# Copyright The Royal Society of Chemistry, 1998. # 3 CIF's belonging to 7/04170E (From A.L.Spek - Utrecht University) # ***** Complex 1 ******* # CIF-file generated for (C26H22ClNPPd)2 CP339 #================================================================ data_cp339 #================================================================ # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Cl2 N2 P2 Pd2' _chemical_formula_structural ? _chemical_formula_sum 'C52 H44 Cl2 N2 P2 Pd2' _chemical_formula_weight 1042.63 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #================================================================ # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 17.789(5) _cell_length_b 14.170(4) _cell_length_c 19.423(7) _cell_angle_alpha 90 _cell_angle_beta 113.02(2) _cell_angle_gamma 90 _cell_volume 4506(3) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 18.00 _cell_measurement_theta_max 20.47 _cell_special_details ; ? ; _exptl_crystal_description 'irregular fragment' _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.19 _exptl_crystal_size_rad ? _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method ? _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 1.03 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #================================================================ # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4F _diffrn_measurement_method '\w/2\q scan' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temperature unit (Bolhuis, 1971), on an Enraf-Nonius CAD4-4F diffractometer. Graphite-monochromated Mo K\a radiation, \w/2\q scan, \D\w = (1.00 + 0.34 tg \q)\%. ; _diffrn_standards_number 3 _diffrn_standards_interval_count ?' _diffrn_standards_interval_time 10800 _diffrn_standards_decay_% .7? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -3 0 -2 2 -2 1 3 -4 # number of measured reflections (redundant set) _diffrn_reflns_number 9610 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI 0.036 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 26.5 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, scale variation, but not for absorption and reduced to F~o~^2^ ; # number of unique reflections _reflns_number_total 4678 # number of observed reflections (> n sig(I)) _reflns_number_gt ? _reflns_threshold_expression >0 _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'DIRDIF4 (Beurskens, 1994)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material 'PLATON (Spek, 1990)' #================================================================ # 8. REFINEMENT DATA _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.06622P)^2^+28.60P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment 'isotropic refinement ' _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ; ? ; _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4269 _refine_ls_number_parameters 359 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_obs .1298 _refine_ls_wR_factor_ref ? _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max ? _refine_ls_shift/esd_mean '< 0.001' _refine_diff_density_max 1.22(13) _refine_diff_density_min -1.14 #================================================================ # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Pd Uani .05929(2) .27636(2) .09370(2) 1.000 .0279(1) Cl Uani -.07207(6) .20936(7) .03460(6) 1.000 .0306(3) P Uani .18205(7) .33582(9) .15168(7) 1.000 .0326(4) N Uani .0878(2) .2244(3) .2100(2) 1.000 .0267(11) C1 Uani .2635(3) .2536(4) .1610(3) 1.000 .0370(14) C2 Uani .2604(4) .2023(5) .0996(4) 1.000 .0489(19) C3 Uani .3215(5) .1408(5) .1045(5) 1.000 .062(3) C4 Uani .3866(4) .1275(5) .1717(5) 1.000 .062(2) C5 Uani .3899(4) .1773(5) .2341(5) 1.000 .060(2) C6 Uani .3284(3) .2401(4) .2271(4) 1.000 .0432(17) C7 Uani .2145(3) .4466(4) .1255(3) 1.000 .0369(16) C8 Uani .1686(4) .5264(4) .1215(4) 1.000 .0495(19) C9 Uani .1914(4) .6115(4) .0997(4) 1.000 .054(2) C10 Uani .2564(3) .6158(4) .0792(3) 1.000 .0462(17) C11 Uani .3006(3) .5370(4) .0806(3) 1.000 .0460(17) C12 Uani .2810(3) .4511(4) .1048(3) 1.000 .0383(16) C13 Uani .1842(3) .3535(3) .2443(3) 1.000 .0315(12) C14 Uani .2339(3) .4164(4) .2968(3) 1.000 .0403(17) C15 Uani .2282(3) .4257(4) .3651(3) 1.000 .0426(17) C16 Uani .1704(3) .3748(4) .3802(3) 1.000 .0407(17) C17 Uani .1217(3) .3104(3) .3299(3) 1.000 .0346(16) C18 Uani .1298(3) .2965(3) .2624(3) 1.000 .0281(12) C19 Uani .0768(3) .1452(3) .2372(3) 1.000 .0254(12) C20 Uani .0481(3) .0599(3) .1930(3) 1.000 .0267(12) C21 Uani .0678(3) .0468(3) .1306(3) 1.000 .0325(14) C22 Uani .0501(3) -.0358(4) .0904(3) 1.000 .0374(16) C23 Uani .0099(3) -.1065(4) .1110(3) 1.000 .0420(16) C24 Uani -.0098(3) -.0952(3) .1731(3) 1.000 .0362(16) C25 Uani .0093(3) -.0133(3) .2159(2) 1.000 .0258(11) C26 Uani .0444(4) .3446(5) -.0021(3) 1.000 .048(2) H2 Uiso .217(4) .205(4) .062(4) 1.000 .043(17) H3 Uiso .322(4) .100(5) .066(4) 1.000 .06(2) H4 Uiso .428(4) .088(5) .178(4) 1.000 .060(19) H5 Uiso .438(4) .164(4) .281(4) 1.000 .039(15) H6 Uiso .335(4) .260(4) .264(4) 1.000 .034(16) H8 Uiso .124(4) .517(4) .139(4) 1.000 .051(17) H9 Uiso .161(3) .655(4) .096(3) 1.000 .028(14) H10 Uiso .269(3) .669(4) .063(3) 1.000 .036(14) H11 Uiso .344(4) .543(5) .067(4) 1.000 .058(19) H12 Uiso .318(3) .402(4) .112(3) 1.000 .021(11) H14 Uiso .272(4) .453(5) .287(4) 1.000 .07(2) H15 Uiso .260(4) .461(4) .391(4) 1.000 .043(16) H16 Uiso .163(3) .389(4) .426(3) 1.000 .041(15) H17 Uiso .090(3) .278(4) .345(3) 1.000 .034(14) H19 Uiso .087(3) .141(3) .279(3) 1.000 .015(11) H21 Uiso .089(3) .088(4) .114(3) 1.000 .033(14) H22 Uiso .061(3) -.042(4) .044(3) 1.000 .037(14) H23 Uiso -.004(4) -.156(5) .084(4) 1.000 .049(17) H24 Uiso -.035(3) -.144(4) .190(3) 1.000 .037(14) H26 Uiso .036(6) .398(8) .008(6) 1.000 .11(4) H26' Uiso -.002(5) .330(6) -.040(5) 1.000 .07(2) H26" Uiso .083(5) .321(6) -.016(5) 1.000 .08(2) 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 .0312(2) .0289(2) .0273(2) -.0004(1) .0155(2) -.0088(1) Cl .0307(5) .0289(5) .0358(6) -.0049(4) .0170(4) -.0060(4) P .0335(6) .0333(6) .0353(7) -.0002(5) .0182(5) -.0109(5) N .0304(18) .0261(18) .0274(19) -.0017(15) .0154(15) -.0045(14) C1 .037(2) .036(2) .046(3) .002(2) .025(2) -.010(2) C2 .052(3) .051(3) .051(4) -.004(3) .028(3) -.009(3) C3 .071(4) .051(4) .090(5) -.016(4) .059(4) -.012(3) C4 .043(3) .049(3) .108(6) -.004(4) .044(4) -.002(3) C5 .043(3) .053(4) .089(5) .005(4) .030(4) -.001(3) C6 .036(3) .050(3) .047(3) .002(3) .020(3) .000(2) C7 .036(2) .038(3) .038(3) .004(2) .016(2) -.013(2) C8 .047(3) .042(3) .065(4) .007(3) .028(3) -.008(2) C9 .058(4) .036(3) .065(4) .007(3) .021(3) -.008(3) C10 .048(3) .045(3) .036(3) .009(2) .006(2) -.027(3) C11 .040(3) .054(3) .043(3) .007(3) .015(2) -.025(3) C12 .034(2) .044(3) .037(3) .007(2) .014(2) -.011(2) C13 .032(2) .033(2) .030(2) -.0001(19) .0128(19) -.0066(18) C14 .039(3) .038(3) .043(3) -.006(2) .015(2) -.013(2) C15 .045(3) .038(3) .039(3) -.012(2) .010(2) -.011(2) C16 .055(3) .038(3) .032(3) -.004(2) .020(2) -.003(2) C17 .046(3) .031(2) .033(3) -.0008(19) .022(2) -.005(2) C18 .031(2) .028(2) .027(2) -.0011(18) .0133(18) -.0068(18) C19 .026(2) .030(2) .024(2) .0041(18) .0140(17) .0017(17) C20 .026(2) .025(2) .029(2) .0045(17) .0108(17) .0070(16) C21 .034(2) .031(2) .034(3) .005(2) .015(2) .0057(19) C22 .044(3) .042(3) .028(2) -.003(2) .016(2) .013(2) C23 .055(3) .029(2) .042(3) -.013(2) .019(2) .003(2) C24 .041(3) .025(2) .043(3) -.004(2) .017(2) -.0007(19) C25 .028(2) .0206(19) .029(2) .0009(17) .0115(18) .0029(16) C26 .055(4) .057(4) .031(3) .008(3) .016(3) -.023(3) #================================================================ # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd Cl 2.3625(15) . . yes Pd P 2.1963(16) . . yes Pd N 2.237(4) . . yes Pd C26 2.020(6) . . yes P C1 1.812(6) . . yes P C7 1.813(6) . . yes P C13 1.802(6) . . yes N C18 1.429(6) . . yes N C19 1.288(6) . . yes C1 C2 1.379(9) . . no C1 C6 1.363(9) . . no C2 C3 1.367(11) . . no C3 C4 1.378(13) . . no C4 C5 1.384(12) . . no C5 C6 1.375(10) . . no C7 C8 1.379(9) . . no C7 C12 1.392(8) . . no C8 C9 1.390(9) . . no C9 C10 1.364(10) . . no C10 C11 1.360(8) . . no C11 C12 1.397(8) . . no C13 C14 1.382(7) . . no C13 C18 1.407(8) . . no C14 C15 1.376(8) . . no C15 C16 1.378(8) . . no C16 C17 1.370(7) . . no C17 C18 1.388(8) . . no C19 C20 1.455(7) . . no C20 C21 1.399(8) . . no C20 C25 1.411(7) . . no C21 C22 1.373(7) . . no C22 C23 1.378(8) . . no C23 C24 1.391(8) . . no C24 C25 1.390(6) . . no C25 C25 1.486(6) . 2_555 no C2 H2 .83(7) . . no C3 H3 .95(7) . . no C4 H4 .89(8) . . no C5 H5 .99(7) . . no C6 H6 .74(7) . . no C8 H8 .99(8) . . no C9 H9 .80(6) . . no C10 H10 .88(6) . . no C11 H11 .91(8) . . no C12 H12 .93(6) . . no C14 H14 .93(8) . . no C15 H15 .78(7) . . no C16 H16 .97(6) . . no C17 H17 .86(6) . . no C19 H19 .76(5) . . no C21 H21 .83(6) . . no C22 H22 1.00(6) . . no C23 H23 .85(7) . . no C24 H24 .95(6) . . no C26 H26 .81(11) . . no C26 H26' .89(9) . . no C26 H26" .90(9) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Pd P 178.21(5) . . . yes Cl Pd N 98.57(11) . . . yes Cl Pd C26 89.8(2) . . . yes P Pd N 79.70(11) . . . yes P Pd C26 92.0(2) . . . yes N Pd C26 169.6(2) . . . yes Pd P C1 113.60(19) . . . yes Pd P C7 123.39(19) . . . yes Pd P C13 101.18(19) . . . yes C1 P C7 104.8(3) . . . yes C1 P C13 106.6(2) . . . yes C7 P C13 106.0(2) . . . yes Pd N C18 109.4(3) . . . yes Pd N C19 133.7(3) . . . yes C18 N C19 116.9(4) . . . yes P C1 C2 119.5(5) . . . yes P C1 C6 122.3(4) . . . yes C2 C1 C6 118.2(6) . . . no C1 C2 C3 120.9(7) . . . no C2 C3 C4 120.3(8) . . . no C3 C4 C5 119.5(7) . . . no C4 C5 C6 118.9(8) . . . no C1 C6 C5 122.1(7) . . . no P C7 C8 118.6(5) . . . yes P C7 C12 121.4(4) . . . yes C8 C7 C12 119.8(6) . . . no C7 C8 C9 119.4(7) . . . no C8 C9 C10 120.6(6) . . . no C9 C10 C11 120.5(5) . . . no C10 C11 C12 120.2(5) . . . no C7 C12 C11 119.3(5) . . . no P C13 C14 125.7(4) . . . yes P C13 C18 114.9(4) . . . yes C14 C13 C18 119.3(5) . . . no C13 C14 C15 120.4(5) . . . no C14 C15 C16 119.8(5) . . . no C15 C16 C17 120.9(5) . . . no C16 C17 C18 119.9(5) . . . no N C18 C13 116.8(5) . . . yes N C18 C17 123.8(5) . . . yes C13 C18 C17 119.4(5) . . . no N C19 C20 123.8(5) . . . yes C19 C20 C21 118.2(5) . . . no C19 C20 C25 121.8(5) . . . no C21 C20 C25 119.6(4) . . . no C20 C21 C22 121.7(5) . . . no C21 C22 C23 119.0(5) . . . no C22 C23 C24 120.2(5) . . . no C23 C24 C25 122.0(5) . . . no C20 C25 C24 117.4(4) . . . no C20 C25 C25 126.0(4) . . 2_555 no C24 C25 C25 116.5(4) . . 