# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email gilles.gasser@aci.unizh.ch _publ_contact_author_name 'G. Gasser' loop_ _publ_author_name 'G .Gasser' 'C. Mari' 'M. Burkart' 'S. J. Green' 'J. Ribas' 'H.Stoeckli-Evans.J. H.R. Tucker' data_HL1 _database_code_depnum_ccdc_archive 'CCDC 870327' #TrackingRef 'web_deposit_cif_file_0_HelenStoeckli-Evans_1331020702.1-HL1.cif' _audit_update_record ; 2011-06-03 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H17 Fe N3 O4' _chemical_formula_sum 'C23 H17 Fe N3 O4' _chemical_formula_weight 455.25 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 11.6164(11) _cell_length_b 7.8216(6) _cell_length_c 22.0190(19) _cell_angle_alpha 90.00 _cell_angle_beta 100.544(11) _cell_angle_gamma 90.00 _cell_volume 1966.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6115 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 25.94 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2009)' _exptl_special_details ? _diffrn_ambient_temperature 153(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 'STOE IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13597 _diffrn_reflns_av_R_equivalents 0.0894 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3473 _reflns_number_gt 2164 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'EXPOSE (Stoe & Cie, 2000)' _computing_cell_refinement 'CELL (Stoe & Cie, 2000)' _computing_data_reduction 'INTEGRATE (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL-97 _refine_special_details ; In the Cp ring (C1-C5), atoms C4 and C5 have distorted displacement parameters. Attemps to split the atoms in this group were not very succesful. Only three of the atoms in the ring could be located and refinemt of the occupancies of the two fragments gave a ratio of 95:5%. It was decided not to continue with such a small fraction. The NH H-atom was located in difference electron-density map and was freely refined. The C-bound H-atoms were included in calculated positions and treated as riding atoms: C-H = 0.95 \%A for CH(aromatic), with U~iso~(H) = 1.2U~eq~(parent C-atom). ; _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^)+(0.0511P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3473 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.901 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe Uani 0.74098(4) -0.00729(7) -0.13745(2) 1.000 0.0263(2) d . . . O1 O Uani 0.6636(2) 0.1244(3) 0.01977(11) 1.000 0.0327(8) d . . . O2 O Uani 0.8526(2) 0.1624(3) 0.01094(9) 1.000 0.0248(8) d . . . O3 O Uani 0.8767(2) -0.0279(3) 0.11900(10) 1.000 0.0333(8) d . . . O4 O Uani 0.8964(2) -0.1580(3) 0.24248(11) 1.000 0.0386(9) d . . . N1 N Uani 0.8898(2) 0.4128(3) 0.15462(12) 1.000 0.0240(9) d . . . N2 N Uani 0.8689(3) 0.1197(4) 0.20832(12) 1.000 0.0282(10) d . . . N3 N Uani 0.8751(2) 0.2303(4) 0.32246(13) 1.000 0.0285(10) d . . . C1 C Uani 0.7944(5) 0.2353(6) -0.15060(19) 1.000 0.0567(18) d . . . C2 C Uani 0.6783(5) 0.2348(6) -0.15839(19) 1.000 0.0523(19) d . . . C3 C Uani 0.6314(4) 0.1256(5) -0.20474(18) 1.000 0.0448(14) d . . . C4 C Uani 0.7241(6) 0.0495(6) -0.22889(17) 1.000 0.072(2) d . . . C5 C Uani 0.8312(4) 0.1254(7) -0.1923(3) 1.000 0.068(2) d . . . C6 C Uani 0.6486(3) -0.1395(5) -0.08185(14) 1.000 0.0281(11) d . . . C7 C Uani 0.6881(3) -0.2530(5) -0.12348(16) 1.000 0.0346(12) d . . . C8 C Uani 0.8114(3) -0.2456(5) -0.11487(15) 1.000 0.0335(12) d . . . C9 C Uani 0.8516(3) -0.1229(4) -0.06746(14) 1.000 0.0265(11) d . . . C10 C Uani 0.7508(3) -0.0578(4) -0.04663(14) 1.000 0.0236(10) d . . . C11 C Uani 0.7460(3) 0.0811(4) -0.00253(14) 1.000 0.0231(11) d . . . C12 C Uani 0.8639(3) 0.3000(4) 0.05243(14) 1.000 0.0230(11) d . . . C13 C Uani 0.8712(3) 0.4621(4) 0.02848(15) 1.000 0.0274(11) d . . . C14 C Uani 0.8894(3) 0.5985(4) 0.06860(16) 1.000 0.0308(11) d . . . C15 C Uani 0.8972(3) 0.5691(4) 0.13141(16) 1.000 0.0269(11) d . . . C16 C Uani 0.8745(3) 0.2787(4) 0.11542(14) 1.000 0.0222(10) d . . . C17 C Uani 0.8728(3) 0.1064(4) 0.14657(14) 1.000 0.0239(11) d . . . C18 C Uani 0.8826(3) -0.0073(5) 0.25254(14) 1.000 0.0269(10) d . . . C19 C Uani 0.8841(3) 0.0593(4) 0.31630(15) 1.000 0.0245(11) d . . . C20 C Uani 0.8983(3) -0.0540(5) 0.36611(15) 1.000 0.0300(11) d . . . C21 C Uani 0.9048(3) 0.0106(6) 0.42455(15) 1.000 0.0388(13) d . . . C22 C Uani 0.8975(3) 0.1881(6) 0.43162(17) 1.000 0.0409(14) d . . . C23 C Uani 0.8815(3) 0.2903(5) 0.37953(17) 1.000 0.0359(12) d . . . H1 H Uiso 0.84480 0.30150 -0.12070 1.000 0.0680 d R . . H2 H Uiso 0.63390 0.30130 -0.13490 1.000 0.0620 d R . . H2N H Uiso 0.868(3) 0.226(5) 0.2230(16) 1.000 0.036(11) d . . . H3 H Uiso 0.55030 0.10430 -0.21850 1.000 0.0540 d R . . H4 H Uiso 0.71860 -0.03200 -0.26130 1.000 0.0860 d R . . H5 H Uiso 0.90970 0.10320 -0.19670 1.000 0.0820 d R . . H6 H Uiso 0.56960 -0.12050 -0.07780 1.000 0.0340 d R . . H7 H Uiso 0.63940 -0.32320 -0.15270 1.000 0.0420 d R . . H8 H Uiso 0.85950 -0.31080 -0.13670 1.000 0.0400 d R . . H9 H Uiso 0.93060 -0.09080 -0.05270 1.000 0.0320 d R . . H13 H Uiso 0.86370 0.47910 -0.01480 1.000 0.0330 c R . . H14 H Uiso 0.89670 0.71110 0.05350 1.000 0.0370 c R . . H15 H Uiso 0.90810 0.66380 0.15890 1.000 0.0320 c R . . H20 H Uiso 0.90330 -0.17360 0.35960 1.000 0.0360 c R . . H21 H Uiso 0.91390 -0.06320 0.45940 1.000 0.0470 c R . . H22 H Uiso 0.90350 0.23740 0.47150 1.000 0.0490 c R . . H23 H Uiso 0.87460 0.41020 0.38480 1.000 0.0430 c 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 Fe1 0.0283(3) 0.0300(3) 0.0202(2) 0.0010(2) 0.0032(2) -0.0011(3) O1 0.0324(15) 0.0304(14) 0.0365(14) -0.0064(11) 0.0099(11) -0.0020(12) O2 0.0295(14) 0.0201(13) 0.0248(12) -0.0085(10) 0.0050(9) -0.0014(11) O3 0.0533(16) 0.0158(14) 0.0306(13) -0.0037(10) 0.0074(11) 0.0002(12) O4 0.0618(19) 0.0201(15) 0.0339(14) -0.0012(11) 0.0091(12) 0.0013(13) N1 0.0269(16) 0.0169(15) 0.0271(15) -0.0041(12) 0.0017(12) -0.0012(13) N2 0.044(2) 0.0166(16) 0.0253(16) -0.0028(13) 0.0097(13) -0.0003(15) N3 0.0255(17) 0.0280(18) 0.0331(16) -0.0061(13) 0.0085(12) -0.0027(14) C1 0.073(4) 0.058(3) 0.035(2) 0.018(2) -0.001(2) -0.016(3) C2 0.078(4) 0.035(3) 0.047(3) 0.009(2) 0.020(2) -0.003(3) C3 0.041(2) 0.047(3) 0.043(2) 0.014(2) -0.0009(19) 0.005(2) C4 0.163(6) 0.040(3) 0.0133(19) 0.0004(17) 0.020(3) 0.016(3) C5 0.043(3) 0.090(4) 0.081(4) 0.060(3) 0.035(3) 0.028(3) C6 0.033(2) 0.027(2) 0.0250(17) -0.0008(15) 0.0069(14) -0.0066(17) C7 0.042(2) 0.028(2) 0.033(2) -0.0080(16) 0.0047(17) -0.0093(19) C8 0.044(2) 0.023(2) 0.033(2) -0.0078(16) 0.0058(17) 0.0027(18) C9 0.032(2) 0.0225(19) 0.0236(17) -0.0022(14) 0.0016(14) -0.0001(16) C10 0.031(2) 0.0159(17) 0.0231(17) 0.0018(13) 0.0030(14) -0.0004(14) C11 0.028(2) 0.0205(18) 0.0194(17) 0.0049(14) 0.0006(14) 0.0037(16) C12 0.0239(19) 0.0193(18) 0.0260(18) -0.0053(14) 0.0050(14) -0.0015(15) C13 0.032(2) 0.023(2) 0.0270(17) 0.0037(14) 0.0051(14) 0.0018(16) C14 0.037(2) 0.0170(19) 0.039(2) 0.0015(16) 0.0088(16) -0.0009(17) C15 0.024(2) 0.0176(18) 0.038(2) -0.0064(15) 0.0030(15) -0.0006(15) C16 0.0216(18) 0.0148(18) 0.0301(18) -0.0038(14) 0.0044(14) 0.0027(14) C17 0.0260(19) 0.0196(19) 0.0252(17) -0.0017(14) 0.0022(14) 0.0000(16) C18 0.0283(17) 0.0238(19) 0.0288(17) 0.0023(17) 0.0056(13) -0.0031(19) C19 0.0180(17) 0.027(2) 0.0286(19) -0.0027(14) 0.0047(13) -0.0026(14) C20 0.0264(19) 0.033(2) 0.031(2) 0.0029(15) 0.0065(15) -0.0003(16) C21 0.034(2) 0.055(3) 0.0276(18) 0.002(2) 0.0059(14) 0.001(2) C22 0.041(2) 0.057(3) 0.0263(19) -0.0094(18) 0.0101(16) -0.002(2) C23 0.031(2) 0.037(2) 0.042(2) -0.0144(18) 0.0126(17) -0.0018(18) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 2.034(5) . . yes Fe1 C2 2.051(5) . . yes Fe1 C3 2.051(4) . . yes Fe1 C4 2.036(4) . . yes Fe1 C5 2.024(6) . . yes Fe1 C6 2.050(4) . . yes Fe1 C7 2.058(4) . . yes Fe1 C8 2.060(4) . . yes Fe1 C9 2.030(3) . . yes Fe1 C10 2.021(3) . . yes O1 C11 1.202(4) . . yes O2 C11 1.375(4) . . yes O2 C12 1.402(4) . . yes O3 C17 1.218(4) . . yes O4 C18 1.215(5) . . yes N1 C15 1.334(4) . . yes N1 C16 1.349(4) . . yes N2 C17 1.373(4) . . yes N2 C18 1.380(5) . . yes N3 C19 1.350(4) . . yes N3 C23 1.331(5) . . yes N2 H2N 0.89(4) . . no C1 C5 1.381(7) . . no C1 C2 1.328(8) . . no C2 C3 1.365(6) . . no C3 C4 1.416(8) . . no C4 C5 1.477(8) . . no C6 C7 1.412(5) . . no C6 C10 1.443(5) . . no C7 C8 1.411(5) . . no C8 C9 1.432(5) . . no C9 C10 1.427(5) . . no C10 C11 1.465(4) . . no C12 C16 1.380(4) . . no C12 C13 1.382(4) . . no C13 C14 1.377(5) . . no C14 C15 1.389(5) . . no C16 C17 1.514(4) . . no C18 C19 1.495(5) . . no C19 C20 1.396(5) . . no C20 C21 1.372(5) . . no C21 C22 1.401(7) . . no C22 C23 1.382(6) . . no C1 H1 0.9500 . . no C2 H2 0.9500 . . no C3 H3 0.9500 . . no C4 H4 0.9500 . . no C5 H5 0.9500 . . no C6 H6 0.9500 . . no C7 H7 0.9500 . . no C8 H8 0.9500 . . no C9 H9 0.9500 . . no C13 H13 0.9500 . . no C14 H14 0.9500 . . no C15 H15 0.9500 . . no C20 H20 0.9500 . . no C21 H21 0.9500 . . no C22 H22 0.9500 . . no C23 H23 0.9500 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C2 38.0(2) . . . yes C1 Fe1 C3 65.76(18) . . . yes C1 Fe1 C4 68.43(18) . . . yes C1 Fe1 C5 39.8(2) . . . yes C1 Fe1 C6 139.70(17) . . . yes C1 Fe1 C7 179.49(18) . . . yes C1 Fe1 C8 139.53(19) . . . yes C1 Fe1 C9 110.89(17) . . . yes C1 Fe1 C10 111.09(15) . . . yes C2 Fe1 C3 38.89(17) . . . yes C2 Fe1 C4 67.06(19) . . . yes C2 Fe1 C5 66.0(2) . . . yes C2 Fe1 C6 113.39(19) . . . yes C2 Fe1 C7 142.42(19) . . . yes C2 Fe1 C8 177.36(19) . . . yes C2 Fe1 C9 137.02(16) . . . yes C2 Fe1 C10 110.88(15) . . . yes C3 Fe1 C4 40.6(2) . . . yes C3 Fe1 C5 68.3(2) . . . yes C3 Fe1 C6 111.33(16) . . . yes C3 Fe1 C7 114.74(15) . . . yes C3 Fe1 C8 143.10(15) . . . yes C3 Fe1 C9 175.91(14) . . . yes C3 Fe1 C10 136.81(16) . . . yes C4 Fe1 C5 42.7(2) . . . yes C4 Fe1 C6 137.3(2) . . . yes C4 Fe1 C7 111.98(17) . . . yes C4 Fe1 C8 113.47(17) . . . yes C4 Fe1 C9 141.4(2) . . . yes C4 Fe1 C10 177.4(2) . . . yes C5 Fe1 C6 179.42(19) . . . yes C5 Fe1 C7 140.30(19) . . . yes C5 Fe1 C8 112.45(18) . . . yes C5 Fe1 C9 110.89(18) . . . yes C5 Fe1 C10 138.5(2) . . . yes C6 Fe1 C7 40.20(14) . . . yes C6 Fe1 C8 68.13(14) . . . yes C6 Fe1 C9 69.49(14) . . . yes C6 Fe1 C10 41.52(13) . . . yes C7 Fe1 C8 40.09(14) . . . yes C7 Fe1 C9 68.61(14) . . . yes C7 Fe1 C10 68.52(13) . . . yes C8 Fe1 C9 40.99(13) . . . yes C8 Fe1 C10 68.67(13) . . . yes C9 Fe1 C10 41.26(14) . . . yes C11 O2 C12 118.0(3) . . . yes C15 N1 C16 118.5(3) . . . yes C17 N2 C18 128.6(3) . . . yes C19 N3 C23 116.9(3) . . . yes C18 N2 H2N 115(2) . . . no C17 N2 H2N 116(2) . . . no Fe1 C1 C5 69.7(3) . . . yes Fe1 C1 C2 71.7(3) . . . yes C2 C1 C5 110.1(4) . . . no Fe1 C2 C3 70.6(3) . . . yes Fe1 C2 C1 70.3(3) . . . yes C1 C2 C3 110.8(4) . . . no Fe1 C3 C4 69.2(2) . . . yes C2 C3 C4 108.5(4) . . . no Fe1 C3 C2 70.6(3) . . . yes C3 C4 C5 104.4(4) . . . no Fe1 C4 C3 70.3(2) . . . yes Fe1 C4 C5 68.2(3) . . . yes C1 C5 C4 106.3(4) . . . no Fe1 C5 C4 69.1(3) . . . yes Fe1 C5 C1 70.5(3) . . . yes Fe1 C6 C10 68.18(19) . . . yes Fe1 C6 C7 70.2(2) . . . yes C7 C6 C10 107.1(3) . . . no Fe1 C7 C8 70.0(2) . . . yes Fe1 C7 C6 69.6(2) . . . yes C6 C7 C8 109.2(3) . . . no Fe1 C8 C9 68.4(2) . . . yes C7 C8 C9 108.2(3) . . . no Fe1 C8 C7 69.9(2) . . . yes C8 C9 C10 107.2(3) . . . no Fe1 C9 C8 70.6(2) . . . yes Fe1 C9 C10 69.05(18) . . . yes Fe1 C10 C11 120.6(2) . . . yes C6 C10 C9 108.2(3) . . . no C6 C10 C11 123.9(3) . . . no C9 C10 C11 127.6(3) . . . no Fe1 C10 C6 70.30(18) . . . yes Fe1 C10 C9 69.69(18) . . . yes O2 C11 C10 110.1(3) . . . yes O1 C11 O2 122.3(3) . . . yes O1 C11 C10 127.6(3) . . . yes C13 C12 C16 119.6(3) . . . no O2 C12 C13 117.4(3) . . . yes O2 C12 C16 122.9(3) . . . yes C12 C13 C14 118.6(3) . . . no C13 C14 C15 119.0(3) . . . no N1 C15 C14 122.4(3) . . . yes N1 C16 C12 121.8(3) . . . yes C12 C16 C17 123.8(3) . . . no N1 C16 C17 114.4(3) . . . yes O3 C17 C16 122.5(3) . . . yes N2 C17 C16 112.8(3) . . . yes O3 C17 N2 124.8(3) . . . yes N2 C18 C19 113.1(3) . . . yes O4 C18 N2 124.9(3) . . . yes O4 C18 C19 122.0(3) . . . yes C18 C19 C20 119.7(3) . . . no N3 C19 C18 116.9(3) . . . yes N3 C19 C20 123.4(3) . . . yes C19 C20 C21 118.8(4) . . . no C20 C21 C22 118.4(4) . . . no C21 C22 C23 118.8(3) . . . no N3 C23 C22 123.7(4) . . . yes Fe1 C1 H1 125.00 . . . no C2 C1 H1 125.00 . . . no C5 C1 H1 125.00 . . . no Fe1 C2 H2 126.00 . . . no C1 C2 H2 125.00 . . . no C3 C2 H2 125.00 . . . no Fe1 C3 H3 126.00 . . . no C2 C3 H3 126.00 . . . no C4 C3 H3 126.00 . . . no Fe1 C4 H4 125.00 . . . no C3 C4 H4 128.00 . . . no C5 C4 H4 128.00 . . . no Fe1 C5 H5 125.00 . . . no C1 C5 H5 127.00 . . . no C4 C5 H5 127.00 . . . no Fe1 C6 H6 127.00 . . . no C7 C6 H6 126.00 . . . no C10 C6 H6 126.00 . . . no Fe1 C7 H7 127.00 . . . no C6 C7 H7 125.00 . . . no C8 C7 H7 125.00 . . . no Fe1 C8 H8 