Hydroxy- and Mercaptopyridine Pincer Platinum and Palladium Complexes Generated by Silver-Free Halide Abstraction
Chuchuryukin, Alexey V.; Chase, Preston A.; Mills, Allison M.; Lutz, Martin; Spek, Anthony L.; van Klink, Gerard P. M.; van Koten, Gerard; Inorganic Chemistry 45 (2006) 2045–2054; doi:10.1021/ic051773x

data_4331884
_publ_section_title
;
 Hydroxy- and Mercaptopyridine Pincer Platinum and Palladium Complexes
 Generated by Silver-Free Halide Abstraction
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2045
_journal_page_last               2054
_journal_paper_doi               10.1021/ic051773x
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C17 H23 N3 O Pd, 2.5(H2 O)'
_chemical_formula_sum            'C17 H28 N3 O3.5 Pd'
_chemical_formula_weight         436.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.786(5)
_cell_angle_beta                 87.660(4)
_cell_angle_gamma                88.475(4)
_cell_formula_units_Z            4
_cell_length_a                   8.9685(4)
_cell_length_b                   10.3356(6)
_cell_length_c                   20.2901(11)
_cell_measurement_reflns_used    181
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      3.64
_cell_volume                     1873.61(17)
_computing_cell_refinement       DirAX
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD. Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-97 (Beurskens et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40141
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8598
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0202
_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^)+(0.0210P)^2^+1.5174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0491
_reflns_number_gt                7491
_reflns_number_total             8598
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic051773xsup1.cif
_cod_data_source_block           s2919a
_cod_original_formula_sum        'C17 H28 N3 O3.50 Pd'
_cod_database_code               4331884