# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Marc D. Walter' _publ_contact_author_email mdwalter@email.unc.edu loop_ _publ_author_name 'Marc D. Walter' 'Peter S. White' 'Maurice Brookhart' data_c09205 _database_code_depnum_ccdc_archive 'CCDC 743856' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C21 H39 N2 Pd' _chemical_formula_sum 'C53 H51 B F24 N2 Pd' _chemical_formula_weight 1289.17 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' B B 0.0090 0.0039 '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' Pd Pd 0.1215 3.9337 '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 ' _symmetry_space_group_name_Hall '-P 2ybc' 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 12.9847(3) _cell_length_b 31.1704(6) _cell_length_c 17.3760(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.9810(10) _cell_angle_gamma 90.00 _cell_volume 6609.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9363 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 70.75 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 3.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4500 _exptl_absorpt_correction_T_max 0.5048 _exptl_absorpt_process_details '(Blessing, 1995)' _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81207 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 71.67 _reflns_number_total 12241 _reflns_number_gt 11021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. ; _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^)+(0.0898P)^2^+16.8136P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12241 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1670 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7946(4) 0.35404(19) 0.2382(3) 0.0508(13) Uani 1 1 d . . . H1A H 0.7739 0.3636 0.2846 0.076 Uiso 1 1 calc R . . H1B H 0.7602 0.3263 0.2186 0.076 Uiso 1 1 calc R . . H1C H 0.7698 0.3752 0.1939 0.076 Uiso 1 1 calc R . . C2 C 0.9478(4) 0.31412(16) 0.3237(3) 0.0457(11) Uani 1 1 d . . . H2A H 0.9238 0.3202 0.3703 0.069 Uiso 1 1 calc R . . H2B H 1.0278 0.3113 0.3430 0.069 Uiso 1 1 calc R . . H2C H 0.9143 0.2873 0.2974 0.069 Uiso 1 1 calc R . . C3 C 0.9666(4) 0.39046(15) 0.3019(3) 0.0432(11) Uani 1 1 d . . . H3A H 0.9200 0.4148 0.2733 0.052 Uiso 1 1 calc R . . H3B H 0.9708 0.3912 0.3598 0.052 Uiso 1 1 calc R . . C4 C 1.0757(4) 0.39608(17) 0.2984(3) 0.0528(13) Uani 1 1 d . . . H4A H 1.1249 0.3739 0.3328 0.063 Uiso 1 1 calc R . . H4B H 1.1042 0.4246 0.3210 0.063 Uiso 1 1 calc R . . C5 C 1.0202(6) 0.42976(17) 0.1632(4) 0.0670(17) Uani 1 1 d . . . H5A H 1.0536 0.4561 0.1915 0.101 Uiso 1 1 calc R . . H5B H 0.9425 0.4290 0.1575 0.101 Uiso 1 1 calc R . . H5C H 1.0271 0.4290 0.1088 0.101 Uiso 1 1 calc R . . C6 C 1.1897(4) 0.39215(18) 0.2182(4) 0.0644(16) Uani 1 1 d . . . H6A H 1.1961 0.3880 0.1641 0.097 Uiso 1 1 calc R . . H6B H 1.2270 0.3686 0.2545 0.097 Uiso 1 1 calc R . . H6C H 1.2237 0.4195 0.2412 0.097 Uiso 1 1 calc R . . C7 C 0.7960(4) 0.35617(15) -0.0444(3) 0.0433(10) Uani 1 1 d . . . H7A H 0.7975 0.3397 -0.0921 0.065 Uiso 1 1 calc R . . H7B H 0.8670 0.3702 -0.0185 0.065 Uiso 1 1 calc R . . H7C H 0.7383 0.3780 -0.0620 0.065 Uiso 1 1 calc R . . C8 C 0.7729(3) 0.32611(14) 0.0165(3) 0.0328(9) Uani 1 1 d . . . C9 C 0.8629(3) 0.29016(12) 0.0555(2) 0.0285(8) Uani 1 1 d . . . C10 C 0.7934(3) 0.24852(13) 0.0364(3) 0.0322(8) Uani 1 1 d . . . H10 H 0.8367 0.2215 0.0408 0.039 Uiso 1 1 calc R . . C11 C 0.7145(3) 0.24839(14) 0.0860(3) 0.0340(9) Uani 1 1 d . . . H11A H 0.7534 0.2566 0.1437 0.041 Uiso 1 1 calc R . . H11B H 0.6811 0.2197 0.0846 0.041 Uiso 1 1 calc R . . C12 C 0.6262(3) 0.28229(15) 0.0419(3) 0.0408(10) Uani 1 1 d . . . H12A H 0.5531 0.2689 0.0174 0.049 Uiso 1 1 calc R . . H12B H 0.6219 0.3053 0.0800 0.049 Uiso 1 1 calc R . . C13 C 0.6682(3) 0.29943(14) -0.0237(3) 0.0367(9) Uani 1 1 d . . . H13 H 0.6113 0.3144 -0.0697 0.044 Uiso 1 1 calc R . . C14 C 0.7148(4) 0.25875(15) -0.0500(3) 0.0394(10) Uani 1 1 d . . . H14A H 0.6587 0.2362 -0.0721 0.047 Uiso 1 1 calc R . . H14B H 0.7534 0.2648 -0.0891 0.047 Uiso 1 1 calc R . . C15 C 0.9621(3) 0.29009(13) 0.0258(3) 0.0302(8) Uani 1 1 d . . . C16 C 1.0465(3) 0.32388(13) 0.0760(2) 0.0305(8) Uani 1 1 d . . . C17 C 1.1538(3) 0.29929(13) 0.1095(3) 0.0355(9) Uani 1 1 d . . . H17 H 1.2111 0.3132 0.1568 0.043 Uiso 1 1 calc R . . C18 C 1.1900(4) 0.28877(16) 0.0352(3) 0.0436(11) Uani 1 1 d . . . H18A H 1.1835 0.3142 -0.0002 0.052 Uiso 1 1 calc R . . H18B H 1.2665 0.2782 0.0533 0.052 Uiso 1 1 calc R . . C19 C 1.1089(4) 0.25346(17) -0.0093(3) 0.0449(11) Uani 1 1 d . . . H19A H 1.0668 0.2621 -0.0662 0.054 Uiso 1 1 calc R . . H19B H 1.1478 0.2263 -0.0104 0.054 Uiso 1 1 calc R . . C20 C 1.0335(3) 0.24868(13) 0.0415(3) 0.0342(9) Uani 1 1 d . . . H20 H 0.9914 0.2212 0.0328 0.041 Uiso 1 1 calc R . . C21 C 1.1147(3) 0.25519(14) 0.1278(3) 0.0362(9) Uani 1 1 d . . . H21A H 1.1739 0.2335 0.1433 0.043 Uiso 1 1 calc R . . H21B H 1.0788 0.2565 0.1697 0.043 Uiso 1 1 calc R . . C22 C 0.4135(3) 0.10987(11) 0.4159(2) 0.0257(8) Uani 1 1 d . . . C23 C 0.4057(3) 0.12421(12) 0.4897(2) 0.0270(8) Uani 1 1 d . . . H23 H 0.3492 0.1439 0.4882 0.032 Uiso 1 1 calc R . . C24 C 0.4781(3) 0.11067(12) 0.5660(2) 0.0288(8) Uani 1 1 d . . . C25 C 0.4620(3) 0.12480(15) 0.6434(3) 0.0380(10) Uani 1 1 d . . . C26 C 0.5613(3) 0.08228(12) 0.5695(2) 0.0290(8) Uani 1 1 d . . . H26 H 0.6098 0.0723 0.6207 0.035 Uiso 1 1 calc R . . C27 C 0.5727(3) 0.06889(12) 0.4978(2) 0.0291(8) Uani 1 1 d . . . C28 C 0.6633(4) 0.03756(15) 0.5033(3) 0.0402(10) Uani 1 1 d . . . C29 C 0.5003(3) 0.08224(12) 0.4215(3) 0.0283(8) Uani 1 1 d . . . H29 H 0.5103 0.0723 0.3729 0.034 Uiso 1 1 calc R . . C30 C 0.3106(3) 0.09575(11) 0.2512(2) 0.0261(8) Uani 1 1 d . . . C31 C 0.3107(4) 0.05106(13) 0.2591(3) 0.0369(9) Uani 1 1 d . . . H31 H 0.3253 0.0389 0.3119 0.044 Uiso 1 1 calc R . . C32 C 0.2902(4) 0.02400(14) 0.1919(3) 0.0448(11) Uani 1 1 d . . . C33 C 0.2915(7) -0.02390(18) 0.2061(3) 0.072(2) Uani 1 1 d . . . C34 C 0.2699(4) 0.04016(14) 0.1141(3) 0.0428(11) Uani 1 1 d . . . H34 H 0.2590 0.0216 0.0686 0.051 Uiso 1 1 calc R . . C35 C 0.2661(4) 0.08393(14) 0.1048(3) 0.0436(11) Uani 1 1 d . . . C36 C 0.2418(7) 0.10238(18) 0.0206(3) 0.075(2) Uani 1 1 d . . . C37 C 0.2849(3) 0.11079(12) 0.1714(3) 0.0330(9) Uani 1 1 d . . . H37 H 0.2801 0.1409 0.1623 0.040 Uiso 1 1 calc R . . C38 C 0.3601(3) 0.17565(12) 0.3157(2) 0.0246(7) Uani 1 1 d . . . C39 C 0.4356(3) 0.18345(12) 0.2760(2) 0.0251(7) Uani 1 1 d . . . H39 H 0.4630 0.1598 0.2544 0.030 Uiso 1 1 calc R . . C40 C 0.4718(3) 0.22419(12) 0.2669(2) 0.0260(7) Uani 1 1 d . . . C41 C 0.5473(3) 0.22990(14) 0.2189(3) 0.0342(9) Uani 1 1 d . . . C42 C 0.4370(3) 0.25971(12) 0.2997(2) 0.0261(8) Uani 1 1 d . . . H42 H 0.4605 0.2878 0.2928 0.031 Uiso 1 1 calc R . . C43 C 0.3671(3) 0.25253(11) 0.3428(2) 0.0253(7) Uani 1 1 d . . . C44 C 0.3302(3) 0.28941(12) 0.3823(3) 0.0322(9) Uani 1 1 d . . . C45 C 0.3289(3) 0.21177(11) 0.3505(2) 0.0239(7) Uani 1 1 d . . . H45 H 0.2801 0.2082 0.3802 0.029 Uiso 1 1 calc R . . C46 C 0.1996(3) 0.12512(11) 0.3378(2) 0.0250(7) Uani 1 1 d . . . C47 C 0.1132(3) 0.15254(12) 0.2940(2) 0.0274(8) Uani 1 1 d . . . H47 H 0.1273 0.1750 0.2621 0.033 Uiso 1 1 calc R . . C48 C 0.0081(3) 0.14753(13) 0.2963(2) 0.0298(8) Uani 1 1 d . . . C49 C -0.0815(3) 0.17751(14) 0.2495(3) 0.0341(9) Uani 1 1 d . . . C50 C -0.0164(3) 0.11458(12) 0.3418(3) 0.0326(9) Uani 1 1 d . . . H50 H -0.0883 0.1112 0.3433 0.039 Uiso 1 1 calc R . . C51 C 0.0666(3) 0.08708(12) 0.3843(3) 0.0333(9) Uani 1 1 d . . . C52 C 0.0462(5) 0.05032(15) 0.4324(4) 0.0562(15) Uani 1 1 d . . . C53 C 0.1722(3) 0.09254(12) 0.3822(2) 0.0277(8) Uani 1 1 d . . . H53 H 0.2279 0.0732 0.4124 0.033 Uiso 1 1 calc R . . B1 B 0.3223(3) 0.12700(13) 0.3295(3) 0.0245(8) Uani 1 1 d . . . N1 N 0.9140(3) 0.34964(11) 0.2641(2) 0.0332(7) Uani 1 1 d . . . N2 N 1.0759(3) 0.39262(11) 0.2105(2) 0.0345(8) Uani 1 1 d . . . F1 F 0.4100(3) 0.16212(12) 0.6355(2) 0.0810(13) Uani 1 1 d . . . F2 F 0.4035(3) 0.09636(15) 0.6685(2) 0.0875(13) Uani 1 1 d . . . F3 F 0.5544(2) 0.12929(10) 0.70492(16) 0.0517(7) Uani 1 1 d . . . F4 F 0.6512(3) 0.00100(10) 0.5350(3) 0.0820(12) Uani 1 1 d . . . F5 F 0.7612(3) 0.05270(12) 0.5531(3) 0.0760(11) Uani 1 1 d . . . F6 F 0.6802(3) 0.03203(13) 0.4335(2) 0.0825(12) Uani 1 1 d . . . F7 F 0.2434(3) -0.03464(10) 0.2599(2) 0.0764(11) Uani 1 1 d . . . F8 F 0.2397(6) -0.04530(11) 0.1389(2) 0.143(3) Uani 1 1 d . . . F9 F 0.3963(5) -0.03816(13) 0.2403(3) 0.1114(18) Uani 1 1 d . . . F10 F 0.1570(7) 0.1257(3) -0.0017(3) 0.188(4) Uani 1 1 d . . . F11 F 0.2436(8) 0.07555(15) -0.0338(3) 0.176(4) Uani 1 1 d . . . F12 F 0.3138(10) 0.1304(2) 0.0173(4) 0.215(5) Uani 1 1 d . . . F13 F 0.4952(3) 0.22850(13) 0.13952(18) 0.0682(10) Uani 1 1 d . . . F14 F 0.6232(3) 0.19942(11) 0.2351(2) 0.0650(9) Uani 1 1 d . . . F15 F 0.6027(3) 0.26657(10) 0.2355(2) 0.0571(8) Uani 1 1 d . . . F16 F 0.3734(2) 0.32688(8) 0.3730(2) 0.0518(7) Uani 1 1 d . . . F17 F 0.3513(3) 0.28315(9) 0.46221(17) 0.0530(7) Uani 1 1 d . . . F18 F 0.2201(2) 0.29479(9) 0.3506(2) 0.0538(7) Uani 1 1 d . . . F19 F -0.0534(3) 0.20507(16) 0.2047(3) 0.110(2) Uani 1 1 d . . . F20 F -0.1704(3) 0.15786(12) 0.2033(3) 0.0957(16) Uani 1 1 d . . . F21 F -0.1181(3) 0.20137(11) 0.2992(2) 0.0703(10) Uani 1 1 d . . . F22 F -0.0502(3) 0.05248(10) 0.4425(3) 0.0717(11) Uani 1 1 d . . . F23 F 0.1238(3) 0.04874(13) 0.5104(3) 0.0827(12) Uani 1 1 d . . . F24 F 0.0571(4) 0.01359(9) 0.4027(3) 0.0850(13) Uani 1 1 d . . . Pd1 Pd 0.98120(2) 0.337858(8) 0.163015(17) 0.02643(11) Uani 1 1 d . . . H100 H 0.771(5) 0.3431(17) 0.060(4) 0.050(15) Uiso 1 1 d . . . H101 H 0.889(5) 0.2909(18) 0.117(4) 0.055(16) Uiso 1 1 d . . . H102 H 0.935(5) 0.296(2) -0.036(4) 0.067(18) Uiso 1 1 d . . . H103 H 1.045(5) 0.352(2) 0.041(4) 0.067(18) 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 C1 0.033(2) 0.067(3) 0.047(3) -0.017(2) 0.007(2) 0.011(2) C2 0.055(3) 0.051(3) 0.035(2) 0.009(2) 0.020(2) 0.013(2) C3 0.049(3) 0.043(2) 0.033(2) -0.0072(18) 0.007(2) 0.004(2) C4 0.054(3) 0.048(3) 0.047(3) -0.011(2) 0.005(2) 0.004(2) C5 0.079(4) 0.039(3) 0.063(4) 0.007(2) -0.001(3) -0.002(3) C6 0.045(3) 0.045(3) 0.096(5) -0.019(3) 0.013(3) -0.010(2) C7 0.044(3) 0.039(2) 0.044(3) 0.0087(19) 0.012(2) 0.0018(19) C8 0.030(2) 0.035(2) 0.029(2) 0.0036(17) 0.0049(16) 0.0031(16) C9 0.0223(18) 0.033(2) 0.027(2) 0.0025(15) 0.0041(15) -0.0024(14) C10 0.0276(19) 0.035(2) 0.032(2) 0.0000(16) 0.0065(16) -0.0044(16) C11 0.0262(19) 0.041(2) 0.033(2) 0.0028(17) 0.0073(16) -0.0010(16) C12 0.023(2) 0.049(3) 0.045(3) 0.003(2) 0.0061(18) 0.0012(18) C13 0.0234(19) 0.047(2) 0.031(2) 0.0051(17) -0.0022(16) 0.0013(17) C14 0.033(2) 0.044(2) 0.034(2) -0.0017(18) 0.0025(18) -0.0070(18) C15 0.0274(19) 0.035(2) 0.028(2) 0.0004(16) 0.0082(16) -0.0022(15) C16 0.030(2) 0.031(2) 0.029(2) -0.0016(15) 0.0080(16) -0.0055(16) C17 0.0252(19) 0.037(2) 0.043(2) -0.0068(18) 0.0096(17) -0.0032(16) C18 0.034(2) 0.053(3) 0.050(3) -0.013(2) 0.022(2) -0.0103(19) C19 0.036(2) 0.055(3) 0.048(3) -0.018(2) 0.020(2) -0.006(2) C20 0.032(2) 0.033(2) 0.040(2) -0.0077(17) 0.0140(17) -0.0039(16) C21 0.029(2) 0.039(2) 0.042(2) 0.0027(18) 0.0141(18) 0.0032(17) C22 0.0260(18) 0.0171(16) 0.032(2) 0.0084(14) 0.0075(15) -0.0001(13) C23 0.0255(18) 0.0237(18) 0.030(2) 0.0042(14) 0.0076(15) 0.0017(14) C24 0.0250(18) 0.0278(19) 0.031(2) 0.0048(15) 0.0065(15) 0.0010(14) C25 0.029(2) 0.050(3) 0.033(2) 0.0027(18) 0.0070(17) 0.0073(18) C26 0.0221(18) 0.0294(19) 0.030(2) 0.0062(15) 0.0011(15) 0.0020(14) C27 0.0260(18) 0.0262(18) 0.033(2) 0.0086(15) 0.0074(15) 0.0064(14) C28 0.038(2) 0.042(2) 0.036(2) 0.0088(18) 0.0084(18) 0.0194(19) C29 0.0267(18) 0.0252(18) 0.033(2) 0.0055(15) 0.0098(15) 0.0039(14) C30 0.0232(17) 0.0229(18) 0.031(2) 0.0071(14) 0.0077(15) 0.0005(13) C31 0.052(3) 0.025(2) 0.031(2) 0.0070(15) 0.0115(19) 0.0046(17) C32 0.064(3) 0.029(2) 0.036(2) 0.0058(17) 0.010(2) 0.004(2) C33 0.132(6) 0.041(3) 0.036(3) -0.007(2) 0.019(3) 0.010(3) C34 0.060(3) 0.032(2) 0.031(2) -0.0020(17) 0.009(2) 0.002(2) C35 0.055(3) 0.036(2) 0.032(2) 0.0080(18) 0.004(2) -0.007(2) C36 0.128(6) 0.038(3) 0.037(3) 0.012(2) 0.001(3) -0.008(3) C37 0.034(2) 0.0244(19) 0.035(2) 0.0084(15) 0.0051(17) -0.0012(15) C38 0.0196(16) 0.0244(17) 0.0277(19) 0.0097(14) 0.0054(14) 0.0037(13) C39 0.0229(17) 0.0250(18) 0.0267(19) 0.0021(14) 0.0075(14) 0.0036(13) C40 0.0188(17) 0.0332(19) 0.0244(19) 0.0037(14) 0.0053(14) 0.0004(14) C41 0.029(2) 0.039(2) 0.038(2) 0.0058(17) 0.0148(17) -0.0035(16) C42 0.0230(17) 0.0270(18) 0.0242(19) 0.0089(14) 0.0027(14) -0.0006(14) C43 0.0200(17) 0.0248(18) 0.0281(19) 0.0057(14) 0.0044(14) 0.0048(13) C44 0.032(2) 0.0228(18) 0.043(2) 0.0024(16) 0.0139(17) 0.0045(15) C45 0.0202(16) 0.0251(17) 0.0272(19) 0.0067(14) 0.0089(14) 0.0022(13) C46 0.0250(18) 0.0217(17) 0.0279(19) 0.0017(14) 0.0086(14) 0.0003(13) C47 0.0249(18) 0.0283(18) 0.028(2) 0.0066(15) 0.0079(15) -0.0016(14) C48 0.0272(19) 0.0306(19) 0.029(2) -0.0002(15) 0.0063(15) -0.0003(15) C49 0.0225(19) 0.044(2) 0.035(2) 0.0048(18) 0.0091(16) -0.0004(16) C50 0.0283(19) 0.030(2) 0.046(2) -0.0027(17) 0.0208(17) -0.0026(15) C51 0.038(2) 0.0223(18) 0.048(3) 0.0027(16) 0.0254(19) 0.0005(15) C52 0.056(3) 0.029(2) 0.104(5) 0.015(3) 0.055(3) 0.005(2) C53 0.0305(19) 0.0234(18) 0.031(2) 0.0065(14) 0.0133(16) 0.0043(14) B1 0.0220(19) 0.0231(19) 0.029(2) 0.0091(16) 0.0088(16) 0.0032(15) N1 0.0355(18) 0.0331(17) 0.0296(18) -0.0026(14) 0.0090(14) 0.0096(14) N2 0.0349(18) 0.0257(16) 0.0373(19) -0.0032(13) 0.0052(15) -0.0018(13) F1 0.097(3) 0.094(3) 0.0387(17) -0.0049(16) 0.0071(17) 0.066(2) F2 0.094(3) 0.129(3) 0.058(2) -0.031(2) 0.051(2) -0.057(3) F3 0.0396(14) 0.0702(19) 0.0354(14) -0.0088(13) -0.0001(11) 0.0093(13) F4 0.089(3) 0.0394(17) 0.138(4) 0.0387(19) 0.065(3) 0.0336(17) F5 0.0409(17) 0.076(2) 0.099(3) -0.001(2) 0.0073(17) 0.0237(16) F6 0.090(3) 0.099(3) 0.064(2) 0.0174(19) 0.0335(19) 0.066(2) F7 0.108(3) 0.0359(16) 0.065(2) 0.0145(14) 0.003(2) -0.0225(17) F8 0.317(8) 0.0339(18) 0.048(2) -0.0081(15) 0.023(3) -0.014(3) F9 0.190(5) 0.059(2) 0.111(3) 0.040(2) 0.084(4) 0.071(3) F10 0.222(8) 0.260(9) 0.068(3) 0.095(5) 0.032(4) 0.130(7) F11 0.410(12) 0.073(3) 0.043(2) 0.007(2) 0.073(4) 0.021(5) F12 0.407(15) 0.158(6) 0.088(4) 0.039(4) 0.095(6) -0.110(8) F13 0.0524(17) 0.125(3) 0.0336(16) 0.0009(17) 0.0224(13) -0.0203(18) F14 0.0533(17) 0.0643(19) 0.099(3) 0.0233(18) 0.0545(18) 0.0169(15) F15 0.0620(18) 0.0542(17) 0.070(2) -0.0075(14) 0.0420(16) -0.0278(14) F16 0.0613(18) 0.0264(12) 0.079(2) -0.0039(12) 0.0388(16) -0.0043(12) F17 0.077(2) 0.0442(15) 0.0405(16) -0.0006(11) 0.0230(14) 0.0163(14) F18 0.0344(14) 0.0439(15) 0.082(2) -0.0078(14) 0.0181(13) 0.0107(11) F19 0.0462(18) 0.149(4) 0.151(4) 0.120(3) 0.053(2) 0.053(2) F20 0.058(2) 0.065(2) 0.110(3) -0.013(2) -0.040(2) 0.0074(17) F21 0.077(2) 0.073(2) 0.0552(19) 0.0108(16) 0.0162(16) 0.0451(18) F22 0.0596(19) 0.0546(18) 0.126(3) 0.0407(19) 0.064(2) 0.0124(14) F23 0.077(2) 0.093(3) 0.088(3) 0.059(2) 0.040(2) 0.011(2) F24 0.114(3) 0.0256(15) 0.152(4) 0.0102(18) 0.092(3) -0.0001(16) Pd1 0.02522(16) 0.02538(16) 0.02586(17) -0.00032(10) 0.00508(11) 0.00077(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.466(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.476(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.449(7) . ? C3 N1 1.486(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N2 1.533(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N2 1.460(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N2 