Comparison of macrocyclic and acyclic chelators for gallium-68 radiolabelling
Tsionou, Maria Iris; Knapp, Caroline E.; Foley, Calum A.; Munteanu, Catherine R.; Cakebread, Andrew; Imberti, Cinzia; Eykyn, Thomas R.; Young, Jennifer D.; Paterson, Brett M.; Blower, Philip J.; Ma, Michelle T.; RSC Adv. 7 (2017) 49586–; doi:10.1039/C7RA09076E

data_7229405
_publ_section_title
;
 Comparison of macrocyclic and acyclic chelators for gallium-68
 radiolabelling
;
_journal_issue                   78
_journal_name_full               'RSC Adv.'
_journal_page_first              49586
_journal_paper_doi               10.1039/C7RA09076E
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C20 H23 Ga N2 O7, C2 H3 N'
_chemical_formula_sum            'C22 H26 Ga N3 O7'
_chemical_formula_weight         514.18
_chemical_name_systematic        Ga-HBED.H2O
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-25 deposited with the CCDC.
2017-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.7700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.96001(14)
_cell_length_b                   7.01939(10)
_cell_length_c                   25.0910(3)
_cell_measurement_reflns_used    18452
_cell_measurement_temperature    150.4(5)
_cell_measurement_theta_max      73.4290
_cell_measurement_theta_min      4.5580
_cell_volume                     2261.61(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.4(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_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    -45.00 -10.00   1.00    1.00    --  -42.62 -77.00 -30.00   35
  2  \w    -51.00 -10.00   1.00    1.00    --  -42.62 -77.00 -90.00   41
  3  \w    -55.00 -10.00   1.00    1.00    --  -42.62 -77.00  30.00   45
  4  \w    -51.00 -10.00   1.00    1.00    --  -42.62 -77.00 120.00   41
  5  \w    -68.00 -21.00   1.00    1.00    --  -42.62 -38.00  60.00   47
  6  \w    -79.00  37.00   1.00    1.00    --  -42.62  19.00  60.00  116
  7  \w      2.00  79.00   1.00    1.00    --   42.62 -99.00-120.00   77
  8  \w     25.00  95.00   1.00    2.00    --  106.36 -95.00 -60.00   70
  9  \w     41.00 121.00   1.00    2.00    --  106.36-125.00-180.00   80
 10  \w     29.00 103.00   1.00    2.00    --  106.36 -95.00-150.00   74
 11  \w     30.00 139.00   1.00    2.00    --  106.36 -77.00 -30.00  109
 12  \w     77.00 154.00   1.00    2.00    --  106.36  61.00  60.00   77
 13  \w    145.00 178.00   1.00    2.00    --  106.36  75.00  23.64   33
 14  \w    129.00 178.00   1.00    2.00    --  106.36  61.00  14.04   49
 15  \w    113.00 175.00   1.00    2.00    --  106.36  77.00 -60.00   62
 16  \w    129.00 178.00   1.00    2.00    --  106.36  77.00-120.00   49
 17  \w    119.00 178.00   1.00    2.00    --  106.36  66.00-172.32   59
 18  \w    109.00 178.00   1.00    2.00    --  106.36  61.00   0.00   69
 19  \w     74.00 105.00   1.00    2.00    --  106.36  77.00-150.00   31
 20  \w     78.00 150.00   1.00    2.00    --  106.36  61.00-120.00   72
 21  \w     77.00 109.00   1.00    2.00    --  106.36  61.00 -30.00   32
 22  \w     74.00 101.00   1.00    2.00    --  106.36  75.00  23.64   27
 23  \w     77.00 103.00   1.00    2.00    --  106.36  61.00  30.00   26
 24  \w     77.00 106.00   1.00    2.00    --  106.36  61.00   0.00   29
 25  \w     78.00 107.00   1.00    2.00    --  106.36  61.00  14.04   29
 26  \w     77.00 177.00   1.00    2.00    --  106.36  61.00  90.00  100
 27  \w     78.00 103.00   1.00    2.00    --  106.36  61.00 120.00   25
 28  \w     77.00 166.00   1.00    2.00    --  106.36  61.00 150.00   89
 29  \w     74.00 101.00   1.00    2.00    --  106.36  77.00 150.00   27
