# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'M. Concepcion Gimeno' 'Javier E. Aguado' 'Olga Crespo' 'P. Jones' 'Antonio Laguna' 'M. Dolores Villacampa' _publ_contact_author_name 'M. Concepcion Gimeno' _publ_contact_author_email GIMENO@UNIZAR.ES _publ_section_title ; Coordination Properties of the 1,1'-Bis[((6-methyl)-2-pyridyl) amido-ferrocene Ligand towards Group 11 and Palladium Complexes ; # Attachment 'complex1.CIF' data_magnum _database_code_depnum_ccdc_archive 'CCDC 760667' #TrackingRef 'complex1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H52 Au2 F6 Fe N4 O8 P2 S2' _chemical_formula_weight 1670.92 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 9.494(3) _cell_length_b 11.430(4) _cell_length_c 16.213(6) _cell_angle_alpha 100.608(12) _cell_angle_beta 102.036(12) _cell_angle_gamma 110.857(12) _cell_volume 1542.4(10) _cell_formula_units_Z 1 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 4486 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 5.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.477 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method '/w-scans & /f-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28783 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7642 _reflns_number_gt 6126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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. The triflate anion is disordered over two positions with occupation factors 0.54, 0.46. The residual electron density can be attributed to the broad and irregular reflection profiles associated with a fibrous crystal. ; _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^)+(0.0790P)^2^] 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 'N-H free, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7642 _refine_ls_number_parameters 472 _refine_ls_number_restraints 579 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1267 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.005 _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 Au Au 0.26288(3) 0.26396(2) 0.287822(15) 0.01781(9) Uani 1 1 d . . . Fe Fe 1.0000 0.5000 0.5000 0.0233(3) Uani 1 2 d S . . P P 0.23208(19) 0.34902(16) 0.17523(10) 0.0181(3) Uani 1 1 d . . . O1 O 0.6494(6) 0.4855(5) 0.5732(3) 0.0340(12) Uani 1 1 d U . . C1 C 0.7987(8) 0.5293(7) 0.4737(4) 0.0259(14) Uani 1 1 d DU . . C2 C 0.8375(8) 0.4966(7) 0.3947(5) 0.0295(15) Uani 1 1 d DU . . H2 H 0.7740 0.4236 0.3449 0.035 Uiso 1 1 calc R . . C3 C 0.9873(8) 0.5925(8) 0.4040(5) 0.0361(17) Uani 1 1 d DU . . H3 H 1.0422 0.5952 0.3612 0.043 Uiso 1 1 calc R . . C4 C 1.0430(9) 0.6847(7) 0.4883(5) 0.0364(17) Uani 1 1 d DU . . H4 H 1.1406 0.7593 0.5115 0.044 Uiso 1 1 calc R . . C5 C 0.9261(8) 0.6447(7) 0.5312(5) 0.0322(15) Uani 1 1 d DU . . H5 H 0.9320 0.6878 0.5887 0.039 Uiso 1 1 calc R . . C6 C 0.6641(8) 0.4515(7) 0.5008(5) 0.0266(14) Uani 1 1 d U . . N2 N 0.5545(6) 0.3376(6) 0.4385(4) 0.0247(12) Uani 1 1 d DU . . H02 H 0.571(9) 0.309(7) 0.389(3) 0.03(2) Uiso 1 1 d D . . N11 N 0.2949(6) 0.1844(5) 0.3942(3) 0.0164(10) Uani 1 1 d DU . . C12 C 0.4342(8) 0.2436(6) 0.4568(4) 0.0218(12) Uani 1 1 d DU . . C13 C 0.4592(10) 0.2082(8) 0.5347(5) 0.0381(18) Uani 1 1 d DU . . H13 H 0.5579 0.2523 0.5794 0.046 Uiso 1 1 calc R . . C14 C 0.3374(12) 0.1080(8) 0.5449(5) 0.046(2) Uani 1 1 d DU . . H14 H 0.3501 0.0834 0.5979 0.056 Uiso 1 1 calc R . . C15 C 0.1969(11) 0.0432(7) 0.4786(5) 0.0369(17) Uani 1 1 d DU . . H15 H 0.1148 -0.0292 0.4844 0.044 Uiso 1 1 calc R . . C16 C 0.1750(9) 0.0832(6) 0.4033(4) 0.0261(14) Uani 1 1 d DU . . C17 C 0.0250(9) 0.0183(8) 0.3303(5) 0.0358(18) Uani 1 1 d U . . H17A H -0.0223 0.0807 0.3232 0.043 Uiso 1 1 calc R . . H17B H -0.0481 -0.0558 0.3438 0.043 Uiso 1 1 calc R . . H17C H 0.0464 -0.0128 0.2758 0.043 Uiso 1 1 calc R . . C21 C 0.0706(8) 0.3992(6) 0.1612(4) 0.0228(13) Uani 1 1 d DU . . C22 C 0.0829(10) 0.5166(8) 0.1453(5) 0.0395(19) Uani 1 1 d DU . . H22 H 0.1811 0.5766 0.1436 0.047 Uiso 1 1 calc R . . C23 C -0.0480(11) 0.5479(9) 0.1316(7) 0.057(3) Uani 1 1 d DU . . H23 H -0.0391 0.6292 0.1216 0.068 Uiso 1 1 calc R . . C24 C -0.1901(10) 0.4591(8) 0.1329(6) 0.045(2) Uani 1 1 d DU . . H24 H -0.2807 0.4780 0.1213 0.055 Uiso 1 1 calc R . . C25 C -0.2024(9) 0.3456(9) 0.1504(6) 0.044(2) Uani 1 1 d DU . . H25 H -0.3011 0.2862 0.1519 0.053 Uiso 1 1 calc R . . C26 C -0.0717(8) 0.3148(8) 0.1663(5) 0.0335(16) Uani 1 1 d DU . . H26 H -0.0804 0.2361 0.1806 0.040 Uiso 1 1 calc R . . C31 C 0.1962(7) 0.2315(6) 0.0729(4) 0.0197(12) Uani 1 1 d DU . . C32 C 