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_1568630
_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 H32 N4 Pd, 2(Cl O4), 2(C2 H3 N)'
_chemical_formula_sum            'C30 H38 Cl2 N6 O8 Pd'
_chemical_formula_weight         787.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-12-18 deposited with the CCDC.	2023-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.1932(5)
_cell_length_b                   11.4548(3)
_cell_length_c                   8.6473(3)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.64
_cell_volume                     1703.04(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            37189
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.074
_diffrn_reflns_theta_min         2.136
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs v2012/1'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.316
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
; 
 Flack x determined using 2196 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.028(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         5494
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0321P)^2^+0.2948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.847
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                5111
_reflns_number_total             5494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00034f2.cif
_cod_data_source_block           l6813
_cod_depositor_comments
'Adding full bibliography for 1568629--1568633.cif.'
_cod_database_code               1568630
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.933
_shelxl_version_number           2013-3
_shelx_res_checksum              30842
_shelx_hkl_checksum              71669