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_4307159
_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         'C38 H73 B Fe3 Mo N13 S4'
_chemical_formula_sum            'C38 H73 B Fe3 Mo N13 S4'
_chemical_formula_weight         1116.22
_chemical_name_common            (Et4N)3(C9BH10N6)MoFe3S4(CN)3(MeCN)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.51(4)
_cell_angle_beta                 75.03(3)
_cell_angle_gamma                66.86(3)
_cell_formula_units_Z            2
_cell_length_a                   12.790(5)
_cell_length_b                   13.476(7)
_cell_length_c                   17.120(6)
_cell_measurement_reflns_used    18546
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.735
_cell_measurement_theta_min      3.300
_cell_volume                     2607(2)
_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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18546
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  0.5731
_exptl_absorpt_correction_T_min  0.5203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1122
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.0000(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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         12225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          8.630
_refine_ls_shift/su_mean         0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+2.9573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                9920
_reflns_number_total             12225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061704ysi20060908_111817_2.cif
_cod_data_source_block           (Et4N)3[(Tp)MoFe3S4(CN)3]
_cod_database_code               4307159