X-ray Crystallographic Characterization of New Soluble Endohedral Fullerenes Utilizing the Popular C82 Bucky Cage. Isolation and Structural Characterization of Sm@C3v(7)-C82, Sm@Cs(6)-C82, and Sm@C2(5)-C82
Hua Yang; Hongxiao Jin; Xinqing Wang; Ziyang Liu; Meilan Yu; Fukun Zhao; Brandon Q. Mercado; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 134 (2012) 14127–14136; doi:10.1021/ja304867j

data_4118546
_publ_section_title
;
 X-ray Crystallographic Characterization of New Soluble Endohedral
 Fullerenes Utilizing the Popular C82 Bucky Cage. Isolation and Structural
 Characterization of Sm@C3v(7)-C82, Sm@Cs(6)-C82, and Sm@C2(5)-C82
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14127
_journal_page_last               14136
_journal_paper_doi               10.1021/ja304867j
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C82 Sm, C36 H44 N4 Ni, 2(C7 H8)'
_chemical_formula_sum            'C132 H60 N4 Ni Sm'
_chemical_formula_weight         1910.90
_chemical_name_common
'Sm@C82.NiOEP.2toluene 0.6667/0.3333 C3v(7)/Cs(6)'
_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                 97.050(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.3373(11)
_cell_length_b                   14.8267(11)
_cell_length_c                   20.4311(11)
_cell_measurement_reflns_used    7870
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.7
_cell_measurement_theta_min      2.7
_cell_volume                     7617.3(8)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'Apex2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL, XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(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 SMART 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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            61700
_diffrn_reflns_theta_full        30.99
_diffrn_reflns_theta_max         30.99
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2006)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       block
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1102
_refine_ls_number_reflns         12552
_refine_ls_number_restraints     1065
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+31.5695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1688
_reflns_number_gt                10309
_reflns_number_total             12552
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja304867j_si_001.cif
_cod_data_source_block           mn1894
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4118546