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_4317952
_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
;
 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         Na14[(NiOH2)2Fe2(P2W15O56)2].24H2O
_chemical_formula_sum            'Fe2 H52 Na5 Ni2 O138 P4 W30'
_chemical_formula_weight         8243.87
_chemical_melting_point          ?
_chemical_name_common            'sandwich-type polyoxymetalate'
_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   'not included'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.553(2)
_cell_angle_beta                 96.024(2)
_cell_angle_gamma                118.480(2)
_cell_formula_units_Z            1
_cell_length_a                   13.7810(18)
_cell_length_b                   13.8779(18)
_cell_length_c                   21.444(3)
_cell_measurement_reflns_used    8866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.479
_cell_measurement_theta_min      2.384
_cell_volume                     3571.0(8)
_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_detector_area_resol_mean '83.333 pixels/mm'
_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  0.1063
_diffrn_reflns_av_sigmaI/netI    0.1491
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40806
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    24.667
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.532283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.03, Sheldrick'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.833
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             3599
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         6.021
_refine_diff_density_min         -3.586
_refine_diff_density_rms         0.635
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         12184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1475
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.1985
_reflns_number_gt                5926
_reflns_number_total             12184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0112443_4.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

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        'H52 Fe2 Na5 Ni2 O138 P4 W30'
_cod_database_code               4317952