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_7716426
_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         'C37 H40 N7 Pd, 2(C F3 O3 S), B F4'
_chemical_formula_sum            'C39 H40 B F10 N7 O6 Pd S2'
_chemical_formula_weight         1074.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2023-10-03 deposited with the CCDC.	2024-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.110(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7271(4)
_cell_length_b                   21.7582(7)
_cell_length_c                   16.9612(6)
_cell_measurement_reflns_used    9756
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      56.897
_cell_measurement_theta_min      3.534
_cell_volume                     4316.7(3)
_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      150.00
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.971
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39816
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.406
_diffrn_reflns_theta_min         1.525
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1299 before and 0.0685 after correction.
The Ratio of minimum to maximum transmission is 0.6920.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.944
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         8601
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0763
_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^)+(0.1288P)^2^+15.4757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2129
_refine_ls_wR_factor_ref         0.2259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7029
_reflns_number_total             8601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00980k2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7716424--7716428.cif.'
_cod_database_code               7716426
_shelx_shelxl_version_number     2018/3
_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. Uiso/Uaniso restraints and constraints
S2 \\sim O5 \\sim O9 \\sim F8 \\sim F10 \\sim F11 \\sim O7 \\sim C2 \\sim S3
\\sim F9 \\sim F13 \\sim C1 \\sim F12 \\sim O6 \\sim O8 \\sim O4: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
3. Others
 Sof(F11)=Sof(S3)=Sof(F13)=Sof(C1)=Sof(F12)=Sof(O6)=Sof(O8)=Sof(O4)=1-FVAR(1)
 Sof(S2)=Sof(O5)=Sof(O9)=Sof(F8)=Sof(F10)=Sof(O7)=Sof(C2)=Sof(F9)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C6(H6A,H6B), C17(H17A,H17B), C10(H10A,H10B), C4(H4A,H4B),
 C22(H22A,H22B), C5(H5A,H5B), C23(H23A,H23B)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C39(H39), C28(H28), C25(H25), C19(H19), C12(H12), C36(H36),
 C20(H20), C31(H31), C26(H26), C14(H14), C27(H27), C38(H38), C37(H37), C33(H33),
  C32(H32), C13(H13)
4.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              32099
_shelx_hkl_checksum              2110
_olex2_submission_special_instructions 'No special instructions were received'