? C25 Ti1 C23 C24 -39.9(4) . . . . ? Cl1 Ti1 C23 C24 -164.1(4) . . . . ? C19 Ti1 C23 C24 56.1(4) . . . . ? C22 Ti1 C23 C24 113.4(4) . . . . ? C18 Ti1 C23 C24 83.8(5) . . . . ? C26 Ti1 C23 C24 -82.4(4) . . . . ? C21 Ti1 C23 C24 110.4(4) . . . . ? C27 Ti1 C23 C24 -116.8(6) . . . . ? C20 Ti1 C23 C24 64.7(5) . . . . ? C27 C23 C24 C25 -1.7(6) . . . . ? Ti1 C23 C24 C25 66.3(3) . . . . ? C27 C23 C24 Ti1 -68.0(4) . . . . ? O6 Ti1 C24 C23 139.5(4) . . . . ? C25 Ti1 C24 C23 112.7(6) . . . . ? Cl1 Ti1 C24 C23 20.7(5) . . . . ? C19 Ti1 C24 C23 -124.4(5) . . . . ? C22 Ti1 C24 C23 -73.7(4) . . . . ? C18 Ti1 C24 C23 -89.7(5) . . . . ? C26 Ti1 C24 C23 72.7(5) . . . . ? C21 Ti1 C24 C23 -102.0(4) . . . . ? C27 Ti1 C24 C23 34.2(4) . . . . ? C20 Ti1 C24 C23 -134.4(4) . . . . ? O6 Ti1 C24 C25 26.8(5) . . . . ? C23 Ti1 C24 C25 -112.7(6) . . . . ? Cl1 Ti1 C24 C25 -92.1(5) . . . . ? C19 Ti1 C24 C25 122.9(5) . . . . ? C22 Ti1 C24 C25 173.5(4) . . . . ? C18 Ti1 C24 C25 157.5(5) . . . . ? C26 Ti1 C24 C25 -40.0(4) . . . . ? C21 Ti1 C24 C25 145.2(4) . . . . ? C27 Ti1 C24 C25 -78.6(4) . . . . ? C20 Ti1 C24 C25 112.8(4) . . . . ? C23 C24 C25 C26 0.8(5) . . . . ? Ti1 C24 C25 C26 67.7(3) . . . . ? C23 C24 C25 Ti1 -66.9(4) . . . . ? O6 Ti1 C25 C26 94.8(4) . . . . ? C24 Ti1 C25 C26 -109.9(5) . . . . ? C23 Ti1 C25 C26 -72.1(4) . . . . ? Cl1 Ti1 C25 C26 4.6(5) . . . . ? C19 Ti1 C25 C26 -167.6(4) . . . . ? C22 Ti1 C25 C26 -120.2(5) . . . . ? C18 Ti1 C25 C26 -133.6(4) . . . . ? C21 Ti1 C25 C26 170.9(4) . . . . ? C27 Ti1 C25 C26 -34.9(4) . . . . ? C20 Ti1 C25 C26 163.8(3) . . . . ? O6 Ti1 C25 C24 -155.3(4) . . . . ? C23 Ti1 C25 C24 37.9(4) . . . . ? Cl1 Ti1 C25 C24 114.5(5) . . . . ? C19 Ti1 C25 C24 -57.7(4) . . . . ? C22 Ti1 C25 C24 -10.3(6) . . . . ? C18 Ti1 C25 C24 -23.7(5) . . . . ? C26 Ti1 C25 C24 109.9(5) . . . . ? C21 Ti1 C25 C24 -79.2(6) . . . . ? C27 Ti1 C25 C24 75.0(4) . . . . ? C20 Ti1 C25 C24 -86.3(4) . . . . ? C24 C25 C26 C27 0.3(6) . . . . ? Ti1 C25 C26 C27 66.7(4) . . . . ? C24 C25 C26 Ti1 -66.4(3) . . . . ? O6 Ti1 C26 C27 162.9(5) . . . . ? C24 Ti1 C26 C27 -74.9(5) . . . . ? C25 Ti1 C26 C27 -116.0(6) . . . . ? C23 Ti1 C26 C27 -33.4(4) . . . . ? Cl1 Ti1 C26 C27 67.8(4) . . . . ? C19 Ti1 C26 C27 -98.9(5) . . . . ? C22 Ti1 C26 C27 -4.3(7) . . . . ? C18 Ti1 C26 C27 -51.7(6) . . . . ? C21 Ti1 C26 C27 84.6(12) . . . . ? C20 Ti1 C26 C27 -148.8(5) . . . . ? O6 Ti1 C26 C25 -81.1(4) . . . . ? C24 Ti1 C26 C25 41.1(4) . . . . ? C23 Ti1 C26 C25 82.6(4) . . . . ? Cl1 Ti1 C26 C25 -176.2(4) . . . . ? C19 Ti1 C26 C25 17.1(6) . . . . ? C22 Ti1 C26 C25 111.7(6) . . . . ? C18 Ti1 C26 C25 64.2(6) . . . . ? C21 Ti1 C26 C25 -159.4(11) . . . . ? C27 Ti1 C26 C25 116.0(6) . . . . ? C20 Ti1 C26 C25 -32.8(6) . . . . ? C24 C23 C27 C26 2.0(7) . . . . ? Ti1 C23 C27 C26 -63.4(4) . . . . ? C24 C23 C27 Ti1 65.5(4) . . . . ? C25 C26 C27 C23 -1.5(7) . . . . ? Ti1 C26 C27 C23 63.1(5) . . . . ? C25 C26 C27 Ti1 -64.5(4) . . . . ? O6 Ti1 C27 C23 -139.0(4) . . . . ? C24 Ti1 C27 C23 -37.7(4) . . . . ? C25 Ti1 C27 C23 -81.6(5) . . . . ? Cl1 Ti1 C27 C23 131.7(5) . . . . ? C19 Ti1 C27 C23 -9.2(6) . . . . ? C22 Ti1 C27 C23 57.4(5) . . . . ? C18 Ti1 C27 C23 21.5(5) . . . . ? C26 Ti1 C27 C23 -120.0(6) . . . . ? C21 Ti1 C27 C23 79.5(6) . . . . ? C20 Ti1 C27 C23 4.0(11) . . . . ? O6 Ti1 C27 C26 -19.0(5) . . . . ? C24 Ti1 C27 C26 82.3(5) . . . . ? C25 Ti1 C27 C26 38.4(4) . . . . ? C23 Ti1 C27 C26 120.0(6) . . . . ? Cl1 Ti1 C27 C26 -108.3(5) . . . . ? C19 Ti1 C27 C26 110.8(5) . . . . ? C22 Ti1 C27 C26 177.4(4) . . . . ? C18 Ti1 C27 C26 141.5(4) . . . . ? C21 Ti1 C27 C26 -160.5(4) . . . . ? C20 Ti1 C27 C26 124.0(8) . . . . ? #END data_EvdW03_Complex_3b _database_code_depnum_ccdc_archive 'CCDC 810997' #TrackingRef '- Bezuidenhout_Barnard_vdWesthuizen_vdWatt_Liles_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Ethoxy-(\h^6^-tricarbonylchromium-benzo[b]thien-2-yl)-methylidene)- (pentacarbonyl)-tungsten ; _chemical_name_common ; (Ethoxy-(eta$6!-tricarbonylchromium-benzo(b)thien-2-yl)- methylidene)-(pentacarbonyl)-tungsten ; _chemical_melting_point ? _chemical_formula_moiety 'C19 H10 Cr O9 S W' _chemical_formula_sum 'C19 H10 Cr O9 S W' _chemical_formula_weight 650.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4597(6) _cell_length_b 10.8010(8) _cell_length_c 13.1159(10) _cell_angle_alpha 109.659(1) _cell_angle_beta 108.080(1) _cell_angle_gamma 95.910(1) _cell_volume 1043.68(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5050 _cell_measurement_theta_min 2.554 _cell_measurement_theta_max 26.605 _exptl_crystal_description plate _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 2.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 6.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.283 _exptl_absorpt_correction_T_max 0.610 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _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 'Bruker (Siemens) P4' _diffrn_measurement_method '\f and \w scans' _diffrn_detector 'SMART 1000 CCD' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 5686 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 26.61 _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _reflns_number_total 3784 _reflns_number_gt 3646 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement ;SHELXTL and SHELXL-97 (Sheldrick, 1997) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 1997), POV-Ray (Cason, 2004) ; _computing_publication_material SHELXL-97 _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^)+(0.0963P)^2^+0.4070P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3784 _refine_ls_number_parameters 290 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 3.985 _refine_diff_density_min -1.675 _refine_diff_density_rms 0.196 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.27358(2) 0.319696(17) 0.581758(16) 0.03549(13) Uani 1 1 d . . . Cr1 Cr 0.81077(12) 0.20809(9) 1.01478(8) 0.0395(2) Uani 1 1 d . A . C1 C 0.0438(9) 0.3659(7) 0.5549(7) 0.0489(15) Uani 1 1 d . . . O1 O -0.0865(8) 0.3932(7) 0.5417(7) 0.0824(19) Uani 1 1 d . . . C2 C 0.2859(10) 0.3754(7) 0.4473(7) 0.0501(16) Uani 1 1 d . . . O2 O 0.2888(9) 0.4064(7) 0.3754(6) 0.0708(17) Uani 1 1 d . . . C3 C 0.3840(10) 0.5157(7) 0.6929(6) 0.0496(16) Uani 1 1 d . . . O3 O 0.4427(11) 0.6259(6) 0.7541(7) 0.086(2) Uani 1 1 d . . . C4 C 0.2482(10) 0.2647(7) 0.7128(6) 0.0465(16) Uani 1 1 d . . . O4 O 0.2297(8) 0.2364(7) 0.7830(5) 0.0673(15) Uani 1 1 d . . . C5 C 0.1422(9) 0.1260(7) 0.4661(6) 0.0440(14) Uani 1 1 d . . . O5 O 0.0609(8) 0.0228(6) 0.4051(6) 0.0673(15) Uani 1 1 d . . . C6 C 0.5213(8) 0.2673(6) 0.6173(5) 0.0346(12) Uani 1 1 d . A . O6 O 0.5917(5) 0.2026(5) 0.5448(3) 0.0448(9) Uani 1 1 d . . . S1 S 0.8221(2) 0.21968(19) 0.74312(15) 0.0401(6) Uani 0.846(7) 1 d P A 1 S1A S 0.6115(10) 0.4069(9) 0.8572(6) 0.035(3) Uiso 0.154(7) 1 d PD A 2 C7 C 0.6442(7) 0.2956(5) 0.7345(4) 0.0342(10) Uani 1 1 d D . . C8 C 0.6451(9) 0.3660(8) 0.8417(6) 0.0386(14) Uani 0.846(7) 1 d P A 1 H8 H 0.5602 0.4112 0.8528 0.046 Uiso 0.846(7) 1 calc PR A 1 C8A C 0.786(3) 0.251(3) 0.7723(11) 0.031(8) Uiso 0.154(7) 1 d PD A 2 H8A H 0.8207 0.1938 0.7165 0.037 Uiso 0.154(7) 1 calc PR A 2 C9 C 0.7865(7) 0.3663(5) 0.9377(5) 0.0404(12) Uani 1 1 d D . . C10 C 0.8281(9) 0.4260(6) 1.0597(5) 0.0502(14) Uani 1 1 d . A . H10 H 0.7577 0.4755 1.0896 0.060 Uiso 1 1 calc R . . C11 C 0.9718(11) 0.4103(7) 1.1327(6) 0.0577(19) Uani 1 1 d . . . H11 H 1.0032 0.4546 1.2127 0.069 Uiso 1 1 calc R A . C12 C 1.0756(8) 0.3267(6) 1.0881(5) 0.0513(15) Uani 1 1 d . A . H12 H 1.1728 0.3160 1.1390 0.062 Uiso 1 1 calc R . . C13 C 1.0305(8) 0.2618(7) 0.9689(6) 0.0469(14) Uani 1 1 d . . . H13 H 1.0932 0.2033 0.9390 0.056 Uiso 1 1 calc R A . C14 C 0.8882(7) 0.2856(6) 0.8937(5) 0.0396(12) Uani 1 1 d D A . C15 C 0.5816(10) 0.1760(8) 0.9972(7) 0.0549(17) Uani 1 1 d . . . O15 O 0.4428(7) 0.1581(7) 0.9851(6) 0.0860(18) Uani 1 1 d . . . C16 C 0.8568(10) 0.1501(9) 1.1363(7) 0.067(2) Uani 1 1 d . . . O16 O 0.8873(12) 0.1157(10) 1.2110(7) 0.117(3) Uani 1 1 d . . . C17 C 0.7724(9) 0.0308(6) 0.9124(6) 0.0521(15) Uani 1 1 d . . . O17 O 0.7489(9) -0.0782(6) 0.8493(6) 0.0810(19) Uani 1 1 d . . . C18 C 0.5101(9) 0.1551(8) 0.4185(5) 0.0584(17) Uani 1 1 d . . . H18A H 0.5047 0.2312 0.3951 0.070 Uiso 1 1 calc R . . H18B H 0.3947 0.1025 0.3924 0.070 Uiso 1 1 calc R . . C19 C 0.6148(10) 0.0700(8) 0.3667(6) 0.0603(17) Uani 1 1 d . . . H19A H 0.7290 0.1227 0.3938 0.090 Uiso 1 1 calc R . . H19B H 0.5652 0.0380 0.2833 0.090 Uiso 1 1 calc R . . H19C H 0.6177 -0.0057 0.3894 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.03420(19) 0.03970(18) 0.03353(19) 0.01531(12) 0.01217(13) 0.00979(11) Cr1 0.0397(5) 0.0455(4) 0.0311(4) 0.0183(4) 0.0093(4) 0.0006(4) C1 0.042(4) 0.051(3) 0.060(4) 0.027(3) 0.020(3) 0.015(3) O1 0.055(3) 0.091(4) 0.133(6) 0.065(4) 0.045(4) 0.039(3) C2 0.058(4) 0.053(4) 0.047(4) 0.020(3) 0.026(3) 0.019(3) O2 0.091(4) 0.098(4) 0.063(3) 0.058(3) 0.042(3) 0.048(4) C3 0.061(4) 0.044(3) 0.045(4) 0.012(3) 0.025(3) 0.014(3) O3 0.099(6) 0.051(3) 0.088(5) 0.004(3) 0.038(4) -0.001(3) C4 0.047(4) 0.048(3) 0.040(3) 0.009(3) 0.020(3) 0.003(3) O4 0.062(3) 0.100(4) 0.056(3) 0.044(3) 0.030(3) 0.012(3) C5 0.042(3) 0.046(3) 0.040(3) 0.013(3) 0.014(3) 0.011(3) O5 0.068(4) 0.051(3) 0.064(3) 0.011(3) 0.017(3) 0.000(3) C17 0.051(4) 0.047(3) 0.053(4) 0.026(3) 0.009(3) 0.005(3) O17 0.091(5) 0.053(3) 0.084(4) 0.018(3) 0.024(4) 0.013(3) C15 0.052(4) 0.060(4) 0.053(4) 0.025(3) 0.020(3) 0.002(3) O15 0.048(3) 0.115(5) 0.098(5) 0.051(4) 0.025(3) 0.001(3) C16 0.055(4) 0.091(5) 0.056(4) 0.046(4) 0.010(3) -0.002(4) O16 0.118(7) 0.169(8) 0.084(5) 0.096(6) 0.022(5) 0.004(6) C6 0.034(3) 0.040(3) 0.030(3) 0.015(2) 0.011(2) 0.005(2) O6 0.041(2) 0.065(3) 0.030(2) 0.0182(18) 0.0147(18) 0.0187(19) S1 0.0373(9) 0.0542(10) 0.0299(9) 0.0161(7) 0.0131(7) 0.0139(7) C7 0.035(3) 0.036(2) 0.032(3) 0.014(2) 0.014(2) 0.005(2) C8 0.037(4) 0.037(3) 0.040(4) 0.017(3) 0.010(3) 0.008(3) C9 0.041(3) 0.039(3) 0.038(3) 0.015(2) 0.012(2) 0.001(2) C10 0.061(4) 0.045(3) 0.036(3) 0.010(2) 0.016(3) 0.006(3) C11 0.075(5) 0.050(3) 0.031(3) 0.010(3) 0.011(3) -0.009(3) C12 0.038(3) 0.061(3) 0.040(3) 0.028(3) -0.006(3) -0.009(3) C13 0.038(3) 0.058(3) 0.047(3) 0.026(3) 0.014(3) 0.005(3) C14 0.038(3) 0.046(3) 0.033(3) 0.017(2) 0.012(2) 0.000(2) C18 0.056(4) 0.087(5) 0.032(3) 0.018(3) 0.017(3) 0.030(3) C19 0.060(4) 0.074(4) 0.043(4) 0.014(3) 0.021(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C1 2.011(7) . ? W1 C3 2.037(7) . ? W1 C4 2.059(8) . ? W1 C5 2.062(7) . ? W1 