# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ms12 _database_code_depnum_ccdc_archive 'CCDC 848667' #TrackingRef '203MS12(SB-SD-4)-RRR.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H57 Cl N5 O3 P3 Pd Ru' _chemical_formula_weight 1316.01 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' Ru Ru -1.2594 0.8363 '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 10.2779(2) _cell_length_b 13.7689(2) _cell_length_c 22.0341(3) _cell_angle_alpha 99.3150(10) _cell_angle_beta 103.3020(10) _cell_angle_gamma 100.3930(10) _cell_volume 2916.58(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340.0 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.869 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44521 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 40.60 _reflns_number_total 28857 _reflns_number_gt 21050 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28857 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1404 _refine_ls_wR_factor_gt 0.1180 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.877 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.406466(15) 0.095756(10) 0.836848(6) 0.01369(3) Uani 1 d . . . Pd Pd 0.270611(15) 0.253612(10) 0.656711(6) 0.01607(3) Uani 1 d . . . P1 P 0.34332(6) 0.35021(4) 0.59170(2) 0.01785(9) Uani 1 d . . . P2 P 0.38513(5) -0.06508(4) 0.77176(2) 0.01691(8) Uani 1 d . . . P3 P 0.43958(5) 0.25592(4) 0.90561(2) 0.01538(8) Uani 1 d . . . O1 O 0.07576(16) 0.25192(13) 0.61459(8) 0.0253(3) Uani 1 d . . . O2 O 0.55105(14) 0.16712(11) 0.78595(7) 0.0188(2) Uani 1 d . . . O3 O 0.15961(18) 0.01349(13) 0.87703(10) 0.0325(4) Uani 1 d . . . N1 N 0.21760(17) 0.16925(12) 0.71774(7) 0.0154(3) Uani 1 d . . . N2 N 0.32812(17) 0.15050(12) 0.75759(7) 0.0169(3) Uani 1 d . . . N3 N 0.45511(18) 0.23949(14) 0.70145(8) 0.0204(3) Uani 1 d . . . H3A H 0.5296 0.2639 0.6923 0.024 Uiso 1 calc R . . Cl Cl 0.56585(5) 0.05265(4) 0.92061(2) 0.02104(8) Uani 1 d . . . C1 C -0.0306(2) 0.20676(15) 0.63097(9) 0.0203(3) Uani 1 d . . . C2 C -0.1621(2) 0.21041(18) 0.59420(11) 0.0267(4) Uani 1 d . . . H2 H -0.1676 0.2417 0.5596 0.032 Uiso 1 calc R . . C3 C -0.2813(2) 0.16946(18) 0.60787(11) 0.0269(4) Uani 1 d . . . H3 H -0.3652 0.1742 0.5828 0.032 Uiso 1 calc R . . C4 C -0.2782(2) 0.12090(17) 0.65876(11) 0.0239(4) Uani 1 d . . . H4 H -0.3589 0.0937 0.6683 0.029 Uiso 1 calc R . . C5 C -0.1522(2) 0.11411(16) 0.69471(10) 0.0222(4) Uani 1 d . . . H5 H -0.1495 0.0814 0.7286 0.027 Uiso 1 calc R . . C6 C -0.0274(2) 0.15473(14) 0.68207(9) 0.0183(3) Uani 1 d . . . C7 C 0.0957(2) 0.13982(14) 0.72353(9) 0.0176(3) Uani 1 d . . . H7 H 0.0860 0.1069 0.7564 0.021 Uiso 1 calc R . . C8 C 0.4500(2) 0.18803(14) 0.74698(9) 0.0174(3) Uani 1 d . . . C9 C 0.2564(2) 0.04578(14) 0.86270(9) 0.0197(3) Uani 1 d . . . C111 C 0.2949(2) 0.27839(15) 0.51023(9) 0.0205(3) Uani 1 d . . . C112 C 0.2964(3) 0.17538(16) 0.50127(11) 0.0280(4) Uani 1 d . . . H112 H 0.3131 0.1452 0.5363 0.034 Uiso 1 calc R . . C113 C 0.2730(3) 0.11893(19) 0.44052(12) 0.0374(6) Uani 1 d . . . H113 H 0.2747 0.0508 0.4347 0.045 Uiso 1 calc R . . C114 C 0.2467(3) 0.1633(2) 0.38769(12) 0.0403(6) Uani 1 d . . . H114 H 0.2318 0.1250 0.3468 0.048 Uiso 1 calc R . . C115 C 0.2430(3) 0.2637(2) 0.39629(11) 0.0400(6) Uani 1 d . . . H115 H 0.2241 0.2931 0.3610 0.048 Uiso 1 calc R . . C116 C 0.2671(3) 0.32196(18) 0.45727(10) 0.0305(5) Uani 1 d . . . H116 H 0.2647 0.3899 0.4626 0.037 Uiso 1 calc R . . C121 C 0.5283(2) 0.39406(15) 0.60970(9) 0.0205(3) Uani 1 d . . . C122 C 0.5987(2) 0.38507(17) 0.56274(11) 0.0255(4) Uani 1 d . . . H122 H 0.5518 0.3512 0.5212 0.031 Uiso 1 calc R . . C123 C 0.7386(3) 0.42652(19) 0.57784(13) 0.0312(5) Uani 1 d . . . H123 H 0.7856 0.4194 0.5466 0.037 Uiso 1 calc R . . C124 C 0.8074(3) 0.4778(2) 0.63863(13) 0.0337(5) Uani 1 d . . . H124 H 0.9013 0.5050 0.6487 0.040 Uiso 1 calc R . . C125 C 0.7376(3) 0.4893(2) 0.68536(12) 0.0332(5) Uani 1 d . . . H125 H 0.7843 0.5263 0.7262 0.040 Uiso 1 calc R . . C126 C 0.5994(2) 0.44608(17) 0.67154(10) 0.0266(4) Uani 1 d . . . H126 H 0.5539 0.4516 0.7034 0.032 Uiso 1 calc R . . C131 C 0.2856(2) 0.46771(16) 0.58869(10) 0.0227(4) Uani 1 d . . . C132 C 0.3780(3) 0.55923(16) 0.59563(12) 0.0291(4) Uani 1 d . . . H132 H 0.4710 0.5609 0.6016 0.035 Uiso 1 calc R . . C133 C 0.3318(3) 0.64778(18) 0.59361(13) 0.0355(5) Uani 1 d . . . H133 H 0.3945 0.7084 0.5990 0.043 Uiso 1 calc R . . C134 C 0.1939(3) 0.6467(2) 0.58375(13) 0.0362(6) Uani 1 d . . . H134 H 0.1631 0.7059 0.5818 0.043 Uiso 1 calc R . . C135 C 0.1017(3) 0.5556(2) 0.57674(16) 0.0419(7) Uani 1 d . . . H135 H 0.0085 0.5541 0.5699 0.050 Uiso 1 calc R . . C136 C 0.1470(3) 0.4665(2) 0.57982(14) 0.0338(5) Uani 1 d . . . H136 H 0.0846 0.4064 0.5759 0.041 Uiso 1 calc R . . C211 C 0.2744(2) -0.16656(14) 0.79215(10) 0.0211(3) Uani 1 d . . . C212 C 0.2992(3) -0.16919(17) 0.85715(11) 0.0273(4) Uani 1 d . . . H212 H 0.3716 -0.1224 0.8869 0.033 Uiso 1 calc R . . C213 C 0.2159(3) -0.24135(19) 0.87704(14) 0.0351(5) Uani 1 d . . . H213 H 0.2328 -0.2427 0.9202 0.042 Uiso 1 calc R . . C214 C 0.1079(3) -0.3114(2) 0.83329(15) 0.0371(6) Uani 1 d . . . H214 H 0.0513 -0.3590 0.8469 0.045 Uiso 1 calc R . . C215 C 0.0846(3) -0.31001(19) 0.76902(15) 0.0364(5) Uani 1 d . . . H215 H 0.0127 -0.3575 0.7394 0.044 Uiso 1 calc R . . C216 C 0.1674(3) -0.23861(17) 0.74834(12) 0.0290(4) Uani 1 d . . . H216 H 0.1513 -0.2389 0.7050 0.035 Uiso 1 calc R . . C221 C 0.5411(2) -0.11261(15) 0.77399(9) 0.0198(3) Uani 1 d . . . C222 C 0.5319(3) -0.21632(16) 0.75703(11) 0.0265(4) Uani 1 d . . . H222 H 0.4466 -0.2611 0.7448 0.032 Uiso 1 calc R . . C223 C 0.6497(3) -0.25276(19) 0.75832(12) 0.0324(5) Uani 1 d . . . H223 H 0.6429 -0.3218 0.7464 0.039 Uiso 1 calc R . . C224 C 0.7770(3) -0.1866(2) 0.77730(11) 0.0314(5) Uani 1 d . . . H224 H 0.8560 -0.2112 0.7787 0.038 Uiso 1 calc R . . C225 C 0.7866(2) -0.08401(19) 0.79410(11) 0.0276(4) Uani 1 d . . . H225 H 0.8724 -0.0397 0.8068 0.033 Uiso 1 calc R . . C226 C 0.6692(2) -0.04621(16) 0.79228(10) 0.0221(4) Uani 1 d . . . H226 H 0.6764 0.0231 0.8032 0.027 Uiso 1 calc R . . C231 C 0.3130(2) -0.07270(15) 0.68667(9) 0.0223(4) Uani 1 d . . . C232 C 0.1764(3) -0.06677(18) 0.66462(11) 0.0299(5) Uani 1 d . . . H232 H 0.1214 -0.0641 0.6927 0.036 Uiso 1 calc R . . C233 C 0.1223(3) -0.0649(2) 0.60099(12) 0.0387(6) Uani 1 d . . . H233 H 0.0310 -0.0617 0.5867 0.046 Uiso 1 calc R . . C234 C 0.2031(4) -0.0678(2) 0.55904(12) 0.0418(7) Uani 1 d . . . H234 H 0.1665 -0.0664 0.5165 0.050 Uiso 1 calc R . . C235 C 0.3383(3) -0.0727(2) 0.58030(12) 0.0389(6) Uani 1 d . . . H235 H 0.3931 -0.0742 0.5521 0.047 Uiso 1 calc R . . C236 C 0.3935(3) -0.07545(17) 0.64385(10) 0.0281(4) Uani 1 d . . . H236 H 0.4847 -0.0791 0.6577 0.034 Uiso 1 calc R . . C311 C 0.6155(2) 0.31516(14) 0.95260(9) 0.0184(3) Uani 1 d . . . C312 C 0.6395(2) 0.38344(16) 1.01064(9) 0.0223(4) Uani 1 d . . . H312 H 0.5661 0.3960 1.0262 0.027 Uiso 1 calc R . . C313 C 0.7728(2) 0.43247(16) 1.04495(10) 0.0247(4) Uani 1 d . . . H313 H 0.7884 0.4773 1.0837 0.030 Uiso 1 calc R . . C314 C 0.8824(2) 0.41501(16) 1.02186(11) 0.0256(4) Uani 1 d . . . H314 H 0.9715 0.4486 1.0447 0.031 Uiso 1 calc R . . C315 C 0.8590(2) 0.34702(18) 0.96433(11) 0.0273(4) Uani 1 d . . . H315 H 0.9327 0.3353 0.9487 0.033 Uiso 1 calc R . . C316 C 0.7262(2) 0.29660(16) 0.93016(10) 0.0227(4) Uani 1 d . . . H316 H 0.7114 0.2503 0.8921 0.027 Uiso 1 calc R . . C321 C 0.3496(2) 0.25639(14) 0.96788(9) 0.0178(3) Uani 1 d . . . C322 C 0.2809(2) 0.33121(16) 0.98251(10) 0.0233(4) Uani 1 d . . . H322 H 0.2708 0.3785 0.9571 0.028 Uiso 1 calc R . . C323 C 0.2270(2) 0.33580(19) 1.03502(10) 0.0276(4) Uani 1 d . . . H323 H 0.1815 0.3864 1.0448 0.033 Uiso 1 calc R . . C324 C 0.2409(3) 0.2653(2) 1.07270(11) 0.0298(5) Uani 1 d . . . H324 H 0.2046 0.2685 1.1078 0.036 Uiso 1 calc R . . C325 C 0.3085(3) 0.18988(19) 1.05842(10) 0.0293(4) Uani 1 d . . . H325 H 0.3181 0.1429 1.0841 0.035 Uiso 1 calc R . . C326 C 0.3624(2) 0.18410(16) 1.00561(10) 0.0228(4) Uani 1 d . . . H326 H 0.4063 0.1327 0.9955 0.027 Uiso 1 calc R . . C331 C 0.3917(2) 0.35435(14) 0.86415(9) 0.0185(3) Uani 1 d . . . C332 C 0.2548(2) 0.34377(15) 0.83070(9) 0.0213(3) Uani 1 d . . . H332 H 0.1878 0.2899 0.8326 0.026 Uiso 1 calc R . . C333 C 0.2186(3) 0.41384(18) 0.79452(11) 0.0279(4) Uani 1 d . . . H333 H 0.1278 0.4057 0.7717 0.033 Uiso 1 calc R . . C334 C 0.3169(3) 0.49528(19) 0.79243(12) 0.0334(5) Uani 1 d . . . H334 H 0.2921 0.5423 0.7687 0.040 Uiso 1 calc R . . C335 C 0.4525(3) 0.50669(19) 0.82574(13) 0.0331(5) Uani 1 d . . . H335 H 0.5186 0.5615 0.8243 0.040 Uiso 1 calc R . . C336 C 0.4903(3) 0.43695(17) 0.86121(11) 0.0269(4) Uani 1 d . . . H336 H 0.5818 0.4450 0.8832 0.032 Uiso 1 calc R . . C101 C -0.0657(3) 0.0947(3) 0.95703(18) 0.0536(8) Uani 1 d . . . H10A H -0.0546 0.0263 0.9501 0.080 Uiso 1 calc R . . H10B H -0.1571 0.0951 0.9603 0.080 Uiso 1 calc R . . H10C H -0.0006 0.1332 0.9958 0.080 Uiso 1 calc R . . C102 C -0.0427(3) 0.1388(2) 0.90407(14) 0.0360(5) Uani 1 d . . . N103 N -0.0244(3) 0.1730(2) 0.86259(14) 0.0468(6) Uani 1 d . . . C201 C 0.8359(3) 0.3275(2) 0.78770(15) 0.0390(6) Uani 1 d . . . H20A H 0.7493 0.2823 0.7824 0.058 Uiso 1 calc R . . H20B H 0.9082 0.3033 0.8125 0.058 Uiso 1 calc R . . H20C H 0.8512 0.3307 0.7466 0.058 Uiso 1 calc R . . C202 C 0.8347(3) 0.4277(2) 0.82046(12) 0.0345(5) Uani 1 d . . . N203 N 0.8324(3) 0.5065(2) 0.84491(12) 0.0475(6) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01402(7) 0.01239(5) 0.01535(5) 0.00410(4) 0.00435(5) 0.00317(5) Pd 0.01767(7) 0.01609(6) 0.01674(5) 0.00683(4) 0.00677(5) 0.00379(5) P1 0.0215(2) 0.01623(19) 0.01850(18) 0.00677(16) 0.00859(17) 0.00414(18) P2 0.0180(2) 0.01326(18) 0.01920(19) 0.00306(15) 0.00499(17) 0.00327(17) P3 0.0169(2) 0.01339(17) 0.01645(17) 0.00352(14) 0.00510(16) 0.00395(17) O1 0.0202(7) 0.0314(8) 0.0281(7) 0.0173(6) 0.0056(6) 0.0067(6) O2 0.0161(6) 0.0211(6) 0.0204(6) 0.0070(5) 0.0058(5) 0.0039(5) O3 0.0271(9) 0.0272(8) 0.0497(10) 0.0122(7) 0.0207(8) 0.0053(7) N1 0.0171(7) 0.0152(6) 0.0148(5) 0.0053(5) 0.0041(5) 0.0042(6) N2 0.0161(7) 0.0187(6) 0.0178(6) 0.0075(5) 0.0049(5) 0.0049(6) N3 0.0175(8) 0.0234(7) 0.0235(7) 0.0107(6) 0.0086(6) 0.0035(6) Cl 0.0215(2) 0.02032(19) 0.02140(18) 0.00633(15) 0.00252(16) 0.00737(17) C1 0.0201(9) 0.0196(8) 0.0224(7) 0.0067(6) 0.0050(7) 0.0064(7) C2 0.0247(10) 0.0288(10) 0.0284(9) 0.0115(8) 0.0038(8) 0.0103(9) C3 0.0193(9) 0.0281(10) 0.0319(10) 0.0058(8) 0.0022(8) 0.0084(8) C4 0.0167(9) 0.0249(9) 0.0304(9) 0.0049(8) 0.0087(8) 0.0031(8) C5 0.0208(9) 0.0215(8) 0.0252(8) 0.0051(7) 0.0082(7) 0.0039(8) C6 0.0183(8) 0.0166(7) 0.0198(7) 0.0033(6) 0.0052(6) 0.0038(7) C7 0.0190(8) 0.0170(7) 0.0190(7) 0.0069(6) 0.0075(6) 0.0039(7) C8 0.0190(8) 0.0164(7) 0.0183(7) 0.0044(6) 0.0080(6) 0.0037(7) C9 0.0202(9) 0.0166(7) 0.0240(8) 0.0062(6) 0.0067(7) 0.0057(7) C111 0.0254(10) 0.0192(8) 0.0195(7) 0.0066(6) 0.0095(7) 0.0052(8) C112 0.0409(13) 0.0187(8) 0.0266(9) 0.0066(7) 0.0111(9) 0.0076(9) C113 0.0587(18) 0.0228(10) 0.0312(11) 0.0024(8) 0.0144(12) 0.0101(11) C114 0.0591(18) 0.0350(12) 0.0225(9) -0.0007(9) 0.0116(11) 0.0055(13) C115 0.0621(19) 0.0379(13) 0.0197(9) 0.0079(9) 0.0076(10) 0.0135(13) C116 0.0479(14) 0.0248(9) 0.0213(8) 0.0096(7) 0.0100(9) 0.0096(10) C121 0.0235(9) 0.0172(7) 0.0239(8) 0.0082(6) 0.0096(7) 0.0042(7) C122 0.0287(11) 0.0233(9) 0.0271(9) 0.0063(7) 0.0125(8) 0.0053(8) C123 0.0315(12) 0.0294(11) 0.0380(12) 0.0083(9) 0.0196(10) 0.0058(10) C124 0.0257(11) 0.0338(12) 0.0409(13) 0.0107(10) 0.0104(10) 0.0001(10) C125 0.0329(13) 0.0317(11) 0.0279(10) 0.0054(9) 0.0031(9) -0.0031(10) C126 0.0290(11) 0.0256(9) 0.0244(8) 0.0053(7) 0.0092(8) 0.0017(9) C131 0.0298(10) 0.0209(8) 0.0223(8) 0.0089(7) 0.0121(8) 0.0079(8) C132 0.0342(12) 0.0174(8) 0.0362(11) 0.0066(8) 0.0104(10) 0.0052(9) C133 0.0498(16) 0.0188(9) 0.0387(12) 0.0065(9) 0.0116(12) 0.0095(10) C134 0.0583(17) 0.0283(10) 0.0390(12) 0.0151(9) 0.0284(12) 0.0252(12) C135 0.0434(15) 0.0407(14) 0.0628(18) 0.0272(13) 0.0310(14) 0.0265(13) C136 0.0307(12) 0.0313(11) 0.0511(14) 0.0227(11) 0.0204(11) 0.0122(10) C211 0.0209(9) 0.0134(7) 0.0300(9) 0.0049(6) 0.0088(7) 0.0032(7) C212 0.0288(11) 0.0200(8) 0.0331(10) 0.0116(8) 0.0061(9) 0.0033(8) C213 0.0404(14) 0.0267(10) 0.0417(13) 0.0191(10) 0.0124(11) 0.0046(10) C214 0.0323(13) 0.0265(11) 0.0550(16) 0.0178(11) 0.0146(12) 0.0009(10) C215 0.0273(12) 0.0249(10) 0.0513(15) 0.0063(10) 0.0089(11) -0.0050(10) C216 0.0278(11) 0.0221(9) 0.0327(10) 0.0020(8) 0.0070(9) -0.0005(9) C221 0.0236(9) 0.0175(7) 0.0209(7) 0.0045(6) 0.0080(7) 0.0082(7) C222 0.0302(11) 0.0185(8) 0.0323(10) 0.0044(7) 0.0112(9) 0.0065(8) C223 0.0433(14) 0.0257(10) 0.0373(11) 0.0088(9) 0.0190(11) 0.0186(10) C224 0.0377(12) 0.0396(12) 0.0304(10) 0.0152(9) 0.0181(9) 0.0246(11) C225 0.0238(10) 0.0353(11) 0.0280(9) 0.0088(8) 0.0110(8) 0.0102(9) C226 0.0232(9) 0.0214(8) 0.0246(8) 0.0066(7) 0.0083(7) 0.0081(8) C231 0.0286(10) 0.0162(7) 0.0198(7) 0.0014(6) 0.0034(7) 0.0052(8) C232 0.0334(12) 0.0281(10) 0.0241(9) -0.0002(8) -0.0004(8) 0.0124(10) C233 0.0450(15) 0.0325(12) 0.0294(10) 0.0002(9) -0.0093(10) 0.0161(11) C234 0.0635(19) 0.0310(12) 0.0229(9) 0.0060(9) -0.0030(11) 0.0088(13) C235 0.0542(17) 0.0367(13) 0.0254(10) 0.0086(9) 0.0107(11) 0.0075(12) C236 0.0341(12) 0.0245(9) 0.0236(8) 0.0061(7) 0.0078(8) 0.0007(9) C311 0.0204(9) 0.0150(7) 0.0192(7) 0.0040(6) 0.0047(6) 0.0030(7) C312 0.0248(10) 0.0208(8) 0.0202(7) 0.0015(6) 0.0052(7) 0.0057(8) C313 0.0305(11) 0.0181(8) 0.0219(8) 0.0013(6) 0.0023(8) 0.0054(8) C314 0.0249(10) 0.0209(8) 0.0268(9) 0.0048(7) 0.0017(8) 0.0013(8) C315 0.0207(10) 0.0279(10) 0.0303(10) 0.0012(8) 0.0070(8) 0.0020(9) C316 0.0222(10) 0.0199(8) 0.0239(8) -0.0004(7) 0.0073(7) 0.0024(8) C321 0.0192(8) 0.0178(7) 0.0176(7) 0.0039(6) 0.0070(6) 0.0042(7) C322 0.0262(10) 0.0229(8) 0.0227(8) 0.0041(7) 0.0074(7) 0.0105(8) C323 0.0262(10) 0.0345(11) 0.0240(8) 0.0017(8) 0.0087(8) 0.0134(9) C324 0.0287(11) 0.0412(12) 0.0232(9) 0.0074(8) 0.0129(8) 0.0090(10) C325 0.0355(12) 0.0336(11) 0.0239(9) 0.0131(8) 0.0127(9) 0.0083(10) C326 