Efficient uptake of dimethyl sulfoxide by the desoxomolybdenum(iv) dithiolate complex containing bulky hydrophobic groups.
Hasenaka, Yuki; Okamura, Taka-Aki; Onitsuka, Kiyotaka; Dalton transactions (Cambridge, England : 2003) 44 (2015) 6260–6267; doi:10.1039/c5dt00075k

data_7034143
_publ_section_title
;
 Efficient uptake of dimethyl sulfoxide by the desoxomolybdenum(iv)
 dithiolate complex containing bulky hydrophobic groups.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6260
_journal_page_last               6267
_journal_paper_doi               10.1039/c5dt00075k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C171 H218.5 N8.5 O8.5 S4 Si W'
_chemical_formula_sum            'C171 H218.5 N8.5 O8.5 S4 Si W'
_chemical_formula_weight         2869.22
_chemical_name_systematic
; 
(NEt4)[WO(OSitBuPh2)[S2C6H2[NHCOC(C6H4tBu)3]2}2]-7/2(CH3CN)-5/2(H2O)
;
_chemical_properties_physical    'Air-sensitive, Efflorescent'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-27
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-13 deposited with the CCDC.
2015-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                93.493(7)
_cell_angle_beta                 104.138(7)
_cell_angle_gamma                90.070(6)
_cell_formula_units_Z            2
_cell_length_a                   18.246(3)
_cell_length_b                   20.495(4)
_cell_length_c                   26.099(4)
_cell_measurement_reflns_used    9725
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      3.00
_cell_volume                     9445(3)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'PATTY (Beurskens, P.T. et al., 1991)'
_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_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2138
_diffrn_reflns_av_sigmaI/netI    0.4241
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            72482
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.9653
_exptl_absorpt_correction_T_min  0.8423
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3048
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.210
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1790
_refine_ls_number_reflns         33198
_refine_ls_number_restraints     1847
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.2707
_refine_ls_R_factor_gt           0.1028
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.2029
_reflns_number_gt                8375
_reflns_number_total             33198
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5dt00075k2.cif
_cod_data_source_block           3-7/2(CH3CN)-5/2(H2O)
_cod_depositor_comments
'Adding full bibliography for 7034142--7034143.cif.'
_cod_original_formula_sum        'C171 H218.50 N8.50 O8.50 S4 Si W'
_cod_database_code               7034143