# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1682 # Formation, Characterization, and Structural Studies of Novel # Thiosemicarbazone Palladium(II) Complexes. X-Ray Crystal Structures # of [Pd{C6H4C(Et)=NN=C(s)NH2}]4, [Pd{C6H4C(Et)=NN=C(s)NH2}(PMePh2)] # and [{Pd[C6H4C(Et)=NN=C(s)NH2]}2(mu-Ph2PCH2PPh2)] data_1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H49 N12 O Pd4 S4' _chemical_formula_weight 1291.77 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' 'S' 'S' 0.1246 0.1234 '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' 'O' 'O' 0.0106 0.0060 '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 12.0858(2) _cell_length_b 30.0403(3) _cell_length_c 17.6950(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.7089(6) _cell_angle_gamma 90.00 _cell_volume 6084.90(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 50 _exptl_crystal_size_mid 45 _exptl_crystal_size_min 20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2564 _exptl_absorpt_coefficient_mu 1.338 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.6121 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'using SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'siemens CCD SMART' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1' _diffrn_reflns_number 25325 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10690 _reflns_number_gt 8110 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0576P)^2^+47.3515P] 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 10690 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1561 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 0.84101(5) 0.186760(17) 0.71943(3) 0.02014(14) Uani 1 1 d . . . Pd2 Pd 0.66436(5) 0.188615(17) 0.83345(3) 0.01997(14) Uani 1 1 d . . . Pd3 Pd 0.86992(5) 0.287518(18) 0.86257(3) 0.02209(15) Uani 1 1 d . . . Pd4 Pd 0.63909(5) 0.287157(18) 0.68804(3) 0.02348(15) Uani 1 1 d . . . S1 S 0.96941(16) 0.23800(6) 0.80741(11) 0.0251(4) Uani 1 1 d . . . S2 S 0.53607(17) 0.23937(6) 0.74393(11) 0.0266(4) Uani 1 1 d . . . S3 S 0.77917(16) 0.23700(6) 0.92648(11) 0.0232(4) Uani 1 1 d . . . S4 S 0.72636(16) 0.23481(6) 0.62519(11) 0.0246(4) Uani 1 1 d . . . N1 N 0.9352(5) 0.1419(2) 0.7976(4) 0.0255(14) Uani 1 1 d . . . N2 N 1.0152(6) 0.1533(2) 0.8703(4) 0.0301(15) Uani 1 1 d . . . N3 N 1.0962(7) 0.2108(3) 0.9502(4) 0.047(2) Uani 1 1 d . . . H3B H 1.1095 0.2401 0.9591 0.080 Uiso 1 1 d R . . H3A H 1.1288 0.1910 0.9892 0.080 Uiso 1 1 d R . . N4 N 0.5702(5) 0.1433(2) 0.7569(3) 0.0238(13) Uani 1 1 d . . . N5 N 0.4889(6) 0.1543(2) 0.6840(4) 0.0286(14) Uani 1 1 d . . . N6 N 0.4068(6) 0.2109(2) 0.5962(5) 0.048(2) Uani 1 1 d . . . H6A H 0.3941 0.2401 0.5855 0.080 Uiso 1 1 d R . . H6B H 0.3749 0.1906 0.5581 0.080 Uiso 1 1 d R . . N7 N 0.7810(5) 0.33293(19) 0.9032(3) 0.0227(13) Uani 1 1 d . . . N8 N 0.6943(6) 0.3211(2) 0.9373(4) 0.0270(14) Uani 1 1 d . . . N9 N 0.5951(6) 0.2641(2) 0.9670(4) 0.0363(16) Uani 1 1 d . . . H9D H 0.5880 0.2348 0.9749 0.080 Uiso 1 1 d R . . H9E H 0.5438 0.2835 0.9759 0.080 Uiso 1 1 d R . . N10 N 0.7313(5) 0.3302(2) 0.6467(4) 0.0258(14) Uani 1 1 d . . . N11 N 0.8145(6) 0.3185(2) 0.6136(4) 0.0298(15) Uani 1 1 d . . . N12 N 0.9112(6) 0.2587(2) 0.5842(4) 0.0347(16) Uani 1 1 d . . . H12B H 0.9158 0.2292 0.5769 0.080 Uiso 1 1 d R . . H12C H 0.9639 0.2771 0.5746 0.080 Uiso 1 1 d R . . C1 C 0.7700(6) 0.1316(2) 0.6609(4) 0.0243(16) Uani 1 1 d . . . C2 C 0.6853(7) 0.1260(3) 0.5872(5) 0.0293(17) Uani 1 1 d . . . H2A H 0.6462 0.1515 0.5580 0.080 Uiso 1 1 d R . . C3 C 0.6551(7) 0.0832(3) 0.5546(5) 0.0357(19) Uani 1 1 d . . . H3C H 0.5957 0.0801 0.5036 0.080 Uiso 1 1 d R . . C4 C 0.7106(8) 0.0460(3) 0.5940(5) 0.040(2) Uani 1 1 d . . . H4A H 0.6932 0.0175 0.5683 0.080 Uiso 1 1 d R . . C5 C 0.7938(8) 0.0501(3) 0.6690(5) 0.0351(19) Uani 1 1 d . . . H5A H 0.8280 0.0242 0.6991 0.080 Uiso 1 1 d R . . C6 C 0.8249(7) 0.0928(2) 0.7029(4) 0.0263(16) Uani 1 1 d . . . C7 C 0.9152(7) 0.0996(2) 0.7794(5) 0.0278(17) Uani 1 1 d . . . C8 C 0.9826(8) 0.0639(3) 0.8338(5) 0.043(2) Uani 1 1 d . . . H8A H 0.9407 0.0364 0.8195 0.080 Uiso 1 1 d R . . H8B H 0.9895 0.0702 0.8883 0.080 Uiso 1 1 d R . . C9 C 1.1029(10) 0.0570(4) 0.8262(7) 0.062(3) Uani 1 1 d . . . H9A H 1.1422 0.0333 0.8607 0.080 Uiso 1 1 d R . . H9B H 1.0970 0.0499 0.7721 0.080 Uiso 1 1 d R . . H9C H 1.1464 0.0841 0.8417 0.080 Uiso 1 1 d R . . C10 C 1.0275(7) 0.1962(3) 0.8818(5) 0.0294(17) Uani 1 1 d . . . C11 C 0.7339(7) 0.1335(2) 0.8940(4) 0.0254(16) Uani 1 1 d . . . C12 C 0.8213(7) 0.1287(3) 0.9673(5) 0.0300(18) Uani 1 1 d . . . H12A H 0.8602 0.1546 0.9951 0.080 Uiso 1 1 d R . . C13 C 0.8513(8) 0.0863(3) 1.0014(5) 0.042(2) Uani 1 1 d . . . H13A H 0.9143 0.0833 1.0506 0.080 Uiso 1 1 d R . . C14 C 0.7955(9) 0.0491(3) 0.9624(6) 0.050(3) Uani 1 1 d . . . H14A H 0.8145 0.0205 0.9873 0.080 Uiso 1 1 d R . . C15 C 0.7080(8) 0.0524(3) 0.8889(6) 0.042(2) Uani 1 1 d . . . H15A H 0.6709 0.0262 0.8611 0.080 Uiso 1 1 d R . . C16 C 0.6775(7) 0.0947(3) 0.8546(5) 0.0291(17) Uani 1 1 d . . . C17 C 0.5874(7) 0.1016(2) 0.7761(4) 0.0272(16) Uani 1 1 d . . . C18 C 0.5183(8) 0.0649(3) 0.7242(5) 0.038(2) Uani 1 1 d . . . H18A H 0.5606 0.0374 0.7369 0.080 Uiso 1 1 d R . . H18B H 0.5080 0.0720 0.6694 0.080 Uiso 1 1 d R . . C19 C 0.4005(9) 0.0593(3) 0.7358(6) 0.056(3) Uani 1 1 d . . . H19A H 0.3570 0.0360 0.7019 0.080 Uiso 1 1 d R . . H19B H 0.4114 0.0520 0.7905 0.080 Uiso 1 1 d R . . H19C H 0.3584 0.0868 0.7225 0.080 Uiso 1 1 d R . . C20 C 0.4750(7) 0.1970(3) 0.6714(4) 0.0294(17) Uani 1 1 d . . . C21 C 0.9374(7) 0.3431(3) 0.8312(4) 0.0269(17) Uani 1 1 d . . . C22 C 1.0212(7) 0.3480(3) 0.7938(5) 0.0318(18) Uani 1 1 d . . . H22A H 1.0507 0.3221 0.7749 0.080 Uiso 1 1 d R . . C23 C 1.0601(8) 0.3908(3) 0.7811(5) 0.042(2) Uani 1 1 d . . . H23A H 1.1175 0.3940 0.7545 0.080 Uiso 1 1 d R . . C24 C 1.0159(8) 0.4282(3) 0.8053(6) 0.043(2) Uani 1 1 d . . . H24A H 1.0443 0.4573 0.7990 0.080 Uiso 1 1 d R . . C25 C 0.9303(8) 0.4240(3) 0.8427(5) 0.037(2) Uani 1 1 d . . . H25A H 0.8968 0.4500 0.8585 0.080 Uiso 1 1 d R . . C26 C 0.8904(7) 0.3822(3) 0.8560(5) 0.0295(17) Uani 1 1 d . . . C27 C 0.8021(7) 0.3748(2) 0.8946(4) 0.0273(17) Uani 1 1 d . . . C28 C 0.7402(7) 0.4114(3) 0.9229(5) 0.0342(19) Uani 1 1 d . . . H28A H 0.6604 0.4036 0.9156 0.080 Uiso 1 1 d R . . H28B H 0.7410 0.4372 0.8910 0.080 Uiso 1 1 d R . . C29 C 0.8057(9) 0.4237(3) 1.0097(5) 0.044(2) Uani 1 1 d . . . H29A H 0.7677 0.4480 1.0266 0.080 Uiso 1 1 d R . . H29B H 0.8041 0.3978 1.0413 0.080 Uiso 1 1 d R . . H29C H 0.8852 0.4316 1.0165 0.080 Uiso 1 1 d R . . C30 C 0.6818(6) 0.2786(2) 0.9425(5) 0.0278(17) Uani 1 1 d . . . C31 C 0.5773(7) 0.3443(3) 0.7186(5) 0.0327(19) Uani 1 1 d . . . C32 C 0.4917(7) 0.3509(3) 0.7546(5) 0.036(2) Uani 1 1 d . . . H32A H 0.4579 0.3261 0.7735 0.080 Uiso 1 1 d R . . C33 C 0.4557(8) 0.3940(3) 0.7649(6) 0.046(2) Uani 1 1 d . . . H33A H 0.3970 0.3984 0.7900 0.080 Uiso 1 1 d R . . C34 C 0.5022(8) 0.4305(3) 0.7388(5) 0.041(2) Uani 1 1 d . . . H34A H 0.4751 0.4601 0.7440 0.080 Uiso 1 1 d R . . C35 C 0.5879(7) 0.4249(3) 0.7034(5) 0.036(2) Uani 1 1 d . . . H35A H 0.6229 0.4501 0.6866 0.080 Uiso 1 1 d R . . C36 C 0.6245(7) 0.3817(3) 0.6926(4) 0.0273(17) Uani 1 1 d . . . C37 C 0.7143(6) 0.3730(2) 0.6544(4) 0.0261(16) Uani 1 1 d . . . C38 C 0.7771(7) 0.4085(3) 0.6240(5) 0.0337(18) Uani 1 1 d . . . H38A H 0.8545 0.3987 0.6282 0.080 Uiso 1 1 d R . . H38B H 0.7833 0.4349 0.6555 0.080 Uiso 1 1 d R . . C39 C 0.7132(9) 0.4193(3) 0.5370(6) 0.048(2) Uani 1 1 d . . . H39A H 0.7525 0.4421 0.5174 0.080 Uiso 1 1 d R . . H39B H 0.7078 0.3928 0.5057 0.080 Uiso 1 1 d R . . H39C H 0.6361 0.4293 0.5332 0.080 Uiso 1 1 d R . . C40 C 0.8266(7) 0.2750(2) 0.6090(4) 0.0246(16) Uani 1 1 d . . . O1S O 1.3798(6) 0.0003(2) 0.9095(4) 0.0581(19) Uani 1 1 d . . . C1S C 1.3226(9) -0.0321(3) 0.8517(6) 0.054(3) Uani 1 1 d . . . H11A H 1.2596 -0.0182 0.8110 0.080 Uiso 1 1 d R . . H11B H 1.3771 -0.0445 0.8282 0.080 Uiso 1 1 d R . . H11C H 1.2923 -0.0554 0.8767 0.080 Uiso 1 1 d R . . C2S C 1.4704(9) -0.0177(3) 0.9709(6) 0.052(2) Uani 1 1 d . . . H12D H 1.5271 -0.0301 0.9494 0.080 Uiso 1 1 d R . . H12E H 1.4426 -0.0402 0.9989 0.080 Uiso 1 1 d R . . 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 0.0216(3) 0.0183(3) 0.0186(3) -0.0003(2) 0.0039(2) 0.0015(2) Pd2 0.0209(3) 0.0193(3) 0.0177(3) 0.0008(2) 0.0035(2) -0.0010(2) Pd3 0.0231(3) 0.0199(3) 0.0204(3) -0.0006(2) 0.0030(2) -0.0036(2) Pd4 0.0246(3) 0.0200(3) 0.0220(3) 0.0004(2) 0.0022(2) 0.0041(2) S1 0.0251(9) 0.0222(9) 0.0250(9) -0.0003(7) 0.0037(7) -0.0014(7) S2 0.0268(10) 0.0240(9) 0.0253(9) 0.0006(8) 0.0032(8) 0.0013(8) S3 0.0254(9) 0.0193(9) 0.0217(9) -0.0003(7) 0.0032(7) -0.0028(7) S4 0.0268(9) 0.0191(9) 0.0238(9) 0.0009(7) 0.0024(7) 0.0038(7) N1 0.026(3) 0.027(3) 0.021(3) 0.002(3) 0.005(3) 0.001(3) N2 0.027(3) 0.035(4) 0.022(3) -0.001(3) -0.001(3) -0.001(3) N3 0.066(5) 0.043(4) 0.013(3) -0.002(3) -0.013(3) 0.000(4) N4 0.026(3) 0.024(3) 0.019(3) 0.000(2) 0.003(3) -0.001(3) N5 0.031(4) 0.029(4) 0.021(3) 0.000(3) 0.000(3) -0.003(3) N6 0.037(4) 0.032(4) 0.051(5) 0.004(4) -0.021(4) -0.004(3) N7 0.026(3) 0.018(3) 0.025(3) 0.001(2) 0.009(3) -0.001(2) N8 0.033(4) 0.021(3) 0.029(3) 0.001(3) 0.013(3) 0.002(3) N9 0.039(4) 0.028(4) 0.047(4) -0.001(3) 0.021(3) -0.002(3) N10 0.024(3) 0.024(3) 0.023(3) 0.002(3) -0.001(3) 0.006(3) N11 0.033(4) 0.026(3) 0.027(3) 0.002(3) 0.004(3) 0.005(3) N12 0.041(4) 0.026(3) 0.043(4) 0.003(3) 0.022(3) 0.005(3) C1 0.023(4) 0.025(4) 0.027(4) -0.006(3) 0.010(3) -0.002(3) C2 0.028(4) 0.030(4) 0.029(4) -0.001(3) 0.007(3) -0.003(3) C3 0.033(4) 0.036(5) 0.034(4) -0.008(4) 0.005(4) 0.003(4) C4 0.049(5) 0.032(5) 0.037(5) -0.006(4) 0.010(4) -0.007(4) C5 0.040(5) 0.025(4) 0.036(5) 0.001(3) 0.007(4) -0.001(4) C6 0.029(4) 0.022(4) 0.028(4) 0.001(3) 0.010(3) -0.002(3) C7 0.029(4) 0.020(4) 0.032(4) -0.001(3) 0.006(3) -0.003(3) C8 0.054(6) 0.028(5) 0.036(5) 0.003(4) -0.003(4) 0.003(4) C9 0.062(7) 0.055(7) 0.060(7) 0.001(5) 0.007(6) 0.022(5) C10 0.022(4) 0.036(4) 0.025(4) -0.001(3) 0.000(3) -0.006(3) C11 0.030(4) 0.022(4) 0.025(4) 0.000(3) 0.009(3) 0.001(3) C12 0.031(4) 0.027(4) 0.026(4) 0.005(3) 0.000(3) -0.008(3) C13 