Tuning N-donor coordination and assembly structures in uranyl compounds of carboxylate ligands with divergent vinyl pyridine groups
Song, Meng-ran; Wu, Qun-yan; Jin, Wei; Huang, Zhi-wei; Hu, Kong-qiu; Yuan, Li-yong; Wen, Wei; Shi, Wei-qun; Mei, Lei; CrystEngComm 27 (2025) 5603–5612; doi:10.1039/D5CE00556F

data_7250691
_publ_section_title
;
 Tuning N-donor coordination and assembly structures in uranyl compounds
 of carboxylate ligands with divergent vinyl pyridine groups
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              5603
_journal_page_last               5612
_journal_paper_doi               10.1039/D5CE00556F
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C46 H34 N2 O22 U4'
_chemical_formula_sum            'C46 H34 N2 O22 U4'
_chemical_formula_weight         1918.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-04-03
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-07-07 deposited with the CCDC.	2025-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                100.371(4)
_cell_angle_beta                 96.142(4)
_cell_angle_gamma                95.899(4)
_cell_formula_units_Z            2
_cell_length_a                   12.9936(13)
_cell_length_b                   14.0664(17)
_cell_length_c                   14.0763(16)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.534
_cell_measurement_theta_min      2.995
_cell_volume                     2496.5(5)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            84209
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_min         2.967
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.018
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0988 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.7491.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.258
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         11491
_refine_ls_number_restraints     483
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+6.1676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11137
_reflns_number_total             11491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00556f2.cif
_cod_data_source_block           6
_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 7250686--7250691.cif.
;
_cod_database_code               7250691
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.356
_shelx_estimated_absorpt_t_min   0.282
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.73094
 0.26906
2. Uiso/Uaniso restraints and constraints
C1 \\sim N1A \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8
\\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim N1A
\\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim C9A
\\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
3. Same fragment restrains
{C1, N1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A, C12A, C13A, C14A,
C15A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C1, N1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15}
4. Others
 Sof(N1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=
 Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=
 Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=
 Sof(H14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(N1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(H6)=
 Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(C11)=Sof(H11)=
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C18(H18), C19(H19), C21(H21), C22(H22), C26(H26), C27(H27), C29(H29),
  C30(H30), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40),
 C42(H42), C43(H43), C44(H44), C45(H45), C3A(H3A), C4A(H4A), C6A(H6A), C7A(H7A),
  C8A(H8A), C9A(H9A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A)
5.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C46(H46A,H46B,H46C), C15A(H15D,H15E,H15F)
;
_shelx_res_checksum              12030
_olex2_submission_special_instructions 'No special instructions were received'