0.0259(10) 0.0232(8) 0.0234(8) 0.0088(7) 0.0102(7) 0.0078(8) C331 0.0233(9) 0.0145(7) 0.0197(7) 0.0047(6) 0.0068(7) 0.0070(7) C332 0.0249(10) 0.0189(8) 0.0215(7) 0.0058(6) 0.0059(7) 0.0077(8) C333 0.0314(11) 0.0294(10) 0.0260(9) 0.0085(8) 0.0046(8) 0.0161(9) C334 0.0460(14) 0.0295(11) 0.0330(11) 0.0175(9) 0.0125(10) 0.0175(11) C335 0.0405(14) 0.0252(10) 0.0399(12) 0.0188(9) 0.0142(11) 0.0079(10) C336 0.0272(11) 0.0231(9) 0.0313(10) 0.0108(8) 0.0077(9) 0.0032(8) C101 0.0365(16) 0.066(2) 0.0560(19) 0.0244(17) 0.0031(14) 0.0086(16) C102 0.0277(12) 0.0352(13) 0.0420(13) 0.0045(11) 0.0034(10) 0.0100(10) N103 0.0518(16) 0.0425(14) 0.0487(14) 0.0077(11) 0.0132(12) 0.0188(12) C201 0.0373(14) 0.0338(13) 0.0456(14) 0.0086(11) 0.0108(12) 0.0074(11) C202 0.0322(13) 0.0389(13) 0.0274(10) 0.0079(9) 0.0057(9) -0.0029(11) N203 0.0596(17) 0.0429(13) 0.0349(11) -0.0004(10) 0.0187(12) -0.0013(12) _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 Ru C9 1.824(2) . ? Ru N2 2.0650(15) . ? Ru O2 2.2423(14) . ? Ru P2 2.3793(5) . ? Ru P3 2.3843(5) . ? Ru Cl 2.3992(5) . ? Ru C8 2.5986(18) . ? Pd N3 1.9850(17) . ? Pd O1 1.9984(15) . ? Pd N1 2.0171(15) . ? Pd P1 2.2650(5) . ? P1 C111 1.812(2) . ? P1 C121 1.815(2) . ? P1 C131 1.826(2) . ? P2 C211 1.820(2) . ? P2 C231 1.829(2) . ? P2 C221 1.831(2) . ? P3 C321 1.8221(19) . ? P3 C311 1.827(2) . ? P3 C331 1.8297(18) . ? O1 C1 1.312(3) . ? O2 C8 1.295(2) . ? O3 C9 1.148(3) . ? N1 C7 1.287(3) . ? N1 N2 1.360(2) . ? N2 C8 1.353(2) . ? N3 C8 1.324(2) . ? C1 C2 1.421(3) . ? C1 C6 1.426(3) . ? C2 C3 1.373(3) . ? C3 C4 1.393(3) . ? C4 C5 1.382(3) . ? C5 C6 1.411(3) . ? C6 C7 1.449(3) . ? C111 C116 1.392(3) . ? C111 C112 1.403(3) . ? C112 C113 1.379(3) . ? C113 C114 1.395(4) . ? C114 C115 1.374(4) . ? C115 C116 1.391(3) . ? C121 C126 1.393(3) . ? C121 C122 1.395(3) . ? C122 C123 1.388(3) . ? C123 C124 1.367(4) . ? C124 C125 1.389(4) . ? C125 C126 1.379(4) . ? C131 C136 1.389(3) . ? C131 C132 1.397(3) . ? C132 C133 1.389(3) . ? C133 C134 1.381(4) . ? C134 C135 1.392(4) . ? C135 C136 1.395(4) . ? C211 C216 1.390(3) . ? C211 C212 1.403(3) . ? C212 C213 1.385(3) . ? C213 C214 1.383(4) . ? C214 C215 1.385(4) . ? C215 C216 1.385(4) . ? C221 C226 1.391(3) . ? C221 C222 1.397(3) . ? C222 C223 1.387(3) . ? C223 C224 1.383(4) . ? C224 C225 1.381(4) . ? C225 C226 1.393(3) . ? C231 C236 1.391(3) . ? C231 C232 1.398(3) . ? C232 C233 1.391(3) . ? C233 C234 1.378(5) . ? C234 C235 1.379(5) . ? C235 C236 1.394(3) . ? C311 C316 1.388(3) . ? C311 C312 1.401(3) . ? C312 C313 1.389(3) . ? C313 C314 1.381(3) . ? C314 C315 1.391(3) . ? C315 C316 1.389(3) . ? C321 C322 1.387(3) . ? C321 C326 1.401(3) . ? C322 C323 1.390(3) . ? C323 C324 1.381(3) . ? C324 C325 1.384(3) . ? C325 C326 1.396(3) . ? C331 C332 1.400(3) . ? C331 C336 1.401(3) . ? C332 C333 1.395(3) . ? C333 C334 1.382(4) . ? C334 C335 1.385(4) . ? C335 C336 1.386(3) . ? C101 C102 1.446(5) . ? C102 N103 1.131(4) . ? C201 C202 1.453(4) . ? C202 N203 1.138(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 C9 Ru N2 104.45(8) . . ? C9 Ru O2 165.42(7) . . ? N2 Ru O2 60.97(6) . . ? C9 Ru P2 90.45(6) . . ? N2 Ru P2 90.99(5) . . ? O2 Ru P2 90.01(4) . . ? C9 Ru P3 90.86(6) . . ? N2 Ru P3 91.49(5) . . ? O2 Ru P3 89.45(4) . . ? P2 Ru P3 176.825(18) . . ? C9 Ru Cl 94.31(6) . . ? N2 Ru Cl 161.24(5) . . ? O2 Ru Cl 100.27(4) . . ? P2 Ru Cl 89.028(17) . . ? P3 Ru Cl 87.989(17) . . ? C9 Ru C8 135.54(7) . . ? N2 Ru C8 31.14(6) . . ? O2 Ru C8 29.88(6) . . ? P2 Ru C8 91.95(4) . . ? P3 Ru C8 89.15(4) . . ? Cl Ru C8 130.11(5) . . ? N3 Pd O1 172.92(7) . . ? N3 Pd N1 80.50(7) . . ? O1 Pd N1 93.10(6) . . ? N3 Pd P1 96.18(5) . . ? O1 Pd P1 90.26(5) . . ? N1 Pd P1 176.58(5) . . ? C111 P1 C121 103.93(10) . . ? C111 P1 C131 106.48(9) . . ? C121 P1 C131 101.85(10) . . ? C111 P1 Pd 110.52(7) . . ? C121 P1 Pd 114.89(6) . . ? C131 P1 Pd 117.86(7) . . ? C211 P2 C231 105.52(10) . . ? C211 P2 C221 102.34(9) . . ? C231 P2 C221 103.24(9) . . ? C211 P2 Ru 112.72(7) . . ? C231 P2 Ru 113.68(7) . . ? C221 P2 Ru 117.91(7) . . ? C321 P3 C311 101.15(9) . . ? C321 P3 C331 105.71(9) . . ? C311 P3 C331 102.23(9) . . ? C321 P3 Ru 115.48(7) . . ? C311 P3 Ru 116.33(6) . . ? C331 P3 Ru 114.17(6) . . ? C1 O1 Pd 124.39(12) . . ? C8 O2 Ru 90.47(11) . . ? C7 N1 N2 120.91(15) . . ? C7 N1 Pd 126.33(13) . . ? N2 N1 Pd 112.61(12) . . ? C8 N2 N1 114.45(15) . . ? C8 N2 Ru 96.75(11) . . ? N1 N2 Ru 148.58(13) . . ? C8 N3 Pd 112.05(14) . . ? O1 C1 C2 116.65(18) . . ? O1 C1 C6 126.51(18) . . ? C2 C1 C6 116.84(19) . . ? C3 C2 C1 122.4(2) . . ? C2 C3 C4 120.8(2) . . ? C5 C4 C3 118.3(2) . . ? C4 C5 C6 122.7(2) . . ? C5 C6 C1 118.93(18) . . ? C5 C6 C7 115.89(17) . . ? C1 C6 C7 125.19(18) . . ? N1 C7 C6 124.21(17) . . ? O2 C8 N3 128.07(18) . . ? O2 C8 N2 111.61(16) . . ? N3 C8 N2 120.32(17) . . ? O2 C8 Ru 59.64(9) . . ? N3 C8 Ru 171.47(15) . . ? N2 C8 Ru 52.11(9) . . ? O3 C9 Ru 177.9(2) . . ? C116 C111 C112 119.33(19) . . ? C116 C111 P1 123.23(16) . . ? C112 C111 P1 117.25(15) . . ? C113 C112 C111 119.9(2) . . ? C112 C113 C114 120.5(2) . . ? C115 C114 C113 119.7(2) . . ? C114 C115 C116 120.6(2) . . ? C115 C116 C111 120.0(2) . . ? C126 C121 C122 119.3(2) . . ? C126 C121 P1 118.22(16) . . ? C122 C121 P1 122.22(17) . . ? C123 C122 C121 120.2(2) . . ? C124 C123 C122 120.0(2) . . ? C123 C124 C125 120.3(2) . . ? C126 C125 C124 120.4(2) . . ? C125 C126 C121 119.8(2) . . ? C136 C131 C132 119.1(2) . . ? C136 C131 P1 119.46(17) . . ? C132 C131 P1 121.46(18) . . ? C133 C132 C131 120.4(2) . . ? C134 C133 C132 120.7(2) . . ? C133 C134 C135 119.0(2) . . ? C134 C135 C136 120.9(3) . . ? C131 C136 C135 119.9(2) . . ? C216 C211 C212 119.0(2) . . ? C216 C211 P2 124.62(17) . . ? C212 C211 P2 116.40(16) . . ? C213 C212 C211 120.1(2) . . ? C214 C213 C212 120.6(3) . . ? C213 C214 C215 119.4(2) . . ? C214 C215 C216 120.7(2) . . ? C215 C216 C211 120.2(2) . . ? C226 C221 C222 119.43(19) . . ? C226 C221 P2 120.57(15) . . ? C222 C221 P2 120.00(17) . . ? C223 C222 C221 120.3(2) . . ? C224 C223 C222 120.2(2) . . ? C225 C224 C223 119.8(2) . . ? C224 C225 C226 120.7(2) . . ? C221 C226 C225 119.6(2) . . ? C236 C231 C232 118.6(2) . . ? C236 C231 P2 121.75(17) . . ? C232 C231 P2 119.42(17) . . ? C233 C232 C231 120.4(2) . . ? C234 C233 C232 120.4(3) . . ? C233 C234 C235 119.7(2) . . ? C234 C235 C236 120.4(3) . . ? C231 C236 C235 120.4(2) . . ? C316 C311 C312 119.29(19) . . ? C316 C311 P3 120.71(15) . . ? C312 C311 P3 119.95(16) . . ? C313 C312 C311 120.1(2) . . ? C314 C313 C312 120.32(19) . . ? C313 C314 C315 119.7(2) . . ? C316 C315 C314 120.3(2) . . ? C311 C316 C315 120.19(19) . . ? C322 C321 C326 119.68(18) . . ? C322 C321 P3 121.94(15) . . ? C326 C321 P3 118.10(14) . . ? C321 C322 C323 120.3(2) . . ? C324 C323 C322 120.1(2) . . ? C323 C324 C325 120.2(2) . . ? C324 C325 C326 120.3(2) . . ? C325 C326 C321 119.45(19) . . ? C332 C331 C336 118.77(18) . . ? C332 C331 P3 119.47(15) . . ? C336 C331 P3 121.61(16) . . ? C333 C332 C331 120.1(2) . . ? C334 C333 C332 120.4(2) . . ? C333 C334 C335 119.8(2) . . ? C334 C335 C336 120.4(2) . . ? C335 C336 C331 120.4(2) . . ? N103 C102 C101 179.6(3) . . ? N203 C202 C201 178.6(3) . . ? _diffrn_measured_fraction_theta_max 0.769 _diffrn_reflns_theta_full 40.60 _diffrn_measured_fraction_theta_full 0.769 _refine_diff_density_max 1.601 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.115 data_ss154_0m _database_code_depnum_ccdc_archive 'CCDC 848668' #TrackingRef '226SB-SD-11-r.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H53 Cl N3 O3 P3 Pd Ru' _chemical_formula_weight 1283.95 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' Cl Cl 0.1484 0.1585 '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' Ru Ru -1.2594 0.8363 '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 19.145(4) _cell_length_b 26.722(6) _cell_length_c 26.880(6) _cell_angle_alpha 66.307(6) _cell_angle_beta 89.242(7) _cell_angle_gamma 87.514(7) _cell_volume 12580(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 0.8 _cell_measurement_theta_max 17.7 _exptl_crystal_description block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5216 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8975 _exptl_absorpt_correction_T_max 0.9094 _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 'CCD area detector' _diffrn_measurement_method 'Phi and omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66604 _diffrn_reflns_av_R_equivalents 0.1153 _diffrn_reflns_av_sigmaI/netI 0.0998 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 0.83 _diffrn_reflns_theta_max 17.74 _reflns_number_total 16255 _reflns_number_gt 10509 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXLTL' _computing_publication_material 'MERCURY 1.4' _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^)+(0.0672P)^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 16255 _refine_ls_number_parameters 1470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _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 Pd2 Pd 0.14317(6) 0.57938(5) 0.27600(4) 0.0491(4) Uani 1 1 d . . . Pd4 Pd 0.62598(5) 0.41623(5) 0.23347(4) 0.0475(4) Uani 1 1 d . . . Pd3 Pd 0.13630(5) 0.07739(4) 0.16279(4) 0.0425(4) Uani 1 1 d . . . Pd1 Pd 0.63888(5) 0.92127(4) 0.33789(4) 0.0448(4) Uani 1 1 d . . . Ru1 Ru 0.74304(6) 0.98202(5) 0.46737(4) 0.0432(4) Uani 1 1 d . . . Ru2 Ru 0.23825(6) 0.54518(5) 0.45390(5) 0.0521(4) Uani 1 1 d . . . Ru4 Ru 0.73415(6) 0.47565(5) 0.05508(5) 0.0526(4) Uani 1 1 d . . . Ru3 Ru 0.24271(6) 0.01838(5) 0.02912(4) 0.0426(4) Uani 1 1 d . . . P7 P 0.03644(19) 0.07972(16) 0.20791(15) 0.0494(12) Uani 1 1 d . . . P3 P 0.53965(19) 0.91906(16) 0.29291(15) 0.0489(12) Uani 1 1 d . . . P9 P 0.2675(2) -0.07385(16) 0.09247(15) 0.0492(12) Uani 1 1 d . . . P6 P 0.2476(2) 0.44900(17) 0.47458(16) 0.0558(12) Uani 1 1 d . . . P8 P 0.19988(19) 0.10406(16) -0.03741(15) 0.0488(12) Uani 1 1 d . . . P11 P 0.7577(2) 0.55998(17) 0.06132(17) 0.0594(13) Uani 1 1 d . . . Cl1 Cl 0.74424(19) 1.01843(15) 0.53624(14) 0.0578(11) Uani 1 1 d . . . P2 P 0.7127(2) 0.89642(16) 0.53708(16) 0.0519(12) Uani 1 1 d . . . Cl2 Cl 0.23476(19) 0.52132(16) 0.55040(14) 0.0647(12) Uani 1 1 d . . . O2 O 0.6330(4) 1.0010(3) 0.4385(3) 0.048(3) Uani 1 1 d . . . P1 P 0.7577(2) 1.07231(16) 0.40097(15) 0.0493(12) Uani 1 1 d . . . C246 C 0.7595(8) 0.5493(6) 0.1348(6) 0.060(4) Uiso 1 1 d . . . P12 P 0.70716(19) 0.39114(17) 0.05078(15) 0.0524(12) Uani 1 1 d . . . P4 P 0.0476(2) 0.57056(16) 0.23219(15) 0.0529(12) Uani 1 1 d . . . Cl4 Cl 0.73355(19) 0.51979(16) -0.04302(15) 0.0676(12) Uani 1 1 d . . . O12 O 0.6232(4) 0.4922(4) 0.0692(3) 0.060(3) Uani 1 1 d . . . N6 N 0.2254(6) 0.5793(4) 0.3212(4) 0.045(3) Uiso 1 1 d . . . N4 N 0.0977(6) 0.5507(4) 0.3488(4) 0.057(3) Uiso 1 1 d . . . H4' H 0.0552 0.5407 0.3539 0.068 Uiso 1 1 calc R . . Cl3 Cl 0.24505(18) -0.01587(15) -0.04102(14) 0.0554(11) Uani 1 1 d . . . P10 P 0.52541(19) 0.41550(16) 0.27986(15) 0.0510(12) Uani 1 1 d . . . P5 P 0.2138(2) 0.63898(17) 0.43568(16) 0.0592(13) Uani 1 1 d . . . O9 O 0.1343(4) 0.0011(3) 0.0603(3) 0.048(3) Uani 1 1 d . . . N9 N 0.2223(5) 0.0696(4) 0.1225(4) 0.040(3) Uiso 1 1 d . . . O3 O 0.6936(5) 0.8773(4) 0.3048(4) 0.063(3) Uani 1 1 d . . . O11 O 0.6803(5) 0.3725(4) 0.3018(3) 0.069(3) Uani 1 1 d . . . N12 N 0.7107(6) 0.4194(4) 0.1894(5) 0.051(3) Uiso 1 1 d . . . O8 O 0.1865(5) 0.1215(4) 0.1948(4) 0.064(3) Uani 1 1 d . . . N1 N 0.5974(6) 0.9653(4) 0.3752(4) 0.049(3) Uiso 1 1 d . . . H1 H 0.5542 0.9766 0.3715 0.059 Uiso 1 1 calc R . . C156 C 0.1169(7) 0.1370(6) -0.1316(6) 0.062(5) Uiso 1 1 d . . . H156 H 0.1491 0.1638 -0.1483 0.074 Uiso 1 1 calc R . . C137 C -0.0026(7) 0.1454(5) 0.1975(5) 0.046(4) Uiso 1 1 d . . . N7 N 0.0989(6) 0.0337(4) 0.1262(4) 0.055(3) Uiso 1 1 d . . . H7 H 0.0571 0.0220 0.1316 0.066 Uiso 1 1 calc R . . O5 O 0.1987(5) 0.6125(4) 0.2067(3) 0.069(3) Uani 1 1 d . . . C149 C 0.0493(7) 0.0464(5) 0.2803(5) 0.048(4) Uiso 1 1 d . . . O6 O 0.1272(4) 0.5353(4) 0.4386(4) 0.061(3) Uani 1 1 d . . . C259 C 0.6880(7) 0.3373(5) 0.1180(5) 0.047(4) Uiso 1 1 d . . . N11 N 0.6978(5) 0.4460(4) 0.1337(4) 0.048(3) Uiso 1 1 d . . . N5 N 0.2079(6) 0.5610(4) 0.3752(4) 0.052(3) Uiso 1 1 d . . . C223 C 0.7745(7) 0.4018(5) 0.2057(6) 0.048(4) Uani 1 1 d . . . H223 H 0.8091 0.4096 0.1793 0.058 Uiso 1 1 calc R . . C82 C 0.0664(7) 0.5371(5) 0.1880(5) 0.050(4) Uiso 1 1 d . . . C176 C 0.3010(7) 0.1203(5) 0.1531(5) 0.050(4) Uiso 1 1 d . . . C185 C 0.2512(8) 0.1349(6) 0.1848(6) 0.051(4) Uiso 1 1 d . . . C30 C 0.6373(7) 0.8756(6) 0.6335(6) 0.059(4) Uiso 1 1 d . . . H30 H 0.6761 0.8543 0.6519 0.071 Uiso 1 1 calc R . . C25 C 0.6379(7) 0.9017(6) 0.5781(6) 0.059(4) Uiso 1 1 d . . . C222 C 0.6327(7) 0.4671(6) 0.1205(6) 0.046(4) Uiso 1 1 d . . . C113 C 0.2517(8) 0.6987(6) 0.3253(6) 0.077(5) Uiso 1 1 d . . . H113 H 0.2977 0.6941 0.3377 0.092 Uiso 1 1 calc R . . C19 C 0.7759(7) 0.8575(6) 0.5912(5) 0.053(4) Uiso 1 1 d . . . C112 C 0.1956(8) 0.6797(6) 0.3629(6) 0.063(5) Uiso 1 1 d . . . C89 C 0.2880(7) 0.5926(5) 0.3063(6) 0.058(4) Uani 1 1 d . . . H89 H 0.3218 0.5866 0.3329 0.070 Uiso 1 1 calc R . . C155 C 0.1271(7) 0.1001(6) -0.0787(6) 0.055(4) Uiso 1 1 d . . . C52 C 0.5511(7) 0.9528(5) 0.2204(5) 0.049(4) Uiso 1 1 d . . . C6 C 0.8784(7) 1.0884(6) 0.4459(6) 0.063(5) Uiso 1 1 d . . . H6 H 0.8599 1.0640 0.4784 0.076 Uiso 1 1 calc R . . C125 C 0.3325(7) 0.4144(6) 0.4967(6) 0.055(4) Uiso 1 1 d . . . C88 C 0.1396(7) 0.5485(5) 0.3881(6) 0.045(4) Uiso 1 1 d . . . C58 C 0.5092(7) 0.8531(6) 0.3035(5) 0.055(4) Uiso 1 1 d . . . C239 C 0.8756(8) 0.5742(6) -0.0028(6) 0.082(5) Uiso 1 1 d . . . H239 H 0.8552 0.5493 -0.0137 0.098 Uiso 1 1 calc R . . C100 C 0.1353(8) 0.6538(6) 0.4685(6) 0.065(5) Uiso 1 1 d . . . C247 C 0.6973(9) 0.5609(7) 0.1566(7) 0.099(6) Uiso 1 1 d . . . H247 H 0.6590 0.5778 0.1343 0.119 Uiso 1 1 calc R . . C186 C 0.2497(7) -0.0848(5) 0.1625(5) 0.050(4) Uiso 1 1 d . . . C168 C 0.0915(8) 0.1566(6) 0.0000(6) 0.070(5) Uiso 1 1 d . . . H168 H 0.0597 0.1403 -0.0141 0.084 Uiso 1 1 calc R . . N8 N 0.2094(5) 0.0405(4) 0.0916(4) 0.041(3) Uiso 1 1 d . . . C57 C 0.5006(8) 0.9506(6) 