0.045(5) 0.042(5) 0.030(4) 0.017(4) 0.000(4) 0.007(4) C14 0.057(6) 0.028(5) 0.052(6) 0.014(4) -0.002(5) 0.000(4) C15 0.053(6) 0.026(4) 0.046(5) 0.005(4) 0.014(4) 0.001(4) C16 0.035(4) 0.025(4) 0.026(4) 0.001(3) 0.007(3) 0.004(3) C17 0.030(4) 0.021(4) 0.029(4) -0.004(3) 0.007(3) -0.006(3) C18 0.048(5) 0.023(4) 0.038(5) -0.007(4) 0.005(4) -0.009(4) C19 0.061(7) 0.046(6) 0.058(6) -0.004(5) 0.014(5) -0.029(5) C20 0.031(4) 0.024(4) 0.025(4) 0.001(3) -0.003(3) -0.003(3) C21 0.029(4) 0.028(4) 0.021(4) 0.004(3) 0.003(3) -0.011(3) C22 0.036(5) 0.028(4) 0.034(4) 0.004(3) 0.014(4) -0.002(3) C23 0.044(5) 0.036(5) 0.046(5) 0.008(4) 0.016(4) -0.015(4) C24 0.049(6) 0.033(5) 0.049(5) 0.012(4) 0.015(4) -0.011(4) C25 0.042(5) 0.030(4) 0.034(4) 0.006(4) 0.004(4) -0.005(4) C26 0.026(4) 0.029(4) 0.026(4) 0.002(3) -0.002(3) -0.008(3) C27 0.029(4) 0.024(4) 0.024(4) 0.001(3) 0.002(3) 0.001(3) C28 0.036(5) 0.022(4) 0.041(5) 0.007(4) 0.008(4) 0.003(3) C29 0.063(6) 0.037(5) 0.029(4) -0.006(4) 0.012(4) 0.004(4) C30 0.023(4) 0.021(4) 0.037(4) 0.000(3) 0.006(3) 0.002(3) C31 0.031(4) 0.030(4) 0.023(4) -0.002(3) -0.010(3) 0.005(3) C32 0.028(4) 0.037(5) 0.039(5) -0.004(4) 0.003(4) 0.008(4) C33 0.037(5) 0.049(6) 0.046(5) -0.014(5) 0.005(4) 0.012(4) C34 0.038(5) 0.033(5) 0.045(5) -0.007(4) 0.005(4) 0.013(4) C35 0.039(5) 0.026(4) 0.034(4) -0.001(3) -0.001(4) 0.004(4) C36 0.030(4) 0.027(4) 0.021(4) -0.004(3) 0.002(3) 0.001(3) C37 0.023(4) 0.025(4) 0.023(4) 0.001(3) -0.003(3) 0.003(3) C38 0.032(4) 0.026(4) 0.039(5) -0.003(4) 0.007(4) 0.001(3) C39 0.052(6) 0.040(5) 0.049(6) 0.010(4) 0.011(5) -0.008(4) C40 0.032(4) 0.025(4) 0.013(3) -0.003(3) 0.003(3) -0.004(3) O1S 0.063(5) 0.050(4) 0.057(4) -0.001(4) 0.013(4) 0.005(4) C1S 0.055(6) 0.047(6) 0.056(6) -0.008(5) 0.014(5) -0.001(5) C2S 0.045(6) 0.045(6) 0.065(7) 0.001(5) 0.017(5) -0.004(5) _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 C1 1.997(7) . ? Pd1 N1 2.004(6) . ? Pd1 S4 2.3025(18) . ? Pd1 S1 2.3773(19) . ? Pd2 N4 1.997(6) . ? Pd2 C11 2.005(7) . ? Pd2 S3 2.2983(18) . ? Pd2 S2 2.3795(19) . ? Pd3 N7 2.007(6) . ? Pd3 C21 2.014(7) . ? Pd3 S1 2.316(2) . ? Pd3 S3 2.3624(19) . ? Pd4 N10 1.994(7) . ? Pd4 C31 2.015(8) . ? Pd4 S2 2.319(2) . ? Pd4 S4 2.3611(19) . ? S1 C10 1.790(8) . ? S2 C20 1.790(8) . ? S3 C30 1.800(8) . ? S4 C40 1.797(8) . ? N1 C7 1.313(10) . ? N1 N2 1.382(8) . ? N2 C10 1.306(10) . ? N3 C10 1.304(10) . ? N4 C17 1.298(10) . ? N4 N5 1.388(8) . ? N5 C20 1.303(10) . ? N6 C20 1.385(10) . ? N7 C27 1.303(9) . ? N7 N8 1.412(9) . ? N8 C30 1.292(9) . ? N9 C30 1.330(10) . ? N10 C37 1.314(9) . ? N10 N11 1.361(9) . ? N11 C40 1.322(10) . ? N12 C40 1.328(10) . ? C1 C2 1.385(10) . ? C1 C6 1.427(10) . ? C2 C3 1.409(11) . ? C3 C4 1.371(12) . ? C4 C5 1.390(12) . ? C5 C6 1.413(11) . ? C6 C7 1.455(10) . ? C7 C8 1.496(11) . ? C8 C9 1.517(14) . ? C11 C12 1.392(10) . ? C11 C16 1.415(11) . ? C12 C13 1.405(11) . ? C13 C14 1.372(13) . ? C14 C15 1.392(13) . ? C15 C16 1.405(11) . ? C16 C17 1.480(10) . ? C17 C18 1.505(10) . ? C18 C19 1.511(13) . ? C21 C22 1.385(11) . ? C21 C26 1.431(11) . ? C22 C23 1.411(11) . ? C23 C24 1.371(13) . ? C24 C25 1.402(13) . ? C25 C26 1.391(11) . ? C26 C27 1.457(11) . ? C27 C28 1.502(11) . ? C28 C29 1.530(11) . ? C31 C32 1.392(12) . ? C31 C36 1.401(12) . ? C32 C33 1.394(12) . ? C33 C34 1.379(14) . ? C34 C35 1.383(13) . ? C35 C36 1.403(11) . ? C36 C37 1.474(11) . ? C37 C38 1.506(11) . ? C38 C39 1.519(12) . ? O1S C2S 1.382(12) . ? O1S C1S 1.421(11) . ? C2S C2S 1.493(19) 3_857 ? 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 C1 Pd1 N1 81.6(3) . . ? C1 Pd1 S4 94.9(2) . . ? N1 Pd1 S4 176.53(18) . . ? C1 Pd1 S1 163.5(2) . . ? N1 Pd1 S1 82.92(18) . . ? S4 Pd1 S1 100.55(7) . . ? N4 Pd2 C11 81.4(3) . . ? N4 Pd2 S3 176.31(18) . . ? C11 Pd2 S3 94.9(2) . . ? N4 Pd2 S2 82.94(18) . . ? C11 Pd2 S2 163.1(2) . . ? S3 Pd2 S2 100.74(7) . . ? N7 Pd3 C21 81.1(3) . . ? N7 Pd3 S1 175.95(17) . . ? C21 Pd3 S1 96.1(2) . . ? N7 Pd3 S3 83.17(17) . . ? C21 Pd3 S3 163.0(2) . . ? S1 Pd3 S3 99.94(7) . . ? N10 Pd4 C31 81.0(3) . . ? N10 Pd4 S2 176.35(18) . . ? C31 Pd4 S2 96.7(3) . . ? N10 Pd4 S4 82.66(18) . . ? C31 Pd4 S4 162.6(3) . . ? S2 Pd4 S4 99.82(7) . . ? C10 S1 Pd3 105.9(3) . . ? C10 S1 Pd1 92.7(3) . . ? Pd3 S1 Pd1 111.95(8) . . ? C20 S2 Pd4 106.8(3) . . ? C20 S2 Pd2 93.0(3) . . ? Pd4 S2 Pd2 110.86(8) . . ? C30 S3 Pd2 106.1(3) . . ? C30 S3 Pd3 93.2(3) . . ? Pd2 S3 Pd3 109.25(7) . . ? C40 S4 Pd1 104.9(2) . . ? C40 S4 Pd4 93.1(2) . . ? Pd1 S4 Pd4 109.41(8) . . ? C7 N1 N2 119.2(6) . . ? C7 N1 Pd1 117.5(5) . . ? N2 N1 Pd1 123.2(5) . . ? C10 N2 N1 113.6(6) . . ? C17 N4 N5 118.6(6) . . ? C17 N4 Pd2 118.2(5) . . ? N5 N4 Pd2 123.2(5) . . ? C20 N5 N4 114.1(6) . . ? C27 N7 N8 119.5(6) . . ? C27 N7 Pd3 117.9(5) . . ? N8 N7 Pd3 122.5(4) . . ? C30 N8 N7 113.5(6) . . ? C37 N10 N11 117.4(7) . . ? C37 N10 Pd4 118.0(5) . . ? N11 N10 Pd4 124.5(5) . . ? C40 N11 N10 113.2(6) . . ? C2 C1 C6 118.1(7) . . ? C2 C1 Pd1 130.8(6) . . ? C6 C1 Pd1 110.9(5) . . ? C1 C2 C3 120.8(7) . . ? C4 C3 C2 121.0(8) . . ? C3 C4 C5 119.9(8) . . ? C4 C5 C6 119.9(8) . . ? C5 C6 C1 120.2(7) . . ? C5 C6 C7 122.8(7) . . ? C1 C6 C7 117.0(7) . . ? N1 C7 C6 112.9(7) . . ? N1 C7 C8 121.0(7) . . ? C6 C7 C8 126.0(7) . . ? C7 C8 C9 112.4(8) . . ? N3 C10 N2 118.8(7) . . ? N3 C10 S1 115.5(6) . . ? N2 C10 S1 125.4(6) . . ? C12 C11 C16 118.4(7) . . ? C12 C11 Pd2 130.3(6) . . ? C16 C11 Pd2 111.3(5) . . ? C11 C12 C13 120.5(7) . . ? C14 C13 C12 120.3(8) . . ? C13 C14 C15 121.0(8) . . ? C14 C15 C16 118.9(8) . . ? C15 C16 C11 120.9(7) . . ? C15 C16 C17 123.0(7) . . ? C11 C16 C17 116.2(7) . . ? N4 C17 C16 112.8(6) . . ? N4 C17 C18 122.5(7) . . ? C16 C17 C18 124.6(7) . . ? C17 C18 C19 111.2(7) . . ? N5 C20 N6 117.8(7) . . ? N5 C20 S2 125.1(6) . . ? N6 C20 S2 117.1(6) . . ? C22 C21 C26 118.9(7) . . ? C22 C21 Pd3 129.9(6) . . ? C26 C21 Pd3 111.1(5) . . ? C21 C22 C23 120.3(8) . . ? C24 C23 C22 120.9(8) . . ? C23 C24 C25 119.7(8) . . ? C26 C25 C24 120.5(9) . . ? C25 C26 C21 119.7(8) . . ? C25 C26 C27 124.1(8) . . ? C21 C26 C27 116.2(7) . . ? N7 C27 C26 113.7(7) . . ? N7 C27 C28 122.0(7) . . ? C26 C27 C28 124.3(7) . . ? C27 C28 C29 111.0(7) . . ? N8 C30 N9 118.0(7) . . ? N8 C30 S3 125.3(6) . . ? N9 C30 S3 116.6(6) . . ? C32 C31 C36 118.5(8) . . ? C32 C31 Pd4 129.6(7) . . ? C36 C31 Pd4 111.7(6) . . ? C31 C32 C33 120.0(9) . . ? C34 C33 C32 121.2(9) . . ? C33 C34 C35 119.8(8) . . ? C34 C35 C36 119.4(8) . . ? C31 C36 C35 121.1(8) . . ? C31 C36 C37 116.4(7) . . ? C35 C36 C37 122.5(7) . . ? N10 C37 C36 112.7(7) . . ? N10 C37 C38 122.7(7) . . ? C36 C37 C38 124.6(7) . . ? C37 C38 C39 111.3(7) . . ? N11 C40 N12 119.9(7) . . ? N11 C40 S4 124.1(6) . . ? N12 C40 S4 115.8(6) . . ? C2S O1S C1S 112.1(8) . . ? O1S C2S C2S 110.3(10) . 3_857 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 Pd3 S1 C10 179(100) . . . . ? C21 Pd3 S1 C10 133.4(3) . . . . ? S3 Pd3 S1 C10 -40.8(3) . . . . ? N7 Pd3 S1 Pd1 -81(3) . . . . ? C21 Pd3 S1 Pd1 -126.9(2) . . . . ? S3 Pd3 S1 Pd1 58.84(9) . . . . ? C1 Pd1 S1 C10 -30.7(8) . . . . ? N1 Pd1 S1 C10 -10.5(3) . . . . ? S4 Pd1 S1 C10 169.6(3) . . . . ? C1 Pd1 S1 Pd3 -139.0(8) . . . . ? N1 Pd1 S1 Pd3 -118.85(19) . . . . ? S4 Pd1 S1 Pd3 61.22(9) . . . . ? N10 Pd4 S2 C20 -173(3) . . . . ? C31 Pd4 S2 C20 134.1(3) . . . . ? S4 Pd4 S2 C20 -40.6(3) . . . . ? N10 Pd4 S2 Pd2 -73(3) . . . . ? C31 Pd4 S2 Pd2 -125.9(2) . . . . ? S4 Pd4 S2 Pd2 59.44(9) . . . . ? N4 Pd2 S2 C20 -9.3(3) . . . . ? C11 Pd2 S2 C20 -30.9(8) . . . . ? S3 Pd2 S2 C20 170.9(3) . . . . ? N4 Pd2 S2 Pd4 -118.54(19) . . . . ? C11 Pd2 S2 Pd4 -140.2(7) . . . . ? S3 Pd2 S2 Pd4 61.67(9) . . . . ? N4 Pd2 S3 C30 -136(3) . . . . ? C11 Pd2 S3 C30 -132.6(3) . . . . ? S2 Pd2 S3 C30 41.1(3) . . . . ? N4 Pd2 S3 Pd3 125(3) . . . . ? C11 Pd2 S3 Pd3 128.0(2) . . . . ? S2 Pd2 S3 Pd3 -58.24(9) . . . . ? N7 Pd3 S3 C30 10.9(3) . . . . ? C21 Pd3 S3 C30 33.4(8) . . . . ? S1 Pd3 S3 C30 -166.5(3) . . . . ? N7 Pd3 S3 Pd2 119.12(18) . . . . ? C21 Pd3 S3 Pd2 141.7(7) . . . . ? S1 Pd3 S3 Pd2 -58.26(8) . . . . ? C1 Pd1 S4 C40 -132.6(3) . . . . ? N1 Pd1 S4 C40 -137(3) . . . . ? S1 Pd1 S4 C40 41.7(3) . . . . ? C1 Pd1 S4 Pd4 128.6(2) . . . . ? N1 Pd1 S4 Pd4 124(3) . . . . ? S1 Pd1 S4 Pd4 -57.06(9) . . . . ? N10 Pd4 S4 C40 10.9(3) . . . . ? C31 Pd4 S4 C40 31.7(8) . . . . ? S2 Pd4 S4 C40 -166.4(2) . . . . ? N10 Pd4 S4 Pd1 117.89(18) . . . . ? C31 Pd4 S4 Pd1 138.6(7) . . . . ? S2 Pd4 S4 Pd1 -59.41(9) . . . . ? C1 Pd1 N1 C7 1.1(6) . . . . ? S4 Pd1 N1 C7 6(4) . . . . ? S1 Pd1 N1 C7 -173.2(6) . . . . ? C1 Pd1 N1 N2 -175.8(6) . . . . ? S4 Pd1 N1 N2 -171(3) . . . . ? S1 Pd1 N1 N2 9.9(5) . . . . ? C7 N1 N2 C10 -179.8(7) . . . . ? Pd1 N1 N2 C10 -2.9(9) . . . . ? C11 Pd2 N4 C17 1.9(6) . . . . ? S3 Pd2 N4 C17 5(3) . . . . ? S2 Pd2 N4 C17 -171.9(6) . . . . ? C11 Pd2 N4 N5 -177.1(6) . . . . ? S3 Pd2 N4 N5 -174(3) . . . . ? S2 Pd2 N4 N5 9.1(5) . . . . ? C17 N4 N5 C20 177.7(7) . . . . ? Pd2 N4 N5 C20 -3.3(9) . . . . ? C21 Pd3 N7 C27 -0.8(6) . . . . ? S1 Pd3 N7 C27 -47(3) . . . . ? S3 Pd3 N7 C27 172.7(6) . . . . ? C21 Pd3 N7 N8 176.5(6) . . . . ? S1 Pd3 N7 N8 130(2) . . . . ? S3 Pd3 N7 N8 -10.0(5) . . . . ? C27 N7 N8 C30 179.9(7) . . . . ? Pd3 N7 N8 C30 2.7(8) . . . . ? C31 Pd4 N10 C37 -1.0(5) . . . . ? S2 Pd4 N10 C37 -54(3) . . . . ? S4 Pd4 N10 C37 172.9(5) . . . . ? C31 Pd4 N10 N11 176.4(6) . . . . ? S2 Pd4 N10 N11 123(3) . . . . ? S4 Pd4 N10 N11 -9.8(5) . . . . ? C37 N10 N11 C40 179.3(6) . . . . ? Pd4 N10 N11 C40 1.9(8) . . . . ? N1 Pd1 C1 C2 -177.5(8) . . . . ? S4 Pd1 C1 C2 2.8(7) . . . . ? S1 Pd1 C1 C2 -157.3(6) . . . . ? N1 Pd1 C1 C6 -2.0(5) . . . . ? S4 Pd1 C1 C6 178.3(5) . . . . ? S1 Pd1 C1 C6 18.3(12) . . . . ? C6 C1 C2 C3 -0.5(11) . . . . ? Pd1 C1 C2 C3 174.8(6) . . . . ? C1 C2 C3 C4 -1.6(13) . . . . ? C2 C3 C4 C5 3.4(14) . . . . ? C3 C4 C5 C6 -3.1(14) . . . . ? C4 C5 C6 C1 0.9(12) . . . . ? C4 C5 C6 C7 -176.9(8) . . . . ? C2 C1 C6 C5 0.8(11) . . . . ? Pd1 C1 C6 C5 -175.3(6) . . . . ? C2 C1 C6 C7 178.8(7) . . . . ? Pd1 C1 C6 C7 2.6(8) . . . . ? N2 N1 C7 C6 177.1(6) . . . . ? Pd1 N1 C7 C6 0.0(9) . . . . ? N2 N1 C7 C8 -3.8(11) . . . . ? Pd1 N1 C7 C8 179.2(6) . . . . ? C5 C6 C7 N1 176.1(7) . . . . ? C1 