# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Martin Broring' 'Carsten D. Brandt' _publ_contact_author_name 'Prof Martin Broring' _publ_contact_author_address ; Fachbereich Chemie Philipps-Universitat Marburg Hans-Meerwein-Strasse Marburg D-35032 GERMANY ; _publ_contact_author_phone '049 6421 282 5418' _publ_contact_author_fax ? _publ_contact_author_email Martin.Broering@chemie.uni-marburg.de _publ_requested_journal 'Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in "Chem. Commun." ; _publ_section_title ; A five coordinate PdII complex stable in solution and in the solid state ; _publ_section_abstract ; The treatment of the strained complex TrpyPdOAcF 1 with NaBArF, followed by the addition of trimethylphosphane, yields the stable cationic 16VE- or 18VE-complexes 3 and 4, depending on the amount of phosphine added. ; data_bispme3 _database_code_CSD 195925 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H68 B F24 N3 P2 Pd' _chemical_formula_weight 1538.38 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' B B 0.0013 0.0007 '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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.5341(11) _cell_length_b 15.1714(11) _cell_length_c 17.1442(12) _cell_angle_alpha 95.9710(10) _cell_angle_beta 97.2310(10) _cell_angle_gamma 105.8260(10) _cell_volume 3570.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7929 _cell_measurement_theta_min 5.558 _cell_measurement_theta_max 56.316 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1564 _exptl_absorpt_coefficient_mu 0.408 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS2.0 (Sheldrick 2000)' _exptl_special_details ; 6 CF3-groups of the B(ArF)4-anion are rotational disordered and could be refined anisotropically with an occupancy of 72.7450:27.2550, 66.3300:33.6700, 51.8860:48.1140, 70.2960:29.7040, 67.7160:32.2840 and 63.4390:36.5610, respectively. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex with D8-Goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67837 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 26.37 _reflns_number_total 14572 _reflns_number_gt 13891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.6' _computing_cell_refinement 'SAINT-NT V6.0' _computing_data_reduction 'SAINT-NT V6.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material 'XSHELL in SHELXTL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+2.6821P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14572 _refine_ls_number_parameters 1056 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _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 B1 B 0.50496(19) 0.22857(18) 0.82508(15) 0.0315(5) Uani 1 1 d . . . C1 C 1.0357(2) 0.69053(19) 0.87117(15) 0.0421(6) Uani 1 1 d . . . H1A H 1.0814 0.7412 0.9088 0.063 Uiso 1 1 calc R . . H1B H 1.0326 0.6316 0.8908 0.063 Uiso 1 1 calc R . . H1C H 0.9713 0.7001 0.8657 0.063 Uiso 1 1 calc R . . C2 C 1.06867(17) 0.68858(16) 0.79264(14) 0.0347(5) Uani 1 1 d . . . C3 C 1.14536(18) 0.65218(17) 0.77099(16) 0.0384(5) Uani 1 1 d . . . C4 C 1.15236(17) 0.66574(16) 0.69427(16) 0.0357(5) Uani 1 1 d . . . C5 C 1.08214(17) 0.71305(16) 0.66905(14) 0.0326(5) Uani 1 1 d . . . C6 C 1.07296(17) 0.74427(17) 0.59681(14) 0.0343(5) Uani 1 1 d . . . H6 H 1.1170 0.7323 0.5635 0.041 Uiso 1 1 calc R . . C7 C 1.00922(17) 0.79106(17) 0.56374(14) 0.0339(5) Uani 1 1 d . . . C8 C 1.00261(17) 0.82255(18) 0.48738(14) 0.0353(5) Uani 1 1 d . . . C9 C 0.92746(17) 0.86122(17) 0.48254(14) 0.0339(5) Uani 1 1 d . . . C10 C 0.88962(17) 0.85166(17) 0.55616(13) 0.0333(5) Uani 1 1 d . . . C11 C 0.80872(17) 0.87581(17) 0.57918(13) 0.0329(5) Uani 1 1 d . . . H11 H 0.7794 0.9073 0.5429 0.039 Uiso 1 1 calc R . . C12 C 0.76528(17) 0.86146(16) 0.64531(13) 0.0316(5) Uani 1 1 d . . . C13 C 0.67856(17) 0.88583(17) 0.65916(14) 0.0342(5) Uani 1 1 d . . . C14 C 0.65602(17) 0.85810(17) 0.72899(14) 0.0343(5) Uani 1 1 d . . . C15 C 0.72925(16) 0.81851(16) 0.76019(13) 0.0316(5) Uani 1 1 d . . . C16 C 0.73608(19) 0.7828(2) 0.83778(15) 0.0416(6) Uani 1 1 d . . . H16A H 0.7916 0.7578 0.8443 0.062 Uiso 1 1 calc R . . H16B H 0.6765 0.7338 0.8390 0.062 Uiso 1 1 calc R . . H16C H 0.7446 0.8334 0.8810 0.062 Uiso 1 1 calc R . . C17 C 1.2017(2) 0.6054(2) 0.82408(19) 0.0515(7) Uani 1 1 d . . . H17A H 1.2065 0.6327 0.8800 0.062 Uiso 1 1 calc R . . H17B H 1.2682 0.6179 0.8115 0.062 Uiso 1 1 calc R . . C18 C 1.1564(3) 0.5017(2) 0.8157(2) 0.0714(10) Uani 1 1 d . . . H18A H 1.0903 0.4887 0.8278 0.107 Uiso 1 1 calc R . . H18B H 1.1951 0.4755 0.8527 0.107 Uiso 1 1 calc R . . H18C H 1.1546 0.4737 0.7612 0.107 Uiso 1 1 calc R . . C19 C 1.21486(19) 0.63262(19) 0.64140(18) 0.0448(6) Uani 1 1 d . . . H19A H 1.2676 0.6175 0.6747 0.054 Uiso 1 1 calc R . . H19B H 1.2449 0.6832 0.6123 0.054 Uiso 1 1 calc R . . C20 C 1.1582(2) 0.5480(2) 0.5820(2) 0.0588(8) Uani 1 1 d . . . H20A H 1.1302 0.4970 0.6106 0.088 Uiso 1 1 calc R . . H20B H 1.2016 0.5296 0.5485 0.088 Uiso 1 1 calc R . . H20C H 1.1061 0.5627 0.5487 0.088 Uiso 1 1 calc R . . C21 C 1.0663(2) 0.8125(2) 0.42598(16) 0.0509(7) Uani 1 1 d . . . H21A H 1.1329 0.8208 0.4534 0.061 Uiso 1 1 calc R . . H21B H 1.0690 0.8621 0.3924 0.061 Uiso 1 1 calc R . . C22 C 1.0308(3) 0.7192(4) 0.3731(3) 0.0989(16) Uani 1 1 d . . . H22A H 1.0281 0.6697 0.4060 0.148 Uiso 1 1 calc R . . H22B H 1.0755 0.7161 0.3353 0.148 Uiso 1 1 calc R . . H22C H 0.9660 0.7116 0.3440 0.148 Uiso 1 1 calc R . . C23 C 0.8885(2) 0.9041(2) 0.41581(16) 0.0483(7) Uani 1 1 d . . . H23A H 0.9401 0.9252 0.3836 0.058 Uiso 1 1 calc R . . H23B H 0.8718 0.9594 0.4385 0.058 Uiso 1 1 calc R . . C24 C 0.8000(3) 0.8396(3) 0.3619(2) 0.0757(11) Uani 1 1 d . . . H24A H 0.8162 0.7855 0.3379 0.114 Uiso 1 1 calc R . . H24B H 0.7785 0.8722 0.3199 0.114 Uiso 1 1 calc R . . H24C H 0.7479 0.8195 0.3930 0.114 Uiso 1 1 calc R . . C25 C 0.62575(19) 0.9361(2) 0.60680(16) 0.0435(6) Uani 1 1 d . . . H25A H 0.5557 0.9146 0.6095 0.052 Uiso 1 1 calc R . . H25B H 0.6342 0.9210 0.5511 0.052 Uiso 1 1 calc R . . C26 C 0.6627(3) 1.0407(2) 0.6315(2) 0.0637(9) Uani 1 1 d . . . H26A H 0.6546 1.0559 0.6867 0.096 Uiso 1 1 calc R . . H26B H 0.6257 1.0708 0.5969 0.096 Uiso 1 1 calc R . . H26C H 0.7314 1.0625 0.6268 0.096 Uiso 1 1 calc R . . C27 C 0.56706(18) 0.8583(2) 0.76536(17) 0.0439(6) Uani 1 1 d . . . H27A H 0.5469 0.9137 0.7544 0.053 Uiso 1 1 calc R . . H27B H 0.5821 0.8614 0.8237 0.053 Uiso 1 1 calc R . . C28 C 0.4841(2) 0.7707(2) 0.7312(2) 0.0535(7) Uani 1 1 d . . . H28A H 0.4619 0.7730 0.6753 0.080 Uiso 1 1 calc R . . H28B H 0.4304 0.7671 0.7612 0.080 Uiso 1 1 calc R . . H28C H 0.5071 0.7161 0.7354 0.080 Uiso 1 1 calc R . . C29 C 0.7131(3) 0.5716(3) 0.7256(3) 0.0840(13) Uani 1 1 d . . . H29A H 0.6791 0.5085 0.6992 0.126 Uiso 1 1 calc R . . H29B H 0.6679 0.6092 0.7245 0.126 Uiso 1 1 calc R . . H29C H 0.7387 0.5697 0.7809 0.126 Uiso 1 1 calc R . . C30 C 0.7503(4) 0.6184(3) 0.5757(2) 0.0960(16) Uani 1 1 d . . . H30A H 0.7983 0.6403 0.5413 0.144 Uiso 1 1 calc R . . H30B H 0.7075 0.6582 0.5774 0.144 Uiso 1 1 calc R . . H30C H 0.7119 0.5546 0.5546 0.144 Uiso 1 1 calc R . . C31 C 0.8720(3) 0.5327(2) 0.6642(3) 0.0730(11) Uani 1 1 d . . . H31A H 0.8242 0.4736 0.6407 0.109 Uiso 1 1 calc R . . H31B H 0.9035 0.5266 0.7165 0.109 Uiso 1 1 calc R . . H31C H 0.9208 0.5493 0.6295 0.109 Uiso 1 1 calc R . . C32 C 1.1283(2) 0.9400(2) 0.7972(3) 0.0779(12) Uani 1 1 d . . . H32A H 1.1412 0.9353 0.7424 0.117 Uiso 1 1 calc R . . H32B H 1.1531 0.8958 0.8249 0.117 Uiso 1 1 calc R . . H32C H 1.1606 1.0030 0.8247 0.117 Uiso 1 1 calc R . . C33 C 0.9865(3) 0.9386(2) 0.90014(16) 0.0548(8) Uani 1 1 d . . . H33A H 1.0289 1.0005 0.9229 0.082 Uiso 1 1 calc R . . H33B H 1.0046 0.8924 0.9299 0.082 Uiso 1 1 calc R . . H33C H 0.9191 0.9362 0.9034 0.082 Uiso 1 1 calc R . . C34 C 0.9677(2) 1.00805(18) 0.75405(17) 0.0489(7) Uani 1 1 d . . . H34A H 1.0112 1.0673 0.7819 0.073 Uiso 1 1 calc R . . H34B H 0.9006 1.0051 0.7595 0.073 Uiso 1 1 calc R . . H34C H 0.9740 1.0026 0.6976 0.073 Uiso 1 1 calc R . . C35 C 0.45004(16) 0.11747(16) 0.79975(13) 0.0301(5) Uani 1 1 d . . . C36 C 0.43447(17) 0.05963(16) 0.85872(14) 0.0328(5) Uani 1 1 d . . . H36 H 0.4580 0.0858 0.9128 0.039 Uiso 1 1 calc R . . C37 C 0.38605(16) -0.03418(17) 0.84087(14) 0.0322(5) Uani 1 1 d . . . C38 C 0.35048(15) -0.07539(16) 0.76238(14) 0.0307(5) Uani 1 1 d . . . H38 H 0.3166 -0.1395 0.7499 0.037 Uiso 1 1 calc R . . C39 C 0.36608(16) -0.02009(16) 0.70308(13) 0.0301(5) Uani 1 1 d . A . C40 C 0.41473(16) 0.07413(16) 0.72153(13) 0.0298(5) Uani 1 1 d . . . H40 H 0.4242 0.1101 0.6795 0.036 Uiso 1 1 calc R . . C41 C 0.3745(2) -0.09236(19) 0.90631(16) 0.0430(6) Uani 1 1 d . . . C42 C 0.32888(19) -0.06067(17) 0.61782(15) 0.0389(6) Uani 1 1 d . . . C43 C 0.50034(17) 0.28319(15) 0.74723(13) 0.0317(5) Uani 1 1 d . . . C44 C 0.55533(18) 0.26989(16) 0.68751(14) 0.0351(5) Uani 1 1 d . . . H44 H 0.5959 0.2307 0.6940 0.042 Uiso 1 1 calc R . . C45 C 0.5525(2) 0.31196(17) 0.61926(15) 0.0398(6) Uani 1 1 d . B . C46 C 0.4956(2) 0.37081(17) 0.60816(15) 0.0437(6) Uani 1 1 d . . . H46 H 0.4931 0.3993 0.5615 0.052 Uiso 1 1 calc R . . C47 C 0.4423(2) 0.38709(17) 0.66699(15) 0.0416(6) Uani 1 1 d . C . C48 C 0.44503(18) 0.34397(16) 0.73486(14) 0.0357(5) Uani 1 1 d . . . H48 H 0.4078 0.3565 0.7741 0.043 Uiso 1 1 calc R . . C49 C 0.6100(3) 0.2926(2) 0.55662(18) 0.0541(8) Uani 1 1 d . . . C50 C 0.3795(3) 0.4501(2) 0.65661(19) 0.0624(9) Uani 1 1 d . . . C51 C 0.44784(17) 0.26692(16) 0.89206(14) 0.0319(5) Uani 1 1 d . . . C52 C 0.34670(18) 0.24529(17) 0.87762(14) 0.0356(5) Uani 1 1 d . . . H52 H 0.3124 0.2064 0.8299 0.043 Uiso 1 1 calc R . . C53 C 0.29442(18) 0.27846(17) 0.93040(15) 0.0364(5) Uani 1 1 d . D . C54 C 0.34144(19) 0.33490(17) 1.00076(15) 0.0375(5) Uani 1 1 d . . . H54 H 0.3062 0.3583 1.0368 0.045 Uiso 1 1 calc R . . C55 C 0.44138(18) 0.35619(16) 1.01709(14) 0.0349(5) Uani 1 1 d . . . C56 C 0.49322(18) 0.32227(16) 0.96434(13) 0.0334(5) Uani 1 1 d . . . H56 H 0.5617 0.3372 0.9779 0.040 Uiso 1 1 calc R . . C57 C 0.1860(2) 0.2498(2) 0.91244(19) 0.0513(7) Uani 1 1 d . . . C58 C 0.4953(2) 0.4146(2) 1.09343(15) 0.0456(6) Uani 1 1 d . . . C59 C 0.62008(17) 0.24703(17) 0.85920(13) 0.0330(5) Uani 1 1 d . . . C60 C 0.68071(18) 0.33850(17) 0.87706(14) 0.0364(5) Uani 1 1 d . . . H60 H 0.6532 0.3878 0.8703 0.044 Uiso 1 1 calc R . . C61 C 0.77921(19) 0.35944(19) 0.90417(15) 0.0415(6) Uani 1 1 d . E . C62 C 0.82273(18) 0.2895(2) 0.91285(16) 0.0436(6) Uani 1 1 d . . . H62 H 0.8904 0.3037 0.9307 0.052 Uiso 1 1 calc R . . C63 C 0.76541(19) 0.19881(19) 0.89502(15) 0.0405(6) Uani 1 1 d . F . C64 C 0.66578(18) 0.17812(18) 0.86929(14) 0.0360(5) Uani 1 1 d . . . H64 H 0.6279 0.1151 0.8583 0.043 Uiso 1 1 calc R . . C65 C 0.8405(2) 0.4578(2) 0.9224(2) 0.0590(8) Uani 1 1 d . . . C66 C 0.8120(2) 0.1230(3) 0.9036(2) 0.0588(8) Uani 1 1 d . . . F1 F 0.37091(19) -0.04582(14) 0.97495(11) 0.0827(7) Uani 1 1 d . . . F2 F 0.45019(17) -0.12438(19) 0.92379(14) 0.0900(8) Uani 1 1 d . . . F3 F 0.29757(17) -0.16449(14) 0.89047(12) 0.0835(7) Uani 1 1 d . . . F4 F 0.3983(7) -0.0280(6) 0.5707(5) 0.0582(15) Uani 0.63(5) 1 d P A 1 F5 F 0.3113(10) -0.1509(5) 0.6024(6) 0.059(2) Uani 0.63(5) 1 d P A 1 F6 F 0.2533(13) -0.0388(15) 0.5854(8) 0.077(5) Uani 0.63(5) 1 d P A 1 F4' F 0.329(2) -0.1468(11) 0.6043(11) 0.075(5) Uani 0.37(5) 1 d P A 2 F5' F 0.362(3) -0.0130(16) 0.5687(7) 0.083(9) Uani 0.37(5) 1 d P A 2 F6' F 0.2300(10) -0.0693(13) 0.6064(13) 0.064(3) Uani 0.37(5) 1 d P A 2 F7 F 0.6985(3) 0.2889(6) 0.5877(3) 0.090(2) Uani 0.727(13) 1 d P B 1 F8 F 0.5723(4) 0.2113(4) 0.5151(4) 0.083(2) Uani 0.727(13) 1 d P B 1 F9 F 0.6271(8) 0.3540(6) 0.5086(5) 0.116(4) Uani 0.727(13) 1 d P B 1 F7' F 0.5514(10) 0.269(3) 0.4834(7) 0.137(10) Uani 0.273(13) 1 d P B 2 F8' F 0.6668(17) 0.3653(12) 0.5444(14) 0.114(10) Uani 0.273(13) 1 d P B 2 F9' F 0.648(3) 0.234(2) 0.5622(18) 0.199(17) Uani 0.273(13) 1 d P B 2 F10 F 0.3993(5) 0.5038(6) 0.6018(4) 0.082(2) Uani 0.663(17) 1 d P C 1 F11 F 0.2848(4) 0.4011(4) 0.6286(5) 0.089(2) Uani 0.663(17) 1 d P C 1 F12 F 0.3761(9) 0.5010(7) 0.7211(4) 0.108(4) Uani 0.663(17) 1 d P C 1 F10' F 0.3442(16) 0.4673(17) 0.7179(10) 0.106(7) Uani 0.337(17) 1 d P C 2 F11' F 0.4433(16) 0.5386(10) 0.657(2) 0.156(10) Uani 0.337(17) 1 d P C 2 F12' F 0.326(3) 0.433(2) 0.5980(12) 0.199(15) Uani 0.337(17) 1 d P C 2 F13 F 0.1480(12) 0.3123(10) 0.9401(12) 0.085(4) Uani 0.52(3) 1 d P D 1 F14 F 0.1498(10) 0.1722(11) 0.9427(15) 0.111(5) Uani 0.52(3) 1 d P D 1 F15 F 0.1499(9) 0.2301(15) 0.8369(6) 0.102(5) Uani 0.52(3) 1 d P D 1 F13' F 0.1455(9) 0.1635(7) 0.9126(15) 0.093(5) Uani 0.48(3) 1 d P D 2 F14' F 0.1542(11) 0.2645(19) 0.8420(10) 0.111(5) Uani 0.48(3) 1 d P D 2 F15' F 0.1451(12) 0.2899(18) 0.9644(17) 0.111(6) Uani 0.48(3) 1 d P D 2 F16 F 0.5268(2) 0.36507(16) 1.14352(12) 0.1086(10) Uani 1 1 d . . . F17 F 0.44321(17) 0.4565(2) 1.13145(15) 0.1230(12) Uani 1 1 d . . . F18 F 0.57282(15) 0.47885(14) 1.08502(11) 0.0734(6) Uani 1 1 d . . . F19 F 0.7962(6) 0.5208(6) 0.9126(7) 0.101(3) Uani 0.703(19) 1 d P E 1 F20 F 0.8849(8) 0.4799(6) 0.9973(4) 0.111(3) Uani 0.703(19) 1 d P E 1 F21 F 0.9114(6) 0.4765(3) 0.8803(7) 0.108(3) Uani 0.703(19) 1 d P E 1 F19' F 0.9180(12) 0.4724(13) 0.9661(18) 0.119(10) Uani 0.297(19) 1 d P E 2 F20' F 0.861(2) 0.4829(15) 0.8522(10) 0.178(11) Uani 0.297(19) 1 d P E 2 F21' F 0.7916(18) 0.5086(14) 0.948(3) 0.175(15) Uani 0.297(19) 1 d P E 2 F22 F 0.9033(3) 0.1441(3) 0.8923(6) 0.083(2) Uani 0.677(16) 1 d P F 1 F23 F 0.7673(6) 0.0448(6) 0.8597(7) 0.103(4) Uani 0.677(16) 1 d P F 1 F24 F 0.8211(5) 0.1045(5) 0.9794(3) 0.088(2) Uani 0.677(16) 1 d P F 1 F22' F 0.7479(14) 0.0416(12) 0.8903(17) 0.113(7) Uani 0.323(16) 1 d P F 2 F23' F 0.867(2) 0.1302(15) 0.9620(17) 0.190(13) Uani 0.323(16) 1 d P F 2 F24' F 0.858(3) 0.119(2) 0.8389(19) 0.179(11) Uani 0.323(16) 1 d P F 2 N1 N 1.03036(14) 0.72339(13) 0.73270(11) 0.0312(4) Uani 1 1 d . . . N2 N 0.94113(15) 0.81044(15) 0.60377(12) 0.0374(5) Uani 1 1 d . . . N3 N 0.79358(13) 0.81897(13) 0.71095(11) 0.0291(4) Uani 1 1 d . . . P1 P 0.81174(5) 0.62193(5) 0.67465(4) 0.03872(15) Uani 1 1 d . . . P2 P 0.99949(4) 0.91407(4) 0.79668(4) 0.03249(13) Uani 1 1 d . . . Pd1 Pd 0.911330(12) 0.770703(11) 0.725859(9) 0.02584(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0313(13) 0.0332(13) 0.0295(12) 0.0020(10) 0.0016(10) 0.0107(11) C1 0.0470(15) 0.0457(15) 0.0367(13) 0.0104(11) 0.0004(11) 0.0198(12) C2 0.0345(12) 0.0298(12) 0.0378(12) 0.0050(10) -0.0023(10) 0.0094(10) C3 0.0333(12) 0.0324(12) 0.0498(15) 0.0063(11) -0.0015(11) 0.0136(10) C4 0.0284(11) 0.0304(12) 0.0490(14) 0.0047(10) 0.0023(10) 0.0117(9) C5 0.0293(11) 0.0314(12) 0.0383(12) 0.0019(9) 0.0044(9) 0.0125(9) C6 0.0300(12) 0.0385(13) 0.0362(12) 0.0019(10) 0.0086(10) 0.0127(10) C7 0.0337(12) 0.0383(13) 0.0318(12) 0.0048(10) 0.0076(9) 0.0130(10) C8 0.0332(12) 0.0426(13) 0.0295(11) 0.0048(10) 0.0068(9) 0.0095(10) C9 0.0325(12) 0.0390(13) 0.0294(11) 0.0078(9) 0.0057(9) 0.0077(10) C10 0.0344(12) 0.0408(13) 0.0280(11) 0.0083(9) 0.0060(9) 0.0148(10) C11 0.0344(12) 0.0391(13) 0.0287(11) 0.0092(9) 0.0019(9) 0.0164(10) C12 0.0310(11) 0.0361(12) 0.0306(11) 0.0084(9) 0.0023(9) 0.0147(10) C13 0.0289(11) 0.0401(13) 0.0353(12) 0.0051(10) 0.0023(9) 0.0143(10) C14 0.0274(11) 0.0409(13) 0.0368(12) 0.0050(10) 0.0043(9) 0.0140(10) C15 0.0274(11) 0.0372(12) 0.0301(11) 0.0055(9) 0.0041(9) 0.0091(9) C16 0.0376(13) 0.0578(16) 0.0360(13) 0.0163(12) 0.0107(10) 0.0191(12) C17 0.0444(15) 0.0546(17) 0.0632(18) 0.0198(14) 0.0014(13) 0.0264(14) C18 0.086(3) 0.056(2) 0.087(3) 0.0316(18) 0.016(2) 0.0357(19) C19 0.0363(13) 0.0451(15) 0.0612(17) 0.0112(13) 0.0122(12) 0.0220(12) C20 0.066(2) 0.0526(18) 0.068(2) 0.0013(15) 0.0193(16) 0.0324(16) C21 0.0460(16) 0.077(2) 0.0386(14) 0.0153(14) 0.0192(12) 0.0247(15) C22 0.098(3) 0.131(4) 0.068(2) -0.028(3) 0.030(2) 0.040(3) C23 0.0470(15) 0.0708(19) 0.0353(13) 0.0250(13) 0.0113(12) 0.0223(14) C24 0.088(3) 0.092(3) 0.0463(18) -0.0024(17) -0.0215(18) 0.044(2) C25 0.0387(14) 0.0583(17) 0.0433(14) 0.0146(12) 0.0066(11) 0.0279(13) C26 0.083(2) 0.0541(19) 0.067(2) 0.0205(16) 0.0142(18) 0.0352(18) C27 0.0308(13) 0.0586(17) 0.0503(15) 0.0140(13) 0.0141(11) 0.0207(12) C28 0.0344(14) 0.0553(17) 0.078(2) 0.0253(15) 0.0145(14) 0.0165(13) C29 0.062(2) 0.064(2) 0.102(3) -0.017(2) 0.028(2) -0.0168(18) C30 0.137(4) 0.059(2) 0.062(2) -0.0112(18) -0.053(2) 0.018(2) C31 0.059(2) 0.0377(16) 0.114(3) -0.0089(18) 0.002(2) 0.0141(15) C32 0.0272(14) 0.0543(19) 0.139(4) -0.025(2) 0.0119(18) 0.0048(13) C33 0.079(2) 0.0459(16) 0.0335(14) -0.0012(12) -0.0010(14) 0.0152(15) C34 0.0631(18) 0.0339(13) 0.0477(15) 0.0091(11) 0.0081(13) 0.0099(13) C35 0.0269(11) 0.0328(12) 0.0312(11) 0.0020(9) 0.0028(9) 0.0113(9) C36 0.0312(12) 0.0376(12) 0.0294(11) 0.0023(9) 0.0021(9) 0.0119(10) C37 0.0264(11) 0.0380(12) 0.0355(12) 0.0085(10) 0.0074(9) 0.0124(9) C38 0.0221(10) 0.0313(11) 0.0391(12) 0.0045(9) 0.0040(9) 0.0091(9) C39 0.0241(10) 0.0344(12) 0.0328(11) 0.0022(9) 0.0013(9) 0.0122(9) C40 0.0262(11) 0.0329(12) 0.0310(11) 0.0054(9) 0.0014(9) 0.0111(9) C41 0.0466(15) 0.0437(15) 0.0403(14) 0.0113(11) 0.0118(11) 0.0115(12) C42 0.0407(14) 0.0343(13) 0.0374(13) 0.0010(10) -0.0056(11) 0.0106(11) C43 0.0332(12) 0.0273(11) 0.0302(11) -0.0014(9) -0.0012(9) 0.0064(9) C44 0.0381(13) 0.0286(11) 0.0376(13) 0.0033(9) 0.0048(10) 0.0093(10) C45 0.0515(15) 0.0296(12) 0.0342(12) 0.0016(10) 0.0079(11) 0.0056(11) C46 0.0632(17) 0.0328(13) 0.0317(12) 0.0057(10) 0.0003(12) 0.0111(12) C47 0.0545(16) 0.0329(13) 0.0358(13) -0.0001(10) -0.0054(11) 0.0176(12) C48 0.0398(13) 0.0342(12) 0.0317(12) -0.0012(9) -0.0011(10) 0.0139(10) C49 0.074(2) 0.0440(16) 0.0472(16) 0.0102(13) 0.0248(15) 0.0139(15) C50 0.093(3) 0.0557(19) 0.0458(17) 0.0056(14) -0.0055(18) 0.0425(19) C51 0.0331(12) 0.0306(11) 0.0310(11) 0.0047(9) 0.0024(9) 0.0088(9) C52 0.0347(12) 0.0348(12) 0.0333(12) -0.0012(10) 0.0012(10) 0.0077(10) C53 0.0327(12) 0.0323(12) 0.0417(13) 0.0039(10) 0.0069(10) 0.0055(10) C54 0.0444(14) 0.0332(12) 0.0350(12) 0.0049(10) 0.0139(11) 0.0080(11) C55 0.0406(13) 0.0323(12) 0.0283(11) 0.0050(9) 0.0053(10) 0.0046(10) C56 0.0340(12) 0.0350(12) 0.0295(11) 0.0063(9) 0.0028(9) 0.0076(10) C57 0.0372(14) 0.0511(17) 0.0611(19) -0.0061(14) 0.0098(13) 0.0097(13) C58 0.0506(16) 0.0474(15) 0.0318(13) -0.0002(11) 0.0087(11) 0.0036(13) C59 0.0338(12) 0.0402(13) 0.0252(11) 0.0040(9) 0.0037(9) 0.0114(10) C60 0.0346(12) 0.0378(13) 0.0351(12) 0.0063(10) 0.0017(10) 0.0093(10) C61 0.0354(13) 0.0468(15) 0.0370(13) 0.0059(11) 0.0019(10) 0.0048(11) C62 0.0285(12) 0.0611(17) 0.0387(13) 0.0042(12) 0.0009(10) 0.0119(12) C63 0.0381(13) 0.0531(16) 0.0341(12) 0.0030(11) 0.0035(10) 0.0217(12) C64 0.0354(12) 0.0402(13) 0.0316(12) -0.0004(10) 0.0033(10) 0.0127(10) C65 0.0443(17) 0.0543(19) 0.068(2) 0.0133(16) -0.0045(15) 0.0009(14) C66 0.0458(17) 0.067(2) 0.068(2) -0.0028(17) 0.0042(15) 0.0296(16) F1 0.139(2) 0.0608(12) 0.0465(10) 0.0136(9) 0.0408(12) 0.0127(12) F2 0.0896(16) 0.133(2) 0.0857(15) 0.0723(15) 0.0322(12) 0.0664(15) F3 0.0912(15) 0.0642(12) 0.0655(12) 0.0325(10) -0.0089(11) -0.0255(11) F4 0.059(3) 0.073(3) 0.0327(19) 0.0002(16) 0.0066(19) 0.005(3) F5 0.089(4) 0.034(3) 0.039(3) -0.001(2) 0.001(2) -0.001(4) F6 0.076(6) 0.106(8) 0.054(4) -0.023(4) -0.029(4) 0.065(6) F4' 0.122(10) 0.066(9) 0.047(6) -0.023(5) -0.009(5) 0.067(9) F5' 0.119(19) 0.065(7) 0.025(3) 0.008(3) 0.000(6) -0.033(9) F6' 0.049(4) 0.082(6) 0.047(6) -0.006(4) -0.025(3) 0.016(5) F7 0.056(2) 0.146(6) 0.075(2) 0.006(3) 0.0253(18) 0.036(2) F8 0.086(3) 0.079(3) 0.071(4) -0.031(3) 0.031(2) 0.008(2) F9 0.195(9) 0.111(6) 0.109(5) 0.082(5) 0.110(6) 0.095(6) F7' 0.105(9) 0.26(3) 0.026(5) -0.033(9) 0.012(5) 0.037(13) F8' 0.121(13) 0.073(9) 0.123(15) -0.016(11) 0.087(11) -0.029(10) F9' 0.42(4) 0.18(2) 0.18(2) 0.148(19) 0.24(3) 0.25(3) F10 0.109(4) 0.069(3) 0.087(4) 0.041(3) 0.012(3) 0.048(3) F11 0.060(3) 0.080(3) 0.130(7) 0.022(4) -0.015(3) 0.036(2) F12 0.187(8) 0.106(5) 0.050(3) -0.028(4) -0.042(5) 0.116(6) F10' 0.153(12) 0.142(15) 0.095(11) 0.051(9) 0.066(10) 0.130(12) F11' 0.174(15) 0.063(7) 0.27(3) 0.054(12) 0.070(19) 0.076(9) F12' 0.29(3) 0.25(3) 0.081(12) -0.085(14) -0.121(16) 0.24(2) F13 0.042(4) 0.067(4) 0.141(12) -0.025(5) 0.006(5) 0.027(3) F14 0.046(4) 0.120(10) 0.153(11) 0.073(8) 0.012(5) -0.019(5) F15 0.033(3) 0.186(12) 0.059(5) -0.043(8) -0.004(3) 0.013(5) F13' 0.043(3) 0.042(4) 0.177(14) -0.003(6) -0.003(6) -0.001(3) F14' 