Efficient (11)C-Carbonylation of Isolated Aryl Palladium Complexes for PET: Application to Challenging Radiopharmaceutical Synthesis.
Andersen, Thomas L.; Friis, Stig D.; Audrain, Hélène; Nordeman, Patrik; Antoni, Gunnar; Skrydstrup, Troels; Journal of the American Chemical Society 137 (2015) 1548–1555; doi:10.1021/ja511441u

data_4123402
_publ_section_title
;
 Efficient (11)C-Carbonylation of Isolated Aryl Palladium Complexes for
 PET: Application to Challenging Radiopharmaceutical Synthesis.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1548
_journal_page_last               1555
_journal_paper_doi               10.1021/ja511441u
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C51 H40 F I N2 O P2 Pd, 2(C H Cl3)'
_chemical_formula_sum            'C53 H42 Cl6 F I N2 O P2 Pd'
_chemical_formula_weight         1249.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                82.131(3)
_cell_angle_beta                 81.984(3)
_cell_angle_gamma                74.532(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9999(3)
_cell_length_b                   12.0363(4)
_cell_length_c                   20.4093(7)
_cell_measurement_reflns_used    10362
_cell_measurement_temperature    159
_cell_measurement_theta_max      27.9600
_cell_measurement_theta_min      1.9250
_cell_volume                     2564.72(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      159
_diffrn_detector                 'Agilent Atlas CCD-area detector'
_diffrn_detector_area_resol_mean 10.3590
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_details
;
  1 omega   24.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8912  -99.0000 -120.0000 46

  2 omega  -20.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8912  -99.0000   90.0000 90

  3 omega  -23.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8912   57.0000 -120.0000 134

  4 omega  -81.00   62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8912  -77.0000  -30.0000 143

  5 omega  -72.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8912  -38.0000  -60.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0463592000
_diffrn_orient_matrix_UB_12      0.0529532000
_diffrn_orient_matrix_UB_13      0.0042192000
_diffrn_orient_matrix_UB_21      -0.0110319000
_diffrn_orient_matrix_UB_22      -0.0180634000
_diffrn_orient_matrix_UB_23      0.0343879000
_diffrn_orient_matrix_UB_31      0.0475197000
_diffrn_orient_matrix_UB_32      0.0254876000
_diffrn_orient_matrix_UB_33      0.0067111000
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21341
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.514
_diffrn_reflns_theta_min         1.765
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_type              'Agilent Mova'
_exptl_absorpt_coefficient_mu    1.383
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.4581
_exptl_crystal_size_mid          0.3144
_exptl_crystal_size_min          0.1706
_refine_diff_density_max         2.711
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         11420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0879P)^2^+9.7011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8559
_reflns_number_total             11420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja511441u_si_003.cif
_cod_data_source_block           2014_09_18
_cod_depositor_comments
'Adding full bibliography for 4123400--4123403.cif.'
_cod_original_cell_volume        2564.73(14)
_cod_database_code               4123402
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'Pd I3 C30 O5 H20'
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Others
 Sof(I1)=1-FVAR(1)
 Sof(I2)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C88(H88), C86(H86)
3.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B)
3.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C21(H21), C22(H22), C23(H23), N24(H24), C26(H26), C28(H28),
 C30(H30), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C39(H39), C42(H42),
  C43(H43), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51),
 C52(H52), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C66(H66),
  C70(H70), C72(H72), C78(H78), C87(H87), C91(H91), C1(H1), C5(H5), C6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'