# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'R Van Eldik' _publ_contact_author_email VANELDIK@CHEMIE.UNI-ERLANGEN.DE _publ_section_title ; Is bis(trifluorosulfonyl)amide an innocent anion? X-ray structure data and DFT calculations ; loop_ _publ_author_name 'R Van Eldik' 'Frank W Heinemann' 'Peter Illner' 'Ralph Puchta' # Attachment '2a_publ.cif' data_pi0701 _database_code_depnum_ccdc_archive 'CCDC 708967' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H11 N4 O3 Pd, C2 F6 N O4 S2' _chemical_formula_sum 'C17 H11 F6 N5 O7 Pd S2' _chemical_formula_weight 681.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0079(8) _cell_length_b 9.6124(2) _cell_length_c 13.5373(9) _cell_angle_alpha 105.085(4) _cell_angle_beta 94.861(7) _cell_angle_gamma 96.944(4) _cell_volume 1115.18(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 152 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.031 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 2.00 \% and 120 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31846 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 28.70 _reflns_number_total 5746 _reflns_number_gt 5198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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^)+(0.0190P)^2^+0.8757P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5746 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_gt 0.0453 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.003 _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 0.936254(13) 0.909390(12) 0.076028(9) 0.00908(4) Uani 1 1 d . . . N1 N 0.89848(15) 1.08773(14) 0.18328(10) 0.0116(2) Uani 1 1 d . . . N2 N 1.12419(14) 0.94587(14) 0.16389(10) 0.0103(2) Uani 1 1 d . . . N3 N 1.03133(15) 0.74062(14) -0.00152(10) 0.0110(2) Uani 1 1 d . . . N4 N 0.62978(15) 0.80764(15) -0.01481(11) 0.0145(3) Uani 1 1 d . . . O1 O 0.75120(13) 0.88852(13) -0.02732(9) 0.0160(2) Uani 1 1 d . . . O2 O 0.63756(14) 0.74744(16) 0.05494(11) 0.0268(3) Uani 1 1 d . . . O3 O 0.51643(14) 0.79874(16) -0.07380(11) 0.0281(3) Uani 1 1 d . . . C1 C 0.77215(18) 1.14839(17) 0.18904(12) 0.0138(3) Uani 1 1 d . . . H1A H 0.6893 1.1081 0.1370 0.017 Uiso 1 1 calc R . . C2 C 0.75900(19) 1.26849(18) 0.26907(13) 0.0167(3) Uani 1 1 d . . . H2A H 0.6684 1.3100 0.2719 0.020 Uiso 1 1 calc R . . C3 C 0.8801(2) 1.32704(18) 0.34485(13) 0.0174(3) Uani 1 1 d . . . H3A H 0.8733 1.4093 0.4002 0.021 Uiso 1 1 calc R . . C4 C 1.01172(19) 1.26460(17) 0.33928(13) 0.0152(3) Uani 1 1 d . . . H4A H 1.0955 1.3036 0.3907 0.018 Uiso 1 1 calc R . . C5 C 1.01893(18) 1.14483(16) 0.25776(12) 0.0121(3) Uani 1 1 d . . . C6 C 1.15086(17) 1.06803(16) 0.24316(12) 0.0114(3) Uani 1 1 d . . . C7 C 1.29325(18) 1.10936(17) 0.29875(12) 0.0137(3) Uani 1 1 d . . . H7A H 1.3156 1.1958 0.3541 0.016 Uiso 1 1 calc R . . C8 C 1.40240(18) 1.02037(18) 0.27104(12) 0.0142(3) Uani 1 1 d . . . H8A H 1.5001 1.0463 0.3088 0.017 Uiso 1 1 calc R . . C9 C 1.37195(18) 0.89462(17) 0.18945(12) 0.0137(3) Uani 1 1 d . . . H9A H 1.4469 0.8340 0.1717 0.016 Uiso 1 1 calc R . . C10 C 1.22878(17) 0.85982(16) 0.13444(12) 0.0111(3) Uani 1 1 d . . . C11 C 1.17365(17) 0.73769(16) 0.04196(12) 0.0110(3) Uani 1 1 d . . . C12 C 1.25461(18) 0.62812(17) -0.00029(12) 0.0127(3) Uani 1 1 d . . . H12A H 1.3530 0.6265 0.0304 0.015 Uiso 1 1 calc R . . C13 C 1.18921(19) 0.51997(17) -0.08875(12) 0.0151(3) Uani 1 1 d . . . H13A H 1.2433 0.4443 -0.1195 0.018 Uiso 1 1 calc R . . C14 C 1.04515(19) 0.52351(17) -0.13143(12) 0.0148(3) Uani 1 1 d . . . H14A H 0.9993 0.4501 -0.1914 0.018 Uiso 1 1 calc R . . C15 C 0.96833(18) 0.63545(17) -0.08578(12) 0.0127(3) Uani 1 1 d . . . H15A H 0.8691 0.6376 -0.1148 0.015 Uiso 1 1 calc R . . N5 N 0.42543(16) 0.32535(15) 0.70213(11) 0.0155(3) Uani 1 1 d . . . S1 S 0.27332(4) 0.29766(4) 0.62801(3) 0.01488(8) Uani 1 1 d . . . O4 O 0.14728(15) 0.30915(17) 0.68534(11) 0.0317(3) Uani 1 1 d . . . O5 O 0.27595(15) 0.36104(13) 0.54317(10) 0.0231(3) Uani 1 1 d . . . S2 S 0.56851(5) 0.43690(4) 0.70111(3) 0.01443(8) Uani 1 1 d . . . O6 O 0.66820(15) 0.45226(14) 0.79273(10) 0.0227(3) Uani 1 1 d . . . O7 O 0.53877(15) 0.56502(13) 0.67269(10) 0.0221(3) Uani 1 1 d . . . C16 C 0.25988(18) 0.10144(17) 0.56908(13) 0.0150(3) Uani 1 1 d . . . F1 F 0.38356(11) 0.06946(11) 0.52686(8) 0.0211(2) Uani 1 1 d . . . F2 F 0.14327(11) 0.05790(11) 0.49539(8) 0.0220(2) Uani 1 1 d . . . F3 F 0.24015(13) 0.02632(12) 0.63790(9) 0.0296(3) Uani 1 1 d . . . C17 C 0.67235(19) 0.34200(18) 0.59880(13) 0.0173(3) Uani 1 1 d . . . F4 F 0.59546(12) 0.31242(12) 0.50607(8) 0.0252(2) Uani 1 1 d . . . F5 F 0.70539(13) 0.21799(11) 0.61486(9) 0.0257(2) Uani 1 1 d . . . F6 F 0.80175(12) 0.42686(12) 0.59984(9) 0.0267(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.00733(6) 0.01055(6) 0.00892(6) 0.00304(4) -0.00104(4) 0.00023(4) N1 0.0118(6) 0.0122(6) 0.0114(6) 0.0047(5) 0.0008(5) 0.0016(5) N2 0.0096(6) 0.0116(6) 0.0098(6) 0.0041(5) -0.0008(5) 0.0000(5) N3 0.0108(6) 0.0114(6) 0.0106(6) 0.0036(5) 0.0008(5) 0.0005(5) N4 0.0082(6) 0.0183(7) 0.0185(7) 0.0080(5) 0.0007(5) 0.0019(5) O1 0.0098(5) 0.0220(6) 0.0171(6) 0.0110(5) -0.0030(4) -0.0036(4) O2 0.0147(6) 0.0402(8) 0.0351(8) 0.0291(6) 0.0012(5) 0.0009(5) O3 0.0107(6) 0.0402(8) 0.0357(8) 0.0215(6) -0.0091(5) -0.0033(5) C1 0.0128(7) 0.0152(7) 0.0154(8) 0.0072(6) 0.0018(6) 0.0029(6) C2 0.0184(8) 0.0159(7) 0.0201(8) 0.0089(6) 0.0061(6) 0.0073(6) C3 0.0248(9) 0.0138(7) 0.0154(8) 0.0045(6) 0.0057(6) 0.0062(6) C4 0.0193(8) 0.0126(7) 0.0137(8) 0.0046(6) -0.0007(6) 0.0016(6) C5 0.0135(7) 0.0120(7) 0.0121(7) 0.0062(6) 0.0002(6) 0.0011(5) C6 0.0122(7) 0.0112(7) 0.0108(7) 0.0048(5) -0.0002(5) -0.0004(5) C7 0.0148(8) 0.0136(7) 0.0117(7) 0.0045(6) -0.0022(6) -0.0013(6) C8 0.0103(7) 0.0183(8) 0.0138(7) 0.0072(6) -0.0036(6) -0.0020(6) C9 0.0107(7) 0.0161(7) 0.0155(8) 0.0071(6) 0.0001(6) 0.0013(6) C10 0.0107(7) 0.0121(7) 0.0120(7) 0.0067(5) 0.0006(5) 0.0008(5) C11 0.0105(7) 0.0125(7) 0.0111(7) 0.0062(6) 0.0009(5) -0.0009(5) C12 0.0124(7) 0.0150(7) 0.0129(7) 0.0073(6) 0.0020(6) 0.0022(6) C13 0.0187(8) 0.0144(7) 0.0138(8) 0.0054(6) 0.0054(6) 0.0034(6) C14 0.0176(8) 0.0136(7) 0.0123(7) 0.0033(6) 0.0025(6) -0.0008(6) C15 0.0114(7) 0.0141(7) 0.0117(7) 0.0038(6) 0.0001(5) -0.0015(6) N5 0.0145(7) 0.0181(7) 0.0128(7) 0.0045(5) -0.0029(5) 0.0002(5) S1 0.01355(18) 0.01506(18) 0.01325(19) -0.00140(14) -0.00197(14) 0.00542(14) O4 0.0178(7) 0.0444(9) 0.0245(7) -0.0090(6) 0.0039(5) 0.0112(6) O5 0.0291(7) 0.0157(6) 0.0221(7) 0.0059(5) -0.0124(5) 0.0028(5) S2 0.01671(19) 0.01179(17) 0.01255(19) 