0.048(4) 0.172(12) 0.115(10) 0.066(9) -0.010(5) 0.031(6) F15' 0.038(4) 0.148(14) 0.117(11) -0.076(9) 0.020(5) 0.006(7) F16 0.173(3) 0.0717(14) 0.0467(11) 0.0120(10) -0.0406(14) 0.0029(16) F17 0.0671(14) 0.177(3) 0.0897(17) -0.0910(18) 0.0043(12) 0.0217(16) F18 0.0787(13) 0.0655(12) 0.0450(10) -0.0081(9) 0.0063(9) -0.0230(10) F19 0.052(3) 0.044(3) 0.186(6) 0.008(3) -0.024(4) 0.002(2) F20 0.132(7) 0.073(3) 0.078(3) -0.005(2) -0.032(3) -0.029(4) F21 0.088(4) 0.069(2) 0.156(7) 0.004(3) 0.072(4) -0.016(3) F19' 0.045(7) 0.086(8) 0.18(2) 0.027(13) -0.073(10) -0.013(6) F20' 0.169(18) 0.140(13) 0.143(12) 0.087(11) -0.041(14) -0.085(13) F21' 0.093(12) 0.031(7) 0.37(4) -0.057(15) 0.032(19) -0.004(6) F22 0.051(2) 0.088(3) 0.128(5) 0.016(3) 0.034(3) 0.040(2) F23 0.075(4) 0.073(4) 0.142(6) -0.052(4) -0.055(5) 0.047(3) F24 0.105(4) 0.117(4) 0.080(3) 0.046(4) 0.025(4) 0.081(4) F22' 0.093(8) 0.053(6) 0.21(2) 0.008(9) 0.013(10) 0.054(6) F23' 0.19(2) 0.135(13) 0.206(19) -0.107(14) -0.179(16) 0.126(14) F24' 0.24(2) 0.23(2) 0.176(19) 0.068(16) 0.130(19) 0.197(19) N1 0.0314(10) 0.0332(10) 0.0313(10) 0.0044(8) 0.0018(8) 0.0147(8) N2 0.0382(11) 0.0528(13) 0.0314(10) 0.0121(9) 0.0098(8) 0.0257(10) N3 0.0260(9) 0.0364(10) 0.0277(9) 0.0084(8) 0.0034(7) 0.0126(8) P1 0.0388(3) 0.0369(3) 0.0363(3) -0.0003(3) -0.0025(3) 0.0101(3) P2 0.0278(3) 0.0345(3) 0.0359(3) 0.0021(2) 0.0059(2) 0.0110(2) Pd1 0.02509(9) 0.03041(10) 0.02421(9) 0.00507(6) 0.00277(6) 0.01179(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 C59 1.638(3) . ? B1 C35 1.641(3) . ? B1 C43 1.646(3) . ? B1 C51 1.646(3) . ? C1 C2 1.485(4) . ? C2 N1 1.332(3) . ? C2 C3 1.443(3) . ? C3 C4 1.364(4) . ? C3 C17 1.505(3) . ? C4 C5 1.448(3) . ? C4 C19 1.504(3) . ? C5 C6 1.375(3) . ? C5 N1 1.420(3) . ? C6 C7 1.412(3) . ? C7 N2 1.351(3) . ? C7 C8 1.440(3) . ? C8 C9 1.371(3) . ? C8 C21 1.509(3) . ? C9 C10 1.444(3) . ? C9 C23 1.498(3) . ? C10 N2 1.351(3) . ? C10 C11 1.412(3) . ? C11 C12 1.374(3) . ? C12 N3 1.425(3) . ? C12 C13 1.447(3) . ? C13 C14 1.359(3) . ? C13 C25 1.505(3) . ? C14 C15 1.432(3) . ? C14 C27 1.505(3) . ? C15 N3 1.335(3) . ? C15 C16 1.490(3) . ? C17 C18 1.515(4) . ? C19 C20 1.517(4) . ? C21 C22 1.519(5) . ? C23 C24 1.515(5) . ? C25 C26 1.524(4) . ? C27 C28 1.532(4) . ? C29 P1 1.806(4) . ? C30 P1 1.803(3) . ? C31 P1 1.808(3) . ? C32 P2 1.803(3) . ? C33 P2 1.818(3) . ? C34 P2 1.809(3) . ? C35 C40 1.398(3) . ? C35 C36 1.406(3) . ? C36 C37 1.387(3) . ? C37 C38 1.394(3) . ? C37 C41 1.496(3) . ? C38 C39 1.386(3) . ? C39 C40 1.393(3) . ? C39 C42 1.497(3) . ? C41 F3 1.310(3) . ? C41 F1 1.322(3) . ? C41 F2 1.333(3) . ? C42 F5' 1.226(13) . ? C42 F4' 1.303(14) . ? C42 F6 1.307(7) . ? C42 F5 1.314(8) . ? C42 F4 1.389(8) . ? C42 F6' 1.393(13) . ? C43 C48 1.394(3) . ? C43 C44 1.407(3) . ? C44 C45 1.391(3) . ? C45 C46 1.384(4) . ? C45 C49 1.494(4) . ? C46 C47 1.388(4) . ? C47 C48 1.394(4) . ? C47 C50 1.500(4) . ? C49 F9' 1.173(14) . ? C49 F8' 1.239(15) . ? C49 F8 1.296(5) . ? C49 F9 1.300(6) . ? C49 F7 1.348(6) . ? C49 F7' 1.379(12) . ? C50 F12' 1.146(11) . ? C50 F10' 1.260(14) . ? C50 F12 1.295(7) . ? C50 F10 1.314(5) . ? C50 F11 1.370(7) . ? C50 F11' 1.406(15) . ? C51 C56 1.397(3) . ? C51 C52 1.399(3) . ? C52 C53 1.392(3) . ? C53 C54 1.383(3) . ? C53 C57 1.498(4) . ? C54 C55 1.384(4) . ? C55 C56 1.392(3) . ? C55 C58 1.495(3) . ? C57 F13' 1.282(12) . ? C57 F13 1.298(13) . ? C57 F14' 1.301(14) . ? C57 F15 1.306(11) . ? C57 F15' 1.317(16) . ? C57 F14 1.338(13) . ? C58 F17 1.305(4) . ? C58 F18 1.308(3) . ? C58 F16 1.317(4) . ? C59 C64 1.397(3) . ? C59 C60 1.405(3) . ? C60 C61 1.386(3) . ? C61 C62 1.387(4) . ? C61 C65 1.492(4) . ? C62 C63 1.380(4) . ? C63 C64 1.397(3) . ? C63 C66 1.495(4) . ? C65 F19' 1.223(12) . ? C65 F21' 1.26(3) . ? C65 F19 1.303(9) . ? C65 F21 1.318(6) . ? C65 F20 1.326(7) . ? C65 F20' 1.342(18) . ? C66 F23' 1.172(12) . ? C66 F23 1.292(8) . ? C66 F22' 1.31(2) . ? C66 F22 1.322(5) . ? C66 F24 1.356(6) . ? C66 F24' 1.374(13) . ? N1 Pd1 2.0410(18) . ? N2 Pd1 2.298(2) . ? N3 Pd1 2.0354(18) . ? P1 Pd1 2.3337(7) . ? P2 Pd1 2.3207(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C59 B1 C35 111.06(19) . . ? C59 B1 C43 106.36(19) . . ? C35 B1 C43 110.55(19) . . ? C59 B1 C51 111.90(19) . . ? C35 B1 C51 106.64(19) . . ? C43 B1 C51 110.39(19) . . ? N1 C2 C3 111.2(2) . . ? N1 C2 C1 122.6(2) . . ? C3 C2 C1 126.2(2) . . ? C4 C3 C2 106.6(2) . . ? C4 C3 C17 128.5(2) . . ? C2 C3 C17 124.8(2) . . ? C3 C4 C5 107.5(2) . . ? C3 C4 C19 127.8(2) . . ? C5 C4 C19 124.6(2) . . ? C6 C5 N1 128.1(2) . . ? C6 C5 C4 124.1(2) . . ? N1 C5 C4 107.7(2) . . ? C5 C6 C7 131.0(2) . . ? N2 C7 C6 120.9(2) . . ? N2 C7 C8 110.3(2) . . ? C6 C7 C8 128.8(2) . . ? C9 C8 C7 106.3(2) . . ? C9 C8 C21 128.2(2) . . ? C7 C8 C21 125.5(2) . . ? C8 C9 C10 106.0(2) . . ? C8 C9 C23 128.9(2) . . ? C10 C9 C23 125.1(2) . . ? N2 C10 C11 121.1(2) . . ? N2 C10 C9 110.3(2) . . ? C11 C10 C9 128.6(2) . . ? C12 C11 C10 130.8(2) . . ? C11 C12 N3 127.9(2) . . ? C11 C12 C13 124.8(2) . . ? N3 C12 C13 107.32(19) . . ? C14 C13 C12 107.6(2) . . ? C14 C13 C25 126.6(2) . . ? C12 C13 C25 125.7(2) . . ? C13 C14 C15 107.1(2) . . ? C13 C14 C27 128.3(2) . . ? C15 C14 C27 124.3(2) . . ? N3 C15 C14 111.1(2) . . ? N3 C15 C16 123.2(2) . . ? C14 C15 C16 125.7(2) . . ? C3 C17 C18 113.3(3) . . ? C4 C19 C20 112.5(2) . . ? C8 C21 C22 113.0(3) . . ? C9 C23 C24 113.9(3) . . ? C13 C25 C26 111.9(2) . . ? C14 C27 C28 110.5(2) . . ? C40 C35 C36 115.7(2) . . ? C40 C35 B1 124.3(2) . . ? C36 C35 B1 120.0(2) . . ? C37 C36 C35 122.4(2) . . ? C36 C37 C38 120.7(2) . . ? C36 C37 C41 119.7(2) . . ? C38 C37 C41 119.6(2) . . ? C39 C38 C37 118.0(2) . . ? C38 C39 C40 120.9(2) . . ? C38 C39 C42 120.2(2) . . ? C40 C39 C42 118.8(2) . . ? C39 C40 C35 122.3(2) . . ? F3 C41 F1 107.4(2) . . ? F3 C41 F2 106.6(3) . . ? F1 C41 F2 102.8(3) . . ? F3 C41 C37 113.6(2) . . ? F1 C41 C37 113.3(2) . . ? F2 C41 C37 112.3(2) . . ? F5' C42 F4' 114.5(18) . . ? F5' C42 F6 77.6(14) . . ? F4' C42 F6 117.9(10) . . ? F5' C42 F5 118.6(16) . . ? F4' C42 F5 10.7(14) . . ? F6 C42 F5 108.2(8) . . ? F5' C42 F4 27(2) . . ? F4' C42 F4 95.4(9) . . ? F6 C42 F4 103.4(9) . . ? F5 C42 F4 102.8(5) . . ? F5' C42 F6' 105.5(15) . . ? F4' C42 F6' 101.7(11) . . ? F6 C42 F6' 28.2(5) . . ? F5 C42 F6' 91.0(8) . . ? F4 C42 F6' 130.1(9) . . ? F5' C42 C39 115.9(6) . . ? F4' C42 C39 111.7(9) . . ? F6 C42 C39 115.5(4) . . ? F5 C42 C39 115.1(5) . . ? F4 C42 C39 110.4(4) . . ? F6' C42 C39 106.0(8) . . ? C48 C43 C44 115.5(2) . . ? C48 C43 B1 124.8(2) . . ? C44 C43 B1 119.7(2) . . ? C45 C44 C43 122.5(2) . . ? C46 C45 C44 120.5(2) . . ? C46 C45 C49 119.4(2) . . ? C44 C45 C49 120.0(2) . . ? C45 C46 C47 118.3(2) . . ? C46 C47 C48 120.7(2) . . ? C46 C47 C50 119.6(3) . . ? C48 C47 C50 119.7(3) . . ? C43 C48 C47 122.4(2) . . ? F9' C49 F8' 111.5(19) . . ? F9' C49 F8 59(2) . . ? F8' C49 F8 133.6(8) . . ? F9' C49 F9 125.2(9) . . ? F8' C49 F9 34.6(11) . . ? F8 C49 F9 108.9(4) . . ? F9' C49 F7 44(2) . . ? F8' C49 F7 75.1(13) . . ? F8 C49 F7 102.4(4) . . ? F9 C49 F7 104.4(5) . . ? F9' C49 F7' 105.8(15) . . ? F8' C49 F7' 98.6(11) . . ? F8 C49 F7' 51.4(14) . . ? F9 C49 F7' 64.6(12) . . ? F7 C49 F7' 137.0(8) . . ? F9' C49 C45 118.4(6) . . ? F8' C49 C45 110.8(9) . . ? F8 C49 C45 112.7(3) . . ? F9 C49 C45 115.1(4) . . ? F7 C49 C45 112.3(3) . . ? F7' C49 C45 109.7(6) . . ? F12' C50 F10' 115.4(16) . . ? F12' C50 F12 127.6(10) . . ? F10' C50 F12 26.3(12) . . ? F12' C50 F10 62(2) . . ? F10' C50 F10 126.8(9) . . ? F12 C50 F10 108.4(5) . . ? F12' C50 F11 42(2) . . ? F10' C50 F11 81.8(11) . . ? F12 C50 F11 104.5(6) . . ? F10 C50 F11 101.7(4) . . ? F12' C50 F11' 107.2(14) . . ? F10' C50 F11' 98.5(11) . . ? F12 C50 F11' 72.7(11) . . ? F10 C50 F11' 46.3(13) . . ? F11 C50 F11' 139.4(11) . . ? F12' C50 C47 115.0(7) . . ? F10' C50 C47 113.0(8) . . ? F12 C50 C47 115.0(4) . . ? F10 C50 C47 114.5(4) . . ? F11 C50 C47 111.5(4) . . ? F11' C50 C47 105.7(7) . . ? C56 C51 C52 115.5(2) . . ? C56 C51 B1 124.7(2) . . ? C52 C51 B1 119.8(2) . . ? C53 C52 C51 122.6(2) . . ? C54 C53 C52 120.6(2) . . ? C54 C53 C57 119.6(2) . . ? C52 C53 C57 119.7(2) . . ? C53 C54 C55 118.0(2) . . ? C54 C55 C56 121.2(2) . . ? C54 C55 C58 120.0(2) . . ? C56 C55 C58 118.8(2) . . ? C55 C56 C51 122.1(2) . . ? F13' C57 F13 121.2(9) . . ? F13' C57 F14' 104.1(10) . . ? F13 C57 F14' 86.7(11) . . ? F13' C57 F15 83.5(10) . . ? F13 C57 F15 104.8(10) . . ? F14' C57 F15 22.3(12) . . ? F13' C57 F15' 102.7(11) . . ? F13 C57 F15' 24.9(15) . . ? F14' C57 F15' 108.3(12) . . ? F15 C57 F15' 122.1(11) . . ? F13' C57 F14 22.4(12) . . ? F13 C57 F14 108.4(9) . . ? F14' C57 F14 123.9(9) . . ? F15 C57 F14 104.9(9) . . ? F15' C57 F14 85.8(11) . . ? F13' C57 C53 114.6(6) . . ? F13 C57 C53 113.6(8) . . ? F14' C57 C53 112.3(8) . . ? F15 C57 C53 114.8(6) . . ? F15' C57 C53 114.0(9) . . ? F14 C57 C53 109.8(7) . . ? F17 C58 F18 106.5(3) . . ? F17 C58 F16 105.5(3) . . ? F18 C58 F16 104.9(3) . . ? F17 C58 C55 113.7(3) . . ? F18 C58 C55 113.7(2) . . ? F16 C58 C55 111.7(2) . . ? C64 C59 C60 115.6(2) . . ? C64 C59 B1 125.2(2) . . ? C60 C59 B1 119.1(2) . . ? C61 C60 C59 122.4(2) . . ? C60 C61 C62 120.6(2) . . ? C60 C61 C65 120.3(3) . . ? C62 C61 C65 119.0(3) . . ? C63 C62 C61 118.4(2) . . ? C62 C63 C64 120.7(2) . . ? C62 C63 C66 118.7(3) . . ? C64 C63 C66 120.6(3) . . ? C59 C64 C63 122.2(2) . . ? F19' C65 F21' 111.3(15) . . ? F19' C65 F19 123.5(11) . . ? F21' C65 F19 30(2) . . ? F19' C65 F21 70.7(12) . . ? F21' C65 F21 129.9(18) . . ? F19 C65 F21 105.2(6) . . ? F19' C65 F20 35.4(13) . . ? F21' C65 F20 81.4(18) . . ? F19 C65 F20 104.2(7) . . ? F21 C65 F20 104.3(5) . . ? F19' C65 F20' 107.1(12) . . ? F21' C65 F20' 106.1(18) . . ? F19 C65 F20' 76.6(16) . . ? F21 C65 F20' 37.9(12) . . ? F20 C65 F20' 136.0(8) . . ? F19' C65 C61 116.2(9) . . ? F21' C65 C61 109.9(11) . . ? F19 C65 C61 116.6(4) . . ? F21 C65 C61 113.0(4) . . ? F20 C65 C61 112.4(4) . . ? F20' C65 C61 105.5(8) . . ? F23' C66 F23 123.3(10) . . ? F23' C66 F22' 110.4(16) . . ? F23 C66 F22' 27.9(13) . . ? F23' C66 F22 67.0(19) . . ? F23 C66 F22 107.0(5) . . ? F22' C66 F22 127.9(9) . . ? F23' C66 F24 35(2) . . ? F23 C66 F24 105.8(7) . . ? F22' C66 F24 82.9(12) . . ? F22 C66 F24 100.9(4) . . ? F23' C66 