0.0681(8) 0.1949(7) -0.0006(4) 0.0273(14) Uani 1 1 d DU . . H32 H -0.0082 0.2302 0.0013 0.033 Uiso 1 1 calc R . . C33 C 0.0519(9) 0.1063(7) -0.0769(4) 0.0323(16) Uani 1 1 d DU . . H33 H -0.0372 0.0800 -0.1267 0.039 Uiso 1 1 calc R . . C34 C 0.1620(8) 0.0566(7) -0.0814(5) 0.0319(15) Uani 1 1 d DU . . H34 H 0.1501 -0.0026 -0.1345 0.038 Uiso 1 1 calc R . . C35 C 0.2910(9) 0.0923(7) -0.0088(5) 0.0313(15) Uani 1 1 d DU . . H35 H 0.3675 0.0574 -0.0116 0.038 Uiso 1 1 calc R . . C36 C 0.3072(8) 0.1793(7) 0.0678(4) 0.0267(14) Uani 1 1 d DU . . H36 H 0.3955 0.2039 0.1177 0.032 Uiso 1 1 calc R . . C41 C 0.4063(7) 0.4897(6) 0.1828(4) 0.0210(13) Uani 1 1 d DU . . C42 C 0.5212(7) 0.5555(6) 0.2625(4) 0.0247(14) Uani 1 1 d DU . . H42 H 0.5105 0.5261 0.3129 0.030 Uiso 1 1 calc R . . C43 C 0.6532(9) 0.6656(7) 0.2686(5) 0.0321(16) Uani 1 1 d DU . . H43 H 0.7331 0.7112 0.3233 0.038 Uiso 1 1 calc R . . C44 C 0.6686(9) 0.7089(7) 0.1951(4) 0.0338(16) Uani 1 1 d DU . . H44 H 0.7583 0.7845 0.1997 0.041 Uiso 1 1 calc R . . C45 C 0.5534(8) 0.6421(6) 0.1153(4) 0.0291(15) Uani 1 1 d DU . . H45 H 0.5633 0.6718 0.0649 0.035 Uiso 1 1 calc R . . C46 C 0.4229(8) 0.5313(6) 0.1088(4) 0.0247(14) Uani 1 1 d DU . . H46 H 0.3448 0.4839 0.0536 0.030 Uiso 1 1 calc R . . S S 0.5937(11) 1.0881(11) 0.2559(6) 0.0279(15) Uani 0.544(13) 1 d PDU A 1 O2 O 0.568(2) 1.2065(15) 0.2728(10) 0.022(3) Uani 0.544(13) 1 d PDU A 1 O3 O 0.611(2) 1.0530(13) 0.1673(8) 0.071(5) Uani 0.544(13) 1 d PDU A 1 O4 O 0.7064(15) 1.0766(12) 0.3223(9) 0.063(4) Uani 0.544(13) 1 d PDU A 1 C99 C 0.4174(16) 0.9458(14) 0.2227(9) 0.043(5) Uani 0.544(13) 1 d PDU A 1 F1 F 0.433(3) 0.8387(18) 0.2309(15) 0.073(10) Uani 0.544(13) 1 d PDU A 1 F2 F 0.3045(15) 0.9544(12) 0.2552(12) 0.068(5) Uani 0.544(13) 1 d PDU A 1 F3 F 0.365(2) 0.9317(13) 0.1364(7) 0.089(5) Uani 0.544(13) 1 d PDU A 1 S' S 0.5975(15) 1.0902(15) 0.2746(8) 0.044(3) Uani 0.456(13) 1 d PDU A 2 O2' O 0.7068(18) 1.0782(15) 0.2277(13) 0.064(5) Uani 0.456(13) 1 d PDU A 2 O3' O 0.534(2) 1.1844(19) 0.2601(15) 0.028(5) Uani 0.456(13) 1 d PDU A 2 O4' O 0.6383(19) 1.0942(13) 0.3658(8) 0.053(4) Uani 0.456(13) 1 d PDU A 2 C99' C 0.4184(18) 0.9513(17) 0.2496(12) 0.053(6) Uani 0.456(13) 1 d PDU A 2 F1' F 0.436(3) 0.8402(19) 0.2336(15) 0.049(9) Uani 0.456(13) 1 d PDU A 2 F2' F 0.385(2) 0.9585(13) 0.3262(13) 0.076(6) Uani 0.456(13) 1 d PDU A 2 F3' F 0.294(2) 0.9412(19) 0.1917(17) 0.100(9) Uani 0.456(13) 1 d PDU 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 Au 0.01909(13) 0.02358(13) 0.01129(12) 0.00831(9) 0.00124(8) 0.00953(10) Fe 0.0170(6) 0.0277(7) 0.0231(7) 0.0058(5) 0.0004(5) 0.0106(5) P 0.0205(8) 0.0221(8) 0.0138(7) 0.0089(6) 0.0027(6) 0.0106(7) O1 0.032(3) 0.038(3) 0.028(3) -0.001(2) 0.010(2) 0.016(2) C1 0.018(3) 0.032(3) 0.024(3) 0.003(3) -0.003(2) 0.014(3) C2 0.021(3) 0.038(4) 0.026(3) 0.012(3) -0.002(3) 0.013(3) C3 0.027(4) 0.048(5) 0.037(4) 0.024(3) 0.008(3) 0.016(3) C4 0.027(3) 0.032(4) 0.048(5) 0.014(3) 0.000(3) 0.014(3) C5 0.027(3) 0.026(3) 0.037(4) 0.002(3) -0.002(3) 0.014(3) C6 0.022(3) 0.032(3) 0.026(3) 0.003(3) 0.003(3) 0.017(3) N2 0.019(3) 0.034(3) 0.014(3) 0.002(2) -0.004(2) 0.010(2) N11 0.020(2) 0.022(2) 0.011(2) 0.0060(19) 0.0023(19) 0.013(2) C12 0.030(3) 0.029(3) 0.011(3) 0.006(2) 0.001(2) 0.020(3) C13 0.046(4) 0.043(4) 0.019(3) 0.012(3) -0.010(3) 0.021(3) C14 0.073(6) 0.042(5) 0.026(4) 0.022(3) 0.005(4) 0.026(4) C15 0.058(5) 0.029(4) 0.026(4) 0.016(3) 0.016(3) 0.015(3) C16 0.037(4) 0.024(3) 0.019(3) 0.008(3) 0.008(3) 0.013(3) C17 0.033(4) 0.032(4) 0.031(4) 0.012(3) 0.008(3) -0.001(3) C21 0.026(3) 0.029(3) 0.016(3) 0.008(3) 0.004(3) 0.015(3) C22 0.045(4) 0.039(4) 0.057(5) 0.031(4) 0.023(4) 0.030(4) C23 0.056(5) 0.061(6) 0.087(7) 0.050(6) 0.031(5) 0.042(4) C24 0.044(4) 0.074(6) 0.046(5) 0.033(5) 0.019(4) 0.045(4) C25 0.030(4) 0.055(5) 0.055(5) 0.021(4) 0.012(4) 0.025(4) C26 0.026(3) 0.039(4) 0.044(4) 0.019(4) 0.012(3) 0.019(3) C31 0.021(3) 0.023(3) 0.015(3) 0.008(2) 0.001(2) 0.010(3) C32 0.028(3) 0.037(4) 0.017(3) 0.011(3) 0.001(3) 0.015(3) C33 0.038(4) 0.039(4) 0.014(3) 0.006(3) -0.001(3) 0.014(3) C34 0.041(4) 0.024(3) 0.022(3) 0.004(3) 0.006(3) 0.007(3) C35 0.039(4) 0.033(4) 0.028(4) 0.010(3) 0.011(3) 0.021(3) C36 0.032(4) 0.032(4) 0.016(3) 0.008(3) 0.003(3) 0.013(3) C41 0.022(3) 0.023(3) 0.019(3) 0.009(2) 0.005(2) 0.010(3) C42 0.026(3) 0.029(3) 0.016(3) 0.008(3) 0.002(2) 0.010(3) C43 0.032(4) 0.031(4) 0.025(3) 0.007(3) 0.005(3) 0.007(3) C44 0.030(4) 0.032(4) 0.035(4) 0.013(3) 0.011(3) 0.005(3) C45 0.040(4) 0.028(3) 0.021(3) 0.012(3) 