Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global # *** Added by check_cif _journal_coden_Cambridge 186 loop_ _publ_author_name 'Van Eldik, R.' 'Bugarcic, Zivandin D.' 'Liehr, Gunter' _publ_contact_author_name 'Prof R Van Eldik' _publ_contact_author_address ; Institute for Inorganic Chemistry University of Erlangen-Nurnberg Egerlandstr. 1 Erlangen 91058 GERMANY ; _publ_contact_author_email vaneldik@chemie.uni-erlangen.de _publ_contact_author_fax +49-9131-8527387 _publ_contact_author_phone +49-9131-8527350 _publ_requested_journal 'Dalton' _publ_requested_category CM # ---------------------------------------- # 2. TITLE AND AUTHOR LIST # ---------------------------------------- _publ_contact_letter # Include date of submission ; Date of submission ? Please consider this CIF submission for publication as a Paper in Dalton ; _publ_section_title ; Kinetics and mechanism of the reaction of chelated Pd(II) complexes with thiols in acidic aqueous solution. Synthesis and crystal structure of [Pd(bpma)Cl]Cl.H2O (bpma = bis(2-pyridylmethyl)amine) ; data_zivatt _database_code_CSD 173337 # ---------------------------------------- # 3. CHEMICAL DATA # ---------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H13 Cl2 N3 O Pd' _chemical_formula_weight 392.55 # ---------------------------------------- # 4. CYSTAL DATA # ---------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1' #(No. 2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.039(5) _cell_length_b 8.534(5) _cell_length_c 12.831(5) _cell_angle_alpha 106.52(2) _cell_angle_beta 102.56(2) _cell_angle_gamma 91.46(2) _cell_volume 718.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 14.8 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max .43 _exptl_crystal_size_mid .06 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 1.658 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min .85 _exptl_absorpt_correction_T_max .90 _exptl_special_details ; ? ; # ---------------------------------------- # 5. EXPERIMENTAL DATA # ---------------------------------------- _diffrn_ambient_temperature 190 _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device Cad4 _diffrn_measurement_method w/2The _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 6110 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.1017 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.03 _reflns_number_total 2854 _reflns_number_gt 2043 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PWCH (Gomm, 1993)' _computing_cell_refinement 'PWCH (Gomm, 1993)' _computing_data_reduction 'Inread (Liehr, 1992)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLUTON (Spek, 1998)' _computing_molecular_graphics ? _computing_publication_material ? # ---------------------------------------- # 6. REFINEMENT DATA # ---------------------------------------- _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2854 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 0.853 _refine_ls_restrained_S_all 0.853 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # ---------------------------------------- # 7. ATOMIC COORDINATES and ADP # ---------------------------------------- loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.18415(8) 0.47738(7) 0.91560(5) 0.01938(19) Uani 1 d . . . Cl1 Cl 0.2231(3) 0.2662(2) 0.99507(16) 0.0282(4) Uani 1 d . . . N1 N 0.1724(10) 0.6554(8) 0.8413(5) 0.0274(14) Uani 1 d . . . N2 N 0.0361(9) 0.3416(8) 0.7630(5) 0.0243(14) Uani 1 d . . . N3 N 0.3092(8) 0.6596(7) 1.0541(5) 0.0187(12) Uani 1 d . . . C1 C -0.0085(12) 0.6156(9) 0.7494(7) 0.0300(18) Uani 1 d . . . H1A H 0.0041 0.6705 0.6943 0.036 Uiso 1 calc R . . H1B H -0.1200 0.6535 0.7793 0.036 Uiso 1 calc R . . C2 C -0.0393(10) 0.4306(10) 0.6950(6) 0.0271(17) Uani 1 d . . . C3 C -0.1406(12) 0.3582(11) 0.5855(7) 0.037(2) Uani 1 d . . . H3 H -0.1860 0.4221 0.5391 0.044 Uiso 1 calc R . . C4 C -0.1723(12) 0.1917(12) 0.5470(7) 0.041(2) Uani 1 d . . . H4 H -0.2455 0.1416 0.4746 0.049 Uiso 1 calc R . . C5 C -0.0968(12) 0.0963(11) 0.6142(7) 0.040(2) Uani 1 d . . . H5 H -0.1161 -0.0177 0.5877 0.047 Uiso 1 calc R . . C6 C 0.0075(11) 0.1749(10) 0.7212(7) 0.0311(18) Uani 1 d . . . H6 H 0.0607 