An N-heterocyclic carbene-based pincer system of palladium and its versatile reactivity under oxidizing conditions.
Li, Haobin; Zhang, Bo; Feng, Rui; Guo, Shuai; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11470–11480; doi:10.1039/d4dt00980k

data_7716427
_publ_section_title
;
 An N-heterocyclic carbene-based pincer system of palladium and its
 versatile reactivity under oxidizing conditions.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11470
_journal_page_last               11480
_journal_paper_doi               10.1039/d4dt00980k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C22 H29 Cl3 N4 Pd'
_chemical_formula_sum            'C22 H29 Cl3 N4 Pd'
_chemical_formula_weight         562.24
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-10-03 deposited with the CCDC.	2024-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   29.2798(6)
_cell_length_b                   29.2798(6)
_cell_length_c                   16.1106(4)
_cell_measurement_reflns_used    9719
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      60.544
_cell_measurement_theta_min      3.860
_cell_volume                     11961.3(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            70746
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.516
_diffrn_reflns_theta_min         1.391
_diffrn_source_current           2.86
_diffrn_source_power             0.1997996
_diffrn_source_voltage           69.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.2102
_exptl_absorpt_correction_T_min  0.0895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1761 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.4258.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             5148
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.700
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         6106
_refine_ls_number_restraints     410
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0939P)^2^+70.4253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5429
_reflns_number_total             6106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00980k2.cif
_cod_data_source_block           2_sq
_cod_depositor_comments
'Adding full bibliography for 7716424--7716428.cif.'
_cod_original_cell_volume        11961.3(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7716427
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.808
_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
 C00Q-C00L = C1-C00Q = C2-C1 = C3-C00N = C5-C3 = C00N-C00J
 1.54 with sigma of 0.01
 H5A-H5C_$1
 2.1 with sigma of 0.01
3. Rigid bond restraints
 C00F, Cl04
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Pd01 \\sim Cl02 \\sim Cl03 \\sim Cl04 \\sim N005 \\sim N006 \\sim N007 \\sim
N008 \\sim C009 \\sim C00A \\sim C00B \\sim C00C \\sim C00D \\sim C00E \\sim
C00F \\sim C00G \\sim C00H \\sim C00I \\sim C00J \\sim C00K \\sim C00L \\sim
C00M \\sim C00N \\sim C00O \\sim C00P \\sim C00Q \\sim C1 \\sim C2 \\sim C3
\\sim C5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
5. Rigid body (RIGU) restrains
 Pd01, Cl02, Cl03, Cl04, N005, N006, N007, N008, C009, C00A, C00B, C00C, C00D,
 C00E, C00F, C00G, C00H, C00I, C00J, C00K, C00L, C00M, C00N, C00O, C00P, C00Q,
 C1, C2, C3, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6.a Secondary CH2 refined with riding coordinates:
 C00J(H00A,H00D), C00L(H00F,H00H), C00M(H00I,H00J), C00N(H00L,H00M), C00P(H00N,
 H00P), C00Q(H00Q,H00R), C1(H1A,H1B), C3(H3A,H3B)
6.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00B(H00B), C00C(H00C), C00E(H00E), C00G(H00G), C00K(H00K),
 C00O(H00O)
6.c Fitted hexagon refined as free rotating group:
 C00G(C00K,C00I,C00F,C00H,C00O)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              69045
_shelx_hkl_checksum              81827
_shelx_fab_checksum              10479
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'