Isomerism and transformation of Zr-hydroxamate metal-organic frameworks.
Shao, Zhen-Wu; Qiu, Yuqing; Xiong, Chaozhi; Liu, Chong; Chemical communications (Cambridge, England) 61 (2025) 12960–12963; doi:10.1039/d5cc03911h

data_7134864
_publ_section_title
;
 Isomerism and transformation of Zr-hydroxamate metal-organic frameworks.
;
_journal_issue                   69
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12960
_journal_page_last               12963
_journal_paper_doi               10.1039/d5cc03911h
_journal_volume                  61
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 H12 N4 O8 Zr, 6.8[CH3OH]'
_chemical_formula_sum            'C22.8 H39.2 N4 O14.8 Zr'
_chemical_formula_weight         697.40
_chemical_name_systematic        SUM-16
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-24
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7311)
;
_audit_update_record
;
2025-07-24 deposited with the CCDC.	2025-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9734(12)
_cell_length_b                   8.9734(12)
_cell_length_c                   41.816(8)
_cell_measurement_reflns_used    4184
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      51.34
_cell_measurement_theta_min      6.29
_cell_volume                     3367.1(9)
_computing_cell_refinement       'SAINT V8.41 (Bruker, 2024)'
_computing_data_collection       'APEX6 V2024.9-1 (Bruker, 2025)'
_computing_data_reduction        'SAINT V8.41 (Bruker, 2024)'
_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      150.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE MetalJet PHOTON II'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            5210
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        51.341
_diffrn_reflns_theta_max         51.341
_diffrn_reflns_theta_min         6.294
_diffrn_source                   'Excillum MetalJet'
_diffrn_source_current           2.86
_diffrn_source_power             0.1997996
_diffrn_source_target            'Gallium (Ga) rich alloy'
_diffrn_source_type              'Liquid Metal Source'
_diffrn_source_voltage           69.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.174
_exptl_absorpt_correction_T_max  0.4528
_exptl_absorpt_correction_T_min  0.2769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1653 before and 0.0612 after correction.
The Ratio of minimum to maximum transmission is 0.6115.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       block
_exptl_crystal_F_000             1450
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1356
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0856P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    0.947
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                1246
_reflns_number_total             1356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03911h2.cif
_cod_data_source_block           SUM-16
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7134864--7134865.cif.
;
_cod_original_cell_volume        3367.1(11)
_cod_original_formula_sum        'C22.80 H39.20 N4 O14.80 Zr'
_cod_database_code               7134864
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.845
_shelx_estimated_absorpt_t_min   0.780
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(4)
 0.49(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Restrained distances
 C2-C1
 1.5 with sigma of 0.01
 C5-C1_$1
 1.5 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
5. Others
 Fixed Sof: C2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) C6(0.5) H6(0.5)
 C7(0.5) H7(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C6(H6), C7(H7)
6.b Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 461 electrons were 
found in a volume of 1960\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
6.8[CH3OH] per Asymmetric Unit 
which account for 490 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              33739
_shelx_hkl_checksum              49650
_shelx_fab_checksum              95517
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU