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_4317604
_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
'(C16 H36 N)2 (C9 H10 B1 Cl3 Fe3 Mo1 S4) (C2 H3 N)'
_chemical_formula_sum            'C43 H85 B Cl3 Fe3 Mo N9 S4'
_chemical_formula_weight         1237.09
_chemical_name_systematic
;

  ?

;
_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                 113.477(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7182(12)
_cell_length_b                   29.809(3)
_cell_length_c                   15.9875(15)
_cell_measurement_temperature    213(2)
_cell_volume                     5996.5(10)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0961
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40639
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed in SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          .431
_exptl_crystal_size_mid          .098
_exptl_crystal_size_min          .031
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         14594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1595
_reflns_number_gt                7795
_reflns_number_total             14594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011106d_5.cif
_cod_data_source_block           '[Bu4N]2[5].MeCN'
_cod_original_cell_volume        5996.4(9)
_cod_database_code               4317604