Radical Coupling Reaction of Paramagnetic Endohedral Metallofullerene La@C82
Yuta Takano; Akinori Yomogida; Hidefumi Nikawa; Michio Yamada; Takatsugu Wakahara; Takahiro Tsuchiya; Midori O. Ishitsuka; Yutaka Maeda; Takeshi Akasaka; Tatsuhisa Kato; Zdenek Slanina; Naomi Mizorogi; Shigeru Nagase; Journal of the American Chemical Society 130 (2008) 16224–16230; doi:10.1021/ja802748q

data_4108758
_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
;
 Radical Coupling Reaction of Paramagnetic Endohedral Metallofullerene
 La@C82
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16224
_journal_page_last               16230
_journal_paper_doi               10.1021/ja802748q
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C89 H4 Cl3 La, C1 S2'
_chemical_formula_sum            'C90 H4 Cl3 La S2'
_chemical_formula_weight         1394.31
_chemical_name_common            La@C82BzCl3
_chemical_name_systematic        La@C82BzCl3
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.723(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.276(6)
_cell_length_b                   21.827(13)
_cell_length_c                   19.094(11)
_cell_measurement_reflns_used    25282
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      69.69
_cell_measurement_theta_min      2.75
_cell_volume                     4699(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        Yadokari-XG,SHELXTL(Bruker-2001)
_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      130(2)
_diffrn_measured_fraction_theta_full 0.502
_diffrn_measured_fraction_theta_max 0.502
_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     0.68880
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            36674
_diffrn_reflns_theta_full        34.87
_diffrn_reflns_theta_max         34.87
_diffrn_reflns_theta_min         1.81
_diffrn_source                   synchrotron
_diffrn_source_type              'KEK-PF BL-1B'
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  0.9184
_exptl_absorpt_correction_T_min  0.8863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Higashi, T. (1995). Program for Absorption Correction.
 Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            Block
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_description       Black
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.250
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.300
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1735
_refine_ls_number_reflns         11298
_refine_ls_number_restraints     2341
_refine_ls_restrained_S_all      1.362
_refine_ls_R_factor_all          0.1712
_refine_ls_R_factor_gt           0.1235
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3320
_refine_ls_wR_factor_ref         0.3617
_reflns_number_gt                6135
_reflns_number_total             11298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802748q_si_002.cif
_cod_data_source_block           taka01
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4108758