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_7063372
_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         'C21 H25 N7 O6 U'
_chemical_formula_sum            'C21 H25 N7 O6 U'
_chemical_formula_weight         709.51
_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             2024-03-14
_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                109.3150(10)
_cell_angle_beta                 93.6850(10)
_cell_angle_gamma                94.3070(10)
_cell_formula_units_Z            2
_cell_length_a                   10.39940(10)
_cell_length_b                   10.40700(10)
_cell_length_c                   11.93030(10)
_cell_measurement_reflns_used    39440
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.5560
_cell_measurement_theta_min      3.9400
_cell_volume                     1209.60(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.91a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.90a 64-bit (release 14-04-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.91a (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_temperature      293(2)
_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 0.958
_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     25.00 120.00   0.50    0.10    --   47.19  77.00 120.00  190
  2  \w     35.00 131.00   0.50    0.10    --   58.00  77.00 113.59  192
  3  \w     35.00 131.00   0.50    0.10    --   58.00  77.00  27.07  192
  4  \w     28.00 122.00   0.50    0.10    --   50.00  76.00 -88.89  188
  5  \w     36.00 131.00   0.50    0.10    --   58.00  76.00-140.33  190
  6  \w     35.00 121.00   0.50    0.10    --   47.19  28.00-161.00  172
  7  \w     44.00  75.00   0.50    0.10    --   66.00  77.00 -37.87   62
  8  \w     48.00  73.00   0.50    0.10    --   70.00  76.00  50.76   50
  9  \w     32.00 126.00   0.50    0.10    --   54.00  76.00 152.05  188
 10  \w    113.00 138.00   0.50    0.10    --   66.00  76.00 141.92   50
 11  \w     36.00 131.00   0.50    0.10    --   58.00  76.00 169.12  190
 12  \w     44.00  70.00   0.50    0.10    --   66.00  76.00 141.92   52
 13  \w     32.00 126.00   0.50    0.10    --   54.00  75.00  68.16  188
 14  \w     58.00  92.00   0.50    0.20    --   78.00  71.00 -24.27   68
 15  \w     32.00 126.00   0.50    0.10    --   54.00  75.00-147.50  188
 16  \w     93.00 178.00   0.50    0.20    --  106.24  28.00-161.00  170
 17  \w     37.00 131.00   0.50    0.10    --   58.00  73.00 -74.29  188
 18  \w     41.00 135.00   0.50    0.10    --   62.00  72.00 -54.43  188
 19  \w     17.00  43.00   0.50    0.10    --   46.00  90.00   1.26   52
 20  \w     12.00  41.00   0.50    0.10    --   42.00  92.00  57.66   58
 21  \w    -20.00  14.00   0.50    0.10    --   14.00 102.00  28.60   68
 22  \w    -15.00  18.00   0.50    0.10    --   18.00 101.00 158.55   66
 23  \w     12.00  41.00   0.50    0.10    --   42.00  92.00 177.57   58
 24  \w    -42.00 -14.00   0.50    0.10    --    6.00 127.00  68.94   56
 25  \w      5.00  42.00   0.50    0.10    --   34.00  91.00 -17.75   74
 26  \w    -70.00  26.00   0.50    0.10    --  -47.19  77.00 -60.00  192
 27  \w    -71.00 -42.00   0.50    0.20    -- -106.00  61.00 -60.00   58
 28  \w    -35.00  27.00   0.50    0.10    --  -47.19  28.00-161.00  124
 29  \w    -67.00 -36.00   0.50    0.20    -- -106.00  61.00  30.00   62
 30  \w    -97.00 -34.00   0.50    0.20    -- -106.00  77.00 150.00  126
 31  \w   -126.00 -58.00   0.50    0.20    -- -106.00 144.00  93.51  136
