data_global #============================================================================ data_publication_text _publ_requested_journal 'Organometallics' _publ_contact_author_name 'Dr. Gomez-Ruiz' _publ_contact_author_address ;Departamento de Biologia y Geologia, Fisica y Quimica Inorganica, E.S.C.E.T., Universidad Rey Juan Carlos, 28933 Mostoles, Madrid, Spain ; _publ_contact_author_email santiago.gomez@urjc.es _publ_contact_author_fax (+34)914888143 #============================================================================ # TITLE AND AUTHOR LIST _publ_section_title ; Ether-substituted group 4 metallocene complexes: cytostatic effects and applications in ethylene polymerization ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Ceballos-Torres, Jes\'us' ;Departamento de Biologia y Geologia, Fisica y Quimica Inorganica, E.S.C.E.T., Universidad Rey Juan Carlos, 28933 Mostoles, Madrid, Spain ; 'Prashar, Sanjiv' ;Departamento de Biologia y Geologia, Fisica y Quimica Inorganica, E.S.C.E.T., Universidad Rey Juan Carlos, 28933 Mostoles, Madrid, Spain ; 'Fajardo, Mariano' ;Departamento de Biologia y Geologia, Fisica y Quimica Inorganica, E.S.C.E.T., Universidad Rey Juan Carlos, 28933 Mostoles, Madrid, Spain ; 'Chicca, Andrea' ;Institute of Biochemistry and Molecular Medicine, NCCR TransCure, University of Bern, Bühlstrasse 28, CH-3012 Bern, Switzerland ; 'Gertsch, Juerg' ;Institute of Biochemistry and Molecular Medicine, NCCR TransCure, University of Bern, Bühlstrasse 28, CH-3012 Bern, Switzerland ; 'Pinar, Ana B.' ;Department of Materials, ETH Hönggerberg, Vladimir-Prelog-Weg 1-5, CH-8093 Zürich, Switzerland ; 'G\'omez-Ruiz, Santiago' ;Departamento de Biologia y Geologia, Fisica y Quimica Inorganica, E.S.C.E.T., Universidad Rey Juan Carlos, 28933 Mostoles, Madrid, Spain ; #============================================================================ data_s7b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H34 Cl2 O4 Zr' _chemical_formula_weight 524.61 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' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.577(5) _cell_length_b 6.6615(13) _cell_length_c 14.001(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.620(4) _cell_angle_gamma 90.00 _cell_volume 2377.