1.438(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.519(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.542(6) . ? C8 C9 1.594(5) . ? C8 H100 0.93(6) . ? C9 C15 1.543(5) . ? C9 C10 1.550(5) . ? C9 Pd1 2.469(4) . ? C9 H101 1.00(6) . ? C10 C14 1.534(6) . ? C10 C11 1.547(6) . ? C10 H10 1.0000 . ? C11 C12 1.555(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.520(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.540(6) . ? C13 H13 1.0000 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.555(5) . ? C15 C20 1.558(6) . ? C15 H102 1.03(6) . ? C16 C17 1.521(6) . ? C16 Pd1 2.018(4) . ? C16 H103 1.05(7) . ? C17 C21 1.536(6) . ? C17 C18 1.552(6) . ? C17 H17 1.0000 . ? C18 C19 1.537(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.533(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.524(6) . ? C20 H20 1.0000 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.394(6) . ? C22 C29 1.395(5) . ? C22 B1 1.651(5) . ? C23 C24 1.402(5) . ? C23 H23 0.9500 . ? C24 C26 1.383(5) . ? C24 C25 1.496(6) . ? C25 F3 1.313(5) . ? C25 F1 1.329(5) . ? C25 F2 1.335(6) . ? C26 C27 1.369(6) . ? C26 H26 0.9500 . ? C27 C29 1.401(5) . ? C27 C28 1.506(5) . ? C28 F4 1.299(6) . ? C28 F6 1.316(6) . ? C28 F5 1.355(6) . ? C29 H29 0.9500 . ? C30 C37 1.393(6) . ? C30 C31 1.400(5) . ? C30 B1 1.638(6) . ? C31 C32 1.390(6) . ? C31 H31 0.9500 . ? C32 C34 1.382(6) . ? C32 C33 1.512(7) . ? C33 F8 1.313(7) . ? C33 F7 1.333(8) . ? C33 F9 1.360(9) . ? C34 C35 1.373(6) . ? C34 H34 0.9500 . ? C35 C37 1.380(6) . ? C35 C36 1.503(7) . ? C36 F10 1.263(10) . ? C36 F11 1.268(8) . ? C36 F12 1.296(10) . ? C37 H37 0.9500 . ? C38 C39 1.399(5) . ? C38 C45 1.402(5) . ? C38 B1 1.637(5) . ? C39 C40 1.382(5) . ? C39 H39 0.9500 . ? C40 C42 1.389(5) . ? C40 C41 1.500(5) . ? C41 F13 1.313(5) . ? C41 F15 1.329(5) . ? C41 F14 1.329(5) . ? C42 C43 1.377(5) . ? C42 H42 0.9500 . ? C43 C45 1.387(5) . ? C43 C44 1.499(5) . ? C44 F16 1.330(5) . ? C44 F17 1.335(5) . ? C44 F18 1.356(5) . ? C45 H45 0.9500 . ? C46 C53 1.393(5) . ? C46 C47 1.409(5) . ? C46 B1 1.649(5) . ? C47 C48 1.387(5) . ? C47 H47 0.9500 . ? C48 C50 1.397(6) . ? C48 C49 1.498(6) . ? C49 F19 1.293(5) . ? C49 F20 1.311(5) . ? C49 F21 1.344(5) . ? C50 C51 1.377(6) . ? C50 H50 0.9500 . ? C51 C53 1.395(5) . ? C51 C52 1.494(6) . ? C52 F24 1.283(6) . ? C52 F22 1.325(5) . ? C52 F23 1.386(8) . ? C53 H53 0.9500 . ? N1 Pd1 2.243(4) . ? N2 Pd1 2.101(3) . ? Pd1 H101 1.89(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 N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 N1 113.1(4) . . ? C4 C3 H3A 108.9 . . ? N1 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? N1 C3 H3B 108.9 . . ? H3A C3 H3B 107.8 . . ? C3 C4 N2 111.6(4) . . ? C3 C4 H4A 109.3 . . ? N2 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? N2 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? 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 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C7 C8 C13 111.7(4) . . ? C7 C8 C9 116.1(4) . . ? C13 C8 C9 102.6(3) . . ? C7 C8 H100 107(3) . . ? C13 C8 H100 114(3) . . ? C9 C8 H100 106(3) . . ? C15 C9 C10 114.7(3) . . ? C15 C9 C8 115.7(3) . . ? C10 C9 C8 102.1(3) . . ? C15 C9 Pd1 83.1(2) . . ? C10 C9 Pd1 146.3(3) . . ? C8 C9 Pd1 94.3(2) . . ? C15 C9 H101 110(3) . . ? C10 C9 H101 102(3) . . ? C8 C9 H101 112(3) . . ? Pd1 C9 H101 44(3) . . ? C14 C10 C11 101.5(3) . . ? C14 C10 C9 100.3(3) . . ? C11 C10 C9 109.3(3) . . ? C14 C10 H10 114.7 . . ? C11 C10 H10 114.7 . . ? C9 C10 H10 114.7 . . ? C10 C11 C12 104.0(3) . . ? C10 C11 H11A 111.0 . . ? C12 C11 H11A 111.0 . . ? C10 C11 H11B 111.0 . . ? C12 C11 H11B 111.0 . . ? H11A C11 H11B 109.0 . . ? C13 C12 C11 102.4(3) . . ? C13 C12 H12A 111.3 . . ? C11 C12 H12A 111.3 . . ? C13 C12 H12B 111.3 . . ? C11 C12 H12B 111.3 . . ? H12A C12 H12B 109.2 . . ? C12 C13 C14 102.2(4) . . ? C12 C13 C8 109.7(3) . . ? C14 C13 C8 101.8(3) . . ? C12 C13 H13 114.0 . . ? C14 C13 H13 114.0 . . ? C8 C13 H13 114.0 . . ? C10 C14 C13 94.5(3) . . ? C10 C14 H14A 112.8 . . ? C13 C14 H14A 112.8 . . ? C10 C14 H14B 112.8 . . ? C13 C14 H14B 112.8 . . ? H14A C14 H14B 110.3 . . ? C9 C15 C16 108.7(3) . . ? C9 C15 C20 117.2(3) . . ? C16 C15 C20 101.5(3) . . ? C9 C15 H102 109(3) . . ? C16 C15 H102 113(3) . . ? C20 C15 H102 108(3) . . ? C17 C16 C15 104.5(3) . . ? C17 C16 Pd1 112.7(3) . . ? C15 C16 Pd1 99.8(3) . . ? C17 C16 H103 118(3) . . ? C15 C16 H103 112(3) . . ? Pd1 C16 H103 109(4) . . ? C16 C17 C21 101.9(3) . . ? C16 C17 C18 106.6(4) . . ? C21 C17 C18 101.5(3) . . ? C16 C17 H17 115.0 . . ? C21 C17 H17 115.0 . . ? C18 C17 H17 115.0 . . ? C19 C18 C17 102.7(3) . . ? C19 C18 H18A 111.2 . . ? C17 C18 H18A 111.2 . . ? C19 C18 H18B 111.2 . . ? C17 C18 H18B 111.2 . . ? H18A C18 H18B 109.1 . . ? C20 C19 C18 104.0(4) . . ? C20 C19 H19A 110.9 . . ? C18 C19 H19A 110.9 . . ? C20 C19 H19B 110.9 . . ? C18 C19 H19B 110.9 . . ? H19A C19 H19B 109.0 . . ? C21 C20 C19 101.0(3) . . ? C21 C20 C15 103.4(3) . . ? C19 C20 C15 106.1(4) . . ? C21 C20 H20 114.9 . . ? C19 C20 H20 114.9 . . ? C15 C20 H20 114.9 . . ? C20 C21 C17 94.7(3) . . ? C20 C21 H21A 112.8 . . ? C17 C21 H21A 112.8 . . ? C20 C21 H21B 112.8 . . ? C17 C21 H21B 112.8 . . ? H21A C21 H21B 110.3 . . ? C23 C22 C29 116.4(3) . . ? C23 C22 B1 118.5(3) . . ? C29 C22 B1 125.1(4) . . ? C22 C23 C24 122.5(3) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C26 C24 C23 119.7(4) . . ? C26 C24 C25 119.7(4) . . ? C23 C24 C25 120.5(3) . . ? F3 C25 F1 106.4(4) . . ? F3 C25 F2 105.6(4) . . ? F1 C25 F2 106.8(4) . . ? F3 C25 C24 113.2(3) . . ? F1 C25 C24 112.7(4) . . ? F2 C25 C24 111.6(4) . . ? C27 C26 C24 118.8(3) . . ? C27 C26 H26 120.6 . . ? C24 C26 H26 120.6 . . ? C26 C27 C29 121.6(3) . . ? C26 C27 C28 117.7(3) . . ? C29 C27 C28 120.7(4) . . ? F4 C28 F6 111.0(4) . . ? F4 C28 F5 104.9(4) . . ? F6 C28 F5 102.6(4) . . ? F4 C28 C27 113.0(4) . . ? F6 C28 C27 113.5(3) . . ? F5 C28 C27 110.9(4) . . ? C22 C29 C27 121.0(4) . . ? C22 C29 H29 119.5 . . ? C27 C29 H29 119.5 . . ? C37 C30 C31 115.1(4) . . ? C37 C30 B1 123.4(3) . . ? C31 C30 B1 120.9(3) . . ? C32 C31 C30 121.9(4) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C34 C32 C31 121.2(4) . . ? C34 C32 C33 120.5(4) . . ? C31 C32 C33 118.3(4) . . ? F8 C33 F7 106.0(7) . . ? F8 C33 F9 110.8(6) . . ? F7 C33 F9 104.5(5) . . ? F8 C33 C32 112.5(5) . . ? F7 C33 C32 112.3(5) . . ? F9 C33 C32 110.4(6) . . ? C35 C34 C32 117.7(4) . . ? C35 C34 H34 121.2 . . ? C32 C34 H34 121.2 . . ? C34 C35 C37 121.1(4) . . ? C34 C35 C36 118.8(4) . . ? C37 C35 C36 120.1(4) . . ? F10 C36 F11 112.8(7) . . ? F10 C36 F12 99.5(7) . . ? F11 C36 F12 102.4(8) . . ? F10 C36 C35 112.9(7) . . ? F11 C36 C35 115.0(5) . . ? F12 C36 C35 112.7(6) . . ? C35 C37 C30 123.0(4) . . ? C35 C37 H37 118.5 . . ? C30 C37 H37 118.5 . . ? C39 C38 C45 115.3(3) . . ? C39 C38 B1 121.9(3) . . ? C45 C38 B1 122.4(3) . . ? C40 C39 C38 122.6(3) . . ? C40 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C39 C40 C42 121.0(3) . . ? C39 C40 C41 119.0(4) . . ? C42 C40 C41 120.0(3) . . ? F13 C41 F15 107.6(4) . . ? F13 C41 F14 106.1(4) . . ? F15 C41 F14 105.1(3) . . ? F13 C41 C40 112.4(3) . . ? F15 C41 C40 113.0(4) . . ? F14 C41 C40 112.1(3) . . ? C43 C42 C40 117.4(3) . . ? C43 C42 H42 121.3 . . ? C40 C42 H42 121.3 . . ? C42 C43 C45 121.7(3) . . ? C42 C43 C44 119.8(3) . . ? C45 C43 C44 118.5(3) . . ? F16 C44 F17 108.1(4) . . ? F16 C44 F18 105.8(3) . . ? F17 C44 F18 104.6(3) . . ? F16 C44 C43 113.8(3) . . ? F17 C44 C43 112.4(3) . . ? F18 C44 C43 111.5(3) . . ? C43 C45 C38 121.9(3) . . ? C43 C45 H45 119.1 . . ? C38 C45 H45 119.1 . . ? C53 C46 C47 115.8(3) . . ? C53 C46 B1 120.8(3) . . ? C47 C46 B1 123.1(3) . . ? C48 C47 C46 121.7(3) . . ? C48 C47 H47 119.1 . . ? C46 C47 H47 119.1 . . ? C47 C48 C50 