2_555 no C1 C2 H2 116(5) . . . no C3 C2 H2 122(5) . . . no C2 C3 H3 126(5) . . . no C4 C3 H3 114(5) . . . no C3 C4 H4 124(5) . . . no C5 C4 H4 117(5) . . . no C4 C5 H5 116(4) . . . no C6 C5 H5 125(4) . . . no C1 C6 H6 128(6) . . . no C5 C6 H6 110(6) . . . no C7 C8 H8 114(3) . . . no C9 C8 H8 126(3) . . . no C8 C9 H9 115(4) . . . no C10 C9 H9 124(4) . . . no C9 C10 H10 120(4) . . . no C11 C10 H10 119(4) . . . no C10 C11 H11 118(5) . . . no C12 C11 H11 122(5) . . . no C7 C12 H12 124(4) . . . no C11 C12 H12 117(4) . . . no C13 C14 H14 121(4) . . . no C15 C14 H14 119(4) . . . no C14 C15 H15 112(6) . . . no C16 C15 H15 128(6) . . . no C15 C16 H16 118(3) . . . no C17 C16 H16 121(3) . . . no C16 C17 H17 115(4) . . . no C18 C17 H17 125(4) . . . no N C19 H19 120(3) . . . no C20 C19 H19 117(3) . . . no C20 C21 H21 123(4) . . . no C22 C21 H21 115(4) . . . no C21 C22 H22 120(3) . . . no C23 C22 H22 120(3) . . . no C22 C23 H23 119(5) . . . no C24 C23 H23 121(5) . . . no C23 C24 H24 122(3) . . . no C25 C24 H24 116(3) . . . no Pd C26 H26 101(8) . . . no Pd C26 H26' 113(6) . . . no Pd C26 H26" 105(6) . . . no H26 C26 H26' 103(10) . . . no H26 C26 H26" 131(10) . . . no H26' C26 H26" 104(8) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N Pd P C1 83.8(2) . . . . no N Pd P C7 -147.8(3) . . . . no N Pd P C13 -30.05(19) . . . . no C26 Pd P C1 -102.5(3) . . . . no C26 Pd P C7 25.9(3) . . . . no C26 Pd P C13 143.7(3) . . . . no Cl Pd N C18 -141.1(3) . . . . no Cl Pd N C19 41.7(5) . . . . no P Pd N C18 39.3(3) . . . . no P Pd N C19 -137.8(5) . . . . no Pd P C1 C2 47.6(6) . . . . no Pd P C1 C6 -132.3(5) . . . . no C7 P C1 C2 -89.9(5) . . . . no C7 P C1 C6 90.3(5) . . . . no C13 P C1 C2 158.1(5) . . . . no C13 P C1 C6 -21.7(6) . . . . no Pd P C7 C8 54.4(5) . . . . no Pd P C7 C12 -121.3(4) . . . . no C1 P C7 C8 -173.5(5) . . . . no C1 P C7 C12 10.8(5) . . . . no C13 P C7 C8 -61.0(5) . . . . no C13 P C7 C12 123.3(5) . . . . no Pd P C13 C14 -157.0(5) . . . . no Pd P C13 C18 23.3(4) . . . . no C1 P C13 C14 84.0(5) . . . . no C1 P C13 C18 -95.7(4) . . . . no C7 P C13 C14 -27.2(6) . . . . no C7 P C13 C18 153.1(4) . . . . no Pd N C18 C13 -35.5(5) . . . . no Pd N C18 C17 146.8(4) . . . . no C19 N C18 C13 142.2(5) . . . . no C19 N C18 C17 -35.5(7) . . . . no Pd N C19 C20 7.9(8) . . . . no C18 N C19 C20 -169.1(5) . . . . no P C1 C2 C3 179.0(6) . . . . no C6 C1 C2 C3 -1.2(10) . . . . no P C1 C6 C5 179.7(6) . . . . no C2 C1 C6 C5 -.2(10) . . . . no C1 C2 C3 C4 1.5(12) . . . . no C2 C3 C4 C5 -.4(12) . . . . no C3 C4 C5 C6 -.9(11) . . . . no C4 C5 C6 C1 1.3(10) . . . . no P C7 C8 C9 -178.4(5) . . . . no C12 C7 C8 C9 -2.6(9) . . . . no P C7 C12 C11 176.0(4) . . . . no C8 C7 C12 C11 .4(8) . . . . no C7 C8 C9 C10 2.9(10) . . . . no C8 C9 C10 C11 -.8(10) . . . . no C9 C10 C11 C12 -1.5(9) . . . . no C10 C11 C12 C7 1.7(8) . . . . no P C13 C14 C15 178.0(4) . . . . no C18 C13 C14 C15 -2.3(8) . . . . no P C13 C18 N 7.7(6) . . . . no P C13 C18 C17 -174.5(4) . . . . no C14 C13 C18 N -172.0(5) . . . . no C14 C13 C18 C17 5.8(8) . . . . no C13 C14 C15 C16 -2.6(9) . . . . no C14 C15 C16 C17 4.1(9) . . . . no C15 C16 C17 C18 -.6(8) . . . . no C16 C17 C18 N 173.3(5) . . . . no C16 C17 C18 C13 -4.3(8) . . . . no N C19 C20 C21 30.3(8) . . . . no N C19 C20 C25 -156.7(5) . . . . no C19 C20 C21 C22 173.4(5) . . . . no C25 C20 C21 C22 .2(8) . . . . no C19 C20 C25 C24 -174.8(5) . . . . no C19 C20 C25 C25 1.7(8) . . . 2_555 no C21 C20 C25 C24 -1.8(8) . . . . no C21 C20 C25 C25 174.7(5) . . . 2_555 no C20 C21 C22 C23 1.8(8) . . . . no C21 C22 C23 C24 -2.2(8) . . . . no C22 C23 C24 C25 .5(8) . . . . no C23 C24 C25 C20 1.5(8) . . . . no C23 C24 C25 C25 -175.4(5) . . . 2_555 no C20 C25 C25 C20 49.2(8) . . 2_555 2_555 no C20 C25 C25 C24 -134.2(5) . . 2_555 2_555 no C24 C25 C25 C20 -134.2(5) . . 2_555 2_555 no C24 C25 C25 C24 42.3(7) . . 2_555 2_555 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd C21 3.322(4) . . no Pd C17 4.067(6) . 2_555 no Cl C22 3.583(6) . 3_555 no Cl C17 3.402(6) . 2_555 no Cl C21 3.368(5) . . no C2 C12 3.542(9) . . no C3 C15 3.291(9) . 6_545 no C4 C15 3.423(9) . 6_545 no C6 C14 3.561(8) . . no C8 C14 3.504(9) . . no C10 C16 3.560(8) . 4_564 no C10 C17 3.525(8) . 6_555 no C12 C24 3.490(8) . 5_555 no C12 C2 3.542(9) . . no C14 C8 3.504(9) . . no C14 C6 3.561(8) . . no C15 C3 3.291(9) . 6_555 no C15 C4 3.423(9) . 6_555 no C16 C10 3.560(8) . 4_565 no C17 C10 3.525(8) . 6_545 no C17 Cl 3.402(6) . 2_555 no C17 Pd 4.067(6) . 2_555 no C19 C20 3.254(8) . 2_555 no C19 C19 2.962(8) . 2_555 no C20 C19 3.254(8) . 2_555 no C21 Pd 3.322(4) . . no C21 Cl 3.368(5) . . no C22 Cl 3.583(6) . 3_555 no C22 C22 3.412(8) . 3_555 no C24 C12 3.490(8) . 5_445 no Pd H17 3.31(6) . 2_555 no Pd H8 3.60(6) . . no Pd H23 3.62(7) . 3_555 no Pd H2 3.26(8) . . no Pd H21 2.72(6) . . no Cl H22 2.87(6) . 3_555 no Cl H11 2.99(7) . 5_445 no Cl H10 3.14(6) . 5_445 no Cl H9 3.08(6) . 3_565 no Cl H17 2.66(6) . 2_555 no N H21 2.69(6) . . no C1 H12 2.64(6) . . no C2 H12 2.99(6) . . no C3 H26" 2.90(9) . 7_555 no C3 H15 2.95(6) . 6_545 no C4 H5 2.93(8) . 2_655 no C7 H14 2.90(7) . . no C10 H16 2.78(5) . 4_564 no C10 H19 3.08(6) . 6_555 no C11 H19 3.06(5) . 6_555 no C13 H8 3.00(6) . . no C13 H6 2.88(7) . . no C14 H6 3.07(7) . . no C17 H10 2.99(6) . 6_545 no C17 H19 2.58(4) . . no C19 H17 2.76(6) . . no C19 H19 2.81(6) . 2_555 no C20 H19 2.90(6) . 2_555 no C21 H14 2.98(7) . 6_545 no C22 H22 2.81(5) . 3_555 no C24 H24 2.55(5) . 2_555 no C24 H12 2.82(6) . 5_445 no C25 H19 2.80(5) . 2_555 no C26 H23 3.05(7) . 3_555 no H2 Pd 3.26(8) . . no H3 H26" 2.52(12) . 7_555 no H4 H5 2.45(11) . 2_655 no H5 C4 2.93(8) . 2_655 no H5 H4 2.45(11) . 2_655 no H6 C13 2.88(7) . . no H6 C14 3.07(7) . . no H8 Pd 3.60(6) . . no H8 C13 3.00(6) . . no H9 Cl 3.08(6) . 3_565 no H10 Cl 3.14(6) . 5_555 no H10 C17 2.99(6) . 6_555 no H11 Cl 2.99(7) . 5_555 no H12 C1 2.64(6) . . no H12 C2 2.99(6) . . no H12 C24 2.82(6) . 5_555 no H12 H24 2.54(8) . 5_555 no H14 C7 2.90(7) . . no H14 C21 2.98(8) . 6_555 no H15 C3 2.95(6) . 6_555 no H16 C10 2.78(5) . 4_565 no H17 C19 2.76(6) . . no H17 H19 2.32(7) . . no H17 Pd 3.31(6) . 2_555 no H17 Cl 2.66(5) . 2_555 no H19 C17 2.58(4) . . no H19 H17 2.32(7) . . no H19 C19 2.81(6) . 2_555 no H19 C20 2.90(6) . 2_555 no H19 C25 2.80(5) . 2_555 no H19 C10 3.08(6) . 6_545 no H19 C11 3.06(5) . 6_545 no H21 Pd 2.72(6) . . no H21 N 2.69(6) . . no H22 Cl 2.87(6) . 3_555 no H22 C22 2.81(5) . 3_555 no H22 H22 2.48(8) . 3_555 no H23 Pd 3.62(7) . 3_555 no H23 C26 3.05(7) . 3_555 no H24 C24 2.56(5) . 2_555 no H24 H24 2.17(8) . 2_555 no H24 H12 2.54(8) . 5_445 no H26" C3 2.90(9) . 7_555 no H26" H3 2.52(12) . 7_555 no loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A # #D H A D - H H...A D...A D - H...A symm(A) # C17 H17 Cl .86(6) 2.66(5) 3.402(6) 144(5) 2_555 # End of Crystallographic Information File #=== COMPLEX 6 #=============================================================== data_s1420c #================================================================ # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H38 N2 P2 Pd , 2(Cl), 3.5(CH2 Cl2)' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2O)' _chemical_formula_sum '?' _chemical_formula_weight 1203.38 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #================================================================ # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 15.1653(18) _cell_length_b 19.369(2) _cell_length_c 20.3003(17) _cell_angle_alpha 100.755(9) _cell_angle_beta 99.828(8) _cell_angle_gamma 111.470(10) _cell_volume 5262.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method ? _exptl_crystal_F_000 2436 _exptl_absorpt_coefficient_mu 0.91 _exptl_absorpt_correction_type none #================================================================ # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Graphite _diffrn_measurement_device_type 'CAD4T' _diffrn_measurement_method '\w-scan' # number of measured reflections (redundant set) _diffrn_reflns_number ? _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.36 # number of unique reflections _reflns_number_total 19488 # number of observed reflections (> n sig(I)) _reflns_number_gt 11771 _reflns_threshold_expression >2sigma(i) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' #================================================================ # 8. REFINEMENT DATA _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'CALC W=1/[\S^2^(FO^2^)+(0.0675P)^2^+18.2225P] WHERE P=(FO^2^+2FC^2^)/3' _refine_ls_hydrogen_treatment 'H-atom refinement: see text' _refine_ls_number_reflns 18889 _refine_ls_number_parameters 1331 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1735 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.168 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.142 #================================================================ # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Pd1 Uani 0.15699(4) 0.23185(3) 0.68334(3) 1.000 0.0154(2) Cl1 Uani 0.11967(13) 0.17999(10) 0.79988(9) 1.000 0.0234(6) P1 Uani -0.00609(13) 0.18941(10) 0.64312(9) 1.000 0.0159(5) P2 Uani 0.19177(13) 0.35886(10) 0.70101(9) 1.000 0.0166(6) N1 Uani 0.3071(4) 0.2615(3) 0.7181(3) 1.000 0.0168(17) N2 Uani 0.1337(4) 0.1147(3) 0.6358(3) 1.000 0.0158(17) C11 Uani 0.1072(5) 0.3885(4) 0.6511(4) 1.000 0.021(2) C21 Uani 0.0610(5) 0.4311(4) 0.6823(4) 1.000 0.026(2) C31 Uani -0.0032(5) 0.4531(4) 0.6416(5) 1.000 0.030(3) C41 Uani -0.0213(6) 0.4313(5) 0.5705(5) 1.000 0.040(3) C51 Uani 0.0221(6) 0.3881(5) 0.5389(5) 1.000 0.040(3) C61 Uani 0.0869(6) 0.3681(4) 0.5796(4) 1.000 0.028(3) C71 Uani 0.2201(5) 0.4127(4) 0.7914(3) 1.000 0.0158(19) C81 Uani 0.2048(6) 0.3738(4) 0.8421(4) 1.000 0.028(3) C91 Uani 0.2268(6) 0.4151(5) 0.9094(4) 1.000 0.037(3) C101 Uani 0.2647(6) 0.4947(5) 0.9285(4) 1.000 0.036(3) C111 Uani 0.2813(6) 0.5333(5) 0.8786(4) 1.000 0.029(3) C121 Uani 0.2593(5) 0.4926(4) 0.8095(4) 1.000 0.021(2) C131 Uani 0.3042(5) 0.4050(4) 0.6763(3) 1.000 0.017(2) C141 Uani 0.3189(5) 0.4709(4) 0.6517(4) 1.000 0.023(2) C151 Uani 0.4061(5) 0.5115(4) 0.6373(4) 1.000 0.026(3) C161 Uani 0.4815(5) 0.4868(4) 0.6462(4) 1.000 0.023(2) C171 Uani 0.4695(5) 0.4224(4) 0.6704(4) 1.000 0.023(2) C181 Uani 0.3816(5) 0.3810(4) 0.6853(4) 1.000 0.021(2) C191 Uani 0.3814(5) 0.3175(4) 0.7131(4) 1.000 0.019(2) C201 Uani 0.3339(5) 0.2093(4) 0.7523(4) 1.000 0.019(2) C211 Uani 0.3690(5) 0.2320(5) 0.8239(4) 1.000 0.027(3) C221 Uani 0.4042(6) 0.1858(5) 0.8556(4) 1.000 0.039(3) C231 Uani 0.4043(6) 0.1198(5) 0.8171(4) 1.000 0.035(3) C241 Uani 0.3686(5) 0.0982(4) 0.7464(4) 1.000 0.025(2) C251 Uani 0.3323(5) 0.1421(4) 0.7122(4) 1.000 0.018(2) C261 Uani 0.2998(5) 0.1188(4) 0.6359(4) 1.000 0.0183(19) C271 Uani 0.3603(6) 0.1040(4) 0.5968(4) 1.000 0.027(3) C281 Uani 0.3302(5) 0.0755(4) 0.5257(4) 1.000 0.026(3) C291 Uani 0.2361(5) 0.0626(4) 0.4908(4) 1.000 0.025(2) C301 Uani 0.1735(5) 0.0773(4) 0.5282(4) 1.000 0.022(2) C311 Uani 0.2045(5) 0.1047(4) 0.5993(4) 1.000 0.0173(19) C321 Uani 0.0621(5) 0.0514(4) 0.6330(3) 1.000 0.016(2) C331 Uani -0.0260(5) 0.0428(4) 0.6565(4) 1.000 0.019(2) C341 Uani -0.0733(5) -0.0269(4) 0.6708(3) 1.000 0.018(2) C351 Uani -0.1584(5) -0.0419(4) 0.6934(4) 1.000 0.022(2) C361 Uani -0.1962(6) 0.0135(4) 0.7012(4) 1.000 0.026(2) C371 Uani -0.1496(5) 0.0824(4) 0.6857(4) 1.000 0.021(2) C381 Uani -0.0638(5) 0.0991(4) 0.6638(3) 1.000 0.015(2) C391 Uani -0.0639(5) 0.2475(4) 0.6809(4) 1.000 0.020(2) C401 Uani -0.0434(5) 0.2686(4) 0.7527(4) 1.000 0.024(3) C411 Uani -0.0915(6) 0.3083(4) 0.7852(5) 1.000 0.033(3) C421 Uani -0.1579(6) 0.3274(5) 0.7462(5) 1.000 0.036(3) C431 Uani -0.1782(5) 0.3068(4) 0.6747(4) 1.000 0.029(3) C441 Uani -0.1317(5) 0.2671(4) 0.6411(4) 1.000 0.025(3) C451 Uani -0.0461(5) 0.1657(4) 0.5494(4) 1.000 0.021(2) C461 Uani -0.1451(6) 0.1284(4) 0.5143(4) 1.000 0.030(3) C471 Uani -0.1746(7) 0.1128(5) 0.4434(4) 1.000 0.035(3) C481 Uani -0.1049(7) 0.1331(5) 0.4068(4) 1.000 0.037(3) C491 Uani -0.0064(7) 0.1683(5) 0.4401(4) 1.000 0.032(3) C501 Uani 0.0225(6) 0.1835(4) 0.5107(4) 1.000 0.029(3) Pd2 Uani 0.17064(4) 0.25634(3) 0.18083(3) 1.000 0.0157(2) P3 Uani 0.00681(13) 0.21212(10) 0.14163(9) 1.000 0.0169(6) P4 Uani 0.20516(13) 0.38369(10) 0.19723(10) 1.000 0.0173(6) N3 Uani 0.3221(4) 0.2872(3) 0.2146(3) 1.000 0.0159(17) N4 Uani 0.1452(4) 0.1375(3) 0.1381(3) 1.000 0.0184(17) C12 Uani 0.1179(5) 0.4108(4) 0.1473(4) 1.000 0.020(2) C22 Uani 0.0764(5) 0.4567(4) 0.1796(4) 1.000 0.025(3) C32 Uani 0.0092(6) 0.4757(4) 0.1396(4) 1.000 0.030(3) C42 Uani -0.0148(6) 0.4508(5) 0.0682(5) 1.000 0.035(3) C52 Uani 0.0274(6) 0.4072(5) 0.0363(4) 1.000 0.033(3) C62 Uani 0.0938(6) 0.3870(4) 0.0752(4) 1.000 0.028(3) C72 Uani 0.2343(5) 0.4403(4) 0.2870(4) 1.000 0.018(2) C82 Uani 0.2100(6) 0.4063(4) 0.3388(4) 1.000 0.027(3) C92 Uani 0.2297(7) 0.4512(5) 0.4052(4) 1.000 0.042(3) C102 Uani 0.2768(6) 0.5303(5) 0.4213(4) 1.000 0.034(3) C112 Uani 0.3034(6) 0.5650(5) 0.3691(4) 1.000 0.030(3) C122 Uani 0.2818(5) 0.5209(4) 0.3027(4) 1.000 0.023(3) C132 Uani 0.3174(5) 0.4293(4) 0.1713(4) 1.000 0.019(2) C142 Uani 0.3283(6) 0.4926(4) 0.1445(4) 1.000 0.030(3) C152 Uani 0.4163(6) 0.5328(5) 0.1293(4) 1.000 0.031(3) C162 Uani 0.4930(6) 0.5111(5) 0.1412(4) 1.000 0.029(3) C172 Uani 0.4827(5) 0.4495(4) 0.1689(4) 1.000 0.021(2) C182 Uani 0.3952(5) 0.4078(4) 0.1832(4) 1.000 0.019(2) C192 Uani 0.3939(5) 0.3435(4) 0.2116(4) 1.000 0.019(2) C202 Uani 0.3497(5) 0.2369(4) 0.2509(3) 1.000 0.017(2) C212 Uani 0.3863(6) 0.2615(4) 0.3218(4) 1.000 0.027(3) C222 Uani 0.4221(6) 0.2193(5) 0.3577(4) 1.000 0.030(3) C232 Uani 0.4196(5) 0.1502(5) 0.3200(4) 1.000 0.032(3) C242 Uani 0.3826(5) 0.1252(4) 0.2489(4) 1.000 0.025(3) C252 Uani 0.3446(5) 0.1670(4) 0.2126(4) 1.000 0.018(2) C262 Uani 0.3089(5) 0.1403(4) 0.1362(4) 1.000 0.021(2) C272 Uani 0.3692(6) 0.1234(5) 0.0969(4) 1.000 