#------------------------------------------------------------------------------ #$Date: 2019-10-28 07:23:29 +0000 (Mon, 28 Oct 2019) $ #$Revision: 219800 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/49/2104982.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2104982 loop_ _publ_author_name 'Cole, Jacqueline M.' 'Chan, Michael C. W.' 'Gibson, Vernon C.' 'Howard, Judith A. K.' _publ_section_title ; Effects of the [OC~6~F~5~] moiety upon structural geometry: crystal structures of half-sandwich tantalum(V) aryloxide complexes from reaction of Cp*Ta(N^t^Bu)(CH~2~R)~2~ with pentafluorophenol ; _journal_coeditor_code ZB5019 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 416 _journal_page_last 424 _journal_paper_doi 10.1107/S0108768111029259 _journal_volume 67 _journal_year 2011 _chemical_formula_structural '[(C6F5.O).(C6H5.CH2).(Cp*).Ta.O]2' _chemical_formula_sum 'C46 H44 F10 O4 Ta2' _chemical_formula_weight 1212.72 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 117.25(3) _cell_angle_beta 96.37(3) _cell_angle_gamma 106.63(3) _cell_formula_units_Z 1 _cell_length_a 9.239(2) _cell_length_b 11.647(2) _cell_length_c 11.803(2) _cell_measurement_reflns_used 50 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 12.271 _cell_measurement_theta_min 4.744 _cell_volume 1037.3(6) _computing_cell_refinement 'Siemens XSCANS' _computing_data_collection 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material SHELXL-93 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.9093 _diffrn_measured_fraction_theta_max 0.9093 _diffrn_measurement_device 'Siemens P4 diffractometer' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1448 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 3942 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.05 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.360 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.261 _exptl_absorpt_correction_type empirical _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.941 _exptl_crystal_description 'irregular block' _exptl_crystal_F_000 588 _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.64 _exptl_crystal_size_min 0.44 _refine_diff_density_max 5.300 _refine_diff_density_min -3.767 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 221 _refine_ls_number_reflns 3309 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_restrained_S_obs 1.049 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0727 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1572P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1890 _refine_ls_wR_factor_ref 0.1824 _reflns_number_gt 2985 _reflns_number_total 3310 _reflns_threshold_expression >2sigma(I) _cod_data_source_file zb5019.cif _cod_data_source_block final _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.1572P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.1572P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 2019-10-16 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_formula_sum 'C23 H22 F5 O2 Ta' _cod_original_formula_weight 606.36 _cod_original_formula_units_Z 2 _cod_original_cell_volume 1037.3(3) _cod_original_sg_symbol_Hall p_1 _cod_original_sg_symbol_H-M P-1 _cod_database_code 2104982 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.0252(3) 0.0181(4) 0.0243(3) 0.0069(2) 0.0030(2) 0.0122(2) F2 0.038(4) 0.043(5) 0.048(4) 0.015(4) 0.012(3) 0.024(4) F3 0.066(5) 0.055(6) 0.042(4) 0.026(4) 0.029(4) 0.022(4) F4 0.071(6) 0.042(5) 0.033(4) 0.011(4) 0.002(4) 0.023(4) F5 0.044(4) 0.042(5) 0.050(4) 0.016(4) -0.003(4) 0.024(4) F6 0.036(4) 0.033(4) 0.034(4) 0.011(3) 0.008(3) 0.015(3) O1 0.035(4) 0.021(4) 0.032(4) 0.006(4) 0.000(3) 0.013(4) O2 0.033(4) 0.020(4) 0.027(4) 0.007(3) 0.004(3) 0.017(3) C1 0.048(7) 0.009(6) 0.025(5) 0.003(5) 0.002(5) 0.009(5) C2 0.035(7) 0.024(7) 0.043(7) 0.005(5) 0.007(5) 0.010(6) C3 0.056(8) 0.032(8) 0.036(7) 0.003(6) 0.011(6) 0.020(6) C4 0.059(9) 0.035(8) 0.026(6) 0.003(7) -0.001(6) 0.020(6) C5 0.039(6) 0.029(7) 0.038(6) 0.008(5) 0.003(5) 0.020(6) C6 0.039(6) 0.017(6) 0.026(5) 0.004(5) 0.001(5) 0.012(5) C7 0.033(6) 0.034(7) 0.030(6) 0.010(5) 0.004(4) 0.020(5) C8 0.033(6) 0.023(6) 0.029(5) 0.013(5) 0.005(4) 0.012(5) C9 0.040(6) 0.025(7) 0.040(6) 0.013(5) 0.014(5) 0.022(6) C10 0.038(7) 0.069(11) 0.051(8) 0.022(7) 0.016(6) 0.043(8) C11 0.040(7) 0.061(10) 0.033(6) 0.027(7) 0.012(5) 0.024(7) C12 0.034(6) 0.042(8) 0.038(6) 0.016(6) 0.012(5) 0.018(6) C13 0.033(6) 0.036(8) 0.038(6) 0.015(6) 0.009(5) 0.022(6) loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy Ta Ta 0.07331(4) 0.14666(4) 0.02121(3) 0.0227(3) Uani d . 1 F F2 0.0398(9) 0.3517(9) 0.3795(7) 0.043(2) Uani d . 1 F F3 0.1504(11) 0.4073(10) 0.6275(8) 0.053(2) Uani d . 1 F F4 0.4415(11) 0.4098(9) 0.7073(7) 0.051(2) Uani d . 1 F F5 0.6121(9) 0.3448(9) 0.5299(8) 0.047(2) Uani d . 1 F F6 0.5032(8) 0.2935(8) 0.2836(7) 0.037(2) Uani d . 1 O O1 0.2143(10) 0.2989(9) 0.2031(8) 0.031(2) Uani d . 1 O O2 0.0221(9) 0.0498(8) 0.1188(7) 0.026(2) Uani d . 