# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1550 data_hmc9813 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C148 H192 Cl8 N16 O24 Pd8' _chemical_formula_weight 3713.98 _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' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/nnc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 22.0685(8) _cell_length_b 22.0685(8) _cell_length_c 17.4908(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8518.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 6.45 _cell_measurement_theta_max 27.52 _exptl_crystal_description prisms _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method ? _exptl_crystal_F_000 3776 _exptl_absorpt_coefficient_mu 8.335 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1541 _exptl_absorpt_correction_T_max 0.2820 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4/RA' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6174 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 59.97 _reflns_number_total 3175 _reflns_number_observed 2107 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 309 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^)+(0.0617P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000054(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2866 _refine_ls_number_parameters 248 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_obs 0.0501 _refine_ls_wR_factor_all 0.1277 _refine_ls_wR_factor_obs 0.1080 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.131 _refine_ls_restrained_S_all 1.070 _refine_ls_restrained_S_obs 1.131 _refine_ls_shift/esd_max 0.060 _refine_ls_shift/esd_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.50362(2) 0.01566(2) 0.84340(3) 0.0302(2) Uani 1 d . . O1 O 0.4081(2) 0.0054(2) 0.8261(3) 0.0407(12) Uani 1 d . . C1 C 0.3774(3) 0.0030(3) 0.7671(4) 0.0345(14) Uani 1 d . . N2 N 0.3972(2) 0.0007(3) 0.6938(4) 0.0376(12) Uani 1 d . . C3 C 0.3474(3) -0.0004(4) 0.6447(4) 0.044(2) Uani 1 d . . O3 O 0.3491(2) -0.0013(4) 0.5755(3) 0.062(2) Uani 1 d . . C4 C 0.2911(3) 0.0010(3) 0.6936(4) 0.041(2) Uani 1 d . . C5 C 0.3097(3) 0.0014(3) 0.7666(4) 0.0355(14) Uani 1 d . . C6 C 0.2691(3) 0.0015(4) 0.8292(4) 0.0410(15) Uani 1 d . . H6A H 0.2818(3) 0.0019(4) 0.8811(4) 0.049 Uiso 1 calc R . C7 C 0.5887(3) 0.0223(3) 0.8745(5) 0.042(2) Uani 1 d . . C8 C 0.6327(4) 0.0638(4) 0.8517(6) 0.056(2) Uani 1 d . . H8A H 0.6223(4) 0.0943(4) 0.8156(6) 0.067 Uiso 1 calc R . C9 C 0.6910(4) 0.0618(5) 0.8800(8) 0.076(3) Uani 1 d . . H9A H 0.7206(4) 0.0900(5) 0.8630(8) 0.091 Uiso 1 calc R . C10 C 0.7061(4) 0.0175(6) 0.9342(8) 0.080(3) Uani 1 d . . H10A H 0.7460(4) 0.0162(6) 0.9543(8) 0.096 Uiso 1 calc R . C11 C 0.6639(4) -0.0239(5) 0.9588(7) 0.068(3) Uani 