Isolation and Characterization of a Carbene Derivative of La@C82
Yutaka Maeda; Yoichiro Matsunaga; Takatsugu Wakahara; Satomi Takahashi; Takahiro Tsuchiya; Midori O. Ishitsuka; Tadashi Hasegawa; Takeshi Akasaka; Michael T. H. Liu; Kisato Kokura; Ernst Horn; Kenji Yoza; Tatsuhisa Kato; Shingo Okubo; Kaoru Kobayashi; Shigeru Nagase; Kazunori Yamamoto; Journal of the American Chemical Society 126 (2004) 6858–6859; doi:10.1021/ja0316115

data_4112620
_publ_section_title
;
 Isolation and Characterization of a Carbene Derivative of La@C82
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6858
_journal_page_last               6859
_journal_paper_doi               10.1021/ja0316115
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C94.5 H14 La S5'
_chemical_formula_weight         1448.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 100.9350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3249(5)
_cell_length_b                   21.9882(10)
_cell_length_c                   21.0171(10)
_cell_measurement_reflns_used    5919
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.294
_cell_measurement_theta_min      2.240
_cell_volume                     5138.5(4)
_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      293
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58180
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  0.9269
_exptl_absorpt_correction_T_min  0.8884
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.671
_refine_diff_density_min         -3.081
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         10500
_refine_ls_number_restraints     6337
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1530
_refine_ls_R_factor_gt           0.1452
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1367P)^2^+119.4723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3389
_refine_ls_wR_factor_ref         0.3448
_reflns_number_gt                9711
_reflns_number_total             10500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0316115si20040409_080721.cif
_cod_data_source_block           24jc10
_cod_original_formula_sum        'C94.50 H14 La S5'
_cod_database_code               4112620