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_2104984
_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_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     Cp*Ta(C6F5O-)4
_chemical_formula_sum            'C34 H15 F20 O4 Ta'
_chemical_formula_weight         1048.41
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.341(2)
_cell_length_b                   26.389(5)
_cell_length_c                   15.145(3)
_cell_measurement_reflns_used    57
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      12.0735
_cell_measurement_theta_min      5.2975
_cell_volume                     3333.6(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Siemens P4'
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0905
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3749
_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    3.451
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_description       needle
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.845
_refine_diff_density_min         -1.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                2150
_reflns_number_total             3043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zb5019.cif
_cod_data_source_block           xmas1
_cod_original_sg_symbol_Hall     -P2c2b
_cod_original_sg_symbol_H-M      Pbcm
_cod_database_code               2104984
_cod_database_fobs_code          2104984