A self-assembled supramolecular capsule that cocrystallizes with 1,4-disubstituted benzene derivatives
Wu, Yingcong; Ma, Wanzun; Wei, Dehui; Liu, Gen; Wei, Huiqi; Zhao, Xinyun; Wu, Lamei; Huang, Zhengxi; Zhang, Zhan; CrystEngComm 27 (2025) 2287–2291; doi:10.1039/D5CE00115C

data_7250639
_publ_section_title
;
 A self-assembled supramolecular capsule that cocrystallizes with
 1,4-disubstituted benzene derivatives
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2287
_journal_page_last               2291
_journal_paper_doi               10.1039/D5CE00115C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C43 H57 N5 O4, 0.25(C16 H8 N4)'
_chemical_formula_sum            'C47 H59 N6 O4'
_chemical_formula_weight         772.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-02
_audit_creation_method
; 
Olex2 1.3 
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) 
;
_audit_update_record
;
2025-01-23 deposited with the CCDC.	2025-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.797(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5541(10)
_cell_length_b                   25.3522(19)
_cell_length_c                   15.2379(11)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      59.44
_cell_measurement_theta_min      3.03
_cell_volume                     5062.5(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XM  (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Photon III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27051
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         59.468
_diffrn_reflns_theta_min         2.609
_diffrn_source_current           3.58
_diffrn_source_power             0.250421
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.013
_exptl_crystal_description       block
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.042
_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-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0751P)^2^+2.6374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4824
_reflns_number_total             5675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00115c2.cif
_cod_data_source_block           211108n_0m
_cod_database_code               7250639
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.952
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups, All N(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Others 
 Fixed Sof: C25(0.5) H25(0.5) C26(0.5) H26(0.5) 
3.a Riding coordinates: 
 C25(H25), C26(H26) 
3.b Secondary CH2 refined with riding coordinates: 
 C10(H10A,H10B), C8(H8A,H8B), C18(H18A,H18B), C21(H21A,H21B), C16(H16A,H16B) 
3.c Aromatic/amide H refined with riding coordinates: 
 N004(H004), N005(H005), C1(H1), C2(H2) 
3.d Idealised Me refined as rotating group: 
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C22(H22A,H22B, 
 H22C), C19(H19A,H19B,H19C) 
;
_olex2_submission_special_instructions 'No special instructions were received'