Crystallographic Characterization and Structural Analysis of the First Organic Functionalization Product of the Endohedral Fullerene Sc3N@C80
Hon Man Lee; Marilyn M. Olmstead; Erick Iezzi; James C. Duchamp; Harry C. Dorn; Alan L. Balch; Journal of the American Chemical Society 124 (2002) 3494–3495; doi:10.1021/ja020065x

data_4114722
_publ_section_title
;
 Crystallographic Characterization and Structural Analysis of the First
 Organic Functionalization Product of the Endohedral Fullerene Sc3N@C80
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3494
_journal_page_last               3495
_journal_paper_doi               10.1021/ja020065x
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C102 H24 N O2 Sc3'
_chemical_formula_weight         1430.10
_chemical_name_common            4,5-dimethoxyl-o-quinodimethane-Sc3N@C80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 117.548(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.972(7)
_cell_length_b                   14.196(5)
_cell_length_c                   20.986(8)
_cell_measurement_reflns_used    819
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      24.295
_cell_measurement_theta_min      2.188
_cell_volume                     5275(3)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXL 5.1 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \W
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2438
_diffrn_reflns_av_sigmaI/netI    0.2536
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            70657
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.9734
_exptl_absorpt_correction_T_min  0.9520
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_description       bipyramid
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         16838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.848
_refine_ls_R_factor_all          0.2161
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0511P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1513
_reflns_number_gt                6304
_reflns_number_total             16838
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja020065x.cif
_cod_data_source_block           hml02
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4114722