Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Setharampattu S. Krishnamurthy' _publ_contact_author_address ; Department of Chemistry Indian Institute of Science Bangalore 560012 INDIA ; _publ_contact_author_email SSKRISH@IPC.IISC.ERNET.IN _publ_section_title ; Unusual reactivity of a sterically hindered diphosphazane ligand, EtN{P(OR)2}2, (R = C6H3(Pri)2-2,6) towards (eta3-allyl)palladium precursors ; _publ_requested_category CM loop_ _publ_author_name 'Krishnamurthy Setharampattu' 'Heera Krishna' 'Ramaswamy Murugavel' 'Munirathinam Nethaji' 'Ganesan Prabusankar' ###END data_complex6_ _database_code_depnum_ccdc_archive 'CCDC 618420' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H84 Cl N O5 P2 Pd2' _chemical_formula_sum 'C56 H84 Cl N O5 P2 Pd2' _chemical_formula_weight 1161.43 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' 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.616(2) _cell_length_b 40.964(9) _cell_length_c 13.602(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.722(4) _cell_angle_gamma 90.00 _cell_volume 5874(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 26.4 _exptl_crystal_description rectangular _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7273 _exptl_absorpt_correction_T_max 0.8514 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'bruker smart apex ccd' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47088 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.37 _reflns_number_total 11990 _reflns_number_gt 8413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'bruker smart apex ccd' _computing_cell_refinement 'bruker smart apex ccd' _computing_data_reduction 'bruker saint' _computing_structure_solution shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ortep-iii _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11990 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1193 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.008 _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 Pd1 Pd 0.93031(3) 0.395539(8) 0.73747(3) 0.04292(10) Uani 1 1 d . . . Pd2 Pd 0.88761(3) 0.387823(7) 0.54859(3) 0.04392(10) Uani 1 1 d . . . Cl1 Cl 1.14630(12) 0.38577(4) 0.76693(12) 0.0824(4) Uani 1 1 d . . . P1 P 0.73009(9) 0.40356(2) 0.72437(7) 0.0308(2) Uani 1 1 d . . . P2 P 0.70792(10) 0.35967(2) 0.56365(8) 0.0333(2) Uani 1 1 d . . . O1 O 0.6574(2) 0.43769(5) 0.69459(18) 0.0323(6) Uani 1 1 d . . . O2 O 0.6820(2) 0.39845(6) 0.83323(19) 0.0359(6) Uani 1 1 d . . . O3 O 0.6026(3) 0.35602(6) 0.46802(19) 0.0428(7) Uani 1 1 d . . . O4 O 0.7037(2) 0.32353(6) 0.6107(2) 0.0409(7) Uani 1 1 d . . . O5 O 1.1748(11) 0.3812(4) 1.2271(9) 0.353(9) Uani 1 1 d . . . N1 N 0.6322(3) 0.37933(7) 0.6484(2) 0.0322(7) Uani 1 1 d . . . C1 C 0.6670(4) 0.46701(8) 0.7494(3) 0.0329(9) Uani 1 1 d . . . C2 C 0.5683(4) 0.47442(9) 0.8043(3) 0.0385(9) Uani 1 1 d . . . C3 C 0.5755(4) 0.50390(10) 0.8554(3) 0.0499(11) Uani 1 1 d . . . H3 H 0.5107 0.5096 0.8925 0.060 Uiso 1 1 calc R . . C4 C 0.6763(5) 0.52477(10) 0.8521(3) 0.0550(12) Uani 1 1 d . . . H4 H 0.6811 0.5439 0.8890 0.066 Uiso 1 1 calc R . . C5 C 0.7698(4) 0.51729(10) 0.7944(3) 0.0526(12) Uani 1 1 d . . . H5 H 0.8366 0.5318 0.7915 0.063 Uiso 1 1 calc R . . C6 C 0.7676(4) 0.48848(9) 0.7398(3) 0.0408(10) Uani 1 1 d . . . C7 C 0.8669(4) 0.48227(10) 0.6700(3) 0.0505(12) Uani 1 1 d . . . H7 H 0.8602 0.4593 0.6495 0.061 Uiso 1 1 calc R . . C8 C 0.8361(6) 0.50322(18) 0.5781(4) 0.100(2) Uani 1 1 d . . . H8A H 0.8443 0.5259 0.5959 0.150 Uiso 1 1 calc R . . H8B H 0.7508 0.4989 0.5494 0.150 Uiso 1 1 calc R . . H8C H 0.8938 0.4981 0.5310 0.150 Uiso 1 1 calc R . . C9 C 1.0007(5) 0.4882(2) 0.7151(5) 0.109(2) Uani 1 1 d . . . H9A H 1.0583 0.4796 0.6722 0.164 Uiso 1 1 calc R . . H9B H 1.0148 0.4775 0.7782 0.164 Uiso 1 1 calc R . . H9C H 1.0146 0.5112 0.7236 0.164 Uiso 1 1 calc R . . C10 C 0.4512(4) 0.45336(10) 0.8026(3) 0.0434(10) Uani 1 1 d . . . H10 H 0.4747 0.4315 0.7817 0.052 Uiso 1 1 calc R . . C11 C 0.3478(5) 0.46540(17) 0.7261(6) 0.110(3) Uani 1 1 d . . . H11A H 0.3170 0.4860 0.7466 0.166 Uiso 1 1 calc R . . H11B H 0.2796 0.4499 0.7190 0.166 Uiso 1 1 calc R . . H11C H 0.3809 0.4679 0.6638 0.166 Uiso 1 1 calc R . . C12 C 0.4033(6) 0.44947(18) 0.9017(5) 0.111(3) Uani 1 1 d . . . H12A H 0.4701 0.4412 0.9488 0.167 Uiso 1 1 calc R . . H12B H 0.3333 0.4345 0.8959 0.167 Uiso 1 1 calc R . . H12C H 0.3758 0.4703 0.9238 0.167 Uiso 1 1 calc R . . C13 C 0.7632(4) 0.38146(10) 0.9074(3) 0.0427(10) Uani 1 1 d . . . C14 C 0.8576(5) 0.39915(11) 0.9638(3) 0.0547(12) Uani 1 1 d . . . C15 C 0.9328(5) 0.38144(15) 1.0354(4) 0.0796(17) Uani 1 1 d . . . H15 H 0.9967 0.3922 1.0756 0.096 Uiso 1 1 calc R . . C16 C 0.9157(6) 0.34851(16) 1.0487(4) 0.0843(18) Uani 1 1 d . . . H16 H 0.9702 0.3371 1.0949 0.101 Uiso 1 1 calc R . . C17 C 0.8188(6) 0.33274(12) 0.9938(4) 0.0673(14) Uani 1 1 d . . . H17 H 0.8067 0.3106 1.0044 0.081 Uiso 1 1 calc R . . C18 C 0.7379(4) 0.34884(11) 0.9228(3) 0.0499(11) Uani 1 1 d . . . C19 C 0.6228(5) 0.33223(11) 0.8702(4) 0.0641(14) Uani 1 1 d . . . H19 H 0.6160 0.3390 0.8006 0.077 Uiso 1 1 calc R . . C20 C 0.6272(7) 0.29486(13) 0.8719(5) 0.108(2) Uani 1 1 d . . . H20A H 0.6976 0.2875 0.8394 0.162 Uiso 1 1 calc R . . H20B H 0.5498 0.2863 0.8380 0.162 Uiso 1 1 calc R . . H20C H 0.6371 0.2874 0.9392 0.162 Uiso 1 1 calc R . . C21 C 0.5025(5) 0.34396(15) 0.9114(4) 0.0845(18) Uani 1 1 d . . . H21A H 0.5055 0.3376 0.9796 0.127 Uiso 1 1 calc R . . H21B H 0.4295 0.3343 0.8741 0.127 Uiso 1 1 calc R . . H21C H 0.4970 0.3673 0.9065 0.127 Uiso 1 1 calc R . . C22 C 0.8750(5) 0.43568(12) 0.9554(4) 0.0670(15) Uani 1 1 d . . . H22 H 0.8405 0.4420 0.8881 0.080 Uiso 1 1 calc R . . C23 C 1.0149(6) 0.44640(16) 0.9703(5) 0.105(2) Uani 1 1 d . . . H23A H 1.0216 0.4685 0.9482 0.158 Uiso 1 1 calc R . . H23B H 1.0638 0.4324 0.9328 0.158 Uiso 1 1 calc R . . H23C H 1.0465 0.4450 1.0393 0.158 Uiso 1 1 calc R . . C24 C 0.8008(6) 0.45339(14) 1.0248(5) 0.099(2) Uani 1 1 d . . . H24A H 0.7125 0.4481 1.0099 0.149 Uiso 1 1 calc R . . H24B H 0.8124 0.4765 1.0178 0.149 Uiso 1 1 calc R . . H24C H 0.8296 0.4470 1.0915 0.149 Uiso 1 1 calc R . . C25 C 0.4946(4) 0.37799(13) 0.6588(4) 0.0623(14) Uani 1 1 d . . . H25A H 0.4885 0.3806 0.7290 0.075 Uiso 1 1 calc R . . H25B H 0.4583 0.3976 0.6270 0.075 Uiso 1 1 calc R . . C26 C 0.4125(6) 0.3532(3) 0.6279(6) 0.169(5) Uani 1 1 d . . . H26A H 0.4144 0.3495 0.5584 0.253 Uiso 1 1 calc R . . H26B H 0.3282 0.3592 0.6398 0.253 Uiso 1 1 calc R . . H26C H 0.4375 0.3337 0.6639 0.253 Uiso 1 1 calc R . . C27 C 0.6144(4) 0.36946(12) 0.3733(3) 0.0518(11) Uani 1 1 d . . . C28 C 0.5776(5) 0.40162(12) 0.3543(4) 0.0610(13) Uani 1 1 d . . . C29 C 0.5846(6) 0.41360(16) 0.2603(4) 0.0857(19) Uani 1 1 d . . . H29 H 0.5613 0.4351 0.2458 0.103 Uiso 1 1 calc R . . C30 C 0.6251(7) 0.39435(18) 0.1879(4) 0.093(2) Uani 1 1 d . . . H30 H 0.6299 0.4029 0.1252 0.111 Uiso 1 1 calc R . . C31 C 0.6584(6) 0.36283(16) 0.2072(4) 0.0796(17) Uani 1 1 d . . . H31 H 0.6857 0.3501 0.1572 0.096 Uiso 1 1 calc R . . C32 C 0.6525(5) 0.34895(12) 0.3014(3) 0.0589(13) Uani 1 1 d . . . C33 C 0.6934(6) 0.31386(13) 0.3193(4) 0.0801(17) Uani 1 1 d . . . H33 H 0.6680 0.3073 0.3834 0.096 Uiso 1 1 calc R . . C34 C 0.6276(8) 0.29068(18) 0.2410(5) 0.137(3) Uani 1 1 d . . . H34A H 0.5373 0.2934 0.2374 0.206 Uiso 1 1 calc R . . H34B H 0.6494 0.2685 0.2587 0.206 Uiso 1 1 calc R . . H34C H 0.6548 0.2956 0.1777 0.206 Uiso 1 1 calc R . . C35 C 0.8372(7) 0.30991(18) 0.3255(5) 0.112(2) Uani 1 1 d . . . H35A H 0.8654 0.3166 0.2641 0.167 Uiso 1 1 calc R . . H35B H 0.8593 0.2874 0.3379 0.167 Uiso 1 1 calc R . . H35C H 0.8772 0.3232 0.3783 0.167 Uiso 1 1 calc R . . C36 C 0.5256(6) 0.42292(13) 0.4304(4) 0.0749(16) Uani 1 1 d . . . H36 H 0.5577 0.4146 0.4961 0.090 Uiso 1 1 calc R . . C37 C 0.3763(7) 0.4202(2) 0.4184(6) 0.152(4) Uani 1 1 d . . . H37A H 0.3432 0.4261 0.3521 0.228 Uiso 1 1 calc R . . H37B H 0.3428 0.4347 0.4644 0.228 Uiso 1 1 calc R . . H37C H 0.3522 0.3982 0.4313 0.228 Uiso 1 1 calc R . . C38 C 0.5629(12) 0.45766(18) 0.4258(7) 0.208(6) Uani 1 1 d . . . H38A H 0.6536 0.4592 0.4309 0.312 Uiso 1 1 calc R . . H38B H 0.5326 0.4694 0.4794 0.312 Uiso 1 1 calc R . . H38C H 0.5266 0.4669 0.3640 0.312 Uiso 1 1 calc R . . C39 C 0.7424(4) 0.29346(9) 0.5733(3) 0.0474(11) Uani 1 1 d . . . C40 C 0.6469(5) 0.27132(11) 0.5384(4) 0.0652(14) Uani 1 1 d . . . C41 C 0.6881(7) 0.24149(12) 0.5039(5) 0.091(2) Uani 1 1 d . . . H41 H 0.6282 0.2261 0.4790 0.109 Uiso 1 1 calc R . . C42 C 0.8126(8) 0.23436(15) 0.5057(6) 0.105(2) Uani 1 1 d . . . H42 H 0.8370 0.2146 0.4802 0.126 Uiso 1 1 calc R . . C43 C 0.9024(6) 0.25585(15) 0.5444(5) 0.093(2) Uani 1 1 d . . . H43 H 0.9874 0.2502 0.5463 0.111 Uiso 1 1 calc R . . C44 C 0.8711(5) 0.28621(11) 0.5814(4) 0.0607(13) Uani 1 1 d . . . C45 C 0.9716(5) 0.30875(13) 0.6345(5) 0.0723(16) Uani 1 1 d . . . H45 H 0.9430 0.3313 0.6222 0.087 Uiso 1 1 calc R . . C46 C 0.9819(7) 0.30293(16) 0.7445(5) 0.112(2) Uani 1 1 d . . . H46A H 0.9964 0.2801 0.7578 0.168 Uiso 1 1 calc R . . H46B H 0.9045 0.3095 0.7689 0.168 Uiso 1 1 calc R . . H46C H 1.0513 0.3154 0.7768 0.168 Uiso 1 1 calc R . . C47 C 1.0998(6) 0.3054(2) 0.5982(7) 0.152(4) Uani 1 1 d . . . H47A H 1.1590 0.3197 0.6353 0.228 Uiso 1 1 calc R . . H47B H 1.0933 0.3110 0.5293 0.228 Uiso 1 1 calc R . . H47C H 1.1286 0.2833 0.6069 0.228 Uiso 1 1 calc R . . C48 C 0.5088(6) 0.27764(14) 0.5441(5) 0.088(2) Uani 1 1 d . . . H48 H 0.5005 0.3006 0.5628 0.105 Uiso 1 1 calc R . . C49 C 0.4250(7) 0.2724(3) 0.4491(7) 0.164(4) Uani 1 1 d . . . H49A H 0.4433 0.2887 0.4018 0.246 Uiso 1 1 calc R . . H49B H 0.3378 0.2742 0.4608 0.246 Uiso 1 1 calc R . . H49C H 0.4401 0.2511 0.4236 0.246 Uiso 1 1 calc R . . C50 C 0.4599(8) 0.2573(3) 0.6232(6) 0.148(4) Uani 1 1 d . . . H50A H 0.4787 0.2347 0.6127 0.222 Uiso 1 1 calc R . . H50B H 0.3698 0.2601 0.6206 0.222 Uiso 1 1 calc R . . H50C H 0.4999 0.2640 0.6869 0.222 Uiso 1 1 calc R . . C51 C 0.9181(7) 0.39359(19) 0.3938(5) 0.106(2) Uani 1 1 d . . . H51A H 0.9395 0.3740 0.3593 0.128 Uiso 1 1 calc R . . H51B H 0.8599 0.4079 0.3540 0.128 Uiso 1 1 calc R . . C52 C 1.0043(11) 0.4067(3) 0.4466(6) 0.213(7) Uani 1 1 d . . . H52 H 1.0674 0.4098 0.4055 0.255 Uiso 1 1 calc R . . C53 C 1.0504(5) 0.41804(15) 0.5285(5) 0.0789(17) Uani 1 1 d . . . H53A H 1.0408 0.4413 0.5380 0.095 Uiso 1 1 calc R . . H53B H 1.1327 0.4097 0.5555 0.095 Uiso 1 1 calc R . . C54 C 1.233(2) 0.3302(6) 1.2697(18) 0.43(2) Uani 1 1 d . . . H54A H 1.1684 0.3340 1.3123 0.644 Uiso 1 1 calc R . . H54B H 1.3127 0.3265 1.3092 0.644 Uiso 1 1 calc R . . H54C H 1.2110 0.3113 1.2294 0.644 Uiso 1 1 calc R . . C55 C 1.2431(14) 0.3590(8) 1.205(2) 0.329(19) Uani 1 1 d . . . C56 C 1.2855(14) 0.3613(6) 1.122(2) 0.46(3) Uani 1 1 d . . . H56A H 1.2187 0.3566 1.0700 0.687 Uiso 1 1 calc R . . H56B H 1.3534 0.3460 1.1190 0.687 Uiso 1 1 calc R . . H56C H 1.3163 0.3831 1.1138 0.687 Uiso 1 1 calc R . . 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 0.03024(17) 0.04556(18) 0.0531(2) -0.00314(15) 0.00534(15) -0.00111(13) Pd2 0.0429(2) 0.04139(18) 0.0505(2) 0.00009(15) 0.01846(16) -0.00557(14) Cl1 0.0350(7) 0.0935(10) 0.1172(13) -0.0122(8) 0.0020(7) 0.0040(6) P1 0.0304(5) 0.0292(5) 0.0335(6) -0.0005(4) 0.0065(4) -0.0022(4) P2 0.0378(6) 0.0287(5) 0.0351(6) -0.0019(4) 0.0107(5) 0.0007(4) O1 0.0349(14) 0.0293(13) 0.0336(14) -0.0023(11) 0.0076(11) -0.0005(11) O2 0.0368(15) 0.0400(14) 0.0312(15) 0.0010(11) 0.0055(12) -0.0034(11) O3 0.0506(18) 0.0443(16) 0.0345(17) -0.0063(12) 0.0089(14) -0.0049(13) O4 0.0468(17) 0.0301(13) 0.0484(17) -0.0020(12) 0.0166(14) 0.0032(12) O5 0.220(12) 0.59(3) 0.228(12) -0.203(14) -0.075(9) 0.095(13) N1 0.0302(17) 0.0344(16) 0.0333(18) -0.0055(13) 0.0086(14) -0.0011(13) C1 0.037(2) 0.0284(18) 0.033(2) -0.0011(15) 0.0023(18) 0.0012(15) C2 0.040(2) 0.039(2) 0.037(2) -0.0040(18) 0.0076(19) 0.0000(17) C3 0.060(3) 0.043(2) 0.048(3) -0.011(2) 0.015(2) -0.001(2) C4 0.074(3) 0.035(2) 0.057(3) -0.014(2) 0.013(3) -0.006(2) C5 0.056(3) 0.040(2) 0.062(3) -0.006(2) 0.009(2) -0.012(2) C6 0.044(2) 0.033(2) 0.045(3) 0.0027(18) 0.006(2) -0.0031(17) C7 0.047(3) 0.040(2) 0.070(3) 0.003(2) 0.027(2) -0.0063(19) C8 0.087(4) 0.140(6) 0.083(5) 0.025(4) 0.052(4) 0.020(4) C9 0.051(4) 0.167(7) 0.113(6) -0.017(5) 0.020(4) -0.004(4) C10 0.040(2) 0.041(2) 0.052(3) -0.0107(19) 0.017(2) -0.0034(18) C11 0.052(4) 0.104(5) 0.165(7) 0.036(5) -0.032(4) -0.020(3) C12 0.117(6) 0.145(6) 0.082(5) -0.035(4) 0.057(4) -0.073(5) C13 0.048(3) 0.048(2) 0.033(2) 0.0040(18) 0.009(2) 0.0007(19) C14 0.055(3) 0.059(3) 0.048(3) 0.007(2) -0.004(2) -0.007(2) C15 0.066(4) 0.094(4) 0.072(4) 0.017(3) -0.021(3) -0.010(3) C16 0.085(4) 0.093(5) 0.072(4) 0.032(3) -0.004(4) 0.015(4) C17 0.088(4) 0.048(3) 0.069(4) 0.016(3) 0.020(3) 0.010(3) C18 0.061(3) 0.052(3) 0.039(3) 0.006(2) 0.013(2) 0.003(2) C19 0.090(4) 0.050(3) 0.054(3) 0.004(2) 0.016(3) -0.020(3) C20 0.160(7) 0.055(3) 0.109(5) -0.002(3) 0.016(5) -0.035(4) C21 0.077(4) 0.096(4) 0.085(4) 0.007(3) 0.027(3) -0.030(3) C22 0.074(4) 0.065(3) 0.056(3) 0.004(3) -0.019(3) -0.022(3) C23 0.091(5) 0.107(5) 0.115(6) -0.016(4) -0.001(4) -0.047(4) C24 0.105(5) 0.063(4) 0.129(6) 0.006(4) 0.010(4) 0.000(3) C25 0.036(3) 0.097(4) 0.058(3) -0.030(3) 0.020(2) -0.025(2) C26 0.072(5) 0.293(13) 0.151(8) -0.121(8) 0.056(5) -0.070(6) C27 0.054(3) 0.063(3) 0.037(3) -0.004(2) 0.003(2) -0.007(2) C28 0.078(4) 0.055(3) 0.049(3) 0.012(2) 0.004(3) 0.006(2) C29 0.118(5) 0.091(4) 0.048(4) 0.021(3) 0.011(3) 0.012(4) C30 0.115(6) 0.117(6) 0.046(4) 0.022(4) 0.008(3) -0.002(4) C31 0.097(5) 0.102(5) 0.043(3) -0.007(3) 0.021(3) -0.007(4) C32 0.068(3) 0.070(3) 0.040(3) -0.011(2) 0.011(2) -0.010(3) C33 0.123(5) 0.067(3) 0.055(3) -0.021(3) 0.035(3) -0.008(3) C34 0.202(9) 0.108(6) 0.105(6) -0.052(5) 0.035(6) -0.037(6) C35 0.116(6) 0.107(5) 0.114(6) 0.000(4) 0.029(5) 0.030(5) C36 0.105(5) 0.061(3) 0.058(3) 0.010(3) 0.006(3) 0.021(3) C37 0.100(6) 0.211(10) 0.137(7) -0.046(7) -0.017(5) 0.078(6) C38 0.449(19) 0.062(5) 0.134(8) -0.009(5) 0.125(10) -0.030(8) C39 0.058(3) 0.030(2) 0.057(3) 0.0031(19) 0.021(2) 0.0059(19) C40 0.077(4) 0.036(2) 0.086(4) -0.011(2) 0.022(3) -0.003(2) C41 0.118(6) 0.038(3) 0.120(5) -0.019(3) 0.022(4) -0.008(3) C42 0.136(7) 0.048(3) 0.136(6) -0.022(4) 0.040(5) 0.026(4) C43 0.092(5) 0.067(4) 0.124(6) 0.005(4) 0.038(4) 0.035(4) C44 0.064(3) 0.044(3) 0.078(4) 0.009(2) 0.026(3) 0.018(2) C45 0.048(3) 0.062(3) 0.107(5) 0.026(3) 0.012(3) 0.017(2) C46 0.134(6) 0.083(5) 0.110(6) 0.016(4) -0.019(5) -0.006(4) C47 0.064(5) 0.163(8) 0.239(11) -0.014(7) 0.054(6) -0.010(5) C48 0.067(4) 0.059(3) 0.140(6) -0.020(4) 0.023(4) -0.019(3) C49 0.090(6) 0.244(12) 0.156(9) 0.056(8) 0.005(6) -0.018(7) C50 0.111(6) 0.227(11) 0.114(7) -0.008(7) 0.047(5) -0.033(7) C51 0.111(6) 0.152(7) 0.067(4) 0.001(4) 0.053(4) -0.048(5) C52 0.236(12) 0.336(15) 0.082(6) -0.037(7) 0.082(7) -0.239(12) C53 0.060(4) 0.095(4) 0.089(5) -0.001(3) 0.037(3) -0.031(3) C54 0.27(3) 0.55(5) 0.45(4) 0.27(3) -0.05(2) 0.09(3) C55 0.079(9) 0.51(4) 0.39(3) -0.32(3) -0.015(12) 0.054(15) C56 0.145(13) 0.45(3) 0.82(6) -0.38(4) 0.23(2) -0.068(17) _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 P1 2.1376(10) . ? Pd1 Cl1 2.3158(13) . ? Pd1 Pd2 2.5755(7) . ? Pd2 C52 2.111(6) . ? Pd2 C53 2.168(5) . ? Pd2 C51 2.180(6) . ? Pd2 P2 2.2588(11) . ? P1 O1 1.625(2) . ? P1 O2 1.635(3) . ? P1 N1 1.698(3) . ? P2 O4 1.615(3) . ? P2 O3 1.620(3) . ? P2 N1 1.685(3) . ? O1 C1 1.411(4) . ? O2 C13 1.429(5) . ? O3 C27 1.421(5) . ? O4 C39 1.412(4) . ? O5 C55 1.220(18) . ? N1 C25 1.485(5) . ? C1 C2 1.390(5) . ? C1 C6 1.401(5) . ? C2 C3 1.391(5) . ? C2 C10 1.512(5) . ? C3 C4 1.375(6) . ? C3 H3 0.9300 . ? C4 C5 1.371(6) . ? C4 H4 0.9300 . ? C5 C6 1.393(6) . ? C5 H5 0.9300 . ? C6 C7 1.521(6) . ? C7 C9 1.499(7) . ? C7 C8 1.520(7) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C12 1.504(6) . ? C10 C11 1.505(7) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.384(6) . ? C13 C14 1.392(6) . ? C14 C15 1.390(7) . ? C14 C22 1.514(6) . ? C15 C16 1.376(8) . ? C15 H15 0.9300 . ? C16 C17 1.361(8) . ? C16 H16 0.9300 . ? C17 C18 1.383(7) . ? C17 H17 0.9300 . ? C18 C19 1.505(6) . ? C19 C21 1.531(7) . ? C19 C20 1.532(7) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C24 1.488(8) . ? C22 C23 1.539(7) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.371(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C32 1.384(6) . ? C27 C28 1.390(7) . ? C28 C29 1.380(7) . ? C28 C36 1.508(7) . ? C29 C30 1.369(8) . ? C29 H29 0.9300 . ? C30 C31 1.356(8) . ? C30 H30 0.9300 . ? C31 C32 1.411(7) . ? C31 H31 0.9300 . ? C32 C33 1.513(7) . ? C33 C35 1.528(8) . ? C33 C34 1.533(8) . ? C33 H33 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C38 1.481(9) . ? C36 C37 1.578(9) . ? C36 H36 0.9800 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C44 1.390(6) . ? C39 C40 1.401(6) . ? C40 C41 1.397(7) . ? C40 C48 1.499(8) . ? C41 C42 1.351(9) . ? C41 H41 0.9300 . ? C42 C43 1.358(9) . ? C42 H42 0.9300 . ? C43 C44 1.396(7) . ? C43 H43 0.9300 . ? C44 C45 1.527(7) . ? C45 C46 1.506(8) . ? C45 C47 1.507(7) . ? C45 H45 0.9800 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.496(10) . ? C48 C50 1.502(9) . ? C48 H48 0.9800 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.219(10) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.253(9) . ? C52 H52 0.9300 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.48(4) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.27(4) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? 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 P1 Pd1 Cl1 174.71(4) . . ? P1 Pd1 Pd2 83.02(3) . . ? Cl1 Pd1 Pd2 101.92(4) . . ? C52 Pd2 C53 34.0(3) . . ? C52 Pd2 C51 32.9(3) . . ? C53 Pd2 C51 66.8(3) . . ? C52 Pd2 P2 144.4(3) . . ? C53 Pd2 P2 175.29(18) . . ? C51 Pd2 P2 111.4(2) . . ? C52 Pd2 Pd1 124.2(3) . . ? C53 Pd2 Pd1 90.33(17) . . ? C51 Pd2 Pd1 157.12(19) . . ? P2 Pd2 Pd1 91.38(3) . . ? O1 P1 O2 98.41(13) . . ? O1 P1 N1 96.44(14) . . ? O2 P1 N1 104.05(14) . . ? O1 P1 Pd1 126.27(10) . . ? O2 P1 Pd1 108.53(10) . . ? N1 P1 Pd1 119.52(11) . . ? O4 P2 O3 100.66(15) . . ? O4 P2 N1 97.45(14) . . ? O3 P2 N1 104.68(15) . . ? O4 P2 Pd2 124.51(11) . . ? O3 P2 Pd2 119.03(11) . . ? N1 P2 Pd2 107.06(11) . . ? C1 O1 P1 126.7(2) . . ? C13 O2 P1 118.3(2) . . ? C27 O3 P2 124.5(3) . . ? C39 O4 P2 129.4(2) . . ? C25 N1 P2 126.9(3) . . ? C25 N1 P1 120.1(3) . . ? P2 N1 P1 112.89(17) . . ? C2 C1 C6 122.9(3) . . ? C2 C1 O1 117.2(3) . . ? C6 C1 O1 119.7(3) . . ? C1 C2 C3 117.2(4) . . ? C1 C2 C10 122.6(3) . . ? C3 C2 C10 120.0(4) . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.7(4) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 116.7(4) . . ? C5 C6 C7 120.3(4) . . ? C1 C6 C7 123.0(3) . . ? C9 C7 C8 110.3(5) . . ? C9 C7 C6 114.3(4) . . ? C8 C7 C6 108.7(4) . . ? C9 C7 H7 107.8 . . ? C8 C7 H7 107.8 . . ? C6 C7 H7 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 111.0(5) . . ? C12 C10 C2 114.3(4) . . ? C11 C10 C2 110.8(4) . . ? C12 C10 H10 106.7 . . ? C11 C10 H10 106.7 . . ? C2 C10 H10 106.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 124.0(4) . . ? C18 C13 O2 117.7(4) . . ? C14 C13 O2 118.1(4) . . ? C15 C14 C13 115.6(4) . . ? C15 C14 C22 120.3(5) . . ? C13 C14 C22 124.0(4) . . ? C16 C15 C14 122.0(5) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C17 C16 C15 119.8(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 121.6(5) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C18 C13 116.8(5) . . ? C17 C18 C19 121.4(4) . . ? C13 C18 C19 121.7(4) . . ? C18 C19 C21 110.5(4) . . ? C18 C19 C20 115.0(5) . . ? C21 C19 C20 109.5(5) . . ? C18 C19 H19 107.2 . . ? C21 C19 H19 107.2 . . ? C20 C19 H19 107.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C14 110.8(5) . . ? C24 C22 C23 110.6(5) . . ? C14 C22 C23 113.3(5) . . ? C24 C22 H22 107.3 . . ? C14 C22 H22 107.3 . . ? C23 C22 H22 107.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N1 126.5(5) . . ? C26 C25 H25A 105.7 . . ? N1 C25 H25A 105.7 . . ? C26 C25 H25B 105.7 . . ? N1 C25 H25B 105.7 . . ? H25A C25 H25B 106.