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_7248063
_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(C17 H14 Br2), C7 H8'
_chemical_formula_sum            'C41 H36 Br4'
_chemical_formula_weight         848.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 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                90
_cell_angle_beta                 94.187(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2611(14)
_cell_length_b                   7.1873(7)
_cell_length_c                   25.1626(19)
_cell_measurement_reflns_used    1590
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      23.5450
_cell_measurement_theta_min      2.1420
_cell_volume                     3474.1(5)
_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 0.998
_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    -16.00  15.00   0.50    6.00    --   20.00  54.00-150.00   62
  2  \w     68.00  94.00   0.50    6.00    --   20.00  54.00-150.00   52
  3  \w    -70.00 104.00   0.50    6.00    --   20.00  54.00  60.00  348
  4  \w    -69.00 -31.00   0.50    6.00    --   20.00  54.00-180.00   76
  5  \w    -21.00  39.00   0.50    6.00    --   20.00  54.00-180.00  120
  6  \w     76.00 101.00   0.50    6.00    --   20.00  54.00-180.00   50
  7  \w    -48.00 -23.00   0.50    6.00    --   20.00  54.00   0.00   50
  8  \w    -11.00  14.00   0.50    6.00    --   20.00  54.00   0.00   50
  9  \w     32.00  71.00   0.50    6.00    --   20.00  54.00   0.00   78
 10  \w      4.00  60.00   0.50    6.00    --   20.00  54.00 -60.00  112
;
_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      -0.0302584000
_diffrn_orient_matrix_UB_12      0.0256709000
_diffrn_orient_matrix_UB_13      -0.0160915000
_diffrn_orient_matrix_UB_21      -0.0175410000
_diffrn_orient_matrix_UB_22      0.0187902000
_diffrn_orient_matrix_UB_23      0.0232436000
_diffrn_orient_matrix_UB_31      0.0118518000
_diffrn_orient_matrix_UB_32      0.0933758000
_diffrn_orient_matrix_UB_33      -0.0002859000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11552
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.120
_diffrn_reflns_theta_max         25.120
_diffrn_reflns_theta_min         2.435
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.662
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.408
_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    1.622
_exptl_crystal_description       plate
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Flack x determined using 1357 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         11552
_refine_ls_number_restraints     370
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0132P)^2^+24.3319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1064
_reflns_Friedel_coverage         0.660
_reflns_Friedel_fraction_full    0.785
_reflns_Friedel_fraction_max     0.785
_reflns_number_gt                9515
_reflns_number_total             11552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00037d2.cif
_cod_data_source_block           nl-20cryo
_cod_depositor_comments
'Adding full bibliography for 7248060--7248064.cif.'
_cod_database_code               7248063
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C164 H144 Br16'
_shelx_estimated_absorpt_t_max   0.767
_shelx_estimated_absorpt_t_min   0.360
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.892(3)
 0.108(3)
2. 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
3. Uiso/Uaniso restraints and constraints
C5 \\sim C6: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C1 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C3 \\sim C4: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 H21, Br3, Br4, C19, C20, H20, C21, C22, C23, H23, C24, H24, C25, C26, H26,
 C27, H27, C28, C29, H29, C30, H30, C31, C32, C33, H33A, H33B, C34, H34A, H34B,
 C35, H35A, H35B, C36, H36A, H36B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Br1, C1, C2, H2, Br2, C3, H3, C4, C5, H5, C6, H6, C7, C8, H8, C9, H9, C10,
 C11, H11, C12, H12, C13, C14, C15, H15A, H15B, C16, H16A, H16B, C17, H17A,
 H17B, C18, H18A, H18B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 H42, H43, H41, C38, C39, H39, C40, H40, C41, C42, C43, C44, H44A, H44B, H44C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: H17A(0.5) H17B(0.5) H18A(0.5) H18B(0.5) H34A(0.5) H34B(0.5)
 H36A(0.5) H36B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C20(H20),
 C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C39(H39),
  C40(H40), C41(H41), C42(H42), C43(H43)
6.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C)
;
_shelx_res_checksum              40454
_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 1.308
_oxdiff_exptl_absorpt_empirical_full_min 0.880