C~60~ in a peptidic cage: a case of symmetry mismatch studied by crystallography and solid-state NMR
Gilski, Miroslaw; Bernatowicz, Piotr; Sakowicz, Arkadiusz; Szymański, Marek P.; Zalewska, Aldona; Szumna, Agnieszka; Jaskólski, Mariusz; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620009944

data_2108657
_publ_section_title
;
 C~60~ in a peptidic cage: a case of symmetry mismatch studied by
 crystallography and solid-state NMR
;
_journal_coeditor_code           LO5072
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620009944
_journal_volume                  76
_journal_year                    2020
_chemical_formula_sum            'C260 H264 N24 O40'
_chemical_formula_weight         4365.00
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.91(2)
_cell_length_b                   21.91(2)
_cell_length_c                   25.44(3)
_cell_measurement_reflns_used    5405
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.553
_cell_measurement_theta_min      1.427
_cell_volume                     12212(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 13.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  MD3_Microdiffractometer
_diffrn_measurement_method       rotation
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8266
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31450
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        29.553
_diffrn_reflns_theta_max         29.553
_diffrn_reflns_theta_min         1.427
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.112
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       prism
_exptl_crystal_F_000             4624
_refine_diff_density_max         1.492
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 2276 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         5405
_refine_ls_number_restraints     1669
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0845
_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^)+(0.1753P)^2^+10.7774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2386
_refine_ls_wR_factor_ref         0.2587
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                5281
_reflns_number_total             5405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5072sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        12212(27)
_cod_database_code               2108657
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              86044
_shelx_hkl_checksum              55042
_cod_database_fobs_code 2108657