Location of the metal atoms in Ce2@C78 and its bis-silylated derivative.
Yamada, Michio; Wakahara, Takatsugu; Tsuchiya, Takahiro; Maeda, Yutaka; Kako, Masahiro; Akasaka, Takeshi; Yoza, Kenji; Horn, Ernst; Mizorogi, Naomi; Nagase, Shigeru; Chemical communications (Cambridge, England)  (2008) 558–560; doi:10.1039/b712568b

data_7102854
_publ_section_title
;
 Location of the metal atoms in Ce2@C78 and its bis-silylated
 derivative.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              558
_journal_page_last               560
_journal_paper_doi               10.1039/b712568b
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_formula_sum            'C117.5 H46 Ce2 S5 Si2'
_chemical_formula_weight         1954.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.351(3)
_cell_length_b                   23.560(6)
_cell_length_c                   28.117(7)
_cell_measurement_temperature    270(2)
_cell_volume                     7519(3)
_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      270(2)
_diffrn_measured_fraction_theta_full 0.752
_diffrn_measured_fraction_theta_max 0.752
_diffrn_measurement_device_type  IPDSC
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68880
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34267
_diffrn_reflns_theta_full        24.52
_diffrn_reflns_theta_max         24.52
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  0.9858
_exptl_absorpt_correction_T_min  0.8142
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3900
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.328(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1186
_refine_ls_number_reflns         10346
_refine_ls_number_restraints     977
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0475
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                8500
_reflns_number_total             10346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712568b.txt
_cod_data_source_block           Ce2@C78Si270krev2
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C117.50 H46 Ce2 S5 Si2'
_cod_database_code               7102854