0.1856(6) 0.067(5) Uiso 1 1 d . . . H57 H 0.4601 0.9323 0.2002 0.081 Uiso 1 1 calc R . . C13 C 0.7400(8) 1.0785(6) 0.3322(6) 0.058(4) Uiso 1 1 d . . . C40 C 0.6421(7) 0.9758(6) 0.4063(6) 0.047(4) Uiso 1 1 d . . . C210 C 0.4528(7) 0.4503(6) 0.2367(5) 0.054(4) Uiso 1 1 d . . . N3 N 0.7241(5) 0.9289(4) 0.3770(4) 0.046(3) Uiso 1 1 d . . . C253 C 0.7774(7) 0.3591(6) 0.0235(6) 0.056(4) Uiso 1 1 d . . . C174 C 0.1430(7) 0.0235(6) 0.0925(6) 0.047(4) Uiso 1 1 d . . . C41 C 0.7866(7) 0.9105(5) 0.3753(5) 0.056(4) Uiso 1 1 d . . . H41 H 0.8208 0.9177 0.3955 0.067 Uiso 1 1 calc R . . N2 N 0.7109(5) 0.9579(4) 0.4081(4) 0.043(3) Uiso 1 1 d . . . C53 C 0.6118(8) 0.9776(6) 0.2012(6) 0.067(5) Uiso 1 1 d . . . H53 H 0.6468 0.9783 0.2246 0.080 Uiso 1 1 calc R . . C59 C 0.5554(9) 0.8081(7) 0.3148(6) 0.085(5) Uiso 1 1 d . . . H59 H 0.6026 0.8119 0.3199 0.102 Uiso 1 1 calc R . . C143 C -0.0321(7) 0.0450(6) 0.1922(6) 0.051(4) Uiso 1 1 d . . . C192 C 0.3553(7) -0.1030(6) 0.0950(6) 0.058(4) Uiso 1 1 d . . . C90 C 0.3091(7) 0.6173(5) 0.2482(6) 0.048(4) Uiso 1 1 d . . . C235 C 0.8758(8) 0.6240(6) 0.0533(6) 0.075(5) Uiso 1 1 d . . . H235 H 0.8556 0.6324 0.0808 0.090 Uiso 1 1 calc R . . C154 C 0.1122(8) 0.0170(6) 0.3001(6) 0.066(5) Uiso 1 1 d . . . H154 H 0.1471 0.0143 0.2769 0.079 Uiso 1 1 calc R . . C221 C 0.4710(8) 0.4616(6) 0.3472(6) 0.078(5) Uiso 1 1 d . . . H221 H 0.4277 0.4592 0.3331 0.094 Uiso 1 1 calc R . . C234 C 0.8449(7) 0.5884(6) 0.0362(6) 0.054(4) Uiso 1 1 d . . . C51 C 0.7609(8) 0.8642(6) 0.3123(6) 0.056(4) Uiso 1 1 d . . . C224 C 0.7951(8) 0.3714(6) 0.2609(7) 0.057(4) Uiso 1 1 d . . . N10 N 0.5851(6) 0.4597(4) 0.1592(4) 0.056(3) Uiso 1 1 d . . . H10' H 0.5424 0.4719 0.1532 0.068 Uiso 1 1 calc R . . C63 C 0.4397(8) 0.8434(7) 0.2987(6) 0.076(5) Uiso 1 1 d . . . H63 H 0.4063 0.8715 0.2924 0.091 Uiso 1 1 calc R . . C233 C 0.7476(9) 0.3591(6) 0.3027(6) 0.060(5) Uiso 1 1 d . . . C216 C 0.5301(8) 0.4469(5) 0.3272(5) 0.055(4) Uiso 1 1 d . . . C24 C 0.7747(7) 0.8008(6) 0.6169(6) 0.067(5) Uiso 1 1 d . . . H24 H 0.7472 0.7812 0.6034 0.081 Uiso 1 1 calc R . . C167 C 0.1618(7) 0.1504(5) -0.0076(5) 0.050(4) Uiso 1 1 d . . . C172 C 0.2097(8) 0.1765(6) 0.0140(6) 0.072(5) Uiso 1 1 d . . . H172 H 0.2577 0.1719 0.0105 0.086 Uiso 1 1 calc R . . C87 C 0.0153(8) 0.5346(6) 0.1515(6) 0.076(5) Uiso 1 1 d . . . H87 H -0.0283 0.5519 0.1502 0.091 Uiso 1 1 calc R . . C86 C 0.0274(8) 0.5072(6) 0.1176(6) 0.073(5) Uiso 1 1 d . . . H86 H -0.0072 0.5060 0.0942 0.087 Uiso 1 1 calc R . . C177 C 0.3717(7) 0.1394(6) 0.1485(6) 0.058(4) Uiso 1 1 d . . . C197 C 0.3861(8) -0.1388(6) 0.1447(6) 0.071(5) Uiso 1 1 d . . . H197 H 0.3628 -0.1461 0.1773 0.085 Uiso 1 1 calc R . . C161 C 0.2611(7) 0.1449(6) -0.0890(5) 0.053(4) Uiso 1 1 d . . . C220 C 0.4747(8) 0.4806(6) 0.3898(6) 0.076(5) Uiso 1 1 d . . . H220 H 0.4341 0.4908 0.4032 0.092 Uiso 1 1 calc R . . C260 C 0.7408(8) 0.3166(6) 0.1570(6) 0.061(5) Uiso 1 1 d . . . H260 H 0.7859 0.3286 0.1476 0.073 Uiso 1 1 calc R . . C31 C 0.6910(8) 0.8479(6) 0.5092(6) 0.060(4) Uiso 1 1 d . . . C42 C 0.8078(7) 0.8788(5) 0.3436(5) 0.046(4) Uiso 1 1 d . . . C205 C 0.5079(8) 0.3082(6) 0.2964(6) 0.072(5) Uiso 1 1 d . . . H205 H 0.5380 0.3159 0.2671 0.087 Uiso 1 1 calc R . . C206 C 0.4793(9) 0.2575(7) 0.3179(7) 0.094(6) Uiso 1 1 d . . . H206 H 0.4874 0.2322 0.3025 0.113 Uiso 1 1 calc R . . C204 C 0.4948(7) 0.3487(5) 0.3158(5) 0.046(4) Uiso 1 1 d . . . C254 C 0.8040(8) 0.3913(7) -0.0257(6) 0.076(5) Uiso 1 1 d . . . H254 H 0.7900 0.4280 -0.0429 0.091 Uiso 1 1 calc R . . C1 C 0.8432(7) 1.1013(6) 0.3971(6) 0.057(4) Uiso 1 1 d . . . C236 C 0.9382(8) 0.6476(6) 0.0288(6) 0.081(5) Uiso 1 1 d . . . H236 H 0.9580 0.6734 0.0388 0.097 Uiso 1 1 calc R . . C131 C 0.2284(8) 0.4324(6) 0.4166(6) 0.069(5) Uiso 1 1 d . . . C166 C 0.3036(7) 0.1187(6) -0.1145(6) 0.066(5) Uiso 1 1 d . . . H166 H 0.3038 0.0808 -0.1022 0.079 Uiso 1 1 calc R . . C106 C 0.2804(8) 0.6774(7) 0.4533(6) 0.070(5) Uiso 1 1 d . . . C130 C 0.3608(8) 0.3755(6) 0.4796(6) 0.076(5) Uiso 1 1 d . . . H130 H 0.3368 0.3666 0.4546 0.091 Uiso 1 1 calc R . . C183 C 0.3371(8) 0.1902(6) 0.2031(6) 0.068(5) Uiso 1 1 d . . . H183 H 0.3477 0.2135 0.2197 0.081 Uiso 1 1 calc R . . C182 C 0.3894(8) 0.1763(6) 0.1737(6) 0.073(5) Uiso 1 1 d . . . C184 C 0.2725(7) 0.1716(5) 0.2085(5) 0.059(4) Uiso 1 1 d . . . H184 H 0.2399 0.1828 0.2284 0.070 Uiso 1 1 calc R . . C264 C 0.6197(8) 0.3204(6) 0.1334(6) 0.072(5) Uiso 1 1 d . . . H264 H 0.5832 0.3337 0.1084 0.087 Uiso 1 1 calc R . . C181 C 0.4590(8) 0.1940(6) 0.1685(6) 0.084(5) Uiso 1 1 d . . . H181 H 0.4711 0.2173 0.1847 0.100 Uiso 1 1 calc R . . C171 C 0.1826(9) 0.2090(6) 0.0405(6) 0.088(6) Uiso 1 1 d . . . H171 H 0.2121 0.2275 0.0539 0.105 Uiso 1 1 calc R . . C70 C -0.0151(7) 0.5299(6) 0.2788(5) 0.056(4) Uiso 1 1 d . . . C23 C 0.8157(8) 0.7740(7) 0.6634(6) 0.072(5) Uiso 1 1 d . . . H23 H 0.8131 0.7363 0.6822 0.087 Uiso 1 1 calc R . . C65 C 0.4344(7) 1.0022(6) 0.2725(6) 0.060(5) Uiso 1 1 d . . . H65 H 0.4521 1.0188 0.2375 0.072 Uiso 1 1 calc R . . C47 C 0.9747(8) 0.8099(6) 0.3213(6) 0.071(5) Uiso 1 1 d . . . H47 H 0.9889 0.7859 0.3055 0.086 Uiso 1 1 calc R . . C20 C 0.8196(7) 0.8839(6) 0.6101(6) 0.058(4) Uiso 1 1 d . . . H20 H 0.8225 0.9215 0.5918 0.070 Uiso 1 1 calc R . . C45 C 1.0026(9) 0.8600(6) 0.3728(6) 0.089(6) Uiso 1 1 d . . . H45 H 1.0354 0.8709 0.3912 0.107 Uiso 1 1 calc R . . C170 C 0.1142(9) 0.2124(7) 0.0458(6) 0.088(6) Uiso 1 1 d . . . H170 H 0.0971 0.2346 0.0628 0.105 Uiso 1 1 calc R . . C144 C -0.0652(7) 0.0697(6) 0.1401(5) 0.053(4) Uiso 1 1 d . . . H144 H -0.0513 0.1038 0.1159 0.064 Uiso 1 1 calc R . . C64 C 0.4650(7) 0.9536(6) 0.3083(6) 0.050(4) Uiso 1 1 d . . . C46 C 1.0227(9) 0.8271(6) 0.3462(6) 0.084(5) Uiso 1 1 d . . . H46 H 1.0696 0.8167 0.3456 0.101 Uiso 1 1 calc R . . C153 C 0.1202(9) -0.0087(6) 0.3581(7) 0.083(5) Uiso 1 1 d . . . H153 H 0.1619 -0.0280 0.3725 0.100 Uiso 1 1 calc R . . C162 C 0.2621(7) 0.2018(6) -0.1077(6) 0.069(5) Uiso 1 1 d . . . H162 H 0.2345 0.2201 -0.0910 0.083 Uiso 1 1 calc R . . C72 C -0.1068(8) 0.5183(7) 0.3464(6) 0.081(5) Uiso 1 1 d . . . H72 H -0.1390 0.5335 0.3631 0.097 Uiso 1 1 calc R . . C71 C -0.0608(7) 0.5518(6) 0.3070(5) 0.057(4) Uiso 1 1 d . . . H71 H -0.0606 0.5889 0.2996 0.068 Uiso 1 1 calc R . . C66 C 0.3770(8) 1.0268(7) 0.2880(7) 0.080(5) Uiso 1 1 d . . . H66 H 0.3570 1.0600 0.2640 0.096 Uiso 1 1 calc R . . C193 C 0.3937(8) -0.0900(6) 0.0480(6) 0.070(5) Uiso 1 1 d . . . H193 H 0.3747 -0.0639 0.0159 0.085 Uiso 1 1 calc R . . C120 C 0.1270(8) 0.4271(6) 0.5364(6) 0.070(5) Uiso 1 1 d . . . H120 H 0.1149 0.4640 0.5173 0.084 Uiso 1 1 calc R . . C148 C -0.0539(7) -0.0058(6) 0.2270(6) 0.064(5) Uiso 1 1 d . . . H148 H -0.0336 -0.0232 0.2613 0.077 Uiso 1 1 calc R . . C225 C 0.8685(8) 0.3526(6) 0.2729(6) 0.066(5) Uiso 1 1 d . . . C73 C -0.1039(8) 0.4639(7) 0.3596(6) 0.079(5) Uiso 1 1 d . . . H73 H -0.1350 0.4421 0.3853 0.094 Uiso 1 1 calc R . . C119 C 0.1883(8) 0.4064(6) 0.5271(6) 0.067(5) Uiso 1 1 d . . . C165 C 0.3462(8) 0.1490(7) -0.1586(7) 0.089(6) Uiso 1 1 d . . . H165 H 0.3742 0.1318 -0.1760 0.107 Uiso 1 1 calc R . . C68 C 0.3766(8) 0.9537(6) 0.3754(7) 0.076(5) Uiso 1 1 d . . . H68 H 0.3560 0.9376 0.4094 0.092 Uiso 1 1 calc R . . C67 C 0.3512(8) 1.0011(6) 0.3389(6) 0.071(5) Uiso 1 1 d . . . H67 H 0.3131 1.0178 0.3488 0.085 Uiso 1 1 calc R . . C187 C 0.2833(7) -0.0565(6) 0.1866(6) 0.064(5) Uiso 1 1 d . . . H187 H 0.3168 -0.0320 0.1672 0.077 Uiso 1 1 calc R . . C85 C 0.0925(9) 0.4818(6) 0.1196(7) 0.088(6) Uiso 1 1 d . . . H85 H 0.1023 0.4643 0.0965 0.106 Uiso 1 1 calc R . . C163 C 0.3054(8) 0.2317(7) -0.1524(6) 0.080(5) Uiso 1 1 d . . . H163 H 0.3063 0.2696 -0.1659 0.096 Uiso 1 1 calc R . . C8 C 0.6424(7) 1.1130(6) 0.4414(6) 0.069(5) Uiso 1 1 d . . . H8 H 0.6336 1.0764 0.4615 0.083 Uiso 1 1 calc R . . C178 C 0.4258(8) 0.1240(6) 0.1206(6) 0.074(5) Uiso 1 1 d . . . H178 H 0.4156 0.1001 0.1046 0.088 Uiso 1 1 calc R . . C7 C 0.6996(7) 1.1257(6) 0.4077(5) 0.052(4) Uiso 1 1 d . . . C217 C 0.5941(8) 0.4517(6) 0.3480(6) 0.079(5) Uiso 1 1 d . . . H217 H 0.6354 0.4424 0.3346 0.095 Uiso 1 1 calc R . . C261 C 0.7287(9) 0.2789(6) 0.2091(7) 0.082(5) Uiso 1 1 d . . . H261 H 0.7646 0.2644 0.2344 0.098 Uiso 1 1 calc R . . C150 C -0.0018(8) 0.0485(6) 0.3168(6) 0.065(5) Uiso 1 1 d . . . H150 H -0.0434 0.0686 0.3036 0.079 Uiso 1 1 calc R . . C211 C 0.4498(8) 0.5076(6) 0.2106(6) 0.071(5) Uiso 1 1 d . . . H211 H 0.4848 0.5269 0.2176 0.085 Uiso 1 1 calc R . . C60 C 0.5335(10) 0.7584(8) 0.3187(7) 0.104(6) Uiso 1 1 d . . . H60 H 0.5658 0.7294 0.3257 0.125 Uiso 1 1 calc R . . C132 C 0.2705(8) 0.4528(6) 0.3705(6) 0.079(5) Uiso 1 1 d . . . H132 H 0.3077 0.4743 0.3698 0.095 Uiso 1 1 calc R . . C175 C 0.2831(7) 0.0894(5) 0.1225(5) 0.049(4) Uiso 1 1 d . . . H175 H 0.3177 0.0830 0.1010 0.058 Uiso 1 1 calc R . . C75 C -0.0138(8) 0.4735(6) 0.2942(6) 0.071(5) Uiso 1 1 d . . . H75 H 0.0158 0.4576 0.2764 0.086 Uiso 1 1 calc R . . C14 C 0.7868(8) 1.0533(6) 0.3086(6) 0.070(5) Uiso 1 1 d . . . H14 H 0.8275 1.0356 0.3269 0.084 Uiso 1 1 calc R . . C9 C 0.5969(8) 1.1531(7) 0.4468(6) 0.084(5) Uiso 1 1 d . . . H9 H 0.5602 1.1441 0.4714 0.101 Uiso 1 1 calc R . . C18 C 0.6788(9) 1.1036(6) 0.3055(7) 0.089(6) Uiso 1 1 d . . . H18 H 0.6465 1.1195 0.3216 0.107 Uiso 1 1 calc R . . C160 C 0.0803(8) 0.0593(6) -0.0552(6) 0.068(5) Uiso 1 1 d . . . H160 H 0.0884 0.0331 -0.0203 0.082 Uiso 1 1 calc R . . C26 C 0.5791(8) 0.9328(6) 0.5525(7) 0.084(5) Uiso 1 1 d . . . H26 H 0.5783 0.9509 0.5149 0.101 Uiso 1 1 calc R . . C265 C 0.6308(7) 0.3923(6) 0.0093(6) 0.060(4) Uiso 1 1 d . . . C54 C 0.6199(9) 1.0032(7) 0.1422(7) 0.100(6) Uiso 1 1 d . . . H54 H 0.6603 1.0214 0.1272 0.120 Uiso 1 1 calc R . . C97 C 0.3522(8) 0.6774(6) 0.1448(7) 0.078(5) Uiso 1 1 d . . . H97 H 0.3646 0.7014 0.1101 0.093 Uiso 1 1 calc R . . C80 C -0.1062(9) 0.6858(7) 0.1514(7) 0.093(6) Uiso 1 1 d . . . H80 H -0.1534 0.6865 0.1431 0.111 Uiso 1 1 calc R . . C256 C 0.8757(8) 0.3152(7) -0.0251(6) 0.074(5) Uiso 1 1 d . . . H256 H 0.9093 0.3008 -0.0416 0.089 Uiso 1 1 calc R . . C28 C 0.5210(8) 0.9102(6) 0.6369(7) 0.077(5) Uiso 1 1 d . . . H28 H 0.4815 0.9117 0.6569 0.093 Uiso 1 1 calc R . . C44 C 0.9315(8) 0.8771(6) 0.3717(6) 0.071(5) Uiso 1 1 d . . . H44 H 0.9187 0.9006 0.3883 0.085 Uiso 1 1 calc R . . C93 C 0.5020(9) 0.6324(7) 0.2679(7) 0.093(6) Uiso 1 1 d . . . H93 H 0.5355 0.6206 0.2954 0.111 Uiso 1 1 calc R . . C49 C 0.8550(8) 0.8122(6) 0.2904(6) 0.065(5) Uiso 1 1 d . . . H49 H 0.8701 0.7893 0.2736 0.078 Uiso 1 1 calc R . . C5 C 0.9413(8) 1.1124(6) 0.4457(7) 0.083(5) Uiso 1 1 d . . . H5 H 0.9660 1.1032 0.4779 0.099 Uiso 1 1 calc R . . C103 C 0.0164(9) 0.6801(7) 0.5133(6) 0.085(5) Uiso 1 1 d . . . H103 H -0.0237 0.6885 0.5288 0.103 Uiso 1 1 calc R . . C99 C 0.2630(9) 0.6274(6) 0.2058(6) 0.062(5) Uiso 1 1 d . . . C250 C 0.8129(9) 0.5127(7) 0.2226(7) 0.095(6) Uiso 1 1 d . . . H250 H 0.8518 0.4973 0.2446 0.114 Uiso 1 1 calc R . . C3 C 0.9346(8) 1.1633(6) 0.3501(7) 0.079(5) Uiso 1 1 d . . . H3 H 0.9536 1.1881 0.3181 0.095 Uiso 1 1 calc R . . C96 C 0.4004(9) 0.6655(6) 0.1833(7) 0.074(5) Uiso 1 1 d . . . C91 C 0.3818(8) 0.6331(6) 0.2393(6) 0.060(4) Uiso 1 1 d . . . C188 C 0.2685(8) -0.0635(7) 0.2396(7) 0.086(5) Uiso 1 1 d . . . H188 H 0.2923 -0.0448 0.2563 0.103 Uiso 1 1 calc R . . C151 C 0.0080(8) 0.0211(6) 0.3729(6) 0.076(5) Uiso 1 1 d . . . H151 H -0.0275 0.0214 0.3967 0.091 Uiso 1 1 calc R . . C198 C 0.2170(8) -0.1216(6) 0.0796(6) 0.063(5) Uiso 1 1 d . . . C196 C 0.4544(8) -0.1639(6) 0.1443(7) 0.086(5) Uiso 1 1 d . . . H196 H 0.4751 -0.1891 0.1762 0.103 Uiso 1 1 calc R . . C2 C 0.8707(8) 1.1387(6) 0.3503(6) 0.071(5) Uiso 1 1 d . . . H2 H 0.8467 1.1481 0.3177 0.085 Uiso 1 1 calc R . . C76 C 0.0006(8) 0.6339(6) 0.1937(6) 0.067(5) Uiso 1 1 d . . . C232 C 0.7719(9) 0.3297(6) 0.3576(7) 0.085(5) Uiso 1 1 d . . . H232 H 0.7418 0.3226 0.3869 0.102 Uiso 1 1 calc R . . C43 C 0.8800(7) 0.8601(5) 0.3466(5) 0.054(4) Uiso 1 1 d . . . C180 C 0.5081(9) 0.1781(7) 0.1410(7) 0.093(6) Uiso 1 1 d . . . H180 H 0.5529 0.1909 0.1387 0.112 Uiso 1 1 calc R . . C48 C 0.9020(7) 0.8274(5) 0.3182(5) 0.054(4) Uiso 1 1 d . . . C215 C 0.3997(8) 0.4223(7) 0.2265(6) 0.088(6) Uiso 1 1 d . . . H215 H 0.3988 0.3845 0.2444 0.105 Uiso 1 1 calc R . . C145 C -0.1172(7) 0.0446(6) 0.1247(6) 0.068(5) Uiso 1 1 d . . . H145 H -0.1375 0.0611 0.0904 0.082 Uiso 1 1 calc R . . C159 C 0.0189(8) 0.0574(6) -0.0848(6) 0.073(5) Uiso 1 1 d . . . H159 H -0.0133 0.0305 -0.0690 0.087 Uiso 1 1 calc R . . C50 C 0.7855(8) 0.8291(6) 0.2859(6) 0.070(5) Uiso 1 1 d . . . H50 H 0.7547 0.8182 0.2661 0.084 Uiso 1 1 calc R . . C164 C 0.3450(9) 0.2031(7) -0.1744(7) 0.092(6) Uiso 1 1 d . . . H164 H 0.3739 0.2227 -0.2030 0.110 Uiso 1 1 calc R . . C138 C 0.0409(9) 0.1876(7) 0.1893(6) 0.080(5) Uiso 1 1 d . . . H138 H 0.0891 0.1811 0.1892 0.096 Uiso 1 1 calc R . . C214 C 0.3452(10) 0.4526(8) 0.1878(8) 0.116(7) Uiso 1 1 d . . . H214 H 0.3099 0.4343 0.1795 0.139 Uiso 1 1 calc R . . C158 C 0.0092(8) 0.0957(6) -0.1359(6) 0.073(5) Uiso 1 1 d . . . H158 H -0.0313 0.0956 -0.1546 0.087 Uiso 1 1 calc R . . C114 C 0.2368(9) 0.7238(6) 0.2704(7) 0.087(5) Uiso 1 1 d . . . H114 H 0.2726 0.7358 0.2451 0.104 Uiso 1 1 calc R . . C115 C 0.1691(9) 0.7307(6) 0.2539(7) 0.090(6) Uiso 1 1 d . . . H115 H 0.1600 0.7488 0.2169 0.108 Uiso 1 1 calc R . . C255 C 0.8533(8) 0.3671(7) -0.0495(7) 0.090(6) Uiso 1 1 d . . . H255 H 0.8709 0.3883 -0.0836 0.108 Uiso 1 1 calc R . . C69 C 0.4350(7) 0.9287(6) 0.3618(6) 0.062(5) Uiso 1 1 d . . . H69 H 0.4544 0.8960 0.3871 0.074 Uiso 1 1 calc R . . C194 C 0.4589(9) -0.1135(6) 0.0461(7) 0.089(6) Uiso 1 1 d . . . H194 H 0.4823 -0.1056 0.0135 0.107 Uiso 1 1 calc R . . C146 C -0.1384(8) -0.0060(6) 0.1615(6) 0.073(5) Uiso 1 1 d . . . H146 H -0.1747 -0.0226 0.1521 0.087 Uiso 1 1 calc R . . C107 C 0.3168(8) 0.6488(7) 0.5005(6) 0.079(5) Uiso 1 1 d . . . H107 H 0.3066 0.6126 0.5211 0.095 Uiso 1 1 calc R . . C15 C 0.7719(9) 1.0550(7) 0.2564(7) 0.091(6) Uiso 1 1 d . . . H15 H 0.8030 1.0387 0.2399 0.110 Uiso 1 1 calc R . . C258 C 0.7973(8) 0.3055(7) 0.0490(7) 0.086(5) Uiso 1 1 d . . . H258 H 