Rhenium(i) complexation‒dissociation strategy for synthesising fluorine-18 labelled pyridine bidentate radiotracers
Klenner, Mitchell A.; Zhang, Bo; Ciancaleoni, Gianluca; Howard, James K.; Maynard-Casely, Helen E.; Clegg, Jack K.; Massi, Massimiliano; Fraser, Benjamin H.; Pascali, Giancarlo; RSC Advances 10 (2020) 8853–8865; doi:10.1039/D0RA00318B

data_7240001
_publ_section_title
;
 Rhenium(i) complexation--dissociation strategy for synthesising
 fluorine-18 labelled pyridine bidentate radiotracers
;
_journal_issue                   15
_journal_name_full               'RSC Advances'
_journal_page_first              8853
_journal_page_last               8865
_journal_paper_doi               10.1039/D0RA00318B
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C13 H7 Cl F N2 O3 Re'
_chemical_formula_sum            'C13 H7 Cl F N2 O3 Re'
_chemical_formula_weight         479.86
_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   geom
_audit_creation_date             2019-12-10
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-10 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.25(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9600(16)
_cell_length_b                   17.171(3)
_cell_length_c                   10.245(2)
_cell_measurement_reflns_used    19995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.484
_cell_measurement_theta_min      2.337
_cell_volume                     1382.1(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.886
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'MX1 Beamline Australian Synchrotron'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.886
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19995
_diffrn_reflns_point_group_measured_fraction_full 0.886
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.337
_exptl_absorpt_coefficient_mu    9.007
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.306
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.087
_refine_diff_density_min         -1.623
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       0.0089(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+5.9471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2728
_reflns_number_total             2754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra00318b2.cif
_cod_data_source_block           re6
_cod_depositor_comments
'Adding full bibliography for 7239999--7240003.cif.'
_cod_database_code               7240001
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{C1, C1A}
{C9, C9A}
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C1A)
Uanis(C9) = Uanis(C9A)
4. Others
 Fixed Sof: H0AA(0.25) H0AB(0.75) H2A(0.75) H2B(0.25) F2(0.25) C1(0.75)
 C9(0.25) H9(0.75) F1(0.75) C1A(0.25) H1A(0.25) C9A(0.75)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C0AA(H0AA), C0AA(H0AB), C8(H8), C2(H2A), C2(H2B), C7(H7),
 C9(H9), C1A(H1A)
;
_shelx_res_checksum              52476
_olex2_submission_special_instructions 'No special instructions were received'