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_7134865
_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_formula_moiety
'C16 H12 N4 O8 Zr, 2(Cl), 2(C2 H8 N), 0.45[C3H7NO], 0.15[C3H7NO]'
_chemical_formula_sum            'C21.8 H32.2 Cl2 N6.6 O8.6 Zr'
_chemical_formula_weight         686.46
_chemical_name_systematic        SUM-17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   mixed
_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            16
_cell_length_a                   25.7241(18)
_cell_length_b                   38.687(3)
_cell_length_c                   17.6068(13)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.50
_cell_volume                     17522(2)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS 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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            65360
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.401
_diffrn_reflns_theta_min         2.112
_diffrn_source                   'Turbo X-Ray Source (TXS)'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_type              'Rotaing Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1026 before and 0.0737 after correction.
The Ratio of minimum to maximum transmission is 0.9035.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.041
_exptl_crystal_description       block
_exptl_crystal_F_000             5632
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8042
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0853
_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^)+(0.0407P)^2^+317.0657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5921
_reflns_number_total             8042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03911h2.cif
_cod_data_source_block           SUM-17
_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_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_original_formula_sum        'C21.80 H32.20 Cl2 N6.60 O8.60 Zr'
_cod_database_code               7134865
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.952
_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
 C3A-C2 = C4A-C3A = C4A-C8 = C5A-C8 = C5A-C6A = C6A-C2
 1.39 with sigma of 0.01
 C11A-C10 = C12A-C11A = C12A-C16 = C13A-C16 = C13A-C14A = C14A-C10
 1.39 with sigma of 0.01
 N5-C17 = N5-C18
 1.5 with sigma of 0.01
 C17-C18
 2.5 with sigma of 0.01
3. Restrained planarity
 C3A, C4A, C5A, C6A, C8, C2
 with sigma of 0.01
 C11A, C12A, C13A, C14A, C16, C10
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C3A \\sim C4A \\sim C5A \\sim C6A \\sim C8 \\sim C5 \\sim C6 \\sim C2 \\sim C3
\\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C11A \\sim C12A \\sim C13A \\sim C14A \\sim C16 \\sim C13 \\sim C14 \\sim C10
\\sim C11 \\sim C12: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
N5 \\sim C17 \\sim C18: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
N6 \\sim C19 \\sim C20: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
5. Others
 Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=
 Sof(H14A)=1-FVAR(1)
 Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=FVAR(1)
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=1-
 FVAR(2)
 Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C3)=Sof(H3b)=Sof(C4)=Sof(H4b)=FVAR(2)
6.a Riding coordinates:
 C18(H18a,H18b,H18c)
6.b Secondary CH2 refined with riding coordinates:
 N5(H5b,H5c), N6(H6b,H6c)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A),
 C5(H5), C6(H6), C3(H3b), C4(H4b), C11A(H11A), C12A(H12A), C13A(H13A),
 C14A(H14A), C13(H13), C14(H14), C11(H11), C12(H12)
6.d Fitted hexagon refined as free rotating group:
 C8(C5,C6,C2,C3,C4), C16(C13,C14,C10,C11,C12)
6.e Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 388 electrons were 
found in a volume of 7708\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.45[C3H7NO], 0.15[C3H7NO] per Asymmetric Unit 
which account for 384 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38051
_shelx_hkl_checksum              76810
_shelx_fab_checksum              67572
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU