#Copyright The Royal Society of Chemistry, 1998 #Crystallographic Information File relative to the #two crystal structures reported in the paper #Pd(II) Coordination by Linear N-Methylated Polyamines. #A Solution and Solid State Study. #Authors: #C. Bazzicalupi, A. Bencini, H. Cohen, C. Giorgi, G. Golub, #D. Meyerstein, N. Navon, P. Paoletti, B. Valtancoli #Submitted for publication in Dalton Trans. #Manuscript No. 7/09284I data_[Pd2LCl2](ClO4)2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; (Pd2+)2, C18 H44 N6, (Cl-)2, (Cl O4-)2 ; _chemical_formula_structural ; (Pd)2 (Cl)2 (C18 H44 N6) (Cl O4)2 ; _chemical_formula_analytical ? _chemical_formula_sum 'C18 H44 Cl4 N6 O8 Pd2' _chemical_formula_weight 827.2 _chemical_melting_point ? _chemical_compound_source ? 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 'monoclinic' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.700(10) _cell_length_b 12.298(2) _cell_length_c 16.410(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.30(10) _cell_angle_gamma 90.00 _cell_volume 1541.3(22) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 16 _cell_measurement_theta_min 7 _cell_measurement_theta_max 12 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.035 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method ? _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 1.563 _exptl_absorpt_correction_type 'refdelf (Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method '\q/2\q' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2909 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 24.95 _reflns_number_total 2695 _reflns_number_observed 2112 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction 'Enraf-Nonius CAD4' _computing_structure_solution 'Patterson method' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson,1971)' _computing_publication_material 'PARST93 (Nardelli,1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1050P)^2^+5.6559P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2689 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_obs 0.0560 _refine_ls_wR_factor_all 0.1822 _refine_ls_wR_factor_obs 0.1486 _refine_ls_goodness_of_fit_all 0.982 _refine_ls_goodness_of_fit_obs 0.985 _refine_ls_restrained_S_all 1.063 _refine_ls_restrained_S_obs 0.985 _refine_ls_shift/esd_max -0.050 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd -0.03282(7) 0.18807(5) -0.12527(3) 0.0413(2) Uani 1 d . . Cl1 Cl -0.2878(3) 0.0912(2) -0.1604(2) 0.0655(6) Uani 1 d . . C1 C -0.2951(13) 