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_4319122
_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            'Cu3 K12 O90 Sb2 W18'
_chemical_formula_weight         5652.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.2359(3)
_cell_length_b                   14.9889(2)
_cell_length_c                   19.1354(3)
_cell_measurement_reflns_used    36627
_cell_measurement_temperature    296(2)
_cell_volume                     8672.2(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 0.931
_diffrn_measured_fraction_theta_max 0.931
_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  0.0952
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58313
_diffrn_reflns_theta_full        29.72
_diffrn_reflns_theta_max         29.72
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.788
_exptl_absorpt_correction_T_max  0.1229
_exptl_absorpt_correction_T_min  0.0311
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             9876
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.549
_refine_diff_density_min         -3.228
_refine_diff_density_rms         0.498
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         11885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0875P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1522
_reflns_number_gt                8483
_reflns_number_total             11885
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000641v_4.cif
_cod_data_source_block           K12[Sb2W18{Cu(H2O)}3O66].41H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_database_code               4319122