An NNN Pd(II) pincer complex with 1,1-diaminoazine: a versatile catalyst for acceptorless dehydrogenative coupling reactions.
Wani, Aabid A.; Bhujbal, Shivkanya Madhavrao; Sherpa, Deekey; Kathuria, Deepika; Chourasiya, Sumit S.; Sahoo, Subash C.; Bharatam, Prasad V.; Organic & biomolecular chemistry 23 (2025) 343–351; doi:10.1039/d4ob01576b

data_7160203
_publ_section_title
;
 An NNN Pd(II) pincer complex with 1,1-diaminoazine: a versatile catalyst
 for acceptorless dehydrogenative coupling reactions.
;
_journal_issue                   2
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              343
_journal_page_last               351
_journal_paper_doi               10.1039/d4ob01576b
_journal_volume                  23
_journal_year                    2025
_chemical_compound_source        synthesized
_chemical_formula_moiety         '2(C29 H22 N2)'
_chemical_formula_sum            'C58 H44 N4'
_chemical_formula_weight         796.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-31
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-05 deposited with the CCDC.	2024-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5849(5)
_cell_length_b                   17.0570(7)
_cell_length_c                   26.1460(17)
_cell_measurement_reflns_used    11610
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.1600
_cell_measurement_theta_min      3.5310
_cell_volume                     4274.6(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.1062
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22670
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.197
_diffrn_source                   'sealed tube x-ray'
_diffrn_source_type              'supernova Mo'
_exptl_absorpt_coefficient_mu    0.072
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 1064 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.6(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         8007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.1614
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0796P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1779
_reflns_Friedel_coverage         0.655
_reflns_Friedel_fraction_full    0.844
_reflns_Friedel_fraction_max     0.822
_reflns_number_gt                3569
_reflns_number_total             8007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01576b2.cif
_cod_data_source_block           PVB-MD-55
_cod_depositor_comments          'Adding full bibliography for 7160203.cif.'
_cod_database_code               7160203
_shelx_shelxl_version_number     2017/1
_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:
 C19(H19A,H19B), C48(H48A,H48B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C21(H21), C10(H10), C28(H28), C52(H52), C50(H50), C9(H9), C51(H51),
 C16(H16), C6(H6), C38(H38), C22(H22), C33(H33), C4(H4), C25(H25), C23(H23),
 C14(H14), C8(H8), C31(H31), C32(H32), C15(H15), C57(H57), C45(H45), C43(H43),
 C5(H5), C27(H27), C56(H56), C26(H26), C37(H37), C36(H36), C35(H35), C44(H44),
 C54(H54), C55(H55)
2.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              18626
_olex2_submission_special_instructions 'No special instructions were received'