0.010(3) 0.013(3) C46 0.028(3) 0.027(3) 0.018(3) 0.008(3) 0.004(3) 0.011(3) S 0.024(3) 0.040(3) 0.035(3) 0.026(2) 0.011(2) 0.022(2) O2 0.012(6) 0.026(6) 0.019(6) -0.007(4) -0.004(4) 0.007(5) O3 0.107(9) 0.063(7) 0.061(7) 0.018(5) 0.054(7) 0.038(6) O4 0.048(6) 0.055(6) 0.079(8) 0.030(6) -0.016(5) 0.028(5) C99 0.036(8) 0.030(8) 0.048(10) -0.007(7) -0.004(7) 0.017(7) F1 0.061(14) 0.035(14) 0.109(17) 0.010(12) -0.008(12) 0.027(11) F2 0.043(8) 0.045(6) 0.130(14) 0.027(10) 0.044(10) 0.024(6) F3 0.131(13) 0.074(8) 0.028(6) -0.008(6) -0.031(7) 0.044(9) S' 0.031(4) 0.042(4) 0.055(6) 0.022(4) -0.002(4) 0.017(3) O2' 0.048(7) 0.052(7) 0.097(9) 0.009(6) 0.031(7) 0.028(6) O3' 0.019(8) 0.023(7) 0.029(7) 0.001(6) -0.003(6) 0.004(6) O4' 0.071(8) 0.035(6) 0.040(7) 0.010(5) -0.016(5) 0.025(6) C99' 0.035(9) 0.040(10) 0.075(14) -0.009(10) -0.002(9) 0.028(8) F1' 0.045(13) 0.035(15) 0.065(13) 0.001(11) 0.021(11) 0.018(11) F2' 0.088(12) 0.061(8) 0.129(16) 0.049(9) 0.086(12) 0.045(8) F3' 0.046(10) 0.082(12) 0.123(18) 0.009(15) -0.046(12) 0.021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au N11 2.110(5) . y Au P 2.2353(17) . y Fe C1 2.029(6) 2_766 ? Fe C1 2.029(6) . ? Fe C2 2.033(7) . ? Fe C2 2.033(7) 2_766 ? Fe C5 2.037(7) . ? Fe C5 2.037(7) 2_766 ? Fe C3 2.043(7) . ? Fe C3 2.043(7) 2_766 ? Fe C4 2.056(8) 2_766 ? Fe C4 2.056(8) . ? P C21 1.805(7) . ? P C41 1.812(6) . ? P C31 1.814(7) . ? O1 C6 1.220(8) . ? C1 C5 1.420(9) . ? C1 C2 1.427(9) . ? C1 C6 1.478(10) . ? C2 C3 1.410(9) . ? C3 C4 1.425(12) . ? C4 C5 1.415(10) . ? C6 N2 1.382(9) . ? N2 C12 1.389(9) . ? N11 C12 1.336(8) . ? N11 C16 1.360(8) . ? C12 C13 1.395(9) . ? C13 C14 1.373(12) . ? C14 C15 1.374(12) . ? C15 C16 1.381(10) . ? C16 C17 1.483(10) . ? C21 C26 1.382(9) . ? C21 C22 1.382(9) . ? C22 C23 1.397(10) . ? C23 C24 1.376(10) . ? C24 C25 1.348(10) . ? C25 C26 1.393(10) . ? C31 C32 1.386(8) . ? C31 C36 1.393(8) . ? C32 C33 1.388(9) . ? C33 C34 1.364(9) . ? C34 C35 1.385(9) . ? C35 C36 1.382(9) . ? C41 C42 1.377(8) . ? C41 C46 1.387(8) . ? C42 C43 1.395(9) . ? C43 C44 1.387(9) . ? C44 C45 1.381(9) . ? C45 C46 1.389(9) . ? S O4 1.411(10) . ? S O2 1.449(10) . ? S O3 1.478(11) . ? S C99 1.760(13) . ? C99 F1 1.309(12) . ? C99 F2 1.315(12) . ? C99 F3 1.342(13) . ? S' O4' 1.435(12) . ? S' O2' 1.436(12) . ? S' O3' 1.438(12) . ? S' C99' 1.769(15) . ? C99' F3' 1.300(13) . ? C99' F1' 1.326(13) . ? C99' F2' 1.340(14) . ? 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 N11 Au P 179.31(14) . . y C1 Fe C1 180.000(2) 2_766 . ? C1 Fe C2 138.9(3) 2_766 . ? C1 Fe C2 41.1(3) . . ? C1 Fe C2 41.1(3) 2_766 2_766 ? C1 Fe C2 138.9(3) . 2_766 ? C2 Fe C2 180.000(2) . 2_766 ? C1 Fe C5 139.1(3) 2_766 . ? C1 Fe C5 40.9(2) . . ? C2 Fe C5 68.9(3) . . ? C2 Fe C5 111.1(3) 2_766 . ? C1 Fe C5 40.9(2) 2_766 2_766 ? C1 Fe C5 139.1(3) . 2_766 ? C2 Fe C5 111.1(3) . 2_766 ? C2 Fe C5 68.9(3) 2_766 2_766 ? C5 Fe C5 180.000(2) . 2_766 ? C1 Fe C3 111.7(3) 2_766 . ? C1 Fe C3 68.3(3) . . ? C2 Fe C3 40.5(3) . . ? C2 Fe C3 139.5(3) 2_766 . ? C5 Fe C3 68.3(3) . . ? C5 Fe C3 111.7(3) 2_766 . ? C1 Fe C3 68.3(3) 2_766 2_766 ? C1 Fe C3 111.7(3) . 2_766 ? C2 Fe C3 139.5(3) . 2_766 ? C2 Fe C3 40.5(3) 2_766 2_766 ? C5 Fe C3 111.7(3) . 2_766 ? C5 Fe C3 68.3(3) 2_766 2_766 ? C3 Fe C3 180.000(2) . 2_766 ? C1 Fe C4 68.4(3) 2_766 2_766 ? C1 Fe C4 111.6(3) . 2_766 ? C2 Fe C4 111.4(3) . 2_766 ? C2 Fe C4 68.6(3) 2_766 2_766 ? C5 Fe C4 139.6(3) . 2_766 ? C5 Fe C4 40.4(3) 2_766 2_766 ? C3 Fe C4 139.3(3) . 2_766 ? C3 Fe C4 40.7(3) 2_766 2_766 ? C1 Fe C4 111.6(3) 2_766 . ? C1 Fe C4 68.4(3) . . ? C2 Fe C4 68.6(3) . . ? C2 Fe C4 111.4(3) 2_766 . ? C5 Fe C4 40.4(3) . . ? C5 Fe C4 139.6(3) 2_766 . ? C3 Fe C4 40.7(3) . . ? C3 Fe C4 139.3(3) 2_766 . ? C4 Fe C4 180.000(2) 2_766 . ? C21 P C41 106.5(3) . . ? C21 P C31 107.1(3) . . ? C41 P C31 104.8(3) . . ? C21 P Au 114.1(2) . . y C41 P Au 113.4(2) . . y C31 P Au 110.4(2) . . y C5 C1 C2 108.0(6) . . ? C5 C1 C6 123.0(6) . . ? C2 C1 C6 128.4(6) . . ? C5 C1 Fe 69.9(4) . . ? C2 C1 Fe 69.6(4) . . ? C6 C1 Fe 119.3(5) . . ? C3 C2 C1 107.5(6) . . ? C3 C2 Fe 70.2(4) . . ? C1 C2 Fe 69.3(4) . . ? C2 C3 C4 108.8(6) . . ? C2 C3 Fe 69.4(4) . . ? C4 C3 Fe 70.1(4) . . ? C5 C4 C3 107.5(6) . . ? C5 C4 Fe 69.1(4) . . ? C3 C4 Fe 69.2(4) . . ? C4 C5 C1 108.2(6) . . ? C4 C5 Fe 70.5(4) . . ? C1 C5 Fe 69.2(4) . . ? O1 C6 N2 121.7(7) . . ? O1 C6 C1 122.5(6) . . ? N2 C6 C1 115.8(6) . . ? C6 N2 C12 123.4(6) . . ? C12 N11 C16 120.5(5) . . ? C12 N11 Au 117.6(4) . . y C16 N11 Au 121.7(4) . . y N11 C12 N2 116.7(5) . . ? N11 C12 C13 