Palladium(II) and platinum(II) complexes of disubstituted imidazo[1,5-<i>a</i>]pyridine and imidazolylpyridine: coordination chemistry, versatile catalysis, and biophysical study.
Rayasingh, Amlan Ranjan; Manivannan, Vadivelu; Dalton transactions (Cambridge, England : 2003) 54 (2025) 7741–7752; doi:10.1039/d5dt00346f

data_7718488
_publ_section_title
;
 Palladium(II) and platinum(II) complexes of disubstituted
 imidazo[1,5-<i>a</i>]pyridine and imidazolylpyridine: coordination
 chemistry, versatile catalysis, and biophysical study.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7741
_journal_page_last               7752
_journal_paper_doi               10.1039/d5dt00346f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C72 H50 N20 Pd3, C18 H12 N5, 3(Cl)'
_chemical_formula_sum            'C90 H62 Cl3 N25 Pd3'
_chemical_formula_weight         1919.19
_chemical_name_systematic        c4
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-10-11 deposited with the CCDC.	2025-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.451(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4490(10)
_cell_length_b                   29.6984(16)
_cell_length_c                   22.8003(15)
_cell_measurement_reflns_used    4783
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.8450
_cell_measurement_theta_min      2.5760
_cell_volume                     11070.6(12)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2760
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -56.00  47.00   1.00   23.52    --  -17.48  19.00-120.00  103
  2  \w    -12.00  61.00   1.00   23.52    --   20.61 -99.00  30.00   73
  3  \w     24.00  62.00   1.00   23.52    --   20.61 -99.00-180.00   38
;
_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      0.0125276000
_diffrn_orient_matrix_UB_12      -0.0173799000
_diffrn_orient_matrix_UB_13      -0.0159952000
_diffrn_orient_matrix_UB_21      0.0193615000
_diffrn_orient_matrix_UB_22      0.0161957000
_diffrn_orient_matrix_UB_23      -0.0130106000
_diffrn_orient_matrix_UB_31      0.0367363000
_diffrn_orient_matrix_UB_32      -0.0026191000
_diffrn_orient_matrix_UB_33      0.0260044000
_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  0.0810
_diffrn_reflns_av_unetI/netI     0.1803
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38453
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.267
_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    0.603
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44312
_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            'metallic dark orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       block
_exptl_crystal_F_000             3864
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1157
_refine_ls_number_reflns         19441
_refine_ls_number_restraints     975
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.1662
_refine_ls_R_factor_gt           0.0804
_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^)+(0.0714P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.2212
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8244
_reflns_number_total             19441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00346f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7718485--7718490.cif.'
_cod_database_code               7718488
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         CHNPdCl
_chemical_oxdiff_usercomment     Mo
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.920
_diffrn_oxdiff_ac4_digest_frames
;
018c50703de6f9585f6ccb0cdbbfffda29002264d1e
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C1-C5 \\sim C1A-C5A
 with sigma of 0.04
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 C1-C3 \\sim C1A-C3A
 with sigma of 0.04
 C6-C2 \\sim C6-C2A
 with sigma of 0.04
 C6-N1 \\sim C6-N1A
 with sigma of 0.04
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 N1-C2 \\sim N1A-C2A
 with sigma of 0.04
 N1-C5 \\sim N1A-C5A
 with sigma of 0.02
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
 C2-C4 \\sim C2A-C4A
 with sigma of 0.04
 N1-C4 \\sim N1A-C4A
 with sigma of 0.04
 C6-C1 \\sim C6-C1A
 with sigma of 0.02
 C1-N1 \\sim C1A-N1A
 with sigma of 0.02
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
3. 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
Uanis(C1A) = Uanis(C1)
4. Others
 Sof(N1A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=
 Sof(H3AA)=Sof(C1A)=1-FVAR(1)
 Sof(N1)=Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3A)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(H5)=FVAR(1)
 Fixed Sof: Cl4(0.5) Cl1(0.5) Cl2(0.5) Cl5(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N19(H19), C2(H2), C3(H3A), C4(H4), C5(H5), C10(H10), C11(H11),
 C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19A),
 C20(H20), C21(H21), C22(H22), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
 C45(H45), C46(H46), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C54(H54),
  C55(H55), C56(H56), C57(H57), C58(H58), C63(H63), C64(H64), C65(H65),
 C66(H66), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
  C76(H76), C81(H81), C82(H82), C83(H83), C84(H84), C87(H87), C88(H88),
 C89(H89), C90(H90), C4A(H4A), C5A(H5A), C2A(H2A), C3A(H3AA)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_original_sample_id c4
_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 1.822
_oxdiff_exptl_absorpt_empirical_full_min 0.582