# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H33 N9 O Pd2, 2(B F4), 2(C H2 Cl2)' _chemical_formula_sum 'C41 H37 B2 Cl4 F8 N9 O Pd2' _chemical_formula_weight 1200.02 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' Pd Pd -0.9988 1.0072 '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' F F 0.0171 0.0103 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4647(16) _cell_length_b 14.1481(19) _cell_length_c 15.650(2) _cell_angle_alpha 111.841(2) _cell_angle_beta 91.505(2) _cell_angle_gamma 108.809(2) _cell_volume 2199.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3620 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 25.08 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7479 _exptl_absorpt_correction_T_max 0.7712 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15527 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 24.71 _reflns_number_total 7459 _reflns_number_gt 5782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ciftab _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. All H-atoms except those of water molecules were introduced into geometrically calculated positions in the final stages of refinement and were refined according to 'riding model'. Hydrogen atoms of the coordinated water molecules were not located, but were included in the formula sum for the calculation of the intensive properties. ; _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^)+(0.0646P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7459 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1200 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.83725(3) 0.77881(3) 0.35432(3) 0.02126(12) Uani 1 1 d . . . N1 N 0.7613(4) 0.7286(3) 0.2191(3) 0.0230(9) Uani 1 1 d . . . C1 C 0.6765(5) 0.7724(4) 0.2093(4) 0.0281(12) Uani 1 1 d . . . H1 H 0.6705 0.8305 0.2625 0.034 Uiso 1 1 calc R . . Pd2 Pd 1.01411(3) 0.66921(3) 0.25718(3) 0.02193(12) Uani 1 1 d . . . N2 N 0.8583(4) 0.6018(3) 0.1530(3) 0.0208(9) Uani 1 1 d . . . C2 C 0.5976(5) 0.7384(4) 0.1273(4) 0.0299(12) Uani 1 1 d . . . H2 H 0.5404 0.7732 0.1237 0.036 Uiso 1 1 calc R . . N3 N 0.9694(4) 0.3727(3) 0.0579(3) 0.0268(10) Uani 1 1 d . . . C3 C 0.6042(5) 0.6531(4) 0.0509(4) 0.0286(12) Uani 1 1 d . . . H3 H 0.5508 0.6280 -0.0065 0.034 Uiso 1 1 calc R . . N4 N 0.7566(4) 0.7774(3) 0.5536(3) 0.0257(10) Uani 1 1 d . . . C4 C 0.6886(4) 0.6031(4) 0.0573(3) 0.0238(11) Uani 1 1 d . . . N5 N 0.9322(4) 0.8434(3) 0.4911(3) 0.0201(9) Uani 1 1 d . . . C5 C 0.7706(4) 0.6445(4) 0.1432(3) 0.0231(11) Uani 1 1 d . . . N6 N 1.2052(4) 0.9563(3) 0.3964(3) 0.0232(9) Uani 1 1 d . . . C6 C 0.6957(5) 0.5122(4) -0.0168(4) 0.0292(12) Uani 1 1 d . . . H6 H 0.6459 0.4858 -0.0761 0.035 Uiso 1 1 calc R . . N7 N 1.1689(4) 0.7083(3) 0.3474(3) 0.0240(9) Uani 1 1 d . . . C7 C 0.7732(5) 0.4618(4) -0.0045(4) 0.0294(12) Uani 1 1 d . . . H7 H 0.7722 0.3964 -0.0530 0.035 Uiso 1 1 calc R . . N8 N 1.0279(4) 0.6464(3) 0.4339(3) 0.0235(9) Uani 1 1 d . . . C8 C 0.8562(4) 0.5077(4) 0.0819(3) 0.0250(11) Uani 1 1 d . . . N9 N 0.7748(4) 0.5280(3) 0.4404(3) 0.0262(10) Uani 1 1 d . . . C9 C 0.9457(4) 0.4676(4) 0.1043(3) 0.0228(11) Uani 1 1 d . . . C10 C 1.0305(4) 0.5286(4) 0.1874(3) 0.0233(11) Uani 1 1 d . . . C11 C 1.1080(5) 0.4707(4) 0.1920(4) 0.0283(12) Uani 1 1 d . . . H11 H 1.1752 0.4923 0.2401 0.034 Uiso 1 1 calc R . . C12 C 1.0655(5) 0.3749(4) 0.1108(4) 0.0303(12) Uani 1 1 d . . . H12 H 1.0998 0.3189 0.0951 0.036 Uiso 1 1 calc R . . C13 C 0.9017(5) 0.2810(4) -0.0290(3) 0.0326(13) Uani 1 1 d . . . H13A H 0.9357 0.2228 -0.0406 0.049 Uiso 1 1 calc R . . H13B H 0.9108 0.3048 -0.0806 0.049 Uiso 1 1 calc R . . H13C H 0.8130 0.2534 -0.0244 0.049 Uiso 1 1 calc R . . C14 C 0.7069(5) 0.7650(4) 0.6258(4) 0.0282(12) Uani 1 1 d . . . H14 H 0.6193 0.7274 0.6165 0.034 Uiso 1 1 calc R . . C15 C 0.7751(5) 0.8039(4) 0.7151(4) 0.0353(13) Uani 1 1 d . . . H15 H 0.7346 0.7936 0.7648 0.042 Uiso 1 1 calc R . . C16 C 0.8999(5) 0.8564(4) 0.7290(4) 0.0304(12) Uani 1 1 d . . . H16 H 0.9481 0.8822 0.7888 0.037 Uiso 1 1 calc R . . C17 C 0.9591(5) 0.8730(4) 0.6551(3) 0.0253(11) Uani 1 1 d . . . C18 C 0.8828(5) 0.8311(4) 0.5668(3) 0.0232(11) Uani 1 1 d . . . C19 C 1.0877(5) 0.9259(4) 0.6626(4) 0.0286(12) Uani 1 1 d . . . H19 H 1.1415 0.9524 0.7201 0.034 Uiso 1 1 calc R . . C20 C 1.1354(4) 0.9394(4) 0.5879(3) 0.0230(11) Uani 1 1 d . . . H20 H 1.2223 0.9768 0.5935 0.028 Uiso 1 1 calc R . . C21 C 1.0568(4) 0.8983(4) 0.5025(3) 0.0238(11) Uani 1 1 d . . . C22 C 1.0929(4) 0.9034(4) 0.4166(3) 0.0223(11) Uani 1 1 d . . . C23 C 1.0047(4) 0.8484(4) 0.3351(3) 0.0227(11) Uani 1 1 d . . . C24 C 1.0671(4) 0.8707(4) 0.2635(3) 0.0239(11) Uani 1 1 d . . . H24 H 1.0314 0.8450 0.1999 0.029 Uiso 1 1 calc R . . C25 C 1.1882(5) 0.9361(4) 0.3036(3) 0.0264(12) Uani 1 1 d . . . H25 H 1.2511 0.9634 0.2716 0.032 Uiso 1 1 calc R . . C26 C 1.3247(4) 1.0217(4) 0.4591(3) 0.0270(12) Uani 1 1 d . . . H26A H 1.3881 1.0481 0.4244 0.040 Uiso 1 1 calc R . . H26B H 1.3503 0.9768 0.4852 0.040 Uiso 1 1 calc R . . H26C H 1.3158 1.0840 0.5100 0.040 Uiso 1 1 calc R . . C27 C 1.2862(5) 0.7475(4) 0.3345(4) 0.0272(12) Uani 1 1 d . . . H27 H 1.2999 0.7576 0.2784 0.033 Uiso 1 1 calc R . . C28 C 1.3893(5) 0.7744(4) 0.3991(4) 0.0313(13) Uani 1 1 d . . . H28 H 1.4714 0.7994 0.3859 0.038 Uiso 1 1 calc R . . C29 C 1.3716(5) 0.7647(4) 0.4813(4) 0.0315(13) Uani 1 1 d . . . H29 H 1.4414 0.7858 0.5273 0.038 Uiso 1 1 calc R . . C30 C 1.2498(5) 0.7233(4) 0.4980(3) 0.0259(11) Uani 1 1 d . . . C31 C 1.1487(5) 0.6924(4) 0.4284(3) 0.0240(11) Uani 1 1 d . . . C32 C 1.2179(5) 0.7092(4) 0.5815(4) 0.0303(13) Uani 1 1 d . . . H32 H 1.2817 0.7318 0.6325 0.036 Uiso 1 1 calc R . . C33 C 1.0975(5) 0.6640(4) 0.5873(3) 0.0280(12) Uani 1 1 d . . . H33 H 1.0759 0.6551 0.6427 0.034 Uiso 1 1 calc R . . C34 C 1.0016(5) 0.6292(4) 0.5101(3) 0.0256(12) Uani 1 1 d . . . C35 C 0.8720(5) 0.5770(4) 0.5156(3) 0.0246(11) Uani 1 1 d . . . C36 C 0.8186(5) 0.5671(4) 0.5918(4) 0.0311(12) Uani 1 1 d . . . H36 H 0.8629 0.5926 0.6529 0.037 Uiso 1 1 calc R . . C37 C 0.6907(5) 0.5142(4) 0.5646(4) 0.0345(13) Uani 1 1 d . . . H37 H 0.6315 0.4980 0.6032 0.041 Uiso 1 1 calc R . . C38 C 0.6661(5) 0.4895(4) 0.4701(4) 0.0331(13) Uani 1 1 d . . . H38 H 0.5859 0.4516 0.4321 0.040 Uiso 1 1 calc R . . C39 C 0.7811(5) 0.5044(4) 0.3418(3) 0.0293(12) Uani 1 1 d . . . H39A H 0.7039 0.4457 0.3034 0.044 Uiso 1 1 calc R . . H39B H 0.8526 0.4818 0.3253 0.044 Uiso 1 1 calc R . . H39C H 0.7910 0.5700 0.3305 0.044 Uiso 1 1 calc R . . F1A F 0.3453(3) 0.3628(3) 0.1527(2) 0.0413(8) Uani 1 1 d . . . B1A B 0.4633(6) 0.4157(5) 0.2077(4) 0.0346(15) Uani 1 1 d . . . F2A F 0.4770(3) 0.3615(3) 0.2620(2) 0.0503(9) Uani 1 1 d . . . B2A B 0.5289(6) -0.0159(5) 0.2628(4) 0.0310(14) Uani 1 1 d . . . F3A F 0.5553(3) 0.4209(3) 0.1525(2) 0.0494(9) Uani 1 1 d . . . F4A F 0.4742(3) 0.5221(3) 0.2645(3) 0.0583(10) Uani 1 1 d . . . F5A F 0.4269(3) -0.1082(3) 0.2071(2) 0.0413(8) Uani 1 1 d . . . F6A F 0.5651(3) -0.0301(3) 0.3416(2) 0.0416(8) Uani 1 1 d . . . F7A F 0.6281(3) -0.0035(3) 0.2134(2) 0.0399(8) Uani 1 1 d . . . F8A F 0.4954(3) 0.0758(2) 0.2902(2) 0.0391(8) Uani 1 1 d . . . Cl1S Cl 0.57047(14) 0.15157(14) 0.00920(11) 0.0505(4) Uani 1 1 d . . . C1S C 0.6080(6) 0.1756(5) 0.1277(4) 0.0462(16) Uani 1 1 d . . . H1S1 H 0.5712 0.2278 0.1671 0.055 Uiso 1 1 calc R . . H1S2 H 0.5715 0.1064 0.1358 0.055 Uiso 1 1 calc R . . Cl2S Cl 0.77164(15) 0.22863(14) 0.16404(10) 0.0503(4) Uani 1 1 d . . . C2S C 0.7449(6) 0.8977(5) 0.0143(4) 0.0482(16) Uani 1 1 d . . . H2S1 H 0.6913 0.8215 -0.0253 0.058 Uiso 1 1 calc R . . H2S2 H 0.7010 0.9262 0.0660 0.058 Uiso 1 1 calc R . . Cl3S Cl 0.7658(2) 0.97567(15) -0.05228(13) 0.0707(6) Uani 1 1 d . . . Cl4S Cl 0.88654(16) 0.89893(15) 0.06113(14) 0.0706(6) Uani 1 1 d . . . O1W O 0.6515(3) 0.7137(3) 0.3814(2) 0.0258(8) 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 0.0165(2) 0.0218(2) 0.0231(2) 0.00559(17) 0.00234(16) 0.00794(16) N1 0.021(2) 0.019(2) 0.026(2) 0.0065(19) 0.0036(18) 0.0072(18) C1 0.024(3) 0.030(3) 0.034(3) 0.012(2) 0.005(2) 0.014(2) Pd2 0.0191(2) 0.0231(2) 0.0224(2) 0.00628(17) 0.00251(16) 0.00953(17) N2 0.019(2) 0.024(2) 0.019(2) 0.0079(18) 0.0049(17) 0.0081(18) C2 0.023(3) 0.033(3) 0.032(3) 0.011(3) 0.000(2) 0.011(2) N3 0.031(2) 0.022(2) 0.026(2) 0.0077(19) 0.012(2) 0.010(2) C3 0.021(3) 0.034(3) 0.027(3) 0.012(2) -0.002(2) 0.006(2) N4 0.021(2) 0.024(2) 0.033(2) 0.011(2) 0.0064(19) 0.0090(19) C4 0.017(3) 0.025(3) 0.028(3) 0.013(2) 0.005(2) 0.003(2) N5 0.021(2) 0.018(2) 0.022(2) 0.0049(18) 0.0024(17) 0.0102(18) C5 0.018(3) 0.025(3) 0.027(3) 0.013(2) 0.004(2) 0.006(2) N6 0.016(2) 0.023(2) 0.028(2) 0.0077(19) 0.0028(18) 0.0078(18) C6 0.021(3) 0.034(3) 0.025(3) 0.010(2) 0.000(2) 0.003(2) N7 0.022(2) 0.022(2) 0.026(2) 0.0062(19) 0.0026(18) 0.0095(18) C7 0.028(3) 0.025(3) 0.026(3) 0.005(2) 0.004(2) 0.004(2) N8 0.023(2) 0.024(2) 0.023(2) 0.0070(19) 0.0044(18) 0.0104(19) C8 0.021(3) 0.028(3) 0.021(3) 0.008(2) 0.006(2) 0.004(2) N9 0.025(2) 0.029(2) 0.027(2) 0.013(2) 0.0070(19) 0.010(2) C9 0.025(3) 0.020(3) 0.022(3) 0.006(2) 0.009(2) 0.009(2) C10 0.024(3) 0.024(3) 0.024(3) 0.009(2) 0.008(2) 0.012(2) C11 0.025(3) 0.028(3) 0.032(3) 0.013(2) 0.006(2) 0.008(2) C12 0.028(3) 0.033(3) 0.038(3) 0.017(3) 0.014(3) 0.017(3) C13 0.040(3) 0.026(3) 0.028(3) 0.005(2) 0.010(3) 0.013(3) C14 0.023(3) 0.022(3) 0.035(3) 0.009(2) 0.008(2) 0.006(2) C15 0.039(3) 0.032(3) 0.032(3) 0.012(3) 0.010(3) 0.011(3) C16 0.035(3) 0.029(3) 0.021(3) 0.004(2) 0.002(2) 0.010(3) C17 0.026(3) 0.020(3) 0.027(3) 0.007(2) 0.004(2) 0.008(2) C18 0.024(3) 0.016(2) 0.027(3) 0.005(2) 0.003(2) 0.008(2) C19 0.026(3) 0.024(3) 0.029(3) 0.003(2) -0.002(2) 0.010(2) C20 0.017(3) 0.023(3) 0.030(3) 0.010(2) 0.004(2) 0.010(2) C21 0.018(3) 0.018(3) 0.030(3) 0.002(2) 0.003(2) 0.010(2) C22 0.015(3) 0.024(3) 0.029(3) 0.009(2) 0.006(2) 0.010(2) C23 0.017(3) 0.021(3) 0.026(3) 0.006(2) 0.000(2) 0.007(2) C24 0.024(3) 0.023(3) 0.024(3) 0.007(2) 0.005(2) 0.011(2) C25 0.024(3) 0.026(3) 0.031(3) 0.010(2) 0.011(2) 0.014(2) C26 0.021(3) 0.026(3) 0.027(3) 0.005(2) 0.001(2) 0.007(2) C27 0.024(3) 0.026(3) 0.031(3) 0.009(2) 0.004(2) 0.011(2) C28 0.018(3) 0.031(3) 0.043(3) 0.013(3) 0.001(2) 0.010(2) C29 0.021(3) 0.024(3) 0.037(3) -0.001(2) -0.010(2) 0.009(2) C30 0.025(3) 0.019(3) 0.029(3) 0.004(2) 0.001(2) 0.010(2) C31 0.025(3) 0.018(3) 0.026(3) 0.003(2) 0.001(2) 0.012(2) C32 0.031(3) 0.023(3) 0.030(3) 0.005(2) -0.010(2) 0.010(2) C33 0.038(3) 0.022(3) 0.025(3) 0.008(2) -0.002(2) 0.014(2) C34 0.033(3) 0.019(3) 0.027(3) 0.005(2) 0.004(2) 0.017(2) C35 0.028(3) 0.021(3) 0.026(3) 0.008(2) 0.004(2) 0.012(2) C36 0.037(3) 0.025(3) 0.028(3) 0.008(2) 0.004(2) 0.011(3) C37 0.040(3) 0.026(3) 0.038(3) 0.013(3) 0.014(3) 0.011(3) C38 0.027(3) 0.029(3) 0.045(4) 0.017(3) 0.007(3) 0.010(2) C39 0.024(3) 0.033(3) 0.028(3) 0.010(2) 0.001(2) 0.011(2) F1A 0.0246(17) 0.049(2) 0.0399(19) 0.0134(16) -0.0050(14) 0.0070(15) B1A 0.026(3) 0.041(4) 0.026(3) 0.010(3) 0.000(3) 0.003(3) F2A 0.0317(19) 0.069(2) 0.058(2) 0.042(2) 0.0012(17) 0.0083(18) B2A 0.033(4) 0.031(3) 0.032(4) 0.011(3) 0.005(3) 0.016(3) F3A 0.0298(18) 0.079(3) 0.0344(19) 0.0247(18) 0.0069(15) 0.0110(18) F4A 0.053(2) 0.038(2) 0.058(2) 0.0036(18) 0.0040(19) 0.0039(18) F5A 0.0294(18) 0.045(2) 0.0387(19) 0.0065(16) 0.0041(15) 0.0127(16) F6A 0.0344(18) 0.060(2) 0.0413(19) 0.0280(17) 0.0100(15) 0.0207(17) F7A 0.0324(18) 0.050(2) 0.0433(19) 0.0226(16) 0.0177(15) 0.0174(16) F8A 0.0414(19) 0.0421(19) 0.0396(19) 0.0164(16) 0.0105(15) 0.0220(16) Cl1S 0.0385(9) 0.0677(11) 0.0475(9) 0.0288(8) 0.0023(7) 0.0155(8) C1S 0.041(4) 0.058(4) 0.041(4) 0.023(3) 0.010(3) 0.015(3) Cl2S 0.0433(9) 0.0604(10) 0.0332(8) 0.0151(8) -0.0004(7) 0.0060(8) C2S 0.040(4) 0.053(4) 0.050(4) 0.021(3) 0.008(3) 0.014(3) Cl3S 0.0935(15) 0.0521(11) 0.0665(12) 0.0252(10) 0.0297(11) 0.0231(11) Cl4S 0.0377(9) 0.0625(12) 0.0855(14) 0.0003(10) -0.0066(9) 0.0210(9) O1W 0.0151(17) 0.0296(19) 0.033(2) 0.0109(16) 0.0074(15) 0.0103(15) _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 C23 1.944(5) . ? Pd1 N1 2.031(4) . ? Pd1 N5 2.093(4) . ? Pd1 O1W 2.154(3) . ? Pd1 Pd2 3.0434(6) . ? N1 C1 1.342(6) . ? N1 C5 1.370(6) . ? C1 C2 1.378(7) . ? Pd2 C10 1.955(5) . ? Pd2 N7 2.025(4) . ? Pd2 N2 2.086(4) . ? Pd2 C23 2.410(5) . ? N2 C5 1.360(6) . ? N2 C8 1.374(6) . ? C2 C3 1.371(7) . ? N3 C12 1.346(6) . ? N3 C9 1.387(6) . ? N3 C13 1.456(6) . ? C3 C4 1.391(7) . ? N4 C14 1.322(6) . ? N4 C18 1.368(6) . ? C4 C6 1.403(7) . ? C4 C5 1.424(7) . ? N5 C21 1.358(6) . ? N5 C18 1.372(6) . ? N6 C25 1.367(6) . ? N6 C22 1.377(6) . ? N6 C26 1.460(6) . ? C6 C7 1.356(7) . ? N7 C27 1.332(6) . ? N7 C31 1.379(6) . ? C7 C8 1.427(7) . ? N8 C34 1.326(6) . ? N8 C31 1.348(6) . ? C8 C9 1.415(7) . ? N9 C38 1.359(6) . ? N9 C35 1.391(6) . ? N9 C39 1.461(6) . ? C9 C10 1.393(6) . ? C10 C11 1.405(7) . ? C11 C12 1.395(7) . ? C14 C15 1.400(7) . ? C15 C16 1.351(7) . ? C16 C17 1.412(7) . ? C17 C19 1.400(7) . ? C17 C18 1.421(7) . ? C19 C20 1.354(7) . ? C20 C21 1.399(7) . ? C21 C22 1.438(7) . ? C22 C23 1.393(6) . ? C23 C24 1.423(7) . ? C24 C25 1.367(7) . ? C27 C28 1.388(7) . ? C28 C29 1.358(7) . ? C29 C30 1.403(7) . ? C30 C31 1.405(7) . ? C30 C32 1.431(7) . ? C32 C33 1.344(7) . ? C33 C34 1.431(7) . ? C34 C35 1.452(7) . ? C35 C36 1.386(7) . ? C36 C37 1.384(7) . ? C37 C38 1.385(7) . ? F1A B1A 1.392(7) . ? B1A F2A 1.375(7) . ? B1A F3A 1.382(7) . ? B1A F4A 1.397(7) . ? B2A F8A 1.389(6) . ? B2A F7A 1.393(7) . ? B2A F6A 1.394(7) . ? B2A F5A 1.395(7) . ? Cl1S C1S 1.771(6) . ? C1S Cl2S 1.768(6) . ? C2S Cl3S 1.749(6) . ? C2S Cl4S 1.756(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 C23 Pd1 N1 93.22(18) . . ? C23 Pd1 N5 80.78(18) . . ? N1 Pd1 N5 173.60(15) . . ? C23 Pd1 O1W 175.72(16) . . ? N1 Pd1 O1W 88.12(14) . . ? N5 Pd1 O1W 97.71(14) . . ? C23 Pd1 Pd2 52.32(14) . . ? N1 Pd1 Pd2 80.35(11) . . ? N5 Pd1 Pd2 97.54(10) . . ? O1W Pd1 Pd2 131.96(9) . . ? C1 N1 C5 118.5(4) . . ? C1 N1 Pd1 113.1(3) . . ? C5 N1 Pd1 127.3(3) . . ? N1 C1 C2 124.2(5) . . ? C10 Pd2 N7 88.39(18) . . ? C10 Pd2 N2 81.32(18) . . ? N7 Pd2 N2 169.68(15) . . ? C10 Pd2 C23 175.22(18) . . ? N7 Pd2 C23 91.59(16) . . ? N2 Pd2 C23 98.73(15) . . ? C10 Pd2 Pd1 144.30(14) . . ? N7 Pd2 Pd1 111.34(11) . . ? N2 Pd2 Pd1 77.27(11) . . ? C23 Pd2 Pd1 39.67(11) . . ? C5 N2 C8 118.5(4) . . ? C5 N2 Pd2 128.6(3) . . ? C8 N2 Pd2 112.5(3) . . ? C3 C2 C1 118.1(5) . . ? C12 N3 C9 107.7(4) . . ? C12 N3 C13 123.5(4) . . ? C9 N3 C13 128.7(4) . . ? C2 C3 C4 120.3(5) . . ? C14 N4 C18 118.0(4) . . ? C3 C4 C6 123.1(5) . . ? C3 C4 C5 118.9(4) . . ? C6 C4 C5 118.0(5) . . ? C21 N5 C18 118.3(4) . . ? C21 N5 Pd1 114.8(3) . . ? C18 N5 Pd1 126.9(3) . . ? N2 C5 N1 118.2(4) . . ? N2 C5 C4 121.8(4) . . ? N1 C5 C4 119.9(4) . . ? C25 N6 C22 107.9(4) . . ? C25 N6 C26 123.9(4) . . ? C22 N6 C26 128.2(4) . . ? C7 C6 C4 120.5(5) . . ? C27 N7 C31 118.5(4) . . ? C27 N7 Pd2 125.3(3) . . ? C31 N7 Pd2 116.2(3) . . ? C6 C7 C8 119.5(5) . . ? C34 N8 C31 118.3(4) . . ? N2 C8 C9 112.6(4) . . ? N2 C8 C7 121.0(5) . . ? C9 C8 C7 126.4(5) . . ? C38 N9 C35 108.5(4) . . ? C38 N9 C39 122.1(4) . . ? C35 N9 C39 128.9(4) . . ? N3 C9 C10 108.2(4) . . ? N3 C9 C8 132.2(5) . . ? C10 C9 C8 119.6(4) . . ? C9 C10 C11 107.8(4) . . ? C9 C10 Pd2 112.6(3) . . ? C11 C10 Pd2 139.4(4) . . ? C12 C11 C10 105.6(5) . . ? N3 C12 C11 110.7(5) . . ? N4 C14 C15 124.2(5) . . ? C16 C15 C14 118.5(5) . . ? C15 C16 C17 120.4(5) . . ? C19 C17 C16 124.5(5) . . ? C19 C17 C18 118.1(5) . . ? C16 C17 C18 117.4(5) . . ? N4 C18 N5 116.9(4) . . ? N4 C18 C17 121.6(5) . . ? N5 C18 C17 121.5(4) . . ? C20 C19 C17 120.1(5) . . ? C19 C20 C21 120.1(5) . . ? N5 C21 C20 122.0(5) . . ? N5 C21 C22 111.0(4) . . ? C20 C21 C22 127.0(4) . . ? N6 C22 C23 108.7(4) . . ? N6 C22 C21 131.6(4) . . ? C23 C22 C21 119.7(4) . . ? C22 C23 C24 106.5(4) . . ? C22 C23 Pd1 113.6(4) . . ? C24 C23 Pd1 139.6(4) . . ? C22 C23 Pd2 108.0(3) . . ? C24 C23 Pd2 84.5(3) . . ? Pd1 C23 Pd2 88.01(18) . . ? C25 C24 C23 107.0(4) . . ? C24 C25 N6 109.9(4) . . ? N7 C27 C28 123.2(5) . . ? C29 C28 C27 119.3(5) . . ? C28 C29 C30 119.6(5) . . ? C29 C30 C31 118.7(5) . . ? C29 C30 C32 125.4(5) . . ? C31 C30 C32 115.9(5) . . ? N8 C31 N7 115.1(4) . . ? N8 C31 C30 124.3(5) . . ? N7 C31 C30 120.6(5) . . ? C33 C32 C30 119.7(5) . . ? C32 C33 C34 120.1(5) . . ? N8 C34 C33 121.4(5) . . ? N8 C34 C35 118.7(4) . . ? C33 C34 C35 119.8(5) . . ? C36 C35 N9 106.6(4) . . ? C36 C35 C34 129.6(5) . . ? N9 C35 C34 123.8(4) . . ? C37 C36 C35 109.2(5) . . ? C36 C37 C38 106.5(5) . . ? N9 C38 C37 109.3(5) . . ? F2A B1A F3A 110.2(5) . . ? F2A B1A F1A 109.6(5) . . ? F3A B1A F1A 110.5(5) . . ? F2A B1A F4A 110.0(5) . . ? F3A B1A F4A 108.2(5) . . ? F1A B1A F4A 108.3(5) . . ? F8A B2A F7A 110.2(5) . . ? F8A B2A F6A 109.4(5) . . ? F7A B2A F6A 109.0(5) . . ? F8A B2A F5A 109.8(5) . . ? F7A B2A F5A 109.7(5) . . ? F6A B2A F5A 108.5(5) . . ? Cl2S C1S Cl1S 111.0(3) . . ? Cl3S C2S Cl4S 112.8(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.461 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.125 _iucr_refine_instructions_details ; TITL compound_1 CELL 0.71073 11.4647 14.1481 15.6504 111.841 91.505 108.809 ZERR 2.0000 0.0016 0.0019 0.0021 0.002 0.002 0.002 LATT 1 SFAC C H N O PD B F CL UNIT 82 70 18 2 4 4 16 8 MERG 2 SHEL 99999.00 0.85 FMAP 2 GRID PLAN 2 TEMP -173 SIZE 0.25 0.27 0.24 L.S. 5 ACTA WGHT 0.06460 0.00000 0.00000 0.00000 0.00000 0.33330 FVAR 0.20701 Pd1 5 0.83725 0.77881 0.35432 11.00000 0.01647 0.02182 = 0.02311 0.00559 0.00234 0.00795 N1 3 0.76129 0.72863 0.21912 11.00000 0.02123 0.01897 = 0.02627 0.00649 0.00362 0.00717 C1 1 0.67652 0.77236 0.20935 11.00000 0.02362 0.02997 = 0.03360 0.01238 0.00464 0.01385 AFIX 43 H1 2 0.67050 0.83047 0.26245 11.00000 -1.20000 AFIX 0 Pd2 5 1.01411 0.66921 0.25718 11.00000 0.01907 0.02312 = 0.02245 0.00629 0.00252 0.00953 N2 3 0.85830 0.60181 0.15298 11.00000 0.01900 0.02425 = 0.01880 0.00794 0.00494 0.00808 C2 1 0.59764 0.73843 0.12726 11.00000 0.02303 0.03342 = 0.03175 0.01089 0.00013 0.01127 AFIX 43 H2 2 0.54036 0.77315 0.12365 11.00000 -1.20000 AFIX 0 N3 3 0.96936 0.37268 0.05790 11.00000 0.03090 0.02249 = 0.02609 0.00772 0.01223 0.01025 C3 1 0.60419 0.65312 0.05094 11.00000 0.02044 0.03439 = 0.02745 0.01247 -0.00161 0.00569 AFIX 43 H3 2 0.55084 0.62804 -0.00652 11.00000 -1.20000 AFIX 0 N4 3 0.75662 0.77735 0.55361 11.00000 0.02070 0.02423 = 0.03268 0.01103 0.00644 0.00899 C4 1 0.68860 0.60313 0.05725 11.00000 0.01746 0.02511 = 0.02759 0.01290 0.00536 0.00340 N5 3 0.93216 0.84337 0.49105 11.00000 0.02070 0.01754 = 0.02187 0.00487 0.00240 0.01017 C5 1 0.77060 0.64448 0.14317 11.00000 0.01832 0.02496 = 0.02699 0.01253 0.00411 0.00640 N6 3 1.20520 0.95626 0.39637 11.00000 0.01609 0.02348 = 0.02793 0.00772 0.00275 0.00777 C6 1 0.69571 0.51222 -0.01684 11.00000 0.02137 0.03389 = 0.02450 0.01003 -0.00039 0.00253 AFIX 43 H6 2 0.64586 0.48583 -0.07608 11.00000 -1.20000 AFIX 0 N7 3 1.16887 0.70825 0.34740 11.00000 0.02179 0.02233 = 0.02578 0.00616 0.00256 0.00947 C7 1 0.77318 0.46176 -0.00454 11.00000 0.02804 0.02497 = 0.02646 0.00527 0.00438 0.00451 AFIX 43 H7 2 0.77222 0.39638 -0.05304 11.00000 -1.20000 AFIX 0 N8 3 1.02791 0.64640 0.43394 11.00000 0.02294 0.02362 = 0.02328 0.00695 0.00438 0.01038 C8 1 0.85622 0.50768 0.08187 11.00000 0.02058 0.02827 = 0.02080 0.00784 0.00616 0.00433 N9 3 0.77478 0.52802 0.44035 11.00000 0.02455 0.02901 = 0.02737 0.01344 0.00702 0.00974 C9 1 0.94576 0.46760 0.10430 11.00000 0.02470 0.02035 = 0.02169 0.00581 0.00918 0.00854 C10 1 1.03052 0.52860 0.18744 11.00000 0.02373 0.02430 = 0.02390 0.00864 0.00849 0.01206 C11 1 1.10799 0.47072 0.19195 11.00000 0.02453 0.02795 = 0.03220 0.01276 0.00637 0.00817 AFIX 43 H11 2 1.17523 0.49228 0.24013 11.00000 -1.20000 AFIX 0 C12 1 1.06552 0.37492 0.11085 11.00000 0.02804 0.03342 = 0.03792 0.01747 0.01370 0.01736 AFIX 43 H12 2 1.09977 0.31895 0.09514 11.00000 -1.20000 AFIX 0 C13 1 0.90170 0.28096 -0.02905 11.00000 0.04017 0.02586 = 0.02787 0.00520 0.00952 0.01337 AFIX 137 H13A 2 0.93568 0.22282 -0.04063 11.00000 -1.50000 H13B 2 0.91088 0.30481 -0.08061 11.00000 -1.50000 H13C 2 0.81299 0.25349 -0.02443 11.00000 -1.50000 AFIX 0 C14 1 0.70691 0.76501 0.62579 11.00000 0.02315 0.02197 = 0.03530 0.00853 0.00789 0.00603 AFIX 43 H14 2 0.61934 0.72739 0.61648 11.00000 -1.20000 AFIX 0 C15 1 0.77512 0.80387 0.71507 11.00000 0.03929 0.03213 = 0.03198 0.01185 0.01017 0.01053 AFIX 43 H15 2 0.73454 0.79355 0.76477 11.00000 -1.20000 AFIX 0 C16 1 0.89994 0.85637 0.72896 11.00000 0.03544 0.02856 = 0.02058 0.00384 0.00203 0.01025 AFIX 43 H16 2 0.94813 0.88220 0.78875 11.00000 -1.20000 AFIX 0 C17 1 0.95914 0.87303 0.65511 11.00000 0.02639 0.01965 = 0.02711 0.00661 0.00353 0.00826 C18 1 0.88279 0.83109 0.56681 11.00000 0.02445 0.01561 = 0.02673 0.00476 0.00253 0.00831 C19 1 1.08770 0.92592 0.66257 11.00000 0.02610 0.02369 = 0.02891 0.00298 -0.00231 0.00959 AFIX 43 H19 2 1.14152 0.95238 0.72010 11.00000 -1.20000 AFIX 0 C20 1 1.13538 0.93938 0.58792 11.00000 0.01665 0.02333 = 0.03016 0.00963 0.00427 0.00984 AFIX 43 H20 2 1.22236 0.97678 0.59354 11.00000 -1.20000 AFIX 0 C21 1 1.05682 0.89831 0.50252 11.00000 0.01794 0.01839 = 0.03036 0.00206 0.00301 0.00990 C22 1 1.09285 0.90337 0.41658 11.00000 0.01537 0.02402 = 0.02900 0.00928 0.00555 0.01043 C23 1 1.00473 0.84839 0.33505 11.00000 0.01718 0.02089 = 0.02635 0.00602 0.00001 0.00672 C24 1 1.06711 0.87067 0.26349 11.00000 0.02419 0.02278 = 0.02442 0.00714 0.00473 0.01065 AFIX 43 H24 2 1.03143 0.84500 0.19994 11.00000 -1.20000 AFIX 0 C25 1 1.18816 0.93606 0.30356 11.00000 0.02422 0.02630 = 0.03133 0.00971 0.01081 0.01417 AFIX 43 H25 2 1.25110 0.96340 0.27165 11.00000 -1.20000 AFIX 0 C26 1 1.32466 1.02167 0.45914 11.00000 0.02104 0.02607 = 0.02655 0.00454 0.00055 0.00665 AFIX 137 H26A 2 1.38808 1.04806 0.42440 11.00000 -1.50000 H26B 2 1.35025 0.97685 0.48518 11.00000 -1.50000 H26C 2 1.31581 1.08400 0.50995 11.00000 -1.50000 AFIX 0 C27 1 1.28617 0.74752 0.33452 11.00000 0.02386 0.02566 = 0.03126 0.00918 0.00388 0.01055 AFIX 43 H27 2 1.29990 0.75759 0.27840 11.00000 -1.20000 AFIX 0 C28 1 1.38930 0.77443 0.39910 11.00000 0.01841 0.03071 = 0.04323 0.01281 0.00136 0.00976 AFIX 43 H28 2 1.47137 0.79940 0.38594 11.00000 -1.20000 AFIX 0 C29 1 1.37163 0.76468 0.48132 11.00000 0.02060 0.02444 = 0.03657 -0.00089 -0.00971 0.00856 AFIX 43 H29 2 1.44141 0.78579 0.52729 11.00000 -1.20000 AFIX 0 C30 1 1.24978 0.72327 0.49804 11.00000 0.02521 0.01938 = 0.02879 0.00355 0.00133 0.01027 C31 1 1.14875 0.69239 0.42835 11.00000 0.02510 0.01828 = 0.02610 0.00343 0.00078 0.01155 C32 1 1.21796 0.70923 0.58145 11.00000 0.03106 0.02332 = 0.03028 0.00477 -0.01004 0.01032 AFIX 43 H32 2 1.28170 0.73179 0.63245 11.00000 -1.20000 AFIX 0 C33 1 1.09746 0.66399 0.58730 11.00000 0.03791 0.02230 = 0.02451 0.00781 -0.00227 0.01409 AFIX 43 H33 2 1.07588 0.65507 0.64273 11.00000 -1.20000 AFIX 0 C34 1 1.00162 0.62924 0.51011 11.00000 0.03335 0.01856 = 0.02696 0.00478 0.00406 0.01724 C35 1 0.87196 0.57700 0.51560 11.00000 0.02781 0.02084 = 0.02594 0.00770 0.00379 0.01191 C36 1 0.81864 0.56711 0.59177 11.00000 0.03742 0.02529 = 0.02774 0.00771 0.00394 0.01115 AFIX 43 H36 2 0.86289 0.59263 0.65290 11.00000 -1.20000 AFIX 0 C37 1 0.69072 0.51418 0.56462 11.00000 0.04030 0.02559 = 0.03760 0.01312 0.01423 0.01072 AFIX 43 H37 2 0.63145 0.49797 0.60317 11.00000 -1.20000 AFIX 0 C38 1 0.66613 0.48951 0.47012 11.00000 0.02687 0.02934 = 0.04471 0.01693 0.00714 0.00962 AFIX 43 H38 2 0.58595 0.45163 0.43211 11.00000 -1.20000 AFIX 0 C39 1 0.78109 0.50444 0.34181 11.00000 0.02445 0.03315 = 0.02809 0.00957 0.00049 0.01098 AFIX 137 H39A 2 0.70392 0.44571 0.30345 11.00000 -1.50000 H39B 2 0.85258 0.48176 0.32533 11.00000 -1.50000 H39C 2 0.79099 0.57004 0.33052 11.00000 -1.50000 AFIX 0 F1A 7 0.34532 0.36277 0.15272 11.00000 0.02460 0.04947 = 0.03989 0.01334 -0.00496 0.00704 B1A 6 0.46332 0.41573 0.20775 11.00000 0.02575 0.04136 = 0.02600 0.00989 -0.00030 0.00304 F2A 7 0.47705 0.36146 0.26199 11.00000 0.03166 0.06906 = 0.05778 0.04222 0.00123 0.00828 B2A 6 0.52892 -0.01591 0.26280 11.00000 0.03301 0.03065 = 0.03207 0.01122 0.00552 0.01649 F3A 7 0.55531 0.42090 0.15250 11.00000 0.02985 0.07909 = 0.03440 0.02471 0.00687 0.01098 F4A 7 0.47417 0.52214 0.26453 11.00000 0.05321 0.03828 = 0.05812 0.00352 0.00398 0.00379 F5A 7 0.42690 -0.10818 0.20709 11.00000 0.02940 0.04528 = 0.03866 0.00647 0.00410 0.01267 F6A 7 0.56511 -0.03013 0.34157 11.00000 0.03446 0.05968 = 0.04132 0.02805 0.01002 0.02068 F7A 7 0.62812 -0.00349 0.21337 11.00000 0.03240 0.05015 = 0.04325 0.02255 0.01769 0.01734 F8A 7 0.49543 0.07578 0.29022 11.00000 0.04140 0.04212 = 0.03961 0.01643 0.01052 0.02196 Cl1S 8 0.57048 0.15157 0.00921 11.00000 0.03851 0.06779 = 0.04755 0.02885 0.00227 0.01548 C1S 1 0.60798 0.17556 0.12769 11.00000 0.04061 0.05811 = 0.04116 0.02299 0.01002 0.01546 AFIX 23 H1S1 2 0.57121 0.22781 0.16714 11.00000 -1.20000 H1S2 2 0.57147 0.10641 0.13584 11.00000 -1.20000 AFIX 0 Cl2S 8 0.77163 0.22863 0.16404 11.00000 0.04336 0.06045 = 0.03324 0.01514 -0.00038 0.00600 C2S 1 0.74494 0.89772 0.01433 11.00000 0.04030 0.05305 = 0.04967 0.02106 0.00820 0.01404 AFIX 23 H2S1 2 0.69131 0.82151 -0.02529 11.00000 -1.20000 H2S2 2 0.70101 0.92626 0.06600 11.00000 -1.20000 AFIX 0 Cl3S 8 0.76583 0.97567 -0.05228 11.00000 0.09358 0.05217 = 0.06650 0.02523 0.02977 0.02311 Cl4S 8 0.88653 0.89893 0.06112 11.00000 0.03769 0.06251 = 0.08560 0.00030 -0.00661 0.02103 O1W 4 0.65147 0.71370 0.38142 11.00000 0.01510 0.02956 = 0.03327 0.01095 0.00740 0.01028 HKLF 4 ; _database_code_depnum_ccdc_archive 'CCDC 940018' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H47 N8 O Pd3 S4, 3(BF4), H2O, 2(CH2Cl2)' _chemical_formula_sum 'C58 H53 B3 Cl4 F12 N8 O2 Pd3 S4' _chemical_formula_weight 1743.84 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' Pd Pd -0.9988 1.0072 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.485(2) _cell_length_b 22.628(3) _cell_length_c 14.2391(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.457(2) _cell_angle_gamma 90.00 _cell_volume 6173.