# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1785 data_1a _audit_creation_method 'SHELXL and manual editing' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'Pd2 Co3 C28 O22 N4 H22' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H22 Co3 N4 O22 Pd2' _chemical_formula_weight 1156.09 _chemical_melting_point 'n/a' _chemical_compound_source 'Hydrothermal synthesis' 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' 'Co' 'Co' 0.3494 0.9721 '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' _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 6.500(1) _cell_length_b 7.957(4) _cell_length_c 16.507(2) _cell_angle_alpha 76.73(2) _cell_angle_beta 89.38(1) _cell_angle_gamma 85.06(2) _cell_volume 827.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.319 _exptl_crystal_density_method ? _exptl_crystal_F_000 567 _exptl_absorpt_coefficient_mu 2.643 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-axis IIc' _diffrn_measurement_method 'image plate oscillation photographs' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4959 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.54 _reflns_number_total 2698 _reflns_number_observed 2391 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MSC Raxis II control software' _computing_cell_refinement 'DENZO AND SCALEPACK (Otwinowski and Minor, 1985)' _computing_data_reduction 'SHELX97-SHELXPRO (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL+XP' _computing_publication_material 'SHELXTL+XCIF' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 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^)+(0.0579P)^2^+0.4256P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2689 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_obs 0.0365 _refine_ls_wR_factor_all 0.1584 _refine_ls_wR_factor_obs 0.0991 _refine_ls_goodness_of_fit_all 1.065 _refine_ls_goodness_of_fit_obs 1.107 _refine_ls_restrained_S_all 1.655 _refine_ls_restrained_S_obs 1.107 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.50612(5) 0.27489(4) 0.46182(2) 0.03148(15) Uani 1 d . . Co1 Co 0.01881(7) -0.17262(7) 0.97229(3) 0.0240(2) Uani 1 d . . Co2 Co 0.5000 0.0000 1.0000 0.0230(2) Uani 1 d S . O1 O 0.7401(5) 0.3307(5) 0.5235(2) 0.0452(8) Uani 1 d . . O2 O 0.8533(5) 0.3101(5) 0.6521(2) 0.0482(9) Uani 1 d . . O3 O 0.1251(4) -0.0674(4) 0.8547(2) 0.0324(6) Uani 1 d . . O4 O 0.4595(4) -0.0667(4) 