0.00176(14) -0.00300(14) 0.00018(14) O6 0.0218(6) 0.0253(6) 0.0163(6) 0.0040(5) -0.0073(5) -0.0037(5) O7 0.0280(7) 0.0126(6) 0.0253(7) 0.0053(5) -0.0002(5) 0.0037(5) C16 0.0115(7) 0.0150(7) 0.0181(8) 0.0046(6) 0.0009(6) 0.0009(6) F1 0.0151(5) 0.0170(5) 0.0273(6) -0.0022(4) 0.0047(4) 0.0047(4) F2 0.0143(5) 0.0203(5) 0.0251(6) -0.0005(4) -0.0042(4) -0.0028(4) F3 0.0304(6) 0.0278(6) 0.0359(7) 0.0209(5) 0.0038(5) -0.0024(5) C17 0.0167(8) 0.0144(7) 0.0206(8) 0.0061(6) 0.0013(6) -0.0006(6) F4 0.0256(6) 0.0326(6) 0.0145(5) 0.0033(4) 0.0027(4) 0.0007(5) F5 0.0288(6) 0.0160(5) 0.0357(6) 0.0097(4) 0.0091(5) 0.0076(4) F6 0.0193(5) 0.0238(5) 0.0357(6) 0.0091(5) 0.0051(5) -0.0049(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 1.9240(13) . ? Pd1 N3 2.0172(13) . ? Pd1 N1 2.0229(13) . ? Pd1 O1 2.0381(11) . ? Pd1 Pd1 3.2208(3) 2_775 ? N1 C1 1.339(2) . ? N1 C5 1.370(2) . ? N2 C10 1.346(2) . ? N2 C6 1.3492(19) . ? N3 C15 1.3403(19) . ? N3 C11 1.371(2) . ? N4 O3 1.2218(18) . ? N4 O2 1.2306(18) . ? N4 O1 1.3128(17) . ? C1 C2 1.387(2) . ? C1 H1A 0.9500 . ? C2 C3 1.386(2) . ? C2 H2A 0.9500 . ? C3 C4 1.391(2) . ? C3 H3A 0.9500 . ? C4 C5 1.384(2) . ? C4 H4A 0.9500 . ? C5 C6 1.474(2) . ? C6 C7 1.388(2) . ? C7 C8 1.392(2) . ? C7 H7A 0.9500 . ? C8 C9 1.389(2) . ? C8 H8A 0.9500 . ? C9 C10 1.390(2) . ? C9 H9A 0.9500 . ? C10 C11 1.477(2) . ? C11 C12 1.382(2) . ? C12 C13 1.395(2) . ? C12 H12A 0.9500 . ? C13 C14 1.383(2) . ? C13 H13A 0.9500 . ? C14 C15 1.387(2) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? N5 S2 1.5772(14) . ? N5 S1 1.5795(14) . ? S1 O4 1.4278(14) . ? S1 O5 1.4339(13) . ? S1 C16 1.8314(17) . ? S2 O7 1.4302(13) . ? S2 O6 1.4319(13) . ? S2 C17 1.8422(18) . ? C16 F1 1.3272(19) . ? C16 F3 1.3297(19) . ? C16 F2 1.3314(18) . ? C17 F4 1.325(2) . ? C17 F5 1.3291(19) . ? C17 F6 1.3362(19) . ? 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 N2 Pd1 N3 81.25(5) . . ? N2 Pd1 N1 81.45(5) . . ? N3 Pd1 N1 162.67(5) . . ? N2 Pd1 O1 172.31(5) . . ? N3 Pd1 O1 98.84(5) . . ? N1 Pd1 O1 98.45(5) . . ? N2 Pd1 Pd1 94.35(4) . 2_775 ? N3 Pd1 Pd1 88.04(4) . 2_775 ? N1 Pd1 Pd1 94.40(4) . 2_775 ? O1 Pd1 Pd1 77.98(3) . 2_775 ? C1 N1 C5 119.77(14) . . ? C1 N1 Pd1 127.45(11) . . ? C5 N1 Pd1 112.75(10) . . ? C10 N2 C6 123.69(13) . . ? C10 N2 Pd1 117.98(10) . . ? C6 N2 Pd1 117.65(10) . . ? C15 N3 C11 119.92(14) . . ? C15 N3 Pd1 126.80(11) . . ? C11 N3 Pd1 113.26(10) . . ? O3 N4 O2 124.87(14) . . ? O3 N4 O1 116.82(13) . . ? O2 N4 O1 118.31(13) . . ? N4 O1 Pd1 116.15(9) . . ? N1 C1 C2 121.74(15) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C3 C2 C1 118.96(15) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C2 C3 C4 119.59(15) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 119.12(15) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? N1 C5 C4 120.82(15) . . ? N1 C5 C6 114.62(13) . . ? C4 C5 C6 124.56(14) . . ? N2 C6 C7 119.27(14) . . ? N2 C6 C5 113.04(13) . . ? C7 C6 C5 127.67(14) . . ? C6 C7 C8 118.05(14) . . ? C6 C7 H7A 121.0 . . ? C8 C7 H7A 121.0 . . ? C9 C8 C7 121.60(15) . . ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C8 C9 C10 118.20(15) . . ? C8 C9 H9A 120.9 . . ? C10 C9 H9A 120.9 . . ? N2 C10 C9 119.15(14) . . ? N2 C10 C11 113.05(13) . . ? C9 C10 C11 127.77(14) . . ? N3 C11 C12 121.01(14) . . ? N3 C11 C10 114.16(13) . . ? C12 C11 C10 124.83(14) . . ? C11 C12 C13 118.81(15) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C14 C13 C12 119.63(15) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 119.32(15) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? N3 C15 C14 121.30(15) . . ? N3 C15 H15A 119.4 . . ? C14 C15 H15A 119.4 . . ? S2 N5 S1 125.07(9) . . ? O4 S1 O5 118.27(9) . . ? O4 S1 N5 110.93(8) . . ? O5 S1 N5 116.42(8) . . ? O4 S1 C16 103.54(8) . . ? O5 S1 C16 104.75(8) . . ? N5 S1 C16 99.98(7) . . ? O7 S2 O6 118.91(8) . . ? O7 S2 N5 115.67(8) . . ? O6 S2 N5 107.50(8) . . ? O7 S2 C17 104.47(8) . . ? O6 S2 C17 102.60(8) . . ? N5 S2 C17 106.05(8) . . ? F1 C16 F3 108.07(13) . . ? F1 C16 F2 108.23(13) . . ? F3 C16 F2 108.41(13) . . ? F1 C16 S1 111.11(11) . . ? F3 C16 S1 111.54(12) . . ? F2 C16 S1 109.38(11) . . ? F4 C17 F5 108.49(14) . . ? F4 C17 F6 108.31(14) . . ? F5 C17 F6 107.95(14) . . ? F4 C17 S2 112.23(12) . . ? F5 C17 S2 110.86(12) . . ? F6 C17 S2 108.87(11) . . ? 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 N2 Pd1 N1 C1 -175.90(14) . . . . ? N3 Pd1 N1 C1 -172.08(15) . . . . ? O1 Pd1 N1 C1 11.87(14) . . . . ? Pd1 Pd1 N1 C1 90.35(13) 2_775 . . . ? N2 Pd1 N1 C5 2.07(10) . . . . ? N3 Pd1 N1 C5 5.9(2) . . . . ? O1 Pd1 N1 C5 -170.16(10) . . . . ? Pd1 Pd1 N1 C5 -91.68(10) 2_775 . . . ? N3 Pd1 N2 C10 4.46(11) . . . . ? N1 Pd1 N2 C10 -176.69(12) . . . . ? Pd1 Pd1 N2 C10 -82.88(11) 2_775 . . . ? N3 Pd1 N2 C6 175.38(12) . . . . ? N1 Pd1 N2 C6 -5.77(11) . . . . ? Pd1 Pd1 N2 C6 88.03(11) 2_775 . . . ? N2 Pd1 N3 C15 176.86(13) . . . . ? N1 Pd1 N3 C15 173.04(15) . . . . ? O1 Pd1 N3 C15 -10.92(13) . . . . ? Pd1 Pd1 N3 C15 -88.43(13) 2_775 . . . ? N2 Pd1 N3 C11 -1.46(10) . . . . ? N1 Pd1 N3 C11 -5.3(2) . . . . ? O1 Pd1 N3 C11 170.76(10) . . . . ? Pd1 Pd1 N3 C11 93.25(10) 2_775 . . . ? O3 N4 O1 Pd1 177.28(12) . . . . ? O2 N4 O1 Pd1 -2.33(19) . . . . ? N3 Pd1 O1 N4 91.43(11) . . . . ? N1 Pd1 O1 N4 -89.76(11) . . . . ? Pd1 Pd1 O1 N4 177.50(11) 2_775 . . . ? C5 N1 C1 C2 -0.1(2) . . . . ? Pd1 N1 C1 C2 177.72(12) . . . . ? N1 C1 C2 C3 0.1(2) . . . . ? C1 C2 C3 C4 0.0(2) . . . . ? C2 C3 C4 C5 0.0(2) . . . . ? C1 N1 C5 C4 0.1(2) . . . . ? Pd1 N1 C5 C4 -178.02(12) . . . . ? C1 N1 C5 C6 179.66(13) . . . . ? Pd1 N1 C5 C6 1.52(16) . . . . ? C3 C4 C5 N1 -0.1(2) . . . . ? C3 C4 C5 C6 -179.57(15) . . . . ? C10 N2 C6 C7 -0.1(2) . . . . ? Pd1 N2 C6 C7 -170.47(11) . . . . ? C10 N2 C6 C5 178.39(13) . . . . ? Pd1 N2 C6 C5 8.04(17) . . . . ? N1 C5 C6 N2 -6.04(19) . . . . ? C4 C5 C6 N2 173.48(14) . . . . ? N1 C5 C6 C7 172.33(15) . . . . ? C4 C5 C6 C7 -8.2(3) . . . . ? N2 C6 C7 C8 -1.2(2) . . . . ? C5 C6 C7 C8 -179.47(15) . . . . ? C6 C7 C8 C9 0.9(2) . . . . ? C7 C8 C9 C10 0.8(2) . . . . ? C6 N2 C10 C9 1.8(2) . . . . ? Pd1 N2 C10 C9 172.12(11) . . . . ? C6 N2 C10 C11 -176.65(13) . . . . ? Pd1 N2 C10 C11 -6.33(17) . . . . ? C8 C9 C10 N2 -2.1(2) . . . . ? C8 C9 C10 C11 176.13(15) . . . . ? C15 N3 C11 C12 0.6(2) . . . . ? Pd1 N3 C11 C12 179.01(11) . . . . ? C15 N3 C11 C10 -179.84(13) . . . . ? Pd1 N3 C11 C10 -1.39(16) . . . . ? N2 C10 C11 N3 4.87(19) . . . . ? C9 C10 C11 N3 -173.42(15) . . . . ? N2 C10 C11 C12 -175.55(14) . . . . ? C9 C10 C11 C12 6.2(2) . . . . ? N3 C11 C12 C13 0.2(2) . . . . ? C10 C11 