Supplementary Material (ESI) for Chemical Science This journal is (c) The Royal Society of Chemistry 2010 data_publication_text _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _publ_contact_author_name 'Magnus Rueping' _publ_section_title 'Asymmetric Br\/onsted Acid Catalysis in Aqueous Solution' _publ_section_abstract ; (type here to add abstract) ; loop_ _publ_contact_author_address ;Institute of Organic Chemistry RWTH Aachen University Landoltweg 1 D-52074, Aachen Germany ; _publ_contact_author_email magnus.rueping@rwth-aachen.de _publ_contact_author_phone '(49) 241 80 94686' _publ_contact_author_fax '(+49) 241 80 92665' loop_ _publ_author_name _publ_author_address M.Rueping ;Institute of Organic Chemistry RWTH Aachen University Landoltweg 1 D-52074, Aachen Germany ; T.Theissmann ;Institute of Organic Chemistry RWTH Aachen University Landoltweg 1 D-52074, Aachen Germany ; data_1c _database_code_depnum_ccdc_archive 'CCDC 783865' #TrackingRef 'web_deposit_cif_file_0_RuepingMagnus_1278784359.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H57 O4 P, 0.5(H2 O)' _chemical_formula_sum 'C50 H58 O4.50 P' _chemical_formula_weight 761.93 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41212' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 16.2608(16) _cell_length_b 16.2608(16) _cell_length_c 34.648(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9161.4(18) _cell_formula_units_Z 8 _cell_measurement_temperature 167(2) _cell_measurement_reflns_used 217 _cell_measurement_theta_min 3 _cell_measurement_theta_max 23 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.927 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details 'SHELXTL (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 167(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type SIEMENS_SMART_CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1023 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1200 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 77950 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9721 _reflns_number_gt 8113 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.04P)^2^+2P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(10) _refine_ls_number_reflns 9721 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0993 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.296 _refine_ls_restrained_S_all 1.296 _refine_ls_shift/su_max 0.001 _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 P1 P 0.60724(4) 0.47815(4) 0.050227(19) 0.02464(16) Uani 1 1 d . . . O2 O 0.60143(10) 0.42429(10) 0.08819(5) 0.0245(4) Uani 1 1 d . . . O1 O 0.65605(10) 0.42244(10) 0.02035(5) 0.0250(4) Uani 1 1 d . . . O3 O 0.52316(11) 0.48979(12) 0.03402(5) 0.0367(5) Uani 1 1 d . . . H3B H 0.5260 0.4936 0.0099 0.055 Uiso 0.50 1 calc PR . . O4 O 0.65485(12) 0.55390(11) 0.06027(5) 0.0349(5) Uani 1 1 d . . . H4B H 0.6511 0.5881 0.0422 0.052 Uiso 0.50 1 calc PR . . C11 C 0.61622(15) 0.28583(15) 0.06560(7) 0.0237(6) Uani 1 1 d . . . C36 C 0.43672(16) 0.39510(16) 0.11697(7) 0.0272(6) Uani 1 1 d . . . C7 C 0.86286(16) 0.33870(16) 0.02779(7) 0.0278(6) Uani 1 1 d . . . H7A H 0.9162 0.3489 0.0177 0.033 Uiso 1 1 calc R . . C37 C 0.45540(16) 0.41394(17) 0.15552(8) 0.0318(6) Uani 1 1 d . . . C12 C 0.56819(16) 0.34450(15) 0.08286(7) 0.0238(5) Uani 1 1 d . . . C14 C 0.45742(17) 0.25219(17) 0.09265(8) 0.0330(7) Uani 1 1 d . . . H14A H 0.4053 0.2394 0.1035 0.040 Uiso 1 1 calc R . . C8 C 0.80064(15) 0.39238(16) 0.01910(7) 0.0251(6) Uani 1 1 d . . . C10 C 0.70314(16) 0.30353(15) 0.05410(7) 0.0239(6) Uani 1 1 d . . . C13 C 0.48679(16) 0.32996(15) 0.09671(7) 0.0259(6) Uani 1 1 d . . . C45 C 0.29176(19) 0.57619(19) 0.17882(8) 0.0390(7) Uani 1 1 d . . . H45A H 0.2503 0.5995 0.1605 0.047 Uiso 1 1 calc R . . C26 C 0.85645(15) 0.53547(16) 0.01702(7) 0.0262(6) Uani 1 1 d . . . C21 C 0.81742(15) 0.47071(16) -0.00233(7) 0.0244(6) Uani 1 1 d . . . C24 C 0.85246(15) 0.61623(16) -0.04217(8) 0.0285(6) Uani 1 1 d . . . C41 C 0.37027(15) 0.43330(16) 0.09854(7) 0.0260(6) Uani 1 1 d . . . C6 C 0.85043(17) 0.26839(16) 0.05136(7) 0.0294(6) Uani 1 1 d . . . C9 C 0.72126(15) 0.37166(15) 0.03231(7) 0.0234(6) Uani 1 1 d . . . C48 C 0.34424(18) 0.41276(17) 0.05723(8) 0.0344(7) Uani 1 1 d . . . H48A H 0.3921 0.3860 0.0442 0.041 Uiso 1 1 calc R . . C22 C 0.79587(15) 0.47777(17) -0.04159(7) 0.0269(6) Uani 1 1 d . . . C15 C 0.50052(17) 0.18964(16) 0.07315(8) 0.0313(6) Uani 1 1 d . . . C2 C 0.76138(17) 0.18420(16) 0.09110(8) 0.0308(6) Uani 1 1 d . . . H2A H 0.7089 0.1727 0.1018 0.037 Uiso 1 1 calc R . . C19 C 0.61923(18) 0.14575(16) 0.03525(8) 0.0340(7) Uani 1 1 d . . . H19A H 0.6705 0.1575 0.0233 0.041 Uiso 1 1 calc R . . C40 C 0.32394(16) 0.49050(16) 0.11919(7) 0.0290(6) Uani 1 1 d . . . H40A H 0.2784 0.5159 0.1069 0.035 Uiso 1 1 calc R . . C4 C 0.90527(18) 0.15096(18) 0.08542(8) 0.0388(7) Uani 1 1 d . . . H4A H 0.9499 0.1155 0.0915 0.047 Uiso 1 1 calc R . . C25 C 0.87102(15) 0.60790(16) -0.00379(7) 0.0244(6) Uani 1 1 d . . . H25A H 0.8949 0.6533 0.0093 0.029 Uiso 1 1 calc R . . C20 C 0.58012(16) 0.20683(16) 0.05798(7) 0.0278(6) Uani 1 1 d . . . C42 C 0.52280(19) 0.37070(18) 0.17800(8) 0.0407(8) Uani 1 1 d . . . H42A H 0.5541 0.3357 0.1594 0.049 Uiso 1 1 calc R . . C23 C 0.81395(16) 0.55040(17) -0.06087(8) 0.0318(7) Uani 1 1 d . . . H23A H 0.7998 0.5555 -0.0874 0.038 Uiso 1 1 calc R . . C33 C 0.88313(17) 0.52930(17) 0.05878(7) 0.0310(6) Uani 1 1 d . . . H33A H 0.8529 0.4819 0.0705 0.037 Uiso 1 1 calc R . . C38 C 0.40769(17) 0.47246(17) 0.17463(8) 0.0350(7) Uani 1 1 d . . . H38A H 0.4208 0.4859 0.2006 0.042 Uiso 1 1 calc R . . C1 C 0.77061(16) 0.25158(15) 0.06535(7) 0.0261(6) Uani 1 1 d . . . C29 C 0.6781(2) 0.4348(2) -0.08450(11) 0.0590(10) Uani 1 1 d . . . H29A H 0.6544 0.3881 -0.0985 0.088 Uiso 1 1 calc R . . H29B H 0.6920 0.4786 -0.1028 0.088 Uiso 1 1 calc R . . H29C H 0.6382 0.4555 -0.0657 0.088 Uiso 1 1 calc R . . C35 C 0.86298(19) 0.60520(19) 0.08277(8) 0.0399(7) Uani 1 1 d . . . H35A H 0.8040 0.6170 0.0809 0.060 Uiso 1 1 calc R . . H35B H 0.8943 0.6523 0.0730 0.060 Uiso 1 1 calc R . . H35C H 0.8777 0.5951 0.1098 0.060 Uiso 1 1 calc R . . C30 C 0.86983(18) 0.69620(17) -0.06386(8) 0.0355(7) Uani 1 1 d . . . H30A H 0.9091 0.7288 -0.0478 0.043 Uiso 1 1 calc R . . C5 C 0.91726(18) 0.21633(17) 0.06198(8) 0.0360(7) Uani 1 1 d . . . H5A H 0.9709 0.2277 0.0525 0.043 Uiso 1 1 calc R . . C27 C 0.75571(19) 0.40719(18) -0.06354(8) 0.0411(8) Uani 1 1 d . . . H27A H 0.7393 0.3646 -0.0442 0.049 Uiso 1 1 calc R . . C3 C 0.82700(19) 0.13554(18) 0.10068(8) 0.0380(7) Uani 1 1 d . . . H3A H 0.8194 0.0907 0.1179 0.046 Uiso 1 1 calc R . . C31 C 0.9105(2) 0.6826(2) -0.10301(9) 0.0538(9) Uani 1 1 d . . . H31A H 0.9206 0.7358 -0.1154 0.081 Uiso 1 1 calc R . . H31B H 0.8741 0.6495 -0.1194 0.081 Uiso 1 