C6 C7 N1 -1.8(10) . . . . ? C5 C6 C7 C8 -3.0(13) . . . . ? C1 C6 C7 C8 179.1(8) . . . . ? N1 C7 C8 C9 -79.1(11) . . . . ? C6 C7 C8 C9 99.9(10) . . . . ? N1 N2 C10 N3 176.4(7) . . . . ? N1 N2 C10 S1 -10.5(10) . . . . ? Pd3 S1 C10 N3 -57.8(7) . . . . ? Pd1 S1 C10 N3 -171.6(7) . . . . ? Pd3 S1 C10 N2 128.9(7) . . . . ? Pd1 S1 C10 N2 15.1(7) . . . . ? N4 Pd2 C11 C12 -180.0(8) . . . . ? S3 Pd2 C11 C12 0.2(8) . . . . ? S2 Pd2 C11 C12 -158.3(6) . . . . ? N4 Pd2 C11 C16 -3.3(5) . . . . ? S3 Pd2 C11 C16 176.9(5) . . . . ? S2 Pd2 C11 C16 18.4(12) . . . . ? C16 C11 C12 C13 -0.8(12) . . . . ? Pd2 C11 C12 C13 175.6(7) . . . . ? C11 C12 C13 C14 0.8(14) . . . . ? C12 C13 C14 C15 -0.4(16) . . . . ? C13 C14 C15 C16 0.2(16) . . . . ? C14 C15 C16 C11 -0.3(14) . . . . ? C14 C15 C16 C17 178.7(9) . . . . ? C12 C11 C16 C15 0.6(12) . . . . ? Pd2 C11 C16 C15 -176.5(7) . . . . ? C12 C11 C16 C17 -178.5(7) . . . . ? Pd2 C11 C16 C17 4.4(9) . . . . ? N5 N4 C17 C16 179.1(6) . . . . ? Pd2 N4 C17 C16 0.0(9) . . . . ? N5 N4 C17 C18 -3.2(11) . . . . ? Pd2 N4 C17 C18 177.8(6) . . . . ? C15 C16 C17 N4 177.9(8) . . . . ? C11 C16 C17 N4 -3.0(10) . . . . ? C15 C16 C17 C18 0.2(13) . . . . ? C11 C16 C17 C18 179.3(8) . . . . ? N4 C17 C18 C19 -80.5(10) . . . . ? C16 C17 C18 C19 96.9(10) . . . . ? N4 N5 C20 N6 172.0(7) . . . . ? N4 N5 C20 S2 -8.6(10) . . . . ? Pd4 S2 C20 N5 125.8(7) . . . . ? Pd2 S2 C20 N5 13.0(8) . . . . ? Pd4 S2 C20 N6 -54.7(7) . . . . ? Pd2 S2 C20 N6 -167.6(7) . . . . ? N7 Pd3 C21 C22 179.2(8) . . . . ? S1 Pd3 C21 C22 -3.7(7) . . . . ? S3 Pd3 C21 C22 156.6(6) . . . . ? N7 Pd3 C21 C26 1.8(5) . . . . ? S1 Pd3 C21 C26 178.8(5) . . . . ? S3 Pd3 C21 C26 -20.9(11) . . . . ? C26 C21 C22 C23 0.6(12) . . . . ? Pd3 C21 C22 C23 -176.7(6) . . . . ? C21 C22 C23 C24 0.0(13) . . . . ? C22 C23 C24 C25 -0.5(14) . . . . ? C23 C24 C25 C26 0.5(13) . . . . ? C24 C25 C26 C21 0.1(12) . . . . ? C24 C25 C26 C27 179.8(7) . . . . ? C22 C21 C26 C25 -0.6(11) . . . . ? Pd3 C21 C26 C25 177.2(6) . . . . ? C22 C21 C26 C27 179.7(7) . . . . ? Pd3 C21 C26 C27 -2.5(8) . . . . ? N8 N7 C27 C26 -177.8(6) . . . . ? Pd3 N7 C27 C26 -0.4(8) . . . . ? N8 N7 C27 C28 2.6(11) . . . . ? Pd3 N7 C27 C28 180.0(5) . . . . ? C25 C26 C27 N7 -177.7(7) . . . . ? C21 C26 C27 N7 2.0(10) . . . . ? C25 C26 C27 C28 1.8(12) . . . . ? C21 C26 C27 C28 -178.4(7) . . . . ? N7 C27 C28 C29 88.7(9) . . . . ? C26 C27 C28 C29 -90.9(9) . . . . ? N7 N8 C30 N9 -174.0(6) . . . . ? N7 N8 C30 S3 11.0(10) . . . . ? Pd2 S3 C30 N8 -126.9(7) . . . . ? Pd3 S3 C30 N8 -15.8(7) . . . . ? Pd2 S3 C30 N9 58.0(6) . . . . ? Pd3 S3 C30 N9 169.1(6) . . . . ? N10 Pd4 C31 C32 177.4(7) . . . . ? S2 Pd4 C31 C32 -5.5(7) . . . . ? S4 Pd4 C31 C32 156.6(6) . . . . ? N10 Pd4 C31 C36 2.9(5) . . . . ? S2 Pd4 C31 C36 179.9(5) . . . . ? S4 Pd4 C31 C36 -18.0(11) . . . . ? C36 C31 C32 C33 -0.8(11) . . . . ? Pd4 C31 C32 C33 -175.0(6) . . . . ? C31 C32 C33 C34 1.1(13) . . . . ? C32 C33 C34 C35 -1.5(13) . . . . ? C33 C34 C35 C36 1.5(13) . . . . ? C32 C31 C36 C35 0.9(11) . . . . ? Pd4 C31 C36 C35 176.1(6) . . . . ? C32 C31 C36 C37 -179.6(6) . . . . ? Pd4 C31 C36 C37 -4.3(8) . . . . ? C34 C35 C36 C31 -1.3(12) . . . . ? C34 C35 C36 C37 179.2(7) . . . . ? N11 N10 C37 C36 -178.6(6) . . . . ? Pd4 N10 C37 C36 -1.1(8) . . . . ? N11 N10 C37 C38 3.8(10) . . . . ? Pd4 N10 C37 C38 -178.7(5) . . . . ? C31 C36 C37 N10 3.7(9) . . . . ? C35 C36 C37 N10 -176.8(7) . . . . ? C31 C36 C37 C38 -178.8(7) . . . . ? C35 C36 C37 C38 0.7(11) . . . . ? N10 C37 C38 C39 86.6(9) . . . . ? C36 C37 C38 C39 -90.7(9) . . . . ? N10 N11 C40 N12 -174.3(6) . . . . ? N10 N11 C40 S4 11.9(9) . . . . ? Pd1 S4 C40 N11 -127.3(6) . . . . ? Pd4 S4 C40 N11 -16.3(6) . . . . ? Pd1 S4 C40 N12 58.7(6) . . . . ? Pd4 S4 C40 N12 169.8(5) . . . . ? C1S O1S C2S C2S 178.7(10) . . . 3_857 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.893 _refine_diff_density_min -2.137 _refine_diff_density_rms 0.214 #===END data_3b _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H26 Cl2 N3 P Pd S' _chemical_formula_weight 596.81 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 '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' '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 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 15.366(3) _cell_length_b 9.174(2) _cell_length_c 18.525(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.20(2) _cell_angle_gamma 90.00 _cell_volume 2531.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 9.366 _cell_measurement_theta_max 24.949 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method ? _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 9.92 _diffrn_reflns_number 5653 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4448 _reflns_number_observed 3794 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+2.7320P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4446 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_obs 0.0500 _refine_ls_wR_factor_all 0.1468 _refine_ls_wR_factor_obs 0.1393 _refine_ls_goodness_of_fit_all 1.150 _refine_ls_goodness_of_fit_obs 1.189 _refine_ls_restrained_S_all 1.153 _refine_ls_restrained_S_obs 1.189 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.45546(2) 0.22976(4) 0.22918(2) 0.0341(2) Uani 1 d . . S1 S 0.35237(9) 0.2018(2) 0.11484(7) 0.0485(3) Uani 1 d . . P1 P 0.36912(9) 0.36493(14) 0.28568(7) 0.0390(3) Uani 1 d . . N1 N 0.5356(3) 0.1104(4) 0.1795(2) 0.0379(9) Uani 1 d . . N2 N 0.5081(3) 0.0604(5) 0.1064(2) 0.0432(10) Uani 1 d . . N3 N 0.3896(3) 0.0549(6) 0.0041(2) 0.0606(13) Uani 1 d . . H3A H 0.3326(3) 0.0771(6) -0.0192(2) 0.080 Uiso 1 d R . H3B H 0.4234(3) 0.0017(6) -0.0195(2) 0.080 Uiso 1 d R . C1 C 0.5672(3) 0.2239(5) 0.3148(3) 0.0370(10) Uani 1 d . . C2 C 0.5860(4) 0.2829(6) 0.3865(3) 0.0446(12) Uani 1 d . . H2B H 0.5413(4) 0.3414(6) 0.4009(3) 0.080 Uiso 1 d R . C3 C 0.6686(4) 0.2603(6) 0.4369(3) 0.0474(13) Uani 1 d . . H3C H 0.6791(4) 0.2994(6) 0.4864(3) 0.080 Uiso 1 d R . C4 C 0.7346(4) 0.1780(7) 0.4161(3) 0.0513(13) Uani 1 d . . H4A H 0.7917(4) 0.1631(7) 0.4506(3) 0.080 Uiso 1 d R . C5 C 0.7183(4) 0.1213(6) 0.3452(3) 0.0504(13) Uani 1 d . . H5A H 0.7641(4) 0.0655(6) 0.3307(3) 0.080 Uiso 1 d R . C6 C 0.6365(3) 0.1418(5) 0.2950(3) 0.0390(10) Uani 1 d . . C7 C 0.6162(3) 0.0801(5) 0.2190(3) 0.0405(11) Uani 1 d . . C8 C 0.4247(3) 0.0992(6) 0.0752(3) 0.0439(11) Uani 1 d . . C9 C 0.3412(4) 0.2819(6) 0.3658(3) 0.0445(12) Uani 1 d . . C10 C 0.2779(5) 0.3437(8) 0.3989(4) 0.081(2) Uani 1 d . . H10A H 0.2473(5) 0.4317(8) 0.3793(4) 0.080 Uiso 1 d R . C11 C 0.2535(7) 0.2740(11) 0.4566(6) 0.105(3) Uani 1 d . . H11A H 0.2141(7) 0.3203(11) 0.4826(6) 0.080 Uiso 1 d R . C12 C 0.2916(6) 0.1440(9) 0.4830(4) 0.088(2) Uani 1 d . . H12A H 0.2709(6) 0.0957(9) 0.5217(4) 0.080 Uiso 1 d R . C13 C 0.3543(4) 0.0805(7) 0.4520(3) 0.064(2) Uani 1 d . . H13A H 0.3815(4) -0.0102(7) 0.4713(3) 0.080 Uiso 1 d R . C14 C 0.3793(4) 0.1500(6) 0.3933(3) 0.0487(12) Uani 1 d . . H14A H 0.4219(4) 0.1059(6) 0.3699(3) 0.080 Uiso 1 d R . C15 C 0.4189(4) 0.5422(6) 0.3142(3) 0.0502(13) Uani 1 d . . C16 C 0.4435(6) 0.6272(8) 0.2608(5) 0.082(2) Uani 1 d . . H16A H 0.4331(6) 0.5929(8) 0.2104(5) 0.080 Uiso 1 d R . C17 C 0.4852(7) 0.7627(9) 0.2805(8) 0.106(4) Uani 1 d . . H17A H 0.4985(7) 0.8263(9) 0.2435(8) 0.080 Uiso 1 d R . C18 C 0.5024(6) 0.8094(9) 0.3514(8) 0.105(3) Uani 1 d . . H18A H 0.5347(6) 0.8988(9) 0.3653(8) 0.080 Uiso 1 d R . C19 C 0.4801(6) 0.7277(8) 0.4045(6) 0.093(3) Uani 1 d . . H19A H 0.4925(6) 0.7658(8) 0.4542(6) 0.080 Uiso 1 d R . C20 C 0.4371(5) 0.5950(7) 0.3863(4) 0.068(2) Uani 1 d . . H20A H 0.4202(5) 0.5389(7) 0.4244(4) 0.080 Uiso 1 d R . C21 C 0.2600(4) 0.4118(8) 0.2255(3) 0.064(2) Uani 1 d . . H21A H 0.2267(4) 0.4693(8) 0.2527(3) 0.080 Uiso 1 d R . H21B H 0.2681(4) 0.4662(8) 0.1834(3) 0.080 Uiso 1 d R . H21C H 0.2276(4) 0.3237(8) 0.2086(3) 0.080 Uiso 1 d R . C22 C 0.6836(4) -0.0051(7) 0.1898(3) 0.058(2) Uani 1 d . . H22A H 0.6537(4) -0.0700(7) 0.1509(3) 0.080 Uiso 1 d R . H22B H 0.7186(4) -0.0624(7) 0.2299(3) 0.080 Uiso 1 d R . C23 C 0.7458(5) 0.0905(10) 0.1616(4) 0.090(3) Uani 1 d . . H23A H 0.7896(5) 0.0352(10) 0.1441(4) 0.080 Uiso 1 d R . H23B H 0.7105(5) 0.1469(10) 0.1213(4) 0.080 Uiso 1 d R . H23C H 0.7757(5) 0.1546(10) 0.2008(4) 0.080 Uiso 1 d R . Cl1 Cl 0.4980(7) 0.6494(15) 0.0636(8) 0.406(7) Uani 1 d D . Cl2 Cl 0.5698(4) 0.4175(9) 0.0621(7) 0.331(6) Uani 1 d D . C1S C 0.4720(12) 0.4885(22) 0.0278(12) 0.401(29) Uani 1 d D . H1SA H 0.4507(12) 0.4801(22) -0.0253(12) 0.080 Uiso 1 d R . H1SB H 0.4282(12) 0.4493(22) 0.0516(12) 0.080 Uiso 1 d R . 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 0.0404(2) 0.0351(2) 0.0265(2) -0.00211(13) 0.0077(2) 0.00120(14) S1 0.0451(7) 0.0648(9) 0.0326(6) -0.0083(6) 0.0040(5) 0.0077(6) P1 0.0463(7) 0.0364(7) 0.0352(6) -0.0009(5) 0.0116(5) 0.0046(5) N1 0.046(2) 0.038(2) 0.029(2) -0.003(2) 0.008(2) -0.002(2) N2 0.054(2) 0.044(2) 0.030(2) -0.009(2) 0.007(2) 0.004(2) N3 0.059(3) 0.086(4) 0.035(2) -0.017(2) 0.008(2) 0.008(3) C1 0.044(3) 0.038(3) 0.028(2) 0.001(2) 0.007(2) -0.002(2) C2 0.049(3) 0.050(3) 0.034(3) -0.007(2) 0.009(2) -0.002(2) C3 0.056(3) 0.054(3) 0.029(2) -0.002(2) 0.005(2) -0.003(2) C4 0.049(3) 0.056(3) 0.043(3) 0.000(3) -0.002(2) 0.003(3) C5 0.052(3) 0.051(3) 0.045(3) -0.002(2) 0.007(2) 0.006(2) C6 0.044(3) 0.037(3) 0.034(2) 0.000(2) 0.007(2) 0.002(2) C7 0.048(3) 0.038(3) 0.033(2) -0.002(2) 0.007(2) 0.003(2) C8 0.050(3) 0.049(3) 0.032(2) -0.003(2) 0.010(2) 0.003(2) C9 0.054(3) 0.041(3) 0.041(3) -0.002(2) 0.018(2) 0.002(2) C10 0.113(6) 0.061(4) 0.090(5) 0.015(4) 0.064(5) 0.029(4) C11 0.137(8) 0.106(7) 0.104(7) 0.020(5) 0.091(6) 0.022(6) C12 0.127(7) 0.081(5) 0.075(5) 0.019(4) 0.056(5) -0.005(5) C13 0.081(4) 0.058(4) 0.054(3) 0.012(3) 0.021(3) -0.004(3) C14 0.056(3) 0.040(3) 0.048(3) -0.001(2) 0.011(2) -0.006(2) C15 0.057(3) 0.035(3) 0.061(3) -0.002(2) 0.019(3) 0.007(2) C16 0.123(6) 0.051(4) 0.087(5) 0.002(4) 0.056(5) -0.008(4) C17 0.128(8) 0.058(5) 0.157(11) 0.022(6) 0.083(8) -0.007(5) C18 0.096(6) 0.045(4) 0.184(11) -0.032(6) 0.055(7) -0.008(4) C19 0.110(7) 0.054(4) 0.115(7) -0.033(5) 0.029(6) -0.019(4) C20 0.088(4) 0.044(3) 