Heterometal Cubane-Type MFe3S4 Clusters (M = Mo, V) Trigonally Symmetrized with Hydrotris(pyrazolyl)borate(1-) and Tris(pyrazolyl)methanesulfonate(1-) Capping Ligands
Dmitry V. Fomitchev; Craig C. McLauchlan; R. H. Holm; Inorganic Chemistry 41 (2002) 958–966; doi:10.1021/ic011106d

data_4317605
_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
;
 Heterometal Cubane-Type MFe3S4 Clusters (M = Mo, V) Trigonally
 Symmetrized with Hydrotris(pyrazolyl)borate(1-) and
 Tris(pyrazolyl)methanesulfonate(1-) Capping Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              958
_journal_page_last               966
_journal_paper_doi               10.1021/ic011106d
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '(C10 H9 Cl3 Fe3 N6 O3 S5 V) (C4 H12 N)2'
_chemical_formula_sum            'C18 H33 Cl3 Fe3 N8 O3 S5 V'
_chemical_formula_weight         894.66
_chemical_name_systematic
;

  ?

;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   9.1692(18)
_cell_length_b                   15.161(3)
_cell_length_c                   24.777(5)
_cell_measurement_temperature    213(2)
_cell_volume                     3444.4(12)
_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    SHELXTL
_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 0.792
_diffrn_measured_fraction_theta_max 0.792
_diffrn_measurement_device_type
'Bruker P4 with SMART CCD area detector system'
_diffrn_measurement_method       '\p, \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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            9584
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    2.073
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed in SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0328
_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

  1/[\s^2^(Fo^2^)+(0.0306Fo^2^)^2^]

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                4935
_reflns_number_total             5771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011106d_6.cif
_cod_data_source_block           '[Me4N]2[8]'
_cod_original_cell_volume        3444.2(12)
_cod_database_code               4317605