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_4322385
_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            'C82 H99 N5 O S10 W2'
_chemical_formula_weight         1858.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                87.9620(10)
_cell_angle_beta                 76.6010(10)
_cell_angle_gamma                79.4020(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7885(2)
_cell_length_b                   15.9465(3)
_cell_length_c                   23.7428(5)
_cell_measurement_temperature    213(2)
_cell_volume                     4267.63(14)
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.1068
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23011
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.88
_exptl_absorpt_coefficient_mu    2.983
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             1884
_refine_diff_density_max         2.135
_refine_diff_density_min         -2.853
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.318
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         14855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_restrained_S_obs      1.318
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_obs          0.0428
_refine_ls_shift/esd_max         -0.043
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 [0.00000+1.00000exp(2.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0341P)^2^+0.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1028
_refine_ls_wR_factor_obs         0.0936
_reflns_number_observed          8438
_reflns_number_total             14862
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9903329_7.cif
_cod_data_source_block           cag25b
_cod_database_code               4322385