# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2274 #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_requested_journal 'Dalton' #============================================================================== #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Solid and Solution State Structure of Mononuclear Fe(III) Complexes Formed with Related Hexadentate and pentadentate Aminopyridyl ligands; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. ; loop_ _publ_author_name _publ_author_address 'Lars Duelund' ; Institut f\"ur Physik Medizinische Universit\"at L\"ubeck D-23538 L\"ubeck Germany ; 'Rita Hazell ' ; Department of Chemistry Aarhus University Langelandsgade 140 DK-8000 \%Arhus C Denmark ; 'Christine J. McKenzie ' ; Department of Chemistry University of Southern Denmark Main Campus Odense University DK-5230 Odense M Denmark ; 'Lars Preuss Nielsen ' ; Department of Chemistry University of Southern Denmark Main Campus Odense University DK-5230 Odense M Denmark ; 'Hans Toftlund' ; Department of Chemistry University of Southern Denmark Main Campus Odense University DK-5230 Odense M Denmark ; #============================================================================== # 4. TEXT _publ_section_references ; Allibon,J. (1995). MAD (Aarhus version). Institut Laue-Langevin, Grenoble, France. Altomare,A., Cascarano,G., Giacovazzo,C., Guagliardi,A., Burla,M.C., Polidori,G. & Camalli,M. (1994). J.Appl. Cryst. 27, 435. Burnett,M.N. & Johnson,C.K. (1996). ORTEP-III. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. Busing,W.R., Martin,K.O. & Levy,H.A. (1962). ORFLS. Report ORNL-TM-305. Oak Ridge National Laboratory, Tennessee, USA. Hazell,A. (1995). KRYSTAL, An integrated system of crystallographic programs. Aarhus University, Denmark. Pawley,G.S.,(1971) Advances in Structure Research by Diffraction Methods. 4, 1-64. ; data_tc #================================== # 5. CHEMICAL DATA _chemical_name_systematic ; N,N,N',N'-tetrakis(2-pyridylmethyl)ethylenediamine-Iron(III)- perchlorate ; _chemical_formula_sum 'C26H28Cl3Fe1N6O12' _chemical_formula_moiety 'C26H28N6Fe, 3ClO4' _chemical_formula_weight 778.78 #================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2-x,1/2+y,1/2-z' '-x,-y,-z' '1/2+x,1/2-y,1/2+z' _cell_length_a 9.816(2) _cell_length_b 18.486(2) _cell_length_c 