C12 C13 -179.31(14) . . . . ? C11 C12 C13 C14 -0.7(2) . . . . ? C12 C13 C14 C15 0.4(2) . . . . ? C11 N3 C15 C14 -0.9(2) . . . . ? Pd1 N3 C15 C14 -179.10(11) . . . . ? C13 C14 C15 N3 0.4(2) . . . . ? S2 N5 S1 O4 -128.25(12) . . . . ? S2 N5 S1 O5 10.88(14) . . . . ? S2 N5 S1 C16 122.98(11) . . . . ? S1 N5 S2 O7 32.19(14) . . . . ? S1 N5 S2 O6 167.75(10) . . . . ? S1 N5 S2 C17 -83.06(12) . . . . ? O4 S1 C16 F1 -169.41(12) . . . . ? O5 S1 C16 F1 66.04(13) . . . . ? N5 S1 C16 F1 -54.86(13) . . . . ? O4 S1 C16 F3 -48.76(13) . . . . ? O5 S1 C16 F3 -173.31(11) . . . . ? N5 S1 C16 F3 65.79(13) . . . . ? O4 S1 C16 F2 71.16(13) . . . . ? O5 S1 C16 F2 -53.39(13) . . . . ? N5 S1 C16 F2 -174.29(11) . . . . ? O7 S2 C17 F4 -57.44(13) . . . . ? O6 S2 C17 F4 177.86(11) . . . . ? N5 S2 C17 F4 65.22(13) . . . . ? O7 S2 C17 F5 -178.93(11) . . . . ? O6 S2 C17 F5 56.37(13) . . . . ? N5 S2 C17 F5 -56.27(13) . . . . ? O7 S2 C17 F6 62.45(13) . . . . ? O6 S2 C17 F6 -62.25(13) . . . . ? N5 S2 C17 F6 -174.89(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.459 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.070 #===END OF DATA FOR 2a # 4.2 RESULTS FOR 2b data_pi0702 _database_code_depnum_ccdc_archive 'CCDC 708968' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H11 N4 O3 Pd, C2 F6 N O4 S2' _chemical_formula_sum 'C17 H11 F6 N5 O7 Pd S2' _chemical_formula_weight 681.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4578(5) _cell_length_b 8.9850(3) _cell_length_c 15.7908(12) _cell_angle_alpha 75.595(4) _cell_angle_beta 76.794(6) _cell_angle_gamma 74.882(4) _cell_volume 1104.74(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 128 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.839 _exptl_absorpt_correction_T_max 0.967 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \w-rotations with 2.00 \% and 180 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28358 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 28.50 _reflns_number_total 5586 _reflns_number_gt 4807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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^)+(0.0360P)^2^+0.1294P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5586 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.692931(19) 0.400298(18) 0.990728(11) 0.01393(5) Uani 1 1 d . . . N1 N 0.6110(2) 0.3140(2) 1.11973(13) 0.0191(4) Uani 1 1 d . . . N2 N 0.7531(2) 0.5451(2) 1.04271(12) 0.0146(3) Uani 1 1 d . . . N3 N 0.8022(2) 0.5296(2) 0.87864(12) 0.0158(4) Uani 1 1 d . . . N4 N 0.7014(2) 0.1364(2) 0.91575(13) 0.0201(4) Uani 1 1 d . . . O1 O 0.59710(19) 0.26013(18) 0.94195(11) 0.0233(3) Uani 1 1 d . . . O2 O 0.8508(2) 0.12499(19) 0.91165(14) 0.0330(4) Uani 1 1 d . . . O3 O 0.6427(2) 0.04029(19) 0.89762(12) 0.0301(4) Uani 1 1 d . . . C1 C 0.5438(3) 0.1861(3) 1.15313(17) 0.0250(5) Uani 1 1 d . . . H1A H 0.5303 0.1275 1.1138 0.030 Uiso 1 1 calc R . . C2 C 0.4944(3) 0.1389(3) 1.24318(18) 0.0316(6) Uani 1 1 d . . . H2A H 0.4479 0.0484 1.2657 0.038 Uiso 1 1 calc R . . C3 C 0.5129(3) 0.2242(3) 1.30022(18) 0.0335(6) Uani 1 1 d . . . H3A H 0.4786 0.1932 1.3624 0.040 Uiso 1 1 calc R . . C4 C 0.5822(3) 0.3562(3) 1.26637(16) 0.0262(5) Uani 1 1 d . . . H4A H 0.5956 0.4161 1.3050 0.031 Uiso 1 1 calc R . . C5 C 0.6313(2) 0.3984(3) 1.17562(15) 0.0186(4) Uani 1 1 d . . . C6 C 0.7085(2) 0.5339(2) 1.13145(14) 0.0169(4) Uani 1 1 d . . . C7 C 0.7386(3) 0.6431(3) 1.17014(15) 0.0210(5) Uani 1 1 d . . . H7A H 0.7066 0.6384 1.2323 0.025 Uiso 1 1 calc R . . C8 C 0.8168(3) 0.7603(3) 1.11621(16) 0.0217(5) Uani 1 1 d . . . H8A H 0.8406 0.8350 1.1421 0.026 Uiso 1 1 calc R . . C9 C 0.8606(3) 0.7702(3) 1.02513(15) 0.0193(4) Uani 1 1 d . . . H9A H 0.9145 0.8502 0.9886 0.023 Uiso 1 1 calc R . . C10 C 0.8241(2) 0.6607(2) 0.98880(14) 0.0151(4) Uani 1 1 d . . . C11 C 0.8562(2) 0.6498(2) 0.89439(14) 0.0156(4) Uani 1 1 d . . . C12 C 0.9327(3) 0.7500(3) 0.82523(15) 0.0193(4) Uani 1 1 d . . . H12A H 0.9659 0.8354 0.8365 0.023 Uiso 1 1 calc R . . C13 C 0.9605(3) 0.7251(3) 0.73959(15) 0.0225(5) Uani 1 1 d . . . H13A H 1.0136 0.7926 0.6916 0.027 Uiso 1 1 calc R . . C14 C 0.9100(3) 0.6005(3) 0.72443(15) 0.0232(5) Uani 1 1 d . . . H14A H 0.9307 0.5800 0.6662 0.028 Uiso 1 1 calc R . . C15 C 0.8289(3) 0.5063(2) 0.79530(15) 0.0189(4) Uani 1 1 d . . . H15A H 0.7912 0.4230 0.7847 0.023 Uiso 1 1 calc R . . N5 N 0.9255(2) 0.2882(2) 0.64485(13) 0.0232(4) Uani 1 1 d . . . S1 S 0.76548(6) 0.22198(6) 0.65346(4) 0.02066(12) Uani 1 1 d . . . O4 O 0.7913(2) 0.05838(19) 0.65425(13) 0.0299(4) Uani 1 1 d . . . O5 O 0.6354(2) 0.2884(2) 0.71781(13) 0.0393(5) Uani 1 1 d . . . S2 S 1.10424(7) 0.18676(7) 0.65402(4) 0.02211(12) Uani 1 1 d . . . O6 O 1.2025(2) 0.2889(3) 0.66058(14) 0.0410(5) Uani 1 1 d . . . O7 O 1.1114(2) 0.0394(2) 0.71497(13) 0.0428(5) Uani 1 1 d . . . C16 C 0.7015(3) 0.3234(3) 0.54767(19) 0.0332(6) Uani 1 1 d . . . F1 F 0.8219(2) 0.2978(2) 0.47934(11) 0.0488(5) Uani 1 1 d . . . F2 F 0.5741(2) 0.2714(2) 0.53872(14) 0.0589(6) Uani 1 1 d . . . F3 F 0.6545(2) 0.47689(19) 0.54384(14) 0.0576(5) Uani 1 1 d . . . C17 C 1.1940(3) 0.1353(3) 0.54581(17) 0.0278(5) Uani 1 1 d . . . F4 F 1.1853(2) 0.2602(2) 0.48169(11) 0.0518(5) Uani 1 1 d . . . F5 F 1.35377(18) 0.0664(2) 0.54403(12) 0.0444(4) Uani 1 1 d . . . F6 F 1.1176(2) 0.0378(2) 0.53020(14) 0.0597(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01342(8) 0.01268(8) 0.01662(9) -0.00369(6) -0.00310(6) -0.00328(5) N1 0.0138(8) 0.0194(9) 0.0220(10) -0.0021(8) -0.0016(7) -0.0033(7) N2 0.0123(8) 0.0151(8) 0.0166(9) -0.0053(7) -0.0024(7) -0.0011(7) N3 0.0151(8) 0.0143(8) 0.0172(9) -0.0035(7) -0.0031(7) -0.0011(7) N4 0.0234(9) 0.0145(9) 0.0231(10) -0.0031(7) -0.0043(8) -0.0057(7) O1 0.0172(7) 0.0210(8) 0.0357(10) -0.0138(7) -0.0061(7) -0.0019(6) O2 0.0173(8) 0.0227(9) 0.0598(13) -0.0139(8) -0.0026(8) -0.0040(7) O3 0.0362(10) 0.0229(8) 0.0393(11) -0.0123(8) -0.0098(8) -0.0120(7) C1 0.0162(10) 0.0192(11) 0.0367(14) 0.0009(10) -0.0042(10) -0.0051(9) C2 0.0208(11) 0.0265(12) 0.0378(15) 0.0084(11) 0.0008(10) -0.0079(10) C3 0.0232(12) 0.0365(14) 0.0260(13) 0.0086(11) 0.0044(10) -0.0029(11) C4 0.0215(11) 0.0324(13) 0.0193(11) -0.0017(10) -0.0015(9) -0.0014(10) C5 0.0122(9) 0.0210(10) 0.0201(11) -0.0025(9) -0.0020(8) -0.0015(8) C6 0.0112(9) 0.0199(10) 0.0175(10) -0.0031(8) -0.0025(8) -0.0006(8) C7 0.0164(10) 0.0288(12) 0.0195(11) -0.0111(9) -0.0046(8) -0.0010(9) C8 0.0203(10) 0.0240(11) 0.0257(12) -0.0116(9) -0.0082(9) -0.0034(9) C9 0.0170(10) 0.0171(10) 0.0252(11) -0.0048(9) -0.0050(9) -0.0044(8) C10 0.0119(9) 0.0158(9) 