F24' 109.8(13) . . ? F23 C66 F24' 73.4(14) . . ? F22' C66 F24' 101.1(13) . . ? F22 C66 F24' 44.7(15) . . ? F24 C66 F24' 138.6(11) . . ? F23' C66 C63 117.3(7) . . ? F23 C66 C63 115.6(4) . . ? F22' C66 C63 111.7(8) . . ? F22 C66 C63 114.7(4) . . ? F24 C66 C63 111.5(4) . . ? F24' C66 C63 105.2(7) . . ? C2 N1 C5 106.95(19) . . ? C2 N1 Pd1 127.95(17) . . ? C5 N1 Pd1 124.82(15) . . ? C7 N2 C10 107.1(2) . . ? C7 N2 Pd1 126.29(16) . . ? C10 N2 Pd1 126.47(15) . . ? C15 N3 C12 106.88(18) . . ? C15 N3 Pd1 127.38(15) . . ? C12 N3 Pd1 125.73(14) . . ? C30 P1 C29 102.5(2) . . ? C30 P1 C31 104.1(2) . . ? C29 P1 C31 103.2(2) . . ? C30 P1 Pd1 111.19(14) . . ? C29 P1 Pd1 118.10(12) . . ? C31 P1 Pd1 116.01(12) . . ? C32 P2 C34 103.99(18) . . ? C32 P2 C33 105.02(19) . . ? C34 P2 C33 102.40(14) . . ? C32 P2 Pd1 113.66(11) . . ? C34 P2 Pd1 111.98(10) . . ? C33 P2 Pd1 118.27(11) . . ? N3 Pd1 N1 175.97(7) . . ? N3 Pd1 N2 87.93(7) . . ? N1 Pd1 N2 88.08(7) . . ? N3 Pd1 P2 88.58(6) . . ? N1 Pd1 P2 92.38(6) . . ? N2 Pd1 P2 95.10(6) . . ? N3 Pd1 P1 89.33(6) . . ? N1 Pd1 P1 90.37(6) . . ? N2 Pd1 P1 94.44(6) . . ? P2 Pd1 P1 170.15(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 -0.3(3) . . . . ? C1 C2 C3 C4 -179.0(2) . . . . ? N1 C2 C3 C17 -178.1(2) . . . . ? C1 C2 C3 C17 3.2(4) . . . . ? C2 C3 C4 C5 1.7(3) . . . . ? C17 C3 C4 C5 179.4(3) . . . . ? C2 C3 C4 C19 -174.0(2) . . . . ? C17 C3 C4 C19 3.6(5) . . . . ? C3 C4 C5 C6 175.2(2) . . . . ? C19 C4 C5 C6 -8.9(4) . . . . ? C3 C4 C5 N1 -2.5(3) . . . . ? C19 C4 C5 N1 173.4(2) . . . . ? N1 C5 C6 C7 -2.8(4) . . . . ? C4 C5 C6 C7 -179.9(2) . . . . ? C5 C6 C7 N2 -1.7(4) . . . . ? C5 C6 C7 C8 179.9(3) . . . . ? N2 C7 C8 C9 -0.4(3) . . . . ? C6 C7 C8 C9 178.2(2) . . . . ? N2 C7 C8 C21 -179.6(3) . . . . ? C6 C7 C8 C21 -1.1(4) . . . . ? C7 C8 C9 C10 -0.4(3) . . . . ? C21 C8 C9 C10 178.8(3) . . . . ? C7 C8 C9 C23 -179.5(3) . . . . ? C21 C8 C9 C23 -0.3(5) . . . . ? C8 C9 C10 N2 1.1(3) . . . . ? C23 C9 C10 N2 -179.8(2) . . . . ? C8 C9 C10 C11 -176.3(3) . . . . ? C23 C9 C10 C11 2.9(4) . . . . ? N2 C10 C11 C12 -3.0(4) . . . . ? C9 C10 C11 C12 174.0(3) . . . . ? C10 C11 C12 N3 1.8(4) . . . . ? C10 C11 C12 C13 -176.4(3) . . . . ? C11 C12 C13 C14 177.8(2) . . . . ? N3 C12 C13 C14 -0.7(3) . . . . ? C11 C12 C13 C25 -4.3(4) . . . . ? N3 C12 C13 C25 177.1(2) . . . . ? C12 C13 C14 C15 1.4(3) . . . . ? C25 C13 C14 C15 -176.4(2) . . . . ? C12 C13 C14 C27 -172.9(3) . . . . ? C25 C13 C14 C27 9.3(4) . . . . ? C13 C14 C15 N3 -1.7(3) . . . . ? C27 C14 C15 N3 172.9(2) . . . . ? C13 C14 C15 C16 177.1(2) . . . . ? C27 C14 C15 C16 -8.3(4) . . . . ? C4 C3 C17 C18 -87.4(4) . . . . ? C2 C3 C17 C18 89.9(4) . . . . ? C3 C4 C19 C20 101.9(3) . . . . ? C5 C4 C19 C20 -73.2(3) . . . . ? C9 C8 C21 C22 -94.4(4) . . . . ? C7 C8 C21 C22 84.7(4) . . . . ? C8 C9 C23 C24 97.8(3) . . . . ? C10 C9 C23 C24 -81.2(4) . . . . ? C14 C13 C25 C26 86.8(3) . . . . ? C12 C13 C25 C26 -90.6(3) . . . . ? C13 C14 C27 C28 84.1(3) . . . . ? C15 C14 C27 C28 -89.3(3) . . . . ? C59 B1 C35 C40 -110.7(2) . . . . ? C43 B1 C35 C40 7.1(3) . . . . ? C51 B1 C35 C40 127.1(2) . . . . ? C59 B1 C35 C36 70.4(3) . . . . ? C43 B1 C35 C36 -171.8(2) . . . . ? C51 B1 C35 C36 -51.8(3) . . . . ? C40 C35 C36 C37 -0.9(3) . . . . ? B1 C35 C36 C37 178.1(2) . . . . ? C35 C36 C37 C38 0.1(3) . . . . ? C35 C36 C37 C41 178.2(2) . . . . ? C36 C37 C38 C39 0.8(3) . . . . ? C41 C37 C38 C39 -177.4(2) . . . . ? C37 C38 C39 C40 -0.8(3) . . . . ? C37 C38 C39 C42 -179.6(2) . . . . ? C38 C39 C40 C35 0.0(3) . . . . ? C42 C39 C40 C35 178.8(2) . . . . ? C36 C35 C40 C39 0.8(3) . . . . ? B1 C35 C40 C39 -178.1(2) . . . . ? C36 C37 C41 F3 152.4(2) . . . . ? C38 C37 C41 F3 -29.5(3) . . . . ? C36 C37 C41 F1 29.4(3) . . . . ? C38 C37 C41 F1 -152.4(2) . . . . ? C36 C37 C41 F2 -86.5(3) . . . . ? C38 C37 C41 F2 91.7(3) . . . . ? C38 C39 C42 F5' -166(3) . . . . ? C40 C39 C42 F5' 15(3) . . . . ? C38 C39 C42 F4' -32.2(13) . . . . ? C40 C39 C42 F4' 149.0(13) . . . . ? C38 C39 C42 F6 106.1(15) . . . . ? C40 C39 C42 F6 -72.7(15) . . . . ? C38 C39 C42 F5 -21.2(7) . . . . ? C40 C39 C42 F5 160.0(6) . . . . ? C38 C39 C42 F4 -137.0(5) . . . . ? C40 C39 C42 F4 44.2(6) . . . . ? C38 C39 C42 F6' 77.7(11) . . . . ? C40 C39 C42 F6' -101.1(11) . . . . ? C59 B1 C43 C48 -129.7(2) . . . . ? C35 B1 C43 C48 109.7(2) . . . . ? C51 B1 C43 C48 -8.1(3) . . . . ? C59 B1 C43 C44 50.1(3) . . . . ? C35 B1 C43 C44 -70.6(3) . . . . ? C51 B1 C43 C44 171.6(2) . . . . ? C48 C43 C44 C45 -2.1(3) . . . . ? B1 C43 C44 C45 178.2(2) . . . . ? C43 C44 C45 C46 1.1(4) . . . . ? C43 C44 C45 C49 -177.9(2) . . . . ? C44 C45 C46 C47 0.5(4) . . . . ? C49 C45 C46 C47 179.5(3) . . . . ? C45 C46 C47 C48 -1.0(4) . . . . ? C45 C46 C47 C50 -179.7(3) . . . . ? C44 C43 C48 C47 1.5(3) . . . . ? B1 C43 C48 C47 -178.7(2) . . . . ? C46 C47 C48 C43 0.0(4) . . . . ? C50 C47 C48 C43 178.6(3) . . . . ? C46 C45 C49 F9' -171(3) . . . . ? C44 C45 C49 F9' 8(3) . . . . ? C46 C45 C49 F8' 58.6(16) . . . . ? C44 C45 C49 F8' -122.3(16) . . . . ? C46 C45 C49 F8 -104.6(6) . . . . ? C44 C45 C49 F8 74.5(6) . . . . ? C46 C45 C49 F9 21.2(8) . . . . ? C44 C45 C49 F9 -159.7(7) . . . . ? C46 C45 C49 F7 140.4(4) . . . . ? C44 C45 C49 F7 -40.5(5) . . . . ? C46 C45 C49 F7' -49.2(19) . . . . ? C44 C45 C49 F7' 129.9(18) . . . . ? C46 C47 C50 F12' 52(3) . . . . ? C48 C47 C50 F12' -126(3) . . . . ? C46 C47 C50 F10' -172.2(14) . . . . ? C48 C47 C50 F10' 9.1(15) . . . . ? C46 C47 C50 F12 -143.5(7) . . . . ? C48 C47 C50 F12 37.8(8) . . . . ? C46 C47 C50 F10 -17.0(6) . . . . ? C48 C47 C50 F10 164.3(5) . . . . ? C46 C47 C50 F11 97.7(5) . . . . ? C48 C47 C50 F11 -80.9(5) . . . . ? C46 C47 C50 F11' -65.6(16) . . . . ? C48 C47 C50 F11' 115.7(16) . . . . ? C59 B1 C51 C56 10.2(3) . . . . ? C35 B1 C51 C56 131.8(2) . . . . ? C43 B1 C51 C56 -108.0(3) . . . . ? C59 B1 C51 C52 -170.7(2) . . . . ? C35 B1 C51 C52 -49.1(3) . . . . ? C43 B1 C51 C52 71.0(3) . . . . ? C56 C51 C52 C53 1.7(4) . . . . ? B1 C51 C52 C53 -177.5(2) . . . . ? C51 C52 C53 C54 -0.3(4) . . . . ? C51 C52 C53 C57 -177.9(3) . . . . ? C52 C53 C54 C55 -0.7(4) . . . . ? C57 C53 C54 C55 176.9(2) . . . . ? C53 C54 C55 C56 0.3(4) . . . . ? C53 C54 C55 C58 -178.2(2) . . . . ? C54 C55 C56 C51 1.2(4) . . . . ? C58 C55 C56 C51 179.7(2) . . . . ? C52 C51 C56 C55 -2.1(3) . . . . ? B1 C51 C56 C55 177.0(2) . . . . ? C54 C53 C57 F13' -111.9(13) . . . . ? C52 C53 C57 F13' 65.7(13) . . . . ? C54 C53 C57 F13 33.4(10) . . . . ? C52 C53 C57 F13 -149.0(10) . . . . ? C54 C53 C57 F14' 129.7(13) . . . . ? C52 C53 C57 F14' -52.7(14) . . . . ? C54 C53 C57 F15 153.9(12) . . . . ? C52 C53 C57 F15 -28.5(12) . . . . ? C54 C53 C57 F15' 6.1(18) . . . . ? C52 C53 C57 F15' -176.3(18) . . . . ? C54 C53 C57 F14 -88.2(12) . . . . ? C52 C53 C57 F14 89.4(12) . . . . ? C54 C55 C58 F17 -13.4(4) . . . . ? C56 C55 C58 F17 168.1(3) . . . . ? C54 C55 C58 F18 -135.5(3) . . . . ? C56 C55 C58 F18 46.0(4) . . . . ? C54 C55 C58 F16 105.9(3) . . . . ? C56 C55 C58 F16 -72.6(3) . . . . ? C35 B1 C59 C64 -2.8(3) . . . . ? C43 B1 C59 C64 -123.1(2) . . . . ? C51 B1 C59 C64 116.3(2) . . . . ? C35 B1 C59 C60 174.3(2) . . . . ? C43 B1 C59 C60 53.9(3) . . . . ? C51 B1 C59 C60 -66.7(3) . . . . ? C64 C59 C60 C61 -1.0(3) . . . . ? B1 C59 C60 C61 -178.3(2) . . . . ? C59 C60 C61 C62 1.7(4) . . . . ? C59 C60 C61 C65 -179.9(3) . . . . ? C60 C61 C62 C63 -1.0(4) . . . . ? C65 C61 C62 C63 -179.4(3) . . . . ? C61 C62 C63 C64 -0.4(4) . . . . ? C61 C62 C63 C66 179.5(3) . . . . ? C60 C59 C64 C63 -0.4(3) . . . . ? B1 C59 C64 C63 176.7(2) . . . . ? C62 C63 C64 C59 1.1(4) . . . . ? C66 C63 C64 C59 -178.8(2) . . . . ? C60 C61 C65 F19' 159.9(18) . . . . ? C62 C61 C65 F19' -21.6(19) . . . . ? C60 C61 C65 F21' 32(3) . . . . ? C62 C61 C65 F21' -149(3) . . . . ? C60 C61 C65 F19 1.0(8) . . . . ? C62 C61 C65 F19 179.4(7) . . . . ? C60 C61 C65 F21 -121.1(7) . . . . ? C62 C61 C65 F21 57.3(7) . . . . ? C60 C61 C65 F20 121.2(6) . . . . ? C62 C61 C65 F20 -60.4(7) . . . . ? C60 C61 C65 F20' -81.6(19) . . . . ? C62 C61 C65 F20' 96.8(19) . . . . ? C62 C63 C66 F23' 46(3) . . . . ? C64 C63 C66 F23' -134(3) . . . . ? C62 C63 C66 F23 -154.5(8) . . . . ? C64 C63 C66 F23 25.4(8) . . . . ? C62 C63 C66 F22' 175.3(14) . . . . ? C64 C63 C66 F22' -4.9(14) . . . . ? C62 C63 C66 F22 -29.3(6) . . . . ? C64 C63 C66 F22 150.6(5) . . . . ? C62 C63 C66 F24 84.5(5) . . . . ? C64 C63 C66 F24 -95.6(5) . . . . ? C62 C63 C66 F24' -76(2) . . . . ? C64 C63 C66 F24' 104(2) . . . . ? C3 C2 N1 C5 -1.2(3) . . . . ? C1 C2 N1 C5 177.5(2) . . . . ? C3 C2 N1 Pd1 172.79(16) . . . . ? C1 C2 N1 Pd1 -8.5(3) . . . . ? C6 C5 N1 C2 -175.3(2) . . . . ? C4 C5 N1 C2 2.3(3) . . . . ? C6 C5 N1 Pd1 10.5(3) . . . . ? C4 C5 N1 Pd1 -172.00(15) . . . . ? C6 C7 N2 C10 -177.6(2) . . . . ? C8 C7 N2 C10 1.0(3) . . . . ? C6 C7 N2 Pd1 -1.9(3) . . . . ? C8 C7 N2 Pd1 176.81(16) . . . . ? C11 C10 N2 C7 176.3(2) . . . . ? C9 C10 N2 C7 -1.3(3) . . . . ? C11 C10 N2 Pd1 0.5(4) . . . . ? C9 C10 N2 Pd1 -177.06(16) . . . . ? C14 C15 N3 C12 1.2(3) . . . . ? C16 C15 N3 C12 -177.6(2) . . . . ? C14 C15 N3 Pd1 -179.67(16) . . . . ? C16 C15 N3 Pd1 1.5(3) . . . . ? C11 C12 N3 C15 -178.8(2) . . . . ? C13 C12 N3 C15 -0.3(3) . . . . ? C11 C12 N3 Pd1 2.0(4) . . . . ? C13 C12 N3 Pd1 -179.46(15) . . . . ? C15 N3 Pd1 N1 169.4(10) . . . . ? C12 N3 Pd1 N1 -11.7(12) . . . . ? C15 N3 Pd1 N2 178.1(2) . . . . ? C12 N3 Pd1 N2 -2.95(19) . . . . ? C15 N3 Pd1 P2 -86.77(19) . . . . ? C12 N3 Pd1 P2 92.20(18) . . . . ? C15 N3 Pd1 P1 83.61(19) . . . . ? C12 N3 Pd1 P1 -97.43(18) . . . . ? C2 N1 Pd1 N3 -174.0(10) . . . . ? C5 N1 Pd1 N3 -1.0(12) . . . . ? C2 N1 Pd1 N2 177.3(2) . . . . ? C5 N1 Pd1 N2 -9.70(18) . . . . ? C2 N1 Pd1 P2 82.2(2) . . . . ? C5 N1 Pd1 P2 -104.73(18) . . . . ? C2 N1 Pd1 P1 -88.3(2) . . . . ? C5 N1 Pd1 P1 84.73(18) . . . . ? C7 N2 Pd1 N3 -173.1(2) . . . . ? C10 N2 Pd1 N3 1.9(2) . . . . ? C7 N2 Pd1 N1 6.3(2) . . . . ? C10 N2 Pd1 N1 -178.7(2) . . . . ? C7 N2 Pd1 P2 98.5(2) . . . . ? C10 N2 Pd1 P2 -86.5(2) . . . . ? C7 N2 Pd1 P1 -83.9(2) . . . . ? C10 N2 Pd1 P1 91.0(2) . . . . ? C32 P2 Pd1 N3 -156.08(18) . . . . ? C34 P2 Pd1 N3 -38.60(12) . . . . ? C33 P2 Pd1 N3 80.08(14) . . . . ? C32 P2 Pd1 N1 20.00(18) . . . . ? C34 P2 Pd1 N1 137.48(12) . . . . ? C33 P2 Pd1 N1 -103.84(14) . . . . ? C32 P2 Pd1 N2 -68.28(18) . . . . ? C34 P2 Pd1 N2 49.20(12) . . . . ? C33 P2 Pd1 N2 167.88(13) . . . . ? C32 P2 Pd1 P1 126.1(2) . . . . ? C34 P2 Pd1 P1 -116.43(17) . . . . ? C33 P2 Pd1 P1 2.3(2) . . . . ? C30 P1 Pd1 N3 58.4(2) . . . . ? C29 P1 Pd1 N3 -59.7(2) . . . . ? C31 P1 Pd1 N3 177.06(18) . . . . ? C30 P1 Pd1 N1 -117.6(2) . . . . ? C29 P1 Pd1 N1 124.3(2) . . . . ? C31 P1 Pd1 N1 1.08(18) . . . . ? C30 P1 Pd1 N2 -29.5(2) . . . . ? C29 P1 Pd1 N2 -147.6(2) . . . . ? C31 P1 Pd1 N2 89.19(17) . . . . ? C30 P1 Pd1 P2 136.2(2) . . . . ? C29 P1 Pd1 P2 18.1(2) . . . . ? C31 P1 Pd1 P2 -105.