Tris(tetrabutylammonium) hexakis(<i>tert</i>-butanethiolato-κ<i>S</i>)hepta-μ~3~-chlorido-μ~3~-sulfido-hexamolybdate dihydrate
Petrov, Pavel A.; Naumov, Dmitry Yu.; Konchenko, Sergey N.; Acta Crystallographica Section E 68 (2012) m333–m334; doi:10.1107/S1600536812007416

data_2234032
_publ_section_title
;
 Tris(tetrabutylammonium)
 hexakis(<i>tert</i>-butanethiolato-\k<i>S</i>)hepta-\m~3~-chlorido-\m~3~-sulfido-hexamolybdate
 dihydrate
;
_journal_coeditor_code           WM2589
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m333
_journal_page_last               m334
_journal_paper_doi               10.1107/S1600536812007416
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C16 H36 N)3 [Mo6 (C4 H9 S)6 Cl7 S], 2H2 O'
_chemical_formula_moiety
'3(C16 H36 N +), C24 H54 Cl7 Mo6 S7 3-, 2(H2 O)'
_chemical_formula_sum            'C72 H166 Cl7 Mo6 N3 O2 S7'
_chemical_formula_weight         2154.29
_chemical_name_systematic
;
Tris(tetrabutylammonium)
hexakis(<i>tert</i>-butanethiolato-\k<i>S</i>)hepta-\m~3~-
chlorido-\m~3~-sulfido-hexamolybdate dihydrate
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.7481(5)
_cell_length_b                   18.7481(5)
_cell_length_c                   52.4233(12)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.47
_cell_volume                     15957.7(7)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008), Mercury (Macrae <i>et al.</i>, 2006)
and
POV-Ray (Persistence of Vision, 2004)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker--Nonius X8 APEX CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            36925
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.17
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.035
_exptl_absorpt_correction_T_max  0.7967
_exptl_absorpt_correction_T_min  0.6704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6708
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.758
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3637
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+69.7786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                3092
_reflns_number_total             3637
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2589.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               2234032
_cod_database_fobs_code          2234032