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_1573990
_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_formula_moiety         'C10 H17 N2 O4 Re S2'
_chemical_formula_sum            'C10 H17 N2 O4 Re S2'
_chemical_formula_weight         479.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-09-16 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4253(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.79663(15)
_cell_length_b                   10.5671(2)
_cell_length_c                   18.0745(3)
_cell_measurement_reflns_used    10710
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.9480
_cell_measurement_theta_min      2.5190
_cell_volume                     1459.61(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     91.00 178.00   0.50    0.07    --  113.25  77.00   0.00  174
  2  \w     93.00 178.00   0.50    0.07    --  113.25  71.00 106.00  170
  3  \w    -68.00  24.00   0.50    0.05    --  -48.28  71.00 106.00  184
  4  \w    -96.00 -19.00   0.50    0.07    --  -91.75  71.00 106.00  154
  5  \w    -74.00 -19.00   0.50    0.07    --  -91.75  61.00 -60.00  110
  6  \w     28.00 120.00   0.50    0.05    --   48.28  71.00 106.00  184
  7  \w    101.00 178.00   0.50    0.07    --  113.25  30.00  60.00  154
  8  \w    100.00 178.00   0.50    0.07    --  113.25  15.00-180.00  156
  9  \w     42.00 105.00   0.50    0.07    --  113.25 -95.00-180.00  126
 10  \w     42.00 106.00   0.50    0.07    --  113.25 -95.00-150.00  128
 11  \w     42.00 106.00   0.50    0.07    --  113.25 -95.00 -90.00  128
 12  \w     42.00 111.00   0.50    0.07    --  113.25-125.00   0.00  138
 13  \w     42.00 106.00   0.50    0.07    --  113.25 -95.00  30.00  128
 14  \w     42.00 136.00   0.50    0.07    --  113.25 -77.00  30.00  188
 15  \w     42.00  74.00   0.50    0.07    --  113.25 -61.00 120.00   64
 16  \w     42.00  74.00   0.50    0.07    --  113.25 -61.00  30.00   64
 17  \w     42.00  74.00   0.50    0.07    --  113.25 -61.00  60.00   64
 18  \w     42.00  96.00   0.50    0.07    --  113.25 -71.00 -24.00  108
 19  \w    -23.00  69.00   0.50    0.05    --   48.28 -71.00 -24.00  184
 20  \w     42.00  74.00   0.50    0.07    --  113.25 -61.00  90.00   64
 21  \w     42.00  74.00   0.50    0.07    --  113.25 -61.00 -90.00   64
 22  \w     42.00  74.00   0.50    0.07    --  113.25 -61.00-180.00   64
 23  \w   -120.00 -28.00   0.50    0.05    --  -48.28 -71.00 -24.00  184
 24  \w   -163.00 -71.00   0.50    0.07    --  -91.75 -71.00 -24.00  184
 25  \w   -120.00 -73.00   0.50    0.05    --  -48.28-125.00 120.00   94
;
_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      -0.0677223000
_diffrn_orient_matrix_UB_12      -0.0876129000
_diffrn_orient_matrix_UB_13      0.0561225000
_diffrn_orient_matrix_UB_21      0.1723756000
_diffrn_orient_matrix_UB_22      -0.0752718000
_diffrn_orient_matrix_UB_23      0.0119717000
_diffrn_orient_matrix_UB_31      0.0796406000
_diffrn_orient_matrix_UB_32      0.0888370000
_diffrn_orient_matrix_UB_33      0.0653781000
_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  0.0284
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14212
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.229
_diffrn_reflns_theta_min         4.873
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.077
_exptl_absorpt_correction_T_max  0.408
_exptl_absorpt_correction_T_min  0.211
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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            violet
_exptl_crystal_density_diffrn    2.182
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.847
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.00023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL (Sheldrick, 2015b)'
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2676
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+6.9084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2638
_reflns_number_total             2676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07743a2.cif
_cod_data_source_block           Re-1
_cod_depositor_comments
'Adding full bibliography for 1573990--1573991.cif.'
_cod_original_cell_volume        1459.62(5)
_cod_database_code               1573990
_shelx_estimated_absorpt_t_max   0.349
_shelx_estimated_absorpt_t_min   0.228
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C10A-C9A = C9B-C10B
 1.5 with sigma of 0.01
 O4-C9B \\sim O4-C9A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O4 \\sim C9A \\sim C10A \\sim C9B \\sim C10B: within 3A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 3A
4. Others
 Sof(C9B)=Sof(H9C)=Sof(H9D)=Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C9A)=Sof(H9A)=Sof(H9B)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
5.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),
 C9A(H9A,H9B), C9B(H9C,H9D)
5.b Idealised Me refined as rotating group:
 C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F)
;
_shelx_res_checksum              63350