Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 _publ_contact_author ; Prof. Judith Walmsley Department of Chemistry The University of Texas at San Antonio 6900 N. Loop 1604 W. San Antonio, TX 78249-0698 USA ; _publ_contact_author_email jwalmsley@utsa.edu _publ_contact_author_fax 1(210)4587428 _publ_contact_author_phone 1(210)4585469 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Judith Walmsley' 'Rafael A. Adrian' 'Grant A. Broker' 'Douglas R. Powell' 'Edward A. Tieking' 'Shurong Zhu.' _publ_section_title ; Dinuclear palladium(II) complexes with bridging amidate ligands ; _publ_section_references ; Bruker (1998) SMART and SAINT, Bruker AXS, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2000) SADABS, University of Gottingen, Germany Sheldrick, G. M. (1997) SHELXTL, Bruker AXS, Inc., Madison, Wisconsin, USA. ; _publ_section_acknowledgements ; The authors wish to thank the National Science Foundation (CHE-0079282) and the University of Kansas for funds to acquire the diffractometer and computers used in this work. ; data_3 _database_code_depnum_ccdc_archive 'CCDC 648488' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C24 H24 N6 O2 Pd2)2+, 2(N1 O3) 1-, (H2 O1), 0.5(C3 H6 O), 0.5 (C2 H3 N) ; _chemical_formula_sum 'C26.50 H30.50 N8.50 O9.50 Pd2' _chemical_formula_weight 832.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.351(3) _cell_length_b 12.440(3) _cell_length_c 13.067(3) _cell_angle_alpha 116.880(4) _cell_angle_beta 94.893(5) _cell_angle_gamma 107.786(4) _cell_volume 1511.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1766 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 30.00 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 1.259 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5891 _exptl_absorpt_correction_T_max 0.8844 _exptl_absorpt_process_details 'SADABS, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scan frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 212 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.26 _diffrn_reflns_number 12903 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 31.51 _reflns_number_total 8852 _reflns_number_gt 7778 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0574P)^2^+1.1756P] 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 8852 _refine_ls_number_parameters 505 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.066 _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 0.541873(18) 0.552497(18) 0.142960(16) 0.01808(6) Uani 1 1 d . . . Pd2 Pd 0.588317(17) 0.626877(17) 0.387852(15) 0.01599(6) Uani 1 1 d . . . O1 O 0.56871(19) 0.74187(18) 0.21341(16) 0.0225(4) Uani 1 1 d . . . O2 O 0.7322(2) 0.5995(3) 0.17469(19) 0.0339(5) Uani 1 1 d . . . O3 O 0.6793(3) 1.1433(3) 0.6640(2) 0.0636(9) Uani 1 1 d . . . O4 O 0.7898(3) 1.1778(3) 0.8249(2) 0.0503(7) Uani 1 1 d . . . O5 O 0.7786(2) 1.0202(2) 0.6554(2) 0.0415(6) Uani 1 1 d . . . O6A O 0.8442(6) 0.3592(5) 0.2719(9) 0.087(4) Uani 0.441(6) 1 d PDU A 1 O6B O 0.8730(9) 0.3372(10) 0.3322(6) 0.0289(16) Uani 0.4463(15) 1 d PDU B 2 O6C O 0.865(6) 0.312(5) 0.324(5) 0.057(16) Uiso 0.113(6) 1 d PDU C 3 O7A O 0.9330(8) 0.2463(7) 0.1554(8) 0.082(3) Uani 0.441(6) 1 d PDU A 1 O7B O 0.8445(8) 0.3352(8) 0.1679(7) 0.0480(17) Uani 0.4463(15) 1 d PDU B 2 O7C O 0.805(2) 0.289(2) 0.154(2) 0.027(5) Uiso 0.113(6) 1 d PDU C 3 O8A O 0.7744(6) 0.1528(6) 0.2037(7) 0.0534(19) Uani 0.441(6) 1 d PDU A 1 O8B O 0.8481(16) 0.1658(7) 0.1707(6) 0.099(5) Uani 0.4463(15) 1 d PDU B 2 O8C O 0.9249(16) 0.201(2) 0.1794(17) 0.017(4) Uiso 0.113(6) 1 d PDU C 3 O9 O 0.9713(9) 0.8177(7) 0.5857(8) 0.053(2) Uani 0.50 1 d P D 1 O10 O 1.0348(5) 1.0146(5) 0.2257(5) 0.0479(13) Uani 0.50 1 d P E 2 O11 O 1.0027(7) 1.2178(7) 0.4199(7) 0.0330(13) Uani 0.50 1 d P F 2 N1 N 0.5018(3) 0.3609(2) 0.0623(2) 0.0304(6) Uani 1 1 d . . . N2 N 0.3511(2) 0.4887(2) 0.10291(18) 0.0201(4) Uani 1 1 d . . . N3 N 0.5274(2) 0.4391(2) 0.35206(18) 0.0210(4) Uani 1 1 d . . . N4 N 0.4070(2) 0.5979(2) 0.40341(19) 0.0219(4) Uani 1 1 d . . . N5 N 0.6288(2) 0.8049(2) 0.41036(19) 0.0208(4) Uani 1 1 d . . . H5A H 0.6604 0.8717 0.4835 0.025 Uiso 1 1 calc R . . N6 N 0.7648(2) 0.6446(2) 0.3677(2) 0.0212(4) Uani 1 1 d . . . H6A H 0.8218 0.6614 0.4286 0.025 Uiso 1 1 calc R . . N7 N 0.7482(2) 1.1136(2) 0.7142(2) 0.0263(5) Uani 1 1 d . . . N8A N 0.8501(5) 0.2522(5) 0.2103(5) 0.044(3) Uani 0.441(6) 1 d PDU A 1 N8B N 0.8551(6) 0.2792(5) 0.2234(5) 0.0211(15) Uani 0.4463(15) 1 d PDU B 2 N8C N 0.871(2) 0.256(2) 0.204(3) 0.019(7) Uiso 0.113(6) 1 d PDU C 3 N9 N 1.026(2) -0.010(5) 0.034(4) 0.38(2) Uiso 0.50 1 d PD . . C5 C 0.6120(2) 0.8293(2) 0.3248(2) 0.0217(5) Uani 1 1 d . . . C6 C 0.6415(4) 0.9676(3) 0.3529(3) 0.0365(7) Uani 1 1 d . . . H6B H 0.7083 0.9923 0.3157 0.055 Uiso 1 1 calc R . . H6C H 0.6717 1.0264 0.4393 0.055 Uiso 1 1 calc R . . H6D H 0.5638 0.9742 0.3221 0.055 Uiso 1 1 calc R . . C7 C 0.8046(3) 0.6339(3) 0.2746(2) 0.0248(5) Uani 1 1 d . . . C8 C 0.9430(3) 0.6576(4) 0.2765(3) 0.0367(7) Uani 1 1 d . . . H8A H 0.9718 0.7069 0.2362 0.055 Uiso 1 1 calc R . . H8B H 0.9523 0.5737 0.2355 0.055 Uiso 1 1 calc R . . H8C H 0.9951 0.7077 0.3591 0.055 Uiso 1 1 calc R . . C11 C 0.5912(4) 0.3081(4) 0.0422(3) 0.0434(9) Uani 1 1 d . . . H11A H 0.6793 0.3631 0.0661 0.052 Uiso 1 1 calc R . . C12 C 0.5542(6) 0.1743(4) -0.0132(3) 0.0631(15) Uani 1 1 d . . . H12A H 0.6166 0.1367 -0.0293 0.076 Uiso 1 1 calc R . . C13 C 0.4282(7) 0.0963(4) -0.0445(4) 0.0706(17) Uani 1 1 d . . . H13A H 0.4029 0.0044 -0.0801 0.085 Uiso 1 1 calc R . . C14 C 0.3359(5) 0.1505(3) -0.0245(3) 0.0607(14) Uani 1 1 d . . . H14A H 0.2477 0.0964 -0.0472 0.073 Uiso 1 1 calc R . . C15 C 0.3755(4) 0.2855(3) 0.0292(3) 0.0374(8) Uani 1 1 d . . . C16 C 0.2899(3) 0.3567(3) 0.0519(3) 0.0324(7) Uani 1 1 d . . . C17 C 0.1575(4) 0.3008(3) 0.0247(4) 0.0569(12) Uani 1 1 d . . . H17A H 0.1149 0.2090 -0.0095 0.068 Uiso 1 1 calc R . . C18 C 0.0877(4) 0.3780(4) 0.0471(4) 0.0587(12) Uani 1 1 d . . . H18A H -0.0033 0.3402 0.0279 0.070 Uiso 1 1 calc R . . C19 C 0.1514(3) 0.5107(3) 0.0976(3) 0.0378(7) Uani 1 1 d . . . H19A H 0.1045 0.5654 0.1138 0.045 Uiso 1 1 calc R . . C20 C 0.2836(3) 0.5645(3) 0.1250(2) 0.0228(5) Uani 1 1 d . . . H20A H 0.3272 0.6563 0.1600 0.027 Uiso 1 1 calc R . . C21 C 0.5986(3) 0.3661(3) 0.3257(2) 0.0260(5) Uani 1 1 d . . . H21A H 0.6874 0.4061 0.3337 0.031 Uiso 1 1 calc R . . C22 C 0.5449(4) 0.2336(3) 0.2870(3) 0.0368(7) Uani 1 1 d . . . H22A H 0.5961 0.1830 0.2690 0.044 Uiso 1 1 calc R . . C23 C 0.4159(4) 0.1768(3) 0.2753(3) 0.0437(9) Uani 1 1 d . . . H23A H 0.3771 0.0858 0.2470 0.052 Uiso 1 1 calc R . . C24 C 0.3420(3) 0.2529(3) 0.3050(3) 0.0361(7) Uani 1 1 d . . . H24A H 0.2536 0.2153 0.2997 0.043 Uiso 1 1 calc R . . C25 C 0.4010(3) 0.3839(3) 0.3421(2) 0.0263(5) Uani 1 1 d . . . C26 C 0.3332(3) 0.4741(3) 0.3743(2) 0.0271(6) Uani 1 1 d . . . C27 C 0.2055(3) 0.4400(4) 0.3777(3) 0.0393(8) Uani 1 1 d . . . H27A H 0.1547 0.3532 0.3572 0.047 Uiso 1 1 calc R . . C28 C 0.1536(3) 0.5336(4) 0.4112(3) 0.0465(9) Uani 1 1 d . . . H28D H 0.0664 0.5118 0.4133 0.056 Uiso 1 1 calc R . . C29 C 0.2292(3) 0.6587(4) 0.4415(3) 0.0418(8) Uani 1 1 d . . . H29D H 0.1949 0.7245 0.4660 0.050 Uiso 1 1 calc R . . C30 C 0.3553(3) 0.6884(3) 0.4363(3) 0.0292(6) Uani 1 1 d . . . H30A H 0.4067 0.7749 0.4564 0.035 Uiso 1 1 calc R . . C31 C 0.9425(5) 0.0098(5) -0.0037(5) 0.0252(10) Uiso 0.50 1 d PD . . C32 C 0.8563(4) 0.0471(4) -0.0653(4) 0.0176(8) Uiso 0.50 1 d PD . . H32B H 0.8224 0.1043 -0.0070 0.026 Uiso 0.50 1 calc PR . . H32A H 0.7849 -0.0320 -0.1272 0.026 Uiso 0.50 1 calc PR . . H32C H 0.9057 0.0932 -0.1015 0.026 Uiso 0.50 1 calc PR . . C33 C 1.0095(6) 0.9320(7) 0.6124(6) 0.0367(14) Uani 0.50 1 d P D 1 C34 C 0.9977(7) 0.9768(6) 0.5242(6) 0.0336(13) Uani 0.50 1 d P D 1 H34A H 1.0694 0.9759 0.4874 0.050 Uiso 0.50 1 calc PR D 1 H34B H 0.9996 1.0657 0.5651 0.050 Uiso 0.50 1 calc PR D 1 H34C H 0.9166 0.9179 0.4627 0.050 Uiso 0.50 1 calc PR D 1 C35 C 1.0690(7) 1.0344(7) 0.7396(6) 0.0406(15) Uani 0.50 1 d P D 1 H35A H 1.0019 1.0534 0.7783 0.061 Uiso 0.50 1 calc PR D 1 H35B H 1.1285 1.1140 0.7452 0.061 Uiso 0.50 1 calc PR D 1 H35C H 1.1158 1.0031 0.7791 0.061 Uiso 0.50 1 calc PR D 1 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 0.02581(10) 0.02229(10) 0.01335(9) 0.01093(7) 0.00837(7) 0.01425(8) Pd2 0.01784(9) 0.02096(10) 0.01334(9) 0.01062(7) 0.00641(6) 0.00895(7) O1 0.0278(9) 0.0203(8) 0.0182(8) 0.0101(7) 0.0043(7) 0.0076(7) O2 0.0319(11) 0.0610(15) 0.0274(10) 0.0279(11) 0.0181(9) 0.0293(11) O3 0.100(3) 0.0687(19) 0.0360(14) 0.0213(14) 0.0052(15) 0.0614(19) O4 0.084(2) 0.0447(14) 0.0217(11) 0.0102(10) 0.0074(12) 0.0364(14) O5 0.0455(14) 0.0414(13) 0.0296(12) 0.0060(10) 0.0047(10) 0.0269(11) O6A 0.029(3) 0.032(3) 0.152(11) 0.009(5) 0.012(5) 0.012(3) O6B 0.028(3) 0.036(4) 0.025(3) 0.012(3) 0.013(2) 0.019(3) O7A 0.107(7) 0.054(4) 0.104(7) 0.046(5) 0.081(6) 0.031(4) O7B 0.060(5) 0.062(5) 0.064(4) 0.052(4) 0.031(4) 0.039(4) O8A 0.053(4) 0.052(4) 0.073(5) 0.041(4) 0.032(3) 0.023(3) O8B 0.228(16) 0.032(4) 0.042(4) 0.017(3) 0.039(7) 0.060(7) O9 0.070(6) 0.032(4) 0.033(3) 0.018(3) -0.007(3) -0.006(3) O10 0.045(3) 0.034(2) 0.047(3) 0.007(2) -0.003(2) 0.019(2) O11 0.032(3) 0.030(3) 0.035(3) 0.017(3) 0.004(2) 0.010(2) N1 0.0613(17) 0.0300(12) 0.0188(10) 0.0169(10) 0.0207(11) 0.0311(12) N2 0.0267(11) 0.0188(9) 0.0141(9) 0.0085(8) 0.0086(8) 0.0067(8) N3 0.0288(11) 0.0215(10) 0.0127(9) 0.0101(8) 0.0056(8) 0.0073(8) N4 0.0206(10) 0.0331(11) 0.0168(9) 0.0154(9) 0.0073(8) 0.0114(9) N5 0.0241(10) 0.0204(10) 0.0178(10) 0.0096(8) 0.0057(8) 0.0086(8) N6 0.0200(10) 0.0282(11) 0.0202(10) 0.0141(9) 0.0066(8) 0.0118(8) N7 0.0304(12) 0.0267(11) 0.0256(11) 0.0153(10) 0.0099(9) 0.0117(9) N8A 0.020(5) 0.035(4) 0.058(7) 0.010(4) 0.009(4) 0.011(3) N8B 0.027(4) 0.024(3) 0.021(3) 0.013(3) 0.013(3) 0.015(3) C5 0.0225(11) 0.0204(11) 0.0220(12) 0.0114(10) 0.0063(9) 0.0068(9) C6 0.056(2) 0.0215(13) 0.0289(15) 0.0142(12) 0.0097(14) 0.0099(13) C7 0.0234(12) 0.0323(13) 0.0282(13) 0.0188(11) 0.0124(10) 0.0155(10) C8 0.0252(14) 0.0530(19) 0.0460(18) 0.0297(16) 0.0193(13) 0.0223(14) C11 0.087(3) 0.053(2) 0.0228(14) 0.0244(14) 0.0260(16) 0.057(2) C12 0.149(5) 0.054(2) 0.0291(17) 0.0282(18) 0.040(2) 0.075(3) C13 0.175(6) 0.039(2) 0.040(2) 0.0312(18) 0.059(3) 0.068(3) C14 0.127(4) 0.0240(15) 0.045(2) 0.0228(15) 0.054(2) 0.028(2) C15 0.076(2) 0.0217(13) 0.0265(14) 0.0161(11) 0.0323(15) 0.0220(14) C16 0.0494(18) 0.0181(12) 0.0245(13) 0.0086(10) 0.0238(13) 0.0063(11) C17 0.053(2) 0.0263(15) 0.054(2) 0.0021(15) 0.0373(19) -0.0082(14) C18 0.0317(17) 0.049(2) 0.049(2) 0.0004(17) 0.0242(16) -0.0073(15) C19 0.0255(14) 0.0432(17) 0.0275(15) 0.0052(13) 0.0137(11) 0.0101(12) C20 0.0234(12) 0.0254(12) 0.0173(11) 0.0079(10) 0.0082(9) 0.0104(10) C21 0.0426(16) 0.0252(12) 0.0170(11) 0.0134(10) 0.0126(11) 0.0160(11) C22 0.070(2) 0.0249(13) 0.0215(13) 0.0136(11) 0.0181(14) 0.0213(14) C23 0.074(3) 0.0223(13) 0.0254(15) 0.0135(12) 0.0117(15) 0.0043(15) C24 0.0433(17) 0.0258(14) 0.0269(14) 0.0154(12) 0.0037(12) -0.0039(12) C25 0.0318(14) 0.0294(13) 0.0149(11) 0.0137(10) 0.0058(10) 0.0043(11) C26 0.0228(12) 0.0415(15) 0.0164(11) 0.0177(11) 0.0056(9) 0.0065(11) C27 0.0218(13) 0.062(2) 0.0329(16) 0.0322(16) 0.0050(11) 0.0031(13) C28 0.0187(13) 0.089(3) 0.0450(19) 0.045(2) 0.0130(13) 0.0196(16) C29 0.0288(15) 0.077(3) 0.0401(18) 0.0367(18) 0.0186(13) 0.0315(17) C30 0.0281(14) 0.0462(17) 0.0249(13) 0.0217(13) 0.0123(11) 0.0215(12) C33 0.028(3) 0.042(3) 0.027(3) 0.016(3) 0.002(2) 0.001(2) C34 0.040(3) 0.031(3) 0.030(3) 0.017(2) 0.015(2) 0.009(2) C35 0.036(3) 0.043(4) 0.031(3) 0.013(3) 0.007(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 1.994(2) . ? Pd1 N1 1.996(2) . ? Pd1 O2 2.009(2) . ? Pd1 O1 2.0106(19) . ? Pd1 Pd2 2.8480(8) . ? Pd2 N5 1.992(2) . ? Pd2 N6 2.001(2) . ? Pd2 N4 2.023(2) . ? Pd2 N3 2.030(2) . ? Pd2 Pd2 8.970(2) 2_665 ? O1 C5 1.289(3) . ? O2 C7 1.289(3) . ? O3 N7 1.219(3) . ? O4 N7 1.250(3) . ? O5 N7 1.242(3) . ? O6A N8A 1.232(4) . ? O6B N8B 1.232(4) . ? O6C N8C 1.42(6) . ? O7A N8A 1.231(4) . ? O7B N8B 1.232(4) . ? O7C N8C 1.22(4) . ? O8A N8A 1.231(4) . ? O8B N8B 1.231(4) . ? O8C N8C 1.02(4) . ? O9 C33 1.217(10) . ? N1 C11 1.351(4) . ? N1 C15 1.352(5) . ? N2 C20 1.339(3) . ? N2 C16 1.363(3) . ? N3 C21 1.346(4) . ? N3 C25 1.353(4) . ? N4 C30 1.344(4) . ? N4 C26 1.359(4) . ? N5 C5 1.298(3) . ? N5 H5A 0.8800 . ? N6 C7 1.298(3) . ? N6 H6A 0.8800 . ? N9 C31 0.55(4) 2_755 ? N9 C31 1.176(4) . ? C5 C6 1.503(4) . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C6 H6D 0.9800 . ? C7 C8 1.503(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 C12 1.380(5) . ? C11 H11A 0.9500 . ? C12 C13 1.360(8) . ? C12 H12A 0.9500 . ? C13 C14 1.392(7) . ? C13 H13A 0.9500 . ? C14 C15 1.391(4) . ? C14 H14A 0.9500 . ? C15 C16 1.467(5) . ? C16 C17 1.384(5) . ? C17 C18 1.374(6) . ? C17 H17A 0.9500 . ? C18 C19 1.374(5) . ? C18 H18A 0.9500 . ? C19 C20 1.381(4) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.387(4) . ? C21 H21A 0.9500 . ? C22 C23 1.378(5) . ? C22 H22A 0.9500 . ? C23 C24 1.399(5) . ? C23 H23A 0.9500 . ? C24 C25 1.380(4) . ? C24 H24A 0.9500 . ? C25 C26 1.478(4) . ? C26 C27 1.392(4) . ? C27 C28 1.377(5) . ? C27 H27A 0.9500 . ? C28 C29 1.372(6) . ? C28 H28D 0.9500 . ? C29 C30 1.381(4) . ? C29 H29D 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.517(3) . ? C32 H32B 0.9800 . ? C32 H32A 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.487(9) . ? C33 C34 1.501(9) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? 