1 calc R . . H31C H 0.9628 0.6537 -0.0994 0.081 Uiso 1 1 calc R . . C50 C 0.32052(18) 0.4887(2) 0.03349(8) 0.0413(8) Uani 1 1 d . . . H50A H 0.3050 0.4716 0.0074 0.062 Uiso 1 1 calc R . . H50B H 0.3675 0.5264 0.0321 0.062 Uiso 1 1 calc R . . H50C H 0.2739 0.5165 0.0458 0.062 Uiso 1 1 calc R . . C43 C 0.5834(2) 0.4310(2) 0.19588(10) 0.0546(9) Uani 1 1 d . . . H43A H 0.6068 0.4660 0.1756 0.082 Uiso 1 1 calc R . . H43B H 0.6276 0.4005 0.2087 0.082 Uiso 1 1 calc R . . H43C H 0.5548 0.4654 0.2148 0.082 Uiso 1 1 calc R . . C32 C 0.7920(2) 0.7465(2) -0.06763(10) 0.0492(9) Uani 1 1 d . . . H32A H 0.8042 0.7978 -0.0813 0.074 Uiso 1 1 calc R . . H32B H 0.7706 0.7592 -0.0419 0.074 Uiso 1 1 calc R . . H32C H 0.7509 0.7150 -0.0821 0.074 Uiso 1 1 calc R . . C39 C 0.34186(16) 0.51168(17) 0.15708(8) 0.0308(6) Uani 1 1 d . . . C18 C 0.5842(2) 0.07067(18) 0.03031(10) 0.0470(8) Uani 1 1 d . . . H18A H 0.6120 0.0301 0.0155 0.056 Uiso 1 1 calc R . . C44 C 0.4860(2) 0.3138(2) 0.20829(10) 0.0614(10) Uani 1 1 d . . . H44A H 0.4471 0.2760 0.1959 0.092 Uiso 1 1 calc R . . H44B H 0.4571 0.3466 0.2278 0.092 Uiso 1 1 calc R . . H44C H 0.5300 0.2822 0.2207 0.092 Uiso 1 1 calc R . . C47 C 0.3464(2) 0.6469(2) 0.19280(10) 0.0539(9) Uani 1 1 d . . . H47A H 0.3746 0.6717 0.1707 0.081 Uiso 1 1 calc R . . H47B H 0.3872 0.6257 0.2111 0.081 Uiso 1 1 calc R . . H47C H 0.3123 0.6885 0.2056 0.081 Uiso 1 1 calc R . . C34 C 0.9755(2) 0.5108(2) 0.06216(9) 0.0530(9) Uani 1 1 d . . . H34A H 0.9888 0.4618 0.0469 0.079 Uiso 1 1 calc R . . H34B H 0.9896 0.5010 0.0893 0.079 Uiso 1 1 calc R . . H34C H 1.0071 0.5578 0.0525 0.079 Uiso 1 1 calc R . . C17 C 0.5076(2) 0.05218(18) 0.04677(11) 0.0535(9) Uani 1 1 d . . . H17A H 0.4841 -0.0009 0.0434 0.064 Uiso 1 1 calc R . . C49 C 0.2730(2) 0.3512(2) 0.05711(10) 0.0556(9) Uani 1 1 d . . . H49A H 0.2577 0.3385 0.0304 0.083 Uiso 1 1 calc R . . H49B H 0.2257 0.3751 0.0706 0.083 Uiso 1 1 calc R . . H49C H 0.2900 0.3006 0.0703 0.083 Uiso 1 1 calc R . . C16 C 0.46723(19) 0.10986(18) 0.06728(10) 0.0452(8) Uani 1 1 d . . . H16A H 0.4152 0.0968 0.0781 0.054 Uiso 1 1 calc R . . C46 C 0.2450(2) 0.5371(2) 0.21260(10) 0.0554(9) Uani 1 1 d . . . H46A H 0.2135 0.5796 0.2262 0.083 Uiso 1 1 calc R . . H46B H 0.2843 0.5118 0.2305 0.083 Uiso 1 1 calc R . . H46C H 0.2074 0.4950 0.2027 0.083 Uiso 1 1 calc R . . C28 C 0.8154(3) 0.3677(3) -0.09121(13) 0.0800(13) Uani 1 1 d . . . H28A H 0.8646 0.3501 -0.0771 0.120 Uiso 1 1 calc R . . H28B H 0.8309 0.4075 -0.1112 0.120 Uiso 1 1 calc R . . H28C H 0.7894 0.3198 -0.1033 0.120 Uiso 1 1 calc R . . O5 O 0.6646(3) 0.6450(3) -0.00760(18) 0.0458(13) Uiso 0.50 1 d P . . H5B H 0.669(3) 0.633(3) 0.0142(13) 0.072(13) Uiso 1 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 P1 0.0242(3) 0.0213(3) 0.0284(3) 0.0018(3) 0.0006(3) 0.0003(3) O2 0.0253(9) 0.0218(9) 0.0263(9) -0.0054(7) -0.0014(8) -0.0002(8) O1 0.0257(9) 0.0247(10) 0.0245(9) 0.0031(7) -0.0030(8) 0.0010(8) O3 0.0323(10) 0.0396(11) 0.0382(10) -0.0030(10) 0.0010(9) 0.0066(9) O4 0.0443(12) 0.0264(10) 0.0341(10) -0.0002(8) 0.0026(9) -0.0063(9) C11 0.0272(14) 0.0230(13) 0.0208(13) 0.0062(11) -0.0041(11) -0.0006(11) C36 0.0257(14) 0.0285(14) 0.0275(14) 0.0008(12) 0.0082(11) -0.0055(12) C7 0.0227(14) 0.0324(15) 0.0282(14) -0.0007(12) 0.0005(11) 0.0000(12) C37 0.0304(15) 0.0335(16) 0.0316(15) -0.0001(13) 0.0012(12) 0.0008(12) C12 0.0276(14) 0.0234(13) 0.0204(13) 0.0031(11) -0.0040(11) -0.0003(11) C14 0.0263(15) 0.0334(16) 0.0393(16) 0.0054(13) 0.0040(12) -0.0027(12) C8 0.0246(14) 0.0278(14) 0.0230(13) -0.0020(11) -0.0006(11) -0.0008(12) C10 0.0282(14) 0.0257(14) 0.0178(12) -0.0029(11) -0.0001(11) 0.0015(11) C13 0.0299(14) 0.0267(14) 0.0210(13) 0.0021(11) -0.0010(11) 0.0014(12) C45 0.0388(17) 0.0475(18) 0.0307(16) -0.0018(14) -0.0004(14) 0.0146(15) C26 0.0200(13) 0.0293(15) 0.0294(14) -0.0020(11) 0.0046(11) 0.0039(11) C21 0.0203(13) 0.0265(14) 0.0265(13) 0.0019(12) 0.0055(11) 0.0024(11) C24 0.0196(13) 0.0323(15) 0.0335(16) 0.0020(12) 0.0009(11) 0.0000(12) C41 0.0223(14) 0.0275(14) 0.0282(14) 0.0021(11) 0.0013(11) -0.0033(11) C6 0.0341(15) 0.0270(14) 0.0272(14) -0.0028(12) -0.0031(12) 0.0029(12) C9 0.0263(14) 0.0228(14) 0.0212(13) -0.0033(11) -0.0032(11) 0.0042(11) C48 0.0357(16) 0.0393(17) 0.0283(15) 0.0027(13) 0.0007(13) 0.0033(13) C22 0.0246(13) 0.0314(15) 0.0245(14) -0.0019(12) 0.0015(11) -0.0029(12) C15 0.0317(16) 0.0247(14) 0.0374(16) 0.0021(12) -0.0031(12) -0.0030(12) C2 0.0350(16) 0.0299(15) 0.0275(15) 0.0056(12) -0.0006(12) 0.0025(13) C19 0.0340(16) 0.0286(16) 0.0394(16) -0.0061(13) -0.0012(13) 0.0029(13) C40 0.0224(14) 0.0354(16) 0.0291(14) 0.0071(12) -0.0007(11) 0.0027(12) C4 0.0402(18) 0.0379(17) 0.0382(17) 0.0056(14) -0.0059(14) 0.0108(14) C25 0.0221(13) 0.0240(14) 0.0271(14) -0.0038(12) 0.0036(11) -0.0034(11) C20 0.0315(15) 0.0256(14) 0.0262(14) 0.0010(12) -0.0049(12) 0.0009(12) C42 0.0442(18) 0.0489(19) 0.0289(15) -0.0030(13) -0.0052(14) 0.0177(15) C23 0.0321(15) 0.0394(17) 0.0239(14) 0.0042(13) -0.0025(12) -0.0007(13) C33 0.0338(15) 0.0330(15) 0.0262(14) 0.0008(12) 0.0023(12) -0.0021(13) C38 0.0387(17) 0.0419(17) 0.0244(14) 0.0014(12) -0.0004(12) 0.0061(14) C1 0.0274(15) 0.0233(13) 0.0277(14) -0.0041(11) -0.0005(12) 0.0036(11) C29 0.054(2) 0.059(2) 0.063(2) -0.0016(19) -0.0193(18) -0.0202(18) C35 0.0457(18) 0.0442(18) 0.0298(16) -0.0061(14) 0.0010(14) -0.0010(15) C30 0.0392(17) 0.0326(16) 0.0349(15) 0.0092(13) -0.0055(13) -0.0069(14) C5 0.0300(16) 0.0353(16) 0.0426(17) -0.0021(14) 0.0018(13) 0.0096(13) C27 0.0559(19) 0.0359(17) 0.0316(16) -0.0016(13) -0.0032(15) -0.0113(15) C3 0.0499(19) 0.0331(16) 0.0310(15) 0.0066(13) -0.0051(14) 0.0046(14) C31 0.064(2) 0.052(2) 0.045(2) 0.0130(16) 0.0104(17) -0.0102(18) C50 0.0349(16) 0.063(2) 0.0257(14) -0.0008(15) -0.0008(13) 0.0033(15) C43 0.0416(19) 0.066(2) 0.056(2) -0.0059(18) -0.0161(17) 0.0132(17) C32 0.052(2) 0.0402(18) 0.056(2) 0.0163(16) -0.0099(17) -0.0027(16) C39 0.0276(14) 0.0339(16) 0.0308(14) 0.0047(12) 0.0043(12) 0.0041(12) C18 0.048(2) 0.0289(17) 0.064(2) -0.0120(16) 0.0018(17) 0.0020(15) C44 0.074(3) 0.053(2) 0.058(2) 0.0117(18) -0.016(2) 0.0137(19) C47 0.064(2) 0.0410(19) 0.056(2) -0.0048(17) 0.0069(18) 0.0146(17) C34 0.054(2) 0.068(2) 0.0365(17) -0.0051(17) -0.0103(16) 0.0143(18) C17 0.053(2) 0.0231(16) 0.085(3) -0.0110(17) -0.0049(19) -0.0103(15) C49 0.056(2) 0.059(2) 0.052(2) -0.0025(18) -0.0150(17) -0.0183(17) C16 0.0372(17) 0.0317(16) 0.067(2) -0.0008(16) 0.0020(16) -0.0087(15) C46 0.0462(19) 0.071(2) 0.049(2) -0.0043(18) 0.0151(17) 0.0077(18) C28 0.069(3) 0.085(3) 0.086(3) -0.053(3) -0.005(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 P1 O3 1.4901(19) . ? P1 O4 1.4959(19) . ? P1 O2 1.5831(18) . ? P1 O1 1.5883(18) . ? O2 C12 1.418(3) . ? O1 C9 1.406(3) . ? C11 C12 1.370(4) . ? C11 C20 