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_4118547
_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(C6 H6)'
_chemical_formula_sum            'C130 H56 N4 Ni Sm'
_chemical_formula_weight         1882.85
_chemical_name_common            Sm@C2(5)-C82.Ni(OEP).2benzene
_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
_audit_update_record
;
2010-11-12 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.208(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.3364(4)
_cell_length_b                   15.0718(2)
_cell_length_c                   19.7948(3)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      33.6
_cell_measurement_theta_min      2.7
_cell_volume                     7538.6(2)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_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 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART ApexII'
_diffrn_measurement_method       '\w and \f'
_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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            98570
_diffrn_reflns_theta_full        32.58
_diffrn_reflns_theta_max         32.58
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             3816
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.382
_refine_diff_density_min         -1.676
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         14174
_refine_ls_number_restraints     2752
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1136P)^2^+20.9782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2036
_reflns_number_gt                11674
_reflns_number_total             14174
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja304867j_si_002.cif
_cod_data_source_block           mn2044
_cod_original_cell_volume        7538.57(19)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4118547