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_7064307
_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
'0.091(C40 H34 Cl2 N10 Pd2), 0.182(F6 P), 0.273(C3 H7 N O), 0.1[C3H7NO]'
_chemical_formula_sum
'C4.45 H5 Cl0.18 F1.09 N1.18 O0.27 P0.18 Pd0.18'
_chemical_formula_weight         131.65
_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             2025-09-22
_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                74.945(4)
_cell_angle_beta                 75.354(4)
_cell_angle_gamma                74.117(4)
_cell_formula_units_Z            22
_cell_length_a                   11.5271(16)
_cell_length_b                   16.201(2)
_cell_length_c                   19.385(3)
_cell_measurement_reflns_used    9713
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.34
_cell_volume                     3297.4(8)
_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      298.00
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  CMOS-PHOTONII-7
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            86769
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.106
_diffrn_reflns_theta_min         2.044
_diffrn_source                   'X-ray Tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0939 before and 0.0597 after correction.
The Ratio of minimum to maximum transmission is 0.9097.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.938
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         14424
_refine_ls_number_restraints     1174
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0832P)^2^+8.9896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11477
_reflns_number_total             14424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj04746c2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7064300--7064310.cif.'
_cod_original_cell_volume        3297.5(8)
_cod_database_code               7064307
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.870
_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 Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C2(H2), C1(H1), C24(H24), C23(H23), C22(H22), C21(H21),
 C29(H29), C30(H30), C31(H31), C32(H32), C39(H39), C38(H38), C36(H36), C35(H35),
  C9(H9), C10(H10), C11(H11), C12(H12), C20(H20), C19(H19), C16(H16), C15(H15),
 C50(H50), C51(H51), C56(H56)
4.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N7(H7A,H7B)
4.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C18(H18A,H18B,H18C), C52(H52A,H52B,H52C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C58(H58A,
 H58B,H58C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              33119
_shelx_fab_checksum              50404
_olex2_submission_special_instructions 'No special instructions were received'