1.437(4) . ? C11 C10 1.496(4) . ? C36 C41 1.400(4) . ? C36 C37 1.404(4) . ? C36 C13 1.509(4) . ? C7 C8 1.370(4) . ? C7 C6 1.419(4) . ? C37 C38 1.395(4) . ? C37 C42 1.517(4) . ? C12 C13 1.428(4) . ? C14 C13 1.359(4) . ? C14 C15 1.408(4) . ? C8 C9 1.410(3) . ? C8 C21 1.499(4) . ? C10 C9 1.373(3) . ? C10 C1 1.438(4) . ? C45 C39 1.527(4) . ? C45 C47 1.532(5) . ? C45 C46 1.533(4) . ? C26 C21 1.400(4) . ? C26 C25 1.401(4) . ? C26 C33 1.514(4) . ? C21 C22 1.409(4) . ? C24 C25 1.370(4) . ? C24 C23 1.399(4) . ? C24 C30 1.528(4) . ? C41 C40 1.395(4) . ? C41 C48 1.529(4) . ? C6 C1 1.412(4) . ? C6 C5 1.426(4) . ? C48 C49 1.531(4) . ? C48 C50 1.532(4) . ? C22 C23 1.388(4) . ? C22 C27 1.524(4) . ? C15 C16 1.420(4) . ? C15 C20 1.425(4) . ? C2 C3 1.369(4) . ? C2 C1 1.421(4) . ? C19 C18 1.358(4) . ? C19 C20 1.418(4) . ? C40 C39 1.388(4) . ? C4 C5 1.352(4) . ? C4 C3 1.401(4) . ? C42 C44 1.522(5) . ? C42 C43 1.522(4) . ? C33 C35 1.524(4) . ? C33 C34 1.537(4) . ? C38 C39 1.386(4) . ? C29 C27 1.523(4) . ? C30 C32 1.512(4) . ? C30 C31 1.525(4) . ? C27 C28 1.508(5) . ? C18 C17 1.404(5) . ? C17 C16 1.347(4) . ? O5 O5 0.693(9) 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 O3 P1 O4 117.25(11) . . ? O3 P1 O2 109.18(10) . . ? O4 P1 O2 107.04(10) . . ? O3 P1 O1 106.58(10) . . ? O4 P1 O1 111.27(10) . . ? O2 P1 O1 104.83(9) . . ? C12 O2 P1 114.89(15) . . ? C9 O1 P1 121.31(15) . . ? C12 C11 C20 118.0(2) . . ? C12 C11 C10 121.4(2) . . ? C20 C11 C10 120.6(2) . . ? C41 C36 C37 120.3(2) . . ? C41 C36 C13 121.0(2) . . ? C37 C36 C13 118.6(2) . . ? C8 C7 C6 122.3(2) . . ? C38 C37 C36 118.7(2) . . ? C38 C37 C42 118.3(2) . . ? C36 C37 C42 122.9(2) . . ? C11 C12 O2 118.5(2) . . ? C11 C12 C13 124.0(2) . . ? O2 C12 C13 117.5(2) . . ? C13 C14 C15 123.2(3) . . ? C7 C8 C9 116.9(2) . . ? C7 C8 C21 121.0(2) . . ? C9 C8 C21 122.0(2) . . ? C9 C10 C1 117.3(2) . . ? C9 C10 C11 120.3(2) . . ? C1 C10 C11 122.4(2) . . ? C14 C13 C12 116.4(2) . . ? C14 C13 C36 120.8(2) . . ? C12 C13 C36 122.7(2) . . ? C39 C45 C47 111.2(3) . . ? C39 C45 C46 110.9(3) . . ? C47 C45 C46 110.9(3) . . ? C21 C26 C25 117.5(2) . . ? C21 C26 C33 122.5(2) . . ? C25 C26 C33 119.9(2) . . ? C26 C21 C22 120.9(2) . . ? C26 C21 C8 119.0(2) . . ? C22 C21 C8 120.1(2) . . ? C25 C24 C23 118.2(2) . . ? C25 C24 C30 121.4(2) . . ? C23 C24 C30 120.4(2) . . ? C40 C41 C36 118.6(2) . . ? C40 C41 C48 118.4(2) . . ? C36 C41 C48 122.9(2) . . ? C1 C6 C7 119.0(2) . . ? C1 C6 C5 119.8(2) . . ? C7 C6 C5 121.2(3) . . ? C10 C9 O1 118.3(2) . . ? C10 C9 C8 124.6(2) . . ? O1 C9 C8 117.0(2) . . ? C41 C48 C49 110.8(2) . . ? C41 C48 C50 113.3(2) . . ? C49 C48 C50 109.5(2) . . ? C23 C22 C21 118.8(2) . . ? C23 C22 C27 119.4(2) . . ? C21 C22 C27 121.8(2) . . ? C14 C15 C16 122.6(3) . . ? C14 C15 C20 119.2(2) . . ? C16 C15 C20 118.2(3) . . ? C3 C2 C1 121.0(3) . . ? C18 C19 C20 120.8(3) . . ? C39 C40 C41 122.5(2) . . ? C5 C4 C3 119.9(3) . . ? C24 C25 C26 123.0(2) . . ? C19 C20 C15 118.4(2) . . ? C19 C20 C11 123.0(2) . . ? C15 C20 C11 118.6(2) . . ? C37 C42 C44 110.6(3) . . ? C37 C42 C43 112.2(2) . . ? C44 C42 C43 111.4(3) . . ? C22 C23 C24 121.5(2) . . ? C26 C33 C35 114.0(2) . . ? C26 C33 C34 111.5(2) . . ? C35 C33 C34 109.1(2) . . ? C39 C38 C37 122.3(2) . . ? C6 C1 C2 117.5(2) . . ? C6 C1 C10 119.6(2) . . ? C2 C1 C10 122.9(2) . . ? C32 C30 C31 111.3(3) . . ? C32 C30 C24 110.4(2) . . ? C31 C30 C24 113.2(2) . . ? C4 C5 C6 120.8(3) . . ? C28 C27 C29 110.8(3) . . ? C28 C27 C22 111.2(3) . . ? C29 C27 C22 111.8(3) . . ? C2 C3 C4 120.9(3) . . ? C38 C39 C40 117.6(2) . . ? C38 C39 C45 120.8(2) . . ? C40 C39 C45 121.7(2) . . ? C19 C18 C17 120.9(3) . . ? C16 C17 C18 119.8(3) . . ? C17 C16 C15 121.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O2 C12 60.58(18) . . . . ? O4 P1 O2 C12 -171.56(16) . . . . ? O1 P1 O2 C12 -53.29(18) . . . . ? O3 P1 O1 C9 -152.92(18) . . . . ? O4 P1 O1 C9 78.13(19) . . . . ? O2 P1 O1 C9 -37.23(19) . . . . ? C41 C36 C37 C38 -1.4(4) . . . . ? C13 C36 C37 C38 -178.2(2) . . . . ? C41 C36 C37 C42 175.8(2) . . . . ? C13 C36 C37 C42 -1.1(4) . . . . ? C20 C11 C12 O2 -175.9(2) . . . . ? C10 C11 C12 O2 2.7(3) . . . . ? C20 C11 C12 C13 5.5(4) . . . . ? C10 C11 C12 C13 -175.8(2) . . . . ? P1 O2 C12 C11 74.6(2) . . . . ? P1 O2 C12 C13 -106.8(2) . . . . ? C6 C7 C8 C9 -4.6(4) . . . . ? C6 C7 C8 C21 173.5(2) . . . . ? C12 C11 C10 C9 -51.2(3) . . . . ? C20 C11 C10 C9 127.4(3) . . . . ? C12 C11 C10 C1 128.3(3) . . . . ? C20 C11 C10 C1 -53.2(3) . . . . ? C15 C14 C13 C12 -5.1(4) . . . . ? C15 C14 C13 C36 178.3(2) . . . . ? C11 C12 C13 C14 1.1(4) . . . . ? O2 C12 C13 C14 -177.5(2) . . . . ? C11 C12 C13 C36 177.6(2) . . . . ? O2 C12 C13 C36 -1.0(3) . . . . ? C41 C36 C13 C14 -76.7(3) . . . . ? C37 C36 C13 C14 100.1(3) . . . . ? C41 C36 C13 C12 106.9(3) . . . . ? C37 C36 C13 C12 -76.3(3) . . . . ? C25 C26 C21 C22 1.7(4) . . . . ? C33 C26 C21 C22 -177.9(2) . . . . ? C25 C26 C21 C8 -179.8(2) . . . . ? C33 C26 C21 C8 0.5(4) . . . . ? C7 C8 C21 C26 -73.7(3) . . . . ? C9 C8 C21 C26 104.2(3) . . . . ? C7 C8 C21 C22 104.8(3) . . . . ? C9 C8 C21 C22 -77.3(3) . . . . ? C37 C36 C41 C40 0.5(4) . . . . ? C13 C36 C41 C40 177.2(2) . . . . ? C37 C36 C41 C48 -177.2(2) . . . . ? C13 C36 C41 C48 -0.4(4) . . . . ? C8 C7 C6 C1 2.1(4) . . . . ? C8 C7 C6 C5 -176.0(2) . . . . ? C1 C10 C9 O1 178.8(2) . . . . ? C11 C10 C9 O1 -1.7(3) . . . . ? C1 C10 C9 C8 2.4(4) . . . . ? C11 C10 C9 C8 -178.1(2) . . . . ? P1 O1 C9 C10 70.4(3) . . . . ? P1 O1 C9 C8 -112.9(2) . . . . ? C7 C8 C9 C10 2.3(4) . . . . ? C21 C8 C9 C10 -175.7(2) . . . . ? C7 C8 C9 O1 -174.1(2) . . . . ? C21 C8 C9 O1 7.9(3) . . . . ? C40 C41 C48 C49 -80.2(3) . . . . ? C36 C41 C48 C49 97.5(3) . . . . ? C40 C41 C48 C50 43.4(3) . . . . ? C36 C41 C48 C50 -138.9(3) . . . . ? C26 C21 C22 C23 -0.1(4) . . . . ? C8 C21 C22 C23 -178.5(2) . . . . ? C26 C21 C22 C27 178.1(2) . . . . ? C8 C21 C22 C27 -0.3(4) . . . . ? C13 C14 C15 C16 -176.5(3) . . . . ? C13 C14 C15 C20 2.3(4) . . . . ? C36 C41 C40 C39 0.8(4) . . . . ? C48 C41 C40 C39 178.6(2) . . . . ? C23 C24 C25 C26 2.9(4) . . . . ? C30 C24 C25 C26 -179.6(2) . . . . ? C21 C26 C25 C24 -3.2(4) . . . . ? C33 C26 C25 C24 176.5(2) . . . . ? C18 C19 C20 C15 -4.5(4) . . . . ? C18 C19 C20 C11 177.0(3) . . . . ? C14 C15 C20 C19 -174.0(3) . . . . ? C16 C15 C20 C19 4.9(4) . . . . ? C14 C15 C20 C11 4.5(4) . . . . ? C16 C15 C20 C11 -176.6(2) . . . . ? C12 C11 C20 C19 170.3(2) . . . . ? C10 C11 C20 C19 -8.4(4) . . . . ? C12 C11 C20 C15 -8.2(3) . . . . ? C10 C11 C20 C15 173.2(2) . . . . ? C38 C37 C42 C44 68.8(3) . . . . ? C36 C37 C42 C44 -108.4(3) . . . . ? C38 C37 C42 C43 -56.3(4) . . . . ? C36 C37 C42 C43 126.5(3) . . . . ? C21 C22 C23 C24 -0.3(4) . . . . ? C27 C22 C23 C24 -178.6(2) . . . . ? C25 C24 C23 C22 -1.0(4) . . . . ? C30 C24 C23 C22 -178.6(2) . . . . ? C21 C26 C33 C35 -136.0(3) . . . . ? C25 