Ambidextrous fine-tuning of zeolite-like hydrogen-bonded organic frameworks (HOFs) <i>via</i> scalable green synthesis for efficient biogas upgrading.
Tang, Baobing; Yu, Xueyue; Li, Guanghua; Liu, Xin; Li, Jiantang; Liu, Yunling; Chemical science 16 (2025) 19130–19139; doi:10.1039/d5sc02892b

data_1575340
_publ_section_title
;
 Ambidextrous fine-tuning of zeolite-like hydrogen-bonded organic
 frameworks (HOFs) <i>via</i> scalable green synthesis for efficient
 biogas upgrading.
;
_journal_issue                   41
_journal_name_full               'Chemical science'
_journal_page_first              19130
_journal_page_last               19139
_journal_paper_doi               10.1039/d5sc02892b
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '2(C44 H60 Co4 N16 O16)'
_chemical_formula_sum            'C88 H120 Co8 N32 O32'
_chemical_formula_weight         2609.59
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-04
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-04 deposited with the CCDC.	2025-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.2801(3)
_cell_length_b                   17.2801(3)
_cell_length_c                   23.4245(11)
_cell_measurement_reflns_used    3985
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.86
_cell_volume                     6994.6(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.00
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10132
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.353
_diffrn_reflns_theta_min         2.863
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6264
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0590 before and 0.0407 after correction.
The Ratio of minimum to maximum transmission is 0.8406.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         1699
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0712
_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^)+(0.1256P)^2^+21.4359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1350
_reflns_number_total             1699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02892b2.cif
_cod_data_source_block           ZSA-12
_cod_depositor_comments
'Adding full bibliography for 1575339--1575340.cif.'
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               1575340
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.907
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 Co1-N2 = Co1-N2' = Co1-N2" = Co1-N2A
 2.1 with sigma of 0.02
 N2-C4 = C4-C5 = C5-C6 = C6-C6A = N2A-C4A = C4A-C5A = C5A-C6A
 1.5 with sigma of 0.02
 C5-C6A = C5A-C6
 2.6 with sigma of 0.02
 C4-C4A
 1.5 with sigma of 0.02
 C4'-C4"
 1.5 with sigma of 0.01
 C6'-C4" \\sim C6"-C4' \\sim C5'-C5"
 with sigma of 0.02
 C4"-C5' \\sim C4'-C5"
 with sigma of 0.02
 C4A-C6 \\sim C4-C6A \\sim C5-C5A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2 \\sim C4 \\sim C5 \\sim C6 \\sim C4A \\sim C5A \\sim C6A \\sim N2' \\sim C4'
\\sim C5' \\sim C6' \\sim N2" \\sim C4" \\sim C5" \\sim C6": within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq,
Uanis(N2') \\sim Ueq, Uanis(C4') \\sim Ueq, Uanis(C5') \\sim Ueq, Uanis(C6')
\\sim Ueq, Uanis(N2") \\sim Ueq, Uanis(C4") \\sim Ueq, Uanis(C5") \\sim Ueq,
Uanis(C6") \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4") = Uanis(N2A)
4. Others
 Fixed Sof: N2(0.25) H2A(0.25) H2B(0.25) C4(0.25) H4(0.25) C5(0.25) H5A(0.25)
 H5B(0.25) C6(0.25) H6A(0.25) H6B(0.25) N2A(0.25) H2AA(0.25) H2AB(0.25)
 C4A(0.25) H4A(0.25) C5A(0.25) H5AA(0.25) H5AB(0.25) C6A(0.25) H6AA(0.25)
 H6AB(0.25) N2'(0.25) H2'A(0.25) H2'B(0.25) C4'(0.25) H4'(0.25) C5'(0.25)
 H5'A(0.25) H5'B(0.25) C6'(0.25) H6'A(0.25) H6'B(0.25) N2"(0.25) H2"A(0.25)
 H2"B(0.25) C4"(0.25) H4"(0.25) C5"(0.25) H5"A(0.25) H5"B(0.25) C6"(0.25)
 H6"A(0.25) H6"B(0.25)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C4A(H4A), C4'(H4'), C4"(H4")
5.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), N2A(H2AA,H2AB), C5A(H5AA,H5AB),
 C6A(H6AA,H6AB), N2'(H2'A,H2'B), C5'(H5'A,H5'B), C6'(H6'A,H6'B), N2"(H2"A,H2"B),
  C5"(H5"A,H5"B), C6"(H6"A,H6"B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34233
_shelx_fab_checksum              81451
_olex2_submission_special_instructions 'No special instructions were received'