Tris[<i>N</i>,<i>N</i>-bis(3,5-di-<i>tert</i>-butylbenzyl)dithiocarbamato-κ^2^<i>S</i>,<i>S</i>']-μ~3~-sulfido-tris-μ~2~-disulfido-<i>triangulo</i>-trimolybdenum(IV) iodide
Chen, Yueli; Wang, Bo; Fontenot, Patricia; Donahue, James P.; IUCrData 5 (2020) x200939–; doi:10.1107/S2414314620009396

data_1558621
_publ_section_title
;
 Tris[<i>N</i>,<i>N</i>-bis(3,5-di-<i>tert</i>-butylbenzyl)dithiocarbamato-\k^2^<i>S</i>,<i>S</i>']-\m~3~-sulfido-tris-\m~2~-disulfido-<i>triangulo</i>-trimolybdenum(IV)
 iodide
;
_journal_coeditor_code           PK4027
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x200939
_journal_paper_doi               10.1107/S2414314620009396
_journal_volume                  5
_journal_year                    2020
_chemical_formula_iupac          '[Mo3 (C31 H46 N1 S2)3 S7] I'
_chemical_formula_moiety         'C93 H138 Mo3 N3 S13 +, I -'
_chemical_formula_sum            'C93 H138 I Mo3 N3 S13'
_chemical_formula_weight         2129.56
_chemical_name_systematic
'Tris[<i>N</i>,<i>N</i>-bis(3,5-di-<i>tert</i>-butylbenzyl)dithiocarbamato-\k^2^<i>S</i>,<i>S</i>']-\m~3~-sulfido-tris-\m~2~-disulfido-<i>triangulo</i>-trimolybdenum(IV) iodide'
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   23.6627(12)
_cell_length_b                   23.6627(12)
_cell_length_c                   10.9815(6)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.003
_cell_measurement_theta_min      2.7645
_cell_volume                     5325.0(5)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT/5</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            89878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.108
_diffrn_reflns_theta_min         1.721
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause et al., 2015)
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.128
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.542
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3209 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         7810
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+6.2404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                7053
_reflns_number_total             7810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk4027sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        5325.0(6)
_cod_database_code               1558621
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.890
_shelx_hkl_checksum              46901
_shelx_res_checksum              50814
_cod_database_fobs_code 1558621