Supplementary information (ESI) for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_section_title ;Complexes as metalloligands in network formation: synthesis and characterisation of a mixed-metal coordination network containing palladium and zinc ; _publ_contact_author_name 'Andrew Burrows' _publ_contact_author_email A.D.BURROWS@BATH.AC.UK loop_ _publ_author_name A.Burrows M.Mahon C.T.F.Wong # Attachment 'B718961C1.cif' data_c:\x-ray\compound_2(h06adb12) _database_code_depnum_ccdc_archive 'CCDC 670772' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H94 Cl4 N4 O29.25 Pd2 Zn4' _chemical_formula_weight 2015.52 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' Zn Zn 0.2839 1.4301 '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 orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.5100(1) _cell_length_b 27.3700(2) _cell_length_c 27.9910(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10350.20(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 346299 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4104 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.76 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 118101 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 27.49 _reflns_number_total 22846 _reflns_number_gt 19707 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The THF molecules exhibited signs of disorder in this structure, but only one (that based on O21) could be resolved with any success into a model dispersed over 2 sites in a 65:35 ratio. The lattice solvent in the fragments based on O25, O26, O29 and O30 exhibited 85, 100, 70 and 70% occupancies respectively. ADPs in disordered THFs were constrained in the final least squares, as were the O-C and C-C distances. Despite the inability to resolves the solvent disorder throughout, the structure is unambiguous. O...O distances between the non-bridging ligated waters and the oxygens in proximate lattice THF suggests that additional hydrogen-bonding is present. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1209P)^2^+19.4435P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(15) _refine_ls_number_reflns 22846 _refine_ls_number_parameters 1005 _refine_ls_number_restraints 257 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1847 _refine_ls_wR_factor_gt 0.1716 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.06508(4) 0.36275(2) 1.00432(2) 0.03436(15) Uani 1 1 d . . . Pd2 Pd 0.20022(4) 0.71132(2) 0.88543(2) 0.03304(15) Uani 1 1 d . . . Zn1 Zn 0.61598(6) 0.49630(3) 0.95858(3) 0.02996(19) Uani 1 1 d . A . Zn2 Zn 0.40809(6) 0.53620(3) 1.02705(3) 0.02920(19) Uani 1 1 d . . . Zn3 Zn 0.76001(6) 0.68700(3) 0.75520(3) 0.02983(19) Uani 1 1 d . . . Zn4 Zn 0.56382(6) 0.76478(3) 0.71517(3) 0.02930(19) Uani 1 1 d . . . Cl1 Cl 0.15236(19) 0.36782(14) 1.07548(9) 0.0650(7) Uani 1 1 d . . . Cl2 Cl -0.02173(19) 0.35961(14) 0.93409(9) 0.0661(8) Uani 1 1 d . . . Cl3 Cl 0.11693(17) 0.63890(9) 0.89416(12) 0.0613(7) Uani 1 1 d . . . Cl4 Cl 0.2819(2) 0.78374(11) 0.87548(14) 0.0719(8) Uani 1 1 d . . . O1 O 0.9122(4) 0.2929(2) 1.1690(2) 0.0398(13) Uani 1 1 d . . . O2 O 0.7748(4) 0.3352(2) 1.18889(19) 0.0386(13) Uani 1 1 d . . . O3 O 0.7062(5) 0.4502(2) 0.9957(2) 0.0441(14) Uani 1 1 d . . . O4 O 0.6457(5) 0.4570(3) 1.0691(2) 0.0545(19) Uani 1 1 d . . . O5 O 0.5490(4) 0.5491(2) 0.91934(19) 0.0355(12) Uani 1 1 d . . . O6 O 0.4031(4) 0.5579(2) 0.95716(19) 0.0359(12) Uani 1 1 d . . . O7 O 0.6314(4) 0.6673(2) 0.7889(2) 0.0378(12) Uani 1 1 d . . . O8 O 0.5151(4) 0.7231(2) 0.7703(2) 0.0379(13) Uani 1 1 d . . . O9 O 0.3939(4) 0.3122(2) 0.8379(2) 0.0404(13) Uani 1 1 d . . . O10 O 0.2336(5) 0.2918(3) 0.8410(3) 0.059(2) Uani 1 1 d . . . O11 O 0.5021(4) 0.4462(2) 0.9530(2) 0.0357(12) Uani 1 1 d . . . O12 O 0.3945(5) 0.4643(2) 1.01117(19) 0.0365(12) Uani 1 1 d . . . O13 O 0.8268(4) 0.7110(2) 0.8168(2) 0.0404(13) Uani 1 1 d . . . O14 O 0.7693(5) 0.7874(3) 0.8225(2) 0.0512(17) Uani 