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1159 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 20.89 _exptl_crystal_description 'Prismatic' _exptl_crystal_colour 'Yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Axs APEX automatic diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6807 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2424 _reflns_number_gt 1941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart' _computing_cell_refinement 'Bruker smart' _computing_data_reduction 'Bruker smart' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0667P)^2^+6.7380P] 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 2424 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 1.0000 0.11102(8) 0.7500 0.0174(2) Uani 1 2 d S . . Cl1 Cl 0.98032(5) -0.14483(19) 0.86878(9) 0.0359(3) Uani 1 1 d . . . C1 C 0.90508(15) 0.2352(6) 0.7682(3) 0.0183(9) Uani 1 1 d . . . C2 C 0.90258(16) 0.0949(6) 0.6916(3) 0.0197(9) Uani 1 1 d . . . H2 H 0.8857 -0.0288 0.6914 0.024 Uiso 1 1 calc R . . C3 C 0.92980(17) 0.1728(7) 0.6158(3) 0.0238(10) Uani 1 1 d . . . H3 H 0.9330 0.1120 0.5568 0.029 Uiso 1 1 calc R . . C4 C 0.95112(17) 0.3583(6) 0.6458(3) 0.0222(9) Uani 1 1 d . . . H4 H 0.9715 0.4417 0.6105 0.027 Uiso 1 1 calc R . . C5 C 0.93617(16) 0.3966(6) 0.7396(3) 0.0201(9) Uani 1 1 d . . . H5 H 0.9453 0.5095 0.7762 0.024 Uiso 1 1 calc R . . C6 C 0.87408(16) 0.2301(6) 0.8563(3) 0.0204(9) Uani 1 1 d . . . C7 C 0.90804(17) 0.3009(7) 0.9462(3) 0.0263(10) Uani 1 1 d . . . H7A H 0.8875 0.2988 1.0006 0.039 Uiso 1 1 d R . . H7B H 0.9201 0.4352 0.9361 0.039 Uiso 1 1 d R . . H7C H 0.9377 0.2132 0.9578 0.039 Uiso 1 1 d R . . C8 C 0.85028(18) 0.0239(7) 0.8707(3) 0.0275(10) Uani 1 1 d . . . H8A H 0.8246 -0.0047 0.8186 0.041 Uiso 1 1 d R . . H8B H 0.8338 0.0224 0.9299 0.041 Uiso 1 1 d R . . H8C H 0.8774 -0.0760 0.8727 0.041 Uiso 1 1 d R . . C9 C 0.82955(16) 0.3864(7) 0.8366(3) 0.0215(9) Uani 1 1 d . . . H9 H 0.8444 0.5220 0.8369 0.026 Uiso 1 1 calc R . . C10 C 0.75709(19) 0.5191(9) 0.9101(3) 0.0380(13) Uani 1 1 d . . . H10A H 0.7733 0.6488 0.9172 0.057 Uiso 1 1 d R . . H10B H 0.7353 0.4969 0.9618 0.057 Uiso 1 1 d R . . H10C H 0.7360 0.5135 0.8502 0.057 Uiso 1 1 d R . . C11 C 0.80430(18) 0.5015(8) 0.6769(3) 0.0327(11) Uani 1 1 d . . . H11A H 0.7939 0.6283 0.7018 0.049 Uiso 1 1 d R . . H11B H 0.7818 0.4685 0.6209 0.049 Uiso 1 1 d R . . H11C H 0.8399 0.5100 0.6603 0.049 Uiso 1 1 d R . . O1 O 0.79629(12) 0.3670(5) 0.9115(2) 0.0286(8) Uani 1 1 d . . . O2 O 0.80009(12) 0.3499(5) 0.7480(2) 0.0255(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0159(3) 0.0190(3) 0.0170(3) 0.000 0.0001(2) 0.000 Cl1 0.0375(7) 0.0398(8) 0.0306(6) 0.0003(5) 0.0028(5) 0.0001(5) C1 0.014(2) 0.023(2) 0.017(2) 0.0008(17) -0.0023(16) 0.0021(17) C2 0.017(2) 0.023(2) 0.019(2) -0.0018(17) -0.0032(16) 