#------------------------------------------------------------------------------ #$Date: 2008-02-24 21:54:22 +0200 (Sun, 24 Feb 2008) $ #$Revision: 172 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100983.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100983 _chemical_formula_moiety '3[C42 H48 F6 N2 O2 Pd]2+,6 (B F4)-,2 HBF4,4 CH2Cl' _chemical_formula_sum 'C43.33 H51.33 B2.67 Cl2.67 F16.67 N2 O2 Pd' _chemical_formula_weight 1178.62 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' 'Cl' 'Cl' 0.1484 0.1585 '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 , No. 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5833(5) _cell_length_b 16.8101(7) _cell_length_c 18.3743(7) _cell_angle_alpha 78.548(5) _cell_angle_beta 72.946(5) _cell_angle_gamma 78.209(5) _cell_volume 3883.1(3) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent' _exptl_crystal_colour 'deep green' _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type 'Gaussian, face-indexed' _exptl_absorpt_correction_T_min 0.7185 _exptl_absorpt_correction_T_max 0.9065 _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '851 images at 0.5 deg. in \w and 726 images at 0.5 deg. in phi, 15 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54535 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.50 _reflns_number_total 17684 _reflns_number_gt 15319 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+12.9878P] 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 17684 _refine_ls_number_parameters 1012 _refine_ls_number_restraints 415 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1331 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 1.06196(2) 1.085760(15) 1.167811(15) 0.01853(7) Uani 1 d . . . O1 O 0.92583(19) 1.04982(15) 1.17797(15) 0.0229(5) Uani 1 d . . . C1 C 0.9212(3) 0.9758(2) 1.2069(2) 0.0196(7) Uani 1 d . . . C2 C 0.8275(3) 0.9400(2) 1.2250(2) 0.0235(7) Uani 1 d . . . C3 C 0.8386(3) 0.8575(2) 1.2470(2) 0.0237(7) Uani 1 d . . . H3 H 0.7798 0.8316 1.2543 0.028 Uiso 1 calc R . . C4 C 0.9343(3) 0.8048(2) 1.2604(2) 0.0241(7) Uani 1 d . . . C5 C 1.0217(3) 0.8380(2) 1.2483(2) 0.0233(7) Uani 1 d . . . H5 H 1.0833 0.8047 1.2580 0.028 Uiso 1 calc R . . C6 C 1.0200(3) 0.9241(2) 1.2206(2) 0.0199(7) Uani 1 d . . . N7 N 1.0969(2) 0.96555(18) 1.20302(17) 0.0205(6) Uani 1 d . . . C8 C 1.1977(3) 0.9300(2) 1.2150(2) 0.0247(7) Uani 1 d . . . C9 C 1.2837(3) 0.9171(2) 1.1523(3) 0.0315(9) Uani 1 d . . . C10 C 1.3813(3) 0.8883(3) 1.1653(3) 0.0451(12) Uani 1 d . . . H10 H 1.4405 0.8788 1.1232 0.054 Uiso 1 calc R . . C11 C 1.3926(4) 0.8736(3) 1.2394(4) 0.0486(14) Uani 1 d . . . H11 H 1.4596 0.8539 1.2480 0.058 Uiso 1 calc R . . C12 C 1.3073(4) 0.8874(3) 