Tantalum Alkyl and Silyl Complexes of the Bulky (Terphenyl)imido Ligand [2,6-(2,4,6-Me3C6H2)2C6H3N]2-([Ar*N]2-). Generation and Reactivity of [(Ar*N)(Ar*NH)Ta(H)(OSO2CF3)], Which Reversibly Transfers Hydride to an Aromatic Ring of the Arylamide Ligand
Gavenonis, John; Tilley, T. Don; Organometallics 21 (2002) 5549–; doi:10.1021/om020509y

data_4077053
_publ_section_title
;
 Tantalum Alkyl and Silyl Complexes of the Bulky (Terphenyl)imido Ligand
 [2,6-(2,4,6-Me3C6H2)2C6H3N]2-([Ar*N]2-). Generation and Reactivity of
 [(Ar*N)(Ar*NH)Ta(H)(OSO2CF3)], Which Reversibly Transfers Hydride to an
 Aromatic Ring of the Arylamide Ligand
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5549
_journal_paper_doi               10.1021/om020509y
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         '(C58 H73 N2 Ta)2, (C5 H12)'
_chemical_formula_sum            'C60.5 H79 N2 Ta'
_chemical_formula_weight         1015.21
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 115.977(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9435(9)
_cell_length_b                   43.319(4)
_cell_length_c                   12.4363(10)
_cell_measurement_reflns_used    5338
_cell_measurement_temperature    159(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      1.73
_cell_volume                     5299.9(8)
_computing_cell_refinement       'Bruker SAINT v5.04'
_computing_data_collection       'Bruker SMART v5.052d'
_computing_data_reduction        'Bruker SAINT v5.04'
_computing_molecular_graphics    SHELXTL-XP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      159(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.1289
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24124
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    2.112
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       plate
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.942
_refine_ls_goodness_of_fit_obs   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         16563
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.942
_refine_ls_restrained_S_obs      0.940
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_obs          0.0506
_refine_ls_shift/esd_max         0.018
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0895
_refine_ls_wR_factor_obs         0.0791
_reflns_number_observed          13184
_reflns_number_total             16564
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om020509y.cif
_cod_data_source_block           Complex_8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^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^)+(0.0000P)^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 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C60.50 H79 N2 Ta'
_cod_database_code               4077053