1 1 d . . . O15 O 1.0783(5) 0.8794(3) 0.9654(3) 0.058(2) Uani 1 1 d . . . O16 O 0.9184(4) 0.8938(2) 0.9494(2) 0.0433(14) Uani 1 1 d . . . O17 O 0.6714(5) 0.4667(3) 0.8931(2) 0.0476(15) Uani 1 1 d . . . O18 O 0.7424(5) 0.5478(3) 0.9599(3) 0.066(2) Uani 1 1 d D . . O19 O 0.4013(6) 0.5152(3) 1.1016(2) 0.0526(17) Uani 1 1 d D . . O20 O 0.2508(4) 0.5423(3) 1.0304(2) 0.0456(14) Uani 1 1 d D . . O21 O 0.8124(6) 0.6150(3) 0.7711(2) 0.0506(16) Uani 1 1 d D . . O22 O 0.9041(5) 0.7026(3) 0.7243(3) 0.0576(18) Uani 1 1 d . . . O23 O 0.5535(5) 0.8283(3) 0.7615(3) 0.0550(17) Uani 1 1 d D . . O24 O 0.4195(4) 0.7752(3) 0.6951(2) 0.0475(15) Uani 1 1 d . . . O25 O 0.3488(11) 0.7898(9) 0.6055(5) 0.145(8) Uani 0.85 1 d PD . . O26 O 0.2846(15) 0.7068(8) 0.7207(10) 0.193(10) Uani 1 1 d D . . O27 O 0.5636(4) 0.52780(19) 1.02443(18) 0.0296(10) Uani 1 1 d . . . O28 O 0.7118(4) 0.7590(2) 0.7396(2) 0.0324(11) Uani 1 1 d . . . O29 O 0.3879(19) 0.5229(9) 0.7168(9) 0.137(8) Uani 0.70 1 d P . . O30 O 0.971(2) 0.6885(8) 0.6375(6) 0.154(11) Uani 0.70 1 d PD . . N1 N 0.9383(5) 0.3655(3) 1.0424(2) 0.0350(14) Uani 1 1 d . . . N2 N 0.1942(5) 0.3650(3) 0.9679(2) 0.0350(14) Uani 1 1 d . . . N3 N 0.3291(5) 0.6744(3) 0.8740(2) 0.0350(14) Uani 1 1 d . . . N4 N 1.0725(5) 0.7497(3) 0.8944(2) 0.0353(14) Uani 1 1 d . . . C1 C 0.9274(6) 0.3418(3) 1.0839(3) 0.0342(16) Uani 1 1 d . . . H1 H 0.9770 0.3190 1.0930 0.041 Uiso 1 1 calc R . . C2 C 0.8477(6) 0.3488(3) 1.1141(3) 0.0317(15) Uani 1 1 d . . . C3 C 0.7740(6) 0.3817(3) 1.1005(3) 0.0348(17) Uani 1 1 d . . . H3 H 0.7196 0.3883 1.1210 0.042 Uiso 1 1 calc R . . C4 C 0.7819(6) 0.4045(3) 1.0565(3) 0.0358(17) Uani 1 1 d . . . C5 C 0.8640(6) 0.3957(3) 1.0277(3) 0.0363(17) Uani 1 1 d . . . H5 H 0.8684 0.4110 0.9974 0.044 Uiso 1 1 calc R . . C6 C 0.8434(6) 0.3227(3) 1.1615(3) 0.0324(16) Uani 1 1 d . . . C7 C 0.7037(6) 0.4406(3) 1.0387(3) 0.0379(17) Uani 1 1 d . . . C8 C 0.3533(6) 0.6365(3) 0.9006(3) 0.0329(16) Uani 1 1 d . . . H8 H 0.3089 0.6257 0.9246 0.039 Uiso 1 1 calc R . . C9 C 0.4436(5) 0.6120(3) 0.8941(3) 0.0307(15) Uani 1 1 d . . . C10 C 0.5056(6) 0.6271(3) 0.8596(3) 0.0318(16) Uani 1 1 d . . . H10 H 0.5663 0.6103 0.8545 0.038 Uiso 1 1 calc R . . C11 C 0.4815(5) 0.6671(3) 0.8315(3) 0.0305(15) Uani 1 1 d . . . C12 C 0.3908(6) 0.6901(3) 0.8395(3) 0.0346(16) Uani 1 1 d . . . H12 H 0.3724 0.7172 0.8204 0.042 Uiso 1 1 calc R . . C13 C 0.4688(6) 0.5694(3) 0.9265(3) 0.0324(16) Uani 1 1 d . . . C14 C 0.5477(6) 0.6876(3) 0.7931(3) 0.0333(16) Uani 1 1 d . . . C15 C 0.2650(6) 0.3964(3) 0.9818(3) 0.0358(17) Uani 1 1 d . . . H15 H 0.2541 0.4153 1.0098 0.043 Uiso 1 1 calc R . . C16 C 0.3527(6) 0.4022(3) 0.9574(3) 0.0334(16) Uani 1 1 d . . . C17 C 0.3704(6) 0.3748(3) 0.9170(3) 0.0356(17) Uani 1 1 d . . . H17 H 0.4308 0.3779 0.8999 0.043 Uiso 1 1 calc R . . C18 C 0.2972(6) 0.3421(3) 0.9019(3) 0.0355(16) Uani 1 1 d . . . C19 C 0.2100(7) 0.3380(3) 0.9269(3) 0.0394(18) Uani 1 1 d . . . H19 H 0.1600 0.3164 0.9158 0.047 Uiso 1 1 calc R . . C20 C 0.3093(7) 0.3130(4) 0.8563(3) 0.045(2) Uani 1 1 d . . . C21 C 0.4243(6) 0.4407(3) 0.9754(2) 0.0294(15) Uani 1 1 d . . . C22 C 0.9931(6) 0.7365(3) 0.8687(3) 0.0355(17) Uani 1 1 d . . . H22 H 0.9944 0.7068 0.8511 0.043 Uiso 1 1 calc R . . C23 C 0.9081(6) 0.7660(3) 0.8676(3) 0.0364(17) Uani 1 1 d . . . C24 C 0.9076(6) 0.8088(3) 0.8935(3) 0.0364(17) Uani 1 1 d . . . H24 H 0.8516 0.8298 0.8927 0.044 Uiso 1 1 calc R . . C25 C 0.9890(6) 0.8209(3) 0.9208(3) 0.0364(17) Uani 1 1 d . . . C26 C 1.0712(6) 0.7902(3) 0.9197(3) 0.0325(15) Uani 1 1 d . . . H26 H 1.1281 0.7987 0.9378 0.039 Uiso 1 1 calc R . . C27 C 0.8255(6) 0.7533(3) 0.8330(3) 0.0382(19) Uani 1 1 d . . . C28 C 0.9952(6) 0.8686(3) 0.9474(3) 0.0387(18) Uani 1 1 d . . . C29 C 0.7317(17) 0.4244(8) 0.8911(7) 0.110(6) Uani 1 1 d U . . H29A H 0.7059 0.3990 0.9130 0.132 Uiso 1 1 calc R . . H29B H 0.8003 0.4324 0.9007 0.132 Uiso 1 1 calc R . . C30 C 0.729(2) 0.4054(10) 0.8373(9) 