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_2104983
_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.C(t-Bu)2.N(t-Bu)
_chemical_formula_sum            'C24 H46 N Ta'
_chemical_formula_weight         529.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 99.76(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.083(2)
_cell_length_b                   16.216(3)
_cell_length_c                   16.872(3)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      12.47
_cell_measurement_theta_min      12.41
_cell_volume                     2449.1(9)
_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 1
_diffrn_measured_fraction_theta_max 0.726
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\t/\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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            13104
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.495
_exptl_absorpt_correction_T_max  0.365
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       cube
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.785
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         10777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+0.0105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                7822
_reflns_number_total             10777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zb5019.cif
_cod_data_source_block           combined
_cod_original_cell_volume        2449.1(8)
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               2104983
_cod_database_fobs_code          2104983