Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_nkb _database_code_CSD 189781 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Fujita, Makoto' 'Biradha, Kumar' 'Chand, Dillip K.' 'Sakamoto, Shigeru' 'Yamaguchi, Kentaro' _publ_contact_author_name 'Prof Makoto Fujita' _publ_contact_author_address ; Department of Applied Chemistry Nagoya University and CREST Graduate School of Engineering Japan Science and Technology Corpor Chikusaku Nagoya 464-8603 JAPAN ; _publ_contact_author_email 'MFUJITA@APPCHEM.T.U-TOKYO.AC.JP' _publ_requested_journal 'Chemical Communications' _publ_section_title ; A molecular sphere ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C192 H168 N36 O36 Pd6' _chemical_formula_weight 4194.13 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' 'Pd' 'Pd' -0.9988 1.0072 '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(2)/nnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'y, x, -z' '-y+1/2, -x+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-y, -x, z' 'y-1/2, x-1/2, z' _cell_length_a 34.312(4) _cell_length_b 34.312(4) _cell_length_c 29.063(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 34217(7) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7800 _exptl_absorpt_coefficient_mu 0.347 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9339 _exptl_absorpt_correction_T_max 0.9339 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 89663 _diffrn_reflns_av_R_equivalents 0.1662 _diffrn_reflns_av_sigmaI/netI 0.1029 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11580 _reflns_number_gt 4117 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11580 _refine_ls_number_parameters 592 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2748 _refine_ls_R_factor_gt 0.1203 _refine_ls_wR_factor_ref 0.3134 _refine_ls_wR_factor_gt 0.2800 _refine_ls_goodness_of_fit_ref 1.397 _refine_ls_restrained_S_all 1.397 _refine_ls_shift/su_max 0.099 _refine_ls_shift/su_mean 0.010 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 0.16283(6) 0.83717(6) 0.01551(10) 0.0625(5) Uani 1 2 d S . . Pd2 Pd -0.00993(2) 1.00993(2) 0.24338(5) 0.0646(5) Uani 1 2 d S . . Pd3 Pd 0.16205(7) 1.16205(7) 0.0000 0.0659(11) Uani 1 2 d S . . C11 C 0.2149(2) 0.9926(5) -0.2080(3) 0.111(8) Uani 1 1 d G . . C12 C 0.2272(4) 1.0279(4) -0.1896(5) 0.102(8) Uani 1 1 d G . . H12 H 0.2183 1.0517 -0.2024 0.123 Uiso 1 1 calc R . . C13 C 0.2526(4) 1.0283(3) -0.1523(5) 0.101(7) Uani 1 1 d G . . C14 C 0.2657(2) 0.9934(5) -0.1334(3) 0.099(6) Uani 1 1 d G . . H14 H 0.2830 0.9937 -0.1080 0.118 Uiso 1 1 calc R . . C15 C 0.2534(4) 0.9581(3) -0.1519(5) 0.098(5) Uiso 1 1 d G . . C16 C 0.2280(3) 0.9577(4) -0.1892(5) 0.090(7) Uani 1 1 d G . . H16 H 0.2196 0.9336 -0.2018 0.108 Uiso 1 1 calc R . . N11A N 0.06792(14) 0.9893(2) -0.2425(3) 0.061(3) Uani 1 1 d G . . C11A C 0.0871(2) 0.9885(4) -0.2846(3) 0.103(6) Uani 1 1 d G . . H11A H 0.0726 0.9872 -0.3124 0.124 Uiso 1 1 calc R . . C12A C 0.1276(2) 0.9895(5) -0.2860(2) 0.124(9) Uani 1 1 d G . . H12A H 0.1408 0.9889 -0.3148 0.149 Uiso 1 1 calc R . . C13A C 0.14887(14) 0.9914(5) -0.2454(3) 0.127(8) Uani 1 1 d G . . C14A C 0.1297(2) 0.9922(4) -0.2033(2) 0.089(5) Uani 1 1 d G . . H14A H 0.1442 0.9935 -0.1755 0.106 Uiso 1 1 calc R . . C15A C 0.0892(2) 0.9912(3) -0.2018(3) 0.068(4) Uani 1 1 d G . . H15A H 0.0760 0.9918 -0.1731 0.082 Uiso 1 1 calc R . . C16A C 0.1926(3) 0.9920(13) -0.2525(5) 0.195(14) Uani 1 1 d . . . H16A H 0.2003 0.9687 -0.2704 0.234 Uiso 1 1 calc . . . H16B H 0.1996 1.0153 -0.2708 0.234 Uiso 1 1 calc . . . N21A N 0.1943(3) 1.1301(3) -0.0426(3) 0.062(4) Uani 1 1 d G . . C21A C 0.2280(4) 1.1472(3) -0.0597(4) 0.089(6) Uani 1 1 d G . . H21A H 0.2350 1.1728 -0.0506 0.107 Uiso 1 1 calc R . . C22A C 0.2516(3) 1.1267(4) -0.0901(5) 0.113(8) Uani 1 1 d G . . H22A H 0.2747 1.1383 -0.1018 0.136 Uiso 1 1 calc R . . C23A C 0.2414(4) 1.0891(4) -0.1034(6) 0.140(11) Uani 1 1 d G . . C24A C 0.2076(4) 1.0721(3) -0.0863(6) 0.114(8) Uani 1 1 d G . . H24A H 0.2007 1.0464 -0.0954 0.137 Uiso 1 1 calc R . . C25A C 0.1841(3) 1.0926(3) -0.0559(4) 0.090(5) Uani 1 1 d G . . H25A H 0.1610 1.0809 -0.0442 0.108 Uiso 1 1 calc R . . C26A C 0.2667(11) 1.0709(11) -0.1392(13) 0.215(16) Uiso 1 1 d . . . H26A H 0.2938 1.0697 -0.1277 0.259 Uiso 1 1 calc . . . H26B H 0.2665 1.0874 -0.1672 0.259 Uiso 1 1 calc . . . N31A N 0.1931(4) 0.8630(3) -0.0325(4) 0.097(5) Uani 1 1 d G . . C31A C 0.2275(4) 0.8458(3) -0.0473(5) 0.132(8) Uani 1 1 d G . . H31A H 0.2351 0.8210 -0.0357 0.159 Uiso 1 1 calc R . . C32A C 0.2510(4) 0.8648(4) -0.0792(6) 0.142(10) Uani 1 1 d G . . H32A H 0.2745 0.8530 -0.0894 0.171 Uiso 1 1 calc R . . C33A C 0.2400(4) 0.9010(5) -0.0963(5) 0.124(8) Uani 1 1 d G . . C34A C 0.2055(4) 0.9182(3) -0.0814(5) 0.113(8) Uani 1 1 d G . . H34A H 0.1980 0.9429 -0.0931 0.135 Uiso 1 1 calc R . . C35A C 0.1821(3) 0.8992(3) -0.0495(5) 0.088(6) Uani 1 1 d G . . H35A H 0.1585 0.9109 -0.0394 0.106 Uiso 1 1 calc R . . C36A C 0.2694(7) 0.9257(9) -0.1294(11) 0.25(2) Uani 1 1 d . . . H36A H 0.2916 0.9347 -0.1105 0.299 Uiso 1 1 calc . . . H36B H 0.2799 0.9077 -0.1530 0.299 Uiso 1 1 calc . . . C21 C -0.0092(7) 0.8030(3) 0.2320(3) 0.181(16) Uani 1 1 d G . . C22 C -0.0423(5) 0.7882(4) 0.2107(6) 0.118(8) Uani 1 1 d G . . H22 H -0.0674 0.7967 0.2201 0.141 Uiso 1 1 calc R . . C23 C -0.0387(4) 0.7611(5) 0.1754(5) 0.088(5) Uiso 1 1 d G . . C24 C -0.0020(6) 0.7488(3) 0.1615(3) 0.124(8) Uani 1 1 d G . . H24 H 0.0005 0.7303 0.1373 0.149 Uiso 1 1 calc R . . C25 C 0.0311(4) 0.7635(5) 0.1829(6) 0.174(16) Uani 1 1 d G . . C26 C 0.0275(5) 0.7906(5) 0.2182(6) 0.145(14) Uani 1 1 d G . . H26 H 0.0501 0.8007 0.2328 0.173 Uiso 1 1 calc R . . N11B N -0.0092(3) 0.95262(16) 0.2501(4) 0.082(4) Uani 1 1 d G . . C11B C -0.0095(5) 0.9373(2) 0.2944(3) 0.156(10) Uani 1 1 d G . . H11B H -0.0092 0.9543 0.3202 0.187 Uiso 1 1 calc R . . C12B C -0.0102(7) 0.8972(3) 0.3008(3) 0.199(14) Uani 1 1 d G . . H12B H -0.0105 0.8867 0.3311 0.239 Uiso 1 1 calc R . . C13B C -0.0106(6) 0.87235(16) 0.2630(3) 0.148(11) Uani 1 1 d G . . C14B C -0.0103(5) 0.8877(2) 0.2188(3) 0.104(7) Uani 1 1 d G . . H14B H -0.0106 0.8707 0.1929 0.125 Uiso 1 1 calc R . . C15B C -0.0096(4) 0.9278(2) 0.2123(3) 0.084(5) Uani 1 1 d G . . H15B H -0.0093 0.9383 0.1820 0.101 Uiso 1 1 calc R . . C16B C -0.0113(19) 0.8290(4) 0.2706(6) 0.40(3) Uani 1 1 d . . . H16C H 0.0108 0.8226 0.2912 0.475 Uiso 1 1 calc . . . H16D H -0.0355 0.8228 0.2876 0.475 Uiso 1 1 calc . . . N21B N -0.1333(4) 0.8105(4) 0.0494(4) 0.084(5) Uani 1 1 d G . . C21B C -0.1508(4) 0.7774(4) 0.0677(5) 0.106(7) Uani 1 1 d G . . H21B H -0.1751 0.7686 0.0558 0.127 Uiso 1 1 calc R . . C22B C -0.1329(5) 0.7573(4) 0.1034(5) 0.133(10) Uani 1 1 d G . . H22B H -0.1449 0.7347 0.1159 0.159 Uiso 1 1 calc R . . C23B C -0.0975(5) 0.7702(5) 0.1208(5) 0.134(10) Uani 1 1 d G . . C24B C -0.0799(4) 0.8033(5) 0.1025(6) 0.127(9) Uani 1 1 d G . . H24B H -0.0557 0.8121 0.1144 0.152 Uiso 1 1 calc R . . C25B C -0.0979(4) 0.8234(4) 0.0668(5) 0.128(9) Uani 1 1 d G . . H25B H -0.0859 0.8460 0.0543 0.153 Uiso 1 1 calc R . . C26B C -0.0789(7) 0.7472(12) 0.1593(13) 0.29(3) Uani 1 1 d . . . H26C H -0.0766 0.7197 0.1492 0.343 Uiso 1 1 calc . . . H26D H -0.0968 0.7477 0.1860 0.343 Uiso 1 1 calc . . . N31B N 0.1319(3) 0.8086(3) 0.0638(3) 0.060(4) Uani 1 1 d G . . C31B C 0.1460(3) 0.7746(3) 0.0839(4) 0.086(6) Uani 1 1 d G . . H31B H 0.1708 0.7647 0.0752 0.103 Uiso 1 1 calc R . . C32B C 0.1238(4) 0.7552(3) 0.1166(5) 0.142(11) Uani 1 1 d G . . H32B H 0.1334 0.7319 0.1303 0.170 Uiso 1 1 calc R . . C33B C 0.0875(3) 0.7697(4) 0.1293(5) 0.146(11) Uani 1 1 d G . . C34B C 0.0735(3) 0.8036(4) 0.1093(5) 0.105(7) Uani 1 1 d G . . H34B H 0.0487 0.8135 0.1179 0.126 Uiso 1 1 calc R . . C35B C 0.0956(3) 0.8231(3) 0.0765(4) 0.062(4) Uiso 1 1 d G . . H35B H 0.0860 0.8463 0.0628 0.074 Uiso 1 1 calc R . . C36B C 0.0653(8) 0.7428(8) 0.1586(15) 0.32(3) Uani 1 1 d . . . H36C H 0.0829 0.7315 0.1820 0.385 Uiso 1 1 calc . . . H36D H 0.0550 0.7212 0.1395 0.385 Uiso 1 1 calc . . . O101 O 0.2256(4) 1.2256(4) 0.0000 0.100(5) Uiso 1 2 d S . . O102 O 0.2500 1.2500 0.0000 0.087(6) Uiso 1 4 d S . . O103 O -0.2730(3) 1.2270(3) 0.5275(6) 0.095(4) Uiso 1 2 d S . . O104 O 0.0982(3) 0.9018(3) 0.0037(3) 0.056(3) Uiso 1 2 d S . . O105 O -0.0139(3) 1.0139(3) 0.3611(5) 0.114(5) Uiso 1 2 d S . . C101 C -0.0085(6) 1.0085(6) 0.1388(10) 0.106(9) Uiso 1 2 d S . . C102 C -0.2500 1.2500 0.4612(9) 0.068(7) Uiso 1 4 d S . . C103 C -0.227(3) 1.227(3) 0.545(4) 0.32(6) Uiso 0.50 2 d SP . . C104 C 0.113(2) 0.887(2) -0.126(4) 0.54(6) Uiso 1 2 d S . . C105 C 0.0018(13) 0.9982(13) 0.402(3) 0.37(4) Uiso 1 2 d S . . C106 C 0.3315(19) 1.112(2) -0.0053(17) 0.36(3) Uiso 1 1 d . . . C107 C 0.0506(15) 0.9494(15) 0.0022(14) 0.26(3) Uiso 1 2 d S . . C108 C 0.264(2) 1.044(2) 0.0110(16) 0.29(3) Uiso 1 1 d . . . C109 C 0.274(3) 0.998(10) 0.006(2) 0.35(4) Uiso 1 1 d . . . C110 C 0.0495(12) 0.9505(12) 0.1061(18) 0.23(2) Uiso 1 2 d S . . C111 C 0.2745(11) 1.2221(11) -0.1261(14) 0.240(15) Uiso 1 1 d . . . C112 C 0.0764(9) 1.0797(9) 0.0188(10) 0.200(14) Uiso 1 1 