C2 2.073(8) . ? W1 C6 2.179(6) . ? Cr1 C16 1.849(7) . ? Cr1 C17 1.857(7) . ? Cr1 C15 1.861(8) . ? Cr1 C11 2.196(7) . ? Cr1 C12 2.197(6) . ? Cr1 C10 2.202(6) . ? Cr1 C13 2.205(6) . ? Cr1 C14 2.254(5) . ? Cr1 C9 2.256(5) . ? C1 O1 1.146(9) . ? C2 O2 1.108(9) . ? C3 O3 1.138(10) . ? C4 O4 1.112(10) . ? C5 O5 1.121(9) . ? C17 O17 1.142(9) . ? C15 O15 1.121(9) . ? C16 O16 1.128(10) . ? C6 O6 1.317(8) . ? C6 C7 1.471(8) . ? O6 C18 1.459(7) . ? S1 C14 1.734(6) . ? S1 C7 1.778(5) . ? S1A C9 1.725(6) . ? S1A C7 1.776(5) . ? C7 C8 1.353(9) . ? C7 C8A 1.355(9) . ? C8 C9 1.441(9) . ? C8 H8 0.9300 . ? C8A C14 1.449(9) . ? C8A H8A 0.9300 . ? C9 C14 1.399(8) . ? C9 C10 1.417(8) . ? C10 C11 1.361(11) . ? C10 H10 0.9300 . ? C11 C12 1.434(11) . ? C11 H11 0.9300 . ? C12 C13 1.385(9) . ? C12 H12 0.9300 . ? C13 C14 1.410(9) . ? C13 H13 0.9300 . ? C18 C19 1.488(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 W1 C3 88.7(3) . . ? C1 W1 C4 89.1(3) . . ? C3 W1 C4 92.5(3) . . ? C1 W1 C5 86.4(3) . . ? C3 W1 C5 175.1(2) . . ? C4 W1 C5 87.9(3) . . ? C1 W1 C2 88.0(3) . . ? C3 W1 C2 88.0(3) . . ? C4 W1 C2 177.0(2) . . ? C5 W1 C2 91.4(3) . . ? C1 W1 C6 177.4(2) . . ? C3 W1 C6 91.3(3) . . ? C4 W1 C6 88.3(3) . . ? C5 W1 C6 93.6(3) . . ? C2 W1 C6 94.7(3) . . ? C16 Cr1 C17 89.1(4) . . ? C16 Cr1 C15 88.2(3) . . ? C17 Cr1 C15 88.8(3) . . ? C16 Cr1 C11 91.1(3) . . ? C17 Cr1 C11 153.6(3) . . ? C15 Cr1 C11 117.6(4) . . ? C16 Cr1 C12 90.2(3) . . ? C17 Cr1 C12 115.5(3) . . ? C15 Cr1 C12 155.6(3) . . ? C11 Cr1 C12 38.1(3) . . ? C16 Cr1 C10 116.9(3) . . ? C17 Cr1 C10 154.0(3) . . ? C15 Cr1 C10 92.0(3) . . ? C11 Cr1 C10 36.1(3) . . ? C12 Cr1 C10 67.2(3) . . ? C16 Cr1 C13 116.0(3) . . ? C17 Cr1 C13 89.0(3) . . ? C15 Cr1 C13 155.7(3) . . ? C11 Cr1 C13 67.3(3) . . ? C12 Cr1 C13 36.7(3) . . ? C10 Cr1 C13 79.7(3) . . ? C16 Cr1 C14 152.8(3) . . ? C17 Cr1 C14 90.8(3) . . ? C15 Cr1 C14 119.0(3) . . ? C11 Cr1 C14 77.3(2) . . ? C12 Cr1 C14 65.5(2) . . ? C10 Cr1 C14 66.2(2) . . ? C13 Cr1 C14 36.8(2) . . ? C16 Cr1 C9 153.9(3) . . ? C17 Cr1 C9 116.9(2) . . ? C15 Cr1 C9 93.2(3) . . ? C11 Cr1 C9 65.2(2) . . ? C12 Cr1 C9 77.9(2) . . ? C10 Cr1 C9 37.0(2) . . ? C13 Cr1 C9 66.4(2) . . ? C14 Cr1 C9 36.1(2) . . ? O1 C1 W1 178.8(7) . . ? O2 C2 W1 178.2(7) . . ? O3 C3 W1 178.6(8) . . ? O4 C4 W1 177.7(7) . . ? O5 C5 W1 175.0(6) . . ? O17 C17 Cr1 179.9(8) . . ? O15 C15 Cr1 178.5(7) . . ? O16 C16 Cr1 179.0(8) . . ? O6 C6 C7 105.5(5) . . ? O6 C6 W1 130.0(4) . . ? C7 C6 W1 124.4(4) . . ? C6 O6 C18 123.2(5) . . ? C14 S1 C7 89.9(3) . . ? C9 S1A C7 84.9(4) . . ? C8 C7 C8A 95.6(8) . . ? C8 C7 C6 131.8(5) . . ? C8A C7 C6 132.4(7) . . ? C8A C7 S1A 108.8(8) . . ? C6 C7 S1A 118.8(5) . . ? C8 C7 S1 111.2(5) . . ? C6 C7 S1 117.0(4) . . ? C7 C8 C9 115.5(7) . . ? C7 C8 H8 122.2 . . ? C9 C8 H8 122.2 . . ? C7 C8A C14 124.4(12) . . ? C7 C8A H8A 117.8 . . ? C14 C8A H8A 117.8 . . ? C14 C9 C10 119.6(6) . . ? C14 C9 C8 108.9(6) . . ? C10 C9 C8 131.4(6) . . ? C14 C9 S1A 126.2(5) . . ? C10 C9 S1A 114.2(5) . . ? C14 C9 Cr1 71.9(3) . . ? C10 C9 Cr1 69.4(3) . . ? C8 C9 Cr1 127.8(4) . . ? S1A C9 Cr1 132.3(5) . . ? C11 C10 C9 119.5(6) . . ? C11 C10 Cr1 71.7(4) . . ? C9 C10 Cr1 73.5(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? Cr1 C10 H10 126.3 . . ? C10 C11 C12 121.1(6) . . ? C10 C11 Cr1 72.2(4) . . ? C12 C11 Cr1 71.0(4) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? Cr1 C11 H11 129.9 . . ? C13 C12 C11 119.7(6) . . ? C13 C12 Cr1 71.9(4) . . ? C11 C12 Cr1 70.9(4) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? Cr1 C12 H12 129.3 . . ? C12 C13 C14 119.0(6) . . ? C12 C13 Cr1 71.4(4) . . ? C14 C13 Cr1 73.5(3) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? Cr1 C13 H13 126.5 . . ? C9 C14 C13 120.9(5) . . ? C9 C14 C8A 95.5(8) . . ? C13 C14 C8A 143.5(8) . . ? C9 C14 S1 114.4(5) . . ? C13 C14 S1 124.7(5) . . ? C9 C14 Cr1 72.0(3) . . ? C13 C14 Cr1 69.7(3) . . ? C8A C14 Cr1 125.5(14) . . ? S1 C14 Cr1 131.2(3) . . ? O6 C18 C19 107.4(5) . . ? O6 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? O6 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? 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 C3 W1 C6 O6 -129.4(6) . . . . ? C4 W1 C6 O6 138.1(6) . . . . ? C5 W1 C6 O6 50.4(6) . . . . ? C2 W1 C6 O6 -41.3(6) . . . . ? C3 W1 C6 C7 53.2(5) . . . . ? C4 W1 C6 C7 -39.3(5) . . . . ? C5 W1 C6 C7 -127.0(5) . . . . ? C2 W1 C6 C7 141.3(5) . . . . ? C7 C6 O6 C18 179.7(6) . . . . ? W1 C6 O6 C18 2.0(9) . . . . ? O6 C6 C7 C8 175.3(6) . . . . ? W1 C6 C7 C8 -6.7(9) . . . . ? O6 C6 C7 C8A -12(2) . . . . ? W1 C6 C7 C8A 166(2) . . . . ? O6 C6 C7 S1A 169.5(5) . . . . ? W1 C6 C7 S1A -12.6(7) . . . . ? O6 C6 C7 S1 -8.2(6) . . . . ? W1 C6 C7 S1 169.7(3) . . . . ? C9 S1A C7 C8 14.6(19) . . . . ? C9 S1A C7 C8A -3.3(16) . . . . ? C9 S1A C7 C6 175.9(5) . . . . ? C9 S1A C7 S1 -6.6(6) . . . . ? C14 S1 C7 C8 0.9(5) . . . . ? C14 S1 C7 C8A -5(5) . . . . ? C14 S1 C7 C6 -176.2(4) . . . . ? C14 S1 C7 S1A 6.2(5) . . . . ? C8A C7 C8 C9 2.4(16) . . . . ? C6 C7 C8 C9 177.3(5) . . . . ? S1A C7 C8 C9 -161(2) . . . . ? S1 C7 C8 C9 0.7(7) . . . . ? C8 C7 C8A C14 -2(3) . . . . ? C6 C7 C8A C14 -176.8(14) . . . . ? S1A C7 C8A C14 2(3) . . . . ? S1 C7 C8A C14 172(8) . . . . ? C7 C8 C9 C14 -2.4(8) . . . . ? C7 C8 C9 C10 -178.9(6) . . . . ? C7 C8 C9 S1A 164(2) . . . . ? C7 C8 C9 Cr1 -83.7(7) . . . . ? C7 S1A C9 C14 4.8(7) . . . . ? C7 S1A C9 C10 -177.1(5) . . . . ? C7 S1A C9 C8 -10.6(14) . . . . ? C7 S1A C9 Cr1 -93.5(5) . . . . ? C16 Cr1 C9 C14 129.3(7) . . . . ? C17 Cr1 C9 C14 -48.0(4) . . . . ? C15 Cr1 C9 C14 -138.3(4) . . . . ? C11 Cr1 C9 C14 102.7(4) . . . . ? C12 Cr1 C9 C14 64.7(4) . . . . ? C10 Cr1 C9 C14 132.7(5) . . . . ? C13 Cr1 C9 C14 28.0(4) . . . . ? C16 Cr1 C9 C10 -3.4(8) . . . . ? C17 Cr1 C9 C10 179.4(4) . . . . ? C15 Cr1 C9 C10 89.1(4) . . . . ? C11 Cr1 C9 C10 -29.9(4) . . . . ? C12 Cr1 C9 C10 -67.9(4) . . . . ? C13 Cr1 C9 C10 -104.6(4) . . . . ? C14 Cr1 C9 C10 -132.7(5) . . . . ? C16 Cr1 C9 C8 -130.5(8) . . . . ? C17 Cr1 C9 C8 52.3(7) . . . . ? C15 Cr1 C9 C8 -38.0(6) . . . . ? C11 Cr1 C9 C8 -157.0(7) . . . . ? C12 Cr1 C9 C8 165.0(6) . . . . ? C10 Cr1 C9 C8 -127.1(7) . . . . ? C13 Cr1 C9 C8 128.3(6) . . . . ? C14 Cr1 C9 C8 100.2(7) . . . . ? C16 Cr1 C9 S1A -108.0(8) . . . . ? C17 Cr1 C9 S1A 74.8(6) . . . . ? C15 Cr1 C9 S1A -15.5(5) . . . . ? C11 Cr1 C9 S1A -134.5(6) . . . . ? C12 Cr1 C9 S1A -172.5(5) . . . . ? C10 Cr1 C9 S1A -104.6(6) . . . . ? C13 Cr1 C9 S1A 150.8(6) . . . . ? C14 Cr1 C9 S1A 122.8(6) . . . . ? C14 C9 C10 C11 3.6(9) . . . . ? C8 C9 C10 C11 179.9(6) . . . . ? S1A C9 C10 C11 -174.7(6) . . . . ? Cr1 C9 C10 C11 57.1(5) . . . . ? C14 C9 C10 Cr1 -53.5(5) . . . . ? C8 C9 C10 Cr1 122.8(6) . . . . ? S1A C9 C10 Cr1 128.2(5) . . . . ? C16 Cr1 C10 C11 48.6(5) . . . . ? C17 Cr1 C10 C11 -131.0(7) . . . . ? C15 Cr1 C10 C11 137.6(5) . . . . ? C12 Cr1 C10 C11 -29.2(4) . . . . ? C13 Cr1 C10 C11 -65.4(4) . . . . ? C14 Cr1 C10 C11 -101.4(5) . . . . ? C9 Cr1 C10 C11 -129.7(6) . . . . ? C16 Cr1 C10 C9 178.3(4) . . . . ? C17 Cr1 C10 C9 -1.2(8) . . . . ? C15 Cr1 C10 C9 -92.7(4) . . . . ? C11 Cr1 C10 C9 129.7(6) . . . . ? C12 Cr1 C10 C9 100.5(4) . . . . ? C13 Cr1 C10 C9 64.3(4) . . . . ? C14 Cr1 C10 C9 28.3(3) . . . . ? C9 C10 C11 C12 -4.3(10) . . . . ? Cr1 C10 C11 C12 53.6(6) . . . . ? C9 C10 C11 Cr1 -58.0(5) . . . . ? C16 Cr1 C11 C10 -138.0(5) . . . . ? C17 Cr1 C11 C10 131.8(6) . . . . ? C15 Cr1 C11 C10 -49.4(5) . . . . ? C12 Cr1 C11 C10 133.1(6) . . . . ? C13 Cr1 C11 C10 104.2(4) . . . . ? C14 Cr1 C11 C10 66.8(4) . . . . ? C9 Cr1 C11 C10 30.7(4) . . . . ? C16 Cr1 C11 C12 88.8(4) . . . . ? C17 Cr1 C11 C12 -1.3(8) . . . . ? C15 Cr1 C11 C12 177.4(4) . . . . ? C10 Cr1 C11 C12 -133.1(6) . . . . ? C13 Cr1 C11 C12 -29.0(4) . . . . ? C14 Cr1 C11 C12 -66.3(4) . . . . ? C9 Cr1 C11 C12 -102.5(4) . . . . ? C10 C11 C12 C13 0.7(10) . . . . ? Cr1 C11 C12 C13 54.9(5) . . . . ? C10 C11 C12 Cr1 -54.2(6) . . . . ? C16 Cr1 C12 C13 136.8(5) . . . . ? C17 Cr1 C12 C13 47.7(5) . . . . ? C15 Cr1 C12 C13 -137.1(7) . . . . ? C11 Cr1 C12 C13 -131.6(6) . . . . ? C10 Cr1 C12 C13 -103.8(4) . . . . ? C14 Cr1 C12 C13 -30.7(4) . . . . ? C9 Cr1 C12 C13 -66.6(4) . . . . ? C16 Cr1 C12 C11 -91.6(5) . . . . ? C17 Cr1 C12 C11 179.3(4) . . . . ? C15 Cr1 C12 C11 -5.5(9) . . . . ? C10 Cr1 C12 C11 27.8(4) . . . . ? C13 Cr1 C12 C11 131.6(6) . . . . ? C14 Cr1 C12 C11 100.9(4) . . . . ? C9 Cr1 C12 C11 65.0(4) . . . . ? C11 C12 C13 C14 3.6(9) . . . . ? Cr1 C12 C13 C14 58.0(5) . . . . ? C11 C12 C13 Cr1 -54.4(5) . . . . ? C16 Cr1 C13 C12 -49.6(5) . . . . ? C17 Cr1 C13 C12 -138.1(4) . . . . ? C15 Cr1 C13 C12 137.0(7) . . . . ? C11 Cr1 C13 C12 30.0(4) . . . . ? C10 Cr1 C13 C12 65.5(4) . . . . ? C14 Cr1 C13 C12 129.3(6) . . . . ? C9 Cr1 C13 C12 101.8(4) . . . . ? C16 Cr1 C13 C14 -178.9(4) . . . . ? C17 Cr1 C13 C14 92.6(4) . . . . ? C15 Cr1 C13 C14 7.7(9) . . . . ? C11 Cr1 C13 C14 -99.3(4) . . . . ? C12 Cr1 C13 C14 -129.3(6) . . . . ? C10 Cr1 C13 C14 -63.8(4) . . . . ? C9 Cr1 C13 C14 -27.5(3) . . . . ? C10 C9 C14 C13 0.7(8) . . . . ? C8 C9 C14 C13 -176.3(5) . . . . ? S1A C9 C14 C13 178.7(6) . . . . ? Cr1 C9 C14 C13 -51.7(5) . . . . ? C10 C9 C14 C8A 177.9(14) . . . . ? C8 C9 C14 C8A 0.9(15) . . . . ? S1A C9 C14 C8A -4.0(16) . . . . ? Cr1 C9 C14 C8A 125.6(14) . . . . ? C10 C9 C14 S1 -179.9(4) . . . . ? C8 C9 C14 S1 3.1(6) . . . . ? S1A C9 C14 S1 -1.8(8) . . . . ? Cr1 C9 C14 S1 127.8(4) . . . . ? C10 C9 C14 Cr1 52.3(5) . . . . ? C8 C9 C14 Cr1 -124.7(5) . . . . ? S1A C9 C14 Cr1 -129.6(6) . . . . ? C12 C13 C14 C9 -4.3(9) . . . . ? Cr1 C13 C14 C9 52.7(5) . . . . ? C12 C13 C14 C8A -180(2) . . . . ? Cr1 C13 C14 C8A -123(2) . . . . ? C12 C13 C14 S1 176.4(4) . . . . ? Cr1 C13 C14 S1 -126.7(4) . . . . ? C12 C13 C14 Cr1 -57.0(5) . . . . ? C7 C8A C14 C9 1(3) . . . . ? C7 C8A C14 C13 176.7(11) . . . . ? C7 C8A C14 S1 -173(7) . . . . ? C7 C8A C14 Cr1 72(3) . . . . ? C7 S1 C14 C9 -2.4(4) . . . . ? C7 S1 C14 C13 177.0(5) . . . . ? C7 S1 C14 C8A 4(4) . . . . ? C7 S1 C14 Cr1 84.5(4) . . . . ? C16 Cr1 C14 C9 -131.9(7) . . . . ? C17 Cr1 C14 C9 138.5(4) . . . . ? C15 Cr1 C14 C9 49.5(5) . . . . ? C11 Cr1 C14 C9 -65.2(4) . . . . ? C12 Cr1 C14 C9 -103.6(4) . . . . ? C10 Cr1 C14 C9 -29.0(4) . . . . ? C13 Cr1 C14 C9 -134.1(5) . . . . ? C16 Cr1 C14 C13 2.2(9) . . . . ? C17 Cr1 C14 C13 -87.3(4) . . . . ? C15 Cr1 C14 C13 -176.4(4) . . . . ? C11 Cr1 C14 C13 68.9(4) . . . . ? C12 Cr1 C14 C13 30.5(4) . . . . ? C10 Cr1 C14 C13 105.2(4) . . . . ? C9 Cr1 C14 C13 134.1(5) . . . . ? C16 Cr1 C14 C8A 144.3(11) . . . . ? C17 Cr1 C14 C8A 54.8(10) . . . . ? C15 Cr1 C14 C8A -34.3(10) . . . . ? C11 Cr1 C14 C8A -149.0(10) . . . . ? C12 Cr1 C14 C8A 172.7(10) . . . . ? C10 Cr1 C14 C8A -112.7(10) . . . . ? C13 Cr1 C14 C8A 142.1(10) . . . . ? C9 Cr1 C14 C8A -83.7(10) . . . . ? C16 Cr1 C14 S1 121.0(7) . . . . ? C17 Cr1 C14 S1 31.5(5) . . . . ? C15 Cr1 C14 S1 -57.6(6) . . . . ? C11 Cr1 C14 S1 -172.3(5) . . . . ? C12 Cr1 C14 S1 149.3(5) . . . . ? C10 Cr1 C14 S1 -136.0(5) . . . . ? C13 Cr1 C14 S1 118.8(6) . . . . ? C9 Cr1 C14 S1 -107.1(6) . . . . ? C6 O6 C18 C19 -171.6(6) . . . . ? #END data_EvdW07_Complex_4b _database_code_depnum_ccdc_archive 'CCDC 810998' #TrackingRef '- Bezuidenhout_Barnard_vdWesthuizen_vdWatt_Liles_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ((Chloro-bis(\h^5^-pentadienyl)-titanium-oxy)-(\h^6^-tricarbonylchromium- benzo[b]thien-2-yl)-methylidene)-(pentacarbonyl)-tungsten dichloromethane solvate ; _chemical_name_common ; ((Chloro-bis(eta$5!