Substituent Effects in the Crystallization of Zr−Hydroxamate Metal−Organic Frameworks
Liu, Yuxin; Shao, Zhen-Wu; Duan, Xiangping; Xiong, Chaozhi; Li, Xiaoting; Liu, Chong; CrystEngComm  (2026) –; doi:10.1039/D6CE00114A

data_7251803
_publ_section_title
;
 Substituent effects in the crystallization of Zr-hydroxamate
 metal--organic frameworks
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2120
_journal_page_last               2124
_journal_paper_doi               10.1039/D6CE00114A
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         'C16 H8 F4 N4 O8 Zr, 2(Cl), 2(C2 H8 N)'
_chemical_formula_sum            'C20 H24 Cl2 F4 N6 O8 Zr'
_chemical_formula_weight         714.57
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-24
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2026-02-03 deposited with the CCDC.	2026-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   23.2456(12)
_cell_length_b                   23.2456(12)
_cell_length_c                   16.2338(11)
_cell_measurement_reflns_used    7250
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      74.81
_cell_measurement_theta_min      3.80
_cell_volume                     7596.8(8)
_computing_cell_refinement       'SAINT V8.41 (Bruker, 2024)'
_computing_data_collection       'APEX6 V2024.9-1 (Bruker, 2024)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1202
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46976
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.881
_diffrn_reflns_theta_min         3.803
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_type              'Incoatec I\ms DIAMOND'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.164
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1347 before and 0.0584 after correction.
The Ratio of minimum to maximum transmission is 0.7327.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.937
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.453
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5196
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0909P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4246
_reflns_number_total             5196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6ce00114a2.cif
_cod_data_source_block           SUM-1-F
_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 7251803--7251805.cif.
;
_cod_original_cell_volume        7596.8(9)
_cod_original_sg_symbol_H-M      P-3c1
_cod_database_code               7251803
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.764
_shelx_estimated_absorpt_t_min   0.684
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-C10 = N3-C9
 1.5 with sigma of 0.01
 C9-C10
 2.5 with sigma of 0.01
 N3A-C9A \\sim N3A-C10A \\sim N3-C10 \\sim N3-C9
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N3 \\sim C9 \\sim C10 \\sim N3A \\sim C9A \\sim C10A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(N3A)=Sof(H3AA)=Sof(H3AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(N3)=Sof(H3A)=Sof(H3B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N3A(H3AA,H3AB)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C3(H3), C6(H6)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              28512
_shelx_fab_checksum              41991
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU