Cleavage of Formamidinate Ligands on a TaTa Double Bond: Formation of HxCNAryl (x= 0 and 1) and Arylimido-Bridged Complexes
F. Albert Cotton; Lee M. Daniels; Carlos A. Murillo; Xiaoping Wang; Inorganic Chemistry 36 (1997) 896–901; doi:10.1021/ic9611507

data_4323326
_publ_section_title
;
 Cleavage of Formamidinate Ligands on a TaTa Double Bond: Formation of
 HxCNAryl (x= 0 and 1) and Arylimido-Bridged Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              896
_journal_page_last               901
_journal_paper_doi               10.1021/ic9611507
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        synthesis
_chemical_formula_structural     ((DPhF)2Ta)2(mu-NPh)(mu-HCNPh)
_chemical_formula_sum            'C72 H62 N10 Ta2'
_chemical_formula_weight         1429.22
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 97.840(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.437(2)
_cell_length_b                   15.5870(10)
_cell_length_c                   20.4010(10)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.9
_cell_measurement_theta_min      9.0
_cell_volume                     6123.0(8)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        ABSURD
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  'XP (Siemens, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST'
_diffrn_measurement_method       'frame data from omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5082
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         2.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.623
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.923
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.125
_refine_ls_goodness_of_fit_obs   1.161
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5079
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.139
_refine_ls_restrained_S_obs      1.165
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_obs          0.0571
_refine_ls_shift/esd_max         0.010
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+67.9472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1464
_refine_ls_wR_factor_obs         0.1366
_reflns_number_observed          4259
_reflns_number_total             5082
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9611507_1.cif
_cod_data_source_block           cmpd_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+67.9472P] 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^)+(0.0654P)^2^+67.9472P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323326