Bioconjugated arylpalladium complexes on solid supports for a convenient last-step synthesis of 11C-labelled tracers for positron emission tomography
Tabey, Alexis; Audrain, Hélène; Fouquet, Eric; Hermange, Philippe; Chemical Communications  (2019) –; doi:10.1039/C9CC03215K

data_7123636
_publ_section_title
;
 Bioconjugated arylpalladium complexes on solid supports for a convenient
 last-step synthesis of 11C-labelled tracers for positron emission
 tomography
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03215K
_journal_year                    2019
_chemical_formula_moiety         'C45 H41 I O2 P2 Pd'
_chemical_formula_sum            'C45 H41 I O2 P2 Pd'
_chemical_formula_weight         909.02
_chemical_name_common            '2a, AT485'
_chemical_name_systematic
'[(2-Hydroxymethyl-4-methoxy-5-(methyl))phenyl]iodobis(triphenyl-phosphine)palladium'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-02-18 deposited with the CCDC.    2019-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.186(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.4172(17)
_cell_length_b                   16.1367(16)
_cell_length_c                   30.889(3)
_cell_measurement_reflns_used    12760
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.474
_cell_measurement_theta_min      2.209
_cell_volume                     8668.1(15)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SUPERFLIP(Palatinus & Chapuis, 2007) EDMA(Palatinus et al., 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.938
_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  0.0339
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            79437
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.474
_diffrn_reflns_theta_min         2.209
_diffrn_source                   'microfocus sealed tude'
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2012/1 (Bruker AXS)'
_exptl_crystal_colour            'yellow oranged'
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       \,cube
_exptl_crystal_F_000             3648
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane'
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.350
_platon_squeeze_details
;
The unit cell contains 1 dichloromethane molecule and 1/2 carbon dioxid molecule
which have been treated as a diffuse contribution 
to the overall scattering without specific atom positions
by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         14684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+7.6062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12760
_reflns_number_total             14684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03215k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7123636
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.475
_shelx_estimated_absorpt_t_max   0.669
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              88834