d . . . C113 C -0.0818(19) 0.9286(19) 0.100(3) 0.37(4) Uiso 1 1 d . . . C114 C -0.1367(18) 0.8920(16) 0.173(2) 0.34(3) Uiso 1 1 d . . . C115 C 0.075(2) 0.925(2) -0.083(3) 0.38(5) Uiso 1 2 d S . . C116 C -0.0046(8) 0.8672(5) 0.0948(6) 0.142(6) Uiso 1 1 d . . . C117 C 0.2649(14) 0.9595(15) 0.0282(16) 0.261(18) Uiso 1 1 d . . . C118 C -0.1133(12) 0.8671(13) 0.1969(15) 0.240(16) Uiso 1 1 d . . . C119 C 0.1498(8) 0.8502(8) 0.1802(12) 0.152(11) Uiso 1 2 d S . . C120 C -0.1769(18) 0.862(2) 0.174(2) 0.39(3) Uiso 1 1 d . . . C121 C 0.4050(17) 1.1325(16) -0.1566(19) 0.39(3) Uiso 1 1 d . . . C122 C 0.3490(12) 1.2500 -0.2500 0.220(17) Uiso 1 2 d S . . C123 C 0.3395(10) 1.0102(13) 0.0950(12) 0.273(16) Uiso 1 1 d . . . C124 C 0.3591(10) 0.8591(10) -0.1039(16) 0.231(19) Uiso 1 2 d S . . C125 C 0.1440(6) 0.9968(10) -0.0758(7) 0.162(7) Uiso 1 1 d . . . C126 C 0.3294(9) 0.8294(9) 0.0395(17) 0.242(19) Uiso 1 2 d S . . C127 C -0.1810(12) 1.1810(12) 0.330(2) 0.31(3) Uiso 1 2 d S . . C128 C -0.2500 1.2500 0.5340(19) 0.141(15) Uiso 1 4 d S . . C129 C -0.1236(14) 0.8355(14) 0.2254(17) 0.292(19) Uiso 1 1 d . . . C130 C 0.153(2) 0.857(2) -0.1723(13) 0.34(2) Uiso 1 1 d . . . C131 C 0.3853(12) 0.9630(13) 0.0785(14) 0.264(18) Uiso 1 1 d . . . C132 C -0.2276(10) 0.8690(9) 0.2626(13) 0.247(15) Uiso 1 1 d . . . C133 C 0.3652(14) 0.997(2) -0.0742(16) 0.37(2) Uiso 1 1 d . . . C134 C 0.3269(8) 1.1731(8) 0.0000 0.138(12) Uiso 1 2 d S . . C135 C -0.0033(15) 1.0033(15) 0.124(3) 0.36(4) Uiso 1 2 d S . . C136 C 0.444(3) 0.944(3) 0.178(5) 0.86(12) Uiso 1 2 d S . . C137 C 0.3523(12) 1.1464(12) -0.1383(16) 0.255(17) Uiso 1 1 d . . . C138 C 0.2402(9) 1.2257(8) -0.1503(11) 0.179(10) Uiso 1 1 d . . . C139 C 0.0568(15) 0.9432(15) -0.097(2) 0.28(3) Uiso 1 2 d S . . C140 C -0.1238(14) 0.8953(12) 0.2335(16) 0.267(17) Uiso 1 1 d . . . C141 C -0.1578(10) 0.8918(8) 0.2131(11) 0.170(9) Uiso 1 1 d . . . C142 C 0.2355(16) 1.003(3) 0.0168(15) 0.36(3) Uiso 1 1 d . . . C143 C 0.3589(11) 1.2013(11) -0.2369(13) 0.258(15) Uiso 1 1 d . . . C144 C 0.3585(18) 1.1760(15) -0.0155(19) 0.32(3) Uiso 1 1 d . . . C145 C 0.3499(13) 0.9632(13) 0.0977(15) 0.29(2) Uiso 1 1 d . . . C146 C -0.1897(14) 0.8800(12) 0.2351(15) 0.280(18) Uiso 1 1 d . . . C147 C 0.3856(12) 1.0547(12) -0.1192(14) 0.265(18) Uiso 1 1 d . . . C148 C 0.044(2) 0.915(2) 0.114(2) 0.55(5) Uiso 1 1 d . . . C149 C -0.0143(5) 1.0143(5) 0.4116(8) 0.085(7) Uiso 1 2 d S . . C150 C 0.3283(12) 1.1722(13) -0.1921(18) 0.28(2) Uiso 1 1 d . . . C151 C 0.3695(16) 1.0574(17) 0.1047(19) 0.36(3) Uiso 1 1 d . . . C152 C 0.286(2) 0.973(3) -0.004(2) 0.33(4) Uiso 1 1 d . . . C153 C 0.3776(14) 0.9602(15) -0.0876(17) 0.30(2) Uiso 1 1 d . . . C154 C 0.395(2) 0.895(2) -0.095(4) 0.59(6) Uiso 1 2 d S . . 