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 122.9(4) . . ? C32 C27 O3 118.0(4) . . ? C28 C27 O3 118.9(4) . . ? C29 C28 C27 117.7(5) . . ? C29 C28 C36 119.6(5) . . ? C27 C28 C36 122.6(4) . . ? C30 C29 C28 121.1(6) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C31 C30 C29 120.4(6) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 121.4(5) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C27 C32 C31 116.4(5) . . ? C27 C32 C33 124.4(4) . . ? C31 C32 C33 119.1(5) . . ? C32 C33 C35 112.0(5) . . ? C32 C33 C34 112.2(6) . . ? C35 C33 C34 110.1(5) . . ? C32 C33 H33 107.4 . . ? C35 C33 H33 107.4 . . ? C34 C33 H33 107.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 C28 113.9(5) . . ? C38 C36 C37 109.5(7) . . ? C28 C36 C37 109.4(5) . . ? C38 C36 H36 107.9 . . ? C28 C36 H36 107.9 . . ? C37 C36 H36 107.9 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C44 C39 C40 123.6(4) . . ? C44 C39 O4 118.8(4) . . ? C40 C39 O4 117.2(4) . . ? C41 C40 C39 115.9(5) . . ? C41 C40 C48 121.0(5) . . ? C39 C40 C48 122.9(4) . . ? C42 C41 C40 121.8(6) . . ? C42 C41 H41 119.1 . . ? C40 C41 H41 119.1 . . ? C41 C42 C43 120.5(5) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C44 122.1(6) . . ? C42 C43 H43 118.9 . . ? C44 C43 H43 118.9 . . ? C39 C44 C43 115.8(5) . . ? C39 C44 C45 122.3(4) . . ? C43 C44 C45 121.8(5) . . ? C46 C45 C47 110.3(6) . . ? C46 C45 C44 109.9(5) . . ? C47 C45 C44 113.4(6) . . ? C46 C45 H45 107.7 . . ? C47 C45 H45 107.7 . . ? C44 C45 H45 107.7 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C40 114.6(6) . . ? C49 C48 C50 108.6(6) . . ? C40 C48 C50 111.3(6) . . ? C49 C48 H48 107.3 . . ? C40 C48 H48 107.3 . . ? C50 C48 H48 107.3 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 Pd2 70.4(4) . . ? C52 C51 H51A 116.6 . . ? Pd2 C51 H51A 116.6 . . ? C52 C51 H51B 116.6 . . ? Pd2 C51 H51B 116.6 . . ? H51A C51 H51B 113.6 . . ? C51 C52 C53 151.1(8) . . ? C51 C52 Pd2 76.6(4) . . ? C53 C52 Pd2 75.5(4) . . ? C51 C52 H52 104.5 . . ? C53 C52 H52 104.5 . . ? Pd2 C52 H52 164.6 . . ? C52 C53 Pd2 70.5(4) . . ? C52 C53 H53A 116.6 . . ? Pd2 C53 H53A 116.6 . . ? C52 C53 H53B 116.6 . . ? Pd2 C53 H53B 116.6 . . ? H53A C53 H53B 113.6 . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O5 C55 C56 116(4) . . ? O5 C55 C54 111(3) . . ? C56 C55 C54 130(2) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? 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 P1 Pd1 Pd2 C52 138.2(5) . . . . ? Cl1 Pd1 Pd2 C52 -43.8(5) . . . . ? P1 Pd1 Pd2 C53 134.99(18) . . . . ? Cl1 Pd1 Pd2 C53 -46.93(17) . . . . ? P1 Pd1 Pd2 C51 135.1(6) . . . . ? Cl1 Pd1 Pd2 C51 -46.8(6) . . . . ? P1 Pd1 Pd2 P2 -40.63(4) . . . . ? Cl1 Pd1 Pd2 P2 137.46(4) . . . . ? Cl1 Pd1 P1 O1 117.5(4) . . . . ? Pd2 Pd1 P1 O1 -83.24(12) . . . . ? Cl1 Pd1 P1 O2 1.6(4) . . . . ? Pd2 Pd1 P1 O2 160.83(10) . . . . ? Cl1 Pd1 P1 N1 -117.3(4) . . . . ? Pd2 Pd1 P1 N1 41.88(13) . . . . ? C52 Pd2 P2 O4 112.1(7) . . . . ? C53 Pd2 P2 O4 179(100) . . . . ? C51 Pd2 P2 O4 112.1(3) . . . . ? Pd1 Pd2 P2 O4 -69.64(13) . . . . ? C52 Pd2 P2 O3 -17.6(7) . . . . ? C53 Pd2 P2 O3 49(2) . . . . ? C51 Pd2 P2 O3 -17.5(3) . . . . ? Pd1 Pd2 P2 O3 160.68(12) . . . . ? C52 Pd2 P2 N1 -135.9(7) . . . . ? C53 Pd2 P2 N1 -69(2) . . . . ? C51 Pd2 P2 N1 -135.8(3) . . . . ? Pd1 Pd2 P2 N1 42.42(12) . . . . ? O2 P1 O1 C1 55.8(3) . . . . ? N1 P1 O1 C1 161.1(3) . . . . ? Pd1 P1 O1 C1 -64.6(3) . . . . ? O1 P1 O2 C13 -150.2(3) . . . . ? N1 P1 O2 C13 111.0(3) . . . . ? Pd1 P1 O2 C13 -17.3(3) . . . . ? O4 P2 O3 C27 -139.9(3) . . . . ? N1 P2 O3 C27 119.4(3) . . . . ? Pd2 P2 O3 C27 -0.1(3) . . . . ? O3 P2 O4 C39 68.0(4) . . . . ? N1 P2 O4 C39 174.5(3) . . . . ? Pd2 P2 O4 C39 -68.8(4) . . . . ? O4 P2 N1 C25 -73.7(4) . . . . ? O3 P2 N1 C25 29.5(4) . . . . ? Pd2 P2 N1 C25 156.7(3) . . . . ? O4 P2 N1 P1 108.33(19) . . . . ? O3 P2 N1 P1 -148.54(17) . . . . ? Pd2 P2 N1 P1 -21.30(19) . . . . ? O1 P1 N1 C25 -58.9(3) . . . . ? O2 P1 N1 C25 41.5(4) . . . . ? Pd1 P1 N1 C25 162.7(3) . . . . ? O1 P1 N1 P2 119.28(18) . . . . ? O2 P1 N1 P2 -140.35(17) . . . . ? Pd1 P1 N1 P2 -19.1(2) . . . . ? P1 O1 C1 C2 -101.9(4) . . . . ? P1 O1 C1 C6 83.6(4) . . . . ? C6 C1 C2 C3 -3.4(6) . . . . ? O1 C1 C2 C3 -177.7(3) . . . . ? C6 C1 C2 C10 171.1(4) . . . . ? O1 C1 C2 C10 -3.2(6) . . . . ? C1 C2 C3 C4 -0.3(6) . . . . ? C10 C2 C3 C4 -175.0(4) . . . . ? C2 C3 C4 C5 2.7(7) . . . . ? C3 C4 C5 C6 -1.5(7) . . . . ? C4 C5 C6 C1 -2.0(7) . . . . ? C4 C5 C6 C7 174.9(4) . . . . ? C2 C1 C6 C5 4.5(6) . . . . ? O1 C1 C6 C5 178.6(3) . . . . ? C2 C1 C6 C7 -172.3(4) . . . . ? O1 C1 C6 C7 1.8(6) . . . . ? C5 C6 C7 C9 48.8(6) . . . . ? C1 C6 C7 C9 -134.5(5) . . . . ? C5 C6 C7 C8 -74.9(6) . . . . ? C1 C6 C7 C8 101.9(5) . . . . ? C1 C2 C10 C12 140.5(5) . . . . ? C3 C2 C10 C12 -45.2(6) . . . . ? C1 C2 C10 C11 -93.1(5) . . . . ? C3 C2 C10 C11 81.2(6) . . . . ? P1 O2 C13 C18 -99.4(4) . . . . ? P1 O2 C13 C14 84.7(4) . . . . ? C18 C13 C14 C15 3.7(7) . . . . ? O2 C13 C14 C15 179.3(4) . . . . ? C18 C13 C14 C22 -172.1(5) . . . . ? O2 C13 C14 C22 3.5(7) . . . . ? C13 C14 C15 C16 0.7(9) . . . . ? C22 C14 C15 C16 176.7(6) . . . . ? C14 C15 C16 C17 -3.2(10) . . . . ? C15 C16 C17 C18 1.5(9) . . . . ? C16 C17 C18 C13 2.5(8) . . . . ? C16 C17 C18 C19 -173.3(5) . . . . ? C14 C13 C18 C17 -5.2(7) . . . . ? O2 C13 C18 C17 179.1(4) . . . . ? C14 C13 C18 C19 170.6(4) . . . . ? O2 C13 C18 C19 -5.1(6) . . . . ? C17 C18 C19 C21 103.6(5) . . . . ? C13 C18 C19 C21 -72.0(6) . . . . ? C17 C18 C19 C20 -21.0(7) . . . . ? C13 C18 C19 C20 163.4(5) . . . . ? C15 C14 C22 C24 -85.3(7) . . . . ? C13 C14 C22 C24 90.3(6) . . . . ? C15 C14 C22 C23 39.7(7) . . . . ? C13 C14 C22 C23 -144.7(5) . . . . ? P2 N1 C25 C26 24.6(9) . . . . ? P1 N1 C25 C26 -157.5(7) . . . . ? P2 O3 C27 C32 100.0(4) . . . . ? P2 O3 C27 C28 -85.3(5) . . . . ? C32 C27 C28 C29 -2.6(8) . . . . ? O3 C27 C28 C29 -177.1(4) . . . . ? C32 C27 C28 C36 174.6(5) . . . . ? O3 C27 C28 C36 0.1(7) . . . . ? C27 C28 C29 C30 0.7(9) . . . . ? C36 C28 C29 C30 -176.6(6) . . . . ? C28 C29 C30 C31 0.6(11) . . . . ? C29 C30 C31 C32 0.0(10) . . . . ? C28 C27 C32 C31 3.1(8) . . . . ? O3 C27 C32 C31 177.6(4) . . . . ? C28 C27 C32 C33 179.9(5) . . . . ? O3 C27 C32 C33 -5.6(7) . . . . ? C30 C31 C32 C27 -1.7(9) . . . . ? C30 C31 C32 C33 -178.7(6) . . . . ? C27 C32 C33 C35 -104.0(6) . . . . ? C31 C32 C33 C35 72.7(7) . . . . ? C27 C32 C33 C34 131.5(6) . . . . ? C31 C32 C33 C34 -51.8(7) . . . . ? C29 C28 C36 C38 -38.0(9) . . . . ? C27 C28 C36 C38 144.9(7) . . . . ? C29 C28 C36 C37 84.9(7) . . . . ? C27 C28 C36 C37 -92.2(7) . . . . ? P2 O4 C39 C44 77.1(5) . . . . ? P2 O4 C39 C40 -108.8(4) . . . . ? C44 C39 C40 C41 -4.8(8) . . . . ? O4 C39 C40 C41 -178.6(5) . . . . ? C44 C39 C40 C48 170.6(5) . . . . ? O4 C39 C40 C48 -3.1(8) . . . . ? C39 C40 C41 C42 1.0(9) . . . . ? C48 C40 C41 C42 -174.5(6) . . . . ? C40 C41 C42 C43 2.0(11) . . . . ? C41 C42 C43 C44 -1.6(11) . . . . ? C40 C39 C44 C43 5.3(8) . . . . ? O4 C39 C44 C43 179.0(4) . . . . ? C40 C39 C44 C45 -170.2(5) . . . . ? O4 C39 C44 C45 3.5(7) . . . . ? C42 C43 C44 C39 -1.9(9) . . . . ? C42 C43 C44 C45 173.5(6) . . . . ? C39 C44 C45 C46 81.9(6) . . . . ? C43 C44 C45 C46 -93.3(6) . . . . ? C39 C44 C45 C47 -154.2(6) . . . . ? C43 C44 C45 C47 30.7(8) . . . . ? C41 C40 C48 C49 -54.6(9) . . . . ? C39 C40 C48 C49 130.1(7) . . . . ? C41 C40 C48 C50 69.1(8) . . . . ? C39 C40 C48 C50 -106.1(7) . . . . ? C53 Pd2 C51 C52 4.8(8) . . . . ? P2 Pd2 C51 C52 -180.0(8) . . . . ? Pd1 Pd2 C51 C52 4.6(12) . . . . ? Pd2 C51 C52 C53 -16(3) . . . . ? C53 Pd2 C52 C51 -172.2(14) . . . . ? P2 Pd2 C52 C51 0.1(13) . . . . ? Pd1 Pd2 C52 C51 -177.8(6) . . . . ? C51 Pd2 C52 C53 172.2(14) . . . . ? P2 Pd2 C52 C53 172.2(3) . . . . ? Pd1 Pd2 C52 C53 -5.7(9) . . . . ? C51 C52 C53 Pd2 16(3) . . . . ? C51 Pd2 C53 C52 -4.6(8) . . . . ? P2 Pd2 C53 C52 -73(2) . . . . ? Pd1 Pd2 C53 C52 175.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.167 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.085 data_complex2_ _database_code_depnum_ccdc_archive 'CCDC 637406' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C115 H172 Cl10 N2 O10 P4 Pd8' _chemical_formula_sum 'C115 H172 Cl10 N2 O10 P4 Pd8' _chemical_formula_weight 3072.13 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.714(3) _cell_length_b 15.294(3) _cell_length_c 16.424(3) _cell_angle_alpha 78.172(4) _cell_angle_beta 81.154(4) _cell_angle_gamma 80.768(4) _cell_volume 3301.8(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 28.0 _exptl_crystal_description rhombus _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1554 _exptl_absorpt_coefficient_mu 1.366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4946 _exptl_absorpt_correction_T_max 0.6848 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker Smart Apex CCD' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38813 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.02 _reflns_number_total 15311 _reflns_number_gt 11056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart Apex CCD' _computing_cell_refinement 'Bruker Smart Apex CCD' _computing_data_reduction 'Bruker Saint' _computing_structure_solution Shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ortep-iii _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1388P)^2^+16.2472P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15311 _refine_ls_number_parameters 711 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2411 _refine_ls_wR_factor_gt 0.2210 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.005 _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 Pd1 Pd 0.62851(7) 0.47400(6) 0.01233(6) 0.0807(3) Uani 1 1 d . . . Pd2 Pd 0.67272(4) 0.29659(3) 0.16642(3) 0.03620(13) Uani 1 1 d . . . Pd3 Pd 0.68024(4) 0.28692(4) 0.32106(3) 0.03830(14) Uani 1 1 d . . . Pd4 Pd 0.49209(6) 0.26151(5) 0.48275(5) 0.0632(2) Uani 1 1 d . . . Cl1 Cl 0.52357(17) 0.59075(16) -0.08332(15) 0.0628(5) Uani 1 1 d . . . Cl2 Cl 0.62009(17) 0.31513(15) 0.02773(13) 0.0566(5) Uani 1 1 d . . . Cl3 Cl 0.59037(16) 0.44977(13) 0.16378(14) 0.0542(5) Uani 1 1 d . . . Cl4 Cl 0.50082(15) 0.29673(17) 0.33369(15) 0.0616(5) Uani 1 1 d . . . Cl5 Cl 0.65029(18) 0.3121(2) 0.46543(15) 0.0700(7) Uani 1 1 d . . . P1 P 0.77139(12) 0.17064(11) 0.18115(10) 0.0296(3) Uani 1 1 d . . . P2 P 0.84015(13) 0.25323(11) 0.29521(10) 0.0316(3) Uani 1 1 d . . . O1 O 0.7370(3) 0.0772(3) 0.2328(3) 0.0353(10) Uani 1 1 d . . . O2 O 0.8260(4) 0.1392(3) 0.0954(3) 0.0362(10) Uani 1 1 d . . . O3 O 0.9003(4) 0.2121(3) 0.3740(3) 0.0387(10) Uani 1 1 d . . . O4 O 0.9144(4) 0.3225(3) 0.2432(3) 0.0370(10) Uani 1 1 d . . . O5 O 0.2848(13) 0.5610(16) 0.3147(11) 0.107(6) Uani 0.50 1 d P . . O6 O 0.4849(19) 0.4115(19) 0.386(2) 0.200(16) Uani 0.50 1 d P . . N1 N 0.8677(4) 0.1741(3) 0.2342(3) 0.0300(11) Uani 1 1 d . . . C1 C 0.6937(5) 0.0115(4) 0.2070(4) 0.0381(15) Uani 1 1 d . . . C2 C 0.5893(6) 0.0226(6) 0.2085(6) 0.0512(19) Uani 1 1 d . . . C3 C 0.5510(8) -0.0456(7) 0.1834(7) 0.071(3) Uani 1 1 d . . . H3 H 0.4829 -0.0407 0.1816 0.085 Uiso 1 1 calc R . . C4 C 0.6109(9) -0.1184(7) 0.1617(7) 0.076(3) Uani 1 1 d . . . H4 H 0.5835 -0.1615 0.1431 0.091 Uiso 1 1 calc R . . C5 C 0.7108(8) -0.1301(6) 0.1665(6) 0.066(3) Uani 1 1 d . . . H5 H 0.7502 -0.1817 0.1526 0.080 Uiso 1 1 calc R . . C6 C 0.7542(6) -0.0661(5) 0.1919(5) 0.0467(17) Uani 1 1 d . . . C7 C 0.5208(6) 0.1015(6) 0.2374(6) 0.059(2) Uani 1 1 d . . . H7 H 0.5624 0.1423 0.2500 0.071 Uiso 1 1 calc R . . C8 C 0.4560(8) 0.0676(8) 0.3182(8) 0.083(3) Uani 1 1 d . . . H8A H 0.4146 0.0272 0.3077 0.125 Uiso 1 1 calc R . . H8B H 0.4148 0.1178 0.3381 0.125 Uiso 1 1 calc R . . H8C H 0.4977 0.0364 0.3599 0.125 Uiso 1 1 calc R . . C9 C 0.4554(9) 0.1554(9) 0.1727(9) 0.091(4) Uani 1 1 d . . . H9A H 0.4964 0.1743 0.1212 0.136 Uiso 1 1 calc R . . H9B H 0.4191 0.2074 0.1930 0.136 Uiso 1 1 calc R . . H9C H 0.4095 0.1185 0.1632 0.136 Uiso 1 1 calc R . . C10 C 0.8633(7) -0.0830(6) 0.2024(6) 0.056(2) Uani 1 1 d . . . H10 H 0.8755 -0.0361 0.2308 0.068 Uiso 1 1 calc R . . C11 C 0.9337(8) -0.0769(7) 0.1222(8) 0.080(3) Uani 1 1 d . . . H11A H 0.9308 -0.1268 0.0959 0.121 Uiso 1 1 calc R . . H11B H 1.0003 -0.0784 0.1344 0.121 Uiso 1 1 calc R . . H11C H 0.9149 -0.0214 0.0851 0.121 Uiso 1 1 calc R . . C12 C 0.8900(9) -0.1744(7) 0.2606(8) 0.083(3) Uani 1 1 d . . . H12A H 0.8537 -0.1736 0.3153 0.125 Uiso 1 1 calc R . . H12B H 0.9602 -0.1841 0.2646 0.125 Uiso 1 1 calc R . . H12C H 0.8728 -0.2221 0.2379 0.125 Uiso 1 1 calc R . . C13 C 0.8282(5) 0.1849(5) 0.0104(4) 0.0379(15) Uani 1 1 d . . . C14 C 0.8792(6) 0.2588(5) -0.0192(5) 0.0447(16) Uani 1 1 d . . . C15 C 0.8789(7) 0.2997(6) -0.1023(5) 0.059(2) Uani 1 1 d . . . H15 H 0.9111 0.3504 -0.1226 0.071 Uiso 1 1 calc R . . C16 C 0.8323(8) 0.2672(7) -0.1553(5) 0.068(3) Uani 1 1 d . . . H16 H 0.8322 0.2957 -0.2110 0.082 Uiso 1 1 calc R . . C17 C 0.7858(7) 0.1923(7) -0.1256(5) 0.061(2) Uani 1 1 d . . . H17 H 0.7552 0.1700 -0.1623 0.073 Uiso 1 1 calc R . . C18 C 0.7827(6) 0.1485(6) -0.0428(5) 0.0494(18) Uani 1 1 d . . . C19 C 0.9387(6) 0.2969(6) 0.0347(5) 0.0495(18) Uani 1 1 d . . . H19 H 0.9271 0.2652 0.0929 0.059 Uiso 1 1 calc R . . C20 C 1.0503(8) 0.2782(9) 0.0030(8) 0.086(3) Uani 1 1 d . . . H20A H 1.0685 0.2148 0.0033 0.129 Uiso 1 1 calc R . . H20B H 1.0886 0.2969 0.0390 0.129 Uiso 1 1 calc R . . H20C H 1.0633 0.3111 -0.0530 0.129 Uiso 1 1 calc R . . C21 C 0.9079(10) 0.3990(6) 0.0327(7) 0.081(3) Uani 1 1 d . . . H21A H 0.9192 0.4311 -0.0239 0.121 Uiso 1 1 calc R . . H21B H 0.9468 0.4194 0.0672 0.121 Uiso 1 1 calc R . . H21C H 0.8386 0.4100 0.0535 0.121 Uiso 1 1 calc R . . C22 C 0.7282(7) 0.0654(6) -0.0140(6) 0.058(2) Uani 1 1 d . . . H22 H 0.7316 0.0439 0.0461 0.069 Uiso 1 1 calc R . . C23 C 0.6198(8) 0.0866(9) -0.0285(8) 0.090(4) Uani 1 1 d . . . H23A H 0.5885 0.1362 -0.0020 0.135 Uiso 1 1 calc R . . H23B H 0.5867 0.0347 -0.0052 0.135 Uiso 1 1 calc R . . H23C H 0.6155 0.1025 -0.0877 0.135 Uiso 1 1 calc R . . C24 C 0.7790(11) -0.0112(7) -0.0618(7) 0.088(4) Uani 1 1 d . . . H24A H 0.7711 0.0071 -0.1202 0.133 Uiso 1 1 calc R . . H24B H 0.7485 -0.0648 -0.0391 0.133 Uiso 1 1 calc R . . H24C H 0.8486 -0.0231 -0.0555 0.133 Uiso 1 1 calc R . . C25 C 0.8654(6) 0.1860(5) 0.4613(4) 0.0473(18) Uani 1 1 d . . . C26 C 0.8163(8) 0.1091(6) 0.4902(5) 0.056(2) Uani 1 1 d . . . C27 C 0.7878(10) 0.0875(7) 0.5743(6) 0.076(3) Uani 1 1 d . . . H27 H 0.7540 0.0380 0.5952 0.091 Uiso 1 1 calc R . . C28 C 0.8083(10) 0.1381(9) 0.6295(6) 0.092(4) Uani 1 1 d . . . H28 H 0.7905 0.1209 0.6869 0.111 Uiso 1 1 calc R . . C29 C 0.8543(9) 0.2126(7) 0.5998(6) 0.073(3) Uani 1 1 d . . . H29 H 0.8634 0.2478 0.6372 0.088 Uiso 1 1 calc R . . C30 C 0.8884(7) 0.2381(6) 0.5152(5) 0.054(2) Uani 1 1 d . . . C31 C 0.7993(8) 0.0481(6) 0.4342(6) 0.064(3) Uani 1 1 d . . . H31 H 0.8240 0.0743 0.3766 0.076 Uiso 1 1 calc R . . C32 C 0.6855(9) 0.0444(8) 0.4373(7) 0.080(3) Uani 1 1 d . . . H32A H 0.6594 0.0169 0.4926 0.121 Uiso 1 1 calc R . . H32B H 0.6757 0.0094 0.3975 0.121 Uiso 1 1 calc R . . H32C H 0.6515 0.1044 0.4235 0.121 Uiso 1 1 calc R . . C33 C 0.8586(11) -0.0441(7) 0.4557(7) 0.091(4) Uani 1 1 d . . . H33A H 0.9282 -0.0383 0.4492 0.136 Uiso 1 1 calc R . . H33B H 0.8475 -0.0818 0.4188 0.136 Uiso 1 1 calc R . . H33C H 0.8378 -0.0707 0.5127 0.136 Uiso 1 1 calc R . . C34 C 0.9438(8) 0.3166(6) 0.4874(5) 0.059(2) Uani 1 1 d . . . H34 H 0.9692 0.3189 0.4279 0.071 Uiso 1 1 calc R . . C35 C 0.8761(10) 0.4046(7) 0.4954(8) 0.084(3) Uani 1 1 d . . . H35A H 0.8191 0.4084 0.4669 0.127 Uiso 1 1 calc R . . H35B H 0.9119 0.4545 0.4708 0.127 Uiso 1 1 calc R . . H35C H 0.8546 0.4062 0.5536 0.127 Uiso 1 1 calc R . . C36 C 1.0325(9) 0.3093(8) 0.5349(7) 0.082(3) Uani 1 1 d . . . H36A H 1.0092 0.3130 0.5925 0.123 Uiso 1 1 calc R . . H36B H 1.0706 0.3577 0.5102 0.123 Uiso 1 1 calc R . . H36C H 1.0735 0.2527 0.5321 0.123 Uiso 1 1 calc R . . C37 C 0.9567(6) 0.3904(5) 0.2658(4) 0.0415(16) Uani 1 1 d . . . C38 C 0.9047(7) 0.4756(5) 0.2642(5) 0.0497(18) Uani 1 1 d . . . C39 C 0.9557(8) 0.5407(6) 0.2823(6) 0.066(3) Uani 1 1 d . . . H39 H 0.9225 0.5984 0.2841 0.079 Uiso 1 1 calc R . . C40 C 1.0529(8) 0.5212(7) 0.2972(6) 0.068(3) Uani 1 1 d . . . H40 H 1.0850 0.5658 0.3083 0.081 Uiso 1 1 calc R . . C41 C 1.1025(8) 0.4377(7) 0.2960(6) 0.067(3) Uani 1 1 d . . . H41 H 1.1690 0.4263 0.3052 0.081 Uiso 1 1 calc R . . C42 C 1.0577(6) 0.3692(6) 0.2815(5) 0.0504(19) Uani 1 1 d . . . C43 C 0.8001(7) 0.5014(5) 0.2427(6) 0.055(2) Uani 1 1 d . . . H43 H 0.7797 0.4484 0.2283 0.066 Uiso 1 1 calc R . . C44 C 0.7963(9) 0.5762(7) 0.1655(7) 0.076(3) Uani 1 1 d . . . H44A H 0.8149 0.6296 0.1778 0.114 Uiso 1 1 calc R . . H44B H 0.7299 0.5889 0.1503 0.114 Uiso 1 1 calc R . . H44C H 0.8416 0.5573 0.1198 0.114 Uiso 1 1 calc R . . C45 C 0.7256(9) 0.5285(9) 0.3150(7) 0.084(3) Uani 1 1 d . . . H45A H 0.7157 0.4763 0.3575 0.126 Uiso 1 1 calc R . . H45B H 0.6633 0.5546 0.2948 0.126 Uiso 1 1 calc R . . H45C H 0.7507 0.5719 0.3382 0.126 Uiso 1 1 calc R . . C46 C 1.1181(6) 0.2771(7) 0.2761(6) 0.062(2) Uani 1 1 d . . . H46 H 1.0706 0.2336 0.2845 0.074 Uiso 1 1 calc R . . C47 C 1.1891(11) 0.2434(11) 0.3422(9) 0.109(5) Uani 1 1 d . . . H47A H 1.1961 0.1787 0.3557 0.164 Uiso 1 1 calc R . . H47B H 1.1629 0.2677 0.3918 0.164 Uiso 1 1 calc R . . H47C H 1.2530 0.2625 0.3207 0.164 Uiso 1 1 calc R . . C48 C 1.1755(11) 0.2751(10) 0.1941(8) 0.100(4) Uani 1 1 d . . . H48A H 1.1357 0.3069 0.1513 0.150 Uiso 1 1 calc R . . H48B H 1.1944 0.2137 0.1868 0.150 Uiso 1 1 calc R . . H48C H 1.2341 0.3034 0.1900 0.150 Uiso 1 1 calc R . . C49 C 0.9705(6) 0.1286(5) 0.2126(5) 0.0474(17) Uani 1 1 d . . . H49A H 1.0141 0.1748 0.1935 0.057 Uiso 1 1 calc R . . H49B H 0.9698 0.0992 0.1657 0.057 Uiso 1 1 calc R . . C50 C 1.0159(6) 0.0590(6) 0.2820(6) 0.059(2) Uani 1 1 d . . . H50A H 1.0204 0.0875 0.3279 0.089 Uiso 1 1 calc R . . H50B H 1.0812 0.0338 0.2607 0.089 Uiso 1 1 calc R . . H50C H 0.9745 0.0119 0.3010 0.089 Uiso 1 1 calc R . . C51 C 0.6782(10) 0.5081(10) -0.1190(8) 0.093(4) Uani 1 1 d . . . C52 C 0.6371(15) 0.5787(17) -0.0883(12) 0.152(8) Uani 1 1 d . . . C53 C 0.6526(10) 0.6148(9) -0.0222(8) 0.090(4) Uani 1 1 d . . . C54 C 0.3450(13) 0.2190(15) 0.5165(12) 0.144(7) Uani 1 1 d . . . C55 C 0.3985(16) 0.1905(18) 0.5782(13) 0.179(11) Uani 1 1 d . . . C56 C 0.4568(17) 0.2301(15) 0.6141(9) 0.155(8) Uani 1 1 d . . . C57 C 0.402(3) 0.523(2) 0.384(2) 0.148(16) Uani 0.50 1 d P . . C58 C 0.3567(18) 0.568(2) 0.327(2) 0.108(12) Uani 0.50 1 d P . . C59 C 0.416(3) 0.637(3) 0.261(3) 0.16(2) Uani 0.50 1 d P . . 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 0.0799(6) 0.0767(6) 0.0795(6) -0.0015(4) -0.0137(4) -0.0057(4) Pd2 0.0355(3) 0.0324(3) 0.0396(3) -0.0070(2) -0.0068(2) 0.0014(2) Pd3 0.0369(3) 0.0390(3) 0.0393(3) -0.0131(2) 0.0011(2) -0.0041(2) Pd4 0.0685(5) 0.0603(4) 0.0613(4) -0.0146(3) 0.0050(3) -0.0177(3) Cl1 0.0574(12) 0.0627(13) 0.0621(13) -0.0019(10) -0.0121(10) 0.0029(10) Cl2 0.0603(12) 0.0566(12) 0.0523(11) -0.0150(9) -0.0163(9) 0.0087(9) Cl3 0.0602(12) 0.0396(9) 0.0604(12) -0.0115(8) -0.0135(9) 0.0088(8) Cl4 0.0396(10) 0.0783(15) 0.0661(13) -0.0211(11) 0.0017(9) -0.0030(10) Cl5 0.0569(13) 0.1032(19) 0.0593(13) -0.0429(13) 0.0038(10) -0.0130(12) P1 0.0319(8) 0.0282(8) 0.0304(8) -0.0086(6) -0.0039(6) -0.0046(6) P2 0.0372(8) 0.0298(8) 0.0295(8) -0.0087(6) -0.0023(6) -0.0078(6) O1 0.041(2) 0.031(2) 0.037(2) -0.0060(18) -0.005(2) -0.0113(19) O2 0.043(3) 0.035(2) 0.032(2) -0.0092(19) -0.0051(19) -0.005(2) O3 0.047(3) 0.044(3) 0.029(2) -0.008(2) -0.009(2) -0.010(2) O4 0.042(3) 0.035(2) 0.036(2) -0.0071(19) -0.004(2) -0.013(2) O5 0.066(10) 0.18(2) 0.087(12) -0.037(12) -0.016(9) -0.012(11) O6 0.14(2) 0.17(2) 0.32(4) -0.18(3) 0.11(2) -0.075(18) N1 0.031(3) 0.032(3) 0.031(3) -0.013(2) -0.005(2) -0.006(2) C1 0.044(4) 0.032(3) 0.041(4) -0.008(3) -0.008(3) -0.010(3) C2 0.044(4) 0.053(5) 0.061(5) -0.013(4) -0.013(4) -0.012(3) C3 0.068(6) 0.063(6) 0.094(8) -0.021(5) -0.025(5) -0.023(5) C4 0.090(8) 0.058(6) 0.097(8) -0.027(5) -0.030(6) -0.027(5) C5 0.091(7) 0.042(5) 0.076(6) -0.027(4) -0.018(5) -0.011(5) C6 0.052(4) 0.041(4) 0.047(4) -0.011(3) -0.005(3) -0.005(3) C7 0.038(4) 0.060(5) 0.083(6) -0.021(5) 0.001(4) -0.014(4) C8 0.062(6) 0.092(8) 0.091(8) -0.020(7) 0.003(6) -0.005(6) C9 0.076(8) 0.083(8) 0.107(10) -0.006(7) -0.016(7) -0.005(6) C10 0.058(5) 0.046(4) 0.069(6) -0.023(4) -0.016(4) 0.008(4) C11 0.063(6) 0.064(6) 0.108(9) -0.023(6) 0.002(6) 0.009(5) C12 0.096(8) 0.062(6) 0.088(8) -0.007(6) -0.029(7) 0.006(6) C13 0.037(3) 0.044(4) 0.032(3) -0.012(3) -0.002(3) -0.002(3) C14 0.056(4) 0.042(4) 0.036(4) -0.007(3) -0.004(3) -0.007(3) C15 0.075(6) 0.060(5) 0.039(4) -0.006(4) 0.001(4) -0.015(4) C16 0.087(7) 0.081(7) 0.033(4) -0.001(4) -0.010(4) -0.011(6) C17 0.070(6) 0.079(6) 0.037(4) -0.018(4) -0.012(4) -0.008(5) C18 0.046(4) 0.062(5) 0.043(4) -0.020(4) -0.005(3) -0.001(4) C19 0.058(5) 0.052(5) 0.041(4) -0.008(3) 0.001(3) -0.021(4) C20 0.065(6) 0.118(10) 0.086(8) -0.032(7) 0.001(6) -0.038(7) C21 0.127(10) 0.048(5) 0.074(7) -0.007(5) -0.020(7) -0.029(6) C22 0.068(6) 0.065(5) 0.050(5) -0.021(4) -0.015(4) -0.013(4) C23 0.071(7) 0.119(10) 0.098(9) -0.033(8) -0.021(6) -0.038(7) C24 0.129(11) 0.064(7) 0.077(7) -0.020(6) -0.016(7) -0.015(7) C25 0.062(5) 0.052(4) 0.029(3) -0.007(3) -0.007(3) -0.010(4) C26 0.084(6) 0.049(5) 0.037(4) -0.004(3) -0.010(4) -0.018(4) C27 0.121(9) 0.062(6) 0.045(5) -0.005(4) 0.000(5) -0.035(6) C28 0.118(10) 0.119(10) 0.035(5) -0.008(6) -0.001(6) -0.019(8) C29 0.107(8) 0.080(7) 0.042(5) -0.015(5) -0.012(5) -0.032(6) C30 0.076(6) 0.056(5) 0.033(4) -0.008(3) -0.014(4) -0.013(4) C31 0.104(8) 0.044(4) 0.046(5) 0.002(4) -0.004(5) -0.034(5) C32 0.093(8) 0.082(7) 0.068(6) 0.002(5) 0.001(6) -0.047(6) C33 0.147(12) 0.044(5) 0.075(7) -0.003(5) -0.008(7) -0.009(6) C34 0.085(6) 0.060(5) 0.041(4) -0.018(4) -0.014(4) -0.018(5) C35 0.110(9) 0.062(6) 0.087(8) -0.007(6) -0.041(7) -0.012(6) C36 0.090(8) 0.087(8) 0.079(7) -0.023(6) -0.026(6) -0.018(6) C37 0.053(4) 0.045(4) 0.032(3) -0.007(3) -0.004(3) -0.023(3) C38 0.065(5) 0.038(4) 0.049(4) -0.008(3) -0.008(4) -0.015(4) C39 0.092(7) 0.040(4) 0.074(6) -0.009(4) -0.020(5) -0.026(5) C40 0.079(7) 0.064(6) 0.074(6) -0.015(5) -0.019(5) -0.036(5) C41 0.064(6) 0.082(7) 0.063(6) -0.005(5) -0.013(5) -0.039(5) C42 0.050(4) 0.054(5) 0.050(4) -0.002(4) -0.010(4) -0.020(4) C43 0.064(5) 0.038(4) 0.065(5) -0.008(4) -0.016(4) -0.008(4) C44 0.101(8) 0.055(6) 0.069(6) 0.003(5) -0.022(6) -0.011(5) C45 0.080(8) 0.090(8) 0.076(7) -0.007(6) -0.009(6) -0.007(6) C46 0.042(4) 0.068(6) 0.076(6) -0.008(5) -0.006(4) -0.014(4) C47 0.099(10) 0.120(11) 0.105(10) -0.030(9) -0.028(8) 0.025(8) C48 0.113(11) 0.102(10) 0.079(8) -0.029(7) 0.014(7) -0.009(8) C49 0.047(4) 0.052(4) 0.046(4) -0.017(3) -0.010(3) -0.002(3) C50 0.046(4) 0.062(5) 0.072(6) -0.020(4) -0.019(4) 0.008(4) C51 0.097(9) 0.103(10) 0.063(7) -0.008(6) 0.021(6) -0.005(7) C52 0.136(15) 0.21(2) 0.122(14) -0.033(14) 0.047(12) -0.118(16) C53 0.101(9) 0.085(8) 0.085(8) 0.005(7) -0.011(7) -0.040(7) C54 0.110(12) 0.21(2) 0.104(12) 0.029(12) 0.010(10) -0.086(13) C55 0.145(17) 0.27(3) 0.116(14) 0.065(16) -0.012(12) -0.133(19) C56 0.20(2) 0.22(2) 0.057(8) 0.003(10) 0.018(10) -0.122(18) C57 0.21(4) 0.11(2) 0.13(3) -0.10(2) -0.07(3) 0.10(2) C58 0.057(13) 0.14(2) 0.17(3) -0.13(2) -0.049(17) 0.023(15) C59 0.09(2) 0.16(3) 0.29(6) -0.15(4) -0.11(3) 0.05(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 C52 2.06(2) . ? Pd1 C51 2.142(12) . ? Pd1 C53 2.177(12) . ? Pd1 Cl2 2.410(2) . ? Pd1 Cl3 2.425(2) . ? Pd1 Cl1 2.476(2) 2_665 ? Pd1 Cl1 2.539(2) . ? Pd2 P1 2.1618(16) . ? Pd2 Cl3 2.4270(19) . ? Pd2 Cl2 2.442(2) . ? Pd2 Pd3 2.5309(9) . ? Pd3 P2 2.1669(18) . ? Pd3 Cl4 2.420(2) . ? Pd3 Cl5 2.442(2) . ? Pd4 C55 2.100(14) . ? Pd4 C56 2.109(14) . ? Pd4 C54 2.175(15) . ? Pd4 Cl5 2.376(2) . ? Pd4 Cl4 2.385(2) . ? Pd4 O6 2.51(4) . ? Cl1 C52 1.53(2) . ? Cl1 Cl3 2.419(3) 2_665 ? Cl1 Cl2 2.421(3) 2_665 ? Cl1 Pd1 2.476(2) 2_665 ? Cl2 Cl1 2.421(3) 2_665 ? Cl3 Cl1 2.419(3) 2_665 ? Cl4 O6 2.07(2) . ? P1 O1 1.607(5) . ? P1 O2 1.616(5) . ? P1 N1 1.703(5) . ? P2 O3 1.606(5) . ? P2 O4 1.611(5) . ? P2 N1 1.687(5) . ? O1 C1 1.408(8) . ? O2 C13 1.425(8) . ? O3 C25 1.437(8) . ? O4 C37 1.404(8) . ? O5 C58 1.06(3) . ? O6 C57 1.88(4) . ? N1 C49 1.493(9) . ? C1 C6 1.379(10) . ? C1 C2 1.411(11) . ? C2 C3 1.398(12) . ? C2 C7 1.516(12) . ? C3 C4 1.349(15) . ? C3 H3 0.9300 . ? C4 C5 1.366(15) . ? C4 H4 0.9300 . ? C5 C6 1.385(11) . ? C5 H5 0.9300 . ? C6 C10 1.508(12) . ? C7 C9 1.518(15) . ? C7 C8 1.525(14) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.504(14) . ? C10 C12 1.549(13) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.389(10) . ? C13 C18 1.393(10) . ? C14 C15 1.380(11) . ? C14 C19 1.541(11) . ? C15 C16 1.365(13) . ? C15 H15 0.9300 . ? C16 C17 1.366(14) . ? C16 H16 0.9300 . ? C17 C18 1.384(12) . ? C17 H17 0.9300 . ? C18 C22 1.533(12) . ? C19 C20 1.539(13) . ? C19 C21 1.546(13) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.515(14) . ? C22 C24 1.556(14) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C30 1.404(11) . ? C25 C26 1.410(12) . ? C26 C27 1.363(12) . ? C26 C31 1.503(12) . ? C27 C28 1.391(15) . ? C27 H27 0.9300 . ? C28 C29 1.357(16) . ? C28 H28 0.9300 . ? C29 C30 1.392(12) . ? C29 H29 0.9300 . ? C30 C34 1.479(12) . ? C31 C33 1.514(14) . ? C31 C32 1.564(15) . ? C31 H31 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C36 1.522(14) . ? C34 C35 1.524(15) . ? C34 H34 0.9800 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.378(11) . ? C37 C42 1.423(11) . ? C38 C39 1.405(11) . ? C38 C43 1.502(12) . ? C39 C40 1.367(14) . ? C39 H39 0.9300 . ? C40 C41 1.350(15) . ? C40 H40 0.9300 . ? C41 C42 1.372(12) . ? C41 H41 0.9300 . ? C42 C46 1.527(13) . ? C43 C45 1.524(15) . ? C43 C44 1.525(13) . ? C43 H43 0.9800 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C48 1.456(15) . ? C46 C47 1.524(16) . ? C46 H46 0.9800 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.527(11) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.29(2) . ? C52 C53 1.37(2) . ? C54 C55 1.30(3) . ? C55 C56 1.34(3) . ? C57 C58 1.24(4) . ? C58 C59 1.57(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C52 Pd1 C51 35.8(7) . . ? C52 Pd1 C53 37.7(6) . . ? C51 Pd1 C53 69.2(5) . . ? C52 Pd1 Cl2 134.2(6) . . ? C51 Pd1 Cl2 101.2(4) . . ? C53 Pd1 Cl2 169.9(4) . . ? C52 Pd1 Cl3 139.5(7) . . ? C51 Pd1 Cl3 171.2(4) . . ? C53 Pd1 Cl3 103.9(4) . . ? Cl2 Pd1 Cl3 85.31(7) . . ? C52 Pd1 Cl1 126.7(6) . 2_665 ? C51 Pd1 Cl1 129.3(4) . 2_665 ? C53 Pd1 Cl1 128.9(4) . 2_665 ? Cl2 Pd1 Cl1 59.39(8) . 2_665 ? Cl3 Pd1 Cl1 59.15(8) . 2_665 ? C52 Pd1 Cl1 37.0(6) . . ? C51 Pd1 Cl1 59.4(4) . . ? C53 Pd1 Cl1 57.1(4) . . ? Cl2 Pd1 Cl1 121.46(8) . . ? Cl3 Pd1 Cl1 122.13(7) . . ? Cl1 Pd1 Cl1 89.78(8) 2_665 . ? P1 Pd2 Cl3 166.96(7) . . ? P1 Pd2 Cl2 105.12(6) . . ? Cl3 Pd2 Cl2 84.58(7) . . ? P1 Pd2 Pd3 84.78(4) . . ? Cl3 Pd2 Pd3 87.46(5) . . ? Cl2 Pd2 Pd3 165.39(5) . . ? P2 Pd3 Cl4 166.98(7) . . ? P2 Pd3 Cl5 105.27(7) . . ? Cl4 Pd3 Cl5 84.39(8) . . ? P2 Pd3 Pd2 87.47(4) . . ? Cl4 Pd3 Pd2 84.62(6) . . ? Cl5 Pd3 Pd2 164.14(7) . . ? C55 Pd4 C56 37.2(8) . . ? C55 Pd4 C54 35.5(7) . . ? C56 Pd4 C54 69.1(7) . . ? C55 Pd4 Cl5 138.1(6) . . ? C56 Pd4 Cl5 103.3(6) . . ? C54 Pd4 Cl5 171.9(6) . . ? C55 Pd4 Cl4 134.0(7) . . ? C56 Pd4 Cl4 169.7(6) . . ? C54 Pd4 Cl4 100.9(5) . . ? Cl5 Pd4 Cl4 86.62(8) . . ? C55 Pd4 O6 138.3(9) . . ? C56 Pd4 O6 130.0(8) . . ? C54 Pd4 O6 110.9(8) . . ? Cl5 Pd4 O6 71.5(7) . . ? Cl4 Pd4 O6 50.1(6) . . ? C52 Cl1 Cl3 133.7(8) . 2_665 ? C52 Cl1 Cl2 139.2(9) . 2_665 ? Cl3 Cl1 Cl2 85.20(10) 2_665 2_665 ? C52 Cl1 Pd1 144.1(8) . 2_665 ? Cl3 Cl1 Pd1 59.38(8) 2_665 2_665 ? Cl2 Cl1 Pd1 58.95(8) 2_665 2_665 ? C52 Cl1 Pd1 54.0(8) . . ? Cl3 Cl1 Pd1 122.48(11) 2_665 . ? Cl2 Cl1 Pd1 121.57(11) 2_665 . ? Pd1 Cl1 Pd1 90.22(8) 2_665 . ? Pd1 Cl2 Cl1 61.66(8) . 2_665 ? Pd1 Cl2 Pd2 87.51(7) . . ? Cl1 Cl2 Pd2 84.80(9) 2_665 . ? Cl1 Cl3 Pd1 61.48(8) 2_665 . ? Cl1 Cl3 Pd2 85.17(9) 2_665 . ? Pd1 Cl3 Pd2 87.52(7) . . ? O6 Cl4 Pd4 68.0(11) . . ? O6 Cl4 Pd3 90.6(7) . . ? Pd4 Cl4 Pd3 90.53(8) . . ? Pd4 Cl5 Pd3 90.22(8) . . ? O1 P1 O2 100.4(2) . . ? O1 P1 N1 98.5(3) . . ? O2 P1 N1 103.6(3) . . ? O1 P1 Pd2 123.33(19) . . ? O2 P1 Pd2 115.95(19) . . ? N1 P1 Pd2 112.17(19) . . ? O3 P2 O4 99.1(3) . . ? O3 P2 N1 104.2(3) . . ? O4 P2 N1 98.2(3) . . ? O3 P2 Pd3 117.3(2) . . ? O4 P2 Pd3 124.6(2) . . ? N1 P2 Pd3 110.30(19) . . ? C1 O1 P1 130.5(4) . . ? C13 O2 P1 130.8(4) . . ? C25 O3 P2 130.7(5) . . ? C37 O4 P2 132.3(4) . . ? C57 O6 Cl4 139(2) . . ? C57 O6 Pd4 134.9(18) . . ? Cl4 O6 Pd4 61.9(8) . . ? C49 N1 P2 123.9(4) . . ? C49 N1 P1 122.6(4) . . ? P2 N1 P1 111.9(3) . . ? C6 C1 O1 117.8(6) . . ? C6 C1 C2 122.9(7) . . ? O1 C1 C2 118.7(6) . . ? C3 C2 C1 115.8(8) . . ? C3 C2 C7 120.9(8) . . ? C1 C2 C7 123.3(7) . . ? C4 C3 C2 121.3(9) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 121.3(9) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 120.8(9) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 117.3(8) . . ? C1 C6 C10 122.7(7) . . ? C5 C6 C10 120.0(8) . . ? C2 C7 C9 114.1(9) . . ? C2 C7 C8 109.4(8) . . ? C9 C7 C8 109.8(9) . . ? C2 C7 H7 107.8 . . ? C9 C7 H7 107.8 . . ? C8 C7 H7 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C6 115.4(8) . . ? C11 C10 C12 109.7(8) . . ? C6 C10 C12 111.4(8) . . ? C11 C10 H10 106.6 . . ? C6 C10 H10 106.6 . . ? C12 C10 H10 106.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 121.5(7) . . ? C14 C13 O2 121.3(6) . . ? C18 C13 O2 117.1(7) . . ? C15 C14 C13 118.4(7) . . ? C15 C14 C19 117.6(7) . . ? C13 C14 C19 123.9(7) . . ? C16 C15 C14 121.2(9) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 119.3(8) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 122.3(8) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C17 C18 C13 117.1(8) . . ? C17 C18 C22 119.3(8) . . ? C13 C18 C22 123.6(7) . . ? C20 C19 C14 108.5(7) . . ? C20 C19 C21 110.0(8) . . ? C14 C19 C21 112.7(8) . . ? C20 C19 H19 108.5 . . ? C14 C19 H19 108.5 . . ? C21 C19 H19 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C18 111.8(8) . . ? C23 C22 C24 108.6(9) . . ? C18 C22 C24 110.3(8) . . ? C23 C22 H22 108.7 . . ? C18 C22 H22 108.7 . . ? C24 C22 H22 108.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 C26 123.1(7) . . ? C30 C25 O3 116.0(7) . . ? C26 C25 O3 120.8(6) . . ? C27 C26 C25 117.2(8) . . ? C27 C26 C31 119.1(8) . . ? C25 C26 C31 123.6(7) . . ? C26 C27 C28 121.3(10) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C29 C28 C27 120.1(9) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 122.3(9) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C29 C30 C25 115.8(8) . . ? C29 C30 C34 119.7(8) . . ? C25 C30 C34 124.5(7) . . ? C26 C31 C33 110.6(9) . . ? C26 C31 C32 110.6(9) . . ? C33 C31 C32 112.9(9) . . ? C26 C31 H31 107.5 . . ? C33 C31 H31 107.5 . . ? C32 C31 H31 107.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 C36 112.6(8) . . ? C30 C34 C35 111.4(9) . . ? C36 C34 C35 109.4(8) . . ? C30 C34 H34 107.8 . . ? C36 C34 H34 107.8 . . ? C35 C34 H34 107.8 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 O4 120.5(7) . . ? C38 C37 C42 122.5(7) . . ? O4 C37 C42 116.6(7) . . ? C37 C38 C39 116.4(8) . . ? C37 C38 C43 123.7(7) . . ? C39 C38 C43 119.9(8) . . ? C40 C39 C38 121.6(9) . . ? C40 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? C41 C40 C39 120.4(8) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C42 122.0(9) . . ? C40 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? C41 C42 C37 117.0(8) . . ? C41 C42 C46 120.2(8) . . ? C37 C42 C46 122.6(7) . . ? C38 C43 C45 113.4(8) . . ? C38 C43 C44 110.6(8) . . ? C45 C43 C44 110.3(8) . . ? C38 C43 H43 107.4 . . ? C45 C43 H43 107.4 . . ? C44 C43 H43 107.4 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C48 C46 C47 108.0(10) . . ? C48 C46 C42 112.2(9) . . ? C47 C46 C42 114.6(9) . . ? C48 C46 H46 107.2 . . ? C47 C46 H46 107.2 . . ? C42 C46 H46 107.2 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N1 C49 C50 116.9(7) . . ? N1 C49 H49A 108.1 . . ? C50 C49 H49A 108.1 . . ? N1 C49 H49B 108.1 . . ? C50 C49 H49B 108.1 . . ? H49A C49 H49B 107.3 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 Pd1 68.5(10) . . ? C51 C52 C53 134(2) . . ? C51 C52 Cl1 112.0(15) . . ? C53 C52 Cl1 103.2(15) . . ? C51 C52 Pd1 75.7(13) . . ? C53 C52 Pd1 75.9(11) . . ? Cl1 C52 Pd1 88.9(6) . . ? C52 C53 Pd1 66.3(10) . . ? C55 C54 Pd4 69.2(10) . . ? C54 C55 C56 133(2) . . ? C54 C55 Pd4 75.4(10) . . ? C56 C55 Pd4 71.8(9) . . ? C55 C56 Pd4 71.1(10) . . ? C58 C57 O6 129(2) . . ? O5 C58 C57 126(5) . . ? O5 C58 C59 117(3) . . ? C57 C58 C59 116(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 P1 Pd2 Pd3 P2 46.26(6) . . . . ? Cl3 Pd2 Pd3 P2 -123.25(7) . . . . ? Cl2 Pd2 Pd3 P2 179.8(2) . . . . ? P1 Pd2 Pd3 Cl4 -123.38(7) . . . . ? Cl3 Pd2 Pd3 Cl4 67.11(8) . . . . ? Cl2 Pd2 Pd3 Cl4 10.1(2) . . . . ? P1 Pd2 Pd3 Cl5 -169.7(2) . . . . ? Cl3 Pd2 Pd3 Cl5 20.8(2) . . . . ? Cl2 Pd2 Pd3 Cl5 -36.2(3) . . . . ? C51 Pd1 Cl1 C52 -38.8(11) . . . . ? C53 Pd1 Cl1 C52 45.0(11) . . . . ? Cl2 Pd1 Cl1 C52 -123.2(11) . . . . ? Cl3 Pd1 Cl1 C52 131.1(11) . . . . ? Cl1 Pd1 Cl1 C52 -176.3(11) 2_665 . . . ? C52 Pd1 Cl1 Cl3 123.3(11) . . . 2_665 ? C51 Pd1 Cl1 Cl3 84.5(5) . . . 2_665 ? C53 Pd1 Cl1 Cl3 168.3(5) . . . 2_665 ? Cl2 Pd1 Cl1 Cl3 0.14(16) . . . 2_665 ? Cl3 Pd1 Cl1 Cl3 -105.58(12) . . . 2_665 ? Cl1 Pd1 Cl1 Cl3 -53.03(10) 2_665 . . 2_665 ? C52 Pd1 Cl1 Cl2 -130.7(11) . . . 2_665 ? C51 Pd1 Cl1 Cl2 -169.5(5) . . . 2_665 ? C53 Pd1 Cl1 Cl2 -85.7(5) . . . 2_665 ? Cl2 Pd1 Cl1 Cl2 106.09(13) . . . 2_665 ? Cl3 Pd1 Cl1 Cl2 0.37(17) . . . 2_665 ? Cl1 Pd1 Cl1 Cl2 52.92(11) 2_665 . . 2_665 ? C52 Pd1 Cl1 Pd1 176.3(11) . . . 2_665 ? C51 Pd1 Cl1 Pd1 137.6(5) . . . 2_665 ? C53 Pd1 Cl1 Pd1 -138.6(5) . . . 2_665 ? Cl2 Pd1 Cl1 Pd1 53.17(11) . . . 2_665 ? Cl3 Pd1 Cl1 Pd1 -52.55(11) . . . 2_665 ? Cl1 Pd1 Cl1 Pd1 0.0 2_665 . . 2_665 ? C52 Pd1 Cl2 Cl1 -113.2(8) . . . 2_665 ? C51 Pd1 Cl2 Cl1 -129.3(4) . . . 2_665 ? C53 Pd1 Cl2 Cl1 -147(2) . . . 2_665 ? Cl3 Pd1 Cl2 Cl1 56.68(8) . . . 2_665 ? Cl1 Pd1 Cl2 Cl1 -68.45(12) . . . 2_665 ? C52 Pd1 Cl2 Pd2 161.4(8) . . . . ? C51 Pd1 Cl2 Pd2 145.3(4) . . . . ? C53 Pd1 Cl2 Pd2 127(2) . . . . ? Cl3 Pd1 Cl2 Pd2 -28.76(7) . . . . ? Cl1 Pd1 Cl2 Pd2 -85.43(9) 2_665 . . . ? Cl1 Pd1 Cl2 Pd2 -153.88(7) . . . . ? P1 Pd2 Cl2 Pd1 -142.37(6) . . . . ? Cl3 Pd2 Cl2 Pd1 28.77(7) . . . . ? Pd3 Pd2 Cl2 Pd1 86.1(2) . . . . ? P1 Pd2 Cl2 Cl1 155.87(8) . . . 2_665 ? Cl3 Pd2 Cl2 Cl1 -32.99(9) . . . 2_665 ? Pd3 Pd2 Cl2 Cl1 24.3(3) . . . 2_665 ? C52 Pd1 Cl3 Cl1 111.9(8) . . . 2_665 ? C53 Pd1 Cl3 Cl1 127.3(4) . . . 2_665 ? Cl2 Pd1 Cl3 Cl1 -56.90(8) . . . 2_665 ? Cl1 Pd1 Cl3 Cl1 67.64(12) . . . 2_665 ? C52 Pd1 Cl3 Pd2 -162.2(8) . . . . ? C53 Pd1 Cl3 Pd2 -146.9(4) . . . . ? Cl2 Pd1 Cl3 Pd2 28.95(7) . . . . ? Cl1 Pd1 Cl3 Pd2 85.85(8) 2_665 . . . ? Cl1 Pd1 Cl3 Pd2 153.49(7) . . . . ? P1 Pd2 Cl3 Cl1 171.8(3) . . . 2_665 ? Cl2 Pd2 Cl3 Cl1 33.00(9) . . . 2_665 ? Pd3 Pd2 Cl3 Cl1 -134.74(8) . . . 2_665 ? P1 Pd2 Cl3 Pd1 110.2(3) . . . . ? Cl2 Pd2 Cl3 Pd1 -28.58(7) . . . . ? Pd3 Pd2 Cl3 Pd1 163.69(5) . . . . ? C55 Pd4 Cl4 O6 123.1(14) . . . . ? C56 Pd4 Cl4 O6 95(4) . . . . ? C54 Pd4 Cl4 O6 108.3(10) . . . . ? Cl5 Pd4 Cl4 O6 -68.6(8) . . . . ? C55 Pd4 Cl4 Pd3 -146.5(11) . . . . ? C56 Pd4 Cl4 Pd3 -174(4) . . . . ? C54 Pd4 Cl4 Pd3 -161.3(6) . . . . ? Cl5 Pd4 Cl4 Pd3 21.77(9) . . . . ? O6 Pd4 Cl4 Pd3 90.4(8) . . . . ? P2 Pd3 Cl4 O6 -174.7(11) . . . . ? Cl5 Pd3 Cl4 O6 46.7(11) . . . . ? Pd2 Pd3 Cl4 O6 -121.8(11) . . . . ? P2 Pd3 Cl4 Pd4 117.4(3) . . . . ? Cl5 Pd3 Cl4 Pd4 -21.22(9) . . . . ? Pd2 Pd3 Cl4 Pd4 170.23(7) . . . . ? C55 Pd4 Cl5 Pd3 145.8(13) . . . . ? C56 Pd4 Cl5 Pd3 161.4(7) . . . . ? Cl4 Pd4 Cl5 Pd3 -21.57(9) . . . . ? O6 Pd4 Cl5 Pd3 -70.5(6) . . . . ? P2 Pd3 Cl5 Pd4 -149.81(7) . . . . ? Cl4 Pd3 Cl5 Pd4 21.31(9) . . . . ? Pd2 Pd3 Cl5 Pd4 67.6(3) . . . . ? Cl3 Pd2 P1 O1 123.7(3) . . . . ? Cl2 Pd2 P1 O1 -99.1(2) . . . . ? Pd3 Pd2 P1 O1 69.9(2) . . . . ? Cl3 Pd2 P1 O2 -112.3(3) . . . . ? Cl2 Pd2 P1 O2 24.9(2) . . . . ? Pd3 Pd2 P1 O2 -166.0(2) . . . . ? Cl3 Pd2 P1 N1 6.4(4) . . . . ? Cl2 Pd2 P1 N1 143.6(2) . . . . ? Pd3 Pd2 P1 N1 -47.3(2) . . . . ? Cl4 Pd3 P2 O3 -112.8(4) . . . . ? Cl5 Pd3 P2 O3 24.1(2) . . . . ? Pd2 Pd3 P2 O3 -165.4(2) . . . . ? Cl4 Pd3 P2 O4 122.3(4) . . . . ? Cl5 Pd3 P2 O4 -100.7(2) . . . . ? Pd2 Pd3 P2 O4 69.7(2) . . . . ? Cl4 Pd3 P2 N1 6.2(4) . . . . ? Cl5 Pd3 P2 N1 143.2(2) . . . . ? Pd2 Pd3 P2 N1 -46.4(2) . . . . ? O2 P1 O1 C1 -43.3(6) . . . . ? N1 P1 O1 C1 -148.9(6) . . . . ? Pd2 P1 O1 C1 87.4(6) . . . . ? O1 P1 O2 C13 142.4(6) . . . . ? N1 P1 O2 C13 -116.2(6) . . . . ? Pd2 P1 O2 C13 7.1(6) . . . . ? O4 P2 O3 C25 142.5(6) . . . . ? N1 P2 O3 C25 -116.6(6) . . . . ? Pd3 P2 O3 C25 5.7(6) . . . . ? O3 P2 O4 C37 -52.0(7) . . . . ? N1 P2 O4 C37 -157.9(6) . . . . ? Pd3 P2 O4 C37 80.4(7) . . . . ? Pd4 Cl4 O6 C57 -127(3) . . . . ? Pd3 Cl4 O6 C57 142(3) . . . . ? Pd3 Cl4 O6 Pd4 -90.3(3) . . . . ? C55 Pd4 O6 C57 18(3) . . . . ? C56 Pd4 O6 C57 -33(3) . . . . ? C54 Pd4 O6 C57 46(3) . . . . ? Cl5 Pd4 O6 C57 -125(3) . . . . ? Cl4 Pd4 O6 C57 133(3) . . . . ? C55 Pd4 O6 Cl4 -115.0(12) . . . . ? C56 Pd4 O6 Cl4 -166.5(8) . . . . ? C54 Pd4 O6 Cl4 -86.8(8) . . . . ? Cl5 Pd4 O6 Cl4 101.4(5) . . . . ? O3 P2 N1 C49 -46.3(6) . . . . ? O4 P2 N1 C49 55.3(6) . . . . ? Pd3 P2 N1 C49 -173.0(5) . . . . ? O3 P2 N1 P1 147.8(3) . . . . ? O4 P2 N1 P1 -110.6(3) . . . . ? Pd3 P2 N1 P1 21.1(3) . . . . ? O1 P1 N1 C49 86.0(6) . . . . ? O2 P1 N1 C49 -16.9(6) . . . . ? Pd2 P1 N1 C49 -142.6(5) . . . . ? O1 P1 N1 P2 -107.9(3) . . . . ? O2 P1 N1 P2 149.2(3) . . . . ? Pd2 P1 N1 P2 23.5(3) . . . . ? P1 O1 C1 C6 102.2(7) . . . . ? P1 O1 C1 C2 -86.0(8) . . . . ? C6 C1 C2 C3 -7.7(12) . . . . ? O1 C1 C2 C3 -179.0(8) . . . . ? C6 C1 C2 C7 170.7(8) . . . . ? O1 C1 C2 C7 -0.7(12) . . . . ? C1 C2 C3 C4 1.9(15) . . . . ? C7 C2 C3 C4 -176.5(10) . . . . ? C2 C3 C4 C5 2.6(18) . . . . ? C3 C4 C5 C6 -1.6(18) . . . . ? O1 C1 C6 C5 -180.0(7) . . . . ? C2 C1 C6 C5 8.6(12) . . . . ? O1 C1 C6 C10 0.3(11) . . . . ? C2 C1 C6 C10 -171.1(8) . . . . ? C4 C5 C6 C1 -3.8(14) . . . . ? C4 C5 C6 C10 176.0(10) . . . . ? C3 C2 C7 C9 -58.3(12) . . . . ? C1 C2 C7 C9 123.4(10) . . . . ? C3 C2 C7 C8 65.1(12) . . . . ? C1 C2 C7 C8 -113.1(10) . . . . ? C1 C6 C10 C11 -107.5(9) . . . . ? C5 C6 C10 C11 72.7(11) . . . . ? C1 C6 C10 C12 126.5(9) . . . . ? C5 C6 C10 C12 -53.2(11) . . . . ? P1 O2 C13 C14 69.9(9) . . . . ? P1 O2 C13 C18 -114.2(7) . . . . ? C18 C13 C14 C15 4.0(12) . . . . ? O2 C13 C14 C15 179.7(7) . . . . ? C18 C13 C14 C19 -174.5(7) . . . . ? O2 C13 C14 C19 1.2(11) . . . . ? C13 C14 C15 C16 -1.9(14) . . . . ? C19 C14 C15 C16 176.6(9) . . . . ? C14 C15 C16 C17 -0.5(16) . . . . ? C15 C16 C17 C18 1.1(16) . . . . ? C16 C17 C18 C13 0.9(14) . . . . ? C16 C17 C18 C22 179.4(9) . . . . ? C14 C13 C18 C17 -3.5(12) . . . . ? O2 C13 C18 C17 -179.3(7) . . . . ? C14 C13 C18 C22 178.1(7) . . . . ? O2 C13 C18 C22 2.2(11) . . . . ? C15 C14 C19 C20 -67.5(11) . . . . ? C13 C14 C19 C20 111.0(9) . . . . ? C15 C14 C19 C21 54.6(11) . . . . ? C13 C14 C19 C21 -126.9(9) . . . . ? C17 C18 C22 C23 -58.5(11) . . . . ? C13 C18 C22 C23 119.9(9) . . . . ? C17 C18 C22 C24 62.5(11) . . . . ? C13 C18 C22 C24 -119.1(9) . . . . ? P2 O3 C25 C30 -113.1(8) . . . . ? P2 O3 C25 C26 70.6(10) . . . . ? C30 C25 C26 C27 2.2(15) . . . . ? O3 C25 C26 C27 178.3(9) . . . . ? C30 C25 C26 C31 -174.4(9) . . . . ? O3 C25 C26 C31 1.6(14) . . . . ? C25 C26 C27 C28 -1.5(17) . . . . ? C31 C26 C27 C28 175.4(11) . . . . ? C26 C27 C28 C29 2(2) . . . . ? C27 C28 C29 C30 -4(2) . . . . ? C28 C29 C30 C25 4.8(17) . . . . ? C28 C29 C30 C34 -176.0(12) . . . . ? C26 C25 C30 C29 -3.8(14) . . . . ? O3 C25 C30 C29 180.0(8) . . . . ? C26 C25 C30 C34 177.0(9) . . . . ? O3 C25 C30 C34 0.8(13) . . . . ? C27 C26 C31 C33 -63.1(13) . . . . ? C25 C26 C31 C33 113.5(11) . . . . ? C27 C26 C31 C32 62.8(12) . . . . ? C25 C26 C31 C32 -120.6(10) . . . . ? C29 C30 C34 C36 53.7(13) . . . . ? C25 C30 C34 C36 -127.2(10) . . . . ? C29 C30 C34 C35 -69.6(12) . . . . ? C25 C30 C34 C35 109.6(10) . . . . ? P2 O4 C37 C38 -84.5(8) . . . . ? P2 O4 C37 C42 101.8(7) . . . . ? O4 C37 C38 C39 -175.7(7) . . . . ? C42 C37 C38 C39 -2.4(12) . . . . ? O4 C37 C38 C43 2.7(12) . . . . ? C42 C37 C38 C43 176.1(8) . . . . ? C37 C38 C39 C40 2.5(14) . . . . ? C43 C38 C39 C40 -176.0(9) . . . . ? C38 C39 C40 C41 -0.8(16) . . . . ? C39 C40 C41 C42 -1.3(16) . . . . ? C40 C41 C42 C37 1.5(14) . . . . ? C40 C41 C42 C46 176.8(9) . . . . ? C38 C37 C42 C41 0.5(12) . . . . ? O4 C37 C42 C41 174.1(7) . . . . ? C38 C37 C42 C46 -174.8(8) . . . . ? O4 C37 C42 C46 -1.2(11) . . . . ? C37 C38 C43 C45 116.1(10) . . . . ? C39 C38 C43 C45 -65.5(11) . . . . ? C37 C38 C43 C44 -119.4(9) . . . . ? C39 C38 C43 C44 59.0(11) . . . . ? C41 C42 C46 C48 -81.0(12) . . . . ? C37 C42 C46 C48 94.1(11) . . . . ? C41 C42 C46 C47 42.6(13) . . . . ? C37 C42 C46 C47 -142.3(10) . . . . ? P2 N1 C49 C50 73.3(8) . . . . ? P1 N1 C49 C50 -122.3(7) . . . . ? C53 Pd1 C51 C52 -23.1(11) . . . . ? Cl2 Pd1 C51 C52 160.2(11) . . . . ? Cl1 Pd1 C51 C52 100.8(12) 2_665 . . . ? Cl1 Pd1 C51 C52 40.1(10) . . . . ? Pd1 C51 C52 C53 53.7(17) . . . . ? Pd1 C51 C52 Cl1 -82.9(11) . . . . ? Cl3 Cl1 C52 C51 -29(2) 2_665 . . . ? Cl2 Cl1 C52 C51 172.7(8) 2_665 . . . ? Pd1 Cl1 C52 C51 68(2) 2_665 . . . ? Pd1 Cl1 C52 C51 74.1(15) . . . . ? Cl3 Cl1 C52 C53 -178.3(7) 2_665 . . . ? Cl2 Cl1 C52 C53 23(2) 2_665 . . . ? Pd1 Cl1 C52 C53 -82(2) 2_665 . . . ? Pd1 Cl1 C52 C53 -75.3(12) . . . . ? Cl3 Cl1 C52 Pd1 -103.0(8) 2_665 . . . ? Cl2 Cl1 C52 Pd1 98.6(11) 2_665 . . . ? Pd1 Cl1 C52 Pd1 -6.2(18) 2_665 . . . ? C53 Pd1 C52 C51 143.1(18) . . . . ? Cl2 Pd1 C52 C51 -27.7(15) . . . . ? Cl3 Pd1 C52 C51 168.0(7) . . . . ? Cl1 Pd1 C52 C51 -108.4(11) 2_665 . . . ? Cl1 Pd1 C52 C51 -113.0(15) . . . . ? C51 Pd1 C52 C53 -143.1(18) . . . . ? Cl2 Pd1 C52 C53 -170.8(7) . . . . ? Cl3 Pd1 C52 C53 24.9(15) . . . . ? Cl1 Pd1 C52 C53 108.4(9) 2_665 . . . ? Cl1 Pd1 C52 C53 103.9(15) . . . . ? C51 Pd1 C52 Cl1 113.0(15) . . . . ? C53 Pd1 C52 Cl1 -103.9(15) . . . . ? Cl2 Pd1 C52 Cl1 85.3(12) . . . . ? Cl3 Pd1 C52 Cl1 -79.0(11) . . . . ? Cl1 Pd1 C52 Cl1 4.6(14) 2_665 . . . ? C51 C52 C53 Pd1 -53.6(18) . . . . ? Cl1 C52 C53 Pd1 85.5(9) . . . . ? C51 Pd1 C53 C52 22.1(12) . . . . ? Cl2 Pd1 C53 C52 41(3) . . . . ? Cl3 Pd1 C53 C52 -163.6(11) . . . . ? Cl1 Pd1 C53 C52 -102.3(11) 2_665 . . . ? Cl1 Pd1 C53 C52 -44.1(11) . . . . ? C56 Pd4 C54 C55 -21.0(19) . . . . ? Cl4 Pd4 C54 C55 161.5(18) . . . . ? O6 Pd4 C54 C55 -147.2(18) . . . . ? Pd4 C54 C55 C56 46(3) . . . . ? C56 Pd4 C55 C54 146(3) . . . . ? Cl5 Pd4 C55 C54 172.0(12) . . . . ? Cl4 Pd4 C55 C54 -26(2) . . . . ? O6 Pd4 C55 C54 49(3) . . . . ? C54 Pd4 C55 C56 -146(3) . . . . ? Cl5 Pd4 C55 C56 26(2) . . . . ? Cl4 Pd4 C55 C56 -172.0(12) . . . . ? O6 Pd4 C55 C56 -96.9(19) . . . . ? C54 C55 C56 Pd4 -47(3) . . . . ? C54 Pd4 C56 C55 20.1(18) . . . . ? Cl5 Pd4 C56 C55 -162.7(16) . . . . ? Cl4 Pd4 C56 C55 34(5) . . . . ? O6 Pd4 C56 C55 120.4(18) . . . . ? Cl4 O6 C57 C58 -29(7) . . . . ? Pd4 O6 C57 C58 -127(4) . . . . ? O6 C57 C58 O5 86(5) . . . . ? O6 C57 C58 C59 -88(5) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.636 _refine_diff_density_min -3.086 _refine_diff_density_rms 0.178 ### END data_complex3_ _database_code_depnum_ccdc_archive 'CCDC 637407' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H79 Cl2 N O5 P2 Pd2' _chemical_formula_sum 'C53 H79 Cl2 N O5 P2 Pd2' _chemical_formula_weight 1155.81 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6926(13) _cell_length_b 22.839(3) _cell_length_c 24.066(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.332(2) _cell_angle_gamma 90.00 _cell_volume 5814.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.0 _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7077 _exptl_absorpt_correction_T_max 0.8115 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Bruker Smart Apex CCD' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51983 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.98 _reflns_number_total 13990 _reflns_number_gt 10207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart Apex CCD' _computing_cell_refinement 'Bruker Smart Apex CCD' _computing_data_reduction 'Bruker Saint' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-iii _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^)+(0.0504P)^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 13990 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.003 _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 C1 C 0.0062(4) 0.32918(17) 0.02545(15) 0.0401(9) Uani 1 1 d . . . C2 C 0.0829(4) 0.30017(18) -0.00756(16) 0.0486(10) Uani 1 1 d . . . C3 C 0.0229(5) 0.2689(2) -0.05314(19) 0.0675(14) Uani 1 1 d . . . H3 H 0.0717 0.2496 -0.0764 0.081 Uiso 1 1 calc R . . C4 C -0.1054(6) 0.2656(2) -0.0648(2) 0.0767(16) Uani 1 1 d . . . H4 H -0.1433 0.2430 -0.0947 0.092 Uiso 1 1 calc R . . C5 C -0.1778(5) 0.2958(2) -0.0323(2) 0.0702(14) Uani 1 1 d . . . H5 H -0.2653 0.2939 -0.0410 0.084 Uiso 1 1 calc R . . C6 C -0.1249(4) 0.3294(2) 0.01383(17) 0.0529(11) Uani 1 1 d . . . C7 C -0.2084(4) 0.3659(3) 0.0463(2) 0.0745(16) Uani 1 1 d . . . H7 H -0.1562 0.3785 0.0811 0.089 Uiso 1 1 calc R . . C8 C -0.2497(7) 0.4213(3) 0.0123(3) 0.136(3) Uani 1 1 d . . . H8A H -0.1769 0.4399 0.0010 0.204 Uiso 1 1 calc R . . H8B H -0.2901 0.4478 0.0351 0.204 Uiso 1 1 calc R . . H8C H -0.3079 0.4108 -0.0204 0.204 Uiso 1 1 calc R . . C9 C -0.3184(6) 0.3328(4) 0.0626(4) 0.156(4) Uani 1 1 d . . . H9A H -0.3689 0.3176 0.0295 0.234 Uiso 1 1 calc R . . H9B H -0.3688 0.3586 0.0818 0.234 Uiso 1 1 calc R . . H9C H -0.2881 0.3010 0.0870 0.234 Uiso 1 1 calc R . . C10 C 0.2266(4) 0.3045(2) 0.00271(18) 0.0560(12) Uani 1 1 d . . . H10 H 0.2501 0.3231 0.0394 0.067 Uiso 1 1 calc R . . C11 C 0.2754(6) 0.3434(3) -0.0404(3) 0.104(2) Uani 1 1 d . . . H11A H 0.3661 0.3442 -0.0335 0.156 Uiso 1 1 calc R . . H11B H 0.2432 0.3824 -0.0376 0.156 Uiso 1 1 calc R . . H11C H 0.2477 0.3283 -0.0773 0.156 Uiso 1 1 calc R . . C12 C 0.2899(5) 0.2447(2) 0.0055(2) 0.0866(18) Uani 1 1 d . . . H12A H 0.2725 0.2260 -0.0305 0.130 Uiso 1 1 calc R . . H12B H 0.2576 0.2211 0.0332 0.130 Uiso 1 1 calc R . . H12C H 0.3795 0.2494 0.0156 0.130 Uiso 1 1 calc R . . C13 C 0.1858(4) 0.22789(16) 0.15589(17) 0.0402(9) Uani 1 1 d . . . C14 C 0.0941(4) 0.18515(18) 0.14417(17) 0.0467(10) Uani 1 1 d . . . C15 C 0.1154(5) 0.1322(2) 0.1733(2) 0.0605(12) Uani 1 1 d . . . H15 H 0.0561 0.1023 0.1663 0.073 Uiso 1 1 calc R . . C16 C 0.2206(5) 0.1232(2) 0.2117(2) 0.0672(14) Uani 1 1 d . . . H16 H 0.2322 0.0876 0.2306 0.081 Uiso 1 1 calc R . . C17 C 0.3092(4) 0.16653(19) 0.2222(2) 0.0618(13) Uani 1 1 d . . . H17 H 0.3809 0.1600 0.2483 0.074 Uiso 1 1 calc R . . C18 C 0.2942(4) 0.22007(18) 0.19484(18) 0.0482(10) Uani 1 1 d . . . C19 C 0.3954(4) 0.26713(19) 0.2054(2) 0.0591(13) Uani 1 1 d . . . H19 H 0.3541 0.3049 0.1961 0.071 Uiso 1 1 calc R . . C20 C 0.4928(6) 0.2586(3) 0.1663(3) 0.099(2) Uani 1 1 d . . . H20A H 0.5338 0.2214 0.1738 0.148 Uiso 1 1 calc R . . H20B H 0.5544 0.2893 0.1722 0.148 Uiso 1 1 calc R . . H20C H 0.4518 0.2595 0.1281 0.148 Uiso 1 1 calc R . . C21 C 0.4604(5) 0.2709(3) 0.2656(2) 0.0924(19) Uani 1 1 d . . . H21A H 0.3979 0.2710 0.2905 0.139 Uiso 1 1 calc R . . H21B H 0.5092 0.3062 0.2707 0.139 Uiso 1 1 calc R . . H21C H 0.5151 0.2377 0.2738 0.139 Uiso 1 1 calc R . . C22 C -0.0216(4) 0.1909(2) 0.1002(2) 0.0606(13) Uani 1 1 d . . . H22 H -0.0218 0.2307 0.0850 0.073 Uiso 1 1 calc R . . C23 C -0.0157(6) 0.1485(2) 0.0512(2) 0.100(2) Uani 1 1 d . . . H23A H 0.0653 0.1516 0.0387 0.151 Uiso 1 1 calc R . . H23B H -0.0809 0.1581 0.0208 0.151 Uiso 1 1 calc R . . H23C H -0.0277 0.1091 0.0634 0.151 Uiso 1 1 calc R . . C24 C -0.1429(5) 0.1833(3) 0.1250(3) 0.113(2) Uani 1 1 d . . . H24A H -0.1462 0.1444 0.1399 0.169 Uiso 1 1 calc R . . H24B H -0.2140 0.1894 0.0963 0.169 Uiso 1 1 calc R . . H24C H -0.1453 0.2113 0.1546 0.169 Uiso 1 1 calc R . . C25 C -0.1612(4) 0.4120(2) 0.2634(2) 0.0675(14) Uani 1 1 d . . . H25 H -0.1510 0.4161 0.3022 0.081 Uiso 1 1 calc R . . C26 C -0.2784(6) 0.4142(5) 0.2292(4) 0.190(5) Uani 1 1 d . . . H26A H -0.2789 0.3872 0.1986 0.285 Uiso 1 1 calc R . . H26B H -0.2931 0.4532 0.2147 0.285 Uiso 1 1 calc R . . H26C H -0.3438 0.4038 0.2508 0.285 Uiso 1 1 calc R . . C27 C 0.0111(4) 0.52704(17) 0.26331(17) 0.0432(10) Uani 1 1 d . . . C28 C -0.0409(5) 0.5495(2) 0.3090(2) 0.0625(13) Uani 1 1 d . . . C29 C -0.1273(5) 0.5944(2) 0.2983(3) 0.0785(16) Uani 1 1 d . . . H29 H -0.1649 0.6096 0.3277 0.094 Uiso 1 1 calc R . . C30 C -0.1588(5) 0.6171(2) 0.2458(3) 0.0758(16) Uani 1 1 d . . . H30 H -0.2188 0.6468 0.2397 0.091 Uiso 1 1 calc R . . C31 C -0.1030(4) 0.59659(19) 0.2020(2) 0.0621(13) Uani 1 1 d . . . H31 H -0.1244 0.6132 0.1666 0.075 Uiso 1 1 calc R . . C32 C -0.0141(4) 0.55095(17) 0.20938(18) 0.0472(10) Uani 1 1 d . . . C33 C 0.0497(5) 0.5325(2) 0.16038(18) 0.0581(12) Uani 1 1 d . . . H33 H 0.1114 0.5020 0.1739 0.070 Uiso 1 1 calc R . . C34 C 0.1223(6) 0.5828(2) 0.1378(2) 0.0871(18) Uani 1 1 d . . . H34A H 0.0649 0.6142 0.1257 0.131 Uiso 1 1 calc R . . H34B H 0.1610 0.5692 0.1066 0.131 Uiso 1 1 calc R . . H34C H 0.1865 0.5966 0.1669 0.131 Uiso 1 1 calc R . . C35 C -0.0436(6) 0.5057(2) 0.1134(2) 0.0899(19) Uani 1 1 d . . . H35A H -0.0966 0.4781 0.1290 0.135 Uiso 1 1 calc R . . H35B H 0.0019 0.4861 0.0873 0.135 Uiso 1 1 calc R . . H35C H -0.0950 0.5361 0.0943 0.135 Uiso 1 1 calc R . . C36 C -0.0013(7) 0.5297(3) 0.3691(2) 0.095(2) Uani 1 1 d . . . H36 H 0.0574 0.4968 0.3687 0.114 Uiso 1 1 calc R . . C37 C -0.1139(9) 0.5088(3) 0.3965(3) 0.148(3) Uani 1 1 d . . . H37A H -0.1691 0.5412 0.4003 0.223 Uiso 1 1 calc R . . H37B H -0.0841 0.4928 0.4329 0.223 Uiso 1 1 calc R . . H37C H -0.1591 0.4791 0.3734 0.223 Uiso 1 1 calc R . . C38 C 0.0680(7) 0.5791(3) 0.4039(3) 0.129(3) Uani 1 1 d . . . H38A H 0.1395 0.5913 0.3869 0.193 Uiso 1 1 calc R . . H38B H 0.0963 0.5653 0.4413 0.193 Uiso 1 1 calc R . . H38C H 0.0116 0.6116 0.4054 0.193 Uiso 1 1 calc R . . C39 C 0.1360(4) 0.36951(18) 0.35416(16) 0.0446(10) Uani 1 1 d . . . C40 C 0.0505(4) 0.3247(2) 0.36196(18) 0.0558(12) Uani 1 1 d . . . C41 C 0.0263(6) 0.3169(3) 0.4171(2) 0.0819(17) Uani 1 1 d . . . H41 H -0.0314 0.2885 0.4245 0.098 Uiso 1 1 calc R . . C42 C 0.0849(7) 0.3496(3) 0.4598(2) 0.094(2) Uani 1 1 d . . . H42 H 0.0646 0.3443 0.4958 0.113 Uiso 1 1 calc R . . C43 C 0.1734(6) 0.3904(3) 0.4511(2) 0.0837(18) Uani 1 1 d . . . H43 H 0.2142 0.4116 0.4815 0.100 Uiso 1 1 calc R . . C44 C 0.2039(5) 0.40091(19) 0.39757(18) 0.0589(12) Uani 1 1 d . . . C45 C 0.3138(5) 0.4397(2) 0.3875(2) 0.0719(16) Uani 1 1 d . . . H45 H 0.2872 0.4624 0.3533 0.086 Uiso 1 1 calc R . . C46 C 0.4270(5) 0.4017(3) 0.3774(2) 0.0907(19) Uani 1 1 d . . . H46A H 0.4532 0.3779 0.4099 0.136 Uiso 1 1 calc R . . H46B H 0.4957 0.4265 0.3705 0.136 Uiso 1 1 calc R . . H46C H 0.4028 0.3769 0.3454 0.136 Uiso 1 1 calc R . . C47 C 0.3573(7) 0.4833(3) 0.4352(3) 0.124(3) Uani 1 1 d . . . H47A H 0.2886 0.5088 0.4403 0.187 Uiso 1 1 calc R . . H47B H 0.4268 0.5060 0.4258 0.187 Uiso 1 1 calc R . . H47C H 0.3837 0.4621 0.4694 0.187 Uiso 1 1 calc R . . C48 C 0.0012(5) 0.2827(2) 0.3153(2) 0.0661(14) Uani 1 1 d . . . H48 H -0.0109 0.3049 0.2801 0.079 Uiso 1 1 calc R . . C49 C 0.0973(6) 0.2356(2) 0.3101(3) 0.0947(19) Uani 1 1 d . . . H49A H 0.1759 0.2532 0.3043 0.142 Uiso 1 1 calc R . . H49B H 0.0674 0.2108 0.2787 0.142 Uiso 1 1 calc R . . H49C H 0.1099 0.2126 0.3438 0.142 Uiso 1 1 calc R . . C50 C -0.1249(6) 0.2545(3) 0.3220(3) 0.127(3) Uani 1 1 d . . . H50A H -0.1134 0.2282 0.3534 0.191 Uiso 1 1 calc R . . H50B H -0.1564 0.2333 0.2885 0.191 Uiso 1 1 calc R . . H50C H -0.1844 0.2844 0.3283 0.191 Uiso 1 1 calc R . . C51 C 0.5352(6) 0.5757(3) 0.1826(3) 0.097(2) Uani 1 1 d . . . H51A H 0.5826 0.5446 0.1992 0.117 Uiso 1 1 calc R . . H51B H 0.5094 0.6054 0.2048 0.117 Uiso 1 1 calc R . . C52 C 0.5039(7) 0.5779(3) 0.1263(4) 0.107(2) Uani 1 1 d . . . H52 H 0.4392 0.6059 0.1102 0.128 Uiso 1 1 calc R . . C53 C 0.5406(6) 0.5347(3) 0.0925(3) 0.0905(19) Uani 1 1 d . . . H53A H 0.5880 0.5032 0.1083 0.109 Uiso 1 1 calc R . . H53B H 0.5180 0.5370 0.0537 0.109 Uiso 1 1 calc R . . Cl1 Cl 0.37157(10) 0.46687(5) 0.23848(5) 0.0550(3) Uani 1 1 d . . . Cl2 Cl 0.35982(11) 0.40703(5) 0.11357(5) 0.0607(3) Uani 1 1 d . . . H1 H -0.067(4) 0.3792(18) 0.2091(16) 0.041(13) Uiso 1 1 d . . . N1 N -0.0561(3) 0.40252(17) 0.23166(15) 0.0444(9) Uani 1 1 d . . . O1 O 0.1643(2) 0.37844(11) 0.29918(10) 0.0394(6) Uani 1 1 d . . . O2 O 0.0975(2) 0.48057(11) 0.27558(10) 0.0390(6) Uani 1 1 d . . . O3 O 0.1756(2) 0.28035(10) 0.12462(10) 0.0372(6) Uani 1 1 d . . . O4 O 0.0656(2) 0.36229(11) 0.07162(10) 0.0388(6) Uani 1 1 d . . . O5 O -0.0257(2) 0.31810(12) 0.15575(10) 0.0445(7) Uani 1 1 d . . . P1 P 0.09280(9) 0.41614(4) 0.24813(4) 0.0324(2) Uani 1 1 d . . . P2 P 0.09153(9) 0.33675(4) 0.13459(4) 0.0329(2) Uani 1 1 d . . . Pd1 Pd 0.21825(3) 0.404188(12) 0.182160(11) 0.03156(8) Uani 1 1 d . . . Pd2 Pd 0.44566(3) 0.496534(15) 0.154376(15) 0.05117(11) Uani 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 C1 0.046(2) 0.041(2) 0.033(2) 0.0027(17) 0.0044(17) 0.0018(18) C2 0.063(3) 0.047(3) 0.037(2) 0.0009(19) 0.011(2) 0.006(2) C3 0.091(4) 0.065(3) 0.046(3) -0.015(2) 0.011(3) 0.020(3) C4 0.095(4) 0.068(4) 0.059(3) -0.021(3) -0.014(3) 0.000(3) C5 0.061(3) 0.083(4) 0.061(3) -0.004(3) -0.012(3) -0.006(3) C6 0.052(3) 0.063(3) 0.042(2) 0.000(2) 0.001(2) 0.006(2) C7 0.044(3) 0.127(5) 0.050(3) -0.018(3) -0.001(2) 0.014(3) C8 0.176(7) 0.145(7) 0.076(4) -0.021(4) -0.015(4) 0.107(6) C9 0.076(5) 0.216(10) 0.189(9) -0.061(7) 0.063(5) -0.033(6) C10 0.055(3) 0.072(3) 0.045(2) 0.000(2) 0.019(2) 0.012(2) C11 0.082(4) 0.139(6) 0.096(5) 0.039(4) 0.033(4) -0.003(4) C12 0.084(4) 0.089(4) 0.090(4) -0.010(3) 0.022(3) 0.033(3) C13 0.043(2) 0.031(2) 0.049(2) -0.0015(18) 0.0151(18) 0.0025(18) C14 0.055(3) 0.041(2) 0.045(2) -0.0001(19) 0.011(2) -0.001(2) C15 0.068(3) 0.046(3) 0.070(3) 0.003(2) 0.015(3) -0.011(2) C16 0.078(4) 0.044(3) 0.081(4) 0.021(3) 0.013(3) 0.006(3) C17 0.059(3) 0.042(3) 0.080(3) 0.014(2) -0.003(2) 0.010(2) C18 0.048(3) 0.043(2) 0.054(3) 0.000(2) 0.007(2) 0.004(2) C19 0.045(3) 0.041(3) 0.088(4) 0.010(2) -0.002(2) 0.001(2) C20 0.087(4) 0.104(5) 0.110(5) 0.001(4) 0.029(4) -0.045(4) C21 0.074(4) 0.106(5) 0.093(4) -0.011(4) -0.006(3) -0.016(3) C22 0.066(3) 0.042(3) 0.070(3) 0.003(2) -0.004(2) -0.020(2) C23 0.137(6) 0.071(4) 0.080(4) -0.015(3) -0.029(4) -0.010(4) C24 0.060(4) 0.139(6) 0.137(6) 0.030(5) 0.004(4) -0.030(4) C25 0.042(3) 0.089(4) 0.076(3) -0.018(3) 0.024(2) -0.004(3) C26 0.043(4) 0.389(16) 0.142(7) 0.041(8) 0.026(4) 0.044(6) C27 0.042(2) 0.033(2) 0.055(3) -0.0041(19) 0.0062(19) 0.0021(18) C28 0.074(3) 0.048(3) 0.072(3) -0.005(2) 0.029(3) 0.014(2) C29 0.076(4) 0.063(4) 0.100(4) -0.017(3) 0.028(3) 0.022(3) C30 0.049(3) 0.047(3) 0.128(5) -0.019(3) 0.001(3) 0.017(2) C31 0.052(3) 0.043(3) 0.084(4) 0.000(2) -0.014(3) 0.008(2) C32 0.040(2) 0.037(2) 0.061(3) -0.003(2) -0.003(2) 0.0046(19) C33 0.078(3) 0.047(3) 0.047(3) 0.011(2) 0.002(2) 0.016(2) C34 0.104(5) 0.080(4) 0.082(4) 0.021(3) 0.029(3) -0.003(3) C35 0.128(5) 0.072(4) 0.065(3) -0.009(3) -0.001(3) 0.002(4) C36 0.141(6) 0.092(4) 0.061(3) -0.001(3) 0.045(4) 0.048(4) C37 0.226(10) 0.134(7) 0.104(6) 0.010(5) 0.089(7) 0.002(6) C38 0.160(7) 0.153(7) 0.072(4) -0.024(5) 0.011(4) 0.027(6) C39 0.057(3) 0.039(2) 0.038(2) 0.0034(18) 0.0094(19) 0.000(2) C40 0.065(3) 0.059(3) 0.046(3) 0.013(2) 0.016(2) -0.004(2) C41 0.095(4) 0.096(4) 0.061(3) 0.018(3) 0.032(3) -0.015(4) C42 0.126(6) 0.111(5) 0.052(3) 0.011(3) 0.037(4) -0.001(4) C43 0.125(5) 0.082(4) 0.039(3) -0.010(3) -0.007(3) 0.016(4) C44 0.081(3) 0.048(3) 0.045(2) 0.002(2) -0.002(2) -0.003(3) C45 0.091(4) 0.051(3) 0.062(3) 0.007(2) -0.029(3) -0.015(3) C46 0.077(4) 0.095(5) 0.092(4) 0.020(3) -0.013(3) -0.025(3) C47 0.167(7) 0.072(4) 0.112(5) -0.010(4) -0.054(5) -0.034(4) C48 0.078(3) 0.060(3) 0.060(3) 0.013(2) 0.009(3) -0.026(3) C49 0.126(5) 0.065(4) 0.094(5) -0.020(3) 0.019(4) -0.006(4) C50 0.113(6) 0.111(6) 0.157(7) 0.009(5) 0.017(5) -0.067(5) C51 0.114(5) 0.054(3) 0.123(6) 0.002(4) 0.015(4) -0.040(3) C52 0.124(6) 0.073(5) 0.127(6) 0.021(4) 0.030(5) -0.039(4) C53 0.118(5) 0.055(4) 0.112(5) 0.025(3) 0.063(4) -0.006(3) Cl1 0.0471(6) 0.0637(7) 0.0543(6) -0.0118(5) 0.0083(5) -0.0195(5) Cl2 0.0618(7) 0.0598(7) 0.0686(7) -0.0187(6) 0.0364(6) -0.0218(6) N1 0.0333(18) 0.052(2) 0.049(2) -0.0124(19) 0.0118(15) 0.0007(17) O1 0.0456(15) 0.0361(15) 0.0369(14) 0.0066(11) 0.0069(12) 0.0001(12) O2 0.0432(15) 0.0341(14) 0.0395(14) -0.0045(11) 0.0053(12) 0.0072(12) O3 0.0434(15) 0.0309(14) 0.0390(14) 0.0053(11) 0.0114(12) 0.0006(12) O4 0.0441(15) 0.0373(15) 0.0347(14) -0.0021(11) 0.0050(11) 0.0044(12) O5 0.0425(15) 0.0461(17) 0.0474(16) -0.0118(13) 0.0153(13) -0.0128(13) P1 0.0339(5) 0.0318(5) 0.0319(5) 0.0007(4) 0.0059(4) 0.0012(4) P2 0.0341(5) 0.0336(5) 0.0323(5) -0.0028(4) 0.0085(4) -0.0019(4) Pd1 0.03059(15) 0.03037(15) 0.03467(15) -0.00083(12) 0.00793(11) -0.00264(12) Pd2 0.04043(19) 0.0476(2) 0.0665(2) 0.00084(17) 0.01112(16) -0.01147(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.389(5) . ? C1 C6 1.389(5) . ? C1 O4 1.416(4) . ? C2 C3 1.386(6) . ? C2 C10 1.524(6) . ? C3 C4 1.362(7) . ? C3 H3 0.9300 . ? C4 C5 1.365(7) . ? C4 H4 0.9300 . ? C5 C6 1.400(6) . ? C5 H5 0.9300 . ? C6 C7 1.518(6) . ? C7 C9 1.497(8) . ? C7 C8 1.537(8) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.514(6) . ? C10 C12 1.521(6) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.383(5) . ? C13 C18 1.392(5) . ? C13 O3 1.411(4) . ? C14 C15 1.400(6) . ? C14 C22 1.514(6) . ? C15 C16 1.364(6) . ? C15 H15 0.9300 . ? C16 C17 1.369(6) . ? C16 H16 0.9300 . ? C17 C18 1.388(6) . ? C17 H17 0.9300 . ? C18 C19 1.520(6) . ? C19 C20 1.514(7) . ? C19 C21 1.516(7) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C24 1.514(7) . ? C22 C23 1.534(7) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.397(8) . ? C25 N1 1.463(5) . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C32 1.398(6) . ? C27 C28 1.399(6) . ? C27 O2 1.410(4) . ? C28 C29 1.380(7) . ? C28 C36 1.517(7) . ? C29 C30 1.362(8) . ? C29 H29 0.9300 . ? C30 C31 1.368(7) . ? C30 H30 0.9300 . ? C31 C32 1.405(6) . ? C31 H31 0.9300 . ? C32 C33 1.506(6) . ? C33 C35 1.524(7) . ? C33 C34 1.531(7) . ? C33 H33 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.530(9) . ? C36 C38 1.531(9) . ? C36 H36 0.9800 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C44 1.383(6) . ? C39 C40 1.402(6) . ? C39 O1 1.414(4) . ? C40 C41 1.400(6) . ? C40 C48 1.512(6) . ? C41 C42 1.349(8) . ? C41 H41 0.9300 . ? C42 C43 1.367(8) . ? C42 H42 0.9300 . ? C43 C44 1.395(7) . ? C43 H43 0.9300 . ? C44 C45 1.520(7) . ? C45 C46 1.538(8) . ? C45 C47 1.539(7) . ? C45 H45 0.9800 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.507(7) . ? C48 C50 1.524(7) . ? C48 H48 0.9800 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.348(8) . ? C51 Pd2 2.112(5) . ? C51 H51A 0.9300 . ? C51 H51B 0.9300 . ? C52 C53 1.372(8) . ? C52 Pd2 2.101(6) . ? C52 H52 0.9800 . ? C53 Pd2 2.109(5) . ? C53 H53A 0.9300 . ? C53 H53B 0.9300 . ? Cl1 Pd2 2.3766(12) . ? Cl1 Pd1 2.4352(10) . ? Cl2 Pd2 2.3925(11) . ? Cl2 Pd1 2.3968(11) . ? N1 P1 1.615(3) . ? N1 H1 0.76(4) . ? O1 P1 1.601(3) . ? O2 P1 1.611(3) . ? O3 P2 1.609(3) . ? O4 P2 1.610(3) . ? O5 P2 1.482(3) . ? P1 Pd1 2.2385(10) . ? P2 Pd1 2.2516(10) . ? 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 C2 C1 C6 123.2(4) . . ? C2 C1 O4 118.0(3) . . ? C6 C1 O4 118.7(3) . . ? C3 C2 C1 117.1(4) . . ? C3 C2 C10 120.1(4) . . ? C1 C2 C10 122.7(4) . . ? C4 C3 C2 121.9(5) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 122.2(5) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C1 C6 C5 116.0(4) . . ? C1 C6 C7 123.4(4) . . ? C5 C6 C7 120.6(4) . . ? C9 C7 C6 113.7(5) . . ? C9 C7 C8 112.3(5) . . ? C6 C7 C8 108.8(4) . . ? C9 C7 H7 107.2 . . ? C6 C7 H7 107.2 . . ? C8 C7 H7 107.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 111.2(4) . . ? C11 C10 C2 111.5(4) . . ? C12 C10 C2 112.4(4) . . ? C11 C10 H10 107.2 . . ? C12 C10 H10 107.2 . . ? C2 C10 H10 107.