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 81.56(10) . . ? N2 Pd1 O2 174.71(9) . . ? N1 Pd1 O2 93.18(11) . . ? N2 Pd1 O1 94.41(8) . . ? N1 Pd1 O1 174.92(9) . . ? O2 Pd1 O1 90.81(9) . . ? N2 Pd1 Pd2 98.39(6) . . ? N1 Pd1 Pd2 102.65(6) . . ? O2 Pd1 Pd2 83.23(6) . . ? O1 Pd1 Pd2 80.93(5) . . ? N5 Pd2 N6 88.00(9) . . ? N5 Pd2 N4 95.04(9) . . ? N6 Pd2 N4 176.76(9) . . ? N5 Pd2 N3 173.37(9) . . ? N6 Pd2 N3 96.62(9) . . ? N4 Pd2 N3 80.27(9) . . ? N5 Pd2 Pd1 82.71(6) . . ? N6 Pd2 Pd1 80.63(6) . . ? N4 Pd2 Pd1 98.59(6) . . ? N3 Pd2 Pd1 93.31(6) . . ? N5 Pd2 Pd2 83.82(6) . 2_665 ? N6 Pd2 Pd2 82.50(6) . 2_665 ? N4 Pd2 Pd2 96.67(6) . 2_665 ? N3 Pd2 Pd2 92.03(6) . 2_665 ? Pd1 Pd2 Pd2 2.155(4) . 2_665 ? C5 O1 Pd1 125.85(17) . . ? C7 O2 Pd1 123.87(17) . . ? C11 N1 C15 121.6(3) . . ? C11 N1 Pd1 124.1(3) . . ? C15 N1 Pd1 114.26(19) . . ? C20 N2 C16 120.3(3) . . ? C20 N2 Pd1 125.32(18) . . ? C16 N2 Pd1 114.3(2) . . ? C21 N3 C25 120.1(2) . . ? C21 N3 Pd2 124.92(19) . . ? C25 N3 Pd2 114.55(18) . . ? C30 N4 C26 119.2(2) . . ? C30 N4 Pd2 125.6(2) . . ? C26 N4 Pd2 115.13(19) . . ? C5 N5 Pd2 124.65(18) . . ? C5 N5 H5A 117.7 . . ? Pd2 N5 H5A 117.7 . . ? C7 N6 Pd2 127.16(19) . . ? C7 N6 H6A 116.4 . . ? Pd2 N6 H6A 116.4 . . ? O3 N7 O5 120.1(3) . . ? O3 N7 O4 120.2(3) . . ? O5 N7 O4 119.6(3) . . ? O8A N8A O7A 120.5(4) . . ? O8A N8A O6A 120.6(4) . . ? O7A N8A O6A 118.9(4) . . ? O8B N8B O7B 120.4(4) . . ? O8B N8B O6B 119.8(4) . . ? O7B N8B O6B 119.8(4) . . ? O8C N8C O7C 136(4) . . ? O8C N8C O6C 117(4) . . ? O7C N8C O6C 108(4) . . ? C31 N9 C31 103(3) 2_755 . ? O1 C5 N5 124.7(2) . . ? O1 C5 C6 115.4(2) . . ? N5 C5 C6 119.9(2) . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C6 H6D 109.5 . . ? H6B C6 H6D 109.5 . . ? H6C C6 H6D 109.5 . . ? O2 C7 N6 124.7(3) . . ? O2 C7 C8 114.9(2) . . ? N6 C7 C8 120.4(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C11 C12 119.9(4) . . ? N1 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C13 C12 C11 119.7(4) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C14 120.3(4) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C15 C14 C13 118.7(5) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? N1 C15 C14 119.6(4) . . ? N1 C15 C16 115.2(2) . . ? C14 C15 C16 125.2(4) . . ? N2 C16 C17 119.9(3) . . ? N2 C16 C15 114.4(3) . . ? C17 C16 C15 125.6(3) . . ? C18 C17 C16 120.1(3) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C19 C18 C17 119.0(3) . . ? C19 C18 H18A 120.5 . . ? C17 C18 H18A 120.5 . . ? C18 C19 C20 120.0(3) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? N2 C20 C19 120.7(3) . . ? N2 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? N3 C21 C22 121.3(3) . . ? N3 C21 H21A 119.4 . . ? C22 C21 H21A 119.4 . . ? C23 C22 C21 118.8(3) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C22 C23 C24 120.2(3) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C25 C24 C23 118.1(3) . . ? C25 C24 H24A 120.9 . . ? C23 C24 H24A 120.9 . . ? N3 C25 C24 121.5(3) . . ? N3 C25 C26 115.1(2) . . ? C24 C25 C26 123.4(3) . . ? N4 C26 C27 121.0(3) . . ? N4 C26 C25 114.4(2) . . ? C27 C26 C25 124.7(3) . . ? C28 C27 C26 119.2(3) . . ? C28 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? C29 C28 C27 119.4(3) . . ? C29 C28 H28D 120.3 . . ? C27 C28 H28D 120.3 . . ? C28 C29 C30 119.7(3) . . ? C28 C29 H29D 120.2 . . ? C30 C29 H29D 120.2 . . ? N4 C30 C29 121.6(3) . . ? N4 C30 H30A 119.2 . . ? C29 C30 H30A 119.2 . . ? N9 C31 C32 166.8(17) . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? C31 C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? O9 C33 C35 118.7(7) . . ? O9 C33 C34 123.8(7) . . ? C35 C33 C34 117.4(6) . . ? 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 Pd2 N5 -100.36(9) . . . . ? N1 Pd1 Pd2 N5 176.47(10) . . . . ? O2 Pd1 Pd2 N5 84.72(10) . . . . ? O1 Pd1 Pd2 N5 -7.19(8) . . . . ? N2 Pd1 Pd2 N6 170.48(9) . . . . ? N1 Pd1 Pd2 N6 87.31(11) . . . . ? O2 Pd1 Pd2 N6 -4.44(9) . . . . ? O1 Pd1 Pd2 N6 -96.36(9) . . . . ? N2 Pd1 Pd2 N4 -6.33(9) . . . . ? N1 Pd1 Pd2 N4 -89.50(11) . . . . ? O2 Pd1 Pd2 N4 178.75(9) . . . . ? O1 Pd1 Pd2 N4 86.83(9) . . . . ? N2 Pd1 Pd2 N3 74.31(9) . . . . ? N1 Pd1 Pd2 N3 -8.85(11) . . . . ? O2 Pd1 Pd2 N3 -100.61(10) . . . . ? O1 Pd1 Pd2 N3 167.48(9) . . . . ? N2 Pd1 Pd2 Pd2 20.59(11) . . . 2_665 ? N1 Pd1 Pd2 Pd2 -62.57(13) . . . 2_665 ? O2 Pd1 Pd2 Pd2 -154.32(12) . . . 2_665 ? O1 Pd1 Pd2 Pd2 113.76(11) . . . 2_665 ? N2 Pd1 O1 C5 108.6(2) . . . . ? N1 Pd1 O1 C5 145.9(9) . . . . ? O2 Pd1 O1 C5 -72.2(2) . . . . ? Pd2 Pd1 O1 C5 10.8(2) . . . . ? N2 Pd1 O2 C7 -103.8(9) . . . . ? N1 Pd1 O2 C7 -98.0(2) . . . . ? O1 Pd1 O2 C7 85.1(2) . . . . ? Pd2 Pd1 O2 C7 4.3(2) . . . . ? N2 Pd1 N1 C11 176.4(2) . . . . ? O2 Pd1 N1 C11 -3.0(2) . . . . ? O1 Pd1 N1 C11 138.8(9) . . . . ? Pd2 Pd1 N1 C11 -86.8(2) . . . . ? N2 Pd1 N1 C15 -4.13(19) . . . . ? O2 Pd1 N1 C15 176.41(19) . . . . ? O1 Pd1 N1 C15 -41.8(10) . . . . ? Pd2 Pd1 N1 C15 92.64(19) . . . . ? N1 Pd1 N2 C20 -177.5(2) . . . . ? O2 Pd1 N2 C20 -171.7(8) . . . . ? O1 Pd1 N2 C20 -0.6(2) . . . . ? Pd2 Pd1 N2 C20 80.8(2) . . . . ? N1 Pd1 N2 C16 4.22(18) . . . . ? O2 Pd1 N2 C16 10.1(9) . . . . ? O1 Pd1 N2 C16 -178.88(18) . . . . ? Pd2 Pd1 N2 C16 -97.42(18) . . . . ? N5 Pd2 N3 C21 134.3(7) . . . . ? N6 Pd2 N3 C21 0.4(2) . . . . ? N4 Pd2 N3 C21 179.5(2) . . . . ? Pd1 Pd2 N3 C21 81.3(2) . . . . ? Pd2 Pd2 N3 C21 83.1(2) 2_665 . . . ? N5 Pd2 N3 C25 -38.1(8) . . . . ? N6 Pd2 N3 C25 -171.95(17) . . . . ? N4 Pd2 N3 C25 7.15(17) . . . . ? Pd1 Pd2 N3 C25 -91.01(17) . . . . ? Pd2 Pd2 N3 C25 -89.27(17) 2_665 . . . ? N5 Pd2 N4 C30 -8.3(2) . . . . ? N6 Pd2 N4 C30 -167.6(14) . . . . ? N3 Pd2 N4 C30 176.4(2) . . . . ? Pd1 Pd2 N4 C30 -91.7(2) . . . . ? Pd2 Pd2 N4 C30 -92.7(2) 2_665 . . . ? N5 Pd2 N4 C26 169.87(18) . . . . ? N6 Pd2 N4 C26 10.6(15) . . . . ? N3 Pd2 N4 C26 -5.41(17) . . . . ? Pd1 Pd2 N4 C26 86.50(17) . . . . ? Pd2 Pd2 N4 C26 85.52(17) 2_665 . . . ? N6 Pd2 N5 C5 87.6(2) . . . . ? N4 Pd2 N5 C5 -91.2(2) . . . . ? N3 Pd2 N5 C5 -46.6(8) . . . . ? Pd1 Pd2 N5 C5 6.8(2) . . . . ? Pd2 Pd2 N5 C5 5.0(2) 2_665 . . . ? N5 Pd2 N6 C7 -76.3(2) . . . . ? N4 Pd2 N6 C7 83.0(15) . . . . ? N3 Pd2 N6 C7 98.9(2) . . . . ? Pd1 Pd2 N6 C7 6.6(2) . . . . ? Pd2 Pd2 N6 C7 7.7(2) 2_665 . . . ? Pd1 O1 C5 N5 -9.7(4) . . . . ? Pd1 O1 C5 C6 171.3(2) . . . . ? Pd2 N5 C5 O1 -1.2(4) . . . . ? Pd2 N5 C5 C6 177.7(2) . . . . ? Pd1 O2 C7 N6 -1.1(4) . . . . ? Pd1 O2 C7 C8 176.8(2) . . . . ? Pd2 N6 C7 O2 -5.7(4) . . . . ? Pd2 N6 C7 C8 176.5(2) . . . . ? C15 N1 C11 C12 -0.1(4) . . . . ? Pd1 N1 C11 C12 179.3(2) . . . . ? N1 C11 C12 C13 -1.7(5) . . . . ? C11 C12 C13 C14 2.1(5) . . . . ? C12 C13 C14 C15 -0.8(5) . . . . ? C11 N1 C15 C14 1.5(4) . . . . ? Pd1 N1 C15 C14 -178.0(2) . . . . ? C11 N1 C15 C16 -177.2(2) . . . . ? Pd1 N1 C15 C16 3.4(3) . . . . ? C13 C14 C15 N1 -1.0(5) . . . . ? C13 C14 C15 C16 177.5(3) . . . . ? C20 N2 C16 C17 -1.2(4) . . . . ? Pd1 N2 C16 C17 177.2(3) . . . . ? C20 N2 C16 C15 178.1(2) . . . . ? Pd1 N2 C16 C15 -3.6(3) . . . . ? N1 C15 C16 N2 0.2(4) . . . . ? C14 C15 C16 N2 -178.4(3) . . . . ? N1 C15 C16 C17 179.3(3) . . . . ? C14 C15 C16 C17 0.8(5) . . . . ? N2 C16 C17 C18 1.2(6) . . . . ? C15 C16 C17 C18 -177.9(3) . . . . ? C16 C17 C18 C19 -0.7(6) . . . . ? C17 C18 C19 C20 0.1(6) . . . . ? C16 N2 C20 C19 0.6(4) . . . . ? Pd1 N2 C20 C19 -177.6(2) . . . . ? C18 C19 C20 N2 0.0(5) . . . . ? C25 N3 C21 C22 0.6(4) . . . . ? Pd2 N3 C21 C22 -171.4(2) . . . . ? N3 C21 C22 C23 0.3(4) . . . . ? C21 C22 C23 C24 -1.6(4) . . . . ? C22 C23 C24 C25 2.1(5) . . . . ? C21 N3 C25 C24 -0.1(4) . . . . ? Pd2 N3 C25 C24 172.6(2) . . . . ? C21 N3 C25 C26 179.6(2) . . . . ? Pd2 N3 C25 C26 -7.7(3) . . . . ? C23 C24 C25 N3 -1.2(4) . . . . ? C23 C24 C25 C26 179.1(3) . . . . ? C30 N4 C26 C27 0.2(4) . . . . ? Pd2 N4 C26 C27 -178.1(2) . . . . ? C30 N4 C26 C25 -178.8(2) . . . . ? Pd2 N4 C26 C25 2.9(3) . . . . ? N3 C25 C26 N4 3.1(3) . . . . ? C24 C25 C26 N4 -177.2(2) . . . . ? N3 C25 C26 C27 -175.8(3) . . . . ? C24 C25 C26 C27 3.9(4) . . . . ? N4 C26 C27 C28 0.0(4) . . . . ? C25 C26 C27 C28 178.9(3) . . . . ? C26 C27 C28 C29 -0.6(5) . . . . ? C27 C28 C29 C30 1.0(5) . . . . ? C26 N4 C30 C29 0.2(4) . . . . ? Pd2 N4 C30 C29 178.3(2) . . . . ? C28 C29 C30 N4 -0.8(5) . . . . ? C31 N9 C31 C32 -18(17) 2_755 . . . ? 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 N6 H6A O9 0.88 2.16 2.912(9) 143.4 . N6 H6A O11 0.88 2.23 3.048(8) 155.5 2_776 N5 H5A O5 0.88 2.12 2.975(3) 165.1 . _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.377 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.135 # Attachment 'JW-Complex 4.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 648489' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 N6 O2 Pd2, 2(C F3 O3 S)' _chemical_formula_sum 'C26 H24 F6 N6 O8 Pd2 S2' _chemical_formula_weight 939.43 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 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 13.099(2) _cell_length_b 22.755(4) _cell_length_c 22.203(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.854(5) _cell_angle_gamma 90.00 _cell_volume 6366.3(19) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7109 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.25 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 1.355 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7195 _exptl_absorpt_correction_T_max 0.8764 _exptl_absorpt_process_details 'SADABS (Sheldrick, 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 'CCD Bruker APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49452 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12472 _reflns_number_gt 9866 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 2000)' _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^)+(0.0747P)^2^+14.6865P] 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 12472 _refine_ls_number_parameters 974 _refine_ls_number_restraints 234 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1322 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.074 _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 0.61596(3) 0.600536(17) 0.273445(18) 0.01934(11) Uani 1 1 d . . . Pd2 Pd 0.83692(3) 0.576512(17) 0.312489(19) 0.02090(11) Uani 1 1 d . . . Pd3 Pd 0.14775(3) 0.671408(18) 0.21750(2) 0.02510(12) Uani 1 1 d . . . Pd4 Pd 0.36579(3) 0.645009(16) 0.235997(18) 0.01951(11) Uani 1 1 d . . . S1 S 0.99948(13) 0.40029(7) 0.40151(8) 0.0376(4) Uani 1 1 d . . . S2 S 0.23666(13) 0.82581(6) 0.44058(7) 0.0315(3) Uani 1 1 d . . . S3 S -0.01097(12) 0.84158(6) 0.11655(6) 0.0263(3) Uani 1 1 d . . . S4A S 0.7193(3) 0.4309(2) 0.0843(2) 0.0242(9) Uani 0.512(7) 1 d PU A 1 S4B S 0.7565(7) 0.4237(3) 0.0787(3) 0.0592(15) Uani 0.488(7) 1 d PU A 2 F1 F 1.1293(4) 0.32466(17) 0.37261(18) 0.0524(11) Uani 1 1 d . . . F2 F 1.1834(3) 0.35856(17) 0.46680(17) 0.0485(10) Uani 1 1 d . . . F3 F 1.1919(3) 0.41307(19) 0.38890(19) 0.0507(10) Uani 1 1 d . . . F4 F 0.4227(3) 0.79102(18) 0.4293(2) 0.0534(11) Uani 1 1 d . . . F5 F 0.3949(3) 0.88450(17) 0.41797(18) 0.0501(10) Uani 1 1 d . . . F6 F 0.4329(3) 0.84549(17) 0.51006(16) 0.0441(9) Uani 1 1 d . . . F7 F -0.1939(3) 0.86791(16) 0.03748(15) 0.0381(8) Uani 1 1 d . . . F8 F -0.2065(3) 0.82111(17) 0.11971(19) 0.0477(10) Uani 1 1 d . . . F9 F -0.1631(3) 0.91270(16) 0.12574(17) 0.0499(11) Uani 1 1 d . . . F10A F 0.6981(11) 0.4570(6) -0.0305(4) 0.080(3) Uani 0.512(7) 1 d PU A 1 F10B F 0.6613(8) 0.4886(4) -0.0203(4) 0.049(2) Uani 0.488(7) 1 d PU A 2 F11A F 0.8499(9) 0.4190(4) 0.0161(6) 0.072(2) Uani 0.512(7) 1 d PU A 1 F11B F 0.7872(8) 0.4301(4) -0.0294(4) 0.048(2) Uani 0.488(7) 1 d PU A 2 F12A F 0.821(3) 0.5072(16) 0.0335(15) 0.053(4) Uani 0.512(7) 1 d PU A 1 F12B F 0.829(3) 0.5090(16) 0.0240(15) 0.043(3) Uani 0.488(7) 1 d PU A 2 O1 O 0.6050(3) 0.51419(16) 0.25383(18) 0.0276(8) Uani 1 1 d . . . O2 O 0.6389(3) 0.58307(16) 0.36658(17) 0.0244(8) Uani 1 1 d . . . O3 O 0.3321(3) 0.66363(16) 0.14380(18) 0.0284(9) Uani 1 1 d . . . O4 O 0.3822(3) 0.73130(15) 0.25596(18) 0.0250(8) Uani 1 1 d . . . O5 O 0.9499(4) 0.3514(2) 0.4232(3) 0.0549(14) Uani 1 1 d . . . O6 O 0.9612(4) 0.41239(19) 0.3354(2) 0.0461(12) Uani 1 1 d . . . O7 O 1.0173(4) 0.45174(19) 0.4410(2) 0.0511(13) Uani 1 1 d . . . O8 O 0.1958(4) 0.81846(18) 0.37381(19) 0.0367(10) Uani 1 1 d . . . O9 O 0.2340(4) 0.77395(18) 0.47716(19) 0.0390(10) Uani 1 1 d . . . O10 O 0.2044(4) 0.8791(2) 0.4649(2) 0.0429(11) Uani 1 1 d . . . O11 O -0.0118(3) 0.78754(16) 0.08254(18) 0.0297(9) Uani 1 1 d . . . O12 O 0.0354(4) 0.89121(17) 0.09338(19) 0.0373(10) Uani 1 1 d . . . O13 O 0.0193(3) 0.83528(16) 0.18432(18) 0.0301(9) Uani 1 1 d . . . O14A O 