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_7036548
_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         'C46 H86 N4 O9 S4 W2'
_chemical_formula_sum            'C46 H86 N4 O9 S4 W2'
_chemical_formula_weight         1335.12
_chemical_name_systematic
;
(NEt4)2[W2O5(1,2-S2-3-t-BuNHCOC6H3)2]-2Et2O
;
_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-07-16 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.438(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.9606(14)
_cell_length_b                   8.7047(8)
_cell_length_c                   18.3212(14)
_cell_measurement_reflns_used    19911
_cell_measurement_temperature    200
_cell_measurement_theta_max      'not measured'
_cell_measurement_theta_min      3.14
_cell_volume                     2863.5(4)
_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 4.1 (Rigaku, 2014)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26944
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.138
_exptl_absorpt_coefficient_mu    4.210
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.858
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         6532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.858
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0437
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4605
_reflns_number_total             6532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03278d2.cif
_cod_data_source_block           4-2Et2O
_cod_depositor_comments
'Adding full bibliography for 7036546--7036548.cif.'
_cod_database_code               7036548
_shelxl_version_number           2014/6