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_7058498
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 92.15(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.4346(9)
_cell_length_b                   10.181(4)
_cell_length_c                   21.341(7)
_cell_measurement_reflns_used    289
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.8540
_cell_measurement_theta_min      4.5960
_cell_volume                     962.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'SIR2008 (Burla et al.,  2007)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.885
_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    -19.00  21.00   1.00   30.00    --  -15.60 -99.00   0.00   40
  2  \w    -82.00 -25.00   1.00   30.00    --  -15.60 -77.00 120.00   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      -0.0117488000
_diffrn_orient_matrix_UB_12      -0.0574365000
_diffrn_orient_matrix_UB_13      -0.0186862000
_diffrn_orient_matrix_UB_21      -0.1504546000
_diffrn_orient_matrix_UB_22      -0.0091610000
_diffrn_orient_matrix_UB_23      0.0093101000
_diffrn_orient_matrix_UB_31      -0.0533290000
_diffrn_orient_matrix_UB_32      0.0383499000
_diffrn_orient_matrix_UB_33      -0.0258907000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1108
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            2623
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.499
_diffrn_reflns_theta_min         2.217
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.659
_exptl_crystal_description       needle
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.269
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0838P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1804
_reflns_number_total             2623
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9079\% 
 around [0.98 0.00 -0.19] (reciprocal) or [1.00 0.00 -0.00] (direct)
;
_cod_data_source_file            c9nj02278c2.cif
_cod_data_source_block           shi_4015_rola_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7058495--7058498.cif.'
_cod_original_cell_volume        962.9(5)
_cod_database_code               7058498
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20N6Pd1
_chemical_oxdiff_usercomment     s-Pd(Liso)2
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.756
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.655(2)
 0.345(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C8(H8)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_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 1.509
_oxdiff_exptl_absorpt_empirical_full_min 0.650
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2