Hexadentate Technetium-99m Bis(thiosemicarbazonato) Complexes: Synthesis, Characterisation and Biodistribution
Kelderman, Cormac; Davey, Patrick; Ma, Michelle; de Veer, Michael; Salimova, Ekaterina; Donnelly, Paul Stephen; Paterson, Brett Michael; Dalton Transactions  (2022) –; doi:10.1039/D2DT01264B

data_7710691
_publ_section_title
;
 Hexadentate Technetium-99m Bis(thiosemicarbazonato) Complexes: Synthesis,
 Characterisation and Biodistribution
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01264B
_journal_year                    2022
_chemical_formula_moiety         '2(Cl), C13 H28 N2 O2'
_chemical_formula_sum            'C13 H28 Cl2 N2 O2'
_chemical_formula_weight         315.27
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-09 deposited with the CCDC.	2022-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.9584(3)
_cell_length_b                   20.1197(4)
_cell_length_c                   23.6121(4)
_cell_measurement_reflns_used    7828
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      76.3660
_cell_measurement_theta_min      4.2690
_cell_volume                     6631.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      122.99(10)
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_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    -61.00  25.00   0.50    0.10    --  -47.64  38.00 150.00  172
  2  \w   -120.00 -76.00   0.50    0.10    --  -47.64-125.00 -30.00   88
  3  \w   -123.00 -34.00   0.50    0.10    --  -47.64 -20.00 -75.00  178
  4  \w     32.00  78.00   0.50    0.31    --  107.75 -20.00 -75.00   92
  5  \w     38.00  66.00   0.50    0.31    --  107.75 -30.00   0.00   56
  6  \w     35.00  61.00   0.50    0.31    --  107.75 -30.00  30.00   52
  7  \w     33.00  65.00   0.50    0.31    --  107.75 -30.00  90.00   64
  8  \w     36.00  64.00   0.50    0.31    --  107.75 -30.00 150.00   56
  9  \w     35.00 108.00   0.50    0.31    --  107.75-110.00 101.00  146
 10  \w     34.00  65.00   0.50    0.31    --  107.75 -30.00 -30.00   62
 11  \w     37.00  63.00   0.50    0.31    --  107.75 -30.00 -90.00   52
 12  \w     36.00  74.00   0.50    0.31    --  107.75 -45.00 -30.00   76
 13  \w     41.00  94.00   0.50    0.31    --  107.75-125.00-120.00  106
 14  \w     52.00 106.00   0.50    0.31    --  107.75 -94.00-180.00  108
 15  \w     33.00  59.00   0.50    0.31    --  107.75 -30.00-180.00   52
 16  \w    101.00 178.00   0.50    0.31    --  107.75 116.00 -74.00  154
 17  \w   -159.00 -82.00   0.50    0.31    --  -86.25-110.00 101.00  154
;
_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      -0.0925300000
_diffrn_orient_matrix_UB_12      0.0367326000
_diffrn_orient_matrix_UB_13      0.0168958000
_diffrn_orient_matrix_UB_21      0.0555694000
_diffrn_orient_matrix_UB_22      0.0660758000
_diffrn_orient_matrix_UB_23      0.0022350000
_diffrn_orient_matrix_UB_31      -0.0228015000
_diffrn_orient_matrix_UB_32      0.0122026000
_diffrn_orient_matrix_UB_33      -0.0630048000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9251
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.729
_diffrn_reflns_theta_min         4.286
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.528
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2720
_exptl_crystal_recrystallization_method
'Crystals formed during a recrsytalisation in methanol and diethyl ether.'
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0495P)^2^+8.3970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1688
_reflns_number_total             1735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01264b2.cif
_cod_data_source_block           ck-c051_meohet2o
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7710691
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.566
_shelx_estimated_absorpt_t_min   0.447
_reflns_odcompleteness_completeness 99.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Others
 Fixed Sof: H1C(0.5) H1D(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1C,H1D), C2(H2A,H2B)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              76002
_shelx_hkl_checksum              10599
_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 1.802
_oxdiff_exptl_absorpt_empirical_full_min 0.505