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_7034142
_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         'C174 H222 Mo N10 O7 S4 Si'
_chemical_formula_sum            'C174 H222 Mo N10 O7 S4 Si'
_chemical_formula_weight         2817.87
_chemical_name_systematic
; 
(NEt4)[MoOSi(t-Bu)Ph2{S2C6H2[NHCOC(C6H4-t-Bu)3]2}2]-5(CH3CN)-2(H2O)
;
_chemical_properties_physical    'Air-sensitive, Efflorescent'
_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_date             2014-11-27
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-02-13 deposited with the CCDC.
2015-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.832(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.8827(13)
_cell_length_b                   23.9699(18)
_cell_length_c                   20.0864(14)
_cell_measurement_reflns_used    18773
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.05
_cell_volume                     8864.4(11)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1199
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_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            66615
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.076
_diffrn_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1206
_refine_ls_number_reflns         15579
_refine_ls_number_restraints     829
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1866
_refine_ls_R_factor_gt           0.0908
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1770P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2439
_refine_ls_wR_factor_ref         0.3094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6651
_reflns_number_total             15579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00075k2.cif
_cod_data_source_block           1-5(CH3CN)-2(H2O)
_cod_depositor_comments
'Adding full bibliography for 7034142--7034143.cif.'
_cod_database_code               7034142
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.965
_shelx_estimated_absorpt_t_max   0.982