Significant differences of monooxotungsten(iv) and dioxotungsten(vi) benzenedithiolates containing two intramolecular NHS hydrogen bonds from molybdenum analogues.
Okamura, A Taka-Aki; Omi, Yui; Fujii, Manami; Tatsumi, Miki; Onitsuka, Kiyotaka; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18090–18100; doi:10.1039/c5dt03278d

data_7036546
_publ_section_title
;
 Significant differences of monooxotungsten(iv) and dioxotungsten(vi)
 benzenedithiolates containing two intramolecular NHS hydrogen bonds from
 molybdenum analogues.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18090
_journal_page_last               18100
_journal_paper_doi               10.1039/c5dt03278d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C38 H66 N4 O3 S4 W'
_chemical_formula_sum            'C38 H66 N4 O3 S4 W'
_chemical_formula_weight         939.04
_chemical_name_systematic
; 
(NEt4)2[WO(S2C6H3CONH-t-Bu)2] 
;
_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-08-17
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-16 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.865(2)
_cell_length_b                   16.289(3)
_cell_length_c                   29.929(7)
_cell_measurement_reflns_used    27666
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      3.08
_cell_volume                     4321.8(16)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            28811
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    2.905
_exptl_absorpt_correction_T_max  0.8684
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.983
_refine_diff_density_min         -2.664
_refine_diff_density_rms         0.180
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3157 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.002(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7323
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+64.7205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                6972
_reflns_number_total             7323
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5dt03278d2.cif
_cod_data_source_block           1-W
_cod_depositor_comments
'Adding full bibliography for 7036546--7036548.cif.'
_cod_database_code               7036546