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_4317601
_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_sum            'C25 H46 B Cl3 Fe3 Mo N7 S4'
_chemical_formula_weight         953.58
_chemical_name_systematic
;

  ?

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.04(3)
_cell_angle_beta                 103.88(3)
_cell_angle_gamma                115.80(3)
_cell_formula_units_Z            2
_cell_length_a                   10.205(2)
_cell_length_b                   11.452(2)
_cell_length_c                   19.570(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1973.2(9)
_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-97 (Bruker AXS, 1997)'
_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 0.861
_diffrn_measured_fraction_theta_max 0.861
_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  0.0883
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12703
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    1.834
_exptl_absorpt_process_details   'performed in SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             970
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.929
_refine_diff_density_min         -1.548
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         8088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0660P)^2^+0.4903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                6206
_reflns_number_total             8088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011106d_2.cif
_cod_data_source_block           '[Bu4N][1]'
_cod_original_cell_volume        1973.2(7)
_cod_database_code               4317601