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 0.0665(9) 0.0665(9) 0.0546(11) 0.0039(10) -0.0039(10) -0.0057(11) Pd2 0.0385(5) 0.0385(5) 0.1169(12) 0.0028(5) -0.0028(5) -0.0012(5) Pd3 0.0661(10) 0.0661(10) 0.065(2) -0.0015(5) 0.0015(5) 0.0000(12) C11 0.048(8) 0.19(2) 0.092(13) 0.093(16) 0.049(8) 0.058(13) C12 0.067(13) 0.057(10) 0.18(2) 0.075(12) 0.035(13) 0.013(9) C13 0.055(10) 0.079(12) 0.17(2) -0.053(12) 0.066(12) -0.019(9) C14 0.052(7) 0.187(19) 0.057(9) -0.024(13) 0.009(6) 0.017(12) C16 0.048(9) 0.130(17) 0.092(13) -0.071(12) 0.071(9) -0.045(10) N11A 0.032(4) 0.057(7) 0.094(8) -0.010(6) 0.010(6) -0.005(4) C11A 0.054(9) 0.17(2) 0.087(12) -0.012(11) -0.013(8) -0.004(10) C12A 0.054(8) 0.26(3) 0.059(10) -0.008(13) 0.003(7) -0.033(13) C13A 0.061(7) 0.28(2) 0.045(9) -0.026(14) 0.004(7) -0.034(14) C14A 0.052(7) 0.135(15) 0.079(10) -0.028(11) 0.015(7) -0.023(10) C15A 0.036(6) 0.084(12) 0.085(10) -0.019(8) 0.011(6) -0.003(7) C16A 0.037(6) 0.50(4) 0.044(9) -0.04(2) 0.012(7) -0.05(2) N21A 0.072(9) 0.070(8) 0.045(8) -0.005(6) 0.026(6) -0.005(7) C21A 0.064(11) 0.120(14) 0.082(13) -0.050(10) 0.028(9) -0.033(10) C22A 0.092(14) 0.107(14) 0.141(18) -0.078(13) 0.043(13) -0.017(11) C23A 0.083(14) 0.123(16) 0.21(2) -0.115(17) 0.076(15) -0.018(12) C24A 0.095(15) 0.100(14) 0.148(19) -0.051(13) 0.068(14) -0.006(11) C25A 0.091(13) 0.099(13) 0.079(13) -0.018(10) 0.015(10) 0.011(11) N31A 0.079(11) 0.072(9) 0.140(15) 0.036(10) 0.000(10) -0.002(8) C31A 0.133(19) 0.16(2) 0.102(17) 0.037(14) 0.052(14) 0.017(16) C32A 0.126(19) 0.16(2) 0.14(2) 0.058(17) 0.059(17) 0.086(16) C33A 0.15(2) 0.114(16) 0.110(18) 0.065(13) 0.068(14) 0.028(14) C34A 0.101(15) 0.106(14) 0.131(18) 0.061(12) 0.077(14) 0.054(12) C35A 0.084(12) 0.050(10) 0.130(17) 0.038(9) 0.043(11) 0.017(8) C36A 0.134(18) 0.31(4) 0.30(3) 0.24(3) 0.18(2) 0.15(2) C21 0.42(5) 0.061(10) 0.064(13) 0.058(9) -0.06(3) -0.09(2) C22 0.15(2) 0.055(12) 0.15(2) 0.073(13) 0.049(15) 0.038(12) C24 0.26(2) 0.051(8) 0.063(11) 0.012(7) 0.061(19) 0.030(19) C25 0.35(5) 0.055(14) 0.12(2) 0.080(14) 0.09(2) 0.031(19) C26 0.17(2) 0.11(2) 0.15(3) 0.110(18) -0.106(19) -0.097(17) N11B 0.105(10) 0.045(5) 0.096(9) -0.008(6) -0.012(8) 0.010(6) C11B 0.30(3) 0.045(8) 0.126(16) -0.016(9) -0.023(19) -0.006(15) C12B 0.44(5) 0.051(9) 0.107(15) 0.000(9) 0.03(2) 0.01(2) C13B 0.34(3) 0.041(7) 0.063(11) 0.021(7) 0.011(16) 0.056(13) C14B 0.21(2) 0.040(7) 0.065(10) 0.002(6) 0.010(11) -0.003(10) C15B 0.101(15) 0.044(7) 0.106(12) 0.024(8) 0.012(10) 0.008(8) C16B 1.10(10) 0.030(7) 0.056(12) -0.013(7) 0.06(4) 0.00(3) N21B 0.102(11) 0.075(9) 0.075(10) 0.052(7) -0.017(8) -0.024(8) C21B 0.090(13) 0.098(14) 0.130(17) 0.058(12) -0.027(11) -0.038(11) C22B 0.106(15) 0.15(2) 0.139(19) 0.094(16) -0.064(14) -0.044(14) C23B 0.106(15) 0.127(18) 0.17(2) 0.107(16) -0.068(15) -0.051(13) C24B 0.087(13) 0.14(2) 0.16(2) 0.101(17) -0.042(13) -0.027(13) C25B 0.093(14) 0.147(19) 0.144(19) 0.083(15) -0.031(12) -0.020(13) C26B 0.117(18) 0.40(5) 0.34(5) 0.31(4) -0.10(2) -0.12(3) N31B 0.088(9) 0.071(9) 0.021(7) 0.008(6) -0.005(6) -0.024(7) C31B 0.062(10) 0.081(12) 0.114(15) 0.048(11) 0.028(9) 0.027(9) C32B 0.103(15) 0.118(16) 0.20(3) 0.097(16) 0.096(16) 0.044(13) C33B 0.076(12) 0.122(18) 0.24(3) 0.106(19) 0.071(15) 0.040(11) C34B 0.103(14) 0.067(12) 0.15(2) 