0.8835(2) 0.0312(6) Uani 1 d . . O5 O 0.2758(5) 0.2233(4) 0.3940(2) 0.0392(7) Uani 1 d . . O6 O 0.1623(5) 0.2709(4) 0.2635(2) 0.0386(7) Uani 1 d . . O7 O 0.5699(4) 0.7361(3) 0.0590(2) 0.0289(6) Uani 1 d . . O8 O 0.9081(4) 0.6973(4) 0.0872(2) 0.0302(6) Uani 1 d . . O9 O -0.1854(4) -0.2962(4) 0.9052(2) 0.0295(6) Uani 1 d . . O10 O 0.2473(4) -0.3844(4) 0.9863(2) 0.0326(6) Uani 1 d . . O11 O 0.2011(4) -0.0366(3) 1.03472(15) 0.0250(5) Uani 1 d . . H11 H 0.2068(4) -0.1001(3) 1.09314(15) 0.030 Uiso 1 calc R . N1 N 0.4158(6) 0.1604(5) 0.5768(2) 0.0311(8) Uani 1 d . . N2 N 0.6032(6) 0.3925(5) 0.3504(2) 0.0307(8) Uani 1 d . . C1 C 0.5514(6) 0.1740(5) 0.6352(2) 0.0298(9) Uani 1 d . . C2 C 0.5253(6) 0.1030(5) 0.7178(2) 0.0302(8) Uani 1 d . . H2 H 0.6244(6) 0.1113(5) 0.7566(2) 0.036 Uiso 1 calc R . C3 C 0.3504(6) 0.0187(5) 0.7431(2) 0.0276(8) Uani 1 d . . C4 C 0.2088(6) 0.0061(6) 0.6822(2) 0.0321(9) Uani 1 d . . H4 H 0.0891(6) -0.0492(6) 0.6971(2) 0.038 Uiso 1 calc R . C5 C 0.2484(7) 0.0768(6) 0.5996(2) 0.0349(10) Uani 1 d . . H5 H 0.1558(7) 0.0657(6) 0.5590(2) 0.042 Uiso 1 calc R . C6 C 0.7327(6) 0.2781(6) 0.6035(3) 0.0356(10) Uani 1 d . . C7 C 0.3079(6) -0.0465(5) 0.8349(2) 0.0260(8) Uani 1 d . . C8 C 0.4703(6) 0.3944(5) 0.2883(2) 0.0289(8) Uani 1 d . . C9 C 0.5040(6) 0.4831(5) 0.2083(2) 0.0296(8) Uani 1 d . . H9 H 0.4082(6) 0.4865(5) 0.1664(2) 0.035 Uiso 1 calc R . C10 C 0.6830(6) 0.5676(5) 0.1906(2) 0.0273(8) Uani 1 d . . C11 C 0.8221(7) 0.5586(6) 0.2550(2) 0.0329(9) Uani 1 d . . H11 H 0.9459(7) 0.6098(6) 0.2444(2) 0.040 Uiso 1 calc R . C12 C 0.7759(6) 0.4736(6) 0.3345(2) 0.0341(10) Uani 1 d . . H12 H 0.8663(6) 0.4726(6) 0.3779(2) 0.041 Uiso 1 calc R . C13 C 0.2870(6) 0.2896(6) 0.3153(2) 0.0320(9) Uani 1 d . . C14 C 0.7255(6) 0.6739(5) 0.1049(2) 0.0255(8) 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 0.0340(2) 0.0413(2) 0.0192(2) -0.00360(14) 0.00075(14) -0.0121(2) Co1 0.0237(3) 0.0285(3) 0.0212(3) -0.0070(2) -0.0002(2) -0.0074(2) Co2 0.0216(4) 0.0283(4) 0.0196(3) -0.0051(3) -0.0017(3) -0.0061(3) O1 0.042(2) 0.067(2) 0.0260(15) -0.0019(15) 0.0011(14) -0.024(2) O2 0.044(2) 0.070(2) 0.031(2) -0.004(2) -0.0042(14) -0.032(2) O3 0.029(2) 0.047(2) 0.0216(13) -0.0075(12) 0.0006(11) -0.0081(12) O4 0.0288(15) 0.045(2) 0.0216(13) -0.0084(12) -0.0025(11) -0.0080(12) O5 0.042(2) 0.052(2) 0.0241(14) -0.0028(13) 0.0010(13) -0.0194(15) O6 