data_shelxl _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24 F6 N2 O10 Pd' _chemical_formula_weight 864.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.9656(11) _cell_length_b 9.6793(7) _cell_length_c 21.8956(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.748(3) _cell_angle_gamma 90.00 _cell_volume 3805.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _exptl_crystal_description rod _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details '(SADABS; Sheldrick, 2007)' _exptl_absorpt_correction_T_min 0.5019 _exptl_absorpt_correction_T_max 0.7456 _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CCD Area Detector' _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 141143 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.73 _reflns_number_total 8803 _reflns_number_gt 7923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0367P)^2^+87.6152P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8803 _refine_ls_number_parameters 535 _refine_ls_number_restraints 259 _refine_ls_R_factor_all 0.1153 _refine_ls_R_factor_gt 0.1089 _refine_ls_wR_factor_ref 0.2578 _refine_ls_wR_factor_gt 0.2554 _refine_ls_goodness_of_fit_ref 1.235 _refine_ls_restrained_S_all 1.221 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _refine_special_details ; The crystal grew as a non-merohedral twin. The twin components were related by a rotation of 180 degs about the a* reciprocal axis. ; 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.50083(3) 0.67733(6) 0.78290(3) 0.01680(17) Uani 1 1 d . . . O1 O 0.6159(3) 0.4903(6) 0.6416(3) 0.0202(12) Uani 1 1 d . . . O2 O 0.5786(4) 0.5921(6) 0.5525(3) 0.0271(14) Uani 1 1 d . . . O3 O 0.7514(4) 0.1523(7) 0.8614(3) 0.0308(15) Uani 1 1 d . . . O4 O 0.3765(3) 0.8586(5) 0.6385(3) 0.0190(12) Uani 1 1 d . . . O5 O 0.4054(4) 0.7509(6) 0.5515(3) 0.0260(13) Uani 1 1 d . . . O6 O 0.2533(4) 1.1953(7) 0.8589(3) 0.0290(14) Uani 1 1 d . . . O7 O 0.5754(3) 0.6283(6) 0.8494(3) 0.0204(12) Uani 1 1 d . . . O8 O 0.6304(4) 0.8381(8) 0.8414(3) 0.0428(19) Uani 1 1 d . . . O9 O 0.4306(3) 0.7261(6) 0.8492(3) 0.0206(12) Uani 1 1 d . . . O10 O 0.3807(4) 0.5119(8) 0.8468(3) 0.0349(16) Uani 1 1 d . . . N1 N 0.5641(4) 0.6236(7) 0.7121(3) 0.0161(13) Uani 1 1 d . . . N2 N 0.4316(4) 0.7283(7) 0.7113(3) 0.0157(13) Uani 