18.156(2) _cell_angle_alpha 90 _cell_angle_beta 93.702(7) _cell_angle_gamma 90 _cell_volume 3288(1) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description box _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.57 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 0.77 _exptl_absorpt_correction_type 'none' #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Huber four-circle diffractometer' _diffrn_measurement_method \q/2\q _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 6 1 -5 0 _diffrn_reflns_number 109 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_reduction_process 6279 _reflns_number_total 5793 _reflns_number_observed 4371 _reflns_observed_criterion I>3\s(I) _computing_data_collection 'MAD (Allibon, 1995)' _computing_cell_refinement MAD _computing_data_reduction 'KRYSTAL (Hazell, 1995)' _computing_structure_solution ; SIR92 (Altomare et al., 1994) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; Least squares refinement with constraints according to Pawley (1971): Perchlorate groups identical with tetrahedral symmetry; two of the three sites disordered, occupancies refined; atomic displacement parameters for each ClO4 site modelled by the TLS approximation. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^ ; _refine_ls_hydrogen_treatment calculated _refine_ls_extinction_method none _refine_ls_number_reflns 4371 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.045 _refine_ls_wR_factor_obs 0.065 _refine_ls_goodness_of_fit_obs 2.27 _refine_ls_shift/esd_max 0.044 _refine_ls_shift/esd_mean 0.003 _refine_diff_density_max 0.66(6) _refine_diff_density_min -0.52(6) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy Fe 0.38744(5) 0.20990(3) 0.71837(3) 0.0321(3) Uij 1.0 N 1 0.5276(3) 0.2705(2) 0.6734(2) 0.043(2) Uij 1.0 N 2 0.5407(3) 0.1532(2) 0.7661(2) 0.045(2) Uij 1.0 C 1 0.6567(4) 0.2275(2) 0.6808(3) 0.059(3) Uij 1.0 C 2 0.6676(4) 0.1976(2) 0.7575(3) 0.062(3) Uij 1.0 C 3 0.5466(4) 0.3410(2) 0.7139(2) 0.054(2) Uij 1.0 C31 0.4726(4) 0.3428(2) 0.7823(2) 0.048(2) Uij 1.0 C32 0.4866(5) 0.3996(3) 0.8315(3) 0.071(3) Uij 1.0 C33 0.4094(6) 0.4004(3) 0.8919(3) 0.088(4) Uij 1.0 C34 0.3190(5) 0.3457(3) 0.9009(3) 0.079(3) Uij 1.0 C35 0.3099(4) 0.2904(2) 0.8515(2) 0.056(2) Uij 1.0 N 3 0.3881(3) 0.2870(2) 0.7934(2) 0.041(2) Uij 1.0 C 4 0.4738(5) 0.2836(2) 0.5956(2) 0.055(2) Uij 