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_4304785
_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)VFe3S4(N3)3)'
_chemical_formula_sum            'C25 H50 B Fe3 N17 S4 V'
_chemical_formula_weight         946.09
_chemical_melting_point          ?
_chemical_name_common            'Azide vanadium single cubane'
_chemical_name_systematic
;
 bis(Tetraethylammoinum) 
 Tetrakis(\m3-sulfido)-trisazido-(hydrogen 
 tri(pyrazolyl)borato-N,N',N")-tri-iron-vanadium
;
_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                 108.308(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   23.671(8)
_cell_length_b                   34.548(12)
_cell_length_c                   15.700(5)
_cell_measurement_reflns_used    986
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.77
_cell_volume                     12189(7)
_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 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.1090
_diffrn_reflns_av_sigmaI/netI    0.1531
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            80994
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         0.91
_exptl_absorpt_coefficient_mu    1.522
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5868
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1414
_refine_ls_number_reflns         29462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1715
_refine_ls_R_factor_gt           0.0795
_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^)+(0.0360P)^2^+11.7127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1566
_reflns_number_gt                14703
_reflns_number_total             29462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702372f-file001_4.cif
_cod_data_source_block           ts1151bsad1
_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               4304785