A pirouette on a metallofullerene sphere: interconversion of isomers of N-tritylpyrrolidino I(h) Sc3N@C80.
Cai, Ting; Slebodnick, Carla; Xu, Liaosa; Harich, Kim; Glass, Thomas E; Chancellor, Christopher; Fettinger, James C; Olmstead, Marilyn M; Balch, Alan L; Gibson, Harry W; Dorn, Harry C; Journal of the American Chemical Society 128 (2006) 6486–6492; doi:10.1021/ja0601843

data_4101474
_publ_section_title
;
 A pirouette on a metallofullerene sphere: interconversion of isomers
 of N-tritylpyrrolidino I(h) Sc3N@C80.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6486
_journal_page_last               6492
_journal_paper_doi               10.1021/ja0601843
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         '(C101 H19 N2 Sc3), 2.25(C S2), 0.75(C6 H6)'
_chemical_formula_sum            'C107.75 H23.5 N2 S4.5 Sc3'
_chemical_formula_weight         1624.94
_chemical_name_common
'Sc3N@N-trityl-3,4-fullero[C80]pyrrolidine, 2.25CS2, 0.75benzene solvate'
_chemical_name_systematic
; 
 ? 
;
_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                99.521(1)
_cell_angle_beta                 106.034(1)
_cell_angle_gamma                102.488(1)
_cell_formula_units_Z            2
_cell_length_a                   11.0127(8)
_cell_length_b                   16.3870(8)
_cell_length_c                   18.7355(11)
_cell_measurement_reflns_used    8425
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.5
_cell_volume                     3080.0(3)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       \w
_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    0.0653
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35232
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2004)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1638
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.016
_refine_diff_density_max         1.819
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1214
_refine_ls_number_reflns         14160
_refine_ls_number_restraints     463
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1408
_refine_ls_R_factor_gt           0.0987
_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^)+(0.1728P)^2^+4.7778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2809
_refine_ls_wR_factor_ref         0.3050
_reflns_number_gt                9232
_reflns_number_total             14160
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0601843si20060324_072944.cif
_cod_data_source_block           cjc91z
_cod_original_formula_sum        'C107.75 H23.50 N2 S4.50 Sc3'
_cod_database_code               4101474