127.00 . . . no C7 C8 H8 126.00 . . . no C9 C8 H8 126.00 . . . no Fe1 C9 H9 125.00 . . . no C8 C9 H9 126.00 . . . no C10 C9 H9 126.00 . . . no C12 C13 H13 121.00 . . . no C14 C13 H13 121.00 . . . no C13 C14 H14 120.00 . . . no C15 C14 H14 121.00 . . . no N1 C15 H15 119.00 . . . no C14 C15 H15 119.00 . . . no C19 C20 H20 121.00 . . . no C21 C20 H20 121.00 . . . no C20 C21 H21 121.00 . . . no C22 C21 H21 121.00 . . . no C21 C22 H22 121.00 . . . no C23 C22 H22 121.00 . . . no N3 C23 H23 118.00 . . . no C22 C23 H23 118.00 . . . no 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 C2 Fe1 C1 C5 -120.4(4) . . . . no C3 Fe1 C1 C2 35.8(3) . . . . no C3 Fe1 C1 C5 -84.6(3) . . . . no C4 Fe1 C1 C2 80.0(3) . . . . no C4 Fe1 C1 C5 -40.5(3) . . . . no C5 Fe1 C1 C2 120.4(4) . . . . no C6 Fe1 C1 C2 -59.1(4) . . . . no C6 Fe1 C1 C5 -179.5(3) . . . . no C8 Fe1 C1 C2 -178.7(2) . . . . no C8 Fe1 C1 C5 60.8(4) . . . . no C9 Fe1 C1 C2 -141.6(2) . . . . no C9 Fe1 C1 C5 97.9(3) . . . . no C10 Fe1 C1 C2 -97.3(3) . . . . no C10 Fe1 C1 C5 142.3(3) . . . . no C1 Fe1 C2 C3 121.8(4) . . . . no C3 Fe1 C2 C1 -121.8(4) . . . . no C4 Fe1 C2 C1 -83.9(3) . . . . no C4 Fe1 C2 C3 37.9(3) . . . . no C5 Fe1 C2 C1 -37.2(3) . . . . no C5 Fe1 C2 C3 84.6(3) . . . . no C6 Fe1 C2 C1 142.8(2) . . . . no C6 Fe1 C2 C3 -95.4(3) . . . . no C7 Fe1 C2 C1 179.4(3) . . . . no C7 Fe1 C2 C3 -58.8(4) . . . . no C9 Fe1 C2 C1 58.3(4) . . . . no C9 Fe1 C2 C3 -179.9(3) . . . . no C10 Fe1 C2 C1 97.9(3) . . . . no C10 Fe1 C2 C3 -140.4(3) . . . . no C1 Fe1 C3 C2 -35.0(3) . . . . no C1 Fe1 C3 C4 84.6(3) . . . . no C2 Fe1 C3 C4 119.6(4) . . . . no C4 Fe1 C3 C2 -119.6(4) . . . . no C5 Fe1 C3 C2 -78.3(3) . . . . no C5 Fe1 C3 C4 41.3(3) . . . . no C6 Fe1 C3 C2 101.2(3) . . . . no C6 Fe1 C3 C4 -139.2(3) . . . . no C7 Fe1 C3 C2 145.0(3) . . . . no C7 Fe1 C3 C4 -95.5(3) . . . . no C8 Fe1 C3 C2 -177.2(3) . . . . no C8 Fe1 C3 C4 -57.6(4) . . . . no C10 Fe1 C3 C2 60.6(4) . . . . no C10 Fe1 C3 C4 -179.8(3) . . . . no C1 Fe1 C4 C3 -77.5(3) . . . . no C1 Fe1 C4 C5 37.8(3) . . . . no C2 Fe1 C4 C3 -36.4(3) . . . . no C2 Fe1 C4 C5 78.9(3) . . . . no C3 Fe1 C4 C5 115.3(4) . . . . no C5 Fe1 C4 C3 -115.3(4) . . . . no C6 Fe1 C4 C3 63.8(3) . . . . no C6 Fe1 C4 C5 179.2(3) . . . . no C7 Fe1 C4 C3 102.9(3) . . . . no C7 Fe1 C4 C5 -141.8(3) . . . . no C8 Fe1 C4 C3 146.5(2) . . . . no C8 Fe1 C4 C5 -98.2(3) . . . . no C9 Fe1 C4 C3 -174.3(2) . . . . no C9 Fe1 C4 C5 -59.0(4) . . . . no C1 Fe1 C5 C4 -117.0(4) . . . . no C2 Fe1 C5 C1 35.5(3) . . . . no C2 Fe1 C5 C4 -81.5(3) . . . . no C3 Fe1 C5 C1 77.8(3) . . . . no C3 Fe1 C5 C4 -39.3(3) . . . . no C4 Fe1 C5 C1 117.0(4) . . . . no C7 Fe1 C5 C1 -179.2(3) . . . . no C7 Fe1 C5 C4 63.8(4) . . . . no C8 Fe1 C5 C1 -142.2(3) . . . . no C8 Fe1 C5 C4 100.8(3) . . . . no C9 Fe1 C5 C1 -98.0(3) . . . . no C9 Fe1 C5 C4 145.0(3) . . . . no C10 Fe1 C5 C1 -59.5(4) . . . . no C10 Fe1 C5 C4 -176.5(3) . . . . no C1 Fe1 C6 C7 -179.2(3) . . . . no C1 Fe1 C6 C10 -60.5(3) . . . . no C2 Fe1 C6 C7 145.7(2) . . . . no C2 Fe1 C6 C10 -95.6(2) . . . . no C3 Fe1 C6 C7 103.5(2) . . . . no C3 Fe1 C6 C10 -137.7(2) . . . . no C4 Fe1 C6 C7 64.8(3) . . . . no C4 Fe1 C6 C10 -176.5(3) . . . . no C7 Fe1 C6 C10 118.7(3) . . . . no C8 Fe1 C6 C7 -36.7(2) . . . . no C8 Fe1 C6 C10 82.1(2) . . . . no C9 Fe1 C6 C7 -80.8(2) . . . . no C9 Fe1 C6 C10 37.99(19) . . . . no C10 Fe1 C6 C7 -118.7(3) . . . . no C2 Fe1 C7 C6 -58.1(3) . . . . no C2 Fe1 C7 C8 -178.7(2) . . . . no C3 Fe1 C7 C6 -94.3(2) . . . . no C3 Fe1 C7 C8 145.1(2) . . . . no C4 Fe1 C7 C6 -138.6(3) . . . . no C4 Fe1 C7 C8 100.8(3) . . . . no C5 Fe1 C7 C6 -179.5(3) . . . . no C5 Fe1 C7 C8 59.8(4) . . . . no C6 Fe1 C7 C8 -120.6(3) . . . . no C8 Fe1 C7 C6 120.6(3) . . . . no C9 Fe1 C7 C6 83.1(2) . . . . no C9 Fe1 C7 C8 -37.49(19) . . . . no C10 Fe1 C7 C6 38.7(2) . . . . no C10 Fe1 C7 C8 -82.0(2) . . . . no C1 Fe1 C8 C7 179.5(2) . . . . no C1 Fe1 C8 C9 59.2(3) . . . . no C3 Fe1 C8 C7 -60.0(3) . . . . no C3 Fe1 C8 C9 179.8(3) . . . . no C4 Fe1 C8 C7 -96.8(3) . . . . no C4 Fe1 C8 C9 143.0(3) . . . . no C5 Fe1 C8 C7 -143.3(3) . . . . no C5 Fe1 C8 C9 96.5(3) . . . . no C6 Fe1 C8 C7 36.8(2) . . . . no C6 Fe1 C8 C9 -83.5(2) . . . . no C7 Fe1 C8 C9 -120.2(3) . . . . no C9 Fe1 C8 C7 120.2(3) . . . . no C10 Fe1 C8 C7 81.6(2) . . . . no C10 Fe1 C8 C9 -38.7(2) . . . . no C1 Fe1 C9 C8 -143.4(2) . . . . no C1 Fe1 C9 C10 98.6(2) . . . . no C2 Fe1 C9 C8 -177.4(3) . . . . no C2 Fe1 C9 C10 64.5(3) . . . . no C4 Fe1 C9 C8 -62.2(3) . . . . no C4 Fe1 C9 C10 179.8(3) . . . . no C5 Fe1 C9 C8 -100.6(3) . . . . no C5 Fe1 C9 C10 141.3(2) . . . . no C6 Fe1 C9 C8 79.9(2) . . . . no C6 Fe1 C9 C10 -38.21(19) . . . . no C7 Fe1 C9 C8 36.7(2) . . . . no C7 Fe1 C9 C10 -81.4(2) . . . . no C8 Fe1 C9 C10 -118.1(3) . . . . no C10 Fe1 C9 C8 118.1(3) . . . . no C1 Fe1 C10 C6 142.9(2) . . . . no C1 Fe1 C10 C9 -98.0(2) . . . . no C1 Fe1 C10 C11 24.5(3) . . . . no C2 Fe1 C10 C6 102.1(3) . . . . no C2 Fe1 C10 C9 -138.8(2) . . . . no C2 Fe1 C10 C11 -16.3(3) . . . . no C3 Fe1 C10 C6 66.3(3) . . . . no C3 Fe1 C10 C9 -174.6(2) . . . . no C3 Fe1 C10 C11 -52.1(4) . . . . no C5 Fe1 C10 C6 179.1(3) . . . . no C5 Fe1 C10 C9 -61.8(3) . . . . no C5 Fe1 C10 C11 60.7(4) . . . . no C6 Fe1 C10 C9 119.1(3) . . . . no C6 Fe1 C10 C11 -118.4(4) . . . . no C7 Fe1 C10 C6 -37.5(2) . . . . no C7 Fe1 C10 C9 81.6(2) . . . . no C7 Fe1 C10 C11 -155.9(3) . . . . no C8 Fe1 C10 C6 -80.7(2) . . . . no C8 Fe1 C10 C9 38.41(19) . . . . no C8 Fe1 C10 C11 160.9(3) . . . . no C9 Fe1 C10 C6 -119.1(3) . . . . no C9 Fe1 C10 C11 122.5(4) . . . . no C12 O2 C11 O1 0.2(4) . . . . no C12 O2 C11 C10 179.7(2) . . . . no C11 O2 C12 C13 -108.0(3) . . . . no C11 O2 C12 C16 75.8(4) . . . . no C16 N1 C15 C14 0.2(5) . . . . no C15 N1 C16 C12 -1.4(5) . . . . no C15 N1 C16 C17 177.3(3) . . . . no C18 N2 C17 O3 8.6(6) . . . . no C18 N2 C17 C16 -170.1(3) . . . . no C17 N2 C18 O4 -3.1(6) . . . . no C17 N2 C18 C19 174.4(4) . . . . no C23 N3 C19 C18 -177.2(3) . . . . no C23 N3 C19 C20 0.7(5) . . . . no C19 N3 C23 C22 0.5(5) . . . . no Fe1 C1 C2 C3 -59.1(3) . . . . no C5 C1 C2 Fe1 59.4(4) . . . . no C5 C1 C2 C3 0.4(6) . . . . no Fe1 C1 C5 C4 60.1(3) . . . . no C2 C1 C5 Fe1 -60.6(4) . . . . no C2 C1 C5 C4 -0.5(6) . . . . no Fe1 C2 C3 C4 -59.0(3) . . . . no C1 C2 C3 Fe1 58.9(3) . . . . no C1 C2 C3 C4 0.0(5) . . . . no Fe1 C3 C4 C5 -60.1(3) . . . . no C2 C3 C4 Fe1 59.8(3) . . . . no C2 C3 C4 C5 -0.3(5) . . . . no Fe1 C4 C5 C1 -61.0(4) . . . . no C3 C4 C5 Fe1 61.5(3) . . . . no C3 C4 C5 C1 0.5(5) . . . . no Fe1 C6 C7 C8 58.9(3) . . . . no C10 C6 C7 Fe1 -58.4(2) . . . . no C10 C6 C7 C8 0.5(4) . . . . no Fe1 C6 C10 C9 -59.6(2) . . . . no Fe1 C6 C10 C11 114.2(3) . . . . no C7 C6 C10 Fe1 59.7(2) . . . . no C7 C6 C10 C9 0.1(4) . . . . no C7 C6 C10 C11 173.9(3) . . . . no Fe1 C7 C8 C9 57.7(2) . . . . no C6 C7 C8 Fe1 -58.7(3) . . . . no C6 C7 C8 C9 -0.9(4) . . . . no Fe1 C8 C9 C10 59.6(2) . . . . no C7 C8 C9 Fe1 -58.7(3) . . . . no C7 C8 C9 C10 1.0(4) . . . . no Fe1 C9 C10 C6 60.0(2) . . . . no Fe1 C9 C10 C11 -113.6(3) . . . . no C8 C9 C10 Fe1 -60.6(2) . . . . no C8 C9 C10 C6 -0.6(4) . . . . no C8 C9 C10 C11 -174.2(3) . . . . no Fe1 C10 C11 O1 101.3(4) . . . . no Fe1 C10 C11 O2 -78.1(3) . . . . no C6 C10 C11 O1 15.6(5) . . . . no C6 C10 C11 O2 -163.8(3) . . . . no C9 C10 C11 O1 -171.7(3) . . . . no C9 C10 C11 O2 8.8(4) . . . . no O2 C12 C13 C14 -176.2(3) . . . . no C16 C12 C13 C14 0.2(5) . . . . no O2 C12 C16 N1 177.4(3) . . . . no O2 C12 C16 C17 -1.2(5) . . . . no C13 C12 C16 N1 1.2(5) . . . . no C13 C12 C16 C17 -177.4(3) . . . . no C12 C13 C14 C15 -1.4(5) . . . . no C13 C14 C15 N1 1.2(5) . . . . no N1 C16 C17 O3 -169.2(3) . . . . no N1 C16 C17 N2 9.6(4) . . . . no C12 C16 C17 O3 9.5(6) . . . . no C12 C16 C17 N2 -171.7(3) . . . . no O4 C18 C19 N3 176.0(3) . . . . no O4 C18 C19 C20 -1.9(5) . . . . no N2 C18 C19 N3 -1.6(5) . . . . no N2 C18 C19 C20 -179.5(3) . . . . no N3 C19 C20 C21 -0.7(5) . . . . no C18 C19 C20 C21 177.1(3) . . . . no C19 C20 C21 C22 -0.3(5) . . . . no C20 C21 C22 C23 1.4(5) . . . . no C21 C22 C23 N3 -1.6(5) . . . . no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # N2 H2N N1 0.89(4) 2.15(4) 2.611(4) 112(3) . yes N2 H2N N3 0.89(4) 2.18(3) 2.647(4) 112(3) . yes C9 H9 O2 0.95 2.58 3.448(4) 152 3_755 yes C14 H14 O3 0.95 2.53 3.139(4) 122 1_565 yes C15 H15 O3 0.95 2.57 3.169(4) 121 1_565 yes C15 H15 O4 0.95 2.33 3.247(4) 161 1_565 yes _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.761 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.071 #============================= # Attachment 'web_deposit_cif_file_1_HelenStoeckli-Evans_1331020702.2_H2L2.cif' data_H2L2 _database_code_depnum_ccdc_archive 'CCDC 870328' #TrackingRef 'web_deposit_cif_file_1_HelenStoeckli-Evans_1331020702.2_H2L2.cif' _audit_update_record ; 2011-06-03 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 Fe N6 O8, 2(C H Cl3)' _chemical_formula_sum 'C38 H26 Cl6 Fe N6 O8' _chemical_formula_weight 963.20 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 16.391(5) _cell_length_b 18.117(5) _cell_length_c 13.078(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.029(5) _cell_angle_gamma 90.00 _cell_volume 3883(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 19933 _cell_measurement_theta_max 29.54 _cell_measurement_theta_min 1.50 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9415 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2009)' _exptl_special_details ? _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'plane graphite' _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_measurement_method '\f + \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25659 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.10 _reflns_number_total 6912 _reflns_number_gt 5050 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2002)' _computing_cell_refinement X-Area _computing_data_reduction 'X-RED32 (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009) and Mercury (Macrae et al., 2006)' _computing_publication_material 'SHELXL-97, PLATON and Publcif (Westrip, 2010)' _refine_special_details ; The NH H-atoms were located in difference electron-density maps and were freely refined. The C-bound H-atoms were included in calculated positions and treated as riding atoms: C-H = 1.0 and 0.95 \%A for CH(methine) and CH(aromatic), respectively, with U~iso~(H) = 1.2U~eq~(parent C-atom). ; _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^)+(0.0502P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6912 _refine_ls_number_parameters 540 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe Uani 0.24022(3) 0.57204(2) 0.29667(4) 1.000 0.0268(1) d . . . O1 O Uani 0.26575(14) 0.37183(12) 0.18879(17) 1.000 0.0320(7) d . . . O2 O Uani 0.30490(13) 0.38619(11) 0.35391(16) 1.000 0.0290(7) d . . . O3 O Uani 0.17700(13) 0.28893(12) 0.36187(18) 1.000 0.0321(7) d . . . O4 O Uani 0.06721(14) 0.16775(13) 0.36071(19) 1.000 0.0349(7) d . . . O5 O Uani 0.22511(15) 0.72360(14) 0.08746(18) 1.000 0.0391(8) d . . . O6 O Uani 0.17997(14) 0.76198(12) 0.24051(17) 1.000 0.0326(7) d . . . O7 O Uani 0.31277(14) 0.84750(13) 0.1914(2) 1.000 0.0431(8) d . . . O8 O Uani 0.42451(14) 0.95323(13) 0.1217(2) 1.000 0.0385(8) d . . . N1 N Uani 0.36406(16) 0.19117(15) 0.3606(2) 1.000 0.0294(8) d . . . N2 N Uani 0.20739(17) 0.16582(15) 0.3664(2) 1.000 0.0304(9) d . . . N3 N Uani 0.20777(18) 0.02394(15) 0.4065(2) 1.000 0.0373(9) d . . . N4 N Uani 0.13009(16) 0.94476(14) 0.1395(2) 1.000 0.0291(8) d . . . N5 N Uani 0.28684(17) 0.96667(16) 0.1434(2) 1.000 0.0306(9) d . . . N6 N Uani 0.29744(16) 1.11036(15) 0.1200(2) 1.000 0.0306(8) d . . . C1 C Uani 0.20451(19) 0.46502(17) 0.2894(2) 1.000 0.0272(9) d . . . C2 C Uani 0.1854(2) 0.49525(18) 0.3870(3) 1.000 0.0305(10) d . . . C3 C Uani 0.1324(2) 0.55504(18) 0.3699(3) 1.000 0.0363(10) d . . . C4 C Uani 0.1181(2) 0.56291(19) 0.2635(3) 1.000 0.0366(10) d . . . C5 C Uani 0.16246(19) 0.50694(18) 0.2121(3) 1.000 0.0319(10) d . . . C6 C Uani 0.25883(19) 0.40327(17) 0.2684(2) 1.000 0.0264(9) d . . . C7 C Uani 0.35106(19) 0.32236(17) 0.3507(2) 1.000 0.0267(9) d . . . C8 C Uani 0.4351(2) 0.32982(19) 0.3499(3) 1.000 0.0331(10) d . . . C9 C Uani 0.4829(2) 0.2674(2) 0.3530(3) 1.000 0.0370(11) d . . . C10 C Uani 0.4447(2) 0.1989(2) 0.3582(3) 1.000 0.0342(10) d . . . C11 C Uani 0.31740(19) 0.25197(16) 0.3563(2) 1.000 0.0244(9) d . . . C12 C Uani 0.22672(19) 0.23953(17) 0.3610(2) 1.000 0.0271(9) d . . . C13 C Uani 0.13049(19) 0.13459(18) 0.3702(2) 1.000 0.0286(10) d . . . C14 C Uani 0.1343(2) 0.05292(17) 0.3907(2) 1.000 0.0292(9) d . . . C15 C Uani 0.0633(2) 0.0129(2) 0.3933(3) 1.000 0.0373(11) d . . . C16 C Uani 0.0682(2) -0.0615(2) 0.4165(3) 1.000 0.0424(11) d . . . C17 C Uani 0.1429(3) -0.09215(19) 0.4353(3) 1.000 0.0423(13) d . . . C18 C Uani 0.2104(2) -0.0482(2) 0.4289(3) 1.000 0.0452(14) d . . . C19 C Uani 0.27879(19) 0.67020(17) 0.2410(3) 1.000 0.0305(10) d . . . C20 C Uani 0.3270(2) 0.61192(19) 0.2009(3) 1.000 0.0354(11) d . . . C21 C Uani 0.3645(2) 0.57499(19) 0.2851(3) 1.000 0.0358(10) d . . . C22 C Uani 0.3410(2) 0.61111(19) 0.3762(3) 1.000 0.0336(10) d . . . C23 C Uani 0.28730(19) 0.66964(18) 0.3498(3) 1.000 0.0310(10) d . . . C24 C Uani 0.2277(2) 0.71978(17) 0.1789(3) 1.000 0.0308(10) d . . . C25 C Uani 0.13645(19) 0.82016(18) 0.1977(2) 1.000 0.0278(9) d . . . C26 C Uani 0.0525(2) 0.81507(19) 0.1945(2) 1.000 0.0309(10) d . . . C27 C Uani 0.0081(2) 0.87614(18) 0.1649(3) 1.000 0.0309(10) d . . . C28 C Uani 0.0490(2) 0.93964(19) 0.1386(3) 1.000 0.0323(10) d . . . C29 C Uani 0.17368(19) 0.88551(17) 0.1691(2) 1.000 0.0264(9) d . . . C30 C Uani 0.2647(2) 0.89554(18) 0.1694(3) 1.000 0.0302(10) d . . . C31 C Uani 0.36458(19) 0.99243(18) 0.1271(2) 1.000 0.0298(10) d . . . C32 C Uani 0.36827(19) 1.07409(18) 0.1155(2) 1.000 0.0288(9) d . . . C33 C Uani 0.4423(2) 1.1080(2) 0.1032(3) 1.000 0.0370(11) d . . . C34 C Uani 0.4447(2) 1.1844(2) 0.1001(3) 1.000 0.0400(12) d . . . C35 C Uani 0.3728(2) 1.2225(2) 0.1052(3) 1.000 0.0397(11) d . . . C36 C Uani 0.3009(2) 1.18375(19) 0.1149(3) 1.000 0.0359(11) d . . . Cl1 Cl Uani 0.59368(7) 0.34503(6) 0.06484(8) 1.000 0.0551(3) d . . . Cl2 Cl Uani 0.59335(7) 0.49904(5) 0.12607(8) 1.000 0.0497(3) d . . . Cl3 Cl Uani 0.44328(6) 0.41634(6) 0.12050(8) 1.000 0.0540(3) d . . . C37 C Uani 0.5490(2) 0.4117(2) 0.1433(3) 1.000 0.0413(12) d . . . Cl4 Cl Uani 0.08820(6) 0.13391(5) 0.08795(7) 1.000 0.0418(3) d . . . Cl5 Cl Uani -0.05033(5) 0.23122(5) 0.06298(7) 1.000 0.0407(3) d . . . Cl6 Cl Uani 0.10881(5) 0.29167(5) 0.11209(7) 1.000 0.0377(3) d . . . C38 C Uani 0.05507(19) 0.22183(17) 0.0459(3) 1.000 0.0299(10) d . . . H2A H Uiso 0.20500 0.47810 0.45150 1.000 0.0370 c R . . H2N H Uiso 0.247(3) 0.136(2) 0.372(3) 1.000 0.043(11) d . . . H3A H Uiso 0.10980 0.58530 0.42140 1.000 0.0440 c R . . H4A H Uiso 0.08460 0.59940 0.23180 1.000 0.0440 c R . . H5A H Uiso 0.16390 0.49900 0.14030 1.000 0.0380 c R . . H5N H Uiso 0.249(3) 0.997(2) 0.135(3) 1.000 0.050(12) d . . . H8A H Uiso 0.45950 0.37740 0.34720 1.000 0.0400 c R . . H9A H Uiso 0.54070 0.27090 0.35170 1.000 0.0440 c R . . H10A H Uiso 0.47770 0.15570 0.36000 1.000 0.0410 c R . . H15A H Uiso 0.01210 0.03570 0.37940 1.000 0.0450 c R . . H16A H Uiso 0.02020 -0.09080 0.41930 1.000 0.0510 c R . . H17A H Uiso 0.14800 -0.14290 0.45260 1.000 0.0510 c R . . H18A H Uiso 0.26230 -0.07020 0.44090 1.000 0.0540 c R . . H20A H Uiso 0.33290 0.60000 0.13070 1.000 0.0420 c R . . H21A H Uiso 0.39940 0.53320 0.28110 1.000 0.0430 c R . . H22A H Uiso 0.35840 0.59820 0.44360 1.000 0.0400 c R . . H23A H Uiso 0.26170 0.70240 0.39590 1.000 0.0370 c R . . H26A H Uiso 0.02590 0.77040 0.21240 1.000 0.0370 c R . . H27A H Uiso -0.04990 0.87460 0.16260 1.000 0.0370 c R . . H28A H Uiso 0.01790 0.98170 0.11880 1.000 0.0390 c R . . H33A H Uiso 0.49080 1.07970 0.09700 1.000 0.0440 c R . . H34A H Uiso 0.49520 1.20980 0.09460 1.000 0.0480 c R . . H35A H Uiso 0.37250 1.27490 0.10200 1.000 0.0480 c R . . H36A H Uiso 0.25130 1.21080 0.11810 1.000 0.0430 c R . . H37A H Uiso 0.55850 0.39660 0.21620 1.000 0.0500 c R . . H38A H Uiso 0.06650 0.22650 -0.02860 1.000 0.0360 c 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 Fe1 0.0214(2) 0.0216(2) 0.0374(3) 0.0029(2) -0.0008(2) -0.0021(2) O1 0.0320(12) 0.0314(12) 0.0326(13) -0.0020(10) -0.0031(10) -0.0001(10) O2 0.0331(12) 0.0222(11) 0.0314(12) 0.0003(9) -0.0055(10) -0.0003(9) O3 0.0276(11) 0.0262(12) 0.0427(13) 0.0036(10) 0.0037(10) 0.0042(10) O4 0.0259(12) 0.0319(12) 0.0468(14) 0.0022(11) -0.0002(10) 0.0017(10) O5 0.0448(14) 0.0375(14) 0.0348(14) 0.0004(11) -0.0008(11) 0.0021(11) O6 0.0354(13) 0.0285(12) 0.0340(12) 0.0074(10) 0.0032(10) 0.0037(10) O7 0.0279(13) 0.0293(12) 0.0717(18) 0.0086(12) -0.0062(12) 0.0017(11) O8 0.0240(12) 0.0370(13) 0.0545(15) 0.0057(11) 0.0033(11) 0.0068(11) N1 0.0276(14) 0.0283(14) 0.0322(15) -0.0001(11) 0.0003(11) 0.0038(11) N2 0.0229(14) 0.0214(13) 0.0469(17) 0.0018(12) 0.0043(12) 0.0021(12) N3 0.0360(16) 0.0253(15) 0.0505(18) -0.0003(13) 0.0004(14) 0.0023(12) N4 0.0227(13) 0.0283(14) 0.0363(15) 0.0022(12) -0.0008(11) 0.0022(11) N5 0.0206(14) 0.0264(14) 0.0446(17) 0.0061(12) -0.0008(12) 0.0011(12) N6 0.0243(14) 0.0294(14) 0.0382(15) 0.0010(12) 0.0004(12) 0.0044(11) C1 0.0225(15) 0.0242(15) 0.0349(17) 0.0009(13) 0.0000(13) -0.0058(13) C2 0.0279(16) 0.0274(17) 0.0363(18) 0.0013(14) 0.0032(14) -0.0059(14) C3 0.0288(17) 0.0285(17) 0.052(2) -0.0041(16) 0.0088(16) -0.0055(14) C4 0.0223(16) 0.0304(18) 0.057(2) 0.0072(16) -0.0053(15) -0.0035(14) C5 0.0247(16) 0.0283(17) 0.0423(19) 0.0042(14) -0.0067(14) -0.0049(14) C6 0.0262(16) 0.0224(15) 0.0306(18) 0.0035(13) -0.0018(13) -0.0069(12) C7 0.0289(16) 0.0264(16) 0.0248(16) 0.0016(13) -0.0027(13) 0.0012(13) C8 0.0301(17) 0.0359(18) 0.0331(18) 0.0046(15) -0.0032(14) -0.0080(15) C9 0.0258(17) 0.047(2) 0.0380(19) 0.0036(16) -0.0016(14) -0.0015(16) C10 0.0278(17) 0.0363(18) 0.0384(19) 0.0012(15) -0.0024(14) 0.0072(15) C11 0.0272(16) 0.0229(15) 0.0230(15) 0.0005(12) -0.0007(12) 0.0005(12) C12 0.0274(16) 0.0261(16) 0.0279(16) 0.0038(13) 0.0037(13) 0.0023(14) C13 0.0271(17) 0.0281(16) 0.0306(17) -0.0028(14) 0.0017(13) -0.0020(14) C14 0.0337(17) 0.0258(16) 0.0280(16) -0.0015(13) 0.0012(13) 0.0005(14) C15 0.0325(18) 0.0372(19) 0.042(2) 0.0004(16) -0.0045(15) -0.0052(15) C16 0.045(2) 0.0312(19) 0.051(2) 0.0013(16) 0.0010(17) -0.0127(17) C17 0.060(3) 0.0231(17) 0.044(2) -0.0004(15) 0.0052(18) -0.0043(17) C18 0.045(2) 0.0284(19) 0.062(3) 0.0017(17) -0.0001(19) 0.0063(16) C19 0.0278(17) 0.0243(16) 0.0393(18) 0.0037(14) -0.0006(14) -0.0061(13) C20 0.0278(17) 0.0336(18) 0.045(2) 0.0007(15) 0.0051(15) -0.0066(14) C21 0.0217(15) 0.0295(17) 0.056(2) 0.0050(16) -0.0007(15) -0.0019(14) C22 0.0231(16) 0.0334(18) 0.044(2) 0.0065(15) -0.0063(14) -0.0065(14) C23 0.0254(16) 0.0281(17) 0.0395(18) -0.0006(14) -0.0025(14) -0.0060(14) C24 0.0336(17) 0.0227(16) 0.036(2) 0.0018(13) 0.0003(14) -0.0086(14) C25 0.0292(16) 0.0285(16) 0.0256(16) 0.0007(13) -0.0010(13) 0.0041(13) C26 0.0333(17) 0.0311(17) 0.0284(16) 0.0013(14) 0.0012(14) -0.0066(14) C27 0.0230(15) 0.0342(18) 0.0356(18) -0.0019(14) -0.0004(13) -0.0012(14) C28 0.0272(17) 0.0308(17) 0.0389(19) 0.0030(14) 0.0005(14) 0.0050(14) C29 0.0235(16) 0.0263(16) 0.0295(16) 0.0000(13) -0.0001(12) 0.0006(13) C30 0.0275(17) 0.0261(16) 0.0369(18) 0.0021(14) -0.0016(14) 0.0001(14) C31 0.0229(16) 0.0319(17) 0.0346(18) 0.0004(14) -0.0023(13) 0.0002(14) C32 0.0243(15) 0.0305(16) 0.0315(16) 0.0021(14) -0.0037(13) 0.0013(14) C33 0.0250(17) 0.041(2) 0.045(2) 0.0043(16) -0.0030(15) -0.0024(15) C34 0.037(2) 0.044(2) 0.039(2) 0.0053(16) -0.0004(16) -0.0126(17) C35 0.054(2) 0.0286(18) 0.0363(19) 0.0024(15) -0.0025(17) -0.0063(17) C36 0.0384(19) 0.0308(18) 0.0384(19) 0.0013(15) 0.0023(15) 0.0054(15) Cl1 0.0583(6) 0.0488(6) 0.0583(6) -0.0118(5) 0.0074(5) -0.0171(5) Cl2 0.0552(6) 0.0387(5) 0.0554(6) 0.0055(4) 0.0039(5) -0.0137(4) Cl3 0.0422(5) 0.0662(7) 0.0533(6) 0.0080(5) -0.0047(4) -0.0118(5) C37 0.044(2) 0.044(2) 0.036(2) 0.0045(16) 0.0012(16) -0.0115(17) Cl4 0.0416(5) 0.0296(4) 0.0540(5) 0.0039(4) -0.0049(4) 0.0038(4) Cl5 0.0271(4) 0.0385(5) 0.0567(6) -0.0102(4) 0.0053(4) 0.0009(4) Cl6 0.0344(4) 0.0336(4) 0.0448(5) -0.0090(4) -0.0046(4) -0.0022(4) C38 0.0303(17) 0.0271(17) 0.0323(18) -0.0030(13) -0.0007(14) 0.0010(14) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 2.027(3) . . no Fe1 C2 2.044(4) . . no Fe1 C3 2.048(4) . . no Fe1 C4 2.047(3) . . no Fe1 C5 2.047(4) . . no Fe1 C19 2.027(3) . . no Fe1 C20 2.044(4) . . no Fe1 C21 2.046(3) . . no Fe1 C22 2.062(4) . . no Fe1 C23 2.046(3) . . no Cl1 C37 1.754(4) . . no Cl2 C37 1.758(4) . . no Cl3 C37 1.755(4) . . no Cl4 C38 1.767(3) . . no Cl5 C38 1.754(3) . . no Cl6 C38 1.760(3) . . no O1 C6 1.194(4) . . no O2 C7 1.383(4) . . no O2 C6 1.373(4) . . no O3 C12 1.211(4) . . no O4 C13 1.203(4) . . no O5 C24 1.198(5) . . no O6 C24 1.367(4) . . no O6 C25 1.385(4) . . no O7 C30 1.205(4) . . no O8 C31 1.215(4) . . no N1 C11 1.342(4) . . no N1 C10 1.330(4) . . no N2 C12 1.375(4) . . no N2 C13 1.383(4) . . no N3 C18 1.340(5) . . no N3 C14 1.327(4) . . no N4 C29 1.343(4) . . no N4 C28 1.332(4) . . no N5 C30 1.383(4) . . no N5 C31 1.377(4) . . no N6 C32 1.336(4) . . no N6 C36 1.333(4) . . no N2 H2N 0.85(4) . . no N5 H5N 0.83(4) . . no C1 C2 1.429(5) . . no C1 C6 1.459(4) . . no C1 C5 1.431(5) . . no C2 C3 1.404(5) . . no C3 C4 1.414(6) . . no C4 C5 1.424(5) . . no C7 C8 1.384(5) . . no C7 C11 1.392(4) . . no C8 C9 1.376(5) . . no C9 C10 1.392(5) . . no C11 C12 1.506(4) . . no C13 C14 1.505(4) . . no C14 C15 1.372(5) . . no C15 C16 1.384(5) . . no C16 C17 1.363(6) . . no C17 C18 1.367(6) . . no C19 C20 1.425(5) . . no C19 C24 1.464(5) . . no C19 C23 1.427(6) . . no C20 C21 1.419(5) . . no C21 C22 1.419(5) . . no C22 C23 1.417(5) . . no C25 C26 1.379(5) . . no C25 C29 1.386(4) . . no C26 C27 1.376(5) . . no C27 C28 1.378(5) . . no C29 C30 1.503(5) . . no C31 C32 1.489(5) . . no C32 C33 1.372(5) . . no C33 C34 1.385(5) . . no C34 C35 1.368(5) . . no C35 C36 1.380(5) . . no C2 H2A 0.9500 . . no C3 H3A 0.9500 . . no C4 H4A 0.9500 . . no C5 H5A 0.9500 . . no C8 H8A 0.9500 . . no C9 H9A 0.9500 . . no C10 H10A 0.9500 . . no C15 H15A 0.9500 . . no C16 H16A 0.9500 . . no C17 H17A 0.9500 . . no C18 H18A 0.9500 . . no C20 H20A 0.9500 . . no C21 H21A 0.9500 . . no C22 H22A 0.9500 . . no C23 H23A 0.9500 . . no C26 H26A 0.9500 . . no C27 H27A 0.9500 . . no C28 H28A 0.9500 . . no C33 H33A 0.9500 . . no C34 H34A 0.9500 . . no C35 H35A 0.9500 . . no C36 H36A 0.9500 . . no C37 H37A 1.0000 . . no C38 H38A 1.0000 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C2 41.10(13) . . . no C1 Fe1 C3 68.12(13) . . . no C1 Fe1 C4 68.43(13) . . . no C1 Fe1 C5 41.14(13) . . . no C1 Fe1 C19 156.06(13) . . . no C1 Fe1 C20 120.86(13) . . . no C1 Fe1 C21 107.97(13) . . . no C1 Fe1 C22 125.46(13) . . . no C1 Fe1 C23 161.71(13) . . . no C2 Fe1 C3 40.13(13) . . . no C2 Fe1 C4 68.23(14) . . . no C2 Fe1 C5 69.15(15) . . . no C2 Fe1 C19 161.45(14) . . . no C2 Fe1 C20 155.90(14) . . . no C2 Fe1 C21 120.61(14) . . . no C2 Fe1 C22 107.38(15) . . . no C2 Fe1 C23 123.99(15) . . . no C3 Fe1 C4 40.40(15) . . . no C3 Fe1 C5 68.40(14) . . . no C3 Fe1 C19 125.25(13) . . . no C3 Fe1 C20 162.81(14) . . . no C3 Fe1 C21 155.09(15) . . . no C3 Fe1 C22 120.40(15) . . . no C3 Fe1 C23 107.13(14) . . . no C4 Fe1 C5 40.70(14) . . . no C4 Fe1 C19 107.75(14) . . . no C4 Fe1 C20 125.96(15) . . . no C4 Fe1 C21 163.22(16) . . . no C4 Fe1 C22 154.99(15) . . . no C4 Fe1 C23 120.21(13) . . . no C5 Fe1 C19 120.45(15) . . . no C5 Fe1 C20 107.82(15) . . . no C5 Fe1 C21 125.90(14) . . . no C5 Fe1 C22 162.98(13) . . . no C5 Fe1 C23 155.38(14) . . . no C19 Fe1 C20 40.96(14) . . . no C19 Fe1 C21 68.48(13) . . . no C19 Fe1 C22 68.14(14) . . . no C19 Fe1 C23 41.02(15) . . . no C20 Fe1 C21 40.60(15) . . . no C20 Fe1 C22 68.14(15) . . . no C20 Fe1 C23 68.91(14) . . . no C21 Fe1 C22 40.41(15) . . . no C21 Fe1 C23 68.44(13) . . . no C22 Fe1 C23 40.36(13) . . . no C6 O2 C7 117.2(2) . . . no C24 O6 C25 118.9(2) . . . no C10 N1 C11 118.6(3) . . . no C12 N2 C13 127.6(3) . . . no C14 N3 C18 116.5(3) . . . no C28 N4 C29 118.2(3) . . . no C30 N5 C31 127.0(3) . . . no C32 N6 C36 116.8(3) . . . no C12 N2 H2N 117(3) . . . no C13 N2 H2N 116(3) . . . no C30 N5 H5N 117(3) . . . no C31 N5 H5N 116(3) . . . no Fe1 C1 C2 70.08(18) . . . no C5 C1 C6 124.2(3) . . . no Fe1 C1 C6 124.4(2) . . . no C2 C1 C5 108.5(3) . . . no Fe1 C1 C5 70.16(18) . . . no C2 C1 C6 127.3(3) . . . no Fe1 C2 C1 68.83(19) . . . no Fe1 C2 C3 70.1(2) . . . no C1 C2 C3 107.4(3) . . . no C2 C3 C4 109.0(3) . . . no Fe1 C3 C2 69.8(2) . . . no Fe1 C3 C4 69.8(2) . . . no Fe1 C4 C5 69.63(19) . . . no C3 C4 C5 108.4(3) . . . no Fe1 C4 C3 69.85(19) . . . no Fe1 C5 C1 68.70(19) . . . no Fe1 C5 C4 69.7(2) . . . no C1 C5 C4 106.7(3) . . . no O1 C6 O2 122.9(3) . . . no O2 C6 C1 110.4(2) . . . no O1 C6 C1 126.7(3) . . . no O2 C7 C8 117.6(3) . . . no O2 C7 C11 123.2(3) . . . no C8 C7 C11 119.0(3) . . . no C7 C8 C9 119.1(3) . . . no C8 C9 C10 118.5(3) . . . no N1 C10 C9 122.9(3) . . . no C7 C11 C12 122.1(3) . . . no N1 C11 C12 116.0(3) . . . no N1 C11 C7 121.9(3) . . . no O3 C12 C11 123.7(3) . . . no N2 C12 C11 112.1(3) . . . no O3 C12 N2 124.2(3) . . . no O4 C13 N2 125.2(3) . . . no O4 C13 C14 122.8(3) . . . no N2 C13 C14 111.9(3) . . . no N3 C14 C15 123.7(3) . . . no C13 C14 C15 119.4(3) . . . no N3 C14 C13 116.9(3) . . . no C14 C15 C16 118.3(3) . . . no C15 C16 C17 119.0(3) . . . no C16 C17 C18 118.5(3) . . . no