-pentadienyl)-titanium-oxy)-(eta$6!- tricarbonylchromium-benzo(b)thien-2-yl)-methylidene)-(pentacarbonyl)- tungsten dichloromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C27 H15 Cl Cr O9 S Ti W, C H2 Cl2' _chemical_formula_sum 'C28 H17 Cl3 Cr O9 S Ti W' _chemical_formula_weight 919.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.2280(5) _cell_length_b 12.2398(5) _cell_length_c 23.9446(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.298(1) _cell_angle_gamma 90.00 _cell_volume 3226.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9031 _cell_measurement_theta_min 2.404 _cell_measurement_theta_max 26.503 _exptl_crystal_description plate _exptl_crystal_colour dark-purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 4.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 0.764 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _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 'Bruker (Siemens) P4' _diffrn_measurement_method '\f and \w scans' _diffrn_detector 'SMART 1000 CCD' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 17325 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.56 _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 6124 _reflns_number_gt 4947 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement ;SHELXTL and SHELXL-97 (Sheldrick, 1997) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 1997), POV-Ray (Cason, 2004) ; _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal structure contains a dichloromethane solvate. This molecule is disorderd and two main orientations of the dichloromethane were identified at the solvate site. The two orientations were refined as rigid bodies with a geometry for the Cl---C---Cl fragment (C---Cl = 1.723 \%A, Cl---C---Cl = 112.6 \% ) derived from mean values obtained from some 3900 structures containing a dicloromethane solvate, with R < 0.05 in the Cambridge Structural Database using Mogul. The hydrogen atoms were placed in calculated positions and constraned to ride on carbon atoms. The site occupation factors of the two orientations were refined, but constrained to sum to 1.0. ; _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^)+(0.0452P)^2^+4.0918P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6124 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.155 _refine_diff_density_min -1.003 _refine_diff_density_rms 0.089 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.355502(19) 0.522886(14) 0.381348(8) 0.05010(9) Uani 1 1 d . . . Cr1 Cr 0.02602(6) 0.21383(5) 0.52664(3) 0.04324(17) Uani 1 1 d . . . Ti1 Ti 0.44983(7) 0.16182(6) 0.33827(3) 0.04343(19) Uani 1 1 d . . . Cl1 Cl 0.53318(15) 0.28349(12) 0.27981(7) 0.0776(4) Uani 1 1 d . . . C1 C 0.3666(8) 0.6792(5) 0.3585(3) 0.094(2) Uani 1 1 d . . . O1 O 0.3762(8) 0.7706(4) 0.3489(3) 0.155(3) Uani 1 1 d . . . C2 C 0.5368(6) 0.5004(4) 0.3818(2) 0.0598(13) Uani 1 1 d . . . O2 O 0.6370(4) 0.4877(4) 0.3824(2) 0.0903(14) Uani 1 1 d . . . C3 C 0.3888(5) 0.5867(4) 0.4607(2) 0.0559(12) Uani 1 1 d . . . O3 O 0.4043(4) 0.6309(3) 0.50371(17) 0.0775(11) Uani 1 1 d . . . C4 C 0.1768(6) 0.5345(5) 0.3810(2) 0.0690(16) Uani 1 1 d . . . O4 O 0.0745(5) 0.5392(6) 0.3802(3) 0.122(2) Uani 1 1 d . . . C5 C 0.3109(5) 0.4786(4) 0.2980(2) 0.0589(13) Uani 1 1 d . . . O5 O 0.2812(5) 0.4591(4) 0.25088(18) 0.0889(13) Uani 1 1 d . . . C6 C 0.3520(4) 0.3514(3) 0.40942(18) 0.0391(9) Uani 1 1 d . . . O6 O 0.3958(3) 0.2743(2) 0.38340(13) 0.0447(7) Uani 1 1 d . . . S1 S 0.30048(11) 0.16913(9) 0.47149(5) 0.0505(3) Uani 1 1 d . . . C7 C 0.3001(4) 0.3113(3) 0.45694(18) 0.0403(9) Uani 1 1 d . . . C8 C 0.2463(4) 0.3693(4) 0.49372(18) 0.0435(10) Uani 1 1 d . . . H8 H 0.2371 0.4448 0.4919 0.052 Uiso 1 1 calc R . . C9 C 0.2050(4) 0.3025(3) 0.53566(19) 0.0435(10) Uani 1 1 d . . . C10 C 0.1439(4) 0.3336(4) 0.57992(19) 0.0485(10) Uani 1 1 d . . . H10 H 0.1257 0.4066 0.5850 0.058 Uiso 1 1 calc R . . C11 C 0.1113(4) 0.2535(4) 0.61572(19) 0.0542(12) Uani 1 1 d . . . H11 H 0.0769 0.2738 0.6465 0.065 Uiso 1 1 calc R . . C12 C 0.1305(4) 0.1417(4) 0.6054(2) 0.0553(12) Uani 1 1 d . . . H12 H 0.1058 0.0893 0.6289 0.066 Uiso 1 1 calc R . . C13 C 0.1855(4) 0.1087(4) 0.5611(2) 0.0503(11) Uani 1 1 d . . . H13 H 0.1953 0.0349 0.5538 0.060 Uiso 1 1 calc R . . C14 C 0.2262(4) 0.1896(3) 0.52713(19) 0.0437(10) Uani 1 1 d . . . C15 C -0.0657(4) 0.3292(4) 0.4928(2) 0.0570(12) Uani 1 1 d . . . O15 O -0.1234(4) 0.4000(3) 0.4714(2) 0.0899(13) Uani 1 1 d . . . C16 C -0.1130(5) 0.1537(5) 0.5433(2) 0.0630(13) Uani 1 1 d . . . O16 O -0.2007(4) 0.1166(4) 0.5527(2) 0.0974(15) Uani 1 1 d . . . C17 C -0.0050(4) 0.1459(4) 0.4575(2) 0.0555(12) Uani 1 1 d . . . O17 O -0.0211(4) 0.1052(4) 0.41300(19) 0.0891(13) Uani 1 1 d . . . C18 C 0.5824(5) 0.0108(4) 0.3580(3) 0.0678(15) Uani 1 1 d . . . H18 H 0.5704 -0.0498 0.3342 0.081 Uiso 1 1 calc R . . C19 C 0.5302(5) 0.0283(4) 0.4064(3) 0.0635(14) Uani 1 1 d . . . H19 H 0.4763 -0.0184 0.4195 0.076 Uiso 1 1 calc R . . C20 C 0.5728(4) 0.1266(4) 0.4308(2) 0.0593(13) Uani 1 1 d . . . H20 H 0.5547 0.1567 0.4638 0.071 Uiso 1 1 calc R . . C21 C 0.6478(4) 0.1727(4) 0.3972(2) 0.0628(13) Uani 1 1 d . . . H21 H 0.6866 0.2400 0.4032 0.075 Uiso 1 1 calc R . . C22 C 0.6546(5) 0.1000(5) 0.3525(3) 0.0654(14) Uani 1 1 d . . . H22 H 0.6998 0.1101 0.3242 0.079 Uiso 1 1 calc R . . C23 C 0.3469(9) 0.0218(8) 0.2828(6) 0.125(4) Uani 1 1 d . . . H23 H 0.3900 -0.0405 0.2766 0.150 Uiso 1 1 calc R . . C24 C 0.2897(9) 0.0368(8) 0.3246(5) 0.113(3) Uani 1 1 d . . . H24 H 0.2874 -0.0133 0.3536 0.135 Uiso 1 1 calc R . . C25 C 0.2374(6) 0.1300(9) 0.3200(4) 0.096(2) Uani 1 1 d . . . H25 H 0.1892 0.1568 0.3444 0.115 Uiso 1 1 calc R . . C26 C 0.2623(7) 0.1831(5) 0.2749(4) 0.099(3) Uani 1 1 d . . . H26 H 0.2372 0.2531 0.2630 0.119 Uiso 1 1 calc R . . C27 C 0.3327(9) 0.1137(13) 0.2495(3) 0.130(4) Uani 1 1 d . . . H27 H 0.3637 0.1265 0.2168 0.156 Uiso 1 1 calc R . . C28 C 0.8843(11) 0.3174(4) 0.2720(7) 0.114(5) Uani 0.551(6) 1 d PG A 1 H28A H 0.8010 0.3331 0.2539 0.137 Uiso 0.551(6) 1 calc PR A 1 H28B H 0.8932 0.3336 0.3123 0.137 Uiso 0.551(6) 1 calc PR A 1 Cl2 Cl 0.9801(5) 0.4010(4) 0.2432(3) 0.133(2) Uani 0.551(6) 1 d PG A 1 Cl3 Cl 0.9132(4) 0.1807(3) 0.2637(3) 0.149(3) Uani 0.551(6) 1 d PG A 1 C28A C 0.954(4) 0.3882(13) 0.2821(6) 0.30(3) Uani 0.449(6) 1 d PG A 2 H28C H 0.9002 0.4498 0.2824 0.359 Uiso 0.449(6) 1 calc PR A 2 H28D H 1.0371 0.4149 0.2930 0.359 Uiso 0.449(6) 1 calc PR A 2 Cl2A Cl 0.9332(15) 0.3353(19) 0.2142(4) 0.47(2) Uani 0.449(6) 1 d PG A 2 Cl3A Cl 0.9282(9) 0.2934(14) 0.3316(4) 0.283(8) Uani 0.449(6) 1 d PG A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.07272(15) 0.03237(11) 0.04888(13) 0.00311(7) 0.02095(10) 0.00343(8) Cr1 0.0444(4) 0.0383(3) 0.0495(4) 0.0036(3) 0.0154(3) 0.0010(3) Ti1 0.0540(5) 0.0339(4) 0.0448(4) -0.0033(3) 0.0157(4) 0.0054(3) Cl1 0.1029(11) 0.0672(8) 0.0751(9) 0.0155(7) 0.0478(8) 0.0064(8) C1 0.172(7) 0.045(3) 0.077(4) 0.010(3) 0.058(4) 0.011(4) O1 0.307(9) 0.042(2) 0.144(5) 0.028(3) 0.112(5) 0.015(4) C2 0.079(4) 0.055(3) 0.049(3) -0.002(2) 0.021(3) -0.018(3) O2 0.065(3) 0.125(4) 0.086(3) -0.008(3) 0.027(2) -0.024(3) C3 0.066(3) 0.041(2) 0.063(3) 0.000(2) 0.019(3) -0.006(2) O3 0.090(3) 0.074(3) 0.068(3) -0.023(2) 0.014(2) -0.012(2) C4 0.086(4) 0.075(4) 0.047(3) -0.004(3) 0.018(3) 0.026(3) O4 0.078(3) 0.183(6) 0.105(4) -0.013(4) 0.021(3) 0.048(4) C5 0.080(4) 0.046(3) 0.053(3) 0.006(2) 0.019(3) 0.010(2) O5 0.133(4) 0.084(3) 0.050(3) 0.004(2) 0.019(2) 0.007(3) C6 0.043(2) 0.0325(19) 0.043(2) -0.0013(17) 0.0132(18) -0.0009(17) O6 0.0537(17) 0.0331(14) 0.0520(18) -0.0042(13) 0.0218(14) 0.0029(13) S1 0.0595(7) 0.0348(5) 0.0642(8) 0.0039(5) 0.0291(6) 0.0063(5) C7 0.042(2) 0.0314(19) 0.050(2) -0.0008(17) 0.0151(19) -0.0002(16) C8 0.047(2) 0.040(2) 0.046(2) -0.0014(19) 0.0144(19) -0.0009(18) C9 0.042(2) 0.042(2) 0.049(3) -0.0014(19) 0.0145(19) 0.0009(18) C10 0.054(3) 0.045(2) 0.049(3) -0.005(2) 0.016(2) -0.001(2) C11 0.060(3) 0.065(3) 0.041(3) -0.003(2) 0.016(2) -0.001(2) C12 0.057(3) 0.055(3) 0.055(3) 0.018(2) 0.014(2) -0.001(2) C13 0.051(3) 0.043(2) 0.059(3) 0.013(2) 0.015(2) 0.008(2) C14 0.042(2) 0.041(2) 0.052(3) 0.0035(19) 0.0166(19) 0.0032(18) C15 0.052(3) 0.048(3) 0.071(3) -0.002(2) 0.010(2) 0.006(2) O15 0.089(3) 0.064(2) 0.110(4) 0.012(2) 0.003(3) 0.029(2) C16 0.055(3) 0.067(3) 0.069(3) 0.008(3) 0.017(3) -0.007(3) O16 0.065(3) 0.120(4) 0.113(4) 0.017(3) 0.033(2) -0.024(3) C17 0.054(3) 0.050(3) 0.062(3) 0.003(2) 0.010(2) -0.006(2) O17 0.110(3) 0.087(3) 0.071(3) -0.023(2) 0.017(2) -0.016(3) C18 0.068(3) 0.055(3) 0.079(4) -0.007(3) 0.010(3) 0.026(3) C19 0.060(3) 0.059(3) 0.071(4) 0.019(3) 0.009(3) 0.011(2) C20 0.055(3) 0.069(3) 0.053(3) -0.002(2) 0.008(2) 0.013(2) C21 0.050(3) 0.062(3) 0.074(4) -0.006(3) 0.007(3) 0.006(2) C22 0.054(3) 0.071(3) 0.076(4) 0.001(3) 0.025(3) 0.017(3) C23 0.097(6) 0.091(6) 0.163(10) -0.081(7) -0.034(7) 0.028(5) C24 0.101(6) 0.088(6) 0.125(8) 0.030(5) -0.036(6) -0.045(5) C25 0.063(4) 0.130(7) 0.091(5) -0.036(5) 0.008(4) -0.014(4) C26 0.102(5) 0.051(3) 0.113(6) 0.003(4) -0.054(5) -0.002(3) C27 0.119(7) 0.227(13) 0.043(4) -0.040(6) 0.016(4) -0.058(8) C28 0.081(9) 0.161(16) 0.110(12) 0.020(11) 0.043(9) 0.012(10) Cl2 0.120(4) 0.138(4) 0.141(5) 0.039(4) 0.022(4) 0.003(3) Cl3 0.120(4) 0.131(4) 0.187(6) 0.014(4) 0.006(3) -0.015(3) C28A 0.46(7) 0.059(13) 0.27(5) 0.00(2) -0.20(5) 0.01(2) Cl2A 0.307(19) 0.88(5) 0.219(13) -0.11(2) 0.061(12) 0.31(3) Cl3A 0.207(9) 0.47(2) 0.177(9) 0.119(12) 0.038(7) -0.026(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 W1 C1 2.000(6) . ? W1 C4 2.010(7) . ? W1 C3 