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_4327502
_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(depe)2Cl}2(u-depe)
_chemical_formula_sum            'C62 H120 Cl10 Fe6 Mo2 O4 P10 S8'
_chemical_formula_weight         2377.24
_chemical_name_common
'MoFe3 singly bridged double cubane with depe'
_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            4
_cell_length_a                   23.420(5)
_cell_length_b                   17.376(4)
_cell_length_c                   23.773(5)
_cell_measurement_temperature    293(2)
_cell_volume                     9674(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.6328
_diffrn_reflns_av_sigmaI/netI    0.1394
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6355
_diffrn_reflns_theta_full        22.55
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.778
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             4848
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1838
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_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          0.1664
_refine_ls_wR_factor_ref         0.2092
_reflns_number_gt                2490
_reflns_number_total             6354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0109132B_1.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        9674(3)
_cod_database_code               4327502