0.137(8) Uani 1 1 d U . . H30A H 0.7852 0.4186 0.8186 0.164 Uiso 1 1 calc R . . H30B H 0.7304 0.3692 0.8359 0.164 Uiso 1 1 calc R . . C31 C 0.6346(19) 0.4246(9) 0.8201(8) 0.125(7) Uani 1 1 d U . . H31A H 0.5826 0.3993 0.8221 0.150 Uiso 1 1 calc R . . H31B H 0.6407 0.4353 0.7864 0.150 Uiso 1 1 calc R . . C32 C 0.6097(11) 0.4664(6) 0.8511(4) 0.075(3) Uani 1 1 d U . . H32A H 0.6192 0.4973 0.8332 0.090 Uiso 1 1 calc R . . H32B H 0.5393 0.4643 0.8606 0.090 Uiso 1 1 calc R . . C33 C 0.847(2) 0.5383(9) 0.9673(11) 0.147(9) Uani 1 1 d DU A 1 H33A H 0.8806 0.5303 0.9369 0.176 Uiso 1 1 calc R A 1 H33B H 0.8571 0.5112 0.9902 0.176 Uiso 1 1 calc R A 1 C34 C 0.884(2) 0.5865(10) 0.988(2) 0.38(4) Uani 1 1 d DU A 1 H34A H 0.8684 0.5893 1.0222 0.458 Uiso 1 1 calc R A 1 H34B H 0.9556 0.5905 0.9828 0.458 Uiso 1 1 calc R A 1 C35 C 0.8260(16) 0.6228(6) 0.9591(10) 0.142(8) Uani 1 1 d DU A 1 H35A H 0.8084 0.6515 0.9790 0.171 Uiso 1 1 calc R A 1 H35B H 0.8651 0.6341 0.9313 0.171 Uiso 1 1 calc R A 1 C36 C 0.7369(12) 0.5971(6) 0.9433(6) 0.092(5) Uani 1 1 d DU A 1 H36A H 0.6772 0.6133 0.9564 0.111 Uiso 1 1 calc R A 1 H36B H 0.7325 0.5977 0.9080 0.111 Uiso 1 1 calc R A 1 C37 C 0.3999(19) 0.5476(7) 1.1414(5) 0.109(5) Uani 1 1 d DU . . H37A H 0.3494 0.5733 1.1365 0.131 Uiso 1 1 calc R . . H37B H 0.4652 0.5635 1.1451 0.131 Uiso 1 1 calc R . . C38 C 0.376(2) 0.5191(9) 1.1847(8) 0.141(8) Uani 1 1 d DU . . H38A H 0.3048 0.5114 1.1873 0.169 Uiso 1 1 calc R . . H38B H 0.3997 0.5350 1.2143 0.169 Uiso 1 1 calc R . . C39 C 0.437(3) 0.4759(10) 1.1713(8) 0.161(10) Uani 1 1 d DU . . H39A H 0.4169 0.4471 1.1905 0.193 Uiso 1 1 calc R . . H39B H 0.5077 0.4825 1.1770 0.193 Uiso 1 1 calc R . . C40 C 0.4181(17) 0.4668(6) 1.1190(6) 0.102(5) Uani 1 1 d DU . . H40A H 0.4762 0.4516 1.1034 0.123 Uiso 1 1 calc R . . H40B H 0.3593 0.4457 1.1140 0.123 Uiso 1 1 calc R . . C41 C 0.1837(15) 0.5299(10) 0.9925(7) 0.127(7) Uani 1 1 d DU B 1 H41A H 0.2129 0.5033 0.9729 0.152 Uiso 1 1 calc R B 1 H41B H 0.1741 0.5586 0.9715 0.152 Uiso 1 1 calc R B 1 C42 C 0.0869(18) 0.5138(13) 1.0112(9) 0.178(12) Uani 1 1 d DU B 1 H42A H 0.0314 0.5253 0.9909 0.213 Uiso 1 1 calc R B 1 H42B H 0.0834 0.4779 1.0147 0.213 Uiso 1 1 calc R B 1 C43 C 0.0888(17) 0.5386(11) 1.0573(9) 0.144(8) Uani 1 1 d DU B 1 H43A H 0.0418 0.5239 1.0803 0.172 Uiso 1 1 calc R B 1 H43B H 0.0756 0.5740 1.0543 0.172 Uiso 1 1 calc R B 1 C44 C 0.1924(19) 0.5284 1.0700(9) 0.205(15) Uani 1 1 d DU B 1 H44A H 0.2117 0.5474 1.0987 0.246 Uiso 1 1 calc R B 1 H44B H 0.2014 0.4932 1.0769 0.246 Uiso 1 1 calc R B 1 C45 C 0.804(2) 0.5940(8) 0.8162(6) 0.080(6) Uani 0.65 1 d PDU C 1 H45A H 0.7335 0.5877 0.8235 0.096 Uiso 0.65 1 calc PR C 1 H45B H 0.8305 0.6166 0.8406 0.096 Uiso 0.65 1 calc PR C 1 C46 C 0.860(2) 0.5477(10) 0.8174(8) 0.107(8) Uani 0.65 1 d PDU C 1 H46A H 0.8162 0.5204 0.8274 0.128 Uiso 0.65 1 calc PR C 1 H46B H 0.9159 0.5500 0.8399 0.128 Uiso 0.65 1 calc PR C 1 C47 C 0.896(3) 0.5400(12) 0.7682(9) 0.129(11) Uani 0.65 1 d PDU C 1 H47A H 0.8769 0.5071 0.7566 0.155 Uiso 0.65 1 calc PR C 1 H47B H 0.9685 0.5433 0.7667 0.155 Uiso 0.65 1 calc PR C 1 C48 C 0.847(2) 0.5786(8) 0.7392(7) 0.090(7) Uani 0.65 1 d PDU C 1 H48A H 0.8944 0.5928 0.7163 0.108 Uiso 0.65 1 calc PR C 1 H48B H 0.7906 0.5646 0.7211 0.108 Uiso 0.65 1 calc PR C 1 C49 C 0.6136(11) 0.8718(4) 0.7586(5) 0.077(4) Uani 1 1 d D . . H49A H 0.5808 0.8966 0.7383 0.092 Uiso 1 1 calc R . . H49B H 0.6790 0.8641 0.7446 0.092 Uiso 1 1 calc R . . C50 C 0.6250(15) 0.8900(6) 0.8068(6) 0.103(6) Uani 1 1 d D . . H50A H 0.6820 0.8744 0.8230 0.124 Uiso 1 1 calc R . . H50B H 0.6339 0.9259 0.8071 0.124 Uiso 1 1 calc R . . C51 C 0.532(2) 0.8761(8) 0.8288(8) 0.164(13) Uani 1 1 d D . . H51A H 0.5405 0.8724 0.8638 0.197 Uiso 1 1 calc R . . H51B H 0.4808 0.9009 0.8225 0.197 Uiso 1 1 calc R . . C52 C 0.5065(19) 0.8301(6) 0.8071(6) 0.124(9) Uani 1 1 d D . . H52A H 0.5294 0.8026 0.8273 0.149 Uiso 1 1 calc R . . H52B H 0.4338 0.8276 