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.652 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.059 #===END data_cb21cb _database_code_CSD 195926 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H59 B F24 N3 P Pd' _chemical_formula_weight 1462.31 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' B B 0.0013 0.0007 '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' 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9944(11) _cell_length_b 20.5527(17) _cell_length_c 25.0962(21) _cell_angle_alpha 90.000 _cell_angle_beta 104.331(1) _cell_angle_gamma 90.000 _cell_volume 6493.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5435 _cell_measurement_theta_min 4.459 _cell_measurement_theta_max 56.667 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS2.0 (Sheldrick 2000)' _exptl_special_details ; All CF3-groups and one ethyl-group are disordered. ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex with D8-Goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66958 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 26.37 _reflns_number_total 13271 _reflns_number_gt 10167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.6' _computing_cell_refinement 'SMART-NT V5.6' _computing_data_reduction 'SMART-NT V5.6' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material 'XSHELL in SHELXTL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+2.4109P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13271 _refine_ls_number_parameters 1048 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B B 0.5028(3) 0.3989(2) 0.82270(15) 0.0301(9) Uani 1 1 d . . . C1 C 0.0455(3) 0.1366(2) 0.82969(15) 0.0471(10) Uani 1 1 d . . . H1A H 0.0014 0.1637 0.8474 0.071 Uiso 1 1 calc R . . H1B H -0.0003 0.1115 0.7998 0.071 Uiso 1 1 calc R . . H1C H 0.0928 0.1644 0.8147 0.071 Uiso 1 1 calc R . . C2 C 0.1096(3) 0.09152(19) 0.87066(14) 0.0374(9) Uani 1 1 d . . . C3 C 0.1745(3) 0.0394(2) 0.85938(15) 0.0409(9) Uani 1 1 d . . . C4 C 0.2094(3) 0.00530(19) 0.90742(15) 0.0384(9) Uani 1 1 d . . . C5 C 0.1642(3) 0.03629(18) 0.94748(14) 0.0358(8) Uani 1 1 d . . . C6 C 0.1628(3) 0.01209(19) 0.99780(14) 0.0362(8) Uani 1 1 d . . . H6 H 0.2039 -0.0260 1.0088 0.043 Uiso 1 1 calc R . . C7 C 0.1087(3) 0.03609(18) 1.03534(13) 0.0334(8) Uani 1 1 d . . . C8 C 0.1183(3) 0.01200(18) 1.08963(14) 0.0357(8) Uani 1 1 d . . . C9 C 0.0620(3) 0.05373(18) 1.11450(13) 0.0334(8) Uani 1 1 d . . . C10 C 0.0186(3) 0.10246(18) 1.07482(13) 0.0320(8) Uani 1 1 d . . . C11 C -0.0372(3) 0.15786(19) 1.08437(14) 0.0366(8) Uani 1 1 d . . . H11 H -0.0547 0.1596 1.1189 0.044 Uiso 1 1 calc R . . C12 C -0.0696(3) 0.20953(19) 1.05024(14) 0.0357(8) Uani 1 1 d . . . C13 C -0.1342(3) 0.2634(2) 1.05949(15) 0.0399(9) Uani 1 1 d . B . C14 C -0.1607(3) 0.29826(19) 1.01210(15) 0.0381(9) Uani 1 1 d . . . C15 C -0.1123(3) 0.2652(2) 0.97401(14) 0.0398(9) Uani 1 1 d . . . C16 C -0.1341(4) 0.2817(3) 0.91428(16) 0.0583(12) Uani 1 1 d . . . H16A H -0.1010 0.3236 0.9098 0.088 Uiso 1 1 calc R . . H16B H -0.2110 0.2847 0.8988 0.088 Uiso 1 1 calc R . . H16C H -0.1047 0.2477 0.8950 0.088 Uiso 1 1 calc R . . C17 C 0.1957(4) 0.0265(2) 0.80381(17) 0.0525(11) Uani 1 1 d . . . H17A H 0.1558 0.0586 0.7772 0.063 Uiso 1 1 calc R . . H17B H 0.1683 -0.0173 0.7912 0.063 Uiso 1 1 calc R . . C18 C 0.3126(4) 0.0299(2) 0.80353(19) 0.0626(13) Uani 1 1 d . . . H18A H 0.3419 0.0720 0.8183 0.094 Uiso 1 1 calc R . . H18B H 0.3197 0.0252 0.7657 0.094 Uiso 1 1 calc R . . H18C H 0.3514 -0.0052 0.8263 0.094 Uiso 1 1 calc R . . C19 C 0.2803(3) -0.0528(2) 0.91872(17) 0.0504(10) Uani 1 1 d . . . H19A H 0.2849 -0.0728 0.8835 0.060 Uiso 1 1 calc R . . H19B H 0.2496 -0.0855 0.9394 0.060 Uiso 1 1 calc R . . C20 C 0.3910(4) -0.0344(3) 0.9517(2) 0.0650(13) Uani 1 1 d . . . H20A H 0.4206 -0.0013 0.9317 0.098 Uiso 1 1 calc R . . H20B H 0.4367 -0.0730 0.9572 0.098 Uiso 1 1 calc R . . H20C H 0.3870 -0.0171 0.9876 0.098 Uiso 1 1 calc R . . C21 C 0.1832(3) -0.0458(2) 1.11434(16) 0.0458(10) Uani 1 1 d . . . H21A H 0.1759 -0.0802 1.0860 0.055 Uiso 1 1 calc R . . H21B H 0.1548 -0.0632 1.1446 0.055 Uiso 1 1 calc R . . C22 C 0.3001(4) -0.0299(2) 1.1365(2) 0.0709(15) Uani 1 1 d . . . H22A H 0.3287 -0.0125 1.1068 0.106 Uiso 1 1 calc R . . H22B H 0.3389 -0.0696 1.1512 0.106 Uiso 1 1 calc R . . H22C H 0.3082 0.0025 1.1659 0.106 Uiso 1 1 calc R . . C23 C 0.0543(3) 0.05399(19) 1.17320(14) 0.0388(9) Uani 1 1 d . . . H23A H 0.0672 0.0094 1.1884 0.047 Uiso 1 1 calc R . . H23B H -0.0184 0.0669 1.1745 0.047 Uiso 1 1 calc R . . C24 C 0.1334(3) 0.1001(2) 1.20841(15) 0.0494(10) Uani 1 1 d . . . H24A H 0.2057 0.0863 1.2087 0.074 Uiso 1 1 calc R . . H24B H 0.1244 0.0998 1.2461 0.074 Uiso 1 1 calc R . . H24C H 0.1213 0.1442 1.1933 0.074 Uiso 1 1 calc R . . C25 C -0.1656(3) 0.2757(2) 1.11230(16) 0.0495(10) Uani 1 1 d . . . H25A H -0.2199 0.3106 1.1059 0.059 Uiso 1 1 calc R A 1 H25B H -0.1990 0.2358 1.1224 0.059 Uiso 1 1 calc R A 1 C26 C -0.0805(5) 0.2941(3) 1.1575(2) 0.0523(16) Uani 0.66 1 d P B 1 H26A H -0.1090 0.3066 1.1888 0.078 Uiso 0.66 1 calc PR B 1 H26B H -0.0422 0.3310 1.1469 0.078 Uiso 0.66 1 calc PR B 1 H26C H -0.0318 0.2573 1.1681 0.078 Uiso 0.66 1 calc PR B 1 C26' C -0.2682(11) 0.2561(9) 1.1149(6) 0.076(5) Uani 0.34 1 d P B 2 H26D H -0.3213 0.2784 1.0862 0.114 Uiso 0.34 1 calc PR B 2 H26E H -0.2793 0.2672 1.1511 0.114 Uiso 0.34 1 calc PR B 2 H26F H -0.2753 0.2089 1.1094 0.114 Uiso 0.34 1 calc PR B 2 C27 C -0.2213(3) 0.3608(2) 1.00015(17) 0.0464(10) Uani 1 1 d . . . H27A H -0.2623 0.3676 1.0281 0.056 Uiso 1 1 calc R . . H27B H -0.2724 0.3576 0.9637 0.056 Uiso 1 1 calc R . . C28 C -0.1500(4) 0.4184(2) 1.00033(19) 0.0586(12) Uani 1 1 d . . . H28A H -0.0977 0.4210 1.0359 0.088 Uiso 1 1 calc R . . H28B H -0.1926 0.4582 0.9943 0.088 Uiso 1 1 calc R . . H28C H -0.1130 0.4134 0.9709 0.088 Uiso 1 1 calc R . . C29 C 0.1614(4) 0.2970(3) 1.0002(2) 0.0793(16) Uani 1 1 d . . . H29A H 0.1853 0.2716 1.0341 0.119 Uiso 1 1 calc R . . H29B H 0.0961 0.3204 1.0010 0.119 Uiso 1 1 calc R . . H29C H 0.2166 0.3283 0.9972 0.119 Uiso 1 1 calc R . . C30 C 0.1087(5) 0.2977(3) 0.8831(2) 0.0898(19) Uani 1 1 d . . . H30A H 0.0538 0.3289 0.8866 0.135 Uiso 1 1 calc R . . H30B H 0.0839 0.2727 0.8491 0.135 Uiso 1 1 calc R . . H30C H 0.1737 0.3212 0.8819 0.135 Uiso 1 1 calc R . . C31 C 0.2663(3) 0.2115(3) 0.9420(2) 0.0632(13) Uani 1 1 d . . . H31A H 0.3158 0.2478 0.9437 0.095 Uiso 1 1 calc R . . H31B H 0.2623 0.1862 0.9085 0.095 Uiso 1 1 calc R . . H31C H 0.2912 0.1834 0.9742 0.095 Uiso 1 1 calc R . . C40 C 0.4335(3) 0.46630(17) 0.81651(13) 0.0293(7) Uani 1 1 d . . . C41 C 0.4616(3) 0.52516(19) 0.79641(14) 0.0377(9) Uani 1 1 d . . . H41 H 0.5281 0.5282 0.7872 0.045 Uiso 1 1 calc R . . C42 C 0.3965(3) 0.57913(19) 0.78943(17) 0.0445(9) Uani 1 1 d . C . C43 C 0.2984(3) 0.5769(2) 0.80178(16) 0.0452(10) Uani 1 1 d . . . H43 H 0.2537 0.6141 0.7974 0.054 Uiso 1 1 calc R . . C44 C 0.2680(3) 0.51901(18) 0.82064(14) 0.0353(8) Uani 1 1 d . D . C45 C 0.3337(3) 0.46520(18) 0.82756(13) 0.0316(8) Uani 1 1 d . . . H45 H 0.3098 0.4259 0.8404 0.038 Uiso 1 1 calc R . . C46 C 0.4319(5) 0.6421(3) 0.7702(3) 0.0728(15) Uani 1 1 d . . . C47 C 0.1632(3) 0.5160(2) 0.83509(19) 0.0489(11) Uani 1 1 d . . . C48 C 0.5090(2) 0.36212(17) 0.88127(13) 0.0294(8) Uani 1 1 d . . . C49 C 0.4878(3) 0.39157(19) 0.92720(13) 0.0333(8) Uani 1 1 d . . . H49 H 0.4671 0.4360 0.9250 0.040 Uiso 1 1 calc R . . C50 C 0.4958(3) 0.3581(2) 0.97661(15) 0.0394(9) Uani 1 1 d . E . C51 C 0.5255(3) 0.2938(2) 0.98146(16) 0.0448(10) Uani 1 1 d . . . H51 H 0.5296 0.2708 1.0148 0.054 Uiso 1 1 calc R . . C52 C 0.5491(3) 0.26334(19) 0.93689(16) 0.0440(10) Uani 1 1 d . F . C53 C 0.5415(3) 0.29699(19) 0.88796(15) 0.0379(9) Uani 1 1 d . . . H53 H 0.5590 0.2751 0.8581 0.046 Uiso 1 1 calc R . . C54 C 0.4727(4) 0.3932(3) 1.02431(17) 0.0575(12) Uani 1 1 d . . . C55 C 0.5813(5) 0.1932(2) 0.9407(2) 0.0662(14) Uani 1 1 d . . . C56 C 0.4402(2) 0.35389(16) 0.77070(14) 0.0294(7) Uani 1 1 d . . . C57 C 0.4487(3) 0.36545(18) 0.71706(14) 0.0345(8) Uani 1 1 d . . . H57 H 0.4934 0.3996 0.7107 0.041 Uiso 1 1 calc R . . C58 C 0.3940(3) 0.3287(2) 0.67290(15) 0.0449(10) Uani 1 1 d . G . C59 C 0.3259(3) 0.2795(2) 0.68017(17) 0.0477(10) Uani 1 1 d . . . H59 H 0.2884 0.2542 0.6499 0.057 Uiso 1 1 calc R . . C60 C 0.3141(3) 0.2683(2) 0.73218(18) 0.0467(10) Uani 1 1 d . H . C61 C 0.3699(3) 0.30501(18) 0.77621(15) 0.0362(8) Uani 1 1 d . . . H61 H 0.3595 0.2964 0.8117 0.043 Uiso 1 1 calc R . . C62 C 0.4078(5) 0.3408(4) 0.6164(2) 0.0729(15) Uani 1 1 d . . . C63 C 0.2409(6) 0.2161(4) 0.7425(3) 0.0743(17) Uani 1 1 d . . . C64 C 0.6274(3) 0.41076(18) 0.82086(13) 0.0318(8) Uani 1 1 d . . . C65 C 0.6876(3) 0.4615(2) 0.85044(14) 0.0389(9) Uani 1 1 d . . . H65 H 0.6551 0.4899 0.8713 0.047 Uiso 1 1 calc R . . C66 C 0.7928(3) 0.4718(2) 0.85022(16) 0.0495(11) Uani 1 1 d . . . C67 C 0.8432(3) 0.4307(2) 0.82082(16) 0.0496(11) Uani 1 1 d . . . H67 H 0.9150 0.4380 0.8201 0.060 Uiso 1 1 calc R . . C68 C 0.7871(3) 0.3796(2) 0.79283(16) 0.0456(10) Uani 1 1 d . I . C69 C 0.6811(3) 0.3697(2) 0.79274(14) 0.0365(8) Uani 1 1 d . . . H69 H 0.6442 0.3339 0.7729 0.044 Uiso 1 1 calc R . . C70 C 0.8533(4) 0.5281(3) 0.8798(2) 0.0713(16) Uani 1 1 d . . . C71 C 0.8378(4) 0.3344(3) 0.7602(2) 0.0643(14) Uani 1 1 d . . . F1 F 0.5061(11) 0.6366(7) 0.7436(6) 0.105(6) Uani 0.60 1 d P C 1 F2 F 0.4515(10) 0.6858(4) 0.8046(4) 0.098(3) Uani 0.60 1 d P C 1 F3 F 0.3495(10) 0.6678(5) 0.7290(4) 0.100(3) Uani 0.60 1 d P C 1 F1' F 0.375(2) 0.6888(8) 0.7650(16) 0.23(2) Uani 0.40 1 d P C 2 F2' F 0.4749(18) 0.6376(12) 