121.0(4) . . ? C47 C48 C49 120.3(4) . . ? C50 C48 C49 118.7(4) . . ? F19 C49 F20 108.3(5) . . ? F19 C49 F21 104.7(4) . . ? F20 C49 F21 102.8(4) . . ? F19 C49 C48 114.5(3) . . ? F20 C49 C48 113.6(4) . . ? F21 C49 C48 112.1(3) . . ? C51 C50 C48 118.3(4) . . ? C51 C50 H50 120.9 . . ? C48 C50 H50 120.9 . . ? C50 C51 C53 120.4(4) . . ? C50 C51 C52 121.5(4) . . ? C53 C51 C52 118.1(4) . . ? F24 C52 F22 109.7(4) . . ? F24 C52 F23 102.6(5) . . ? F22 C52 F23 106.0(5) . . ? F24 C52 C51 113.3(5) . . ? F22 C52 C51 113.0(4) . . ? F23 C52 C51 111.5(4) . . ? C46 C53 C51 122.9(3) . . ? C46 C53 H53 118.6 . . ? C51 C53 H53 118.6 . . ? C38 B1 C30 112.1(3) . . ? C38 B1 C46 113.1(3) . . ? C30 B1 C46 103.5(3) . . ? C38 B1 C22 106.0(3) . . ? C30 B1 C22 113.4(3) . . ? C46 B1 C22 108.9(3) . . ? C1 N1 C2 108.4(4) . . ? C1 N1 C3 109.5(3) . . ? C2 N1 C3 110.6(4) . . ? C1 N1 Pd1 115.3(3) . . ? C2 N1 Pd1 108.9(3) . . ? C3 N1 Pd1 104.1(3) . . ? C6 N2 C5 110.9(5) . . ? C6 N2 C4 105.1(4) . . ? C5 N2 C4 109.6(4) . . ? C6 N2 Pd1 118.2(3) . . ? C5 N2 Pd1 108.2(3) . . ? C4 N2 Pd1 104.4(3) . . ? C16 Pd1 N2 97.48(15) . . ? C16 Pd1 N1 176.32(14) . . ? N2 Pd1 N1 83.78(14) . . ? C16 Pd1 C9 67.38(14) . . ? N2 Pd1 C9 156.30(14) . . ? N1 Pd1 C9 112.52(13) . . ? C16 Pd1 H101 83.1(17) . . ? N2 Pd1 H101 176.4(17) . . ? N1 Pd1 H101 95.9(18) . . ? C9 Pd1 H101 21.6(18) . . ? 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 C3 C4 N2 55.2(5) . . . . ? C7 C8 C9 C15 -0.6(5) . . . . ? C13 C8 C9 C15 121.6(4) . . . . ? C7 C8 C9 C10 -125.8(4) . . . . ? C13 C8 C9 C10 -3.7(4) . . . . ? C7 C8 C9 Pd1 83.8(4) . . . . ? C13 C8 C9 Pd1 -154.1(3) . . . . ? C15 C9 C10 C14 -86.8(4) . . . . ? C8 C9 C10 C14 39.1(4) . . . . ? Pd1 C9 C10 C14 156.4(4) . . . . ? C15 C9 C10 C11 167.0(3) . . . . ? C8 C9 C10 C11 -67.1(4) . . . . ? Pd1 C9 C10 C11 50.2(6) . . . . ? C14 C10 C11 C12 -32.3(4) . . . . ? C9 C10 C11 C12 73.1(4) . . . . ? C10 C11 C12 C13 -3.1(4) . . . . ? C11 C12 C13 C14 37.5(4) . . . . ? C11 C12 C13 C8 -69.9(4) . . . . ? C7 C8 C13 C12 -160.1(4) . . . . ? C9 C8 C13 C12 74.8(4) . . . . ? C7 C8 C13 C14 92.2(4) . . . . ? C9 C8 C13 C14 -32.9(4) . . . . ? C11 C10 C14 C13 53.5(4) . . . . ? C9 C10 C14 C13 -58.8(4) . . . . ? C12 C13 C14 C10 -56.7(4) . . . . ? C8 C13 C14 C10 56.7(4) . . . . ? C10 C9 C15 C16 -158.4(3) . . . . ? C8 C9 C15 C16 83.1(4) . . . . ? Pd1 C9 C15 C16 -8.4(3) . . . . ? C10 C9 C15 C20 -44.1(5) . . . . ? C8 C9 C15 C20 -162.6(3) . . . . ? Pd1 C9 C15 C20 106.0(3) . . . . ? C9 C15 C16 C17 127.0(3) . . . . ? C20 C15 C16 C17 2.8(4) . . . . ? C9 C15 C16 Pd1 10.3(3) . . . . ? C20 C15 C16 Pd1 -113.9(3) . . . . ? C15 C16 C17 C21 -36.5(4) . . . . ? Pd1 C16 C17 C21 70.9(4) . . . . ? C15 C16 C17 C18 69.5(4) . . . . ? Pd1 C16 C17 C18 176.9(3) . . . . ? C16 C17 C18 C19 -72.9(4) . . . . ? C21 C17 C18 C19 33.4(4) . . . . ? C17 C18 C19 C20 1.9(5) . . . . ? C18 C19 C20 C21 -36.9(5) . . . . ? C18 C19 C20 C15 70.7(4) . . . . ? C9 C15 C20 C21 -86.0(4) . . . . ? C16 C15 C20 C21 32.2(4) . . . . ? C9 C15 C20 C19 168.1(3) . . . . ? C16 C15 C20 C19 -73.6(4) . . . . ? C19 C20 C21 C17 56.3(4) . . . . ? C15 C20 C21 C17 -53.5(4) . . . . ? C16 C17 C21 C20 54.9(4) . . . . ? C18 C17 C21 C20 -55.1(4) . . . . ? C29 C22 C23 C24 -2.3(5) . . . . ? B1 C22 C23 C24 178.6(3) . . . . ? C22 C23 C24 C26 0.5(6) . . . . ? C22 C23 C24 C25 -176.1(4) . . . . ? C26 C24 C25 F3 35.9(6) . . . . ? C23 C24 C25 F3 -147.5(4) . . . . ? C26 C24 C25 F1 156.7(4) . . . . ? C23 C24 C25 F1 -26.6(6) . . . . ? C26 C24 C25 F2 -83.1(5) . . . . ? C23 C24 C25 F2 93.5(5) . . . . ? C23 C24 C26 C27 1.6(6) . . . . ? C25 C24 C26 C27 178.3(4) . . . . ? C24 C26 C27 C29 -2.0(6) . . . . ? C24 C26 C27 C28 -179.3(4) . . . . ? C26 C27 C28 F4 63.3(6) . . . . ? C29 C27 C28 F4 -114.1(5) . . . . ? C26 C27 C28 F6 -169.1(4) . . . . ? C29 C27 C28 F6 13.5(6) . . . . ? C26 C27 C28 F5 -54.3(5) . . . . ? C29 C27 C28 F5 128.4(4) . . . . ? C23 C22 C29 C27 1.9(5) . . . . ? B1 C22 C29 C27 -179.0(3) . . . . ? C26 C27 C29 C22 0.1(6) . . . . ? C28 C27 C29 C22 177.4(4) . . . . ? C37 C30 C31 C32 2.1(6) . . . . ? B1 C30 C31 C32 173.6(4) . . . . ? C30 C31 C32 C34 0.8(8) . . . . ? C30 C31 C32 C33 -179.7(5) . . . . ? C34 C32 C33 F8 -20.1(10) . . . . ? C31 C32 C33 F8 160.5(6) . . . . ? C34 C32 C33 F7 -139.6(5) . . . . ? C31 C32 C33 F7 40.9(8) . . . . ? C34 C32 C33 F9 104.2(6) . . . . ? C31 C32 C33 F9 -75.3(7) . . . . ? C31 C32 C34 C35 -2.7(8) . . . . ? C33 C32 C34 C35 177.8(6) . . . . ? C32 C34 C35 C37 1.7(8) . . . . ? C32 C34 C35 C36 -178.7(6) . . . . ? C34 C35 C36 F10 120.7(8) . . . . ? C37 C35 C36 F10 -59.7(9) . . . . ? C34 C35 C36 F11 -10.7(10) . . . . ? C37 C35 C36 F11 168.9(7) . . . . ? C34 C35 C36 F12 -127.5(8) . . . . ? C37 C35 C36 F12 52.1(10) . . . . ? C34 C35 C37 C30 1.3(7) . . . . ? C36 C35 C37 C30 -178.3(5) . . . . ? C31 C30 C37 C35 -3.1(6) . . . . ? B1 C30 C37 C35 -174.4(4) . . . . ? C45 C38 C39 C40 -4.0(5) . . . . ? B1 C38 C39 C40 -177.2(3) . . . . ? C38 C39 C40 C42 2.2(6) . . . . ? C38 C39 C40 C41 -176.2(3) . . . . ? C39 C40 C41 F13 78.0(5) . . . . ? C42 C40 C41 F13 -100.4(5) . . . . ? C39 C40 C41 F15 -160.0(4) . . . . ? C42 C40 C41 F15 21.6(5) . . . . ? C39 C40 C41 F14 -41.4(5) . . . . ? C42 C40 C41 F14 140.2(4) . . . . ? C39 C40 C42 C43 1.2(5) . . . . ? C41 C40 C42 C43 179.5(3) . . . . ? C40 C42 C43 C45 -2.6(5) . . . . ? C40 C42 C43 C44 177.7(3) . . . . ? C42 C43 C44 F16 -1.8(5) . . . . ? C45 C43 C44 F16 178.5(3) . . . . ? C42 C43 C44 F17 -125.1(4) . . . . ? C45 C43 C44 F17 55.2(5) . . . . ? C42 C43 C44 F18 117.8(4) . . . . ? C45 C43 C44 F18 -61.9(5) . . . . ? C42 C43 C45 C38 0.7(5) . . . . ? C44 C43 C45 C38 -179.6(3) . . . . ? C39 C38 C45 C43 2.5(5) . . . . ? B1 C38 C45 C43 175.8(3) . . . . ? C53 C46 C47 C48 0.9(6) . . . . ? B1 C46 C47 C48 173.8(4) . . . . ? C46 C47 C48 C50 -0.7(6) . . . . ? C46 C47 C48 C49 179.5(4) . . . . ? C47 C48 C49 F19 4.4(6) . . . . ? C50 C48 C49 F19 -175.4(5) . . . . ? C47 C48 C49 F20 129.4(5) . . . . ? C50 C48 C49 F20 -50.4(6) . . . . ? C47 C48 C49 F21 -114.6(4) . . . . ? C50 C48 C49 F21 65.6(5) . . . . ? C47 C48 C50 C51 -0.1(6) . . . . ? C49 C48 C50 C51 179.7(4) . . . . ? C48 C50 C51 C53 0.7(6) . . . . ? C48 C50 C51 C52 -178.2(4) . . . . ? C50 C51 C52 F24 113.1(5) . . . . ? C53 C51 C52 F24 -65.9(7) . . . . ? C50 C51 C52 F22 -12.5(8) . . . . ? C53 C51 C52 F22 168.5(5) . . . . ? C50 C51 C52 F23 -131.8(5) . . . . ? C53 C51 C52 F23 49.3(6) . . . . ? C47 C46 C53 C51 -0.4(6) . . . . ? B1 C46 C53 C51 -173.4(4) . . . . ? C50 C51 C53 C46 -0.4(6) . . . . ? C52 C51 C53 C46 178.5(4) . . . . ? C39 C38 B1 C30 -37.5(5) . . . . ? C45 C38 B1 C30 149.7(3) . . . . ? C39 C38 B1 C46 -154.1(3) . . . . ? C45 C38 B1 C46 33.1(5) . . . . ? C39 C38 B1 C22 86.7(4) . . . . ? C45 C38 B1 C22 -86.0(4) . . . . ? C37 C30 B1 C38 -27.9(5) . . . . ? C31 C30 B1 C38 161.3(3) . . . . ? C37 C30 B1 C46 94.3(4) . . . . ? C31 C30 B1 C46 -76.5(4) . . . . ? C37 C30 B1 C22 -147.9(4) . . . . ? C31 C30 B1 C22 41.3(5) . . . . ? C53 C46 B1 C38 -152.7(3) . . . . ? C47 C46 B1 C38 34.9(5) . . . . ? C53 C46 B1 C30 85.8(4) . . . . ? C47 C46 B1 C30 -86.7(4) . . . . ? C53 C46 B1 C22 -35.1(5) . . . . ? C47 C46 B1 C22 152.4(3) . . . . ? C23 C22 B1 C38 78.1(4) . . . . ? C29 C22 B1 C38 -100.9(4) . . . . ? C23 C22 B1 C30 -158.5(3) . . . . ? C29 C22 B1 C30 22.5(5) . . . . ? C23 C22 B1 C46 -43.8(4) . . . . ? C29 C22 B1 C46 137.1(4) . . . . ? C4 C3 N1 C1 -155.9(4) . . . . ? C4 C3 N1 C2 84.7(5) . . . . ? C4 C3 N1 Pd1 -32.1(4) . . . . ? C3 C4 N2 C6 -171.4(4) . . . . ? C3 C4 N2 C5 69.4(5) . . . . ? C3 C4 N2 Pd1 -46.3(4) . . . . ? C17 C16 Pd1 N2 82.0(3) . . . . ? C15 C16 Pd1 N2 -167.6(2) . . . . ? C17 C16 Pd1 N1 -28(2) . . . . ? C15 C16 Pd1 N1 83(2) . . . . ? C17 C16 Pd1 C9 -117.0(3) . . . . ? C15 C16 Pd1 C9 -6.6(2) . . . . ? C6 N2 Pd1 C16 -39.3(4) . . . . ? C5 N2 Pd1 C16 87.7(4) . . . . ? C4 N2 Pd1 C16 -155.6(3) . . . . ? C6 N2 Pd1 N1 137.2(4) . . . . ? C5 N2 Pd1 N1 -95.7(4) . . . . ? C4 N2 Pd1 N1 21.0(3) . . . . ? C6 N2 Pd1 C9 -87.5(5) . . . . ? C5 N2 Pd1 C9 39.5(6) . . . . ? C4 N2 Pd1 C9 156.2(3) . . . . ? C1 N1 Pd1 C16 -126(2) . . . . ? C2 N1 Pd1 C16 -3(2) . . . . ? C3 N1 Pd1 C16 115(2) . . . . ? C1 N1 Pd1 N2 124.4(3) . . . . ? C2 N1 Pd1 N2 -113.5(3) . . . . ? C3 N1 Pd1 N2 4.4(3) . . . . ? C1 N1 Pd1 C9 -37.8(4) . . . . ? C2 N1 Pd1 C9 84.3(3) . . . . ? C3 N1 Pd1 C9 -157.7(2) . . . . ? C15 C9 Pd1 C16 6.6(2) . . . . ? C10 C9 Pd1 C16 131.9(5) . . . . ? C8 C9 Pd1 C16 -108.8(3) . . . . ? C15 C9 Pd1 N2 59.8(4) . . . . ? C10 C9 Pd1 N2 -174.9(4) . . . . ? C8 C9 Pd1 N2 -55.6(4) . . . . ? C15 C9 Pd1 N1 -169.4(2) . . . . ? C10 C9 Pd1 N1 -44.2(5) . . . . ? C8 C9 Pd1 N1 75.