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_4323328
_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         'Ta2 N8 Cl2 C60 H60'
_chemical_formula_structural     (DTolF)Cl2Ta(mu-NTol)(mu-HCNTol)Ta(DTolF)2
_chemical_formula_sum            'C60 H60 Cl2 N8 Ta2'
_chemical_formula_weight         1325.96
_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                 90.126(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.962(3)
_cell_length_b                   15.539(4)
_cell_length_c                   19.973(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      14
_cell_volume                     5574.7(19)
_computing_cell_refinement       'CAD4 V5'
_computing_data_collection       'CAD4 V5'
_computing_data_reduction        SDP
_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      168(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       '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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7582
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.064
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.113
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         7264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_obs          0.0317
_refine_ls_shift/esd_max         0.073
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+11.6397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0827
_refine_ls_wR_factor_obs         0.0641
_reflns_number_observed          5167
_reflns_number_total             7266
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9611507_3.cif
_cod_data_source_block           cmpd_3
_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^)+(0.0221P)^2^+11.6397P] 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^)+(0.0221P)^2^+11.6397P] 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               4323328