Missing Metallofullerene with C80 Cage
Hidefumi Nikawa; Tomoya Yamada; Baopeng Cao; Naomi Mizorogi; Zdenek Slanina; Takahiro Tsuchiya; Takeshi Akasaka; Kenji Yoza; Shigeru Nagase; Journal of the American Chemical Society 131 (2009) 10950–10954; doi:10.1021/ja900972r

data_4104804
_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
;
 Missing Metallofullerene with C80 Cage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10950
_journal_page_last               10954
_journal_paper_doi               10.1021/ja900972r
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'La C86 H3, 1.5(C7H8)'
_chemical_formula_sum            'C96.5 H15 Cl2 La'
_chemical_formula_weight         1383.90
_chemical_name_common            La@C80C6H3Cl2
_chemical_name_systematic        La@C80C6H3Cl2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 105.548(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5336(16)
_cell_length_b                   22.057(3)
_cell_length_c                   20.237(3)
_cell_measurement_reflns_used    8032
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.72
_cell_measurement_theta_min      2.38
_cell_volume                     4959.8(12)
_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
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54901
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.39
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Bruker AXS APECII URTRA'
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.9309
_exptl_absorpt_correction_T_min  0.8351
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       Block
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1196
_refine_ls_number_reflns         11248
_refine_ls_number_restraints     1473
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0983
_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^)+(0.0656P)^2^+38.2288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2288
_refine_ls_wR_factor_ref         0.2390
_reflns_number_gt                9123
_reflns_number_total             11248
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja900972r_si_002.cif
_cod_data_source_block           la@c80c6h3cl2_p21c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C96.50 H15 Cl2 La'
_cod_database_code               4104804