Last-step 18F-fluorination of supported 2-(aryl-di-tert-butylsilyl)-N-methyl-imidazole conjugates for applications in positron emission tomography
Steffann, Marine; Tisseraud, Marion; Bluet, Guillaume; Roy, Sebastien; Aubert, Catherine; Fouquet, Eric; Hermange, Philippe; Chemical Communications  (2022) –; doi:10.1039/D2CC03258A

data_7130425
_publ_section_title
;
 Last-step 18F-fluorination of supported
 2-(aryl-di-tert-butylsilyl)-N-methyl-imidazole conjugates for
 applications in positron emission tomography
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03258A
_journal_year                    2022
_chemical_formula_moiety         'C21 H34 N2 O2 Si'
_chemical_formula_sum            'C21 H34 N2 O2 Si'
_chemical_formula_weight         374.59
_chemical_name_common            'Compound 6'
_chemical_name_systematic        'UVX1 Phenol'
_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_method           SHELXL-2018/3
_audit_update_record
;
2022-05-02 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.646(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6666(12)
_cell_length_b                   14.7352(16)
_cell_length_c                   13.3183(14)
_cell_measurement_reflns_used    3055
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.402
_cell_measurement_theta_min      2.063
_cell_volume                     2204.7(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker AXS Inc.)'
_computing_data_collection       'APEX2 20133.10-0 (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT v8.34A (Bruker AXS Inc.)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
'SUPERFLIP(Palatinus & Chapuis, 2007) EDMA(Palatinus et al., 2012)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX Duo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30764
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.402
_diffrn_reflns_theta_min         2.063
_diffrn_source                   'microfocus sealed tude'
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2012/1 (Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             816
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethyle acetate/toluene'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4533
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+1.6166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3055
_reflns_number_total             4533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03258a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7130425
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              72224
_shelx_hkl_checksum              64707