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_4117457
_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            'C97.3 H16.8 Cl1.4 S2.2 Sc2'
_chemical_formula_weight         1395.59
_chemical_name_common            Sc2C2@C80Ad-G
_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                 100.2230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9836(2)
_cell_length_b                   21.6821(4)
_cell_length_c                   21.2588(4)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.50
_cell_measurement_theta_min      2.46
_cell_volume                     4982.36(16)
_computing_cell_refinement       'APEX2 '
_computing_data_collection       'APEX2 '
_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, 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 APEX-II CCD'
_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  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0352
_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            74402
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  0.9749
_exptl_absorpt_correction_T_min  0.8535
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       block
_exptl_crystal_F_000             2806
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    consr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1795
_refine_ls_number_reflns         11441
_refine_ls_number_restraints     3342
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0645P)^2^+10.5607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                9019
_reflns_number_total             11441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210101f_si_005.cif
_cod_data_source_block           g_01a
_cod_original_formula_sum        'C97.30 H16.80 Cl1.40 S2.20 Sc2'
_cod_database_code               4117457