0.6824(14) 0.3748(8) 0.0671(8) 0.035(3) Uani 0.512(7) 1 d PU A 1 O14B O 0.6604(18) 0.3826(10) 0.0527(10) 0.048(4) Uani 0.488(7) 1 d PU A 2 O15A O 0.6389(11) 0.4741(5) 0.0838(6) 0.066(3) Uani 0.512(7) 1 d PU A 1 O15B O 0.7077(15) 0.4737(6) 0.1123(6) 0.080(3) Uani 0.488(7) 1 d PU A 2 O16A O 0.8083(8) 0.4376(5) 0.1387(4) 0.053(2) Uani 0.512(7) 1 d PU A 1 O16B O 0.8464(12) 0.4012(6) 0.1015(7) 0.095(4) Uani 0.488(7) 1 d PU A 2 N1 N 0.6219(3) 0.68776(19) 0.2837(2) 0.0224(9) Uani 1 1 d . . . N2 N 0.5853(3) 0.6233(2) 0.1831(2) 0.0246(10) Uani 1 1 d . . . N3 N 0.8863(3) 0.65776(19) 0.3472(2) 0.0233(10) Uani 1 1 d . . . N4 N 0.8542(3) 0.61470(18) 0.2332(2) 0.0207(9) Uani 1 1 d . . . N5 N 0.7835(4) 0.49822(19) 0.2743(2) 0.0266(10) Uani 1 1 d D . . H5A H 0.8314 0.4733 0.2687 0.032 Uiso 1 1 calc RD . . N6 N 0.8089(4) 0.5476(2) 0.3915(2) 0.0303(11) Uani 1 1 d D . . H6A H 0.8597 0.5294 0.4194 0.036 Uiso 1 1 calc RD . . N7 N 0.1360(3) 0.64293(19) 0.3027(2) 0.0260(10) Uani 1 1 d . . . N8 N 0.0959(4) 0.58852(19) 0.1945(2) 0.0269(10) Uani 1 1 d . . . N9 N 0.3993(3) 0.61985(18) 0.3256(2) 0.0213(9) Uani 1 1 d . . . N10 N 0.3614(3) 0.55824(19) 0.2235(2) 0.0232(9) Uani 1 1 d . . . N11 N 0.1612(4) 0.6932(2) 0.1326(2) 0.0324(11) Uani 1 1 d D . . H11A H 0.1041 0.7078 0.1061 0.039 Uiso 1 1 calc RD . . N12 N 0.2072(4) 0.75121(19) 0.2449(2) 0.0303(11) Uani 1 1 d D . . H12A H 0.1625 0.7779 0.2512 0.036 Uiso 1 1 calc RD . . C5 C 0.6858(4) 0.4809(2) 0.2572(2) 0.0243(12) Uani 1 1 d . . . C6 C 0.6583(5) 0.4185(2) 0.2367(3) 0.0357(14) Uani 1 1 d . . . H6B H 0.5811 0.4134 0.2256 0.054 Uiso 1 1 calc R . . H6C H 0.6916 0.3917 0.2710 0.054 Uiso 1 1 calc R . . H6D H 0.6842 0.4097 0.2002 0.054 Uiso 1 1 calc R . . C7 C 0.7172(4) 0.5550(2) 0.4024(2) 0.0230(11) Uani 1 1 d . . . C8 C 0.6968(5) 0.5307(3) 0.4619(3) 0.0349(14) Uani 1 1 d . . . H8A H 0.6242 0.5403 0.4626 0.052 Uiso 1 1 calc R . . H8B H 0.7472 0.5481 0.4985 0.052 Uiso 1 1 calc R . . H8C H 0.7058 0.4879 0.4629 0.052 Uiso 1 1 calc R . . C11 C 0.6390(4) 0.7161(2) 0.3381(3) 0.0277(12) Uani 1 1 d . . . H11B H 0.6479 0.6941 0.3755 0.033 Uiso 1 1 calc R . . C12 C 0.6440(5) 0.7775(2) 0.3414(3) 0.0325(13) Uani 1 1 d . . . H12B H 0.6551 0.7972 0.3803 0.039 Uiso 1 1 calc R . . C13 C 0.6323(5) 0.8088(3) 0.2863(3) 0.0367(15) Uani 1 1 d . . . H13A H 0.6360 0.8505 0.2874 0.044 Uiso 1 1 calc R . . C14 C 0.6151(5) 0.7795(3) 0.2295(3) 0.0329(14) Uani 1 1 d . . . H14A H 0.6067 0.8007 0.1916 0.040 Uiso 1 1 calc R . . C15 C 0.6104(4) 0.7183(2) 0.2293(3) 0.0268(12) Uani 1 1 d . . . C16 C 0.5906(4) 0.6820(2) 0.1726(3) 0.0258(12) Uani 1 1 d . . . C17 C 0.5769(5) 0.7034(3) 0.1123(3) 0.0373(15) Uani 1 1 d . . . H17A H 0.5807 0.7443 0.1049 0.045 Uiso 1 1 calc R . . C18 C 0.5577(5) 0.6637(3) 0.0630(3) 0.0427(16) Uani 1 1 d . . . H18A H 0.5496 0.6774 0.0216 0.051 Uiso 1 1 calc R . . C19 C 0.5502(5) 0.6043(3) 0.0739(3) 0.0365(14) Uani 1 1 d . . . H19A H 0.5351 0.5770 0.0402 0.044 Uiso 1 1 calc R . . C20 C 0.5652(5) 0.5855(3) 0.1346(3) 0.0322(13) Uani 1 1 d . . . H20A H 0.5613 0.5446 0.1426 0.039 Uiso 1 1 calc R . . C21 C 0.9012(4) 0.6745(3) 0.4065(3) 0.0302(13) Uani 1 1 d . . . H21A H 0.8940 0.6465 0.4368 0.036 Uiso 1 1 calc R . . C22 C 0.9274(5) 0.7326(3) 0.4248(3) 0.0365(14) Uani 1 1 d . . . H22A H 0.9350 0.7444 0.4669 0.044 Uiso 1 1 calc R . . C23 C 0.9420(5) 0.7726(3) 0.3814(3) 0.0351(14) Uani 1 1 d . . . H23A H 0.9611 0.8121 0.3934 0.042 Uiso 1 1 calc R . . C24 C 0.9286(4) 0.7549(2) 0.3199(3) 0.0279(12) Uani 1 1 d . . . H24A H 0.9386 0.7819 0.2895 0.034 Uiso 1 1 calc R . . C25 C 0.9000(4) 0.6964(2) 0.3035(2) 0.0215(11) Uani 1 1 d . . . C26 C 0.8802(4) 0.6724(2) 0.2395(2) 0.0213(11) Uani 1 1 d . . . C27 C 0.8858(4) 0.7061(2) 0.1884(3) 0.0259(12) Uani 1 1 d . . . H27A H 0.9088 0.7458 0.1939 0.031 Uiso 1 1 calc R . . C28 C 0.8573(5) 0.6812(2) 0.1293(3) 0.0276(12) Uani 1 1 d . . . H28A H 0.8566 0.7041 0.0934 0.033 Uiso 1 1 calc R . . C29 C 0.8295(4) 0.6215(2) 0.1233(3) 0.0272(12) Uani 1 1 d . . . H29A H 0.8107 0.6032 0.0833 0.033 Uiso 1 1 calc R . . C30 C 0.8300(4) 0.5898(2) 0.1760(2) 0.0221(11) Uani 1 1 d . . . H30A H 0.8128 0.5492 0.1720 0.027 Uiso 1 1 calc R . . C35 C 0.2441(5) 0.6883(2) 0.1125(3) 0.0285(13) Uani 1 1 d . . . C36 C 0.2441(6) 0.7100(3) 0.0482(3) 0.0417(16) Uani 1 1 d . . . H36A H 0.1753 0.7279 0.0279 0.063 Uiso 1 1 calc R . . H36B H 0.2565 0.6768 0.0229 0.063 Uiso 1 1 calc R . . H36C H 0.3005 0.7392 0.0521 0.063 Uiso 1 1 calc R . . C37 C 0.3045(5) 0.7670(2) 0.2543(3) 0.0249(12) Uani 1 1 d . . . C38 C 0.3360(5) 0.8306(2) 0.2656(3) 0.0357(14) Uani 1 1 d . . . H38A H 0.2728 0.8544 0.2635 0.054 Uiso 1 1 calc R . . H38B H 0.3694 0.8440 0.2335 0.054 Uiso 1 1 calc R . . H38C H 0.3863 0.8348 0.3071 0.054 Uiso 1 1 calc R . . C41 C 0.1564(4) 0.6752(3) 0.3557(3) 0.0302(13) Uani 1 1 d . . . H41A H 0.1757 0.7153 0.3545 0.036 Uiso 1 1 calc R . . C42 C 0.1498(4) 0.6509(3) 0.4115(3) 0.0316(13) Uani 1 1 d . . . H42A H 0.1656 0.6743 0.4483 0.038 Uiso 1 1 calc R . . C43 C 0.1202(5) 0.5927(3) 0.4138(3) 0.0343(14) Uani 1 1 d . . . H43A H 0.1147 0.5758 0.4519 0.041 Uiso 1 1 calc R . . C44 C 0.0988(4) 0.5598(3) 0.3593(3) 0.0319(13) Uani 1 1 d . . . H44A H 0.0782 0.5198 0.3597 0.038 Uiso 1 1 calc R . . C45 C 0.1075(4) 0.5855(2) 0.3039(3) 0.0253(12) Uani 1 1 d . . . C46 C 0.0858(4) 0.5544(2) 0.2431(3) 0.0281(12) Uani 1 1 d . . . C47 C 0.0572(5) 0.4956(2) 0.2346(3) 0.0346(14) Uani 1 1 d . . . H47A H 0.0506 0.4722 0.2688 0.042 Uiso 1 1 calc R . . C48 C 0.0382(5) 0.4718(3) 0.1749(3) 0.0408(16) Uani 1 1 d . . . H48A H 0.0182 0.4318 0.1677 0.049 Uiso 1 1 calc R . . C49 C 0.0488(5) 0.5069(3) 0.1259(3) 0.0390(15) Uani 1 1 d . . . H49A H 0.0367 0.4911 0.0850 0.047 Uiso 1 1 calc R . . C50 C 0.0769(5) 0.5649(3) 0.1372(3) 0.0342(14) Uani 1 1 d . . . H50A H 0.0830 0.5889 0.1034 0.041 Uiso 1 1 calc R . . C51 C 0.4207(4) 0.6564(2) 0.3752(2) 0.0229(11) Uani 1 1 d . . . H51A H 0.4235 0.6975 0.3683 0.027 Uiso 1 1 calc R . . C52 C 0.4387(5) 0.6359(2) 0.4355(3) 0.0287(12) Uani 1 1 d . . . H52A H 0.4548 0.6623 0.4699 0.034 Uiso 1 1 calc R . . C53 C 0.4328(5) 0.5755(2) 0.4451(3) 0.0312(13) Uani 1 1 d . . . H53A H 0.4440 0.5604 0.4863 0.037 Uiso 1 1 calc R . . C54 C 0.4105(4) 0.5378(2) 0.3943(3) 0.0268(12) Uani 1 1 d . . . H54A H 0.4056 0.4966 0.4002 0.032 Uiso 1 1 calc R . . C55 C 0.3954(4) 0.5608(2) 0.3346(3) 0.0220(11) Uani 1 1 d . . . C56 C 0.3760(4) 0.5255(2) 0.2765(3) 0.0220(11) Uani 1 1 d . . . C57 C 0.3773(4) 0.4646(2) 0.2748(3) 0.0260(12) Uani 1 1 d . . . H57A H 0.3875 0.4422 0.3121 0.031 Uiso 1 1 calc R . . C58 C 0.3633(4) 0.4372(2) 0.2174(3) 0.0277(12) Uani 1 1 d . . . H58A H 0.3647 0.3955 0.2152 0.033 Uiso 1 1 calc R . . C59 C 0.3472(4) 0.4706(2) 0.1631(3) 0.0286(12) Uani 1 1 d . . . H59A H 0.3365 0.4521 0.1235 0.034 Uiso 1 1 calc R . . C60 C 0.3470(4) 0.5315(2) 0.1680(3) 0.0264(12) Uani 1 1 d . . . H60A H 0.3365 0.5547 0.1312 0.032 Uiso 1 1 calc R . . C61 C 1.1292(6) 0.3735(3) 0.4074(3) 0.0387(15) Uani 1 1 d . . . C62 C 0.3795(5) 0.8370(2) 0.4503(3) 0.0331(14) Uani 1 1 d . . . C63 C -0.1504(5) 0.8612(3) 0.0993(3) 0.0334(14) Uani 1 1 d . . . C64A C 0.773(2) 0.4546(9) 0.0230(9) 0.049(2) Uani 0.512(7) 1 d PU A 1 C64B C 0.761(2) 0.4660(9) 0.0112(10) 0.046(2) Uani 0.488(7) 1 d PU A 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 0.0227(2) 0.0170(2) 0.0186(2) 0.00094(15) 0.00628(16) 0.00024(15) Pd2 0.0232(2) 0.0194(2) 0.0214(2) 0.00223(15) 0.00831(16) 0.00039(15) Pd3 0.0237(2) 0.0179(2) 0.0326(3) -0.00044(17) 0.00580(18) 0.00130(16) Pd4 0.0241(2) 0.01306(19) 0.0212(2) -0.00061(15) 0.00589(16) 0.00108(15) S1 0.0454(9) 0.0233(7) 0.0460(10) -0.0039(7) 0.0158(8) -0.0030(6) S2 0.0490(9) 0.0245(7) 0.0217(7) 0.0014(6) 0.0110(6) -0.0056(6) S3 0.0365(8) 0.0174(6) 0.0232(7) -0.0003(5) 0.0048(6) -0.0019(5) S4A 0.030(2) 0.0219(16) 0.0234(16) 0.0020(11) 0.0120(14) 0.0035(14) S4B 0.089(4) 0.045(3) 0.036(2) 0.0033(19) 0.003(3) -0.022(3) F1 0.081(3) 0.040(2) 0.032(2) -0.0051(17) 0.010(2) 0.024(2) F2 0.068(3) 0.048(2) 0.0250(19) 0.0000(16) 0.0037(18) 0.003(2) F3 0.048(2) 0.060(3) 0.045(2) 0.011(2) 0.0153(19) 0.003(2) F4 0.062(3) 0.051(2) 0.053(3) -0.012(2) 0.025(2) 0.003(2) F5 0.076(3) 0.041(2) 0.038(2) 0.0031(17) 0.023(2) -0.024(2) F6 0.053(2) 0.051(2) 0.027(2) -0.0038(16) 0.0096(17) -0.0110(18) F7 0.046(2) 0.042(2) 0.0226(18) 0.0019(15) 0.0032(15) 0.0092(16) F8 0.042(2) 0.052(2) 0.052(2) 0.0191(19) 0.0174(19) 0.0088(18) F9 0.084(3) 0.037(2) 0.028(2) 0.0001(16) 0.0142(19) 0.028(2) F10A 0.113(6) 0.088(7) 0.028(4) 0.006(5) 0.001(4) -0.041(5) F10B 0.075(5) 0.024(4) 0.045(5) 0.015(3) 0.010(4) 0.006(3) F11A 0.095(6) 0.053(4) 0.090(6) -0.026(5) 0.062(5) -0.023(4) F11B 0.072(5) 0.036(4) 0.037(4) -0.013(3) 0.017(4) -0.009(4) F12A 0.083(7) 0.031(5) 0.040(9) 0.006(6) 0.011(6) -0.019(4) F12B 0.077(6) 0.025(4) 0.026(7) 0.007(4) 0.011(5) -0.008(4) O1 0.032(2) 0.0212(19) 0.028(2) -0.0006(16) 0.0048(17) -0.0024(16) O2 0.032(2) 0.0226(19) 0.0202(19) 0.0016(15) 0.0094(16) 0.0017(16) O3 0.039(2) 0.023(2) 0.023(2) 0.0010(16) 0.0100(18) 0.0037(17) O4 0.028(2) 0.0168(18) 0.031(2) -0.0018(15) 0.0087(16) -0.0007(15) O5 0.063(3) 0.037(3) 0.072(4) -0.006(2) 0.030(3) -0.017(2) O6 0.047(3) 0.032(2) 0.053(3) -0.003(2) 0.003(2) 0.007(2) O7 0.073(4) 0.031(3) 0.058(3) -0.019(2) 0.033(3) -0.008(2) O8 0.058(3) 0.030(2) 0.022(2) -0.0005(17) 0.010(2) -0.007(2) O9 0.059(3) 0.029(2) 0.028(2) 0.0083(18) 0.011(2) -0.012(2) O10 0.065(3) 0.039(3) 0.028(2) -0.0035(19) 0.017(2) 0.003(2) O11 0.035(2) 0.0193(19) 0.033(2) -0.0056(16) 0.0074(18) -0.0010(16) O12 0.058(3) 0.025(2) 0.026(2) -0.0006(17) 0.008(2) -0.0132(19) O13 0.041(2) 0.0217(19) 0.024(2) 0.0005(16) 0.0017(18) 0.0007(17) O14A 0.049(7) 0.028(5) 0.027(7) -0.002(5) 0.008(5) -0.005(4) O14B 0.064(7) 0.041(6) 0.036(8) 0.006(5) 0.009(5) -0.011(6) O15A 0.082(7) 0.055(5) 0.066(7) -0.012(5) 0.027(5) 0.028(5) O15B 0.133(7) 0.068(5) 0.045(6) -0.015(5) 0.033(5) -0.036(6) O16A 0.059(5) 0.069(6) 0.027(4) -0.004(4) 0.006(3) -0.037(4) O16B 0.089(6) 0.058(6) 0.093(8) 0.039(5) -0.050(6) -0.032(5) N1 0.019(2) 0.020(2) 0.030(3) 0.0008(18) 0.0093(19) 0.0023(17) N2 0.025(2) 0.026(2) 0.024(2) 0.0047(19) 0.0087(19) 0.0045(19) N3 0.020(2) 0.026(2) 0.023(2) -0.0021(18) 0.0059(19) 0.0027(18) N4 0.022(2) 0.016(2) 0.023(2) -0.0001(17) 0.0040(18) 0.0004(17) N5 0.031(3) 0.016(2) 0.036(3) 0.0030(19) 0.017(2) 0.0044(18) N6 0.029(3) 0.034(3) 0.027(3) 0.009(2) 0.006(2) 0.002(2) N7 0.017(2) 0.023(2) 0.038(3) 0.001(2) 0.008(2) 0.0017(18) N8 0.022(2) 0.020(2) 0.036(3) 0.001(2) 0.003(2) 0.0049(18) N9 0.023(2) 0.016(2) 0.025(2) 0.0026(17) 0.0078(19) 0.0002(17) N10 0.019(2) 0.020(2) 0.029(3) -0.0041(18) 0.0033(19) 0.0018(17) N11 0.034(3) 0.029(3) 0.028(3) 0.005(2) -0.002(2) 0.009(2) N12 0.033(3) 0.017(2) 0.044(3) -0.001(2) 0.017(2) 0.0020(19) C5 0.035(3) 0.020(3) 0.021(3) 0.001(2) 0.015(2) 0.000(2) C6 0.058(4) 0.018(3) 0.037(3) -0.004(2) 0.022(3) -0.005(3) C7 0.030(3) 0.016(2) 0.022(3) 0.001(2) 0.007(2) -0.005(2) C8 0.047(4) 0.036(3) 0.024(3) 0.006(3) 0.013(3) -0.002(3) C11 0.030(3) 0.023(3) 0.032(3) 0.004(2) 0.012(2) 0.000(2) C12 0.029(3) 0.024(3) 0.046(4) -0.010(3) 0.012(3) -0.005(2) C13 0.031(3) 0.022(3) 0.059(4) 0.000(3) 0.016(3) -0.001(2) C14 0.032(3) 0.026(3) 0.045(4) 0.010(3) 0.017(3) 0.005(2) C15 0.021(3) 0.025(3) 0.035(3) 0.007(2) 0.010(2) 0.003(2) C16 0.024(3) 0.032(3) 0.021(3) 0.005(2) 0.006(2) 0.006(2) C17 0.044(4) 0.035(3) 0.034(3) 0.013(3) 0.013(3) 0.011(3) C18 0.047(4) 0.059(4) 0.023(3) 0.012(3) 0.011(3) 0.018(3) C19 0.035(3) 0.048(4) 0.025(3) -0.001(3) 0.008(3) 0.012(3) C20 0.029(3) 0.037(3) 0.028(3) -0.001(3) 0.003(2) 0.004(3) C21 0.027(3) 0.042(3) 0.025(3) -0.006(2) 0.012(2) -0.003(2) C22 0.036(3) 0.044(4) 0.031(3) -0.014(3) 0.013(3) -0.006(3) C23 0.031(3) 0.029(3) 0.044(4) -0.016(3) 0.008(3) 0.001(2) C24 0.028(3) 0.021(3) 0.035(3) -0.006(2) 0.008(2) -0.001(2) C25 0.020(3) 0.020(3) 0.024(3) -0.005(2) 0.005(2) 0.000(2) C26 0.019(3) 0.020(3) 0.025(3) -0.003(2) 0.007(2) 0.000(2) C27 0.027(3) 0.022(3) 0.027(3) -0.001(2) 0.006(2) -0.003(2) C28 0.035(3) 0.025(3) 0.024(3) 0.003(2) 0.010(2) 0.003(2) C29 0.029(3) 0.028(3) 0.024(3) -0.006(2) 0.008(2) -0.003(2) C30 0.021(3) 0.020(3) 0.026(3) -0.005(2) 0.009(2) 0.004(2) C35 0.049(4) 0.010(2) 0.024(3) -0.003(2) 0.006(3) -0.002(2) C36 0.073(5) 0.024(3) 0.025(3) 0.005(2) 0.008(3) 0.001(3) C37 0.039(3) 0.015(2) 0.024(3) 0.000(2) 0.014(2) 0.001(2) C38 0.051(4) 0.020(3) 0.044(4) -0.006(3) 0.028(3) -0.004(3) C41 0.023(3) 0.028(3) 0.037(3) -0.004(2) 0.003(2) 0.001(2) C42 0.021(3) 0.031(3) 0.036(3) 0.003(3) -0.005(2) 0.004(2) C43 0.030(3) 0.035(3) 0.035(3) 0.010(3) 0.004(3) 0.005(3) C44 0.024(3) 0.025(3) 0.046(4) 0.007(3) 0.008(3) 0.005(2) C45 0.017(3) 0.019(3) 0.039(3) -0.001(2) 0.004(2) 0.001(2) C46 0.016(3) 0.023(3) 0.043(4) -0.001(2) 0.005(2) 0.002(2) C47 0.030(3) 0.019(3) 0.053(4) 0.002(3) 0.009(3) 0.002(2) C48 0.036(4) 0.018(3) 0.065(5) -0.013(3) 0.008(3) 0.000(2) C49 0.037(4) 0.031(3) 0.044(4) -0.013(3) 0.004(3) 0.008(3) C50 0.031(3) 0.029(3) 0.039(4) -0.004(3) 0.005(3) 0.004(2) C51 0.024(3) 0.023(3) 0.023(3) -0.003(2) 