Structural Elucidation and Regioselective Functionalization of An Unexplored Carbide Cluster Metallofullerene Sc2C2@Cs(6)-C82
Xing Lu; Koji Nakajima; Yuko Iiduka; Hidefumi Nikawa; Naomi Mizorogi; Zdenek Slanina; Takahiro Tsuchiya; Shigeru Nagase; Takeshi Akasaka; Journal of the American Chemical Society 133 (2011) 19553–19558; doi:10.1021/ja208841w

data_4107185
_publ_section_title
;
 Structural Elucidation and Regioselective Functionalization of An
 Unexplored Carbide Cluster Metallofullerene Sc2C2@Cs(6)-C82
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19553
_journal_page_last               19558
_journal_paper_doi               10.1021/ja208841w
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'Sc2 C84 C21H19N 1.5(C6H14) 0.5(C7H8)'
_chemical_formula_sum            'C117.5 H44 N Sc2'
_chemical_formula_weight         1559.46
_chemical_name_common            Sc2C2@Cs(6)-C82Triphenyle
_chemical_name_systematic
; 
 Sc2C2@Cs(6)-C82Triphenylemethyl pyrrolidine 
;
_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                71.951(5)
_cell_angle_beta                 73.731(5)
_cell_angle_gamma                77.086(5)
_cell_formula_units_Z            2
_cell_length_a                   11.048(4)
_cell_length_b                   16.791(6)
_cell_length_c                   19.079(7)
_cell_measurement_temperature    100(2)
_cell_volume                     3194(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11023
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_T_max  0.9916
_exptl_absorpt_correction_T_min  0.9561
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0056(7)
_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   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1383
_refine_ls_number_reflns         7811
_refine_ls_number_restraints     5793
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.1589
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0855P)^2^+13.8946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2478
_reflns_number_gt                4586
_reflns_number_total             7811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja208841w_si_002.cif
_cod_data_source_block           Sc2C2@Cs(6)-C82Triphenyle
_cod_original_cell_volume        3194.1(19)
_cod_original_formula_sum        'C117.50 H44 N Sc2'
_cod_database_code               4107185