0.7309(7) 0.101(8) Uani 0.40 1 d P C 2 F3' F 0.5272(16) 0.6623(9) 0.8111(7) 0.158(8) Uani 0.40 1 d P C 2 F4 F 0.1631(12) 0.5579(8) 0.8785(6) 0.059(3) Uani 0.55 1 d P D 1 F5 F 0.0819(10) 0.5395(6) 0.7903(5) 0.062(2) Uani 0.55 1 d P D 1 F6 F 0.1338(12) 0.4652(7) 0.8487(8) 0.140(7) Uani 0.55 1 d P D 1 F4' F 0.1357(10) 0.4507(7) 0.8439(5) 0.051(2) Uani 0.45 1 d P D 2 F5' F 0.1567(18) 0.5437(12) 0.8753(10) 0.115(8) Uani 0.45 1 d P D 2 F6' F 0.0887(16) 0.5347(14) 0.8039(8) 0.150(10) Uani 0.45 1 d P D 2 F7 F 0.3956(11) 0.4370(7) 1.0095(5) 0.109(5) Uani 0.70 1 d P E 1 F8 F 0.5533(7) 0.4246(6) 1.0543(4) 0.100(4) Uani 0.70 1 d P E 1 F9 F 0.4374(8) 0.3547(7) 1.0582(4) 0.100(4) Uani 0.70 1 d P E 1 F7' F 0.503(3) 0.3592(14) 1.0697(8) 0.138(11) Uani 0.30 1 d P E 2 F8' F 0.3849(19) 0.412(2) 1.0191(11) 0.152(17) Uani 0.30 1 d P E 2 F9' F 0.539(3) 0.4407(12) 1.0380(10) 0.104(10) Uani 0.30 1 d P E 2 F10 F 0.6389(11) 0.1778(4) 0.9907(4) 0.110(4) Uani 0.65 1 d P F 1 F11 F 0.5083(6) 0.1533(4) 0.9272(6) 0.101(4) Uani 0.65 1 d P F 1 F12 F 0.6509(12) 0.1808(7) 0.9113(6) 0.131(6) Uani 0.65 1 d P F 1 F10' F 0.517(2) 0.1609(8) 0.8970(9) 0.133(10) Uani 0.35 1 d P F 2 F11' F 0.6682(11) 0.1796(9) 0.943(2) 0.171(18) Uani 0.35 1 d P F 2 F12' F 0.545(3) 0.1635(8) 0.9804(13) 0.172(10) Uani 0.35 1 d P F 2 F13 F 0.4644(15) 0.3922(8) 0.6133(4) 0.107(6) Uani 0.55 1 d P G 1 F14 F 0.4342(14) 0.2920(6) 0.5934(4) 0.102(5) Uani 0.55 1 d P G 1 F15 F 0.3098(8) 0.3582(7) 0.5822(3) 0.092(3) Uani 0.55 1 d P G 1 F13' F 0.377(4) 0.2994(17) 0.5819(8) 0.27(2) Uani 0.45 1 d P G 2 F14' F 0.394(3) 0.3920(12) 0.5975(10) 0.187(14) Uani 0.45 1 d P G 2 F15' F 0.5165(12) 0.3343(18) 0.6172(7) 0.162(6) Uani 0.45 1 d P G 2 F16 F 0.2754(4) 0.1885(3) 0.7940(2) 0.0791(15) Uani 0.75 1 d P H 1 F17 F 0.1487(4) 0.2453(3) 0.7521(3) 0.0904(17) Uani 0.75 1 d P H 1 F18 F 0.2263(12) 0.1681(5) 0.7104(4) 0.157(5) Uani 0.75 1 d P H 1 F16' F 0.1657(18) 0.2114(14) 0.6864(8) 0.118(8) Uani 0.25 1 d P H 2 F17' F 0.2733(16) 0.1685(11) 0.7460(19) 0.182(19) Uani 0.25 1 d P H 2 F18' F 0.170(3) 0.2203(11) 0.738(3) 0.25(3) Uani 0.25 1 d P H 2 F19 F 0.9461(3) 0.5074(2) 0.91325(15) 0.1231(15) Uani 1 1 d . . . F20 F 0.8066(3) 0.5594(2) 0.90955(19) 0.1349(18) Uani 1 1 d . . . F21 F 0.8875(3) 0.56732(16) 0.84639(14) 0.0911(10) Uani 1 1 d . . . F22 F 0.8373(9) 0.2749(6) 0.7718(4) 0.111(4) Uani 0.75 1 d P I 1 F23 F 0.9349(7) 0.3527(4) 0.7602(4) 0.121(4) Uani 0.75 1 d P I 1 F24 F 0.8045(7) 0.3453(3) 0.7094(3) 0.108(3) Uani 0.75 1 d P I 1 F22' F 0.8356(15) 0.2735(16) 0.7852(8) 0.055(5) Uani 0.25 1 d P I 2 F23' F 0.9432(15) 0.3304(12) 0.7773(9) 0.084(7) Uani 0.25 1 d PU I 2 F24' F 0.7677(13) 0.3111(11) 0.7100(8) 0.091(8) Uani 0.25 1 d P I 2 N1 N 0.1075(2) 0.09102(15) 0.92392(11) 0.0343(7) Uani 1 1 d . . . N2 N 0.0460(2) 0.08997(14) 1.02640(11) 0.0314(6) Uani 1 1 d . . . N3 N -0.0547(2) 0.21469(15) 0.99674(11) 0.0357(7) Uani 1 1 d . . . P P 0.13587(9) 0.24281(6) 0.94159(4) 0.0462(3) Uani 1 1 d . . . Pd Pd 0.04097(2) 0.156787(14) 0.965045(10) 0.03211(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B 0.0240(18) 0.036(2) 0.0323(19) 0.0004(17) 0.0104(15) -0.0008(16) C1 0.062(3) 0.050(3) 0.0316(19) 0.0039(18) 0.0156(18) -0.005(2) C2 0.043(2) 0.038(2) 0.0340(18) -0.0049(16) 0.0141(15) -0.0141(17) C3 0.045(2) 0.043(2) 0.039(2) -0.0102(17) 0.0175(16) -0.0147(18) C4 0.040(2) 0.039(2) 0.0389(19) -0.0097(17) 0.0142(16) -0.0063(17) C5 0.0378(19) 0.037(2) 0.0328(18) -0.0059(16) 0.0097(15) -0.0064(16) C6 0.0369(19) 0.036(2) 0.0341(18) -0.0031(16) 0.0062(15) -0.0039(16) C7 0.0357(18) 0.034(2) 0.0301(17) 0.0011(15) 0.0081(14) -0.0054(16) C8 0.039(2) 0.034(2) 0.0330(18) 0.0030(15) 0.0073(15) -0.0044(16) C9 0.0381(19) 0.033(2) 0.0291(17) 0.0035(15) 0.0089(14) -0.0076(16) C10 0.0332(18) 0.036(2) 0.0276(16) -0.0005(15) 0.0096(14) -0.0072(16) C11 0.0359(18) 0.042(2) 0.0335(18) 0.0014(17) 0.0121(14) -0.0010(17) C12 0.0326(18) 0.041(2) 0.0339(18) 0.0023(16) 0.0100(15) 0.0008(16) C13 0.0333(19) 0.044(2) 0.042(2) 0.0009(18) 0.0094(16) 0.0020(17) C14 0.0279(18) 0.040(2) 0.043(2) 0.0018(17) 0.0044(15) 0.0012(16) C15 0.037(2) 0.048(3) 0.0315(18) 0.0061(17) 0.0024(15) 0.0029(18) C16 0.058(3) 0.078(3) 0.037(2) 0.012(2) 0.0092(19) 0.022(2) C17 0.069(3) 0.053(3) 0.044(2) -0.013(2) 0.030(2) -0.013(2) C18 0.075(3) 0.068(3) 0.058(3) 0.006(2) 0.043(2) 0.006(3) C19 0.061(3) 0.049(3) 0.047(2) -0.0074(19) 0.023(2) -0.002(2) C20 0.056(3) 0.074(4) 0.066(3) 0.000(3) 0.017(2) 0.012(2) C21 0.059(3) 0.039(2) 0.039(2) 0.0062(17) 0.0117(18) 0.0052(19) C22 0.070(3) 0.060(3) 0.071(3) 0.004(3) -0.006(2) 0.023(3) C23 0.043(2) 0.041(2) 0.0331(18) 0.0069(16) 0.0114(15) -0.0016(17) C24 0.050(2) 0.064(3) 0.0338(19) -0.0038(19) 0.0097(17) -0.009(2) C25 0.058(3) 0.050(3) 0.047(2) 0.008(2) 0.026(2) 0.016(2) C26 0.059(4) 0.054(4) 0.044(3) -0.009(3) 0.010(3) 0.008(3) C26' 0.061(9) 0.115(14) 0.056(8) 0.014(9) 0.024(7) 0.016(9) C27 0.039(2) 0.051(3) 0.046(2) 0.0060(19) 0.0038(17) 0.0092(19) C28 0.068(3) 0.049(3) 0.060(3) 0.006(2) 0.020(2) 0.000(2) C29 0.077(4) 0.072(4) 0.091(4) -0.032(3) 0.023(3) -0.033(3) C30 0.103(4) 0.071(4) 0.093(4) 0.038(3) 0.020(3) -0.017(3) C31 0.046(2) 0.070(3) 0.077(3) -0.007(3) 0.024(2) -0.018(2) C40 0.0281(16) 0.034(2) 0.0252(15) -0.0046(14) 0.0057(13) -0.0047(15) C41 0.0364(19) 0.040(2) 0.0391(19) -0.0017(17) 0.0143(15) -0.0040(17) C42 0.050(2) 0.035(2) 0.053(2) 0.0016(18) 0.0200(19) 0.0010(19) C43 0.051(2) 0.036(2) 0.050(2) -0.0064(18) 0.0152(18) 0.0109(19) C44 0.0316(18) 0.035(2) 0.0402(19) -0.0079(16) 0.0118(15) 0.0005(16) C45 0.0294(17) 0.031(2) 0.0347(17) -0.0050(15) 0.0078(14) -0.0057(15) C46 0.093(4) 0.036(3) 0.105(5) 0.008(3) 0.051(4) 0.007(3) C47 0.037(2) 0.053(3) 0.059(3) -0.010(2) 0.016(2) 0.008(2) C48 0.0208(15) 0.034(2) 0.0334(17) 0.0005(14) 0.0055(13) -0.0047(14) C49 0.0278(17) 0.039(2) 0.0337(18) -0.0016(16) 0.0095(14) -0.0012(15) C50 0.0325(18) 0.052(3) 0.0342(19) -0.0007(17) 0.0100(15) -0.0091(17) C51 0.046(2) 0.051(3) 0.036(2) 0.0128(18) 0.0082(17) -0.0108(19) C52 0.042(2) 0.035(2) 0.051(2) 0.0092(18) 0.0040(17) -0.0029(17) C53 0.0330(19) 0.039(2) 0.041(2) -0.0011(17) 0.0083(15) 0.0016(16) C54 0.070(3) 0.069(4) 0.039(2) -0.001(2) 0.024(2) -0.010(3) C55 0.086(4) 0.045(3) 0.065(3) 0.016(3) 0.016(3) 0.008(3) C56 0.0256(16) 0.029(2) 0.0345(17) -0.0024(14) 0.0084(13) 0.0036(14) C57 0.0364(19) 0.032(2) 0.0367(19) 0.0017(15) 0.0126(15) -0.0010(16) C58 0.049(2) 0.049(3) 0.037(2) -0.0043(18) 0.0121(17) 0.0036(19) C59 0.048(2) 0.042(3) 0.049(2) -0.0168(19) 0.0059(18) -0.006(2) C60 0.037(2) 0.041(3) 0.062(3) -0.011(2) 0.0126(18) -0.0070(18) C61 0.0324(18) 0.036(2) 0.041(2) -0.0031(16) 0.0106(15) -0.0009(16) C62 0.091(4) 0.087(5) 0.039(3) -0.008(3) 0.012(3) -0.013(4) C63 0.058(4) 0.066(5) 0.099(4) -0.017(4) 0.021(3) -0.026(3) C64 0.0254(16) 0.040(2) 0.0308(17) 0.0082(15) 0.0082(13) -0.0003(15) C65 0.0335(19) 0.050(3) 0.0327(18) 0.0030(17) 0.0065(15) -0.0061(17) C66 0.035(2) 0.069(3) 0.039(2) 0.015(2) -0.0014(16) -0.019(2) C67 0.0244(18) 0.077(3) 0.047(2) 0.025(2) 0.0090(17) -0.002(2) C68 0.0322(19) 0.067(3) 0.041(2) 0.024(2) 0.0163(16) 0.011(2) C69 0.0286(17) 0.045(2) 0.0371(19) 0.0095(17) 0.0099(15) 0.0053(16) C70 0.050(3) 0.091(4) 0.065(3) 0.014(3) -0.001(2) -0.037(3) C71 0.046(3) 0.093(4) 0.063(3) 0.030(3) 0.030(2) 0.026(3) F1 0.103(7) 0.050(6) 0.197(16) 0.041(8) 0.106(9) 0.015(5) F2 0.147(10) 0.046(5) 0.108(7) -0.019(5) 0.045(7) -0.043(6) F3 0.115(6) 0.058(6) 0.125(6) 0.055(5) 0.028(5) 0.017(5) F1' 0.19(3) 0.046(11) 0.53(6) 0.08(2) 0.24(3) 0.046(16) F2' 0.159(19) 0.092(13) 0.053(5) 0.006(5) 0.031(8) -0.060(12) F3' 0.205(17) 0.122(14) 0.120(11) 0.036(10) -0.013(12) -0.125(13) F4 0.065(5) 0.055(4) 0.064(5) -0.029(4) 0.032(4) -0.005(4) F5 0.033(4) 0.106(6) 0.042(4) 0.006(4) 0.001(3) 0.027(3) F6 0.100(7) 0.034(6) 0.338(19) 0.000(7) 0.153(10) 0.005(5) F4' 0.041(4) 0.027(6) 0.097(6) -0.004(4) 0.041(4) -0.001(3) F5' 0.093(9) 0.155(18) 0.127(11) -0.106(10) 0.082(8) -0.065(9) F6' 0.043(7) 0.30(2) 0.104(14) 0.064(11) 0.017(8) 0.040(9) F7 0.142(11) 0.147(7) 0.054(3) 0.021(4) 0.052(5) 0.087(7) F8 0.082(4) 0.151(12) 0.072(6) -0.057(6) 0.026(4) -0.034(5) F9 0.156(8) 0.101(5) 0.068(7) 0.010(5) 0.075(6) -0.019(7) F7' 0.29(3) 0.105(18) 0.027(6) 0.011(7) 0.053(16) 0.03(3) F8' 0.055(11) 0.32(5) 0.10(2) -0.10(2) 0.040(12) 0.000(19) F9' 0.22(3) 0.046(8) 0.057(11) -0.022(8) 0.064(13) -0.026(10) F10 0.136(8) 0.063(4) 0.100(5) 0.033(4) -0.026(5) 0.025(5) F11 0.076(4) 0.039(4) 0.165(10) 0.010(6) -0.015(6) -0.015(3) F12 0.178(15) 0.066(6) 0.182(10) 0.048(6) 0.107(10) 0.064(8) F10' 0.22(2) 0.023(7) 0.114(13) 0.005(7) -0.035(12) 0.006(8) F11' 0.031(6) 0.042(9) 0.40(5) -0.03(2) -0.017(17) 0.014(5) F12' 0.34(3) 0.056(9) 0.18(2) 0.059(11) 0.17(2) 0.060(14) F13 0.146(11) 0.141(13) 0.043(4) -0.010(7) 0.041(6) -0.059(11) F14 0.164(11) 0.107(9) 0.052(5) -0.004(5) 0.058(6) 0.081(10) F15 0.097(5) 0.132(9) 0.040(3) 0.012(4) 0.001(4) 0.027(5) F13' 0.47(4) 0.28(4) 0.072(9) -0.088(16) 0.106(18) -0.25(3) F14' 0.32(3) 0.17(2) 0.123(19) 0.102(17) 0.15(2) 0.16(3) F15' 0.135(11) 0.29(2) 0.091(9) 0.053(12) 0.078(9) 0.054(16) F16 0.086(3) 0.058(3) 0.087(3) 0.025(2) 0.008(3) -0.031(3) F17 0.052(3) 0.079(4) 0.151(5) 0.043(3) 0.046(3) 0.003(3) F18 0.254(13) 0.112(7) 0.109(6) -0.056(5) 0.055(7) -0.140(8) F16' 0.085(13) 0.132(19) 0.126(15) 0.000(13) 0.010(10) -0.091(13) F17' 0.087(12) 0.042(13) 0.35(5) 0.07(2) -0.08(2) -0.037(10) F18' 0.17(3) 0.035(12) 0.66(8) 0.04(2) 0.30(4) 0.023(12) F19 0.082(2) 0.142(3) 0.110(3) 0.032(2) -0.043(2) -0.061(2) F20 0.113(3) 0.140(4) 0.175(4) -0.107(3) 0.080(3) -0.084(3) F21 0.090(2) 0.079(2) 0.102(2) 0.0218(19) 0.0211(18) -0.0302(18) F22 0.186(8) 0.065(5) 0.128(8) 0.023(5) 0.125(6) 0.031(4) F23 0.090(6) 0.113(5) 0.202(9) 0.040(5) 0.114(6) 0.027(4) F24 0.167(8) 0.113(6) 0.051(3) 0.016(4) 0.039(4) 0.068(5) F22' 0.055(8) 0.089(14) 0.030(6) 0.007(6) 0.028(6) 0.024(8) F23' 0.024(6) 0.128(16) 0.100(11) -0.015(11) 0.014(7) 0.023(9) F24' 0.054(8) 0.16(2) 0.049(9) -0.048(12) -0.005(6) 0.076(11) N1 0.0391(16) 0.0362(18) 0.0290(14) -0.0031(13) 0.0113(12) -0.0025(14) N2 0.0368(16) 0.0313(17) 0.0269(14) 0.0020(12) 0.0092(12) -0.0031(13) N3 0.0325(15) 0.0427(19) 0.0321(15) 0.0040(13) 