# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 839286' #TrackingRef '291221b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H76 N16 O2 Pd4, 4.2(H2 O), 4(N O3), 2(H0.80 O0.40)' _chemical_formula_sum 'C94 H86 N20 O19 Pd4' _chemical_formula_weight 2225.43 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' 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 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 40.030(3) _cell_length_b 12.6014(18) _cell_length_c 21.3785(15) _cell_angle_alpha 90.00 _cell_angle_beta 92.539(3) _cell_angle_gamma 90.00 _cell_volume 10773.6(19) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 4036 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 21.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4504 _exptl_absorpt_coefficient_mu 0.727 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8223 _exptl_absorpt_correction_T_max 0.8564 _exptl_absorpt_process_details 'sadabs; bRUKER, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36308 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10593 _reflns_number_gt 7348 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.06P)^2^+1.55P] 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 10593 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1322 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.000 _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 C1 C 0.81581(12) 0.3825(4) 0.1901(3) 0.0470(12) Uani 1 1 d . . . H1 H 0.8256 0.3468 0.2243 0.056 Uiso 1 1 calc R . . C2 C 0.78416(12) 0.4327(4) 0.1942(2) 0.0447(12) Uani 1 1 d . . . H2 H 0.7737 0.4319 0.2322 0.054 Uiso 1 1 calc R . . C3 C 0.76887(12) 0.4810(4) 0.1450(2) 0.0476(13) Uani 1 1 d . . . H3 H 0.7480 0.5120 0.1491 0.057 Uiso 1 1 calc R . . C4 C 0.78415(11) 0.4850(4) 0.0874(2) 0.0379(10) Uani 1 1 d . . . C5 C 0.77000(13) 0.5304(4) 0.0308(2) 0.0445(11) Uani 1 1 d . . . H5 H 0.7486 0.5590 0.0312 0.053 Uiso 1 1 calc R . . C6 C 0.78590(12) 0.5335(4) -0.0219(2) 0.0428(11) Uani 1 1 d . . . H6 H 0.7763 0.5680 -0.0567 0.051 Uiso 1 1 calc R . . C7 C 0.81820(13) 0.4833(4) -0.0255(2) 0.0456(12) Uani 1 1 d . . . C8 C 0.83680(12) 0.4845(4) -0.0792(2) 0.0431(11) Uani 1 1 d . . . H8 H 0.8288 0.5190 -0.1153 0.052 Uiso 1 1 calc R . . C9 C 0.86801(11) 0.4325(4) -0.0776(2) 0.0390(11) Uani 1 1 d . . . H9 H 0.8807 0.4318 -0.1130 0.047 Uiso 1 1 calc R . . C10 C 0.87974(12) 0.3823(4) -0.0230(2) 0.0402(11) Uani 1 1 d . . . H10 H 0.8997 0.3443 -0.0230 0.048 Uiso 1 1 calc R . . C11 C 0.83258(12) 0.4380(4) 0.0282(2) 0.0458(12) Uani 1 1 d . . . C12 C 0.81530(12) 0.4379(3) 0.0848(2) 0.0411(11) Uani 1 1 d . . . C13 C 0.83324(13) 0.0118(4) 0.2162(3) 0.0474(12) Uani 1 1 d . . . H13 H 0.8420 0.0589 0.2462 0.057 Uiso 1 1 calc R . . C14 C 0.80407(12) -0.0489(4) 0.2290(2) 0.0433(12) Uani 1 1 d . . . H14 H 0.7949 -0.0440 0.2682 0.052 Uiso 1 1 calc R . . C15 C 0.78945(12) -0.1138(4) 0.1846(2) 0.0422(11) Uani 1 1 d . . . H15 H 0.7699 -0.1503 0.1925 0.051 Uiso 1 1 calc R . . C16 C 0.80462(12) -0.1248(4) 0.1255(2) 0.0412(11) Uani 1 1 d . . . C17 C 0.79203(13) -0.1889(4) 0.0740(3) 0.0487(13) Uani 1 1 d . . . H17 H 0.7726 -0.2284 0.0782 0.058 Uiso 1 1 calc R . . C18 C 0.80793(12) -0.1928(4) 0.0196(2) 0.0431(11) Uani 1 1 d . . . H18 H 0.7997 -0.2369 -0.0123 0.052 Uiso 1 1 calc R . . C19 C 0.83628(12) -0.1325(4) 0.0102(2) 0.0428(11) Uani 1 1 d . . . C20 C 0.85406(12) -0.1326(4) -0.0456(2) 0.0401(11) Uani 1 1 d . . . H20 H 0.8466 -0.1742 -0.0793 0.048 Uiso 1 1 calc R . . C21 C 0.88200(13) -0.0723(4) -0.0501(2) 0.0476(12) Uani 1 1 d . . . H21 H 0.8937 -0.0735 -0.0867 0.057 Uiso 1 1 calc R . . C22 C 0.89307(13) -0.0097(4) -0.0009(2) 0.0433(11) Uani 1 1 d . . . H22 H 0.9119 0.0324 -0.0051 0.052 Uiso 1 1 calc R . . C23 C 0.85015(12) -0.0694(4) 0.0589(2) 0.0411(11) Uani 1 1 d . . . C24 C 0.83413(11) -0.0636(4) 0.1167(2) 0.0376(10) Uani 1 1 d . . . C25 C 0.97161(12) 0.0319(4) 0.1020(2) 0.0421(11) Uani 1 1 d . . . H25A H 0.9571 -0.0102 0.1265 0.063 Uiso 1 1 calc R . . H25B H 0.9935 0.0342 0.1222 0.063 Uiso 1 1 calc R . . H25C H 0.9730 0.0008 0.0612 0.063 Uiso 1 1 calc R . . C26 C 0.95774(12) 0.1439(4) 0.0956(2) 0.0420(11) Uani 1 1 d . . . C27 C 0.97538(12) 0.2394(4) 0.0882(2) 0.0398(11) Uani 1 1 d . . . C28 C 0.94982(13) 0.3172(4) 0.0856(2) 0.0447(11) Uani 1 1 d . . . C29 C 0.95373(12) 0.4380(4) 0.0799(2) 0.0424(11) Uani 1 1 d . . . H29A H 0.9390 0.4638 0.0466 0.064 Uiso 1 1 calc R . . H29B H 0.9764 0.4547 0.0709 0.064 Uiso 1 1 calc R . . H29C H 0.9482 0.4711 0.1186 0.064 Uiso 1 1 calc R . . C30 C 0.92395(12) 0.0426(4) 0.2790(2) 0.0408(11) Uani 1 1 d . . . H30A H 0.9073 0.0094 0.3034 0.061 Uiso 1 1 calc R . . H30B H 0.9445 0.0480 0.3036 0.061 Uiso 1 1 calc R . . H30C H 0.9274 0.0008 0.2424 0.061 Uiso 1 1 calc R . . C31 C 0.91226(12) 0.1523(4) 0.2597(2) 0.0390(11) Uani 1 1 d . . . C32 C 0.91637(12) 0.2501(4) 0.2923(2) 0.0378(10) Uani 1 1 d . . . C33 C 0.90110(13) 0.3258(4) 0.2528(3) 0.0474(12) Uani 1 1 d . . . C34 C 0.89825(12) 0.4440(4) 0.2621(2) 0.0449(12) Uani 1 1 d . . . H34A H 0.9102 0.4801 0.2305 0.067 Uiso 1 1 calc R . . H34B H 0.9076 0.4628 0.3027 0.067 Uiso 1 1 calc R . . H34C H 0.8751 0.4644 0.2589 0.067 Uiso 1 1 calc R . . C35 C 0.93551(12) 0.2639(4) 0.3527(2) 0.0409(11) Uani 1 1 d . . . C36 C 0.92020(13) 0.2939(4) 0.4067(2) 0.0420(11) Uani 1 1 d . . . H36 H 0.8976 0.3109 0.4052 0.050 Uiso 1 1 calc R . . C37 C 0.93842(14) 0.2984(4) 0.4624(2) 0.0486(12) Uani 1 1 d . . . C38 C 0.97276(13) 0.2807(4) 0.4671(3) 0.0494(13) Uani 1 1 d . . . H38 H 0.9847 0.2850 0.5053 0.059 Uiso 1 1 calc R . . C39 C 0.98876(12) 0.2555(4) 0.4104(2) 0.0425(11) Uani 1 1 d . . . C40 C 0.97013(12) 0.2459(4) 0.3547(2) 0.0434(11) Uani 1 1 d . . . H40 H 0.9806 0.2274 0.3183 0.052 Uiso 1 1 calc R . . C41 C 0.93466(13) 0.2871(4) 0.5728(2) 0.0428(11) Uani 1 1 d . . . H41A H 0.9535 0.3324 0.5845 0.051 Uiso 1 1 calc R . . H41B H 0.9428 0.2150 0.5687 0.051 Uiso 1 1 calc R . . C42 C 0.90875(12) 0.2918(4) 0.6226(2) 0.0428(11) Uani 1 1 d . . . C43 C 0.87779(12) 0.3360(4) 0.6117(2) 0.0427(11) Uani 1 1 d . . . H43 H 0.8721 0.3656 0.5728 0.051 Uiso 1 1 calc R . . C44 C 0.85426(13) 0.3367(4) 0.6599(2) 0.0420(11) Uani 1 1 d . . . H44 H 0.8328 0.3632 0.6518 0.050 Uiso 1 1 calc R . . C45 C 0.86332(12) 0.2985(4) 0.7175(2) 0.0449(12) Uani 1 1 d . . . H45 H 0.8482 0.3019 0.7493 0.054 Uiso 1 1 calc R . . C46 C 0.89522(14) 0.2538(4) 0.7303(2) 0.0500(13) Uani 1 1 d . . . H46 H 0.9011 0.2263 0.7696 0.060 Uiso 1 1 calc R . . C47 C 0.91797(13) 0.2522(4) 0.6814(2) 0.0423(12) Uani 1 1 d . . . H47 H 0.9393 0.2244 0.6888 0.051 Uiso 1 1 calc R . . N1 N 0.83142(11) 0.3879(3) 0.1352(2) 0.0474(10) Uani 1 1 d . . . N2 N 0.86290(12) 0.3878(3) 0.0295(2) 0.0485(10) Uani 1 1 d . . . N3 N 0.87684(10) -0.0077(3) 0.0548(2) 0.0448(10) Uani 1 1 d . . . N4 N 0.84833(11) 0.0014(4) 0.1609(2) 0.0506(11) Uani 1 1 d . . . N5 N 0.92502(11) 0.1629(3) 0.0966(2) 0.0434(9) Uani 1 1 d . . . N6 N 0.92041(10) 0.2717(3) 0.09104(19) 0.0427(9) Uani 1 1 d . . . N7 N 0.89495(11) 0.1715(3) 0.20672(19) 0.0463(10) Uani 1 1 d . . . N8 N 0.88814(10) 0.2759(3) 0.20156(19) 0.0415(9) Uani 1 1 d . . . N9 N 0.95152(12) 0.1659(4) 0.8926(2) 0.0517(11) Uani 1 1 d . . . N13 N 0.79874(11) 0.7618(3) 0.83368(19) 0.0441(10) Uani 1 1 d . . . O1 O 0.91975(8) 0.3212(3) 0.51550(15) 0.0421(8) Uani 1 1 d . . . O2 O 0.78372(10) 0.8276(3) 0.86257(17) 0.0529(9) Uani 1 1 d . . . O3 O 0.82597(9) 0.7819(3) 0.81324(16) 0.0473(9) Uani 1 1 d . . . O4 O 0.78751(9) 0.6728(3) 0.82782(17) 0.0530(9) Uani 1 1 d . . . O5 O 0.95843(9) 0.0811(3) 0.91739(18) 0.0538(9) Uani 1 1 d . . . O6 O 0.96881(9) 0.2007(3) 0.85145(17) 0.0501(9) Uani 1 1 d . . . O7 O 0.92675(9) 0.2140(3) 0.90658(17) 0.0502(9) Uani 1 1 d . . . O1W O 0.8370(2) 0.1433(6) 0.8806(4) 0.045(2) Uani 0.40 1 d P . . H1X H 0.8553 0.1115 0.8899 0.054 Uiso 0.40 1 d PR . . H1Y H 0.8207 0.1038 0.8898 0.054 Uiso 0.40 1 d PR . . O2W O 0.7699(2) 0.6700(8) 0.3117(4) 0.056(2) Uani 0.40 1 d P . . H2X H 0.7609 0.7296 0.3187 0.067 Uiso 0.40 1 d PR . . H2Y H 0.7567 0.6327 0.2885 0.067 Uiso 0.40 1 d PR . . O3W O 0.0192(2) 0.6088(7) 0.1294(4) 0.053(2) Uani 0.40 1 d P . . H3X H 0.0134 0.6398 0.0953 0.064 Uiso 0.40 1 d PR . . H3Y H 0.0127 0.5447 0.1279 0.064 Uiso 0.40 1 d PR . . O4W O 1.0000 0.5052(5) 0.2500 0.0492(15) Uani 0.80 2 d SP . . H4X H 0.9789 0.4992 0.2501 0.059 Uiso 0.40 1 d PR . . H4Y H 1.0068 0.5432 0.2809 0.059 Uiso 0.40 1 d PR . . O5W O 0.0000 0.8361(4) 0.2500 0.0517(13) Uani 1 2 d S . . H5X H -0.0057 0.8586 0.2855 0.062 Uiso 0.50 1 d PR . . H5Y H 0.0195 0.8586 0.2429 0.062 Uiso 0.50 1 d PR . . O6W O 0.78219(18) 0.2182(6) 0.9968(3) 0.0326(16) Uiso 0.40 1 d P . . H6X H 0.7995 0.1868 1.0120 0.039 Uiso 0.40 1 d PR . . H6Y H 0.7804 0.2786 1.0140 0.039 Uiso 0.40 1 d PR . . Pd1 Pd 0.876297(10) 0.33063(3) 0.115373(18) 0.04442(12) Uani 1 1 d . . . Pd2 Pd 0.887115(9) 0.08168(3) 0.130758(18) 0.04285(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(3) 0.044(3) 0.057(3) -0.001(2) 0.010(2) 0.016(2) C2 0.043(3) 0.047(3) 0.045(3) 0.009(2) 0.009(2) 0.015(2) C3 0.036(3) 0.059(3) 0.049(3) 0.012(2) 0.013(2) 0.019(2) C4 0.036(2) 0.038(3) 0.039(3) -0.0008(19) -0.0068(19) 0.0115(19) C5 0.049(3) 0.041(3) 0.042(3) 0.010(2) -0.014(2) 0.002(2) C6 0.045(3) 0.038(3) 0.043(3) 0.008(2) -0.017(2) -0.006(2) C7 0.045(3) 0.052(3) 0.039(3) 0.024(2) -0.004(2) 0.007(2) C8 0.042(3) 0.046(3) 0.041(3) 0.021(2) 0.003(2) 0.010(2) C9 0.038(2) 0.039(3) 0.040(2) 0.012(2) 0.007(2) 0.015(2) C10 0.046(3) 0.039(3) 0.036(3) 0.015(2) 0.008(2) 0.015(2) C11 0.037(3) 0.050(3) 0.050(3) 0.016(2) 0.000(2) 0.004(2) C12 0.041(2) 0.027(2) 0.055(3) 0.001(2) -0.010(2) 0.0006(19) C13 0.041(3) 0.040(3) 0.062(3) -0.009(2) 0.014(2) -0.007(2) C14 0.047(3) 0.038(3) 0.047(3) -0.013(2) 0.025(2) -0.014(2) C15 0.040(3) 0.033(2) 0.055(3) 0.010(2) 0.015(2) -0.008(2) C16 0.042(3) 0.042(3) 0.039(3) -0.004(2) -0.011(2) -0.004(2) C17 0.037(3) 0.051(3) 0.057(3) -0.005(2) -0.014(2) -0.007(2) C18 0.044(3) 0.041(3) 0.043(3) -0.004(2) -0.011(2) 0.007(2) C19 0.042(3) 0.047(3) 0.038(3) -0.013(2) -0.015(2) 0.011(2) C20 0.049(3) 0.034(2) 0.036(2) -0.0136(19) -0.011(2) 0.012(2) C21 0.053(3) 0.046(3) 0.044(3) -0.018(2) 0.009(2) 0.005(2) C22 0.051(3) 0.033(2) 0.047(3) -0.001(2) 0.013(2) 0.005(2) C23 0.046(3) 0.034(2) 0.043(3) -0.006(2) -0.006(2) 0.000(2) C24 0.034(2) 0.037(3) 0.040(3) 0.0033(19) -0.0094(19) 0.0002(19) C25 0.042(3) 0.045(3) 0.039(3) 0.007(2) -0.008(2) 0.011(2) C26 0.042(3) 0.039(3) 0.046(3) -0.015(2) 0.017(2) 0.001(2) C27 0.036(2) 0.041(3) 0.041(3) -0.013(2) -0.007(2) 0.002(2) C28 0.042(3) 0.042(3) 0.050(3) 0.001(2) -0.001(2) 0.000(2) C29 0.042(3) 0.039(3) 0.047(3) 0.019(2) 0.004(2) -0.005(2) C30 0.044(3) 0.032(2) 0.045(3) -0.001(2) -0.012(2) 0.009(2) C31 0.039(3) 0.036(3) 0.042(3) 0.007(2) 0.000(2) 0.0025(19) C32 0.038(2) 0.042(3) 0.033(2) 0.0002(19) -0.0092(19) -0.001(2) C33 0.045(3) 0.049(3) 0.049(3) -0.001(2) 0.006(2) 0.008(2) C34 0.039(2) 0.048(3) 0.047(3) -0.014(2) -0.013(2) 0.023(2) C35 0.046(3) 0.040(3) 0.036(2) -0.006(2) -0.003(2) -0.001(2) C36 0.049(3) 0.040(3) 0.037(3) -0.001(2) 0.009(2) -0.006(2) C37 0.053(3) 0.057(3) 0.036(3) 0.005(2) 0.003(2) 0.005(2) C38 0.043(3) 0.045(3) 0.060(3) -0.014(2) 0.001(2) 0.003(2) C39 0.036(3) 0.044(3) 0.049(3) 0.001(2) 0.015(2) 0.012(2) C40 0.043(3) 0.048(3) 0.039(3) -0.003(2) 0.001(2) -0.003(2) C41 0.044(3) 0.043(3) 0.042(3) 0.010(2) 0.007(2) 0.009(2) C42 0.042(3) 0.046(3) 0.041(3) -0.011(2) 0.010(2) 0.005(2) C43 0.043(3) 0.041(3) 0.045(3) -0.008(2) 0.013(2) -0.005(2) C44 0.048(3) 0.041(3) 0.037(3) -0.002(2) 0.008(2) -0.004(2) C45 0.038(3) 0.059(3) 0.039(3) -0.003(2) 0.013(2) -0.008(2) C46 0.059(3) 0.055(3) 0.038(3) 0.006(2) 0.016(2) 0.015(3) C47 0.046(3) 0.046(3) 0.036(3) 0.011(2) 0.019(2) 0.013(2) N1 0.047(2) 0.050(3) 0.045(2) 0.0002(19) -0.004(2) 0.0077(19) N2 0.060(3) 0.042(2) 0.043(2) -0.0044(19) 0.004(2) 0.008(2) N3 0.038(2) 0.048(2) 0.049(2) -0.0102(19) 0.0047(18) 0.0061(18) N4 0.051(3) 0.054(3) 0.048(3) -0.009(2) 0.008(2) -0.011(2) N5 0.045(2) 0.041(2) 0.044(2) 0.0019(18) 0.0079(18) 0.0010(18) N6 0.037(2) 0.047(2) 0.044(2) 0.0018(19) -0.0014(17) 0.0094(18) N7 0.051(2) 0.046(2) 0.042(2) 0.0030(19) -0.0024(19) 0.009(2) N8 0.041(2) 0.040(2) 0.043(2) -0.0059(18) -0.0026(18) 0.0069(17) N9 0.052(3) 0.050(3) 0.053(3) 0.018(2) -0.004(2) -0.018(2) N13 0.052(3) 0.042(2) 0.039(2) -0.0158(18) 0.0136(19) -0.0165(19) O1 0.0455(19) 0.0406(18) 0.0401(18) -0.0013(14) 0.0006(15) 0.0186(15) O2 0.056(2) 0.054(2) 0.048(2) -0.0129(17) -0.0113(17) 0.0185(18) O3 0.050(2) 0.049(2) 0.0443(19) -0.0142(16) 0.0153(16) -0.0221(16) O4 0.053(2) 0.055(2) 0.049(2) 0.0185(17) -0.0148(17) -0.0180(18) O5 0.053(2) 0.057(2) 0.053(2) -0.0136(19) 0.0161(18) -0.0128(18) O6 0.057(2) 0.045(2) 0.047(2) 0.0164(16) -0.0191(17) -0.0170(16) O7 0.044(2) 0.052(2) 0.052(2) -0.0163(17) -0.0181(16) 0.0204(16) O1W 0.049(5) 0.035(5) 0.051(5) 0.012(4) -0.012(4) 0.005(4) O2W 0.063(6) 0.067(6) 0.042(5) 0.003(4) 0.028(4) 0.003(5) O3W 0.057(5) 0.054(5) 0.046(5) 0.013(4) -0.028(4) -0.024(4) O4W 0.044(3) 0.055(4) 0.050(4) 0.000 0.019(3) 0.000 O5W 0.049(3) 0.057(3) 0.048(3) 0.000 -0.021(2) 0.000 Pd1 0.0382(2) 0.0516(2) 0.0430(2) 0.00128(17) -0.00312(16) 0.00575(17) Pd2 0.0392(2) 0.0473(2) 0.0420(2) -0.00503(17) 0.00162(16) -0.00324(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.356(6) . ? C1 C2 1.422(7) . ? C1 H1 0.9300 . ? C2 C3 1.340(7) . ? C2 H2 0.9300 . ? C3 C4 1.400(7) . ? C3 H3 0.9300 . ? C4 C12 1.384(6) . ? C4 C5 1.432(6) . ? C5 C6 1.319(7) . ? C5 H5 0.9300 . ? C6 C7 1.445(7) . ? C6 H6 0.9300 . ? C7 C11 1.384(7) . ? C7 C8 1.396(7) . ? C8 C9 1.410(6) . ? C8 H8 0.9300 . ? C9 C10 1.391(6) . ? C9 H9 0.9300 . ? C10 N2 1.337(6) . ? C10 H10 0.9300 . ? C11 N2 1.368(6) . ? C11 C12 1.420(7) . ? C12 N1 1.383(6) . ? C13 N4 1.358(7) . ? C13 C14 1.432(6) . ? C13 H13 0.9300 . ? C14 C15 1.365(7) . ? C14 H14 0.9300 . ? C15 C16 1.431(7) . ? C15 H15 0.9300 . ? C16 C24 1.430(7) . ? C16 C17 1.439(7) . ? C17 C18 1.351(8) . ? C17 H17 0.9300 . ? C18 C19 1.388(7) . ? C18 H18 0.9300 . ? C19 C23 1.405(6) . ? C19 C20 1.415(7) . ? C20 C21 1.359(7) . ? C20 H20 0.9300 . ? C21 C22 1.373(7) . ? C21 H21 0.9300 . ? C22 N3 1.380(6) . ? C22 H22 0.9300 . ? C23 N3 1.328(6) . ? C23 C24 1.418(7) . ? C24 N4 1.356(6) . ? C25 C26 1.521(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N5 1.333(6) . ? C26 C27 1.408(7) . ? C27 C28 1.417(7) . ? C27 C39 1.449(6) 2_755 ? C28 N6 1.319(6) . ? C28 C29 1.535(7) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.511(6) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 N7 1.324(6) . ? C31 C32 1.420(7) . ? C32 C33 1.396(7) . ? C32 C35 1.484(6) . ? C33 N8 1.347(7) . ? C33 C34 1.508(7) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.382(7) . ? C35 C40 1.403(7) . ? C36 C37 1.370(7) . ? C36 H36 0.9300 . ? C37 C38 1.392(8) . ? C37 O1 1.416(6) . ? C38 C39 1.431(7) . ? C38 H38 0.9300 . ? C39 C40 1.383(7) . ? C39 C27 1.449(6) 2_755 ? C40 H40 0.9300 . ? C41 O1 1.405(6) . ? C41 C42 1.521(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.370(7) . ? C42 C47 1.386(7) . ? C43 C44 1.426(6) . ? C43 H43 0.9300 . ? C44 C45 1.358(7) . ? C44 H44 0.9300 . ? C45 C46 1.411(7) . ? C45 H45 0.9300 . ? C46 C47 1.417(6) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? N1 Pd1 1.999(4) . ? N2 Pd1 2.022(4) . ? N3 Pd2 2.004(4) . ? N4 Pd2 1.984(4) . ? N5 N6 1.387(6) . ? N5 Pd2 1.996(4) . ? N6 Pd1 2.006(4) . ? N7 N8 1.347(6) . ? N7 Pd2 1.993(4) . ? N8 Pd1 2.004(4) . ? N9 O7 1.211(6) . ? N9 O5 1.219(6) . ? N9 O6 1.225(6) . ? N13 O2 1.209(5) . ? N13 O4 1.213(5) . ? N13 O3 1.219(5) . ? O1W H1X 0.8500 . ? O1W H1Y 0.8498 . ? O2W H2X 0.8500 . ? O2W H2Y 0.8499 . ? O3W H3X 0.8499 . ? O3W H3Y 0.8500 . ? O4W H4X 0.8501 . ? O4W H4Y 0.8500 . ? O5W H5X 0.8499 . ? O5W H5Y 0.8501 . ? O6W H6X 0.8500 . ? O6W H6Y 0.8500 . ? Pd1 Pd2 3.1820(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 118.5(5) . . ? N1 C1 H1 120.8 . . ? C2 C1 H1 120.8 . . ? C3 C2 C1 122.1(5) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C2 C3 C4 120.3(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C12 C4 C3 116.7(4) . . ? C12 C4 C5 117.4(5) . . ? C3 C4 C5 125.8(4) . . ? C6 C5 C4 123.1(5) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C5 C6 C7 120.0(4) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C11 C7 C8 118.0(4) . . ? C11 C7 C6 118.4(5) . . ? C8 C7 C6 123.4(4) . . ? C7 C8 C9 118.6(4) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C10 C9 C8 119.8(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 C9 121.2(4) . . ? N2 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? N2 C11 C7 122.9(5) . . ? N2 C11 C12 116.6(4) . . ? C7 C11 C12 120.5(5) . . ? N1 C12 C4 123.6(5) . . ? N1 C12 C11 115.9(4) . . ? C4 C12 C11 120.5(4) . . ? N4 C13 C14 120.8(5) . . ? N4 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 121.0(4) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 119.1(4) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C24 C16 C15 116.7(4) . . ? C24 C16 C17 117.7(5) . . ? C15 C16 C17 125.5(5) . . ? C18 C17 C16 121.1(5) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 121.6(5) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C18 C19 C23 120.1(5) . . ? C18 C19 C20 124.5(4) . . ? C23 C19 C20 115.4(5) . . ? C21 C20 C19 120.3(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.4(5) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 N3 121.5(5) . . ? C21 C22 H22 119.3 . . ? N3 C22 H22 119.3 . . ? N3 C23 C19 125.0(5) . . ? N3 C23 C24 115.1(4) . . ? C19 C23 C24 119.7(5) . . ? N4 C24 C23 116.5(4) . . ? N4 C24 C16 123.8(4) . . ? C23 C24 C16 119.7(4) . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N5 C26 C27 110.2(4) . . ? N5 C26 C25 121.4(4) . . ? C27 C26 C25 128.4(4) . . ? C26 C27 C28 103.4(4) . . ? C26 C27 C39 128.2(5) . 2_755 ? C28 C27 C39 128.1(5) . 2_755 ? N6 C28 C27 109.9(4) . . ? N6 C28 C29 122.2(4) . . ? C27 C28 C29 127.8(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N7 C31 C32 107.8(4) . . ? N7 C31 C30 123.0(4) . . ? C32 C31 C30 129.2(4) . . ? C33 C32 C31 105.0(4) . . ? C33 C32 C35 129.9(5) . . ? C31 C32 C35 124.9(4) . . ? N8 C33 C32 108.4(4) . . ? N8 C33 C34 122.6(5) . . ? C32 C33 C34 129.0(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 119.6(5) . . ? C36 C35 C32 121.9(5) . . ? C40 C35 C32 118.6(4) . . ? C37 C36 C35 119.9(5) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C36 C37 C38 122.9(5) . . ? C36 C37 O1 115.2(5) . . ? C38 C37 O1 121.9(5) . . ? C37 C38 C39 116.8(5) . . ? C37 C38 H38 121.6 . . ? C39 C38 H38 121.6 . . ? C40 C39 C38 120.3(5) . . ? C40 C39 C27 120.1(4) . 2_755 ? C38 C39 C27 119.6(5) . 2_755 ? C39 C40 C35 120.4(4) . . ? C39 C40 H40 119.8 . . ? C35 C40 H40 119.8 . . ? O1 C41 C42 108.8(4) . . ? O1 C41 H41A 109.9 . . ? C42 C41 H41A 109.9 . . ? O1 C41 H41B 109.9 . . ? C42 C41 H41B 109.9 . . ? H41A C41 H41B 108.3 . . ? C43 C42 C47 120.2(4) . . ? C43 C42 C41 122.4(5) . . ? C47 C42 C41 117.3(4) . . ? C42 C43 C44 120.1(5) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 119.7(5) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 121.3(5) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C45 C46 C47 118.0(5) . . ? C45 C46 H46 121.0 . . ? C47 C46 H46 121.0 . . ? C42 C47 C46 120.6(5) . . ? C42 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C1 N1 C12 118.7(4) . . ? C1 N1 Pd1 128.2(4) . . ? C12 N1 Pd1 113.1(3) . . ? C10 N2 C11 119.1(4) . . ? C10 N2 Pd1 128.4(3) . . ? C11 N2 Pd1 112.5(3) . . ? C23 N3 C22 117.3(4) . . ? C23 N3 Pd2 114.3(3) . . ? C22 N3 Pd2 128.4(3) . . ? C24 N4 C13 118.4(4) . . ? C24 N4 Pd2 113.1(3) . . ? C13 N4 Pd2 128.2(4) . . ? C26 N5 N6 107.7(4) . . ? C26 N5 Pd2 132.6(4) . . ? N6 N5 Pd2 116.0(3) . . ? C28 N6 N5 108.8(4) . . ? C28 N6 Pd1 131.3(3) . . ? N5 N6 Pd1 117.3(3) . . ? C31 N7 N8 110.2(4) . . ? C31 N7 Pd2 130.6(3) . . ? N8 N7 Pd2 117.7(3) . . ? N7 N8 C33 108.6(4) . . ? N7 N8 Pd1 116.7(3) . . ? C33 N8 Pd1 130.9(4) . . ? O7 N9 O5 120.3(4) . . ? O7 N9 O6 119.5(5) . . ? O5 N9 O6 120.1(5) . . ? O2 N13 O4 119.7(4) . . ? O2 N13 O3 120.9(4) . . ? O4 N13 O3 119.2(4) . . ? C41 O1 C37 114.7(4) . . ? H1X O1W H1Y 109.5 . . ? H2X O2W H2Y 109.5 . . ? H3X O3W H3Y 109.5 . . ? H4X O4W H4Y 109.5 . . ? H5X O5W H5Y 109.5 . . ? H6X O6W H6Y 109.5 . . ? N1 Pd1 N8 96.17(17) . . ? N1 Pd1 N6 177.09(17) . . ? N8 Pd1 N6 86.32(16) . . ? N1 Pd1 N2 81.89(17) . . ? N8 Pd1 N2 178.06(17) . . ? N6 Pd1 N2 95.61(17) . . ? N1 Pd1 Pd2 116.98(13) . . ? N8 Pd1 Pd2 62.64(11) . . ? N6 Pd1 Pd2 62.88(12) . . ? N2 Pd1 Pd2 118.33(12) . . ? N4 Pd2 N7 97.03(18) . . ? N4 Pd2 N5 177.35(18) . . ? N7 Pd2 N5 84.94(18) . . ? N4 Pd2 N3 80.87(17) . . ? N7 Pd2 N3 177.21(17) . . ? N5 Pd2 N3 97.11(17) . . ? N4 Pd2 Pd1 115.55(14) . . ? N7 Pd2 Pd1 62.60(12) . . ? N5 Pd2 Pd1 63.80(12) . . ? N3 Pd2 Pd1 116.61(13) . . ? 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 C1 C2 C3 2.7(8) . . . . ? C1 C2 C3 C4 -1.0(9) . . . . ? C2 C3 C4 C12 -0.5(8) . . . . ? C2 C3 C4 C5 177.4(5) . . . . ? C12 C4 C5 C6 -3.3(8) . . . . ? C3 C4 C5 C6 178.8(5) . . . . ? C4 C5 C6 C7 4.3(8) . . . . ? C5 C6 C7 C11 -3.7(8) . . . . ? C5 C6 C7 C8 -179.0(5) . . . . ? C11 C7 C8 C9 5.0(8) . . . . ? C6 C7 C8 C9 -179.7(5) . . . . ? C7 C8 C9 C10 -0.6(8) . . . . ? C8 C9 C10 N2 -4.1(8) . . . . ? C8 C7 C11 N2 -5.1(8) . . . . ? C6 C7 C11 N2 179.4(5) . . . . ? C8 C7 C11 C12 177.8(5) . . . . ? C6 C7 C11 C12 2.2(8) . . . . ? C3 C4 C12 N1 0.3(7) . . . . ? C5 C4 C12 N1 -177.8(4) . . . . ? C3 C4 C12 C11 179.9(5) . . . . ? C5 C4 C12 C11 1.8(7) . . . . ? N2 C11 C12 N1 0.9(7) . . . . ? C7 C11 C12 N1 178.2(5) . . . . ? N2 C11 C12 C4 -178.7(5) . . . . ? C7 C11 C12 C4 -1.4(8) . . . . ? N4 C13 C14 C15 -4.1(8) . . . . ? C13 C14 C15 C16 3.1(8) . . . . ? C14 C15 C16 C24 -1.6(7) . . . . ? C14 C15 C16 C17 -179.2(5) . . . . ? C24 C16 C17 C18 1.3(7) . . . . ? C15 C16 C17 C18 178.9(5) . . . . ? C16 C17 C18 C19 -2.3(8) . . . . ? C17 C18 C19 C23 3.2(7) . . . . ? C17 C18 C19 C20 -179.9(5) . . . . ? C18 C19 C20 C21 -178.7(5) . . . . ? C23 C19 C20 C21 -1.7(7) . . . . ? C19 C20 C21 C22 -0.8(8) . . . . ? C20 C21 C22 N3 1.5(8) . . . . ? C18 C19 C23 N3 -179.0(5) . . . . ? C20 C19 C23 N3 3.8(7) . . . . ? C18 C19 C23 C24 -3.1(7) . . . . ? C20 C19 C23 C24 179.8(4) . . . . ? N3 C23 C24 N4 -1.7(7) . . . . ? C19 C23 C24 N4 -178.0(4) . . . . ? N3 C23 C24 C16 178.4(4) . . . . ? C19 C23 C24 C16 2.1(7) . . . . ? C15 C16 C24 N4 1.1(7) . . . . ? C17 C16 C24 N4 178.9(5) . . . . ? C15 C16 C24 C23 -179.0(4) . . . . ? C17 C16 C24 C23 -1.2(7) . . . . ? N5 C26 C27 C28 0.7(5) . . . . ? C25 C26 C27 C28 -179.3(5) . . . . ? N5 C26 C27 C39 174.8(5) . . . 