0.8034 0.149 Uiso 1 1 calc R . . C53 C 0.395(2) 0.7909(13) 0.5596(8) 0.142(10) Uani 0.85 1 d PDU . . H53A H 0.4377 0.7620 0.5545 0.170 Uiso 0.85 1 calc PR . . H53B H 0.4340 0.8211 0.5550 0.170 Uiso 0.85 1 calc PR . . C54 C 0.3080(19) 0.7898(12) 0.5284(11) 0.134(9) Uani 0.85 1 d PDU . . H54A H 0.2864 0.8237 0.5217 0.161 Uiso 0.85 1 calc PR . . H54B H 0.3260 0.7743 0.4976 0.161 Uiso 0.85 1 calc PR . . C55 C 0.228(2) 0.7633(11) 0.5499(8) 0.124(8) Uani 0.85 1 d PDU . . H55A H 0.1628 0.7776 0.5417 0.149 Uiso 0.85 1 calc PR . . H55B H 0.2288 0.7283 0.5408 0.149 Uiso 0.85 1 calc PR . . C56 C 0.2511(17) 0.7699(10) 0.5996(9) 0.121(8) Uani 0.85 1 d PDU . . H56A H 0.2468 0.7381 0.6163 0.145 Uiso 0.85 1 calc PR . . H56B H 0.2021 0.7922 0.6142 0.145 Uiso 0.85 1 calc PR . . C57 C 0.288(3) 0.6552(11) 0.718(2) 0.28(3) Uani 1 1 d DU . . H57A H 0.3581 0.6452 0.7232 0.334 Uiso 1 1 calc R . . H57B H 0.2696 0.6453 0.6856 0.334 Uiso 1 1 calc R . . C58 C 0.227(3) 0.6268(11) 0.7520(15) 0.214(16) Uani 1 1 d DU . . H58A H 0.2103 0.5940 0.7393 0.256 Uiso 1 1 calc R . . H58B H 0.2585 0.6235 0.7837 0.256 Uiso 1 1 calc R . . C59 C 0.141(3) 0.6590(11) 0.7533(15) 0.216(17) Uani 1 1 d DU . . H59A H 0.0916 0.6505 0.7284 0.259 Uiso 1 1 calc R . . H59B H 0.1080 0.6587 0.7850 0.259 Uiso 1 1 calc R . . C60 C 0.1891(15) 0.7054(8) 0.7436(8) 0.118(6) Uani 1 1 d DU . . H60A H 0.1433 0.7249 0.7236 0.141 Uiso 1 1 calc R . . H60B H 0.1957 0.7227 0.7744 0.141 Uiso 1 1 calc R . . C61 C 0.432(3) 0.5251(13) 0.6782(12) 0.119(9) Uani 0.70 1 d PU . . H61A H 0.3868 0.5336 0.6516 0.142 Uiso 0.70 1 calc PR . . H61B H 0.4674 0.4944 0.6707 0.142 Uiso 0.70 1 calc PR . . C62 C 0.508(3) 0.5699(12) 0.6916(11) 0.118(9) Uani 0.70 1 d PU . . H62A H 0.5710 0.5686 0.6737 0.142 Uiso 0.70 1 calc PR . . H62B H 0.4772 0.6027 0.6888 0.142 Uiso 0.70 1 calc PR . . C63 C 0.518(3) 0.5512(16) 0.7460(15) 0.144(12) Uani 0.70 1 d PU . . H63A H 0.5838 0.5366 0.7508 0.173 Uiso 0.70 1 calc PR . . H63B H 0.5115 0.5795 0.7679 0.173 Uiso 0.70 1 calc PR . . C64 C 0.465(3) 0.5261(15) 0.7543(14) 0.133(11) Uani 0.70 1 d PU . . H64A H 0.4336 0.5352 0.7851 0.159 Uiso 0.70 1 calc PR . . H64B H 0.4965 0.4938 0.7584 0.159 Uiso 0.70 1 calc PR . . C65 C 1.014(2) 0.6483(10) 0.6203(9) 0.102(6) Uiso 0.70 1 d PDU . . H65A H 0.9650 0.6214 0.6201 0.122 Uiso 0.70 1 calc PR . . H65B H 1.0685 0.6387 0.6421 0.122 Uiso 0.70 1 calc PR . . C66 C 1.054(2) 0.6541(11) 0.5728(8) 0.124(6) Uiso 0.70 1 d PDU . . H66A H 1.1203 0.6690 0.5729 0.149 Uiso 0.70 1 calc PR . . H66B H 1.0554 0.6228 0.5550 0.149 Uiso 0.70 1 calc PR . . C67 C 0.980(3) 0.6865(14) 0.5547(6) 0.150 Uiso 0.70 1 d PDU . . H67A H 0.9236 0.6680 0.5413 0.180 Uiso 0.70 1 calc PR . . H67B H 1.0080 0.7077 0.5295 0.180 Uiso 0.70 1 calc PR . . C68 C 0.949(3) 0.7154(15) 0.5960(13) 0.155(8) Uiso 0.70 1 d PDU . . H68A H 0.9848 0.7470 0.5965 0.186 Uiso 0.70 1 calc PR . . H68B H 0.8771 0.7222 0.5943 0.186 Uiso 0.70 1 calc PR . . C45A C 0.859(4) 0.6001(19) 0.8133(12) 0.099(16) Uiso 0.35 1 d PD C 2 H45C H 0.8112 0.5882 0.8373 0.119 Uiso 0.35 1 calc PR C 2 H45D H 0.9000 0.6265 0.8274 0.119 Uiso 0.35 1 calc PR C 2 C46A C 0.926(5) 0.5565(19) 0.792(2) 0.119(19) Uiso 0.35 1 d PD C 2 H46C H 0.9571 0.5365 0.8178 0.143 Uiso 0.35 1 calc PR C 2 H46D H 0.9773 0.5681 0.7698 0.143 Uiso 0.35 1 calc PR C 2 C47A C 0.836(3) 0.5289(14) 0.7662(13) 0.066(9) Uiso 0.35 1 d PD C 2 H47C H 0.8595 0.5045 0.7427 0.079 Uiso 0.35 1 calc PR C 2 H47D H 0.7905 0.5132 0.7892 0.079 Uiso 0.35 1 calc PR C 2 C48A C 0.788(4) 0.5759(11) 0.7411(14) 0.084(12) Uiso 0.35 1 d PD C 2 H48C H 0.8153 0.5808 0.7087 0.101 Uiso 0.35 1 calc PR C 2 H48D H 0.7149 0.5723 0.7386 0.101 Uiso 0.35 1 calc PR C 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 Pd1 0.0256(3) 0.0458(3) 0.0317(3) -0.0001(2) 0.0084(2) 0.0035(2) Pd2 0.0263(3) 0.0356(3) 0.0373(3) 0.0023(2) 0.0026(2) 0.0074(2) Zn1 0.0245(4) 0.0353(5) 0.0301(4) 0.0053(3) 0.0020(3) 0.0040(3) Zn2 0.0263(4) 0.0318(4) 0.0294(4) -0.0029(3) 0.0032(3) -0.0015(3) Zn3 0.0263(4) 0.0389(5) 0.0243(4) -0.0020(3) -0.0022(3) 0.0034(3) Zn4 0.0260(4) 0.0361(5) 0.0258(4) 0.0046(3) 0.0028(3) 0.0036(3) Cl1 0.0394(12) 0.110(2) 0.0453(12) 0.0141(14) 0.0034(10) -0.0053(14) Cl2 0.0398(12) 0.117(2) 0.0412(12) -0.0165(14) 0.0035(9) 0.0056(14) Cl3 0.0350(11) 0.0431(12) 0.106(2) 0.0127(13) 0.0067(12) 0.0043(9) Cl4 0.0472(14) 0.0510(14) 0.117(3) -0.0014(15) 0.0260(15) 0.0040(11) O1 0.030(3) 0.053(3) 0.036(3) 0.012(2) 0.005(2) 0.010(2) O2 0.040(3) 0.050(3) 0.026(3) 0.008(2) 0.006(2) 0.006(3) O3 0.034(3) 0.060(4) 0.038(3) 0.011(3) 0.000(3) 0.018(3) O4 0.056(4) 0.069(5) 0.039(3) 0.019(3) 0.016(3) 0.035(4) O5 0.030(3) 0.042(3) 0.034(3) 0.013(2) 0.005(2) 0.008(2) O6 0.025(3) 0.054(3) 0.030(3) 0.015(2) 0.005(2) 0.001(2) O7 0.030(3) 0.042(3) 0.042(3) 0.011(2) 0.009(2) 0.004(2) O8 0.034(3) 0.042(3) 0.038(3) 0.020(2) 0.011(2) 0.008(2) O9 0.030(3) 0.049(3) 0.043(3) -0.023(3) 0.008(2) -0.006(2) O10 0.026(3) 0.091(5) 0.060(4) -0.037(4) 0.010(3) -0.014(3) O11 0.033(3) 0.036(3) 0.038(3) -0.004(2) 0.005(2) -0.004(2) O12 0.048(3) 0.031(3) 0.031(3) -0.003(2) 0.005(2) -0.006(2) O13 0.037(3) 0.043(3) 0.041(3) -0.010(3) -0.015(2) 0.003(3) O14 0.049(4) 0.057(4) 0.047(3) -0.020(3) -0.023(3) 0.022(3) O15 0.028(3) 0.051(4) 0.095(5) -0.031(4) -0.016(3) 0.005(3) O16 0.027(3) 0.033(3) 0.069(4) -0.019(3) -0.007(3) 0.007(2) O17 0.043(3) 0.064(4) 0.035(3) 0.002(3) 0.011(3) 0.018(3) O18 0.034(4) 0.092(6) 0.072(5) -0.001(4) 0.001(3) -0.014(4) O19 0.064(4) 0.066(4) 0.028(3) 0.002(3) 0.003(3) -0.008(3) O20 0.022(3) 0.056(4) 0.058(4) -0.002(3) 0.006(3) -0.001(2) O21 0.056(4) 0.050(4) 0.045(3) -0.003(3) -0.002(3) 0.019(3) O22 0.025(3) 0.084(5) 0.064(4) 0.004(4) 0.007(3) -0.002(3) O23 0.052(4) 0.054(4) 0.059(4) -0.013(3) 0.008(3) 0.002(3) O24 0.025(3) 0.064(4) 0.054(4) 0.010(3) -0.007(3) 0.005(3) O25 0.082(9) 0.28(3) 0.073(8) 0.040(12) -0.027(7) -0.017(12) O26 0.142(15) 0.134(14) 0.30(3) 0.036(15) 0.109(18) -0.019(12) O27 0.018(2) 0.039(3) 0.032(2) -0.007(2) 0.000(2) 0.001(2) O28 0.021(2) 0.038(3) 0.038(3) 0.000(2) 0.000(2) 0.001(2) O29 0.144(19) 0.140(17) 0.128(17) 0.040(14) -0.033(15) -0.047(15) O30 0.23(3) 0.151(17) 0.084(11) 0.024(11) 0.090(14) 0.112(18) N1 0.021(3) 0.045(4) 0.039(3) 0.004(3) 0.007(3) 0.007(3) N2 0.018(3) 0.048(4) 0.039(3) -0.004(3) 0.005(3) 0.003(3) N3 0.027(3) 0.035(4) 0.043(4) 0.000(3) 0.007(3) 0.009(3) N4 0.028(3) 0.046(4) 0.033(3) -0.007(3) -0.004(3) 0.005(3) C1 0.035(4) 0.036(4) 0.032(4) 0.008(3) 0.000(3) 0.000(3) C2 0.031(4) 0.033(4) 0.031(3) 0.002(3) -0.002(3) 0.002(3) C3 0.023(4) 0.046(5) 0.036(4) 0.007(3) 0.006(3) 0.004(3) C4 0.021(4) 0.054(5) 0.033(4) 0.005(3) 0.000(3) 0.008(3) C5 0.030(4) 0.046(5) 0.032(4) 0.010(3) 0.002(3) 0.013(3) C6 0.025(4) 0.043(4) 0.029(3) 0.001(3) -0.003(3) 0.005(3) C7 0.028(4) 0.047(5) 0.039(4) 0.005(3) 0.004(3) 0.012(3) C8 0.027(4) 0.036(4) 0.035(4) 0.005(3) 0.001(3) 0.007(3) C9 0.024(3) 0.033(4) 0.035(4) 0.004(3) 0.003(3) 0.002(3) C10 0.029(4) 0.033(4) 0.033(4) -0.004(3) 0.000(3) 0.003(3) C11 0.021(3) 0.042(4) 0.028(3) 0.006(3) 0.003(3) 0.000(3) C12 0.030(4) 0.038(4) 0.036(4) 0.005(3) 0.002(3) 0.005(3) C13 0.028(4) 0.035(4) 0.034(4) 0.006(3) -0.002(3) -0.003(3) C14 0.027(4) 0.044(4) 0.029(3) 0.003(3) 0.006(3) -0.003(3) C15 0.032(4) 0.039(4) 0.036(4) -0.006(3) 0.006(3) 0.002(3) C16 0.029(4) 0.032(4) 0.039(4) 0.000(3) 0.007(3) 0.004(3) C17 0.034(4) 0.038(4) 0.034(4) -0.002(3) 0.004(3) -0.002(3) C18 0.034(4) 0.037(4) 0.036(4) -0.004(3) 0.008(3) -0.003(3) C19 0.031(4) 0.050(5) 0.037(4) -0.008(3) 0.006(3) 0.000(3) C20 0.028(4) 0.059(5) 0.048(5) -0.015(4) 0.008(4) -0.010(4) C21 0.039(4) 0.029(4) 0.021(3) 0.001(3) 0.004(3) -0.001(3) C22 0.039(4) 0.033(4) 0.035(4) -0.011(3) -0.007(3) 0.007(3) C23 0.034(4) 0.041(4) 0.034(4) 0.001(3) -0.006(3) 0.002(3) C24 0.030(4) 0.042(4) 0.037(4) -0.009(3) -0.007(3) 0.008(3) C25 0.033(4) 0.036(4) 0.040(4) -0.008(3) -0.008(3) 