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_7064309
_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         '2(C40 H34 Cl2 N10 O2 Pd2), 3.75[C3H7NO]'
_chemical_formula_sum            'C91.25 H94.25 Cl4 N23.75 O7.75 Pd4'
_chemical_formula_weight         2215.05
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-15
_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                68.860(4)
_cell_angle_beta                 78.938(4)
_cell_angle_gamma                88.158(4)
_cell_formula_units_Z            2
_cell_length_a                   14.662(2)
_cell_length_b                   17.696(2)
_cell_length_c                   19.747(3)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    293.00
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.25
_cell_volume                     4686.1(11)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.00
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0836
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            100506
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.841
_diffrn_source                   'X-ray Tube'
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_target            Mo
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1550 before and 0.0765 after correction.
The Ratio of minimum to maximum transmission is 0.8969.
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    1.570
_exptl_crystal_description       plate
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.192
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1016
_refine_ls_number_reflns         16081
_refine_ls_number_restraints     1688
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1616
_refine_ls_R_factor_gt           0.0897
_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^)+(0.1369P)^2^+42.0620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2205
_refine_ls_wR_factor_ref         0.3133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8790
_reflns_number_total             16081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj04746c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7064300--7064310.cif.'
_cod_database_code               7064309
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.857
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Rotating group:
 N15(H15A,H15B), N20(H20A,H20B), N7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C49(H49), C12(H12), C69(H69), C41(H41), C48(H48), C53(H53), C51(H51),
 C29(H29), C50(H50), C35(H35), C9(H9), C44(H44), C70(H70), C32(H32), C11(H11),
 C67(H67), C43(H43), C76(H76), C54(H54), C30(H30), C68(H68), C78(H78), C42(H42),
  C56(H56), C77(H77), C31(H31), C36(H36), C64(H64), C1(H1), C38(H38), C15(H15),
 C75(H75), C4(H4), C24(H24), C55(H55), C18(H18), C37(H37), C2(H2), C10(H10),
 C61(H61), C21(H21), C63(H63), C22(H22), C3(H3), C62(H62), C17(H17), C23(H23),
 C16(H16)
4.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C58(H58A,H58B,H58C), C40(H40A,H40B,H40C), C20(H20C,H20D,
 H20E)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 315 electrons were 
found in a volume of 1212\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3.75[C3H7NO] per Formula Unit 
which account for 300 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              26300
_shelx_fab_checksum              40645
_olex2_submission_special_instructions 'No special instructions were received'