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_7058495
_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         'C20 H22 N8 Pd'
_chemical_formula_sum            'C20 H22 N8 Pd'
_chemical_formula_weight         480.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_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                88.134(3)
_cell_angle_beta                 80.550(4)
_cell_angle_gamma                76.336(4)
_cell_formula_units_Z            1
_cell_length_a                   5.4343(3)
_cell_length_b                   8.4913(3)
_cell_length_c                   10.9739(5)
_cell_measurement_reflns_used    483
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      26.9690
_cell_measurement_theta_min      3.0870
_cell_volume                     485.36(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      200.00(10)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -25.00   15.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789  -99.0000   30.0000 40

  2 omega  -22.00    3.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789  -99.0000  -90.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1228541000
_diffrn_orient_matrix_UB_12      -0.0020071000
_diffrn_orient_matrix_UB_13      -0.0130365000
_diffrn_orient_matrix_UB_21      -0.0299717000
_diffrn_orient_matrix_UB_22      -0.0333461000
_diffrn_orient_matrix_UB_23      0.0591264000
_diffrn_orient_matrix_UB_31      -0.0504158000
_diffrn_orient_matrix_UB_32      0.0792348000
_diffrn_orient_matrix_UB_33      0.0250109000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3495
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         1.881
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+0.0035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1696
_reflns_number_total             1724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02278c2.cif
_cod_data_source_block           shi_2057_rola
_cod_depositor_comments
'Adding full bibliography for 7058495--7058498.cif.'
_cod_database_code               7058495
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H20 N8 Cl2 Pd1'
_chemical_oxdiff_usercomment     '_2'
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.828
_reflns_odcompleteness_completeness 30.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'