# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Forgan, Ross' 'Friedman, Douglas' 'Stern, Charlotte' 'Bruns, Carson' 'Stoddart, J.' _publ_contact_author_name 'Stoddart, J.' _publ_contact_author_email stoddart@northwestern.edu _publ_section_title ; Directed self-assembly of a ring-in-ring complex ; # Attachment '- 2-8PF6.cif' data_n0076 _database_code_depnum_ccdc_archive 'CCDC 772267' #TrackingRef '- 2-8PF6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H90 F48 N16 O P8 Pd2' _chemical_formula_weight 2496.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 8.719(2) _cell_length_b 13.919(3) _cell_length_c 22.991(6) _cell_angle_alpha 67.791(20) _cell_angle_beta 79.998(19) _cell_angle_gamma 76.088(19) _cell_volume 2496.7(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 246 _cell_measurement_theta_min 5.47 _cell_measurement_theta_max 58.02 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1250 _exptl_absorpt_coefficient_mu 5.383 _exptl_absorpt_correction_type 'Empirical, Twinabs (multi-scan)' _exptl_absorpt_correction_T_min 0.3759 _exptl_absorpt_correction_T_max 0.9000 _exptl_absorpt_process_details 'TWINABS V2008/1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6170 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1956 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.17 _diffrn_reflns_theta_max 66.27 _reflns_number_total 6170 _reflns_number_gt 3582 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V2.1-4 (Bruker, 2007)' _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The crystal under investigation was found to be non-merohedrally twinned. The orientation matrices for the two components were identified using the program Cell_Now (Sheldrick, 2005), and the data were processed using both orientation matrices with SAINT, The exact twin matrix identified by the integration program was found to be (-0.999 -0.001 0.000 / 0.002 -1.002 0.003 / -0.487 -1.172 1.002). The second domain is rotated from first domain by 179.9 deg about the reciprocal lattice c axis. The absorption correction was carried out using TWINABS (Sheldrick 2007) to create an hklf5 file which was used in all refinements; the structure was solved using direct methods with only the non-overlapping reflections of component 1. The twin fraction refined to a value of 0.387 (2). The data was collected to 0.9 angstroms there was virtually no diffraction passed that, since the mean I/sigma equaled 1.2 at 1.0 angstrom. Soft restraints were refined for C25 displacement parameter. ; _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^)+(0.1076P)^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 6170 _refine_ls_number_parameters 641 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1391 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.2187 _refine_ls_wR_factor_gt 0.1801 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 Pd1 Pd 0.3551(2) 0.30355(12) 0.37775(6) 0.0275(4) Uani 1 1 d . . . P1 P 0.7563(7) 0.4436(4) 0.8896(2) 0.0363(13) Uani 1 1 d . . . P2 P 0.3016(7) 0.9148(4) 0.9269(2) 0.0355(13) Uani 1 1 d . . . P3 P 0.1353(7) 0.9154(4) 0.6503(2) 0.0367(14) Uani 1 1 d . . . P4 P 0.1318(7) 0.4664(4) 0.6280(3) 0.0388(13) Uani 1 1 d . . . F1 F 0.9151(13) 0.4822(9) 0.8520(5) 0.043(3) Uani 1 1 d . . . F2 F 0.8557(14) 0.3621(9) 0.9475(5) 0.041(3) Uani 1 1 d . . . F3 F 0.5972(14) 0.4023(9) 0.9276(5) 0.046(3) Uani 1 1 d . . . F4 F 0.6603(14) 0.5259(9) 0.8311(5) 0.041(3) Uani 1 1 d . . . F5 F 0.7893(15) 0.3536(10) 0.8588(5) 0.051(3) Uani 1 1 d . . . F6 F 0.7236(15) 0.5299(8) 0.9213(5) 0.047(3) Uani 1 1 d . . . F7 F 0.4439(14) 0.8139(8) 0.9414(5) 0.047(3) Uani 1 1 d . . . F8 F 0.4148(15) 0.9829(9) 0.9373(6) 0.051(3) Uani 1 1 d . . . F9 F 0.1592(15) 1.0169(9) 0.9120(5) 0.045(3) Uani 1 1 d . . . F10 F 0.1881(15) 0.8484(9) 0.9179(5) 0.050(3) Uani 1 1 d . . . F11 F 0.3603(14) 0.9494(10) 0.8534(5) 0.045(3) Uani 1 1 d . . . F12 F 0.2426(15) 0.8816(9) 1.0002(5) 0.044(3) Uani 1 1 d . . . F13 F 0.3172(13) 0.9001(10) 0.6208(5) 0.049(3) Uani 1 1 d . . . F14 F 0.1987(15) 0.8643(10) 0.7192(5) 0.050(3) Uani 1 1 d . . . F15 F -0.0396(14) 0.9297(9) 0.6798(6) 0.048(3) Uani 1 1 d . . . F16 F 0.0787(15) 0.9656(9) 0.5801(5) 0.043(3) Uani 1 1 d . . . F17 F 0.1309(17) 0.8013(9) 0.6531(5) 0.053(3) Uani 1 1 d . . . F18 F 0.1436(16) 1.0320(9) 0.6456(5) 0.056(4) Uani 1 1 d . . . F19 F 0.3127(16) 0.4129(11) 0.6524(7) 0.065(4) Uani 1 1 d . . . F20 F 0.0597(18) 0.4119(11) 0.6975(5) 0.062(4) Uani 1 1 d . . . F21 F -0.0438(15) 0.5165(10) 0.6063(5) 0.050(3) Uani 1 1 d . . . F22 F 0.2059(17) 0.5218(11) 0.5599(5) 0.063(4) Uani 1 1 d . . . F23 F 0.1361(18) 0.3639(10) 0.6136(7) 0.070(4) Uani 1 1 d . . . F24 F 0.1327(14) 0.5669(9) 0.6449(5) 0.042(3) Uani 1 1 d . . . N1 N 0.299(2) 0.2762(12) 0.3033(6) 0.027(4) Uani 1 1 d . . . N2 N 0.1514(18) 0.1609(11) 0.0510(6) 0.024(4) Uani 1 1 d . . . N3 N 0.784(2) 0.8013(12) 0.0612(6) 0.029(4) Uani 1 1 d . . . N4 N 0.445(2) 0.4263(12) 0.3126(6) 0.028(4) Uani 1 1 d . . . N5 N 0.426(2) 0.3259(13) 0.4517(7) 0.034(4) Uani 1 1 d . . . N6 N 0.2594(19) 0.1797(12) 0.4452(6) 0.029(4) Uani 1 1 d . . . N7 N 0.198(3) 0.4542(16) 0.9344(8) 0.061(6) Uani 1 1 d . . . N8 N -0.187(3) 0.1424(16) 0.8126(13) 0.086(9) Uani 1 1 d . . . C1 C 0.160(3) 0.3148(14) 0.2808(8) 0.035(5) Uani 1 1 d . . . H1 H 0.0814 0.3578 0.2994 0.042 Uiso 1 1 calc R . . C2 C 0.123(2) 0.2946(14) 0.2312(8) 0.028(5) Uani 1 1 d . . . H2 H 0.0219 0.3239 0.2158 0.033 Uiso 1 1 calc R . . C3 C 0.236(2) 0.2315(14) 0.2037(7) 0.024(4) Uani 1 1 d . . . C4 C 0.386(3) 0.1943(16) 0.2265(8) 0.044(6) Uani 1 1 d . . . H4 H 0.4667 0.1544 0.2068 0.053 Uiso 1 1 calc R . . C5 C 0.419(3) 0.2145(17) 0.2776(8) 0.044(6) Uani 1 1 d . . . H5 H 0.5191 0.1870 0.2941 0.052 Uiso 1 1 calc R . . C6 C 0.204(3) 0.2041(15) 0.1522(8) 0.033(5) Uani 1 1 d . . . C7 C 0.116(3) 0.2831(16) 0.1023(8) 0.038(5) Uani 1 1 d . . . H7 H 0.0727 0.3517 0.1039 0.046 Uiso 1 1 calc R . . C8 C 0.095(2) 0.2584(16) 0.0530(8) 0.032(5) Uani 1 1 d . . . H8 H 0.0402 0.3110 0.0191 0.039 Uiso 1 1 calc R . . C9 C 0.223(2) 0.0842(14) 0.0999(8) 0.031(5) Uani 1 1 d . . . H9 H 0.2570 0.0143 0.0995 0.037 Uiso 1 1 calc R . . C10 C 0.247(2) 0.1076(15) 0.1515(8) 0.035(5) Uani 1 1 d . . . H10 H 0.2947 0.0527 0.1864 0.042 Uiso 1 1 calc R . . C11 C 0.131(2) 0.1340(15) -0.0031(7) 0.027(5) Uani 1 1 d . . . H11A H 0.0172 0.1477 -0.0088 0.033 Uiso 1 1 calc R . . H11B H 0.1746 0.0579 0.0050 0.033 Uiso 1 1 calc R . . C12 C 0.862(2) 0.7474(15) 0.1125(8) 0.032(5) Uani 1 1 d . . . H12 H 0.9682 0.7543 0.1119 0.038 Uiso 1 1 calc R . . C13 C 0.789(3) 0.6801(13) 0.1675(8) 0.034(6) Uani 1 1 d . . . H13 H 0.8442 0.6416 0.2041 0.041 Uiso 1 1 calc R . . C14 C 0.637(2) 0.6724(14) 0.1661(8) 0.021(4) Uani 1 1 d . . . C15 C 0.560(3) 0.7338(14) 0.1157(7) 0.033(5) Uani 1 1 d . . . H15 H 0.4510 0.7316 0.1170 0.040 Uiso 1 1 calc R . . C16 C 0.629(3) 0.8001(14) 0.0619(7) 0.029(5) Uani 1 1 d . . . H16 H 0.5704 0.8431 0.0267 0.034 Uiso 1 1 calc R . . C17 C 0.572(2) 0.5862(14) 0.2190(8) 0.031(5) Uani 1 1 d . . . C18 C 0.417(2) 0.6051(14) 0.2443(7) 0.023(4) Uani 1 1 d . . . H18 H 0.3526 0.6734 0.2296 0.028 Uiso 1 1 calc R . . C19 C 0.359(2) 0.5235(13) 0.2910(7) 0.029(5) Uani 1 1 d . . . H19 H 0.2530 0.5367 0.3089 0.035 Uiso 1 1 calc R . . C20 C 0.600(2) 0.4075(16) 0.2875(7) 0.027(5) Uani 1 1 d . . . H20 H 0.6650 0.3394 0.3029 0.032 Uiso 1 1 calc R . . C21 C 0.660(2) 0.4888(16) 0.2399(8) 0.030(4) Uani 1 1 d . . . H21 H 0.7652 0.4755 0.2215 0.036 Uiso 1 1 calc R . . C22 C 0.332(3) 0.2629(17) 0.5101(8) 0.041(5) Uani 1 1 d . . . H22A H 0.3826 0.2504 0.5483 0.049 Uiso 1 1 calc R . . H22B H 0.2226 0.3028 0.5135 0.049 Uiso 1 1 calc R . . C23 C 0.329(3) 0.1609(18) 0.5048(9) 0.054(7) Uani 1 1 d . . . H23A H 0.2644 0.1203 0.5417 0.065 Uiso 1 1 calc R . . H23B H 0.4381 0.1190 0.5046 0.065 Uiso 1 1 calc R . . C24 C 0.600(3) 0.2849(18) 0.4537(10) 0.053(7) Uani 1 1 d . . . H24A H 0.6557 0.3261 0.4149 0.079 Uiso 1 1 calc R . . H24B H 0.6229 0.2105 0.4573 0.079 Uiso 1 1 calc R . . H24C H 0.6347 0.2910 0.4902 0.079 Uiso 1 1 calc R . . C25 C 0.391(3) 0.4371(15) 0.4488(8) 0.036(5) Uani 1 1 d U . . H25A H 0.4282 0.4405 0.4857 0.053 Uiso 1 1 calc R . . H25B H 0.2763 0.4640 0.4486 0.053 Uiso 1 1 calc R . . H25C H 0.4454 0.4802 0.4103 0.053 Uiso 1 1 calc R . . C26 C 0.299(3) 0.0801(17) 0.4281(10) 0.049(6) Uani 1 1 d . . . H26A H 0.3872 0.0306 0.4516 0.074 Uiso 1 1 calc R . . H26B H 0.3308 0.0989 0.3828 0.074 Uiso 1 1 calc R . . H26C H 0.2062 0.0469 0.4391 0.074 Uiso 1 1 calc R . . C27 C 0.085(2) 0.2163(16) 0.4517(10) 0.040(5) Uani 1 1 d . . . H27A H 0.0377 0.1643 0.4882 0.060 Uiso 1 1 calc R . . H27B H 0.0403 0.2243 0.4134 0.060 Uiso 1 1 calc R . . H27C H 0.0610 0.2845 0.4579 0.060 Uiso 1 1 calc R . . C28 C 0.257(3) 0.5232(19) 0.9277(9) 0.045(6) Uani 1 1 d . . . C29 C 0.340(4) 0.608(2) 0.9171(12) 0.075(9) Uani 1 1 d . . . H29A H 0.4308 0.6045 0.8855 0.112 Uiso 1 1 calc R . . H29B H 0.3779 0.5995 0.9567 0.112 Uiso 1 1 calc R . . H29C H 0.2679 0.6758 0.9018 0.112 Uiso 1 1 calc R . . C30 C -0.065(4) 0.1397(19) 0.7884(11) 0.058(7) Uani 1 1 d . . . C31 C 0.081(3) 0.1356(18) 0.7563(11) 0.070(8) Uani 1 1 d . . . H31A H 0.1293 0.1916 0.7572 0.105 Uiso 1 1 calc R . . H31B H 0.0714 0.1456 0.7124 0.105 Uiso 1 1 calc R . . H31C H 0.1477 0.0666 0.7760 0.105 Uiso 1 1 calc R . . O1 O 0.621(3) 0.174(2) 0.6203(13) 0.043(7) Uiso 0.50 1 d P . . C32 C 0.520(12) 0.162(7) 0.721(4) 0.18(4) Uiso 0.50 1 d PD . . H32A H 0.5655 0.2258 0.6978 0.270 Uiso 0.50 1 calc PR . . H32B H 0.5750 0.1196 0.7585 0.270 Uiso 0.50 1 calc PR . . H32C H 0.4070 0.1828 0.7327 0.270 Uiso 0.50 1 calc PR . . C33 C 0.539(7) 0.099(5) 0.679(3) 0.080(17) Uiso 0.50 1 d PD . . H33A H 0.4362 0.0909 0.6707 0.097 Uiso 0.50 1 calc PR . . H33B H 0.6079 0.0285 0.6959 0.097 Uiso 0.50 1 calc PR . . C34 C 0.760(5) 0.181(3) 0.619(2) 0.043(9) Uiso 0.50 1 d P . . H34A H 0.8197 0.1747 0.5795 0.052 Uiso 0.50 1 calc PR . . H34B H 0.8101 0.1213 0.6548 0.052 Uiso 0.50 1 calc PR . . C35 C 0.770(6) 0.273(4) 0.623(3) 0.070(14) Uiso 0.50 1 d P . . H35A H 0.6733 0.3248 0.6101 0.105 Uiso 0.50 1 calc PR . . H35B H 0.8620 0.2990 0.5958 0.105 Uiso 0.50 1 calc PR . . H35C H 0.7831 0.2619 0.6670 0.105 Uiso 0.50 1 calc PR . . 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 0.0394(10) 0.0237(7) 0.0213(6) -0.0083(6) 0.0022(7) -0.0123(6) P1 0.043(4) 0.033(3) 0.033(3) -0.009(2) -0.005(2) -0.012(3) P2 0.046(4) 0.027(3) 0.035(3) -0.014(2) 0.001(2) -0.009(3) P3 0.041(4) 0.029(3) 0.035(3) -0.007(2) 0.003(2) -0.010(3) P4 0.043(4) 0.037(3) 0.042(3) -0.024(3) 0.000(3) -0.004(3) F1 0.026(7) 0.036(7) 0.054(7) -0.008(5) 0.001(5) 0.001(6) F2 0.040(8) 0.043(7) 0.035(6) -0.001(5) -0.010(5) -0.017(6) F3 0.042(8) 0.046(7) 0.053(7) -0.016(6) -0.006(5) -0.016(6) F4 0.041(8) 0.036(7) 0.047(6) -0.020(5) -0.011(5) 0.005(5) F5 0.051(9) 0.062(8) 0.046(6) -0.031(6) -0.019(6) 0.007(7) F6 0.069(10) 0.029(6) 0.050(7) -0.014(5) -0.013(6) -0.017(6) F7 0.048(8) 0.027(6) 0.069(7) -0.012(5) -0.007(6) -0.018(6) F8 0.054(9) 0.040(7) 0.073(8) -0.035(6) 0.002(6) -0.019(6) F9 0.061(9) 0.036(7) 0.038(6) -0.014(5) -0.011(5) -0.003(6) F10 0.054(9) 0.050(8) 0.064(7) -0.036(6) 0.009(6) -0.026(7) F11 0.044(9) 0.044(7) 0.051(6) -0.026(6) -0.001(5) -0.004(6) F12 0.037(8) 0.052(8) 0.039(6) -0.016(5) 0.004(4) -0.007(6) F13 0.040(8) 0.073(9) 0.036(5) -0.019(6) 0.010(6) -0.026(6) F14 0.046(8) 0.062(9) 0.040(6) -0.016(6) -0.004(5) -0.011(7) F15 0.037(8) 0.031(7) 0.061(7) -0.006(6) 0.001(6) 0.001(6) F16 0.041(8) 0.034(7) 0.041(6) 0.004(5) -0.018(5) -0.004(6) F17 0.077(11) 0.028(7) 0.052(7) -0.008(5) 0.002(6) -0.020(7) F18 0.090(11) 0.030(7) 0.055(7) -0.026(5) 0.021(6) -0.024(7) F19 0.030(8) 0.045(8) 0.120(11) -0.021(7) -0.034(7) 0.001(6) F20 0.085(11) 0.058(9) 0.034(6) -0.003(6) 0.005(6) -0.026(8) F21 0.053(9) 0.052(8) 0.046(7) -0.010(5) -0.013(5) -0.016(7) F22 0.080(11) 0.080(10) 0.047(7) -0.039(7) 0.033(7) -0.047(8) F23 0.094(12) 0.060(9) 0.089(10) -0.050(8) 0.007(8) -0.047(9) F24 0.048(9) 0.025(6) 0.056(7) -0.024(5) 0.015(5) -0.009(5) N1 0.041(12) 0.023(9) 0.013(7) -0.012(6) 0.007(7) 0.004(8) N2 0.029(10) 0.027(9) 0.018(7) -0.013(6) 0.013(6) -0.012(7) N3 0.048(13) 0.033(9) 0.010(7) -0.008(6) 0.003(7) -0.019(9) N4 0.049(13) 0.027(9) 0.010(7) 0.000(6) 0.001(7) -0.024(9) N5 0.043(13) 0.027(9) 0.032(8) -0.002(7) -0.003(8) -0.018(9) N6 0.031(11) 0.033(9) 0.027(8) -0.016(7) 0.008(7) -0.013(8) N7 0.092(19) 0.052(14) 0.038(10) -0.011(9) 0.004(10) -0.025(13) N8 0.09(2) 0.019(11) 0.11(2) 0.007(12) -0.003(17) 0.012(12) C1 0.053(17) 0.015(10) 0.026(9) -0.004(8) 0.000(9) 0.003(10) C2 0.040(14) 0.023(10) 0.021(9) -0.002(7) -0.003(8) -0.016(9) C3 0.014(11) 0.034(11) 0.029(9) -0.016(8) 0.002(8) -0.010(9) C4 0.08(2) 0.038(12) 0.026(10) -0.028(9) 0.012(10) -0.021(12) C5 0.058(17) 0.053(14) 0.022(9) -0.017(9) 0.012(9) -0.020(12) C6 0.046(15) 0.028(11) 0.034(10) -0.017(8) 0.021(9) -0.029(10) C7 0.056(17) 0.029(11) 0.030(10) -0.014(8) -0.003(9) -0.001(11) C8 0.029(13) 0.040(12) 0.031(9) -0.014(8) 0.003(8) -0.013(10) C9 0.044(15) 0.020(10) 0.026(9) -0.006(7) 0.007(8) -0.010(9) C10 0.039(14) 0.028(11) 0.026(9) -0.003(8) -0.012(8) 0.010(10) C11 0.038(14) 0.033(11) 0.016(8) -0.014(7) 0.003(7) -0.011(9) C12 0.036(14) 0.032(11) 0.031(10) -0.012(8) 0.001(9) -0.016(10) C13 0.063(18) 0.008(9) 0.025(9) -0.003(7) 0.000(9) -0.006(10) C14 0.008(12) 0.025(10) 0.034(10) -0.014(8) 0.000(8) -0.004(9) C15 0.058(16) 0.022(10) 0.023(9) -0.012(8) 0.004(9) -0.015(10) C16 0.052(17) 0.018(10) 0.018(8) -0.005(7) -0.019(9) -0.002(9) C17 0.037(14) 0.021(10) 0.033(10) -0.006(8) -0.010(9) -0.005(9) C18 0.009(11) 0.029(10) 0.031(9) -0.014(8) -0.001(7) 0.001(8) C19 0.026(13) 0.021(10) 0.025(9) 0.000(7) -0.004(8) 0.009(9) C20 0.026(13) 0.037(11) 0.019(9) -0.014(8) 0.002(8) -0.007(9) C21 0.017(12) 0.033(11) 0.037(10) -0.010(8) 0.001(8) -0.007(9) C22 0.031(14) 0.059(14) 0.031(10) -0.017(9) 0.010(8) -0.013(11) C23 0.076(19) 0.063(16) 0.025(10) 0.003(10) -0.006(10) -0.046(14) C24 0.06(2) 0.053(16) 0.051(14) -0.012(11) -0.008(12) -0.036(15) C25 0.052(10) 0.031(8) 0.039(8) -0.026(6) -0.007(7) -0.012(7) C26 0.049(16) 0.042(13) 0.055(13) 0.001(10) -0.019(11) -0.025(12) C27 0.012(12) 0.034(12) 0.064(13) -0.005(10) 0.004(10) -0.012(10) C28 0.046(17) 0.045(14) 0.041(12) -0.016(10) 0.017(10) -0.017(13) C29 0.09(3) 0.07(2) 0.10(2) -0.062(17) 0.021(17) -0.053(18) C30 0.08(2) 0.036(14) 0.050(14) -0.009(11) -0.008(14) -0.010(15) C31 0.10(2) 0.034(14) 0.061(15) -0.011(11) 0.015(16) -0.005(14) _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 N4 2.020(13) . ? Pd1 N1 2.046(14) . ? Pd1 N5 2.055(16) . ? Pd1 N6 2.072(15) . ? P1 F6 1.575(12) . ? P1 F1 1.595(13) . ? P1 F5 1.606(12) . ? P1 F4 1.608(11) . ? P1 F2 1.612(11) . ? P1 F3 1.613(13) . ? P2 F10 1.591(12) . ? P2 F12 1.595(11) . ? P2 F11 1.598(12) . ? P2 F7 1.605(13) . ? P2 F9 1.615(13) . ? P2 F8 1.622(12) . ? P3 F15 1.557(13) . ? P3 F17 1.574(13) . ? P3 F18 1.603(12) . ? P3 F14 1.607(12) . ? P3 F16 1.610(11) . ? P3 F13 1.611(13) . ? P4 F22 1.562(12) . ? P4 F23 1.572(12) . ? P4 F20 1.578(13) . ? P4 F24 1.590(12) . ? P4 F21 1.602(14) . ? P4 F19 1.669(14) . ? N1 C1 1.31(3) . ? N1 C5 1.38(3) . ? N2 C8 1.34(2) . ? N2 C9 1.34(2) . ? N2 C11 1.48(2) . ? N3 C12 1.33(2) . ? N3 C16 1.35(2) . ? N3 C11 1.49(2) 2_665 ? N4 C19 1.33(2) . ? N4 C20 1.38(2) . ? N5 C25 1.48(2) . ? N5 C24 1.49(3) . ? N5 C22 1.52(2) . ? N6 C27 1.49(2) . ? N6 C23 1.50(2) . ? N6 C26 1.53(3) . ? N7 C28 1.15(3) . ? N8 C30 1.11(3) . ? C1 C2 1.37(3) . ? C1 H1 0.9500 . ? C2 C3 1.39(3) . ? C2 H2 0.9500 . ? C3 C4 1.40(3) . ? C3 C6 1.46(2) . ? C4 C5 1.40(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C10 1.31(3) . ? C6 C7 1.44(3) . ? C7 C8 1.35(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.40(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 N3 1.49(2) 2_665 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.41(3) . ? C12 H12 0.9500 . ? C13 C14 1.36(3) . ? C13 H13 0.9500 . ? C14 C15 1.33(3) . ? C14 C17 1.49(2) . ? C15 C16 1.38(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C21 1.34(3) . ? C17 C18 1.37(3) . ? C18 C19 1.37(2) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.38(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.48(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.45(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.36(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? O1 C34 1.23(4) . ? O1 C33 1.54(6) . ? C32 C33 1.494(11) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.35(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? 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 Pd1 N1 86.4(5) . . ? N4 Pd1 N5 93.1(6) . . ? N1 Pd1 N5 176.4(7) . . ? N4 Pd1 N6 178.9(7) . . ? N1 Pd1 N6 94.1(6) . . ? N5 Pd1 N6 86.5(6) . . ? F6 P1 F1 91.0(7) . . ? F6 P1 F5 178.7(7) . . ? F1 P1 F5 89.8(7) . . ? F6 P1 F4 90.4(6) . . ? F1 P1 F4 88.9(6) . . ? F5 P1 F4 90.6(6) . . ? F6 P1 F2 89.4(6) . . ? F1 P1 F2 89.9(6) . . ? F5 P1 F2 89.5(6) . . ? F4 P1 F2 178.8(7) . . ? F6 P1 F3 90.0(7) . . ? F1 P1 F3 178.9(7) . . ? F5 P1 F3 89.3(7) . . ? F4 P1 F3 91.6(7) . . ? F2 P1 F3 89.5(6) . . ? F10 P2 F12 90.3(6) . . ? F10 P2 F11 90.1(6) . . ? F12 P2 F11 179.4(7) . . ? F10 P2 F7 91.1(7) . . ? F12 P2 F7 90.3(7) . . ? F11 P2 F7 90.2(7) . . ? F10 P2 F9 89.2(7) . . ? F12 P2 F9 90.1(7) . . ? F11 P2 F9 89.5(7) . . ? F7 P2 F9 179.6(8) . . ? F10 P2 F8 178.8(7) . . ? F12 P2 F8 88.7(7) . . ? F11 P2 F8 90.9(7) . . ? F7 P2 F8 89.5(7) . . ? F9 P2 F8 90.3(7) . . ? F15 P3 F17 91.3(7) . . ? F15 P3 F18 90.2(7) . . ? F17 P3 F18 178.3(7) . . ? F15 P3 F14 91.0(7) . . ? F17 P3 F14 89.2(7) . . ? F18 P3 F14 91.7(7) . . ? F15 P3 F16 91.2(7) . . ? F17 P3 F16 90.5(7) . . ? F18 P3 F16 88.6(7) . . ? F14 P3 F16 177.8(7) . . ? F15 P3 F13 179.2(8) . . ? F17 P3 F13 88.8(7) . . ? F18 P3 F13 89.8(7) . . ? F14 P3 F13 88.3(7) . . ? F16 P3 F13 89.6(7) . . ? F22 P4 F23 91.7(8) . . ? F22 P4 F20 178.4(8) . . ? F23 P4 F20 89.6(8) . . ? F22 P4 F24 89.5(6) . . ? F23 P4 F24 177.4(9) . . ? F20 P4 F24 89.1(7) . . ? F22 P4 F21 91.0(7) . . ? F23 P4 F21 92.0(8) . . ? F20 P4 F21 89.9(7) . . ? F24 P4 F21 90.2(7) . . ? F22 P4 F19 90.4(8) . . ? F23 P4 F19 88.0(8) . . ? F20 P4 F19 88.7(8) . . ? F24 P4 F19 89.7(7) . . ? F21 P4 F19 178.6(8) . . ? C1 N1 C5 121.9(16) . . ? C1 N1 Pd1 122.8(12) . . ? C5 N1 Pd1 115.3(14) . . ? C8 N2 C9 120.1(15) . . ? C8 N2 C11 121.4(15) . . ? C9 N2 C11 118.4(15) . . ? C12 N3 C16 121.2(14) . . ? C12 N3 C11 119.0(17) . 2_665 ? C16 N3 C11 119.8(14) . 2_665 ? C19 N4 C20 118.7(15) . . ? C19 N4 Pd1 122.7(13) . . ? C20 N4 Pd1 118.5(13) . . ? C25 N5 C24 109.1(16) . . ? C25 N5 C22 107.9(16) . . ? C24 N5 C22 111.8(15) . . ? C25 N5 Pd1 114.9(11) . . ? C24 N5 Pd1 108.2(12) . . ? C22 N5 Pd1 105.0(12) . . ? C27 N6 C23 110.4(16) . . ? C27 N6 C26 110.4(16) . . ? C23 N6 C26 111.1(16) . . ? C27 N6 Pd1 107.5(11) . . ? C23 N6 Pd1 104.7(11) . . ? C26 N6 Pd1 112.7(11) . . ? N1 C1 C2 121.9(18) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 119.7(19) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 117.7(15) . . ? C2 C3 C6 122.5(18) . . ? C4 C3 C6 119.8(16) . . ? C5 C4 C3 121.4(19) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? N1 C5 C4 117(2) . . ? N1 C5 H5 121.4 . . ? C4 C5 H5 121.4 . . ? C10 C6 C7 118.4(18) . . ? C10 C6 C3 121.9(19) . . ? C7 C6 C3 119.6(17) . . ? C8 C7 C6 118.9(19) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? N2 C8 C7 121.2(18) . . ? N2 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? N2 C9 C10 119.9(17) . . ? N2 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C6 C10 C9 121.0(17) . . ? C6 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? N2 C11 N3 109.7(14) . 