2_755 ? C25 C26 C27 C39 -5.2(8) . . . 2_755 ? C26 C27 C28 N6 0.0(6) . . . . ? C39 C27 C28 N6 -174.1(5) 2_755 . . . ? C26 C27 C28 C29 178.0(5) . . . . ? C39 C27 C28 C29 3.8(9) 2_755 . . . ? N7 C31 C32 C33 -1.9(5) . . . . ? C30 C31 C32 C33 179.4(5) . . . . ? N7 C31 C32 C35 -177.5(5) . . . . ? C30 C31 C32 C35 3.8(8) . . . . ? C31 C32 C33 N8 1.5(6) . . . . ? C35 C32 C33 N8 176.9(5) . . . . ? C31 C32 C33 C34 -178.6(5) . . . . ? C35 C32 C33 C34 -3.3(9) . . . . ? C33 C32 C35 C36 70.3(7) . . . . ? C31 C32 C35 C36 -115.2(6) . . . . ? C33 C32 C35 C40 -109.7(6) . . . . ? C31 C32 C35 C40 64.8(7) . . . . ? C40 C35 C36 C37 -4.6(7) . . . . ? C32 C35 C36 C37 175.4(5) . . . . ? C35 C36 C37 C38 4.3(8) . . . . ? C35 C36 C37 O1 -174.9(4) . . . . ? C36 C37 C38 C39 -0.8(8) . . . . ? O1 C37 C38 C39 178.3(5) . . . . ? C37 C38 C39 C40 -2.3(8) . . . . ? C37 C38 C39 C27 178.1(5) . . . 2_755 ? C38 C39 C40 C35 1.9(8) . . . . ? C27 C39 C40 C35 -178.5(5) 2_755 . . . ? C36 C35 C40 C39 1.6(8) . . . . ? C32 C35 C40 C39 -178.5(5) . . . . ? O1 C41 C42 C43 -7.6(7) . . . . ? O1 C41 C42 C47 174.5(4) . . . . ? C47 C42 C43 C44 -3.2(8) . . . . ? C41 C42 C43 C44 179.0(5) . . . . ? C42 C43 C44 C45 3.5(7) . . . . ? C43 C44 C45 C46 -2.7(8) . . . . ? C44 C45 C46 C47 1.5(8) . . . . ? C43 C42 C47 C46 2.1(8) . . . . ? C41 C42 C47 C46 180.0(5) . . . . ? C45 C46 C47 C42 -1.2(8) . . . . ? C2 C1 N1 C12 -2.8(8) . . . . ? C2 C1 N1 Pd1 177.7(4) . . . . ? C4 C12 N1 C1 1.4(7) . . . . ? C11 C12 N1 C1 -178.2(5) . . . . ? C4 C12 N1 Pd1 -179.1(4) . . . . ? C11 C12 N1 Pd1 1.4(5) . . . . ? C9 C10 N2 C11 4.2(8) . . . . ? C9 C10 N2 Pd1 -175.4(4) . . . . ? C7 C11 N2 C10 0.5(8) . . . . ? C12 C11 N2 C10 177.7(5) . . . . ? C7 C11 N2 Pd1 -179.8(4) . . . . ? C12 C11 N2 Pd1 -2.6(6) . . . . ? C19 C23 N3 C22 -3.2(7) . . . . ? C24 C23 N3 C22 -179.3(4) . . . . ? C19 C23 N3 Pd2 174.5(4) . . . . ? C24 C23 N3 Pd2 -1.6(6) . . . . ? C21 C22 N3 C23 0.4(7) . . . . ? C21 C22 N3 Pd2 -176.9(4) . . . . ? C23 C24 N4 C13 178.1(5) . . . . ? C16 C24 N4 C13 -2.0(8) . . . . ? C23 C24 N4 Pd2 4.1(6) . . . . ? C16 C24 N4 Pd2 -176.0(4) . . . . ? C14 C13 N4 C24 3.4(8) . . . . ? C14 C13 N4 Pd2 176.4(4) . . . . ? C27 C26 N5 N6 -1.1(5) . . . . ? C25 C26 N5 N6 178.9(4) . . . . ? C27 C26 N5 Pd2 -157.7(4) . . . . ? C25 C26 N5 Pd2 22.3(7) . . . . ? C27 C28 N6 N5 -0.7(6) . . . . ? C29 C28 N6 N5 -178.8(4) . . . . ? C27 C28 N6 Pd1 160.2(3) . . . . ? C29 C28 N6 Pd1 -17.9(8) . . . . ? C26 N5 N6 C28 1.1(6) . . . . ? Pd2 N5 N6 C28 162.2(3) . . . . ? C26 N5 N6 Pd1 -162.8(3) . . . . ? Pd2 N5 N6 Pd1 -1.8(4) . . . . ? C32 C31 N7 N8 1.6(6) . . . . ? C30 C31 N7 N8 -179.6(4) . . . . ? C32 C31 N7 Pd2 166.7(4) . . . . ? C30 C31 N7 Pd2 -14.5(7) . . . . ? C31 N7 N8 C33 -0.6(6) . . . . ? Pd2 N7 N8 C33 -167.9(3) . . . . ? C31 N7 N8 Pd1 160.0(3) . . . . ? Pd2 N7 N8 Pd1 -7.2(5) . . . . ? C32 C33 N8 N7 -0.6(6) . . . . ? C34 C33 N8 N7 179.5(5) . . . . ? C32 C33 N8 Pd1 -157.6(4) . . . . ? C34 C33 N8 Pd1 22.6(7) . . . . ? C42 C41 O1 C37 -166.3(4) . . . . ? C36 C37 O1 C41 156.8(5) . . . . ? C38 C37 O1 C41 -22.4(7) . . . . ? C1 N1 Pd1 N8 -2.7(5) . . . . ? C12 N1 Pd1 N8 177.8(3) . . . . ? C1 N1 Pd1 N2 177.4(5) . . . . ? C12 N1 Pd1 N2 -2.1(3) . . . . ? C1 N1 Pd1 Pd2 59.6(5) . . . . ? C12 N1 Pd1 Pd2 -119.9(3) . . . . ? N7 N8 Pd1 N1 121.8(3) . . . . ? C33 N8 Pd1 N1 -82.8(5) . . . . ? N7 N8 Pd1 N6 -56.7(3) . . . . ? C33 N8 Pd1 N6 98.7(4) . . . . ? N7 N8 Pd1 Pd2 4.5(3) . . . . ? C33 N8 Pd1 Pd2 159.9(5) . . . . ? C28 N6 Pd1 N8 -97.4(5) . . . . ? N5 N6 Pd1 N8 62.1(3) . . . . ? C28 N6 Pd1 N2 82.5(5) . . . . ? N5 N6 Pd1 N2 -117.9(3) . . . . ? C28 N6 Pd1 Pd2 -158.5(5) . . . . ? N5 N6 Pd1 Pd2 1.1(3) . . . . ? C10 N2 Pd1 N1 -177.8(5) . . . . ? C11 N2 Pd1 N1 2.6(4) . . . . ? C10 N2 Pd1 N6 0.7(5) . . . . ? C11 N2 Pd1 N6 -179.0(4) . . . . ? C10 N2 Pd1 Pd2 -61.4(5) . . . . ? C11 N2 Pd1 Pd2 118.9(3) . . . . ? C24 N4 Pd2 N7 174.4(4) . . . . ? C13 N4 Pd2 N7 1.1(5) . . . . ? C24 N4 Pd2 N3 -3.8(4) . . . . ? C13 N4 Pd2 N3 -177.0(5) . . . . ? C24 N4 Pd2 Pd1 111.4(3) . . . . ? C13 N4 Pd2 Pd1 -61.8(5) . . . . ? C31 N7 Pd2 N4 85.2(5) . . . . ? N8 N7 Pd2 N4 -110.6(4) . . . . ? C31 N7 Pd2 N5 -96.6(5) . . . . ? N8 N7 Pd2 N5 67.6(4) . . . . ? C31 N7 Pd2 Pd1 -159.6(5) . . . . ? N8 N7 Pd2 Pd1 4.6(3) . . . . ? C26 N5 Pd2 N7 94.4(5) . . . . ? N6 N5 Pd2 N7 -60.8(3) . . . . ? C26 N5 Pd2 N3 -87.5(5) . . . . ? N6 N5 Pd2 N3 117.3(3) . . . . ? C26 N5 Pd2 Pd1 156.3(5) . . . . ? N6 N5 Pd2 Pd1 1.1(3) . . . . ? C23 N3 Pd2 N4 2.9(4) . . . . ? C22 N3 Pd2 N4 -179.7(5) . . . . ? C23 N3 Pd2 N5 -175.3(4) . . . . ? C22 N3 Pd2 N5 2.0(4) . . . . ? C23 N3 Pd2 Pd1 -111.1(3) . . . . ? C22 N3 Pd2 Pd1 66.2(4) . . . . ? N1 Pd1 Pd2 N4 -1.2(2) . . . . ? N8 Pd1 Pd2 N4 81.48(19) . . . . ? N6 Pd1 Pd2 N4 -177.9(2) . . . . ? N2 Pd1 Pd2 N4 -96.6(2) . . . . ? N1 Pd1 Pd2 N7 -85.7(2) . . . . ? N8 Pd1 Pd2 N7 -3.07(19) . . . . ? N6 Pd1 Pd2 N7 97.5(2) . . . . ? N2 Pd1 Pd2 N7 178.8(2) . . . . ? N1 Pd1 Pd2 N5 176.0(2) . . . . ? N8 Pd1 Pd2 N5 -101.37(19) . . . . ? N6 Pd1 Pd2 N5 -0.77(19) . . . . ? N2 Pd1 Pd2 N5 80.5(2) . . . . ? N1 Pd1 Pd2 N3 91.26(19) . . . . ? N8 Pd1 Pd2 N3 173.92(18) . . . . ? N6 Pd1 Pd2 N3 -85.48(19) . . . . ? N2 Pd1 Pd2 N3 -4.18(19) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.464 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.093 data_yy _database_code_depnum_ccdc_archive 'CCDC 885166' #TrackingRef 'm110704f.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H80 Fe2 N16 Pd4, 4(N O3)' _chemical_formula_sum 'C84 H80 Fe2 N20 O12 Pd4' _chemical_formula_weight 2098.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 Tetragonal _symmetry_space_group_name_H-M 'I4/m ' _symmetry_space_group_name_Hall '-I 4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 26.922(12) _cell_length_b 26.922(12) _cell_length_c 15.467(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11210(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3138' _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 23.75 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 0.935 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.70 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD ' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46675 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 25.07 _reflns_number_total 5177 _reflns_number_gt 3778 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.019 -0.016 -0.078 3221 293 ' ' _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^)+(0.04P)^2^+1.22P] 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 5177 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 C1 C 0.69795(12) 0.12735(13) 0.6544(2) 0.0455(8) Uani 1 1 d . . . H1 H 0.6905 0.1036 0.6126 0.055 Uiso 1 1 calc R . . C2 C 0.74001(13) 0.12199(13) 0.7062(2) 0.0447(9) Uani 1 1 d . . . H2 H 0.7607 0.0947 0.6989 0.054 Uiso 1 1 calc R . . C3 C 0.75087(13) 0.15715(13) 0.7681(2) 0.0464(9) Uani 1 1 d . . . H3 H 0.7789 0.1534 0.8027 0.056 Uiso 1 1 calc R . . C4 C 0.72025(12) 