121.5(7) . . ? N2 C12 C13 121.8(6) . . ? C14 C13 C12 118.1(7) . . ? C13 C14 C15 120.1(7) . . ? C14 C15 C16 120.1(7) . . ? N11 C16 C15 119.6(7) . . ? N11 C16 C17 118.0(6) . . ? C15 C16 C17 122.4(7) . . ? C26 C21 C22 119.1(7) . . ? C26 C21 P 117.8(5) . . ? C22 C21 P 123.2(5) . . ? C21 C22 C23 120.5(7) . . ? C24 C23 C22 119.0(8) . . ? C25 C24 C23 120.9(8) . . ? C24 C25 C26 120.6(8) . . ? C21 C26 C25 119.8(7) . . ? C32 C31 C36 118.8(6) . . ? C32 C31 P 123.7(5) . . ? C36 C31 P 117.5(4) . . ? C31 C32 C33 119.8(7) . . ? C34 C33 C32 121.0(6) . . ? C33 C34 C35 120.1(7) . . ? C36 C35 C34 119.3(7) . . ? C35 C36 C31 121.1(6) . . ? C42 C41 C46 120.3(6) . . ? C42 C41 P 119.5(5) . . ? C46 C41 P 120.1(5) . . ? C41 C42 C43 119.4(6) . . ? C44 C43 C42 120.4(6) . . ? C45 C44 C43 119.9(7) . . ? C44 C45 C46 119.8(6) . . ? C41 C46 C45 120.1(6) . . ? O4 S O2 117.5(9) . . ? O4 S O3 113.4(9) . . ? O2 S O3 111.8(8) . . ? O4 S C99 109.1(9) . . ? O2 S C99 112.8(10) . . ? O3 S C99 88.8(9) . . ? F1 C99 F2 108.5(12) . . ? F1 C99 F3 107.4(12) . . ? F2 C99 F3 105.7(11) . . ? F1 C99 S 116.0(14) . . ? F2 C99 S 116.1(11) . . ? F3 C99 S 101.9(11) . . ? O4' S' O2' 117.2(14) . . ? O4' S' O3' 111.5(13) . . ? O2' S' O3' 116.3(13) . . ? O4' S' C99' 92.1(10) . . ? O2' S' C99' 116.9(12) . . ? O3' S' C99' 99.1(12) . . ? F3' C99' F1' 110.1(16) . . ? F3' C99' F2' 106.5(18) . . ? F1' C99' F2' 102.9(14) . . ? F3' C99' S' 119.1(14) . . ? F1' C99' S' 112.9(14) . . ? F2' C99' S' 103.6(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.071 _refine_diff_density_min -4.888 _refine_diff_density_rms 0.264 # Attachment 'complex5.CIF' data_phewfe _database_code_depnum_ccdc_archive 'CCDC 760668' #TrackingRef 'complex5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H22 Ag F3 Fe N4 O5 S' _chemical_formula_weight 711.25 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 12.0259(6) _cell_length_b 12.0259(6) _cell_length_c 17.3790(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2513.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 7138 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w- & \f-scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48819 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6237 _reflns_number_gt 5715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0270P)^2^] 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 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.014(11) _refine_ls_number_reflns 6237 _refine_ls_number_parameters 371 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0491 _refine_ls_wR_factor_gt 0.0478 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.006 _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 Ag Ag 0.579690(13) 0.535783(13) 0.180895(10) 0.01816(4) Uani 1 1 d . . . Fe Fe 0.18531(2) 0.35275(2) 0.17750(2) 0.01611(7) Uani 1 1 d . . . C1 C 0.2826(2) 0.2995(2) 0.26480(14) 0.0201(5) Uani 1 1 d . . . C2 C 0.2583(2) 0.4144(2) 0.27444(14) 0.0210(5) Uani 1 1 d . . . H2 H 0.3114 0.4727 0.2767 0.025 Uiso 1 1 calc R . . C3 C 0.1408(2) 0.4272(2) 0.28005(15) 0.0258(6) Uani 1 1 d . . . H3 H 0.1016 0.4952 0.2861 0.031 Uiso 1 1 calc R . . C4 C 0.0932(2) 0.3193(2) 0.27488(14) 0.0273(6) Uani 1 1 d . . . H4 H 0.0160 0.3030 0.2776 0.033 Uiso 1 1 calc R . . C5 C 0.1779(2) 0.2407(2) 0.26517(14) 0.0253(5) Uani 1 1 d . . . H5 H 0.1682 0.1627 0.2598 0.030 Uiso 1 1 calc R . . C6 C 0.2565(2) 0.43233(19) 0.08765(14) 0.0175(5) Uani 1 1 d . . . C7 C 0.1388(2) 0.4537(2) 0.08854(14) 0.0203(5) Uani 1 1 d . . . H7 H 0.1041 0.5243 0.0932 0.024 Uiso 1 1 calc R . . C8 C 0.0845(2) 0.3495(2) 0.08114(14) 0.0225(5) Uani 1 1 d . . . H8 H 0.0063 0.3386 0.0796 0.027 Uiso 1 1 calc R . . C9 C 0.1660(2) 0.2641(2) 0.07644(13) 0.0218(5) Uani 1 1 d . . . H9 H 0.1516 0.1867 0.0719 0.026 Uiso 1 1 calc R . . C10 C 0.2724(2) 0.3147(2) 0.07966(13) 0.0196(5) Uani 1 1 d . . . H10 H 0.3418 0.2773 0.0770 0.023 Uiso 1 1 calc R . . C11 C 0.38993(19) 0.2450(2) 0.24833(13) 0.0207(5) Uani 1 1 d . . . C12 C 0.34935(19) 0.51158(19) 0.09483(13) 0.0171(5) Uani 1 1 d . . . N11 N 0.47989(17) 0.31563(17) 0.24947(12) 0.0196(4) Uani 1 1 d . . . H11 H 0.469(2) 0.377(2) 0.2614(16) 0.023(8) Uiso 1 1 d . . . N12 N 0.32571(17) 0.61228(17) 0.12570(13) 0.0193(4) Uani 1 1 d . . . H12 H 0.264(2) 0.626(2) 0.1418(17) 0.027(8) Uiso 1 1 d . . . O1 O 0.39847(15) 0.14576(14) 0.23442(11) 0.0306(4) Uani 1 1 d . . . O2 O 0.44463(13) 0.48557(13) 0.07243(9) 0.0197(3) Uani 1 1 d . . . N21 N 0.65365(16) 0.37702(16) 0.21253(11) 0.0170(4) Uani 1 1 d . . . C22 C 0.5905(2) 0.2890(2) 0.23267(13) 