Spectroscopically labelled hydroxylamino-triazine (BHT) siderophores toward the quantification of iron(iii), vanadium(v) and uranium(vi) hard metal ions
Amoiridis, Angelos; Papanikolaou, Michael; Drouza, Chryssoula; Kabanos, Themistoklis A.; Keramidas, Anastasios D.; New Journal of Chemistry 48 (2024) 14884–14895; doi:10.1039/D4NJ02645D

data_7063376
_publ_section_title
;
 Spectroscopically labelled hydroxylamino-triazine (BHT) siderophores
 toward the quantification of iron(iii), vanadium(v) and uranium(vi) hard
 metal ions
;
_journal_issue                   34
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14884
_journal_page_last               14895
_journal_paper_doi               10.1039/D4NJ02645D
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety
'C17 H15 N6 O3 U0.5, C34 H29 N12 O6 U, C24 H19 P, C H4 O, C4 H10 O, 0.75(O)'
_chemical_formula_sum            'C80 H79.5 N18 O11.75 P U1.5'
_chemical_formula_weight         1869.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-07-19 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 136.637(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7499(9)
_cell_length_b                   34.5643(3)
_cell_length_c                   13.4753(5)
_cell_measurement_reflns_used    29913
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      77.0920
_cell_measurement_theta_min      3.3710
_cell_volume                     7915.1(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a 64-bit (release'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_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)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyP'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            56751
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.431
_diffrn_reflns_theta_min         2.898
_exptl_absorpt_coefficient_mu    9.390
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       plate
_exptl_crystal_F_000             3730
_exptl_crystal_size_max          0.087
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.998
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1075
_refine_ls_number_reflns         16196
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+10.0062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14214
_reflns_number_total             16196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02645d2.cif
_cod_data_source_block           2_u_agg
_cod_depositor_comments
'Adding full bibliography for 7063372--7063376.cif.'
_cod_original_cell_volume        7915.1(8)
_cod_original_formula_sum        'C80 H79.50 N18 O11.75 P U1.50'
_cod_database_code               7063376
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H16A of C16A, H14B of C14B, H7B of C7B, H16B of C16B,
  H10B of C10B, H9B of C9B, H7A of C7A, H22s of C22s, H5 of C5, H28s of C28s,
  H20s of C20s, H13 of C13, H17s of C17s, H8B' of C8B', H14 of C14, H16s of
  C16s, H23s of C23s, H16 of C16, H21s of C21s, H17 of C17, H18 of C18, H7B' of
  C7B', H9B' of C9B', H27s of C27s, H15s of C15s, H6 of C6, H25s of C25s, H11s
  of C11s, H19s of C19s, H13B of C13B, H8s of C8s, H8A of C8A, H14A of C14A, H3
  of C3, H13A of C13A, H4 of C4, H7s of C7s, H15B of C15B, H29s of C29s, H14s
  of C14s, H13s of C13s, H8B of C8B, H10A of C10A, H9s of C9s, H9A of C9A, H15A
  of C15A, H10s of C10s
 At 1.5 times of:
  All H(H) groups, H3B' of C25s, All C(H,H,H) groups
2. Restrained distances
 O3B'-H3B'
 0.87 with sigma of 0.01
 O3A-H3A
 0.877 with sigma of 0.02
 N1B'-H3B'
 1.892696 with sigma of 0.02
 U1B-H3B'
 3.214529 with sigma of 0.02
3. Others
 Sof(C10)=Sof(C13)=Sof(H13)=Sof(C7B')=Sof(H7B')=Sof(C9B')=Sof(H9B')=Sof(C8B')=
 Sof(H8B')=1-FVAR(1)
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=Sof(C18)=
 Sof(H18)=FVAR(1)
 Fixed Sof: O3s(0.25) O4s(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C4s(H4sa,H4sb), C3s(H3sa,H3sb)
4.b Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C9B(H9B), C10B(H10B), C16B(H16B), C16A(H16A), C14B(H14B), C7B(H7B),
 C8B(H8B), C8A(H8A), C15B(H15B), C10A(H10A), C13B(H13B), C9A(H9A), C13A(H13A),
 C15A(H15A), C10s(H10s), C9s(H9s), C11s(H11s), C8s(H8s), C7s(H7s), C14A(H14A),
 C3(H3), C29s(H29s), C19s(H19s), C4(H4), C14s(H14s), C13s(H13s), C5(H5),
 C21s(H21s), C15s(H15s), C6(H6), C16s(H16s), C28s(H28s), C17s(H17s), C20s(H20s),
  C27s(H27s), C23s(H23s), C22s(H22s), C13(H13), C7B'(H7B'), C9B'(H9B'),
 C8B'(H8B'), C14(H14), C16(H16), C17(H17), C18(H18), C25s(H25s)
4.c Fitted hexagon refined as free rotating group:
 C6s(C10s,C9s,C11s,C8s,C7s)
4.d Idealised Me refined as rotating group:
 C1B(H1Ba,H1Bb,H1Bc), C1B'(H1Bd,H1Be,H1Bf), C2B(H2Ba,H2Bb,H2Bc), C2B'(H2Bd,
 H2Be,H2Bf), C1A(H1Aa,H1Ab,H1Ac), C1s(H1sa,H1sb,H1sc), C2s(H2sa,H2sb,H2sc),
 C5s(H5sa,H5sb,H5sc)
;
_shelx_res_checksum              42243
_shelx_hkl_checksum              67614
_olex2_submission_special_instructions 'No special instructions were received'