Synthesis and Reactivity Aspects of the Bis(dithiolene) Chalcogenide Series [WIVQ(S2C2R2)2]2- (Q = O, S, Se)
Christine A. Goddard; R. H. Holm; Inorganic Chemistry 38 (1999) 5389–5398; doi:10.1021/ic9903329

data_4322381
_publ_section_title
;
 Synthesis and Reactivity Aspects of the Bis(dithiolene) Chalcogenide
 Series [WIVQ(S2C2R2)2]2- (Q = O, S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5389
_journal_page_last               5398
_journal_paper_doi               10.1021/ic9903329
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C46 H64 N2 O1.5 S4 W'
_chemical_formula_weight         981.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.5920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.3362(3)
_cell_length_b                   17.6679(3)
_cell_length_c                   30.9649(2)
_cell_measurement_temperature    213(2)
_cell_volume                     9218.7(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_method       'phi and 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  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            48614
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    2.724
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_F_000             4032
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.005
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         16229
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.006
_refine_ls_restrained_S_obs      1.123
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_obs          0.0412
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1035
_refine_ls_wR_factor_obs         0.0973
_reflns_number_observed          11774
_reflns_number_total             16232
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9903329_3.cif
_cod_data_source_block           cag19a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.0000P] 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^)+(0.0560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C46 H64 N2 O1.50 S4 W'
_cod_database_code               4322381