0.3716(9) -0.1535(7) 0.076(3) Uani 1 d . . H1A H -0.2796(30) 0.3817(54) -0.0951(9) 0.089(7) Uiso 1 calc R . H1B H -0.3873(23) 0.3200(28) -0.1684(38) 0.089(7) Uiso 1 calc R . H1C H -0.3252(50) 0.4397(29) -0.1802(33) 0.089(7) Uiso 1 calc R . C2 C -0.1589(16) 0.3086(8) -0.2701(6) 0.073(3) Uani 1 d . . H2A H -0.0522(28) 0.2823(52) -0.2875(9) 0.089(7) Uiso 1 calc R . H2B H -0.1935(86) 0.3747(14) -0.2988(6) 0.089(7) Uiso 1 calc R . H2C H -0.2491(62) 0.2550(40) -0.2819(8) 0.089(7) Uiso 1 calc R . N1 N -0.1305(9) 0.3303(5) -0.1798(4) 0.053(2) Uani 1 d . . C3 C 0.0112(14) 0.4138(8) -0.1611(8) 0.081(3) Uani 1 d . . H3A H 0.0027(14) 0.4676(8) -0.2046(8) 0.089(7) Uiso 1 calc R . H3B H -0.0031(14) 0.4506(8) -0.1101(8) 0.089(7) Uiso 1 calc R . C4 C 0.1880(14) 0.3597(9) -0.1536(8) 0.079(3) Uani 1 d . . H4A H 0.2798(14) 0.4126(9) -0.1387(8) 0.089(7) Uiso 1 calc R . H4B H 0.2066(14) 0.3267(9) -0.2055(8) 0.089(7) Uiso 1 calc R . N2 N 0.1904(9) 0.2750(6) -0.0887(5) 0.057(2) Uani 1 d . . C5 C 0.1946(15) 0.3199(9) -0.0058(7) 0.079(3) Uani 1 d . . H5A H 0.0903(45) 0.3615(46) -0.0025(14) 0.089(7) Uiso 1 calc R . H5B H 0.2953(52) 0.3660(45) 0.0061(17) 0.089(7) Uiso 1 calc R . H5C H 0.2010(89) 0.2615(9) 0.0333(8) 0.089(7) Uiso 1 calc R . C6 C 0.3350(11) 0.1951(8) -0.0902(6) 0.065(3) Uani 1 d . . H6A H 0.4425(11) 0.2247(8) -0.0615(6) 0.089(7) Uiso 1 calc R . H6B H 0.3536(11) 0.1807(8) -0.1466(6) 0.089(7) Uiso 1 calc R . C7 C 0.2898(10) 0.0918(8) -0.0501(5) 0.060(2) Uani 1 d . . H7A H 0.2857(10) 0.1044(8) 0.0080(5) 0.089(7) Uiso 1 calc R . H7B H 0.3792(10) 0.0376(8) -0.0555(5) 0.089(7) Uiso 1 calc R . N3 N 0.1129(8) 0.0503(5) -0.0899(4) 0.049(2) Uani 1 d . . C8 C 0.1372(13) -0.0068(8) -0.1677(5) 0.064(2) Uani 1 d . . H8A H 0.2094(71) 0.0366(26) -0.1985(19) 0.089(7) Uiso 1 calc R . H8B H 0.0252(14) -0.0181(47) -0.1996(19) 0.089(7) Uiso 1 calc R . H8C H 0.1926(78) -0.0758(24) -0.1552(5) 0.089(7) Uiso 1 calc R . C9 C 0.0360(11) -0.0264(7) -0.0356(5) 0.055(2) Uani 1 d . . H9A H 0.1249(11) -0.0786(7) -0.0144(5) 0.089(7) Uiso 1 calc R . H9B H -0.0575(11) -0.0663(7) -0.0678(5) 0.089(7) Uiso 1 calc R . Cl2 Cl -0.2817(4) 0.3209(2) 0.1088(2) 0.0695(7) Uani 1 d . . O1 O -0.3685(13) 0.2283(7) 0.0789(6) 0.110(3) Uani 1 d . . O2 O -0.2008(21) 0.3789(14) 0.0558(8) 0.195(7) Uani 1 d . . O3 O -0.1913(31) 0.3038(14) 0.1770(11) 0.258(12) Uani 1 d . . O4 O -0.3950(25) 0.3919(13) 0.1327(14) 0.246(10) 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 0.0412(4) 0.0404(4) 0.0428(4) 0.0072(2) 0.0077(2) 0.0032(2) Cl1 