Reduced Mono-, Di-, and Tetracubane-Type Clusters Containing the [MoFe3S4]2+ Core Stabilized by Tertiary Phosphine Ligation
Frank Osterloh; Brent M. Segal; Catalina Achim; R. H. Holm; Inorganic Chemistry 39 (2000) 980–989; doi:10.1021/ic991016x

data_4300165
_publ_contact_author             R.H.Holm
_publ_contact_author_address
;
   R.H.Holm
   Dept. of Chemistry and Chemical Biology 
   Harvard University 
   Cambridge, MA 02138
   USA
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_section_title
;
Reduced Mono-, Di-, and Tetracubane-Type Clusters Containing the
[MoFe3S4]2+ Core Stabilized by Tertiary Phosphine Ligation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              980
_journal_page_last               989
_journal_paper_doi               10.1021/ic991016x
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C47 H90 Cl10 Fe3 Mo N O2 P3 S4'
_chemical_formula_weight         1540.34
_chemical_name_common            '[(Cl4cat)MoFe3S4(PBut3)3(CH3CN)].3CH2Cl2'
_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                 106.45(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.545(3)
_cell_length_b                   22.339(5)
_cell_length_c                   23.070(5)
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.81
_cell_volume                     6695(3)
_computing_cell_refinement       'SMART (Bruker, V4.050, 1995)'
_computing_data_collection       'ASTRO (Bruker, V4.050, 1995)'
_computing_data_reduction        'SAINT (Bruker, V5.A06, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998, ver 5.10)'
_computing_publication_material  'CIFTAB (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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Siemens CCD '
_diffrn_measurement_method       '\w, 0.3 deg'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35645
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.451
_exptl_absorpt_correction_T_max  0.970459
_exptl_absorpt_correction_T_min  0.793878
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic_block
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         11767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+6.9178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                9614
_reflns_number_total             11767
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        6695(2)
_cod_original_sg_symbol_H-M      'P 1 2/c 1'
_cod_database_code               4300165