0.0173(10) -0.0040(8) -0.0033(8) -0.0014(7) C11 0.0137(9) 0.0145(9) 0.0178(10) -0.0040(8) -0.0036(8) -0.0004(8) C12 0.0174(10) 0.0158(10) 0.0227(11) -0.0026(9) -0.0021(9) -0.0025(8) C13 0.0218(11) 0.0178(10) 0.0208(11) 0.0014(9) -0.0001(9) -0.0002(9) C14 0.0278(12) 0.0216(11) 0.0153(11) -0.0039(9) -0.0031(9) 0.0026(9) C15 0.0219(10) 0.0163(10) 0.0195(11) -0.0065(8) -0.0068(9) -0.0002(8) N5 0.0207(9) 0.0228(10) 0.0284(11) -0.0106(8) -0.0035(8) -0.0038(8) S1 0.0162(2) 0.0198(3) 0.0237(3) -0.0039(2) -0.0001(2) -0.0034(2) O4 0.0234(8) 0.0204(8) 0.0426(11) -0.0012(7) -0.0012(8) -0.0079(7) O5 0.0247(9) 0.0473(12) 0.0400(11) -0.0175(9) 0.0074(8) -0.0008(8) S2 0.0179(3) 0.0330(3) 0.0168(3) -0.0091(2) -0.0027(2) -0.0043(2) O6 0.0314(10) 0.0604(13) 0.0470(12) -0.0333(10) -0.0080(9) -0.0150(9) O7 0.0259(9) 0.0510(12) 0.0363(11) 0.0123(9) -0.0045(8) -0.0031(9) C16 0.0315(13) 0.0305(13) 0.0395(15) 0.0012(11) -0.0167(12) -0.0088(11) F1 0.0534(11) 0.0678(12) 0.0249(8) -0.0003(8) -0.0114(8) -0.0170(9) F2 0.0452(10) 0.0648(13) 0.0768(14) 0.0019(11) -0.0377(10) -0.0211(9) F3 0.0652(12) 0.0267(9) 0.0735(14) 0.0083(9) -0.0310(11) 0.0019(8) C17 0.0209(11) 0.0393(14) 0.0278(13) -0.0181(11) 0.0035(10) -0.0102(10) F4 0.0466(10) 0.0764(13) 0.0205(8) 0.0015(8) 0.0027(7) -0.0111(9) F5 0.0201(7) 0.0581(11) 0.0508(11) -0.0219(9) 0.0062(7) -0.0017(7) F6 0.0435(10) 0.0856(14) 0.0741(14) -0.0667(12) 0.0178(9) -0.0317(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 1.9218(18) . ? Pd1 N1 2.0200(19) . ? Pd1 N3 2.0314(18) . ? Pd1 O1 2.0339(16) . ? N1 C1 1.351(3) . ? N1 C5 1.362(3) . ? N2 C10 1.348(3) . ? N2 C6 1.351(3) . ? N3 C15 1.343(3) . ? N3 C11 1.371(3) . ? N4 O3 1.218(2) . ? N4 O2 1.229(2) . ? N4 O1 1.318(2) . ? C1 C2 1.377(4) . ? C1 H1A 0.9500 . ? C2 C3 1.376(4) . ? C2 H2A 0.9500 . ? C3 C4 1.393(4) . ? C3 H3A 0.9500 . ? C4 C5 1.382(3) . ? C4 H4A 0.9500 . ? C5 C6 1.476(3) . ? C6 C7 1.379(3) . ? C7 C8 1.390(3) . ? C7 H7A 0.9500 . ? C8 C9 1.387(3) . ? C8 H8A 0.9500 . ? C9 C10 1.383(3) . ? C9 H9A 0.9500 . ? C10 C11 1.476(3) . ? C11 C12 1.383(3) . ? C12 C13 1.383(3) . ? C12 H12A 0.9500 . ? C13 C14 1.386(3) . ? C13 H13A 0.9500 . ? C14 C15 1.386(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? N5 S2 1.5663(19) . ? N5 S1 1.5807(19) . ? S1 O4 1.4259(17) . ? S1 O5 1.4309(19) . ? S1 C16 1.820(3) . ? S2 O6 1.4242(19) . ? S2 O7 1.4259(19) . ? S2 C17 1.824(3) . ? C16 F3 1.322(3) . ? C16 F1 1.324(3) . ? C16 F2 1.329(3) . ? C17 F4 1.310(3) . ? C17 F6 1.311(3) . ? C17 F5 1.328(3) . ? 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 N2 Pd1 N1 81.40(8) . . ? N2 Pd1 N3 80.73(7) . . ? N1 Pd1 N3 162.03(7) . . ? N2 Pd1 O1 172.30(7) . . ? N1 Pd1 O1 95.36(7) . . ? N3 Pd1 O1 102.60(7) . . ? C1 N1 C5 119.8(2) . . ? C1 N1 Pd1 127.21(17) . . ? C5 N1 Pd1 112.97(14) . . ? C10 N2 C6 123.06(19) . . ? C10 N2 Pd1 118.87(15) . . ? C6 N2 Pd1 117.81(14) . . ? C15 N3 C11 119.36(18) . . ? C15 N3 Pd1 127.35(15) . . ? C11 N3 Pd1 113.26(14) . . ? O3 N4 O2 124.4(2) . . ? O3 N4 O1 117.60(18) . . ? O2 N4 O1 118.02(18) . . ? N4 O1 Pd1 116.94(12) . . ? N1 C1 C2 121.3(3) . . ? N1 C1 H1A 119.4 . . ? C2 C1 H1A 119.4 . . ? C3 C2 C1 119.4(2) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 119.7(2) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C5 C4 C3 118.9(2) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? N1 C5 C4 120.9(2) . . ? N1 C5 C6 114.82(19) . . ? C4 C5 C6 124.3(2) . . ? N2 C6 C7 119.4(2) . . ? N2 C6 C5 112.79(19) . . ? C7 C6 C5 127.8(2) . . ? C6 C7 C8 118.5(2) . . ? C6 C7 H7A 120.7 . . ? C8 C7 H7A 120.7 . . ? C9 C8 C7 121.1(2) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C10 C9 C8 118.4(2) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? N2 C10 C9 119.4(2) . . ? N2 C10 C11 112.66(18) . . ? C9 C10 C11 127.9(2) . . ? N3 C11 C12 120.8(2) . . ? N3 C11 C10 114.35(18) . . ? C12 C11 C10 124.9(2) . . ? C13 C12 C11 119.5(2) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C12 C13 C14 119.4(2) . . ? C12 C13 H13A 120.3 . . ? C14 C13 H13A 120.3 . . ? C15 C14 C13 119.1(2) . . ? C15 C14 H14A 120.5 . . ? C13 C14 H14A 120.5 . . ? N3 C15 C14 121.8(2) . . ? N3 C15 H15A 119.1 . . ? C14 C15 H15A 119.1 . . ? S2 N5 S1 125.77(13) . . ? O4 S1 O5 118.45(12) . . ? O4 S1 N5 116.81(10) . . ? O5 S1 N5 109.44(12) . . ? O4 S1 C16 105.43(12) . . ? O5 S1 C16 103.94(13) . . ? N5 S1 C16 100.06(11) . . ? O6 S2 O7 118.43(13) . . ? O6 S2 N5 107.57(11) . . ? O7 S2 N5 115.73(11) . . ? O6 S2 C17 103.30(12) . . ? O7 S2 C17 104.70(13) . . ? N5 S2 C17 105.52(11) . . ? F3 C16 F1 108.3(2) . . ? F3 C16 F2 108.6(2) . . ? F1 C16 F2 107.5(2) . . ? F3 C16 S1 110.9(2) . . ? F1 C16 S1 112.25(17) . . ? F2 C16 S1 109.17(18) . . ? F4 C17 F6 108.8(2) . . ? F4 C17 F5 107.5(2) . . ? F6 C17 F5 108.6(2) . . ? F4 C17 S2 111.56(18) . . ? F6 C17 S2 110.82(17) . . ? F5 C17 S2 109.49(17) . . ? 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 N2 Pd1 N1 C1 -176.89(18) . . . . ? N3 Pd1 N1 C1 -170.87(19) . . . . ? O1 Pd1 N1 C1 10.15(18) . . . . ? N2 Pd1 N1 C5 2.24(14) . . . . ? N3 Pd1 N1 C5 8.3(3) . . . . ? O1 Pd1 N1 C5 -170.72(14) . . . . ? N1 Pd1 N2 C10 -178.57(16) . . . . ? N3 Pd1 N2 C10 3.31(15) . . . . ? N1 Pd1 N2 C6 -4.21(14) . . . . ? N3 Pd1 N2 C6 177.67(15) . . . . ? N2 Pd1 N3 C15 176.43(18) . . . . ? N1 Pd1 N3 C15 170.40(19) . . . . ? O1 Pd1 N3 C15 -10.64(18) . . . . ? N2 Pd1 N3 C11 -1.64(13) . . . . ? N1 Pd1 N3 C11 -7.7(3) . . . . ? O1 Pd1 N3 C11 171.29(13) . . . . ? O3 N4 O1 Pd1 170.42(15) . . . . ? O2 N4 O1 Pd1 -9.2(3) . . . . ? N1 Pd1 O1 N4 -101.34(15) . . . . ? N3 Pd1 O1 N4 78.99(15) . . . . ? C5 N1 C1 C2 0.2(3) . . . . ? Pd1 N1 C1 C2 179.29(16) . . . . ? N1 C1 C2 C3 0.4(3) . . . . ? C1 C2 C3 C4 -0.4(4) . . . . ? C2 C3 C4 C5 -0.1(3) . . . . ? C1 N1 C5 C4 -0.8(3) . . . . ? Pd1 N1 C5 C4 -179.95(16) . . . . ? C1 N1 C5 C6 179.02(18) . . . . ? Pd1 N1 C5 C6 -0.2(2) . . . . ? C3 C4 C5 N1 0.7(3) . . . . ? C3 C4 C5 C6 -179.1(2) . . . . ? C10 N2 C6 C7 -1.1(3) . . . . ? Pd1 N2 C6 C7 -175.23(15) . . . . ? C10 N2 C6 C5 179.27(17) . . . . ? Pd1 N2 C6 C5 5.2(2) . . . . ? N1 C5 C6 N2 -3.1(3) . . . . ? C4 C5 C6 N2 176.68(19) . . . . ? N1 C5 C6 C7 177.3(2) . . . . ? C4 C5 C6 C7 -2.9(3) . . . . ? N2 C6 C7 C8 -1.0(3) . . . . ? C5 C6 C7 C8 178.5(2) . . . . ? C6 C7 C8 C9 1.4(3) . . . . ? C7 C8 C9 C10 0.3(3) . . . . ? C6 N2 C10 C9 2.9(3) . . . . ? Pd1 N2 C10 C9 176.91(14) . . . . ? C6 N2 C10 C11 -178.21(16) . . . . ? Pd1 N2 C10 C11 -4.2(2) . . . . ? C8 C9 C10 N2 -2.4(3) . . . . ? C8 C9 C10 C11 178.89(19) . . . . ? C15 N3 C11 C12 2.1(3) . . . . ? Pd1 N3 C11 C12 -179.63(15) . . . . ? C15 