1.3005(3) 0.0445(12) Uani 1 d . . . H12 H 1.3160 0.8773 1.3512 0.053 Uiso 1 calc R . . C13 C 1.2081(3) 0.9160(2) 1.2895(2) 0.0301(8) Uani 1 d . . . H13 H 1.1493 0.9256 1.3318 0.036 Uiso 1 calc R . . C14 C 0.7252(3) 0.9943(2) 1.2173(3) 0.0305(8) Uani 1 d . . . C15 C 0.7333(4) 1.0292(3) 1.1326(3) 0.0396(10) Uani 1 d . . . H15A H 0.7899 1.0621 1.1130 0.059 Uiso 1 calc R . . H15B H 0.6674 1.0638 1.1279 0.059 Uiso 1 calc R . . H15C H 0.7478 0.9839 1.1027 0.059 Uiso 1 calc R . . C16 C 0.7009(3) 1.0647(3) 1.2661(3) 0.0393(10) Uani 1 d . . . H16A H 0.7028 1.0415 1.3191 0.059 Uiso 1 calc R . . H16B H 0.6315 1.0957 1.2660 0.059 Uiso 1 calc R . . H16C H 0.7531 1.1015 1.2441 0.059 Uiso 1 calc R . . C17 C 0.6343(3) 0.9449(3) 1.2473(3) 0.0425(11) Uani 1 d . . . H17A H 0.6296 0.9206 1.3011 0.064 Uiso 1 calc R . . H17B H 0.6463 0.9011 1.2162 0.064 Uiso 1 calc R . . H17C H 0.5691 0.9814 1.2439 0.064 Uiso 1 calc R . . C18 C 0.9261(3) 0.7148(2) 1.2898(2) 0.0285(8) Uani 1 d . . . C19 C 0.8313(3) 0.7087(3) 1.3614(2) 0.0338(9) Uani 1 d . . . H19A H 0.8307 0.6510 1.3850 0.051 Uiso 1 calc R . . H19B H 0.7667 0.7303 1.3458 0.051 Uiso 1 calc R . . H19C H 0.8367 0.7408 1.3988 0.051 Uiso 1 calc R . . C20 C 0.9098(4) 0.6755(3) 1.2261(3) 0.0368(10) Uani 1 d . . . H20A H 0.8951 0.6195 1.2468 0.055 Uiso 1 calc R . . H20B H 0.9730 0.6737 1.1832 0.055 Uiso 1 calc R . . H20C H 0.8509 0.7082 1.2077 0.055 Uiso 1 calc R . . C21 C 1.0240(4) 0.6678(3) 1.3135(3) 0.0437(11) Uani 1 d . . . H21A H 1.0151 0.6103 1.3331 0.066 Uiso 1 calc R . . H21B H 1.0347 0.6929 1.3538 0.066 Uiso 1 calc R . . H21C H 1.0847 0.6700 1.2687 0.066 Uiso 1 calc R . . C22 C 1.2719(3) 0.9325(3) 1.0716(3) 0.0406(10) Uani 1 d . . . F23 F 1.2587(3) 1.01234(19) 1.04464(17) 0.0573(8) Uani 1 d . . . F24 F 1.1904(2) 0.9043(2) 1.06682(17) 0.0554(8) Uani 1 d . . . F25 F 1.3543(3) 0.8962(3) 1.0238(2) 0.0799(12) Uani 1 d . . . O31 O 1.19628(18) 1.12013(15) 1.16290(14) 0.0213(5) Uani 1 d . . . C31 C 1.1965(3) 1.1958(2) 1.1481(2) 0.0204(7) Uani 1 d . . . C32 C 1.2838(3) 1.2332(2) 1.1476(2) 0.0230(7) Uani 1 d . . . C33 C 1.2718(3) 1.3159(2) 1.1289(2) 0.0261(8) Uani 1 d . . . H33 H 1.3270 1.3422 1.1296 0.031 Uiso 1 calc R . . C34 C 1.1811(3) 1.3688(2) 1.1073(2) 0.0261(8) Uani 1 d . . . C35 C 1.0972(3) 1.3362(2) 1.1107(2) 0.0260(8) Uani 1 d . . . H35 H 1.0368 1.3705 1.0998 0.031 Uiso 1 calc R . . C36 C 1.0997(3) 1.2490(2) 1.1311(2) 0.0206(7) Uani 1 d . . . N37 N 1.0274(2) 1.20696(18) 1.13513(17) 0.0212(6) Uani 1 d . . . C38 C 0.9250(3) 1.2456(2) 1.1287(2) 0.0230(7) Uani 1 d . . . C39 C 0.8915(3) 1.2424(2) 1.0643(2) 0.0262(8) Uani 1 d . . . C40 C 0.7891(3) 1.2760(3) 1.0632(3) 0.0325(9) Uani 1 d . . . H40 H 0.7654 1.2744 