C-H bond activation <i>via</i> concerted metalation-deprotonation at a palladium(iii) center.
Bouley, Bailey S.; Tang, Fengzhi; Bae, Dae Young; Mirica, Liviu M.; Chemical science 14 (2023) 3800–3808; doi:10.1039/d3sc00034f

data_1568633
_publ_section_title
;
 C-H bond activation <i>via</i> concerted metalation-deprotonation at a
 palladium(iii) center.
;
_journal_issue                   14
_journal_name_full               'Chemical science'
_journal_page_first              3800
_journal_page_last               3808
_journal_paper_doi               10.1039/d3sc00034f
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C26 H33 Cl N4 Pd'
_chemical_formula_sum            'C26 H33 Cl N4 Pd'
_chemical_formula_weight         543.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-18 deposited with the CCDC.	2023-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.69
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7777(2)
_cell_length_b                   30.6361(6)
_cell_length_c                   9.7205(2)
_cell_measurement_reflns_used    56458
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.284
_cell_measurement_theta_min      2.534
_cell_volume                     2393.71(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            81975
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.295
_diffrn_reflns_theta_min         2.383
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0785 before and 0.0430 after correction.
The Ratio of minimum to maximum transmission is 0.9338.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       Block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0178
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+1.6900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0435
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5769
_reflns_number_total             5949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00034f2.cif
_cod_data_source_block           men4pdneophylcl
_cod_depositor_comments
'Adding full bibliography for 1568629--1568633.cif.'
_cod_original_cell_volume        2393.64(9)
_cod_database_code               1568633
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.822
_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.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C8(H8A,H8B), C16(H16A,H16B), C14(H14A,H14B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C12(H12), C2(H2), C3(H3), C26(H26), C24(H24), C10(H10), C25(H25),
 C22(H22), C23(H23), C11(H11)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              74183
_shelx_hkl_checksum              33109
_olex2_submission_special_instructions 'No special instructions were received'