Dioxotungsten 1,2-benzenedithiolate complex stabilized by NH...S hydrogen bonds.
Baba, Koji; Okamura, Taka-aki; Yamamoto, Hitoshi; Yamamoto, Tetsuo; Ohama, Mitsuo; Ueyama, Norikazu; Inorganic chemistry 45 (2006) 8365–8371; doi:10.1021/ic060719t

data_4350360
_publ_section_title
;
 Dioxotungsten 1,2-benzenedithiolate complex stabilized by NH...S hydrogen
 bonds.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8365
_journal_page_last               8371
_journal_paper_doi               10.1021/ic060719t
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C42 H74 N8 O7 S4 W'
_chemical_formula_sum            'C42 H74 N8 O7 S4 W'
_chemical_formula_weight         1115.18
_chemical_name_systematic
; 
(NEt4)2[WO{S2C6H2(NHCOCH3)2}2]-2(DMF) 
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_date             'Mon Sep 13 18:24:35 2004'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.854(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.371(4)
_cell_length_b                   9.099(5)
_cell_length_c                   28.513(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      11.0
_cell_volume                     5247(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_sigmaI/netI    0.2329
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            6178
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0.15
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.412
_exptl_absorpt_correction_T_max  0.617
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.092
_refine_diff_density_min         -1.341
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.00025(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         6023
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.2498
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.2174
_reflns_number_gt                2233
_reflns_number_total             6023
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic060719tsi20060428_120729.cif
_cod_data_source_block           3-DMF
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4350360