1.0198 0.039 Uiso 1 calc R . . C41 C 0.7219(3) 1.3115(3) 1.1247(3) 0.0341(9) Uani 1 d . . . H41 H 0.6519 1.3332 1.1237 0.041 Uiso 1 calc R . . C42 C 0.7559(3) 1.3157(2) 1.1878(3) 0.0338(9) Uani 1 d . . . H42 H 0.7099 1.3417 1.2292 0.041 Uiso 1 calc R . . C43 C 0.8576(3) 1.2817(2) 1.1904(2) 0.0293(8) Uani 1 d . . . H43 H 0.8806 1.2832 1.2341 0.035 Uiso 1 calc R . . C44 C 1.3819(3) 1.1780(2) 1.1646(2) 0.0281(8) Uani 1 d . . . C45 C 1.3541(3) 1.1248(3) 1.2444(3) 0.0358(9) Uani 1 d . . . H45A H 1.3052 1.0890 1.2448 0.054 Uiso 1 calc R . . H45B H 1.3218 1.1605 1.2839 0.054 Uiso 1 calc R . . H45C H 1.4177 1.0910 1.2551 0.054 Uiso 1 calc R . . C46 C 1.4615(4) 1.2306(3) 1.1647(3) 0.0440(12) Uani 1 d . . . H46A H 1.5215 1.1950 1.1795 0.066 Uiso 1 calc R . . H46B H 1.4291 1.2693 1.2017 0.066 Uiso 1 calc R . . H46C H 1.4849 1.2613 1.1132 0.066 Uiso 1 calc R . . C47 C 1.4293(3) 1.1232(3) 1.1020(3) 0.0379(10) Uani 1 d . . . H47A H 1.3788 1.0891 1.1022 0.057 Uiso 1 calc R . . H47B H 1.4924 1.0879 1.1118 0.057 Uiso 1 calc R . . H47C H 1.4472 1.1576 1.0517 0.057 Uiso 1 calc R . . C48 C 1.1888(4) 1.4602(2) 1.0804(3) 0.0375(10) Uani 1 d . . . C49 C 1.0930(4) 1.5069(3) 1.0561(4) 0.0569(16) Uani 1 d . . . H49A H 1.0835 1.4825 1.0150 0.085 Uiso 1 calc R . . H49B H 1.1019 1.5645 1.0374 0.085 Uiso 1 calc R . . H49C H 1.0316 1.5041 1.1003 0.085 Uiso 1 calc R . . C50 C 1.2844(5) 1.4670(3) 1.0096(3) 0.0561(14) Uani 1 d . . . H50A H 1.2764 1.4402 0.9694 0.084 Uiso 1 calc R . . H50B H 1.3480 1.4400 1.0249 0.084 Uiso 1 calc R . . H50C H 1.2893 1.5250 0.9899 0.084 Uiso 1 calc R . . C51 C 1.2018(5) 1.4983(3) 1.1457(3) 0.0505(13) Uani 1 d . . . H51A H 1.2030 1.5573 1.1293 0.076 Uiso 1 calc R . . H51B H 1.2673 1.4720 1.1583 0.076 Uiso 1 calc R . . H51C H 1.1433 1.4899 1.1913 0.076 Uiso 1 calc R . . C52 C 0.9659(3) 1.2084(3) 0.9961(2) 0.0360(10) Uani 1 d . . . F53 F 0.9239(2) 1.21614(19) 0.93729(15) 0.0451(7) Uani 1 d . . . F54 F 1.0492(2) 1.2467(2) 0.96900(16) 0.0573(9) Uani 1 d . . . F55 F 1.0015(3) 1.1278(2) 1.01189(17) 0.0598(9) Uani 1 d . . . Pd2 Pd 0.5000 1.5000 1.5000 0.01793(9) Uani 1 d S . . O61 O 0.48923(18) 1.61540(14) 1.51979(15) 0.0208(5) Uani 1 d . . . C61 C 0.5692(3) 1.6301(2) 1.5317(2) 0.0191(7) Uani 1 d . . . C62 C 0.5794(3) 1.7093(2) 1.5466(2) 0.0204(7) Uani 1 d . . . C63 C 0.6683(3) 1.7112(2) 1.5647(2) 0.0219(7) Uani 1 d . . . H63 H 0.6763 1.7620 1.5758 0.026 Uiso 1 calc R . . C64 C 0.7540(3) 1.6422(2) 1.5689(2) 0.0199(7) Uani 1 d . . . C65 C 0.7488(3) 1.5692(2) 1.5514(2) 0.0209(7) Uani 1 d . . . H65 H 0.8046 1.5248 1.5520 0.025 Uiso 1 calc R . . C66 C 0.6584(3) 1.5600(2) 1.5318(2) 0.0196(7) Uani 1 d . . . N67 N 0.6406(2) 1.49318(17) 1.51538(17) 