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_7248064
_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_formula_moiety         'C34 H28 Br4'
_chemical_formula_sum            'C34 H28 Br4'
_chemical_formula_weight         756.20
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-18
_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                67.615(5)
_cell_angle_beta                 80.075(5)
_cell_angle_gamma                74.356(5)
_cell_formula_units_Z            4
_cell_length_a                   10.8095(7)
_cell_length_b                   15.4233(9)
_cell_length_c                   19.8301(10)
_cell_measurement_reflns_used    10103
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      24.8690
_cell_measurement_theta_min      1.9620
_cell_volume                     2934.6(3)
_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 0.995
_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    -66.00 -34.00   0.50   25.00    --   20.00  54.00-150.00   64
  2  \w     -1.00  49.00   0.50   25.00    --   20.00  54.00-150.00  100
  3  \w     71.00 108.00   0.50   25.00    --   20.00  54.00-150.00   74
  4  \w    -73.00   3.00   0.50   25.00    --   20.00  54.00  60.00  152
  5  \w     21.00  48.00   0.50   25.00    --   20.00  54.00  60.00   54
  6  \w     71.00 105.00   0.50   25.00    --   20.00  54.00  60.00   68
  7  \w    -73.00  -9.00   0.50   25.00    --   20.00  54.00 -60.00  128
  8  \w    -70.00  88.00   0.50   25.00    --   20.00  54.00  90.00  316
  9  \w    -66.00 -13.00   0.50   25.00    --   20.00  54.00 -30.00  106
 10  \w      3.00 107.00   0.50   25.00    --   20.00  54.00 -30.00  208
 11  \w    -65.00 -38.00   0.50   25.00    --   20.00  54.00-180.00   54
 12  \w     34.00  60.00   0.50   25.00    --   20.00  54.00-180.00   52
 13  \w      3.00  28.00   0.50   25.00    --   20.00  54.00 -90.00   50
 14  \w    -64.00  28.00   0.50   25.00    --   20.00  54.00   0.00  184
 15  \w    -71.00 -43.00   0.50   25.00    --   20.00  54.00-120.00   56
 16  \w    -29.00   0.00   0.50   25.00    --   20.00  54.00 150.00   58
 17  \w     13.00  38.00   0.50   25.00    --   20.00  54.00 150.00   50
 18  \w    -69.00  29.00   0.50   25.00    --   20.00  54.00 120.00  196
 19  \w    -65.00   7.00   0.50   25.00    --   20.00  54.00 143.38  144
;
_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      -0.0071932000
_diffrn_orient_matrix_UB_12      0.0441988000
_diffrn_orient_matrix_UB_13      -0.0299976000
_diffrn_orient_matrix_UB_21      -0.0091954000
_diffrn_orient_matrix_UB_22      0.0252807000
_diffrn_orient_matrix_UB_23      0.0244355000
_diffrn_orient_matrix_UB_31      0.0673477000
_diffrn_orient_matrix_UB_32      -0.0034293000
_diffrn_orient_matrix_UB_33      -0.0029487000
_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  0.0676
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39921
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         1.962
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.508
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.422
_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    1.712
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.272
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0584P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6694
_reflns_number_total             10436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00037d2.cif
_cod_data_source_block           nl-19cryo8
_cod_depositor_comments
'Adding full bibliography for 7248060--7248064.cif.'
_cod_original_cell_volume        2934.7(3)
_cod_database_code               7248064
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C34 H28 Br4'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B),
 C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C36(H36),
  C37(H37), C39(H39), C40(H40), C42(H42), C43(H43), C45(H45), C46(H46),
 C48(H48), C49(H49), C51(H51), C52(H52), C54(H54), C55(H55), C57(H57), C58(H58)
;
_shelx_res_checksum              70055
_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 1.881
_oxdiff_exptl_absorpt_empirical_full_min 0.574