2_665 ? N2 C11 H11A 109.7 . . ? N3 C11 H11A 109.7 2_665 . ? N2 C11 H11B 109.7 . . ? N3 C11 H11B 109.7 2_665 . ? H11A C11 H11B 108.2 . . ? N3 C12 C13 120.8(19) . . ? N3 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 117.6(17) . . ? C14 C13 H13 121.2 . . ? C12 C13 H13 121.2 . . ? C15 C14 C13 119.4(17) . . ? C15 C14 C17 123.0(18) . . ? C13 C14 C17 117.2(16) . . ? C14 C15 C16 123(2) . . ? C14 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? N3 C16 C15 117.1(16) . . ? N3 C16 H16 121.5 . . ? C15 C16 H16 121.5 . . ? C21 C17 C18 119.5(17) . . ? C21 C17 C14 120.4(18) . . ? C18 C17 C14 120.0(16) . . ? C19 C18 C17 118.6(17) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? N4 C19 C18 122.7(17) . . ? N4 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C21 C20 N4 119.1(18) . . ? C21 C20 H20 120.4 . . ? N4 C20 H20 120.4 . . ? C17 C21 C20 121.3(19) . . ? C17 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C23 C22 N5 108.8(16) . . ? C23 C22 H22A 109.9 . . ? N5 C22 H22A 109.9 . . ? C23 C22 H22B 109.9 . . ? N5 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C22 C23 N6 110.0(17) . . ? C22 C23 H23A 109.7 . . ? N6 C23 H23A 109.7 . . ? C22 C23 H23B 109.7 . . ? N6 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? N5 C24 H24A 109.5 . . ? N5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 H25A 109.5 . . ? N5 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N5 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N6 C26 H26A 109.5 . . ? N6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N6 C27 H27A 109.5 . . ? N6 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N6 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N7 C28 C29 176(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N8 C30 C31 177(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 O1 C33 121(4) . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C32 C33 O1 97(6) . . ? C32 C33 H33A 112.3 . . ? O1 C33 H33A 112.3 . . ? C32 C33 H33B 112.3 . . ? O1 C33 H33B 112.3 . . ? H33A C33 H33B 109.9 . . ? O1 C34 C35 112(4) . . ? O1 C34 H34A 109.3 . . ? C35 C34 H34A 109.3 . . ? O1 C34 H34B 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Pd1 N1 C1 -93.7(15) . . . . ? N5 Pd1 N1 C1 -176(9) . . . . ? N6 Pd1 N1 C1 85.3(15) . . . . ? N4 Pd1 N1 C5 85.9(14) . . . . ? N5 Pd1 N1 C5 4(11) . . . . ? N6 Pd1 N1 C5 -95.1(14) . . . . ? N1 Pd1 N4 C19 90.6(14) . . . . ? N5 Pd1 N4 C19 -93.0(14) . . . . ? N6 Pd1 N4 C19 -23(36) . . . . ? N1 Pd1 N4 C20 -86.7(13) . . . . ? N5 Pd1 N4 C20 89.8(14) . . . . ? N6 Pd1 N4 C20 160(35) . . . . ? N4 Pd1 N5 C25 45.8(14) . . . . ? N1 Pd1 N5 C25 128(10) . . . . ? N6 Pd1 N5 C25 -133.2(14) . . . . ? N4 Pd1 N5 C24 -76.3(12) . . . . ? N1 Pd1 N5 C24 6(11) . . . . ? N6 Pd1 N5 C24 104.7(12) . . . . ? N4 Pd1 N5 C22 164.2(13) . . . . ? N1 Pd1 N5 C22 -114(10) . . . . ? N6 Pd1 N5 C22 -14.8(13) . . . . ? N4 Pd1 N6 C27 34(36) . . . . ? N1 Pd1 N6 C27 -79.5(13) . . . . ? N5 Pd1 N6 C27 104.1(13) . . . . ? N4 Pd1 N6 C23 -84(35) . . . . ? N1 Pd1 N6 C23 163.1(14) . . . . ? N5 Pd1 N6 C23 -13.3(14) . . . . ? N4 Pd1 N6 C26 155(35) . . . . ? N1 Pd1 N6 C26 42.3(14) . . . . ? N5 Pd1 N6 C26 -134.1(14) . . . . ? C5 N1 C1 C2 1(3) . . . . ? Pd1 N1 C1 C2 -179.3(13) . . . . ? N1 C1 C2 C3 0(3) . . . . ? C1 C2 C3 C4 -3(3) . . . . ? C1 C2 C3 C6 177.9(17) . . . . ? C2 C3 C4 C5 4(3) . . . . ? C6 C3 C4 C5 -176.8(18) . . . . ? C1 N1 C5 C4 0(3) . . . . ? Pd1 N1 C5 C4 -179.7(15) . . . . ? C3 C4 C5 N1 -2(3) . . . . ? C2 C3 C6 C10 -136(2) . . . . ? C4 C3 C6 C10 45(3) . . . . ? C2 C3 C6 C7 41(3) . . . . ? C4 C3 C6 C7 -138(2) . . . . ? C10 C6 C7 C8 -7(3) . . . . ? C3 C6 C7 C8 175.9(18) . . . . ? C9 N2 C8 C7 3(3) . . . . ? C11 N2 C8 C7 -179.1(17) . . . . ? C6 C7 C8 N2 2(3) . . . . ? C8 N2 C9 C10 -4(3) . . . . ? C11 N2 C9 C10 178.7(17) . . . . ? C7 C6 C10 C9 7(3) . . . . ? C3 C6 C10 C9 -176.2(18) . . . . ? N2 C9 C10 C6 -2(3) . . . . ? C8 N2 C11 N3 63(2) . . . 2_665 ? C9 N2 C11 N3 -119.6(17) . . . 2_665 ? C16 N3 C12 C13 5(3) . . . . ? C11 N3 C12 C13 -176.3(16) 2_665 . . . ? N3 C12 C13 C14 0(3) . . . . ? C12 C13 C14 C15 -5(2) . . . . ? C12 C13 C14 C17 168.3(17) . . . . ? C13 C14 C15 C16 5(3) . . . . ? C17 C14 C15 C16 -167.9(17) . . . . ? C12 N3 C16 C15 -6(2) . . . . ? C11 N3 C16 C15 176.2(16) 2_665 . . . ? C14 C15 C16 N3 0(3) . . . . ? C15 C14 C17 C21 130(2) . . . . ? C13 C14 C17 C21 -43(2) . . . . ? C15 C14 C17 C18 -47(3) . . . . ? C13 C14 C17 C18 140.1(18) . . . . ? C21 C17 C18 C19 1(3) . . . . ? C14 C17 C18 C19 177.5(16) . . . . ? C20 N4 C19 C18 1(3) . . . . ? Pd1 N4 C19 C18 -176.0(13) . . . . ? C17 C18 C19 N4 -1(3) . . . . ? C19 N4 C20 C21 -2(3) . . . . ? Pd1 N4 C20 C21 175.5(13) . . . . ? C18 C17 C21 C20 -2(3) . . . . ? C14 C17 C21 C20 -178.2(17) . . . . ? N4 C20 C21 C17 2(3) . . . . ? C25 N5 C22 C23 164.5(17) . . . . ? C24 N5 C22 C23 -76(2) . . . . ? Pd1 N5 C22 C23 41.5(19) . . . . ? N5 C22 C23 N6 -57(2) . . . . ? C27 N6 C23 C22 -74(2) . . . . ? C26 N6 C23 C22 162.8(17) . . . . ? Pd1 N6 C23 C22 40.9(19) . . . . ? C34 O1 C33 C32 73(6) . . . . ? C33 O1 C34 C35 -108(5) . . . . ? _diffrn_measured_fraction_theta_max 0.662 _diffrn_reflns_theta_full 66.27 _diffrn_measured_fraction_theta_full 0.662 _refine_diff_density_max 0.911 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.175 # Attachment '- 4-8PF6.cif' data_n0075 _database_code_depnum_ccdc_archive 'CCDC 772268' #TrackingRef '- 4-8PF6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C297 H380 F96 N38 O64 P16 Pd4' _chemical_formula_weight 8251.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 19.0335(6) _cell_length_b 21.1652(7) _cell_length_c 26.7873(8) _cell_angle_alpha 72.664(2) _cell_angle_beta 79.146(2) _cell_angle_gamma 71.025(2) _cell_volume 9691.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3423 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 53.74 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.822 _exptl_crystal_size_mid 0.263 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4228 _exptl_absorpt_coefficient_mu 3.133 _exptl_absorpt_correction_type 'Empirical, Twinabs (multi-scan)' _exptl_absorpt_correction_T_min 0.516163 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'TWINABS V2008/1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27227 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 54.59 _reflns_number_total 27227 _reflns_number_gt 17398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V2.1-4 (Bruker, 2007)' _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Chemically equivalent, but not symmetry equivalent O15 - C135 atoms were restrained so that bond distances and angles were similar to O1 - C91. Rigid bond restraints (esd 0.01) were imposed on the displacement parameters as well as restraints on similar amplitudes (esd 0.05) separated by less than 1.7 Ang. The crystal under investigation was found to be non-merohedrally twinned. The orientation matrices for the two components were identified using the program Cell_Now (Sheldrick, 2005), and the data were processed using both orientation matrices with SAINT, The exact twin matrix identified by the integration program was found to be (-1.000 0.001 - 0.001 / 0.003 - 1.000 0.001 / 0.669 0.006 1.000). The second domain is rotated from first domain by 180 about the reciprocal lattice c axis. The absorption correction was carried out using TWINABS (Sheldrick 2007) to create an hklf5 file which was used in all refinements; the structure was solved using direct methods with only the non-overlapping reflections of component 1. The twin fraction refined to a value of 0.224 (2). The hydrogen atoms on the water molecules were not found. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 27227 _refine_ls_number_parameters 2345 _refine_ls_number_restraints 3777 _refine_ls_R_factor_all 0.1690 _refine_ls_R_factor_gt 0.1125 _refine_ls_wR_factor_ref 0.3507 _refine_ls_wR_factor_gt 0.3009 _refine_ls_goodness_of_fit_ref 1.262 _refine_ls_restrained_S_all 1.212 _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 0.66558(4) 0.83066(4) 0.04531(3) 0.0413(3) Uani 1 1 d U . . N1 N 0.6551(5) 0.9159(4) 0.0677(4) 0.048(2) Uani 1 1 d U . . H1A H 0.6642 0.9040 0.1015 0.058 Uiso 1 1 calc R . . H1B H 0.6890 0.9370 0.0481 0.058 Uiso 1 1 calc R . . N2 N 0.5508(5) 0.8638(4) 0.0519(4) 0.0444(19) Uani 1 1 d U . . H2A H 0.5343 0.8767 0.0200 0.053 Uiso 1 1 calc R . . H2B H 0.5321 0.8294 0.0722 0.053 Uiso 1 1 calc R . . N3 N 0.7808(4) 0.8021(3) 0.0378(3) 0.0300(15) Uani 1 1 d U . . N4 N 0.6679(4) 0.7418(4) 0.0300(3) 0.0377(17) Uani 1 1 d U . . N5 N 1.1732(4) 0.6844(4) 0.0140(3) 0.0338(17) Uani 1 1 d U . . N6 N 0.7237(4) 0.4119(4) -0.0034(3) 0.0343(17) Uani 1 1 d U . . C1 C 0.5812(7) 0.9630(6) 0.0617(6) 0.065(3) Uani 1 1 d U . . H1C H 0.5781 0.9909 0.0257 0.078 Uiso 1 1 calc R . . H1D H 0.5702 0.9938 0.0846 0.078 Uiso 1 1 calc R . . C2 C 0.5263(7) 0.9226(6) 0.0757(6) 0.066(3) Uani 1 1 d U . . H2C H 0.5194 0.9057 0.1136 0.079 Uiso 1 1 calc R . . H2D H 0.4786 0.9526 0.0639 0.079 Uiso 1 1 calc R . . C3 C 0.8180(6) 0.8217(5) -0.0089(4) 0.039(2) Uani 1 1 d U . . H3 H 0.7918 0.8496 -0.0374 0.047 Uiso 1 1 calc R . . C4 C 0.8938(5) 0.8013(5) -0.0151(3) 0.035(2) Uani 1 1 d U . . H4 H 0.9191 0.8153 -0.0478 0.042 Uiso 1 1 calc R . . C5 C 0.9344(5) 0.7590(4) 0.0277(3) 0.0298(18) Uani 1 1 d U . . C6 C 0.8930(5) 0.7414(5) 0.0757(4) 0.039(2) Uani 1 1 d U . . H6 H 0.9171 0.7145 0.1054 0.047 Uiso 1 1 calc R . . C7 C 0.8180(5) 0.7635(5) 0.0789(4) 0.036(2) Uani 1 1 d U . . H7 H 0.7911 0.7514 0.1113 0.043 Uiso 1 1 calc R . . C8 C 1.0173(5) 0.7330(4) 0.0225(3) 0.0287(18) Uani 1 1 d U . . C9 C 1.0598(5) 0.7321(5) -0.0276(4) 0.0300(19) Uani 1 1 d U . . H9 H 1.0356 0.7482 -0.0580 0.036 Uiso 1 1 calc R . . C10 C 1.1337(5) 0.7082(5) -0.0306(4) 0.035(2) Uani 1 1 d U . . H10 H 1.1604 0.7072 -0.0633 0.043 Uiso 1 1 calc R . . C11 C 1.1323(5) 0.6851(4) 0.0618(4) 0.032(2) Uani 1 1 d U . . H11 H 1.1574 0.6692 0.0917 0.039 Uiso 1 1 calc R . . C12 C 1.0572(5) 0.7078(4) 0.0672(3) 0.0277(18) Uani 1 1 d U . . H12 H 1.0315 0.7068 0.1004 0.033 Uiso 1 1 calc R . . C13 C 0.6575(6) 0.7364(5) -0.0155(4) 0.048(2) Uani 1 1 d U . . H13 H 0.6463 0.7761 -0.0428 0.058 Uiso 1 1 calc R . . C14 C 0.6624(6) 0.6737(5) -0.0243(4) 0.050(2) Uani 1 1 d U . . H14 H 0.6550 0.6721 -0.0572 0.059 Uiso 1 1 calc R . . C15 C 0.6780(5) 0.6141(5) 0.0152(4) 0.037(2) Uani 1 1 d U . . C16 C 0.6867(8) 0.6217(5) 0.0630(4) 0.059(3) Uani 1 1 d U . . H16 H 0.6950 0.5836 0.0919 0.070 Uiso 1 1 calc R . . C17 C 0.6834(8) 0.6841(5) 0.0680(4) 0.061(3) Uani 1 1 d U . . H17 H 0.6924 0.6869 0.1001 0.074 Uiso 1 1 calc R . . C18 C 0.6901(5) 0.5441(5) 0.0082(4) 0.0339(19) Uani 1 1 d U . . C19 C 0.6874(6) 0.4886(5) 0.0506(4) 0.043(2) Uani 1 1 d U . . H19 H 0.6741 0.4957 0.0842 0.051 Uiso 1 1 calc R . . C20 C 0.7037(5) 0.4234(5) 0.0445(4) 0.038(2) Uani 1 1 d U . . H20 H 0.7009 0.3868 0.0737 0.046 Uiso 1 1 calc R . . C22 C 0.7236(6) 0.4652(5) -0.0464(4) 0.040(2) Uani 1 1 d U . . H22 H 0.7344 0.4569 -0.0795 0.048 Uiso 1 1 calc R . . C23 C 0.7079(5) 0.5302(5) -0.0420(4) 0.042(2) Uani 1 1 d U . . H23 H 0.7088 0.5662 -0.0720 0.050 Uiso 1 1 calc R . . C24 C 0.7458(6) 0.3410(5) -0.0097(4) 0.045(2) Uani 1 1 d U . . H24A H 0.7247 0.3115 0.0204 0.053 Uiso 1 1 calc R . . H24B H 0.7274 0.3408 -0.0410 0.053 Uiso 1 1 calc R . . Pd2 Pd 0.66356(8) 0.34518(8) 0.50910(4) 0.0934(4) Uani 1 1 d U . . N7 N 0.6571(9) 0.2687(9) 0.4822(6) 0.122(5) Uani 1 1 d U . . H7A H 0.6707 0.2776 0.4474 0.146 Uiso 1 1 calc R . . H7B H 0.6893 0.2289 0.4977 0.146 Uiso 1 1 calc R . . N8 N 0.5509(8) 0.3730(10) 0.5138(5) 0.120(5) Uani 1 1 d U . . H8A H 0.5311 0.3625 0.5474 0.144 Uiso 1 1 calc R . . H8B H 0.5324 0.4186 0.4997 0.144 Uiso 1 1 calc R . . N9 N 0.7755(8) 0.3136(6) 0.5038(4) 0.080(3) Uani 1 1 d U . . N10 N 0.6657(7) 0.4319(7) 0.5250(4) 0.079(3) Uani 1 1 d U . . N11 N 1.1660(7) 0.2258(5) 0.4634(4) 0.072(3) Uani 1 1 d U . . N12 N 0.7285(7) 0.7313(6) 0.5458(4) 0.075(3) Uani 1 1 d U . . C25 C 0.5813(13) 0.2606(14) 0.4925(9) 0.140(7) Uani 1 1 d U . . H25A H 0.5742 0.2360 0.4694 0.168 Uiso 1 1 calc R . . H25B H 0.5715 0.2360 0.5287 0.168 Uiso 1 1 calc R . . C26 C 0.5348(13) 0.3303(14) 0.4817(9) 0.137(6) Uani 1 1 d U . . H26A H 0.4829 0.3303 0.4899 0.165 Uiso 1 1 calc R . . H26B H 0.5424 0.3520 0.4445 0.165 Uiso 1 1 calc R . . C27 C 0.8150(10) 0.2736(8) 0.5431(5) 0.082(4) Uani 1 1 d U . . H27 H 0.7896 0.2585 0.5754 0.099 Uiso 1 1 calc R . . C28 C 0.8923(9) 0.2530(7) 0.5386(5) 0.073(3) Uani 1 1 d U . . H28 H 0.9173 0.2244 0.5675 0.087 Uiso 1 1 calc R . . C29 C 0.9335(9) 0.2752(7) 0.4901(5) 0.069(3) Uani 1 1 d U . . C30 C 0.8878(9) 0.3181(8) 0.4494(5) 0.077(3) Uani 1 1 d U . . H30 H 0.9108 0.3353 0.4166 0.093 Uiso 1 1 calc R . . C31 C 0.8120(10) 0.3350(9) 0.4563(6) 0.088(4) Uani 1 1 d U . . H31 H 0.7848 0.3616 0.4280 0.105 Uiso 1 1 calc R . . C32 C 1.0117(9) 0.2567(6) 0.4814(4) 0.066(3) Uani 1 1 d U . . C33 C 1.0574(9) 0.2372(7) 0.5222(5) 0.071(3) Uani 1 1 d U . . H33 H 1.0352 0.2354 0.5564 0.085 Uiso 1 1 calc R . . C34 C 1.1333(9) 0.2209(7) 0.5129(5) 0.071(3) Uani 1 1 d U . . H34 H 1.1623 0.2064 0.5407 0.085 Uiso 1 1 calc R . . C35 C 1.1234(9) 0.2464(6) 0.4228(5) 0.073(3) Uani 1 1 d U . . H35 H 1.1466 0.2507 0.3887 0.088 Uiso 1 1 calc R . . C36 C 1.0498(9) 0.2607(7) 0.4306(4) 0.074(3) Uani 1 1 d U . . H36 H 1.0227 0.2735 0.4019 0.089 Uiso 1 1 calc R . . C37 C 0.6777(8) 0.4345(8) 0.5728(5) 0.072(3) Uani 1 1 d U . . H37 H 0.6822 0.3956 0.6010 0.086 Uiso 1 1 calc R . . C38 C 0.6833(7) 0.4960(7) 0.5796(4) 0.068(3) Uani 1 1 d U . . H38 H 0.6900 0.4977 0.6127 0.081 Uiso 1 1 calc R . . C39 C 0.6789(7) 0.5543(7) 0.5379(5) 0.065(3) Uani 1 1 d U . . C40 C 0.6654(8) 0.5495(8) 0.4905(5) 0.073(3) Uani 1 1 d U . . H40 H 0.6623 0.5871 0.4613 0.088 Uiso 1 1 calc R . . C41 C 0.6566(8) 0.4887(9) 0.4861(5) 0.083(3) Uani 1 1 d U . . H41 H 0.6437 0.4880 0.4545 0.099 Uiso 1 1 calc R . . C42 C 0.6918(7) 0.6173(7) 0.5425(4) 0.064(3) Uani 1 1 d U . . C43 C 0.7206(7) 0.6192(7) 0.5858(4) 0.063(3) Uani 1 1 d U . . H43 H 0.7287 0.5805 0.6142 0.075 Uiso 1 1 calc R . . C44 C 0.7370(8) 0.6750(7) 0.5877(5) 0.069(3) Uani 1 1 d U . . H44 H 0.7544 0.6754 0.6178 0.082 Uiso 1 1 calc R . . C45 C 0.6995(9) 0.7326(8) 0.5034(6) 0.083(4) Uani 1 1 d U . . H45 H 0.6910 0.7720 0.4756 0.100 Uiso 1 1 calc R . . C46 C 0.6837(8) 0.6788(8) 0.5015(5) 0.080(4) Uani 1 1 d U . . H46 H 0.6657 0.6805 0.4711 0.096 Uiso 1 1 calc R . . C47 C 0.7499(10) 0.7909(7) 0.5471(6) 0.090(4) Uani 1 1 d U . . H47A H 0.7337 0.8007 0.5812 0.108 Uiso 1 1 calc R . . H47B H 0.7266 0.8312 0.5206 0.108 Uiso 1 1 calc R . . O1 O 0.0866(4) 0.5853(4) -0.0721(3) 0.059(2) Uani 1 1 d DU . . O2 O 0.2079(5) 0.6329(5) -0.1387(3) 0.066(2) Uani 1 1 d DU . . O3 O 0.2802(4) 0.7282(4) -0.1332(3) 0.0593(19) Uani 1 1 d DU . . O4 O 0.4065(4) 0.6599(4) -0.0722(3) 0.0588(19) Uani 1 1 d DU . . O5 O 0.4198(4) 0.5773(4) 0.0338(3) 0.064(2) Uani 1 1 d DU . . O6 O 0.3328(4) 0.6671(4) 0.1019(3) 0.0573(19) Uani 1 1 d DU . . O7 O 0.2164(4) 0.7916(4) 0.0654(3) 0.0473(16) Uani 1 1 d DU . . O8 O -0.0357(4) 0.9457(4) -0.0643(3) 0.061(2) Uani 1 1 d DU . . O9 O -0.1868(5) 0.9737(4) -0.0789(3) 0.069(2) Uani 1 1 d DU . . O10 O -0.2180(5) 0.9725(4) 0.0351(4) 0.070(2) Uani 1 1 d DU . . O11 O -0.2544(7) 0.9171(6) 0.1490(4) 0.097(3) Uani 1 1 d DU . . O12 O -0.3106(4) 0.8085(4) 0.1750(3) 0.0609(19) Uani 1 1 d DU . . O13 O -0.2540(4) 0.6636(4) 0.1792(3) 0.059(2) Uani 1 1 d DU . . O14 O -0.1327(4) 0.5840(4) 0.1182(3) 0.0550(19) Uani 1 1 d DU . . C48 C 0.0170(6) 0.5961(5) -0.0475(4) 0.048(2) Uani 1 1 d DU . . C49 C -0.0457(7) 0.6241(6) -0.0724(4) 0.057(3) Uani 1 1 d DU . . H49 H -0.0422 0.6367 -0.1090 0.068 Uiso 1 1 calc R . . C50 C -0.1173(7) 0.6345(6) -0.0430(4) 0.058(3) Uani 1 1 d DU . . H50 H -0.1603 0.6530 -0.0603 0.070 Uiso 1 1 calc R . . C51 C -0.1228(6) 0.6171(5) 0.0116(4) 0.047(2) Uani 1 1 d DU . . H51 H -0.1695 0.6252 0.0307 0.056 Uiso 1 1 calc R . . C52 C -0.0578(5) 0.5872(4) 0.0381(3) 0.039(2) Uani 1 1 d DU . . C53 C -0.0619(6) 0.5691(5) 0.0945(4) 0.050(2) Uani 1 1 d DU . . C54 C 0.0023(6) 0.5408(5) 0.1187(4) 0.057(3) Uani 1 1 d DU . . H54 H -0.0008 0.5304 0.1552 0.068 Uiso 1 1 calc R . . C55 C 0.0733(7) 0.5268(5) 0.0897(4) 0.055(3) Uani 1 1 d DU . . H55 H 0.1162 0.5055 0.1071 0.066 Uiso 1 1 calc R . . C56 C 0.0785(6) 0.5450(5) 0.0356(4) 0.050(2) Uani 1 1 d DU . . H56 H 0.1251 0.5371 0.0162 0.060 Uiso 1 1 calc R . . C57 C 0.0127(6) 0.5759(5) 0.0096(4) 0.046(2) Uani 1 1 d DU . . C58 C 0.0924(7) 0.6007(7) -0.1278(4) 0.067(3) Uani 1 1 d DU . . H58A H 0.0666 0.6489 -0.1422 0.081 Uiso 1 1 calc R . . H58B H 0.0702 0.5723 -0.1387 0.081 Uiso 1 1 calc R . . C59 C 0.1717(7) 0.5864(8) -0.1468(6) 0.076(3) Uani 1 1 d DU . . H59A H 0.1973 0.5395 -0.1290 0.091 Uiso 1 1 calc R . . H59B H 0.1773 0.5892 -0.1840 0.091 Uiso 1 1 calc R . . C60 C 0.2030(7) 0.6958(7) -0.1756(4) 0.072(3) Uani 1 1 d DU . . H60A H 0.1604 0.7309 -0.1648 0.086 Uiso 1 1 calc R . . H60B H 0.1952 0.6920 -0.2093 0.086 Uiso 1 1 calc R . . C61 C 0.2706(8) 0.7163(7) -0.1813(4) 0.067(3) Uani 1 1 d DU . . H61A H 0.3135 0.6803 -0.1906 0.081 Uiso 1 1 calc R . . H61B H 0.2677 0.7582 -0.2094 0.081 Uiso 1 1 calc R . . C62 C 0.3451(7) 0.7525(6) -0.1354(5) 0.069(3) Uani 1 1 d DU . . H62A H 0.3528 0.7823 -0.1700 0.083 Uiso 1 1 calc R . . H62B H 0.3347 0.7798 -0.1100 0.083 Uiso 1 1 calc R . . C63 C 0.4132(7) 0.6960(7) -0.1243(5) 0.072(3) Uani 1 1 d DU . . H63 H 0.4546 0.6858 -0.1485 0.086 Uiso 1 1 calc R . . C64 C 0.4704(7) 0.6073(7) -0.0569(6) 0.077(3) Uani 1 1 d DU . . H64A H 0.5135 0.6173 -0.0798 0.093 Uiso 1 1 calc R . . H64B H 0.4665 0.5642 -0.0603 0.093 Uiso 1 1 calc R . . C65 C 0.4812(7) 0.5995(8) -0.0006(6) 0.083(4) Uani 1 1 d DU . . H65A H 0.5284 0.5655 0.0084 0.099 Uiso 1 1 calc R . . H65B H 0.4818 0.6432 0.0036 0.099 Uiso 1 1 calc R . . C66 C 0.4256(8) 0.5666(7) 0.0877(6) 0.079(3) Uani 1 1 d DU . . H66A H 0.4754 0.5374 0.0955 0.095 Uiso 1 1 calc R . . H66B H 0.3905 0.5419 0.1083 0.095 Uiso 1 1 calc R . . C67 C 0.4113(7) 0.6303(7) 0.1040(6) 0.075(3) Uani 1 1 d DU . . H67A H 0.4245 0.6193 0.1395 0.090 Uiso 1 1 calc R . . H67B H 0.4412 0.6588 0.0808 0.090 Uiso 1 1 calc R . . C68 C 0.3181(7) 0.7287(6) 0.1178(5) 0.066(3) Uani 1 1 d DU . . H68A H 0.3463 0.7581 0.0936 0.079 Uiso 1 1 calc R . . H68B H 0.3342 0.7175 0.1525 0.079 Uiso 1 1 calc R . . C69 C 0.2378(7) 0.7661(6) 0.1190(4) 0.055(3) Uani 1 1 d DU . . H69A H 0.2090 0.7353 0.1403 0.066 Uiso 1 1 calc R . . H69B H 0.2275 0.8045 0.1346 0.066 Uiso 1 1 calc R . . C70 C 0.1451(6) 0.8278(5) 0.0591(4) 0.044(2) Uani 1 1 d DU . . C71 C 0.0881(6) 0.8415(6) 0.0980(4) 0.050(2) Uani 1 1 d DU . . H71 H 0.0992 0.8271 0.1327 0.060 Uiso 1 1 calc R . . C72 C 0.0170(6) 0.8751(6) 0.0877(4) 0.053(3) Uani 1 1 d DU . . H72 H -0.0203 0.8827 0.1149 0.063 Uiso 1 1 calc R . . C73 C -0.0001(6) 0.8985(6) 0.0351(4) 0.050(2) Uani 1 1 d DU . . H73 H -0.0493 0.9207 0.0276 0.060 Uiso 1 1 calc R . . C74 C 0.0544(6) 0.8888(5) -0.0043(4) 0.044(2) Uani 1 1 d DU . . C75 C 0.0353(6) 0.9120(5) -0.0594(4) 0.046(2) Uani 1 1 d DU . . C76 C 0.0914(6) 0.8967(6) -0.0983(4) 0.054(3) Uani 1 1 d DU . . H76 H 0.0795 0.9097 -0.1328 0.065 Uiso 1 1 calc R . . C77 C 0.1647(6) 0.8629(5) -0.0884(4) 0.051(2) Uani 1 1 d DU . . H77 H 0.2012 0.8547 -0.1160 0.061 Uiso 1 1 calc R . . C78 C 0.1840(6) 0.8413(5) -0.0373(4) 0.046(2) Uani 1 1 d DU . . H78 H 0.2334 0.8191 -0.0303 0.055 Uiso 1 1 calc R . . C79 C 0.1267(5) 0.8539(5) 0.0046(4) 0.0383(19) Uani 1 1 d DU . . C80 C -0.0613(7) 0.9682(7) -0.1183(5) 0.069(3) Uani 1 1 d DU . . H80A H -0.0318 0.9960 -0.1430 0.083 Uiso 1 1 calc R . . H80B H -0.0570 0.9285 -0.1309 0.083 Uiso 1 1 calc R . . C81 C -0.1407(7) 1.0095(7) -0.1121(5) 0.073(3) Uani 1 1 d DU . . H81A H -0.1430 1.0484 -0.0991 0.088 Uiso 1 1 calc R . . H81B H -0.1592 1.0279 -0.1464 0.088 Uiso 1 1 calc R . . C82 C -0.2497(7) 1.0158(6) -0.0512(6) 0.074(3) Uani 1 1 d DU . . H82A H -0.2876 0.9918 -0.0378 0.089 Uiso 1 1 calc R . . H82B H -0.2716 1.0591 -0.0758 0.089 Uiso 1 1 calc R . . C83 C -0.2264(8) 1.0306(7) -0.0069(5) 0.079(3) Uani 1 1 d DU . . H83A H -0.1796 1.0421 -0.0176 0.094 Uiso 1 1 calc R . . H83B H -0.2639 1.0695 0.0033 0.094 Uiso 1 1 calc R . . C84 C -0.2002(8) 0.9901(7) 0.0772(5) 0.079(3) Uani 1 1 d DU . . H84A H -0.2418 1.0259 0.0880 0.095 Uiso 1 1 calc R . . H84B H -0.1570 1.0076 0.0660 0.095 Uiso 1 1 calc R . . C85 C -0.1843(9) 0.9290(8) 0.1207(6) 0.094(4) Uani 1 1 d DU . . H85A H -0.1558 0.9353 0.1444 0.113 Uiso 1 1 calc R . . H85B H -0.1547 0.8893 0.1076 