1 1 d . . . C1 C 0.5401(4) 0.6845(8) 0.6528(3) 0.0161(14) Uani 1 1 d . . . C2 C 0.5779(5) 0.5897(8) 0.6061(4) 0.0199(16) Uani 1 1 d . . . C3 C 0.6039(4) 0.5131(8) 0.7015(4) 0.0181(16) Uani 1 1 d . . . C4 C 0.6371(5) 0.4150(8) 0.7437(4) 0.0215(17) Uani 1 1 d . . . C5 C 0.7090(5) 0.3645(9) 0.7309(4) 0.0235(17) Uani 1 1 d . . . H5 H 0.7321 0.3916 0.6954 0.031 Uiso 1 1 calc R . . C6 C 0.7443(5) 0.2760(9) 0.7707(4) 0.0267(18) Uani 1 1 d . . . H6 H 0.7915 0.2430 0.7623 0.036 Uiso 1 1 calc R . . C7 C 0.7097(5) 0.2344(9) 0.8245(4) 0.0262(18) Uani 1 1 d . . . C8 C 0.6369(5) 0.2771(9) 0.8358(4) 0.0246(18) Uani 1 1 d . . . H8 H 0.6128 0.2454 0.8701 0.033 Uiso 1 1 calc R . . C9 C 0.6010(5) 0.3676(8) 0.7952(4) 0.0232(17) Uani 1 1 d . . . H9 H 0.5528 0.3967 0.8025 0.031 Uiso 1 1 calc R . . C10 C 0.7201(7) 0.1096(12) 0.9192(4) 0.039(3) Uani 1 1 d . . . H10a H 0.7097 0.1898 0.9433 0.059 Uiso 1 1 calc R . . H10b H 0.7551 0.0517 0.9411 0.059 Uiso 1 1 calc R . . H10c H 0.6748 0.0592 0.9113 0.059 Uiso 1 1 calc R . . C11 C 0.5621(5) 0.8375(8) 0.6447(4) 0.0234(17) Uani 1 1 d U . . C12 C 0.5609(6) 0.8923(9) 0.5861(4) 0.0282(19) Uani 1 1 d U . . H12 H 0.5497 0.8362 0.5526 0.038 Uiso 1 1 calc R . . C13 C 0.5764(6) 1.0306(9) 0.5779(4) 0.0272(19) Uani 1 1 d U . . H13 H 0.5757 1.0680 0.5388 0.036 Uiso 1 1 calc R . . C14 C 0.5929(5) 1.1139(9) 0.6283(5) 0.0294(19) Uani 1 1 d U . . H14 H 0.6032 1.2071 0.6227 0.039 Uiso 1 1 calc R . . C15 C 0.5941(5) 1.0592(9) 0.6859(4) 0.0280(19) Uani 1 1 d U . . H15 H 0.6050 1.1159 0.7193 0.037 Uiso 1 1 calc R . . C16 C 0.5793(5) 0.9186(9) 0.6953(4) 0.0238(17) Uani 1 1 d U . . H16 H 0.5809 0.8810 0.7344 0.032 Uiso 1 1 calc R . . C17 C 0.4526(4) 0.6653(8) 0.6526(3) 0.0175(15) Uani 1 1 d . . . C18 C 0.4101(5) 0.7558(8) 0.6051(4) 0.0216(17) Uani 1 1 d . . . C19 C 0.3922(5) 0.8391(8) 0.6990(4) 0.0196(16) Uani 1 1 d . . . C20 C 0.3603(4) 0.9379(8) 0.7403(4) 0.0185(16) Uani 1 1 d . . . C21 C 0.2890(5) 0.9846(8) 0.7275(4) 0.0211(17) Uani 1 1 d . . . H21 H 0.2639 0.9564 0.6920 0.028 Uiso 1 1 calc R . . C22 C 0.2549(5) 1.0730(8) 0.7675(4) 0.0213(17) Uani 1 1 d . . . H22 H 0.2071 1.1054 0.7586 0.028 Uiso 1 1 calc R . . C23 C 0.2931(5) 1.1142(8) 0.8219(4) 0.0195(16) Uani 1 1 d . . . C24 C 0.3663(5) 1.0722(9) 0.8328(4) 0.0217(17) Uani 1 1 d . . . H24 