Isolation of Three Isomers of Sm@C84 and X-ray Crystallographic Characterization of Sm@D3d(19)-C84 and Sm@C2(13)-C84
Hua Yang; Meilan Yu; Hongxiao Jin; Ziyang Liu; Mingguang Yao; Bingbing Liu; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 134 (2012) 5331–5338; doi:10.1021/ja211785u

data_4117713
_publ_section_title
;
 Isolation of Three Isomers of Sm@C84 and X-ray Crystallographic
 Characterization of Sm@D3d(19)-C84 and Sm@C2(13)-C84
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5331
_journal_page_last               5338
_journal_paper_doi               10.1021/ja211785u
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C36 H44 N4 Ni, C84, 2(C7 H8)'
_chemical_formula_sum            'C134 H60 N4 Ni Sm'
_chemical_formula_weight         1934.92
_chemical_name_common            Sm@C2(13)-C84.NiOEP.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                 97.439(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.3572(10)
_cell_length_b                   14.9526(6)
_cell_length_c                   20.5748(8)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.6
_cell_volume                     7735.4(5)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL, XP (Sheldrick, 1994)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59369
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       needle
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.420
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1160
_refine_ls_number_reflns         11714
_refine_ls_number_restraints     2877
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+28.3973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1787
_reflns_number_gt                9573
_reflns_number_total             11714
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja211785u_si_001.cif
_cod_data_source_block           mn1904
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4117713