0.0000(17) C3 0.023(2) 0.035(3) 0.013(2) -0.0025(18) 0.0017(17) 0.007(2) C4 0.017(2) 0.027(3) 0.022(2) 0.0052(18) 0.0002(17) 0.0028(18) C5 0.017(2) 0.022(2) 0.020(2) -0.0024(17) -0.0010(16) 0.0015(18) C6 0.018(2) 0.026(2) 0.017(2) -0.0006(17) 0.0009(17) -0.0011(18) C7 0.024(2) 0.036(3) 0.019(2) -0.0038(19) 0.0008(18) 0.006(2) C8 0.025(2) 0.030(3) 0.028(2) 0.003(2) 0.0082(19) -0.001(2) C9 0.019(2) 0.031(2) 0.015(2) -0.0038(18) 0.0021(16) 0.0020(18) C10 0.030(3) 0.055(3) 0.030(3) -0.005(2) 0.006(2) 0.021(3) C11 0.025(2) 0.050(3) 0.022(2) 0.004(2) -0.0046(19) 0.006(2) O1 0.0221(16) 0.042(2) 0.0219(16) 0.0018(14) 0.0035(13) 0.0079(14) O2 0.0203(16) 0.0356(19) 0.0198(16) 0.0001(13) -0.0019(12) 0.0008(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 Cl1 2.4615(14) 2_756 ? Zr1 Cl1 2.4615(14) . ? Zr1 C4 2.472(4) 2_756 ? Zr1 C4 2.472(4) . ? Zr1 C5 2.503(4) 2_756 ? Zr1 C5 2.503(4) . ? Zr1 C3 2.526(4) 2_756 ? Zr1 C3 2.526(4) . ? Zr1 C2 2.561(4) 2_756 ? Zr1 C2 2.561(4) . ? Zr1 C1 2.597(4) 2_756 ? Zr1 C1 2.597(4) . ? C1 C5 1.414(6) . ? C1 C2 1.420(6) . ? C1 C6 1.520(6) . ? C2 C3 1.414(6) . ? C3 C4 1.402(6) . ? C4 C5 1.419(6) . ? C6 C8 1.523(6) . ? C6 C7 1.545(6) . ? C6 C9 1.551(6) . ? C9 O1 1.408(5) . ? C9 O2 1.420(5) . ? C10 O1 1.424(5) . ? C11 O2 1.428(6) . ? 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 Cl1 Zr1 Cl1 92.36(6) 2_756 . ? Cl1 Zr1 C4 137.63(11) 2_756 2_756 ? Cl1 Zr1 C4 100.61(11) . 2_756 ? Cl1 Zr1 C4 100.61(11) 2_756 . ? Cl1 Zr1 C4 137.63(11) . . ? C4 Zr1 C4 96.4(2) 2_756 . ? Cl1 Zr1 C5 113.43(10) 2_756 2_756 ? Cl1 Zr1 C5 130.89(10) . 2_756 ? C4 Zr1 C5 33.14(14) 2_756 2_756 ? C4 Zr1 C5 79.89(14) . 2_756 ? Cl1 Zr1 C5 130.89(10) 2_756 . ? Cl1 Zr1 C5 113.43(10) . . ? C4 Zr1 C5 79.89(14) 2_756 . ? C4 Zr1 C5 33.14(14) . . ? C5 Zr1 C5 81.1(2) 2_756 . ? Cl1 Zr1 C3 116.33(11) 2_756 2_756 ? Cl1 Zr1 C3 77.41(10) . 2_756 ? C4 Zr1 C3 32.55(14) 2_756 2_756 ? C4 Zr1 C3 128.74(16) . 2_756 ? C5 Zr1 C3 53.96(14) 2_756 2_756 ? C5 Zr1 C3 109.92(15) . 2_756 ? Cl1 Zr1 C3 77.41(10) 2_756 . ? Cl1 Zr1 C3 116.33(11) . . ? C4 Zr1 C3 128.74(15) 2_756 . ? C4 Zr1 C3 32.55(14) . . ? C5 Zr1 C3 109.92(14) 2_756 . ? C5 Zr1 C3 53.96(14) . . ? C3 Zr1 C3 161.2(2) 2_756 . ? Cl1 Zr1 C2 86.55(10) 2_756 2_756 ? Cl1 Zr1 C2 90.11(10) . 2_756 ? C4 Zr1 C2 53.62(14) 2_756 2_756 ? C4 Zr1 C2 130.47(14) . 2_756 ? C5 Zr1 C2 53.14(14) 2_756 2_756 ? C5 Zr1 C2 131.58(14) . 2_756 ? C3 Zr1 C2 32.27(13) 2_756 2_756 ? C3 Zr1 C2 149.23(13) . 