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_4327504
_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         Fe(dmpe)2(MeCN)Cl
_chemical_formula_sum            'C38 H55 B Cl Fe N P4'
_chemical_formula_weight         751.82
_chemical_name_systematic
;
  Iron bis(bis(dimethylphosphino)ethane)acetonitrilechloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.781(3)
_cell_length_b                   14.847(3)
_cell_length_c                   18.490(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4043.8(15)
_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 0.517
_diffrn_measured_fraction_theta_max 0.517
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2894
_diffrn_reflns_theta_full        22.54
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.309
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.624
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         2749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.624
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.1042
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_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          0.3264
_refine_ls_wR_factor_ref         0.3432
_reflns_number_gt                2267
_reflns_number_total             2749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0109132B_3.cif
_cod_data_source_block           compound7
_cod_original_cell_volume        4043.6(14)
_cod_database_code               4327504