0.0177(5) Uani 1 1 d . . . C23 C 0.6328(2) 0.1814(2) 0.23897(15) 0.0219(5) Uani 1 1 d . . . H23 H 0.5866 0.1212 0.2540 0.026 Uiso 1 1 calc R . . C24 C 0.7442(2) 0.1653(2) 0.22256(15) 0.0246(5) Uani 1 1 d . . . H24 H 0.7755 0.0929 0.2249 0.030 Uiso 1 1 calc R . . C25 C 0.8100(2) 0.2556(2) 0.20262(14) 0.0226(5) Uani 1 1 d . . . H25 H 0.8864 0.2451 0.1909 0.027 Uiso 1 1 calc R . . C26 C 0.76410(18) 0.36102(19) 0.19991(12) 0.0175(5) Uani 1 1 d . . . C27 C 0.83201(17) 0.46348(18) 0.18404(17) 0.0227(5) Uani 1 1 d . . . H27A H 0.8085 0.4964 0.1351 0.027 Uiso 1 1 calc R . . H27B H 0.9109 0.4434 0.1810 0.027 Uiso 1 1 calc R . . H27C H 0.8210 0.5174 0.2256 0.027 Uiso 1 1 calc R . . N31 N 0.50286(15) 0.69506(16) 0.14852(11) 0.0169(4) Uani 1 1 d . . . C32 C 0.3946(2) 0.7071(2) 0.13039(14) 0.0182(5) Uani 1 1 d . . . C33 C 0.3451(2) 0.8095(2) 0.11819(16) 0.0225(5) Uani 1 1 d . . . H33 H 0.2693 0.8146 0.1032 0.027 Uiso 1 1 calc R . . C34 C 0.4089(2) 0.9045(2) 0.12832(15) 0.0252(5) Uani 1 1 d . . . H34 H 0.3765 0.9761 0.1229 0.030 Uiso 1 1 calc R . . C35 C 0.5199(2) 0.89331(19) 0.14635(14) 0.0231(5) Uani 1 1 d . . . H35 H 0.5649 0.9576 0.1525 0.028 Uiso 1 1 calc R . . C36 C 0.56622(19) 0.7885(2) 0.15558(13) 0.0196(5) Uani 1 1 d . . . C37 C 0.68709(18) 0.7726(2) 0.17307(17) 0.0253(5) Uani 1 1 d . . . H37A H 0.6952 0.7212 0.2165 0.030 Uiso 1 1 calc R . . H37B H 0.7205 0.8444 0.1863 0.030 Uiso 1 1 calc R . . H37C H 0.7247 0.7416 0.1278 0.030 Uiso 1 1 calc R . . S S 0.03418(5) 0.73610(5) 0.15612(4) 0.02502(13) Uani 1 1 d . . . O3 O 0.12442(14) 0.69696(15) 0.20381(11) 0.0315(4) Uani 1 1 d . . . O4 O -0.07263(14) 0.69050(16) 0.17243(16) 0.0475(6) Uani 1 1 d . . . O5 O 0.06377(17) 0.73979(17) 0.07547(12) 0.0409(5) Uani 1 1 d . . . C99 C 0.0191(2) 0.8827(2) 0.1822(2) 0.0307(5) Uani 1 1 d . . . F1 F 0.11273(13) 0.93978(12) 0.17164(12) 0.0426(4) Uani 1 1 d . . . F2 F -0.06002(14) 0.93074(15) 0.13976(12) 0.0480(5) Uani 1 1 d . . . F3 F -0.00838(17) 0.89382(16) 0.25551(11) 0.0554(5) 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 Ag 0.01808(8) 0.01738(8) 0.01904(8) 0.00158(8) -0.00001(8) 0.00138(6) Fe 0.01477(14) 0.01991(15) 0.01364(14) -0.00015(14) -0.00038(15) -0.00202(11) C1 0.0201(12) 0.0238(12) 0.0163(12) 0.0051(9) -0.0028(9) -0.0058(9) C2 0.0179(12) 0.0315(14) 0.0136(11) -0.0031(10) -0.0001(9) -0.0049(10) C3 0.0214(12) 0.0394(15) 0.0165(12) -0.0061(11) 0.0033(10) 0.0008(11) C4 0.0178(12) 0.0474(17) 0.0166(12) 0.0032(12) 0.0011(9) -0.0082(11) C5 0.0264(13) 0.0314(14) 0.0182(12) 0.0069(10) -0.0042(10) -0.0095(11) C6 0.0203(12) 0.0183(12) 0.0141(11) 0.0018(9) -0.0003(9) -0.0016(9) C7 0.0197(12) 0.0232(12) 0.0180(12) 0.0019(9) -0.0017(9) 0.0006(10) C8 0.0217(12) 0.0294(14) 0.0164(12) 0.0000(10) -0.0040(10) -0.0022(10) C9 0.0261(13) 0.0233(13) 0.0161(12) -0.0019(10) 0.0004(10) -0.0058(10) C10 0.0196(12) 0.0233(12) 0.0158(12) -0.0024(9) 0.0018(9) 0.0008(9) C11 0.0211(12) 0.0238(12) 0.0172(12) 0.0059(9) -0.0058(9) -0.0046(9) C12 0.0195(12) 0.0186(11) 0.0132(11) 0.0026(9) -0.0007(8) 0.0016(9) N11 0.0193(10) 0.0154(10) 0.0241(11) 0.0009(9) 0.0004(8) -0.0005(8) N12 0.0148(10) 0.0176(10) 0.0257(11) 0.0004(8) 0.0035(9) -0.0003(8) O1 0.0287(10) 0.0187(9) 0.0443(12) 0.0042(8) -0.0092(9) -0.0037(7) O2 0.0193(8) 0.0220(9) 0.0180(9) -0.0008(7) 0.0017(6) 0.0014(7) N21 0.0184(10) 0.0184(10) 0.0142(9) -0.0017(8) -0.0010(8) 0.0003(8) C22 0.0188(12) 0.0194(12) 0.0150(11) -0.0002(9) -0.0020(9) 0.0005(9) C23 0.0275(13) 0.0186(12) 0.0196(12) 0.0022(10) -0.0019(10) 0.0015(10) C24 0.0286(13) 0.0235(13) 0.0217(13) -0.0012(10) -0.0046(10) 0.0087(10) C25 0.0171(11) 0.0300(13) 0.0208(12) -0.0017(9) -0.0023(9) 0.0057(10) C26 0.0188(11) 0.0218(11) 0.0120(12) -0.0018(8) -0.0017(8) -0.0001(9) C27 0.0174(10) 0.0266(11) 0.0241(12) 0.0004(12) 0.0020(11) 0.0005(9) N31 0.0182(10) 0.0182(10) 0.0142(9) -0.0010(8) 0.0034(8) -0.0010(7) C32 0.0212(12) 0.0177(12) 0.0156(11) -0.0008(9) 0.0050(9) -0.0008(9) C33 0.0215(12) 0.0196(13) 0.0265(14) 0.0037(10) 0.0046(10) 0.0028(10) C34 0.0315(14) 0.0156(12) 0.0284(14) 0.0030(10) 0.0063(11) 0.0026(10) C35 0.0301(13) 0.0169(11) 0.0224(12) -0.0004(9) 0.0056(10) -0.0085(10) C36 0.0210(12) 0.0237(12) 0.0139(11) -0.0001(9) 0.0037(9) -0.0026(9) C37 0.0220(12) 0.0274(12) 0.0266(13) -0.0002(11) -0.0025(11) -0.0049(9) S 0.0177(3) 0.0242(3) 0.0332(3) -0.0018(2) -0.0024(2) -0.0007(2) O3 0.0271(9) 0.0307(10) 0.0367(11) 0.0005(8) -0.0048(8) 0.0032(8) O4 0.0243(10) 0.0356(11) 0.0827(17) 0.0075(13) 0.0025(12) -0.0065(8) O5 0.0407(12) 0.0477(13) 