1 C C1 0.2678(15) 0.3175(12) 0.3217(10) 0.029(3) Uani d . 1 C C2 0.1807(15) 0.3467(15) 0.4138(14) 0.039(3) Uani d . 1 C C3 0.2366(17) 0.3758(15) 0.5418(13) 0.044(4) Uani d . 1 C C4 0.3809(18) 0.3750(16) 0.5798(12) 0.043(4) Uani d . 1 C C5 0.4719(16) 0.3455(14) 0.4918(12) 0.036(3) Uani d . 1 C C6 0.4124(14) 0.3173(13) 0.3641(11) 0.029(3) Uani d . 1 C C7 0.2984(14) 0.1553(14) -0.0272(11) 0.032(3) Uani d . 1 H H7A 0.3681 0.2554 0.0214 0.039 Uiso calc . 1 H H7B 0.3445 0.1119 0.0144 0.039 Uiso calc . 1 C C8 0.3170(14) 0.0951(13) -0.1647(11) 0.029(3) Uani d . 1 C C9 0.4144(15) 0.1776(14) -0.2021(12) 0.032(3) Uani d . 1 H H9A 0.4747(15) 0.2744(14) -0.1376(12) 0.039 Uiso d R 1 C C10 0.4270(16) 0.1223(18) -0.3333(14) 0.047(4) Uani d . 1 H H10A 0.4942(16) 0.1819(18) -0.3574(14) 0.056 Uiso d R 1 C C11 0.3455(16) -0.0128(17) -0.4242(12) 0.043(3) Uani d . 1 H H11A 0.3518(16) -0.0497(17) -0.5140(12) 0.051 Uiso d R 1 C C12 0.2506(15) -0.0997(16) -0.3875(12) 0.039(3) Uani d . 1 H H12A 0.1947(15) -0.1971(16) -0.4522(12) 0.046 Uiso d R 1 C C13 0.2365(14) -0.0487(14) -0.2611(12) 0.034(3) Uani d . 1 H H13A 0.1720(14) -0.1104(14) -0.2377(12) 0.040 Uiso d R 1 C C14 0.1002(15) 0.3316(15) -0.0438(12) 0.0361(9) Uiso d . 1 C C15 -0.0041(15) 0.1989(15) -0.1569(12) 0.0361(9) Uiso d . 1 C C16 -0.1400(15) 0.1532(15) -0.1155(12) 0.0361(9) Uiso d . 1 C C17 -0.1136(15) 0.2512(14) 0.0187(12) 0.0361(9) Uiso d . 1 C C18 0.0309(15) 0.3613(15) 0.0610(12) 0.0361(9) Uiso d . 1 C C14A 0.2501(14) 0.4282(14) -0.0396(12) 0.0361(9) Uiso d . 1 H H14A 0.2266(14) 0.4868(14) -0.0693(12) 0.043 Uiso d R 1 H H14B 0.3182(14) 0.4852(14) 0.0497(12) 0.043 Uiso d R 1 H H14C 0.3015(14) 0.3750(14) -0.0968(12) 0.043 Uiso d R 1 C C15A 0.0125(15) 0.1263(15) -0.2925(12) 0.0361(9) Uiso d . 1 H H15A -0.0240(15) 0.1627(15) -0.3432(12) 0.043 Uiso d R 1 H H15B 0.1212(15) 0.1407(15) -0.2872(12) 0.043 Uiso d R 1 H H15C -0.0491(15) 0.0281(15) -0.3350(12) 0.043 Uiso d R 1 C C16A -0.2844(15) 0.0233(15) -0.2066(12) 0.0361(9) Uiso d . 1 H H16A -0.3553(15) 0.0450(15) -0.2521(12) 0.043 Uiso d R 1 H H16B -0.2544(15) -0.0467(15) -0.2704(12) 0.043 Uiso d R 1 H H16C -0.3356(15) -0.0111(15) -0.1557(12) 0.043 Uiso d R 1 C C17A -0.2362(15) 0.2485(15) 0.0926(12) 0.0361(9) Uiso d . 1 H H17A -0.2988(15) 0.2964(15) 0.0784(12) 0.043 Uiso d R 1 H H17B -0.3029(15) 0.1535(15) 0.0606(12) 0.043 Uiso d R 1 H H17C -0.1852(15) 0.2943(15) 0.1858(12) 0.043 Uiso d R 1 C C18A 0.1005(15) 0.4993(14) 0.1920(12) 0.0361(9) Uiso d . 