From 3-fold to 6-fold: tuning interpenetration of Zn-triphenylenehexathiolate MOF through precursor hydration
Qin, Haihan; Hu, Jieying; Li, Jian-Rong; Jiang, Long; Chung, Lai-Hon; He, Jun; CrystEngComm  (2026) –; doi:10.1039/D6CE00077K

data_7251777
_publ_section_title
;
 From 3-fold to 6-fold: tuning interpenetration of
 Zn-triphenylenehexathiolate MOF through precursor hydration
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2305
_journal_page_last               2310
_journal_paper_doi               10.1039/D6CE00077K
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         'C108 H36 S36 Zn9, C6 H24 N6 Zn'
_chemical_formula_sum            'C114 H60 N6 S36 Zn10'
_chemical_formula_weight         3321.54
_chemical_name_systematic        Zn-HTT
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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             2025-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-08-06 deposited with the CCDC.	2026-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                112.136(2)
_cell_angle_beta                 92.155(2)
_cell_angle_gamma                91.899(2)
_cell_formula_units_Z            2
_cell_length_a                   20.8124(10)
_cell_length_b                   24.2224(11)
_cell_length_c                   31.0731(11)
_cell_measurement_reflns_used    9481
_cell_measurement_temperature    80.00
_cell_measurement_theta_max      55.453
_cell_measurement_theta_min      3.205
_cell_volume                     14480.9(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      80.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            378242
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        53.000
_diffrn_reflns_theta_max         53.000
_diffrn_reflns_theta_min         1.715
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.237
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.6026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1253 before and 0.0723 after correction. The Ratio of minimum to maximum transmission is 0.8018. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.762
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3324
_exptl_crystal_size_max          0.046
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.034
_refine_diff_density_max         1.557
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.000267(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1424
_refine_ls_number_reflns         50783
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.1199
_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^)+(0.0052P)^2^+142.8700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2443
_refine_ls_wR_factor_ref         0.2534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                34268
_reflns_number_total             50783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6ce00077k2.cif
_cod_data_source_block           b24112202ahjhttzn80k_0m
_cod_depositor_comments          'Adding full bibliography for 7251777.cif.'
_cod_database_code               7251777
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.904
_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. Uiso/Uaniso restraints and constraints
N3 \\sim C111 \\sim C112 \\sim N4 \\sim Zn10 \\sim N2 \\sim C109 \\sim C110
\\sim N1: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N3) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(N4)
\\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(N6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Riding coordinates:
 C92(H92), C107(H107)
3.b Secondary CH2 refined with riding coordinates:
 C109(H10A,H10B), C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F), C113(H11G,
 H11H), C114(H11I,H11J), N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B),
 N5(H5A,H5B), N6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C11(H11), C14(H14), C17(H17), C20(H20), C23(H23),
 C26(H26), C29(H29), C32(H32), C35(H35), C38(H38), C41(H41), C44(H44), C47(H47),
  C50(H50), C53(H53), C56(H56), C59(H59), C62(H62), C65(H65), C68(H68),
 C71(H71), C74(H74), C77(H77), C80(H80), C83(H83), C86(H86), C89(H89), C95(H95),
  C104(H104), C101(H101), C98(H98)
3.d Fitted hexagon refined as free rotating group:
 C38(C39,C40,C41,C42,C37), C48(C43,C44,C45,C46,C47), C54(C49,C50,C51,C52,C53),
 C91(C96,C95,C94,C93,C92), C108(C107,C106,C105,C104,C103), C101(C100,C99,C98,
 C97,C102)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              43237
_shelx_fab_checksum              49139
_olex2_submission_special_instructions 'No special instructions were received'