C26 C33 C35 44.3(3) . . . . ? C21 C26 C33 C34 99.9(3) . . . . ? C25 C26 C33 C34 -79.7(3) . . . . ? C36 C37 C38 C39 1.0(4) . . . . ? C42 C37 C38 C39 -176.3(3) . . . . ? C7 C6 C1 C2 -175.6(2) . . . . ? C5 C6 C1 C2 2.6(4) . . . . ? C7 C6 C1 C10 2.8(4) . . . . ? C5 C6 C1 C10 -179.1(2) . . . . ? C3 C2 C1 C6 -2.6(4) . . . . ? C3 C2 C1 C10 179.1(3) . . . . ? C9 C10 C1 C6 -4.9(3) . . . . ? C11 C10 C1 C6 175.6(2) . . . . ? C9 C10 C1 C2 173.4(2) . . . . ? C11 C10 C1 C2 -6.1(4) . . . . ? C25 C24 C30 C32 -100.1(3) . . . . ? C23 C24 C30 C32 77.4(3) . . . . ? C25 C24 C30 C31 134.3(3) . . . . ? C23 C24 C30 C31 -48.2(4) . . . . ? C3 C4 C5 C6 -2.3(4) . . . . ? C1 C6 C5 C4 -0.1(4) . . . . ? C7 C6 C5 C4 177.9(3) . . . . ? C23 C22 C27 C28 71.5(4) . . . . ? C21 C22 C27 C28 -106.7(3) . . . . ? C23 C22 C27 C29 -53.0(4) . . . . ? C21 C22 C27 C29 128.8(3) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C5 C4 C3 C2 2.4(4) . . . . ? C37 C38 C39 C40 0.3(4) . . . . ? C37 C38 C39 C45 -179.2(3) . . . . ? C41 C40 C39 C38 -1.2(4) . . . . ? C41 C40 C39 C45 178.3(3) . . . . ? C47 C45 C39 C38 57.8(4) . . . . ? C46 C45 C39 C38 -66.1(4) . . . . ? C47 C45 C39 C40 -121.7(3) . . . . ? C46 C45 C39 C40 114.3(3) . . . . ? C20 C19 C18 C17 1.6(5) . . . . ? C19 C18 C17 C16 1.0(5) . . . . ? C18 C17 C16 C15 -0.5(5) . . . . ? C14 C15 C16 C17 176.4(3) . . . . ? C20 C15 C16 C17 -2.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.174 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.042 # Attachment 'web_deposit_cif_file_1_RuepingMagnus_1278784359.cif' data_1e _database_code_depnum_ccdc_archive 'CCDC 783866' #TrackingRef 'web_deposit_cif_file_1_RuepingMagnus_1278784359.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48.50 H29 Cl O4 P Pd0.25' _chemical_formula_weight 768.78 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 25.774(9) _cell_length_b 17.105(4) _cell_length_c 22.731(7) _cell_angle_alpha 90.00 _cell_angle_beta 121.38(2) _cell_angle_gamma 90.00 _cell_volume 8555(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3379 _cell_measurement_theta_min 3.7 _cell_measurement_theta_max 23.2 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 0.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9531 _exptl_absorpt_correction_T_max 0.9893 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33275 _diffrn_reflns_av_R_equivalents 0.4581 _diffrn_reflns_av_sigmaI/netI 0.6674 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 25.81 _reflns_number_total 16128 _reflns_number_gt 2758 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.2000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.4(3) _refine_ls_number_reflns 16128 _refine_ls_number_parameters 308 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.4924 _refine_ls_R_factor_gt 0.2523 _refine_ls_wR_factor_ref 0.6271 _refine_ls_wR_factor_gt 0.4892 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 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 P1 P 0.4596(3) 0.3177(4) 0.3892(4) 0.041(2) Uani 1 1 d . . . O1 O 0.3872(8) 0.2980(9) 0.3566(9) 0.037(4) Uiso 1 1 d . . . O2 O 0.4680(8) 0.2909(9) 0.3263(9) 0.036(4) Uiso 1 1 d . . . O3 O 0.4976(8) 0.2628(9) 0.4466(9) 0.037(4) Uiso 1 1 d . . . O4 O 0.4674(7) 0.4033(8) 0.4082(8) 0.027(4) Uiso 1 1 d . . . C1 C 0.3615(9) 0.2295(12) 0.3153(12) 0.024(5) Uiso 1 1 d D . . C2 C 0.3531(9) 0.2322(12) 0.2525(13) 0.029(6) Uiso 1 1 d D . . C3 C 0.3237(7) 0.1567(8) 0.2127(9) 0.050(8) Uiso 1 1 d GD . . C4 C 0.3113(10) 0.1509(10) 0.1456(10) 0.062(9) Uiso 1 1 d GD . . H4 H 0.3217 0.1926 0.1260 0.074 Uiso 1 1 calc R . . C5 C 0.2838(11) 0.0840(13) 0.1071(8) 0.108(15) Uiso 1 1 d GD . . H5 H 0.2753 0.0800 0.0612 0.129 Uiso 1 1 calc R . . C6 C 0.2686(10) 0.0229(10) 0.1357(10) 0.061(9) Uiso 1 1 d GD . . H6 H 0.2498 -0.0228 0.1094 0.074 Uiso 1 1 calc R . . C7 C 0.2810(10) 0.0288(9) 0.2028(10) 0.085(12) Uiso 1 1 d GD . . H7 H 0.2706 -0.0130 0.2224 0.102 Uiso 1 1 calc R . . C8 C 0.3086(9) 0.0957(10) 0.2413(8) 0.034(6) Uiso 1 1 d GD . . C9 C 0.3256(12) 0.1004(15) 0.3114(14) 0.042(7) Uiso 1 1 d D . . H9 H 0.3231 0.0541 0.3328 0.050 Uiso 1 1 calc R . . C10 C 0.3457(12) 0.1680(15) 0.3509(14) 0.037(6) Uiso 1 1 d D . . C11 C 0.4306(17) 0.3134(16) 0.2562(18) 0.069(10) Uiso 1 1 d D . . C12 C 0.3696(16) 0.2978(14) 0.2286(16) 0.059(9) Uiso 1 1 d D . . C13 C 0.3272(9) 0.3383(8) 0.1603(8) 0.043(7) Uiso 1 1 d GD . . C14 C 0.2643(9) 0.3334(10) 0.1277(10) 0.055(8) Uiso 1 1 d GD . . H14 H 0.2464 0.3023 0.1471 0.066 Uiso 1 1 calc R . . C15 C 0.2276(8) 0.3739(12) 0.0666(11) 0.070(10) Uiso 1 1 d GD . . H15 H 0.1847 0.3705 0.0443 0.085 Uiso 1 1 calc R . . C16 C 0.2539(11) 0.4193(11) 0.0383(9) 0.083(12) Uiso 1 1 d GD . . H16 H 0.2288 0.4470 -0.0034 0.100 Uiso 1 1 calc R . . C17 C 0.3168(11) 0.4243(12) 0.0709(12) 0.087(12) Uiso 1 1 d GD . . H17 H 0.3347 0.4554 0.0515 0.104 Uiso 1 1 calc R . . C18 C 0.3534(8) 0.3838(11) 0.1320(11) 0.066(10) Uiso 1 1 d GD . . C19 C 0.4164(16) 0.3934(17) 0.1646(17) 0.060(9) Uiso 1 1 d D . . H19 H 0.4325 0.4206 0.1412 0.072 Uiso 1 1 calc R . . C20 C 0.4549(14) 0.3653(16) 0.2282(16) 0.047(7) Uiso 1 1 d D . . C21 C 0.3657(10) 0.1700(12) 0.4267(12) 0.026(5) Uiso 1 1 d D . . C22 C 0.3321(6) 0.2328(7) 0.4447(9) 0.048(7) Uiso 1 1 d GD . . C23 C 0.2870(7) 0.2836(8) 0.3987(7) 0.022(5) Uiso 1 1 d GD . . H23 H 0.2746 0.2828 0.3514 0.027 Uiso 1 1 calc R . . C24 C 0.2601(7) 0.3355(8) 0.4220(9) 0.059(9) Uiso 1 1 d GD . . H24 H 0.2293 0.3701 0.3906 0.070 Uiso 1 1 calc R . . C25 C 0.2783(9) 0.3366(9) 0.4913(10) 0.068(10) Uiso 1 1 d GD . . H25 H 0.2599 0.3721 0.5072 0.081 Uiso 1 1 calc R . . C26 C 0.3234(9) 0.2859(11) 0.5373(7) 0.059(9) Uiso 1 1 d GD . . H26 H 0.3358 0.2866 0.5847 0.071 Uiso 1 1 calc R . . C27 C 0.3503(6) 0.2340(8) 0.5140(8) 0.040(7) Uiso 1 1 d GD . . C28 C 0.4005(7) 0.1781(10) 0.5681(9) 0.038(6) Uiso 1 1 d GD . . C29 C 0.4218(9) 0.1785(10) 0.6383(9) 0.045(7) Uiso 1 1 d GD . . H29 H 0.4039 0.2123 0.6560 0.054 Uiso 1 1 calc R . . C30 C 0.4692(10) 0.1293(13) 0.6825(8) 0.073(10) Uiso 1 1 d GD . . H30 H 0.4838 0.1296 0.7304 0.088 Uiso 1 1 calc R . . C31 C 0.4954(9) 0.0798(12) 0.6566(11) 0.085(12) Uiso 1 1 d GD . . H31 H 0.5278 0.0462 0.6868 0.102 Uiso 1 1 calc R . . C32 C 0.4741(10) 0.0795(11) 0.5864(12) 0.092(13) Uiso 1 1 d GD . . H32 H 0.4919 0.0456 0.5687 0.110 Uiso 1 1 calc R . . C33 C 0.4266(10) 0.1286(12) 0.5422(8) 0.058(9) Uiso 1 1 d GD . . C34 C 0.4027(11) 0.1259(13) 0.4724(13) 0.029(6) Uiso 1 1 d D . . H34 H 0.4166 0.0838 0.4569 0.034 Uiso 1 1 calc R . . C41 C 0.5225(13) 0.3813(13) 0.2625(13) 0.037(7) Uiso 1 1 d D . . C42 C 0.5617(14) 0.3483(12) 0.2474(12) 0.070(10) Uiso 1 1 d GD . . C43 C 0.5323(11) 0.2902(15) 0.1982(13) 0.119(17) Uiso 1 1 d GD . . H43 H 0.4905 0.2794 0.1807 0.142 Uiso 1 1 calc R . . C44 C 0.5638(17) 0.2478(13) 0.1745(12) 0.129(19) Uiso 