Palladium(II) Complexes of Readily Functionalized Bidentate 2-Pyridyl-1,2,3-triazole "Click" Ligands: A Synthetic, Structural, Spectroscopic, and Computational Study
Kelly J. Kilpin; Emma L. Gavey; C. John McAdam; Christopher B. Anderson; Samuel J. Lind; Courtney C. Keep; Keith C. Gordon; James D. Crowley; Inorganic Chemistry 50 (2011) 6334–6346; doi:10.1021/ic200789b

data_4325555
_publ_section_title
;
 Palladium(II) Complexes of Readily Functionalized Bidentate
 2-Pyridyl-1,2,3-triazole "Click" Ligands: A Synthetic, Structural,
 Spectroscopic, and Computational Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6334
_journal_page_last               6346
_journal_paper_doi               10.1021/ic200789b
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C46 H56 N8 O20 Pd, 2(B F4), 3.5(C2 H3 N)'
_chemical_formula_sum            'C53 H66.5 B2 F8 N11.5 O20 Pd'
_chemical_formula_weight         1464.70
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.852(12)
_cell_angle_beta                 96.818(12)
_cell_angle_gamma                104.357(11)
_cell_formula_units_Z            1
_cell_length_a                   8.111(3)
_cell_length_b                   8.746(3)
_cell_length_c                   24.179(8)
_cell_measurement_reflns_used    3857
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      17.20
_cell_measurement_theta_min      2.55
_cell_volume                     1648.2(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      91(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.1022
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20759
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.8170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       plate
_exptl_crystal_F_000             753
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.927
_refine_diff_density_min         -1.623
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         9985
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0996P)^2^+0.4339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1692
_reflns_number_gt                8406
_reflns_number_total             9985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200789b_si_001_12.cif
_cod_data_source_block           820918
_cod_original_cell_volume        1648.2(9)
_cod_original_formula_sum        'C53 H66.50 B2 F8 N11.50 O20 Pd'
_cod_database_code               4325555