0.031(3) C282 Uani 0.3379(6) 0.0938(5) 0.0261(4) 1.000 0.037(3) C292 Uani 0.2431(6) 0.0785(5) -0.0075(4) 1.000 0.031(3) C302 Uani 0.1808(6) 0.0944(4) 0.0290(4) 1.000 0.026(3) C312 Uani 0.2148(5) 0.1256(4) 0.1000(4) 1.000 0.021(2) C322 Uani 0.0753(5) 0.0764(4) 0.1375(4) 1.000 0.019(2) C332 Uani -0.0123(5) 0.0686(4) 0.1623(4) 1.000 0.019(2) C342 Uani -0.0606(5) 0.0002(4) 0.1769(4) 1.000 0.021(2) C352 Uani -0.1445(5) -0.0118(4) 0.2008(4) 1.000 0.023(2) C362 Uani -0.1793(6) 0.0436(4) 0.2093(4) 1.000 0.027(3) C372 Uani -0.1325(5) 0.1126(4) 0.1933(4) 1.000 0.022(2) C382 Uani -0.0489(5) 0.1266(4) 0.1703(3) 1.000 0.016(2) C392 Uani -0.0555(5) 0.2700(4) 0.1711(4) 1.000 0.017(2) C402 Uani -0.0370(5) 0.3000(4) 0.2418(4) 1.000 0.025(3) C412 Uani -0.0850(6) 0.3418(4) 0.2680(5) 1.000 0.031(3) C422 Uani -0.1543(6) 0.3532(5) 0.2230(5) 1.000 0.036(3) C432 Uani -0.1733(6) 0.3250(4) 0.1536(5) 1.000 0.036(3) C442 Uani -0.1244(5) 0.2832(4) 0.1252(4) 1.000 0.024(2) C452 Uani -0.0368(5) 0.1760(4) 0.0474(4) 1.000 0.024(2) C462 Uani -0.1345(6) 0.1277(4) 0.0154(4) 1.000 0.028(3) C472 Uani -0.1650(7) 0.1007(5) -0.0560(5) 1.000 0.042(3) C482 Uani -0.0974(8) 0.1217(5) -0.0951(5) 1.000 0.043(3) C492 Uani -0.0022(7) 0.1685(5) -0.0645(4) 1.000 0.037(3) C502 Uani 0.0297(6) 0.1962(4) 0.0071(4) 1.000 0.027(3) Cl19 Uani 0.2174(2) 0.61731(16) 0.08744(14) 1.000 0.0618(10) Cl20 Uiso 0.3363(7) 0.7527(10) 0.0411(7) 0.52(3) 0.078(4) C7 Uani 0.3216(10) 0.7045(6) 0.1053(6) 1.000 0.080(5) Cl22 Uiso 0.3472(17) 0.710(2) 0.0286(8) 0.32(3) 0.114(11) Cl21 Uiso 0.265(3) 0.7661(12) 0.0837(13) 0.158(10) 0.118(15) Cl15 Uiso 0.5375(5) 0.0239(3) 0.6745(4) 0.607(14) 0.073(2) Cl16 Uiso 0.6847(7) 0.1209(5) 0.7991(3) 0.607(14) 0.080(3) C6 Uani 0.6198(8) 0.1207(6) 0.7255(6) 1.000 0.064(4) Cl18 Uiso 0.5951(11) 0.0685(10) 0.6510(5) 0.393(14) 0.097(6) Cl17 Uiso 0.6228(17) 0.0824(13) 0.7981(9) 0.393(14) 0.139(7) Cl5 Uani 0.3221(3) 0.25552(16) 0.51623(16) 1.000 0.0908(16) Cl6 Uani 0.4414(2) 0.39167(15) 0.48132(13) 1.000 0.0719(10) C1 Uani 0.3236(8) 0.3298(5) 0.4810(5) 1.000 0.058(4) Cl7 Uani 0.4825(2) 0.37123(19) -0.00543(14) 1.000 0.0870(11) Cl8 Uani 0.2955(2) 0.28631(18) 0.01782(16) 1.000 0.0765(11) C2 Uani 0.4161(8) 0.2974(6) 0.0286(5) 1.000 0.059(4) Cl9 Uani 0.7668(2) 0.38243(18) 0.39270(15) 1.000 0.0667(11) Cl10 Uani 0.7490(3) 0.2262(2) 0.3477(2) 1.000 0.108(2) C3 Uani 0.6908(8) 0.2884(7) 0.3396(6) 1.000 0.068(5) Cl11 Uani 0.6581(2) 0.26230(14) 0.50181(12) 1.000 0.0542(9) Cl12 Uani 0.5820(3) 0.10729(19) 0.5127(3) 1.000 0.144(3) C4 Uani 0.5816(8) 0.1974(5) 0.5376(5) 1.000 0.057(4) Cl13 Uani 0.6147(4) 0.1047(3) 0.0567(4) 1.000 0.181(4) Cl14 Uani 0.5783(3) 0.0731(3) 0.1846(4) 1.000 0.161(3) C5 Uani 0.6322(9) 0.1416(9) 0.1446(13) 1.000 0.155(11) Cl2 Uani 0.13642(13) 0.21416(10) 0.30874(9) 1.000 0.0246(6) Cl3 Uani 0.41078(14) 0.71306(11) 0.28358(11) 1.000 0.0338(7) Cl4 Uani 0.58694(15) 0.30788(13) 0.18176(13) 1.000 0.0445(8) H21 Uiso 0.0731(11) 0.4453(12) 0.732(4) 1.000 0.0310 H31 Uiso -0.035(3) 0.484(3) 0.6636(19) 1.000 0.0360 H41 Uiso -0.061(4) 0.4453(15) 0.545(3) 1.000 0.0480 H51 Uiso 0.0099(14) 0.3746(16) 0.497(5) 1.000 0.0470 H61 Uiso 0.120(3) 0.338(2) 0.5564(18) 1.000 0.0330 H81 Uiso 0.178(2) 0.317(5) 0.8297(11) 1.000 0.0330 H91 Uiso 0.2168(12) 0.391(3) 0.941(3) 1.000 0.0450 H101 Uiso 0.27870 0.52180 0.97460 1.000 0.0420 H111 Uiso 0.308(2) 0.588(5) 0.8912(11) 1.000 0.0340 H121 Uiso 0.2690(10) 0.515(2) 0.781(3) 1.000 0.0260 H141 Uiso 0.269(4) 0.4872(14) 0.6451(7) 1.000 0.0280 H151 Uiso 0.4150(9) 0.559(4) 0.6206(13) 1.000 0.0310 H161 Uiso 0.542(5) 0.515(2) 0.6356(9) 1.000 0.0280 H171 Uiso 0.515(4) 0.4083(14) 0.6761(6) 1.000 0.0280 H191 Uiso 0.438(5) 0.3173(4) 0.7282(13) 1.000 0.0230 H211 Uiso 0.3691(5) 0.277(4) 0.850(2) 1.000 0.0320 H221 Uiso 0.424(2) 0.1976(15) 0.895(5) 1.000 0.0470 H231 Uiso 0.426(2) 0.093(3) 0.837(2) 1.000 0.0420 H241 Uiso 0.3686(5) 0.050(4) 0.719(2) 1.000 0.0300 H271 Uiso 0.417(6) 0.1125(9) 0.617(2) 1.000 0.0330 H281 Uiso 0.373(4) 0.0650(10) 0.501(2) 1.000 0.0310 H291 Uiso 0.2165(18) 0.0454(16) 0.446(4) 1.000 0.0300 H301 Uiso 0.107(5) 0.0681(8) 0.5039(19) 1.000 0.0270 H321 Uiso 0.0671(6) 0.006(4) 0.6139(15) 1.000 0.0200 H341 Uiso -0.047(2) -0.065(3) 0.6650(6) 1.000 0.0220 H351 Uiso -0.190(3) -0.089(4) 0.7033(9) 1.000 0.0270 H361 Uiso -0.253(5) 0.0045(9) 0.7166(14) 1.000 0.0310 H371 Uiso -0.175(2) 0.116(3) 0.6898(5) 1.000 0.0250 H401 Uiso 0.005(4) 0.2558(11) 0.781(2) 1.000 0.0290 H411 Uiso -0.0787(13) 0.3218(13) 0.833(4) 1.000 0.0400 H421 Uiso -0.188(3) 0.354(3) 0.767(2) 1.000 0.0430 H431 Uiso -0.224(4) 0.3198(12) 0.649(2) 1.000 0.0350 H441 Uiso -0.1455(12) 0.2533(12) 0.591(4) 1.000 0.0300 H461 Uiso -0.193(4) 0.1136(13) 0.540(2) 1.000 0.0350 H471 Uiso -0.245(6) 0.087(2) 0.419(2) 1.000 0.0420 H481 Uiso -0.122(2) 0.1245(11) 0.366(5) 1.000 0.0450 H491 Uiso 0.032(4) 0.1790(13) 0.420(2) 1.000 0.0390 H501 Uiso 0.086(6) 0.205(2) 0.532(2) 1.000 0.0350 H22 Uiso 0.0934(15) 0.4744(15) 0.228(4) 1.000 0.0290 H32 Uiso -0.020(3) 0.506(3) 0.1614(19) 1.000 0.0360 H42 Uiso -0.062(4) 0.4643(12) 0.040(2) 1.000 0.0420 H52 Uiso 0.0129(16) 0.3926(15) -0.007(4) 1.000 0.0400 H62 Uiso 0.123(3) 0.357(3) 0.0528(19) 1.000 0.0340 H82 Uiso 0.179(3) 0.351(5) 0.3287(9) 1.000 0.0330 H92 Uiso 0.214(2) 0.432(2) 0.434(3) 1.000 0.0500 H102 Uiso 0.2914(14) 0.562(3) 0.469(4) 1.000 0.0410 H112 Uiso 0.337(3) 0.621(5) 0.3799(10) 1.000 0.0360 H122 Uiso 0.2973(15) 0.543(2) 0.270(3) 1.000 0.0270 H142 Uiso 0.280(5) 0.5070(14) 0.1372(8) 1.000 0.0360 H152 Uiso 0.4229(8) 0.574(4) 0.1112(17) 1.000 0.0370 H162 Uiso 0.550(5) 0.537(2) 0.1310(10) 1.000 0.0350 H172 Uiso 0.538(4) 0.4349(12) 0.1786(8) 1.000 0.0250 H192 Uiso 0.456(5) 0.3447(4) 0.2302(15) 1.000 0.0230 H212 Uiso 0.3871(6) 0.307(4) 0.346(2) 1.000 0.0320 H222 Uiso 0.449(2) 0.2373(16) 0.408(4) 1.000 0.0360 H232 Uiso 0.440(2) 0.125(3) 0.340(2) 1.000 0.0390 H242 Uiso 0.3829(5) 0.077(4) 0.223(2) 1.000 0.0300 H272 Uiso 0.425(6) 0.1314(9) 0.117(2) 1.000 0.0370 H282 Uiso 0.382(4) 0.0837(10) 0.000(2) 1.000 0.0440 H292 Uiso 0.223(2) 0.0590(19) -0.051(4) 1.000 0.0380 H302 Uiso 0.120(5) 0.0848(10) 0.007(2) 1.000 0.0320 H322 Uiso 0.0800(6) 0.031(4) 0.1191(15) 1.000 0.0230 H342 Uiso -0.0404(19) -0.033(3) 0.1717(6) 1.000 0.0250 H352 Uiso -0.175(3) -0.055(4) 0.2103(9) 1.000 0.0280 H362 Uiso -0.235(5) 0.0355(8) 0.2259(15) 1.000 0.0320 H372 Uiso -0.159(2) 0.152(3) 0.1985(5) 1.000 0.0270 H402 Uiso 0.002(4) 0.2929(8) 0.268(3) 1.000 0.0300 H412 Uiso -0.0710(14) 0.3626(19) 0.316(4) 1.000 0.0370 H422 Uiso -0.189(3) 0.381(3) 0.2408(17) 1.000 0.0430 H432 Uiso -0.216(4) 0.3329(9) 0.127(3) 1.000 0.0430 H442 Uiso -0.1379(12) 0.2633(16) 0.074(4) 1.000 0.0290 H462 Uiso -0.179(4) 0.1137(13) 0.042(2) 1.000 0.0340 H472 Uiso -0.231(6) 0.069(3) -0.078(2) 1.000 0.0500 H482 Uiso -0.120(2) 0.1019(19) -0.147(5) 1.000 0.0520 H492 Uiso 0.039(4) 0.1811(14) -0.090(3) 1.000 0.0430 H502 Uiso 0.093(6) 0.227(3) 0.0278(18) 1.000 0.0320 H320 Uiso 0.37920 0.69410 0.11760 0.52(3) 0.1080 H310 Uiso 0.32120 0.73960 0.14610 0.52(3) 0.1080 H330 Uiso 0.36490 0.70000 0.07620 0.158(10) 0.1080 H340 Uiso 0.35790 0.72210 0.15380 0.158(10) 0.1080 H350 Uiso 0.30790 0.74790 0.12500 0.32(3) 0.1080 H360 Uiso 0.37640 0.70450 0.13780 0.32(3) 0.1080 H620 Uiso 0.58190 0.15050 0.73510 0.607(14) 0.0870 H610 Uiso 0.66370 0.14500 0.69900 0.607(14) 0.0870 H630 Uiso 0.57260 0.14360 0.72540 0.393(14) 0.0870 H640 Uiso 0.68360 0.16250 0.73370 0.393(14) 0.0870 H11 Uiso 0.29500 0.35940 0.50700 1.000 0.0780 H201 Uiso 0.28300 0.30850 0.43350 1.000 0.0780 H12 Uiso 0.44710 0.30950 0.07770 1.000 0.0790 H202 Uiso 0.41740 0.24940 0.00550 1.000 0.0790 H13 Uiso 0.62960 0.26950 0.35280 1.000 0.0910 H203 Uiso 0.67570 0.28960 0.29150 1.000 0.0910 H14 Uiso 0.60310 0.21640 0.58790 1.000 0.0770 H204 Uiso 0.51520 0.19350 0.52290 1.000 0.0770 H15 Uiso 0.70210 0.16690 0.16680 1.000 0.2090 H205 Uiso 0.60570 0.18030 0.15100 1.000 0.2090 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 Pd1 0.0145(3) 0.0131(3) 0.0217(3) 0.0063(2) 0.0057(2) 0.0079(2) Cl1 0.0297(10) 0.0212(9) 0.0259(10) 0.0121(8) 0.0112(8) 0.0131(8) P1 0.0153(9) 0.0153(9) 0.0222(10) 0.0081(8) 0.0069(8) 0.0094(8) P2 0.0177(9) 0.0164(10) 0.0209(10) 0.0072(8) 0.0077(8) 0.0105(8) N1 0.014(3) 0.014(3) 0.021(3) 0.001(2) 0.002(2) 0.007(3) N2 0.017(3) 0.021(3) 0.013(3) 0.009(2) 0.001(2) 0.011(3) C11 0.020(4) 0.020(4) 0.028(4) 0.010(3) 0.008(3) 0.010(3) C21 0.025(4) 0.024(4) 0.028(4) 0.006(3) 0.003(3) 0.012(3) C31 0.022(4) 0.021(4) 0.055(6) 0.014(4) 0.009(4) 0.015(3) C41 0.035(5) 0.037(5) 0.056(6) 0.028(5) -0.001(4) 0.023(4) C51 0.039(5) 0.037(5) 0.040(5) 0.016(4) -0.002(4) 0.015(4) C61 0.033(5) 0.032(5) 0.030(5) 0.018(4) 0.011(4) 0.021(4) C71 0.009(3) 0.011(3) 0.021(4) 0.001(3) 0.001(3) 0.000(3) C81 0.040(5) 0.016(4) 0.028(4) 0.009(3) 0.012(4) 0.010(4) C91 0.054(6) 0.030(5) 0.029(5) 0.018(4) 0.016(4) 0.011(4) C101 0.043(5) 0.034(5) 0.026(5) -0.001(4) 0.009(4) 0.016(4) C111 0.026(4) 0.028(4) 0.028(5) 0.000(4) 0.004(3) 0.012(4) C121 0.016(4) 0.022(4) 0.034(4) 0.011(3) 0.009(3) 0.014(3) C131 0.016(4) 0.010(3) 0.020(4) 0.002(3) 0.005(3) 0.002(3) C141 0.027(4) 0.016(4) 0.032(4) 0.006(3) 0.008(3) 0.014(3) C151 0.027(4) 0.022(4) 0.035(5) 0.021(4) 0.012(4) 0.010(3) C161 0.020(4) 0.020(4) 0.021(4) 0.006(3) 0.007(3) -0.002(3) C171 0.021(4) 0.028(4) 0.022(4) 0.010(3) 0.009(3) 0.009(3) C181 0.019(4) 0.013(4) 0.029(4) 0.005(3) 0.004(3) 0.007(3) C191 0.014(4) 0.023(4) 0.022(4) 0.004(3) 0.004(3) 0.011(3) C201 0.021(4) 0.012(4) 0.027(4) 0.009(3) 0.012(3) 0.005(3) C211 0.025(4) 0.032(5) 0.026(4) 0.010(4) 0.002(3) 0.016(4) C221 0.041(5) 0.053(6) 0.024(5) 0.015(4) 0.000(4) 0.022(5) C231 0.038(5) 0.035(5) 0.046(6) 0.023(4) 0.012(4) 0.023(4) C241 0.025(4) 0.027(4) 0.031(4) 0.013(3) 0.011(3) 0.017(3) C251 0.013(4) 0.020(4) 0.021(4) 0.008(3) 0.002(3) 0.007(3) C261 0.012(3) 0.011(3) 0.027(4) 0.008(3) 0.005(3) -0.002(3) C271 0.020(4) 0.024(4) 0.040(5) 0.010(4) 0.010(4) 0.011(3) C281 0.021(4) 0.028(4) 0.031(5) 0.004(3) 0.013(4) 0.012(3) C291 0.024(4) 0.019(4) 0.026(4) -0.001(3) 0.005(3) 0.006(3) C301 0.022(4) 0.015(4) 0.024(4) 0.000(3) 0.001(3) 0.007(3) C311 0.011(3) 0.012(3) 0.031(4) 0.005(3) 0.009(3) 0.006(3) C321 0.017(4) 0.017(4) 0.022(4) 0.007(3) 0.006(3) 0.013(3) C331 0.019(4) 0.021(4) 0.020(4) 0.009(3) 0.004(3) 0.010(3) C341 0.022(4) 0.012(4) 0.022(4) 0.006(3) 0.006(3) 0.007(3) C351 0.019(4) 0.016(4) 0.030(4) 0.011(3) 0.005(3) 0.003(3) C361 0.028(4) 0.025(4) 0.028(4) 0.009(3) 0.011(4) 0.011(4) C371 0.020(4) 0.014(4) 0.033(4) 0.009(3) 0.011(3) 0.008(3) C381 0.018(4) 0.008(3) 0.022(4) 0.001(3) 0.008(3) 0.008(3) C391 0.015(4) 0.017(4) 0.033(4) 0.011(3) 0.009(3) 0.010(3) C401 0.022(4) 0.017(4) 0.036(5) 0.007(3) 0.012(3) 0.010(3) C411 0.035(5) 0.029(5) 0.034(5) 0.000(4) 0.014(4) 0.013(4) C421 0.024(4) 0.032(5) 0.052(6) -0.002(4) 0.008(4) 0.018(4) C431 0.013(4) 0.024(4) 0.049(5) 0.003(4) 0.002(4) 0.013(3) C441 0.017(4) 0.023(4) 0.035(5) 0.008(3) 0.004(3) 0.008(3) C451 0.022(4) 0.019(4) 0.026(4) 0.010(3) 0.008(3) 0.011(3) C461 0.026(4) 0.019(4) 0.041(5) 0.007(4) 0.004(4) 0.009(3) C471 0.044(5) 0.031(5) 0.027(5) 0.006(4) 0.000(4) 0.018(4) C481 0.065(7) 0.028(5) 0.022(4) 0.006(4) 0.003(4) 0.026(5) C491 0.054(6) 0.039(5) 0.023(4) 0.020(4) 0.025(4) 0.030(5) C501 0.035(5) 0.019(4) 0.035(5) 0.006(3) 0.012(4) 0.012(4) Pd2 0.0144(3) 0.0149(3) 0.0219(3) 0.0080(2) 0.0053(2) 0.0087(2) P3 0.0156(9) 0.0191(10) 0.0219(10) 0.0086(8) 0.0074(8) 0.0111(8) P4 0.0166(9) 0.0164(10) 0.0253(10) 0.0109(8) 0.0085(8) 0.0100(8) N3 0.016(3) 0.010(3) 0.017(3) 0.003(2) -0.001(2) 0.003(3) N4 0.014(3) 0.018(3) 0.024(3) 0.004(3) 0.003(3) 0.009(3) C12 0.019(4) 0.014(4) 0.029(4) 0.011(3) 0.006(3) 0.007(3) C22 0.022(4) 0.024(4) 0.034(5) 0.014(3) 0.013(3) 0.011(3) C32 0.027(4) 0.027(4) 0.042(5) 0.010(4) 0.002(4) 0.019(4) C42 0.036(5) 0.035(5) 0.046(6) 0.021(4) 0.007(4) 0.025(4) C52 0.042(5) 0.035(5) 0.027(5) 0.018(4) 0.008(4) 0.016(4) C62 0.033(5) 0.021(4) 0.032(5) 0.011(3) 0.008(4) 0.012(4) C72 0.014(4) 0.015(4) 0.026(4) 0.004(3) 0.002(3) 0.008(3) C82 0.037(5) 0.015(4) 0.031(5) 0.011(3) 0.006(4) 0.011(3) C92 0.069(7) 0.036(5) 0.027(5) 0.013(4) 0.023(5) 0.022(5) C102 0.039(5) 0.028(5) 0.027(5) 0.001(4) -0.002(4) 0.013(4) C112 0.023(4) 