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_4308146
_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            'C20 H161 Fe6 K9 N8 O162 Si3 W30'
_chemical_formula_weight         9393.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   20.3314(9)
_cell_length_b                   20.3314(9)
_cell_length_c                   33.390(3)
_cell_measurement_reflns_used    8934
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.54
_cell_measurement_theta_min      2.35
_cell_volume                     11953.1(13)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            107393
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    22.464
_exptl_absorpt_correction_T_max  0.4669
_exptl_absorpt_correction_T_min  0.1336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10, Sheldrick 2003'
_exptl_crystal_colour            light-green
_exptl_crystal_density_diffrn    3.915
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             12666
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.613
_refine_diff_density_min         -2.592
_refine_diff_density_rms         0.640
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.037(16)
_refine_ls_extinction_coef       0.000042(5)
_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   1.293
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         17405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0300P)^2^+800.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                16924
_reflns_number_total             17405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070126y-file003_2.cif
_cod_data_source_block           trimer
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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 
;
_cod_original_cell_volume        11953.3(12)
_cod_database_code               4308146