H 0.3924 1.1036 0.8674 0.029 Uiso 1 1 calc R . . C25 C 0.4003(5) 0.9850(8) 0.7930(4) 0.0215(17) Uani 1 1 d . . . H25 H 0.4492 0.9570 0.8005 0.029 Uiso 1 1 calc R . . C26 C 0.2884(6) 1.2364(11) 0.9157(4) 0.032(2) Uani 1 1 d . . . H26a H 0.3018 1.1557 0.9390 0.048 Uiso 1 1 calc R . . H26b H 0.2545 1.2918 0.9382 0.048 Uiso 1 1 calc R . . H26c H 0.3323 1.2890 0.9078 0.048 Uiso 1 1 calc R . . C27 C 0.4289(5) 0.5123(8) 0.6467(4) 0.0205(16) Uani 1 1 d . . . C28 C 0.4239(6) 0.4500(10) 0.5887(4) 0.031(2) Uani 1 1 d . . . H28 H 0.4320 0.5020 0.5538 0.041 Uiso 1 1 calc R . . C29 C 0.4072(7) 0.3130(11) 0.5839(5) 0.043(3) Uani 1 1 d . . . H29 H 0.4030 0.2734 0.5452 0.057 Uiso 1 1 calc R . . C30 C 0.3963(7) 0.2315(10) 0.6339(5) 0.038(2) Uani 1 1 d . . . H30 H 0.3861 0.1378 0.6293 0.050 Uiso 1 1 calc R . . C31 C 0.4005(5) 0.2916(9) 0.6925(4) 0.0276(19) Uani 1 1 d . . . H31 H 0.3920 0.2383 0.7269 0.037 Uiso 1 1 calc R . . C32 C 0.4179(5) 0.4332(8) 0.6986(4) 0.0192(16) Uani 1 1 d . . . H32 H 0.4220 0.4734 0.7372 0.025 Uiso 1 1 calc R . . C33 C 0.6236(5) 0.7221(10) 0.8615(4) 0.0251(18) Uani 1 1 d . . . C34 C 0.6864(5) 0.6617(8) 0.9079(4) 0.042(2) Uani 1 1 d GU . . F1 F 0.7317(7) 0.5904(13) 0.8744(5) 0.055(3) Uani 0.60 1 d PGU . . F2 F 0.7218(10) 0.7685(15) 0.9314(9) 0.055(5) Uani 0.60 1 d PGU . . F3 F 0.6625(8) 0.5835(13) 0.9521(6) 0.057(4) Uani 0.60 1 d PGU . . C35 C 0.3869(5) 0.6306(10) 0.8641(4) 0.0236(17) Uani 1 1 d U . . C36 C 0.3287(5) 0.6898(8) 0.9111(4) 0.044(2) Uani 1 1 d GU . . F4 F 0.2761(6) 0.7498(14) 0.8780(5) 0.062(3) Uani 0.55 1 d PGU . . F5 F 0.3574(6) 0.7790(13) 0.9502(5) 0.062(3) Uani 0.55 1 d PGU . . F6 F 0.3006(10) 0.5856(14) 0.9408(8) 0.072(5) Uani 0.55 1 d PGU . . F1' F 0.6458(14) 0.648(2) 0.9612(10) 0.066(5) Uani 0.40 1 d PGU . . F2' F 0.7377(15) 0.759(2) 0.9252(16) 0.049(5) Uani 0.40 1 d PGU . . F3' F 0.7141(13) 0.5533(17) 0.8948(9) 0.055(4) Uani 0.40 1 d PGU . . F4' F 0.3760(9) 0.678(2) 0.9680(7) 0.075(4) Uani 0.45 1 d PGU . . F5' F 0.2784(11) 0.5886(15) 0.9260(11) 0.059(4) Uani 0.45 1 d PGU . . F6' F 0.3067(11) 0.7988(13) 0.9075(8) 0.064(4) Uani 0.45 1 d PGU . . 