1 1 d GD . . H44 H 0.5437 0.2081 0.1408 0.155 Uiso 1 1 calc R . . C45 C 0.6248(17) 0.2635(17) 0.2001(17) 0.116(16) Uiso 1 1 d GD . . H45 H 0.6464 0.2346 0.1839 0.139 Uiso 1 1 calc R . . C46 C 0.6543(11) 0.3216(19) 0.2493(16) 0.18(3) Uiso 1 1 d GD . . H46 H 0.6960 0.3324 0.2668 0.215 Uiso 1 1 calc R . . C47 C 0.6228(14) 0.3640(12) 0.2730(10) 0.098(14) Uiso 1 1 d GD . . C48 C 0.6509(11) 0.4280(10) 0.3268(10) 0.062(9) Uiso 1 1 d GD . . C49 C 0.7116(10) 0.4492(12) 0.3573(12) 0.090(13) Uiso 1 1 d GD . . H49 H 0.7370 0.4233 0.3447 0.108 Uiso 1 1 calc R . . C50 C 0.7352(8) 0.5085(13) 0.4063(12) 0.071(10) Uiso 1 1 d GD . . H50 H 0.7767 0.5230 0.4272 0.086 Uiso 1 1 calc R . . C51 C 0.6981(10) 0.5465(11) 0.4248(10) 0.074(11) Uiso 1 1 d GD . . H51 H 0.7143 0.5869 0.4583 0.088 Uiso 1 1 calc R . . C52 C 0.6374(10) 0.5252(11) 0.3943(11) 0.060(9) Uiso 1 1 d GD . . H52 H 0.6120 0.5512 0.4069 0.072 Uiso 1 1 calc R . . C53 C 0.6138(8) 0.4660(12) 0.3453(11) 0.065(10) Uiso 1 1 d GD . . C54 C 0.5489(13) 0.4377(13) 0.3149(13) 0.037(7) Uiso 1 1 d D . . H54 H 0.5252 0.4591 0.3320 0.045 Uiso 1 1 calc R . . P1A P 0.5070(4) 0.6693(4) 0.4096(5) 0.051(2) Uani 1 1 d . . . O1A O 0.5787(8) 0.6865(8) 0.4343(8) 0.031(4) Uiso 1 1 d . . . O2A O 0.4699(8) 0.6889(9) 0.3274(9) 0.032(4) Uiso 1 1 d . . . O3A O 0.4824(9) 0.7300(10) 0.4426(10) 0.046(5) Uiso 1 1 d . . . O4A O 0.4985(9) 0.5839(10) 0.4210(10) 0.049(5) Uiso 1 1 d . . . C1A C 0.5939(10) 0.7598(14) 0.4133(15) 0.038(7) Uiso 1 1 d D . . C2A C 0.5766(11) 0.7618(17) 0.3463(18) 0.058(9) Uiso 1 1 d D . . C3A C 0.5888(7) 0.8417(7) 0.3270(9) 0.051(8) Uiso 1 1 d GD . . C4A C 0.5705(9) 0.8527(10) 0.2583(8) 0.064(9) Uiso 1 1 d GD . . H4A H 0.5512 0.8114 0.2261 0.077 Uiso 1 1 calc R . . C5A C 0.5806(10) 0.9241(12) 0.2366(7) 0.062(9) Uiso 1 1 d GD . . H5A H 0.5681 0.9316 0.1897 0.075 Uiso 1 1 calc R . . C6A C 0.6089(10) 0.9845(9) 0.2837(10) 0.081(11) Uiso 1 1 d GD . . H6A H 0.6157 1.0333 0.2690 0.098 Uiso 1 1 calc R . . C7A C 0.6271(9) 0.9735(8) 0.3525(9) 0.068(10) Uiso 1 1 d GD . . H7A H 0.6465 1.0147 0.3847 0.082 Uiso 1 1 calc R . . C8A C 0.6171(7) 0.9021(9) 0.3741(7) 0.019(5) Uiso 1 1 d GD . . C9A C 0.6258(10) 0.8898(12) 0.4318(12) 0.025(5) Uiso 1 1 d D . . H9A H 0.6410 0.9342 0.4610 0.030 Uiso 1 1 calc R . . C10A C 0.6180(14) 0.8238(18) 0.4645(17) 0.055(8) Uiso 1 1 d D . . C11A C 0.4876(15) 0.6742(16) 0.2837(15) 0.059(9) Uiso 1 1 d D . . C12A C 0.5495(14) 0.6959(13) 0.2991(14) 0.052(8) Uiso 1 1 d D . . C13A C 0.5748(9) 0.6623(10) 0.2618(9) 0.053(8) Uiso 1 1 d GD . . C14A C 0.6338(9) 0.6804(10) 0.2797(9) 0.068(10) Uiso 1 1 d GD . . H14A H 0.6571 0.7166 0.3158 0.081 Uiso 1 1 calc R . . C15A C 0.6588(8) 0.6457(12) 0.2447(12) 0.065(10) Uiso 1 1 d GD . . H15A H 0.6992 0.6581 0.2570 0.078 Uiso 1 1 calc R . . C16A C 0.6248(11) 0.5929(12) 0.1919(11) 0.100(14) Uiso 1 1 d GD . . H16A H 0.6419 0.5692 0.1680 0.120 Uiso 1 1 calc R . . C17A C 0.5658(10) 0.5747(11) 0.1740(10) 0.065(9) Uiso 1 1 d GD . . H17A H 0.5425 0.5386 0.1379 0.078 Uiso 1 1 calc R . . C18A C 0.5408(8) 0.6094(11) 0.2090(11) 0.069(10) Uiso 1 1 d GD . . C19A C 0.4779(15) 0.5916(16) 0.1949(17) 0.054(8) Uiso 1 1 d D . . H19A H 0.4537 0.5582 0.1568 0.065 Uiso 1 1 calc R . . C20A C 0.452(2) 0.617(2) 0.229(2) 0.095(14) Uiso 1 1 d D . . C21A C 0.6324(10) 0.8084(11) 0.5337(12) 0.025(5) Uiso 1 1 d D . . C22A C 0.6754(7) 0.7507(9) 0.5872(12) 0.074(11) Uiso 1 1 d GD . . C23A C 0.7041(11) 0.7027(13) 0.5635(10) 0.061(9) Uiso 1 1 d GD . . H23A H 0.6962 0.7089 0.5180 0.073 Uiso 1 1 calc R . . C24A C 0.7446(10) 0.6456(11) 0.6064(14) 0.15(2) Uiso 1 1 d GD . . H24A H 0.7643 0.6128 0.5901 0.175 Uiso 1 1 calc R . . C25A C 0.7562(10) 0.6365(12) 0.6730(13) 0.080(11) Uiso 1 1 d GD . . H25A H 0.7839 0.5975 0.7022 0.096 Uiso 1 1 calc R . . C26A C 0.7275(12) 0.6845(15) 0.6967(10) 0.092(13) Uiso 1 1 d GD . . H26A H 0.7354 0.6783 0.7422 0.110 Uiso 1 1 calc R . . C27A C 0.6870(9) 0.7416(11) 0.6538(14) 0.108(15) Uiso 1 1 d GD . . C28A C 0.6578(10) 0.7970(12) 0.6795(12) 0.055(8) Uiso 1 1 d GD . . C29A C 0.6678(10) 0.7885(12) 0.7455(11) 0.070(10) Uiso 1 1 d GD . . H29A H 0.6958 0.7505 0.7759 0.084 Uiso 1 1 calc R . . C30A C 0.6368(13) 0.8358(15) 0.7669(11) 0.079(11) Uiso 1 1 d GD . . H30A H 0.6437 0.8300 0.8120 0.094 Uiso 1 1 calc R . . C31A C 0.5958(13) 0.8914(14) 0.7224(16) 0.15(2) Uiso 1 1 d GD . . H31A H 0.5747 0.9237 0.7371 0.183 Uiso 1 1 calc R . . C32A C 0.5858(11) 0.8998(13) 0.6564(15) 0.117(17) Uiso 1 1 d GD . . H32A H 0.5578 0.9379 0.6260 0.140 Uiso 1 1 calc R . . C33A C 0.6168(12) 0.8526(14) 0.6350(10) 0.083(12) Uiso 1 1 d GD . . C34A C 0.6093(14) 0.8513(16) 0.5628(16) 0.050(8) Uiso 1 1 d D . . H34A H 0.5819 0.8901 0.5327 0.060 Uiso 1 1 calc R . . C41A C 0.3890(13) 0.5967(13) 0.2108(13) 0.039(7) Uiso 1 1 d D . . C42A C 0.3423(10) 0.6350(11) 0.1524(9) 0.081(12) Uiso 1 1 d GD . . C43A C 0.3516(9) 0.6897(13) 0.1136(13) 0.075(11) Uiso 1 1 d GD . . H43A H 0.3918 0.7023 0.1252 0.090 Uiso 1 1 calc R . . C44A C 0.3022(13) 0.7258(10) 0.0577(12) 0.115(16) Uiso 1 1 d GD . . H44A H 0.3086 0.7631 0.0311 0.139 Uiso 1 1 calc R . . C45A C 0.2435(11) 0.7073(11) 0.0406(10) 0.077(11) Uiso 1 1 d GD . . H45A H 0.2097 0.7319 0.0024 0.092 Uiso 1 1 calc R . . C46A C 0.2341(9) 0.6526(12) 0.0794(12) 0.059(9) Uiso 1 1 d GD . . H46A H 0.1940 0.6400 0.0678 0.071 Uiso 1 1 calc R . . C47A C 0.2835(12) 0.6165(8) 0.1353(10) 0.070(10) Uiso 1 1 d GD . . C48A C 0.2722(10) 0.5524(9) 0.1772(10) 0.056(8) Uiso 1 1 d GD . . C49A C 0.2138(8) 0.5301(11) 0.1586(9) 0.060(9) Uiso 1 1 d GD . . H49A H 0.1797 0.5523 0.1191 0.072 Uiso 1 1 calc R . . C50A C 0.2052(8) 0.4753(12) 0.1980(12) 0.072(11) Uiso 1 1 d GD . . H50A H 0.1653 0.4601 0.1853 0.087 Uiso 1 1 calc R . . C51A C 0.2551(11) 0.4429(11) 0.2559(11) 0.069(10) Uiso 1 1 d GD . . H51A H 0.2493 0.4055 0.2828 0.082 Uiso 1 1 calc R . . C52A C 0.3136(9) 0.4652(11) 0.2745(9) 0.103(15) Uiso 1 1 d GD . . H52A H 0.3477 0.4430 0.3141 0.124 Uiso 1 1 calc R . . C53A C 0.3221(7) 0.5200(11) 0.2351(11) 0.035(6) Uiso 1 1 d GD . . C54A C 0.3804(14) 0.5458(14) 0.2489(15) 0.041(7) Uiso 1 1 d D . . H54A H 0.4154 0.5250 0.2883 0.049 Uiso 1 1 calc R . . Pd1 Pd 0.5000 0.4942(5) 0.5000 0.218(5) Uani 1 2 d S . . C1L C 0.917(2) 0.500(3) 0.136(3) 0.121(16) Uiso 1 1 d . . . H1L1 H 0.9488 0.4955 0.1849 0.145 Uiso 1 1 calc R . . H1L2 H 0.8777 0.5057 0.1339 0.145 Uiso 1 1 calc R . . Cl11 Cl 0.9301(12) 0.5922(14) 0.1031(13) 0.212(9) Uiso 1 1 d . . . Cl12 Cl 0.9142(9) 0.4220(11) 0.1026(10) 0.164(7) Uiso 1 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 P1 0.024(4) 0.029(3) 0.061(5) -0.011(3) 0.016(4) -0.013(3) P1A 0.062(6) 0.024(3) 0.088(7) 0.005(4) 0.053(5) -0.013(4) Pd1 0.143(8) 0.130(5) 0.393(16) 0.000 0.148(10) 0.000 _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 P1 O3 1.488(19) . ? P1 O4 1.510(16) . ? P1 O2 1.620(19) . ? P1 O1 1.64(2) . ? O1 C1 1.43(3) . ? O2 C11 1.42(4) . ? O4 Pd1 2.376(16) . ? C1 C2 1.33(3) . ? C1 C10 1.51(3) . ? C2 C12 1.41(4) . ? C2 C3 1.53(3) . ? C3 C4 1.3900 . ? C3 C8 1.3900 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 C7 1.3900 . ? C6 H6 0.9500 . ? C7 C8 1.3900 . ? C7 H7 0.9500 . ? C8 C9 1.42(3) . ? C9 C10 1.39(4) . ? C9 H9 0.9500 . ? C10 C21 1.52(4) . ? C11 C12 1.38(5) . ? C11 C20 1.41(4) . ? C12 C13 1.52(4) . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9500 . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 H16 0.9500 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 C19 1.40(4) . ? C19 C20 1.35(4) . ? C19 H19 0.9500 . ? C20 C41 1.52(4) . ? C21 C34 1.24(3) . ? C21 C22 1.56(3) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 C25 1.3900 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 C27 1.3900 . ? C26 H26 0.9500 . ? C27 C28 1.562(19) . ? C28 C29 1.3900 . ? C28 C33 1.3900 . ? C29 C30 1.3900 . ? C29 H29 0.9500 . ? C30 C31 1.3900 . ? C30 H30 0.9500 . ? C31 C32 1.3900 . ? C31 H31 0.9500 . ? C32 C33 1.3900 . ? C32 H32 0.9500 . ? C33 C34 1.37(3) . ? C34 H34 0.9500 . ? C41 C42 1.35(4) . ? C41 C54 1.40(3) . ? C42 C43 1.3900 . ? C42 C47 1.3900 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 C47 1.3900 . ? C46 H46 0.9500 . ? C47 C48 1.52(3) . ? C48 C49 1.3900 . ? C48 C53 1.3900 . ? C49 C50 1.3900 . ? C49 H49 0.9500 . ? C50 C51 1.3900 . ? C50 H50 0.9500 . ? C51 C52 1.3900 . ? C51 H51 0.9500 . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.52(3) . ? C54 H54 0.9500 . ? P1A O4A 1.518(19) . ? P1A O3A 1.59(2) . ? P1A O2A 1.631(19) . ? P1A O1A 1.654(19) . ? O1A C1A 1.47(3) . ? O2A C11A 1.31(4) . ? O4A Pd1 2.35(2) . ? C1A C2A 1.35(4) . ? C1A C10A 1.48(4) . ? C2A C12A 1.46(4) . ? C2A C3A 1.52(3) . ? C3A C4A 1.3900 . ? C3A C8A 1.3900 . ? C4A C5A 1.3900 . ? C4A H4A 0.9500 . ? C5A C6A 1.3900 . ? C5A H5A 0.9500 . ? C6A C7A 1.3900 . ? C6A H6A 0.9500 . ? C7A C8A 1.3900 . ? C7A H7A 0.9500 . ? C8A C9A 1.23(3) . ? C9A C10A 1.42(4) . ? C9A H9A 0.9500 . ? C10A C21A 1.44(4) . ? C11A C20A 1.47(5) . ? C11A C12A 1.49(5) . ? C12A C13A 1.43(4) . ? C13A C14A 1.3900 . ? C13A C18A 1.3900 . ? C14A C15A 1.3900 . ? C14A H14A 0.9500 . ? C15A C16A 1.3900 . ? C15A H15A 0.9500 . ? C16A C17A 1.3900 . ? C16A H16A 0.9500 . ? C17A C18A 1.3900 . ? C17A H17A 0.9500 . ? C18A C19A 1.51(4) . ? C19A C20A 1.34(5) . ? C19A H19A 0.9500 . ? C20A C41A 1.48(5) . ? C21A C34A 1.32(4) . ? C21A C22A 1.51(3) . ? C22A C23A 1.3900 . ? C22A C27A 1.3900 . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A C28A 1.50(3) . ? C28A C29A 1.3900 . ? C28A C33A 1.3900 . ? C29A C30A 1.3900 . ? C29A H29A 0.9500 . ? C30A C31A 1.3900 . ? C30A H30A 0.9500 . ? C31A C32A 1.3900 . ? C31A H31A 0.9500 . ? C32A C33A 1.3900 . ? C32A H32A 0.9500 . ? C33A C34A 1.55(4) . ? C34A H34A 0.9500 . ? C41A C54A 1.33(4) . ? C41A C42A 1.41(3) . ? C42A C43A 1.3900 . ? C42A C47A 1.3900 . ? C43A C44A 1.3900 . ? C43A H43A 0.9500 . ? C44A C45A 1.3900 . ? C44A H44A 0.9500 . ? C45A C46A 1.3900 . ? C45A H45A 0.9500 . ? C46A C47A 1.3900 . ? C46A H46A 0.9500 . ? C47A C48A 1.57(2) . ? C48A C49A 1.3900 . ? C48A C53A 1.3900 . ? C49A C50A 1.3900 . ? C49A H49A 0.9500 . ? C50A C51A 1.3900 . ? C50A H50A 0.9500 . ? C51A C52A 1.3900 . ? C51A H51A 0.9500 . ? C52A C53A 1.3900 . ? C52A H52A 0.9500 . ? C53A C54A 1.44(3) . ? C54A H54A 0.9500 . ? Pd1 O4A 2.35(2) 2_656 ? Pd1 O4 2.376(16) 2_656 ? C1L Cl12 1.51(5) . ? C1L Cl11 1.85(5) . ? C1L H1L1 0.9900 . ? C1L H1L2 0.9900 . ? 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 O3 P1 O4 115.6(10) . . ? O3 P1 O2 105.5(10) . . ? O4 P1 O2 117.9(10) . . ? O3 P1 O1 109.9(10) . . ? O4 P1 O1 106.2(9) . . ? O2 P1 O1 100.7(10) . . ? C1 O1 P1 119.4(14) . . ? C11 O2 P1 126.1(16) . . ? P1 O4 Pd1 145.0(10) . . ? C2 C1 O1 116(2) . . ? C2 C1 C10 132(2) . . ? O1 C1 C10 112(2) . . ? C1 C2 C12 122(2) . . ? C1 C2 C3 111(2) . . ? C12 C2 C3 127(2) . . ? C4 C3 C8 120.0 . . ? C4 C3 C2 118.0(16) . . ? C8 C3 C2 122.0(16) . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C3 120.0 . . ? C7 C8 C9 120.9(17) . . ? C3 C8 C9 119.0(17) . . ? C10 C9 C8 125(2) . . ? C10 C9 H9 117.7 . . ? C8 C9 H9 117.7 . . ? C9 C10 C1 110(2) . . ? C9 C10 C21 123(2) . . ? C1 C10 C21 125(2) . . ? C12 C11 C20 126(3) . . ? C12 C11 O2 114(3) . . ? C20 C11 O2 118(3) . . ? C11 C12 C2 119(3) . . ? C11 C12 C13 115(3) . . ? C2 C12 C13 124(3) . . ? C14 C13 C18 120.0 . . ? C14 C13 C12 122.4(19) . . ? C18 C13 C12 117.6(19) . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 C19 118(2) . . ? C13 C18 C19 122(2) . . ? C20 C19 C18 122(3) . . ? C20 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C19 C20 C11 117(3) . . ? C19 C20 C41 120(3) . . ? C11 C20 C41 123(3) . . ? C34 C21 C10 127(2) . . ? C34 C21 C22 119(2) . . ? C10 C21 C22 114.0(19) . . ? C23 C22 C27 120.0 . . ? C23 C22 C21 126.4(14) . . ? C27 C22 C21 113.6(14) . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C22 120.0 . . ? C26 C27 C28 117.6(13) . . ? C22 C27 C28 122.4(13) . . ? C29 C28 C33 120.0 . . ? C29 C28 C27 124.8(14) . . ? C33 C28 C27 115.1(14) . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.8(18) . . ? C34 C33 C28 119.1(18) . . ? C32 C33 C28 120.0 . . ? C21 C34 C33 130(3) . . ? C21 C34 H34 115.2 . . ? C33 C34 H34 115.2 . . ? C42 C41 C54 114(3) . . ? C42 C41 C20 127(3) . . ? C54 C41 C20 119(2) . . ? C41 C42 C43 110(3) . . ? C41 C42 C47 130(3) . . ? C43 C42 C47 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C42 120.0 . . ? C46 C47 C48 124(3) . . ? C42 C47 C48 116(2) . . ? C49 C48 C53 120.0 . . ? C49 C48 C47 122(2) . . ? C53 C48 C47 118(2) . . ? C48 C49 C50 120.0 . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C51 C50 C49 120.0 . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C52 120.0 . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C48 120.0 . . ? C52 C53 C54 121.0(18) . . ? C48 C53 C54 118.8(18) . . ? C41 C54 C53 123(3) . . ? C41 C54 H54 118.7 . . ? C53 C54 H54 118.7 . . ? O4A P1A O3A 114.8(12) . . ? O4A P1A O2A 110.0(10) . . ? O3A P1A O2A 105.5(10) . . ? O4A P1A O1A 110.4(10) . . ? O3A P1A O1A 111.8(10) . . ? O2A P1A O1A 103.7(10) . . ? C1A O1A P1A 118.9(13) . . ? C11A O2A P1A 126.9(17) . . ? P1A O4A Pd1 144.4(12) . . ? C2A C1A O1A 114(2) . . ? C2A C1A C10A 129(3) . . ? O1A C1A C10A 117(2) . . ? C1A C2A C12A 124(3) . . ? C1A C2A C3A 111(2) . . ? C12A C2A C3A 125(3) . . ? C4A C3A C8A 120.0 . . ? C4A C3A C2A 116.5(17) . . ? C8A C3A C2A 123.5(17) . . ? C5A C4A C3A 120.0 . . ? C5A C4A H4A 120.0 . . ? C3A C4A H4A 120.0 . . ? C6A C5A C4A 120.0 . . ? C6A C5A H5A 120.0 . . ? C4A C5A H5A 120.0 . . ? C7A C6A C5A 120.0 . . ? C7A C6A H6A 120.0 . . ? C5A C6A H6A 120.0 . . ? C6A C7A C8A 120.0 . . ? C6A C7A H7A 120.0 . . ? C8A C7A H7A 120.0 . . ? C9A C8A C7A 124.3(16) . . ? C9A C8A C3A 