Robust copper-based cationic metal-organic frameworks for efficient sequestration of perrhenate/pertechnetate.
Wang, Wenchang; Li, Lei; Zhang, Meiyu; Kang, Kang; Xiao, Chengliang; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13529–13539; doi:10.1039/d5dt01471a

data_1575402
_publ_section_title
;
 Robust copper-based cationic metal-organic frameworks for efficient
 sequestration of perrhenate/pertechnetate.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13529
_journal_page_last               13539
_journal_paper_doi               10.1039/d5dt01471a
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C50 H38 Cu N4 O2, 2[NO3], 6[H2O]'
_chemical_formula_sum            'C50 H50 Cu N6 O14'
_chemical_formula_weight         1022.50
_space_group_crystal_system      tetragonal
_space_group_IT_number           90
_space_group_name_Hall           'P 4ab 2ab'
_space_group_name_H-M_alt        'P 4 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2h09d7
_audit_creation_date             2025-08-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2025-08-04 deposited with the CCDC.	2025-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9504(18)
_cell_length_b                   12.9504(18)
_cell_length_c                   15.371(3)
_cell_measurement_reflns_used    3346
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.59
_cell_volume                     2577.9(7)
_computing_cell_refinement       'SAINT V8.41 (?, 2016)'
_computing_data_collection       'APEX6 V2024.9-1 (Bruker, 2025)'
_computing_data_reduction        'SAINT V8.41 (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS PHOTON II'
_diffrn_measurement_method       '\f and \w 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  0.0866
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13992
_diffrn_reflns_point_group_measured_fraction_full 0.997
_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         2.056
_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    0.493
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3234
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1205 before and 0.0920 after correction.
The Ratio of minimum to maximum transmission is 0.4340.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             1066
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.26(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         2383
_refine_ls_number_restraints     709
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.1050
_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^)+(0.1849P)^2^+2.5051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2736
_refine_ls_wR_factor_ref         0.2887
_reflns_Friedel_coverage         0.671
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1814
_reflns_number_total             2383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01471a2.cif
_cod_data_source_block           230323li_lidz207377_c2_0m
_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 1575402--1575403.cif.
;
_cod_original_cell_volume        2577.9(9)
_cod_database_code               1575402
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.74(9)
 0.26(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 C8-C7 = C9-C8 = C9-C10 = C11-C10 = C6-C11 = C7-C6 = C2-C1 = C3-C2 = C4-C3 =
 C5-C4 = N1-C5 = N1-C1
 1.39 with sigma of 0.01
 Cu1-O1B \\sim Cu1A-O1A
 with sigma of 0.02
4. Restrained planarity
 C3A, C6A, C7A, C8A, C9A, C10A, C11A
 with sigma of 0.1
 N1A, C1A, C2A, C3A, C4A, C5A, C6A
 with sigma of 0.1
 C3, C6, C7, C8, C9, C10, C11
 with sigma of 0.1
 N1, C1, C2, C3, C4, C5, C6
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Cu1 \\sim N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7
\\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim O1B \\sim Cu1A \\sim N1A \\sim C1A
\\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim C9A
\\sim C10A \\sim C11A: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
C12 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim C13: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
O1A \\sim O1B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(Cu1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O1B) \\sim Ueq, Uanis(Cu1A)
\\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2A) \\sim Ueq,
Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A)
\\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C9A) \\sim Ueq,
Uanis(C10A) \\sim Ueq, Uanis(C11A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O1A) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
6. Same fragment restrains
{Cu1A, N1A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A} sigma for
1-2: 0.01, 1-3: 0.02
as in
{Cu1, N1, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11}
7. Others
 Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=Sof(H4A)=
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=
 Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=1-FVAR(1)
 Sof(O1A)=Sof(H1Aa)=Sof(H1Ab)=0.5*(1-FVAR(2))
 Sof(Cu1A)=0.25*(1-FVAR(2))
 Sof(Cu1)=0.25*FVAR(2)
 Sof(O1B)=Sof(H1Ba)=Sof(H1Bb)=0.5*FVAR(2)
 Sof(N1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(H5)=Sof(C6)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(C10)=Sof(H10)=
 Sof(C11)=Sof(H11)=FVAR(1)
 Fixed Sof: C12(0.25) C17(0.25) C16(0.25) H16(0.25) C15(0.25) C14(0.25)
 C13(0.25) H13(0.25)
8.a Riding coordinates:
 O1B(H1Ba,H1Bb), O1A(H1Aa,H1Ab)
8.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C1A(H1A),
 C2A(H2A), C4A(H4A), C5A(H5A), C7A(H7A), C8A(H8A), C10A(H10A), C11A(H11A),
 C16(H16), C13(H13)
8.c Fitted hexagon refined as free rotating group:
 C12(C17,C16,C15,C14,C13)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 238 electrons were 
found in a volume of 688\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[NO3], 6[H2O] per Asymmetric Unit 
which account for 244 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94397
_shelx_hkl_checksum              52549
_shelx_fab_checksum              20759
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU