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_4306608
_publ_contact_author
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      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
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_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
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Octa- and Nonanuclear Nickel(II) Polyoxometalate Clusters: Synthesis and
Electrochemical and Magnetic Characterizations
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_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            'C12 H18 N6 Na16 Ni8 O121 Si2 W18'
_chemical_formula_weight         6385.32
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.9660(7)
_cell_length_b                   11.9660(7)
_cell_length_c                   72.753(7)
_cell_measurement_reflns_used    9102
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      2.26
_cell_volume                     9021.5(11)
_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      100(2)
_diffrn_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       102
_diffrn_reflns_limit_l_min       -102
_diffrn_reflns_number            113265
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         0.84
_exptl_absorpt_coefficient_mu    18.557
_exptl_absorpt_correction_T_max  0.7079
_exptl_absorpt_correction_T_min  0.2584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             8580
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.804
_refine_diff_density_min         -3.740
_refine_diff_density_rms         0.676
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.263
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5901
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.263
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+131.1312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                5379
_reflns_number_total             5901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801431f_si_003_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
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_sg_symbol_H-M      'R -3'
_cod_database_code               4306608