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 122.9(4) . . ? C14 C13 O3 119.5(3) . . ? C18 C13 O3 117.4(3) . . ? C13 C14 C15 116.7(4) . . ? C13 C14 C22 124.4(4) . . ? C15 C14 C22 118.8(4) . . ? C16 C15 C14 121.9(4) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 119.8(4) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 121.3(4) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C13 117.4(4) . . ? C17 C18 C19 120.9(4) . . ? C13 C18 C19 121.7(4) . . ? C20 C19 C21 109.9(4) . . ? C20 C19 C18 110.0(4) . . ? C21 C19 C18 114.6(4) . . ? C20 C19 H19 107.3 . . ? C21 C19 H19 107.3 . . ? C18 C19 H19 107.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 C24 112.0(4) . . ? C14 C22 C23 111.2(4) . . ? C24 C22 C23 111.4(5) . . ? C14 C22 H22 107.3 . . ? C24 C22 H22 107.3 . . ? C23 C22 H22 107.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N1 112.9(5) . . ? C26 C25 H25 123.5 . . ? N1 C25 H25 123.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 122.8(4) . . ? C32 C27 O2 121.4(4) . . ? C28 C27 O2 115.7(4) . . ? C29 C28 C27 117.3(5) . . ? C29 C28 C36 119.1(5) . . ? C27 C28 C36 123.5(4) . . ? C30 C29 C28 121.6(5) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 120.5(5) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C32 121.3(5) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C27 C32 C31 116.3(4) . . ? C27 C32 C33 124.7(4) . . ? C31 C32 C33 119.0(4) . . ? C32 C33 C35 111.8(4) . . ? C32 C33 C34 112.2(4) . . ? C35 C33 C34 110.4(4) . . ? C32 C33 H33 107.4 . . ? C35 C33 H33 107.4 . . ? C34 C33 H33 107.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C28 C36 C37 112.1(6) . . ? C28 C36 C38 110.3(5) . . ? C37 C36 C38 110.1(5) . . ? C28 C36 H36 108.1 . . ? C37 C36 H36 108.1 . . ? C38 C36 H36 108.1 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C44 C39 C40 123.9(4) . . ? C44 C39 O1 118.1(4) . . ? C40 C39 O1 117.5(3) . . ? C41 C40 C39 115.7(4) . . ? C41 C40 C48 122.0(4) . . ? C39 C40 C48 121.8(4) . . ? C42 C41 C40 121.5(5) . . ? C42 C41 H41 119.2 . . ? C40 C41 H41 119.2 . . ? C41 C42 C43 121.1(5) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C42 C43 C44 121.2(5) . . ? C42 C43 H43 119.4 . . ? C44 C43 H43 119.4 . . ? C39 C44 C43 116.2(5) . . ? C39 C44 C45 121.0(4) . . ? C43 C44 C45 122.5(5) . . ? C44 C45 C46 109.9(4) . . ? C44 C45 C47 114.5(5) . . ? C46 C45 C47 108.9(5) . . ? C44 C45 H45 107.8 . . ? C46 C45 H45 107.8 . . ? C47 C45 H45 107.8 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C40 110.3(4) . . ? C49 C48 C50 109.4(5) . . ? C40 C48 C50 114.1(5) . . ? C49 C48 H48 107.6 . . ? C40 C48 H48 107.6 . . ? C50 C48 H48 107.6 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 Pd2 70.9(4) . . ? C52 C51 H51A 120.0 . . ? Pd2 C51 H51A 71.1 . . ? C52 C51 H51B 120.0 . . ? Pd2 C51 H51B 130.6 . . ? H51A C51 H51B 120.0 . . ? C51 C52 C53 121.3(8) . . ? C51 C52 Pd2 71.8(4) . . ? C53 C52 Pd2 71.3(3) . . ? C51 C52 H52 118.7 . . ? C53 C52 H52 118.7 . . ? Pd2 C52 H52 118.7 . . ? C52 C53 Pd2 70.7(3) . . ? C52 C53 H53A 120.0 . . ? Pd2 C53 H53A 71.4 . . ? C52 C53 H53B 120.0 . . ? Pd2 C53 H53B 130.5 . . ? H53A C53 H53B 120.0 . . ? Pd2 Cl1 Pd1 88.52(4) . . ? Pd2 Cl2 Pd1 89.05(4) . . ? C25 N1 P1 130.4(3) . . ? C25 N1 H1 115(3) . . ? P1 N1 H1 111(3) . . ? C39 O1 P1 130.7(2) . . ? C27 O2 P1 128.4(2) . . ? C13 O3 P2 127.0(2) . . ? C1 O4 P2 122.8(2) . . ? O1 P1 O2 101.17(13) . . ? O1 P1 N1 115.41(17) . . ? O2 P1 N1 104.32(17) . . ? O1 P1 Pd1 102.12(10) . . ? O2 P1 Pd1 114.59(10) . . ? N1 P1 Pd1 118.27(14) . . ? O5 P2 O3 109.87(15) . . ? O5 P2 O4 112.90(15) . . ? O3 P2 O4 99.98(13) . . ? O5 P2 Pd1 119.90(11) . . ? O3 P2 Pd1 108.39(10) . . ? O4 P2 Pd1 103.85(10) . . ? P1 Pd1 P2 93.77(4) . . ? P1 Pd1 Cl2 171.21(4) . . ? P2 Pd1 Cl2 93.55(4) . . ? P1 Pd1 Cl1 87.59(4) . . ? P2 Pd1 Cl1 172.82(4) . . ? Cl2 Pd1 Cl1 85.75(4) . . ? C52 Pd2 C53 38.0(2) . . ? C52 Pd2 C51 37.3(2) . . ? C53 Pd2 C51 68.4(3) . . ? C52 Pd2 Cl1 132.6(2) . . ? C53 Pd2 Cl1 166.75(19) . . ? C51 Pd2 Cl1 99.3(2) . . ? C52 Pd2 Cl2 137.5(2) . . ? C53 Pd2 Cl2 104.99(19) . . ? C51 Pd2 Cl2 173.1(2) . . ? Cl1 Pd2 Cl2 87.17(4) . . ? 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 C6 C1 C2 C3 -1.9(6) . . . . ? O4 C1 C2 C3 -178.8(4) . . . . ? C6 C1 C2 C10 174.6(4) . . . . ? O4 C1 C2 C10 -2.3(6) . . . . ? C1 C2 C3 C4 -1.2(7) . . . . ? C10 C2 C3 C4 -177.8(5) . . . . ? C2 C3 C4 C5 2.7(8) . . . . ? C3 C4 C5 C6 -1.3(8) . . . . ? C2 C1 C6 C5 3.2(6) . . . . ? O4 C1 C6 C5 -179.9(4) . . . . ? C2 C1 C6 C7 -173.7(4) . . . . ? O4 C1 C6 C7 3.2(6) . . . . ? C4 C5 C6 C1 -1.6(7) . . . . ? C4 C5 C6 C7 175.4(5) . . . . ? C1 C6 C7 C9 -134.1(6) . . . . ? C5 C6 C7 C9 49.1(7) . . . . ? C1 C6 C7 C8 99.9(5) . . . . ? C5 C6 C7 C8 -76.8(6) . . . . ? C3 C2 C10 C11 71.3(6) . . . . ? C1 C2 C10 C11 -105.1(5) . . . . ? C3 C2 C10 C12 -54.3(6) . . . . ? C1 C2 C10 C12 129.3(5) . . . . ? C18 C13 C14 C15 -0.5(6) . . . . ? O3 C13 C14 C15 174.6(4) . . . . ? C18 C13 C14 C22 -176.9(4) . . . . ? O3 C13 C14 C22 -1.7(6) . . . . ? C13 C14 C15 C16 0.5(7) . . . . ? C22 C14 C15 C16 177.0(4) . . . . ? C14 C15 C16 C17 -0.4(8) . . . . ? C15 C16 C17 C18 0.3(8) . . . . ? C16 C17 C18 C13 -0.4(7) . . . . ? C16 C17 C18 C19 -177.8(5) . . . . ? C14 C13 C18 C17 0.5(6) . . . . ? O3 C13 C18 C17 -174.8(4) . . . . ? C14 C13 C18 C19 177.9(4) . . . . ? O3 C13 C18 C19 2.7(6) . . . . ? C17 C18 C19 C20 87.4(6) . . . . ? C13 C18 C19 C20 -89.9(5) . . . . ? C17 C18 C19 C21 -37.0(6) . . . . ? C13 C18 C19 C21 145.7(5) . . . . ? C13 C14 C22 C24 -122.5(5) . . . . ? C15 C14 C22 C24 61.2(6) . . . . ? C13 C14 C22 C23 112.2(5) . . . . ? C15 C14 C22 C23 -64.1(6) . . . . ? C32 C27 C28 C29 4.8(7) . . . . ? O2 C27 C28 C29 -179.0(4) . . . . ? C32 C27 C28 C36 -171.4(5) . . . . ? O2 C27 C28 C36 4.8(7) . . . . ? C27 C28 C29 C30 -1.5(8) . . . . ? C36 C28 C29 C30 174.8(5) . . . . ? C28 C29 C30 C31 -1.5(9) . . . . ? C29 C30 C31 C32 1.4(8) . . . . ? C28 C27 C32 C31 -4.8(6) . . . . ? O2 C27 C32 C31 179.2(3) . . . . ? C28 C27 C32 C33 173.3(4) . . . . ? O2 C27 C32 C33 -2.7(6) . . . . ? C30 C31 C32 C27 1.6(6) . . . . ? C30 C31 C32 C33 -176.6(4) . . . . ? C27 C32 C33 C35 116.3(5) . . . . ? C31 C32 C33 C35 -65.7(5) . . . . ? C27 C32 C33 C34 -119.0(5) . . . . ? C31 C32 C33 C34 59.0(5) . . . . ? C29 C28 C36 C37 58.9(7) . . . . ? C27 C28 C36 C37 -125.0(6) . . . . ? C29 C28 C36 C38 -64.1(7) . . . . ? C27 C28 C36 C38 112.0(6) . . . . ? C44 C39 C40 C41 6.5(7) . . . . ? O1 C39 C40 C41 179.2(4) . . . . ? C44 C39 C40 C48 -165.9(4) . . . . ? O1 C39 C40 C48 6.9(6) . . . . ? C39 C40 C41 C42 -1.8(8) . . . . ? C48 C40 C41 C42 170.6(6) . . . . ? C40 C41 C42 C43 -2.2(10) . . . . ? C41 C42 C43 C44 1.8(10) . . . . ? C40 C39 C44 C43 -6.8(7) . . . . ? O1 C39 C44 C43 -179.5(4) . . . . ? C40 C39 C44 C45 167.2(4) . . . . ? O1 C39 C44 C45 -5.5(6) . . . . ? C42 C43 C44 C39 2.5(8) . . . . ? C42 C43 C44 C45 -171.5(5) . . . . ? C39 C44 C45 C46 -72.0(6) . . . . ? C43 C44 C45 C46 101.7(6) . . . . ? C39 C44 C45 C47 165.1(5) . . . . ? C43 C44 C45 C47 -21.2(7) . . . . ? C41 C40 C48 C49 -91.9(6) . . . . ? C39 C40 C48 C49 80.0(6) . . . . ? C41 C40 C48 C50 31.7(7) . . . . ? C39 C40 C48 C50 -156.4(5) . . . . ? Pd2 C51 C52 C53 -53.4(6) . . . . ? C51 C52 C53 Pd2 53.7(6) . . . . ? C26 C25 N1 P1 158.8(6) . . . . ? C44 C39 O1 P1 -101.5(4) . . . . ? C40 C39 O1 P1 85.3(4) . . . . ? C32 C27 O2 P1 -59.7(5) . . . . ? C28 C27 O2 P1 124.1(4) . . . . ? C14 C13 O3 P2 82.1(4) . . . . ? C18 C13 O3 P2 -102.5(4) . . . . ? C2 C1 O4 P2 -95.9(4) . . . . ? C6 C1 O4 P2 87.0(4) . . . . ? C39 O1 P1 O2 59.3(3) . . . . ? C39 O1 P1 N1 -52.6(4) . . . . ? C39 O1 P1 Pd1 177.7(3) . . . . ? C27 O2 P1 O1 -150.8(3) . . . . ? C27 O2 P1 N1 -30.6(3) . . . . ? C27 O2 P1 Pd1 100.2(3) . . . . ? C25 N1 P1 O1 65.8(5) . . . . ? C25 N1 P1 O2 -44.2(5) . . . . ? C25 N1 P1 Pd1 -172.9(4) . . . . ? C13 O3 P2 O5 -33.2(3) . . . . ? C13 O3 P2 O4 -152.1(3) . . . . ? C13 O3 P2 Pd1 99.5(3) . . . . ? C1 O4 P2 O5 -58.9(3) . . . . ? C1 O4 P2 O3 57.8(3) . . . . ? C1 O4 P2 Pd1 169.7(2) . . . . ? O1 P1 Pd1 P2 101.46(10) . . . . ? O2 P1 Pd1 P2 -150.11(11) . . . . ? N1 P1 Pd1 P2 -26.41(16) . . . . ? O1 P1 Pd1 Cl1 -71.48(10) . . . . ? O2 P1 Pd1 Cl1 36.95(11) . . . . ? N1 P1 Pd1 Cl1 160.65(16) . . . . ? O5 P2 Pd1 P1 -1.21(14) . . . . ? O3 P2 Pd1 P1 -128.39(10) . . . . ? O4 P2 Pd1 P1 125.94(10) . . . . ? O5 P2 Pd1 Cl2 -176.34(14) . . . . ? O3 P2 Pd1 Cl2 56.48(10) . . . . ? O4 P2 Pd1 Cl2 -49.19(10) . . . . ? Pd2 Cl2 Pd1 P2 164.37(4) . . . . ? Pd2 Cl2 Pd1 Cl1 -22.79(4) . . . . ? Pd2 Cl1 Pd1 P1 -151.30(4) . . . . ? Pd2 Cl1 Pd1 Cl2 22.96(4) . . . . ? C51 C52 Pd2 C53 -133.6(8) . . . . ? C53 C52 Pd2 C51 133.6(8) . . . . ? C51 C52 Pd2 Cl1 32.6(6) . . . . ? C53 C52 Pd2 Cl1 166.2(3) . . . . ? C51 C52 Pd2 Cl2 -172.8(3) . . . . ? C53 C52 Pd2 Cl2 -39.3(6) . . . . ? C52 C53 Pd2 C51 -28.2(5) . . . . ? C52 C53 Pd2 Cl1 -50.2(10) . . . . ? C52 C53 Pd2 Cl2 153.7(4) . . . . ? C52 C51 Pd2 C53 28.7(5) . . . . ? C52 C51 Pd2 Cl1 -156.3(5) . . . . ? Pd1 Cl1 Pd2 C52 140.1(3) . . . . ? Pd1 Cl1 Pd2 C53 -179.8(8) . . . . ? Pd1 Cl1 Pd2 C51 159.5(2) . . . . ? Pd1 Cl1 Pd2 Cl2 -22.97(4) . . . . ? Pd1 Cl2 Pd2 C52 -138.2(3) . . . . ? Pd1 Cl2 Pd2 C53 -161.99(18) . . . . ? Pd1 Cl2 Pd2 Cl1 23.35(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.085 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.085 ### END data_Complex4_ _database_code_depnum_ccdc_archive 'CCDC 637408' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C106 H158 Cl2 N2 O12 P4 Pd2' _chemical_formula_sum 'C106 H158 Cl2 N2 O12 P4 Pd2' _chemical_formula_weight 2059.92 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.134(2) _cell_length_b 17.393(3) _cell_length_c 27.747(5) _cell_angle_alpha 85.016(4) _cell_angle_beta 79.956(4) _cell_angle_gamma 73.461(4) _cell_volume 5523.4(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 22.6 _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2180 _exptl_absorpt_coefficient_mu 0.487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7266 _exptl_absorpt_correction_T_max 0.9088 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker Smart Apex CCD' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43509 _diffrn_reflns_av_R_equivalents 0.1114 _diffrn_reflns_av_sigmaI/netI 0.1339 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 22.56 _reflns_number_total 14545 _reflns_number_gt 9019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart Apex CCD' _computing_cell_refinement 'Bruker Smart Apex CCD' _computing_data_reduction 'Bruker Saint' _computing_structure_solution Shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ortep-iii _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+15.6395P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14545 _refine_ls_number_parameters 1192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1491 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.2050 _refine_ls_wR_factor_gt 0.1796 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 0.68600(6) 1.04066(4) 0.24607(3) 0.0294(2) Uani 1 1 d . . . Pd2 Pd 0.81518(6) 0.83057(4) 0.25685(3) 0.0320(2) Uani 1 1 d . . . Cl1 Cl 0.7073(2) 0.92163(15) 0.20089(9) 0.0436(7) Uani 1 1 d . . . Cl2 Cl 0.7351(2) 0.94348(15) 0.31104(9) 0.0429(7) Uani 1 1 d . . . P1 P 0.6305(2) 1.12628(18) 0.18357(11) 0.0344(7) Uani 1 1 d . . . P2 P 0.6778(3) 1.14368(18) 0.29166(11) 0.0357(8) Uani 1 1 d . . . P3 P 0.9029(3) 0.74959(19) 0.31526(12) 0.0408(8) Uani 1 1 d . . . P4 P 0.8870(3) 0.73358(18) 0.20188(11) 0.0367(8) Uani 1 1 d . . . O1 O 0.6563(6) 1.0874(4) 0.1313(2) 0.0367(19) Uani 1 1 d . . . O2 O 0.4920(6) 1.1446(5) 0.1955(3) 0.044(2) Uani 1 1 d . . . O3 O 0.8004(6) 1.1112(4) 0.3111(3) 0.042(2) Uani 1 1 d . . . O4 O 0.5909(6) 1.1438(4) 0.3426(3) 0.043(2) Uani 1 1 d . . . O5 O 0.6582(7) 1.2260(4) 0.2696(3) 0.047(2) Uani 1 1 d . . . O6 O 0.9192(7) 0.7941(5) 0.3610(3) 0.049(2) Uani 1 1 d . . . O7 O 0.8028(7) 0.7092(5) 0.3406(3) 0.048(2) Uani 1 1 d . . . O8 O 0.9339(6) 0.7832(4) 0.1551(3) 0.0376(19) Uani 1 1 d . . . O9 O 0.7852(6) 0.7116(5) 0.1806(3) 0.045(2) Uani 1 1 d . . . O10 O 0.9753(7) 0.6589(4) 0.2134(3) 0.047(2) Uani 1 1 d . . . O11 O 0.3746(19) 0.5589(13) 0.9723(9) 0.226(11) Uani 1 1 d . . . O12 O 1.3226(7) 0.5359(5) 0.4204(3) 0.106(2) Uani 1 1 d . . . N1 N 0.6766(8) 1.2053(5) 0.1737(3) 0.041(2) Uani 1 1 d . . . H1 H 0.7147 1.2127 0.1955 0.050 Uiso 1 1 calc R . . N2 N 1.0273(8) 0.6875(6) 0.2991(4) 0.055(3) Uani 1 1 d . . . H2 H 1.0483 0.6827 0.2681 0.067 Uiso 1 1 calc R . . C1 C 0.7407(10) 1.0958(7) 0.0900(4) 0.042(3) Uani 1 1 d . . . C2 C 0.6975(11) 1.1239(8) 0.0465(4) 0.050(3) Uani 1 1 d . . . C3 C 0.7776(14) 1.1308(9) 0.0051(5) 0.071(4) Uani 1 1 d . . . H3 H 0.7517 1.1495 -0.0245 0.085 Uiso 1 1 calc R . . C4 C 0.8957(14) 1.1100(9) 0.0074(5) 0.069(4) Uani 1 1 d . . . H4 H 0.9482 1.1149 -0.0206 0.082 Uiso 1 1 calc R . . C5 C 0.9351(11) 1.0828(8) 0.0502(5) 0.057(4) Uani 1 1 d . . . H5 H 1.0146 1.0697 0.0512 0.069 Uiso 1 1 calc R . . C6 C 0.8586(10) 1.0739(7) 0.0928(4) 0.040(3) Uani 1 1 d . . . C7 C 0.5698(11) 1.1495(9) 0.0420(5) 0.066(4) Uani 1 1 d . . . H7 H 0.5257 1.1410 0.0742 0.080 Uiso 1 1 calc R . . C8 C 0.5258(13) 1.2374(9) 0.0263(5) 0.082(5) Uani 1 1 d . . . H8A H 0.5418 1.2704 0.0487 0.123 Uiso 1 1 calc R . . H8B H 0.4434 1.2507 0.0262 0.123 Uiso 1 1 calc R . . H8C H 0.5644 1.2465 -0.0061 0.123 Uiso 1 1 calc R . . C9 C 0.5450(15) 1.0976(10) 0.0059(6) 0.099(6) Uani 1 1 d . . . H9A H 0.5844 1.1069 -0.0263 0.148 Uiso 1 1 calc R . . H9B H 0.4627 1.1113 0.0055 0.148 Uiso 1 1 calc R . . H9C H 0.5723 1.0420 0.0157 0.148 Uiso 1 1 calc R . . C10 C 0.9114(10) 1.0405(7) 0.1382(4) 0.043(3) Uani 1 1 d . . . H10 H 0.8476 1.0371 0.1646 0.051 Uiso 1 1 calc R . . C11 C 0.9749(12) 1.0959(8) 0.1543(5) 0.072(4) Uani 1 1 d . . . H11A H 1.0395 1.0991 0.1295 0.108 Uiso 1 1 calc R . . H11B H 1.0029 1.0749 0.1844 0.108 Uiso 1 1 calc R . . H11C H 0.9223 1.1485 0.1592 0.108 Uiso 1 1 calc R . . C12 C 0.9933(12) 0.9572(8) 0.1319(5) 0.068(4) Uani 1 1 d . . . H12A H 0.9522 0.9217 0.1237 0.102 Uiso 1 1 calc R . . H12B H 1.0231 0.9383 0.1619 0.102 Uiso 1 1 calc R . . H12C H 1.0567 0.9588 0.1061 0.102 Uiso 1 1 calc R . . C13 C 0.4027(10) 1.1772(8) 0.1663(4) 0.046(3) Uani 1 1 d . . . C14 C 0.3543(11) 1.2596(8) 0.1654(5) 0.054(4) Uani 1 1 d . . . C15 C 0.2679(12) 1.2872(9) 0.1351(6) 0.074(5) Uani 1 1 d . . . H15 H 0.2343 1.3421 0.1313 0.088 Uiso 1 1 calc R . . C16 C 0.2326(12) 1.2362(11) 0.1118(6) 0.078(5) Uani 1 1 d . . . H16 H 0.1752 1.2568 0.0922 0.094 Uiso 1 1 calc R . . C17 C 0.2786(13) 1.1547(10) 0.1158(6) 0.073(4) Uani 1 1 d . . . H17 H 0.2530 1.1209 0.0989 0.087 Uiso 1 1 calc R . . C18 C 0.3640(10) 1.1225(8) 0.1454(5) 0.049(3) Uani 1 1 d . . . C19 C 0.3798(12) 1.3152(8) 0.1977(5) 0.065(4) Uani 1 1 d . . . H19 H 0.4601 1.2919 0.2036 0.078 Uiso 1 1 calc R . . C20 C 0.3716(16) 1.3998(9) 0.1755(8) 0.125(8) Uani 1 1 d . . . H20A H 0.4237 1.3967 0.1449 0.187 Uiso 1 1 calc R . . H20B H 0.3927 1.4307 0.1976 0.187 Uiso 1 1 calc R . . H20C H 0.2933 1.4251 0.1699 0.187 Uiso 1 1 calc R . . C21 C 0.3007(14) 1.3184(11) 0.2477(6) 0.110(7) Uani 1 1 d . . . H21A H 0.2208 1.3397 0.2432 0.165 Uiso 1 1 calc R . . H21B H 0.3197 1.3523 0.2687 0.165 Uiso 1 1 calc R . . H21C H 0.3122 1.2653 0.2624 0.165 Uiso 1 1 calc R . . C22 C 0.4031(12) 1.0319(8) 0.1565(6) 0.064(4) Uani 1 1 d . . . H22 H 0.4709 1.0206 0.1734 0.076 Uiso 1 1 calc R . . C23 C 0.436(3) 0.9847(12) 0.1132(8) 0.221(16) Uani 1 1 d . . . H23A H 0.3719 0.9964 0.0954 0.332 Uiso 1 1 calc R . . H23B H 0.4570 0.9286 0.1228 0.332 Uiso 1 1 calc R . . H23C H 0.5015 0.9976 0.0929 0.332 Uiso 1 1 calc R . . C24 C 0.3097(17) 1.0079(11) 0.1899(8) 0.145(10) Uani 1 1 d . . . H24A H 0.2379 1.0283 0.1771 0.218 Uiso 1 1 calc R . . H24B H 0.3015 1.0293 0.2215 0.218 Uiso 1 1 calc R . . H24C H 0.3285 0.9504 0.1930 0.218 Uiso 1 1 calc R . . C25 C 0.8374(10) 1.1572(7) 0.3415(5) 0.044(3) Uani 1 1 d . . . C26 C 0.8212(12) 1.1409(9) 0.3919(5) 0.062(4) Uani 1 1 d . . . C27 C 0.8588(15) 1.1877(11) 0.4194(6) 0.093(5) Uani 1 1 d . . . H27 H 0.8506 1.1783 0.4531 0.112 Uiso 1 1 calc R . . C28 C 0.9070(18) 1.2465(12) 0.3998(6) 0.108(7) Uani 1 1 d . . . H28 H 0.9261 1.2791 0.4200 0.130 Uiso 1 1 calc R . . C29 C 0.9276(13) 1.2577(9) 0.3505(6) 0.082(5) Uani 1 1 d . . . H29 H 0.9643 1.2966 0.3372 0.098 Uiso 1 1 calc R . . C30 C 0.8953(11) 1.2127(7) 0.3193(5) 0.052(3) Uani 1 1 d . . . C31 C 0.7763(14) 1.0709(9) 0.4148(5) 0.067(4) Uani 1 1 d . . . H31 H 0.7520 1.0473 0.3890 0.080 Uiso 1 1 calc R . . C32 C 0.8745(17) 1.0065(11) 0.4352(7) 0.129(8) Uani 1 1 d . . . H32A H 0.9438 0.9965 0.4112 0.194 Uiso 1 1 calc R . . H32B H 0.8516 0.9578 0.4428 0.194 Uiso 1 1 calc R . . H32C H 0.8895 1.0248 0.4644 0.194 Uiso 1 1 calc R . . C33 C 0.6722(16) 1.0970(12) 0.4547(6) 0.118(7) Uani 1 1 d . . . H33A H 0.6929 1.1233 0.4793 0.177 Uiso 1 1 calc R . . H33B H 0.6489 1.0508 0.4691 0.177 Uiso 1 1 calc R . . H33C H 0.6090 1.1334 0.4408 0.177 Uiso 1 1 calc R . . C34 C 0.9283(11) 1.2238(8) 0.2643(5) 0.056(4) Uani 1 1 d . . . H34 H 0.8932 1.1906 0.2484 0.067 Uiso 1 1 calc R . . C35 C 1.0629(13) 1.1912(9) 0.2511(6) 0.091(5) Uani 1 1 d . . . H35A H 1.0857 1.1981 0.2164 0.137 Uiso 1 1 calc R . . H35B H 1.0863 1.1352 0.2605 0.137 Uiso 1 1 calc R . . H35C H 1.0996 1.2201 0.2682 0.137 Uiso 1 1 calc R . . C36 C 0.8854(14) 1.3073(8) 0.2461(6) 0.088(5) Uani 1 1 d . . . H36A H 0.8019 1.3239 0.2530 0.132 Uiso 1 1 calc R . . H36B H 0.9101 1.3108 0.2114 0.132 Uiso 1 1 calc R . . H36C H 0.9162 1.3416 0.2620 0.132 Uiso 1 1 calc R . . C37 C 0.4791(10) 1.1954(8) 0.3542(4) 0.050(3) Uani 1 1 d . . . C38 C 0.3868(11) 1.1594(9) 0.3592(5) 0.065(4) Uani 1 1 d . . . C39 C 0.2743(12) 1.2099(11) 0.3731(6) 0.084(5) Uani 1 1 d . . . H39 H 0.2111 1.1885 0.3769 0.101 Uiso 1 1 calc R . . C40 C 0.2547(14) 1.2896(11) 0.3812(6) 0.088(6) Uani 1 1 d . . . H40 H 0.1793 1.3222 0.3892 0.106 Uiso 1 1 calc R . . C41 C 0.3472(15) 1.3203(9) 0.3773(5) 0.078(5) Uani 1 1 d . . . H41 H 0.3337 1.3741 0.3835 0.093 Uiso 1 1 calc R . . C42 C 0.4601(12) 1.2746(8) 0.3647(5) 0.059(4) Uani 1 1 d . . . C43 C 0.4095(12) 1.0703(10) 0.3544(7) 0.083(5) Uani 1 1 d . . . H43 H 0.4938 1.0454 0.3495 0.100 Uiso 1 1 calc R . . C44 C 0.361(2) 1.0522(13) 0.3116(9) 0.175(11) Uani 1 1 d . . . H44A H 0.2781 1.0767 0.3159 0.263 Uiso 1 1 calc R . . H44B H 0.3757 0.9951 0.3098 0.263 Uiso 1 1 calc R . . H44C H 0.3968 1.0732 0.2818 0.263 Uiso 1 1 calc R . . C45 C 0.356(3) 1.0337(13) 0.3993(9) 0.206(14) Uani 1 1 d . . . H45A H 0.3706 1.0546 0.4276 0.309 Uiso 1 1 calc R . . H45B H 0.3881 0.9765 0.3996 0.309 Uiso 1 1 calc R . . H45C H 0.2731 1.0464 0.3997 0.309 Uiso 1 1 calc R . . C46 C 0.5571(14) 1.3143(9) 0.3649(6) 0.076(5) Uani 1 1 d . . . H46 H 0.6310 1.2742 0.3547 0.091 Uiso 1 1 calc R . . C47 C 0.5486(14) 1.3849(9) 0.3272(6) 0.093(5) Uani 1 1 d . . . H47A H 0.5454 1.3671 0.2958 0.139 Uiso 1 1 calc R . . H47B H 0.6157 1.4046 0.3250 0.139 Uiso 1 1 calc R . . H47C H 0.4795 1.4270 0.3373 0.139 Uiso 1 1 calc R . . C48 C 0.5596(15) 1.3377(10) 0.4160(6) 0.105(6) Uani 1 1 d . . . H48A H 0.6217 1.3621 0.4150 0.157 Uiso 1 1 calc R . . H48B H 0.5719 1.2907 0.4375 0.157 Uiso 1 1 calc R . . H48C H 0.4868 1.3751 0.4279 0.157 Uiso 1 1 calc R . . C49 C 0.6643(12) 1.2666(8) 0.1339(5) 0.059(4) Uani 1 1 d . . . H49 H 0.6064 1.2750 0.1145 0.071 Uiso 1 1 calc R . . C50 C 0.741(3) 1.3094(16) 0.1271(10) 0.26(2) Uani 1 1 d . . . H50A H 0.7977 1.2996 0.1471 0.311 Uiso 1 1 calc R . . H50B H 0.7374 1.3493 0.1024 0.311 Uiso 1 1 calc R . . C51 C 1.0227(11) 0.8050(8) 0.3735(5) 0.054(4) Uani 1 1 d . . . C52 C 1.0882(10) 0.8462(8) 0.3419(5) 0.056(4) Uani 1 1 d . . . C53 C 1.1845(12) 0.8581(10) 0.3581(6) 0.080(5) Uani 1 1 d . . . H53 H 1.2322 0.8846 0.3375 0.096 Uiso 1 1 calc R . . C54 C 1.2096(15) 0.8312(13) 0.4037(7) 0.114(7) Uani 1 1 d . . . H54 H 1.2734 0.8407 0.4139 0.137 Uiso 1 1 calc R . . C55 C 1.1422(16) 0.7900(13) 0.4351(7) 0.112(7) Uani 1 1 d . . . H55 H 1.1607 0.7721 0.4661 0.135 Uiso 1 1 calc R . . C56 C 1.0472(13) 0.7759(10) 0.4201(5) 0.074(5) Uani 1 1 d . . . C57 C 1.0643(11) 0.8813(8) 0.2914(5) 0.055(4) Uani 1 1 d . . . H57 H 0.9917 0.8717 0.2859 0.066 Uiso 1 1 calc R . . C58 C 1.0480(13) 0.9708(8) 0.2884(6) 0.090(5) Uani 1 1 d . . . H58A H 0.9883 