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^<i>t^</i>Bu)(CH~2~<i>R</i>)~2~ with pentafluorophenol
Cole, Jacqueline M.; Chan, Michael C. W.; Gibson, Vernon C.; Howard, Judith A. K.; Acta Crystallographica Section B 67 (2011) 416–424; doi:10.1107/S0108768111029259

data_2104982
_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^<i>t^</i>Bu)(CH~2~<i>R</i>)~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