Molecular Spinning Top: Visualizing the Dynamics of M3N@C80 with Variable Temperature Single Crystal X-ray Diffraction
Liu, Fupin; Spree, Lukas; Chemical Communications  (2019) –; doi:10.1039/C9CC06363C

data_7124276
_publ_section_title
;
 Molecular Spinning Top: Visualizing the Dynamics of M3N@C80 with Variable
 Temperature Single Crystal X-ray Diffraction
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06363C
_journal_year                    2019
_chemical_formula_moiety         ;Lu3N@C80/NiOEP/2C6H6;
_chemical_formula_sum            'C128 H56 Lu3 N5 Ni'
_chemical_formula_weight         2247.39
_chemical_name_common            ;Lu3N@Ih(7)-C80/NiOEP/2C6H6;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-08-14 deposited with the CCDC.    2019-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                81.04(3)
_cell_angle_beta                 74.47(3)
_cell_angle_gamma                86.42(3)
_cell_formula_units_Z            2
_cell_length_a                   14.700(3)
_cell_length_b                   15.380(3)
_cell_length_c                   17.730(4)
_cell_measurement_reflns_used    33548
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.575
_cell_measurement_theta_min      1.058
_cell_volume                     3814.1(15)
_computing_cell_refinement       XDS
_computing_data_collection       XDS
_computing_data_reduction        XDS
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  MAR225CCD
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.89429
_diffrn_reflns_av_R_equivalents  0.1360
_diffrn_reflns_av_unetI/netI     0.0988
_diffrn_reflns_Laue_measured_fraction_full 0.896
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33548
_diffrn_reflns_point_group_measured_fraction_full 0.896
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        29.475
_diffrn_reflns_theta_max         29.475
_diffrn_reflns_theta_min         2.099
_diffrn_source                   'BESSY BL MX-14.3'
_exptl_absorpt_coefficient_mu    7.923
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.642
_refine_diff_density_min         -1.750
_refine_diff_density_rms         0.237
_refine_ls_extinction_coef       0.00021(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1263
_refine_ls_number_reflns         9532
_refine_ls_number_restraints     1020
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0673
_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^)+(0.1397P)^2^+5.0788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7538
_reflns_number_total             9532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06363c2.cif
_cod_data_source_block           lu3n@c80-100k
_cod_database_code               7124276
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              99589