0.0517(12) 0.0615(13) 0.082(2) -0.0056(11) 0.0020(10) -0.0069(10) C1 0.071(6) 0.075(7) 0.081(7) 0.014(6) 0.012(5) 0.023(5) C2 0.095(8) 0.073(7) 0.053(5) 0.017(5) 0.013(5) 0.020(6) N1 0.055(4) 0.050(4) 0.054(4) 0.012(3) 0.008(3) 0.014(3) C3 0.084(7) 0.047(5) 0.114(9) 0.018(6) 0.024(6) -0.003(5) C4 0.074(7) 0.059(6) 0.107(9) 0.009(6) 0.026(6) -0.020(5) N2 0.047(4) 0.064(4) 0.061(4) 0.002(4) 0.012(3) -0.008(3) C5 0.072(7) 0.090(8) 0.073(7) -0.024(6) 0.002(5) -0.003(5) C6 0.038(4) 0.093(7) 0.066(6) 0.004(5) 0.007(4) 0.004(4) C7 0.043(4) 0.075(6) 0.061(5) 0.012(5) 0.005(4) 0.018(4) N3 0.047(3) 0.051(4) 0.050(4) 0.012(3) 0.016(3) 0.010(3) C8 0.079(6) 0.061(5) 0.060(5) 0.006(4) 0.033(5) 0.016(5) C9 0.062(5) 0.048(5) 0.059(5) 0.015(4) 0.027(4) 0.013(4) Cl2 0.089(2) 0.0651(15) 0.0556(13) -0.0052(11) 0.0140(12) -0.0095(13) O1 0.123(7) 0.074(5) 0.122(7) -0.024(5) -0.023(6) 0.013(5) O2 0.242(16) 0.233(16) 0.125(10) -0.024(10) 0.086(10) -0.092(14) O3 0.330(24) 0.200(17) 0.197(16) 0.054(12) -0.151(17) -0.123(16) O4 0.207(15) 0.150(13) 0.398(29) -0.133(17) 0.112(17) -0.056(12) _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. ; 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 N2 2.049(7) . ? Pd N1 2.063(6) . ? Pd N3 2.074(6) . ? Pd Cl1 2.306(3) . ? C1 N1 1.479(12) . ? C2 N1 1.494(12) . ? N1 C3 1.501(12) . ? C3 C4 1.506(15) . ? C4 N2 1.487(13) . ? N2 C5 1.464(13) . ? N2 C6 1.488(11) . ? C6 C7 1.492(13) . ? C7 N3 1.523(11) . ? N3 C9 1.473(10) . ? N3 C8 1.489(11) . ? C9 C9 1.50(2) 3 ? Cl2 O3 1.259(14) . ? Cl2 O4 1.33(2) . ? Cl2 O2 1.338(12) . ? Cl2 O1 1.378(9) . ? 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 N2 Pd N1 86.0(3) . . ? N2 Pd N3 86.6(3) . . ? N1 Pd N3 165.6(3) . . ? N2 Pd Cl1 177.4(2) . . ? N1 Pd Cl1 94.4(2) . . ? N3 Pd Cl1 93.5(2) . . ? C1 N1 C2 109.1(8) . . ? C1 N1 C3 109.5(8) . . ? C2 N1 C3 109.6(8) . . ? C1 N1 Pd 116.3(6) . . ? C2 N1 Pd 106.1(5) . . ? C3 N1 Pd 106.0(5) . . ? C4 C3 N1 109.9(8) . . ? C3 C4 N2 107.2(8) . . ? C5 N2 C6 109.6(8) . . ? C5 N2 C4 113.5(9) . . ? C6 N2 C4 113.1(7) . . ? C5 N2 Pd 112.8(6) . . ? C6 N2 Pd 104.6(6) . . ? C4 N2 Pd 102.8(6) . . ? N2 C6 C7 109.8(7) . . ? C6 C7 N3 110.0(7) . . ? C9 N3 C8 108.7(7) . . ? C9 N3 C7 111.2(6) . . ? C8 N3 C7 108.8(6) . . ? C9 N3 Pd 116.6(5) . . ? C8 N3 Pd 105.6(5) . . ? C7 N3 Pd 105.6(5) . . ? N3 C9 C9 114.2(9) . 