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_7715922
_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         'C28 H26 F3 N3 O5 Pd, C H Cl3'
_chemical_formula_sum            'C29 H27 Cl3 F3 N3 O5 Pd'
_chemical_formula_weight         767.28
_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.cc2jfkyh
_audit_creation_date             2023-05-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-03-01 deposited with the CCDC.	2024-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                89.484(2)
_cell_angle_beta                 80.014(2)
_cell_angle_gamma                80.670(2)
_cell_formula_units_Z            4
_cell_length_a                   12.1193(6)
_cell_length_b                   14.8888(7)
_cell_length_c                   18.4550(8)
_cell_measurement_reflns_used    9255
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.996
_cell_measurement_theta_min      2.241
_cell_volume                     3235.6(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 0.995
_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  0.0943
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            416895
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.997
_diffrn_reflns_theta_min         1.890
_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    0.880
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.7056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1090 before and 0.0710 after correction.
The Ratio of minimum to maximum transmission is 0.9450.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       needle
_exptl_crystal_F_000             1544
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         26272
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0418P)^2^+4.5601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17560
_reflns_number_total             26272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00730a2.cif
_cod_data_source_block           cmpnd_A
_cod_depositor_comments
'Adding full bibliography for 7715922--7715926.cif.'
_cod_database_code               7715922
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.898
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C77-C78 \\sim C77-C78A
 with sigma of 0.02
 C78-F51A \\sim C78A-F53B
 with sigma of 0.02
 C78-F53A \\sim C78A-F52B
 with sigma of 0.02
 C78-F52A \\sim C78A-F51B
 with sigma of 0.02
 C77-F51A \\sim C77-F53B
 with sigma of 0.04
 C77-F53A \\sim C77-F52B
 with sigma of 0.04
 C77-F52A \\sim C77-F51B
 with sigma of 0.04
 F51A-F53A \\sim F53B-F52B
 with sigma of 0.04
 F51A-F52A \\sim F53B-F51B
 with sigma of 0.04
 F53A-F52A \\sim F52B-F51B
 with sigma of 0.04
3. Others
 Sof(F1B)=Sof(F3B)=Sof(F2B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
 Sof(C78A)=Sof(F53B)=Sof(F52B)=Sof(F51B)=1-FVAR(2)
 Sof(C78)=Sof(F51A)=Sof(F53A)=Sof(F52A)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C81(H81), C91(H91)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C63(H63A,H63B), C64(H64A,H64B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C52(H52), C55(H55), C59(H59),
  C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73),
 C74(H74), C75(H75), C76(H76)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C57(H57A,H57B,H57C),
 C58(H58A,H58B,H58C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              42820
_olex2_submission_special_instructions 'No special instructions were received'