Visualizing Kinetically Robust Co<sup>III</sup><sub>4</sub>L<sub>6</sub> Assemblies in Vivo: SPECT Imaging of the Encapsulated [<sup>99m</sup>Tc]TcO<sub>4</sub><sup>-</sup> Anion.
Burke, Benjamin P.; Grantham, William; Burke, Michael J.; Nichol, Gary S.; Roberts, David; Renard, Isaline; Hargreaves, Rebecca; Cawthorne, Christopher; Archibald, Stephen J.; Lusby, Paul J.; Journal of the American Chemical Society 140 (2018) 16877–16881; doi:10.1021/jacs.8b09582

data_4133316
_publ_section_title
;
 Visualizing Kinetically Robust Co<sup>III</sup><sub>4</sub>L<sub>6</sub>
 Assemblies in Vivo: SPECT Imaging of the Encapsulated
 [<sup>99m</sup>Tc]TcO<sub>4</sub><sup>-</sup> Anion.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16877
_journal_page_last               16881
_journal_paper_doi               10.1021/jacs.8b09582
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C120 H84 Co4 N24, 12(Cl0.33 O1.33), 12(F6 P), 4(H4 N1), 4 C2 H3 N2'
_chemical_formula_sum            'C216 H244 Cl4 Co4 F72 N76 O16 P12'
_chemical_formula_weight         6278.02
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_Hall           'P -4n 2 3'
_space_group_name_H-M_alt        'P -4 3 n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.728
_cell_length_b                   21.728
_cell_length_c                   21.728
_cell_measurement_reflns_used    67367
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.9040
_cell_measurement_theta_min      3.5210
_cell_volume                     10257.919
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega -113.00  -21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -38.0000 -120.0000 92

  2 omega  -65.00   26.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   57.0000  150.0000 91

  3 omega  -93.00  -67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686 -146.0000  128.0000 26

  4 omega -113.00  -18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000    0.0000 95

  5 omega  -73.00  -14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  125.0000  120.0000 59

  6 omega   46.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000  -30.0000 47

  7 omega   56.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -120.0000 26

  8 omega   89.00  137.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000 -180.0000 48

  9 omega  109.00  135.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   60.0000 26

 10 omega   44.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000 -180.0000 26

 11 omega   86.00  122.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   48.0000  -37.8939 36

 12 omega   92.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   90.0000 82

 13 omega   44.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 26

 14 omega   80.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 26

 15 omega   38.00   73.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  120.0000 35

 16 omega   79.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  150.0000 37

 17 omega   89.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 32

 18 omega   40.00   72.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 32

 19 omega   83.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 30

 20 omega   88.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  120.0000 27

 21 omega   39.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 30

 22 omega   85.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 36

 23 omega  131.00  168.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   48.0000  -37.8939 37

 24 omega   92.00  141.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 49

 25 omega   40.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -90.0000 29

 26 omega   64.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 41

 27 omega   42.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  120.0000 55

 28 omega  107.00  135.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  120.0000 28

 29 omega   51.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   90.0000 30

 30 omega   96.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 25

 31 omega   91.00  136.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 45

 32 omega   95.00  130.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   90.0000 35

 33 omega  143.00  169.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   70.0000  -96.0346 26

 34 omega   87.00  159.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 72

 35 omega  140.00  165.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   90.0000 25

 36 omega   37.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 51

 37 omega   93.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   49.0000   -4.3165 85

 38 omega   51.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  120.0000 26

 39 omega  104.00  130.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   70.0000  -96.0346 26

 40 omega   48.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -30.0000 37

 41 omega   96.00  169.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  150.0000 73

 42 omega   72.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 25

 43 omega  142.00  168.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   60.0000 26

 44 omega   67.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  -30.0000 72

 45 omega   91.00  134.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -120.0000 43

 46 omega   64.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 51

 47 omega   40.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 65

 48 omega  143.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   30.0000 33

 49 omega   36.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 26

 50 omega   77.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 26

 51 omega   95.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000    0.0000 26

 52 omega  141.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000    0.0000 36

 53 omega   41.00   66.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 25

 54 omega   93.00  118.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 25

 55 omega   44.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -180.0000 26

 56 omega   62.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000    0.0000 25

 57 omega  113.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000 -150.0000 26

 58 omega  137.00  163.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000   90.0000 26

 59 omega  129.00  154.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   30.0000 25

 60 omega   97.00  149.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  120.0000 52

 61 omega  103.00  129.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -120.0000 26

 62 omega   54.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   90.0000 37

 63 omega  142.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   60.0000 36

 64 omega   51.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -53.0000    8.8022 52

 65 omega   75.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  150.0000 26

 66 omega   40.00   65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 25

 67 omega   82.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 39

 68 omega   96.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   60.0000 25

 69 omega   96.00  148.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -150.0000 52

 70 omega   85.00  146.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -89.0000 -106.1944 61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0232989000
_diffrn_orient_matrix_UB_12      -0.0212352000
_diffrn_orient_matrix_UB_13      0.0635406000
_diffrn_orient_matrix_UB_21      -0.0546590000
_diffrn_orient_matrix_UB_22      -0.0328420000
_diffrn_orient_matrix_UB_23      -0.0310063000
_diffrn_orient_matrix_UB_31      0.0386858000
_diffrn_orient_matrix_UB_32      -0.0591287000
_diffrn_orient_matrix_UB_33      -0.0054915000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            179104
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.323
_diffrn_reflns_theta_min         4.550
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.275
_exptl_absorpt_correction_T_max  0.4717
_exptl_absorpt_correction_T_min  0.3174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1055 before and 0.0880 after correction.
The Ratio of minimum to maximum transmission is 0.6729.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.033
_exptl_crystal_description       block
_exptl_crystal_F_000             6408
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of acetonitrile and diisopropyl ether by vapour diffusion'
_exptl_crystal_size_max          0.2923
_exptl_crystal_size_mid          0.1923
_exptl_crystal_size_min          0.1339
_platon_squeeze_details          'Four MeCN per asymmetric unit'
_refine_diff_density_max         1.995
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.331
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_coef       0.0074(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3595
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.986
_refine_ls_R_factor_all          0.1452
_refine_ls_R_factor_gt           0.1451
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3653
_refine_ls_wR_factor_ref         0.3656
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3584
_reflns_number_total             3595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09582_si_002.cif
_cod_data_source_block           pl16010_sq
_cod_original_cell_volume        10257.6
_cod_database_code               4133316
_chemical_oxdiff_formula         'C120 H84 Co4 F72 N24 P12'
_platon_squeeze_void_probe_radius 1.20
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(2) 0.50(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
3. Restrained distances
 N3-H3A = N3-H3B
 0.9 with sigma of 0.02
 H3A-H3B
 1.47 with sigma of 0.04
 Cl1-O1A \\sim Cl1-O1
 with sigma of 0.02
 Cl1-O1A \\sim Cl1-O1
 with sigma of 0.02
4. Restrained planarity
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
6. Rigid body (RIGU) restrains
 P1, F1, F2, F3, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, O2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O1A)=0.33333*(1-FVAR(2))
 Sof(O1)=0.33333*FVAR(2)
 Sof(O2A)=1-FVAR(2)
 Sof(O2)=FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9)
;
_shelx_res_checksum              53810
_shelx_hkl_checksum              75967
_shelx_fab_checksum              35374
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-24
_olex2_date_sample_submission    2016-03-18
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id MB4085
_olex2_submission_special_instructions 'No special instructions were received'