0.023(4) 0.040(5) -0.001(4) 0.001(4) 0.013(3) C122 0.016(4) 0.023(4) 0.034(5) 0.012(4) 0.008(3) 0.011(3) C132 0.015(4) 0.019(4) 0.028(4) 0.009(3) 0.010(3) 0.009(3) C142 0.029(4) 0.031(5) 0.045(5) 0.022(4) 0.018(4) 0.019(4) C152 0.029(5) 0.030(5) 0.043(5) 0.026(4) 0.018(4) 0.012(4) C162 0.026(4) 0.033(5) 0.037(5) 0.018(4) 0.019(4) 0.014(4) C172 0.021(4) 0.019(4) 0.021(4) 0.005(3) 0.003(3) 0.006(3) C182 0.021(4) 0.019(4) 0.019(4) 0.005(3) 0.004(3) 0.010(3) C192 0.019(4) 0.019(4) 0.024(4) 0.008(3) 0.006(3) 0.012(3) C202 0.013(3) 0.022(4) 0.016(4) 0.010(3) 0.003(3) 0.005(3) C212 0.033(5) 0.023(4) 0.030(4) 0.012(3) 0.009(4) 0.015(4) C222 0.030(5) 0.040(5) 0.027(4) 0.020(4) 0.005(4) 0.018(4) C232 0.024(4) 0.043(5) 0.049(6) 0.036(5) 0.012(4) 0.023(4) C242 0.015(4) 0.025(4) 0.039(5) 0.010(4) 0.005(3) 0.013(3) C252 0.009(3) 0.013(4) 0.031(4) 0.009(3) 0.006(3) 0.001(3) C262 0.020(4) 0.013(4) 0.031(4) 0.009(3) 0.009(3) 0.007(3) C272 0.020(4) 0.040(5) 0.037(5) 0.006(4) 0.009(4) 0.019(4) C282 0.028(5) 0.047(6) 0.038(5) 0.002(4) 0.015(4) 0.020(4) C292 0.038(5) 0.033(5) 0.021(4) 0.002(4) 0.010(4) 0.015(4) C302 0.018(4) 0.031(4) 0.031(5) 0.006(4) 0.005(3) 0.013(3) C312 0.021(4) 0.023(4) 0.027(4) 0.009(3) 0.008(3) 0.015(3) C322 0.019(4) 0.014(4) 0.025(4) 0.005(3) 0.005(3) 0.007(3) C332 0.016(4) 0.020(4) 0.024(4) 0.009(3) 0.005(3) 0.010(3) C342 0.019(4) 0.026(4) 0.024(4) 0.012(3) 0.002(3) 0.014(3) C352 0.022(4) 0.016(4) 0.023(4) 0.011(3) 0.001(3) -0.001(3) C362 0.026(4) 0.033(5) 0.034(5) 0.019(4) 0.014(4) 0.018(4) C372 0.018(4) 0.025(4) 0.033(4) 0.015(3) 0.012(3) 0.014(3) C382 0.014(4) 0.009(3) 0.022(4) 0.003(3) 0.001(3) 0.004(3) C392 0.008(3) 0.012(4) 0.027(4) 0.004(3) 0.002(3) 0.000(3) C402 0.024(4) 0.019(4) 0.034(5) 0.007(3) 0.010(3) 0.009(3) C412 0.031(5) 0.022(4) 0.045(5) 0.008(4) 0.019(4) 0.012(4) C422 0.035(5) 0.025(4) 0.064(7) 0.014(4) 0.032(5) 0.021(4) C432 0.025(4) 0.028(5) 0.063(6) 0.019(4) 0.011(4) 0.018(4) C442 0.022(4) 0.023(4) 0.031(4) 0.011(3) 0.006(3) 0.011(3) C452 0.022(4) 0.024(4) 0.032(4) 0.013(3) 0.006(3) 0.015(3) C462 0.031(4) 0.016(4) 0.032(5) 0.005(3) 0.000(4) 0.007(3) C472 0.040(5) 0.030(5) 0.043(6) 0.005(4) -0.010(4) 0.012(4) C482 0.069(7) 0.039(5) 0.027(5) 0.007(4) 0.008(5) 0.031(5) C492 0.055(6) 0.036(5) 0.027(5) 0.008(4) 0.017(4) 0.025(5) C502 0.033(5) 0.026(4) 0.034(5) 0.012(4) 0.020(4) 0.020(4) Cl19 0.0733(19) 0.0611(17) 0.0494(16) 0.0057(13) -0.0007(14) 0.0378(15) C7 0.107(11) 0.053(7) 0.072(9) 0.022(6) 0.007(8) 0.030(7) C6 0.066(7) 0.065(7) 0.094(9) 0.047(7) 0.029(7) 0.046(6) Cl5 0.161(4) 0.0423(16) 0.068(2) 0.0292(15) 0.048(2) 0.0259(19) Cl6 0.085(2) 0.0506(16) 0.0397(15) -0.0048(12) 0.0251(14) -0.0122(15) C1 0.069(7) 0.037(6) 0.055(7) 0.016(5) 0.021(6) 0.004(5) Cl7 0.078(2) 0.085(2) 0.0441(16) -0.0025(15) 0.0239(15) -0.0194(17) Cl8 0.0652(19) 0.0669(19) 0.075(2) 0.0245(16) 0.0132(16) 0.0022(15) C2 0.070(7) 0.057(7) 0.040(6) -0.003(5) 0.021(5) 0.020(6) Cl9 0.089(2) 0.081(2) 0.0662(18) 0.0394(16) 0.0358(16) 0.0584(18) Cl10 0.163(4) 0.097(3) 0.155(4) 0.091(3) 0.109(3) 0.096(3) C3 0.070(8) 0.088(9) 0.081(8) 0.058(7) 0.037(7) 0.048(7) Cl11 0.0676(17) 0.0501(15) 0.0372(13) 0.0151(11) 0.0161(12) 0.0132(13) Cl12 0.062(2) 0.052(2) 0.346(7) 0.071(3) 0.084(3) 0.0324(17) C4 0.056(7) 0.047(6) 0.059(7) 0.010(5) 0.023(5) 0.009(5) Cl13 0.100(4) 0.135(5) 0.328(9) 0.046(5) 0.105(5) 0.056(3) Cl14 0.086(3) 0.101(3) 0.342(8) 0.097(4) 0.066(4) 0.068(3) C5 0.043(8) 0.085(11) 0.37(3) 0.075(16) 0.060(14) 0.053(8) Cl2 0.0294(10) 0.0211(9) 0.0262(10) 0.0107(8) 0.0075(8) 0.0113(8) Cl3 0.0260(10) 0.0349(11) 0.0519(13) 0.0213(10) 0.0150(9) 0.0183(9) Cl4 0.0329(12) 0.0418(13) 0.0783(17) 0.0331(12) 0.0239(12) 0.0246(10) #================================================================ # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.8025(19) . . yes Pd1 P1 2.243(2) . . yes Pd1 P2 2.262(2) . . yes Pd1 N1 2.086(6) . . yes Pd1 N2 2.164(6) . . yes P1 C381 1.811(8) . . yes P1 C391 1.803(8) . . yes P1 C451 1.810(8) . . yes P2 C11 1.820(8) . . yes P2 C71 1.824(6) . . yes P2 C131 1.817(8) . . yes N1 C191 1.281(10) . . yes N1 C201 1.461(10) . . yes N2 C311 1.452(10) . . yes N2 C321 1.290(10) . . yes C11 C21 1.397(11) . . no C11 C61 1.379(11) . . no C21 C31 1.405(12) . . no C31 C41 1.375(14) . . no C41 C51 1.375(14) . . no C51 C61 1.385(13) . . no C71 C81 1.387(10) . . no C71 C121 1.387(11) . . no C81 C91 1.363(11) . . no C91 C101 1.382(13) . . no C101 C111 1.371(12) . . no C111 C121 1.391(11) . . no C131 C141 1.413(10) . . no C131 C181 1.409(11) . . no C141 C151 1.382(11) . . no C151 C161 1.390(11) . . no C161 C171 1.387(11) . . no C171 C181 1.399(11) . . no C181 C191 1.445(11) . . no C201 C211 1.384(11) . . no C201 C251 1.390(11) . . no C211 C221 1.395(13) . . no C221 C231 1.369(13) . . no C231 C241 1.369(11) . . no C241 C251 1.393(11) . . no C251 C261 1.470(11) . . no C261 C271 1.382(12) . . no C261 C311 1.409(11) . . no C271 C281 1.375(11) . . no C281 C291 1.389(11) . . no C291 C301 1.386(11) . . no C301 C311 1.373(11) . . no C321 C331 1.458(11) . . no C331 C341 1.389(11) . . no C331 C381 1.402(11) . . no C341 C351 1.392(11) . . no C351 C361 1.387(12) . . no C361 C371 1.386(11) . . no C371 C381 1.392(11) . . no C391 C401 1.385(11) . . no C391 C441 1.404(11) . . no C401 C411 1.394(12) . . no C411 C421 1.374(14) . . no C421 C431 1.379(12) . . no C431 C441 1.385(11) . . no C451 C461 1.390(12) . . no C451 C501 1.391(12) . . no C461 C471 1.372(11) . . no C471 C481 1.377(14) . . no C481 C491 1.375(15) . . no C491 C501 1.366(11) . . no C21 H21 0.96(8) . . no C31 H31 0.99(5) . . no C41 H41 0.88(6) . . no C51 H51 0.81(10) . . no C61 H61 1.00(4) . . no C81 H81 0.99(9) . . no C91 H91 0.86(6) . . no C101 H101 0.9293 . . no C111 H111 0.95(9) . . no C121 H121 0.79(5) . . no C141 H141 0.92(6) . . no C151 H151 1.01(7) . . no C161 H161 0.96(6) . . no C171 H171 0.83(6) . . no C191 H191 0.86(7) . . no C211 H211 0.93(6) . . no C221 H221 0.76(10) . . no C231 H231 0.84(5) . . no C241 H241 0.99(6) . . no C271 H271 0.83(8) . . no C281 H281 0.94(6) . . no C291 H291 0.87(8) . . no C301 H301 0.98(7) . . no C321 H321 0.93(6) . . no C341 H341 0.96(5) . . no C351 H351 0.94(7) . . no C361 H361 0.93(7) . . no C371 H371 0.87(5) . . no C401 H401 0.99(5) . . no C411 H411 0.92(8) . . no C421 H421 0.90(5) . . no C431 H431 0.93(5) . . no C441 H441 0.97(8) . . no C461 H461 0.96(5) . . no C471 H471 0.99(8) . . no C481 H481 0.79(10) . . no C491 H491 0.76(5) . . no C501 H501 0.89(8) . . no Pd2 P3 2.248(2) . . yes Pd2 P4 2.271(2) . . yes Pd2 N3 2.099(6) . . yes Pd2 N4 2.166(6) . . yes P3 C382 1.816(8) . . yes P3 C392 1.796(8) . . yes P3 C452 1.821(8) . . yes P4 C12 1.818(8) . . yes P4 C72 1.828(8) . . yes P4 C132 1.826(8) . . yes N3 C192 1.248(10) . . yes N3 C202 1.459(9) . . yes N4 C312 1.468(10) . . yes N4 C322 1.263(10) . . yes C12 C22 1.396(11) . . no C12 C62 1.389(11) . . no C22 C32 1.392(12) . . no C32 C42 1.377(12) . . no C42 C52 1.369(14) . . no C52 C62 1.387(13) . . no C72 C82 1.374(11) . . no C72 C122 1.404(11) . . no C82 C92 1.377(11) . . no C92 C102 1.377(13) . . no C102 C112 1.397(12) . . no C112 C122 1.367(11) . . no C132 C142 1.399(11) . . no C132 C182 1.387(11) . . no C142 C152 1.397(13) . . no C152 C162 1.374(14) . . no C162 C172 1.381(12) . . no C172 C182 1.390(11) . . no C182 C192 1.462(11) . . no C202 C212 1.373(10) . . no C202 C252 1.398(10) . . no C212 C222 1.381(12) . . no C222 C232 1.396(13) . . no C232 C242 1.377(11) . . no C242 C252 1.396(11) . . no C252 C262 1.475(11) . . no C262 C272 1.397(12) . . no C262 C312 1.387(11) . . no C272 C282 1.371(11) . . no C282 C292 1.378(13) . . no C292 C302 1.380(13) . . no C302 C312 1.379(11) . . no C322 C332 1.467(12) . . no C332 C342 1.375(11) . . no C332 C382 1.420(11) . . no C342 C352 1.395(11) . . no C352 C362 1.355(12) . . no C362 C372 1.393(11) . . no C372 C382 1.377(11) . . no C392 C402 1.381(11) . . no C392 C442 1.406(11) . . no C402 C412 1.368(12) . . no C412 C422 1.380(14) . . no C422 C432 1.351(14) . . no C432 C442 1.396(12) . . no C452 C462 1.387(12) . . no C452 C502 1.397(12) . . no C462 C472 1.378(12) . . no C472 C482 1.393(15) . . no C482 C492 1.348(15) . . no C492 C502 1.383(11) . . no C22 H22 0.93(8) . . no C32 H32 0.95(5) . . no C42 H42 0.98(5) . . no C52 H52 0.83(8) . . no C62 H62 0.95(5) . . no C82 H82 0.96(9) . . no C92 H92 0.78(5) . . no C102 H102 0.98(7) . . no C112 H112 0.98(9) . . no C122 H122 0.87(5) . . no C142 H142 0.87(7) . . no C152 H152 0.92(7) . . no C162 H162 0.91(7) . . no C172 H172 0.98(6) . . no C192 H192 0.94(7) . . no C212 H212 0.92(6) . . no C222 H222 0.98(8) . . no C232 H232 0.80(5) . . no C242 H242 0.98(6) . . no C272 H272 0.82(8) . . no C282 H282 0.97(6) . . no C292 H292 0.85(8) . . no C302 H302 0.89(7) . . no C322 H322 0.92(6) . . no C342 H342 0.81(5) . . no C352 H352 0.87(7) . . no C362 H362 0.93(7) . . no C372 H372 0.98(5) . . no C402 H402 0.79(6) . . no C412 H412 0.94(8) . . no C422 H422 0.95(5) . . no C432 H432 0.85(6) . . no C442 H442 1.00(8) . . no C462 H462 0.93(5) . . no C472 H472 0.93(8) . . no C482 H482 1.00(10) . . no C492 H492 0.87(6) . . no C502 H502 0.90(8) . . no Cl19 C7 1.762(13) . . yes Cl20 C7 1.74(2) . . yes Cl21 C7 1.78(4) . . yes Cl22 C7 1.68(2) . . yes C7 H310 0.9710 . . no C7 H320 0.9691 . . no C7 H330 0.9710 . . no C7 H340 0.9700 . . no C7 H350 0.9698 . . no C7 H360 0.9689 . . no Cl15 C6 1.807(13) . . yes Cl16 C6 1.641(14) . . yes Cl17 C6 1.77(2) . . yes Cl18 C6 1.552(16) . . yes C6 H610 0.9703 . . no C6 H620 0.9698 . . no C6 H630 0.9702 . . no C6 H640 0.9699 . . no Cl5 C1 1.717(10) . . yes Cl6 C1 1.747(12) . . yes C1 H11 0.9709 . . no C1 H201 0.9706 . . no Cl7 C2 1.757(12) . . yes Cl8 C2 1.731(13) . . yes C2 H12 0.9704 . . no C2 H202 0.9688 . . no Cl9 C3 1.765(13) . . yes Cl10 C3 1.749(14) . . yes C3 H13 0.9695 . . no C3 H203 0.9708 . . no Cl11 C4 1.736(11) . . yes Cl12 C4 1.727(11) . . yes C4 H14 0.9709 . . no C4 H204 0.9706 . . no Cl13 C5 1.73(3) . . yes Cl14 C5 1.71(2) . . yes C5 H15 0.9701 . . no C5 H205 0.9707 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd1 P1 86.86(7) . . . yes Cl1 Pd1 P2 112.39(6) . . . yes Cl1 Pd1 N1 92.08(17) . . . yes Cl1 Pd1 N2 85.59(16) . . . yes P1 Pd1 P2 96.56(8) . . . yes P1 Pd1 N1 175.08(17) . . . yes P1 Pd1 N2 85.08(18) . . . yes P2 Pd1 N1 88.29(17) . . . yes P2 Pd1 N2 161.98(16) . . . yes N1 Pd1 N2 90.0(2) . . . yes Pd1 P1 C381 108.2(3) . . . yes Pd1 P1 C391 117.4(3) . . . yes Pd1 P1 C451 113.0(3) . . . yes C381 P1 C391 103.1(4) . . . yes C381 P1 C451 104.6(3) . . . yes C391 P1 C451 109.4(4) . . . yes Pd1 P2 C11 119.3(3) . . . yes Pd1 P2 C71 115.2(2) . . . yes Pd1 P2 C131 108.8(3) . . . yes C11 P2 C71 106.4(4) . . . yes C11 P2 C131 102.2(3) . . . yes C71 P2 C131 103.1(3) . . . yes Pd1 N1 C191 130.8(5) . . . yes Pd1 N1 C201 115.9(5) . . . yes C191 N1 C201 113.3(7) . . . yes Pd1 N2 C311 117.0(4) . . . yes Pd1 N2 C321 128.4(5) . . . yes C311 N2 C321 114.6(6) . . . yes P2 C11 C21 122.6(6) . . . yes P2 C11 C61 119.3(6) . . . yes C21 C11 C61 118.1(7) . . . no C11 C21 C31 120.5(7) . . . no C21 C31 C41 119.2(8) . . . no C31 C41 C51 121.0(9) . . . no C41 C51 C61 119.3(9) . . . no C11 C61 C51 121.8(8) . . . no P2 C71 C81 120.0(6) . . . yes P2 C71 C121 119.8(5) . . . yes C81 C71 C121 120.1(6) . . . no C71 C81 C91 119.1(7) . . . no C81 C91 C101 121.7(8) . . . no C91 C101 C111 119.2(7) . . . no C101 C111 C121 120.2(8) . . . no C71 C121 C111 119.5(7) . . . no P2 C131 C141 119.6(6) . . . yes P2 C131 C181 122.5(6) . . . yes C141 C131 C181 117.8(7) . . . no C131 C141 C151 121.8(7) . . . no C141 C151 C161 119.6(7) . . . no C151 C161 C171 120.0(7) . . . no C161 C171 C181 120.8(7) . . . no C131 C181 C171 120.0(7) . . . no C131 C181 C191 125.3(7) . . . no C171 C181 C191 114.6(7) . . . no N1 C191 C181 127.7(7) . . . yes N1 C201 C211 118.5(7) . . . yes N1 C201 C251 119.5(7) . . . yes C211 C201 C251 121.7(7) . . . no C201 C211 C221 118.2(8) . . . no C211 C221 C231 121.1(7) . . . no C221 C231 C241 119.7(8) . . . no C231 C241 C251 121.5(8) . . . no C201 C251 C241 117.8(7) . . . no C201 C251 C261 122.6(7) . . . no C241 C251 C261 119.5(7) . . . no C251 C261 C271 120.5(7) . . . no C251 C261 C311 122.5(7) . . . no C271 