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_1575339
_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         '0.25(C48 H68 Co4 N16 O16), 3[H2O]'
_chemical_formula_sum            'C12 H23 Co N4 O7'
_chemical_formula_weight         394.27
_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             2025-07-02
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_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            16
_cell_length_a                   18.6622(13)
_cell_length_b                   18.6622(13)
_cell_length_c                   21.2684(16)
_cell_measurement_reflns_used    3024
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.69
_cell_measurement_theta_min      2.46
_cell_volume                     7407.3(9)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21179
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.759
_diffrn_reflns_theta_min         1.452
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1868
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0577P)^2^+6.9580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1257
_reflns_number_total             1868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02892b2.cif
_cod_data_source_block           ZSA-13
_cod_depositor_comments
'Adding full bibliography for 1575339--1575340.cif.'
_cod_original_cell_volume        7407.3(12)
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               1575339
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.781
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6A-C5A = C6-C5 = C7-C6 = C7A-C6A
 1.5 with sigma of 0.02
 N2-C5A = N2-C5
 1.4 with sigma of 0.02
 C7-C7_$1 = C7A-C7A_$1
 1.5 with sigma of 0.02
 C5-C6 \\sim C5A-C6
 with sigma of 0.02
 C5-N2 \\sim C5A-N2
 with sigma of 0.02
 C6-C7 \\sim C6-C7A
 with sigma of 0.02
 C6-C7A \\sim C6A-C7A
 with sigma of 0.02
 C5-C6 \\sim C5-C6A
 with sigma of 0.02
 C6-C7 \\sim C6A-C7
 with sigma of 0.02
 C6-C5A \\sim C6A-C5A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Others
 Sof(H2BC)=Sof(H2BD)=Sof(C5A)=Sof(H5A)=1-FVAR(1)
 Sof(C5)=Sof(H5)=Sof(H2AA)=Sof(H2AB)=FVAR(1)
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=1-FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=FVAR(2)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(3)
 Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(3)
 Fixed Sof: H4A(0.5) H4B(0.5) H4C(0.5)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C5A(H5A)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), N2(H2AA,H2AB), N2(H2BC,H2BD), C7A(H7AA,H7AB),
 C6A(H6AA,H6AB)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              65800
_shelx_fab_checksum              30582
_olex2_submission_special_instructions 'No special instructions were received'