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 0.0205(3) 0.0113(3) 0.0186(3) -0.0027(2) 0.0017(2) 0.0013(2) O1 0.025(3) 0.013(3) 0.023(3) -0.002(2) 0.004(2) 0.002(2) O2 0.048(4) 0.021(3) 0.013(3) -0.003(2) 0.007(3) 0.003(3) O3 0.035(4) 0.028(3) 0.030(3) 0.007(3) 0.004(3) 0.010(3) O4 0.026(3) 0.009(2) 0.022(3) -0.001(2) -0.002(2) 0.001(2) O5 0.044(4) 0.020(3) 0.013(3) 0.001(2) -0.001(2) 0.000(3) O6 0.035(4) 0.026(3) 0.026(3) -0.010(3) -0.003(3) 0.015(3) O7 0.025(3) 0.020(3) 0.017(3) 0.001(2) -0.001(2) 0.004(2) O8 0.053(5) 0.040(4) 0.035(4) 0.007(3) -0.006(3) -0.021(4) O9 0.028(3) 0.019(3) 0.015(3) -0.001(2) 0.005(2) 0.001(2) O10 0.045(4) 0.035(4) 0.024(3) -0.003(3) 0.003(3) -0.009(3) N1 0.024(3) 0.010(3) 0.015(3) -0.004(2) 0.001(3) -0.002(3) N2 0.018(3) 0.010(3) 0.019(3) -0.006(2) 0.002(2) -0.003(2) C1 0.018(4) 0.013(3) 0.018(3) -0.002(3) 0.002(3) -0.001(3) C2 0.027(4) 0.016(4) 0.017(4) -0.001(3) 0.006(3) -0.005(3) C3 0.019(4) 0.012(3) 0.024(4) -0.002(3) 0.000(3) -0.002(3) C4 0.027(4) 0.014(4) 0.024(4) -0.001(3) 0.003(3) 0.001(3) C5 0.025(4) 0.016(4) 0.031(4) -0.001(3) 0.008(3) -0.001(3) C6 0.026(4) 0.022(4) 0.032(5) 0.000(4) 0.006(4) 0.001(3) C7 0.031(5) 0.021(4) 0.027(4) -0.002(4) 0.003(4) 0.004(4) C8 0.034(5) 0.017(4) 0.024(4) -0.002(3) 0.009(4) 0.002(3) C9 0.025(4) 0.014(4) 0.031(4) -0.006(3) 0.007(3) 0.002(3) C10 0.061(7) 0.037(6) 0.020(5) 0.002(4) 0.001(4) 0.008(5) C11 0.030(4) 0.011(3) 0.029(4) 0.003(3) 0.004(3) -0.006(3) C12 0.040(5) 0.017(4) 0.028(4) -0.004(3) 0.007(4) -0.006(4) C13 0.051(6) 0.021(4) 0.010(3) 0.004(3) 0.006(3) 0.003(4) C14 0.036(5) 0.013(4) 0.040(5) -0.004(3) 0.001(4) -0.012(4) C15 0.035(5) 0.015(4) 0.034(4) -0.006(3) 0.000(4) -0.008(4) C16 0.033(5) 0.017(4) 0.023(4) -0.005(3) 0.008(3) -0.001(3) C17 0.020(4) 0.015(4) 0.018(4) 0.005(3) 0.003(3) -0.006(3) C18 0.031(5) 0.015(4) 0.020(4) 0.000(3) 0.009(3) -0.003(3) C19 0.024(4) 0.013(4) 0.022(4) 0.000(3) -0.003(3) -0.005(3) C20 0.019(4) 0.014(4) 0.023(4) -0.001(3) 0.002(3) 0.002(3) C21 0.021(4) 0.016(4) 0.026(4) -0.002(3) -0.003(3) 0.001(3) C22 0.025(4) 0.017(4) 0.021(4) -0.002(3) -0.008(3) 0.006(3) C23 0.025(4) 0.015(4) 0.019(4) -0.003(3) 0.002(3) 0.004(3) C24 0.029(4) 0.021(4) 0.015(4) -0.008(3) -0.006(3) -0.003(3) C25 0.028(4) 0.013(4) 0.024(4) -0.003(3) 0.002(3) 0.007(3) C26 0.041(6) 0.033(5) 0.022(4) -0.015(4) -0.002(4) 0.005(4) C27 0.023(4) 0.014(4) 0.025(4) -0.005(3) 0.002(3) 0.001(3) C28 0.043(6) 0.021(4) 0.029(5) 0.003(4) 