0.19793(13) 0.7791(2) 0.0433(8) Uani 1 1 d . . . H4 H 0.7279 0.2215 0.8210 0.052 Uiso 1 1 calc R . . C5 C 0.67804(12) 0.20390(12) 0.7280(2) 0.0411(8) Uani 1 1 d . . . C6 C 0.64390(12) 0.24779(12) 0.7330(2) 0.0416(8) Uani 1 1 d . . . C7 C 0.65119(12) 0.28650(12) 0.7912(2) 0.0423(8) Uani 1 1 d . . . H7 H 0.6752 0.2838 0.8341 0.051 Uiso 1 1 calc R . . C8 C 0.62243(13) 0.32931(13) 0.7849(2) 0.0459(8) Uani 1 1 d . . . H8 H 0.6277 0.3555 0.8231 0.055 Uiso 1 1 calc R . . C9 C 0.58637(13) 0.33307(12) 0.7226(2) 0.0450(8) Uani 1 1 d . . . H9 H 0.5670 0.3616 0.7189 0.054 Uiso 1 1 calc R . . C10 C 0.57878(12) 0.29381(12) 0.6646(2) 0.0447(8) Uani 1 1 d . . . H10 H 0.5543 0.2963 0.6224 0.054 Uiso 1 1 calc R . . C11 C 0.58435(12) 0.05714(12) 0.6694(2) 0.0446(8) Uani 1 1 d . . . H11A H 0.5598 0.0323 0.6818 0.067 Uiso 1 1 calc R . . H11B H 0.5767 0.0870 0.7006 0.067 Uiso 1 1 calc R . . H11C H 0.6165 0.0452 0.6866 0.067 Uiso 1 1 calc R . . C12 C 0.58458(13) 0.06798(13) 0.5736(2) 0.0473(9) Uani 1 1 d . . . C13 C 0.57859(17) 0.03756(18) 0.5000 0.0436(11) Uani 1 2 d S . . C14 C 0.56469(18) -0.01649(16) 0.5000 0.0474(12) Uani 1 2 d S . . H14A H 0.5675 -0.0293 0.4423 0.057 Uiso 0.50 1 d PR . . H14B H 0.5306 -0.0196 0.5174 0.057 Uiso 0.50 1 d PR . . C15 C 0.4015(2) 0.0496(2) 0.4369(4) 0.0410(16) Uani 0.50 1 d P . . C16 C 0.3513(3) 0.0509(3) 0.4110(5) 0.0485(18) Uani 0.50 1 d P . . H16A H 0.3278 0.0240 0.4143 0.058 Uiso 0.50 1 d PR . . C17 C 0.34061(13) 0.10340(14) 0.3788(2) 0.0495(9) Uani 1 1 d . . . H17A H 0.3098 0.1158 0.3561 0.059 Uiso 0.50 1 d PR . . H17B H 0.3382 0.0745 0.3428 0.059 Uiso 0.50 1 d PR . . C18 C 0.38424(13) 0.13243(13) 0.3920(2) 0.0501(9) Uani 1 1 d . . . H18A H 0.3892 0.1669 0.3790 0.060 Uiso 0.50 1 d PR . . H18B H 0.4162 0.1265 0.3664 0.060 Uiso 0.50 1 d PR . . C19 C 0.4226(3) 0.0962(2) 0.4180(4) 0.0402(15) Uani 0.50 1 d P . . H19 H 0.4565 0.1055 0.4347 0.048 Uiso 0.50 1 d PR . . C20 C 0.3741(3) 0.1694(2) 0.4590(5) 0.0485(17) Uani 0.50 1 d P . . C21 C 0.3235(2) 0.1623(2) 0.4811(4) 0.034(2) Uani 0.50 1 d P . . H21A H 0.3066 0.1808 0.5252 0.041 Uiso 0.50 1 d PR . . C22 C 0.3025(3) 0.1229(2) 0.4345(5) 0.0437(17) Uani 0.50 1 d P . . H22A H 0.2699 0.1090 0.4414 0.052 Uiso 0.50 1 d PR . . C23 C 0.40143(18) 0.21341(19) 0.5000 0.0458(12) Uani 1 2 d S . . H23A H 0.3903 0.2167 0.5587 0.055 Uiso 0.50 1 d PR . . H23B H 0.3921 0.2432 0.4699 0.055 Uiso 0.50 1 d PR . . C24 C 0.45615(18) 0.20969(18) 0.5000 0.0465(12) Uani 1 2 d S . . C25 C 0.48686(12) 0.20661(13) 0.5742(2) 0.0426(8) Uani 1 1 d . . . C26 C 0.47932(12) 0.20636(12) 0.6698(2) 0.0468(9) Uani 1 1 d . . . H26A H 0.4503 0.2255 0.6839 0.070 Uiso 1 1 calc R . . H26B H 0.5078 0.2206 0.6976 0.070 Uiso 1 1 calc R . . H26C H 0.4749 0.1728 0.6894 0.070 Uiso 1 1 calc R . . Fe1 Fe 0.36119(3) 0.10506(3) 0.5000 0.04643(19) Uani 1 2 d S . . N1 N 0.66704(10) 0.16856(11) 0.66553(19) 0.0482(7) Uani 1 1 d . . . N2 N 0.60739(10) 0.25158(10) 0.6697(2) 0.0471(7) Uani 1 1 d . . . N3 N 0.59377(10) 0.11720(10) 0.54493(18) 0.0442(7) Uani 1 1 d . . . N4 N 0.53652(10) 0.19972(10) 0.54682(17) 0.0410(6) Uani 1 1 d . . . N5 N 0.54617(11) 0.61614(11) 0.6754(2) 0.0508(8) Uani 1 1 d . . . O1 O 0.53142(9) 0.65540(9) 0.64168(16) 0.0500(6) Uani 1 1 d . . . O2 O 0.58176(8) 0.59287(8) 0.64480(16) 0.0473(6) Uani 1 1 d . . . O3 O 0.52518(8) 0.60071(8) 0.74210(14) 0.0434(6) Uani 1 1 d . . . Pd1 Pd 0.601445(10) 0.184181(9) 0.605821(17) 0.04081(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0431(18) 0.0461(18) 0.047(2) -0.0083(17) 0.0014(16) -0.0062(16) C2 0.0491(19) 0.0429(18) 0.042(2) 0.0130(16) 0.0116(16) 0.0139(16) C3 0.0422(18) 0.050(2) 0.047(2) 0.0160(17) -0.0101(16) -0.0114(17) C4 0.0448(19) 0.0499(19) 0.0352(19) -0.0073(16) -0.0004(15) -0.0071(16) C5 0.0431(17) 0.0364(16) 0.044(2) 0.0084(15) -0.0109(16) -0.0147(15) C6 0.0455(18) 0.0377(17) 0.042(2) 0.0094(15) -0.0096(16) -0.0165(15) C7 0.0458(18) 0.0466(19) 0.0346(19) 0.0069(15) -0.0075(15) -0.0123(16) C8 0.0474(19) 0.049(2) 0.041(2) -0.0082(16) 0.0077(16) -0.0096(17) C9 0.054(2) 0.0381(17) 0.043(2) 0.0061(15) 0.0137(16) 0.0142(16) C10 0.0434(18) 0.0386(17) 0.052(2) 0.0080(16) -0.0093(16) -0.0066(15) C11 0.0442(18) 0.0462(19) 0.043(2) -0.0125(16) -0.0174(16) 0.0152(15) C12 0.050(2) 0.0452(19) 0.047(2) -0.0086(17) -0.0081(17) 0.0100(17) C13 0.044(3) 0.049(3) 0.037(3) 0.000 0.000 -0.018(2) C14 0.048(3) 0.033(2) 0.061(3) 0.000 0.000 0.017(2) C15 0.047(4) 0.042(4) 0.034(4) -0.007(3) 0.003(3) 0.010(3) C16 0.039(3) 0.046(4) 0.061(5) -0.013(3) 0.020(3) 0.002(3) C17 0.0449(18) 0.055(2) 0.049(2) -0.0050(18) -0.0008(17) 0.0161(18) C18 0.0470(19) 0.0449(19) 0.059(2) 0.0001(18) 0.0086(18) 0.0079(16) C19 0.044(4) 0.043(4) 0.033(4) -0.012(3) -0.006(3) 0.003(3) C20 0.044(4) 0.042(4) 0.060(4) -0.002(3) 0.011(3) 0.003(3) C21 0.042(3) 0.031(2) 0.029(8) 0.005(3) 0.008(3) -0.004(2) C22 0.041(4) 0.041(4) 0.049(5) 0.004(3) -0.002(3) 0.003(3) C23 0.047(3) 0.054(3) 0.037(3) 0.000 0.000 -0.006(2) C24 0.044(3) 0.046(3) 0.049(3) 0.000 0.000 0.015(2) C25 0.0393(17) 0.0469(19) 0.041(2) 0.0104(15) 0.0125(15) 0.0143(16) C26 0.0459(18) 0.0483(19) 0.046(2) 0.0113(17) 0.0187(17) -0.0172(16) Fe1 0.0440(4) 0.0434(4) 0.0519(5) 0.000 0.000 0.0181(3) N1 0.0458(16) 0.0573(17) 0.0414(17) -0.0077(14) -0.0139(14) 0.0061(14) N2 0.0469(16) 0.0482(16) 0.0462(19) -0.0140(14) -0.0062(14) 0.0081(14) N3 0.0422(15) 0.0469(15) 0.0436(16) -0.0105(13) -0.0135(13) 0.0066(13) N4 0.0371(14) 0.0483(16) 0.0376(15) 0.0051(13) 0.0084(12) 0.0067(13) N5 0.0501(17) 0.0497(17) 0.053(2) 0.0221(15) 0.0226(15) 0.0145(14) O1 0.0533(14) 0.0519(14) 0.0449(15) 0.0160(12) 0.0166(11) 0.0148(12) O2 0.0429(12) 0.0469(13) 0.0522(15) 0.0148(12) 0.0134(11) 0.0122(11) O3 0.0511(13) 0.0466(13) 0.0323(13) 0.0156(10) 0.0131(11) 0.0167(11) Pd1 0.04149(15) 0.04110(15) 0.03985(16) -0.00522(12) -0.00371(12) -0.00113(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 C1 C2 1.395(5) . ? C1 N1 1.397(4) . ? C1 H1 0.9300 . ? C2 C3 1.379(5) . ? C2 H2 0.9300 . ? C3 C4 1.384(5) . ? C3 H3 0.9300 . ? C4 C5 1.394(5) . ? C4 H4 0.9300 . ? C5 N1 1.388(4) . ? C5 C6 1.499(5) . ? C6 N2 1.391(4) . ? C6 C7 1.391(5) . ? C7 C8 1.392(5) . ? C7 H7 0.9300 . ? C8 C9 1.371(5) . ? C8 H8 0.9300 . ? C9 C10 1.402(5) . ? C9 H9 0.9300 . ? C10 N2 1.376(4) . ? C10 H10 0.9300 . ? C11 C12 1.510(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.411(5) . ? C12 N3 1.419(5) . ? C13 C12 1.411(5) 11_556 ? C13 C14 1.503(6) . ? C14 C15 1.604(7) 9_656 ? C14 C15 1.604(7) 3_655 ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C15 C16 1.411(10) . ? C15 C19 1.409(9) . ? C15 C14 1.604(7) 9_656 ? C15 C15 1.952(13) 11_556 ? C15 Fe1 2.089(6) . ? C16 C17 1.527(8) . ? C16 Fe1 2.024(7) . ? C16 H16A 0.9602 . ? C16 H17B 1.2809 . ? C17 C18 1.426(5) . ? C17 C22 1.438(8) . ? C17 Fe1 1.955(4) . ? C17 H17A 0.9602 . ? C17 H17B 0.9600 . ? C18 C20 1.463(8) . ? C18 C19 1.477(7) . ? C18 Fe1 1.928(4) . ? C18 H18A 0.9601 . ? C18 H18B 0.9601 . ? C19 Fe1 2.098(7) . ? C19 H18B 1.1542 . ? C19 H19 0.9805 . ? C20 C20 1.268(15) 11_556 ? C20 C21 1.416(9) . ? C20 C23 1.532(8) . ? C20 C21 1.657(9) 11_556 ? C20 Fe1 1.877(7) . ? C21 C21 0.584(14) 11_556 ? C21 C22 1.402(9) . ? C21 C20 1.657(9) 11_556 ? C21 C22 1.774(9) 11_556 ? C21 Fe1 1.868(6) . ? C21 H21A 0.9601 . ? C22 C21 1.774(9) 11_556 ? C22 Fe1 1.937(7) . ? C22 H17A 1.2435 . ? C22 H22A 0.9600 . ? C23 C24 1.477(7) . ? C23 C20 1.532(8) 11_556 ? C23 H23A 0.9600 . ? C23 H23B 0.9603 . ? C24 C25 1.417(5) . ? C24 C25 1.417(5) 11_556 ? C25 N4 1.415(4) . ? C25 C26 1.492(5) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? Fe1 C21 1.868(6) 11_556 ? Fe1 C20 1.877(7) 11_556 ? Fe1 C18 1.928(4) 11_556 ? Fe1 C22 1.937(7) 11_556 ? Fe1 C17 1.955(4) 11_556 ? Fe1 C16 2.024(7) 11_556 ? N1 Pd1 2.037(3) . ? N2 Pd1 2.072(3) . ? N3 N3 1.390(6) 11_556 ? N3 Pd1 2.045(3) . ? N4 N4 1.448(5) 11_556 ? N4 Pd1 2.016(3) . ? N5 O2 1.239(3) . ? N5 O3 1.248(3) . ? N5 O1 1.244(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 119.7(3) . . ? C2 C1 H1 120.2 . . ? N1 C1 H1 120.2 . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 119.3(3) . . ? N1 C5 C6 116.5(3) . . ? C4 C5 C6 124.2(3) . . ? N2 C6 C7 120.0(3) . . ? N2 C6 C5 117.0(3) . . ? C7 C6 C5 122.5(3) . . ? C8 C7 C6 119.8(3) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C9 C8 C7 120.3(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N2 C10 C9 120.3(3) . . ? N2 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 N3 108.1(3) . . ? C13 C12 C11 132.7(3) . . ? N3 C12 C11 119.2(3) . . ? C12 C13 C12 107.5(5) . 11_556 ? C12 C13 C14 126.2(2) . . ? C12 C13 C14 126.2(2) 11_556 . ? C13 C14 C15 113.4(4) . 9_656 ? C13 C14 C15 113.4(4) . 3_655 ? C15 C14 C15 75.0(5) 9_656 3_655 ? C13 C14 H14A 109.1 . . ? C15 C14 H14A 108.8 9_656 . ? C13 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 9_656 . ? C15 C14 H14B 131.7 3_655 . ? H14A C14 H14B 107.8 . . ? C16 C15 C19 107.8(6) . . ? C16 C15 C14 136.9(6) . 9_656 ? C19 C15 C14 113.1(6) . 9_656 ? C16 C15 C15 106.5(4) . 11_556 ? C19 C15 C15 102.0(4) . 11_556 ? C14 C15 C15 52.5(2) 9_656 11_556 ? C16 C15 Fe1 67.5(4) . . ? C19 C15 Fe1 70.7(4) . . ? C14 C15 Fe1 114.0(4) 9_656 . ? C15 C15 Fe1 62.15(19) 11_556 . ? C15 C16 C17 107.2(6) . . ? C15 C16 Fe1 72.4(4) . . ? C17 C16 Fe1 65.1(3) . . ? C15 C16 H16A 126.6 . . ? C17 C16 H16A 126.2 . . ? Fe1 C16 H16A 126.3 . . ? C15 C16 H17B 120.7 . . ? Fe1 C16 H17B 103.8 . . ? H16A C16 H17B 103.7 . . ? C18 C17 C22 107.5(4) . . ? C18 C17 C16 107.8(4) . . ? C22 C17 C16 106.1(4) . . ? C18 C17 Fe1 67.4(2) . . ? C22 C17 Fe1 67.6(3) . . ? C16 C17 Fe1 69.8(3) . . ? C18 C17 H17A 125.0 . . ? C22 C17 H17A 58.5 . . ? C16 C17 H17A 127.1 . . ? Fe1 C17 H17A 126.0 . . ? C18 C17 H17B 125.8 . . ? C22 C17 H17B 126.5 . . ? C16 C17 H17B 56.6 . . ? Fe1 C17 H17B 126.5 . . ? H17A C17 H17B 90.5 . . ? C17 C18 C20 108.7(4) . . ? C17 C18 C19 104.7(4) . . ? C20 C18 C19 112.8(4) . . ? C17 C18 Fe1 69.5(2) . . ? C20 C18 Fe1 65.6(3) . . ? C19 C18 Fe1 74.8(3) . . ? C17 C18 H18A 128.0 . . ? C20 C18 H18A 61.1 . . ? C19 C18 H18A 126.8 . . ? Fe1 C18 H18A 126.6 . . ? C17 C18 H18B 126.0 . . ? C20 C18 H18B 125.0 . . ? C19 C18 H18B 51.4 . . ? Fe1 C18 H18B 125.6 . . ? H18A C18 H18B 87.1 . . ? C15 C19 C18 111.3(6) . . ? C15 C19 Fe1 70.0(4) . . ? C18 C19 Fe1 62.5(3) . . ? C15 C19 H18B 135.4 . . ? Fe1 C19 H18B 102.6 . . ? C15 C19 H19 123.1 . . ? C18 C19 H19 123.8 . . ? Fe1 C19 H19 123.0 . . ? H18B C19 H19 98.3 . . ? C20 C20 C21 76.0(4) 11_556 . ? C20 C20 C18 135.1(3) 11_556 . ? C21 C20 C18 105.0(5) . . ? C20 C20 C23 65.6(3) 11_556 . ? C21 C20 C23 117.8(6) . . ? C18 C20 C23 136.8(5) . . ? C20 C20 C21 56.0(3) 11_556 11_556 ? C18 C20 C21 118.1(5) . 11_556 ? C23 C20 C21 104.7(5) . 11_556 ? C20 C20 Fe1 70.3(2) 11_556 . ? C21 C20 Fe1 67.4(4) . . ? C18 C20 Fe1 69.2(3) . . ? C23 C20 Fe1 131.5(5) . . ? C21 C20 Fe1 63.4(3) 11_556 . ? C20 C20 H18A 161.5 11_556 . ? C21 C20 H18A 121.5 . . ? C23 C20 H18A 106.4 . . ? C21 C20 H18A 141.3 11_556 . ? Fe1 C20 H18A 109.3 . . ? C21 C21 C20 104.0(4) 11_556 . ? C21 C21 C22 121.0(4) 11_556 . ? C20 C21 C22 111.4(6) . . ? C21 C21 C20 56.0(3) 11_556 11_556 ? C20 C21 C20 47.9(6) . 11_556 ? C22 C21 C20 134.9(5) . 11_556 ? C20 C21 C22 124.4(5) . 11_556 ? C22 C21 C22 78.3(6) . 11_556 ? C20 C21 C22 85.4(5) 11_556 11_556 ? C21 C21 Fe1 81.0(2) 11_556 . ? C20 C21 Fe1 68.1(4) . . ? C22 C21 Fe1 71.0(4) . . ? C20 C21 Fe1 64.0(3) 11_556 . ? C22 C21 Fe1 64.2(3) 11_556 . ? C20 C21 H21A 123.8 . . ? C22 C21 H21A 124.6 . . ? C20 C21 H21A 86.1 11_556 . ? C22 C21 H21A 68.8 11_556 . ? Fe1 C21 H21A 125.2 . . ? C21 C22 C17 107.3(6) . . ? C17 C22 C21 115.6(5) . 11_556 ? C21 C22 Fe1 65.8(4) . . ? C17 C22 Fe1 69.0(3) . . ? C21 C22 Fe1 60.2(3) 11_556 . ? C21 C22 H17A 123.7 . . ? C21 C22 H17A 139.4 11_556 . ? Fe1 C22 H17A 110.1 . . ? C21 C22 H22A 127.3 . . ? C17 C22 H22A 125.2 . . ? C21 C22 H22A 116.2 11_556 . ? Fe1 C22 H22A 126.2 . . ? H17A C22 H22A 101.2 . . ? C24 C23 C20 115.3(4) . 11_556 ? C24 C23 C20 115.3(4) . . ? C20 C23 C20 48.9(6) 11_556 . ? C24 C23 H23A 108.5 . . ? C20 C23 H23A 61.9 11_556 . ? C20 C23 H23A 108.2 . . ? C24 C23 H23B 108.5 . . ? C20 C23 H23B 136.1 11_556 . ? C20 C23 H23B 108.7 . . ? H23A C23 H23B 107.5 . . ? C25 C24 C25 108.2(4) . 11_556 ? C25 C24 C23 125.9(2) . . ? C25 C24 C23 125.9(2) 11_556 . ? N4 C25 C24 108.4(3) . . ? N4 C25 C26 115.2(3) . . ? C24 C25 C26 136.3(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C21 Fe1 C21 18.0(4) . 11_556 ? C21 Fe1 C20 52.5(3) . 11_556 ? C21 Fe1 C20 44.4(3) 11_556 11_556 ? C21 Fe1 C20 44.4(3) . . ? C21 Fe1 C20 52.5(3) 11_556 . ? C20 Fe1 C20 39.5(5) 11_556 . ? C21 Fe1 C18 89.7(2) . 11_556 ? C21 Fe1 C18 74.0(2) 11_556 11_556 ? C20 Fe1 C18 45.2(2) 11_556 11_556 ? C20 Fe1 C18 83.1(3) . 11_556 ? C21 Fe1 C18 74.0(2) . . ? C21 Fe1 C18 89.7(2) 11_556 . ? C20 Fe1 C18 83.1(3) 11_556 . ? C20 Fe1 C18 45.2(2) . . ? C18 Fe1 C18 120.0(2) 11_556 . ? C21 Fe1 C22 43.2(3) . . ? C21 Fe1 C22 55.6(3) 11_556 . ? C20 Fe1 C22 95.7(3) 11_556 . ? C20 Fe1 C22 75.2(3) . . ? C18 Fe1 C22 128.4(2) 11_556 . ? C18 Fe1 C22 73.4(2) . . ? C21 Fe1 C22 55.6(3) . 11_556 ? C21 Fe1 C22 43.2(3) 11_556 11_556 ? C20 Fe1 C22 75.2(3) 11_556 11_556 ? C20 Fe1 C22 95.7(3) . 11_556 ? C18 Fe1 C22 73.4(2) 11_556 11_556 ? C18 Fe1 C22 128.4(2) . 11_556 ? C22 Fe1 C22 63.1(5) . 11_556 ? C21 Fe1 C17 90.9(2) . 11_556 ? C21 Fe1 C17 73.4(2) 11_556 11_556 ? C20 Fe1 C17 75.5(3) 11_556 11_556 ? C20 Fe1 C17 113.4(2) . 11_556 ? C18 Fe1 C17 43.07(16) 11_556 11_556 ? C18 Fe1 C17 158.50(16) . 11_556 ? C22 Fe1 C17 106.0(2) . 11_556 ? C22 Fe1 C17 43.4(2) 11_556 11_556 ? C21 Fe1 C17 73.4(2) . . ? C21 Fe1 C17 90.9(2) 11_556 . ? C20 Fe1 C17 113.4(2) 11_556 . ? C20 Fe1 C17 75.5(3) . . ? C18 Fe1 C17 158.50(16) 11_556 . ? C18 Fe1 C17 43.07(16) . . ? C22 Fe1 C17 43.4(3) . . ? C22 Fe1 C17 106.0(2) 11_556 . ? C17 Fe1 C17 147.0(2) 11_556 . ? C21 Fe1 C16 129.0(3) . 11_556 ? C21 Fe1 C16 114.6(3) 11_556 11_556 ? C20 Fe1 C16 117.4(3) 11_556 11_556 ? C20 Fe1 C16 156.9(3) . 11_556 ? C18 Fe1 C16 74.3(2) 11_556 11_556 ? C18 Fe1 C16 155.1(2) . 11_556 ? C22 Fe1 C16 115.3(3) . 11_556 ? C22 Fe1 C16 73.4(3) 11_556 11_556 ? C17 Fe1 C16 45.1(2) 11_556 11_556 ? C17 Fe1 C16 126.8(2) . 11_556 ? C21 Fe1 C16 114.6(3) . . ? C21 Fe1 C16 129.0(3) 11_556 . ? C20 Fe1 C16 156.9(3) 11_556 . ? C20 Fe1 C16 117.4(3) . . ? C18 Fe1 C16 155.1(2) 11_556 . ? C18 Fe1 C16 74.3(2) . . ? C22 Fe1 C16 73.4(3) . . ? C22 Fe1 C16 115.3(3) 11_556 . ? C17 Fe1 C16 126.8(2) 11_556 . ? C17 Fe1 C16 45.1(2) . . ? C16 Fe1 C16 85.7(4) 11_556 . ? C5 N1 C1 120.2(3) . . ? C5 N1 Pd1 111.0(2) . . ? C1 N1 Pd1 128.6(2) . . ? C10 N2 C6 119.8(3) . . ? C10 N2 Pd1 130.8(2) . . ? C6 N2 Pd1 109.0(2) . . ? N3 N3 C12 108.20(19) 11_556 . ? N3 N3 Pd1 117.42(8) 11_556 . ? C12 N3 Pd1 134.2(2) . . ? C25 N4 N4 107.45(19) . 