Guest water-induced reversible regulation of proton conduction in a two-dimensional nickel(II) coordination polymer
Sun, Ao-Na; Dong, Fu-Wan; Chen, Yi; Zhang, Si-Chen; Liu, Rui-Han; Zhu, Junlun; Shao, Dong; CrystEngComm  (2025) –; doi:10.1039/D5CE00938C

data_7251297
_publ_section_title
;
 Guest water-induced reversible regulation of proton conduction in a
 two-dimensional nickel(II) coordination polymer
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00938C
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C36 H42 N4 Ni2 O14, 2.125(H2 O)'
_chemical_formula_sum            'C36 H46.25 N4 Ni2 O16.12'
_chemical_formula_weight         910.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-09-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-09-24 deposited with the CCDC.	2025-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.347(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9528(19)
_cell_length_b                   19.424(4)
_cell_length_c                   23.595(4)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    360(2)
_cell_measurement_theta_max      23.22
_cell_measurement_theta_min      2.27
_cell_volume                     4500.9(15)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      360(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture_Air'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26516
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        23.355
_diffrn_reflns_theta_max         23.355
_diffrn_reflns_theta_min         2.272
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1901
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         6273
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+38.1444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.928
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                5532
_reflns_number_total             6273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00938c2.cif
_cod_data_source_block           a_a_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7251297
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.891
_exptl_crystal_mounting_method
;
 Crystals were removed from the crystallisation vial and immediately coated
 with PDMS (polydimethylsiloxane/Dimethicone, CAS: 9006-65-9 on a glass slide.
 A suitable single crystal was selected and mounted on a glass fiber using
 vacuum silicone grease as adhesive. The glass fiber with single crystal was
 mounted on copper pin with solid paraffin. Operator: DJ_Tokyo.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(4)
 0.47(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
N3 \\sim C13 \\sim C2 \\sim C15 \\sim C17 \\sim C31 \\sim C33 \\sim C35 \\sim
C2A \\sim C15A \\sim C17A \\sim C31A \\sim C33A \\sim C35A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O17) \\sim Ueq, Uanis(O18) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Same fragment restrains
{N3, C13, C2A, C15A, C17A, C31A, C33A, C35A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{N3, C13, C2, C15, C17, C31, C33, C35}
5. Others
 Sof(H13C)=Sof(H13D)=Sof(C2A)=Sof(H2A)=Sof(C15A)=Sof(H15A)=Sof(C17A)=Sof(H17C)=
 Sof(H17D)=Sof(C31A)=Sof(C33A)=Sof(H33A)=Sof(C35A)=Sof(H35A)=1-FVAR(1)
 Sof(H13A)=Sof(H13B)=Sof(C2)=Sof(H2)=Sof(C15)=Sof(H15)=Sof(C17)=Sof(H17A)=
 Sof(H17B)=Sof(C31)=Sof(C33)=Sof(H33)=Sof(C35)=Sof(H35)=FVAR(1)
 Fixed Sof: O18(0.5) H18A(0.5) H18B(0.5) O19(0.5) H19A(0.5) H19B(0.5)
 O17(0.125) H17E(0.125) H17F(0.125)
6.a Riding coordinates:
 O1(H1A,H1B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B), O17(H17E,H17F)
6.b Rotating group:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B), O10(H10A,H10B), O11(H11A,H11B)
6.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C13(H13C,H13D), C17(H17A,H17B), C23(H23A,H23B), C25(H25A,
 H25B), C29(H29A,H29B), C36(H36A,H36B), C17A(H17C,H17D)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C15(H15), C33(H33), C35(H35), C3(H3), C4(H4), C5(H5), C9(H9),
 C11(H11), C12(H12), C18(H18), C19(H19), C21(H21), C22(H22), C26(H26), C27(H27),
  C28(H28), C34(H34), C2A(H2A), C15A(H15A), C33A(H33A), C35A(H35A)
;
_shelx_res_checksum              68705
_olex2_submission_special_instructions 'No special instructions were received'