Cysteine-selective [<sup>188</sup>Re]Re(v) radiolabelling of a Nanobody® for targeted radionuclide therapy using a "chelate-then-click" approach.
Melis, Diana R.; Segers, Charlotte; Wellens, Jasmien; Van de Voorde, Michiel; Blacque, Olivier; Ooms, Maarten; Gasser, Gilles; Opsomer, Tomas; Chemical science 16 (2025) 6089–6098; doi:10.1039/d4sc07743a

data_1573991
_publ_section_title
;
 Cysteine-selective [<sup>188</sup>Re]Re(v) radiolabelling of a
 Nanobody&#xae; for targeted radionuclide therapy using a
 "chelate-then-click" approach.
;
_journal_issue                   14
_journal_name_full               'Chemical science'
_journal_page_first              6089
_journal_page_last               6098
_journal_paper_doi               10.1039/d4sc07743a
_journal_volume                  16
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 H13 N2 O4 Re S2'
_chemical_formula_sum            'C8 H13 N2 O4 Re S2'
_chemical_formula_weight         451.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-16
_audit_creation_method
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_audit_update_record
;
2024-09-16 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   27.8226(4)
_cell_length_b                   20.2490(3)
_cell_length_c                   8.86174(14)
_cell_measurement_reflns_used    2954
_cell_measurement_temperature    160.0(1)
_cell_measurement_theta_max      79.2750
_cell_measurement_theta_min      5.3950
_cell_volume                     4992.53(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 42.51a 64-bit (release 28-03-2022))'
_computing_data_reduction        'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.0(1)
_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 0.999
_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   -161.00 -76.00   0.50    0.10    --  -90.00 -60.00  79.00  170
  2  \w   -123.00 -37.00   0.50    0.05    --  -50.90 -60.00  79.00  172
  3  \w     41.00 132.00   0.50    0.10    --  111.50 -77.00-150.00  182
  4  \w     41.00  67.00   0.50    0.10    --  111.50 -61.00-180.00   52
  5  \w     41.00  74.00   0.50    0.10    --  111.50 -61.00  30.00   66
  6  \w     41.00  69.00   0.50    0.10    --  111.50 -61.00 -90.00   56
  7  \w     46.00  74.00   0.50    0.10    --  111.50 -61.00 -60.00   56
  8  \w     47.00  72.00   0.50    0.10    --  111.50 -61.00-120.00   50
  9  \w     41.00  72.00   0.50    0.10    --  111.50 -60.00  79.00   62
 10  \w    -20.00  65.00   0.50    0.05    --   50.90 -60.00  79.00  170
 11  \w     41.00  74.00   0.50    0.10    --  111.50 -61.00 150.00   66
 12  \w    153.00 178.00   0.50    0.10    --  111.50 125.00 -60.00   50
 13  \w     95.00 132.00   0.50    0.10    --  111.50 125.00 -60.00   74
 14  \w    -21.00  16.00   0.50    0.05    --   50.90 -19.00-150.00   74
 15  \w     41.00 105.00   0.50    0.10    --  111.50-125.00   0.00  128
 16  \w     42.00  78.00   0.50    0.10    --  111.50 -95.00 -90.00   72
 17  \w     43.00  69.00   0.50    0.10    --  111.50-125.00 -60.00   52
 18  \w     67.00 104.00   0.50    0.10    --  111.50 -95.00   0.00   74
 19  \w    107.00 178.00   0.50    0.10    --  111.50  15.00 150.00  142
 20  \w    125.00 174.00   0.50    0.10    --  111.50  30.00  90.00   98
 21  \w    104.00 178.00   0.50    0.10    --  111.50  30.00   0.00  148
 22  \w     98.00 178.00   0.50    0.10    --  111.50  60.00-141.00  160
 23  \w    104.00 178.00   0.50    0.10    --  111.50  30.00-180.00  148
 24  \w     37.00 123.00   0.50    0.05    --   50.90  60.00-141.00  172
 25  \w    -65.00  21.00   0.50    0.05    --  -50.90  60.00-141.00  172
 26  \w    -72.00 -18.00   0.50    0.10    --  -90.00  60.00-141.00  108
 27  \w    -16.00  23.00   0.50    0.05    --  -50.90  19.00-150.00   78
 28  \w    -49.00 -18.00   0.50    0.10    --  -90.00  45.00  30.00   62
 29  \w    -49.00 -18.00   0.50    0.10    --  -90.00  45.00  60.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0336032000
_diffrn_orient_matrix_UB_12      -0.0241029000
_diffrn_orient_matrix_UB_13      -0.1268635000
_diffrn_orient_matrix_UB_21      0.0202534000
_diffrn_orient_matrix_UB_22      -0.0704885000
_diffrn_orient_matrix_UB_23      0.0172024000
_diffrn_orient_matrix_UB_31      -0.0392104000
_diffrn_orient_matrix_UB_32      -0.0158028000
_diffrn_orient_matrix_UB_33      0.1177208000
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12564
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.238
_diffrn_reflns_theta_min         5.404
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.251
_exptl_absorpt_correction_T_max  0.410
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.136a (Rigaku Oxford Diffraction, 2024)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.403
_exptl_crystal_description       plate
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.035
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_coef       0.000176(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2223
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+15.4748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                2221
_reflns_number_total             2223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07743a2.cif
_cod_data_source_block           dm2204_new
_cod_depositor_comments
'Adding full bibliography for 1573990--1573991.cif.'
_cod_original_cell_volume        4992.52(13)
_cod_database_code               1573991
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C8 H13 N2 O4 Re S2'
_chemical_oxdiff_usercomment     'sample DM079'
_shelx_estimated_absorpt_t_max   0.305
_shelx_estimated_absorpt_t_min   0.095
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
2.b Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              65857
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.399
_oxdiff_exptl_absorpt_empirical_full_min 0.587