0.074(4) -0.017(3) 0.023(3) -0.005(3) C21 0.056(3) 0.078(4) 0.056(3) 0.001(3) 0.007(3) 0.020(3) C22 0.060(3) 0.068(4) 0.043(3) -0.021(3) 0.005(2) 0.017(3) C23 0.073(4) 0.116(7) 0.091(5) -0.037(5) 0.039(4) 0.003(4) Cl1 0.317(11) 0.467(18) 0.509(18) -0.045(16) 0.243(13) -0.125(13) Cl2 0.176(5) 0.221(7) 0.563(16) 0.177(9) 0.025(7) -0.056(5) C1S 0.360(35) 0.679(65) 0.144(16) 0.028(25) 0.027(18) -0.401(45) _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 N1 2.029(4) . ? Pd1 C1 2.033(5) . ? Pd1 P1 2.2527(13) . ? Pd1 S1 2.3270(14) . ? S1 C8 1.750(5) . ? P1 C9 1.811(5) . ? P1 C15 1.820(6) . ? P1 C21 1.823(5) . ? N1 C7 1.304(6) . ? N1 N2 1.394(5) . ? N2 C8 1.319(6) . ? N3 C8 1.356(6) . ? C1 C2 1.397(7) . ? C1 C6 1.424(7) . ? C2 C3 1.395(8) . ? C3 C4 1.394(8) . ? C4 C5 1.377(7) . ? C5 C6 1.381(7) . ? C6 C7 1.477(6) . ? C7 C22 1.501(7) . ? C9 C14 1.386(8) . ? C9 C10 1.392(8) . ? C10 C11 1.374(10) . ? C11 C12 1.365(12) . ? C12 C13 1.367(10) . ? C13 C14 1.393(8) . ? C15 C20 1.383(8) . ? C15 C16 1.384(9) . ? C16 C17 1.404(12) . ? C17 C18 1.35(2) . ? C18 C19 1.346(14) . ? C19 C20 1.386(10) . ? C22 C23 1.483(10) . ? Cl1 C1S 1.63(2) . ? Cl1 C1S 2.25(3) 3_665 ? Cl1 Cl2 2.387(14) 3_665 ? Cl1 Cl2 2.40(2) . ? Cl2 C1S 1.62(2) . ? Cl2 C1S 1.85(2) 3_665 ? Cl2 Cl1 2.387(14) 3_665 ? C1S C1S 1.51(4) 3_665 ? C1S Cl2 1.85(2) 3_665 ? C1S Cl1 2.25(3) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 C1 81.3(2) . . ? N1 Pd1 P1 178.75(11) . . ? C1 Pd1 P1 97.65(14) . . ? N1 Pd1 S1 83.19(11) . . ? C1 Pd1 S1 164.49(15) . . ? P1 Pd1 S1 97.85(5) . . ? C8 S1 Pd1 94.6(2) . . ? C9 P1 C15 107.8(2) . . ? C9 P1 C21 103.5(3) . . ? C15 P1 C21 103.0(3) . . ? C9 P1 Pd1 115.7(2) . . ? C15 P1 Pd1 111.9(2) . . ? C21 P1 Pd1 113.8(2) . . ? C7 N1 N2 119.7(4) . . ? C7 N1 Pd1 117.3(3) . . ? N2 N1 Pd1 123.0(3) . . ? C8 N2 N1 111.6(4) . . ? C2 C1 C6 117.2(5) . . ? C2 C1 Pd1 132.0(4) . . ? C6 C1 Pd1 110.8(3) . . ? C3 C2 C1 121.5(5) . . ? C4 C3 C2 119.9(5) . . ? C5 C4 C3 119.7(5) . . ? C4 C5 C6 120.9(5) . . ? C5 C6 C1 120.9(4) . . ? C5 C6 C7 122.3(4) . . ? C1 C6 C7 116.9(4) . . ? N1 C7 C6 113.7(4) . . ? N1 C7 C22 123.6(4) . . ? C6 C7 C22 122.7(4) . . ? N2 C8 N3 117.2(4) . . ? N2 C8 S1 127.6(4) . . ? N3 C8 S1 115.3(4) . . ? C14 C9 C10 118.1(5) . . ? C14 C9 P1 120.3(4) . . ? C10 C9 P1 121.5(4) . . ? C11 C10 C9 120.5(7) . . ? C12 C11 C10 120.7(7) . . ? C11 C12 C13 120.4(6) . . ? C12 C13 C14 119.4(6) . . ? C9 C14 C13 121.0(6) . . ? C20 C15 C16 117.8(6) . . ? C20 C15 P1 124.4(5) . . ? C16 C15 P1 117.7(5) . . ? C15 C16 C17 120.0(8) . . ? C18 C17 C16 120.3(9) . . ? C19 C18 C17 120.8(8) . . ? C18 C19 C20 120.2(9) . . ? C15 C20 C19 120.9(8) . . ? C23 C22 C7 112.4(5) . . ? C1S Cl1 C1S 42.1(11) . 3_665 ? C1S Cl1 Cl2 50.5(9) . 3_665 ? C1S Cl1 Cl2 40.7(5) 3_665 3_665 ? C1S Cl1 Cl2 42.2(7) . . ? C1S Cl1 Cl2 46.6(7) 3_665 . ? Cl2 Cl1 Cl2 81.5(5) 3_665 . ? C1S Cl2 C1S 51.2(12) . 3_665 ? C1S Cl2 Cl1 65.1(9) . 3_665 ? C1S Cl2 Cl1 42.9(6) 3_665 3_665 ? C1S Cl2 Cl1 42.5(7) . . ? C1S Cl2 Cl1 62.4(8) 3_665 . ? Cl1 Cl2 Cl1 98.5(5) 3_665 . ? C1S C1S Cl2 72.2(14) 3_665 . ? C1S C1S Cl1 91.6(16) 3_665 . ? Cl2 C1S Cl1 95.4(11) . . ? C1S C1S Cl2 56.6(13) 3_665 3_665 ? Cl2 C1S Cl2 128.8(12) . 3_665 ? Cl1 C1S Cl2 86.6(11) . 3_665 ? C1S C1S Cl1 46.3(12) 3_665 3_665 ? Cl2 C1S Cl1 74.2(9) . 3_665 ? Cl1 C1S Cl1 137.9(11) . 3_665 ? Cl2 C1S Cl1 70.9(8) 3_665 3_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 S1 C8 0.0(2) . . . . ? C1 Pd1 S1 C8 2.4(6) . . . . ? P1 Pd1 S1 C8 179.3(2) . . . . ? N1 Pd1 P1 C9 -97.5(50) . . . . ? C1 Pd1 P1 C9 -64.5(2) . . . . ? S1 Pd1 P1 C9 116.3(2) . . . . ? N1 Pd1 P1 C15 26.5(50) . . . . ? C1 Pd1 P1 C15 59.5(2) . . . . ? S1 Pd1 P1 C15 -119.7(2) . . . . ? N1 Pd1 P1 C21 142.8(50) . . . . ? C1 Pd1 P1 C21 175.8(3) . . . . ? S1 Pd1 P1 C21 -3.4(3) . . . . ? C1 Pd1 N1 C7 1.1(4) . . . . ? P1 Pd1 N1 C7 34.2(52) . . . . ? S1 Pd1 N1 C7 -179.5(4) . . . . ? C1 Pd1 N1 N2 -179.1(4) . . . . ? P1 Pd1 N1 N2 -146.0(48) . . . . ? S1 Pd1 N1 N2 0.3(3) . . . . ? C7 N1 N2 C8 179.2(5) . . . . ? Pd1 N1 N2 C8 -0.6(6) . . . . ? N1 Pd1 C1 C2 179.7(5) . . . . ? P1 Pd1 C1 C2 0.4(5) . . . . ? S1 Pd1 C1 C2 177.4(4) . . . . ? N1 Pd1 C1 C6 -0.9(3) . . . . ? P1 Pd1 C1 C6 179.8(3) . . . . ? S1 Pd1 C1 C6 -3.2(8) . . . . ? C6 C1 C2 C3 -1.2(8) . . . . ? Pd1 C1 C2 C3 178.2(4) . . . . ? C1 C2 C3 C4 0.4(8) . . . . ? C2 C3 C4 C5 1.0(9) . . . . ? C3 C4 C5 C6 -1.6(9) . . . . ? C4 C5 C6 C1 0.8(8) . . . . ? C4 C5 C6 C7 -178.8(5) . . . . ? C2 C1 C6 C5 0.5(7) . . . . ? Pd1 C1 C6 C5 -179.0(4) . . . . ? C2 C1 C6 C7 -179.8(4) . . . . ? Pd1 C1 C6 C7 0.7(5) . . . . ? N2 N1 C7 C6 179.2(4) . . . . ? Pd1 N1 C7 C6 -1.0(6) . . . . ? N2 N1 C7 C22 1.2(8) . . . . ? Pd1 N1 C7 C22 -179.0(4) . . . . ? C5 C6 C7 N1 179.8(5) . . . . ? C1 C6 C7 N1 0.2(7) . . . . ? C5 C6 C7 C22 -2.1(8) . . . . ? C1 C6 C7 C22 178.2(5) . . . . ? N1 N2 C8 N3 -179.0(5) . . . . ? N1 N2 C8 S1 0.7(7) . . . . ? Pd1 S1 C8 N2 -0.4(5) . . . . ? Pd1 S1 C8 N3 179.3(4) . . . . ? C15 P1 C9 C14 -120.0(5) . . . . ? C21 P1 C9 C14 131.4(5) . . . . ? Pd1 P1 C9 C14 6.1(5) . . . . ? C15 P1 C9 C10 63.6(6) . . . . ? C21 P1 C9 C10 -45.0(6) . . . . ? Pd1 P1 C9 C10 -170.3(5) . . . . ? C14 C9 C10 C11 -0.7(12) . . . . ? P1 C9 C10 C11 175.8(8) . . . . ? C9 C10 C11 C12 0.7(16) . . . . ? C10 C11 C12 C13 -0.5(16) . . . . ? C11 C12 C13 C14 0.3(13) . . . . ? C10 C9 C14 C13 0.5(9) . . . . ? P1 C9 C14 C13 -176.0(5) . . . . ? C12 C13 C14 C9 -0.3(10) . . . . ? C9 P1 C15 C20 4.3(6) . . . . ? C21 P1 C15 C20 113.3(6) . . . . ? Pd1 P1 C15 C20 -124.0(5) . . . . ? C9 P1 C15 C16 -178.4(5) . . . . ? C21 P1 C15 C16 -69.4(6) . . . . ? Pd1 P1 C15 C16 53.3(6) . . . . ? C20 C15 C16 C17 -0.3(11) . . . . ? P1 C15 C16 C17 -177.7(7) . . . . ? C15 C16 C17 C18 0.9(15) . . . . ? C16 C17 C18 C19 0.0(16) . . . . ? C17 C18 C19 C20 -1.4(15) . . . . ? C16 C15 C20 C19 -1.1(10) . . . . ? P1 C15 C20 C19 176.1(6) . . . . ? C18 C19 C20 C15 2.0(13) . . . . ? N1 C7 C22 C23 95.3(7) . . . . ? C6 C7 C22 C23 -82.5(7) . . . . ? C1S Cl1 Cl2 C1S 0.000(2) . . . . ? C1S Cl1 Cl2 C1S -61.5(15) 3_665 . . . ? Cl2 Cl1 Cl2 C1S -37.5(11) 3_665 . . . ? C1S Cl1 Cl2 C1S 61.5(15) . . . 3_665 ? C1S Cl1 Cl2 C1S 0.000(1) 3_665 . . 3_665 ? Cl2 Cl1 Cl2 C1S 24.0(6) 3_665 . . 3_665 ? C1S Cl1 Cl2 Cl1 37.5(11) . . . 3_665 ? C1S Cl1 Cl2 Cl1 -24.0(6) 3_665 . . 3_665 ? Cl2 Cl1 Cl2 Cl1 0.000(2) 3_665 . . 3_665 ? C1S Cl2 C1S C1S 0.0 3_665 . . 3_665 ? Cl1 Cl2 C1S C1S -48.4(11) 3_665 . . 3_665 ? Cl1 Cl2 C1S C1S 90.0(15) . . . 3_665 ? C1S Cl2 C1S Cl1 -90.0(15) 3_665 . . . ? Cl1 Cl2 C1S Cl1 -138.4(11) 3_665 . . . ? Cl1 Cl2 C1S Cl1 0.000(2) . . . . ? C1S Cl2 C1S Cl2 0.000(3) 3_665 . . 3_665 ? Cl1 Cl2 C1S Cl2 -48.4(11) 3_665 . . 3_665 ? Cl1 Cl2 C1S Cl2 90.0(15) . . . 3_665 ? C1S Cl2 C1S Cl1 48.4(11) 3_665 . . 3_665 ? Cl1 Cl2 C1S Cl1 0.0 3_665 . . 3_665 ? Cl1 Cl2 C1S Cl1 138.4(11) . . . 3_665 ? C1S Cl1 C1S C1S 0.0 3_665 . . 3_665 ? Cl2 Cl1 C1S C1S 56.4(14) 3_665 . . 3_665 ? Cl2 Cl1 C1S C1S -72.3(15) . . . 3_665 ? C1S Cl1 C1S Cl2 72.3(15) 3_665 . . . ? Cl2 Cl1 C1S Cl2 128.7(12) 3_665 . . . ? Cl2 Cl1 C1S Cl2 0.000(1) . . . . ? C1S Cl1 C1S Cl2 -56.4(14) 3_665 . . 3_665 ? Cl2 Cl1 C1S Cl2 0.000(2) 3_665 . . 3_665 ? Cl2 Cl1 C1S Cl2 -128.7(12) . . . 3_665 ? C1S Cl1 C1S Cl1 0.000(4) 3_665 . . 3_665 ? Cl2 Cl1 C1S Cl1 56.4(14) 3_665 . . 3_665 ? Cl2 Cl1 C1S Cl1 -72.3(15) . . . 3_665 ? _refine_diff_density_max 1.273 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.135 #===END data_7b' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H56 N6 O2 P2 Pd2 S2' _chemical_formula_weight 1123.88 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' 'P' 'P' 0.1023 0.0942 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8547(2) _cell_length_b 17.8565(2) _cell_length_c 21.11840(10) _cell_angle_alpha 93.9370(10) _cell_angle_beta 90.9930(10) _cell_angle_gamma 92.30 _cell_volume 5207.02(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 0.876 _exptl_absorpt_correction_type 'empirical using SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7589 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 '\w scans' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1' _diffrn_reflns_number 27248 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.1136 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17986 _reflns_number_gt 10201 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+3.2609P] 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 17986 _refine_ls_number_parameters 1171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1334 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1424 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6611(6) 0.2537(4) -0.8427(4) 0.058(2) Uani 1 d . . . C2 C 0.6408(7) 0.2312(5) -0.9049(4) 0.075(3) Uani 1 d . . . H2A H 0.5752 0.2167 -0.9168 0.080 Uiso 1 d R . . C3 C 0.7136(8) 0.2295(5) -0.9516(5) 0.090(3) Uani 1 d . . . H3A H 0.6978 0.2123 -0.9947 0.080 Uiso 1 d R . . C4 C 0.8066(8) 0.2516(6) -0.9338(5) 0.088(3) Uani 1 d . . . H4A H 0.8563 0.2511 -0.9650 0.080 Uiso 1 d R . . C5 C 0.8289(7) 0.2749(5) -0.8717(5) 0.082(3) Uani 1 d . . . H5A H 0.8941 0.2906 -0.8598 0.080 Uiso 1 d R . . C6 C 0.7580(6) 0.2763(5) -0.8252(4) 0.069(3) Uani 1 d . . . C7 C 0.7786(6) 0.3041(5) -0.7597(4) 0.068(3) Uani 1 d . . . C8 C 0.6320(6) 0.3299(4) -0.6313(4) 0.057(2) Uani 1 d . . . C9 C 0.8747(7) 0.3338(8) -0.7360(5) 0.110(4) Uani 1 d . . . H9A H 0.9247 0.3119 -0.7612 0.080 Uiso 1 d R . . H9B H 0.8843 0.3212 -0.6929 0.080 Uiso 1 d R . . C10 C 0.8826(9) 0.4135(8) -0.7362(7) 0.174(8) Uani 1 d . . . H10A H 0.9446 0.4334 -0.7206 0.080 Uiso 1 d R . . H10B H 0.8735 0.4257 -0.7794 0.080 Uiso 1 d R . . H10C H 0.8328 0.4351 -0.7107 0.080 Uiso 1 d R . . C11 C 0.1525(5) 0.3406(4) -0.7847(4) 0.053(2) Uani 1 d . . . C12 C 0.1816(6) 0.3591(5) -0.7217(4) 0.061(2) Uani 1 d . . . H12A H 0.2031 0.3195 -0.6970 0.080 Uiso 1 d R . . C13 C 0.1808(7) 0.4326(6) -0.6945(5) 0.078(3) Uani 1 d . . . H13A H 0.2018 0.4429 -0.6511 0.080 Uiso 1 d R . . C14 C 0.1513(7) 0.4897(5) -0.7287(5) 0.081(3) Uani 1 d . . . H14A H 0.1511 0.5399 -0.7093 0.080 Uiso 1 d R . . C15 C 0.1206(6) 0.4749(5) -0.7915(5) 0.073(3) Uani 1 d . . . H15A H 0.0994 0.5147 -0.8159 