0.0344(11) -0.0096(10) -0.0024(9) 0.0038(10) C99 0.0287(13) 0.0283(13) 0.0351(14) -0.0007(14) 0.0012(14) 0.0023(10) F1 0.0377(9) 0.0277(8) 0.0624(12) -0.0022(9) -0.0009(9) -0.0059(6) F2 0.0379(10) 0.0379(10) 0.0682(13) 0.0067(9) -0.0077(9) 0.0152(8) F3 0.0694(13) 0.0552(12) 0.0417(11) -0.0142(9) 0.0178(10) 0.0135(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N21 2.1768(19) . Y Ag N31 2.1998(19) . Y Ag O2 2.5605(16) . Y Ag O2 2.7178(17) 4_565 Y Fe C1 2.020(2) . ? Fe C6 2.022(2) . ? Fe C5 2.036(3) . ? Fe C2 2.039(2) . ? Fe C7 2.044(2) . ? Fe C10 2.048(2) . ? Fe C4 2.063(3) . ? Fe C3 2.065(3) . ? Fe C9 2.068(2) . ? Fe C8 2.068(2) . ? C1 C2 1.422(4) . Y C1 C5 1.443(3) . Y C1 C11 1.476(3) . Y C2 C3 1.424(3) . Y C3 C4 1.421(4) . Y C4 C5 1.400(4) . Y C6 C10 1.434(3) . Y C6 C7 1.439(3) . Y C6 C12 1.473(3) . Y C7 C8 1.419(3) . Y C8 C9 1.422(4) . Y C9 C10 1.418(3) . Y C11 O1 1.222(3) . Y C11 N11 1.376(3) . Y C12 O2 1.250(3) . Y C12 N12 1.355(3) . Y N11 C22 1.399(3) . Y N12 C32 1.412(3) . Y O2 Ag 2.7178(17) 3_654 ? N21 C22 1.349(3) . Y N21 C26 1.360(3) . Y C22 C23 1.395(3) . Y C23 C24 1.384(3) . Y C24 C25 1.388(3) . Y C25 C26 1.383(3) . Y C26 C27 1.504(3) . Y N31 C32 1.347(3) . Y N31 C36 1.363(3) . Y C32 C33 1.384(3) . Y C33 C34 1.387(3) . Y C34 C35 1.378(4) . Y C35 C36 1.387(3) . Y C36 C37 1.497(3) . Y S O4 1.4251(18) . Y S O3 1.4443(18) . Y S O5 1.447(2) . Y S C99 1.829(3) . Y C99 F3 1.324(4) . Y C99 F1 1.331(3) . Y C99 F2 1.335(3) . Y 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 N21 Ag N31 179.23(7) . . Y N21 Ag O2 103.79(6) . . Y N31 Ag O2 75.56(6) . . Y N21 Ag O2 91.01(6) . 4_565 Y N31 Ag O2 88.92(6) . 4_565 Y O2 Ag O2 115.00(4) . 4_565 Y C1 Fe C6 119.00(10) . . ? C1 Fe C5 41.69(9) . . ? C6 Fe C5 155.48(10) . . ? C1 Fe C2 41.02(10) . . ? C6 Fe C2 106.49(9) . . ? C5 Fe C2 68.96(10) . . ? C1 Fe C7 156.20(10) . . ? C6 Fe C7 41.44(9) . . ? C5 Fe C7 161.33(10) . . ? C2 Fe C7 121.78(10) . . ? C1 Fe C10 104.87(10) . . ? C6 Fe C10 41.25(9) . . ? C5 Fe C10 119.72(10) . . ? C2 Fe C10 123.17(10) . . ? C7 Fe C10 69.18(10) . . ? C1 Fe C4 68.46(10) . . ? C6 Fe C4 162.50(11) . . ? C5 Fe C4 39.93(11) . . ? C2 Fe C4 67.92(10) . . ? C7 Fe C4 126.14(10) . . ? C10 Fe C4 155.79(10) . . ? C1 Fe C3 68.86(11) . . ? C6 Fe C3 124.84(10) . . ? C5 Fe C3 68.25(11) . . ? C2 Fe C3 40.61(9) . . ? C7 Fe C3 108.93(10) . . ? C10 Fe C3 161.03(10) . . ? C4 Fe C3 40.28(11) . . ? C1 Fe C9 122.65(10) . . ? C6 Fe C9 68.64(10) . . ? C5 Fe C9 106.83(10) . . ? C2 Fe C9 159.66(10) . . ? C7 Fe C9 68.48(10) . . ? C10 Fe C9 40.30(9) . . ? C4 Fe C9 122.40(10) . . ? C3 Fe C9 158.03(10) . . ? C1 Fe C8 160.36(10) . . ? C6 Fe C8 68.40(10) . . ? C5 Fe C8 124.61(10) . . ? C2 Fe C8 158.17(11) . . ? C7 Fe C8 40.38(10) . . ? C10 Fe C8 67.87(10) . . ? C4 Fe C8 110.23(9) . . ? C3 Fe C8 123.71(10) . . ? C9 Fe C8 40.23(10) . . ? C2 C1 C5 107.2(2) . . y C2 C1 C11 129.3(2) . . y C5 C1 C11 123.1(2) . . y C2 C1 Fe 70.20(14) . . ? C5 C1 Fe 69.74(14) . . ? C11 C1 Fe 120.12(17) . . ? C1 C2 C3 108.5(2) . . y C1 C2 Fe 68.78(14) . . ? C3 C2 Fe 70.68(14) . . ? C4 C3 C2 107.3(2) . . y C4 C3 Fe 69.77(14) . . ? C2 C3 Fe 68.71(14) . . ? C5 C4 C3 109.3(2) . . y C5 C4 Fe 69.00(15) . . ? C3 C4 Fe 69.96(14) . . ? C4 C5 C1 107.8(2) . . y C4 C5 Fe 71.06(15) . . ? C1 C5 Fe 68.57(14) . . ? C10 C6 C7 107.9(2) . . y C10 C6 C12 123.1(2) . . y C7 C6 C12 129.0(2) . . y C10 C6 Fe 70.37(13) . . ? C7 C6 Fe 70.09(13) . . ? C12 C6 Fe 124.19(17) . . ? C8 C7 C6 107.1(2) . . y C8 C7 Fe 70.72(14) . . ? C6 C7 Fe 68.46(13) . . ? C7 C8 C9 109.0(2) . . y C7 C8 Fe 68.89(14) . . ? C9 C8 Fe 69.89(14) . . ? C10 C9 C8 108.0(2) . . y C10 C9 Fe 69.11(13) . . ? C8 C9 Fe 69.88(14) . . ? C9 C10 C6 107.9(2) . . y C9 C10 Fe 70.59(14) . . ? C6 C10 Fe 68.38(13) . . ? O1 C11 N11 122.7(2) . . Y O1 C11 C1 123.1(2) . . Y N11 C11 C1 114.3(2) . . Y O2 C12 N12 122.6(2) . . Y O2 C12 C6 120.4(2) . . Y N12 C12 C6 116.9(2) . . Y C11 N11 C22 127.1(2) . . Y C12 N12 C32 128.4(2) . . Y C12 O2 Ag 107.05(14) . . Y C12 O2 Ag 104.90(14) . 3_654 Y Ag O2 Ag 120.87(6) . 