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6172 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.71 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 1.262 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7302 _exptl_absorpt_correction_T_max 0.8046 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42227 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 24.71 _reflns_number_total 10510 _reflns_number_gt 6415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ortep _computing_publication_material ciftab _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. All H-atoms except those of water molecules were introduced into geometrically calculated positions in the final stages of refinement and were refined according to 'riding model'. Hydrogen atoms of the coordinated water molecules were not located, but were included in the formula sum for the calculation of the intensive properties. ; _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^)+(0.0952P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10510 _refine_ls_number_parameters 792 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1630 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.38358(3) 0.51849(3) 0.16237(4) 0.04018(19) Uani 1 1 d . . . S1 S 0.18252(12) 0.29102(9) 0.33350(15) 0.0469(5) Uani 1 1 d . . . N1 N 0.3767(3) 0.5507(3) 0.2931(4) 0.0397(16) Uani 1 1 d . . . C1 C 0.4034(4) 0.6048(3) 0.3121(6) 0.046(2) Uani 1 1 d . . . H1 H 0.4310 0.6211 0.2700 0.055 Uiso 1 1 calc R . . Pd2 Pd 0.33863(3) 0.41258(2) 0.23556(4) 0.03454(17) Uani 1 1 d . . . S2 S 0.55208(12) 0.38851(10) 0.28383(16) 0.0499(6) Uani 1 1 d . . . N2 N 0.3137(3) 0.4707(3) 0.3353(4) 0.0396(16) Uani 1 1 d . . . C2 C 0.3932(5) 0.6382(4) 0.3901(6) 0.057(2) Uani 1 1 d . . . H2 H 0.4144 0.6759 0.4021 0.069 Uiso 1 1 calc R . . Pd3 Pd 0.22920(3) 0.43548(3) 0.09756(4) 0.03807(18) Uani 1 1 d . . . S3 S 0.09822(14) 0.48794(12) -0.18345(17) 0.0665(7) Uani 1 1 d . . . N3 N 0.3068(4) 0.5441(3) -0.0550(5) 0.0502(18) Uani 1 1 d . . . C3 C 0.3521(4) 0.6158(4) 0.4486(6) 0.048(2) Uani 1 1 d . . . H3 H 0.3423 0.6385 0.5007 0.057 Uiso 1 1 calc R . . S4 S 0.01121(15) 0.22870(13) 0.0328(3) 0.0853(9) Uani 1 1 d . . . N4 N 0.3970(4) 0.4853(3) 0.0320(4) 0.0429(16) Uani 1 1 d . . . C4 C 0.3243(4) 0.5593(4) 0.4320(6) 0.044(2) Uani 1 1 d . . . N5 N 0.3592(3) 0.3477(3) 0.1475(4) 0.0364(15) Uani 1 1 d . . . C5 C 0.3385(4) 0.5264(3) 0.3530(5) 0.0363(18) Uani 1 1 d . . . N6 N 0.2804(3) 0.3830(3) 0.0173(4) 0.0368(15) Uani 1 1 d . . . C6 C 0.2819(5) 0.5332(4) 0.4882(6) 0.049(2) Uani 1 1 d . . . H6 H 0.2709 0.5543 0.5411 0.059 Uiso 1 1 calc R . . N7 N 0.1725(3) 0.4839(3) 0.1763(4) 0.0427(16) Uani 1 1 d . . . C7 C 0.2556(5) 0.4781(4) 0.4695(6) 0.051(2) Uani 1 1 d . . . H7 H 0.2264 0.4608 0.5088 0.061 Uiso 1 1 calc R . . N8 N 0.1036(4) 0.4013(3) 0.1648(5) 0.0486(18) Uani 1 1 d . . . C8 C 0.2721(4) 0.4468(3) 0.3910(5) 0.0396(19) Uani 1 1 d . . . C9 C 0.2451(4) 0.3894(3) 0.3612(5) 0.0376(18) Uani 1 1 d . . . C10 C 0.2641(4) 0.3646(3) 0.2755(5) 0.0372(18) Uani 1 1 d . . . C11 C 0.2331(4) 0.3123(3) 0.2503(5) 0.0404(19) Uani 1 1 d . . . C12 C 0.2023(4) 0.3530(4) 0.4010(6) 0.045(2) Uani 1 1 d . . . C13 C 0.2306(4) 0.2708(3) 0.1669(6) 0.043(2) Uani 1 1 d . . . H13A H 0.2192 0.2931 0.1071 0.064 Uiso 1 1 calc R . . H13B H 0.1947 0.2407 0.1688 0.064 Uiso 1 1 calc R . . H13C H 0.2761 0.2517 0.1705 0.064 Uiso 1 1 calc R . . C14 C 0.1724(5) 0.3586(4) 0.4913(6) 0.058(2) Uani 1 1 d . . . H14A H 0.2094 0.3700 0.5444 0.087 Uiso 1 1 calc R . . H14B H 0.1524 0.3207 0.5057 0.087 Uiso 1 1 calc R . . H14C H 0.1358 0.3889 0.4824 0.087 Uiso 1 1 calc R . . C15 C 0.2688(5) 0.5599(4) -0.1377(6) 0.059(3) Uani 1 1 d . . . H15 H 0.2327 0.5881 -0.1376 0.070 Uiso 1 1 calc R . . C16 C 0.2791(6) 0.5374(5) -0.2242(7) 0.073(3) Uani 1 1 d . . . H16 H 0.2494 0.5494 -0.2814 0.088 Uiso 1 1 calc R . . C17 C 0.3307(5) 0.4987(4) -0.2285(6) 0.056(2) Uani 1 1 d . . . H17 H 0.3378 0.4842 -0.2886 0.067 Uiso 1 1 calc R . . C18 C 0.3748(5) 0.4793(4) -0.1431(6) 0.051(2) Uani 1 1 d . . . C19 C 0.3579(5) 0.5036(4) -0.0562(5) 0.046(2) Uani 1 1 d . . . C20 C 0.4272(5) 0.4378(4) -0.1359(5) 0.050(2) Uani 1 1 d . . . H20 H 0.4388 0.4215 -0.1925 0.059 Uiso 1 1 calc R . . C21 C 0.4630(5) 0.4197(4) -0.0491(6) 0.050(2) Uani 1 1 d . . . H21 H 0.4984 0.3905 -0.0451 0.060 Uiso 1 1 calc R . . C22 C 0.4460(5) 0.4454(3) 0.0360(5) 0.041(2) Uani 1 1 d . . . C23 C 0.4799(4) 0.4286(3) 0.1308(6) 0.044(2) Uani 1 1 d . . . C24 C 0.4525(4) 0.4563(3) 0.2096(5) 0.0402(19) Uani 1 1 d . . . C25 C 0.4904(4) 0.4393(3) 0.2964(6) 0.046(2) Uani 1 1 d . . . C26 C 0.5329(5) 0.3907(4) 0.1607(6) 0.046(2) Uani 1 1 d . . . C27 C 0.4859(5) 0.4578(4) 0.3987(5) 0.053(2) Uani 1 1 d . . . H27C H 0.4902 0.5008 0.4045 0.080 Uiso 1 1 calc R . . H27A H 0.5237 0.4389 0.4434 0.080 Uiso 1 1 calc R . . H27B H 0.4409 0.4454 0.4134 0.080 Uiso 1 1 calc R . . C28 C 0.5755(5) 0.3512(4) 0.1086(6) 0.058(2) Uani 1 1 d . . . H28A H 0.5453 0.3207 0.0738 0.087 Uiso 1 1 calc R . . H28B H 0.6125 0.3323 0.1547 0.087 Uiso 1 1 calc R . . H28C H 0.5964 0.3747 0.0634 0.087 Uiso 1 1 calc R . . C29 C 0.4057(4) 0.3073(3) 0.1875(6) 0.046(2) Uani 1 1 d . . . H29 H 0.4213 0.3078 0.2547 0.055 Uiso 1 1 calc R . . C30 C 0.4318(5) 0.2642(4) 0.1321(6) 0.054(2) Uani 1 1 d . . . H30 H 0.4649 0.2359 0.1613 0.064 Uiso 1 1 calc R . . C31 C 0.4091(4) 0.2638(4) 0.0375(6) 0.048(2) Uani 1 1 d . . . H31 H 0.4276 0.2356 -0.0006 0.057 Uiso 1 1 calc R . . C32 C 0.3601(4) 0.3031(3) -0.0052(6) 0.043(2) Uani 1 1 d . . . C33 C 0.3325(4) 0.3451(3) 0.0526(5) 0.0360(18) Uani 1 1 d . . . C34 C 0.3317(5) 0.3061(4) -0.1060(6) 0.052(2) Uani 1 1 d . . . H34 H 0.3484 0.2796 -0.1486 0.063 Uiso 1 1 calc R . . C35 C 0.2833(5) 0.3446(4) -0.1400(6) 0.048(2) Uani 1 1 d . . . H35 H 0.2681 0.3475 -0.2071 0.058 Uiso 1 1 calc R . . C36 C 0.2532(5) 0.3822(4) -0.0790(6) 0.048(2) Uani 1 1 d . . . C37 C 0.1958(4) 0.4238(4) -0.1045(5) 0.046(2) Uani 1 1 d . . . C38 C 0.1758(4) 0.4566(4) -0.0285(6) 0.043(2) Uani 1 1 d . . . C39 C 0.1234(5) 0.4939(4) -0.0595(6) 0.056(2) Uani 1 1 d . . . C40 C 0.1577(5) 0.4352(4) -0.1924(6) 0.057(2) Uani 1 1 d . . . C41 C 0.0856(5) 0.5389(4) -0.0094(7) 0.064(3) Uani 1 1 d . . . H41B H 0.0634 0.5190 0.0384 0.095 Uiso 1 1 calc R . . H41C H 0.0498 0.5587 -0.0562 0.095 Uiso 1 1 calc R . . H41A H 0.1190 0.5683 0.0222 0.095 Uiso 1 1 calc R . . C42 C 0.1618(5) 0.4096(4) -0.2898(6) 0.064(3) Uani 1 1 d . . . H42A H 0.2072 0.4191 -0.3062 0.096 Uiso 1 1 calc R . . H42C H 0.1246 0.4265 -0.3378 0.096 Uiso 1 1 calc R . . H42B H 0.1563 0.3666 -0.2881 0.096 Uiso 1 1 calc R . . C43 C 0.1897(5) 0.5371(4) 0.2105(6) 0.049(2) Uani 1 1 d . . . H43 H 0.2237 0.5588 0.1847 0.059 Uiso 1 1 calc R . . C44 C 0.1603(5) 0.5630(5) 0.2827(7) 0.067(3) Uani 1 1 d . . . H44 H 0.1742 0.6013 0.3059 0.080 Uiso 1 1 calc R . . C45 C 0.1105(5) 0.5315(4) 0.3197(7) 0.065(3) Uani 1 1 d . . . H45 H 0.0907 0.5480 0.3701 0.078 Uiso 1 1 calc R . . C46 C 0.0893(5) 0.4766(5) 0.2845(7) 0.059(3) Uani 1 1 d . . . C47 C 0.1205(5) 0.4537(4) 0.2079(6) 0.048(2) Uani 1 1 d . . . C48 C 0.0390(5) 0.4410(5) 0.3151(8) 0.071(3) Uani 1 1 d . . . H48 H 0.0175 0.4545 0.3659 0.085 Uiso 1 1 calc R . . C49 C 0.0203(5) 0.3885(5) 0.2752(8) 0.072(3) Uani 1 1 d . . . H49 H -0.0134 0.3644 0.2973 0.086 Uiso 1 1 calc R . . C50 C 0.0539(5) 0.3697(4) 0.1960(7) 0.061(3) Uani 1 1 d . . . C51 C 0.0349(5) 0.3141(5) 0.1496(8) 0.063(3) Uani 1 1 d . . . C52 C 0.0083(6) 0.2662(5) 0.1995(9) 0.085(4) Uani 1 1 d . . . H52 H 0.0010 0.2689 0.2635 0.103 Uiso 1 1 calc R . . C53 C -0.0053(6) 0.2164(5) 0.1440(9) 0.086(4) Uani 1 1 d . . . C54 C 0.0392(5) 0.2994(4) 0.0559(8) 0.063(3) Uani 1 1 d . . . C55 C -0.0312(8) 0.1572(6) 0.1718(11) 0.139(6) Uani 1 1 d . . . H55A H 0.0063 0.1280 0.1758 0.208 Uiso 1 1 calc R . . H55B H -0.0711 0.1447 0.1236 0.208 Uiso 1 1 calc R . . H55C H -0.0457 0.1605 0.2340 0.208 Uiso 1 1 calc R . . C56 C 0.0622(6) 0.3352(5) -0.0200(8) 0.089(4) Uani 1 1 d . . . H56A H 0.0384 0.3735 -0.0248 0.133 Uiso 1 1 calc R . . H56B H 0.0506 0.3144 -0.0811 0.133 Uiso 1 1 calc R . . H56C H 0.1128 0.3414 -0.0041 0.133 Uiso 1 1 calc R . . F1A F 0.1635(4) 0.6225(3) 0.5149(5) 0.098(2) Uani 1 1 d . . . B1A B 0.1262(8) 0.5928(7) 0.5756(10) 0.079(4) Uani 1 1 d . . . F2A F 0.1438(4) 0.5345(3) 0.5840(5) 0.105(2) Uani 1 1 d . . . B2A B 0.3887(6) 0.3892(5) 0.5995(8) 0.054(3) Uani 1 1 d . . . F3A F 0.1307(4) 0.6190(4) 0.6607(6) 0.135(3) Uani 1 1 d . . . B3A B 0.5645(8) 0.2304(5) 0.3673(7) 0.063(3) Uani 1 1 d . . . F4A F 0.0540(4) 0.5932(4) 0.5292(6) 0.128(3) Uani 1 1 d . . . F5A F 0.3840(3) 0.3657(2) 0.5086(4) 0.0760(16) Uani 1 1 d . . . F6A F 0.4462(3) 0.3672(2) 0.6581(4) 0.0794(17) Uani 1 1 d . . . F7A F 0.3295(3) 0.3753(2) 0.6357(4) 0.0746(16) Uani 1 1 d . . . F8A F 0.3952(3) 0.4497(2) 0.5953(4) 0.0777(16) Uani 1 1 d . . . F9A F 0.5796(3) 0.2451(2) 0.2804(3) 0.0665(14) Uani 1 1 d . . . F10A F 0.5797(4) 0.1710(2) 0.3866(4) 0.089(2) Uani 1 1 d . . . F11A F 0.5939(5) 0.2631(3) 0.4394(5) 0.130(3) Uani 1 1 d . . . F12A F 0.4929(4) 0.2357(4) 0.3618(5) 0.120(3) Uani 1 1 d . . . O1W O 0.3142(3) 0.5896(2) 0.1097(4) 0.0556(15) 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 0.0605(4) 0.0355(4) 0.0249(3) -0.0006(2) 0.0087(3) -0.0081(3) S1 0.0553(14) 0.0411(12) 0.0473(13) 0.0108(10) 0.0177(10) 0.0002(10) N1 0.056(4) 0.028(4) 0.033(4) -0.002(3) 0.003(3) -0.005(3) C1 0.056(6) 0.041(5) 0.039(5) -0.003(4) 0.004(4) -0.007(4) Pd2 0.0490(4) 0.0312(3) 0.0241(3) -0.0003(2) 0.0082(3) -0.0007(3) S2 0.0597(15) 0.0465(13) 0.0447(13) 0.0010(10) 0.0127(11) 0.0033(11) N2 0.051(4) 0.045(4) 0.021(3) -0.001(3) 0.004(3) -0.002(3) C2 0.084(7) 0.044(5) 0.038(5) -0.011(4) -0.003(5) 0.005(5) Pd3 0.0472(4) 0.0408(4) 0.0265(3) -0.0005(3) 0.0074(3) 0.0015(3) S3 0.0691(17) 0.0838(19) 0.0419(13) 0.0136(13) -0.0023(12) 0.0044(14) N3 0.067(5) 0.043(4) 0.036(4) 0.013(3) -0.002(4) -0.010(4) C3 0.061(6) 0.050(5) 0.033(5) 0.003(4) 0.011(4) 0.016(4) S4 0.0723(19) 0.0633(18) 0.124(3) -0.0022(17) 0.0272(18) -0.0119(14) N4 0.058(5) 0.037(4) 0.035(4) -0.004(3) 0.014(3) -0.015(4) C4 0.060(6) 0.043(5) 0.032(4) -0.002(4) 0.014(4) 0.002(4) N5 0.041(4) 0.035(4) 0.034(4) -0.004(3) 0.008(3) 0.002(3) C5 0.049(5) 0.031(4) 0.028(4) 0.003(3) 0.005(4) 0.000(4) N6 0.048(4) 0.032(4) 0.032(4) -0.007(3) 0.012(3) -0.006(3) C6 0.071(6) 0.045(5) 0.033(4) -0.010(4) 0.013(4) 0.011(5) N7 0.046(4) 0.050(4) 0.032(4) 0.006(3) 0.006(3) 0.011(3) C7 0.075(6) 0.050(6) 0.037(5) 0.000(4) 0.032(4) 0.006(5) N8 0.045(4) 0.049(5) 0.053(5) 0.018(4) 0.011(3) 0.006(4) C8 0.048(5) 0.042(5) 0.028(4) 0.003(3) 0.003(4) 0.009(4) C9 0.049(5) 0.037(4) 0.029(4) 0.002(3) 0.011(4) 0.009(4) C10 0.041(5) 0.041(5) 0.031(4) 0.010(3) 0.010(3) 0.004(4) C11 0.047(5) 0.035(5) 0.038(5) 0.006(3) 0.004(4) 0.002(4) C12 0.051(5) 0.047(5) 0.038(5) 0.006(4) 0.011(4) 0.001(4) C13 0.049(5) 0.032(4) 0.048(5) -0.004(4) 0.010(4) -0.006(4) C14 0.071(6) 0.075(7) 0.033(5) 0.005(4) 0.020(4) -0.003(5) C15 0.060(6) 0.074(7) 0.041(5) 0.017(5) 0.006(4) -0.007(5) C16 0.096(9) 0.082(8) 0.040(6) 0.005(5) 0.008(6) -0.009(7) C17 0.081(7) 0.063(6) 0.023(4) 0.007(4) 0.008(4) -0.012(5) C18 0.073(7) 0.048(5) 0.032(5) -0.001(4) 0.012(4) -0.028(5) C19 0.065(6) 0.045(5) 0.025(4) 0.002(4) 0.005(4) -0.029(5) C20 0.077(7) 0.052(5) 0.023(4) -0.005(4) 0.017(4) -0.017(5) C21 0.059(6) 0.042(5) 0.052(6) -0.013(4) 0.019(4) -0.021(4) C22 0.059(6) 0.038(5) 0.028(4) 0.000(3) 0.011(4) -0.013(4) C23 0.047(5) 0.037(5) 0.049(5) -0.004(4) 0.015(4) -0.006(4) C24 0.057(5) 0.033(4) 0.034(4) -0.004(3) 0.018(4) -0.011(4) C25 0.061(6) 0.041(5) 0.032(4) 0.001(4) 0.002(4) -0.003(4) C26 0.060(6) 0.043(5) 0.037(5) -0.005(4) 0.017(4) -0.011(4) C27 0.076(6) 0.056(5) 0.027(4) -0.004(4) 0.008(4) 0.011(5) C28 0.068(6) 0.057(6) 0.055(6) -0.004(5) 0.027(5) 0.002(5) C29 0.055(5) 0.037(5) 0.046(5) 0.001(4) 0.013(4) -0.005(4) C30 0.060(6) 0.049(5) 0.055(6) 0.000(4) 0.020(5) 0.004(4) C31 0.055(6) 0.038(5) 0.055(6) -0.007(4) 0.025(5) -0.004(4) C32 0.048(5) 0.038(5) 0.047(5) -0.007(4) 0.016(4) -0.010(4) C33 0.045(5) 0.029(4) 0.039(5) -0.005(3) 0.019(4) -0.006(4) C34 0.077(7) 0.047(5) 0.042(5) -0.016(4) 0.032(5) -0.015(5) C35 0.063(6) 0.049(5) 0.036(5) -0.013(4) 0.016(4) -0.010(5) C36 0.061(6) 0.057(6) 0.030(5) -0.006(4) 0.014(4) -0.018(5) C37 0.052(5) 0.057(6) 0.028(4) 0.000(4) 0.006(4) -0.006(4) C38 0.046(5) 0.044(5) 0.039(5) 0.007(4) 0.006(4) -0.003(4) C39 0.062(6) 0.072(6) 0.035(5) 0.004(4) 0.010(4) -0.005(5) C40 0.065(6) 0.072(6) 0.031(5) -0.002(4) 0.000(4) -0.019(5) C41 0.060(6) 0.073(7) 0.055(6) 0.009(5) 0.003(5) 0.025(5) C42 0.086(7) 0.081(7) 0.021(4) -0.005(4) -0.002(4) -0.007(6) C43 0.062(6) 0.044(5) 0.042(5) -0.003(4) 0.007(4) 0.017(4) C44 0.070(7) 0.070(7) 0.057(6) -0.001(5) 0.006(5) 0.027(6) C45 0.081(8) 0.059(7) 0.062(6) 0.009(5) 0.031(6) 0.023(6) C46 0.056(6) 0.068(7) 0.057(6) 0.018(5) 0.015(5) 0.018(5) C47 0.053(6) 0.048(5) 0.044(5) 0.011(4) 0.014(4) 0.019(4) C48 0.062(7) 0.084(8) 0.069(7) 0.016(6) 0.019(5) 0.007(6) C49 0.056(7) 0.087(8) 0.077(8) 0.033(7) 0.027(6) 0.009(6) C50 0.049(6) 0.065(7) 0.069(7) 0.024(5) 0.008(5) 0.019(5) C51 0.064(7) 0.063(7) 0.065(7) 0.020(5) 0.017(5) 0.002(5) C52 0.086(8) 0.080(8) 0.085(8) 0.023(7) 0.001(6) -0.023(7) C53 0.106(9) 0.074(8) 0.083(8) 0.011(7) 0.030(7) -0.028(7) C54 0.043(6) 0.046(6) 0.100(8) 0.001(5) 0.011(5) -0.004(4) C55 0.166(14) 0.109(11) 0.128(12) 0.038(9) -0.006(10) -0.075(10) C56 0.106(9) 0.071(8) 0.103(9) -0.004(7) 0.056(8) -0.010(7) F1A 0.115(5) 0.096(5) 0.097(5) 0.024(4) 0.057(4) 0.026(4) B1A 0.099(11) 0.086(10) 0.061(8) 0.008(7) 0.036(8) 0.030(9) F2A 0.135(6) 0.107(5) 0.085(5) 0.033(4) 0.054(4) 0.041(5) B2A 0.071(8) 0.043(6) 0.044(6) -0.004(5) 0.004(6) 0.003(5) F3A 0.154(7) 0.163(8) 0.102(6) -0.041(5) 0.062(5) -0.002(6) B3A 0.105(10) 0.046(7) 0.034(6) -0.004(5) 0.005(6) 0.017(6) F4A 0.098(6) 0.183(8) 0.111(6) 0.057(6) 0.038(5) 0.033(5) F5A 0.099(4) 0.059(3) 0.067(4) 0.000(3) 0.006(3) 0.011(3) F6A 0.076(4) 0.071(4) 0.080(4) -0.014(3) -0.015(3) 0.015(3) F7A 0.072(4) 0.073(4) 0.077(4) 0.009(3) 0.010(3) -0.001(3) F8A 0.100(4) 0.054(4) 0.086(4) -0.001(3) 0.034(3) -0.001(3) F9A 0.100(4) 0.054(3) 0.049(3) 0.012(2) 0.024(3) 0.003(3) F10A 0.173(6) 0.052(3) 0.051(3) 0.006(3) 0.046(4) 0.018(4) F11A 0.246(9) 0.059(4) 0.069(4) -0.018(3) -0.017(5) -0.009(5) F12A 0.127(6) 0.170(8) 0.073(5) 0.025(5) 0.044(4) 0.044(5) O1W 0.071(4) 0.051(4) 0.045(3) 0.017(3) 0.013(3) 0.011(3) _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 C24 1.976(8) . ? Pd1 N1 2.026(6) . ? Pd1 N4 2.064(6) . ? Pd1 O1W 2.147(5) . ? Pd1 Pd2 2.8158(8) . ? S1 C12 1.704(8) . ? S1 C11 1.741(8) . ? N1 C1 1.338(9) . ? N1 C5 1.347(9) . ? C1 C2 1.388(11) . ? Pd2 C10 1.978(7) . ? Pd2 N5 2.018(6) . ? Pd2 N2 2.058(6) . ? Pd2 C24 2.517(8) . ? Pd2 Pd3 2.6750(8) . ? S2 C25 1.695(9) . ? S2 C26 1.726(8) . ? N2 C8 1.345(9) . ? N2 C5 1.357(9) . ? C2 C3 1.354(12) . ? Pd3 C38 1.963(8) . ? Pd3 N7 2.032(6) . ? Pd3 N6 2.032(6) . ? S3 C40 1.685(10) . ? S3 C39 1.749(8) . ? N3 C15 1.321(10) . ? N3 C19 1.356(11) . ? C3 C4 1.393(11) . ? S4 C53 1.695(12) . ? S4 C54 1.703(9) . ? N4 C22 1.307(10) . ? N4 C19 1.407(10) . ? C4 C6 1.383(11) . ? C4 C5 1.417(10) . ? N5 C29 1.339(10) . ? N5 C33 1.358(9) . ? N6 C33 1.355(9) . ? N6 C36 1.377(10) . ? C6 C7 1.355(11) . ? N7 C43 1.318(10) . ? N7 C47 1.365(10) . ? C7 C8 1.409(10) . ? N8 C50 1.341(11) . ? N8 C47 1.347(11) . ? C8 C9 1.435(11) . ? C9 C12 1.367(10) . ? C9 C10 1.451(10) . ? C10 C11 1.347(10) . ? C11 C13 1.507(10) . ? C12 C14 1.511(11) . ? C15 C16 1.382(13) . ? C16 C17 1.341(13) . ? C17 C18 1.425(12) . ? C18 C20 1.378(12) . ? C18 C19 1.445(11) . ? C20 C21 1.368(12) . ? C21 C22 1.435(11) . ? C22 C23 1.442(11) . ? C23 C26 1.352(11) . ? C23 C24 1.468(10) . ? C24 C25 1.375(11) . ? C25 C27 1.533(10) . ? C26 C28 1.503(11) . ? C29 C30 1.405(11) . ? C30 C31 1.340(11) . ? C31 C32 1.364(11) . ? C32 C33 1.425(10) . ? C32 C34 1.443(12) . ? C34 C35 1.311(12) . ? C35 C36 1.415(11) . ? C36 C37 1.458(12) . ? C37 C40 1.359(11) . ? C37 C38 1.424(11) . ? C38 C39 1.337(12) . ? C39 C41 1.510(12) . ? C40 C42 1.518(12) . ? C43 C44 1.393(12) . ? C44 C45 1.383(13) . ? C45 C46 1.374(13) . ? C46 C48 1.398(13) . ? C46 C47 1.439(12) . ? C48 C49 1.338(14) . ? C49 C50 1.466(14) . ? C50 C51 1.438(14) . ? C51 C54 1.392(14) . ? C51 C52 1.443(13) . ? C52 C53 1.374(15) . ? C53 C55 1.510(15) . ? C54 C56 1.483(14) . ? F1A B1A 1.397(14) . ? B1A F3A 1.337(14) . ? B1A F2A 1.363(15) . ? B1A F4A 1.442(16) . ? B2A F6A 1.364(12) . ? B2A F8A 1.376(12) . ? B2A F7A 1.383(12) . ? B2A F5A 1.386(11) . ? B3A F11A 1.310(12) . ? B3A F9A 1.363(12) . ? B3A F12A 1.388(14) . ? B3A F10A 1.394(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Pd1 N1 95.6(3) . . ? C24 Pd1 N4 81.8(3) . . ? N1 Pd1 N4 176.6(3) . . ? C24 Pd1 O1W 176.4(3) . . ? N1 Pd1 O1W 84.8(2) . . ? N4 Pd1 O1W 97.6(3) . . ? C24 Pd1 Pd2 60.4(2) . . ? N1 Pd1 Pd2 83.64(17) . . ? N4 Pd1 Pd2 96.98(17) . . ? O1W Pd1 Pd2 123.26(16) . . ? C12 S1 C11 93.3(4) . . ? C1 N1 C5 119.0(7) . . ? C1 N1 Pd1 115.3(5) . . ? C5 N1 Pd1 124.8(5) . . ? N1 C1 C2 123.6(8) . . ? C10 Pd2 N5 91.0(3) . . ? C10 Pd2 N2 82.8(3) . . ? N5 Pd2 N2 173.0(2) . . ? C10 Pd2 C24 166.1(3) . . ? N5 Pd2 C24 85.1(2) . . ? N2 Pd2 C24 100.1(2) . . ? C10 Pd2 Pd3 77.8(2) . . ? N5 Pd2 Pd3 84.62(18) . . ? N2 Pd2 Pd3 97.27(17) . . ? C24 Pd2 Pd3 114.98(18) . . ? C10 Pd2 Pd1 150.2(2) . . ? N5 Pd2 Pd1 106.21(18) . . ? N2 Pd2 Pd1 80.81(18) . . ? C24 Pd2 Pd1 43.06(18) . . ? Pd3 Pd2 Pd1 79.82(2) . . ? C25 S2 C26 93.5(4) . . ? C8 N2 C5 119.8(7) . . ? C8 N2 Pd2 113.2(5) . . ? C5 N2 Pd2 126.9(5) . . ? C3 C2 C1 118.3(8) . . ? C38 Pd3 N7 97.0(3) . . ? C38 Pd3 N6 82.0(3) . . ? N7 Pd3 N6 176.1(3) . . ? C38 Pd3 Pd2 159.7(2) . . ? N7 Pd3 Pd2 98.04(17) . . ? N6 Pd3 Pd2 83.84(18) . . ? C40 S3 C39 93.5(4) . . ? C15 N3 C19 117.8(8) . . ? C2 C3 C4 119.7(8) . . ? C53 S4 C54 94.7(6) . . ? C22 N4 C19 121.0(7) . . ? C22 N4 Pd1 115.0(5) . . ? C19 N4 Pd1 124.0(6) . . ? C6 C4 C3 123.3(8) . . ? C6 C4 C5 117.3(7) . . ? C3 C4 C5 119.4(7) . . ? C29 N5 C33 120.0(7) . . ? C29 N5 Pd2 115.3(5) . . ? C33 N5 Pd2 124.5(5) . . ? N1 C5 N2 118.8(7) . . ? N1 C5 C4 119.8(7) . . ? N2 C5 C4 121.3(7) . . ? C33 N6 C36 119.2(7) . . ? C33 N6 Pd3 124.9(5) . . ? C36 N6 Pd3 115.4(6) . . ? C7 C6 C4 121.6(8) . . ? C43 N7 C47 119.4(7) . . ? C43 N7 Pd3 124.7(6) . . ? C47 N7 Pd3 114.9(5) . . ? C6 C7 C8 119.0(8) . . ? C50 N8 C47 116.8(8) . . ? N2 C8 C7 121.0(7) . . ? N2 C8 C9 114.5(7) . . ? C7 C8 C9 124.4(7) . . ? C12 C9 C8 129.8(7) . . ? C12 C9 C10 112.5(7) . . ? C8 C9 C10 117.7(7) . . ? C11 C10 C9 113.3(7) . . ? C11 C10 Pd2 136.3(6) . . ? C9 C10 Pd2 109.9(6) . . ? C10 C11 C13 134.9(7) . . ? C10 C11 S1 110.0(6) . . ? C13 C11 S1 115.0(6) . . ? C9 C12 C14 131.4(8) . . ? C9 C12 S1 110.8(6) . . ? C14 C12 S1 117.8(6) . . ? N3 C15 C16 123.0(10) . . ? C17 C16 C15 120.9(10) . . ? C16 C17 C18 120.1(9) . . ? C20 C18 C17 126.7(8) . . ? C20 C18 C19 118.4(8) . . ? C17 C18 C19 114.8(9) . . ? N3 C19 N4 117.9(7) . . ? N3 C19 C18 123.2(8) . . ? N4 C19 C18 118.8(8) . . ? C21 C20 C18 121.4(8) . . ? C20 C21 C22 118.9(8) . . ? N4 C22 C21 121.4(8) . . ? N4 C22 C23 115.4(7) . . ? C21 C22 C23 123.2(8) . . ? C26 C23 C22 130.9(8) . . ? C26 C23 C24 113.2(7) . . ? C22 C23 C24 115.9(7) . . ? C25 C24 C23 110.9(7) . . ? C25 C24 Pd1 136.6(6) . . ? C23 C24 Pd1 111.2(6) . . ? C25 C24 Pd2 95.8(5) . . ? C23 C24 Pd2 113.4(5) . . ? Pd1 C24 Pd2 76.6(3) . . ? C24 C25 C27 131.6(8) . . ? C24 C25 S2 111.8(6) . . ? C27 C25 S2 116.7(6) . . ? C23 C26 C28 133.0(8) . . ? C23 C26 S2 110.4(6) . . ? C28 C26 S2 116.6(7) . . ? N5 C29 C30 121.4(8) . . ? C31 C30 C29 118.8(8) . . ? C30 C31 C32 121.4(8) . . ? C31 C32 C33 118.9(8) . . ? C31 C32 C34 125.8(8) . . ? C33 C32 C34 115.3(8) . . ? N6 C33 N5 117.9(6) . . ? N6 C33 C32 122.9(7) . . ? N5 C33 C32 119.2(7) . . ? C35 C34 C32 121.2(8) . . ? C34 C35 C36 121.6(8) . . ? N6 C36 C35 119.5(8) . . ? N6 C36 C37 112.3(7) . . ? C35 C36 C37 128.3(8) . . ? C40 C37 C38 115.0(8) . . ? C40 C37 C36 128.2(8) . . ? C38 C37 C36 116.8(7) . . ? C39 C38 C37 112.0(7) . . ? C39 C38 Pd3 134.6(7) . . ? C37 C38 Pd3 113.3(6) . . ? C38 C39 C41 132.7(8) . . ? C38 C39 S3 110.0(7) . . ? C41 C39 S3 117.2(7) . . ? C37 C40 C42 131.2(9) . . ? C37 C40 S3 109.4(7) . . ? C42 C40 S3 119.4(7) . . ? N7 C43 C44 123.0(9) . . ? C45 C44 C43 118.4(10) . . ? C46 C45 C44 120.8(9) . . ? C45 C46 C48 126.1(10) . . ? C45 C46 C47 117.5(9) . . ? C48 C46 C47 116.4(10) . . ? N8 C47 N7 115.3(7) . . ? N8 C47 C46 124.0(8) . . ? N7 C47 C46 120.6(8) . . ? C49 C48 C46 122.1(10) . . ? C48 C49 C50 117.4(10) . . ? N8 C50 C51 117.1(9) . . ? N8 C50 C49 123.3(10) . . ? C51 C50 C49 119.6(10) . . ? C54 C51 C50 126.5(9) . . ? C54 C51 C52 112.5(10) . . ? C50 C51 C52 121.1(10) . . ? C53 C52 C51 112.4(11) . . ? C52 C53 C55 128.0(12) . . ? C52 C53 S4 110.7(8) . . ? C55 C53 S4 121.3(10) . . ? C51 C54 C56 130.2(9) . . ? C51 C54 S4 109.7(8) . . ? C56 C54 S4 120.1(9) . . ? F3A B1A F2A 112.0(11) . . ? F3A B1A F1A 113.1(13) . . ? F2A B1A F1A 111.6(10) . . ? F3A B1A F4A 108.1(10) . . ? F2A B1A F4A 104.7(12) . . ? F1A B1A F4A 106.7(10) . . ? F6A B2A F8A 108.5(8) . . ? F6A B2A F7A 109.7(8) . . ? F8A B2A F7A 109.4(8) . . ? F6A B2A F5A 109.9(8) . . ? F8A B2A F5A 109.4(8) . . ? F7A B2A F5A 110.0(8) . . ? F11A B3A F9A 116.0(11) . . ? F11A B3A F12A 106.7(10) . . ? F9A B3A F12A 107.9(8) . . ? F11A B3A F10A 110.1(9) . . ? F9A B3A F10A 109.9(8) . . ? F12A B3A F10A 105.6(10) . . ? 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 0.206 0.750 0.004 416 198 ' ' 2 0.794 0.250 0.010 416 197 ' ' _platon_squeeze_details ; PLATON/SQUEEZE estimated the solvent-accessible region to contain 395 (198+197) electrons per unit cell. This amounts to nearly 99 electrons per formula unit. The electron densities are tentatively modelled as to two CH2Cl2 and one H2O molecules per formula unit. These solvent and water molecules are included in the formula sum for the calculation of the intensive properties. ; _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.992 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.151 _iucr_refine_instructions_details ; TITL _compound_2 CELL 0.71073 19.4846 22.6280 14.2391 90.000 100.457 90.000 ZERR 4.0000 0.0022 0.0026 0.0016 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O PD B F S UNIT 224 180 32 4 12 12 48 16 MERG 2 SHEL 99999.00 0.85 FMAP 2 GRID PLAN 2 TEMP -173 SIZE 0.21 0.23 0.31 L.S. 5 ACTA WGHT 0.09520 0.00000 0.00000 0.00000 0.00000 0.33330 FVAR 1.38480 Pd1 5 0.38358 0.51849 0.16237 11.00000 0.06045 0.03553 = 0.02491 -0.00061 0.00873 -0.00808 S1 8 0.18252 0.29102 0.33350 11.00000 0.05532 0.04107 = 0.04733 0.01076 0.01769 0.00022 N1 3 0.37666 0.55071 0.29305 11.00000 0.05609 0.02815 = 0.03298 -0.00164 0.00306 -0.00520 C1 1 0.40344 0.60477 0.31215 11.00000 0.05582 0.04124 = 0.03907 -0.00330 0.00403 -0.00658 AFIX 43 H1 2 0.43102 0.62113 0.27003 11.00000 -1.20000 AFIX 0 Pd2 5 0.33863 0.41258 0.23556 11.00000 0.04897 0.03117 = 0.02406 -0.00033 0.00816 -0.00066 S2 8 0.55208 0.38851 0.28383 11.00000 0.05967 0.04652 = 0.04473 0.00098 0.01272 0.00328 N2 3 0.31365 0.47066 0.33533 11.00000 0.05083 0.04544 = 0.02140 -0.00102 0.00380 -0.00205 C2 1 0.39315 0.63822 0.39009 11.00000 0.08379 0.04432 = 0.03785 -0.01135 -0.00334 0.00533 AFIX 43 H2 2 0.41438 0.67592 0.40210 11.00000 -1.20000 AFIX 0 Pd3 5 0.22920 0.43549 0.09756 11.00000 0.04720 0.04081 = 0.02645 -0.00051 0.00741 0.00149 S3 8 0.09822 0.48794 -0.18345 11.00000 0.06910 0.08377 = 0.04187 0.01356 -0.00234 0.00441 N3 3 0.30680 0.54411 -0.05503 11.00000 0.06684 0.04349 = 0.03614 0.01257 -0.00153 -0.00976 C3 1 0.35210 0.61579 0.44859 11.00000 0.06094 0.04974 = 0.03335 0.00263 0.01141 0.01590 AFIX 43 H3 2 0.34231 0.63849 0.50071 11.00000 -1.20000 AFIX 0 S4 8 0.01121 0.22870 0.03281 11.00000 0.07230 0.06334 = 0.12379 -0.00219 0.02721 -0.01185 N4 3 0.39701 0.48526 0.03195 11.00000 0.05838 0.03695 = 0.03524 -0.00394 0.01383 -0.01522 C4 1 0.32430 0.55925 0.43198 11.00000 0.06004 0.04324 = 0.03237 -0.00153 0.01432 0.00196 N5 3 0.35919 0.34768 0.14748 11.00000 0.04110 0.03452 = 0.03388 -0.00403 0.00780 0.00156 C5 1 0.33852 0.52635 0.35299 11.00000 0.04908 0.03118 = 0.02780 0.00299 0.00491 0.00009 N6 3 0.28040 0.38297 0.01727 11.00000 0.04824 0.03199 = 0.03182 -0.00694 0.01186 -0.00565 C6 1 0.28188 0.53316 0.48816 11.00000 0.07131 0.04499 = 0.03265 -0.00988 0.01250 0.01130 AFIX 43 H6 2 0.27092 0.55434 0.54112 11.00000 -1.20000 AFIX 0 N7 3 0.17252 0.48394 0.17630 11.00000 0.04592 0.04951 = 0.03218 0.00607 0.00568 0.01068 C7 1 0.25556 0.47809 0.46951 11.00000 0.07467 0.05002 = 0.03701 0.00001 0.03172 0.00597 AFIX 43 H7 2 0.22641 0.46085 0.50877 11.00000 -1.20000 AFIX 0 N8 3 0.10355 0.40132 0.16483 11.00000 0.04502 0.04874 = 0.05279 0.01780 0.01085 0.00583 C8 1 0.27208 0.44680 0.39102 11.00000 0.04753 0.04180 = 0.02780 0.00308 0.00277 0.00898 C9 1 0.24514 0.38944 0.36118 11.00000 0.04914 0.03664 = 0.02869 0.00248 0.01142 0.00893 C10 1 0.26409 0.36456 0.27552 11.00000 0.04113 0.04110 = 0.03064 0.00953 0.00975 0.00352 C11 1 0.23314 0.31227 0.25032 11.00000 0.04694 0.03493 = 0.03795 0.00644 0.00425 0.00250 C12 1 0.20235 0.35299 0.40101 11.00000 0.05125 0.04652 = 0.03847 0.00620 0.01143 0.00123 C13 1 0.23057 0.27081 0.16692 11.00000 0.04946 0.03185 = 0.04751 -0.00358 0.00957 -0.00624 AFIX 137 H13A 2 0.21921 0.29314 0.10714 11.00000 -1.50000 H13B 2 0.19474 0.24066 0.16884 11.00000 -1.50000 H13C 2 0.27609 0.25167 0.17055 11.00000 -1.50000 AFIX 0 C14 1 0.17236 0.35863 0.49130 11.00000 0.07053 0.07526 = 0.03302 0.00459 0.01975 -0.00329 AFIX 137 H14A 2 0.20943 0.36998 0.54436 11.00000 -1.50000 H14B 2 0.15240 0.32066 0.50570 11.00000 -1.50000 H14C 2 0.13579 0.38891 0.48240 11.00000 -1.50000 AFIX 0 C15 1 0.26879 0.55993 -0.13767 11.00000 0.06030 0.07357 = 0.04106 0.01706 0.00587 -0.00730 AFIX 43 H15 2 0.23267 0.58812 -0.13762 11.00000 -1.20000 AFIX 0 C16 1 0.27914 0.53736 -0.22423 11.00000 0.09578 0.08212 = 0.03994 0.00453 0.00841 -0.00935 AFIX 43 H16 2 0.24937 0.54939 -0.28143 11.00000 -1.20000 AFIX 0 C17 1 0.33066 0.49870 -0.22852 11.00000 0.08140 0.06317 = 0.02255 0.00728 0.00799 -0.01175 AFIX 43 H17 2 0.33777 0.48420 -0.28863 11.00000 -1.20000 AFIX 0 C18 1 0.37476 0.47933 -0.14312 11.00000 0.07304 0.04826 = 0.03192 -0.00072 0.01160 -0.02826 C19 1 0.35793 0.50357 -0.05615 11.00000 0.06522 0.04540 = 0.02511 0.00209 0.00466 -0.02917 C20 1 0.42722 0.43783 -0.13591 11.00000 0.07708 0.05178 = 0.02266 -0.00488 0.01660 -0.01686 AFIX 43 H20 2 0.43881 0.42148 -0.19248 11.00000 -1.20000 AFIX 0 C21 1 0.46296 0.41967 -0.04907 11.00000 0.05928 0.04234 = 0.05162 -0.01285 0.01946 -0.02087 AFIX 43 H21 2 0.49843 0.39049 -0.04512 11.00000 -1.20000 AFIX 0 C22 1 0.44603 0.44539 0.03597 11.00000 0.05929 0.03801 = 0.02752 -0.00029 0.01150 -0.01312 C23 1 0.47985 0.42864 0.13080 11.00000 0.04689 0.03730 = 0.04932 -0.00443 0.01455 -0.00587 C24 1 0.45247 0.45631 0.20962 11.00000 0.05697 0.03265 = 0.03444 -0.00350 0.01782 -0.01083 C25 1 0.49037 0.43925 0.29642 11.00000 0.06112 0.04109 = 0.03197 0.00115 0.00210 -0.00316 C26 1 0.53294 0.39066 0.16067 11.00000 0.06050 0.04320 = 0.03703 -0.00503 0.01651 -0.01120 C27 1 0.48590 0.45776 0.39867 11.00000 0.07584 0.05607 = 0.02654 -0.00402 0.00758 0.01076 AFIX 137 H27C 2 0.49024 0.50081 0.40451 11.00000 -1.50000 H27A 2 0.52374 0.43895 0.44343 11.00000 -1.50000 H27B 2 0.44085 0.44536 0.41345 11.00000 -1.50000 AFIX 0 C28 1 0.57546 0.35116 0.10859 11.00000 0.06802 0.05694 = 0.05536 -0.00414 0.02694 0.00185 AFIX 137 H28A 2 0.54526 0.32072 0.07380 11.00000 -1.50000 H28B 2 0.61245 0.33229 0.15465 11.00000 -1.50000 H28C 2 0.59639 0.37471 0.06337 11.00000 -1.50000 AFIX 0 C29 1 0.40568 0.30730 0.18747 11.00000 0.05467 