0.007(3) C26 0.023(3) 0.040(4) 0.035(4) -0.005(3) -0.004(3) 0.008(3) C27 0.027(4) 0.057(5) 0.031(4) -0.010(3) -0.008(3) 0.004(3) C28 0.028(4) 0.043(5) 0.045(4) -0.014(4) -0.009(3) 0.007(3) C29 0.120(9) 0.109(9) 0.102(9) -0.005(7) -0.006(7) 0.042(8) C30 0.142(11) 0.142(11) 0.126(10) -0.020(8) 0.009(9) 0.021(9) C31 0.131(10) 0.130(10) 0.115(10) -0.017(8) -0.012(8) 0.016(8) C32 0.077(7) 0.092(7) 0.055(5) -0.009(5) 0.000(5) 0.015(6) C33 0.129(11) 0.152(12) 0.159(12) 0.011(9) -0.001(9) -0.004(9) C34 0.38(4) 0.38(4) 0.38(4) 0.001(10) -0.003(10) -0.002(10) C35 0.140(11) 0.135(11) 0.152(11) 0.006(9) 0.014(9) -0.046(9) C36 0.086(8) 0.094(8) 0.097(8) 0.011(7) -0.002(7) -0.032(7) C37 0.135(10) 0.125(9) 0.068(7) -0.013(7) 0.005(7) -0.006(8) C38 0.152(12) 0.153(11) 0.117(10) 0.004(8) 0.007(9) -0.005(9) C39 0.184(13) 0.156(13) 0.143(12) 0.020(9) -0.007(9) 0.008(9) C40 0.125(9) 0.105(8) 0.077(7) 0.033(6) 0.010(7) 0.008(7) C41 0.111(10) 0.141(11) 0.128(10) -0.009(8) -0.007(8) -0.011(8) C42 0.165(14) 0.177(14) 0.191(15) -0.003(9) -0.009(10) 0.003(9) C43 0.121(11) 0.161(12) 0.148(11) 0.013(9) 0.009(9) -0.002(9) C44 0.194(17) 0.222(18) 0.199(17) 0.010(10) -0.005(10) 0.001(10) C45 0.082(9) 0.089(9) 0.069(8) 0.013(7) 0.003(8) 0.014(8) C46 0.115(12) 0.103(11) 0.103(11) 0.021(9) -0.006(9) 0.017(9) C47 0.130(14) 0.126(14) 0.131(14) 0.001(9) -0.005(9) 0.008(9) C48 0.096(10) 0.083(9) 0.090(10) -0.007(8) 0.012(8) 0.028(8) C49 0.075(8) 0.051(7) 0.104(10) -0.010(6) 0.006(8) 0.001(6) C50 0.120(14) 0.073(9) 0.118(13) -0.035(9) -0.051(12) 0.029(10) C51 0.24(3) 0.14(2) 0.110(15) -0.078(15) 0.073(19) -0.03(2) C52 0.18(2) 0.084(11) 0.105(12) -0.034(10) 0.090(14) -0.024(12) C53 0.144(13) 0.145(13) 0.136(12) -0.002(9) -0.007(9) 0.006(9) C54 0.134(12) 0.137(12) 0.132(12) -0.006(9) -0.011(9) 0.001(9) C55 0.119(11) 0.127(11) 0.127(11) -0.007(9) -0.015(9) 0.014(9) C56 0.113(11) 0.130(11) 0.119(11) -0.005(8) -0.015(8) 0.003(9) C57 0.28(3) 0.28(3) 0.28(3) -0.003(10) -0.004(10) 0.006(10) C58 0.213(18) 0.217(18) 0.211(18) -0.010(10) -0.006(10) -0.011(10) C59 0.214(19) 0.229(19) 0.206(18) -0.002(10) -0.019(10) -0.006(10) C60 0.114(10) 0.119(10) 0.120(9) -0.003(8) -0.010(8) -0.002(8) C61 0.119(12) 0.138(12) 0.099(11) -0.020(9) -0.008(9) -0.002(9) C62 0.122(12) 0.116(12) 0.115(12) 0.029(9) 0.007(9) -0.006(9) C63 0.149(15) 0.140(15) 0.144(15) -0.003(9) -0.007(10) -0.011(10) C64 0.126(13) 0.140(14) 0.132(13) 0.014(9) -0.003(9) -0.016(9) _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 N1 2.019(6) 1_455 ? Pd1 N2 2.022(6) . ? Pd1 Cl2 2.291(3) . ? Pd1 Cl1 2.319(3) . ? Pd2 N4 2.035(7) 1_455 ? Pd2 N3 2.039(6) . ? Pd2 Cl4 2.286(3) . ? Pd2 Cl3 2.292(3) . ? Zn1 O5 2.029(5) . ? Zn1 O3 2.039(6) . ? Zn1 O11 2.068(6) . ? Zn1 O17 2.140(6) . ? Zn1 O27 2.154(5) . ? Zn1 O18 2.215(7) . ? Zn2 O12 2.025(5) . ? Zn2 O16 2.031(6) 3_467 ? Zn2 O6 2.046(5) . ? Zn2 O27 2.115(5) . ? Zn2 O20 2.134(6) . ? Zn2 O19 2.165(6) . ? Zn3 O2 2.009(5) 2_664 ? Zn3 O7 2.050(6) . ? Zn3 O13 2.054(5) . ? Zn3 O28 2.121(6) . ? Zn3 O21 2.140(7) . ? Zn3 O22 2.173(7) . ? Zn4 O8 2.028(5) . ? Zn4 O24 2.049(6) . ? Zn4 O9 2.054(5) 4_656 ? Zn4 O1 2.067(6) 2_664 ? Zn4 O28 2.118(5) . ? Zn4 O23 2.174(7) . ? O1 C6 1.253(10) . ? O1 Zn4 2.067(6) 2_665 ? O2 C6 1.251(10) . ? O2 Zn3 2.009(5) 2_665 ? O3 C7 1.233(10) . ? O4 C7 1.239(10) . ? O5 C13 1.234(10) . ? O6 C13 1.275(10) . ? O7 C14 1.266(10) . ? O8 C14 1.244(10) . ? O9 C20 1.255(11) . ? O9 Zn4 2.054(5) 4_646 ? O10 C20 1.251(11) . ? O11 C21 1.232(10) . ? O12 C21 1.258(9) . ? O13 C27 1.243(11) . ? O14 C27 1.239(11) . ? O15 C28 1.266(11) . ? O16 C28 1.247(10) . ? O16 Zn2 2.031(6) 3_567 ? O17 C29 1.416(18) . ? O17 C32 1.441(15) . ? O18 C36 1.430(19) . ? O18 C33 1.45(3) . ? O19 C37 1.426(13) . ? O19 C40 1.431(13) . ? O20 C44 1.41(2) . ? O20 C41 1.44(2) . ? O21 C45 1.393(16) . ? O21 C48A 1.40(2) . ? O21 C45A 1.40(2) . ? O21 C48 1.416(16) . ? O23 C52 1.426(12) . ? O23 C49 1.444(12) . ? O25 C53 1.43(2) . ? O25 