Single-Crystal X-ray Diffraction Study of Three Yb@C82 Isomers Cocrystallized with NiII(octaethylporphyrin)
Mitsuaki Suzuki; Zdenek Slanina; Naomi Mizorogi; Xing Lu; Shigeru Nagase; Marilyn M. Olmstead; Alan L. Balch; Takeshi Akasaka; Journal of the American Chemical Society 134 (2012) 18772–18778; doi:10.1021/ja308706d

data_4118888
_publ_section_title
;
 Single-Crystal X-ray Diffraction Study of Three Yb@C82 Isomers
 Cocrystallized with NiII(octaethylporphyrin)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18772
_journal_page_last               18778
_journal_paper_doi               10.1021/ja308706d
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'Yb C82, Ni N4 C36 H44, 2.0(C6 H6)'
_chemical_formula_sum            'C130 H56 N4 Ni Yb'
_chemical_formula_weight         1905.54
_chemical_name_common            Yb@Cs(6)-C82/NiOEP/2.0benzene
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.130(2)
_cell_angle_beta                 86.023(2)
_cell_angle_gamma                61.312(2)
_cell_formula_units_Z            2
_cell_length_a                   14.613(2)
_cell_length_b                   14.816(2)
_cell_length_c                   19.934(3)
_cell_measurement_reflns_used    9058
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.86
_cell_measurement_theta_min      4.33
_cell_volume                     3774.0(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46939
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         4.31
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.6977
_exptl_absorpt_correction_T_min  0.5551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       block
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.329
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1886
_refine_ls_number_reflns         19878
_refine_ls_number_restraints     2052
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0789P)^2^+8.2692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1762
_reflns_number_gt                16508
_reflns_number_total             19878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja308706d_si_002.cif
_cod_data_source_block           yb82i
_cod_original_cell_volume        3774.2(11)
_cod_database_code               4118888