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 71.67 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 1.540 _refine_diff_density_min -1.153 _refine_diff_density_rms 0.106 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.014 0.000 0.000 859 313 ' ' 2 -0.215 0.500 0.500 859 315 ' ' _platon_squeeze_details ; ; # Attachment 'c09219.cif' data_c09219_0m _database_code_depnum_ccdc_archive 'CCDC 743857' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H29 N2 O Pd, C32 H12 B F24' _chemical_formula_sum 'C43 H41 B F24 N2 O Pd' _chemical_formula_weight 1174.99 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' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.9055(8) _cell_length_b 19.9639(9) _cell_length_c 27.1312(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9698.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9965 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 26.71 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4704 _exptl_absorpt_coefficient_mu 0.511 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8618 _exptl_absorpt_correction_T_max 0.8829 _exptl_absorpt_process_details '(Blessing, 1995)' _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62819 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9916 _reflns_number_gt 7556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. ; _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^)+(0.0834P)^2^+24.6288P] 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 9916 _refine_ls_number_parameters 725 _refine_ls_number_restraints 111 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1505 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _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 0.765159(17) 0.111088(14) 0.580726(11) 0.03202(12) Uani 0.421(6) 1 d PD A 1 N1 N 0.8261(6) 0.1958(5) 0.6012(5) 0.050(3) Uani 0.421(6) 1 d PDU A 1 N2 N 0.8755(7) 0.0615(6) 0.5823(5) 0.0337(12) Uani 0.421(6) 1 d PDU A 1 C1 C 0.8069(10) 0.2563(7) 0.5733(7) 0.076(6) Uani 0.421(6) 1 d PDU A 1 H1A H 0.8367 0.2941 0.5854 0.114 Uiso 0.421(6) 1 calc PR A 1 H1B H 0.7537 0.2663 0.5777 0.114 Uiso 0.421(6) 1 calc PR A 1 H1C H 0.8174 0.2490 0.5383 0.114 Uiso 0.421(6) 1 calc PR A 1 C2 C 0.8132(7) 0.2098(7) 0.6568(5) 0.067(4) Uani 0.421(6) 1 d PDU A 1 H2A H 0.8400 0.2507 0.6663 0.101 Uiso 0.421(6) 1 calc PR A 1 H2B H 0.8318 0.1720 0.6762 0.101 Uiso 0.421(6) 1 calc PR A 1 H2C H 0.7597 0.2158 0.6629 0.101 Uiso 0.421(6) 1 calc PR A 1 C3 C 0.9065(8) 0.1790(7) 0.5951(12) 0.0559(13) Uani 0.421(6) 1 d PDU A 1 H3A H 0.9207 0.1853 0.5601 0.067 Uiso 0.421(6) 1 calc PR A 1 H3B H 0.9368 0.2103 0.6151 0.067 Uiso 0.421(6) 1 calc PR A 1 C4 C 0.9240(6) 0.1094(6) 0.6100(6) 0.053(3) Uani 0.421(6) 1 d PDU A 1 H4A H 0.9156 0.1041 0.6458 0.064 Uiso 0.421(6) 1 calc PR A 1 H4B H 0.9771 0.0996 0.6030 0.064 Uiso 0.421(6) 1 calc PR A 1 C5 C 0.9016(6) 0.0529(6) 0.5313(4) 0.044(3) Uani 0.421(6) 1 d PDU A 1 H5A H 0.9532 0.0364 0.5315 0.067 Uiso 0.421(6) 1 calc PR A 1 H5B H 0.8995 0.0960 0.5141 0.067 Uiso 0.421(6) 1 calc PR A 1 H5C H 0.8695 0.0205 0.5143 0.067 Uiso 0.421(6) 1 calc PR A 1 C6 C 0.8787(8) -0.0056(6) 0.6060(5) 0.069(4) Uani 0.421(6) 1 d PDU A 1 H6A H 0.9287 -0.0246 0.6018 0.104 Uiso 0.421(6) 1 calc PR A 1 H6B H 0.8418 -0.0352 0.5906 0.104 Uiso 0.421(6) 1 calc PR A 1 H6C H 0.8676 -0.0011 0.6413 0.104 Uiso 0.421(6) 1 calc PR A 1 C11 C 0.6685(13) 0.1638(17) 0.576(4) 0.076(4) Uani 0.421(6) 1 d PD A 1 H11A H 0.6269 0.1358 0.5872 0.114 Uiso 0.421(6) 1 calc PR A 1 H11B H 0.6600 0.1771 0.5416 0.114 Uiso 0.421(6) 1 calc PR A 1 H11C H 0.6719 0.2039 0.5967 0.114 Uiso 0.421(6) 1 calc PR A 1 Pd1' Pd 0.765159(17) 0.111088(14) 0.580726(11) 0.03202(12) Uani 0.579(6) 1 d PD A 2 N1' N 0.8282(4) 0.1979(3) 0.5734(3) 0.041(2) Uani 0.579(6) 1 d PDU A 2 N2' N 0.8732(5) 0.0606(4) 0.5905(4) 0.0337(12) Uani 0.579(6) 1 d PDU A 2 C1' C 0.8354(6) 0.2205(5) 0.5218(4) 0.067(3) Uani 0.579(6) 1 d PDU A 2 H1'1 H 0.8676 0.2602 0.5205 0.100 Uiso 0.579(6) 1 calc PR A 2 H1'2 H 0.7859 0.2319 0.5088 0.100 Uiso 0.579(6) 1 calc PR A 2 H1'3 H 0.8574 0.1846 0.5019 0.100 Uiso 0.579(6) 1 calc PR A 2 C2' C 0.7978(8) 0.2552(5) 0.6049(5) 0.065(3) Uani 0.579(6) 1 d PDU A 2 H2'1 H 0.8334 0.2925 0.6047 0.097 Uiso 0.579(6) 1 calc PR A 2 H2'2 H 0.7907 0.2396 0.6388 0.097 Uiso 0.579(6) 1 calc PR A 2 H2'3 H 0.7499 0.2703 0.5915 0.097 Uiso 0.579(6) 1 calc PR A 2 C3' C 0.9024(6) 0.1807(6) 0.5957(9) 0.0559(13) Uani 0.579(6) 1 d PDU A 2 H3'1 H 0.9396 0.2150 0.5862 0.067 Uiso 0.579(6) 1 calc PR A 2 H3'2 H 0.8982 0.1806 0.6320 0.067 Uiso 0.579(6) 1 calc PR A 2 C4' C 0.9277(5) 0.1138(4) 0.5784(4) 0.052(2) Uani 0.579(6) 1 d PDU A 2 H4'1 H 0.9352 0.1151 0.5422 0.063 Uiso 0.579(6) 1 calc PR A 2 H4'2 H 0.9763 0.1030 0.5939 0.063 Uiso 0.579(6) 1 calc PR A 2 C5' C 0.8875(5) 0.0016(4) 0.5601(4) 0.056(2) Uani 0.579(6) 1 d PDU A 2 H5'1 H 0.8851 0.0140 0.5252 0.083 Uiso 0.579(6) 1 calc PR A 2 H5'2 H 0.8497 -0.0327 0.5670 0.083 Uiso 0.579(6) 1 calc PR A 2 H5'3 H 0.9372 -0.0162 0.5676 0.083 Uiso 0.579(6) 1 calc PR A 2 C6' C 0.8810(5) 0.0414(4) 0.6429(3) 0.045(2) Uani 0.579(6) 1 d PDU A 2 H6'1 H 0.9327 0.0278 0.6494 0.067 Uiso 0.579(6) 1 calc PR A 2 H6'2 H 0.8474 0.0040 0.6502 0.067 Uiso 0.579(6) 1 calc PR A 2 H6'3 H 0.8682 0.0797 0.6639 0.067 Uiso 0.579(6) 1 calc PR A 2 C11' C 0.6672(10) 0.1611(13) 0.572(3) 0.076(4) Uani 0.579(6) 1 d PD A 2 H11D H 0.6518 0.1803 0.6038 0.114 Uiso 0.579(6) 1 calc PR A 2 H11E H 0.6287 0.1301 0.5604 0.114 Uiso 0.579(6) 1 calc PR A 2 H11F H 0.6738 0.1971 0.5479 0.114 Uiso 0.579(6) 1 calc PR A 2 C7 C 0.7118(4) 0.0144(4) 0.4910(2) 0.084(2) Uani 1 1 d . . . H7A H 0.7246 0.0621 0.4896 0.125 Uiso 1 1 calc R . . H7B H 0.6848 0.0018 0.4610 0.125 Uiso 1 1 calc R . . H7C H 0.7576 -0.0122 0.4936 0.125 Uiso 1 1 calc R . . C8 C 0.6638(3) 0.0016(3) 0.5346(2) 0.0715(17) Uani 1 1 d . A . H8A H 0.6167 0.0271 0.5314 0.086 Uiso 1 1 calc R . . H8B H 0.6513 -0.0466 0.5362 0.086 Uiso 1 1 calc R . . C9 C 0.6506(3) 0.0116(4) 0.6207(2) 0.0748(19) Uani 1 1 d . A . H9A H 0.6314 -0.0349 0.6201 0.090 Uiso 1 1 calc R . . H9B H 0.6076 0.0424 0.6172 0.090 Uiso 1 1 calc R . . C10 C 0.6884(4) 0.0243(4) 0.6680(2) 0.092(3) Uani 1 1 d . . . H10A H 0.7315 -0.0058 0.6711 0.138 Uiso 1 1 calc R . . H10B H 0.6535 0.0160 0.6952 0.138 Uiso 1 1 calc R . . H10C H 0.7054 0.0709 0.6691 0.138 Uiso 1 1 calc R . . C12 C 0.67336(19) 0.26033(17) 0.28267(12) 0.0223(7) Uani 1 1 d . . . C13 C 0.62220(19) 0.31386(18) 0.28151(13) 0.0248(7) Uani 1 1 d . . . H13 H 0.6234 0.3461 0.3072 0.030 Uiso 1 1 calc R . . C14 C 0.5700(2) 0.32103(19) 0.24393(14) 0.0315(8) Uani 1 1 d . . . C15 C 0.5152(3) 0.3779(2) 0.24413(18) 0.0453(11) Uani 1 1 d . . . C16 C 0.5655(2) 0.2739(2) 0.20570(14) 0.0338(9) Uani 1 1 d . . . H16 H 0.5302 0.2787 0.1798 0.041 Uiso 1 1 calc R . . C17 C 0.6140(2) 0.22024(19) 0.20696(13) 0.0287(8) Uani 1 1 d . . . C18 C 0.6094(2) 0.1661(2) 0.16866(15) 