0.009(2) -0.002(2) C52 0.035(3) 0.029(3) 0.025(3) -0.004(2) 0.014(2) -0.001(2) C53 0.040(3) 0.028(3) 0.031(3) 0.006(2) 0.018(3) 0.002(2) C54 0.030(3) 0.019(3) 0.033(3) 0.006(2) 0.011(2) -0.003(2) C55 0.017(3) 0.019(3) 0.030(3) 0.000(2) 0.008(2) 0.000(2) C56 0.017(3) 0.020(3) 0.028(3) 0.001(2) 0.005(2) 0.000(2) C57 0.024(3) 0.021(3) 0.031(3) 0.001(2) 0.006(2) -0.001(2) C58 0.026(3) 0.013(2) 0.041(3) -0.001(2) 0.005(2) -0.003(2) C59 0.027(3) 0.021(3) 0.034(3) -0.010(2) 0.003(2) 0.001(2) C60 0.028(3) 0.023(3) 0.025(3) 0.000(2) 0.003(2) 0.001(2) C61 0.070(5) 0.023(3) 0.018(3) 0.001(2) 0.003(3) 0.000(3) C62 0.059(4) 0.021(3) 0.021(3) -0.002(2) 0.015(3) -0.006(3) C63 0.053(4) 0.026(3) 0.018(3) 0.004(2) 0.005(3) 0.010(3) C64A 0.078(5) 0.039(5) 0.034(4) -0.007(4) 0.019(3) -0.020(4) C64B 0.074(5) 0.033(5) 0.030(5) -0.001(3) 0.013(4) -0.013(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 N1 1.997(4) . ? Pd1 N2 2.003(4) . ? Pd1 O1 2.009(4) . ? Pd1 O2 2.046(4) . ? Pd1 Pd2 2.8385(7) . ? Pd2 N6 1.999(5) . ? Pd2 N5 2.015(5) . ? Pd2 N4 2.030(4) . ? Pd2 N3 2.039(4) . ? Pd3 N11 2.003(5) . ? Pd3 N12 2.004(5) . ? Pd3 N8 2.022(5) . ? Pd3 N7 2.045(5) . ? Pd3 Pd4 2.8365(7) . ? Pd4 N10 1.992(4) . ? Pd4 N9 2.000(4) . ? Pd4 O4 2.012(3) . ? Pd4 O3 2.018(4) . ? S1 O5 1.437(5) . ? S1 O6 1.441(5) . ? S1 O7 1.443(4) . ? S1 C61 1.776(7) . ? S2 O10 1.437(5) . ? S2 O9 1.438(4) . ? S2 O8 1.442(4) . ? S2 C62 1.842(7) . ? S3 O11 1.442(4) . ? S3 O12 1.442(4) . ? S3 O13 1.455(4) . ? S3 C63 1.817(7) . ? S4A O14A 1.38(2) . ? S4A O15A 1.437(11) . ? S4A O16A 1.438(11) . ? S4A C64A 1.78(2) . ? S4B O16B 1.257(15) . ? S4B O14B 1.55(2) . ? S4B O15B 1.587(16) . ? S4B C64B 1.795(19) . ? F1 C61 1.355(7) . ? F2 C61 1.359(7) . ? F3 C61 1.355(7) . ? F4 C62 1.333(7) . ? F5 C62 1.342(6) . ? F6 C62 1.335(7) . ? F7 C63 1.344(6) . ? F8 C63 1.327(7) . ? F9 C63 1.340(7) . ? F10A C64A 1.32(2) . ? F10B C64B 1.40(3) . ? F11A C64A 1.34(3) . ? F11B C64B 1.33(3) . ? F12A C64A 1.34(4) . ? F12B C64B 1.30(4) . ? O1 C5 1.288(6) . ? O2 C7 1.282(6) . ? O3 C35 1.299(7) . ? O4 C37 1.294(6) . ? N1 C11 1.333(7) . ? N1 C15 1.364(7) . ? N2 C20 1.346(7) . ? N2 C16 1.362(7) . ? N3 C21 1.333(7) . ? N3 C25 1.358(7) . ? N4 C30 1.347(7) . ? N4 C26 1.353(7) . ? N5 C5 1.292(7) . ? N5 H5A 0.8800 . ? N6 C7 1.300(7) . ? N6 H6A 0.8800 . ? N7 C41 1.350(7) . ? N7 C45 1.361(7) . ? N8 C50 1.339(8) . ? N8 C46 1.365(7) . ? N9 C51 1.347(7) . ? N9 C55 1.361(7) . ? N10 C60 1.341(7) . ? N10 C56 1.362(7) . ? N11 C35 1.287(8) . ? N11 H11A 0.8800 . ? N12 C37 1.286(7) . ? N12 H12A 0.8800 . ? C5 C6 1.504(7) . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C6 H6D 0.9800 . ? C7 C8 1.521(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 C12 1.398(8) . ? C11 H11B 0.9500 . ? C12 C13 1.388(9) . ? C12 H12B 0.9500 . ? C13 C14 1.388(9) . ? C13 H13A 0.9500 . ? C14 C15 1.394(8) . ? C14 H14A 0.9500 . ? C15 C16 1.468(8) . ? C16 C17 1.390(8) . ? C17 C18 1.387(9) . ? C17 H17A 0.9500 . ? C18 C19 1.381(9) . ? C18 H18A 0.9500 . ? C19 C20 1.377(8) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.398(8) . ? C21 H21A 0.9500 . ? C22 C23 1.376(9) . ? C22 H22A 0.9500 . ? C23 C24 1.387(8) . ? C23 H23A 0.9500 . ? C24 C25 1.405(7) . ? C24 H24A 0.9500 . ? C25 C26 1.477(7) . ? C26 C27 1.389(7) . ? C27 C28 1.383(8) . ? C27 H27A 0.9500 . ? C28 C29 1.404(8) . ? C28 H28A 0.9500 . ? C29 C30 1.373(8) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C35 C36 1.510(8) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.508(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C41 C42 1.380(9) . ? C41 H41A 0.9500 . ? C42 C43 1.385(8) . ? C42 H42A 0.9500 . ? C43 C44 1.385(9) . ? C43 H43A 0.9500 . ? C44 C45 1.395(8) . ? C44 H44A 0.9500 . ? C45 C46 1.481(8) . ? C46 C47 1.388(8) . ? C47 C48 1.390(9) . ? C47 H47A 0.9500 . ? C48 C49 1.387(10) . ? C48 H48A 0.9500 . ? C49 C50 1.374(8) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C52 1.376(8) . ? C51 H51A 0.9500 . ? C52 C53 1.397(8) . ? C52 H52A 0.9500 . ? C53 C54 1.383(8) . ? C53 H53A 0.9500 . ? C54 C55 1.389(8) . ? C54 H54A 0.9500 . ? C55 C56 1.482(7) . ? C56 C57 1.387(7) . ? C57 C58 1.383(8) . ? C57 H57A 0.9500 . ? C58 C59 1.391(8) . ? C58 H58A 0.9500 . ? C59 C60 1.391(7) . ? C59 H59A 0.9500 . ? C60 H60A 0.9500 . ? 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 N2 81.29(18) . . ? N1 Pd1 O1 174.25(17) . . ? N2 Pd1 O1 93.00(17) . . ? N1 Pd1 O2 95.03(16) . . ? N2 Pd1 O2 175.12(16) . . ? O1 Pd1 O2 90.64(15) . . ? N1 Pd1 Pd2 98.72(12) . . ? N2 Pd1 Pd2 105.31(13) . . ? O1 Pd1 Pd2 83.37(11) . . ? O2 Pd1 Pd2 78.33(10) . . ? N6 Pd2 N5 87.25(19) . . ? N6 Pd2 N4 172.88(18) . . ? N5 Pd2 N4 97.00(18) . . ? N6 Pd2 N3 94.71(19) . . ? N5 Pd2 N3 177.11(18) . . ? N4 Pd2 N3 80.84(17) . . ? N6 Pd2 Pd1 85.13(14) . . ? N5 Pd2 Pd1 80.42(13) . . ? N4 Pd2 Pd1 89.94(12) . . ? N3 Pd2 Pd1 97.61(12) . . ? N11 Pd3 N12 86.3(2) . . ? N11 Pd3 N8 95.9(2) . . ? N12 Pd3 N8 176.1(2) . . ? N11 Pd3 N7 175.82(19) . . ? N12 Pd3 N7 97.31(19) . . ? N8 Pd3 N7 80.41(19) . . ? N11 Pd3 Pd4 81.07(14) . . ? N12 Pd3 Pd4 81.71(14) . . ? N8 Pd3 Pd4 95.41(13) . . ? N7 Pd3 Pd4 97.26(12) . . ? N10 Pd4 N9 81.09(18) . . ? N10 Pd4 O4 174.44(17) . . ? N9 Pd4 O4 94.53(16) . . ? N10 Pd4 O3 94.41(17) . . ? N9 Pd4 O3 175.49(16) . . ? O4 Pd4 O3 89.95(15) . . ? N10 Pd4 Pd3 101.54(12) . . ? N9 Pd4 Pd3 98.24(12) . . ? O4 Pd4 Pd3 82.41(10) . . ? O3 Pd4 Pd3 82.87(11) . . ? O5 S1 O6 115.2(3) . . ? O5 S1 O7 115.9(3) . . ? O6 S1 O7 114.7(3) . . ? O5 S1 C61 102.8(3) . . ? O6 S1 C61 101.6(3) . . ? O7 S1 C61 103.9(3) . . ? O10 S2 O9 115.2(3) . . ? O10 S2 O8 114.8(3) . . ? O9 S2 O8 115.2(3) . . ? O10 S2 C62 103.5(3) . . ? O9 S2 C62 103.2(3) . . ? O8 S2 C62 102.5(3) . . ? O11 S3 O12 115.1(2) . . ? O11 S3 O13 114.7(2) . . ? O12 S3 O13 115.1(2) . . ? O11 S3 C63 103.7(3) . . ? O12 S3 C63 103.3(3) . . ? O13 S3 C63 102.5(3) . . ? O14A S4A O15A 115.4(10) . . ? O14A S4A O16A 118.2(8) . . ? O15A S4A O16A 111.0(8) . . ? O14A S4A C64A 104.3(11) . . ? O15A S4A C64A 103.2(10) . . ? O16A S4A C64A 102.3(9) . . ? O16B S4B O14B 118.8(11) . . ? O16B S4B O15B 123.7(11) . . ? O14B S4B O15B 102.6(13) . . ? O16B S4B C64B 108.3(12) . . ? O14B S4B C64B 102.8(11) . . ? O15B S4B C64B 96.8(10) . . ? C5 O1 Pd1 123.6(3) . . ? C7 O2 Pd1 126.5(3) . . ? C35 O3 Pd4 123.4(4) . . ? C37 O4 Pd4 124.8(3) . . ? C11 N1 C15 120.3(5) . . ? C11 N1 Pd1 125.2(4) . . ? C15 N1 Pd1 114.4(4) . . ? C20 N2 C16 119.9(5) . . ? C20 N2 Pd1 125.3(4) . . ? C16 N2 Pd1 114.7(4) . . ? C21 N3 C25 120.6(5) . . ? C21 N3 Pd2 125.4(4) . . ? C25 N3 Pd2 114.0(3) . . ? C30 N4 C26 119.5(5) . . ? C30 N4 Pd2 125.7(4) . . ? C26 N4 Pd2 114.2(3) . . ? C5 N5 Pd2 126.6(4) . . ? C5 N5 H5A 116.7 . . ? Pd2 N5 H5A 116.7 . . ? C7 N6 Pd2 121.4(4) . . ? C7 N6 H6A 119.3 . . ? Pd2 N6 H6A 119.3 . . ? C41 N7 C45 119.7(5) . . ? C41 N7 Pd3 125.9(4) . . ? C45 N7 Pd3 114.4(4) . . ? C50 N8 C46 119.3(5) . . ? C50 N8 Pd3 125.3(4) . . ? C46 N8 Pd3 115.4(4) . . ? C51 N9 C55 119.8(5) . . ? C51 N9 Pd4 125.2(4) . . ? C55 N9 Pd4 114.9(4) . . ? C60 N10 C56 119.8(5) . . ? C60 N10 Pd4 124.7(4) . . ? C56 N10 Pd4 115.5(3) . . ? C35 N11 Pd3 127.2(4) . . ? C35 N11 H11A 116.4 . . ? Pd3 N11 H11A 116.4 . . ? C37 N12 Pd3 126.0(4) . . ? C37 N12 H12A 117.0 . . ? Pd3 N12 H12A 117.0 . . ? O1 C5 N5 124.8(5) . . ? O1 C5 C6 114.3(5) . . ? N5 C5 C6 120.9(5) . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C6 H6D 109.5 . . ? H6B C6 H6D 109.5 . . ? H6C C6 H6D 109.5 . . ? O2 C7 N6 124.9(5) . . ? O2 C7 C8 114.8(5) . . ? N6 C7 C8 120.3(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C11 C12 121.7(5) . . ? N1 C11 H11B 119.2 . . ? C12 C11 H11B 119.2 . . ? C13 C12 C11 118.3(6) . . ? C13 C12 H12B 120.9 . . ? C11 C12 H12B 120.9 . . ? C12 C13 C14 120.3(6) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C13 C14 C15 118.6(6) . . ? C13 C14 H14A 120.7 . . ? C15 C14 H14A 120.7 . . ? N1 C15 C14 120.8(5) . . ? N1 C15 C16 115.1(5) . . ? C14 C15 C16 124.1(5) . . ? N2 C16 C17 120.5(5) . . ? N2 C16 C15 114.2(5) . . ? C17 C16 C15 125.2(5) . . ? C18 C17 C16 118.7(6) . . ? C18 C17 H17A 120.6 . . ? C16 C17 H17A 120.6 . . ? C19 C18 C17 120.4(6) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C20 C19 C18 118.5(6) . . ? C20 C19 H19A 120.8 . . ? C18 C19 H19A 120.8 . . ? N2 C20 C19 122.0(6) . . ? N2 C20 H20A 119.0 . . ? C19 C20 H20A 119.0 . . ? N3 C21 C22 121.1(6) . . ? N3 C21 H21A 119.5 . . ? C22 C21 H21A 119.5 . . ? C23 C22 C21 119.4(6) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? C22 C23 C24 119.5(5) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C23 C24 C25 119.0(5) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? N3 C25 C24 120.4(5) . . ? N3 C25 C26 115.2(4) . . ? C24 C25 C26 124.4(5) . . ? N4 C26 C27 121.3(5) . . ? N4 C26 C25 115.5(5) . . ? C27 C26 C25 123.2(5) . . ? C28 C27 C26 119.2(5) . . ? C28 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? C27 C28 C29 118.9(5) . . ? C27 C28 H28A 120.6 . . ? C29 C28 H28A 120.6 . . ? C30 C29 C28 119.1(5) . . ? C30 C29 H29A 120.5 . . ? C28 C29 H29A 120.5 . . ? N4 C30 C29 121.9(5) . . ? N4 C30 H30A 119.1 . . ? C29 C30 H30A 119.1 . . ? N11 C35 O3 124.1(5) . . ? N11 C35 C36 121.1(6) . . ? O3 C35 C36 114.7(5) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N12 C37 O4 124.5(5) . . ? N12 C37 C38 120.6(5) . . ? O4 C37 C38 114.9(5) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N7 C41 C42 121.3(5) . . ? N7 C41 H41A 119.4 . . ? C42 C41 H41A 119.4 . . ? C41 C42 C43 120.2(6) . . ? C41 C42 H42A 119.9 . . ? C43 C42 H42A 119.9 . . ? C42 C43 C44 118.4(6) . . ? C42 C43 H43A 120.8 . . ? C44 C43 H43A 120.8 . . ? C43 C44 C45 119.9(5) . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? N7 C45 C44 120.6(5) . . ? N7 C45 C46 115.2(5) . . ? C44 C45 C46 124.2(5) . . ? N8 C46 C47 121.4(6) . . ? N8 C46 C45 114.4(5) . . ? C47 C46 C45 124.2(6) . . ? C46 C47 C48 118.5(6) . . ? C46 C47 H47A 120.8 . . ? C48 C47 H47A 120.8 . . ? C49 C48 C47 119.5(6) . . ? C49 C48 H48A 120.2 . . ? C47 C48 H48A 120.2 . . ? C50 C49 C48 119.3(6) . . ? C50 C49 H49A 120.4 . . ? C48 C49 H49A 120.4 . . ? N8 C50 C49 122.0(6) . . ? N8 C50 H50A 119.0 . . ? C49 C50 H50A 119.0 . . ? N9 C51 C52 121.9(5) . . ? N9 C51 H51A 119.1 . . ? C52 C51 H51A 119.1 . . ? C51 C52 C53 118.7(5) . . ? C51 C52 H52A 120.6 . . ? C53 C52 H52A 120.6 . . ? C54 C53 C52 119.6(5) . . ? C54 C53 H53A 120.2 . . ? C52 C53 H53A 120.2 . . ? C53 C54 C55 119.1(5) . . ? C53 C54 H54A 120.4 . . ? C55 C54 H54A 120.4 . . ? N9 C55 C54 120.8(5) . . ? N9 C55 C56 114.4(5) . . ? C54 C55 C56 124.8(5) . . ? N10 C56 C57 121.6(5) . . ? N10 C56 C55 113.9(4) . . ? C57 C56 C55 124.5(5) . . ? C58 C57 C56 118.4(5) . . ? C58 C57 H57A 120.8 . . ? C56 C57 H57A 120.8 . . ? C57 C58 C59 120.2(5) . . ? C57 C58 H58A 119.9 . . ? C59 C58 H58A 119.9 . . ? C60 C59 C58 118.7(5) . . ? C60 C59 H59A 120.7 . . ? C58 C59 H59A 120.7 . . ? N10 C60 C59 121.4(5) . . ? N10 C60 H60A 119.3 . . ? C59 C60 H60A 119.3 . . ? F1 C61 F3 106.1(5) . . ? F1 C61 F2 105.4(5) . . ? F3 C61 F2 105.2(5) . . ? F1 C61 S1 112.9(5) . . ? F3 C61 S1 113.4(4) . . ? F2 C61 S1 113.1(5) . . ? F4 C62 F6 107.6(5) . . ? F4 C62 F5 107.8(5) . . ? F6 C62 F5 107.5(5) . . ? F4 C62 S2 111.4(4) . . ? F6 C62 S2 112.1(4) . . ? F5 C62 S2 110.2(4) . . ? F8 C63 F9 107.8(5) . . ? F8 C63 F7 107.9(5) . . ? F9 C63 F7 106.2(4) . . ? F8 C63 S3 112.2(4) . . ? F9 C63 S3 111.1(4) . . ? F7 C63 S3 111.3(4) . . ? F10A C64A F11A 108.7(19) . . ? F10A C64A F12A 109(2) . . ? F11A C64A F12A 103(3) . . ? F10A C64A S4A 110.7(17) . . ? F11A C64A S4A 111.9(12) . . ? F12A C64A S4A 113.5(19) . . ? F12B C64B F11B 109(3) . . ? F12B C64B F10B 109(2) . . ? F11B C64B F10B 105.4(17) . . ? F12B C64B S4B 113.4(18) . . ? F11B C64B S4B 108.1(13) . . ? F10B C64B S4B 112.0(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 N1 Pd1 Pd2 N6 104.78(19) . . . . ? N2 Pd1 Pd2 N6 -171.9(2) . . . . ? O1 Pd1 Pd2 N6 -80.63(18) . . . . ? O2 Pd1 Pd2 N6 11.41(17) . . . . ? N1 Pd1 Pd2 N5 -167.20(18) . . . . ? N2 Pd1 Pd2 N5 -83.91(19) . . . . ? O1 Pd1 Pd2 N5 7.40(17) . . . . ? O2 Pd1 Pd2 N5 99.43(17) . . . . ? N1 Pd1 Pd2 N4 -70.08(18) . . . . ? N2 Pd1 Pd2 N4 13.20(18) . . . . ? O1 Pd1 Pd2 N4 104.51(16) . . . . ? O2 Pd1 Pd2 N4 -163.46(16) . . . . ? N1 Pd1 Pd2 N3 10.67(18) . . . . ? N2 Pd1 Pd2 N3 93.96(19) . . . . ? O1 Pd1 Pd2 N3 -174.74(17) . . . . ? O2 Pd1 Pd2 N3 -82.70(16) . . . . ? N11 Pd3 Pd4 N10 -99.0(2) . . . . ? N12 Pd3 Pd4 N10 173.5(2) . . . . ? N8 Pd3 Pd4 N10 -3.89(19) . . . . ? N7 Pd3 Pd4 N10 77.09(19) . . . . ? N11 Pd3 Pd4 N9 178.44(19) . . . . ? N12 Pd3 Pd4 N9 90.94(19) . . . . ? N8 Pd3 Pd4 N9 -86.41(18) . . . . ? N7 Pd3 Pd4 N9 -5.43(18) . . . . ? N11 Pd3 Pd4 O4 84.93(18) . . . . ? N12 Pd3 Pd4 O4 -2.57(18) . . . . ? N8 Pd3 Pd4 O4 -179.92(18) . . . . ? N7 Pd3 Pd4 O4 -98.94(17) . . . . ? N11 Pd3 Pd4 O3 -5.98(18) . . . . ? N12 Pd3 Pd4 O3 -93.47(18) . . . . ? N8 Pd3 Pd4 O3 89.17(18) . . . . ? N7 Pd3 Pd4 O3 170.16(17) . . . . ? N1 Pd1 O1 C5 104.7(16) . . . . ? N2 Pd1 O1 C5 98.1(4) . . . . ? O2 Pd1 O1 C5 -85.2(4) . . . . ? Pd2 Pd1 O1 C5 -7.0(4) . . . . ? N1 Pd1 O2 C7 -117.7(4) . . . . ? N2 Pd1 O2 C7 -158.4(19) . . . . ? O1 Pd1 