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_4300166
_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_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C35 H66 Cl4 Fe3 Mo N O2 P3 S4'
_chemical_formula_weight         1159.33
_chemical_name_common            '[(Cl4cat)(CH3CN)MoFe3S4(PPri)3]'
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                   23.493(1)
_cell_length_b                   11.4994(6)
_cell_length_c                   18.265(1)
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      1.97
_cell_volume                     4934.4(4)
_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 0.898
_diffrn_measured_fraction_theta_max 0.898
_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  0.1214
_diffrn_reflns_av_sigmaI/netI    0.1780
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29881
_diffrn_reflns_theta_full        27.76
_diffrn_reflns_theta_max         27.76
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_T_max  0.977621
_exptl_absorpt_correction_T_min  0.838394
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         10047
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.2038
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1711
_reflns_number_gt                4163
_reflns_number_total             10047
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        4934.2(4)
_cod_database_code               4300166
_journal_paper_doi 10.1021/ic991016x