Chemical Understanding of a Non-IPR Metallofullerene: Stabilization of Encaged Metals on Fused-Pentagon Bonds in La2@C72
Xing Lu; Hidefumi Nikawa; Tsukasa Nakahodo; Takahiro Tsuchiya; Midori O. Ishitsuka; Yutaka Maeda; Takeshi Akasaka; Makoto Toki; Hiroshi Sawa; Zdenek Slanina; Naomi Mizorogi; Shigeru Nagase; Journal of the American Chemical Society 130 (2008) 9129–9136; doi:10.1021/ja8019577

data_4108060
_publ_contact_author_address
;Aspect of Creation of New Materials
Center for Tsukuba Advanced Research Alliance
University of Tsukuba
Tsukuba, Ibaraki 305-8577, Japan
;
_publ_contact_author_email       akasaka@tara.tsukuba.ac.jp
_publ_contact_author_fax         +81-298-53-6409
_publ_contact_author_name        'Takeshi AKASAKA'
_publ_contact_author_phone       +81-298-53-6409
_publ_section_title
;
 Chemical Understanding of a Non-IPR Metallofullerene: Stabilization of
 Encaged Metals on Fused-Pentagon Bonds in La2@C72
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9129
_journal_page_last               9136
_journal_paper_doi               10.1021/ja8019577
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C82 H14 La2, 2(C6 H4 Cl2)'
_chemical_formula_sum            'C94 H22 Cl4 La2'
_chemical_formula_weight         1570.74
_chemical_name_common            La@C72Ad
_chemical_name_systematic        La@C72Ad
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                110.931(5)
_cell_angle_beta                 95.813(4)
_cell_angle_gamma                104.328(5)
_cell_formula_units_Z            2
_cell_length_a                   10.4412(9)
_cell_length_b                   15.5000(16)
_cell_length_c                   17.9190(14)
_cell_measurement_reflns_used    28597
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      140.53
_cell_measurement_theta_min      4.15
_cell_volume                     2566.1(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        Yadokari-XG
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.716
_diffrn_measured_fraction_theta_max 0.716
_diffrn_measurement_device_type  IPDSC
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.99830
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25678
_diffrn_reflns_theta_full        46.00
_diffrn_reflns_theta_max         46.00
_diffrn_reflns_theta_min         2.07
_diffrn_source                   synchrotron
_diffrn_source_type              'KEK-PF BL-1A'
_exptl_absorpt_coefficient_mu    1.918
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.5702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Higashi, T. (1995). Program for Absorption Correction.
 Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.033
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.427
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.0004(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1151
_refine_ls_number_reflns         11510
_refine_ls_number_restraints     1226
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1566P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2131
_reflns_number_gt                8398
_reflns_number_total             11510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8019577-file003.cif
_cod_data_source_block           La2@C72(Ad)-2d
_cod_database_code               4108060