Polar organic cages for efficiently separating azeotropic mixtures.
Alimi, Lukman O.; Liu, Xin; Zhang, Gengwu; Moosa, Basem; Khashab, Niveen M.; Chemical communications (Cambridge, England) 60 (2024) 10768–10771; doi:10.1039/d4cc03520h

data_7133621
_publ_section_title
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 Polar organic cages for efficiently separating azeotropic mixtures.
;
_journal_issue                   77
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10768
_journal_page_last               10771
_journal_paper_doi               10.1039/d4cc03520h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C36 H42 N8 O6, C7 H8'
_chemical_formula_sum            'C43 H50 N8 O6'
_chemical_formula_weight         774.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-09 deposited with the CCDC.	2024-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.251(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.658(3)
_cell_length_b                   9.8012(18)
_cell_length_c                   30.782(5)
_cell_measurement_reflns_used    5110
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      57.169
_cell_measurement_theta_min      2.909
_cell_volume                     4067.0(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            36177
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        65.083
_diffrn_reflns_theta_max         65.083
_diffrn_reflns_theta_min         2.909
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1078 before and 0.0620 after correction.
The Ratio of minimum to maximum transmission is 0.8611.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       Block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.985
_exptl_transmission_factor_min   0.976
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         6639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3527
_reflns_number_total             6639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03520h2.cif
_cod_data_source_block           DIHO-cage@Tol
_cod_depositor_comments
'Adding full bibliography for 7133620--7133624.cif.'
_cod_database_code               7133621
_shelx_shelxl_version_number     2019/1
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C13(H13A,H13B), C34(H34A,H34B), C33(H33A,H33B), C11(H11A,
 H11B), C23(H23A,H23B), C12(H12A,H12B), C24(H24A,H24B), C21(H21A,H21B),
 C22(H22A,H22B), C2(H2A,H2B), C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C31(H31), C36(H36), C17(H17), C25(H25), C32(H32), C10(H10), C6(H6A),
  C28(H28), C20(H20), C9(H9), C3(H3A), C42(H42), C38(H38), C39(H39), C40(H40),
 C41(H41)
2.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O5(H5), O6(H6), O3(H3), O2(H2), O1(H1)
;
_shelx_res_checksum              33392
_shelx_hkl_checksum              4995
_olex2_submission_special_instructions 'No special instructions were received'