 30  \w     74.00 144.00   1.00    2.00    --  106.36  77.00 120.00   70
 31  \w     74.00 100.00   1.00    2.00    --  106.36  77.00  90.00   26
 32  \w     74.00 100.00   1.00    2.00    --  106.36  77.00  60.00   26
 33  \w     74.00 101.00   1.00    2.00    --  106.36  77.00  30.00   27
 34  \w     74.00 101.00   1.00    2.00    --  106.36  77.00 -30.00   27
 35  \w     77.00 103.00   1.00    2.00    --  106.36  61.00 -60.00   26
 36  \w     77.00 103.00   1.00    2.00    --  106.36  61.00 -90.00   26
 37  \w     75.00 100.00   1.00    2.00    --  106.36  77.00 -60.00   25
 38  \w     78.00 104.00   1.00    2.00    --  106.36  56.00 -44.84   26
 39  \w     74.00 149.00   1.00    2.00    --  106.36  77.00 -90.00   75
 40  \w     77.00 103.00   1.00    2.00    --  106.36  61.00-150.00   26
 41  \w     76.00 102.00   1.00    2.00    --  106.36  66.00-172.32   26
 42  \w     74.00 101.00   1.00    2.00    --  106.36  77.00-120.00   27
 43  \w     74.00 176.00   1.00    2.00    --  106.36  76.00 159.77  102
 44  \w     24.00  99.00   1.00    1.00    --   42.62-125.00 150.00   75
 45  \w    -70.00 -10.00   1.00    1.00    --  -42.62 -77.00-150.00   60
 46  \w    -79.00 -18.00   1.00    1.00    --  -42.62 -38.00-180.00   61
 47  \w   -119.00 -66.00   1.00    1.00    --  -42.62 -77.00  30.00   53
 48  \w   -116.00 -89.00   1.00    1.00    --  -42.62 -38.00  60.00   27
 49  \w   -119.00 -88.00   1.00    1.00    --  -42.62 -77.00 120.00   31
 50  \w   -118.00  -4.00   1.00    1.00    --  -42.62 -19.00-120.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1191988000
_diffrn_orient_matrix_UB_12      0.0177948000
_diffrn_orient_matrix_UB_13      0.0034818000
_diffrn_orient_matrix_UB_21      0.0114801000
_diffrn_orient_matrix_UB_22      -0.0507434000
_diffrn_orient_matrix_UB_23      0.0602700000
_diffrn_orient_matrix_UB_31      0.0073040000
_diffrn_orient_matrix_UB_32      -0.2126987000
_diffrn_orient_matrix_UB_33      -0.0140728000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            34357
_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         73.677
_diffrn_reflns_theta_min         3.442
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.510
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_preparation
'Gallium nitrate hydrate was mixed with HBED (bis(2-hydroxybenzyl)ethylenediaminediacetic acid) in aqueous ammonium acetate solution'
_exptl_crystal_recrystallization_method
'Crystallised from a solution of D2O and CD3CN'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+1.8748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4173
_reflns_number_total             4541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra09076e2.cif
_cod_data_source_block           xstr0762
_cod_original_cell_volume        2261.60(5)
_cod_database_code               7229405
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ga C20 H21 N2 O6'
_chemical_oxdiff_usercomment     'CEK MM'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Rotating group:
 O1(H1A)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C2(H2A,H2B), C5(H5A,H5B), C3(H3A,H3B), C14(H14A,H14B), C4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C10(H10), C19(H19), C17(H17), C20(H20), C11(H11), C18(H18), C12(H12)
2.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
2.e Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              98625
_olex2_date_sample_data_collection 2017-06-30
_olex2_exptl_crystal_mounting_method 'Mounted on a nylon loop'
_olex2_submission_original_sample_id xstr0762
_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 1.464
_oxdiff_exptl_absorpt_empirical_full_min 0.514