0.03711 = 0.04617 0.00066 0.01275 -0.00459 AFIX 43 H29 2 0.42134 0.30777 0.25466 11.00000 -1.20000 AFIX 0 C30 1 0.43180 0.26424 0.13215 11.00000 0.06035 0.04919 = 0.05479 0.00043 0.01981 0.00407 AFIX 43 H30 2 0.46493 0.23592 0.16133 11.00000 -1.20000 AFIX 0 C31 1 0.40915 0.26384 0.03751 11.00000 0.05542 0.03800 = 0.05518 -0.00655 0.02546 -0.00441 AFIX 43 H31 2 0.42761 0.23564 -0.00063 11.00000 -1.20000 AFIX 0 C32 1 0.36011 0.30310 -0.00522 11.00000 0.04773 0.03822 = 0.04658 -0.00702 0.01553 -0.01016 C33 1 0.33253 0.34506 0.05262 11.00000 0.04462 0.02877 = 0.03871 -0.00499 0.01858 -0.00637 C34 1 0.33171 0.30606 -0.10604 11.00000 0.07655 0.04651 = 0.04152 -0.01621 0.03195 -0.01474 AFIX 43 H34 2 0.34837 0.27959 -0.14858 11.00000 -1.20000 AFIX 0 C35 1 0.28331 0.34465 -0.13997 11.00000 0.06268 0.04914 = 0.03553 -0.01262 0.01590 -0.00988 AFIX 43 H35 2 0.26808 0.34749 -0.20708 11.00000 -1.20000 AFIX 0 C36 1 0.25323 0.38215 -0.07897 11.00000 0.06080 0.05683 = 0.03003 -0.00555 0.01404 -0.01773 C37 1 0.19578 0.42380 -0.10452 11.00000 0.05189 0.05716 = 0.02803 0.00011 0.00619 -0.00625 C38 1 0.17584 0.45659 -0.02845 11.00000 0.04566 0.04411 = 0.03923 0.00693 0.00585 -0.00256 C39 1 0.12341 0.49392 -0.05953 11.00000 0.06209 0.07201 = 0.03453 0.00395 0.01024 -0.00537 C40 1 0.15774 0.43522 -0.19244 11.00000 0.06531 0.07219 = 0.03062 -0.00193 0.00009 -0.01872 C41 1 0.08557 0.53890 -0.00936 11.00000 0.05956 0.07276 = 0.05539 0.00907 0.00291 0.02453 AFIX 137 H41B 2 0.06338 0.51898 0.03845 11.00000 -1.50000 H41C 2 0.04982 0.55865 -0.05616 11.00000 -1.50000 H41A 2 0.11896 0.56827 0.02219 11.00000 -1.50000 AFIX 0 C42 1 0.16182 0.40958 -0.28979 11.00000 0.08640 0.08094 = 0.02127 -0.00498 -0.00177 -0.00747 AFIX 137 H42A 2 0.20725 0.41914 -0.30625 11.00000 -1.50000 H42C 2 0.12458 0.42649 -0.33783 11.00000 -1.50000 H42B 2 0.15626 0.36657 -0.28815 11.00000 -1.50000 AFIX 0 C43 1 0.18974 0.53712 0.21049 11.00000 0.06195 0.04370 = 0.04172 -0.00283 0.00719 0.01655 AFIX 43 H43 2 0.22375 0.55880 0.18473 11.00000 -1.20000 AFIX 0 C44 1 0.16033 0.56298 0.28267 11.00000 0.07040 0.06982 = 0.05713 -0.00110 0.00576 0.02690 AFIX 43 H44 2 0.17415 0.60133 0.30590 11.00000 -1.20000 AFIX 0 C45 1 0.11052 0.53149 0.31971 11.00000 0.08075 0.05898 = 0.06199 0.00917 0.03058 0.02311 AFIX 43 H45 2 0.09075 0.54800 0.37006 11.00000 -1.20000 AFIX 0 C46 1 0.08931 0.47662 0.28452 11.00000 0.05556 0.06770 = 0.05665 0.01845 0.01474 0.01789 C47 1 0.12052 0.45366 0.20789 11.00000 0.05256 0.04798 = 0.04410 0.01059 0.01371 0.01870 C48 1 0.03904 0.44101 0.31511 11.00000 0.06250 0.08430 = 0.06880 0.01641 0.01886 0.00693 AFIX 43 H48 2 0.01747 0.45448 0.36587 11.00000 -1.20000 AFIX 0 C49 1 0.02034 0.38854 0.27517 11.00000 0.05601 0.08737 = 0.07737 0.03274 0.02726 0.00875 AFIX 43 H49 2 -0.01337 0.36444 0.29726 11.00000 -1.20000 AFIX 0 C50 1 0.05394 0.36969 0.19597 11.00000 0.04856 0.06483 = 0.06852 0.02402 0.00759 0.01879 C51 1 0.03495 0.31411 0.14955 11.00000 0.06418 0.06318 = 0.06509 0.02002 0.01703 0.00170 C52 1 0.00828 0.26624 0.19948 11.00000 0.08614 0.07991 = 0.08486 0.02261 0.00071 -0.02308 AFIX 43 H52 2 0.00097 0.26886 0.26352 11.00000 -1.20000 AFIX 0 C53 1 -0.00534 0.21644 0.14399 11.00000 0.10628 0.07429 = 0.08344 0.01146 0.02970 -0.02794 C54 1 0.03921 0.29942 0.05586 11.00000 0.04262 0.04576 = 0.09977 0.00129 0.01087 -0.00424 C55 1 -0.03120 0.15719 0.17178 11.00000 0.16612 0.10923 = 0.12819 0.03818 -0.00562 -0.07520 AFIX 137 H55A 2 0.00633 0.12796 0.17576 11.00000 -1.50000 H55B 2 -0.07106 0.14465 0.12363 11.00000 -1.50000 H55C 2 -0.04566 0.16051 0.23400 11.00000 -1.50000 AFIX 0 C56 1 0.06222 0.33521 -0.01997 11.00000 0.10577 0.07134 = 0.10341 -0.00403 0.05569 -0.01029 AFIX 137 H56A 2 0.03844 0.37354 -0.02484 11.00000 -1.50000 H56B 2 0.05065 0.31438 -0.08115 11.00000 -1.50000 H56C 2 0.11279 0.34136 -0.00406 11.00000 -1.50000 AFIX 0 F1A 7 0.16346 0.62249 0.51493 11.00000 0.11484 0.09624 = 0.09702 0.02368 0.05675 0.02586 B1A 6 0.12622 0.59285 0.57559 11.00000 0.09874 0.08615 = 0.06071 0.00785 0.03603 0.03041 F2A 7 0.14378 0.53451 0.58396 11.00000 0.13478 0.10652 = 0.08491 0.03286 0.05373 0.04129 B2A 6 0.38874 0.38922 0.59949 11.00000 0.07110 0.04311 = 0.04409 -0.00402 0.00388 0.00333 F3A 7 0.13073 0.61899 0.66069 11.00000 0.15370 0.16333 = 0.10186 -0.04081 0.06246 -0.00229 B3A 6 0.56451 0.23045 0.36729 11.00000 0.10460 0.04589 = 0.03421 -0.00398 0.00471 0.01679 F4A 7 0.05398 0.59316 0.52921 11.00000 0.09777 0.18324 = 0.11108 0.05668 0.03774 0.03320 F5A 7 0.38397 0.36570 0.50863 11.00000 0.09948 0.05869 = 0.06655 0.00050 0.00594 0.01148 F6A 7 0.44624 0.36723 0.65812 11.00000 0.07590 0.07118 = 0.08017 -0.01383 -0.01514 0.01534 F7A 7 0.32953 0.37531 0.63573 11.00000 0.07232 0.07300 = 0.07721 0.00930 0.00990 -0.00101 F8A 7 0.39523 0.44968 0.59531 11.00000 0.09963 0.05402 = 0.08590 -0.00125 0.03438 -0.00092 F9A 7 0.57963 0.24508 0.28043 11.00000 0.10043 0.05359 = 0.04948 0.01163 0.02402 0.00292 F10A 7 0.57971 0.17102 0.38659 11.00000 0.17311 0.05167 = 0.05113 0.00583 0.04595 0.01832 F11A 7 0.59386 0.26314 0.43938 11.00000 0.24552 0.05876 = 0.06852 -0.01796 -0.01708 -0.00935 F12A 7 0.49291 0.23573 0.36177 11.00000 0.12738 0.16973 = 0.07270 0.02526 0.04414 0.04363 O1W 4 0.31419 0.58956 0.10967 11.00000 0.07144 0.05102 = 0.04530 0.01674 0.01317 0.01085 HKLF 4 ; _database_code_depnum_ccdc_archive 'CCDC 940019' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H46 Br N8 O Pd3 S4, 2.5(C6 H6), 3(B F4)' _chemical_formula_sum 'C71 H61 B3 Br F12 N8 O Pd3 S4' _chemical_formula_weight 1830.14 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.464(4) _cell_length_b 22.228(4) _cell_length_c 25.760(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.596(4) _cell_angle_gamma 90.00 _cell_volume 12643(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9957 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 24.32 _exptl_crystal_description neddle _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.92 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7288 _exptl_absorpt_coefficient_mu 1.692 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6770 _exptl_absorpt_correction_T_max 0.7735 _exptl_absorpt_process_details SADABS _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 '\f and \w scans' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37413 _diffrn_reflns_av_R_equivalents 0.1189 _diffrn_reflns_av_sigmaI/netI 0.2471 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 24.71 _reflns_number_total 20264 _reflns_number_gt 8979 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ciftab _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. All H-atoms except those of water molecules were introduced into geometrically calculated positions in the final stages of the refinement and were refined according to 'riding model'. H-atoms of the water molecules were not located, but were included in the formula sum. SADI and DFIX restraints were applied to model one of the BF4 and the associated atoms were refined isotropically. Anisotropic treatment of C30, C31, C33, C60, C111, C112, N12 atoms in the main residue and B4A, F16A in the anion resulted in non-positive definite displacement tensors, and were therefore subjected to isotropic refinement. Please see iucr_refine_instructions_details for full information. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20264 _refine_ls_number_parameters 1585 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1871 _refine_ls_R_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.2092 _refine_ls_wR_factor_gt 0.1776 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.005 _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 0.25277(4) 0.93245(5) 0.30808(5) 0.027 Uani 1 1 d . . . Br1 Br 0.49734(6) 0.53218(7) 0.33981(7) 0.040 Uani 1 1 d . . . S1 S 0.47161(15) 0.70064(17) 0.30169(15) 0.028 Uani 1 1 d . . . N1 N 0.3181(5) 0.9595(5) 0.3677(5) 0.030 Uani 1 1 d . . . C1 C 0.3084(6) 1.0097(8) 0.3934(7) 0.051 Uani 1 1 d . . . H1 H 0.2763 1.0349 0.3768 0.061 Uiso 1 1 calc R . . Pd2 Pd 0.34445(4) 0.86001(5) 0.28226(4) 0.023 Uani 1 1 d . . . Br2 Br 0.51239(6) 0.79882(7) 0.12971(6) 0.031 Uani 1 1 d . . . S2 S 0.34598(17) 1.01865(19) 0.18558(19) 0.045 Uani 1 1 d . . . N2 N 0.3795(4) 0.8763(5) 0.3606(4) 0.020 Uani 1 1 d . . . C2 C 0.3416(8) 1.0298(8) 0.4438(8) 0.062 Uani 1 1 d . . . H2 H 0.3325 1.0662 0.4599 0.074 Uiso 1 1 calc R . . Pd3 Pd 0.26836(4) 0.76829(5) 0.29264(4) 0.023 Uani 1 1 d . . . S3 S 0.09334(17) 0.66499(18) 0.28391(19) 0.045 Uani 1 1 d . . . N3 N 0.1239(5) 0.8613(5) 0.2958(4) 0.025 Uani 1 1 d . . . C3 C 0.3852(7) 0.9937(8) 0.4655(7) 0.057 Uani 1 1 d . . . H3 H 0.4079 1.0038 0.4992 0.068 Uiso 1 1 calc R . . Pd4 Pd 0.77216(4) 0.41382(5) 0.21486(4) 0.021 Uani 1 1 d . . . S4 S 0.35450(16) 0.54271(17) 0.20086(15) 0.029 Uani 1 1 d . . . N4 N 0.1861(4) 0.9127(5) 0.2454(5) 0.026 Uani 1 1 d . . . C4 C 0.4004(7) 0.9384(8) 0.4397(8) 0.060 Uani 1 1 d . . . Pd5 Pd 0.67719(5) 0.48697(5) 0.22701(4) 0.026 Uani 1 1 d . . . S5 S 0.54454(14) 0.64170(16) 0.20333(15) 0.025 Uani 1 1 d . . . N5 N 0.3204(5) 0.8408(5) 0.2043(5) 0.032 Uani 1 1 d . . . C5 C 0.3644(6) 0.9232(7) 0.3904(6) 0.032 Uani 1 1 d . . . Pd6 Pd 0.75458(5) 0.57728(5) 0.22072(5) 0.029 Uani 1 1 d . . . S6 S 0.64069(15) 0.31698(17) 0.29920(15) 0.031 Uani 1 1 d . . . N6 N 0.2381(4) 0.7827(4) 0.2137(4) 0.020 Uani 1 1 d . . . C6 C 0.4466(7) 0.8952(8) 0.4635(7) 0.060 Uani 1 1 d . . . H6 H 0.4684 0.9007 0.4984 0.072 Uiso 1 1 calc R . . S7 S 0.93039(17) 0.67978(19) 0.24117(19) 0.050 Uani 1 1 d . . . N7 N 0.2969(4) 0.7480(5) 0.3704(4) 0.022 Uani 1 1 d . . . C7 C 0.4573(7) 0.8467(8) 0.4340(6) 0.047 Uani 1 1 d . . . H7 H 0.4880 0.8187 0.4480 0.056 Uiso 1 1 calc R . . S8 S 0.63417(15) 0.80245(16) 0.28162(15) 0.026 Uani 1 1 d . . . N8 N 0.3365(4) 0.6608(5) 0.3379(4) 0.022 Uani 1 1 d . . . C8 C 0.4230(6) 0.8379(6) 0.3824(6) 0.034 Uani 1 1 d . . . N9 N 0.7203(4) 0.3962(5) 0.1427(4) 0.019 Uani 1 1 d . . . C9 C 0.4344(6) 0.7890(6) 0.3477(5) 0.023 Uani 1 1 d . . . N10 N 0.6514(4) 0.4752(5) 0.1471(4) 0.019 Uani 1 1 d . . . C10 C 0.3971(5) 0.7882(6) 0.2955(5) 0.023 Uani 1 1 d . . . N11 N 0.8983(4) 0.4849(5) 0.2632(4) 0.022 Uani 1 1 d . . . C11 C 0.4111(5) 0.7409(6) 0.2650(6) 0.022 Uani 1 1 d . . . N12 N 0.8222(4) 0.4248(5) 0.2897(4) 0.020 Uiso 1 1 d . . . C12 C 0.4786(5) 0.7462(6) 0.3561(6) 0.033 Uani 1 1 d . . . N13 N 0.6927(6) 0.5037(5) 0.3059(5) 0.040 Uani 1 1 d . . . C13 C 0.3877(5) 0.7177(6) 0.2111(5) 0.029 Uani 1 1 d . . . H13A H 0.3440 0.7107 0.2069 0.043 Uiso 1 1 calc R . . H13B H 0.4081 0.6798 0.2058 0.043 Uiso 1 1 calc R . . H13C H 0.3955 0.7472 0.1849 0.043 Uiso 1 1 calc R . . N14 N 0.7755(5) 0.5653(5) 0.3022(5) 0.035 Uani 1 1 d . . . C14 C 0.5280(6) 0.7317(6) 0.4039(5) 0.036 Uani 1 1 d . . . H14A H 0.5515 0.7681 0.4151 0.054 Uiso 1 1 calc R . . H14B H 0.5549 0.7006 0.3942 0.054 Uiso 1 1 calc R . . H14C H 0.5092 0.7171 0.4330 0.054 Uiso 1 1 calc R . . N15 N 0.7363(4) 0.5929(4) 0.1410(4) 0.019 Uani 1 1 d . . . C15 C 0.0746(6) 0.8301(6) 0.2983(6) 0.026 Uani 1 1 d . . . H15 H 0.0697 0.8148 0.3317 0.031 Uiso 1 1 calc R . . N16 N 0.6838(4) 0.6765(5) 0.1611(4) 0.020 Uani 1 1 d . . . C16 C 0.0300(6) 0.8184(6) 0.2557(6) 0.032 Uani 1 1 d . . . H16 H -0.0046 0.7956 0.2600 0.039 Uiso 1 1 calc R . . C17 C 0.0354(6) 0.8395(6) 0.2073(6) 0.033 Uani 1 1 d . . . H17 H 0.0043 0.8320 0.1777 0.039 Uiso 1 1 calc R . . C18 C 0.0877(6) 0.8728(6) 0.2010(6) 0.024 Uani 1 1 d . . . C19 C 0.1318(5) 0.8810(6) 0.2487(5) 0.020 Uani 1 1 d . . . C20 C 0.0985(6) 0.8947(6) 0.1522(6) 0.034 Uani 1 1 d . . . H20 H 0.0691 0.8886 0.1211 0.041 Uiso 1 1 calc R . . C21 C 0.1497(6) 0.9240(6) 0.1494(6) 0.031 Uani 1 1 d . . . H21 H 0.1571 0.9390 0.1167 0.038 Uiso 1 1 calc R . . C22 C 0.1938(5) 0.9322(6) 0.1974(6) 0.024 Uani 1 1 d . . . C23 C 0.2531(6) 0.9638(6) 0.2007(6) 0.033 Uani 1 1 d . . . C24 C 0.2924(6) 0.9615(6) 0.2518(6) 0.035 Uani 1 1 d . . . C25 C 0.3467(6) 0.9922(6) 0.2488(7) 0.040 Uani 1 1 d . . . C26 C 0.2760(6) 0.9918(6) 0.1592(7) 0.049 Uani 1 1 d . . . C27 C 0.4008(6) 1.0097(7) 0.2898(6) 0.043 Uani 1 1 d . . . H27A H 0.3892 1.0418 0.3120 0.064 Uiso 1 1 calc R . . H27B H 0.4333 1.0239 0.2722 0.064 Uiso 1 1 calc R . . H27C H 0.4149 0.9747 0.3117 0.064 Uiso 1 1 calc R . . C28 C 0.2479(6) 1.0037(7) 0.1020(6) 0.051 Uani 1 1 d . . . H28A H 0.2481 0.9665 0.0816 0.076 Uiso 1 1 calc R . . H28B H 0.2712 1.0347 0.0877 0.076 Uiso 1 1 calc R . . H28C H 0.2060 1.0175 0.0999 0.076 Uiso 1 1 calc R . . C29 C 0.3547(5) 0.8669(6) 0.1732(6) 0.029 Uani 1 1 d . . . H29 H 0.3901 0.8876 0.1899 0.034 Uiso 1 1 calc R . . C30 C 0.3425(6) 0.8660(6) 0.1185(6) 0.039 Uiso 1 1 d . . . H30 H 0.3692 0.8844 0.0986 0.047 Uiso 1 1 calc R . . C31 C 0.2900(6) 0.8374(6) 0.0940(6) 0.037 Uiso 1 1 d . . . H31 H 0.2797 0.8359 0.0565 0.044 Uiso 1 1 calc R . . C32 C 0.2522(6) 0.8107(6) 0.1252(6) 0.029 Uani 1 1 d . . . C33 C 0.2695(5) 0.8111(6) 0.1803(5) 0.020 Uiso 1 1 d . . . C34 C 0.1957(6) 0.7808(6) 0.1042(6) 0.033 Uani 1 1 d . . . H34 H 0.1806 0.7806 0.0672 0.040 Uiso 1 1 calc R . . C35 C 0.1651(6) 0.7536(6) 0.1367(6) 0.031 Uani 1 1 d . . . H35 H 0.1278 0.7342 0.1231 0.038 Uiso 1 1 calc R . . C36 C 0.1874(6) 0.7533(6) 0.1910(6) 0.024 Uani 1 1 d . . . C37 C 0.1598(5) 0.7229(6) 0.2308(6) 0.023 Uani 1 1 d . . . C38 C 0.1890(5) 0.7255(6) 0.2849(6) 0.031 Uani 1 1 d . . . C39 C 0.1588(6) 0.6957(6) 0.3201(7) 0.036 Uani 1 1 d . . . C40 C 0.1071(6) 0.6901(6) 0.2246(7) 0.035 Uani 1 1 d . . . C41 C 0.1718(6) 0.6860(7) 0.3793(7) 0.056 Uani 1 1 d . . . H41A H 0.2095 0.6631 0.3892 0.084 Uiso 1 1 calc R . . H41B H 0.1384 0.6637 0.3898 0.084 Uiso 1 1 calc R . . H41C H 0.1761 0.7251 0.3973 0.084 Uiso 1 1 calc R . . C42 C 0.0613(7) 0.6725(6) 0.1741(6) 0.052 Uani 1 1 d . . . H42A H 0.0392 0.7083 0.1591 0.078 Uiso 1 1 calc R . . H42B H 0.0326 0.6428 0.1831 0.078 Uiso 1 1 calc R . . H42C H 0.0832 0.6551 0.1481 0.078 Uiso 1 1 calc R . . C43 C 0.2868(6) 0.7828(6) 0.4101(6) 0.029 Uani 1 1 d . . . H43 H 0.2639 0.8187 0.4023 0.034 Uiso 1 1 calc R . . C44 C 0.3087(7) 0.7682(7) 0.4623(6) 0.046 Uani 1 1 d . . . H44 H 0.3017 0.7942 0.4898 0.055 Uiso 1 1 calc R . . C45 C 0.3405(7) 0.7158(7) 0.4740(6) 0.045 Uani 1 1 d . . . H45 H 0.3555 0.7056 0.5098 0.054 Uiso 1 1 calc R . . C46 C 0.3517(6) 0.6762(6) 0.4329(6) 0.032 Uani 1 1 d . . . C47 C 0.3292(5) 0.6935(7) 0.3817(6) 0.031 Uani 1 1 d . . . C48 C 0.3842(7) 0.6207(7) 0.4407(6) 0.048 Uani 1 1 d . . . H48 H 0.4008 0.6070 0.4753 0.058 Uiso 1 1 calc R . . C49 C 0.3906(6) 0.5888(6) 0.3985(6) 0.031 Uani 1 1 d . . . H49 H 0.4116 0.5516 0.4033 0.037 Uiso 1 1 calc R . . C50 C 0.3669(5) 0.6088(6) 0.3467(6) 0.020 Uani 1 1 d . . . C51 C 0.3730(6) 0.5772(6) 0.2974(6) 0.026 Uani 1 1 d . . . C52 C 0.4264(6) 0.5441(6) 0.2872(5) 0.021 Uani 1 1 d . . . C53 C 0.4231(6) 0.5227(6) 0.2386(6) 0.025 Uani 1 1 d . . . C54 C 0.3308(5) 0.5779(6) 0.2514(5) 0.023 Uani 1 1 d . . . C55 C 0.4700(6) 0.4882(6) 0.2154(6) 0.033 Uani 1 1 d . . . H55A H 0.5094 0.5081 0.2251 0.049 Uiso 1 1 calc R . . H55B H 0.4582 0.4873 0.1768 0.049 Uiso 1 1 calc R . . H55C H 0.4728 0.4470 0.2291 0.049 Uiso 1 1 calc R . . C56 C 0.2679(6) 0.6061(6) 0.2433(5) 0.026 Uani 1 1 d . . . H56A H 0.2516 0.6025 0.2760 0.038 Uiso 1 1 calc R . . H56B H 0.2411 0.5852 0.2147 0.038 Uiso 1 1 calc R . . H56C H 0.2706 0.6487 0.2342 0.038 Uiso 1 1 calc R . . C57 C 0.7393(6) 0.3505(7) 0.1151(6) 0.033 Uani 1 1 d . . . H57 H 0.7733 0.3276 0.1316 0.040 Uiso 1 1 calc R . . C58 C 0.7124(6) 0.3353(6) 0.0651(5) 0.029 Uani 1 1 d . . . H58 H 0.7250 0.3008 0.0482 0.035 Uiso 1 1 calc R . . C59 C 0.6666(5) 0.3714(6) 0.0400(5) 0.027 Uani 1 1 d . . . H59 H 0.6484 0.3630 0.0045 0.032 Uiso 1 1 calc R . . C60 C 0.6466(5) 0.4199(6) 0.0655(5) 0.018 Uiso 1 1 d . . . C61 C 0.6725(5) 0.4287(5) 0.1178(5) 0.016 Uani 1 1 d . . . C62 C 0.6021(5) 0.4595(6) 0.0414(5) 0.020 Uani 1 1 d . . . H62 H 0.5841 0.4535 0.0054 0.024 Uiso 1 1 calc R . . C63 C 0.5838(5) 0.5063(6) 0.0677(5) 0.019 Uani 1 1 d . . . H63 H 0.5547 0.5343 0.0506 0.023 Uiso 1 1 calc R . . C64 C 0.6092(5) 0.5118(5) 0.1210(5) 0.016 Uani 1 1 d . . . C65 C 0.5910(5) 0.5564(6) 0.1585(5) 0.016 Uani 1 1 d . . . C66 C 0.6220(5) 0.5569(6) 0.2115(5) 0.023 Uani 1 1 d . . . C67 C 0.6038(5) 0.6016(6) 0.2413(6) 0.024 Uani 1 1 d . . . C68 C 0.5455(5) 0.5989(5) 0.1473(5) 0.017 Uani 1 1 d . . . C69 C 0.6234(5) 0.6234(6) 0.2970(5) 0.028 Uani 1 1 d . . . H69A H 0.6139 0.5928 0.3216 0.042 Uiso 1 1 calc R . . H69B H 0.6019 0.6608 0.3019 0.042 Uiso 1 1 calc R . . H69C H 0.6671 0.6310 0.3038 0.042 Uiso 1 1 calc R . . C70 C 0.4991(5) 0.6141(6) 0.0985(5) 0.031 Uani 1 1 d . . . H70A H 0.5199 0.6288 0.0707 0.046 Uiso 1 1 calc R . . H70B H 0.4717 0.6454 0.1072 0.046 Uiso 1 1 calc R . . H70C H 0.4757 0.5780 0.0861 0.046 Uiso 1 1 calc R . . C71 C 0.9495(5) 0.5164(6) 0.2756(6) 0.030 Uani 1 1 d . . . H71 H 0.9627 0.5387 0.2484 0.036 Uiso 1 1 calc R . . C72 C 0.9848(6) 0.5185(6) 0.3261(6) 0.032 Uani 1 1 d . . . H72 H 1.0215 0.5409 0.3325 0.039 Uiso 1 1 calc R . . C73 C 0.9661(6) 0.4880(6) 0.3665(6) 0.037 Uani 1 1 d . . . H73 H 0.9898 0.4880 0.4011 0.045 Uiso 1 1 calc R . . C74 C 0.9095(5) 0.4560(6) 0.3550(5) 0.026 Uani 1 1 d . . . C75 C 0.8772(6) 0.4561(7) 0.3032(5) 0.032 Uani 1 1 d . . . C76 C 0.8855(6) 0.4249(6) 0.3951(5) 0.030 Uani 1 1 d . . . H76 H 0.9068 0.4240 0.4305 0.036 Uiso 1 1 calc R . . C77 C 0.8322(5) 0.3973(6) 0.3811(6) 0.027 Uani 1 1 d . . . H77 H 0.8150 0.3762 0.4069 0.032 Uiso 1 1 calc R . . C78 C 0.8008(6) 0.3992(6) 0.3272(6) 0.025 Uani 1 1 d . . . C79 C 0.7422(6) 0.3691(6) 0.3117(6) 0.024 Uani 1 1 d . . . C80 C 0.7153(5) 0.3770(5) 0.2575(5) 0.016 Uani 1 1 d . . . C81 C 0.6600(6) 0.3495(6) 0.2434(6) 0.027 Uani 1 1 d . . . C82 C 0.7058(6) 0.3391(6) 0.3409(6) 0.031 Uani 1 1 d . . . C83 C 0.6162(6) 0.3361(6) 0.1913(5) 0.034 Uani 1 1 d . . . H83A H 0.5994 0.3739 0.1754 0.051 Uiso 1 1 calc R . . H83B H 0.5832 0.3103 0.1985 0.051 Uiso 1 1 calc R . . H83C H 0.6381 0.3155 0.1669 0.051 Uiso 1 1 calc R . . C84 C 0.7161(6) 0.3196(6) 0.3974(6) 0.033 Uani 1 1 d . . . H84A H 0.7522 0.2939 0.4048 0.049 Uiso 1 1 calc R . . H84B H 0.6808 0.2970 0.4040 0.049 Uiso 1 1 calc R . . H84C H 0.7221 0.3550 0.4203 0.049 Uiso 1 1 calc R . . C85 C 0.6567(7) 0.4751(6) 0.3352(6) 0.045 Uani 1 1 d . . . H85 H 0.6230 0.4525 0.3176 0.054 Uiso 1 1 calc R . . C86 C 0.6678(9) 0.4778(7) 0.3907(7) 0.063 Uani 1 1 d . . . H86 H 0.6402 0.4585 0.4091 0.075 Uiso 1 1 calc R . . C87 C 0.7150(8) 0.5061(8) 0.4185(7) 0.061 Uani 1 1 d . . . H87 H 0.7223 0.5073 0.4560 0.073 Uiso 1 1 calc R . . C88 C 0.7539(7) 0.5345(7) 0.3885(6) 0.045 Uani 1 1 d . . . C89 C 0.7408(6) 0.5342(7) 0.3321(6) 0.036 Uani 1 1 d . . . C90 C 0.8060(8) 0.5661(8) 0.4102(7) 0.069 Uani 1 1 d . . . H90 H 0.8185 0.5657 0.4475 0.082 Uiso 1 1 calc R . . C91 C 0.8404(7) 0.5978(7) 0.3806(7) 0.050 Uani 1 1 d . . . H91 H 0.8753 0.6193 0.3973 0.060 Uiso 1 1 calc R . . C92 C 0.8237(7) 0.5981(7) 0.3256(7) 0.048 Uani 1 1 d . . . C93 C 0.8568(6) 0.6278(6) 0.2894(6) 0.031 Uani 1 1 d . . . C94 C 0.8303(6) 0.6230(6) 0.2328(6) 0.027 Uani 1 1 d . . . C95 C 0.8644(6) 0.6484(6) 0.2010(6) 0.033 Uani 1 1 d . . . C96 C 0.9102(7) 0.6575(7) 0.2995(6) 0.047 Uani 1 1 d . . . C97 C 0.8591(6) 0.6559(6) 0.1428(6) 0.036 Uani 1 1 d . . . H97A H 0.8605 0.6163 0.1263 0.054 Uiso 1 1 calc R . . H97B H 0.8928 0.6806 0.1355 0.054 Uiso 1 1 calc R . . H97C H 0.8207 0.6757 0.1284 0.054 Uiso 1 1 calc R . . C98 C 0.9520(7) 0.6760(7) 0.3512(6) 0.055 Uani 1 1 d . . . H98A H 0.9281 0.6957 0.3745 0.083 Uiso 1 1 calc R . . H98B H 0.9829 0.7039 0.3433 0.083 Uiso 1 1 calc R . . H98C H 0.9717 0.6402 0.3687 0.083 Uiso 1 1 calc R . . C99 C 0.7539(5) 0.5559(6) 0.1063(6) 0.028 Uani 1 1 d . . . H99 H 0.7787 0.5226 0.1192 0.034 Uiso 1 1 calc R . . C100 C 0.7377(5) 0.5634(6) 0.0521(6) 0.030 Uani 1 1 d . . . H100 H 0.7520 0.5363 0.0287 0.036 Uiso 1 1 calc R . . C101 C 0.7008(5) 0.6105(6) 0.0327(6) 0.033 Uani 1 1 d . . . H101 H 0.6873 0.6150 -0.0043 0.039 Uiso 1 1 calc R . . C102 C 0.6832(5) 0.6518(6) 0.0680(5) 0.020 Uani 1 1 d . . . C103 C 0.7000(5) 0.6421(6) 0.1224(5) 0.022 Uani 1 1 d . . . C104 C 0.6458(5) 0.7029(6) 0.0519(6) 0.023 Uani 1 1 d . . . H104 H 0.6313 0.7115 0.0156 0.028 Uiso 1 1 calc R . . C105 C 0.6318(5) 0.7388(6) 0.0907(6) 0.026 Uani 1 1 d . . . H105 H 0.6094 0.7747 0.0813 0.031 Uiso 1 1 calc R . . C106 C 0.6498(5) 0.7241(5) 0.1450(5) 0.015 Uani 1 1 d . . . C107 C 0.6327(5) 0.7592(6) 0.1890(5) 0.018 Uani 1 1 d . . . C108 C 0.5773(5) 0.7938(6) 0.1885(6) 0.022 Uani 1 1 d . . . C109 C 0.5716(6) 0.8198(6) 0.2343(5) 0.023 Uani 1 1 d . . . C110 C 0.6676(6) 0.7616(6) 0.2376(6) 0.026 Uani 1 1 d . . . C111 C 0.5203(6) 0.8556(6) 0.2482(6) 0.030 Uiso 1 1 d . . . H11D H 0.4822 0.8341 0.2364 0.044 Uiso 1 1 calc R . . H11E H 0.5186 0.8950 0.2308 0.044 Uiso 1 1 calc R . . H11F H 0.5267 0.8613 0.2866 0.044 Uiso 1 1 calc R . . C112 C 0.7301(5) 0.7353(6) 0.2600(6) 0.029 Uiso 1 1 d . . . H11A H 0.7258 0.6928 0.2687 0.043 Uiso 1 1 calc R . . H11B H 0.7481 0.7574 0.2919 0.043 Uiso 1 1 calc R . . H11C H 0.7562 0.7388 0.2336 0.043 Uiso 1 1 calc R . . F1A F 0.9670(4) 0.5532(4) 0.1604(4) 0.053 Uani 1 1 d . . . B1A B 0.9664(10) 0.5283(11) 0.1118(11) 0.074 Uani 1 1 d . . . F2A F 1.0039(5) 0.5604(6) 0.0852(5) 0.107 Uani 1 1 d . . . B2A B 0.8026(9) 0.1871(9) 0.0641(8) 0.052 Uani 1 1 d . . . F3A F 0.9845(5) 0.4687(5) 0.1167(6) 0.122 Uani 1 1 d . . . B3A B 0.4584(8) 0.3988(8) 0.0696(8) 0.035 Uani 1 1 d . . . F4A F 0.9073(5) 0.5287(6) 0.0840(5) 0.121 Uani 1 1 d . . . B4A B 0.3792(7) 0.0252(8) 0.0349(7) 0.027 Uiso 1 1 d . . . F5A F 0.7982(5) 0.2214(5) 0.1064(4) 0.091 Uani 1 1 d . . . B5A B 0.2948(8) 0.6522(10) 0.0835(7) 0.042 Uani 1 1 d . . . F6A F 0.8315(4) 0.2193(4) 0.0292(4) 0.082 Uani 1 1 d . . . B6A B -0.0216(7) 0.8061(9) 0.0632(7) 0.418 Uiso 1 1 d D . . F7A F 0.8349(4) 0.1362(4) 0.0783(4) 0.071 Uani 1 1 d . . . F8A F 0.7453(4) 0.1732(5) 0.0370(4) 0.078 Uani 1 1 d . . . F9A F 0.4443(3) 0.4621(4) 0.0720(3) 0.044 Uani 1 1 d . . . F10A F 0.5049(3) 0.3858(4) 0.1100(4) 0.056 Uani 1 1 d . . . F11A F 0.4724(4) 0.3887(4) 0.0210(3) 0.050 Uani 1 1 d . . . F12A F 0.4050(3) 0.3671(3) 0.0750(3) 0.037 Uani 1 1 d . . . F13A F 0.3987(4) 0.0507(5) 0.0823(4) 0.068 Uani 1 1 d . . . F14A F 0.3391(3) 0.0640(4) 0.0038(3) 0.058 Uani 1 1 d . . . F15A F 0.3507(4) -0.0283(4) 0.0388(4) 0.067 Uani 1 1 d . . . F16A F 0.4284(3) 0.0146(4) 0.0092(3) 0.042 Uiso 1 1 d . . . F17A F 0.3556(4) 0.6484(7) 0.0939(4) 0.131 Uani 1 1 d . . . F18A F 0.2745(6) 0.5998(4) 0.0572(5) 0.100 Uani 1 1 d . . . F19A F 0.2773(5) 0.6979(4) 0.0506(4) 0.082 Uani 1 1 d . . . F20A F 0.2736(4) 0.6562(4) 0.1305(3) 0.052 Uani 1 1 d . . . F21A F 0.0337(5) 0.7881(5) 0.0891(5) 0.095 Uiso 1 1 d D . . F22A F -0.0301(6) 0.7792(6) 0.0153(6) 0.140 Uiso 1 1 d D . . F23A F -0.0420(8) 0.8633(8) 0.0667(8) 0.208 Uiso 1 1 d D . . F24A F -0.0621(7) 0.7811(7) 0.0905(7) 0.161 Uiso 1 1 d D . . C1S C 0.5420(7) 0.2540(7) 0.0149(6) 0.042 Uani 1 1 d . . . H1S H 0.5493 0.2960 0.0180 0.051 Uiso 1 1 calc R . . C2S C 0.5848(7) 0.2162(7) -0.0002(6) 0.038 Uani 1 1 d . . . H2S H 0.6215 0.2323 -0.0077 0.046 Uiso 1 1 calc R . . C3S C 0.5742(6) 0.1561(7) -0.0043(5) 0.038 Uani 1 1 d . . . H3S H 0.6037 0.1304 -0.0145 0.046 Uiso 1 1 calc R . . C4S C 0.5213(7) 0.1320(7) 0.0063(6) 0.043 Uani 1 1 d . . . H4S H 0.5148 0.0898 0.0039 0.052 Uiso 1 1 calc R . . C5S C 0.4770(7) 0.1701(7) 0.0205(6) 0.049 Uani 1 1 d . . . H5S H 0.4396 0.1543 0.0266 0.059 Uiso 1 1 calc R . . C6S C 0.4888(6) 0.2304(6) 0.0254(6) 0.030 Uani 1 1 d . . . H6S H 0.4599 0.2564 0.0362 0.036 Uiso 1 1 calc R . . O1W O 0.2090(4) 0.9020(4) 0.3708(4) 0.028 Uani 1 1 d . . . O2W O 0.8355(3) 0.4526(4) 0.1708(3) 0.024 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 0.019 0.029 0.036 -0.006 0.010 -0.002 Br1 0.021 0.042 0.055 0.001 0.004 0.004 S1 0.020 0.034 0.031 0.003 0.006 0.002 N1 0.039 0.020 0.038 -0.022 0.023 -0.005 C1 0.022 0.086 0.049 -0.007 0.016 0.008 Pd2 0.018 0.032 0.021 -0.004 0.004 0.000 Br2 0.019 0.039 0.032 -0.001 -0.003 -0.002 S2 0.027 0.043 0.071 0.007 0.025 -0.007 N2 0.020 0.020 0.020 0.000 0.004 0.000 C2 0.068 0.036 0.087 -0.011 0.026 0.008 Pd3 0.019 0.028 0.023 -0.001 0.004 0.001 S3 0.027 0.036 0.071 0.013 0.004 -0.004 N3 0.031 0.016 0.030 0.000 0.013 -0.003 C3 0.062 0.068 0.037 -0.034 -0.001 -0.006 Pd4 0.015 0.030 0.018 -0.001 0.000 0.005 S4 0.030 0.029 0.028 -0.005 0.008 -0.003 N4 0.024 0.019 0.038 -0.015 0.016 0.001 C4 0.039 0.069 0.076 -0.021 0.018 -0.017 Pd5 0.025 0.032 0.018 -0.003 0.000 0.010 S5 0.016 0.030 0.030 0.000 0.006 0.005 N5 0.036 0.021 0.039 0.006 0.007 -0.004 C5 0.024 0.041 0.030 0.011 0.002 0.008 Pd6 0.027 0.032 0.023 -0.006 -0.008 0.005 S6 0.026 0.042 0.025 0.011 0.003 0.000 N6 0.024 0.004 0.035 0.002 0.011 0.002 C6 0.047 0.098 0.029 -0.014 -0.005 -0.014 S7 0.026 0.047 0.067 -0.015 -0.021 0.003 N7 0.018 0.031 0.021 0.009 0.014 0.005 C7 0.042 0.072 0.018 -0.008 -0.016 0.002 S8 0.021 0.029 0.026 -0.002 -0.001 -0.006 N8 0.017 0.040 0.011 -0.003 0.007 -0.005 C8 0.025 0.029 0.041 0.015 -0.009 -0.007 N9 0.017 0.023 0.018 0.003 0.001 0.001 C9 0.028 0.031 0.013 -0.005 0.012 -0.004 N10 0.012 0.034 0.009 -0.001 -0.002 -0.003 C10 0.006 0.037 0.026 0.001 -0.001 -0.005 N11 0.018 0.020 0.026 -0.005 0.000 0.015 C11 0.006 0.018 0.045 0.010 0.011 -0.001 C12 0.005 0.046 0.050 0.001 0.008 0.000 N13 0.077 0.021 0.020 -0.010 0.002 0.025 C13 0.005 0.052 0.031 -0.013 0.007 0.003 N14 0.032 0.031 0.035 -0.016 -0.012 0.024 C14 0.032 0.054 0.025 0.005 0.012 0.016 N15 0.025 0.016 0.017 0.000 0.005 0.001 C15 0.032 0.017 0.034 0.003 0.018 0.000 N16 0.024 0.012 0.021 -0.007 -0.006 -0.005 C16 0.019 0.036 0.045 -0.011 0.013 -0.004 C17 0.031 0.035 0.033 -0.008 0.009 -0.005 C18 0.023 0.017 0.032 -0.010 0.004 0.009 C19 0.022 0.020 0.021 -0.008 0.011 0.009 C20 0.024 0.050 0.029 0.012 0.005 0.005 C21 0.030 0.036 0.029 0.004 0.008 0.016 C22 0.015 0.031 0.031 0.000 0.016 0.005 C23 0.020 0.022 0.064 0.004 0.024 -0.003 C24 0.034 0.030 0.042 0.005 0.009 0.001 C25 0.030 0.033 0.064 0.001 0.024 0.004 C26 0.033 0.027 0.096 0.000 0.040 -0.001 C27 0.022 0.055 0.052 -0.015 0.008 -0.011 C28 0.030 0.071 0.062 0.032 0.035 0.011 C29 0.010 0.039 0.030 -0.001 -0.014 0.004 C32 0.020 0.041 0.027 -0.001 0.008 0.015 C34 0.038 0.033 0.020 -0.008 -0.015 0.026 C35 0.043 0.036 0.015 -0.017 0.003 -0.006 C36 0.023 0.019 0.027 -0.001 -0.004 -0.001 C37 0.018 0.014 0.034 0.009 -0.003 0.008 C38 0.013 0.032 0.045 0.008 0.001 0.015 C39 0.038 0.011 0.060 0.005 0.013 -0.001 C40 0.030 0.009 0.067 -0.009 0.007 -0.004 C41 0.033 0.060 0.074 0.030 0.008 -0.008 C42 0.053 0.024 0.070 0.016 -0.013 -0.007 C43 0.034 0.037 0.020 -0.004 0.017 0.006 C44 0.063 0.047 0.030 -0.012 0.015 0.018 C45 0.071 0.039 0.020 -0.001 -0.006 0.005 C46 0.048 0.036 0.012 0.004 0.003 0.018 C47 0.010 0.045 0.040 0.002 0.008 -0.008 C48 0.076 0.044 0.021 0.007 -0.001 0.016 C49 0.021 