0.113 Uiso 1 1 calc R . . C86 C -0.2338(10) 0.8618(9) 0.1950(5) 0.096(4) Uani 1 1 d DU . . H86A H -0.2236 0.8790 0.2217 0.115 Uiso 1 1 calc R . . H86B H -0.1895 0.8266 0.1863 0.115 Uiso 1 1 calc R . . C87 C -0.2986(9) 0.8326(8) 0.2142(5) 0.085(4) Uani 1 1 d DU . . H87A H -0.2879 0.7952 0.2456 0.102 Uiso 1 1 calc R . . H87B H -0.3427 0.8681 0.2226 0.102 Uiso 1 1 calc R . . C88 C -0.3540(7) 0.7607(6) 0.1942(5) 0.063(3) Uani 1 1 d DU . . H88A H -0.3781 0.7605 0.1654 0.076 Uiso 1 1 calc R . . H88B H -0.3929 0.7765 0.2206 0.076 Uiso 1 1 calc R . . C89 C -0.3096(7) 0.6893(6) 0.2174(4) 0.059(3) Uani 1 1 d DU . . H89A H -0.2861 0.6888 0.2467 0.071 Uiso 1 1 calc R . . H89B H -0.3423 0.6598 0.2306 0.071 Uiso 1 1 calc R . . C90 C -0.2173(8) 0.5917(6) 0.1962(5) 0.074(4) Uani 1 1 d DU . . H90A H -0.2430 0.5660 0.1854 0.088 Uiso 1 1 calc R . . H90B H -0.2206 0.5783 0.2343 0.088 Uiso 1 1 calc R . . C91 C -0.1387(7) 0.5729(6) 0.1754(4) 0.065(3) Uani 1 1 d DU . . H91A H -0.1150 0.5247 0.1916 0.078 Uiso 1 1 calc R . . H91B H -0.1132 0.6007 0.1838 0.078 Uiso 1 1 calc R . . O15 O 1.1466(5) 0.5134(5) 0.5938(3) 0.075(2) Uani 1 1 d DU . . O16 O 1.2752(6) 0.5304(7) 0.6310(4) 0.107(3) Uani 1 1 d DU . . O17 O 1.2869(7) 0.6645(8) 0.6261(4) 0.121(4) Uani 1 1 d DU . . O18 O 1.2376(16) 0.8029(12) 0.5960(10) 0.284(12) Uani 1 1 d DU . . O19 O 1.268(2) 0.8672(15) 0.4917(10) 0.345(14) Uani 1 1 d DU . . O20 O 1.1933(16) 0.8734(10) 0.4011(7) 0.252(9) Uani 1 1 d DU . . O21 O 1.0393(13) 0.9250(9) 0.4366(6) 0.217(7) Uani 1 1 d DU . . O22 O 0.7832(11) 0.9023(8) 0.6035(5) 0.173(5) Uani 1 1 d DU . . O23 O 0.6227(15) 0.8491(12) 0.6684(9) 0.269(9) Uani 1 1 d DU . . O24 O 0.5589(18) 0.8011(14) 0.5802(10) 0.289(12) Uani 1 1 d DU . . O25 O 0.5984(10) 0.8880(10) 0.4873(6) 0.195(8) Uani 1 1 d DU . . O26 O 0.7215(8) 0.8754(6) 0.4086(4) 0.133(5) Uani 1 1 d DU . . O27 O 0.7841(5) 0.7401(5) 0.3981(3) 0.080(3) Uani 1 1 d DU . . O28 O 0.9125(5) 0.6312(4) 0.4441(3) 0.069(2) Uani 1 1 d DU . . C92 C 1.0762(6) 0.5337(6) 0.5818(4) 0.062(3) Uani 1 1 d DU . . C93 C 1.0159(7) 0.5373(7) 0.6170(4) 0.073(3) Uani 1 1 d DU . . H93 H 1.0227 0.5237 0.6525 0.088 Uiso 1 1 calc R . . C94 C 0.9420(7) 0.5611(7) 0.6024(4) 0.072(3) Uani 1 1 d DU . . H94 H 0.9012 0.5628 0.6278 0.086 Uiso 1 1 calc R . . C95 C 0.9323(7) 0.5818(6) 0.5491(4) 0.065(3) Uani 1 1 d DU . . H95 H 0.8844 0.5964 0.5386 0.078 Uiso 1 1 calc R . . C96 C 0.9944(6) 0.5807(6) 0.5109(4) 0.057(3) Uani 1 1 d DU . . C97 C 0.9849(6) 0.6056(6) 0.4555(4) 0.060(3) Uani 1 1 d DU . . C98 C 1.0466(6) 0.6026(7) 0.4195(4) 0.069(3) Uani 1 1 d DU . . H98 H 1.0406 0.6180 0.3838 0.083 Uiso 1 1 calc R . . C99 C 1.1179(7) 0.5767(7) 0.4357(4) 0.063(3) Uani 1 1 d DU . . H99 H 1.1589 0.5752 0.4104 0.076 Uiso 1 1 calc R . . C100 C 1.1299(7) 0.5531(7) 0.4882(4) 0.067(3) Uani 1 1 d DU . . H100 H 1.1781 0.5354 0.4983 0.080 Uiso 1 1 calc R . . C101 C 1.0668(6) 0.5564(6) 0.5264(4) 0.061(3) Uani 1 1 d DU . . C102 C 1.1624(9) 0.4947(8) 0.6468(4) 0.090(4) Uani 1 1 d DU . . H10A H 1.1415 0.4576 0.6673 0.108 Uiso 1 1 calc R . . H10B H 1.1404 0.5339 0.6620 0.108 Uiso 1 1 calc R . . C103 C 1.2449(9) 0.4719(9) 0.6474(6) 0.110(5) Uani 1 1 d DU . . H10C H 1.2574 0.4457 0.6827 0.132 Uiso 1 1 calc R . . H10D H 1.2674 0.4417 0.6241 0.132 Uiso 1 1 calc R . . C104 C 1.2881(11) 0.5491(11) 0.6730(6) 0.130(5) Uani 1 1 d DU . . H10E H 1.3153 0.5089 0.6978 0.157 Uiso 1 1 calc R . . H10F H 1.2411 0.5705 0.6911 0.157 Uiso 1 1 calc R . . C105 C 1.3326(11) 0.5988(11) 0.6509(9) 0.155(6) Uani 1 1 d DU . . H10G H 1.3551 0.6031 0.6789 0.186 Uiso 1 1 calc R . . H10H H 1.3724 0.5816 0.6256 0.186 Uiso 1 1 calc R . . C106 C 1.2409(14) 0.7066(13) 0.6606(9) 0.182(8) Uani 1 1 d DU . . H106 H 1.2417 0.6936 0.6969 0.218 Uiso 1 1 calc R . . C107 C 1.1947(17) 0.7696(14) 0.6330(12) 0.230(12) Uani 1 1 d DU . . H107 H 1.1430 0.7854 0.6394 0.276 Uiso 1 1 calc R . . C108 C 1.204(3) 0.8722(15) 0.5764(13) 0.359(16) Uani 1 1 d DU . . H10I H 1.2325 0.8981 0.5840 0.431 Uiso 1 1 calc R . . H10J H 1.1546 0.8840 0.5952 0.431 Uiso 1 1 calc R . . C109 C 1.196(2) 0.895(2) 0.5187(14) 0.372(17) Uani 1 1 d DU . . H10K H 1.1585 0.8785 0.5110 0.446 Uiso 1 1 calc R . . H10L H 1.1809 0.9454 0.5072 0.446 Uiso 1 1 calc R . . C110 C 1.273(2) 0.9048(16) 0.4387(11) 0.317(12) Uani 1 1 d DU . . H11A H 1.3197 0.9167 0.4310 0.380 Uiso 1 1 calc R . . H11B H 1.2331 0.9478 0.4353 0.380 Uiso 1 1 calc R . . C111 C 1.2691(18) 0.8736(16) 0.3984(11) 0.270(11) Uani 1 1 d DU . . H11C H 1.2843 0.8999 0.3640 0.324 Uiso 1 1 calc R . . H11D H 1.3021 0.8267 0.4043 0.324 Uiso 1 1 calc R . . C112 C 1.1487(15) 0.9380(11) 0.3754(9) 0.232(9) Uani 1 1 d DU . . H11E H 1.1667 0.9487 0.3384 0.279 Uiso 1 1 calc R . . H11F H 1.1524 0.9734 0.3901 0.279 Uiso 1 1 calc R . . C113 C 1.0696(17) 0.9386(14) 0.3812(8) 0.245(10) Uani 1 1 d DU . . H11G H 1.0404 0.9833 0.3621 0.294 Uiso 1 1 calc R . . H11H H 1.0658 0.9037 0.3660 0.294 Uiso 1 1 calc R . . C114 C 0.9666(14) 0.9300(13) 0.4518(8) 0.197(7) Uani 1 1 d DU . . C115 C 0.9076(15) 0.9465(14) 0.4250(8) 0.201(8) Uani 1 1 d DU . . H115 H 0.9186 0.9530 0.3888 0.241 Uiso 1 1 calc R . . C116 C 0.8359(16) 0.9550(11) 0.4421(8) 0.198(7) Uani 1 1 d DU . . H116 H 0.7987 0.9722 0.4194 0.237 Uiso 1 1 calc R . . C117 C 0.8198(13) 0.9357(9) 0.4986(7) 0.155(5) Uani 1 1 d DU . . H117 H 0.7713 0.9361 0.5131 0.185 Uiso 1 1 calc R . . C118 C 0.8728(15) 0.917(4) 0.5301(9) 0.197(7) Uani 0.50 1 d PDU . . C119 C 0.8523(13) 0.8996(13) 0.5891(8) 0.182(7) Uani 1 1 d DU . . C120 C 0.9111(15) 0.8843(12) 0.6167(9) 0.180(7) Uani 1 1 d DU . . H120 H 0.9010 0.8761 0.6530 0.216 Uiso 1 1 calc R . . C121 C 0.9836(16) 0.8796(14) 0.5967(9) 0.198(8) Uani 1 1 d DU . . H121 H 1.0198 0.8674 0.6195 0.238 Uiso 1 1 calc R . . C122 C 1.0047(13) 0.8931(12) 0.5419(9) 0.164(6) Uani 1 1 d DU . . H122 H 1.0537 0.8899 0.5273 0.197 Uiso 1 1 calc R . . C123 C 0.9436(12) 0.9121(9) 0.5108(7) 0.149(5) Uani 1 1 d DU . . C124 C 0.7392(15) 0.8872(10) 0.6590(7) 0.206(8) Uani 1 1 d DU . . H12A H 0.7734 0.8639 0.6858 0.248 Uiso 1 1 calc R . . H12B H 0.7067 0.9299 0.6667 0.248 Uiso 1 1 calc R . . C125 C 0.6940(15) 0.8415(11) 0.6567(7) 0.182(8) Uani 1 1 d DU . . H12C H 0.7041 0.8372 0.6208 0.218 Uiso 1 1 calc R . . H12D H 0.7178 0.7963 0.6783 0.218 Uiso 1 1 calc R . . C126 C 0.5863(16) 0.8043(15) 0.6563(8) 0.237(10) Uani 1 1 d DU . . H12E H 0.5328 0.8174 0.6658 0.285 Uiso 1 1 calc R . . H12F H 0.6078 0.7558 0.6728 0.285 Uiso 1 1 calc R . . C127 C 0.6058(17) 0.8213(18) 0.5982(9) 0.243(11) Uani 1 1 d DU . . H12G H 0.5991 0.8705 0.5840 0.291 Uiso 1 1 calc R . . H12H H 0.6572 0.7965 0.5892 0.291 Uiso 1 1 calc R . . C128 C 0.5050(16) 0.863(2) 0.5602(11) 0.283(14) Uani 1 1 d DU . . H12I H 0.5062 0.8996 0.5741 0.340 Uiso 1 1 calc R . . H12J H 0.4553 0.8566 0.5684 0.340 Uiso 1 1 calc R . . C129 C 0.5268(16) 0.8765(19) 0.5041(10) 0.257(13) Uani 1 1 d DU . . H12K H 0.5261 0.8377 0.4921 0.308 Uiso 1 1 calc R . . H12L H 0.4896 0.9168 0.4868 0.308 Uiso 1 1 calc R . . C130 C 0.5950(13) 0.9238(14) 0.4314(8) 0.235(13) Uani 1 1 d DU . . H13A H 0.5565 0.9678 0.4270 0.282 Uiso 1 1 calc R . . H13B H 0.5837 0.8961 0.4127 0.282 Uiso 1 1 calc R . . C131 C 0.6701(14) 0.9347(10) 0.4109(9) 0.192(10) Uani 1 1 d DU . . H13C H 0.6675 0.9661 0.3761 0.231 Uiso 1 1 calc R . . H13D H 0.6842 0.9557 0.4336 0.231 Uiso 1 1 calc R . . C132 C 0.7270(12) 0.8589(8) 0.3597(6) 0.133(7) Uani 1 1 d DU . . H13E H 0.7332 0.8979 0.3309 0.159 Uiso 1 1 calc R . . H13F H 0.6813 0.8499 0.3569 0.159 Uiso 1 1 calc R . . C133 C 0.7905(10) 0.7980(7) 0.3561(5) 0.105(5) Uani 1 1 d DU . . H13G H 0.7929 0.7872 0.3229 0.126 Uiso 1 1 calc R . . H13H H 0.8365 0.8082 0.3567 0.126 Uiso 1 1 calc R . . C134 C 0.8195(7) 0.6767(7) 0.3843(5) 0.079(3) Uani 1 1 d DU . . H13I H 0.8105 0.6825 0.3485 0.095 Uiso 1 1 calc R . . H13J H 0.7963 0.6422 0.4070 0.095 Uiso 1 1 calc R . . C135 C 0.9003(7) 0.6504(7) 0.3880(4) 0.070(3) Uani 1 1 d DU . . H13K H 0.9242 0.6857 0.3682 0.084 Uiso 1 1 calc R . . H13L H 0.9214 0.6104 0.3736 0.084 Uiso 1 1 calc R . . P1 P 0.9848(2) 0.3390(2) 0.27141(12) 0.0747(10) Uani 1 1 d U . . F1 F 1.0438(7) 0.2687(6) 0.2889(5) 0.151(4) Uani 1 1 d U . . F2 F 0.9387(6) 0.3046(6) 0.2506(4) 0.122(3) Uani 1 1 d U . . F3 F 0.9257(8) 0.4103(6) 0.2542(4) 0.154(4) Uani 1 1 d U . . F4 F 0.9405(7) 0.3313(7) 0.3272(3) 0.144(4) Uani 1 1 d U . . F5 F 1.0278(7) 0.3557(7) 0.2147(4) 0.142(4) Uani 1 1 d U . . F6 F 1.0333(8) 0.3667(8) 0.2961(5) 0.157(4) Uani 1 1 d U . . P2 P 0.5685(3) 0.7228(3) 0.36290(17) 0.1079(16) Uani 1 1 d U . . F7 F 0.4815(6) 0.7522(8) 0.3702(5) 0.164(5) Uani 1 1 d U . . F8 F 0.5706(8) 0.7502(8) 0.4128(4) 0.168(4) Uani 1 1 d U . . F9 F 0.5605(8) 0.6527(8) 0.3990(5) 0.171(5) Uani 1 1 d U . . F10 F 0.5779(8) 0.7951(8) 0.3258(5) 0.177(5) Uani 1 1 d U . . F11 F 0.5639(7) 0.7017(9) 0.3141(4) 0.163(4) Uani 1 1 d U . . F12 F 0.6563(6) 0.6943(8) 0.3576(6) 0.170(5) Uani 1 1 d U . . P3 P 0.5877(2) 0.5093(2) 0.19745(14) 0.0823(11) Uani 1 1 d U . . F13 F 0.5047(6) 0.5233(6) 0.2188(4) 0.124(3) Uani 1 1 d U . . F14 F 0.6052(7) 0.4453(7) 0.2456(4) 0.140(4) Uani 1 1 d U . . F15 F 0.6737(4) 0.4926(4) 0.1769(3) 0.084(2) Uani 1 1 d U . . F16 F 0.5689(5) 0.5742(5) 0.1492(3) 0.097(2) Uani 1 1 d U . . F17 F 0.6007(6) 0.5567(7) 0.2290(4) 0.131(3) Uani 1 1 d U . . F18 F 0.5765(5) 0.4641(5) 0.1639(3) 0.098(2) Uani 1 1 d U . . P4 P 0.43805(19) 0.82826(19) 0.96894(15) 0.0686(9) Uani 1 1 d U . . F19 F 0.4022(4) 0.8734(5) 1.0107(4) 0.094(2) Uani 1 1 d U . . F20 F 0.5024(4) 0.8665(4) 0.9517(3) 0.0737(19) Uani 1 1 d U . . F21 F 0.4871(4) 0.7708(4) 1.0114(4) 0.091(2) Uani 1 1 d U . . F22 F 0.3753(4) 0.7922(5) 0.9862(4) 0.096(2) Uani 1 1 d U . . F23 F 0.3898(5) 0.8863(5) 0.9251(4) 0.112(3) Uani 1 1 d U . . F24 F 0.4770(5) 0.7834(5) 0.9277(4) 0.104(3) Uani 1 1 d U . . P5 P 0.9650(3) 0.6901(2) 0.23188(13) 0.0890(12) Uani 1 1 d U . . F25 F 0.9304(9) 0.7410(6) 0.2675(4) 0.154(4) Uani 1 1 d U . . F26 F 0.9986(6) 0.6410(6) 0.1937(3) 0.111(3) Uani 1 1 d U . . F27 F 1.0141(7) 0.6386(7) 0.2766(4) 0.146(4) Uani 1 1 d U . . F28 F 0.9045(8) 0.6569(9) 0.2563(5) 0.178(5) Uani 1 1 d U . . F29 F 1.0332(10) 0.7194(8) 0.2076(5) 0.179(5) Uani 1 1 d U . . F30 F 0.9259(10) 0.7439(9) 0.1870(4) 0.221(7) Uani 1 1 d U . . P6 P 0.3319(4) 0.3318(4) 0.1895(2) 0.146(2) Uani 1 1 d U . . F31 F 0.3151(10) 0.3632(8) 0.2372(5) 0.189(5) Uani 1 1 d U . . F32 F 0.4140(8) 0.2914(9) 0.2098(5) 0.190(6) Uani 1 1 d U . . F33 F 0.3651(7) 0.3908(9) 0.1529(5) 0.193(5) Uani 1 1 d U . . F34 F 0.2551(8) 0.3742(10) 0.1685(7) 0.236(7) Uani 1 1 d U . . F35 F 0.3007(8) 0.2723(7) 0.2257(4) 0.156(4) Uani 1 1 d U . . F36 F 0.3538(11) 0.2991(11) 0.1416(4) 0.230(6) Uani 1 1 d U . . P7 P 0.8296(5) 0.0521(4) 0.2655(2) 0.148(2) Uani 1 1 d U . . F37 F 0.8588(16) 0.1071(13) 0.2204(6) 0.279(9) Uani 1 1 d U . . F38 F 0.9248(14) 0.0191(12) 0.2585(15) 0.349(13) Uani 1 1 d U . . F39 F 0.8383(14) 0.0879(13) 0.3025(7) 0.266(8) Uani 1 1 d U . . F40 F 0.7704(19) 0.0271(15) 0.3055(8) 0.342(10) Uani 1 1 d U . . F41 F 0.8316(15) 0.0051(13) 0.2277(9) 0.288(9) Uani 1 1 d U . . F42 F 0.7556(14) 0.1052(9) 0.2387(11) 0.285(9) Uani 1 1 d U . . P8 P 0.2356(6) 0.8394(5) 0.2466(3) 0.180(3) Uani 1 1 d U . . F43 F 0.2768(12) 0.8644(10) 0.1914(6) 0.216(6) Uani 1 1 d U . . F44 F 0.3049(18) 0.8401(16) 0.2766(9) 0.321(10) Uani 1 1 d U . . F45 F 0.1964(16) 0.8145(13) 0.3045(7) 0.278(8) Uani 1 1 d U . . F46 F 0.1937(19) 0.9159(11) 0.2508(9) 0.321(10) Uani 1 1 d U . . F47 F 0.1697(13) 0.8280(14) 0.2237(8) 0.259(8) Uani 1 1 d U . . F48 F 0.2726(14) 0.7644(10) 0.2449(11) 0.276(9) Uani 1 1 d U . . N13 N 0.5482(11) 0.6054(13) 0.6469(7) 0.163(8) Uani 1 1 d U . . C136 C 0.5239(15) 0.6273(15) 0.6826(8) 0.150(8) Uani 1 1 d U . . C137 C 0.4922(14) 0.6581(14) 0.7298(8) 0.161(9) Uani 1 1 d U . . H37D H 0.4468 0.6944 0.7220 0.193 Uiso 1 1 calc R . . H37E H 0.5279 0.6766 0.7372 0.193 Uiso 1 1 calc R . . H37F H 0.4822 0.6228 0.7598 0.193 Uiso 1 1 calc R . . N14 N 0.9855(9) 0.7982(6) 0.8532(5) 0.097(4) Uani 1 1 d U . . C138 C 0.9908(11) 0.8266(8) 0.8077(6) 0.096(5) Uani 1 1 d U . . C139 C 1.0019(16) 0.8599(10) 0.7520(6) 0.156(10) Uani 1 1 d U . . H39D H 0.9642 0.8574 0.7340 0.188 Uiso 1 1 calc R . . H39E H 1.0503 0.8369 0.7376 0.188 Uiso 1 1 calc R . . H39F H 0.9986 0.9075 0.7476 0.188 Uiso 1 1 calc R . . N15 N -0.0010(11) 0.8028(8) 0.3492(5) 0.123(6) Uani 1 1 d U . . C140 C -0.0019(14) 0.8280(11) 0.3061(7) 0.121(7) Uani 1 1 d U . . C141 C -0.0063(17) 0.8718(14) 0.2498(7) 0.177(11) Uani 1 1 d U . . H41D H -0.0042 0.8435 0.2271 0.212 Uiso 1 1 calc R . . H41E H 0.0349 0.8912 0.2393 0.212 Uiso 1 1 calc R . . H41F H -0.0524 0.9083 0.2474 0.212 Uiso 1 1 calc R . . N16 N 0.2060(10) 0.5657(7) 0.1628(4) 0.112(5) Uani 1 1 d U . . C142 C 0.1654(12) 0.5316(11) 0.1958(6) 0.119(6) Uani 1 1 d U . . C143 C 0.1221(11) 0.4888(10) 0.2408(7) 0.113(6) Uani 1 1 d U . . H43D H 0.0695 0.5078 0.2376 0.136 Uiso 1 1 calc R . . H43E H 0.1322 0.4903 0.2741 0.136 Uiso 1 1 calc R . . H43F H 0.1377 0.4417 0.2385 0.136 Uiso 1 1 calc R . . N17 N 0.4873(11) 0.7701(13) 0.1401(7) 0.159(9) Uani 1 1 d U . . C144 C -0.5315(12) 0.7401(12) 0.1787(7) 0.111(6) Uani 1 1 d U . . C145 C 0.4560(14) 0.6990(13) 0.2234(9) 0.155(9) Uani 1 1 d U . . H45D H 0.4072 0.6935 0.2262 0.186 Uiso 1 1 calc R . . H45E H 0.4588 0.7178 0.2511 0.186 Uiso 1 1 calc R . . H45F H 0.4928 0.6548 0.2261 0.186 Uiso 1 1 calc R . . N18 N -0.187(2) 0.7719(18) -0.1588(16) 0.155(17) Uani 0.50 1 d PU . . C146 C 0.807(3) 0.821(3) 0.810(2) 0.141(16) Uani 0.50 1 d PU . . C147 C 0.789(3) 0.881(3) 0.7792(16) 0.157(18) Uani 0.50 1 d PU . . H47D H 0.7636 0.8801 0.7517 0.188 Uiso 0.50 1 calc PR . . H47E H 0.8329 0.8952 0.7642 0.188 Uiso 0.50 1 calc PR . . H47F H 0.7564 0.9126 0.7986 0.188 Uiso 0.50 1 calc PR . . N19 N 0.1641(17) 0.6704(19) 0.2898(13) 0.124(10) Uani 0.50 1 d PU . . C148 C 0.248(2) 0.635(3) 0.2976(16) 0.126(13) Uani 0.50 1 d PU . . C149 C 0.310(2) 0.629(2) 0.3026(11) 0.132(15) Uani 0.50 1 d PU . . H49D H 0.3336 0.6491 0.2697 0.158 Uiso 0.50 1 calc PR . . H49E H 0.3359 0.5806 0.3138 0.158 Uiso 0.50 1 calc PR . . H49F H 0.3101 0.6516 0.3285 0.158 Uiso 0.50 1 calc PR . . N20 N 0.5079(8) 0.5062(10) 0.4319(6) 0.116(5) Uani 1 1 d U . . C150 C 0.5005(11) 0.5260(13) 0.3909(8) 0.122(7) Uani 1 1 d U . . C151 C 0.4930(16) 0.5549(14) 0.3370(8) 0.190(13) Uani 1 1 d U . . H51D H 0.4412 0.5774 0.3321 0.228 Uiso 1 1 calc R . . H51E H 0.5117 0.5191 0.3188 0.228 Uiso 1 1 calc R . . H51F H 0.5208 0.5880 0.3234 0.228 Uiso 1 1 calc R . . O29 O 0.8065(8) 0.6873(7) 0.6861(3) 0.115(4) Uani 1 1 d U . . O30 O 0.6505(12) 0.2877(8) 0.6342(6) 0.169(7) Uani 1 1 d U . . O31 O 0.3485(15) 0.5138(14) 0.2250(10) 0.122(8) Uiso 0.50 1 d P . . O32 O 0.7789(19) 0.4865(17) 0.6889(13) 0.153(11) Uiso 0.50 1 d P . . O33 O 0.645(2) 0.0513(18) 0.1990(13) 0.162(12) Uiso 0.50 1 d P . . O34 O 0.438(3) 0.921(3) 0.2933(19) 0.230(19) Uiso 0.50 1 d P . . O35 C 0.6558(10) 0.9068(9) -0.0801(7) 0.101(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0401(4) 0.0314(4) 0.0515(5) -0.0080(3) -0.0051(3) -0.0111(3) N1 0.048(4) 0.029(4) 0.061(5) -0.004(4) -0.004(4) -0.008(3) N2 0.054(4) 0.021(4) 0.059(5) -0.015(4) -0.015(4) -0.002(3) N3 0.047(4) 0.005(3) 0.038(4) -0.005(3) -0.001(3) -0.010(3) N4 0.026(4) 0.029(4) 0.050(4) -0.004(3) -0.004(4) -0.004(3) N5 0.042(4) 0.029(4) 0.037(4) -0.012(3) 0.001(3) -0.019(4) N6 0.034(4) 0.033(4) 0.041(4) -0.015(3) -0.006(3) -0.010(3) C1 0.061(6) 0.034(6) 0.099(9) -0.027(6) -0.003(6) -0.007(4) C2 0.056(6) 0.049(7) 0.099(9) -0.033(6) -0.016(6) -0.007(5) C3 0.050(5) 0.027(5) 0.033(5) 0.003(4) -0.004(4) -0.013(4) C4 0.038(4) 0.034(5) 0.024(4) 0.004(4) -0.001(3) -0.009(4) C5 0.045(4) 0.022(5) 0.025(4) -0.004(3) -0.002(3) -0.016(4) C6 0.040(4) 0.046(6) 0.029(4) 0.000(4) -0.006(4) -0.017(4) C7 0.044(4) 0.025(5) 0.033(5) 0.000(4) 0.000(4) -0.012(4) C8 0.042(4) 0.019(5) 0.029(4) -0.004(3) -0.002(3) -0.017(4) C9 0.040(4) 0.028(5) 0.030(4) -0.011(4) 0.003(3) -0.019(4) C10 0.046(5) 0.029(5) 0.034(4) -0.008(4) 0.001(4) -0.016(4) C11 0.045(5) 0.021(5) 0.034(4) -0.006(4) -0.007(4) -0.013(4) C12 0.044(4) 0.017(5) 0.027(4) -0.005(3) 0.000(3) -0.018(4) C13 0.056(6) 0.032(5) 0.052(5) -0.003(4) -0.016(5) -0.007(5) C14 0.062(7) 0.045(5) 0.045(5) -0.007(4) -0.022(5) -0.013(5) C15 0.036(5) 0.037(4) 0.042(5) -0.008(3) -0.004(4) -0.016(4) C16 0.112(10) 0.032(5) 0.036(5) -0.006(4) -0.007(6) -0.029(6) C17 0.111(10) 0.031(5) 0.047(6) 0.003(4) -0.014(6) -0.035(6) C18 0.030(5) 0.035(4) 0.036(5) -0.006(3) -0.006(4) -0.009(4) C19 0.055(6) 0.037(5) 0.038(5) -0.009(4) 0.000(4) -0.019(5) C20 0.044(6) 0.039(5) 0.032(4) -0.006(4) -0.006(4) -0.015(5) C22 0.048(6) 0.042(5) 0.031(4) -0.011(4) -0.003(4) -0.012(5) C23 0.040(5) 0.037(5) 0.040(5) -0.001(4) -0.006(4) -0.008(5) C24 0.053(7) 0.035(5) 0.057(6) -0.018(4) -0.007(5) -0.021(5) Pd2 0.1071(9) 0.1363(11) 0.0677(7) -0.0447(7) 0.0087(6) -0.0683(9) N7 0.137(9) 0.182(12) 0.099(9) -0.086(10) 0.037(8) -0.098(9) N8 0.123(6) 0.213(14) 0.086(9) -0.099(10) 0.031(8) -0.097(8) N9 0.126(5) 0.096(8) 0.038(5) -0.026(5) -0.003(4) -0.054(5) N10 0.092(7) 0.112(6) 0.049(5) -0.026(5) 0.009(5) -0.058(6) N11 0.097(7) 0.047(6) 0.060(6) -0.005(5) 0.002(5) -0.021(6) N12 0.088(8) 0.064(6) 0.063(6) -0.001(5) 0.002(5) -0.029(6) C25 0.151(13) 0.214(15) 0.126(13) -0.099(14) 0.041(12) -0.126(12) C26 0.133(10) 0.230(17) 0.120(13) -0.109(14) 0.027(11) -0.111(11) C27 0.115(6) 0.099(10) 0.040(6) -0.026(6) 0.014(5) -0.045(8) C28 0.119(7) 0.068(8) 0.041(6) -0.013(5) 0.001(5) -0.045(7) C29 0.111(6) 0.062(8) 0.041(6) -0.009(5) -0.001(4) -0.040(7) C30 0.113(7) 0.096(10) 0.035(6) -0.014(6) -0.009(5) -0.047(8) C31 0.109(6) 0.102(11) 0.055(6) -0.004(7) -0.006(6) -0.051(8) C32 0.114(6) 0.049(7) 0.033(5) -0.007(5) -0.003(4) -0.026(7) C33 0.110(7) 0.059(8) 0.037(5) 0.000(5) -0.007(5) -0.026(7) C34 0.108(7) 0.058(8) 0.043(5) -0.010(6) -0.003(6) -0.024(7) C35 0.120(8) 0.048(7) 0.038(5) 0.003(5) 0.005(5) -0.025(8) C36 0.118(7) 0.074(9) 0.028(5) -0.005(6) -0.006(5) -0.033(8) C37 0.080(8) 0.096(8) 0.049(6) -0.019(5) -0.005(6) -0.039(8) C38 0.079(8) 0.101(7) 0.029(5) -0.011(5) 0.001(5) -0.041(7) C39 0.052(7) 0.094(7) 0.046(6) -0.012(5) 0.001(5) -0.027(6) C40 0.080(8) 0.097(8) 0.036(5) 0.000(5) -0.010(6) -0.030(8) C41 0.084(9) 0.127(8) 0.054(6) -0.021(6) -0.009(7) -0.054(9) C42 0.053(7) 0.082(6) 0.043(6) -0.010(5) 0.009(5) -0.015(6) C43 0.085(8) 0.060(6) 0.029(5) 0.000(5) 0.005(5) -0.018(6) C44 0.097(9) 0.061(7) 0.039(6) -0.014(4) 0.010(6) -0.020(6) C45 0.093(10) 0.082(8) 0.059(7) 0.005(6) -0.008(6) -0.025(8) C46 0.088(9) 0.100(8) 0.045(6) 0.004(6) -0.015(6) -0.032(8) C47 0.138(14) 0.047(7) 0.072(9) -0.017(6) -0.002(8) -0.015(7) O1 0.077(5) 0.056(5) 0.058(4) -0.025(4) 0.012(4) -0.038(4) O2 0.068(5) 0.100(6) 0.048(4) -0.016(4) -0.002(4) -0.053(5) O3 0.070(5) 0.062(5) 0.053(4) -0.010(4) 0.005(4) -0.039(4) O4 0.047(4) 0.063(5) 0.072(5) -0.028(4) 0.009(3) -0.021(4) O5 0.057(5) 0.058(5) 0.087(5) -0.021(4) -0.028(4) -0.015(4) O6 0.064(4) 0.047(4) 0.066(5) -0.019(4) -0.021(4) -0.011(3) O7 0.052(4) 0.049(4) 0.045(4) -0.011(3) -0.006(3) -0.021(3) O8 0.070(4) 0.058(5) 0.055(4) -0.004(4) -0.015(3) -0.022(4) O9 0.089(5) 0.042(5) 0.081(5) 0.002(4) -0.025(4) -0.031(4) O10 0.076(6) 0.058(5) 0.087(5) -0.025(4) -0.003(4) -0.030(4) O11 0.141(8) 0.114(8) 0.068(6) -0.003(5) -0.027(5) -0.088(7) O12 0.065(5) 0.052(4) 0.062(5) -0.012(4) -0.007(4) -0.014(4) O13 0.079(5) 0.059(4) 0.039(4) -0.014(3) 0.012(3) -0.027(4) O14 0.078(5) 0.050(5) 0.037(4) -0.014(3) 0.008(3) -0.023(4) C48 0.070(5) 0.034(6) 0.050(5) -0.014(4) 0.013(4) -0.037(5) C49 0.090(6) 0.052(7) 0.042(5) -0.015(5) -0.002(4) -0.038(6) C50 0.080(6) 0.056(7) 0.046(5) -0.009(5) -0.006(5) -0.033(6) C51 0.070(6) 0.038(6) 0.039(5) -0.008(4) 0.000(4) -0.027(5) C52 0.069(5) 0.012(5) 0.040(4) -0.010(4) 0.000(3) -0.019(4) C53 0.075(5) 0.030(6) 0.046(5) -0.012(4) 0.000(4) -0.016(5) C54 0.086(6) 0.039(6) 0.047(6) -0.013(5) -0.006(4) -0.019(6) C55 0.080(6) 0.036(6) 0.059(5) -0.022(5) -0.008(5) -0.019(5) C56 0.070(6) 0.032(6) 0.056(5) -0.013(5) 0.006(4) -0.030(5) C57 0.075(5) 0.022(5) 0.052(4) -0.014(4) 