1.0 C41 0.3277(5) 0.3045(2) 0.6002(2) 0.052(2) Uij 1.0 C42 0.2581(6) 0.3535(3) 0.5541(3) 0.075(3) Uij 1.0 C43 0.1249(6) 0.3710(3) 0.5666(3) 0.088(4) Uij 1.0 C44 0.0646(5) 0.3399(3) 0.6240(3) 0.078(3) Uij 1.0 C45 0.1356(4) 0.2915(2) 0.6685(2) 0.054(2) Uij 1.0 N 4 0.2650(3) 0.2730(1) 0.6568(2) 0.041(2) Uij 1.0 C 5 0.5066(4) 0.1429(2) 0.8442(2) 0.056(2) Uij 1.0 C51 0.3592(4) 0.1198(2) 0.8407(2) 0.048(2) Uij 1.0 C52 0.3028(5) 0.0762(3) 0.8917(2) 0.069(3) Uij 1.0 C53 0.1655(5) 0.0590(3) 0.8828(3) 0.072(3) Uij 1.0 C54 0.0909(4) 0.0834(2) 0.8216(2) 0.060(3) Uij 1.0 C55 0.1517(4) 0.1263(2) 0.7715(2) 0.043(2) Uij 1.0 N 5 0.2831(3) 0.1460(1) 0.7812(1) 0.036(2) Uij 1.0 C 6 0.5519(4) 0.0805(2) 0.7295(3) 0.058(3) Uij 1.0 C61 0.4626(4) 0.0748(2) 0.6614(2) 0.049(2) Uij 1.0 C62 0.4614(5) 0.0134(2) 0.6181(3) 0.070(3) Uij 1.0 C63 0.3733(6) 0.0094(3) 0.5575(3) 0.075(3) Uij 1.0 C64 0.2882(5) 0.0661(3) 0.5393(2) 0.066(3) Uij 1.0 C65 0.2923(4) 0.1273(2) 0.5835(2) 0.049(2) Uij 1.0 N 6 0.3799(3) 0.1314(2) 0.6441(2) 0.040(2) Uij 1.0 Cl2 -0.11751(9) 0.09771(5) 0.60510(5) 0.0525(3) Uij 1.0 O21 -0.2498(2) 0.1036(1) 0.5704(1) 0.078(1) Uij 1.0 O22 -0.1263(2) 0.0713(1) 0.6775(1) 0.094(1) Uij 1.0 O23 -0.0392(2) 0.0496(1) 0.5648(1) 0.105(1) Uij 1.0 O24 -0.0547(2) 0.1664(1) 0.6077(2) 0.112(1) Uij 1.0 Cl1 0.7411(3) 0.4695(1) 0.5954(1) 0.048(1) Uij 0.687(3) O11 0.8569(5) 0.5001(2) 0.5653(3) 0.091(1) Uij 0.687(3) O12 0.7436(6) 0.4853(3) 0.6715(2) 0.109(2) Uij 0.687(3) O13 0.6217(5) 0.4987(3) 0.5596(3) 0.143(2) Uij 0.687(3) O14 0.7423(5) 0.3938(1) 0.5853(3) 0.094(2) Uij 0.687(3) Cl1 0.7505(7) 0.4788(3) 0.6046(3) 0.050(1) Uij 0.313(3) O1a 0.6389(9) 0.4430(6) 0.5677(6) 0.100(2) Uij 0.313(3) O1b 0.7933(15) 0.4399(6) 0.6688(6) 0.129(3) Uij 0.313(3) O1c 0.8591(11) 0.4832(6) 0.5575(7) 0.086(1) Uij 0.313(3) O1d 0.7106(12) 0.5492(3) 0.6243(7) 0.131(3) Uij 0.313(3) Cl3 -0.0953(4) 0.2967(2) 0.8841(2) 0.063(1) Uij 0.672(5) O31 0.0042(8) 0.3248(4) 0.9358(4) 0.110(2) Uij 0.672(5) O32 -0.0309(6) 0.2553(4) 0.8310(4) 0.125(3) Uij 0.672(5) O33 -0.1864(9) 0.2523(4) 0.9207(5) 0.152(3) Uij 0.672(5) O34 -0.1681(7) 0.3541(3) 0.8488(4) 0.158(3) Uij 0.672(5) Cl3 -0.0871(9) 0.2914(5) 0.8892(4) 0.064(1) Uij 0.328(5) O3a -0.0227(16) 0.2239(5) 0.9025(9) 0.169(4) Uij 0.328(5) O3b -0.2255(12) 0.2863(12) 0.9053(10) 0.144(4) Uij 0.328(5) O3c -0.0216(22) 0.3445(7) 