Multi-Iron Silicotungstates: Synthesis, Characterization, and Stability Studies of Polyoxometalate Dimers
Travis M. Anderson; Wade A. Neiwert; Kenneth I. Hardcastle; Craig L. Hill; Inorganic Chemistry 43 (2004) 7353–7358; doi:10.1021/ic049517s

data_4312017
_publ_contact_author
;
    Craig L. Hill
    Department of Chemistry
    Emory University
    1515 Dickey Drive
    Atlanta, GA 30322
;
_publ_contact_author_email       chill@emory.edu
_publ_contact_author_fax         '404 727 6076'
_publ_contact_author_phone       '404 727 6611'
_publ_section_title
;
 Multi-Iron Silicotungstates: Synthesis, Characterization, and Stability
 Studies of Polyoxometalate Dimers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7353
_journal_page_last               7358
_journal_paper_doi               10.1021/ic049517s
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
'4(K 1+), 7(Na 1+), Si2 Fe6 W18 O77 H9 11-, 71.2 (H2 O)'
_chemical_formula_sum            'Fe6 H80.2 K4 Na7 O112.6 Si2 W18'
_chemical_formula_weight         5900.35
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.107(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.454(2)
_cell_length_b                   12.3872(12)
_cell_length_c                   37.421(2)
_cell_measurement_reflns_used    7064
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.31
_cell_volume                     10246.8(15)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            69622
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    21.278
_exptl_absorpt_correction_T_max  0.1685
_exptl_absorpt_correction_T_min  0.0723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10, Sheldrick 2003'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.825
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10600
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.121
_refine_diff_density_min         -2.790
_refine_diff_density_rms         0.401
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         12739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.247
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0067P)^2^+1147.0247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                11686
_reflns_number_total             12739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049517ssi20040413_034935_2.cif
_cod_data_source_block           fedarks
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'H80.20 O112.60 Fe6 K4 Na7 Si2 W18'
_cod_database_code               4312017