Coexisting gases regulate the rates of water adsorption by a flexible one-dimensional coordination polymer.
Wang, AnQi; Zheng, Xin; Saito, Yuki; Tateishi, Arata; Huang, Yuan; Kamiya, Yuichi; Sato, Hiroyasu; Kondo, Atsushi; Takahashi, Kiyonori; Nakamura, Takayoshi; Noro, Shin-Ichiro; Chemical science 16 (2025) 18135–18140; doi:10.1039/d5sc01699a

data_1575545
_publ_section_title
;
 Coexisting gases regulate the rates of water adsorption by a flexible
 one-dimensional coordination polymer.
;
_journal_issue                   39
_journal_name_full               'Chemical science'
_journal_page_first              18135
_journal_page_last               18140
_journal_paper_doi               10.1039/d5sc01699a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C27 H22 Cu2 N2 O11'
_chemical_formula_sum            'C27 H22 Cu2 N2 O11'
_chemical_formula_weight         677.57
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-29
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                94.47(2)
_cell_angle_beta                 94.64(2)
_cell_angle_gamma                111.54(3)
_cell_formula_units_Z            2
_cell_length_a                   9.462(3)
_cell_length_b                   9.915(3)
_cell_length_c                   15.687(3)
_cell_measurement_reflns_used    694
_cell_measurement_temperature    293
_cell_measurement_theta_max      0.8730
_cell_measurement_theta_min      0.0780
_cell_volume                     1355.2(7)
_computing_cell_refinement       'CrysAlisPro 1.171.44.76a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.136a 64-bit (release 23-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.44.76a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 0.555
_diffrn_measured_fraction_theta_max 0.552
_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    -50.00  50.00   0.50    1.25    --    0.00   0.00   0.00  200
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'continuous rotation electron diffraction'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0022060000
_diffrn_orient_matrix_UB_12      -0.0006003000
_diffrn_orient_matrix_UB_13      -0.0004521000
_diffrn_orient_matrix_UB_21      -0.0011213000
_diffrn_orient_matrix_UB_22      -0.0024613000
_diffrn_orient_matrix_UB_23      0.0005212000
_diffrn_orient_matrix_UB_31      -0.0014572000
_diffrn_orient_matrix_UB_32      -0.0010440000
_diffrn_orient_matrix_UB_33      -0.0014616000
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.1967
_diffrn_reflns_av_unetI/netI     0.3250
_diffrn_reflns_Laue_measured_fraction_full 0.555
_diffrn_reflns_Laue_measured_fraction_max 0.552
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5778
_diffrn_reflns_point_group_measured_fraction_full 0.555
_diffrn_reflns_point_group_measured_fraction_max 0.552
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.899
_diffrn_reflns_theta_min         0.046
_diffrn_source                   'electron diffractometer'
_diffrn_source_type              'JEOL JSM-2300ED, LaB6'
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.76a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       block
_exptl_crystal_F_000             234
_exptl_crystal_size_max          0.0007
_exptl_crystal_size_mid          0.0003
_exptl_crystal_size_min          0.0001
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       34907(31)
_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   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         3060
_refine_ls_number_restraints     211
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.2993
_refine_ls_R_factor_gt           0.2093
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4185
_refine_ls_wR_factor_ref         0.4895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1093
_reflns_number_total             3060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01699a2.cif
_cod_data_source_block           1DCuCP
_cod_depositor_comments
'Adding full bibliography for 1575544--1575545.cif.'
_cod_database_code               1575545
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Cu'
_diffrn_oxdiff_scatteringfactors_ed
;
UCLA (2022) https://srv.mbi.ucla.edu/faes/data
;
_diffrn_oxdiff_digest_creation
;
CAP 1.171.44.76a, AC 1.5-ac7-010
;
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O9-H9
 0.82 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim O9 \\sim C24 \\sim C25 \\sim C20 \\sim C19:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O5 \\sim O4 \\sim C12: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C26 \\sim O10 \\sim O11 \\sim C27: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C14 \\sim C13 \\sim C12 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim O6:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C11 \\sim C10 \\sim O3 \\sim C6 \\sim C5 \\sim C7 \\sim C8 \\sim C9: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C1 \\sim N2 \\sim N1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
4.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C1(H1), C17(H17), C21(H21), C23(H23), C2(H2), C18(H18), C8(H8),
 C16(H16), C25(H25), C11(H11), C3(H3A), C4(H4), C24(H24), C7(H7), C9(H9A)
4.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C)
4.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6)
;
_shelx_res_checksum              13996
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.772
_oxdiff_exptl_absorpt_empirical_full_min 0.809
_oxdiff_exptl_crystal_thickness  1000.0