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_2104985
_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*).[C6F5O]2.Ta.(O)2.Ta.[C6F5O]2.(Cp*)
_chemical_formula_sum            'C51 H38 F20 O6 Ta2'
_chemical_formula_weight         1488.71
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.178(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.793(2)
_cell_length_b                   15.242(2)
_cell_length_c                   25.708(3)
_cell_measurement_reflns_used    429
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.2
_cell_measurement_theta_min      3.55
_cell_volume                     4933.9(12)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'Siemens SMART CCD 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  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17825
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.559
_exptl_absorpt_correction_T_max  0.447
_exptl_absorpt_correction_T_min  0.343
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.321
_refine_diff_density_min         -0.960
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.263
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         6922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.263
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                6101
_reflns_number_total             6926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zb5019.cif
_cod_data_source_block           95srv082
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C44 H30 F20 O6 Ta2 . C7H8'
_cod_database_code               2104985
_cod_database_fobs_code          2104985