O2 C7 63.3(4) . . . . ? Pd2 Pd1 O2 C7 -19.8(4) . . . . ? N10 Pd4 O3 C35 112.9(4) . . . . ? N9 Pd4 O3 C35 116(2) . . . . ? O4 Pd4 O3 C35 -70.6(4) . . . . ? Pd3 Pd4 O3 C35 11.8(4) . . . . ? N10 Pd4 O4 C37 -136.3(16) . . . . ? N9 Pd4 O4 C37 -98.5(4) . . . . ? O3 Pd4 O4 C37 82.1(4) . . . . ? Pd3 Pd4 O4 C37 -0.8(4) . . . . ? N2 Pd1 N1 C11 178.2(5) . . . . ? O1 Pd1 N1 C11 171.5(14) . . . . ? O2 Pd1 N1 C11 1.5(4) . . . . ? Pd2 Pd1 N1 C11 -77.5(4) . . . . ? N2 Pd1 N1 C15 -3.9(4) . . . . ? O1 Pd1 N1 C15 -10.6(18) . . . . ? O2 Pd1 N1 C15 179.4(4) . . . . ? Pd2 Pd1 N1 C15 100.4(3) . . . . ? N1 Pd1 N2 C20 -178.4(5) . . . . ? O1 Pd1 N2 C20 0.9(5) . . . . ? O2 Pd1 N2 C20 -137.3(18) . . . . ? Pd2 Pd1 N2 C20 84.8(4) . . . . ? N1 Pd1 N2 C16 4.4(4) . . . . ? O1 Pd1 N2 C16 -176.3(4) . . . . ? O2 Pd1 N2 C16 45(2) . . . . ? Pd2 Pd1 N2 C16 -92.4(4) . . . . ? N6 Pd2 N3 C21 6.6(5) . . . . ? N5 Pd2 N3 C21 139(3) . . . . ? N4 Pd2 N3 C21 -179.0(5) . . . . ? Pd1 Pd2 N3 C21 92.3(4) . . . . ? N6 Pd2 N3 C25 -171.0(4) . . . . ? N5 Pd2 N3 C25 -38(4) . . . . ? N4 Pd2 N3 C25 3.4(4) . . . . ? Pd1 Pd2 N3 C25 -85.3(3) . . . . ? N6 Pd2 N4 C30 -124.4(14) . . . . ? N5 Pd2 N4 C30 2.0(4) . . . . ? N3 Pd2 N4 C30 -176.1(4) . . . . ? Pd1 Pd2 N4 C30 -78.4(4) . . . . ? N6 Pd2 N4 C26 47.2(16) . . . . ? N5 Pd2 N4 C26 173.6(4) . . . . ? N3 Pd2 N4 C26 -4.5(4) . . . . ? Pd1 Pd2 N4 C26 93.2(3) . . . . ? N6 Pd2 N5 C5 74.2(5) . . . . ? N4 Pd2 N5 C5 -100.0(5) . . . . ? N3 Pd2 N5 C5 -59(4) . . . . ? Pd1 Pd2 N5 C5 -11.3(4) . . . . ? N5 Pd2 N6 C7 -89.1(5) . . . . ? N4 Pd2 N6 C7 37.8(17) . . . . ? N3 Pd2 N6 C7 88.8(5) . . . . ? Pd1 Pd2 N6 C7 -8.5(4) . . . . ? N11 Pd3 N7 C41 153(2) . . . . ? N12 Pd3 N7 C41 4.8(5) . . . . ? N8 Pd3 N7 C41 -178.4(5) . . . . ? Pd4 Pd3 N7 C41 87.3(4) . . . . ? N11 Pd3 N7 C45 -25(3) . . . . ? N12 Pd3 N7 C45 -173.3(4) . . . . ? N8 Pd3 N7 C45 3.5(4) . . . . ? Pd4 Pd3 N7 C45 -90.8(3) . . . . ? N11 Pd3 N8 C50 -2.6(5) . . . . ? N12 Pd3 N8 C50 -126(3) . . . . ? N7 Pd3 N8 C50 179.4(5) . . . . ? Pd4 Pd3 N8 C50 -84.2(4) . . . . ? N11 Pd3 N8 C46 173.9(4) . . . . ? N12 Pd3 N8 C46 50(3) . . . . ? N7 Pd3 N8 C46 -4.2(4) . . . . ? Pd4 Pd3 N8 C46 92.3(4) . . . . ? N10 Pd4 N9 C51 177.9(4) . . . . ? O4 Pd4 N9 C51 1.4(4) . . . . ? O3 Pd4 N9 C51 174.5(19) . . . . ? Pd3 Pd4 N9 C51 -81.6(4) . . . . ? N10 Pd4 N9 C55 -4.5(4) . . . . ? O4 Pd4 N9 C55 178.9(4) . . . . ? O3 Pd4 N9 C55 -8(2) . . . . ? Pd3 Pd4 N9 C55 96.0(3) . . . . ? N9 Pd4 N10 C60 -175.7(5) . . . . ? O4 Pd4 N10 C60 -137.5(16) . . . . ? O3 Pd4 N10 C60 4.0(4) . . . . ? Pd3 Pd4 N10 C60 87.6(4) . . . . ? N9 Pd4 N10 C56 3.2(4) . . . . ? O4 Pd4 N10 C56 41.5(19) . . . . ? O3 Pd4 N10 C56 -177.0(4) . . . . ? Pd3 Pd4 N10 C56 -93.4(4) . . . . ? N12 Pd3 N11 C35 84.9(5) . . . . ? N8 Pd3 N11 C35 -91.9(5) . . . . ? N7 Pd3 N11 C35 -64(3) . . . . ? Pd4 Pd3 N11 C35 2.7(5) . . . . ? N11 Pd3 N12 C37 -74.3(5) . . . . ? N8 Pd3 N12 C37 50(3) . . . . ? N7 Pd3 N12 C37 103.5(5) . . . . ? Pd4 Pd3 N12 C37 7.2(5) . . . . ? Pd1 O1 C5 N5 1.1(7) . . . . ? Pd1 O1 C5 C6 -176.6(3) . . . . ? Pd2 N5 C5 O1 10.1(8) . . . . ? Pd2 N5 C5 C6 -172.3(4) . . . . ? Pd1 O2 C7 N6 20.9(7) . . . . ? Pd1 O2 C7 C8 -160.2(4) . . . . ? Pd2 N6 C7 O2 -3.3(8) . . . . ? Pd2 N6 C7 C8 177.8(4) . . . . ? C15 N1 C11 C12 1.0(8) . . . . ? Pd1 N1 C11 C12 178.8(4) . . . . ? N1 C11 C12 C13 -0.9(9) . . . . ? C11 C12 C13 C14 0.6(9) . . . . ? C12 C13 C14 C15 -0.3(9) . . . . ? C11 N1 C15 C14 -0.6(8) . . . . ? Pd1 N1 C15 C14 -178.7(4) . . . . ? C11 N1 C15 C16 -179.2(5) . . . . ? Pd1 N1 C15 C16 2.8(6) . . . . ? C13 C14 C15 N1 0.3(8) . . . . ? C13 C14 C15 C16 178.7(5) . . . . ? C20 N2 C16 C17 -1.0(8) . . . . ? Pd1 N2 C16 C17 176.4(4) . . . . ? C20 N2 C16 C15 178.6(5) . . . . ? Pd1 N2 C16 C15 -4.1(6) . . . . ? N1 C15 C16 N2 0.9(7) . . . . ? C14 C15 C16 N2 -177.7(5) . . . . ? N1 C15 C16 C17 -179.6(5) . . . . ? C14 C15 C16 C17 1.9(9) . . . . ? N2 C16 C17 C18 0.1(9) . . . . ? C15 C16 C17 C18 -179.4(6) . . . . ? C16 C17 C18 C19 1.3(10) . . . . ? C17 C18 C19 C20 -1.8(10) . . . . ? C16 N2 C20 C19 0.5(8) . . . . ? Pd1 N2 C20 C19 -176.6(4) . . . . ? C18 C19 C20 N2 0.9(9) . . . . ? C25 N3 C21 C22 2.4(8) . . . . ? Pd2 N3 C21 C22 -175.0(4) . . . . ? N3 C21 C22 C23 -2.5(9) . . . . ? C21 C22 C23 C24 1.2(9) . . . . ? C22 C23 C24 C25 0.2(9) . . . . ? C21 N3 C25 C24 -1.0(8) . . . . ? Pd2 N3 C25 C24 176.7(4) . . . . ? C21 N3 C25 C26 -179.6(5) . . . . ? Pd2 N3 C25 C26 -1.8(6) . . . . ? C23 C24 C25 N3 -0.3(8) . . . . ? C23 C24 C25 C26 178.1(5) . . . . ? C30 N4 C26 C27 -2.1(7) . . . . ? Pd2 N4 C26 C27 -174.3(4) . . . . ? C30 N4 C26 C25 177.0(4) . . . . ? Pd2 N4 C26 C25 4.8(6) . . . . ? N3 C25 C26 N4 -2.0(7) . . . . ? C24 C25 C26 N4 179.5(5) . . . . ? N3 C25 C26 C27 177.1(5) . . . . ? C24 C25 C26 C27 -1.4(8) . . . . ? N4 C26 C27 C28 4.4(8) . . . . ? C25 C26 C27 C28 -174.6(5) . . . . ? C26 C27 C28 C29 -3.7(8) . . . . ? C27 C28 C29 C30 0.9(8) . . . . ? C26 N4 C30 C29 -0.8(8) . . . . ? Pd2 N4 C30 C29 170.3(4) . . . . ? C28 C29 C30 N4 1.5(8) . . . . ? Pd3 N11 C35 O3 5.4(8) . . . . ? Pd3 N11 C35 C36 -176.4(4) . . . . ? Pd4 O3 C35 N11 -14.1(7) . . . . ? Pd4 O3 C35 C36 167.6(4) . . . . ? Pd3 N12 C37 O4 -10.4(8) . . . . ? Pd3 N12 C37 C38 170.9(4) . . . . ? Pd4 O4 C37 N12 6.4(8) . . . . ? Pd4 O4 C37 C38 -174.8(4) . . . . ? C45 N7 C41 C42 0.5(8) . . . . ? Pd3 N7 C41 C42 -177.5(4) . . . . ? N7 C41 C42 C43 -1.0(8) . . . . ? C41 C42 C43 C44 0.7(8) . . . . ? C42 C43 C44 C45 0.1(8) . . . . ? C41 N7 C45 C44 0.3(8) . . . . ? Pd3 N7 C45 C44 178.5(4) . . . . ? C41 N7 C45 C46 179.4(5) . . . . ? Pd3 N7 C45 C46 -2.3(6) . . . . ? C43 C44 C45 N7 -0.6(8) . . . . ? C43 C44 C45 C46 -179.6(5) . . . . ? C50 N8 C46 C47 0.6(8) . . . . ? Pd3 N8 C46 C47 -176.1(4) . . . . ? C50 N8 C46 C45 -179.2(5) . . . . ? Pd3 N8 C46 C45 4.1(6) . . . . ? N7 C45 C46 N8 -1.1(7) . . . . ? C44 C45 C46 N8 178.0(5) . . . . ? N7 C45 C46 C47 179.1(5) . . . . ? C44 C45 C46 C47 -1.8(9) . . . . ? N8 C46 C47 C48 -0.3(8) . . . . ? C45 C46 C47 C48 179.5(5) . . . . ? C46 C47 C48 C49 0.3(9) . . . . ? C47 C48 C49 C50 -0.6(9) . . . . ? C46 N8 C50 C49 -0.9(8) . . . . ? Pd3 N8 C50 C49 175.4(4) . . . . ? C48 C49 C50 N8 0.9(9) . . . . ? C55 N9 C51 C52 -0.3(8) . . . . ? Pd4 N9 C51 C52 177.2(4) . . . . ? N9 C51 C52 C53 -1.0(8) . . . . ? C51 C52 C53 C54 0.8(9) . . . . ? C52 C53 C54 C55 0.6(9) . . . . ? C51 N9 C55 C54 1.7(7) . . . . ? Pd4 N9 C55 C54 -176.0(4) . . . . ? C51 N9 C55 C56 -177.3(4) . . . . ? Pd4 N9 C55 C56 5.0(6) . . . . ? C53 C54 C55 N9 -1.9(8) . . . . ? C53 C54 C55 C56 177.1(5) . . . . ? C60 N10 C56 C57 0.6(8) . . . . ? Pd4 N10 C56 C57 -178.5(4) . . . . ? C60 N10 C56 C55 177.5(5) . . . . ? Pd4 N10 C56 C55 -1.5(6) . . . . ? N9 C55 C56 N10 -2.3(6) . . . . ? C54 C55 C56 N10 178.7(5) . . . . ? N9 C55 C56 C57 174.6(5) . . . . ? C54 C55 C56 C57 -4.4(8) . . . . ? N10 C56 C57 C58 0.0(8) . . . . ? C55 C56 C57 C58 -176.7(5) . . . . ? C56 C57 C58 C59 -0.7(8) . . . . ? C57 C58 C59 C60 0.9(8) . . . . ? C56 N10 C60 C59 -0.3(8) . . . . ? Pd4 N10 C60 C59 178.6(4) . . . . ? C58 C59 C60 N10 -0.4(8) . . . . ? O5 S1 C61 F1 59.2(5) . . . . ? O6 S1 C61 F1 -60.3(5) . . . . ? O7 S1 C61 F1 -179.6(4) . . . . ? O5 S1 C61 F3 179.9(4) . . . . ? O6 S1 C61 F3 60.4(5) . . . . ? O7 S1 C61 F3 -58.9(5) . . . . ? O5 S1 C61 F2 -60.4(5) . . . . ? O6 S1 C61 F2 -179.9(4) . . . . ? O7 S1 C61 F2 60.8(5) . . . . ? O10 S2 C62 F4 -179.7(4) . . . . ? O9 S2 C62 F4 60.0(5) . . . . ? O8 S2 C62 F4 -60.0(5) . . . . ? O10 S2 C62 F6 59.7(4) . . . . ? O9 S2 C62 F6 -60.6(4) . . . . ? O8 S2 C62 F6 179.4(4) . . . . ? O10 S2 C62 F5 -60.0(4) . . . . ? O9 S2 C62 F5 179.6(4) . . . . ? O8 S2 C62 F5 59.6(4) . . . . ? O11 S3 C63 F8 61.9(5) . . . . ? O12 S3 C63 F8 -177.6(4) . . . . ? O13 S3 C63 F8 -57.7(5) . . . . ? O11 S3 C63 F9 -177.3(4) . . . . ? O12 S3 C63 F9 -56.8(4) . . . . ? O13 S3 C63 F9 63.0(4) . . . . ? O11 S3 C63 F7 -59.1(4) . . . . ? O12 S3 C63 F7 61.4(4) . . . . ? O13 S3 C63 F7 -178.7(4) . . . . ? O14A S4A C64A F10A 62.6(18) . . . . ? O15A S4A C64A F10A -58.3(17) . . . . ? O16A S4A C64A F10A -173.7(15) . . . . ? O14A S4A C64A F11A -58.8(18) . . . . ? O15A S4A C64A F11A -179.8(15) . . . . ? O16A S4A C64A F11A 64.9(17) . . . . ? O14A S4A C64A F12A -175(3) . . . . ? O15A S4A C64A F12A 64(3) . . . . ? O16A S4A C64A F12A -51(3) . . . . ? O16B S4B C64B F12B -61(3) . . . . ? O14B S4B C64B F12B 172(3) . . . . ? O15B S4B C64B F12B 68(3) . . . . ? O16B S4B C64B F11B 59.2(19) . . . . ? O14B S4B C64B F11B -67(2) . . . . ? O15B S4B C64B F11B -171.8(16) . . . . ? O16B S4B C64B F10B 174.9(15) . . . . ? O14B S4B C64B F10B 48(2) . . . . ? O15B S4B C64B F10B -56.2(17) . . . . ? 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 N5 H5A O6 0.88 2.37 3.058(6) 134.9 . N6 H6A O7 0.88 2.66 3.432(7) 147.1 . N11 H11A O11 0.88 2.33 3.098(6) 145.6 . N12 H12A O13 0.88 2.43 3.117(6) 135.2 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.082 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.173 # Attachment 'JW-Complex 5.CIF' data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 648490' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H23 N7 O9 Pd2' _chemical_formula_sum 'C6 H23 N7 O9 Pd2' _chemical_formula_weight 550.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 11.052(2) _cell_length_b 10.813(2) _cell_length_c 14.687(3) _cell_angle_alpha 90 _cell_angle_beta 105.70(3) _cell_angle_gamma 90 _cell_volume 1689.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 6366 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 2.186 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type AFC12\K/SATURN724 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1' _diffrn_reflns_number 30834 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_av_sigmaI/netI 0.032 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.4 _diffrn_reflns_theta_max 26.5 _reflns_number_total 3468 _reflns_number_gt 3310 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976) & DIAMOND (Crystal Impact, 2006)' _computing_publication_material SHELXL97 _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^)+(0.0286P)^2^+5.1374P] 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 3766 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.043 _refine_ls_R_factor_gt 0.039 _refine_ls_wR_factor_ref 0.079 _refine_ls_wR_factor_gt 0.077 _refine_ls_goodness_of_fit_ref 1.17 _refine_ls_restrained_S_all 1.17 _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 0.13877(3) 0.27165(3) 0.21772(2) 0.01062(9) Uani 1 1 d . . . Pd2 Pd 0.13286(3) -0.00863(3) 0.16499(2) 0.01102(9) Uani 1 1 d . . . O2 O 0.2201(2) 0.1100(2) 0.26737(18) 0.0133(5) Uani 1 1 d . . . H1 H 0.2833 0.0938 0.3244 0.020 Uiso 1 1 d R . . O1 O 0.2406(3) 0.2745(2) 0.12162(19) 0.0151(6) Uani 1 1 d . . . N1 N 0.0512(3) 0.4324(3) 0.1676(2) 0.0129(6) Uani 1 1 d . . . H1A H 0.1075 0.4863 0.1530 0.015 Uiso 1 1 d R . . H1B H -0.0123 0.4176 0.1136 0.015 Uiso 1 1 d R . . N2 N 0.0415(3) 0.2850(3) 0.3156(2) 0.0140(7) Uani 1 1 d . . . H2A H 0.0042 0.2104 0.3213 0.017 Uiso 1 1 d R . . H2B H 0.0950 0.3051 0.3734 0.017 Uiso 1 1 d R . . N3 N 0.0378(3) -0.0924(3) 0.2489(2) 0.0157(7) Uani 1 1 d . . . H3A H 0.0921 -0.1387 0.2948 0.019 Uiso 1 1 d R . . H3B H 0.0009 -0.0339 0.2782 0.019 Uiso 1 1 d R . . N4 N 0.0465(3) -0.1377(3) 0.0675(2) 0.0150(7) Uani 1 1 d . . . H4A H -0.0180 -0.1018 0.0220 0.018 Uiso 1 1 d R . . H4B H 0.1030 -0.1707 0.0384 0.018 Uiso 1 1 d R . . N5 N 0.2238(3) 0.0698(3) 0.0777(2) 0.0133(6) Uani 1 1 d . . . H5 H 0.2351 0.0207 0.0329 0.016 Uiso 1 1 d R . . C1 C -0.0014(4) 0.4869(3) 0.2414(3) 0.0144(8) Uani 1 1 d . . . H1C H -0.0671 0.5484 0.2129 0.017 Uiso 1 1 calc R . . H1D H 0.0656 0.5290 0.2901 0.017 Uiso 1 1 calc R . . C2 C -0.0568(4) 0.3830(4) 0.2853(3) 0.0163(8) Uani 1 1 d . . . H2C H -0.0830 0.4136 0.3406 0.020 Uiso 1 1 calc R . . H2D H -0.1315 0.3488 0.2388 0.020 Uiso 1 1 calc R . . C3 C -0.0605(4) -0.1737(4) 0.1877(3) 0.0169(8) Uani 1 1 d . . . H3C H -0.1339 -0.1237 0.1538 0.020 Uiso 1 1 calc R . . H3D H -0.0891 -0.2358 0.2269 0.020 Uiso 1 1 calc R . . C4 C -0.0040(4) -0.2370(4) 0.1184(3) 0.0157(8) Uani 1 1 d . . . H4C H -0.0686 -0.2863 0.0729 0.019 Uiso 1 1 calc R . . H4D H 0.0645 -0.2931 0.1517 0.019 Uiso 1 1 calc R . . C5 C 0.2688(4) 0.1817(4) 0.0767(3) 0.0135(8) Uani 1 1 d . . . C6 C 0.3624(4) 0.2076(4) 0.0219(3) 0.0193(9) Uani 1 1 d . . . H6A H 0.3333 0.2776 -0.0208 0.029 Uiso 1 1 calc R . . H6B H 0.3712 0.1344 -0.0151 0.029 Uiso 1 1 calc R . . H6C H 0.4439 0.2278 0.0658 0.029 Uiso 1 1 calc R . . O3 O 0.2662(3) 0.0102(4) 0.5747(2) 0.0455(11) Uani 1 1 d . . . O4 O 0.3563(3) 0.0949(3) 0.4779(2) 0.0261(7) Uani 1 1 d . . . O5 O 0.1576(3) 0.0501(3) 0.4318(2) 0.0230(7) Uani 1 1 d . . . N6 N 0.2592(3) 0.0527(3) 0.4949(2) 0.0184(7) Uani 1 1 d . . . O6 O -0.1552(3) 0.1439(4) 0.1017(2) 0.0383(9) Uani 1 1 d . . . O7 O -0.3457(3) 0.1246(3) 0.0102(2) 0.0353(8) Uani 1 1 d . . . O8 O -0.3146(3) 0.1511(3) 0.1601(2) 0.0274(7) Uani 1 1 d . . . N7 N -0.2710(3) 0.1414(3) 0.0904(2) 0.0196(8) Uani 1 1 d . . . O9 O 0.6186(3) 0.5775(3) 0.1839(2) 0.0184(6) Uani 1 1 d . . . H1O H 0.6451 0.5480 0.1401 0.028 Uiso 