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_7063375
_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
'C68 H56 N24 O14 U3, 2(C24 H20 P), 2(C2.998 H6.998 N O)'
_chemical_formula_sum            'C122 H110 N26 O16 P2 U3'
_chemical_formula_weight         2972.38
_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
_audit_creation_date             2024-04-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-06-05 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                99.7750(10)
_cell_angle_beta                 103.0330(10)
_cell_angle_gamma                106.2090(10)
_cell_formula_units_Z            1
_cell_length_a                   13.5096(2)
_cell_length_b                   13.6013(2)
_cell_length_c                   17.1971(2)
_cell_measurement_reflns_used    24811
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      76.3600
_cell_measurement_theta_min      2.7060
_cell_volume                     2863.23(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))'
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -66.00  27.00   0.50    0.38    --  -46.44  92.00 176.00  186
  2  \w    -23.00  71.00   0.50    0.38    --   46.44 -92.00  63.00  188
  3  \w    -79.00 -53.00   0.50    1.52    -- -106.00  92.00 176.00   52
  4  \w   -125.00 -80.00   0.50    1.52    -- -106.00 -92.00  63.00   90
  5  \w     36.00 101.00   0.50    1.52    --  107.98 -92.00  63.00  130
  6  \w     98.00 148.00   0.50    1.52    --  107.98  92.00 176.00  100
  7  \w    -74.00 -37.00   0.50    0.38    --  -46.44 -38.00  30.00   74
  8  \w   -105.00 -78.00   0.50    0.38    --  -46.44 -38.00  30.00   54
  9  \w     14.00  69.00   0.50    0.38    --   46.44-125.00  60.00  110
 10  \w     34.00 107.00   0.50    0.38    --   46.44  77.00-120.00  146
 11  \w     -8.00  30.00   0.50    0.38    --   46.44 -19.00-120.00   76
 12  \w    -23.00  60.00   0.50    0.38    --   46.44 -57.00 120.00  166
 13  \w    -29.00   4.00   0.50    0.38    --   46.44 -19.00-180.00   66
 14  \w    -71.00 -39.00   0.50    1.52    -- -106.00  61.00 120.00   64
 15  \w    -67.00 -34.00   0.50    1.52    -- -106.00  61.00   0.00   66
 16  \w   -132.00 -34.00   0.50    1.52    -- -106.00 154.00  67.67  196
 17  \w   -129.00 -50.00   0.50    1.52    -- -106.00 150.00 115.58  158
 18  \w   -170.00 -91.00   0.50    1.52    -- -106.00 -30.00  90.00  158
 19  \w    -71.00 -33.00   0.50    1.52    -- -106.00  61.00  30.00   76
 20  \w    -83.00 -57.00   0.50    1.52    -- -106.00 148.00-134.30   52
 21  \w   -175.00 -92.00   0.50    1.52    -- -106.00 -45.00   0.00  166
 22  \w   -103.00 -41.00   0.50    1.52    -- -106.00 125.00-180.00  124
 23  \w   -176.00 -91.00   0.50    1.52    -- -106.00 -61.00 150.00  170
 24  \w   -170.00-142.00   0.50    1.52    -- -106.00 -95.00-150.00   56
 25  \w   -125.00 -83.00   0.50    1.52    -- -106.00 -95.00-150.00   84
 26  \w   -128.00-103.00   0.50    1.52    -- -106.00 148.00-134.30   50
 27  \w   -107.00 -71.00   0.50    1.52    -- -106.00 108.00  41.73   72
 28  \w     39.00 105.00   0.50    1.52    --  107.98 -95.00 -60.00  132
 29  \w     59.00  84.00   0.50    1.52    --  107.98 -77.00 150.00   50
 30  \w    144.00 177.00   0.50    1.52    --  107.98  30.00-150.00   66
 31  \w     93.00 130.00   0.50    1.52    --  107.98  30.00-150.00   74
 32  \w     43.00 111.00   0.50    1.52    --  107.98-125.00 -60.00  136
 33  \w     42.00  70.00   0.50    1.52    --  107.98 -61.00-150.00   56
 34  \w     80.00 105.00   0.50    1.52    --  107.98 -95.00 -30.00   50
 35  \w     70.00  96.00   0.50    1.52    --  107.98 -77.00  60.00   52
 36  \w     40.00  66.00   0.50    1.52    --  107.98 -77.00  60.00   52
 37  \w     44.00  94.00   0.50    1.52    --  107.98 -95.00  30.00  100
 38  \w    108.00 156.00   0.50    1.52    --  107.98  45.00 -90.00   96
 39  \w     35.00  69.00   0.50    1.52    --  107.98 -61.00 -60.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0867872000
_diffrn_orient_matrix_UB_12      0.0029729000
_diffrn_orient_matrix_UB_13      0.0442371000
_diffrn_orient_matrix_UB_21      -0.0865479000
_diffrn_orient_matrix_UB_22      -0.0806563000
_diffrn_orient_matrix_UB_23      -0.0755472000
_diffrn_orient_matrix_UB_31      0.0189588000
_diffrn_orient_matrix_UB_32      -0.0911959000
_diffrn_orient_matrix_UB_33      0.0367214000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37937
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.255
_diffrn_reflns_theta_min         2.723
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.719
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.549
_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    1.724
_exptl_crystal_description       block
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.115
_refine_diff_density_min         -1.813
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         11683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0248P)^2^+9.2283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10645
_reflns_number_total             11683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02645d2.cif
_cod_data_source_block           4cbht3u
_cod_depositor_comments
'Adding full bibliography for 7063372--7063376.cif.'
_cod_database_code               7063375
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C122 H112 N26 O16 P2 U3'
_shelx_estimated_absorpt_t_max   0.569
_shelx_estimated_absorpt_t_min   0.429
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C1B(0.555) H1BA(0.555) H1BB(0.555) H1BC(0.555) C1A(0.445)
 H1AA(0.445) H1AB(0.445) H1AC(0.445) C19(0.40905) H1(0.409) O2B(0.5) O2A(0.5)
 C18(0.589) H4(0.589)
3.a Aromatic/amide H refined with riding coordinates:
 C16'(H16'), C00Y(H00Y), C14'(H14'), C013(H013), C10(H10), C015(H015),
 C13(H13), C01A(H01F), C7(H7), C15'(H15'), C01E(H01I), C01F(H01J), C8(H8),
 C16(H16), C01J(H01K), C01K(H01N), C14(H14), C13'(H13'), C01O(H01O), C01P(H01P),
  C9'(H9'), C7'(H7'), C01W(H01W), C01Y(H01Y), C01Z(H01Z), C9(H9), C10'(H10'),
 C8'(H8'), C15(H15), C024(H024), C025(H025), C026(H026), C027(H027), C028(H028),
  C029(H029), C02A(H02A), C19(H1), C18(H4)
3.b Idealised Me refined as rotating group:
 C00R(H00D,H00E,H00F), C4'(H4'A,H4'B,H4'C), C4(H4A,H4B,H4C), C1(H1A,H1B,H1C),
 C1'(H1'A,H1'B,H1'C), C1B(H1BA,H1BB,H1BC), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              69475
_shelx_hkl_checksum              91594
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.600
_oxdiff_exptl_absorpt_empirical_full_min 0.767