0.057(12) 0.020(12) 0.010(10) C36B 0.18(2) 0.20(3) 0.59(7) 0.31(4) 0.27(3) 0.14(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 N31A 1.951(9) 15_665 ? Pd1 N31A 1.951(9) . ? Pd1 N31B 2.015(8) 15_665 ? Pd1 N31B 2.015(8) . ? Pd2 N11B 1.977(5) 15_665 ? Pd2 N11B 1.977(5) . ? Pd2 N11A 1.990(5) 9_575 ? Pd2 N11A 1.990(5) 7_465 ? Pd3 N21B 1.980(9) 15_665 ? Pd3 N21B 1.980(9) 9_575 ? Pd3 N21A 1.987(8) . ? Pd3 N21A 1.987(8) 7_465 ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C11 C16A 1.503(15) . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C13 C26A 1.59(4) . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C15 C36A 1.40(2) . ? N11A C11A 1.3900 . ? N11A C15A 1.3900 . ? N11A Pd2 1.990(5) 9_575 ? C11A C12A 1.3900 . ? C12A C13A 1.3900 . ? C13A C14A 1.3900 . ? C13A C16A 1.514(12) . ? C14A C15A 1.3900 . ? N21A C21A 1.3900 . ? N21A C25A 1.3900 . ? C21A C22A 1.3900 . ? C22A C23A 1.3900 . ? C23A C24A 1.3900 . ? C23A C26A 1.49(4) . ? C24A C25A 1.3900 . ? N31A C31A 1.3900 . ? N31A C35A 1.3900 . ? C31A C32A 1.3900 . ? C32A C33A 1.3900 . ? C33A C34A 1.3900 . ? C33A C36A 1.63(2) . ? C34A C35A 1.3900 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C21 C16B 1.434(17) . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C23 C26B 1.53(3) . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C25 C36B 1.54(3) . ? N11B C11B 1.3900 . ? N11B C15B 1.3900 . ? C11B C12B 1.3900 . ? C12B C13B 1.3900 . ? C13B C14B 1.3900 . ? C13B C16B 1.503(15) . ? C14B C15B 1.3900 . ? N21B C21B 1.3900 . ? N21B C25B 1.3900 . ? N21B Pd3 1.980(9) 9_575 ? C21B C22B 1.3900 . ? C22B C23B 1.3900 . ? C23B C24B 1.3900 . ? C23B C26B 1.51(3) . ? C24B C25B 1.3900 . ? N31B C31B 1.3900 . ? N31B C35B 1.3900 . ? C31B C32B 1.3900 . ? C32B C33B 1.3900 . ? C33B C34B 1.3900 . ? C33B C36B 1.467(19) . ? C34B C35B 1.3900 . ? O101 O102 1.185(18) . ? O102 O101 1.185(18) 2_575 ? O103 C128 1.133(17) . ? O103 C103 1.64(9) . ? O103 C103 1.64(9) 2_475 ? O105 C105 1.41(7) . ? O105 C149 1.47(3) . ? C103 C128 1.14(12) . ? C103 O103 1.64(9) 2_475 ? C105 C149 0.82(7) . ? C106 C144 1.20(7) 8_665 ? C108 C142 1.74(9) . ? C108 C109 1.6(3) . ? C109 C152 1.0(3) . ? C109 C117 1.5(3) . ? C109 C142 1.38(9) . ? C110 C148 1.25(8) 15_665 ? C110 C148 1.25(8) . ? C111 C138 1.38(4) . ? C111 C138 1.99(4) 2_575 ? C112 C112 1.10(6) 7_465 ? C114 C141 1.38(6) . ? C114 C118 1.37(6) . ? C114 C120 1.73(7) . ? C114 C140 1.83(7) . ? C115 C139 1.00(11) . ? C117 C152 1.28(10) . ? C117 C142 1.83(10) . ? C118 C129 1.41(5) . ? C118 C140 1.48(5) . ? C118 C141 1.81(5) . ? C120 C141 1.67(7) . ? C120 C146 1.94(7) . ? C121 C137 1.94(7) . ? C121 C151 1.99(7) 8_665 ? C122 C143 1.75(4) 6_574 ? C122 C143 1.75(4) . ? C123 C145 1.65(5) . ? C123 C151 1.94(7) . ? C124 C154 1.78(11) . ? C128 O103 1.133(17) 2_475 ? C128 C103 1.14(12) 2_475 ? C129 C143 1.78(5) 13_576 ? C129 C140 2.07(6) . ? C131 C145 1.34(5) . ? C132 C146 1.57(5) . ? C132 C132 1.70(6) 5_455 ? C133 C153 1.40(8) . ? C134 C144 1.18(6) . ? C134 C144 1.18(6) 8_665 ? C138 C138 1.80(6) 2_575 ? C138 C111 1.99(4) 2_575 ? C140 C141 1.31(5) . ? C141 C146 1.33(5) . ? C143 C129 1.78(5) 13_675 ? C143 C150 1.95(5) . ? C144 C106 1.20(7) 8_665 ? C144 C144 1.90(11) 8_665 ? C151 C121 1.99(7) 8_665 ? 