0.039(2) 0.053(2) 0.0256(14) -0.0068(14) -0.0017(12) -0.0215(14) O7 0.0269(14) 0.0317(15) 0.0271(13) -0.0033(11) -0.0045(11) -0.0061(11) O8 0.0270(15) 0.041(2) 0.0224(13) -0.0028(12) -0.0003(11) -0.0103(12) O9 0.0291(14) 0.035(2) 0.0275(14) -0.0120(12) -0.0011(11) -0.0084(11) O10 0.0298(14) 0.033(2) 0.0366(15) -0.0111(12) -0.0008(11) -0.0029(11) O11 0.0245(13) 0.0311(14) 0.0205(12) -0.0063(11) -0.0019(10) -0.0063(11) N1 0.034(2) 0.039(2) 0.021(2) -0.0078(14) 0.0005(14) -0.0094(15) N2 0.034(2) 0.037(2) 0.022(2) -0.0049(14) 0.0016(14) -0.0082(15) C1 0.029(2) 0.038(2) 0.024(2) -0.008(2) 0.001(2) -0.009(2) C2 0.030(2) 0.038(2) 0.024(2) -0.007(2) -0.001(2) -0.009(2) C3 0.031(2) 0.029(2) 0.024(2) -0.007(2) -0.001(2) -0.007(2) C4 0.031(2) 0.044(2) 0.024(2) -0.008(2) 0.000(2) -0.014(2) C5 0.035(2) 0.048(3) 0.023(2) -0.007(2) -0.004(2) -0.015(2) C6 0.032(2) 0.045(3) 0.029(2) -0.004(2) 0.001(2) -0.014(2) C7 0.029(2) 0.028(2) 0.024(2) -0.010(2) -0.002(2) -0.005(2) C8 0.031(2) 0.032(2) 0.025(2) -0.007(2) 0.001(2) -0.010(2) C9 0.029(2) 0.036(2) 0.025(2) -0.008(2) 0.000(2) -0.011(2) C10 0.029(2) 0.030(2) 0.023(2) -0.006(2) -0.002(2) -0.005(2) C11 0.030(2) 0.043(2) 0.025(2) -0.004(2) -0.002(2) -0.011(2) C12 0.029(2) 0.050(3) 0.024(2) -0.007(2) -0.004(2) -0.012(2) C13 0.031(2) 0.037(2) 0.029(2) -0.007(2) 0.005(2) -0.009(2) C14 0.028(2) 0.029(2) 0.023(2) -0.010(2) 0.001(2) -0.0073(15) _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 O1 1.976(3) . ? Pd1 N2 1.986(3) . ? Pd1 O5 2.004(3) . ? Pd1 N1 2.013(3) . ? Co1 O3 2.067(3) . ? Co1 O11 2.082(3) 2_557 ? Co1 O8 2.094(3) 1_446 ? Co1 O11 2.097(2) . ? Co1 O10 2.120(3) . ? Co1 O9 2.171(2) . ? Co2 O11 2.045(2) . ? Co2 O11 2.045(2) 2_657 ? Co2 O7 2.115(3) 2_666 ? Co2 O7 2.115(3) 1_546 ? Co2 O4 2.134(2) 2_657 ? Co2 O4 2.134(2) . ? O1 C6 1.291(5) . ? O2 C6 1.210(5) . ? O3 C7 1.244(5) . ? O4 C7 1.254(4) . ? O5 C13 1.288(5) . ? O6 C13 1.227(5) . ? O7 C14 1.265(5) . ? O7 Co2 2.115(3) 1_564 ? O8 C14 1.239(5) . ? O8 Co1 2.093(3) 1_664 ? O11 Co1 2.082(3) 2_557 ? N1 C5 1.330(5) . ? N1 C1 1.342(5) . ? N2 C12 1.337(5) . ? N2 C8 1.344(5) . ? C1 C2 1.365(5) . ? C1 C6 1.518(6) . ? C2 C3 1.382(6) . ? C3 C4 1.397(5) . ? C3 C7 1.514(5) . ? C4 C5 1.381(6) . ? C8 C9 1.373(5) . ? C8 C13 1.518(5) . ? C9 C10 1.388(5) . ? C10 C11 1.389(6) . ? C10 C14 1.508(5) . ? C11 C12 1.374(6) . ? 