Pentaammonium heptasodium bis[pentakis(μ~2~-oxido)decaoxidobis(μ~5~-phosphato)pentamolybdenum(VI)] henicosahydrate
Bih, Hssain; Bih, Lahcen; Manoun, Bouchaid; Azrour, Mohamed; Lazor, Peter; El Ammari, Lahcen; Acta Crystallographica Section E 66 (2010) i20–i21; doi:10.1107/S160053681000601X

data_2225232
_publ_section_title
;
 Pentaammonium heptasodium
 bis[pentakis(\m~2~-oxido)decaoxidobis(\m~5~-phosphato)pentamolybdenum(VI)]
 henicosahydrate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i20
_journal_page_last               i21
_journal_paper_doi               10.1107/S160053681000601X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(N H4)5 Na7 [Mo5 P2 O23]2, 21H2 O'
_chemical_formula_moiety
'5(H4 N +), 7(Na +), 2(Mo5 O23 P2 6-), 21(H2 O)'
_chemical_formula_sum            'H62 Mo10 N5 Na7 O67 P4'
_chemical_formula_weight         2448.76
_chemical_name_common
;
Pentaammoniun heptasodium heteropolyoxometallate heneicosahydrate
;
_chemical_name_systematic
;
Pentaammonium heptasodium bis[pentakis(\m~2~-oxido)decaoxidobis(\m~5~-
phosphato)pentamolybdenum(VI)] henicosahydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.8600(10)
_cell_angle_beta                 85.323(3)
_cell_angle_gamma                75.772(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2299(3)
_cell_length_b                   18.3516(6)
_cell_length_c                   19.7918(6)
_cell_measurement_reflns_used    33624
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      38.00
_cell_measurement_theta_min      1.37
_cell_volume                     3121.17(18)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker X8 APEXII Diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            132450
_diffrn_reflns_theta_full        38.00
_diffrn_reflns_theta_max         38.00
_diffrn_reflns_theta_min         1.37
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.228
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       paralellipiped
_exptl_crystal_F_000             2380
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.764
_refine_ls_extinction_coef       0.00095(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         33626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+2.3233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                28095
_reflns_number_total             33626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            fj2276.cif
_cod_data_source_block           I
_cod_original_cell_volume        3121.17(17)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               2225232
_cod_database_fobs_code          2225232