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_7716870
_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         'C20 H34 F3 Ga N4 O, 0.067[H2O]'
_chemical_formula_sum            'C20 H34.13 F3 Ga N4 O1.07'
_chemical_formula_weight         474.489
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_Int_Tables_number      148
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-17
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-16 deposited with the CCDC.	2024-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   33.4699(7)
_cell_length_b                   33.4699(7)
_cell_length_c                   10.3165(2)
_cell_measurement_reflns_used    26160
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.4660
_cell_measurement_theta_min      2.0810
_cell_volume                     10008.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_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  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.8782
_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      1.00  56.00   0.20    1.20    --   12.24  57.00 -60.00  275
  2  \w    -32.00  18.00   0.20    1.20    --  -12.09  77.00 -90.00  250
  3  \w    -65.00 -22.00   0.20    1.20    --   12.24 -19.00 -90.00  215
  4  \w    -89.00  -7.00   0.20    1.20    --  -12.09 -25.00  31.00  410
  5  \w    -60.00 -11.00   0.20    1.20    --   12.24 -57.00 150.00  245
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0058462000
_diffrn_orient_matrix_UB_12      0.0233264000
_diffrn_orient_matrix_UB_13      0.0089597000
_diffrn_orient_matrix_UB_21      -0.0224226000
_diffrn_orient_matrix_UB_22      -0.0055281000
_diffrn_orient_matrix_UB_23      -0.0203503000
_diffrn_orient_matrix_UB_31      -0.0078220000
_diffrn_orient_matrix_UB_32      -0.0049441000
_diffrn_orient_matrix_UB_33      0.0650701000
_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  0.0201
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.9998
_diffrn_reflns_Laue_measured_fraction_max 0.8782
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31588
_diffrn_reflns_point_group_measured_fraction_full 0.9998
_diffrn_reflns_point_group_measured_fraction_max 0.8782
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.33
_diffrn_reflns_theta_min         2.10
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
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    1.417
_exptl_crystal_description       plate
_exptl_crystal_F_000             4484.659
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.2703
_refine_diff_density_min         -0.1814
_refine_diff_density_rms         0.0414
_refine_ls_d_res_high            0.6646
_refine_ls_d_res_low             9.7193
_refine_ls_goodness_of_fit_ref   1.0314
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     568
_refine_ls_number_reflns         6970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0314
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0136
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0120P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0264
_refine_ls_wR_factor_ref         0.0270
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              42
_reflns_limit_h_min              0
_reflns_limit_k_max              43
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                6293
_reflns_number_total             6970
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02074j2.cif
_cod_data_source_block           GR_CBG_GaF3L3_auto
_cod_depositor_comments
'Adding full bibliography for 7716867--7716872.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C20 H34.13 F3 Ga1 N4 O1.07'
_cod_database_code               7716870
_chemical_oxdiff_formula         GaF3C20H34N4O
_olex2_refinement_description
;
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      def2-TZVP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2024-01-12_19-17-00
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 12 electrons were 
found in a volume of 747\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.067[H2O] per Formula Unit 
which account for 12 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.704