0.032 0.035 -0.003 -0.002 0.000 C50 0.021 0.009 0.030 -0.012 0.001 0.002 C51 0.024 0.023 0.033 0.004 0.014 -0.003 C52 0.029 0.012 0.022 0.009 0.004 -0.004 C53 0.024 0.028 0.021 -0.007 -0.001 -0.007 C54 0.016 0.033 0.020 0.014 0.003 0.001 C55 0.037 0.022 0.046 -0.018 0.029 -0.003 C56 0.039 0.024 0.015 0.002 0.007 0.011 C57 0.016 0.056 0.025 0.001 -0.004 -0.003 C58 0.026 0.039 0.023 -0.010 0.004 0.015 C59 0.023 0.047 0.014 0.000 0.012 -0.008 C61 0.015 0.009 0.029 0.001 0.015 -0.001 C62 0.006 0.044 0.009 -0.003 -0.002 0.001 C63 0.006 0.026 0.022 -0.002 -0.005 -0.002 C64 0.011 0.011 0.027 -0.001 0.007 -0.005 C65 0.008 0.028 0.013 0.009 0.002 0.004 C66 0.018 0.034 0.019 -0.001 0.012 0.006 C67 0.014 0.027 0.032 0.015 0.009 -0.006 C68 0.021 0.009 0.020 0.004 0.005 -0.003 C69 0.013 0.048 0.023 -0.001 0.002 0.013 C70 0.020 0.049 0.021 -0.002 0.000 0.011 C71 0.019 0.040 0.027 0.010 -0.003 0.017 C72 0.013 0.034 0.049 -0.002 0.003 0.005 C73 0.024 0.037 0.040 -0.014 -0.021 0.010 C74 0.021 0.030 0.021 -0.005 -0.008 0.012 C75 0.030 0.054 0.010 0.004 -0.002 0.011 C76 0.029 0.046 0.012 0.006 -0.005 0.011 C77 0.017 0.030 0.035 0.007 0.009 0.010 C78 0.021 0.024 0.022 -0.006 -0.013 0.013 C79 0.027 0.018 0.027 -0.006 0.004 0.016 C80 0.018 0.018 0.014 -0.006 0.004 0.008 C81 0.029 0.032 0.018 0.006 -0.004 0.001 C82 0.025 0.040 0.027 -0.013 0.002 0.004 C83 0.026 0.050 0.020 -0.008 -0.014 0.007 C84 0.024 0.041 0.034 0.016 0.009 0.001 C85 0.074 0.025 0.036 -0.004 0.011 0.025 C86 0.119 0.051 0.017 -0.002 0.010 0.031 C87 0.086 0.064 0.034 0.011 0.013 0.051 C88 0.060 0.035 0.032 -0.013 -0.014 0.038 C89 0.042 0.030 0.030 -0.002 -0.012 0.025 C90 0.093 0.064 0.041 -0.004 -0.007 0.068 C91 0.044 0.035 0.059 -0.004 -0.023 0.026 C92 0.045 0.059 0.033 -0.006 -0.012 0.038 C93 0.033 0.016 0.039 -0.015 -0.010 0.010 C94 0.027 0.027 0.027 0.000 0.005 0.000 C95 0.025 0.032 0.032 0.002 -0.022 0.009 C96 0.040 0.056 0.030 -0.011 -0.030 0.016 C97 0.022 0.029 0.050 0.005 -0.008 -0.008 C98 0.051 0.049 0.048 -0.011 -0.037 -0.008 C99 0.012 0.041 0.028 0.005 -0.005 0.002 C100 0.013 0.027 0.049 -0.016 0.004 -0.003 C101 0.010 0.043 0.046 -0.011 0.006 -0.011 C102 0.003 0.035 0.022 0.006 0.002 0.000 C103 0.011 0.030 0.021 0.002 -0.002 -0.006 C104 0.010 0.028 0.030 0.006 -0.002 0.013 C105 0.015 0.023 0.037 0.001 -0.006 0.001 C106 0.008 0.017 0.018 -0.003 -0.005 -0.008 C107 0.017 0.017 0.021 -0.010 0.007 -0.010 C108 0.015 0.018 0.030 0.010 -0.009 -0.006 C109 0.027 0.026 0.017 -0.001 0.010 0.007 C110 0.033 0.015 0.031 -0.002 0.006 -0.010 F1A 0.048 0.071 0.041 0.001 0.011 0.008 B1A 0.059 0.071 0.090 -0.038 0.003 0.003 F2A 0.107 0.156 0.066 0.033 0.042 0.021 B2A 0.064 0.044 0.039 0.001 -0.016 -0.014 F3A 0.062 0.086 0.225 -0.066 0.045 0.002 B3A 0.037 0.022 0.041 0.021 -0.009 0.012 F4A 0.077 0.204 0.068 -0.061 -0.024 0.028 F5A 0.127 0.111 0.026 -0.025 -0.013 0.053 B5A 0.029 0.077 0.024 0.013 0.018 -0.010 F6A 0.073 0.070 0.095 0.037 -0.002 -0.038 F7A 0.081 0.047 0.084 0.027 0.013 0.015 F8A 0.066 0.114 0.045 0.016 -0.015 -0.041 F9A 0.029 0.041 0.063 -0.003 0.016 0.003 F10A 0.017 0.100 0.048 0.024 -0.004 0.011 F11A 0.067 0.064 0.023 -0.008 0.019 0.007 F12A 0.032 0.042 0.039 0.004 0.007 -0.004 F13A 0.057 0.109 0.036 -0.011 0.004 0.003 F14A 0.030 0.107 0.039 0.025 0.016 0.018 F15A 0.104 0.037 0.076 -0.006 0.064 -0.014 F17A 0.040 0.316 0.041 0.033 0.017 0.033 F18A 0.176 0.058 0.088 -0.035 0.084 -0.060 F19A 0.159 0.059 0.041 0.015 0.055 0.047 F20A 0.040 0.087 0.028 0.015 0.007 0.013 C1S 0.053 0.043 0.022 0.008 -0.017 0.005 C2S 0.044 0.036 0.032 0.003 -0.001 0.002 C3S 0.038 0.063 0.013 0.020 0.002 0.019 C4S 0.062 0.036 0.027 0.008 -0.003 0.016 C5S 0.052 0.048 0.043 0.011 -0.005 -0.015 C6S 0.024 0.029 0.033 0.005 -0.009 0.004 O1W 0.019 0.035 0.033 0.005 0.006 -0.002 O2W 0.017 0.030 0.025 0.010 0.003 0.009 _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 C24 1.946(14) . ? Pd1 N1 2.012(12) . ? Pd1 N4 2.038(11) . ? Pd1 O1W 2.149(9) . ? Pd1 Pd2 2.7892(15) . ? Br1 C52 1.912(13) . ? S1 C12 1.714(15) . ? S1 C11 1.751(12) . ? N1 C1 1.336(17) . ? N1 C5 1.359(16) . ? C1 C2 1.44(2) . ? Pd2 C10 1.979(13) . ? Pd2 N5 2.026(12) . ? Pd2 N2 2.060(11) . ? Pd2 C24 2.596(14) . ? Pd2 Pd3 2.7051(15) . ? Br2 C108 1.901(12) . ? S2 C26 1.703(16) . ? S2 C25 1.728(17) . ? N2 C8 1.341(16) . ? N2 C5 1.373(16) . ? C2 C3 1.31(2) . ? Pd3 C38 1.998(13) . ? Pd3 N7 2.038(11) . ? Pd3 N6 2.046(11) . ? S3 C40 1.707(16) . ? S3 C39 1.730(15) . ? N3 C15 1.318(15) . ? N3 C19 1.332(16) . ? C3 C4 1.47(2) . ? Pd4 C80 2.006(12) . ? Pd4 N9 2.041(10) . ? Pd4 N12 2.059(11) . ? Pd4 O2W 2.155(8) . ? Pd4 Pd5 2.7456(14) . ? S4 C54 1.687(14) . ? S4 C53 1.722(13) . ? N4 C22 1.349(16) . ? N4 C19 1.427(15) . ? C4 C5 1.42(2) . ? C4 C6 1.46(2) . ? Pd5 C66 1.984(13) . ? Pd5 N13 2.033(12) . ? Pd5 N10 2.049(10) . ? Pd5 Pd6 2.6798(16) . ? S5 C68 1.731(13) . ? S5 C67 1.745(13) . ? N5 C29 1.341(16) . ? N5 C33 1.367(15) . ? Pd6 C94 1.956(13) . ? Pd6 N15 2.049(10) . ? Pd6 N14 2.083(12) . ? S6 C82 1.720(14) . ? S6 C81 1.733(14) . ? N6 C36 1.349(15) . ? N6 C33 1.365(15) . ? C6 C7 1.36(2) . ? S7 C96 1.721(18) . ? S7 C95 1.785(13) . ? N7 C43 1.335(15) . ? N7 C47 1.413(16) . ? C7 C8 1.422(19) . ? S8 C109 1.725(13) . ? S8 C110 1.728(14) . ? N8 C50 1.340(15) . ? N8 C47 1.378(16) . ? C8 C9 1.460(18) . ? N9 C57 1.354(16) . ? N9 C61 1.355(15) . ? C9 C12 1.362(17) . ? C9 C10 1.448(17) . ? N10 C64 1.334(15) . ? N10 C61 1.413(15) . ? C10 C11 1.383(17) . ? N11 C71 1.335(16) . ? N11 C75 1.369(16) . ? C11 C13 1.486(18) . ? N12 C78 1.289(16) . ? N12 C75 1.405(16) . ? C12 C14 1.532(18) . ? N13 C89 1.347(17) . ? N13 C85 1.361(18) . ? N14 C92 1.353(18) . ? N14 C89 1.376(18) . ? N15 C99 1.327(16) . ? N15 C103 1.396(15) . ? C15 C16 1.367(18) . ? N16 C106 1.326(14) . ? N16 C103 1.358(15) . ? C16 C17 1.358(18) . ? C17 C18 1.424(17) . ? C18 C20 1.411(18) . ? C18 C19 1.441(18) . ? C20 C21 1.336(17) . ? C21 C22 1.447(18) . ? C22 C23 1.494(17) . ? C23 C26 1.41(2) . ? C23 C24 1.44(2) . ? C24 C25 1.413(18) . ? C25 C27 1.505(19) . ? C26 C28 1.51(2) . ? C29 C30 1.383(19) . ? C30 C31 1.388(18) . ? C31 C32 1.403(18) . ? C32 C33 1.401(18) . ? C32 C34 1.448(18) . ? C34 C35 1.323(18) . ? C35 C36 1.396(18) . ? C36 C37 1.457(18) . ? C37 C40 1.375(17) . ? C37 C38 1.426(18) . ? C38 C39 1.397(19) . ? C39 C41 1.51(2) . ? C40 C42 1.554(19) . ? C43 C44 1.383(19) . ? C44 C45 1.370(19) . ? C45 C46 1.434(19) . ? C46 C47 1.378(18) . ? C46 C48 1.429(18) . ? C48 C49 1.327(19) . ? C49 C50 1.415(18) . ? C50 C51 1.478(18) . ? C51 C54 1.375(18) . ? C51 C52 1.473(17) . ? C52 C53 1.329(17) . ? C53 C55 1.512(16) . ? C54 C56 1.523(16) . ? C57 C58 1.360(17) . ? C58 C59 1.370(17) . ? C59 C60 1.380(17) . ? C60 C61 1.380(17) . ? C60 C62 1.389(16) . ? C62 C63 1.345(16) . ? C63 C64 1.393(17) . ? C64 C65 1.492(17) . ? C65 C68 1.383(16) . ? C65 C66 1.414(17) . ? C66 C67 1.361(17) . ? C67 C69 1.503(18) . ? C68 C70 1.517(17) . ? C71 C72 1.396(18) . ? C72 C73 1.371(19) . ? C73 C74 1.439(18) . ? C74 C75 1.396(17) . ? C74 C76 1.428(18) . ? C76 C77 1.335(17) . ? C77 C78 1.438(18) . ? C78 C79 1.464(17) . ? C79 C82 1.380(18) . ? C79 C80 1.427(17) . ? C80 C81 1.373(17) . ? C81 C83 1.540(17) . ? C82 C84 1.494(18) . ? C85 C86 1.41(2) . ? C86 C87 1.32(2) . ? C87 C88 1.42(2) . ? C88 C90 1.39(2) . ? C88 C89 1.43(2) . ? C90 C91 1.38(2) . ? C91 C92 1.40(2) . ? C92 C93 1.45(2) . ? C93 C96 1.352(19) . ? C93 C94 1.475(19) . ? C94 C95 1.344(19) . ? C95 C97 1.492(19) . ? C96 C98 1.537(18) . ? C99 C100 1.386(18) . ? C100 C101 1.371(17) . ? C101 C102 1.399(17) . ? C102 C103 1.399(17) . ? C102 C104 1.429(16) . ? C104 C105 1.361(17) . ? C105 C106 1.420(17) . ? C106 C107 1.485(16) . ? C107 C110 1.349(18) . ? C107 C108 1.462(17) . ? C108 C109 1.342(17) . ? C109 C111 1.498(16) . ? C110 C112 1.532(17) . ? F1A B1A 1.36(2) . ? B1A F2A 1.38(3) . ? B1A F3A 1.39(2) . ? B1A F4A 1.39(2) . ? B2A F5A 1.35(2) . ? B2A F7A 1.36(2) . ? B2A F8A 1.38(2) . ? B2A F6A 1.40(2) . ? B3A F10A 1.363(17) . ? B3A F11A 1.36(2) . ? B3A F12A 1.419(18) . ? B3A F9A 1.446(17) . ? B4A F13A 1.344(18) . ? B4A F15A 1.362(17) . ? B4A F14A 1.391(17) . ? B4A F16A 1.409(17) . ? B5A F19A 1.33(2) . ? B5A F17A 1.344(18) . ? B5A F18A 1.38(2) . ? B5A F20A 1.384(18) . ? B6A F22A 1.354(12) . ? B6A F21A 1.358(12) . ? B6A F23A 1.359(12) . ? B6A F24A 1.366(13) . ? C1S C6S 1.375(18) . ? C1S C2S 1.386(19) . ? C2S C3S 1.357(18) . ? C3S C4S 1.374(19) . ? C4S C5S 1.41(2) . ? C5S C6S 1.368(18) . ? 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 C24 Pd1 N1 95.8(5) . . ? C24 Pd1 N4 81.4(5) . . ? N1 Pd1 N4 175.0(5) . . ? C24 Pd1 O1W 179.0(5) . . ? N1 Pd1 O1W 83.7(4) . . ? N4 Pd1 O1W 99.1(4) . . ? C24 Pd1 Pd2 63.6(4) . . ? N1 Pd1 Pd2 83.5(3) . . ? N4 Pd1 Pd2 98.8(3) . . ? O1W Pd1 Pd2 117.2(2) . . ? C12 S1 C11 94.9(7) . . ? C1 N1 C5 117.7(13) . . ? C1 N1 Pd1 117.7(10) . . ? C5 N1 Pd1 122.9(9) . . ? N1 C1 C2 126.7(15) . . ? C10 Pd2 N5 92.5(5) . . ? C10 Pd2 N2 82.2(5) . . ? N5 Pd2 N2 172.9(4) . . ? C10 Pd2 C24 167.2(5) . . ? N5 Pd2 C24 81.9(5) . . ? N2 Pd2 C24 102.3(4) . . ? C10 Pd2 Pd3 75.2(3) . . ? N5 Pd2 Pd3 83.2(3) . . ? N2 Pd2 Pd3 99.8(3) . . ? C24 Pd2 Pd3 115.3(3) . . ? C10 Pd2 Pd1 150.3(4) . . ? N5 Pd2 Pd1 106.5(3) . . ? N2 Pd2 Pd1 80.3(3) . . ? C24 Pd2 Pd1 42.2(3) . . ? Pd3 Pd2 Pd1 84.48(4) . . ? C26 S2 C25 96.0(8) . . ? C8 N2 C5 119.1(12) . . ? C8 N2 Pd2 114.6(10) . . ? C5 N2 Pd2 126.2(9) . . ? C3 C2 C1 114.7(16) . . ? C38 Pd3 N7 96.2(5) . . ? C38 Pd3 N6 81.2(5) . . ? N7 Pd3 N6 176.1(4) . . ? C38 Pd3 Pd2 156.5(4) . . ? N7 Pd3 Pd2 100.0(3) . . ? N6 Pd3 Pd2 83.4(3) . . ? C40 S3 C39 94.5(7) . . ? C15 N3 C19 118.1(12) . . ? C2 C3 C4 122.4(17) . . ? C80 Pd4 N9 96.1(5) . . ? C80 Pd4 N12 80.1(5) . . ? N9 Pd4 N12 175.3(4) . . ? C80 Pd4 O2W 178.3(4) . . ? N9 Pd4 O2W 85.4(4) . . ? N12 Pd4 O2W 98.3(4) . . ? C80 Pd4 Pd5 66.0(3) . . ? N9 Pd4 Pd5 83.8(3) . . ? N12 Pd4 Pd5 97.2(3) . . ? O2W Pd4 Pd5 115.2(2) . . ? C54 S4 C53 93.5(7) . . ? C22 N4 C19 118.0(11) . . ? C22 N4 Pd1 117.2(9) . . ? C19 N4 Pd1 124.8(9) . . ? C5 C4 C6 117.6(15) . . ? C5 C4 C3 117.7(16) . . ? C6 C4 C3 124.5(17) . . ? C66 Pd5 N13 92.5(5) . . ? C66 Pd5 N10 81.2(5) . . ? N13 Pd5 N10 172.9(4) . . ? C66 Pd5 Pd6 77.8(4) . . ? N13 Pd5 Pd6 86.0(4) . . ? N10 Pd5 Pd6 95.8(3) . . ? C66 Pd5 Pd4 155.7(4) . . ? N13 Pd5 Pd4 103.2(3) . . ? N10 Pd5 Pd4 83.8(3) . . ? Pd6 Pd5 Pd4 84.86(5) . . ? C68 S5 C67 93.5(6) . . ? C29 N5 C33 117.6(13) . . ? C29 N5 Pd2 115.1(9) . . ? C33 N5 Pd2 126.8(9) . . ? N1 C5 N2 117.3(13) . . ? N1 C5 C4 120.6(14) . . ? N2 C5 C4 121.5(13) . . ? C94 Pd6 N15 94.6(5) . . ? C94 Pd6 N14 83.0(5) . . ? N15 Pd6 N14 177.3(4) . . ? C94 Pd6 Pd5 159.1(4) . . ? N15 Pd6 Pd5 100.1(3) . . ? N14 Pd6 Pd5 82.6(3) . . ? C82 S6 C81 94.9(7) . . ? C36 N6 C33 116.3(12) . . ? C36 N6 Pd3 117.1(9) . . ? C33 N6 Pd3 125.6(9) . . ? C7 C6 C4 118.0(16) . . ? C96 S7 C95 94.0(7) . . ? C43 N7 C47 119.5(12) . . ? C43 N7 Pd3 123.9(9) . . ? C47 N7 Pd3 116.7(9) . . ? C6 C7 C8 120.6(15) . . ? C109 S8 C110 92.8(7) . . ? C50 N8 C47 116.8(12) . . ? N2 C8 C7 122.1(14) . . ? N2 C8 C9 114.5(13) . . ? C7 C8 C9 123.3(13) . . ? C57 N9 C61 116.7(12) . . ? C57 N9 Pd4 116.1(8) . . ? C61 N9 Pd4 126.9(9) . . ? C12 C9 C10 114.8(12) . . ? C12 C9 C8 128.9(13) . . ? C10 C9 C8 116.1(12) . . ? C64 N10 C61 117.0(11) . . ? C64 N10 Pd5 118.1(9) . . ? C61 N10 Pd5 124.8(8) . . ? C11 C10 C9 112.5(12) . . ? C11 C10 Pd2 135.0(11) . . ? C9 C10 Pd2 112.1(10) . . ? C71 N11 C75 117.8(12) . . ? C10 C11 C13 135.8(12) . . ? C10 C11 S1 108.5(11) . . ? C13 C11 S1 115.7(10) . . ? C78 N12 C75 117.7(12) . . ? C78 N12 Pd4 115.7(9) . . ? C75 N12 Pd4 126.5(9) . . ? C9 C12 C14 132.3(14) . . ? C9 C12 S1 109.2(11) . . ? C14 C12 S1 118.5(10) . . ? C89 N13 C85 117.5(14) . . ? C89 N13 Pd5 124.5(12) . . ? C85 N13 Pd5 117.3(11) . . ? C92 N14 C89 120.7(14) . . ? C92 N14 Pd6 113.2(11) . . ? C89 N14 Pd6 125.6(10) . . ? C99 N15 C103 118.9(12) . . ? C99 N15 Pd6 122.7(9) . . ? C103 N15 Pd6 118.3(8) . . ? N3 C15 C16 124.0(14) . . ? C106 N16 C103 115.8(12) . . ? C17 C16 C15 119.6(13) . . ? C16 C17 C18 119.9(14) . . ? C20 C18 C17 124.2(13) . . ? C20 C18 C19 120.9(12) . . ? C17 C18 C19 114.9(13) . . ? N3 C19 N4 118.5(12) . . ? N3 C19 C18 123.3(12) . . ? N4 C19 C18 118.2(12) . . ? C21 C20 C18 120.5(14) . . ? C20 C21 C22 118.5(13) . . ? N4 C22 C21 124.0(12) . . ? N4 C22 C23 111.2(12) . . ? C21 C22 C23 124.8(13) . . ? C26 C23 C24 117.3(13) . . ? C26 C23 C22 127.5(15) . . ? C24 C23 C22 115.1(12) . . ? C25 C24 C23 108.9(13) . . ? C25 C24 Pd1 135.9(12) . . ? C23 C24 Pd1 113.8(10) . . ? C25 C24 Pd2 95.1(9) . . ? C23 C24 Pd2 118.2(10) . . ? Pd1 C24 Pd2 74.2(5) . . ? C24 C25 C27 132.8(15) . . ? C24 C25 S2 110.9(12) . . ? C27 C25 S2 116.1(11) . . ? C23 C26 C28 131.9(14) . . ? C23 C26 S2 106.9(13) . . ? C28 C26 S2 121.1(11) . . ? N5 C29 C30 125.1(13) . . ? C29 C30 C31 117.6(14) . . ? C30 C31 C32 119.0(15) . . ? C33 C32 C31 119.6(13) . . ? C33 C32 C34 116.2(13) . . ? C31 C32 C34 124.1(14) . . ? N6 C33 N5 115.1(12) . . ? N6 C33 C32 123.9(12) . . ? N5 C33 C32 121.0(12) . . ? C35 C34 C32 119.7(14) . . ? C34 C35 C36 120.3(13) . . ? N6 C36 C35 123.4(13) . . ? N6 C36 C37 110.7(12) . . ? C35 C36 C37 125.9(12) . . ? C40 C37 C38 111.5(13) . . ? C40 C37 C36 129.2(14) . . ? C38 C37 C36 119.3(12) . . ? C39 C38 C37 115.1(13) . . ? C39 C38 Pd3 133.8(12) . . ? C37 C38 Pd3 111.0(10) . . ? C38 C39 C41 134.0(14) . . ? C38 C39 S3 107.6(12) . . ? C41 C39 S3 118.3(10) . . ? C37 C40 C42 130.9(15) . . ? C37 C40 S3 111.3(12) . . ? C42 C40 S3 117.8(10) . . ? N7 C43 C44 121.9(14) . . ? C45 C44 C43 119.4(14) . . ? C44 C45 C46 120.9(15) . . ? C47 C46 C48 117.7(14) . . ? C47 C46 C45 116.9(13) . . ? C48 C46 C45 125.4(14) . . ? C46 C47 N8 123.9(13) . . ? C46 C47 N7 121.4(13) . . ? N8 C47 N7 114.7(13) . . ? C49 C48 C46 118.3(15) . . ? C48 C49 C50 121.8(14) . . ? N8 C50 C49 121.4(12) . . ? N8 C50 C51 112.8(12) . . ? C49 C50 C51 125.7(12) . . ? C54 C51 C52 107.8(12) . . ? C54 C51 C50 125.3(12) . . ? C52 C51 C50 126.7(12) . . ? C53 C52 C51 116.3(12) . . ? C53 C52 Br1 120.9(10) . . ? C51 C52 Br1 122.9(10) . . ? C52 C53 C55 129.2(13) . . ? C52 C53 S4 109.1(10) . . ? C55 C53 S4 121.7(11) . . ? C51 C54 C56 126.6(12) . . ? C51 C54 S4 113.3(10) . . ? C56 C54 S4 120.1(10) . . ? N9 C57 C58 123.8(13) . . ? C57 C58 C59 117.8(13) . . ? C58 C59 C60 121.0(13) . . ? C61 C60 C59 117.3(12) . . ? C61 C60 C62 119.1(12) . . ? C59 C60 C62 123.6(13) . . ? N9 C61 C60 122.9(11) . . ? N9 C61 N10 116.8(12) . . ? C60 C61 N10 120.2(11) . . ? C63 C62 C60 121.8(12) . . ? C62 C63 C64 117.2(12) . . ? N10 C64 C63 124.5(12) . . ? N10 C64 C65 109.4(11) . . ? C63 C64 C65 125.9(11) . . ? C68 C65 C66 114.2(12) . . ? C68 C65 C64 126.8(12) . . ? C66 C65 C64 119.1(11) . . ? C67 C66 C65 113.9(12) . . ? C67 C66 Pd5 134.4(11) . . ? C65 C66 Pd5 111.5(9) . . ? C66 C67 C69 135.1(12) . . ? C66 C67 S5 109.5(11) . . ? C69 C67 S5 115.4(10) . . ? C65 C68 C70 134.0(12) . . ? C65 C68 S5 108.9(10) . . ? C70 C68 S5 117.2(9) . . ? N11 C71 C72 123.9(13) . . ? C73 C72 C71 119.3(13) . . ? C72 C73 C74 118.1(13) . . ? C75 C74 C76 119.5(13) . . ? C75 C74 C73 118.7(14) . . ? C76 C74 C73 121.8(13) . . ? N11 C75 C74 121.9(13) . . ? N11 C75 N12 117.0(12) . . ? C74 C75 N12 121.0(13) . . ? C77 C76 C74 117.9(13) . . ? C76 C77 C78 120.2(13) . . ? N12 C78 C77 123.5(12) . . ? N12 C78 C79 116.0(12) . . ? C77 C78 C79 120.4(13) . . ? C82 C79 C80 113.9(12) . . ? C82 C79 C78 131.7(14) . . ? C80 C79 C78 114.1(12) . . ? C81 C80 C79 113.8(12) . . ? C81 C80 Pd4 132.3(10) . . ? C79 C80 Pd4 112.9(9) . . ? C80 C81 C83 136.0(13) . . ? C80 C81 S6 108.6(10) . . ? C83 C81 S6 115.1(10) . . ? C79 C82 C84 132.0(13) . . ? C79 C82 S6 108.6(11) . . ? C84 C82 S6 119.1(10) . . ? N13 C85 C86 122.1(17) . . ? C87 C86 C85 123(2) . . ? C86 C87 C88 115.5(18) . . ? C90 C88 C87 124.2(18) . . ? C90 C88 C89 114.3(17) . . ? C87 C88 C89 121.4(16) . . ? N13 C89 N14 117.2(14) . . ? N13 C89 C88 120.5(16) . . ? N14 C89 C88 122.3(15) . . ? C91 C90 C88 123.6(18) . . ? C90 C91 C92 119.3(17) . . ? N14 C92 C91 119.6(17) . . ? N14 C92 C93 114.9(15) . . ? C91 C92 C93 125.3(16) . . ? C96 C93 C92 129.7(15) . . ? C96 C93 C94 114.1(14) . . ? C92 C93 C94 116.1(13) . . ? C95 C94 C93 113.6(12) . . ? C95 C94 Pd6 134.3(11) . . ? C93 C94 Pd6 112.1(10) . . ? C94 C95 C97 135.2(13) . . ? C94 C95 S7 108.5(11) . . ? C97 C95 S7 116.3(11) . . ? C93 C96 C98 132.6(16) . . ? C93 C96 S7 109.8(12) . . ? C98 C96 S7 117.5(12) . . ? N15 C99 C100 123.2(13) . . ? C101 C100 C99 119.3(13) . . ? C100 C101 C102 119.2(14) . . ? C103 C102 C101 119.6(13) . . ? C103 C102 C104 116.7(12) . . ? C101 C102 C104 123.7(13) . . ? N16 C103 N15 114.0(12) . . ? N16 C103 C102 126.2(12) . . ? N15 C103 C102 119.8(12) . . ? C105 C104 C102 117.1(13) . . ? C104 C105 C106 121.7(13) . . ? N16 C106 C105 122.4(12) . . ? N16 C106 C107 113.3(12) . . ? C105 C106 C107 124.3(12) . . ? C110 C107 C108 109.7(12) . . ? C110 C107 C106 122.8(12) . . ? C108 C107 C106 127.5(12) . . ? C109 C108 C107 115.8(12) . . ? C109 C108 Br2 119.5(10) . . ? C107 C108 Br2 124.5(10) . . ? C108 C109 C111 129.8(13) . . ? C108 C109 S8 109.2(9) . . ? C111 C109 S8 120.8(10) . . ? C107 C110 C112 132.0(13) . . ? C107 C110 S8 112.5(10) . . ? C112 C110 S8 115.6(10) . . ? F1A B1A F2A 110.0(18) . . ? F1A B1A F3A 111(2) . . ? F2A B1A F3A 110.1(18) . . ? F1A B1A F4A 108.6(18) . . ? F2A B1A F4A 111(2) . . ? F3A B1A F4A 106.9(18) . . ? F5A B2A F7A 111.7(16) . . ? F5A B2A F8A 109.6(18) . . ? F7A B2A F8A 110.5(15) . . ? F5A B2A F6A 110.0(16) . . ? F7A B2A F6A 108.1(17) . . ? F8A B2A F6A 106.8(15) . . ? F10A B3A F11A 113.0(14) . . ? F10A B3A F12A 111.3(13) . . ? F11A B3A F12A 110.5(14) . . ? F10A B3A F9A 108.4(14) . . ? F11A B3A F9A 106.7(12) . . ? F12A B3A F9A 106.5(12) . . ? F13A B4A F15A 112.4(14) . . ? F13A B4A F14A 109.3(13) . . ? F15A B4A F14A 108.7(13) . . ? F13A B4A F16A 110.2(12) . . ? F15A B4A F16A 107.9(12) . . ? F14A B4A F16A 108.3(13) . . ? F19A B5A F17A 110.2(14) . . ? F19A B5A F18A 107.3(15) . . ? F17A B5A F18A 106.0(16) . . ? F19A B5A F20A 113.6(16) . . ? F17A B5A F20A 109.2(15) . . ? F18A B5A F20A 110.2(13) . . ? F22A B6A F21A 106.3(14) . . ? F22A B6A F23A 118.7(16) . . ? F21A B6A F23A 122.1(17) . . ? F22A B6A F24A 107.1(16) . . ? F21A B6A F24A 105.4(15) . . ? F23A B6A F24A 94.7(14) . . ? C6S C1S C2S 119.8(15) . . ? C3S C2S C1S 119.7(15) . . ? C2S C3S C4S 121.0(15) . . ? C3S C4S C5S 119.7(15) . . ? C6S C5S C4S 118.6(15) . . ? C5S C6S C1S 121.2(15) . . ? 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 0.000 0.000 0.000 184 143 ' ' 2 0.822 0.013 0.553 10 14 ' ' 3 0.385 0.141 0.527 94 66 ' ' 4 0.222 0.097 0.008 8 2 ' ' 5 0.305 0.189 0.005 17 9 ' ' 6 0.676 0.231 0.121 7 2 ' ' 7 0.176 0.268 0.621 7 2 ' ' 8 0.885 0.359 1.027 94 67 ' ' 9 0.804 0.313 0.505 17 10 ' ' 10 0.500 0.500 0.500 184 144 ' ' 11 0.721 0.405 0.508 8 2 ' ' 12 0.322 0.487 0.053 10 14 ' ' 13 0.678 0.513 0.947 10 11 ' ' 14 0.115 0.641 0.973 94 72 ' ' 15 0.278 0.597 0.492 8 3 ' ' 16 0.195 0.689 0.495 17 9 ' ' 17 0.824 0.731 0.379 7 3 ' ' 18 0.324 0.768 0.879 7 3 ' ' 19 0.615 0.859 0.473 94 73 ' ' 20 0.696 0.813 0.995 17 9 ' ' 21 0.779 0.904 0.992 8 3 ' ' 22 0.178 0.987 0.447 10 11 ' ' _platon_squeeze_details ; PLATON/SQUEEZE estimated the solvent-accessible region to contain a total of 672 electrons per unit cell. This amounts to 84 electrons per formula unit (z = 8). The electron densities were tentatively modeled as to two C6H6 molecules per formula unit. These solvent molecules were included in the molecular formula for the calculation of the intensive properties. ; _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.628 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.192 _iucr_refine_instructions_details ; TITL _compound_3 CELL 0.71073 22.4637 22.2278 25.7595 90.000 100.596 90.000 ZERR 8.0000 0.0037 0.0036 0.0044 0.000 0.004 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H B N O F S BR PD UNIT 472 376 24 64 8 96 32 8 24 MERG 2 SHEL 99999.00 0.85 FMAP 2 GRID PLAN 2 TEMP -173 SIZE 0.25 0.22 0.16 SADI B6A F21A B6A F22A B6A F23A B6A F24A DFIX 1.38 0.02 B6A F21A B6A F22A B6A F23A B6A F24A OMIT 2 1 4 OMIT -1 0 3 OMIT 1 4 1 OMIT 1 3 0 OMIT -3 5 3 OMIT -1 3 1 OMIT 3 3 1 OMIT 3 3 0 OMIT -2 1 1 OMIT -1 5 2 OMIT 1 0 3 OMIT -1 1 4 OMIT 2 1 2 OMIT -3 1 3 OMIT -1 3 3 OMIT -3 1 1 OMIT 0 0 4 OMIT 3 1 1 OMIT -2 3 2 OMIT 2 3 1 OMIT 0 3 1 BLOC 1 L.S. 4 ACTA WGHT 0.08670 0.00000 0.00000 0.00000 0.00000 0.33330 FVAR 0.22023 Pd1 9 0.25277 0.93245 0.30808 11.00000 0.01857 0.02933 = 0.03573 -0.00619 0.01011 -0.00235 Br1 8 0.49734 0.53218 0.33981 11.00000 0.02075 0.04233 = 0.05507 0.00125 0.00384 0.00390 S1 7 0.47161 0.70065 0.30169 11.00000 0.01963 0.03356 = 0.03123 0.00254 0.00594 0.00167 N1 4 0.31813 0.95948 0.36774 11.00000 0.03863 0.02000 = 0.03809 -0.02177 0.02322 -0.00482 C1 1 0.30838 1.00973 0.39340 11.00000 0.02191 0.08569 = 0.04923 -0.00660 0.01601 0.00835 AFIX 43 H1 2 0.27626 1.03486 0.37676 11.00000 -1.20000 AFIX 0 Pd2 9 0.34445 0.86001 0.28226 11.00000 0.01768 0.03158 = 0.02111 -0.00425 0.00369 0.00029 Br2 8 0.51240 0.79882 0.12971 11.00000 0.01919 0.03883 = 0.03229 -0.00115 -0.00250 -0.00162 S2 7 0.34598 1.01866 0.18558 11.00000 0.02714 0.04256 = 0.07134 0.00695 0.02540 -0.00711 N2 4 0.37954 0.87634 0.36062 11.00000 0.02032 0.02032 = 0.02032 0.00000 0.00374 0.00000 C2 1 0.34159 1.02976 0.44375 11.00000 0.06769 0.03580 = 0.08664 -0.01108 0.02551 0.00842 AFIX 43 H2 2 0.33250 1.06623 0.45987 11.00000 -1.20000 AFIX 0 Pd3 9 0.26836 0.76829 0.29264 11.00000 0.01877 0.02792 = 0.02275 -0.00072 0.00407 0.00137 S3 7 0.09334 0.66499 0.28391 11.00000 0.02702 0.03617 = 0.07127 0.01318 0.00380 -0.00439 N3 4 0.12391 0.86125 0.29582 11.00000 0.03069 0.01623 = 0.02977 0.00012 0.01250 -0.00295 C3 1 0.38524 0.99372 0.46550 11.00000 0.06200 0.06753 = 0.03698 -0.03398 -0.00107 -0.00613 AFIX 43 H3 2 0.40793 1.00376 0.49925 11.00000 -1.20000 AFIX 0 Pd4 9 0.77216 0.41382 0.21486 11.00000 0.01514 0.03014 = 0.01795 -0.00128 -0.00017 0.00492 S4 7 0.35451 0.54271 0.20086 11.00000 0.03025 0.02938 = 0.02845 -0.00510 0.00842 -0.00346 N4 4 0.18615 0.91271 0.24536 11.00000 0.02365 0.01880 = 0.03831 -0.01539 0.01621 0.00094 C4 1 0.40040 0.93844 0.43967 11.00000 0.03867 0.06871 = 0.07602 -0.02129 0.01818 -0.01671 Pd5 9 0.67719 0.48697 0.22701 11.00000 0.02537 0.03212 = 0.01816 -0.00264 -0.00048 0.01039 S5 7 0.54454 0.64170 0.20333 11.00000 0.01606 0.03025 = 0.02955 -0.00018 0.00648 0.00456 N5 4 0.32044 0.84083 0.20431 11.00000 0.03567 0.02120 = 0.03944 0.00635 0.00742 -0.00383 C5 1 0.36439 0.92324 0.39036 11.00000 0.02417 0.04135 = 0.03035 0.01059 0.00205 0.00834 Pd6 9 0.75458 0.57727 0.22072 11.00000 0.02714 0.03167 = 0.02339 -0.00624 -0.00787 0.00540 S6 7 0.64069 0.31698 0.29920 11.00000 0.02602 0.04176 = 0.02511 0.01067 0.00290 -0.00022 N6 4 0.23805 0.78269 0.21373 11.00000 0.02353 0.00352 = 0.03476 0.00241 0.01088 0.00194 C6 1 0.44659 0.89519 0.46348 11.00000 0.04737 0.09843 = 0.02896 -0.01438 -0.00459 -0.01444 AFIX 43 H6 2 0.46843 0.90067 0.49840 11.00000 -1.20000 AFIX 0 S7 7 0.93039 0.67978 0.24117 11.00000 0.02565 0.04691 = 0.06661 -0.01452 -0.02082 0.00251 N7 4 0.29695 0.74799 0.37040 11.00000 0.01792 0.03142 = 0.02110 0.00934 0.01352 0.00505 C7 1 0.45734 0.84675 0.43398 11.00000 0.04186 0.07224 = 0.01813 -0.00763 -0.01635 0.00245 AFIX 43 H7 2 0.48805 0.81873 0.44801 11.00000 -1.20000 AFIX 0 S8 7 0.63418 0.80245 0.28162 11.00000 0.02115 0.02911 = 0.02604 -0.00203 -0.00107 -0.00565 N8 4 0.33650 0.66078 0.33790 11.00000 0.01695 0.03998 = 0.01144 -0.00329 0.00712 -0.00508 C8 1 0.42298 0.83785 0.38244 11.00000 0.02453 0.02920 = 0.04111 0.01496 -0.00891 -0.00738 N9 4 0.72032 0.39623 0.14273 11.00000 0.01677 0.02295 = 0.01778 0.00347 0.00141 0.00110 C9 1 0.43441 0.78895 0.34774 11.00000 0.02766 0.03122 = 0.01300 -0.00523 0.01150 -0.00399 N10 4 0.65139 0.47521 0.14714 11.00000 0.01175 0.03362 = 0.00943 -0.00136 -0.00196 -0.00284 C10 1 0.39714 0.78820 0.29551 11.00000 0.00561 0.03695 = 0.02568 0.00111 -0.00060 -0.00543 N11 4 0.89825 0.48487 0.26320 11.00000 0.01810 0.02049 = 0.02642 -0.00517 0.00032 0.01499 C11 1 0.41113 0.74086 0.26504 11.00000 0.00584 0.01808 = 0.04511 0.01027 0.01057 -0.00134 N12 4 0.82225 0.42477 0.28967 11.00000 0.01957 C12 1 0.47858 0.74620 0.35613 11.00000 0.00463 0.04632 = 0.05008 0.00083 0.00811 0.00009 N13 4 0.69266 0.50375 0.30593 11.00000 0.07694 0.02072 = 0.02021 -0.01029 0.00181 0.02522 C13 1 0.38768 0.71766 0.21106 11.00000 0.00487 0.05177 = 0.03107 -0.01255 0.00668 0.00307 AFIX 137 H13A 2 0.34398 0.71067 0.20688 11.00000 -1.50000 H13B 2 0.40810 0.67978 0.20580 11.00000 -1.50000 H13C 2 0.39550 0.74723 0.18490 11.00000 -1.50000 AFIX 0 N14 4 0.77546 0.56527 0.30223 11.00000 0.03176 0.03080 = 0.03492 -0.01563 -0.01216 0.02410 C14 1 0.52797 0.73169 0.40391 11.00000 0.03214 0.05360 = 0.02511 0.00490 0.01178 0.01576 AFIX 137 H14A 2 0.55144 0.76811 0.41510 11.00000 -1.50000 H14B 2 0.55488 0.70061 0.39423 11.00000 -1.50000 H14C 2 0.50917 0.71708 0.43297 11.00000 -1.50000 AFIX 0 N15 4 0.73626 0.59290 0.14097 11.00000 0.02514 0.01582 = 0.01675 0.00018 0.00494 0.00111 C15 1 0.07458 0.83010 0.29830 11.00000 0.03208 0.01700 = 0.03372 0.00265 0.01770 -0.00034 AFIX 43 H15 2 0.06972 0.81485 0.33172 11.00000 -1.20000 AFIX 0 N16 4 0.68378 0.67648 0.16110 11.00000 0.02389 0.01225 = 0.02093 -0.00733 -0.00561 -0.00476 C16 1 0.02998 0.81837 0.25574 11.00000 0.01934 0.03574 = 0.04455 -0.01143 0.01293 -0.00441 AFIX 43 H16 2 -0.00458 0.79560 0.26001 11.00000 -1.20000 AFIX 0 C17 1 0.03536 0.83946 0.20733 11.00000 0.03124 0.03475 = 0.03303 -0.00791 0.00906 -0.00493 AFIX 43 H17 2 0.00425 0.83196 0.17770 11.00000 -1.20000 AFIX 0 C18 1 0.08769 0.87282 0.20104 11.00000 0.02266 0.01728 = 0.03203 -0.00972 0.00375 0.00876 C19 1 0.13177 0.88098 0.24874 11.00000 0.02170 0.01991 = 0.02059 -0.00782 0.01138 0.00860 C20 1 0.09848 0.89469 0.15220 11.00000 0.02389 0.04994 = 0.02884 0.01200 0.00524 0.00477 AFIX 43 H20 2 0.06910 0.88856 0.12107 11.00000 -1.20000 AFIX 0 C21 1 0.14975 0.92397 0.14942 11.00000 0.03018 0.03608 = 0.02904 0.00409 0.00763 0.01561 AFIX 43 H21 2 0.15710 0.93903 0.11667 11.00000 -1.20000 AFIX 0 C22 1 0.19380 0.93221 0.19744 11.00000 0.01453 0.03117 = 0.03127 0.00038 0.01622 0.00548 C23 1 0.25308 0.96377 0.20072 11.00000 0.01959 0.02230 = 0.06414 0.00437 0.02377 -0.00271 C24 1 0.29236 0.96152 0.25175 11.00000 0.03394 0.02998 = 0.04244 0.00524 0.00912 0.00089 C25 1 0.34675 0.99216 0.24878 11.00000 0.02957 0.03285 = 0.06389 0.00120 0.02440 0.00392 C26 1 0.27599 0.99175 0.15918 11.00000 0.03339 0.02716 = 0.09612 0.00009 0.03974 -0.00129 C27 1 0.40075 1.00967 0.28976 11.00000 0.02206 0.05494 = 0.05215 -0.01533 0.00769 -0.01053 AFIX 137 H27A 2 0.38923 1.04181 0.31202 11.00000 -1.50000 H27B 2 0.43328 1.02394 0.27222 11.00000 -1.50000 H27C 2 0.41489 0.97466 0.31173 11.00000 -1.50000 AFIX 0 C28 1 0.24786 1.00367 0.10203 11.00000 0.03024 0.07051 = 0.06151 