Exploration of the Solid-State Sorption Properties of Shape-persistent Macrocyclic Nanocarbons as Bulk Materials and Small Aggregates.
Schaub, Tobias A.; Prantl, Ephraim A.; Kohn, Julia; Bursch, Markus; Marshall, Checkers R.; Leonhardt, Erik James; Lovell, Terri C.; Zakharov, Lev N.; Brozek, Carl K.; Waldvogel, Siegfried R.; Grimme, Stefan; Jasti, Ramesh; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c01117

data_4134853
_publ_section_title
;
 Exploration of the Solid-State Sorption Properties of Shape-persistent
 Macrocyclic Nanocarbons as Bulk Materials and Small Aggregates.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01117
_journal_year                    2020
_chemical_formula_sum            'C123 H116 N4 O7.5'
_chemical_formula_weight         1770.19
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.970(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.384(3)
_cell_length_b                   15.8148(13)
_cell_length_c                   32.575(3)
_cell_measurement_reflns_used    5208
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      52.51
_cell_measurement_theta_min      3.02
_cell_volume                     19727(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            54002
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        66.913
_diffrn_reflns_theta_max         66.913
_diffrn_reflns_theta_min         2.308
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       strip
_exptl_crystal_F_000             7536
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
In symmetrically independent part of the crystal 
there are 7.5 solvent THF molecules, OC4H8 (40 electrons).
Five of them were located and refined. Others are highly 
disordered and were treated by SQUEEZE.
;
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         17075
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1416
_refine_ls_R_factor_gt           0.0876
_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^)+(0.1544P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2435
_refine_ls_wR_factor_ref         0.2743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8769
_reflns_number_total             17075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01117_si_004.cif
_cod_data_source_block           cu_jastirr162_0m_a_sqd
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C123 H116 N4 O7.50'
_cod_database_code               4134853
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.884
_shelx_estimated_absorpt_t_max   0.989
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              29096
_shelx_hkl_checksum              17641