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 O1 Pd1 N2 95.01(13) . . ? O1 Pd1 O5 177.16(11) . . ? N2 Pd1 O5 82.17(13) . . ? O1 Pd1 N1 82.79(13) . . ? N2 Pd1 N1 177.74(12) . . ? O5 Pd1 N1 100.03(13) . . ? O3 Co1 O11 91.45(11) . 2_557 ? O3 Co1 O8 174.05(11) . 1_446 ? O11 Co1 O8 92.19(11) 2_557 1_446 ? O3 Co1 O11 95.67(10) . . ? O11 Co1 O11 85.11(10) 2_557 . ? O8 Co1 O11 89.33(10) 1_446 . ? O3 Co1 O10 90.79(12) . . ? O11 Co1 O10 176.75(10) 2_557 . ? O8 Co1 O10 85.78(11) 1_446 . ? O11 Co1 O10 92.32(11) . . ? O3 Co1 O9 83.57(11) . . ? O11 Co1 O9 90.74(10) 2_557 . ? O8 Co1 O9 91.67(10) 1_446 . ? O11 Co1 O9 175.77(10) . . ? O10 Co1 O9 91.85(11) . . ? O11 Co2 O11 180.000(2) . 2_657 ? O11 Co2 O7 93.56(11) . 2_666 ? O11 Co2 O7 86.44(11) 2_657 2_666 ? O11 Co2 O7 86.44(11) . 1_546 ? O11 Co2 O7 93.56(11) 2_657 1_546 ? O7 Co2 O7 180.000(1) 2_666 1_546 ? O11 Co2 O4 86.80(10) . 2_657 ? O11 Co2 O4 93.20(10) 2_657 2_657 ? O7 Co2 O4 90.68(11) 2_666 2_657 ? O7 Co2 O4 89.32(11) 1_546 2_657 ? O11 Co2 O4 93.20(10) . . ? O11 Co2 O4 86.80(10) 2_657 . ? O7 Co2 O4 89.32(11) 2_666 . ? O7 Co2 O4 90.68(11) 1_546 . ? O4 Co2 O4 180.000(1) 2_657 . ? C6 O1 Pd1 115.2(3) . . ? C7 O3 Co1 126.4(3) . . ? C7 O4 Co2 132.5(3) . . ? C13 O5 Pd1 114.4(3) . . ? C14 O7 Co2 126.0(2) . 1_564 ? C14 O8 Co1 126.5(2) . 1_664 ? Co2 O11 Co1 121.15(13) . 2_557 ? Co2 O11 Co1 120.53(12) . . ? Co1 O11 Co1 94.89(10) 2_557 . ? C5 N1 C1 119.3(3) . . ? C5 N1 Pd1 129.0(3) . . ? C1 N1 Pd1 111.7(3) . . ? C12 N2 C8 120.1(3) . . ? C12 N2 Pd1 126.2(3) . . ? C8 N2 Pd1 113.6(3) . . ? N1 C1 C2 122.3(4) . . ? N1 C1 C6 115.4(3) . . ? C2 C1 C6 122.3(3) . . ? C1 C2 C3 119.4(4) . . ? C2 C3 C4 118.1(4) . . ? C2 C3 C7 120.4(3) . . ? C4 C3 C7 121.3(4) . . ? C5 C4 C3 119.3(4) . . ? N1 C5 C4 121.6(4) . . ? O2 C6 O1 125.0(4) . . ? O2 C6 C1 120.1(4) . . ? O1 C6 C1 114.8(3) . . ? O3 C7 O4 126.6(4) . . ? O3 C7 C3 116.8(3) . . ? O4 C7 C3 116.6(4) . . ? N2 C8 C9 121.5(4) . . ? N2 C8 C13 113.9(3) . . ? C9 C8 C13 124.6(3) . . ? C8 C9 C10 119.2(3) . . ? C9 C10 C11 118.4(4) . . ? C9 C10 C14 122.0(3) . . ? C11 C10 C14 119.5(4) . . ? C12 C11 C10 119.7(4) . . ? N2 C12 C11 121.1(4) . . ? O6 C13 O5 124.1(4) . . ? O6 C13 C8 120.2(3) . . ? O5 C13 C8 115.6(3) . . ? O8 C14 O7 126.2(4) . . ? O8 C14 C10 117.2(3) . . ? O7 C14 C10 116.6(3) . . ? _refine_diff_density_max 0.670 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.110 #===END