N3 C18 C17 124.0(3) . . . no Fe1 C19 C23 70.20(19) . . . no Fe1 C19 C24 124.0(2) . . . no C20 C19 C23 108.5(3) . . . no C20 C19 C24 124.5(3) . . . no Fe1 C19 C20 70.16(19) . . . no C23 C19 C24 127.0(3) . . . no Fe1 C20 C19 68.9(2) . . . no Fe1 C20 C21 69.8(2) . . . no C19 C20 C21 107.4(3) . . . no Fe1 C21 C22 70.38(19) . . . no C20 C21 C22 108.3(3) . . . no Fe1 C21 C20 69.62(19) . . . no C21 C22 C23 108.5(3) . . . no Fe1 C22 C21 69.2(2) . . . no Fe1 C22 C23 69.23(19) . . . no C19 C23 C22 107.3(3) . . . no Fe1 C23 C22 70.42(19) . . . no Fe1 C23 C19 68.78(19) . . . no O5 C24 C19 126.8(3) . . . no O6 C24 C19 110.1(3) . . . no O5 C24 O6 123.1(3) . . . no O6 C25 C26 117.9(3) . . . no O6 C25 C29 122.2(3) . . . no C26 C25 C29 119.5(3) . . . no C25 C26 C27 118.5(3) . . . no C26 C27 C28 119.0(3) . . . no N4 C28 C27 123.1(3) . . . no N4 C29 C25 121.7(3) . . . no N4 C29 C30 115.3(3) . . . no C25 C29 C30 123.0(3) . . . no N5 C30 C29 112.1(3) . . . no O7 C30 N5 123.9(3) . . . no O7 C30 C29 123.9(3) . . . no O8 C31 C32 122.7(3) . . . no N5 C31 C32 113.1(3) . . . no O8 C31 N5 124.2(3) . . . no N6 C32 C31 116.6(3) . . . no N6 C32 C33 123.8(3) . . . no C31 C32 C33 119.6(3) . . . no C32 C33 C34 118.5(3) . . . no C33 C34 C35 118.5(3) . . . no C34 C35 C36 119.1(3) . . . no N6 C36 C35 123.3(3) . . . no Fe1 C2 H2A 126.00 . . . no C1 C2 H2A 126.00 . . . no C3 C2 H2A 126.00 . . . no Fe1 C3 H3A 127.00 . . . no C2 C3 H3A 126.00 . . . no C4 C3 H3A 125.00 . . . no Fe1 C4 H4A 126.00 . . . no C3 C4 H4A 126.00 . . . no C5 C4 H4A 126.00 . . . no Fe1 C5 H5A 126.00 . . . no C1 C5 H5A 127.00 . . . no C4 C5 H5A 127.00 . . . no C7 C8 H8A 121.00 . . . no C9 C8 H8A 120.00 . . . no C8 C9 H9A 121.00 . . . no C10 C9 H9A 121.00 . . . no N1 C10 H10A 119.00 . . . no C9 C10 H10A 119.00 . . . no C14 C15 H15A 121.00 . . . no C16 C15 H15A 121.00 . . . no C15 C16 H16A 121.00 . . . no C17 C16 H16A 120.00 . . . no C16 C17 H17A 121.00 . . . no C18 C17 H17A 121.00 . . . no N3 C18 H18A 118.00 . . . no C17 C18 H18A 118.00 . . . no Fe1 C20 H20A 127.00 . . . no C19 C20 H20A 126.00 . . . no C21 C20 H20A 126.00 . . . no Fe1 C21 H21A 126.00 . . . no C20 C21 H21A 126.00 . . . no C22 C21 H21A 126.00 . . . no Fe1 C22 H22A 127.00 . . . no C21 C22 H22A 126.00 . . . no C23 C22 H22A 126.00 . . . no Fe1 C23 H23A 126.00 . . . no C19 C23 H23A 126.00 . . . no C22 C23 H23A 126.00 . . . no C25 C26 H26A 121.00 . . . no C27 C26 H26A 121.00 . . . no C26 C27 H27A 121.00 . . . no C28 C27 H27A 120.00 . . . no N4 C28 H28A 118.00 . . . no C27 C28 H28A 118.00 . . . no C32 C33 H33A 121.00 . . . no C34 C33 H33A 121.00 . . . no C33 C34 H34A 121.00 . . . no C35 C34 H34A 121.00 . . . no C34 C35 H35A 120.00 . . . no C36 C35 H35A 121.00 . . . no N6 C36 H36A 118.00 . . . no C35 C36 H36A 118.00 . . . no Cl1 C37 Cl2 111.5(2) . . . no Cl1 C37 Cl3 110.8(2) . . . no Cl2 C37 Cl3 110.2(2) . . . no Cl1 C37 H37A 108.00 . . . no Cl2 C37 H37A 108.00 . . . no Cl3 C37 H37A 108.00 . . . no Cl4 C38 Cl5 110.22(18) . . . no Cl4 C38 Cl6 110.28(19) . . . no Cl5 C38 Cl6 110.67(18) . . . no Cl4 C38 H38A 109.00 . . . no Cl5 C38 H38A 109.00 . . . no Cl6 C38 H38A 109.00 . . . no 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 C2 Fe1 C1 C5 119.3(3) . . . . no C2 Fe1 C1 C6 -122.2(3) . . . . no C3 Fe1 C1 C2 -37.5(2) . . . . no C3 Fe1 C1 C5 81.8(2) . . . . no C3 Fe1 C1 C6 -159.8(3) . . . . no C4 Fe1 C1 C2 -81.2(2) . . . . no C4 Fe1 C1 C5 38.1(2) . . . . no C4 Fe1 C1 C6 156.6(3) . . . . no C5 Fe1 C1 C2 -119.3(3) . . . . no C5 Fe1 C1 C6 118.5(3) . . . . no C19 Fe1 C1 C2 -166.4(3) . . . . no C19 Fe1 C1 C5 -47.1(4) . . . . no C19 Fe1 C1 C6 71.3(4) . . . . no C20 Fe1 C1 C2 158.9(2) . . . . no C20 Fe1 C1 C5 -81.8(2) . . . . no C20 Fe1 C1 C6 36.6(3) . . . . no C21 Fe1 C1 C2 116.3(2) . . . . no C21 Fe1 C1 C5 -124.4(2) . . . . no C21 Fe1 C1 C6 -6.0(3) . . . . no C22 Fe1 C1 C2 75.0(2) . . . . no C22 Fe1 C1 C5 -165.7(2) . . . . no C22 Fe1 C1 C6 -47.2(3) . . . . no C1 Fe1 C2 C3 -118.7(3) . . . . no C3 Fe1 C2 C1 118.7(3) . . . . no C4 Fe1 C2 C1 81.7(2) . . . . no C4 Fe1 C2 C3 -37.0(2) . . . . no C5 Fe1 C2 C1 37.88(18) . . . . no C5 Fe1 C2 C3 -80.8(2) . . . . no C20 Fe1 C2 C1 -49.3(4) . . . . no C20 Fe1 C2 C3 -168.0(3) . . . . no C21 Fe1 C2 C1 -82.4(2) . . . . no C21 Fe1 C2 C3 158.9(2) . . . . no C22 Fe1 C2 C1 -124.47(19) . . . . no C22 Fe1 C2 C3 116.8(2) . . . . no C23 Fe1 C2 C1 -165.71(18) . . . . no C23 Fe1 C2 C3 75.6(2) . . . . no C1 Fe1 C3 C2 38.4(2) . . . . no C1 Fe1 C3 C4 -82.0(2) . . . . no C2 Fe1 C3 C4 -120.4(3) . . . . no C4 Fe1 C3 C2 120.4(3) . . . . no C5 Fe1 C3 C2 82.9(2) . . . . no C5 Fe1 C3 C4 -37.5(2) . . . . no C19 Fe1 C3 C2 -164.3(2) . . . . no C19 Fe1 C3 C4 75.3(2) . . . . no C21 Fe1 C3 C2 -47.3(4) . . . . no C21 Fe1 C3 C4 -167.7(3) . . . . no C22 Fe1 C3 C2 -80.9(2) . . . . no C22 Fe1 C3 C4 158.7(2) . . . . no C23 Fe1 C3 C2 -122.8(2) . . . . no C23 Fe1 C3 C4 116.8(2) . . . . no C1 Fe1 C4 C3 81.2(2) . . . . no C1 Fe1 C4 C5 -38.5(2) . . . . no C2 Fe1 C4 C3 36.8(2) . . . . no C2 Fe1 C4 C5 -82.9(2) . . . . no C3 Fe1 C4 C5 -119.7(3) . . . . no C5 Fe1 C4 C3 119.7(3) . . . . no C19 Fe1 C4 C3 -124.0(2) . . . . no C19 Fe1 C4 C5 116.4(2) . . . . no C20 Fe1 C4 C3 -165.61(19) . . . . no C20 Fe1 C4 C5 74.7(3) . . . . no C22 Fe1 C4 C3 -47.8(4) . . . . no C22 Fe1 C4 C5 -167.5(3) . . . . no C23 Fe1 C4 C3 -80.9(2) . . . . no C23 Fe1 C4 C5 159.4(2) . . . . no C1 Fe1 C5 C4 118.3(3) . . . . no C2 Fe1 C5 C1 -37.84(18) . . . . no C2 Fe1 C5 C4 80.5(2) . . . . no C3 Fe1 C5 C1 -81.0(2) . . . . no C3 Fe1 C5 C4 37.3(2) . . . . no C4 Fe1 C5 C1 -118.3(3) . . . . no C19 Fe1 C5 C1 159.82(18) . . . . no C19 Fe1 C5 C4 -81.9(2) . . . . no C20 Fe1 C5 C1 116.80(19) . . . . no C20 Fe1 C5 C4 -124.9(2) . . . . no C21 Fe1 C5 C1 75.6(2) . . . . no C21 Fe1 C5 C4 -166.2(2) . . . . no C23 Fe1 C5 C1 -165.1(3) . . . . no C23 Fe1 C5 C4 -46.8(4) . . . . no C1 Fe1 C19 C20 -48.2(4) . . . . no C1 Fe1 C19 C23 -167.4(3) . . . . no C1 Fe1 C19 C24 70.7(4) . . . . no C3 Fe1 C19 C20 -166.0(2) . . . . no C3 Fe1 C19 C23 74.8(2) . . . . no C3 Fe1 C19 C24 -47.2(4) . . . . no C4 Fe1 C19 C20 -124.9(2) . . . . no C4 Fe1 C19 C23 115.9(2) . . . . no C4 Fe1 C19 C24 -6.0(3) . . . . no C5 Fe1 C19 C20 -82.2(2) . . . . no C5 Fe1 C19 C23 158.59(18) . . . . no C5 Fe1 C19 C24 36.7(4) . . . . no C20 Fe1 C19 C23 -119.2(3) . . . . no C20 Fe1 C19 C24 118.9(4) . . . . no C21 Fe1 C19 C20 37.7(2) . . . . no C21 Fe1 C19 C23 -81.5(2) . . . . no C21 Fe1 C19 C24 156.6(4) . . . . no C22 Fe1 C19 C20 81.4(2) . . . . no C22 Fe1 C19 C23 -37.83(19) . . . . no C22 Fe1 C19 C24 -159.8(3) . . . . no C23 Fe1 C19 C20 119.2(3) . . . . no C23 Fe1 C19 C24 -121.9(4) . . . . no C1 Fe1 C20 C19 159.4(2) . . . . no C1 Fe1 C20 C21 -81.7(2) . . . . no C2 Fe1 C20 C19 -165.2(3) . . . . no C2 Fe1 C20 C21 -46.2(4) . . . . no C4 Fe1 C20 C19 74.9(3) . . . . no C4 Fe1 C20 C21 -166.2(2) . . . . no C5 Fe1 C20 C19 116.2(2) . . . . no C5 Fe1 C20 C21 -124.8(2) . . . . no C19 Fe1 C20 C21 119.0(3) . . . . no C21 Fe1 C20 C19 -119.0(3) . . . . no C22 Fe1 C20 C19 -81.4(2) . . . . no C22 Fe1 C20 C21 37.6(2) . . . . no C23 Fe1 C20 C19 -37.9(2) . . . . no C23 Fe1 C20 C21 81.1(2) . . . . no C1 Fe1 C21 C20 116.8(2) . . . . no C1 Fe1 C21 C22 -124.1(2) . . . . no C2 Fe1 C21 C20 160.0(2) . . . . no C2 Fe1 C21 C22 -80.8(2) . . . . no C3 Fe1 C21 C20 -166.7(3) . . . . no C3 Fe1 C21 C22 -47.5(4) . . . . no C5 Fe1 C21 C20 74.7(2) . . . . no C5 Fe1 C21 C22 -166.1(2) . . . . no C19 Fe1 C21 C20 -38.1(2) . . . . no C19 Fe1 C21 C22 81.1(2) . . . . no C20 Fe1 C21 C22 119.2(3) . . . . no C22 Fe1 C21 C20 -119.2(3) . . . . no C23 Fe1 C21 C20 -82.3(2) . . . . no C23 Fe1 C21 C22 36.9(2) . . . . no C1 Fe1 C22 C21 75.4(2) . . . . no C1 Fe1 C22 C23 -164.2(2) . . . . no C2 Fe1 C22 C21 117.1(2) . . . . no C2 Fe1 C22 C23 -122.4(2) . . . . no C3 Fe1 C22 C21 158.9(2) . . . . no C3 Fe1 C22 C23 -80.6(2) . . . . no C4 Fe1 C22 C21 -167.3(3) . . . . no C4 Fe1 C22 C23 -46.8(4) . . . . no C19 Fe1 C22 C21 -82.0(2) . . . . no C19 Fe1 C22 C23 38.4(2) . . . . no C20 Fe1 C22 C21 -37.7(2) . . . . no C20 Fe1 C22 C23 82.7(2) . . . . no C21 Fe1 C22 C23 120.5(3) . . . . no C23 Fe1 C22 C21 -120.5(3) . . . . no C2 Fe1 C23 C19 -165.24(18) . . . . no C2 Fe1 C23 C22 76.3(2) . . . . no C3 Fe1 C23 C19 -124.46(19) . . . . no C3 Fe1 C23 C22 117.1(2) . . . . no C4 Fe1 C23 C19 -82.4(2) . . . . no C4 Fe1 C23 C22 159.1(2) . . . . no C5 Fe1 C23 C19 -49.1(4) . . . . no C5 Fe1 C23 C22 -167.6(3) . . . . no C19 Fe1 C23 C22 -118.5(3) . . . . no C20 Fe1 C23 C19 37.83(19) . . . . no C20 Fe1 C23 C22 -80.7(2) . . . . no C21 Fe1 C23 C19 81.6(2) . . . . no C21 Fe1 C23 C22 -36.9(2) . . . . no C22 Fe1 C23 C19 118.5(3) . . . . no C7 O2 C6 O1 -10.7(4) . . . . no C7 O2 C6 C1 171.1(2) . . . . no C6 O2 C7 C8 111.8(3) . . . . no C6 O2 C7 C11 -73.4(3) . . . . no C25 O6 C24 O5 -11.0(5) . . . . no C25 O6 C24 C19 170.2(3) . . . . no C24 O6 C25 C26 112.8(3) . . . . no C24 O6 C25 C29 -74.5(4) . . . . no C11 N1 C10 C9 1.0(5) . . . . no C10 N1 C11 C7 -0.8(4) . . . . no C10 N1 C11 C12 -179.1(3) . . . . no C13 N2 C12 O3 2.3(5) . . . . no C13 N2 C12 C11 -179.0(3) . . . . no C12 N2 C13 O4 6.6(5) . . . . no C12 N2 C13 C14 -171.9(3) . . . . no C18 N3 C14 C13 177.3(3) . . . . no C18 N3 C14 C15 -1.9(5) . . . . no C14 N3 C18 C17 0.5(5) . . . . no C29 N4 C28 C27 -1.1(5) . . . . no C28 N4 C29 C25 0.3(4) . . . . no C28 N4 C29 C30 -179.3(3) . . . . no C31 N5 C30 O7 7.8(6) . . . . no C31 N5 C30 C29 -173.4(3) . . . . no C30 N5 C31 O8 9.1(5) . . . . no C30 N5 C31 C32 -171.4(3) . . . . no C36 N6 C32 C31 176.7(3) . . . . no C36 N6 C32 C33 -1.9(5) . . . . no C32 N6 C36 C35 0.2(5) . . . . no Fe1 C1 C2 C3 59.8(2) . . . . no C5 C1 C2 Fe1 -59.9(2) . . . . no C5 C1 C2 C3 -0.1(4) . . . . no C6 C1 C2 Fe1 118.7(3) . . . . no C6 C1 C2 C3 178.5(3) . . . . no Fe1 C1 C5 C4 -59.6(2) . . . . no C2 C1 C5 Fe1 59.8(2) . . . . no C2 C1 C5 C4 0.3(4) . . . . no C6 C1 C5 Fe1 -118.8(3) . . . . no C6 C1 C5 C4 -178.4(3) . . . . no Fe1 C1 C6 O1 -101.1(4) . . . . no Fe1 C1 C6 O2 77.0(3) . . . . no C2 C1 C6 O1 168.7(3) . . . . no C2 C1 C6 O2 -13.2(4) . . . . no C5 C1 C6 O1 -12.9(5) . . . . no C5 C1 C6 O2 165.2(3) . . . . no Fe1 C2 C3 C4 58.9(2) . . . . no C1 C2 C3 Fe1 -59.0(2) . . . . no C1 C2 C3 C4 -0.1(4) . . . . no Fe1 C3 C4 C5 59.1(2) . . . . no C2 C3 C4 Fe1 -58.9(2) . . . . no C2 C3 C4 C5 0.3(4) . . . . no Fe1 C4 C5 C1 58.9(2) . . . . no C3 C4 C5 Fe1 -59.3(2) . . . . no C3 C4 C5 C1 -0.3(4) . . . . no O2 C7 C8 C9 176.1(3) . . . . no C11 C7 C8 C9 1.0(5) . . . . no O2 C7 C11 N1 -175.0(2) . . . . no O2 C7 C11 C12 3.2(4) . . . . no C8 C7 C11 N1 -0.2(4) . . . . no C8 C7 C11 C12 178.0(3) . . . . no C7 C8 C9 C10 -0.8(6) . . . . no C8 C9 C10 N1 -0.2(6) . . . . no N1 C11 C12 O3 177.1(3) . . . . no N1 C11 C12 N2 -1.6(3) . . . . no C7 C11 C12 O3 -1.2(4) . . . . no C7 C11 C12 N2 -179.9(2) . . . . no O4 C13 C14 N3 -175.5(3) . . . . no O4 C13 C14 C15 3.8(4) . . . . no N2 C13 C14 N3 3.0(3) . . . . no N2 C13 C14 C15 -177.7(3) . . . . no N3 C14 C15 C16 1.9(5) . . . . no C13 C14 C15 C16 -177.4(3) . . . . no C14 C15 C16 C17 -0.3(6) . . . . no C15 C16 C17 C18 -1.0(6) . . . . no C16 C17 C18 N3 1.0(6) . . . . no Fe1 C19 C20 C21 -59.4(2) . . . . no C23 C19 C20 Fe1 60.0(2) . . . . no C23 C19 C20 C21 0.6(4) . . . . no C24 C19 C20 Fe1 -118.2(3) . . . . no C24 C19 C20 C21 -177.6(3) . . . . no Fe1 C19 C23 C22 60.2(2) . . . . no C20 C19 C23 Fe1 -60.0(2) . . . . no C20 C19 C23 C22 0.2(4) . . . . no C24 C19 C23 Fe1 118.2(3) . . . . no C24 C19 C23 C22 178.3(3) . . . . no Fe1 C19 C24 O5 -96.0(4) . . . . no Fe1 C19 C24 O6 82.7(3) . . . . no C20 C19 C24 O5 -7.9(5) . . . . no C20 C19 C24 O6 170.8(3) . . . . no C23 C19 C24 O5 174.3(3) . . . . no C23 C19 C24 O6 -7.1(4) . . . . no Fe1 C20 C21 C22 -60.0(2) . . . . no C19 C20 C21 Fe1 58.8(2) . . . . no C19 C20 C21 C22 -1.2(4) . . . . no Fe1 C21 C22 C23 -58.2(2) . . . . no C20 C21 C22 Fe1 59.5(2) . . . . no C20 C21 C22 C23 1.3(4) . . . . no Fe1 C22 C23 C19 -59.1(2) . . . . no C21 C22 C23 Fe1 58.2(2) . . . . no C21 C22 C23 C19 -0.9(4) . . . . no O6 C25 C26 C27 171.5(3) . . . . no C29 C25 C26 C27 -1.4(4) . . . . no O6 C25 C29 N4 -171.7(3) . . . . no O6 C25 C29 C30 8.0(4) . . . . no C26 C25 C29 N4 0.9(4) . . . . no C26 C25 C29 C30 -179.4(3) . . . . no C25 C26 C27 C28 0.7(5) . . . . no C26 C27 C28 N4 0.6(6) . . . . no N4 C29 C30 O7 -178.1(3) . . . . no N4 C29 C30 N5 3.1(4) . . . . no C25 C29 C30 O7 2.3(5) . . . . no C25 C29 C30 N5 -176.6(3) . . . . no O8 C31 C32 N6 178.0(3) . . . . no O8 C31 C32 C33 -3.3(4) . . . . no N5 C31 C32 N6 -1.4(4) . . . . no N5 C31 C32 C33 177.2(3) . . . . no N6 C32 C33 C34 3.2(5) . . . . no C31 C32 C33 C34 -175.3(3) . . . . no C32 C33 C34 C35 -2.7(6) . . . . no C33 C34 C35 C36 1.1(6) . . . . no C34 C35 C36 N6 0.2(6) . . . . no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # N2 H2N N1 0.85(4) 2.17(5) 2.611(4) 112(3) . yes N2 H2N N3 0.85(4) 2.18(4) 2.623(4) 113(4) . yes N5 H5N N4 0.83(4) 2.17(5) 2.599(4) 112(3) . yes N5 H5N N6 0.83(4) 2.21(4) 2.627(4) 111(4) . y C3 H3A Cl5 0.9500 2.8300 3.579(4) 137.00 2_555 no C8 H8A O8 0.9500 2.3700 3.225(4) 149.00 2_645 no C17 H17A Cl5 0.9500 2.7900 3.542(4) 136.00 2_545 no C18 H18A Cl1 0.9500 2.8200 3.749(4) 166.00 2_645 no C26 H26A O4 0.9500 2.5800 3.383(4) 143.00 2_555 no C35 H35A Cl3 0.9500 2.8200 3.701(4) 154.00 1_565 no C36 H36A Cl6 0.9500 2.7600 3.706(4) 176.00 1_565 no C37 H37A O7 1.0000 2.5700 3.314(5) 131.00 2_645 no C37 H37A O8 1.0000 2.3700 3.186(5) 138.00 2_645 no C38 H38A O3 1.0000 2.3500 3.162(4) 138.00 4_554 no C38 H38A O4 1.0000 2.4000 3.150(5) 131.00 4_554 no _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.427 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.061 # Attachment '9968_web_deposit_cif_file_2_HelenStoeckli-Evans_1331020702.3_Cu2L12(I)2.cif' data_Cu2L12(I)2 _database_code_depnum_ccdc_archive 'CCDC 870329' #TrackingRef '9968_web_deposit_cif_file_2_HelenStoeckli-Evans_1331020702.3_Cu2L12(I)2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H32 Cu2 Fe2 I2 N6 O8, C2 H3 N' _chemical_formula_sum 'C48 H35 Cu2 Fe2 I2 N7 O8' _chemical_formula_weight 1330.41 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' Cu Cu 0.3201 1.2651 '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' I I -0.4742 1.8119 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 20.0421(16) _cell_length_b 14.6971(7) _cell_length_c 15.7895(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.747(6) _cell_angle_gamma 90.00 _cell_volume 4608.