3 ? O3 Cl2 O4 99.0(15) . . ? O3 Cl2 O2 114.6(12) . . ? O4 Cl2 O2 102.6(12) . . ? O3 Cl2 O1 111.5(8) . . ? O4 Cl2 O1 110.0(8) . . ? O2 Cl2 O1 117.0(8) . . ? _refine_diff_density_max 0.847 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.163 #===END data_[Pd2LCl2](ClO4)4.2H2O _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; (Pd2+)2, C24 H54 N8, (Cl O4-)4, (H2 O)2 ; _chemical_formula_structural ; (Pd)2 (C24 H54 N8) (Cl O4)4 (H2 O) ; _chemical_formula_analytical ? _chemical_formula_sum 'C24 H58 Cl4 N8 O18 Pd2' _chemical_formula_weight 1101.38 _chemical_melting_point ? _chemical_compound_source ? 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 'monoclinic' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.986(8) _cell_length_b 29.980(10) _cell_length_c 9.040(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.24(4) _cell_angle_gamma 90.00 _cell_volume 2155.3(23) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 16 _cell_measurement_theta_min 8 _cell_measurement_theta_max 10 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method ? _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 1.159 _exptl_absorpt_correction_type 'refdelf (Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method '\q/2\q' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2388 _diffrn_reflns_av_R_equivalents 0.1410 _diffrn_reflns_av_sigmaI/netI 0.1767 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 21.99 _reflns_number_total 2227 _reflns_number_observed 1244 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction 'Enraf-Nonius CAD4' _computing_structure_solution 'Patterson method' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson,1971)' _computing_publication_material 'PARST93 (Nardelli,1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0949P)^2^+9.5663P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2221 _refine_ls_number_parameters 269 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1714 _refine_ls_R_factor_obs 0.0722 _refine_ls_wR_factor_all 0.2340 _refine_ls_wR_factor_obs 0.1752 _refine_ls_goodness_of_fit_all 1.054 _refine_ls_goodness_of_fit_obs 1.133 _refine_ls_restrained_S_all 1.080 _refine_ls_restrained_S_obs 1.134 _refine_ls_shift/esd_max -0.020 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.1331(2) 0.11633(5) 0.0801(2) 0.0398(6) Uani 1 d . . Cl1 Cl 0.7973(8) 0.1975(2) 0.3930(7) 0.066(2) Uani 1 d . . O11 O 0.9429(24) 0.2046(7) 0.4857(21) 0.080(7) Uani 0.80 d P . O12 O 0.6577(31) 0.2230(9) 0.4179(39) 0.142(12) Uani 0.80 d P . O13 O 0.7847(39) 0.1555(10) 0.3311(43) 0.169(15) Uani 0.80 d PU . O14 O 0.8274(41) 0.2211(12) 0.2605(31) 0.165(13) Uani 0.80 d P . O15 O 0.7147(62) 0.1704(18) 0.4723(64) 