C56 1.44(2) . ? O26 C57 1.42(2) . ? O26 C60 1.440(19) . ? O29 C61 1.23(4) . ? O29 C64 1.48(4) . ? O30 C65 1.33(3) . ? O30 C68 1.41(4) . ? N1 C1 1.338(10) . ? N1 C5 1.364(10) . ? N1 Pd1 2.019(6) 1_655 ? N2 C15 1.344(11) . ? N2 C19 1.381(11) . ? N3 C8 1.317(11) . ? N3 C12 1.344(11) . ? N4 C26 1.315(10) . ? N4 C22 1.341(11) . ? N4 Pd2 2.035(7) 1_655 ? C1 C2 1.383(12) . ? C2 C3 1.394(11) . ? C2 C6 1.510(11) . ? C3 C4 1.386(11) . ? C4 C5 1.392(11) . ? C4 C7 1.530(11) . ? C8 C9 1.404(10) . ? C9 C10 1.344(11) . ? C9 C13 1.514(11) . ? C10 C11 1.388(11) . ? C11 C12 1.396(11) . ? C11 C14 1.506(10) . ? C15 C16 1.377(11) . ? C16 C17 1.379(11) . ? C16 C21 1.517(11) . ? C17 C18 1.399(12) . ? C18 C19 1.374(12) . ? C18 C20 1.513(11) . ? C22 C23 1.404(12) . ? C23 C24 1.378(12) . ? C23 C27 1.517(11) . ? C24 C25 1.380(12) . ? C25 C26 1.393(11) . ? C25 C28 1.504(12) . ? C29 C30 1.59(3) . ? C30 C31 1.46(3) . ? C31 C32 1.47(2) . ? C33 C34 1.52(2) . ? C34 C35 1.49(2) . ? C35 C36 1.463(16) . ? C37 C38 1.48(2) . ? C38 C39 1.49(2) . ? C39 C40 1.51(2) . ? C41 C42 1.48(2) . ? C42 C43 1.46(2) . ? C43 C44 1.47(2) . ? C45 C46 1.473(19) . ? C46 C47 1.474(19) . ? C47 C48 1.49(2) . ? C49 C50 1.446(15) . ? C50 C51 1.445(17) . ? C51 C52 1.441(16) . ? C53 C54 1.46(2) . ? C54 C55 1.44(2) . ? C55 C56 1.44(2) . ? C57 C58 1.48(2) . ? C58 C59 1.46(2) . ? C59 C60 1.46(2) . ? C61 C62 1.65(5) . ? C62 C63 1.61(5) . ? C63 C64 1.01(4) . ? C65 C66 1.44(2) . ? C66 C67 1.42(2) . ? C67 C68 1.46(2) . ? C45A C46A 1.61(4) . ? C46A C47A 1.61(4) . ? C47A C48A 1.61(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 175.8(3) 1_455 . ? N1 Pd1 Cl2 91.2(2) 1_455 . ? N2 Pd1 Cl2 90.6(2) . . ? N1 Pd1 Cl1 88.6(2) 1_455 . ? N2 Pd1 Cl1 89.6(2) . . ? Cl2 Pd1 Cl1 178.70(14) . . ? N4 Pd2 N3 177.7(3) 1_455 . ? N4 Pd2 Cl4 88.7(2) 1_455 . ? N3 Pd2 Cl4 89.9(2) . . ? N4 Pd2 Cl3 90.9(2) 1_455 . ? N3 Pd2 Cl3 90.4(2) . . ? Cl4 Pd2 Cl3 179.00(13) . . ? O5 Zn1 O3 169.6(3) . . ? O5 Zn1 O11 95.8(2) . . ? O3 Zn1 O11 94.1(3) . . ? O5 Zn1 O17 87.9(2) . . ? O3 Zn1 O17 89.6(2) . . ? O11 Zn1 O17 86.8(3) . . ? O5 Zn1 O27 91.8(2) . . ? O3 Zn1 O27 90.5(2) . . ? O11 Zn1 O27 94.9(2) . . ? O17 Zn1 O27 178.3(3) . . ? O5 Zn1 O18 84.2(3) . . ? O3 Zn1 O18 85.7(3) . . ? O11 Zn1 O18 176.0(3) . . ? O17 Zn1 O18 89.2(3) . . ? O27 Zn1 O18 89.1(3) . . ? O12 Zn2 O16 173.6(3) . 3_467 ? O12 Zn2 O6 94.0(2) . . ? O16 Zn2 O6 92.2(3) 3_467 . ? O12 Zn2 O27 88.7(2) . . ? O16 Zn2 O27 92.6(2) 3_467 . ? O6 Zn2 O27 91.8(2) . . ? O12 Zn2 O20 89.7(3) . . ? O16 Zn2 O20 88.9(2) 3_467 . ? O6 Zn2 O20 89.2(2) . . ? O27 Zn2 O20 178.2(2) . . ? O12 Zn2 O19 87.1(2) . . ? O16 Zn2 O19 86.6(3) 3_467 . ? O6 Zn2 O19 175.4(3) . . ? O27 Zn2 O19 92.7(3) . . ? O20 Zn2 O19 86.4(3) . . ? O2 Zn3 O7 98.5(3) 2_664 . ? O2 Zn3 O13 167.2(3) 2_664 . ? O7 Zn3 O13 94.0(3) . . ? O2 Zn3 O28 91.1(2) 2_664 . ? O7 Zn3 O28 94.5(2) . . ? O13 Zn3 O28 90.6(2) . . ? O2 Zn3 O21 89.4(2) 2_664 . ? O7 Zn3 O21 86.7(3) . . ? O13 Zn3 O21 88.6(3) . . ? O28 Zn3 O21 178.6(3) . . ? O2 Zn3 O22 84.3(3) 2_664 . ? O7 Zn3 O22 174.1(3) . . ? O13 Zn3 O22 83.0(3) . . ? O28 Zn3 O22 90.6(3) . . ? O21 Zn3 O22 88.1(3) . . ? O8 Zn4 O24 88.7(3) . . ? O8 Zn4 O9 174.7(2) . 4_656 ? O24 Zn4 O9 88.7(2) . 4_656 ? O8 Zn4 O1 95.6(3) . 2_664 ? O24 Zn4 O1 94.8(3) . 2_664 ? O9 Zn4 O1 89.3(3) 4_656 2_664 ? O8 Zn4 O28 91.1(2) . . ? O24 Zn4 O28 175.3(3) . . ? O9 Zn4 O28 91.0(2) 4_656 . ? O1 Zn4 O28 89.8(2) 2_664 . ? O8 Zn4 O23 88.5(3) . . ? O24 Zn4 O23 89.5(3) . . ? O9 Zn4 O23 86.8(3) 4_656 . ? O1 Zn4 O23 174.1(3) 2_664 . ? O28 Zn4 O23 85.8(3) . . ? C6 O1 Zn4 135.8(5) . 2_665 ? C6 O2 Zn3 131.0(5) . 2_665 ? C7 O3 Zn1 127.8(6) . . ? C13 O5 Zn1 128.7(5) . . ? C13 O6 Zn2 133.9(5) . . ? C14 O7 Zn3 133.2(5) . . ? C14 O8 Zn4 135.6(5) . . ? C20 O9 Zn4 124.2(5) . 4_646 ? C21 O11 Zn1 132.6(5) . . ? C21 O12 Zn2 130.1(5) . . ? C27 O13 Zn3 126.8(5) . . ? C28 O16 Zn2 126.4(5) . 