Large Endohedral Fullerenes Containing Two Metal Ions, Sm2@D2(35)-C88, Sm2@C1(21)-C90, and Sm2@D3(85)-C92, and Their Relationship to Endohedral Fullerenes Containing Two Gadolinium Ions
Hua Yang; Hongxiao Jin; Bo Hong; Ziyang Liu; Christine M. Beavers; Hongyu Zhen; Zhimin Wang; Brandon Q. Mercado; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 133 (2011) 16911–16919; doi:10.1021/ja206244w

data_4106988
_publ_section_title
;
 Large Endohedral Fullerenes Containing Two Metal Ions, Sm2@D2(35)-C88,
 Sm2@C1(21)-C90, and Sm2@D3(85)-C92, and Their Relationship to Endohedral
 Fullerenes Containing Two Gadolinium Ions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16911
_journal_page_last               16919
_journal_paper_doi               10.1021/ja206244w
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C92 Sm2, C36 H44 N4 Ni, 2(C6 H5 Cl)'
_chemical_formula_sum            'C140 H54 Cl2 N4 Ni Sm2'
_chemical_formula_weight         2222.18
_chemical_name_common            'Sm2@C92.NiOEP.2chlorobenzene D3(No. 85)'
_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                 97.638(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.5870(9)
_cell_length_b                   14.9402(6)
_cell_length_c                   21.3995(7)
_cell_measurement_reflns_used    9756
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.6
_cell_measurement_theta_min      8.9
_cell_volume                     8107.9(5)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'Apex2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 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      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART Apex II'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Beamline 11.3.1, ALS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       40
_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            77139
_diffrn_reflns_theta_full        37.95
_diffrn_reflns_theta_max         37.95
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    1.798
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       plate
_exptl_crystal_F_000             4432
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.700
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1202
_refine_ls_number_reflns         17327
_refine_ls_number_restraints     900
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+13.2547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1412
_reflns_number_gt                13411
_reflns_number_total             17327
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja206244w_si_003.cif
_cod_data_source_block           mn1801
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4106988