A Wonderful Bond That Wasn't There: Reformulation of a Compound "Containing a Ta-Ta Bond without Bridging Ligands" as [(Cy~2~N)~2~ClTa(μ-H)]~2~
F. Albert Cotton; Lee M. Daniels; Carlos A. Murillo; Xiaoping Wang; Journal of the American Chemical Society 118 (1996) 12449–12450; doi:10.1021/ja9629165

data_4117217
_publ_contact_author
;
 Prof. F.A. Cotton
 Department of Chemistry
 Mail Stop 3255
 Texas A&M University
 College Station, TX 77843
 USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '409 845 9351'
_publ_contact_author_phone       '409 845 4432'
_publ_section_title
;
 A Wonderful Bond That Wasn't There: Reformulation of a Compound
 "Containing a Ta-Ta Bond without Bridging Ligands" as
 [(Cy~2~N)~2~ClTa(\m-H)]~2~
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12449
_journal_page_last               12450
_journal_paper_doi               10.1021/ja9629165
_journal_volume                  118
_journal_year                    1996
_chemical_compound_source        synthesis
_chemical_formula_sum            'C48 H90 Cl2 N4 Ta2'
_chemical_formula_weight         1156.04
_chemical_name_common            Ta2(\m-H)2Cl2(Cy2N)4
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 94.702(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.234(5)
_cell_length_b                   10.804(1)
_cell_length_c                   22.765(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.9
_cell_measurement_theta_min      9.0
_cell_volume                     10352.6(18)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'SHELXTL V5'
_computing_publication_material  'SHELXTL V5'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Enraf-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    0.0237
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5447
_diffrn_reflns_theta_max         22.12
_diffrn_reflns_theta_min         1.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.362
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            'dark red '
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       rod-shaped
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.090
_refine_ls_goodness_of_fit_obs   1.089
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         5388
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.117
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_obs          0.0324
_refine_ls_shift/esd_max         -0.978
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+134.3155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0861
_refine_ls_wR_factor_obs         0.0804
_reflns_number_observed          5055
_reflns_number_total             5447
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9629165.cif
_cod_data_source_block           JA9629165-234
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+134.3155P] 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^)+(0.0404P)^2^+134.3155P] 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        10353(2)
_cod_original_formula_sum        'C48 H2 H88 Cl2 N4 Ta2'
_cod_database_code               4117217