0.0391(10) Uani 1 1 d . . . C19 C 0.66711(19) 0.21358(18) 0.24495(13) 0.0249(7) Uani 1 1 d . . . H19 H 0.6996 0.1760 0.2448 0.030 Uiso 1 1 calc R . . C20 C 0.67653(18) 0.24435(17) 0.37795(12) 0.0205(7) Uani 1 1 d . . . C21 C 0.66817(19) 0.29215(17) 0.41491(12) 0.0220(7) Uani 1 1 d . . . H21 H 0.6982 0.3313 0.4139 0.026 Uiso 1 1 calc R . . C22 C 0.6168(2) 0.28442(18) 0.45362(12) 0.0250(7) Uani 1 1 d . . . C23 C 0.6108(2) 0.3390(2) 0.49157(14) 0.0344(9) Uani 1 1 d . . . C24 C 0.5720(2) 0.22821(18) 0.45658(12) 0.0252(7) Uani 1 1 d . . . H24 H 0.5378 0.2226 0.4830 0.030 Uiso 1 1 calc R . . C25 C 0.57848(19) 0.18022(17) 0.41980(12) 0.0230(7) Uani 1 1 d . . . C26 C 0.5281(2) 0.12022(19) 0.42209(14) 0.0302(8) Uani 1 1 d . . . C27 C 0.62924(18) 0.18835(17) 0.38130(12) 0.0212(7) Uani 1 1 d . . . H27 H 0.6320 0.1549 0.3565 0.025 Uiso 1 1 calc R . . C28 C 0.78278(18) 0.32116(17) 0.33671(12) 0.0218(7) Uani 1 1 d . . . C29 C 0.78078(19) 0.37912(17) 0.30812(13) 0.0241(7) Uani 1 1 d . . . H29 H 0.7479 0.3809 0.2807 0.029 Uiso 1 1 calc R . . C30 C 0.8258(2) 0.43487(18) 0.31862(14) 0.0275(8) Uani 1 1 d . . . C31 C 0.8223(2) 0.4950(2) 0.28590(17) 0.0391(10) Uani 1 1 d . . . C32 C 0.8748(2) 0.43446(19) 0.35798(14) 0.0287(8) Uani 1 1 d . . . H32 H 0.9046 0.4725 0.3655 0.034 Uiso 1 1 calc R . . C33 C 0.8789(2) 0.37646(19) 0.38613(14) 0.0282(8) Uani 1 1 d . . . C34 C 0.9313(2) 0.3723(2) 0.42869(16) 0.0400(10) Uani 1 1 d . . . C35 C 0.83436(19) 0.32159(18) 0.37580(13) 0.0252(7) Uani 1 1 d . . . H35 H 0.8388 0.2828 0.3958 0.030 Uiso 1 1 calc R . . C36 C 0.79025(19) 0.19206(17) 0.32198(12) 0.0231(7) Uani 1 1 d . . . C37 C 0.8354(2) 0.1916(2) 0.27957(14) 0.0289(8) Uani 1 1 d . . . H37 H 0.8301 0.2267 0.2562 0.035 Uiso 1 1 calc R . . C38 C 0.8878(2) 0.1414(2) 0.27075(15) 0.0342(9) Uani 1 1 d . . . C39 C 0.9296(3) 0.1416(3) 0.22301(17) 0.0514(13) Uani 1 1 d . . . C40 C 0.8990(2) 0.0906(2) 0.30453(17) 0.0394(10) Uani 1 1 d . . . H40 H 0.9352 0.0566 0.2988 0.047 Uiso 1 1 calc R . . C41 C 0.8561(2) 0.0905(2) 0.34676(16) 0.0372(9) Uani 1 1 d . . . C42 C 0.8670(3) 0.0367(3) 0.3840(2) 0.0575(14) Uani 1 1 d . . . C43 C 0.8025(2) 0.14006(19) 0.35518(14) 0.0288(8) Uani 1 1 d . . . H43 H 0.7735 0.1382 0.3845 0.035 Uiso 1 1 calc R . . B1 B 0.7310(2) 0.25404(18) 0.32961(13) 0.0203(7) Uani 1 1 d . . . O1 O 0.70194(19) 0.02154(16) 0.57962(11) 0.0464(8) Uani 1 1 d . . . F1 F 0.52822(18) 0.42251(15) 0.27950(13) 0.0751(10) Uani 1 1 d . . . F2 F 0.44503(15) 0.35668(15) 0.25057(15) 0.0687(9) Uani 1 1 d . . . F3 F 0.51537(19) 0.41187(16) 0.20172(13) 0.0711(9) Uani 1 1 d . . . F4 F 0.5636(3) 0.18080(19) 0.13224(12) 0.1017(15) Uani 1 1 d . . . F5 F 0.58326(19) 0.10932(14) 0.18655(11) 0.0620(8) Uani 1 1 d . . . F6 F 0.67478(18) 0.1512(2) 0.14896(13) 0.0865(13) Uani 1 1 d . . . F7 F 0.67210(17) 0.34357(15) 0.51970(10) 0.0587(8) Uani 1 1 d . . . F8 F 0.55305(18) 0.33148(15) 0.52185(10) 0.0637(9) Uani 1 1 d . . . F9 F 0.60254(17) 0.39947(12) 0.47117(9) 0.0482(7) Uani 1 1 d . . . F10 F 0.45528(14) 0.13848(14) 0.42462(12) 0.0551(8) Uani 1 1 d . . . F11 F 0.53873(19) 0.08332(15) 0.46206(11) 0.0641(9) Uani 1 1 d . . . F12 F 0.53223(14) 0.08062(12) 0.38285(9) 0.0418(6) Uani 1 1 d . . . F13 F 0.8595(2) 0.48579(17) 0.24437(13) 0.0846(12) Uani 1 1 d . . . F14 F 0.75302(16) 0.51086(14) 0.27216(11) 0.0562(7) Uani 1 1 d . . . F15 F 0.8491(2) 0.55012(14) 0.30659(14) 0.0861(12) Uani 1 1 d . . . F16 F 0.89621(18) 0.3613(2) 0.47111(11) 0.0786(11) Uani 1 1 d . . . F17 F 0.98016(19) 0.32274(18) 0.42460(12) 0.0729(10) Uani 1 1 d . . . F18 F 0.97118(19) 0.42799(15) 0.43588(13) 0.0696(10) Uani 1 1 d . . . F19 F 0.88654(17) 0.12841(16) 0.18485(10) 0.0562(7) Uani 1 1 d . . . F20 F 0.9839(3) 0.0975(3) 0.22129(13) 0.137(2) Uani 1 1 d . . . F21 F 0.9604(2) 0.2001(2) 0.21279(14) 0.1096(18) Uani 1 1 d . . . F22 F 0.8055(2) 0.00372(18) 0.39403(15) 0.0818(11) Uani 1 1 d . . . F23 F 0.8906(3) 0.0584(3) 0.42629(17) 0.135(2) Uani 1 1 d . . . F24 F 0.9162(3) -0.0085(3) 0.3709(2) 0.159(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02800(19) 0.02489(17) 0.0432(2) 0.00268(12) -0.00027(13) -0.00122(11) N1 0.041(6) 0.029(5) 0.080(9) -0.007(6) 0.014(7) 0.001(4) N2 0.036(2) 0.0344(18) 0.031(3) 0.0019(18) 0.0015(19) 0.0067(15) C1 0.059(9) 0.033(7) 0.137(18) 0.013(10) 0.004(12) -0.008(6) C2 0.053(8) 0.071(9) 0.077(9) -0.049(7) 0.020(7) -0.018(6) C3 0.043(3) 0.043(3) 0.081(4) -0.002(3) -0.002(3) -0.014(2) C4 0.029(6) 0.075(8) 0.055(8) 0.000(7) -0.002(6) 0.003(5) C5 0.051(7) 0.046(6) 0.037(6) -0.005(5) 0.013(5) 0.007(5) C6 0.086(10) 0.061(8) 0.062(9) 0.024(7) 0.017(7) 0.038(7) C11 0.031(3) 0.054(4) 0.145(13) 0.011(4) -0.008(3) 0.009(3) Pd1' 0.02800(19) 0.02489(17) 0.0432(2) 0.00268(12) -0.00027(13) -0.00122(11) N1' 0.039(4) 0.025(3) 0.061(5) 0.006(4) -0.003(4) -0.004(3) N2' 0.036(2) 0.0344(18) 0.031(3) 0.0019(18) 0.0015(19) 0.0067(15) C1' 0.058(6) 0.058(6) 0.085(7) 0.040(5) 0.013(5) -0.010(5) C2' 0.073(8) 0.032(5) 0.089(9) -0.011(6) -0.014(7) 0.001(5) C3' 0.043(3) 0.043(3) 0.081(4) -0.002(3) -0.002(3) -0.014(2) C4' 0.032(4) 0.053(5) 0.073(7) 0.012(5) 0.008(5) -0.004(4) C5' 0.054(5) 0.051(5) 0.063(6) -0.011(4) -0.003(4) 0.019(4) C6' 0.045(4) 0.047(4) 0.042(4) 0.002(3) -0.007(3) 0.006(3) C11' 0.031(3) 0.054(4) 0.145(13) 0.011(4) -0.008(3) 0.009(3) C7 0.059(4) 0.134(6) 0.058(4) -0.038(4) -0.002(3) -0.024(4) C8 0.062(4) 0.093(4) 0.059(3) -0.015(3) -0.006(3) -0.035(3) C9 0.057(3) 0.100(5) 0.067(4) 0.035(3) -0.004(3) -0.042(3) C10 0.069(4) 0.155(7) 0.053(3) 0.034(4) -0.007(3) -0.049(5) C12 0.0211(16) 0.0282(17) 0.0177(16) 0.0020(13) 0.0026(13) -0.0055(13) C13 0.0224(17) 0.0299(18) 0.0221(17) -0.0018(14) -0.0018(14) -0.0034(14) C14 0.0281(19) 0.0340(19) 0.032(2) 0.0028(16) -0.0082(16) -0.0006(15) C15 0.042(2) 0.038(2) 0.056(3) -0.002(2) -0.024(2) 0.0003(19) C16 0.035(2) 0.042(2) 0.0237(18) 0.0046(16) -0.0107(16) -0.0085(17) C17 0.033(2) 0.035(2) 0.0180(17) -0.0005(14) 0.0007(14) -0.0087(16) C18 0.045(2) 0.046(2) 0.026(2) -0.0073(17) -0.0022(18) -0.010(2) C19 0.0233(17) 0.0293(18) 0.0223(17) -0.0003(14) 0.0015(14) -0.0046(14) C20 0.0184(16) 0.0254(16) 0.0176(16) -0.0012(13) -0.0028(12) 0.0024(13) C21 0.0223(17) 0.0247(17) 0.0191(16) -0.0012(13) -0.0010(13) -0.0008(13) C22 0.0284(18) 0.0300(18) 0.0166(16) -0.0043(13) 0.0013(13) 0.0037(14) C23 0.041(2) 0.038(2) 0.0234(19) -0.0078(16) 0.0047(16) 0.0038(18) C24 0.0255(18) 0.0318(18) 0.0183(16) 0.0034(14) 0.0041(14) 0.0052(14) C25 0.0210(17) 0.0245(17) 0.0236(17) 0.0034(13) 0.0002(13) 0.0001(13) C26 0.032(2) 0.0262(18) 0.032(2) 0.0034(15) 0.0078(16) -0.0022(15) C27 0.0204(17) 0.0253(16) 0.0178(16) -0.0015(13) 0.0005(13) 0.0021(13) C28 0.0171(16) 0.0277(17) 0.0206(16) 0.0002(13) 0.0017(13) -0.0018(13) C29 0.0208(17) 0.0269(17) 0.0246(17) 0.0003(14) 0.0002(13) -0.0014(13) C30 0.0236(18) 0.0259(18) 0.0330(19) 0.0023(15) 0.0050(15) 0.0017(14) C31 0.038(2) 0.028(2) 0.051(3) 0.0073(18) -0.0036(19) -0.0010(17) C32 0.0247(18) 0.0294(18) 0.0319(19) -0.0040(15) 0.0000(15) -0.0041(14) C33 0.0211(18) 0.035(2) 0.0283(19) -0.0015(15) -0.0013(14) -0.0030(15) C34 0.031(2) 0.048(2) 0.041(2) 0.0027(19) -0.0146(18) -0.0079(19) C35 0.0225(17) 0.0299(18) 0.0231(17) 0.0007(14) -0.0023(14) -0.0031(14) C36 0.0187(16) 0.0295(17) 0.0213(16) -0.0043(13) -0.0018(13) -0.0024(13) C37 0.0233(18) 0.038(2) 0.0256(18) -0.0052(15) 0.0016(14) 0.0004(15) C38 0.0223(18) 0.049(2) 0.031(2) -0.0149(18) -0.0001(15) 0.0032(17) C39 0.034(2) 0.082(4) 0.038(2) -0.024(2) 0.007(2) 0.010(2) C40 0.0219(19) 0.046(2) 0.051(3) -0.014(2) -0.0045(18) 0.0100(17) C41 0.028(2) 0.036(2) 0.048(2) 0.0017(18) -0.0043(18) 0.0063(16) C42 0.034(3) 0.058(3) 0.081(4) 0.020(3) -0.002(2) 0.018(2) C43 0.0215(17) 0.035(2) 0.0297(19) 0.0004(15) 0.0000(15) 0.0038(15) B1 