A nonporous crystalline organic cage for selective water uptake and storage
Alimi, Lukman O.; Khalfay, Nida; Khlifi, Soumaya; Lin, Weibin; Moosa, Basem; Khashab, Niveen M.; Chemical Science  (2025) –; doi:10.1039/D5SC06328K

data_1576246
_publ_section_title
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 A nonporous crystalline organic cage for selective water uptake and
 storage
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC06328K
_journal_year                    2025
_chemical_formula_moiety         'C54 H54 N8 O3, H1.944 O0.944, 5(H2 O)'
_chemical_formula_sum            'C54 H65.94 N8 O8.95'
_chemical_formula_weight         970.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-02 deposited with the CCDC.	2025-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.611(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4759(12)
_cell_length_b                   10.6707(5)
_cell_length_c                   23.6099(13)
_cell_measurement_reflns_used    9194
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.236
_cell_measurement_theta_min      2.205
_cell_volume                     5064.2(5)
_computing_cell_refinement       '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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            353130
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.297
_diffrn_reflns_theta_min         1.591
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1455 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.9729.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       block
_exptl_crystal_F_000             2070
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         12571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0687P)^2^+2.8002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10702
_reflns_number_total             12571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06328k2.cif
_cod_data_source_block           Oba-cage@H2O
_cod_database_code               1576246
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.974
_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 O(H) groups, All O(H,H) groups
2. Others
 Sof(O4)=Sof(H4BA)=FVAR(1)
 Fixed Sof: H4A(0.5) H4BB(0.5)
3.a Free rotating group:
 O4(H4BA), O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B), O9(H9A,H9B), O8(H8A,H8B)
3.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C38(H38A,H38B), C37(H37A,H37B), C20(H20A,H20B), C1(H1A,H1B),
 C2(H2A,H2B), C39(H39A,H39B), C19(H19A,H19B), C54(H54A,H54B), C18(H18A,H18B),
 C36(H36A,H36B), C21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
 C43(H43), C6(H6), C48(H48), C42(H42), C30(H30), C49(H49), C51(H51), C52(H52),
 C17(H17), C16(H16), C24(H24), C22(H22), C53(H53), C11(H11), C27(H27), C28(H28),
  C31(H31), C45(H45), C40(H40), C35(H35), C34(H34), C25(H25), C33(H33),
 C46(H46), C3(H3), C12(H12), C9(H9), C14(H14), C8(H8), C15(H15)
;
_shelx_res_checksum              32273
_olex2_submission_special_instructions 'No special instructions were received'