Chemical Understanding of Carbide Cluster Metallofullerenes: A Case Study on Sc2C2@C2v(5)-C80 with Complete X-ray Crystallographic Characterizations
Hiroki Kurihara; Xing Lu; Yuko Iiduka; Hidefumi Nikawa; Naomi Mizorogi; Zdenek Slanina; Takahiro Tsuchiya; Shigeru Nagase; Takeshi Akasaka; Journal of the American Chemical Society 134 (2012) 3139–3144; doi:10.1021/ja210101f

data_4117456
_publ_section_title
;
 Chemical Understanding of Carbide Cluster Metallofullerenes: A Case Study
 on Sc2C2@C2v(5)-C80 with Complete X-ray Crystallographic
 Characterizations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3139
_journal_page_last               3144
_journal_paper_doi               10.1021/ja210101f
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C98.5 H18 Cl2 S Sc2'
_chemical_formula_weight         1394.01
_chemical_name_common            Sc2C2@C80Ad-C
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 99.8220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.11660(10)
_cell_length_b                   21.7692(3)
_cell_length_c                   21.0084(3)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.25
_cell_volume                     5009.50(11)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78868
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  0.9344
_exptl_absorpt_correction_T_min  0.8707
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       block
_exptl_crystal_F_000             2804
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    consr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1883
_refine_ls_number_reflns         11953
_refine_ls_number_restraints     3766
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1014P)^2^+7.0465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1903
_reflns_number_gt                9708
_reflns_number_total             11953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210101f_si_004.cif
_cod_data_source_block           adc_aa
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C98.50 H18 Cl2 S Sc2'
_cod_database_code               4117456