Dinuclear palladium(ii) complexes of N-(imidazo[1,5-a]pyridin-1-yl)picolinimidamides: highly active catalysts for C–C and C–P bond formation
Rayasingh, Amlan Ranjan; Manivannan, Vadivelu; New Journal of Chemistry 50 (2026) 5541–5550; doi:10.1039/D5NJ04746C

data_7064304
_publ_section_title
;
 Dinuclear palladium(ii) complexes of
 N-(imidazo[1,5-a]pyridin-1-yl)picolinimidamides: highly active catalysts
 for C--C and C--P bond formation
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5541
_journal_page_last               5550
_journal_paper_doi               10.1039/D5NJ04746C
_journal_volume                  50
_journal_year                    2026
_chemical_formula_moiety         'C19 H14 Br N5'
_chemical_formula_sum            'C19 H14 Br N5'
_chemical_formula_weight         392.26
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-09-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-10-16 deposited with the CCDC.	2026-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                75.582(10)
_cell_angle_beta                 74.358(8)
_cell_angle_gamma                87.772(7)
_cell_formula_units_Z            2
_cell_length_a                   6.7421(5)
_cell_length_b                   11.0790(13)
_cell_length_c                   12.2068(15)
_cell_measurement_reflns_used    1359
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.8830
_cell_measurement_theta_min      2.9270
_cell_volume                     849.98(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2760
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  19.00   1.00   12.12    --  -17.33 -99.00 -90.00   39
  2  \w    -11.00  24.00   1.00   12.12    --  -17.33 -99.00  90.00   35
  3  \w     43.00  85.00   1.00   12.12    --   20.92-178.00   0.00   42
  4  \w    -36.00  39.00   1.00   12.12    --   20.92 -57.00-180.00   75
  5  \w     -5.00  89.00   1.00   12.12    --   20.92  38.00 120.00   94
  6  \w    -49.00  45.00   1.00   12.12    --   20.92 -38.00 -60.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0022882000
_diffrn_orient_matrix_UB_12      -0.0277417000
_diffrn_orient_matrix_UB_13      -0.0467829000
_diffrn_orient_matrix_UB_21      -0.0018523000
_diffrn_orient_matrix_UB_22      0.0599262000
_diffrn_orient_matrix_UB_23      -0.0377096000
_diffrn_orient_matrix_UB_31      0.1092616000
_diffrn_orient_matrix_UB_32      0.0036016000
_diffrn_orient_matrix_UB_33      -0.0163953000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.1271
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5226
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.139
_diffrn_reflns_theta_max         25.139
_diffrn_reflns_theta_min         2.263
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0732
_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^)+(0.0888P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.2051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1607
_reflns_number_total             2935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj04746c2.cif
_cod_data_source_block           L5H
_cod_depositor_comments
'Adding full bibliography for 7064300--7064310.cif.'
_cod_database_code               7064304
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNBr
_chemical_oxdiff_usercomment     Mo
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.727
_diffrn_oxdiff_ac4_digest_frames
;
010df86aeb1737700cb713c7fba9d988f2003976922
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C19(H19), C9(H9), C18(H18), C16(H16), C2(H2), C4(H4), C12(H12),
 C3(H3), C10(H10), C1(H1), C11(H11)
2.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_shelx_res_checksum              21695
_olex2_date_sample_data_collection 2023-03-17
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.748
_oxdiff_exptl_absorpt_empirical_full_min 0.140