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_4304787
_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)2 ((C9H10N6B)VFe3S4F3)(CH3CN)'
_chemical_formula_sum            'C27 H53 B F3 Fe3 N9 S4 V'
_chemical_formula_weight         918.08
_chemical_melting_point          ?
_chemical_name_common            'Floride vanadium single cubane'
_chemical_name_systematic
;
 bis(Tetraethylammoinum) 
 Tetrakis(\m3-sulfido)-trisfluorido-(hydrogen 
 tri(pyrazolyl)borato-N,N',N")-tri-iron-vanadium acetonitrile solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.1270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8425(6)
_cell_length_b                   16.8430(10)
_cell_length_c                   21.8996(13)
_cell_measurement_reflns_used    3489
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      2.51
_cell_volume                     3976.5(4)
_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 0.890
_diffrn_measured_fraction_theta_max 0.890
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13493
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.557
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0000(2)
_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   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         8110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          15.000
_refine_ls_shift/su_mean         0.036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.6702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                6068
_reflns_number_total             8110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702372f-file001_6.cif
_cod_data_source_block           ts201fu_0m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'not measured' 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_database_code               4304787