X-ray Structures of Sc2C2@C2n (n= 40-42): In-Depth Understanding of the Core-Shell Interplay in Carbide Cluster Metallofullerenes
Hiroki Kurihara; Xing Lu; Yuko Iiduka; Hidefumi Nikawa; Makoto Hachiya; Naomi Mizorogi; Zdenek Slanina; Takahiro Tsuchiya; Shigeru Nagase; Takeshi Akasaka; Inorganic Chemistry 51 (2012) 746–750; doi:10.1021/ic202438u

data_4327933
_publ_section_title
;
 X-ray Structures of Sc2C2@C2n (n= 40-42): In-Depth Understanding of the
 Core-Shell Interplay in Carbide Cluster Metallofullerenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              746
_journal_page_last               750
_journal_paper_doi               10.1021/ic202438u
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C122 H46 Cl6 Co N4 Sc2'
_chemical_formula_weight         1929.17
_chemical_name_common            Sc2C2@C82(C3v)/Co(OEP)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 93.1030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.0092(4)
_cell_length_b                   15.4199(3)
_cell_length_c                   19.3935(3)
_cell_measurement_temperature    90(2)
_cell_volume                     7467.9(2)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'Yadokari-XG, SHELXS-97'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'Yadokari-XG, SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Yadokari-XG, SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            80841
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.8989
_exptl_absorpt_correction_T_min  0.8376
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       block
_exptl_crystal_F_000             3908
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2111
_refine_ls_number_reflns         19948
_refine_ls_number_restraints     4026
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.182
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+20.6123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1792
_reflns_number_gt                15581
_reflns_number_total             19948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202438u_si_003.cif
_cod_data_source_block           c3v02b
_cod_database_code               4327933