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_4319119
_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 H60 K10.94 Mn3 Na1.06 O96 W18'
_chemical_formula_weight         5672.56
_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                   30.6484(4)
_cell_length_b                   14.9946(2)
_cell_length_c                   19.17080(10)
_cell_measurement_reflns_used    31426
_cell_measurement_temperature    296(2)
_cell_volume                     8810.14(17)
_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 0.935
_diffrn_measured_fraction_theta_max 0.935
_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  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59318
_diffrn_reflns_theta_full        29.75
_diffrn_reflns_theta_max         29.75
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.201
_exptl_absorpt_correction_T_max  0.4322
_exptl_absorpt_correction_T_min  0.0813
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             10082
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.149
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.380
_refine_ls_extinction_coef       0.000024(2)
_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   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         12160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+119.2879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                8698
_reflns_number_total             12160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000641v_1.cif
_cod_data_source_block           K11Na1[As2W18{Mn(H2O)}3O66].27H2O
_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_original_formula_sum        'H60 As2 K10.94 Mn3 Na1.06 O96 W18'
_cod_database_code               4319119