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_7244434
_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, 2(H2.5 O)'
_chemical_formula_sum            'C16 H29 Bi N4 O10'
_chemical_formula_weight         646.41
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_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
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.13250(10)
_cell_length_b                   12.13250(10)
_cell_length_c                   6.56530(10)
_cell_measurement_reflns_used    28818
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.3730
_cell_measurement_theta_min      3.5150
_cell_volume                     966.396(19)
_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 0.999
_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    -25.00  69.00   1.00    1.56    --   -3.94  19.00  90.00   94
  2  \w    -25.00  64.00   1.00    1.56    --   -3.94  57.00   0.00   89
  3  \w    -25.00  69.00   1.00    1.56    --   -3.94  19.00-150.00   94
  4  \w    -25.00  69.00   1.00    1.56    --   -3.94  19.00-180.00   94
  5  \w    -25.00  69.00   1.00    1.56    --   -3.94  19.00 -90.00   94
  6  \w    -25.00  69.00   1.00    1.56    --   -3.94  19.00  30.00   94
  7  \w    -25.00  64.00   1.00    1.56    --   -3.94  57.00-150.00   89
  8  \w    -25.00  69.00   1.00    1.56    --   -3.94  19.00 120.00   94
  9  \w    -36.00  71.00   1.00    1.56    --   -3.94  14.00 -24.04  107
 10  \w    -24.00   1.00   1.00    1.56    --    2.84 -99.00  90.00   25
 11  \w    -65.00  24.00   1.00    1.56    --    2.84 -57.00 120.00   89
 12  \w    -20.00  62.00   1.00    1.56    --   -3.94  38.00 -30.00   82
 13  \w    -24.00  32.00   1.00    1.56    --   -3.94 -99.00   0.00   56
;
_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      -0.0139422000
_diffrn_orient_matrix_UB_12      0.0546784000
_diffrn_orient_matrix_UB_13      -0.0280549000
_diffrn_orient_matrix_UB_21      -0.0414880000
_diffrn_orient_matrix_UB_22      -0.0204956000
_diffrn_orient_matrix_UB_23      -0.0660872000
_diffrn_orient_matrix_UB_31      -0.0387886000
_diffrn_orient_matrix_UB_32      0.0022331000
_diffrn_orient_matrix_UB_33      0.0807498000
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            41527
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.579
_diffrn_reflns_theta_min         3.103
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.190
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.366
_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    2.221
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_recrystallization_method
'Crystallised from aqueous reaction mixture'
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00091(19)
_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   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1468
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0116
_refine_ls_R_factor_gt           0.0109
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+0.4519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0233
_refine_ls_wR_factor_ref         0.0235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1444
_reflns_number_total             1468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra00642a2.cif
_cod_data_source_block           exp_851biph2
_cod_original_cell_volume        966.40(2)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7244434
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Bi C16 H24 N4 O8'
_shelx_estimated_absorpt_t_max   0.566
_shelx_estimated_absorpt_t_min   0.362
_reflns_odcompleteness_completeness 99.81
_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. Shared sites
{C3, C3'}
3. Restrained distances
 O5-H5A = O5-H5B
 0.83 with sigma of 0.02
 H5A-H5B
 1.35 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C3')
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C3', C4', O1', O2'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C3, C4, O1, O2}
7. Others
 Sof(C3')=Sof(H3'A)=Sof(H3'B)=Sof(C4')=Sof(O1')=Sof(O2')=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(O1)=Sof(O2)=FVAR(1)
 Fixed Sof: O5(0.5) H5B(0.75)
8.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C3'(H3'A,H3'B)
;
_shelx_res_checksum              29945
_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 1.256
_oxdiff_exptl_absorpt_empirical_full_min 0.845