2.020(5) . ? W1 C5 2.034(6) . ? W1 C2 2.053(7) . ? W1 C6 2.207(4) . ? Cr1 C17 1.825(6) . ? Cr1 C16 1.839(5) . ? Cr1 C15 1.839(5) . ? Cr1 C12 2.202(5) . ? Cr1 C10 2.206(5) . ? Cr1 C11 2.214(5) . ? Cr1 C13 2.228(4) . ? Cr1 C9 2.257(4) . ? Cr1 C14 2.265(4) . ? Ti1 O6 1.921(3) . ? Ti1 C23 2.331(7) . ? Ti1 C24 2.335(7) . ? Ti1 C27 2.345(7) . ? Ti1 C26 2.356(6) . ? Ti1 Cl1 2.3593(15) . ? Ti1 C19 2.360(5) . ? Ti1 C18 2.362(5) . ? Ti1 C25 2.372(6) . ? Ti1 C22 2.381(5) . ? Ti1 C21 2.391(5) . ? Ti1 C20 2.409(5) . ? C1 O1 1.151(7) . ? C2 O2 1.133(7) . ? C3 O3 1.146(6) . ? C4 O4 1.146(8) . ? C5 O5 1.137(7) . ? C6 O6 1.280(5) . ? C6 C7 1.461(6) . ? S1 C14 1.723(4) . ? S1 C7 1.775(4) . ? C7 C8 1.361(6) . ? C8 C9 1.440(6) . ? C8 H8 0.9300 . ? C9 C10 1.423(6) . ? C9 C14 1.424(6) . ? C10 C11 1.397(7) . ? C10 H10 0.9300 . ? C11 C12 1.414(7) . ? C11 H11 0.9300 . ? C12 C13 1.390(7) . ? C12 H12 0.9300 . ? C13 C14 1.413(6) . ? C13 H13 0.9300 . ? C15 O15 1.142(6) . ? C16 O16 1.146(6) . ? C17 O17 1.158(6) . ? C18 C22 1.381(8) . ? C18 C19 1.413(8) . ? C18 H18 0.9300 . ? C19 C20 1.383(7) . ? C19 H19 0.9300 . ? C20 C21 1.393(7) . ? C20 H20 0.9300 . ? C21 C22 1.405(7) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.303(14) . ? C23 C27 1.369(14) . ? C23 H23 0.9300 . ? C24 C25 1.278(12) . ? C24 H24 0.9300 . ? C25 C26 1.336(11) . ? C25 H25 0.9300 . ? C26 C27 1.380(13) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 Cl2 1.7230 . ? C28 Cl3 1.7232 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28A Cl2A 1.7230 . ? C28A Cl3A 1.7232 . ? C28A H28C 0.9700 . ? C28A H28D 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 W1 C4 92.7(3) . . ? C1 W1 C3 83.0(2) . . ? C4 W1 C3 88.7(2) . . ? C1 W1 C5 90.1(2) . . ? C4 W1 C5 87.8(2) . . ? C3 W1 C5 172.13(19) . . ? C1 W1 C2 90.8(3) . . ? C4 W1 C2 176.3(2) . . ? C3 W1 C2 92.7(2) . . ? C5 W1 C2 91.3(2) . . ? C1 W1 C6 177.2(3) . . ? C4 W1 C6 89.5(2) . . ? C3 W1 C6 95.30(17) . . ? C5 W1 C6 91.71(17) . . ? C2 W1 C6 87.01(18) . . ? C17 Cr1 C16 89.7(2) . . ? C17 Cr1 C15 87.6(2) . . ? C16 Cr1 C15 88.7(2) . . ? C17 Cr1 C12 124.8(2) . . ? C16 Cr1 C12 89.2(2) . . ? C15 Cr1 C12 147.5(2) . . ? C17 Cr1 C10 144.5(2) . . ? C16 Cr1 C10 125.4(2) . . ? C15 Cr1 C10 88.0(2) . . ? C12 Cr1 C10 67.19(18) . . ? C17 Cr1 C11 160.7(2) . . ? C16 Cr1 C11 96.0(2) . . ? C15 Cr1 C11 110.8(2) . . ? C12 Cr1 C11 37.3(2) . . ? C10 Cr1 C11 36.86(17) . . ? C17 Cr1 C13 94.0(2) . . ? C16 Cr1 C13 110.1(2) . . ? C15 Cr1 C13 161.1(2) . . ? C12 Cr1 C13 36.56(17) . . ? C10 Cr1 C13 79.78(18) . . ? C11 Cr1 C13 66.78(19) . . ? C17 Cr1 C9 108.30(19) . . ? C16 Cr1 C9 161.7(2) . . ? C15 Cr1 C9 94.82(19) . . ? C12 Cr1 C9 78.22(17) . . ? C10 Cr1 C9 37.16(16) . . ? C11 Cr1 C9 66.01(17) . . ? C13 Cr1 C9 66.82(16) . . ? C17 Cr1 C14 87.59(19) . . ? C16 Cr1 C14 146.1(2) . . ? C15 Cr1 C14 124.87(19) . . ? C12 Cr1 C14 65.26(17) . . ? C10 Cr1 C14 66.53(16) . . ? C11 Cr1 C14 77.42(17) . . ? C13 Cr1 C14 36.65(16) . . ? C9 Cr1 C14 36.70(15) . . ? O6 Ti1 C23 132.2(3) . . ? O6 Ti1 C24 103.3(4) . . ? C23 Ti1 C24 32.4(4) . . ? O6 Ti1 C27 120.5(4) . . ? C23 Ti1 C27 34.0(4) . . ? C24 Ti1 C27 55.1(3) . . ? O6 Ti1 C26 86.7(2) . . ? C23 Ti1 C26 55.5(3) . . ? C24 Ti1 C26 54.2(3) . . ? C27 Ti1 C26 34.1(3) . . ? O6 Ti1 Cl1 94.99(10) . . ? C23 Ti1 Cl1 109.6(4) . . ? C24 Ti1 Cl1 135.6(3) . . ? C27 Ti1 Cl1 80.7(3) . . ? C26 Ti1 Cl1 87.5(2) . . ? O6 Ti1 C19 103.18(18) . . ? C23 Ti1 C19 88.0(4) . . ? C24 Ti1 C19 79.8(3) . . ? C27 Ti1 C19 121.5(4) . . ? C26 Ti1 C19 133.9(2) . . ? Cl1 Ti1 C19 134.82(15) . . ? O6 Ti1 C18 134.79(18) . . ? C23 Ti1 C18 76.2(3) . . ? C24 Ti1 C18 87.3(3) . . ? C27 Ti1 C18 101.8(4) . . ? C26 Ti1 C18 131.6(2) . . ? Cl1 Ti1 C18 107.75(17) . . ? C19 Ti1 C18 34.8(2) . . ? O6 Ti1 C25 78.7(2) . . ? C23 Ti1 C25 53.6(3) . . ? C24 Ti1 C25 31.5(3) . . ? C27 Ti1 C25 55.0(3) . . ? C26 Ti1 C25 32.8(3) . . ? Cl1 Ti1 C25 119.7(3) . . ? C19 Ti1 C25 104.4(3) . . ? C18 Ti1 C25 118.7(3) . . ? O6 Ti1 C22 123.36(17) . . ? C23 Ti1 C22 101.8(3) . . ? C24 Ti1 C22 120.5(3) . . ? C27 Ti1 C22 113.8(3) . . ? C26 Ti1 C22 147.5(3) . . ? Cl1 Ti1 C22 78.54(15) . . ? C19 Ti1 C22 56.9(2) . . ? C18 Ti1 C22 33.9(2) . . ? C25 Ti1 C22 151.9(3) . . ? O6 Ti1 C21 89.30(16) . . ? C23 Ti1 C21 132.6(2) . . ? C24 Ti1 C21 136.1(3) . . ? C27 Ti1 C21 147.1(3) . . ? C26 Ti1 C21 169.7(2) . . ? Cl1 Ti1 C21 83.34(15) . . ? C19 Ti1 C21 56.3(2) . . ? C18 Ti1 C21 56.6(2) . . ? C25 Ti1 C21 154.5(3) . . ? C22 Ti1 C21 34.23(18) . . ? O6 Ti1 C20 78.35(15) . . ? C23 Ti1 C20 121.6(4) . . ? C24 Ti1 C20 107.4(3) . . ? C27 Ti1 C20 155.2(4) . . ? C26 Ti1 C20 153.0(3) . . ? Cl1 Ti1 C20 115.85(14) . . ? C19 Ti1 C20 33.69(18) . . ? C18 Ti1 C20 56.7(2) . . ? C25 Ti1 C20 121.0(3) . . ? C22 Ti1 C20 56.49(19) . . ? C21 Ti1 C20 33.73(18) . . ? O1 C1 W1 175.6(7) . . ? O2 C2 W1 179.5(5) . . ? O3 C3 W1 174.4(4) . . ? O4 C4 W1 178.7(6) . . ? O5 C5 W1 175.8(5) . . ? O6 C6 C7 112.5(3) . . ? O6 C6 W1 121.4(3) . . ? C7 C6 W1 126.1(3) . . ? C6 O6 Ti1 174.6(3) . . ? C14 S1 C7 91.5(2) . . ? C8 C7 C6 128.7(4) . . ? C8 C7 S1 111.6(3) . . ? C6 C7 S1 119.7(3) . . ? C7 C8 C9 113.6(4) . . ? C7 C8 H8 123.2 . . ? C9 C8 H8 123.2 . . ? C10 C9 C14 119.0(4) . . ? C10 C9 C8 129.5(4) . . ? C14 C9 C8 111.4(4) . . ? C10 C9 Cr1 69.5(2) . . ? C14 C9 Cr1 72.0(2) . . ? C8 C9 Cr1 127.5(3) . . ? C11 C10 C9 119.4(4) . . ? C11 C10 Cr1 71.9(3) . . ? C9 C10 Cr1 73.4(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? Cr1 C10 H10 126.3 . . ? C10 C11 C12 120.3(4) . . ? C10 C11 Cr1 71.3(3) . . ? C12 C11 Cr1 70.9(3) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? Cr1 C11 H11 130.7 . . ? C13 C12 C11 121.4(4) . . ? C13 C12 Cr1 72.7(3) . . ? C11 C12 Cr1 71.8(3) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? Cr1 C12 H12 128.5 . . ? C12 C13 C14 118.5(4) . . ? C12 C13 Cr1 70.7(3) . . ? C14 C13 Cr1 73.1(2) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? Cr1 C13 H13 127.4 . . ? C13 C14 C9 121.1(4) . . ? C13 C14 S1 127.1(3) . . ? C9 C14 S1 111.9(3) . . ? C13 C14 Cr1 70.2(2) . . ? C9 C14 Cr1 71.3(2) . . ? S1 C14 Cr1 130.2(2) . . ? O15 C15 Cr1 179.2(5) . . ? O16 C16 Cr1 178.8(5) . . ? O17 C17 Cr1 177.4(5) . . ? C22 C18 C19 107.7(5) . . ? C22 C18 Ti1 73.8(3) . . ? C19 C18 Ti1 72.5(3) . . ? C22 C18 H18 126.1 . . ? C19 C18 H18 126.1 . . ? Ti1 C18 H18 119.4 . . ? C20 C19 C18 108.2(5) . . ? C20 C19 Ti1 75.1(3) . . ? C18 C19 Ti1 72.7(3) . . ? C20 C19 H19 125.9 . . ? C18 C19 H19 125.9 . . ? Ti1 C19 H19 118.3 . . ? C19 C20 C21 107.8(5) . . ? C19 C20 Ti1 71.2(3) . . ? C21 C20 Ti1 72.5(3) . . ? C19 C20 H20 126.1 . . ? C21 C20 H20 126.1 . . ? Ti1 C20 H20 122.0 . . ? C20 C21 C22 108.3(5) . . ? C20 C21 Ti1 73.8(3) . . ? C22 C21 Ti1 72.5(3) . . ? C20 C21 H21 125.9 . . ? C22 C21 H21 125.9 . . ? Ti1 C21 H21 119.7 . . ? C18 C22 C21 107.9(5) . . ? C18 C22 Ti1 72.3(3) . . ? C21 C22 Ti1 73.3(3) . . ? C18 C22 H22 126.1 . . ? C21 C22 H22 126.1 . . ? Ti1 C22 H22 120.1 . . ? C24 C23 C27 108.2(8) . . ? C24 C23 Ti1 73.9(4) . . ? C27 C23 Ti1 73.5(5) . . ? C24 C23 H23 125.9 . . ? C27 C23 H23 125.9 . . ? Ti1 C23 H23 118.5 . . ? C25 C24 C23 110.3(9) . . ? C25 C24 Ti1 75.9(4) . . ? C23 C24 Ti1 73.6(5) . . ? C25 C24 H24 124.8 . . ? C23 C24 H24 124.8 . . ? Ti1 C24 H24 117.4 . . ? C24 C25 C26 109.7(8) . . ? C24 C25 Ti1 72.6(4) . . ? C26 C25 Ti1 72.9(4) . . ? C24 C25 H25 125.1 . . ? C26 C25 H25 125.1 . . ? Ti1 C25 H25 120.9 . . ? C25 C26 C27 106.6(7) . . ? C25 C26 Ti1 74.2(4) . . ? C27 C26 Ti1 72.5(4) . . ? C25 C26 H26 126.7 . . ? C27 C26 H26 126.7 . . ? Ti1 C26 H26 118.6 . . ? C23 C27 C26 105.1(8) . . ? C23 C27 Ti1 72.4(4) . . ? C26 C27 Ti1 73.4(4) . . ? C23 C27 H27 127.5 . . ? C26 C27 H27 127.5 . . ? Ti1 C27 H27 118.9 . . ? Cl2 C28 Cl3 112.6 . . ? Cl2 C28 H28A 109.1 . . ? Cl3 C28 H28A 109.1 . . ? Cl2 C28 H28B 109.1 . . ? Cl3 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? Cl2A C28A Cl3A 112.6 . . ? Cl2A C28A H28C 109.1 . . ? Cl3A C28A H28C 109.1 . . ? Cl2A C28A H28D 109.1 . . ? Cl3A C28A H28D 109.1 . . ? H28C C28A H28D 107.8 . . ? 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 C4 W1 C6 O6 128.6(4) . . . . ? C3 W1 C6 O6 -142.7(3) . . . . ? C5 W1 C6 O6 40.9(4) . . . . ? C2 W1 C6 O6 -50.3(4) . . . . ? C4 W1 C6 C7 -50.1(4) . . . . ? C3 W1 C6 C7 38.5(4) . . . . ? C5 W1 C6 C7 -137.9(4) . . . . ? C2 W1 C6 C7 130.9(4) . . . . ? O6 C6 C7 C8 179.9(4) . . . . ? W1 C6 C7 C8 -1.3(7) . . . . ? O6 C6 C7 S1 -1.3(5) . . . . ? W1 C6 C7 S1 177.6(2) . . . . ? C14 S1 C7 C8 0.5(4) . . . . ? C14 S1 C7 C6 -178.5(4) . . . . ? C6 C7 C8 C9 179.9(4) . . . . ? S1 C7 C8 C9 1.0(5) . . . . ? C7 C8 C9 C10 -179.0(4) . . . . ? C7 C8 C9 C14 -2.4(5) . . . . ? C7 C8 C9 Cr1 -85.6(5) . . . . ? C17 Cr1 C9 C10 169.4(3) . . . . ? C16 Cr1 C9 C10 -20.3(8) . . . . ? C15 Cr1 C9 C10 80.3(3) . . . . ? C12 Cr1 C9 C10 -67.6(3) . . . . ? C11 Cr1 C9 C10 -30.4(3) . . . . ? C13 Cr1 C9 C10 -104.2(3) . . . . ? C14 Cr1 C9 C10 -131.8(4) . . . . ? C17 Cr1 C9 C14 -58.8(3) . . . . ? C16 Cr1 C9 C14 111.6(7) . . . . ? C15 Cr1 C9 C14 -147.9(3) . . . . ? C12 Cr1 C9 C14 64.2(3) . . . . ? C10 Cr1 C9 C14 131.8(4) . . . . ? C11 Cr1 C9 C14 101.4(3) . . . . ? C13 Cr1 C9 C14 27.6(3) . . . . ? C17 Cr1 C9 C8 44.7(4) . . . . ? C16 Cr1 C9 C8 -144.9(6) . . . . ? C15 Cr1 C9 C8 -44.4(4) . . . . ? C12 Cr1 C9 C8 167.7(4) . . . . ? C10 Cr1 C9 C8 -124.6(5) . . . . ? C11 Cr1 C9 C8 -155.0(4) . . . . ? C13 Cr1 C9 C8 131.2(4) . . . . ? C14 Cr1 C9 C8 103.6(5) . . . . ? C14 C9 C10 C11 3.1(7) . . . . ? C8 C9 C10 C11 179.5(4) . . . . ? Cr1 C9 C10 C11 57.2(4) . . . . ? C14 C9 C10 Cr1 -54.1(4) . . . . ? C8 C9 C10 Cr1 122.2(5) . . . . ? C17 Cr1 C10 C11 -147.2(4) . . . . ? C16 Cr1 C10 C11 42.8(4) . . . . ? C15 Cr1 C10 C11 129.7(3) . . . . ? C12 Cr1 C10 C11 -28.8(3) . . . . ? C13 Cr1 C10 C11 -64.7(3) . . . . ? C9 Cr1 C10 C11 -129.6(4) . . . . ? C14 Cr1 C10 C11 -100.6(3) . . . . ? C17 Cr1 C10 C9 -17.6(5) . . . . ? C16 Cr1 C10 C9 172.4(3) . . . . ? C15 Cr1 C10 C9 -100.7(3) . . . . ? C12 Cr1 C10 C9 100.8(3) . . . . ? C11 Cr1 C10 C9 129.6(4) . . . . ? C13 Cr1 C10 C9 64.9(3) . . . . ? C14 Cr1 C10 C9 29.0(3) . . . . ? C9 C10 C11 C12 -4.8(7) . . . . ? Cr1 C10 C11 C12 53.1(4) . . . . ? C9 C10 C11 Cr1 -58.0(4) . . . . ? C17 Cr1 C11 C10 107.2(6) . . . . ? C16 Cr1 C11 C10 -146.2(3) . . . . ? C15 Cr1 C11 C10 -55.3(3) . . . . ? C12 Cr1 C11 C10 133.0(4) . . . . ? C13 Cr1 C11 C10 104.5(3) . . . . ? C9 Cr1 C11 C10 30.6(3) . . . . ? C14 Cr1 C11 C10 67.5(3) . . . . ? C17 Cr1 C11 C12 -25.8(7) . . . . ? C16 Cr1 C11 C12 80.8(3) . . . . ? C15 Cr1 C11 C12 171.7(3) . . . . ? C10 Cr1 C11 C12 -133.0(4) . . . . ? C13 Cr1 C11 C12 -28.5(3) . . . . ? C9 Cr1 C11 C12 -102.4(3) . . . . ? C14 Cr1 C11 C12 -65.5(3) . . . . ? C10 C11 C12 C13 2.2(8) . . . . ? Cr1 C11 C12 C13 55.5(4) . . . . ? C10 C11 C12 Cr1 -53.3(4) . . . . ? C17 Cr1 C12 C13 37.4(4) . . . . ? C16 Cr1 C12 C13 126.5(3) . . . . ? C15 Cr1 C12 C13 -147.1(4) . . . . ? C10 Cr1 C12 C13 -104.1(3) . . . . ? C11 Cr1 C12 C13 -132.5(4) . . . . ? C9 Cr1 C12 C13 -66.8(3) . . . . ? C14 Cr1 C12 C13 -30.5(3) . . . . ? C17 Cr1 C12 C11 169.9(3) . . . . ? C16 Cr1 C12 C11 -101.0(3) . . . . ? C15 Cr1 C12 C11 -14.6(5) . . . . ? C10 Cr1 C12 C11 28.4(3) . . . . ? C13 Cr1 C12 C11 132.5(4) . . . . ? C9 Cr1 C12 C11 65.7(3) . . . . ? C14 Cr1 C12 C11 102.0(3) . . . . ? C11 C12 C13 C14 2.2(7) . . . . ? Cr1 C12 C13 C14 57.2(4) . . . . ? C11 C12 C13 Cr1 -55.1(4) . . . . ? C17 Cr1 C13 C12 -150.0(3) . . . . ? C16 Cr1 C13 C12 -58.8(4) . . . . ? C15 Cr1 C13 C12 115.7(7) . . . . ? C10 Cr1 C13 C12 65.3(3) . . . . ? C11 Cr1 C13 C12 29.1(3) . . . . ? C9 Cr1 C13 C12 101.8(3) . . . . ? C14 Cr1 C13 C12 129.5(4) . . . . ? C17 Cr1 C13 C14 80.6(3) . . . . ? C16 Cr1 C13 C14 171.7(3) . . . . ? C15 Cr1 C13 C14 -13.8(8) . . . . ? C12 Cr1 C13 C14 -129.5(4) . . . . ? C10 Cr1 C13 C14 -64.2(3) . . . . ? C11 Cr1 C13 C14 -100.3(3) . . . . ? C9 Cr1 C13 C14 -27.7(3) . . . . ? C12 C13 C14 C9 -3.9(7) . . . . ? Cr1 C13 C14 C9 52.2(4) . . . . ? C12 C13 C14 S1 178.0(4) . . . . ? Cr1 C13 C14 S1 -126.0(4) . . . . ? C12 C13 C14 Cr1 -56.0(4) . . . . ? C10 C9 C14 C13 1.3(7) . . . . ? C8 C9 C14 C13 -175.7(4) . . . . ? Cr1 C9 C14 C13 -51.7(4) . . . . ? C10 C9 C14 S1 179.7(3) . . . . ? C8 C9 C14 S1 2.7(5) . . . . ? Cr1 C9 C14 S1 126.7(3) . . . . ? C10 C9 C14 Cr1 53.0(4) . . . . ? C8 C9 C14 Cr1 -124.0(4) . . . . ? C7 S1 C14 C13 176.5(4) . . . . ? C7 S1 C14 C9 -1.8(4) . . . . ? C7 S1 C14 Cr1 81.7(3) . . . . ? C17 Cr1 C14 C13 -100.0(3) . . . . ? C16 Cr1 C14 C13 -14.1(5) . . . . ? C15 Cr1 C14 C13 174.6(3) . . . . ? C12 Cr1 C14 C13 30.4(3) . . . . ? C10 Cr1 C14 C13 105.0(3) . . . . ? C11 Cr1 C14 C13 67.9(3) . . . . ? C9 Cr1 C14 C13 134.4(4) . . . . ? C17 Cr1 C14 C9 125.6(3) . . . . ? C16 Cr1 C14 C9 -148.5(4) . . . . ? C15 Cr1 C14 C9 40.2(4) . . . . ? C12 Cr1 C14 C9 -104.0(3) . . . . ? C10 Cr1 C14 C9 -29.4(3) . . . . ? C11 Cr1 C14 C9 -66.6(3) . . . . ? C13 Cr1 C14 C9 -134.4(4) . . . . ? C17 Cr1 C14 S1 22.4(3) . . . . ? C16 Cr1 C14 S1 108.3(4) . . . . ? C15 Cr1 C14 S1 -63.0(4) . . . . ? C12 Cr1 C14 S1 152.8(4) . . . . ? C10 Cr1 C14 S1 -132.6(3) . . . . ? C11 Cr1 C14 S1 -169.8(3) . . . . ? C13 Cr1 C14 S1 122.3(4) . . . . ? C9 Cr1 C14 S1 -103.2(4) . . . . ? O6 Ti1 C18 C22 -84.9(4) . . . . ? C23 Ti1 C18 C22 138.1(6) . . . . ? C24 Ti1 C18 C22 169.0(5) . . . . ? C27 Ti1 C18 C22 115.5(4) . . . . ? C26 Ti1 C18 C22 134.5(5) . . . . ? Cl1 Ti1 C18 C22 31.6(4) . . . . ? C19 Ti1 C18 C22 -115.1(5) . . . . ? C25 Ti1 C18 C22 171.9(4) . . . . ? C21 Ti1 C18 C22 -37.4(3) . . . . ? C20 Ti1 C18 C22 -78.1(4) . . . . ? O6 Ti1 C18 C19 30.2(5) . . . . ? C23 Ti1 C18 C19 -106.8(6) . . . . ? C24 Ti1 C18 C19 -75.9(5) . . . . ? C27 Ti1 C18 C19 -129.4(4) . . . . ? C26 Ti1 C18 C19 -110.4(5) . . . . ? Cl1 Ti1 C18 C19 146.7(3) . . . . ? C25 Ti1 C18 C19 -73.1(4) . . . . ? C22 Ti1 C18 C19 115.1(5) . . . . ? C21 Ti1 C18 C19 77.7(4) . . . . ? C20 Ti1 C18 C19 37.0(3) . . . . ? C22 C18 C19 C20 -1.3(6) . . . . ? Ti1 C18 C19 C20 -67.3(4) . . . . ? C22 C18 C19 Ti1 65.9(4) . . . . ? O6 Ti1 C19 C20 -43.5(3) . . . . ? C23 Ti1 C19 C20 -176.5(5) . . . . ? C24 Ti1 C19 C20 -144.9(5) . . . . ? C27 Ti1 C19 C20 177.5(4) . . . . ? C26 Ti1 C19 C20 -141.8(4) . . . . ? Cl1 Ti1 C19 C20 67.5(4) . . . . ? C18 Ti1 C19 C20 115.0(5) . . . . ? C25 Ti1 C19 C20 -125.0(4) . . . . ? C22 Ti1 C19 C20 77.9(4) . . . . ? C21 Ti1 C19 C20 36.6(3) . . . . ? O6 Ti1 C19 C18 -158.5(3) . . . . ? C23 Ti1 C19 C18 68.5(5) . . . . ? C24 Ti1 C19 C18 100.1(5) . . . . ? C27 Ti1 C19 C18 62.5(5) . . . . ? C26 Ti1 C19 C18 103.3(5) . . . . ? Cl1 Ti1 C19 C18 -47.5(4) . . . . ? C25 Ti1 C19 C18 120.0(4) . . . . ? C22 Ti1 C19 C18 -37.1(3) . . . . ? C21 Ti1 C19 C18 -78.3(4) . . . . ? C20 Ti1 C19 C18 -115.0(5) . . . . ? C18 C19 C20 C21 2.0(6) . . . . ? Ti1 C19 C20 C21 -63.6(4) . . . . ? C18 C19 C20 Ti1 65.7(4) . . . . ? O6 Ti1 C20 C19 136.8(3) . . . . ? C23 Ti1 C20 C19 4.1(5) . . . . ? C24 Ti1 C20 C19 36.4(5) . . . . ? C27 Ti1 C20 C19 -5.1(8) . . . . ? C26 Ti1 C20 C19 79.1(6) . . . . ? Cl1 Ti1 C20 C19 -133.3(3) . . . . ? C18 Ti1 C20 C19 -38.3(3) . . . . ? C25 Ti1 C20 C19 67.7(4) . . . . ? C22 Ti1 C20 C19 -79.1(4) . . . . ? C21 Ti1 C20 C19 -116.5(5) . . . . ? O6 Ti1 C20 C21 -106.7(3) . . . . ? C23 Ti1 C20 C21 120.6(5) . . . . ? C24 Ti1 C20 C21 152.9(5) . . . . ? C27 Ti1 C20 C21 111.4(7) . . . . ? C26 Ti1 C20 C21 -164.3(4) . . . . ? Cl1 Ti1 C20 C21 -16.7(3) . . . . ? C19 Ti1 C20 C21 116.5(5) . . . . ? C18 Ti1 C20 C21 78.3(3) . . . . ? C25 Ti1 C20 C21 -175.7(4) . . . . ? C22 Ti1 C20 C21 37.4(3) . . . . ? C19 C20 C21 C22 -2.0(6) . . . . ? Ti1 C20 C21 C22 -64.8(4) . . . . ? C19 C20 C21 Ti1 62.8(4) . . . . ? O6 Ti1 C21 C20 69.8(3) . . . . ? C23 Ti1 C21 C20 -84.5(7) . . . . ? C24 Ti1 C21 C20 -38.8(6) . . . . ? C27 Ti1 C21 C20 -133.9(7) . . . . ? C26 Ti1 C21 C20 137.0(17) . . . . ? Cl1 Ti1 C21 C20 164.9(3) . . . . ? C19 Ti1 C21 C20 -36.6(3) . . . . ? C18 Ti1 C21 C20 -78.7(4) . . . . ? C25 Ti1 C21 C20 8.5(8) . . . . ? C22 Ti1 C21 C20 -115.7(5) . . . . ? O6 Ti1 C21 C22 -174.5(3) . . . . ? C23 Ti1 C21 C22 31.2(7) . . . . ? C24 Ti1 C21 C22 76.9(6) . . . . ? C27 Ti1 C21 C22 -18.2(8) . . . . ? C26 Ti1 C21 C22 -107.3(17) . . . . ? Cl1 Ti1 C21 C22 -79.4(3) . . . . ? C19 Ti1 C21 C22 79.1(4) . . . . ? C18 Ti1 C21 C22 37.0(3) . . . . ? C25 Ti1 C21 C22 124.2(7) . . . . ? C20 Ti1 C21 C22 115.7(5) . . . . ? C19 C18 C22 C21 0.1(6) . . . . ? Ti1 C18 C22 C21 65.2(4) . . . . ? C19 C18 C22 Ti1 -65.1(4) . . . . ? C20 C21 C22 C18 1.1(6) . . . . ? Ti1 C21 C22 C18 -64.5(4) . . . . ? C20 C21 C22 Ti1 65.7(4) . . . . ? O6 Ti1 C22 C18 122.2(4) . . . . ? C23 Ti1 C22 C18 -41.5(6) . . . . ? C24 Ti1 C22 C18 -12.8(5) . . . . ? C27 Ti1 C22 C18 -75.1(5) . . . . ? C26 Ti1 C22 C18 -83.0(6) . . . . ? Cl1 Ti1 C22 C18 -149.4(4) . . . . ? C19 Ti1 C22 C18 38.2(4) . . . . ? C25 Ti1 C22 C18 -15.3(7) . . . . ? C21 Ti1 C22 C18 115.6(5) . . . . ? C20 Ti1 C22 C18 78.7(4) . . . . ? O6 Ti1 C22 C21 6.6(4) . . . . ? C23 Ti1 C22 C21 -157.1(5) . . . . ? C24 Ti1 C22 C21 -128.4(5) . . . . ? C27 Ti1 C22 C21 169.3(5) . . . . ? C26 Ti1 C22 C21 161.4(4) . . . . ? Cl1 Ti1 C22 C21 95.0(3) . . . . ? C19 Ti1 C22 C21 -77.5(4) . . . . ? C18 Ti1 C22 C21 -115.6(5) . . . . ? C25 Ti1 C22 C21 -130.9(6) . . . . ? C20 Ti1 C22 C21 -36.9(3) . . . . ? O6 Ti1 C23 C24 -32.0(10) . . . . ? C27 Ti1 C23 C24 -115.1(8) . . . . ? C26 Ti1 C23 C24 -76.1(6) . . . . ? Cl1 Ti1 C23 C24 -148.6(6) . . . . ? C19 Ti1 C23 C24 74.0(7) . . . . ? C18 Ti1 C23 C24 107.2(8) . . . . ? C25 Ti1 C23 C24 -35.5(5) . . . . ? C22 Ti1 C23 C24 129.5(6) . . . . ? C21 Ti1 C23 C24 112.2(6) . . . . ? C20 Ti1 C23 C24 71.8(6) . . . . ? O6 Ti1 C23 C27 83.2(10) . . . . ? C24 Ti1 C23 C27 115.1(8) . . . . ? C26 Ti1 C23 C27 39.1(5) . . . . ? Cl1 Ti1 C23 C27 -33.4(8) . . . . ? C19 Ti1 C23 C27 -170.8(8) . . . . ? C18 Ti1 C23 C27 -137.7(8) . . . . ? C25 Ti1 C23 C27 79.6(6) . . . . ? C22 Ti1 C23 C27 -115.3(7) . . . . ? C21 Ti1 C23 C27 -132.6(6) . . . . ? C20 Ti1 C23 C27 -173.1(6) . . . . ? C27 C23 C24 C25 1.6(10) . . . . ? Ti1 C23 C24 C25 67.6(6) . . . . ? C27 C23 C24 Ti1 -66.1(6) . . . . ? O6 Ti1 C24 C25 39.7(7) . . . . ? C23 Ti1 C24 C25 -116.6(9) . . . . ? C27 Ti1 C24 C25 -78.4(7) . . . . ? C26 Ti1 C24 C25 -36.3(5) . . . . ? Cl1 Ti1 C24 C25 -72.0(9) . . . . ? C19 Ti1 C24 C25 141.0(7) . . . . ? C18 Ti1 C24 C25 175.2(7) . . . . ? C22 Ti1 C24 C25 -177.7(6) . . . . ? C21 Ti1 C24 C25 142.8(5) . . . . ? C20 Ti1 C24 C25 121.4(6) . . . . ? O6 Ti1 C24 C23 156.2(7) . . . . ? C27 Ti1 C24 C23 38.2(6) . . . . ? C26 Ti1 C24 C23 80.3(6) . . . . ? Cl1 Ti1 C24 C23 44.6(9) . . . . ? C19 Ti1 C24 C23 -102.5(7) . . . . ? C18 Ti1 C24 C23 -68.2(7) . . . . ? C25 Ti1 C24 C23 116.6(9) . . . . ? C22 Ti1 C24 C23 -61.2(7) . . . . ? C21 Ti1 C24 C23 -100.6(6) . . . . ? C20 Ti1 C24 C23 -122.0(6) . . . . ? C23 C24 C25 C26 -2.2(9) . . . . ? Ti1 C24 C25 C26 64.0(5) . . . . ? C23 C24 C25 Ti1 -66.2(6) . . . . ? O6 Ti1 C25 C24 -140.7(7) . . . . ? C23 Ti1 C25 C24 36.6(6) . . . . ? C27 Ti1 C25 C24 78.9(7) . . . . ? C26 Ti1 C25 C24 117.7(8) . . . . ? Cl1 Ti1 C25 C24 130.0(7) . . . . ? C19 Ti1 C25 C24 -39.8(7) . . . . ? C18 Ti1 C25 C24 -5.5(8) . . . . ? C22 Ti1 C25 C24 4.2(11) . . . . ? C21 Ti1 C25 C24 -77.3(8) . . . . ? C20 Ti1 C25 C24 -71.8(7) . . . . ? O6 Ti1 C25 C26 101.6(6) . . . . ? C23 Ti1 C25 C26 -81.1(6) . . . . ? C24 Ti1 C25 C26 -117.7(8) . . . . ? C27 Ti1 C25 C26 -38.9(5) . . . . ? Cl1 Ti1 C25 C26 12.2(6) . . . . ? C19 Ti1 C25 C26 -157.5(5) . . . . ? C18 Ti1 C25 C26 -123.2(6) . . . . ? C22 Ti1 C25 C26 -113.6(8) . . . . ? C21 Ti1 C25 C26 165.0(5) . . . . ? C20 Ti1 C25 C26 170.5(5) . . . . ? C24 C25 C26 C27 2.0(8) . . . . ? Ti1 C25 C26 C27 65.8(5) . . . . ? C24 C25 C26 Ti1 -63.8(5) . . . . ? O6 Ti1 C26 C25 -74.2(5) . . . . ? C23 Ti1 C26 C25 74.7(6) . . . . ? C24 Ti1 C26 C25 34.8(5) . . . . ? C27 Ti1 C26 C25 113.6(7) . . . . ? Cl1 Ti1 C26 C25 -169.4(5) . . . . ? C19 Ti1 C26 C25 30.9(8) . . . . ? C18 Ti1 C26 C25 78.9(7) . . . . ? C22 Ti1 C26 C25 126.6(7) . . . . ? C21 Ti1 C26 C25 -141.6(14) . . . . ? C20 Ti1 C26 C25 -18.2(8) . . . . ? O6 Ti1 C26 C27 172.2(7) . . . . ? C23 Ti1 C26 C27 -38.9(6) . . . . ? C24 Ti1 C26 C27 -78.9(6) . . . . ? Cl1 Ti1 C26 C27 77.0(7) . . . . ? C19 Ti1 C26 C27 -82.7(9) . . . . ? C18 Ti1 C26 C27 -34.7(9) . . . . ? C25 Ti1 C26 C27 -113.6(7) . . . . ? C22 Ti1 C26 C27 13.0(9) . . . . ? C21 Ti1 C26 C27 104.7(15) . . . . ? C20 Ti1 C26 C27 -131.8(8) . . . . ? C24 C23 C27 C26 -0.3(9) . . . . ? Ti1 C23 C27 C26 -66.6(5) . . . . ? C24 C23 C27 Ti1 66.3(6) . . . . ? C25 C26 C27 C23 -1.0(8) . . . . ? Ti1 C26 C27 C23 66.0(6) . . . . ? C25 C26 C27 Ti1 -67.0(5) . . . . ? O6 Ti1 C27 C23 -121.4(8) . . . . ? C24 Ti1 C27 C23 -36.3(6) . . . . ? C26 Ti1 C27 C23 -112.3(8) . . . . ? Cl1 Ti1 C27 C23 148.3(8) . . . . ? C19 Ti1 C27 C23 10.8(9) . . . . ? C18 Ti1 C27 C23 41.9(8) . . . . ? C25 Ti1 C27 C23 -75.0(7) . . . . ? C22 Ti1 C27 C23 75.3(7) . . . . ? C21 Ti1 C27 C23 86.4(7) . . . . ? C20 Ti1 C27 C23 14.1(12) . . . . ? O6 Ti1 C27 C26 -9.1(8) . . . . ? C23 Ti1 C27 C26 112.3(8) . . . . ? C24 Ti1 C27 C26 76.0(6) . . . . ? Cl1 Ti1 C27 C26 -99.4(7) . . . . ? C19 Ti1 C27 C26 123.1(7) . . . . ? C18 Ti1 C27 C26 154.2(6) . . . . ? C25 Ti1 C27 C26 37.3(5) . . . . ? C22 Ti1 C27 C26 -172.4(6) . . . . ? C21 Ti1 C27 C26 -161.3(5) . . . . ? C20 Ti1 C27 C26 126.4(9) . . . . ? #END data_BvdW01_Complex_6b _database_code_depnum_ccdc_archive 'CCDC 810999' #TrackingRef '- Bezuidenhout_Barnard_vdWesthuizen_vdWatt_Liles_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ((Chloro-bis(\h^5^-pentadienyl)-titanium-oxy)-(ferrocenyl)-methylidene)- (pentacarbonyl)-tungsten ; _chemical_name_common ; ((Chloro-bis(eta$5!