0.004(4) -0.009(4) C29 0.076(8) 0.024(5) 0.029(5) -0.014(4) 0.010(5) -0.009(5) C30 0.063(7) 0.016(4) 0.034(5) -0.007(4) 0.008(5) -0.014(4) C31 0.038(5) 0.013(4) 0.032(5) -0.001(3) 0.002(4) -0.005(3) C32 0.027(4) 0.013(4) 0.018(4) -0.003(3) 0.003(3) -0.005(3) C33 0.032(5) 0.032(5) 0.011(4) -0.005(3) 0.002(3) 0.001(4) C34 0.044(6) 0.052(5) 0.030(4) -0.002(4) -0.011(4) -0.007(4) F1 0.041(7) 0.068(9) 0.055(8) -0.003(6) -0.004(5) 0.008(6) F2 0.044(11) 0.073(9) 0.048(9) -0.015(7) -0.017(7) -0.015(8) F3 0.054(8) 0.073(9) 0.043(7) 0.026(7) -0.015(5) -0.001(7) C35 0.028(4) 0.030(4) 0.013(3) 0.002(3) -0.002(3) 0.003(3) C36 0.053(6) 0.042(5) 0.038(5) -0.005(4) 0.021(4) 0.003(4) F4 0.048(7) 0.077(9) 0.063(8) -0.004(6) 0.015(5) 0.026(7) F5 0.064(8) 0.080(8) 0.045(7) -0.038(6) 0.031(5) -0.002(6) F6 0.080(13) 0.068(8) 0.070(11) 0.017(7) 0.044(7) -0.005(8) F1' 0.072(13) 0.090(14) 0.034(8) 0.010(11) -0.005(7) -0.010(11) F2' 0.024(9) 0.049(8) 0.072(17) 0.005(8) -0.028(7) 0.008(6) F3' 0.065(8) 0.049(6) 0.051(7) 0.013(6) -0.021(5) 0.012(6) F4' 0.095(10) 0.100(11) 0.031(6) -0.027(8) 0.011(6) 0.016(9) F5' 0.048(9) 0.050(7) 0.081(13) -0.002(7) 0.048(7) 0.011(6) F6' 0.082(12) 0.041(6) 0.070(10) -0.012(6) 0.034(6) 0.015(6) 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 O7 2.005(6) . ? Pd1 O9 2.009(6) . ? Pd1 N1 2.018(7) . ? Pd1 N2 2.031(7) . ? O1 C3 1.353(10) . ? O1 C2 1.403(10) . ? O2 C2 1.172(10) . ? O3 C7 1.346(11) . ? O3 C10 1.460(12) . ? O4 C19 1.358(10) . ? O4 C18 1.384(10) . ? O5 C18 1.176(10) . ? O6 C23 1.349(10) . ? O6 C26 1.433(10) . ? O7 C33 1.277(11) . ? O8 C33 1.215(12) . ? O9 C35 1.262(11) . ? O10 C35 1.214(11) . ? N1 C3 1.311(10) . ? N1 C1 1.477(10) . ? N2 C19 1.309(10) . ? N2 C17 1.481(10) . ? C1 C11 1.545(11) . ? C1 C2 1.547(11) . ? C1 C17 1.584(10) . ? C3 C4 1.441(11) . ? C4 C9 1.397(12) . ? C4 C5 1.417(12) . ? C5 C6 1.365(13) . ? C6 C7 1.406(13) . ? C7 C8 1.401(13) . ? C8 C9 1.392(13) . ? C11 C16 1.385(12) . ? C11 C12 1.387(12) . ? C12 C13 1.380(12) . ? C13 C14 1.391(12) . ? C14 C15 1.368(14) . ? C15 C16 1.403(12) . ? C17 C18 1.544(11) . ? C17 C27 1.545(11) . ? C19 C20 1.446(11) . ? C20 C21 1.379(11) . ? C20 C25 1.416(12) . ? C21 C22 1.380(12) . ? C22 C23 1.413(11) . ? C23 C24 1.389(12) . ? C24 C25 1.370(11) . ? C27 C32 1.390(12) . ? C27 