Octa- and Nonanuclear Nickel(II) Polyoxometalate Clusters: Synthesis and Electrochemical and Magnetic Characterizations
Céline Pichon; Pierre Mialane; Anne Dolbecq; Jérôme Marrot; Eric Rivière; Bassem S. Bassil; Ulrich Kortz; Bineta Keita; Louis Nadjo; Francis Sécheresse; Inorganic Chemistry 47 (2008) 11120–11128; doi:10.1021/ic801431f

data_4306609
_publ_contact_author
; 
      Dr P. Mialane
      Institut Lavoisier de Versailles, UMR 8180
      Universit\'e de Versailles Saint-Quentin-en-Yvelines
      45 Avenue des Etats Unis
      78035 Versailles cedex
      France
;
_publ_contact_author_email       mialane@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_phone       '(33) 1 39 25 43 83'
_publ_section_title
;
Octa- and Nonanuclear Nickel(II) Polyoxometalate Clusters: Synthesis and
Electrochemical and Magnetic Characterizations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11120
_journal_page_last               11128
_journal_paper_doi               10.1021/ic801431f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C3 K9.75 Na1.25 Ni9 O107.5 Si2 W18'
_chemical_formula_weight         6059.86
_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                63.423(2)
_cell_angle_beta                 73.4760(10)
_cell_angle_gamma                89.820(2)
_cell_formula_units_Z            2
_cell_length_a                   13.6466(5)
_cell_length_b                   22.9583(8)
_cell_length_c                   23.2340(8)
_cell_measurement_reflns_used    8077
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.35
_cell_volume                     6175.5(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_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_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            123932
_diffrn_reflns_theta_full        30.11
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    18.475
_exptl_absorpt_correction_T_max  0.5253
_exptl_absorpt_correction_T_min  0.1681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5378
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.596
_refine_diff_density_min         -5.340
_refine_diff_density_rms         0.724
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1429
_refine_ls_number_reflns         35749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1054P)^2^+71.5244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1938
_reflns_number_gt                24091
_reflns_number_total             35749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801431f_si_003_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C3 K9.75 Na1.25 Ni9 O107.50 Si2 W18'
_cod_database_code               4306609