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 29002 _cell_measurement_theta_max 27.15 _cell_measurement_theta_min 1.50 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 2.931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'plane graphite' _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_measurement_method '\f + \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 27902 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.10 _reflns_number_total 8212 _reflns_number_gt 5815 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2002)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED32 (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009) and Mercury (Macrae et al., 2006)' _computing_publication_material 'SHELXL-97, PLATON and Publcif (Westrip, 2010)' _refine_special_details ; Squeeze routine in PLATON (Spek, 2009) Total Potential Solvent Accessible Void Vol = 295.2 \%A^3^ Electron Count / Cell = 100 - included in D(calc), F000 & Mol.Wght. Equated to one molecule of CH~3~CN per molecule of complex. Distance restraints used for the disordered O-C=O group of atoms in part of the molecule: DFIX 1.47 .02 C44 C43B DFIX 1.20 .02 C43B O8B The C-bound H-atoms were included in calculated positions and treated as riding atoms: C-H = 0.95 \%A, with U~iso~(H) = 1.2U~eq~(parent C-atom). ; _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^)+(0.0676P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00126(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8212 _refine_ls_number_parameters 624 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I Uani 0.15116(2) -0.60548(3) 0.29664(2) 1.000 0.0407(1) d . . . I2 I Uani 0.24237(3) -0.39927(3) 0.45798(3) 1.000 0.0533(2) d . . . Cu1 Cu Uani 0.10499(4) -0.49766(5) 0.40489(4) 1.000 0.0328(2) d . . . Cu2 Cu Uani 0.29925(4) -0.49329(5) 0.35000(4) 1.000 0.0390(2) d . . . Fe1 Fe Uani 0.13700(4) -0.49526(6) 0.95711(5) 1.000 0.0343(3) d . . . Fe2 Fe Uani 0.41936(5) -1.05449(7) 0.29316(6) 1.000 0.0464(3) d . A . O1 O Uani -0.0020(2) -0.2910(3) 0.4891(3) 1.000 0.0427(14) d . . . O2 O Uani 0.0399(3) -0.4140(4) 0.6233(3) 1.000 0.077(2) d . . . O3 O Uani 0.1055(2) -0.5357(3) 0.7350(2) 1.000 0.0395(13) d . . . O4 O Uani 0.1910(3) -0.4347(3) 0.7373(3) 1.000 0.0508(16) d . . . O5 O Uani 0.3725(2) -0.5534(3) 0.1304(2) 1.000 0.0444(16) d . . . O6 O Uani 0.3651(4) -0.7119(4) 0.2327(3) 1.000 0.091(3) d . . . O7A O Uani 0.3937(6) -0.8287(7) 0.3683(7) 0.584(12) 0.046(3) d P A 1 O8A O Uani 0.2897(4) -0.8575(6) 0.3039(5) 0.584(12) 0.059(3) d P A 1 N1 N Uani 0.0693(2) -0.3990(3) 0.3222(3) 1.000 0.0341(16) d . . . N2 N Uani 0.0611(3) -0.4233(3) 0.4829(3) 1.000 0.0356(16) d . . . N3 N Uani 0.1270(3) -0.5748(3) 0.5115(3) 1.000 0.0350(16) d . . . N4 N Uani 0.2877(3) -0.4017(3) 0.2537(3) 1.000 0.0368(17) d . . . N5 N Uani 0.3375(3) -0.5648(3) 0.2651(3) 1.000 0.0403(16) d . . . N6 N Uani 0.3247(3) -0.6052(4) 0.4204(3) 1.000 0.0450(18) d . . . C1 C Uani 0.0776(3) -0.3893(4) 0.2385(3) 1.000 0.0388(19) d . . . C2 C Uani 0.0491(3) -0.3177(5) 0.1906(4) 1.000 0.044(2) d . . . C3 C Uani 0.0110(3) -0.2544(4) 0.2260(4) 1.000 0.0393(19) d . . . C4 C Uani 0.0021(3) -0.2638(4) 0.3108(4) 1.000 0.0387(19) d . . . C5 C Uani 0.0331(3) -0.3357(4) 0.3575(3) 1.000 0.0349(17) d . . . C6 C Uani 0.0277(3) -0.3471(4) 0.4510(4) 1.000 0.0375(19) d . . . C7 C Uani 0.0663(4) -0.4490(4) 0.5661(4) 1.000 0.044(2) d . . . C8 C Uani 0.1075(3) -0.5344(4) 0.5818(3) 1.000 0.0340(17) d . . . C9 C Uani 0.1251(3) -0.5745(4) 0.6612(3) 1.000 0.0373(19) d . . . C10 C Uani 0.1596(3) -0.6545(4) 0.6698(3) 1.000 0.0412(19) d . . . C11 C Uani 0.1777(3) -0.6958(4) 0.5973(4) 1.000 0.0430(19) d . . . C12 C Uani 0.1608(3) -0.6524(4) 0.5193(4) 1.000 0.0391(19) d . . . C13 C Uani 0.1431(3) -0.4633(4) 0.7678(3) 1.000 0.0360(18) d . . . C14 C Uani 0.1187(3) -0.4277(4) 0.8448(3) 1.000 0.0364(19) d . . . C15 C Uani 0.1577(3) -0.3722(4) 0.9062(4) 1.000 0.040(2) d . . . C16 C Uani 0.1206(3) -0.3584(5) 0.9747(4) 1.000 0.042(2) d . . . C17 C Uani 0.0586(3) -0.4067(4) 0.9572(4) 1.000 0.041(2) d . . . C18 C Uani 0.0565(3) -0.4489(4) 0.8761(3) 1.000 0.0358(17) d . . . C19 C Uani 0.1881(3) -0.5479(5) 1.0673(4) 1.000 0.045(2) d . . . C20 C Uani 0.1251(3) -0.5923(5) 1.0466(4) 1.000 0.050(2) d . . . C21 C Uani 0.1238(4) -0.6321(5) 0.9661(4) 1.000 0.054(2) d . . . C22 C Uani 0.1845(4) -0.6139(5) 0.9364(4) 1.000 0.055(2) d . . . C23 C Uani 0.2263(3) -0.5605(5) 0.9990(4) 1.000 0.049(2) d . . . C31 C Uani 0.2568(4) -0.3197(5) 0.2496(5) 1.000 0.052(2) d . . . C32 C Uani 0.2582(4) -0.2628(5) 0.1792(5) 1.000 0.058(3) d . . . C33 C Uani 0.2928(4) -0.2900(5) 0.1144(4) 1.000 0.062(3) d . . . C34 C Uani 0.3235(4) -0.3724(5) 0.1179(4) 1.000 0.050(2) d . . . C35 C Uani 0.3187(3) -0.4286(4) 0.1878(3) 1.000 0.0356(17) d . . . C36 C Uani 0.3463(3) -0.5228(4) 0.1908(4) 1.000 0.0396(19) d . . . C37 C Uani 0.3496(4) -0.6542(5) 0.2812(4) 1.000 0.051(2) d . . . C38 C Uani 0.3435(4) -0.6752(5) 0.3742(4) 1.000 0.051(2) d . A . C39 C Uani 0.3591(5) -0.7601(5) 0.4131(4) 1.000 0.063(3) d . . . C40 C Uani 0.3573(5) -0.7709(6) 0.5003(5) 1.000 0.069(3) d . A . C41 C Uani 0.3403(4) -0.6974(6) 0.5455(4) 1.000 0.064(3) d . . . C42 C Uani 0.3239(4) -0.6169(5) 0.5047(4) 1.000 0.054(3) d . A . C43A C Uani 0.3492(7) -0.8702(8) 0.3081(10) 0.584(12) 0.045(4) d P A 1 C44 C Uani 0.3926(7) -0.9253(7) 0.2601(6) 1.000 0.086(4) d D . . C45 C Uani 0.4593(5) -0.9437(6) 0.2442(5) 1.000 0.075(3) d . A . C46 C Uani 0.4572(5) -1.0134(6) 0.1857(5) 1.000 0.068(3) d . . . C47 C Uani 0.3909(6) -1.0397(7) 0.1652(5) 1.000 0.083(4) d . A . C48 C Uani 0.3508(5) -0.9877(9) 0.2102(8) 1.000 0.098(5) d . A . C49 C Uani 0.4754(4) -1.0851(5) 0.4074(4) 1.000 0.050(2) d . . . C50 C Uani 0.4088(4) -1.0729(5) 0.4182(5) 1.000 0.058(3) d . A . C51 C Uani 0.3696(4) -1.1376(6) 0.3664(5) 1.000 0.065(3) d . . . C52 C Uani 0.4136(4) -1.1892(6) 0.3219(5) 1.000 0.063(3) d . A . C53 C Uani 0.4792(4) -1.1564(5) 0.3472(5) 1.000 0.057(3) d . A . C43B C Uani 0.4136(10) -0.8489(13) 0.3269(12) 0.416(12) 0.052(7) d DP A 2 O7B O Uani 0.3527(8) -0.8384(9) 0.3620(10) 0.416(12) 0.042(4) d P A 2 O8B O Uani 0.4596(6) -0.7982(8) 0.3570(8) 0.416(12) 0.059(5) d DP A 2 H1 H Uiso 0.10350 -0.43290 0.21270 1.000 0.0470 c R . . H10 H Uiso 0.17110 -0.68160 0.72440 1.000 0.0490 c R . . H11 H Uiso 0.20090 -0.75230 0.60080 1.000 0.0510 c R . . H12 H Uiso 0.17410 -0.67940 0.46950 1.000 0.0470 c R . . H15 H Uiso 0.20140 -0.34900 0.90190 1.000 0.0480 d R . . H16 H Uiso 0.13440 -0.32250 1.02400 1.000 0.0510 d R . . H17 H Uiso 0.02470 -0.41040 0.99370 1.000 0.0490 d R . . H18 H Uiso 0.02070 -0.48460 0.84780 1.000 0.0430 d R . . H19 H Uiso 0.20230 -0.51510 1.11840 1.000 0.0540 d R . . H20 H Uiso 0.08990 -0.59400 1.08120 1.000 0.0590 d R . . H21 H Uiso 0.08780 -0.66670 0.93680 1.000 0.0640 d R . . H22 H Uiso 0.19650 -0.63320 0.88300 1.000 0.0650 d R . . H23 H Uiso 0.27040 -0.53860 0.99530 1.000 0.0590 d R . . H31A H Uiso 0.23380 -0.30060 0.29540 1.000 0.0620 c R . . H32 H Uiso 0.23540 -0.20600 0.17610 1.000 0.0690 c R . . H33 H Uiso 0.29540 -0.25100 0.06690 1.000 0.0750 c R . . H34 H Uiso 0.34780 -0.39150 0.07340 1.000 0.0590 c R . . H40 H Uiso 0.36760 -0.82780 0.52750 1.000 0.0830 c R . . H41 H Uiso 0.33990 -0.70210 0.60540 1.000 0.0770 c R A . H42 H Uiso 0.31130 -0.56700 0.53730 1.000 0.0640 c R . . H45 H Uiso 0.49820 -0.91190 0.26980 1.000 0.0900 d R . . H46 H Uiso 0.49490 -1.03860 0.16360 1.000 0.0820 d R A . H47 H Uiso 0.37590 -1.08700 0.12620 1.000 0.0990 d R . . H48 H Uiso 0.30330 -0.99340 0.20720 1.000 0.1170 d R . . H49 H Uiso 0.51250 -1.05200 0.43610 1.000 0.0600 d R A . H50 H Uiso 0.39190 -1.02840 0.45340 1.000 0.0690 d R . . H51 H Uiso 0.32220 -1.14560 0.36260 1.000 0.0780 d R A . H52 H Uiso 0.40090 -1.23670 0.28210 1.000 0.0750 d R . . H53 H Uiso 0.51900 -1.17790 0.32730 1.000 0.0680 d R . . H2 H Uiso 0.05590 -0.31210 0.13240 1.000 0.0530 c R . . H3 H Uiso -0.00890 -0.20500 0.19290 1.000 0.0470 c R . . H4 H Uiso -0.02490 -0.22170 0.33670 1.000 0.0460 c 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 I1 0.0625(3) 0.0358(2) 0.0252(2) -0.0070(2) 0.0116(2) 0.0027(2) I2 0.0738(3) 0.0458(3) 0.0423(2) -0.0166(2) 0.0153(2) -0.0085(2) Cu1 0.0505(4) 0.0285(4) 0.0207(3) -0.0023(3) 0.0099(3) 0.0012(3) Cu2 0.0520(4) 0.0369(4) 0.0285(4) -0.0021(3) 0.0070(3) 0.0014(3) Fe1 0.0401(5) 0.0402(5) 0.0223(4) -0.0020(3) 0.0033(3) -0.0008(4) Fe2 0.0512(6) 0.0461(6) 0.0417(5) 0.0023(4) 0.0053(4) 0.0014(4) O1 0.061(3) 0.032(2) 0.039(2) 0.0027(19) 0.021(2) 0.006(2) O2 0.138(5) 0.065(4) 0.031(2) -0.002(2) 0.025(3) 0.046(4) O3 0.058(3) 0.040(2) 0.0212(18) -0.0063(17) 0.0084(17) -0.013(2) O4 0.076(3) 0.043(3) 0.039(2) -0.009(2) 0.028(2) -0.017(2) O5 0.058(3) 0.044(3) 0.033(2) -0.0005(19) 0.0132(19) 0.008(2) O6 0.199(7) 0.036(3) 0.042(3) -0.004(2) 0.029(4) 0.029(4) O7A 0.048(7) 0.039(5) 0.047(6) 0.013(4) -0.005(5) -0.004(5) O8A 0.054(6) 0.060(6) 0.062(5) -0.003(4) 0.009(4) 0.001(4) N1 0.046(3) 0.032(3) 0.025(2) -0.001(2) 0.0077(19) -0.004(2) N2 0.056(3) 0.031(3) 0.021(2) -0.0003(19) 0.010(2) 0.000(2) N3 0.055(3) 0.030(3) 0.021(2) -0.0033(19) 0.009(2) -0.001(2) N4 0.046(3) 0.028(3) 0.036(3) -0.004(2) 0.004(2) -0.004(2) N5 0.060(3) 0.030(3) 0.032(2) 0.004(2) 0.010(2) 0.004(2) N6 0.069(4) 0.040(3) 0.026(2) -0.002(2) 0.007(2) -0.003(3) C1 0.052(4) 0.038(3) 0.027(3) 0.004(3) 0.008(2) 0.002(3) C2 0.052(4) 0.051(4) 0.029(3) 0.009(3) 0.004(3) -0.006(3) C3 0.046(4) 0.036(3) 0.036(3) 0.011(3) 0.006(3) -0.003(3) C4 0.047(4) 0.031(3) 0.039(3) 0.004(3) 0.009(3) 0.002(3) C5 0.049(3) 0.030(3) 0.027(3) -0.002(2) 0.010(2) -0.003(3) C6 0.052(4) 0.031(3) 0.031(3) 0.000(3) 0.011(3) -0.003(3) C7 0.067(4) 0.040(4) 0.026(3) -0.004(3) 0.012(3) 0.006(3) C8 0.050(3) 0.030(3) 0.024(3) -0.003(2) 0.012(2) -0.001(3) C9 0.061(4) 0.031(3) 0.022(3) -0.005(2) 0.013(3) -0.008(3) C10 0.065(4) 0.033(3) 0.025(3) 0.006(2) 0.004(3) -0.006(3) C11 0.068(4) 0.029(3) 0.033(3) -0.001(3) 0.010(3) 0.000(3) C12 0.060(4) 0.030(3) 0.028(3) -0.001(2) 0.008(3) 0.003(3) C13 0.055(4) 0.032(3) 0.021(2) 0.004(2) 0.005(2) 0.000(3) C14 0.053(4) 0.030(3) 0.027(3) -0.006(2) 0.008(2) 0.000(3) C15 0.048(4) 0.040(4) 0.032(3) -0.003(3) 0.006(3) -0.001(3) C16 0.051(4) 0.048(4) 0.028(3) -0.011(3) 0.006(3) -0.003(3) C17 0.047(4) 0.049(4) 0.029(3) -0.005(3) 0.008(2) 0.002(3) C18 0.044(3) 0.034(3) 0.029(3) 0.003(2) 0.003(2) 0.002(3) C19 0.053(4) 0.057(4) 0.025(3) 0.002(3) 0.003(3) -0.001(3) C20 0.046(4) 0.058(5) 0.042(3) 0.016(3) -0.003(3) -0.006(3) C21 0.055(4) 0.048(4) 0.052(4) 0.005(3) -0.014(3) 0.000(3) C22 0.075(5) 0.052(4) 0.034(3) -0.003(3) -0.003(3) 0.018(4) C23 0.046(4) 0.064(5) 0.037(3) 0.008(3) 0.006(3) 0.011(3) C31 0.059(4) 0.039(4) 0.056(4) -0.008(3) 0.004(3) 0.006(3) C32 0.077(5) 0.032(4) 0.062(4) 0.007(3) 0.000(4) 0.008(3) C33 0.098(6) 0.042(4) 0.044(4) 0.011(3) -0.001(4) 0.003(4) C34 0.068(4) 0.039(4) 0.041(3) 0.007(3) 0.006(3) -0.002(3) C35 0.046(3) 0.032(3) 0.028(3) -0.003(2) 0.002(2) -0.004(3) C36 0.052(4) 0.030(3) 0.035(3) -0.005(3) -0.001(3) 0.003(3) C37 0.075(5) 0.037(4) 0.043(3) -0.001(3) 0.011(3) 0.005(3) C38 0.081(5) 