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_4323327
_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_moiety         'Ta2N10C75H74, 1.5(C6H14)'
_chemical_formula_structural
'Ta2(MePhNC(H)NPhMe)4(mu-NPhMe)(mu-CNPhMe), 1.5(C6H14)'
_chemical_formula_sum            'C84 H95 N10 Ta2'
_chemical_formula_weight         1606.60
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                98.98(1)
_cell_angle_beta                 104.07(1)
_cell_angle_gamma                109.59(1)
_cell_formula_units_Z            2
_cell_length_a                   13.990(2)
_cell_length_b                   15.841(1)
_cell_length_c                   19.442(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      40.1
_cell_measurement_theta_min      9.1
_cell_volume                     3802.1(11)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_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  0.074
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_diffrn_reflns_limit_h_max       15
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_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
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_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.926
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1630
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    noref
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_refine_ls_restrained_S_obs      1.117
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_obs          0.0400
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_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+7.4786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1215
_refine_ls_wR_factor_obs         0.1056
_reflns_number_observed          5727
_reflns_number_total             7074
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9611507_2.cif
_cod_data_source_block           cmpd_2
_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^)+(0.0592P)^2^+7.4786P] 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^)+(0.0592P)^2^+7.4786P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3802.1(1)
_cod_database_code               4323327