Regioselective Bis-functionalization of Endohedral Dimetallofullerene, La2@C80: Extremal La-La Distance
Midori O. Ishitsuka; Shogo Sano; Haruka Enoki; Satoru Sato; Hidefumi Nikawa; Takahiro Tsuchiya; Zdenek Slanina; Naomi Mizorogi; Michael T. H. Liu; Takeshi Akasaka; Shigeru Nagase; Journal of the American Chemical Society 133 (2011) 7128–7134; doi:10.1021/ja200903q

data_4106119
_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@dmb.chem.tsukuba.ac.jp
_publ_contact_author_fax         +81-29-853-6409
_publ_contact_author_name        'Takeshi AKASAKA'
_publ_contact_author_phone       +81-29-853-6409
_publ_section_title
;
 Regioselective Bis-functionalization of Endohedral Dimetallofullerene,
 La2@C80: Extremal La-La Distance
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7128
_journal_page_last               7134
_journal_paper_doi               10.1021/ja200903q
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C93 H9 Cl3 La2'
_chemical_formula_sum            'C93 H9 Cl3 La2'
_chemical_formula_weight         1510.17
_chemical_name_common            La2@C80(CClPh)
_chemical_name_systematic        La2@C80(CClPh)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.468(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9639(5)
_cell_length_b                   20.6081(10)
_cell_length_c                   21.6433(13)
_cell_measurement_reflns_used    52580
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      140.70
_cell_measurement_theta_min      3.87
_cell_volume                     4792.6(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        Yadokari-XG,SHELXTL
_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 0.720
_diffrn_measured_fraction_theta_max 0.720
_diffrn_measurement_device_type  'RAPID AXIS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.99830
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59295
_diffrn_reflns_theta_full        70.35
_diffrn_reflns_theta_max         70.35
_diffrn_reflns_theta_min         1.94
_diffrn_source                   synchrotron
_diffrn_source_type              'KEK beamline BL1A'
_exptl_absorpt_coefficient_mu    4.956
_exptl_absorpt_correction_T_max  0.8264
_exptl_absorpt_correction_T_min  0.5877
_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    2.093
_exptl_crystal_description       Block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         8.711
_refine_diff_density_min         -5.518
_refine_diff_density_rms         0.315
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1749
_refine_ls_number_reflns         24285
_refine_ls_number_restraints     32243
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.1626
_refine_ls_R_factor_gt           0.1299
_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^)+(0.1944P)^2^+61.6185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3638
_refine_ls_wR_factor_ref         0.3825
_reflns_number_gt                15268
_reflns_number_total             24285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200903q_si_002.cif
_cod_data_source_block           La2@C80(CClPh)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4106119