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_7710690
_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         'C4 H11 N3 O S'
_chemical_formula_sum            'C4 H11 N3 O S'
_chemical_formula_weight         149.22
_chemical_properties_physical    Deliquescent
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 92.937(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9054(3)
_cell_length_b                   7.1107(2)
_cell_length_c                   10.2511(4)
_cell_measurement_reflns_used    3874
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      31.1700
_cell_measurement_theta_min      3.4700
_cell_volume                     721.08(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (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      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.832
_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     -4.00  41.00   0.50    0.20    --    8.03  38.00  60.00   90
  2  \w     50.00  79.00   0.50    0.20    --    8.03  38.00  60.00   58
  3  \w    -41.00  32.00   0.50    0.20    --    8.03 -91.00  -1.00  146
  4  \w    -18.00  39.00   0.50    0.20    --    8.03 -99.00-120.00  114
  5  \w    -21.00  13.00   0.50    0.20    --   -8.65 -99.00-150.00   68
  6  \w    -36.00  19.00   0.50    0.20    --   -8.65  91.00 111.00  110
  7  \w     10.00  36.00   0.50    0.20    --   -8.65  38.00-120.00   52
  8  \w    -23.00  21.00   0.50    0.20    --   -8.65 -99.00 120.00   88
  9  \w    -25.00   0.00   0.50    0.20    --   -8.65 -91.00  -1.00   50
;
_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      0.0078531000
_diffrn_orient_matrix_UB_12      -0.0527002000
_diffrn_orient_matrix_UB_13      -0.0578673000
_diffrn_orient_matrix_UB_21      -0.0375660000
_diffrn_orient_matrix_UB_22      -0.0748945000
_diffrn_orient_matrix_UB_23      0.0260447000
_diffrn_orient_matrix_UB_31      -0.0605711000
_diffrn_orient_matrix_UB_32      0.0395890000
_diffrn_orient_matrix_UB_33      -0.0277565000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.953
_diffrn_reflns_theta_min         3.489
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (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    1.374
_exptl_crystal_description       irregular
_exptl_crystal_F_000             320
_exptl_crystal_recrystallization_method
'Crystallised from residual ethyl acetate from work up of reaction mixture'
_exptl_crystal_size_max          0.575
_exptl_crystal_size_mid          0.477
_exptl_crystal_size_min          0.256
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.252
_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     99
_refine_ls_number_reflns         2079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.2243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1747
_reflns_number_total             2079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01264b2.cif
_cod_data_source_block           ck-b079
_cod_database_code               7710690
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_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.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C2(H2a,H2b)
2.b Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c)
;
_shelx_res_checksum              97975
_shelx_hkl_checksum              36138
_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 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.682