0.9346(8) 0.114(2) Uij 0.328(5) O3d -0.0786(17) 0.3106(8) 0.8144(5) 0.121(3) Uij 0.328(5) H1a 0.733 0.258 0.673 0.072 Uiso 1.0 H1b 0.653 0.189 0.646 0.072 Uiso 1.0 H2a 0.673 0.236 0.793 0.074 Uiso 1.0 H2b 0.746 0.168 0.764 0.074 Uiso 1.0 H3a 0.514 0.379 0.682 0.066 Uiso 1.0 H3b 0.641 0.348 0.726 0.066 Uiso 1.0 H32 0.549 0.438 0.824 0.086 Uiso 1.0 H33 0.419 0.439 0.927 0.106 Uiso 1.0 H34 0.263 0.346 0.942 0.097 Uiso 1.0 H35 0.246 0.253 0.858 0.068 Uiso 1.0 H4a 0.481 0.241 0.567 0.067 Uiso 1.0 H4b 0.523 0.321 0.574 0.067 Uiso 1.0 H42 0.302 0.375 0.514 0.089 Uiso 1.0 H43 0.076 0.405 0.535 0.103 Uiso 1.0 H44 -0.027 0.352 0.633 0.093 Uiso 1.0 H45 0.093 0.270 0.709 0.065 Uiso 1.0 H5a 0.518 0.187 0.871 0.066 Uiso 1.0 H5b 0.563 0.107 0.867 0.066 Uiso 1.0 H52 0.357 0.058 0.933 0.082 Uiso 1.0 H53 0.124 0.031 0.919 0.087 Uiso 1.0 H54 -0.003 0.071 0.814 0.072 Uiso 1.0 H55 0.099 0.143 0.729 0.051 Uiso 1.0 H6a 0.527 0.044 0.763 0.070 Uiso 1.0 H6b 0.644 0.073 0.718 0.070 Uiso 1.0 H62 0.522 -0.026 0.631 0.085 Uiso 1.0 H63 0.371 -0.033 0.528 0.092 Uiso 1.0 H64 0.227 0.064 0.497 0.080 Uiso 1.0 H65 0.233 0.167 0.571 0.059 Uiso 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe 0.0279(3) 0.0322(3) 0.0362(3) -0.0016(2) 0.0040(2) -0.0029(2) N 1 0.038(2) 0.040(2) 0.053(2) -0.008(1) 0.015(1) -0.008(1) N 2 0.030(2) 0.049(2) 0.055(2) 0.003(1) -0.003(1) -0.002(1) C 1 0.033(2) 0.064(3) 0.083(3) -0.007(2) 0.019(2) -0.015(2) C 2 0.027(2) 0.064(3) 0.095(4) -0.003(2) 0.001(2) -0.008(2) C 3 0.055(2) 0.042(2) 0.067(3) -0.019(2) 0.012(2) -0.012(2) C31 0.042(2) 0.045(2) 0.057(2) -0.005(2) 0.006(2) -0.013(2) C32 0.065(3) 0.061(3) 0.089(3) -0.021(2) 0.016(3) -0.034(3) C33 0.095(4) 0.084(4) 0.087(4) -0.024(3) 0.025(3) -0.051(3) C34 0.076(3) 0.087(4) 0.079(3) -0.017(3) 0.031(3) -0.042(3) C35 0.056(2) 0.063(3) 0.052(2) -0.014(2) 0.019(2) -0.016(2) N 3 0.037(2) 0.041(2) 0.045(2) -0.005(1) 0.006(1) -0.011(1) C 4 0.071(3) 0.049(2) 0.047(2) -0.017(2) 0.021(2) 0.001(2) C41 0.067(3) 0.043(2) 0.047(2) -0.005(2) 0.007(2) 0.004(2) C42 0.104(4) 0.060(3) 0.058(3) -0.008(3) -0.001(3) 0.019(2) C43 0.090(4) 0.067(3) 0.102(4) 0.013(3) -0.023(3) 0.028(3) C44 0.059(3) 0.065(3) 0.110(4) 0.015(2) -0.007(3) 0.021(3) C45 0.043(2) 0.048(2) 0.071(3) 0.002(2) -0.001(2) 0.007(2) N 4 0.042(2) 0.035(2) 0.044(2) -0.002(1) 0.002(1) 0.003(1) C 5 0.044(2) 0.064(3) 