Synthesis and Structural Characterization of Endohedral Pyrrolidinodimetallofullerene: La2@C80(CH2)2NTrt
Michio Yamada; Takatsugu Wakahara; Tsukasa Nakahodo; Takahiro Tsuchiya; Yutaka Maeda; Takeshi Akasaka; Kenji Yoza; Ernst Horn; Naomi Mizorogi; Shigeru Nagase; Journal of the American Chemical Society 128 (2006) 1402–1403; doi:10.1021/ja056560l

data_4110382
_publ_contact_author_address
;Center for Tsukuba Advanced Research Alliance (TARA Center)
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
;
 Synthesis and Structural Characterization of Endohedral
 Pyrrolidinodimetallofullerene: La2@C80(CH2)2NTrt
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1402
_journal_page_last               1403
_journal_paper_doi               10.1021/ja056560l
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C110 H40 La2 N'
_chemical_formula_weight         1653.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                100.1510(10)
_cell_angle_beta                 104.6820(10)
_cell_angle_gamma                103.9560(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0097(11)
_cell_length_b                   16.4849(16)
_cell_length_c                   18.5435(18)
_cell_measurement_reflns_used    7104
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.35
_cell_volume                     3056.9(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      90(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47153
_diffrn_reflns_theta_full        27.84
_diffrn_reflns_theta_max         27.84
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    1.447
_exptl_absorpt_correction_T_max  0.9182
_exptl_absorpt_correction_T_min  0.6708
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       plate
_exptl_crystal_F_000             1642
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.705
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1415
_refine_ls_number_reflns         13868
_refine_ls_number_restraints     2342
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0768
_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^)+(0.1072P)^2^+14.9217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2046
_refine_ls_wR_factor_ref         0.2216
_reflns_number_gt                10943
_reflns_number_total             13868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056560lsi20051229_040304.cif
_cod_data_source_block           p1bar9
_cod_database_code               4110382