0.0081(12) 0.0054(14) P 0.0491(6) 0.0438(7) 0.0449(6) 0.0017(5) 0.0102(5) -0.0057(5) Pd 0.03434(15) 0.03683(18) 0.02562(14) 0.00223(12) 0.00828(10) -0.00062(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B C48 1.637(5) . ? B C40 1.639(5) . ? B C56 1.642(5) . ? B C64 1.649(5) . ? C1 C2 1.478(5) . ? C2 N1 1.344(4) . ? C2 C3 1.435(5) . ? C3 C4 1.371(5) . ? C3 C17 1.510(5) . ? C4 C5 1.433(5) . ? C4 C19 1.493(6) . ? C5 C6 1.362(5) . ? C5 N1 1.394(5) . ? C6 C7 1.398(5) . ? C7 N2 1.360(5) . ? C7 C8 1.426(5) . ? C8 C9 1.374(5) . ? C8 C21 1.499(5) . ? C9 C10 1.426(5) . ? C9 C23 1.501(5) . ? C10 N2 1.372(4) . ? C10 C11 1.402(5) . ? C11 C12 1.364(5) . ? C12 N3 1.407(4) . ? C12 C13 1.443(5) . ? C13 C14 1.357(5) . ? C13 C25 1.502(5) . ? C14 C15 1.438(5) . ? C14 C27 1.499(5) . ? C15 N3 1.324(5) . ? C15 C16 1.494(5) . ? C17 C18 1.522(6) . ? C19 C20 1.519(6) . ? C21 C22 1.519(6) . ? C23 C24 1.512(5) . ? C25 C26' 1.410(15) . ? C25 C26 1.426(7) . ? C27 C28 1.502(6) . ? C29 P 1.808(5) . ? C30 P 1.816(5) . ? C31 P 1.810(5) . ? C40 C45 1.393(4) . ? C40 C41 1.394(5) . ? C41 C42 1.380(5) . ? C42 C43 1.386(5) . ? C42 C46 1.492(6) . ? C43 C44 1.373(5) . ? C44 C45 1.381(5) . ? C44 C47 1.495(5) . ? C46 F1' 1.201(17) . ? C46 F2 1.227(10) . ? C46 F2' 1.25(2) . ? C46 F1 1.306(13) . ? C46 F3 1.396(12) . ? C46 F3' 1.460(15) . ? C47 F6' 1.150(19) . ? C47 F5' 1.18(2) . ? C47 F6 1.191(16) . ? C47 F4 1.389(16) . ? C47 F4' 1.419(15) . ? C47 F5 1.423(13) . ? C48 C49 1.389(5) . ? C48 C53 1.401(5) . ? C49 C50 1.399(5) . ? C50 C51 1.374(6) . ? C50 C54 1.490(6) . ? C51 C52 1.381(6) . ? C52 C53 1.391(5) . ? C52 C55 1.496(6) . ? C54 F8' 1.18(3) . ? C54 F9' 1.29(3) . ? C54 F8 1.300(11) . ? C54 F7' 1.31(2) . ? C54 F9 1.324(11) . ? C54 F7 1.330(12) . ? C55 F11' 1.152(19) . ? C55 F11 1.237(9) . ? C55 F12 1.327(13) . ? C55 F10 1.331(9) . ? C55 F12' 1.351(15) . ? C55 F10' 1.374(19) . ? C56 C61 1.388(5) . ? C56 C57 1.398(5) . ? C57 C58 1.383(5) . ? C58 C59 1.385(6) . ? C58 C62 1.494(6) . ? C59 C60 1.371(6) . ? C60 C61 1.386(5) . ? C60 C63 1.496(7) . ? C62 F14' 1.150(17) . ? C62 F13' 1.209(17) . ? C62 F14 1.247(10) . ? C62 F13 1.301(13) . ? C62 F15 1.394(11) . ? C62 F15' 1.414(13) . ? C63 F18' 0.91(3) . ? C63 F17' 1.06(2) . ? C63 F18 1.258(10) . ? C63 F16 1.382(9) . ? C63 F17 1.413(9) . ? C63 F16' 1.51(2) . ? C64 C69 1.392(5) . ? C64 C65 1.401(5) . ? C65 C66 1.384(5) . ? C66 C67 1.387(6) . ? C66 C70 1.491(7) . ? C67 C68 1.370(6) . ? C68 C69 1.392(5) . ? C68 C71 1.494(7) . ? C70 F20 1.250(7) . ? C70 F21 1.316(5) . ? C70 F19 1.356(6) . ? C71 F22 1.257(13) . ? C71 F24 1.261(9) . ? C71 F23 1.316(10) . ? C71 F23' 1.332(19) . ? C71 F22' 1.40(3) . ? C71 F24' 1.442(18) . ? F16' F18' 1.30(5) . ? F17' F18' 1.69(3) . ? N1 Pd 2.020(3) . ? N2 Pd 2.052(3) . ? N3 Pd 2.021(3) . ? P Pd 2.3136(12) . ? 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 C48 B C40 112.3(3) . . ? C48 B C56 111.0(3) . . ? C40 B C56 104.4(3) . . ? C48 B C64 105.3(3) . . ? C40 B C64 113.1(3) . . ? C56 B C64 111.0(3) . . ? N1 C2 C3 110.4(3) . . ? N1 C2 C1 123.4(4) . . ? C3 C2 C1 126.0(3) . . ? C4 C3 C2 106.9(3) . . ? C4 C3 C17 128.8(4) . . ? C2 C3 C17 124.3(4) . . ? C3 C4 C5 106.6(3) . . ? C3 C4 C19 129.1(3) . . ? C5 C4 C19 124.3(3) . . ? C6 C5 N1 124.1(3) . . ? C6 C5 C4 126.2(4) . . ? N1 C5 C4 109.1(3) . . ? C5 C6 C7 128.4(4) . . ? N2 C7 C6 123.8(3) . . ? N2 C7 C8 110.3(3) . . ? C6 C7 C8 125.6(3) . . ? C9 C8 C7 106.7(3) . . ? C9 C8 C21 128.0(3) . . ? C7 C8 C21 125.3(3) . . ? C8 C9 C10 106.5(3) . . ? C8 C9 C23 128.3(3) . . ? C10 C9 C23 124.9(3) . . ? N2 C10 C11 124.2(3) . . ? N2 C10 C9 110.0(3) . . ? C11 C10 C9 125.6(3) . . ? C12 C11 C10 128.1(3) . . ? C11 C12 N3 124.3(3) . . ? C11 C12 C13 126.7(3) . . ? N3 C12 C13 108.6(3) . . ? C14 C13 C12 107.2(3) . . ? C14 C13 C25 128.2(4) . . ? C12 C13 C25 124.6(3) . . ? C13 C14 C15 106.0(3) . . ? C13 C14 C27 129.4(4) . . ? C15 C14 C27 124.5(3) . . ? N3 C15 C14 112.2(3) . . ? N3 C15 C16 123.8(4) . . ? C14 C15 C16 123.7(3) . . ? C3 C17 C18 114.0(4) . . ? C4 C19 C20 111.1(4) . . ? C8 C21 C22 113.0(4) . . ? C9 C23 C24 112.0(3) . . ? C26' C25 C26 126.5(7) . . ? C26' C25 C13 117.4(7) . . ? C26 C25 C13 114.9(4) . . ? C14 C27 C28 112.5(3) . . ? C45 C40 C41 115.3(3) . . ? C45 C40 B 119.0(3) . . ? C41 C40 B 125.5(3) . . ? C42 C41 C40 122.4(3) . . ? C41 C42 C43 120.9(4) . . ? C41 C42 C46 120.6(4) . . ? C43 C42 C46 118.4(4) . . ? C44 C43 C42 117.7(4) . . ? C43 C44 C45 121.0(3) . . ? C43 C44 C47 118.5(4) . . ? C45 C44 C47 120.5(4) . . ? C44 C45 C40 122.6(3) . . ? F1' C46 F2 60.4(17) . . ? F1' C46 F2' 111.0(19) . . ? F2 C46 F2' 123.5(12) . . ? F1' C46 F1 121.9(13) . . ? F2 C46 F1 111.8(10) . . ? F2' C46 F1 20.1(13) . . ? F1' C46 F3 43.6(19) . . ? F2 C46 F3 103.3(8) . . ? F2' C46 F3 81.6(12) . . ? F1 C46 F3 100.5(9) . . ? F1' C46 F3' 104.1(18) . . ? F2 C46 F3' 46.0(9) . . ? F2' C46 F3' 96.3(13) . . ? F1 C46 F3' 77.2(12) . . ? F3 C46 F3' 140.8(9) . . ? F1' C46 C42 119.7(10) . . ? F2 C46 C42 115.8(6) . . ? F2' C46 C42 115.1(12) . . ? F1 C46 C42 114.6(7) . . ? F3 C46 C42 109.1(7) . . ? F3' C46 C42 107.2(7) . . ? F6' C47 F5' 101.1(16) . . ? F6' C47 F6 102.3(15) . . ? F5' C47 F6 94.7(15) . . ? F6' C47 F4 99.3(13) . . ? F5' C47 F4 10.2(18) . . ? F6 C47 F4 104.8(11) . . ? F6' C47 F4' 102.7(16) . . ? F5' C47 F4' 104.4(13) . . ? F6 C47 F4' 10.1(12) . . ? F4 C47 F4' 114.5(9) . . ? F6' C47 F5 9.5(16) . . ? F5' C47 F5 108.4(12) . . ? F6 C47 F5 107.2(11) . . ? F4 C47 F5 105.3(7) . . ? F4' C47 F5 106.1(7) . . ? F6' C47 C44 119.1(12) . . ? F5' C47 C44 116.7(12) . . ? F6 C47 C44 118.8(8) . . ? F4 C47 C44 110.0(8) . . ? F4' C47 C44 110.9(6) . . ? F5 C47 C44 109.7(7) . . ? C49 C48 C53 115.7(3) . . ? C49 C48 B 124.6(3) . . ? C53 C48 B 119.7(3) . . ? C48 C49 C50 122.4(4) . . ? C51 C50 C49 120.6(4) . . ? C51 C50 C54 120.1(4) . . ? C49 C50 C54 119.3(4) . . ? C50 C51 C52 118.6(4) . . ? C51 C52 C53 120.5(4) . . ? C51 C52 C55 120.0(4) . . ? C53 C52 C55 119.5(4) . . ? C52 C53 C48 122.3(4) . . ? F8' C54 F9' 110(2) . . ? F8' C54 F8 121.3(18) . . ? F9' C54 F8 23.3(14) . . ? F8' C54 F7' 110(2) . . ? F9' C54 F7' 97.6(16) . . ? F8 C54 F7' 74.5(14) . . ? F8' C54 F9 77.7(19) . . ? F9' C54 F9 126.5(11) . . ? F8 C54 F9 106.4(7) . . ? F7' C54 F9 37.1(14) . . ? F8' C54 F7 27(2) . . ? F9' C54 F7 88.1(16) . . ? F8 C54 F7 105.5(10) . . ? F7' C54 F7 130.5(14) . . ? F9 C54 F7 103.1(8) . . ? F8' C54 C50 116.7(14) . . ? F9' C54 C50 109.1(12) . . ? F8 C54 C50 114.3(6) . . ? F7' C54 C50 111.3(13) . . ? F9 C54 C50 113.5(7) . . ? F7 C54 C50 113.0(6) . . ? F11' C55 F11 121.8(11) . . ? F11' C55 F12 35(2) . . ? F11 C55 F12 107.5(9) . . ? F11' C55 F10 65(2) . . ? F11 C55 F10 108.4(7) . . ? F12 C55 F10 100.2(8) . . ? F11' C55 F12' 111.9(18) . . ? F11 C55 F12' 61.0(16) . . ? F12 C55 F12' 137.4(10) . . ? F10 C55 F12' 54.3(15) . . ? F11' C55 F10' 108.2(19) . . ? F11 C55 F10' 35.7(11) . . ? F12 C55 F10' 79.8(14) . . ? F10 C55 F10' 136.5(8) . . ? F12' C55 F10' 96.6(16) . . ? F11' C55 C52 119.6(11) . . ? F11 C55 C52 116.0(6) . . ? F12 C55 C52 111.6(7) . . ? F10 C55 C52 111.9(6) . . ? F12' C55 C52 109.8(8) . . ? F10' C55 C52 108.1(8) . . ? C61 C56 C57 115.5(3) . . ? C61 C56 B 122.5(3) . . ? C57 C56 B 121.9(3) . . ? C58 C57 C56 122.1(3) . . ? C57 C58 C59 120.7(4) . . ? C57 C58 C62 120.8(4) . . ? C59 C58 C62 118.5(4) . . ? C60 C59 C58 118.3(4) . . ? C59 C60 C61 120.5(4) . . ? C59 C60 C63 120.7(4) . . ? C61 C60 C63 118.8(4) . . ? C60 C61 C56 122.9(4) . . ? F14' C62 F13' 111.1(16) . . ? F14' C62 F14 125.3(11) . . ? F13' C62 F14 35(2) . . ? F14' C62 F13 42.5(17) . . ? F13' C62 F13 128.5(12) . . ? F14 C62 F13 113.6(10) . . ? F14' C62 F15 59(2) . . ? F13' C62 F15 69(3) . . ? F14 C62 F15 103.7(8) . . ? F13 C62 F15 101.5(9) . . ? F14' C62 F15' 98.2(15) . . ? F13' C62 F15' 95.8(19) . . ? F14 C62 F15' 62.8(12) . . ? F13 C62 F15' 59.9(10) . . ? F15 C62 F15' 142.3(7) . . ? F14' C62 C58 120.1(10) . . ? F13' C62 C58 117.7(11) . . ? F14 C62 C58 114.6(7) . . ? F13 C62 C58 113.2(6) . . ? F15 C62 C58 108.7(6) . . ? F15' C62 C58 108.9(6) . . ? F18' C63 F17' 118(2) . . ? F18' C63 F18 91(3) . . ? F17' C63 F18 47.4(18) . . ? F18' C63 F16 103(4) . . ? F17' C63 F16 61(3) . . ? F18 C63 F16 103.9(9) . . ? F18' C63 F17 26(3) . . ? F17' C63 F17 136(2) . . ? F18 C63 F17 116.3(9) . . ? F16 C63 F17 96.1(5) . . ? F18' C63 C60 125.7(18) . . ? F17' C63 C60 114.8(15) . . ? F18 C63 C60 116.9(7) . . ? F16 C63 C60 112.5(5) . . ? F17 C63 C60 109.1(6) . . ? F18' C63 F16' 59(3) . . ? F17' C63 F16' 100(2) . . ? F18 C63 F16' 52.5(11) . . ? F16 C63 F16' 146.6(9) . . ? F17 C63 F16' 78.8(14) . . ? C60 C63 F16' 100.2(8) . . ? C69 C64 C65 115.8(3) . . ? C69 C64 B 122.9(3) . . ? C65 C64 B 121.2(3) . . ? C66 C65 C64 122.2(4) . . ? C65 C66 C67 120.4(4) . . ? C65 C66 C70 121.1(5) . . ? C67 C66 C70 118.5(4) . . ? C68 C67 C66 118.6(4) . . ? C67 C68 C69 120.9(4) . . ? C67 C68 C71 120.5(4) . . ? C69 C68 C71 118.6(4) . . ? C68 C69 C64 122.0(4) . . ? F20 C70 F21 110.9(6) . . ? F20 C70 F19 106.3(5) . . ? F21 C70 F19 101.4(4) . . ? F20 C70 C66 115.0(4) . . ? F21 C70 C66 112.2(4) . . ? F19 C70 C66 110.0(5) . . ? F22 C71 F24 112.8(8) . . ? F22 C71 F23 109.7(7) . . ? F24 C71 F23 92.2(7) . . ? F22 C71 F23' 85.9(12) . . ? F24 C71 F23' 113.8(11) . . ? F23 C71 F23' 27.0(11) . . ? F22 C71 F22' 13.4(13) . . ? F24 C71 F22' 124.8(11) . . ? F23 C71 F22' 112.3(9) . . ? F23' C71 F22' 86.2(13) . . ? F22 C71 F24' 80.8(11) . . ? F24 C71 F24' 36.0(10) . . ? F23 C71 F24' 119.5(10) . . ? F23' C71 F24' 129.6(12) . . ? F22' C71 F24' 90.9(13) . . ? F22 C71 C68 116.7(5) . . ? F24 C71 C68 110.9(5) . . ? F23 C71 C68 112.0(7) . . ? F23' C71 C68 114.8(11) . . ? F22' C71 C68 104.5(10) . . ? F24' C71 C68 114.6(6) . . ? F18' F16' C63 36.9(15) . . ? C63 F17' F18' 28.4(13) . . ? C63 F18' F16' 84(2) . . ? C63 F18' F17' 33.7(11) . . ? F16' F18' F17' 82(2) . . ? C2 N1 C5 106.8(3) . . ? C2 N1 Pd 128.3(3) . . ? C5 N1 Pd 124.9(2) . . ? C7 N2 C10 106.4(3) . . ? C7 N2 Pd 125.1(2) . . ? C10 N2 Pd 124.9(2) . . ? C15 N3 C12 105.9(3) . . ? C15 N3 Pd 129.0(2) . . ? C12 N3 Pd 125.1(2) . . ? C29 P C31 103.4(2) . . ? C29 P C30 103.6(3) . . ? C31 P C30 102.7(3) . . ? C29 P Pd 105.40(19) . . ? C31 P Pd 106.46(17) . . ? C30 P Pd 132.2(2) . . ? N1 Pd N3 167.90(12) . . ? N1 Pd N2 89.86(12) . . ? N3 Pd N2 90.40(12) . . ? N1 Pd P 93.38(9) . . ? N3 Pd P 93.94(9) . . ? N2 Pd P 141.48(8) . . ? 