Synthesis and Structure of Pd(II) Pincer Complexes: Catalytic Application to β-Alkylation of Secondary Alcohols Involving Sequential Dehydrogenation of Alcohols via Borrowing Hydrogen Approach
Sekar, Pranesh Kavin; Rengan, Ramesh; Dalton Transactions  (2023) –; doi:10.1039/D3DT01628E

data_7713238
_publ_section_title
;
 Synthesis and Structure of Pd(II) Pincer Complexes: Catalytic Application
 to \b-Alkylation of Secondary Alcohols Involving Sequential
 Dehydrogenation of Alcohols via Borrowing Hydrogen Approach
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01628E
_journal_year                    2023
_chemical_formula_moiety         'C37 H36 N3 O3 P Pd'
_chemical_formula_sum            'C37 H36 N3 O3 P Pd'
_chemical_formula_weight         708.06
_chemical_name_common            Inorganic
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-19 deposited with the CCDC.	2023-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.9295(12)
_cell_length_b                   52.455(3)
_cell_length_c                   10.7669(6)
_cell_measurement_reflns_used    9667
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.6953
_cell_measurement_theta_min      2.3042
_cell_volume                     13514.8(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Apex3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 924)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 Quest XRD'
_diffrn_measurement_method       'Omega and Phi Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       72
_diffrn_reflns_limit_k_min       -73
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            74297
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.093
_diffrn_reflns_theta_min         2.110
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5530
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5824
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Flack x determined using 2997 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         9273
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1267
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                7481
_reflns_number_total             9273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01628e2.cif
_cod_data_source_block           BDU_DrRR_PdSP1OMe_01072022_0ma
_cod_original_cell_volume        13514.7(12)
_cod_database_code               7713238
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.845
_shelx_estimated_absorpt_t_max   0.909
_shelx_res_checksum              92327