Hysteresis in the gas sorption isotherms of metal-organic cages accompanied by subtle changes in molecular packing.
Craig, Gavin A.; Larpent, Patrick; Urabe, Hinano; Legrand, Alexandre; Bonneau, Mickaele; Kusaka, Shinpei; Furukawa, Shuhei; Chemical communications (Cambridge, England) 56 (2020) 3689–3692; doi:10.1039/d0cc00932f

data_7126334
_publ_section_title
;
 Hysteresis in the gas sorption isotherms of metal-organic cages
 accompanied by subtle changes in molecular packing.
;
_journal_issue                   25
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3689
_journal_page_last               3692
_journal_paper_doi               10.1039/d0cc00932f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C116 H94 Cu4 N2 O24'
_chemical_formula_sum            'C134 H136 Cu4 N8 O30'
_chemical_formula_weight         2592.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-18 deposited with the CCDC.	2020-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.051(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2966(4)
_cell_length_b                   17.7385(3)
_cell_length_c                   24.6648(5)
_cell_measurement_reflns_used    35516
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.3350
_cell_measurement_theta_min      1.9800
_cell_volume                     6666.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -85.00  93.00   0.50   16.00    --    4.00  45.00 120.00  356
  2  \w    -28.00   2.00   0.50   16.00    --  -16.40  45.00 -18.65   60
  3  \w      6.00  72.00   0.50   16.00    --  -16.40  45.00 -18.65  132
  4  \w    -33.00  73.00   0.50   16.00    --  -16.40  45.00  60.00  212
  5  \w   -105.00  72.00   0.50   16.00    --  -16.40  45.00  30.00  354
  6  \w    -88.00 -59.00   0.50   16.00    --  -16.40  45.00 -18.65   58
  7  \w    -12.00  16.00   0.50   16.00    --  -16.40  45.00 153.56   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0099989000
_diffrn_orient_matrix_UB_12      -0.0078115000
_diffrn_orient_matrix_UB_13      -0.0269757000
_diffrn_orient_matrix_UB_21      0.0012450000
_diffrn_orient_matrix_UB_22      0.0391950000
_diffrn_orient_matrix_UB_23      -0.0055251000
_diffrn_orient_matrix_UB_31      0.0454734000
_diffrn_orient_matrix_UB_32      0.0005538000
_diffrn_orient_matrix_UB_33      0.0086524000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            84020
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.896
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       plate
_exptl_crystal_F_000             2704
_exptl_crystal_preparation       'Gas sorption'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         12664
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+5.2946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9661
_reflns_number_total             12664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00932f2.cif
_cod_data_source_block           gac321_sq
_cod_database_code               7126334
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu4 C112 H80 O28 N2'
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.816
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1M-O1M
 1.38 with sigma of 0.02
 O1M-H1M
 0.82 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C52(H52A,H52B), C53(H53A,H53B)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C37(H37), C23(H23), C41(H41), C50(H50), C12(H12), C46(H46),
 C21(H21), C39(H39), C47(H47), C38(H38), C6(H6), C2(H2), C48(H48), C31(H31),
 C33(H33), C4(H4), C29(H29), C10(H10), C19(H19), C20(H20), C11(H11), C2D(H2D)
3.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C4D(H4DA,H4DB,H4DC), C5D(H5DA,H5DB,H5DC), C54(H54A,H54B,
 H54C), C1M(H1MA,H1MB,H1MC)
;
_shelx_res_checksum              9552
_shelx_fab_checksum              14596
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.608