Highly Regioselective Derivatization of Trimetallic Nitride Templated Endohedral Metallofullerenes via a Facile Photochemical Reaction
Chunying Shu; Carla Slebodnick; Liaosa Xu; Hunter Champion; Tim Fuhrer; Ting Cai; Jonathan E. Reid; Wujun Fu; Kim Harich; Harry C. Dorn; Harry W. Gibson; Journal of the American Chemical Society 130 (2008) 17755–17760; doi:10.1021/ja804909t

data_4108916
_publ_section_title
;
 Highly Regioselective Derivatization of Trimetallic Nitride Templated
 Endohedral Metallofullerenes via a Facile Photochemical Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17755
_journal_page_last               17760
_journal_paper_doi               10.1021/ja804909t
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C94 H14 N Sc3, C7 H8'
_chemical_formula_sum            'C101 H22 N Sc3'
_chemical_formula_weight         1384.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0377(4)
_cell_length_b                   18.4948(8)
_cell_length_c                   25.2391(7)
_cell_measurement_reflns_used    4564
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.6197
_cell_measurement_theta_min      2.9643
_cell_volume                     5152.3(3)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_publication_material
'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_structure_refinement
'SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_structure_solution
'SIR92 (Altomare, A. et al. (1993) J. Appl. Cryst. 26, 343-350)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.3174
_diffrn_detector_type            'Oxford Diffraction Onyx CCD'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Nova'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19675
_diffrn_reflns_theta_full        62.50
_diffrn_reflns_theta_max         63.75
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'Nova Micro-focus X-ray Source (Cu)'
_diffrn_source_current           0.95
_diffrn_source_voltage           49.5
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    3.864
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       needle
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.981
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.329
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.329
_refine_ls_R_factor_all          0.1738
_refine_ls_R_factor_gt           0.1281
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3527
_refine_ls_wR_factor_ref         0.3839
_reflns_number_gt                2597
_reflns_number_total             4227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja804909t_si_001.cif
_cod_data_source_block           cs1225
_cod_database_code               4108916