Reactions of Trivacant Wells-Dawson Heteropolytungstates. Ionic Strength and Jahn-Teller Effects on Formation in Multi-Iron Complexes
Travis M. Anderson; Xuan Zhang; Kenneth I. Hardcastle; Craig L. Hill; Inorganic Chemistry 41 (2002) 2477–2488; doi:10.1021/ic0112443

data_4317951
_publ_section_title
;
 Reactions of Trivacant Wells-Dawson Heteropolytungstates. Ionic Strength
 and Jahn-Teller Effects on Formation in Multi-Iron Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2477
_journal_page_last               2488
_journal_paper_doi               10.1021/ic0112443
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'Fe3 Na10.5 O143.5 P4 W30'
_chemical_formula_weight         8344.33
_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                109.9490(10)
_cell_angle_beta                 99.0410(10)
_cell_angle_gamma                93.7480(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7970(7)
_cell_length_b                   22.0512(12)
_cell_length_c                   24.5937(13)
_cell_measurement_reflns_used    9303
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.874
_cell_measurement_theta_min      2.343
_cell_volume                     6888.8(6)
_computing_cell_refinement       'Bruker SMART,SAINT'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0770
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            106050
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        'not measured'
_exptl_absorpt_coefficient_mu    25.433
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.549752
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    4.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7243
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.783
_refine_diff_density_min         -2.859
_refine_diff_density_rms         0.568
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1142
_refine_ls_number_reflns         27027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.285
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0900
_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^)+(0.0325P)^2^+968.2581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.1867
_reflns_number_gt                25002
_reflns_number_total             27027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0112443_3.cif
_cod_data_source_block           4
_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        'Fe3 Na10.50 O143.50 P4 W30'
_cod_database_code               4317951