A hexatopic-carboxylate-based <b>csq</b> type luminescent zirconium-organic framework for the detection of glutathione.
Chu, Jin-Peng; Ma, Zhen-Sha; Xia, Jun; Zhou, Kang; Zhang, Zhi-Qiang; Liu, Xiao-Yuan; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13035–13039; doi:10.1039/d5dt01810b

data_1575345
_publ_section_title
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 A hexatopic-carboxylate-based <b>csq</b> type luminescent
 zirconium-organic framework for the detection of glutathione.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13035
_journal_page_last               13039
_journal_paper_doi               10.1039/d5dt01810b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C63 H42 N4 O20 S Zr3, 1[C5H11NO]'
_chemical_formula_sum            'C68 H53 N5 O21 S Zr3'
_chemical_formula_weight         1581.87
_chemical_name_systematic        HIAM-4062
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-07-24 deposited with the CCDC.	2025-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   40.0687(13)
_cell_length_b                   40.0687(13)
_cell_length_c                   20.3005(11)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    193.15
_cell_measurement_theta_max      56.045
_cell_measurement_theta_min      2.193
_cell_volume                     28226(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1272
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            167608
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.012
_diffrn_reflns_theta_min         6.594
_diffrn_source_current           2.86
_diffrn_source_power             0.1993134
_diffrn_source_voltage           69.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0912 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.8726.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.558
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         10566
_refine_ls_number_restraints     529
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1209P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6945
_reflns_number_total             10566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01810b2.cif
_cod_data_source_block           230831zh_zhcz250355_3_0m
_cod_depositor_comments          'Adding full bibliography for 1575345.cif.'
_cod_database_code               1575345
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.868
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C19-C27
 1.5 with sigma of 0.01
 N3-C18 = N4-C18
 1.35 with sigma of 0.01
 C18-C13 = C20-C19 = C28-C27 = C34-C31 = C24-C23
 1.5 with sigma of 0.01
 N3-C27 = N4-C19
 1.4 with sigma of 0.01
 O3-C24 = O4-C24 = O6-C34 = O5-C34
 1.25 with sigma of 0.01
 O6-O5 = O3-O4
 2.2 with sigma of 0.01
 C18-C27
 2.2 with sigma of 0.01
 C19-C18
 2.2 with sigma of 0.01
 N1-C16 \\sim N2-C17
 with sigma of 0.02
 S1-N1 \\sim S1-N2
 with sigma of 0.02
 C19-C21 \\sim C26-C19 \\sim C28-C19 \\sim N3-C28
 with sigma of 0.02
 C24-C25 \\sim C24-C22
 with sigma of 0.02
 O6-C31 \\sim O5-C31 \\sim O4-C23 \\sim O3-C23
 with sigma of 0.02
 C27-C29 \\sim C33-C27
 with sigma of 0.02
 C34-C32 \\sim C34-C30
 with sigma of 0.02
 S1-C17 \\sim S1-C16
 with sigma of 0.02
3. Restrained planarity
 C12, S1, C17, C13, C16, C15, C14, N1, N2
 with sigma of 0.1
 C23, C24, O4, O3
 with sigma of 0.1
 C31, O5, O6, C34
 with sigma of 0.1
 C18, N3, C27, C19, N4
 with sigma of 0.1
 C27, C28, C33, C32, C31, C30, C29, C34
 with sigma of 0.1
 C20, C26, C25, C23, C22, C21, C24, C19
 with sigma of 0.1
 C16, C17, S1, N2, N1
 with sigma of 0.1
 C33, C32, H32, C30, C29, C31, C34, C28
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.04 and sigma for 1-3 distances of 0.08
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
6. Others
 Fixed Sof: H9A(0.5) H9B(0.5) C12(0.25) C13(0.25) C14(0.25) H14(0.25)
 C15(0.25) C16(0.25) C17(0.25) S1(0.25) N2(0.25) N1(0.25) C18(0.25) N3(0.25)
 C27(0.25) C19(0.25) N4(0.25) H4A(0.25) C28(0.25) C33(0.25) H33(0.25) C32(0.25)
 H32(0.25) C31(0.25) C30(0.25) H30(0.25) C29(0.25) H29(0.25) C20(0.25)
 C26(0.25) H26(0.25) C25(0.25) H25(0.25) C23(0.25) C22(0.25) H22(0.25)
 C21(0.25) H21(0.25) O5(0.25) H5(0.25) O6(0.25) C24(0.25) O4(0.25) H4B(0.25)
 O3(0.25) C34(0.25)
7.a Riding coordinates:
 O10(H10A,H10B), O9(H9A,H9B), C8(H8), C10(H10), O5(H5), O4(H4B)
7.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C4(H4), C3(H3), C14(H14), N4(H4A), C33(H33), C32(H32),
 C30(H30), C29(H29), C26(H26), C25(H25), C22(H22), C21(H21)
7.c Fitted hexagon refined as free rotating group:
 C12(C13,C14,C15,C16,C17), C28(C33,C32,C31,C30,C29), C20(C26,C25,C23,C22,C21)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 325 electrons were 
found in a volume of 17141\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C5H11NO] per Asymmetric Unit 
which account for 336 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'