IPaul<sup>Het</sup> - spatially-defined, wingtip-flexible, N,C-chelating oxazole and thiazole donor N-heterocyclic carbene ligands.
Podchorodecka, Pamela; Dziuk, Błażej; Szostak, Roman; Szostak, Michal; Bisz, Elwira; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14267–14276; doi:10.1039/d5dt01576f

data_7719244
_publ_section_title
;
 IPaul<sup>Het</sup> - spatially-defined, wingtip-flexible, N,C-chelating
 oxazole and thiazole donor N-heterocyclic carbene ligands.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14267
_journal_page_last               14276
_journal_paper_doi               10.1039/d5dt01576f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C33 H29 Cl2 N3 Pd S'
_chemical_formula_sum            'C33 H29 Cl2 N3 Pd S'
_chemical_formula_weight         676.95
_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_date             2025-05-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-05-21 deposited with the CCDC.	2025-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                92.378(4)
_cell_angle_beta                 90.992(4)
_cell_angle_gamma                111.940(5)
_cell_formula_units_Z            2
_cell_length_a                   8.2937(5)
_cell_length_b                   9.1141(4)
_cell_length_c                   20.2862(9)
_cell_measurement_reflns_used    5542
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.9910
_cell_measurement_theta_min      2.1790
_cell_volume                     1420.25(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.105a 64-bit (release 11-01-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     35.00  62.00   0.50   12.00    --   62.50  15.00-150.00   54
  2  \w     28.00  61.00   0.50   12.00    --   62.50-125.00-120.00   66
  3  \w     39.00  97.00   0.50   12.00    --   62.50   0.00-120.00  116
  4  \w     28.00 100.00   0.50   12.00    --   62.50   0.00 -30.00  144
  5  \w     27.00  53.00   0.50   12.00    --   62.50 -95.00 -60.00   52
  6  \w     31.00  62.00   0.50   12.00    --   62.50 -95.00   0.00   62
  7  \w     67.00  95.00   0.50   12.00    --   62.50  15.00-150.00   56
  8  \w    -62.00 -32.00   0.50   12.00    --  -63.51 -15.00 -60.00   60
  9  \w   -109.00 -80.00   0.50   12.00    --  -63.51 -15.00-120.00   58
 10  \w   -100.00 -74.00   0.50   12.00    --  -63.51 -15.00 -60.00   52
 11  \w    -75.00 -36.00   0.50   12.00    --  -63.51 -15.00-120.00   78
 12  \w   -102.00 -75.00   0.50   12.00    --  -70.64 -15.00  30.00   54
 13  \w    -95.00 -64.00   0.50   12.00    --  -70.64 125.00-180.00   62
 14  \w    -71.00 -46.00   0.50   12.00    --  -70.64 -15.00  30.00   50
 15  \w    -97.00 -66.00   0.50   12.00    --  -70.64 125.00  60.00   62
 16  \w    -92.00 -61.00   0.50   12.00    --  -70.64 125.00 -90.00   62
 17  \w    -54.00 -29.00   0.50   12.00    --  -70.64 125.00-180.00   50
 18  \w     59.00 104.00   0.50   12.00    --   70.79  15.00 120.00   90
 19  \w     73.00 108.00   0.50   12.00    --   70.79  15.00-120.00   70
 20  \w     31.00  57.00   0.50   12.00    --   70.79-125.00 -60.00   52
 21  \w     35.00  79.00   0.50   12.00    --   70.79 -95.00  60.00   88
 22  \w     34.00  78.00   0.50   12.00    --   70.79 -95.00 150.00   88
 23  \w     72.00  98.00   0.50   12.00    --   70.79-125.00 -60.00   52
 24  \w   -115.00 -66.00   0.50   12.00    --  -74.00 146.00  -3.27   98
 25  \w     38.00  63.00   0.50   12.00    --   75.87 -95.00 -60.00   50
 26  \w     47.00  97.00   0.50   12.00    --   75.87  15.00 -90.00  100
 27  \w     39.00  64.00   0.50   12.00    --   75.87 -95.00-150.00   50
 28  \w     39.00 113.00   0.50   12.00    --   75.87   0.00  30.00  148
 29  \w   -110.00 -84.00   0.50   12.00    --  -75.92 135.00  18.00   52
 30  \w   -104.00 -35.00   0.50   12.00    --  -75.92 126.00-139.14  138
 31  \w   -113.00 -35.00   0.50   12.00    --  -75.92 140.00 -43.38  156
 32  \w    -72.00 -39.00   0.50   12.00    --  -75.92 135.00  18.00   66
 33  \w    -60.00 -35.00   0.50   12.00    --  -76.86 125.00  90.00   50
 34  \w   -101.00 -75.00   0.50   12.00    --  -76.86 125.00  90.00   52
 35  \w   -101.00 -45.00   0.50   12.00    --  -76.86 125.00-180.00  112
 36  \w   -103.00 -38.00   0.50   12.00    --  -76.86 125.00 120.00  130
 37  \w    -61.00 -36.00   0.50   12.00    --  -76.86 125.00 -60.00   50
 38  \w    -69.00 -40.00   0.50   12.00    --  -76.86 125.00  60.00   58
 39  \w    -68.00 -43.00   0.50   12.00    --  -76.86 125.00 -90.00   50
 40  \w   -103.00 -77.00   0.50   12.00    --  -76.86 125.00 -90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18075
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.431
_diffrn_reflns_theta_min         2.181
_exptl_absorpt_coefficient_mu    7.908
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.879
_refine_diff_density_min         -1.680
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0717P)^2^+4.0290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3981
_reflns_number_total             5438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01576f2.cif
_cod_data_source_block           pdipaultiaz
_cod_depositor_comments
'Adding full bibliography for 7719242--7719244.cif.'
_cod_original_cell_volume        1420.27(13)
_cod_database_code               7719244
_shelx_shelxl_version_number     2014/7
_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.a Ternary CH refined with riding coordinates:
 C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C33(H33), C24(H24), C14(H14), C32(H32), C20(H20), C8(H8), C15(H15),
 C31(H31), C16(H16), C18(H18), C6(H6), C17(H17), C23(H23), C22(H22), C21(H21)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C11(H11A,H11B,H11C), C26(H26A,H26B,H26C), C10(H10A,H10B,
 H10C)
;
_shelx_res_checksum              4168
_shelx_hkl_checksum              31620
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;