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_4118175
_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         'C94 Sm,C36 H44 Ni N4,2(C7 H8)'
_chemical_formula_sum            'C144 H60 N4 Ni Sm'
_chemical_formula_weight         2055.02
_chemical_name_common            Sm@C3v(134)-C94.Ni(OEP).2toluene
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 97.368(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.6869(8)
_cell_length_b                   15.1248(5)
_cell_length_c                   21.3153(6)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.3
_cell_measurement_theta_min      2.7
_cell_volume                     8212.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker ApexII CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'Advanced Light Source, BL 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            129486
_diffrn_reflns_theta_full        37.32
_diffrn_reflns_theta_max         37.32
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    1.263
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2006)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4168
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.996
_refine_diff_density_min         -1.625
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1377
_refine_ls_number_reflns         16962
_refine_ls_number_restraints     2683
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+12.6624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1523
_reflns_number_gt                15111
_reflns_number_total             16962
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja302859r_si_002.cif
_cod_data_source_block           cb171
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4118175