0.0213(19) 0.0232(18) 0.0164(17) -0.0011(14) 0.0015(14) -0.0017(15) O1 0.0497(19) 0.0433(17) 0.0462(18) 0.0054(13) -0.0079(14) -0.0160(15) F1 0.068(2) 0.0533(17) 0.104(3) -0.0278(17) -0.0458(19) 0.0308(15) F2 0.0321(14) 0.0543(17) 0.120(3) 0.0070(18) -0.0107(16) 0.0075(13) F3 0.071(2) 0.0552(17) 0.088(2) 0.0299(17) -0.0206(18) 0.0093(16) F4 0.170(4) 0.083(2) 0.052(2) -0.0287(18) -0.070(2) 0.031(3) F5 0.085(2) 0.0488(16) 0.0518(17) -0.0178(13) 0.0111(15) -0.0287(15) F6 0.064(2) 0.113(3) 0.082(2) -0.072(2) 0.0374(18) -0.039(2) F7 0.0666(18) 0.0632(17) 0.0462(15) -0.0300(13) -0.0279(14) 0.0179(14) F8 0.080(2) 0.0642(18) 0.0465(16) -0.0236(14) 0.0370(15) -0.0128(16) F9 0.0741(19) 0.0349(13) 0.0356(13) -0.0080(10) -0.0003(12) 0.0141(12) F10 0.0282(13) 0.0439(15) 0.093(2) -0.0126(14) 0.0171(13) -0.0068(11) F11 0.086(2) 0.0514(16) 0.0548(17) 0.0289(14) -0.0133(16) -0.0250(16) F12 0.0432(14) 0.0337(12) 0.0486(14) -0.0101(11) 0.0140(11) -0.0121(10) F13 0.101(3) 0.073(2) 0.080(2) 0.0485(18) 0.053(2) 0.0369(19) F14 0.0508(16) 0.0452(15) 0.0725(19) 0.0216(14) -0.0135(14) 0.0071(12) F15 0.119(3) 0.0325(15) 0.107(3) 0.0196(16) -0.053(2) -0.0246(17) F16 0.061(2) 0.141(3) 0.0338(15) 0.0090(18) -0.0179(14) -0.032(2) F17 0.063(2) 0.073(2) 0.083(2) -0.0145(17) -0.0449(17) 0.0235(17) F18 0.071(2) 0.0580(18) 0.080(2) 0.0071(16) -0.0469(18) -0.0303(16) F19 0.0588(18) 0.0752(19) 0.0345(14) -0.0141(13) 0.0026(12) -0.0119(15) F20 0.103(3) 0.255(6) 0.054(2) -0.006(3) 0.022(2) 0.127(4) F21 0.103(3) 0.149(4) 0.077(2) -0.063(2) 0.067(2) -0.085(3) F22 0.065(2) 0.071(2) 0.110(3) 0.047(2) -0.008(2) -0.0014(17) F23 0.185(5) 0.111(4) 0.109(3) 0.064(3) -0.098(4) -0.055(4) F24 0.151(4) 0.133(4) 0.192(5) 0.096(4) 0.084(4) 0.116(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C11 2.030(12) . ? Pd1 N1 2.088(10) . ? Pd1 O1 2.116(3) . ? Pd1 N2 2.210(10) . ? N1 C1 1.466(16) . ? N1 C3 1.487(15) . ? N1 C2 1.550(15) . ? N2 C5 1.471(14) . ? N2 C6 1.486(13) . ? N2 C4 1.494(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.480(16) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N1' C1' 1.477(12) . ? N1' C3' 1.499(13) . ? N1' C2' 1.528(13) . ? N2' C5' 1.462(10) . ? N2' C4' 1.479(11) . ? N2' C6' 1.481(11) . ? C1' H1'1 0.9800 . ? C1' H1'2 0.9800 . ? C1' H1'3 0.9800 . ? C2' H2'1 0.9800 . ? C2' H2'2 0.9800 . ? C2' H2'3 0.9800 . ? C3' C4' 1.486(13) . ? C3' H3'1 0.9900 . ? C3' H3'2 0.9900 . ? C4' H4'1 0.9900 . ? C4' H4'2 0.9900 . ? C5' H5'1 0.9800 . ? C5' H5'2 0.9800 . ? C5' H5'3 0.9800 . ? C6' H6'1 0.9800 . ? C6' H6'2 0.9800 . ? C6' H6'3 0.9800 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C7 C8 1.483(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O1 1.454(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O1 1.458(6) . ? C9 C10 1.473(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 C19 1.390(5) . ? C12 C13 1.408(5) . ? C12 B1 1.644(5) . ? C13 C14 1.391(5) . ? C13 H13 0.9500 . ? C14 C16 1.403(6) . ? C14 C15 1.500(6) . ? C15 F1 1.330(5) . ? C15 F3 1.336(6) . ? C15 F2 1.337(6) . ? C16 C17 1.380(6) . ? C16 H16 0.9500 . ? C17 C19 1.408(5) . ? C17 C18 1.502(5) . ? C18 F4 1.318(5) . ? C18 F5 1.319(5) . ? C18 F6 1.321(5) . ? C19 H19 0.9500 . ? C20 C21 1.392(5) . ? C20 C27 1.405(5) . ? C20 B1 1.646(5) . ? C21 C22 1.405(5) . ? C21 H21 0.9500 . ? C22 C24 1.382(5) . ? C22 C23 1.503(5) . ? C23 F8 1.330(5) . ? C23 F9 1.336(5) . ? C23 F7 1.340(5) . ? C24 C25 1.388(5) . ? C24 H24 0.9500 . ? C25 C27 1.394(5) . ? C25 C26 1.500(5) . ? C26 F11 1.325(5) . ? C26 F12 1.328(4) . ? C26 F10 1.356(5) . ? C27 H27 0.9500 . ? C28 C29 1.394(5) . ? C28 C35 1.406(5) . ? C28 B1 1.641(5) . ? C29 C30 1.403(5) . ? C29 H29 0.9500 . ? C30 C32 1.383(5) . ? C30 C31 1.494(5) . ? C31 F13 1.321(5) . ? C31 F15 1.326(5) . ? C31 F14 1.334(5) . ? C32 C33 1.389(5) . ? C32 H32 0.9500 . ? C33 C35 1.383(5) . ? C33 C34 1.491(5) . ? C34 F17 1.326(6) . ? C34 F16 1.330(5) . ? C34 F18 1.335(5) . ? C35 H35 0.9500 . ? C36 C43 1.392(5) . ? C36 C37 1.407(5) . ? C36 B1 1.643(5) . ? C37 C38 1.394(5) . ? C37 H37 0.9500 . ? C38 C40 1.381(6) . ? C38 C39 1.495(6) . ? C39 F20 1.313(6) . ? C39 F19 1.317(5) . ? C39 F21 1.321(7) . ? C40 C41 1.379(6) . ? C40 H40 0.9500 . ? C41 C43 1.397(5) . ? C41 C42 1.487(6) . ? C42 F23 1.297(7) . ? C42 F24 1.310(6) . ? C42 F22 1.313(6) . ? C43 H43 0.9500 . ? 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 C11 Pd1 N1 92.5(11) . . ? C11 Pd1 O1 88.9(11) . . ? N1 Pd1 O1 165.4(4) . . ? C11 Pd1 N2 175(2) . . ? N1 Pd1 N2 83.7(4) . . ? O1 Pd1 N2 95.7(4) . . ? C1 N1 C3 110.8(13) . . ? C1 N1 C2 108.5(11) . . ? C3 N1 C2 107.1(15) . . ? C1 N1 Pd1 114.0(10) . . ? C3 N1 Pd1 107.1(8) . . ? C2 N1 Pd1 109.1(8) . . ? C5 N2 C6 106.9(10) . . ? C5 N2 C4 111.2(11) . . ? C6 N2 C4 109.7(12) . . ? C5 N2 Pd1 108.5(8) . . ? C6 N2 Pd1 116.5(9) . . ? C4 N2 Pd1 104.0(7) . . ? C4 C3 N1 112.7(14) . . ? C4 C3 H3A 109.1 . . ? N1 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? N1 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C3 C4 N2 110.0(12) . . ? C3 C4 H4A 109.7 . . ? N2 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? N2 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C1' N1' C3' 112.0(11) . . ? C1' N1' C2' 109.4(8) . . ? C3' N1' C2' 105.1(10) . . ? C5' N2' C4' 109.8(8) . . ? C5' N2' C6' 108.4(7) . . ? C4' N2' C6' 109.7(8) . . ? N1' C1' H1'1 109.5 . . ? N1' C1' H1'2 109.5 . . ? H1'1 C1' H1'2 109.5 . . ? N1' C1' H1'3 109.5 . . ? H1'1 C1' H1'3 109.5 . . ? H1'2 C1' H1'3 109.5 . . ? N1' C2' H2'1 109.5 . . ? N1' C2' H2'2 109.5 . . ? H2'1 C2' H2'2 109.5 . . ? N1' C2' H2'3 109.5 . . ? H2'1 C2' H2'3 109.5 . . ? H2'2 C2' H2'3 109.5 . . ? C4' C3' N1' 110.4(11) . . ? C4' C3' H3'1 109.6 . . ? N1' C3' H3'1 109.6 . . ? C4' C3' H3'2 109.6 . . ? N1' C3' H3'2 109.6 . . ? H3'1 C3' H3'2 108.1 . . ? N2' C4' C3' 111.9(9) . . ? N2' C4' H4'1 109.2 . . ? C3' C4' H4'1 109.2 . . ? N2' C4' H4'2 109.2 . . ? C3' C4' H4'2 109.2 . . ? H4'1 C4' H4'2 107.9 . . ? N2' C5' H5'1 109.5 . . ? N2' C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? N2' C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? N2' C6' H6'1 109.5 . . ? N2' C6' H6'2 109.5 . . ? H6'1 C6' H6'2 109.5 . . ? N2' C6' H6'3 109.5 . . ? H6'1 C6' H6'3 109.5 . . ? H6'2 C6' H6'3 109.5 . . ? H11D C11' H11E 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 C7 110.6(4) . . ? O1 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O1 C9 C10 110.6(4) . . ? O1 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? O1 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C19 C12 C13 116.2(3) . . ? C19 C12 B1 124.7(3) . . ? C13 C12 B1 118.9(3) . . ? C14 C13 C12 122.2(3) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C16 120.7(4) . . ? C13 C14 C15 121.0(4) . . ? C16 C14 C15 118.2(3) . . ? F1 C15 F3 106.3(4) . . ? F1 C15 F2 106.4(4) . . ? F3 C15 F2 106.0(4) . . ? F1 C15 C14 113.3(3) . . ? F3 C15 C14 112.3(4) . . ? F2 C15 C14 112.0(4) . . ? C17 C16 C14 117.8(3) . . ? C17 C16 H16 121.1 . . ? C14 C16 H16 121.1 . . ? C16 C17 C19 121.1(3) . . ? C16 C17 C18 120.4(3) . . ? C19 C17 C18 118.4(4) . . ? F4 C18 F5 104.2(4) . . ? F4 C18 F6 107.4(4) . . ? F5 C18 F6 105.6(4) . . ? F4 C18 C17 113.2(4) . . ? F5 C18 C17 112.5(3) . . ? F6 C18 C17 113.2(3) . . ? C12 C19 C17 122.0(3) . . ? C12 C19 H19 119.0 . . ? C17 C19 H19 119.0 . . ? C21 C20 C27 115.7(3) . . ? C21 C20 B1 123.8(3) . . ? C27 C20 B1 120.1(3) . . ? C20 C21 C22 122.2(3) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C24 C22 C21 120.8(3) . . ? C24 C22 C23 120.5(3) . . ? C21 C22 C23 118.6(3) . . ? F8 C23 F9 105.8(3) . . ? F8 C23 F7 107.0(3) . . ? F9 C23 F7 105.4(3) . . ? F8 C23 C22 113.4(3) . . ? F9 C23 C22 112.3(3) . . ? F7 C23 C22 112.4(3) . . ? C22 C24 C25 118.1(3) . . ? C22 C24 H24 121.0 . . ? C25 C24 H24 121.0 . . ? C24 