0.000(4) -0.028(5) C58 0.091(7) 0.073(8) 0.058(6) -0.024(6) 0.010(6) -0.054(7) C59 0.082(7) 0.093(9) 0.076(8) -0.043(7) -0.003(6) -0.038(7) C60 0.075(8) 0.104(8) 0.040(6) -0.014(6) -0.013(6) -0.032(7) C61 0.090(8) 0.068(8) 0.042(6) 0.000(5) 0.004(6) -0.040(6) C62 0.081(7) 0.065(7) 0.061(7) -0.005(5) 0.011(6) -0.041(5) C63 0.062(6) 0.082(8) 0.069(7) -0.023(6) 0.022(6) -0.031(6) C64 0.042(6) 0.071(8) 0.111(7) -0.022(7) 0.013(6) -0.018(5) C65 0.055(7) 0.069(9) 0.121(7) -0.017(7) -0.014(6) -0.019(6) C66 0.075(8) 0.063(7) 0.094(7) -0.016(7) -0.041(7) 0.000(6) C67 0.071(7) 0.077(8) 0.075(8) -0.020(6) -0.034(7) -0.003(6) C68 0.070(7) 0.064(7) 0.072(8) -0.021(6) -0.033(6) -0.013(5) C69 0.070(6) 0.052(7) 0.054(6) -0.022(5) -0.019(5) -0.016(5) C70 0.047(5) 0.041(6) 0.054(5) -0.017(4) -0.004(4) -0.022(4) C71 0.060(5) 0.051(7) 0.046(5) -0.015(5) -0.009(4) -0.021(5) C72 0.049(5) 0.069(8) 0.049(5) -0.028(5) 0.007(5) -0.024(5) C73 0.056(6) 0.046(6) 0.053(5) -0.017(5) -0.010(4) -0.016(5) C74 0.059(5) 0.031(5) 0.050(4) -0.018(4) -0.003(4) -0.019(4) C75 0.058(5) 0.026(5) 0.053(5) -0.003(4) -0.006(4) -0.018(4) C76 0.071(6) 0.046(7) 0.043(5) 0.000(5) -0.005(4) -0.025(5) C77 0.067(6) 0.036(6) 0.049(5) -0.009(5) 0.005(5) -0.022(5) C78 0.056(6) 0.033(6) 0.052(5) -0.009(4) -0.002(4) -0.020(5) C79 0.055(5) 0.028(5) 0.044(4) -0.008(4) -0.003(3) -0.030(4) C80 0.087(6) 0.066(8) 0.056(6) -0.002(6) -0.026(5) -0.027(6) C81 0.081(7) 0.063(8) 0.069(8) 0.009(6) -0.024(5) -0.028(6) C82 0.062(7) 0.043(7) 0.109(8) 0.003(6) -0.020(6) -0.018(6) C83 0.072(8) 0.059(8) 0.089(7) -0.017(5) 0.003(6) -0.006(7) C84 0.078(9) 0.089(9) 0.092(7) -0.033(6) 0.009(7) -0.052(7) C85 0.101(10) 0.091(10) 0.105(8) -0.027(7) -0.021(7) -0.040(8) C86 0.120(11) 0.113(11) 0.070(8) -0.003(7) -0.041(7) -0.054(9) C87 0.118(10) 0.086(9) 0.058(7) 0.003(6) -0.033(7) -0.046(8) C88 0.068(8) 0.068(6) 0.058(7) -0.019(5) -0.008(5) -0.020(5) C89 0.070(7) 0.060(5) 0.055(7) -0.029(5) 0.013(5) -0.028(5) C90 0.116(9) 0.048(6) 0.055(7) -0.015(5) 0.019(6) -0.036(6) C91 0.107(8) 0.043(6) 0.028(5) -0.004(5) 0.004(5) -0.010(6) O15 0.093(5) 0.096(7) 0.030(4) -0.010(4) -0.009(4) -0.021(5) O16 0.111(8) 0.162(10) 0.046(5) -0.019(6) -0.022(5) -0.036(7) O17 0.105(9) 0.210(11) 0.086(7) -0.079(7) 0.020(6) -0.076(8) O18 0.36(3) 0.177(15) 0.262(19) -0.118(13) 0.095(17) -0.023(17) O19 0.55(3) 0.25(2) 0.177(14) -0.074(16) 0.00(2) -0.03(2) O20 0.47(2) 0.120(10) 0.138(12) -0.037(9) 0.106(15) -0.124(14) O21 0.417(17) 0.102(10) 0.118(10) -0.036(9) 0.052(11) -0.094(15) O22 0.338(15) 0.071(8) 0.098(8) -0.017(7) -0.007(8) -0.054(12) O23 0.310(19) 0.201(19) 0.160(14) 0.047(13) -0.014(16) 0.017(15) O24 0.28(3) 0.27(2) 0.222(16) 0.001(16) 0.040(16) -0.038(17) O25 0.174(14) 0.197(15) 0.114(10) 0.010(10) 0.015(9) 0.017(12) O26 0.194(12) 0.074(7) 0.075(6) 0.006(5) 0.019(8) -0.004(7) O27 0.088(6) 0.071(5) 0.066(5) 0.006(4) -0.012(5) -0.020(4) O28 0.076(5) 0.071(6) 0.045(4) 0.000(4) -0.003(3) -0.017(4) C92 0.083(6) 0.058(7) 0.037(5) -0.002(5) -0.001(4) -0.021(6) C93 0.098(6) 0.070(8) 0.042(6) 0.002(6) 0.001(5) -0.030(7) C94 0.089(6) 0.070(8) 0.058(6) -0.016(6) 0.011(6) -0.036(7) C95 0.076(6) 0.055(7) 0.058(5) -0.006(6) 0.000(5) -0.020(6) C96 0.078(6) 0.043(6) 0.045(4) -0.010(5) -0.001(4) -0.016(6) C97 0.073(5) 0.055(7) 0.048(5) -0.010(5) -0.006(4) -0.014(6) C98 0.079(6) 0.085(9) 0.039(5) -0.005(6) -0.006(4) -0.027(7) C99 0.071(6) 0.078(8) 0.034(5) -0.012(5) 0.000(5) -0.019(6) C100 0.076(6) 0.077(8) 0.034(5) -0.004(6) -0.005(4) -0.013(7) C101 0.076(6) 0.059(7) 0.040(4) -0.005(5) -0.001(4) -0.018(6) C102 0.136(9) 0.101(11) 0.037(6) 0.000(7) -0.023(7) -0.046(9) C103 0.134(10) 0.130(13) 0.057(8) -0.009(8) -0.037(8) -0.025(10) C104 0.118(12) 0.240(14) 0.063(9) -0.028(9) -0.023(9) -0.093(12) C105 0.108(13) 0.236(15) 0.142(16) -0.030(12) -0.026(11) -0.086(9) C106 0.194(19) 0.256(17) 0.148(16) -0.127(12) 0.080(14) -0.121(14) C107 0.26(3) 0.257(19) 0.20(2) -0.170(16) 0.055(16) -0.048(14) C108 0.50(3) 0.204(17) 0.27(2) -0.123(19) 0.06(2) 0.04(2) C109 0.54(3) 0.22(2) 0.28(2) -0.10(2) 0.02(2) -0.02(3) C110 0.56(3) 0.19(2) 0.176(17) -0.081(16) -0.05(2) -0.03(2) C111 0.50(2) 0.153(18) 0.175(17) -0.065(15) 0.02(2) -0.13(2) C112 0.46(2) 0.095(11) 0.146(17) -0.073(11) 0.094(16) -0.122(16) C113 0.48(2) 0.135(15) 0.125(13) -0.034(13) 0.069(15) -0.151(18) C114 0.395(17) 0.061(11) 0.129(10) -0.037(12) 0.024(9) -0.076(18) C115 0.407(19) 0.069(12) 0.097(12) -0.028(12) 0.022(10) -0.05(2) C116 0.399(18) 0.057(11) 0.125(10) -0.018(11) 0.017(13) -0.079(18) C117 0.270(13) 0.060(10) 0.143(10) -0.019(10) -0.007(10) -0.074(12) C118 0.198(7) 0.196(7) 0.196(7) -0.050(2) -0.0195(12) -0.056(2) C119 0.324(15) 0.061(11) 0.162(9) -0.048(12) -0.015(8) -0.045(17) C120 0.332(18) 0.096(14) 0.139(12) -0.057(12) 0.015(10) -0.093(19) C121 0.323(17) 0.126(16) 0.142(12) -0.032(15) -0.006(14) -0.07(2) C122 0.232(12) 0.111(15) 0.163(12) -0.050(14) 0.001(11) -0.065(15) C123 0.262(11) 0.043(9) 0.150(9) -0.025(9) -0.013(7) -0.059(12) C124 0.43(2) 0.051(10) 0.088(11) -0.011(9) 0.008(12) -0.035(13) C125 0.32(2) 0.080(12) 0.064(10) -0.001(9) 0.057(14) -0.012(13) C126 0.22(2) 0.19(2) 0.145(12) 0.076(14) 0.067(14) 0.003(14) C127 0.25(2) 0.21(2) 0.154(13) 0.007(15) 0.091(15) -0.029(18) C128 0.25(2) 0.27(3) 0.200(18) 0.00(2) 0.080(15) -0.02(2) C129 0.193(19) 0.29(2) 0.189(17) -0.018(17) 0.057(16) -0.013(19) C130 0.204(15) 0.186(19) 0.146(13) 0.060(15) 0.014(14) 0.059(15) C131 0.233(19) 0.111(14) 0.120(14) 0.007(9) 0.036(13) 0.038(13) C132 0.171(16) 0.083(9) 0.099(10) 0.006(8) -0.010(11) -0.005(9) C133 0.141(13) 0.083(7) 0.058(8) 0.009(6) -0.014(8) -0.012(8) C134 0.081(7) 0.082(7) 0.068(8) 0.002(6) -0.021(6) -0.027(7) C135 0.081(7) 0.068(8) 0.058(6) -0.004(6) -0.018(6) -0.024(6) P1 0.116(3) 0.082(2) 0.0341(16) -0.0104(16) -0.0098(17) -0.042(2) F1 0.150(9) 0.124(7) 0.157(9) -0.021(6) -0.055(7) -0.003(6) F2 0.151(8) 0.150(8) 0.101(6) -0.047(6) -0.022(6) -0.072(7) F3 0.231(11) 0.092(6) 0.090(6) -0.008(5) -0.023(6) 0.009(6) F4 0.156(8) 0.233(12) 0.027(4) -0.013(5) 0.001(4) -0.058(7) F5 0.165(9) 0.201(11) 0.060(5) -0.020(6) 0.016(5) -0.081(7) F6 0.211(11) 0.198(11) 0.124(8) -0.067(8) -0.022(7) -0.114(9) P2 0.078(3) 0.158(4) 0.064(2) -0.016(2) -0.001(2) -0.016(3) F7 0.078(5) 0.238(13) 0.135(9) -0.022(8) 0.002(5) -0.023(6) F8 0.155(10) 0.247(13) 0.087(6) -0.058(7) -0.018(6) -0.022(9) F9 0.177(11) 0.182(8) 0.101(7) 0.018(6) 0.005(7) -0.040(8) F10 0.158(10) 0.210(9) 0.118(8) 0.025(7) 0.005(8) -0.063(8) F11 0.129(8) 0.292(14) 0.070(5) -0.048(7) 0.003(5) -0.069(9) F12 0.078(5) 0.237(12) 0.202(12) -0.107(10) -0.014(6) -0.010(6) P3 0.076(2) 0.119(3) 0.057(2) -0.0229(19) -0.0055(17) -0.034(2) F13 0.097(5) 0.184(10) 0.104(7) -0.048(6) 0.023(5) -0.064(6) F14 0.155(8) 0.189(8) 0.075(5) 0.020(6) -0.035(5) -0.083(7) F15 0.071(4) 0.101(6) 0.085(5) -0.031(4) -0.014(4) -0.021(4) F16 0.072(5) 0.103(5) 0.102(5) -0.017(4) -0.008(4) -0.016(4) F17 0.098(6) 0.197(9) 0.136(7) -0.109(7) 0.011(6) -0.045(7) F18 0.105(6) 0.117(6) 0.085(5) -0.019(4) -0.029(4) -0.043(5) P4 0.0523(19) 0.072(2) 0.085(2) -0.0269(18) -0.0075(16) -0.0171(16) F19 0.069(5) 0.109(6) 0.110(6) -0.051(5) -0.015(4) -0.009(4) F20 0.083(5) 0.067(4) 0.077(5) -0.012(3) -0.012(3) -0.032(4) F21 0.066(5) 0.065(5) 0.129(6) 0.003(4) -0.024(4) -0.021(4) F22 0.056(4) 0.126(7) 0.119(7) -0.043(5) 0.004(4) -0.038(4) F23 0.101(6) 0.114(6) 0.111(6) -0.016(5) -0.048(5) -0.007(5) F24 0.101(6) 0.109(6) 0.128(6) -0.071(5) 0.030(5) -0.051(5) P5 0.128(3) 0.104(3) 0.0391(19) -0.0144(18) -0.0133(19) -0.040(3) F25 0.273(13) 0.128(7) 0.060(5) -0.026(5) -0.001(6) -0.063(7) F26 0.132(8) 0.142(7) 0.074(5) -0.040(5) 0.004(5) -0.055(6) F27 0.169(9) 0.184(10) 0.059(5) 0.000(5) -0.032(5) -0.032(7) F28 0.176(9) 0.310(15) 0.137(9) -0.137(9) 0.047(7) -0.149(11) F29 0.275(12) 0.213(13) 0.102(8) -0.041(7) 0.035(7) -0.170(11) F30 0.283(13) 0.224(12) 0.062(6) -0.039(6) -0.059(8) 0.079(10) P6 0.125(4) 0.179(6) 0.070(3) 0.013(3) 0.008(3) -0.010(4) F31 0.237(13) 0.189(11) 0.116(7) -0.026(7) 0.076(8) -0.093(10) F32 0.161(8) 0.242(14) 0.103(8) 0.019(8) -0.039(7) -0.014(8) F33 0.130(9) 0.248(11) 0.107(8) 0.057(7) 0.019(7) -0.040(8) F34 0.120(7) 0.272(16) 0.202(12) 0.087(10) -0.019(7) -0.037(8) F35 0.191(10) 0.168(8) 0.070(6) -0.005(6) 0.011(6) -0.036(8) F36 0.282(16) 0.313(15) 0.047(5) -0.023(7) -0.013(7) -0.044(12) P7 0.221(6) 0.148(5) 0.086(3) 0.001(3) -0.042(4) -0.083(5) F37 0.40(2) 0.310(17) 0.111(9) 0.027(11) 0.015(14) -0.171(16) F38 0.251(9) 0.204(15) 0.67(4) -0.23(2) -0.129(15) -0.022(12) F39 0.37(2) 0.39(3) 0.140(10) -0.129(14) 0.007(12) -0.193(16) F40 0.51(2) 0.42(3) 0.160(14) 0.025(12) 0.029(14) -0.34(2) F41 0.36(2) 0.285(16) 0.278(18) -0.145(15) -0.159(16) -0.029(14) F42 0.322(15) 0.123(11) 0.41(2) 0.022(11) -0.204(16) -0.054(10) P8 0.234(9) 0.164(6) 0.132(5) -0.026(5) -0.036(5) -0.046(6) F43 0.284(18) 0.234(14) 0.126(8) -0.025(9) -0.020(8) -0.091(13) F44 0.38(2) 0.43(2) 0.196(14) 0.003(19) -0.132(16) -0.187(19) F45 0.38(2) 0.332(19) 0.114(8) -0.022(11) -0.010(10) -0.142(19) F46 0.50(3) 0.183(10) 0.208(17) -0.077(11) -0.039(16) 0.016(14) F47 0.232(15) 0.39(2) 0.173(13) -0.081(16) -0.035(11) -0.102(13) F48 0.254(18) 0.139(8) 0.38(2) -0.050(11) 0.029(16) -0.036(10) N13 0.145(16) 0.26(2) 0.114(14) -0.099(14) 0.022(11) -0.078(15) C136 0.18(2) 0.23(2) 0.096(14) -0.078(13) 0.030(12) -0.126(18) C137 0.18(2) 0.24(3) 0.098(14) -0.081(15) 0.023(13) -0.10(2) N14 0.164(13) 0.076(8) 0.051(5) -0.031(6) -0.033(7) -0.010(8) C138 0.170(16) 0.075(10) 0.063(6) -0.033(7) -0.026(9) -0.038(10) C139 0.33(3) 0.103(14) 0.064(7) -0.010(9) -0.028(14) -0.099(17) N15 0.201(17) 0.104(11) 0.055(6) -0.012(7) 0.015(9) -0.057(11) C140 0.20(2) 0.120(14) 0.058(7) -0.025(8) 0.007(11) -0.073(14) C141 0.29(3) 0.21(2) 0.058(9) -0.011(11) -0.025(15) -0.12(2) N16 0.192(15) 0.080(9) 0.036(6) -0.002(6) -0.010(7) -0.014(8) C142 0.153(17) 0.137(16) 0.049(9) -0.008(9) -0.016(9) -0.030(11) C143 0.126(14) 0.121(15) 0.093(11) -0.001(10) -0.033(10) -0.048(11) N17 0.161(17) 0.26(2) 0.104(13) -0.005(14) -0.023(11) -0.159(18) C144 0.138(16) 0.152(18) 0.072(11) -0.010(11) -0.005(10) -0.099(14) C145 0.16(2) 0.19(2) 0.14(2) -0.010(18) -0.060(16) -0.078(19) N18 0.18(3) 0.11(3) 0.17(3) 0.07(2) -0.12(3) -0.08(2) C146 0.20(4) 0.17(4) 0.12(3) -0.08(2) 0.04(3) -0.13(3) C147 0.18(4) 0.22(4) 0.07(2) -0.06(2) 0.02(3) -0.06(4) N19 0.099(15) 0.15(3) 0.13(2) -0.02(2) -0.031(18) -0.052(18) C148 0.098(16) 0.16(3) 0.10(2) -0.03(2) 0.01(2) -0.03(2) C149 0.091(15) 0.22(4) 0.043(15) -0.04(2) -0.022(16) 0.02(2) N20 0.098(10) 0.204(17) 0.079(7) -0.070(10) 0.001(8) -0.061(11) C150 0.100(13) 0.22(2) 0.075(8) -0.065(12) 0.012(10) -0.070(13) C151 0.20(3) 0.20(2) 0.091(9) -0.030(15) -0.010(15) 0.04(2) O29 0.171(11) 0.156(11) 0.038(5) 0.000(6) -0.006(6) -0.099(9) O30 0.26(2) 0.130(12) 0.107(10) -0.014(9) 0.031(11) -0.088(13) _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 N1 2.005(8) . ? Pd1 N4 2.026(8) . ? Pd1 N2 2.057(8) . ? Pd1 N3 2.064(7) . ? N1 C1 1.441(15) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.469(14) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C7 1.329(12) . ? N3 C3 1.335(12) . ? N4 C13 1.313(13) . ? N4 C17 1.324(13) . ? N5 C11 1.369(12) . ? N5 C10 1.405(13) . ? N5 C24 1.454(13) 2_765 ? N6 C20 1.339(12) . ? N6 C22 1.349(12) . ? N6 C24 1.474(12) . ? C1 C2 1.485(17) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.357(14) . ? C3 H3 0.9300 . ? C4 C5 1.410(13) . ? C4 H4 0.9300 . ? C5 C6 1.392(13) . ? C5 C8 1.487(13) . ? C6 C7 1.344(14) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C12 1.409(13) . ? C8 C9 1.434(13) . ? C9 C10 1.326(13) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.347(13) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.387(15) . ? C13 H13 0.9300 . ? C14 C15 1.371(14) . ? C14 H14 0.9300 . ? C15 C16 1.385(15) . ? C15 C18 1.486(14) . ? C16 C17 1.346(15) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.376(13) . ? C18 C23 1.417(14) . ? C19 C20 1.365(14) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C23 1.345(14) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 N5 1.454(13) 2_765 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? Pd2 N7 2.002(13) . ? Pd2 N9 2.006(14) . ? Pd2 N10 2.018(12) . ? Pd2 N8 2.020(15) . ? N7 C25 1.47(2) . ? N7 H7A 0.9000 . ? N7 H7B 0.9000 . ? N8 C26 1.55(2) . ? N8 H8A 0.9000 . ? N8 H8B 0.9000 . ? N9 C27 1.320(19) . ? N9 C31 1.354(17) . ? N10 C41 1.322(18) . ? N10 C37 1.363(16) . ? N11 C34 1.342(16) . ? N11 C35 1.361(19) . ? N11 C47 1.51(2) 2_766 ? N12 C45 1.342(19) . ? N12 C44 1.361(16) . ? N12 C47 1.457(19) . ? C25 C26 1.43(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.38(2) . ? C27 H27 0.9300 . ? C28 C29 1.419(18) . ? C28 H28 0.9300 . ? C29 C32 1.40(2) . ? C29 C30 1.42(2) . ? C30 C31 1.36(2) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.406(19) . ? C32 C36 1.408(17) . ? C33 C34 1.363(19) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.32(2) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.407(19) . ? C37 H37 0.9300 . ? C38 C39 1.386(18) . ? C38 H38 0.9300 . ? C39 C40 1.380(18) . ? C39 C42 1.475(19) . ? C40 C41 1.39(2) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.390(18) . ? C42 C46 1.416(18) . ? C43 C44 1.332(18) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.28(2) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 N11 1.51(2) 2_766 ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? O1 C48 1.342(11) . ? O1 C58 1.421(12) . ? O2 C60 1.388(13) . ? O2 C59 1.453(13) . ? O3 C61 1.436(13) . ? O3 C62 1.471(14) . ? O4 C63 1.382(14) . ? O4 C64 1.387(15) . ? O5 C66 1.413(15) . ? O5 C65 1.458(15) . ? O6 C68 1.417(13) . ? O6 C67 1.445(14) . ? O7 C70 1.338(12) . ? O7 C69 1.463(12) . ? O8 C75 1.318(13) . ? O8 C80 1.504(13) . ? O9 C81 1.369(14) . ? O9 C82 1.465(16) . ? O10 C83 1.385(15) . ? O10 C84 1.415(15) . ? O11 C86 1.437(15) . ? O11 C85 1.464(17) . ? O12 C87 1.378(14) . ? O12 C88 1.430(13) . ? O13 C89 1.420(12) . ? O13 C90 1.424(13) . ? O14 C53 1.357(12) . ? O14 C91 1.469(11) . ? C48 C49 1.352(14) . ? C48 C57 1.456(13) . ? C49 C50 1.424(15) . ? C49 H49 0.9300 . ? C50 C51 1.390(13) . ? C50 H50 0.9300 . ? C51 C52 1.410(13) . ? C51 H51 0.9300 . ? C52 C57 1.398(13) . ? C52 C53 1.436(12) . ? C53 C54 1.365(14) . ? C54 C55 1.415(14) . ? C54 H54 0.9300 . ? C55 C56 1.378(13) . ? C55 H55 0.9300 . ? C56 C57 1.417(14) . ? C56 H56 0.9300 . ? C58 C59 1.460(16) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.456(16) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.458(18) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63 0.9300 . ? C64 C65 1.51(2) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.468(18) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.474(16) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.378(15) . ? C70 C79 1.464(14) . ? C71 C72 1.345(15) . ? C71 H71 0.9300 . ? C72 C73 1.410(14) . ? C72 H72 0.9300 . ? C73 C74 1.345(15) . ? C73 H73 0.9300 . ? C74 C79 1.361(14) . ? C74 C75 1.487(15) . ? C75 C76 1.374(15) . ? C76 C77 1.381(15) . ? C76 H76 0.9300 . ? C77 C78 1.389(15) . ? C77 H77 0.9300 . ? C78 C79 1.432(14) . ? C78 H78 0.9300 . ? C80 C81 1.486(17) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 C83 1.487(19) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C84 C85 1.451(19) . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C86 C87 1.494(19) . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C88 C89 1.481(15) . ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C90 C91 1.462(15) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? O15 C92 1.337(13) . ? O15 C102 1.417(13) . ? O16 C104 1.383(15) . ? O16 C103 1.452(16) . ? O17 C105 1.419(18) . ? O17 C106 1.447(18) . ? O18 C107 1.34(2) . ? O18 C108 1.38(2) . ? O19 C110 1.41(2) . ? O19 C109 1.46(2) . ? O20 C112 1.40(2) . ? O20 C111 1.43(2) . ? O21 C114 1.345(19) . ? O21 C113 1.466(18) . ? O22 C119 1.288(19) . ? O22 C124 1.559(17) . ? O23 C125 1.30(2) . ? O23 C126 1.47(2) . ? O24 C127 1.32(2) . ? O24 C128 1.40(2) . ? O25 C129 1.43(2) . ? O25 C130 1.465(19) . ? O26 C131 1.327(17) . ? O26 C132 1.429(17) . ? O27 C134 1.416(14) . ? O27 C133 1.418(14) . ? O28 C97 1.364(13) . ? O28 C135 1.479(12) . ? C92 C93 1.339(14) . ? C92 C101 1.445(13) . ? C93 C94 1.418(16) . ? C93 H93 0.9300 . ? C94 C95 1.394(14) . ? C94 H94 0.9300 . ? C95 C96 1.409(14) . ? C95 H95 0.9300 . ? C96 C101 1.401(14) . ? C96 C97 1.442(13) . ? C97 C98 1.370(14) . ? C98 C99 1.389(15) . ? C98 H98 0.9300 . ? C99 C100 1.380(14) . ? C99 H99 0.9300 . ? C100 C101 1.421(14) . ? C100 H100 0.9300 . ? C102 C103 1.488(18) . ? C102 H10A 0.9700 . ? C102 H10B 0.9700 . ? C103 H10C 0.9700 . ? C103 H10D 0.9700 . ? C104 C105 1.481(19) . ? C104 H10E 0.9700 . ? C104 H10F 0.9700 . ? C105 H10G 0.9700 . ? C105 H10H 0.9700 . ? C106 C107 1.41(2) . ? C106 H106 0.9300 . ? C107 H107 0.9300 . ? C108 C109 1.50(3) . ? C108 H10I 0.9700 . ? C108 H10J 0.9700 . ? C109 H10K 0.9700 . ? C109 H10L 0.9700 . ? C110 C111 1.45(2) . ? C110 H11A 0.9700 . ? C110 H11B 0.9700 . ? C111 H11C 0.9700 . ? C111 H11D 0.9700 . ? C112 C113 1.48(2) . ? C112 H11E 0.9700 . ? C112 H11F 0.9700 . ? C113 H11G 0.9700 . ? C113 H11H 0.9700 . ? C114 C115 1.34(2) . ? C114 C123 1.525(19) . ? C115 C116 1.33(2) . ? C115 H115 0.9300 . ? C116 C117 1.446(19) . ? C116 H116 0.9300 . ? C117 C118 1.32(2) . ? C117 H117 0.9300 . ? C118 C123 1.33(2) . ? C118 C119 1.51(2) . ? C119 C120 1.36(2) . ? C120 C121 1.37(2) . ? C120 H120 0.9300 . ? C121 C122 1.41(2) . ? C121 H121 0.9300 . ? C122 C123 1.44(2) . ? C122 H122 0.9300 . ? C124 C125 1.51(2) . ? C124 H12A 0.9700 . ? C124 H12B 0.9700 . ? C125 H12C 0.9700 . ? C125 H12D 0.9700 . ? C126 C127 1.49(2) . ? C126 H12E 0.9700 . ? C126 H12F 0.9700 . ? C127 H12G 0.9700 . ? C127 H12H 0.9700 . ? C128 C129 1.45(2) . ? C128 H12I 0.9700 . ? C128 H12J 0.9700 . ? C129 H12K 0.9700 . ? C129 H12L 0.9700 . ? C130 C131 1.50(2) . ? C130 H13A 0.9700 . ? C130 H13B 0.9700 . ? C131 H13C 0.9700 . ? C131 H13D 0.9700 . ? C132 C133 1.467(17) . ? C132 H13E 0.9700 . ? C132 H13F 0.9700 . ? C133 H13G 0.9700 . ? C133 H13H 0.9700 . ? C134 C135 1.467(15) . ? C134 H13I 0.9700 . ? C134 H13J 0.9700 . ? C135 H13K 0.9700 . ? C135 H13L 0.9700 . ? P1 F1 1.546(12) . ? P1 F3 1.559(11) . ? P1 F4 1.562(9) . ? P1 F6 1.564(12) . ? P1 F2 1.565(10) . ? P1 F5 1.582(10) . ? P2 F11 1.528(13) . ? P2 F9 1.548(14) . ? P2 F7 1.565(12) . ? P2 F12 1.576(12) . ? P2 F10 1.602(14) . ? P2 F8 1.619(14) . ? P3 F13 1.537(10) . ? P3 F14 1.560(11) . ? P3 F18 1.575(10) . ? P3 F16 1.576(9) . ? P3 F15 1.585(9) . ? P3 F17 1.591(11) . ? P4 F22 1.548(9) . ? P4 F21 1.575(9) . ? P4 F24 1.591(9) . ? P4 F23 1.596(9) . ? P4 F19 1.599(9) . ? P4 F20 1.606(8) . ? P5 F28 1.487(13) . ? P5 F30 1.506(12) . ? P5 F25 1.555(12) . ? P5 F29 1.568(14) . ? P5 F27 1.575(11) . ? P5 F26 1.579(10) . ? P6 F31 1.547(16) . ? P6 F34 1.555(16) . ? P6 F35 1.556(14) . ? P6 F36 1.560(17) . ? P6 F33 1.573(15) . ? P6 F32 1.625(15) . ? P7 F39 1.478(17) . ? P7 F40 1.51(2) . ? P7 F37 1.567(18) . ? P7 F41 1.604(19) . ? P7 F42 1.62(2) . ? P7 F38 1.71(2) . ? P8 F48 1.525(19) . ? P8 F43 1.566(18) . ? P8 F46 1.58(2) . ? P8 F45 1.60(2) . ? P8 F47 1.61(2) . ? P8 F44 1.67(2) . ? N13 C136 1.14(2) . ? C136 C137 1.53(3) . ? C137 H37D 0.9600 . ? C137 H37E 0.9600 . ? C137 H37F 0.9600 . ? N14 C138 1.190(19) . ? C138 C139 1.46(2) . ? C139 H39D 0.9600 . ? C139 H39E 0.9600 . ? C139 H39F 0.9600 . ? N15 C140 1.12(2) . ? C140 C141 1.52(3) . ? C141 H41D 0.9600 . ? C141 H41E 0.9600 . ? C141 H41F 0.9600 . ? N16 C142 1.27(2) . ? C142 C143 1.55(3) . ? C143 H43D 0.9600 . ? C143 H43E 0.9600 . ? C143 H43F 0.9600 . ? N17 C144 1.10(2) 1_655 ? C144 N17 1.10(2) 1_455 ? C144 C145 1.29(3) 1_455 ? C145 C144 1.29(3) 1_655 ? C145 H45D 0.9600 . ? C145 H45E 0.9600 . ? C145 H45F 0.9600 . ? N18 C146 1.11(6) 1_454 ? C146 N18 1.11(6) 1_656 ? C146 C147 1.27(7) . ? C147 H47D 0.9600 . ? C147 H47E 0.9600 . ? C147 H47F 0.9600 . ? N19 C148 1.55(5) . ? C148 C149 1.17(5) . ? C149 H49D 0.9600 . ? C149 H49E 0.9600 . ? C149 H49F 0.9600 . ? N20 C150 1.07(2) . ? C150 C151 1.40(3) . ? C151 H51D 0.9600 . ? C151 H51E 0.9600 . ? C151 H51F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N4 173.5(3) . . ? N1 Pd1 N2 83.8(3) . . ? N4 Pd1 N2 92.2(3) . . ? N1 Pd1 N3 94.0(3) . . ? N4 Pd1 N3 90.2(3) . . ? N2 Pd1 N3 177.4(3) . . ? C1 N1 Pd1 111.0(7) . . ? C1 N1 H1A 109.4 . . ? Pd1 N1 H1A 109.4 . . ? C1 N1 H1B 109.4 . . ? Pd1 N1 H1B 109.4 . . ? H1A N1 H1B 108.0 . . ? C2 N2 Pd1 108.0(7) . . ? C2 N2 H2A 110.1 . . ? Pd1 N2 H2A 110.1 . . ? C2 N2 H2B 110.1 . . ? Pd1 N2 H2B 110.1 . . ? H2A N2 H2B 108.4 . . ? C7 N3 C3 120.0(8) . . ? C7 N3 Pd1 120.2(6) . . ? C3 N3 Pd1 119.8(6) . . ? C13 N4 C17 116.9(9) . . ? C13 N4 Pd1 125.1(6) . . ? C17 N4 Pd1 117.9(7) . . ? C11 N5 C10 117.4(8) . . ? C11 N5 C24 121.1(8) . 