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_7716428
_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 ad
_chemical_formula_moiety         'C26 H36 N6 O Pd, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C28 H39 B2 F8 N7 O Pd'
_chemical_formula_weight         769.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2024-04-03 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            8
_cell_length_a                   17.7077(7)
_cell_length_b                   19.2040(7)
_cell_length_c                   20.5693(7)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      56.90
_cell_measurement_theta_min      2.86
_cell_volume                     6994.8(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            78110
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.400
_diffrn_reflns_theta_min         1.451
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1176 before and 0.0840 after correction.
The Ratio of minimum to maximum transmission is 0.8232.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 4803 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.745(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         14285
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0756P)^2^+3.1741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1408
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                12271
_reflns_number_total             14285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00980k2.cif
_cod_data_source_block           20231120_2_0m
_cod_depositor_comments
'Adding full bibliography for 7716424--7716428.cif.'
_cod_database_code               7716428
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N14 \\sim C57 \\sim C58: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
F3 \\sim B1 \\sim F2 \\sim F1 \\sim F4: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
F10 \\sim F11 \\sim B3 \\sim F12 \\sim F9: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N13 \\sim C55 \\sim C56: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
3. Others
 Sof(H15A)=Sof(Pd3)=1-FVAR(1)
 Sof(Pd2)=Sof(H15)=FVAR(1)
 Sof(H16A)=Sof(Pd4)=1-FVAR(2)
 Sof(Pd1)=Sof(H16)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C14(H14A,H14B), C21(H21A,H21B),
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C30(H30A,H30B), C31(H31A,H31B),
  C32(H32A,H32B), C36(H36A,H36B), C43(H43A,H43B), C47(H47A,H47B), C48(H48A,
 H48B), C49(H49A,H49B)
4.b Aromatic/amide H refined with riding coordinates:
 N16(H16), N16(H16A), C9(H9), C10(H10), C16(H16B), C17(H17), C18(H18),
 C22(H22), C23(H23), N15(H15), N15(H15A), C33(H33), C34(H34), C38(H38),
 C39(H39), C40(H40), C45(H45), C46(H46)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C28(H28A,H28B,H28C), C60(H60A,H60B,
 H60C), C29(H29A,H29B,H29C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,
 H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              40110
_shelx_hkl_checksum              39428
_olex2_submission_special_instructions 'No special instructions were received'