Azide Addition to an Endohedral Metallofullerene: Formation of Azafulleroids of Sc3N@Ih-C80
Tong-Xin Liu; Tao Wei; San-E Zhu; Guan-Wu Wang; Mingzhi Jiao; Shangfeng Yang; Faye L. Bowles; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 134 (2012) 11956–11959; doi:10.1021/ja305446v

data_4118381
_publ_section_title
;
 Azide Addition to an Endohedral Metallofullerene: Formation of
 Azafulleroids of Sc3N@Ih-C80
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11956
_journal_page_last               11959
_journal_paper_doi               10.1021/ja305446v
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         ' C89 H11 N2 O Sc3, 0.88(C6 H6), 0.12(C S2)'
_chemical_formula_sum            'C94.4 H16.27 N2 O S0.24 Sc3'
_chemical_formula_weight         1336.75
_chemical_name_common
'(5,6)Sc3N@C80N-(4-isopropoxyphenyl)nitrene 0.88 benzene 0.12 CS2 '
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-05-06 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.033(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.5387(5)
_cell_length_b                   17.1238(6)
_cell_length_c                   38.6297(13)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.477
_cell_measurement_theta_min      2.205
_cell_volume                     9497.9(6)
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_collection       'Apex2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            104836
_diffrn_reflns_theta_full        40.15
_diffrn_reflns_theta_max         40.15
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.9977
_exptl_absorpt_correction_T_min  0.9687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_description       plate
_exptl_crystal_F_000             5372
_exptl_crystal_size_max          0.064
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         22470
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0740P)^2^+13.2834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1580
_reflns_number_gt                18357
_reflns_number_total             22470
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja305446v_si_001.cif
_cod_data_source_block           fb48
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C94.40 H16.27 N2 O S0.24 Sc3'
_cod_database_code               4118381