0.080 Uiso 1 d R . . C16 C 0.1204(5) 0.4017(5) -0.8190(4) 0.055(2) Uani 1 d . . . C17 C 0.0899(6) 0.3843(5) -0.8852(4) 0.060(2) Uani 1 d . . . C18 C 0.0816(5) 0.2205(5) -0.9802(4) 0.055(2) Uani 1 d . . . C19 C 0.0585(7) 0.4429(5) -0.9279(4) 0.086(3) Uani 1 d . . . H19A H 0.0671 0.4250 -0.9713 0.080 Uiso 1 d R . . H19B H 0.0983 0.4879 -0.9196 0.080 Uiso 1 d R . . C20 C -0.0467(8) 0.4608(6) -0.9186(5) 0.112(4) Uani 1 d . . . H20A H -0.0652 0.4982 -0.9465 0.080 Uiso 1 d R . . H20B H -0.0864 0.4159 -0.9276 0.080 Uiso 1 d R . . H20C H -0.0550 0.4792 -0.8754 0.080 Uiso 1 d R . . C21 C 0.3435(5) 0.2045(4) -0.7528(3) 0.050(2) Uani 1 d . . . H21A H 0.3405 0.2506 -0.7269 0.080 Uiso 1 d R . . H21B H 0.3691 0.1683 -0.7261 0.080 Uiso 1 d R . . C22 C 0.2150(7) 0.0709(4) -0.7892(4) 0.059(2) Uani 1 d . . . C23 C 0.2917(8) 0.0259(5) -0.7771(4) 0.081(3) Uani 1 d . . . H23A H 0.3506 0.0493 -0.7594 0.080 Uiso 1 d R . . C24 C 0.2844(11) -0.0514(7) -0.7894(6) 0.110(4) Uani 1 d . . . H24A H 0.3387 -0.0815 -0.7817 0.080 Uiso 1 d R . . C25 C 0.1978(14) -0.0855(7) -0.8130(7) 0.139(7) Uani 1 d . . . H25A H 0.1928 -0.1390 -0.8218 0.080 Uiso 1 d R . . C26 C 0.1239(11) -0.0428(7) -0.8241(6) 0.123(5) Uani 1 d . . . H26A H 0.0640 -0.0666 -0.8397 0.080 Uiso 1 d R . . C27 C 0.1315(8) 0.0345(5) -0.8123(4) 0.084(3) Uani 1 d . . . H27A H 0.0774 0.0647 -0.8205 0.080 Uiso 1 d R . . C28 C 0.1644(6) 0.1764(4) -0.6925(3) 0.049(2) Uani 1 d . . . C29 C 0.2140(6) 0.1606(5) -0.6386(4) 0.060(2) Uani 1 d . . . H29A H 0.2799 0.1464 -0.6420 0.080 Uiso 1 d R . . C30 C 0.1702(7) 0.1640(5) -0.5806(4) 0.072(3) Uani 1 d . . . H30A H 0.2058 0.1545 -0.5427 0.080 Uiso 1 d R . . C31 C 0.0752(8) 0.1810(5) -0.5771(4) 0.077(3) Uani 1 d . . . H31A H 0.0446 0.1835 -0.5366 0.080 Uiso 1 d R . . C32 C 0.0217(7) 0.1945(5) -0.6308(5) 0.079(3) Uani 1 d . . . H32A H -0.0451 0.2061 -0.6273 0.080 Uiso 1 d R . . C33 C 0.0673(6) 0.1926(4) -0.6883(4) 0.064(2) Uani 1 d . . . H33A H 0.0312 0.2017 -0.7261 0.080 Uiso 1 d R . . C34 C 0.3904(5) 0.2928(4) -0.8604(4) 0.049(2) Uani 1 d . . . C35 C 0.3856(6) 0.3646(5) -0.8313(4) 0.070(3) Uani 1 d . . . H35A H 0.4065 0.3729 -0.7877 0.080 Uiso 1 d R . . C36 C 0.3527(7) 0.4227(5) -0.8632(6) 0.088(3) Uani 1 d . . . H36A H 0.3496 0.4719 -0.8421 0.080 Uiso 1 d R . . C37 C 0.3232(7) 0.4109(7) -0.9258(6) 0.093(4) Uani 1 d . . . H37A H 0.2979 0.4512 -0.9480 0.080 Uiso 1 d R . . C38 C 0.3306(7) 0.3433(6) -0.9556(5) 0.085(3) Uani 1 d . . . H38A H 0.3126 0.3358 -0.9998 0.080 Uiso 1 d R . . C39 C 0.3625(6) 0.2837(5) -0.9243(4) 0.064(2) Uani 1 d . . . H39A H 0.3671 0.2349 -0.9459 0.080 Uiso 1 d R . . C40 C 0.4418(6) 0.1319(4) -0.8598(4) 0.053(2) Uani 1 d . . . C41 C 0.5174(7) 0.0872(5) -0.8495(4) 0.076(3) Uani 1 d . . . H41A H 0.5682 0.1053 -0.8202 0.080 Uiso 1 d R . . C42 C 0.5214(9) 0.0173(6) -0.8806(6) 0.101(4) Uani 1 d . . . H42A H 0.5742 -0.0140 -0.8720 0.080 Uiso 1 d R . . C43 C 0.4490(10) -0.0085(6) -0.9242(5) 0.104(4) Uani 1 d . . . H43A H 0.4525 -0.0567 -0.9469 0.080 Uiso 1 d R . . C44 C 0.3735(8) 0.0357(6) -0.9342(4) 0.081(3) Uani 1 d . . . H44A H 0.3226 0.0182 -0.9636 0.080 Uiso 1 d R . . C45 C 0.3682(6) 0.1047(5) -0.9022(4) 0.062(2) Uani 1 d . . . H45A H 0.3144 0.1356 -0.9092 0.080 Uiso 1 d R . . C51 C -0.1285(5) 0.2492(5) -0.3535(3) 0.054(2) Uani 1 d . . . C52 C -0.1096(6) 0.2281(5) -0.4165(4) 0.065(2) Uani 1 d . . . H52A H -0.0454 0.2148 -0.4279 0.080 Uiso 1 d R . . C53 C -0.1830(7) 0.2262(5) -0.4632(4) 0.074(3) Uani 1 d . . . H53A H -0.1680 0.2123 -0.5065 0.080 Uiso 1 d R . . C54 C -0.2752(6) 0.2440(5) -0.4479(4) 0.072(3) Uani 1 d . . . H54A H -0.3248 0.2421 -0.4803 0.080 Uiso 1 d R . . C55 C -0.2954(6) 0.2643(5) -0.3854(4) 0.067(2) Uani 1 d . . . H55A H -0.3599 0.2771 -0.3745 0.080 Uiso 1 d R . . C56 C -0.2249(6) 0.2669(4) -0.3379(4) 0.054(2) Uani 1 d . . . C57 C -0.2437(5) 0.2872(4) -0.2717(4) 0.053(2) Uani 1 d . . . C58 C -0.0936(6) 0.3167(4) -0.1397(4) 0.054(2) Uani 1 d . . . C59 C -0.3419(5) 0.3052(5) -0.2468(4) 0.072(3) Uani 1 d . . . H59A H -0.3514 0.2814 -0.2079 0.080 Uiso 1 d R . . H59B H -0.3901 0.2845 -0.2769 0.080 Uiso 1 d R . . C60 C -0.3571(6) 0.3879(6) -0.2353(5) 0.093(3) Uani 1 d . . . H60A H -0.4209 0.3957 -0.2197 0.080 Uiso 1 d R . . H60B H -0.3101 0.4089 -0.2045 0.080 Uiso 1 d R . . H60C H -0.3493 0.4120 -0.2743 0.080 Uiso 1 d R . . C61 C 0.3868(5) 0.3466(4) -0.2851(3) 0.0466(19) Uani 1 d . . . C62 C 0.3554(6) 0.3646(5) -0.2237(4) 0.057(2) Uani 1 d . . . H62A H 0.3309 0.3245 -0.1997 0.080 Uiso 1 d R . . C63 C 0.3570(6) 0.4387(5) -0.1971(4) 0.074(3) Uani 1 d . . . H63A H 0.3351 0.4483 -0.1545 0.080 Uiso 1 d R . . C64 C 0.3905(6) 0.4969(5) -0.2303(4) 0.072(3) Uani 1 d . . . H64A H 0.3908 0.5475 -0.2118 0.080 Uiso 1 d R . . C65 C 0.4235(6) 0.4814(5) -0.2917(4) 0.060(2) Uani 1 d . . . H65A H 0.4480 0.5216 -0.3156 0.080 Uiso 1 d R . . C66 C 0.4217(5) 0.4084(4) -0.3188(4) 0.0468(19) Uani 1 d . . . C67 C 0.4525(5) 0.3907(4) -0.3837(4) 0.0456(19) Uani 1 d . . . C68 C 0.4502(5) 0.2250(4) -0.4772(3) 0.0461(19) Uani 1 d . . . C69 C 0.4886(6) 0.4499(4) -0.4258(4) 0.060(2) Uani 1 d . . . H69A H 0.4511 0.4936 -0.4186 0.080 Uiso 1 d R . . H69B H 0.4801 0.4320 -0.4695 0.080 Uiso 1 d R . . C70 C 0.5949(6) 0.4711(5) -0.4131(4) 0.085(3) Uani 1 d . . . H70A H 0.6162 0.5093 -0.4401 0.080 Uiso 1 d R . . H70B H 0.6030 0.4896 -0.3695 0.080 Uiso 1 d R . . H70C H 0.6323 0.4274 -0.4208 0.080 Uiso 1 d R . . C71 C 0.1850(5) 0.2074(4) -0.2578(3) 0.0430(18) Uani 1 d . . . H71A H 0.1557 0.1714 -0.2316 0.080 Uiso 1 d R . . H71B H 0.1916 0.2540 -0.2322 0.080 Uiso 1 d R . . C72 C 0.0830(5) 0.1320(4) -0.3659(3) 0.051(2) Uani 1 d . . . C73 C 0.0034(6) 0.0854(5) -0.3553(4) 0.068(2) Uani 1 d . . . H73A H -0.0452 0.1026 -0.3265 0.080 Uiso 1 d R . . C74 C -0.0057(7) 0.0146(5) -0.3864(5) 0.091(3) Uani 1 d . . . H74A H -0.0614 -0.0172 -0.3793 0.080 Uiso 1 d R . . C75 C 0.0631(9) -0.0109(6) -0.4271(5) 0.105(4) Uani 1 d . . . H75A H 0.0569 -0.0607 -0.4475 0.080 Uiso 1 d R . . C76 C 0.1430(8) 0.0350(6) -0.4366(4) 0.079(3) Uani 1 d . . . H76A H 0.1910 0.0182 -0.4660 0.080 Uiso 1 d R . . C77 C 0.1535(6) 0.1049(5) -0.4063(4) 0.056(2) Uani 1 d . . . H77A H 0.2103 0.1358 -0.4126 0.080 Uiso 1 d R . . C78 C 0.1491(5) 0.2934(4) -0.3686(4) 0.0467(19) Uani 1 d . . . C79 C 0.1701(6) 0.2820(5) -0.4324(4) 0.065(2) Uani 1 d . . . H79A H 0.1602 0.2324 -0.4525 0.080 Uiso 1 d R . . C80 C 0.2047(7) 0.3397(6) -0.4666(5) 0.084(3) Uani 1 d . . . H80A H 0.2180 0.3306 -0.5108 0.080 Uiso 1 d R . . C81 C 0.2207(6) 0.4074(6) -0.4381(6) 0.081(3) Uani 1 d . . . H81A H 0.2471 0.4467 -0.4623 0.080 Uiso 1 d R . . C82 C 0.2002(6) 0.4231(5) -0.3761(5) 0.076(3) Uani 1 d . . . H82A H 0.2119 0.4731 -0.3570 0.080 Uiso 1 d R . . C83 C 0.1633(6) 0.3650(5) -0.3418(4) 0.066(2) Uani 1 d . . . H83A H 0.1473 0.3756 -0.2981 0.080 Uiso 1 d R . . C84 C 0.3031(6) 0.0751(4) -0.2891(3) 0.051(2) Uani 1 d . . . C85 C 0.2237(7) 0.0282(5) -0.2777(4) 0.075(3) Uani 1 d . . . H85A H 0.1658 0.0495 -0.2615 0.080 Uiso 1 d R . . C86 C 0.2277(10) -0.0489(6) -0.2901(5) 0.104(4) Uani 1 d . . . H86A H 0.1729 -0.0810 -0.2814 0.080 Uiso 1 d R . . C87 C 0.3086(13) -0.0801(7) -0.3132(5) 0.118(5) Uani 1 d . . . H87A H 0.3105 -0.1334 -0.3225 0.080 Uiso 1 d R . . C88 C 0.3885(11) -0.0358(7) -0.3239(5) 0.105(4) Uani 1 d . . . H88A H 0.4462 -0.0576 -0.3400 0.080 Uiso 1 d R . . C89 C 0.3859(7) 0.0421(5) -0.3117(4) 0.076(3) Uani 1 d . . . H89A H 0.4419 0.0735 -0.3191 0.080 Uiso 1 d R . . C90 C 0.3590(5) 0.1811(4) -0.1908(3) 0.0437(18) Uani 1 d . . . C91 C 0.3043(6) 0.1665(4) -0.1382(4) 0.057(2) Uani 1 d . . . H91A H 0.2366 0.1539 -0.1436 0.080 Uiso 1 d R . . C92 C 0.3481(7) 0.1693(5) -0.0785(4) 0.072(3) Uani 1 d . . . H92A H 0.3092 0.1614 -0.0422 0.080 Uiso 1 d R . . C93 C 0.4437(7) 0.1840(5) -0.0702(4) 0.072(3) Uani 1 d . . . H93A H 0.4727 0.1847 -0.0285 0.080 Uiso 1 d R . . C94 C 0.5000(6) 0.1971(5) -0.1218(4) 0.071(3) Uani 1 d . . . H94A H 0.5683 0.2071 -0.1159 0.080 Uiso 1 d R . . C95 C 0.4571(6) 0.1962(5) -0.1819(4) 0.063(2) Uani 1 d . . . H95A H 0.4960 0.2061 -0.2178 0.080 Uiso 1 d R . . N1 N 0.7032(4) 0.3043(4) -0.7238(3) 0.0577(18) Uani 1 d . . . N2 N 0.7137(5) 0.3311(4) -0.6610(3) 0.069(2) Uani 1 d . . . N3 N 0.6306(5) 0.3565(4) -0.5700(3) 0.073(2) Uani 1 d . . . H3B H 0.5745 0.3560 -0.5491 0.080 Uiso 1 d R . . H3C H 0.6854 0.3744 -0.5498 0.080 Uiso 1 d R . . N4 N 0.0926(4) 0.3147(4) -0.9040(3) 0.0492(16) Uani 1 d . . . N5 N 0.0676(5) 0.2920(4) -0.9664(3) 0.0588(18) Uani 1 d . . . N6 N 0.0626(5) 0.1907(4) -1.0401(3) 0.081(2) Uani 1 d . . . H6A H 0.0701 0.1415 -1.0502 0.080 Uiso 1 d R . . H6B H 0.0423 0.2205 -1.0699 0.080 Uiso 1 d R . . N7 N -0.1669(4) 0.2932(3) -0.2351(3) 0.0519(17) Uani 1 d . . . N8 N -0.1765(5) 0.3141(4) -0.1711(3) 0.0582(18) Uani 1 d . . . N9 N -0.0950(5) 0.3384(4) -0.0770(3) 0.075(2) Uani 1 d . . . H9C H -0.0398 0.3401 -0.0537 0.080 Uiso 1 d R . . H9D H -0.1506 0.3514 -0.0587 0.080 Uiso 1 d R . . N10 N 0.4445(4) 0.3200(3) -0.4026(3) 0.0425(15) Uani 1 d . . . N11 N 0.4690(4) 0.2963(3) -0.4640(3) 0.0470(15) Uani 1 d . . . N12 N 0.4658(5) 0.1949(4) -0.5365(3) 0.068(2) Uani 1 d . . . H12B H 0.4533 0.1455 -0.5461 0.080 Uiso 1 d R . . H12C H 0.4885 0.2242 -0.5663 0.080 Uiso 1 d R . . P1 P 0.43662(15) 0.22085(12) -0.81265(9) 0.0499(5) Uani 1 d . . . P2 P 0.21772(15) 0.17240(11) -0.77154(9) 0.0471(5) Uani 1 d . . . P3 P 0.09476(14) 0.22216(11) -0.32006(9) 0.0450(5) Uani 1 d . . . P4 P 0.30855(14) 0.17701(11) -0.27153(9) 0.0412(5) Uani 1 d . . . S1 S 0.51812(15) 0.29723(13) -0.66308(9) 0.0606(6) Uani 1 d . . . S2 S 0.12054(17) 0.15506(12) -0.92739(10) 0.0632(6) Uani 1 d . . . S3 S 0.01814(15) 0.29235(13) -0.17047(10) 0.0634(6) Uani 1 d . . . S4 S 0.40624(15) 0.15953(11) -0.42457(9) 0.0546(5) Uani 1 d . . . Pd1 Pd 0.57624(4) 0.26420(4) -0.76456(3) 0.05397(19) Uani 1 d . . . Pd2 Pd 0.14645(4) 0.24403(3) -0.84149(3) 0.04789(17) Uani 1 d . . . Pd3 Pd -0.04168(4) 0.26156(3) -0.27424(3) 0.04766(17) Uani 1 d . . . Pd4 Pd 0.38661(4) 0.24898(3) -0.34008(2) 0.04006(16) Uani 1 d . . . O1S O -0.1938(6) 0.4272(5) -0.4946(5) 0.139(3) Uani 1 d . . . C1S C -0.1118(9) 0.4119(6) -0.4910(6) 0.084(3) Uani 1 d . . . C2S C -0.0537(9) 0.4276(6) -0.4318(5) 0.124(4) Uani 1 d . . . H2SA H -0.0937 0.4524 -0.4009 0.080 Uiso 1 d R . . H2SB H -0.0327 0.3816 -0.4162 0.080 Uiso 1 d R . . H2SC H 0.0016 0.4597 -0.4393 0.080 Uiso 1 d R . . C3S C -0.0629(10) 0.3753(7) -0.5430(6) 0.145(5) Uani 1 d . . . H3SA H -0.1077 0.3683 -0.5783 0.080 Uiso 1 d R . . H3SB H -0.0079 0.4054 -0.5547 0.080 Uiso 1 d R . . H3SC H -0.0422 0.3273 -0.5315 0.080 Uiso 1 d R . . O2S O 0.7298(8) 0.4064(6) -1.0227(6) 0.213(7) Uani 1 d . . . C4S C 0.6517(11) 0.4056(6) -1.0062(7) 0.103(4) Uani 1 d . . . C5S C 0.5759(14) 0.3820(9) -1.0511(7) 0.243(12) Uani 1 d . . . H5SA H 0.5997 0.3701 -1.0929 0.080 Uiso 1 d R . . H5SB H 0.5404 0.3392 -1.0370 0.080 Uiso 1 d R . . H5SC H 0.5343 0.4236 -1.0522 0.080 Uiso 1 d R . . C6S C 0.6198(11) 0.4234(7) -0.9459(6) 0.166(6) Uani 1 d . . . H6SA H 0.6761 0.4360 -0.9196 0.080 Uiso 1 d R . . H6SB H 0.5790 0.4657 -0.9452 0.080 Uiso 1 d R . . H6SC H 0.5851 0.3812 -0.9301 0.080 Uiso 1 d R . . O3S O 0.3894(5) 0.0455(4) -0.5928(4) 0.113(3) Uani 1 d . . . C7S C 0.3543(8) -0.0132(6) -0.5772(6) 0.084(3) Uani 1 d . . . C8S C 0.3746(8) -0.0437(6) -0.5162(5) 0.111(4) Uani 1 d . . . H8SA H 0.4188 -0.0108 -0.4910 0.080 Uiso 1 d R . . H8SB H 0.3150 -0.0494 -0.4941 0.080 Uiso 1 d R . . H8SC H 0.4021 -0.0919 -0.5236 0.080 Uiso 1 d R . . C9S C 0.2931(13) -0.0586(8) -0.6198(7) 0.293(14) Uani 1 d . . . H9SA H 0.2792 -0.0391 -0.6601 0.080 Uiso 1 d R . . H9SB H 0.3185 -0.1077 -0.6266 0.080 Uiso 1 d R . . H9SC H 0.2349 -0.0619 -0.5960 0.080 Uiso 1 d R . . O4S O 0.1118(7) 0.0439(5) -0.0994(5) 0.150(4) Uani 1 d . . . C10S C 0.1356(9) -0.0160(9) -0.0845(7) 0.118(5) Uani 1 d . . . C11S C 0.1699(15) -0.0684(9) -0.1281(7) 0.41(2) Uani 1 d . . . H11B H 0.1765 -0.0450 -0.1675 0.080 Uiso 1 d R . . H11C H 0.2316 -0.0851 -0.1148 0.080 Uiso 1 d R . . H11D H 0.1248 -0.1107 -0.1338 0.080 Uiso 1 d R . . C12S C 0.1235(9) -0.0460(7) -0.0220(6) 0.140(5) Uani 1 d . . . H12D H 0.1004 -0.0070 0.0066 0.080 Uiso 1 d R . . H12E H 0.0774 -0.0878 -0.0253 0.080 Uiso 1 d R . . H12F H 0.1841 -0.0622 -0.0062 0.080 Uiso 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.060(6) 0.065(6) 0.052(5) 0.012(5) 0.016(5) 0.009(4) C2 0.074(7) 0.091(7) 0.061(6) 0.016(5) 0.015(5) 0.000(5) C3 0.112(9) 0.090(8) 0.071(7) 0.025(6) 0.031(7) 0.008(7) C4 0.084(8) 0.111(9) 0.073(8) 0.020(7) 0.038(7) 0.012(7) C5 0.061(6) 0.108(8) 0.080(7) 0.026(6) 0.025(6) 0.014(6) C6 0.056(6) 0.090(7) 0.065(6) 0.025(5) 0.020(5) 0.009(5) C7 0.040(5) 0.103(7) 0.062(6) 0.021(5) 0.000(5) 0.011(5) C8 0.061(6) 0.063(6) 0.047(5) 0.011(4) -0.006(4) 0.000(4) C9 0.065(7) 0.200(14) 0.061(7) -0.005(9) 0.000(6) -0.004(9) C10 0.102(11) 0.239(19) 0.162(14) -0.095(15) 0.036(10) -0.054(12) C11 0.046(5) 0.059(5) 0.058(5) 0.017(4) 0.018(4) 0.001(4) C12 0.074(6) 0.053(6) 0.055(6) 0.002(5) 0.008(5) -0.005(4) C13 0.083(7) 0.074(7) 0.074(7) -0.014(6) 0.002(6) -0.014(6) C14 0.090(7) 0.049(6) 0.104(9) -0.004(6) 0.017(7) -0.001(5) C15 0.080(7) 0.064(7) 0.075(7) 0.015(6) 0.012(6) -0.001(5) C16 0.048(5) 0.058(6) 0.060(6) 0.009(5) 0.010(4) -0.002(4) C17 0.070(6) 0.045(5) 0.069(6) 0.021(5) 0.010(5) 0.007(4) C18 0.054(5) 0.069(6) 0.043(5) 0.017(5) -0.001(4) -0.001(4) C19 0.122(9) 0.064(6) 0.076(7) 0.026(5) 0.008(6) 0.018(6) C20 0.132(10) 0.093(8) 0.119(10) 0.048(7) 0.000(8) 0.034(7) C21 0.058(5) 0.061(5) 0.031(4) 0.007(4) 0.002(4) 0.004(4) C22 0.093(7) 0.049(5) 0.035(5) 0.015(4) 0.011(5) 0.001(5) C23 0.119(9) 0.051(6) 0.075(7) 0.020(5) 0.011(6) 0.006(6) C24 0.161(13) 0.074(9) 0.103(10) 0.039(8) 0.024(9) 0.040(8) C25 0.26(2) 0.050(9) 0.107(11) 0.016(8) 0.041(13) -0.012(11) C26 0.203(16) 0.058(8) 0.103(10) 0.011(7) -0.026(10) -0.051(8) C27 0.119(9) 0.059(7) 0.072(7) 0.009(5) -0.024(6) -0.020(6) C28 0.065(6) 0.048(5) 0.035(4) 0.006(4) 0.010(4) -0.004(4) C29 0.063(6) 0.077(6) 0.041(5) 0.010(4) 0.007(4) 0.003(5) C30 0.088(7) 0.088(7) 0.039(5) 0.001(5) 0.002(5) -0.022(6) C31 0.084(8) 0.092(7) 0.051(6) -0.009(5) 0.028(6) -0.022(6) C32 0.062(6) 0.091(7) 0.083(7) 0.000(6) 0.027(6) 0.000(5) C33 0.060(6) 0.073(6) 0.062(6) 0.013(5) 0.011(5) -0.002(5) C34 0.040(4) 0.054(5) 0.054(5) 0.016(4) 0.012(4) 0.004(4) C35 0.078(6) 0.055(6) 0.077(6) 0.003(5) 0.018(5) 0.000(5) C36 0.095(8) 0.046(6) 0.128(10) 0.023(7) 0.042(8) 0.016(5) C37 0.083(8) 0.093(9) 0.114(10) 0.067(8) 0.032(7) 0.030(7) C38 0.089(7) 0.090(8) 0.082(7) 0.048(7) 0.011(6) 0.019(6) C39 0.075(6) 0.064(6) 0.052(6) 0.008(5) 0.002(5) -0.002(5) C40 0.068(6) 0.050(5) 0.043(5) 0.011(4) 0.010(4) 0.017(4) C41 0.083(7) 0.076(7) 0.070(6) 0.008(6) 0.014(5) 0.020(6) C42 0.119(10) 0.079(8) 0.110(10) 0.015(7) 0.008(8) 0.051(7) C43 0.154(12) 0.073(8) 0.086(9) -0.012(7) 0.016(8) 0.036(8) C44 0.120(9) 0.071(7) 0.049(6) -0.011(5) 0.004(6) -0.001(6) C45 0.079(6) 0.057(6) 0.049(5) 0.000(5) 0.006(5) 0.004(5) C51 0.047(5) 0.078(6) 0.039(5) 0.018(4) -0.003(4) -0.002(4) C52 0.050(5) 0.083(6) 0.063(6) 0.004(5) -0.001(5) 0.001(5) C53 0.076(7) 0.107(8) 0.039(5) 0.013(5) -0.017(5) -0.005(6) C54 0.054(6) 0.093(7) 0.070(7) 0.015(6) -0.026(5) -0.006(5) C55 0.052(5) 0.074(6) 0.076(7) 0.006(5) -0.013(5) 0.003(4) C56 0.047(5) 0.061(5) 0.053(5) 0.012(4) -0.005(4) 0.000(4) C57 0.041(5) 0.064(5) 0.057(5) 0.014(4) 0.004(4) 0.004(4) C58 0.063(6) 0.057(5) 0.045(5) 0.012(4) 0.013(4) 0.009(4) C59 0.040(5) 0.100(8) 0.077(6) 0.012(6) 0.001(5) -0.003(5) C60 0.057(6) 0.120(9) 0.100(8) -0.014(7) -0.003(6) 0.027(6) C61 0.047(5) 0.052(5) 0.041(4) 0.004(4) 0.000(4) 0.002(4) C62 0.061(5) 0.056(5) 0.055(5) 0.002(4) 0.004(4) -0.001(4) C63 0.090(7) 0.079(7) 0.049(5) -0.010(5) 0.014(5) -0.003(6) C64 0.085(7) 0.060(6) 0.068(6) -0.014(5) 0.007(5) 0.003(5) C65 0.067(6) 0.053(6) 0.062(6) 0.012(5) 0.000(5) 0.004(4) C66 0.037(4) 0.050(5) 0.054(5) 0.003(4) -0.004(4) 0.003(4) C67 0.033(4) 0.051(5) 0.053(5) 0.013(4) -0.003(4) -0.005(4) C68 0.041(4) 0.060(5) 0.039(5) 0.012(4) 0.009(4) 0.002(4) C69 0.078(6) 0.050(5) 0.055(5) 0.019(4) 0.003(5) 0.001(4) C70 0.083(7) 0.091(7) 0.083(7) 0.031(6) -0.002(6) -0.034(5) C71 0.040(4) 0.060(5) 0.028(4) 0.004(4) -0.006(3) -0.001(4) C72 0.049(5) 0.061(5) 0.042(5) 0.005(4) -0.007(4) -0.002(4) C73 0.058(6) 0.068(6) 0.075(6) -0.008(5) 0.000(5) -0.012(5) C74 0.085(7) 0.066(7) 0.117(9) -0.013(6) 0.008(7) -0.024(6) C75 0.130(11) 0.075(8) 0.105(9) -0.030(7) 0.009(8) -0.008(8) C76 0.096(8) 0.077(7) 0.065(6) -0.009(6) 0.010(6) 0.015(6) C77 0.053(5) 0.065(6) 0.049(5) 0.001(4) 0.000(4) 0.004(4) C78 0.043(5) 0.050(5) 0.047(5) 0.004(4) -0.006(4) 0.006(4) C79 0.073(6) 0.069(6) 0.055(6) 0.016(5) 0.002(5) -0.001(5) C80 0.092(8) 0.088(8) 0.075(7) 0.025(7) 0.020(6) -0.004(6) C81 0.062(6) 0.077(8) 0.108(9) 0.053(7) -0.003(6) -0.009(5) C82 0.067(6) 0.055(6) 0.105(8) 0.017(6) -0.027(6) -0.003(5) C83 0.060(6) 0.077(7) 0.061(6) 0.010(5) -0.015(5) 0.005(5) C84 0.078(6) 0.047(5) 0.028(4) 0.011(4) -0.002(4) 0.005(4) C85 0.100(8) 0.060(6) 0.064(6) 0.008(5) 0.000(5) -0.010(5) C86 0.156(12) 0.054(8) 0.102(9) 0.021(6) -0.009(8) -0.024(7) C87 0.221(18) 0.056(8) 0.078(8) -0.003(7) -0.013(10) 0.023(10) C88 0.173(13) 0.074(8) 0.074(7) 0.017(7) 0.021(8) 0.054(8) C89 0.103(8) 0.073(7) 0.057(6) 0.017(5) 0.018(6) 0.031(6) C90 0.048(5) 0.053(5) 0.032(4) 0.012(4) 0.001(4) 0.005(4) C91 0.056(5) 0.070(6) 0.045(5) 0.011(4) 0.001(4) 0.001(4) C92 0.087(7) 0.096(7) 0.035(5) 0.010(5) 0.003(5) 0.012(6) C93 0.080(7) 0.097(7) 0.039(5) 0.009(5) -0.011(5) 0.020(6) C94 0.048(5) 0.100(7) 0.066(6) 0.011(5) -0.022(5) 0.006(5) C95 0.047(5) 0.098(7) 0.046(5) 0.015(5) -0.007(4) -0.002(5) N1 0.041(4) 0.079(5) 0.056(4) 0.020(4) 0.005(3) 0.008(3) N2 0.052(4) 0.112(6) 0.045(4) 0.012(4) 0.000(4) -0.004(4) N3 0.058(5) 0.103(6) 0.057(5) 0.004(4) -0.002(4) -0.009(4) N4 0.053(4) 0.053(4) 0.042(4) 0.014(3) -0.002(3) -0.001(3) N5 0.070(5) 0.057(5) 0.051(4) 0.011(4) 0.001(4) 0.008(4) N6 0.123(7) 0.073(5) 0.048(4) 0.003(4) -0.027(4) 0.021(5) N7 0.044(4) 0.061(4) 0.053(4) 0.018(4) 0.004(3) 0.004(3) N8 0.051(4) 0.077(5) 0.047(4) 0.003(4) 0.005(4) 0.013(4) N9 0.065(5) 0.120(6) 0.041(4) 0.003(4) 0.007(4) 0.027(4) N10 0.037(3) 0.054(4) 0.038(4) 0.008(3) -0.002(3) 0.005(3) N11 0.048(4) 0.053(4) 0.040(4) 0.005(3) 0.001(3) -0.007(3) N12 0.103(6) 0.057(4) 0.043(4) 0.001(3) 0.020(4) -0.009(4) P1 0.0522(13) 0.0592(14) 0.0394(11) 0.0072(10) 0.0072(10) 0.0073(10) P2 0.0534(13) 0.0542(13) 0.0345(11) 0.0102(10) 0.0018(10) -0.0002(10) P3 0.0407(11) 0.0567(13) 0.0378(11) 0.0046(10) -0.0017(9) 0.0030(10) P4 0.0441(11) 0.0477(12) 0.0326(10) 0.0077(9) 0.0020(9) 0.0041(9) S1 0.0545(13) 0.0837(16) 0.0439(12) 0.0107(11) 0.0051(10) -0.0072(11) S2 0.0845(16) 0.0563(14) 0.0490(13) 0.0098(11) -0.0133(12) 0.0012(12) S3 0.0491(13) 0.0980(18) 0.0437(12) 0.0032(12) -0.0018(10) 0.0157(12) S4 0.0726(14) 0.0481(12) 0.0438(12) 0.0054(10) 0.0143(11) 0.0006(10) Pd1 0.0496(4) 0.0717(5) 0.0423(4) 0.0136(3) 0.0068(3) 0.0034(3) Pd2 0.0514(4) 0.0500(4) 0.0430(4) 0.0110(3) -0.0010(3) -0.0019(3) Pd3 0.0413(3) 0.0624(4) 0.0401(3) 0.0075(3) -0.0011(3) 0.0058(3) Pd4 0.0402(3) 0.0457(4) 0.0352(3) 0.0085(3) 0.0026(3) 0.0023(3) O1S 0.078(5) 0.120(7) 0.222(10) 0.027(7) -0.029(6) 0.016(5) C1S 0.082(8) 0.067(7) 0.103(9) 0.009(6) -0.014(7) -0.002(6) C2S 0.147(11) 0.107(10) 0.117(10) 0.009(8) -0.028(9) 0.011(8) C3S 0.188(15) 0.134(12) 0.113(11) 0.006(9) 0.018(11) 0.004(10) O2S 0.165(10) 0.219(12) 0.282(14) 0.122(11) 0.134(11) 0.108(9) C4S 0.134(11) 0.062(7) 0.118(11) 0.007(7) 0.052(10) 0.033(8) C5S 0.42(3) 0.175(17) 0.123(15) -0.002(13) 0.025(19) -0.151(19) C6S 0.220(17) 0.116(11) 0.159(14) -0.017(10) 0.053(13) 0.014(11) O3S 0.117(6) 0.069(5) 0.153(7) 0.009(5) -0.016(5) -0.010(4) C7S 0.091(8) 0.064(7) 0.096(8) -0.005(7) -0.023(7) 0.004(6) C8S 0.093(8) 0.103(9) 0.133(11) -0.031(8) -0.019(8) 0.018(7) C9S 0.52(4) 0.182(16) 0.162(16) 0.102(14) -0.19(2) -0.19(2) O4S 0.165(9) 0.090(7) 0.195(10) 0.008(7) 0.006(7) 0.025(6) C10S 0.112(10) 0.115(12) 0.127(12) -0.004(10) 0.048(9) 0.011(9) C11S 0.76(6) 0.26(2) 0.27(2) 0.19(2) 0.34(3) 0.32(3) C12S 0.117(11) 0.121(11) 0.177(15) -0.032(11) 0.001(11) -0.002(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.367(11) . ? C1 C6 1.421(12) . ? C1 Pd1 2.046(7) . ? C2 C3 1.423(11) . ? C3 C4 