2_756 ? Cl1 Zr1 C2 90.11(10) 2_756 . ? Cl1 Zr1 C2 86.55(10) . . ? C4 Zr1 C2 130.47(14) 2_756 . ? C4 Zr1 C2 53.62(14) . . ? C5 Zr1 C2 131.58(14) 2_756 . ? C5 Zr1 C2 53.14(14) . . ? C3 Zr1 C2 149.23(13) 2_756 . ? C3 Zr1 C2 32.27(13) . . ? C2 Zr1 C2 175.19(19) 2_756 . ? Cl1 Zr1 C1 84.88(9) 2_756 2_756 ? Cl1 Zr1 C1 122.04(9) . 2_756 ? C4 Zr1 C1 54.06(13) 2_756 2_756 ? C4 Zr1 C1 99.34(14) . 2_756 ? C5 Zr1 C1 32.13(13) 2_756 2_756 ? C5 Zr1 C1 111.26(14) . 2_756 ? C3 Zr1 C1 53.61(13) 2_756 2_756 ? C3 Zr1 C1 119.31(14) . 2_756 ? C2 Zr1 C1 31.94(13) 2_756 2_756 ? C2 Zr1 C1 151.08(13) . 2_756 ? Cl1 Zr1 C1 122.04(9) 2_756 . ? Cl1 Zr1 C1 84.88(10) . . ? C4 Zr1 C1 99.34(14) 2_756 . ? C4 Zr1 C1 54.06(13) . . ? C5 Zr1 C1 111.26(14) 2_756 . ? C5 Zr1 C1 32.13(13) . . ? C3 Zr1 C1 119.31(13) 2_756 . ? C3 Zr1 C1 53.61(13) . . ? C2 Zr1 C1 151.08(13) 2_756 . ? C2 Zr1 C1 31.94(13) . . ? C1 Zr1 C1 142.84(18) 2_756 . ? C5 C1 C2 106.2(4) . . ? C5 C1 C6 126.1(4) . . ? C2 C1 C6 127.1(4) . . ? C5 C1 Zr1 70.3(2) . . ? C2 C1 Zr1 72.7(2) . . ? C6 C1 Zr1 128.7(3) . . ? C3 C2 C1 109.3(4) . . ? C3 C2 Zr1 72.5(2) . . ? C1 C2 Zr1 75.4(2) . . ? C4 C3 C2 107.6(4) . . ? C4 C3 Zr1 71.6(2) . . ? C2 C3 Zr1 75.2(2) . . ? C3 C4 C5 108.0(4) . . ? C3 C4 Zr1 75.8(2) . . ? C5 C4 Zr1 74.6(2) . . ? C1 C5 C4 109.0(4) . . ? C1 C5 Zr1 77.6(2) . . ? C4 C5 Zr1 72.2(2) . . ? C1 C6 C8 111.6(3) . . ? C1 C6 C7 111.1(3) . . ? C8 C6 C7 111.8(4) . . ? C1 C6 C9 105.3(3) . . ? C8 C6 C9 109.5(4) . . ? C7 C6 C9 107.2(3) . . ? O1 C9 O2 109.0(3) . . ? O1 C9 C6 106.6(3) . . ? O2 C9 C6 111.7(3) . . ? C9 O1 C10 113.1(3) . . ? C9 O2 C11 115.1(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.677 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.118 #============================================================================ data_p21n _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H15 Cl O2 Ti' _chemical_formula_weight 298.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ti' 'Ti' 0.2776 0.4457 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 1 21 /n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.5000(2) _cell_length_b 14.8600(5) _cell_length_c 13.9790(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.328(4) _cell_angle_gamma 90.00 _cell_volume 1323.93(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8245 _cell_measurement_theta_min 2.0173 _cell_measurement_theta_max 29.662 _exptl_crystal_description 'cubic shaped crystals' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET) (compiled Nov 29 2007,17:23:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.97588 