Single Samarium Atoms in Large Fullerene Cages. Characterization of Two Isomers of Sm@C92 and Four Isomers of Sm@C94 with the X-ray Crystallographic Identification of Sm@C1(42)-C92, Sm@Cs(24)-C92, and Sm@C3v(134)-C94
Hongxiao Jin; Hua Yang; Meilan Yu; Ziyang Liu; Christine M. Beavers; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 134 (2012) 10933–10941; doi:10.1021/ja302859r

data_4118176
_publ_section_title
;
 Single Samarium Atoms in Large Fullerene Cages. Characterization of Two
 Isomers of Sm@C92 and Four Isomers of Sm@C94 with the X-ray
 Crystallographic Identification of Sm@C1(42)-C92, Sm@Cs(24)-C92, and
 Sm@C3v(134)-C94
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10933
_journal_page_last               10941
_journal_paper_doi               10.1021/ja302859r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety
'C92 Sm, C36 H44 N4 Ni, 1.6(C7 H8), 0.4(C6 H6)'
_chemical_formula_sum            'C141.6 H59.2 N4 Ni Sm'
_chemical_formula_weight         2025.39
_chemical_name_common            Sm@Cs(24)-C92.Ni(OEP).1.6toluene.0.4benzene
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 117.664(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   47.306(4)
_cell_length_b                   15.0840(12)
_cell_length_c                   25.625(2)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.5
_cell_volume                     16195(2)
_computing_cell_refinement       'Apex2 (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'Apex2 (Bruker, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART Apex II'
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       69
_diffrn_reflns_limit_h_min       -69
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            133290
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       prism
_exptl_crystal_F_000             8214
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.35
_refine_diff_density_max         5.050
_refine_diff_density_min         -1.856
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.493
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1622
_refine_ls_number_reflns         26909
_refine_ls_number_restraints     6003
_refine_ls_restrained_S_all      2.335
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.1203
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3335
_refine_ls_wR_factor_ref         0.3520
_reflns_number_gt                18786
_reflns_number_total             26909
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja302859r_si_003.cif
_cod_data_source_block           mn2035
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C141.60 H59.20 N4 Ni Sm'
_cod_database_code               4118176