 32  \w    -98.00 -57.00   0.50    0.20    -- -106.00 126.00  30.00   82
 33  \w   -120.00 -34.00   0.50    0.10    --  -47.19 -38.00 -30.00  172
 34  \w   -121.00 -34.00   0.50    0.10    --  -47.19 -28.00  36.00  174
 35  \w    -27.00  35.00   0.50    0.10    --   47.19 -28.00  36.00  124
 36  \w     41.00  78.00   0.50    0.20    --  106.24 -77.00 150.00   74
 37  \w     34.00  71.00   0.50    0.20    --  106.24 -61.00  60.00   74
 38  \w     76.00 101.00   0.50    0.20    --  106.24 -77.00-120.00   50
 39  \w     34.00  68.00   0.50    0.20    --  106.24 -77.00-120.00   68
 40  \w     38.00  71.00   0.50    0.20    --  106.24 -61.00 -90.00   66
 41  \w     67.00 105.00   0.50    0.20    --  106.24 -95.00   0.00   76
 42  \w     87.00 112.00   0.50    0.20    --  106.24-126.00  30.00   50
 43  \w     38.00  77.00   0.50    0.20    --  106.24-126.00  30.00   78
 44  \w     62.00 113.00   0.50    0.20    --  106.24-126.00   0.00  102
 45  \w     67.00 103.00   0.50    0.20    --  106.24 -95.00  30.00   72
 46  \w     36.00 107.00   0.50    0.20    --  106.24-126.00 -90.00  142
 47  \w     44.00 113.00   0.50    0.20    --  106.24-126.00-120.00  138
 48  \w     13.00  94.00   0.50    0.10    --   47.19-126.00 -90.00  162
 49  \w   -109.00 -75.00   0.50    0.20    --  -98.00 -77.00 -94.00   68
 50  \w   -129.00 -73.00   0.50    0.20    --  -94.00 -75.00-179.01  112
 51  \w   -169.00-127.00   0.50    0.20    --  -98.00 -77.00 -94.00   84
 52  \w   -168.00-135.00   0.50    0.20    --  -98.00 -76.00 -14.12   66
 53  \w   -126.00 -76.00   0.50    0.20    --  -98.00 -76.00 -14.12  100
 54  \w    -93.00 -67.00   0.50    0.20    --  -90.00 -76.00  38.70   52
 55  \w   -167.00 -72.00   0.50    0.20    --  -94.00 -74.00  -8.75  190
 56  \w   -135.00 -40.00   0.50    0.10    --  -62.00 -75.00 -58.53  190
 57  \w    -80.00 -52.00   0.50    0.10    --  -74.00 -74.00 -39.17   56
 58  \w    -96.00 -70.00   0.50    0.20    --  -90.00 -74.00 -58.39   52
 59  \w   -157.00-106.00   0.50    0.20    --  -90.00 -74.00 -58.39  102
 60  \w   -159.00-133.00   0.50    0.20    --  -94.00 -75.00-179.01   52
 61  \w   -160.00 -68.00   0.50    0.20    --  -90.00 -74.00-158.37  184
 62  \w    -86.00 -60.00   0.50    0.20    --  -82.00 -74.00-151.13   52
 63  \w    -80.00 -52.00   0.50    0.10    --  -74.00 -74.00-107.75   56
 64  \w    -83.00 -57.00   0.50    0.20    --  -78.00 -73.00  -5.21   52
 65  \w    -93.00 -67.00   0.50    0.20    --  -86.00 -72.00  38.09   52
 66  \w   -139.00 -45.00   0.50    0.10    --  -66.00 -72.00  56.53  188
 67  \w   -160.00-129.00   0.50    0.20    --  -90.00 -72.00 123.52   62
 68  \w   -103.00 -57.00   0.50    0.20    --  -78.00 -72.00 137.81   92
 69  \w    -87.00 -58.00   0.50    0.20    --  -78.00 -73.00 165.02   58
 70  \w    -98.00 -67.00   0.50    0.20    --  -86.00 -72.00 146.58   62
 71  \w   -107.00 -69.00   0.50    0.20    --  -90.00 -72.00 123.52   76
 72  \w    -95.00 -63.00   0.50    0.20    --  -82.00 -71.00  93.64   64
 73  \w   -159.00-111.00   0.50    0.20    --  -86.00 -71.00  70.72   96
 74  \w   -170.00 -78.00   0.50    0.20    --  -98.00 -71.00-114.27  184
 75  \w    -86.00 -61.00   0.50    0.20    --  -78.00 -71.00 -80.54   50
 76  \w    -84.00 -58.00   0.50    0.20    --  -78.00 -71.00 -21.71   52
 77  \w    -96.00 -70.00   0.50    0.20    --  -90.00 -70.00  10.42   52
 78  \w    -74.00 -48.00   0.50    0.10    --  -66.00 -68.00  -8.98   52