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur, Onyx' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.1188 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74651 _diffrn_reflns_av_R_equivalents 0.1265 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2711 _reflns_number_gt 1604 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET) (compiled Nov 29 2007,17:23:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET) (compiled Nov 29 2007,17:23:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET) (compiled Nov 29 2007,17:23:28) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0939P)^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_number_reflns 2711 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1343 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.08695(10) 1.04593(4) 0.73403(4) 0.0470(3) Uani 1 1 d . . . Cl1 Cl -0.21199(17) 1.05436(9) 0.60694(7) 0.0800(4) Uani 1 1 d . . . O1 O -0.0674(4) 1.03353(15) 0.83986(17) 0.0558(6) Uani 1 1 d . . . O2 O -0.2307(4) 1.0785(2) 0.95505(19) 0.0696(8) Uani 1 1 d . . . C1 C 0.1403(6) 1.1796(2) 0.8289(3) 0.0528(9) Uani 1 1 d . . . C2 C 0.3359(6) 1.1454(2) 0.8182(3) 0.0626(10) Uani 1 1 d . . . H2 H 0.4526 1.1296 0.8714 0.088(14) Uiso 1 1 calc R . . C3 C 0.3455(7) 1.1521(3) 0.7179(4) 0.0757(13) Uani 1 1 d . . . H3 H 0.4700 1.1403 0.6901 0.091(14) Uiso 1 1 calc R . . C4 C 0.1596(8) 1.1869(3) 0.6681(3) 0.0717(12) Uani 1 1 d . . . H4 H 0.1283 1.2036 0.5989 0.103(16) Uiso 1 1 calc R . . C5 C 0.0327(7) 1.2035(2) 0.7354(3) 0.0623(10) Uani 1 1 d . . . H5 H -0.1045 1.2333 0.7208 0.067(11) Uiso 1 1 calc R . . C6 C 0.3907(7) 0.9532(3) 0.7618(3) 0.0693(12) Uani 1 1 d . . . H6 H 0.5332 0.9721 0.7918 0.113(18) Uiso 1 1 calc R . . C7 C 0.2438(8) 0.9143(3) 0.8100(3) 0.0732(13) Uani 1 1 d . . . H7 H 0.2661 0.9008 0.8799 0.111(17) Uiso 1 1 calc R . . C8 C 0.0708(7) 0.8862(3) 0.7387(3) 0.0700(11) Uani 1 1 d . . . H8 H -0.0483 0.8502 0.7503 0.126(19) Uiso 1 1 calc R . . C9 C 0.1135(7) 0.9090(3) 0.6487(3) 0.0726(11) Uani 1 1 d . . . H9 H 0.0268 0.8927 0.5855 0.080(12) Uiso 1 1 calc R . . C10 C 0.3055(7) 0.9511(3) 0.6616(3) 0.0695(12) Uani 1 1 d . . . H10 H 0.3788 0.9684 0.6094 0.095(15) Uiso 1 1 calc R . . C11 C 0.0441(6) 1.1745(2) 0.9185(3) 0.0562(9) Uani 1 1 d . . . C12 C -0.0989(5) 1.0915(3) 0.9060(2) 0.0514(9) Uani 1 1 d . . . C13 C 0.2110(9) 1.1591(4) 1.0113(3) 0.0987(18) Uani 1 1 d . . . H13A H 0.3103 1.2077 1.0193 0.14(2) Uiso 1 1 calc R . . H13B H 0.2825 1.1034 1.0057 0.15(3) Uiso 1 1 calc R . . H13C H 0.1446 1.1566 1.0668 0.097(16) Uiso 1 1 calc R . . C14 C -0.0885(11) 1.2568(3) 0.9283(5) 0.0997(19) Uani 1 1 d . . . H14A H -0.1466 1.2514 0.9861 0.070(12) Uiso 1 1 calc R . . H14B H -0.2001 1.2612 0.8722 0.17(3) Uiso 1 1 calc R . . H14C H -0.0026 1.3097 0.9328 0.093(15) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0451(4) 0.0504(4) 0.0470(4) 0.0002(3) 0.0127(3) -0.0018(3) Cl1 0.0563(6) 0.1266(10) 0.0542(6) -0.0028(6) 0.0037(5) 0.0067(6) O1 0.0605(16) 0.0601(15) 0.0488(14) -0.0046(11) 0.0158(12) -0.0118(12) O2 0.0591(17) 0.097(2) 0.0592(16) 0.0001(14) 0.0267(14) -0.0016(15) C1 0.056(2) 0.0391(18) 0.064(2) -0.0007(16) 0.0153(18) -0.0022(16) C2 0.050(2) 0.055(2) 0.081(3) -0.0110(19) 0.010(2) -0.0114(18) C3 0.076(3) 0.059(2) 0.108(4) -0.017(2) 0.055(3) -0.022(2) C4 0.092(3) 0.058(2) 0.074(3) 0.014(2) 0.039(3) -0.002(2) C5 0.075(3) 0.051(2) 0.063(3) 0.0112(17) 0.020(2) 0.0081(19) C6 0.058(3) 0.056(2) 0.091(3) -0.006(2) 0.009(2) 0.0131(19) C7 0.106(4) 0.053(2) 0.060(3) 0.0042(19) 0.015(3) 0.024(2) C8 0.085(3) 0.051(2) 0.079(3) -0.0048(19) 0.027(3) -0.012(2) C9 0.086(3) 0.061(2) 0.069(3) -0.022(2) 0.008(2) -0.004(2) C10 0.080(3) 0.062(2) 0.073(3) -0.012(2) 0.031(2) 0.011(2) C11 0.059(2) 0.058(2) 0.053(2) -0.0005(16) 0.0163(18) 0.0005(17) C12 0.045(2) 0.065(2) 0.0416(18) 0.0050(16) 0.0032(16) 0.0059(17) C13 0.100(4) 0.132(5) 0.057(3) -0.006(3) 0.000(3) -0.051(4) C14 0.143(5) 0.062(3) 0.118(5) -0.003(2) 0.085(5) 0.013(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.953(2) . ? Ti1 C2 2.333(4) . ? Ti1 C3 2.348(4) . ? Ti1 C7 2.360(4) . ? Ti1 Cl1 2.3646(12) . ? Ti1 C10 2.365(4) . ? Ti1 C5 2.369(4) . ? Ti1 C4 2.374(4) . ? Ti1 C6 2.376(4) . ? Ti1 C1 2.376(3) . ? Ti1 C8 2.378(4) . ? Ti1 C9 2.382(4) . ? O1 C12 1.309(4) . ? O2 C12 1.213(4) . ? C1 C5 1.402(5) . ? C1 C2 1.405(5) . ? C1 C11 1.507(5) . ? C2 C3 1.419(6) . ? C3 C4 1.372(7) . ? C4 C5 1.390(5) . ? C6 C7 1.397(6) . ? C6 C10 1.402(6) . ? C7 C8 1.412(6) . ? C8 C9 1.383(6) . ? C9 C10 1.376(6) . ? C11 C14 1.517(6) . ? C11 C12 1.534(5) . ? C11 C13 1.536(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 C2 94.95(13) . . ? O1 Ti1 C3 128.33(13) . . ? C2 Ti1 C3 35.30(15) . . ? O1 Ti1 C7 79.73(13) . . ? C2 Ti1 C7 95.88(16) . . ? C3 Ti1 C7 110.23(19) . . ? O1 Ti1 Cl1 96.05(8) . . ? C2 Ti1 Cl1 137.04(11) . . ? C3 Ti1 Cl1 112.98(14) . . ? C7 Ti1 Cl1 126.93(12) . . ? O1 Ti1 C10 135.21(13) . . ? C2 Ti1 C10 100.25(16) . . ? C3 Ti1 C10 81.81(16) . . ? C7 Ti1 C10 57.07(16) . . ? Cl1 Ti1 C10 100.59(12) . . ? O1 Ti1 C5 89.29(12) . . ? C2 Ti1 C5 57.26(14) . . ? C3 Ti1 C5 56.43(15) . . ? C7 