Tetrairon and Hexairon Hydroxo/Acetato Clusters Stabilized by Multiple Polyoxometalate Scaffolds. Structures, Magnetic Properties, and Chemistry of a Dimer and a Trimer
Bogdan Botar; Paul Kögerler; Craig L. Hill; Inorganic Chemistry 46 (2007) 5398–5403; doi:10.1021/ic070126y

data_4308145
_publ_contact_author_address
;
Emory University
Department of Chemistry
Atlanta GA 30322-2210
USA
;
_publ_contact_author_email       bbotar@emory.edu
_publ_contact_author_fax         404-727-6076
_publ_contact_author_name        'Bogdan Botar'
_publ_contact_author_phone       404-727-4419
_publ_section_title
;
Tetrairon and Hexairon Hydroxo/Acetato Clusters Stabilized by Multiple
Polyoxometalate Scaffolds. Structures, Magnetic Properties, and Chemistry
of a Dimer and a Trimer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5398
_journal_page_last               5403
_journal_paper_doi               10.1021/ic070126y
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C24 H112 Fe4 K4 N8 O100 Si2 W20'
_chemical_formula_weight         6226.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.430(2)
_cell_length_b                   37.430(2)
_cell_length_c                   19.6822(14)
_cell_measurement_reflns_used    8864
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.91
_cell_measurement_theta_min      2.21
_cell_volume                     27575(3)
_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      173(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  0.1191
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            218748
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    17.248
_exptl_absorpt_correction_T_max  0.2774
_exptl_absorpt_correction_T_min  0.1963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10, Sheldrick 2003'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.999
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             22400
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         6.386
_refine_diff_density_min         -2.942
_refine_diff_density_rms         0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         20749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1072P)^2^+67.8407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1898
_reflns_number_gt                13798
_reflns_number_total             20749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070126y-file003_1.cif
_cod_data_source_block           dimer
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 
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_cod_database_code               4308145