Hemicarceplex formation allows ready identification of the isomers of the metallofullerene Sc3N@C80 using 1H and 13C NMR spectroscopy
Min-Yen Ku; Shing-Jong Huang; Shou-Ling Huang; Yi-Hung Liu; Chien-Chen Lai; Shie-Ming Peng; Sheng-Hsien Chiu; Chem.Commun. 50 (2014) 11709–; doi:10.1039/C4cc04695A

data_7115695
_publ_section_title
;
 Hemicarceplex formation allows ready identification of the isomers of the
 metallofullerene Sc3N@C80 using 1H and 13C NMR spectroscopy
;
_journal_name_full               Chem.Commun.
_journal_page_first              11709
_journal_paper_doi               10.1039/C4cc04695A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C194 H156 N O24 Sc3'
_chemical_formula_weight         3020.08
_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                72.2680(10)
_cell_angle_beta                 88.0360(10)
_cell_angle_gamma                63.205(2)
_cell_formula_units_Z            2
_cell_length_a                   17.8883(3)
_cell_length_b                   18.2158(3)
_cell_length_c                   28.6383(3)
_cell_measurement_reflns_used    18830
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.8880
_cell_measurement_theta_min      3.3140
_cell_volume                     7875.6(3)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A'
_diffrn_measurement_method       CCD
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            69852
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3164
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.794
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2080
_refine_ls_number_reflns         34755
_refine_ls_number_restraints     434
_refine_ls_restrained_S_all      0.812
_refine_ls_R_factor_all          0.1749
_refine_ls_R_factor_gt           0.1337
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+62.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3022
_refine_ls_wR_factor_ref         0.3244
_reflns_number_gt                20680
_reflns_number_total             34755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc04695a2.cif
_cod_data_source_block           ic16155_sqd
_cod_original_cell_volume        7875.6(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115695