Caught in Phase Transition: Snapshot of the Metallofullerene Sc3N@C70 Rotation in the Crystal
Hao, Yajuan; Wang, Yaofeng; Dubrovin, Vasilii; Avdoshenko, Stanislav M.; Popov, Alexey A.; Liu, Fupin; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c10758

data_4135484
_publ_section_title
;
 Caught in Phase Transition: Snapshot of the Metallofullerene Sc3N@C70
 Rotation in the Crystal
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c10758
_journal_year                    2020
_chemical_formula_moiety         ;Sc3N@C70/NiOEP/C6H6/C7H8;
_chemical_formula_sum            'C116 H55 N5 Ni Sc3'
_chemical_formula_weight         1712.24
_chemical_name_common            ;Sc3N@C2v(7854)-C70/NiOEP/C6H6/C7H8;
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 106.05(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.650(5)
_cell_length_b                   16.480(3)
_cell_length_c                   17.350(4)
_cell_measurement_reflns_used    63692
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      36.635
_cell_measurement_theta_min      1.673
_cell_volume                     7048(3)
_computing_cell_refinement       XDS
_computing_data_collection       XDS
_computing_data_reduction        XDS
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  PILATUS
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7999
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            63692
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        28.681
_diffrn_reflns_theta_max         36.635
_diffrn_reflns_theta_min         1.673
_diffrn_source                   'BESSY BL MX-14.2'
_exptl_absorpt_coefficient_mu    0.839
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             3508
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.049
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0024(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         11341
_refine_ls_number_restraints     1338
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0925
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1965P)^2^+6.7006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2737
_refine_ls_wR_factor_ref         0.3143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7928
_reflns_number_total             11341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c10758_si_003.cif
_cod_data_source_block           sc3n@c70-160k
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4135484
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              63605
_shelx_hkl_checksum              43451