Characterization of the Bis-Silylated Endofullerene Sc3N@C80
Takatsugu Wakahara; Yuko Iiduka; Ozora Ikenaga; Tsukasa Nakahodo; Akihiro Sakuraba; Takahiro Tsuchiya; Yutaka Maeda; Masahiro Kako; Takeshi Akasaka; Kenji Yoza; Ernst Horn; Naomi Mizorogi; Shigeru Nagase; Journal of the American Chemical Society 128 (2006) 9919–9925; doi:10.1021/ja062233h

data_4110757
_publ_section_title
;
 Characterization of the Bis-Silylated Endofullerene Sc3N@C80
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9919
_journal_page_last               9925
_journal_paper_doi               10.1021/ja062233h
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C117 H46 N Sc3 Si2'
_chemical_formula_weight         1656.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           80
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_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                   20.4678(14)
_cell_length_b                   20.4678(14)
_cell_length_c                   15.804(2)
_cell_measurement_reflns_used    6771
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      2.22
_cell_volume                     6620.8(11)
_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 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38848
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.9607
_exptl_absorpt_correction_T_min  0.9607
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       plate
_exptl_crystal_F_000             3384
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         7902
_refine_ls_number_restraints     1510
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1501
_refine_ls_R_factor_gt           0.1474
_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^)+(0.1429P)^2^+180.6240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3787
_refine_ls_wR_factor_ref         0.3804
_reflns_number_gt                7576
_reflns_number_total             7902
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja062233hsi20060402_010536.cif
_cod_data_source_block           i41
_cod_original_cell_volume        6620.8(12)
_cod_database_code               4110757