0.9953 0.3144 0.135 Uiso 1 1 calc R . . H58B H 1.0256 0.9925 0.2575 0.135 Uiso 1 1 calc R . . H58C H 1.1197 0.9816 0.2916 0.135 Uiso 1 1 calc R . . C59 C 1.1602(13) 0.8408(9) 0.2518(5) 0.080(5) Uani 1 1 d . . . H59A H 1.1423 0.8633 0.2203 0.121 Uiso 1 1 calc R . . H59B H 1.1668 0.7843 0.2533 0.121 Uiso 1 1 calc R . . H59C H 1.2325 0.8489 0.2566 0.121 Uiso 1 1 calc R . . C60 C 0.9743(17) 0.7308(12) 0.4554(6) 0.095(6) Uani 1 1 d . . . H60 H 0.9173 0.7207 0.4375 0.114 Uiso 1 1 calc R . . C61 C 1.0404(19) 0.6517(12) 0.4744(7) 0.140(8) Uani 1 1 d . . . H61A H 1.0965 0.6592 0.4927 0.210 Uiso 1 1 calc R . . H61B H 1.0798 0.6181 0.4474 0.210 Uiso 1 1 calc R . . H61C H 0.9876 0.6266 0.4953 0.210 Uiso 1 1 calc R . . C62 C 0.9054(17) 0.7846(13) 0.4977(7) 0.132(8) Uani 1 1 d . . . H62A H 0.8709 0.7533 0.5229 0.198 Uiso 1 1 calc R . . H62B H 0.8454 0.8271 0.4858 0.198 Uiso 1 1 calc R . . H62C H 0.9569 0.8071 0.5109 0.198 Uiso 1 1 calc R . . C63 C 0.7834(12) 0.6720(8) 0.3874(5) 0.059(4) Uani 1 1 d . . . C64 C 0.8321(14) 0.5897(9) 0.3931(6) 0.074(4) Uani 1 1 d . . . C65 C 0.8101(19) 0.5550(12) 0.4398(8) 0.109(7) Uani 1 1 d . . . H65 H 0.8408 0.5002 0.4455 0.130 Uiso 1 1 calc R . . C66 C 0.744(2) 0.6010(17) 0.4770(8) 0.139(9) Uani 1 1 d . . . H66 H 0.7326 0.5768 0.5079 0.167 Uiso 1 1 calc R . . C67 C 0.6933(19) 0.6818(14) 0.4710(7) 0.119(8) Uani 1 1 d . . . H67 H 0.6487 0.7114 0.4975 0.143 Uiso 1 1 calc R . . C68 C 0.7098(14) 0.7187(11) 0.4244(6) 0.076(5) Uani 1 1 d . . . C69 C 0.8920(14) 0.5383(9) 0.3495(6) 0.080(5) Uani 1 1 d . . . H69 H 0.9309 0.5710 0.3257 0.096 Uiso 1 1 calc R . . C70 C 0.9848(17) 0.4635(10) 0.3622(8) 0.129(8) Uani 1 1 d . . . H70A H 1.0317 0.4773 0.3828 0.194 Uiso 1 1 calc R . . H70B H 1.0331 0.4415 0.3327 0.194 Uiso 1 1 calc R . . H70C H 0.9483 0.4246 0.3792 0.194 Uiso 1 1 calc R . . C71 C 0.8047(18) 0.5158(12) 0.3247(7) 0.133(8) Uani 1 1 d . . . H71A H 0.7672 0.4816 0.3465 0.200 Uiso 1 1 calc R . . H71B H 0.8441 0.4879 0.2955 0.200 Uiso 1 1 calc R . . H71C H 0.7473 0.5635 0.3163 0.200 Uiso 1 1 calc R . . C72 C 0.6453(15) 0.8048(10) 0.4141(7) 0.094(6) Uani 1 1 d . . . H72 H 0.6872 0.8249 0.3845 0.112 Uiso 1 1 calc R . . C73 C 0.628(2) 0.8595(14) 0.4530(10) 0.202(14) Uani 1 1 d . . . H73A H 0.5644 0.9057 0.4488 0.302 Uiso 1 1 calc R . . H73B H 0.6977 0.8761 0.4520 0.302 Uiso 1 1 calc R . . H73C H 0.6116 0.8329 0.4841 0.302 Uiso 1 1 calc R . . C74 C 0.531(3) 0.8100(15) 0.4057(16) 0.32(3) Uani 1 1 d . . . H74A H 0.4973 0.7759 0.4293 0.473 Uiso 1 1 calc R . . H74B H 0.5342 0.7932 0.3733 0.473 Uiso 1 1 calc R . . H74C H 0.4835 0.8645 0.4089 0.473 Uiso 1 1 calc R . . C75 C 0.9857(11) 0.7483(7) 0.1097(4) 0.043(3) Uani 1 1 d . . . C76 C 0.9169(11) 0.7574(7) 0.0736(5) 0.051(3) Uani 1 1 d . . . C77 C 0.9693(14) 0.7242(9) 0.0291(5) 0.071(4) Uani 1 1 d . . . H77 H 0.9249 0.7300 0.0042 0.086 Uiso 1 1 calc R . . C78 C 1.0844(16) 0.6829(10) 0.0205(6) 0.083(5) Uani 1 1 d . . . H78 H 1.1172 0.6582 -0.0090 0.099 Uiso 1 1 calc R . . C79 C 1.1510(13) 0.6788(9) 0.0570(6) 0.078(5) Uani 1 1 d . . . H79 H 1.2303 0.6533 0.0508 0.094 Uiso 1 1 calc R . . C80 C 1.1038(11) 0.7113(8) 0.1025(5) 0.052(3) Uani 1 1 d . . . C81 C 0.7914(10) 0.8078(8) 0.0794(5) 0.051(3) Uani 1 1 d . . . H81 H 0.7683 0.8245 0.1134 0.061 Uiso 1 1 calc R . . C82 C 0.7108(12) 0.7599(9) 0.0698(5) 0.080(5) Uani 1 1 d . . . H82A H 0.7259 0.7480 0.0357 0.121 Uiso 1 1 calc R . . H82B H 0.6314 0.7908 0.0783 0.121 Uiso 1 1 calc R . . H82C H 0.7244 0.7108 0.0893 0.121 Uiso 1 1 calc R . . C83 C 0.7784(13) 0.8846(9) 0.0455(6) 0.082(5) Uani 1 1 d . . . H83A H 0.7872 0.8704 0.0121 0.123 Uiso 1 1 calc R . . H83B H 0.8372 0.9099 0.0489 0.123 Uiso 1 1 calc R . . H83C H 0.7028 0.9209 0.0546 0.123 Uiso 1 1 calc R . . C84 C 1.1832(11) 0.7075(9) 0.1400(5) 0.062(4) Uani 1 1 d . . . H84 H 1.1335 0.7308 0.1699 0.075 Uiso 1 1 calc R . . C85 C 1.2664(12) 0.7587(9) 0.1228(6) 0.084(5) Uani 1 1 d . . . H85A H 1.3196 0.7359 0.0945 0.127 Uiso 1 1 calc R . . H85B H 1.3092 0.7604 0.1485 0.127 Uiso 1 1 calc R . . H85C H 1.2230 0.8122 0.1145 0.127 Uiso 1 1 calc R . . C86 C 1.2465(13) 0.6205(10) 0.1535(6) 0.104(6) Uani 1 1 d . . . H86A H 1.1904 0.5925 0.1679 0.156 Uiso 1 1 calc R . . H86B H 1.2971 0.6204 0.1765 0.156 Uiso 1 1 calc R . . H86C H 1.2916 0.5943 0.1245 0.156 Uiso 1 1 calc R . . C87 C 0.7432(11) 0.6449(7) 0.1948(5) 0.046(3) Uani 1 1 d . . . C88 C 0.6393(12) 0.6560(9) 0.2249(5) 0.061(4) Uani 1 1 d . . . C89 C 0.5900(14) 0.5931(11) 0.2356(6) 0.085(5) Uani 1 1 d . . . H89 H 0.5179 0.6008 0.2554 0.101 Uiso 1 1 calc R . . C90 C 0.6477(18) 0.5179(12) 0.2168(7) 0.099(6) Uani 1 1 d . . . H90 H 0.6174 0.4743 0.2253 0.119 Uiso 1 1 calc R . . C91 C 0.7506(17) 0.5103(10) 0.1856(7) 0.091(5) Uani 1 1 d . . . H91 H 0.7880 0.4607 0.1720 0.110 Uiso 1 1 calc R . . C92 C 0.8019(13) 0.5726(8) 0.1730(5) 0.060(4) Uani 1 1 d . . . C93 C 0.5756(12) 0.7367(10) 0.2455(6) 0.077(5) Uani 1 1 d . . . H93 H 0.6344 0.7617 0.2518 0.092 Uiso 1 1 calc R . . C94 C 0.5117(15) 0.7888(11) 0.2067(8) 0.126(7) Uani 1 1 d . . . H94A H 0.5621 0.7832 0.1757 0.189 Uiso 1 1 calc R . . H94B H 0.4884 0.8438 0.2156 0.189 Uiso 1 1 calc R . . H94C H 0.4439 0.7721 0.2043 0.189 Uiso 1 1 calc R . . C95 C 0.4912(18) 0.7380(14) 0.2924(8) 0.155(10) Uani 1 1 d . . . H95A H 0.4331 0.7129 0.2877 0.233 Uiso 1 1 calc R . . H95B H 0.4545 0.7925 0.3013 0.233 Uiso 1 1 calc R . . H95C H 0.5323 0.7093 0.3180 0.233 Uiso 1 1 calc R . . C96 C 0.9149(14) 0.5552(9) 0.1383(6) 0.079(5) Uani 1 1 d . . . H96 H 0.9382 0.6052 0.1327 0.095 Uiso 1 1 calc R . . C97 C 0.8998(17) 0.5308(10) 0.0885(7) 0.117(7) Uani 1 1 d . . . H97A H 0.8488 0.4966 0.0935 0.176 Uiso 1 1 calc R . . H97B H 0.9742 0.5026 0.0713 0.176 Uiso 1 1 calc R . . H97C H 0.8669 0.5780 0.0695 0.176 Uiso 1 1 calc R . . C98 C 1.0129(14) 0.4925(9) 0.1587(7) 0.103(6) Uani 1 1 d . . . H98A H 1.0205 0.5082 0.1900 0.154 Uiso 1 1 calc R . . H98B H 1.0845 0.4881 0.1365 0.154 Uiso 1 1 calc R . . H98C H 0.9955 0.4416 0.1623 0.154 Uiso 1 1 calc R . . C99 C 1.1113(10) 0.6375(8) 0.3294(5) 0.068(4) Uani 1 1 d . . . H99A H 1.1490 0.6711 0.3428 0.081 Uiso 1 1 calc R . . H99B H 1.0703 0.6123 0.3565 0.081 Uiso 1 1 calc R . . C100 C 1.1994(16) 0.5755(13) 0.3006(8) 0.154(10) Uani 1 1 d . . . H10A H 1.1619 0.5477 0.2830 0.231 Uiso 1 1 calc R . . H10B H 1.2445 0.5381 0.3220 0.231 Uiso 1 1 calc R . . H10C H 1.2496 0.6000 0.2777 0.231 Uiso 1 1 calc R . . C101 C 0.440(2) 0.4368(17) 0.9339(10) 0.213(15) Uani 1 1 d . . . H10D H 0.3947 0.4039 0.9257 0.319 Uiso 1 1 calc R . . H10E H 0.5114 0.4033 0.9428 0.319 Uiso 1 1 calc R . . H10F H 0.4562 0.4709 0.9060 0.319 Uiso 1 1 calc R . . C102 C 0.375(2) 0.4853(18) 0.9741(13) 0.153(10) Uani 1 1 d . . . C103 C 0.309(3) 0.4538(17) 1.0177(11) 0.227(15) Uani 1 1 d . . . H10G H 0.2351 0.4921 1.0265 0.340 Uiso 1 1 calc R . . H10H H 0.3523 0.4447 1.0445 0.340 Uiso 1 1 calc R . . H10I H 0.2972 0.4042 1.0102 0.340 Uiso 1 1 calc R . . C105 C 1.390(3) 0.5769(17) 0.4295(15) 0.208(14) Uani 1 1 d . . . C104 C 1.4609(11) 0.6008(8) 0.3880(4) 0.113(3) Uani 1 1 d . . . H10J H 1.4492 0.5796 0.3591 0.170 Uiso 1 1 calc R . . H10K H 1.5412 0.5807 0.3921 0.170 Uiso 1 1 calc R . . H10L H 1.4405 0.6583 0.3848 0.170 Uiso 1 1 calc R . . C106 C 1.3788(11) 0.5862(8) 0.4817(5) 0.107(3) Uani 1 1 d . . . H10M H 1.2999 0.5907 0.4968 0.160 Uiso 1 1 calc R . . H10N H 1.3994 0.6337 0.4871 0.160 Uiso 1 1 calc R . . H10O H 1.4298 0.5402 0.4957 0.160 Uiso 1 1 calc R . . 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 0.0322(4) 0.0281(5) 0.0280(5) -0.0030(3) -0.0047(3) -0.0076(3) Pd2 0.0353(4) 0.0299(5) 0.0308(5) 0.0000(4) -0.0064(4) -0.0085(4) Cl1 0.0618(17) 0.0313(15) 0.0396(16) -0.0013(12) -0.0197(13) -0.0090(13) Cl2 0.0582(17) 0.0358(16) 0.0315(15) -0.0022(12) -0.0072(13) -0.0071(13) P1 0.0348(17) 0.0320(18) 0.0354(19) 0.0045(14) -0.0075(14) -0.0081(14) P2 0.0383(18) 0.0327(19) 0.0354(19) -0.0085(15) -0.0015(15) -0.0091(15) P3 0.0398(19) 0.044(2) 0.039(2) 0.0051(16) -0.0072(15) -0.0140(16) P4 0.0389(18) 0.0343(19) 0.0361(19) 0.0007(15) -0.0109(15) -0.0062(15) O1 0.042(5) 0.044(5) 0.025(5) 0.003(4) -0.008(4) -0.012(4) O2 0.038(5) 0.047(5) 0.043(5) 0.001(4) -0.004(4) -0.007(4) O3 0.050(5) 0.041(5) 0.037(5) -0.013(4) -0.004(4) -0.017(4) O4 0.045(5) 0.038(5) 0.041(5) -0.005(4) 0.001(4) -0.005(4) O5 0.059(5) 0.033(5) 0.044(5) -0.014(4) -0.002(4) -0.006(4) O6 0.052(5) 0.062(6) 0.036(5) -0.002(4) -0.011(4) -0.018(4) O7 0.059(5) 0.040(5) 0.048(6) 0.017(4) -0.013(4) -0.020(4) O8 0.041(5) 0.036(5) 0.033(5) -0.001(4) -0.006(4) -0.008(4) O9 0.043(5) 0.045(5) 0.048(5) -0.004(4) -0.015(4) -0.009(4) O10 0.060(5) 0.037(5) 0.043(5) 0.000(4) -0.016(4) -0.007(4) O11 0.22(2) 0.132(17) 0.27(3) -0.021(18) 0.026(17) 0.008(16) O12 0.108(5) 0.100(6) 0.109(6) -0.007(4) -0.014(4) -0.027(4) N1 0.052(6) 0.039(6) 0.034(6) 0.007(5) -0.015(5) -0.011(5) N2 0.040(6) 0.073(8) 0.051(7) -0.002(6) -0.015(5) -0.006(6) C1 0.050(8) 0.031(7) 0.039(8) 0.001(6) -0.006(6) -0.006(6) C2 0.054(8) 0.057(9) 0.033(8) 0.008(7) -0.003(7) -0.011(7) C3 0.088(12) 0.077(11) 0.040(9) 0.010(8) -0.008(9) -0.014(9) C4 0.075(11) 0.079(11) 0.048(10) 0.014(9) 0.012(8) -0.033(9) C5 0.050(8) 0.052(9) 0.061(10) -0.001(8) 0.004(8) -0.007(7) C6 0.033(7) 0.051(8) 0.036(8) 0.001(6) -0.003(6) -0.016(6) C7 0.059(9) 0.096(12) 0.043(9) 0.010(8) -0.014(7) -0.020(9) C8 0.084(11) 0.078(13) 0.070(11) 0.006(9) -0.027(9) 0.006(9) C9 0.123(14) 0.103(14) 0.095(14) 0.010(11) -0.063(12) -0.045(12) C10 0.044(7) 0.042(8) 0.043(8) 0.004(6) -0.004(6) -0.017(6) C11 0.068(10) 0.065(10) 0.085(11) -0.007(9) -0.011(8) -0.019(8) C12 0.068(10) 0.053(10) 0.075(11) 0.009(8) -0.016(8) -0.006(8) C13 0.033(7) 0.050(9) 0.046(8) 0.007(7) -0.002(6) -0.003(7) C14 0.048(8) 0.042(9) 0.058(9) 0.020(7) -0.011(7) 0.004(7) C15 0.061(10) 0.051(10) 0.097(13) 0.023(9) -0.028(9) 0.006(8) C16 0.048(9) 0.098(14) 0.087(13) 0.003(11) -0.035(9) -0.007(10) C17 0.064(10) 0.077(13) 0.084(12) -0.013(10) -0.022(9) -0.022(9) C18 0.036(7) 0.065(10) 0.050(9) -0.002(7) -0.005(7) -0.019(7) C19 0.068(10) 0.044(9) 0.077(11) -0.015(8) -0.008(8) -0.001(7) C20 0.131(16) 0.044(11) 0.20(2) 0.003(13) -0.053(15) -0.015(11) C21 0.100(13) 0.125(16) 0.104(15) -0.069(13) 0.004(12) -0.022(12) C22 0.054(9) 0.047(10) 0.093(12) -0.014(9) -0.013(8) -0.015(7) C23 0.43(5) 0.066(15) 0.12(2) -0.031(14) 0.07(2) -0.05(2) C24 0.125(17) 0.090(15) 0.17(2) 0.042(15) 0.051(16) -0.009(13) C25 0.049(8) 0.043(8) 0.041(8) -0.007(6) -0.014(6) -0.006(6) C26 0.081(10) 0.065(10) 0.047(9) -0.009(8) -0.016(8) -0.025(8) C27 0.137(15) 0.107(14) 0.057(11) -0.021(10) -0.029(11) -0.052(13) C28 0.18(2) 0.124(17) 0.061(13) -0.012(11) -0.042(13) -0.091(16) C29 0.101(12) 0.081(12) 0.086(14) -0.006(10) -0.035(11) -0.049(10) C30 0.059(9) 0.045(8) 0.063(10) -0.004(7) -0.020(7) -0.027(7) C31 0.106(12) 0.069(11) 0.035(9) -0.001(8) -0.018(8) -0.035(10) C32 0.133(17) 0.086(15) 0.14(2) 0.023(14) -0.015(15) -0.004(13) C33 0.143(17) 0.141(18) 0.069(13) -0.019(12) 0.018(12) -0.052(14) C34 0.065(9) 0.047(9) 0.060(10) -0.004(7) -0.005(7) -0.024(7) C35 0.088(12) 0.086(13) 0.106(14) -0.017(11) 0.004(10) -0.043(10) C36 0.107(13) 0.052(11) 0.098(14) 0.013(9) -0.004(10) -0.024(9) C37 0.042(8) 0.044(9) 0.046(9) 0.006(7) 0.010(6) 0.004(7) C38 0.045(9) 0.071(11) 0.064(10) 0.007(8) 0.008(7) -0.005(8) C39 0.045(9) 0.086(13) 0.098(14) 0.007(11) 0.009(9) 0.002(9) C40 0.066(11) 0.086(14) 0.071(12) 0.001(10) 0.022(9) 0.026(10) C41 0.078(12) 0.064(11) 0.072(12) -0.012(9) 0.022(9) -0.006(10) C42 0.067(10) 0.042(9) 0.054(9) 0.000(7) 0.007(7) -0.002(8) C43 0.044(9) 0.076(13) 0.129(16) -0.029(12) 0.009(9) -0.022(8) C44 0.28(3) 0.111(19) 0.17(2) -0.008(17) -0.07(2) -0.08(2) C45 0.34(4) 0.10(2) 0.17(3) 0.032(18) -0.01(3) -0.08(2) C46 0.090(11) 0.060(11) 0.076(12) -0.024(9) -0.002(9) -0.017(9) C47 0.113(14) 0.057(11) 0.106(14) -0.010(10) 0.008(11) -0.036(10) C48 0.116(14) 0.096(14) 0.103(15) -0.046(12) -0.007(12) -0.024(11) C49 0.086(10) 0.053(9) 0.049(9) 0.028(7) -0.024(8) -0.036(8) C50 0.35(4) 0.25(3) 0.30(4) 0.25(3) -0.24(3) -0.25(3) C51 0.044(8) 0.068(10) 0.053(9) -0.006(8) -0.016(7) -0.014(7) C52 0.036(8) 0.067(10) 0.074(11) -0.010(8) -0.005(7) -0.026(7) C53 0.059(10) 0.108(14) 0.083(13) -0.004(11) -0.013(9) -0.036(10) C54 0.084(13) 0.19(2) 0.093(15) 0.003(15) -0.035(12) -0.069(14) C55 0.095(14) 0.17(2) 0.092(15) 0.010(14) -0.046(12) -0.052(14) C56 0.082(11) 0.108(13) 0.043(10) 0.007(9) -0.021(8) -0.038(10) C57 0.059(9) 0.057(10) 0.053(9) -0.003(7) -0.008(7) -0.024(7) C58 0.091(12) 0.048(10) 0.114(14) -0.001(9) 0.011(10) -0.009(9) C59 0.080(11) 0.083(12) 0.071(11) -0.006(9) 0.004(9) -0.020(9) C60 0.130(15) 0.127(17) 0.054(11) 0.018(12) -0.034(11) -0.069(14) C61 0.17(2) 0.128(19) 0.124(18) 0.055(15) -0.050(16) -0.054(17) C62 0.129(18) 0.16(2) 0.087(16) 0.016(15) -0.009(14) -0.025(16) C63 0.071(10) 0.050(10) 0.057(10) 0.017(8) -0.007(8) -0.024(8) C64 0.097(12) 0.052(11) 0.077(12) 0.011(9) -0.013(10) -0.031(9) C65 0.17(2) 0.080(14) 0.087(15) 0.058(13) -0.044(14) -0.048(14) C66 0.19(3) 0.15(2) 0.086(17) 0.023(17) 0.023(16) -0.10(2) C67 0.17(2) 0.114(17) 0.075(14) 0.004(13) 0.039(13) -0.078(16) C68 0.080(11) 0.082(13) 0.065(12) 0.002(10) 0.005(9) -0.034(10) C69 0.102(13) 0.040(10) 0.102(14) 0.021(9) -0.032(11) -0.022(9) C70 0.147(18) 0.071(14) 0.16(2) 0.008(14) -0.052(16) -0.010(13) C71 0.154(19) 0.133(19) 0.141(19) -0.019(15) -0.050(16) -0.066(16) C72 0.090(13) 0.072(13) 0.098(14) -0.025(11) 0.053(11) -0.023(11) C73 0.25(3) 0.11(2) 0.25(3) -0.07(2) -0.11(3) 0.01(2) C74 0.21(3) 0.12(2) 0.66(8) -0.11(3) -0.27(4) 0.03(2) C75 0.054(8) 0.038(8) 0.035(8) -0.008(6) -0.008(7) -0.005(6) C76 0.071(9) 0.043(8) 0.039(8) 0.000(7) -0.008(7) -0.014(7) C77 0.087(12) 0.072(11) 0.050(10) -0.020(8) 0.000(9) -0.017(9) C78 0.114(14) 0.080(12) 0.042(10) -0.031(9) 0.009(10) -0.011(11) C79 0.073(11) 0.081(12) 0.057(11) -0.013(9) 0.019(9) 0.002(9) C80 0.053(9) 0.053(9) 0.040(9) 0.008(7) 0.003(7) -0.009(7) C81 0.056(8) 0.061(9) 0.037(8) -0.004(7) -0.024(7) -0.011(7) C82 0.075(10) 0.096(13) 0.078(12) 0.005(10) -0.041(9) -0.020(9) C83 0.087(11) 0.073(11) 0.085(12) 0.012(10) -0.034(10) -0.013(9) C84 0.037(8) 0.084(11) 0.053(9) -0.002(8) -0.002(7) 0.002(8) C85 0.071(11) 0.103(13) 0.077(12) 0.004(10) -0.010(9) -0.025(10) C86 0.077(12) 0.105(15) 0.103(14) 0.031(12) -0.024(10) 0.014(10) C87 0.054(9) 0.031(8) 0.059(9) 0.014(7) -0.026(7) -0.014(7) C88 0.052(9) 0.073(11) 0.067(11) 0.000(9) -0.018(8) -0.024(9) C89 0.074(11) 0.083(14) 0.105(15) 0.021(11) -0.019(10) -0.038(11) C90 0.111(16) 0.087(15) 0.118(17) 0.018(13) -0.025(13) -0.060(13) C91 0.114(15) 0.060(12) 0.105(15) -0.010(10) -0.018(12) -0.029(11) C92 0.081(11) 0.050(10) 0.063(10) -0.001(8) -0.019(8) -0.035(8) C93 0.045(9) 0.096(14) 0.090(13) -0.006(11) 0.003(9) -0.027(9) C94 0.097(14) 0.091(16) 0.18(2) -0.011(15) -0.040(14) 0.008(12) C95 0.120(18) 0.17(2) 0.13(2) -0.015(17) 0.041(15) -0.007(16) C96 0.091(12) 0.041(10) 0.102(14) -0.011(9) -0.007(11) -0.015(9) C97 0.151(18) 0.083(14) 0.117(17) -0.039(12) 0.009(14) -0.037(13) C98 0.093(13) 0.050(11) 0.146(18) -0.009(11) -0.019(12) 0.013(9) C99 0.037(8) 0.066(10) 0.083(11) 0.008(9) -0.023(7) 0.018(7) C100 0.096(15) 0.16(2) 0.15(2) 0.010(16) -0.042(14) 0.063(15) C101 0.19(3) 0.20(3) 0.20(3) -0.09(2) 0.09(2) -0.03(2) C102 0.14(2) 0.10(2) 0.20(3) 0.00(2) -0.05(2) 0.007(19) C103 0.26(4) 0.19(3) 0.19(3) 0.05(2) 0.02(3) -0.06(3) C105 0.27(3) 0.27(3) 0.13(4) -0.05(3) 0.07(3) -0.21(2) C104 0.125(8) 0.102(9) 0.117(9) -0.011(7) -0.013(7) -0.041(7) C106 0.100(8) 0.116(9) 0.103(9) -0.006(7) -0.014(7) -0.028(7) _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 P1 2.251(3) . ? Pd1 P2 2.251(3) . ? Pd1 Cl2 2.394(3) . ? Pd1 Cl1 2.441(3) . ? Pd2 P4 2.253(3) . ? Pd2 P3 2.257(3) . ? Pd2 Cl1 2.395(3) . ? Pd2 Cl2 2.445(3) . ? P1 O1 1.597(7) . ? P1 O2 1.599(8) . ? P1 N1 1.611(9) . ? P2 O5 1.477(8) . ? P2 O3 1.603(8) . ? P2 O4 1.610(8) . ? P3 O7 1.601(8) . ? P3 N2 1.602(10) . ? P3 O6 1.610(8) . ? P4 O10 1.482(8) . ? P4 O8 1.605(8) . ? P4 O9 1.606(8) . ? O1 C1 1.425(13) . ? O2 C13 1.426(13) . ? O3 C25 1.417(13) . ? O4 C37 1.397(13) . ? O6 C51 1.426(13) . ? O7 C63 1.412(14) . ? O8 C75 1.410(13) . ? O9 C87 1.397(13) . ? O11 C102 1.27(3) . ? O12 C105 1.29(3) . ? N1 C49 1.463(14) . ? N1 H1 0.8600 . ? N2 C99 1.471(14) . ? N2 H2 0.8600 . ? C1 C6 1.386(15) . ? C1 C2 1.395(16) . ? C2 C3 1.389(17) . ? C2 C7 1.510(17) . ? C3 C4 1.387(19) . ? C3 H3 0.9300 . ? C4 C5 1.353(18) . ? C4 H4 0.9300 . ? C5 C6 1.397(16) . ? C5 H5 0.9300 . ? C6 C10 1.509(15) . ? C7 C8 1.521(18) . ? C7 C9 1.526(19) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C12 1.510(16) . ? C10 C11 1.531(16) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.380(16) . ? C13 C14 1.385(16) . ? C14 C15 1.409(18) . ? C14 C19 1.502(18) . ? C15 C16 1.343(19) . ? C15 H15 0.9300 . ? C16 C17 1.37(2) . ? C16 H16 0.9300 . ? C17 C18 1.396(18) . ? C17 H17 0.9300 . ? C18 C22 1.531(17) . ? C19 C20 1.528(19) . ? C19 C21 1.539(19) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.45(2) . ? C22 C24 1.468(19) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.394(17) . ? C25 C30 1.392(16) . ? C26 C27 1.376(18) . ? C26 C31 1.518(18) . ? C27 C28 1.35(2) . ? C27 H27 0.9300 . ? C28 C29 1.36(2) . ? C28 H28 0.9300 . ? C29 C30 1.386(17) . ? C29 H29 0.9300 . ? C30 C34 1.519(17) . ? C31 C33 1.517(19) . ? C31 C32 1.54(2) . ? C31 H31 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C36 1.472(17) . ? C34 C35 1.557(18) . ? C34 H34 0.9800 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C42 1.381(17) . ? C37 C38 1.412(17) . ? C38 C39 1.405(18) . ? C38 C43 1.51(2) . ? C39 C40 1.37(2) . ? C39 H39 0.9300 . ? C40 C41 1.36(2) . ? C40 H40 0.9300 . ? C41 C42 1.375(18) . ? C41 H41 0.9300 . ? C42 C46 1.524(19) . ? C43 C45 1.48(2) . ? C43 C44 1.51(2) . ? C43 H43 0.9800 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C48 1.516(19) . ? C46 C47 1.535(19) . ? C46 H46 0.9800 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.33(2) . ? C49 H49 0.9300 . ? C50 H50A 0.9300 . ? C50 H50B 0.9300 . ? C51 C52 1.373(17) . ? C51 C56 1.398(17) . ? C52 C53 1.395(17) . ? C52 C57 1.521(17) . ? C53 C54 1.37(2) . ? C53 H53 0.9300 . ? C54 C55 1.38(2) . ? C54 H54 0.9300 . ? C55 C56 1.38(2) . ? C55 H55 0.9300 . ? C56 C60 1.52(2) . ? C57 C58 1.509(17) . ? C57 C59 1.509(17) . ? C57 H57 0.9800 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C61 1.48(2) . ? C60 C62 1.53(2) . ? C60 H60 0.9800 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 C68 1.389(19) . ? C63 C64 1.391(19) . ? C64 C65 1.40(2) . ? C64 C69 1.52(2) . ? C65 C66 1.35(3) . ? C65 H65 0.9300 . ? C66 C67 1.37(3) . ? C66 H66 0.9300 . ? C67 C68 1.40(2) . ? C67 H67 0.9300 . ? C68 C72 1.51(2) . ? C69 C71 1.51(2) . ? C69 C70 1.52(2) . ? C69 H69 0.9800 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 C74 1.43(3) . ? C72 C73 1.45(2) . ? C72 H72 0.9800 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 C80 1.381(16) . ? C75 C76 1.385(16) . ? C76 C77 1.380(17) . ? C76 C81 1.514(17) . ? C77 C78 1.37(2) . ? C77 H77 0.9300 . ? C78 C79 1.39(2) . ? C78 H78 0.9300 . ? C79 C80 1.388(17) . ? C79 H79 0.9300 . ? C80 C84 1.522(17) . ? C81 C82 1.520(17) . ? C81 C83 1.551(17) . ? C81 H81 0.9800 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 C85 1.520(18) . ? C84 C86 1.536(19) . ? C84 H84 0.9800 . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C87 C88 1.360(17) . ? C87 C92 1.388(17) . ? C88 C89 1.378(19) . ? C88 C93 1.504(19) . ? C89 C90 1.39(2) . ? C89 H89 0.9300 . ? C90 C91 1.37(2) . ? C90 H90 0.9300 . ? C91 C92 1.389(19) . ? C91 H91 0.9300 . ? C92 C96 1.501(19) . ? C93 C95 1.51(2) . ? C93 C94 1.52(2) . ? C93 H93 0.9800 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C95 H95C 0.9600 . ? C96 C98 1.52(2) . ? C96 C97 1.54(2) . ? C96 H96 0.9800 . ? C97 H97A 0.9600 . ? C97 H97B 0.9600 . ? C97 H97C 0.9600 . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? C99 C100 1.46(2) . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? C101 C102 1.43(3) . ? C101 H10D 0.9600 . ? C101 H10E 0.9600 . ? C101 H10F 0.9600 . ? C102 C103 1.48(3) . ? C103 H10G 0.9600 . ? C103 H10H 0.9600 . ? C103 H10I 0.9600 . ? C105 C106 1.45(4) . ? C105 C104 1.42(3) . ? C104 H10J 0.9600 . ? C104 H10K 0.9600 . ? C104 H10L 0.9600 . ? C106 H10M 0.9600 . ? C106 H10N 0.9600 . ? C106 H10O 0.9600 . ? 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 P1 Pd1 P2 90.78(11) . . ? P1 Pd1 Cl2 175.37(7) . . ? P2 Pd1 Cl2 92.78(8) . . ? P1 Pd1 Cl1 93.74(8) . . ? P2 Pd1 Cl1 174.99(8) . . ? Cl2 Pd1 Cl1 82.83(9) . . ? P4 Pd2 P3 91.32(11) . . ? P4 Pd2 Cl1 93.11(8) . . ? P3 Pd2 Cl1 174.58(8) . . ? P4 Pd2 Cl2 175.47(8) . . ? P3 Pd2 Cl2 92.93(9) . . ? Cl1 Pd2 Cl2 82.74(9) . . ? Pd2 Cl1 Pd1 94.51(9) . . ? Pd1 Cl2 Pd2 94.41(9) . . ? O1 P1 O2 101.0(4) . . ? O1 P1 N1 104.8(4) . . ? O2 P1 N1 114.2(5) . . ? O1 P1 Pd1 115.5(3) . . ? O2 P1 Pd1 101.5(3) . . ? N1 P1 Pd1 118.7(4) . . ? O5 P2 O3 113.2(4) . . ? O5 P2 O4 109.9(4) . . ? O3 P2 O4 99.8(4) . . ? O5 P2 Pd1 120.2(3) . . ? O3 P2 Pd1 100.1(3) . . ? O4 P2 Pd1 111.4(3) . . ? O7 P3 N2 114.8(5) . . ? O7 P3 O6 100.6(4) . . ? N2 P3 O6 104.9(5) . . ? O7 P3 Pd2 101.3(3) . . ? N2 P3 Pd2 118.4(4) . . ? O6 P3 Pd2 115.7(3) . . ? O10 P4 O8 112.6(4) . . ? O10 P4 O9 109.6(4) . . ? O8 P4 O9 99.2(4) . . ? O10 P4 Pd2 120.4(3) . . ? O8 P4 Pd2 100.9(3) . . ? O9 P4 Pd2 111.8(3) . . ? C1 O1 P1 128.8(7) . . ? C13 O2 P1 132.2(7) . . ? C25 O3 P2 121.7(7) . . ? C37 O4 P2 126.3(7) . . ? C51 O6 P3 129.4(8) . . ? C63 O7 P3 131.6(8) . . ? C75 O8 P4 123.0(7) . . ? C87 O9 P4 126.0(7) . . ? C49 N1 P1 130.7(8) . . ? C49 N1 H1 114.7 . . ? P1 N1 H1 114.7 . . ? C99 N2 P3 129.9(9) . . ? C99 N2 H2 115.0 . . ? P3 N2 H2 115.0 . . ? C6 C1 C2 122.5(11) . . ? C6 C1 O1 121.7(10) . . ? C2 C1 O1 115.8(10) . . ? C3 C2 C1 117.4(12) . . ? C3 C2 C7 118.4(12) . . ? C1 C2 C7 124.2(11) . . ? C4 C3 C2 120.8(13) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 120.5(13) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 121.1(13) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C1 C6 C5 117.7(12) . . ? C1 C6 C10 125.2(10) . . ? C5 C6 C10 117.1(11) . . ? C2 C7 C8 113.5(12) . . ? C2 C7 C9 110.3(12) . . ? C8 C7 C9 109.0(12) . . ? C2 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C6 112.7(11) . . ? C12 C10 C11 109.4(10) . . ? C6 C10 C11 111.5(10) . . ? C12 C10 H10 107.7 . . ? C6 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 125.7(12) . . ? C18 C13 O2 116.2(11) . . ? C14 C13 O2 117.7(12) . . ? C13 C14 C15 114.3(13) . . ? C13 C14 C19 124.0(12) . . ? C15 C14 C19 121.3(13) . . ? C16 C15 C14 121.6(14) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C17 122.1(14) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C16 C17 C18 119.8(14) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C13 C18 C17 116.1(13) . . ? C13 C18 C22 123.4(12) . . ? C17 C18 C22 120.4(13) . . ? C14 C19 C20 114.6(13) . . ? C14 C19 C21 109.9(12) . . ? C20 C19 C21 110.7(13) . . ? C14 C19 H19 107.1 . . ? C20 C19 H19 107.1 . . ? C21 C19 H19 107.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C24 110.0(16) . . ? C23 C22 C18 113.7(14) . . ? C24 C22 C18 109.1(12) . . ? C23 C22 H22 107.9 . . ? C24 C22 H22 107.9 . . ? C18 C22 H22 107.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 123.1(12) . . ? C26 C25 O3 118.5(11) . . ? C30 C25 O3 118.3(11) . . ? C27 C26 C25 115.6(14) . . ? C27 C26 C31 121.7(14) . . ? C25 C26 C31 122.4(12) . . ? C28 C27 C26 123.3(16) . . ? C28 C27 H27 118.3 . . ? C26 C27 H27 118.3 . . ? C27 C28 C29 119.5(15) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 121.9(15) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C25 116.3(13) . . ? C29 C30 C34 119.5(12) . . ? C25 C30 C34 124.2(11) . . ? C33 C31 C26 112.2(13) . . ? C33 C31 C32 110.3(14) . . ? C26 C31 C32 109.9(13) . . ? C33 C31 H31 108.1 . . ? C26 C31 H31 108.1 . . ? C32 C31 H31 108.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C34 C30 113.2(12) . . ? C36 C34 C35 112.1(12) . . ? C30 C34 C35 108.1(12) . . ? C36 C34 H34 107.7 . . ? C30 C34 H34 107.7 . . ? C35 C34 H34 107.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C42 C37 O4 122.3(12) . . ? C42 C37 C38 121.7(12) . . ? O4 C37 C38 115.7(11) . . ? C39 C38 C37 116.3(14) . . ? C39 C38 C43 122.2(14) . . ? C37 C38 C43 121.3(12) . . ? C40 C39 C38 122.1(15) . . ? C40 C39 H39 118.9 . . ? C38 C39 H39 118.9 . . ? C41 C40 C39 119.0(14) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C40 C41 C42 122.5(15) . . ? C40 C41 H41 118.7 . . ? C42 C41 H41 118.7 . . ? C41 C42 C37 118.3(14) . . ? C41 C42 C46 117.7(13) . . ? C37 C42 C46 124.0(12) . . ? C45 C43 C44 107.8(17) . . ? C45 C43 C38 110.7(15) . . ? C44 C43 C38 111.7(16) . . ? C45 C43 H43 108.8 . . ? C44 C43 H43 108.8 . . ? C38 C43 H43 108.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C48 C46 C42 111.4(13) . . ? C48 C46 C47 112.9(13) . . ? C42 C46 C47 110.9(13) . . ? C48 C46 H46 107.1 . . ? C42 C46 H46 107.1 . . ? C47 C46 H46 107.1 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 N1 116.0(13) . . ? C50 C49 H49 122.0 . . ? N1 C49 H49 122.0 . . ? C49 C50 H50A 120.0 . . ? C49 C50 H50B 120.0 . . ? H50A C50 H50B 120.0 . . ? C52 C51 C56 123.6(12) . . ? C52 C51 O6 120.5(12) . . ? C56 C51 O6 115.8(12) . . ? C51 C52 C53 116.8(14) . . ? C51 C52 C57 126.1(11) . . ? C53 C52 C57 117.1(12) . . ? C54 C53 C52 120.8(15) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C53 C54 C55 121.5(16) . . ? C53 C54 H54 119.2 . . ? C55 C54 H54 119.2 . . ? C56 C55 C54 119.3(17) . . ? C56 C55 H55 120.3 . . ? C54 C55 H55 120.3 . . ? C55 C56 C51 117.9(15) . . ? C55 C56 C60 118.3(15) . . ? C51 C56 C60 123.8(13) . . ? C58 C57 C59 110.7(11) . . ? C58 C57 C52 110.9(12) . . ? C59 C57 C52 111.2(12) . . ? C58 C57 H57 108.0 . . ? C59 C57 H57 108.0 . . ? C52 C57 H57 108.0 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C61 C60 C56 115.0(17) . . ? C61 C60 C62 110.9(15) . . ? C56 C60 C62 109.5(16) . . ? C61 C60 H60 107.0 . . ? C56 C60 H60 107.0 . . ? C62 C60 H60 107.0 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C68 C63 C64 123.4(14) . . ? C68 C63 O7 117.9(13) . . ? C64 C63 O7 118.5(14) . . ? C65 C64 C63 116.8(17) . . ? C65 C64 C69 121.2(16) . . ? C63 C64 C69 121.5(14) . . ? C66 C65 C64 120.2(19) . . ? C66 C65 H65 119.9 . . ? C64 C65 H65 119.9 . . ? C65 C66 C67 123(2) . . ? C65 C66 H66 118.5 . . ? C67 C66 H66 118.5 . . ? C66 C67 C68 118.8(19) . . ? C66 C67 H67 120.6 . . ? C68 C67 H67 120.6 . . ? C63 C68 C67 117.5(17) . . ? C63 C68 C72 121.0(14) . . ? C67 C68 C72 121.4(17) . . ? C71 C69 C64 111.3(15) . . ? C71 C69 C70 110.2(14) . . ? C64 C69 C70 113.4(15) . . ? C71 C69 H69 107.2 . . ? C64 C69 H69 107.2 . . ? C70 C69 H69 107.2 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C74 C72 C73 104.7(19) . . ? C74 C72 C68 110.3(17) . . ? C73 C72 C68 115.9(19) . . ? C74 C72 H72 108.5 . . ? C73 C72 H72 108.5 . . ? C68 C72 H72 108.5 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C80 C75 C76 123.2(12) . . ? C80 C75 O8 118.4(11) . . ? C76 C75 O8 118.2(11) . . ? C77 C76 C75 117.5(13) . . ? C77 C76 C81 119.3(13) . . ? C75 C76 C81 123.0(11) . . ? C78 C77 C76 122.0(15) . . ? C78 C77 H77 119.0 . . ? C76 C77 H77 119.0 . . ? C77 C78 C79 118.2(14) . . ? C77 C78 H78 120.9 . . ? C79 C78 H78 120.9 . . ? C78 C79 C80 122.5(14) . . ? C78 C79 H79 118.7 . . ? C80 C79 H79 118.7 . . ? C75 C80 C79 116.2(13) . . ? C75 C80 C84 124.2(12) . . ? C79 C80 C84 119.5(13) . . ? C76 C81 C82 111.6(11) . . ? C76 C81 C83 110.7(11) . . ? C82 C81 C83 110.8(11) . . ? C76 C81 H81 107.9 . . ? C82 C81 H81 107.9 . . ? C83 C81 H81 107.9 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C85 C84 C80 111.0(11) . . ? C85 C84 C86 112.6(12) . . ? C80 C84 C86 111.7(13) . . ? C85 C84 H84 107.1 . . ? C80 C84 H84 107.1 . . ? C86 C84 H84 107.1 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C88 C87 C92 122.8(12) . . ? C88 C87 O9 118.2(12) . . ? C92 C87 O9 118.6(12) . . ? C87 C88 C89 119.5(15) . . ? C87 C88 C93 120.9(13) . . ? C89 C88 C93 119.5(14) . . ? C88 C89 C90 120.3(16) . . ? C88 C89 H89 119.8 . . ? C90 C89 H89 119.8 . . ? C91 C90 C89 118.0(16) . . ? C91 C90 H90 121.0 . . ? C89 C90 H90 121.0 . . ? C90 C91 C92 123.5(16) . . ? C90 C91 H91 118.3 . . ? C92 C91 H91 118.3 . . ? C91 C92 C87 115.8(14) . . ? C91 C92 C96 117.5(14) . . ? C87 C92 C96 126.7(12) . . ? C88 C93 C95 117.1(15) . . ? C88 C93 C94 108.6(14) . . ? C95 C93 C94 108.8(15) . . ? C88 C93 H93 107.3 . . ? C95 C93 H93 107.3 . . ? C94 C93 H93 107.3 . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C93 C95 H95A 109.5 . . ? C93 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C93 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C92 C96 C98 113.2(14) . . ? C92 C96 C97 111.0(14) . . ? C98 C96 C97 110.4(14) . . ? C92 C96 H96 107.3 . . ? C98 C96 H96 107.3 . . ? C97 C96 H96 107.3 . . ? C96 C97 H97A 109.5 . . ? C96 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C96 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C96 C98 H98A 109.5 . . ? C96 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C96 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C100 C99 N2 111.1(13) . . ? C100 C99 H99A 109.4 . . ? N2 C99 H99A 109.4 . . ? C100 C99 H99B 109.4 . . ? N2 C99 H99B 109.4 . . ? H99A C99 H99B 108.0 . . ? C99 C100 H10A 109.5 . . ? C99 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C99 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C102 C101 H10D 109.5 . . ? C102 C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? C102 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? O11 C102 C101 118(3) . . ? O11 C102 C103 119(3) . . ? C101 C102 C103 123(3) . . ? C102 C103 H10G 109.5 . . ? C102 C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? C102 C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? O12 C105 C106 111(3) . . ? O12 C105 C104 116(3) . . ? C106 C105 C104 133(2) . . ? C105 C104 H10J 109.5 . . ? C105 C104 H10K 109.5 . . ? H10J C104 H10K 109.5 . . ? C105 C104 H10L 109.5 . . ? H10J C104 H10L 109.5 . . ? H10K C104 H10L 109.5 . . ? C105 C106 H10M 109.5 . . ? C105 C106 H10N 109.5 . . ? H10M C106 H10N 109.5 . . ? C105 C106 H10O 109.5 . . ? H10M C106 H10O 109.5 . . ? H10N C106 H10O 109.5 . . ? 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 P4 Pd2 Cl1 Pd1 -160.71(7) . . . . ? Cl2 Pd2 Cl1 Pd1 17.50(8) . . . . ? P1 Pd1 Cl1 Pd2 165.25(7) . . . . ? Cl2 Pd1 Cl1 Pd2 -17.88(9) . . . . ? P2 Pd1 Cl2 Pd2 -160.09(7) . . . . ? Cl1 Pd1 Cl2 Pd2 17.49(9) . . . . ? P3 Pd2 Cl2 Pd1 165.42(7) . . . . ? Cl1 Pd2 Cl2 Pd1 -17.85(9) . . . . ? P2 Pd1 P1 O1 161.9(3) . . . . ? Cl1 Pd1 P1 O1 -15.9(3) . . . . ? P2 Pd1 P1 O2 -89.8(3) . . . . ? Cl1 Pd1 P1 O2 92.3(3) . . . . ? P2 Pd1 P1 N1 36.2(4) . . . . ? Cl1 Pd1 P1 N1 -141.6(4) . . . . ? P1 Pd1 P2 O5 -7.7(4) . . . . ? Cl2 Pd1 P2 O5 175.3(4) . . . . ? P1 Pd1 P2 O3 -132.2(3) . . . . ? Cl2 Pd1 P2 O3 50.7(3) . . . . ? P1 Pd1 P2 O4 122.9(3) . . . . ? Cl2 Pd1 P2 O4 -54.1(3) . . . . ? P4 Pd2 P3 O7 -91.6(3) . . . . ? Cl2 Pd2 P3 O7 89.9(3) . . . . ? P4 Pd2 P3 N2 34.9(4) . . . . ? Cl2 Pd2 P3 N2 -143.5(4) . . . . ? P4 Pd2 P3 O6 160.6(3) . . . . ? Cl2 Pd2 P3 O6 -17.8(3) . . . . ? P3 Pd2 P4 O10 -9.3(4) . . . . ? Cl1 Pd2 P4 O10 173.9(4) . . . . ? P3 Pd2 P4 O8 -133.8(3) . . . . ? Cl1 Pd2 P4 O8 49.3(3) . . . . ? P3 Pd2 P4 O9 121.6(3) . . . . ? Cl1 Pd2 P4 O9 -55.3(3) . . . . ? O2 P1 O1 C1 143.1(9) . . . . ? N1 P1 O1 C1 24.2(10) . . . . ? Pd1 P1 O1 C1 -108.4(8) . . . . ? O1 P1 O2 C13 -43.0(11) . . . . ? N1 P1 O2 C13 68.9(11) . . . . ? Pd1 P1 O2 C13 -162.1(10) . . . . ? O5 P2 O3 C25 49.5(9) . . . . ? O4 P2 O3 C25 -67.3(9) . . . . ? Pd1 P2 O3 C25 178.7(8) . . . . ? O5 P2 O4 C37 31.1(10) . . . . ? O3 P2 O4 C37 150.3(9) . . . . ? Pd1 P2 O4 C37 -104.6(9) . . . . ? O7 P3 O6 C51 143.5(10) . . . . ? N2 P3 O6 C51 24.1(11) . . . . ? Pd2 P3 O6 C51 -108.3(10) . . . . ? N2 P3 O7 C63 72.9(12) . . . . ? O6 P3 O7 C63 -39.1(12) . . . . ? Pd2 P3 O7 C63 -158.3(11) . . . . ? O10 P4 O8 C75 51.7(9) . . . . ? O9 P4 O8 C75 -64.1(9) . . . . ? Pd2 P4 O8 C75 -178.6(8) . . . . ? O10 P4 O9 C87 34.4(10) . . . . ? O8 P4 O9 C87 152.5(9) . . . . ? Pd2 P4 O9 C87 -101.7(9) . . . . ? O1 P1 N1 C49 42.8(11) . . . . ? O2 P1 N1 C49 -66.7(11) . . . . ? Pd1 P1 N1 C49 173.6(9) . . . . ? O7 P3 N2 C99 -70.9(12) . . . . ? O6 P3 N2 C99 38.6(12) . . . . ? Pd2 P3 N2 C99 169.4(10) . . . . ? P1 O1 C1 C6 58.8(14) . . . . ? P1 O1 C1 C2 -123.8(10) . . . . ? C6 C1 C2 C3 -0.9(19) . . . . ? O1 C1 C2 C3 -178.3(11) . . . . ? C6 C1 C2 C7 -179.0(12) . . . . ? O1 C1 C2 C7 3.6(18) . . . . ? C1 C2 C3 C4 0(2) . . . . ? C7 C2 C3 C4 178.4(14) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C3 C4 C5 C6 1(2) . . . . ? C2 C1 C6 C5 1.5(18) . . . . ? O1 C1 C6 C5 178.7(10) . . . . ? C2 C1 C6 C10 -177.9(11) . . . . ? O1 C1 C6 C10 -0.6(18) . . . . ? C4 C5 C6 C1 -1.4(19) . . . . ? C4 C5 C6 C10 178.0(12) . . . . ? C3 C2 C7 C8 -60.2(17) . . . . ? C1 C2 C7 C8 117.9(14) . . . . ? C3 C2 C7 C9 62.5(17) . . . . ? C1 C2 C7 C9 -119.5(14) . . . . ? C1 C6 C10 C12 118.9(13) . . . . ? C5 C6 C10 C12 -60.5(14) . . . . ? C1 C6 C10 C11 -117.6(13) . . . . ? C5 C6 C10 C11 63.1(15) . . . . ? P1 O2 C13 C18 95.9(12) . . . . ? P1 O2 C13 C14 -90.7(13) . . . . ? C18 C13 C14 C15 -8.1(19) . . . . ? O2 C13 C14 C15 179.2(11) . . . . ? C18 C13 C14 C19 165.2(12) . . . . ? O2 C13 C14 C19 -7.6(18) . . . . ? C13 C14 C15 C16 3(2) . . . . ? C19 C14 C15 C16 -170.0(14) . . . . ? C14 C15 C16 C17 0(3) . . . . ? C15 C16 C17 C18 1(2) . . . . ? C14 C13 C18 C17 8.7(19) . . . . ? O2 C13 C18 C17 -178.5(10) . . . . ? C14 C13 C18 C22 -166.5(12) . . . . ? O2 C13 C18 C22 6.3(17) . . . . ? C16 C17 C18 C13 -5(2) . . . . ? C16 C17 C18 C22 170.8(13) . . . . ? C13 C14 C19 C20 150.3(13) . . . . ? C15 C14 C19 C20 -37.0(19) . . . . ? C13 C14 C19 C21 -84.3(16) . . . . ? C15 C14 C19 C21 88.4(16) . . . . ? C13 C18 C22 C23 -133.2(18) . . . . ? C17 C18 C22 C23 52(2) . . . . ? C13 C18 C22 C24 103.6(16) . . . . ? C17 C18 C22 C24 -71.5(19) . . . . ? P2 O3 C25 C26 98.1(12) . . . . ? P2 O3 C25 C30 -86.3(12) . . . . ? C30 C25 C26 C27 5(2) . . . . ? O3 C25 C26 C27 -180.0(12) . . . . ? C30 C25 C26 C31 -169.5(13) . . . . ? O3 C25 C26 C31 6(2) . . . . ? C25 C26 C27 C28 1(3) . . . . ? C31 C26 C27 C28 175.0(18) . . . . ? C26 C27 C28 C29 -5(3) . . . . ? C27 C28 C29 C30 3(3) . . . . ? C28 C29 C30 C25 2(2) . . . . ? C28 C29 C30 C34 -175.7(17) . . . . ? C26 C25 C30 C29 -6(2) . . . . ? O3 C25 C30 C29 178.6(11) . . . . ? C26 C25 C30 C34 171.6(13) . . . . ? O3 C25 C30 C34 -3.9(19) . . . . ? C27 C26 C31 C33 59(2) . . . . ? C25 C26 C31 C33 -127.2(15) . . . . ? C27 C26 C31 C32 -64(2) . . . . ? C25 C26 C31 C32 109.8(16) . . . . ? C29 C30 C34 C36 -56.6(18) . . . . ? C25 C30 C34 C36 125.9(14) . . . . ? C29 C30 C34 C35 68.2(16) . . . . ? C25 C30 C34 C35 -109.2(14) . . . . ? P2 O4 C37 C42 -74.6(15) . . . . ? P2 O4 C37 C38 111.4(11) . . . . ? C42 C37 C38 C39 3(2) . . . . ? O4 C37 C38 C39 177.1(12) . . . . ? C42 C37 C38 C43 -171.5(15) . . . . ? O4 C37 C38 C43 2(2) . . . . ? C37 C38 C39 C40 0(2) . . . . ? C43 C38 C39 C40 174.8(17) . . . . ? C38 C39 C40 C41 -2(3) . . . . ? C39 C40 C41 C42 1(3) . . . . ? C40 C41 C42 C37 2(2) . . . . ? C40 C41 C42 C46 -176.0(14) . . . . ? O4 C37 C42 C41 -177.8(12) . . . . ? C38 C37 C42 C41 -4(2) . . . . ? O4 C37 C42 C46 0(2) . . . . ? C38 C37 C42 C46 173.6(13) . . . . ? C39 C38 C43 C45 -52(2) . . . . ? C37 C38 C43 C45 122.7(18) . . . . ? C39 C38 C43 C44 69(2) . . . . ? C37 C38 C43 C44 -117.1(17) . . . . ? C41 C42 C46 C48 64.0(18) . . . . ? C37 C42 C46 C48 -113.8(16) . . . . ? C41 C42 C46 C47 -62.6(17) . . . . ? C37 C42 C46 C47 119.6(15) . . . . ? P1 N1 C49 C50 -159.3(19) . . . . ? P3 O6 C51 C52 60.3(16) . . . . ? P3 O6 C51 C56 -123.6(12) . . . . ? C56 C51 C52 C53 1(2) . . . . ? O6 C51 C52 C53 176.5(12) . . . . ? C56 C51 C52 C57 -178.2(14) . . . . ? O6 C51 C52 C57 -2(2) . . . . ? C51 C52 C53 C54 -1(2) . . . . ? C57 C52 C53 C54 177.5(16) . . . . ? C52 C53 C54 C55 1(3) . . . . ? C53 C54 C55 C56 0(3) . . . . ? C54 C55 C56 C51 -1(3) . . . . ? C54 C55 C56 C60 -179.8(19) . . . . ? C52 C51 C56 C55 0(2) . . . . ? O6 C51 C56 C55 -175.6(14) . . . . ? C52 C51 C56 C60 179.5(16) . . . . ? O6 C51 C56 C60 3(2) . . . . ? C51 C52 C57 C58 120.8(15) . . . . ? C53 C52 C57 C58 -58.0(17) . . . . ? C51 C52 C57 C59 -115.5(15) . . . . ? C53 C52 C57 C59 65.7(16) . . . . ? C55 C56 C60 C61 -55(2) . . . . ? C51 C56 C60 C61 126.3(18) . . . . ? C55 C56 C60 C62 71(2) . . . . ? C51 C56 C60 C62 -108.1(18) . . . . ? P3 O7 C63 C68 94.0(15) . . . . ? P3 O7 C63 C64 -90.5(15) . . . . ? C68 C63 C64 C65 -4(2) . . . . ? O7 C63 C64 C65 -179.5(14) . . . . ? C68 C63 C64 C69 167.7(14) . . . . ? O7 C63 C64 C69 -8(2) . . . . ? C63 C64 C65 C66 0(3) . . . . ? C69 C64 C65 C66 -171.8(19) . . . . ? C64 C65 C66 C67 2(4) . . . . ? C65 C66 C67 C68 0(4) . . . . ? C64 C63 C68 C67 6(2) . . . . ? O7 C63 C68 C67 -178.5(14) . . . . ? C64 C63 C68 C72 -170.6(15) . . . . ? O7 C63 C68 C72 5(2) . . . . ? C66 C67 C68 C63 -4(3) . . . . ? C66 C67 C68 C72 173(2) . . . . ? C65 C64 C69 C71 89(2) . . . . ? C63 C64 C69 C71 -82.2(18) . . . . ? C65 C64 C69 C70 -36(2) . . . . ? C63 C64 C69 C70 152.9(15) . . . . ? C63 C68 C72 C74 96(2) . . . . ? C67 C68 C72 C74 -81(3) . . . . ? C63 C68 C72 C73 -145.6(19) . . . . ? C67 C68 C72 C73 38(3) . . . . ? P4 O8 C75 C80 -86.8(12) . . . . ? P4 O8 C75 C76 97.3(11) . . . . ? C80 C75 C76 C77 3.2(19) . . . . ? O8 C75 C76 C77 178.9(11) . . . . ? C80 C75 C76 C81 -171.3(12) . . . . ? O8 C75 C76 C81 4.4(18) . . . . ? C75 C76 C77 C78 1(2) . . . . ? C81 C76 C77 C78 175.4(13) . . . . ? C76 C77 C78 C79 -4(2) . . . . ? C77 C78 C79 C80 3(2) . . . . ? C76 C75 C80 C79 -3.5(19) . . . . ? O8 C75 C80 C79 -179.2(11) . . . . ? C76 C75 C80 C84 174.0(12) . . . . ? O8 C75 C80 C84 -1.7(18) . . . . ? C78 C79 C80 C75 0(2) . . . . ? C78 C79 C80 C84 -177.5(14) . . . . ? C77 C76 C81 C82 59.7(16) . . . . ? C75 C76 C81 C82 -125.9(13) . . . . ? C77 C76 C81 C83 -64.2(15) . . . . ? C75 C76 C81 C83 110.2(14) . . . . ? C75 C80 C84 C85 -111.1(14) . . . . ? C79 C80 C84 C85 66.4(17) . . . . ? C75 C80 C84 C86 122.4(14) . . . . ? C79 C80 C84 C86 -60.2(16) . . . . ? P4 O9 C87 C88 103.5(12) . . . . ? P4 O9 C87 C92 -84.1(13) . . . . ? C92 C87 C88 C89 1(2) . . . . ? O9 C87 C88 C89 173.5(12) . . . . ? C92 C87 C88 C93 -176.5(13) . . . . ? O9 C87 C88 C93 -4.5(19) . . . . ? C87 C88 C89 C90 2(2) . . . . ? C93 C88 C89 C90 179.9(16) . . . . ? C88 C89 C90 C91 -4(3) . . . . ? C89 C90 C91 C92 2(3) . . . . ? C90 C91 C92 C87 1(2) . . . . ? C90 C91 C92 C96 179.9(16) . . . . ? C88 C87 C92 C91 -3(2) . . . . ? O9 C87 C92 C91 -174.9(12) . . . . ? C88 C87 C92 C96 178.3(14) . . . . ? O9 C87 C92 C96 6(2) . . . . ? C87 C88 C93 C95 -156.0(15) . . . . ? C89 C88 C93 C95 26(2) . . . . ? C87 C88 C93 C94 80.3(17) . . . . ? C89 C88 C93 C94 -97.7(17) . . . . ? C91 C92 C96 C98 -63.1(19) . . . . ? C87 C92 C96 C98 115.7(16) . . . . ? C91 C92 C96 C97 61.8(19) . . . . ? C87 C92 C96 C97 -119.4(16) . . . . ? P3 N2 C99 C100 165.