0.03178 0.03468 0.01074 AFIX 137 H28A 2 0.24810 0.96654 0.08155 11.00000 -1.50000 H28B 2 0.27124 1.03471 0.08766 11.00000 -1.50000 H28C 2 0.20605 1.01746 0.09989 11.00000 -1.50000 AFIX 0 C29 1 0.35471 0.86692 0.17317 11.00000 0.01012 0.03947 = 0.02951 -0.00092 -0.01371 0.00382 AFIX 43 H29 2 0.39007 0.88760 0.18992 11.00000 -1.20000 AFIX 0 C30 1 0.34254 0.86605 0.11854 11.00000 0.03936 AFIX 43 H30 2 0.36919 0.88439 0.09858 11.00000 -1.20000 AFIX 0 C31 1 0.28996 0.83739 0.09396 11.00000 0.03700 AFIX 43 H31 2 0.27968 0.83585 0.05652 11.00000 -1.20000 AFIX 0 C32 1 0.25222 0.81073 0.12519 11.00000 0.01965 0.04089 = 0.02725 -0.00105 0.00791 0.01518 C33 1 0.26953 0.81107 0.18028 11.00000 0.01967 C34 1 0.19569 0.78075 0.10420 11.00000 0.03802 0.03340 = 0.02043 -0.00785 -0.01515 0.02557 AFIX 43 H34 2 0.18064 0.78057 0.06723 11.00000 -1.20000 AFIX 0 C35 1 0.16510 0.75362 0.13672 11.00000 0.04275 0.03615 = 0.01461 -0.01677 0.00340 -0.00572 AFIX 43 H35 2 0.12781 0.73424 0.12307 11.00000 -1.20000 AFIX 0 C36 1 0.18737 0.75334 0.19103 11.00000 0.02321 0.01913 = 0.02704 -0.00055 -0.00448 -0.00093 C37 1 0.15983 0.72295 0.23083 11.00000 0.01766 0.01369 = 0.03434 0.00913 -0.00317 0.00774 C38 1 0.18899 0.72550 0.28486 11.00000 0.01325 0.03206 = 0.04519 0.00826 0.00120 0.01534 C39 1 0.15882 0.69568 0.32012 11.00000 0.03843 0.01130 = 0.05960 0.00467 0.01330 -0.00056 C40 1 0.10708 0.69015 0.22461 11.00000 0.02973 0.00896 = 0.06653 -0.00937 0.00651 -0.00391 C41 1 0.17184 0.68603 0.37933 11.00000 0.03321 0.06046 = 0.07359 0.02964 0.00842 -0.00797 AFIX 137 H41A 2 0.20947 0.66309 0.38923 11.00000 -1.50000 H41B 2 0.13836 0.66367 0.38981 11.00000 -1.50000 H41C 2 0.17612 0.72510 0.39726 11.00000 -1.50000 AFIX 0 C42 1 0.06131 0.67246 0.17407 11.00000 0.05348 0.02394 = 0.06962 0.01605 -0.01287 -0.00670 AFIX 137 H42A 2 0.03924 0.70833 0.15907 11.00000 -1.50000 H42B 2 0.03259 0.64283 0.18315 11.00000 -1.50000 H42C 2 0.08324 0.65506 0.14811 11.00000 -1.50000 AFIX 0 C43 1 0.28680 0.78279 0.41010 11.00000 0.03354 0.03741 = 0.01961 -0.00377 0.01728 0.00586 AFIX 43 H43 2 0.26390 0.81865 0.40226 11.00000 -1.20000 AFIX 0 C44 1 0.30867 0.76816 0.46231 11.00000 0.06255 0.04700 = 0.03025 -0.01218 0.01474 0.01801 AFIX 43 H44 2 0.30166 0.79417 0.48983 11.00000 -1.20000 AFIX 0 C45 1 0.34053 0.71582 0.47400 11.00000 0.07093 0.03878 = 0.02013 -0.00135 -0.00551 0.00462 AFIX 43 H45 2 0.35546 0.70563 0.50984 11.00000 -1.20000 AFIX 0 C46 1 0.35167 0.67622 0.43289 11.00000 0.04774 0.03588 = 0.01192 0.00446 0.00288 0.01753 C47 1 0.32919 0.69355 0.38169 11.00000 0.00987 0.04525 = 0.04013 0.00193 0.00773 -0.00817 C48 1 0.38420 0.62070 0.44074 11.00000 0.07607 0.04382 = 0.02110 0.00700 -0.00134 0.01601 AFIX 43 H48 2 0.40083 0.60696 0.47529 11.00000 -1.20000 AFIX 0 C49 1 0.39058 0.58883 0.39855 11.00000 0.02095 0.03249 = 0.03528 -0.00274 -0.00245 0.00007 AFIX 43 H49 2 0.41165 0.55160 0.40329 11.00000 -1.20000 AFIX 0 C50 1 0.36688 0.60877 0.34670 11.00000 0.02112 0.00922 = 0.02958 -0.01159 0.00080 0.00201 C51 1 0.37296 0.57725 0.29743 11.00000 0.02379 0.02316 = 0.03335 0.00383 0.01442 -0.00327 C52 1 0.42640 0.54414 0.28716 11.00000 0.02910 0.01214 = 0.02197 0.00930 0.00369 -0.00374 C53 1 0.42310 0.52265 0.23857 11.00000 0.02370 0.02839 = 0.02109 -0.00682 -0.00070 -0.00713 C54 1 0.33078 0.57789 0.25142 11.00000 0.01573 0.03330 = 0.02016 0.01388 0.00287 0.00125 C55 1 0.47003 0.48824 0.21538 11.00000 0.03740 0.02196 = 0.04642 -0.01848 0.02854 -0.00348 AFIX 137 H55A 2 0.50945 0.50811 0.22515 11.00000 -1.50000 H55B 2 0.45823 0.48727 0.17682 11.00000 -1.50000 H55C 2 0.47284 0.44703 0.22914 11.00000 -1.50000 AFIX 0 C56 1 0.26793 0.60608 0.24333 11.00000 0.03872 0.02380 = 0.01498 0.00195 0.00677 0.01117 AFIX 137 H56A 2 0.25160 0.60254 0.27596 11.00000 -1.50000 H56B 2 0.24113 0.58516 0.21466 11.00000 -1.50000 H56C 2 0.27063 0.64866 0.23417 11.00000 -1.50000 AFIX 0 C57 1 0.73929 0.35047 0.11512 11.00000 0.01564 0.05581 = 0.02516 0.00116 -0.00409 -0.00349 AFIX 43 H57 2 0.77331 0.32765 0.13161 11.00000 -1.20000 AFIX 0 C58 1 0.71243 0.33531 0.06512 11.00000 0.02562 0.03946 = 0.02264 -0.00972 0.00385 0.01479 AFIX 43 H58 2 0.72501 0.30083 0.04819 11.00000 -1.20000 AFIX 0 C59 1 0.66663 0.37143 0.03999 11.00000 0.02281 0.04696 = 0.01356 0.00005 0.01162 -0.00758 AFIX 43 H59 2 0.64840 0.36295 0.00447 11.00000 -1.20000 AFIX 0 C60 1 0.64658 0.41994 0.06547 11.00000 0.01803 C61 1 0.67251 0.42873 0.11777 11.00000 0.01533 0.00872 = 0.02917 0.00141 0.01502 -0.00109 C62 1 0.60210 0.45954 0.04142 11.00000 0.00552 0.04384 = 0.00858 -0.00273 -0.00174 0.00135 AFIX 43 H62 2 0.58414 0.45345 0.00544 11.00000 -1.20000 AFIX 0 C63 1 0.58378 0.50628 0.06770 11.00000 0.00580 0.02649 = 0.02218 -0.00175 -0.00490 -0.00214 AFIX 43 H63 2 0.55474 0.53433 0.05060 11.00000 -1.20000 AFIX 0 C64 1 0.60916 0.51184 0.12104 11.00000 0.01143 0.01142 = 0.02740 -0.00089 0.00735 -0.00457 C65 1 0.59097 0.55638 0.15853 11.00000 0.00797 0.02776 = 0.01342 0.00884 0.00241 0.00415 C66 1 0.62197 0.55694 0.21151 11.00000 0.01845 0.03447 = 0.01910 -0.00145 0.01230 0.00552 C67 1 0.60377 0.60156 0.24127 11.00000 0.01387 0.02719 = 0.03227 0.01540 0.00913 -0.00627 C68 1 0.54549 0.59891 0.14732 11.00000 0.02139 0.00945 = 0.02030 0.00429 0.00512 -0.00344 C69 1 0.62337 0.62345 0.29699 11.00000 0.01250 0.04781 = 0.02339 -0.00147 0.00190 0.01266 AFIX 137 H69A 2 0.61392 0.59282 0.32162 11.00000 -1.50000 H69B 2 0.60186 0.66077 0.30193 11.00000 -1.50000 H69C 2 0.66709 0.63102 0.30375 11.00000 -1.50000 AFIX 0 C70 1 0.49908 0.61414 0.09849 11.00000 0.01988 0.04918 = 0.02129 -0.00214 -0.00033 0.01055 AFIX 137 H70A 2 0.51986 0.62881 0.07068 11.00000 -1.50000 H70B 2 0.47174 0.64540 0.10715 11.00000 -1.50000 H70C 2 0.47567 0.57804 0.08609 11.00000 -1.50000 AFIX 0 C71 1 0.94949 0.51640 0.27559 11.00000 0.01910 0.04003 = 0.02729 0.01019 -0.00273 0.01708 AFIX 43 H71 2 0.96269 0.53872 0.24836 11.00000 -1.20000 AFIX 0 C72 1 0.98483 0.51854 0.32615 11.00000 0.01302 0.03395 = 0.04948 -0.00181 0.00342 0.00457 AFIX 43 H72 2 1.02147 0.54093 0.33252 11.00000 -1.20000 AFIX 0 C73 1 0.96611 0.48802 0.36651 11.00000 0.02418 0.03731 = 0.03964 -0.01365 -0.02104 0.01018 AFIX 43 H73 2 0.98981 0.48799 0.40109 11.00000 -1.20000 AFIX 0 C74 1 0.90954 0.45601 0.35499 11.00000 0.02149 0.02960 = 0.02104 -0.00485 -0.00817 0.01235 C75 1 0.87721 0.45612 0.30321 11.00000 0.02965 0.05363 = 0.00952 0.00448 -0.00162 0.01073 C76 1 0.88550 0.42492 0.39507 11.00000 0.02914 0.04595 = 0.01196 0.00602 -0.00526 0.01148 AFIX 43 H76 2 0.90676 0.42395 0.43053 11.00000 -1.20000 AFIX 0 C77 1 0.83221 0.39727 0.38111 11.00000 0.01736 0.03023 = 0.03475 0.00748 0.00867 0.01038 AFIX 43 H77 2 0.81501 0.37623 0.40686 11.00000 -1.20000 AFIX 0 C78 1 0.80075 0.39924 0.32721 11.00000 0.02137 0.02384 = 0.02193 -0.00640 -0.01338 0.01339 C79 1 0.74224 0.36911 0.31173 11.00000 0.02708 0.01790 = 0.02652 -0.00587 0.00446 0.01576 C80 1 0.71534 0.37696 0.25752 11.00000 0.01781 0.01797 = 0.01426 -0.00615 0.00437 0.00849 C81 1 0.66001 0.34946 0.24343 11.00000 0.02925 0.03177 = 0.01820 0.00635 -0.00416 0.00116 C82 1 0.70579 0.33914 0.34092 11.00000 0.02528 0.03956 = 0.02736 -0.01305 0.00163 0.00445 C83 1 0.61617 0.33607 0.19134 11.00000 0.02561 0.05029 = 0.01984 -0.00848 -0.01409 0.00664 AFIX 137 H83A 2 0.59937 0.37390 0.17545 11.00000 -1.50000 H83B 2 0.58320 0.31032 0.19849 11.00000 -1.50000 H83C 2 0.63806 0.31546 0.16693 11.00000 -1.50000 AFIX 0 C84 1 0.71611 0.31959 0.39736 11.00000 0.02423 0.04135 = 0.03372 0.01556 0.00906 0.00136 AFIX 137 H84A 2 0.75215 0.29394 0.40476 11.00000 -1.50000 H84B 2 0.68082 0.29697 0.40400 11.00000 -1.50000 H84C 2 0.72212 0.35505 0.42034 11.00000 -1.50000 AFIX 0 C85 1 0.65669 0.47508 0.33521 11.00000 0.07351 0.02456 = 0.03639 -0.00375 0.01060 0.02499 AFIX 43 H85 2 0.62302 0.45253 0.31762 11.00000 -1.20000 AFIX 0 C86 1 0.66781 0.47780 0.39075 11.00000 0.11891 0.05140 = 0.01726 -0.00225 0.00968 0.03133 AFIX 43 H86 2 0.64019 0.45846 0.40915 11.00000 -1.20000 AFIX 0 C87 1 0.71502 0.50610 0.41848 11.00000 0.08633 0.06417 = 0.03371 0.01145 0.01341 0.05093 AFIX 43 H87 2 0.72235 0.50728 0.45598 11.00000 -1.20000 AFIX 0 C88 1 0.75387 0.53449 0.38847 11.00000 0.05967 0.03513 = 0.03186 -0.01291 -0.01435 0.03780 C89 1 0.74085 0.53417 0.33210 11.00000 0.04174 0.02980 = 0.03019 -0.00221 -0.01152 0.02469 C90 1 0.80600 0.56609 0.41019 11.00000 0.09333 0.06392 = 0.04105 -0.00360 -0.00743 0.06810 AFIX 43 H90 2 0.81851 0.56574 0.44749 11.00000 -1.20000 AFIX 0 C91 1 0.84044 0.59783 0.38057 11.00000 0.04449 0.03490 = 0.05918 -0.00351 -0.02273 0.02579 AFIX 43 H91 2 0.87525 0.61933 0.39735 11.00000 -1.20000 AFIX 0 C92 1 0.82370 0.59810 0.32564 11.00000 0.04536 0.05907 = 0.03281 -0.00621 -0.01179 0.03808 C93 1 0.85679 0.62783 0.28942 11.00000 0.03261 0.01627 = 0.03875 -0.01520 -0.01014 0.00995 C94 1 0.83028 0.62300 0.23277 11.00000 0.02660 0.02660 = 0.02660 0.00000 0.00489 0.00000 C95 1 0.86444 0.64841 0.20101 11.00000 0.02463 0.03198 = 0.03238 0.00211 -0.02197 0.00915 C96 1 0.91020 0.65749 0.29954 11.00000 0.04047 0.05553 = 0.03039 -0.01119 -0.03043 0.01589 C97 1 0.85913 0.65591 0.14279 11.00000 0.02235 0.02943 = 0.04973 0.00528 -0.00824 -0.00844 AFIX 137 H97A 2 0.86045 0.61634 0.12626 11.00000 -1.50000 H97B 2 0.89278 0.68061 0.13550 11.00000 -1.50000 H97C 2 0.82066 0.67571 0.12837 11.00000 -1.50000 AFIX 0 C98 1 0.95201 0.67599 0.35120 11.00000 0.05058 0.04945 = 0.04802 -0.01080 -0.03715 -0.00847 AFIX 137 H98A 2 0.92807 0.69569 0.37452 11.00000 -1.50000 H98B 2 0.98291 0.70393 0.34331 11.00000 -1.50000 H98C 2 0.97171 0.64016 0.36871 11.00000 -1.50000 AFIX 0 C99 1 0.75385 0.55585 0.10630 11.00000 0.01193 0.04124 = 0.02816 0.00495 -0.00544 0.00248 AFIX 43 H99 2 0.77873 0.52256 0.11924 11.00000 -1.20000 AFIX 0 C100 1 0.73767 0.56341 0.05212 11.00000 0.01292 0.02714 = 0.04938 -0.01574 0.00381 -0.00277 AFIX 43 H100 2 0.75199 0.53627 0.02870 11.00000 -1.20000 AFIX 0 C101 1 0.70077 0.61049 0.03269 11.00000 0.00951 0.04302 = 0.04615 -0.01077 0.00553 -0.01086 AFIX 43 H101 2 0.68729 0.61499 -0.00428 11.00000 -1.20000 AFIX 0 C102 1 0.68322 0.65182 0.06799 11.00000 0.00298 0.03502 = 0.02177 0.00637 0.00192 -0.00026 C103 1 0.69996 0.64212 0.12237 11.00000 0.01144 0.03033 = 0.02137 0.00161 -0.00193 -0.00553 C104 1 0.64580 0.70293 0.05189 11.00000 0.00959 0.02807 = 0.03043 0.00562 -0.00156 0.01257 AFIX 43 H104 2 0.63130 0.71149 0.01564 11.00000 -1.20000 AFIX 0 C105 1 0.63182 0.73884 0.09075 11.00000 0.01483 0.02257 = 0.03668 0.00099 -0.00564 0.00122 AFIX 43 H105 2 0.60943 0.77470 0.08132 11.00000 -1.20000 AFIX 0 C106 1 0.64984 0.72410 0.14500 11.00000 0.00799 0.01672 = 0.01844 -0.00343 -0.00478 -0.00811 C107 1 0.63272 0.75921 0.18903 11.00000 0.01741 0.01700 = 0.02086 -0.01006 0.00654 -0.01042 C108 1 0.57727 0.79382 0.18845 11.00000 0.01459 0.01772 = 0.02992 0.01032 -0.00882 -0.00588 C109 1 0.57163 0.81977 0.23434 11.00000 0.02688 0.02649 = 0.01721 -0.00076 0.01028 0.00685 C110 1 0.66756 0.76164 0.23757 11.00000 0.03293 0.01523 = 0.03142 -0.00198 0.00645 -0.01029 C111 1 0.52033 0.85564 0.24823 11.00000 0.02966 AFIX 137 H11D 2 0.48215 0.83419 0.23628 11.00000 -1.50000 H11E 2 0.51865 0.89501 0.23089 11.00000 -1.50000 H11F 2 0.52661 0.86118 0.28659 11.00000 -1.50000 AFIX 0 C112 1 0.73006 0.73530 0.25995 11.00000 0.02857 AFIX 137 H11A 2 0.72579 0.69280 0.26872 11.00000 -1.50000 H11B 2 0.74812 0.75743 0.29189 11.00000 -1.50000 H11C 2 0.75622 0.73882 0.23357 11.00000 -1.50000 AFIX 0 F1A 6 0.96703 0.55316 0.16037 11.00000 0.04832 0.07057 = 0.04103 0.00140 0.01074 0.00758 B1A 3 0.96637 0.52829 0.11182 11.00000 0.05893 0.07066 = 0.08953 -0.03829 0.00257 0.00276 F2A 6 1.00388 0.56039 0.08520 11.00000 0.10685 0.15643 = 0.06640 0.03313 0.04163 0.02104 B2A 3 0.80259 0.18712 0.06415 11.00000 0.06426 0.04388 = 0.03942 0.00100 -0.01639 -0.01434 F3A 6 0.98449 0.46867 0.11672 11.00000 0.06227 0.08598 = 0.22500 -0.06632 0.04451 0.00216 B3A 3 0.45839 0.39879 0.06960 11.00000 0.03720 0.02158 = 0.04050 0.02128 -0.00870 0.01236 F4A 6 0.90734 0.52869 0.08404 11.00000 0.07748 0.20362 = 0.06764 -0.06112 -0.02395 0.02788 B4A 3 0.37921 0.02522 0.03495 11.00000 0.02689 F5A 6 0.79819 0.22136 0.10641 11.00000 0.12659 0.11052 = 0.02641 -0.02468 -0.01337 0.05334 B5A 3 0.29483 0.65223 0.08349 11.00000 0.02886 0.07716 = 0.02446 0.01280 0.01760 -0.00986 F6A 6 0.83146 0.21934 0.02923 11.00000 0.07327 0.07024 = 0.09458 0.03694 -0.00177 -0.03798 B6A 3 -0.02161 0.80610 0.06322 11.00000 0.41755 F7A 6 0.83487 0.13625 0.07826 11.00000 0.08109 0.04712 = 0.08428 0.02663 0.01308 0.01500 F8A 6 0.74526 0.17317 0.03700 11.00000 0.06590 0.11358 = 0.04456 0.01647 -0.01470 -0.04111 F9A 6 0.44432 0.46207 0.07197 11.00000 0.02905 0.04114 = 0.06347 -0.00335 0.01577 0.00295 F10A 6 0.50493 0.38583 0.10998 11.00000 0.01692 0.10029 = 0.04778 0.02398 -0.00399 0.01057 F11A 6 0.47241 0.38872 0.02103 11.00000 0.06672 0.06380 = 0.02331 -0.00774 0.01891 0.00681 F12A 6 0.40504 0.36708 0.07498 11.00000 0.03174 0.04156 = 0.03893 0.00381 0.00676 -0.00439 F13A 6 0.39874 0.05074 0.08233 11.00000 0.05658 0.10865 = 0.03573 -0.01114 0.00436 0.00325 F14A 6 0.33913 0.06405 0.00379 11.00000 0.03027 0.10710 = 0.03946 0.02527 0.01594 0.01762 F15A 6 0.35073 -0.02825 0.03878 11.00000 0.10400 0.03716 = 0.07635 -0.00613 0.06377 -0.01384 F16A 6 0.42838 0.01456 0.00924 11.00000 0.04157 F17A 6 0.35558 0.64836 0.09395 11.00000 0.03967 0.31622 = 0.04114 0.03272 0.01717 0.03286 F18A 6 0.27452 0.59983 0.05725 11.00000 0.17609 0.05838 = 0.08807 -0.03532 0.08399 -0.05994 F19A 6 0.27733 0.69788 0.05056 11.00000 0.15876 0.05927 = 0.04146 0.01504 0.05543 0.04693 F20A 6 0.27363 0.65617 0.13053 11.00000 0.03982 0.08724 = 0.02844 0.01511 0.00713 0.01330 F21A 6 0.03375 0.78814 0.08910 11.00000 0.09517 F22A 6 -0.03009 0.77918 0.01529 11.00000 0.14011 F23A 6 -0.04195 0.86326 0.06667 11.00000 0.20814 F24A 6 -0.06214 0.78114 0.09049 11.00000 0.16100 C1S 1 0.54196 0.25397 0.01493 11.00000 0.05333 0.04258 = 0.02243 0.00825 -0.01665 0.00461 AFIX 43 H1S 2 0.54926 0.29602 0.01805 11.00000 -1.20000 AFIX 0 C2S 1 0.58483 0.21620 -0.00019 11.00000 0.04399 0.03558 = 0.03231 0.00331 -0.00061 0.00233 AFIX 43 H2S 2 0.62151 0.23230 -0.00767 11.00000 -1.20000 AFIX 0 C3S 1 0.57419 0.15613 -0.00425 11.00000 0.03821 0.06288 = 0.01287 0.01974 0.00161 0.01892 AFIX 43 H3S 2 0.60373 0.13037 -0.01452 11.00000 -1.20000 AFIX 0 C4S 1 0.52135 0.13198 0.00626 11.00000 0.06183 0.03647 = 0.02694 0.00805 -0.00264 0.01587 AFIX 43 H4S 2 0.51480 0.08977 0.00392 11.00000 -1.20000 AFIX 0 C5S 1 0.47698 0.17009 0.02051 11.00000 0.05185 0.04750 = 0.04316 0.01066 -0.00500 -0.01454 AFIX 43 H5S 2 0.43959 0.15427 0.02661 11.00000 -1.20000 AFIX 0 C6S 1 0.48884 0.23037 0.02539 11.00000 0.02426 0.02852 = 0.03308 0.00461 -0.00854 0.00378 AFIX 43 H6S 2 0.45986 0.25640 0.03619 11.00000 -1.20000 AFIX 0 O1W 5 0.20904 0.90195 0.37080 11.00000 0.01867 0.03469 = 0.03259 0.00527 0.00601 -0.00165 O2W 5 0.83548 0.45259 0.17084 11.00000 0.01695 0.02985 = 0.02489 0.00998 0.00286 0.00925 HKLF 4 ; _database_code_depnum_ccdc_archive 'CCDC 940020' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H2 B2 F30 N), C52 H42 N12 Pd2, 2(C H2 Cl2)' _chemical_formula_sum 'C126 H50 B4 Cl4 F60 N14 Pd2' _chemical_formula_weight 3297.64 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.389(3) _cell_length_b 18.555(3) _cell_length_c 22.215(3) _cell_angle_alpha 100.835(2) _cell_angle_beta 103.159(2) _cell_angle_gamma 119.476(2) _cell_volume 6009.7(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8764 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 24.92 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3248 _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8204 _exptl_absorpt_correction_T_max 0.8900 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44041 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.03 _reflns_number_total 21075 _reflns_number_gt 14916 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ortep _computing_publication_material ciftab _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. All H-atoms were introduced in calculated positions and refined according to 'riding model', except hydrogens attached to nitrogen atoms in the anion, which were located and refined with restraints. For full information, see _iucr_refine_instructions_details. ; _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^)+(0.0826P)^2^+1.5737P] 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 21075 _refine_ls_number_parameters 1911 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.00414(2) 0.87949(2) 0.195601(17) 0.01837(10) Uani 1 1 d . . . N1 N -0.1001(2) 0.8842(2) 0.14717(18) 0.0176(8) Uani 1 1 d . . . C1 C -0.1076(3) 0.8866(3) 0.0861(2) 0.0226(11) Uani 1 1 d . . . H1 H -0.0660 0.8838 0.0689 0.027 Uiso 1 1 calc R . . Pd2 Pd -0.09014(3) 0.83031(3) 0.282522(19) 0.02511(11) Uani 1 1 d . . . N2 N -0.1513(2) 0.8835(2) 0.23398(18) 0.0181(8) Uani 1 1 d . . . C2 C -0.1731(3) 0.8930(3) 0.0471(2) 0.0225(11) Uani 1 1 d . . . H2 H -0.1777 0.8922 0.0034 0.027 Uiso 1 1 calc R . . N3 N -0.2109(3) 0.9169(3) 0.3783(2) 0.0332(11) Uani 1 1 d . . . C3 C -0.2311(3) 0.9004(3) 0.0731(2) 0.0251(11) Uani 1 1 d . . . H3 H -0.2759 0.9060 0.0477 0.030 Uiso 1 1 calc R . . N4 N 0.2224(3) 0.9925(3) 0.27733(19) 0.0255(9) Uani 1 1 d . . . C4 C -0.2248(3) 0.8997(3) 0.1365(2) 0.0207(10) Uani 1 1 d . . . N5 N 0.0959(3) 0.8494(3) 0.23837(18) 0.0209(9) Uani 1 1 d . . . C5 C -0.1594(3) 0.8884(3) 0.1724(2) 0.0177(10) Uani 1 1 d . . . N6 N -0.1051(3) 0.6240(3) 0.1842(2) 0.0302(10) Uani 1 1 d . . . C6 C -0.2791(3) 0.9120(3) 0.1682(2) 0.0254(11) Uani 1 1 d . . . H6 H -0.3248 0.9180 0.1449 0.031 Uiso 1 1 calc R . . N7 N -0.0539(3) 0.7655(3) 0.3351(2) 0.0359(11) Uani 1 1 d . . . C7 C -0.2659(3) 0.9152(3) 0.2306(2) 0.0246(11) Uani 1 1 d . . . H7 H -0.2991 0.9278 0.2527 0.029 Uiso 1 1 calc R . . N8 N 0.0950(3) 0.8840(3) 0.3846(2) 0.0328(11) Uani 1 1 d . . . C8 C -0.2016(3) 0.8997(3) 0.2643(2) 0.0226(11) Uani 1 1 d . . . N9 N 0.2265(3) 1.0722(3) 0.4263(2) 0.0383(11) Uani 1 1 d . . . C9 C -0.1831(3) 0.8967(3) 0.3284(2) 0.0259(11) Uani 1 1 d . . . N10 N 0.0906(2) 1.0128(2) 0.20127(18) 0.0194(8) Uani 1 1 d . . . C10 C -0.1280(4) 0.8682(4) 0.3509(3) 0.0327(12) Uani 1 1 d . . . N11 N 0.1253(2) 0.9579(2) 0.11901(18) 0.0184(8) Uani 1 1 d . . . C11 C -0.1220(5) 0.8711(5) 0.4151(3) 0.0577(19) Uani 1 1 d . . . H11 H -0.0893 0.8555 0.4431 0.069 Uiso 1 1 calc R . . N12 N 0.1035(3) 0.8090(3) 0.02518(19) 0.0256(9) Uani 1 1 d . . . C12 C -0.1730(5) 0.9010(5) 0.4295(3) 0.062(2) Uani 1 1 d . . . H12 H -0.1809 0.9097 0.4705 0.075 Uiso 1 1 calc R . . C13 C -0.2650(4) 0.9542(4) 0.3802(3) 0.0356(13) Uani 1 1 d . . . H13A H -0.3271 0.9101 0.3491 0.053 Uiso 1 1 calc R . . H13B H -0.2395 1.0069 0.3679 0.053 Uiso 1 1 calc R . . H13C H -0.2645 0.9704 0.4250 0.053 Uiso 1 1 calc R . . C14 C 0.3113(3) 1.0488(4) 0.3066(2) 0.0317(12) Uani 1 1 d . . . H14 H 0.3361 1.1094 0.3125 0.038 Uiso 1 1 calc R . . C15 C 0.3713(4) 1.0250(4) 0.3296(3) 0.0348(13) Uani 1 1 d . . . H15 H 0.4342 1.0684 0.3511 0.042 Uiso 1 1 calc R . . C16 C 0.3360(4) 0.9372(4) 0.3198(3) 0.0351(14) Uani 1 1 d . . . H16 H 0.3747 0.9186 0.3338 0.042 Uiso 1 1 calc R . . C17 C 0.2429(3) 0.8753(4) 0.2892(2) 0.0271(12) Uani 1 1 d . . . C18 C 0.1882(3) 0.9065(3) 0.2683(2) 0.0245(11) Uani 1 1 d . . . C19 C 0.1996(4) 0.7836(4) 0.2781(3) 0.0350(13) Uani 1 1 d . . . H19 H 0.2346 0.7607 0.2902 0.042 Uiso 1 1 calc R . . C20 C 0.1095(4) 0.7290(4) 0.2507(2) 0.0302(12) Uani 1 1 d . . . H20 H 0.0809 0.6679 0.2445 0.036 Uiso 1 1 calc R . . C21 C 0.0566(3) 0.7624(3) 0.2307(2) 0.0233(11) Uani 1 1 d . . . C22 C -0.0401(3) 0.7128(3) 0.2017(2) 0.0258(11) Uani 1 1 d . . . C23 C -0.0815(3) 0.7557(3) 0.1860(2) 0.0226(11) Uani 1 1 d . . . C24 C -0.1750(3) 0.6903(3) 0.1556(3) 0.0291(12) Uani 1 1 d . . . H24 H -0.2207 0.6994 0.1379 0.035 Uiso 1 1 calc R . . C25 C -0.1879(4) 0.6112(3) 0.1566(3) 0.0335(13) Uani 1 1 d . . . H25 H -0.2446 0.5563 0.1407 0.040 Uiso 1 1 calc R . . C26 C -0.0951(4) 0.5531(4) 0.1942(3) 0.0426(15) Uani 1 1 d . . . H26A H -0.0623 0.5436 0.1679 0.064 Uiso 1 1 calc R . . H26B H -0.1548 0.4985 0.1802 0.064 Uiso 1 1 calc R . . H26C H -0.0614 0.5699 0.2411 0.064 Uiso 1 1 calc R . . C27 C -0.1199(5) 0.6842(4) 0.3271(3) 0.0432(15) Uani 1 1 d . . . H27 H -0.1801 0.6625 0.3011 0.052 Uiso 1 1 calc R . . C28 C -0.1038(5) 0.6295(5) 0.3554(3) 0.0531(17) Uani 1 1 d . . . H28 H -0.1527 0.5731 0.3506 0.064 Uiso 1 1 calc R . . C29 C -0.0179(5) 0.6577(5) 0.3899(3) 0.0554(19) Uani 1 1 d . . . H29 H -0.0060 0.6202 0.4077 0.066 Uiso 1 1 calc R . . C30 C 0.0534(4) 0.7428(4) 0.3990(3) 0.0405(15) Uani 1 1 d . . . C31 C 0.0332(4) 0.7987(4) 0.3736(3) 0.0348(13) Uani 1 1 d . . . C32 C 0.1455(5) 0.7797(5) 0.4342(3) 0.0504(18) Uani 1 1 d . . . H32 H 0.1636 0.7445 0.4497 0.061 Uiso 1 1 calc R . . C33 C 0.2080(4) 0.8663(5) 0.4457(3) 0.0463(16) Uani 1 1 d . . . H33 H 0.2699 0.8915 0.4696 0.056 Uiso 1 1 calc R . . C34 C 0.1810(4) 0.9188(4) 0.4221(3) 0.0378(14) Uani 1 1 d . . . C35 C 0.2466(4) 1.0115(4) 0.4390(3) 0.0395(15) Uani 1 1 d . . . C36 C 0.3401(4) 1.0609(5) 0.4723(3) 0.0509(17) Uani 1 1 d . . . H36 H 0.3737 1.0379 0.4881 0.061 Uiso 1 1 calc R . . C37 C 0.3763(4) 1.1491(5) 0.4786(3) 0.0547(18) Uani 1 1 d . . . H37 H 0.4382 1.1963 0.4987 0.066 Uiso 1 1 calc R . . C38 C 0.3053(4) 1.1551(5) 0.4501(3) 0.0505(17) Uani 1 1 d . . . H38 H 0.3101 1.2076 0.4473 0.061 Uiso 1 1 calc R . . C39 C 0.1394(4) 1.0565(4) 0.3938(3) 0.0431(15) Uani 1 1 d . . . H39A H 0.1466 1.1131 0.3964 0.065 Uiso 1 1 calc R . . H39B H 0.0987 1.0268 0.4156 0.065 Uiso 1 1 calc R . . H39C H 0.1142 1.0189 0.3473 0.065 Uiso 1 1 calc R . . C40 C 0.1002(3) 1.0802(3) 0.2448(2) 0.0249(11) Uani 1 1 d . . . H40 H 0.0597 1.0674 0.2674 0.030 Uiso 1 1 calc R . . C41 C 0.1670(4) 1.1690(3) 0.2588(2) 0.0311(12) Uani 1 1 d . . . H41 H 0.1720 1.2150 0.2906 0.037 Uiso 1 1 calc R . . C42 C 0.2247(4) 1.1884(3) 0.2262(3) 0.0312(12) Uani 1 1 d . . . H42 H 0.2713 1.2482 0.2358 0.037 Uiso 1 1 calc R . . C43 C 0.2151(3) 1.1194(3) 0.1780(2) 0.0239(11) Uani 1 1 d . . . C44 C 0.1451(3) 1.0313(3) 0.1660(2) 0.0201(10) Uani 1 1 d . . . C45 C 0.2693(3) 1.1301(3) 0.1398(2) 0.0260(11) Uani 1 1 d . . . H45 H 0.3179 1.1876 0.1463 0.031 Uiso 1 1 calc R . . C46 C 0.2520(3) 1.0594(3) 0.0947(2) 0.0248(11) Uani 1 1 d . . . H46 H 0.2890 1.0667 0.0697 0.030 Uiso 1 1 calc R . . C47 C 0.1779(3) 0.9723(3) 0.0836(2) 0.0211(10) Uani 1 1 d . . . C48 C 0.1582(3) 0.8977(3) 0.0321(2) 0.0239(11) Uani 1 1 d . . . C49 C 0.1857(4) 0.8980(4) -0.0215(2) 0.0303(12) Uani 1 1 d . . . H49 H 0.2237 0.9490 -0.0303 0.036 Uiso 1 1 calc R . . C50 C 0.1479(4) 0.8103(4) -0.0599(3) 0.0362(14) Uani 1 1 d . . . H50 H 0.1553 0.7910 -0.0995 0.043 Uiso 1 1 calc R . . C51 C 0.0988(4) 0.7576(3) -0.0304(2) 0.0313(12) Uani 1 1 d . . . H51 H 0.0663 0.6948 -0.0459 0.038 Uiso 1 1 calc R . . C52 C 0.0686(4) 0.7754(3) 0.0736(3) 0.0321(12) Uani 1 1 d . . . H52A H 0.0181 0.7808 0.0733 0.048 Uiso 1 1 calc R . . H52B H 0.1163 0.8098 0.1177 0.048 Uiso 1 1 calc R . . H52C H 0.0479 0.7130 0.0624 0.048 Uiso 1 1 calc R . . F1A F 0.53656(18) 0.77786(17) 0.31171(14) 0.0300(7) Uani 1 1 d . . . N1A N 0.3058(3) 0.4960(3) 0.2259(2) 0.0229(9) Uani 1 1 d D . . H1A1 H 0.298(4) 0.449(3) 0.244(3) 0.048(17) Uiso 1 1 d D . . H1A2 H 0.271(3) 0.515(4) 0.243(3) 0.060(19) Uiso 1 1 d D . . C1A C 0.4073(3) 0.6587(3) 0.3188(2) 0.0242(11) Uani 1 1 d . . . B1A B 0.4093(4) 0.5770(4) 0.2733(3) 0.0224(12) Uani 1 1 d . . . F2A F 0.5235(2) 0.90084(18) 0.38091(14) 0.0362(7) Uani 1 1 d . . . N2A N 0.7168(3) 0.2005(3) 0.23119(19) 0.0206(9) Uani 1 1 d D . . H2A1 H 0.745(3) 0.235(3) 0.2052(19) 0.021(12) Uiso 1 1 d D . . H2A2 H 0.715(3) 0.1462(18) 0.217(2) 0.015(12) Uiso 1 1 d D . . C2A C 0.4677(3) 0.7489(3) 0.3332(2) 0.0265(11) Uani 1 1 d . . . B2A B 0.2556(4) 0.4451(4) 0.1465(3) 0.0211(12) Uani 1 1 d . . . F3A F 0.3948(2) 0.85620(19) 0.43428(14) 0.0383(7) Uani 1 1 d . . . C3A C 0.4642(3) 0.8149(3) 0.3710(2) 0.0273(11) Uani 1 1 d . . . B3A B 0.7987(4) 0.2605(4) 0.3039(3) 0.0222(12) Uani 1 1 d . . . F4A F 0.27586(19) 0.68295(19) 0.41400(14) 0.0344(7) Uani 1 1 d . . . C4A C 0.3993(4) 0.7930(3) 0.3981(2) 0.0289(12) Uani 1 1 d . . . B4A B 0.6114(4) 0.1658(4) 0.2035(3) 0.0227(12) Uani 1 1 d . . . F5A F 0.28548(18) 0.55624(17) 0.34245(14) 0.0299(7) Uani 1 1 d . . . C5A C 0.3387(3) 0.7051(3) 0.3874(2) 0.0263(11) Uani 1 1 d . . . F6A F 0.3188(2) 0.40422(18) 0.30869(15) 0.0341(7) Uani 1 1 d . . . C6A C 0.3457(3) 0.6422(3) 0.3496(2) 0.0253(11) Uani 1 1 d . . . F7A F 0.4007(2) 0.3726(2) 0.40244(16) 0.0460(9) Uani 1 1 d . . . C7A C 0.4505(3) 0.5465(3) 0.3308(2) 0.0246(11) Uani 1 1 d . . . F8A F 0.5785(2) 0.4928(2) 0.48114(15) 0.0497(9) Uani 1 1 d . . . C8A C 0.4078(3) 0.4687(3) 0.3448(2) 0.0280(12) Uani 1 1 d . . . F9A F 0.6694(2) 0.6508(2) 0.46460(16) 0.0507(9) Uani 1 1 d . . . C9A C 0.4486(4) 0.4510(4) 0.3936(3) 0.0347(13) Uani 1 1 d . . . F10A F 0.59041(19) 0.68509(19) 0.36892(15) 0.0381(7) Uani 1 1 d . . . C10A C 0.5364(4) 0.5101(4) 0.4328(3) 0.0366(14) Uani 1 1 d . . . F11A F 0.40050(18) 0.67831(18) 0.18855(14) 0.0301(7) Uani 1 1 d . . . C11A C 0.5822(4) 0.5899(4) 0.4249(3) 0.0371(13) Uani 1 1 d . . . F12A F 0.5058(2) 0.7403(2) 0.12046(15) 0.0429(8) Uani 1 1 d . . . C12A C 0.5400(4) 0.6053(4) 0.3749(3) 0.0326(12) Uani 1 1 d . . . F13A F 0.6306(2) 0.7021(2) 0.11810(17) 0.0484(9) Uani 1 1 d . . . C13A C 0.4703(3) 0.6086(3) 0.2281(2) 0.0228(11) Uani 1 1 d . . . F14A F 0.6462(2) 0.5976(2) 0.18424(18) 0.0508(9) Uani 1 1 d . . . C14A C 0.4623(3) 0.6582(3) 0.1902(2) 0.0267(11) Uani 1 1 d . . . F15A F 0.54548(19) 0.5378(2) 0.25360(15) 0.0356(7) Uani 1 1 d . . . C15A C 0.5150(4) 0.6900(3) 0.1542(3) 0.0331(13) Uani 1 1 d . . . F16A F 0.24020(19) 0.59945(18) 0.20653(14) 0.0310(7) Uani 1 1 d . . . C16A C 0.5777(4) 0.6705(3) 0.1528(3) 0.0340(13) Uani 1 1 d . . . F17A F 0.1572(2) 0.65766(19) 0.13836(15) 0.0373(7) Uani 1 1 d . . . C17A C 0.5863(3) 0.6192(4) 0.1866(3) 0.0341(13) Uani 1 1 d . . . F18A F 0.07414(19) 0.58033(19) 0.00408(15) 0.0384(8) Uani 1 1 d . . . C18A C 0.5340(3) 0.5899(3) 0.2236(3) 0.0297(12) Uani 1 1 d . . . F19A F 0.0721(2) 0.43888(19) -0.05929(14) 0.0381(7) Uani 1 1 d . . . C19A C 0.2068(3) 0.4874(3) 0.1105(2) 0.0216(10) Uani 1 1 d . . . F20A F 0.15296(18) 0.37647(18) 0.00804(13) 0.0284(6) Uani 1 1 d . . . C20A C 0.2017(3) 0.5581(3) 0.1407(2) 0.0245(11) Uani 1 1 d . . . F21A F 0.12898(18) 0.41020(17) 0.21299(14) 0.0289(7) Uani 1 1 d . . . C21A C 0.1582(3) 0.5893(3) 0.1060(3) 0.0265(11) Uani 1 1 d . . . F22A F -0.00240(19) 0.25581(19) 0.20853(14) 0.0343(7) Uani 1 1 d . . . C22A C 0.1162(3) 0.5506(3) 0.0386(3) 0.0273(12) Uani 1 1 d . . . F23A F -0.04017(18) 0.10008(17) 0.12861(14) 0.0320(7) Uani 1 1 d . . . C23A C 0.1159(3) 0.4785(3) 0.0066(2) 0.0279(12) Uani 1 1 d . . . F24A F 0.05507(19) 