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_7058496
_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         'C18 H18 N8 Pd'
_chemical_formula_sum            'C18 H18 N8 Pd'
_chemical_formula_weight         452.80
_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             2019-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-16 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                71.200(11)
_cell_angle_beta                 86.444(11)
_cell_angle_gamma                76.934(12)
_cell_formula_units_Z            1
_cell_length_a                   4.5732(7)
_cell_length_b                   9.8193(12)
_cell_length_c                   10.5527(13)
_cell_measurement_reflns_used    648
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.7460
_cell_measurement_theta_min      2.0540
_cell_volume                     436.95(11)
_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 0.997
_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    -83.00   3.00   1.00   30.00    --  -15.44 -38.00  30.00   86
  2  \w    -17.00  23.00   1.00   30.00    --  -15.44 -99.00-150.00   40
  3  \w     41.00  85.00   1.00   30.00    --   17.79  77.00-150.00   44
  4  \w      2.00  85.00   1.00   30.00    --   17.79  57.00 -30.00   83
  5  \w     24.00  76.00   1.00   30.00    --   17.79  57.00  30.00   52
  6  \w     35.00  90.00   1.00   30.00    --   17.79 178.00 -90.00   55
;
_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      -0.1523687000
_diffrn_orient_matrix_UB_12      -0.0036513000
_diffrn_orient_matrix_UB_13      -0.0032704000
_diffrn_orient_matrix_UB_21      0.0336508000
_diffrn_orient_matrix_UB_22      -0.0741739000
_diffrn_orient_matrix_UB_23      0.0425990000
_diffrn_orient_matrix_UB_31      -0.0317197000
_diffrn_orient_matrix_UB_32      0.0244637000
_diffrn_orient_matrix_UB_33      0.0567166000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2905
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.039
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91951
_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_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       prism
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0185P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1409
_reflns_number_total             1543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02278c2.cif
_cod_data_source_block           shi_4129_rola
_cod_depositor_comments
'Adding full bibliography for 7058495--7058498.cif.'
_cod_database_code               7058496
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H15N8Pd1
_chemical_oxdiff_usercomment     s-Pd(LEt)2
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.899
_reflns_odcompleteness_completeness 99.33
_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)
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:
 C9(H9A,H9B,H9C)
;
_olex2_date_sample_data_collection 2019-03-04
_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 1.179
_oxdiff_exptl_absorpt_empirical_full_min 0.862