Synthesis and Redox Characterization of the Polyoxo Anion, γ*-[S2W18O62]4-: A Unique Fast Oxidation Pathway Determines the Characteristic Reversible Electrochemical Behavior of Polyoxometalate Anions in Acidic Media
Peter J. S. Richardt; Robert W. Gable; Alan M. Bond; Anthony G. Wedd; Inorganic Chemistry 40 (2001) 703–709; doi:10.1021/ic000793q

data_4319240
_publ_section_title
;
 Synthesis and Redox Characterization of the Polyoxo Anion,
 \g*-[S2W18O62]4-: A Unique Fast Oxidation Pathway Determines the
 Characteristic Reversible Electrochemical Behavior of Polyoxometalate
 Anions in Acidic Media
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              703
_journal_page_last               709
_journal_paper_doi               10.1021/ic000793q
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C68.92 H152.46 N6.46 O62.54 S2 W18'
_chemical_formula_weight         5445.97
_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   'not located'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.690(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.389(6)
_cell_length_b                   22.104(3)
_cell_length_c                   25.505(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.2
_cell_measurement_theta_min      11.1
_cell_volume                     12560(5)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCESS_DATA (Gable et al., 1993)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4MachS diffractometer'
_diffrn_measurement_method       \w:2\q
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12465
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        10
_diffrn_standards_interval_time  160
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    16.526
_exptl_absorpt_correction_T_max  0.3839
_exptl_absorpt_correction_T_min  0.1418
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Sheldrick, 1976'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.880
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             9902
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.898
_refine_diff_density_min         -2.629
_refine_diff_density_rms         0.312
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     915
_refine_ls_number_reflns         10991
_refine_ls_number_restraints     607
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0886P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                7249
_reflns_number_total             10991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000793q.cif
_cod_data_source_block           wedd_11
_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.

'_exptl_absorpt_correction_type' value 'Gaussian'
changed to 'gaussian' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4319240