0.10587(17) 0.04993(14) 0.0329(7) Uani 1 1 d . . . C24A C 0.1582(3) 0.4490(3) 0.0422(2) 0.0240(11) Uani 1 1 d . . . F25A F 0.18759(19) 0.25751(18) 0.05414(14) 0.0319(7) Uani 1 1 d . . . C25A C 0.1700(3) 0.3441(3) 0.1370(2) 0.0204(10) Uani 1 1 d . . . F26A F 0.34790(18) 0.36502(18) 0.18988(14) 0.0301(7) Uani 1 1 d . . . C26A C 0.1155(3) 0.3350(3) 0.1731(2) 0.0224(11) Uani 1 1 d . . . F27A F 0.4483(2) 0.3292(2) 0.13819(16) 0.0406(8) Uani 1 1 d . . . C27A C 0.0466(3) 0.2574(3) 0.1715(2) 0.0241(11) Uani 1 1 d . . . F28A F 0.4769(2) 0.3712(2) 0.03041(18) 0.0498(9) Uani 1 1 d . . . C28A C 0.0262(3) 0.1788(3) 0.1306(2) 0.0249(11) Uani 1 1 d . . . F29A F 0.4080(2) 0.4596(2) -0.01863(15) 0.0399(8) Uani 1 1 d . . . C29A C 0.0746(3) 0.1819(3) 0.0912(2) 0.0252(11) Uani 1 1 d . . . F30A F 0.32340(18) 0.51032(18) 0.03938(14) 0.0292(7) Uani 1 1 d . . . C30A C 0.1443(3) 0.2626(3) 0.0954(2) 0.0222(11) Uani 1 1 d . . . F31A F 0.83453(18) 0.30598(18) 0.18029(13) 0.0274(6) Uani 1 1 d . . . C31A C 0.3255(3) 0.4351(3) 0.1157(2) 0.0216(10) Uani 1 1 d . . . F32A F 0.98349(19) 0.43853(19) 0.18252(14) 0.0324(7) Uani 1 1 d . . . C32A C 0.3628(3) 0.3919(3) 0.1384(2) 0.0251(11) Uani 1 1 d . . . F33A F 1.1212(2) 0.5618(2) 0.29825(16) 0.0441(8) Uani 1 1 d . . . C33A C 0.4149(3) 0.3720(3) 0.1125(3) 0.0286(12) Uani 1 1 d . . . F34A F 1.1060(2) 0.5410(2) 0.41524(15) 0.0476(9) Uani 1 1 d . . . C34A C 0.4300(4) 0.3939(3) 0.0585(3) 0.0343(13) Uani 1 1 d . . . F35A F 0.9584(2) 0.40450(19) 0.41474(13) 0.0365(7) Uani 1 1 d . . . C35A C 0.3956(3) 0.4375(3) 0.0341(3) 0.0289(12) Uani 1 1 d . . . F36A F 0.86736(19) 0.25019(19) 0.43991(13) 0.0306(7) Uani 1 1 d . . . C36A C 0.3481(3) 0.4605(3) 0.0646(2) 0.0254(11) Uani 1 1 d . . . F37A F 0.95351(19) 0.1739(2) 0.46869(14) 0.0342(7) Uani 1 1 d . . . C37A C 0.8859(3) 0.3474(3) 0.2988(2) 0.0220(10) Uani 1 1 d . . . F38A F 0.99060(19) 0.09480(19) 0.37457(15) 0.0344(7) Uani 1 1 d . . . C38A C 0.8987(3) 0.3612(3) 0.2413(2) 0.0227(11) Uani 1 1 d . . . F39A F 0.92983(18) 0.08696(18) 0.24848(14) 0.0281(6) Uani 1 1 d . . . C39A C 0.9770(3) 0.4304(3) 0.2405(3) 0.0279(12) Uani 1 1 d . . . F40A F 0.83475(17) 0.15430(17) 0.21582(12) 0.0245(6) Uani 1 1 d . . . C40A C 1.0470(3) 0.4925(3) 0.2989(3) 0.0314(12) Uani 1 1 d . . . F41A F 0.68352(19) 0.14277(19) 0.36132(14) 0.0324(7) Uani 1 1 d . . . C41A C 1.0381(3) 0.4826(3) 0.3567(3) 0.0325(12) Uani 1 1 d . . . F42A F 0.6093(2) 0.1799(3) 0.44119(16) 0.0507(9) Uani 1 1 d . . . C42A C 0.9604(4) 0.4107(3) 0.3553(2) 0.0293(12) Uani 1 1 d . . . F43A F 0.6402(3) 0.3446(3) 0.48174(18) 0.0708(13) Uani 1 1 d . . . C43A C 0.8435(3) 0.2055(3) 0.3250(2) 0.0216(10) Uani 1 1 d . . . F44A F 0.7496(3) 0.4708(3) 0.44038(18) 0.0694(12) Uani 1 1 d . . . C44A C 0.8778(3) 0.2076(3) 0.3886(2) 0.0225(11) Uani 1 1 d . . . F45A F 0.8238(2) 0.4365(2) 0.36109(15) 0.0399(8) Uani 1 1 d . . . C45A C 0.9242(3) 0.1702(3) 0.4061(2) 0.0244(11) Uani 1 1 d . . . F46A F 0.65660(17) 0.03810(17) 0.24384(13) 0.0262(6) Uani 1 1 d . . . C46A C 0.9425(3) 0.1293(3) 0.3582(2) 0.0258(11) Uani 1 1 d . . . F47A F 0.53969(19) -0.11832(18) 0.24315(14) 0.0313(7) Uani 1 1 d . . . C47A C 0.9118(3) 0.1254(3) 0.2953(2) 0.0240(11) Uani 1 1 d . . . F48A F 0.36019(19) -0.18360(19) 0.20391(15) 0.0382(7) Uani 1 1 d . . . C48A C 0.8631(3) 0.1619(3) 0.2797(2) 0.0188(10) Uani 1 1 d . . . F49A F 0.30131(18) -0.0857(2) 0.16104(15) 0.0388(8) Uani 1 1 d . . . C49A C 0.7589(3) 0.2871(3) 0.3566(2) 0.0265(11) Uani 1 1 d . . . F50A F 0.41862(18) 0.0735(2) 0.16205(14) 0.0331(7) Uani 1 1 d . . . C50A C 0.7032(3) 0.2259(4) 0.3801(2) 0.0296(12) Uani 1 1 d . . . F51A F 0.5049(2) 0.1692(2) 0.29218(15) 0.0365(7) Uani 1 1 d . . . C51A C 0.6642(4) 0.2439(4) 0.4223(3) 0.0397(14) Uani 1 1 d . . . F52A F 0.4955(3) 0.3042(3) 0.34170(18) 0.0633(11) Uani 1 1 d . . . C52A C 0.6797(5) 0.3266(5) 0.4431(3) 0.0472(17) Uani 1 1 d . . . F53A F 0.5923(3) 0.4600(3) 0.32388(19) 0.0705(13) Uani 1 1 d . . . C53A C 0.7349(5) 0.3899(4) 0.4225(3) 0.0467(16) Uani 1 1 d . . . F54A F 0.6937(3) 0.4751(2) 0.24813(16) 0.0499(9) Uani 1 1 d . . . C54A C 0.7729(4) 0.3699(4) 0.3803(2) 0.0316(12) Uani 1 1 d . . . F55A F 0.70385(19) 0.34009(18) 0.19739(14) 0.0306(7) Uani 1 1 d . . . C55A C 0.5449(3) 0.0685(3) 0.2071(2) 0.0234(11) Uani 1 1 d . . . F56A F 0.49243(19) 0.2089(2) 0.11724(14) 0.0332(7) Uani 1 1 d . . . C56A C 0.5692(3) 0.0131(3) 0.2253(2) 0.0245(11) Uani 1 1 d . . . F57A F 0.44796(19) 0.17521(19) -0.01014(14) 0.0352(7) Uani 1 1 d . . . C57A C 0.5096(3) -0.0701(3) 0.2241(2) 0.0252(11) Uani 1 1 d . . . F58A F 0.50881(19) 0.09777(19) -0.08106(13) 0.0351(7) Uani 1 1 d . . . C58A C 0.4186(3) -0.1036(3) 0.2039(2) 0.0281(12) Uani 1 1 d . . . F59A F 0.61531(18) 0.04957(18) -0.01964(13) 0.0305(7) Uani 1 1 d . . . C59A C 0.3900(3) -0.0535(3) 0.1828(2) 0.0277(12) Uani 1 1 d . . . F60A F 0.65952(17) 0.07822(17) 0.10891(13) 0.0251(6) Uani 1 1 d . . . C60A C 0.4518(3) 0.0284(3) 0.1840(2) 0.0273(12) Uani 1 1 d . . . C61A C 0.6029(3) 0.2454(3) 0.2396(2) 0.0241(11) Uani 1 1 d . . . C62A C 0.5517(4) 0.2422(4) 0.2774(3) 0.0318(13) Uani 1 1 d . . . C63A C 0.5449(4) 0.3117(4) 0.3038(3) 0.0435(16) Uani 1 1 d . . . C64A C 0.5928(5) 0.3902(4) 0.2949(3) 0.0485(17) Uani 1 1 d . . . C65A C 0.6462(4) 0.3989(4) 0.2584(3) 0.0370(14) Uani 1 1 d . . . C66A C 0.6498(3) 0.3276(3) 0.2326(2) 0.0265(11) Uani 1 1 d . . . C67A C 0.5823(3) 0.1489(3) 0.1227(2) 0.0208(10) Uani 1 1 d . . . C68A C 0.5264(3) 0.1692(3) 0.0871(2) 0.0245(11) Uani 1 1 d . . . C69A C 0.5026(3) 0.1533(3) 0.0203(2) 0.0280(12) Uani 1 1 d . . . C70A C 0.5330(3) 0.1139(3) -0.0158(2) 0.0261(11) Uani 1 1 d . . . C71A C 0.5870(3) 0.0912(3) 0.0152(2) 0.0250(11) Uani 1 1 d . . . C72A C 0.6090(3) 0.1077(3) 0.0823(2) 0.0222(11) Uani 1 1 d . . . Cl1S Cl 0.27561(14) 0.74105(14) 0.03294(14) 0.0955(8) Uani 1 1 d . . . C1S C 0.3244(6) 0.6816(6) 0.0229(5) 0.101(3) Uani 1 1 d . . . H1S1 H 0.3895 0.7226 0.0501 0.121 Uiso 1 1 calc R . . H1S2 H 0.2994 0.6353 0.0424 0.121 Uiso 1 1 calc R . . Cl2S Cl 0.3148(2) 0.63306(14) -0.05092(12) 0.1203(11) Uani 1 1 d . . . C2S C 0.2000(5) 0.3815(5) 0.4302(3) 0.081(3) Uani 1 1 d . . . H2S1 H 0.2276 0.4456 0.4513 0.097 Uiso 1 1 calc R . . H2S2 H 0.2487 0.3729 0.4289 0.097 Uiso 1 1 calc R . . Cl3S Cl 0.14396(14) 0.32389(18) 0.47709(11) 0.1194(11) Uani 1 1 d . . . Cl4S Cl 0.12461(11) 0.34342(11) 0.34976(8) 0.0540(4) 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 0.0197(2) 0.0204(2) 0.0225(2) 0.01106(16) 0.01143(16) 0.01365(17) N1 0.018(2) 0.016(2) 0.021(2) 0.0050(17) 0.0101(17) 0.0094(17) C1 0.022(3) 0.020(3) 0.022(3) 0.006(2) 0.009(2) 0.010(2) Pd2 0.0310(2) 0.0305(2) 0.0267(2) 0.01568(18) 0.01696(18) 0.0213(2) N2 0.017(2) 0.016(2) 0.022(2) 0.0061(17) 0.0106(17) 0.0091(17) C2 0.027(3) 0.021(3) 0.020(2) 0.007(2) 0.010(2) 0.013(2) N3 0.034(3) 0.050(3) 0.024(2) 0.011(2) 0.018(2) 0.027(2) C3 0.023(3) 0.024(3) 0.027(3) 0.008(2) 0.004(2) 0.014(2) N4 0.020(2) 0.032(2) 0.029(2) 0.017(2) 0.0116(19) 0.016(2) C4 0.018(2) 0.014(2) 0.029(3) 0.007(2) 0.009(2) 0.008(2) N5 0.024(2) 0.026(2) 0.021(2) 0.0105(18) 0.0106(18) 0.0177(19) C5 0.016(2) 0.012(2) 0.026(3) 0.007(2) 0.009(2) 0.008(2) N6 0.040(3) 0.019(2) 0.039(3) 0.016(2) 0.021(2) 0.018(2) C6 0.021(3) 0.025(3) 0.031(3) 0.009(2) 0.010(2) 0.013(2) N7 0.056(3) 0.049(3) 0.031(3) 0.025(2) 0.027(2) 0.041(3) C7 0.018(3) 0.023(3) 0.034(3) 0.007(2) 0.014(2) 0.012(2) N8 0.041(3) 0.053(3) 0.026(2) 0.023(2) 0.019(2) 0.035(3) C8 0.019(2) 0.013(2) 0.032(3) 0.006(2) 0.013(2) 0.006(2) N9 0.043(3) 0.056(3) 0.027(2) 0.016(2) 0.015(2) 0.034(3) C9 0.025(3) 0.028(3) 0.028(3) 0.010(2) 0.016(2) 0.015(2) N10 0.019(2) 0.023(2) 0.024(2) 0.0120(18) 0.0111(17) 0.0142(18) C10 0.032(3) 0.043(3) 0.028(3) 0.014(3) 0.018(2) 0.022(3) N11 0.022(2) 0.025(2) 0.021(2) 0.0135(18) 0.0108(17) 0.0188(19) C11 0.080(5) 0.101(6) 0.046(4) 0.048(4) 0.042(4) 0.071(5) N12 0.032(2) 0.027(2) 0.022(2) 0.0064(18) 0.0095(19) 0.019(2) C12 0.087(5) 0.108(6) 0.038(4) 0.036(4) 0.045(4) 0.072(5) C13 0.028(3) 0.040(3) 0.034(3) 0.003(3) 0.018(3) 0.017(3) C14 0.026(3) 0.044(3) 0.029(3) 0.021(3) 0.013(2) 0.017(3) C15 0.028(3) 0.057(4) 0.033(3) 0.029(3) 0.019(2) 0.025(3) C16 0.032(3) 0.066(4) 0.036(3) 0.034(3) 0.022(3) 0.037(3) C17 0.031(3) 0.044(3) 0.026(3) 0.022(2) 0.018(2) 0.028(3) C18 0.021(3) 0.040(3) 0.025(3) 0.019(2) 0.013(2) 0.021(2) C19 0.047(4) 0.053(4) 0.036(3) 0.030(3) 0.024(3) 0.040(3) C20 0.045(3) 0.035(3) 0.031(3) 0.019(3) 0.022(3) 0.031(3) C21 0.033(3) 0.032(3) 0.023(3) 0.014(2) 0.015(2) 0.026(3) C22 0.028(3) 0.022(3) 0.029(3) 0.010(2) 0.014(2) 0.014(2) C23 0.026(3) 0.024(3) 0.026(3) 0.011(2) 0.016(2) 0.016(2) C24 0.030(3) 0.026(3) 0.040(3) 0.017(2) 0.018(2) 0.017(2) C25 0.034(3) 0.019(3) 0.048(3) 0.015(3) 0.021(3) 0.012(2) C26 0.056(4) 0.027(3) 0.048(4) 0.015(3) 0.017(3) 0.026(3) C27 0.065(4) 0.042(4) 0.036(3) 0.025(3) 0.025(3) 0.033(3) C28 0.077(5) 0.056(4) 0.049(4) 0.036(3) 0.031(4) 0.044(4) C29 0.112(6) 0.062(5) 0.044(4) 0.039(4) 0.045(4) 0.069(5) C30 0.069(4) 0.063(4) 0.031(3) 0.028(3) 0.034(3) 0.054(4) C31 0.052(4) 0.059(4) 0.025(3) 0.027(3) 0.025(3) 0.044(3) C32 0.088(5) 0.093(6) 0.040(4) 0.043(4) 0.044(4) 0.082(5) C33 0.056(4) 0.085(5) 0.037(3) 0.034(3) 0.027(3) 0.056(4) C34 0.050(4) 0.070(4) 0.025(3) 0.025(3) 0.027(3) 0.047(4) C35 0.046(4) 0.071(4) 0.027(3) 0.023(3) 0.019(3) 0.045(4) C36 0.048(4) 0.089(6) 0.026(3) 0.020(3) 0.012(3) 0.046(4) C37 0.038(4) 0.071(5) 0.039(4) 0.013(4) 0.007(3) 0.025(4) C38 0.044(4) 0.059(4) 0.030(3) 0.005(3) 0.008(3) 0.022(4) C39 0.045(4) 0.054(4) 0.040(3) 0.018(3) 0.013(3) 0.035(3) C40 0.026(3) 0.029(3) 0.029(3) 0.012(2) 0.012(2) 0.020(2) C41 0.043(3) 0.021(3) 0.030(3) 0.006(2) 0.008(3) 0.021(3) C42 0.039(3) 0.019(3) 0.034(3) 0.013(2) 0.009(3) 0.016(3) C43 0.022(3) 0.021(3) 0.028(3) 0.012(2) 0.007(2) 0.011(2) C44 0.019(2) 0.022(3) 0.026(3) 0.014(2) 0.008(2) 0.015(2) C45 0.021(3) 0.023(3) 0.026(3) 0.015(2) 0.004(2) 0.007(2) C46 0.025(3) 0.031(3) 0.029(3) 0.019(2) 0.016(2) 0.018(2) C47 0.020(2) 0.024(3) 0.025(3) 0.014(2) 0.008(2) 0.014(2) C48 0.026(3) 0.027(3) 0.029(3) 0.016(2) 0.013(2) 0.018(2) C49 0.036(3) 0.041(3) 0.031(3) 0.020(3) 0.021(2) 0.027(3) C50 0.057(4) 0.050(4) 0.031(3) 0.020(3) 0.026(3) 0.043(3) C51 0.042(3) 0.026(3) 0.031(3) 0.005(2) 0.010(3) 0.025(3) C52 0.040(3) 0.018(3) 0.039(3) 0.012(2) 0.022(3) 0.013(3) F1A 0.0278(16) 0.0206(15) 0.0380(17) 0.0113(13) 0.0129(14) 0.0104(13) N1A 0.020(2) 0.021(2) 0.026(2) 0.0094(19) 0.0107(18) 0.0093(19) C1A 0.023(3) 0.026(3) 0.029(3) 0.014(2) 0.012(2) 0.016(2) B1A 0.016(3) 0.020(3) 0.030(3) 0.011(2) 0.010(2) 0.008(2) F2A 0.0444(19) 0.0177(15) 0.0396(18) 0.0107(13) 0.0141(15) 0.0133(15) N2A 0.020(2) 0.023(2) 0.022(2) 0.0091(18) 0.0108(18) 0.0127(19) C2A 0.026(3) 0.027(3) 0.029(3) 0.013(2) 0.009(2) 0.015(2) B2A 0.018(3) 0.020(3) 0.020(3) 0.004(2) 0.010(2) 0.008(2) F3A 0.050(2) 0.0348(18) 0.0353(17) 0.0085(14) 0.0139(15) 0.0294(17) C3A 0.028(3) 0.019(3) 0.027(3) 0.007(2) 0.003(2) 0.012(2) B3A 0.026(3) 0.025(3) 0.022(3) 0.008(2) 0.012(2) 0.018(3) F4A 0.0311(17) 0.0398(18) 0.0347(17) 0.0082(14) 0.0166(14) 0.0214(15) C4A 0.040(3) 0.029(3) 0.021(3) 0.007(2) 0.005(2) 0.026(3) B4A 0.025(3) 0.026(3) 0.029(3) 0.013(3) 0.016(3) 0.018(3) F5A 0.0274(16) 0.0195(15) 0.0398(17) 0.0108(13) 0.0186(14) 0.0085(13) C5A 0.027(3) 0.034(3) 0.027(3) 0.013(2) 0.012(2) 0.021(3) F6A 0.0401(18) 0.0285(16) 0.0459(18) 0.0240(15) 0.0268(15) 0.0192(15) C6A 0.023(3) 0.020(3) 0.031(3) 0.009(2) 0.007(2) 0.012(2) F7A 0.076(2) 0.050(2) 0.055(2) 0.0401(18) 0.0458(19) 0.047(2) C7A 0.028(3) 0.020(3) 0.031(3) 0.010(2) 0.015(2) 0.016(2) F8A 0.078(3) 0.075(3) 0.0340(18) 0.0302(18) 0.0241(18) 0.063(2) C8A 0.031(3) 0.030(3) 0.030(3) 0.013(2) 0.017(2) 0.019(3) F9A 0.046(2) 0.054(2) 0.045(2) 0.0128(17) 0.0011(17) 0.0321(19) C9A 0.059(4) 0.038(3) 0.035(3) 0.023(3) 0.030(3) 0.037(3) F10A 0.0275(17) 0.0281(17) 0.0468(19) 0.0130(15) 0.0037(14) 0.0120(14) C10A 0.054(4) 0.061(4) 0.020(3) 0.020(3) 0.016(3) 0.046(4) F11A 0.0270(16) 0.0267(16) 0.0361(17) 0.0154(13) 0.0090(13) 0.0144(14) C11A 0.043(4) 0.043(4) 0.032(3) 0.012(3) 0.014(3) 0.029(3) F12A 0.056(2) 0.0319(17) 0.0418(19) 0.0248(15) 0.0219(16) 0.0200(17) C12A 0.041(3) 0.034(3) 0.033(3) 0.014(3) 0.016(3) 0.026(3) F13A 0.052(2) 0.0388(19) 0.062(2) 0.0273(17) 0.0452(19) 0.0183(17) C13A 0.017(2) 0.018(2) 0.031(3) 0.007(2) 0.008(2) 0.009(2) F14A 0.043(2) 0.056(2) 0.081(3) 0.035(2) 0.0452(19) 0.0331(19) C14A 0.025(3) 0.018(3) 0.032(3) 0.007(2) 0.011(2) 0.009(2) F15A 0.0353(17) 0.0419(18) 0.0520(19) 0.0282(16) 0.0258(15) 0.0287(16) C15A 0.041(3) 0.018(3) 0.032(3) 0.012(2) 0.017(3) 0.009(3) F16A 0.0349(17) 0.0247(16) 0.0338(17) 0.0065(13) 0.0155(14) 0.0170(14) C16A 0.033(3) 0.026(3) 0.037(3) 0.012(3) 0.023(3) 0.008(3) F17A 0.0374(18) 0.0276(17) 0.054(2) 0.0103(15) 0.0188(15) 0.0239(15) C17A 0.026(3) 0.033(3) 0.048(3) 0.013(3) 0.022(3) 0.016(3) F18A 0.0258(16) 0.0309(17) 0.059(2) 0.0242(16) 0.0104(15) 0.0158(14) C18A 0.023(3) 0.026(3) 0.037(3) 0.014(2) 0.012(2) 0.011(2) F19A 0.0367(18) 0.0338(17) 0.0351(18) 0.0156(15) 0.0089(14) 0.0147(15) C19A 0.017(2) 0.018(2) 0.032(3) 0.011(2) 0.017(2) 0.008(2) F20A 0.0322(16) 0.0267(16) 0.0294(15) 0.0087(13) 0.0144(13) 0.0177(14) C20A 0.020(3) 0.020(3) 0.032(3) 0.009(2) 0.013(2) 0.009(2) F21A 0.0242(15) 0.0218(15) 0.0384(17) 0.0049(13) 0.0186(13) 0.0106(13) C21A 0.021(3) 0.019(3) 0.043(3) 0.011(2) 0.017(2) 0.011(2) F22A 0.0266(16) 0.0346(17) 0.0381(17) 0.0103(14) 0.0218(14) 0.0115(14) C22A 0.018(3) 0.021(3) 0.047(3) 0.019(3) 0.014(2) 0.010(2) F23A 0.0264(16) 0.0204(15) 0.0403(17) 0.0142(13) 0.0147(14) 0.0052(13) C23A 0.020(3) 0.027(3) 0.023(3) 0.009(2) 0.007(2) 0.005(2) F24A 0.0320(17) 0.0193(15) 0.0403(18) 0.0054(13) 0.0152(14) 0.0105(14) C24A 0.023(3) 0.022(3) 0.029(3) 0.010(2) 0.016(2) 0.011(2) F25A 0.0323(17) 0.0226(15) 0.0416(17) 0.0071(13) 0.0234(14) 0.0134(14) C25A 0.016(2) 0.020(3) 0.028(3) 0.011(2) 0.011(2) 0.011(2) F26A 0.0334(17) 0.0309(16) 0.0410(17) 0.0225(14) 0.0221(14) 0.0214(14) C26A 0.021(3) 0.018(3) 0.026(3) 0.004(2) 0.008(2) 0.012(2) F27A 0.047(2) 0.0423(19) 0.071(2) 0.0384(17) 0.0377(18) 0.0384(17) C27A 0.019(3) 0.027(3) 0.025(3) 0.008(2) 0.012(2) 0.012(2) F28A 0.063(2) 0.054(2) 0.081(3) 0.041(2) 0.057(2) 0.047(2) C28A 0.020(3) 0.015(2) 0.032(3) 0.013(2) 0.008(2) 0.005(2) F29A 0.052(2) 0.0467(19) 0.051(2) 0.0310(17) 0.0396(17) 0.0343(18) C29A 0.026(3) 0.019(3) 0.034(3) 0.009(2) 0.011(2) 0.015(2) F30A 0.0319(16) 0.0312(16) 0.0400(17) 0.0213(14) 0.0220(14) 0.0216(14) C30A 0.024(3) 0.021(3) 0.032(3) 0.015(2) 0.018(2) 0.015(2) F31A 0.0305(16) 0.0267(15) 0.0254(15) 0.0095(13) 0.0158(13) 0.0139(14) C31A 0.023(3) 0.014(2) 0.032(3) 0.011(2) 0.015(2) 0.010(2) F32A 0.0344(17) 0.0339(17) 0.0432(18) 0.0238(15) 0.0250(15) 0.0208(15) C32A 0.024(3) 0.022(3) 0.033(3) 0.013(2) 0.016(2) 0.011(2) F33A 0.0285(17) 0.0298(17) 0.064(2) 0.0223(16) 0.0185(16) 0.0073(15) C33A 0.027(3) 0.026(3) 0.048(3) 0.022(3) 0.021(3) 0.019(2) F34A 0.0362(19) 0.0326(18) 0.0415(19) 0.0079(16) 0.0017(16) 0.0045(16) C34A 0.032(3) 0.030(3) 0.058(4) 0.020(3) 0.030(3) 0.021(3) F35A 0.0389(18) 0.0332(17) 0.0272(16) 0.0086(14) 0.0083(14) 0.0158(15) C35A 0.030(3) 0.031(3) 0.035(3) 0.017(2) 0.022(2) 0.017(3) F36A 0.0383(17) 0.0398(18) 0.0242(15) 0.0123(13) 0.0152(13) 0.0271(15) C36A 0.023(3) 0.020(3) 0.035(3) 0.014(2) 0.012(2) 0.012(2) F37A 0.0365(18) 0.0461(19) 0.0338(17) 0.0226(15) 0.0137(14) 0.0292(16) C37A 0.026(3) 0.016(2) 0.027(3) 0.006(2) 0.009(2) 0.015(2) F38A 0.0327(17) 0.0349(17) 0.0468(18) 0.0195(15) 0.0121(14) 0.0258(15) C38A 0.023(3) 0.020(3) 0.028(3) 0.007(2) 0.008(2) 0.015(2) F39A 0.0248(15) 0.0265(15) 0.0415(17) 0.0104(13) 0.0172(13) 0.0186(13) C39A 0.028(3) 0.030(3) 0.038(3) 0.020(3) 0.019(3) 0.019(3) F40A 0.0235(15) 0.0317(16) 0.0242(15) 0.0113(12) 0.0119(12) 0.0177(13) C40A 0.024(3) 0.025(3) 0.046(3) 0.015(3) 0.012(3) 0.013(2) F41A 0.0300(16) 0.0355(18) 0.0336(17) 0.0157(14) 0.0168(14) 0.0165(15) C41A 0.026(3) 0.023(3) 0.036(3) 0.004(2) 0.003(2) 0.011(2) F42A 0.048(2) 0.089(3) 0.044(2) 0.039(2) 0.0335(17) 0.046(2) C42A 0.034(3) 0.029(3) 0.028(3) 0.013(2) 0.013(2) 0.018(3) F43A 0.117(3) 0.131(4) 0.059(2) 0.055(3) 0.066(2) 0.112(3) C43A 0.019(2) 0.021(3) 0.029(3) 0.012(2) 0.011(2) 0.011(2) F44A 0.131(4) 0.079(3) 0.056(2) 0.027(2) 0.050(2) 0.090(3) C44A 0.020(3) 0.021(3) 0.030(3) 0.011(2) 0.011(2) 0.012(2) F45A 0.062(2) 0.0346(18) 0.0404(18) 0.0160(15) 0.0230(17) 0.0358(18) C45A 0.021(3) 0.028(3) 0.023(3) 0.012(2) 0.004(2) 0.015(2) F46A 0.0182(14) 0.0268(15) 0.0399(17) 0.0149(13) 0.0134(13) 0.0149(13) C46A 0.019(3) 0.024(3) 0.035(3) 0.013(2) 0.007(2) 0.013(2) F47A 0.0328(17) 0.0285(16) 0.0431(18) 0.0210(14) 0.0172(14) 0.0202(14) C47A 0.022(3) 0.021(3) 0.033(3) 0.010(2) 0.012(2) 0.014(2) F48A 0.0298(17) 0.0331(17) 0.054(2) 0.0236(16) 0.0217(15) 0.0137(15) C48A 0.016(2) 0.018(2) 0.024(3) 0.008(2) 0.008(2) 0.010(2) F49A 0.0187(16) 0.048(2) 0.053(2) 0.0253(17) 0.0159(14) 0.0181(15) C49A 0.028(3) 0.041(3) 0.020(3) 0.009(2) 0.009(2) 0.026(3) F50A 0.0261(16) 0.0444(18) 0.0454(18) 0.0284(15) 0.0155(14) 0.0257(15) C50A 0.035(3) 0.040(3) 0.023(3) 0.009(2) 0.007(2) 0.030(3) F51A 0.0413(18) 0.051(2) 0.0441(18) 0.0300(16) 0.0307(15) 0.0335(17) C51A 0.039(3) 0.072(4) 0.032(3) 0.029(3) 0.024(3) 0.040(3) F52A 0.107(3) 0.103(3) 0.072(3) 0.061(2) 0.073(2) 0.094(3) C52A 0.075(5) 0.082(5) 0.035(3) 0.030(3) 0.035(3) 0.068(4) F53A 0.147(4) 0.082(3) 0.071(3) 0.049(2) 0.074(3) 0.103(3) C53A 0.079(5) 0.060(4) 0.035(3) 0.016(3) 0.025(3) 0.060(4) F54A 0.086(3) 0.041(2) 0.052(2) 0.0273(17) 0.036(2) 0.048(2) C54A 0.044(3) 0.042(3) 0.023(3) 0.013(3) 0.012(2) 0.033(3) F55A 0.0378(17) 0.0296(16) 0.0351(16) 0.0144(14) 0.0203(14) 0.0221(15) C55A 0.020(3) 0.029(3) 0.027(3) 0.012(2) 0.012(2) 0.015(2) F56A 0.0384(18) 0.0459(19) 0.0343(17) 0.0185(15) 0.0144(14) 0.0344(16) C56A 0.024(3) 0.028(3) 0.026(3) 0.010(2) 0.012(2) 0.015(2) F57A 0.0319(17) 0.0400(18) 0.0369(17) 0.0206(15) 0.0071(14) 0.0222(15) C57A 0.029(3) 0.032(3) 0.024(3) 0.015(2) 0.012(2) 0.021(3) F58A 0.0335(17) 0.0394(18) 0.0239(16) 0.0153(14) 0.0091(13) 0.0139(15) C58A 0.021(3) 0.028(3) 0.034(3) 0.016(2) 0.015(2) 0.008(2) F59A 0.0286(16) 0.0320(16) 0.0246(15) 0.0054(13) 0.0138(13) 0.0128(14) C59A 0.017(3) 0.038(3) 0.033(3) 0.019(2) 0.013(2) 0.015(2) F60A 0.0239(15) 0.0265(15) 0.0274(15) 0.0087(12) 0.0094(12) 0.0162(13) C60A 0.028(3) 0.037(3) 0.030(3) 0.020(2) 0.015(2) 0.022(3) C61A 0.029(3) 0.036(3) 0.021(3) 0.013(2) 0.010(2) 0.026(3) C62A 0.039(3) 0.050(4) 0.035(3) 0.028(3) 0.021(3) 0.037(3) C63A 0.069(4) 0.068(4) 0.045(4) 0.036(3) 0.041(3) 0.059(4) C64A 0.089(5) 0.068(4) 0.041(4) 0.031(3) 0.037(4) 0.070(4) C65A 0.064(4) 0.040(3) 0.036(3) 0.024(3) 0.026(3) 0.041(3) C66A 0.030(3) 0.034(3) 0.027(3) 0.013(2) 0.012(2) 0.024(3) C67A 0.017(2) 0.020(3) 0.027(3) 0.011(2) 0.010(2) 0.011(2) C68A 0.021(3) 0.023(3) 0.029(3) 0.012(2) 0.011(2) 0.011(2) C69A 0.017(3) 0.025(3) 0.032(3) 0.012(2) 0.003(2) 0.007(2) C70A 0.023(3) 0.026(3) 0.020(3) 0.013(2) 0.006(2) 0.008(2) C71A 0.020(3) 0.020(3) 0.025(3) 0.004(2) 0.010(2) 0.005(2) C72A 0.013(2) 0.022(3) 0.031(3) 0.015(2) 0.008(2) 0.007(2) Cl1S 0.0602(12) 0.0726(14) 0.197(3) 0.0927(17) 0.0730(15) 0.0403(11) C1S 0.061(6) 0.099(7) 0.139(9) 0.077(7) 0.034(6) 0.032(5) Cl2S 0.183(3) 0.0493(13) 0.0718(15) 0.0118(11) 0.0245(17) 0.0402(16) C2S 0.046(4) 0.071(5) 0.055(5) 0.012(4) 0.005(4) -0.005(4) Cl3S 0.0523(13) 0.126(2) 0.0823(16) 0.0568(15) -0.0053(11) -0.0094(13) Cl4S 0.0491(10) 0.0605(11) 0.0498(9) 0.0113(8) 0.0141(8) 0.0335(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C23 1.976(5) . ? Pd1 N1 2.025(4) . ? Pd1 N5 2.112(4) . ? Pd1 N10 2.140(4) . ? Pd1 Pd2 2.8630(6) . ? N1 C1 1.343(6) . ? N1 C5 1.362(6) . ? C1 C2 1.385(6) . ? Pd2 C10 1.961(5) . ? Pd2 N7 2.054(4) . ? Pd2 N2 2.083(4) . ? Pd2 C23 2.407(5) . ? N2 C5 1.367(6) . ? N2 C8 1.372(6) . ? C2 C3 1.375(6) . ? N3 C12 1.354(7) . ? N3 C9 1.386(6) . ? N3 C13 1.468(6) . ? C3 C4 1.389(6) . ? N4 C14 1.329(6) . ? N4 C18 1.347(6) . ? C4 C5 1.414(6) . ? C4 C6 1.424(6) . ? N5 C21 1.359(6) . ? N5 C18 1.378(6) . ? N6 C22 1.381(6) . ? N6 C25 1.383(7) . ? N6 C26 1.463(6) . ? C6 C7 1.337(7) . ? N7 C27 1.333(7) . ? N7 C31 1.372(7) . ? C7 C8 1.433(7) . ? N8 C34 1.344(7) . ? N8 C31 1.347(7) . ? C8 C9 1.405(7) . ? N9 C38 1.377(8) . ? N9 C35 1.403(7) . ? N9 C39 1.450(7) . ? C9 C10 1.398(7) . ? N10 C40 1.335(6) . ? N10 C44 1.362(6) . ? C10 C11 1.395(8) . ? N11 C47 1.339(6) . ? N11 C44 1.372(6) . ? C11 C12 1.368(9) . ? N12 C51 1.368(6) . ? N12 C48 1.395(6) . ? N12 C52 1.461(6) . ? C14 C15 1.406(7) . ? C15 C16 1.374(8) . ? C16 C17 1.399(7) . ? C17 C19 1.418(7) . ? C17 C18 1.422(6) . ? C19 C20 1.341(7) . ? C20 C21 1.423(6) . ? C21 C22 1.439(7) . ? C22 C23 1.382(7) . ? C23 C24 1.413(7) . ? C24 C25 1.373(7) . ? C27 C28 1.403(8) . ? C28 C29 1.357(9) . ? C29 C30 1.405(9) . ? C30 C32 1.415(9) . ? C30 C31 1.426(7) . ? C32 C33 1.364(9) . ? C33 C34 1.422(8) . ? C34 C35 1.437(9) . ? C35 C36 1.400(8) . ? C36 C37 1.392(9) . ? C37 C38 1.383(9) . ? C40 C41 1.401(7) . ? C41 C42 1.361(7) . ? C42 C43 1.411(7) . ? C43 C45 1.416(7) . ? C43 C44 1.419(6) . ? C45 C46 1.333(7) . ? C46 C47 1.435(6) . ? C47 C48 1.442(7) . ? C48 C49 1.396(7) . ? C49 C50 1.398(7) . ? C50 C51 1.358(7) . ? F1A C2A 1.350(6) . ? N1A B2A 1.621(6) . ? N1A B1A 1.634(7) . ? C1A C6A 1.390(7) . ? C1A C2A 1.395(7) . ? C1A B1A 1.678(7) . ? B1A C13A 1.642(7) . ? B1A C7A 1.668(7) . ? F2A C3A 1.352(5) . ? N2A B4A 1.621(6) . ? N2A B3A 1.638(7) . ? C2A C3A 1.387(7) . ? B2A C19A 1.633(7) . ? B2A C31A 1.656(7) . ? B2A C25A 1.683(7) . ? F3A C4A 1.342(5) . ? C3A C4A 1.376(7) . ? B3A C49A 1.637(7) . ? B3A C43A 1.663(7) . ? B3A C37A 1.671(7) . ? F4A C5A 1.338(5) . ? C4A C5A 1.380(7) . ? B4A C55A 1.639(7) . ? B4A C61A 1.640(7) . ? B4A C67A 1.671(7) . ? F5A C6A 1.372(5) . ? C5A C6A 1.383(7) . ? F6A C8A 1.367(6) . ? F7A C9A 1.362(6) . ? C7A C12A 1.398(7) . ? C7A C8A 1.401(7) . ? F8A C10A 1.361(5) . ? C8A C9A 1.361(7) . ? F9A C11A 1.351(6) . ? C9A C10A 1.351(8) . ? F10A C12A 1.360(6) . ? C10A C11A 1.368(8) . ? F11A C14A 1.356(5) . ? C11A C12A 1.365(7) . ? F12A C15A 1.350(6) . ? F13A C16A 1.355(6) . ? C13A C18A 1.394(7) . ? C13A C14A 1.394(7) . ? F14A C17A 1.353(6) . ? C14A C15A 1.375(7) . ? F15A C18A 1.342(5) . ? C15A C16A 1.374(8) . ? F16A C20A 1.341(5) . ? C16A C17A 1.363(7) . ? F17A C21A 1.347(5) . ? C17A C18A 1.382(7) . ? F18A C22A 1.341(5) . ? F19A C23A 1.345(5) . ? C19A C24A 1.400(7) . ? C19A C20A 1.413(7) . ? F20A C24A 1.361(5) . ? C20A C21A 1.383(7) . ? F21A C26A 1.374(5) . ? C21A C22A 1.369(7) . ? F22A C27A 1.345(5) . ? C22A C23A 1.389(7) . ? F23A C28A 1.349(5) . ? C23A C24A 1.354(7) . ? F24A C29A 1.350(5) . ? F25A C30A 1.361(5) . ? C25A C26A 1.388(6) . ? C25A C30A 1.392(6) . ? F26A C32A 1.362(5) . ? C26A C27A 1.358(6) . ? F27A C33A 1.350(5) . ? C27A C28A 1.379(7) . ? F28A C34A 1.347(6) . ? C28A C29A 1.375(7) . ? F29A C35A 1.341(5) . ? C29A C30A 1.378(6) . ? F30A C36A 1.366(5) . ? F31A C38A 1.357(5) . ? C31A C32A 1.379(6) . ? C31A C36A 1.381(6) . ? F32A C39A 1.349(5) . ? C32A C33A 1.381(7) . ? F33A C40A 1.344(6) . ? C33A C34A 1.381(7) . ? F34A C41A 1.350(6) . ? C34A C35A 1.364(7) . ? F35A C42A 1.353(6) . ? C35A C36A 1.390(7) . ? F36A C44A 1.367(5) . ? F37A C45A 1.348(5) . ? C37A C42A 1.383(7) . ? C37A C38A 1.396(7) . ? F38A C46A 1.350(5) . ? C38A C39A 1.387(7) . ? F39A C47A 1.346(5) . ? C39A C40A 1.374(7) . ? F40A C48A 1.349(5) . ? C40A C41A 1.365(7) . ? F41A C50A 1.351(6) . ? C41A C42A 1.383(7) . ? F42A C51A 1.344(6) . ? F43A C52A 1.339(6) . ? C43A C44A 1.395(6) . ? C43A C48A 1.395(6) . ? F44A C53A 1.345(7) . ? C44A C45A 1.376(6) . ? F45A C54A 1.352(6) . ? C45A C46A 1.389(7) . ? F46A C56A 1.364(5) . ? C46A C47A 1.356(7) . ? F47A C57A 1.344(5) . ? C47A C48A 1.388(6) . ? F48A C58A 1.337(5) . ? F49A C59A 1.351(5) . ? C49A C50A 1.389(7) . ? C49A C54A 1.396(7) . ? F50A C60A 1.351(5) . ? C50A C51A 1.389(7) . ? F51A C62A 1.353(6) . ? C51A C52A 1.376(9) . ? F52A C63A 1.350(6) . ? C52A C53A 1.364(9) . ? F53A C64A 1.339(6) . ? C53A C54A 1.388(7) . ? F54A C65A 1.345(6) . ? F55A C66A 1.360(5) . ? C55A C56A 1.396(6) . ? C55A C60A 1.396(6) . ? F56A C68A 1.356(5) . ? C56A C57A 1.375(7) . ? F57A C69A 1.353(5) . ? C57A C58A 1.385(7) . ? F58A C70A 1.341(5) . ? C58A C59A 1.376(7) . ? F59A C71A 1.349(5) . ? C59A C60A 1.369(7) . ? F60A C72A 1.371(5) . ? C61A C62A 1.385(7) . ? C61A C66A 1.397(7) . ? C62A C63A 1.389(7) . ? C63A C64A 1.366(9) . ? C64A C65A 1.378(8) . ? C65A C66A 1.380(7) . ? C67A C72A 1.395(6) . ? C67A C68A 1.395(6) . ? C68A C69A 1.376(7) . ? C69A C70A 1.369(7) . ? C70A C71A 1.359(7) . ? C71A C72A 1.384(7) . ? Cl1S C1S 1.744(10) . ? C1S Cl2S 1.640(10) . ? C2S Cl4S 1.746(7) . ? C2S Cl3S 1.764(7) . ? 