Synthesis and properties of metal trifluoride complexes with amide-functionalised tacn macrocycles and radiofluorination of [GaF<sub>3</sub>(L1)] by <sup>18</sup>F/<sup>19</sup>F isotopic exchange.
O'Callaghan, Charley; Greenacre, Victoria K.; King, Rhys P.; Grigg, Julian; Herniman, Julie M.; McRobbie, Graeme; Reid, Gillian; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14897–14909; doi:10.1039/d4dt02074j

data_7716868
_publ_section_title
;
 Synthesis and properties of metal trifluoride complexes with
 amide-functionalised tacn macrocycles and radiofluorination of
 [GaF<sub>3</sub>(L1)] by <sup>18</sup>F/<sup>19</sup>F isotopic exchange.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14897
_journal_page_last               14909
_journal_paper_doi               10.1039/d4dt02074j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C30 H36 F3 Ga N6 O3, 1.5(C H4 O), 0.5(H2 O)'
_chemical_formula_sum            'C31.5 H43 F3 Ga N6 O5'
_chemical_formula_weight         712.448
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-16 deposited with the CCDC.	2024-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.495(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0116(5)
_cell_length_b                   12.0324(3)
_cell_length_c                   17.3324(6)
_cell_measurement_reflns_used    11603
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7500
_cell_measurement_theta_min      3.6160
_cell_volume                     3202.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.9959
_diffrn_measured_fraction_theta_max 0.9950
_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    -47.00  41.00   0.50   16.00    --  -18.50  68.00 -48.00  176
  2  \w     -7.00  41.00   0.50   16.00    --   21.15  68.00 -48.00   96
  3  \w    -35.00  48.00   0.50   16.00    --   21.15 -68.00 178.00  166
  4  \w     32.00  59.00   0.50   16.00    --  -18.50  19.00 -60.00   54
  5  \w     23.00  63.00   0.50   16.00    --  -18.50  19.00-180.00   80
  6  \w    -56.00  -2.00   0.50   16.00    --  -18.50 -57.00-180.00  108
  7  \w    -64.00 -38.00   0.50   16.00    --   21.15 -19.00 -90.00   52
  8  \w      0.00  64.00   0.50   16.00    --   21.15 -99.00 120.00  128
  9  \w      9.00  64.00   0.50   16.00    --   21.15 -99.00  90.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ diffractometer with Arc)Sec VHF Varimax confocal mirrors, a UG2 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0343727000
_diffrn_orient_matrix_UB_12      -0.0192391000
_diffrn_orient_matrix_UB_13      -0.0093345000
_diffrn_orient_matrix_UB_21      0.0101161000
_diffrn_orient_matrix_UB_22      -0.0415846000
_diffrn_orient_matrix_UB_23      0.0318648000
_diffrn_orient_matrix_UB_31      -0.0291632000
_diffrn_orient_matrix_UB_32      -0.0371097000
_diffrn_orient_matrix_UB_33      -0.0308507000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, Arc)Sec VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.9959
_diffrn_reflns_Laue_measured_fraction_max 0.9950
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31373
_diffrn_reflns_point_group_measured_fraction_full 0.9959
_diffrn_reflns_point_group_measured_fraction_max 0.9950
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         3.62
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
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    1.478
_exptl_crystal_description       block
_exptl_crystal_F_000             1490.224
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.9148
_refine_diff_density_min         -1.1348
_refine_diff_density_rms         0.1106
_refine_ls_d_res_high            0.7400
_refine_ls_d_res_low             5.6338
_refine_ls_goodness_of_fit_ref   1.0622
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    102
_refine_ls_number_parameters     593
_refine_ls_number_reflns         8240
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.0559
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          -0.0031
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+2.8628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1468
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -22
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -11
_reflns_number_gt                5777
_reflns_number_total             8240
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02074j2.cif
_cod_data_source_block           2021_DPT_CBG_Ga(L)_vg1a
_cod_depositor_comments
'Adding full bibliography for 7716867--7716872.cif.'
_cod_database_code               7716868
_chemical_oxdiff_formula         C30H34F3GaN6O3
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 N7-H7
 0.9 with sigma of 0.02
 N6-H6
 1 with sigma of 0.02
 N4-H4
 1 with sigma of 0.02
 O5-C41 \\sim O5A-C7A
 with sigma of 0.02
 C37-C38 \\sim C39-C40 \\sim C43-C42
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5 \\sim C41 \\sim H \\sim Ha \\sim Hb \\sim Hc: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(C33) = Uanis(C36)
4. Rigid body (RIGU) restrains
 C31, C35, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6, C37, C38, C39, C40, C42, C43
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C16, N5, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O5A)=Sof(Hj)=Sof(C7A)=Sof(Hk)=Sof(Hl)=Sof(Hm)=1-FVAR(1)
 Sof(O5)=Sof(H)=Sof(C41)=Sof(Ha)=Sof(Hb)=Sof(Hc)=FVAR(1)
 Fixed Sof: O2(0.5) N5(0.5) H5(0.5) C17(0.5) C18(0.5) H18(0.5) C19(0.5)
 H19(0.5) C20(0.5) H20(0.5) C21(0.5) H21(0.5) C22(0.5) H22(0.5) C25(0.5)
 C26(0.5) H26(0.5) C27(0.5) H27(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5)
 C30(0.5) H30(0.5) O4(0.5) N7(0.5) C31(0.5) C32(0.5) H32(0.5) C33(0.5) H33(0.5)
 C34(0.5) H34(0.5) C35(0.5) H35(0.5) C36(0.5) H36(0.5) C37(0.5) C38(0.5)
 H38(0.5) C39(0.5) H39(0.5) C40(0.5) H40(0.5) C42(0.5) H42(0.5) C43(0.5)
 H43(0.5) H7(0.5) O5B(0.5) Hd(0.5) He(0.5) O6(0.5) Hf(0.5) C44(0.5) Hg(0.5)
 Hh(0.5) Hi(0.5)
6.a Free rotating group:
 O5B(Hd,He)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b),
 C7(H7a,H7b), C15(H15a,H15b), C23(H23a,H23b)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), N5(H5), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
 C40(H40), C42(H42), C43(H43)
6.d Idealised Me refined as rotating group:
 C41(Ha,Hb,Hc), C44(Hg,Hh,Hi), C7A(Hk,Hl,Hm)
6.e Idealised tetrahedral OH refined as rotating group:
 O5(H), O6(Hf), O5A(Hj)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   1722
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.636