Facile transmetallation of [SbIII(DOTA)]− renders it unsuitable for medical applications
Chen, Catherine; Sommer, Charlotte; Thisgaard, Helge; McKee, Vickie; McKenzie, Christine J.; RSC Advances 12 (2022) 5772–5781; doi:10.1039/D2RA00642A

data_7244431
_publ_section_title
;
 Facile transmetallation of [SbIII(DOTA)]&#x2212; renders it unsuitable
 for medical applications
;
_journal_issue                   10
_journal_name_full               'RSC Advances'
_journal_page_first              5772
_journal_page_last               5781
_journal_paper_doi               10.1039/D2RA00642A
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C16 H30 N4 O8, 2(Cl), C2 H6 O S, 4(H2 O)'
_chemical_formula_sum            'C18 H44 Cl2 N4 O13 S'
_chemical_formula_weight         627.53
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-11-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-14 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.5130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1185(2)
_cell_length_b                   21.3172(4)
_cell_length_c                   12.1038(2)
_cell_measurement_reflns_used    13228
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.5250
_cell_measurement_theta_min      16.1420
_cell_volume                     2868.67(9)
_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    'Mercury (Macrae at al., 2008)'
_computing_publication_material
'Olex2 (Dolomanov et al. 2009), PublCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015a)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2923
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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    -66.00  16.00   1.00    2.57    --    0.58 -38.00 -60.00   82
  2  \w    -66.00  16.00   1.00    2.57    --    0.58 -38.00  90.00   82
  3  \w    -22.00  68.00   1.00    2.57    --   -0.58  57.00 150.00   90
  4  \w     28.00 107.00   1.00   10.30    --  100.40 -94.00 -30.00   79
  5  \w     33.00  68.00   1.00   10.30    --  100.40 -61.00-120.00   35
  6  \w     24.00 176.00   1.00   10.30    --  100.40   0.00-150.00  152
  7  \w     88.00 169.00   1.00   10.30    --  100.40  30.00   0.00   81
  8  \w     88.00 169.00   1.00   10.30    --  100.40  30.00  60.00   81
  9  \w     78.00 168.00   1.00   10.30    --  100.40  61.00  30.00   90
 10  \w     82.00 167.00   1.00   10.30    --  100.40  45.00 -30.00   85
 11  \w     33.00  68.00   1.00   10.30    --  100.40 -61.00  30.00   35
 12  \w     33.00  68.00   1.00   10.30    --  100.40 -61.00 -30.00   35
 13  \w     33.00 112.00   1.00   10.30    --  100.40-125.00 -30.00   79
 14  \w     33.00 112.00   1.00   10.30    --  100.40-125.00-150.00   79
 15  \w     33.00 112.00   1.00   10.30    --  100.40-125.00-180.00   79
 16  \w     33.00 112.00   1.00   10.30    --  100.40-125.00 -90.00   79
 17  \w     33.00 112.00   1.00   10.30    --  100.40-125.00-120.00   79
 18  \w     33.00  68.00   1.00   10.30    --  100.40 -61.00  60.00   35
 19  \w     31.00 108.00   1.00   10.30    --  100.40-110.00  78.00   77
 20  \w     33.00 112.00   1.00   10.30    --  100.40-125.00 150.00   79
 21  \w    -72.00  15.00   1.00    2.57    --    0.58 -19.00-180.00   87
 22  \w    -67.00  15.00   1.00    2.57    --   -0.58 -38.00-120.00   82
 23  \w    -77.00 -15.00   1.00   10.30    --  -82.50  61.00  30.00   62
 24  \w    -73.00  15.00   1.00    2.57    --   -0.58 -19.00   0.00   88
 25  \w   -150.00 -60.00   1.00   10.30    --  -82.50 -61.00 -97.90   90
 26  \w   -150.00 -59.00   1.00   10.30    --  -82.50 -64.00 -39.75   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0929957000
_diffrn_orient_matrix_UB_12      0.0413894000
_diffrn_orient_matrix_UB_13      0.0591736000
_diffrn_orient_matrix_UB_21      -0.0420870000
_diffrn_orient_matrix_UB_22      -0.0572333000
_diffrn_orient_matrix_UB_23      0.0670848000
_diffrn_orient_matrix_UB_31      0.0936517000
_diffrn_orient_matrix_UB_32      0.0153265000
_diffrn_orient_matrix_UB_33      0.0905816000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9137
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.669
_diffrn_reflns_theta_min         4.148
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.310
_exptl_absorpt_correction_T_max  -0.010
_exptl_absorpt_correction_T_min  10000000.000
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
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            colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dilute HCl'
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         9137
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0900P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6924
_reflns_number_total             9137
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 1.5575\% 
around [0.10 -0.99 0.09] (reciprocal) or [0.34 -0.90 0.27] (direct)
;
_cod_data_source_file            d2ra00642a2.cif
_cod_data_source_block           H6DOTAtwin
_cod_database_code               7244431
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C18H40N4O5ClS
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.75035
 0.24965
2. Restrained distances
 O1-H1 = O4-H4 = O6-H6 = O8-H8 = O11-H11C = O11-H11D = O12-H12A = O12-H12B
 0.83 with sigma of 0.02
 O13-H13C = O13-H13D = O14-H14C = O14-H14D = O11'-H11E = O11'-H11F
 0.83 with sigma of 0.02
 H11C-H11D
 1.35 with sigma of 0.02
3. Others
 Fixed Sof: O11(0.9) H11C(0.9) H11D(0.9) Cl2(0.9) O11'(0.1) H11E(0.1)
 H11F(0.1) Cl2'(0.1)
4.a Riding coordinates:
 O11'(H11E,H11F)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B)
4.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C)
4.d Idealised tetrahedral OH refined as rotating group with stretchable bonds:
 O1(H1), O4(H4), O6(H6)
;
_shelx_res_checksum              95845
_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 1.271
_oxdiff_exptl_absorpt_empirical_full_min 0.772
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2