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 C23 Pd1 N1 89.87(17) . . ? C23 Pd1 N5 80.21(17) . . ? N1 Pd1 N5 169.55(15) . . ? C23 Pd1 N10 176.54(17) . . ? N1 Pd1 N10 86.84(14) . . ? N5 Pd1 N10 103.01(14) . . ? C23 Pd1 Pd2 56.12(13) . . ? N1 Pd1 Pd2 84.23(10) . . ? N5 Pd1 Pd2 92.85(10) . . ? N10 Pd1 Pd2 124.50(10) . . ? C1 N1 C5 118.8(4) . . ? C1 N1 Pd1 115.8(3) . . ? C5 N1 Pd1 125.4(3) . . ? N1 C1 C2 123.3(4) . . ? C10 Pd2 N7 90.49(19) . . ? C10 Pd2 N2 80.91(18) . . ? N7 Pd2 N2 167.83(16) . . ? C10 Pd2 C23 166.2(2) . . ? N7 Pd2 C23 90.97(16) . . ? N2 Pd2 C23 95.37(15) . . ? C10 Pd2 Pd1 146.72(16) . . ? N7 Pd2 Pd1 112.79(12) . . ? N2 Pd2 Pd1 78.67(10) . . ? C23 Pd2 Pd1 42.97(11) . . ? C5 N2 C8 118.4(4) . . ? C5 N2 Pd2 127.7(3) . . ? C8 N2 Pd2 112.8(3) . . ? C3 C2 C1 118.2(4) . . ? C12 N3 C9 106.4(4) . . ? C12 N3 C13 124.4(4) . . ? C9 N3 C13 129.0(4) . . ? C2 C3 C4 120.4(4) . . ? C14 N4 C18 117.2(4) . . ? C3 C4 C5 118.5(4) . . ? C3 C4 C6 123.5(4) . . ? C5 C4 C6 117.9(4) . . ? C21 N5 C18 119.2(4) . . ? C21 N5 Pd1 113.7(3) . . ? C18 N5 Pd1 126.9(3) . . ? N1 C5 N2 117.2(4) . . ? N1 C5 C4 120.7(4) . . ? N2 C5 C4 122.0(4) . . ? C22 N6 C25 107.2(4) . . ? C22 N6 C26 129.5(5) . . ? C25 N6 C26 123.2(4) . . ? C7 C6 C4 120.2(5) . . ? C27 N7 C31 119.6(5) . . ? C27 N7 Pd2 116.3(4) . . ? C31 N7 Pd2 123.9(4) . . ? C6 C7 C8 120.1(4) . . ? C34 N8 C31 117.9(5) . . ? N2 C8 C9 112.1(4) . . ? N2 C8 C7 121.0(4) . . ? C9 C8 C7 126.8(4) . . ? C38 N9 C35 109.0(5) . . ? C38 N9 C39 122.2(5) . . ? C35 N9 C39 128.8(5) . . ? N3 C9 C10 108.2(4) . . ? N3 C9 C8 131.9(5) . . ? C10 C9 C8 119.9(4) . . ? C40 N10 C44 118.4(4) . . ? C40 N10 Pd1 121.0(3) . . ? C44 N10 Pd1 120.2(3) . . ? C11 C10 C9 107.7(5) . . ? C11 C10 Pd2 139.9(5) . . ? C9 C10 Pd2 112.3(4) . . ? C47 N11 C44 116.4(4) . . ? C12 C11 C10 105.8(6) . . ? C51 N12 C48 108.7(4) . . ? C51 N12 C52 124.0(4) . . ? C48 N12 C52 126.6(4) . . ? N3 C12 C11 111.8(5) . . ? N4 C14 C15 124.6(5) . . ? C16 C15 C14 117.9(5) . . ? C15 C16 C17 119.6(5) . . ? C16 C17 C19 124.1(5) . . ? C16 C17 C18 117.9(5) . . ? C19 C17 C18 118.0(5) . . ? N4 C18 N5 116.2(4) . . ? N4 C18 C17 122.7(4) . . ? N5 C18 C17 121.0(5) . . ? C20 C19 C17 120.4(5) . . ? C19 C20 C21 120.2(5) . . ? N5 C21 C20 121.1(5) . . ? N5 C21 C22 112.2(4) . . ? C20 C21 C22 126.7(5) . . ? N6 C22 C23 109.2(4) . . ? N6 C22 C21 131.2(4) . . ? C23 C22 C21 119.6(4) . . ? C22 C23 C24 106.8(4) . . ? C22 C23 Pd1 113.3(3) . . ? C24 C23 Pd1 138.4(4) . . ? C22 C23 Pd2 110.8(3) . . ? C24 C23 Pd2 95.0(3) . . ? Pd1 C23 Pd2 80.91(16) . . ? C25 C24 C23 107.4(5) . . ? C24 C25 N6 109.3(5) . . ? N7 C27 C28 122.4(6) . . ? C29 C28 C27 119.5(6) . . ? C28 C29 C30 119.5(6) . . ? C29 C30 C32 124.7(6) . . ? C29 C30 C31 118.9(6) . . ? C32 C30 C31 116.3(6) . . ? N8 C31 N7 116.3(5) . . ? N8 C31 C30 124.2(5) . . ? N7 C31 C30 119.6(6) . . ? C33 C32 C30 119.4(5) . . ? C32 C33 C34 120.3(6) . . ? N8 C34 C33 121.6(6) . . ? N8 C34 C35 118.7(5) . . ? C33 C34 C35 119.7(5) . . ? C36 C35 N9 105.8(6) . . ? C36 C35 C34 129.3(6) . . ? N9 C35 C34 124.9(5) . . ? C37 C36 C35 109.3(6) . . ? C38 C37 C36 107.1(6) . . ? N9 C38 C37 108.7(6) . . ? N10 C40 C41 123.3(5) . . ? C42 C41 C40 119.0(5) . . ? C41 C42 C43 119.8(5) . . ? C42 C43 C45 125.7(5) . . ? C42 C43 C44 117.8(4) . . ? C45 C43 C44 116.4(4) . . ? N10 C44 N11 114.0(4) . . ? N10 C44 C43 121.6(4) . . ? N11 C44 C43 124.4(4) . . ? C46 C45 C43 119.9(5) . . ? C45 C46 C47 120.7(4) . . ? N11 C47 C46 122.2(4) . . ? N11 C47 C48 118.6(4) . . ? C46 C47 C48 119.2(4) . . ? N12 C48 C49 106.2(4) . . ? N12 C48 C47 125.6(4) . . ? C49 C48 C47 128.1(5) . . ? C48 C49 C50 108.3(5) . . ? C51 C50 C49 107.5(5) . . ? C50 C51 N12 109.3(5) . . ? B2A N1A B1A 132.8(4) . . ? C6A C1A C2A 112.4(4) . . ? C6A C1A B1A 122.1(4) . . ? C2A C1A B1A 125.4(4) . . ? N1A B1A C13A 109.9(4) . . ? N1A B1A C7A 109.8(4) . . ? C13A B1A C7A 113.1(4) . . ? N1A B1A C1A 108.4(4) . . ? C13A B1A C1A 113.2(4) . . ? C7A B1A C1A 102.2(4) . . ? B4A N2A B3A 133.9(4) . . ? F1A C2A C3A 115.1(4) . . ? F1A C2A C1A 120.8(4) . . ? C3A C2A C1A 124.1(5) . . ? N1A B2A C19A 112.8(4) . . ? N1A B2A C31A 109.5(4) . . ? C19A B2A C31A 115.5(4) . . ? N1A B2A C25A 104.4(4) . . ? C19A B2A C25A 104.5(4) . . ? C31A B2A C25A 109.4(4) . . ? F2A C3A C4A 119.5(4) . . ? F2A C3A C2A 120.6(5) . . ? C4A C3A C2A 119.9(5) . . ? C49A B3A N2A 108.4(4) . . ? C49A B3A C43A 113.5(4) . . ? N2A B3A C43A 109.6(4) . . ? C49A B3A C37A 113.9(4) . . ? N2A B3A C37A 110.0(4) . . ? C43A B3A C37A 101.3(4) . . ? F3A C4A C3A 120.5(5) . . ? F3A C4A C5A 120.4(5) . . ? C3A C4A C5A 119.1(5) . . ? N2A B4A C55A 113.0(4) . . ? N2A B4A C61A 107.9(4) . . ? C55A B4A C61A 116.2(4) . . ? N2A B4A C67A 106.2(4) . . ? C55A B4A C67A 104.4(4) . . ? C61A B4A C67A 108.6(4) . . ? F4A C5A C4A 119.7(4) . . ? F4A C5A C6A 122.0(5) . . ? C4A C5A C6A 118.4(5) . . ? F5A C6A C5A 115.6(4) . . ? F5A C6A C1A 118.4(4) . . ? C5A C6A C1A 126.0(5) . . ? C12A C7A C8A 111.3(4) . . ? C12A C7A B1A 118.9(4) . . ? C8A C7A B1A 129.8(4) . . ? C9A C8A F6A 115.2(4) . . ? C9A C8A C7A 124.6(5) . . ? F6A C8A C7A 120.2(4) . . ? C10A C9A C8A 120.5(5) . . ? C10A C9A F7A 119.8(5) . . ? C8A C9A F7A 119.7(5) . . ? C9A C10A F8A 121.2(5) . . ? C9A C10A C11A 118.8(5) . . ? F8A C10A C11A 119.9(5) . . ? F9A C11A C12A 120.8(5) . . ? F9A C11A C10A 119.9(5) . . ? C12A C11A C10A 119.3(5) . . ? F10A C12A C11A 116.0(5) . . ? F10A C12A C7A 118.7(4) . . ? C11A C12A C7A 125.3(5) . . ? C18A C13A C14A 113.6(4) . . ? C18A C13A B1A 124.6(4) . . ? C14A C13A B1A 121.7(4) . . ? F11A C14A C15A 116.7(4) . . ? F11A C14A C13A 119.4(4) . . ? C15A C14A C13A 123.9(5) . . ? F12A C15A C16A 119.7(5) . . ? F12A C15A C14A 120.8(5) . . ? C16A C15A C14A 119.6(5) . . ? F13A C16A C17A 120.4(5) . . ? F13A C16A C15A 120.2(5) . . ? C17A C16A C15A 119.4(5) . . ? F14A C17A C16A 120.1(5) . . ? F14A C17A C18A 120.2(5) . . ? C16A C17A C18A 119.7(5) . . ? F15A C18A C17A 115.3(4) . . ? F15A C18A C13A 121.0(4) . . ? C17A C18A C13A 123.7(5) . . ? C24A C19A C20A 112.5(4) . . ? C24A C19A B2A 119.6(4) . . ? C20A C19A B2A 127.7(4) . . ? F16A C20A C21A 115.8(4) . . ? F16A C20A C19A 120.6(4) . . ? C21A C20A C19A 123.6(5) . . ? F17A C21A C22A 120.0(4) . . ? F17A C21A C20A 120.0(5) . . ? C22A C21A C20A 120.0(5) . . ? F18A C22A C21A 120.8(4) . . ? F18A C22A C23A 120.3(5) . . ? C21A C22A C23A 118.9(4) . . ? F19A C23A C24A 121.5(5) . . ? F19A C23A C22A 118.8(5) . . ? C24A C23A C22A 119.6(5) . . ? C23A C24A F20A 116.6(4) . . ? C23A C24A C19A 125.2(5) . . ? F20A C24A C19A 118.2(4) . . ? C26A C25A C30A 112.1(4) . . ? C26A C25A B2A 120.5(4) . . ? C30A C25A B2A 127.4(4) . . ? C27A C26A F21A 115.5(4) . . ? C27A C26A C25A 126.0(4) . . ? F21A C26A C25A 118.5(4) . . ? F22A C27A C26A 121.3(4) . . ? F22A C27A C28A 119.5(4) . . ? C26A C27A C28A 119.2(4) . . ? F23A C28A C29A 120.2(4) . . ? F23A C28A C27A 121.3(4) . . ? C29A C28A C27A 118.5(4) . . ? F24A C29A C28A 119.8(4) . . ? F24A C29A C30A 120.5(4) . . ? C28A C29A C30A 119.7(4) . . ? F25A C30A C29A 114.5(4) . . ? F25A C30A C25A 121.0(4) . . ? C29A C30A C25A 124.5(4) . . ? C32A C31A C36A 113.0(4) . . ? C32A C31A B2A 119.6(4) . . ? C36A C31A B2A 127.2(4) . . ? F26A C32A C31A 119.4(4) . . ? F26A C32A C33A 115.5(4) . . ? C31A C32A C33A 125.1(4) . . ? F27A C33A C34A 120.4(4) . . ? F27A C33A C32A 120.6(4) . . ? C34A C33A C32A 118.9(5) . . ? F28A C34A C35A 121.3(5) . . ? F28A C34A C33A 119.9(5) . . ? C35A C34A C33A 118.8(5) . . ? F29A C35A C34A 120.9(4) . . ? F29A C35A C36A 119.4(4) . . ? C34A C35A C36A 119.7(5) . . ? F30A C36A C31A 121.3(4) . . ? F30A C36A C35A 114.6(4) . . ? C31A C36A C35A 124.1(4) . . ? C42A C37A C38A 112.4(4) . . ? C42A C37A B3A 120.0(4) . . ? C38A C37A B3A 127.2(4) . . ? F31A C38A C39A 113.6(4) . . ? F31A C38A C37A 122.1(4) . . ? C39A C38A C37A 124.3(5) . . ? F32A C39A C40A 119.9(4) . . ? F32A C39A C38A 120.2(4) . . ? C40A C39A C38A 119.9(5) . . ? F33A C40A C41A 121.6(5) . . ? F33A C40A C39A 120.0(5) . . ? C41A C40A C39A 118.4(5) . . ? F34A C41A C40A 120.4(5) . . ? F34A C41A C42A 119.7(5) . . ? C40A C41A C42A 119.9(5) . . ? F35A C42A C37A 119.0(4) . . ? F35A C42A C41A 116.0(4) . . ? C37A C42A C41A 125.0(5) . . ? C44A C43A C48A 112.1(4) . . ? C44A C43A B3A 126.5(4) . . ? C48A C43A B3A 120.8(4) . . ? F36A C44A C45A 114.6(4) . . ? F36A C44A C43A 120.1(4) . . ? C45A C44A C43A 125.3(5) . . ? F37A C45A C44A 121.3(4) . . ? F37A C45A C46A 119.6(4) . . ? C44A C45A C46A 119.1(4) . . ? F38A C46A C47A 121.0(4) . . ? F38A C46A C45A 120.2(4) . . ? C47A C46A C45A 118.8(4) . . ? F39A C47A C46A 119.6(4) . . ? F39A C47A C48A 120.3(4) . . ? C46A C47A C48A 120.0(4) . . ? F40A C48A C47A 115.8(4) . . ? F40A C48A C43A 119.5(4) . . ? C47A C48A C43A 124.6(4) . . ? C50A C49A C54A 113.1(4) . . ? C50A C49A B3A 121.8(4) . . ? C54A C49A B3A 125.0(5) . . ? F41A C50A C51A 116.0(5) . . ? F41A C50A C49A 119.8(4) . . ? C51A C50A C49A 124.2(5) . . ? F42A C51A C52A 120.0(5) . . ? F42A C51A C50A 120.1(5) . . ? C52A C51A C50A 119.8(5) . . ? F43A C52A C53A 120.2(6) . . ? F43A C52A C51A 121.0(6) . . ? C53A C52A C51A 118.8(5) . . ? F44A C53A C52A 120.4(5) . . ? F44A C53A C54A 119.6(6) . . ? C52A C53A C54A 120.0(5) . . ? F45A C54A C53A 115.1(5) . . ? F45A C54A C49A 120.7(4) . . ? C53A C54A C49A 124.2(5) . . ? C56A C55A C60A 112.5(4) . . ? C56A C55A B4A 127.0(4) . . ? C60A C55A B4A 120.2(4) . . ? F46A C56A C57A 114.7(4) . . ? F46A C56A C55A 120.7(4) . . ? C57A C56A C55A 124.5(4) . . ? F47A C57A C56A 120.1(4) . . ? F47A C57A C58A 120.2(4) . . ? C56A C57A C58A 119.7(4) . . ? F48A C58A C59A 121.2(4) . . ? F48A C58A C57A 120.2(4) . . ? C59A C58A C57A 118.5(4) . . ? F49A C59A C60A 120.7(4) . . ? F49A C59A C58A 119.7(4) . . ? C60A C59A C58A 119.6(4) . . ? F50A C60A C59A 116.2(4) . . ? F50A C60A C55A 118.7(4) . . ? C59A C60A C55A 125.1(5) . . ? C62A C61A C66A 112.5(4) . . ? C62A C61A B4A 127.7(5) . . ? C66A C61A B4A 119.7(4) . . ? F51A C62A C61A 121.0(4) . . ? F51A C62A C63A 114.8(4) . . ? C61A C62A C63A 124.1(5) . . ? F52A C63A C64A 119.4(5) . . ? F52A C63A C62A 120.5(5) . . ? C64A C63A C62A 120.0(5) . . ? F53A C64A C63A 120.9(5) . . ? F53A C64A C65A 119.7(6) . . ? C63A C64A C65A 119.3(5) . . ? F54A C65A C64A 120.9(5) . . ? F54A C65A C66A 120.6(5) . . ? C64A C65A C66A 118.5(5) . . ? F55A C66A C65A 115.9(5) . . ? F55A C66A C61A 118.6(4) . . ? C65A C66A C61A 125.6(5) . . ? C72A C67A C68A 112.2(4) . . ? C72A C67A B4A 122.2(4) . . ? C68A C67A B4A 125.6(4) . . ? F56A C68A C69A 114.5(4) . . ? F56A C68A C67A 121.4(4) . . ? C69A C68A C67A 124.1(5) . . ? F57A C69A C70A 119.7(4) . . ? F57A C69A C68A 120.1(5) . . ? C70A C69A C68A 120.2(5) . . ? F58A C70A C71A 121.0(5) . . ? F58A C70A C69A 119.9(4) . . ? C71A C70A C69A 119.1(4) . . ? F59A C71A C70A 120.4(4) . . ? F59A C71A C72A 120.5(4) . . ? C70A C71A C72A 119.1(5) . . ? F60A C72A C71A 115.2(4) . . ? F60A C72A C67A 119.6(4) . . ? C71A C72A C67A 125.2(4) . . ? Cl2S C1S Cl1S 120.5(5) . . ? Cl4S C2S Cl3S 110.5(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.675 _refine_diff_density_min -1.722 _refine_diff_density_rms 0.111 _iucr_refine_instructions_details ; TITL _compound_4 CELL 0.71073 18.3890 18.5550 22.2150 100.835 103.159 119.476 ZERR 2.0000 0.0030 0.0030 0.0030 0.002 0.002 0.002 LATT 1 SFAC C B CL F N PD H UNIT 252 8 8 120 28 4 100 MERG 2 SHEL 99999.00 0.84 FMAP 2 GRID PLAN 2 TEMP -173 SIZE 0.22 0.32 0.38 OMIT 18 -10 9 OMIT -5 -2 26 OMIT -4 1 3 OMIT 0 0 4 OMIT 0 0 1 OMIT 1 0 0 OMIT -1 0 1 OMIT -1 1 0 OMIT -18 3 19 OMIT 3 9 14 OMIT -20 3 13 OMIT -11 7 23 OMIT -2 -18 12 OMIT -2 -7 26 OMIT -14 12 4 OMIT 2 -1 1 OMIT -15 21 0 OMIT -12 8 22 OMIT -11 -5 7 DFIX 1.01 N1A H1A1 N1A H1A2 N2A H2A1 N2A H2A2 SADI N1A H1A1 N1A H1A2 SADI N2A H2A1 N2A H2A2 L.S. 5 ACTA WGHT 0.08260 1.57370 0.00000 0.00000 0.00000 0.33330 FVAR 0.19928 Pd1 6 0.00414 0.87949 0.19560 11.00000 0.01976 0.02042 = 0.02255 0.01107 0.01144 0.01366 N1 5 -0.10012 0.88417 0.14717 11.00000 0.01773 0.01553 = 0.02088 0.00501 0.01005 0.00945 C1 1 -0.10764 0.88660 0.08615 11.00000 0.02247 0.02001 = 0.02240 0.00556 0.00856 0.01047 AFIX 43 H1 7 -0.06595 0.88382 0.06890 11.00000 -1.20000 AFIX 0 Pd2 6 -0.09014 0.83031 0.28252 11.00000 0.03104 0.03048 = 0.02667 0.01568 0.01696 0.02133 N2 5 -0.15126 0.88350 0.23399 11.00000 0.01744 0.01626 = 0.02186 0.00608 0.01052 0.00912 C2 1 -0.17309 0.89296 0.04705 11.00000 0.02662 0.02124 = 0.02036 0.00732 0.01038 0.01324 AFIX 43 H2 7 -0.17772 0.89222 0.00344 11.00000 -1.20000 AFIX 0 N3 5 -0.21092 0.91692 0.37829 11.00000 0.03396 0.05009 = 0.02386 0.01119 0.01794 0.02676 C3 1 -0.23116 0.90036 0.07311 11.00000 0.02256 0.02363 = 0.02702 0.00845 0.00429 0.01379 AFIX 43 H3 7 -0.27589 0.90599 0.04764 11.00000 -1.20000 AFIX 0 N4 5 0.22245 0.99248 0.27733 11.00000 0.02051 0.03246 = 0.02914 0.01654 0.01158 0.01563 C4 1 -0.22478 0.89967 0.13649 11.00000 0.01800 0.01396 = 0.02854 0.00692 0.00886 0.00805 N5 5 0.09588 0.84937 0.23836 11.00000 0.02421 0.02554 = 0.02132 0.01058 0.01064 0.01776 C5 1 -0.15937 0.88842 0.17242 11.00000 0.01591 0.01221 = 0.02569 0.00728 0.00882 0.00760 N6 5 -0.10514 0.62396 0.18418 11.00000 0.04034 0.01927 = 0.03912 0.01574 0.02082 0.01784 C6 1 -0.27906 0.91205 0.16818 11.00000 0.02088 0.02472 = 0.03105 0.00949 0.00961 0.01315 AFIX 43 H6 7 -0.32475 0.91808 0.14489 11.00000 -1.20000 AFIX 0 N7 5 -0.05390 0.76552 0.33513 11.00000 0.05579 0.04902 = 0.03140 0.02488 0.02660 0.04051 C7 1 -0.26587 0.91521 0.23059 11.00000 0.01786 0.02306 = 0.03412 0.00700 0.01379 0.01166 AFIX 43 H7 7 -0.29913 0.92778 0.25265 11.00000 -1.20000 AFIX 0 N8 5 0.09496 0.88405 0.38463 11.00000 0.04050 0.05339 = 0.02641 0.02274 0.01913 0.03526 C8 1 -0.20162 0.89966 0.26425 11.00000 0.01914 0.01314 = 0.03218 0.00556 0.01307 0.00615 N9 5 0.22647 1.07222 0.42631 11.00000 0.04274 0.05596 = 0.02707 0.01632 0.01457 0.03367 C9 1 -0.18313 0.89673 0.32838 11.00000 0.02527 0.02799 = 0.02838 0.00993 0.01636 0.01496 N10 5 0.09057 1.01276 0.20128 11.00000 0.01878 0.02284 = 0.02426 0.01204 0.01110 0.01416 C10 1 -0.12799 0.86824 0.35086 11.00000 0.03245 0.04335 = 0.02843 0.01435 0.01789 0.02191 N11 5 0.12532 0.95785 0.11900 11.00000 0.02220 0.02527 = 0.02075 0.01356 0.01083 0.01888 C11 1 -0.12201 0.87111 0.41512 11.00000 0.07966 0.10083 = 0.04553 0.04753 0.04178 0.07097 AFIX 43 H11 7 -0.08928 0.85549 0.44313 11.00000 -1.20000 AFIX 0 N12 5 0.10353 0.80903 0.02519 11.00000 0.03191 0.02649 = 0.02175 0.00646 0.00960 0.01949 C12 1 -0.17302 0.90107 0.42950 11.00000 0.08687 0.10750 = 0.03760 0.03610 0.04497 0.07232 AFIX 43 H12 7 -0.18088 0.90969 0.47046 11.00000 -1.20000 AFIX 0 C13 1 -0.26502 0.95419 0.38022 11.00000 0.02846 0.03952 = 0.03429 0.00337 0.01851 0.01648 AFIX 137 H13A 7 -0.32711 0.91011 0.34902 11.00000 -1.50000 H13B 7 -0.23948 1.00698 0.36794 11.00000 -1.50000 H13C 7 -0.26458 0.97036 0.42497 11.00000 -1.50000 AFIX 0 C14 1 0.31132 1.04876 0.30662 11.00000 0.02583 0.04353 = 0.02880 0.02127 0.01306 0.01741 AFIX 43 H14 7 0.33611 1.10935 0.31246 11.00000 -1.20000 AFIX 0 C15 1 0.37127 1.02500 0.32957 11.00000 0.02783 0.05720 = 0.03250 0.02943 0.01888 0.02474 AFIX 43 H15 7 0.43420 1.06835 0.35114 11.00000 -1.20000 AFIX 0 C16 1 0.33606 0.93722 0.31985 11.00000 0.03169 0.06577 = 0.03640 0.03359 0.02189 0.03725 AFIX 43 H16 7 0.37473 0.91863 0.33386 11.00000 -1.20000 AFIX 0 C17 1 0.24286 0.87531 0.28918 11.00000 0.03115 0.04425 = 0.02597 0.02238 0.01838 0.02795 C18 1 0.18819 0.90649 0.26828 11.00000 0.02121 0.03986 = 0.02467 0.01873 0.01338 0.02074 C19 1 0.19960 0.78362 0.27813 11.00000 0.04703 0.05312 = 0.03597 0.02996 0.02407 0.04038 AFIX 43 H19 7 0.23464 0.76070 0.29025 11.00000 -1.20000 AFIX 0 C20 1 0.10950 0.72903 0.25065 11.00000 0.04511 0.03527 = 0.03109 0.01895 0.02231 0.03070 AFIX 43 H20 7 0.08091 0.66795 0.24452 11.00000 -1.20000 AFIX 0 C21 1 0.05662 0.76240 0.23066 11.00000 0.03319 0.03162 = 0.02262 0.01422 0.01542 0.02604 C22 1 -0.04012 0.71285 0.20174 11.00000 0.02838 0.02190 = 0.02923 0.00959 0.01396 0.01386 C23 1 -0.08146 0.75571 0.18603 11.00000 0.02626 0.02377 = 0.02616 0.01087 0.01597 0.01642 C24 1 -0.17505 0.69032 0.15564 11.00000 0.02950 0.02566 = 0.03969 0.01664 0.01789 0.01680 AFIX 43 H24 7 -0.22067 0.69944 0.13786 11.00000 -1.20000 AFIX 0 C25 1 -0.18786 0.61120 0.15657 11.00000 0.03362 0.01922 = 0.04839 0.01461 0.02065 0.01224 AFIX 43 H25 7 -0.24463 0.55631 0.14072 11.00000 -1.20000 AFIX 0 C26 1 -0.09508 0.55314 0.19418 11.00000 0.05563 0.02717 = 0.04786 0.01512 0.01661 0.02558 AFIX 137 H26A 7 -0.06238 0.54355 0.16790 11.00000 -1.50000 H26B 7 -0.15475 0.49850 0.18026 11.00000 -1.50000 H26C 7 -0.06138 0.56994 0.24108 11.00000 -1.50000 AFIX 0 C27 1 -0.11990 0.68423 0.32705 11.00000 0.06527 0.04180 = 0.03656 0.02507 0.02549 0.03290 AFIX 43 H27 7 -0.18006 0.66256 0.30110 11.00000 -1.20000 AFIX 0 C28 1 -0.10380 0.62951 0.35544 11.00000 0.07730 0.05623 = 0.04958 0.03604 0.03087 0.04434 AFIX 43 H28 7 -0.15269 0.57312 0.35061 11.00000 -1.20000 AFIX 0 C29 1 -0.01785 0.65775 0.38988 11.00000 0.11154 0.06175 = 0.04426 0.03860 0.04527 0.06940 AFIX 43 H29 7 -0.00595 0.62026 0.40769 11.00000 -1.20000 AFIX 0 C30 1 0.05340 0.74285 0.39899 11.00000 0.06856 0.06258 = 0.03069 0.02768 0.03356 0.05359 C31 1 0.03322 0.79871 0.37357 11.00000 0.05231 0.05885 = 0.02512 0.02684 0.02526 0.04370 C32 1 0.14550 0.77977 0.43422 11.00000 0.08858 0.09288 = 0.03953 0.04355 0.04415 0.08195 AFIX 43 H32 7 0.16361 0.74457 0.44972 11.00000 -1.20000 AFIX 0 C33 1 0.20802 0.86629 0.44574 11.00000 0.05591 0.08425 = 0.03664 0.03359 0.02735 0.05626 AFIX 43 H33 7 0.26989 0.89158 0.46964 11.00000 -1.20000 AFIX 0 C34 1 0.18099 0.91881 0.42215 11.00000 0.04988 0.07042 = 0.02469 0.02448 0.02671 0.04686 C35 1 0.24657 1.01153 0.43903 11.00000 0.04582 0.07104 = 0.02658 0.02335 0.01931 0.04484 C36 1 0.34011 1.06091 0.47227 11.00000 0.04809 0.08880 = 0.02582 0.01979 0.01209 0.04580 AFIX 43 H36 7 0.37363 1.03788 0.48803 11.00000 -1.20000 AFIX 0 C37 1 0.37631 1.14906 0.47861 11.00000 0.03752 0.07152 = 0.03876 0.01281 0.00652 0.02502 AFIX 43 H37 7 0.43820 1.19626 0.49875 11.00000 -1.20000 AFIX 0 C38 1 0.30530 1.15501 0.45008 11.00000 0.04382 0.05881 = 0.03032 0.00496 0.00831 0.02223 AFIX 43 H38 7 0.31010 1.20756 0.44733 11.00000 -1.20000 AFIX 0 C39 1 0.13941 1.05643 0.39375 11.00000 0.04514 0.05382 = 0.03971 0.01799 0.01295 0.03463 AFIX 137 H39A 7 0.14660 1.11303 0.39639 11.00000 -1.50000 H39B 7 0.09866 1.02676 0.41560 11.00000 -1.50000 H39C 7 0.11416 1.01884 0.34728 11.00000 -1.50000 AFIX 0 C40 1 0.10021 1.08021 0.24477 11.00000 0.02638 0.02866 = 0.02862 0.01163 0.01190 0.02015 AFIX 43 H40 7 0.05976 1.06737 0.26736 11.00000 -1.20000 AFIX 0 C41 1 0.16703 1.16901 0.25878 11.00000 0.04256 0.02053 = 0.02974 0.00572 0.00814 0.02069 AFIX 43 H41 7 0.17199 1.21500 0.29056 11.00000 -1.20000 AFIX 0 C42 1 0.22474 1.18840 0.22616 11.00000 0.03867 0.01890 = 0.03406 0.01301 0.00877 0.01553 AFIX 43 H42 7 0.27134 1.24819 0.23581 11.00000 -1.20000 AFIX 0 C43 1 0.21511 1.11941 0.17799 11.00000 0.02168 0.02062 = 0.02789 0.01250 0.00677 0.01052 C44 1 0.14509 1.03124 0.16604 11.00000 0.01920 0.02237 = 0.02638 0.01422 0.00786 0.01506 C45 1 0.26930 1.13011 0.13982 11.00000 0.02102 0.02293 = 0.02645 0.01464 0.00422 0.00712 AFIX 43 H45 7 0.31793 1.18759 0.14634 11.00000 -1.20000 AFIX 0 C46 1 0.25194 1.05935 0.09472 11.00000 0.02489 0.03136 = 0.02881 0.01916 0.01552 0.01775 AFIX 43 H46 7 0.28900 1.06666 0.06967 11.00000 -1.20000 AFIX 0 C47 1 0.17786 0.97226 0.08363 11.00000 0.01959 0.02416 = 0.02501 0.01425 0.00770 0.01423 C48 1 0.15815 0.89768 0.03210 11.00000 0.02639 0.02660 = 0.02879 0.01597 0.01301 0.01829 C49 1 0.18574 0.89796 -0.02145 11.00000 0.03576 0.04101 = 0.03120 0.02052 0.02089 0.02677 AFIX 43 H49 7 0.22369 0.94896 -0.03025 11.00000 -1.20000 AFIX 0 C50 1 0.14793 0.81027 -0.05993 11.00000 0.05676 0.05009 = 0.03077 0.02040 0.02594 0.04319 AFIX 43 H50 7 0.15527 0.79105 -0.09952 11.00000 -1.20000 AFIX 0 C51 1 0.09880 0.75756 -0.03040 11.00000 0.04159 0.02626 = 0.03089 0.00517 0.01038 0.02523 AFIX 43 H51 7 0.06626 0.69480 -0.04592 11.00000 -1.20000 AFIX 0 C52 1 0.06858 0.77540 0.07363 11.00000 0.03974 0.01834 = 0.03854 0.01221 0.02226 0.01264 AFIX 137 H52A 7 0.01809 0.78079 0.07326 11.00000 -1.50000 H52B 7 0.11636 0.80981 0.11774 11.00000 -1.50000 H52C 7 0.04785 0.71305 0.06240 11.00000 -1.50000 AFIX 0 F1A 4 0.53656 0.77786 0.31171 11.00000 0.02774 0.02061 = 0.03796 0.01133 0.01296 0.01041 N1A 5 0.30583 0.49599 0.22588 11.00000 0.02041 0.02102 = 0.02574 0.00944 0.01072 0.00930 H1A1 7 0.29779 0.44944 0.24393 11.00000 0.04787 H1A2 7 0.27069 0.51473 0.24285 11.00000 0.06087 C1A 1 0.40729 0.65866 0.31880 11.00000 0.02346 0.02639 = 0.02937 0.01434 0.01191 0.01603 B1A 2 0.40936 0.57706 0.27331 11.00000 0.01648 0.01982 = 0.02972 0.01064 0.00954 0.00830 F2A 4 0.52351 0.90083 0.38091 11.00000 0.04448 0.01776 = 0.03962 0.01068 0.01413 0.01329 N2A 5 0.71679 0.20046 0.23119 11.00000 0.02018 0.02264 = 0.02244 0.00914 0.01074 0.01271 H2A1 7 0.74437 0.23542 0.20517 11.00000 0.02110 H2A2 7 0.71485 0.14612 0.21717 11.00000 0.01534 C2A 1 0.46774 0.74889 0.33322 11.00000 0.02557 0.02671 = 0.02870 0.01305 0.00883 0.01501 B2A 2 0.25556 0.44505 0.14649 11.00000 0.01837 0.02002 = 0.02032 0.00425 0.00988 0.00758 F3A 4 0.39480 0.85620 0.43427 11.00000 0.05008 0.03473 = 0.03534 0.00848 0.01393 0.02940 C3A 1 0.46423 0.81491 0.37096 11.00000 0.02803 0.01943 = 0.02698 0.00675 0.00287 0.01188 B3A 2 0.79870 0.26044 0.30390 11.00000 0.02613 0.02523 = 0.02215 0.00792 0.01185 0.01799 F4A 4 0.27586 0.68295 0.41400 11.00000 0.03115 0.03974 = 0.03473 0.00817 0.01652 0.02140 C4A 1 0.39930 0.79301 0.39804 11.00000 0.04007 0.02938 = 0.02140 0.00678 0.00509 0.02555 B4A 2 0.61140 0.16576 0.20350 11.00000 0.02469 0.02592 = 0.02862 0.01271 0.01647 0.01789 F5A 4 0.28548 0.55624 0.34245 11.00000 0.02738 0.01950 = 0.03977 0.01079 0.01853 0.00849 C5A 1 0.33874 0.70505 0.38742 11.00000 0.02713 0.03373 = 0.02694 0.01262 0.01230 0.02144 F6A 4 0.31883 0.40423 0.30868 11.00000 0.04015 0.02850 = 0.04591 0.02397 0.02681 0.01923 C6A 1 0.34575 0.64219 0.34957 11.00000 0.02265 0.02024 = 0.03119 0.00891 0.00722 0.01196 F7A 4 0.40072 0.37258 0.40244 11.00000 0.07577 0.04973 = 0.05519 0.04008 0.04584 0.04742 C7A 1 0.45054 0.54653 0.33083 11.00000 0.02843 0.02045 = 0.03094 0.01003 0.01498 0.01572 F8A 4 0.57847 0.49276 0.48114 11.00000 0.07797 0.07490 = 0.03393 0.03015 0.02406 0.06290 C8A 1 0.40784 0.46869 0.34479 11.00000 0.03075 0.02990 = 0.03017 0.01341 0.01666 0.01851 F9A 4 0.66941 0.65086 0.46460 11.00000 0.04620 0.05434 = 0.04530 0.01281 0.00108 0.03211 C9A 1 0.44865 0.45095 0.39355 11.00000 0.05949 0.03802 = 0.03501 0.02308 0.03049 0.03745 F10A 4 0.59041 0.68509 0.36892 11.00000 0.02749 0.02810 = 0.04681 0.01297 0.00365 0.01200 C10A 1 0.53641 0.51009 0.43282 11.00000 0.05353 0.06070 = 0.02045 0.01990 0.01647 0.04566 F11A 4 0.40051 0.67831 0.18855 11.00000 0.02704 0.02672 = 0.03618 0.01540 0.00901 0.01441 C11A 1 0.58221 0.58987 0.42485 11.00000 0.04280 0.04265 = 0.03203 0.01189 0.01371 0.02847 F12A 4 0.50577 0.74027 0.12047 11.00000 0.05616 0.03196 = 0.04185 0.02481 0.02189 0.01999 C12A 1 0.53999 0.60529 0.37486 11.00000 0.04094 0.03391 = 0.03327 0.01383 0.01575 0.02644 F13A 4 0.63064 0.70209 0.11811 11.00000 0.05250 0.03880 = 0.06246 0.02726 0.04515 0.01827 C13A 1 0.47028 0.60861 0.22806 11.00000 0.01674 0.01840 = 0.03091 0.00744 0.00807 0.00907 F14A 4 0.64618 0.59755 0.18424 11.00000 0.04256 0.05606 = 0.08113 0.03494 0.04518 0.03303 C14A 1 0.46235 0.65817 0.19018 11.00000 0.02512 0.01755 = 0.03240 0.00672 0.01104 0.00906 F15A 4 0.54548 0.53783 0.25360 11.00000 0.03536 0.04196 = 0.05202 0.02822 0.02582 0.02877 C15A 1 0.51496 0.68999 0.15423 11.00000 0.04107 0.01776 = 0.03215 0.01224 0.01666 0.00858 F16A 4 0.24020 0.59945 0.20653 11.00000 0.03489 0.02464 = 0.03378 0.00649 0.01546 0.01695 C16A 1 0.57770 0.67048 0.15278 11.00000 0.03297 0.02577 = 0.03712 0.01238 0.02341 0.00772 F17A 4 0.15717 0.65766 0.13836 11.00000 0.03736 0.02766 = 0.05433 0.01031 0.01885 0.02392 C17A 1 0.58630 0.61920 0.18663 11.00000 0.02635 0.03259 = 0.04772 0.01342 0.02209 0.01624 F18A 4 0.07413 0.58033 0.00408 11.00000 0.02585 0.03102 = 0.05907 0.02424 0.01038 0.01588 C18A 1 0.53395 0.58988 0.22358 11.00000 0.02301 0.02584 = 0.03738 0.01426 0.01186 0.01056 F19A 4 0.07210 0.43887 -0.05930 11.00000 0.03670 0.03382 = 0.03509 0.01563 0.00888 0.01467 C19A 1 0.20674 0.48743 0.11052 11.00000 0.01722 0.01777 = 0.03231 0.01096 0.01662 0.00762 F20A 4 0.15296 0.37648 0.00804 11.00000 0.03219 0.02672 = 0.02944 0.00872 0.01442 0.01771 C20A 1 0.20169 0.55810 0.14074 11.00000 0.01974 0.01999 = 0.03206 0.00882 0.01261 0.00882 F21A 4 0.12897 0.41020 0.21299 11.00000 0.02427 0.02188 = 0.03837 0.00489 0.01861 0.01061 C21A 1 0.15823 0.58929 0.10596 11.00000 0.02073 0.01851 = 0.04337 0.01084 0.01732 0.01092 F22A 4 -0.00240 0.25581 0.20853 11.00000 0.02664 0.03448 = 0.03816 0.01023 0.02182 0.01149 C22A 1 0.11619 0.55065 0.03865 11.00000 0.01775 0.02090 = 0.04724 0.01893 0.01364 0.01043 F23A 4 -0.04018 0.10007 0.12861 11.00000 0.02646 0.02040 = 0.04028 0.01420 0.01466 0.00515 C23A 1 0.11585 0.47854 0.00661 11.00000 0.01961 0.02745 = 0.02304 0.00873 0.00660 0.00462 F24A 4 0.05508 0.10587 0.04993 11.00000 0.03197 0.01927 = 0.04033 0.00539 0.01522 0.01047 C24A 1 0.15817 0.44899 0.04222 11.00000 0.02267 0.02192 = 0.02941 0.01043 0.01550 0.01097 F25A 4 0.18759 0.25750 0.05414 11.00000 0.03233 0.02262 = 0.04159 0.00712 0.02340 0.01341 C25A 1 0.16994 0.34405 0.13698 11.00000 0.01629 0.02049 = 0.02811 0.01125 0.01114 0.01055 F26A 4 0.34790 0.36503 0.18989 11.00000 0.03344 0.03098 = 0.04099 0.02255 0.02214 0.02147 C26A 1 0.11549 0.33500 0.17310 11.00000 0.02147 0.01854 = 0.02596 0.00445 0.00830 0.01170 F27A 4 0.44829 0.32920 0.13820 11.00000 0.04720 0.04232 = 0.07097 0.03837 0.03764 0.03832 C27A 1 0.04659 0.25738 0.17151 11.00000 0.01925 0.02739 = 0.02503 0.00817 0.01170 0.01153 F28A 4 0.47685 0.37115 0.03042 11.00000 0.06311 0.05417 = 0.08119 0.04066 0.05749 0.04726 C28A 1 0.02616 0.17874 0.13063 11.00000 0.02037 0.01543 = 0.03241 0.01265 0.00768 0.00522 F29A 4 0.40803 0.45962 -0.01862 11.00000 0.05155 0.04675 = 0.05120 0.03099 0.03953 0.03428 C29A 1 0.07461 0.18188 0.09116 11.00000 0.02584 0.01918 = 0.03428 0.00878 0.01105 0.01545 F30A 4 0.32339 0.51031 0.03938 11.00000 0.03189 0.03120 = 0.04004 0.02127 0.02195 0.02162 C30A 1 0.14434 0.26258 0.09536 11.00000 0.02361 0.02086 = 0.03256 0.01479 0.01759 0.01470 F31A 4 0.83452 0.30597 0.18029 11.00000 0.03058 0.02672 = 0.02536 0.00953 0.01585 0.01388 C31A 1 0.32551 0.43514 0.11573 11.00000 0.02269 0.01400 = 0.03211 0.01123 0.01458 0.01000 F32A 4 0.98349 0.43853 0.18252 11.00000 0.03438 0.03387 = 0.04323 0.02381 0.02500 0.02077 C32A 1 0.36281 0.39194 0.13842 11.00000 0.02411 0.02188 = 0.03272 0.01317 0.01623 0.01148 F33A 4 1.12122 0.56184 0.29825 11.00000 0.02851 0.02980 = 0.06419 0.02230 0.01846 0.00731 C33A 1 0.41491 0.37196 0.11250 11.00000 0.02729 0.02583 = 0.04770 0.02218 0.02137 0.01874 F34A 4 1.10604 0.54098 0.41523 11.00000 0.03616 0.03260 = 0.04144 0.00793 0.00165 0.00449 C34A 1 0.42997 0.39389 0.05849 11.00000 0.03183 0.02972 = 0.05765 0.02036 0.02959 0.02106 F35A 4 0.95837 0.40450 0.41473 11.00000 0.03896 0.03317 = 0.02721 0.00858 0.00833 0.01578 C35A 1 0.39563 0.43754 0.03405 11.00000 0.03048 0.03085 = 0.03484 0.01660 0.02250 0.01749 F36A 4 0.86735 0.25017 0.43990 11.00000 0.03828 0.03986 = 0.02417 0.01232 0.01521 0.02709 C36A 1 0.34808 0.46048 0.06457 11.00000 0.02334 0.02043 = 0.03487 0.01376 0.01202 0.01216 F37A 4 0.95351 0.17390 0.46869 11.00000 0.03653 0.04613 = 0.03379 0.02253 0.01372 0.02918 C37A 1 0.88585 0.34743 0.29876 11.00000 0.02592 0.01643 = 0.02709 0.00605 0.00904 0.01501 F38A 4 0.99060 0.09480 0.37457 11.00000 0.03260 0.03494 = 0.04689 0.01947 0.01213 0.02577 C38A 1 0.89871 0.36122 0.24134 11.00000 0.02313 0.01977 = 0.02754 0.00687 0.00824 0.01454 F39A 4 0.92983 0.08695 0.24847 11.00000 0.02478 0.02649 = 0.04154 0.01041 0.01722 0.01860 C39A 1 0.97696 0.43042 0.24048 11.00000 0.02785 0.03032 = 0.03771 0.01980 0.01859 0.01914 F40A 4 0.83475 0.15430 0.21582 11.00000 0.02351 0.03171 = 0.02421 0.01129 0.01190 0.01774 C40A 1 1.04695 0.49252 0.29890 11.00000 0.02359 0.02472 = 0.04599 0.01543 0.01234 0.01290 F41A 4 0.68352 0.14277 0.36132 11.00000 0.03008 0.03548 = 0.03369 0.01574 0.01684 0.01652 C41A 1 1.03815 0.48258 0.35669 11.00000 0.02558 0.02352 = 0.03568 0.00361 0.00339 0.01079 F42A 4 0.60926 0.17987 0.44119 11.00000 0.04840 0.08930 = 0.04359 0.03953 0.03357 0.04574 C42A 1 0.96035 0.41066 0.35533 11.00000 0.03434 0.02850 = 0.02829 0.01288 0.01302 0.01821 F43A 4 0.64019 0.34460 0.48173 11.00000 0.11729 0.13109 = 0.05867 0.05486 0.06603 0.11166 C43A 1 0.84347 0.20552 0.32504 11.00000 0.01891 0.02057 = 0.02880 0.01227 0.01105 0.01122 F44A 4 0.74965 0.47081 0.44038 11.00000 0.13104 0.07866 = 0.05643 0.02683 0.05026 0.09000 C44A 1 0.87780 0.20760 0.38864 11.00000 0.01964 0.02111 = 0.03022 0.01145 0.01143 0.01206 F45A 4 0.82381 0.43646 0.36109 11.00000 0.06183 0.03462 = 0.04041 0.01607 0.02300 0.03579 C45A 1 0.92424 0.17024 0.40607 