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_4300168
_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            'C316 H496 B3 Cl Fe14 Mo4 N8 O16 P12 S16'
_chemical_formula_weight         6781.35
_chemical_name_common
'[{(Meida)MoFe3S4(PCy3)3}4Fe2(mu-Cl)(CH3CN)2](BPh4)3.2CH3CN'
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_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                   32.9623(3)
_cell_length_b                   32.9623(3)
_cell_length_c                   35.6578(4)
_cell_measurement_temperature    213(2)
_cell_volume                     38742.7(7)
_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_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            119695
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.970459
_exptl_absorpt_correction_T_min  0.777254
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular-block
_exptl_crystal_F_000             14980
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.462
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         12682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+247.3292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2129
_refine_ls_wR_factor_ref         0.2373
_reflns_number_gt                9872
_reflns_number_total             12682
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4300168