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_7248062
_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, C H Cl3'
_chemical_formula_sum            'C35 H29 Br4 Cl3'
_chemical_formula_weight         875.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 101.643(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7063(12)
_cell_length_b                   7.1729(5)
_cell_length_c                   25.574(2)
_cell_measurement_reflns_used    1774
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      21.2860
_cell_measurement_theta_min      2.4580
_cell_volume                     3360.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.81a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.94a 64-bit (release 21-06-2023))'
_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    -23.00  71.00   0.50   47.00    --   20.00  54.00-150.00  188
  2  \w    -74.00 -30.00   0.50   47.00    --   20.00  54.00 -60.00   88
  3  \w    -22.00  10.00   0.50   47.00    --   20.00  54.00 -60.00   64
  4  \w     17.00  43.00   0.50   47.00    --   20.00  54.00 -60.00   52
  5  \w     70.00  97.00   0.50   47.00    --   20.00  54.00 -60.00   54
  6  \w      4.00  44.00   0.50   47.00    --   20.00  54.00-180.00   80
  7  \w     72.00  98.00   0.50   47.00    --   20.00  54.00-180.00   52
  8  \w    -72.00  69.00   0.50   47.00    --   20.00  54.00 -90.00  282
  9  \w     -6.00  19.00   0.50   47.00    --   20.00  54.00  60.00   50
 10  \w    -63.00  25.00   0.50   47.00    --   20.00  54.00 -30.00  176
 11  \w    -66.00 -41.50   0.50   47.00    --   20.00  54.00-150.00   49
;
_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      0.0148810000
_diffrn_orient_matrix_UB_12      -0.0078195000
_diffrn_orient_matrix_UB_13      0.0276533000
_diffrn_orient_matrix_UB_21      0.0355592000
_diffrn_orient_matrix_UB_22      -0.0077374000
_diffrn_orient_matrix_UB_23      -0.0055536000
_diffrn_orient_matrix_UB_31      0.0039372000
_diffrn_orient_matrix_UB_32      0.0983743000
_diffrn_orient_matrix_UB_33      0.0018780000
_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  0.0758
_diffrn_reflns_av_unetI/netI     0.1008
_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       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11599
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.120
_diffrn_reflns_theta_max         25.120
_diffrn_reflns_theta_min         2.476
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.053
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.502
_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    1.730
_exptl_crystal_description       plate
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.022
_refine_diff_density_max         1.779
_refine_diff_density_min         -1.347
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2975
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0805P)^2^+30.7269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1915
_reflns_number_total             2975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00037d2.cif
_cod_data_source_block           nl-18cryo2
_cod_depositor_comments
'Adding full bibliography for 7248060--7248064.cif.'
_cod_database_code               7248062
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C140 H116 Br16 Cl12'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 Cl1, Cl2, Cl3, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: H15A(0.5) H15B(0.5) H18A(0.5) H18B(0.5) Cl2(0.5) Cl1(0.5) Cl3(0.5)
 C19(0.5) H19(0.5)
4.a Free rotating group:
 Cl2(Cl1,Cl3,C19)
4.b Ternary CH refined with riding coordinates:
 C19(H19)
4.c Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12)
;
_shelx_res_checksum              79292
_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 1.780
_oxdiff_exptl_absorpt_empirical_full_min 0.704