1.372(14) . ? C4 C5 1.375(13) . ? C5 C6 1.400(10) . ? C6 C7 1.458(12) . ? C7 N1 1.301(9) . ? C7 C9 1.480(13) . ? C8 N2 1.304(9) . ? C8 N3 1.348(9) . ? C8 S1 1.766(9) . ? C9 C10 1.423(15) . ? C11 C12 1.397(11) . ? C11 C16 1.430(10) . ? C11 Pd2 2.031(8) . ? C12 C13 1.396(11) . ? C13 C14 1.361(12) . ? C14 C15 1.391(12) . ? C15 C16 1.392(11) . ? C16 C17 1.462(11) . ? C17 N4 1.281(9) . ? C17 C19 1.500(10) . ? C18 N5 1.312(9) . ? C18 N6 1.356(10) . ? C18 S2 1.764(8) . ? C19 C20 1.518(12) . ? C21 P2 1.840(7) . ? C21 P1 1.850(7) . ? C22 C27 1.370(12) . ? C22 C23 1.389(11) . ? C22 P2 1.823(8) . ? C23 C24 1.385(13) . ? C24 C25 1.393(18) . ? C25 C26 1.327(18) . ? C26 C27 1.385(13) . ? C28 C29 1.371(10) . ? C28 C33 1.391(10) . ? C28 P2 1.835(7) . ? C29 C30 1.375(10) . ? C30 C31 1.364(12) . ? C31 C32 1.385(12) . ? C32 C33 1.377(10) . ? C34 C35 1.387(10) . ? C34 C39 1.395(10) . ? C34 P1 1.816(7) . ? C35 C36 1.364(12) . ? C36 C37 1.377(14) . ? C37 C38 1.332(13) . ? C38 C39 1.375(11) . ? C40 C41 1.366(11) . ? C40 C45 1.394(11) . ? C40 P1 1.820(8) . ? C41 C42 1.373(13) . ? C42 C43 1.393(15) . ? C43 C44 1.357(13) . ? C44 C45 1.369(11) . ? C51 C52 1.391(10) . ? C51 C56 1.423(10) . ? C51 Pd3 2.038(8) . ? C52 C53 1.402(11) . ? C53 C54 1.367(11) . ? C54 C55 1.380(11) . ? C55 C56 1.386(11) . ? C56 C57 1.451(10) . ? C57 N7 1.301(9) . ? C57 C59 1.506(10) . ? C58 N8 1.313(10) . ? C58 N9 1.355(9) . ? C58 S3 1.749(8) . ? C59 C60 1.503(11) . ? C61 C62 1.396(10) . ? C61 C66 1.426(9) . ? C61 Pd4 2.028(7) . ? C62 C63 1.401(11) . ? C63 C64 1.364(11) . ? C64 C65 1.394(10) . ? C65 C66 1.386(10) . ? C66 C67 1.461(10) . ? C67 N10 1.298(8) . ? C67 C69 1.502(9) . ? C68 N11 1.299(9) . ? C68 N12 1.353(9) . ? C68 S4 1.766(7) . ? C69 C70 1.520(11) . ? C71 P4 1.838(6) . ? C71 P3 1.838(7) . ? C72 C73 1.386(10) . ? C72 C77 1.387(9) . ? C72 P3 1.821(8) . ? C73 C74 1.384(11) . ? C74 C75 1.366(12) . ? C75 C76 1.377(13) . ? C76 C77 1.363(11) . ? C78 C83 1.367(10) . ? C78 C79 1.388(10) . ? C78 P3 1.834(7) . ? C79 C80 1.373(11) . ? C80 C81 1.322(12) . ? C81 C82 1.357(12) . ? C82 C83 1.393(11) . ? C84 C89 1.387(10) . ? C84 C85 1.390(11) . ? C84 P4 1.831(8) . ? C85 C86 1.387(12) . ? C86 C87 1.356(15) . ? C87 C88 1.365(16) . ? C88 C89 1.400(13) . ? C90 C95 1.382(10) . ? C90 C91 1.389(9) . ? C90 P4 1.827(7) . ? C91 C92 1.386(11) . ? C92 C93 1.347(12) . ? C93 C94 1.378(11) . ? C94 C95 1.391(10) . ? N1 N2 1.380(9) . ? N1 Pd1 2.028(7) . ? N4 N5 1.387(8) . ? N4 Pd2 2.040(6) . ? N7 N8 1.388(8) . ? N7 Pd3 2.019(6) . ? N10 N11 1.387(7) . ? N10 Pd4 2.045(5) . ? P1 Pd1 2.253(2) . ? P2 Pd2 2.259(2) . ? P3 Pd3 2.2541(19) . ? P4 Pd4 2.2616(18) . ? S1 Pd1 2.348(2) . ? S2 Pd2 2.341(2) . ? S3 Pd3 2.351(2) . ? S4 Pd4 2.339(2) . ? O1S C1S 1.181(11) . ? C1S C3S 1.435(13) . ? C1S C2S 1.480(14) . ? O2S C4S 1.143(13) . ? C4S C6S 1.377(14) . ? C4S C5S 1.433(19) . ? O3S C7S 1.206(11) . ? C7S C9S 1.417(15) . ? C7S C8S 1.460(13) . ? O4S C10S 1.194(14) . ? C10S C11S 1.372(16) . ? C10S C12S 1.468(16) . ? 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 C2 C1 C6 118.3(8) . . ? C2 C1 Pd1 132.4(7) . . ? C6 C1 Pd1 109.4(6) . . ? C1 C2 C3 121.9(9) . . ? C4 C3 C2 119.0(10) . . ? C3 C4 C5 120.2(9) . . ? C4 C5 C6 121.2(10) . . ? C5 C6 C1 119.4(9) . . ? C5 C6 C7 122.3(9) . . ? C1 C6 C7 118.2(7) . . ? N1 C7 C6 113.9(8) . . ? N1 C7 C9 122.1(9) . . ? C6 C7 C9 123.9(8) . . ? N2 C8 N3 119.1(8) . . ? N2 C8 S1 126.7(6) . . ? N3 C8 S1 114.2(6) . . ? C10 C9 C7 111.5(11) . . ? C12 C11 C16 115.6(8) . . ? C12 C11 Pd2 134.1(6) . . ? C16 C11 Pd2 110.3(6) . . ? C13 C12 C11 122.0(8) . . ? C14 C13 C12 121.0(9) . . ? C13 C14 C15 119.8(9) . . ? C14 C15 C16 119.7(9) . . ? C15 C16 C11 121.9(8) . . ? C15 C16 C17 121.1(8) . . ? C11 C16 C17 117.0(8) . . ? N4 C17 C16 114.4(7) . . ? N4 C17 C19 122.4(8) . . ? C16 C17 C19 123.1(8) . . ? N5 C18 N6 119.3(7) . . ? N5 C18 S2 126.6(6) . . ? N6 C18 S2 114.0(7) . . ? C17 C19 C20 111.7(7) . . ? P2 C21 P1 124.7(4) . . ? C27 C22 C23 116.3(9) . . ? C27 C22 P2 119.6(7) . . ? C23 C22 P2 124.0(8) . . ? C24 C23 C22 121.6(11) . . ? C23 C24 C25 119.7(13) . . ? C26 C25 C24 119.0(14) . . ? C25 C26 C27 121.3(14) . . ? C22 C27 C26 122.1(11) . . ? C29 C28 C33 119.0(7) . . ? C29 C28 P2 123.3(6) . . ? C33 C28 P2 117.6(6) . . ? C28 C29 C30 120.9(8) . . ? C31 C30 C29 119.3(9) . . ? C30 C31 C32 121.5(8) . . ? C33 C32 C31 118.5(8) . . ? C32 C33 C28 120.8(8) . . ? C35 C34 C39 116.5(7) . . ? C35 C34 P1 117.1(7) . . ? C39 C34 P1 126.3(6) . . ? C36 C35 C34 121.7(9) . . ? C35 C36 C37 120.0(10) . . ? C38 C37 C36 119.6(10) . . ? C37 C38 C39 121.4(10) . . ? C38 C39 C34 120.7(9) . . ? C41 C40 C45 118.5(8) . . ? C41 C40 P1 118.4(7) . . ? C45 C40 P1 122.9(6) . . ? C40 C41 C42 120.8(10) . . ? C41 C42 C43 120.3(10) . . ? C44 C43 C42 118.9(10) . . ? C43 C44 C45 120.9(11) . . ? C44 C45 C40 120.5(9) . . ? C52 C51 C56 117.9(7) . . ? C52 C51 Pd3 132.0(6) . . ? C56 C51 Pd3 110.1(5) . . ? C51 C52 C53 120.7(8) . . ? C54 C53 C52 121.0(8) . . ? C53 C54 C55 119.0(8) . . ? C54 C55 C56 121.7(8) . . ? C55 C56 C51 119.7(7) . . ? C55 C56 C57 123.2(8) . . ? C51 C56 C57 117.1(7) . . ? N7 C57 C56 114.3(7) . . ? N7 C57 C59 121.6(7) . . ? C56 C57 C59 124.0(8) . . ? N8 C58 N9 117.0(7) . . ? N8 C58 S3 126.4(6) . . ? N9 C58 S3 116.6(7) . . ? C60 C59 C57 114.1(7) . . ? C62 C61 C66 115.8(7) . . ? C62 C61 Pd4 132.8(6) . . ? C66 C61 Pd4 111.3(5) . . ? C61 C62 C63 122.1(7) . . ? C64 C63 C62 121.1(8) . . ? C63 C64 C65 118.7(8) . . ? C66 C65 C64 121.0(8) . . ? C65 C66 C61 121.4(7) . . ? C65 C66 C67 122.2(7) . . ? C61 C66 C67 116.4(7) . . ? N10 C67 C66 114.7(6) . . ? N10 C67 C69 122.7(7) . . ? C66 C67 C69 122.6(7) . . ? N11 C68 N12 119.3(6) . . ? N11 C68 S4 126.7(6) . . ? N12 C68 S4 114.0(6) . . ? C67 C69 C70 111.9(7) . . ? P4 C71 P3 125.4(4) . . ? C73 C72 C77 118.4(8) . . ? C73 C72 P3 117.8(6) . . ? C77 C72 P3 123.5(6) . . ? C74 C73 C72 119.8(8) . . ? C75 C74 C73 121.2(9) . . ? C74 C75 C76 118.8(10) . . ? C77 C76 C75 120.9(9) . . ? C76 C77 C72 120.8(8) . . ? C83 C78 C79 116.7(7) . . ? C83 C78 P3 118.1(6) . . ? C79 C78 P3 125.0(7) . . ? C80 C79 C78 121.5(9) . . ? C81 C80 C79 119.8(10) . . ? C80 C81 C82 122.1(9) . . ? C81 C82 C83 118.2(9) . . ? C78 C83 C82 121.8(9) . . ? C89 C84 C85 117.9(8) . . ? C89 C84 P4 117.6(7) . . ? C85 C84 P4 124.3(7) . . ? C86 C85 C84 120.3(9) . . ? C87 C86 C85 121.0(12) . . ? C86 C87 C88 120.2(12) . . ? C87 C88 C89 119.6(12) . . ? C84 C89 C88 121.0(10) . . ? C95 C90 C91 118.2(7) . . ? C95 C90 P4 118.5(5) . . ? C91 C90 P4 123.2(6) . . ? C92 C91 C90 119.9(8) . . ? C93 C92 C91 121.5(8) . . ? C92 C93 C94 119.8(8) . . ? C93 C94 C95 119.6(8) . . ? C90 C95 C94 121.0(7) . . ? C7 N1 N2 119.0(7) . . ? C7 N1 Pd1 117.0(6) . . ? N2 N1 Pd1 124.0(5) . . ? C8 N2 N1 112.4(7) . . ? C17 N4 N5 119.5(7) . . ? C17 N4 Pd2 117.2(6) . . ? N5 N4 Pd2 123.1(5) . . ? C18 N5 N4 112.6(6) . . ? C57 N7 N8 119.0(6) . . ? C57 N7 Pd3 117.0(5) . . ? N8 N7 Pd3 123.8(5) . . ? C58 N8 N7 112.4(6) . . ? C67 N10 N11 120.2(6) . . ? C67 N10 Pd4 116.7(5) . . ? N11 N10 Pd4 123.0(5) . . ? C68 N11 N10 112.8(6) . . ? C34 P1 C40 110.5(4) . . ? C34 P1 C21 105.6(3) . . ? C40 P1 C21 105.0(3) . . ? C34 P1 Pd1 109.1(3) . . ? C40 P1 Pd1 115.8(3) . . ? C21 P1 Pd1 110.2(2) . . ? C22 P2 C28 99.9(3) . . ? C22 P2 C21 108.2(4) . . ? C28 P2 C21 101.7(3) . . ? C22 P2 Pd2 118.4(3) . . ? C28 P2 Pd2 114.7(3) . . ? C21 P2 Pd2 112.1(2) . . ? C72 P3 C78 109.9(3) . . ? C72 P3 C71 104.2(3) . . ? C78 P3 C71 105.9(3) . . ? C72 P3 Pd3 115.3(3) . . ? C78 P3 Pd3 111.6(2) . . ? C71 P3 Pd3 109.1(2) . . ? C90 P4 C84 99.4(3) . . ? C90 P4 C71 101.9(3) . . ? C84 P4 C71 108.2(4) . . ? C90 P4 Pd4 116.0(2) . . ? C84 P4 Pd4 118.0(2) . . ? C71 P4 Pd4 111.6(2) . . ? C8 S1 Pd1 94.6(3) . . ? C18 S2 Pd2 94.8(3) . . ? C58 S3 Pd3 95.0(3) . . ? C68 S4 Pd4 94.9(3) . . ? N1 Pd1 C1 81.5(3) . . ? N1 Pd1 P1 178.31(18) . . ? C1 Pd1 P1 97.1(3) . . ? N1 Pd1 S1 82.27(19) . . ? C1 Pd1 S1 163.3(3) . . ? P1 Pd1 S1 99.16(7) . . ? C11 Pd2 N4 81.0(3) . . ? C11 Pd2 P2 96.4(2) . . ? N4 Pd2 P2 175.02(18) . . ? C11 Pd2 S2 163.7(2) . . ? N4 Pd2 S2 82.7(2) . . ? P2 Pd2 S2 99.96(7) . . ? N7 Pd3 C51 81.1(3) . . ? N7 Pd3 P3 177.7(2) . . ? C51 Pd3 P3 97.2(2) . . ? N7 Pd3 S3 82.2(2) . . ? C51 Pd3 S3 163.1(2) . . ? P3 Pd3 S3 99.50(7) . . ? C61 Pd4 N10 80.8(3) . . ? C61 Pd4 P4 96.7(2) . . ? N10 Pd4 P4 174.13(16) . . ? C61 Pd4 S4 163.2(2) . . ? N10 Pd4 S4 82.43(18) . . ? P4 Pd4 S4 100.01(7) . . ? O1S C1S C3S 122.2(13) . . ? O1S C1S C2S 122.1(12) . . ? C3S C1S C2S 115.7(11) . . ? O2S C4S C6S 127.2(18) . . ? O2S C4S C5S 118.9(14) . . ? C6S C4S C5S 113.9(15) . . ? O3S C7S C9S 120.4(12) . . ? O3S C7S C8S 123.7(11) . . ? C9S C7S C8S 115.9(11) . . ? O4S C10S C11S 121.6(15) . . ? O4S C10S C12S 126.2(13) . . ? C11S C10S C12S 111.9(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.5(13) . . . . ? Pd1 C1 C2 C3 179.1(6) . . . . ? C1 C2 C3 C4 -0.5(14) . . . . ? C2 C3 C4 C5 0.1(15) . . . . ? C3 C4 C5 C6 0.3(16) . . . . ? C4 C5 C6 C1 -0.4(14) . . . . ? C4 C5 C6 C7 -177.0(9) . . . . ? C2 C1 C6 C5 0.0(13) . . . . ? Pd1 C1 C6 C5 -179.0(7) . . . . ? C2 C1 C6 C7 176.7(8) . . . . ? Pd1 C1 C6 C7 -2.2(10) . . . . ? C5 C6 C7 N1 177.1(8) . . . . ? C1 C6 C7 N1 0.5(12) . . . . ? C5 C6 C7 C9 0.5(15) . . . . ? C1 C6 C7 C9 -176.1(9) . . . . ? N1 C7 C9 C10 -80.9(13) . . . . ? C6 C7 C9 C10 95.4(13) . . . . ? C16 C11 C12 C13 -0.9(11) . . . . ? Pd2 C11 C12 C13 178.0(6) . . . . ? C11 C12 C13 C14 -0.1(13) . . . . ? C12 C13 C14 C15 0.7(14) . . . . ? C13 C14 C15 C16 -0.2(14) . . . . ? C14 C15 C16 C11 -0.9(12) . . . . ? C14 C15 C16 C17 -179.1(8) . . . . ? C12 C11 C16 C15 1.4(11) . . . . ? Pd2 C11 C16 C15 -177.8(6) . . . . ? C12 C11 C16 C17 179.7(7) . . . . ? Pd2 C11 C16 C17 0.5(8) . . . . ? C15 C16 C17 N4 -179.4(7) . . . . ? C11 C16 C17 N4 2.3(10) . . . . ? C15 C16 C17 C19 0.9(12) . . . . ? C11 C16 C17 C19 -177.3(7) . . . . ? N4 C17 C19 C20 97.7(10) . . . . ? C16 C17 C19 C20 -82.7(11) . . . . ? C27 C22 C23 C24 1.8(13) . . . . ? P2 C22 C23 C24 177.7(7) . . . . ? C22 C23 C24 C25 -1.8(17) . . . . ? C23 C24 C25 C26 1(2) . . . . ? C24 C25 C26 C27 0(2) . . . . ? C23 C22 C27 C26 -1.1(13) . . . . ? P2 C22 C27 C26 -177.2(8) . . . . ? C25 C26 C27 C22 