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_7240002
_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 Cl2 N2 O3 Re'
_chemical_formula_sum            'C13 H7 Cl2 N2 O3 Re'
_chemical_formula_weight         496.3159
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-02-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-12-10 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                102.17(3)
_cell_angle_beta                 99.94(3)
_cell_angle_gamma                102.50(3)
_cell_formula_units_Z            6
_cell_length_a                   11.318(2)
_cell_length_b                   12.872(3)
_cell_length_c                   15.669(3)
_cell_measurement_reflns_used    31430
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.677
_cell_volume                     2120.8(9)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.888
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.888
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31430
_diffrn_reflns_point_group_measured_fraction_full 0.888
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.677
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.981
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.331
_exptl_crystal_description       block
_exptl_crystal_F_000             1295
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.531
_refine_diff_density_min         -2.672
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       0.0054(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         8464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0285P)^2^+23.4685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8326
_reflns_number_total             8464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra00318b2.cif
_cod_data_source_block           re5
_cod_depositor_comments
'Adding full bibliography for 7239999--7240003.cif.'
_cod_original_cell_volume        2120.8(8)
_cod_original_formula_sum        ' C13 H7 Cl2 N2 O3 Re'
_cod_database_code               7240002
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C27(H27), C7(H7), C17(H17), C23(H23), C16(H16), C2(H2),
 C3(H3), C14(H14), C36(H36), C8(H8), C22(H22), C30(H30), C4(H4), C35(H35),
 C29(H29), C34(H34), C33(H33), C21(H21), C20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'