 79  \w    -82.00 -47.00   0.50    0.10    --  -66.00 -69.00  78.72   70
 80  \w    -81.00 -55.00   0.50    0.10    --  -74.00 -68.00 165.76   52
 81  \w   -139.00 -46.00   0.50    0.10    --  -66.00 -69.00 122.44  186
 82  \w   -100.00 -66.00   0.50    0.20    --  -86.00 -71.00  70.72   68
 83  \w   -169.00 -82.00   0.50    0.20    -- -102.00 -70.00  28.19  174
 84  \w   -171.00 -88.00   0.50    0.20    -- -106.00 -66.00 -86.59  166
 85  \w    -80.00 -52.00   0.50    0.10    --  -70.00 -68.00-142.07   56
 86  \w    -88.00 -57.00   0.50    0.10    --  -74.00 -65.00-157.14   62
 87  \w    -91.00 -65.00   0.50    0.20    --  -82.00 -65.00-127.87   52
 88  \w    -98.00 -72.00   0.50    0.20    --  -90.00 -64.00 -88.59   52
 89  \w   -119.00 -77.00   0.50    0.20    --  -94.00 -63.00 -54.92   84
 90  \w   -155.00-129.00   0.50    0.20    --  -94.00 -63.00 -54.92   52
 91  \w    -99.00 -68.00   0.50    0.20    --  -86.00 -64.00  76.78   62
 92  \w   -167.00 -78.00   0.50    0.20    --  -94.00 -64.00  48.08  178
 93  \w   -177.00 -90.00   0.50    0.20    -- -106.00 -61.00 150.00  174
 94  \w   -159.00 -90.00   0.50    0.20    --  -98.00 -47.00 113.48  138
 95  \w   -151.00-125.00   0.50    0.20    --  -90.00 -53.00  74.70   52
 96  \w   -121.00 -76.00   0.50    0.20    --  -90.00 -53.00  74.70   90
 97  \w   -177.00 -92.00   0.50    0.20    -- -106.00 -28.00  36.00  170
;
_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      -0.1001098000
_diffrn_orient_matrix_UB_12      -0.1028495000
_diffrn_orient_matrix_UB_13      0.0232934000
_diffrn_orient_matrix_UB_21      0.0896873000
_diffrn_orient_matrix_UB_22      -0.1139801000
_diffrn_orient_matrix_UB_23      -0.0447662000
_diffrn_orient_matrix_UB_31      0.0648345000
_diffrn_orient_matrix_UB_32      0.0359986000
_diffrn_orient_matrix_UB_33      0.1278504000
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43635
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.805
_diffrn_reflns_theta_min         3.944
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.335
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.099
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.91a (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_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0161
_refine_ls_R_factor_gt           0.0161
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0134P)^2^+2.0155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0401
_refine_ls_wR_factor_ref         0.0401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4872
_reflns_number_total             4883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02645d2.cif
_cod_data_source_block           u-cbbht
_cod_depositor_comments
'Adding full bibliography for 7063372--7063376.cif.'
_cod_database_code               7063372
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C21 H26 N7 O6 U'
_chemical_oxdiff_usercomment     245.1
_shelx_estimated_absorpt_t_max   0.512
_shelx_estimated_absorpt_t_min   0.095
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C00N(H00N), C8(H8), C16(H16), C9(H9), C10(H10), C14(H14),
 C15(H15)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C00U(H00A,H00B,H00C), C1(H1A,H1B,H1C), C00Y(H00D,H00E,H00F),
 C00Z(H00G,H00H,H00I)
2.c Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_shelx_res_checksum              14003
_shelx_hkl_checksum              39432
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.421
_oxdiff_exptl_absorpt_empirical_full_min 0.722