0.7781 0.2833 0.0821 0.103 Uiso 1 1 calc R . . C147 C -0.1074(8) -0.0315(6) 0.2108(6) 0.073(5) Uiso 1 1 d . . . H147 H -0.1212 -0.0660 0.2341 0.088 Uiso 1 1 calc R . . C117 C 0.1266(9) 0.6870(6) 0.3454(7) 0.084(5) Uiso 1 1 d . . . H117 H 0.0900 0.6755 0.3700 0.101 Uiso 1 1 calc R . . C266 C 0.5828(8) 0.4362(6) -0.0089(6) 0.071(5) Uiso 1 1 d . . . H266 H 0.5901 0.4668 -0.0017 0.085 Uiso 1 1 calc R . . C228 C 1.0060(9) 0.3180(7) 0.2979(7) 0.095(6) Uiso 1 1 d . . . H228 H 1.0518 0.3044 0.3065 0.114 Uiso 1 1 calc R . . C229 C 0.9610(9) 0.3038(7) 0.3374(7) 0.094(6) Uiso 1 1 d . . . H229 H 0.9761 0.2820 0.3726 0.113 Uiso 1 1 calc R . . C11 C 0.6638(8) 1.2228(7) 0.3776(6) 0.079(5) Uiso 1 1 d . . . H11 H 0.6700 1.2594 0.3556 0.095 Uiso 1 1 calc R . . C29 C 0.5776(8) 0.8810(6) 0.6629(7) 0.076(5) Uiso 1 1 d . . . H29 H 0.5779 0.8640 0.7007 0.091 Uiso 1 1 calc R . . C12 C 0.7104(8) 1.1803(6) 0.3759(6) 0.070(5) Uiso 1 1 d . . . H12 H 0.7489 1.1895 0.3530 0.084 Uiso 1 1 calc R . . C226 C 0.9198(8) 0.3690(6) 0.2322(6) 0.075(5) Uiso 1 1 d . . . H226 H 0.9069 0.3916 0.1967 0.090 Uiso 1 1 calc R . . C191 C 0.1957(9) -0.1180(7) 0.1908(7) 0.097(6) Uiso 1 1 d . . . H191 H 0.1692 -0.1354 0.1743 0.116 Uiso 1 1 calc R . . C270 C 0.6195(9) 0.3469(7) -0.0006(6) 0.092(6) Uiso 1 1 d . . . H270 H 0.6513 0.3171 0.0116 0.110 Uiso 1 1 calc R . . C230 C 0.8887(9) 0.3210(6) 0.3277(7) 0.076(5) Uiso 1 1 d . . . C21 C 0.8611(8) 0.8562(7) 0.6564(6) 0.083(5) Uiso 1 1 d . . . H21 H 0.8897 0.8753 0.6697 0.100 Uiso 1 1 calc R . . C179 C 0.4935(9) 0.1425(6) 0.1155(6) 0.089(6) Uiso 1 1 d . . . H179 H 0.5276 0.1319 0.0963 0.107 Uiso 1 1 calc R . . C142 C -0.0731(8) 0.1576(7) 0.1959(6) 0.076(5) Uiso 1 1 d . . . H142 H -0.1037 0.1301 0.2002 0.092 Uiso 1 1 calc R . . C98 C 0.2875(8) 0.6584(6) 0.1506(6) 0.076(5) Uiso 1 1 d . . . H98 H 0.2593 0.6647 0.1205 0.091 Uiso 1 1 calc R . . C81 C -0.0710(8) 0.6367(6) 0.1840(6) 0.066(5) Uiso 1 1 d . . . H81 H -0.0961 0.6051 0.1996 0.079 Uiso 1 1 calc R . . C251 C 0.8148(9) 0.5266(6) 0.1657(7) 0.081(5) Uiso 1 1 d . . . H251 H 0.8556 0.5195 0.1501 0.097 Uiso 1 1 calc R . . C240 C 0.7006(9) 0.6212(7) 0.0291(7) 0.085(5) Uiso 1 1 d . . . C92 C 0.4325(8) 0.6183(6) 0.2780(6) 0.067(5) Uiso 1 1 d . . . H92 H 0.4200 0.5973 0.3136 0.081 Uiso 1 1 calc R . . C212 C 0.3955(8) 0.5369(7) 0.1741(6) 0.085(5) Uiso 1 1 d . . . H212 H 0.3941 0.5749 0.1579 0.101 Uiso 1 1 calc R . . C83 C 0.1312(8) 0.5109(6) 0.1886(6) 0.073(5) Uiso 1 1 d . . . H83 H 0.1667 0.5126 0.2110 0.088 Uiso 1 1 calc R . . C10 C 0.6098(8) 1.2070(7) 0.4131(6) 0.084(5) Uiso 1 1 d . . . H10 H 0.5793 1.2342 0.4151 0.101 Uiso 1 1 calc R . . C84 C 0.1429(9) 0.4821(7) 0.1553(7) 0.095(6) Uiso 1 1 d . . . H84 H 0.1853 0.4629 0.1575 0.114 Uiso 1 1 calc R . . C248 C 0.6940(10) 0.5462(7) 0.2134(8) 0.114(7) Uiso 1 1 d . . . H248 H 0.6533 0.5522 0.2297 0.137 Uiso 1 1 calc R . . C22 C 0.8584(8) 0.8010(7) 0.6814(6) 0.076(5) Uiso 1 1 d . . . H22 H 0.8867 0.7818 0.7115 0.091 Uiso 1 1 calc R . . C195 C 0.4877(10) -0.1493(7) 0.0951(8) 0.104(6) Uiso 1 1 d . . . H195 H 0.5323 -0.1644 0.0947 0.124 Uiso 1 1 calc R . . C213 C 0.3467(9) 0.5088(7) 0.1635(7) 0.087(6) Uiso 1 1 d . . . H213 H 0.3118 0.5279 0.1385 0.104 Uiso 1 1 calc R . . C16 C 0.7153(10) 1.0792(7) 0.2323(8) 0.106(6) Uiso 1 1 d . . . H16 H 0.7069 1.0794 0.1982 0.127 Uiso 1 1 calc R . . C238 C 0.9396(9) 0.5985(7) -0.0264(7) 0.097(6) Uiso 1 1 d . . . H238 H 0.9607 0.5903 -0.0537 0.117 Uiso 1 1 calc R . . C231 C 0.8404(9) 0.3125(7) 0.3652(7) 0.091(6) Uiso 1 1 d . . . H231 H 0.8546 0.2925 0.4010 0.110 Uiso 1 1 calc R . . C94 C 0.5189(10) 0.6654(7) 0.2139(8) 0.107(6) Uiso 1 1 d . . . H94 H 0.5645 0.6766 0.2059 0.129 Uiso 1 1 calc R . . C267 C 0.5228(9) 0.4348(7) -0.0382(7) 0.095(6) Uiso 1 1 d . . . H267 H 0.4903 0.4641 -0.0507 0.114 Uiso 1 1 calc R . . C55 C 0.5672(9) 1.0001(7) 0.1087(7) 0.095(6) Uiso 1 1 d . . . H55 H 0.5739 1.0162 0.0713 0.114 Uiso 1 1 calc R . . C140 C -0.0576(10) 0.2486(8) 0.1815(7) 0.097(6) Uiso 1 1 d . . . H140 H -0.0767 0.2827 0.1770 0.117 Uiso 1 1 calc R . . C134 C 0.2022(10) 0.4129(7) 0.3259(8) 0.113(7) Uiso 1 1 d . . . H134 H 0.1929 0.4069 0.2949 0.135 Uiso 1 1 calc R . . C136 C 0.1719(10) 0.4016(7) 0.4168(8) 0.110(6) Uiso 1 1 d . . . H136 H 0.1436 0.3875 0.4473 0.132 Uiso 1 1 calc R . . C61 C 0.4658(11) 0.7516(8) 0.3124(7) 0.120(7) Uiso 1 1 d . . . H61 H 0.4513 0.7180 0.3145 0.144 Uiso 1 1 calc R . . C139 C 0.0136(10) 0.2418(8) 0.1809(7) 0.110(6) Uiso 1 1 d . . . H139 H 0.0428 0.2705 0.1754 0.132 Uiso 1 1 calc R . . C27 C 0.5196(8) 0.9373(6) 0.5834(6) 0.075(5) Uiso 1 1 d . . . H27 H 0.4805 0.9589 0.5661 0.090 Uiso 1 1 calc R . . C105 C 0.0896(8) 0.6155(6) 0.4957(6) 0.074(5) Uiso 1 1 d . . . H105 H 0.0987 0.5798 0.4992 0.088 Uiso 1 1 calc R . . C169 C 0.0674(9) 0.1871(7) 0.0290(7) 0.093(6) Uiso 1 1 d . . . H169 H 0.0201 0.1896 0.0363 0.111 Uiso 1 1 calc R . . C56 C 0.5080(9) 0.9756(6) 0.1272(7) 0.091(6) Uiso 1 1 d . . . H56 H 0.4731 0.9745 0.1040 0.109 Uiso 1 1 calc R . . C126 C 0.3680(9) 0.4262(7) 0.5362(7) 0.090(6) Uiso 1 1 d . . . H126 H 0.3489 0.4515 0.5489 0.108 Uiso 1 1 calc R . . C237 C 0.9692(9) 0.6336(7) -0.0085(7) 0.092(6) Uiso 1 1 d . . . H237 H 1.0120 0.6481 -0.0226 0.110 Uiso 1 1 calc R . . C199 C 0.2434(12) -0.1735(9) 0.0919(8) 0.140(8) Uiso 1 1 d . . . H199 H 0.2879 -0.1840 0.1067 0.168 Uiso 1 1 calc R . . C133 C 0.2570(9) 0.4409(7) 0.3250(7) 0.090(6) Uiso 1 1 d . . . H133 H 0.2863 0.4527 0.2950 0.108 Uiso 1 1 calc R . . C135 C 0.1576(11) 0.3917(8) 0.3686(8) 0.124(7) Uiso 1 1 d . . . H135 H 0.1197 0.3718 0.3670 0.149 Uiso 1 1 calc R . . C110 C 0.3478(9) 0.7566(7) 0.4375(7) 0.095(6) Uiso 1 1 d . . . H110 H 0.3603 0.7920 0.4158 0.114 Uiso 1 1 calc R . . C109 C 0.3810(10) 0.7283(8) 0.4835(8) 0.108(6) Uiso 1 1 d . . . H109 H 0.4148 0.7461 0.4942 0.129 Uiso 1 1 calc R . . C202 C 0.1108(10) -0.1441(8) 0.0429(7) 0.100(6) Uiso 1 1 d . . . H202 H 0.0681 -0.1318 0.0251 0.120 Uiso 1 1 calc R . . C101 C 0.1214(9) 0.7076(7) 0.4645(7) 0.094(6) Uiso 1 1 d . . . H101 H 0.1533 0.7344 0.4473 0.112 Uiso 1 1 calc R . . C104 C 0.0280(9) 0.6278(7) 0.5191(7) 0.099(6) Uiso 1 1 d . . . H104 H -0.0032 0.6009 0.5378 0.118 Uiso 1 1 calc R . . C157 C 0.0565(8) 0.1340(6) -0.1608(6) 0.075(5) Uiso 1 1 d . . . H157 H 0.0496 0.1583 -0.1967 0.090 Uiso 1 1 calc R . . C203 C 0.1535(9) -0.1085(7) 0.0564(6) 0.087(6) Uiso 1 1 d . . . H203 H 0.1356 -0.0732 0.0484 0.104 Uiso 1 1 calc R . . C152 C 0.0699(8) -0.0060(6) 0.3921(7) 0.073(5) Uiso 1 1 d . . . H152 H 0.0775 -0.0230 0.4294 0.088 Uiso 1 1 calc R . . C116 C 0.1136(10) 0.7131(7) 0.2876(7) 0.099(6) Uiso 1 1 d . . . H116 H 0.0683 0.7177 0.2738 0.119 Uiso 1 1 calc R . . C111 C 0.2919(9) 0.7318(7) 0.4211(7) 0.095(6) Uiso 1 1 d . . . H111 H 0.2649 0.7515 0.3904 0.114 Uiso 1 1 calc R . . C127 C 0.4319(9) 0.3994(7) 0.5556(7) 0.100(6) Uiso 1 1 d . . . H127 H 0.4556 0.4071 0.5815 0.120 Uiso 1 1 calc R . . C227 C 0.9914(10) 0.3513(7) 0.2445(8) 0.107(6) Uiso 1 1 d . . . H227 H 1.0260 0.3617 0.2180 0.128 Uiso 1 1 calc R . . C141 C -0.1011(10) 0.2087(8) 0.1883(7) 0.105(6) Uiso 1 1 d . . . H141 H -0.1493 0.2151 0.1880 0.126 Uiso 1 1 calc R . . C74 C -0.0568(9) 0.4400(7) 0.3366(7) 0.097(6) Uiso 1 1 d . . . H74 H -0.0531 0.4021 0.3485 0.116 Uiso 1 1 calc R . . C36 C 0.6211(8) 0.8423(6) 0.4951(6) 0.083(5) Uiso 1 1 d . . . H36 H 0.5838 0.8600 0.5048 0.100 Uiso 1 1 calc R . . C32 C 0.7428(8) 0.8189(6) 0.4951(6) 0.080(5) Uiso 1 1 d . . . H32 H 0.7889 0.8205 0.5047 0.096 Uiso 1 1 calc R . . C219 C 0.5359(9) 0.4835(6) 0.4099(7) 0.092(6) Uiso 1 1 d . . . H219 H 0.5378 0.4946 0.4385 0.110 Uiso 1 1 calc R . . C208 C 0.4244(9) 0.2825(8) 0.3849(7) 0.105(6) Uiso 1 1 d . . . H208 H 0.3957 0.2736 0.4152 0.126 Uiso 1 1 calc R . . C62 C 0.4186(9) 0.7931(7) 0.3029(6) 0.087(6) Uiso 1 1 d . . . H62 H 0.3716 0.7880 0.2992 0.104 Uiso 1 1 calc R . . C207 C 0.4384(9) 0.2462(7) 0.3630(7) 0.098(6) Uiso 1 1 d . . . H207 H 0.4195 0.2118 0.3791 0.118 Uiso 1 1 calc R . . C124 C 0.2071(11) 0.3517(8) 0.5553(8) 0.122(7) Uiso 1 1 d . . . H124 H 0.2509 0.3377 0.5507 0.147 Uiso 1 1 calc R . . C129 C 0.4258(9) 0.3493(7) 0.5000(7) 0.092(6) Uiso 1 1 d . . . H129 H 0.4445 0.3236 0.4877 0.110 Uiso 1 1 calc R . . C189 C 0.2183(10) -0.0985(8) 0.2663(8) 0.109(7) Uiso 1 1 d . . . H189 H 0.2095 -0.1040 0.3022 0.130 Uiso 1 1 calc R . . C245 C 0.6589(9) 0.6244(7) -0.0121(7) 0.104(6) Uiso 1 1 d . . . H245 H 0.6566 0.5952 -0.0224 0.124 Uiso 1 1 calc R . . C209 C 0.4536(9) 0.3345(7) 0.3615(7) 0.100(6) Uiso 1 1 d . . . H209 H 0.4448 0.3595 0.3771 0.119 Uiso 1 1 calc R . . C128 C 0.4624(9) 0.3606(7) 0.5375(7) 0.095(6) Uiso 1 1 d . . . H128 H 0.5057 0.3434 0.5505 0.114 Uiso 1 1 calc R . . C244 C 0.6154(10) 0.6773(8) -0.0415(8) 0.116(7) Uiso 1 1 d . . . H244 H 0.5844 0.6815 -0.0694 0.140 Uiso 1 1 calc R . . C268 C 0.5143(9) 0.3893(7) -0.0473(7) 0.091(6) Uiso 1 1 d . . . H268 H 0.4752 0.3887 -0.0671 0.109 Uiso 1 1 calc R . . C218 C 0.5959(10) 0.4709(7) 0.3900(8) 0.115(7) Uiso 1 1 d . . . H218 H 0.6386 0.4748 0.4038 0.138 Uiso 1 1 calc R . . C79 C -0.0692(10) 0.7334(8) 0.1318(7) 0.111(7) Uiso 1 1 d . . . H79 H -0.0925 0.7665 0.1116 0.133 Uiso 1 1 calc R . . C102 C 0.0596(10) 0.7210(8) 0.4863(7) 0.112(7) Uiso 1 1 d . . . H102 H 0.0488 0.7567 0.4823 0.135 Uiso 1 1 calc R . . C17 C 0.6658(11) 1.1049(8) 0.2521(8) 0.122(7) Uiso 1 1 d . . . H17 H 0.6259 1.1223 0.2323 0.146 Uiso 1 1 calc R . . C269 C 0.5572(10) 0.3459(8) -0.0304(7) 0.111(6) Uiso 1 1 d . . . H269 H 0.5479 0.3154 -0.0373 0.133 Uiso 1 1 calc R . . C4 C 0.9668(9) 1.1493(7) 0.3981(7) 0.095(6) Uiso 1 1 d . . . H4 H 1.0084 1.1656 0.3991 0.114 Uiso 1 1 calc R . . C201 C 0.1350(12) -0.1959(9) 0.0571(8) 0.139(8) Uiso 1 1 d . . . H201 H 0.1083 -0.2211 0.0509 0.167 Uiso 1 1 calc R . . C243 C 0.6249(10) 0.7166(9) -0.0246(9) 0.128(7) Uiso 1 1 d . . . H243 H 0.6071 0.7512 -0.0468 0.153 Uiso 1 1 calc R . . C108 C 0.3693(9) 0.6729(7) 0.5185(7) 0.100(6) Uiso 1 1 d . . . H108 H 0.3944 0.6542 0.5505 0.120 Uiso 1 1 calc R . . C249 C 0.7522(11) 0.5230(7) 0.2429(8) 0.115(7) Uiso 1 1 d . . . H249 H 0.7501 0.5135 0.2802 0.138 Uiso 1 1 calc R . . C78 C 0.0015(11) 0.7327(8) 0.1417(8) 0.120(7) Uiso 1 1 d . . . H78 H 0.0255 0.7649 0.1287 0.144 Uiso 1 1 calc R . . C95 C 0.4713(10) 0.6816(7) 0.1730(8) 0.106(6) Uiso 1 1 d . . . H95 H 0.4849 0.7033 0.1378 0.127 Uiso 1 1 calc R . . C257 C 0.8502(9) 0.2843(8) 0.0222(8) 0.114(7) Uiso 1 1 d . . . H257 H 0.8662 0.2480 0.0392 0.136 Uiso 1 1 calc R . . C241 C 0.7036(11) 0.6642(9) 0.0460(9) 0.140(8) Uiso 1 1 d . . . H241 H 0.7353 0.6617 0.0728 0.168 Uiso 1 1 calc R . . C77 C 0.0367(9) 0.6819(7) 0.1722(6) 0.090(6) Uiso 1 1 d . . . H77 H 0.0847 0.6807 0.1778 0.108 Uiso 1 1 calc R . . C263 C 0.6074(9) 0.2838(7) 0.1860(7) 0.091(6) Uiso 1 1 d . . . H263 H 0.5624 0.2726 0.1968 0.109 Uiso 1 1 calc R . . C190 C 0.1818(11) -0.1248(9) 0.2454(9) 0.139(8) Uiso 1 1 d . . . H190 H 0.1471 -0.1477 0.2655 0.167 Uiso 1 1 calc R . . C242 C 0.6583(12) 0.7121(10) 0.0223(10) 0.161(9) Uiso 1 1 d . . . H242 H 0.6520 0.7379 0.0373 0.193 Uiso 1 1 calc R . . C262 C 0.6612(9) 0.2642(7) 0.2214(7) 0.098(6) Uiso 1 1 d . . . H262 H 0.6516 0.2392 0.2563 0.118 Uiso 1 1 calc R . . C200 C 0.2018(15) -0.2115(11) 0.0816(10) 0.190(11) Uiso 1 1 d . . . H200 H 0.2191 -0.2473 0.0913 0.228 Uiso 1 1 calc R . . C121 C 0.0796(9) 0.3919(7) 0.5759(7) 0.089(6) Uiso 1 1 d . . . H121 H 0.0376 0.4063 0.5833 0.106 Uiso 1 1 calc R . . C122 C 0.0962(10) 0.3395(8) 0.6014(8) 0.118(7) Uiso 1 1 d . . . H122 H 0.0654 0.3170 0.6268 0.142 Uiso 1 1 calc R . . C123 C 0.1573(11) 0.3174(9) 0.5915(8) 0.130(7) Uiso 1 1 d . . . H123 H 0.1666 0.2798 0.6084 0.156 Uiso 1 1 calc R . . C34 C 0.6602(9) 0.7839(7) 0.4552(7) 0.090(6) Uiso 1 1 d . . . H34 H 0.6494 0.7611 0.4381 0.108 Uiso 1 1 calc R . . C33 C 0.7266(10) 0.7854(7) 0.4652(7) 0.110(6) Uiso 1 1 d . . . H33 H 0.7612 0.7666 0.4541 0.131 Uiso 1 1 calc R . . C35 C 0.6091(10) 0.8091(7) 0.4656(7) 0.097(6) Uiso 1 1 d . . . H35 H 0.5642 0.8062 0.4544 0.116 Uiso 1 1 calc R . . C173 C 0.3316(8) 0.0372(6) 0.0195(5) 0.043(4) Uani 1 1 d . . . C252 C 0.8255(9) 0.4545(6) 0.0632(6) 0.053(5) Uani 1 1 d . . . C118 C 0.3319(8) 0.5547(5) 0.4498(5) 0.043(4) Uiso 1 1 d . . . C39 C 0.8329(8) 0.9630(6) 0.4740(5) 0.046(4) Uani 1 1 d . . . O1 O 0.8930(6) 0.9483(4) 0.4784(4) 0.071(3) Uani 1 1 d . . . O4 O 0.3918(5) 0.5623(4) 0.4448(4) 0.080(3) Uani 1 1 d . . . O7 O 0.3897(6) 0.0509(4) 0.0150(4) 0.080(4) Uani 1 1 d . . . O10 O 0.8841(6) 0.4373(5) 0.0714(5) 0.086(4) 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 Pd2 0.0522(8) 0.0586(9) 0.0347(8) -0.0168(7) 0.0013(6) -0.0040(7) Pd4 0.0410(8) 0.0571(9) 0.0376(8) -0.0122(7) 0.0000(6) -0.0011(7) Pd3 0.0416(8) 0.0517(8) 0.0384(8) -0.0224(7) 0.0036(6) -0.0048(6) Pd1 0.0417(8) 0.0558(8) 0.0410(8) -0.0240(7) -0.0012(6) -0.0002(6) Ru1 0.0386(9) 0.0535(9) 0.0393(8) -0.0206(7) -0.0005(6) -0.0006(7) Ru2 0.0481(9) 0.0684(10) 0.0421(9) -0.0241(8) 0.0020(7) -0.0085(7) Ru4 0.0425(9) 0.0677(10) 0.0457(9) -0.0207(8) 0.0011(7) -0.0036(7) Ru3 0.0395(9) 0.0514(9) 0.0398(8) -0.0208(7) 0.0033(6) -0.0067(7) P7 0.045(3) 0.057(3) 0.047(3) -0.022(2) 0.004(2) -0.001(2) P3 0.050(3) 0.061(3) 0.039(3) -0.023(2) 0.004(2) -0.006(2) P9 0.049(3) 0.052(3) 0.047(3) -0.021(2) 0.004(2) -0.002(2) P6 0.053(3) 0.067(3) 0.047(3) -0.022(3) 0.005(2) -0.013(2) P8 0.040(3) 0.055(3) 0.053(3) -0.023(2) 0.000(2) -0.009(2) P11 0.042(3) 0.065(3) 0.065(3) -0.019(3) -0.001(2) -0.001(2) Cl1 0.062(3) 0.071(3) 0.048(3) -0.032(2) -0.003(2) 0.001(2) P2 0.048(3) 0.052(3) 0.057(3) -0.024(2) -0.002(2) 0.001(2) Cl2 0.058(3) 0.093(3) 0.044(3) -0.029(2) 0.004(2) -0.010(2) O2 0.049(6) 0.056(7) 0.050(6) -0.034(6) -0.006(5) -0.004(5) P1 0.053(3) 0.050(3) 0.045(3) -0.019(2) 0.001(2) -0.004(2) P12 0.035(3) 0.078(3) 0.045(3) -0.026(3) 0.004(2) -0.005(2) P4 0.056(3) 0.057(3) 0.042(3) -0.016(2) 0.000(2) 0.000(2) Cl4 0.068(3) 0.081(3) 0.049(3) -0.020(2) 0.009(2) -0.012(2) O12 0.049(6) 0.090(8) 0.025(7) -0.007(6) 0.000(5) 0.008(6) Cl3 0.051(3) 0.072(3) 0.051(3) -0.032(2) -0.002(2) -0.004(2) P10 0.046(3) 0.055(3) 0.048(3) -0.016(2) 