Group 10 complexes of benzothiazolehydrazone- and imidazo[1,5-<i>a</i>]pyridine-based ligands: structural artistry, biophysical study, and catalytic activity.
Rayasingh, Amlan Ranjan; Manivannan, Vadivelu; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16939–16954; doi:10.1039/d5dt02077h

data_7719708
_publ_section_title
;
 Group 10 complexes of benzothiazolehydrazone- and
 imidazo[1,5-<i>a</i>]pyridine-based ligands: structural artistry,
 biophysical study, and catalytic activity.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16939
_journal_page_last               16954
_journal_paper_doi               10.1039/d5dt02077h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C26 H19 Cl N3 P Pd S, [+ solvents]'
_chemical_formula_sum            'C26 H19 Cl N3 P Pd S'
_chemical_formula_weight         578.32
_chemical_name_systematic        151-2Pd
_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             2025-04-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2025-05-22 deposited with the CCDC.	2025-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                95.326(7)
_cell_angle_beta                 98.449(10)
_cell_angle_gamma                94.143(8)
_cell_formula_units_Z            2
_cell_length_a                   9.3817(13)
_cell_length_b                   9.4039(7)
_cell_length_c                   13.3104(15)
_cell_measurement_reflns_used    1746
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.9650
_cell_measurement_theta_min      2.8710
_cell_volume                     1152.1(2)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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    -90.00  19.00   1.00   16.25    --  -17.48 -19.00 -90.00  109
  2  \w    -88.00  13.00   1.00   16.25    --  -17.48 -77.00  90.00  101
  3  \w    -25.00   0.00   1.00   16.25    --  -17.48 -57.00-150.00   25
  4  \w    -43.00  45.00   1.00   16.25    --  -17.48  77.00-150.00   88
  5  \w     19.00  63.00   1.00   16.25    --   20.61 -99.00   0.00   44
;
_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      -0.0604990000
_diffrn_orient_matrix_UB_12      -0.0409626000
_diffrn_orient_matrix_UB_13      0.0120804000
_diffrn_orient_matrix_UB_21      -0.0461641000
_diffrn_orient_matrix_UB_22      0.0307268000
_diffrn_orient_matrix_UB_23      -0.0376261000
_diffrn_orient_matrix_UB_31      0.0098000000
_diffrn_orient_matrix_UB_32      -0.0562175000
_diffrn_orient_matrix_UB_33      -0.0370519000
_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  0.0761
_diffrn_reflns_av_unetI/netI     0.1203
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7147
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.493
_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    1.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75692
_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 brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_preparation       'slow evaporation'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.325
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4022
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0367P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2878
_reflns_number_total             4022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02077h2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7719702--7719718.cif.'
_cod_database_code               7719708
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         CHNOPdPCl
_chemical_oxdiff_usercomment     Mo
_diffrn_oxdiff_ac4_digest_frames
;
0131c66b102a0aee348342f49c156abad90038516ed
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C5-C20
 1.39 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C1(H1), C19(H19), C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10),
 C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C8(H8), C22(H22), C23(H23),
 C24(H24), C25(H25)
;
_olex2_submission_original_sample_id 151-2pd
_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 1.489
_oxdiff_exptl_absorpt_empirical_full_min 0.623