115.2(16) . . ? C7A C8A C3A 120.0 . . ? C8A C9A C10A 134(2) . . ? C8A C9A H9A 112.9 . . ? C10A C9A H9A 112.9 . . ? C9A C10A C21A 134(3) . . ? C9A C10A C1A 107(3) . . ? C21A C10A C1A 119(2) . . ? O2A C11A C20A 117(3) . . ? O2A C11A C12A 122(3) . . ? C20A C11A C12A 120(3) . . ? C13A C12A C2A 124(3) . . ? C13A C12A C11A 122(3) . . ? C2A C12A C11A 114(3) . . ? C14A C13A C18A 120.0 . . ? C14A C13A C12A 120.3(19) . . ? C18A C13A C12A 120(2) . . ? C13A C14A C15A 120.0 . . ? C13A C14A H14A 120.0 . . ? C15A C14A H14A 120.0 . . ? C16A C15A C14A 120.0 . . ? C16A C15A H15A 120.0 . . ? C14A C15A H15A 120.0 . . ? C17A C16A C15A 120.0 . . ? C17A C16A H16A 120.0 . . ? C15A C16A H16A 120.0 . . ? C18A C17A C16A 120.0 . . ? C18A C17A H17A 120.0 . . ? C16A C17A H17A 120.0 . . ? C17A C18A C13A 120.0 . . ? C17A C18A C19A 123.9(19) . . ? C13A C18A C19A 116.0(19) . . ? C20A C19A C18A 128(3) . . ? C20A C19A H19A 115.8 . . ? C18A C19A H19A 115.8 . . ? C19A C20A C11A 115(4) . . ? C19A C20A C41A 124(4) . . ? C11A C20A C41A 121(4) . . ? C34A C21A C10A 121(2) . . ? C34A C21A C22A 107(2) . . ? C10A C21A C22A 132(2) . . ? C23A C22A C27A 120.0 . . ? C23A C22A C21A 113(2) . . ? C27A C22A C21A 127(2) . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26A 120.0 . . ? C25A C26A H26A 120.0 . . ? C26A C27A C22A 120.0 . . ? C26A C27A C28A 121(2) . . ? C22A C27A C28A 119(2) . . ? C29A C28A C33A 120.0 . . ? C29A C28A C27A 120.3(19) . . ? C33A C28A C27A 120(2) . . ? C28A C29A C30A 120.0 . . ? C28A C29A H29A 120.0 . . ? C30A C29A H29A 120.0 . . ? C29A C30A C31A 120.0 . . ? C29A C30A H30A 120.0 . . ? C31A C30A H30A 120.0 . . ? C32A C31A C30A 120.0 . . ? C32A C31A H31A 120.0 . . ? C30A C31A H31A 120.0 . . ? C33A C32A C31A 120.0 . . ? C33A C32A H32A 120.0 . . ? C31A C32A H32A 120.0 . . ? C32A C33A C28A 120.0 . . ? C32A C33A C34A 127(2) . . ? C28A C33A C34A 113(2) . . ? C21A C34A C33A 134(3) . . ? C21A C34A H34A 112.8 . . ? C33A C34A H34A 112.8 . . ? C54A C41A C42A 125(3) . . ? C54A C41A C20A 120(3) . . ? C42A C41A C20A 115(3) . . ? C43A C42A C47A 120.0 . . ? C43A C42A C41A 125(2) . . ? C47A C42A C41A 115(2) . . ? C44A C43A C42A 120.0 . . ? C44A C43A H43A 120.0 . . ? C42A C43A H43A 120.0 . . ? C43A C44A C45A 120.0 . . ? C43A C44A H44A 120.0 . . ? C45A C44A H44A 120.0 . . ? C46A C45A C44A 120.0 . . ? C46A C45A H45A 120.0 . . ? C44A C45A H45A 120.0 . . ? C45A C46A C47A 120.0 . . ? C45A C46A H46A 120.0 . . ? C47A C46A H46A 120.0 . . ? C46A C47A C42A 120.0 . . ? C46A C47A C48A 119.5(17) . . ? C42A C47A C48A 120.5(17) . . ? C49A C48A C53A 120.0 . . ? C49A C48A C47A 121.3(16) . . ? C53A C48A C47A 118.6(16) . . ? C48A C49A C50A 120.0 . . ? C48A C49A H49A 120.0 . . ? C50A C49A H49A 120.0 . . ? C51A C50A C49A 120.0 . . ? C51A C50A H50A 120.0 . . ? C49A C50A H50A 120.0 . . ? C50A C51A C52A 120.0 . . ? C50A C51A H51A 120.0 . . ? C52A C51A H51A 120.0 . . ? C53A C52A C51A 120.0 . . ? C53A C52A H52A 120.0 . . ? C51A C52A H52A 120.0 . . ? C52A C53A C48A 120.0 . . ? C52A C53A C54A 124.4(18) . . ? C48A C53A C54A 115.6(18) . . ? C41A C54A C53A 125(3) . . ? C41A C54A H54A 117.6 . . ? C53A C54A H54A 117.6 . . ? O4A Pd1 O4A 98.3(10) 2_656 . ? O4A Pd1 O4 84.2(6) 2_656 2_656 ? O4A Pd1 O4 163.1(6) . 2_656 ? O4A Pd1 O4 163.1(6) 2_656 . ? O4A Pd1 O4 84.2(6) . . ? O4 Pd1 O4 98.3(8) 2_656 . ? Cl12 C1L Cl11 121(3) . . ? Cl12 C1L H1L1 107.0 . . ? Cl11 C1L H1L1 107.0 . . ? Cl12 C1L H1L2 107.0 . . ? Cl11 C1L H1L2 107.0 . . ? H1L1 C1L H1L2 106.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 C1 -73.0(19) . . . . ? O4 P1 O1 C1 161.3(16) . . . . ? O2 P1 O1 C1 37.9(18) . . . . ? O3 P1 O2 C11 165(2) . . . . ? O4 P1 O2 C11 -65(2) . . . . ? O1 P1 O2 C11 50(2) . . . . ? O3 P1 O4 Pd1 -22(2) . . . . ? O2 P1 O4 Pd1 -147.5(16) . . . . ? O1 P1 O4 Pd1 100.6(18) . . . . ? P1 O1 C1 C2 -73.2(17) . . . . ? P1 O1 C1 C10 109.9(17) . . . . ? O1 C1 C2 C12 1(2) . . . . ? C10 C1 C2 C12 178(3) . . . . ? O1 C1 C2 C3 -178.3(14) . . . . ? C10 C1 C2 C3 -2.1(17) . . . . ? C1 C2 C3 C4 179.3(9) . . . . ? C12 C2 C3 C4 0(2) . . . . ? C1 C2 C3 C8 0.4(10) . . . . ? C12 C2 C3 C8 -179(2) . . . . ? C8 C3 C4 C5 0.0 . . . . ? C2 C3 C4 C5 -178.9(7) . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C8 0.0 . . . . ? C6 C7 C8 C3 0.0 . . . . ? C6 C7 C8 C9 -175.3(19) . . . . ? C4 C3 C8 C7 0.0 . . . . ? C2 C3 C8 C7 178.9(8) . . . . ? C4 C3 C8 C9 175.4(18) . . . . ? C2 C3 C8 C9 -5.7(19) . . . . ? C7 C8 C9 C10 -171(2) . . . . ? C3 C8 C9 C10 14(3) . . . . ? C8 C9 C10 C1 -14(3) . . . . ? C8 C9 C10 C21 -178(2) . . . . ? C2 C1 C10 C9 8(3) . . . . ? O1 C1 C10 C9 -175.2(19) . . . . ? C2 C1 C10 C21 172.1(19) . . . . ? O1 C1 C10 C21 -12(3) . . . . ? P1 O2 C11 C12 -55(2) . . . . ? P1 O2 C11 C20 109(3) . . . . ? C20 C11 C12 C2 165(3) . . . . ? O2 C11 C12 C2 -32(2) . . . . ? C20 C11 C12 C13 3.3(18) . . . . ? O2 C11 C12 C13 165.9(17) . . . . ? C1 C2 C12 C11 71(2) . . . . ? C3 C2 C12 C11 -110(2) . . . . ? C1 C2 C12 C13 -129.2(16) . . . . ? C3 C2 C12 C13 50(3) . . . . ? C11 C12 C13 C14 -175.6(10) . . . . ? C2 C12 C13 C14 24(2) . . . . ? C11 C12 C13 C18 2.0(10) . . . . ? C2 C12 C13 C18 -159(2) . . . . ? C18 C13 C14 C15 0.0 . . . . ? C12 C13 C14 C15 177.6(8) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C13 0.0 . . . . ? C16 C17 C18 C19 -177.2(19) . . . . ? C14 C13 C18 C17 0.0 . . . . ? C12 C13 C18 C17 -177.7(7) . . . . ? C14 C13 C18 C19 177(2) . . . . ? C12 C13 C18 C19 -1(2) . . . . ? C17 C18 C19 C20 171(2) . . . . ? C13 C18 C19 C20 -6(3) . . . . ? C18 C19 C20 C11 11(4) . . . . ? C18 C19 C20 C41 -177(2) . . . . ? C12 C11 C20 C19 -10(3) . . . . ? O2 C11 C20 C19 -172(2) . . . . ? C12 C11 C20 C41 178(2) . . . . ? O2 C11 C20 C41 16(3) . . . . ? C9 C10 C21 C34 51(4) . . . . ? C1 C10 C21 C34 -111(3) . . . . ? C9 C10 C21 C22 -126(2) . . . . ? C1 C10 C21 C22 72(2) . . . . ? C34 C21 C22 C23 -176.1(15) . . . . ? C10 C21 C22 C23 1.0(16) . . . . ? C34 C21 C22 C27 2.5(17) . . . . ? C10 C21 C22 C27 179.6(15) . . . . ? C27 C22 C23 C24 0.0 . . . . ? C21 C22 C23 C24 178.5(7) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C22 0.0 . . . . ? C25 C26 C27 C28 -179.7(10) . . . . ? C23 C22 C27 C26 0.0 . . . . ? C21 C22 C27 C26 -178.7(6) . . . . ? C23 C22 C27 C28 179.7(10) . . . . ? C21 C22 C27 C28 1.0(13) . . . . ? C26 C27 C28 C29 -2.5(15) . . . . ? C22 C27 C28 C29 177.8(10) . . . . ? C26 C27 C28 C33 -178.8(9) . . . . ? C22 C27 C28 C33 1.5(15) . . . . ? C33 C28 C29 C30 0.0 . . . . ? C27 C28 C29 C30 -176.1(16) . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 -176(2) . . . . ? C31 C32 C33 C28 0.0 . . . . ? C29 C28 C33 C34 176(2) . . . . ? C27 C28 C33 C34 -7.3(19) . . . . ? C29 C28 C33 C32 0.0 . . . . ? C27 C28 C33 C32 176.5(14) . . . . ? C10 C21 C34 C33 174(2) . . . . ? C22 C21 C34 C33 -10(3) . . . . ? C32 C33 C34 C21 -171(2) . . . . ? C28 C33 C34 C21 13(3) . . . . ? C19 C20 C41 C42 -74(3) . . . . ? C11 C20 C41 C42 98(3) . . . . ? C19 C20 C41 C54 104(3) . . . . ? C11 C20 C41 C54 -84(3) . . . . ? C54 C41 C42 C43 176.4(13) . . . . ? C20 C41 C42 C43 -5(2) . . . . ? C54 C41 C42 C47 -3.6(17) . . . . ? C20 C41 C42 C47 175(2) . . . . ? C41 C42 C43 C44 180.0(8) . . . . ? C47 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C42 0.0 . . . . ? C45 C46 C47 C48 179.6(12) . . . . ? C41 C42 C47 C46 -180.0(9) . . . . ? C43 C42 C47 C46 0.0 . . . . ? C41 C42 C47 C48 0.4(17) . . . . ? C43 C42 C47 C48 -179.6(11) . . . . ? C46 C47 C48 C49 -0.4(16) . . . . ? C42 C47 C48 C49 179.3(11) . . . . ? C46 C47 C48 C53 179.5(9) . . . . ? C42 C47 C48 C53 -0.9(17) . . . . ? C53 C48 C49 C50 0.0 . . . . ? C47 C48 C49 C50 179.9(17) . . . . ? C48 C49 C50 C51 0.0 . . . . ? C49 C50 C51 C52 0.0 . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C48 0.0 . . . . ? C51 C52 C53 C54 175.6(19) . . . . ? C49 C48 C53 C52 0.0 . . . . ? C47 C48 C53 C52 -179.9(16) . . . . ? C49 C48 C53 C54 -175.7(19) . . . . ? C47 C48 C53 C54 4.4(18) . . . . ? C42 C41 C54 C53 7(3) . . . . ? C20 C41 C54 C53 -171(2) . . . . ? C52 C53 C54 C41 176.2(16) . . . . ? C48 C53 C54 C41 -8(3) . . . . ? O4A P1A O1A C1A 166.0(17) . . . . ? O3A P1A O1A C1A -65.0(19) . . . . ? O2A P1A O1A C1A 48.2(18) . . . . ? O4A P1A O2A C11A -81(2) . . . . ? O3A P1A O2A C11A 155(2) . . . . ? O1A P1A O2A C11A 37(2) . . . . ? O3A P1A O4A Pd1 -37(3) . . . . ? O2A P1A O4A Pd1 -155.9(18) . . . . ? O1A P1A O4A Pd1 90(2) . . . . ? P1A O1A C1A C2A -73.5(17) . . . . ? P1A O1A C1A C10A 99(2) . . . . ? O1A C1A C2A C12A -5(2) . . . . ? C10A C1A C2A C12A -176(3) . . . . ? O1A C1A C2A C3A 175.0(16) . . . . ? C10A C1A C2A C3A 3.9(18) . . . . ? C1A C2A C3A C4A -177.3(9) . . . . ? C12A C2A C3A C4A 2(2) . . . . ? C1A C2A C3A C8A 3.2(10) . . . . ? C12A C2A C3A C8A -177(2) . . . . ? C8A C3A C4A C5A 0.0 . . . . ? C2A C3A C4A C5A -179.5(7) . . . . ? C3A C4A C5A C6A 0.0 . . . . ? C4A C5A C6A C7A 0.0 . . . . ? C5A C6A C7A C8A 0.0 . . . . ? C6A C7A C8A C9A -171.9(19) . . . . ? C6A C7A C8A C3A 0.0 . . . . ? C4A C3A C8A C9A 172.6(17) . . . . ? C2A C3A C8A C9A -7.9(18) . . . . ? C4A C3A C8A C7A 0.0 . . . . ? C2A C3A C8A C7A 179.5(8) . . . . ? C7A C8A C9A C10A 179(2) . . . . ? C3A C8A C9A C10A 7(4) . . . . ? C8A C9A C10A C21A 175(3) . . . . ? C8A C9A C10A C1A 0(4) . . . . ? C2A C1A C10A C9A -5(3) . . . . ? O1A C1A C10A C9A -176.4(19) . . . . ? C2A C1A C10A C21A 179(2) . . . . ? O1A C1A C10A C21A 8(3) . . . . ? P1A O2A C11A C20A 114(3) . . . . ? P1A O2A C11A C12A -49(3) . . . . ? C1A C2A C12A C13A -121.8(17) . . . . ? C3A C2A C12A C13A 59(2) . . . . ? C1A C2A C12A C11A 68(2) . . . . ? C3A C2A C12A C11A -112.0(18) . . . . ? O2A C11A C12A C13A 163(2) . . . . ? C20A C11A C12A C13A 0.2(18) . . . . ? O2A C11A C12A C2A -26(2) . . . . ? C20A C11A C12A C2A 171(3) . . . . ? C2A C12A C13A C14A 14(2) . . . . ? C11A C12A C13A C14A -176.6(10) . . . . ? C2A C12A C13A C18A -168(2) . . . . ? C11A C12A C13A C18A 1.4(10) . . . . ? C18A C13A C14A C15A 0.0 . . . . ? C12A C13A C14A C15A 178.0(8) . . . . ? C13A C14A C15A C16A 0.0 . . . . ? C14A C15A C16A C17A 0.0 . . . . ? C15A C16A C17A C18A 0.0 . . . . ? C16A C17A C18A C13A 0.0 . . . . ? C16A C17A C18A C19A -178.0(19) . . . . ? C14A C13A C18A C17A 0.0 . . . . ? C12A C13A C18A C17A -178.0(8) . . . . ? C14A C13A C18A C19A 178.1(17) . . . . ? C12A C13A C18A C19A 0.1(18) . . . . ? C17A C18A C19A C20A 174(3) . . . . ? C13A C18A C19A C20A -4(4) . . . . ? C18A C19A C20A C11A 6(4) . . . . ? C18A C19A C20A C41A 179(3) . . . . ? O2A C11A C20A C19A -167(3) . . . . ? C12A C11A C20A C19A -3(3) . . . . ? O2A C11A C20A C41A 19(4) . . . . ? C12A C11A C20A C41A -177(2) . . . . ? C9A C10A C21A C34A 60(4) . . . . ? C1A C10A C21A C34A -126(2) . . . . ? C9A C10A C21A C22A -116(3) . . . . ? C1A C10A C21A C22A 58(3) . . . . ? C34A C21A C22A C23A -178.6(14) . . . . ? C10A C21A C22A C23A -2(2) . . . . ? C34A C21A C22A C27A 2.3(16) . . . . ? C10A C21A C22A C27A 178(2) . . . . ? C27A C22A C23A C24A 0.0 . . . . ? C21A C22A C23A C24A -179.2(7) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C27A 0.0 . . . . ? C25A C26A C27A C22A 0.0 . . . . ? C25A C26A C27A C28A -176.8(11) . . . . ? C23A C22A C27A C26A 0.0 . . . . ? C21A C22A C27A C26A 179.1(8) . . . . ? C23A C22A C27A C28A 176.9(11) . . . . ? C21A C22A C27A C28A -4.1(16) . . . . ? C26A C27A C28A C29A -4.2(16) . . . . ? C22A C27A C28A C29A 179.0(10) . . . . ? C26A C27A C28A C33A -179.0(10) . . . . ? C22A C27A C28A C33A 4.2(18) . . . . ? C33A C28A C29A C30A 0.0 . . . . ? C27A C28A C29A C30A -174.8(18) . . . . ? C28A C29A C30A C31A 0.0 . . . . ? C29A C30A C31A C32A 0.0 . . . . ? C30A C31A C32A C33A 0.0 . . . . ? C31A C32A C33A C28A 0.0 . . . . ? C31A C32A C33A C34A 177(2) . . . . ? C29A C28A C33A C32A 0.0 . . . . ? C27A C28A C33A C32A 174.8(17) . . . . ? C29A C28A C33A C34A -177.5(19) . . . . ? C27A C28A C33A C34A -2.7(19) . . . . ? C10A C21A C34A C33A -177(3) . . . . ? C22A C21A C34A C33A -1(3) . . . . ? C32A C33A C34A C21A -176(2) . . . . ? C28A C33A C34A C21A 1(4) . . . . ? C19A C20A C41A C54A 106(4) . . . . ? C11A C20A C41A C54A -81(3) . . . . ? C19A C20A C41A C42A -74(4) . . . . ? C11A C20A C41A C42A 99(3) . . . . ? C54A C41A C42A C43A 178.4(16) . . . . ? C20A C41A C42A C43A -1(2) . . . . ? C54A C41A C42A C47A 0.1(19) . . . . ? C20A C41A C42A C47A -180(2) . . . . ? C47A C42A C43A C44A 0.0 . . . . ? C41A C42A C43A C44A -178.3(8) . . . . ? C42A C43A C44A C45A 0.0 . . . . ? C43A C44A C45A C46A 0.0 . . . . ? C44A C45A C46A C47A 0.0 . . . . ? C45A C46A C47A C42A 0.0 . . . . ? C45A C46A C47A C48A -177.7(10) . . . . ? C43A C42A C47A C46A 0.0 . . . . ? C41A C42A C47A C46A 178.5(7) . . . . ? C43A C42A C47A C48A 177.7(11) . . . . ? C41A C42A C47A C48A -3.8(14) . . . . ? C46A C47A C48A C49A 1.2(14) . . . . ? C42A C47A C48A C49A -176.5(10) . . . . ? C46A C47A C48A C53A -176.6(9) . . . . ? C42A C47A C48A C53A 5.7(17) . . . . ? C53A C48A C49A C50A 0.0 . . . . ? C47A C48A C49A C50A -177.8(16) . . . . ? C48A C49A C50A C51A 0.0 . . . . ? C49A C50A C51A C52A 0.0 . . . . ? C50A C51A C52A C53A 0.0 . . . . ? C51A C52A C53A C48A 0.0 . . . . ? C51A C52A C53A C54A -179(2) . . . . ? C49A C48A C53A C52A 0.0 . . . . ? C47A C48A C53A C52A 177.8(15) . . . . ? C49A C48A C53A C54A 178.8(18) . . . . ? C47A C48A C53A C54A -3.3(19) . . . . ? C42A C41A C54A C53A 2(3) . . . . ? C20A C41A C54A C53A -178(3) . . . . ? C52A C53A C54A C41A 178.4(18) . . . . ? C48A C53A C54A C41A 0(3) . . . . ? P1A O4A Pd1 O4A 12.7(17) . . . 2_656 ? P1A O4A Pd1 O4 -85(3) . . . 2_656 ? P1A O4A Pd1 O4 176(2) . . . . ? P1 O4 Pd1 O4A -96(3) . . . 2_656 ? P1 O4 Pd1 O4A 164.9(19) . . . . ? P1 O4 Pd1 O4 1.8(14) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.109 _refine_diff_density_min -1.374 _refine_diff_density_rms 0.170