Does Gd@C82 Have an Anomalous Endohedral Structure? Synthesis and Single Crystal X-ray Structure of the Carbene Adduct
Takeshi Akasaka; Takayoshi Kono; Yuji Takematsu; Hidefumi Nikawa; Tsukasa Nakahodo; Takatsugu Wakahara; Midori O. Ishitsuka; Takahiro Tsuchiya; Yutaka Maeda; Michael T. H. Liu; Kenji Yoza; Tatsuhisa Kato; Kazunori Yamamoto; Naomi Mizorogi; Zdenek Slanina; Shigeru Nagase; Journal of the American Chemical Society 130 (2008) 12840–12841; doi:10.1021/ja802156n

data_4108385
_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
;
 Does Gd@C82 Have an Anomalous Endohedral Structure? Synthesis and Single
 Crystal X-ray Structure of the Carbene Adduct
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12840
_journal_page_last               12841
_journal_paper_doi               10.1021/ja802156n
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'Gd C92 H14, 0.5(C6 H3 Cl3), 1.5(C S2)'
_chemical_formula_sum            'C96.5 H15.5 Cl1.5 Gd S3'
_chemical_formula_weight         1481.19
_chemical_name_common            Gd@C82Ad
_chemical_name_systematic        Gd@C82Ad
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 101.3500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3584(13)
_cell_length_b                   22.030(3)
_cell_length_c                   20.938(2)
_cell_measurement_reflns_used    7323
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.60
_cell_volume                     5136.8(10)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            57008
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.36
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'APEXII ULTRA'
_exptl_absorpt_coefficient_mu    1.560
_exptl_absorpt_correction_T_max  0.8724
_exptl_absorpt_correction_T_min  0.7559
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.915
_exptl_crystal_description       Block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.482
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         11669
_refine_ls_number_restraints     1577
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+56.1672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1644
_reflns_number_gt                9999
_reflns_number_total             11669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802156n_si_002.cif
_cod_data_source_block           gd@c82ad_90k_060823
_cod_original_cell_volume        5136.6(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C96.50 H15.50 Cl1.50 Gd S3'
_cod_database_code               4108385