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_4123400
_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         'C47 H39 I N P2 Pd'
_chemical_formula_sum            'C47 H39 I N P2 Pd'
_chemical_formula_weight         913.03
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.523(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.98013(19)
_cell_length_b                   40.0170(6)
_cell_length_c                   10.6433(2)
_cell_measurement_reflns_used    20893
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.6380
_cell_measurement_theta_min      2.5570
_cell_volume                     3867.23(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      100
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0093313000
_diffrn_orient_matrix_UB_12      -0.0105422000
_diffrn_orient_matrix_UB_13      0.0493005000
_diffrn_orient_matrix_UB_21      -0.0652793000
_diffrn_orient_matrix_UB_22      -0.0065967000
_diffrn_orient_matrix_UB_23      -0.0523304000
_diffrn_orient_matrix_UB_31      0.0419113000
_diffrn_orient_matrix_UB_32      -0.0126226000
_diffrn_orient_matrix_UB_33      -0.0139019000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41392
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.93
_diffrn_reflns_theta_min         2.16
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.1907
_exptl_crystal_size_mid          0.0875
_exptl_crystal_size_min          0.0789
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.422
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.344
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.344
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+17.9852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                8497
_reflns_number_total             9328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja511441u_si_004.cif
_cod_data_source_block           2013_01_20c
_cod_depositor_comments
'Adding full bibliography for 4123400--4123403.cif.'
_cod_original_cell_volume        3867.21(12)
_cod_database_code               4123400
_chemical_oxdiff_formula         'C47 H38 I Pd P2 N'
_reflns_odcompleteness_completeness 99.94
_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 N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C11(H11), C14(H14), C16(H16), C18(H18), C20(H20), C23(H23),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), N33(H33),
  C34(H34), C35(H35), C37(H37), C39(H39), C40(H40), C41(H41), C43(H43),
 C46(H46), C47(H47), C48(H48), C50(H50), C52(H52), C55(H55), C59(H59), C60(H60),
  C61(H61), C64(H64), C2(H2), C3(H3), C6(H6), C10(H10), C12(H12), C13(H13)
;