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_7248061
_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         'C34 H28 Br4, C8 H10'
_chemical_formula_sum            'C42 H38 Br4'
_chemical_formula_weight         862.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-15 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.729(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.1953(3)
_cell_length_b                   25.4666(9)
_cell_length_c                   10.1699(4)
_cell_measurement_reflns_used    6228
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      25.9550
_cell_measurement_theta_min      2.0970
_cell_volume                     1775.03(13)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      101(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -73.00 -23.00   0.50    8.00    --   20.00  54.00 -90.00  100
  2  \w    -18.00  64.00   0.50    8.00    --   20.00  54.00 -90.00  164
  3  \w     67.00 104.00   0.50    8.00    --   20.00  54.00 -90.00   74
  4  \w    -74.00  56.00   0.50    8.00    --   20.00  54.00-180.00  260
  5  \w     63.00  91.00   0.50    8.00    --   20.00  54.00-180.00   56
  6  \w    -19.00   7.00   0.50    8.00    --   20.00  54.00   0.00   52
  7  \w     47.00  72.00   0.50    8.00    --   20.00  54.00   0.00   50
  8  \w    -16.00   9.00   0.50    8.00    --   20.00  54.00 -60.00   50
  9  \w     40.00  65.00   0.50    8.00    --   20.00  54.00 -60.00   50
 10  \w    -72.00 110.00   0.50    8.00    --   20.00  54.00  60.00  364
;
_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      0.0793050000
_diffrn_orient_matrix_UB_12      -0.0131404000
_diffrn_orient_matrix_UB_13      0.0474939000
_diffrn_orient_matrix_UB_21      -0.0502396000
_diffrn_orient_matrix_UB_22      0.0005431000
_diffrn_orient_matrix_UB_23      0.0501397000
_diffrn_orient_matrix_UB_31      -0.0435137000
_diffrn_orient_matrix_UB_32      -0.0245657000
_diffrn_orient_matrix_UB_33      -0.0242281000
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14726
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         2.102
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.564
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.376
_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    1.613
_exptl_crystal_description       plate
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 2218 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6146
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0191P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.936
_reflns_number_gt                5485
_reflns_number_total             6146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00037d2.cif
_cod_data_source_block           nl-23cryo3
_cod_depositor_comments
'Adding full bibliography for 7248060--7248064.cif.'
_cod_database_code               7248061
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C42H38Br4
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.317
_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.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C33(H33A,H33B), C34(H34A,H34B), C32(H32A,H32B), C30(H30A,
 H30B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C36(H36), C17(H17), C12(H12), C39(H39), C9(H9), C2(H2), C11(H11),
 C20(H20), C24(H24), C8(H8), C18(H18), C3(H3), C21(H21), C40(H40), C5(H5),
 C14(H14), C6(H6), C23(H23), C15(H15)
2.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              35044
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.438
_oxdiff_exptl_absorpt_empirical_full_min 0.748