0.242(19) Uani 0.80 d PU . Cl2 Cl 0.4602(8) 0.4414(2) 0.2639(7) 0.064(2) Uani 1 d . . O21 O 0.4477(33) 0.4003(9) 0.1828(30) 0.166(10) Uani 1 d . . O22 O 0.6213(24) 0.4569(7) 0.2601(24) 0.119(7) Uani 1 d . . O23 O 0.4283(27) 0.4320(9) 0.4066(21) 0.152(10) Uani 1 d . . O24 O 0.3395(25) 0.4691(7) 0.1944(22) 0.115(7) Uani 1 d . . N1 N 0.0080(21) 0.1452(5) -0.1166(18) 0.049(5) Uani 1 d . . C1 C -0.0007(27) 0.1158(8) -0.2459(24) 0.072(7) Uani 1 d . . H1A H -0.0750(135) 0.0914(25) -0.2312(68) 0.095(22) Uiso 1 calc R . H1B H 0.1095(40) 0.1045(36) -0.2589(91) 0.095(22) Uiso 1 calc R . H1C H -0.0422(161) 0.1323(14) -0.3328(34) 0.095(22) Uiso 1 calc R . C2 C -0.1610(29) 0.1602(8) -0.0909(29) 0.082(8) Uani 1 d . . H2A H -0.2311(53) 0.1348(9) -0.0777(148) 0.095(22) Uiso 1 calc R . H2B H -0.2074(71) 0.1772(39) -0.1748(72) 0.095(22) Uiso 1 calc R . H2C H -0.1556(36) 0.1785(37) -0.0034(90) 0.095(22) Uiso 1 calc R . C3 C 0.1141(30) 0.1830(9) -0.1416(30) 0.083(8) Uani 1 d . . H3A H 0.0521(30) 0.2037(9) -0.2086(30) 0.107(25) Uiso 1 calc R . H3B H 0.2111(30) 0.1729(9) -0.1893(30) 0.107(25) Uiso 1 calc R . C4 C 0.1731(31) 0.2071(8) -0.0001(31) 0.083(8) Uani 1 d . . H4A H 0.2460(31) 0.2317(8) -0.0209(31) 0.107(25) Uiso 1 calc R . H4B H 0.0778(31) 0.2187(8) 0.0468(31) 0.107(25) Uiso 1 calc R . N2 N 0.2653(18) 0.1745(5) 0.0977(18) 0.045(4) Uani 1 d . . C5 C 0.4396(25) 0.1706(9) 0.0580(30) 0.089(9) Uani 1 d . . H5A H 0.4991(54) 0.1492(34) 0.1221(104) 0.095(22) Uiso 1 calc R . H5B H 0.4942(60) 0.1991(13) 0.0693(149) 0.095(22) Uiso 1 calc R . H5C H 0.4388(25) 0.1609(46) -0.0433(56) 0.095(22) Uiso 1 calc R . C6 C 0.2641(39) 0.1842(9) 0.2594(25) 0.090(9) Uani 1 d . . H6A H 0.3464(39) 0.2072(9) 0.2870(25) 0.107(25) Uiso 1 calc R . H6B H 0.1544(39) 0.1956(9) 0.2781(25) 0.107(25) Uiso 1 calc R . C7 C 0.3022(35) 0.1447(8) 0.3530(26) 0.080(8) Uani 1 d . . H7A H 0.4215(35) 0.1446(8) 0.3847(26) 0.107(25) Uiso 1 calc R . H7B H 0.2424(35) 0.1473(8) 0.4413(26) 0.107(25) Uiso 1 calc R . N3 N 0.2592(22) 0.1024(5) 0.2830(17) 0.050(5) Uani 1 d . . C8 C 0.4167(32) 0.0763(10) 0.2726(27) 0.102(10) Uani 1 d . . H8A H 0.5043(56) 0.0958(13) 0.2461(149) 0.095(22) Uiso 1 calc R . H8B H 0.3972(58) 0.0536(31) 0.1982(115) 0.095(22) Uiso 1 calc R . H8C H 0.4498(103) 0.0627(40) 0.3668(54) 0.095(22) Uiso 1 calc R . C9 C 0.1367(30) 0.0765(8) 0.3545(27) 0.074(7) Uani 1 d . . H9A H 0.0431(30) 0.0956(8) 0.3744(27) 0.107(25) Uiso 1 calc R . H9B H 0.1877(30) 0.0654(8) 0.4489(27) 0.107(25) Uiso 1 calc R . C10 C 0.0724(32) 