0.4(18) . . . . ? C33 C28 C29 C30 -3.1(12) . . . . ? P2 C28 C29 C30 -179.6(6) . . . . ? C28 C29 C30 C31 2.3(13) . . . . ? C29 C30 C31 C32 0.3(14) . . . . ? C30 C31 C32 C33 -1.8(14) . . . . ? C31 C32 C33 C28 1.0(13) . . . . ? C29 C28 C33 C32 1.4(12) . . . . ? P2 C28 C33 C32 178.1(7) . . . . ? C39 C34 C35 C36 1.8(11) . . . . ? P1 C34 C35 C36 179.5(7) . . . . ? C34 C35 C36 C37 0.0(14) . . . . ? C35 C36 C37 C38 -2.6(15) . . . . ? C36 C37 C38 C39 3.4(15) . . . . ? C37 C38 C39 C34 -1.5(14) . . . . ? C35 C34 C39 C38 -1.1(11) . . . . ? P1 C34 C39 C38 -178.5(6) . . . . ? C45 C40 C41 C42 0.5(12) . . . . ? P1 C40 C41 C42 175.4(7) . . . . ? C40 C41 C42 C43 1.4(15) . . . . ? C41 C42 C43 C44 -1.8(17) . . . . ? C42 C43 C44 C45 0.2(16) . . . . ? C43 C44 C45 C40 1.7(13) . . . . ? C41 C40 C45 C44 -2.0(11) . . . . ? P1 C40 C45 C44 -176.7(6) . . . . ? C56 C51 C52 C53 1.5(12) . . . . ? Pd3 C51 C52 C53 -177.9(6) . . . . ? C51 C52 C53 C54 -0.9(14) . . . . ? C52 C53 C54 C55 0.3(14) . . . . ? C53 C54 C55 C56 -0.3(14) . . . . ? C54 C55 C56 C51 1.0(13) . . . . ? C54 C55 C56 C57 -179.3(8) . . . . ? C52 C51 C56 C55 -1.5(12) . . . . ? Pd3 C51 C56 C55 178.0(6) . . . . ? C52 C51 C56 C57 178.7(7) . . . . ? Pd3 C51 C56 C57 -1.8(9) . . . . ? C55 C56 C57 N7 -173.9(7) . . . . ? C51 C56 C57 N7 5.9(11) . . . . ? C55 C56 C57 C59 2.0(13) . . . . ? C51 C56 C57 C59 -178.2(7) . . . . ? N7 C57 C59 C60 74.9(10) . . . . ? C56 C57 C59 C60 -100.8(10) . . . . ? C66 C61 C62 C63 0.7(12) . . . . ? Pd4 C61 C62 C63 -175.3(6) . . . . ? C61 C62 C63 C64 -0.6(14) . . . . ? C62 C63 C64 C65 -0.1(14) . . . . ? C63 C64 C65 C66 0.5(13) . . . . ? C64 C65 C66 C61 -0.4(12) . . . . ? C64 C65 C66 C67 177.7(7) . . . . ? C62 C61 C66 C65 -0.3(11) . . . . ? Pd4 C61 C66 C65 176.6(6) . . . . ? C62 C61 C66 C67 -178.5(6) . . . . ? Pd4 C61 C66 C67 -1.6(8) . . . . ? C65 C66 C67 N10 -178.5(7) . . . . ? C61 C66 C67 N10 -0.3(9) . . . . ? C65 C66 C67 C69 0.2(11) . . . . ? C61 C66 C67 C69 178.4(6) . . . . ? N10 C67 C69 C70 -98.6(9) . . . . ? C66 C67 C69 C70 82.8(9) . . . . ? C77 C72 C73 C74 -2.2(13) . . . . ? P3 C72 C73 C74 -176.3(7) . . . . ? C72 C73 C74 C75 0.8(16) . . . . ? C73 C74 C75 C76 0.5(17) . . . . ? C74 C75 C76 C77 -0.2(17) . . . . ? C75 C76 C77 C72 -1.3(14) . . . . ? C73 C72 C77 C76 2.5(12) . . . . ? P3 C72 C77 C76 176.2(7) . . . . ? C83 C78 C79 C80 1.0(12) . . . . ? P3 C78 C79 C80 175.5(7) . . . . ? C78 C79 C80 C81 1.5(14) . . . . ? C79 C80 C81 C82 -2.8(16) . . . . ? C80 C81 C82 C83 1.5(15) . . . . ? C79 C78 C83 C82 -2.2(12) . . . . ? P3 C78 C83 C82 -177.2(6) . . . . ? C81 C82 C83 C78 1.1(13) . . . . ? C89 C84 C85 C86 -1.3(13) . . . . ? P4 C84 C85 C86 -177.2(7) . . . . ? C84 C85 C86 C87 0.1(16) . . . . ? C85 C86 C87 C88 1.1(19) . . . . ? C86 C87 C88 C89 -1.0(19) . . . . ? C85 C84 C89 C88 1.4(12) . . . . ? P4 C84 C89 C88 177.5(7) . . . . ? C87 C88 C89 C84 -0.2(16) . . . . ? C95 C90 C91 C92 1.8(11) . . . . ? P4 C90 C91 C92 178.7(6) . . . . ? C90 C91 C92 C93 -1.8(13) . . . . ? C91 C92 C93 C94 0.3(14) . . . . ? C92 C93 C94 C95 1.1(14) . . . . ? C91 C90 C95 C94 -0.4(12) . . . . ? P4 C90 C95 C94 -177.5(7) . . . . ? C93 C94 C95 C90 -1.0(13) . . . . ? C6 C7 N1 N2 -178.6(7) . . . . ? C9 C7 N1 N2 -1.9(13) . . . . ? C6 C7 N1 Pd1 1.6(10) . . . . ? C9 C7 N1 Pd1 178.3(8) . . . . ? N3 C8 N2 N1 -178.2(7) . . . . ? S1 C8 N2 N1 1.2(11) . . . . ? C7 N1 N2 C8 178.2(7) . . . . ? Pd1 N1 N2 C8 -2.0(9) . . . . ? C16 C17 N4 N5 -178.4(6) . . . . ? C19 C17 N4 N5 1.2(11) . . . . ? C16 C17 N4 Pd2 -4.0(9) . . . . ? C19 C17 N4 Pd2 175.6(6) . . . . ? N6 C18 N5 N4 -178.3(7) . . . . ? S2 C18 N5 N4 3.8(10) . . . . ? C17 N4 N5 C18 174.5(7) . . . . ? Pd2 N4 N5 C18 0.5(8) . . . . ? C56 C57 N7 N8 178.6(6) . . . . ? C59 C57 N7 N8 2.5(11) . . . . ? C56 C57 N7 Pd3 -7.2(9) . . . . ? C59 C57 N7 Pd3 176.7(6) . . . . ? N9 C58 N8 N7 178.4(6) . . . . ? S3 C58 N8 N7 -3.5(10) . . . . ? C57 N7 N8 C58 178.8(7) . . . . ? Pd3 N7 N8 C58 5.0(9) . . . . ? C66 C67 N10 N11 178.3(6) . . . . ? C69 C67 N10 N11 -0.5(10) . . . . ? C66 C67 N10 Pd4 2.2(8) . . . . ? C69 C67 N10 Pd4 -176.6(5) . . . . ? N12 C68 N11 N10 176.7(6) . . . . ? S4 C68 N11 N10 -4.3(9) . . . . ? C67 N10 N11 C68 -175.1(6) . . . . ? Pd4 N10 N11 C68 0.7(8) . . . . ? C35 C34 P1 C40 -177.7(6) . . . . ? C39 C34 P1 C40 -0.4(8) . . . . ? C35 C34 P1 C21 69.2(6) . . . . ? C39 C34 P1 C21 -113.5(7) . . . . ? C35 C34 P1 Pd1 -49.3(6) . . . . ? C39 C34 P1 Pd1 128.1(6) . . . . ? C41 C40 P1 C34 142.9(6) . . . . ? C45 C40 P1 C34 -42.4(7) . . . . ? C41 C40 P1 C21 -103.6(6) . . . . ? C45 C40 P1 C21 71.1(7) . . . . ? C41 C40 P1 Pd1 18.3(7) . . . . ? C45 C40 P1 Pd1 -167.1(5) . . . . ? P2 C21 P1 C34 59.9(6) . . . . ? P2 C21 P1 C40 -56.9(6) . . . . ? P2 C21 P1 Pd1 177.6(4) . . . . ? C27 C22 P2 C28 82.1(7) . . . . ? C23 C22 P2 C28 -93.7(7) . . . . ? C27 C22 P2 C21 -171.9(7) . . . . ? C23 C22 P2 C21 12.3(7) . . . . ? C27 C22 P2 Pd2 -43.1(7) . . . . ? C23 C22 P2 Pd2 141.2(6) . . . . ? C29 C28 P2 C22 76.4(8) . . . . ? C33 C28 P2 C22 -100.2(7) . . . . ? C29 C28 P2 C21 -34.7(8) . . . . ? C33 C28 P2 C21 148.7(6) . . . . ? C29 C28 P2 Pd2 -156.0(6) . . . . ? C33 C28 P2 Pd2 27.4(7) . . . . ? P1 C21 P2 C22 80.3(5) . . . . ? P1 C21 P2 C28 -175.1(5) . . . . ? P1 C21 P2 Pd2 -52.0(5) . . . . ? C73 C72 P3 C78 -145.2(6) . . . . ? C77 C72 P3 C78 41.1(7) . . . . ? C73 C72 P3 C71 101.7(7) . . . . ? C77 C72 P3 C71 -72.0(7) . . . . ? C73 C72 P3 Pd3 -17.9(7) . . . . ? C77 C72 P3 Pd3 168.4(6) . . . . ? C83 C78 P3 C72 179.8(6) . . . . ? C79 C78 P3 C72 5.4(8) . . . . ? C83 C78 P3 C71 -68.1(7) . . . . ? C79 C78 P3 C71 117.4(7) . . . . ? C83 C78 P3 Pd3 50.5(7) . . . . ? C79 C78 P3 Pd3 -123.9(6) . . . . ? P4 C71 P3 C72 57.5(5) . . . . ? P4 C71 P3 C78 -58.5(6) . . . . ? P4 C71 P3 Pd3 -178.8(4) . . . . ? C95 C90 P4 C84 98.5(7) . . . . ? C91 C90 P4 C84 -78.5(7) . . . . ? C95 C90 P4 C71 -150.5(6) . . . . ? C91 C90 P4 C71 32.5(7) . . . . ? C95 C90 P4 Pd4 -29.1(7) . . . . ? C91 C90 P4 Pd4 153.9(5) . . . . ? C89 C84 P4 C90 -85.0(6) . . . . ? C85 C84 P4 C90 90.9(7) . . . . ? C89 C84 P4 C71 169.1(6) . . . . ? C85 C84 P4 C71 -15.0(8) . . . . ? C89 C84 P4 Pd4 41.3(7) . . . . ? C85 C84 P4 Pd4 -142.8(6) . . . . ? P3 C71 P4 C90 175.9(5) . . . . ? P3 C71 P4 C84 -79.9(5) . . . . ? P3 C71 P4 Pd4 51.5(5) . . . . ? N2 C8 S1 Pd1 -0.1(8) . . . . ? N3 C8 S1 Pd1 179.3(6) . . . . ? N5 C18 S2 Pd2 -5.2(7) . . . . ? N6 C18 S2 Pd2 176.8(6) . . . . ? N8 C58 S3 Pd3 0.8(7) . . . . ? N9 C58 S3 Pd3 179.0(6) . . . . ? N11 C68 S4 Pd4 4.9(7) . . . . ? N12 C68 S4 Pd4 -176.0(5) . . . . ? C7 N1 Pd1 C1 -2.3(6) . . . . ? N2 N1 Pd1 C1 177.9(6) . . . . ? C7 N1 Pd1 P1 -31(7) . . . . ? N2 N1 Pd1 P1 149(6) . . . . ? C7 N1 Pd1 S1 -178.6(6) . . . . ? N2 N1 Pd1 S1 1.6(6) . . . . ? C2 C1 Pd1 N1 -176.5(9) . . . . ? C6 C1 Pd1 N1 2.3(6) . . . . ? C2 C1 Pd1 P1 2.7(9) . . . . ? C6 C1 Pd1 P1 -178.6(5) . . . . ? C2 C1 Pd1 S1 -163.7(6) . . . . ? C6 C1 Pd1 S1 15.1(12) . . . . ? C34 P1 Pd1 N1 -47(6) . . . . ? C40 P1 Pd1 N1 79(6) . . . . ? C21 P1 Pd1 N1 -162(6) . . . . ? C34 P1 Pd1 C1 -75.3(3) . . . . ? C40 P1 Pd1 C1 50.1(3) . . . . ? C21 P1 Pd1 C1 169.2(3) . . . . ? C34 P1 Pd1 S1 100.8(3) . . . . ? C40 P1 Pd1 S1 -133.8(3) . . . . ? C21 P1 Pd1 S1 -14.7(3) . . . . ? C8 S1 Pd1 N1 -0.7(3) . . . . ? C8 S1 Pd1 C1 -13.5(8) . . . . ? C8 S1 Pd1 P1 -179.7(3) . . . . ? C12 C11 Pd2 N4 179.1(8) . . . . ? C16 C11 Pd2 N4 -1.9(5) . . . . ? C12 C11 Pd2 P2 -5.1(8) . . . . ? C16 C11 Pd2 P2 173.9(5) . . . . ? C12 C11 Pd2 S2 177.4(5) . . . . ? C16 C11 Pd2 S2 -3.7(11) . . . . ? C17 N4 Pd2 C11 3.4(6) . . . . ? N5 N4 Pd2 C11 177.6(6) . . . . ? C17 N4 Pd2 P2 -55(2) . . . . ? N5 N4 Pd2 P2 119(2) . . . . ? C17 N4 Pd2 S2 -177.1(6) . . . . ? N5 N4 Pd2 S2 -2.9(5) . . . . ? C22 P2 Pd2 C11 169.0(4) . . . . ? C28 P2 Pd2 C11 51.4(3) . . . . ? C21 P2 Pd2 C11 -64.0(3) . . . . ? C22 P2 Pd2 N4 -133(2) . . . . ? C28 P2 Pd2 N4 109(2) . . . . ? C21 P2 Pd2 N4 -6(2) . . . . ? C22 P2 Pd2 S2 -11.7(3) . . . . ? C28 P2 Pd2 S2 -129.3(3) . . . . ? C21 P2 Pd2 S2 115.3(3) . . . . ? C18 S2 Pd2 C11 5.1(8) . . . . ? C18 S2 Pd2 N4 3.3(3) . . . . ? C18 S2 Pd2 P2 -172.4(3) . . . . ? C57 N7 Pd3 C51 5.0(6) . . . . ? N8 N7 Pd3 C51 178.9(6) . . . . ? C57 N7 Pd3 P3 -40(5) . . . . ? N8 N7 Pd3 P3 134(4) . . . . ? C57 N7 Pd3 S3 -177.6(6) . . . . ? N8 N7 Pd3 S3 -3.7(5) . . . . ? C52 C51 Pd3 N7 178.0(9) . . . . ? C56 C51 Pd3 N7 -1.5(5) . . . . ? C52 C51 Pd3 P3 -3.7(8) . . . . ? C56 C51 Pd3 P3 176.8(5) . . . . ? C52 C51 Pd3 S3 168.8(5) . . . . ? C56 C51 Pd3 S3 -10.7(12) . . . . ? C72 P3 Pd3 N7 -6(4) . . . . ? C78 P3 Pd3 N7 120(4) . . . . ? C71 P3 Pd3 N7 -123(4) . . . . ? C72 P3 Pd3 C51 -51.6(3) . . . . ? C78 P3 Pd3 C51 74.9(4) . . . . ? C71 P3 Pd3 C51 -168.4(3) . . . . ? C72 P3 Pd3 S3 130.6(3) . . . . ? C78 P3 Pd3 S3 -102.9(3) . . . . ? C71 P3 Pd3 S3 13.8(3) . . . . ? C58 S3 Pd3 N7 1.3(3) . . . . ? C58 S3 Pd3 C51 10.5(8) . . . . ? C58 S3 Pd3 P3 -177.0(3) . . . . ? C62 C61 Pd4 N10 178.2(8) . . . . ? C66 C61 Pd4 N10 2.1(5) . . . . ? C62 C61 Pd4 P4 3.6(8) . . . . ? C66 C61 Pd4 P4 -172.6(5) . . . . ? C62 C61 Pd4 S4 178.8(5) . . . . ? C66 C61 Pd4 S4 2.7(11) . . . . ? C67 N10 Pd4 C61 -2.5(5) . . . . ? N11 N10 Pd4 C61 -178.4(5) . . . . ? C67 N10 Pd4 P4 63(2) . . . . ? N11 N10 Pd4 P4 -113.2(17) . . . . ? C67 N10 Pd4 S4 177.7(5) . . . . ? N11 N10 Pd4 S4 1.8(5) . . . . ? C90 P4 Pd4 C61 -52.2(3) . . . . ? C84 P4 Pd4 C61 -169.9(4) . . . . ? C71 P4 Pd4 C61 63.9(3) . . . . ? C90 P4 Pd4 N10 -116.7(18) . . . . ? C84 P4 Pd4 N10 125.6(18) . . . . ? C71 P4 Pd4 N10 -0.6(18) . . . . ? C90 P4 Pd4 S4 129.2(3) . . . . ? C84 P4 Pd4 S4 11.5(3) . . . . ? C71 P4 Pd4 S4 -114.7(3) . . . . ? C68 S4 Pd4 C61 -3.4(8) . . . . ? C68 S4 Pd4 N10 -2.7(3) . . . . ? C68 S4 Pd4 P4 171.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B N11 0.90 2.60 3.389(8) 147.6 . N3 H3C O1S 0.90 2.17 3.064(11) 172.9 1_655 N6 H6A O4S 0.90 2.07 2.936(11) 160.1 1_554 N6 H6B S3 0.90 2.58 3.460(7) 166.1 1_554 N9 H9C N5 0.90 2.56 3.383(9) 151.6 1_556 N9 H9D O2S 0.90 2.09 2.970(11) 166.5 1_456 N12 H12B O3S 0.90 2.13 2.991(10) 159.1 . N12 H12C S1 0.90 2.53 3.413(6) 167.4 . _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.738 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.097