3_567 ? C29 O17 C32 107.3(11) . . ? C29 O17 Zn1 123.0(9) . . ? C32 O17 Zn1 119.9(6) . . ? C36 O18 C33 105.5(13) . . ? C36 O18 Zn1 123.7(8) . . ? C33 O18 Zn1 129.7(11) . . ? C37 O19 C40 108.2(12) . . ? C37 O19 Zn2 126.2(9) . . ? C40 O19 Zn2 124.6(8) . . ? C44 O20 C41 99.4(15) . . ? C44 O20 Zn2 124.7(11) . . ? C41 O20 Zn2 125.2(9) . . ? C45 O21 C48A 102(2) . . ? C45 O21 C45A 32(2) . . ? C48A O21 C45A 113(3) . . ? C45 O21 C48 107.8(14) . . ? C48A O21 C48 33(2) . . ? C45A O21 C48 100(2) . . ? C45 O21 Zn3 122.9(9) . . ? C48A O21 Zn3 120.0(18) . . ? C45A O21 Zn3 126(2) . . ? C48 O21 Zn3 128.8(9) . . ? C52 O23 C49 105.9(10) . . ? C52 O23 Zn4 126.2(8) . . ? C49 O23 Zn4 126.1(7) . . ? C53 O25 C56 107.7(19) . . ? C57 O26 C60 91(2) . . ? Zn2 O27 Zn1 113.5(2) . . ? Zn4 O28 Zn3 115.2(2) . . ? C61 O29 C64 106(3) . . ? C65 O30 C68 103(2) . . ? C1 N1 C5 118.3(7) . . ? C1 N1 Pd1 122.2(5) . 1_655 ? C5 N1 Pd1 119.2(5) . 1_655 ? C15 N2 C19 118.2(7) . . ? C15 N2 Pd1 119.1(5) . . ? C19 N2 Pd1 122.5(6) . . ? C8 N3 C12 120.2(7) . . ? C8 N3 Pd2 120.9(5) . . ? C12 N3 Pd2 119.0(5) . . ? C26 N4 C22 120.3(7) . . ? C26 N4 Pd2 120.8(5) . 1_655 ? C22 N4 Pd2 118.2(5) . 1_655 ? N1 C1 C2 123.3(7) . . ? C1 C2 C3 118.7(7) . . ? C1 C2 C6 120.1(7) . . ? C3 C2 C6 121.2(7) . . ? C4 C3 C2 118.6(7) . . ? C3 C4 C5 119.8(7) . . ? C3 C4 C7 121.8(7) . . ? C5 C4 C7 118.3(7) . . ? N1 C5 C4 121.2(7) . . ? O2 C6 O1 128.8(7) . . ? O2 C6 C2 115.9(7) . . ? O1 C6 C2 115.3(7) . . ? O3 C7 O4 127.6(8) . . ? O3 C7 C4 115.8(7) . . ? O4 C7 C4 116.6(7) . . ? N3 C8 C9 121.3(7) . . ? C10 C9 C8 119.1(7) . . ? C10 C9 C13 121.7(7) . . ? C8 C9 C13 119.1(7) . . ? C9 C10 C11 120.3(7) . . ? C10 C11 C12 118.0(7) . . ? C10 C11 C14 124.0(7) . . ? C12 C11 C14 118.0(7) . . ? N3 C12 C11 121.1(7) . . ? O5 C13 O6 127.6(7) . . ? O5 C13 C9 116.5(7) . . ? O6 C13 C9 115.9(7) . . ? O8 C14 O7 127.8(7) . . ? O8 C14 C11 116.6(7) . . ? O7 C14 C11 115.6(7) . . ? N2 C15 C16 122.8(7) . . ? C15 C16 C17 119.6(8) . . ? C15 C16 C21 117.7(7) . . ? C17 C16 C21 122.7(7) . . ? C16 C17 C18 118.2(8) . . ? C19 C18 C17 120.3(7) . . ? C19 C18 C20 118.6(8) . . ? C17 C18 C20 121.0(7) . . ? C18 C19 N2 120.8(8) . . ? O10 C20 O9 126.6(8) . . ? O10 C20 C18 116.4(7) . . ? O9 C20 C18 117.0(7) . . ? O11 C21 O12 128.0(7) . . ? O11 C21 C16 117.4(6) . . ? O12 C21 C16 114.6(7) . . ? N4 C22 C23 120.8(7) . . ? C24 C23 C22 118.8(7) . . ? C24 C23 C27 121.8(7) . . ? C22 C23 C27 118.9(7) . . ? C23 C24 C25 119.4(7) . . ? C24 C25 C26 118.6(7) . . ? C24 C25 C28 121.7(7) . . ? C26 C25 C28 119.4(7) . . ? N4 C26 C25 122.1(7) . . ? O14 C27 O13 128.5(7) . . ? O14 C27 C23 115.5(8) . . ? O13 C27 C23 115.9(7) . . ? O16 C28 O15 126.2(8) . . ? O16 C28 C25 117.1(7) . . ? O15 C28 C25 116.7(7) . . ? O17 C29 C30 106.9(16) . . ? C31 C30 C29 102.3(19) . . ? C30 C31 C32 106.6(19) . . ? O17 C32 C31 110.6(13) . . ? O18 C33 C34 102.4(16) . . ? C35 C34 C33 102.0(15) . . ? C36 C35 C34 105.7(10) . . ? O18 C36 C35 108.2(11) . . ? O19 C37 C38 108.5(16) . . ? C37 C38 C39 95.4(19) . . ? C38 C39 C40 107(2) . . ? O19 C40 C39 101.8(15) . . ? O20 C41 C42 111.5(15) . . ? C43 C42 C41 99.2(15) . . ? C42 C43 C44 98.2(14) . . ? O20 C44 C43 106.9(16) . . ? O21 C45 C46 109.6(13) . . ? C45 C46 C47 105.7(11) . . ? C46 C47 C48 105.1(12) . . ? O21 C48 C47 107.6(14) . . ? O23 C49 C50 106.9(12) . . ? C51 C50 C49 102.4(14) . . ? C52 C51 C50 105.2(15) . . ? O23 C52 C51 107.3(12) . . ? O25 C53 C54 101(2) . . ? C55 C54 C53 111(2) . . ? C56 C55 C54 100(2) . . ? C55 C56 O25 111(2) . . ? O26 C57 C58 118(2) . . ? C59 C58 C57 98.5(16) . . ? C60 C59 C58 99.3(16) . . ? O26 C60 C59 121(2) . . ? O29 C61 C62 98(2) . . ? C63 C62 C61 92(2) . . ? C64 C63 C62 112(4) . . ? C63 C64 O29 112(4) . . ? O30 C65 C66 114(2) . . ? C67 C66 C65 97.9(18) . . ? C66 C67 C68 105(2) . . ? O30 C68 C67 108(2) . . ? O21 C45A C46A 99(3) . . ? C45A C46A C47A 95(4) . . ? C48A C47A C46A 98(3) . . ? O21 C48A C47A 105(2) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.014 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.155