Anisotropic Magnetic Behavior of Anionic Ce@C82 Carbene Adducts
Yuta Takano; Motoki Aoyagi; Michio Yamada; Hidefumi Nikawa; Zdenek Slanina; Naomi Mizorogi; Midori O. Ishitsuka; Takahiro Tsuchiya; Yutaka Maeda; Takeshi Akasaka; Tatsuhisa Kato; Shigeru Nagase; Journal of the American Chemical Society 131 (2009) 9340–9346; doi:10.1021/ja902106a

data_4104650
_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         +81-29-853-6409
_publ_contact_author_name        'Takeshi AKASAKA'
_publ_contact_author_phone       +81-29-853-6409
_publ_section_title
;
 Anisotropic Magnetic Behavior of Anionic Ce@C82 Carbene Adducts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9340
_journal_page_last               9346
_journal_paper_doi               10.1021/ja902106a
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C92 H14 Ce 1-, C16 H36 N 1+, C S2'
_chemical_formula_sum            'C109 H50 Ce N S2'
_chemical_formula_weight         1577.74
_chemical_name_common            Ce@C82(Ad)-II
_chemical_name_systematic        Ce@C82(Ad)-II
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                75.603(7)
_cell_angle_beta                 65.440(8)
_cell_angle_gamma                78.677(9)
_cell_formula_units_Z            2
_cell_length_a                   14.709(4)
_cell_length_b                   15.587(3)
_cell_length_c                   15.703(3)
_cell_measurement_reflns_used    36968
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      64.07
_cell_measurement_theta_min      6.13
_cell_volume                     3153.9(12)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        Yadokari-XG,SHELXTL
_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      120(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22612
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Rigaku R-AXIS RAPID'
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.9271
_exptl_absorpt_correction_T_min  0.8278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Higashi, T. (1995). Program for Absorption Correction.
 Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       Block
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         10805
_refine_ls_number_restraints     247
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0808P)^2^+17.6228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1539
_reflns_number_gt                9304
_reflns_number_total             10805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902106a_si_002.cif
_cod_data_source_block           071028ceadb
_cod_original_cell_volume        3154.0(13)
_cod_database_code               4104650