Multi-Iron Tungstodiarsenates. Synthesis, Characterization, and Electrocatalytic Studies of αββα-(FeIIIOH2)2FeIII2(As2W15O56)212-
Israel Martyr Mbomekalle; Bineta Keita; Louis Nadjo; Patrick Berthet; Kenneth I. Hardcastle; Craig L. Hill; Travis M. Anderson; Inorganic Chemistry 42 (2003) 1163–1169; doi:10.1021/ic0261169

data_4313185
_publ_contact_author_address
; 
Emory University 
Department of Chemistry 
X-ray Crystallography Laboratory 
Atlanta GA 30322-2210 
USA 
;
_publ_contact_author_email       khardca@emory.edu
_publ_contact_author_fax         404-727-6586
_publ_contact_author_name        'Kenneth I. Hardcastle'
_publ_contact_author_phone       404-727-6140
_publ_section_title
;
 Multi-Iron Tungstodiarsenates. Synthesis, Characterization, and
 Electrocatalytic Studies of \a\b\b\a-(FeIIIOH2)2FeIII2(As2W15O56)212-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1163
_journal_page_last               1169
_journal_paper_doi               10.1021/ic0261169
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety
'Na11 O53.5 11+, H3 O 1+. As4 Fe4 O114 W30 12-'
_chemical_formula_sum            'As4 Fe4 Na11 O167.5 W30'
_chemical_formula_weight         8971.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.246(2)
_cell_angle_beta                 102.887(2)
_cell_angle_gamma                116.9720(10)
_cell_formula_units_Z            1
_cell_length_a                   13.4341(11)
_cell_length_b                   13.7628(11)
_cell_length_c                   22.9990(18)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.05
_cell_measurement_theta_min      2.32
_cell_volume                     3667.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_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  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            62284
_diffrn_reflns_theta_full        33.08
_diffrn_reflns_theta_max         33.08
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    24.858
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.225765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick 1996'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.063
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3917
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         7.697
_refine_diff_density_min         -4.018
_refine_diff_density_rms         0.702
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         25342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0848P)^2^+13.9572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1554
_reflns_number_gt                21112
_reflns_number_total             25342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0261169-2_s2.cif
_cod_data_source_block           ta1s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        'As4 Fe4 Na11 O167.50 W30'
_cod_database_code               4313185