data_3a _audit_creation_method 'SHELXL and manual editing' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'Pd2 Zn3 C28 H22 N4 O22' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H22 N4 O22 Pd2 Zn3' _chemical_formula_weight 1175.41 _chemical_melting_point 'n/a' _chemical_compound_source 'Hydrothermal synthesis' 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' _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 6.529(1) _cell_length_b 8.124(2) _cell_length_c 16.719(3) _cell_angle_alpha 75.94(3) _cell_angle_beta 88.73(3) _cell_angle_gamma 84.78(3) _cell_volume 856.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yelow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.278 _exptl_crystal_density_method ? _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 3.202 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-axis IIc' _diffrn_measurement_method 'image plate oscillation photographs' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5386 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0864 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2862 _reflns_number_observed 2165 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MSC Raxis II control software' _computing_cell_refinement 'DENZO AND SCALEPACK (Otwinowski and Minor, 1985)' _computing_data_reduction 'SHELX97-SHELXPRO (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL+XP' _computing_publication_material 'SHELXTL+XCIF' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 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^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2858 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_obs 0.0412 _refine_ls_wR_factor_all 0.1348 _refine_ls_wR_factor_obs 0.1000 _refine_ls_goodness_of_fit_all 0.976 _refine_ls_goodness_of_fit_obs 1.061 _refine_ls_restrained_S_all 1.225 _refine_ls_restrained_S_obs 1.061 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.49350(7) 0.72472(6) 0.03825(3) 0.0343(2) Uani 1 d . . Zn1 Zn 0.97891(9) 1.17211(8) -0.47230(4) 0.0284(2) Uani 1 d . . Zn2 Zn 0.5000 1.0000 -0.5000 0.0280(2) Uani 1 d S . N1 N 0.5830(7) 0.8396(6) -0.0764(3) 0.0332(11) Uani 1 d . . N2 N 0.3976(7) 0.6054(6) 0.1489(3) 0.0304(11) Uani 1 d . . O1 O 0.2584(6) 0.6709(6) -0.0229(3) 0.0480(12) Uani 1 d . . O2 O 0.1487(7) 0.6882(6) -0.1519(3) 0.0502(12) Uani 1 d . . O3 O 0.8761(6) 