Synthesis and Structure of Singly Bridged and Doubly Bridged [MoFe3S4] Double Cubanes with Bidentate Phosphine Ligands
Jaehong Han; Dimitri Coucouvanis; Inorganic Chemistry 41 (2002) 2738–2746; doi:10.1021/ic010913+

data_4327503
_publ_section_title
;
 Synthesis and Structure of Singly Bridged and Doubly Bridged [MoFe3S4]
 Double Cubanes with Bidentate Phosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2738
_journal_page_last               2746
_journal_paper_doi               10.1021/ic010913+
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         {(Cl4-cat)MoFe3S4(dmpe)2}2(u-S)(u-dmpe)
_chemical_formula_sum            'C55 H105 Cl22 Fe6 Mo2 O4 P10 S9'
_chemical_formula_weight         2735.51
_chemical_name_common
'MoFe3 doubly bridged double cubane with dmpe and S brigding ligands'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   25.5705(3)
_cell_length_b                   24.9521(3)
_cell_length_c                   32.8954(4)
_cell_measurement_temperature    158(2)
_cell_volume                     20988.5(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.1321
_diffrn_reflns_av_sigmaI/netI    0.0954
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            207708
_diffrn_reflns_theta_full        29.46
_diffrn_reflns_theta_max         29.46
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.966
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       plate
_exptl_crystal_F_000             11000
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.511
_refine_diff_density_min         -1.370
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         27411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.1736
_refine_ls_R_factor_gt           0.1188
_refine_ls_shift/su_max          0.242
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2121
_refine_ls_wR_factor_ref         0.2347
_reflns_number_gt                18633
_reflns_number_total             27411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0109132B_2.cif
_cod_data_source_block           compound6
_cod_database_code               4327503