1 d . . H11A H 0.6743(4) -0.0536(5) 0.9958(7) 0.082 Uiso 1 calc R . C12 C 0.6056(3) -0.0215(4) 0.9285(5) 0.048(2) Uani 1 d . . C13 C 0.5568(3) -0.0640(3) 0.9540(5) 0.043(2) Uani 1 d . . H13A H 0.5365(3) -0.0478(3) 1.0002(5) 0.051 Uiso 1 calc R . H13B H 0.5744(3) -0.1040(3) 0.9667(5) 0.051 Uiso 1 calc R . N14 N 0.5117(2) -0.0705(2) 0.8904(4) 0.0366(12) Uani 1 d . . C15 C 0.4539(4) -0.0952(3) 0.9194(6) 0.052(2) Uani 1 d . . H15A H 0.4372(4) -0.0677(3) 0.9580(6) 0.078 Uiso 1 calc R . H15B H 0.4610(4) -0.1350(3) 0.9425(6) 0.078 Uiso 1 calc R . H15C H 0.4251(4) -0.0993(3) 0.8771(6) 0.078 Uiso 1 calc R . C16 C 0.5356(4) -0.1135(3) 0.8321(5) 0.054(2) Uani 1 d . . H16A H 0.5741(4) -0.0981(3) 0.8119(5) 0.081 Uiso 1 calc R . H16B H 0.5063(4) -0.1175(3) 0.7903(5) 0.081 Uiso 1 calc R . H16C H 0.5422(4) -0.1532(3) 0.8558(5) 0.081 Uiso 1 calc R . C17 C 0.2045(12) -0.1592(14) 0.5807(18) 0.101(8) Uiso 0.50 d PD . H17A H 0.1973(12) -0.1967(14) 0.5510(18) 0.121 Uiso 0.50 calc PR . H17B H 0.1817(12) -0.1255(14) 0.5567(18) 0.121 Uiso 0.50 calc PR . Cl1 Cl 0.1826(6) -0.1688(5) 0.6763(14) 0.230(10) Uani 0.50 d PD . Cl2 Cl 0.2794(6) -0.1429(6) 0.5849(10) 0.187(6) Uani 0.50 d PD . O18 O 0.6528(13) -0.1629(15) 0.3841(18) 0.188(11) Uani 0.65 d PU . C19 C 0.6676(18) -0.1607(16) 0.3014(20) 0.244(17) Uani 1 d U . C20 C 0.7155(11) -0.1371(10) 0.4306(22) 0.218(15) Uani 1 d U . C21 C 0.7717(15) -0.0933(17) 0.7182(18) 0.231(18) Uani 1 d U . O22 O 0.7618(32) -0.1304(31) 0.6658(47) 0.224(27) Uiso 0.35 d P . C23 C 0.7020(37) -0.1757(37) 0.6784(45) 0.236(34) Uiso 0.45 d P . C24 C 0.7263(29) -0.1501(29) 0.5750(41) 0.238(28) Uani 0.55 d PU . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0315(2) 0.0279(2) 0.0312(3) 0.0087(2) 0.0017(2) 0.00095(14) O1 0.033(2) 0.049(3) 0.040(3) 0.010(2) 0.007(2) 0.007(2) C1 0.036(3) 0.039(3) 0.029(4) 0.009(3) 0.001(3) 0.002(2) N2 0.031(2) 0.050(3) 0.032(3) 0.001(3) 0.005(2) -0.001(2) C3 0.037(3) 0.067(4) 0.027(4) 0.008(4) 0.010(3) 0.002(3) O3 0.038(3) 0.115(5) 0.032(4) 0.001(3) 0.007(2) 0.001(3) C4 0.030(3) 0.056(4) 0.037(4) 0.001(4) 0.008(3) -0.003(3) C5 0.030(3) 0.051(4) 0.026(4) 0.006(3) 0.002(2) -0.001(2) C6 0.032(3) 0.067(4) 0.024(4) -0.002(3) 0.003(2) -0.003(3) C7 0.037(3) 0.048(4) 0.042(5) 0.000(3) 0.006(3) 0.002(3) C8 0.046(4) 0.056(4) 0.066(6) 0.006(4) 0.003(4) -0.014(3) C9 0.043(5) 0.087(7) 0.096(9) -0.007(6) 0.009(5) -0.022(4) C10 0.047(5) 0.106(9) 0.086(9) -0.006(7) -0.013(5) -0.008(5) C11 0.045(4) 0.089(7) 0.070(7) 0.006(5) -0.016(4) 0.012(4) C12 0.044(4) 0.054(4) 0.045(5) -0.004(4) -0.012(3) 0.011(3) C13 0.051(4) 0.044(4) 0.032(4) 0.013(3) -0.007(3) 0.010(3) N14 0.039(3) 0.038(3) 0.033(3) 0.004(2) 0.002(2) 0.006(2) C15 0.059(5) 0.042(4) 0.055(6) 