1 1 d R . . H2O H 0.6771 0.5950 0.2316 0.028 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 0.01125(15) 0.00980(15) 0.01068(16) 0.00022(10) 0.00276(12) 0.00021(10) Pd2 0.01200(15) 0.01035(15) 0.01073(16) 0.00086(10) 0.00310(12) 0.00082(11) O2 0.0127(13) 0.0145(13) 0.0087(13) 0.0013(10) -0.0041(11) 0.0043(11) O1 0.0192(14) 0.0126(13) 0.0162(14) -0.0007(11) 0.0093(12) -0.0009(11) N1 0.0134(15) 0.0122(15) 0.0134(16) 0.0020(12) 0.0044(13) 0.0011(13) N2 0.0169(16) 0.0117(15) 0.0145(17) 0.0022(12) 0.0061(14) 0.0011(13) N3 0.0189(17) 0.0127(16) 0.0159(17) 0.0027(13) 0.0055(14) 0.0033(13) N4 0.0161(16) 0.0148(16) 0.0137(17) 0.0020(13) 0.0033(14) -0.0002(13) N5 0.0137(15) 0.0161(16) 0.0097(16) -0.0019(13) 0.0027(13) -0.0019(13) C1 0.0160(19) 0.0134(18) 0.013(2) -0.0007(15) 0.0029(16) -0.0001(15) C2 0.0172(19) 0.0151(19) 0.017(2) 0.0010(15) 0.0050(17) 0.0043(16) C3 0.0165(19) 0.0126(18) 0.023(2) 0.0025(16) 0.0080(17) 0.0013(15) C4 0.0163(19) 0.0120(18) 0.018(2) 0.0018(15) 0.0040(17) -0.0025(15) C5 0.0115(18) 0.0184(19) 0.0085(18) 0.0030(15) -0.0009(15) 0.0000(15) C6 0.018(2) 0.022(2) 0.020(2) -0.0024(17) 0.0087(18) -0.0025(17) O3 0.0250(18) 0.094(3) 0.0131(17) 0.0163(18) -0.0025(15) -0.0213(19) O4 0.0234(16) 0.0384(18) 0.0180(16) 0.0028(13) 0.0081(13) -0.0130(14) O5 0.0183(15) 0.0317(17) 0.0161(15) 0.0039(13) -0.0004(13) 0.0007(13) N6 0.0202(18) 0.0221(18) 0.0128(18) 0.0017(14) 0.0042(15) -0.0023(15) O6 0.0287(19) 0.063(3) 0.0279(19) -0.0049(17) 0.0156(16) -0.0071(17) O7 0.037(2) 0.047(2) 0.0183(18) -0.0036(15) 0.0006(16) 0.0162(17) O8 0.0259(17) 0.0406(19) 0.0179(16) 0.0013(14) 0.0100(14) 0.0017(14) N7 0.0262(19) 0.0159(17) 0.0165(19) -0.0011(14) 0.0053(16) 0.0029(15) O9 0.0181(14) 0.0212(15) 0.0162(15) -0.0035(12) 0.0051(12) 0.0009(12) _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 O2 2.010(3) . ? Pd1 N2 2.020(3) . ? Pd1 N1 2.029(3) . ? Pd1 O1 2.029(3) . ? Pd1 Pd2 3.1243(7) . ? Pd2 O2 2.013(3) . ? Pd2 N5 2.018(3) . ? Pd2 N3 2.035(3) . ? Pd2 N4 2.042(3) . ? O2 H1 0.9501 . ? O1 C5 1.286(5) . ? N1 C1 1.484(5) . ? N1 H1A 0.9193 . ? N1 H1B 0.9197 . ? N2 C2 1.495(5) . ? N2 H2A 0.9200 . ? N2 H2B 0.9197 . ? N3 C3 1.494(5) . ? N3 H3A 0.9199 . ? N3 H3B 0.9201 . ? N4 C4 1.500(5) . ? N4 H4A 0.9207 . ? N4 H4B 0.9189 . ? N5 C5 1.309(5) . ? N5 H5 0.8803 . ? C1 C2 1.506(5) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C3 C4 1.497(6) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 H4C 0.9900 . ? C4 H4D 0.9900 . ? C5 C6 1.499(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O3 N6 1.243(5) . ? O4 N6 1.251(4) . ? O5 N6 1.248(5) . ? O6 N7 1.245(5) . ? O7 N7 1.255(5) . ? O8 N7 1.248(4) . ? O9 H1O 0.8385 . ? O9 H2O 0.8364 . ? 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 O2 Pd1 N2 94.37(12) . . ? O2 Pd1 N1 178.15(12) . . ? N2 Pd1 N1 84.42(13) . . ? O2 Pd1 O1 89.31(11) . . ? N2 Pd1 O1 174.83(12) . . ? N1 Pd1 O1 91.98(12) . . ? O2 Pd1 Pd2 39.08(8) . . ? N2 Pd1 Pd2 105.45(9) . . ? N1 Pd1 Pd2 139.95(10) . . ? O1 Pd1 Pd2 79.68(7) . . ? O2 Pd2 N5 89.21(12) . . ? O2 Pd2 N3 93.03(12) . . ? N5 Pd2 N3 177.76(13) . . ? O2 Pd2 N4 176.34(12) . . ? N5 Pd2 N4 93.47(13) . . ? N3 Pd2 N4 84.29(13) . . ? O2 Pd2 Pd1 39.02(7) . . ? N5 Pd2 Pd1 76.65(9) . . ? N3 Pd2 Pd1 105.13(9) . . ? N4 Pd2 Pd1 144.22(9) . . ? Pd1 O2 Pd2 101.90(11) . . ? Pd1 O2 H1 129.1 . . ? Pd2 O2 H1 129.1 . . ? C5 O1 Pd1 127.0(2) . . ? C1 N1 Pd1 108.6(2) . . ? C1 N1 H1A 110.0 . . ? Pd1 N1 H1A 110.0 . . ? C1 N1 H1B 109.9 . . ? Pd1 N1 H1B 110.0 . . ? H1A N1 H1B 108.4 . . ? C2 N2 Pd1 108.8(2) . . ? C2 N2 H2A 109.9 . . ? Pd1 N2 H2A 109.9 . . ? C2 N2 H2B 109.9 . . ? Pd1 N2 H2B 109.9 . . ? H2A N2 H2B 108.4 . . ? C3 N3 Pd2 108.0(2) . . ? C3 N3 H3A 110.1 . . ? Pd2 N3 H3A 110.1 . . ? C3 N3 H3B 110.1 . . ? Pd2 N3 H3B 110.1 . . ? H3A N3 H3B 108.4 . . ? C4 N4 Pd2 107.8(2) . . ? C4 N4 H4A 110.1 . . ? Pd2 N4 H4A 110.1 . . ? C4 N4 H4B 110.2 . . ? Pd2 N4 H4B 110.1 . . ? H4A N4 H4B 108.4 . . ? C5 N5 Pd2 130.7(3) . . ? C5 N5 H5 114.7 . . ? Pd2 N5 H5 114.7 . . ? N1 C1 C2 107.5(3) . . ? N1 C1 H1C 110.2 . . ? C2 C1 H1C 110.2 . . ? N1 C1 H1D 110.2 . . ? C2 C1 H1D 110.2 . . ? H1C C1 H1D 108.5 . . ? N2 C2 C1 108.0(3) . . ? N2 C2 H2C 110.1 . . ? C1 C2 H2C 110.1 . . ? N2 C2 H2D 110.1 . . ? C1 C2 H2D 110.1 . . ? H2C C2 H2D 108.4 . . ? N3 C3 C4 108.0(3) . . ? N3 C3 H3C 110.1 . . ? C4 C3 H3C 110.1 . . ? N3 C3 H3D 110.1 . . ? C4 C3 H3D 110.1 . . ? H3C C3 H3D 108.4 . . ? C3 C4 N4 107.0(3) . . ? C3 C4 H4C 110.3 . . ? N4 C4 H4C 110.3 . . ? C3 C4 H4D 110.3 . . ? N4 C4 H4D 110.3 . . ? H4C C4 H4D 108.6 . . ? O1 C5 N5 124.8(4) . . ? O1 C5 C6 115.3(3) . . ? N5 C5 C6 119.9(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 N6 O5 120.3(3) . . ? O3 N6 O4 119.0(4) . . ? O5 N6 O4 120.6(3) . . ? O6 N7 O8 120.0(4) . . ? O6 N7 O7 121.3(4) . . ? O8 N7 O7 118.6(4) . . ? H1O O9 H2O 112.2 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.34 _refine_diff_density_min -1.24 _refine_diff_density_rms 0.166 # Attachment 'JW-Complex 6.CIF' data_6 _database_code_depnum_ccdc_archive 'CCDC 648491' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H24 N6 O2 Pd2, 2(C F3 O3 S), (H2 O)' _chemical_formula_sum 'C10 H26 F6 N6 O9 Pd2 S2' _chemical_formula_weight 765.29 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.265(3) _cell_length_b 13.134(2) _cell_length_c 20.892(3) _cell_angle_alpha 90.00 _cell_angle_beta 119.338(5) _cell_angle_gamma 90.00 _cell_volume 5086.6(13) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7851 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 28.34 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.999 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024 _exptl_absorpt_coefficient_mu 1.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5401 _exptl_absorpt_correction_T_max 0.9063 _exptl_absorpt_process_details 'SADABS (Sheldrick, 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 'CCD Bruker APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39284 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9988 _reflns_number_gt 9241 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 2000)' _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^)+(0.036P)^2^+11.6P] 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 9988 _refine_ls_number_parameters 836 _refine_ls_number_restraints 844 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.039 _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 -0.024611(11) 0.340512(16) 0.212493(12) 0.01422(6) Uani 1 1 d . . . Pd2 Pd 0.031047(11) 0.121340(16) 0.234377(12) 0.01421(6) Uani 1 1 d . . . Pd3 Pd 0.454735(11) 0.484317(16) 0.222448(12) 0.01409(6) Uani 1 1 d . . . Pd4 Pd 0.473947(11) 0.249956(16) 0.215894(11) 0.01362(6) Uani 1 1 d . . . S2 S -0.18987(4) 0.16127(6) -0.04775(4) 0.02154(16) Uani 1 1 d . . . S3 S 0.18260(4) 0.35359(6) 0.13567(5) 0.02653(18) Uani 1 1 d . . . S4 S 0.36081(4) 0.63599(6) 0.35731(4) 0.02015(15) Uani 1 1 d . . . F4 F -0.27066(12) 0.20031(18) 0.01094(13) 0.0421(5) Uani 1 1 d . . . F5 F -0.23833(13) 0.04401(18) 0.01868(13) 0.0459(6) Uani 1 1 d . . . F6 F -0.32146(11) 0.10306(17) -0.08386(12) 0.0366(5) Uani 1 1 d . . . F7 F 0.14720(12) 0.19581(16) 0.04690(12) 0.0386(5) Uani 1 1 d . . . F8 F 0.06926(13) 0.3174(2) 0.00885(14) 0.0590(7) Uani 1 1 d . . . F9 F 0.16841(14) 0.33460(18) 0.00513(13) 0.0467(6) Uani 1 1 d . . . F10 F 0.24210(11) 0.5429(2) 0.33182(14) 0.0503(6) Uani 1 1 d . . . F11 F 0.33761(12) 0.48636(19) 0.42560(13) 0.0459(6) Uani 1 1 d . . . F12 F 0.31721(14) 0.44923(17) 0.31646(14) 0.0463(6) Uani 1 1 d . . . O1 O 0.07279(11) 0.35553(16) 0.30381(12) 0.0199(4) Uani 1 1 d . . . O2 O -0.02759(12) 0.11306(15) 0.28713(12) 0.0202(4) Uani 1 1 d . . . O3 O 0.56075(11) 0.47949(15) 0.25175(12) 0.0189(4) Uani 1 1 d . . . O4 O 0.49996(11) 0.26131(15) 0.32262(11) 0.0189(4) Uani 1 1 d . . . O5 O -0.17929(13) 0.0711(2) -0.08016(14) 0.0345(6) Uani 1 1 d . . . O6 O -0.22049(14) 0.2474(2) -0.09553(14) 0.0371(6) Uani 1 1 d . . . O7 O -0.12925(12) 0.18498(18) 0.02403(12) 0.0258(5) Uani 1 1 d . . . O8 O 0.17087(16) 0.46057(19) 0.12122(18) 0.0433(7) Uani 1 1 d . . . O9 O 0.25691(12) 0.32022(18) 0.16756(14) 0.0306(5) Uani 1 1 d . . . O10 O 0.14367(13) 0.30761(18) 0.16879(14) 0.0296(5) Uani 1 1 d . . . O11 O 0.43515(12) 0.60195(17) 0.39188(12) 0.0230(5) Uani 1 1 d . . . O12 O 0.32962(12) 0.65868(17) 0.28007(12) 0.0240(5) Uani 1 1 d . . . O13 O 0.34585(13) 0.7091(2) 0.39924(13) 0.0329(6) Uani 1 1 d . . . O17 O 0.16143(12) -0.07679(18) 0.20690(14) 0.0223(5) Uani 1 1 d . . . H17B H 0.190(2) -0.093(3) 0.250(2) 0.027 Uiso 1 1 d . . . H17A H 0.172(2) -0.082(3) 0.181(2) 0.027 Uiso 1 1 d . . . O18 O -0.24060(14) 0.3585(2) 0.15100(15) 0.0293(6) Uani 1 1 d . . . H18B H -0.265(2) 0.398(3) 0.136(2) 0.035 Uiso 1 1 d . . . H18A H -0.257(2) 0.312(4) 0.147(2) 0.035 Uiso 1 1 d . . . N1 N 0.01338(14) 0.4147(2) 0.15244(14) 0.0177(5) Uani 1 1 d . . . H1B H 0.0227(19) 0.473(3) 0.170(2) 0.021 Uiso 1 1 d . . . H1A H 0.048(2) 0.390(3) 0.156(2) 0.021 Uiso 1 1 d . . . N2 N -0.12034(14) 0.3501(2) 0.11919(15) 0.0197(5) Uani 1 1 d . . . H2B H -0.1251(19) 0.294(3) 0.096(2) 0.024 Uiso 1 1 d . . . H2A H -0.157(2) 0.366(3) 0.127(2) 0.024 Uiso 1 1 d . . . N4 N 0.08718(13) 0.11106(19) 0.17992(14) 0.0187(5) Uani 1 1 d . . . H4B H 0.1092 0.1723 0.1822 0.022 Uiso 1 1 calc R . . H4A H 0.1224 0.0620 0.2013 0.022 Uiso 1 1 calc R . . N3 N -0.04683(14) 0.0454(2) 0.14540(15) 0.0187(5) Uani 1 1 d . . . H3B H -0.062(2) 0.001(3) 0.158(2) 0.022 Uiso 1 1 d . . . H3A H -0.079(2) 0.086(3) 0.120(2) 0.022 Uiso 1 1 d . . . N5 N 0.11319(15) 0.1918(2) 0.31964(15) 0.0208(5) Uani 1 1 d . . . H5A H 0.147(2) 0.165(3) 0.343(2) 0.025 Uiso 1 1 d . . . N6 N -0.06857(14) 0.2768(2) 0.26872(14) 0.0187(5) Uani 1 1 d . . . H6A H -0.092(2) 0.310(3) 0.276(2) 0.022 Uiso 1 1 d . . . N7 N 0.43388(15) 0.5557(2) 0.12710(15) 0.0206(5) Uani 1 1 d . . . H7B H 0.463(2) 0.606(3) 0.136(2) 0.025 Uiso 1 1 d . . . H7A H 0.435(2) 0.520(3) 0.100(2) 0.025 Uiso 1 1 d . . . N8 N 0.34836(14) 0.5048(2) 0.18549(15) 0.0197(5) Uani 1 1 d . . . H8Bn H 0.328(2) 0.453(3) 0.189(2) 0.024 Uiso 1 1 d . . . H8An H 0.342(2) 0.550(3) 0.209(2) 0.024 Uiso 1 1 d . . . N10 N 0.44646(15) 0.2168(2) 0.11088(14) 0.0194(5) Uani 1 1 d . . . H10B H 0.433(2) 0.266(3) 0.084(2) 0.023 Uiso 1 1 d . . . H10A H 0.481(2) 0.193(3) 0.108(2) 0.023 Uiso 1 1 d . . . N9 N 0.37789(13) 0.1809(2) 0.18955(14) 0.0180(5) Uani 1 1 d . . . H9B H 0.391(2) 0.127(3) 0.210(2) 0.022 Uiso 1 1 d . . . H9A H 0.350(2) 0.209(3) 0.2052(19) 0.022 Uiso 1 1 d . . . N11 N 0.56897(13) 0.3079(2) 0.23606(14) 0.0174(5) Uani 1 1 d . . . H11A H 0.595(2) 0.271(3) 0.236(2) 0.021 Uiso 1 1 d . . . N12 N 0.47179(14) 0.4294(2) 0.31943(14) 0.0187(5) Uani 1 1 d . . . H12A H 0.468(2) 0.470(3) 0.339(2) 0.022 Uiso 1 1 d . . . C1 C -0.04370(17) 0.4187(2) 0.07441(17) 0.0234(6) Uani 1 1 d . . . H1D H -0.0441 0.3547 0.0491 0.028 Uiso 1 1 calc R . . H1C H -0.0349 0.4762 0.0492 0.028 Uiso 1 1 calc R . . C2 C -0.11497(17) 0.4328(3) 0.07296(18) 0.0256(7) Uani 1 1 d . . . H2D H -0.1168 0.5004 0.0930 0.031 Uiso 1 1 calc R . . H2C H -0.1554 0.4280 0.0220 0.031 Uiso 1 1 calc R . . C4 C 0.03699(17) 0.0840(3) 0.10189(17) 0.0238(7) Uani 1 1 d . . . H4D H 0.0644 0.0560 0.0788 0.029 Uiso 1 1 calc R . . H4C H 0.0105 0.1452 0.0741 0.029 Uiso 1 1 calc R . . C3 C -0.01539(17) 0.0053(2) 0.10092(17) 0.0236(6) Uani 1 1 d . . . H3D H -0.0540 -0.0073 0.0499 0.028 Uiso 1 1 calc R . . H3C H 0.0100 -0.0597 0.1219 0.028 Uiso 1 1 calc R . . C5 C 0.12059(16) 0.2870(2) 0.33847(16) 0.0186(6) Uani 1 1 d . . . C6 C 0.18756(18) 0.3261(3) 0.40439(18) 0.0293(7) Uani 1 1 d . . . H6D H 0.2113 0.3763 0.3886 0.044 Uiso 1 1 d R . . H6C H 0.2206 0.2692 0.4289 0.044 Uiso 1 1 d R . . H6B H 0.1744 0.3582 0.4385 0.044 Uiso 1 1 d R . . C7 C -0.06380(15) 0.1864(2) 0.29490(16) 0.0181(6) Uani 1 1 d . . . C8 C -0.10165(18) 0.1594(2) 0.33766(19) 0.0248(7) Uani 1 1 d . . . H8A H -0.1344 0.1020 0.3139 0.037 Uiso 1 1 d R . . H8B H -0.1293 0.2183 0.3390 0.037 Uiso 1 1 d R . . H8C H -0.0658 0.1404 0.3879 0.037 Uiso 1 1 d R . . C9 C 0.35941(19) 0.6004(3) 0.0927(2) 0.0383(9) Uani 1 1 d . . . H9D H 0.3611 0.6680 0.1144 0.046 Uiso 1 1 calc R . . H9C H 0.3403 0.6092 0.0393 0.046 Uiso 1 1 calc R . . C10 C 0.31206(19) 0.5316(3) 0.1058(2) 0.0396(9) Uani 1 1 d . . . H10D H 0.3025 0.4691 0.0759 0.048 Uiso 1 1 calc R . . H10C H 0.2654 0.5655 0.0913 0.048 Uiso 1 1 calc R . . C12 C 0.38775(17) 0.1392(2) 0.08243(17) 0.0230(6) Uani 1 1 d . . . H12C H 0.4081 0.0708 0.1010 0.028 Uiso 1 1 calc R . . H12B H 0.3628 0.1376 0.0281 0.028 Uiso 1 1 calc R . . C11 C 0.33554(16) 0.1682(2) 0.10850(17) 0.0220(6) Uani 1 1 d . . . H11C H 0.3107 0.2325 0.0850 0.026 Uiso 1 1 calc R . . H11B H 0.2988 0.1142 0.0957 0.026 Uiso 1 1 calc R . . C13 C 0.59425(15) 0.3997(2) 0.24791(15) 0.0168(6) Uani 1 1 d . . . C14 C 0.66758(16) 0.4199(2) 0.25639(18) 0.0214(6) Uani 1 1 d . . . H14C H 0.6947 0.3560 0.2675 0.032 Uiso 1 1 d R . . H14B H 0.6936 0.4684 0.2965 0.032 Uiso 1 1 d R . . H14A H 0.6622 0.4485 0.2106 0.032 Uiso 1 1 d R . . C15 C 0.49254(15) 0.3427(2) 0.35234(16) 0.0174(6) Uani 