C261 C311 116.8(7) . . . no C261 C271 C281 122.7(8) . . . no C271 C281 C291 119.3(8) . . . no C281 C291 C301 119.6(7) . . . no C291 C301 C311 120.2(8) . . . no N2 C311 C261 121.0(7) . . . yes N2 C311 C301 117.5(7) . . . yes C261 C311 C301 121.3(7) . . . no N2 C321 C331 127.5(7) . . . yes C321 C331 C341 115.5(7) . . . no C321 C331 C381 123.9(7) . . . no C341 C331 C381 120.6(7) . . . no C331 C341 C351 120.7(7) . . . no C341 C351 C361 119.2(7) . . . no C351 C361 C371 119.7(8) . . . no C361 C371 C381 122.1(8) . . . no P1 C381 C331 121.7(6) . . . yes P1 C381 C371 120.6(6) . . . yes C331 C381 C371 117.6(7) . . . no P1 C391 C401 116.7(6) . . . yes P1 C391 C441 123.1(6) . . . yes C401 C391 C441 120.1(7) . . . no C391 C401 C411 119.7(8) . . . no C401 C411 C421 120.1(9) . . . no C411 C421 C431 120.3(9) . . . no C421 C431 C441 120.7(8) . . . no C391 C441 C431 119.0(7) . . . no P1 C451 C461 121.3(6) . . . yes P1 C451 C501 120.2(6) . . . yes C461 C451 C501 118.5(7) . . . no C451 C461 C471 120.7(8) . . . no C461 C471 C481 119.3(9) . . . no C471 C481 C491 121.1(8) . . . no C481 C491 C501 119.3(9) . . . no C451 C501 C491 121.1(9) . . . no C11 C21 H21 119.7(17) . . . no C31 C21 H21 119.8(17) . . . no C21 C31 H31 121(2) . . . no C41 C31 H31 120(2) . . . no C31 C41 H41 119(4) . . . no C51 C41 H41 120(4) . . . no C41 C51 H51 120(3) . . . no C61 C51 H51 120(3) . . . no C11 C61 H61 119(2) . . . no C51 C61 H61 119(2) . . . no C71 C81 H81 120.6(19) . . . no C91 C81 H81 120.3(19) . . . no C81 C91 H91 119(4) . . . no C101 C91 H91 119(4) . . . no C91 C101 H101 120.45 . . . no C111 C101 H101 120.32 . . . no C101 C111 H111 120(2) . . . no C121 C111 H111 120(2) . . . no C71 C121 H121 121(4) . . . no C111 C121 H121 120(4) . . . no C131 C141 H141 119(2) . . . no C151 C141 H141 119(2) . . . no C141 C151 H151 120(2) . . . no C161 C151 H151 120(2) . . . no C151 C161 H161 119(3) . . . no C171 C161 H161 121(3) . . . no C161 C171 H171 120(2) . . . no C181 C171 H171 120(2) . . . no N1 C191 H191 116.1(14) . . . no C181 C191 H191 116.2(14) . . . no C201 C211 H211 121(3) . . . no C221 C211 H211 121(3) . . . no C211 C221 H221 120(3) . . . no C231 C221 H221 119(3) . . . no C221 C231 H231 120(3) . . . no C241 C231 H231 121(3) . . . no C231 C241 H241 119(3) . . . no C251 C241 H241 119(3) . . . no C261 C271 H271 119(4) . . . no C281 C271 H271 119(4) . . . no C271 C281 H281 120(3) . . . no C291 C281 H281 120(3) . . . no C281 C291 H291 120(2) . . . no C301 C291 H291 120(2) . . . no C291 C301 H301 120(3) . . . no C311 C301 H301 120(3) . . . no N2 C321 H321 116(3) . . . no C331 C321 H321 116(3) . . . no C331 C341 H341 120(3) . . . no C351 C341 H341 120(3) . . . no C341 C351 H351 121(3) . . . no C361 C351 H351 120(3) . . . no C351 C361 H361 120.3(19) . . . no C371 C361 H361 119.9(19) . . . no C361 C371 H371 119(3) . . . no C381 C371 H371 119(3) . . . no C391 C401 H401 120(3) . . . no C411 C401 H401 120(3) . . . no C401 C411 H411 120.0(19) . . . no C421 C411 H411 120(2) . . . no C411 C421 H421 120(3) . . . no C431 C421 H421 119(3) . . . no C421 C431 H431 119(3) . . . no C441 C431 H431 120(3) . . . no C391 C441 H441 120.5(17) . . . no C431 C441 H441 120.5(17) . . . no C451 C461 H461 119(3) . . . no C471 C461 H461 120(3) . . . no C461 C471 H471 120(3) . . . no C481 C471 H471 121(3) . . . no C471 C481 H481 119(3) . . . no C491 C481 H481 120(3) . . . no C481 C491 H491 121(4) . . . no C501 C491 H491 120(4) . . . no C451 C501 H501 120(3) . . . no C491 C501 H501 119(3) . . . no P3 Pd2 P4 97.19(8) . . . yes P3 Pd2 N3 174.79(16) . . . yes P3 Pd2 N4 84.04(18) . . . yes P4 Pd2 N3 87.93(17) . . . yes P4 Pd2 N4 164.41(16) . . . yes N3 Pd2 N4 90.8(2) . . . yes Pd2 P3 C382 108.0(3) . . . yes Pd2 P3 C392 120.1(3) . . . yes Pd2 P3 C452 113.2(3) . . . yes C382 P3 C392 102.3(4) . . . yes C382 P3 C452 102.9(3) . . . yes C392 P3 C452 108.5(4) . . . yes Pd2 P4 C12 118.3(3) . . . yes Pd2 P4 C72 116.3(3) . . . yes Pd2 P4 C132 108.7(3) . . . yes C12 P4 C72 105.6(4) . . . yes C12 P4 C132 103.2(4) . . . yes C72 P4 C132 102.9(4) . . . yes Pd2 N3 C192 131.0(5) . . . yes Pd2 N3 C202 115.5(5) . . . yes C192 N3 C202 113.4(7) . . . yes Pd2 N4 C312 115.9(4) . . . yes Pd2 N4 C322 129.2(5) . . . yes C312 N4 C322 114.8(6) . . . yes P4 C12 C22 121.6(6) . . . yes P4 C12 C62 119.3(6) . . . yes C22 C12 C62 119.1(7) . . . no C12 C22 C32 119.9(7) . . . no C22 C32 C42 120.2(8) . . . no C32 C42 C52 120.1(9) . . . no C42 C52 C62 120.7(8) . . . no C12 C62 C52 120.0(8) . . . no P4 C72 C82 122.0(6) . . . yes P4 C72 C122 118.5(6) . . . yes C82 C72 C122 119.5(7) . . . no C72 C82 C92 120.1(7) . . . no C82 C92 C102 120.8(8) . . . no C92 C102 C112 119.2(7) . . . no C102 C112 C122 120.3(8) . . . no C72 C122 C112 120.0(7) . . . no P4 C132 C142 118.4(6) . . . yes P4 C132 C182 122.1(6) . . . yes C142 C132 C182 119.2(8) . . . no C132 C142 C152 120.1(8) . . . no C142 C152 C162 120.4(8) . . . no C152 C162 C172 119.4(9) . . . no C162 C172 C182 121.1(8) . . . no C132 C182 C172 119.8(7) . . . no C132 C182 C192 124.7(7) . . . no C172 C182 C192 115.5(7) . . . no N3 C192 C182 129.1(8) . . . yes N3 C202 C212 119.2(6) . . . yes N3 C202 C252 119.5(6) . . . yes C212 C202 C252 121.2(7) . . . no C202 C212 C222 121.3(7) . . . no C212 C222 C232 118.2(7) . . . no C222 C232 C242 120.6(8) . . . no C232 C242 C252 121.3(7) . . . no C202 C252 C242 117.3(7) . . . no C202 C252 C262 122.4(7) . . . no C242 C252 C262 120.0(7) . . . no C252 C262 C272 119.6(7) . . . no C252 C262 C312 123.7(7) . . . no C272 C262 C312 116.6(7) . . . no C262 C272 C282 122.2(9) . . . no C272 C282 C292 119.1(9) . . . no C282 C292 C302 120.8(7) . . . no C292 C302 C312 118.9(8) . . . no N4 C312 C262 119.8(7) . . . yes N4 C312 C302 117.7(7) . . . yes C262 C312 C302 122.3(8) . . . no N4 C322 C332 128.2(7) . . . yes C322 C332 C342 116.5(7) . . . no C322 C332 C382 123.5(7) . . . no C342 C332 C382 120.0(7) . . . no C332 C342 C352 120.1(7) . . . no C342 C352 C362 120.3(7) . . . no C352 C362 C372 120.4(8) . . . no C362 C372 C382 120.8(8) . . . no P3 C382 C332 119.8(6) . . . yes P3 C382 C372 121.5(6) . . . yes C332 C382 C372 118.4(7) . . . no P3 C392 C402 118.1(6) . . . yes P3 C392 C442 122.5(6) . . . yes C402 C392 C442 119.4(7) . . . no C392 C402 C412 121.2(8) . . . no C402 C412 C422 119.4(9) . . . no C412 C422 C432 120.6(9) . . . no C422 C432 C442 121.4(9) . . . no C392 C442 C432 118.0(7) . . . no P3 C452 C462 120.9(6) . . . yes P3 C452 C502 119.4(6) . . . yes C462 C452 C502 119.8(7) . . . no C452 C462 C472 119.5(8) . . . no C462 C472 C482 119.7(9) . . . no C472 C482 C492 121.3(9) . . . no C482 C492 C502 119.8(9) . . . no C452 C502 C492 120.0(8) . . . no C12 C22 H22 120(2) . . . no C32 C22 H22 120(2) . . . no C22 C32 H32 120(3) . . . no C42 C32 H32 120(3) . . . no C32 C42 H42 120(3) . . . no C52 C42 H42 120(3) . . . no C42 C52 H52 120(2) . . . no C62 C52 H52 120(2) . . . no C12 C62 H62 120(3) . . . no C52 C62 H62 120(3) . . . no C72 C82 H82 120.0(18) . . . no C92 C82 H82 119.9(18) . . . no C82 C92 H92 120(4) . . . no C102 C92 H92 119(4) . . . no C92 C102 H102 120(4) . . . no C112 C102 H102 120(4) . . . no C102 C112 H112 120.0(18) . . . no C122 C112 H112 119.8(18) . . . no C72 C122 H122 120(3) . . . no C112 C122 H122 120(3) . . . no C132 C142 H142 120(3) . . . no C152 C142 H142 120(3) . . . no C142 C152 H152 120(2) . . . no C162 C152 H152 120(2) . . . no C152 C162 H162 120(4) . . . no C172 C162 H162 120(4) . . . no C162 C172 H172 119.5(19) . . . no C182 C172 H172 119.4(19) . . . no N3 C192 H192 115.5(14) . . . no C182 C192 H192 115.5(13) . . . no C202 C212 H212 120(3) . . . no C222 C212 H212 119(3) . . . no C212 C222 H222 121(2) . . . no C232 C222 H222 121(2) . . . no C222 C232 H232 120(3) . . . no C242 C232 H232 120(3) . . . no C232 C242 H242 120(3) . . . no C252 C242 H242 119(3) . . . no C262 C272 H272 119(4) . . . no C282 C272 H272 119(4) . . . no C272 C282 H282 120(3) . . . no C292 C282 H282 120(3) . . . no C282 C292 H292 119(3) . . . no C302 C292 H292 120(3) . . . no C292 C302 H302 120(3) . . . no C312 C302 H302 121(3) . . . no N4 C322 H322 116(3) . . . no C332 C322 H322 116(3) . . . no C332 C342 H342 120(3) . . . no C352 C342 H342 120(3) . . . no C342 C352 H352 120(4) . . . no C362 C352 H352 119(4) . . . no C352 C362 H362 119.9(18) . . . no C372 C362 H362 119.8(19) . . . no C362 C372 H372 120(3) . . . no C382 C372 H372 119(3) . . . no C392 C402 H402 120(4) . . . no C412 C402 H402 119(4) . . . no C402 C412 H412 120(2) . . . no C422 C412 H412 120(2) . . . no C412 C422 H422 120(2) . . . no C432 C422 H422 120(2) . . . no C422 C432 H432 119(4) . . . no C442 C432 H432 120(4) . . . no C392 C442 H442 121.0(19) . . . no C432 C442 H442 121.0(19) . . . no C452 C462 H462 120(3) . . . no C472 C462 H462 120(3) . . . no C462 C472 H472 120(3) . . . no C482 C472 H472 120(3) . . . no C472 C482 H482 119(3) . . . no C492 C482 H482 119(2) . . . no C482 C492 H492 120(4) . . . no C502 C492 H492 120(4) . . . no C452 C502 H502 120(3) . . . no C492 C502 H502 120(3) . . . no Cl19 C7 Cl20 118.6(9) . . . yes Cl19 C7 Cl21 100.5(14) . . . yes Cl19 C7 Cl22 105.8(13) . . . yes Cl19 C7 H310 107.68 . . . no Cl19 C7 H320 107.76 . . . no Cl19 C7 H330 111.67 . . . no Cl19 C7 H340 111.71 . . . no Cl19 C7 H350 110.58 . . . no Cl19 C7 H360 110.63 . . . no Cl20 C7 H310 107.64 . . . no Cl20 C7 H320 107.57 . . . no H310 C7 H320 107.12 . . . no Cl21 C7 H330 111.58 . . . no Cl21 C7 H340 111.64 . . . no Cl22 C7 H350 110.49 . . . no Cl22 C7 H360 110.60 . . . no H330 C7 H340 109.57 . . . no H350 C7 H360 108.71 . . . no Cl15 C6 Cl16 111.6(7) . . . yes Cl17 C6 Cl18 120.8(12) . . . yes Cl15 C6 H610 109.27 . . . no Cl15 C6 H620 109.24 . . . no Cl16 C6 H610 109.34 . . . no Cl16 C6 H620 109.32 . . . no H610 C6 H620 108.05 . . . no Cl17 C6 H630 107.22 . . . no Cl17 C6 H640 107.15 . . . no Cl18 C6 H630 107.05 . . . no Cl18 C6 H640 107.13 . . . no H630 C6 H640 106.77 . . . no Cl5 C1 Cl6 113.3(7) . . . yes Cl5 C1 H11 108.94 . . . no Cl5 C1 H201 108.99 . . . no Cl6 C1 H11 108.85 . . . no Cl6 C1 H201 108.92 . . . no H11 C1 H201 107.72 . . . no Cl7 C2 Cl8 111.4(6) . . . yes Cl7 C2 H12 109.32 . . . no Cl7 C2 H202 109.39 . . . no Cl8 C2 H12 109.33 . . . no Cl8 C2 H202 109.40 . . . no H12 C2 H202 107.97 . . . no Cl9 C3 Cl10 110.6(7) . . . yes Cl9 C3 H13 109.60 . . . no Cl9 C3 H203 109.43 . . . no Cl10 C3 H13 109.56 . . . no Cl10 C3 H203 109.46 . . . no H13 C3 H203 108.10 . . . no Cl11 C4 Cl12 111.5(7) . . . yes Cl11 C4 H14 109.35 . . . no Cl11 C4 H204 109.30 . . . no Cl12 C4 H14 109.32 . . . no Cl12 C4 H204 109.43 . . . no H14 C4 H204 107.87 . . . no Cl13 C5 Cl14 113.4(11) . . . yes Cl13 C5 H15 108.94 . . . no Cl13 C5 H205 108.87 . . . no Cl14 C5 H15 108.86 . . . no Cl14 C5 H205 108.95 . . . no H15 C5 H205 107.71 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd1 P1 C381 -39.4(2) . . . . no Cl1 Pd1 P1 C391 76.6(3) . . . . no Cl1 Pd1 P1 C451 -154.7(3) . . . . no P2 Pd1 P1 C381 -151.6(2) . . . . no P2 Pd1 P1 C391 -35.6(3) . . . . no P2 Pd1 P1 C451 93.1(3) . . . . no N2 Pd1 P1 C381 46.4(3) . . . . no N2 Pd1 P1 C391 162.4(3) . . . . no N2 Pd1 P1 C451 -68.9(3) . . . . no Cl1 Pd1 P2 C11 -114.0(3) . . . . no Cl1 Pd1 P2 C71 14.4(3) . . . . no Cl1 Pd1 P2 C131 129.6(2) . . . . no P1 Pd1 P2 C11 -24.7(3) . . . . no P1 Pd1 P2 C71 103.7(3) . . . . no P1 Pd1 P2 C131 -141.1(2) . . . . no N1 Pd1 P2 C11 154.5(3) . . . . no N1 Pd1 P2 C71 -77.1(3) . . . . no N1 Pd1 P2 C131 38.0(3) . . . . no Cl1 Pd1 N1 C191 -144.3(7) . . . . no Cl1 Pd1 N1 C201 37.7(5) . . . . no P2 Pd1 N1 C191 -32.0(7) . . . . no P2 Pd1 N1 C201 150.1(5) . . . . no N2 Pd1 N1 C191 130.1(7) . . . . no N2 Pd1 N1 C201 -47.9(5) . . . . no Cl1 Pd1 N2 C311 -134.0(5) . . . . no Cl1 Pd1 N2 C321 49.1(6) . . . . no P1 Pd1 N2 C311 138.8(5) . . . . no P1 Pd1 N2 C321 -38.1(6) . . . . no N1 Pd1 N2 C311 -41.9(5) . . . . no N1 Pd1 N2 C321 141.2(6) . . . . no C451 P1 C391 C441 2.1(8) . . . . no C391 P1 C381 C371 15.3(6) . . . . no C451 P1 C381 C371 -99.0(6) . . . . no Pd1 P1 C391 C401 -51.6(7) . . . . no Pd1 P1 C381 C331 -41.6(6) . . . . no C391 P1 C381 C331 -166.6(6) . . . . no C451 P1 C381 C331 79.1(6) . . . . no Pd1 P1 C381 C371 140.4(5) . . . . no C391 P1 C451 C501 124.7(7) . . . . no