Regioselective Benzyl Radical Addition to an Open-Shell Cluster Metallofullerene. Crystallographic Studies of Cocrystallized Sc3C2@Ih-C80 and Its Singly Bonded Derivative.
Fang, Hongyun; Cong, Hailin; Suzuki, Mitsuaki; Bao, Lipiao; Yu, Bing; Xie, Yunpeng; Mizorogi, Naomi; Olmstead, Marilyn M.; Balch, Alan L.; Nagase, Shigeru; Akasaka, Takeshi; Lu, Xing; Journal of the American Chemical Society 136 (2014) 10534–10540; doi:10.1021/ja505858y

data_4122259
_publ_section_title
;
 Regioselective Benzyl Radical Addition to an Open-Shell Cluster
 Metallofullerene. Crystallographic Studies of Cocrystallized Sc3C2@Ih-C80
 and Its Singly Bonded Derivative.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10534
_journal_page_last               10540
_journal_paper_doi               10.1021/ja505858y
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'Sc3C89H7, 1.5(CS2)'
_chemical_formula_sum            'C90.5 H7 S3 Sc3'
_chemical_formula_weight         1325.02
_chemical_name_common            Sc3C2@C80(C7H7)l1.5CS2
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 96.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.053(2)
_cell_length_b                   18.656(4)
_cell_length_c                   22.247(4)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      36.69
_cell_measurement_theta_min      2.43
_cell_volume                     4554.6(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            55165
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.123
_diffrn_reflns_theta_min         4.289
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 2012)'
_exptl_crystal_colour            black
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_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         12056
_refine_ls_number_restraints     770
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1701P)^2^+9.5479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2424
_refine_ls_wR_factor_ref         0.2535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10712
_reflns_number_total             12056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja505858y_si_003.cif
_cod_data_source_block           msnew3
_cod_depositor_comments
'Adding full bibliography for 4122259--4122260.cif.'
_cod_original_formula_sum        'C90.50 H7 S3 Sc3'
_cod_database_code               4122259
_shelx_estimated_absorpt_t_min   0.846
_shelx_estimated_absorpt_t_max   0.877
_shelxl_version_number           2014-3
_shelx_res_checksum              15304
_shelx_hkl_checksum              94068