0.041(4) 0.030(3) 0.004(3) 0.002(3) -0.003(3) C39 0.110(6) 0.034(4) 0.043(4) 0.004(3) 0.007(4) 0.011(4) C40 0.108(7) 0.053(5) 0.043(4) 0.019(4) 0.001(4) 0.000(4) C41 0.091(6) 0.063(5) 0.037(4) 0.015(4) 0.001(4) 0.003(4) C42 0.082(5) 0.055(5) 0.024(3) -0.001(3) 0.005(3) -0.006(4) C43A 0.058(9) 0.024(6) 0.052(8) 0.004(6) 0.002(6) 0.003(5) C44 0.142(10) 0.065(6) 0.063(5) 0.022(5) 0.054(6) 0.041(6) C45 0.109(7) 0.057(5) 0.054(4) 0.018(4) -0.010(5) -0.027(5) C46 0.086(6) 0.066(6) 0.058(5) 0.020(4) 0.028(4) 0.019(5) C47 0.110(8) 0.082(7) 0.049(5) 0.012(4) -0.014(5) -0.017(6) C48 0.065(6) 0.129(10) 0.104(8) 0.081(8) 0.027(6) 0.027(6) C49 0.058(4) 0.050(4) 0.041(3) 0.004(3) 0.000(3) -0.005(3) C50 0.068(5) 0.052(4) 0.055(4) 0.009(4) 0.017(4) -0.001(4) C51 0.050(4) 0.072(6) 0.072(5) 0.021(4) 0.004(4) -0.007(4) C52 0.068(5) 0.053(5) 0.065(5) 0.002(4) 0.003(4) -0.014(4) C53 0.061(5) 0.049(4) 0.058(4) 0.000(3) 0.000(3) -0.002(3) C43B 0.037(11) 0.071(14) 0.050(11) 0.018(10) 0.013(9) -0.012(9) O7B 0.047(8) 0.025(6) 0.051(9) 0.006(6) -0.008(7) -0.009(6) O8B 0.057(8) 0.051(8) 0.066(8) -0.001(6) -0.003(6) -0.005(6) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.5914(8) . . yes I2 Cu1 3.1229(10) . . yes I2 Cu2 2.5768(9) . . yes Cu1 N1 2.017(5) . . yes Cu1 N2 1.944(5) . . yes Cu1 N3 2.028(5) . . yes Cu2 N4 2.021(5) . . yes Cu2 N5 1.941(5) . . yes Cu2 N6 2.012(6) . . yes Fe1 C14 2.022(5) . . yes Fe1 C15 2.044(6) . . yes Fe1 C16 2.063(7) . . yes Fe1 C17 2.041(6) . . yes Fe1 C18 2.036(6) . . yes Fe1 C19 2.048(6) . . yes Fe1 C20 2.044(7) . . yes Fe1 C21 2.036(7) . . yes Fe1 C22 2.034(8) . . yes Fe1 C23 2.059(6) . . yes Fe2 C44 2.022(11) . . yes Fe2 C45 2.014(9) . . yes Fe2 C46 2.041(9) . . yes Fe2 C47 2.036(8) . . yes Fe2 C48 2.021(12) . . yes Fe2 C49 2.042(7) . . yes Fe2 C50 2.032(8) . . yes Fe2 C51 2.033(8) . . yes Fe2 C52 2.038(9) . . yes Fe2 C53 2.033(8) . . yes O1 C6 1.222(7) . . yes O2 C7 1.220(9) . . yes O3 C9 1.400(6) . . yes O3 C13 1.365(7) . . yes O4 C13 1.206(8) . . yes O5 C36 1.234(7) . . yes O6 C37 1.211(9) . . yes O7A C39 1.460(14) . . yes O7A C43A 1.357(18) . . yes O7B C43B 1.42(3) . . yes O7B C39 1.401(16) . . yes O8A C43A 1.200(16) . . yes O8B C43B 1.23(2) . . yes N1 C1 1.362(7) . . yes N1 C5 1.346(7) . . yes N2 C7 1.357(8) . . yes N2 C6 1.366(8) . . yes N3 C8 1.362(7) . . yes N3 C12 1.324(8) . . yes N4 C31 1.353(9) . . yes N4 C35 1.341(7) . . yes N5 C37 1.354(9) . . yes N5 C36 1.358(8) . . yes N6 C38 1.344(9) . . yes N6 C42 1.344(8) . . yes C1 C2 1.375(9) . . no C2 C3 1.370(9) . . no C3 C4 1.381(9) . . no C4 C5 1.387(8) . . no C5 C6 1.504(8) . . no C7 C8 1.505(9) . . no C8 C9 1.387(7) . . no C9 C10 1.362(8) . . no C10 C11 1.387(8) . . no C11 C12 1.388(9) . . no C13 C14 1.467(7) . . no C14 C18 1.436(8) . . no C14 C15 1.418(8) . . no C15 C16 1.407(9) . . no C16 C17 1.425(9) . . no C17 C18 1.418(8) . . no C19 C20 1.420(9) . . no C19 C23 1.416(9) . . no C20 C21 1.396(9) . . no C21 C22 1.388(11) . . no C22 C23 1.439(10) . . no C31 C32 1.394(11) . . no C32 C33 1.371(11) . . no C33 C34 1.356(11) . . no C34 C35 1.392(8) . . no C35 C36 1.489(8) . . no C37 C38 1.522(9) . . no C38 C39 1.407(10) . . no C39 C40 1.391(10) . . no C40 C41 1.363(12) . . no C41 C42 1.366(11) . . no C43A C44 1.471(18) . . no C43B C44 1.56(2) . . no C44 C48 1.409(17) . . no C44 C45 1.419(17) . . no C45 C46 1.376(12) . . no C46 C47 1.380(15) . . no C47 C48 1.374(16) . . no C49 C50 1.380(11) . . no C49 C53 1.424(10) . . no C50 C51 1.420(11) . . no C51 C52 1.419(12) . . no C52 C53 1.407(11) . . no C1 H1 0.9500 . . no C2 H2 0.9500 . . no C3 H3 0.9500 . . no C4 H4 0.9500 . . no C10 H10 0.9500 . . no C11 H11 0.9500 . . no C12 H12 0.9500 . . no C15 H15 0.9500 . . no C16 H16 0.9500 . . no C17 H17 0.9500 . . no C18 H18 0.9500 . . no C19 H19 0.9500 . . no C20 H20 0.9500 . . no C21 H21 0.9500 . . no C22 H22 0.9500 . . no C23 H23 0.9500 . . no C31 H31A 0.9500 . . no C32 H32 0.9500 . . no C33 H33 0.9500 . . no C34 H34 0.9500 . . no C40 H40 0.9500 . . no C41 H41 0.9500 . . no C42 H42 0.9500 . . no C45 H45 0.9500 . . no C46 H46 0.9500 . . no C47 H47 0.9500 . . no C48 H48 0.9500 . . no C49 H49 0.9500 . . no C50 H50 0.9500 . . no C51 H51 0.9500 . . no C52 H52 0.9500 . . no C53 H53 0.9500 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I2 Cu2 91.53(3) . . . yes I1 Cu1 I2 94.58(3) . . . yes I1 Cu1 N1 98.03(13) . . . yes I1 Cu1 N2 173.84(17) . . . yes I1 Cu1 N3 98.54(14) . . . yes I2 Cu1 N1 93.66(12) . . . yes I2 Cu1 N2 91.58(17) . . . yes I2 Cu1 N3 87.18(16) . . . yes N1 Cu1 N2 81.64(19) . . . yes N1 Cu1 N3 163.3(2) . . . yes N2 Cu1 N3 81.7(2) . . . yes I2 Cu2 N4 97.16(15) . . . yes I2 Cu2 N5 177.00(17) . . . yes I2 Cu2 N6 100.06(15) . . . yes N4 Cu2 N5 81.8(2) . . . yes N4 Cu2 N6 162.8(2) . . . yes N5 Cu2 N6 81.1(2) . . . yes C14 Fe1 C15 40.8(2) . . . yes C14 Fe1 C16 68.0(2) . . . yes C14 Fe1 C17 68.8(2) . . . yes C14 Fe1 C18 41.4(2) . . . yes C14 Fe1 C19 160.3(3) . . . yes C14 Fe1 C20 157.6(2) . . . yes C14 Fe1 C21 122.4(2) . . . yes C14 Fe1 C22 108.3(2) . . . yes C14 Fe1 C23 123.9(2) . . . yes C15 Fe1 C16 40.1(2) . . . yes C15 Fe1 C17 68.5(2) . . . yes C15 Fe1 C18 69.1(2) . . . yes C15 Fe1 C19 124.3(3) . . . yes C15 Fe1 C20 159.7(3) . . . yes C15 Fe1 C21 159.5(3) . . . yes C15 Fe1 C22 124.8(3) . . . yes C15 Fe1 C23 108.9(3) . . . yes C16 Fe1 C17 40.7(2) . . . yes C16 Fe1 C18 68.4(2) . . . yes C16 Fe1 C19 108.9(3) . . . yes C16 Fe1 C20 123.5(3) . . . yes C16 Fe1 C21 158.3(3) . . . yes C16 Fe1 C22 160.7(3) . . . yes C16 Fe1 C23 123.9(3) . . . yes C17 Fe1 C18 40.7(2) . . . yes C17 Fe1 C19 122.5(3) . . . yes C17 Fe1 C20 106.4(3) . . . yes C17 Fe1 C21 121.5(3) . . . yes C17 Fe1 C22 157.5(3) . . . yes C17 Fe1 C23 158.9(3) . . . yes C18 Fe1 C19 157.4(2) . . . yes C18 Fe1 C20 120.8(2) . . . yes C18 Fe1 C21 106.0(3) . . . yes C18 Fe1 C22 122.3(3) . . . yes C18 Fe1 C23 159.8(2) . . . yes C19 Fe1 C20 40.6(3) . . . yes C19 Fe1 C21 67.8(3) . . . yes C19 Fe1 C22 67.8(3) . . . yes C19 Fe1 C23 40.3(2) . . . yes C20 Fe1 C21 40.0(3) . . . yes C20 Fe1 C22 67.3(3) . . . yes C20 Fe1 C23 68.3(3) . . . yes C21 Fe1 C22 39.9(3) . . . yes C21 Fe1 C23 68.5(3) . . . yes C22 Fe1 C23 41.2(3) . . . yes C44 Fe2 C45 41.2(5) . . . yes C44 Fe2 C46 67.9(4) . . . yes C44 Fe2 C47 67.3(4) . . . yes C44 Fe2 C48 40.8(5) . . . yes C44 Fe2 C49 122.0(4) . . . yes C44 Fe2 C50 108.5(4) . . . yes C44 Fe2 C51 125.3(4) . . . yes C44 Fe2 C52 161.6(5) . . . yes C44 Fe2 C53 157.1(4) . . . yes C45 Fe2 C46 39.7(3) . . . yes C45 Fe2 C47 66.8(4) . . . yes C45 Fe2 C48 68.2(4) . . . yes C45 Fe2 C49 108.5(3) . . . yes C45 Fe2 C50 125.4(3) . . . yes C45 Fe2 C51 162.7(3) . . . yes C45 Fe2 C52 155.3(4) . . . yes C45 Fe2 C53 120.9(4) . . . yes C46 Fe2 C47 39.6(4) . . . yes C46 Fe2 C48 67.3(4) . . . yes C46 Fe2 C49 125.3(3) . . . yes C46 Fe2 C50 161.1(3) . . . yes C46 Fe2 C51 156.4(3) . . . yes C46 Fe2 C52 120.7(3) . . . yes C46 Fe2 C53 107.6(3) . . . yes C47 Fe2 C48 39.6(5) . . . yes C47 Fe2 C49 161.3(4) . . . yes C47 Fe2 C50 157.9(4) . . . yes C47 Fe2 C51 122.4(4) . . . yes C47 Fe2 C52 107.9(4) . . . yes C47 Fe2 C53 124.5(4) . . . yes C48 Fe2 C49 157.6(4) . . . yes C48 Fe2 C50 122.9(4) . . . yes C48 Fe2 C51 108.5(4) . . . yes C48 Fe2 C52 124.2(4) . . . yes C48 Fe2 C53 160.2(4) . . . yes C49 Fe2 C50 39.6(3) . . . yes C49 Fe2 C51 67.6(3) . . . yes C49 Fe2 C52 68.3(3) . . . yes C49 Fe2 C53 40.9(3) . . . yes C50 Fe2 C51 40.9(3) . . . yes C50 Fe2 C52 68.8(3) . . . yes C50 Fe2 C53 68.1(3) . . . yes C51 Fe2 C52 40.8(3) . . . yes C51 Fe2 C53 68.0(3) . . . yes C52 Fe2 C53 40.4(3) . . . yes C9 O3 C13 115.5(4) . . . yes C39 O7A C43A 109.9(10) . . . yes C39 O7B C43B 107.4(13) . . . yes Cu1 N1 C1 128.7(4) . . . yes Cu1 N1 C5 113.1(4) . . . yes C1 N1 C5 118.2(5) . . . yes Cu1 N2 C6 117.9(4) . . . yes Cu1 N2 C7 118.3(4) . . . yes C6 N2 C7 123.7(5) . . . yes Cu1 N3 C12 127.6(4) . . . yes C8 N3 C12 120.0(5) . . . yes Cu1 N3 C8 112.3(4) . . . yes Cu2 N4 C35 111.7(4) . . . yes C31 N4 C35 118.9(5) . . . yes Cu2 N4 C31 129.4(5) . . . yes Cu2 N5 C37 118.3(4) . . . yes C36 N5 C37 124.2(5) . . . yes Cu2 N5 C36 117.4(4) . . . yes Cu2 N6 C42 128.0(5) . . . yes C38 N6 C42 118.8(6) . . . yes Cu2 N6 C38 113.2(4) . . . yes N1 C1 C2 121.2(5) . . . yes C1 C2 C3 120.6(6) . . . no C2 C3 C4 118.7(6) . . . no C3 C4 C5 119.0(5) . . . no N1 C5 C4 122.3(5) . . . yes C4 C5 C6 121.4(5) . . . no N1 C5 C6 116.3(5) . . . yes O1 C6 N2 128.2(6) . . . yes O1 C6 C5 120.8(5) . . . yes N2 C6 C5 110.9(5) . . . yes O2 C7 N2 127.9(6) . . . yes O2 C7 C8 120.9(6) . . . yes N2 C7 C8 111.1(5) . . . yes N3 C8 C9 119.0(5) . . . yes C7 C8 C9 124.8(5) . . . no N3 C8 C7 116.2(5) . . . yes O3 C9 C8 120.9(5) . . . yes C8 C9 C10 121.4(5) . . . no O3 C9 C10 117.7(4) . . . yes C9 C10 C11 118.8(5) . . . no C10 C11 C12 118.2(5) . . . no N3 C12 C11 122.6(6) . . . yes O3 C13 O4 123.3(5) . . . yes O3 C13 C14 111.3(5) . . . yes O4 C13 C14 125.4(5) . . . yes Fe1 C14 C13 120.7(4) . . . yes Fe1 C14 C15 70.4(3) . . . yes C13 C14 C15 123.9(5) . . . no C13 C14 C18 127.6(5) . . . no C15 C14 C18 108.3(5) . . . no Fe1 C14 C18 69.8(3) . . . yes Fe1 C15 C14 68.8(3) . . . yes Fe1 C15 C16 70.7(4) . . . yes C14 C15 C16 108.0(5) . . . no Fe1 C16 C15 69.3(4) . . . yes Fe1 C16 C17 68.8(4) . . . yes C15 C16 C17 108.4(6) . . . no Fe1 C17 C18 69.5(3) . . . yes C16 C17 C18 108.2(5) . . . no Fe1 C17 C16 70.5(4) . . . yes Fe1 C18 C17 69.8(3) . . . yes C14 C18 C17 107.1(5) . . . no Fe1 C18 C14 68.8(3) . . . yes Fe1 C19 C23 70.3(4) . . . yes C20 C19 C23 108.7(6) . . . no Fe1 C19 C20 69.6(4) . . . yes Fe1 C20 C19 69.8(4) . . . yes Fe1 C20 C21 69.7(4) . . . yes C19 C20 C21 108.0(6) . . . no Fe1 C21 C20 70.3(4) . . . yes Fe1 C21 C22 70.0(4) . . . yes C20 C21 C22 108.5(6) . . . no Fe1 C22 C23 70.4(4) . . . yes C21 C22 C23 109.2(6) . . . no Fe1 C22 C21 70.1(4) . . . yes Fe1 C23 C22 68.5(4) . . . yes C19 C23 C22 105.7(6) . . . no Fe1 C23 C19 69.4(4) . . . yes N4 C31 C32 121.0(7) . . . yes C31 C32 C33 119.1(7) . . . no C32 C33 C34 120.2(6) . . . no C33 C34 C35 118.9(6) . . . no N4 C35 C36 117.3(5) . . . yes C34 C35 C36 120.8(5) . . . no N4 C35 C34 121.9(6) . . . yes O5 C36 C35 120.6(5) . . . yes N5 C36 C35 111.0(5) . . . yes O5 C36 N5 128.3(5) . . . yes O6 C37 C38 122.0(7) . . . yes N5 C37 C38 110.0(6) . . . yes O6 C37 N5 128.0(6) . . . yes N6 C38 C37 115.7(6) . . . yes C37 C38 C39 124.0(6) . . . no N6 C38 C39 120.3(6) . . . yes O7A C39 C38 119.6(7) . . . yes C38 C39 C40 120.0(7) . . . no O7B C39 C38 118.6(8) . . . yes O7B C39 C40 117.6(9) . . . yes O7A C39 C40 118.6(8) . . . yes C39 C40 C41 118.0(8) . . . no C40 C41 C42 120.1(6) . . . no N6 C42 C41 122.9(7) . . . yes O7A C43A O8A 121.5(13) . . . yes O8A C43A C44 135.2(13) . . . yes O7A C43A C44 103.3(11) . . . yes O8B C43B C44 144.9(18) . . . yes O7B C43B O8B 115.1(16) . . . yes O7B C43B C44 100.1(14) . . . yes C43A C44 C45 146.4(11) . . . no Fe2 C44 C48 69.5(7) . . . yes Fe2 C44 C43B 117.6(9) . . . yes Fe2 C44 C43A 122.6(8) . . . yes Fe2 C44 C45 69.1(6) . . . yes C43B C44 C48 158.9(13) . . . no C43B C44 C45 94.7(11) . . . no C43A C44 C48 107.3(11) . . . no C45 C44 C48 106.3(9) . . . no Fe2 C45 C46 71.2(5) . . . yes C44 C45 C46 108.4(9) . . . no Fe2 C45 C44 69.7(6) . . . yes Fe2 C46 C45 69.1(5) . . . yes Fe2 C46 C47 70.0(5) . . . yes C45 C46 C47 107.9(9) . . . no Fe2 C47 C46 70.4(5) . . . yes Fe2 C47 C48 69.6(6) . . . yes C46 C47 C48 109.6(9) . . . no Fe2 C48 C47 70.8(6) . . . yes C44 C48 C47 107.8(10) . . . no Fe2 C48 C44 69.7(6) . . . yes C50 C49 C53 108.5(7) . . . no Fe2 C49 C50 69.8(4) . . . yes Fe2 C49 C53 69.2(4) . . . yes Fe2 C50 C51 69.6(5) . . . yes C49 C50 C51 108.1(7) . . . no Fe2 C50 C49 70.6(4) . . . yes Fe2 C51 C50 69.5(5) . . . yes Fe2 C51 C52 69.8(5) . . . yes C50 C51 C52 108.1(7) . . . no Fe2 C52 C51 69.4(5) . . . yes Fe2 C52 C53 69.6(5) . . . yes C51 C52 C53 107.2(7) . . . no Fe2 C53 C52 70.0(5) . . . yes C49 C53 C52 108.0(7) . . . no Fe2 C53 C49 69.9(4) . . . yes N1 C1 H1 119.00 . . . no C2 C1 H1 119.00 . . . no C1 C2 H2 120.00 . . . no C3 C2 H2 120.00 . . . no C2 C3 H3 121.00 . . . no C4 C3 H3 121.00 . . . no C3 C4 H4 121.00 . . . no C5 C4 H4 121.00 . . . no C9 C10 H10 121.00 . . . no C11 C10 H10 120.00 . . . no C10 C11 H11 121.00 . . . no C12 C11 H11 121.00 . . . no N3 C12 H12 119.00 . . . no C11 C12 H12 119.00 . . . no Fe1 C15 H15 126.00 . . . no C14 C15 H15 126.00 . . . no C16 C15 H15 126.00 . . . no Fe1 C16 H16 128.00 . . . no C15 C16 H16 126.00 . . . no C17 C16 H16 126.00 . . . no Fe1 C17 H17 125.00 . . . no C16 C17 H17 126.00 . . . no C18 C17 H17 126.00 . . . no Fe1 C18 H18 126.00 . . . no C14 C18 H18 126.00 . . . no C17 C18 H18 126.00 . . . no Fe1 C19 H19 126.00 . . . no C20 C19 H19 126.00 . . . no C23 C19 H19 126.00 . . . no Fe1 C20 H20 126.00 . . . no C19 C20 H20 126.00 . . . no C21 C20 