Sandwich-Type Phosphotungstates: Structure, Electrochemistry, and Magnetism of the Trinickel-Substituted Polyoxoanion [Ni~3~Na(H~2~O)~2~(PW~9~O~34~)~2~]^11-^
Ulrich Kortz; Israel M. Mbomekalle; Bineta Keita; Louis Nadjo; Patrick Berthet; Inorganic Chemistry 41 (2002) 6412–6416; doi:10.1021/ic0255353

data_4318931
_publ_contact_author_address
; 
Department of Chemistry
American University of Beirut
P.O. Box: 11-0236
Riad El Solh Beirut 1107 2020
LEBANON
;
_publ_contact_author_email
;
ulrich.kortz@aub.edu.lb
;
_publ_contact_author_fax
;
+961 1 744 461
;
_publ_contact_author_name
;
Ulrich KORTZ
;
_publ_contact_author_phone
;
+961 3 776 439
;
_publ_section_title
;
 Sandwich-Type Phosphotungstates: Structure, Electrochemistry, and
 Magnetism of the Trinickel-Substituted Polyoxoanion
 [Ni~3~Na(H~2~O)~2~(PW~9~O~34~)~2~]^11-^
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6412
_journal_page_last               6416
_journal_paper_doi               10.1021/ic0255353
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         Na7.5(Ni3NaP2W18O68)*23.25H2O
_chemical_formula_sum            'H46.5 Na8.5 Ni3 O91.25 P2 W18'
_chemical_formula_weight         5249.75
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.9870(10)
_cell_angle_beta                 87.6060(10)
_cell_angle_gamma                79.344(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2467(6)
_cell_length_b                   16.6031(7)
_cell_length_c                   22.4017(12)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.46
_cell_volume                     4302.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            46011
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    24.789
_exptl_absorpt_correction_T_max  0.3559
_exptl_absorpt_correction_T_min  0.1752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4539
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         5.255
_refine_diff_density_min         -2.178
_refine_diff_density_rms         0.436
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         21241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+117.2962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1292
_reflns_number_gt                16423
_reflns_number_total             21241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255353-2_s2.cif
_cod_data_source_block           u164abs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'H46.5 Na8.50 Ni3 O91.25 P2 W18'
_cod_database_code               4318931