IPr*Thia – wingtip-flexible, sterically hindered, modular, N,C/S,C-chelating thiazole-donor N-heterocyclic carbene ligands
Podchorodecka, Pamela; Dziuk, Błażej; Junga, Robert; Szostak, Roman; Szostak, Michal; Bisz, Elwira; Dalton Transactions 53 (2024) 14975–14985; doi:10.1039/D4DT01468E

data_7716931
_publ_section_title
;
 IPr*Thia -- wingtip-flexible, sterically hindered, modular,
 N,C/S,C-chelating thiazole-donor N-heterocyclic carbene ligands
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              14975
_journal_page_last               14985
_journal_paper_doi               10.1039/D4DT01468E
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C45 H37 Cl2 N3 O Pd S'
_chemical_formula_sum            'C45 H37 Cl2 N3 O Pd S'
_chemical_formula_weight         845.13
_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_date             2024-06-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-08-26 deposited with the CCDC.	2024-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3287(3)
_cell_length_b                   9.49130(10)
_cell_length_c                   35.0477(3)
_cell_measurement_reflns_used    33757
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.156
_cell_measurement_theta_min      3.490
_cell_volume                     8425.55(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.42a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.42a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.42a (Rigaku OD, 2022)'
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            33757
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.156
_diffrn_reflns_theta_min         3.490
_exptl_absorpt_coefficient_mu    5.464
_exptl_absorpt_correction_T_max  0.579
_exptl_absorpt_correction_T_min  0.430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SCALE3 ABSPACK (Rigaku Oxford Diffraction, 2015).
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+13.6357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7670
_reflns_number_total             8078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01468e2.cif
_cod_data_source_block           pdbenzotiazol_auto_a
_cod_depositor_comments
'Adding full bibliography for 7716928--7716932.cif.'
_cod_database_code               7716931
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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:
 C19(H19), C33(H33)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C15(H15), C17(H17), C21(H21), C22(H22),
 C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
  C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C32(H32A,H32B,H32C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86327
_shelx_hkl_checksum              35774
_shelx_fab_checksum              61402
_olex2_submission_special_instructions 'No special instructions were received'