Mild and selective Pd-Ar protonolysis and C-H activation promoted by a ligand aryloxide group.
Behnia, Ava; Fard, Mahmood A.; Blacquiere, Johanna M.; Puddephatt, Richard J.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3538–3548; doi:10.1039/c8dt00437d

data_7045635
_publ_section_title
;
 Mild and selective Pd-Ar protonolysis and C-H activation promoted by a
 ligand aryloxide group.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3538
_journal_page_last               3548
_journal_paper_doi               10.1039/c8dt00437d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C28 H28 N2 O Pd'
_chemical_formula_weight         514.92
_chemical_name_systematic
'[Pd(C6H4(2-t-Bu))(\k3-N,N',O-OC6H4N=CH(2-C5H4N))]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-12-15 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.146(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.509(4)
_cell_length_b                   9.397(4)
_cell_length_c                   14.443(7)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    110
_cell_measurement_theta_max      32.59
_cell_measurement_theta_min      2.59
_cell_volume                     1154.6(9)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  SHELXL-2014
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Bruker Apex2'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Axis Apex2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24450
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.249
_diffrn_reflns_theta_max         24.249
_diffrn_reflns_theta_min         3.230
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3724
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0583P)^2^+1.8042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0948
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3471
_reflns_number_total             3724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00437d2.cif
_cod_data_source_block           b17133
_cod_depositor_comments
'Adding full bibliography for 7045635--7045637.cif.'
_cod_database_code               7045635
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              62649