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 N1 C2 C3 C4 2.1(4) . . . . ? C1 C2 C3 C4 -172.9(4) . . . . ? N1 C2 C3 C17 -178.9(3) . . . . ? C1 C2 C3 C17 6.1(6) . . . . ? C2 C3 C4 C5 0.8(4) . . . . ? C17 C3 C4 C5 -178.1(4) . . . . ? C2 C3 C4 C19 -179.2(4) . . . . ? C17 C3 C4 C19 1.9(7) . . . . ? C3 C4 C5 C6 167.8(4) . . . . ? C19 C4 C5 C6 -12.2(6) . . . . ? C3 C4 C5 N1 -3.4(4) . . . . ? C19 C4 C5 N1 176.6(3) . . . . ? N1 C5 C6 C7 -1.2(6) . . . . ? C4 C5 C6 C7 -171.1(4) . . . . ? C5 C6 C7 N2 0.2(6) . . . . ? C5 C6 C7 C8 -173.7(4) . . . . ? N2 C7 C8 C9 -1.6(4) . . . . ? C6 C7 C8 C9 173.0(3) . . . . ? N2 C7 C8 C21 -178.6(3) . . . . ? C6 C7 C8 C21 -3.9(6) . . . . ? C7 C8 C9 C10 0.2(4) . . . . ? C21 C8 C9 C10 177.1(4) . . . . ? C7 C8 C9 C23 -174.1(3) . . . . ? C21 C8 C9 C23 2.7(6) . . . . ? C8 C9 C10 N2 1.2(4) . . . . ? C23 C9 C10 N2 175.8(3) . . . . ? C8 C9 C10 C11 -174.3(3) . . . . ? C23 C9 C10 C11 0.2(6) . . . . ? N2 C10 C11 C12 -3.3(6) . . . . ? C9 C10 C11 C12 171.7(4) . . . . ? C10 C11 C12 N3 2.5(6) . . . . ? C10 C11 C12 C13 174.7(4) . . . . ? C11 C12 C13 C14 -170.9(4) . . . . ? N3 C12 C13 C14 2.4(4) . . . . ? C11 C12 C13 C25 8.1(6) . . . . ? N3 C12 C13 C25 -178.7(4) . . . . ? C12 C13 C14 C15 0.2(4) . . . . ? C25 C13 C14 C15 -178.7(4) . . . . ? C12 C13 C14 C27 -176.1(4) . . . . ? C25 C13 C14 C27 5.0(7) . . . . ? C13 C14 C15 N3 -2.9(4) . . . . ? C27 C14 C15 N3 173.6(3) . . . . ? C13 C14 C15 C16 170.9(4) . . . . ? C27 C14 C15 C16 -12.6(6) . . . . ? C4 C3 C17 C18 -61.6(6) . . . . ? C2 C3 C17 C18 119.7(4) . . . . ? C3 C4 C19 C20 105.0(5) . . . . ? C5 C4 C19 C20 -75.0(5) . . . . ? C9 C8 C21 C22 -94.4(5) . . . . ? C7 C8 C21 C22 81.8(5) . . . . ? C8 C9 C23 C24 95.0(5) . . . . ? C10 C9 C23 C24 -78.4(5) . . . . ? C14 C13 C25 C26' 79.2(9) . . . . ? C12 C13 C25 C26' -99.5(9) . . . . ? C14 C13 C25 C26 -112.9(5) . . . . ? C12 C13 C25 C26 68.4(6) . . . . ? C13 C14 C27 C28 101.9(5) . . . . ? C15 C14 C27 C28 -73.7(5) . . . . ? C48 B C40 C45 -49.2(4) . . . . ? C56 B C40 C45 71.1(4) . . . . ? C64 B C40 C45 -168.1(3) . . . . ? C48 B C40 C41 136.5(3) . . . . ? C56 B C40 C41 -103.2(4) . . . . ? C64 B C40 C41 17.6(4) . . . . ? C45 C40 C41 C42 1.8(5) . . . . ? B C40 C41 C42 176.3(3) . . . . ? C40 C41 C42 C43 -0.7(6) . . . . ? C40 C41 C42 C46 177.2(4) . . . . ? C41 C42 C43 C44 -0.6(6) . . . . ? C46 C42 C43 C44 -178.5(4) . . . . ? C42 C43 C44 C45 0.7(5) . . . . ? C42 C43 C44 C47 179.0(4) . . . . ? C43 C44 C45 C40 0.6(5) . . . . ? C47 C44 C45 C40 -177.7(3) . . . . ? C41 C40 C45 C44 -1.7(5) . . . . ? B C40 C45 C44 -176.6(3) . . . . ? C41 C42 C46 F1' -179(2) . . . . ? C43 C42 C46 F1' -1(3) . . . . ? C41 C42 C46 F2 -109.9(9) . . . . ? C43 C42 C46 F2 68.0(10) . . . . ? C41 C42 C46 F2' 44.7(13) . . . . ? C43 C42 C46 F2' -137.5(12) . . . . ? C41 C42 C46 F1 22.5(11) . . . . ? C43 C42 C46 F1 -159.7(9) . . . . ? C41 C42 C46 F3 134.2(7) . . . . ? C43 C42 C46 F3 -47.9(8) . . . . ? C41 C42 C46 F3' -61.1(13) . . . . ? C43 C42 C46 F3' 116.8(12) . . . . ? C43 C44 C47 F6' 50.4(16) . . . . ? C45 C44 C47 F6' -131.3(16) . . . . ? C43 C44 C47 F5' -71.4(14) . . . . ? C45 C44 C47 F5' 106.9(14) . . . . ? C43 C44 C47 F6 176.1(11) . . . . ? C45 C44 C47 F6 -5.5(12) . . . . ? C43 C44 C47 F4 -63.1(7) . . . . ? C45 C44 C47 F4 115.2(7) . . . . ? C43 C44 C47 F4' 169.2(6) . . . . ? C45 C44 C47 F4' -12.5(7) . . . . ? C43 C44 C47 F5 52.3(7) . . . . ? C45 C44 C47 F5 -129.4(6) . . . . ? C40 B C48 C49 -18.3(4) . . . . ? C56 B C48 C49 -134.7(3) . . . . ? C64 B C48 C49 105.1(4) . . . . ? C40 B C48 C53 164.2(3) . . . . ? C56 B C48 C53 47.8(4) . . . . ? C64 B C48 C53 -72.3(4) . . . . ? C53 C48 C49 C50 -1.5(5) . . . . ? B C48 C49 C50 -179.0(3) . . . . ? C48 C49 C50 C51 0.0(5) . . . . ? C48 C49 C50 C54 179.4(4) . . . . ? C49 C50 C51 C52 1.2(5) . . . . ? C54 C50 C51 C52 -178.2(4) . . . . ? C50 C51 C52 C53 -0.8(6) . . . . ? C50 C51 C52 C55 -179.7(4) . . . . ? C51 C52 C53 C48 -0.7(6) . . . . ? C55 C52 C53 C48 178.2(4) . . . . ? C49 C48 C53 C52 1.8(5) . . . . ? B C48 C53 C52 179.5(3) . . . . ? C51 C50 C54 F8' -116(2) . . . . ? C49 C50 C54 F8' 64(2) . . . . ? C51 C50 C54 F9' 118.2(14) . . . . ? C49 C50 C54 F9' -61.2(15) . . . . ? C51 C50 C54 F8 93.7(8) . . . . ? C49 C50 C54 F8 -85.7(8) . . . . ? C51 C50 C54 F7' 11.7(17) . . . . ? C49 C50 C54 F7' -167.7(17) . . . . ? C51 C50 C54 F9 -28.5(8) . . . . ? C49 C50 C54 F9 152.1(7) . . . . ? C51 C50 C54 F7 -145.5(8) . . . . ? C49 C50 C54 F7 35.1(9) . . . . ? C51 C52 C55 F11' -108(3) . . . . ? C53 C52 C55 F11' 73(3) . . . . ? C51 C52 C55 F11 89.7(10) . . . . ? C53 C52 C55 F11 -89.2(10) . . . . ? C51 C52 C55 F12 -146.7(9) . . . . ? C53 C52 C55 F12 34.4(10) . . . . ? C51 C52 C55 F10 -35.4(11) . . . . ? C53 C52 C55 F10 145.7(9) . . . . ? C51 C52 C55 F12' 23(2) . . . . ? C53 C52 C55 F12' -156(2) . . . . ? C51 C52 C55 F10' 127.4(16) . . . . ? C53 C52 C55 F10' -51.5(17) . . . . ? C48 B C56 C61 22.1(4) . . . . ? C40 B C56 C61 -99.0(4) . . . . ? C64 B C56 C61 138.8(3) . . . . ? C48 B C56 C57 -162.4(3) . . . . ? C40 B C56 C57 76.4(4) . . . . ? C64 B C56 C57 -45.7(4) . . . . ? C61 C56 C57 C58 -2.6(5) . . . . ? B C56 C57 C58 -178.4(3) . . . . ? C56 C57 C58 C59 1.6(6) . . . . ? C56 C57 C58 C62 -177.8(4) . . . . ? C57 C58 C59 C60 0.1(6) . . . . ? C62 C58 C59 C60 179.6(5) . . . . ? C58 C59 C60 C61 -0.6(6) . . . . ? C58 C59 C60 C63 179.5(5) . . . . ? C59 C60 C61 C56 -0.5(6) . . . . ? C63 C60 C61 C56 179.3(5) . . . . ? C57 C56 C61 C60 2.1(5) . . . . ? B C56 C61 C60 177.8(3) . . . . ? C57 C58 C62 F14' -55(3) . . . . ? C59 C58 C62 F14' 126(3) . . . . ? C57 C58 C62 F13' 165(3) . . . . ? C59 C58 C62 F13' -15(3) . . . . ? C57 C58 C62 F14 125.2(11) . . . . ? C59 C58 C62 F14 -54.2(12) . . . . ? C57 C58 C62 F13 -7.3(14) . . . . ? C59 C58 C62 F13 173.2(12) . . . . ? C57 C58 C62 F15 -119.3(8) . . . . ? C59 C58 C62 F15 61.3(10) . . . . ? C57 C58 C62 F15' 57.3(18) . . . . ? C59 C58 C62 F15' -122.2(18) . . . . ? C59 C60 C63 F18' -84(5) . . . . ? C61 C60 C63 F18' 96(5) . . . . ? C59 C60 C63 F17' 81(3) . . . . ? C61 C60 C63 F17' -98(3) . . . . ? C59 C60 C63 F18 28.5(14) . . . . ? C61 C60 C63 F18 -151.4(11) . . . . ? C59 C60 C63 F16 148.6(6) . . . . ? C61 C60 C63 F16 -31.3(9) . . . . ? C59 C60 C63 F17 -106.0(6) . . . . ? C61 C60 C63 F17 74.1(6) . . . . ? C59 C60 C63 F16' -24.5(17) . . . . ? C61 C60 C63 F16' 155.7(14) . . . . ? C48 B C64 C69 98.0(4) . . . . ? C40 B C64 C69 -139.0(3) . . . . ? C56 B C64 C69 -22.1(5) . . . . ? C48 B C64 C65 -78.4(4) . . . . ? C40 B C64 C65 44.5(4) . . . . ? C56 B C64 C65 161.4(3) . . . . ? C69 C64 C65 C66 2.2(5) . . . . ? B C64 C65 C66 178.9(3) . . . . ? C64 C65 C66 C67 -1.0(6) . . . . ? C64 C65 C66 C70 176.9(4) . . . . ? C65 C66 C67 C68 -1.0(6) . . . . ? C70 C66 C67 C68 -178.9(4) . . . . ? C66 C67 C68 C69 1.5(6) . . . . ? C66 C67 C68 C71 179.5(4) . . . . ? C67 C68 C69 C64 -0.2(6) . . . . ? C71 C68 C69 C64 -178.2(3) . . . . ? C65 C64 C69 C68 -1.6(5) . . . . ? B C64 C69 C68 -178.3(3) . . . . ? C65 C66 C70 F20 8.5(7) . . . . ? C67 C66 C70 F20 -173.6(5) . . . . ? C65 C66 C70 F21 -119.4(5) . . . . ? C67 C66 C70 F21 58.5(6) . . . . ? C65 C66 C70 F19 128.4(5) . . . . ? C67 C66 C70 F19 -53.7(6) . . . . ? C67 C68 C71 F22 124.2(8) . . . . ? C69 C68 C71 F22 -57.8(8) . . . . ? C67 C68 C71 F24 -104.9(6) . . . . ? C69 C68 C71 F24 73.2(7) . . . . ? C67 C68 C71 F23 -3.5(7) . . . . ? C69 C68 C71 F23 174.6(5) . . . . ? C67 C68 C71 F23' 25.9(13) . . . . ? C69 C68 C71 F23' -156.1(12) . . . . ? C67 C68 C71 F22' 118.4(9) . . . . ? C69 C68 C71 F22' -63.6(10) . . . . ? C67 C68 C71 F24' -143.9(11) . . . . ? C69 C68 C71 F24' 34.2(12) . . . . ? F17' C63 F16' F18' 117(3) . . . . ? F18 C63 F16' F18' 118(2) . . . . ? F16 C63 F16' F18' 66(4) . . . . ? F17 C63 F16' F18' -18(2) . . . . ? C60 C63 F16' F18' -126(2) . . . . ? F18 C63 F17' F18' -62(5) . . . . ? F16 C63 F17' F18' 90(4) . . . . ? F17 C63 F17' F18' 24(5) . . . . ? C60 C63 F17' F18' -167(4) . . . . ? F16' C63 F17' F18' -60(4) . . . . ? F17' C63 F18' F16' -85(4) . . . . ? F18 C63 F18' F16' -44.4(16) . . . . ? F16 C63 F18' F16' -148.8(19) . . . . ? F17 C63 F18' F16' 135(8) . . . . ? C60 C63 F18' F16' 80(3) . . . . ? F18 C63 F18' F17' 40(3) . . . . ? F16 C63 F18' F17' -64(3) . . . . ? F17 C63 F18' F17' -140(6) . . . . ? C60 C63 F18' F17' 165(5) . . . . ? F16' C63 F18' F17' 85(4) . . . . ? C63 F16' F18' F17' -33.9(12) . . . . ? C63 F17' F18' F16' 91(4) . . . . ? C3 C2 N1 C5 -4.2(4) . . . . ? C1 C2 N1 C5 171.0(3) . . . . ? C3 C2 N1 Pd 173.9(2) . . . . ? C1 C2 N1 Pd -10.9(5) . . . . ? C6 C5 N1 C2 -166.7(3) . . . . ? C4 C5 N1 C2 4.7(4) . . . . ? C6 C5 N1 Pd 15.1(5) . . . . ? C4 C5 N1 Pd -173.5(2) . . . . ? C6 C7 N2 C10 -172.4(3) . . . . ? C8 C7 N2 C10 2.4(4) . . . . ? C6 C7 N2 Pd -13.0(5) . . . . ? C8 C7 N2 Pd 161.7(2) . . . . ? C11 C10 N2 C7 173.4(3) . . . . ? C9 C10 N2 C7 -2.2(4) . . . . ? C11 C10 N2 Pd 14.0(5) . . . . ? C9 C10 N2 Pd -161.6(2) . . . . ? C14 C15 N3 C12 4.3(4) . . . . ? C16 C15 N3 C12 -169.5(4) . . . . ? C14 C15 N3 Pd -173.5(2) . . . . ? C16 C15 N3 Pd 12.7(6) . . . . ? C11 C12 N3 C15 169.4(4) . . . . ? C13 C12 N3 C15 -4.1(4) . . . . ? C11 C12 N3 Pd -12.7(5) . . . . ? C13 C12 N3 Pd 173.9(2) . . . . ? C2 N1 Pd N3 71.2(7) . . . . ? C5 N1 Pd N3 -111.0(6) . . . . ? C2 N1 Pd N2 162.4(3) . . . . ? C5 N1 Pd N2 -19.8(3) . . . . ? C2 N1 Pd P -56.0(3) . . . . ? C5 N1 Pd P 121.8(3) . . . . ? C15 N3 Pd N1 -74.6(7) . . . . ? C12 N3 Pd N1 107.9(6) . . . . ? C15 N3 Pd N2 -165.8(3) . . . . ? C12 N3 Pd N2 16.7(3) . . . . ? C15 N3 Pd P 52.5(3) . . . . ? C12 N3 Pd P -125.0(3) . . . . ? C7 N2 Pd N1 19.0(3) . . . . ? C10 N2 Pd N1 174.6(3) . . . . ? C7 N2 Pd N3 -173.1(3) . . . . ? C10 N2 Pd N3 -17.4(3) . . . . ? C7 N2 Pd P -76.3(3) . . . . ? C10 N2 Pd P 79.4(3) . . . . ? C29 P Pd N1 -145.8(2) . . . . ? C31 P Pd N1 -36.47(19) . . . . ? C30 P Pd N1 88.9(3) . . . . ? C29 P Pd N3 43.8(2) . . . . ? C31 P Pd N3 153.17(18) . . . . ? C30 P Pd N3 -81.5(3) . . . . ? C29 P Pd N2 -51.8(3) . . . . ? C31 P Pd N2 57.6(2) . . . . ? C30 P Pd N2 -177.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.847 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.081