-pentadienyl)-titanium-oxy)-(ferrocenyl)- methylidene)-(pentacarbonyl)-tungsten ; _chemical_melting_point ? _chemical_formula_moiety 'C26 H19 Cl Fe O6 Ti W' _chemical_formula_sum 'C26 H19 Cl Fe O6 Ti W' _chemical_formula_weight 750.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' 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' _cell_length_a 23.220(3) _cell_length_b 10.0663(14) _cell_length_c 10.8634(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2539.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4454 _cell_measurement_theta_min 2.567 _cell_measurement_theta_max 24.669 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.963 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 5.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.328 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _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 'Bruker (Siemens) P4' _diffrn_measurement_method '\f and \w scans' _diffrn_detector 'SMART 1000 CCD' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 12791 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 26.43 _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 4518 _reflns_number_gt 3469 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement ;SHELXTL and SHELXL-97 (Sheldrick, 1997) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 1997), POV-Ray (Cason, 2004) ; _computing_publication_material SHELXL-97 _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^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(14) _refine_ls_number_reflns 4518 _refine_ls_number_parameters 325 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.977 _refine_diff_density_min -2.287 _refine_diff_density_rms 0.160 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.115085(14) 0.96545(3) 1.07371(6) 0.03646(12) Uani 1 1 d . . . C1 C 0.0939(5) 1.1270(13) 1.1722(12) 0.052(3) Uani 1 1 d . . . O1 O 0.0837(5) 1.2207(10) 1.2297(10) 0.089(3) Uani 1 1 d . . . C2 C 0.1190(5) 0.8544(13) 1.2321(12) 0.051(3) Uani 1 1 d . . . O2 O 0.1153(4) 0.7884(12) 1.3190(9) 0.083(4) Uani 1 1 d . . . C3 C 0.0311(4) 0.9255(11) 1.0687(18) 0.059(3) Uani 1 1 d . . . O3 O -0.0186(4) 0.9095(11) 1.0684(18) 0.123(5) Uani 1 1 d . . . C4 C 0.1043(5) 1.0684(12) 0.9171(12) 0.047(3) Uani 1 1 d . . . O4 O 0.0946(5) 1.1256(10) 0.8323(11) 0.083(3) Uani 1 1 d . . . C5 C 0.1981(4) 1.0294(9) 1.0785(19) 0.046(2) Uani 1 1 d . . . O5 O 0.2438(3) 1.0740(7) 1.0844(12) 0.061(2) Uani 1 1 d . . . C6 C 0.1469(4) 0.7829(9) 0.9749(9) 0.032(2) Uani 1 1 d . . . O6 O 0.1886(3) 0.7180(7) 1.0218(6) 0.0355(15) Uani 1 1 d . . . Fe1 Fe 0.05873(6) 0.59515(15) 0.84703(13) 0.0383(3) Uani 1 1 d . . . C7 C 0.1249(4) 0.7279(11) 0.8592(10) 0.035(3) Uani 1 1 d . . . C8 C 0.0778(5) 0.7785(11) 0.7858(9) 0.046(3) Uani 1 1 d . . . H8 H 0.0567 0.8547 0.8033 0.055 Uiso 1 1 calc R . . C9 C 0.0689(5) 0.6970(13) 0.6866(9) 0.054(3) Uani 1 1 d . . . H9 H 0.0414 0.7093 0.6254 0.065 Uiso 1 1 calc R . . C10 C 0.1093(5) 0.5896(14) 0.6933(11) 0.055(3) Uani 1 1 d . . . H10 H 0.1122 0.5194 0.6381 0.066 Uiso 1 1 calc R . . C11 C 0.1437(5) 0.6093(11) 0.7984(9) 0.043(3) Uani 1 1 d . . . H11 H 0.1736 0.5544 0.8241 0.051 Uiso 1 1 calc R . . C12 C 0.0264(5) 0.5586(13) 1.0190(12) 0.058(3) Uani 1 1 d . . . H12 H 0.0399 0.5983 1.0907 0.070 Uiso 1 1 calc R . . C13 C -0.0179(5) 0.6052(13) 0.9438(11) 0.054(3) Uani 1 1 d . . . H13 H -0.0401 0.6804 0.9589 0.065 Uiso 1 1 calc R . . C14 C -0.0237(5) 0.5211(13) 0.8419(13) 0.055(3) Uani 1 1 d . . . H14 H -0.0497 0.5323 0.7776 0.066 Uiso 1 1 calc R . . C15 C 0.0170(5) 0.4152(12) 0.8528(14) 0.056(3) Uani 1 1 d . . . H15 H 0.0226 0.3458 0.7976 0.067 Uiso 1 1 calc R . . C16 C 0.0471(5) 0.4373(13) 0.9645(14) 0.064(4) Uani 1 1 d . . . H16 H 0.0755 0.3826 0.9972 0.077 Uiso 1 1 calc R . . Ti1 Ti 0.25472(7) 0.63245(15) 1.08771(19) 0.0312(4) Uani 1 1 d . . . Cl1 Cl 0.27049(12) 0.7881(3) 1.2518(2) 0.0440(6) Uani 1 1 d . . . C18 C 0.2623(6) 0.3996(11) 1.1284(18) 0.083(6) Uani 1 1 d . . . H18 H 0.2919 0.3483 1.0955 0.099 Uiso 1 1 calc R . . C19 C 0.2087(7) 0.4239(11) 1.0772(18) 0.070(4) Uani 1 1 d . . . H19 H 0.1966 0.3959 0.9998 0.084 Uiso 1 1 calc R . . C20 C 0.1775(6) 0.4931(14) 1.1557(17) 0.070(5) Uani 1 1 d . . . H20 H 0.1394 0.5176 1.1430 0.084 Uiso 1 1 calc R . . C21 C 0.2076(8) 0.5227(13) 1.2543(14) 0.069(4) Uani 1 1 d . . . H21 H 0.1943 0.5712 1.3214 0.083 Uiso 1 1 calc R . . C22 C 0.2626(8) 0.4698(14) 1.2421(17) 0.087(6) Uani 1 1 d . . . H22 H 0.2931 0.4784 1.2968 0.105 Uiso 1 1 calc R . . C23 C 0.3464(4) 0.5724(11) 1.0106(12) 0.051(3) Uani 1 1 d . . . H23 H 0.3658 0.5001 1.0439 0.061 Uiso 1 1 calc R . . C24 C 0.3071(5) 0.5677(12) 0.9146(11) 0.052(3) Uani 1 1 d . . . H24 H 0.2958 0.4909 0.8738 0.062 Uiso 1 1 calc R . . C25 C 0.2870(5) 0.6958(12) 0.8883(10) 0.049(3) Uani 1 1 d . . . H25 H 0.2613 0.7206 0.8268 0.059 Uiso 1 1 calc R . . C26 C 0.3138(4) 0.7778(11) 0.9736(10) 0.044(3) Uani 1 1 d . . . H26 H 0.3076 0.8688 0.9804 0.052 Uiso 1 1 calc R . . C27 C 0.3518(4) 0.7043(11) 1.0487(11) 0.047(3) Uani 1 1 d . . . H27 H 0.3755 0.7369 1.1107 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.03667(19) 0.03077(19) 0.0419(2) -0.0059(3) -0.0006(3) 0.00387(16) C1 0.050(7) 0.050(8) 0.056(8) -0.006(7) -0.010(6) 0.007(6) O1 0.105(8) 0.065(7) 0.098(8) -0.046(6) -0.005(6) 0.042(6) C2 0.044(7) 0.049(8) 0.061(8) -0.011(7) 0.002(6) -0.006(5) O2 0.121(10) 0.083(9) 0.044(6) 0.026(6) 0.002(5) -0.012(6) C3 0.038(5) 0.066(7) 0.071(7) -0.032(12) 0.003(9) 0.002(5) O3 0.047(5) 0.134(10) 0.188(12) -0.080(14) 0.005(10) -0.009(5) C4 0.058(8) 0.037(7) 0.046(7) 0.011(6) 0.001(6) 0.005(5) O4 0.100(8) 0.066(7) 0.084(8) 0.013(6) -0.001(6) 0.009(6) C5 0.045(5) 0.032(5) 0.061(7) 0.001(8) -0.008(10) 0.013(4) O5 0.045(4) 0.049(4) 0.090(6) -0.004(6) -0.008(6) -0.009(3) C6 0.039(6) 0.025(5) 0.033(5) 0.006(4) 0.009(4) -0.003(5) O6 0.033(4) 0.031(4) 0.042(4) -0.003(3) -0.007(3) 0.007(3) Fe1 0.0417(8) 0.0318(8) 0.0413(9) -0.0010(7) -0.0065(7) -0.0001(7) C7 0.037(6) 0.034(6) 0.034(6) 0.002(5) -0.001(4) 0.001(4) C8 0.055(7) 0.040(7) 0.041(7) 0.000(5) -0.014(5) 0.001(5) C9 0.075(9) 0.066(9) 0.021(6) 0.000(5) -0.009(5) 0.004(7) C10 0.066(8) 0.053(7) 0.045(7) -0.018(6) -0.001(6) 0.001(6) C11 0.042(6) 0.047(7) 0.039(6) -0.005(5) -0.001(5) 0.002(5) C12 0.068(8) 0.056(8) 0.051(7) 0.002(6) 0.004(6) -0.014(6) C13 0.043(7) 0.048(8) 0.071(8) -0.003(7) 0.001(6) -0.001(6) C14 0.047(7) 0.053(8) 0.066(9) 0.000(7) -0.012(6) -0.015(6) C15 0.052(7) 0.026(6) 0.090(10) -0.002(7) -0.015(7) 0.002(5) C16 0.056(8) 0.057(9) 0.080(10) 0.026(7) -0.024(7) -0.013(6) Ti1 0.0348(8) 0.0236(7) 0.0353(11) 0.0007(9) -0.0025(9) 0.0021(6) Cl1 0.0569(17) 0.0350(15) 0.0402(14) -0.0109(12) -0.0060(12) -0.0030(12) C18 0.072(9) 0.012(5) 0.165(19) 0.026(8) 0.044(10) 0.007(6) C19 0.113(11) 0.047(7) 0.050(7) 0.007(11) -0.005(13) -0.044(7) C20 0.048(8) 0.059(9) 0.102(12) 0.056(9) 0.015(8) 0.010(6) C21 0.106(12) 0.047(8) 0.053(8) 0.018(7) 0.013(9) -0.002(8) C22 0.113(14) 0.038(8) 0.110(14) 0.042(9) -0.053(11) -0.043(9) C23 0.028(5) 0.045(7) 0.079(8) 0.009(6) 0.009(5) 0.005(5) C24 0.049(7) 0.046(7) 0.060(8) -0.012(6) 0.011(6) -0.003(5) C25 0.061(7) 0.047(7) 0.040(6) 0.010(6) 0.009(5) -0.005(6) C26 0.050(6) 0.024(6) 0.057(7) 0.000(5) 0.004(5) -0.010(5) C27 0.041(5) 0.044(6) 0.056(9) 0.008(6) -0.005(5) -0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C3 1.993(10) . ? W1 C4 2.008(13) . ? W1 C1 2.008(13) . ? W1 C5 2.033(10) . ? W1 C2 2.053(14) . ? W1 C6 2.253(9) . ? C1 O1 1.155(14) . ? C2 O2 1.158(15) . ? C3 O3 1.163(12) . ? C4 O4 1.109(14) . ? C5 O5 1.154(11) . ? C6 O6 1.273(11) . ? C6 C7 1.465(15) . ? O6 Ti1 1.901(6) . ? Fe1 C8 2.011(11) . ? Fe1 C9 2.036(11) . ? Fe1 C7 2.042(11) . ? Fe1 C10 2.042(12) . ? Fe1 C11 2.047(11) . ? Fe1 C12 2.047(12) . ? Fe1 C14 2.054(12) . ? Fe1 C15 2.055(12) . ? Fe1 C16 2.056(13) . ? Fe1 C13 2.069(11) . ? C7 C11 1.432(14) . ? C7 C8 1.447(14) . ? C8 C9 1.370(15) . ? C8 H8 0.9300 . ? C9 C10 1.433(17) . ? C9 H9 0.9300 . ? C10 C11 1.407(15) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.395(16) . ? C12 C16 1.440(18) . ? C12 H12 0.9300 . ? C13 C14 1.400(17) . ? C13 H13 0.9300 . ? C14 C15 1.430(17) . ? C14 H14 0.9300 . ? C15 C16 1.419(18) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? Ti1 C24 2.332(11) . ? Ti1 C22 2.351(13) . ? Ti1 C26 2.358(10) . ? Ti1 C19 2.359(10) . ? Ti1 C23 2.366(10) . ? Ti1 C25 2.380(11) . ? Ti1 C21 2.386(13) . ? Ti1 C18 2.392(11) . ? Ti1 C20 2.393(13) . ? Ti1 Cl1 2.402(3) . ? Ti1 C27 2.404(10) . ? C18 C19 1.387(18) . ? C18 C22 1.42(2) . ? C18 H18 0.9300 . ? C19 C20 1.32(2) . ? C19 H19 0.9300 . ? C20 C21 1.31(2) . ? C20 H20 0.9300 . ? C21 C22 1.39(2) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.386(16) . ? C23 C27 1.396(14) . ? C23 H23 0.9300 . ? C24 C25 1.401(16) . ? C24 H24 0.9300 . ? C25 C26 1.389(15) . ? C25 H25 0.9300 . ? C26 C27 1.411(14) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? 