1 H H18A 0.0674(15) 0.5666(14) 0.1834(12) 0.043 Uiso d R 1 H H18B 0.0650(15) 0.4869(14) 0.2605(12) 0.043 Uiso d R 1 H H18C 0.2133(15) 0.5318(14) 0.2147(12) 0.043 Uiso d R 1 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O2 Ta O2 2 . 76.7(3) O2 Ta O1 2 . 150.8(4) O2 Ta O1 . . 80.7(3) O2 Ta C7 2 . 89.1(4) O2 Ta C7 . . 113.4(4) O1 Ta C7 . . 83.2(4) O2 Ta C17 2 . 108.4(4) O2 Ta C17 . . 107.7(4) O1 Ta C17 . . 95.9(4) C7 Ta C17 . . 138.1(5) O2 Ta C16 2 . 80.3(4) O2 Ta C16 . . 119.3(4) O1 Ta C16 . . 127.5(4) C7 Ta C16 . . 121.5(4) C17 Ta C16 . . 33.7(4) O2 Ta C18 2 . 135.0(4) O2 Ta C18 . . 126.5(4) O1 Ta C18 . . 73.8(4) C7 Ta C18 . . 109.3(5) C17 Ta C18 . . 33.4(4) C16 Ta C18 . . 54.9(4) O2 Ta C15 2 . 86.3(4) O2 Ta C15 . . 151.5(4) O1 Ta C15 . . 121.5(4) C7 Ta C15 . . 88.7(4) C17 Ta C15 . . 56.1(4) C16 Ta C15 . . 33.7(4) C18 Ta C15 . . 54.8(4) O2 Ta C14 2 . 118.5(4) O2 Ta C14 . . 158.8(4) O1 Ta C14 . . 88.6(4) C7 Ta C14 . . 83.2(5) C17 Ta C14 . . 54.9(4) C16 Ta C14 . . 54.7(4) C18 Ta C14 . . 32.3(4) C15 Ta C14 . . 32.9(4) O2 Ta Ta 2 2 38.4(2) O2 Ta Ta . 2 38.3(2) O1 Ta Ta . 2 116.9(3) C7 Ta Ta . 2 104.1(4) C17 Ta Ta . 2 113.3(3) C16 Ta Ta . 2 101.8(3) C18 Ta Ta . 2 146.0(3) C15 Ta Ta . 2 121.3(3) C14 Ta Ta . 2 154.0(3) C1 O1 Ta . . 139.8(8) Ta O2 Ta 2 . 103.3(3) O1 C1 C6 . . 123.0(12) O1 C1 C2 . . 120.4(12) C6 C1 C2 . . 116.4(11) F2 C2 C3 . . 118.3(13) F2 C2 C1 . . 119.3(12) C3 C2 C1 . . 122.4(13) F3 C3 C4 . . 120.8(12) F3 C3 C2 . . 119.9(14) C4 C3 C2 . . 119.3(13) C3 C4 F4 . . 120.2(14) C3 C4 C5 . . 120.7(12) F4 C4 C5 . . 118.9(14) F5 C5 C4 . . 120.2(12) F5 C5 C6 . . 121.3(12) C4 C5 C6 . . 118.5(13) F6 C6 C1 . . 120.0(10) F6 C6 C5 . . 117.3(11) C1 C6 C5 . . 122.7(12) C8 C7 Ta . . 125.2(8) C8 C7 H7A . . 106.0(10) Ta C7 H7A . . 106.0(9) C8 C7 H7B . . 106.0(12) Ta C7 H7B . . 106.0(8) H7A C7 H7B . . 106.3(10) C9 C8 C13 . . 117.4(11) C9 C8 C7 . . 121.2(11) C13 C8 C7 . . 121.3(11) C8 C9 C10 . . 121.3(12) C8 C9 H9A . . 119.4(7) C10 C9 H9A . . 119.3(9) C11 C10 C9 . . 120.2(13) C11 C10 H10A . . 119.9(8) C9 C10 H10A . . 119.9(9) C10 C11 C12 . . 119.5(12) C10 C11 H11A . . 120.2(8) C12 C11 H11A . . 120.3(8) C13 C12 C11 . . 121.3(13) C13 C12 H12A . . 119.3(8) C11 C12 H12A . . 119.3(8) C12 C13 C8 . . 120.1(12) C12 C13 H13A . . 120.0(8) C8 C13 H13A . . 119.9(7) C18 C14 C15 . . 108.3(11) C18 C14 C14A . . 124.9(12) C15 C14 C14A . . 126.6(11) C18 C14 Ta . . 70.8(8) C15 C14 Ta . . 72.4(8) C14A C14 Ta . . 126.3(9) C14 C15 C16 . . 