3_654 Y C22 N21 C26 118.8(2) . . Y C22 N21 Ag 121.56(16) . . Y C26 N21 Ag 118.85(15) . . Y N21 C22 C23 122.9(2) . . Y N21 C22 N11 114.2(2) . . Y C23 C22 N11 122.9(2) . . Y C24 C23 C22 117.8(2) . . Y C23 C24 C25 119.6(2) . . Y C26 C25 C24 119.9(2) . . Y N21 C26 C25 120.9(2) . . Y N21 C26 C27 116.4(2) . . Y C25 C26 C27 122.7(2) . . Y C32 N31 C36 118.2(2) . . Y C32 N31 Ag 124.01(15) . . Y C36 N31 Ag 117.38(15) . . Y N31 C32 C33 123.2(2) . . Y N31 C32 N12 119.6(2) . . Y C33 C32 N12 117.2(2) . . Y C32 C33 C34 118.4(2) . . Y C35 C34 C33 118.9(2) . . Y C34 C35 C36 120.3(2) . . Y N31 C36 C35 120.9(2) . . Y N31 C36 C37 117.1(2) . . Y C35 C36 C37 122.0(2) . . Y O4 S O3 115.95(13) . . Y O4 S O5 115.23(15) . . Y O3 S O5 112.40(12) . . Y O4 S C99 103.45(12) . . Y O3 S C99 104.26(12) . . Y O5 S C99 103.56(14) . . Y F3 C99 F1 107.0(2) . . Y F3 C99 F2 108.0(2) . . Y F1 C99 F2 107.7(2) . . Y F3 C99 S 111.1(2) . . Y F1 C99 S 112.29(17) . . Y F2 C99 S 110.5(2) . . Y 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 N12 H12 O3 0.81(3) 2.17(3) 2.956(3) 164(3) . N11 H11 O2 0.78(3) 2.40(3) 3.150(3) 162(3) 4_565 C8 H8 O1 0.95 2.57 3.292(3) 133.2 3_554 C2 H2 O2 0.95 2.45 3.323(3) 152.7 4_565 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.456 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.058 # Attachment 'complex_20.cif' data_lol20as _database_code_depnum_ccdc_archive 'CCDC 760669' #TrackingRef 'complex_20.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22 Cl2 Fe N4 O2 Pd' _chemical_formula_weight 631.63 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' Cl Cl 0.1484 0.1585 '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' 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' H H 0.0000 0.0000 '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 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 18.883(13) _cell_length_b 12.044(7) _cell_length_c 12.081(8) _cell_angle_alpha 90.00 _cell_angle_beta 121.67(2) _cell_angle_gamma 90.00 _cell_volume 2338(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2085 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6930 _exptl_absorpt_correction_T_max 0.8794 _exptl_absorpt_process_details ; SADABS; Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.02 (1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7208 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2541 _reflns_number_gt 2055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_data_reduction 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.10 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.10 (Bruker, 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^)+(0.0301P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2541 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 Pd1 Pd 0.0000 0.31931(3) 0.2500 0.02855(12) Uani 1 2 d S . . Fe1 Fe 0.0000 -0.11779(5) 0.2500 0.02605(16) Uani 1 2 d S . . Cl1 Cl 0.07316(6) 0.30937(9) 0.14841(8) 0.0502(3) Uani 1 1 d . . . O1 O 0.19005(15) -0.0002(2) 0.5612(2) 0.0486(7) Uani 1 1 d . . . N1 N 0.12515(15) 0.1367(2) 0.4117(2) 0.0293(6) Uani 1 1 d . . . H1 H 0.0901 0.1476 0.3280 0.035 Uiso 1 1 calc R . . N2 N 0.10722(16) 0.3236(2) 0.4291(2) 0.0312(6) Uani 1 1 d . . . C1 C 0.11639(18) -0.0509(3) 0.3404(3) 0.0277(7) Uani 1 1 d . . . C2 C 0.1216(2) -0.1683(3) 0.3575(3) 0.0359(8) Uani 1 1 d . . . H2 H 0.1475 -0.2061 0.4385 0.043 Uiso 1 1 calc R . . C3 C 0.0818(2) -0.2183(3) 0.2344(3) 0.0370(8) Uani 1 1 d . . . H3 H 0.0759 -0.2959 0.2178 0.044 Uiso 1 1 calc R . . C4 C 0.0521(2) -0.1339(3) 0.1394(3) 0.0346(8) Uani 1 1 d . . . H4 H 0.0229 -0.1449 0.0479 0.042 Uiso 1 1 calc R . . C5 C 0.07309(19) -0.0304(3) 0.2033(3) 0.0308(7) Uani 1 1 d . . . H5 H 0.0607 0.0404 0.1627 0.037 Uiso 1 1 calc R . . C11 C 0.14788(18) 0.0287(3) 0.4482(3) 0.0293(7) Uani 1 1 d . . . C12 C 0.14986(18) 0.2310(3) 0.4887(3) 0.0287(7) Uani 1 1 d . . . C13 C 0.21513(19) 0.2326(3) 0.6178(3) 0.0349(8) Uani 1 1 d . . . H13 H 0.2453 0.1669 0.6592 0.042 Uiso 1 1 calc R . . C14 C 0.2350(2) 0.3315(3) 0.6839(3) 0.0427(9) Uani 1 1 d . . . H14 H 0.2775 0.3338 0.7734 0.051 Uiso 1 1 calc R . . C15 C 0.1942(2) 0.4262(3) 0.6222(3) 0.0458(10) Uani 1 1 d . . . H15 H 0.2090 0.4948 0.6677 0.055 Uiso 1 1 calc R . . C16 C 0.1310(2) 0.4221(3) 0.4929(3) 0.0400(9) Uani 1 1 d . . . C17 C 0.0869(3) 0.5240(3) 0.4193(4) 0.0686(14) Uani 1 1 d . . . H17A H 0.0886 0.5282 0.3397 0.103 Uiso 1 1 calc R . . H17B H 0.1143 0.5896 0.4732 0.103 Uiso 1 1 calc R . . H17C H 0.0289 0.5214 0.3966 0.103 Uiso 1 1 calc 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 0.0402(2) 0.0225(2) 0.02065(18) 0.000 0.01436(16) 0.000 Fe1 0.0296(4) 0.0234(4) 0.0268(3) 0.000 0.0159(3) 0.000 Cl1 0.0442(5) 0.0786(8) 0.0302(4) -0.0081(5) 0.0213(4) -0.0180(5) O1 0.0583(16) 0.0452(16) 0.0240(12) 0.0114(12) 0.0090(12) 0.0072(13) N1 0.0303(14) 0.0304(15) 0.0184(13) -0.0003(12) 0.0067(11) -0.0028(11) N2 0.0399(16) 0.0296(15) 0.0231(13) -0.0031(12) 0.0157(12) -0.0088(13) C1 0.0256(17) 0.0297(18) 0.0276(16) 0.0049(14) 0.0138(14) 0.0017(13) C2 0.0349(19) 