1 1 d . . . C16 C 0.51096(19) 0.3317(3) 0.43179(17) 0.0273(7) Uani 1 1 d . . . H16C H 0.4839 0.2746 0.4365 0.041 Uiso 1 1 d R . . H16B H 0.4981 0.3945 0.4480 0.041 Uiso 1 1 d R . . H16A H 0.5628 0.3191 0.4623 0.041 Uiso 1 1 d R . . C17 C -0.25907(17) 0.1255(2) -0.02456(18) 0.0241(7) Uani 1 1 d . . . C18 C 0.1394(2) 0.2975(3) 0.0444(2) 0.0342(8) Uani 1 1 d . . . C19 C 0.31156(19) 0.5223(3) 0.3577(2) 0.0338(8) Uani 1 1 d . . . S1F S 0.31715(14) 0.3961(2) -0.08154(15) 0.0302(7) Uani 0.444(3) 1 d PDU A 1 O1F O 0.2464(2) 0.4267(5) -0.0964(3) 0.0305(16) Uani 0.444(3) 1 d PDU A 1 O2F O 0.3610(3) 0.4799(4) -0.0798(3) 0.0435(18) Uani 0.444(3) 1 d PDU A 1 O3F O 0.3496(3) 0.3215(4) -0.0247(3) 0.0521(16) Uani 0.444(3) 1 d PDU A 1 C1F C 0.2996(2) 0.3280(3) -0.1651(4) 0.0258(14) Uani 0.444(3) 1 d PDU A 1 F1F F 0.3607(3) 0.3072(5) -0.1650(3) 0.0549(15) Uani 0.444(3) 1 d PDU A 1 F2F F 0.2651(3) 0.2414(2) -0.1711(2) 0.0358(11) Uani 0.444(3) 1 d PDU A 1 F3F F 0.2594(3) 0.3843(4) -0.2240(2) 0.0303(13) Uani 0.444(3) 1 d PDU A 1 S1F'' S 0.33553(15) 0.4242(2) -0.05974(15) 0.0184(6) Uani 0.386(3) 1 d PDU B 2 O1F'' O 0.2643(2) 0.4167(5) -0.0690(3) 0.0241(16) Uani 0.386(3) 1 d PDU B 2 O2F'' O 0.3532(3) 0.5218(3) -0.0772(3) 0.0180(13) Uani 0.386(3) 1 d PDU B 2 O3F'' O 0.3902(3) 0.3804(4) 0.0075(3) 0.0415(16) Uani 0.386(3) 1 d PDU B 2 C1F'' C 0.3328(2) 0.3414(4) -0.1310(4) 0.0307(14) Uani 0.386(3) 1 d PDU B 2 F1F'' F 0.3912(3) 0.3539(4) -0.1379(3) 0.0414(14) Uani 0.386(3) 1 d PDU B 2 F2F'' F 0.3296(3) 0.2443(3) -0.1151(3) 0.0477(14) Uani 0.386(3) 1 d PDU B 2 F3F'' F 0.2759(3) 0.3623(5) -0.1958(3) 0.0398(17) Uani 0.386(3) 1 d PDU B 2 S1F''' S 0.3502(5) 0.3761(7) -0.0541(5) 0.0207(15) Uiso 0.0826(19) 1 d PDU C 3 O1F''' O 0.2888(6) 0.4292(14) -0.1095(9) 0.028(3) Uiso 0.0826(19) 1 d PDU C 3 O2F''' O 0.3608(10) 0.2763(8) -0.0748(12) 0.037(3) Uiso 0.0826(19) 1 d PDU C 3 O3F''' O 0.3577(10) 0.3814(16) 0.0178(7) 0.032(3) Uiso 0.0826(19) 1 d PDU C 3 C1F''' C 0.4272(6) 0.4486(9) -0.0452(7) 0.032(3) Uiso 0.0826(19) 1 d PDU C 3 F1F''' F 0.4861(5) 0.4267(14) 0.0178(9) 0.038(5) Uiso 0.0826(19) 1 d PDU C 3 F2F''' F 0.4153(8) 0.5480(8) -0.0462(11) 0.031(3) Uiso 0.0826(19) 1 d PDU C 3 F3F''' F 0.4396(10) 0.4277(15) -0.1003(10) 0.056(5) Uiso 0.0826(19) 1 d PDU C 3 S1F' S 0.5010(3) 0.4226(5) 0.0590(4) 0.010 Uiso 0.0878(15) 1 d PDU D 4 O1F' O 0.5273(8) 0.388(2) 0.0115(9) 0.079(8) Uiso 0.0878(15) 1 d PDU D 4 O2F' O 0.5177(9) 0.357(2) 0.1202(10) 0.098(10) Uiso 0.0878(15) 1 d PDU D 4 O3F' O 0.5127(9) 0.5287(8) 0.0767(15) 0.092(10) Uiso 0.0878(15) 1 d PDU D 4 C1F' C 0.4032(6) 0.4122(10) 0.0025(7) 0.030(2) Uiso 0.0878(15) 1 d PDU D 4 F1F' F 0.3714(6) 0.4200(19) 0.0434(11) 0.067(5) Uiso 0.0878(15) 1 d PDU D 4 F2F' F 0.3772(7) 0.4852(14) -0.0480(9) 0.038(3) Uiso 0.0878(15) 1 d PDU D 4 F3F' F 0.3849(7) 0.3230(12) -0.0317(10) 0.039(3) Uiso 0.0878(15) 1 d PDU D 4 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 0.01526(11) 0.01194(11) 0.01748(11) 0.00045(8) 0.00958(9) -0.00025(8) Pd2 0.01543(11) 0.01147(11) 0.01649(11) -0.00042(8) 0.00842(9) -0.00101(8) Pd3 0.01295(10) 0.01237(11) 0.01644(11) -0.00027(8) 0.00679(9) 0.00080(8) Pd4 0.01371(11) 0.01200(11) 0.01457(11) -0.00067(8) 0.00649(9) 0.00078(7) S2 0.0202(4) 0.0274(4) 0.0171(4) 0.0007(3) 0.0092(3) -0.0013(3) S3 0.0277(4) 0.0177(4) 0.0453(5) -0.0020(3) 0.0265(4) 0.0004(3) S4 0.0222(4) 0.0210(4) 0.0208(4) 0.0017(3) 0.0133(3) 0.0007(3) F4 0.0415(12) 0.0485(14) 0.0459(13) -0.0123(11) 0.0288(11) 0.0029(10) F5 0.0520(14) 0.0415(13) 0.0495(14) 0.0235(11) 0.0289(12) 0.0016(11) F6 0.0245(10) 0.0482(13) 0.0361(12) -0.0055(10) 0.0140(9) -0.0092(9) F7 0.0471(13) 0.0283(11) 0.0462(13) -0.0082(10) 0.0273(11) -0.0080(9) F8 0.0333(13) 0.080(2) 0.0485(15) 0.0031(14) 0.0085(11) 0.0133(13) F9 0.0651(16) 0.0435(13) 0.0456(14) 0.0078(11) 0.0381(13) 0.0041(12) F10 0.0256(11) 0.0708(17) 0.0547(15) 0.0242(13) 0.0197(11) -0.0038(11) F11 0.0428(13) 0.0581(15) 0.0408(13) 0.0279(11) 0.0236(11) -0.0001(11) F12 0.0603(15) 0.0273(11) 0.0542(14) -0.0016(10) 0.0304(12) -0.0166(11) O1 0.0196(10) 0.0165(10) 0.0216(11) -0.0028(8) 0.0087(9) -0.0015(8) O2 0.0283(11) 0.0131(10) 0.0272(11) 0.0001(8) 0.0197(10) -0.0008(8) O3 0.0160(10) 0.0149(10) 0.0264(11) -0.0013(8) 0.0108(9) 0.0000(8) O4 0.0229(11) 0.0172(10) 0.0160(10) 0.0008(8) 0.0090(9) 0.0022(8) O5 0.0303(13) 0.0426(15) 0.0314(13) -0.0113(11) 0.0158(11) 0.0023(11) O6 0.0363(14) 0.0377(15) 0.0324(14) 0.0155(11) 0.0130(12) -0.0018(11) O7 0.0225(11) 0.0296(12) 0.0202(11) -0.0008(9) 0.0064(9) -0.0004(9) O8 0.0559(17) 0.0192(12) 0.080(2) 0.0022(13) 0.0523(17) 0.0054(12) O9 0.0248(12) 0.0271(12) 0.0448(15) -0.0065(11) 0.0210(11) -0.0013(10) O10 0.0307(12) 0.0228(12) 0.0446(14) 0.0019(10) 0.0258(11) 0.0007(10) O11 0.0234(11) 0.0208(11) 0.0281(12) -0.0009(9) 0.0151(10) 0.0008(9) O12 0.0301(12) 0.0213(11) 0.0236(11) 0.0020(9) 0.0154(10) -0.0045(9) O13 0.0344(13) 0.0391(14) 0.0258(12) 0.0009(11) 0.0151(11) 0.0158(11) O17 0.0209(11) 0.0251(12) 0.0263(13) 0.0009(10) 0.0158(10) 0.0019(9) O18 0.0247(13) 0.0282(14) 0.0371(15) -0.0053(12) 0.0168(12) -0.0046(10) N1 0.0203(13) 0.0137(12) 0.0239(14) -0.0005(10) 0.0144(11) -0.0003(10) N2 0.0186(12) 0.0208(13) 0.0204(13) 0.0006(11) 0.0101(11) 0.0007(10) N4 0.0187(12) 0.0179(12) 0.0217(13) 0.0000(10) 0.0117(11) 0.0003(10) N3 0.0209(13) 0.0155(13) 0.0192(13) 0.0025(10) 0.0094(11) -0.0010(10) N5 0.0195(13) 0.0167(13) 0.0197(13) 0.0021(10) 0.0046(11) 0.0000(10) N6 0.0204(13) 0.0153(12) 0.0250(14) 0.0002(10) 0.0146(11) 0.0016(10) N7 0.0244(13) 0.0161(13) 0.0219(14) -0.0008(10) 0.0119(11) -0.0015(11) N8 0.0166(12) 0.0192(13) 0.0218(13) 0.0000(11) 0.0084(11) 0.0014(10) N10 0.0213(13) 0.0183(13) 0.0174(13) 0.0002(10) 0.0086(11) 0.0036(11) N9 0.0161(12) 0.0151(12) 0.0218(13) -0.0005(10) 0.0084(11) 0.0019(10) N11 0.0159(12) 0.0167(13) 0.0214(13) -0.0009(10) 0.0105(10) 0.0025(10) N12 0.0196(12) 0.0186(13) 0.0195(13) -0.0035(10) 0.0108(11) 0.0015(10) C1 0.0288(16) 0.0230(16) 0.0222(16) 0.0034(13) 0.0153(14) -0.0006(13) C2 0.0246(16) 0.0263(17) 0.0230(16) 0.0068(13) 0.0094(13) 0.0038(13) C4 0.0282(16) 0.0251(16) 0.0217(16) 0.0006(13) 0.0151(14) 0.0024(13) C3 0.0273(16) 0.0224(16) 0.0202(15) -0.0040(12) 0.0111(13) -0.0016(13) C5 0.0215(14) 0.0185(15) 0.0162(14) 0.0002(11) 0.0094(12) -0.0033(12) C6 0.0291(17) 0.0234(17) 0.0239(17) -0.0008(13) 0.0041(14) -0.0055(13) C7 0.0180(14) 0.0185(15) 0.0187(14) -0.0008(12) 0.0096(12) -0.0023(11) C8 0.0296(17) 0.0225(16) 0.0313(18) 0.0037(13) 0.0220(15) 0.0007(13) C9 0.0268(18) 0.048(2) 0.0311(19) 0.0132(17) 0.0070(15) 0.0013(16) C10 0.0249(17) 0.052(2) 0.032(2) 0.0132(18) 0.0066(15) 0.0024(16) C12 0.0231(15) 0.0195(15) 0.0196(15) -0.0043(12) 0.0051(13) 0.0021(12) C11 0.0169(14) 0.0205(15) 0.0212(15) -0.0020(12) 0.0037(12) 0.0014(12) C13 0.0164(13) 0.0195(14) 0.0139(13) 0.0009(11) 0.0070(11) 0.0016(11) C14 0.0179(14) 0.0217(15) 0.0269(16) 0.0013(13) 0.0127(13) 0.0006(12) C15 0.0126(13) 0.0218(15) 0.0172(14) -0.0020(12) 0.0068(11) -0.0003(11) C16 0.0345(18) 0.0286(17) 0.0194(16) -0.0006(13) 0.0137(14) 0.0028(14) C17 0.0260(16) 0.0255(16) 0.0241(16) -0.0001(13) 0.0149(14) -0.0005(13) C18 0.0336(19) 0.0327(19) 0.041(2) 0.0046(16) 0.0220(17) 0.0048(15) C19 0.0283(18) 0.041(2) 0.035(2) 0.0148(17) 0.0178(16) -0.0051(15) S1F 0.0296(12) 0.0240(13) 0.0220(13) 0.0096(10) 0.0010(10) -0.0092(10) O1F 0.034(3) 0.027(3) 0.022(3) -0.009(3) 0.008(3) -0.008(2) O2F 0.034(3) 0.047(3) 0.023(3) 0.007(3) -0.006(2) -0.010(3) O3F 0.049(3) 0.048(3) 0.038(3) 0.017(3) 0.005(2) -0.001(3) C1F 0.025(3) 0.023(3) 0.034(3) 0.014(3) 0.019(3) 0.010(2) F1F 0.030(3) 0.082(4) 0.060(3) 0.007(3) 0.027(2) 0.016(3) F2F 0.065(3) 0.0124(19) 0.050(3) 0.0019(18) 0.044(3) 0.0021(19) F3F 0.033(3) 0.023(2) 0.024(3) 0.014(2) 0.006(2) -0.0003(19) S1F' 0.0248(13) 0.0141(13) 0.0159(12) -0.0003(9) 0.0098(10) -0.0055(10) O1F' 0.030(3) 0.028(3) 0.018(4) -0.007(3) 0.015(3) -0.011(3) O2F' 0.015(2) 0.011(3) 0.025(3) 0.010(2) 0.008(2) 0.007(2) O3F' 0.051(3) 0.029(3) 0.033(3) 0.016(2) 0.012(3) -0.002(3) C1F' 0.037(3) 0.026(2) 0.032(3) 0.000(2) 0.019(2) 0.000(2) F1F' 0.050(3) 0.037(3) 0.057(4) 0.001(3) 0.041(3) 0.007(3) F2F' 0.074(3) 0.021(2) 0.068(3) -0.006(2) 0.050(3) -0.006(2) F3F' 0.049(4) 0.042(4) 0.028(4) -0.012(3) 0.019(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N6 2.007(3) . ? Pd1 N2 2.018(3) . ? Pd1 O1 2.024(2) . ? Pd1 N1 2.042(3) . ? Pd1 Pd2 3.0604(5) . ? Pd2 N5 2.008(3) . ? Pd2 N4 2.017(2) . ? Pd2 O2 2.032(2) . ? Pd2 N3 2.044(3) . ? Pd3 N12 2.009(3) . ? Pd3 N8 2.018(3) . ? Pd3 O3 2.027(2) . ? Pd3 N7 2.044(3) . ? Pd3 Pd4 3.1169(5) . ? Pd4 N11 2.002(3) . ? Pd4 N10 2.022(3) . ? Pd4 O4 2.023(2) . ? Pd4 N9 2.048(3) . ? S2 O5 1.436(3) . ? S2 O6 1.436(3) . ? S2 O7 1.454(2) . ? S2 C17 1.822(3) . ? S3 O8 1.433(3) . ? S3 O10 1.446(2) . ? S3 O9 1.450(2) . ? S3 C18 1.819(4) . ? S4 O13 1.437(2) . ? S4 O12 1.444(2) . ? S4 O11 1.450(2) . ? S4 C19 1.826(4) . ? F4 C17 1.325(4) . ? F5 C17 1.329(4) . ? F6 C17 1.331(4) . ? F7 C18 1.343(4) . ? F8 C18 1.326(4) . ? F9 C18 1.337(4) . ? F10 C19 1.328(4) . ? F11 C19 1.331(4) . ? F12 C19 1.334(5) . ? O1 C5 1.283(4) . ? O2 C7 1.292(4) . ? O3 C13 1.291(4) . ? O4 C15 1.284(4) . ? O17 H17B 0.84(4) . ? O17 H17A 0.68(4) . ? O18 H18B 0.70(4) . ? O18 H18A 0.69(5) . ? N1 C1 1.481(4) . ? N1 H1B 0.82(4) . ? N1 H1A 0.78(4) . ? N2 C2 1.494(4) . ? N2 H2B 0.86(4) . ? N2 H2A 0.89(4) . ? N4 C4 1.490(4) . ? N4 H4B 0.9200 . ? N4 H4A 0.9200 . ? N3 C3 1.482(4) . ? N3 H3B 0.78(4) . ? N3 H3A 0.82(4) . ? N5 C5 1.298(4) . ? N5 H5A 0.73(4) . ? N6 C7 1.290(4) . ? N6 H6A 0.74(4) . ? N7 C9 1.501(4) . ? N7 H7B 0.86(4) . ? N7 H7A 0.75(4) . ? N8 C10 1.494(4) . ? N8 H8B 0.84(4) . ? N8 H8A 0.82(4) . ? N10 C12 1.491(4) . ? N10 H10B 0.81(4) . ? N10 H10A 0.84(4) . ? N9 C11 1.487(4) . ? N9 H9B 0.80(4) . ? N9 H9A 0.88(4) . ? N11 C13 1.293(4) . ? N11 H11A 0.73(4) . ? N12 C15 1.292(4) . ? N12 H12A 0.70(4) . ? C1 C2 1.513(4) . ? C1 H1D 0.9900 . ? C1 H1C 0.9900 . ? C2 H2D 0.9900 . ? C2 H2C 0.9900 . ? C4 C3 1.512(4) . ? C4 H4D 0.9900 . ? C4 H4C 0.9900 . ? C3 H3D 0.9900 . ? C3 H3C 0.9900 . ? C5 C6 1.505(4) . ? C6 H6D 0.9799 . ? C6 H6C 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.509(4) . ? C8 H8A 0.9801 . ? C8 H8B 0.9799 . ? C8 H8C 0.9800 . ? C9 C10 1.474(5) . ? C9 H9D 0.9900 . ? C9 H9C 0.9900 . ? C10 H10D 0.9900 . ? C10 H10C 0.9900 . ? C12 C11 1.505(4) . ? C12 H12C 0.9900 . ? C12 H12B 0.9900 . ? C11 H11C 0.9900 . ? C11 H11B 0.9900 . ? C13 C14 1.504(4) . ? C14 H14C 0.9800 . ? C14 H14B 0.9801 . ? C14 H14A 0.9800 . ? C15 C16 1.514(4) . ? C16 H16C 0.9799 . ? C16 H16B 0.9801 . ? C16 H16A 0.9801 . ? S1F O3F 1.429(3) . ? S1F O2F 1.431(3) . ? S1F O1F 1.436(3) . ? S1F C1F 1.830(8) . ? C1F F2F 1.325(4) . ? C1F F1F 1.327(4) . ? C1F F3F 1.328(4) . ? S1F' O1F' 1.433(3) . ? S1F' O3F' 1.433(3) . ? S1F' O2F' 1.433(3) . ? S1F' C1F' 1.823(8) . ? C1F' F2F' 1.328(4) . ? C1F' F3F' 1.329(4) . ? C1F' F1F' 1.329(4) . ? S1F" O1F" 1.431(3) . ? S1F" O3F" 1.433(3) . ? S1F" O2F" 1.433(3) . ? S1F" C1F" 1.824(10) . ? C1F" F3F" 1.328(4) . ? C1F" F2F" 1.329(4) . ? C1F" F1F" 1.330(4) . ? S1F# O1F# 1.432(3) . ? S1F# O2F# 1.432(3) . ? S1F# O3F# 1.432(3) . ? S1F# C1F# 1.826(10) . ? C1F# F1F# 1.328(4) . ? C1F# F3F# 1.328(4) . ? C1F# F2F# 1.328(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 N6 Pd1 N2 93.02(11) . . ? N6 Pd1 O1 92.52(10) . . ? N2 Pd1 O1 170.64(10) . . ? N6 Pd1 N1 175.08(11) . . ? N2 Pd1 N1 83.82(11) . . ? O1 Pd1 N1 90.13(10) . . ? N6 Pd1 Pd2 77.14(8) . . ? N2 Pd1 Pd2 109.64(8) . . ? O1 Pd1 Pd2 78.97(6) . . ? N1 Pd1 Pd2 107.46(8) . . ? N5 Pd2 N4 91.90(11) . . ? N5 Pd2 O2 92.39(10) . . ? N4 Pd2 O2 172.98(9) . . ? N5 Pd2 N3 175.52(11) . . ? N4 Pd2 N3 83.92(10) . . ? O2 Pd2 N3 91.61(10) . . ? N5 Pd2 Pd1 78.68(8) . . ? N4 Pd2 Pd1 105.73(7) . . ? O2 Pd2 Pd1 80.57(6) . . ? N3 Pd2 Pd1 103.98(8) . . ? N12 Pd3 N8 92.76(11) . . ? N12 Pd3 O3 93.42(9) . . ? N8 Pd3 O3 172.70(10) . . ? N12 Pd3 N7 173.31(11) . . ? N8 Pd3 N7 84.19(11) . . ? O3 Pd3 N7 89.24(10) . . ? N12 Pd3 Pd4 74.17(8) . . ? N8 Pd3 Pd4 105.13(8) . . ? O3 Pd3 Pd4 80.33(6) . . ? N7 Pd3 Pd4 112.36(8) . . ? N11 Pd4 N10 92.04(11) . . ? N11 Pd4 O4 92.14(9) . . ? N10 Pd4 O4 171.72(10) . . ? N11 Pd4 N9 174.84(11) . . ? N10 Pd4 N9 83.86(11) . . ? O4 Pd4 N9 91.54(10) . . ? N11 Pd4 Pd3 75.85(8) . . ? N10 Pd4 Pd3 106.60(8) . . ? O4 Pd4 Pd3 81.36(6) . . ? N9 Pd4 Pd3 108.30(8) . . ? O5 S2 O6 116.39(17) . . ? O5 S2 O7 113.49(14) . . ? O6 S2 O7 114.79(15) . . ? O5 S2 C17 104.25(15) . . ? O6 S2 C17 103.75(15) . . ? O7 S2 C17 101.79(14) . . ? O8 S3 O10 115.41(15) . . ? O8 S3 O9 115.55(16) . . ? O10 S3 O9 113.87(15) . . ? O8 S3 C18 103.31(18) . . ? O10 S3 C18 102.65(16) . . ? O9 S3 C18 103.67(16) . . ? O13 S4 O12 115.20(14) . . ? O13 S4 O11 114.56(14) . . ? O12 S4 O11 114.35(14) . . ? O13 S4 C19 104.18(17) . . ? O12 S4 C19 102.90(15) . . ? O11 S4 C19 103.50(15) . . ? C5 O1 Pd1 128.73(19) . . ? C7 O2 Pd2 126.14(18) . . ? C13 O3 Pd3 124.92(18) . . ? C15 O4 Pd4 124.22(19) . . ? H17B O17 H17A 120(4) . . ? H18B O18 H18A 113(5) . . ? C1 N1 Pd1 109.60(18) . . ? C1 N1 H1B 