Synthesis of carbon-11 radiolabelled transition metal complexes using 11C-dithiocarbamates
Cesarec, Sara; Edgar, Fraser; Lai, Titan; White, Andrew J. P.; Plisson, Christophe; Miller, Philip; Dalton Transactions  (2022) –; doi:10.1039/D2DT00266C

data_7709730
_publ_section_title
;
 Synthesis of carbon-11 radiolabelled transition metal complexes using
 11C-dithiocarbamates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00266C
_journal_year                    2022
_chemical_formula_moiety         'C32 H36 N P2 Pd S2, 2(C H Cl3), Cl'
_chemical_formula_sum            'C34 H38 Cl7 N P2 Pd S2'
_chemical_formula_weight         941.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-21 deposited with the CCDC.	2022-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                91.6478(16)
_cell_angle_beta                 92.6572(16)
_cell_angle_gamma                92.2153(12)
_cell_formula_units_Z            4
_cell_length_a                   15.3553(2)
_cell_length_b                   15.3770(2)
_cell_length_c                   17.2255(4)
_cell_measurement_reflns_used    40413
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.1410
_cell_measurement_theta_min      2.7200
_cell_volume                     4057.95(12)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23485
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.333
_diffrn_reflns_theta_min         2.660
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.176
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         23485
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0652P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19348
_reflns_number_total             23485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00266c2.cif
_cod_data_source_block           8
_cod_original_cell_volume        4057.94(13)
_cod_database_code               7709730
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              48629
_shelx_hkl_checksum              41919