C28 1.407(12) . ? C28 C29 1.363(13) . ? C29 C30 1.370(15) . ? C30 C31 1.407(13) . ? C31 C32 1.412(11) . ? C33 C34 1.604(12) . ? C34 F3' 1.20(2) . ? C34 F2 1.3100 . ? C34 F1 1.3100 . ? C34 F3 1.3101 . ? C34 F2' 1.36(2) . ? C34 F1' 1.40(2) . ? F1 F3' 0.66(2) . ? F3 F1' 0.73(2) . ? F3 F3' 1.609(19) . ? C35 C36 1.596(11) . ? C36 F6' 1.128(15) . ? C36 F5 1.3098 . ? C36 F4 1.3100 . ? C36 F6 1.3100 . ? C36 F5' 1.379(19) . ? C36 F4' 1.491(16) . ? F4 F6' 0.960(18) . ? F5 F4' 1.101(19) . ? F5 F6' 1.300(17) . ? F6 F5' 0.51(3) . ? F6 F4' 1.71(2) . ? 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 O7 Pd1 O9 87.2(2) . . ? O7 Pd1 N1 96.7(3) . . ? O9 Pd1 N1 175.4(3) . . ? O7 Pd1 N2 175.8(3) . . ? O9 Pd1 N2 96.7(3) . . ? N1 Pd1 N2 79.4(3) . . ? C3 O1 C2 109.6(6) . . ? C7 O3 C10 117.8(8) . . ? C19 O4 C18 109.6(6) . . ? C23 O6 C26 117.1(7) . . ? C33 O7 Pd1 114.7(5) . . ? C35 O9 Pd1 115.0(5) . . ? C3 N1 C1 108.4(6) . . ? C3 N1 Pd1 132.0(6) . . ? C1 N1 Pd1 114.6(5) . . ? C19 N2 C17 108.0(7) . . ? C19 N2 Pd1 132.3(5) . . ? C17 N2 Pd1 113.8(5) . . ? N1 C1 C11 114.5(6) . . ? N1 C1 C2 102.9(6) . . ? C11 C1 C2 111.9(6) . . ? N1 C1 C17 102.6(6) . . ? C11 C1 C17 111.7(6) . . ? C2 C1 C17 112.5(6) . . ? O2 C2 O1 123.2(8) . . ? O2 C2 C1 132.0(8) . . ? O1 C2 C1 104.8(6) . . ? N1 C3 O1 114.2(7) . . ? N1 C3 C4 129.8(8) . . ? O1 C3 C4 116.0(7) . . ? C9 C4 C5 119.7(8) . . ? C9 C4 C3 122.8(8) . . ? C5 C4 C3 117.6(8) . . ? C6 C5 C4 119.9(8) . . ? C5 C6 C7 120.4(9) . . ? O3 C7 C8 125.0(8) . . ? O3 C7 C6 114.8(8) . . ? C8 C7 C6 120.2(8) . . ? C9 C8 C7 119.2(8) . . ? C8 C9 C4 120.4(8) . . ? C16 C11 C12 121.3(8) . . ? C16 C11 C1 120.2(8) . . ? C12 C11 C1 118.4(8) . . ? C13 C12 C11 119.6(8) . . ? C12 C13 C14 119.8(8) . . ? C15 C14 C13 120.3(8) . . ? C14 C15 C16 120.9(8) . . ? C11 C16 C15 118.1(8) . . ? N2 C17 C18 102.5(6) . . ? N2 C17 C27 113.1(6) . . ? C18 C17 C27 111.0(7) . . ? N2 C17 C1 103.1(6) . . ? C18 C17 C1 113.9(6) . . ? C27 C17 C1 112.5(7) . . ? O5 C18 O4 122.6(8) . . ? O5 C18 C17 132.0(8) . . ? O4 C18 C17 105.4(6) . . ? N2 C19 O4 114.2(7) . . ? N2 C19 C20 129.4(7) . . ? O4 C19 C20 116.3(7) . . ? C21 C20 C25 120.3(7) . . ? C21 C20 C19 118.2(8) . . ? C25 C20 C19 121.5(7) . . ? C20 C21 C22 120.2(8) . . ? C21 C22 C23 119.7(8) . . ? O6 C23 C24 125.6(7) . . ? O6 C23 