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_4317949
_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_sum            'Cl2 Fe3 H0 Na5.93 O88 P2 W15'
_chemical_formula_weight         4602.36
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.139(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3430(15)
_cell_length_b                   28.535(3)
_cell_length_c                   21.574(2)
_cell_measurement_reflns_used    9102
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.642
_cell_measurement_theta_min      2.340
_cell_volume                     8208.4(15)
_computing_cell_refinement       'Bruker 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 0.943
_diffrn_measured_fraction_theta_max 0.943
_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  0.1839
_diffrn_reflns_av_sigmaI/netI    0.1099
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            146918
_diffrn_reflns_theta_full        32.94
_diffrn_reflns_theta_max         32.94
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    21.695
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.415104
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'yellow orange'
_exptl_crystal_density_diffrn    3.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irreg
_exptl_crystal_F_000             8085
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         8.956
_refine_diff_density_min         -6.796
_refine_diff_density_rms         0.874
_refine_ls_extinction_coef       0.000015(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         29048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2351
_refine_ls_wR_factor_ref         0.2488
_reflns_number_gt                19884
_reflns_number_total             29048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0112443_1.cif
_cod_data_source_block           1
_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_original_cell_volume        8208.3(16)
_cod_original_formula_sum        'H0 Cl2 Fe3 Na5.93 O88 P2 W15'
_cod_database_code               4317949