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_4106986
_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         'C88 Sm2, C36 H44 N4 Ni, 2.0(C7 H8)'
_chemical_formula_sum            'C138 H60 N4 Ni Sm2'
_chemical_formula_weight         2133.31
_chemical_name_common            'Sm2@C88.Ni(OEP).2toluene D2(No. 35)'
_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                 94.469(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.108(5)
_cell_length_b                   15.372(3)
_cell_length_c                   20.633(4)
_cell_measurement_reflns_used    9404
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.3
_cell_measurement_theta_min      2.4
_cell_volume                     7939(3)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type
'Rigaku Crystal-Logic Kappa diffractometer equipped with a Saturn 724+ detector'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Beamline I19, Diamond Light Source'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            60249
_diffrn_reflns_theta_full        29.48
_diffrn_reflns_theta_max         29.48
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.767
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       black
_exptl_crystal_F_000             4272
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.632
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1332
_refine_ls_number_reflns         12105
_refine_ls_number_restraints     4072
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+27.5945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1709
_reflns_number_gt                10949
_reflns_number_total             12105
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja206244w_si_001.cif
_cod_data_source_block           mn1930
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4106986