Single- and Double-Cubane Clusters in the Multiple Oxidation States [VFe3S4]3+,2+,1+
Christina Hauser; Eckhard Bill; R. H. Holm; Inorganic Chemistry 41 (2002) 1615–1624; doi:10.1021/ic011011b

data_4317722
_publ_contact_author
;
        R.H. Holm
        Department of Chemistry and Chemical Biology
        Harvard University
        Cambridge, MA 02138
        USA
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_contact_author_fax         '+1 (617) 496-9289'
_publ_contact_author_phone       '+1 (617) 495-0853'
_publ_section_title
;
 Single- and Double-Cubane Clusters in the Multiple Oxidation States
 [VFe3S4]3+,2+,1+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1615
_journal_page_last               1624
_journal_paper_doi               10.1021/ic011011b
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C42 H80 B2 Fe6 N12 P4 S8 V2'
_chemical_formula_sum            'C42 H80 B2 Fe6 N12 P4 S8 V2'
_chemical_formula_weight         1592.14
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 112.2380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3645(6)
_cell_length_b                   25.1144(14)
_cell_length_c                   12.7090(7)
_cell_measurement_temperature    213(2)
_cell_volume                     3357.5(3)
_computing_cell_refinement       'SMART, Version 5.618 (Bruker AXS, 2000)'
_computing_data_collection       'SMART, Version 5.618 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+, Version 6.02 (Bruker AXS, 1999)'
_computing_molecular_graphics    SHELTXTL-97
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area detector system'
_diffrn_measurement_method       '\o, 0.3 deg/frame'
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14271
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    1.907
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed by SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4395
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+15.5373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                3156
_reflns_number_total             4395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011011b_4.cif
_cod_data_source_block           '[5]'
_cod_database_code               4317722