C451 P1 C391 C401 178.0(6) . . . . no Pd1 P1 C451 C461 170.8(6) . . . . no C381 P1 C391 C401 67.1(7) . . . . no C381 P1 C451 C461 53.4(7) . . . . no Pd1 P1 C391 C441 132.5(6) . . . . no C381 P1 C391 C441 -108.7(7) . . . . no C381 P1 C451 C501 -125.5(7) . . . . no C391 P1 C451 C461 -56.4(7) . . . . no Pd1 P1 C451 C501 -8.1(7) . . . . no C131 P2 C11 C21 -120.0(7) . . . . no C131 P2 C71 C81 -128.2(7) . . . . no Pd1 P2 C11 C61 -59.5(7) . . . . no C71 P2 C11 C21 -12.2(8) . . . . no Pd1 P2 C11 C21 120.1(6) . . . . no C71 P2 C131 C141 -86.3(6) . . . . no Pd1 P2 C71 C121 168.5(6) . . . . no C11 P2 C71 C121 -57.0(8) . . . . no C131 P2 C71 C121 50.1(7) . . . . no C71 P2 C11 C61 168.2(6) . . . . no C131 P2 C11 C61 60.4(7) . . . . no C11 P2 C131 C181 -160.7(6) . . . . no Pd1 P2 C131 C141 150.9(5) . . . . no Pd1 P2 C131 C181 -33.7(6) . . . . no Pd1 P2 C71 C81 -9.9(8) . . . . no C71 P2 C131 C181 89.0(6) . . . . no C11 P2 C131 C141 24.0(6) . . . . no C11 P2 C71 C81 124.7(7) . . . . no C191 N1 C201 C251 -96.8(9) . . . . no Pd1 N1 C201 C211 -104.4(7) . . . . no Pd1 N1 C201 C251 81.6(8) . . . . no C191 N1 C201 C211 77.3(9) . . . . no Pd1 N1 C191 C181 5.1(12) . . . . no C201 N1 C191 C181 -176.9(7) . . . . no Pd1 N2 C311 C261 73.1(8) . . . . no C321 N2 C311 C301 67.2(9) . . . . no Pd1 N2 C321 C331 5.4(10) . . . . no Pd1 N2 C311 C301 -110.2(7) . . . . no C311 N2 C321 C331 -171.6(7) . . . . no C321 N2 C311 C261 -109.6(8) . . . . no C21 C11 C61 C51 -0.6(12) . . . . no P2 C11 C21 C31 179.6(6) . . . . no P2 C11 C61 C51 179.1(7) . . . . no C61 C11 C21 C31 -0.8(11) . . . . no C11 C21 C31 C41 0.9(12) . . . . no C21 C31 C41 C51 0.3(13) . . . . no C31 C41 C51 C61 -1.7(14) . . . . no C41 C51 C61 C11 1.8(13) . . . . no P2 C71 C81 C91 179.7(8) . . . . no C121 C71 C81 C91 1.4(13) . . . . no P2 C71 C121 C111 -179.6(7) . . . . no C81 C71 C121 C111 -1.3(13) . . . . no C71 C81 C91 C101 -0.6(15) . . . . no C81 C91 C101 C111 -0.5(15) . . . . no C91 C101 C111 C121 0.6(14) . . . . no C101 C111 C121 C71 0.3(15) . . . . no P2 C131 C181 C191 1.4(10) . . . . no P2 C131 C181 C171 -175.0(6) . . . . no C141 C131 C181 C171 0.4(11) . . . . no P2 C131 C141 C151 175.0(6) . . . . no C181 C131 C141 C151 -0.6(11) . . . . no C141 C131 C181 C191 176.8(7) . . . . no C131 C141 C151 C161 0.9(11) . . . . no C141 C151 C161 C171 -1.0(12) . . . . no C151 C161 C171 C181 0.8(12) . . . . no C161 C171 C181 C191 -177.3(7) . . . . no C161 C171 C181 C131 -0.5(11) . . . . no C131 C181 C191 N1 18.8(13) . . . . no C171 C181 C191 N1 -164.7(8) . . . . no N1 C201 C211 C221 -173.3(8) . . . . no N1 C201 C251 C261 -3.1(12) . . . . no C251 C201 C211 C221 0.6(13) . . . . no N1 C201 C251 C241 173.0(7) . . . . no C211 C201 C251 C261 -177.0(8) . . . . no C211 C201 C251 C241 -0.8(12) . . . . no C201 C211 C221 C231 0.1(17) . . . . no C211 C221 C231 C241 -0.6(14) . . . . no C221 C231 C241 C251 0.3(14) . . . . no C231 C241 C251 C201 0.3(12) . . . . no C231 C241 C251 C261 176.6(8) . . . . no C201 C251 C261 C271 124.7(9) . . . . no C241 C251 C261 C311 123.6(9) . . . . no C201 C251 C261 C311 -60.3(11) . . . . no C241 C251 C261 C271 -51.4(11) . . . . no C251 C261 C311 N2 1.7(11) . . . . no C271 C261 C311 N2 176.9(7) . . . . no C271 C261 C311 C301 0.2(11) . . . . no C311 C261 C271 C281 -1.2(11) . . . . no C251 C261 C271 C281 174.0(7) . . . . no C251 C261 C311 C301 -174.9(7) . . . . no C261 C271 C281 C291 1.7(12) . . . . no C271 C281 C291 C301 -1.2(11) . . . . no C281 C291 C301 C311 0.2(10) . . . . no C291 C301 C311 C261 0.2(12) . . . . no C291 C301 C311 N2 -176.5(7) . . . . no N2 C321 C331 C381 23.1(11) . . . . no N2 C321 C331 C341 -157.9(7) . . . . no C341 C331 C381 C371 0.0(10) . . . . no C381 C331 C341 C351 -0.7(11) . . . . no C321 C331 C341 C351 -179.8(6) . . . . no C321 C331 C381 C371 179.0(7) . . . . no C341 C331 C381 P1 -178.1(5) . . . . no C321 C331 C381 P1 0.8(10) . . . . no C331 C341 C351 C361 0.4(11) . . . . no C341 C351 C361 C371 0.7(11) . . . . no C351 C361 C371 C381 -1.5(12) . . . . no C361 C371 C381 C331 1.1(11) . . . . no C361 C371 C381 P1 179.3(5) . . . . no P1 C391 C401 C411 -175.0(6) . . . . no C401 C391 C441 C431 -0.8(11) . . . . no C441 C391 C401 C411 1.0(12) . . . . no P1 C391 C441 C431 174.9(6) . . . . no C391 C401 C411 C421 -0.9(12) . . . . no C401 C411 C421 C431 0.7(13) . . . . no C411 C421 C431 C441 -0.4(13) . . . . no C421 C431 C441 C391 0.5(12) . . . . no P1 C451 C461 C471 178.1(7) . . . . no C501 C451 C461 C471 -3.0(12) . . . . no P1 C451 C501 C491 -177.9(7) . . . . no C461 C451 C501 C491 3.2(12) . . . . no C451 C461 C471 C481 1.3(13) . . . . no C461 C471 C481 C491 0.4(14) . . . . no C471 C481 C491 C501 -0.2(15) . . . . no C481 C491 C501 C451 -1.6(13) . . . . no P4 Pd2 P3 C382 -147.0(2) . . . . no P4 Pd2 P3 C392 -30.5(3) . . . . no P4 Pd2 P3 C452 99.8(3) . . . . no N4 Pd2 P3 C382 48.7(3) . . . . no N4 Pd2 P3 C392 165.2(3) . . . . no N4 Pd2 P3 C452 -64.6(3) . . . . no P3 Pd2 P4 C12 -24.1(3) . . . . no P3 Pd2 P4 C72 103.2(3) . . . . no P3 Pd2 P4 C132 -141.3(3) . . . . no N3 Pd2 P4 C12 154.9(3) . . . . no N3 Pd2 P4 C72 -77.7(3) . . . . no N3 Pd2 P4 C132 37.7(3) . . . . no P4 Pd2 N3 C192 -28.1(7) . . . . no P4 Pd2 N3 C202 148.5(4) . . . . no N4 Pd2 N3 C192 136.4(7) . . . . no N4 Pd2 N3 C202 -47.0(5) . . . . no P3 Pd2 N4 C312 137.6(5) . . . . no P3 Pd2 N4 C322 -37.6(7) . . . . no N3 Pd2 N4 C312 -42.9(5) . . . . no N3 Pd2 N4 C322 142.0(7) . . . . no C452 P3 C392 C442 -0.9(8) . . . . no C392 P3 C382 C372 12.6(7) . . . . no C452 P3 C382 C372 -99.9(6) . . . . no Pd2 P3 C392 C402 -51.0(7) . . . . no Pd2 P3 C382 C332 -46.6(6) . . . . no C392 P3 C382 C332 -174.1(6) . . . . no C452 P3 C382 C332 73.4(6) . . . . no Pd2 P3 C382 C372 140.1(5) . . . . no C392 P3 C452 C502 118.8(7) . . . . no C452 P3 C392 C402 176.7(6) . . . . no Pd2 P3 C452 C462 161.7(6) . . . . no C382 P3 C392 C402 68.4(7) . . . . no C382 P3 C452 C462 45.4(7) . . . . no Pd2 P3 C392 C442 131.4(6) . . . . no C382 P3 C392 C442 -109.2(7) . . . . no C382 P3 C452 C502 -133.3(7) . . . . no C392 P3 C452 C462 -62.4(7) . . . . no Pd2 P3 C452 C502 -17.0(7) . . . . no C132 P4 C12 C22 -116.5(7) . . . . no C132 P4 C72 C82 -136.8(7) . . . . no Pd2 P4 C12 C62 -58.2(7) . . . . no C72 P4 C12 C22 -8.8(8) . . . . no Pd2 P4 C12 C22 123.5(6) . . . . no C72 P4 C132 C142 -86.9(7) . . . . no Pd2 P4 C72 C122 162.7(6) . . . . no C12 P4 C72 C122 -63.9(7) . . . . no C132 P4 C72 C122 44.0(7) . . . . no C72 P4 C12 C62 169.5(6) . . . . no C132 P4 C12 C62 61.8(7) . . . . no C12 P4 C132 C182 -163.2(7) . . . . no Pd2 P4 C132 C142 149.2(6) . . . . no Pd2 P4 C132 C182 -36.8(7) . . . . no Pd2 P4 C72 C82 -18.2(8) . . . . no C72 P4 C132 C182 87.1(7) . . . . no C12 P4 C132 C142 22.8(7) . . . . no C12 P4 C72 C82 115.2(8) . . . . no C192 N3 C202 C252 -103.1(8) . . . . no Pd2 N3 C202 C212 -104.5(7) . . . . no Pd2 N3 C202 C252 79.7(8) . . . . no C192 N3 C202 C212 72.7(10) . . . . no Pd2 N3 C192 C182 0.4(13) . . . . no C202 N3 C192 C182 -176.2(7) . . . . no Pd2 N4 C312 C262 74.4(8) . . . . no C322 N4 C312 C302 65.5(9) . . . . no Pd2 N4 C322 C332 3.9(12) . . . . no Pd2 N4 C312 C302 -110.3(7) . . . . no C312 N4 C322 C332 -171.2(7) . . . . no C322 N4 C312 C262 -109.7(8) . . . . no C22 C12 C62 C52 -1.6(12) . . . . no P4 C12 C22 C32 -179.5(6) . . . . no P4 C12 C62 C52 -180.0(7) . . . . no C62 C12 C22 C32 2.3(12) . . . . no C12 C22 C32 C42 -1.5(12) . . . . no C22 C32 C42 C52 0.0(13) . . . . no C32 C42 C52 C62 0.6(14) . . . . no C42 C52 C62 C12 0.2(15) . . . . no P4 C72 C82 C92 -177.4(8) . . . . no C122 C72 C82 C92 1.8(14) . . . . no P4 C72 C122 C112 179.1(7) . . . . no C82 C72 C122 C112 -0.1(13) . . . . no C72 C82 C92 C102 -2.2(16) . . . . no C82 C92 C102 C112 0.9(15) . . . . no C92 C102 C112 C122 0.8(15) . . . . no C102 C112 C122 C72 -1.2(14) . . . . no P4 C132 C182 C192 5.4(11) . . . . no P4 C132 C182 C172 -173.5(6) . . . . no C142 C132 C182 C172 0.5(11) . . . . no P4 C132 C142 C152 174.9(6) . . . . no C182 C132 C142 C152 0.7(12) . . . . no C142 C132 C182 C192 179.4(7) . . . . no C132 C142 C152 C162 -0.7(12) . . . . no C142 C152 C162 C172 -0.5(12) . . . . no C152 C162 C172 C182 1.7(12) . . . . no C162 C172 C182 C192 179.3(7) . . . . no C162 C172 C182 C132 -1.7(12) . . . . no C132 C182 C192 N3 18.8(13) . . . . no C172 C182 C192 N3 -162.2(8) . . . . no N3 C202 C212 C222 -173.8(8) . . . . no N3 C202 C252 C262 -2.1(12) . . . . no C252 C202 C212 C222 1.9(13) . . . . no N3 C202 C252 C242 172.6(7) . . . . no C212 C202 C252 C262 -177.8(8) . . . . no C212 C202 C252 C242 -3.1(12) . . . . no C202 C212 C222 C232 -0.4(14) . . . . no C212 C222 C232 C242 0.2(14) . . . . no C222 C232 C242 C252 -1.4(13) . . . . no C232 C242 C252 C202 2.8(12) . . . . no C232 C242 C252 C262 177.7(8) . . . . no C202 C252 C262 C272 123.1(9) . . . . no C242 C252 C262 C312 123.9(9) . . . . no C202 C252 C262 C312 -61.5(11) . . . . no C242 C252 C262 C272 -51.5(11) . . . . no C252 C262 C312 N4 0.7(11) . . . . no C272 C262 C312 N4 176.3(7) . . . . no C272 C262 C312 C302 1.3(12) . . . . no C312 C262 C272 C282 0.0(13) . . . . no C252 C262 C272 C282 175.8(8) . . . . no C252 C262 C312 C302 -174.3(7) . . . . no C262 C272 C282 C292 -1.5(14) . . . . no C272 C282 C292 C302 1.6(14) . . . . no C282 C292 C302 C312 -0.3(13) . . . . no C292 C302 C312 C262 -1.2(12) . . . . no C292 C302 C312 N4 -176.3(7) . . . . no N4 C322 C332 C382 21.6(13) . . . . no N4 C322 C332 C342 -159.5(8) . . . . no C342 C332 C382 C372 0.5(11) . . . . no C382 C332 C342 C352 -1.2(11) . . . . no C322 C332 C342 C352 179.9(9) . . . . no C322 C332 C382 C372 179.3(7) . . . . no C342 C332 C382 P3 -173.0(6) . . . . no C322 C332 C382 P3 5.8(10) . . . . no C332 C342 C352 C362 0.5(12) . . . . no C342 C352 C362 C372 0.9(12) . . . . no C352 C362 C372 C382 -1.6(12) . . . . no C362 C372 C382 C332 0.9(11) . . . . no C362 C372 C382 P3 174.3(6) . . . . no P3 C392 C402 C412 -177.2(6) . . . . no C402 C392 C442 C432 -1.5(11) . . . . no C442 C392 C402 C412 0.5(12) . . . . no P3 C392 C442 C432 176.0(6) . . . . no C392 C402 C412 C422 1.0(12) . . . . no C402 C412 C422 C432 -1.5(13) . . . . no C412 C422 C432 C442 0.5(13) . . . . no C422 C432 C442 C392 1.1(12) . . . . no P3 C452 C462 C472 -179.3(7) . . . . no C502 C452 C462 C472 -0.6(12) . . . . no P3 C452 C502 C492 179.3(7) . . . . no C462 C452 C502 C492 0.5(11) . . . . no C452 C462 C472 C482 0.5(13) . . . . no C462 C472 C482 C492 -0.3(15) . . . . no C472 C482 C492 C502 0.3(14) . . . . no C482 C492 C502 C452 -0.4(14) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd2 Cl2 2.9361(19) . . no Pd2 Cl8 4.114(3) . . no Cl1 C211 3.457(9) . . no Cl1 C331 3.322(8) . . no Cl1 C81 3.371(8) . . no Cl1 C492 3.565(10) . 1_556 no Cl1 C342 3.417(8) . 2_556 no Cl1 C401 3.590(8) . . no Cl1 C352 3.411(8) . 2_556 no Cl2 C212 3.506(10) . . no Cl2 C332 3.435(8) . . no Cl2 Pd2 2.9361(19) . . no Cl2 C341 3.521(8) . 2_556 no Cl2 C351 3.466(8) . 2_556 no Cl2 C382 3.272(7) . . no Cl2 C82 3.369(8) . . no Cl2 C202 3.533(8) . . no Cl2 P3 3.604(3) . . no Cl3 C112 3.646(9) . . no Cl3 C122 3.647(8) . . no Cl3 C421 3.538(10) . 2_566 no Cl3 C6 3.450(12) . . no Cl3 C191 3.405(9) . 2_666 no Cl3 C7 3.591(12) . . no Cl4 C422 3.599(10) . . no Cl4 C111 3.564(10) . 2_666 no Cl4 C5 3.507(18) . . no Cl4 C192 3.368(9) . . no Cl4 C3 3.472(12) . . no Cl4 C2 3.613(11) . . no Cl5 C301 3.444(8) . . no Cl5 C181 3.567(8) . . no Cl5 C281 3.573(8) . . no Cl5 C291 3.378(8) . . no Cl6 C212 3.468(8) . . no Cl6 C161 3.339(8) . . no Cl7 C101 3.610(10) . 2_666 no Cl7 C211 3.649(9) . . no Cl7 C172 3.580(8) . . no Cl7 C111 3.620(9) . 2_666 no Cl7 C152 3.620(9) . . no Cl7 C162 3.569(9) . . no Cl7 Cl22 3.53(3) . . no Cl8 C132 3.639(8) . . no Cl8 Pd2 4.114(3) . . no Cl8 C302 3.551(8) . . no Cl8 C182 3.436(8) . . no Cl9 Cl11 3.661(4) . . no Cl10 Cl11 3.679(5) . . no Cl10 C481 3.525(11) . . no Cl10 C471 3.554(10) . . no Cl10 C412 3.548(10) . . no Cl11 C112 3.630(9) . 2_666 no Cl11 Cl10 3.679(5) . . no Cl11 C3 3.513(12) . . no Cl11 Cl9 3.661(4) . . no Cl12 Cl18 3.032(13) . . no Cl13 Cl20 3.629(18) . . no Cl14 Cl17 3.54(3) . . no Cl16 C7 3.614(15) . . no Cl16 C482 3.614(15) . . no Cl16 C472 3.577(13) . . no Cl17 Cl14 3.54(3) . 2_656 no Cl18 Cl12 3.032(13) . . no Cl20 Cl13 3.629(18) . . no Cl21 C472 3.52(4) . . no Cl22 Cl7 3.53(3) . 