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 N31A Pd1 N31A 88.4(8) 15_665 . ? N31A Pd1 N31B 177.8(5) 15_665 15_665 ? N31A Pd1 N31B 90.0(5) . 15_665 ? N31A Pd1 N31B 90.0(5) 15_665 . ? N31A Pd1 N31B 177.8(5) . . ? N31B Pd1 N31B 91.6(6) 15_665 . ? N11B Pd2 N11B 87.9(6) 15_665 . ? N11B Pd2 N11A 175.1(4) 15_665 9_575 ? N11B Pd2 N11A 91.6(4) . 9_575 ? N11B Pd2 N11A 91.6(4) 15_665 7_465 ? N11B Pd2 N11A 175.1(4) . 7_465 ? N11A Pd2 N11A 88.5(5) 9_575 7_465 ? N21B Pd3 N21B 178.2(7) 15_665 9_575 ? N21B Pd3 N21A 85.0(7) 15_665 . ? N21B Pd3 N21A 95.0(7) 9_575 . ? N21B Pd3 N21A 95.0(7) 15_665 7_465 ? N21B Pd3 N21A 85.0(7) 9_575 7_465 ? N21A Pd3 N21A 179.6(7) . 7_465 ? C12 C11 C16 120.0 . . ? C12 C11 C16A 120(2) . . ? C16 C11 C16A 119(2) . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 C26A 127.0(18) . . ? C12 C13 C26A 112.7(18) . . ? C13 C14 C15 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 C36A 113(2) . . ? C16 C15 C36A 127(2) . . ? C15 C16 C11 120.0 . . ? C11A N11A C15A 120.0 . . ? C11A N11A Pd2 117.6(5) . 9_575 ? C15A N11A Pd2 122.3(5) . 9_575 ? C12A C11A N11A 120.0 . . ? C11A C12A C13A 120.0 . . ? C14A C13A C12A 120.0 . . ? C14A C13A C16A 126.2(8) . . ? C12A C13A C16A 113.8(8) . . ? C15A C14A C13A 120.0 . . ? C14A C15A N11A 120.0 . . ? C11 C16A C13A 112.8(9) . . ? C21A N21A C25A 120.0 . . ? C21A N21A Pd3 117.0(6) . . ? C25A N21A Pd3 123.0(6) . . ? C22A C21A N21A 120.0 . . ? C21A C22A C23A 120.0 . . ? C24A C23A C22A 120.0 . . ? C24A C23A C26A 123.9(16) . . ? C22A C23A C26A 115.9(17) . . ? C25A C24A C23A 120.0 . . ? C24A C25A N21A 120.0 . . ? C23A C26A C13 112(2) . . ? C31A N31A C35A 120.0 . . ? C31A N31A Pd1 118.8(7) . . ? C35A N31A Pd1 121.0(7) . . ? N31A C31A C32A 120.0 . . ? C33A C32A C31A 120.0 . . ? C32A C33A C34A 120.0 . . ? C32A C33A C36A 120.4(11) . . ? C34A C33A C36A 119.3(12) . . ? C33A C34A C35A 120.0 . . ? C34A C35A N31A 120.0 . . ? C15 C36A C33A 116.4(14) . . ? C22 C21 C26 120.0 . . ? C22 C21 C16B 122(3) . . ? C26 C21 C16B 117(3) . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 C26B 129(2) . . ? C22 C23 C26B 111(2) . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 C36B 136(2) . . ? C24 C25 C36B 104(2) . . ? C25 C26 C21 120.0 . . ? C11B N11B C15B 120.0 . . ? C11B N11B Pd2 117.9(5) . . ? C15B N11B Pd2 122.1(5) . . ? C12B C11B N11B 120.0 . . ? C11B C12B C13B 120.0 . . ? C12B C13B C14B 120.0 . . ? C12B C13B C16B 119.4(9) . . ? C14B C13B C16B 120.6(9) . . ? C13B C14B C15B 120.0 . . ? C14B C15B N11B 120.0 . . ? C21 C16B C13B 120.1(13) . . ? C21B N21B C25B 120.0 . . ? C21B N21B Pd3 116.7(7) . 9_575 ? C25B N21B Pd3 123.2(7) . 