Ammonium tris(tetraethylammonium) hexacosaoxidooctamolybdate
Zebiri, Ikram; Bencharif, Le\?ïla; Direm, Amani; Bencharif, Mustapha; Benali-Cherif, Nourredine; Acta Crystallographica Section E 64 (2008) m474–m475; doi:10.1107/S1600536808004182

data_2217733
_publ_section_title
;
 Ammonium tris(tetraethylammonium) hexacosaoxidooctamolybdate
;
_journal_coeditor_code           BT2676
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m474
_journal_page_last               m475
_journal_paper_doi               10.1107/S1600536808004182
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'N H4 (C8 H20 N)3 [Mo8 O26]'
_chemical_formula_moiety         'N H4 + , 3C8 H20 N + , Mo8 O26 4-'
_chemical_formula_sum            'C24 H64 Mo8 N4 O26'
_chemical_formula_weight         1592.31
_chemical_name_common
'bis[(tris(tetraethylammonium)Hexacosaoxaoctamolybdate ammonium]'
_chemical_name_systematic
;
Ammonium tris(tetraethylammonium) hexacosaoxidooctamolybdate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.906(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7154(2)
_cell_length_b                   22.8873(3)
_cell_length_c                   19.9338(2)
_cell_measurement_reflns_used    29087
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.96
_cell_measurement_theta_min      1.03
_cell_volume                     4853.23(15)
_computing_cell_refinement
'DENZO and SCALEPAK (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1998)'
_computing_data_reduction
'DENZO and SCALEPAK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and PLATON (Spek, 2003)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       \w/\q
_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  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0801
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            57681
_diffrn_reflns_theta_full        30.96
_diffrn_reflns_theta_max         30.96
_diffrn_reflns_theta_min         1.03
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.864
_refine_diff_density_min         -1.289
_refine_ls_abs_structure_details 'Flack (1983), with 13317 Friedel pairs'
_refine_ls_abs_structure_Flack   0.17(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         29087
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0616P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                21795
_reflns_number_total             29087
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2676.cif
_cod_data_source_block           I
_cod_original_cell_volume        4853.23(12)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2217733
_cod_database_fobs_code          2217733