C25 C27 120.8(3) . . ? C24 C25 C26 118.1(3) . . ? C27 C25 C26 121.0(3) . . ? F11 C26 F12 108.5(3) . . ? F11 C26 F10 104.2(3) . . ? F12 C26 F10 104.7(3) . . ? F11 C26 C25 113.1(3) . . ? F12 C26 C25 114.1(3) . . ? F10 C26 C25 111.4(3) . . ? C25 C27 C20 122.3(3) . . ? C25 C27 H27 118.9 . . ? C20 C27 H27 118.9 . . ? C29 C28 C35 115.6(3) . . ? C29 C28 B1 126.7(3) . . ? C35 C28 B1 117.7(3) . . ? C28 C29 C30 122.1(3) . . ? C28 C29 H29 119.0 . . ? C30 C29 H29 119.0 . . ? C32 C30 C29 121.1(3) . . ? C32 C30 C31 119.3(3) . . ? C29 C30 C31 119.5(3) . . ? F13 C31 F15 107.1(4) . . ? F13 C31 F14 105.2(4) . . ? F15 C31 F14 104.9(4) . . ? F13 C31 C30 112.0(3) . . ? F15 C31 C30 113.6(4) . . ? F14 C31 C30 113.3(3) . . ? C30 C32 C33 117.6(3) . . ? C30 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? C35 C33 C32 121.2(3) . . ? C35 C33 C34 118.5(3) . . ? C32 C33 C34 120.3(3) . . ? F17 C34 F16 105.1(4) . . ? F17 C34 F18 106.3(4) . . ? F16 C34 F18 105.3(4) . . ? F17 C34 C33 113.1(4) . . ? F16 C34 C33 112.4(3) . . ? F18 C34 C33 113.8(4) . . ? C33 C35 C28 122.4(3) . . ? C33 C35 H35 118.8 . . ? C28 C35 H35 118.8 . . ? C43 C36 C37 115.7(3) . . ? C43 C36 B1 125.6(3) . . ? C37 C36 B1 118.7(3) . . ? C38 C37 C36 122.2(4) . . ? C38 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C40 C38 C37 120.8(4) . . ? C40 C38 C39 120.3(4) . . ? C37 C38 C39 118.9(4) . . ? F20 C39 F19 105.7(4) . . ? F20 C39 F21 106.0(5) . . ? F19 C39 F21 104.9(5) . . ? F20 C39 C38 113.5(5) . . ? F19 C39 C38 112.8(4) . . ? F21 C39 C38 113.2(4) . . ? C41 C40 C38 118.1(4) . . ? C41 C40 H40 120.9 . . ? C38 C40 H40 120.9 . . ? C40 C41 C43 121.2(4) . . ? C40 C41 C42 119.5(4) . . ? C43 C41 C42 119.4(4) . . ? F23 C42 F24 104.6(5) . . ? F23 C42 F22 104.9(5) . . ? F24 C42 F22 105.9(5) . . ? F23 C42 C41 113.8(5) . . ? F24 C42 C41 113.7(5) . . ? F22 C42 C41 113.2(4) . . ? C36 C43 C41 122.0(4) . . ? C36 C43 H43 119.0 . . ? C41 C43 H43 119.0 . . ? C28 B1 C36 105.4(3) . . ? C28 B1 C12 112.5(3) . . ? C36 B1 C12 111.4(3) . . ? C28 B1 C20 109.7(3) . . ? C36 B1 C20 113.2(3) . . ? C12 B1 C20 104.7(3) . . ? C8 O1 C9 108.0(4) . . ? C8 O1 Pd1 119.6(3) . . ? C9 O1 Pd1 116.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Pd1 N1 C1 -42(3) . . . . ? O1 Pd1 N1 C1 -137.1(14) . . . . ? N2 Pd1 N1 C1 134.3(12) . . . . ? C11 Pd1 N1 C3 -165(3) . . . . ? O1 Pd1 N1 C3 99.9(18) . . . . ? N2 Pd1 N1 C3 11.3(14) . . . . ? C11 Pd1 N1 C2 79(3) . . . . ? O1 Pd1 N1 C2 -15.6(17) . . . . ? N2 Pd1 N1 C2 -104.2(9) . . . . ? C11 Pd1 N2 C5 -59(28) . . . . ? N1 Pd1 N2 C5 -103.1(9) . . . . ? O1 Pd1 N2 C5 91.6(8) . . . . ? C11 Pd1 N2 C6 -180(100) . . . . ? N1 Pd1 N2 C6 136.3(11) . . . . ? O1 Pd1 N2 C6 -29.0(11) . . . . ? C11 Pd1 N2 C4 59(28) . . . . ? N1 Pd1 N2 C4 15.4(9) . . . . ? O1 Pd1 N2 C4 -149.9(9) . . . . ? C1 N1 C3 C4 -163.4(18) . . . . ? C2 N1 C3 C4 78(2) . . . . ? Pd1 N1 C3 C4 -38(2) . . . . ? N1 C3 C4 N2 55(3) . . . . ? C5 N2 C4 C3 76.5(16) . . . . ? C6 N2 C4 C3 -165.4(15) . . . . ? Pd1 N2 C4 C3 -40.1(16) . . . . ? C1' N1' C3' C4' -78.0(14) . . . . ? C2' N1' C3' C4' 163.3(12) . . . . ? C5' N2' C4' C3' 162.0(11) . . . . ? C6' N2' C4' C3' -79.0(13) . . . . ? N1' C3' C4' N2' -57.9(18) . . . . ? C19 C12 C13 C14 -2.1(5) . . . . ? B1 C12 C13 C14 -177.6(3) . . . . ? C12 C13 C14 C16 1.1(6) . . . . ? C12 C13 C14 C15 178.9(4) . . . . ? C13 C14 C15 F1 7.4(6) . . . . ? C16 C14 C15 F1 -174.8(4) . . . . ? C13 C14 C15 F3 127.8(4) . . . . ? C16 C14 C15 F3 -54.3(5) . . . . ? C13 C14 C15 F2 -113.0(4) . . . . ? C16 C14 C15 F2 64.9(5) . . . . ? C13 C14 C16 C17 0.5(6) . . . . ? C15 C14 C16 C17 -177.4(4) . . . . ? C14 C16 C17 C19 -0.9(6) . . . . ? C14 C16 C17 C18 176.7(4) . . . . ? C16 C17 C18 F4 9.0(6) . . . . ? C19 C17 C18 F4 -173.3(4) . . . . ? C16 C17 C18 F5 -108.9(4) . . . . ? C19 C17 C18 F5 68.8(5) . . . . ? C16 C17 C18 F6 131.4(4) . . . . ? C19 C17 C18 F6 -50.9(5) . . . . ? C13 C12 C19 C17 1.7(5) . . . . ? B1 C12 C19 C17 176.9(3) . . . . ? C16 C17 C19 C12 -0.2(5) . . . . ? C18 C17 C19 C12 -177.9(3) . . . . ? C27 C20 C21 C22 1.2(5) . . . . ? B1 C20 C21 C22 174.9(3) . . . . ? C20 C21 C22 C24 0.1(5) . . . . ? C20 C21 C22 C23 -179.2(3) . . . . ? C24 C22 C23 F8 -9.1(5) . . . . ? C21 C22 C23 F8 170.2(3) . . . . ? C24 C22 C23 F9 -128.9(4) . . . . ? C21 C22 C23 F9 50.3(5) . . . . ? C24 C22 C23 F7 112.4(4) . . . . ? C21 C22 C23 F7 -68.3(5) . . . . ? C21 C22 C24 C25 -1.0(5) . . . . ? C23 C22 C24 C25 178.3(3) . . . . ? C22 C24 C25 C27 0.6(5) . . . . ? C22 C24 C25 C26 -178.1(3) . . . . ? C24 C25 C26 F11 -62.3(5) . . . . ? C27 C25 C26 F11 119.0(4) . . . . ? C24 C25 C26 F12 173.0(3) . . . . ? C27 C25 C26 F12 -5.6(5) . . . . ? C24 C25 C26 F10 54.7(4) . . . . ? C27 C25 C26 F10 -123.9(4) . . . . ? C24 C25 C27 C20 0.7(5) . . . . ? C26 C25 C27 C20 179.3(3) . . . . ? C21 C20 C27 C25 -1.6(5) . . . . ? B1 C20 C27 C25 -175.6(3) . . . . ? C35 C28 C29 C30 -1.8(5) . . . . ? B1 C28 C29 C30 177.5(3) . . . . ? C28 C29 C30 C32 0.4(5) . . . . ? C28 C29 C30 C31 178.6(3) . . . . ? C32 C30 C31 F13 101.0(5) . . . . ? C29 C30 C31 F13 -77.2(5) . . . . ? C32 C30 C31 F15 -20.5(6) . . . . ? C29 C30 C31 F15 161.3(4) . . . . ? C32 C30 C31 F14 -140.1(4) . . . . ? C29 C30 C31 F14 41.7(5) . . . . ? C29 C30 C32 C33 1.2(5) . . . . ? C31 C30 C32 C33 -177.0(4) . . . . ? C30 C32 C33 C35 -1.4(5) . . . . ? C30 C32 C33 C34 179.2(4) . . . . ? C35 C33 C34 F17 59.1(5) . . . . ? C32 C33 C34 F17 -121.4(4) . . . . ? C35 C33 C34 F16 -59.7(5) . . . . ? C32 C33 C34 F16 119.8(4) . . . . ? C35 C33 C34 F18 -179.4(4) . . . . ? C32 C33 C34 F18 0.1(6) . . . . ? C32 C33 C35 C28 -0.1(6) . . . . ? C34 C33 C35 C28 179.4(4) . . . . ? C29 C28 C35 C33 1.6(5) . . . . ? B1 C28 C35 C33 -177.7(3) . . . . ? C43 C36 C37 C38 1.5(5) . . . . ? B1 C36 C37 C38 179.0(3) . . . . ? C36 C37 C38 C40 -2.0(6) . . . . ? C36 C37 C38 C39 175.4(4) . . . . ? C40 C38 C39 F20 -10.9(7) . . . . ? C37 C38 C39 F20 171.7(5) . . . . ? C40 C38 C39 F19 109.3(5) . . . . ? C37 C38 C39 F19 -68.0(6) . . . . ? C40 C38 C39 F21 -131.8(5) . . . . ? C37 C38 C39 F21 50.8(6) . . . . ? C37 C38 C40 C41 0.9(6) . . . . ? C39 C38 C40 C41 -176.4(4) . . . . ? C38 C40 C41 C43 0.4(6) . . . . ? C38 C40 C41 C42 -179.7(4) . . . . ? C40 C41 C42 F23 116.5(6) . . . . ? C43 C41 C42 F23 -63.6(6) . . . . ? C40 C41 C42 F24 -3.0(8) . . . . ? C43 C41 C42 F24 176.8(5) . . . . ? C40 C41 C42 F22 -123.9(5) . . . . ? C43 C41 C42 F22 56.0(7) . . . . ? C37 C36 C43 C41 -0.2(5) . . . . ? B1 C36 C43 C41 -177.4(3) . . . . ? C40 C41 C43 C36 -0.8(6) . . . . ? C42 C41 C43 C36 179.3(4) . . . . ? C29 C28 B1 C36 122.3(4) . . . . ? C35 C28 B1 C36 -58.4(4) . . . . ? C29 C28 B1 C12 0.7(5) . . . . ? C35 C28 B1 C12 180.0(3) . . . . ? C29 C28 B1 C20 -115.4(4) . . . . ? C35 C28 B1 C20 63.8(4) . . . . ? C43 C36 B1 C28 111.7(4) . . . . ? C37 C36 B1 C28 -65.5(4) . . . . ? C43 C36 B1 C12 -126.0(4) . . . . ? C37 C36 B1 C12 56.8(4) . . . . ? C43 C36 B1 C20 -8.2(5) . . . . ? C37 C36 B1 C20 174.6(3) . . . . ? C19 C12 B1 C28 127.5(3) . . . . ? C13 C12 B1 C28 -57.4(4) . . . . ? C19 C12 B1 C36 9.4(4) . . . . ? C13 C12 B1 C36 -175.5(3) . . . . ? C19 C12 B1 C20 -113.4(3) . . . . ? C13 C12 B1 C20 61.7(4) . . . . ? C21 C20 B1 C28 9.3(4) . . . . ? C27 C20 B1 C28 -177.2(3) . . . . ? C21 C20 B1 C36 126.7(3) . . . . ? C27 C20 B1 C36 -59.8(4) . . . . ? C21 C20 B1 C12 -111.7(3) . . . . ? C27 C20 B1 C12 61.8(4) . . . . ? C7 C8 O1 C9 176.6(6) . . . . ? C7 C8 O1 Pd1 40.8(7) . . . . ? C10 C9 O1 C8 174.1(6) . . . . ? C10 C9 O1 Pd1 -48.3(7) . . . . ? C11 Pd1 O1 C8 70(3) . . . . ? N1 Pd1 O1 C8 165.2(12) . . . . ? N2 Pd1 O1 C8 -107.8(5) . . . . ? C11 Pd1 O1 C9 -63(3) . . . . ? N1 Pd1 O1 C9 32.8(13) . . . . ? N2 Pd1 O1 C9 119.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.155 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.100