2_665 no P3 Cl2 3.604(3) . . no C2 C172 3.394(13) . . no C2 C182 3.585(13) . . no C2 Cl4 3.613(11) . . no C3 Cl4 3.472(12) . . no C3 Cl11 3.513(12) . . no C5 Cl4 3.507(18) . . no C6 Cl3 3.450(12) . 2_666 no C7 Cl3 3.591(12) . . no C7 Cl16 3.614(15) . . no C11 C441 3.469(11) . . no C11 C391 3.244(11) . . no C12 C442 3.491(11) . . no C12 C392 3.203(11) . . no C21 C431 3.501(11) . . no C21 C121 3.272(11) . . no C21 C391 3.354(11) . . no C21 C441 3.272(11) . . no C22 C442 3.430(11) . . no C22 C392 3.386(11) . . no C22 C432 3.587(12) . . no C22 C122 3.293(11) . . no C22 C402 3.481(11) . . no C31 C441 3.408(11) . . no C31 C431 3.367(11) . . no C32 C432 3.305(12) . . no C32 C442 3.457(11) . . no C42 C442 3.570(12) . . no C61 C501 3.287(11) . . no C61 C141 3.242(12) . . no C61 C451 3.564(11) . . no C62 C142 3.272(13) . . no C62 C502 3.394(11) . . no C81 Cl1 3.371(8) . . no C81 C401 3.505(12) . . no C82 C402 3.531(12) . . no C82 Cl2 3.369(8) . . no C101 Cl7 3.610(10) . 2_666 no C111 Cl4 3.564(10) . 2_666 no C111 Cl7 3.620(9) . 2_666 no C112 Cl3 3.646(9) . . no C112 Cl11 3.630(9) . 2_666 no C121 C141 3.467(11) . . no C121 C172 3.575(12) . 2_666 no C121 C21 3.272(11) . . no C122 Cl3 3.647(8) . . no C122 C142 3.393(11) . . no C122 C22 3.293(11) . . no C122 C171 3.431(12) . 2_666 no C132 Cl8 3.639(8) . . no C141 C61 3.242(12) . . no C141 C121 3.467(11) . . no C142 C62 3.272(13) . . no C142 C122 3.393(11) . . no C152 Cl7 3.620(9) . 2_665 no C161 Cl6 3.339(8) . . no C161 C182 3.466(11) . 2_666 no C161 C192 3.572(11) . 2_666 no C162 C181 3.528(11) . 2_666 no C162 Cl7 3.569(9) . . no C171 C122 3.431(12) . 2_666 no C171 C172 3.490(11) . 2_666 no C172 Cl7 3.580(8) . . no C172 C171 3.490(11) . 2_666 no C172 C2 3.394(13) . . no C172 C121 3.575(12) . 2_666 no C181 C162 3.528(11) . 2_666 no C181 Cl5 3.567(8) . . no C182 Cl8 3.436(8) . . no C182 C2 3.585(13) . . no C182 C161 3.466(11) . 2_666 no C191 C261 3.521(11) . . no C191 Cl3 3.405(9) . 2_666 no C192 C262 3.586(11) . . no C192 Cl4 3.368(9) . . no C192 C161 3.572(11) . 2_666 no C202 Cl2 3.533(8) . . no C211 Cl1 3.457(9) . . no C211 Cl7 3.649(9) . 1_556 no C212 Cl6 3.468(8) . . no C212 Cl2 3.506(10) . . no C231 C362 3.575(13) . 2_556 no C232 C361 3.584(12) . 2_556 no C241 C362 3.553(11) . 2_556 no C242 C361 3.559(11) . 2_556 no C261 C191 3.521(11) . . no C262 C192 3.586(11) . . no C281 Cl5 3.573(8) . . no C291 Cl5 3.378(8) . . no C291 C461 3.416(11) . 2_556 no C291 C341 3.532(10) . 2_556 no C301 Cl5 3.444(8) . . no C302 Cl8 3.551(8) . . no C302 C502 3.553(13) . . no C322 C452 3.552(11) . . no C331 Cl1 3.322(8) . . no C332 Cl2 3.435(8) . . no C341 C291 3.532(10) . 2_556 no C341 C342 3.231(10) . 2_556 no C341 C352 3.576(11) . 2_556 no C341 Cl2 3.521(8) . 2_556 no C342 Cl1 3.417(8) . 2_556 no C342 C351 3.588(11) . 2_556 no C342 C341 3.231(10) . 2_556 no C351 C342 3.588(11) . 2_556 no C351 Cl2 3.466(8) . 2_556 no C352 C341 3.576(11) . 2_556 no C352 Cl1 3.411(8) . 2_556 no C361 C242 3.559(11) . 2_556 no C361 C232 3.584(12) . 2_556 no C362 C241 3.553(11) . 2_556 no C362 C231 3.575(13) . 2_556 no C371 C401 3.259(11) . . no C372 C402 3.252(11) . . no C382 Cl2 3.272(7) . . no C391 C21 3.354(11) . . no C391 C11 3.244(11) . . no C392 C22 3.386(11) . . no C392 C12 3.203(11) . . no C401 C81 3.505(12) . . no C401 Cl1 3.590(8) . . no C401 C371 3.259(11) . . no C402 C372 3.252(11) . . no C402 C82 3.531(12) . . no C402 C22 3.481(11) . . no C412 Cl10 3.548(10) . 1_455 no C421 Cl3 3.538(10) . 2_566 no C422 Cl4 3.599(10) . 1_455 no C431 C31 3.367(11) . . no C431 C21 3.501(11) . . no C432 C22 3.587(12) . . no C432 C32 3.305(12) . . no C441 C11 3.469(11) . . no C441 C21 3.272(11) . . no C441 C31 3.408(11) . . no C441 C461 3.275(11) . . no C442 C42 3.570(12) . . no C442 C32 3.457(11) . . no C442 C22 3.430(11) . . no C442 C12 3.491(11) . . no C442 C462 3.332(11) . . no C451 C61 3.564(11) . . no C452 C322 3.552(11) . . no C461 C291 3.416(11) . 2_556 no C461 C441 3.275(11) . . no C462 C442 3.332(11) . . no C471 Cl10 3.554(10) . 1_455 no C472 Cl21 3.52(4) . . no C472 Cl16 3.577(13) . 1_454 no C481 Cl10 3.525(11) . 1_455 no C482 Cl16 3.614(15) . 1_454 no C492 Cl1 3.565(10) . . no C501 C61 3.287(11) . . no C502 C62 3.394(11) . . no C502 C302 3.553(13) . . no Pd1 H81 3.02(3) . . no Pd1 H401 3.38(6) . . no Pd1 H61 3.68(4) . . no Pd1 H501 2.96(4) . . no Pd2 H62 3.66(5) . . no Pd2 H82 3.17(4) . . no Pd2 H502 2.99(4) . . no Pd2 H402 3.55(6) . . no Cl1 H492 2.73(6) . 1_556 no Cl1 H352 2.82(7) . 2_556 no Cl1 H81 2.39(9) . . no Cl1 H401 2.68(5) . . no Cl1 H342 2.87(5) . 2_556 no Cl2 H82 2.42(9) . . no Cl2 H201 2.8412 . . no Cl2 H341 2.90(5) . 2_556 no Cl2 H491 3.01(5) . . no Cl2 H351 2.81(7) . 2_556 no Cl2 H402 3.06(5) . . no Cl3 H340 2.6774 . . no Cl3 H310 3.1066 . . no Cl3 H122 3.04(4) . . no Cl3 H620 2.7044 . . no Cl3 H360 2.8782 . . no Cl3 H112 2.97(7) . . no Cl3 H630 2.7381 . . no Cl3 H14 2.7903 . 2_666 no Cl3 H421 3.04(5) . 2_566 no Cl3 H171 3.13(4) . 2_666 no Cl3 H191 2.60(7) . 2_666 no Cl4 H12 2.7395 . . no Cl4 H422 3.07(5) . . no Cl4 H203 2.5534 . . no Cl4 H111 2.89(7) . 2_666 no Cl4 H205 2.5645 . . no Cl4 H172 2.83(4) . . no Cl4 H192 2.62(7) . . no Cl6 H212 2.73(4) . . no Cl6 H222 3.13(5) . . no Cl7 H152 2.93(5) . . no Cl7 H211 2.98(4) . . no Cl8 H502 2.92(9) . . no Cl9 H141 2.97(4) . 2_666 no Cl11 H13 3.0186 . . no Cl11 H431 2.97(4) . . no Cl11 H102 3.12(6) . 2_666 no Cl11 H112 2.94(5) . 2_666 no Cl12 H281 2.92(6) . . no Cl13 H462 3.14(6) . . no Cl14 H231 3.14(5) . . no Cl15 H232 2.99(5) . . no Cl15 H241 3.03(3) . . no Cl16 H361 3.08(5) . . no Cl16 H472 3.11(6) . . no Cl17 H242 3.00(7) . . no Cl18 H271 3.13(9) . . no Cl19 H421 3.04(4) . 2_566 no Cl19 H142 2.91(5) . . no Cl19 H42 2.90(4) . . no Cl22 H111 3.11(5) . . no C1 H212 3.06(4) . . no C2 H221 3.07(8) . . no C5 H372 3.09(4) . . no C5 H272 3.02(9) . . no C11 H141 2.54(5) . . no C12 H142 2.55(6) . . no C21 H121 3.08(4) . . no C61 H141 2.77(4) . . no C62 H502 3.06(6) . . no C62 H142 2.80(5) . . no C71 H21 2.69(4) . . no C72 H22 2.63(4) . . no C81 H401 2.92(5) . . no C82 H402 3.01(5) . . no C111 H172 3.06(6) . 2_666 no C112 H431 2.95(5) . 2_566 no C112 H171 2.95(6) . 2_666 no C121 H21 2.71(5) . . no C121 H172 2.82(6) . 2_666 no C122 H22 2.72(5) . . no C122 H171 2.79(6) . 2_666 no C131 H61 3.04(4) . . no C131 H121 2.98(5) . . no C132 H122 2.83(5) . . no C141 H121 2.92(5) . . no C142 H122 2.74(5) . . no C172 H12 2.7903 . . no C182 H12 2.9970 . . no C191 H211 3.04(5) . . no C192 H212 2.95(5) . . no C192 H12 2.9904 . . no C211 H191 2.87(3) . . no C212 H192 2.78(3) . . no C221 H202 3.0050 . 1_556 no C222 H13 2.9599 . . no C231 H362 3.00(4) . 2_556 no C232 H361 2.98(4) . 2_556 no C232 H13 3.0397 . . no C241 H630 3.0207 . . no C241 H620 3.0796 . . no C241 H271 2.88(5) . . no C241 H362 2.87(4) . 2_556 no C241 H352 3.07(6) . 2_556 no C242 H272 2.87(5) . . no C242 H361 2.86(4) . 2_556 no C271 H241 2.87(5) . . no C272 H242 2.87(5) . . no C281 H204 2.9167 . . no C282 H202 2.9486 . . no C301 H321 2.79(5) . . no C302 H322 2.76(5) . . no C321 H301 2.86(4) . . no C322 H302 2.86(5) . . no C331 H291 2.93(6) . 2_556 no C341 H291 2.80(7) . 2_556 no C342 H292 2.93(7) . 2_555 no C351 H291 2.80(8) . 2_556 no C352 H292 2.90(8) . 2_555 no C361 H482 3.02(9) . 1_556 no C361 H291 2.91(8) . 2_556 no C362 H481 3.09(9) . . no C371 H291 3.01(7) . 2_556 no C372 H462 3.04(4) . . no C372 H15 3.0609 . 1_455 no C381 H291 3.05(6) . 2_556 no C381 H461 3.04(5) . . no C382 H462 2.89(5) . . no C391 H371 2.55(5) . . no C392 H372 2.48(5) . . no C401 H371 2.78(5) . . no C402 H372 2.65(5) . . no C412 H31 3.09(5) . 2_566 no C432 H15 3.0435 . 1_455 no C441 H461 2.99(3) . . no C451 H441 2.76(3) . . no C452 H442 2.71(3) . . no C461 H441 2.62(5) . . no C462 H442 2.70(5) . . no C481 H321 2.92(6) . 2_556 no C482 H322 3.02(7) . 2_555 no C491 H321 3.07(7) . 2_556 no C491 H341 3.06(3) . 2_556 no C501 H61 2.69(4) . . no C501 H301 2.95(6) . . no C502 H302 2.95(6) . . no C502 H62 2.79(5) . . no H12 Cl4 2.7395 . . no H12 H172 2.5930 . . no H12 C192 2.9904 . . no H12 C172 2.7903 . . no H12 C182 2.9970 . . no H13 Cl11 3.0186 . . no H13 C232 3.0397 . . no H13 C222 2.9599 . . no H14 H431 2.5580 . . no H14 Cl3 2.7903 . 2_666 no H15 C372 3.0609 . . no H15 H372 2.2330 . . no H15 C432 3.0435 . . no H21 H32 2.57(8) . 2_566 no H21 C121 2.71(5) . . no H21 C71 2.69(4) . . no H22 C122 2.72(5) . . no H22 C72 2.63(4) . . no H31 C412 3.09(5) . 2_566 no H32 H21 2.57(8) . 2_566 no H42 Cl19 2.90(4) . . no H61 Pd1 3.68(4) . . no H61 C131 3.04(4) . . no H61 H501 2.37(6) . . no H61 C501 2.69(4) . . no H62 Pd2 3.66(5) . . no H62 C502 2.79(5) . . no H62 H502 2.33(8) . . no H81 H401 2.38(8) . . no H81 Pd1 3.02(3) . . no H81 Cl1 2.39(9) . . no H82 H402 2.48(8) . . no H82 Cl2 2.42(9) . . no H82 Pd2 3.17(4) . . no H102 Cl11 3.12(6) . 2_666 no H111 H432 2.46(8) . 2_566 no H111 Cl4 2.89(7) . 2_666 no H111 Cl22 3.11(5) . 1_556 no H112 H431 2.44(9) . 2_566 no H112 Cl11 2.94(5) . 2_666 no H112 Cl3 2.97(7) . . no H121 C141 2.92(5) . . no H121 C21 3.08(4) . . no H121 C131 2.98(5) . . no H122 Cl3 3.04(4) . . no H122 C142 2.74(5) . . no H122 H142 2.60(6) . . no H122 C132 2.83(5) . . no H141 Cl9 2.97(4) . 2_666 no H141 C11 2.54(5) . . no H141 C61 2.77(4) . . no H142 Cl19 2.91(5) . . no H142 H122 2.60(6) . . no H142 C62 2.80(5) . . no H142 C12 2.55(6) . . no H152 Cl7 2.93(5) . 2_665 no H171 H191 2.28(4) . . no H171 C122 2.79(6) . 2_666 no H171 C112 2.95(6) . 2_666 no H171 Cl3 3.13(4) . 2_666 no H172 C111 3.06(6) . 2_666 no H172 H12 2.5930 . . no H172 H192 2.29(4) . . no H172 Cl4 2.83(4) . . no H172 C121 2.82(6) . 2_666 no H191 Cl3 2.60(7) . 2_666 no H191 H171 2.28(4) . . no H191 C211 2.87(3) . . no H192 C212 2.78(3) . . no H192 H172 2.29(4) . . no H192 Cl4 2.62(7) . . no H201 H212 2.5729 . . no H201 Cl2 2.8412 . . no H202 H221 2.3149 . . no H202 C221 3.0050 . . no H202 C282 2.9486 . . no H203 Cl4 2.5534 . . no H204 C281 2.9167 . . no H204 H281 2.5246 . . no H205 Cl4 2.5645 . . no H205 H272 2.4685 . . no H211 C191 3.04(5) . . no H211 Cl7 2.98(4) . 1_556 no H212 C1 3.06(4) . . no H212 H201 2.5729 . . no H212 Cl6 2.73(4) . . no H212 C192 2.95(5) . . no H221 H202 2.3149 . 1_556 no H221 C2 3.07(8) . 1_556 no H222 Cl6 3.13(5) . . no H231 Cl14 3.14(5) . 2_656 no H232 Cl15 2.99(5) . . no H241 Cl15 3.03(3) . . no H241 C271 2.87(5) . . no H242 Cl17 3.00(7) . . no H242 C272 2.87(5) . . no H271 C241 2.88(5) . . no H271 Cl18 3.13(9) . . no H272 C242 2.87(5) . . no H272 H205 2.4685 . . no H272 C5 3.02(9) . . no H281 Cl12 2.92(6) . . no H281 H204 2.5246 . . no H291 C341 2.80(7) . 2_556 no H291 C371 3.01(7) . 2_556 no H291 C331 2.93(6) . 2_556 no H291 C381 3.05(6) . 2_556 no H291 C361 2.91(8) . 2_556 no H291 C351 2.80(8) . 2_556 no H292 C352 2.90(8) . 2_555 no H292 C342 2.93(7) . 2_555 no H301 C501 2.95(6) . . no H301 C321 2.86(4) . . no H302 C502 2.95(6) . . no H302 C322 2.86(5) . . no H310 Cl3 3.1066 . . no H321 C301 2.79(5) . . no H321 H341 2.32(7) . . no H321 C491 3.07(7) . 2_556 no H321 C481 2.92(6) . 2_556 no H322 C302 2.76(5) . . no H322 C482 3.02(7) . 2_555 no H322 H342 2.35(6) . . no H340 Cl3 2.6774 . . no H341 Cl2 2.90(5) . 2_556 no H341 H321 2.32(7) . . no H341 C491 3.06(3) . 2_556 no H342 Cl1 2.87(5) . 2_556 no H342 H322 2.35(6) . . no H351 Cl2 2.81(7) . 2_556 no H352 Cl1 2.82(7) . 2_556 no H352 C241 3.07(6) . 2_556 no H360 Cl3 2.8782 . . no H361 Cl16 3.08(5) . 1_455 no H361 C232 2.98(4) . 2_556 no H361 C242 2.86(4) . 2_556 no H362 C241 2.87(4) . 2_556 no H362 C231 3.00(4) . 2_556 no H371 C391 2.55(5) . . no H371 C401 2.78(5) . . no H372 C392 2.48(5) . . no H372 C5 3.09(4) . 1_455 no H372 H15 2.2330 . 1_455 no H372 C402 2.65(5) . . no H401 Cl1 2.68(5) . . no H401 Pd1 3.38(6) . . no H401 C81 2.92(5) . . no H401 H81 2.38(8) . . no H402 H82 2.48(8) . . no H402 Pd2 3.55(6) . . no H402 C82 3.01(5) . . no H402 Cl2 3.06(5) . . no H421 Cl19 3.04(4) . 2_566 no H421 Cl3 3.04(5) . 2_566 no H422 Cl4 3.07(5) . 1_455 no H431 H14 2.5580 . 1_455 no H431 Cl11 2.97(4) . 1_455 no H431 H112 2.44(9) . 2_566 no H431 C112 2.95(5) . 2_566 no H432 H111 2.46(8) . 