Stabilization of Reduced Molybdenum-Iron-Sulfur Single- and Double-Cubane Clusters by Cyanide Ligation
Russell P. Pesavento; Curtis P. Berlinguette; R. H. Holm; Inorganic Chemistry 46 (2007) 510–516; doi:10.1021/ic061704y

data_4307158
_publ_section_title
;
Stabilization of Reduced Molybdenum-Iron-Sulfur Single- and
Double-Cubane Clusters by Cyanide Ligation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              510
_journal_page_last               516
_journal_paper_doi               10.1021/ic061704y
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C44 H82 B Fe3 Mo N11 S4'
_chemical_formula_sum            'C44 H82 B Fe3 Mo N11 S4'
_chemical_formula_weight         1161.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.934(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1891(15)
_cell_length_b                   40.210(5)
_cell_length_c                   12.596(3)
_cell_measurement_reflns_used    24104
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.41
_cell_measurement_theta_min      2.229
_cell_volume                     5612.9(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24104
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.167
_exptl_absorpt_correction_T_max  0.8001
_exptl_absorpt_correction_T_min  0.8001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.533
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         5868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          3.483
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+24.4057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1484
_reflns_number_gt                4819
_reflns_number_total             5868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061704ysi20060908_111817_1.cif
_cod_data_source_block           (Bu4N)2[(Tp)MoFe3S4(CN)3]
_cod_original_cell_volume        5612.7(17)
_cod_database_code               4307158