11.00000 0.02122 0.02836 = 0.02291 0.01174 0.00369 0.01446 F46A 4 0.65660 0.03810 0.24384 11.00000 0.01825 0.02677 = 0.03993 0.01484 0.01336 0.01486 C46A 1 0.94246 0.12926 0.35818 11.00000 0.01862 0.02403 = 0.03539 0.01276 0.00654 0.01305 F47A 4 0.53969 -0.11832 0.24315 11.00000 0.03283 0.02851 = 0.04309 0.02100 0.01721 0.02013 C47A 1 0.91177 0.12535 0.29531 11.00000 0.02190 0.02096 = 0.03320 0.00979 0.01252 0.01368 F48A 4 0.36019 -0.18360 0.20391 11.00000 0.02986 0.03310 = 0.05378 0.02362 0.02172 0.01372 C48A 1 0.86310 0.16193 0.27969 11.00000 0.01610 0.01837 = 0.02398 0.00820 0.00831 0.01044 F49A 4 0.30131 -0.08567 0.16104 11.00000 0.01874 0.04844 = 0.05342 0.02533 0.01592 0.01808 C49A 1 0.75891 0.28709 0.35659 11.00000 0.02771 0.04085 = 0.02047 0.00874 0.00909 0.02610 F50A 4 0.41863 0.07346 0.16206 11.00000 0.02604 0.04440 = 0.04541 0.02843 0.01553 0.02567 C50A 1 0.70322 0.22591 0.38005 11.00000 0.03476 0.04006 = 0.02338 0.00943 0.00667 0.02953 F51A 4 0.50489 0.16920 0.29219 11.00000 0.04133 0.05123 = 0.04421 0.03009 0.03077 0.03350 C51A 1 0.66417 0.24383 0.42226 11.00000 0.03891 0.07208 = 0.03259 0.02910 0.02352 0.03957 F52A 4 0.49548 0.30416 0.34169 11.00000 0.10661 0.10285 = 0.07242 0.06076 0.07321 0.09352 C52A 1 0.67972 0.32654 0.44310 11.00000 0.07484 0.08175 = 0.03495 0.03002 0.03514 0.06799 F53A 4 0.59231 0.46006 0.32388 11.00000 0.14729 0.08248 = 0.07154 0.04926 0.07380 0.10319 C53A 1 0.73492 0.38993 0.42250 11.00000 0.07890 0.06018 = 0.03453 0.01598 0.02532 0.05976 F54A 4 0.69368 0.47509 0.24814 11.00000 0.08601 0.04112 = 0.05207 0.02728 0.03588 0.04751 C54A 1 0.77294 0.36990 0.38032 11.00000 0.04389 0.04241 = 0.02259 0.01328 0.01240 0.03291 F55A 4 0.70385 0.34009 0.19738 11.00000 0.03782 0.02957 = 0.03507 0.01439 0.02028 0.02208 C55A 1 0.54485 0.06846 0.20708 11.00000 0.01963 0.02893 = 0.02661 0.01202 0.01221 0.01463 F56A 4 0.49243 0.20888 0.11724 11.00000 0.03833 0.04584 = 0.03431 0.01851 0.01437 0.03440 C56A 1 0.56917 0.01305 0.22531 11.00000 0.02349 0.02755 = 0.02584 0.00996 0.01163 0.01539 F57A 4 0.44796 0.17521 -0.01015 11.00000 0.03194 0.04005 = 0.03694 0.02068 0.00714 0.02225 C57A 1 0.50957 -0.07013 0.22414 11.00000 0.02881 0.03205 = 0.02452 0.01500 0.01225 0.02085 F58A 4 0.50880 0.09777 -0.08106 11.00000 0.03356 0.03941 = 0.02387 0.01533 0.00906 0.01394 C58A 1 0.41860 -0.10360 0.20386 11.00000 0.02074 0.02777 = 0.03373 0.01632 0.01548 0.00798 F59A 4 0.61530 0.04956 -0.01964 11.00000 0.02864 0.03201 = 0.02459 0.00537 0.01386 0.01279 C59A 1 0.39003 -0.05347 0.18279 11.00000 0.01658 0.03783 = 0.03347 0.01895 0.01298 0.01479 F60A 4 0.65952 0.07822 0.10892 11.00000 0.02390 0.02653 = 0.02744 0.00870 0.00940 0.01624 C60A 1 0.45179 0.02845 0.18399 11.00000 0.02776 0.03701 = 0.03015 0.02015 0.01494 0.02245 C61A 1 0.60290 0.24537 0.23962 11.00000 0.02877 0.03621 = 0.02094 0.01304 0.01031 0.02576 C62A 1 0.55166 0.24216 0.27739 11.00000 0.03940 0.05008 = 0.03498 0.02806 0.02060 0.03718 C63A 1 0.54486 0.31165 0.30375 11.00000 0.06898 0.06818 = 0.04489 0.03646 0.04106 0.05900 C64A 1 0.59281 0.39025 0.29487 11.00000 0.08914 0.06793 = 0.04058 0.03066 0.03685 0.06977 C65A 1 0.64615 0.39892 0.25841 11.00000 0.06360 0.03967 = 0.03615 0.02406 0.02595 0.04112 C66A 1 0.64979 0.32758 0.23260 11.00000 0.03013 0.03427 = 0.02688 0.01342 0.01213 0.02433 C67A 1 0.58226 0.14888 0.12270 11.00000 0.01748 0.02049 = 0.02717 0.01105 0.00976 0.01093 C68A 1 0.52640 0.16923 0.08711 11.00000 0.02150 0.02309 = 0.02934 0.01226 0.01136 0.01099 C69A 1 0.50263 0.15326 0.02030 11.00000 0.01663 0.02542 = 0.03182 0.01243 0.00312 0.00666 C70A 1 0.53298 0.11392 -0.01586 11.00000 0.02342 0.02616 = 0.02050 0.01272 0.00625 0.00761 C71A 1 0.58702 0.09124 0.01518 11.00000 0.01964 0.02047 = 0.02457 0.00369 0.01025 0.00491 C72A 1 0.60904 0.10768 0.08234 11.00000 0.01343 0.02165 = 0.03054 0.01515 0.00831 0.00700 Cl1S 3 0.27562 0.74106 0.03295 11.00000 0.06020 0.07262 = 0.19640 0.09262 0.07300 0.04026 C1S 1 0.32441 0.68165 0.02298 11.00000 0.06133 0.09887 = 0.13816 0.07667 0.03353 0.03152 AFIX 23 H1S1 7 0.38959 0.72266 0.05013 11.00000 -1.20000 H1S2 7 0.29942 0.63534 0.04252 11.00000 -1.20000 AFIX 0 Cl2S 3 0.31479 0.63305 -0.05091 11.00000 0.18333 0.04925 = 0.07190 0.01180 0.02444 0.04018 C2S 1 0.19994 0.38147 0.43018 11.00000 0.04599 0.07125 = 0.05550 0.01246 0.00538 -0.00510 AFIX 23 H2S1 7 0.22756 0.44558 0.45130 11.00000 -1.20000 H2S2 7 0.24869 0.37288 0.42893 11.00000 -1.20000 AFIX 0 Cl3S 3 0.14395 0.32389 0.47709 11.00000 0.05234 0.12608 = 0.08237 0.05678 -0.00531 -0.00931 Cl4S 3 0.12460 0.34341 0.34977 11.00000 0.04917 0.06050 = 0.04984 0.01131 0.01414 0.03355 HKLF 4 ; #===END _database_code_depnum_ccdc_archive 'CCDC 952838' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H26 N4 O4 Pd, C H2 Cl2' _chemical_formula_sum 'C33 H28 Cl2 N4 O4 Pd' _chemical_formula_weight 721.89 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' Cl Cl 0.1484 0.1585 '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 Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 15.8053(16) _cell_length_b 19.5063(19) _cell_length_c 20.140(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6209.3(11) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7479 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 22.02 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7581 _exptl_absorpt_correction_T_max 0.8673 _exptl_absorpt_process_details SADABS _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 SMART APEX' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54617 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.33 _reflns_number_total 15248 _reflns_number_gt 10472 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ciftab _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^)+(0.0752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 15248 _refine_ls_number_parameters 797 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1528 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.15897(3) 0.85662(2) 0.35239(2) 0.03759(12) Uani 1 1 d . . . O1 O 0.1356(3) 0.8527(2) 0.2536(2) 0.0390(10) Uani 1 1 d . . . N1 N 0.2828(3) 0.8386(3) 0.3362(3) 0.0482(14) Uani 1 1 d . . . C1 C 0.1255(4) 0.7959(3) 0.2269(3) 0.0437(15) Uani 1 1 d . . . Pd2 Pd 0.06238(3) 0.355853(19) 0.23926(2) 0.03894(12) Uani 1 1 d . . . O2 O 0.1351(3) 0.7384(2) 0.2524(2) 0.0497(11) Uani 1 1 d . . . N2 N 0.3191(3) 0.9484(3) 0.3626(3) 0.0551(15) Uani 1 1 d . . . C2 C 0.0953(4) 0.7996(4) 0.1540(3) 0.0520(16) Uani 1 1 d . . . H2A H 0.1098 0.7568 0.1312 0.078 Uiso 1 1 calc R . . H2B H 0.1232 0.8381 0.1317 0.078 Uiso 1 1 calc R . . H2C H 0.0339 0.8062 0.1529 0.078 Uiso 1 1 calc R . . O3 O 0.0340(3) 0.86616(19) 0.3671(2) 0.0386(10) Uani 1 1 d . . . N3 N 0.1807(3) 0.8731(3) 0.4500(3) 0.0391(12) Uani 1 1 d . . . C3 C 0.0033(4) 0.9267(3) 0.3710(3) 0.0452(15) Uani 1 1 d . . . O4 O 0.0429(3) 0.9809(2) 0.3661(3) 0.0589(14) Uani 1 1 d . . . N4 N 0.1984(3) 0.7574(3) 0.4690(2) 0.0389(11) Uani 1 1 d . . . C4 C -0.0911(4) 0.9286(4) 0.3812(4) 0.062(2) Uani 1 1 d . . . H4A H -0.1058 0.9677 0.4094 0.092 Uiso 1 1 calc R . . H4B H -0.1095 0.8860 0.4027 0.092 Uiso 1 1 calc R . . H4C H -0.1194 0.9332 0.3382 0.092 Uiso 1 1 calc R . . O5 O 0.1896(3) 0.3766(2) 0.2375(2) 0.0426(9) Uani 1 1 d . . . N5 N 0.0569(3) 0.3627(3) 0.1387(3) 0.0426(15) Uani 1 1 d . . . C5 C 0.2091(4) 0.4338(4) 0.2469(3) 0.0514(16) Uani 1 1 d . . . O6 O 0.1586(3) 0.4855(2) 0.2448(3) 0.0617(14) Uani 1 1 d . . . N6 N 0.0363(3) 0.2456(3) 0.1273(3) 0.0405(12) Uani 1 1 d . . . C6 C 0.3000(5) 0.4467(4) 0.2621(5) 0.077(3) Uani 1 1 d . . . H6A H 0.3085 0.4459 0.3103 0.115 Uiso 1 1 calc R . . H6B H 0.3165 0.4917 0.2447 0.115 Uiso 1 1 calc R . . H6C H 0.3348 0.4110 0.2414 0.115 Uiso 1 1 calc R . . O7 O 0.0734(3) 0.3582(2) 0.3385(2) 0.0403(12) Uani 1 1 d . . . N7 N -0.0631(4) 0.3313(3) 0.2477(3) 0.0478(13) Uani 1 1 d . . . C7 C 0.0924(4) 0.3030(3) 0.3691(3) 0.0405(14) Uani 1 1 d . . . O8 O 0.0911(3) 0.2444(2) 0.3448(3) 0.0537(11) Uani 1 1 d . . . N8 N -0.1034(3) 0.4387(3) 0.2082(3) 0.0476(14) Uani 1 1 d . . . C8 C 0.1190(5) 0.3130(4) 0.4401(4) 0.0585(19) Uani 1 1 d . . . H8A H 0.1118 0.2700 0.4645 0.088 Uiso 1 1 calc R . . H8B H 0.0839 0.3487 0.4605 0.088 Uiso 1 1 calc R . . H8C H 0.1785 0.3269 0.4416 0.088 Uiso 1 1 calc R . . C11 C 0.3068(4) 0.7750(4) 0.3187(3) 0.0509(17) Uani 1 1 d . . . H11 H 0.2648 0.7402 0.3168 0.061 Uiso 1 1 calc R . . C12 C 0.3920(5) 0.7567(5) 0.3025(4) 0.064(2) Uani 1 1 d . . . H12 H 0.4065 0.7107 0.2920 0.077 Uiso 1 1 calc R . . C13 C 0.4501(5) 0.8054(5) 0.3028(4) 0.065(2) Uani 1 1 d . . . H13 H 0.5066 0.7947 0.2904 0.078 Uiso 1 1 calc R . . C14 C 0.4295(4) 0.8725(4) 0.3211(3) 0.0561(19) Uani 1 1 d . . . C15 C 0.3445(4) 0.8874(4) 0.3391(3) 0.0475(16) Uani 1 1 d . . . C16 C 0.4856(5) 0.9270(5) 0.3229(4) 0.074(3) Uani 1 1 d . . . H16 H 0.5423 0.9202 0.3086 0.089 Uiso 1 1 calc R . . C17 C 0.4615(4) 0.9892(4) 0.3443(4) 0.068(2) Uani 1 1 d . . . H17 H 0.5000 1.0266 0.3434 0.081 Uiso 1 1 calc R . . C18 C 0.3785(4) 0.9982(4) 0.3681(4) 0.063(2) Uani 1 1 d . . . C19 C 0.3500(5) 1.0633(4) 0.3988(4) 0.065(2) Uani 1 1 d . . . C20 C 0.4087(5) 1.1063(5) 0.4294(5) 0.084(3) Uani 1 1 d . . . H20 H 0.4664 1.0929 0.4317 0.101 Uiso 1 1 calc R . . C21 C 0.3841(6) 1.1672(5) 0.4562(6) 0.092(3) Uani 1 1 d . . . H21 H 0.4251 1.1961 0.4763 0.110 Uiso 1 1 calc R . . C22 C 0.3036(6) 1.1870(5) 0.4548(5) 0.083(3) Uani 1 1 d . . . H22 H 0.2882 1.2294 0.4745 0.100 Uiso 1 1 calc R . . C23 C 0.2417(6) 1.1470(4) 0.4252(6) 0.084(3) Uani 1 1 d . . . H23 H 0.1844 1.1619 0.4249 0.100 Uiso 1 1 calc R . . C24 C 0.2643(5) 1.0840(5) 0.3955(5) 0.080(3) Uani 1 1 d . . . H24 H 0.2231 1.0563 0.3739 0.096 Uiso 1 1 calc R . . C25 C 0.1764(4) 0.9371(4) 0.4726(4) 0.0527(17) Uani 1 1 d . . . H25 H 0.1616 0.9721 0.4420 0.063 Uiso 1 1 calc R . . C26 C 0.1921(5) 0.9564(4) 0.5379(4) 0.066(2) Uani 1 1 d . . . H26 H 0.1874 1.0028 0.5515 0.079 Uiso 1 1 calc R . . C27 C 0.2145(5) 0.9064(4) 0.5815(4) 0.068(2) Uani 1 1 d . . . H27 H 0.2255 0.9177 0.6266 0.082 Uiso 1 1 calc R . . C28 C 0.2215(4) 0.8377(4) 0.5600(3) 0.0528(17) Uani 1 1 d . . . C29 C 0.2018(4) 0.8216(4) 0.4936(3) 0.0428(15) Uani 1 1 d . . . C30 C 0.2418(5) 0.7821(4) 0.6013(4) 0.065(2) Uani 1 1 d . . . H30 H 0.2573 0.7898 0.6463 0.078 Uiso 1 1 calc R . . C31 C 0.2392(5) 0.7180(5) 0.5770(4) 0.064(2) Uani 1 1 d . . . H31 H 0.2535 0.6803 0.6047 0.077 Uiso 1 1 calc R . . C32 C 0.2155(4) 0.7068(4) 0.5107(3) 0.0474(16) Uani 1 1 d . . . C33 C 0.2071(4) 0.6362(4) 0.4831(3) 0.0484(16) Uani 1 1 d . . . C34 C 0.2123(6) 0.5766(4) 0.5208(4) 0.079(3) Uani 1 1 d . . . H34 H 0.2235 0.5802 0.5671 0.094 Uiso 1 1 calc R . . C35 C 0.2018(7) 0.5136(5) 0.4937(5) 0.095(3) Uani 1 1 d . . . H35 H 0.2041 0.4742 0.5214 0.114 Uiso 1 1 calc R . . C36 C 0.1880(5) 0.5060(4) 0.4271(4) 0.068(2) Uani 1 1 d . . . H36 H 0.1797 0.4618 0.4084 0.081 Uiso 1 1 calc R . . C37 C 0.1863(4) 0.5625(4) 0.3886(4) 0.0563(18) Uani 1 1 d . . . H37 H 0.1817 0.5574 0.3418 0.068 Uiso 1 1 calc R . . C38 C 0.1912(5) 0.6269(4) 0.4150(4) 0.0547(18) Uani 1 1 d . . . H38 H 0.1838 0.6657 0.3871 0.066 Uiso 1 1 calc R . . C39 C 0.0669(5) 0.4251(4) 0.1126(4) 0.060(2) Uani 1 1 d . . . H39 H 0.0816 0.4623 0.1408 0.072 Uiso 1 1 calc R . . C40 C 0.0563(6) 0.4368(4) 0.0442(4) 0.071(2) Uani 1 1 d . . . H40 H 0.0632 0.4819 0.0272 0.086 Uiso 1 1 calc R . . C41 C 0.0364(5) 0.3854(4) 0.0025(4) 0.063(2) Uani 1 1 d . . . H41 H 0.0277 0.3936 -0.0435 0.076 Uiso 1 1 calc R . . C42 C 0.0288(4) 0.3186(4) 0.0295(3) 0.0551(18) Uani 1 1 d . . . C43 C 0.0401(4) 0.3074(3) 0.0984(3) 0.0412(14) Uani 1 1 d . . . C44 C 0.0135(4) 0.2580(4) -0.0093(3) 0.0550(17) Uani 1 1 d . . . H44 H 0.0058 0.2613 -0.0559 0.066 Uiso 1 1 calc R . . C45 C 0.0102(4) 0.1966(4) 0.0209(4) 0.0573(18) Uani 1 1 d . . . H45 H -0.0013 0.1568 -0.0047 0.069 Uiso 1 1 calc R . . C46 C 0.0233(4) 0.1903(3) 0.0897(3) 0.0458(15) Uani 1 1 d . . . C47 C 0.0246(4) 0.1239(3) 0.1216(4) 0.0487(16) Uani 1 1 d . . . C48 C 0.0090(5) 0.1169(4) 0.1880(5) 0.068(2) Uani 1 1 d . . . H48 H -0.0046 0.1569 0.2127 0.081 Uiso 1 1 calc R . . C49 C 0.0118(5) 0.0534(4) 0.2220(6) 0.088(3) Uani 1 1 d . . . H49 H 0.0010 0.0510 0.2683 0.106 Uiso 1 1 calc R . . C50 C 0.0304(5) -0.0040(4) 0.1865(7) 0.085(3) Uani 1 1 d . . . H50 H 0.0313 -0.0476 0.2075 0.103 Uiso 1 1 calc R . . C51 C 0.0483(7) 0.0019(5) 0.1182(6) 0.097(4) Uani 1 1 d . . . H51 H 0.0627 -0.0379 0.0934 0.116 Uiso 1 1 calc R . . C52 C 0.0450(6) 0.0637(4) 0.0877(5) 0.079(3) Uani 1 1 d . . . H52 H 0.0570 0.0662 0.0416 0.095 Uiso 1 1 calc R . . C53 C -0.0817(6) 0.2710(4) 0.2717(4) 0.066(2) Uani 1 1 d . . . H53 H -0.0366 0.2409 0.2828 0.079 Uiso 1 1 calc R . . C54 C -0.1635(7) 0.2489(6) 0.2818(4) 0.086(3) Uani 1 1 d . . . H54 H -0.1743 0.2046 0.2997 0.103 Uiso 1 1 calc R . . C55 C -0.2280(7) 0.2909(7) 0.2661(4) 0.093(4) Uani 1 1 d . . . H55 H -0.2846 0.2754 0.2708 0.111 Uiso 1 1 calc R . . C56 C -0.2120(5) 0.3579(5) 0.2427(4) 0.069(2) Uani 1 1 d . . . C57 C -0.1266(4) 0.3768(4) 0.2313(3) 0.0548(18) Uani 1 1 d . . . C58 C -0.2747(5) 0.4075(7) 0.2304(4) 0.097(4) Uani 1 1 d . . . H58 H -0.3327 0.3964 0.2366 0.116 Uiso 1 1 calc R . . C59 C -0.2523(5) 0.4707(7) 0.2099(4) 0.094(3) Uani 1 1 d . . . H59 H -0.2940 0.5053 0.2039 0.112 Uiso 1 1 calc R . . C60 C -0.1658(4) 0.4851(5) 0.1972(3) 0.059(2) Uani 1 1 d . . . C61 C -0.1395(5) 0.5534(4) 0.1697(3) 0.0572(19) Uani 1 1 d . . . C62 C -0.0546(5) 0.5686(5) 0.1601(5) 0.079(3) Uani 1 1 d . . . H62 H -0.0128 0.5355 0.1715 0.094 Uiso 1 1 calc R . . C63 C -0.0302(7) 0.6302(5) 0.1346(5) 0.088(3) Uani 1 1 d . . . H63 H 0.0283 0.6394 0.1282 0.105 Uiso 1 1 calc R . . C64 C -0.0893(6) 0.6796(4) 0.1179(4) 0.069(2) Uani 1 1 d . . . H64 H -0.0717 0.7228 0.1011 0.083 Uiso 1 1 calc R . . C65 C -0.1712(6) 0.6657(5) 0.1257(6) 0.092(3) Uani 1 1 d . . . H65 H -0.2123 0.6982 0.1118 0.110 Uiso 1 1 calc R . . C66 C -0.1978(5) 0.6030(5) 0.1543(5) 0.085(3) Uani 1 1 d . . . H66 H -0.2561 0.5953 0.1630 0.102 Uiso 1 1 calc R . . Cl1S Cl 0.2956(2) 1.1179(2) 0.60292(16) 0.1366(14) Uani 1 1 d . . . C1S C 0.2580(6) 1.1208(4) 0.6825(5) 0.076(2) Uani 1 1 d . . . H1S1 H 0.2781 1.1631 0.7047 0.091 Uiso 1 1 calc R . . H1S2 H 0.2794 1.0809 0.7079 0.091 Uiso 1 1 calc R . . Cl2S Cl 0.14590(18) 1.11958(15) 0.68142(16) 0.1004(8) Uani 1 1 d . . . C2S C 0.0087(5) -0.1250(4) -0.0676(4) 0.067(2) Uani 1 1 d . . . H2S1 H -0.0098 -0.1633 -0.0964 0.081 Uiso 1 1 calc R . . H2S2 H -0.0079 -0.0814 -0.0891 0.081 Uiso 1 1 calc R . . Cl3S Cl -0.04116(19) -0.13168(13) 0.01063(12) 0.0910(8) Uani 1 1 d . . . Cl4S Cl 0.1193(2) -0.12770(15) -0.05784(19) 0.1151(11) 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 0.0367(2) 0.0420(2) 0.0341(2) 0.0041(2) 0.0040(2) 0.00416(18) O1 0.053(2) 0.037(2) 0.027(2) 0.0019(18) 0.004(2) 0.0028(18) N1 0.044(3) 0.064(4) 0.036(3) 0.016(3) 0.002(2) 0.014(3) C1 0.036(3) 0.044(4) 0.052(4) -0.001(3) 0.003(3) -0.003(3) Pd2 0.0511(3) 0.0284(2) 0.0373(2) -0.0032(2) 0.0109(2) -0.00633(18) O2 0.051(3) 0.033(2) 0.065(3) 0.008(2) 0.007(2) 0.0055(19) N2 0.047(3) 0.059(3) 0.060(4) 0.029(3) 0.007(3) 0.007(3) C2 0.060(4) 0.050(4) 0.047(4) -0.005(3) 0.000(3) -0.002(3) O3 0.032(2) 0.040(2) 0.043(3) -0.0015(18) 0.0001(18) -0.0012(16) N3 0.029(2) 0.052(3) 0.037(3) 0.008(2) 0.005(2) -0.004(2) C3 0.050(4) 0.045(4) 0.041(4) -0.008(3) -0.001(3) 0.006(3) O4 0.057(3) 0.042(3) 0.078(4) -0.008(3) -0.005(3) 0.007(2) N4 0.032(3) 0.052(3) 0.032(3) 0.006(2) 0.006(2) 0.002(2) C4 0.049(4) 0.071(5) 0.065(5) -0.010(4) -0.006(3) 0.015(4) O5 0.040(2) 0.043(2) 0.044(2) 0.005(2) 0.020(2) 0.0115(18) N5 0.052(3) 0.044(3) 0.032(3) 0.001(2) 0.013(2) -0.010(2) C5 0.036(3) 0.078(5) 0.041(4) -0.014(4) 0.009(3) 0.000(3) O6 0.060(3) 0.037(2) 0.087(4) -0.008(3) 0.003(3) 0.000(2) N6 0.037(3) 0.044(3) 0.041(3) -0.009(2) 0.000(2) -0.001(2) C6 0.080(6) 0.053(4) 0.097(7) -0.018(4) -0.013(5) 0.004(4) O7 0.057(3) 0.028(2) 0.036(3) -0.0045(18) 0.0088(19) 0.0002(17) N7 0.057(3) 0.050(3) 0.037(3) -0.007(3) 0.007(3) -0.024(3) C7 0.035(3) 0.043(4) 0.043(4) -0.001(3) 0.011(3) 0.002(3) O8 0.069(3) 0.031(2) 0.061(3) -0.001(2) 0.020(3) 0.005(2) N8 0.040(3) 0.070(4) 0.033(3) -0.010(3) 0.004(2) -0.004(3) C8 0.058(4) 0.047(4) 0.070(5) 0.011(4) -0.012(4) 0.004(3) C11 0.050(4) 0.062(4) 0.040(4) 0.008(3) 0.006(3) 0.012(3) C12 0.067(5) 0.079(6) 0.047(4) 0.015(4) 0.013(4) 0.032(4) C13 0.045(4) 0.099(7) 0.050(4) 0.020(4) 0.011(3) 0.018(4) C14 0.040(4) 0.090(6) 0.038(4) 0.025(4) 0.009(3) 0.008(4) C15 0.046(3) 0.061(4) 0.036(4) 0.023(3) 0.000(3) 0.003(3) C16 0.041(4) 0.114(8) 0.066(5) 0.037(5) 0.016(4) 0.005(5) C17 0.045(4) 0.072(5) 0.087(6) 0.042(5) 0.012(4) -0.001(4) C18 0.034(3) 0.069(5) 0.087(6) 0.050(4) -0.003(3) -0.008(3) C19 0.050(4) 0.055(5) 0.090(6) 0.045(4) 0.008(4) 0.003(3) C20 0.046(5) 0.081(7) 0.125(8) 0.056(6) -0.009(5) -0.013(4) C21 0.069(6) 0.059(5) 0.147(10) 0.045(6) 0.007(6) -0.020(5) C22 0.072(6) 0.056(5) 0.120(8) 0.047(5) 0.008(5) 0.002(4) C23 0.061(5) 0.059(5) 0.131(9) 0.031(5) 0.015(6) 0.011(4) C24 0.069(5) 0.082(6) 0.090(6) 0.055(5) 0.007(5) 0.000(5) C25 0.041(4) 0.057(4) 0.060(5) -0.012(4) 0.001(3) -0.004(3) C26 0.079(5) 0.052(4) 0.066(5) -0.001(4) -0.016(4) -0.022(4) C27 0.073(5) 0.066(5) 0.065(5) -0.006(4) -0.023(4) -0.019(4) C28 0.045(4) 0.071(5) 0.043(4) 0.002(3) -0.008(3) -0.010(3) C29 0.033(3) 0.064(4) 0.032(3) 0.000(3) 0.007(3) -0.013(3) C30 0.083(6) 0.067(5) 0.044(4) -0.004(4) -0.019(4) -0.012(4) C31 0.061(5) 0.085(6) 0.047(4) 0.017(4) -0.013(4) 0.005(4) C32 0.045(4) 0.057(4) 0.040(4) 0.004(3) 0.006(3) -0.002(3) C33 0.035(3) 0.065(4) 0.045(4) 0.012(3) 0.002(3) 0.003(3) C34 0.127(8) 0.055(5) 0.054(5) 0.017(4) -0.004(5) 0.009(5) C35 0.156(10) 0.055(5) 0.074(6) 0.019(5) 0.009(6) 0.007(6) C36 0.075(5) 0.057(5) 0.072(6) -0.002(4) 0.013(4) -0.008(4) C37 0.046(4) 0.066(5) 0.057(4) 0.002(4) -0.005(3) -0.006(3) C38 0.054(4) 0.048(4) 0.062(5) 0.003(3) -0.012(4) -0.009(3) C39 0.069(5) 0.060(5) 0.049(4) 0.008(4) 0.024(4) -0.010(4) C40 0.100(7) 0.060(5) 0.054(5) 0.013(4) 0.019(5) -0.008(5) C41 0.072(5) 0.063(5) 0.054(4) 0.009(4) 0.003(4) 0.011(4) C42 0.045(4) 0.082(5) 0.038(3) 0.001(4) 0.004(3) 0.004(4) C43 0.041(3) 0.048(4) 0.035(3) -0.008(3) 0.007(3) -0.007(3) C44 0.053(4) 0.075(5) 0.037(3) -0.012(4) -0.008(3) 0.003(4) C45 0.048(4) 0.069(5) 0.055(4) -0.015(4) -0.010(3) 0.006(3) C46 0.040(4) 0.049(4) 0.048(4) -0.015(3) -0.011(3) -0.002(3) C47 0.038(3) 0.045(4) 0.063(5) -0.011(3) -0.014(3) -0.001(3) C48 0.077(6) 0.044(4) 0.082(6) 0.000(4) 0.015(4) 0.000(4) C49 0.079(6) 0.045(4) 0.140(9) 0.028(5) 0.039(6) 0.011(4) C50 0.059(5) 0.038(4) 0.160(10) 0.020(5) -0.027(6) -0.006(3) C51 0.125(9) 0.045(5) 0.119(9) -0.011(6) -0.066(7) -0.007(5) C52 0.113(7) 0.050(5) 0.075(6) -0.023(4) -0.040(5) 0.006(4) C53 0.096(6) 0.053(4) 0.049(4) -0.007(3) 0.024(4) -0.044(4) C54 0.111(8) 0.090(7) 0.056(5) -0.015(5) 0.017(5) -0.063(6) C55 0.073(6) 0.152(10) 0.052(5) -0.020(6) 0.008(5) -0.061(7) C56 0.057(5) 0.111(6) 0.038(4) -0.013(4) 0.008(4) -0.047(5) C57 0.046(4) 0.082(5) 0.036(4) -0.015(4) 0.005(3) -0.019(4) C58 0.033(4) 0.199(12) 0.058(5) 0.024(7) -0.001(4) -0.023(6) C59 0.040(4) 0.182(11) 0.059(5) 0.022(6) 0.002(4) -0.002(6) C60 0.035(4) 0.106(6) 0.036(3) -0.012(4) -0.003(3) 0.001(4) C61 0.057(4) 0.079(5) 0.036(3) -0.001(3) -0.009(3) 0.024(4) C62 0.060(5) 0.085(6) 0.092(7) 0.040(5) 0.016(5) 0.021(4) C63 0.091(7) 0.083(6) 0.088(7) 0.037(5) 0.047(6) 0.036(5) C64 0.082(6) 0.069(5) 0.056(5) -0.005(4) -0.010(4) 0.031(4) C65 0.086(7) 0.053(5) 0.135(9) -0.011(6) -0.049(6) 0.017(5) C66 0.047(5) 0.095(7) 0.115(8) -0.041(6) -0.004(5) 0.019(4) Cl1S 0.133(3) 0.180(3) 0.096(2) -0.030(2) 0.0154(19) -0.091(2) C1S 0.089(6) 0.047(4) 0.091(6) -0.002(4) -0.004(5) -0.020(4) Cl2S 0.0870(17) 0.0925(17) 0.122(2) 0.0062(17) -0.0121(15) 0.0164(14) C2S 0.075(5) 0.052(4) 0.075(5) -0.004(4) -0.010(4) -0.010(4) Cl3S 0.120(2) 0.0896(16) 0.0631(14) -0.0092(11) -0.0215(13) -0.0283(14) Cl4S 0.101(2) 0.0866(18) 0.158(3) 0.0182(19) 0.003(2) 0.0173(16) _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 O3 2.006(4) . ? Pd1 N3 2.021(5) . ? Pd1 N1 2.015(5) . ? Pd1 O1 2.026(4) . ? O1 C1 1.241(7) . ? N1 C11 1.344(9) . ? N1 C15 1.365(9) . ? C1 O2 1.242(7) . ? C1 C2 1.544(9) . ? Pd2 O7 2.006(5) . ? Pd2 N5 2.032(6) . ? Pd2 N7 2.047(5) . ? Pd2 O5 2.052(4) . ? N2 C15 1.343(9) . ? N2 C18 1.356(8) . ? O3 C3 1.279(7) . ? N3 C25 1.331(9) . ? N3 C29 1.375(8) . ? C3 O4 1.234(8) . ? C3 C4 1.507(9) . ? N4 C32 1.323(8) . ? N4 C29 1.347(8) . ? O5 C5 1.172(8) . ? N5 C39 1.335(9) . ? N5 C43 1.375(8) . ? C5 O6 1.287(8) . ? C5 C6 1.491(10) . ? N6 C46 1.334(8) . ? N6 C43 1.340(8) . ? O7 C7 1.277(7) . ? N7 C53 1.306(8) . ? N7 C57 1.380(10) . ? C7 O8 1.245(7) . ? C7 C8 1.503(9) . ? N8 C57 1.344(9) . ? N8 C60 1.357(9) . ? C11 C12 1.430(10) . ? C12 C13 1.321(11) . ? C13 C14 1.398(12) . ? C14 C16 1.385(11) . ? C14 C15 1.421(9) . ? C16 C17 1.343(12) . ? C17 C18 1.408(10) . ? C18 C19 1.483(11) . ? C19 C20 1.394(12) . ? C19 C24 1.416(11) . ? C20 C21 1.362(14) . ? C21 C22 1.329(12) . ? C22 C23 1.385(14) . ? C23 C24 1.414(13) . ? C25 C26 1.389(11) . ? C26 C27 1.360(11) . ? C27 C28 1.413(11) . ? C28 C29 1.409(9) . ? C28 C30 1.404(10) . ? C30 C31 1.343(10) . ? C31 C32 1.405(10) . ? C32 C33 1.492(10) . ? C33 C34 1.390(10) . ? C33 C38 1.406(10) . ? C34 C35 1.355(12) . ? C35 C36 1.368(12) . ? C36 C37 1.348(10) . ? C37 C38 1.366(10) . ? C39 C40 1.407(10) . ? C40 C41 1.346(11) . ? C41 C42 1.416(11) . ? C42 C43 1.417(9) . ? C42 C44 1.438(10) . ? C44 C45 1.344(11) . ? C45 C46 1.407(9) . ? C46 C47 1.446(10) . ? C47 C48 1.366(11) . ? C47 C52 1.395(10) . ? C48 C49 1.416(11) . ? C49 C50 1.361(13) . ? C50 C51 1.408(15) . ? C51 C52 1.355(13) . ? C53 C54 1.379(11) . ? C54 C55 1.345(14) . ? C55 C56 1.413(14) . ? C56 C58 1.407(13) . ? C56 C57 1.418(10) . ? C58 C59 1.349(15) . ? C59 C60 1.419(10) . ? C60 C61 1.502(11) . ? C61 C66 1.372(11) . ? C61 C62 1.388(11) . ? C62 C63 1.363(12) . ? C63 C64 1.383(11) . ? C64 C65 1.333(13) . ? C65 C66 1.415(14) . ? Cl1S C1S 1.711(10) . ? C1S Cl2S 1.772(9) . ? C2S Cl4S 1.760(9) . ? C2S Cl3S 1.766(9) . ? 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 O3 Pd1 N3 90.49(18) . . ? O3 Pd1 N1 175.2(2) . . ? N3 Pd1 N1 91.2(2) . . ? O3 Pd1 O1 88.25(18) . . ? N3 Pd1 O1 172.99(19) . . ? N1 Pd1 O1 90.6(2) . . ? C1 O1 Pd1 118.9(4) . . ? C11 N1 C15 116.9(6) . . ? C11 N1 Pd1 118.6(5) . . ? C15 N1 Pd1 124.4(5) . . ? O2 C1 O1 127.6(6) . . ? O2 C1 C2 118.2(6) . . ? O1 C1 C2 114.2(6) . . ? O7 Pd2 N5 174.30(16) . . ? O7 Pd2 N7 90.4(2) . . ? N5 Pd2 N7 93.2(2) . . ? O7 Pd2 O5 85.83(19) . . ? N5 Pd2 O5 90.7(2) . . ? N7 Pd2 O5 175.7(2) . . ? C15 N2 C18 117.1(6) . . ? C3 O3 Pd1 118.0(4) . . ? C25 N3 C29 118.6(6) . . ? C25 N3 Pd1 118.3(5) . . ? C29 N3 Pd1 123.1(5) . . ? O4 C3 O3 126.4(6) . . ? O4 C3 C4 119.5(6) . . ? O3 C3 C4 114.0(6) . . ? C32 N4 C29 116.9(5) . . ? C5 O5 Pd2 116.3(4) . . ? C39 N5 C43 120.5(6) . . ? C39 N5 Pd2 116.5(5) . . ? C43 N5 Pd2 123.0(4) . . ? O5 C5 O6 125.3(6) . . ? O5 C5 C6 116.6(6) . . ? O6 C5 C6 118.1(6) . . ? C46 N6 C43 119.2(5) . . ? C7 O7 Pd2 118.8(4) . . ? C53 N7 C57 120.3(7) . . ? C53 N7 Pd2 117.4(6) . . ? C57 N7 Pd2 122.3(4) . . ? O8 C7 O7 125.6(6) . . ? O8 C7 C8 119.9(6) . . ? O7 C7 C8 114.6(5) . . ? C57 N8 C60 117.2(6) . . ? N1 C11 C12 123.8(7) . . ? C13 C12 C11 118.2(8) . . ? C12 C13 C14 120.8(7) . . ? C16 C14 C13 125.2(7) . . ? C16 C14 C15 116.2(8) . . ? C13 C14 C15 118.7(7) . . ? N2 C15 N1 114.8(6) . . ? N2 C15 C14 123.7(7) . . ? N1 C15 C14 121.4(7) . . ? C17 C16 C14 121.4(7) . . ? C16 C17 C18 119.1(7) . . ? N2 C18 C17 121.9(8) . . ? N2 C18 C19 115.9(6) . . ? C17 C18 C19 122.1(7) . . ? C20 C19 C24 119.1(9) . . ? C20 C19 C18 119.8(7) . . ? C24 C19 C18 121.0(8) . . ? C21 C20 C19 120.7(8) . . ? C22 C21 C20 121.1(9) . . ? C21 C22 C23 121.5(10) . . ? C22 C23 C24 119.5(9) . . ? C23 C24 C19 118.0(9) . . ? N3 C25 C26 124.7(7) . . ? C27 C26 C25 117.7(7) . . ? C26 C27 C28 120.1(7) . . ? C29 C28 C30 116.2(7) . . ? C29 C28 C27 119.0(7) . . ? C30 C28 C27 124.7(7) . . ? N4 C29 N3 115.8(5) . . ? N4 C29 C28 124.3(6) . . ? N3 C29 C28 119.8(6) . . ? C31 C30 C28 119.7(7) . . ? C30 C31 C32 119.9(7) . . ? N4 C32 C31 122.9(7) . . ? N4 C32 C33 115.7(6) . . ? C31 C32 C33 121.4(6) . . ? C34 C33 C38 115.8(7) . . ? C34 C33 C32 124.2(7) . . ? C38 C33 C32 119.9(6) . . ? C35 C34 C33 122.0(8) . . ? C34 C35 C36 120.9(8) . . ? C37 C36 C35 118.6(8) . . ? C36 C37 C38 121.8(7) . . ? C37 C38 C33 120.6(7) . . ? N5 C39 C40 121.2(8) . . ? C41 C40 C39 121.2(8) . . ? C40 C41 C42 117.7(7) . . ? C43 C42 C41 120.5(7) . . ? C43 C42 C44 115.2(7) . . ? C41 C42 C44 124.2(7) . . ? N6 C43 N5 117.3(6) . . ? N6 C43 C42 124.0(6) . . ? N5 C43 C42 118.7(6) . . ? C45 C44 C42 119.6(7) . . ? C44 C45 C46 121.2(7) . . ? N6 C46 C45 120.8(6) . . ? N6 C46 C47 118.0(6) . . ? C45 C46 C47 121.2(6) . . ? C48 C47 C52 115.9(7) . . ? C48 C47 C46 121.4(6) . . ? C52 C47 C46 122.6(7) . . ? C47 C48 C49 123.7(8) . . ? C50 C49 C48 118.2(10) . . ? C49 C50 C51 119.3(8) . . ? C52 C51 C50 120.4(10) . . ? C51 C52 C47 122.4(10) . . ? N7 C53 C54 123.2(9) . . ? C55 C54 C53 119.0(9) . . ? C54 C55 C56 120.5(9) . . ? C58 C56 C55 124.6(8) . . ? C58 C56 C57 117.7(8) . . ? C55 C56 C57 117.7(9) . . ? N8 C57 N7 117.5(6) . . ? N8 C57 C56 123.3(8) . . ? N7 C57 C56 119.1(7) . . ? C59 C58 C56 119.8(8) . . ? C58 C59 C60 119.2(10) . . ? N8 C60 C59 122.7(9) . . ? N8 C60 C61 116.8(6) . . ? C59 C60 C61 120.5(8) . . ? C66 C61 C62 117.9(8) . . ? C66 C61 C60 121.5(8) . . ? C62 C61 C60 120.6(6) . . ? C63 C62 C61 120.9(8) . . ? C62 C63 C64 121.0(10) . . ? C65 C64 C63 119.0(9) . . ? C64 C65 C66 120.8(8) . . ? C61 C66 C65 120.1(8) . . ? Cl1S C1S Cl2S 109.6(5) . . ? Cl4S C2S Cl3S 110.0(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.287 _refine_diff_density_min -0.956 _refine_diff_density_rms 0.102 _iucr_refine_instructions_details ; TITL _compound_5 CELL 0.71073 15.8053 19.5063 20.1403 90.000 90.000 90.000 ZERR 4.0000 0.0016 0.0019 0.0020 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5-X, 0.5+Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SFAC C H N O CL PD UNIT 264 224 32 32 16 8 MERG 2 FMAP 2 GRID PLAN 2 TEMP -173 SIZE 0.2 0.18 0.36 OMIT 11 4 -13 OMIT 3 2 -26 OMIT 18 11 -2 OMIT 12 10 19 OMIT 0 0 -26 OMIT 17 13 0 OMIT 17 13 -1 OMIT 18 11 0 OMIT 13 20 -2 OMIT 8 24 -1 OMIT 12 9 19 OMIT 13 16 10 OMIT 8 19 -14 OMIT 15 17 -2 OMIT 2 4 -26 OMIT 9 8 21 OMIT 3 23 -5 OMIT 8 4 23 OMIT 20 4 1 OMIT 19 8 1 OMIT 20 1 2 OMIT 4 0 0 OMIT 11 21 -2 L.S. 5 ACTA WGHT 0.07520 0.00000 0.00000 0.00000 0.00000 0.33330 FVAR 0.15698 Pd1 6 0.15895 0.85660 0.35239 11.00000 0.03643 0.04158 = 0.03358 0.00411 0.00395 0.00417 O1 4 0.13564 0.85269 0.25352 11.00000 0.05282 0.03695 = 0.03028 0.00267 0.00389 0.00334 N1 3 0.28300 0.83877 0.33624 11.00000 0.04730 0.06020 = 0.03555 0.01466 0.00365 0.01596 ; #===END _database_code_depnum_ccdc_archive 'CCDC 952839'