Addition of Adamantylidene to La2@C78: Isolation and Single-Crystal X-ray Structural Determination of the Monoadducts
Baopeng Cao; Hidefumi Nikawa; Tsukasa Nakahodo; Takahiro Tsuchiya; Yutaka Maeda; Takeshi Akasaka; Hiroshi Sawa; Zdenek Slanina; Naomi Mizorogi; Shigeru Nagase; Journal of the American Chemical Society 130 (2008) 983–989; doi:10.1021/ja076462v

data_4107313
_publ_contact_author_address
;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
;
 Addition of Adamantylidene to La2@C78: Isolation and Single-Crystal X-ray
 Structural Determination of the Monoadducts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              983
_journal_page_last               989
_journal_paper_doi               10.1021/ja076462v
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C88 H14 La2 . 0.33(C6H14)'
_chemical_formula_sum            'C90 H18.67 La2'
_chemical_formula_weight         1377.54
_chemical_name_common            La2@C78Ad
_chemical_name_systematic        La2@C78Ad
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      176
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   26.564(2)
_cell_length_b                   26.564(2)
_cell_length_c                   10.8869(9)
_cell_measurement_reflns_used    64844
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      87.07
_cell_measurement_theta_min      2.97
_cell_volume                     6653.1(9)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        Yadokari-XG
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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     0.68870
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            94503
_diffrn_reflns_theta_full        39.50
_diffrn_reflns_theta_max         39.50
_diffrn_reflns_theta_min         1.49
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.970
_exptl_absorpt_correction_T_max  0.8273
_exptl_absorpt_correction_T_min  0.5895
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.063
_exptl_crystal_description       needle
_exptl_crystal_F_000             4036
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.826
_refine_diff_density_min         -2.082
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1491
_refine_ls_number_reflns         14990
_refine_ls_number_restraints     3596
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0711
_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^)+(0.1434P)^2^+0.0100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2349
_reflns_number_gt                8005
_reflns_number_total             14990
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja076462v-file001.cif
_cod_data_source_block           la2c78ad-p63m
_cod_original_cell_volume        6653.3(9)
_cod_database_code               4107313