Regioselective Cycloaddition of La2@Ih-C80 with Tetracyanoethylene Oxide: Formation of an Endohedral Dimetallofullerene Adduct Featuring Enhanced Electron-Accepting Character
Michio Yamada; Mari Minowa; Satoru Sato; Zdenek Slanina; Takahiro Tsuchiya; Yutaka Maeda; Shigeru Nagase; Takeshi Akasaka; Journal of the American Chemical Society 133 (2011) 3796–3799; doi:10.1021/ja2000243

data_4105795
_publ_contact_author_address
'University of Tsukuba, 1-1-1 Tennnodai, Tsukuba, Ibaraki 305-8577, Japan'
_publ_contact_author_email       akasaka@tara.tsukuba.ac.jp
_publ_contact_author_fax         +81298536409
_publ_contact_author_name        'Takeshi Akasaka'
_publ_contact_author_phone       +81298536409
_publ_section_title
;
 Regioselective Cycloaddition of La2@Ih-C80 with Tetracyanoethylene Oxide:
 Formation of an Endohedral Dimetallofullerene Adduct Featuring Enhanced
 Electron-Accepting Character
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3796
_journal_page_last               3799
_journal_paper_doi               10.1021/ja2000243
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C86 La2 N4 O, C4 H4 Cl8'
_chemical_formula_sum            'C90 H4 Cl8 La2 N4 O'
_chemical_formula_weight         1718.39
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.394(3)
_cell_length_b                   17.580(2)
_cell_length_c                   13.7909(18)
_cell_measurement_reflns_used    6222
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.32
_cell_volume                     5186.8(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)
;
_computing_publication_material
;
Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)' 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20707
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.76
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.111
_exptl_absorpt_correction_T_max  0.9018
_exptl_absorpt_correction_T_min  0.8493
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_description       Block
_exptl_crystal_F_000             3320
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.235
_refine_diff_density_min         -2.656
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         4745
_refine_ls_number_restraints     443
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.1182
_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^)+(0.0000P)^2^+175.7970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2318
_refine_ls_wR_factor_ref         0.2409
_reflns_number_gt                3934
_reflns_number_total             4745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2000243_si_002.cif
_cod_data_source_block           01a
_cod_depositor_comments
;
  Moved the _audit_creation_method data item out of the loop.

  Antanas Vaitkus,
  2019-03-01
;
_cod_original_cell_volume        5186.7(11)
_cod_database_code               4105795