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_7250642
_publ_section_title
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 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, 2(C3 H6 O)'
_chemical_formula_sum            'C49 H69 N5 O6'
_chemical_formula_weight         824.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-12
_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                104.8440(10)
_cell_angle_beta                 113.2370(10)
_cell_angle_gamma                90.513(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1297(6)
_cell_length_b                   14.6354(7)
_cell_length_c                   15.2121(7)
_cell_measurement_reflns_used    9250
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      60.08
_cell_measurement_theta_min      3.48
_cell_volume                     2380.1(2)
_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 0.965
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27901
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.993
_diffrn_reflns_theta_min         2.867
_diffrn_source_current           3.57
_diffrn_source_power             0.2497215
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.6845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0143(16)
_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   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         8726
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0804P)^2^+0.7082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7827
_reflns_number_total             8726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00115c2.cif
_cod_data_source_block           211011j_0m
_cod_database_code               7250642
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.927
_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. Restrained distances 
 C48-C49 \\sim C48A-C49A 
 with sigma of 0.02 
 C49-O6 \\sim C49A-O6A 
 with sigma of 0.04 
 C47-C48 \\sim C47A-C48A 
 with sigma of 0.02 
 C48-O6 \\sim C48A-O6A 
 with sigma of 0.02 
 C47-O6 \\sim C47A-O6A 
 with sigma of 0.04 
 C47-C49 \\sim C47A-C49A 
 with sigma of 0.04 
 C29-C30 \\sim C29A-C30A 
 with sigma of 0.02 
 C26-C30 \\sim C26-C30A 
 with sigma of 0.04 
 C26-C29 \\sim C26-C29A 
 with sigma of 0.02 
3. Uiso/Uaniso restraints and constraints 
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(O6) 
\\sim Ueq, Uanis(C47A) \\sim Ueq, Uanis(C48A) \\sim Ueq, Uanis(C49A) \\sim Ueq, 
Uanis(O6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 
4. Others 
 Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C48A)=Sof(C49A)=Sof(H49D)= 
 Sof(H49E)=Sof(H49F)=Sof(O6A)=1-FVAR(1) 
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=Sof(C49)=Sof(H49A)=Sof(H49B)= 
 Sof(H49C)=Sof(O6)=FVAR(1) 
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(2) 
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(2) 
5.a Secondary CH2 refined with riding coordinates: 
 C2(H2A,H2B), C8(H8A,H8B), C10(H10A,H10B), C16(H16A,H16B), C18(H18A,H18B), 
 C29(H29A,H29B), C31(H31A,H31B), C37(H37A,H37B), C39(H39A,H39B), C42(H42A,H42B), 
  C29A(H29C,H29D) 
5.b Aromatic/amide H refined with riding coordinates: 
 C21(H21), C22(H22), C23(H23), N1(H1), N2(H2), N4(H4), N5(H5) 
5.c Idealised Me refined as rotating group: 
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), 
 C19(H19A,H19B,H19C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C38(H38A,H38B, 
 H38C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A, 
 H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C47A(H47D,H47E,H47F), 
 C49A(H49D,H49E,H49F), C30A(H30D,H30E,H30F) 
;
_shelx_res_checksum              18093
_olex2_submission_special_instructions 'No special instructions were received'