Structure, Magnetism, and Electrochemistry of the Multinickel Polyoxoanions [Ni~6~As~3~W~24~O~94~(H~2~O)~2~]^17-^, [Ni~3~Na(H~2~O)~2~(AsW~9~O~34~)~2~]^11-^, and [Ni~4~Mn~2~P~3~W~24~O~94~(H~2~O)~2~]^17-^
Israel M. Mbomekalle; Bineta Keita; Martine Nierlich; Ulrich Kortz; Patrick Berthet; Louis Nadjo; Inorganic Chemistry 42 (2003) 5143–5152; doi:10.1021/ic0343915

data_4314105
_publ_contact_author_address
;
      CEA/Saclay, SCM 
      B\^at. 125
      91191 Gif-sur-Yvette Cedex
      France
;
_publ_contact_author_email       nierlich@drecam.cea.fr
_publ_contact_author_fax         '01 69 08 66 40'
_publ_contact_author_name        ' Nierlich Martine'
_publ_contact_author_phone       '01 69 08 32 22'
_publ_section_title
;
 Structure, Magnetism, and Electrochemistry of the Multinickel
 Polyoxoanions [Ni~6~As~3~W~24~O~94~(H~2~O)~2~]^17-^,
 [Ni~3~Na(H~2~O)~2~(AsW~9~O~34~)~2~]^11-^, and
 [Ni~4~Mn~2~P~3~W~24~O~94~(H~2~O)~2~]^17-^
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5143
_journal_page_last               5152
_journal_paper_doi               10.1021/ic0343915
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'As2 H65 Na12 Ni3 O100.5 W18'
_chemical_formula_weight         5584.80
_chemical_name_systematic
; 
 ? 
;
_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                78.50(3)
_cell_angle_beta                 80.69(3)
_cell_angle_gamma                78.66(3)
_cell_formula_units_Z            2
_cell_length_a                   12.228(2)
_cell_length_b                   16.743(3)
_cell_length_c                   23.342(5)
_cell_measurement_reflns_used    31549
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     4554.0(16)
_computing_cell_refinement       'DENZO(Otwinowski& Minor,1997)'
_computing_data_collection       'DENZO(Otwinowski& Minor,1997)'
_computing_data_reduction        'DENZO(Otwinowski& Minor,1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick,1997)'
_computing_publication_material  'SHELXTL (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device       'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\f rotation scans with 2\%steps'
_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  0.1108
_diffrn_reflns_av_sigmaI/netI    0.1627
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31549
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         2.63
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    24.137
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.335
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DELABS in PLATON;Spek,1998'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4994
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         3.442
_refine_diff_density_min         -2.221
_refine_diff_density_rms         0.544
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         15966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1319
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1740
_reflns_number_gt                9176
_reflns_number_total             15966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0343915si20030529_111837_2.cif
_cod_data_source_block           Na11[Ni3Na(H2O)2(AsW9O34)2]30.5H2O
_cod_original_cell_volume        4554.1(16)
_cod_original_formula_sum        'H65 As2 Na12 Ni3 O100.5 W18'
_cod_database_code               4314105