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_4134851
_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            'C124 H82 Cl6'
_chemical_formula_weight         1784.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.073(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0821(11)
_cell_length_b                   24.2024(15)
_cell_length_c                   24.6475(14)
_cell_measurement_reflns_used    3297
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      41.21
_cell_measurement_theta_min      2.64
_cell_volume                     10131.3(11)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker ApexII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_unetI/netI     0.1196
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37530
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        49.851
_diffrn_reflns_theta_max         49.851
_diffrn_reflns_theta_min         2.641
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    1.920
_exptl_absorpt_correction_T_max  0.7498
_exptl_absorpt_correction_T_min  0.5805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             3712
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
A mixute of CH2Cl2 and C5H12 solvent molecules are highly 
disordered in six positions in the full unit cell.
These solvents were not recognized and not included
in the total formula given in this CIf file.  
;
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.077
_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     1171
_refine_ls_number_reflns         10263
_refine_ls_number_restraints     1108
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1996
_refine_ls_R_factor_gt           0.1187
_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^)+(0.1850P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3055
_refine_ls_wR_factor_ref         0.3470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4417
_reflns_number_total             10263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01117_si_003.cif
_cod_data_source_block           cu_jastir157_0m_a_sqd
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4134851
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.788
_shelx_estimated_absorpt_t_max   0.945
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              53427
_shelx_hkl_checksum              68822