1.0702(5) -0.3535(2) 0.0360(10) Uani 1 d . . O4 O 0.5394(5) 1.0687(5) -0.3826(2) 0.0320(9) Uani 1 d . . O5 O 0.7251(6) 0.7753(6) 0.1054(2) 0.0411(11) Uani 1 d . . O6 O 0.8371(6) 0.7283(6) 0.2360(3) 0.0413(11) Uani 1 d . . O7 O 0.4304(6) 0.2648(5) 0.4406(2) 0.0341(10) Uani 1 d . . O8 O 0.0904(6) 0.3043(5) 0.4137(2) 0.0331(9) Uani 1 d . . O9 O 1.1846(6) 1.2979(5) -0.4053(2) 0.0333(9) Uani 1 d . . O10 O 0.7510(6) 1.3848(5) -0.4861(2) 0.0354(9) Uani 1 d . . O11 O 0.7971(5) 1.0340(4) -0.5340(2) 0.0271(8) Uani 1 d . . H11 H 0.7921(5) 1.0973(4) -0.5920(2) 0.032 Uiso 1 calc R . C1 C 0.4481(9) 0.8274(7) -0.1345(4) 0.0330(13) Uani 1 d . . C2 C 0.4744(8) 0.8969(7) -0.2181(3) 0.0312(13) Uani 1 d . . H2 H 0.3781(8) 0.8873(7) -0.2566(3) 0.037 Uiso 1 calc R . C3 C 0.6502(8) 0.9815(7) -0.2425(3) 0.0313(13) Uani 1 d . . C4 C 0.7903(9) 0.9953(8) -0.1816(4) 0.0344(14) Uani 1 d . . H4 H 0.9079(9) 1.0520(8) -0.1968(4) 0.041 Uiso 1 calc R . C5 C 0.7515(9) 0.9241(8) -0.0991(4) 0.0372(15) Uani 1 d . . H5 H 0.8426(9) 0.9348(8) -0.0590(4) 0.045 Uiso 1 calc R . C6 C 0.2689(9) 0.7213(8) -0.1040(4) 0.0365(15) Uani 1 d . . C7 C 0.6931(8) 1.0467(7) -0.3340(3) 0.0275(12) Uani 1 d . . C8 C 0.5320(8) 0.6037(7) 0.2111(3) 0.0309(13) Uani 1 d . . C9 C 0.4963(8) 0.5167(7) 0.2916(3) 0.0306(13) Uani 1 d . . H9 H 0.5894(8) 0.5145(7) 0.3333(3) 0.037 Uiso 1 calc R . C10 C 0.3154(8) 0.4316(7) 0.3090(3) 0.0287(13) Uani 1 d . . C11 C 0.1785(9) 0.4394(7) 0.2450(3) 0.0325(14) Uani 1 d . . H11 H 0.0563(9) 0.3876(7) 0.2560(3) 0.039 Uiso 1 calc R . C12 C 0.2243(9) 0.5240(8) 0.1652(4) 0.0359(15) Uani 1 d . . H12 H 0.1351(9) 0.5248(8) 0.1224(4) 0.043 Uiso 1 calc R . C13 C 0.7160(9) 0.7100(7) 0.1849(4) 0.0345(14) Uani 1 d . . C14 C 0.2736(8) 0.3268(7) 0.3947(3) 0.0274(12) 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 0.0380(3) 0.0400(3) 0.0229(3) -0.0016(2) 0.0029(2) -0.0106(2) Zn1 0.0296(4) 0.0282(4) 0.0270(4) -0.0053(3) 0.0028(3) -0.0052(3) Zn2 0.0268(5) 0.0287(5) 0.0273(5) -0.0038(4) 0.0008(4) -0.0041(4) N1 0.030(3) 0.039(3) 0.029(3) -0.004(2) 0.001(2) -0.006(2) N2 0.029(3) 0.036(3) 0.025(3) -0.004(2) -0.001(2) -0.003(2) O1 0.044(3) 0.065(3) 0.031(3) 0.004(2) 0.002(2) -0.023(2) O2 0.045(3) 0.070(3) 0.036(3) -0.005(2) -0.005(2) -0.025(2) O3 0.032(2) 0.046(3) 0.028(2) -0.004(2) 0.002(2) -0.005(2) O4 0.027(2) 0.044(3) 0.026(2) -0.008(2) 0.002(2) -0.005(2) O5 0.040(2) 0.051(3) 