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_7716871
_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 H37 N6 O3, N O3'
_chemical_formula_sum            'C30 H37 N7 O6'
_chemical_formula_weight         591.66
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-01-25
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2024-05-16 deposited with the CCDC.	2024-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.779(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.4918(5)
_cell_length_b                   14.3084(2)
_cell_length_c                   20.9037(5)
_cell_measurement_reflns_used    20712
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.5920
_cell_measurement_theta_min      1.7690
_cell_volume                     5836.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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    -62.00   6.00   0.50    4.38    --  -18.58 100.00 153.00  136
  2  \w      1.00  65.00   0.50    4.38    --   21.24-100.00  48.00  128
  3  \w     22.00  64.00   0.50    4.38    --  -18.58  19.00-120.00   84
  4  \w     22.00  64.00   0.50    4.38    --  -18.58  19.00-150.00   84
  5  \w     22.00  64.00   0.50    4.38    --  -18.58  19.00 -60.00   84
  6  \w     22.00  64.00   0.50    4.38    --  -18.58  19.00-180.00   84
  7  \w    -56.00   9.00   0.50    4.38    --  -18.58 -57.00  30.00  130
  8  \w     22.00  64.00   0.50    4.38    --  -18.58  19.00  30.00   84
  9  \w     22.00  64.00   0.50    4.38    --  -18.58  19.00 -30.00   84
 10  \w     22.00  64.00   0.50    4.38    --  -18.58  19.00  90.00   84
 11  \w      0.00  65.00   0.50    4.38    --   21.24 -99.00 -90.00  130
 12  \w    -56.00 -16.00   0.50    4.38    --  -18.58 -57.00-120.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            65442
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         1.765
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.347
_exptl_crystal_description       plate
_exptl_crystal_F_000             2512
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         15028
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0451P)^2^+2.8866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11228
_reflns_number_total             15028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02074j2.cif
_cod_data_source_block
2021_dpt_gr_cbg_ga(lb)_auto_reprocessed_beamstop
_cod_depositor_comments
'Adding full bibliography for 7716867--7716872.cif.'
_cod_original_cell_volume        5836.3(2)
_cod_database_code               7716871
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 O206-N202 \\sim O6-N7
 with sigma of 0.02
 N202-O205 \\sim N7-O4
 with sigma of 0.02
 N202-O204 \\sim N7-O5
 with sigma of 0.02
 O206-O205 \\sim O6-O4
 with sigma of 0.04
 O206-O204 \\sim O6-O5
 with sigma of 0.04
 O205-O204 \\sim O4-O5
 with sigma of 0.04
3. Others
 Sof(O4)=Sof(N7)=Sof(O5)=Sof(O6)=1-FVAR(1)
 Sof(O206)=Sof(N202)=Sof(O205)=Sof(O204)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C104(H10A,H10B), C3(H3A,H3B), C23(H23A,H23B), C5(H5A,H5B),
 C107(H10C,H10D), C123(H12A,H12B), C6(H6A,H6B), C7(H7A,H7B), C105(H10E,H10F),
 C2(H2A,H2B), C115(H11A,H11B), C106(H10G,H10H), C103(H10I,H10J), C15(H15A,H15B),
  C101(H10K,H10L), C1(H1A,H1B), C102(H10M,H10N)
4.b Aromatic/amide H refined with riding coordinates:
 N104(H104), N4(H4), N106(H106), N6(H6), N5(H5), N105(H105), C110(H110),
 C111(H111), C130(H130), C22(H22), C30(H30), C114(H114), C118(H118), C113(H113),
  C18(H18), C126(H126), C112(H112), C10(H10), C129(H129), C21(H21), C19(H19),
 C14(H14), C29(H29), C128(H128), C127(H127), C26(H26), C28(H28), C122(H122),
 C20(H20), C119(H119), C27(H27), C13(H13), C11(H11), C121(H121), C12(H12),
 C120(H120)
;
_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
;