0.0380(7) 0.2608(22) 0.069(7) Uani 1 d . . H10A H -0.0167(32) 0.0229(7) 0.3074(22) 0.107(25) Uiso 1 calc R . H10B H 0.1623(32) 0.0167(7) 0.2507(22) 0.107(25) Uiso 1 calc R . N4 N 0.0057(20) 0.0552(5) 0.1091(16) 0.044(4) Uani 1 d . . C11 C -0.1780(27) 0.0636(7) 0.1107(23) 0.064(6) Uani 1 d . . H11A H -0.1957(28) 0.0870(33) 0.1800(117) 0.095(22) Uiso 1 calc R . H11B H -0.2324(37) 0.0369(15) 0.1399(153) 0.095(22) Uiso 1 calc R . H11C H -0.2242(43) 0.0723(46) 0.0132(43) 0.095(22) Uiso 1 calc R . C12 C 0.0387(25) 0.0232(6) -0.0092(23) 0.055(6) Uani 1 d . . H12A H 0.1593(25) 0.0199(6) -0.0110(23) 0.107(25) Uiso 1 calc R . H12B H -0.0053(25) 0.0354(6) -0.1042(23) 0.107(25) Uiso 1 calc R . O1 O 0.4673(29) 0.2886(9) 0.1862(30) 0.163(10) 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 0.0414(10) 0.0385(10) 0.0391(8) 0.0002(9) 0.0022(6) 0.0012(9) Cl1 0.061(5) 0.072(5) 0.066(4) -0.004(4) 0.009(3) -0.015(4) O11 0.054(13) 0.108(17) 0.071(13) 0.007(12) -0.025(11) -0.047(12) O12 0.074(17) 0.117(24) 0.237(34) -0.064(23) 0.022(19) 0.053(16) O13 0.138(24) 0.119(22) 0.231(36) -0.137(24) -0.082(24) 0.028(18) O14 0.170(30) 0.233(40) 0.089(20) 0.008(23) 0.006(20) -0.029(27) O15 0.205(36) 0.224(39) 0.281(47) -0.053(38) -0.068(36) -0.028(34) Cl2 0.060(4) 0.066(4) 0.063(4) 0.000(3) 0.000(3) 0.002(4) O21 0.179(24) 0.139(22) 0.180(25) -0.053(20) 0.017(19) 0.015(19) O22 0.074(14) 0.132(18) 0.149(18) 0.025(15) 0.007(12) -0.024(13) O23 0.134(18) 0.254(29) 0.075(14) 0.061(16) 0.047(13) 0.019(19) O24 0.119(16) 0.108(16) 0.114(16) 0.012(13) -0.018(14) 0.033(14) N1 0.056(12) 0.038(11) 0.048(11) 0.000(9) -0.020(9) -0.003(10) C1 0.070(16) 0.084(18) 0.065(15) 0.022(17) 0.016(12) -0.016(17) C2 0.067(18) 0.078(19) 0.101(19) -0.003(16) 0.003(15) 0.028(15) C3 0.059(17) 0.086(21) 0.099(21) 0.025(17) -0.024(15) -0.021(16) C4 0.063(17) 0.064(18) 0.116(22) 0.009(17) -0.019(16) 0.003(15) N2 0.034(11) 0.032(11) 0.069(12) 0.006(9) 0.005(9) -0.004(8) C5 0.036(15) 0.111(23) 0.116(22) -0.042(18) -0.017(14) 0.020(14) C6 0.144(26) 0.075(21) 0.053(16) -0.034(15) 0.014(16) -0.015(19) C7 0.125(23) 0.055(19) 0.055(15) -0.014(14) -0.009(15) 0.007(16) N3 0.054(12) 0.049(13) 0.044(10) 0.001(9) -0.011(9) -0.010(10) C8 0.088(21) 0.158(30) 0.054(16) 0.004(17) -0.017(15) 0.023(21) C9 0.078(18) 0.056(17) 0.083(17) 0.007(14) -0.018(15) -0.001(14) C10 0.111(21) 0.050(15) 0.044(13) 0.012(11) -0.012(13) -0.004(14) N4 0.052(12) 0.035(11) 0.049(10) -0.002(8) 0.021(9) -0.011(8) C11 0.075(18) 0.055(16) 0.061(14) 0.016(12) 