0.000(2) -0.007(2) P5 0.059(3) 0.075(3) 0.044(3) -0.024(3) 0.000(2) -0.007(3) O9 0.043(6) 0.060(7) 0.057(7) -0.039(6) 0.002(5) -0.011(5) O3 0.043(7) 0.091(8) 0.076(8) -0.055(6) -0.005(5) 0.002(6) O11 0.054(7) 0.100(8) 0.039(7) -0.015(6) -0.007(5) 0.007(6) O8 0.043(7) 0.084(8) 0.082(8) -0.051(7) 0.010(6) -0.010(6) O5 0.068(8) 0.095(8) 0.038(7) -0.018(6) 0.014(5) -0.021(7) O6 0.070(7) 0.082(8) 0.029(7) -0.018(6) 0.016(5) -0.014(6) C223 0.040(11) 0.053(11) 0.056(12) -0.026(9) 0.000(8) -0.008(8) C89 0.027(10) 0.070(12) 0.078(13) -0.030(10) -0.004(9) -0.015(9) C173 0.016(10) 0.094(13) 0.025(9) -0.031(9) 0.003(8) 0.004(10) C252 0.048(12) 0.070(12) 0.056(12) -0.042(10) 0.028(10) -0.017(10) C39 0.020(10) 0.105(14) 0.021(9) -0.034(9) -0.006(8) 0.004(10) O1 0.040(7) 0.092(9) 0.076(8) -0.028(7) -0.004(6) 0.000(7) O4 0.041(7) 0.111(9) 0.110(9) -0.068(8) 0.007(6) -0.010(6) O7 0.045(8) 0.106(10) 0.085(9) -0.034(7) 0.004(7) -0.020(7) O10 0.049(8) 0.119(11) 0.103(10) -0.059(8) 0.003(8) 0.002(8) _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 Pd2 N4 1.994(10) . ? Pd2 N6 2.002(11) . ? Pd2 O5 2.021(9) . ? Pd2 P4 2.260(4) . ? Pd4 N12 1.979(11) . ? Pd4 N10 2.011(10) . ? Pd4 O11 2.011(9) . ? Pd4 P10 2.277(4) . ? Pd3 N7 1.964(10) . ? Pd3 O8 1.996(9) . ? Pd3 N9 2.008(10) . ? Pd3 P7 2.262(4) . ? Pd1 N1 1.966(10) . ? Pd1 O3 1.994(9) . ? Pd1 N3 2.013(10) . ? Pd1 P3 2.281(4) . ? Ru1 C39 1.763(15) . ? Ru1 N2 2.054(10) . ? Ru1 O2 2.222(8) . ? Ru1 P1 2.381(4) . ? Ru1 P2 2.392(4) . ? Ru1 Cl1 2.413(4) . ? Ru2 C118 1.818(16) . ? Ru2 N5 2.070(11) . ? Ru2 O6 2.217(9) . ? Ru2 P5 2.379(4) . ? Ru2 P6 2.400(4) . ? Ru2 Cl2 2.410(4) . ? Ru2 C88 2.578(15) . ? Ru4 C252 1.802(17) . ? Ru4 N11 2.059(10) . ? Ru4 O12 2.210(8) . ? Ru4 P12 2.386(4) . ? Ru4 P11 2.388(4) . ? Ru4 Cl4 2.418(4) . ? Ru4 C222 2.556(15) . ? Ru3 C173 1.782(15) . ? Ru3 N8 2.078(10) . ? Ru3 O9 2.225(8) . ? Ru3 P8 2.387(4) . ? Ru3 P9 2.397(4) . ? Ru3 Cl3 2.403(4) . ? Ru3 C174 2.578(15) . ? P7 C143 1.789(14) . ? P7 C137 1.791(13) . ? P7 C149 1.801(14) . ? P3 C58 1.791(14) . ? P3 C64 1.801(13) . ? P3 C52 1.803(14) . ? P9 C198 1.776(15) . ? P9 C192 1.811(14) . ? P9 C186 1.815(14) . ? P6 C125 1.816(14) . ? P6 C131 1.830(15) . ? P6 C119 1.833(15) . ? P8 C155 1.826(14) . ? P8 C161 1.828(14) . ? P8 C167 1.847(14) . ? P11 C240 1.831(17) . ? P11 C234 1.868(14) . ? P11 C246 1.880(15) . ? P2 C31 1.805(15) . ? P2 C25 1.830(14) . ? P2 C19 1.839(14) . ? O2 C40 1.299(14) . ? P1 C13 1.823(14) . ? P1 C1 1.824(14) . ? P1 C7 1.835(14) . ? C246 C251 1.319(17) . ? C246 C247 1.397(18) . ? P12 C265 1.841(15) . ? P12 C259 1.846(14) . ? P12 C253 1.860(14) . ? P4 C82 1.777(14) . ? P4 C70 1.781(14) . ? P4 C76 1.797(15) . ? O12 C222 1.278(14) . ? N6 C89 1.278(14) . ? N6 N5 1.373(12) . ? N4 C88 1.317(15) . ? P10 C204 1.775(14) . ? P10 C216 1.788(14) . ? P10 C210 1.792(14) . ? P5 C100 1.840(15) . ? P5 C112 1.846(15) . ? P5 C106 1.852(16) . ? O9 C174 1.251(14) . ? N9 C175 1.299(13) . ? N9 N8 1.375(12) . ? O3 C51 1.319(15) . ? O11 C233 1.320(16) . ? N12 C223 1.307(14) . ? N12 N11 1.395(13) . ? O8 C185 1.300(15) . ? N1 C40 1.318(15) . ? C156 C155 1.378(16) . ? C156 C157 1.429(17) . ? C137 C142 1.373(17) . ? C137 C138 1.376(17) . ? N7 C174 1.329(15) . ? O5 C99 1.306(16) . ? C149 C150 1.393(16) . ? C149 C154 1.395(16) . ? O6 C88 1.279(14) . ? C259 C260 1.392(16) . ? C259 C264 1.404(17) . ? N11 C222 1.336(14) . ? N5 C88 1.369(14) . ? C223 C224 1.428(17) . ? C82 C83 1.393(16) . ? C82 C87 1.418(17) . ? C176 C185 1.414(16) . ? C176 C175 1.433(16) . ? C176 C177 1.453(17) . ? C185 C184 1.441(17) . ? C30 C25 1.368(16) . ? C30 C29 1.416(17) . ? C25 C26 1.383(17) . ? C222 N10 1.335(15) . ? C113 C114 1.383(18) . ? C113 C112 1.427(18) . ? C19 C20 1.343(16) . ? C19 C24 1.391(17) . ? C112 C117 1.389(18) . ? C89 C90 1.491(17) . ? C155 C160 1.380(16) . ? C52 C53 1.352(16) . ? C52 C57 1.374(16) . ? C6 C5 1.387(18) . ? C6 C1 1.390(17) . ? C125 C130 1.385(17) . ? C125 C126 1.414(18) . ? C58 C63 1.383(17) . ? C58 C59 1.394(17) . ? C239 C234 1.368(17) . ? C239 C238 1.429(19) . ? C100 C105 1.343(17) . ? C100 C101 1.411(18) . ? C247 C248 1.42(2) . ? C186 C187 1.362(16) . ? C186 C191 1.396(18) . ? C168 C167 1.372(16) . ? C168 C169 1.396(18) . ? N8 C174 1.365(14) . ? C57 C56 1.446(18) . ? C13 C18 1.380(18) . ? C13 C14 1.392(16) . ? C40 N2 1.376(14) . ? C210 C215 1.379(18) . ? C210 C211 1.403(17) . ? N3 C41 1.281(14) . ? N3 N2 1.365(12) . ? C253 C258 1.355(17) . ? C253 C254 1.360(17) . ? C41 C42 1.465(16) . ? C53 C54 1.464(19) . ? C59 C60 1.374(19) . ? C143 C148 1.382(16) . ? C143 C144 1.428(16) . ? C192 C193 1.379(17) . ? C192 C197 1.412(17) . ? C90 C99 1.382(17) . ? C90 C91 1.461(17) . ? C235 C234 1.368(17) . ? C235 C236 1.404(18) . ? C154 C153 1.436(18) . ? C221 C216 1.357(17) . ? C221 C220 1.431(18) . ? C51 C42 1.405(17) . ? C51 C50 1.447(17) . ? C224 C233 1.377(17) . ? C224 C225 1.466(18) . ? C63 C62 1.379(18) . ? C233 C232 1.437(18) . ? C216 C217 1.386(17) . ? C24 C23 1.396(18) . ? C167 C172 1.434(17) . ? C172 C171 1.407(18) . ? C87 C86 1.391(17) . ? C86 C85 1.384(18) . ? C177 C178 1.411(17) . ? C177 C182 1.456(18) . ? C197 C196 1.446(18) . ? C161 C166 1.393(16) . ? C161 C162 1.398(17) . ? C220 C219 1.315(18) . ? C260 C261 1.381(17) . ? C31 C32 1.374(17) . ? C31 C36 1.425(18) . ? C42 C43 1.443(16) . ? C205 C206 1.377(18) . ? C205 C204 1.391(16) . ? C206 C207 1.371(19) . ? C204 C209 1.378(18) . ? C254 C255 1.409(18) . ? C1 C2 1.371(17) . ? C236 C237 1.329(18) . ? C131 C136 1.386(19) . ? C131 C132 1.397(18) . ? C166 C165 1.409(18) . ? C106 C107 1.370(18) . ? C106 C111 1.387(19) . ? C130 C129 1.404(18) . ? C183 C184 1.338(16) . ? C183 C182 1.396(17) . ? C182 C181 1.420(18) . ? C264 C263 1.383(18) . ? C181 C180 1.344(18) . ? C171 C170 1.319(18) . ? C70 C75 1.394(17) . ? C70 C71 1.406(16) . ? C23 C22 1.328(17) . ? C65 C64 1.379(16) . ? C65 C66 1.400(17) . ? C47 C46 1.342(18) . ? C47 C48 1.442(17) . ? C20 C21 1.401(18) . ? C45 C46 1.381(18) . ? C45 C44 1.413(18) . ? C170 C169 1.333(19) . ? C144 C145 1.379(16) . ? C64 C69 1.441(16) . ? C153 C152 1.340(17) . ? C162 C163 1.425(18) . ? C72 C73 1.348(18) . ? C72 C71 1.406(17) . ? C66 C67 1.358(17) . ? C193 C194 1.383(18) . ? C120 C119 1.338(17) . ? C120 C121 1.441(18) . ? C148 C147 1.423(17) . ? C225 C226 1.406(17) . ? C225 C230 1.423(18) . ? C73 C74 1.364(18) . ? C119 C124 1.38(2) . ? C165 C164 1.331(19) . ? C68 C67 1.328(17) . ? C68 C69 1.399(17) . ? C187 C188 1.389(18) . ? C85 C84 1.371(19) . ? C163 C164 1.345(18) . ? C8 C7 1.377(16) . ? C8 C9 1.401(18) . ? C178 C179 1.393(18) . ? C7 C12 1.387(17) . ? C217 C218 1.42(2) . ? C261 C262 1.364(19) . ? C150 C151 1.397(17) . ? C211 C212 1.412(18) . ? C60 C61 1.34(2) . ? C132 C133 1.413(19) . ? C75 C74 1.412(19) . ? C14 C15 1.418(19) . ? C9 C10 1.390(19) . ? C18 C17 1.45(2) . ? C160 C159 1.440(18) . ? C26 C27 1.430(18) . ? C265 C270 1.368(18) . ? C265 C266 1.385(17) . ? C54 C55 1.39(2) . ? C97 C96 1.327(18) . ? C97 C98 1.343(18) . ? C80 C79 1.39(2) . ? C80 C81 1.399(18) . ? C256 C257 1.310(19) . ? C256 C255 1.329(18) . ? C28 C27 1.326(17) . ? C28 C29 1.336(17) . ? C44 C43 1.391(17) . ? C93 C92 1.392(18) . ? C93 C94 1.40(2) . ? C49 C48 1.352(16) . ? C49 C50 1.377(17) . ? C5 C4 1.362(19) . ? C103 C104 1.350(19) . ? C103 C102 1.35(2) . ? C99 C98 1.462(18) . ? C250 C249 1.34(2) . ? C250 C251 1.420(19) . ? C3 C4 1.341(19) . ? C3 C2 1.414(18) . ? C96 C95 1.43(2) . ? C96 C91 1.452(18) . ? C91 C92 1.357(17) . ? C188 C189 1.35(2) . ? C151 C152 1.355(17) . ? C198 C203 1.340(18) . ? C198 C199 1.37(2) . ? C196 C195 1.375(19) . ? C76 C77 1.387(18) . ? C76 C81 1.392(17) . ? C232 C231 1.360(19) . ? C43 C48 1.422(16) . ? C180 C179 1.415(19) . ? C215 C214 1.45(2) . ? C145 C146 1.390(17) . ? C159 C158 1.353(17) . ? C138 C139 1.45(2) . ? C214 C213 1.38(2) . ? C158 C157 1.353(17) . ? C114 C115 1.357(19) . ? C115 C116 1.359(19) . ? C194 C195 1.38(2) . ? C146 C147 1.352(17) . ? C107 C108 1.406(19) . ? C15 C16 1.28(2) . ? C258 C257 1.46(2) . ? C117 C116 1.44(2) . ? C266 C267 1.411(19) . ? C228 C229 1.301(19) . ? C228 C227 1.38(2) . ? C229 C230 1.433(19) . ? C11 C10 1.358(18) . ? C11 C12 1.429(17) . ? C226 C227 1.430(19) . ? C191 C190 1.43(2) . ? C270 C269 1.45(2) . ? C230 C231 1.317(18) . ? C21 C22 1.357(18) . ? C142 C141 1.380(19) . ? C240 C245 1.35(2) . ? C240 C241 1.40(2) . ? C212 C213 1.327(18) . ? C83 C84 1.407(18) . ? C248 C249 1.35(2) . ? C16 C17 1.37(2) . ? C238 C237 1.360(19) . ? C94 C95 1.36(2) . ? C267 C268 1.349(19) . ? C55 C56 1.323(19) . ? C140 C141 1.33(2) . ? C140 C139 1.37(2) . ? C134 C133 1.31(2) . ? C134 C135 1.36(2) . ? C136 C135 1.45(2) . ? C61 C62 1.34(2) . ? C105 C104 1.418(19) . ? C126 C127 1.388(19) . ? C199 C200 1.43(3) . ? C110 C109 1.32(2) . ? C110 C111 1.44(2) . ? C109 C108 1.43(2) . ? C202 C201 1.34(2) . ? C202 C203 1.43(2) . ? C101 C102 1.41(2) . ? C127 C128 1.413(19) . ? C36 C35 1.434(19) . ? C32 C33 1.47(2) . ? C219 C218 1.35(2) . ? C208 C207 1.339(19) . ? C208 C209 1.41(2) . ? C124 C123 1.42(2) . ? C129 C128 1.372(19) . ? C189 C190 1.29(2) . ? C245 C244 1.53(2) . ? C244 C243 1.32(2) . ? C268 C269 1.32(2) . ? C79 C78 1.38(2) . ? C201 C200 1.41(3) . ? C243 C242 1.38(2) . ? C78 C77 1.42(2) . ? C241 C242 1.44(3) . ? C263 C262 1.348(19) . ? C121 C122 1.32(2) . ? C122 C123 1.36(2) . ? C34 C35 1.255(19) . ? C34 C33 1.31(2) . ? C173 O7 1.175(13) . ? C252 O10 1.185(15) . ? C118 O4 1.169(14) . ? C39 O1 1.191(13) . ? 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 N4 Pd2 N6 81.2(5) . . ? N4 Pd2 O5 172.4(4) . . ? N6 Pd2 O5 91.7(4) . . ? N4 Pd2 P4 94.0(3) . . ? N6 Pd2 P4 173.7(3) . . ? O5 Pd2 P4 93.2(3) . . ? N12 Pd4 N10 81.0(5) . . ? N12 Pd4 O11 90.4(4) . . ? N10 Pd4 O11 171.4(4) . . ? N12 Pd4 P10 176.8(4) . . ? N10 Pd4 P10 95.8(3) . . ? O11 Pd4 P10 92.8(3) . . ? N7 Pd3 O8 172.2(4) . . ? N7 Pd3 N9 80.8(4) . . ? O8 Pd3 N9 91.4(4) . . ? N7 Pd3 P7 94.9(3) . . ? O8 Pd3 P7 92.9(3) . . ? N9 Pd3 P7 175.2(3) . . ? N1 Pd1 O3 172.0(4) . . ? N1 Pd1 N3 80.4(4) . . ? O3 Pd1 N3 91.6(4) . . ? N1 Pd1 P3 96.1(3) . . ? O3 Pd1 P3 91.9(3) . . ? N3 Pd1 P3 175.7(3) . . ? C39 Ru1 N2 102.9(5) . . ? C39 Ru1 O2 163.9(4) . . ? N2 Ru1 O2 61.4(4) . . ? C39 Ru1 P1 95.3(5) . . ? N2 Ru1 P1 90.4(3) . . ? O2 Ru1 P1 82.0(2) . . ? C39 Ru1 P2 92.3(5) . . ? N2 Ru1 P2 91.2(3) . . ? O2 Ru1 P2 91.6(2) . . ? P1 Ru1 P2 171.74(14) . . ? C39 Ru1 Cl1 94.3(4) . . ? N2 Ru1 Cl1 162.8(3) . . ? O2 Ru1 Cl1 101.4(2) . . ? P1 Ru1 Cl1 88.34(13) . . ? P2 Ru1 Cl1 87.81(13) . . ? C118 Ru2 N5 104.7(5) . . ? C118 Ru2 O6 166.2(5) . . ? N5 Ru2 O6 61.7(4) . . ? C118 Ru2 P5 91.8(4) . . ? N5 Ru2 P5 88.8(3) . . ? O6 Ru2 P5 90.4(3) . . ? C118 Ru2 P6 95.3(4) . . ? N5 Ru2 P6 90.3(3) . . ? O6 Ru2 P6 83.0(3) . . ? P5 Ru2 P6 172.85(14) . . ? C118 Ru2 Cl2 93.5(4) . . ? N5 Ru2 Cl2 161.8(3) . . ? O6 Ru2 Cl2 100.1(2) . . ? P5 Ru2 Cl2 91.09(14) . . ? P6 Ru2 Cl2 87.47(14) . . ? C118 Ru2 C88 136.6(5) . . ? N5 Ru2 C88 31.9(4) . . ? O6 Ru2 C88 29.7(3) . . ? P5 Ru2 C88 90.1(3) . . ? P6 Ru2 C88 85.5(3) . . ? Cl2 Ru2 C88 129.9(4) . . ? C252 Ru4 N11 103.2(5) . . ? C252 Ru4 O12 164.5(5) . . ? N11 Ru4 O12 61.4(4) . . ? C252 Ru4 P12 89.9(5) . . ? N11 Ru4 P12 88.9(3) . . ? O12 Ru4 P12 91.2(3) . . ? C252 Ru4 P11 91.6(5) . . ? N11 Ru4 P11 89.5(3) . . ? O12 Ru4 P11 87.0(3) . . ? P12 Ru4 P11 178.03(14) . . ? C252 Ru4 Cl4 97.0(5) . . ? N11 Ru4 Cl4 159.7(3) . . ? O12 Ru4 Cl4 98.4(2) . . ? P12 Ru4 Cl4 90.22(14) . . ? P11 Ru4 Cl4 90.91(14) . . ? C252 Ru4 C222 134.6(6) . . ? N11 Ru4 C222 31.4(4) . . ? O12 Ru4 C222 30.0(3) . . ? P12 Ru4 C222 90.7(3) . . ? P11 Ru4 C222 87.3(3) . . ? Cl4 Ru4 C222 128.4(4) . . ? C173 Ru3 N8 103.6(5) . . ? C173 Ru3 O9 164.3(4) . . ? N8 Ru3 O9 60.8(3) . . ? C173 Ru3 P8 93.6(5) . . ? N8 Ru3 P8 91.1(3) . . ? O9 Ru3 P8 88.9(2) . . ? C173 Ru3 P9 95.5(5) . . ? N8 Ru3 P9 91.0(3) . . ? O9 Ru3 P9 83.5(2) . . ? P8 Ru3 P9 169.96(14) . . ? C173 Ru3 Cl3 94.0(4) . . ? N8 Ru3 Cl3 162.4(3) . . ? O9 Ru3 Cl3 101.6(2) . . ? P8 Ru3 Cl3 87.80(13) . . ? P9 Ru3 Cl3 87.29(13) . . ? C173 Ru3 C174 135.5(5) . . ? N8 Ru3 C174 31.9(4) . . ? O9 Ru3 C174 29.0(3) . . ? P8 Ru3 C174 88.7(3) . . ? P9 Ru3 C174 87.8(3) . . ? Cl3 Ru3 C174 130.6(4) . . ? C143 P7 C137 104.2(6) . . ? C143 P7 C149 106.0(6) . . ? C137 P7 C149 104.2(6) . . ? C143 P7 Pd3 112.3(4) . . ? C137 P7 Pd3 117.8(5) . . ? C149 P7 Pd3 111.3(5) . . ? C58 P3 C64 104.0(6) . . ? C58 P3 C52 104.5(6) . . ? C64 P3 C52 105.6(6) . . ? C58 P3 Pd1 117.2(5) . . ? C64 P3 Pd1 113.6(4) . . ? C52 P3 Pd1 110.9(5) . . ? C198 P9 C192 101.6(7) . . ? C198 P9 C186 105.5(7) . . ? C192 P9 C186 103.8(6) . . ? C198 P9 Ru3 112.3(5) . . ? C192 P9 Ru3 118.6(5) . . ? C186 P9 Ru3 113.5(4) . . ? C125 P6 C131 102.0(7) . . ? C125 P6 C119 103.3(7) . . ? C131 P6 C119 103.1(7) . . ? C125 P6 Ru2 117.4(5) . . ? C131 P6 Ru2 113.5(5) . . ? C119 P6 Ru2 115.7(5) . . ? C155 P8 C161 102.1(6) . . ? C155 P8 C167 101.4(6) . . ? C161 P8 C167 105.4(6) . . ? C155 P8 Ru3 115.1(5) . . ? C161 P8 Ru3 117.6(5) . . ? C167 P8 Ru3 113.3(4) . . ? C240 P11 C234 100.7(7) . . ? C240 P11 C246 104.0(7) . . ? C234 P11 C246 103.0(7) . . ? C240 P11 Ru4 121.6(6) . . ? C234 P11 Ru4 116.2(5) . . ? C246 P11 Ru4 109.3(5) . . ? C31 P2 C25 106.6(6) . . ? C31 P2 C19 103.2(7) . . ? C25 P2 C19 100.1(7) . . ? C31 P2 Ru1 111.5(5) . . ? C25 P2 Ru1 113.7(5) . . ? C19 P2 Ru1 120.1(5) . . ? C40 O2 Ru1 91.7(8) . . ? C13 P1 C1 105.0(7) . . ? C13 P1 C7 103.3(6) . . ? C1 P1 C7 101.5(6) . . ? C13 P1 Ru1 112.5(5) . . ? C1 P1 Ru1 117.4(5) . . ? C7 P1 Ru1 115.5(5) . . ? C251 C246 C247 121.4(16) . . ? C251 C246 P11 121.3(12) . . ? C247 C246 P11 116.9(13) . . ? C265 P12 C259 103.6(6) . . ? C265 P12 C253 102.6(6) . . ? C259 P12 C253 103.8(6) . . ? C265 P12 Ru4 116.7(5) . . ? C259 P12 Ru4 112.9(4) . . ? C253 P12 Ru4 115.7(5) . . ? C82 P4 C70 105.2(7) . . ? C82 P4 C76 107.8(7) . . ? C70 P4 C76 104.4(7) . . ? C82 P4 Pd2 113.1(5) . . ? C70 P4 Pd2 111.3(5) . . ? C76 P4 Pd2 114.4(5) . . ? C222 O12 Ru4 90.2(8) . . ? C89 N6 N5 119.9(12) . . ? C89 N6 Pd2 129.0(10) . . ? N5 N6 Pd2 111.1(8) . . ? C88 N4 Pd2 113.0(10) . . ? C204 P10 C216 107.3(6) . . ? C204 P10 C210 102.7(6) . . ? C216 P10 C210 