Bis[tris(diisobutyldithiocarbamato)-μ3-sulfido-tri-μ2-disulfido-trimolybdenum(IV)] sulfide tetrahydrofuran monosolvate
Fraker, Addison; Donahue, James P.; McSkimming, Alex; Acta Crystallographica Section E Crystallographic Communications 80 (2024) –; doi:10.1107/S2056989024002949

data_2023090
_publ_section_title
;
 Bis[tris(diisobutyldithiocarbamato)-\m3-sulfido-tri-\m2-disulfido-trimolybdenum(IV)]
 sulfide tetrahydrofuran monosolvate
;
_journal_coeditor_code           OI2005
_journal_issue                   5
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024002949
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Mo3 (C9 H18 N S2)3 (S2)3 S]2 S'
_chemical_formula_moiety         '2(C27 H54 Mo3 N3 S13 +), S 2-'
_chemical_formula_sum            'C54 H108 Mo6 N6 S27'
_chemical_formula_weight         2282.72
_chemical_name_systematic
'Bis[tris(diisobutyldithiocarbamato)-\m~3~-sulfido-tri-\m~2~-disulfido-trimolybdenum(IV)] sulfide tetrahydrofuran monosolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 91.576(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1699(7)
_cell_length_b                   21.1139(10)
_cell_length_c                   30.0046(14)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.316
_cell_measurement_theta_min      5.0035
_cell_volume                     10240.0(8)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2021)
;
_computing_data_collection
;
<i>APEX4</i> (Bruker, 2021)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2021)
;
_computing_molecular_graphics
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Bruker D8 VENTURE PHOTON 3 CPAD'
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 3'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            332865
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.060
_diffrn_reflns_theta_min         2.559
_diffrn_source                   'INCOATEC I\mS micro-focus source'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.240
_exptl_absorpt_correction_T_max  0.355
_exptl_absorpt_correction_T_min  0.120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4632
_exptl_crystal_size_max          0.363
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.116
_refine_diff_density_max         1.552
_refine_diff_density_min         -0.667
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         20942
_refine_ls_number_restraints     492
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+22.8874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                18768
_reflns_number_total             20942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oi2005.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2023090
_shelx_estimated_absorpt_t_min   0.106
_shelx_estimated_absorpt_t_max   0.356
_shelx_hkl_checksum              52290
_shelx_res_checksum              2907
_shelx_fab_checksum              81564