9_575 ? N21B C21B C22B 120.0 . . ? C23B C22B C21B 120.0 . . ? C22B C23B C24B 120.0 . . ? C22B C23B C26B 118.1(13) . . ? C24B C23B C26B 121.9(13) . . ? C25B C24B C23B 120.0 . . ? C24B C25B N21B 120.0 . . ? C23B C26B C23 116.2(17) . . ? C31B N31B C35B 120.0 . . ? C31B N31B Pd1 121.2(6) . . ? C35B N31B Pd1 118.8(6) . . ? N31B C31B C32B 120.0 . . ? C33B C32B C31B 120.0 . . ? C32B C33B C34B 120.0 . . ? C32B C33B C36B 113.2(11) . . ? C34B C33B C36B 126.1(11) . . ? C35B C34B C33B 120.0 . . ? C34B C35B N31B 120.0 . . ? C33B C36B C25 111.8(16) . . ? O101 O102 O101 180.0(9) 2_575 . ? C128 O103 C103 44(3) . . ? C128 O103 C103 44(3) . 2_475 ? C103 O103 C103 84(7) . 2_475 ? C105 O105 C149 33(3) . . ? C128 C103 O103 44(3) . 2_475 ? C128 C103 O103 44(3) . . ? O103 C103 O103 86(6) 2_475 . ? C149 C105 O105 77(6) . . ? C142 C108 C109 48(4) . . ? C152 C109 C117 58(10) . . ? C152 C109 C142 126(10) . . ? C117 C109 C142 79(10) . . ? C152 C109 C108 161(10) . . ? C117 C109 C108 141(8) . . ? C142 C109 C108 70(10) . . ? C148 C110 C148 106(9) 15_665 . ? C138 C111 C138 61(3) . 2_575 ? C141 C114 C118 82(4) . . ? C141 C114 C120 64(3) . . ? C118 C114 C120 95(4) . . ? C141 C114 C140 46(2) . . ? C118 C114 C140 53(3) . . ? C120 C114 C140 102(4) . . ? C152 C117 C109 41(8) . . ? C152 C117 C142 84(5) . . ? C109 C117 C142 48(5) . . ? C114 C118 C129 129(5) . . ? C114 C118 C140 80(4) . . ? C129 C118 C140 91(4) . . ? C114 C118 C141 49(3) . . ? C129 C118 C141 90(3) . . ? C140 C118 C141 46(2) . . ? C114 C120 C141 48(3) . . ? C114 C120 C146 90(4) . . ? C141 C120 C146 42(2) . . ? C137 C121 C151 114(4) . 8_665 ? C143 C122 C143 158(4) 6_574 . ? C145 C123 C151 134(3) . . ? O103 C128 O103 161(6) . 2_475 ? O103 C128 C103 92.6(10) . . ? O103 C128 C103 92.6(10) 2_475 . ? O103 C128 C103 92.6(11) . 2_475 ? O103 C128 C103 92.6(10) 2_475 2_475 ? C103 C128 C103 148(10) . 2_475 ? C118 C129 C143 174(4) . 13_576 ? C118 C129 C140 46(2) . . ? C143 C129 C140 129(3) 13_576 . ? C146 C132 C132 122(4) . 5_455 ? C144 C134 C144 108(6) . 8_665 ? C111 C138 C138 76(2) . 2_575 ? C111 C138 C111 97(3) . 2_575 ? C138 C138 C111 42.3(12) 2_575 2_575 ? C141 C140 C118 80(3) . . ? C141 C140 C114 49(3) . . ? C118 C140 C114 47(3) . . ? C141 C140 C129 82(3) . . ? C118 C140 C129 43(2) . . ? C114 C140 C129 80(3) . . ? C146 C141 C114 147(4) . . ? C146 C141 C140 123(4) . . ? C114 C141 C140 85(4) . . ? C146 C141 C120 79(3) . . ? C114 C141 C120 68(3) . . ? C140 C141 C120 135(4) . . ? C146 C141 C118 133(3) . . ? C114 C141 C118 49(3) . . ? C140 C141 C118 54(2) . . ? C120 C141 C118 82(3) . . ? C109 C142 C108 62(10) . . ? C109 C142 C117 53(10) . . ? C108 C142 C117 112(4) . . ? C122 C143 C129 128(3) . 13_675 ? C122 C143 C150 122(3) . . ? C129 C143 C150 103(3) 13_675 . ? C106 C144 C134 124(7) 8_665 . ? C106 C144 C144 98(5) 8_665 8_665 ? C134 C144 C144 36(3) . 8_665 ? C131 C145 C123 101(4) . . ? C141 C146 C132 176(4) . . ? C141 C146 C120 58(3) . . ? C132 C146 C120 125(4) . . ? C105 C149 O105 70(6) . . ? C123 C151 C121 129(4) . 8_665 ? C109 C152 C117 81(10) . . ? _diffrn_measured_fraction_theta_max 0.748 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.748 _refine_diff_density_max 1.201 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.179