0.0191(6) Uani 1 d . . . C68 C 0.7091(3) 1.4167(2) 1.5223(2) 0.0196(7) Uani 1 d . . . C69 C 0.7704(3) 1.3819(2) 1.4570(2) 0.0211(7) Uani 1 d . . . C70 C 0.8272(3) 1.3037(2) 1.4670(2) 0.0249(7) Uani 1 d . . . H70 H 0.8681 1.2789 1.4233 0.030 Uiso 1 calc R . . C71 C 0.8242(3) 1.2617(2) 1.5404(3) 0.0294(8) Uani 1 d . . . H71 H 0.8632 1.2082 1.5468 0.035 Uiso 1 calc R . . C72 C 0.7648(3) 1.2971(2) 1.6044(2) 0.0288(8) Uani 1 d . . . H72 H 0.7636 1.2681 1.6546 0.035 Uiso 1 calc R . . C73 C 0.7069(3) 1.3753(2) 1.5955(2) 0.0237(7) Uani 1 d . . . H73 H 0.6663 1.3999 1.6393 0.028 Uiso 1 calc R . . C74 C 0.4920(3) 1.7822(2) 1.5424(2) 0.0275(8) Uani 1 d . . . C75 C 0.4683(4) 1.7974(3) 1.4635(3) 0.0398(10) Uani 1 d . . . H75A H 0.4168 1.8472 1.4599 0.060 Uiso 1 calc R . . H75B H 0.4403 1.7503 1.4577 0.060 Uiso 1 calc R . . H75C H 0.5325 1.8042 1.4227 0.060 Uiso 1 calc R . . C76 C 0.3940(3) 1.7647(3) 1.6070(3) 0.0349(9) Uani 1 d . . . H76A H 0.3371 1.8104 1.6033 0.052 Uiso 1 calc R . . H76B H 0.4089 1.7586 1.6570 0.052 Uiso 1 calc R . . H76C H 0.3736 1.7139 1.6018 0.052 Uiso 1 calc R . . C77 C 0.5241(3) 1.8607(2) 1.5528(3) 0.0388(10) Uani 1 d . . . H77A H 0.4681 1.9070 1.5487 0.058 Uiso 1 calc R . . H77B H 0.5878 1.8718 1.5129 0.058 Uiso 1 calc R . . H77C H 0.5371 1.8534 1.6037 0.058 Uiso 1 calc R . . C78 C 0.8430(3) 1.6559(2) 1.5969(2) 0.0241(7) Uani 1 d . . . C79 C 0.7977(4) 1.6673(4) 1.6819(3) 0.0485(13) Uani 1 d . . . H79A H 0.8534 1.6739 1.7030 0.073 Uiso 1 calc R . . H79B H 0.7665 1.6189 1.7109 0.073 Uiso 1 calc R . . H79C H 0.7441 1.7163 1.6860 0.073 Uiso 1 calc R . . C80 C 0.8888(3) 1.7325(3) 1.5510(3) 0.0369(10) Uani 1 d . . . H80A H 0.9222 1.7236 1.4976 0.055 Uiso 1 calc R . . H80B H 0.9407 1.7431 1.5739 0.055 Uiso 1 calc R . . H80C H 0.8330 1.7799 1.5520 0.055 Uiso 1 calc R . . C81 C 0.9298(4) 1.5825(3) 1.5915(4) 0.0492(14) Uani 1 d . . . H81A H 0.9847 1.5928 1.6115 0.074 Uiso 1 calc R . . H81B H 0.9588 1.5741 1.5376 0.074 Uiso 1 calc R . . H81C H 0.9017 1.5334 1.6219 0.074 Uiso 1 calc R . . C82 C 0.7774(3) 1.4294(2) 1.3777(2) 0.0262(8) Uani 1 d . . . F83 F 0.68712(18) 1.44366(15) 1.35835(14) 0.0343(5) Uani 1 d . . . F84 F 0.8053(2) 1.50333(14) 1.37132(14) 0.0350(5) Uani 1 d . . . F85 F 0.8487(2) 1.39101(16) 1.32352(14) 0.0376(6) Uani 1 d . . . B100 B 0.5241(7) 0.5395(4) 0.7456(4) 0.0396(13) Uani 0.679(9) d PD A 1 F101 F 0.5101(9) 0.6181(5) 0.7622(6) 0.145(6) Uani 0.679(9) d PD A 1 F102 F 0.6223(8) 0.4976(6) 0.7487(7) 0.072(2) Uani 0.679(9) d PD A 1 F103 F 0.5172(4) 0.5426(5) 0.6714(3) 0.0580(16) Uani 0.679(9) d PD A 1 F104 F 0.4456(11) 0.4986(8) 0.7962(5) 0.0554(14) Uani 0.679(9) d PD A 1 B105 B 0.5184(15) 0.5395(8) 0.7565(7) 0.0396(13) Uani 