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_4117455
_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-B
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.207(12)
_cell_angle_beta                 74.636(11)
_cell_angle_gamma                74.459(11)
_cell_formula_units_Z            2
_cell_length_a                   11.130(2)
_cell_length_b                   14.730(4)
_cell_length_c                   16.508(4)
_cell_measurement_reflns_used    13418
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      122.69
_cell_measurement_theta_min      5.30
_cell_volume                     2512.0(10)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        Yadokari-XG,SHELXTL
_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(2)
_diffrn_measured_fraction_theta_full 0.405
_diffrn_measured_fraction_theta_max 0.405
_diffrn_measurement_device_type  'RAPID AXIS'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'KEK-PF BL-1B'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.00000
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30808
_diffrn_reflns_theta_full        61.31
_diffrn_reflns_theta_max         61.31
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    4.245
_exptl_absorpt_correction_T_max  0.7276
_exptl_absorpt_correction_T_min  0.2402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Higashi, T. (1995). Program for Absorption Correction.
 Rigaku Corporation, Tokyo, Japan.  
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_description       block
_exptl_crystal_F_000             1402
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.436
_refine_ls_hydrogen_treatment    consr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1883
_refine_ls_number_reflns         11509
_refine_ls_number_restraints     4425
_refine_ls_restrained_S_all      1.357
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.1185
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3540
_refine_ls_wR_factor_ref         0.3791
_reflns_number_gt                6581
_reflns_number_total             11509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210101f_si_003.cif
_cod_data_source_block           ad_b
_cod_original_cell_volume        2511.9(10)
_cod_original_formula_sum        'C98.50 H18 Cl2 S Sc2'
_cod_database_code               4117455