0.057(2) 0.003(2) -0.013(2) 0.008(2) C51 0.047(2) 0.053(2) 0.041(2) 0.000(2) -0.005(2) 0.006(2) C52 0.071(3) 0.083(3) 0.051(3) -0.009(3) -0.007(2) 0.027(2) C53 0.079(3) 0.083(3) 0.057(3) -0.019(3) 0.013(3) 0.027(2) C54 0.051(2) 0.067(3) 0.063(3) -0.015(2) 0.011(2) 0.009(2) C55 0.036(2) 0.048(2) 0.044(2) -0.005(2) -0.001(2) 0.001(2) N 5 0.034(2) 0.037(2) 0.035(1) -0.001(1) 0.000(1) 0.002(1) C 6 0.044(2) 0.046(2) 0.086(3) 0.010(2) 0.008(2) -0.001(2) C61 0.038(2) 0.041(2) 0.069(3) -0.004(2) 0.016(2) -0.010(2) C62 0.062(3) 0.047(2) 0.103(4) -0.004(2) 0.024(3) -0.027(3) C63 0.074(3) 0.061(3) 0.094(4) -0.020(3) 0.034(3) -0.039(3) C64 0.071(3) 0.077(3) 0.053(3) -0.029(3) 0.015(2) -0.026(2) C65 0.052(2) 0.054(2) 0.042(2) -0.013(2) 0.002(2) -0.007(2) N 6 0.037(2) 0.038(2) 0.045(2) -0.006(1) 0.009(1) -0.008(1) Cl2 0.0422(2) 0.0608(3) 0.0550(3) 0.0046(2) 0.0071(2) -0.0109(2) O21 0.054(1) 0.114(1) 0.064(1) -0.001(1) -0.011(1) -0.018(1) O22 0.079(1) 0.147(1) 0.058(1) 0.022(1) 0.008(1) 0.011(1) O23 0.118(1) 0.107(1) 0.094(1) 0.053(1) 0.040(1) -0.010(1) O24 0.079(1) 0.076(1) 0.177(2) -0.020(1) -0.014(1) -0.006(1) Cl1 0.046(1) 0.053(1) 0.045(1) -0.005(1) 0.003(1) -0.003(1) O11 0.106(1) 0.067(1) 0.106(1) -0.031(1) 0.060(1) -0.014(1) O12 0.136(3) 0.145(2) 0.050(1) -0.068(2) 0.022(1) -0.023(1) O13 0.100(1) 0.185(3) 0.139(2) 0.076(2) -0.029(1) -0.009(3) O14 0.088(2) 0.054(1) 0.143(2) -0.023(1) 0.033(2) -0.014(1) Cl1 0.052(1) 0.054(1) 0.046(1) -0.010(1) 0.007(1) -0.004(1) O1a 0.046(1) 0.148(2) 0.103(2) -0.006(1) -0.010(1) -0.054(2) O1b 0.150(4) 0.161(3) 0.070(1) -0.034(3) -0.029(2) 0.047(1) O1c 0.091(1) 0.070(1) 0.104(2) -0.024(1) 0.053(1) -0.015(1) O1d 0.166(4) 0.073(1) 0.164(4) -0.002(2) 0.084(3) -0.039(1) Cl3 0.055(1) 0.073(1) 0.061(1) -0.011(1) 0.002(1) -0.010(1) O31 0.075(2) 0.145(3) 0.107(1) -0.023(2) -0.023(1) -0.033(1) O32 0.113(3) 0.131(3) 0.134(3) -0.014(2) 0.044(2) -0.062(2) O33 0.149(3) 0.210(4) 0.100(2) -0.106(2) 0.038(2) -0.010(2) O34 0.149(3) 0.134(3) 0.183(4) 0.046(2) -0.058(2) 0.009(2) Cl3 0.057(1) 0.072(1) 0.062(1) -0.013(1) 0.002(1) -0.008(1) O3a 0.198(4) 0.084(1) 0.221(5) 0.024(2) -0.024(4) 0.024(3) O3b 0.071(1) 0.248(5) 0.116(4) -0.057(2) 0.030(2) -0.069(3) O3c 0.087(2) 0.131(2) 0.120(2) -0.027(2) -0.013(1) -0.055(2) O3d 0.139(4) 0.154(4) 0.070(1) -0.041(3) 0.011(1) 0.012(2) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe N 3 1.970(3) Fe N 4 1.971(3) Fe N 5 1.974(3) Fe N 6 1.979(3) Fe N 2 1.986(3) Fe N 1 1.990(3) N 1 C 1 1.494(5) N 1 C 4 1.495(5) N 1 C 3 1.503(5) N 2 C 5 1.490(5) N 2 C 6 1.506(5) N 2 C 2 1.507(5) C 1 C 2 1.496(7) C 3 C31 1.478(5) C31 N 3 1.348(5) C31 C32 1.381(6) C32 C33 1.372(7) C33 C34 1.363(7) C34 C35 1.360(6) C35 N 3 1.346(5) C 4 C41 1.493(6) C41 N 4 1.362(5) C41 C42 1.383(6) C42 C43 1.379(8) C43 C44 1.359(8) C44 C45 1.367(6) C45 N 4 1.345(5) C 5 C51 1.506(6) C51 N 5 1.362(4) C51 C52 1.370(6) C52 C53 1.384(7) C53 C54 1.367(6) C54 C55 1.372(5) C55 N 5 1.341(4) C 6 C61 1.473(6) C61 N 6 1.350(5) C61 C62 1.380(6) C62 C63 1.357(7) C63 C64 1.368(8) C64 C65 1.386(6) C65 N 6 1.354(5) Cl2 O21 1.411(1) Cl2 O22 1.411(1) Cl2 O23 1.411(1) Cl2 O24 1.411(1) Cl1 O11 1.411(1) Cl1 O12 1.411(1) Cl1 O13 1.411(1) Cl1 O14 1.411(1) Cl1 O1a 1.411(1) Cl1 O1b 1.411(1) Cl1 O1c 1.411(1) Cl1 O1d 1.411(1) Cl3 O31 1.411(1) Cl3 O32 1.411(1) Cl3 O33 1.411(1) Cl3 O34 1.411(1) Cl3 O3a 1.411(1) Cl3 O3b 1.411(1) Cl3 O3c 1.411(1) Cl3 O3d 1.411(1) C 1 H1a 0.950 C 1 H1b 0.950 C 2 H2a 0.950 C 2 H2b 0.950 C 3 H3a 0.950 C 3 H3b 0.950 C32 H32 0.950 C33 H33 0.950 C34 H34 0.950 C35 H35 0.950 C 4 H4a 0.950 C 4 H4b 0.950 C42 H42 0.950 C43 H43 0.950 C44 H44 0.950 C45 H45 0.950 C 5 H5a 0.950 C 5 H5b 0.950 C52 H52 0.950 C53 H53 0.950 C54 H54 0.950 C55 H55 0.950 C 6 H6a 0.950 C 6 H6b 0.950 C62 H62 0.950 C63 H63 0.950 C64 H64 0.950 C65 H65 0.950 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N 3 Fe N 4 86.5(1) N 3 Fe N 5 90.7(1) N 3 Fe N 6 177.8(1) N 2 Fe N 3 96.4(1) N 1 Fe N 3 84.5(1) N 4 Fe N 5 111.2(1) N 4 Fe N 6 93.0(1) N 2 Fe N 4 167.8(1) N 1 Fe N 4 81.2(1) N 5 Fe N 6 87.5(1) N 2 Fe N 5 80.7(1) N 1 Fe N 5 166.5(1) N 2 Fe N 6 84.5(1) N 1 Fe N 6 97.5(1) N 1 Fe N 2 87.2(1) C 1 N 1 C 4 114.6(3) C 1 N 1 C 3 109.9(3) Fe N 1 C 1 105.6(2) C 3 N 1 C 4 110.3(3) Fe N 1 C 4 105.4(2) Fe N 1 C 3 110.8(2) C 5 N 2 C 6 109.5(3) C 2 N 2 C 5 114.0(3) Fe N 2 C 5 105.8(2) C 2 N 2 C 6 110.8(3) Fe N 2 C 6 110.7(2) Fe N 2 C 2 106.0(2) N 1 C 1 C 2 106.8(3) N 2 C 2 C 1 106.7(3) N 1 C 3 C31 112.1(3) C32 C31 N 3 121.5(4) C 3 C31 N 3 116.8(3) C 3 C31 C32 121.8(4) C31 C32 C33 119.3(4) C32 C33 C34 119.1(4) C33 C34 C35 119.6(4) C34 C35 N 3 122.5(4) C31 N 3 C35 118.0(3) Fe N 3 C35 126.8(3) Fe N 3 C31 115.1(2) N 1 C 4 C41 105.8(3) C42 C41 N 4 