A Palladium(II) Center Activates Nitrile Ligands toward 1,3-Dipolar Cycloaddition of Nitrones Substantially More than the Corresponding Platinum(II) Center
Andreii S. Kritchenkov; Nadezhda A. Bokach; Galina L. Starova; Vadim Yu. Kukushkin; Inorganic Chemistry 51 (2012) 11971–11979; doi:10.1021/ic301866y

data_4330959
_publ_section_title
;
 A Palladium(II) Center Activates Nitrile Ligands toward 1,3-Dipolar
 Cycloaddition of Nitrones Substantially More than the Corresponding
 Platinum(II) Center
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11971
_journal_page_last               11979
_journal_paper_doi               10.1021/ic301866y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C23 H22 Cl N2 O Pd0.5'
_chemical_formula_weight         431.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.089(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4926(16)
_cell_length_b                   11.5375(11)
_cell_length_c                   11.8489(12)
_cell_measurement_reflns_used    2520
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.28
_cell_measurement_theta_min      2.54
_cell_volume                     1989.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker Kappa APEX-II Duo CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1441
_diffrn_reflns_av_sigmaI/netI    0.1761
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19451
_diffrn_reflns_theta_full        30.31
_diffrn_reflns_theta_max         30.31
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.4410
_exptl_absorpt_correction_T_min  0.2642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS;_Bruker,_2007
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       lamina
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.661
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.0018(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5847
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0295P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                3178
_reflns_number_total             5847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301866y_si_002.cif
_cod_data_source_block           7b
_cod_original_formula_sum        'C23 H22 Cl N2 O Pd0.50'
_cod_database_code               4330959