105.7(11) C14 C15 C15A . . 128.8(12) C16 C15 C15A . . 125.3(12) C14 C15 Ta . . 74.7(7) C16 C15 Ta . . 70.0(7) C15A C15 Ta . . 123.8(10) C17 C16 C15 . . 108.6(11) C17 C16 C16A . . 127.7(11) C15 C16 C16A . . 123.7(11) C17 C16 Ta . . 70.7(7) C15 C16 Ta . . 76.2(8) C16A C16 Ta . . 120.6(10) C18 C17 C16 . . 108.2(11) C18 C17 C17A . . 126.7(12) C16 C17 C17A . . 124.1(11) C18 C17 Ta . . 77.0(8) C16 C17 Ta . . 75.5(8) C17A C17 Ta . . 122.9(9) C17 C18 C14 . . 109.1(11) C17 C18 C18A . . 127.8(11) C14 C18 C18A . . 122.8(12) C17 C18 Ta . . 69.6(8) C14 C18 Ta . . 76.9(9) C18A C18 Ta . . 124.5(9) C14 C14A H14A . . 109.1(8) C14 C14A H14B . . 109.6(7) H14A C14A H14B . . 109.5 C14 C14A H14C . . 109.7(8) H14A C14A H14C . . 109.5 H14B C14A H14C . . 109.5 C15 C15A H15A . . 109.6(8) C15 C15A H15B . . 109.5(7) H15A C15A H15B . . 109.5 C15 C15A H15C . . 109.4(8) H15A C15A H15C . . 109.5 H15B C15A H15C . . 109.5 C16 C16A H16A . . 109.3(8) C16 C16A H16B . . 109.5(7) H16A C16A H16B . . 109.5 C16 C16A H16C . . 109.6(7) H16A C16A H16C . . 109.5 H16B C16A H16C . . 109.5 C17 C17A H17A . . 109.3(8) C17 C17A H17B . . 109.7(8) H17A C17A H17B . . 109.5 C17 C17A H17C . . 109.4(7) H17A C17A H17C . . 109.5 H17B C17A H17C . . 109.5 C18 C18A H18A . . 109.4(7) C18 C18A H18B . . 109.7(7) H18A C18A H18B . . 109.5 C18 C18A H18C . . 109.3(7) H18A C18A H18C . . 109.5 H18B C18A H18C . . 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Ta O2 2 1.950(8) Ta O2 . 1.957(7) Ta O1 . 2.005(8) Ta C7 . 2.204(12) Ta C17 . 2.385(14) Ta C16 . 2.446(13) Ta C18 . 2.480(15) Ta C15 . 2.528(13) Ta C14 . 2.558(14) Ta Ta 2 3.0644(13) F2 C2 . 1.35(2) F3 C3 . 1.34(2) F4 C4 . 1.367(14) F5 C5 . 1.33(2) F6 C6 . 1.324(15) O1 C1 . 1.326(13) O2 Ta 2 1.950(8) C1 C6 . 1.37(2) C1 C2 . 1.40(2) C2 C3 . 1.39(2) C3 C4 . 1.36(2) C4 C5 . 1.39(2) C5 C6 . 1.39(2) C7 C8 . 1.50(2) C7 H7A . 0.990(13) C7 H7B . 0.990(13) C8 C9 . 1.38(2) C8 C13 . 1.42(2) C9 C10 . 1.41(2) C9 H9A . 0.96 C10 C11 . 1.34(2) C10 H10A . 0.96 C11 C12 . 1.40(2) C11 H11A . 0.96 C12 C13 . 1.37(2) C12 H12A . 0.96 C13 H13A . 0.96 C14 C18 . 1.40(2) C14 C15 . 1.44(2) C14 C14A . 1.49(2) C15 C16 . 1.45(2) C15 C15A . 1.48(2) C16 C17 . 1.40(2) C16 C16A . 1.50(2) C17 C18 . 1.40(2) C17 C17A . 1.51(2) C18 C18A . 1.52(2) C14A H14A . 0.96 C14A H14B . 0.96 C14A H14C . 0.96 C15A H15A . 0.96 C15A H15B . 0.96 C15A H15C . 0.96 C16A H16A . 0.96 C16A H16B . 0.96 C16A H16C . 0.96 C17A H17A . 0.96 C17A H17B . 0.96 C17A H17C . 0.96 C18A H18A . 0.96 C18A H18B . 0.96 C18A H18C . 0.96