Dual-function Ni-based MOF for hydrogen storage and CO<sub>2</sub> to carbonate cyclic catalysis.
García-Rojas, Elena; Montes-Andrés, Helena; Tapiador, Jesús; Martos, Carmen; Salcedo-Abraira, Pablo; Choquesillo-Lazarte, Duane; Orcajo, Gisela; Leo, Pedro; Dalton transactions (Cambridge, England : 2003) 55 (2026) 761–774; doi:10.1039/d5dt02218e

data_7720497
_publ_section_title
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 Dual-function Ni-based MOF for hydrogen storage and CO<sub>2</sub> to
 carbonate cyclic catalysis.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              761
_journal_page_last               774
_journal_paper_doi               10.1039/d5dt02218e
_journal_volume                  55
_journal_year                    2026
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C25 H27 N5 Ni2 O11, 2.55[C3H7NO]'
_chemical_formula_sum            'C32.65 H43.13 N7.55 Ni2 O13.55'
_chemical_formula_weight         875.53
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
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2024-10-16 deposited with the CCDC.	2025-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7192(12)
_cell_length_b                   13.7192(12)
_cell_length_c                   45.094(4)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.991
_cell_measurement_theta_min      2.701
_cell_volume                     8487.4(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker Apex3, 2019'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_av_unetI/netI     0.1518
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            40553
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.040
_diffrn_reflns_theta_max         25.040
_diffrn_reflns_theta_min         2.770
_exptl_absorpt_coefficient_mu    0.955
_exptl_absorpt_correction_T_max  0.0908
_exptl_absorpt_correction_T_min  0.0677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0906 before and 0.0802 after correction.
The Ratio of minimum to maximum transmission is 0.7456.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             3650
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.005
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         7246
_refine_ls_number_restraints     875
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.1710
_refine_ls_R_factor_gt           0.1259
_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^)+(0.0477P)^2^+133.9200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2402
_refine_ls_wR_factor_ref         0.2548
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                5342
_reflns_number_total             7246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02218e2.cif
_cod_data_source_block           Ni-URJC-3
_cod_original_cell_volume        8487.5(17)
_cod_database_code               7720497
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(7)
 0.50(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N4-C3 \\sim N4-C7
 with sigma of 0.02
 N1-C12 \\sim N1-C14
 with sigma of 0.02
 N2-C1A \\sim N2-C1B
 with sigma of 0.02
 N3-C1D \\sim N3-C1E
 with sigma of 0.02
 Ni1-O37 \\sim Ni1-O37A
 with sigma of 0.02
 O37-C38 \\sim O37A-C38A
 with sigma of 0.02
 N39-C38 \\sim N39A-C38A
 with sigma of 0.02
 N39-C40 \\sim N39A-C40A
 with sigma of 0.02
 N39-C41 \\sim N39A-C41A
 with sigma of 0.02
 Ni1-C38 \\sim Ni1-C38A
 with sigma of 0.04
 O37-N39 \\sim O37A-N39A
 with sigma of 0.04
 C38-C40 \\sim C38A-C40A
 with sigma of 0.04
 C38-C41 \\sim C38A-C41A
 with sigma of 0.04
 C40-C41 \\sim C40A-C41A
 with sigma of 0.04
4. Restrained planarity
 C1, O2, N4, C3, C7
 with sigma of 0.1
 C11, O4, N1, C12, C14
 with sigma of 0.1
 C15, O5, N2, C1A, C1B
 with sigma of 0.1
 C1C, O6, N3, C1D, C1E
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C6 \\sim C5 \\sim C4 \\sim C13 \\sim C9 \\sim C8 \\sim C10 \\sim C16 \\sim C17
\\sim C26 \\sim C22 \\sim C21 \\sim C19 \\sim C18: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
C8 \\sim C6 \\sim C5 \\sim C4 \\sim C2 \\sim C13 \\sim C9 \\sim C10 \\sim N7:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A
C1 \\sim O2 \\sim N4 \\sim C3 \\sim C7: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C11 \\sim O4 \\sim N1 \\sim C12 \\sim C14: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C1 \\sim O2 \\sim N4 \\sim C3 \\sim C7 \\sim C11 \\sim O4 \\sim N1 \\sim C12
\\sim C14: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
C15 \\sim O5 \\sim N2 \\sim C1A \\sim C1B: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C1C \\sim O6 \\sim N3 \\sim C1D \\sim C1E: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O6 \\sim C1C \\sim N3 \\sim C1D \\sim C1E: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
C1A \\sim C15 \\sim O5 \\sim N2 \\sim C1B: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
N39 \\sim C40 \\sim C41 \\sim N39A \\sim C41A \\sim C40A \\sim O37 \\sim C38
\\sim O37A \\sim C38A: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1, O2, N4, C3, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, O4, N1, C12, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, O5, N2, C1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1C, O6, N3, C1D, C1E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C11)=Sof(H11)=Sof(O4)=Sof(N1)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=1-FVAR(1)
 Sof(C1)=Sof(O2)=Sof(N4)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C7)=FVAR(1)
 Sof(C15)=Sof(H15)=Sof(O5)=Sof(N2)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=FVAR(2)
 Sof(O37A)=Sof(C38A)=Sof(H38A)=Sof(N39A)=Sof(C41A)=Sof(H41D)=Sof(H41E)=
 Sof(H41F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(3)
 Sof(O37)=Sof(N39)=Sof(C38)=Sof(H38)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(3)
8.a Free rotating group:
 C1(O2,N4,C3,C7), C11(O4,N1,C12,C14), C15(O5,N2,C1A,C1B), C1C(O6,N3,C1D,C1E)
8.b Me refined with riding coordinates:
 C40(H40A,H40B,H40C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C41(H41A,H41B,
 H41C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C1A(H1AA,
 H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1D(H1DA,H1DB,H1DC), C1E(H1EA,H1EB,H1EC),
 C41A(H41D,H41E,H41F), C40A(H40D,H40E,H40F)
8.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C18(H18), C8(H8), C13(H13), C28(H28), C33(H33), C5(H5), C21(H21),
 C38(H38), C11(H11), C15(H15), C1C(H1C), C38A(H38A)
8.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              10791
_shelx_hkl_checksum              99420
_olex2_submission_special_instructions 'No special instructions were received'