0.321(9) d PD A 2 F106 F 0.528(2) 0.5898(12) 0.8042(9) 0.145(6) Uani 0.321(9) d PD A 2 F107 F 0.609(2) 0.4830(12) 0.7397(17) 0.072(2) Uani 0.321(9) d PD A 2 F108 F 0.5035(10) 0.5859(10) 0.6884(7) 0.0580(16) Uani 0.321(9) d PD A 2 F109 F 0.433(2) 0.4992(16) 0.7929(11) 0.0554(14) Uani 0.321(9) d PD A 2 B200 B 1.5838(4) 0.6663(3) 1.2948(3) 0.0438(13) Uani 1 d . . . F201 F 1.6502(3) 0.6124(2) 1.23237(19) 0.0606(8) Uani 1 d D . . H201 H 1.684(5) 0.634(4) 1.1789(16) 0.091 Uiso 1 d D . . F202 F 1.5892(4) 0.6210(2) 1.36330(19) 0.0973(17) Uani 1 d . . . F203 F 1.4853(2) 0.6819(2) 1.2844(3) 0.0780(12) Uani 1 d . . . F204 F 1.6249(2) 0.73656(18) 1.28043(17) 0.0483(7) Uani 1 d . . . F304 F 0.74769(19) 0.79383(16) 1.00083(12) 0.0381(6) Uani 1 d D . . B300 B 0.7041(3) 0.7708(2) 1.07838(19) 0.0352(13) Uani 0.826(4) d PD B 1 F301 F 0.7369(3) 0.8169(2) 1.11902(19) 0.0573(10) Uani 0.826(4) d PD B 1 F302 F 0.5966(2) 0.7842(3) 1.0944(2) 0.0640(12) Uani 0.826(4) d PD B 1 F303 F 0.7383(4) 0.6881(2) 1.1004(2) 0.0504(10) Uani 0.826(4) d PD B 1 B305 B 0.6802(7) 0.7648(6) 1.0691(4) 0.0352(13) Uani 0.174(4) d PD B 2 F306 F 0.6002(9) 0.7382(10) 1.0526(8) 0.0573(10) Uani 0.174(4) d PD B 2 F307 F 0.6389(10) 0.8267(10) 1.1142(6) 0.0640(12) Uani 0.174(4) d PD B 2 F308 F 0.7336(14) 0.6995(10) 1.1085(8) 0.0504(10) Uani 0.174(4) d PD B 2 B400 B 0.9958(4) 1.1357(3) 1.3475(3) 0.0336(10) Uani 1 d . . . F401 F 1.0861(3) 1.0803(2) 1.33052(18) 0.0650(9) Uani 1 d . . . F402 F 0.9190(3) 1.1160(2) 1.32219(19) 0.0655(9) Uani 1 d . . . F403 F 1.0167(2) 1.21288(18) 1.30838(16) 0.0485(7) Uani 1 d . . . F404 F 0.9635(2) 1.13626(16) 1.42658(15) 0.0398(6) Uani 1 d . . . C500 C 1.5921(3) 1.3320(3) 0.8725(2) 0.0552(14) Uani 1 d D . . H50D H 1.5729 1.3795 0.8352 0.066 Uiso 1 calc R . . H50E H 1.5488 1.2896 0.8770 0.066 Uiso 1 calc R . . Cl51 Cl 1.72595(11) 1.29155(10) 0.83999(13) 0.0762(5) Uani 1 d D . . Cl52 Cl 1.56943(14) 1.36313(17) 0.96307(11) 0.0962(7) Uani 1 d D . . C600 C 0.8649(3) 0.9732(5) 1.4883(3) 0.0389(13) Uani 0.800(4) d PD C 1 H60A H 0.9026 0.9482 1.5279 0.047 Uiso 0.800(4) calc PR C 1 H60B H 0.8817 1.0294 1.4685 0.047 Uiso 0.800(4) calc PR C 1 Cl61 Cl 0.9063(2) 0.91403(10) 1.41212(10) 0.0626(6) Uani 0.800(4) d PD C 1 Cl62 Cl 0.7293(2) 0.9784(2) 1.5301(2) 0.0813(8) Uani 0.800(4) d PD C 1 C605 C 0.8310(13) 0.975(2) 1.4900(14) 0.0389(13) Uani 0.200(4) d PD C 2 H60C H 0.8851 0.9452 1.5159 0.047 Uiso 0.200(4) calc PR C 2 H60D H 0.8491 1.0305 1.4665 0.047 Uiso 0.200(4) calc PR C 2 Cl66 Cl 0.8259(9) 0.9215(4) 1.4180(4) 0.0626(6) Uani 0.200(4) d PD C 2 Cl67 Cl 0.7078(11) 0.9846(11) 1.5577(8) 0.0813(8) Uani 0.200(4) d PD C 2 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 