Structures of Gd<sub>3</sub>N@C<sub>80</sub> Prato Bis-Adducts: Crystal Structure, Thermal Isomerization, and Computational Study.
Semivrazhskaya, Olesya; Romero-Rivera, Adrian; Aroua, Safwan; Troyanov, Sergey I.; Garcia-Borràs, Marc; Stevenson, Steven; Osuna, Sílvia; Yamakoshi, Yoko; Journal of the American Chemical Society 141 (2019) 10988–10993; doi:10.1021/jacs.9b05603

data_4127404
_publ_section_title
;
 Structures of Gd<sub>3</sub>N@C<sub>80</sub> Prato Bis-Adducts: Crystal
 Structure, Thermal Isomerization, and Computational Study.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10988
_journal_page_last               10993
_journal_paper_doi               10.1021/jacs.9b05603
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C88 H18 Gd3 N3'
_chemical_formula_weight         1588.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4190(10)
_cell_length_b                   15.5160(10)
_cell_length_c                   20.404(2)
_cell_measurement_reflns_used    10000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32
_cell_measurement_theta_min      4
_cell_volume                     4575.9(7)
_computing_cell_refinement       XDS
_computing_data_collection       XDS
_computing_data_reduction        XDS
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  MAR225
_diffrn_measurement_method       CCD
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.895
_diffrn_reflns_av_R_equivalents  0.1556
_diffrn_reflns_av_unetI/netI     0.1033
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27479
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        32.450
_diffrn_reflns_theta_max         36.070
_diffrn_reflns_theta_min         3.307
_diffrn_source                   'BL 14.3 PSF, BESSY, Berlin, Germany'
_exptl_absorpt_coefficient_mu    7.926
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             3036
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.005
_refine_diff_density_max         6.269
_refine_diff_density_min         -6.196
_refine_diff_density_rms         0.590
_refine_ls_extinction_coef       0.0023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         5107
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1958
_refine_ls_R_factor_gt           0.1632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+2300.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3732
_refine_ls_wR_factor_ref         0.3901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3808
_reflns_number_total             5107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05603_si_002.cif
_cod_data_source_block           gdetbismod
_cod_database_code               4127404
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.908
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              45449
_shelx_hkl_checksum              65212