0.011(12) -0.005(13) C12 0.048(14) 0.064(16) 0.058(13) 0.002(12) 0.028(11) -0.001(11) O1 0.112(18) 0.204(27) 0.179(25) -0.031(21) 0.053(17) -0.020(18) _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. ; 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 N2 2.038(15) . ? Pd N3 2.053(15) . ? Pd N4 2.123(14) . ? Pd N1 2.141(15) . ? Cl1 O13 1.38(2) . ? Cl1 O15 1.30(6) . ? Cl1 O12 1.39(2) . ? Cl1 O11 1.39(2) . ? Cl1 O14 1.43(3) . ? O12 O15 1.70(6) . ? O13 O15 1.51(6) . ? Cl2 O23 1.37(2) . ? Cl2 O22 1.37(2) . ? Cl2 O24 1.38(2) . ? Cl2 O21 1.43(2) . ? N1 C2 1.46(3) . ? N1 C3 1.45(3) . ? N1 C1 1.46(3) . ? C3 C4 1.51(3) . ? C4 N2 1.47(3) . ? N2 C6 1.49(3) . ? N2 C5 1.47(2) . ? C6 C7 1.47(3) . ? C7 N3 1.44(3) . ? N3 C9 1.45(3) . ? N3 C8 1.49(3) . ? C9 C10 1.50(3) . ? C10 N4 1.52(2) . ? N4 C12 1.48(2) . ? N4 C11 1.49(2) . ? C12 C12 1.53(4) 3 ? 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 N2 Pd N3 84.0(6) . . ? N2 Pd N4 168.4(6) . . ? N3 Pd N4 85.2(6) . . ? N2 Pd N1 85.3(6) . . ? N3 Pd N1 167.9(6) . . ? N4 Pd N1 105.0(6) . . ? O13 Cl1 O15 68.4(26) . . ? O13 Cl1 O12 122.6(18) . . ? O15 Cl1 O12 78.4(25) . . ? O13 Cl1 O11 114.4(15) . . ? O15 Cl1 O11 101.7(21) . . ? O12 Cl1 O11 117.3(16) . . ? O13 Cl1 O14 97.1(23) . . ? O15 Cl1 O14 154.5(24) . . ? O12 Cl1 O14 93.6(21) . . ? O11 Cl1 O14 103.5(15) . . ? Cl1 O12 O15 48.6(21) . . ? Cl1 O13 O15 53.5(21) . . ? Cl1 O15 O13 58.1(31) . . ? Cl1 O15 O12 53.0(23) . . ? O13 O15 O12 98.0(41) . . ? O23 Cl2 O22 110.5(14) . . ? O23 Cl2 O24 111.8(14) . . ? O22 Cl2 O24 113.8(13) . . ? O23 Cl2 O21 107.1(17) . . ? O22 Cl2 O21 107.4(15) . . ? O24 Cl2 O21 105.8(14) . . ? C2 N1 C3 110.3(19) . . ? C2 N1 C1 109.6(17) . . ? C3 N1 C1 109.5(19) . . ? C2 N1 Pd 111.1(15) . . ? C3 N1 Pd 102.2(12) . . ? C1 N1 Pd 113.9(13) . . ? N1 C3 C4 112.6(21) . . ? N2 C4 C3 107.2(20) . . ? C4 N2 C6 114.4(19) . . ? C4 N2 C5 109.8(19) . . ? C6 N2 C5 110.2(19) . . ? C4 N2 Pd 107.1(13) . . ? C6 N2 Pd 101.2(13) . . ? C5 N2 Pd 114.0(14) . . ? C7 C6 N2 112.8(20) . . ? N3 C7 C6 115.2(18) . . ? C9 N3 C7 114.8(19) . . ? C9 N3 C8 110.8(18) . . ? C7 N3 C8 108.7(19) . . ? C9 N3 Pd 102.2(12) . . ? C7 N3 Pd 106.9(13) . . ? C8 N3 Pd 113.5(13) . . ? N3 C9 C10 111.9(20) . . ? C9 C10 N4 108.8(17) . . ? C12 N4 C11 110.9(16) . . ? C12 N4 C10 111.1(16) . . ? C11 N4 C10 108.3(16) . . ? C12 N4 Pd 110.7(11) . . ? C11 N4 Pd 109.8(12) . . ? C10 N4 Pd 105.9(12) . . ? N4 C12 C12 114.2(19) . 3 ? _refine_diff_density_max 0.893 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.152 #===END