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_7032142
_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         'C73.1 H96.4 N2 O6.1 S3'
_chemical_formula_sum            'C73.1 H96.4 N2 O6.1 S3'
_chemical_formula_weight         1193.94
_chemical_name_systematic
;
[{(t-BuC6H4)3CCONH}2C6H2S]2S-3.1(MeOH)-H2O
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 103.207(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.228(9)
_cell_length_b                   20.296(6)
_cell_length_c                   14.423(5)
_cell_measurement_reflns_used    13215
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      3.00
_cell_volume                     7190(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    'SIR2008 (M.C. Burla, et al. 2007)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.969
_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  0.1214
_diffrn_reflns_av_unetI/netI     0.1534
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26258
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.995
_diffrn_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2577
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, methanol'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         11821
_refine_ls_number_restraints     345
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.2918
_refine_ls_R_factor_gt           0.1461
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3355
_refine_ls_wR_factor_ref         0.4201
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4071
_reflns_number_total             11821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01646g2.cif
_cod_data_source_block           L1-3.1(MeOH)-H2O
_cod_depositor_comments
'Adding full bibliography for 7032142--7032147.cif.'
_cod_database_code               7032142
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2014/6