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 C3 W1 C4 87.6(7) . . ? C3 W1 C1 86.5(5) . . ? C4 W1 C1 90.2(6) . . ? C3 W1 C5 173.2(4) . . ? C4 W1 C5 88.7(6) . . ? C1 W1 C5 87.8(5) . . ? C3 W1 C2 87.5(6) . . ? C4 W1 C2 175.1(5) . . ? C1 W1 C2 90.3(5) . . ? C5 W1 C2 96.2(6) . . ? C3 W1 C6 98.3(4) . . ? C4 W1 C6 93.3(4) . . ? C1 W1 C6 174.2(4) . . ? C5 W1 C6 87.7(4) . . ? C2 W1 C6 86.6(4) . . ? O1 C1 W1 177.7(11) . . ? O2 C2 W1 172.8(10) . . ? O3 C3 W1 176.1(10) . . ? O4 C4 W1 175.5(12) . . ? O5 C5 W1 175.2(10) . . ? O6 C6 C7 114.5(8) . . ? O6 C6 W1 118.5(7) . . ? C7 C6 W1 127.0(7) . . ? C6 O6 Ti1 175.4(7) . . ? C8 Fe1 C9 39.6(4) . . ? C8 Fe1 C7 41.8(4) . . ? C9 Fe1 C7 68.8(5) . . ? C8 Fe1 C10 68.2(5) . . ? C9 Fe1 C10 41.2(5) . . ? C7 Fe1 C10 68.8(5) . . ? C8 Fe1 C11 68.8(5) . . ? C9 Fe1 C11 68.4(5) . . ? C7 Fe1 C11 41.0(4) . . ? C10 Fe1 C11 40.3(4) . . ? C8 Fe1 C12 123.2(5) . . ? C9 Fe1 C12 156.1(5) . . ? C7 Fe1 C12 109.6(5) . . ? C10 Fe1 C12 162.3(5) . . ? C11 Fe1 C12 127.0(5) . . ? C8 Fe1 C14 121.9(5) . . ? C9 Fe1 C14 105.5(5) . . ? C7 Fe1 C14 160.2(5) . . ? C10 Fe1 C14 120.2(5) . . ? C11 Fe1 C14 156.3(5) . . ? C12 Fe1 C14 67.5(5) . . ? C8 Fe1 C15 157.3(5) . . ? C9 Fe1 C15 121.6(5) . . ? C7 Fe1 C15 158.4(4) . . ? C10 Fe1 C15 105.8(6) . . ? C11 Fe1 C15 121.6(5) . . ? C12 Fe1 C15 69.0(6) . . ? C14 Fe1 C15 40.7(5) . . ? C8 Fe1 C16 160.6(5) . . ? C9 Fe1 C16 159.4(5) . . ? C7 Fe1 C16 124.4(5) . . ? C10 Fe1 C16 124.2(6) . . ? C11 Fe1 C16 109.9(5) . . ? C12 Fe1 C16 41.1(5) . . ? C14 Fe1 C16 67.3(5) . . ? C15 Fe1 C16 40.4(5) . . ? C8 Fe1 C13 108.2(5) . . ? C9 Fe1 C13 120.6(5) . . ? C7 Fe1 C13 125.6(5) . . ? C10 Fe1 C13 155.7(5) . . ? C11 Fe1 C13 163.0(4) . . ? C12 Fe1 C13 39.6(5) . . ? C14 Fe1 C13 39.7(5) . . ? C15 Fe1 C13 67.8(5) . . ? C16 Fe1 C13 67.0(5) . . ? C11 C7 C8 105.6(9) . . ? C11 C7 C6 127.2(9) . . ? C8 C7 C6 127.1(9) . . ? C11 C7 Fe1 69.7(6) . . ? C8 C7 Fe1 68.0(6) . . ? C6 C7 Fe1 124.4(7) . . ? C9 C8 C7 109.7(10) . . ? C9 C8 Fe1 71.2(7) . . ? C7 C8 Fe1 70.2(6) . . ? C9 C8 H8 125.1 . . ? C7 C8 H8 125.1 . . ? Fe1 C8 H8 125.0 . . ? C8 C9 C10 108.2(10) . . ? C8 C9 Fe1 69.2(6) . . ? C10 C9 Fe1 69.6(7) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe1 C9 H9 126.8 . . ? C11 C10 C9 107.9(10) . . ? C11 C10 Fe1 70.0(7) . . ? C9 C10 Fe1 69.2(6) . . ? C11 C10 H10 126.1 . . ? C9 C10 H10 126.1 . . ? Fe1 C10 H10 126.2 . . ? C10 C11 C7 108.6(10) . . ? C10 C11 Fe1 69.7(6) . . ? C7 C11 Fe1 69.3(6) . . ? C10 C11 H11 125.7 . . ? C7 C11 H11 125.7 . . ? Fe1 C11 H11 126.9 . . ? C13 C12 C16 106.9(11) . . ? C13 C12 Fe1 71.0(7) . . ? C16 C12 Fe1 69.8(7) . . ? C13 C12 H12 126.5 . . ? C16 C12 H12 126.5 . . ? Fe1 C12 H12 124.3 . . ? C12 C13 C14 109.3(12) . . ? C12 C13 Fe1 69.3(7) . . ? C14 C13 Fe1 69.6(7) . . ? C12 C13 H13 125.3 . . ? C14 C13 H13 125.3 . . ? Fe1 C13 H13 127.3 . . ? C13 C14 C15 108.8(11) . . ? C13 C14 Fe1 70.7(7) . . ? C15 C14 Fe1 69.7(7) . . ? C13 C14 H14 125.6 . . ? C15 C14 H14 125.6 . . ? Fe1 C14 H14 125.6 . . ? C16 C15 C14 106.2(12) . . ? C16 C15 Fe1 69.8(7) . . ? C14 C15 Fe1 69.6(8) . . ? C16 C15 H15 126.9 . . ? C14 C15 H15 126.9 . . ? Fe1 C15 H15 125.3 . . ? C15 C16 C12 108.7(11) . . ? C15 C16 Fe1 69.8(7) . . ? C12 C16 Fe1 69.1(7) . . ? C15 C16 H16 125.7 . . ? C12 C16 H16 125.7 . . ? Fe1 C16 H16 127.0 . . ? O6 Ti1 C24 104.2(4) . . ? O6 Ti1 C22 130.3(5) . . ? C24 Ti1 C22 109.9(6) . . ? O6 Ti1 C26 89.5(4) . . ? C24 Ti1 C26 56.4(4) . . ? C22 Ti1 C26 139.7(5) . . ? O6 Ti1 C19 91.1(5) . . ? C24 Ti1 C19 87.1(6) . . ? C22 Ti1 C19 56.6(5) . . ? C26 Ti1 C19 142.3(6) . . ? O6 Ti1 C23 135.2(4) . . ? C24 Ti1 C23 34.3(4) . . ? C22 Ti1 C23 90.3(6) . . ? C26 Ti1 C23 56.6(4) . . ? C19 Ti1 C23 99.4(5) . . ? O6 Ti1 C25 77.9(4) . . ? C24 Ti1 C25 34.6(4) . . ? C22 Ti1 C25 144.3(6) . . ? C26 Ti1 C25 34.1(4) . . ? C19 Ti1 C25 109.7(6) . . ? C23 Ti1 C25 57.5(4) . . ? O6 Ti1 C21 97.2(5) . . ? C24 Ti1 C21 136.2(5) . . ? C22 Ti1 C21 34.1(6) . . ? C26 Ti1 C21 162.3(5) . . ? C19 Ti1 C21 54.3(6) . . ? C23 Ti1 C21 124.3(5) . . ? C25 Ti1 C21 163.6(5) . . ? O6 Ti1 C18 125.0(5) . . ? C24 Ti1 C18 80.6(5) . . ? C22 Ti1 C18 34.9(6) . . ? C26 Ti1 C18 131.5(4) . . ? C19 Ti1 C18 33.9(5) . . ? C23 Ti1 C18 75.4(4) . . ? C25 Ti1 C18 114.1(5) . . ? C21 Ti1 C18 55.9(5) . . ? O6 Ti1 C20 77.1(4) . . ? C24 Ti1 C20 118.4(6) . . ? C22 Ti1 C20 55.2(5) . . ? C26 Ti1 C20 164.1(5) . . ? C19 Ti1 C20 32.2(5) . . ? C23 Ti1 C20 129.3(5) . . ? C25 Ti1 C20 132.4(6) . . ? C21 Ti1 C20 31.9(5) . . ? C18 Ti1 C20 54.8(4) . . ? O6 Ti1 Cl1 96.1(2) . . ? C24 Ti1 Cl1 134.5(3) . . ? C22 Ti1 Cl1 85.0(5) . . ? C26 Ti1 Cl1 84.1(3) . . ? C19 Ti1 Cl1 133.3(5) . . ? C23 Ti1 Cl1 107.0(3) . . ? C25 Ti1 Cl1 116.9(3) . . ? C21 Ti1 Cl1 79.0(4) . . ? C18 Ti1 Cl1 119.4(5) . . ? C20 Ti1 Cl1 105.5(5) . . ? O6 Ti1 C27 123.7(3) . . ? C24 Ti1 C27 56.8(4) . . ? C22 Ti1 C27 105.2(5) . . ? C26 Ti1 C27 34.4(3) . . ? C19 Ti1 C27 133.2(5) . . ? C23 Ti1 C27 34.0(3) . . ? C25 Ti1 C27 57.6(4) . . ? C21 Ti1 C27 134.7(5) . . ? C18 Ti1 C27 105.0(4) . . ? C20 Ti1 C27 158.9(4) . . ? Cl1 Ti1 C27 78.0(3) . . ? C19 C18 C22 105.3(13) . . ? C19 C18 Ti1 71.7(6) . . ? C22 C18 Ti1 71.0(7) . . ? C19 C18 H18 127.3 . . ? C22 C18 H18 127.3 . . ? Ti1 C18 H18 121.8 . . ? C20 C19 C18 109.1(16) . . ? C20 C19 Ti1 75.4(8) . . ? C18 C19 Ti1 74.3(6) . . ? C20 C19 H19 125.5 . . ? C18 C19 H19 125.5 . . ? Ti1 C19 H19 116.8 . . ? C21 C20 C19 110.9(14) . . ? C21 C20 Ti1 73.8(9) . . ? C19 C20 Ti1 72.5(7) . . ? C21 C20 H20 124.5 . . ? C19 C20 H20 124.5 . . ? Ti1 C20 H20 120.8 . . ? C20 C21 C22 108.9(14) . . ? C20 C21 Ti1 74.3(8) . . ? C22 C21 Ti1 71.6(8) . . ? C20 C21 H21 125.6 . . ? C22 C21 H21 125.6 . . ? Ti1 C21 H21 120.2 . . ? C21 C22 C18 105.6(13) . . ? C21 C22 Ti1 74.3(8) . . ? C18 C22 Ti1 74.1(8) . . ? C21 C22 H22 127.2 . . ? C18 C22 H22 127.2 . . ? Ti1 C22 H22 116.7 . . ? C24 C23 C27 108.3(10) . . ? C24 C23 Ti1 71.5(6) . . ? C27 C23 Ti1 74.5(6) . . ? C24 C23 H23 125.8 . . ? C27 C23 H23 125.8 . . ? Ti1 C23 H23 119.9 . . ? C23 C24 C25 110.0(11) . . ? C23 C24 Ti1 74.2(7) . . ? C25 C24 Ti1 74.6(6) . . ? C23 C24 H24 125.0 . . ? C25 C24 H24 125.0 . . ? Ti1 C24 H24 118.0 . . ? C26 C25 C24 105.2(11) . . ? C26 C25 Ti1 72.1(6) . . ? C24 C25 Ti1 70.9(6) . . ? C26 C25 H25 127.4 . . ? C24 C25 H25 127.4 . . ? Ti1 C25 H25 121.5 . . ? C25 C26 C27 110.7(10) . . ? C25 C26 Ti1 73.8(6) . . ? C27 C26 Ti1 74.6(6) . . ? C25 C26 H26 124.6 . . ? C27 C26 H26 124.6 . . ? Ti1 C26 H26 118.6 . . ? C23 C27 C26 105.8(10) . . ? C23 C27 Ti1 71.5(6) . . ? C26 C27 Ti1 71.0(6) . . ? C23 C27 H27 127.1 . . ? C26 C27 H27 127.1 . . ? Ti1 C27 H27 122.2 . . ? 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 C3 W1 C6 O6 -132.0(9) . . . . ? C4 W1 C6 O6 139.9(8) . . . . ? C5 W1 C6 O6 51.4(9) . . . . ? C2 W1 C6 O6 -45.0(7) . . . . ? C3 W1 C6 C7 48.1(10) . . . . ? C4 W1 C6 C7 -39.9(9) . . . . ? C5 W1 C6 C7 -128.5(10) . . . . ? C2 W1 C6 C7 135.1(9) . . . . ? O6 C6 C7 C11 2.6(15) . . . . ? W1 C6 C7 C11 -177.5(8) . . . . ? O6 C6 C7 C8 179.1(9) . . . . ? W1 C6 C7 C8 -1.0(15) . . . . ? O6 C6 C7 Fe1 92.1(10) . . . . ? W1 C6 C7 Fe1 -88.0(10) . . . . ? C8 Fe1 C7 C11 -117.3(9) . . . . ? C9 Fe1 C7 C11 -81.1(7) . . . . ? C10 Fe1 C7 C11 -36.8(7) . . . . ? C12 Fe1 C7 C11 124.3(7) . . . . ? C14 Fe1 C7 C11 -157.7(14) . . . . ? C15 Fe1 C7 C11 42.2(17) . . . . ? C16 Fe1 C7 C11 80.9(8) . . . . ? C13 Fe1 C7 C11 165.7(6) . . . . ? C9 Fe1 C7 C8 36.2(6) . . . . ? C10 Fe1 C7 C8 80.5(7) . . . . ? C11 Fe1 C7 C8 117.3(9) . . . . ? C12 Fe1 C7 C8 -118.3(7) . . . . ? C14 Fe1 C7 C8 -40.4(17) . . . . ? C15 Fe1 C7 C8 159.6(14) . . . . ? C16 Fe1 C7 C8 -161.8(8) . . . . ? C13 Fe1 C7 C8 -77.0(8) . . . . ? C8 Fe1 C7 C6 120.8(11) . . . . ? C9 Fe1 C7 C6 157.0(10) . . . . ? C10 Fe1 C7 C6 -158.7(10) . . . . ? C11 Fe1 C7 C6 -121.9(11) . . . . ? C12 Fe1 C7 C6 2.5(10) . . . . ? C14 Fe1 C7 C6 80.4(17) . . . . ? C15 Fe1 C7 C6 -79.6(17) . . . . ? C16 Fe1 C7 C6 -41.0(11) . . . . ? C13 Fe1 C7 C6 43.8(11) . . . . ? C11 C7 C8 C9 -0.6(12) . . . . ? C6 C7 C8 C9 -177.7(10) . . . . ? Fe1 C7 C8 C9 -60.5(8) . . . . ? C11 C7 C8 Fe1 59.9(7) . . . . ? C6 C7 C8 Fe1 -117.3(11) . . . . ? C7 Fe1 C8 C9 120.1(10) . . . . ? C10 Fe1 C8 C9 38.0(7) . . . . ? C11 Fe1 C8 C9 81.4(7) . . . . ? C12 Fe1 C8 C9 -157.5(7) . . . . ? C14 Fe1 C8 C9 -74.9(8) . . . . ? C15 Fe1 C8 C9 -40.5(16) . . . . ? C16 Fe1 C8 C9 171.3(14) . . . . ? C13 Fe1 C8 C9 -116.4(8) . . . . ? C9 Fe1 C8 C7 -120.1(10) . . . . ? C10 Fe1 C8 C7 -82.1(7) . . . . ? C11 Fe1 C8 C7 -38.7(6) . . . . ? C12 Fe1 C8 C7 82.5(8) . . . . ? C14 Fe1 C8 C7 165.0(7) . . . . ? C15 Fe1 C8 C7 -160.6(12) . . . . ? C16 Fe1 C8 C7 51.2(17) . . . . ? C13 Fe1 C8 C7 123.5(7) . . . . ? C7 C8 C9 C10 1.0(14) . . . . ? Fe1 C8 C9 C10 -58.9(9) . . . . ? C7 C8 C9 Fe1 59.9(8) . . . . ? C7 Fe1 C9 C8 -38.2(7) . . . . ? C10 Fe1 C9 C8 -119.8(10) . . . . ? C11 Fe1 C9 C8 -82.4(7) . . . . ? C12 Fe1 C9 C8 52.4(15) . . . . ? C14 Fe1 C9 C8 121.7(7) . . . . ? C15 Fe1 C9 C8 162.9(7) . . . . ? C16 Fe1 C9 C8 -171.8(13) . . . . ? C13 Fe1 C9 C8 81.5(8) . . . . ? C8 Fe1 C9 C10 119.8(10) . . . . ? C7 Fe1 C9 C10 81.6(7) . . . . ? C11 Fe1 C9 C10 37.4(7) . . . . ? C12 Fe1 C9 C10 172.2(11) . . . . ? C14 Fe1 C9 C10 -118.5(7) . . . . ? C15 Fe1 C9 C10 -77.3(8) . . . . ? C16 Fe1 C9 C10 -52.0(17) . . . . ? C13 Fe1 C9 C10 -158.6(7) . . . . ? C8 C9 C10 C11 -1.0(14) . . . . ? Fe1 C9 C10 C11 -59.6(9) . . . . ? C8 C9 C10 Fe1 58.6(8) . . . . ? C8 Fe1 C10 C11 82.6(8) . . . . ? C9 Fe1 C10 C11 119.1(11) . . . . ? C7 Fe1 C10 C11 37.4(7) . . . . ? C12 Fe1 C10 C11 -50.5(19) . . . . ? C14 Fe1 C10 C11 -162.2(7) . . . . ? C15 Fe1 C10 C11 -120.5(7) . . . . ? C16 Fe1 C10 C11 -80.5(9) . . . . ? C13 Fe1 C10 C11 168.6(11) . . . . ? C8 Fe1 C10 C9 -36.5(7) . . . . ? C7 Fe1 C10 C9 -81.7(7) . . . . ? C11 Fe1 C10 C9 -119.1(11) . . . . ? C12 Fe1 C10 C9 -169.7(15) . . . . ? C14 Fe1 C10 C9 78.7(9) . . . . ? C15 Fe1 C10 C9 120.3(7) . . . . ? C16 Fe1 C10 C9 160.4(7) . . . . ? C13 Fe1 C10 C9 49.5(16) . . . . ? C9 C10 C11 C7 0.6(13) . . . . ? Fe1 C10 C11 C7 -58.5(8) . . . . ? C9 C10 C11 Fe1 59.1(9) . . . . ? C8 C7 C11 C10 0.0(12) . . . . ? C6 C7 C11 C10 177.1(10) . . . . ? Fe1 C7 C11 C10 58.7(8) . . . . ? C8 C7 C11 Fe1 -58.7(7) . . . . ? C6 C7 C11 Fe1 118.4(11) . . . . ? C8 Fe1 C11 C10 -80.8(8) . . . . ? C9 Fe1 C11 C10 -38.2(8) . . . . ? C7 Fe1 C11 C10 -120.3(10) . . . . ? C12 Fe1 C11 C10 162.9(8) . . . . ? C14 Fe1 C11 C10 41.1(16) . . . . ? C15 Fe1 C11 C10 76.6(9) . . . . ? C16 Fe1 C11 C10 119.8(8) . . . . ? C13 Fe1 C11 C10 -163.8(15) . . . . ? C8 Fe1 C11 C7 39.4(6) . . . . ? C9 Fe1 C11 C7 82.1(7) . . . . ? C10 Fe1 C11 C7 120.3(10) . . . . ? C12 Fe1 C11 C7 -76.9(8) . . . . ? C14 Fe1 C11 C7 161.3(12) . . . . ? C15 Fe1 C11 C7 -163.2(7) . . . . ? C16 Fe1 C11 C7 -119.9(7) . . . . ? C13 Fe1 C11 C7 -43.5(18) . . . . ? C8 Fe1 C12 C13 78.1(8) . . . . ? C9 Fe1 C12 C13 41.0(16) . . . . ? C7 Fe1 C12 C13 122.7(7) . . . . ? C10 Fe1 C12 C13 -155.9(15) . . . . ? C11 Fe1 C12 C13 165.4(7) . . . . ? C14 Fe1 C12 C13 -36.3(7) . . . . ? C15 Fe1 C12 C13 -80.2(8) . . . . ? C16 Fe1 C12 C13 -117.0(10) . . . . ? C8 Fe1 C12 C16 -164.8(7) . . . . ? C9 Fe1 C12 C16 158.1(11) . . . . ? C7 Fe1 C12 C16 -120.3(7) . . . . ? C10 Fe1 C12 C16 -38.9(19) . . . . ? C11 Fe1 C12 C16 -77.6(8) . . . . ? C14 Fe1 C12 C16 80.8(8) . . . . ? C15 Fe1 C12 C16 36.8(7) . . . . ? C13 Fe1 C12 C16 117.0(10) . . . . ? C16 C12 C13 C14 -2.7(14) . . . . ? Fe1 C12 C13 C14 58.2(9) . . . . ? C16 C12 C13 Fe1 -60.9(9) . . . . ? C8 Fe1 C13 C12 -120.5(7) . . . . ? C9 Fe1 C13 C12 -162.0(7) . . . . ? C7 Fe1 C13 C12 -77.3(9) . . . . ? C10 Fe1 C13 C12 162.4(12) . . . . ? C11 Fe1 C13 C12 -43.5(19) . . . . ? C14 Fe1 C13 C12 121.1(11) . . . . ? C15 Fe1 C13 C12 83.4(8) . . . . ? C16 Fe1 C13 C12 39.5(7) . . . . ? C8 Fe1 C13 