120.4(4) C 4 C41 N 4 114.4(3) C 4 C41 C42 125.1(4) C41 C42 C43 119.3(5) C42 C43 C44 119.5(4) C43 C44 C45 120.0(5) C44 C45 N 4 121.5(4) C41 N 4 C45 119.2(3) Fe N 4 C45 127.4(3) Fe N 4 C41 113.1(3) N 2 C 5 C51 105.7(3) C52 C51 N 5 121.4(4) C 5 C51 N 5 114.1(3) C 5 C51 C52 124.5(4) C51 C52 C53 119.2(4) C52 C53 C54 119.1(4) C53 C54 C55 119.7(4) C54 C55 N 5 121.8(3) C51 N 5 C55 118.7(3) Fe N 5 C55 128.1(2) Fe N 5 C51 113.1(2) N 2 C 6 C61 112.3(3) C62 C61 N 6 121.5(4) C 6 C61 N 6 117.1(3) C 6 C61 C62 121.4(4) C61 C62 C63 119.3(5) C62 C63 C64 120.1(4) C63 C64 C65 119.5(4) C64 C65 N 6 120.6(4) C61 N 6 C65 119.1(3) Fe N 6 C61 114.5(2) Fe N 6 C65 126.1(3) O21 Cl2 O22 109.47 O21 Cl2 O23 109.47 O21 Cl2 O24 109.47 O22 Cl2 O23 109.47 O22 Cl2 O24 109.47 O23 Cl2 O24 109.47 O11 Cl1 O12 109.47 O11 Cl1 O13 109.47 O11 Cl1 O14 109.47 O12 Cl1 O13 109.47 O12 Cl1 O14 109.47 O13 Cl1 O14 109.47 O1c Cl1 O1a 109.47 O1c Cl1 O1b 109.47 O1c Cl1 O1d 109.47 O1a Cl1 O1b 109.47 O1a Cl1 O1d 109.47 O1b Cl1 O1d 109.47 O31 Cl3 O32 109.47 O31 Cl3 O33 109.47 O31 Cl3 O34 109.47 O32 Cl3 O33 109.47 O32 Cl3 O34 109.47 O33 Cl3 O34 109.47 O3c Cl3 O3a 109.47 O3c Cl3 O3b 109.47 O3c Cl3 O3d 109.47 O3a Cl3 O3b 109.47 O3a Cl3 O3d 109.47 O3b Cl3 O3d 109.47 H1a C 1 H1b 109.5 N 1 C 1 H1a 110.1 C 2 C 1 H1a 110.1 N 1 C 1 H1b 110.1 C 2 C 1 H1b 110.1 H2a C 2 H2b 109.5 C 1 C 2 H2a 110.2 N 2 C 2 H2a 110.2 C 1 C 2 H2b 110.2 N 2 C 2 H2b 110.2 H3a C 3 H3b 109.5 C31 C 3 H3a 108.8 N 1 C 3 H3a 108.8 C31 C 3 H3b 108.8 N 1 C 3 H3b 108.8 C33 C32 H32 120.4 C31 C32 H32 120.4 C34 C33 H33 120.5 C32 C33 H33 120.5 C35 C34 H34 120.2 C33 C34 H34 120.2 N 3 C35 H35 118.8 C34 C35 H35 118.8 H4a C 4 H4b 109.5 C41 C 4 H4a 110.4 N 1 C 4 H4a 110.4 C41 C 4 H4b 110.4 N 1 C 4 H4b 110.4 C43 C42 H42 120.3 C41 C42 H42 120.3 C44 C43 H43 120.3 C42 C43 H43 120.3 C43 C44 H44 120.0 C45 C44 H44 120.0 N 4 C45 H45 119.2 C44 C45 H45 119.2 H5a C 5 H5b 109.5 N 2 C 5 H5a 110.4 C51 C 5 H5a 110.4 N 2 C 5 H5b 110.4 C51 C 5 H5b 110.4 C51 C52 H52 120.4 C53 C52 H52 120.4 C54 C53 H53 120.5 C52 C53 H53 120.5 C53 C54 H54 120.1 C55 C54 H54 120.1 N 5 C55 H55 119.1 C54 C55 H55 119.1 H6a C 6 H6b 109.5 C61 C 6 H6a 108.8 N 2 C 6 H6a 108.8 C61 C 6 H6b 108.8 N 2 C 6 H6b 108.8 C63 C62 H62 120.4 C61 C62 H62 120.4 C62 C63 H63 120.0 C64 C63 H63 120.0 C63 C64 H64 120.3 C65 C64 H64 120.3 N 6 C65 H65 119.7 C64 C65 H65 119.7