Well-defined, air- and moisture-stable palladium–imidazo[1,5-a]pyridin-3-ylidene complexes: a versatile catalyst platform for cross-coupling reactions by L-shaped NHC ligands
Zhou, Tongliang; Gao, Pengcheng; Bisz, Elwira; Dziuk, Błażej; Lalancette, Roger; Szostak, Roman; Szostak, Michal; Catalysis Science & Technology 12 (2022) 6581–6589; doi:10.1039/D2CY01136K

data_1567672
_publ_section_title
;
 Well-defined, air- and moisture-stable
 palladium--imidazo[1,5-a]pyridin-3-ylidene complexes: a versatile
 catalyst platform for cross-coupling reactions by L-shaped NHC ligands
;
_journal_issue                   21
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              6581
_journal_page_last               6589
_journal_paper_doi               10.1039/D2CY01136K
_journal_volume                  12
_journal_year                    2022
_chemical_formula_sum            'C37 H40 Cl N2 Pd'
_chemical_formula_weight         654.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-05-23 deposited with the CCDC.	2022-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.10(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.260(8)
_cell_length_b                   14.479(6)
_cell_length_c                   22.541(8)
_cell_measurement_reflns_used    30836
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.000
_cell_measurement_theta_min      2.276
_cell_volume                     6980(5)
_computing_cell_refinement       'CrysAlisPro (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2014)'
_computing_data_reduction        'CrysAlisPro (Rigaku OD, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'KM4 with Eos CCD'
_diffrn_measurement_method       \w--scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2734
_diffrn_reflns_av_unetI/netI     0.7438
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30836
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.276
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SCALE3 ABSPACK (Rigaku Oxford Diffraction, 2015).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         13715
_refine_ls_number_restraints     1050
_refine_ls_restrained_S_all      0.810
_refine_ls_R_factor_all          0.4374
_refine_ls_R_factor_gt           0.1364
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0978P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2642
_refine_ls_wR_factor_ref         0.3906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2194
_reflns_number_total             13715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cy01136k2.cif
_cod_data_source_block           B4_a
_cod_depositor_comments
;
Adding full bibliography for 1567672--1567675.cif.

2025-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C74 H80 Cl2 N4 Pd2'
_cod_original_formula_weight         1309.12
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               1567672
_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.
;
_shelx_res_checksum              71097