Very Large, Soluble Endohedral Fullerenes in the Series La2C90 to La2C138: Isolation and Crystallographic Characterization of La2@D5(450)-C100
Christine M. Beavers; Hongxiao Jin; Hua Yang; Zhimin Wang; Xinqing Wang; Hongliang Ge; Ziyang Liu; Brandon Q. Mercado; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 133 (2011) 15338–15341; doi:10.1021/ja207090e

data_4106889
_publ_section_title
;
 Very Large, Soluble Endohedral Fullerenes in the Series La2C90 to
 La2C138: Isolation and Crystallographic Characterization of
 La2@D5(450)-C100
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15338
_journal_page_last               15341
_journal_paper_doi               10.1021/ja207090e
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         '(C100 La2),(C36 H44 N4 Ni)2,(C7 H8)2'
_chemical_formula_sum            'C186 H104 La2 N8 Ni2'
_chemical_formula_weight         2846.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.6803(7)
_cell_length_b                   19.0086(6)
_cell_length_c                   24.8761(8)
_cell_measurement_reflns_used    9574
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.74
_cell_measurement_theta_min      2.79
_cell_volume                     11670.3(6)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2010)'
_computing_data_collection       'Apex2 v2010.7-0 (Bruker, 2010)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART ApexII'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon(111)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            292557
_diffrn_reflns_theta_full        50.86
_diffrn_reflns_theta_max         50.86
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.380
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5784
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.639
_refine_diff_density_min         -4.103
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2267
_refine_ls_number_reflns         47472
_refine_ls_number_restraints     6768
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1206P)^2^+7.0705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2027
_refine_ls_wR_factor_ref         0.2411
_reflns_number_gt                29071
_reflns_number_total             47472
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja207090e_si_001.cif
_cod_data_source_block           cb184
_cod_database_code               4106889