VFe3S4 Single and Double Cubane Clusters: Synthesis, Structures, and Dependence of Redox Potentials and Electron Distribution on Ligation and Heterometal
Thomas A. Scott; R. H. Holm; Inorganic Chemistry 47 (2008) 3426–3432; doi:10.1021/ic702372f

data_4304786
_publ_contact_author_address
;Harvard University 
Department of Chemistry and Chemical Biology
12 Oxford St.
Cambridge, MA 02138
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_contact_author_fax         617-496-9289
_publ_contact_author_name        'R. H. Holm'
_publ_contact_author_phone       617-496-3215
_publ_section_title
;
VFe3S4 Single and Double Cubane Clusters: Synthesis, Structures, and
Dependence of Redox Potentials and Electron Distribution on Ligation and
Heterometal
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3426
_journal_page_last               3432
_journal_paper_doi               10.1021/ic702372f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         (Et4N)4[(C9H10N6B)2V2Fe6S8F4](CH3CN)8(H2O)3
_chemical_formula_sum            'C66 H130 B2 F4 Fe6 N24 O3 S8 V2'
_chemical_formula_weight         2098.36
_chemical_melting_point          ?
_chemical_name_common
'Fluoride Vanadium edge bridged double cubane'
_chemical_name_systematic
; 
tetrakis(n-ethylammonium) 
bis(\m~4~-sulfido)-hexakis(\m~3~-sulfido)-tetrafluoro-bis(hydrotris(pyrazolyl)
borato)-hexa-iron-di-vanadium acetonitrile solvate dihydrate 
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n 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            4
_cell_length_a                   14.743(2)
_cell_length_b                   29.397(4)
_cell_length_c                   11.0978(15)
_cell_measurement_reflns_used    4336
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      2.30
_cell_volume                     4809.8(11)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1610
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26410
_diffrn_reflns_theta_full        25.21
_diffrn_reflns_theta_max         25.21
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    2.539
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4512
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          5.650
_refine_ls_shift/su_mean         0.077
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.1934
_reflns_number_gt                3178
_reflns_number_total             4512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702372f-file001_5.cif
_cod_data_source_block           ortho
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 

The following automatic conversions were performed:

'_chemical_melting_point' value 'none' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4809.7(11)
_cod_database_code               4304786