104.6(7) . . ? C204 P10 Pd4 113.1(5) . . ? C216 P10 Pd4 114.8(5) . . ? C210 P10 Pd4 113.4(5) . . ? C100 P5 C112 102.6(7) . . ? C100 P5 C106 101.7(7) . . ? C112 P5 C106 104.3(7) . . ? C100 P5 Ru2 115.8(5) . . ? C112 P5 Ru2 111.7(5) . . ? C106 P5 Ru2 118.9(5) . . ? C174 O9 Ru3 91.3(8) . . ? C175 N9 N8 121.5(10) . . ? C175 N9 Pd3 127.4(9) . . ? N8 N9 Pd3 111.1(7) . . ? C51 O3 Pd1 125.2(9) . . ? C233 O11 Pd4 123.8(9) . . ? C223 N12 N11 118.3(11) . . ? C223 N12 Pd4 128.9(10) . . ? N11 N12 Pd4 112.8(9) . . ? C185 O8 Pd3 124.5(9) . . ? C40 N1 Pd1 113.4(10) . . ? C155 C156 C157 119.5(14) . . ? C142 C137 C138 116.6(14) . . ? C142 C137 P7 125.3(12) . . ? C138 C137 P7 118.1(11) . . ? C174 N7 Pd3 114.9(10) . . ? C99 O5 Pd2 122.9(9) . . ? C150 C149 C154 119.4(13) . . ? C150 C149 P7 122.0(11) . . ? C154 C149 P7 118.7(11) . . ? C88 O6 Ru2 91.0(8) . . ? C260 C259 C264 118.2(13) . . ? C260 C259 P12 119.8(11) . . ? C264 C259 P12 121.7(11) . . ? C222 N11 N12 114.7(12) . . ? C222 N11 Ru4 95.3(9) . . ? N12 N11 Ru4 149.8(9) . . ? C88 N5 N6 116.8(12) . . ? C88 N5 Ru2 95.0(9) . . ? N6 N5 Ru2 148.2(9) . . ? N12 C223 C224 124.9(13) . . ? C83 C82 C87 117.0(13) . . ? C83 C82 P4 121.8(11) . . ? C87 C82 P4 121.2(11) . . ? C185 C176 C175 122.0(13) . . ? C185 C176 C177 119.8(13) . . ? C175 C176 C177 118.1(13) . . ? O8 C185 C176 129.3(13) . . ? O8 C185 C184 113.2(13) . . ? C176 C185 C184 117.4(14) . . ? C25 C30 C29 119.9(14) . . ? C30 C25 C26 118.1(14) . . ? C30 C25 P2 122.7(12) . . ? C26 C25 P2 119.3(12) . . ? O12 C222 N10 126.8(13) . . ? O12 C222 N11 113.1(13) . . ? N10 C222 N11 120.1(14) . . ? O12 C222 Ru4 59.8(7) . . ? N10 C222 Ru4 173.4(12) . . ? N11 C222 Ru4 53.3(7) . . ? C114 C113 C112 119.1(15) . . ? C20 C19 C24 118.7(14) . . ? C20 C19 P2 120.2(11) . . ? C24 C19 P2 120.8(12) . . ? C117 C112 C113 121.3(15) . . ? C117 C112 P5 118.0(12) . . ? C113 C112 P5 120.4(12) . . ? N6 C89 C90 122.7(13) . . ? C156 C155 C160 119.6(14) . . ? C156 C155 P8 122.1(11) . . ? C160 C155 P8 118.3(11) . . ? C53 C52 C57 120.9(14) . . ? C53 C52 P3 118.7(11) . . ? C57 C52 P3 120.3(11) . . ? C5 C6 C1 119.3(15) . . ? C130 C125 C126 119.7(15) . . ? C130 C125 P6 123.6(12) . . ? C126 C125 P6 116.6(12) . . ? O6 C88 N4 130.0(13) . . ? O6 C88 N5 112.4(13) . . ? N4 C88 N5 117.6(14) . . ? O6 C88 Ru2 59.3(7) . . ? N4 C88 Ru2 170.5(11) . . ? N5 C88 Ru2 53.1(7) . . ? C63 C58 C59 115.2(15) . . ? C63 C58 P3 123.4(12) . . ? C59 C58 P3 121.4(12) . . ? C234 C239 C238 118.6(16) . . ? C105 C100 C101 118.2(15) . . ? C105 C100 P5 122.6(12) . . ? C101 C100 P5 119.2(13) . . ? C246 C247 C248 118.3(17) . . ? C187 C186 C191 118.4(14) . . ? C187 C186 P9 120.8(12) . . ? C191 C186 P9 120.4(12) . . ? C167 C168 C169 120.4(15) . . ? C174 N8 N9 117.0(11) . . ? C174 N8 Ru3 94.7(9) . . ? N9 N8 Ru3 147.2(8) . . ? C52 C57 C56 122.5(15) . . ? C18 C13 C14 120.0(15) . . ? C18 C13 P1 121.2(12) . . ? C14 C13 P1 118.5(12) . . ? O2 C40 N1 130.7(13) . . ? O2 C40 N2 109.8(12) . . ? N1 C40 N2 119.5(14) . . ? C215 C210 C211 118.0(14) . . ? C215 C210 P10 121.9(12) . . ? C211 C210 P10 120.1(12) . . ? C41 N3 N2 118.8(11) . . ? C41 N3 Pd1 127.9(10) . . ? N2 N3 Pd1 113.3(8) . . ? C258 C253 C254 121.6(15) . . ? C258 C253 P12 121.9(12) . . ? C254 C253 P12 116.3(12) . . ? O9 C174 N7 131.0(14) . . ? O9 C174 N8 113.0(13) . . ? N7 C174 N8 116.0(14) . . ? O9 C174 Ru3 59.7(7) . . ? N7 C174 Ru3 168.8(11) . . ? N8 C174 Ru3 53.5(7) . . ? N3 C41 C42 124.3(13) . . ? N3 N2 C40 113.4(11) . . ? N3 N2 Ru1 149.0(8) . . ? C40 N2 Ru1 96.9(9) . . ? C52 C53 C54 117.1(15) . . ? C60 C59 C58 122.0(17) . . ? C148 C143 C144 117.3(13) . . ? C148 C143 P7 123.7(11) . . ? C144 C143 P7 118.9(11) . . ? C193 C192 C197 118.6(14) . . ? C193 C192 P9 120.2(12) . . ? C197 C192 P9 121.2(11) . . ? C99 C90 C91 122.5(15) . . ? C99 C90 C89 123.0(13) . . ? C91 C90 C89 114.4(12) . . ? C234 C235 C236 119.1(15) . . ? C149 C154 C153 116.7(14) . . ? C216 C221 C220 120.4(15) . . ? C239 C234 C235 120.8(14) . . ? C239 C234 P11 116.6(12) . . ? C235 C234 P11 122.5(12) . . ? O3 C51 C42 127.6(13) . . ? O3 C51 C50 112.9(13) . . ? C42 C51 C50 119.5(14) . . ? C233 C224 C223 121.5(14) . . ? C233 C224 C225 119.8(15) . . ? C223 C224 C225 118.7(14) . . ? C222 N10 Pd4 111.3(10) . . ? C62 C63 C58 122.0(16) . . ? O11 C233 C224 130.4(15) . . ? O11 C233 C232 110.6(14) . . ? C224 C233 C232 118.9(16) . . ? C221 C216 C217 118.8(14) . . ? C221 C216 P10 120.6(12) . . ? C217 C216 P10 120.4(12) . . ? C19 C24 C23 118.5(15) . . ? C168 C167 C172 118.8(13) . . ? C168 C167 P8 123.9(11) . . ? C172 C167 P8 117.0(11) . . ? C171 C172 C167 118.6(15) . . ? C86 C87 C82 122.8(15) . . ? C85 C86 C87 118.1(16) . . ? C178 C177 C176 123.7(14) . . ? C178 C177 C182 116.8(14) . . ? C176 C177 C182 119.5(13) . . ? C192 C197 C196 119.2(15) . . ? C166 C161 C162 118.8(14) . . ? C166 C161 P8 118.2(11) . . ? C162 C161 P8 122.7(11) . . ? C219 C220 C221 119.8(16) . . ? C261 C260 C259 122.4(14) . . ? C32 C31 C36 117.0(14) . . ? C32 C31 P2 120.5(12) . . ? C36 C31 P2 122.1(12) . . ? C51 C42 C43 118.9(13) . . ? C51 C42 C41 123.4(13) . . ? C43 C42 C41 117.7(12) . . ? C206 C205 C204 124.3(15) . . ? C207 C206 C205 116.7(17) . . ? C209 C204 C205 116.0(14) . . ? C209 C204 P10 123.5(12) . . ? C205 C204 P10 120.4(11) . . ? C253 C254 C255 117.8(16) . . ? C2 C1 C6 118.9(14) . . ? C2 C1 P1 123.9(12) . . ? C6 C1 P1 116.9(11) . . ? C237 C236 C235 120.8(17) . . ? C136 C131 C132 119.5(16) . . ? C136 C131 P6 121.5(13) . . ? C132 C131 P6 119.0(13) . . ? C161 C166 C165 120.7(15) . . ? C107 C106 C111 122.4(16) . . ? C107 C106 P5 115.6(13) . . ? C111 C106 P5 122.0(13) . . ? C125 C130 C129 120.1(15) . . ? C184 C183 C182 123.1(15) . . ? C183 C182 C181 124.5(15) . . ? C183 C182 C177 117.4(14) . . ? C181 C182 C177 118.0(15) . . ? C183 C184 C185 122.6(15) . . ? C263 C264 C259 119.2(15) . . ? C180 C181 C182 122.2(17) . . ? C170 C171 C172 118.1(17) . . ? C75 C70 C71 117.3(14) . . ? C75 C70 P4 120.4(11) . . ? C71 C70 P4 121.7(11) . . ? C22 C23 C24 121.5(16) . . ? C64 C65 C66 120.9(14) . . ? C46 C47 C48 122.2(15) . . ? C19 C20 C21 121.9(15) . . ? C46 C45 C44 119.3(17) . . ? C171 C170 C169 125.9(18) . . ? C145 C144 C143 122.1(14) . . ? C65 C64 C69 117.7(13) . . ? C65 C64 P3 124.4(11) . . ? C69 C64 P3 117.8(11) . . ? C47 C46 C45 120.2(17) . . ? C152 C153 C154 122.4(16) . . ? C161 C162 C163 119.7(14) . . ? C73 C72 C71 119.5(16) . . ? C70 C71 C72 120.9(14) . . ? C67 C66 C65 118.4(16) . . ? C192 C193 C194 123.5(15) . . ? C119 C120 C121 119.8(15) . . ? C143 C148 C147 120.3(14) . . ? C226 C225 C230 119.6(15) . . ? C226 C225 C224 121.5(15) . . ? C230 C225 C224 118.8(15) . . ? C72 C73 C74 122.0(17) . . ? C120 C119 C124 120.8(17) . . ? C120 C119 P6 120.9(13) . . ? C124 C119 P6 118.2(14) . . ? C164 C165 C166 117.7(17) . . ? C67 C68 C69 118.6(16) . . ? C68 C67 C66 124.5(16) . . ? C186 C187 C188 121.1(15) . . ? C84 C85 C86 121.0(17) . . ? C164 C163 C162 117.6(16) . . ? C7 C8 C9 122.7(15) . . ? C179 C178 C177 124.1(15) . . ? C8 C7 C12 118.2(14) . . ? C8 C7 P1 121.7(12) . . ? C12 C7 P1 119.9(11) . . ? C216 C217 C218 119.3(16) . . ? C262 C261 C260 116.5(17) . . ? C149 C150 C151 121.4(14) . . ? C210 C211 C212 122.4(15) . . ? C61 C60 C59 120.3(19) . . ? C131 C132 C133 120.4(16) . . ? N9 C175 C176 125.3(13) . . ? C70 C75 C74 120.9(15) . . ? C13 C14 C15 119.4(15) . . ? C10 C9 C8 116.2(16) . . ? C13 C18 C17 118.9(17) . . ? C155 C160 C159 120.2(15) . . ? C25 C26 C27 120.7(16) . . ? C270 C265 C266 119.6(15) . . ? C270 C265 P12 118.5(12) . . ? C266 C265 P12 121.8(12) . . ? C55 C54 C53 119.8(17) . . ? C96 C97 C98 126.9(17) . . ? C79 C80 C81 118.4(17) . . ? C257 C256 C255 119.6(18) . . ? C27 C28 C29 121.7(17) . . ? C43 C44 C45 122.4(15) . . ? C92 C93 C94 116.4(17) . . ? C48 C49 C50 122.7(15) . . ? C4 C5 C6 119.9(17) . . ? C104 C103 C102 124.0(18) . . ? O5 C99 C90 129.8(15) . . ? O5 C99 C98 112.4(14) . . ? C90 C99 C98 117.8(16) . . ? C249 C250 C251 116.7(18) . . ? C4 C3 C2 117.0(17) . . ? C97 C96 C95 123.8(17) . . ? C97 C96 C91 119.1(16) . . ? C95 C96 C91 117.1(16) . . ? C92 C91 C96 118.6(15) . . ? C92 C91 C90 125.8(14) . . ? C96 C91 C90 115.4(14) . . ? C189 C188 C187 117.9(17) . . ? C152 C151 C150 119.2(15) . . ? C203 C198 C199 117.4(18) . . ? C203 C198 P9 122.5(13) . . ? C199 C198 P9 120.1(15) . . ? C195 C196 C197 117.6(16) . . ? C1 C2 C3 121.8(15) . . ? C77 C76 C81 118.3(15) . . ? C77 C76 P4 119.3(13) . . ? C81 C76 P4 122.4(13) . . ? C231 C232 C233 117.7(17) . . ? C44 C43 C48 117.4(14) . . ? C44 C43 C42 122.9(13) . . ? C48 C43 C42 119.3(13) . . ? C181 C180 C179 122.0(17) . . ? C49 C48 C43 120.2(14) . . ? C49 C48 C47 121.6(14) . . ? C43 C48 C47 118.2(13) . . ? C210 C215 C214 119.3(16) . . ? C144 C145 C146 118.6(15) . . ? C158 C159 C160 118.6(15) . . ? C49 C50 C51 119.3(15) . . ? C165 C164 C163 125.5(18) . . ? C137 C138 C139 121.6(16) . . ? C213 C214 C215 118.9(18) . . ? C157 C158 C159 122.1(16) . . ? C115 C114 C113 118.8(17) . . ? C114 C115 C116 124.7(18) . . ? C256 C255 C254 122.4(17) . . ? C68 C69 C64 119.9(14) . . ? C193 C194 C195 116.9(17) . . ? C147 C146 C145 121.3(16) . . ? C106 C107 C108 121.6(16) . . ? C16 C15 C14 119.2(18) . . ? C253 C258 C257 117.0(16) . . ? C146 C147 C148 120.3(15) . . ? C112 C117 C116 117.6(16) . . ? C265 C266 C267 120.6(15) . . ? C229 C228 C227 125.6(19) . . ? C228 C229 C230 121.2(18) . . ? C10 C11 C12 116.6(16) . . ? C28 C29 C30 120.6(16) . . ? C7 C12 C11 121.5(14) . . ? C225 C226 C227 121.0(16) . . ? C186 C191 C190 119.2(18) . . ? C265 C270 C269 119.2(17) . . ? C231 C230 C225 117.3(17) . . ? C231 C230 C229 125.8(17) . . ? C225 C230 C229 116.7(16) . . ? C22 C21 C20 118.4(16) . . ? C178 C179 C180 116.9(16) . . ? C137 C142 C141 123.5(16) . . ? C97 C98 C99 117.6(16) . . ? C76 C81 C80 121.8(16) . . ? C246 C251 C250 121.0(16) . . ? C245 C240 C241 121.7(19) . . ? C245 C240 P11 118.6(15) . . ? C241 C240 P11 119.6(15) . . ? C91 C92 C93 124.4(16) . . ? C213 C212 C211 118.3(17) . . ? C82 C83 C84 120.2(15) . . ? C11 C10 C9 124.7(17) . . ? C85 C84 C83 120.8(17) . . ? C249 C248 C247 117.6(19) . . ? C23 C22 C21 120.7(17) . . ? C196 C195 C194 124.0(18) . . ? C212 C213 C214 123.0(19) . . ? C15 C16 C17 126(2) . . ? C237 C238 C239 119.4(17) . . ? C230 C231 C232 127.3(18) . . ? C95 C94 C93 122.6(19) . . ? C268 C267 C266 117.5(17) . . ? C56 C55 C54 123.4(19) . . ? C141 C140 C139 123.4(19) . . ? C133 C134 C135 125(2) . . ? C131 C136 C135 119.0(18) . . ? C60 C61 C62 120(2) . . ? C140 C139 C138 116.3(18) . . ? C28 C27 C26 119.0(16) . . ? C100 C105 C104 122.2(16) . . ? C170 C169 C168 118.1(17) . . ? C55 C56 C57 116.2(17) . . ? C127 C126 C125 118.6(16) . . ? C236 C237 C238 121.2(18) . . ? C198 C199 C200 119(2) . . ? C134 C133 C132 118.6(18) . . ? C134 C135 C136 117(2) . . ? C109 C110 C111 119.1(18) . . ? C110 C109 C108 125(2) . . ? C201 C202 C203 117.1(19) . . ? C102 C101 C100 120.5(17) . . ? C103 C104 C105 117.4(17) . . ? C158 C157 C156 119.9(16) . . ? C198 C203 C202 125.8(17) . . ? C153 C152 C151 120.9(16) . . ? C115 C116 C117 118.3(18) . . ? C106 C111 C110 116.9(17) . . ? C126 C127 C128 122.3(18) . . ? C228 C227 C226 115.7(17) . . ? C140 C141 C142 118.6(19) . . ? C73 C74 C75 119.1(17) . . ? C31 C36 C35 118.9(15) . . ? C31 C32 C33 121.1(16) . . ? C220 C219 C218 121.5(19) . . ? C207 C208 C209 119.3(19) . . ? C61 C62 C63 120.3(18) . . ? C208 C207 C206 122.7(19) . . ? C119 C124 C123 118.0(19) . . ? C128 C129 C130 121.8(17) . . ? C190 C189 C188 125(2) . . ? C240 C245 C244 118.3(18) . . ? C204 C209 C208 121.0(17) . . ? C129 C128 C127 117.5(18) . . ? C243 C244 C245 115.3(19) . . ? C269 C268 C267 125.0(19) . . ? C219 C218 C217 120.2(19) . . ? C78 C79 C80 122(2) . . ? C103 C102 C101 117.6(18) . . ? C16 C17 C18 116.6(19) . . ? C268 C269 C270 118.0(19) . . ? C3 C4 C5 123.1(18) . . ? C202 C201 C200 119(2) . . ? C244 C243 C242 128(2) . . ? C107 C108 C109 114.3(18) . . ? C250 C249 C248 125(2) . . ? C79 C78 C77 119(2) . . ? C94 C95 C96 120.7(19) . . ? C256 C257 C258 121.5(19) . . ? C240 C241 C242 121(2) . . ? C76 C77 C78 120.9(17) . . ? C262 C263 C264 119.7(17) . . ? C189 C190 C191 119(2) . . ? C243 C242 C241 114(2) . . ? C263 C262 C261 124.0(19) . . ? C201 C200 C199 121(3) . . ? C122 C121 C120 119.7(18) . . ? C121 C122 C123 121(2) . . ? C122 C123 C124 120(2) . . ? C35 C34 C33 129(2) . . ? C34 C33 C32 115.3(18) . . ? C34 C35 C36 118.9(18) . . ? O7 C173 Ru3 176.6(12) . . ? O10 C252 Ru4 175.3(14) . . ? O4 C118 Ru2 177.0(13) . . ? O1 C39 Ru1 177.5(13) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 17.74 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.530 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.082 data_s2 _database_code_depnum_ccdc_archive 'CCDC 848669' #TrackingRef 's2-r.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 N3 O3 P Pd' _chemical_formula_sum 'C30 H24 N3 O3 P Pd' _chemical_formula_weight 611.89 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.1000(18) _cell_length_b 16.700(3) _cell_length_c 18.400(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.39(3) _cell_angle_gamma 90.00 _cell_volume 2750.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.34759 _exptl_absorpt_correction_T_max 0.42416 _exptl_absorpt_process_details ; XPREP. Sheldrick, G.M., (1995). SHELXTL, Release 5.03 for Siemens R3 crystallographic research system. Siemens Analytical X-Ray Instruments, Inc., Madison, USA. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'Siemens P4 4-circle-diffractometer' _diffrn_measurement_method 'Profile fitted' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 5115 _diffrn_reflns_av_R_equivalents 0.1503 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4798 _reflns_number_gt 3817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens R3m/V (Siemens, 1989)' _computing_cell_refinement 'Siemens R3m/V (Siemens, 1989)' _computing_data_reduction 'XDISK (Siemens, 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS (Sheldrick, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1562P)^2^+5.5955P] 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 4798 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.2253 _refine_ls_wR_factor_gt 0.2106 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.004 _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 Pd1 Pd 0.57842(6) 0.43464(5) 0.23818(3) 0.0434(3) Uani 1 1 d . . . P2 P 0.7467(2) 0.45807(17) 0.34240(13) 0.0397(6) Uani 1 1 d . . . O1 O 0.4499(6) 0.3649(6) 0.2896(4) 0.056(2) Uani 1 1 d . . . N1 N 0.4372(7) 0.4240(6) 0.1434(4) 0.046(2) Uani 1 1 d . . . N2 N 0.4912(9) 0.4592(7) 0.0861(4) 0.057(3) Uani 1 1 d . . . H2A H 0.4438 0.4559 0.0413 0.068 Uiso 1 1 calc R . . N3 N 0.6838(8) 0.4982(7) 0.1738(4) 0.058(3) Uani 1 1 d . . . H3A H 0.7648 0.5235 0.1909 0.070 Uiso 1 1 calc R . . C1A C 0.3066(8) 0.3914(8) 0.1323(5) 0.052(3) Uani 1 1 d . . . H1A H 0.2503 0.3946 0.0849 0.062 Uiso 1 1 calc R . . C2A C 0.6243(9) 0.5000(8) 0.1032(6) 0.055(3) Uani 1 1 d . . . O2 O 0.6773(7) 0.5328(6) 0.0525(4) 0.059(2) Uani 1 1 d . . . C1 C 0.3167(9) 0.3372(7) 0.2593(5) 0.046(2) Uani 1 1 d . . . C2 C 0.2460(9) 0.2892(8) 0.3081(5) 0.052(3) Uani 1 1 d . . . H2 H 0.2992 0.2768 0.3548 0.063 Uiso 1 1 calc R . . C3 C 0.1036(10) 0.2615(8) 0.2883(6) 0.061(3) Uani 1 1 d . . . H3 H 0.0632 0.2283 0.3202 0.073 Uiso 1 1 calc R . . C4 C 0.0180(9) 0.2826(7) 0.2200(6) 0.050(3) Uani 1 1 d . . . C5 C -0.1363(10) 0.2638(9) 0.2036(7) 0.075(4) Uani 1 1 d . . . H5 H -0.1798 0.2358 0.2379 0.089 Uiso 1 1 calc R . . C6 C -0.2215(9) 0.2862(9) 0.1384(7) 0.068(4) Uani 1 1 d . . . H6 H -0.3228 0.2738 0.1283 0.082 Uiso 1 1 calc R . . C7 C -0.1569(10) 0.3274(9) 0.0875(8) 0.074(4) Uani 1 1 d . . . H7 H -0.2150 0.3411 0.0423 0.089 Uiso 1 1 calc R . . C8 C -0.0078(9) 0.3488(8) 0.1020(7) 0.062(3) Uani 1 1 d . . . H8 H 0.0323 0.3783 0.0674 0.074 Uiso 1 1 calc R . . C9 C 0.0821(9) 0.3267(8) 0.1678(6) 0.057(3) Uani 1 1 d . . . C10 C 0.2410(8) 0.3506(6) 0.1874(5) 0.043(2) Uani 1 1 d . . . C11 C 0.8260(8) 0.3686(7) 0.3905(5) 0.044(3) Uani 1 1 d . . . C12 C 0.9681(9) 0.3700(8) 0.4352(5) 0.056(3) Uani 1 1 d . . . H12 H 1.0234 0.4171 0.4406 0.067 Uiso 1 1 calc R . . C13 C 1.0259(10) 0.3015(10) 0.4713(6) 0.065(4) Uani 1 1 d . . . H13 H 1.1221 0.3019 0.4989 0.078 Uiso 1 1 calc R . . C14 C 0.9429(11) 0.2332(10) 0.4666(6) 0.068(4) Uani 1 1 d . . . H14 H 0.9813 0.1878 0.4927 0.082 Uiso 1 1 calc R . . C15 C 0.8019(11) 0.2310(9) 0.4234(7) 0.074(4) Uani 1 1 d . . . H15 H 0.7464 0.1839 0.4194 0.089 Uiso 1 1 calc R . . C16 C 0.7442(9) 0.2984(8) 0.3865(6) 0.055(3) Uani 1 1 d . . . H16 H 0.6486 0.2970 0.3583 0.066 Uiso 1 1 calc R . . C21 C 0.6654(7) 0.5175(7) 0.4070(5) 0.044(2) Uani 1 1 d . . . C22 C 0.7119(8) 0.5097(8) 0.4832(5) 0.051(3) Uani 1 1 d . . . H22 H 0.7802 0.4700 0.5018 0.061 Uiso 1 1 calc R . . C23 C 0.6557(10) 0.5615(9) 0.5319(6) 0.067(4) Uani 1 1 d . . . H23 H 0.6866 0.5569 0.5827 0.081 Uiso 1 1 calc R . . C24 C 0.5526(10) 0.6201(8) 0.5023(6) 0.064(3) Uani 1 1 d . . . H24 H 0.5153 0.6550 0.5339 0.077 Uiso 1 1 calc R . . C25 C 0.5063(9) 0.6270(8) 0.4292(7) 0.061(3) Uani 1 1 d . . . H25 H 0.4374 0.6664 0.4106 0.073 Uiso 1 1 calc R . . C26 C 0.5607(9) 0.5758(8) 0.3814(6) 0.057(3) Uani 1 1 d . . . H26 H 0.5262 0.5805 0.3309 0.068 Uiso 1 1 calc R . . C31 C 0.9074(7) 0.5173(7) 0.3262(5) 0.043(3) Uani 1 1 d . . . C32 C 1.0079(11) 0.4859(10) 0.2884(7) 0.074(4) Uani 1 1 d . . . H32 H 0.9961 0.4332 0.2721 0.089 Uiso 1 1 calc R . . C33 C 1.1281(12) 0.5298(9) 0.2729(9) 0.071(4) Uani 1 1 d . . . H33 H 1.1967 0.5060 0.2478 0.085 Uiso 1 1 calc R . . C34 C 1.1452(10) 0.6068(10) 0.2945(7) 0.075(4) Uani 1 1 d . . . H34 H 1.2238 0.6370 0.2830 0.090 Uiso 1 1 calc R . . C35 C 1.0467(13) 0.6402(12) 0.3331(10) 0.104(6) Uani 1 1 d . . . H35 H 1.0592 0.6930 0.3491 0.124 Uiso 1 1 calc R . . C36 C 0.9273(11) 0.5956(9) 0.3488(8) 0.071(4) Uani 1 1 d . . . H36 H 0.8600 0.6190 0.3749 0.085 Uiso 1 1 calc R . . OW1 O 0.986(2) 0.5594(18) 0.0608(16) 0.277(16) 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 Pd1 0.0362(4) 0.0408(7) 0.0494(5) -0.0003(4) -0.0028(3) -0.0068(3) P2 0.0304(9) 0.0341(19) 0.0519(12) 0.0005(12) -0.0001(8) -0.0059(9) O1 0.039(3) 0.063(7) 0.062(4) 0.006(4) -0.001(2) -0.010(3) N1 0.043(3) 0.049(8) 0.039(4) 0.000(4) -0.009(3) -0.009(3) N2 0.063(4) 0.058(9) 0.042(4) 0.003(5) -0.010(3) -0.026(4) N3 0.051(4) 0.073(9) 0.046(4) -0.005(5) -0.006(3) -0.025(4) C1A 0.041(4) 0.051(10) 0.059(5) -0.009(6) -0.005(4) -0.013(4) C2A 0.048(4) 0.049(9) 0.066(6) -0.003(6) 0.006(4) -0.018(5) O2 0.060(4) 0.051(6) 0.062(4) 0.007(4) -0.003(3) -0.019(3) C1 0.044(4) 0.028(7) 0.064(5) -0.013(5) 0.007(4) -0.016(4) C2 0.051(4) 0.045(9) 0.059(5) -0.010(6) 0.006(4) -0.011(5) C3 0.055(5) 0.048(9) 0.083(7) -0.005(7) 0.024(5) -0.020(5) C4 0.045(4) 0.030(7) 0.074(6) -0.005(6) 0.006(4) 0.000(4) C5 0.046(5) 0.080(12) 0.103(9) -0.031(8) 0.028(5) -0.019(5) C6 0.035(4) 0.059(10) 0.104(8) -0.018(8) -0.004(5) -0.006(5) C7 0.047(5) 0.064(12) 0.103(9) -0.018(8) -0.010(5) -0.005(5) C8 0.043(4) 0.044(9) 0.091(7) 0.002(7) -0.008(4) -0.004(4) C9 0.037(4) 0.058(10) 0.074(6) -0.015(6) 0.008(4) -0.014(4) C10 0.036(4) 0.018(6) 0.070(6) -0.008(5) -0.001(4) -0.004(3) C11 0.034(3) 0.042(8) 0.054(5) -0.003(5) 0.002(3) -0.003(4) C12 0.041(4) 0.049(9) 0.069(6) 0.013(6) -0.011(4) -0.003(4) C13 0.046(5) 0.064(12) 0.078(7) 0.021(7) -0.010(4) 0.003(5) C14 0.066(6) 0.059(11) 0.074(7) 0.029(7) -0.001(5) 0.009(6) C15 0.058(5) 0.049(10) 0.114(9) 0.014(8) 0.011(6) -0.011(5) C16 0.041(4) 0.039(8) 0.078(6) 0.010(6) -0.006(4) -0.003(4) C21 0.027(3) 0.047(8) 0.058(5) 0.001(5) 0.002(3) -0.011(4) C22 0.033(4) 0.058(10) 0.060(5) -0.001(6) 0.001(3) -0.009(4) C23 0.044(5) 0.096(13) 0.061(6) -0.014(7) 0.009(4) -0.023(5) C24 0.046(5) 0.066(10) 0.086(7) -0.018(7) 0.026(5) -0.019(5) C25 0.046(4) 0.038(9) 0.098(8) -0.010(7) 0.015(5) 0.004(4) C26 0.044(4) 0.067(11) 0.059(5) 0.004(6) 0.011(4) -0.006(5) C31 0.030(3) 0.049(9) 0.048(4) -0.004(5) 0.002(3) -0.006(4) C32 0.065(6) 0.051(12) 0.116(10) -0.016(8) 0.041(6) -0.004(6) C33 0.069(6) 0.013(6) 0.141(11) 0.004(8) 0.048(7) 0.005(5) C34 0.044(5) 0.075(13) 0.110(9) 0.006(9) 0.026(5) -0.010(6) C35 0.077(7) 0.071(15) 0.178(15) -0.038(12) 0.065(9) -0.031(8) C36 0.058(5) 0.031(8) 0.131(10) -0.020(8) 0.040(6) -0.011(5) OW1 0.25(2) 0.23(4) 0.39(4) 0.13(3) 0.18(3) 0.044(18) _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 N3 1.965(8) . ? Pd1 N1 1.979(7) . ? Pd1 O1 2.005(7) . ? Pd1 P2 2.262(2) . ? P2 C21 1.806(10) . ? P2 C11 1.819(12) . ? P2 C31 1.834(9) . ? O1 C1 1.323(10) . ? N1 C1A 1.290(11) . ? N1 N2 1.373(11) . ? N2 C2A 1.376(12) . ? N2 H2A 0.8600 . ? N3 C2A 1.313(13) . ? N3 H3A 0.8600 . ? C1A C10 1.438(14) . ? C1A H1A 0.9300 . ? C2A O2 1.251(12) . ? C1 C10 1.393(14) . ? C1 C2 1.440(14) . ? C2 C3 1.362(13) . ? C2 H2 0.9300 . ? C3 C4 1.398(15) . ? C3 H3 0.9300 . ? C4 C9 1.417(15) . ? C4 C5 1.418(12) . ? C5 C6 1.358(17) . ? C5 H5 0.9300 . ? C6 C7 1.376(19) . ? C6 H6 0.9300 . ? C7 C8 1.383(13) . ? C7 H7 0.9300 . ? C8 C9 1.383(15) . ? C8 H8 0.9300 . ? C9 C10 1.481(10) . ? C11 C16 1.384(17) . ? C11 C12 1.402(11) . ? C12 C13 1.377(17) . ? C12 H12 0.9300 . ? C13 C14 1.36(2) . ? C13 H13 0.9300 . ? C14 C15 1.383(15) . ? C14 H14 0.9300 . ? C15 C16 1.370(17) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C26 1.384(16) . ? C21 C22 1.395(13) . ? C22 C23 1.407(16) . ? C22 H22 0.9300 . ? C23 C24 1.397(19) . ? C23 H23 0.9300 . ? C24 C25 1.340(16) . ? C24 H24 0.9300 . ? C25 C26 1.381(16) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C32 1.351(14) . ? C31 C36 1.373(17) . ? C32 C33 1.387(16) . ? C32 H32 0.9300 . ? C33 C34 1.35(2) . ? C33 H33 0.9300 . ? C34 C35 1.360(17) . ? C34 H34 0.9300 . ? C35 C36 1.390(16) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? 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 N3 Pd1 N1 80.0(3) . . ? N3 Pd1 O1 171.2(3) . . ? N1 Pd1 O1 91.3(3) . . ? N3 Pd1 P2 95.1(2) . . ? N1 Pd1 P2 174.5(3) . . ? O1 Pd1 P2 93.66(19) . . ? C21 P2 C11 107.8(4) . . ? C21 P2 C31 104.1(5) . . ? C11 P2 C31 105.3(4) . . ? C21 P2 Pd1 111.0(3) . . ? C11 P2 Pd1 114.8(3) . . ? C31 P2 Pd1 113.1(3) . . ? C1 O1 Pd1 124.9(6) . . ? C1A N1 N2 120.4(8) . . ? C1A N1 Pd1 127.6(7) . . ? N2 N1 Pd1 111.9(5) . . ? N1 N2 C2A 117.3(8) . . ? N1 N2 H2A 121.4 . . ? C2A N2 H2A 121.4 . . ? C2A N3 Pd1 116.7(6) . . ? C2A N3 H3A 121.6 . . ? Pd1 N3 H3A 121.6 . . ? N1 C1A C10 125.2(9) . . ? N1 C1A H1A 117.4 . . ? C10 C1A H1A 117.4 . . ? O2 C2A N3 127.0(8) . . ? O2 C2A N2 119.2(9) . . ? N3 C2A N2 113.8(8) . . ? O1 C1 C10 127.0(9) . . ? O1 C1 C2 114.2(9) . . ? C10 C1 C2 118.8(7) . . ? C3 C2 C1 122.2(10) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C2 C3 C4 120.2(9) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C9 120.6(8) . . ? C3 C4 C5 120.4(10) . . ? C9 C4 C5 118.9(10) . . ? C6 C5 C4 120.9(11) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 119.5(9) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C8 121.6(12) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C7 C8 C9 120.3(11) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C4 118.8(8) . . ? C8 C9 C10 122.6(9) . . ? C4 C9 C10 118.5(9) . . ? C1 C10 C1A 123.3(7) . . ? C1 C10 C9 118.8(8) . . ? C1A C10 C9 117.8(9) . . ? C16 C11 C12 118.4(11) . . ? C16 C11 P2 120.5(7) . . ? C12 C11 P2 121.0(9) . . ? C13 C12 C11 120.0(11) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.4(9) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.3(13) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 119.7(12) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C11 121.1(9) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? C26 C21 C22 118.3(9) . . ? C26 C21 P2 120.0(7) . . ? C22 C21 P2 121.6(8) . . ? C21 C22 C23 120.2(11) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 118.6(10) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C25 C24 C23 121.3(11) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 120.1(11) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 121.5(10) . . ? C25 C26 H26 119.2 . . ? C21 C26 H26 119.2 . . ? C32 C31 C36 117.4(9) . . ? C32 C31 P2 120.6(10) . . ? C36 C31 P2 122.0(6) . . ? C31 C32 C33 122.2(14) . . ? C31 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C34 C33 C32 119.8(11) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 119.6(11) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 120.1(16) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 119.9 . . ? C31 C36 C35 120.9(11) . . ? C31 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.392 _refine_diff_density_min -1.861 _refine_diff_density_rms 0.129 data_x _database_code_depnum_ccdc_archive 'CCDC 848670' #TrackingRef 'sb-sd-1-r.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H24 N3 O2 P Pd' _chemical_formula_weight 554.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 '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 10.1264(9) _cell_length_b 14.1165(12) _cell_length_c 16.8322(12) _cell_angle_alpha 80.414(7) _cell_angle_beta 84.706(7) _cell_angle_gamma 78.503(7) _cell_volume 2320.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16582 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.1335 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 30.00 _reflns_number_total 13031 _reflns_number_gt 7296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 ; _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.0411P)^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 13031 _refine_ls_number_parameters 615 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C13 C 1.0239(4) 0.1361(3) 0.6174(2) 0.0255(8) Uani 1 1 d . . . H13 H 1.0854 0.1774 0.6157 0.031 Uiso 1 1 calc R . . C15 C 0.9089(4) 0.0165(3) 0.6931(2) 0.0285(9) Uani 1 1 d . . . H15 H 0.8916 -0.0236 0.7411 0.034 Uiso 1 1 calc R . . C16 C 0.8446(3) 0.0149(3) 0.6258(2) 0.0237(8) Uani 1 1 d . . . H16 H 0.7835 -0.0272 0.6301 0.028 Uiso 1 1 calc R . . C32 C 1.0377(4) 0.5022(2) 0.3875(2) 0.0221(8) Uani 1 1 d . . . H32 H 1.1266 0.4803 0.4014 0.027 Uiso 1 1 calc R . . C35 C 0.7729(4) 0.5685(3) 0.3463(2) 0.0270(8) Uani 1 1 d . . . H35 H 0.6843 0.5910 0.3320 0.032 Uiso 1 1 calc R . . C36 C 0.8384(4) 0.4758(3) 0.3341(2) 0.0262(8) Uani 1 1 d . . . H36 H 0.7930 0.4355 0.3128 0.031 Uiso 1 1 calc R . . C42 C 1.2542(4) 0.2702(2) 0.4357(2) 0.0236(8) Uani 1 1 d . . . H42 H 1.1830 0.2643 0.4742 0.028 Uiso 1 1 calc R . . C44 C 1.4910(4) 0.2564(3) 0.4036(2) 0.0277(9) Uani 1 1 d . . . H44 H 1.5791 0.2407 0.4197 0.033 Uiso 1 1 calc R . . C45 C 1.4676(4) 0.2875(3) 0.3222(2) 0.0337(10) Uani 1 1 d . . . H45 H 1.5393 0.2946 0.2844 0.040 Uiso 1 1 calc R . . C46 C 1.3362(4) 0.3078(3) 0.2984(2) 0.0282(9) Uani 1 1 d . . . H46 H 1.3201 0.3266 0.2440 0.034 Uiso 1 1 calc R . . C54 C 1.1304(4) 0.3815(3) 0.0504(2) 0.0326(10) Uani 1 1 d . . . H54 H 1.1498 0.3916 -0.0051 0.039 Uiso 1 1 calc R . . C62 C 0.5702(4) 0.8520(2) -0.0170(2) 0.0231(8) Uani 1 1 d . . . C63 C 0.5305(4) 0.8436(3) -0.0939(2) 0.0284(9) Uani 1 1 d . . . H63 H 0.4770 0.7983 -0.0976 0.034 Uiso 1 1 calc R . . C65 C 0.6465(4) 0.9702(3) -0.1582(2) 0.0309(9) Uani 1 1 d . . . H65 H 0.6710 1.0103 -0.2046 0.037 Uiso 1 1 calc R . . C67 C 0.6519(3) 0.9217(3) -0.0118(2) 0.0232(8) Uani 1 1 d . . . C71 C 0.6346(4) 0.8858(3) 0.2754(2) 0.0276(9) Uani 1 1 d . . . C82 C 0.3258(4) 0.7126(3) 0.3486(2) 0.0256(8) Uani 1 1 d . . . H82 H 0.3022 0.7780 0.3261 0.031 Uiso 1 1 calc R . . C83 C 0.3053(4) 0.6837(3) 0.4311(2) 0.0296(9) Uani 1 1 d . . . H83 H 0.2694 0.7302 0.4642 0.036 Uiso 1 1 calc R . . C84 C 0.3378(4) 0.5863(3) 0.4643(2) 0.0308(9) Uani 1 1 d . . . H84 H 0.3227 0.5677 0.5195 0.037 Uiso 1 1 calc R . . C85 C 0.3924(4) 0.5165(3) 0.4161(2) 0.0280(9) Uani 1 1 d . . . H85 H 0.4131 0.4509 0.4385 0.034 Uiso 1 1 calc R . . C86 C 0.4163(4) 0.5449(3) 0.3341(2) 0.0232(8) Uani 1 1 d . . . H86 H 0.4555 0.4981 0.3018 0.028 Uiso 1 1 calc R . . C92 C 0.2275(4) 0.7480(3) 0.0739(2) 0.0281(9) Uani 1 1 d . . . H92 H 0.3026 0.7593 0.0402 0.034 Uiso 1 1 calc R . . C93 C 0.1017(4) 0.7684(3) 0.0427(2) 0.0318(9) Uani 1 1 d . . . H93 H 0.0930 0.7916 -0.0120 0.038 Uiso 1 1 calc R . . C94 C -0.0123(4) 0.7542(3) 0.0932(2) 0.0297(9) Uani 1 1 d . . . H94 H -0.0973 0.7675 0.0725 0.036 Uiso 1 1 calc R . . C95 C 0.0027(4) 0.7199(3) 0.1744(2) 0.0305(9) Uani 1 1 d . . . H95 H -0.0731 