C22 114.7(7) . . ? C24 C23 C22 119.7(7) . . ? C25 C24 C23 120.6(8) . . ? C24 C25 C20 119.5(8) . . ? C32 C27 C28 119.8(8) . . ? C32 C27 C17 120.3(7) . . ? C28 C27 C17 119.8(8) . . ? C29 C28 C27 119.6(9) . . ? C28 C29 C30 122.3(9) . . ? C29 C30 C31 119.1(9) . . ? C30 C31 C32 119.6(9) . . ? C27 C32 C31 119.5(8) . . ? O8 C33 O7 131.0(9) . . ? O8 C33 C34 119.4(8) . . ? O7 C33 C34 109.4(7) . . ? F3' C34 F2 125.7(15) . . ? F3' C34 F1 30.2(10) . . ? F2 C34 F1 109.4 . . ? F3' C34 F3 79.6(10) . . ? F2 C34 F3 109.4 . . ? F1 C34 F3 109.4 . . ? F3' C34 F2' 112.8(18) . . ? F2 C34 F2' 14.1(17) . . ? F1 C34 F2' 95.3(17) . . ? F3 C34 F2' 115(2) . . ? F3' C34 F1' 110.4(13) . . ? F2 C34 F1' 90.3(15) . . ? F1 C34 F1' 140.1(10) . . ? F3 C34 F1' 30.9(10) . . ? F2' C34 F1' 101.4(15) . . ? F3' C34 C33 117.2(13) . . ? F2 C34 C33 106.5(11) . . ? F1 C34 C33 105.9(8) . . ? F3 C34 C33 115.9(9) . . ? F2' C34 C33 112.3(17) . . ? F1' C34 C33 100.8(13) . . ? F3' F1 C34 65.7(17) . . ? F1' F3 C34 81(2) . . ? F1' F3 F3' 129(2) . . ? C34 F3 F3' 47.2(7) . . ? O10 C35 O9 131.7(9) . . ? O10 C35 C36 119.1(8) . . ? O9 C35 C36 109.1(7) . . ? F6' C36 F5 63.9(9) . . ? F6' C36 F4 45.6(9) . . ? F5 C36 F4 109.4 . . ? F6' C36 F6 127.9(12) . . ? F5 C36 F6 109.4 . . ? F4 C36 F6 109.4 . . ? F6' C36 F5' 116.7(15) . . ? F5 C36 F5' 124.2(17) . . ? F4 C36 F5' 88.7(12) . . ? F6 C36 F5' 21.6(12) . . ? F6' C36 F4' 108.7(10) . . ? F5 C36 F4' 45.7(9) . . ? F4 C36 F4' 151.7(8) . . ? F6 C36 F4' 75.2(10) . . ? F5' C36 F4' 96.3(11) . . ? F6' C36 C35 121.7(12) . . ? F5 C36 C35 113.9(8) . . ? F4 C36 C35 106.2(8) . . ? F6 C36 C35 108.3(10) . . ? F5' C36 C35 110.1(12) . . ? F4' C36 C35 98.2(8) . . ? F6' F4 C36 57.1(9) . . ? F4' F5 F6' 125.7(14) . . ? F4' F5 C36 75.8(11) . . ? F6' F5 C36 51.2(7) . . ? F5' F6 C36 87(2) . . ? F5' F6 F4' 142(2) . . ? C36 F6 F4' 57.2(7) . . ? F3 F1' C34 67.7(15) . . ? F1 F3' C34 84.1(19) . . ? F1 F3' F3 137(2) . . ? C34 F3' F3 53.2(7) . . ? F5 F4' C36 58.4(7) . . ? F5 F4' F6 96.4(12) . . ? C36 F4' F6 47.6(6) . . ? F6 F5' C36 71(2) . . ? F4 F6' C36 77.2(11) . . ? F4 F6' F5 141.8(15) . . ? C36 F6' F5 64.8(8) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.73 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.856 _refine_diff_density_min -5.121 _refine_diff_density_rms 0.211