Selective Synthesis of Co8S15 Cluster in Bowl-Shaped Template of the Pentaaryl[60]fullerene Ligand
Masashi Maruyama; Kenta Imoto; Matthias König; Dirk M. Guldi; Shin-ichi Ohkoshi; Eiichi Nakamura; Yutaka Matsuo; Journal of the American Chemical Society 135 (2013) 10914–10917; doi:10.1021/ja405045t

data_4120217
_publ_section_title
;
 Selective Synthesis of Co8S15 Cluster in Bowl-Shaped Template of the
 Pentaaryl[60]fullerene Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10914
_journal_page_last               10917
_journal_paper_doi               10.1021/ja405045t
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C246 H148 Co8 S15'
_chemical_formula_weight         4055.98
_space_group_IT_number           14
_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                 98.9220(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.5786(4)
_cell_length_b                   32.8041(6)
_cell_length_c                   31.8927(6)
_cell_measurement_temperature    223(2)
_cell_volume                     20235.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1651
_diffrn_reflns_av_sigmaI/netI    0.2603
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            225535
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    6.878
_exptl_absorpt_correction_T_max  0.5463
_exptl_absorpt_correction_T_min  0.5463
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_F_000             8320
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.489
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00042(2)
_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   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2359
_refine_ls_number_reflns         35983
_refine_ls_number_restraints     1157
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.2776
_refine_ls_R_factor_gt           0.1147
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2168
_refine_ls_wR_factor_ref         0.2918
_reflns_number_gt                11588
_reflns_number_total             35983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405045t_si_002.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4120217