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_4350361
_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         'C37 H64 N6 O7 S4 W '
_chemical_formula_sum            'C37 H64 N6 O7 S4 W'
_chemical_formula_weight         1017.03
_chemical_name_systematic
; 
(NEt4)2[WO2{S2C6H2(NHCOCH3)2}2]-MeOH 
;
_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             'Wed Apr 26 16:41:22 2006'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.24(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.75(3)
_cell_length_b                   20.38(3)
_cell_length_c                   13.06(2)
_cell_measurement_reflns_used    14582
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     4631(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21533
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    2.723
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.749
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5276
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0351P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                2946
_reflns_number_total             5276
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic060719tsi20060428_120729.cif
_cod_data_source_block           5-MeOH
_cod_original_cell_volume        4632(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4350361