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_4134852
_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            'C101.83 H64.83 Cl14.48'
_chemical_formula_weight         1801.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                71.185(2)
_cell_angle_beta                 88.023(2)
_cell_angle_gamma                83.811(2)
_cell_formula_units_Z            4
_cell_length_a                   20.9020(8)
_cell_length_b                   20.9356(8)
_cell_length_c                   22.3508(8)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.73
_cell_measurement_theta_min      2.24
_cell_volume                     9204.0(6)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHEXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            98597
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        54.999
_diffrn_reflns_theta_max         54.999
_diffrn_reflns_theta_min         2.088
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    4.327
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
Some of solvent molecules (CHCl3, 58 electrons) are 
highly disordered and were treated by SQUEEZE' 
;
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1932
_refine_ls_number_reflns         23096
_refine_ls_number_restraints     1830
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.1065
_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^)+(0.2800P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3295
_refine_ls_wR_factor_ref         0.3545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16670
_reflns_number_total             23096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01117_si_002.cif
_cod_data_source_block           cu_jastir141_0m_a_sqd
_cod_database_code               4134852
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.723
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              79759
_shelx_hkl_checksum              87878