Behavior of anionic molybdenum(iv, vi) and tungsten(iv, vi) complexes containing bulky hydrophobic dithiolate ligands and intramolecular NHS hydrogen bonds in nonpolar solvents.
Hasenaka, Yuki; Okamura, Taka-Aki; Tatsumi, Miki; Inazumi, Naoya; Onitsuka, Kiyotaka; Dalton transactions (Cambridge, England : 2003) 43 (2014) 15491–15502; doi:10.1039/c4dt01646g

data_7032146
_publ_section_title
;
 Behavior of anionic molybdenum(iv, vi) and tungsten(iv, vi) complexes
 containing bulky hydrophobic dithiolate ligands and intramolecular NHS
 hydrogen bonds in nonpolar solvents.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15491
_journal_page_last               15502
_journal_paper_doi               10.1039/c4dt01646g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C190 H247 N9 O6 S4 W'
_chemical_formula_sum            'C190 H247 N9 O6 S4 W'
_chemical_formula_weight         3065.04
_chemical_name_systematic
;
(NEt4)2[WO{S2C6H2[NHCOC(C6H4-t-Bu)3]2}2]-4(toluene)-3(CH3CN)-H2O
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Efflorescent'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-08-06
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 108.061(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.235(5)
_cell_length_b                   23.938(3)
_cell_length_c                   20.131(3)
_cell_measurement_reflns_used    54853
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.02
_cell_volume                     17976(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 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.970
_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  0.0797
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67944
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_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    0.744
_exptl_absorpt_correction_T_max  0.9293
_exptl_absorpt_correction_T_min  0.8654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             6544
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, acetonitrile'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.948
_refine_diff_density_min         -2.106
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         15799
_refine_ls_number_restraints     607
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1484
_refine_ls_R_factor_gt           0.1265
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1143P)^2^+337.8758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3199
_refine_ls_wR_factor_ref         0.3323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12222
_reflns_number_total             15799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01646g2.cif
_cod_data_source_block           1-W-4(toluene)-3(CH3CN)-H2O
_cod_depositor_comments
'Adding full bibliography for 7032142--7032147.cif.'
_cod_database_code               7032146
_shelx_estimated_absorpt_t_min   0.865
_shelx_estimated_absorpt_t_max   0.929
_shelxl_version_number           2014/6