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_7036547
_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         'C49 H81 N5 O4 S6 W'
_chemical_formula_sum            'C49 H81 N5 O4 S6 W'
_chemical_formula_weight         1180.39
_chemical_name_systematic
;
(NEt4)2[W(S2C6H3CONH-t-Bu)3]-H2O
;
_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-11
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-07-16 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.3866(5)
_cell_length_b                   18.6641(4)
_cell_length_c                   29.515(2)
_cell_measurement_reflns_used    65074
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.01
_cell_volume                     11781.3(9)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2008 (Burla et al., 2007)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            85613
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.018
_diffrn_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_exptl_absorpt_coefficient_mu    2.216
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.777
_refine_diff_density_min         -2.605
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.318(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1172
_refine_ls_number_reflns         20684
_refine_ls_number_restraints     579
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+130.5720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1503
_reflns_Friedel_coverage         0.959
_reflns_friedel_fraction_full    0.998
_reflns_friedel_fraction_max     0.998
_reflns_number_gt                15384
_reflns_number_total             20684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03278d2.cif
_cod_data_source_block           3-H2O
_cod_depositor_comments
'Adding full bibliography for 7036546--7036548.cif.'
_cod_original_cell_volume        11781.4(9)
_cod_database_code               7036547
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.556
_shelx_estimated_absorpt_t_max   0.957
_shelx_fab_checksum              22337