Cubane-Type Co4S4 Clusters: Synthesis, Redox Series, and Magnetic Ground States
Liang Deng; Eckhard Bill; Karl Wieghardt; R. H. Holm; Journal of the American Chemical Society 131 (2009) 11213–11221; doi:10.1021/ja903847a

data_4104831
_publ_section_title
;
 Cubane-Type Co4S4 Clusters: Synthesis, Redox Series, and Magnetic Ground
 States
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11213
_journal_page_last               11221
_journal_paper_doi               10.1021/ja903847a
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C54 H126 Co8 P6 S8'
_chemical_formula_weight         1689.29
_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                73.9600(10)
_cell_angle_beta                 84.7400(10)
_cell_angle_gamma                64.2290(10)
_cell_formula_units_Z            1
_cell_length_a                   12.3518(6)
_cell_length_b                   12.4877(6)
_cell_length_c                   13.9495(7)
_cell_measurement_reflns_used    6495
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1861.20(16)
_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_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker CC'
_diffrn_measurement_method       '\w, 0.3 deg'
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10593
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.122
_exptl_absorpt_correction_T_max  0.8486
_exptl_absorpt_correction_T_min  0.6762
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          5.300
_refine_ls_shift/su_mean         0.104
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+1.7746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                5783
_reflns_number_total             6534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903847a_si_002_6.cif
_cod_data_source_block           7
_cod_database_code               4104831