A sustainable strategic approach for <i>N</i>-alkylation of amines with activation of alcohols triggered <i>via</i> a hydrogen auto-transfer reaction using a Pd(II) complex: evidence for metal-ligand cooperativity.
Kumar Chaudhary, Virendra; Kukreti, Prashant; Sharma, Keshav; Kumar, Kapil; Singh, Sain; Kumari, Sheela; Ghosh, Kaushik; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8740–8749; doi:10.1039/d4dt00864b

data_7715806
_publ_section_title
;
 A sustainable strategic approach for <i>N</i>-alkylation of amines with
 activation of alcohols triggered <i>via</i> a hydrogen auto-transfer
 reaction using a Pd(II) complex: evidence for metal-ligand cooperativity.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8740
_journal_page_last               8749
_journal_paper_doi               10.1039/d4dt00864b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C24 H18 Cl N5 Pd'
_chemical_formula_sum            'C24 H18 Cl N5 Pd'
_chemical_formula_weight         518.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-09-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-03-23 deposited with the CCDC.	2024-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                73.308(4)
_cell_angle_beta                 73.136(4)
_cell_angle_gamma                88.997(4)
_cell_formula_units_Z            2
_cell_length_a                   8.8728(9)
_cell_length_b                   10.6090(11)
_cell_length_c                   12.3959(14)
_cell_measurement_reflns_used    111
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.383
_cell_measurement_theta_min      1.14
_cell_volume                     1066.9(2)
_computing_cell_refinement       'Bruker Kappa Apex'
_computing_data_collection       'Bruker Kappa Apex'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Kappa Apex'
_diffrn_measurement_method       'phi omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17989
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.383
_diffrn_reflns_theta_min         3.007
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            'clear dark gray'
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520.0
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_transmission_factor_max   0.967
_exptl_transmission_factor_min   0.437
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0187
_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^)+(0.0170P)^2^+0.4681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4995
_reflns_number_total             5361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00864b2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7715806.cif.'
_cod_database_code               7715806
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24)
;
_shelx_res_checksum              19432
_olex2_submission_special_instructions 'No special instructions were received'