0.030(2) 0.000(2) 0.005(2) -0.016(2) O6 0.043(3) 0.051(3) 0.031(2) -0.006(2) -0.003(2) -0.018(2) O7 0.034(2) 0.028(2) 0.035(2) 0.004(2) 0.000(2) -0.003(2) O8 0.031(2) 0.038(2) 0.028(2) -0.002(2) 0.002(2) -0.008(2) O9 0.037(2) 0.034(2) 0.030(2) -0.009(2) 0.002(2) -0.008(2) O10 0.040(2) 0.027(2) 0.038(2) -0.008(2) 0.003(2) -0.001(2) O11 0.030(2) 0.029(2) 0.023(2) -0.004(2) -0.0010(15) -0.006(2) C1 0.029(3) 0.038(4) 0.030(3) -0.005(3) 0.004(2) -0.004(2) C2 0.030(3) 0.041(4) 0.022(3) -0.006(2) 0.003(2) -0.003(2) C3 0.030(3) 0.037(4) 0.026(3) -0.006(3) 0.002(2) -0.002(2) C4 0.031(3) 0.039(4) 0.033(3) -0.007(3) -0.001(2) -0.008(2) C5 0.040(4) 0.045(4) 0.024(3) -0.001(3) 0.001(2) -0.011(3) C6 0.037(4) 0.036(4) 0.033(4) -0.001(3) 0.000(3) -0.008(3) C7 0.029(3) 0.029(3) 0.025(3) -0.007(2) 0.002(2) -0.003(2) C8 0.035(3) 0.030(3) 0.028(3) -0.004(2) 0.004(2) -0.004(2) C9 0.028(3) 0.033(3) 0.029(3) -0.004(2) 0.000(2) -0.008(2) C10 0.035(3) 0.029(3) 0.021(3) -0.004(2) 0.002(2) -0.004(2) C11 0.031(3) 0.036(3) 0.030(3) -0.005(3) 0.000(2) -0.010(2) C12 0.030(3) 0.049(4) 0.026(3) 0.000(3) -0.004(2) -0.011(3) C13 0.042(4) 0.030(3) 0.031(4) -0.004(3) 0.007(3) -0.006(3) C14 0.033(3) 0.025(3) 0.024(3) -0.005(2) 0.001(2) -0.003(2) _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 N2 1.986(4) . ? Pd1 O1 2.000(4) . ? Pd1 N1 2.017(5) . ? Pd1 O5 2.032(4) . ? Zn1 O3 2.080(4) . ? Zn1 O8 2.098(4) 1_664 ? Zn1 O11 2.105(4) 2_774 ? Zn1 O11 2.142(4) . ? Zn1 O10 2.146(4) . ? Zn1 O9 2.231(4) . ? Zn1 Zn1 3.140(2) 2_774 ? Zn2 O11 2.033(3) 2_674 ? Zn2 O11 2.033(3) . ? Zn2 O7 2.150(4) 1_564 ? Zn2 O7 2.150(4) 2_665 ? Zn2 O4 2.193(4) . ? Zn2 O4 2.193(4) 2_674 ? N1 C5 1.348(7) . ? N1 C1 1.352(8) . ? N2 C12 1.352(7) . ? N2 C8 1.371(7) . ? O1 C6 1.320(7) . ? O2 C6 1.225(7) . ? O3 C7 1.251(6) . ? O4 C7 1.278(7) . ? O5 C13 1.308(7) . ? O6 C13 1.221(7) . ? O7 C14 1.283(6) . ? O7 Zn2 2.150(4) 1_546 ? O8 C14 1.249(6) . ? O8 Zn1 2.098(4) 1_446 ? O11 Zn1 2.105(4) 2_774 ? C1 C2 1.388(7) . ? C1 C6 1.521(7) . ? C2 C3 1.394(7) . ? C3 C4 1.415(8) . ? C3 C7 1.521(7) . ? C4 C5 1.387(8) . ? C8 C9 1.386(7) . ? C8 C13 1.538(8) . ? C9 C10 1.412(7) . ? C10 C11 1.395(8) . ? C10 C14 1.511(7) . ? C11 C12 1.385(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 O1 95.1(2) . . ? N2 Pd1 N1 177.4(2) . . ? O1 Pd1 N1 82.5(2) . . ? N2 Pd1 O5 82.3(2) . . ? O1 Pd1 O5 177.29(15) . . ? N1 Pd1 O5 100.1(2) . . ? O3 Zn1 O8 172.1(2) . 