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_4322383
_publ_section_title
;
 Synthesis and Reactivity Aspects of the Bis(dithiolene) Chalcogenide
 Series [WIVQ(S2C2R2)2]2- (Q = O, S, Se)
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_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            'C47 H67 N O3 S4 W'
_chemical_formula_weight         1006.11
_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                 102.155(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.591(4)
_cell_length_b                   22.396(5)
_cell_length_c                   10.5719(15)
_cell_measurement_temperature    213(2)
_cell_volume                     4766.0(16)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(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  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25299
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    2.638
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_F_000             2072
_refine_diff_density_max         2.173
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.166
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.166
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_obs          0.0446
_refine_ls_shift/esd_max         -0.012
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1059
_refine_ls_wR_factor_obs         0.0979
_reflns_number_observed          5897
_reflns_number_total             8391
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9903329_5.cif
_cod_data_source_block           cag31sa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0500P)^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^)+(0.0500P)^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 
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_cod_original_cell_volume        4765.9(16)
_cod_database_code               4322383