Entrapping a Group-VB Transition Metal, Vanadium, within an Endohedral Metallofullerene: VxSc3-xN@Ih-C80 (x = 1, 2).
Wei, Tao; Wang, Song; Lu, Xing; Tan, Yuanzhi; Huang, Jing; Liu, Fupin; Li, Qunxiang; Xie, Suyuan; Yang, Shangfeng; Journal of the American Chemical Society 138 (2016) 207–214; doi:10.1021/jacs.5b10115

data_4124771
_publ_section_title
;
 Entrapping a Group-VB Transition Metal, Vanadium, within an Endohedral
 Metallofullerene: VxSc3-xN@Ih-C80 (x = 1, 2).
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              207
_journal_page_last               214
_journal_paper_doi               10.1021/jacs.5b10115
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C128.5 H56 N5 Ni Sc V2'
_chemical_formula_weight         1875.33
_chemical_name_common            ScV2N@Ih(7)-C80/Ni(OEP)/2benzene;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.822(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.2821(15)
_cell_length_b                   15.1254(10)
_cell_length_c                   19.7824(16)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.490
_cell_measurement_theta_min      3.971
_cell_volume                     7538.1(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.01(2)
_diffrn_detector_area_resol_mean 10.3415
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_laue_measured_fraction_full 0.972
_diffrn_reflns_laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11946
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        62.488
_diffrn_reflns_theta_max         62.488
_diffrn_reflns_theta_min         3.408
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.593
_exptl_absorpt_correction_T_max  0.6933
_exptl_absorpt_correction_T_min  0.4551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3828
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.258
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.339
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1010
_refine_ls_number_reflns         6101
_refine_ls_number_restraints     1598
_refine_ls_restrained_S_all      1.390
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.1234
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1550P)^2^+48.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3252
_refine_ls_wR_factor_ref         0.3402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5084
_reflns_number_total             6101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10115_si_003.cif
_cod_data_source_block           scv2n@c80
_cod_depositor_comments
'Adding full bibliography for 4124770--4124771.cif.'
_cod_original_formula_sum        'C128.50 H56 N5 Ni Sc V2'
_cod_database_code               4124771
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.455
_shelx_estimated_absorpt_t_max   0.693
_shelx_res_checksum              53615
_shelx_hkl_checksum              17999