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_4317950
_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_moiety         alpha-P2W15O56(FeOH2)3
_chemical_formula_sum            'Fe3 Na7.5 O81 P2 W15'
_chemical_formula_weight         4455.67
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           1
_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                92.471(2)
_cell_angle_beta                 97.309(2)
_cell_angle_gamma                108.181(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8594(11)
_cell_length_b                   13.3491(12)
_cell_length_c                   22.2503(19)
_cell_measurement_reflns_used    8422
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.629
_cell_measurement_theta_min      2.182
_cell_volume                     3585.4(5)
_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 0.923
_diffrn_measured_fraction_theta_max 0.923
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.1183
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            61808
_diffrn_reflns_theta_full        32.76
_diffrn_reflns_theta_max         32.76
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    24.755
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.526029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.03, Sheldrick'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    4.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3897
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.035
_refine_diff_density_max         4.932
_refine_diff_density_min         -2.749
_refine_diff_density_rms         0.442
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.283(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1074
_refine_ls_number_reflns         46442
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                31386
_reflns_number_total             46442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0112443_2.cif
_cod_data_source_block           2
_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 Na7.50 O81 P2 W15'
_cod_database_code               4317950