N3 C11 C10 -178.28(17) . . . . ? Pd1 N3 C11 C10 0.0(2) . . . . ? N2 C10 C11 N3 2.6(2) . . . . ? C9 C10 C11 N3 -178.61(19) . . . . ? N2 C10 C11 C12 -177.86(19) . . . . ? C9 C10 C11 C12 1.0(3) . . . . ? N3 C11 C12 C13 -2.4(3) . . . . ? C10 C11 C12 C13 178.06(19) . . . . ? C11 C12 C13 C14 0.5(3) . . . . ? C12 C13 C14 C15 1.7(3) . . . . ? C11 N3 C15 C14 0.1(3) . . . . ? Pd1 N3 C15 C14 -177.89(15) . . . . ? C13 C14 C15 N3 -2.0(3) . . . . ? S2 N5 S1 O4 -11.5(2) . . . . ? S2 N5 S1 O5 126.56(16) . . . . ? S2 N5 S1 C16 -124.65(17) . . . . ? S1 N5 S2 O6 -167.91(15) . . . . ? S1 N5 S2 O7 -32.9(2) . . . . ? S1 N5 S2 C17 82.31(18) . . . . ? O4 S1 C16 F3 172.41(18) . . . . ? O5 S1 C16 F3 47.1(2) . . . . ? N5 S1 C16 F3 -66.0(2) . . . . ? O4 S1 C16 F1 -66.3(2) . . . . ? O5 S1 C16 F1 168.40(19) . . . . ? N5 S1 C16 F1 55.3(2) . . . . ? O4 S1 C16 F2 52.8(2) . . . . ? O5 S1 C16 F2 -72.4(2) . . . . ? N5 S1 C16 F2 174.5(2) . . . . ? O6 S2 C17 F4 -59.7(2) . . . . ? O7 S2 C17 F4 175.66(17) . . . . ? N5 S2 C17 F4 53.1(2) . . . . ? O6 S2 C17 F6 178.91(19) . . . . ? O7 S2 C17 F6 54.3(2) . . . . ? N5 S2 C17 F6 -68.3(2) . . . . ? O6 S2 C17 F5 59.1(2) . . . . ? O7 S2 C17 F5 -65.5(2) . . . . ? N5 S2 C17 F5 171.88(17) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.525 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.101 #===END OF DATA FOR 2b # 4.3 RESULTS FOR 3 data_pi0703 _database_code_depnum_ccdc_archive 'CCDC 708969' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H13 N3 O Pd, 2(C2 F6 N O4 S2)' _chemical_formula_sum 'C19 H13 F12 N5 O9 Pd S4' _chemical_formula_weight 917.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4959(8) _cell_length_b 12.5011(5) _cell_length_c 15.1571(9) _cell_angle_alpha 78.007(5) _cell_angle_beta 82.377(6) _cell_angle_gamma 78.266(4) _cell_volume 1534.88(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 238 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.986 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.749 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \w-rotations with 2.00 \% and 48 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37261 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.88 _reflns_number_total 7299 _reflns_number_gt 6173 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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^)+(0.0246P)^2^+0.9670P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7299 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.716064(18) 0.585259(12) 0.714679(10) 0.01810(5) Uani 1 1 d . . . O1 O 0.66477(18) 0.65644(12) 0.58350(9) 0.0271(3) Uani 1 1 d . . . H1B H 0.5640 0.6566 0.5729 0.041 Uiso 1 1 d . . . H1C H 0.6913 0.7197 0.5614 0.041 Uiso 1 1 d . . . N1 N 0.6178(2) 0.70996(13) 0.78375(11) 0.0219(3) Uani 1 1 d . . . N2 N 0.7699(2) 0.51074(13) 0.83357(11) 0.0210(3) Uani 1 1 d . . . N3 N 0.8347(2) 0.43893(13) 0.68392(11) 0.0205(3) Uani 1 1 d . . . C1 C 0.5411(3) 0.81266(17) 0.75134(15) 0.0268(4) Uani 1 1 d . . . H1A H 0.5286 0.8335 0.6884 0.032 Uiso 1 1 calc R . . C2 C 0.4798(3) 0.88922(18) 0.80688(16) 0.0336(5) Uani 1 1 d . . . H2A H 0.4261 0.9615 0.7822 0.040 Uiso 1 1 calc R . . C3 C 0.4971(3) 0.85992(19) 0.89814(16) 0.0355(5) Uani 1 1 d . . . H3A H 0.4564 0.9119 0.9370 0.043 Uiso 1 1 calc R . . C4 C 0.5746(3) 0.75368(19) 0.93264(15) 0.0332(5) Uani 1 1 d . . . H4A H 0.5864 0.7316 0.9956 0.040 Uiso 1 1 calc R . . C5 C 0.6346(3) 0.68030(17) 0.87446(14) 0.0256(4) Uani 1 1 d . . . C6 C 0.7215(3) 0.56556(18) 0.90254(14) 0.0284(5) Uani 1 1 d . . . C7 C 0.7553(4) 0.5122(2) 0.98920(16) 0.0476(7) Uani 1 1 d . . . H7A H 0.7237 0.5494 1.0391 0.057 Uiso 1 1 calc R . . C8 C 0.8370(4) 0.4025(2) 1.00132(16) 0.0539(8) Uani 1 1 d . . . H8A H 0.8611 0.3645 1.0604 0.065 Uiso 1 1 calc R . . C9 C 0.8838(3) 0.3478(2) 0.92905(15) 0.0394(6) Uani 1 1 d . . . H9A H 0.9390 0.2728 0.9380 0.047 Uiso 1 1 calc R . . C10 C 0.8485(2) 0.40473(16) 0.84340(13) 0.0239(4) Uani 1 1 d . . . C11 C 0.8874(2) 0.36375(16) 0.75755(13) 0.0223(4) Uani 1 1 d . . . C12 C 0.9723(3) 0.25911(17) 0.74952(15) 0.0289(5) Uani 1 1 d . . . H12A H 1.0081 0.2073 0.8014 0.035 Uiso 1 1 calc R . . C13 C 1.0044(3) 0.23115(18) 0.66419(15) 0.0312(5) Uani 1 1 d . . . H13A H 1.0624 0.1596 0.6569 0.037 Uiso 1 1 calc R . . C14 C 0.9514(3) 0.30796(18) 0.59012(15) 0.0289(5) Uani 1 1 d . . . H14A H 0.9731 0.2900 0.5313 0.035 Uiso 1 1 calc R . . C15 C 0.8665(3) 0.41142(17) 0.60206(14) 0.0250(4) Uani 1 1 d . . . H15A H 0.8300 0.4642 0.5508 0.030 Uiso 1 1 calc R . . N4 N 0.4090(2) 0.49753(15) 0.70334(12) 0.0293(4) Uani 1 1 d . . . S1 S 0.28026(7) 0.56403(5) 0.63661(4) 0.03311(13) Uani 1 1 d . . . O2 O 0.3650(2) 0.62605(16) 0.56124(11) 0.0451(4) Uani 1 1 d . . . O3 O 0.1639(2) 0.50629(15) 0.61785(11) 0.0413(4) Uani 1 1 d . . . S2 S 0.38019(7) 0.39418(4) 0.77991(3) 0.02701(11) Uani 1 1 d . . . O4 O 0.4951(2) 0.38059(13) 0.84420(10) 0.0337(4) Uani 1 1 d . . . O5 O 0.21537(19) 0.39020(13) 0.81284(10) 0.0343(4) Uani 1 1 d . . . C16 C 0.1607(3) 0.6721(2) 0.69591(18) 0.0419(6) Uani 1 1 d . . . F1 F 0.08550(19) 0.62811(13) 0.77355(10) 0.0486(4) Uani 1 1 d . . . F2 F 0.2526(2) 0.73657(14) 0.71434(14) 0.0677(5) Uani 1 1 d . . . F3 F 0.0496(2) 0.73467(14) 0.64462(12) 0.0612(5) Uani 1 1 d . . . C17 C 0.4490(3) 0.2741(2) 0.72305(18) 0.0416(6) Uani 1 1 d . . . F4 F 0.3691(2) 0.28292(15) 0.65212(12) 0.0636(5) Uani 1 1 d . . . F5 F 0.60420(18) 0.26428(14) 0.69619(12) 0.0580(5) Uani 1 1 d . . . F6 F 0.4244(3) 0.18326(13) 0.78084(14) 0.0749(6) Uani 1 1 d . . . N5 N 0.4906(4) 0.9424(3) 0.5378(2) 0.0235(7) Uani 0.50 1 d P . . S3 S 0.66851(7) 0.97183(5) 0.48587(4) 0.03184(13) Uani 1 1 d . . . O6 O 0.7706(4) 0.8585(2) 0.5108(2) 0.0302(7) Uani 0.50 1 d P A 1 O7 O 0.6645(4) 1.0187(3) 0.3966(2) 0.0315(7) Uani 0.50 1 d P . 1 O6' O 0.6711(5) 0.8710(2) 0.5324(3) 0.0374(8) Uani 0.50 1 d P B 2 O7' O 0.7877(4) 0.9966(3) 0.4045(2) 0.0386(8) Uani 0.50 1 d P C 2 C18 C 0.7348(3) 1.0504(2) 0.5589(2) 0.0440(6) Uani 1 1 d . . . F8 F 0.6420(5) 1.0496(4) 0.6372(3) 0.0420(10) Uani 0.50 1 d P B 1 F7 F 0.7674(6) 1.1481(3) 0.5295(2) 0.0590(10) Uani 0.50 1 d P B 1 F9 F 0.8856(4) 0.9879(3) 0.5918(2) 0.0636(10) Uani 0.50 1 d P B 1 F8' F 0.7275(7) 1.0108(5) 0.6369(3) 0.0728(16) Uani 0.50 1 d P B 2 F7' F 0.6151(5) 1.1500(3) 0.5450(3) 0.0609(9) Uani 0.50 1 d P B 2 F9' F 0.8614(5) 1.0799(4) 0.5166(3) 0.0645(11) Uani 0.50 1 d P B 2 N6 N 0.0101(5) -0.0547(3) 0.0361(3) 0.0382(9) Uani 0.50 1 d P . . S4 S 0.13104(8) 0.01640(5) 0.03952(5) 0.04837(17) Uani 1 1 d . . . O8 O 0.2678(5) -0.0519(3) 0.0876(3) 0.0592(12) Uani 0.50 1 d P D 1 O9 O 0.1527(5) 0.1124(3) -0.0199(2) 0.0393(9) Uani 0.50 1 d P . 