11_556 ? C25 N4 Pd1 135.3(2) . . ? N4 N4 Pd1 116.92(7) 11_556 . ? O2 N5 O3 119.9(3) . . ? O2 N5 O1 121.1(3) . . ? O3 N5 O1 119.0(3) . . ? N4 Pd1 N1 179.93(14) . . ? N4 Pd1 N3 83.51(11) . . ? N1 Pd1 N3 96.57(11) . . ? N4 Pd1 N2 95.80(11) . . ? N1 Pd1 N2 84.12(11) . . ? N3 Pd1 N2 178.30(12) . . ? 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 C1 C2 C3 0.2(5) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C3 C4 C5 N1 -0.2(5) . . . . ? C3 C4 C5 C6 -177.5(3) . . . . ? N1 C5 C6 N2 -6.0(4) . . . . ? C4 C5 C6 N2 171.3(3) . . . . ? N1 C5 C6 C7 -178.5(3) . . . . ? C4 C5 C6 C7 -1.1(5) . . . . ? N2 C6 C7 C8 -1.1(5) . . . . ? C5 C6 C7 C8 171.2(3) . . . . ? C6 C7 C8 C9 1.2(5) . . . . ? C7 C8 C9 C10 -0.6(5) . . . . ? C8 C9 C10 N2 -0.1(5) . . . . ? N3 C12 C13 C12 0.6(5) . . . 11_556 ? C11 C12 C13 C12 -177.4(2) . . . 11_556 ? N3 C12 C13 C14 -175.4(4) . . . . ? C11 C12 C13 C14 6.6(8) . . . . ? C12 C13 C14 C15 -50.9(6) . . . 9_656 ? C12 C13 C14 C15 133.9(5) 11_556 . . 9_656 ? C12 C13 C14 C15 -133.9(5) . . . 3_655 ? C12 C13 C14 C15 50.9(6) 11_556 . . 3_655 ? C19 C15 C16 C17 -3.5(7) . . . . ? C14 C15 C16 C17 157.6(6) 9_656 . . . ? C15 C15 C16 C17 105.3(4) 11_556 . . . ? Fe1 C15 C16 C17 55.9(4) . . . . ? C19 C15 C16 Fe1 -59.4(5) . . . . ? C14 C15 C16 Fe1 101.7(7) 9_656 . . . ? C15 C15 C16 Fe1 49.4(2) 11_556 . . . ? C15 C16 C17 C18 -3.7(6) . . . . ? Fe1 C16 C17 C18 56.8(3) . . . . ? C15 C16 C17 C22 -118.7(6) . . . . ? Fe1 C16 C17 C22 -58.2(4) . . . . ? C15 C16 C17 Fe1 -60.5(5) . . . . ? C22 C17 C18 C20 2.1(6) . . . . ? C16 C17 C18 C20 -111.9(5) . . . . ? Fe1 C17 C18 C20 -53.6(4) . . . . ? C22 C17 C18 C19 122.9(5) . . . . ? C16 C17 C18 C19 8.9(5) . . . . ? Fe1 C17 C18 C19 67.2(3) . . . . ? C22 C17 C18 Fe1 55.7(4) . . . . ? C16 C17 C18 Fe1 -58.3(3) . . . . ? C16 C15 C19 C18 9.5(7) . . . . ? C14 C15 C19 C18 -156.6(4) 9_656 . . . ? C15 C15 C19 C18 -102.5(4) 11_556 . . . ? Fe1 C15 C19 C18 -47.9(4) . . . . ? C16 C15 C19 Fe1 57.4(5) . . . . ? C14 C15 C19 Fe1 -108.7(4) 9_656 . . . ? C15 C15 C19 Fe1 -54.52(16) 11_556 . . . ? C17 C18 C19 C15 -11.6(6) . . . . ? C20 C18 C19 C15 106.5(6) . . . . ? Fe1 C18 C19 C15 51.9(5) . . . . ? C17 C18 C19 Fe1 -63.5(3) . . . . ? C20 C18 C19 Fe1 54.6(4) . . . . ? C17 C18 C20 C20 82.8(4) . . . 11_556 ? C19 C18 C20 C20 -32.8(6) . . . 11_556 ? Fe1 C18 C20 C20 26.9(3) . . . 11_556 ? C17 C18 C20 C21 -2.3(6) . . . . ? C19 C18 C20 C21 -117.9(6) . . . . ? Fe1 C18 C20 C21 -58.2(4) . . . . ? C17 C18 C20 C23 -174.9(7) . . . . ? C19 C18 C20 C23 69.5(9) . . . . ? Fe1 C18 C20 C23 129.2(8) . . . . ? C17 C18 C20 C21 14.0(7) . . . 11_556 ? C19 C18 C20 C21 -101.6(6) . . . 11_556 ? Fe1 C18 C20 C21 -41.9(4) . . . 11_556 ? C17 C18 C20 Fe1 55.9(3) . . . . ? C19 C18 C20 Fe1 -59.7(4) . . . . ? C20 C20 C21 C21 0.000(1) 11_556 . . 11_556 ? C18 C20 C21 C21 133.6(4) . . . 11_556 ? C23 C20 C21 C21 -52.2(6) . . . 11_556 ? Fe1 C20 C21 C21 74.13(19) . . . 11_556 ? C20 C20 C21 C22 -131.9(5) 11_556 . . . ? C18 C20 C21 C22 1.7(7) . . . . ? C23 C20 C21 C22 176.0(5) . . . . ? C21 C20 C21 C22 -131.9(5) 11_556 . . . ? Fe1 C20 C21 C22 -57.7(5) . . . . ? C18 C20 C21 C20 133.6(4) . . . 11_556 ? C23 C20 C21 C20 -52.2(6) . . . 11_556 ? C21 C20 C21 C20 0.000(2) 11_556 . . 11_556 ? Fe1 C20 C21 C20 74.13(19) . . . 11_556 ? C20 C20 C21 C22 -41.6(5) 11_556 . . 11_556 ? C18 C20 C21 C22 92.0(7) . . . 11_556 ? C23 C20 C21 C22 -93.7(7) . . . 11_556 ? C21 C20 C21 C22 -41.6(5) 11_556 . . 11_556 ? Fe1 C20 C21 C22 32.6(5) . . . 11_556 ? C20 C20 C21 Fe1 -74.13(19) 11_556 . . . ? C18 C20 C21 Fe1 59.4(4) . . . . ? C23 C20 C21 Fe1 -126.3(6) . . . . ? C21 C20 C21 Fe1 -74.13(19) 11_556 . . . ? C21 C21 C22 C17 -123.0(4) 11_556 . . . ? C20 C21 C22 C17 -0.4(8) . . . . ? C20 C21 C22 C17 -51.8(10) 11_556 . . . ? C22 C21 C22 C17 -123.0(4) 11_556 . . . ? Fe1 C21 C22 C17 -56.5(4) . . . . ? C20 C21 C22 C21 122.6(6) . . . 11_556 ? C20 C21 C22 C21 71.2(7) 11_556 . . 11_556 ? C22 C21 C22 C21 0.000(4) 11_556 . . 11_556 ? Fe1 C21 C22 C21 66.5(3) . . . 11_556 ? C21 C21 C22 Fe1 -66.5(3) 11_556 . . . ? C20 C21 C22 Fe1 56.1(5) . . . . ? C20 C21 C22 Fe1 4.8(7) 11_556 . . . ? C22 C21 C22 Fe1 -66.5(3) 11_556 . . . ? C18 C17 C22 C21 -1.0(6) . . . . ? C16 C17 C22 C21 114.1(6) . . . . ? Fe1 C17 C22 C21 54.6(4) . . . . ? C16 C17 C22 C21 98.9(6) . . . 11_556 ? Fe1 C17 C22 C21 39.4(4) . . . 11_556 ? C18 C17 C22 Fe1 -55.6(3) . . . . ? C16 C17 C22 Fe1 59.6(4) . . . . ? C20 C20 C23 C24 102.4(3) 11_556 . . . ? C21 C20 C23 C24 159.7(5) . . . . ? C18 C20 C23 C24 -28.4(9) . . . . ? C21 C20 C23 C24 143.5(4) 11_556 . . . ? Fe1 C20 C23 C24 76.2(6) . . . . ? C21 C20 C23 C20 57.3(6) . . . 11_556 ? C18 C20 C23 C20 -130.7(7) . . . 11_556 ? C21 C20 C23 C20 41.1(5) 11_556 . . 11_556 ? Fe1 C20 C23 C20 -26.2(6) . . . 11_556 ? C20 C23 C24 C25 -61.4(6) 11_556 . . . ? C20 C23 C24 C25 -115.9(5) . . . . ? C20 C23 C24 C25 115.9(5) 11_556 . . 11_556 ? C20 C23 C24 C25 61.4(6) . . . 11_556 ? C25 C24 C25 N4 -2.2(5) 11_556 . . . ? C23 C24 C25 N4 175.6(4) . . . . ? C25 C24 C25 C26 -178.5(2) 11_556 . . . ? C23 C24 C25 C26 -0.8(8) . . . . ? C20 C21 Fe1 C21 109.1(4) . . . 11_556 ? C22 C21 Fe1 C21 -127.3(4) . . . 11_556 ? C20 C21 Fe1 C21 56.5(3) 11_556 . . 11_556 ? C22 C21 Fe1 C21 -41.3(3) 11_556 . . 11_556 ? C21 C21 Fe1 C20 -56.5(3) 11_556 . . 11_556 ? C20 C21 Fe1 C20 52.6(6) . . . 11_556 ? C22 C21 Fe1 C20 176.2(6) . . . 11_556 ? C22 C21 Fe1 C20 -97.8(4) 11_556 . . 11_556 ? C21 C21 Fe1 C20 -109.1(4) 11_556 . . . ? C22 C21 Fe1 C20 123.7(6) . . . . ? C20 C21 Fe1 C20 -52.6(6) 11_556 . . . ? C22 C21 Fe1 C20 -150.4(5) 11_556 . . . ? C21 C21 Fe1 C18 -28.62(12) 11_556 . . 11_556 ? C20 C21 Fe1 C18 80.5(4) . . . 11_556 ? C22 C21 Fe1 C18 -155.9(4) . . . 11_556 ? C20 C21 Fe1 C18 27.9(3) 11_556 . . 11_556 ? C22 C21 Fe1 C18 -70.0(3) 11_556 . . 11_556 ? C21 C21 Fe1 C18 -150.11(13) 11_556 . . . ? C20 C21 Fe1 C18 -41.0(4) . . . . ? C22 C21 Fe1 C18 82.6(4) . . . . ? C20 C21 Fe1 C18 -93.6(3) 11_556 . . . ? C22 C21 Fe1 C18 168.5(3) 11_556 . . . ? C21 C21 Fe1 C22 127.3(4) 11_556 . . . ? C20 C21 Fe1 C22 -123.7(6) . . . . ? C20 C21 Fe1 C22 -176.2(6) 11_556 . . . ? C22 C21 Fe1 C22 85.9(6) 11_556 . . . ? C21 C21 Fe1 C22 41.3(3) 11_556 . . 11_556 ? C20 C21 Fe1 C22 150.4(5) . . . 11_556 ? C22 C21 Fe1 C22 -85.9(6) . . . 11_556 ? C20 C21 Fe1 C22 97.8(4) 11_556 . . 11_556 ? C21 C21 Fe1 C17 14.44(12) 11_556 . . 11_556 ? C20 C21 Fe1 C17 123.5(4) . . . 11_556 ? C22 C21 Fe1 C17 -112.8(4) . . . 11_556 ? C20 C21 Fe1 C17 70.9(3) 11_556 . . 11_556 ? C22 C21 Fe1 C17 -26.9(3) 11_556 . . 11_556 ? C21 C21 Fe1 C17 164.93(12) 11_556 . . . ? C20 C21 Fe1 C17 -86.0(4) . . . . ? C22 C21 Fe1 C17 37.7(4) . . . . ? C20 C21 Fe1 C17 -138.6(4) 11_556 . . . ? C22 C21 Fe1 C17 123.6(3) 11_556 . . . ? C21 C21 Fe1 C16 40.7(3) 11_556 . . 11_556 ? C20 C21 Fe1 C16 149.8(4) . . . 11_556 ? C22 C21 Fe1 C16 -86.6(5) . . . 11_556 ? C20 C21 Fe1 C16 97.2(4) 11_556 . . 11_556 ? C22 C21 Fe1 C16 -0.7(5) 11_556 . . 11_556 ? C21 C21 Fe1 C16 146.1(2) 11_556 . . . ? C20 C21 Fe1 C16 -104.8(4) . . . . ? C22 C21 Fe1 C16 18.9(5) . . . . ? C20 C21 Fe1 C16 -157.4(4) 11_556 . . . ? C22 C21 Fe1 C16 104.8(4) 11_556 . . . ? C20 C20 Fe1 C21 82.6(4) 11_556 . . . ? C18 C20 Fe1 C21 -117.2(5) . . . . ? C23 C20 Fe1 C21 107.9(7) . . . . ? C21 C20 Fe1 C21 21.6(5) 11_556 . . . ? C20 C20 Fe1 C21 61.0(3) 11_556 . . 11_556 ? C21 C20 Fe1 C21 -21.6(5) . . . 11_556 ? C18 C20 Fe1 C21 -138.8(5) . . . 