Channel confinement and separation properties in an adaptive supramolecular framework using an adamantane tecton
Lutz, Nicholas; Bicknell, Josephine; Loya, Jesus Daniel; Reinheimer, Eric W.; Campillo-Alvarado, Gonzalo; CrystEngComm 26 (2024) 1067–1070; doi:10.1039/D4CE00037D

data_7248060
_publ_section_title
;
 Channel confinement and separation properties in an adaptive
 supramolecular framework using an adamantane tecton
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1067
_journal_page_last               1070
_journal_paper_doi               10.1039/D4CE00037D
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C34 H28 Br4), 8(C6 H6)'
_chemical_formula_sum            'C116 H104 Br8'
_chemical_formula_weight         2137.27
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-11
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-01-15 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   18.4930(7)
_cell_length_b                   18.4930(7)
_cell_length_c                   7.1799(5)
_cell_measurement_reflns_used    3670
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.3210
_cell_measurement_theta_min      2.1840
_cell_volume                     2455.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.81a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.84a 64-bit (release 16-02-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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     84.00 109.00   0.50   30.00    --   20.00  54.00 -60.00   50
  2  \w    -74.00 -34.00   0.50   30.00    --   20.00  54.00 150.00   80
  3  \w      3.00  29.00   0.50   30.00    --   20.00  54.00 150.00   52
  4  \w     73.00 109.00   0.50   30.00    --   20.00  54.00 150.00   72
  5  \w    -58.00 -32.00   0.50   30.00    --   20.00  54.00 -30.00   52
  6  \w    -14.00  94.00   0.50   30.00    --   20.00  54.00 -30.00  216
  7  \w    -55.00  23.00   0.50   30.00    --   20.00  54.00 -60.00  156
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0373978000
_diffrn_orient_matrix_UB_12      0.0002058000
_diffrn_orient_matrix_UB_13      -0.0223893000
_diffrn_orient_matrix_UB_21      0.0015105000
_diffrn_orient_matrix_UB_22      0.0378623000
_diffrn_orient_matrix_UB_23      -0.0156070000
_diffrn_orient_matrix_UB_31      0.0086333000
_diffrn_orient_matrix_UB_32      -0.0061895000
_diffrn_orient_matrix_UB_33      -0.0947694000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12261
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.363
_diffrn_reflns_theta_min         2.203
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.315
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.81a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.482(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0331P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.760
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2156
_reflns_number_total             2967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00037d2.cif
_cod_data_source_block           nl-17cryo-2
_cod_depositor_comments
'Adding full bibliography for 7248060--7248064.cif.'
_cod_original_cell_volume        2455.5(3)
_cod_database_code               7248060
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C116 H104 Br8'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51835
 0.48165
2. Others
 Fixed Sof: H00A(0.5) H00B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C002(H00A,H00B), C005(H00C,H00D)
3.b Aromatic/amide H refined with riding coordinates:
 C006(H006), C007(H007), C009(H009), C00A(H00E), C00B(H00F), C00C(H00G),
 C00D(H00H), C00E(H00I), C00F(H00J), C00G(H00K)
;
_shelx_res_checksum              37894
_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 12.228
_oxdiff_exptl_absorpt_empirical_full_min 0.564