1_664 ? O3 Zn1 O11 92.1(2) . 2_774 ? O8 Zn1 O11 92.07(15) 1_664 2_774 ? O3 Zn1 O11 96.91(15) . . ? O8 Zn1 O11 90.14(15) 1_664 . ? O11 Zn1 O11 84.64(14) 2_774 . ? O3 Zn1 O10 90.8(2) . . ? O8 Zn1 O10 85.18(15) 1_664 . ? O11 Zn1 O10 176.81(15) 2_774 . ? O11 Zn1 O10 93.74(15) . . ? O3 Zn1 O9 82.2(2) . . ? O8 Zn1 O9 90.98(15) 1_664 . ? O11 Zn1 O9 91.08(14) 2_774 . ? O11 Zn1 O9 175.61(14) . . ? O10 Zn1 O9 90.58(15) . . ? O3 Zn1 Zn1 96.12(13) . 2_774 ? O8 Zn1 Zn1 91.48(12) 1_664 2_774 ? O11 Zn1 Zn1 42.78(10) 2_774 2_774 ? O11 Zn1 Zn1 41.86(10) . 2_774 ? O10 Zn1 Zn1 135.53(11) . 2_774 ? O9 Zn1 Zn1 133.85(11) . 2_774 ? O11 Zn2 O11 180.0 2_674 . ? O11 Zn2 O7 93.21(14) 2_674 1_564 ? O11 Zn2 O7 86.79(14) . 1_564 ? O11 Zn2 O7 86.79(14) 2_674 2_665 ? O11 Zn2 O7 93.21(14) . 2_665 ? O7 Zn2 O7 180.0 1_564 2_665 ? O11 Zn2 O4 87.15(14) 2_674 . ? O11 Zn2 O4 92.86(14) . . ? O7 Zn2 O4 89.7(2) 1_564 . ? O7 Zn2 O4 90.3(2) 2_665 . ? O11 Zn2 O4 92.86(14) 2_674 2_674 ? O11 Zn2 O4 87.14(14) . 2_674 ? O7 Zn2 O4 90.3(2) 1_564 2_674 ? O7 Zn2 O4 89.7(2) 2_665 2_674 ? O4 Zn2 O4 180.0 . 2_674 ? C5 N1 C1 119.7(5) . . ? C5 N1 Pd1 128.2(4) . . ? C1 N1 Pd1 112.1(4) . . ? C12 N2 C8 120.5(5) . . ? C12 N2 Pd1 126.0(4) . . ? C8 N2 Pd1 113.4(3) . . ? C6 O1 Pd1 115.3(3) . . ? C7 O3 Zn1 125.1(4) . . ? C7 O4 Zn2 132.0(4) . . ? C13 O5 Pd1 115.4(3) . . ? C14 O7 Zn2 125.4(4) . 1_546 ? C14 O8 Zn1 127.1(3) . 1_446 ? Zn2 O11 Zn1 122.2(2) . 2_774 ? Zn2 O11 Zn1 120.3(2) . . ? Zn1 O11 Zn1 95.36(14) 2_774 . ? N1 C1 C2 123.2(5) . . ? N1 C1 C6 116.1(5) . . ? C2 C1 C6 120.5(5) . . ? C1 C2 C3 117.6(5) . . ? C2 C3 C4 119.1(5) . . ? C2 C3 C7 119.1(5) . . ? C4 C3 C7 121.7(5) . . ? C5 C4 C3 119.7(5) . . ? N1 C5 C4 120.6(5) . . ? O2 C6 O1 124.8(5) . . ? O2 C6 C1 121.6(5) . . ? O1 C6 C1 113.6(5) . . ? O3 C7 O4 127.1(5) . . ? O3 C7 C3 116.3(5) . . ? O4 C7 C3 116.6(4) . . ? N2 C8 C9 121.3(5) . . ? N2 C8 C13 115.1(5) . . ? C9 C8 C13 123.6(5) . . ? C8 C9 C10 118.4(5) . . ? C11 C10 C9 119.1(5) . . ? C11 C10 C14 120.0(5) . . ? C9 C10 C14 120.9(5) . . ? C12 C11 C10 120.2(5) . . ? N2 C12 C11 120.4(5) . . ? O6 C13 O5 125.7(5) . . ? O6 C13 C8 120.8(5) . . ? O5 C13 C8 113.5(5) . . ? O8 C14 O7 125.7(5) . . ? O8 C14 C10 117.3(5) . . ? O7 C14 C10 116.9(5) . . ? _refine_diff_density_max 0.733 _refine_diff_density_min -1.174 _refine_diff_density_rms 0.150 #===END