0.7121 0.2088 0.037 Uiso 1 1 calc R . . C96 C 0.1290(4) 0.6971(3) 0.2050(2) 0.0259(8) Uani 1 1 d . . . H96 H 0.1381 0.6724 0.2594 0.031 Uiso 1 1 calc R . . C101 C 0.4925(4) 0.5716(3) 0.1510(2) 0.0210(8) Uani 1 1 d . . . C103 C 0.4846(4) 0.4234(3) 0.0983(2) 0.0309(9) Uani 1 1 d . . . H103 H 0.4348 0.3835 0.0801 0.037 Uiso 1 1 calc R . . C104 C 0.6229(4) 0.3975(3) 0.0991(2) 0.0348(10) Uani 1 1 d . . . H104 H 0.6664 0.3387 0.0828 0.042 Uiso 1 1 calc R . . C105 C 0.6983(4) 0.4581(3) 0.1240(2) 0.0326(9) Uani 1 1 d . . . H105 H 0.7918 0.4406 0.1241 0.039 Uiso 1 1 calc R . . C106 C 0.6320(4) 0.5452(3) 0.1488(2) 0.0279(9) Uani 1 1 d . . . H106 H 0.6823 0.5867 0.1643 0.034 Uiso 1 1 calc R . . C681 C 0.8053(4) 1.0020(3) 0.0592(2) 0.0329(9) Uani 1 1 d . . . H68A H 0.7614 1.0685 0.0609 0.049 Uiso 1 1 calc R . . H68B H 0.8606 0.9983 0.0099 0.049 Uiso 1 1 calc R . . H68C H 0.8607 0.9792 0.1043 0.049 Uiso 1 1 calc R . . O711 O 0.6513(3) 0.9151(2) 0.33902(15) 0.0371(7) Uani 1 1 d . . . C12 C 0.9599(3) 0.1361(2) 0.5460(2) 0.0198(7) Uani 1 1 d . . . C14 C 0.9992(4) 0.0779(3) 0.6892(2) 0.0279(9) Uani 1 1 d . . . H14 H 1.0434 0.0802 0.7347 0.033 Uiso 1 1 calc R . . C17 C 0.8637(3) 0.0722(2) 0.5502(2) 0.0202(7) Uani 1 1 d . . . C18 C 0.7887(3) 0.0625(2) 0.4829(2) 0.0203(8) Uani 1 1 d . . . C21 C 0.7788(4) 0.1381(3) 0.2707(2) 0.0237(8) Uani 1 1 d . . . C31 C 0.9727(4) 0.4427(2) 0.3535(2) 0.0211(8) Uani 1 1 d . . . C33 C 0.9711(4) 0.5935(3) 0.4009(2) 0.0261(8) Uani 1 1 d . . . H33 H 1.0149 0.6330 0.4242 0.031 Uiso 1 1 calc R . . C34 C 0.8385(4) 0.6272(3) 0.3796(2) 0.0257(8) Uani 1 1 d . . . H34 H 0.7942 0.6894 0.3879 0.031 Uiso 1 1 calc R . . C41 C 1.2269(4) 0.3004(2) 0.3556(2) 0.0206(8) Uani 1 1 d . . . C43 C 1.3857(4) 0.2485(3) 0.4602(2) 0.0272(9) Uani 1 1 d . . . H43 H 1.4022 0.2289 0.5145 0.033 Uiso 1 1 calc R . . C51 C 1.0738(3) 0.3490(2) 0.2160(2) 0.0180(7) Uani 1 1 d . . . C52 C 1.1103(4) 0.2705(3) 0.1736(2) 0.0252(8) Uani 1 1 d . . . H52 H 1.1157 0.2070 0.2008 0.030 Uiso 1 1 calc R . . C53 C 1.1384(4) 0.2865(3) 0.0916(2) 0.0337(10) Uani 1 1 d . . . H53 H 1.1628 0.2336 0.0634 0.040 Uiso 1 1 calc R . . C55 C 1.0936(4) 0.4613(3) 0.0915(2) 0.0269(9) Uani 1 1 d . . . H55 H 1.0879 0.5248 0.0641 0.032 Uiso 1 1 calc R . . C56 C 1.0657(3) 0.4444(3) 0.1742(2) 0.0224(8) Uani 1 1 d . . . H56 H 1.0411 0.4972 0.2025 0.027 Uiso 1 1 calc R . . C64 C 0.5695(4) 0.9014(3) -0.1640(2) 0.0308(9) Uani 1 1 d . . . H64 H 0.5440 0.8938 -0.2139 0.037 Uiso 1 1 calc R . . C66 C 0.6872(4) 0.9802(2) -0.0853(2) 0.0266(9) Uani 1 1 d . . . H66 H 0.7397 1.0268 -0.0836 0.032 Uiso 1 1 calc R . . C68 C 0.7021(3) 0.9401(3) 0.0627(2) 0.0241(8) Uani 1 1 d . . . C81 C 0.3828(3) 0.6415(2) 0.2995(2) 0.0182(7) Uani 1 1 d . . . C91 C 0.2435(4) 0.7111(2) 0.1544(2) 0.0209(8) Uani 1 1 d . . . C102 C 0.4202(4) 0.5098(3) 0.1250(2) 0.0255(8) Uani 1 1 d . . . H102 H 0.3266 0.5268 0.1254 0.031 Uiso 1 1 calc R . . C181 C 0.6784(4) 0.0026(3) 0.4984(2) 0.0317(9) Uani 1 1 d . . . H18A H 0.6143 0.0249 0.4576 0.047 Uiso 1 1 calc R . . H18B H 0.6336 0.0097 0.5505 0.047 Uiso 1 1 calc R . . H18C H 0.7171 -0.0650 0.4970 0.047 Uiso 1 1 calc R . . O11 O 0.9922(3) 0.19784(18) 0.48342(14) 0.0258(6) Uani 1 1 d . . . O22 O 0.7350(3) 0.11839(18) 0.20991(14) 0.0302(6) Uani 1 1 d . . . O61 O 0.5285(3) 0.78975(19) 0.04278(15) 0.0308(6) Uani 1 1 d . . . Pd1 Pd 0.93043(3) 0.206944(19) 0.373454(16) 0.01869(7) Uani 1 1 d . . . Pd2 Pd 0.53870(3) 0.798847(19) 0.158180(16) 0.02109(8) Uani 1 1 d . . . N19 N 0.8139(3) 0.10406(19) 0.41025(16) 0.0149(6) Uani 1 1 d . . . N20 N 0.7480(3) 0.0894(2) 0.34598(17) 0.0231(7) Uani 1 1 d . . . H20 H 0.6901 0.0512 0.3528 0.028 Uiso 1 1 calc R . . N22 N 0.8511(3) 0.2077(2) 0.27037(17) 0.0267(7) Uani 1 1 d . . . H22 H 0.8623 0.2498 0.2283 0.032 Uiso 1 1 calc R . . N69 N 0.6536(3) 0.9034(2) 0.13246(18) 0.0227(7) Uani 1 1 d . . . N70 N 0.6925(3) 0.9269(2) 0.20261(18) 0.0266(7) Uani 1 1 d . . . H70 H 0.7495 0.9650 0.2013 0.032 Uiso 1 1 calc R . . N72 N 0.5670(3) 0.8157(2) 0.26867(17) 0.0274(7) Uani 1 1 d . . . H72 H 0.5374 0.7799 0.3103 0.033 Uiso 1 1 calc R . . P1 P 1.05366(9) 0.32437(6) 0.32572(5) 0.01785(19) Uani 1 1 d . . . P2 P 0.41199(9) 0.68149(7) 0.19166(5) 0.0196(2) 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 C13 0.029(2) 0.0210(19) 0.030(2) -0.0035(16) -0.0050(17) -0.0105(16) C15 0.028(2) 0.026(2) 0.028(2) 0.0050(16) 0.0058(17) -0.0067(17) C16 0.0155(18) 0.0197(19) 0.034(2) -0.0027(16) 0.0057(16) -0.0040(15) C32 0.024(2) 0.0199(19) 0.0252(19) -0.0046(15) -0.0036(16) -0.0094(15) C35 0.020(2) 0.031(2) 0.031(2) -0.0087(17) -0.0025(16) -0.0022(17) C36 0.023(2) 0.028(2) 0.033(2) -0.0100(17) -0.0053(17) -0.0106(17) C42 0.0212(19) 0.0193(19) 0.030(2) 0.0048(15) -0.0056(16) -0.0098(15) C44 0.0177(19) 0.0200(19) 0.047(2) -0.0134(17) -0.0107(18) 0.0041(15) C45 0.027(2) 0.040(2) 0.035(2) -0.0112(19) 0.0034(18) -0.0061(19) C46 0.022(2) 0.037(2) 0.026(2) -0.0087(17) -0.0040(16) -0.0011(17) C54 0.032(2) 0.045(3) 0.0194(19) -0.0020(18) -0.0005(17) -0.007(2) C62 0.026(2) 0.0127(18) 0.028(2) -0.0023(15) 0.0052(16) -0.0015(15) C63 0.028(2) 0.022(2) 0.035(2) -0.0087(16) 0.0031(18) -0.0039(17) C65 0.027(2) 0.028(2) 0.031(2) 0.0027(17) 0.0091(17) -0.0001(17) C67 0.0167(19) 0.0163(18) 0.035(2) -0.0040(15) 0.0043(16) -0.0022(15) C71 0.028(2) 0.025(2) 0.031(2) 0.0000(16) -0.0114(17) -0.0079(17) C82 0.025(2) 0.0187(19) 0.031(2) -0.0023(15) -0.0065(16) 0.0022(15) C83 0.027(2) 0.039(2) 0.0214(19) -0.0108(17) -0.0016(16) 0.0002(18) C84 0.022(2) 0.043(3) 0.024(2) 0.0033(18) -0.0019(16) -0.0036(18) C85 0.028(2) 0.028(2) 0.029(2) -0.0035(17) -0.0057(17) -0.0082(17) C86 0.0192(19) 0.024(2) 0.029(2) -0.0076(16) -0.0028(16) -0.0056(15) C92 0.027(2) 0.030(2) 0.028(2) -0.0005(16) -0.0056(17) -0.0083(17) C93 0.042(3) 0.027(2) 0.029(2) 0.0059(17) -0.0129(19) -0.0158(19) C94 0.024(2) 0.026(2) 0.040(2) -0.0062(17) -0.0095(18) -0.0010(17) C95 0.027(2) 0.030(2) 0.037(2) -0.0110(18) 0.0039(18) -0.0084(18) C96 0.024(2) 0.027(2) 0.028(2) -0.0003(16) -0.0040(16) -0.0085(16) C101 0.0217(19) 0.0227(19) 0.0191(18) -0.0015(14) -0.0038(15) -0.0053(15) C103 0.029(2) 0.029(2) 0.037(2) -0.0129(18) -0.0060(18) -0.0022(17) C104 0.035(2) 0.032(2) 0.038(2) -0.0167(18) 0.0067(19) -0.0011(19) C105 0.0152(19) 0.040(3) 0.044(2) -0.011(2) -0.0004(18) -0.0052(18) C106 0.028(2) 0.033(2) 0.027(2) -0.0094(17) -0.0044(17) -0.0091(18) C681 0.024(2) 0.032(2) 0.044(2) -0.0050(18) 0.0032(18) -0.0103(18) O711 0.0548(19) 0.0365(17) 0.0289(15) -0.0062(12) -0.0111(14) -0.0245(15) C12 0.0224(19) 0.0148(17) 0.0216(18) -0.0017(14) -0.0027(15) -0.0029(15) C14 0.027(2) 0.028(2) 0.026(2) -0.0075(16) -0.0039(16) 0.0044(17) C17 0.0104(17) 0.0197(18) 0.0287(19) -0.0030(15) 0.0005(14) -0.0002(14) C18 0.0148(18) 0.0082(16) 0.038(2) 0.0004(15) -0.0009(15) -0.0060(13) C21 0.0205(19) 0.0170(18) 0.032(2) -0.0040(15) -0.0026(16) 0.0006(15) C31 0.024(2) 0.0172(18) 0.0213(18) 0.0014(14) -0.0009(15) -0.0048(15) C33 0.029(2) 0.0213(19) 0.031(2) -0.0051(16) -0.0064(17) -0.0092(16) C34 0.030(2) 0.0186(19) 0.028(2) -0.0058(15) 0.0011(17) -0.0020(16) C41 0.0226(19) 0.0117(17) 0.030(2) -0.0074(14) -0.0027(16) -0.0051(14) C43 0.032(2) 0.021(2) 0.029(2) 0.0027(16) -0.0096(17) -0.0067(17) C51 0.0113(17) 0.0190(18) 0.0225(18) 0.0025(14) -0.0059(14) -0.0027(14) C52 0.022(2) 0.026(2) 0.026(2) -0.0073(16) -0.0054(16) 0.0031(16) C53 0.028(2) 0.044(3) 0.029(2) -0.0162(18) -0.0054(17) 0.0038(19) C55 0.025(2) 0.030(2) 0.026(2) 0.0059(17) -0.0046(16) -0.0138(17) C56 0.0147(18) 0.030(2) 0.0236(19) -0.0043(15) -0.0016(15) -0.0060(15) C64 0.025(2) 0.034(2) 0.033(2) -0.0104(18) -0.0012(17) 0.0024(18) C66 0.023(2) 0.0132(18) 0.044(2) 0.0029(16) 0.0025(17) -0.0126(15) C68 0.0137(18) 0.024(2) 0.035(2) -0.0076(16) 0.0043(16) -0.0051(15) C81 0.0145(17) 0.0151(17) 0.0279(19) -0.0024(14) -0.0040(15) -0.0094(14) C91 0.0218(19) 0.0196(18) 0.0245(19) -0.0078(15) -0.0062(15) -0.0052(15) C102 0.026(2) 0.0202(19) 0.032(2) -0.0071(16) -0.0030(17) -0.0060(16) C181 0.032(2) 0.029(2) 0.039(2) -0.0081(18) -0.0008(18) -0.0169(18) O11 0.0319(15) 0.0277(14) 0.0219(13) 0.0022(11) -0.0053(11) -0.0186(12) O22 0.0428(17) 0.0244(14) 0.0298(14) -0.0007(11) -0.0147(13) -0.0188(13) O61 0.0362(16) 0.0337(16) 0.0278(14) -0.0079(12) 0.0020(12) -0.0188(13) Pd1 0.01835(15) 0.01684(14) 0.02237(15) -0.00270(11) -0.00342(11) -0.00605(11) Pd2 0.02208(16) 0.01728(15) 0.02614(16) -0.00308(11) -0.00303(12) -0.00849(12) N19 0.0103(14) 0.0097(14) 0.0259(15) -0.0025(11) -0.0043(12) -0.0037(11) N20 0.0200(16) 0.0220(16) 0.0321(17) -0.0036(13) -0.0068(13) -0.0136(13) N22 0.0317(19) 0.0229(17) 0.0278(17) 0.0030(13) -0.0121(14) -0.0120(14) N69 0.0148(15) 0.0206(16) 0.0337(18) -0.0087(13) -0.0071(13) 0.0002(12) N70 0.0248(17) 0.0236(17) 0.0357(18) -0.0038(14) -0.0100(14) -0.0119(14) N72 0.039(2) 0.0199(16) 0.0276(17) 0.0052(13) -0.0145(15) -0.0184(15) P1 0.0180(5) 0.0173(5) 0.0194(5) -0.0036(4) -0.0019(4) -0.0050(4) P2 0.0216(5) 0.0171(5) 0.0219(5) -0.0029(4) -0.0036(4) -0.0072(4) _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 C13 C14 1.376(5) . ? C13 C12 1.418(5) . ? C15 C16 1.363(5) . ? C15 C14 1.370(5) . ? C16 C17 1.410(5) . ? C32 C33 1.375(5) . ? C32 C31 1.384(5) . ? C35 C34 1.373(5) . ? C35 C36 1.383(5) . ? C36 C31 1.397(5) . ? C42 C41 1.382(5) . ? C42 C43 1.391(5) . ? C44 C43 1.371(5) . ? C44 C45 1.394(5) . ? C45 C46 1.386(5) . ? C46 C41 1.406(5) . ? C54 C55 1.390(5) . ? C54 C53 1.395(5) . ? C62 O61 1.318(4) . ? C62 C63 1.421(5) . ? C62 C67 1.424(5) . ? C63 C64 1.390(5) . ? C65 C66 1.368(5) . ? C65 C64 1.381(5) . ? C67 C66 1.427(5) . ? C67 C68 1.476(5) . ? C71 O711 1.246(4) . ? C71 N72 1.336(4) . ? C71 N70 1.396(5) . ? C82 C83 1.390(5) . ? C82 C81 1.406(5) . ? C83 C84 1.381(5) . ? C84 C85 1.379(5) . ? C85 C86 1.385(5) . ? C86 C81 1.379(5) . ? C92 C91 1.380(5) . ? C92 C93 1.381(5) . ? C93 C94 1.397(5) . ? C94 C95 1.384(5) . ? C95 C96 1.381(5) . ? C96 C91 1.400(5) . ? C101 C106 1.386(5) . ? C101 C102 1.389(5) . ? C101 P2 1.813(4) . ? C103 C104 1.376(5) . ? C103 C102 1.388(5) . ? C104 C105 1.389(5) . ? C105 C106 1.388(5) . ? C681 C68 1.481(5) . ? C12 O11 1.312(4) . ? C12 C17 1.444(5) . ? C17 C18 1.459(5) . ? C18 N19 1.292(4) . ? C18 C181 1.510(5) . ? C21 O22 1.246(4) . ? C21 N22 1.336(4) . ? C21 N20 1.377(4) . ? C31 P1 1.824(4) . ? C33 C34 1.391(5) . ? C41 P1 1.820(4) . ? C51 C52 1.387(5) . ? C51 C56 1.402(5) . ? C51 P1 1.822(3) . ? C52 C53 1.374(5) . ? C55 C56 1.385(5) . ? C68 N69 1.296(4) . ? C81 P2 1.824(3) . ? C91 P2 1.818(4) . ? O11 Pd1 1.984(2) . ? O61 Pd2 1.981(2) . ? Pd1 N22 1.976(3) . ? Pd1 N19 2.033(3) . ? Pd1 P1 2.2686(10) . ? Pd2 N72 1.967(3) . ? Pd2 N69 2.024(3) . ? Pd2 P2 2.2609(10) . ? N19 N20 1.386(4) . ? N69 N70 1.389(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 C14 C13 C12 123.0(3) . . ? C16 C15 C14 119.3(3) . . ? C15 C16 C17 124.9(3) . . ? C33 C32 C31 120.1(3) . . ? C34 C35 C36 120.1(3) . . ? C35 C36 C31 120.1(3) . . ? C41 C42 C43 121.5(3) . . ? C43 C44 C45 120.9(3) . . ? C46 C45 C44 119.1(4) . . ? C45 C46 C41 120.8(3) . . ? C55 C54 C53 120.7(3) . . ? O61 C62 C63 114.2(3) . . ? O61 C62 C67 126.9(3) . . ? C63 C62 C67 118.9(3) . . ? C64 C63 C62 121.8(4) . . ? C66 C65 C64 120.9(4) . . ? C62 C67 C66 117.0(3) . . ? C62 C67 C68 126.1(3) . . ? C66 C67 C68 116.9(3) . . ? O711 C71 N72 126.5(4) . . ? O711 C71 N70 119.2(3) . . ? N72 C71 N70 114.3(3) . . ? C83 C82 C81 119.1(3) . . ? C84 C83 C82 120.5(4) . . ? C85 C84 C83 120.4(3) . . ? C84 C85 C86 119.5(4) . . ? C81 C86 C85 121.0(3) . . ? C91 C92 C93 121.1(4) . . ? C92 C93 C94 120.0(3) . . ? C95 C94 C93 119.1(4) . . ? C96 C95 C94 120.6(4) . . ? C95 C96 C91 120.3(3) . . ? C106 C101 C102 118.1(3) . . ? C106 C101 P2 119.0(3) . . ? C102 C101 P2 122.8(3) . . ? C104 C103 C102 119.3(4) . . ? C103 C104 C105 120.7(4) . . ? C106 C105 C104 119.1(4) . . ? C101 C106 C105 121.4(3) . . ? O11 C12 C13 115.3(3) . . ? O11 C12 C17 127.0(3) . . ? C13 C12 C17 117.6(3) . . ? C15 C14 C13 119.5(3) . . ? C16 C17 C12 115.7(3) . . ? C16 C17 C18 119.1(3) . . ? C12 C17 C18 125.2(3) . . ? N19 C18 C17 121.7(3) . . ? N19 C18 C181 118.9(3) . . ? C17 C18 C181 119.4(3) . . ? O22 C21 N22 125.1(3) . . ? O22 C21 N20 119.8(3) . . ? N22 C21 N20 115.1(3) . . ? C32 C31 C36 119.4(3) . . ? C32 C31 P1 124.3(3) . . ? C36 C31 P1 116.2(3) . . ? C32 C33 C34 120.3(3) . . ? C35 C34 C33 119.9(3) . . ? C42 C41 C46 118.2(3) . . ? C42 C41 P1 120.0(3) . . ? C46 C41 P1 121.7(3) . . ? C44 C43 C42 119.4(3) . . ? C52 C51 C56 119.3(3) . . ? C52 C51 P1 118.6(3) . . ? C56 C51 P1 121.8(3) . . ? C53 C52 C51 120.1(4) . . ? C52 C53 C54 120.2(4) . . ? C56 C55 C54 118.6(3) . . ? C55 C56 C51 121.0(3) . . ? C65 C64 C63 119.0(4) . . ? C65 C66 C67 122.3(3) . . ? N69 C68 C67 119.8(3) . . ? N69 C68 C681 119.2(3) . . ? C67 C68 C681 120.9(3) . . ? C86 C81 C82 119.5(3) . . ? C86 C81 P2 122.2(3) . . ? C82 C81 P2 118.3(3) . . ? C92 C91 C96 118.8(3) . . ? C92 C91 P2 119.3(3) . . ? C96 C91 P2 121.9(3) . . ? C103 C102 C101 121.4(4) . . ? C12 O11 Pd1 124.4(2) . . ? C62 O61 Pd2 123.5(2) . . ? N22 Pd1 O11 172.97(11) . . ? N22 Pd1 N19 80.66(11) . . ? O11 Pd1 N19 92.59(10) . . ? N22 Pd1 P1 96.07(9) . . ? O11 Pd1 P1 90.64(7) . . ? N19 Pd1 P1 176.63(8) . . ? N72 Pd2 O61 173.23(11) . . ? N72 Pd2 N69 80.66(12) . . ? O61 Pd2 N69 92.87(11) . . ? N72 Pd2 P2 97.29(9) . . ? O61 Pd2 P2 89.16(8) . . ? N69 Pd2 P2 177.92(9) . . ? C18 N19 N20 121.3(3) . . ? C18 N19 Pd1 128.0(2) . . ? N20 N19 Pd1 110.35(19) . . ? C21 N20 N19 117.5(3) . . ? C21 N22 Pd1 115.2(2) . . ? C68 N69 N70 120.0(3) . . ? C68 N69 Pd2 128.6(2) . . ? N70 N69 Pd2 111.0(2) . . ? N69 N70 C71 116.8(3) . . ? C71 N72 Pd2 116.3(2) . . ? C41 P1 C51 102.81(16) . . ? C41 P1 C31 107.15(15) . . ? C51 P1 C31 103.51(15) . . ? C41 P1 Pd1 116.34(11) . . ? C51 P1 Pd1 114.08(11) . . ? C31 P1 Pd1 111.78(12) . . ? C101 P2 C91 104.78(16) . . ? C101 P2 C81 105.02(15) . . ? C91 P2 C81 103.70(16) . . ? C101 P2 Pd2 110.47(12) . . ? C91 P2 Pd2 115.94(12) . . ? C81 P2 Pd2 115.80(11) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.116 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.114