0.015(4) -0.001(4) -0.010(3) C16 0.080(5) 0.037(3) 0.046(6) 0.004(3) 0.006(4) 0.006(3) Cl1 0.168(11) 0.120(8) 0.403(32) -0.017(13) -0.047(15) 0.017(7) Cl2 0.155(10) 0.168(11) 0.237(18) -0.069(11) 0.021(10) 0.039(7) O18 0.167(20) 0.230(25) 0.168(22) -0.026(21) 0.012(18) 0.013(17) C19 0.257(30) 0.174(24) 0.301(37) -0.018(28) 0.012(30) -0.003(20) C20 0.137(18) 0.118(16) 0.397(47) 0.036(23) -0.046(24) 0.024(12) C21 0.218(30) 0.307(31) 0.169(28) 0.034(23) -0.084(22) 0.064(22) C24 0.224(39) 0.237(41) 0.254(44) 0.018(34) 0.078(33) 0.034(30) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C7 1.961(7) . ? Pd N2 2.033(5) 8_556 ? Pd N14 2.079(5) . ? Pd O1 2.143(4) . ? O1 C1 1.236(9) . ? C1 N2 1.354(9) . ? C1 C5 1.496(9) . ? N2 C3 1.395(9) . ? N2 Pd 2.033(5) 8_556 ? C3 O3 1.211(9) . ? C3 C4 1.509(9) . ? C4 C5 1.342(11) . ? C4 C6 1.387(10) 5_556 ? C5 C6 1.413(9) . ? C6 C4 1.387(10) 5_556 ? C7 C8 1.393(10) . ? C7 C12 1.403(11) . ? C8 C9 1.379(13) . ? C9 C10 1.40(2) . ? C10 C11 1.37(2) . ? C11 C12 1.391(11) . ? C12 C13 1.498(11) . ? C13 N14 1.499(10) . ? N14 C15 1.477(9) . ? N14 C16 1.489(10) . ? C17 Cl2 1.69(3) . ? C17 Cl1 1.75(3) . ? O18 C19 1.48(4) . ? O18 C20 1.70(4) . ? C19 C19 1.81(7) 8 ? C21 O22 1.25(8) . ? C21 C21 1.47(7) 5_656 ? O22 C23 1.67(9) . ? O22 C24 1.82(9) . ? C23 C24 1.97(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Pd N2 93.6(3) . 8_556 ? C7 Pd N14 82.9(3) . . ? N2 Pd N14 174.9(2) 8_556 . ? C7 Pd O1 171.8(3) . . ? N2 Pd O1 90.5(2) 8_556 . ? N14 Pd O1 92.5(2) . . ? C1 O1 Pd 131.3(4) . . ? O1 C1 N2 128.1(6) . . ? O1 C1 C5 123.5(6) . . ? N2 C1 C5 108.4(5) . . ? C1 N2 C3 109.3(5) . . ? C1 N2 Pd 127.6(5) . 8_556 ? C3 N2 Pd 123.1(5) . 8_556 ? O3 C3 N2 126.3(6) . . ? O3 C3 C4 126.2(6) . . ? N2 C3 C4 107.5(6) . . ? C5 C4 C6 124.5(6) . 5_556 ? C5 C4 C3 106.7(6) . . ? C6 C4 C3 128.9(7) 5_556 . ? C4 C5 C6 122.9(6) . . ? C4 C5 C1 108.1(6) . . ? C6 C5 C1 128.9(6) . . ? C4 C6 C5 112.6(6) 5_556 . ? C8 C7 C12 117.4(7) . . ? C8 C7 Pd 129.6(6) . . ? C12 C7 Pd 113.0(5) . . ? C9 C8 C7 121.7(9) . . ? C8 C9 C10 119.2(9) . . ? C11 C10 C9 121.0(9) . . ? C10 C11 C12 118.8(10) . . ? C11 C12 C7 121.9(8) . . ? C11 C12 C13 121.9(8) . . ? C7 C12 C13 116.1(6) . . ? C12 C13 N14 108.5(6) . . ? C15 N14 C16 107.9(6) . . ? C15 N14 C13 110.7(6) . . ? C16 N14 C13 109.5(6) . . ? C15 N14 Pd 113.5(4) . . ? C16 N14 Pd 110.1(5) . . ? C13 N14 Pd 105.2(4) . . ? Cl2 C17 Cl1 104.7(20) . . ? C19 O18 C20 106.0(28) . . ? O18 C19 C19 161.2(44) . 8 ? O22 C21 C21 116.2(50) . 5_656 ? C21 O22 C23 115.8(73) . . ? C21 O22 C24 150.6(63) . . ? C23 O22 C24 68.5(44) . . ? O22 C23 C24 59.5(43) . . ? O22 C24 C23 52.0(33) . . ? _refine_diff_density_max 0.599 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.124