0.01603(13) 0.01483(12) 0.02404(14) 0.00104(9) -0.00746(10) -0.00148(9) O1 0.0181(12) 0.0191(12) 0.0326(14) -0.0007(10) -0.0114(10) -0.0012(9) C1 0.0225(17) 0.0177(16) 0.0200(16) -0.0027(13) -0.0087(13) -0.0015(13) C2 0.0216(17) 0.0245(18) 0.0264(18) -0.0052(14) -0.0081(14) -0.0038(14) C3 0.0238(17) 0.0245(18) 0.0235(17) -0.0024(14) -0.0051(14) -0.0083(14) C4 0.0302(19) 0.0213(17) 0.0207(17) -0.0014(13) -0.0065(14) -0.0060(14) C5 0.0264(18) 0.0180(16) 0.0258(18) -0.0012(13) -0.0102(14) -0.0007(14) C6 0.0195(16) 0.0192(16) 0.0202(16) -0.0032(13) -0.0055(13) -0.0006(13) N7 0.0194(14) 0.0183(14) 0.0229(14) -0.0016(11) -0.0070(11) -0.0001(11) C8 0.0197(17) 0.0149(16) 0.040(2) -0.0005(14) -0.0122(15) 0.0002(13) C9 0.0212(18) 0.0245(19) 0.046(2) -0.0072(17) -0.0065(17) 0.0001(15) C10 0.021(2) 0.028(2) 0.082(4) -0.007(2) -0.009(2) 0.0002(16) C11 0.029(2) 0.023(2) 0.098(4) 0.008(2) -0.036(3) -0.0032(17) C12 0.049(3) 0.026(2) 0.069(3) 0.012(2) -0.042(3) -0.0091(19) C13 0.031(2) 0.0223(18) 0.038(2) 0.0055(16) -0.0173(17) -0.0048(15) C14 0.0194(18) 0.0253(19) 0.048(2) -0.0068(17) -0.0110(17) -0.0024(15) C15 0.033(2) 0.037(2) 0.054(3) 0.002(2) -0.028(2) -0.0034(18) C16 0.023(2) 0.033(2) 0.062(3) -0.016(2) -0.0100(19) 0.0015(17) C17 0.023(2) 0.033(2) 0.072(3) -0.009(2) -0.016(2) -0.0025(17) C18 0.036(2) 0.0194(17) 0.033(2) 0.0015(15) -0.0141(17) -0.0066(15) C19 0.040(2) 0.031(2) 0.031(2) 0.0026(16) -0.0109(18) -0.0137(18) C20 0.056(3) 0.0239(19) 0.034(2) -0.0030(16) -0.012(2) -0.0129(19) C21 0.044(3) 0.024(2) 0.063(3) 0.011(2) -0.024(2) -0.0046(18) C22 0.029(2) 0.040(2) 0.045(3) -0.016(2) 0.0037(19) -0.0004(18) F23 0.088(2) 0.0439(17) 0.0409(16) -0.0013(13) -0.0181(16) -0.0154(16) F24 0.0556(18) 0.077(2) 0.0413(16) -0.0204(15) -0.0076(14) -0.0237(16) F25 0.055(2) 0.102(3) 0.057(2) -0.030(2) 0.0141(16) 0.021(2) O31 0.0168(11) 0.0200(12) 0.0260(13) 0.0014(10) -0.0078(10) -0.0022(9) C31 0.0197(16) 0.0215(17) 0.0186(16) -0.0002(13) -0.0061(13) -0.0010(13) C32 0.0192(16) 0.0244(18) 0.0255(18) -0.0007(14) -0.0079(14) -0.0033(14) C33 0.0256(18) 0.0244(18) 0.0300(19) 0.0025(15) -0.0106(15) -0.0093(15) C34 0.031(2) 0.0175(17) 0.0312(19) 0.0011(14) -0.0144(16) -0.0034(14) C35 0.0281(19) 0.0185(17) 0.032(2) 0.0012(14) -0.0146(16) -0.0004(14) C36 0.0216(17) 0.0196(16) 0.0208(16) -0.0012(13) -0.0082(13) -0.0012(13) N37 0.0208(14) 0.0179(14) 0.0242(15) 0.0014(11) -0.0092(12) -0.0009(11) C38 0.0187(16) 0.0158(16) 0.035(2) 0.0027(14) -0.0115(14) -0.0029(13) C39 0.0252(18) 0.0225(17) 0.0313(19) 0.0052(15) -0.0115(15) -0.0076(14) C40 0.030(2) 0.030(2) 0.039(2) 0.0102(17) -0.0180(18) -0.0102(16) C41 0.0212(18) 0.029(2) 0.050(3) 0.0069(18) -0.0146(18) -0.0040(15) C42 