Syntheses of Metal Dithiolene Complexes from Thiometalates by Induced Internal Redox Reactions
Kun Wang; Jonathan M. McConnachie; Edward I. Stiefel; Inorganic Chemistry 38 (1999) 4334–4341; doi:10.1021/ic990204k

data_4322451
_publ_section_title
;
 Syntheses of Metal Dithiolene Complexes from Thiometalates by Induced
 Internal Redox Reactions
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4334
_journal_page_last               4341
_journal_paper_doi               10.1021/ic990204k
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C28 H40 F18 Mo N2 S6'
_chemical_formula_weight         1034.92
_chemical_name_systematic
;
 ?
;
_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                 110.29(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.905(4)
_cell_length_b                   13.732(3)
_cell_length_c                   17.101(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4164.0(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7312
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.721
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_F_000             2088
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.092
_refine_ls_goodness_of_fit_obs   1.125
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         3665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_obs          0.0454
_refine_ls_shift/esd_max         0.017
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+0.5127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1256
_refine_ls_wR_factor_obs         0.1098
_reflns_number_observed          2733
_reflns_number_total             3666
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990204k_1.cif
_cod_data_source_block           test
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+0.5127P] 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^)+(0.0663P)^2^+0.5127P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        4164.0(14)
_cod_database_code               4322451