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_7244433
_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 H24 Bi N4 O8, C16 H40 Bi N4 Na2 O16'
_chemical_formula_sum            'C32 H64 Bi2 N8 Na2 O24'
_chemical_formula_weight         1408.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-09-24
_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                 101.6200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.1003(2)
_cell_length_b                   6.55970(10)
_cell_length_c                   19.8702(3)
_cell_measurement_reflns_used    42051
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.3280
_cell_measurement_theta_min      3.2540
_cell_volume                     2183.22(5)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2923
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.945
_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    -65.00  23.00   1.00    2.58    --    2.84 -52.00 -72.65   88
  2  \w    -24.00  68.00   1.00    2.58    --   -3.94  20.00 -44.78   92
  3  \w    -28.00  64.00   1.00    2.58    --   -3.94  65.00 158.59   92
  4  \w    -25.00  69.00   1.00    2.58    --   -3.94  19.00 120.00   94
  5  \w    -25.00  69.00   1.00    2.58    --   -3.94  19.00   0.00   94
  6  \w    -20.00  62.00   1.00    2.58    --   -3.94  38.00 120.00   82
  7  \w    -25.00  69.00   1.00    2.58    --   -3.94  19.00  60.00   94
  8  \w    -25.00  69.00   1.00    2.58    --   -3.94  19.00-150.00   94
  9  \w    -22.00  63.00   1.00    2.58    --   -3.94  44.00-118.25   85
 10  \w    -24.00  38.00   1.00    2.58    --    2.84 -99.00  90.00   62
 11  \w    -65.00  23.00   1.00    2.58    --    2.84 -52.00  14.90   88
 12  \w    -25.00  69.00   1.00    2.58    --   -3.94  19.00-120.00   94
 13  \w    -20.00  13.00   1.00    2.58    --   -3.94  38.00 150.00   33
;
_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      0.0049879000
_diffrn_orient_matrix_UB_12      -0.0850445000
_diffrn_orient_matrix_UB_13      -0.0207875000
_diffrn_orient_matrix_UB_21      0.0419241000
_diffrn_orient_matrix_UB_22      0.0151789000
_diffrn_orient_matrix_UB_23      0.0076250000
_diffrn_orient_matrix_UB_31      0.0032693000
_diffrn_orient_matrix_UB_32      -0.0650339000
_diffrn_orient_matrix_UB_33      0.0289448000
_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  0.0354
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            93107
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.594
_diffrn_reflns_theta_min         2.624
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.169
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.264
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water/Ethanol'
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00032(3)
_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   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         6353
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0139
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0099P)^2^+1.5973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0272
_refine_ls_wR_factor_ref         0.0280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5865
_reflns_number_total             6353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra00642a2.cif
_cod_data_source_block           NaBidota
_cod_database_code               7244433
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Bi Na C16 H32 N4 O12'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O9-H9C = O9-H9D = O10-H10C = O10-H10D = O11-H11C = O11-H11D
 0.83 with sigma of 0.02
 O12-H12A = O12-H12B
 0.83 with sigma of 0.02
 H9C-H9D = H10C-H10D = H11C-H11D = H12A-H12B
 1.35 with sigma of 0.02
 Na1-H11D = Na1-H11C
 -3.1 with sigma of 0.04
3.a 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)
;
_shelx_res_checksum              96869
_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 1.197
_oxdiff_exptl_absorpt_empirical_full_min 0.856