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_7239999
_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         'C14 H8 N3 O6 Re'
_chemical_formula_sum            'C14 H8 N3 O6 Re'
_chemical_formula_weight         500.44
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-15
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289)
;
_audit_update_record
;
2019-12-10 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.415(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0671(4)
_cell_length_b                   15.9871(5)
_cell_length_c                   7.5731(2)
_cell_measurement_reflns_used    12428
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.1680
_cell_measurement_theta_min      2.9620
_cell_volume                     1572.15(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.17a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.17a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.17a (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Cd/Te HPAD'
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     23.00  69.00   0.50    1.00    --    7.96  77.00  37.00   92
  2  \w    -59.00  32.00   0.50    1.00    --    7.96 -77.00 -87.00  182
  3  \w     -5.00  41.00   0.50    1.00    --    7.96 -99.00  30.00   92
  4  \w    -68.00  23.00   0.50    1.00    --    7.96 -37.00 120.00  182
  5  \w     -4.00  41.00   0.50    1.00    --    7.96 -99.00   0.00   90
  6  \w     10.00  67.00   0.50    1.00    --    7.96  57.00-120.00  114
  7  \w     -5.00  20.00   0.50    1.00    --    7.96 -99.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0271402000
_diffrn_orient_matrix_UB_12      0.0339637000
_diffrn_orient_matrix_UB_13      0.0330147000
_diffrn_orient_matrix_UB_21      -0.0468313000
_diffrn_orient_matrix_UB_22      -0.0159939000
_diffrn_orient_matrix_UB_23      -0.0433560000
_diffrn_orient_matrix_UB_31      -0.0072961000
_diffrn_orient_matrix_UB_32      -0.0236422000
_diffrn_orient_matrix_UB_33      0.0769137000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19869
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.548
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.17a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.123
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.298
_refine_diff_density_min         -1.991
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0611P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3382
_reflns_number_total             3893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra00318b2.cif
_cod_data_source_block           sjkc19hm01
_cod_depositor_comments
'Adding full bibliography for 7239999--7240003.cif.'
_cod_original_cell_volume        1572.14(8)
_cod_database_code               7239999
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 N2 Cl2 Re H20 P F6'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C10(H10), C9(H9), C8(H8)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_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 3.940
_oxdiff_exptl_absorpt_empirical_full_min 0.410