Synthesis and Characterization of Iron()-Substituted, Dimeric Polyoxotungstates, [Fe~4~(H~2~O)~10~(β-XW~9~O~33~)~2~]^n-^ (n = 6, X = As^III^, Sb^III^; n = 4, X = Se^IV^, Te^IV^)
Ulrich Kortz; Masha G. Savelieff; Bassem S. Bassil; Bineta Keita; Louis Nadjo; Inorganic Chemistry 41 (2002) 783–789; doi:10.1021/ic010855s

data_4317568
_publ_contact_author_address
;
Department of Chemistry
American University of Beirut
P.O. Box: 11-0236
Riad El Solh Beirut 1107 2020
LEBANON
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_publ_contact_author_email
;
ulrich.kortz@aub.edu.lb
;
_publ_contact_author_fax
;
+961 1 744 461
;
_publ_contact_author_name
;
Ulrich KORTZ
;
_publ_contact_author_phone
;
+961 3 776 439
;
_publ_section_title
;
 Synthesis and Characterization of Iron()-Substituted, Dimeric
 Polyoxotungstates, [Fe~4~(H~2~O)~10~(\b-XW~9~O~33~)~2~]^n-^ (n = 6, X =
 As^III^, Sb^III^; n = 4, X = Se^IV^, Te^IV^)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              783
_journal_page_last               789
_journal_paper_doi               10.1021/ic010855s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'As2 Fe4 H84 Na6 O108 W18'
_chemical_formula_weight         5633.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.766(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.2493(18)
_cell_length_b                   15.2678(13)
_cell_length_c                   16.0689(14)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    167(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.17
_cell_volume                     4942.8(7)
_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      167(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28497
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.27
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    22.231
_exptl_absorpt_correction_T_max  0.1451
_exptl_absorpt_correction_T_min  0.0727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.799
_refine_diff_density_min         -5.394
_refine_diff_density_rms         0.530
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         6282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0600P)^2^+532.6932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1565
_reflns_number_gt                5360
_reflns_number_total             6282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010855s_2.cif
_cod_data_source_block           u63abs
_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_database_code               4317568