2_566 no H441 H461 2.49(5) . . no H441 C451 2.76(3) . . no H441 C461 2.62(5) . . no H442 C462 2.70(5) . . no H442 C452 2.71(3) . . no H461 H441 2.49(5) . . no H461 C381 3.04(5) . . no H461 C441 2.99(3) . . no H462 C372 3.04(4) . . no H462 C382 2.89(5) . . no H462 Cl13 3.14(6) . 1_455 no H472 Cl16 3.11(6) . 1_454 no H481 C362 3.09(9) . . no H482 C361 3.02(9) . . no H491 Cl2 3.01(5) . . no H492 Cl1 2.73(6) . . no H501 H61 2.37(6) . . no H501 Pd1 2.96(4) . . no H502 Cl8 2.92(9) . . no H502 C62 3.06(6) . . no H502 Pd2 2.99(4) . . no H502 H62 2.33(8) . . no H620 Cl3 2.7044 . 2_666 no H620 C241 3.0796 . . no H630 C241 3.0207 . . no H630 Cl3 2.7381 . 2_666 no loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A # #D H A D - H H...A D...A D - H...A symm(A) # C2 H12 Cl4 0.9704 2.7395 3.613(11) 149.98 . C4 H14 Cl3 0.9709 2.7903 3.682(10) 153.08 2_666 C81 H81 Cl1 0.99(9) 2.39(9) 3.371(8) 178(4) . C82 H82 Cl2 0.96(9) 2.42(9) 3.369(8) 168(5) . C172 H172 Cl4 0.98(6) 2.83(4) 3.660(8) 143(3) . C191 H191 Cl3 0.86(7) 2.60(7) 3.405(9) 155(3) 2_666 C192 H192 Cl4 0.94(7) 2.62(7) 3.368(9) 137(3) . C3 H203 Cl4 0.9708 2.5534 3.472(12) 157.83 . C5 H205 Cl4 0.9707 2.5645 3.507(18) 163.86 . C212 H212 Cl6 0.92(6) 2.73(4) 3.468(8) 138(4) . C351 H351 Cl2 0.94(7) 2.81(7) 3.466(8) 128(4) 2_556 C352 H352 Cl1 0.87(7) 2.82(7) 3.411(8) 126(4) 2_556 C401 H401 Cl1 0.99(5) 2.68(5) 3.590(8) 154(3) . C492 H492 Cl1 0.87(6) 2.73(6) 3.565(10) 161(4) . C6 H620 Cl3 0.9698 2.7044 3.450(12) 134.06 2_666 # End of Crystallographic Information File # Complex # 4 data_S1421A _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C54 H44 N2 O4 P2 Pd2 , (CH2Cl2)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 1397.45 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' '-x, -x+y, -z+1/3' 'x-y, -y, -z+2/3' _cell_length_a 13.009(2) _cell_length_b 13.009(2) _cell_length_c 29.706(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4353.7(13) _cell_formula_units_Z 3 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_diffrn 1.599 _exptl_crystal_F_000 2106 _exptl_absorpt_coefficient_mu 1.09 _exptl_absorpt_correction_type 'Delta-F' _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4T' _diffrn_measurement_method '\w-scan' _diffrn_reflns_number 12388 _diffrn_reflns_av_R_equivalents 0.1147 _diffrn_reflns_av_sigmaI/netI 0.1329 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5699 _reflns_number_observed 3793 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 186 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^)+( 0.0667P)^2^+0.0000P] where =(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.13(6) _refine_ls_number_reflns 5513 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1111 _refine_ls_R_factor_obs 0.0653 _refine_ls_wR_factor_all 0.1624 _refine_ls_wR_factor_obs 0.1387 _refine_ls_goodness_of_fit_all 0.988 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.011 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max -2.204 _refine_ls_shift/esd_mean 0.006 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 Pd1 Pd 0.36067(6) 0.18223(6) 0.21680(2) 0.0350(2) Uani 1 d . . P1 P 0.5001(2) 0.3676(2) 0.18973(7) 0.0376(6) Uani 1 d . . Cl1 Cl 0.0382(4) 0.1372(4) 0.30919(10) 0.0922(12) Uani 1 d . . Cl2 Cl 0.0745(3) 0.2275(3) 0.21816(9) 0.0725(9) Uani 1 d . . Cl4 Cl 0.1744(5) 0.6864(5) 0.03177(15) 0.132(2) Uani 1 d . . Cl3 Cl 0.0651(5) 0.4351(5) 0.05016(11) 0.120(2) Uani 1 d . . C16 C 0.3011(10) 0.3500(8) 0.0596(3) 0.041(2) Uani 1 d . . H161 H 0.2595(10) 0.3445(8) 0.0334(3) 0.049 Uiso 1 calc R . C20 C 0.1445(8) -0.0197(8) 0.1893(2) 0.030(2) Uani 1 d . . C6 C 0.7267(10) 0.4765(9) 0.1476(3) 0.052(3) Uani 1 d . . H61 H 0.7124(10) 0.5356(9) 0.1372(3) 0.062 Uiso 1 calc R . C15 C 0.4072(10) 0.4530(9) 0.0683(3) 0.046(3) Uani 1 d . . H151 H 0.4368(10) 0.5162(9) 0.0482(3) 0.055 Uiso 1 calc R . C18 C 0.3183(8) 0.2626(8) 0.1274(2) 0.034(2) Uani 1 d . . C7 C 0.5274(10) 0.5019(8) 0.2182(3) 0.043(2) Uani 1 d . . C25 C 0.0393(8) -0.1276(8) 0.1872(3) 0.032(2) Uani 1 d . . C22 C 0.1820(9) -0.0544(8) 0.2638(3) 0.039(2) Uani 1 d . . H221 H 0.2273(9) -0.0316(8) 0.2900(3) 0.047 Uiso 1 calc R . C19 C 0.1818(8) 0.0685(8) 0.1531(3) 0.035(2) Uani 1 d . . H191 H 0.1366(8) 0.0521(8) 0.1267(3) 0.048 Uiso 1 calc R . C26 C 0.4463(9) 0.2375(11) 0.3060(3) 0.049(3) Uani 1 d . . C14 C 0.4685(9) 0.4606(8) 0.1072(3) 0.045(2) Uani 1 d . . H141 H 0.5398(9) 0.5295(8) 0.1132(3) 0.054 Uiso 1 calc R . C12 C 0.6378(10) 0.5805(9) 0.2364(3) 0.058(3) Uani 1 d . . H121 H 0.7027(10) 0.5695(9) 0.2327(3) 0.070 Uiso 1 calc R . C23 C 0.0800(9) -0.1600(9) 0.2632(3) 0.045(3) Uani 1 d . . H231 H 0.0587(9) -0.2076(9) 0.2887(3) 0.054 Uiso 1 calc R . C17 C 0.2568(9) 0.2576(9) 0.0884(2) 0.043(3) Uani 1 d . . H171 H 0.1845(9) 0.1900(9) 0.0822(2) 0.052 Uiso 1 calc R . C2 C 0.6704(10) 0.3024(9) 0.1907(3) 0.055(3) Uani 1 d . . H21 H 0.6180(10) 0.2433(9) 0.2101(3) 0.066 Uiso 1 calc R . C3 C 0.7766(10) 0.3047(12) 0.1778(3) 0.059(3) Uani 1 d . . H31 H 0.7943(10) 0.2485(12) 0.1888(3) 0.071 Uiso 1 calc R . C9 C 0.4436(14) 0.6143(11) 0.2482(3) 0.072(4) Uani 1 d . . H91 H 0.3792(14) 0.6259(11) 0.2521(3) 0.087 Uiso 1 calc R . C5 C 0.8305(11) 0.4787(11) 0.1356(3) 0.057(3) Uani 1 d . . H51 H 0.8869(11) 0.5407(11) 0.1182(3) 0.069 Uiso 1 calc R . C1 C 0.6431(8) 0.3862(9) 0.1751(3) 0.039(2) Uani 1 d . . C8 C 0.4318(12) 0.5196(10) 0.2246(3) 0.059(3) Uani 1 d . . H81 H 0.3583(12) 0.4657(10) 0.2125(3) 0.071 Uiso 1 calc R . C4 C 0.8505(11) 0.3894(12) 0.1495(4) 0.060(3) Uani 1 d . . H41 H 0.9169(11) 0.3878(12) 0.1389(4) 0.072 Uiso 1 calc R . C21 C 0.2223(8) 0.0222(9) 0.2266(3) 0.036(2) Uani 1 d . . C27 C 0.5262(10) 0.2463(12) 0.3451(3) 0.069(4) Uani 1 d . . H271 H 0.6076(11) 0.2885(68) 0.3355(9) 0.103 Uiso 1 calc R . H272 H 0.5060(52) 0.1680(12) 0.3548(19) 0.103 Uiso 1 calc R . H273 H 0.5154(59) 0.2880(69) 0.3696(11) 0.103 Uiso 1 calc R . C10 C 0.5537(15) 0.6933(12) 0.2662(3) 0.073(4) Uani 1 d . . H101 H 0.5623(15) 0.7584(12) 0.2824(3) 0.088 Uiso 1 calc R . C11 C 0.6472(11) 0.6791(11) 0.2612(4) 0.063(3) Uani 1 d . . H111 H 0.7195(11) 0.7338(11) 0.2740(4) 0.075 Uiso 1 calc R . C13 C 0.4258(8) 0.3675(8) 0.1373(2) 0.034(2) Uani 1 d . . C24 C 0.0052(9) -0.2007(9) 0.2257(3) 0.042(2) Uani 1 d . . H241 H -0.0648(9) -0.2735(9) 0.2261(3) 0.051 Uiso 1 calc R . C29 C 0.0447(15) 0.5426(13) 0.0267(4) 0.094(5) Uani 1 d . . H291 H -0.0216(15) 0.5434(13) 0.0414(4) 0.127 Uiso 1 calc R . H292 H 0.0249(15) 0.5246(13) -0.0049(4) 0.127 Uiso 1 calc R . C28 C 0.1336(12) 0.2470(12) 0.2718(4) 0.075(4) Uani 1 d . . H281 H 0.1507(12) 0.3239(12) 0.2832(4) 0.101 Uiso 1 calc R . H282 H 0.2078(12) 0.2465(12) 0.2703(4) 0.101 Uiso 1 calc R . N1 N 0.2762(7) 0.1683(6) 0.1589(2) 0.032(2) Uani 1 d . . O2 O 0.3903(7) 0.2902(7) 0.3074(2) 0.056(2) Uani 1 d . . O1 O 0.4449(6) 0.1759(6) 0.2742(2) 0.049(2) 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 Pd1 0.0362(4) 0.0310(4) 0.0353(3) 0.0003(3) -0.0040(3) 0.0149(4) P1 0.041(2) 0.0285(14) 0.0391(10) -0.0016(10) -0.0037(10) 0.0147(13) Cl1 0.088(3) 0.097(3) 0.076(2) 0.003(2) -0.017(2) 0.034(2) Cl2 0.076(2) 0.079(2) 0.070(2) 0.000(2) 0.005(2) 0.045(2) Cl4 0.147(5) 0.112(4) 0.136(3) -0.029(3) -0.021(3) 0.065(4) Cl3 0.173(5) 0.134(4) 0.079(2) 0.011(2) -0.003(3) 0.095(4) C16 0.054(7) 0.031(6) 0.043(4) 0.003(4) 0.003(4) 0.025(5) C20 0.027(5) 0.025(5) 0.036(4) -0.003(4) 0.002(4) 0.012(5) C6 0.053(8) 0.030(6) 0.066(6) 0.011(5) 0.000(5) 0.015(6) C15 0.064(7) 0.044(7) 0.043(4) 0.016(4) 0.012(4) 0.037(6) C18 0.042(6) 0.032(6) 0.031(3) 0.005(4) 0.004(4) 0.020(5) C7 0.056(7) 0.016(5) 0.045(4) 0.000(4) 0.006(4) 0.009(5) C25 0.026(5) 0.022(5) 0.048(4) 0.000(4) 0.004(4) 0.012(4) C22 0.045(6) 0.026(5) 0.032(4) 0.004(3) -0.003(4) 0.007(5) C19 0.037(6) 0.036(6) 0.037(4) -0.006(4) 0.001(4) 0.021(5) C26 0.045(6) 0.070(9) 0.040(4) 0.003(5) 0.005(4) 0.035(6) C14 0.051(6) 0.023(5) 0.052(4) -0.002(4) 0.000(4) 0.012(5) C12 0.057(7) 0.022(6) 0.059(5) -0.011(5) 0.010(5) -0.007(6) C23 0.039(6) 0.045(6) 0.052(5) 0.012(4) 0.009(4) 0.021(5) C17 0.044(7) 0.050(7) 0.038(4) 0.002(4) 0.002(4) 0.026(6) C2 0.058(8) 0.041(6) 0.056(5) 0.013(5) -0.006(5) 0.018(6) C3 0.046(7) 0.070(9) 0.070(6) -0.003(6) -0.005(6) 0.036(7) C9 0.113(13) 0.058(9) 0.057(6) -0.012(6) -0.010(7) 0.051(9) C5 0.048(8) 0.041(7) 0.068(6) 0.007(5) 0.006(6) 0.011(6) C1 0.027(5) 0.033(6) 0.047(4) 0.004(4) -0.005(4) 0.007(5) C8 0.082(9) 0.051(8) 0.050(5) -0.015(5) -0.014(5) 0.038(8) C4 0.046(7) 0.067(9) 0.067(6) -0.005(6) 0.004(5) 0.028(7) C21 0.035(6) 0.043(6) 0.039(4) -0.002(4) -0.009(4) 0.025(5) C27 0.053(7) 0.101(11) 0.047(5) 0.000(6) -0.001(5) 0.035(8) C10 0.121(14) 0.048(8) 0.046(5) 0.000(5) 0.013(7) 0.039(9) C11 0.055(8) 0.042(7) 0.062(6) 0.005(5) -0.003(6) 0.002(6) C13 0.037(6) 0.027(5) 0.042(4) -0.002(3) -0.001(4) 0.018(5) C24 0.027(5) 0.044(7) 0.051(5) 0.012(4) 0.006(4) 0.015(5) C29 0.145(15) 0.098(12) 0.076(7) 0.018(7) 0.022(9) 0.088(12) C28 0.054(9) 0.078(9) 0.089(7) -0.017(7) -0.016(7) 0.031(8) N1 0.030(4) 0.027(4) 0.039(3) -0.002(3) 0.002(3) 0.013(3) O2 0.074(6) 0.078(6) 0.040(3) -0.010(3) -0.005(3) 0.055(5) O1 0.045(4) 0.054(5) 0.058(4) -0.005(3) -0.011(3) 0.033(4) _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 Pd1 C21 1.978(10) . ? Pd1 N1 1.999(6) . ? Pd1 O1 2.051(6) . ? Pd1 P1 2.319(3) . ? P1 C1 1.805(10) . ? P1 C7 1.809(9) . ? P1 C13 1.833(8) . ? Cl1 C28 1.743(13) . ? Cl2 C28 1.733(11) . ? Cl4 C29 1.79(2) . ? Cl3 C29 1.697(13) . ? C16 C17 1.347(13) . ? C16 C15 1.385(14) . ? C20 C25 1.389(12) . ? C20 C21 1.413(11) . ? C20 C19 1.467(12) . ? C6 C5 1.38(2) . ? C6 C1 1.397(13) . ? C15 C14 1.379(12) . ? C18 C17 1.391(11) . ? C18 C13 1.412(13) . ? C18 N1 1.418(10) . ? C7 C8 1.387(15) . ? C7 C12 1.390(14) . ? C25 C24 1.409(11) . ? C25 C25 1.51(2) 5 ? C22 C23 1.351(13) . ? C22 C21 1.403(12) . ? C19 N1 1.277(11) . ? C26 O2 1.226(13) . ? C26 O1 1.234(11) . ? C26 C27 1.524(13) . ? C14 C13 1.379(11) . ? C12 C11 1.43(2) . ? C23 C24 1.397(13) . ? C2 C1 1.384(14) . ? C2 C3 1.419(15) . ? C3 C4 1.34(2) . ? C9 C8 1.357(15) . ? C9 C10 1.39(2) . ? C5 C4 1.37(2) . ? C10 C11 1.33(2) . ? 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 C21 Pd1 N1 82.0(3) . . ? C21 Pd1 O1 93.4(3) . . ? N1 Pd1 O1 172.7(3) . . ? C21 Pd1 P1 166.6(2) . . ? N1 Pd1 P1 84.5(2) . . ? O1 Pd1 P1 100.0(2) . . ? C1 P1 C7 106.9(5) . . ? C1 P1 C13 107.6(4) . . ? C7 P1 C13 104.3(4) . . ? C1 P1 Pd1 116.2(3) . . ? C7 P1 Pd1 121.0(3) . . ? C13 P1 Pd1 99.0(3) . . ? C17 C16 C15 121.4(9) . . ? C25 C20 C21 125.3(8) . . ? C25 C20 C19 122.1(8) . . ? C21 C20 C19 112.4(8) . . ? C5 C6 C1 120.7(10) . . ? C14 C15 C16 119.0(8) . . ? C17 C18 C13 119.2(8) . . ? C17 C18 N1 123.0(9) . . ? C13 C18 N1 117.8(7) . . ? C8 C7 C12 120.5(10) . . ? C8 C7 P1 117.7(8) . . ? C12 C7 P1 121.6(9) . . ? C20 C25 C24 117.7(8) . . ? C20 C25 C25 122.5(8) . 5 ? C24 C25 C25 119.8(9) . 5 ? C23 C22 C21 122.6(9) . . ? N1 C19 C20 117.9(7) . . ? O2 C26 O1 124.7(9) . . ? O2 C26 C27 120.4(9) . . ? O1 C26 C27 114.8(10) . . ? C13 C14 C15 121.1(9) . . ? C7 C12 C11 116.9(12) . . ? C22 C23 C24 122.7(9) . . ? C16 C17 C18 120.5(10) . . ? C1 C2 C3 121.5(10) . . ? C4 C3 C2 118.6(12) . . ? C8 C9 C10 118.6(14) . . ? C4 C5 C6 120.0(11) . . ? C2 C1 C6 117.4(10) . . ? C2 C1 P1 117.8(8) . . ? C6 C1 P1 124.8(8) . . ? C9 C8 C7 121.2(12) . . ? C3 C4 C5 121.6(12) . . ? C22 C21 C20 113.8(8) . . ? C22 C21 Pd1 133.1(6) . . ? C20 C21 Pd1 112.9(6) . . ? C11 C10 C9 122.1(13) . . ? C10 C11 C12 120.7(12) . . ? C14 C13 C18 118.9(8) . . ? C14 C13 P1 124.7(7) . . ? C18 C13 P1 116.4(6) . . ? C23 C24 C25 117.8(9) . . ? Cl3 C29 Cl4 111.8(9) . . ? Cl2 C28 Cl1 112.6(7) . . ? C19 N1 C18 123.3(7) . . ? C19 N1 Pd1 114.5(6) . . ? C18 N1 Pd1 122.2(6) . . ? C26 O1 Pd1 116.4(7) . . ? _refine_diff_density_max 0.492 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.104 #================================================================ # Dr. A.L.Spek, Laboratory of Crystal and Structural Chemistry # Bijvoet Center for Biomolecular Research, Utrecht University. # (Kruytgebouw, room N801), Padualaan 8, 3584 CH Utrecht, The Netherlands. # E-mail: spea@xray.chem.ruu.nl http://www.cryst.chem.ruu.nl # spea@xray6.chem.ruu.nl # FAX : (31)-30-2533940 PHONE :(31)-30-2532538/2532533/2533502 #================================================================