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_7716867
_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         'Cl, C30 H37 N6 O3'
_chemical_formula_sum            'C30 H37 Cl N6 O3'
_chemical_formula_weight         565.119
_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_Int_Tables_number      14
_audit_creation_date             2024-01-19
_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                 99.705(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8300(3)
_cell_length_b                   23.5152(6)
_cell_length_c                   9.6411(2)
_cell_measurement_reflns_used    22237
_cell_measurement_temperature    102.0(3)
_cell_measurement_theta_max      32.1910
_cell_measurement_theta_min      1.7650
_cell_volume                     2867.09(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      102.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9954
_diffrn_measured_fraction_theta_max 0.8536
_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    -60.00 -11.00   0.50    1.14    --  -12.74 126.00 -14.00   98
  2  \w     22.00  67.00   0.50    1.14    --  -12.74  19.00-150.00   90
  3  \w    -55.00   2.00   0.50    1.14    --  -12.74 -57.00 -90.00  114
  4  \w    -56.00   2.00   0.50    1.14    --  -12.74 -57.00   0.00  116
  5  \w     21.00  68.00   0.50    1.14    --  -12.74  19.00  30.00   94
  6  \w     21.00  97.00   0.50    1.14    --   16.02  19.00   0.00  152
  7  \w      1.00  62.00   0.50    1.14    --   16.02  57.00 -60.00  122
  8  \w     -1.00  35.00   0.50    1.14    --   16.02 -77.00 150.00   72
  9  \w     17.00  64.00   0.50    1.14    --   16.02-126.00 -91.00   94
;
_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      0.0447064000
_diffrn_orient_matrix_UB_12      -0.0181716000
_diffrn_orient_matrix_UB_13      0.0065277000
_diffrn_orient_matrix_UB_21      0.0332973000
_diffrn_orient_matrix_UB_22      0.0239977000
_diffrn_orient_matrix_UB_23      -0.0014752000
_diffrn_orient_matrix_UB_31      0.0061981000
_diffrn_orient_matrix_UB_32      0.0020632000
_diffrn_orient_matrix_UB_33      0.0743088000
_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  0.0293
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.9954
_diffrn_reflns_Laue_measured_fraction_max 0.8536
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33643
_diffrn_reflns_point_group_measured_fraction_full 0.9954
_diffrn_reflns_point_group_measured_fraction_max 0.8536
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.34
_diffrn_reflns_theta_min         1.83
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
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    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             1201.306
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.9785
_refine_diff_density_min         -0.4467
_refine_diff_density_rms         0.0771
_refine_ls_d_res_high            0.6643
_refine_ls_d_res_low             11.1379
_refine_ls_goodness_of_fit_ref   1.0239
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     694
_refine_ls_number_reflns         8740
_refine_ls_number_restraints     651
_refine_ls_restrained_S_all      0.9848
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.4520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                6674
_reflns_number_total             8740
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02074j2.cif
_cod_data_source_block           CB9366_59_Ligand1Cl
_cod_depositor_comments
'Adding full bibliography for 7716867--7716872.cif.'
_cod_database_code               7716867
_chemical_oxdiff_formula         AlC30H36N9O12
_chemical_oxdiff_usercomment     Al(NO3)3(L1)
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 O1, O2, O3, N1, H1, N2, N3, N4, H4, N5, H5, N6, H6, C1, H1a, H1b, C2, H2a,
 H2b, C3, H3a, H3b, C4, H4a, H4b, C5, H5a, H5b, C6, H6a, H6b, C7, H7a, H7b, C8,
 C9, C10, H10, C11, H11, C12, H12, C13, H13, C14, H14, C15, H15a, H15b, C16,
 C17, C18, H18, C19, H19, C20, H20, C21, H21, C22, H22, C23, H23a, H23b, C24,
 C25, C26, H26, C27, H27, C28, H28, C29, H29, C30, H30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_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:           2024-01-18_17-26-23
;
_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 2.552
_oxdiff_exptl_absorpt_empirical_full_min 0.644