Ti1 C5 150.19(15) . . ? Cl1 Ti1 C5 81.48(11) . . ? C10 Ti1 C5 134.04(15) . . ? O1 Ti1 C4 123.27(12) . . ? C2 Ti1 C4 57.68(16) . . ? C3 Ti1 C4 33.79(16) . . ? C7 Ti1 C4 143.63(19) . . ? Cl1 Ti1 C4 81.85(13) . . ? C10 Ti1 C4 100.21(15) . . ? C5 Ti1 C4 34.08(13) . . ? O1 Ti1 C6 110.84(14) . . ? C2 Ti1 C6 79.24(15) . . ? C3 Ti1 C6 79.51(17) . . ? C7 Ti1 C6 34.32(14) . . ? Cl1 Ti1 C6 133.40(11) . . ? C10 Ti1 C6 34.39(15) . . ? C5 Ti1 C6 133.81(16) . . ? C4 Ti1 C6 110.67(17) . . ? O1 Ti1 C1 72.32(11) . . ? C2 Ti1 C1 34.69(13) . . ? C3 Ti1 C1 57.53(13) . . ? C7 Ti1 C1 116.03(14) . . ? Cl1 Ti1 C1 112.54(10) . . ? C10 Ti1 C1 134.67(15) . . ? C5 Ti1 C1 34.38(13) . . ? C4 Ti1 C1 57.35(14) . . ? C6 Ti1 C1 111.61(14) . . ? O1 Ti1 C8 81.55(12) . . ? C2 Ti1 C8 130.46(16) . . ? C3 Ti1 C8 135.22(16) . . ? C7 Ti1 C8 34.69(15) . . ? Cl1 Ti1 C8 92.25(12) . . ? C10 Ti1 C8 56.68(15) . . ? C5 Ti1 C8 168.33(16) . . ? C4 Ti1 C8 154.85(14) . . ? C6 Ti1 C8 57.07(15) . . ? C1 Ti1 C8 145.27(13) . . ? O1 Ti1 C9 113.42(13) . . ? C2 Ti1 C9 133.05(15) . . ? C3 Ti1 C9 113.72(16) . . ? C7 Ti1 C9 56.64(15) . . ? Cl1 Ti1 C9 78.39(12) . . ? C10 Ti1 C9 33.70(15) . . ? C5 Ti1 C9 150.93(15) . . ? C4 Ti1 C9 121.33(16) . . ? C6 Ti1 C9 56.41(15) . . ? C1 Ti1 C9 167.63(15) . . ? C8 Ti1 C9 33.78(13) . . ? C12 O1 Ti1 130.4(2) . . ? C5 C1 C2 106.8(3) . . ? C5 C1 C11 125.1(3) . . ? C2 C1 C11 127.0(3) . . ? C5 C1 Ti1 72.5(2) . . ? C2 C1 Ti1 71.0(2) . . ? C11 C1 Ti1 112.5(2) . . ? C1 C2 C3 107.2(4) . . ? C1 C2 Ti1 74.4(2) . . ? C3 C2 Ti1 72.9(2) . . ? C4 C3 C2 108.8(4) . . ? C4 C3 Ti1 74.1(2) . . ? C2 C3 Ti1 71.8(2) . . ? C3 C4 C5 107.7(4) . . ? C3 C4 Ti1 72.1(2) . . ? C5 C4 Ti1 72.8(2) . . ? C4 C5 C1 109.4(4) . . ? C4 C5 Ti1 73.1(2) . . ? C1 C5 Ti1 73.1(2) . . ? C7 C6 C10 107.5(4) . . ? C7 C6 Ti1 72.2(2) . . ? C10 C6 Ti1 72.4(2) . . ? C6 C7 C8 107.8(4) . . ? C6 C7 Ti1 73.5(2) . . ? C8 C7 Ti1 73.4(2) . . ? C9 C8 C7 107.2(4) . . ? C9 C8 Ti1 73.3(2) . . ? C7 C8 Ti1 72.0(2) . . ? C10 C9 C8 109.4(4) . . ? C10 C9 Ti1 72.5(2) . . ? C8 C9 Ti1 72.9(2) . . ? C9 C10 C6 108.1(4) . . ? C9 C10 Ti1 73.8(2) . . ? C6 C10 Ti1 73.2(2) . . ? C1 C11 C14 111.7(3) . . ? C1 C11 C12 106.7(3) . . ? C14 C11 C12 108.4(4) . . ? C1 C11 C13 111.7(4) . . ? C14 C11 C13 111.3(4) . . ? C12 C11 C13 106.7(3) . . ? O2 C12 O1 121.4(3) . . ? O2 C12 C11 122.9(3) . . ? O1 C12 C11 115.7(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.845 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.076 #============================================================================