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_7064310
_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         'C38 H28 Cl4 N10 Pd2, 2.5[C3H7NO]'
_chemical_formula_sum            'C45.5 H45.5 Cl4 N12.5 O2.5 Pd2'
_chemical_formula_weight         1162.04
_chemical_name_systematic        2413Pd
_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             2025-06-17
_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                71.220(5)
_cell_angle_beta                 80.398(5)
_cell_angle_gamma                78.127(5)
_cell_formula_units_Z            2
_cell_length_a                   12.611(3)
_cell_length_b                   13.376(3)
_cell_length_c                   14.162(3)
_cell_measurement_reflns_used    9073
_cell_measurement_temperature    299.00
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.20
_cell_volume                     2200.3(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      299.00
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            63247
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.975
_diffrn_reflns_theta_min         1.528
_diffrn_source                   'X-ray Tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1100 before and 0.0533 after correction.
The Ratio of minimum to maximum transmission is 0.8607.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         11528
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0413P)^2^+2.9210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9626
_reflns_number_total             11528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj04746c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7064300--7064310.cif.'
_cod_original_cell_volume        2200.3(8)
_cod_original_formula_sum        'C45.50 H45.50 Cl4 N12.50 O2.50 Pd2'
_cod_database_code               7064310
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.877
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 C26-N7 \\sim C26-N7A
 with sigma of 0.02
 C6-N2 \\sim C6-N2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N7) = Uanis(N7A)
Uanis(N2) = Uanis(N2A) = Uanis(N7A) = Uanis(N7)
4. Others
 Sof(N7A)=Sof(H7AA)=Sof(H7AB)=1-FVAR(1)
 Sof(N7)=Sof(H7A)=Sof(H7B)=FVAR(1)
 Sof(N2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(2)
 Sof(N2)=Sof(H2A)=Sof(H2B)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C38(H38), C9(H9), C12(H12), C31(H31), C10(H10), C11(H11), C20(H20), C37(H37),
 C1(H1), C29(H29), C16(H16), C4(H4), C2(H2), C19(H19), C23(H23), C3(H3),
 C35(H35), C28(H28), C18(H18), C21(H21), C30(H30), C36(H36), C17(H17), C22(H22)
5.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N7(H7A,H7B), N7A(H7AA,H7AB), N2A(H2AA,H2AB)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34191
_shelx_fab_checksum              41107
_olex2_submission_special_instructions 'No special instructions were received'