1 O8' O 0.1779(4) -0.1043(3) 0.0548(2) 0.0398(8) Uani 0.50 1 d P E 2 O9' O 0.2561(7) 0.0770(4) -0.0063(3) 0.0591(12) Uani 0.50 1 d P F 2 C19 C 0.0333(4) 0.0737(3) 0.1395(2) 0.0550(7) Uani 1 1 d . . . F10 F 0.0009(8) 0.1716(3) 0.1182(3) 0.0799(14) Uani 0.50 1 d P E 1 F11 F -0.0848(4) 0.0163(3) 0.1677(2) 0.0572(9) Uani 0.50 1 d P E 1 F12 F 0.1498(5) 0.0332(3) 0.1933(2) 0.0663(10) Uani 0.50 1 d P E 1 F10' F -0.1132(4) 0.1498(3) 0.1225(2) 0.0469(8) Uani 0.50 1 d P E 2 F11' F -0.0091(6) 0.0097(3) 0.2168(2) 0.0655(11) Uani 0.50 1 d P E 2 F12' F 0.1136(4) 0.1463(3) 0.1705(3) 0.0573(9) Uani 0.50 1 d P E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02282(8) 0.01723(7) 0.01473(7) -0.00339(5) -0.00231(5) -0.00398(5) O1 0.0353(9) 0.0251(7) 0.0201(7) 0.0000(6) -0.0061(6) -0.0058(6) N1 0.0244(9) 0.0209(8) 0.0211(8) -0.0047(7) -0.0017(7) -0.0051(7) N2 0.0242(9) 0.0222(8) 0.0174(8) -0.0056(6) -0.0025(6) -0.0038(7) N3 0.0222(9) 0.0215(8) 0.0196(8) -0.0063(6) -0.0012(6) -0.0058(7) C1 0.0304(12) 0.0216(10) 0.0272(11) -0.0032(8) -0.0024(9) -0.0033(8) C2 0.0364(13) 0.0202(10) 0.0410(13) -0.0058(9) 0.0011(10) -0.0005(9) C3 0.0405(14) 0.0295(12) 0.0374(13) -0.0159(10) 0.0030(10) -0.0029(10) C4 0.0440(14) 0.0315(12) 0.0240(11) -0.0122(9) 0.0006(9) -0.0018(10) C5 0.0312(11) 0.0233(10) 0.0228(10) -0.0071(8) -0.0016(8) -0.0039(8) C6 0.0349(12) 0.0283(11) 0.0213(10) -0.0073(8) -0.0044(9) -0.0005(9) C7 0.076(2) 0.0408(14) 0.0183(11) -0.0115(10) -0.0075(11) 0.0138(13) C8 0.087(2) 0.0440(15) 0.0187(11) -0.0030(10) -0.0121(12) 0.0179(14) C9 0.0549(16) 0.0312(12) 0.0245(11) -0.0036(9) -0.0078(11) 0.0106(11) C10 0.0263(11) 0.0235(10) 0.0208(10) -0.0041(8) -0.0033(8) -0.0015(8) C11 0.0227(10) 0.0233(10) 0.0212(9) -0.0052(8) -0.0017(8) -0.0038(8) C12 0.0308(12) 0.0238(10) 0.0302(11) -0.0063(9) -0.0039(9) 0.0013(9) C13 0.0298(12) 0.0266(11) 0.0380(12) -0.0150(10) 0.0001(10) -0.0001(9) C14 0.0297(12) 0.0349(12) 0.0259(11) -0.0158(9) 0.0014(9) -0.0069(9) C15 0.0273(11) 0.0293(11) 0.0210(10) -0.0082(8) -0.0018(8) -0.0078(8) N4 0.0341(10) 0.0366(10) 0.0212(9) -0.0026(8) -0.0039(7) -0.0171(8) S1 0.0349(3) 0.0458(3) 0.0224(3) -0.0010(2) -0.0074(2) -0.0183(3) O2 0.0454(11) 0.0619(12) 0.0278(8) 0.0100(8) -0.0096(8) -0.0244(9) O3 0.0406(10) 0.0632(11) 0.0288(8) -0.0091(8) -0.0091(7) -0.0254(9) S2 0.0321(3) 0.0307(3) 0.0210(2) -0.0068(2) 0.0016(2) -0.0128(2) O4 0.0404(9) 0.0366(9) 0.0249(8) -0.0032(7) -0.0054(7) -0.0096(7) O5 0.0354(9) 0.0417(9) 0.0283(8) -0.0088(7) 0.0056(7) -0.0158(7) C16 0.0403(14) 0.0440(14) 0.0440(14) -0.0023(12) -0.0125(12) -0.0141(12) F1 0.0558(10) 0.0516(9) 0.0373(8) -0.0121(7) -0.0008(7) -0.0056(7) F2 0.0586(11) 0.0536(10) 0.1048(15) -0.0314(10) -0.0161(10) -0.0197(8) F3 0.0551(11) 0.0614(11) 0.0584(10) 0.0036(8) -0.0197(8) 0.0035(8) C17 0.0400(14) 0.0414(14) 0.0494(15) -0.0211(12) 0.0085(12) -0.0166(11) F4 0.0572(10) 0.0804(12) 0.0718(12) -0.0543(10) -0.0058(9) -0.0147(9) F5 0.0392(9) 0.0647(10) 0.0814(12) -0.0459(10) 0.0129(8) -0.0141(8) F6 0.0973(15) 0.0336(9) 0.0926(14) -0.0174(9) 0.0227(12) -0.0239(9) N5 0.0239(18) 0.0205(17) 0.0234(17) 0.0001(13) -0.0016(14) -0.0026(14) S3 0.0303(3) 0.0341(3) 0.0257(3) -0.0088(2) -0.0019(2) 0.0093(2) O6 0.0245(18) 0.0197(16) 0.0420(19) -0.0011(13) -0.0030(15) 0.0015(14) O7 0.0337(19) 0.0311(17) 0.0256(16) 0.0004(13) 0.0024(14) -0.0059(14) O6' 0.043(2) 0.0144(15) 0.047(2) -0.0002(14) -0.0013(18) 0.0040(15) O7' 0.036(2) 0.0376(18) 0.0352(18) -0.0094(15) 0.0129(15) 0.0015(15) C18 0.0465(16) 0.0357(14) 0.0513(17) -0.0127(12) 0.0097(13) -0.0156(12) F8 0.046(2) 0.053(2) 0.0342(18) -0.0198(18) 0.0040(18) -0.0178(17) F7 0.090(3) 0.052(2) 0.0480(19) 0.0011(16) -0.013(2) -0.049(2) F9 0.0330(18) 0.095(3) 0.059(2) -0.013(2) -0.0220(16) 0.0072(17) F8' 0.118(5) 0.080(4) 0.038(2) -0.003(2) -0.029(3) -0.052(3) F7' 0.066(2) 0.0378(17) 0.090(3) -0.0381(18) -0.018(2) -0.0013(16) F9' 0.044(2) 0.073(3) 0.094(3) -0.038(2) 0.007(2) -0.0347(19) N6 0.060(3) 0.0227(19) 0.031(2) -0.0055(16) -0.0084(19) -0.0030(18) S4 0.0388(4) 0.0344(3) 0.0658(5) -0.0011(3) -0.0041(3) -0.0015(3) O8 0.056(3) 0.065(3) 0.048(2) -0.021(2) -0.0228(19) 0.032(2) O9 0.032(2) 0.044(2) 0.037(2) -0.0020(16) 0.0036(17) -0.0060(17) O8' 0.0352(19) 0.0354(18) 0.048(2) -0.0128(16) -0.0071(16) 0.0035(15) O9' 0.077(3) 0.062(3) 0.050(3) -0.019(2) 0.008(2) -0.039(3) C19 0.0580(19) 0.058(2) 0.0458(16) 0.0074(14) -0.0137(14) -0.0156(15) F10 0.149(5) 0.038(2) 0.046(2) -0.0210(17) -0.016(3) 0.016(3) F11 0.050(2) 0.075(2) 0.0402(19) -0.0182(18) 0.0054(16) 0.0059(18) F12 0.074(3) 0.091(3) 0.0363(18) -0.0205(18) -0.0201(18) -0.003(2) F10' 0.0344(17) 0.055(2) 0.0507(19) -0.0245(16) -0.0006(15) 0.0055(15) F11' 0.119(4) 0.0418(19) 0.0313(18) -0.0083(15) 0.013(2) -0.016(2) F12' 0.0490(19) 0.065(2) 0.070(2) -0.0413(19) 0.0022(17) -0.0149(17) _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 N2 1.9164(16) . ? Pd1 N3 2.0147(16) . ? Pd1 N1 2.0348(16) . ? Pd1 O1 2.0668(14) . ? O1 H1B 0.8913 . ? O1 H1C 0.8549 . ? N1 C1 1.340(3) . ? N1 C5 1.366(3) . ? N2 C6 1.342(3) . ? N2 C10 1.345(3) . ? N3 C15 1.335(2) . ? N3 C11 1.362(3) . ? C1 C2 1.383(3) . ? C1 H1A 0.9500 . ? C2 C3 1.375(3) . ? C2 H2A 0.9500 . ? C3 C4 1.385(3) . ? C3 H3A 0.9500 . ? C4 C5 1.380(3) . ? C4 H4A 0.9500 . ? C5 C6 1.477(3) . ? C6 C7 1.382(3) . ? C7 C8 1.392(3) . ? C7 H7A 0.9500 . ? C8 C9 1.382(3) . ? C8 H8A 0.9500 . ? C9 C10 1.384(3) . ? C9 H9A 0.9500 . ? C10 C11 1.469(3) . ? C11 C12 1.380(3) . ? C12 C13 1.387(3) . ? C12 H12A 0.9500 . ? C13 C14 1.377(3) . ? C13 H13A 0.9500 . ? C14 C15 1.382(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? N4 S1 1.5761(19) . ? N4 S2 1.5830(18) . ? S1 O3 1.4246(16) . ? S1 O2 1.4372(17) . ? S1 C16 1.835(3) . ? S2 O5 1.4300(16) . ? S2 O4 1.4307(16) . ? S2 C17 1.840(2) . ? C16 F2 1.321(3) . ? C16 F3 1.323(3) . ? C16 F1 1.331(3) . ? C17 F5 1.316(3) . ? C17 F6 1.317(3) . ? C17 F4 1.320(3) . ? N5 S3 1.577(3) 2_676 ? N5 O7 1.599(5) 2_676 ? N5 O6' 1.610(5) . ? N5 N5 1.665(6) 2_676 ? N5 S3 1.682(3) . ? S3 O6' 1.307(3) . ? S3 O7 1.360(3) . ? S3 O6 1.506(3) . ? S3 O7' 1.510(3) . ? S3 N5 1.577(3) 2_676 ? S3 C18 1.830(3) . ? O7 N5 1.599(5) 2_676 ? C18 F8' 1.182(5) . ? C18 F9' 1.258(4) . ? C18 F7 1.283(4) . ? C18 F8 1.334(5) . ? C18 F7' 1.436(4) . ? C18 F9 1.450(4) . ? N6 O8' 1.474(5) . ? N6 S4 1.502(4) . ? N6 N6 1.559(7) 2 ? N6 S4 1.697(4) 2 ? N6 O9 1.749(6) 2 ? S4 O9 1.372(4) . ? S4 O9' 1.449(4) . ? S4 O8' 1.457(3) . ? S4 O8 1.474(4) . ? S4 N6 1.697(4) 2 ? S4 C19 1.837(3) . ? O9 N6 1.749(6) 2 ? C19 F10 1.183(4) . ? C19 F12 1.318(4) . ? C19 F11' 1.325(4) . ? C19 F11 1.325(5) . ? C19 F10' 1.422(4) . ? C19 F12' 1.423(4) . ? 