Structural Characterization and Magnetic Properties of Sandwich-Type Tungstoarsenate Complexes. Study of a Mixed-Valent VIV2/VV Heteropolyanion
Pierre Mialane; Jérôme Marrot; Eric Rivière; Jérôme Nebout; Gilbert Hervé; Inorganic Chemistry 40 (2001) 44–48; doi:10.1021/ic000641v

data_4319120
_publ_section_title
;
 Structural Characterization and Magnetic Properties of Sandwich-Type
 Tungstoarsenate Complexes. Study of a Mixed-Valent VIV2/VV
 Heteropolyanion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              44
_journal_page_last               48
_journal_paper_doi               10.1021/ic000641v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'As2 Co3 H73.5 Na8 O103 W18'
_chemical_formula_weight         5541.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 98.935(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.124(2)
_cell_length_b                   23.294(3)
_cell_length_c                   32.247(3)
_cell_measurement_reflns_used    9353
_cell_measurement_temperature    296(2)
_cell_volume                     10481(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.762
_diffrn_measured_fraction_theta_max 0.762
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0873
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            17184
_diffrn_reflns_theta_full        29.72
_diffrn_reflns_theta_max         29.72
_diffrn_reflns_theta_min         1.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.898
_exptl_absorpt_correction_T_max  0.2857
_exptl_absorpt_correction_T_min  0.0818
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             9858
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.791
_refine_diff_density_min         -4.650
_refine_diff_density_rms         0.754
_refine_ls_extinction_coef       0.000073(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         11356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0732
_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^)+(0.1358P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2109
_reflns_number_gt                8512
_reflns_number_total             11356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000641v_2.cif
_cod_data_source_block           Na12[As2W18{Co(H2O)}3O66].34H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        'H73.50 As2 Co3 Na8 O103 W18'
_cod_database_code               4319120