H20 126.00 . . . no Fe1 C21 H21 126.00 . . . no C20 C21 H21 126.00 . . . no C22 C21 H21 126.00 . . . no Fe1 C22 H22 125.00 . . . no C21 C22 H22 125.00 . . . no C23 C22 H22 125.00 . . . no Fe1 C23 H23 127.00 . . . no C19 C23 H23 127.00 . . . no C22 C23 H23 127.00 . . . no N4 C31 H31A 120.00 . . . no C32 C31 H31A 120.00 . . . no C31 C32 H32 120.00 . . . no C33 C32 H32 120.00 . . . no C32 C33 H33 120.00 . . . no C34 C33 H33 120.00 . . . no C33 C34 H34 121.00 . . . no C35 C34 H34 121.00 . . . no C39 C40 H40 121.00 . . . no C41 C40 H40 121.00 . . . no C40 C41 H41 120.00 . . . no C42 C41 H41 120.00 . . . no N6 C42 H42 119.00 . . . no C41 C42 H42 119.00 . . . no Fe2 C45 H45 125.00 . . . no C44 C45 H45 125.00 . . . no C46 C45 H45 127.00 . . . no Fe2 C46 H46 126.00 . . . no C45 C46 H46 126.00 . . . no C47 C46 H46 126.00 . . . no Fe2 C47 H47 126.00 . . . no C46 C47 H47 125.00 . . . no C48 C47 H47 126.00 . . . no Fe2 C48 H48 125.00 . . . no C44 C48 H48 127.00 . . . no C47 C48 H48 125.00 . . . no Fe2 C49 H49 128.00 . . . no C50 C49 H49 126.00 . . . no C53 C49 H49 126.00 . . . no Fe2 C50 H50 125.00 . . . no C49 C50 H50 126.00 . . . no C51 C50 H50 126.00 . . . no Fe2 C51 H51 127.00 . . . no C50 C51 H51 126.00 . . . no C52 C51 H51 126.00 . . . no Fe2 C52 H52 126.00 . . . no C51 C52 H52 126.00 . . . no C53 C52 H52 127.00 . . . no Fe2 C53 H53 125.00 . . . no C49 C53 H53 126.00 . . . no C52 C53 H53 126.00 . . . no 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 Cu2 I2 Cu1 I1 2.30(3) . . . . no Cu2 I2 Cu1 N1 -96.07(13) . . . . no Cu2 I2 Cu1 N2 -177.79(14) . . . . no Cu2 I2 Cu1 N3 100.65(14) . . . . no Cu1 I2 Cu2 N4 95.54(16) . . . . no Cu1 I2 Cu2 N6 -84.98(17) . . . . no I1 Cu1 N1 C1 -8.6(5) . . . . no I1 Cu1 N1 C5 171.8(4) . . . . no I2 Cu1 N1 C1 86.6(5) . . . . no I2 Cu1 N1 C5 -93.0(4) . . . . no N2 Cu1 N1 C1 177.6(5) . . . . no N2 Cu1 N1 C5 -2.0(4) . . . . no I2 Cu1 N2 C6 95.0(5) . . . . no I2 Cu1 N2 C7 -83.9(5) . . . . no N1 Cu1 N2 C6 1.5(5) . . . . no N1 Cu1 N2 C7 -177.3(5) . . . . no N3 Cu1 N2 C6 -178.1(5) . . . . no N3 Cu1 N2 C7 3.0(5) . . . . no I1 Cu1 N3 C8 -179.7(4) . . . . no I1 Cu1 N3 C12 5.5(6) . . . . no I2 Cu1 N3 C8 86.1(4) . . . . no I2 Cu1 N3 C12 -88.7(5) . . . . no N2 Cu1 N3 C8 -5.9(4) . . . . no N2 Cu1 N3 C12 179.3(6) . . . . no I2 Cu2 N4 C31 -2.5(6) . . . . no I2 Cu2 N4 C35 174.5(4) . . . . no N5 Cu2 N4 C31 174.7(7) . . . . no N5 Cu2 N4 C35 -8.4(4) . . . . no N4 Cu2 N5 C36 7.1(5) . . . . no N4 Cu2 N5 C37 -168.7(6) . . . . no N6 Cu2 N5 C36 -171.5(5) . . . . no N6 Cu2 N5 C37 12.6(5) . . . . no I2 Cu2 N6 C38 167.1(5) . . . . no I2 Cu2 N6 C42 -11.9(6) . . . . no N5 Cu2 N6 C38 -10.0(5) . . . . no N5 Cu2 N6 C42 171.0(7) . . . . no C15 Fe1 C14 C13 118.5(6) . . . . no C15 Fe1 C14 C18 -119.0(5) . . . . no C16 Fe1 C14 C13 155.8(5) . . . . no C16 Fe1 C14 C15 37.3(3) . . . . no C16 Fe1 C14 C18 -81.7(4) . . . . no C17 Fe1 C14 C13 -160.4(5) . . . . no C17 Fe1 C14 C15 81.2(4) . . . . no C17 Fe1 C14 C18 -37.9(3) . . . . no C18 Fe1 C14 C13 -122.5(6) . . . . no C18 Fe1 C14 C15 119.0(5) . . . . no C20 Fe1 C14 C13 -78.6(8) . . . . no C20 Fe1 C14 C15 162.9(6) . . . . no C20 Fe1 C14 C18 43.9(8) . . . . no C21 Fe1 C14 C13 -45.7(6) . . . . no C21 Fe1 C14 C15 -164.1(4) . . . . no C21 Fe1 C14 C18 76.8(4) . . . . no C22 Fe1 C14 C13 -4.1(6) . . . . no C22 Fe1 C14 C15 -122.5(4) . . . . no C22 Fe1 C14 C18 118.4(4) . . . . no C23 Fe1 C14 C13 38.8(6) . . . . no C23 Fe1 C14 C15 -79.7(4) . . . . no C23 Fe1 C14 C18 161.3(4) . . . . no C14 Fe1 C15 C16 119.2(5) . . . . no C16 Fe1 C15 C14 -119.2(5) . . . . no C17 Fe1 C15 C14 -82.1(4) . . . . no C17 Fe1 C15 C16 37.1(4) . . . . no C18 Fe1 C15 C14 -38.3(3) . . . . no C18 Fe1 C15 C16 80.9(4) . . . . no C19 Fe1 C15 C14 162.4(4) . . . . no C19 Fe1 C15 C16 -78.4(4) . . . . no C20 Fe1 C15 C14 -161.2(6) . . . . no C20 Fe1 C15 C16 -42.0(9) . . . . no C21 Fe1 C15 C14 41.2(9) . . . . no C21 Fe1 C15 C16 160.4(7) . . . . no C22 Fe1 C15 C14 77.2(4) . . . . no C22 Fe1 C15 C16 -163.6(4) . . . . no C23 Fe1 C15 C14 120.3(4) . . . . no C23 Fe1 C15 C16 -120.6(4) . . . . no C14 Fe1 C16 C15 -38.0(4) . . . . no C14 Fe1 C16 C17 82.6(4) . . . . no C15 Fe1 C16 C17 120.6(5) . . . . no C17 Fe1 C16 C15 -120.6(5) . . . . no C18 Fe1 C16 C15 -82.8(4) . . . . no C18 Fe1 C16 C17 37.9(4) . . . . no C19 Fe1 C16 C15 121.2(4) . . . . no C19 Fe1 C16 C17 -118.2(4) . . . . no C20 Fe1 C16 C15 163.8(4) . . . . no C20 Fe1 C16 C17 -75.6(4) . . . . no C21 Fe1 C16 C15 -161.4(6) . . . . no C21 Fe1 C16 C17 -40.8(8) . . . . no C23 Fe1 C16 C15 78.9(4) . . . . no C23 Fe1 C16 C17 -160.4(4) . . . . no C14 Fe1 C17 C16 -80.5(4) . . . . no C14 Fe1 C17 C18 38.5(3) . . . . no C15 Fe1 C17 C16 -36.6(4) . . . . no C15 Fe1 C17 C18 82.5(4) . . . . no C16 Fe1 C17 C18 119.0(5) . . . . no C18 Fe1 C17 C16 -119.0(5) . . . . no C19 Fe1 C17 C16 81.3(4) . . . . no C19 Fe1 C17 C18 -159.7(4) . . . . no C20 Fe1 C17 C16 122.6(4) . . . . no C20 Fe1 C17 C18 -118.3(4) . . . . no C21 Fe1 C17 C16 163.6(4) . . . . no C21 Fe1 C17 C18 -77.4(4) . . . . no C22 Fe1 C17 C16 -167.3(6) . . . . no C22 Fe1 C17 C18 -48.2(8) . . . . no C23 Fe1 C17 C16 50.4(8) . . . . no C23 Fe1 C17 C18 169.5(6) . . . . no C14 Fe1 C18 C17 -118.7(5) . . . . no C15 Fe1 C18 C14 37.7(3) . . . . no C15 Fe1 C18 C17 -80.9(4) . . . . no C16 Fe1 C18 C14 80.9(4) . . . . no C16 Fe1 C18 C17 -37.8(3) . . . . no C17 Fe1 C18 C14 118.7(5) . . . . no C19 Fe1 C18 C14 168.3(6) . . . . no C19 Fe1 C18 C17 49.7(8) . . . . no C20 Fe1 C18 C14 -162.1(3) . . . . no C20 Fe1 C18 C17 79.3(4) . . . . no C21 Fe1 C18 C14 -121.3(4) . . . . no C21 Fe1 C18 C17 120.1(4) . . . . no C22 Fe1 C18 C14 -81.0(4) . . . . no C22 Fe1 C18 C17 160.3(4) . . . . no C23 Fe1 C18 C14 -50.4(9) . . . . no C23 Fe1 C18 C17 -169.0(7) . . . . no C15 Fe1 C19 C20 161.6(4) . . . . no C15 Fe1 C19 C23 -78.7(5) . . . . no C16 Fe1 C19 C20 119.7(4) . . . . no C16 Fe1 C19 C23 -120.5(4) . . . . no C17 Fe1 C19 C20 76.8(5) . . . . no C17 Fe1 C19 C23 -163.4(4) . . . . no C18 Fe1 C19 C20 40.7(9) . . . . no C18 Fe1 C19 C23 160.5(6) . . . . no C20 Fe1 C19 C23 119.8(6) . . . . no C21 Fe1 C19 C20 -37.3(4) . . . . no C21 Fe1 C19 C23 82.4(5) . . . . no C22 Fe1 C19 C20 -80.6(4) . . . . no C22 Fe1 C19 C23 39.2(4) . . . . no C23 Fe1 C19 C20 -119.8(6) . . . . no C14 Fe1 C20 C19 164.7(6) . . . . no C14 Fe1 C20 C21 45.6(8) . . . . no C15 Fe1 C20 C19 -48.9(9) . . . . no C15 Fe1 C20 C21 -168.0(7) . . . . no C16 Fe1 C20 C19 -80.0(4) . . . . no C16 Fe1 C20 C21 160.9(4) . . . . no C17 Fe1 C20 C19 -121.1(4) . . . . no C17 Fe1 C20 C21 119.8(4) . . . . no C18 Fe1 C20 C19 -163.0(4) . . . . no C18 Fe1 C20 C21 77.8(5) . . . . no C19 Fe1 C20 C21 -119.1(6) . . . . no C21 Fe1 C20 C19 119.1(6) . . . . no C22 Fe1 C20 C19 81.8(4) . . . . no C22 Fe1 C20 C21 -37.3(4) . . . . no C23 Fe1 C20 C19 37.2(4) . . . . no C23 Fe1 C20 C21 -81.9(5) . . . . no C14 Fe1 C21 C20 -161.2(4) . . . . no C14 Fe1 C21 C22 79.5(5) . . . . no C15 Fe1 C21 C20 168.1(7) . . . . no C15 Fe1 C21 C22 48.9(9) . . . . no C16 Fe1 C21 C20 -47.7(9) . . . . no C16 Fe1 C21 C22 -167.0(6) . . . . no C17 Fe1 C21 C20 -77.6(5) . . . . no C17 Fe1 C21 C22 163.1(4) . . . . no C18 Fe1 C21 C20 -119.1(4) . . . . no C18 Fe1 C21 C22 121.6(4) . . . . no C19 Fe1 C21 C20 37.9(4) . . . . no C19 Fe1 C21 C22 -81.4(4) . . . . no C20 Fe1 C21 C22 -119.3(6) . . . . no C22 Fe1 C21 C20 119.3(6) . . . . no C23 Fe1 C21 C20 81.5(4) . . . . no C23 Fe1 C21 C22 -37.8(4) . . . . no C14 Fe1 C22 C21 -119.1(4) . . . . no C14 Fe1 C22 C23 120.9(4) . . . . no C15 Fe1 C22 C21 -161.2(4) . . . . no C15 Fe1 C22 C23 78.8(4) . . . . no C17 Fe1 C22 C21 -40.4(8) . . . . no C17 Fe1 C22 C23 -160.4(6) . . . . no C18 Fe1 C22 C21 -75.6(4) . . . . no C18 Fe1 C22 C23 164.4(4) . . . . no C19 Fe1 C22 C21 81.6(4) . . . . no C19 Fe1 C22 C23 -38.4(4) . . . . no C20 Fe1 C22 C21 37.5(4) . . . . no C20 Fe1 C22 C23 -82.5(4) . . . . no C21 Fe1 C22 C23 -120.0(5) . . . . no C23 Fe1 C22 C21 120.0(5) . . . . no C14 Fe1 C23 C19 163.9(4) . . . . no C14 Fe1 C23 C22 -78.8(5) . . . . no C15 Fe1 C23 C19 121.1(4) . . . . no C15 Fe1 C23 C22 -121.7(4) . . . . no C16 Fe1 C23 C19 79.2(5) . . . . no C16 Fe1 C23 C22 -163.6(4) . . . . no C17 Fe1 C23 C19 41.9(9) . . . . no C17 Fe1 C23 C22 159.2(6) . . . . no C18 Fe1 C23 C19 -158.2(7) . . . . no C18 Fe1 C23 C22 -40.9(9) . . . . no C19 Fe1 C23 C22 117.3(6) . . . . no C20 Fe1 C23 C19 -37.4(4) . . . . no C20 Fe1 C23 C22 79.8(4) . . . . no C21 Fe1 C23 C19 -80.6(4) . . . . no C21 Fe1 C23 C22 36.6(4) . . . . no C22 Fe1 C23 C19 -117.3(6) . . . . no C45 Fe2 C44 C43A -144.5(13) . . . . no C45 Fe2 C44 C48 117.6(8) . . . . no C46 Fe2 C44 C43A 178.4(12) . . . . no C46 Fe2 C44 C45 -37.2(5) . . . . no C46 Fe2 C44 C48 80.4(7) . . . . no C47 Fe2 C44 C43A 135.5(12) . . . . no C47 Fe2 C44 C45 -80.1(6) . . . . no C47 Fe2 C44 C48 37.5(7) . . . . no C48 Fe2 C44 C43A 98.0(13) . . . . no C48 Fe2 C44 C45 -117.6(8) . . . . no C49 Fe2 C44 C43A -62.9(12) . . . . no C49 Fe2 C44 C45 81.6(6) . . . . no C49 Fe2 C44 C48 -160.8(6) . . . . no C50 Fe2 C44 C43A -21.4(12) . . . . no C50 Fe2 C44 C45 123.1(5) . . . . no C50 Fe2 C44 C48 -119.4(6) . . . . no C51 Fe2 C44 C43A 20.9(12) . . . . no C51 Fe2 C44 C45 165.4(5) . . . . no C51 Fe2 C44 C48 -77.1(7) . . . . no C53 Fe2 C44 C43A -98.7(15) . . . . no C53 Fe2 C44 C45 45.7(11) . . . . no C53 Fe2 C44 C48 163.3(8) . . . . no C44 Fe2 C45 C46 -118.8(8) . . . . no C46 Fe2 C45 C44 118.8(8) . . . . no C47 Fe2 C45 C44 81.6(6) . . . . no C47 Fe2 C45 C46 -37.2(6) . . . . no C48 Fe2 C45 C44 38.6(6) . . . . no C48 Fe2 C45 C46 -80.2(7) . . . . no C49 Fe2 C45 C44 -117.8(5) . . . . no C49 Fe2 C45 C46 123.4(6) . . . . no C50 Fe2 C45 C44 -77.2(6) . . . . no C50 Fe2 C45 C46 164.0(5) . . . . no C52 Fe2 C45 C44 164.1(7) . . . . no C52 Fe2 C45 C46 45.3(10) . . . . no C53 Fe2 C45 C44 -161.0(5) . . . . no C53 Fe2 C45 C46 80.2(6) . . . . no C44 Fe2 C46 C45 38.5(6) . . . . no C44 Fe2 C46 C47 -80.8(7) . . . . no C45 Fe2 C46 C47 -119.3(8) . . . . no C47 Fe2 C46 C45 119.3(8) . . . . no C48 Fe2 C46 C45 82.8(7) . . . . no C48 Fe2 C46 C47 -36.4(7) . . . . no C49 Fe2 C46 C45 -75.9(6) . . . . no C49 Fe2 C46 C47 164.9(5) . . . . no C51 Fe2 C46 C45 167.2(8) . . . . no C51 Fe2 C46 C47 47.9(11) . . . . no C52 Fe2 C46 C45 -159.8(5) . . . . no C52 Fe2 C46 C47 81.0(7) . . . . no C53 Fe2 C46 C45 -117.5(6) . . . . no C53 Fe2 C46 C47 123.2(6) . . . . no C44 Fe2 C47 C46 82.2(7) . . . . no C44 Fe2 C47 C48 -38.6(7) . . . . no C45 Fe2 C47 C46 37.3(6) . . . . no C45 Fe2 C47 C48 -83.5(7) . . . . no C46 Fe2 C47 C48 -120.8(9) . . . . no C48 Fe2 C47 C46 120.8(9) . . . . no C50 Fe2 C47 C46 165.6(8) . . . . no C50 Fe2 C47 C48 44.8(13) . . . . no C51 Fe2 C47 C46 -159.4(5) . . . . no C51 Fe2 C47 C48 79.9(7) . . . . no C52 Fe2 C47 C46 -116.8(6) . . . . no C52 Fe2 C47 C48 122.4(7) . . . . no C53 Fe2 C47 C46 -75.3(7) . . . . no C53 Fe2 C47 C48 164.0(6) . . . . no C44 Fe2 C48 C47 118.3(10) . . . . no C45 Fe2 C48 C44 -38.9(6) . . . . no C45 Fe2 C48 C47 79.4(7) . . . . no C46 Fe2 C48 C44 -81.9(7) . . . . no C46 Fe2 C48 C47 36.4(6) . . . . no C47 Fe2 C48 C44 -118.3(10) . . . . no C49 Fe2 C48 C44 46.9(13) . . . . no C49 Fe2 C48 C47 165.3(9) . . . . no C50 Fe2 C48 C44 80.1(7) . . . . no C50 Fe2 C48 C47 -161.6(6) . . . . no C51 Fe2 C48 C44 122.9(7) . . . . no C51 Fe2 C48 C47 -118.7(7) . . . . no C52 Fe2 C48 C44 165.4(6) . . . . no C52 Fe2 C48 C47 -76.3(7) . . . . no C44 Fe2 C49 C50 80.3(6) . . . . no C44 Fe2 C49 C53 -159.6(6) . . . . no C45 Fe2 C49 C50 123.7(5) . . . . no C45 Fe2 C49 C53 -116.2(5) . . . . no C46 Fe2 C49 C50 164.4(5) . . . . no C46 Fe2 C49 C53 -75.5(6) . . . . no C48 Fe2 C49 C50 46.0(12) . . . . no C48 Fe2 C49 C53 166.2(10) . . . . no C50 Fe2 C49 C53 120.1(6) . . . . no C51 Fe2 C49 C50 -38.3(5) . . . . no C51 Fe2 C49 C53 81.8(5) . . . . no C52 Fe2 C49 C50 -82.5(5) . . . . no C52 Fe2 C49 C53 37.6(5) . . . . no C53 Fe2 C49 C50 -120.1(6) . . . . no C44 Fe2 C50 C49 -118.2(6) . . . . no C44 Fe2 C50 C51 123.0(6) . . . . no C45 Fe2 C50 C49 -75.6(6) . . . . no C45 Fe2 C50 C51 165.5(5) . . . . no C47 Fe2 C50 C49 166.7(9) . . . . no C47 Fe2 C50 C51 47.9(11) . . . . no C48 Fe2 C50 C49 -160.9(6) . . . . no C48 Fe2 C50 C51 80.2(6) . . . . no C49 Fe2 C50 C51 -118.9(6) . . . . no C51 Fe2 C50 C49 118.9(6) . . . . no C52 Fe2 C50 C49 81.2(5) . . . . no C52 Fe2 C50 C51 -37.6(5) . . . . no C53 Fe2 C50 C49 37.6(4) . . . . no C53 Fe2 C50 C51 -81.3(5) . . . . no C44 Fe2 C51 C50 -77.1(6) . . . . no C44 Fe2 C51 C52 163.5(5) . . . . no C46 Fe2 C51 C50 165.2(8) . . . . no C46 Fe2 C51 C52 45.8(11) . . . . no C47 Fe2 C51 C50 -160.7(5) . . . . no C47 Fe2 C51 C52 79.9(6) . . . . no C48 Fe2 C51 C50 -119.3(6) . . . . no C48 Fe2 C51 C52 121.3(6) . . . . no C49 Fe2 C51 C50 37.1(4) . . . . no C49 Fe2 C51 C52 -82.3(5) . . . . no C50 Fe2 C51 C52 -119.4(7) . . . . no C52 Fe2 C51 C50 