Bis(4-aminopyridinium) μ~6~-oxido-dodeca-μ~2~-oxido-hexaoxido[rhenium(VII)tetratungsten(VI)vanadium(V)]ate heptahydrate
Maaloui, Ahlem; Toumi, Samah Akriche; Rzaigui, Mohamed; Acta Crystallographica Section E 69 (2013) m661–m662; doi:10.1107/S1600536813030687

data_2238916
_publ_section_title
;
 Bis(4-aminopyridinium)
 \m~6~-oxido-dodeca-\m~2~-oxido-hexaoxido[rhenium(VII)tetratungsten(VI)vanadium(V)]ate
 heptahydrate
;
_journal_coeditor_code           RZ5088
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m661
_journal_page_last               m662
_journal_paper_doi               10.1107/S1600536813030687
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '(C5 H7 N2)2 [Re V W4 O19], 7H2 O'
_chemical_formula_moiety         '2(C5 H7 N2 +), O19 Re V W4 2-, 7(H2 O)'
_chemical_formula_sum            'C10 H28 N4 O26 Re V W4'
_chemical_formula_weight         1592.90
_chemical_name_systematic
;Bis(4-aminopyridinium)
\m~6~-oxido-dodeca-\m~2~-oxido-hexaoxido[rhenium(VII)tetratungsten(VI)vanadium(V)]ate heptahydrate
;
_space_group_IT_number           51
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2a'
_symmetry_space_group_name_H-M   'P m m a'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.837(2)
_cell_length_b                   9.163(4)
_cell_length_c                   10.552(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     1724.6(9)
_computing_cell_refinement       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1996)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg & Putz,
2005)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       2
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6539
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    9.224
_exptl_absorpt_correction_T_max  0.3058
_exptl_absorpt_correction_T_min  0.0999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.941
_refine_diff_density_min         -2.825
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         4385
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1631
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0813P)^2^+4.9537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1924
_reflns_number_gt                2083
_reflns_number_total             4385
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            rz5088.cif
_cod_data_source_block           I
_cod_original_cell_volume        1724.5(9)
_cod_database_code               2238916