2_765 ? C10 N5 C24 121.5(8) . 2_765 ? C20 N6 C22 120.3(8) . . ? C20 N6 C24 120.2(8) . . ? C22 N6 C24 119.5(8) . . ? N1 C1 C2 108.9(9) . . ? N1 C1 H1C 109.9 . . ? C2 C1 H1C 109.9 . . ? N1 C1 H1D 109.9 . . ? C2 C1 H1D 109.9 . . ? H1C C1 H1D 108.3 . . ? N2 C2 C1 112.0(10) . . ? N2 C2 H2C 109.2 . . ? C1 C2 H2C 109.2 . . ? N2 C2 H2D 109.2 . . ? C1 C2 H2D 109.2 . . ? H2C C2 H2D 107.9 . . ? N3 C3 C4 120.7(9) . . ? N3 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 120.3(8) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 116.7(8) . . ? C6 C5 C8 120.8(8) . . ? C4 C5 C8 122.4(8) . . ? C7 C6 C5 119.6(9) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? N3 C7 C6 122.6(8) . . ? N3 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? C12 C8 C9 117.4(8) . . ? C12 C8 C5 120.9(8) . . ? C9 C8 C5 121.7(8) . . ? C10 C9 C8 119.9(9) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 N5 122.4(8) . . ? C9 C10 H10 118.8 . . ? N5 C10 H10 118.8 . . ? C12 C11 N5 122.6(9) . . ? C12 C11 H11 118.7 . . ? N5 C11 H11 118.7 . . ? C11 C12 C8 120.2(8) . . ? C11 C12 H12 119.9 . . ? C8 C12 H12 119.9 . . ? N4 C13 C14 122.6(9) . . ? N4 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C15 C14 C13 120.4(10) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 115.7(9) . . ? C14 C15 C18 124.1(9) . . ? C16 C15 C18 120.2(9) . . ? C17 C16 C15 120.4(10) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? N4 C17 C16 124.0(11) . . ? N4 C17 H17 118.0 . . ? C16 C17 H17 118.0 . . ? C19 C18 C23 116.3(9) . . ? C19 C18 C15 121.5(9) . . ? C23 C18 C15 122.1(8) . . ? C20 C19 C18 121.5(10) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? N6 C20 C19 120.2(9) . . ? N6 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C23 C22 N6 121.2(9) . . ? C23 C22 H22 119.4 . . ? N6 C22 H22 119.4 . . ? C22 C23 C18 120.3(9) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? N5 C24 N6 108.1(7) 2_765 . ? N5 C24 H24A 110.1 2_765 . ? N6 C24 H24A 110.1 . . ? N5 C24 H24B 110.1 2_765 . ? N6 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? N7 Pd2 N9 93.5(6) . . ? N7 Pd2 N10 171.0(6) . . ? N9 Pd2 N10 89.0(5) . . ? N7 Pd2 N8 83.9(6) . . ? N9 Pd2 N8 177.4(5) . . ? N10 Pd2 N8 93.6(6) . . ? C25 N7 Pd2 112.3(12) . . ? C25 N7 H7A 109.1 . . ? Pd2 N7 H7A 109.1 . . ? C25 N7 H7B 109.1 . . ? Pd2 N7 H7B 109.1 . . ? H7A N7 H7B 107.9 . . ? C26 N8 Pd2 103.8(11) . . ? C26 N8 H8A 111.0 . . ? Pd2 N8 H8A 111.0 . . ? C26 N8 H8B 111.0 . . ? Pd2 N8 H8B 111.0 . . ? H8A N8 H8B 109.0 . . ? C27 N9 C31 118.8(14) . . ? C27 N9 Pd2 124.4(10) . . ? C31 N9 Pd2 116.8(11) . . ? C41 N10 C37 118.8(13) . . ? C41 N10 Pd2 117.4(9) . . ? C37 N10 Pd2 123.8(10) . . ? C34 N11 C35 119.9(13) . . ? C34 N11 C47 120.0(13) . 2_766 ? C35 N11 C47 120.1(11) . 2_766 ? C45 N12 C44 120.2(13) . . ? C45 N12 C47 119.8(12) . . ? C44 N12 C47 120.0(13) . . ? C26 C25 N7 102.9(18) . . ? C26 C25 H25A 111.2 . . ? N7 C25 H25A 111.2 . . ? C26 C25 H25B 111.2 . . ? N7 C25 H25B 111.2 . . ? H25A C25 H25B 109.1 . . ? C25 C26 N8 112(2) . . ? C25 C26 H26A 109.1 . . ? N8 C26 H26A 109.1 . . ? C25 C26 H26B 109.1 . . ? N8 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? N9 C27 C28 123.4(12) . . ? N9 C27 H27 118.3 . . ? C28 C27 H27 118.3 . . ? C27 C28 C29 120.4(13) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C32 C29 C28 124.8(13) . . ? C32 C29 C30 121.7(11) . . ? C28 C29 C30 113.5(14) . . ? C31 C30 C29 123.0(13) . . ? C31 C30 H30 118.5 . . ? C29 C30 H30 118.5 . . ? N9 C31 C30 121.0(14) . . ? N9 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C29 C32 C33 122.5(11) . . ? C29 C32 C36 122.2(13) . . ? C33 C32 C36 115.2(14) . . ? C34 C33 C32 121.8(12) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? N11 C34 C33 119.9(13) . . ? N11 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C36 C35 N11 121.8(12) . . ? C36 C35 H35 119.1 . . ? N11 C35 H35 119.1 . . ? C35 C36 C32 121.4(13) . . ? C35 C36 H36 119.3 . . ? C32 C36 H36 119.3 . . ? N10 C37 C38 120.1(12) . . ? N10 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C39 C38 C37 121.1(12) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C40 C39 C38 116.6(13) . . ? C40 C39 C42 120.9(12) . . ? C38 C39 C42 122.5(12) . . ? C39 C40 C41 120.4(12) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? N10 C41 C40 122.7(13) . . ? N10 C41 H41 118.7 . . ? C40 C41 H41 118.7 . . ? C43 C42 C46 113.4(13) . . ? C43 C42 C39 122.4(11) . . ? C46 C42 C39 123.8(12) . . ? C44 C43 C42 121.8(11) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C43 C44 N12 120.3(13) . . ? C43 C44 H44 119.9 . . ? N12 C44 H44 119.9 . . ? C46 C45 N12 119.5(13) . . ? C46 C45 H45 120.3 . . ? N12 C45 H45 120.3 . . ? C45 C46 C42 124.7(14) . . ? C45 C46 H46 117.6 . . ? C42 C46 H46 117.6 . . ? N12 C47 N11 108.2(11) . 2_766 ? N12 C47 H47A 110.1 . . ? N11 C47 H47A 110.1 2_766 . ? N12 C47 H47B 110.1 . . ? N11 C47 H47B 110.1 2_766 . ? H47A C47 H47B 108.4 . . ? C48 O1 C58 116.1(9) . . ? C60 O2 C59 118.5(9) . . ? C61 O3 C62 115.3(8) . . ? C63 O4 C64 113.5(9) . . ? C66 O5 C65 113.3(10) . . ? C68 O6 C67 108.9(9) . . ? C70 O7 C69 117.2(8) . . ? C75 O8 C80 117.6(9) . . ? C81 O9 C82 114.2(10) . . ? C83 O10 C84 106.8(10) . . ? C86 O11 C85 105.7(12) . . ? C87 O12 C88 112.6(9) . . ? C89 O13 C90 113.3(8) . . ? C53 O14 C91 115.0(8) . . ? O1 C48 C49 124.3(9) . . ? O1 C48 C57 115.0(9) . . ? C49 C48 C57 120.7(9) . . ? C48 C49 C50 120.3(10) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C51 C50 C49 120.0(11) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C52 120.3(10) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C57 C52 C51 120.2(8) . . ? C57 C52 C53 118.3(9) . . ? C51 C52 C53 121.5(9) . . ? O14 C53 C54 126.6(9) . . ? O14 C53 C52 113.5(9) . . ? C54 C53 C52 119.8(9) . . ? C53 C54 C55 121.5(10) . . ? C53 C54 H54 119.2 . . ? C55 C54 H54 119.2 . . ? C56 C55 C54 119.6(11) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C55 C56 C57 119.7(10) . . ? C55 C56 H56 120.1 . . ? C57 C56 H56 120.1 . . ? C52 C57 C56 121.0(9) . . ? C52 C57 C48 118.5(9) . . ? C56 C57 C48 120.5(9) . . ? O1 C58 C59 107.6(11) . . ? O1 C58 H58A 110.2 . . ? C59 C58 H58A 110.2 . . ? O1 C58 H58B 110.2 . . ? C59 C58 H58B 110.2 . . ? H58A C58 H58B 108.5 . . ? O2 C59 C58 114.4(10) . . ? O2 C59 H59A 108.7 . . ? C58 C59 H59A 108.7 . . ? O2 C59 H59B 108.7 . . ? C58 C59 H59B 108.7 . . ? H59A C59 H59B 107.6 . . ? O2 C60 C61 111.0(10) . . ? O2 C60 H60A 109.4 . . ? C61 C60 H60A 109.4 . . ? O2 C60 H60B 109.4 . . ? C61 C60 H60B 109.4 . . ? H60A C60 H60B 108.0 . . ? O3 C61 C60 110.8(9) . . ? O3 C61 H61A 109.5 . . ? C60 C61 H61A 109.5 . . ? O3 C61 H61B 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 108.1 . . ? C63 C62 O3 112.6(10) . . ? C63 C62 H62A 109.1 . . ? O3 C62 H62A 109.1 . . ? C63 C62 H62B 109.1 . . ? O3 C62 H62B 109.1 . . ? H62A C62 H62B 107.8 . . ? O4 C63 C62 109.0(10) . . ? O4 C63 H63 125.5 . . ? C62 C63 H63 125.5 . . ? O4 C64 C65 111.0(11) . . ? O4 C64 H64A 109.4 . . ? C65 C64 H64A 109.4 . . ? O4 C64 H64B 109.4 . . ? C65 C64 H64B 109.4 . . ? H64A C64 H64B 108.0 . . ? O5 C65 C64 108.7(11) . . ? O5 C65 H65A 110.0 . . ? C64 C65 H65A 110.0 . . ? O5 C65 H65B 110.0 . . ? C64 C65 H65B 110.0 . . ? H65A C65 H65B 108.3 . . ? O5 C66 C67 114.2(11) . . ? O5 C66 H66A 108.7 . . ? C67 C66 H66A 108.7 . . ? O5 C66 H66B 108.7 . . ? C67 C66 H66B 108.7 . . ? H66A C66 H66B 107.6 . . ? O6 C67 C66 108.4(11) . . ? O6 C67 H67A 110.0 . . ? C66 C67 H67A 110.0 . . ? O6 C67 H67B 110.0 . . ? C66 C67 H67B 110.0 . . ? H67A C67 H67B 108.4 . . ? O6 C68 C69 110.7(9) . . ? O6 C68 H68A 109.5 . . ? C69 C68 H68A 109.5 . . ? O6 C68 H68B 109.5 . . ? C69 C68 H68B 109.5 . . ? H68A C68 H68B 108.1 . . ? O7 C69 C68 109.2(9) . . ? O7 C69 H69A 109.8 . . ? C68 C69 H69A 109.8 . . ? O7 C69 H69B 109.8 . . ? C68 C69 H69B 109.8 . . ? H69A C69 H69B 108.3 . . ? O7 C70 C71 127.1(9) . . ? O7 C70 C79 115.3(8) . . ? C71 C70 C79 117.6(9) . . ? C72 C71 C70 122.4(10) . . ? C72 C71 H71 118.8 . . ? C70 C71 H71 118.8 . . ? C71 C72 C73 119.3(10) . . ? C71 C72 H72 120.4 . . ? C73 C72 H72 120.4 . . ? C74 C73 C72 120.2(10) . . ? C74 C73 H73 119.9 . . ? C72 C73 H73 119.9 . . ? C73 C74 C79 122.3(10) . . ? C73 C74 C75 119.7(10) . . ? C79 C74 C75 117.9(9) . . ? O8 C75 C76 128.1(10) . . ? O8 C75 C74 113.6(9) . . ? C76 C75 C74 118.3(10) . . ? C75 C76 C77 122.7(10) . . ? C75 C76 H76 118.7 . . ? C77 C76 H76 118.7 . . ? C76 C77 C78 120.1(10) . . ? C76 C77 H77 120.0 . . ? C78 C77 H77 120.0 . . ? C77 C78 C79 118.9(10) . . ? C77 C78 H78 120.6 . . ? C79 C78 H78 120.6 . . ? C74 C79 C78 122.1(9) . . ? C74 C79 C70 118.2(9) . . ? C78 C79 C70 119.7(9) . . ? C81 C80 O8 105.1(10) . . ? C81 C80 H80A 110.7 . . ? O8 C80 H80A 110.7 . . ? C81 C80 H80B 110.7 . . ? O8 C80 H80B 110.7 . . ? H80A C80 H80B 108.8 . . ? O9 C81 C80 114.7(10) . . ? O9 C81 H81A 108.6 . . ? C80 C81 H81A 108.6 . . ? O9 C81 H81B 108.6 . . ? C80 C81 H81B 108.6 . . ? H81A C81 H81B 107.6 . . ? O9 C82 C83 111.9(10) . . ? O9 C82 H82A 109.2 . . ? C83 C82 H82A 109.2 . . ? O9 C82 H82B 109.2 . . ? C83 C82 H82B 109.2 . . ? H82A C82 H82B 107.9 . . ? O10 C83 C82 108.7(11) . . ? O10 C83 H83A 109.9 . . ? C82 C83 H83A 109.9 . . ? O10 C83 H83B 109.9 . . ? C82 C83 H83B 109.9 . . ? H83A C83 H83B 108.3 . . ? O10 C84 C85 108.9(12) . . ? O10 C84 H84A 109.9 . . ? C85 C84 H84A 109.9 . . ? O10 C84 H84B 109.9 . . ? C85 C84 H84B 109.9 . . ? H84A C84 H84B 108.3 . . ? C84 C85 O11 109.6(13) . . ? C84 C85 H85A 109.8 . . ? O11 C85 H85A 109.8 . . ? C84 C85 H85B 109.8 . . ? O11 C85 H85B 109.8 . . ? H85A C85 H85B 108.2 . . ? O11 C86 C87 106.5(12) . . ? O11 C86 H86A 110.4 . . ? C87 C86 H86A 110.4 . . ? O11 C86 H86B 110.4 . . ? C87 C86 H86B 110.4 . . ? H86A C86 H86B 108.6 . . ? O12 C87 C86 108.2(12) . . ? O12 C87 H87A 110.1 . . ? C86 C87 H87A 110.1 . . ? O12 C87 H87B 110.1 . . ? C86 C87 H87B 110.1 . . ? H87A C87 H87B 108.4 . . ? O12 C88 C89 113.6(10) . . ? O12 C88 H88A 108.9 . . ? C89 C88 H88A 108.9 . . ? O12 C88 H88B 108.9 . . ? C89 C88 H88B 108.9 . . ? H88A C88 H88B 107.7 . . ? O13 C89 C88 110.3(9) . . ? O13 C89 H89A 109.6 . . ? C88 C89 H89A 109.6 . . ? O13 C89 H89B 109.6 . . ? C88 C89 H89B 109.6 . . ? H89A C89 H89B 108.1 . . ? O13 C90 C91 113.2(9) . . ? O13 C90 H90A 108.9 . . ? C91 C90 H90A 108.9 . . ? O13 C90 H90B 108.9 . . ? C91 C90 H90B 108.9 . . ? H90A C90 H90B 107.7 . . ? C90 C91 O14 109.9(10) . . ? C90 C91 H91A 109.7 . . ? O14 C91 H91A 109.7 . . ? C90 C91 H91B 109.7 . . ? O14 C91 H91B 109.7 . . ? H91A C91 H91B 108.2 . . ? C92 O15 C102 120.8(10) . . ? C104 O16 C103 112.7(11) . . ? C105 O17 C106 116.1(16) . . ? C107 O18 C108 115(2) . . ? C110 O19 C109 110(3) . . ? C112 O20 C111 111.5(19) . . ? C114 O21 C113 123(2) . . ? C119 O22 C124 131.8(19) . . ? C125 O23 C126 122(2) . . ? C127 O24 C128 104(3) . . ? C129 O25 C130 104.1(18) . . ? C131 O26 C132 112.3(15) . . ? C134 O27 C133 112.5(10) . . ? C97 O28 C135 116.5(8) . . ? O15 C92 C93 124.7(10) . . ? O15 C92 C101 115.8(9) . . ? C93 C92 C101 119.4(11) . . ? C92 C93 C94 122.8(11) . . ? C92 C93 H93 118.6 . . ? C94 C93 H93 118.6 . . ? C95 C94 C93 118.2(11) . . ? C95 C94 H94 120.9 . . ? C93 C94 H94 120.9 . . ? C94 C95 C96 120.5(11) . . ? C94 C95 H95 119.8 . . ? C96 C95 H95 119.8 . . ? C101 C96 C95 120.1(9) . . ? C101 C96 C97 118.8(9) . . ? C95 C96 C97 121.1(10) . . ? O28 C97 C98 125.7(9) . . ? O28 C97 C96 114.9(9) . . ? C98 C97 C96 119.4(10) . . ? C97 C98 C99 120.8(10) . . ? C97 C98 H98 119.6 . . ? C99 C98 H98 119.6 . . ? C100 C99 C98 122.0(10) . . ? C100 C99 H99 119.0 . . ? C98 C99 H99 119.0 . . ? C99 C100 C101 118.4(11) . . ? C99 C100 H100 120.8 . . ? C101 C100 H100 120.8 . . ? C96 C101 C100 120.5(9) . . ? C96 C101 C92 118.9(9) . . ? C100 C101 C92 120.6(10) . . ? O15 C102 C103 108.0(11) . . ? O15 C102 H10A 110.1 . . ? C103 C102 H10A 110.1 . . ? O15 C102 H10B 110.1 . . ? C103 C102 H10B 110.1 . . ? H10A C102 H10B 108.4 . . ? O16 C103 C102 111.3(13) . . ? O16 C103 H10C 109.4 . . ? C102 C103 H10C 109.4 . . ? O16 C103 H10D 109.4 . . ? C102 C103 H10D 109.4 . . ? H10C C103 H10D 108.0 . . ? O16 C104 C105 106.6(14) . . ? O16 C104 H10E 110.4 . . ? C105 C104 H10E 110.4 . . ? O16 C104 H10F 110.4 . . ? C105 C104 H10F 110.4 . . ? H10E C104 H10F 108.6 . . ? O17 C105 C104 110.7(16) . . ? O17 C105 H10G 109.5 . . ? C104 C105 H10G 109.5 . . ? O17 C105 H10H 109.5 . . ? C104 C105 H10H 109.5 . . ? H10G C105 H10H 108.1 . . ? C107 C106 O17 112.5(19) . . ? C107 C106 H106 123.8 . . ? O17 C106 H106 123.8 . . ? O18 C107 C106 109(2) . . ? O18 C107 H107 125.6 . . ? C106 C107 H107 125.6 . . ? O18 C108 C109 116(3) . . ? O18 C108 H10I 108.3 . . ? C109 C108 H10I 108.3 . . ? O18 C108 H10J 108.3 . . ? C109 C108 H10J 108.3 . . ? H10I C108 H10J 107.4 . . ? O19 C109 C108 107(2) . . ? O19 C109 H10K 110.2 . . ? C108 C109 H10K 110.2 . . ? O19 C109 H10L 110.2 . . ? C108 C109 H10L 110.2 . . ? H10K C109 H10L 108.5 . . ? O19 C110 C111 119(3) . . ? O19 C110 H11A 107.6 . . ? C111 C110 H11A 107.6 . . ? O19 C110 H11B 107.6 . . ? C111 C110 H11B 107.6 . . ? H11A C110 H11B 107.0 . . ? O20 C111 C110 107(2) . . ? O20 C111 H11C 110.2 . . ? C110 C111 H11C 110.2 . . ? O20 C111 H11D 110.2 . . ? C110 C111 H11D 110.2 . . ? H11C C111 H11D 108.5 . . ? O20 C112 C113 111.1(19) . . ? O20 C112 H11E 109.4 . . ? C113 C112 H11E 109.4 . . ? O20 C112 H11F 109.4 . . ? C113 C112 H11F 109.4 . . ? H11E C112 H11F 108.0 . . ? O21 C113 C112 111(2) . . ? O21 C113 H11G 109.4 . . ? C112 C113 H11G 109.4 . . ? O21 C113 H11H 109.4 . . ? C112 C113 H11H 109.4 . . ? H11G C113 H11H 108.0 . . ? C115 C114 O21 132.7(19) . . ? C115 C114 C123 110.5(17) . . ? O21 C114 C123 116.8(18) . . ? C116 C115 C114 130(2) . . ? C116 C115 H115 115.0 . . ? C114 C115 H115 115.0 . . ? C115 C116 C117 115(2) . . ? C115 C116 H116 122.5 . . ? C117 C116 H116 122.5 . . ? C118 C117 C116 121(2) . . ? C118 C117 H117 119.3 . . ? C116 C117 H117 119.3 . . ? C117 C118 C123 121.0(19) . . ? C117 C118 C119 119.1(19) . . ? C123 C118 C119 119.9(18) . . ? O22 C119 C120 132(2) . . ? O22 C119 C118 114.8(19) . . ? C120 C119 C118 113.0(18) . . ? C119 C120 C121 127(2) . . ? C119 C120 H120 116.7 . . ? C121 C120 H120 116.7 . . ? C120 C121 C122 121(2) . . ? C120 C121 H121 119.3 . . ? C122 C121 H121 119.3 . . ? C121 C122 C123 113.9(18) . . ? C121 C122 H122 123.0 . . ? C123 C122 H122 123.0 . . ? C118 C123 C122 125.0(17) . . ? C118 C123 C114 121.7(17) . . ? C122 C123 C114 113.2(17) . . ? C125 C124 O22 105.7(15) . . ? C125 C124 H12A 110.6 . . ? O22 C124 H12A 110.6 . . ? C125 C124 H12B 110.6 . . ? O22 C124 H12B 110.6 . . ? H12A C124 H12B 108.7 . . ? O23 C125 C124 129(2) . . ? O23 C125 H12C 104.9 . . ? C124 C125 H12C 104.9 . . ? O23 C125 H12D 104.9 . . ? C124 C125 H12D 104.9 . . ? H12C C125 H12D 105.8 . . ? O23 C126 C127 97.7(17) . . ? O23 C126 H12E 112.2 . . ? C127 C126 H12E 112.2 . . ? O23 C126 H12F 112.2 . . ? C127 C126 H12F 112.2 . . ? H12E C126 H12F 109.8 . . ? O24 C127 C126 104(2) . . ? O24 C127 H12G 110.9 . . ? C126 C127 H12G 110.9 . . ? O24 C127 H12H 110.9 . . ? C126 C127 H12H 110.9 . . ? H12G C127 H12H 108.9 . . ? O24 C128 C129 103(2) . . ? O24 C128 H12I 111.2 . . ? C129 C128 H12I 111.2 . . ? O24 C128 H12J 111.2 . . ? C129 C128 H12J 111.2 . . ? H12I C128 H12J 109.1 . . ? O25 C129 C128 116(2) . . ? O25 C129 H12K 108.3 . . ? C128 C129 H12K 108.3 . . ? O25 C129 H12L 108.3 . . ? C128 C129 H12L 108.3 . . ? H12K C129 H12L 107.4 . . ? O25 C130 C131 106.6(18) . . ? O25 C130 H13A 110.4 . . ? C131 C130 H13A 110.4 . . ? O25 C130 H13B 110.4 . . ? C131 C130 H13B 110.4 . . ? H13A C130 H13B 108.6 . . ? O26 C131 C130 111.2(19) . . ? O26 C131 H13C 109.4 . . ? C130 C131 H13C 109.4 . . ? O26 C131 H13D 109.4 . . ? C130 C131 H13D 109.4 . . ? H13C C131 H13D 108.0 . . ? O26 C132 C133 110.5(14) . . ? O26 C132 H13E 109.5 . . ? C133 C132 H13E 109.5 . . ? O26 C132 H13F 109.5 . . ? C133 C132 H13F 109.5 . . ? H13E C132 H13F 108.1 . . ? O27 C133 C132 111.3(13) . . ? O27 C133 H13G 109.4 . . ? C132 C133 H13G 109.4 . . ? O27 C133 H13H 109.4 . . ? C132 C133 H13H 109.4 . . ? H13G C133 H13H 108.0 . . ? O27 C134 C135 115.0(11) . . ? O27 C134 H13I 108.5 . . ? C135 C134 H13I 108.5 . . ? O27 C134 H13J 108.5 . . ? C135 C134 H13J 108.5 . . ? H13I C134 H13J 107.5 . . ? C134 C135 O28 107.8(10) . . ? C134 C135 H13K 110.1 . . ? O28 C135 H13K 110.1 . . ? C134 C135 H13L 110.1 . . ? O28 C135 H13L 110.1 . . ? H13K C135 H13L 108.5 . . ? F1 P1 F3 179.3(8) . . ? F1 P1 F4 92.4(7) . . ? F3 P1 F4 87.5(7) . . ? F1 P1 F6 84.0(8) . . ? F3 P1 F6 95.2(8) . . ? F4 P1 F6 83.3(7) . . ? F1 P1 F2 91.3(7) . . ? F3 P1 F2 89.5(8) . . ? F4 P1 F2 94.3(7) . . ? F6 P1 F2 174.6(7) . . ? F1 P1 F5 92.6(8) . . ? F3 P1 F5 87.5(7) . . ? F4 P1 F5 173.5(8) . . ? F6 P1 F5 93.1(7) . . ? F2 P1 F5 89.8(6) . . ? F11 P2 F9 91.3(9) . . ? F11 P2 F7 90.7(8) . . ? F9 P2 F7 88.3(8) . . ? F11 P2 F12 91.8(7) . . ? F9 P2 F12 91.8(9) . . ? F7 P2 F12 177.5(8) . . ? F11 P2 F10 89.1(8) . . ? F9 P2 F10 179.2(9) . . ? F7 P2 F10 92.4(8) . . ? F12 P2 F10 87.5(8) . . ? F11 P2 F8 176.3(9) . . ? F9 P2 F8 91.7(8) . . ? F7 P2 F8 87.3(7) . . ? F12 P2 F8 90.2(7) . . ? F10 P2 F8 87.8(9) . . ? F13 P3 F14 88.3(6) . . ? F13 P3 F18 89.8(6) . . ? F14 P3 F18 91.3(6) . . ? F13 P3 F16 91.0(6) . . ? F14 P3 F16 179.3(7) . . ? F18 P3 F16 88.9(5) . . ? F13 P3 F15 178.1(7) . . ? F14 P3 F15 89.9(6) . . ? F18 P3 F15 90.1(5) . . ? F16 P3 F15 90.8(5) . . ? F13 P3 F17 91.8(6) . . ? F14 P3 F17 90.7(7) . . ? F18 P3 F17 177.5(6) . . ? F16 P3 F17 89.2(6) . . ? F15 P3 F17 88.3(5) . . ? F22 P4 F21 90.5(5) . . ? F22 P4 F24 91.2(5) . . ? F21 P4 F24 88.8(6) . . ? F22 P4 F23 90.3(6) . . ? F21 P4 F23 178.8(6) . . ? F24 P4 F23 90.4(6) . . ? F22 P4 F19 90.7(5) . . ? F21 P4 F19 90.0(5) . . ? F24 P4 F19 177.6(5) . . ? F23 P4 F19 90.9(5) . . ? F22 P4 F20 179.0(5) . . ? F21 P4 F20 89.5(4) . . ? F24 P4 F20 89.7(4) . . ? F23 P4 F20 89.6(5) . . ? F19 P4 F20 88.3(5) . . ? F28 P5 F30 98.8(12) . . ? F28 P5 F25 87.6(7) . . ? F30 P5 F25 89.5(7) . . ? F28 P5 F29 175.6(11) . . ? F30 P5 F29 84.9(10) . . ? F25 P5 F29 94.8(8) . . ? F28 P5 F27 88.6(9) . . ? F30 P5 F27 172.5(11) . . ? F25 P5 F27 89.8(7) . . ? F29 P5 F27 87.7(8) . . ? F28 P5 F26 93.0(7) . . ? F30 P5 F26 88.0(7) . . ? F25 P5 F26 177.5(7) . . ? F29 P5 F26 84.8(7) . . ? F27 P5 F26 92.6(7) . . ? F31 P6 F34 93.6(11) . . ? F31 P6 F35 87.5(7) . . ? F34 P6 F35 92.7(9) . . ? F31 P6 F36 176.7(11) . . ? F34 P6 F36 89.4(11) . . ? F35 P6 F36 93.7(10) . . ? F31 P6 F33 93.0(9) . . ? F34 P6 F33 88.4(8) . . ? F35 P6 F33 178.8(9) . . ? F36 P6 F33 85.8(9) . . ? F31 P6 F32 85.9(10) . . ? F34 P6 F32 176.7(11) . . ? F35 P6 F32 90.6(8) . . ? F36 P6 F32 91.0(9) . . ? F33 P6 F32 88.4(8) . . ? F39 P7 F40 88.0(13) . . ? F39 P7 F37 87.1(12) . . ? F40 P7 F37 153.8(18) . . ? F39 P7 F41 171.5(15) . . ? F40 P7 F41 94.3(15) . . ? F37 P7 F41 94.3(13) . . ? F39 P7 F42 101.9(14) . . ? F40 P7 F42 80.8(16) . . ? F37 P7 F42 75.1(13) . . ? F41 P7 F42 86.5(12) . . ? F39 P7 F38 88.1(13) . . ? F40 P7 F38 131.4(19) . . ? F37 P7 F38 74.1(14) . . ? F41 P7 F38 84.3(13) . . ? F42 P7 F38 147.0(17) . . ? F48 P8 F43 90.3(13) . . ? F48 P8 F46 176.8(16) . . ? F43 P8 F46 92.7(13) . . ? F48 P8 F45 90.3(13) . . ? F43 P8 F45 177.1(14) . . ? F46 P8 F45 86.8(14) . . ? F48 P8 F47 81.9(15) . . ? F43 P8 F47 94.8(11) . . ? F46 P8 F47 96.7(17) . . ? F45 P8 F47 88.1(13) . . ? F48 P8 F44 92.1(16) . . ? F43 P8 F44 91.0(13) . . ? F46 P8 F44 89.0(17) . . ? F45 P8 F44 86.2(13) . . ? F47 P8 F44 171.7(15) . . ? N13 C136 C137 179(3) . . ? C136 C137 H37D 109.5 . . ? C136 C137 H37E 109.5 . . ? H37D C137 H37E 109.5 . . ? C136 C137 H37F 109.5 . . ? H37D C137 H37F 109.5 . . ? H37E C137 H37F 109.5 . . ? N14 C138 C139 177(2) . . ? C138 C139 H39D 109.5 . . ? C138 C139 H39E 109.5 . . ? H39D C139 H39E 109.5 . . ? C138 C139 H39F 109.5 . . ? H39D C139 H39F 109.5 . . ? H39E C139 H39F 109.5 . . ? N15 C140 C141 172(2) . . ? C140 C141 H41D 109.5 . . ? C140 C141 H41E 109.5 . . ? H41D C141 H41E 109.5 . . ? C140 C141 H41F 109.5 . . ? H41D C141 H41F 109.5 . . ? H41E C141 H41F 109.5 . . ? N16 C142 C143 173.3(19) . . ? C142 C143 H43D 109.5 . . ? C142 C143 H43E 109.5 . . ? H43D C143 H43E 109.5 . . ? C142 C143 H43F 109.5 . . ? H43D C143 H43F 109.5 . . ? H43E C143 H43F 109.5 . . ? N17 C144 C145 172(3) 1_455 1_455 ? C144 C145 H45D 109.5 1_655 . ? C144 C145 H45E 109.5 1_655 . ? H45D C145 H45E 109.5 . . ? C144 C145 H45F 109.5 1_655 . ? H45D C145 H45F 109.5 . . ? H45E C145 H45F 109.5 . . ? N18 C146 C147 169(6) 1_656 . ? C146 C147 H47D 109.5 . . ? C146 C147 H47E 109.5 . . ? H47D C147 H47E 109.5 . . ? C146 C147 H47F 109.5 . . ? H47D C147 H47F 109.5 . . ? H47E C147 H47F 109.5 . . ? C149 C148 N19 159(5) . . ? C148 C149 H49D 109.5 . . ? C148 C149 H49E 109.5 . . ? H49D C149 H49E 109.5 . . ? C148 C149 H49F 109.5 . . ? H49D C149 H49F 109.5 . . ? H49E C149 H49F 109.5 . . ? N20 C150 C151 176(3) . . ? C150 C151 H51D 109.5 . . ? C150 C151 H51E 109.5 . . ? H51D C151 H51E 109.5 . . ? C150 C151 H51F 109.5 . . ? H51D C151 H51F 109.5 . . ? H51E C151 H51F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Pd1 N1 C1 -68(3) . . . . ? N2 Pd1 N1 C1 -16.4(8) . . . . ? N3 Pd1 N1 C1 162.3(8) . . . . ? N1 Pd1 N2 C2 -8.0(8) . . . . ? N4 Pd1 N2 C2 166.9(8) . . . . ? N3 Pd1 N2 C2 -39(7) . . . . ? N1 Pd1 N3 C7 87.7(7) . . . . ? N4 Pd1 N3 C7 -87.3(7) . . . . ? N2 Pd1 N3 C7 119(7) . . . . ? N1 Pd1 N3 C3 -93.2(7) . . . . ? N4 Pd1 N3 C3 91.8(7) . . . . ? N2 Pd1 N3 C3 -62(7) . . . . ? N1 Pd1 N4 C13 129(3) . . . . ? N2 Pd1 N4 C13 77.8(8) . . . . ? N3 Pd1 N4 C13 -101.1(8) . . . . ? N1 Pd1 N4 C17 -53(3) . . . . ? N2 Pd1 N4 C17 -104.4(9) . . . . ? N3 Pd1 N4 C17 76.8(8) . . . . ? Pd1 N1 C1 C2 37.1(13) . . . . ? Pd1 N2 C2 C1 30.8(13) . . . . ? N1 C1 C2 N2 -45.3(15) . . . . ? C7 N3 C3 C4 1.6(14) . . . . ? Pd1 N3 C3 C4 -177.5(7) . . . . ? N3 C3 C4 C5 0.0(15) . . . . ? C3 C4 C5 C6 -1.5(14) . . . . ? C3 C4 C5 C8 177.5(9) . . . . ? C4 C5 C6 C7 1.5(14) . . . . ? C8 C5 C6 C7 -177.5(9) . . . . ? C3 N3 C7 C6 -1.6(14) . . . . ? Pd1 N3 C7 C6 177.5(8) . . . . ? C5 C6 C7 N3 0.0(15) . . . . ? C6 C5 C8 C12 -18.9(13) . . . . ? C4 C5 C8 C12 162.2(9) . . . . ? C6 C5 C8 C9 160.8(9) . . . . ? C4 C5 C8 C9 -18.2(13) . . . . ? C12 C8 C9 C10 -0.1(12) . . . . ? C5 C8 C9 C10 -179.8(8) . . . . ? C8 C9 C10 N5 -1.1(13) . . . . ? C11 N5 C10 C9 1.4(12) . . . . ? C24 N5 C10 C9 -179.5(8) 2_765 . . . ? C10 N5 C11 C12 -0.4(12) . . . . ? C24 N5 C11 C12 -179.5(8) 2_765 . . . ? N5 C11 C12 C8 -0.8(13) . . . . ? C9 C8 C12 C11 1.1(12) . . . . ? C5 C8 C12 C11 -179.3(8) . . . . ? C17 N4 C13 C14 -0.3(16) . . . . ? Pd1 N4 C13 C14 177.6(8) . . . . ? N4 C13 C14 C15 0.6(17) . . . . ? C13 C14 C15 C16 1.2(16) . . . . ? C13 C14 C15 C18 -175.1(10) . . . . ? C14 C15 C16 C17 -3.2(17) . . . . ? C18 C15 C16 C17 173.2(11) . . . . ? C13 N4 C17 C16 -1.9(18) . . . . ? Pd1 N4 C17 C16 -180.0(11) . . . . ? C15 C16 C17 N4 4(2) . . . . ? C14 C15 C18 C19 -163.8(10) . . . . ? C16 C15 C18 C19 20.1(14) . . . . ? C14 C15 C18 C23 18.8(15) . . . . ? C16 C15 C18 C23 -157.3(10) . . . . ? C23 C18 C19 C20 2.3(14) . . . . ? C15 C18 C19 C20 -175.3(9) . . . . ? C22 N6 C20 C19 -4.1(14) . . . . ? C24 N6 C20 C19 176.3(9) . . . . ? C18 C19 C20 N6 0.8(15) . . . . ? C20 N6 C22 C23 4.2(14) . . . . ? C24 N6 C22 C23 -176.2(9) . . . . ? N6 C22 C23 C18 -0.9(15) . . . . ? C19 C18 C23 C22 -2.2(14) . . . . ? C15 C18 C23 C22 175.3(9) . . . . ? C20 N6 C24 N5 -97.4(10) . . . 2_765 ? C22 N6 C24 N5 83.0(11) . . . 2_765 ? N9 Pd2 N7 C25 164.7(15) . . . . ? N10 Pd2 N7 C25 -89(3) . . . . ? N8 Pd2 N7 C25 -14.8(16) . . . . ? N7 Pd2 N8 C26 -13.4(14) . . . . ? N9 Pd2 N8 C26 -23(13) . . . . ? N10 Pd2 N8 C26 157.9(13) . . . . ? N7 Pd2 N9 C27 -95.3(13) . . . . ? N10 Pd2 N9 C27 93.3(12) . . . . ? N8 Pd2 N9 C27 -86(12) . . . . ? N7 Pd2 N9 C31 84.3(12) . . . . ? N10 Pd2 N9 C31 -87.1(11) . . . . ? N8 Pd2 N9 C31 94(12) . . . . ? N7 Pd2 N10 C41 -6(4) . . . . ? N9 Pd2 N10 C41 100.6(11) . . . . ? N8 Pd2 N10 C41 -79.4(11) . . . . ? N7 Pd2 N10 C37 176(3) . . . . ? N9 Pd2 N10 C37 -77.8(11) . . . . ? N8 Pd2 N10 C37 102.1(12) . . . . ? Pd2 N7 C25 C26 41(2) . . . . ? N7 C25 C26 N8 -55(2) . . . . ? Pd2 N8 C26 C25 43(2) . . . . ? C31 N9 C27 C28 1(2) . . . . ? Pd2 N9 C27 C28 -179.4(10) . . . . ? N9 C27 C28 C29 0(2) . . . . ? C27 C28 C29 C32 -179.4(13) . . . . ? C27 C28 C29 C30 -0.4(19) . . . . ? C32 C29 C30 C31 177.9(14) . . . . ? C28 C29 C30 C31 -1(2) . . . . ? C27 N9 C31 C30 -3(2) . . . . ? Pd2 N9 C31 C30 177.8(12) . . . . ? C29 C30 C31 N9 3(2) . . . . ? C28 C29 C32 C33 -25(2) . . . . ? C30 C29 C32 C33 156.1(13) . . . . ? C28 C29 C32 C36 159.1(13) . . . . ? C30 C29 C32 C36 -20(2) . . . . ? C29 C32 C33 C34 -178.6(13) . . . . ? C36 C32 C33 C34 -2.4(19) . . . . ? C35 N11 C34 C33 -0.6(19) . . . . ? C47 N11 C34 C33 178.7(12) 2_766 . . . ? C32 C33 C34 N11 3(2) . . . . ? C34 N11 C35 C36 -2(2) . . . . ? C47 N11 C35 C36 179.2(12) 2_766 . . . ? N11 C35 C36 C32 2(2) . . . . ? C29 C32 C36 C35 176.5(13) . . . . ? C33 C32 C36 C35 0(2) . . . . ? C41 N10 C37 C38 -3(2) . . . . ? Pd2 N10 C37 C38 175.7(10) . . . . ? N10 C37 C38 C39 -2(2) . . . . ? C37 C38 C39 C40 2.8(19) . . . . ? C37 C38 C39 C42 -173.9(12) . . . . ? C38 C39 C40 C41 0(2) . . . . ? C42 C39 C40 C41 177.2(12) . . . . ? C37 N10 C41 C40 6(2) . . . . ? Pd2 N10 C41 C40 -172.5(11) . . . . ? C39 C40 C41 N10 -5(2) . . . . ? C40 C39 C42 C43 -166.2(12) . . . . ? C38 C39 C42 C43 10.5(18) . . . . ? C40 C39 C42 C46 6.9(19) . . . . ? C38 C39 C42 C46 -176.4(13) . . . . ? C46 C42 C43 C44 1.3(18) . . . . ? C39 C42 C43 C44 175.0(12) . . . . ? C42 C43 C44 N12 -3(2) . . . . ? C45 N12 C44 C43 4(2) . . . . ? C47 N12 C44 C43 -177.0(13) . . . . ? C44 N12 C45 C46 -4(2) . . . . ? C47 N12 C45 C46 177.0(15) . . . . ? N12 C45 C46 C42 3(2) . . . . ? C43 C42 C46 C45 -1(2) . . . . ? C39 C42 C46 C45 -175.0(14) . . . . ? C45 N12 C47 N11 -102.9(15) . . . 2_766 ? C44 N12 C47 N11 77.8(15) . . . 2_766 ? C58 O1 C48 C49 -4.2(14) . . . . ? C58 O1 C48 C57 176.4(9) . . . . ? O1 C48 C49 C50 -179.2(9) . . . . ? C57 C48 C49 C50 0.2(16) . . . . ? C48 C49 C50 C51 1.3(17) . . . . ? C49 C50 C51 C52 -1.9(16) . . . . ? C50 C51 C52 C57 1.1(14) . . . . ? C50 C51 C52 C53 179.6(10) . . . . ? C91 O14 C53 C54 4.9(15) . . . . ? C91 O14 C53 C52 -174.0(9) . . . . ? C57 C52 C53 O14 178.1(8) . . . . ? C51 C52 C53 O14 -0.4(13) . . . . ? C57 C52 C53 C54 -0.9(14) . . . . ? C51 C52 C53 C54 -179.4(10) . . . . ? O14 C53 C54 C55 179.3(10) . . . . ? C52 C53 C54 C55 -1.8(16) . . . . ? C53 C54 C55 C56 3.1(16) . . . . ? C54 C55 C56 C57 -1.6(15) . . . . ? C51 C52 C57 C56 -179.2(9) . . . . ? C53 C52 C57 C56 2.3(13) . . . . ? C51 C52 C57 C48 0.4(13) . . . . ? C53 C52 C57 C48 -178.1(8) . . . . ? C55 C56 C57 C52 -1.1(14) . . . . ? C55 C56 C57 C48 179.4(9) . . . . ? O1 C48 C57 C52 178.4(8) . . . . ? C49 C48 C57 C52 -1.0(14) . . . . ? O1 C48 C57 C56 -2.0(13) . . . . ? C49 C48 C57 C56 178.5(10) . . . . ? C48 O1 C58 C59 179.2(9) . . . . ? C60 O2 C59 C58 -84.2(14) . . . . ? O1 C58 C59 O2 -67.8(14) . . . . ? C59 O2 C60 C61 -146.4(11) . . . . ? C62 O3 C61 C60 -177.2(11) . . . . ? O2 C60 C61 O3 -64.2(15) . . . . ? C61 O3 C62 C63 -86.5(13) . . . . ? C64 O4 C63 C62 -176.5(11) . . . . ? O3 C62 C63 O4 -68.1(14) . . . . ? C63 O4 C64 C65 145.1(11) . . . . ? C66 O5 C65 C64 178.3(10) . . . . ? O4 C64 C65 O5 65.0(14) . . . . ? C65 O5 C66 C67 71.8(14) . . . . ? C68 O6 C67 C66 179.8(11) . . . . ? O5 C66 C67 O6 69.6(15) . . . . ? C67 O6 C68 C69 -176.9(10) . . . . ? C70 O7 C69 C68 -179.1(9) . . . . ? O6 C68 C69 O7 -67.5(12) . . . . ? C69 O7 C70 C71 -2.9(15) . . . . ? C69 O7 C70 C79 178.5(8) . . . . ? O7 C70 C71 C72 -175.9(10) . . . . ? C79 C70 C71 C72 2.7(16) . . . . ? C70 C71 C72 C73 -1.3(17) . . . . ? C71 C72 C73 C74 -1.6(17) . . . . ? C72 C73 C74 C79 3.1(16) . . . . ? C72 C73 C74 C75 178.3(10) . . . . ? C80 O8 C75 C76 3.0(16) . . . . ? C80 O8 C75 C74 -177.0(9) . . . . ? C73 C74 C75 O8 4.9(14) . . . . ? C79 C74 C75 O8 -179.6(9) . . . . ? C73 C74 C75 C76 -175.2(10) . . . . ? C79 C74 C75 C76 0.3(14) . . . . ? O8 C75 C76 C77 177.7(10) . . . . ? C74 C75 C76 C77 -2.2(16) . . . . ? C75 C76 C77 C78 1.7(17) . . . . ? C76 C77 C78 C79 0.8(15) . . . . ? C73 C74 C79 C78 177.5(9) . . . . ? C75 C74 C79 C78 2.2(14) . . . . ? C73 C74 C79 C70 -1.6(14) . . . . ? C75 C74 C79 C70 -177.0(8) . . . . ? C77 C78 C79 C74 -2.8(14) . . . . ? C77 C78 C79 C70 176.3(9) . . . . ? O7 C70 C79 C74 177.5(8) . . . . ? C71 C70 C79 C74 -1.2(14) . . . . ? O7 C70 C79 C78 -1.7(13) . . . . ? C71 C70 C79 C78 179.6(9) . . . . ? C75 O8 C80 C81 -175.1(9) . . . . ? C82 O9 C81 C80 149.4(11) . . . . ? O8 C80 C81 O9 -61.9(14) . . . . ? C81 O9 C82 C83 -77.1(13) . . . . ? C84 O10 C83 C82 -176.6(11) . . . . ? O9 C82 C83 O10 -77.8(13) . . . . ? C83 O10 C84 C85 -175.0(12) . . . . ? O10 C84 C85 O11 -79.2(15) . . . . ? C86 O11 C85 C84 -172.6(13) . . . . ? C85 O11 C86 C87 -161.0(13) . . . . ? C88 O12 C87 C86 161.2(11) . . . . ? O11 C86 C87 O12 60.4(17) . . . . ? C87 O12 C88 C89 -82.3(13) . . . . ? C90 O13 C89 C88 -170.4(10) . . . . ? O12 C88 C89 O13 -60.9(13) . . . . ? C89 O13 C90 C91 -146.3(11) . . . . ? O13 C90 C91 O14 -66.2(14) . . . . ? C53 O14 C91 C90 179.1(9) . . . . ? C102 O15 C92 C93 -1(2) . . . . ? C102 O15 C92 C101 175.6(12) . . . . ? O15 C92 C93 C94 178.2(13) . . . . ? C101 C92 C93 C94 2(2) . . . . ? C92 C93 C94 C95 0(2) . . . . ? C93 C94 C95 C96 -1.7(19) . . . . ? C94 C95 C96 C101 2.4(19) . . . . ? C94 C95 C96 C97 -176.5(12) . . . . ? C135 O28 C97 C98 6.8(19) . . . . ? C135 O28 C97 C96 -173.7(10) . . . . ? C101 C96 C97 O28 -177.2(11) . . . . ? C95 C96 C97 O28 1.7(17) . . . . ? C101 C96 C97 C98 2.4(18) . . . . ? C95 C96 C97 C98 -178.7(12) . . . . ? O28 C97 C98 C99 178.6(12) . . . . ? C96 C97 C98 C99 -1(2) . . . . ? C97 C98 C99 C100 0(2) . . . . ? C98 C99 C100 C101 -1(2) . . . . ? C95 C96 C101 C100 178.0(12) . . . . ? C97 C96 C101 C100 -3.1(19) . . . . ? C95 C96 C101 C92 -1.1(18) . . . . ? C97 C96 C101 C92 177.8(11) . . . . ? C99 C100 C101 C96 2(2) . . . . ? C99 C100 C101 C92 -178.6(13) . . . . ? O15 C92 C101 C96 -177.7(11) . . . . ? C93 C92 C101 C96 -0.8(19) . . . . ? O15 C92 C101 C100 3.1(18) . . . . ? C93 C92 C101 C100 -180.0(13) . . . . ? C92 O15 C102 C103 177.6(12) . . . . ? C104 O16 C103 C102 98.5(16) . . . . ? O15 C102 C103 O16 76.7(16) . . . . ? C103 O16 C104 C105 168.6(15) . . . . ? C106 O17 C105 C104 78(2) . . . . ? O16 C104 C105 O17 76(2) . . . . ? C105 O17 C106 C107 -177(2) . . . . ? C108 O18 C107 C106 -162(3) . . . . ? O17 C106 C107 O18 -55(3) . . . . ? C107 O18 C108 C109 -119(4) . . . . ? C110 O19 C109 C108 -160(3) . . . . ? O18 C108 C109 O19 -49(5) . . . . ? C109 O19 C110 C111 -107(4) . . . . ? C112 O20 C111 C110 81(3) . . . . ? O19 C110 C111 O20 73(4) . . . . ? C111 O20 C112 C113 -177(2) . . . . ? C114 O21 C113 C112 173(2) . . . . ? O20 C112 C113 O21 61(3) . . . . ? C113 O21 C114 C115 0(5) . . . . ? C113 O21 C114 C123 178.1(18) . . . . ? O21 C114 C115 C116 -175(3) . . . . ? C123 C114 C115 C116 7(5) . . . . ? C114 C115 C116 C117 -8(5) . . . . ? C115 C116 C117 C118 6(5) . . . . ? C116 C117 C118 C123 -4(8) . . . . ? C116 C117 C118 C119 178(3) . . . . ? C124 O22 C119 C120 -2(5) . . . . ? C124 O22 C119 C118 179(3) . . . . ? C117 C118 C119 O22 2(7) . . . . ? C123 C118 C119 O22 -176(4) . . . . ? C117 C118 C119 C120 -178(5) . . . . ? C123 C118 C119 C120 5(7) . . . . ? O22 C119 C120 C121 176(3) . . . . ? C118 C119 C120 C121 -4(5) . . . . ? C119 C120 C121 C122 2(5) . . . . ? C120 C121 C122 C123 1(4) . . . . ? C117 C118 C123 C122 180(4) . . . . ? C119 C118 C123 C122 -3(8) . . . . ? C117 C118 C123 C114 3(8) . . . . ? C119 C118 C123 C114 -180(3) . . . . ? C121 C122 C123 C118 0(5) . . . . ? C121 C122 C123 C114 177(2) . . . . ? C115 C114 C123 C118 -4(5) . . . . ? O21 C114 C123 C118 178(4) . . . . ? C115 C114 C123 C122 179(2) . . . . ? O21 C114 C123 C122 1(3) . . . . ? C119 O22 C124 C125 -132(3) . . . . ? C126 O23 C125 C124 171(2) . . . . ? O22 C124 C125 O23 -127(3) . . . . ? C125 O23 C126 C127 -60(3) . . . . ? C128 O24 C127 C126 103(3) . . . . ? O23 C126 C127 O24 -162(3) . . . . ? C127 O24 C128 C129 101(3) . . . . ? C130 O25 C129 C128 -161(3) . . . . ? O24 C128 C129 O25 -63(4) . . . . ? C129 O25 C130 C131 -178(2) . . . . ? C132 O26 C131 C130 88(2) . . . . ? O25 C130 C131 O26 70(3) . . . . ? C131 O26 C132 C133 172.7(18) . . . . ? C134 O27 C133 C132 151.2(15) . . . . ? O26 C132 C133 O27 58(2) . . . . ? C133 O27 C134 C135 82.7(15) . . . . ? O27 C134 C135 O28 67.2(14) . . . . ? C97 O28 C135 C134 -179.9(11) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 54.59 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.445 _refine_diff_density_min -1.003 _refine_diff_density_rms 0.147 # Attachment '- DN50C14-2 ringinring.cif' data_n0049 _database_code_depnum_ccdc_archive 'CCDC 772269' #TrackingRef '- DN50C14-2 ringinring.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C117 H162.50 F48 N18.50 O15.50 P8 Pd2' _chemical_formula_weight 3448.72 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' F F 0.0171 0.0103 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.2493(3) _cell_length_b 17.8612(3) _cell_length_c 23.4887(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.9360(10) _cell_angle_gamma 90.00 _cell_volume 7646.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9839 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.28 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.673 _exptl_crystal_size_mid 0.401 _exptl_crystal_size_min 0.224 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3524 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8505 _exptl_absorpt_correction_T_max 0.9393 _exptl_absorpt_process_details face-indexed _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 139290 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 30.46 _reflns_number_total 23188 _reflns_number_gt 13668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V2.1-4 (Bruker, 2007)' _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Group anisotropic displacement parameters were refined for the disordered Flourines. Similar restraints were refined for the disordered flourines. Bond restraints were imposed on the disordered C48b. ; _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^)+(0.1861P)^2^+3.3797P] 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 23188 _refine_ls_number_parameters 1124 _refine_ls_number_restraints 212 _refine_ls_R_factor_all 0.1270 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.2840 _refine_ls_wR_factor_gt 0.2422 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.229 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.33701(2) 0.51212(2) 0.154368(15) 0.03506(14) Uani 1 1 d . . . P1 P 0.68101(11) 0.52494(9) 0.12744(7) 0.0535(4) Uani 1 1 d D . . P2 P 0.34738(11) 0.25827(9) 0.13180(8) 0.0575(4) Uani 1 1 d . . . P3 P 0.0000 0.5000 0.5000 0.0779(10) Uani 1 2 d S . . O1 O 0.4379(2) 0.3534(2) 0.37532(17) 0.0479(9) Uani 1 1 d . E . O2 O 0.5265(3) 0.2512(3) 0.3102(2) 0.0660(13) Uani 1 1 d . . . O3 O 0.6575(3) 0.2859(2) 0.2558(2) 0.0703(14) Uani 1 1 d . . . O4A O 0.8147(5) 0.3055(3) 0.2858(3) 0.0274(15) Uani 0.50 1 d P A 11 O4B O 0.8194(9) 0.3446(13) 0.2935(9) 0.193(13) Uani 0.50 1 d PD B 12 O5 O 0.3914(2) 0.6135(2) 0.52828(19) 0.0484(9) Uani 1 1 d . . . O6 O 0.2765(2) 0.7108(2) 0.56126(17) 0.0517(10) Uani 1 1 d . . . O7 O 0.1380(2) 0.6705(3) 0.59732(19) 0.0571(11) Uani 1 1 d . . . O8 O 0.1589(4) 0.2985(4) 0.5825(3) 0.075(2) Uani 0.75 1 d P C 8 F1 F 0.6936(3) 0.4839(3) 0.18647(18) 0.0823(15) Uani 1 1 d D . . F2 F 0.6134(3) 0.4749(3) 0.1101(3) 0.130(3) Uani 1 1 d D . . F3 F 0.6685(3) 0.5663(2) 0.06790(17) 0.0855(14) Uani 1 1 d D . . F4 F 0.7502(3) 0.5767(3) 0.1426(2) 0.1070(19) Uani 1 1 d D . . F5 F 0.7326(3) 0.4663(3) 0.09983(19) 0.0799(13) Uani 1 1 d D . . F6 F 0.6308(4) 0.5847(3) 0.1552(2) 0.142(3) Uani 1 1 d D . . F7 F 0.3680(3) 0.1808(3) 0.1043(4) 0.144(3) Uani 1 1 d . . . F8 F 0.4325(3) 0.2802(3) 0.1414(3) 0.115(2) Uani 1 1 d . . . F9 F 0.3454(6) 0.2939(4) 0.0703(2) 0.183(4) Uani 1 1 d . . . F10 F 0.3291(3) 0.3377(3) 0.1555(2) 0.0930(17) Uani 1 1 d . . . F11 F 0.2630(2) 0.2377(2) 0.12177(18) 0.0678(11) Uani 1 1 d . . . F12 F 0.3478(4) 0.2229(4) 0.1914(3) 0.129(3) Uani 1 1 d . . . F13 F 0.0594(4) 0.5658(7) 0.5086(4) 0.1043(18) Uani 0.618(5) 1 d P D 1 F14 F 0.0553(4) 0.4544(7) 0.4633(4) 0.1043(18) Uani 0.618(5) 1 d P D 1 F15 F 0.0334(4) 0.4556(7) 0.5554(4) 0.1043(18) Uani 0.618(5) 1 d P D 1 F13B F 0.0653(6) 0.5390(11) 0.4716(7) 0.1043(18) Uani 0.382(5) 1 d P D 2 F14B F 0.0548(6) 0.4286(10) 0.5140(6) 0.1043(18) Uani 0.382(5) 1 d P D 2 F15B F 0.0239(6) 0.5334(11) 0.5603(6) 0.1043(18) Uani 0.382(5) 1 d P D 2 N1 N 0.2362(3) 0.5147(3) 0.1100(2) 0.0464(11) Uani 1 1 d . . . N2 N 0.3823(3) 0.5274(3) 0.0760(2) 0.0527(13) Uani 1 1 d . . . N3 N 0.2950(2) 0.5052(2) 0.23296(18) 0.0336(8) Uani 1 1 d . . . N4 N 0.2056(2) 0.4979(2) 0.52132(18) 0.0363(9) Uani 1 1 d . . . N6 N 0.2469(2) 0.4983(2) 0.62072(17) 0.0329(9) Uani 1 1 d . . . N5 N 0.4371(2) 0.5084(2) 0.19680(17) 0.0311(8) Uani 1 1 d . . . N7 N 0.5560(4) 0.7348(3) 0.3341(3) 0.0677(16) Uani 1 1 d . . . N8 N 0.1288(4) 0.4719(4) 0.7052(3) 0.0772(19) Uani 1 1 d . . . N9 N 0.0694(7) 0.5190(6) 0.2225(5) 0.127(4) Uani 1 1 d . . . C1 C 0.2539(4) 0.5117(4) 0.0479(3) 0.0635(18) Uani 1 1 d . . . H1A H 0.2616 0.4589 0.0367 0.076 Uiso 1 1 calc R . . H1B H 0.2119 0.5316 0.0243 0.076 Uiso 1 1 calc R . . C2 C 0.3215(4) 0.5564(5) 0.0369(3) 0.0665(19) Uani 1 1 d . . . H2A H 0.3344 0.5507 -0.0033 0.080 Uiso 1 1 calc R . . H2B H 0.3129 0.6102 0.0444 0.080 Uiso 1 1 calc R . . C3 C 0.1902(3) 0.4491(4) 0.1232(3) 0.0575(16) Uani 1 1 d . . . H3A H 0.1768 0.4518 0.1630 0.086 Uiso 1 1 calc R . . H3B H 0.2179 0.4030 0.1173 0.086 Uiso 1 1 calc R . . H3C H 0.1457 0.4492 0.0981 0.086 Uiso 1 1 calc R . . C4 C 0.1971(4) 0.5858(5) 0.1199(3) 0.069(2) Uani 1 1 d . . . H4A H 0.1521 0.5878 0.0952 0.103 Uiso 1 1 calc R . . H4B H 0.2288 0.6281 0.1111 0.103 Uiso 1 1 calc R . . H4C H 0.1844 0.5886 0.1599 0.103 Uiso 1 1 calc R . . C5 C 0.4425(4) 0.5866(4) 0.0758(3) 0.0675(18) Uani 1 1 d . . . H5A H 0.4851 0.5696 0.0995 0.101 Uiso 1 1 calc R . . H5B H 0.4242 0.6337 0.0911 0.101 Uiso 1 1 calc R . . H5C H 0.4571 0.5945 0.0367 0.101 Uiso 1 1 calc R . . C6 C 0.4165(4) 0.4581(4) 0.0565(3) 0.0602(16) Uani 1 1 d . . . H6A H 0.3792 0.4187 0.0521 0.090 Uiso 1 1 calc R . . H6B H 0.4549 0.4422 0.0847 0.090 Uiso 1 1 calc R . . H6C H 0.4382 0.4670 0.0199 0.090 Uiso 1 1 calc R . . C7 C 0.2943(3) 0.4398(3) 0.2624(2) 0.0377(10) Uani 1 1 d . . . H7 H 0.3059 0.3948 0.2433 0.045 Uiso 1 1 calc R . . C8 C 0.2775(3) 0.4361(3) 0.3187(2) 0.0370(10) Uani 1 1 d . . . H8 H 0.2783 0.3892 0.3379 0.044 Uiso 1 1 calc R . . C9 C 0.2594(3) 0.5010(2) 0.3475(2) 0.0313(9) Uani 1 1 d . . . C10 C 0.2588(3) 0.5684(3) 0.3169(2) 0.0384(10) Uani 1 1 d . . . H10 H 0.2460 0.6139 0.3348 0.046 Uiso 1 1 calc R . . C11 C 0.2770(3) 0.5680(3) 0.2600(2) 0.0383(10) Uani 1 1 d . . . H11 H 0.2767 0.6140 0.2397 0.046 Uiso 1 1 calc R . . C12 C 0.2421(2) 0.4997(3) 0.4086(2) 0.0310(9) Uani 1 1 d . . . C13 C 0.2267(3) 0.4319(3) 0.4365(2) 0.0371(10) Uani 1 1 d . . . H13 H 0.2291 0.3856 0.4167 0.045 Uiso 1 1 calc R . . C14 C 0.2083(3) 0.4336(3) 0.4922(2) 0.0400(11) Uani 1 1 d . . . H14 H 0.1972 0.3880 0.5107 0.048 Uiso 1 1 calc R . . C15 C 0.2209(3) 0.5640(3) 0.4961(2) 0.0369(10) Uani 1 1 d . . . H15 H 0.2188 0.6093 0.5172 0.044 Uiso 1 1 calc R . . C16 C 0.2393(3) 0.5655(3) 0.4401(2) 0.0359(10) Uani 1 1 d . . . H16 H 0.2502 0.6120 0.4227 0.043 Uiso 1 1 calc R . . C17 C 0.1825(3) 0.4987(3) 0.5802(2) 0.0406(12) Uani 1 1 d . . . H17A H 0.1517 0.4542 0.5869 0.049 Uiso 1 1 calc R . . H17B H 0.1527 0.5439 0.5864 0.049 Uiso 1 1 calc R . . C18 C 0.4667(3) 0.5707(3) 0.2172(2) 0.0385(11) Uani 1 1 d . . . H18 H 0.4432 0.6169 0.2078 0.046 Uiso 1 1 calc R . . C19 C 0.5310(3) 0.5720(3) 0.2522(2) 0.0364(10) Uani 1 1 d . . . H19 H 0.5508 0.6181 0.2660 0.044 Uiso 1 1 calc R . . C20 C 0.5654(2) 0.5051(2) 0.26630(19) 0.0277(8) Uani 1 1 d . . . C21 C 0.5348(3) 0.4394(3) 0.2433(2) 0.0344(10) Uani 1 1 d . . . H21 H 0.5577 0.3925 0.2512 0.041 Uiso 1 1 calc R . . C22 C 0.4713(3) 0.4428(3) 0.2093(2) 0.0371(10) Uani 1 1 d . . . H22 H 0.4508 0.3977 0.1941 0.045 Uiso 1 1 calc R . . C23 C 0.6317(2) 0.5039(2) 0.30511(19) 0.0274(8) Uani 1 1 d . . . C24 C 0.6648(3) 0.5698(3) 0.3246(3) 0.0454(13) Uani 1 1 d . . . H24 H 0.6450 0.6166 0.3123 0.055 Uiso 1 1 calc R . . C25 C 0.7255(3) 0.5680(3) 0.3613(3) 0.0469(14) Uani 1 1 d . . . H25 H 0.7481 0.6133 0.3741 0.056 Uiso 1 1 calc R . . C26 C 0.7231(3) 0.4370(3) 0.3610(2) 0.0481(15) Uani 1 1 d . . . H26 H 0.7444 0.3910 0.3737 0.058 Uiso 1 1 calc R . . C27 C 0.6622(4) 0.4364(3) 0.3243(2) 0.0487(15) Uani 1 1 d . . . H27 H 0.6409 0.3903 0.3121 0.058 Uiso 1 1 calc R . . C28 C 0.4100(2) 0.5016(2) 0.4776(2) 0.0325(10) Uani 1 1 d . . . C29 C 0.3946(2) 0.4606(3) 0.5273(2) 0.0353(10) Uani 1 1 d . E . H29 H 0.3857 0.4858 0.5619 0.042 Uiso 1 1 calc R . . C30 C 0.3927(3) 0.3848(3) 0.5247(2) 0.0419(11) Uani 1 1 d . . . H30 H 0.3824 0.3571 0.5579 0.050 Uiso 1 1 calc R E . C31 C 0.4057(3) 0.3460(3) 0.4739(2) 0.0428(11) Uani 1 1 d . E . H31 H 0.4030 0.2929 0.4730 0.051 Uiso 1 1 calc R . . C32 C 0.4223(3) 0.3847(3) 0.4259(2) 0.0379(10) Uani 1 1 d . . . C33 C 0.4255(2) 0.4647(3) 0.4269(2) 0.0335(10) Uani 1 1 d . E . C34 C 0.4423(3) 0.5068(3) 0.3780(2) 0.0409(11) Uani 1 1 d . . . H34 H 0.4530 0.4819 0.3436 0.049 Uiso 1 1 calc R E . C35 C 0.4429(3) 0.5828(3) 0.3804(3) 0.0527(15) Uani 1 1 d . E . H35 H 0.4544 0.6105 0.3475 0.063 Uiso 1 1 calc R . . C36 C 0.4271(3) 0.6215(3) 0.4301(3) 0.0488(14) Uani 1 1 d . . . H36 H 0.4279 0.6746 0.4308 0.059 Uiso 1 1 calc R E . C37 C 0.4103(2) 0.5819(3) 0.4781(2) 0.0386(11) Uani 1 1 d . E . C38A C 0.3888(9) 0.6966(8) 0.5187(6) 0.044(3) Uani 0.50 1 d P E 7 H38A H 0.4387 0.7182 0.5179 0.052 Uiso 0.50 1 calc PR E 7 H38B H 0.3607 0.7094 0.4829 0.052 Uiso 0.50 1 calc PR E 7 C39A C 0.3501(6) 0.7225(6) 0.5701(5) 0.045(2) Uani 0.50 1 d P E 7 H39A H 0.3686 0.6944 0.6042 0.054 Uiso 0.50 1 calc PR E 7 H39B H 0.3598 0.7764 0.5767 0.054 Uiso 0.50 1 calc PR E 7 C38B C 0.4018(8) 0.6912(8) 0.5448(6) 0.040(3) Uani 0.50 1 d P E 8 H38C H 0.4455 0.7117 0.5270 0.048 Uiso 0.50 1 calc PR E 8 H38D H 0.4101 0.6947 0.5867 0.048 Uiso 0.50 1 calc PR E 8 C39B C 0.3364(6) 0.7354(6) 0.5266(5) 0.043(2) Uani 0.50 1 d P E 8 H39C H 0.3460 0.7895 0.5325 0.052 Uiso 0.50 1 calc PR E 8 H39D H 0.3235 0.7269 0.4856 0.052 Uiso 0.50 1 calc PR E 8 C40 C 0.2223(5) 0.7633(4) 0.5691(6) 0.115(4) Uani 1 1 d . E . H40A H 0.2240 0.8024 0.5393 0.138 Uiso 1 1 calc R F 9 H40B H 0.2307 0.7876 0.6067 0.138 Uiso 1 1 calc R F 9 C41A C 0.1472(9) 0.7254(9) 0.5657(7) 0.053(5) Uani 0.50 1 d P E 9 H41A H 0.1100 0.7636 0.5742 0.064 Uiso 0.50 1 calc PR E 9 H41B H 0.1368 0.7090 0.5258 0.064 Uiso 0.50 1 calc PR E 9 C41B C 0.1598(11) 0.7537(11) 0.5846(11) 0.079(6) Uani 0.50 1 d P E 10 H41C H 0.1248 0.7737 0.5547 0.095 Uiso 0.50 1 calc PR E 10 H41D H 0.1539 0.7837 0.6195 0.095 Uiso 0.50 1 calc PR E 10 C42 C 0.0874(3) 0.6733(4) 0.6410(3) 0.0622(17) Uani 1 1 d . . . H42A H 0.0791 0.6220 0.6554 0.075 Uiso 1 1 calc R . . H42B H 0.0398 0.6928 0.6252 0.075 Uiso 1 1 calc R . . C43 C 0.4279(4) 0.2726(3) 0.3703(3) 0.0593(17) Uani 1 1 d . . . H43A H 0.3762 0.2591 0.3761 0.071 Uiso 1 1 calc R E . H43B H 0.4596 0.2465 0.3995 0.071 Uiso 1 1 calc R . . C44 C 0.4482(4) 0.2504(4) 0.3123(3) 0.068(2) Uani 1 1 d . E . H44A H 0.4292 0.1996 0.3033 0.082 Uiso 1 1 calc R . . H44B H 0.4262 0.2857 0.2838 0.082 Uiso 1 1 calc R . . C45 C 0.5493(5) 0.2130(4) 0.2620(4) 0.078(2) Uani 1 1 d . . . H45A H 0.5294 0.2383 0.2270 0.094 Uiso 1 1 calc R . . H45B H 0.5301 0.1612 0.2620 0.094 Uiso 1 1 calc R . . C46 C 0.6307(5) 0.2116(4) 0.2624(4) 0.071(2) Uani 1 1 d . . . H46A H 0.6508 0.1902 0.2988 0.085 Uiso 1 1 calc R . . H46B H 0.6467 0.1796 0.2309 0.085 Uiso 1 1 calc R . . C47 C 0.7123(5) 0.2913(5) 0.2188(4) 0.076(2) Uani 1 1 d D . . H47A H 0.7190 0.3446 0.2088 0.091 Uiso 1 1 calc R G 11 H47B H 0.6974 0.2642 0.1833 0.091 Uiso 1 1 calc R G 11 C48A C 0.7838(5) 0.2607(5) 0.2418(4) 0.0262(17) Uani 0.50 1 d P A 11 H48A H 0.7763 0.2094 0.2564 0.031 Uiso 0.50 1 calc PR A 11 H48B H 0.8183 0.2575 0.2107 0.031 Uiso 0.50 1 calc PR A 11 C49A C 0.8831(15) 0.2741(9) 0.3072(12) 0.048(4) Uani 0.50 1 d P . 11 H49A H 0.9187 0.2731 0.2768 0.057 Uiso 0.50 1 calc PR . 11 H49B H 0.8757 0.2223 0.3207 0.057 Uiso 0.50 1 calc PR . 11 C48B C 0.7807(10) 0.3224(19) 0.2407(9) 0.37(5) Uani 0.50 1 d PD B 12 H48C H 0.7836 0.3688 0.2177 0.447 Uiso 0.50 1 calc PR B 12 H48D H 0.8165 0.2880 0.2243 0.447 Uiso 0.50 1 calc PR B 12 C49B C 0.8909(14) 0.3033(17) 0.3106(11) 0.097(10) Uani 0.50 1 d P . 12 H49C H 0.8822 0.2486 0.3119 0.117 Uiso 0.50 1 calc PR . 12 H49D H 0.9284 0.3134 0.2825 0.117 Uiso 0.50 1 calc PR . 12 C50 C 0.0365(7) 0.2696(8) 0.5325(5) 0.091(4) Uani 0.75 1 d P C 8 H50A H 0.0602 0.2478 0.4998 0.137 Uiso 0.75 1 calc PR C 8 H50B H 0.0099 0.3150 0.5203 0.137 Uiso 0.75 1 calc PR C 8 H50C H 0.0021 0.2333 0.5474 0.137 Uiso 0.75 1 calc PR C 8 C51 C 0.0933(6) 0.2890(6) 0.5778(5) 0.075(3) Uani 0.75 1 d P C 8 H51A H 0.0740 0.3360 0.5936 0.090 Uiso 0.75 1 calc PR C 8 H51B H 0.0852 0.2506 0.6073 0.090 Uiso 0.75 1 calc PR C 8 C52 C 0.2686(8) 0.2208(9) 0.5456(14) 0.141(10) Uani 0.75 1 d P C 8 H52A H 0.2754 0.2288 0.5049 0.211 Uiso 0.75 1 calc PR C 8 H52B H 0.2894 0.1722 0.5572 0.211 Uiso 0.75 1 calc PR C 8 H52C H 0.2936 0.2607 0.5677 0.211 Uiso 0.75 1 calc PR C 8 C53 C 0.1885(12) 0.2220(9) 0.5562(11) 0.168(9) Uani 0.75 1 d P C 8 H53A H 0.1779 0.1805 0.5824 0.202 Uiso 0.75 1 calc PR C 8 H53B H 0.1607 0.2122 0.5196 0.202 Uiso 0.75 1 calc PR C 8 C54 C 0.5041(5) 0.7697(4) 0.3367(4) 0.073(2) Uani 1 1 d . . . C55 C 0.4364(7) 0.8154(6) 0.3413(6) 0.124(4) Uani 1 1 d . . . H55A H 0.3932 0.7844 0.3317 0.186 Uiso 1 1 calc R . . H55B H 0.4375 0.8577 0.3147 0.186 Uiso 1 1 calc R . . H55C H 0.4339 0.8343 0.3803 0.186 Uiso 1 1 calc R . . C56 C 0.1257(5) 0.5039(5) 0.7476(5) 0.084(3) Uani 1 1 d . . . C57 C 0.1185(6) 0.5494(8) 0.8011(5) 0.123(4) Uani 1 1 d . . . H57A H 0.0857 0.5919 0.7930 0.184 Uiso 1 1 calc R . . H57B H 0.1670 0.5680 0.8145 0.184 Uiso 1 1 calc R . . H57C H 0.0983 0.5180 0.8307 0.184 Uiso 1 1 calc R . . C58 C 0.0655(5) 0.5189(5) 0.2728(4) 0.077(2) Uani 1 1 d . . . C59 C 0.0552(4) 0.5201(5) 0.3320(4) 0.077(2) Uani 1 1 d . . . H59A H 0.0026 0.5193 0.3384 0.115 Uiso 1 1 calc R . . H59B H 0.0772 0.5656 0.3487 0.115 Uiso 1 1 calc R . . H59C H 0.0786 0.4760 0.3499 0.115 Uiso 1 1 calc R . . P4 P 1.0210(6) 0.6102(7) -0.0059(5) 0.073(3) Uani 0.275(4) 1 d PD H 1 F16 F 0.9770(10) 0.6780(8) -0.0287(7) 0.094(2) Uani 0.275(4) 1 d PD H 1 F20 F 1.0551(10) 0.5900(10) -0.0649(6) 0.094(2) Uani 0.275(4) 1 d PD H 1 F17 F 1.0945(8) 0.6500(9) 0.0143(7) 0.094(2) Uani 0.275(4) 1 d PD H 1 F18 F 0.9893(10) 0.6310(10) 0.0519(7) 0.094(2) Uani 0.275(4) 1 d PD H 1 F19 F 1.0551(12) 0.5373(10) 0.0201(10) 0.094(2) Uani 0.275(4) 1 d PD H 1 F21 F 0.9468(8) 0.5663(10) -0.0254(8) 0.094(2) Uani 0.275(4) 1 d PD H 1 P4A P 0.9978(7) 0.5968(8) -0.0070(6) 0.073(3) Uani 0.225(4) 1 d PD H 2 F16A F 0.9238(10) 0.6382(11) -0.0204(9) 0.094(2) Uani 0.225(4) 1 d PD H 2 F20A F 1.0136(12) 0.5889(11) -0.0732(7) 0.094(2) Uani 0.225(4) 1 d PD H 2 F17A F 1.0517(11) 0.6624(10) 0.0058(9) 0.094(2) Uani 0.225(4) 1 d PD H 2 F18A F 0.9745(13) 0.6054(12) 0.0561(7) 0.094(2) Uani 0.225(4) 1 d PD H 2 F19A F 1.0633(12) 0.5460(13) 0.0109(12) 0.094(2) Uani 0.225(4) 1 d PD . 2 F21A F 0.9472(11) 0.5249(10) -0.0192(10) 0.094(2) Uani 0.225(4) 1 d PD . 2 P5 P 0.14624(11) 0.26336(12) 0.33253(13) 0.0393(7) Uani 0.663(5) 1 d PD I 5 F22 F 0.1347(4) 0.3509(3) 0.3270(4) 0.074(3) Uani 0.663(5) 1 d PD I 5 F23 F 0.2252(3) 0.2761(3) 0.3640(3) 0.074(2) Uani 0.663(5) 1 d PD I 5 F24 F 0.1579(4) 0.1750(4) 0.3407(4) 0.0405(15) Uani 0.663(5) 1 d PD I 5 F26 F 0.0669(4) 0.2484(6) 0.3050(6) 0.078(4) Uani 0.663(5) 1 d PD I 5 F25 F 0.1103(4) 0.2641(4) 0.3923(3) 0.089(2) Uani 0.663(5) 1 d PD I 5 F27 F 0.1837(5) 0.2630(5) 0.2733(3) 0.090(3) Uani 0.663(5) 1 d PD I 5 P5A P 0.1444(4) 0.2733(3) 0.2935(3) 0.0630(18) Uani 0.337(5) 1 d PD I 6 F22A F 0.2305(6) 0.2673(7) 0.2983(7) 0.082(5) Uani 0.337(5) 1 d PD I 6 F23A F 0.1378(8) 0.2243(6) 0.2379(4) 0.072(4) Uani 0.337(5) 1 d PD I 6 F24A F 0.1448(7) 0.3457(6) 0.2573(6) 0.086(5) Uani 0.337(5) 1 d PD I 6 F26A F 0.1501(9) 0.3197(10) 0.3513(6) 0.091(6) Uani 0.337(5) 1 d PD I 6 F25A F 0.0617(8) 0.2707(12) 0.2949(8) 0.075(7) Uani 0.337(5) 1 d PD I 6 F27A F 0.1570(12) 0.1959(9) 0.3289(8) 0.070(7) Uani 0.337(5) 1 d PD I 6 N10 N 0.2432(13) 0.2456(11) 0.4828(10) 0.059(6) Uani 0.25 1 d P J 7 C60 C 0.3106(19) 0.1927(19) 0.5715(12) 0.059(7) Uani 0.25 1 d P J 7 H60A H 0.3110 0.2450 0.5841 0.089 Uiso 0.25 1 calc PR J 7 H60B H 0.3574 0.1690 0.5831 0.089 Uiso 0.25 1 calc PR J 7 H60C H 0.2705 0.1659 0.5888 0.089 Uiso 0.25 1 calc PR J 7 C61 C 0.303(6) 0.191(6) 0.530(3) 0.24(6) Uani 0.25 1 d P J 7 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 0.02685(19) 0.0521(3) 0.0257(2) 0.00124(15) -0.00315(13) 0.00022(14) P1 0.0671(11) 0.0541(9) 0.0400(8) 0.0099(6) 0.0099(7) 0.0077(7) P2 0.0726(11) 0.0432(8) 0.0569(10) -0.0124(7) 0.0034(8) -0.0053(7) P3 0.0225(9) 0.167(3) 0.0431(13) 0.0072(15) -0.0080(9) -0.0098(12) O1 0.050(2) 0.042(2) 0.051(2) -0.0122(17) 0.0022(18) -0.0030(16) O2 0.072(3) 0.069(3) 0.055(3) -0.031(2) -0.007(2) 0.016(2) O3 0.096(4) 0.044(2) 0.074(3) -0.016(2) 0.031(3) -0.005(2) O4A 0.035(4) 0.017(3) 0.030(3) -0.006(2) -0.003(3) 0.011(3) O4B 0.106(14) 0.28(3) 0.20(2) 0.15(2) 0.104(15) 0.138(18) O5 0.0330(18) 0.0351(19) 0.078(3) -0.0152(18) 0.0094(18) -0.0032(14) O6 0.041(2) 0.070(3) 0.044(2) -0.0089(19) 0.0047(17) 0.0167(18) O7 0.047(2) 0.076(3) 0.049(2) -0.011(2) 0.0103(19) 0.017(2) O8 0.074(4) 0.057(4) 0.091(5) 0.027(3) -0.017(4) -0.021(3) F1 0.109(4) 0.090(3) 0.050(2) 0.025(2) 0.026(2) 0.032(3) F2 0.073(3) 0.118(4) 0.194(7) 0.086(5) -0.042(4) -0.032(3) F3 0.142(4) 0.061(2) 0.051(2) 0.0172(18) -0.012(3) -0.012(3) F4 0.136(5) 0.081(3) 0.100(4) 0.008(3) -0.033(3) -0.033(3) F5 0.103(4) 0.078(3) 0.059(3) -0.004(2) 0.015(2) 0.021(3) F6 0.218(7) 0.119(4) 0.095(4) 0.041(3) 0.073(4) 0.105(5) F7 0.074(3) 0.093(4) 0.268(9) -0.102(5) 0.038(4) -0.015(3) F8 0.074(3) 0.083(3) 0.190(6) -0.057(4) 0.029(4) -0.022(3) F9 0.335(12) 0.165(6) 0.049(3) -0.006(3) 0.008(5) -0.149(7) F10 0.097(4) 0.060(3) 0.120(4) -0.050(3) -0.013(3) 0.004(2) F11 0.073(3) 0.053(2) 0.075(3) -0.0153(18) -0.018(2) 0.0066(18) F12 0.141(5) 0.142(5) 0.095(4) 0.050(4) -0.061(4) -0.064(4) F13 0.0316(16) 0.202(5) 0.078(3) -0.002(3) -0.0131(18) -0.006(2) F14 0.0316(16) 0.202(5) 0.078(3) -0.002(3) -0.0131(18) -0.006(2) F15 0.0316(16) 0.202(5) 0.078(3) -0.002(3) -0.0131(18) -0.006(2) F13B 0.0316(16) 0.202(5) 0.078(3) -0.002(3) -0.0131(18) -0.006(2) F14B 0.0316(16) 0.202(5) 0.078(3) -0.002(3) -0.0131(18) -0.006(2) F15B 0.0316(16) 0.202(5) 0.078(3) -0.002(3) -0.0131(18) -0.006(2) N1 0.033(2) 0.069(3) 0.036(2) 0.000(2) -0.0090(18) 0.000(2) N2 0.044(3) 0.082(4) 0.031(2) 0.008(2) -0.002(2) 0.017(2) N3 0.0278(18) 0.041(2) 0.032(2) 0.0016(15) 0.0007(16) -0.0034(15) N4 0.0210(17) 0.059(3) 0.0285(19) 0.0070(17) -0.0022(15) 0.0009(15) N6 0.0231(17) 0.050(2) 0.0259(18) 0.0049(15) 0.0006(14) 0.0085(15) N5 0.0270(18) 0.039(2) 0.0273(18) 0.0047(15) -0.0038(15) -0.0009(14) N7 0.092(5) 0.038(3) 0.074(4) 0.000(3) 0.015(3) -0.005(3) N8 0.085(5) 0.076(4) 0.073(5) 0.010(3) 0.029(4) 0.015(3) N9 0.146(10) 0.130(8) 0.110(8) -0.007(6) 0.056(7) 0.020(7) C1 0.053(4) 0.101(5) 0.035(3) 0.011(3) -0.013(3) -0.005(3) C2 0.061(4) 0.100(5) 0.039(3) 0.012(3) 0.003(3) 0.020(4) C3 0.035(3) 0.087(5) 0.050(3) 0.000(3) -0.008(2) -0.016(3) C4 0.041(3) 0.097(5) 0.065(4) -0.007(4) -0.019(3) 0.016(3) C5 0.069(4) 0.076(5) 0.059(4) 0.018(3) 0.019(3) 0.004(4) C6 0.060(4) 0.074(4) 0.049(3) 0.002(3) 0.025(3) 0.012(3) C7 0.044(3) 0.036(2) 0.033(2) -0.0038(19) -0.001(2) -0.007(2) C8 0.042(3) 0.034(2) 0.034(2) 0.0006(18) -0.004(2) -0.0095(19) C9 0.025(2) 0.039(3) 0.029(2) 0.0007(17) -0.0012(17) -0.0056(16) C10 0.045(3) 0.041(3) 0.030(2) 0.0042(19) 0.004(2) 0.003(2) C11 0.042(3) 0.041(3) 0.033(2) 0.0057(19) 0.006(2) 0.000(2) C12 0.0216(18) 0.041(3) 0.030(2) 0.0063(17) -0.0045(17) -0.0035(15) C13 0.036(2) 0.041(3) 0.035(2) 0.0083(19) 0.000(2) -0.0017(19) C14 0.038(2) 0.045(3) 0.038(3) 0.009(2) 0.005(2) 0.006(2) C15 0.027(2) 0.052(3) 0.031(2) -0.004(2) -0.0028(18) -0.0023(19) C16 0.030(2) 0.046(3) 0.032(2) 0.0022(19) -0.0034(18) -0.0075(19) C17 0.0201(19) 0.069(4) 0.032(2) 0.005(2) -0.0030(18) 0.0066(19) C18 0.034(2) 0.036(2) 0.045(3) 0.011(2) -0.011(2) 0.0031(18) C19 0.031(2) 0.028(2) 0.048(3) 0.0098(19) -0.010(2) 0.0009(17) C20 0.0274(19) 0.028(2) 0.028(2) 0.0073(15) -0.0010(16) 0.0019(15) C21 0.031(2) 0.030(2) 0.041(3) 0.0004(18) -0.0047(19) 0.0017(17) C22 0.034(2) 0.031(2) 0.045(3) -0.0036(19) -0.006(2) -0.0006(18) C23 0.027(2) 0.030(2) 0.025(2) 0.0034(15) 0.0001(16) 0.0038(15) C24 0.039(3) 0.032(2) 0.063(3) 0.021(2) -0.019(2) -0.0069(19) C25 0.038(3) 0.041(3) 0.060(3) 0.020(2) -0.016(2) -0.016(2) C26 0.063(3) 0.041(3) 0.037(3) -0.010(2) -0.022(2) 0.031(3) C27 0.073(4) 0.030(2) 0.040(3) -0.010(2) -0.024(3) 0.020(2) C28 0.0165(17) 0.033(2) 0.048(3) 0.0005(18) -0.0031(18) 0.0009(14) C29 0.024(2) 0.040(2) 0.042(3) -0.001(2) 0.0039(18) 0.0031(17) C30 0.037(3) 0.042(3) 0.047(3) 0.007(2) 0.005(2) 0.005(2) C31 0.040(3) 0.033(2) 0.056(3) 0.002(2) 0.006(2) 0.0038(19) C32 0.029(2) 0.038(2) 0.046(3) -0.005(2) -0.003(2) -0.0001(18) C33 0.0225(19) 0.036(2) 0.042(3) -0.0013(19) -0.0038(18) -0.0058(16) C34 0.035(2) 0.048(3) 0.040(3) 0.001(2) -0.002(2) -0.012(2) C35 0.047(3) 0.054(3) 0.056(3) 0.014(3) -0.007(3) -0.024(3) C36 0.039(3) 0.033(3) 0.074(4) 0.004(2) -0.004(3) -0.008(2) C37 0.022(2) 0.036(2) 0.058(3) -0.004(2) 0.002(2) -0.0016(17) C38A 0.052(8) 0.036(6) 0.044(7) -0.007(7) 0.015(7) -0.007(5) C39A 0.049(6) 0.040(6) 0.048(7) -0.017(5) 0.011(5) -0.006(4) C38B 0.042(6) 0.032(6) 0.046(7) -0.009(6) 0.007(7) -0.004(4) C39B 0.049(6) 0.041(6) 0.040(6) -0.001(4) 0.007(5) 0.000(5) C40 0.068(5) 0.045(4) 0.235(14) -0.037(6) 0.057(7) 0.009(4) C41A 0.057(8) 0.046(9) 0.056(8) -0.018(6) -0.015(6) 0.037(7) C41B 0.069(12) 0.062(12) 0.109(18) 0.029(10) 0.038(12) 0.034(10) C42 0.042(3) 0.067(4) 0.079(5) 0.003(3) 0.024(3) 0.015(3) C43 0.054(4) 0.043(3) 0.080(5) -0.021(3) -0.002(3) -0.004(3) C44 0.071(5) 0.062(4) 0.069(4) -0.030(3) -0.016(4) 0.004(3) C45 0.100(6) 0.062(4) 0.073(5) -0.031(4) 0.007(4) 0.007(4) C46 0.092(6) 0.041(3) 0.082(5) -0.014(3) 0.023(4) 0.003(3) C47 0.090(6) 0.071(5) 0.068(5) -0.013(4) 0.020(4) -0.008(4) C48A 0.034(5) 0.022(4) 0.023(4) -0.008(3) 0.005(3) 0.001(3) C49A 0.056(8) 0.031(6) 0.056(10) -0.011(5) 0.003(6) 0.013(5) C48B 0.19(3) 0.89(12) 0.048(12) 0.11(3) 0.048(15) 0.37(6) C49B 0.060(14) 0.18(3) 0.051(10) -0.015(19) 0.021(10) 0.066(18) C50 0.081(8) 0.130(10) 0.064(6) -0.022(7) 0.008(6) -0.040(7) C51 0.090(8) 0.056(5) 0.077(7) -0.003(5) -0.004(6) -0.031(5) C52 0.053(7) 0.068(8) 0.30(3) -0.025(14) 0.028(13) -0.017(6) C53 0.19(2) 0.087(11) 0.24(2) 0.065(13) 0.058(18) 0.000(11) C54 0.101(6) 0.036(3) 0.085(5) 0.005(3) 0.032(5) 0.007(3) C55 0.135(10) 0.090(7) 0.152(10) 0.026(7) 0.055(8) 0.051(7) C56 0.052(4) 0.107(7) 0.094(7) 0.015(5) 0.006(5) 0.008(4) C57 0.082(7) 0.188(13) 0.098(8) -0.022(8) 0.010(6) 0.016(8) C58 0.054(4) 0.097(6) 0.081(6) 0.003(5) 0.016(4) 0.011(4) C59 0.050(4) 0.112(6) 0.066(5) 0.012(4) -0.002(4) 0.004(4) P4 0.064(7) 0.075(5) 0.075(3) -0.025(3) -0.027(4) 0.012(5) F16 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) F20 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) F17 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) F18 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) F19 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) F21 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) P4A 0.064(7) 0.075(5) 0.075(3) -0.025(3) -0.027(4) 0.012(5) F16A 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) F20A 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) F17A 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) F18A 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) F19A 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) F21A 0.098(4) 0.082(4) 0.099(4) -0.034(3) -0.034(3) 0.032(3) P5 0.0297(9) 0.0343(12) 0.0532(17) -0.0088(9) -0.0031(9) -0.0011(7) F22 0.052(3) 0.037(3) 0.129(7) 0.004(4) -0.026(4) 0.004(3) F23 0.052(3) 0.041(3) 0.125(6) 0.000(3) -0.042(4) -0.004(2) F24 0.042(3) 0.024(3) 0.056(4) -0.003(3) 0.003(3) -0.008(2) F26 0.034(3) 0.044(4) 0.154(11) -0.021(5) -0.020(4) -0.004(2) F25 0.102(5) 0.105(5) 0.061(4) -0.012(4) 0.019(4) 0.046(4) F27 0.095(6) 0.118(7) 0.061(5) 0.041(4) 0.034(5) 0.043(5) P5A 0.093(5) 0.049(3) 0.049(4) -0.018(2) 0.023(3) -0.027(3) F22A 0.080(9) 0.051(7) 0.113(13) -0.015(7) -0.027(9) 0.021(6) F23A 0.114(11) 0.045(6) 0.055(7) -0.011(5) -0.012(7) -0.011(6) F24A 0.091(10) 0.045(6) 0.118(12) -0.001(7) -0.032(8) 0.002(6) F26A 0.094(13) 0.084(12) 0.099(13) -0.057(10) 0.035(10) -0.030(10) F25A 0.075(12) 0.106(19) 0.044(7) -0.022(9) 0.009(7) -0.015(10) F27A 0.097(12) 0.059(13) 0.055(9) 0.019(7) -0.008(7) -0.045(10) N10 0.069(14) 0.035(10) 0.068(15) -0.012(9) -0.026(12) -0.007(9) C60 0.065(18) 0.069(18) 0.044(14) 0.018(13) 0.001(12) -0.019(14) C61 0.29(10) 0.30(11) 0.14(5) -0.17(6) 0.15(6) -0.24(9) _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 N5 2.037(4) . ? Pd1 N3 2.039(4) . ? Pd1 N1 2.068(4) . ? Pd1 N2 2.073(5) . ? P1 F2 1.561(6) . ? P1 F5 1.570(5) . ? P1 F6 1.571(5) . ? P1 F1 1.575(4) . ? P1 F3 1.587(4) . ? P1 F4 1.591(5) . ? P2 F12 1.535(6) . ? P2 F10 1.566(4) . ? P2 F9 1.577(6) . ? P2 F7 1.581(5) . ? P2 F11 1.589(5) . ? P2 F8 1.608(5) . ? P3 F13B 1.560(15) . ? P3 F13B 1.560(15) 3_566 ? P3 F15B 1.577(14) . ? P3 F15B 1.577(14) 3_566 ? P3 F14 1.586(9) . ? P3 F14 1.586(9) 3_566 ? P3 F13 1.605(10) 3_566 ? P3 F13 1.605(10) . ? P3 F15 1.615(9) 3_566 ? P3 F15 1.615(9) . ? P3 F14B 1.643(16) 3_566 ? P3 F14B 1.643(16) . ? O1 C32 1.357(6) . ? O1 C43 1.459(7) . ? O2 C45 1.402(8) . ? O2 C44 1.432(9) . ? O3 C47 1.362(9) . ? O3 C46 1.426(8) . ? O4A C48A 1.404(10) . ? O4A C49A 1.43(3) . ? O4B C48B 1.45(2) . ? O4B C49B 1.53(3) . ? O5 C37 1.366(7) . ? O5 C38B 1.452(14) . ? O5 C38A 1.502(15) . ? O6 C39A 1.365(12) . ? O6 C40 1.381(8) . ? O6 C39B 1.464(12) . ? O7 C41A 1.25(2) . ? O7 C42 1.416(7) . ? O7 C41B 1.57(2) . ? O8 C51 1.209(12) . ? O8 C53 1.61(2) . ? N1 C4 1.482(9) . ? N1 C3 1.483(8) . ? N1 C1 1.509(8) . ? N2 C6 1.472(8) . ? N2 C2 1.495(8) . ? N2 C5 1.526(9) . ? N3 C11 1.338(7) . ? N3 C7 1.357(6) . ? N4 C14 1.338(7) . ? N4 C15 1.357(7) . ? N4 C17 1.466(7) . ? N6 C26 1.339(7) 3_666 ? N6 C25 1.345(6) 3_666 ? N6 C17 1.474(6) . ? N5 C18 1.317(6) . ? N5 C22 1.352(6) . ? N7 C54 1.138(10) . ? N8 C56 1.154(12) . ? N9 C58 1.187(14) . ? C1 C2 1.505(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.375(7) . ? C7 H7 0.9500 . ? C8 C9 1.391(7) . ? C8 H8 0.9500 . ? C9 C10 1.403(7) . ? C9 C12 1.485(7) . ? C10 C11 1.393(7) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C16 1.390(7) . ? C12 C13 1.412(6) . ? C13 C14 1.369(7) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.376(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.397(6) . ? C18 H18 0.9500 . ? C19 C20 1.382(6) . ? C19 H19 0.9500 . ? C20 C21 1.397(6) . ? C20 C23 1.478(6) . ? C21 C22 1.375(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.389(7) . ? C23 C27 1.392(6) . ? C24 C25 1.371(7) . ? C24 H24 0.9500 . ? C25 N6 1.345(6) 3_666 ? C25 H25 0.9500 . ? C26 N6 1.339(7) 3_666 ? C26 C27 1.373(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.402(7) . ? C28 C29 1.419(7) . ? C28 C37 1.435(6) . ? C29 C30 1.356(7) . ? C29 H29 0.9500 . ? C30 C31 1.410(8) . ? C30 H30 0.9500 . ? C31 C32 1.370(8) . ? C31 H31 0.9500 . ? C32 C33 1.429(7) . ? C33 C34 1.421(7) . ? C34 C35 1.359(8) . ? C34 H34 0.9500 . ? C35 C36 1.399(9) . ? C35 H35 0.9500 . ? C36 C37 1.378(8) . ? C36 H36 0.9500 . ? C38A C39A 1.502(18) . ? C38A H38A 0.9900 . ? C38A H38B 0.9900 . ? C39A H39A 0.9900 . ? C39A H39B 0.9900 . ? C38B C39B 1.476(18) . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? C39B H39C 0.9900 . ? C39B H39D 0.9900 . ? C40 C41B 1.23(2) . ? C40 C41A 1.53(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41A H41A 0.9900 . ? C41A H41B 0.9900 . ? C41B H41C 0.9900 . ? C41B H41D 0.9900 . ? C42 C49B 1.26(3) 3_666 ? C42 C49A 1.61(2) 3_666 ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.484(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.486(12) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48B 1.44(2) . ? C47 C48A 1.491(12) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48A H48A 0.9900 . ? C48A H48B 0.9900 . ? C49A C42 1.61(2) 3_666 ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C48B H48C 0.9900 . ? C48B H48D 0.9900 . ? C49B C42 1.26(3) 3_666 ? C49B H49C 0.9900 . ? C49B H49D 0.9900 . ? C50 C51 1.488(14) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.50(2) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.490(12) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.507(16) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.412(13) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? P4 F16 1.535(13) . ? P4 F18 1.548(13) . ? P4 F19 1.554(14) . ? P4 F17 1.570(13) . ? P4 F20 1.591(14) . ? P4 F21 1.611(13) . ? P4A F19A 1.543(14) . ? P4A F17A 1.550(14) . ? P4A F16A 1.557(14) . ? P4A F18A 1.571(15) . ? P4A F21A 1.599(15) . ? P4A F20A 1.603(15) . ? F19A F21A 1.30(3) 3_765 ? F21A F19A 1.30(3) 3_765 ? P5 F26 1.578(8) . ? P5 F25 1.580(7) . ? P5 F27 1.580(7) . ? P5 F22 1.582(6) . ? P5 F24 1.602(7) . ? P5 F23 1.603(5) . ? P5A F25A 1.512(14) . ? P5A F24A 1.549(11) . ? P5A F23A 1.571(10) . ? P5A F22A 1.572(12) . ? P5A F26A 1.589(12) . ? P5A F27A 1.623(12) . ? N10 C61 1.81(15) . ? C60 C61 0.98(8) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? 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 N5 Pd1 N3 85.66(16) . . ? N5 Pd1 N1 178.85(19) . . ? N3 Pd1 N1 95.28(19) . . ? N5 Pd1 N2 92.90(18) . . ? N3 Pd1 N2 175.6(2) . . ? N1 Pd1 N2 86.2(2) . . ? F2 P1 F5 89.5(4) . . ? F2 P1 F6 91.6(5) . . ? F5 P1 F6 178.8(4) . . ? F2 P1 F1 92.4(3) . . ? F5 P1 F1 89.4(2) . . ? F6 P1 F1 90.7(3) . . ? F2 P1 F3 87.7(3) . . ? F5 P1 F3 90.5(3) . . ? F6 P1 F3 89.4(3) . . ? F1 P1 F3 179.9(3) . . ? F2 P1 F4 177.8(4) . . ? F5 P1 F4 89.7(3) . . ? F6 P1 F4 89.2(4) . . ? F1 P1 F4 89.7(3) . . ? F3 P1 F4 90.2(3) . . ? F12 P2 F10 92.3(4) . . ? F12 P2 F9 178.9(4) . . ? F10 P2 F9 88.0(4) . . ? F12 P2 F7 91.3(5) . . ? F10 P2 F7 176.1(4) . . ? F9 P2 F7 88.5(5) . . ? F12 P2 F11 90.0(3) . . ? F10 P2 F11 92.3(2) . . ? F9 P2 F11 88.9(4) . . ? F7 P2 F11 89.2(3) . . ? F12 P2 F8 90.7(4) . . ? F10 P2 F8 87.2(3) . . ? F9 P2 F8 90.4(4) . . ? F7 P2 F8 91.3(3) . . ? F11 P2 F8 179.2(3) . . ? F13B P3 F13B 179.998(3) . 3_566 ? F13B P3 F15B 91.8(8) . . ? F13B P3 F15B 88.2(8) 3_566 . ? F13B P3 F15B 88.2(8) . 3_566 ? F13B P3 F15B 91.8(8) 3_566 3_566 ? F15B P3 F15B 179.999(3) . 3_566 ? F13B P3 F14 58.4(8) . . ? F13B P3 F14 121.6(8) 3_566 . ? F15B P3 F14 121.9(6) . . ? F15B P3 F14 58.1(5) 3_566 . ? F13B P3 F14 121.6(8) . 3_566 ? F13B P3 F14 58.4(8) 3_566 3_566 ? F15B P3 F14 58.1(6) . 3_566 ? F15B P3 F14 121.9(6) 3_566 3_566 ? F14 P3 F14 179.999(2) . 3_566 ? F13B P3 F13 143.1(6) . 3_566 ? F13B P3 F13 36.9(6) 3_566 3_566 ? F15B P3 F13 123.0(6) . 3_566 ? F15B P3 F13 57.0(6) 3_566 3_566 ? F14 P3 F13 90.0(5) . 3_566 ? F14 P3 F13 90.0(5) 3_566 3_566 ? F13B P3 F13 36.9(6) . . ? F13B P3 F13 143.1(6) 3_566 . ? F15B P3 F13 57.0(6) . . ? F15B P3 F13 123.0(6) 3_566 . ? F14 P3 F13 90.0(5) . . ? F14 P3 F13 90.0(5) 3_566 . ? F13 P3 F13 179.996(2) 3_566 . ? F13B P3 F15 72.6(6) . 3_566 ? F13B P3 F15 107.4(6) 3_566 3_566 ? F15B P3 F15 127.8(7) . 3_566 ? F15B P3 F15 52.2(7) 3_566 3_566 ? F14 P3 F15 92.2(5) . 3_566 ? F14 P3 F15 87.8(5) 3_566 3_566 ? F13 P3 F15 91.9(5) 3_566 3_566 ? F13 P3 F15 88.1(5) . 3_566 ? F13B P3 F15 107.4(6) . . ? F13B P3 F15 72.6(6) 3_566 . ? F15B P3 F15 52.2(7) . . ? F15B P3 F15 127.8(7) 3_566 . ? F14 P3 F15 87.8(5) . . ? F14 P3 F15 92.2(5) 3_566 . ? F13 P3 F15 88.1(5) 3_566 . ? F13 P3 F15 91.9(5) . . ? F15 P3 F15 180.0(4) 3_566 . ? F13B P3 F14B 92.2(8) . 3_566 ? F13B P3 F14B 87.8(8) 3_566 3_566 ? F15B P3 F14B 91.4(8) . 3_566 ? F15B P3 F14B 88.7(8) 3_566 3_566 ? F14 P3 F14B 133.4(6) . 3_566 ? F14 P3 F14B 46.6(6) 3_566 3_566 ? F13 P3 F14B 98.2(6) 3_566 3_566 ? F13 P3 F14B 81.8(6) . 3_566 ? F15 P3 F14B 42.1(5) 3_566 3_566 ? F15 P3 F14B 137.9(5) . 3_566 ? F13B P3 F14B 87.8(8) . . ? F13B P3 F14B 92.2(8) 3_566 . ? F15B P3 F14B 88.7(8) . . ? F15B P3 F14B 91.3(8) 3_566 . ? F14 P3 F14B 46.6(6) . . ? F14 P3 F14B 133.4(6) 3_566 . ? F13 P3 F14B 81.8(6) 3_566 . ? F13 P3 F14B 98.2(6) . . ? F15 P3 F14B 137.9(5) 3_566 . ? F15 P3 F14B 42.1(5) . . ? F14B P3 F14B 179.999(4) 3_566 . ? C32 O1 C43 116.6(5) . . ? C45 O2 C44 111.2(5) . . ? C47 O3 C46 113.7(5) . . ? C48A O4A C49A 110.1(9) . . ? C48B O4B C49B 117.6(19) . . ? C37 O5 C38B 126.2(7) . . ? C37 O5 C38A 106.6(7) . . ? C38B O5 C38A 25.4(5) . . ? C39A O6 C40 125.6(7) . . ? C39A O6 C39B 44.0(7) . . ? C40 O6 C39B 115.5(7) . . ? C41A O7 C42 121.1(8) . . ? C41A O7 C41B 25.8(11) . . ? C42 O7 C41B 106.6(8) . . ? C51 O8 C53 101.3(11) . . ? C4 N1 C3 111.2(6) . . ? C4 N1 C1 108.1(5) . . ? C3 N1 C1 109.0(5) . . ? C4 N1 Pd1 111.3(4) . . ? C3 N1 Pd1 112.0(4) . . ? C1 N1 Pd1 104.9(4) . . ? C6 N2 C2 114.4(5) . . ? C6 N2 C5 105.3(5) . . ? C2 N2 C5 105.6(5) . . ? C6 N2 Pd1 111.1(4) . . ? C2 N2 Pd1 105.9(4) . . ? C5 N2 Pd1 114.5(4) . . ? C11 N3 C7 118.1(4) . . ? C11 N3 Pd1 119.4(3) . . ? C7 N3 Pd1 121.8(3) . . ? C14 N4 C15 120.7(5) . . ? C14 N4 C17 120.7(4) . . ? C15 N4 C17 118.5(4) . . ? C26 N6 C25 121.3(4) 3_666 3_666 ? C26 N6 C17 120.1(4) 3_666 . ? C25 N6 C17 118.6(4) 3_666 . ? C18 N5 C22 118.6(4) . . ? C18 N5 Pd1 119.4(3) . . ? C22 N5 Pd1 121.8(3) . . ? C2 C1 N1 111.4(5) . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? N1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 107.4(6) . . ? N2 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? N2 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 122.7(5) . . ? N3 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C7 C8 C9 119.9(5) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C8 C9 C10 117.5(5) . . ? C8 C9 C12 121.7(4) . . ? C10 C9 C12 120.8(4) . . ? C11 C10 C9 119.5(5) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? N3 C11 C10 122.4(5) . . ? N3 C11 H11 118.8 . . ? C10 C11 H11 118.8 . . ? C16 C12 C13 117.8(5) . . ? C16 C12 C9 121.1(4) . . ? C13 C12 C9 121.1(4) . . ? C14 C13 C12 119.2(5) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? N4 C14 C13 121.7(5) . . ? N4 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? N4 C15 C16 120.0(5) . . ? N4 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C12 120.6(5) . . ? C15 C16 H16 119.7 . . ? C12 C16 H16 119.7 . . ? N4 C17 N6 110.5(4) . . ? N4 C17 H17A 109.5 . . ? N6 C17 H17A 109.5 . . ? N4 C17 H17B 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? N5 C18 C19 122.9(4) . . ? N5 C18 H18 118.5 . . ? C19 C18 H18 118.5 . . ? C20 C19 C18 119.0(4) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 117.8(4) . . ? C19 C20 C23 120.6(4) . . ? C21 C20 C23 121.7(4) . . ? C22 C21 C20 119.7(4) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? N5 C22 C21 122.0(4) . . ? N5 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C24 C23 C27 117.9(5) . . ? C24 C23 C20 121.3(4) . . ? C27 C23 C20 120.9(4) . . ? C25 C24 C23 120.7(5) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? N6 C25 C24 119.7(5) 3_666 . ? N6 C25 H25 120.1 3_666 . ? C24 C25 H25 120.1 . . ? N6 C26 C27 120.8(4) 3_666 . ? N6 C26 H26 119.6 3_666 . ? C27 C26 H26 119.6 . . ? C26 C27 C23 119.6(5) . . ? C26 C27 H27 120.2 . . ? C23 C27 H27 120.2 . . ? C33 C28 C29 120.8(4) . . ? C33 C28 C37 118.5(5) . . ? C29 C28 C37 120.7(5) . . ? C30 C29 C28 119.0(5) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C31 121.6(5) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C32 C31 C30 120.1(5) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? O1 C32 C31 125.3(5) . . ? O1 C32 C33 114.6(5) . . ? C31 C32 C33 120.1(5) . . ? C28 C33 C34 119.9(5) . . ? C28 C33 C32 118.3(5) . . ? C34 C33 C32 121.8(5) . . ? C35 C34 C33 119.8(6) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 121.7(6) . . ? C34 C35 H35 119.1 . . ? C36 C35 H35 119.1 . . ? C37 C36 C35 119.6(5) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? O5 C37 C36 124.8(5) . . ? O5 C37 C28 114.8(5) . . ? C36 C37 C28 120.4(5) . . ? C39A C38A O5 101.4(10) . . ? C39A C38A H38A 111.5 . . ? O5 C38A H38A 111.5 . . ? C39A C38A H38B 111.5 . . ? O5 C38A H38B 111.5 . . ? H38A C38A H38B 109.3 . . ? O6 C39A C38A 109.4(10) . . ? O6 C39A H39A 109.8 . . ? C38A C39A H39A 109.8 . . ? O6 C39A H39B 109.8 . . ? C38A C39A H39B 109.8 . . ? H39A C39A H39B 108.3 . . ? O5 C38B C39B 110.0(10) . . ? O5 C38B H38C 109.7 . . ? C39B C38B H38C 109.7 . . ? O5 C38B H38D 109.7 . . ? C39B C38B H38D 109.7 . . ? H38C C38B H38D 108.2 . . ? O6 C39B C38B 107.1(9) . . ? O6 C39B H39C 110.3 . . ? C38B C39B H39C 110.3 . . ? O6 C39B H39D 110.3 . . ? C38B C39B H39D 110.3 . . ? H39C C39B H39D 108.6 . . ? C41B C40 O6 128.9(11) . . ? C41B C40 C41A 26.9(12) . . ? O6 C40 C41A 109.8(7) . . ? C41B C40 H40A 111.8 . . ? O6 C40 H40A 109.7 . . ? C41A C40 H40A 109.7 . . ? C41B C40 H40B 84.1 . . ? O6 C40 H40B 109.7 . . ? C41A C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? O7 C41A C40 117.8(12) . . ? O7 C41A H41A 107.9 . . ? C40 C41A H41A 107.9 . . ? O7 C41A H41B 107.9 . . ? C40 C41A H41B 107.9 . . ? H41A C41A H41B 107.2 . . ? C40 C41B O7 115.9(13) . . ? C40 C41B H41C 108.3 . . ? O7 C41B H41C 108.3 . . ? C40 C41B H41D 108.3 . . ? O7 C41B H41D 108.3 . . ? H41C C41B H41D 107.4 . . ? C49B C42 O7 118.7(13) 3_666 . ? C49B C42 C49A 17(2) 3_666 3_666 ? O7 C42 C49A 111.3(11) . 3_666 ? C49B C42 H42A 92.6 3_666 . ? O7 C42 H42A 109.4 . . ? C49A C42 H42A 109.4 3_666 . ? C49B C42 H42B 116.9 3_666 . ? O7 C42 H42B 109.4 . . ? C49A C42 H42B 109.4 3_666 . ? H42A C42 H42B 108.0 . . ? O1 C43 C44 107.6(6) . . ? O1 C43 H43A 110.2 . . ? C44 C43 H43A 110.2 . . ? O1 C43 H43B 110.2 . . ? C44 C43 H43B 110.2 . . ? H43A C43 H43B 108.5 . . ? O2 C44 C43 109.0(5) . . ? O2 C44 H44A 109.9 . . ? C43 C44 H44A 109.9 . . ? O2 C44 H44B 109.9 . . ? C43 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? O2 C45 C46 110.0(6) . . ? O2 C45 H45A 109.7 . . ? C46 C45 H45A 109.7 . . ? O2 C45 H45B 109.7 . . ? C46 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? O3 C46 C45 109.3(6) . . ? O3 C46 H46A 109.8 . . ? C45 C46 H46A 109.8 . . ? O3 C46 H46B 109.8 . . ? C45 C46 H46B 109.8 . . ? H46A C46 H46B 108.3 . . ? O3 C47 C48B 116.9(10) . . ? O3 C47 C48A 113.7(7) . . ? C48B C47 C48A 44.3(13) . . ? O3 C47 H47A 108.8 . . ? C48B C47 H47A 66.2 . . ? C48A C47 H47A 108.8 . . ? O3 C47 H47B 108.8 . . ? C48B C47 H47B 133.4 . . ? C48A C47 H47B 108.8 . . ? H47A C47 H47B 107.7 . . ? O4A C48A C47 111.6(7) . . ? O4A C48A H48A 109.3 . . ? C47 C48A H48A 109.3 . . ? O4A C48A H48B 109.3 . . ? C47 C48A H48B 109.3 . . ? H48A C48A H48B 108.0 . . ? O4A C49A C42 106.7(12) . 3_666 ? O4A C49A H49A 110.4 . . ? C42 C49A H49A 110.4 3_666 . ? O4A C49A H49B 110.4 . . ? C42 C49A H49B 110.4 3_666 . ? H49A C49A H49B 108.6 . . ? C47 C48B O4B 141.9(19) . . ? C47 C48B H48C 101.5 . . ? O4B C48B H48C 101.5 . . ? C47 C48B H48D 101.5 . . ? O4B C48B H48D 101.5 . . ? H48C C48B H48D 104.6 . . ? C42 C49B O4B 107.5(18) 3_666 . ? C42 C49B H49C 110.2 3_666 . ? O4B C49B H49C 110.2 . . ? C42 C49B H49D 110.2 3_666 . ? O4B C49B H49D 110.2 . . ? H49C C49B H49D 108.5 . . ? O8 C51 C50 138.5(11) . . ? O8 C51 H51A 102.5 . . ? C50 C51 H51A 102.5 . . ? O8 C51 H51B 102.5 . . ? C50 C51 H51B 102.5 . . ? H51A C51 H51B 104.9 . . ? C52 C53 O8 115.3(15) . . ? C52 C53 H53A 108.5 . . ? O8 C53 H53A 108.5 . . ? C52 C53 H53B 108.5 . . ? O8 C53 H53B 108.5 . . ? H53A C53 H53B 107.5 . . ? N7 C54 C55 179.1(10) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N8 C56 C57 176.3(11) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N9 C58 C59 175.7(11) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? F16 P4 F18 84.5(10) . . ? F16 P4 F19 171.9(14) . . ? F18 P4 F19 91.0(11) . . ? F16 P4 F17 99.9(11) . . ? F18 P4 F17 88.7(10) . . ? F19 P4 F17 86.7(11) . . ? F16 P4 F20 95.5(10) . . ? F18 P4 F20 178.8(12) . . ? F19 P4 F20 89.2(11) . . ? F17 P4 F20 90.1(10) . . ? F16 P4 F21 82.4(10) . . ? F18 P4 F21 91.1(10) . . ? F19 P4 F21 91.0(11) . . ? F17 P4 F21 177.7(12) . . ? F20 P4 F21 90.1(10) . . ? F19A P4A F17A 85.2(12) . . ? F19A P4A F16A 170.5(16) . . ? F17A P4A F16A 102.5(13) . . ? F19A P4A F18A 92.5(13) . . ? F17A P4A F18A 86.7(12) . . ? F16A P4A F18A 82.6(11) . . ? F19A P4A F21A 90.5(13) . . ? F17A P4A F21A 175.6(13) . . ? F16A P4A F21A 81.9(11) . . ? F18A P4A F21A 93.8(12) . . ? F19A P4A F20A 92.1(13) . . ? F17A P4A F20A 96.4(12) . . ? F16A P4A F20A 92.5(11) . . ? F18A P4A F20A 174.7(12) . . ? F21A P4A F20A 83.5(11) . . ? F21A F19A P4A 120(2) 3_765 . ? F19A F21A P4A 147.8(19) 3_765 . ? F26 P5 F25 87.3(6) . . ? F26 P5 F27 93.8(6) . . ? F25 P5 F27 178.9(5) . . ? F26 P5 F22 91.1(5) . . ? F25 P5 F22 90.2(5) . . ? F27 P5 F22 89.7(5) . . ? F26 P5 F24 89.7(5) . . ? F25 P5 F24 87.8(4) . . ? F27 P5 F24 92.3(4) . . ? F22 P5 F24 177.8(5) . . ? F26 P5 F23 176.4(6) . . ? F25 P5 F23 89.6(4) . . ? F27 P5 F23 89.3(5) . . ? F22 P5 F23 90.5(3) . . ? F24 P5 F23 88.5(4) . . ? F25A P5A F24A 94.0(10) . . ? F25A P5A F23A 88.1(9) . . ? F24A P5A F23A 90.6(7) . . ? F25A P5A F22A 172.3(11) . . ? F24A P5A F22A 93.7(8) . . ? F23A P5A F22A 93.2(8) . . ? F25A P5A F26A 91.0(9) . . ? F24A P5A F26A 91.8(9) . . ? F23A P5A F26A 177.5(9) . . ? F22A P5A F26A 87.3(8) . . ? F25A P5A F27A 94.5(11) . . ? F24A P5A F27A 171.2(10) . . ? F23A P5A F27A 87.4(9) . . ? F22A P5A F27A 77.9(9) . . ? F26A P5A F27A 90.3(11) . . ? C60 C61 N10 130(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Pd1 N1 C4 -146(9) . . . . ? N3 Pd1 N1 C4 69.1(5) . . . . ? N2 Pd1 N1 C4 -106.7(5) . . . . ? N5 Pd1 N1 C3 89(10) . . . . ? N3 Pd1 N1 C3 -56.1(4) . . . . ? N2 Pd1 N1 C3 128.1(5) . . . . ? N5 Pd1 N1 C1 -29(10) . . . . ? N3 Pd1 N1 C1 -174.1(4) . . . . ? N2 Pd1 N1 C1 10.0(4) . . . . ? N5 Pd1 N2 C6 72.6(4) . . . . ? N3 Pd1 N2 C6 143(2) . . . . ? N1 Pd1 N2 C6 -106.6(5) . . . . ? N5 Pd1 N2 C2 -162.5(5) . . . . ? N3 Pd1 N2 C2 -92(2) . . . . ? N1 Pd1 N2 C2 18.2(5) . . . . ? N5 Pd1 N2 C5 -46.5(4) . . . . ? N3 Pd1 N2 C5 24(2) . . . . ? N1 Pd1 N2 C5 134.2(4) . . . . ? N5 Pd1 N3 C11 94.5(4) . . . . ? N1 Pd1 N3 C11 -86.2(4) . . . . ? N2 Pd1 N3 C11 24(2) . . . . ? N5 Pd1 N3 C7 -75.9(4) . . . . ? N1 Pd1 N3 C7 103.4(4) . . . . ? N2 Pd1 N3 C7 -147(2) . . . . ? N3 Pd1 N5 C18 -85.0(4) . . . . ? N1 Pd1 N5 C18 130(10) . . . . ? N2 Pd1 N5 C18 90.8(4) . . . . ? N3 Pd1 N5 C22 88.7(4) . . . . ? N1 Pd1 N5 C22 -57(10) . . . . ? N2 Pd1 N5 C22 -95.4(4) . . . . ? C4 N1 C1 C2 81.2(7) . . . . ? C3 N1 C1 C2 -157.8(6) . . . . ? Pd1 N1 C1 C2 -37.7(6) . . . . ? C6 N2 C2 C1 79.9(7) . . . . ? C5 N2 C2 C1 -164.7(6) . . . . ? Pd1 N2 C2 C1 -42.9(7) . . . . ? N1 C1 C2 N2 55.6(8) . . . . ? C11 N3 C7 C8 -1.4(7) . . . . ? Pd1 N3 C7 C8 169.1(4) . . . . ? N3 C7 C8 C9 0.8(8) . . . . ? C7 C8 C9 C10 0.4(7) . . . . ? C7 C8 C9 C12 -179.0(4) . . . . ? C8 C9 C10 C11 -0.9(7) . . . . ? C12 C9 C10 C11 178.5(4) . . . . ? C7 N3 C11 C10 0.9(7) . . . . ? Pd1 N3 C11 C10 -169.9(4) . . . . ? C9 C10 C11 N3 0.3(8) . . . . ? C8 C9 C12 C16 166.3(4) . . . . ? C10 C9 C12 C16 -13.0(7) . . . . ? C8 C9 C12 C13 -14.7(7) . . . . ? C10 C9 C12 C13 165.9(5) . . . . ? C16 C12 C13 C14 1.4(7) . . . . ? C9 C12 C13 C14 -177.6(4) . . . . ? C15 N4 C14 C13 0.3(7) . . . . ? C17 N4 C14 C13 177.2(4) . . . . ? C12 C13 C14 N4 -1.0(7) . . . . ? C14 N4 C15 C16 0.1(7) . . . . ? C17 N4 C15 C16 -176.9(4) . . . . ? N4 C15 C16 C12 0.3(7) . . . . ? C13 C12 C16 C15 -1.1(7) . . . . ? C9 C12 C16 C15 177.9(4) . . . . ? C14 N4 C17 N6 97.0(5) . . . . ? C15 N4 C17 N6 -86.1(5) . . . . ? C26 N6 C17 N4 90.2(6) 3_666 . . . ? C25 N6 C17 N4 -89.9(6) 3_666 . . . ? C22 N5 C18 C19 -1.3(8) . . . . ? Pd1 N5 C18 C19 172.7(4) . . . . ? N5 C18 C19 C20 -0.2(8) . . . . ? C18 C19 C20 C21 1.8(8) . . . . ? C18 C19 C20 C23 -177.4(5) . . . . ? C19 C20 C21 C22 -1.9(8) . . . . ? C23 C20 C21 C22 177.3(5) . . . . ? C18 N5 C22 C21 1.2(8) . . . . ? Pd1 N5 C22 C21 -172.6(4) . . . . ? C20 C21 C22 N5 0.4(8) . . . . ? C19 C20 C23 C24 -5.4(7) . . . . ? C21 C20 C23 C24 175.4(5) . . . . ? C19 C20 C23 C27 173.2(5) . . . . ? C21 C20 C23 C27 -6.0(7) . . . . ? C27 C23 C24 C25 0.3(9) . . . . ? C20 C23 C24 C25 178.9(5) . . . . ? C23 C24 C25 N6 -0.8(10) . . . 3_666 ? N6 C26 C27 C23 1.0(10) 3_666 . . . ? C24 C23 C27 C26 -0.4(9) . . . . ? C20 C23 C27 C26 -179.0(5) . . . . ? C33 C28 C29 C30 -2.1(7) . . . . ? C37 C28 C29 C30 178.2(4) . . . . ? C28 C29 C30 C31 0.0(7) . . . . ? C29 C30 C31 C32 1.5(8) . . . . ? C43 O1 C32 C31 7.2(7) . . . . ? C43 O1 C32 C33 -173.8(4) . . . . ? C30 C31 C32 O1 178.0(5) . . . . ? C30 C31 C32 C33 -0.9(7) . . . . ? C29 C28 C33 C34 -178.7(4) . . . . ? C37 C28 C33 C34 1.0(6) . . . . ? C29 C28 C33 C32 2.7(6) . . . . ? C37 C28 C33 C32 -177.6(4) . . . . ? O1 C32 C33 C28 179.8(4) . . . . ? C31 C32 C33 C28 -1.2(7) . . . . ? O1 C32 C33 C34 1.2(7) . . . . ? C31 C32 C33 C34 -179.8(5) . . . . ? C28 C33 C34 C35 -0.2(7) . . . . ? C32 C33 C34 C35 178.3(5) . . . . ? C33 C34 C35 C36 -0.3(8) . . . . ? C34 C35 C36 C37 0.0(8) . . . . ? C38B O5 C37 C36 -15.2(10) . . . . ? C38A O5 C37 C36 3.1(9) . . . . ? C38B O5 C37 C28 166.3(8) . . . . ? C38A O5 C37 C28 -175.3(7) . . . . ? C35 C36 C37 O5 -177.6(5) . . . . ? C35 C36 C37 C28 0.8(7) . . . . ? C33 C28 C37 O5 177.2(4) . . . . ? C29 C28 C37 O5 -3.1(6) . . . . ? C33 C28 C37 C36 -1.3(7) . . . . ? C29 C28 C37 C36 178.4(4) . . . . ? C37 O5 C38A C39A 166.4(8) . . . . ? C38B O5 C38A C39A -50(2) . . . . ? C40 O6 C39A C38A -129.9(11) . . . . ? C39B O6 C39A C38A -38.7(10) . . . . ? O5 C38A C39A O6 -79.4(12) . . . . ? C37 O5 C38B C39B 90.3(11) . . . . ? C38A O5 C38B C39B 46(2) . . . . ? C39A O6 C39B C38B 37.6(9) . . . . ? C40 O6 C39B C38B 153.4(9) . . . . ? O5 C38B C39B O6 68.5(12) . . . . ? C39A O6 C40 C41B -147(2) . . . . ? C39B O6 C40 C41B 162(2) . . . . ? C39A O6 C40 C41A -169.5(11) . . . . ? C39B O6 C40 C41A 140.2(11) . . . . ? C42 O7 C41A C40 115.2(11) . . . . ? C41B O7 C41A C40 54(2) . . . . ? C41B C40 C41A O7 -86(3) . . . . ? O6 C40 C41A O7 53.6(16) . . . . ? O6 C40 C41B O7 0(3) . . . . ? C41A C40 C41B O7 51(2) . . . . ? C41A O7 C41B C40 -83(3) . . . . ? C42 O7 C41B C40 148.7(19) . . . . ? C41A O7 C42 C49B -88.7(19) . . . 3_666 ? C41B O7 C42 C49B -65(2) . . . 3_666 ? C41A O7 C42 C49A -72.0(13) . . . 3_666 ? C41B O7 C42 C49A -48.6(14) . . . 3_666 ? C32 O1 C43 C44 -179.7(5) . . . . ? C45 O2 C44 C43 164.9(6) . . . . ? O1 C43 C44 O2 75.5(7) . . . . ? C44 O2 C45 C46 -177.2(6) . . . . ? C47 O3 C46 C45 -136.7(7) . . . . ? O2 C45 C46 O3 -66.0(9) . . . . ? C46 O3 C47 C48B -122.3(15) . . . . ? C46 O3 C47 C48A -73.1(9) . . . . ? C49A O4A C48A C47 179.6(13) . . . . ? O3 C47 C48A O4A -69.6(9) . . . . ? C48B C47 C48A O4A 35.4(13) . . . . ? C48A O4A C49A C42 -177.5(11) . . . 3_666 ? O3 C47 C48B O4B 11(4) . . . . ? C48A C47 C48B O4B -87(4) . . . . ? C49B O4B C48B C47 118(3) . . . . ? C48B O4B C49B C42 -175(2) . . . 3_666 ? C53 O8 C51 C50 -53.7(18) . . . . ? C51 O8 C53 C52 169(2) . . . . ? F17A P4A F19A F21A 169(3) . . . 3_765 ? F16A P4A F19A F21A 24(10) . . . 3_765 ? F18A P4A F19A F21A 82(2) . . . 3_765 ? F21A P4A F19A F21A -12(3) . . . 3_765 ? F20A P4A F19A F21A -95(3) . . . 3_765 ? F19A P4A F21A F19A 19(5) . . . 3_765 ? F17A P4A F21A F19A 22(21) . . . 3_765 ? F16A P4A F21A F19A -155(4) . . . 3_765 ? F18A P4A F21A F19A -73(4) . . . 3_765 ? F20A P4A F21A F19A 111(4) . . . 3_765 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.036 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.123