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 N2 Pd1 N3 81.33(7) . . ? N2 Pd1 N1 81.14(7) . . ? N3 Pd1 N1 162.44(6) . . ? N2 Pd1 O1 176.35(6) . . ? N3 Pd1 O1 95.03(6) . . ? N1 Pd1 O1 102.50(6) . . ? Pd1 O1 H1B 113.8 . . ? Pd1 O1 H1C 117.4 . . ? H1B O1 H1C 110.6 . . ? C1 N1 C5 118.78(17) . . ? C1 N1 Pd1 128.31(14) . . ? C5 N1 Pd1 112.91(13) . . ? C6 N2 C10 123.85(17) . . ? C6 N2 Pd1 118.28(14) . . ? C10 N2 Pd1 117.81(13) . . ? C15 N3 C11 119.47(17) . . ? C15 N3 Pd1 127.35(14) . . ? C11 N3 Pd1 113.16(12) . . ? N1 C1 C2 121.9(2) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C3 C2 C1 119.5(2) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C4 119.1(2) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 119.3(2) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? N1 C5 C4 121.39(19) . . ? N1 C5 C6 114.13(17) . . ? C4 C5 C6 124.48(19) . . ? N2 C6 C7 119.18(19) . . ? N2 C6 C5 113.51(18) . . ? C7 C6 C5 127.31(19) . . ? C6 C7 C8 118.2(2) . . ? C6 C7 H7A 120.9 . . ? C8 C7 H7A 120.9 . . ? C9 C8 C7 121.3(2) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C8 C9 C10 118.5(2) . . ? C8 C9 H9A 120.7 . . ? C10 C9 H9A 120.7 . . ? N2 C10 C9 118.95(18) . . ? N2 C10 C11 113.28(17) . . ? C9 C10 C11 127.77(19) . . ? N3 C11 C12 121.40(18) . . ? N3 C11 C10 114.36(17) . . ? C12 C11 C10 124.23(18) . . ? C11 C12 C13 118.7(2) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C14 C13 C12 119.46(19) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C13 C14 C15 119.44(19) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? N3 C15 C14 121.52(19) . . ? N3 C15 H15A 119.2 . . ? C14 C15 H15A 119.2 . . ? S1 N4 S2 124.08(12) . . ? O3 S1 O2 117.96(10) . . ? O3 S1 N4 117.55(10) . . ? O2 S1 N4 107.23(10) . . ? O3 S1 C16 104.25(11) . . ? O2 S1 C16 103.36(12) . . ? N4 S1 C16 104.61(11) . . ? O5 S2 O4 118.54(10) . . ? O5 S2 N4 115.61(10) . . ? O4 S2 N4 107.47(9) . . ? O5 S2 C17 105.45(10) . . ? O4 S2 C17 104.10(11) . . ? N4 S2 C17 103.99(11) . . ? F2 C16 F3 108.5(2) . . ? F2 C16 F1 108.0(2) . . ? F3 C16 F1 107.8(2) . . ? F2 C16 S1 111.28(19) . . ? F3 C16 S1 109.65(18) . . ? F1 C16 S1 111.51(18) . . ? F5 C17 F6 108.6(2) . . ? F5 C17 F4 108.7(2) . . ? F6 C17 F4 108.4(2) . . ? F5 C17 S2 110.72(16) . . ? F6 C17 S2 108.73(18) . . ? F4 C17 S2 111.60(19) . . ? S3 N5 O7 50.71(15) 2_676 2_676 ? S3 N5 O6' 163.2(3) 2_676 . ? O7 N5 O6' 145.5(3) 2_676 . ? S3 N5 N5 62.4(2) 2_676 2_676 ? O7 N5 N5 103.3(3) 2_676 2_676 ? O6' N5 N5 102.4(3) . 2_676 ? S3 N5 S3 118.64(19) 2_676 . ? O7 N5 S3 145.3(2) 2_676 . ? O6' N5 S3 46.73(16) . . ? N5 N5 S3 56.20(19) 2_676 . ? O6' S3 O7 134.6(2) . . ? O7 S3 O6 118.3(2) . . ? O6' S3 O7' 121.7(2) . . ? O6 S3 O7' 89.20(19) . . ? O6' S3 N5 124.2(2) . 2_676 ? O7 S3 N5 65.49(19) . 2_676 ? O6 S3 N5 156.00(19) . 2_676 ? O7' S3 N5 104.18(18) . 2_676 ? O6' S3 N5 63.7(2) . . ? O7 S3 N5 114.23(19) . . ? O6 S3 N5 98.33(18) . . ? O7' S3 N5 154.24(19) . . ? N5 S3 N5 61.4(2) 2_676 . ? O6' S3 C18 106.41(19) . . ? O7 S3 C18 116.97(16) . . ? O6 S3 C18 101.86(16) . . ? O7' S3 C18 97.83(17) . . ? N5 S3 C18 96.03(15) 2_676 . ? N5 S3 C18 104.58(14) . . ? S3 O7 N5 63.80(17) . 2_676 ? S3 O6' N5 69.52(19) . . ? F8' C18 F9' 122.1(4) . . ? F8' C18 F7 121.8(4) . . ? F9' C18 F7 50.0(2) . . ? F9' C18 F8 143.2(3) . . ? F7 C18 F8 109.2(3) . . ? F8' C18 F7' 108.7(4) . . ? F9' C18 F7' 103.8(3) . . ? F7 C18 F7' 55.8(3) . . ? F8 C18 F7' 74.5(3) . . ? F8' C18 F9 64.7(4) . . ? F9' C18 F9 64.0(3) . . ? F7 C18 F9 102.6(3) . . ? F8 C18 F9 99.9(3) . . ? F7' C18 F9 151.8(3) . . ? F8' C18 S3 115.3(3) . . ? F9' C18 S3 104.6(2) . . ? F7 C18 S3 122.3(2) . . ? F8 C18 S3 112.0(3) . . ? F7' C18 S3 99.6(2) . . ? F9 C18 S3 108.0(2) . . ? O8' N6 S4 58.6(2) . . ? O8' N6 N6 115.1(5) . 2 ? S4 N6 N6 67.3(3) . 2 ? O8' N6 S4 148.3(3) . 2 ? S4 N6 S4 122.1(2) . 2 ? N6 N6 S4 54.7(3) 2 2 ? O8' N6 O9 132.4(3) . 2 ? S4 N6 O9 168.2(3) . 2 ? N6 N6 O9 101.5(4) 2 2 ? S4 N6 O9 46.89(17) 2 2 ? O9 S4 O8' 143.5(2) . . ? O9' S4 O8' 115.1(3) . . ? O9 S4 O8 119.5(3) . . ? O9' S4 O8 81.6(3) . . ? O8' S4 O8 52.8(2) . . ? O9 S4 N6 126.2(2) . . ? O9' S4 N6 149.4(2) . . ? O8' S4 N6 59.7(2) . . ? O8 S4 N6 109.5(2) . . ? O9 S4 N6 68.5(2) . 2 ? O9' S4 N6 101.7(3) . 2 ? O8' S4 N6 108.25(19) . 2 ? O8 S4 N6 158.8(2) . 2 ? N6 S4 N6 57.9(2) . 2 ? O9 S4 C19 100.39(19) . . ? O9' S4 C19 110.7(2) . . ? O8' S4 C19 115.04(17) . . ? O8 S4 C19 93.48(18) . . ? N6 S4 C19 97.31(19) . . ? N6 S4 C19 104.63(17) 2 . ? S4 O9 N6 64.6(2) . 2 ? S4 O8' N6 61.6(2) . . ? F10 C19 F12 117.1(4) . . ? F10 C19 F11' 128.5(4) . . ? F12 C19 F11' 65.2(3) . . ? F10 C19 F11 119.2(4) . . ? F12 C19 F11 108.1(3) . . ? F11' C19 F11 45.5(2) . . ? F10 C19 F10' 46.4(3) . . ? F12 C19 F10' 147.6(3) . . ? F11' C19 F10' 101.9(3) . . ? F11 C19 F10' 73.7(3) . . ? F10 C19 F12' 57.6(3) . . ? F12 C19 F12' 59.6(3) . . ? F11' C19 F12' 101.4(3) . . ? F11 C19 F12' 139.5(3) . . ? F10' C19 F12' 97.4(3) . . ? F10 C19 S4 108.4(3) . . ? F12 C19 S4 98.3(3) . . ? F11' C19 S4 122.4(3) . . ? F11 C19 S4 102.6(3) . . ? F10' C19 S4 113.0(2) . . ? F12' C19 S4 116.9(2) . . ? 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 N2 Pd1 N1 C1 179.31(18) . . . . ? N3 Pd1 N1 C1 175.70(19) . . . . ? O1 Pd1 N1 C1 -0.77(18) . . . . ? N2 Pd1 N1 C5 -1.19(14) . . . . ? N3 Pd1 N1 C5 -4.8(3) . . . . ? O1 Pd1 N1 C5 178.73(14) . . . . ? N3 Pd1 N2 C6 -179.55(17) . . . . ? N1 Pd1 N2 C6 1.56(16) . . . . ? N3 Pd1 N2 C10 -2.23(15) . . . . ? N1 Pd1 N2 C10 178.87(16) . . . . ? N2 Pd1 N3 C15 -177.49(18) . . . . ? N1 Pd1 N3 C15 -173.88(19) . . . . ? O1 Pd1 N3 C15 2.66(17) . . . . ? N2 Pd1 N3 C11 1.40(13) . . . . ? N1 Pd1 N3 C11 5.0(3) . . . . ? O1 Pd1 N3 C11 -178.45(13) . . . . ? C5 N1 C1 C2 0.4(3) . . . . ? Pd1 N1 C1 C2 179.87(16) . . . . ? N1 C1 C2 C3 -0.1(4) . . . . ? C1 C2 C3 C4 -0.6(4) . . . . ? C2 C3 C4 C5 0.9(4) . . . . ? C1 N1 C5 C4 0.0(3) . . . . ? Pd1 N1 C5 C4 -179.58(17) . . . . ? C1 N1 C5 C6 -179.74(19) . . . . ? Pd1 N1 C5 C6 0.7(2) . . . . ? C3 C4 C5 N1 -0.6(3) . . . . ? C3 C4 C5 C6 179.1(2) . . . . ? C10 N2 C6 C7 1.1(3) . . . . ? Pd1 N2 C6 C7 178.3(2) . . . . ? C10 N2 C6 C5 -178.72(19) . . . . ? Pd1 N2 C6 C5 -1.6(2) . . . . ? N1 C5 C6 N2 0.5(3) . . . . ? C4 C5 C6 N2 -179.2(2) . . . . ? N1 C5 C6 C7 -179.3(2) . . . . ? C4 C5 C6 C7 1.0(4) . . . . ? N2 C6 C7 C8 -0.8(4) . . . . ? C5 C6 C7 C8 179.0(3) . . . . ? C6 C7 C8 C9 0.1(5) . . . . ? C7 C8 C9 C10 0.3(5) . . . . ? C6 N2 C10 C9 -0.6(3) . . . . ? Pd1 N2 C10 C9 -177.77(18) . . . . ? C6 N2 C10 C11 179.71(19) . . . . ? Pd1 N2 C10 C11 2.6(2) . . . . ? C8 C9 C10 N2 -0.1(4) . . . . ? C8 C9 C10 C11 179.5(3) . . . . ? C15 N3 C11 C12 -0.5(3) . . . . ? Pd1 N3 C11 C12 -179.48(16) . . . . ? C15 N3 C11 C10 178.52(18) . . . . ? Pd1 N3 C11 C10 -0.5(2) . . . . ? N2 C10 C11 N3 -1.3(3) . . . . ? C9 C10 C11 N3 179.1(2) . . . . ? N2 C10 C11 C12 177.71(19) . . . . ? C9 C10 C11 C12 -1.9(4) . . . . ? N3 C11 C12 C13 0.3(3) . . . . ? C10 C11 C12 C13 -178.6(2) . . . . ? C11 C12 C13 C14 0.1(3) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C11 N3 C15 C14 0.3(3) . . . . ? Pd1 N3 C15 C14 179.12(15) . . . . ? C13 C14 C15 N3 0.1(3) . . . . ? S2 N4 S1 O3 -26.38(19) . . . . ? S2 N4 S1 O2 -162.05(14) . . . . ? S2 N4 S1 C16 88.63(16) . . . . ? S1 N4 S2 O5 -25.65(18) . . . . ? S1 N4 S2 O4 -160.58(13) . . . . ? S1 N4 S2 C17 89.44(16) . . . . ? O3 S1 C16 F2 -177.11(18) . . . . ? O2 S1 C16 F2 -53.2(2) . . . . ? N4 S1 C16 F2 58.9(2) . . . . ? O3 S1 C16 F3 -57.1(2) . . . . ? O2 S1 C16 F3 66.81(19) . . . . ? N4 S1 C16 F3 178.93(17) . . . . ? O3 S1 C16 F1 62.28(19) . . . . ? O2 S1 C16 F1 -173.84(16) . . . . ? N4 S1 C16 F1 -61.73(19) . . . . ? O5 S2 C17 F5 -174.94(18) . . . . ? O4 S2 C17 F5 -49.5(2) . . . . ? N4 S2 C17 F5 63.0(2) . . . . ? O5 S2 C17 F6 -55.7(2) . . . . ? O4 S2 C17 F6 69.8(2) . . . . ? N4 S2 C17 F6 -177.74(18) . . . . ? O5 S2 C17 F4 63.8(2) . . . . ? O4 S2 C17 F4 -170.72(17) . . . . ? N4 S2 C17 F4 -58.3(2) . . . . ? S3 N5 S3 O6' -169.7(3) 2_676 . . . ? O7 N5 S3 O6' 128.9(5) 2_676 . . . ? N5 N5 S3 O6' -169.7(3) 2_676 . . . ? S3 N5 S3 O7 -40.2(3) 2_676 . . . ? O7 N5 S3 O7 -101.6(4) 2_676 . . . ? O6' N5 S3 O7 129.5(2) . . . . ? N5 N5 S3 O7 -40.2(3) 2_676 . . . ? S3 N5 S3 O6 -166.4(2) 2_676 . . . ? O7 N5 S3 O6 132.2(4) 2_676 . . . ? O6' N5 S3 O6 3.3(3) . . . . ? N5 N5 S3 O6 -166.4(2) 2_676 . . . ? S3 N5 S3 O7' -60.7(5) 2_676 . . . ? O7 N5 S3 O7' -122.1(5) 2_676 . . . ? O6' N5 S3 O7' 109.0(4) . . . . ? N5 N5 S3 O7' -60.7(5) 2_676 . . . ? S3 N5 S3 N5 0.0 2_676 . . 2_676 ? O7 N5 S3 N5 -61.4(4) 2_676 . . 2_676 ? O6' N5 S3 N5 169.7(3) . . . 2_676 ? S3 N5 S3 C18 88.9(2) 2_676 . . . ? O7 N5 S3 C18 27.5(5) 2_676 . . . ? O6' N5 S3 C18 -101.4(2) . . . . ? N5 N5 S3 C18 88.9(2) 2_676 . . . ? O6' S3 O7 N5 114.7(3) . . . 2_676 ? O6 S3 O7 N5 153.5(2) . . . 2_676 ? O7' S3 O7 N5 -154.6(3) . . . 2_676 ? N5 S3 O7 N5 38.5(3) . . . 2_676 ? C18 S3 O7 N5 -84.1(2) . . . 2_676 ? O7 S3 O6' N5 -99.0(3) . . . . ? O6 S3 O6' N5 -174.3(4) . . . . ? O7' S3 O6' N5 -151.1(2) . . . . ? N5 S3 O6' N5 -11.0(3) 2_676 . . . ? C18 S3 O6' N5 98.47(18) . . . . ? S3 N5 O6' S3 32.9(10) 2_676 . . . ? O7 N5 O6' S3 -128.5(5) 2_676 . . . ? N5 N5 O6' S3 8.8(3) 2_676 . . . ? O6' S3 C18 F8' -18.4(4) . . . . ? O7 S3 C18 F8' 175.5(4) . . . . ? O6 S3 C18 F8' -53.9(4) . . . . ? O7' S3 C18 F8' -144.7(4) . . . . ? N5 S3 C18 F8' 110.0(4) 2_676 . . . ? N5 S3 C18 F8' 48.1(4) . . . . ? O6' S3 C18 F9' 118.5(3) . . . . ? O7 S3 C18 F9' -47.6(3) . . . . ? O6 S3 C18 F9' 83.0(3) . . . . ? O7' S3 C18 F9' -7.9(3) . . . . ? N5 S3 C18 F9' -113.1(3) 2_676 . . . ? N5 S3 C18 F9' -175.1(3) . . . . ? O6' S3 C18 F7 170.1(4) . . . . ? O7 S3 C18 F7 4.0(4) . . . . ? O6 S3 C18 F7 134.6(4) . . . . ? O7' S3 C18 F7 43.7(4) . . . . ? N5 S3 C18 F7 -61.5(4) 2_676 . . . ? N5 S3 C18 F7 -123.4(4) . . . . ? O6' S3 C18 F8 -57.4(3) . . . . ? O7 S3 C18 F8 136.5(3) . . . . ? O6 S3 C18 F8 -92.9(3) . . . . ? O7' S3 C18 F8 176.2(3) . . . . ? N5 S3 C18 F8 71.0(3) 2_676 . . . ? N5 S3 C18 F8 9.0(3) . . . . ? O6' S3 C18 F7' -134.4(3) . . . . ? O7 S3 C18 F7' 59.4(3) . . . . ? O6 S3 C18 F7' -170.0(2) . . . . ? O7' S3 C18 F7' 99.2(2) . . . . ? N5 S3 C18 F7' -6.1(2) 2_676 . . . ? N5 S3 C18 F7' -68.0(2) . . . . ? O6' S3 C18 F9 51.6(3) . . . . ? O7 S3 C18 F9 -114.5(3) . . . . ? O6 S3 C18 F9 16.0(3) . . . . ? O7' S3 C18 F9 -74.8(3) . . . . ? N5 S3 C18 F9 180.0(3) 2_676 . . . ? N5 S3 C18 F9 118.0(2) . . . . ? O8' N6 S4 O9 136.6(3) . . . . ? N6 N6 S4 O9 -5.9(4) 2 . . . ? S4 N6 S4 O9 -5.9(4) 2 . . . ? O9 N6 S4 O9 -24.6(17) 2 . . . ? O8' N6 S4 O9' 88.7(5) . . . . ? N6 N6 S4 O9' -53.8(6) 2 . . . ? S4 N6 S4 O9' -53.8(6) 2 . . . ? O9 N6 S4 O9' -72.4(17) 2 . . . ? N6 N6 S4 O8' -142.5(4) 2 . . . ? S4 N6 S4 O8' -142.5(4) 2 . . . ? O8' N6 S4 O8 -18.5(3) . . . . ? N6 N6 S4 O8 -160.9(3) 2 . . . ? S4 N6 S4 O8 -160.9(3) 2 . . . ? O9 N6 S4 O8 -180(10) 2 . . . ? O8' N6 S4 N6 142.5(4) . . . 2 ? S4 N6 S4 N6 0.0 2 . . 2 ? O9 N6 S4 N6 -18.7(13) 2 . . 2 ? O8' N6 S4 C19 -114.8(2) . . . . ? N6 N6 S4 C19 102.7(3) 2 . . . ? S4 N6 S4 C19 102.7(3) 2 . . . ? O9 N6 S4 C19 84.1(15) 2 . . . ? O9' S4 O9 N6 148.0(4) . . . 2 ? O8' S4 O9 N6 92.0(4) . . . 2 ? O8 S4 O9 N6 158.2(2) . . . 2 ? N6 S4 O9 N6 5.4(4) . . . 2 ? C19 S4 O9 N6 -101.76(19) . . . 2 ? O9 S4 O8' N6 -111.2(4) . . . . ? O9' S4 O8' N6 -145.8(3) . . . . ? O8 S4 O8' N6 158.0(3) . . . . ? N6 S4 O8' N6 -32.9(3) 2 . . . ? C19 S4 O8' N6 83.7(2) . . . . ? N6 N6 O8' S4 38.4(3) 2 . . . ? S4 N6 O8' S4 101.3(6) 2 . . . ? O9 N6 O8' S4 174.9(4) 2 . . . ? O9 S4 C19 F10 9.2(4) . . . . ? O9' S4 C19 F10 47.7(5) . . . . ? O8' S4 C19 F10 -179.7(4) . . . . ? O8 S4 C19 F10 130.1(4) . . . . ? N6 S4 C19 F10 -119.8(4) . . . . ? N6 S4 C19 F10 -61.1(4) 2 . . . ? O9 S4 C19 F12 -113.1(3) . . . . ? O9' S4 C19 F12 -74.6(4) . . . . ? O8' S4 C19 F12 58.0(3) . . . . ? O8 S4 C19 F12 7.8(3) . . . . ? N6 S4 C19 F12 117.9(3) . . . . ? N6 S4 C19 F12 176.6(3) 2 . . . ? O9 S4 C19 F11' -178.9(4) . . . . ? O9' S4 C19 F11' -140.4(4) . . . . ? O8' S4 C19 F11' -7.8(4) . . . . ? O8 S4 C19 F11' -58.0(4) . . . . ? N6 S4 C19 F11' 52.1(4) . . . . ? N6 S4 C19 F11' 110.8(4) 2 . . . ? O9 S4 C19 F11 136.2(3) . . . . ? O9' S4 C19 F11 174.7(3) . . . . ? O8' S4 C19 F11 -52.8(3) . . . . ? O8 S4 C19 F11 -103.0(3) . . . . ? N6 S4 C19 F11 7.2(3) . . . . ? N6 S4 C19 F11 65.9(3) 2 . . . ? O9 S4 C19 F10' 58.8(3) . . . . ? O9' S4 C19 F10' 97.3(4) . . . . ? O8' S4 C19 F10' -130.2(3) . . . . ? O8 S4 C19 F10' 179.6(3) . . . . ? N6 S4 C19 F10' -70.2(3) . . . . ? N6 S4 C19 F10' -11.5(3) 2 . . . ? O9 S4 C19 F12' -53.1(3) . . . . ? O9' S4 C19 F12' -14.6(4) . . . . ? O8' S4 C19 F12' 118.0(3) . . . . ? O8 S4 C19 F12' 67.8(3) . . . . ? N6 S4 C19 F12' 177.9(3) . . . . ? N6 S4 C19 F12' -123.4(3) 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 O1 H1B O2 0.89 1.85 2.724(2) 168.1 . O1 H1C O6 0.85 1.96 2.812(3) 175.3 . O1 H1C O6' 0.85 1.83 2.642(3) 158.5 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.618 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.068 #===END OF ALL DATA