11_556 ? C23 C20 Fe1 C21 86.3(6) . . . 11_556 ? C21 C20 Fe1 C20 -82.6(4) . . . 11_556 ? C18 C20 Fe1 C20 160.2(2) . . . 11_556 ? C23 C20 Fe1 C20 25.3(6) . . . 11_556 ? C21 C20 Fe1 C20 -61.0(3) 11_556 . . 11_556 ? C20 C20 Fe1 C18 -14.02(15) 11_556 . . 11_556 ? C21 C20 Fe1 C18 -96.6(4) . . . 11_556 ? C18 C20 Fe1 C18 146.2(4) . . . 11_556 ? C23 C20 Fe1 C18 11.2(6) . . . 11_556 ? C21 C20 Fe1 C18 -75.1(3) 11_556 . . 11_556 ? C20 C20 Fe1 C18 -160.2(2) 11_556 . . . ? C21 C20 Fe1 C18 117.2(5) . . . . ? C23 C20 Fe1 C18 -134.9(7) . . . . ? C21 C20 Fe1 C18 138.8(5) 11_556 . . . ? C20 C20 Fe1 C22 118.7(2) 11_556 . . . ? C21 C20 Fe1 C22 36.1(4) . . . . ? C18 C20 Fe1 C22 -81.1(4) . . . . ? C23 C20 Fe1 C22 144.0(6) . . . . ? C21 C20 Fe1 C22 57.7(4) 11_556 . . . ? C20 C20 Fe1 C22 58.5(2) 11_556 . . 11_556 ? C21 C20 Fe1 C22 -24.2(5) . . . 11_556 ? C18 C20 Fe1 C22 -141.4(3) . . . 11_556 ? C23 C20 Fe1 C22 83.7(6) . . . 11_556 ? C21 C20 Fe1 C22 -2.6(4) 11_556 . . 11_556 ? C20 C20 Fe1 C17 17.33(12) 11_556 . . 11_556 ? C21 C20 Fe1 C17 -65.3(4) . . . 11_556 ? C18 C20 Fe1 C17 177.5(2) . . . 11_556 ? C23 C20 Fe1 C17 42.6(6) . . . 11_556 ? C21 C20 Fe1 C17 -43.7(4) 11_556 . . 11_556 ? C20 C20 Fe1 C17 163.60(11) 11_556 . . . ? C21 C20 Fe1 C17 81.0(4) . . . . ? C18 C20 Fe1 C17 -36.2(3) . . . . ? C23 C20 Fe1 C17 -171.1(6) . . . . ? C21 C20 Fe1 C17 102.6(3) 11_556 . . . ? C20 C20 Fe1 C16 -1.8(6) 11_556 . . 11_556 ? C21 C20 Fe1 C16 -84.4(8) . . . 11_556 ? C18 C20 Fe1 C16 158.4(6) . . . 11_556 ? C23 C20 Fe1 C16 23.5(11) . . . 11_556 ? C21 C20 Fe1 C16 -62.8(8) 11_556 . . 11_556 ? C20 C20 Fe1 C16 -179.2(3) 11_556 . . . ? C21 C20 Fe1 C16 98.2(4) . . . . ? C18 C20 Fe1 C16 -19.0(4) . . . . ? C23 C20 Fe1 C16 -154.0(5) . . . . ? C21 C20 Fe1 C16 119.7(4) 11_556 . . . ? C17 C18 Fe1 C21 -82.7(3) . . . . ? C20 C18 Fe1 C21 40.4(4) . . . . ? C19 C18 Fe1 C21 164.8(4) . . . . ? C17 C18 Fe1 C21 -91.6(3) . . . 11_556 ? C20 C18 Fe1 C21 31.5(4) . . . 11_556 ? C19 C18 Fe1 C21 156.0(3) . . . 11_556 ? C17 C18 Fe1 C20 -135.6(3) . . . 11_556 ? C20 C18 Fe1 C20 -12.5(2) . . . 11_556 ? C19 C18 Fe1 C20 111.9(4) . . . 11_556 ? C17 C18 Fe1 C20 -123.1(4) . . . . ? C19 C18 Fe1 C20 124.4(4) . . . . ? C17 C18 Fe1 C18 -162.80(17) . . . 11_556 ? C20 C18 Fe1 C18 -39.7(4) . . . 11_556 ? C19 C18 Fe1 C18 84.7(3) . . . 11_556 ? C17 C18 Fe1 C22 -37.6(3) . . . . ? C20 C18 Fe1 C22 85.5(4) . . . . ? C19 C18 Fe1 C22 -150.1(4) . . . . ? C17 C18 Fe1 C22 -70.6(3) . . . 11_556 ? C20 C18 Fe1 C22 52.4(4) . . . 11_556 ? C19 C18 Fe1 C22 176.9(4) . . . 11_556 ? C17 C18 Fe1 C17 -129.3(5) . . . 11_556 ? C20 C18 Fe1 C17 -6.3(6) . . . 11_556 ? C19 C18 Fe1 C17 118.2(5) . . . 11_556 ? C20 C18 Fe1 C17 123.1(4) . . . . ? C19 C18 Fe1 C17 -112.5(3) . . . . ? C17 C18 Fe1 C16 77.0(6) . . . 11_556 ? C20 C18 Fe1 C16 -159.9(6) . . . 11_556 ? C17 C18 Fe1 C16 39.4(3) . . . . ? C20 C18 Fe1 C16 162.5(4) . . . . ? C19 C18 Fe1 C16 -73.1(4) . . . . ? C17 C22 Fe1 C21 121.4(5) . . . . ? C21 C22 Fe1 C21 -17.3(4) 11_556 . . . ? C21 C22 Fe1 C21 17.3(4) . . . 11_556 ? C17 C22 Fe1 C21 138.8(4) . . . 11_556 ? C21 C22 Fe1 C20 -3.0(4) . . . 11_556 ? C17 C22 Fe1 C20 118.4(4) . . . 11_556 ? C21 C22 Fe1 C20 -20.3(4) 11_556 . . 11_556 ? C21 C22 Fe1 C20 -37.1(4) . . . . ? C17 C22 Fe1 C20 84.4(4) . . . . ? C21 C22 Fe1 C20 -54.4(3) 11_556 . . . ? C21 C22 Fe1 C18 31.4(5) . . . 11_556 ? C17 C22 Fe1 C18 152.9(3) . . . 11_556 ? C21 C22 Fe1 C18 14.1(4) 11_556 . . 11_556 ? C21 C22 Fe1 C18 -84.1(4) . . . . ? C17 C22 Fe1 C18 37.4(3) . . . . ? C21 C22 Fe1 C18 -101.4(3) 11_556 . . . ? C21 C22 Fe1 C22 67.3(4) . . . 11_556 ? C17 C22 Fe1 C22 -171.26(19) . . . 11_556 ? C21 C22 Fe1 C22 50.0(3) 11_556 . . 11_556 ? C21 C22 Fe1 C17 73.5(4) . . . 11_556 ? C17 C22 Fe1 C17 -165.0(3) . . . 11_556 ? C21 C22 Fe1 C17 56.2(3) 11_556 . . 11_556 ? C21 C22 Fe1 C17 -121.4(5) . . . . ? C21 C22 Fe1 C17 -138.8(4) 11_556 . . . ? C21 C22 Fe1 C16 120.9(4) . . . 11_556 ? C17 C22 Fe1 C16 -117.6(4) . . . 11_556 ? C21 C22 Fe1 C16 103.6(4) 11_556 . . 11_556 ? C21 C22 Fe1 C16 -162.1(5) . . . . ? C17 C22 Fe1 C16 -40.7(3) . . . . ? C21 C22 Fe1 C16 -179.5(4) 11_556 . . . ? C18 C17 Fe1 C21 84.1(3) . . . . ? C22 C17 Fe1 C21 -37.5(3) . . . . ? C16 C17 Fe1 C21 -155.6(4) . . . . ? C18 C17 Fe1 C21 88.7(3) . . . 11_556 ? C22 C17 Fe1 C21 -32.9(4) . . . 11_556 ? C16 C17 Fe1 C21 -151.0(3) . . . 11_556 ? C18 C17 Fe1 C20 49.2(3) . . . 11_556 ? C22 C17 Fe1 C20 -72.4(4) . . . 11_556 ? C16 C17 Fe1 C20 169.5(4) . . . 11_556 ? C18 C17 Fe1 C20 37.9(3) . . . . ? C22 C17 Fe1 C20 -83.7(4) . . . . ? C16 C17 Fe1 C20 158.3(4) . . . . ? C18 C17 Fe1 C18 44.3(4) . . . 11_556 ? C22 C17 Fe1 C18 -77.3(5) . . . 11_556 ? C16 C17 Fe1 C18 164.7(4) . . . 11_556 ? C22 C17 Fe1 C18 -121.6(4) . . . . ? C16 C17 Fe1 C18 120.4(4) . . . . ? C18 C17 Fe1 C22 121.6(4) . . . . ? C16 C17 Fe1 C22 -118.0(5) . . . . ? C18 C17 Fe1 C22 129.7(3) . . . 11_556 ? C22 C17 Fe1 C22 8.10(19) . . . 11_556 ? C16 C17 Fe1 C22 -109.9(4) . . . 11_556 ? C18 C17 Fe1 C17 148.7(3) . . . 11_556 ? C22 C17 Fe1 C17 27.1(6) . . . 11_556 ? C16 C17 Fe1 C17 -90.9(4) . . . 11_556 ? C18 C17 Fe1 C16 -149.2(3) . . . 11_556 ? C22 C17 Fe1 C16 89.2(4) . . . 11_556 ? C16 C17 Fe1 C16 -28.9(3) . . . 11_556 ? C18 C17 Fe1 C16 -120.4(4) . . . . ? C22 C17 Fe1 C16 118.0(5) . . . . ? C15 C16 Fe1 C21 145.2(4) . . . . ? C17 C16 Fe1 C21 25.9(4) . . . . ? C15 C16 Fe1 C21 158.0(4) . . . 11_556 ? C17 C16 Fe1 C21 38.7(4) . . . 11_556 ? C15 C16 Fe1 C20 94.2(8) . . . 11_556 ? C17 C16 Fe1 C20 -25.1(8) . . . 11_556 ? C15 C16 Fe1 C20 95.5(5) . . . . ? C17 C16 Fe1 C20 -23.8(4) . . . . ? C15 C16 Fe1 C18 -47.4(7) . . . 11_556 ? C17 C16 Fe1 C18 -166.7(4) . . . 11_556 ? C15 C16 Fe1 C18 81.6(4) . . . . ? C17 C16 Fe1 C18 -37.7(2) . . . . ? C15 C16 Fe1 C22 158.5(5) . . . . ? C17 C16 Fe1 C22 39.2(3) . . . . ? C15 C16 Fe1 C22 -153.0(4) . . . 11_556 ? C17 C16 Fe1 C22 87.7(4) . . . 11_556 ? C15 C16 Fe1 C17 -103.6(4) . . . 11_556 ? C17 C16 Fe1 C17 137.1(3) . . . 11_556 ? C15 C16 Fe1 C17 119.3(5) . . . . ? C15 C16 Fe1 C16 -83.5(4) . . . 11_556 ? C17 C16 Fe1 C16 157.18(18) . . . 11_556 ? C4 C5 N1 C1 0.2(5) . . . . ? C6 C5 N1 C1 177.7(3) . . . . ? C4 C5 N1 Pd1 176.5(2) . . . . ? C6 C5 N1 Pd1 -6.0(4) . . . . ? C2 C1 N1 C5 -0.2(5) . . . . ? C2 C1 N1 Pd1 -175.7(2) . . . . ? C9 C10 N2 C6 0.2(5) . . . . ? C9 C10 N2 Pd1 171.9(3) . . . . ? C7 C6 N2 C10 0.4(5) . . . . ? C5 C6 N2 C10 -172.3(3) . . . . ? C7 C6 N2 Pd1 -173.0(3) . . . . ? C5 C6 N2 Pd1 14.4(3) . . . . ? C13 C12 N3 N3 -0.4(3) . . . 11_556 ? C11 C12 N3 N3 177.9(2) . . . 11_556 ? C13 C12 N3 Pd1 174.6(3) . . . . ? C11 C12 N3 Pd1 -7.1(5) . . . . ? C24 C25 N4 N4 1.3(3) . . . 11_556 ? C26 C25 N4 N4 178.5(2) . . . 11_556 ? C24 C25 N4 Pd1 -171.6(3) . . . . ? C26 C25 N4 Pd1 5.6(5) . . . . ? C25 N4 Pd1 N3 110.0(3) . . . . ? N4 N4 Pd1 N3 -62.48(9) 11_556 . . . ? C25 N4 Pd1 N2 -68.5(3) . . . . ? N4 N4 Pd1 N2 119.08(9) 11_556 . . . ? C5 N1 Pd1 N3 -167.6(2) . . . . ? C1 N1 Pd1 N3 8.2(3) . . . . ? C5 N1 Pd1 N2 10.8(2) . . . . ? C1 N1 Pd1 N2 -173.3(3) . . . . ? N3 N3 Pd1 N4 62.98(8) 11_556 . . . ? C12 N3 Pd1 N4 -111.7(3) . . . . ? N3 N3 Pd1 N1 -117.03(10) 11_556 . . . ? C12 N3 Pd1 N1 68.3(3) . . . . ? C10 N2 Pd1 N4 -6.1(3) . . . . ? C6 N2 Pd1 N4 166.3(2) . . . . ? C10 N2 Pd1 N1 173.9(3) . . . . ? C6 N2 Pd1 N1 -13.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.236 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.056