110(3) . . ? Pd1 N1 H1B 105(2) . . ? C1 N1 H1A 110(3) . . ? Pd1 N1 H1A 113(3) . . ? H1B N1 H1A 109(4) . . ? C2 N2 Pd1 108.01(19) . . ? C2 N2 H2B 107(2) . . ? Pd1 N2 H2B 106(2) . . ? C2 N2 H2A 107(2) . . ? Pd1 N2 H2A 113(2) . . ? H2B N2 H2A 116(3) . . ? C4 N4 Pd2 109.18(18) . . ? C4 N4 H4B 109.8 . . ? Pd2 N4 H4B 109.8 . . ? C4 N4 H4A 109.8 . . ? Pd2 N4 H4A 109.8 . . ? H4B N4 H4A 108.3 . . ? C3 N3 Pd2 109.28(19) . . ? C3 N3 H3B 110(3) . . ? Pd2 N3 H3B 110(3) . . ? C3 N3 H3A 108(3) . . ? Pd2 N3 H3A 108(3) . . ? H3B N3 H3A 111(4) . . ? C5 N5 Pd2 129.6(2) . . ? C5 N5 H5A 109(3) . . ? Pd2 N5 H5A 121(3) . . ? C7 N6 Pd1 132.0(2) . . ? C7 N6 H6A 112(3) . . ? Pd1 N6 H6A 116(3) . . ? C9 N7 Pd3 108.7(2) . . ? C9 N7 H7B 107(2) . . ? Pd3 N7 H7B 111(3) . . ? C9 N7 H7A 108(3) . . ? Pd3 N7 H7A 112(3) . . ? H7B N7 H7A 110(4) . . ? C10 N8 Pd3 109.1(2) . . ? C10 N8 H8B 106(3) . . ? Pd3 N8 H8B 113(3) . . ? C10 N8 H8A 111(3) . . ? Pd3 N8 H8A 110(3) . . ? H8B N8 H8A 106(4) . . ? C12 N10 Pd4 108.7(2) . . ? C12 N10 H10B 110(3) . . ? Pd4 N10 H10B 113(3) . . ? C12 N10 H10A 108(3) . . ? Pd4 N10 H10A 111(2) . . ? H10B N10 H10A 106(4) . . ? C11 N9 Pd4 108.88(19) . . ? C11 N9 H9B 111(3) . . ? Pd4 N9 H9B 103(3) . . ? C11 N9 H9A 109(2) . . ? Pd4 N9 H9A 118(2) . . ? H9B N9 H9A 107(3) . . ? C13 N11 Pd4 132.6(2) . . ? C13 N11 H11A 112(3) . . ? Pd4 N11 H11A 115(3) . . ? C15 N12 Pd3 134.4(2) . . ? C15 N12 H12A 117(3) . . ? Pd3 N12 H12A 108(3) . . ? N1 C1 C2 107.4(2) . . ? N1 C1 H1D 110.2 . . ? C2 C1 H1D 110.2 . . ? N1 C1 H1C 110.2 . . ? C2 C1 H1C 110.2 . . ? H1D C1 H1C 108.5 . . ? N2 C2 C1 106.9(3) . . ? N2 C2 H2D 110.3 . . ? C1 C2 H2D 110.3 . . ? N2 C2 H2C 110.3 . . ? C1 C2 H2C 110.3 . . ? H2D C2 H2C 108.6 . . ? N4 C4 C3 107.8(2) . . ? N4 C4 H4D 110.1 . . ? C3 C4 H4D 110.1 . . ? N4 C4 H4C 110.1 . . ? C3 C4 H4C 110.1 . . ? H4D C4 H4C 108.5 . . ? N3 C3 C4 107.7(3) . . ? N3 C3 H3D 110.2 . . ? C4 C3 H3D 110.2 . . ? N3 C3 H3C 110.2 . . ? C4 C3 H3C 110.2 . . ? H3D C3 H3C 108.5 . . ? O1 C5 N5 124.1(3) . . ? O1 C5 C6 114.2(3) . . ? N5 C5 C6 121.7(3) . . ? C5 C6 H6D 109.5 . . ? C5 C6 H6C 109.5 . . ? H6D C6 H6C 109.5 . . ? C5 C6 H6B 109.5 . . ? H6D C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? N6 C7 O2 124.1(3) . . ? N6 C7 C8 120.9(3) . . ? O2 C7 C8 115.0(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N7 109.1(3) . . ? C10 C9 H9D 109.9 . . ? N7 C9 H9D 109.9 . . ? C10 C9 H9C 109.9 . . ? N7 C9 H9C 109.9 . . ? H9D C9 H9C 108.3 . . ? C9 C10 N8 108.9(3) . . ? C9 C10 H10D 109.9 . . ? N8 C10 H10D 109.9 . . ? C9 C10 H10C 109.9 . . ? N8 C10 H10C 109.9 . . ? H10D C10 H10C 108.3 . . ? N10 C12 C11 107.8(2) . . ? N10 C12 H12C 110.2 . . ? C11 C12 H12C 110.2 . . ? N10 C12 H12B 110.2 . . ? C11 C12 H12B 110.2 . . ? H12C C12 H12B 108.5 . . ? N9 C11 C12 107.3(2) . . ? N9 C11 H11C 110.2 . . ? C12 C11 H11C 110.2 . . ? N9 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11C C11 H11B 108.5 . . ? O3 C13 N11 125.3(3) . . ? O3 C13 C14 114.9(3) . . ? N11 C13 C14 119.8(3) . . ? C13 C14 H14C 109.5 . . ? C13 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? C13 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? O4 C15 N12 124.6(3) . . ? O4 C15 C16 115.1(3) . . ? N12 C15 C16 120.3(3) . . ? C15 C16 H16C 109.5 . . ? C15 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? C15 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? F4 C17 F5 107.9(3) . . ? F4 C17 F6 108.1(3) . . ? F5 C17 F6 107.6(3) . . ? F4 C17 S2 110.7(2) . . ? F5 C17 S2 110.3(2) . . ? F6 C17 S2 112.1(2) . . ? F8 C18 F9 108.4(3) . . ? F8 C18 F7 107.6(3) . . ? F9 C18 F7 107.6(3) . . ? F8 C18 S3 111.0(3) . . ? F9 C18 S3 110.3(3) . . ? F7 C18 S3 111.9(3) . . ? F10 C19 F11 107.8(3) . . ? F10 C19 F12 108.5(3) . . ? F11 C19 F12 108.1(3) . . ? F10 C19 S4 110.9(3) . . ? F11 C19 S4 110.8(3) . . ? F12 C19 S4 110.6(2) . . ? O3F S1F O2F 117.5(3) . . ? O3F S1F O1F 113.6(3) . . ? O2F S1F O1F 113.0(3) . . ? O3F S1F C1F 104.3(3) . . ? O2F S1F C1F 103.1(3) . . ? O1F S1F C1F 103.2(3) . . ? F2F C1F F1F 108.6(5) . . ? F2F C1F F3F 108.4(5) . . ? F1F C1F F3F 107.6(5) . . ? F2F C1F S1F 110.7(4) . . ? F1F C1F S1F 110.9(4) . . ? F3F C1F S1F 110.5(4) . . ? O1F' S1F' O3F' 113.6(3) . . ? O1F' S1F' O2F' 114.8(3) . . ? O3F' S1F' O2F' 114.9(3) . . ? O1F' S1F' C1F' 103.9(3) . . ? O3F' S1F' C1F' 104.3(3) . . ? O2F' S1F' C1F' 103.4(3) . . ? F2F' C1F' F3F' 108.7(5) . . ? F2F' C1F' F1F' 108.2(5) . . ? F3F' C1F' F1F' 107.3(5) . . ? F2F' C1F' S1F' 110.6(4) . . ? F3F' C1F' S1F' 110.9(4) . . ? F1F' C1F' S1F' 111.0(4) . . ? O1F" S1F" O3F" 114.4(5) . . ? O1F" S1F" O2F" 114.7(5) . . ? O3F" S1F" O2F" 114.0(5) . . ? O1F" S1F" C1F" 104.3(4) . . ? O3F" S1F" C1F" 103.6(4) . . ? O2F" S1F" C1F" 104.0(4) . . ? F3F" C1F" F2F" 107.9(6) . . ? F3F" C1F" F1F" 108.8(6) . . ? F2F" C1F" F1F" 107.9(6) . . ? F3F" C1F" S1F" 110.7(5) . . ? F2F" C1F" S1F" 110.8(5) . . ? F1F" C1F" S1F" 110.6(5) . . ? O1F# S1F# O2F# 114.6(5) . . ? O1F# S1F# O3F# 114.5(5) . . ? O2F# S1F# O3F# 114.6(5) . . ? O1F# S1F# C1F# 103.6(5) . . ? O2F# S1F# C1F# 103.7(5) . . ? O3F# S1F# C1F# 103.7(5) . . ? F1F# C1F# F3F# 107.9(6) . . ? F1F# C1F# F2F# 108.1(6) . . ? F3F# C1F# F2F# 108.2(6) . . ? F1F# C1F# S1F# 110.8(5) . . ? F3F# C1F# S1F# 110.7(5) . . ? F2F# C1F# S1F# 111.0(5) . . ? 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 N6 Pd1 Pd2 N5 -94.88(11) . . . . ? N2 Pd1 Pd2 N5 176.50(11) . . . . ? O1 Pd1 Pd2 N5 0.31(10) . . . . ? N1 Pd1 Pd2 N5 86.94(11) . . . . ? N6 Pd1 Pd2 N4 176.33(11) . . . . ? N2 Pd1 Pd2 N4 87.72(11) . . . . ? O1 Pd1 Pd2 N4 -88.48(10) . . . . ? N1 Pd1 Pd2 N4 -1.85(11) . . . . ? N6 Pd1 Pd2 O2 -0.50(10) . . . . ? N2 Pd1 Pd2 O2 -89.12(10) . . . . ? O1 Pd1 Pd2 O2 94.69(9) . . . . ? N1 Pd1 Pd2 O2 -178.68(10) . . . . ? N6 Pd1 Pd2 N3 88.81(11) . . . . ? N2 Pd1 Pd2 N3 0.20(11) . . . . ? O1 Pd1 Pd2 N3 -176.00(10) . . . . ? N1 Pd1 Pd2 N3 -89.37(11) . . . . ? N12 Pd3 Pd4 N11 -101.92(11) . . . . ? N8 Pd3 Pd4 N11 169.50(11) . . . . ? O3 Pd3 Pd4 N11 -5.53(10) . . . . ? N7 Pd3 Pd4 N11 79.62(11) . . . . ? N12 Pd3 Pd4 N10 170.19(11) . . . . ? N8 Pd3 Pd4 N10 81.61(11) . . . . ? O3 Pd3 Pd4 N10 -93.42(10) . . . . ? N7 Pd3 Pd4 N10 -8.27(12) . . . . ? N12 Pd3 Pd4 O4 -7.49(10) . . . . ? N8 Pd3 Pd4 O4 -96.07(10) . . . . ? O3 Pd3 Pd4 O4 88.90(9) . . . . ? N7 Pd3 Pd4 O4 174.05(10) . . . . ? N12 Pd3 Pd4 N9 81.27(11) . . . . ? N8 Pd3 Pd4 N9 -7.31(11) . . . . ? O3 Pd3 Pd4 N9 177.66(10) . . . . ? N7 Pd3 Pd4 N9 -97.19(11) . . . . ? N6 Pd1 O1 C5 76.4(3) . . . . ? N2 Pd1 O1 C5 -157.3(6) . . . . ? N1 Pd1 O1 C5 -107.7(3) . . . . ? Pd2 Pd1 O1 C5 0.1(2) . . . . ? N5 Pd2 O2 C7 78.1(2) . . . . ? N4 Pd2 O2 C7 -154.3(7) . . . . ? N3 Pd2 O2 C7 -104.0(2) . . . . ? Pd1 Pd2 O2 C7 0.0(2) . . . . ? N12 Pd3 O3 C13 83.3(2) . . . . ? N8 Pd3 O3 C13 -128.8(8) . . . . ? N7 Pd3 O3 C13 -102.8(2) . . . . ? Pd4 Pd3 O3 C13 10.0(2) . . . . ? N11 Pd4 O4 C15 83.8(2) . . . . ? N10 Pd4 O4 C15 -155.9(6) . . . . ? N9 Pd4 O4 C15 -99.8(2) . . . . ? Pd3 Pd4 O4 C15 8.5(2) . . . . ? N6 Pd1 N1 C1 -59.5(13) . . . . ? N2 Pd1 N1 C1 -9.4(2) . . . . ? O1 Pd1 N1 C1 177.8(2) . . . . ? Pd2 Pd1 N1 C1 99.31(19) . . . . ? N6 Pd1 N2 C2 156.3(2) . . . . ? O1 Pd1 N2 C2 30.1(7) . . . . ? N1 Pd1 N2 C2 -19.9(2) . . . . ? Pd2 Pd1 N2 C2 -126.27(19) . . . . ? N5 Pd2 N4 C4 -165.9(2) . . . . ? O2 Pd2 N4 C4 66.4(8) . . . . ? N3 Pd2 N4 C4 15.7(2) . . . . ? Pd1 Pd2 N4 C4 -87.15(19) . . . . ? N5 Pd2 N3 C3 -8.6(15) . . . . ? N4 Pd2 N3 C3 12.6(2) . . . . ? O2 Pd2 N3 C3 -162.0(2) . . . . ? Pd1 Pd2 N3 C3 117.36(19) . . . . ? N4 Pd2 N5 C5 104.8(3) . . . . ? O2 Pd2 N5 C5 -80.7(3) . . . . ? N3 Pd2 N5 C5 125.9(14) . . . . ? Pd1 Pd2 N5 C5 -0.9(3) . . . . ? N2 Pd1 N6 C7 110.9(3) . . . . ? O1 Pd1 N6 C7 -76.7(3) . . . . ? N1 Pd1 N6 C7 160.7(11) . . . . ? Pd2 Pd1 N6 C7 1.4(3) . . . . ? N12 Pd3 N7 C9 -51.9(10) . . . . ? N8 Pd3 N7 C9 11.3(2) . . . . ? O3 Pd3 N7 C9 -165.5(2) . . . . ? Pd4 Pd3 N7 C9 115.3(2) . . . . ? N12 Pd3 N8 C10 -171.0(2) . . . . ? O3 Pd3 N8 C10 41.1(9) . . . . ? N7 Pd3 N8 C10 15.0(2) . . . . ? Pd4 Pd3 N8 C10 -96.7(2) . . . . ? N11 Pd4 N10 C12 160.8(2) . . . . ? O4 Pd4 N10 C12 40.5(8) . . . . ? N9 Pd4 N10 C12 -16.0(2) . . . . ? Pd3 Pd4 N10 C12 -123.34(18) . . . . ? N11 Pd4 N9 C11 -50.5(13) . . . . ? N10 Pd4 N9 C11 -12.9(2) . . . . ? O4 Pd4 N9 C11 173.99(19) . . . . ? Pd3 Pd4 N9 C11 92.58(19) . . . . ? N10 Pd4 N11 C13 110.4(3) . . . . ? O4 Pd4 N11 C13 -76.8(3) . . . . ? N9 Pd4 N11 C13 147.8(11) . . . . ? Pd3 Pd4 N11 C13 3.8(3) . . . . ? N8 Pd3 N12 C15 116.1(3) . . . . ? O3 Pd3 N12 C15 -67.8(3) . . . . ? N7 Pd3 N12 C15 179(16) . . . . ? Pd4 Pd3 N12 C15 11.1(3) . . . . ? Pd1 N1 C1 C2 36.3(3) . . . . ? Pd1 N2 C2 C1 45.0(3) . . . . ? N1 C1 C2 N2 -53.5(3) . . . . ? Pd2 N4 C4 C3 -40.6(3) . . . . ? Pd2 N3 C3 C4 -37.9(3) . . . . ? N4 C4 C3 N3 51.6(3) . . . . ? Pd1 O1 C5 N5 -0.7(4) . . . . ? Pd1 O1 C5 C6 179.5(2) . . . . ? Pd2 N5 C5 O1 1.2(5) . . . . ? Pd2 N5 C5 C6 -178.9(2) . . . . ? Pd1 N6 C7 O2 -1.9(5) . . . . ? Pd1 N6 C7 C8 178.2(2) . . . . ? Pd2 O2 C7 N6 1.0(4) . . . . ? Pd2 O2 C7 C8 -179.1(2) . . . . ? Pd3 N7 C9 C10 -36.0(4) . . . . ? N7 C9 C10 N8 49.6(4) . . . . ? Pd3 N8 C10 C9 -39.2(4) . . . . ? Pd4 N10 C12 C11 41.9(3) . . . . ? Pd4 N9 C11 C12 38.9(3) . . . . ? N10 C12 C11 N9 -53.3(3) . . . . ? Pd3 O3 C13 N11 -11.5(4) . . . . ? Pd3 O3 C13 C14 166.91(19) . . . . ? Pd4 N11 C13 O3 2.6(5) . . . . ? Pd4 N11 C13 C14 -175.7(2) . . . . ? Pd4 O4 C15 N12 -4.5(4) . . . . ? Pd4 O4 C15 C16 176.2(2) . . . . ? Pd3 N12 C15 O4 -8.8(5) . . . . ? Pd3 N12 C15 C16 170.5(2) . . . . ? O5 S2 C17 F4 175.5(2) . . . . ? O6 S2 C17 F4 -62.2(3) . . . . ? O7 S2 C17 F4 57.3(3) . . . . ? O5 S2 C17 F5 56.2(3) . . . . ? O6 S2 C17 F5 178.5(2) . . . . ? O7 S2 C17 F5 -62.0(3) . . . . ? O5 S2 C17 F6 -63.6(3) . . . . ? O6 S2 C17 F6 58.7(3) . . . . ? O7 S2 C17 F6 178.2(2) . . . . ? O8 S3 C18 F8 -62.0(3) . . . . ? O10 S3 C18 F8 58.3(3) . . . . ? O9 S3 C18 F8 177.1(3) . . . . ? O8 S3 C18 F9 58.1(3) . . . . ? O10 S3 C18 F9 178.4(2) . . . . ? O9 S3 C18 F9 -62.8(3) . . . . ? O8 S3 C18 F7 177.8(2) . . . . ? O10 S3 C18 F7 -61.9(3) . . . . ? O9 S3 C18 F7 56.9(3) . . . . ? O13 S4 C19 F10 55.7(3) . . . . ? O12 S4 C19 F10 -64.8(3) . . . . ? O11 S4 C19 F10 175.8(3) . . . . ? O13 S4 C19 F11 -63.9(3) . . . . ? O12 S4 C19 F11 175.5(3) . . . . ? O11 S4 C19 F11 56.2(3) . . . . ? O13 S4 C19 F12 176.2(2) . . . . ? O12 S4 C19 F12 55.7(3) . . . . ? O11 S4 C19 F12 -63.7(3) . . . . ? O3F S1F C1F F2F 50.4(4) . . . . ? O2F S1F C1F F2F 173.7(4) . . . . ? O1F S1F C1F F2F -68.5(4) . . . . ? O3F S1F C1F F1F -70.3(4) . . . . ? O2F S1F C1F F1F 53.0(4) . . . . ? O1F S1F C1F F1F 170.8(4) . . . . ? O3F S1F C1F F3F 170.5(4) . . . . ? O2F S1F C1F F3F -66.2(4) . . . . ? O1F S1F C1F F3F 51.6(4) . . . . ? O1F' S1F' C1F' F2F' -70.8(4) . . . . ? O3F' S1F' C1F' F2F' 48.5(4) . . . . ? O2F' S1F' C1F' F2F' 168.9(4) . . . . ? O1F' S1F' C1F' F3F' 49.9(4) . . . . ? O3F' S1F' C1F' F3F' 169.2(4) . . . . ? O2F' S1F' C1F' F3F' -70.4(4) . . . . ? O1F' S1F' C1F' F1F' 169.1(4) . . . . ? O3F' S1F' C1F' F1F' -71.6(4) . . . . ? O2F' S1F' C1F' F1F' 48.8(4) . . . . ? O1F" S1F" C1F" F3F" -77.4(11) . . . . ? O3F" S1F" C1F" F3F" 162.5(12) . . . . ? O2F" S1F" C1F" F3F" 43.1(12) . . . . ? O1F" S1F" C1F" F2F" 42.2(11) . . . . ? O3F" S1F" C1F" F2F" -77.8(11) . . . . ? O2F" S1F" C1F" F2F" 162.8(11) . . . . ? O1F" S1F" C1F" F1F" 161.9(11) . . . . ? O3F" S1F" C1F" F1F" 41.9(11) . . . . ? O2F" S1F" C1F" F1F" -77.6(11) . . . . ? O1F# S1F# C1F# F1F# 166.0(16) . . . . ? O2F# S1F# C1F# F1F# 45.9(16) . . . . ? O3F# S1F# C1F# F1F# -74.1(16) . . . . ? O1F# S1F# C1F# F3F# 46.3(16) . . . . ? O2F# S1F# C1F# F3F# -73.8(16) . . . . ? O3F# S1F# C1F# F3F# 166.1(16) . . . . ? O1F# S1F# C1F# F2F# -73.9(16) . . . . ? O2F# S1F# C1F# F2F# 166.0(16) . . . . ? O3F# S1F# C1F# F2F# 46.0(16) . . . . ? 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 N1 H1B O2 0.82(4) 2.03(4) 2.846(3) 169(3) 2 N1 H1A O10 0.78(4) 2.20(4) 2.974(4) 175(4) . N2 H2B O7 0.86(4) 2.05(4) 2.885(4) 164(3) . N2 H2A O18 0.89(4) 2.08(4) 2.943(4) 163(3) . N5 H5A O1F 0.73(4) 2.21(4) 2.942(6) 174(4) 4_566 N5 H5A O1F' 0.73(4) 2.50(4) 3.232(6) 175(4) 4_566 N6 H6A O17 0.74(4) 2.24(4) 2.974(3) 174(4) 2 N7 H7B O4 0.86(4) 2.21(4) 2.988(4) 151(3) 2_655 N7 H7B F3F" 0.86(4) 2.56(4) 3.013(11) 114(3) 3_665 N7 H7A F1F" 0.75(4) 2.72(5) 3.44(2) 160(4) . N7 H7A O3F" 0.75(4) 2.49(4) 3.075(17) 136(4) . N7 H7A O3F' 0.75(4) 2.49(4) 3.183(7) 155(4) . N7 H7A O3F# 0.75(4) 1.93(5) 2.40(3) 121(4) . N8 H8A O12 0.82(4) 2.17(4) 2.987(4) 175(4) . N8 H8B O9 0.84(4) 2.20(4) 3.014(4) 165(3) . N11 H11A O12 0.73(4) 2.33(4) 3.053(3) 172(4) 2_645 N12 H12A O11 0.70(4) 2.34(4) 3.031(3) 170(4) . O17 H17B O18 0.84(4) 1.90(4) 2.733(4) 170(4) 2_545 O17 H17A O5 0.68(4) 2.19(4) 2.854(4) 165(5) 3 O18 H18B O2F' 0.70(4) 1.96(5) 2.639(6) 164(5) 3_565 O18 H18B O1F" 0.70(4) 2.33(5) 2.950(16) 150(5) 3_565 O18 H18B O2F 0.70(4) 2.39(5) 3.088(7) 173(5) 3_565 O18 H18B O1F 0.70(4) 2.54(5) 3.023(7) 129(4) 3_565 O18 H18A O13 0.69(5) 2.14(5) 2.768(4) 154(5) 2_545 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.000 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.101