0.026(2) 0.0242(19) 0.047(2) -0.0021(17) -0.0091(18) 0.0018(15) C43 0.0277(19) 0.0242(18) 0.037(2) -0.0045(16) -0.0139(17) 0.0018(15) C44 0.0197(17) 0.0288(19) 0.037(2) 0.0008(16) -0.0128(16) -0.0044(15) C45 0.035(2) 0.033(2) 0.042(2) 0.0043(18) -0.0228(19) -0.0012(17) C46 0.029(2) 0.043(3) 0.066(3) 0.007(2) -0.028(2) -0.0115(19) C47 0.0208(19) 0.041(2) 0.048(3) -0.008(2) -0.0074(18) 0.0028(17) C48 0.045(2) 0.0182(18) 0.058(3) 0.0038(18) -0.029(2) -0.0097(17) C49 0.059(3) 0.020(2) 0.103(5) 0.012(2) -0.051(3) -0.009(2) C50 0.066(4) 0.036(3) 0.062(3) 0.015(2) -0.015(3) -0.022(2) C51 0.065(3) 0.027(2) 0.072(4) -0.006(2) -0.035(3) -0.012(2) C52 0.030(2) 0.050(3) 0.029(2) 0.0013(18) -0.0150(17) -0.0054(19) F53 0.0425(15) 0.0694(19) 0.0314(13) -0.0043(13) -0.0207(12) -0.0134(13) F54 0.0334(14) 0.109(3) 0.0340(14) -0.0055(16) -0.0071(12) -0.0281(16) F55 0.077(2) 0.0562(19) 0.0358(15) -0.0124(13) -0.0167(15) 0.0220(16) Pd2 0.01308(17) 0.01388(17) 0.0284(2) -0.00372(14) -0.00875(14) -0.00014(12) O61 0.0168(11) 0.0159(11) 0.0311(13) -0.0036(10) -0.0095(10) -0.0008(9) C61 0.0159(15) 0.0165(15) 0.0232(16) -0.0005(13) -0.0059(13) -0.0004(12) C62 0.0176(16) 0.0162(15) 0.0262(17) -0.0041(13) -0.0051(13) -0.0002(12) C63 0.0206(17) 0.0182(16) 0.0275(18) -0.0033(13) -0.0064(14) -0.0045(13) C64 0.0172(16) 0.0222(17) 0.0204(16) -0.0019(13) -0.0047(13) -0.0051(13) C65 0.0139(15) 0.0191(16) 0.0291(18) -0.0022(14) -0.0064(13) -0.0015(12) C66 0.0163(15) 0.0165(15) 0.0244(17) -0.0003(13) -0.0060(13) -0.0006(12) N67 0.0142(13) 0.0158(13) 0.0275(15) -0.0032(11) -0.0071(11) -0.0002(10) C68 0.0144(15) 0.0132(15) 0.0326(19) -0.0028(13) -0.0100(13) -0.0003(12) C69 0.0141(15) 0.0175(16) 0.0321(19) -0.0043(14) -0.0066(13) -0.0022(12) C70 0.0164(16) 0.0198(17) 0.037(2) -0.0072(15) -0.0066(15) 0.0014(13) C71 0.0234(18) 0.0178(17) 0.046(2) 0.0000(16) -0.0135(17) 0.0011(14) C72 0.0282(19) 0.0228(18) 0.035(2) 0.0019(15) -0.0139(16) -0.0019(15) C73 0.0184(16) 0.0226(17) 0.0305(19) -0.0030(14) -0.0087(14) -0.0017(13) C74 0.0244(18) 0.0165(16) 0.044(2) -0.0073(15) -0.0148(17) 0.0018(14) C75 0.048(3) 0.0210(19) 0.054(3) -0.0007(18) -0.029(2) 0.0038(18) C76 0.0207(18) 0.031(2) 0.054(3) -0.0174(19) -0.0064(18) 0.0015(16) C77 0.032(2) 0.0191(18) 0.071(3) -0.0143(19) -0.021(2) 0.0019(16) C78 0.0226(17) 0.0229(17) 0.0315(19) -0.0034(14) -0.0134(15) -0.0051(14) C79 0.044(3) 0.079(4) 0.032(2) -0.010(2) -0.015(2) -0.022(3) C80 0.034(2) 0.036(2) 0.050(3) 0.0040(19) -0.022(2) -0.0195(18) C81 0.031(2) 0.033(2) 0.100(4) -0.022(3) -0.042(3) 0.0055(18) C82 0.0224(18) 0.0222(17) 0.034(2) -0.0065(15) -0.0074(15) -0.0015(14) F83 0.0283(12) 0.0397(13) 0.0366(13) 0.0031(10) -0.0167(10) -0.0057(10) F84 