0.031(2) 0.0402(19) 0.0084(16) 0.0184(16) 0.0094(15) C3 0.039(2) 0.0276(19) 0.051(2) -0.0019(17) 0.0279(17) 0.0047(15) C4 0.040(2) 0.037(2) 0.0350(18) -0.0035(16) 0.0255(16) 0.0017(16) C5 0.0300(18) 0.035(2) 0.0338(18) 0.0054(15) 0.0211(15) 0.0004(14) C11 0.0232(17) 0.035(2) 0.0291(17) 0.0038(15) 0.0130(14) 0.0002(14) C12 0.0283(17) 0.0331(19) 0.0258(16) -0.0022(15) 0.0149(14) -0.0092(14) C13 0.0327(18) 0.045(2) 0.0228(16) -0.0029(16) 0.0116(14) -0.0093(16) C14 0.036(2) 0.060(3) 0.0288(18) -0.0144(18) 0.0149(15) -0.0177(18) C15 0.060(3) 0.046(2) 0.036(2) -0.0197(18) 0.0282(19) -0.023(2) C16 0.061(2) 0.029(2) 0.0354(19) -0.0093(16) 0.0290(18) -0.0126(17) C17 0.124(4) 0.025(2) 0.046(2) -0.0080(19) 0.037(3) -0.006(2) _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 2.046(3) 2 y Pd1 N2 2.046(3) . y Pd1 Cl1 2.2825(14) 2 y Pd1 Cl1 2.2825(14) . y Fe1 C5 2.036(3) . ? Fe1 C5 2.036(3) 2 ? Fe1 C1 2.037(3) . ? Fe1 C1 2.037(3) 2 ? Fe1 C4 2.042(3) . ? Fe1 C4 2.042(3) 2 ? Fe1 C3 2.048(3) 2 ? Fe1 C3 2.048(3) . ? Fe1 C2 2.048(3) . ? Fe1 C2 2.048(3) 2 ? O1 C11 1.215(3) . y N1 C11 1.368(4) . y N1 C12 1.385(4) . y N1 H1 0.8800 . ? N2 C12 1.343(4) . ? N2 C16 1.356(4) . ? C1 C2 1.424(5) . ? C1 C5 1.432(4) . ? C1 C11 1.469(4) . y C2 C3 1.402(5) . ? C2 H2 0.9500 . ? C3 C4 1.411(5) . ? C3 H3 0.9500 . ? C4 C5 1.409(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C12 C13 1.390(4) . ? C13 C14 1.372(5) . ? C13 H13 0.9500 . ? C14 C15 1.358(5) . ? C14 H14 0.9500 . ? C15 C16 1.381(5) . ? C15 H15 0.9500 . ? C16 C17 1.488(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 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 N2 177.09(15) 2 . y N2 Pd1 Cl1 91.60(10) 2 2 y N2 Pd1 Cl1 88.56(10) . 2 y N2 Pd1 Cl1 88.56(10) 2 . y N2 Pd1 Cl1 91.60(10) . . y Cl1 Pd1 Cl1 173.99(6) 2 . y C5 Fe1 C5 117.79(19) . 2 ? C5 Fe1 C1 41.15(12) . . ? C5 Fe1 C1 110.16(14) 2 . ? C5 Fe1 C1 110.16(14) . 2 ? C5 Fe1 C1 41.15(12) 2 2 ? C1 Fe1 C1 133.43(19) . 2 ? C5 Fe1 C4 40.42(13) . . ? C5 Fe1 C4 149.27(14) 2 . ? C1 Fe1 C4 68.51(14) . . ? C1 Fe1 C4 116.20(14) 2 . ? C5 Fe1 C4 149.27(14) . 2 ? C5 Fe1 C4 40.42(13) 2 2 ? C1 Fe1 C4 116.20(14) . 2 ? C1 Fe1 C4 68.51(14) 2 2 ? C4 Fe1 C4 169.1(2) . 2 ? C5 Fe1 C3 169.94(13) . 2 ? C5 Fe1 C3 68.05(14) 2 2 ? C1 Fe1 C3 146.93(13) . 2 ? C1 Fe1 C3 68.25(14) 2 2 ? C4 Fe1 C3 130.52(15) . 2 ? C4 Fe1 C3 40.35(13) 2 2 ? C5 Fe1 C3 68.05(14) . . ? C5 Fe1 C3 169.94(13) 2 . ? C1 Fe1 C3 68.25(14) . . ? C1 Fe1 C3 146.93(13) 2 . ? C4 Fe1 C3 40.35(13) . . ? C4 Fe1 C3 130.52(15) 2 . ? C3 Fe1 C3 107.5(2) 2 . ? C5 Fe1 C2 68.40(14) . . ? C5 Fe1 C2 132.43(13) 2 . ? C1 Fe1 C2 40.79(13) . . ? C1 Fe1 C2 172.57(13) 2 . ? C4 Fe1 C2 67.80(14) . . ? C4 Fe1 C2 108.75(14) 2 . ? C3 Fe1 C2 114.51(14) 2 . ? C3 Fe1 C2 40.04(13) . . ? C5 Fe1 C2 132.43(13) . 2 ? C5 Fe1 C2 68.40(14) 2 2 ? C1 Fe1 C2 172.57(13) . 2 ? C1 Fe1 C2 40.79(13) 2 2 ? C4 Fe1 C2 108.75(14) . 2 ? C4 Fe1 C2 67.80(14) 2 2 ? C3 Fe1 C2 40.04(13) 2 2 ? C3 Fe1 C2 114.51(14) . 2 ? C2 Fe1 C2 145.5(2) . 2 ? C11 N1 C12 128.7(3) . . y C11 N1 H1 115.7 . . ? C12 N1 H1 115.7 . . ? C12 N2 C16 119.7(3) . . ? C12 N2 Pd1 121.9(2) . . ? C16 N2 Pd1 118.2(2) . . ? C2 C1 C5 107.0(3) . . ? C2 C1 C11 123.6(3) . . ? C5 C1 C11 129.3(3) . . ? C2 C1 Fe1 70.02(18) . . ? C5 C1 Fe1 69.39(17) . . ? C11 C1 Fe1 123.6(2) . . ? C3 C2 C1 108.4(3) . . ? C3 C2 Fe1 69.98(19) . . ? C1 C2 Fe1 69.19(17) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? Fe1 C2 H2 126.6 . . ? C2 C3 C4 108.4(3) . . ? C2 C3 Fe1 69.98(19) . . ? C4 C3 Fe1 69.60(19) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? Fe1 C3 H3 126.2 . . ? C5 C4 C3 108.3(3) . . ? C5 C4 Fe1 69.57(18) . . ? C3 C4 Fe1 70.05(18) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe1 C4 H4 126.1 . . ? C4 C5 C1 107.9(3) . . ? C4 C5 Fe1 70.02(19) . . ? C1 C5 Fe1 69.46(18) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Fe1 C5 H5 126.0 . . ? O1 C11 N1 123.0(3) . . y O1 C11 C1 122.1(3) . . y N1 C11 C1 115.0(3) . . ? N2 C12 N1 115.2(3) . . ? N2 C12 C13 121.2(3) . . ? N1 C12 C13 123.6(3) . . ? C14 C13 C12 118.4(3) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.6(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? N2 C16 C15 120.4(3) . . ? N2 C16 C17 117.8(3) . . ? C15 C16 C17 121.8(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? 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 C13 H13 O1 0.95 2.29 2.866(5) 118.4 . N1 H1 Cl1 0.88 2.81 3.483(3) 134.8 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.522 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.085