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_4104832
_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 B Co8 F4 P6 S8'
_chemical_formula_weight         1776.10
_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                86.0850(10)
_cell_angle_beta                 81.2200(10)
_cell_angle_gamma                88.4730(10)
_cell_formula_units_Z            6
_cell_length_a                   13.5596(7)
_cell_length_b                   20.8973(10)
_cell_length_c                   41.467(2)
_cell_measurement_temperature    193(2)
_cell_volume                     11583.7(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66596
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    2.057
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            BROWN
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             5550
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.348
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2397
_refine_ls_number_reflns         40596
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                28603
_reflns_number_total             40596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903847a_si_002_7.cif
_cod_data_source_block           8(BF4)
_cod_database_code               4104832