0.0418(14) 0.0265(12) 0.0363(13) 0.0004(10) -0.0075(11) -0.0136(10) F85 0.0355(13) 0.0388(14) 0.0312(12) -0.0082(10) -0.0021(10) 0.0037(11) B100 0.037(3) 0.040(3) 0.038(3) -0.004(2) -0.009(3) -0.002(2) F101 0.136(7) 0.078(7) 0.191(11) -0.084(7) 0.078(9) -0.066(6) F102 0.049(4) 0.079(4) 0.093(4) 0.006(3) -0.039(2) -0.009(3) F103 0.056(3) 0.086(5) 0.036(2) 0.007(3) -0.014(2) -0.033(3) F104 0.056(4) 0.063(2) 0.0433(18) -0.0045(15) 0.0004(18) -0.025(2) B105 0.037(3) 0.040(3) 0.038(3) -0.004(2) -0.009(3) -0.002(2) F106 0.136(7) 0.078(7) 0.191(11) -0.084(7) 0.078(9) -0.066(6) F107 0.049(4) 0.079(4) 0.093(4) 0.006(3) -0.039(2) -0.009(3) F108 0.056(3) 0.086(5) 0.036(2) 0.007(3) -0.014(2) -0.033(3) F109 0.056(4) 0.063(2) 0.0433(18) -0.0045(15) 0.0004(18) -0.025(2) B200 0.040(3) 0.032(3) 0.043(3) 0.001(2) 0.007(2) -0.002(2) F201 0.0545(19) 0.060(2) 0.0535(19) -0.0021(15) -0.0039(15) -0.0004(15) F202 0.159(4) 0.0431(19) 0.0380(18) 0.0105(14) 0.017(2) 0.022(2) F203 0.0333(16) 0.057(2) 0.135(4) -0.033(2) 0.0049(19) -0.0112(15) F204 0.0491(16) 0.0470(16) 0.0500(16) 0.0002(13) -0.0140(13) -0.0161(13) F304 0.0341(13) 0.0514(16) 0.0250(12) -0.0008(11) -0.0067(10) -0.0049(11) B300 0.028(3) 0.045(3) 0.028(3) -0.002(2) -0.003(2) -0.007(2) F301 0.075(3) 0.063(2) 0.0390(19) -0.0162(17) -0.0138(18) -0.015(2) F302 0.0239(17) 0.085(3) 0.066(3) 0.002(2) -0.0011(16) 0.0026(17) F303 0.0448(17) 0.047(2) 0.0480(18) 0.0050(15) -0.0009(14) -0.0091(15) B305 0.028(3) 0.045(3) 0.028(3) -0.002(2) -0.003(2) -0.007(2) F306 0.075(3) 0.063(2) 0.0390(19) -0.0162(17) -0.0138(18) -0.015(2) F307 0.0239(17) 0.085(3) 0.066(3) 0.002(2) -0.0011(16) 0.0026(17) F308 0.0448(17) 0.047(2) 0.0480(18) 0.0050(15) -0.0009(14) -0.0091(15) B400 0.036(3) 0.034(2) 0.035(2) -0.0128(19) -0.011(2) -0.004(2) F401 0.063(2) 0.060(2) 0.0496(18) -0.0084(15) -0.0028(15) 0.0233(16) F402 0.070(2) 0.086(3) 0.0567(19) -0.0028(17) -0.0249(17) -0.042(2) F403 0.0655(19) 0.0443(16) 0.0419(15) 0.0027(12) -0.0245(14) -0.0162(14) F404 0.0474(15) 0.0375(14) 0.0344(13) -0.0126(11) -0.0065(11) -0.0057(12) C500 0.041(3) 0.056(3) 0.059(3) 0.000(3) -0.007(2) -0.005(2) Cl51 0.0437(8) 0.0540(8) 0.1278(15) -0.0354(9) -0.0024(8) -0.0088(6) Cl52 0.0582(10) 0.164(2) 0.0588(10) -0.0190(12) -0.0075(8) -0.0104(12) C600 0.028(3) 0.040(3) 0.046(3) -0.005(2) -0.006(3) -0.007(3) Cl61 0.1043(18) 0.0390(8) 0.0384(8) -0.0043(6) -0.0076(10) -0.0150(10) Cl62 0.0368(14) 0.0698(13) 0.128(3) -0.0198(18) -0.0034(13) -0.0085(12) C605 0.028(3) 0.040(3) 0.046(3) -0.005(2) -0.006(3) -0.007(3) Cl66 0.1043(18) 0.0390(8) 0.0384(8) -0.0043(6) -0.0076(10) -0.0150(10) Cl67 0.0368(14) 0.0698(13) 0.128(3) -0.0198(18) -0.0034(13) -0.0085(12)