Tris(tetramethylammonium) tetra-μ~2~-sulfido-tetrasulfidocopper(I)dimolybdenum(VI) <i>N</i>,<i>N</i>-dimethylformamide solvate
Cao, Yuan; Chen, Yulin; Cheng, Guosheng; Acta Crystallographica Section E 64 (2008) m1546–; doi:10.1107/S1600536808036532

data_2220068
_publ_section_title
;
 Tris(tetramethylammonium)
 tetra-\m~2~-sulfido-tetrasulfidocopper(I)dimolybdenum(VI)
 <i>N</i>,<i>N</i>-dimethylformamide solvate
;
_journal_coeditor_code           BH2199
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1546
_journal_paper_doi               10.1107/S1600536808036532
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '(C4 H12 N)3 [Cu Mo2 S8], C3 H7 N O'
_chemical_formula_moiety         '3(C4 H12 N +), Cu Mo2 S8 3-, C3 H7 N O'
_chemical_formula_sum            'C15 H43 Cu Mo2 N4 O S8'
_chemical_formula_weight         807.43
_chemical_name_systematic
;
Tris(tetramethylammonium)
tetra-\m~2~-sulfido-tetrasulfidocopper(I)dimolybdenum(VI)
<i>N</i>,<i>N</i>-dimethylformamide solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 98.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4380(19)
_cell_length_b                   20.336(4)
_cell_length_c                   17.718(4)
_cell_measurement_reflns_used    7032
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.10
_cell_measurement_theta_min      1.20
_cell_volume                     3362.4(12)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17155
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.873
_exptl_absorpt_correction_T_max  0.618
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            'black red'
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.852
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0646P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                5061
_reflns_number_total             6625
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2199.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2220068
_cod_database_fobs_code          2220068