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_7716424
_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_absolute_configuration rmad
_chemical_formula_moiety         'C32 H37 N6 Pd, B F4'
_chemical_formula_sum            'C32 H37 B F4 N6 Pd'
_chemical_formula_weight         698.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-12-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_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                90
_cell_formula_units_Z            4
_cell_length_a                   16.3760(15)
_cell_length_b                   12.2333(11)
_cell_length_c                   15.8612(14)
_cell_measurement_reflns_used    8900
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.729
_cell_measurement_theta_min      2.439
_cell_volume                     3177.5(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0284
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25210
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         2.078
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0471 before and 0.0412 after correction.
The Ratio of minimum to maximum transmission is 0.9323.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 2394 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.022(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         7000
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+1.0817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                5790
_reflns_number_total             7000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00980k2.cif
_cod_data_source_block           2112011742
_cod_depositor_comments
'Adding full bibliography for 7716424--7716428.cif.'
_cod_database_code               7716424
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.910
_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
 C16-C15 = C16-C17 = C17-C18 = C20-C19 = C20-C21 = C22-C21
 1.53 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N1 \\sim C19 \\sim C20 \\sim C21: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N1 \\sim C19 \\sim C20 \\sim C21 \\sim C22: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C19 \\sim C20 \\sim C21 \\sim C22: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C23(H23),
 C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              34331
_shelx_hkl_checksum              90087
_olex2_submission_special_instructions 'No special instructions were received'