The [MoFe3S4]2+ Oxidation State: Synthesis, Substitution Reactions, and Structures of Phosphine-Ligated Cubane-Type Clusters with the S = 2 Ground State
Bin Xi; R. H. Holm; Inorganic Chemistry 50 (2011) 6280–6288; doi:10.1021/ic200641k

data_4325527
_publ_section_title
;
 The [MoFe3S4]2+ Oxidation State: Synthesis, Substitution Reactions, and
 Structures of Phosphine-Ligated Cubane-Type Clusters with the S = 2
 Ground State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6280
_journal_page_last               6288
_journal_paper_doi               10.1021/ic200641k
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C21 H40 B Fe3 Mo N9 P2 S4'
_chemical_formula_weight         883.10
_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                75.9230(10)
_cell_angle_beta                 82.9910(10)
_cell_angle_gamma                73.1690(10)
_cell_formula_units_Z            4
_cell_length_a                   10.4374(5)
_cell_length_b                   15.5706(7)
_cell_length_c                   23.0073(10)
_cell_measurement_reflns_used    5605
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.523
_cell_volume                     3466.1(3)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS,2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS,2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS,2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30090
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.947
_exptl_absorpt_correction_T_max  0.9262
_exptl_absorpt_correction_T_min  0.5836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.974
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         13022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                8550
_reflns_number_total             13022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200641k_si_001_05.cif
_cod_data_source_block           N3
_cod_database_code               4325527