Unusual coordination of a 1,2,3-triazolyl-pyridine ligand in a Pd(ii) complex: application in the Suzuki–Miyaura coupling reaction
Gahlaut, Puneet Singh; Gautam, Deepak; Lama, Prem; Jana, Barun; New Journal of Chemistry 47 (2023) 6871–6879; doi:10.1039/D3NJ00206C

data_7062360
_publ_section_title
;
 Unusual coordination of a 1,2,3-triazolyl-pyridine ligand in a Pd(ii)
 complex: application in the Suzuki--Miyaura coupling reaction
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6871
_journal_page_last               6879
_journal_paper_doi               10.1039/D3NJ00206C
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C24 H18 Cl2 N8 O4 Pd'
_chemical_formula_sum            'C24 H18 Cl2 N8 O4 Pd'
_chemical_formula_weight         659.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-02-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-04 deposited with the CCDC.	2023-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.345(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5199(13)
_cell_length_b                   20.926(2)
_cell_length_c                   13.1275(13)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.25
_cell_volume                     2967.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-III photon detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            40118
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         1.920
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       ractangular
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   0.7453
_exptl_transmission_factor_min   0.6858
_refine_diff_density_max         1.253
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+4.9349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4855
_reflns_number_total             5430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00206c2.cif
_cod_data_source_block           23feba_sq
_cod_depositor_comments          'Adding full bibliography for 7062360.cif.'
_cod_database_code               7062360
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.761
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2) = Uanis(C6)
Uanis(C16A) = Uanis(C16B)
2. Others
 Sof(O1B)=Sof(O3B)=Sof(C7B)=Sof(C16B)=1-FVAR(1)
 Sof(O1A)=Sof(O3A)=Sof(C7A)=Sof(C16A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C17(H17A,H17B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4A), C5(H5), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              81919
_shelx_fab_checksum              46575
_olex2_submission_special_instructions 'No special instructions were received'