0.1119 0.7668 0.037 Uiso 1 calc R . . C7 C 0.1901(11) 0.8183(9) 0.9249(6) 0.0251(16) Uani 1 d . . . H7A H 0.0609 0.8530 0.9283 0.030 Uiso 1 calc R . . H7B H 0.2600 0.8981 0.9027 0.030 Uiso 1 calc R . . C8 C 0.2983(9) 0.8117(8) 1.0391(6) 0.0198(15) Uani 1 d . . . C9 C 0.3735(11) 0.9514(9) 1.1259(6) 0.0243(16) Uani 1 d . . . H9 H 0.3655 1.0543 1.1147 0.029 Uiso 1 calc R . . C10 C 0.4597(12) 0.9372(10) 1.2281(7) 0.0338(19) Uani 1 d . . . H10 H 0.5088 1.0310 1.2875 0.041 Uiso 1 calc R . . C11 C 0.4746(11) 0.7832(10) 1.2442(6) 0.0293(17) Uani 1 d . . . H11 H 0.5358 0.7719 1.3133 0.035 Uiso 1 calc R . . C12 C 0.3961(10) 0.6484(9) 1.1550(6) 0.0206(15) Uani 1 d . . . H12 H 0.4037 0.5449 1.1652 0.025 Uiso 1 calc R . . Cl2 Cl 0.4525(3) 0.6282(2) 0.68261(16) 0.0304(4) Uani 1 d . . . O1 O 0.3133(10) 0.2847(8) 0.4869(5) 0.0473(16) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0180(3) 0.0174(3) 0.0228(3) 0.0067(2) 0.0038(2) 0.00168(19) Cl1 0.0347(10) 0.0186(9) 0.0340(10) 0.0123(8) 0.0083(8) 0.0016(8) N1 0.035(4) 0.026(3) 0.020(3) 0.013(3) -0.003(3) 0.003(3) N2 0.019(3) 0.033(4) 0.019(3) 0.007(3) 0.001(2) -0.001(3) N3 0.014(3) 0.019(3) 0.025(3) 0.009(3) 0.005(2) 0.003(2) C1 0.033(4) 0.026(4) 0.031(4) 0.009(3) 0.006(3) 0.006(3) C2 0.018(4) 0.038(5) 0.026(4) 0.008(4) 0.007(3) 0.000(3) C3 0.031(4) 0.037(5) 0.032(5) 0.004(4) -0.007(4) 0.003(4) C4 0.028(4) 0.046(5) 0.034(5) -0.001(4) -0.006(4) -0.001(4) C5 0.029(4) 0.035(5) 0.042(5) -0.012(4) 0.011(4) -0.004(4) C6 0.024(4) 0.030(4) 0.031(4) 0.002(4) 0.000(3) -0.003(3) C7 0.027(4) 0.017(3) 0.033(4) 0.010(3) 0.008(3) 0.007(3) C8 0.009(3) 0.019(3) 0.031(4) 0.009(3) 0.003(3) -0.001(3) C9 0.027(4) 0.020(4) 0.026(4) 0.009(3) 0.004(3) -0.001(3) C10 0.033(4) 0.027(4) 0.030(4) -0.001(4) -0.004(4) -0.004(3) C11 0.023(4) 0.043(5) 0.020(4) 0.012(4) 0.000(3) 0.004(3) C12 0.018(3) 0.022(4) 0.026(4) 0.011(3) 0.008(3) 0.003(3) Cl2 0.0356(11) 0.0302(10) 0.0255(10) 0.0074(8) 0.0084(8) 0.0013(8) O1 0.054(4) 0.036(4) 0.049(4) 0.012(3) 0.009(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; # ---------------------------------------- # 8. MOLECULAR GEOMETRY # ---------------------------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N1 2.005(6) . ? Pd N2 2.006(6) . ? Pd N3 2.007(6) . ? Pd Cl1 2.305(2) . ? N1 C7 1.478(9) . ? N1 C1 1.491(10) . ? N2 C6 1.363(10) . ? N2 C2 1.348(10) . ? N3 C12 1.338(9) . ? N3 C8 1.367(9) . ? C1 C2 1.522(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.383(11) . ? C3 C4 1.360(12) . ? C3 H3 0.9300 . ? C4 C5 1.383(13) . ? C4 H4 0.9300 . ? C5 C6 1.373(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.515(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.378(10) . ? C9 C10 1.361(11) . ? C9 H9 0.9300 . ? C10 C11 1.391(12) . ? C10 H10 0.9300 . ? C11 C12 1.372(10) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd N2 82.7(3) . . ? N1 Pd N3 83.8(2) . . ? N2 Pd N3 165.8(2) . . ? N1 Pd Cl1 174.7(2) . . ? N2 Pd Cl1 96.87(19) . . ? N3 Pd Cl1 96.97(17) . . ? C7 N1 C1 115.5(6) . . ? C7 N1 Pd 110.5(4) . . ? C1 N1 Pd 107.4(5) . . ? C6 N2 C2 117.8(7) . . ? C6 N2 Pd 128.2(5) . . ? C2 N2 Pd 114.0(5) . . ? C12 N3 C8 118.6(6) . . ? C12 N3 Pd 128.2(5) . . ? C8 N3 Pd 113.2(5) . . ? N1 C1 C2 108.9(6) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C3 122.2(8) . . ? N2 C2 C1 114.6(7) . . ? C3 C2 C1 123.2(7) . . ? C4 C3 C2 118.7(8) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.7(8) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 118.0(8) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? N2 C6 C5 122.5(8) . . ? N2 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? N1 C7 C8 110.4(6) . . ? N1 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N1 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C9 C8 N3 121.1(7) . . ? C9 C8 C7 122.2(6) . . ? N3 C8 C7 116.6(6) . . ? C8 C9 C10 119.3(7) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 120.3(7) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 117.9(7) . . ? C12 C11 H11 121.0 . . ? C10 C11 H11 121.0 . . ? N3 C12 C11 122.8(7) . . ? N3 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.858 _refine_diff_density_min -0.921 _refine_diff_density_rms 0.175 #========END of CIF