C14 118.4(8) . . . . ? C9 Fe1 C13 C14 76.8(9) . . . . ? C7 Fe1 C13 C14 161.5(7) . . . . ? C10 Fe1 C13 C14 41.3(16) . . . . ? C11 Fe1 C13 C14 -164.7(15) . . . . ? C12 Fe1 C13 C14 -121.1(11) . . . . ? C15 Fe1 C13 C14 -37.8(8) . . . . ? C16 Fe1 C13 C14 -81.7(9) . . . . ? C12 C13 C14 C15 1.4(15) . . . . ? Fe1 C13 C14 C15 59.5(10) . . . . ? C12 C13 C14 Fe1 -58.1(9) . . . . ? C8 Fe1 C14 C13 -80.0(9) . . . . ? C9 Fe1 C14 C13 -119.6(8) . . . . ? C7 Fe1 C14 C13 -49.3(18) . . . . ? C10 Fe1 C14 C13 -161.6(8) . . . . ? C11 Fe1 C14 C13 168.9(10) . . . . ? C12 Fe1 C14 C13 36.2(8) . . . . ? C15 Fe1 C14 C13 119.6(12) . . . . ? C16 Fe1 C14 C13 80.9(9) . . . . ? C8 Fe1 C14 C15 160.5(8) . . . . ? C9 Fe1 C14 C15 120.8(9) . . . . ? C7 Fe1 C14 C15 -168.9(13) . . . . ? C10 Fe1 C14 C15 78.8(10) . . . . ? C11 Fe1 C14 C15 49.3(17) . . . . ? C12 Fe1 C14 C15 -83.4(9) . . . . ? C16 Fe1 C14 C15 -38.7(9) . . . . ? C13 Fe1 C14 C15 -119.6(12) . . . . ? C13 C14 C15 C16 0.5(16) . . . . ? Fe1 C14 C15 C16 60.6(9) . . . . ? C13 C14 C15 Fe1 -60.1(9) . . . . ? C8 Fe1 C15 C16 -164.4(12) . . . . ? C9 Fe1 C15 C16 166.6(8) . . . . ? C7 Fe1 C15 C16 52.8(18) . . . . ? C10 Fe1 C15 C16 124.7(8) . . . . ? C11 Fe1 C15 C16 83.9(9) . . . . ? C12 Fe1 C15 C16 -37.4(8) . . . . ? C14 Fe1 C15 C16 -117.0(12) . . . . ? C13 Fe1 C15 C16 -80.2(9) . . . . ? C8 Fe1 C15 C14 -47.4(17) . . . . ? C9 Fe1 C15 C14 -76.4(10) . . . . ? C7 Fe1 C15 C14 169.8(12) . . . . ? C10 Fe1 C15 C14 -118.3(8) . . . . ? C11 Fe1 C15 C14 -159.1(8) . . . . ? C12 Fe1 C15 C14 79.6(9) . . . . ? C16 Fe1 C15 C14 117.0(12) . . . . ? C13 Fe1 C15 C14 36.9(8) . . . . ? C14 C15 C16 C12 -2.1(16) . . . . ? Fe1 C15 C16 C12 58.3(9) . . . . ? C14 C15 C16 Fe1 -60.4(10) . . . . ? C13 C12 C16 C15 3.0(15) . . . . ? Fe1 C12 C16 C15 -58.7(9) . . . . ? C13 C12 C16 Fe1 61.7(8) . . . . ? C8 Fe1 C16 C15 161.7(13) . . . . ? C9 Fe1 C16 C15 -34.2(18) . . . . ? C7 Fe1 C16 C15 -159.2(7) . . . . ? C10 Fe1 C16 C15 -73.0(9) . . . . ? C11 Fe1 C16 C15 -115.7(8) . . . . ? C12 Fe1 C16 C15 120.4(11) . . . . ? C14 Fe1 C16 C15 39.0(7) . . . . ? C13 Fe1 C16 C15 82.3(8) . . . . ? C8 Fe1 C16 C12 41.4(18) . . . . ? C9 Fe1 C16 C12 -154.6(13) . . . . ? C7 Fe1 C16 C12 80.4(8) . . . . ? C10 Fe1 C16 C12 166.6(7) . . . . ? C11 Fe1 C16 C12 123.9(7) . . . . ? C14 Fe1 C16 C12 -81.3(8) . . . . ? C15 Fe1 C16 C12 -120.4(11) . . . . ? C13 Fe1 C16 C12 -38.1(7) . . . . ? O6 Ti1 C18 C19 2.0(13) . . . . ? C24 Ti1 C18 C19 -98.8(11) . . . . ? C22 Ti1 C18 C19 114.1(14) . . . . ? C26 Ti1 C18 C19 -125.2(10) . . . . ? C23 Ti1 C18 C19 -133.5(12) . . . . ? C25 Ti1 C18 C19 -89.9(11) . . . . ? C21 Ti1 C18 C19 75.1(11) . . . . ? C20 Ti1 C18 C19 36.2(10) . . . . ? Cl1 Ti1 C18 C19 124.9(11) . . . . ? C27 Ti1 C18 C19 -150.6(11) . . . . ? O6 Ti1 C18 C22 -112.1(11) . . . . ? C24 Ti1 C18 C22 147.1(11) . . . . ? C26 Ti1 C18 C22 120.7(10) . . . . ? C19 Ti1 C18 C22 -114.1(14) . . . . ? C23 Ti1 C18 C22 112.4(11) . . . . ? C25 Ti1 C18 C22 156.0(10) . . . . ? C21 Ti1 C18 C22 -38.9(9) . . . . ? C20 Ti1 C18 C22 -77.9(10) . . . . ? Cl1 Ti1 C18 C22 10.8(11) . . . . ? C27 Ti1 C18 C22 95.3(10) . . . . ? C22 C18 C19 C20 -4.5(14) . . . . ? Ti1 C18 C19 C20 -68.0(9) . . . . ? C22 C18 C19 Ti1 63.5(8) . . . . ? O6 Ti1 C19 C20 -63.3(10) . . . . ? C24 Ti1 C19 C20 -167.4(10) . . . . ? C22 Ti1 C19 C20 76.4(12) . . . . ? C26 Ti1 C19 C20 -153.8(9) . . . . ? C23 Ti1 C19 C20 160.4(10) . . . . ? C25 Ti1 C19 C20 -140.8(10) . . . . ? C21 Ti1 C19 C20 34.7(9) . . . . ? C18 Ti1 C19 C20 115.1(15) . . . . ? Cl1 Ti1 C19 C20 36.2(12) . . . . ? C27 Ti1 C19 C20 155.6(9) . . . . ? O6 Ti1 C19 C18 -178.4(11) . . . . ? C24 Ti1 C19 C18 77.5(11) . . . . ? C22 Ti1 C19 C18 -38.7(10) . . . . ? C26 Ti1 C19 C18 91.1(12) . . . . ? C23 Ti1 C19 C18 45.4(11) . . . . ? C25 Ti1 C19 C18 104.1(11) . . . . ? C21 Ti1 C19 C18 -80.3(11) . . . . ? C20 Ti1 C19 C18 -115.1(15) . . . . ? Cl1 Ti1 C19 C18 -78.9(12) . . . . ? C27 Ti1 C19 C18 40.5(14) . . . . ? C18 C19 C20 C21 3.1(16) . . . . ? Ti1 C19 C20 C21 -64.3(11) . . . . ? C18 C19 C20 Ti1 67.3(8) . . . . ? O6 Ti1 C20 C21 -127.6(10) . . . . ? C24 Ti1 C20 C21 133.1(10) . . . . ? C22 Ti1 C20 C21 37.6(9) . . . . ? C26 Ti1 C20 C21 -160.5(15) . . . . ? C19 Ti1 C20 C21 118.8(14) . . . . ? C23 Ti1 C20 C21 93.5(12) . . . . ? C25 Ti1 C20 C21 172.4(9) . . . . ? C18 Ti1 C20 C21 80.6(10) . . . . ? Cl1 Ti1 C20 C21 -34.7(10) . . . . ? C27 Ti1 C20 C21 62(2) . . . . ? O6 Ti1 C20 C19 113.6(11) . . . . ? C24 Ti1 C20 C19 14.3(12) . . . . ? C22 Ti1 C20 C19 -81.2(11) . . . . ? C26 Ti1 C20 C19 80.7(18) . . . . ? C23 Ti1 C20 C19 -25.3(13) . . . . ? C25 Ti1 C20 C19 53.6(12) . . . . ? C21 Ti1 C20 C19 -118.8(14) . . . . ? C18 Ti1 C20 C19 -38.2(9) . . . . ? Cl1 Ti1 C20 C19 -153.5(10) . . . . ? C27 Ti1 C20 C19 -57(2) . . . . ? C19 C20 C21 C22 -0.3(16) . . . . ? Ti1 C20 C21 C22 -63.7(9) . . . . ? C19 C20 C21 Ti1 63.5(10) . . . . ? O6 Ti1 C21 C20 51.1(10) . . . . ? C24 Ti1 C21 C20 -68.0(13) . . . . ? C22 Ti1 C21 C20 -116.6(13) . . . . ? C26 Ti1 C21 C20 162.5(13) . . . . ? C19 Ti1 C21 C20 -35.1(8) . . . . ? C23 Ti1 C21 C20 -110.8(10) . . . . ? C25 Ti1 C21 C20 -20(2) . . . . ? C18 Ti1 C21 C20 -76.7(10) . . . . ? Cl1 Ti1 C21 C20 146.0(10) . . . . ? C27 Ti1 C21 C20 -153.4(9) . . . . ? O6 Ti1 C21 C22 167.7(9) . . . . ? C24 Ti1 C21 C22 48.5(13) . . . . ? C26 Ti1 C21 C22 -80.9(18) . . . . ? C19 Ti1 C21 C22 81.5(10) . . . . ? C23 Ti1 C21 C22 5.7(12) . . . . ? C25 Ti1 C21 C22 96(2) . . . . ? C18 Ti1 C21 C22 39.9(9) . . . . ? C20 Ti1 C21 C22 116.6(13) . . . . ? Cl1 Ti1 C21 C22 -97.4(10) . . . . ? C27 Ti1 C21 C22 -36.8(12) . . . . ? C20 C21 C22 C18 -2.5(15) . . . . ? Ti1 C21 C22 C18 -68.1(9) . . . . ? C20 C21 C22 Ti1 65.5(10) . . . . ? C19 C18 C22 C21 4.2(13) . . . . ? Ti1 C18 C22 C21 68.2(8) . . . . ? C19 C18 C22 Ti1 -64.0(8) . . . . ? O6 Ti1 C22 C21 -16.1(12) . . . . ? C24 Ti1 C22 C21 -146.5(9) . . . . ? C26 Ti1 C22 C21 152.4(9) . . . . ? C19 Ti1 C22 C21 -74.2(10) . . . . ? C23 Ti1 C22 C21 -175.3(10) . . . . ? C25 Ti1 C22 C21 -151.2(10) . . . . ? C18 Ti1 C22 C21 -111.8(12) . . . . ? C20 Ti1 C22 C21 -35.1(9) . . . . ? Cl1 Ti1 C22 C21 77.7(9) . . . . ? C27 Ti1 C22 C21 153.8(9) . . . . ? O6 Ti1 C22 C18 95.6(12) . . . . ? C24 Ti1 C22 C18 -34.7(11) . . . . ? C26 Ti1 C22 C18 -95.8(9) . . . . ? C19 Ti1 C22 C18 37.6(8) . . . . ? C23 Ti1 C22 C18 -63.5(10) . . . . ? C25 Ti1 C22 C18 -39.4(13) . . . . ? C21 Ti1 C22 C18 111.8(12) . . . . ? C20 Ti1 C22 C18 76.7(9) . . . . ? Cl1 Ti1 C22 C18 -170.5(10) . . . . ? C27 Ti1 C22 C18 -94.4(9) . . . . ? O6 Ti1 C23 C24 -30.7(9) . . . . ? C22 Ti1 C23 C24 126.6(8) . . . . ? C26 Ti1 C23 C24 -77.9(7) . . . . ? C19 Ti1 C23 C24 70.4(8) . . . . ? C25 Ti1 C23 C24 -37.0(7) . . . . ? C21 Ti1 C23 C24 123.4(8) . . . . ? C18 Ti1 C23 C24 94.7(8) . . . . ? C20 Ti1 C23 C24 83.8(9) . . . . ? Cl1 Ti1 C23 C24 -148.5(6) . . . . ? C27 Ti1 C23 C24 -115.9(10) . . . . ? O6 Ti1 C23 C27 85.2(8) . . . . ? C24 Ti1 C23 C27 115.9(10) . . . . ? C22 Ti1 C23 C27 -117.5(8) . . . . ? C26 Ti1 C23 C27 38.0(6) . . . . ? C19 Ti1 C23 C27 -173.7(8) . . . . ? C25 Ti1 C23 C27 78.9(7) . . . . ? C21 Ti1 C23 C27 -120.7(8) . . . . ? C18 Ti1 C23 C27 -149.5(9) . . . . ? C20 Ti1 C23 C27 -160.4(8) . . . . ? Cl1 Ti1 C23 C27 -32.6(7) . . . . ? C27 C23 C24 C25 0.6(13) . . . . ? Ti1 C23 C24 C25 66.6(8) . . . . ? C27 C23 C24 Ti1 -66.0(8) . . . . ? O6 Ti1 C24 C23 158.2(6) . . . . ? C22 Ti1 C24 C23 -58.6(8) . . . . ? C26 Ti1 C24 C23 78.5(7) . . . . ? C19 Ti1 C24 C23 -111.4(8) . . . . ? C25 Ti1 C24 C23 116.5(10) . . . . ? C21 Ti1 C24 C23 -85.1(10) . . . . ? C18 Ti1 C24 C23 -77.9(8) . . . . ? C20 Ti1 C24 C23 -119.0(7) . . . . ? Cl1 Ti1 C24 C23 44.5(8) . . . . ? C27 Ti1 C24 C23 37.0(6) . . . . ? O6 Ti1 C24 C25 41.7(8) . . . . ? C22 Ti1 C24 C25 -175.2(7) . . . . ? C26 Ti1 C24 C25 -38.0(7) . . . . ? C19 Ti1 C24 C25 132.0(8) . . . . ? C23 Ti1 C24 C25 -116.5(10) . . . . ? C21 Ti1 C24 C25 158.3(9) . . . . ? C18 Ti1 C24 C25 165.6(8) . . . . ? C20 Ti1 C24 C25 124.5(8) . . . . ? Cl1 Ti1 C24 C25 -72.1(8) . . . . ? C27 Ti1 C24 C25 -79.6(7) . . . . ? C23 C24 C25 C26 -1.9(13) . . . . ? Ti1 C24 C25 C26 64.5(7) . . . . ? C23 C24 C25 Ti1 -66.3(8) . . . . ? O6 Ti1 C25 C26 107.5(7) . . . . ? C24 Ti1 C25 C26 -113.8(10) . . . . ? C22 Ti1 C25 C26 -106.0(9) . . . . ? C19 Ti1 C25 C26 -165.8(7) . . . . ? C23 Ti1 C25 C26 -77.1(8) . . . . ? C21 Ti1 C25 C26 -178.5(17) . . . . ? C18 Ti1 C25 C26 -129.4(8) . . . . ? C20 Ti1 C25 C26 167.2(7) . . . . ? Cl1 Ti1 C25 C26 16.7(8) . . . . ? C27 Ti1 C25 C26 -36.5(6) . . . . ? O6 Ti1 C25 C24 -138.8(7) . . . . ? C22 Ti1 C25 C24 7.8(11) . . . . ? C26 Ti1 C25 C24 113.8(10) . . . . ? C19 Ti1 C25 C24 -52.0(8) . . . . ? C23 Ti1 C25 C24 36.7(7) . . . . ? C21 Ti1 C25 C24 -65(2) . . . . ? C18 Ti1 C25 C24 -15.6(9) . . . . ? C20 Ti1 C25 C24 -79.1(9) . . . . ? Cl1 Ti1 C25 C24 130.4(6) . . . . ? C27 Ti1 C25 C24 77.3(7) . . . . ? C24 C25 C26 C27 2.5(12) . . . . ? Ti1 C25 C26 C27 66.1(8) . . . . ? C24 C25 C26 Ti1 -63.6(7) . . . . ? O6 Ti1 C26 C25 -68.9(7) . . . . ? C24 Ti1 C26 C25 38.6(7) . . . . ? C22 Ti1 C26 C25 119.8(10) . . . . ? C19 Ti1 C26 C25 22.2(11) . . . . ? C23 Ti1 C26 C25 80.0(8) . . . . ? C21 Ti1 C26 C25 178.6(15) . . . . ? C18 Ti1 C26 C25 70.4(10) . . . . ? C20 Ti1 C26 C25 -37(2) . . . . ? Cl1 Ti1 C26 C25 -165.1(7) . . . . ? C27 Ti1 C26 C25 117.5(10) . . . . ? O6 Ti1 C26 C27 173.6(7) . . . . ? C24 Ti1 C26 C27 -78.9(7) . . . . ? C22 Ti1 C26 C27 2.3(12) . . . . ? C19 Ti1 C26 C27 -95.3(10) . . . . ? C23 Ti1 C26 C27 -37.5(7) . . . . ? C25 Ti1 C26 C27 -117.5(10) . . . . ? C21 Ti1 C26 C27 61.1(18) . . . . ? C18 Ti1 C26 C27 -47.2(10) . . . . ? C20 Ti1 C26 C27 -154.4(17) . . . . ? Cl1 Ti1 C26 C27 77.4(6) . . . . ? C24 C23 C27 C26 0.9(12) . . . . ? Ti1 C23 C27 C26 -63.1(7) . . . . ? C24 C23 C27 Ti1 64.0(8) . . . . ? C25 C26 C27 C23 -2.1(12) . . . . ? Ti1 C26 C27 C23 63.5(7) . . . . ? C25 C26 C27 Ti1 -65.6(8) . . . . ? O6 Ti1 C27 C23 -122.4(7) . . . . ? C24 Ti1 C27 C23 -37.3(7) . . . . ? C22 Ti1 C27 C23 66.8(9) . . . . ? C26 Ti1 C27 C23 -114.8(10) . . . . ? C19 Ti1 C27 C23 8.6(11) . . . . ? C25 Ti1 C27 C23 -78.7(8) . . . . ? C21 Ti1 C27 C23 87.2(9) . . . . ? C18 Ti1 C27 C23 30.6(9) . . . . ? C20 Ti1 C27 C23 46.1(18) . . . . ? Cl1 Ti1 C27 C23 148.2(7) . . . . ? O6 Ti1 C27 C26 -7.7(8) . . . . ? C24 Ti1 C27 C26 77.5(7) . . . . ? C22 Ti1 C27 C26 -178.5(8) . . . . ? C19 Ti1 C27 C26 123.3(9) . . . . ? C23 Ti1 C27 C26 114.8(10) . . . . ? C25 Ti1 C27 C26 36.1(6) . . . . ? C21 Ti1 C27 C26 -158.1(7) . . . . ? C18 Ti1 C27 C26 145.4(8) . . . . ? C20 Ti1 C27 C26 160.9(15) . . . . ? Cl1 Ti1 C27 C26 -97.1(6) . . . . ?