Orthopalladated imidazolones and thiazolones: synthesis, photophysical properties and photochemical reactivity.
Dumitraş, Darius; Dalmau, David; García-Orduña, Pilar; Pop, Alexandra; Silvestru, Anca; Urriolabeitia, Esteban P.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8948–8957; doi:10.1039/d4dt00730a

data_7715926
_publ_section_title
;
 Orthopalladated imidazolones and thiazolones: synthesis, photophysical
 properties and photochemical reactivity.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8948
_journal_page_last               8957
_journal_paper_doi               10.1039/d4dt00730a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C25 H19 F3 N2 O5 Pd S, C H Cl3'
_chemical_formula_sum            'C26 H20 Cl3 F3 N2 O5 Pd S'
_chemical_formula_weight         742.25
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2jfkzj
_audit_creation_date             2023-10-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-01 deposited with the CCDC.	2024-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                99.929(2)
_cell_angle_beta                 96.086(2)
_cell_angle_gamma                105.978(2)
_cell_formula_units_Z            6
_cell_length_a                   15.5603(7)
_cell_length_b                   15.6327(7)
_cell_length_c                   18.9399(9)
_cell_measurement_reflns_used    9562
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.306
_cell_measurement_theta_min      2.709
_cell_volume                     4305.1(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS, 2016) in APEX4'
_computing_data_collection       'SAINT V8.40B (Bruker AXS, 2016) in APEX4'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS, 2016) in APEX4'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon III'
_diffrn_detector_type            'Bruker Photon III area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Photon III , D8 Venture diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            311383
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.320
_diffrn_reflns_theta_min         2.213
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Diamond  Incoatec Microfocus Source '
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0759 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.9477.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       prism
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.045
_refine_diff_density_max         2.449
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         21401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+14.5762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19365
_reflns_number_total             21401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00730a2.cif
_cod_data_source_block           cmpnd_B
_cod_depositor_comments
'Adding full bibliography for 7715922--7715926.cif.'
_cod_database_code               7715926
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.879
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
 Sof(F31B)=Sof(F32B)=Sof(F33B)=1-FVAR(2)
 Sof(F31A)=Sof(F32A)=Sof(F33A)=FVAR(2)
 Sof(F61B)=Sof(F62B)=Sof(F63B)=1-FVAR(3)
 Sof(F61A)=Sof(F62A)=Sof(F63A)=FVAR(3)
3.a Ternary CH refined with riding coordinates:
 C92(H92), C91(H91)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C35(H35), C39(H39), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C62(H62), C65(H65),
  C69(H69), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79),
 C80(H80), C81(H81), C82(H82), C83(H83), C2(H2), C5(H5), C9(H9), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23)
3.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C67(H67A,H67B,H67C), C68(H68A,H68B,
 H68C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 124 electrons were 
found in a volume of 326\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[CHCl3] per Unit Cell 
which account for 116 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38125
_shelx_fab_checksum              4313
_olex2_submission_special_instructions 'No special instructions were received'