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.56 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.767 _refine_diff_density_min -1.812 _refine_diff_density_rms 0.098 ###END data_LigandL'_ _database_code_depnum_ccdc_archive 'CCDC 637409' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H73 N O5 P2' _chemical_formula_sum 'C50 H73 N O5 P2' _chemical_formula_weight 830.03 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.465(7) _cell_length_b 14.582(8) _cell_length_c 15.016(8) _cell_angle_alpha 68.274(9) _cell_angle_beta 70.498(8) _cell_angle_gamma 74.301(9) _cell_volume 2545(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 28.1 _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9390 _exptl_absorpt_correction_T_max 0.9472 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'bruker smart apex ccd' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29347 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.10 _reflns_number_total 11659 _reflns_number_gt 8442 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'bruker smart apex ccd' _computing_cell_refinement 'bruker smart apex ccd' _computing_data_reduction 'bruker saint' _computing_structure_solution shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ortep-iii _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^)+(0.0810P)^2^+0.3560P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11659 _refine_ls_number_parameters 540 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1522 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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 0.72273(4) 0.24475(4) 0.31259(4) 0.04027(14) Uani 1 1 d . . . P2 P 0.65908(4) 0.08997(4) 0.27276(3) 0.03828(14) Uani 1 1 d . . . O2 O 0.78120(10) 0.21286(11) 0.40226(10) 0.0470(3) Uani 1 1 d . . . O1 O 0.62148(11) 0.32411(10) 0.35598(10) 0.0459(3) Uani 1 1 d . . . O3 O 0.64105(11) 0.18980(10) 0.18467(9) 0.0440(3) Uani 1 1 d . . . O4 O 0.77344(10) 0.03796(10) 0.22113(10) 0.0437(3) Uani 1 1 d . . . O5 O 0.57842(11) 0.02512(11) 0.31655(10) 0.0495(3) Uani 1 1 d . . . N1 N 0.67048(12) 0.13763(11) 0.35302(11) 0.0392(4) Uani 1 1 d . . . C1 C 0.55948(18) 0.39551(15) 0.29268(15) 0.0477(5) Uani 1 1 d . . . C2 C 0.45312(18) 0.38565(16) 0.31386(17) 0.0548(5) Uani 1 1 d . . . C3 C 0.3936(2) 0.4564(2) 0.2504(2) 0.0740(7) Uani 1 1 d . . . H3 H 0.3226 0.4521 0.2614 0.089 Uiso 1 1 calc R . . C4 C 0.4377(3) 0.5324(2) 0.1719(2) 0.0860(9) Uani 1 1 d . . . H4 H 0.3975 0.5769 0.1289 0.103 Uiso 1 1 calc R . . C5 C 0.5406(3) 0.5427(2) 0.1569(2) 0.0761(8) Uani 1 1 d . . . H5 H 0.5683 0.5960 0.1050 0.091 Uiso 1 1 calc R . . C6 C 0.6050(2) 0.47546(17) 0.21725(17) 0.0588(6) Uani 1 1 d . . . C7 C 0.7136(2) 0.49383(19) 0.2095(2) 0.0720(7) Uani 1 1 d . . . H7 H 0.7612 0.4289 0.2198 0.086 Uiso 1 1 calc R . . C8 C 0.7657(3) 0.5637(3) 0.1090(3) 0.1142(13) Uani 1 1 d . . . H8A H 0.7696 0.5387 0.0569 0.171 Uiso 1 1 calc R . . H8B H 0.8364 0.5666 0.1081 0.171 Uiso 1 1 calc R . . H8C H 0.7237 0.6296 0.0991 0.171 Uiso 1 1 calc R . . C9 C 0.7048(3) 0.5346(2) 0.2936(3) 0.0922(10) Uani 1 1 d . . . H9A H 0.6625 0.6004 0.2830 0.138 Uiso 1 1 calc R . . H9B H 0.7749 0.5379 0.2938 0.138 Uiso 1 1 calc R . . H9C H 0.6715 0.4909 0.3562 0.138 Uiso 1 1 calc R . . C10 C 0.40266(19) 0.30633(19) 0.4054(2) 0.0657(6) Uani 1 1 d . . . H10 H 0.4523 0.2429 0.4082 0.079 Uiso 1 1 calc R . . C11 C 0.2958(2) 0.2896(3) 0.4054(3) 0.0976(10) Uani 1 1 d . . . H11A H 0.2441 0.3496 0.4058 0.146 Uiso 1 1 calc R . . H11B H 0.2717 0.2358 0.4634 0.146 Uiso 1 1 calc R . . H11C H 0.3041 0.2727 0.3469 0.146 Uiso 1 1 calc R . . C12 C 0.3899(3) 0.3311(3) 0.4994(2) 0.0980(10) Uani 1 1 d . . . H12A H 0.4572 0.3418 0.4993 0.147 Uiso 1 1 calc R . . H12B H 0.3667 0.2763 0.5567 0.147 Uiso 1 1 calc R . . H12C H 0.3378 0.3906 0.5013 0.147 Uiso 1 1 calc R . . C13 C 0.82727(17) 0.28175(18) 0.41542(16) 0.0535(5) Uani 1 1 d . . . C14 C 0.77484(19) 0.31422(18) 0.49872(18) 0.0587(6) Uani 1 1 d . . . C15 C 0.8225(3) 0.3796(2) 0.5137(2) 0.0830(8) Uani 1 1 d . . . H15 H 0.7900 0.4030 0.5682 0.100 Uiso 1 1 calc R . . C16 C 0.9162(3) 0.4100(3) 0.4499(3) 0.1009(11) Uani 1 1 d . . . H16 H 0.9456 0.4544 0.4609 0.121 Uiso 1 1 calc R . . C17 C 0.9663(3) 0.3751(3) 0.3699(3) 0.0980(10) Uani 1 1 d . . . H17 H 1.0299 0.3961 0.3275 0.118 Uiso 1 1 calc R . . C18 C 0.9243(2) 0.3090(2) 0.3505(2) 0.0733(7) Uani 1 1 d . . . C19 C 0.9877(2) 0.2640(3) 0.2673(2) 0.0933(10) Uani 1 1 d . . . H19 H 0.9445 0.2215 0.2640 0.112 Uiso 1 1 calc R . . C20 C 1.0907(3) 0.1975(3) 0.2912(3) 0.1167(13) Uani 1 1 d . . . H20A H 1.1319 0.2364 0.3000 0.175 Uiso 1 1 calc R . . H20B H 1.1315 0.1711 0.2374 0.175 Uiso 1 1 calc R . . H20C H 1.0733 0.1433 0.3511 0.175 Uiso 1 1 calc R . . C21 C 1.0136(4) 0.3424(4) 0.1663(3) 0.162(2) Uani 1 1 d . . . H21A H 0.9485 0.3785 0.1484 0.243 Uiso 1 1 calc R . . H21B H 1.0574 0.3101 0.1176 0.243 Uiso 1 1 calc R . . H21C H 1.0513 0.3880 0.1691 0.243 Uiso 1 1 calc R . . C22 C 0.67534(19) 0.27558(19) 0.57176(17) 0.0599(6) Uani 1 1 d . . . H22 H 0.6338 0.2678 0.5332 0.072 Uiso 1 1 calc R . . C23 C 0.7057(2) 0.1714(2) 0.6418(2) 0.0847(8) Uani 1 1 d . . . H23A H 0.7484 0.1276 0.6035 0.127 Uiso 1 1 calc R . . H23B H 0.6419 0.1451 0.6842 0.127 Uiso 1 1 calc R . . H23C H 0.7457 0.1762 0.6817 0.127 Uiso 1 1 calc R . . C24 C 0.6029(3) 0.3451(3) 0.6308(3) 0.1039(11) Uani 1 1 d . . . H24A H 0.6382 0.3489 0.6750 0.156 Uiso 1 1 calc R . . H24B H 0.5376 0.3196 0.6687 0.156 Uiso 1 1 calc R . . H24C H 0.5871 0.4107 0.5860 0.156 Uiso 1 1 calc R . . C25 C 0.61633(17) 0.09128(15) 0.46091(13) 0.0459(5) Uani 1 1 d . . . H25A H 0.6045 0.1383 0.4967 0.055 Uiso 1 1 calc R . . H25B H 0.5471 0.0792 0.4657 0.055 Uiso 1 1 calc R . . C26 C 0.6798(2) -0.00525(19) 0.50940(18) 0.0741(7) Uani 1 1 d . . . H26A H 0.6907 -0.0527 0.4752 0.111 Uiso 1 1 calc R . . H26B H 0.6415 -0.0314 0.5775 0.111 Uiso 1 1 calc R . . H26C H 0.7477 0.0065 0.5066 0.111 Uiso 1 1 calc R . . C27 C 0.63930(18) 0.18915(16) 0.09067(14) 0.0494(5) Uani 1 1 d . . . C28 C 0.7323(2) 0.20151(18) 0.01382(16) 0.0612(6) Uani 1 1 d . . . C29 C 0.7265(3) 0.1966(2) -0.07630(19) 0.0844(9) Uani 1 1 d . . . H29 H 0.7865 0.2031 -0.1303 0.101 Uiso 1 1 calc R . . C30 C 0.6350(3) 0.1827(3) -0.0861(2) 0.0926(10) Uani 1 1 d . . . H30 H 0.6347 0.1771 -0.1457 0.111 Uiso 1 1 calc R . . C31 C 0.5444(3) 0.1769(2) -0.0109(2) 0.0851(9) Uani 1 1 d . . . H31 H 0.4825 0.1697 -0.0205 0.102 Uiso 1 1 calc R . . C32 C 0.5426(2) 0.18144(19) 0.08045(17) 0.0610(6) Uani 1 1 d . . . C33 C 0.4378(2) 0.1850(2) 0.16020(19) 0.0721(7) Uani 1 1 d . . . H33 H 0.4540 0.1854 0.2190 0.086 Uiso 1 1 calc R . . C34 C 0.3838(3) 0.0954(3) 0.1912(3) 0.1081(11) Uani 1 1 d . . . H34A H 0.3695 0.0911 0.1345 0.162 Uiso 1 1 calc R . . H34B H 0.3178 0.1027 0.2408 0.162 Uiso 1 1 calc R . . H34C H 0.4298 0.0355 0.2179 0.162 Uiso 1 1 calc R . . C35 C 0.3634(3) 0.2836(3) 0.1259(3) 0.1036(11) Uani 1 1 d . . . H35A H 0.4012 0.3386 0.1031 0.155 Uiso 1 1 calc R . . H35B H 0.3027 0.2913 0.1804 0.155 Uiso 1 1 calc R . . H35C H 0.3396 0.2826 0.0727 0.155 Uiso 1 1 calc R . . C36 C 0.8296(2) 0.2246(2) 0.0238(2) 0.0803(8) Uani 1 1 d . . . H36 H 0.8219 0.2088 0.0949 0.096 Uiso 1 1 calc R . . C37 C 0.8320(4) 0.3369(3) -0.0234(5) 0.181(3) Uani 1 1 d . . . H37A H 0.8388 0.3552 -0.0933 0.272 Uiso 1 1 calc R . . H37B H 0.8918 0.3523 -0.0136 0.272 Uiso 1 1 calc R . . H37C H 0.7670 0.3736 0.0070 0.272 Uiso 1 1 calc R . . C38 C 0.9331(3) 0.1608(4) -0.0171(3) 0.155(2) Uani 1 1 d . . . H38A H 0.9268 0.0913 0.0131 0.232 Uiso 1 1 calc R . . H38B H 0.9916 0.1730 -0.0024 0.232 Uiso 1 1 calc R . . H38C H 0.9459 0.1780 -0.0877 0.232 Uiso 1 1 calc R . . C39 C 0.81012(16) -0.06734(15) 0.24739(15) 0.0470(5) Uani 1 1 d . . . C40 C 0.77411(18) -0.12613(16) 0.21371(17) 0.0544(5) Uani 1 1 d . . . C41 C 0.8157(2) -0.22846(18) 0.2398(2) 0.0722(7) Uani 1 1 d . . . H41 H 0.7927 -0.2701 0.2193 0.087 Uiso 1 1 calc R . . C42 C 0.8887(2) -0.2690(2) 0.2942(2) 0.0824(8) Uani 1 1 d . . . H42 H 0.9136 -0.3376 0.3117 0.099 Uiso 1 1 calc R . . C43 C 0.9254(2) -0.2087(2) 0.3231(2) 0.0782(8) Uani 1 1 d . . . H43 H 0.9762 -0.2372 0.3594 0.094 Uiso 1 1 calc R . . C44 C 0.88872(18) -0.10514(18) 0.29945(17) 0.0583(6) Uani 1 1 d . . . C45 C 0.9400(2) -0.0370(2) 0.3190(2) 0.0724(7) Uani 1 1 d . . . H45 H 0.8873 0.0234 0.3242 0.087 Uiso 1 1 calc R . . C46 C 0.9750(3) -0.0843(3) 0.4163(3) 0.1150(13) Uani 1 1 d . . . H46A H 0.9166 -0.1103 0.4697 0.173 Uiso 1 1 calc R . . H46B H 0.9961 -0.0343 0.4304 0.173 Uiso 1 1 calc R . . H46C H 1.0343 -0.1377 0.4094 0.173 Uiso 1 1 calc R . . C47 C 1.0345(3) -0.0053(3) 0.2296(3) 0.1077(11) Uani 1 1 d . . . H47A H 1.0868 -0.0634 0.2221 0.162 Uiso 1 1 calc R . . H47B H 1.0661 0.0402 0.2401 0.162 Uiso 1 1 calc R . . H47C H 1.0097 0.0271 0.1706 0.162 Uiso 1 1 calc R . . C48 C 0.69770(19) -0.08530(19) 0.14782(19) 0.0616(6) Uani 1 1 d . . . H48 H 0.6723 -0.0143 0.1425 0.074 Uiso 1 1 calc R . . C49 C 0.6002(2) -0.1373(2) 0.1928(3) 0.0928(10) Uani 1 1 d . . . H49A H 0.6224 -0.2070 0.1978 0.139 Uiso 1 1 calc R . . H49B H 0.5518 -0.1070 0.1513 0.139 Uiso 1 1 calc R . . H49C H 0.5650 -0.1307 0.2578 0.139 Uiso 1 1 calc R . . C50 C 0.7545(3) -0.0916(3) 0.0432(2) 0.0969(10) Uani 1 1 d . . . H50A H 0.8120 -0.0538 0.0147 0.145 Uiso 1 1 calc R . . H50B H 0.7048 -0.0647 0.0029 0.145 Uiso 1 1 calc R . . H50C H 0.7826 -0.1603 0.0462 0.145 Uiso 1 1 calc R . . 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 0.0405(3) 0.0450(3) 0.0349(3) -0.0121(2) -0.0072(2) -0.0101(2) P2 0.0373(3) 0.0420(3) 0.0355(3) -0.0132(2) -0.0096(2) -0.0047(2) O2 0.0433(8) 0.0565(9) 0.0457(8) -0.0186(7) -0.0137(6) -0.0088(6) O1 0.0511(8) 0.0418(7) 0.0427(7) -0.0111(6) -0.0148(6) -0.0039(6) O3 0.0478(8) 0.0476(8) 0.0356(7) -0.0130(6) -0.0135(6) -0.0029(6) O4 0.0413(7) 0.0423(7) 0.0456(7) -0.0164(6) -0.0088(6) -0.0031(6) O5 0.0466(8) 0.0544(8) 0.0497(8) -0.0180(7) -0.0089(6) -0.0139(7) N1 0.0435(9) 0.0412(9) 0.0315(8) -0.0100(7) -0.0081(7) -0.0089(7) C1 0.0603(13) 0.0379(10) 0.0462(11) -0.0124(9) -0.0202(10) -0.0029(9) C2 0.0572(13) 0.0456(12) 0.0638(14) -0.0173(11) -0.0235(11) -0.0022(10) C3 0.0719(17) 0.0610(16) 0.096(2) -0.0180(15) -0.0433(15) -0.0029(13) C4 0.104(2) 0.0634(17) 0.089(2) -0.0017(15) -0.0575(19) -0.0022(16) C5 0.099(2) 0.0548(15) 0.0659(16) 0.0015(12) -0.0318(15) -0.0144(14) C6 0.0740(16) 0.0459(12) 0.0547(13) -0.0112(10) -0.0201(12) -0.0093(11) C7 0.0732(17) 0.0485(14) 0.0811(18) -0.0016(13) -0.0176(14) -0.0188(12) C8 0.113(3) 0.095(2) 0.101(3) 0.010(2) -0.009(2) -0.047(2) C9 0.103(2) 0.0724(19) 0.120(3) -0.0272(18) -0.048(2) -0.0247(17) C10 0.0487(13) 0.0564(14) 0.0796(17) -0.0144(13) -0.0145(12) -0.0015(11) C11 0.0688(19) 0.095(2) 0.124(3) -0.027(2) -0.0179(18) -0.0265(17) C12 0.080(2) 0.126(3) 0.0726(19) -0.0168(19) -0.0101(16) -0.0241(19) C13 0.0491(12) 0.0643(14) 0.0546(12) -0.0179(11) -0.0196(10) -0.0143(10) C14 0.0625(14) 0.0652(14) 0.0610(14) -0.0250(12) -0.0262(12) -0.0097(11) C15 0.098(2) 0.089(2) 0.089(2) -0.0374(17) -0.0373(18) -0.0252(17) C16 0.106(3) 0.107(3) 0.126(3) -0.044(2) -0.042(2) -0.047(2) C17 0.080(2) 0.125(3) 0.106(2) -0.028(2) -0.0231(18) -0.055(2) C18 0.0547(14) 0.102(2) 0.0722(16) -0.0254(15) -0.0166(13) -0.0285(14) C19 0.0519(15) 0.158(3) 0.080(2) -0.048(2) 0.0014(14) -0.0406(18) C20 0.076(2) 0.150(4) 0.133(3) -0.063(3) -0.014(2) -0.023(2) C21 0.116(3) 0.227(6) 0.080(3) -0.019(3) 0.002(2) -0.004(3) C22 0.0595(14) 0.0767(16) 0.0516(13) -0.0305(12) -0.0150(11) -0.0082(12) C23 0.0790(19) 0.104(2) 0.0594(16) -0.0157(16) -0.0148(14) -0.0141(17) C24 0.098(2) 0.117(3) 0.107(3) -0.071(2) -0.004(2) -0.009(2) C25 0.0526(12) 0.0480(11) 0.0320(9) -0.0104(8) -0.0038(8) -0.0121(9) C26 0.0863(19) 0.0663(16) 0.0456(13) 0.0009(12) -0.0141(13) -0.0047(14) C27 0.0614(13) 0.0485(12) 0.0344(10) -0.0103(9) -0.0165(9) -0.0014(10) C28 0.0660(15) 0.0593(14) 0.0416(12) -0.0097(10) -0.0053(11) -0.0034(11) C29 0.096(2) 0.091(2) 0.0425(13) -0.0186(13) -0.0010(14) -0.0033(17) C30 0.121(3) 0.113(3) 0.0502(16) -0.0296(16) -0.0329(18) -0.009(2) C31 0.101(2) 0.108(2) 0.0580(16) -0.0230(16) -0.0374(16) -0.0175(18) C32 0.0715(15) 0.0679(15) 0.0467(12) -0.0114(11) -0.0303(11) -0.0068(12) C33 0.0578(14) 0.103(2) 0.0559(14) -0.0095(14) -0.0282(12) -0.0184(14) C34 0.086(2) 0.108(3) 0.112(3) -0.012(2) -0.020(2) -0.027(2) C35 0.087(2) 0.107(3) 0.094(2) -0.021(2) -0.0208(18) 0.0038(19) C36 0.0636(16) 0.092(2) 0.0596(15) -0.0070(14) 0.0024(13) -0.0196(15) C37 0.185(5) 0.118(4) 0.237(6) 0.032(4) -0.104(5) -0.081(4) C38 0.069(2) 0.245(6) 0.127(3) -0.081(4) 0.003(2) 0.007(3) C39 0.0423(11) 0.0463(11) 0.0449(11) -0.0146(9) -0.0062(9) -0.0013(9) C40 0.0513(12) 0.0468(12) 0.0605(13) -0.0204(10) -0.0064(10) -0.0062(10) C41 0.0727(17) 0.0482(14) 0.0891(19) -0.0231(13) -0.0113(15) -0.0096(12) C42 0.088(2) 0.0473(14) 0.096(2) -0.0126(14) -0.0257(17) 0.0020(14) C43 0.0683(17) 0.0736(18) 0.0723(17) -0.0114(14) -0.0268(14) 0.0149(14) C44 0.0519(13) 0.0654(15) 0.0512(12) -0.0201(11) -0.0147(10) 0.0049(11) C45 0.0586(15) 0.0933(19) 0.0759(17) -0.0444(15) -0.0291(13) 0.0108(13) C46 0.096(2) 0.164(4) 0.107(3) -0.063(3) -0.065(2) 0.022(2) C47 0.093(2) 0.136(3) 0.116(3) -0.062(2) -0.011(2) -0.042(2) C48 0.0616(14) 0.0581(14) 0.0779(16) -0.0338(12) -0.0229(12) -0.0061(11) C49 0.0716(19) 0.094(2) 0.132(3) -0.050(2) -0.0258(18) -0.0225(16) C50 0.100(2) 0.118(3) 0.080(2) -0.0450(19) -0.0280(18) -0.005(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 O2 1.6415(16) . ? P1 O1 1.6534(15) . ? P1 N1 1.7062(18) . ? P2 O5 1.4577(15) . ? P2 O3 1.5891(15) . ? P2 O4 1.5979(15) . ? P2 N1 1.6614(17) . ? O2 C13 1.414(3) . ? O1 C1 1.418(2) . ? O3 C27 1.423(2) . ? O4 C39 1.424(2) . ? N1 C25 1.510(2) . ? C1 C2 1.395(3) . ? C1 C6 1.401(3) . ? C2 C3 1.397(3) . ? C2 C10 1.521(3) . ? C3 C4 1.375(4) . ? C4 C5 1.368(4) . ? C5 C6 1.393(4) . ? C6 C7 1.516(4) . ? C7 C8 1.532(4) . ? C7 C9 1.542(4) . ? C10 C11 1.524(4) . ? C10 C12 1.528(4) . ? C13 C14 1.398(3) . ? C13 C18 1.400(3) . ? C14 C15 1.399(3) . ? C14 C22 1.512(3) . ? C15 C16 1.374(4) . ? C16 C17 1.372(5) . ? C17 C18 1.396(4) . ? C18 C19 1.520(4) . ? C19 C21 1.519(5) . ? C19 C20 1.528(5) . ? C22 C24 1.523(4) . ? C22 C23 1.533(4) . ? C25 C26 1.499(3) . ? C27 C28 1.391(3) . ? C27 C32 1.399(3) . ? C28 C29 1.410(4) . ? C28 C36 1.504(4) . ? C29 C30 1.364(5) . ? C30 C31 1.355(4) . ? C31 C32 1.390(3) . ? C32 C33 1.518(4) . ? C33 C34 1.514(4) . ? C33 C35 1.534(4) . ? C36 C38 1.528(5) . ? C36 C37 1.529(5) . ? C39 C40 1.391(3) . ? C39 C44 1.397(3) . ? C40 C41 1.398(3) . ? C40 C48 1.518(3) . ? C41 C42 1.358(4) . ? C42 C43 1.366(4) . ? C43 C44 1.403(4) . ? C44 C45 1.509(4) . ? C45 C47 1.534(4) . ? C45 C46 1.539(4) . ? C48 C49 1.524(4) . ? C48 C50 1.526(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 P1 O1 96.20(8) . . ? O2 P1 N1 96.03(8) . . ? O1 P1 N1 103.17(8) . . ? O5 P2 O3 118.48(8) . . ? O5 P2 O4 113.54(9) . . ? O3 P2 O4 100.43(8) . . ? O5 P2 N1 112.60(8) . . ? O3 P2 N1 100.06(9) . . ? O4 P2 N1 110.39(8) . . ? C13 O2 P1 121.73(13) . . ? C1 O1 P1 120.02(12) . . ? C27 O3 P2 122.63(13) . . ? C39 O4 P2 124.32(12) . . ? C25 N1 P2 116.27(13) . . ? C25 N1 P1 122.18(12) . . ? P2 N1 P1 120.81(9) . . ? C2 C1 C6 123.5(2) . . ? C2 C1 O1 117.43(18) . . ? C6 C1 O1 119.0(2) . . ? C1 C2 C3 116.5(2) . . ? C1 C2 C10 121.6(2) . . ? C3 C2 C10 121.7(2) . . ? C4 C3 C2 121.4(3) . . ? C5 C4 C3 120.2(3) . . ? C4 C5 C6 121.8(3) . . ? C5 C6 C1 116.4(2) . . ? C5 C6 C7 121.9(2) . . ? C1 C6 C7 121.4(2) . . ? C6 C7 C8 114.7(3) . . ? C6 C7 C9 109.7(2) . . ? C8 C7 C9 109.8(3) . . ? C2 C10 C11 114.8(2) . . ? C2 C10 C12 110.3(2) . . ? C11 C10 C12 109.5(2) . . ? C14 C13 C18 123.3(2) . . ? C14 C13 O2 116.59(19) . . ? C18 C13 O2 120.0(2) . . ? C13 C14 C15 116.6(2) . . ? C13 C14 C22 121.4(2) . . ? C15 C14 C22 121.9(2) . . ? C16 C15 C14 121.6(3) . . ? C17 C16 C15 120.1(3) . . ? C16 C17 C18 121.7(3) . . ? C17 C18 C13 116.7(3) . . ? C17 C18 C19 120.0(3) . . ? C13 C18 C19 123.2(2) . . ? C21 C19 C18 113.1(3) . . ? C21 C19 C20 110.0(3) . . ? C18 C19 C20 109.8(3) . . ? C14 C22 C24 114.7(2) . . ? C14 C22 C23 110.0(2) . . ? C24 C22 C23 110.5(2) . . ? C26 C25 N1 113.10(18) . . ? C28 C27 C32 124.4(2) . . ? C28 C27 O3 117.7(2) . . ? C32 C27 O3 117.73(19) . . ? C27 C28 C29 115.0(2) . . ? C27 C28 C36 122.7(2) . . ? C29 C28 C36 122.2(2) . . ? C30 C29 C28 121.4(3) . . ? C31 C30 C29 121.5(3) . . ? C30 C31 C32 120.9(3) . . ? C31 C32 C27 116.4(2) . . ? C31 C32 C33 120.0(2) . . ? C27 C32 C33 123.4(2) . . ? C34 C33 C32 113.7(3) . . ? C34 C33 C35 111.5(3) . . ? C32 C33 C35 109.5(2) . . ? C28 C36 C38 112.8(3) . . ? C28 C36 C37 109.4(3) . . ? C38 C36 C37 112.6(3) . . ? C40 C39 C44 123.0(2) . . ? C40 C39 O4 119.62(18) . . ? C44 C39 O4 117.13(19) . . ? C39 C40 C41 116.6(2) . . ? C39 C40 C48 124.2(2) . . ? C41 C40 C48 119.2(2) . . ? C42 C41 C40 122.2(3) . . ? C41 C42 C43 119.8(3) . . ? C42 C43 C44 121.8(3) . . ? C39 C44 C43 116.4(2) . . ? C39 C44 C45 121.7(2) . . ? C43 C44 C45 121.6(2) . . ? C44 C45 C47 108.7(2) . . ? C44 C45 C46 113.2(3) . . ? C47 C45 C46 111.3(3) . . ? C40 C48 C49 111.8(2) . . ? C40 C48 C50 111.1(2) . . ? C49 C48 C50 111.2(2) . . ? 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 O1 P1 O2 C13 -66.95(16) . . . . ? N1 P1 O2 C13 -170.96(15) . . . . ? O2 P1 O1 C1 162.49(14) . . . . ? N1 P1 O1 C1 -99.82(15) . . . . ? O5 P2 O3 C27 -65.08(17) . . . . ? O4 P2 O3 C27 59.10(16) . . . . ? N1 P2 O3 C27 172.21(15) . . . . ? O5 P2 O4 C39 -25.34(17) . . . . ? O3 P2 O4 C39 -152.86(15) . . . . ? N1 P2 O4 C39 102.19(16) . . . . ? O5 P2 N1 C25 12.79(16) . . . . ? O3 P2 N1 C25 139.56(13) . . . . ? O4 P2 N1 C25 -115.25(14) . . . . ? O5 P2 N1 P1 -157.56(10) . . . . ? O3 P2 N1 P1 -30.80(12) . . . . ? O4 P2 N1 P1 74.40(12) . . . . ? O2 P1 N1 C25 44.42(15) . . . . ? O1 P1 N1 C25 -53.41(16) . . . . ? O2 P1 N1 P2 -145.81(10) . . . . ? O1 P1 N1 P2 116.36(10) . . . . ? P1 O1 C1 C2 113.67(19) . . . . ? P1 O1 C1 C6 -70.7(2) . . . . ? C6 C1 C2 C3 4.9(3) . . . . ? O1 C1 C2 C3 -179.7(2) . . . . ? C6 C1 C2 C10 -171.0(2) . . . . ? O1 C1 C2 C10 4.4(3) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? C10 C2 C3 C4 175.2(3) . . . . ? C2 C3 C4 C5 -2.8(5) . . . . ? C3 C4 C5 C6 2.5(5) . . . . ? C4 C5 C6 C1 1.4(4) . . . . ? C4 C5 C6 C7 -171.9(3) . . . . ? C2 C1 C6 C5 -5.2(3) . . . . ? O1 C1 C6 C5 179.4(2) . . . . ? C2 C1 C6 C7 168.1(2) . . . . ? O1 C1 C6 C7 -7.2(3) . . . . ? C5 C6 C7 C8 -23.4(4) . . . . ? C1 C6 C7 C8 163.6(3) . . . . ? C5 C6 C7 C9 100.7(3) . . . . ? C1 C6 C7 C9 -72.3(3) . . . . ? C1 C2 C10 C11 -166.5(2) . . . . ? C3 C2 C10 C11 17.7(4) . . . . ? C1 C2 C10 C12 69.2(3) . . . . ? C3 C2 C10 C12 -106.5(3) . . . . ? P1 O2 C13 C14 109.7(2) . . . . ? P1 O2 C13 C18 -74.4(3) . . . . ? C18 C13 C14 C15 2.0(4) . . . . ? O2 C13 C14 C15 177.8(2) . . . . ? C18 C13 C14 C22 -174.5(2) . . . . ? O2 C13 C14 C22 1.3(3) . . . . ? C13 C14 C15 C16 -0.2(4) . . . . ? C22 C14 C15 C16 176.4(3) . . . . ? C14 C15 C16 C17 -1.0(5) . . . . ? C15 C16 C17 C18 0.4(6) . . . . ? C16 C17 C18 C13 1.4(5) . . . . ? C16 C17 C18 C19 -173.9(3) . . . . ? C14 C13 C18 C17 -2.6(4) . . . . ? O2 C13 C18 C17 -178.2(2) . . . . ? C14 C13 C18 C19 172.5(3) . . . . ? O2 C13 C18 C19 -3.2(4) . . . . ? C17 C18 C19 C21 -59.1(4) . . . . ? C13 C18 C19 C21 126.0(3) . . . . ? C17 C18 C19 C20 64.3(4) . . . . ? C13 C18 C19 C20 -110.6(3) . . . . ? C13 C14 C22 C24 -155.6(3) . . . . ? C15 C14 C22 C24 28.0(4) . . . . ? C13 C14 C22 C23 79.0(3) . . . . ? C15 C14 C22 C23 -97.3(3) . . . . ? P2 N1 C25 C26 79.9(2) . . . . ? P1 N1 C25 C26 -109.9(2) . . . . ? P2 O3 C27 C28 -98.4(2) . . . . ? P2 O3 C27 C32 84.9(2) . . . . ? C32 C27 C28 C29 -5.7(4) . . . . ? O3 C27 C28 C29 177.9(2) . . . . ? C32 C27 C28 C36 170.7(2) . . . . ? O3 C27 C28 C36 -5.7(3) . . . . ? C27 C28 C29 C30 1.2(4) . . . . ? C36 C28 C29 C30 -175.2(3) . . . . ? C28 C29 C30 C31 2.6(5) . . . . ? C29 C30 C31 C32 -2.2(5) . . . . ? C30 C31 C32 C27 -1.9(4) . . . . ? C30 C31 C32 C33 174.0(3) . . . . ? C28 C27 C32 C31 6.1(4) . . . . ? O3 C27 C32 C31 -177.4(2) . . . . ? C28 C27 C32 C33 -169.7(2) . . . . ? O3 C27 C32 C33 6.8(3) . . . . ? C31 C32 C33 C34 59.5(3) . . . . ? C27 C32 C33 C34 -124.9(3) . . . . ? C31 C32 C33 C35 -66.0(4) . . . . ? C27 C32 C33 C35 109.6(3) . . . . ? C27 C28 C36 C38 134.6(3) . . . . ? C29 C28 C36 C38 -49.3(4) . . . . ? C27 C28 C36 C37 -99.3(4) . . . . ? C29 C28 C36 C37 76.9(4) . . . . ? P2 O4 C39 C40 78.1(2) . . . . ? P2 O4 C39 C44 -107.27(19) . . . . ? C44 C39 C40 C41 3.9(3) . . . . ? O4 C39 C40 C41 178.18(19) . . . . ? C44 C39 C40 C48 -173.3(2) . . . . ? O4 C39 C40 C48 1.0(3) . . . . ? C39 C40 C41 C42 -0.8(4) . . . . ? C48 C40 C41 C42 176.5(2) . . . . ? C40 C41 C42 C43 -1.5(4) . . . . ? C41 C42 C43 C44 1.0(5) . . . . ? C40 C39 C44 C43 -4.4(3) . . . . ? O4 C39 C44 C43 -178.8(2) . . . . ? C40 C39 C44 C45 168.9(2) . . . . ? O4 C39 C44 C45 -5.5(3) . . . . ? C42 C43 C44 C39 1.9(4) . . . . ? C42 C43 C44 C45 -171.5(3) . . . . ? C39 C44 C45 C47 -86.3(3) . . . . ? C43 C44 C45 C47 86.7(3) . . . . ? C39 C44 C45 C46 149.5(2) . . . . ? C43 C44 C45 C46 -37.5(3) . . . . ? C39 C40 C48 C49 -125.5(3) . . . . ? C41 C40 C48 C49 57.3(3) . . . . ? C39 C40 C48 C50 109.5(3) . . . . ? C41 C40 C48 C50 -67.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 28.10 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.530 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.044 ### END