New palladium(ii) complexes with 3-(2-pyridyl)-5-alkyl-1,2,4-triazole ligands as recyclable C‒C coupling catalysts
Zakharchenko, Borys V.; Khomenko, Dmytro M.; Doroshchuk, Roman O.; Raspertova, Ilona V.; Starova, Viktoriia S.; Trachevsky, Volodymyr V.; Shova, Sergiu; Severynovska, Olga V.; Martins, Luísa M. D. R. S.; Pombeiro, Armando J. L.; Arion, Vladimir B.; Lampeka, Rostyslav D.; New Journal of Chemistry 43 (2019) 10973–; doi:10.1039/C9NJ02278C

data_7058497
_publ_section_title
;
 New palladium(ii) complexes with 3-(2-pyridyl)-5-alkyl-1,2,4-triazole
 ligands as recyclable C--C coupling catalysts
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10973
_journal_paper_doi               10.1039/C9NJ02278C
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         '3(C22 H26 N8 Pd), 2(C H Cl3), H4 O2'
_chemical_formula_sum            'C68 H84 Cl6 N24 O2 Pd3'
_chemical_formula_weight         1801.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-29 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.80(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   30.046(8)
_cell_length_b                   6.8662(12)
_cell_length_c                   23.785(6)
_cell_measurement_reflns_used    1627
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.9650
_cell_measurement_theta_min      1.7520
_cell_volume                     3929(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -41.00  23.00   1.00   30.00    --   26.04 -38.00  90.00   64
  2  \w     40.00  95.00   1.00   30.00    --   26.04  38.00 -90.00   55
  3  \w    -27.00  36.00   1.00   30.00    --   26.04 -57.00-180.00   63
  4  \w    -96.00 -39.00   1.00   30.00    --  -23.85-178.00 -30.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0028073000
_diffrn_orient_matrix_UB_12      -0.0734265000
_diffrn_orient_matrix_UB_13      0.0186359000
_diffrn_orient_matrix_UB_21      -0.0221944000
_diffrn_orient_matrix_UB_22      -0.0421456000
_diffrn_orient_matrix_UB_23      -0.0322859000
_diffrn_orient_matrix_UB_31      0.0192820000
_diffrn_orient_matrix_UB_32      -0.0591997000
_diffrn_orient_matrix_UB_33      -0.0002068000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.1462
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7696
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.693
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.231
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0010P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2353
_reflns_number_total             3784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02278c2.cif
_cod_data_source_block           shi_3790_rola
_cod_depositor_comments
'Adding full bibliography for 7058495--7058498.cif.'
_cod_original_cell_volume        3929(2)
_cod_database_code               7058497
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20N6O2Pd1
_chemical_oxdiff_usercomment     s-Pd(Lt-but)2(cryst)
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.834
_reflns_odcompleteness_completeness 99.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H9AA(0.5) H9AB(0.5) H9AC(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) H1WA(0.5)
3.a Riding coordinates:
 C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C19A(H19A,H19B,H19C), C20A(H20A,
 H20B,H20C), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), O1W(H1WA,H1WB)
3.b Ternary CH refined with riding coordinates:
 C1(H1)
3.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C11A(H11A), C12A(H12A), C13A(H13A),
 C14A(H14A), C1B(H1B), C2B(H2B), C3B(H3B), C4B(H4B)
;
_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 1.102
_oxdiff_exptl_absorpt_empirical_full_min 0.922