Octakis[2,2',5,5'-tetrathiafulvalenium(0.5+)] bis[hexamolybdate(2{-})] acetonitrile solvate
Zebiri, Ikram; Anak, Berkahoum; Djebli, Yacine; Boufas, Sihem; Bencharif, Leïla; Acta Crystallographica Section E 65 (2009) m1063–m1064; doi:10.1107/S1600536809031092

data_2223094
_publ_section_title
;
 Octakis[2,2',5,5'-tetrathiafulvalenium(0.5+)] bis[hexamolybdate(2{-})]
 acetonitrile solvate
;
_journal_coeditor_code           HG2545
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1063
_journal_page_last               m1064
_journal_paper_doi               10.1107/S1600536809031092
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '(C6 H4 S4)8 [Mo6 O19]2, C2 H3 N'
_chemical_formula_moiety         '8(C6 H4 S4 0.5+), 2(Mo6 O19 2-), C2 H3 N'
_chemical_formula_sum            'C50 H35 Mo12 N O38 S32'
_chemical_formula_weight         3434.99
_chemical_name_systematic
;
Octakis[2,2',5,5'-tetrathiafulvalenium(0.5+)] bis[hexamolybdate(2-)]
acetonitrile solvate
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.266(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3179(8)
_cell_length_b                   20.2299(10)
_cell_length_c                   16.7625(10)
_cell_measurement_reflns_used    2190
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.82
_cell_volume                     4761.7(5)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and  Mercury (Macrae <i>et al.</i>,  2006)'
_computing_publication_material
'WinGX (Farrugia, 1999) and PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1993)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45527
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.305
_exptl_absorpt_correction_T_max  0.8022
_exptl_absorpt_correction_T_min  0.5965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             3324
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.699
_refine_ls_extinction_coef       0.08(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         11170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.021P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0732
_reflns_number_gt                8144
_reflns_number_total             11170
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2545.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2223094
_cod_database_fobs_code          2223094