Synthesis and [*C]CO-labelling of (C,N) <i>gem</i>-dimethylbenzylamine-palladium complexes for potential applications in positron emission tomography.
Cormier, Morgan; Tabey, Alexis; Christine, Thifanie; Audrain, Hélène; Fouquet, Eric; Hermange, Philippe; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10608–10614; doi:10.1039/d1dt01633d

data_7707847
_publ_section_title
;
 Synthesis and [*C]CO-labelling of (C,N)
 <i>gem</i>-dimethylbenzylamine-palladium complexes for potential
 applications in positron emission tomography.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10608
_journal_page_last               10614
_journal_paper_doi               10.1039/d1dt01633d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C25 H23 I N P Pd, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C25.5 H24 Cl I N P Pd'
_chemical_formula_weight         644.17
_chemical_name_common            'AT486 / Compound 2'
_chemical_name_systematic
'[2-(Aminomethyl)phenyl-\k2-C,N]iodotriphenylphosphinepalladium'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-03-13 deposited with the CCDC.	2021-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   14.0231(8)
_cell_length_b                   22.4946(16)
_cell_length_c                   30.2437(18)
_cell_measurement_reflns_used    7259
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.396
_cell_measurement_theta_min      1.347
_cell_volume                     9540.2(10)
_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 0.998
_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  0.1076
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56885
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.396
_diffrn_reflns_theta_min         1.347
_diffrn_source                   'microfocus sealed tude'
_exptl_absorpt_coefficient_mu    2.265
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2012/1 (Bruker AXS)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'little leaf'
_exptl_crystal_F_000             5040
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, Et2O'
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.408
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         9754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0829P)^2^+3.2132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7259
_reflns_number_total             9754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01633d2.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 

 Adding full bibliography for 7707847.cif.

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C51 H48 Cl2 I2 N2 P2 Pd2'
_cod_original_formula_weight         1288.35
_cod_original_formula_moiety         'C51 H48 Cl2 I2 N2 P2 Pd2'
_cod_original_formula_units_Z            8
_cod_database_code               7707847
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.580
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              49692
_shelx_hkl_checksum              42372