119.4(7) . . . . no C53 Fe2 C51 C50 81.5(5) . . . . no C53 Fe2 C51 C52 -38.0(5) . . . . no C45 Fe2 C52 C51 167.7(7) . . . . no C45 Fe2 C52 C53 49.2(10) . . . . no C46 Fe2 C52 C51 -160.5(5) . . . . no C46 Fe2 C52 C53 81.1(6) . . . . no C47 Fe2 C52 C51 -119.1(5) . . . . no C47 Fe2 C52 C53 122.5(5) . . . . no C48 Fe2 C52 C51 -78.5(6) . . . . no C48 Fe2 C52 C53 163.1(5) . . . . no C49 Fe2 C52 C51 80.4(5) . . . . no C49 Fe2 C52 C53 -38.1(5) . . . . no C50 Fe2 C52 C51 37.7(5) . . . . no C50 Fe2 C52 C53 -80.7(5) . . . . no C51 Fe2 C52 C53 -118.5(7) . . . . no C53 Fe2 C52 C51 118.5(7) . . . . no C44 Fe2 C53 C49 49.4(11) . . . . no C44 Fe2 C53 C52 168.3(9) . . . . no C45 Fe2 C53 C49 82.7(5) . . . . no C45 Fe2 C53 C52 -158.3(5) . . . . no C46 Fe2 C53 C49 124.0(5) . . . . no C46 Fe2 C53 C52 -117.0(5) . . . . no C47 Fe2 C53 C49 164.3(5) . . . . no C47 Fe2 C53 C52 -76.8(6) . . . . no C49 Fe2 C53 C52 119.0(7) . . . . no C50 Fe2 C53 C49 -36.5(5) . . . . no C50 Fe2 C53 C52 82.5(5) . . . . no C51 Fe2 C53 C49 -80.7(5) . . . . no C51 Fe2 C53 C52 38.3(5) . . . . no C52 Fe2 C53 C49 -119.0(7) . . . . no C13 O3 C9 C8 -78.9(7) . . . . no C13 O3 C9 C10 103.6(6) . . . . no C9 O3 C13 O4 -1.4(8) . . . . no C9 O3 C13 C14 -179.9(4) . . . . no C43A O7A C39 C38 -78.7(12) . . . . no C43A O7A C39 C40 117.2(11) . . . . no C39 O7A C43A O8A -9.0(17) . . . . no C39 O7A C43A C44 171.1(9) . . . . no Cu1 N1 C1 C2 179.5(4) . . . . no C5 N1 C1 C2 -0.9(8) . . . . no Cu1 N1 C5 C4 -177.7(5) . . . . no Cu1 N1 C5 C6 2.1(6) . . . . no C1 N1 C5 C4 2.7(8) . . . . no C1 N1 C5 C6 -177.5(5) . . . . no Cu1 N2 C6 O1 -178.8(5) . . . . no Cu1 N2 C6 C5 -0.8(7) . . . . no C7 N2 C6 O1 0.0(11) . . . . no C7 N2 C6 C5 178.0(6) . . . . no Cu1 N2 C7 O2 -176.2(6) . . . . no Cu1 N2 C7 C8 0.2(8) . . . . no C6 N2 C7 O2 5.0(12) . . . . no C6 N2 C7 C8 -178.6(6) . . . . no Cu1 N3 C8 C7 7.7(7) . . . . no Cu1 N3 C8 C9 -173.6(5) . . . . no C12 N3 C8 C7 -177.0(6) . . . . no C12 N3 C8 C9 1.7(9) . . . . no Cu1 N3 C12 C11 174.6(5) . . . . no C8 N3 C12 C11 0.1(9) . . . . no Cu2 N4 C31 C32 175.3(6) . . . . no C35 N4 C31 C32 -1.4(10) . . . . no Cu2 N4 C35 C34 -173.3(5) . . . . no Cu2 N4 C35 C36 8.5(7) . . . . no C31 N4 C35 C34 4.0(10) . . . . no C31 N4 C35 C36 -174.2(6) . . . . no Cu2 N5 C36 O5 176.1(5) . . . . no Cu2 N5 C36 C35 -4.4(7) . . . . no C37 N5 C36 O5 -8.3(11) . . . . no C37 N5 C36 C35 171.2(6) . . . . no Cu2 N5 C37 O6 170.0(7) . . . . no Cu2 N5 C37 C38 -12.0(8) . . . . no C36 N5 C37 O6 -5.5(13) . . . . no C36 N5 C37 C38 172.4(6) . . . . no Cu2 N6 C38 C37 6.5(8) . . . . no Cu2 N6 C38 C39 -176.3(6) . . . . no C42 N6 C38 C37 -174.4(7) . . . . no C42 N6 C38 C39 2.8(11) . . . . no Cu2 N6 C42 C41 177.8(6) . . . . no C38 N6 C42 C41 -1.1(11) . . . . no N1 C1 C2 C3 -0.5(9) . . . . no C1 C2 C3 C4 0.3(9) . . . . no C2 C3 C4 C5 1.3(9) . . . . no C3 C4 C5 N1 -2.9(9) . . . . no C3 C4 C5 C6 177.3(6) . . . . no N1 C5 C6 O1 177.2(5) . . . . no N1 C5 C6 N2 -0.9(7) . . . . no C4 C5 C6 O1 -3.0(9) . . . . no C4 C5 C6 N2 178.9(6) . . . . no O2 C7 C8 N3 171.3(7) . . . . no O2 C7 C8 C9 -7.2(11) . . . . no N2 C7 C8 N3 -5.4(8) . . . . no N2 C7 C8 C9 176.0(6) . . . . no N3 C8 C9 O3 -179.4(5) . . . . no N3 C8 C9 C10 -2.0(9) . . . . no C7 C8 C9 O3 -0.9(9) . . . . no C7 C8 C9 C10 176.5(6) . . . . no O3 C9 C10 C11 178.0(5) . . . . no C8 C9 C10 C11 0.5(9) . . . . no C9 C10 C11 C12 1.2(9) . . . . no C10 C11 C12 N3 -1.6(9) . . . . no O3 C13 C14 Fe1 74.8(6) . . . . no O3 C13 C14 C15 160.7(5) . . . . no O3 C13 C14 C18 -12.4(8) . . . . no O4 C13 C14 Fe1 -103.7(6) . . . . no O4 C13 C14 C15 -17.8(9) . . . . no O4 C13 C14 C18 169.2(6) . . . . no Fe1 C14 C15 C16 -60.0(5) . . . . no C13 C14 C15 Fe1 -114.4(6) . . . . no C13 C14 C15 C16 -174.5(6) . . . . no C18 C14 C15 Fe1 59.8(4) . . . . no C18 C14 C15 C16 -0.3(7) . . . . no Fe1 C14 C18 C17 59.5(4) . . . . no C13 C14 C18 Fe1 113.8(6) . . . . no C13 C14 C18 C17 173.3(5) . . . . no C15 C14 C18 Fe1 -60.2(4) . . . . no C15 C14 C18 C17 -0.7(7) . . . . no Fe1 C15 C16 C17 -57.8(5) . . . . no C14 C15 C16 Fe1 58.8(4) . . . . no C14 C15 C16 C17 1.1(7) . . . . no Fe1 C16 C17 C18 -59.5(4) . . . . no C15 C16 C17 Fe1 58.0(5) . . . . no C15 C16 C17 C18 -1.5(7) . . . . no Fe1 C17 C18 C14 -58.9(4) . . . . no C16 C17 C18 Fe1 60.2(4) . . . . no C16 C17 C18 C14 1.3(7) . . . . no Fe1 C19 C20 C21 59.5(5) . . . . no C23 C19 C20 Fe1 -59.6(5) . . . . no C23 C19 C20 C21 -0.1(8) . . . . no Fe1 C19 C23 C22 -59.2(5) . . . . no C20 C19 C23 Fe1 59.2(5) . . . . no C20 C19 C23 C22 0.0(8) . . . . no Fe1 C20 C21 C22 59.8(5) . . . . no C19 C20 C21 Fe1 -59.6(5) . . . . no C19 C20 C21 C22 0.3(8) . . . . no Fe1 C21 C22 C23 59.7(5) . . . . no C20 C21 C22 Fe1 -60.0(5) . . . . no C20 C21 C22 C23 -0.3(8) . . . . no Fe1 C22 C23 C19 59.8(5) . . . . no C21 C22 C23 Fe1 -59.6(5) . . . . no C21 C22 C23 C19 0.2(8) . . . . no N4 C31 C32 C33 -1.5(12) . . . . no C31 C32 C33 C34 1.9(12) . . . . no C32 C33 C34 C35 0.5(11) . . . . no C33 C34 C35 N4 -3.6(10) . . . . no C33 C34 C35 C36 174.5(6) . . . . no N4 C35 C36 O5 176.5(6) . . . . no N4 C35 C36 N5 -3.1(8) . . . . no C34 C35 C36 O5 -1.7(9) . . . . no C34 C35 C36 N5 178.7(6) . . . . no O6 C37 C38 N6 -178.8(8) . . . . no O6 C37 C38 C39 4.2(13) . . . . no N5 C37 C38 N6 3.1(10) . . . . no N5 C37 C38 C39 -174.0(8) . . . . no N6 C38 C39 O7A -166.2(8) . . . . no N6 C38 C39 C40 -2.2(13) . . . . no C37 C38 C39 O7A 10.8(13) . . . . no C37 C38 C39 C40 174.7(8) . . . . no O7A C39 C40 C41 164.0(9) . . . . no C38 C39 C40 C41 -0.1(14) . . . . no C39 C40 C41 C42 1.8(13) . . . . no C40 C41 C42 N6 -1.2(13) . . . . no O7A C43A C44 Fe2 89.4(11) . . . . no O7A C43A C44 C45 -12(2) . . . . no O7A C43A C44 C48 165.8(10) . . . . no O8A C43A C44 Fe2 -90.5(18) . . . . no O8A C43A C44 C45 168.2(14) . . . . no O8A C43A C44 C48 -14(2) . . . . no Fe2 C44 C45 C46 61.0(6) . . . . no C43A C44 C45 Fe2 117.8(17) . . . . no C43A C44 C45 C46 178.8(16) . . . . no C48 C44 C45 Fe2 -59.9(8) . . . . no C48 C44 C45 C46 1.1(11) . . . . no Fe2 C44 C48 C47 -60.8(8) . . . . no C43A C44 C48 Fe2 -119.1(9) . . . . no C43A C44 C48 C47 -179.9(10) . . . . no C45 C44 C48 Fe2 59.6(7) . . . . no C45 C44 C48 C47 -1.2(12) . . . . no Fe2 C45 C46 C47 59.5(6) . . . . no C44 C45 C46 Fe2 -60.1(6) . . . . no C44 C45 C46 C47 -0.6(10) . . . . no Fe2 C46 C47 C48 58.7(8) . . . . no C45 C46 C47 Fe2 -58.9(6) . . . . no C45 C46 C47 C48 -0.2(11) . . . . no Fe2 C47 C48 C44 60.1(8) . . . . no C46 C47 C48 Fe2 -59.2(7) . . . . no C46 C47 C48 C44 0.9(12) . . . . no Fe2 C49 C50 C51 59.8(6) . . . . no C53 C49 C50 Fe2 -58.5(5) . . . . no C53 C49 C50 C51 1.2(9) . . . . no Fe2 C49 C53 C52 -59.8(6) . . . . no C50 C49 C53 Fe2 58.9(5) . . . . no C50 C49 C53 C52 -0.9(9) . . . . no Fe2 C50 C51 C52 59.3(6) . . . . no C49 C50 C51 Fe2 -60.4(5) . . . . no C49 C50 C51 C52 -1.1(9) . . . . no Fe2 C51 C52 C53 59.6(6) . . . . no C50 C51 C52 Fe2 -59.1(6) . . . . no C50 C51 C52 C53 0.5(9) . . . . no Fe2 C52 C53 C49 59.8(5) . . . . no C51 C52 C53 Fe2 -59.5(6) . . . . no C51 C52 C53 C49 0.3(9) . . . . no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C1 H1 I1 0.95 2.96 3.570(6) 123 . yes C3 H3 O2 0.95 2.35 3.057(8) 131 4_544 yes C10 H10 O8A 0.95 2.60 3.135(10) 116 4_535 yes C12 H12 I1 0.95 2.92 3.562(6) 126 . yes C22 H22 O8A 0.95 2.39 3.192(11) 142 4_535 yes C31 H31A I2 0.95 2.93 3.540(8) 123 . yes C32 H32 O4 0.95 2.50 3.379(9) 154 4_544 yes C33 H33 I2 0.95 2.91 3.767(7) 150 4_544 yes C40 H40 O5 0.95 2.38 3.288(9) 160 4_535 yes C41 H41 O6 0.95 2.37 3.219(8) 149 4_535 yes C42 H42 I2 0.95 3.01 3.622(7) 123 . yes C48 H48 O4 0.95 2.59 3.480(12) 156 4_534 yes _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.168 _refine_diff_density_min -1.030 _refine_diff_density_rms 0.120 # Attachment '9969_web_deposit_cif_file_3_HelenStoeckli-Evans_1331020702.4_{[Cu2L2][I]2}n.cif' data_{[Cu2L2][I]2}n _database_code_depnum_ccdc_archive 'CCDC 870330' #TrackingRef '9969_web_deposit_cif_file_3_HelenStoeckli-Evans_1331020702.4_{[Cu2L2][I]2}n.cif' _audit_update_record ; 2011-06-03 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H22 Cu2 Fe I2 N6 O8, 1.75(C2 H3 N)' _chemical_formula_sum 'C39.50 H27.25 Cu2 Fe I2 N7.75 O8' _chemical_formula_weight 1175.17 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' Cu Cu 0.3201 1.2651 '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' I I -0.4742 1.8119 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 21.131(2) _cell_length_b 15.2094(10) _cell_length_c 11.9706(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.344(8) _cell_angle_gamma 90.00 _cell_volume 3815.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9980 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 24.95 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.046 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2290 _exptl_absorpt_coefficient_mu 3.165 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2009)' _exptl_special_details ? _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'plane graphite' _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_measurement_method '\f + \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12169 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3328 _reflns_number_gt 2490 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2002)' _computing_cell_refinement X-Area _computing_data_reduction 'X-RED32 V1.48 (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009) and Mercury (Macrae et al., 2006)' _computing_publication_material 'SHELXL-97, PLATON and Publcif (Westrip, 2010)' _refine_special_details ; Platon_squeeze_details: Total Potential Solvent Accessible Void Vol ... 431.8 Ang^3^ N: Electron Count / Cell = 178 - Included in D(calc), F000 & Mol.Wght. Equated to 1.75CH~3~CN molecules per molecule of complex. The C-bound H-atoms were included in calculated positions and treated as riding atoms: C-H = 0.95 \%A with U~iso~(H) = 1.2U~eq~(C). ; _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^)+(0.0588P)^2^+35.3589P] 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 3328 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I Uani 0.33247(3) -0.32656(3) -0.02222(4) 1.000 0.0422(2) d . . . Cu1 Cu Uani 0.30919(5) -0.15993(6) -0.04505(8) 1.000 0.0360(3) d . . . Fe1 Fe Uani 0.50000 0.30599(11) 0.25000 1.000 0.0439(5) d S . . O1 O Uani 0.2539(3) 0.0699(4) -0.1908(5) 1.000 0.0527(19) d . . . O2 O Uani 0.3391(3) 0.0999(3) 0.0058(5) 1.000 0.0417(19) d . . . O3 O Uani 0.4135(3) 0.0959(3) 0.2095(4) 1.000 0.0384(19) d . . . O4 O Uani 0.4774(3) 0.0918(4) 0.0689(5) 1.000 0.0451(19) d . . . N1 N Uani 0.2650(3) -0.1615(4) -0.2042(5) 1.000 0.0364(19) d . . . N2 N Uani 0.3047(3) -0.0340(4) -0.0694(5) 1.000 0.0333(19) d . . . N3 N Uani 0.3582(3) -0.1197(4) 0.1042(5) 1.000 0.0341(19) d . . . C1 C Uani 0.2476(4) -0.2303(5) -0.2718(7) 1.000 0.038(3) d . . . C2 C Uani 0.2140(4) -0.2220(6) -0.3785(7) 1.000 0.042(3) d . . . C3 C Uani 0.1980(5) -0.1381(6) -0.4163(7) 1.000 0.049(3) d . . . C4 C Uani 0.2147(4) -0.0659(5) -0.3489(7) 1.000 0.042(3) d . . . C5 C Uani 0.2483(4) -0.0796(5) -0.2431(7) 1.000 0.037(2) d . . . C6 C Uani 0.2695(4) -0.0042(5) -0.1660(7) 1.000 0.040(3) d . . . C7 C Uani 0.3358(4) 0.0206(5) 0.0096(6) 1.000 0.037(3) d . . . C8 C Uani 0.3676(4) -0.0318(5) 0.1079(7) 1.000 0.035(2) d . . . C9 C Uani 0.4026(4) 0.0060(5) 0.2001(6) 1.000 0.036(3) d . . . C10 C Uani 0.4254(4) -0.0464(6) 0.2938(6) 1.000 0.038(3) d . . . C11 C Uani 0.4129(4) -0.1335(6) 0.2893(7) 1.000 0.042(3) d . . . C12 C Uani 0.3803(4) -0.1693(5) 0.1913(7) 1.000 0.040(3) d . . . C13 C Uani 0.4484(4) 0.1344(6) 0.1304(7) 1.000 0.042(3) d . . . C14 C Uani 0.4457(4) 0.2299(5) 0.1361(7) 1.000 0.043(3) d . . . C15 C Uani 0.4060(4) 0.2830(6) 0.1957(8) 1.000 0.045(3) d . . . C16 C Uani 0.4204(5) 0.3719(7) 0.1785(9) 1.000 0.061(4) d . . . C17 C Uani 0.4680(6) 0.3745(7) 0.1064(9) 1.000 0.070(4) d . . . C18 C Uani 0.4842(5) 0.2864(6) 0.0802(7) 1.000 0.049(3) d . . . H1A H Uiso 0.25890 -0.28770 -0.24500 1.000 0.0460 c R . . H2A H Uiso 0.20240 -0.27210 -0.42390 1.000 0.0510 c R . . H3A H Uiso 0.17530 -0.13000 -0.48930 1.000 0.0590 c R . . H4A H Uiso 0.20340 -0.00820 -0.37450 1.000 0.0500 c R . . H10A H Uiso 0.44910 -0.02110 0.35870 1.000 0.0450 c R . . H11A H Uiso 0.42630 -0.17010 0.35230 1.000 0.0500 c R . . H12A H Uiso 0.37360 -0.23100 0.18690 1.000 0.0480 c R . . H15A H Uiso 0.37490 0.26200 0.23990 1.000 0.0540 c R . . H16A H Uiso 0.40150 0.42120 0.20990 1.000 0.0730 c R . . H17A H Uiso 0.48620 0.42630 0.07960 1.000 0.0840 c R . . H18A H Uiso 0.51530 0.26900 0.03370 1.000 0.0580 c 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 I1 0.0514(4) 0.0319(3) 0.0423(3) 0.0007(2) 0.0018(2) -0.0019(3) Cu1 0.0457(6) 0.0263(5) 0.0337(5) 0.0003(4) -0.0036(4) -0.0039(4) Fe1 0.0476(10) 0.0360(9) 0.0441(9) 0.0000 -0.0096(8) 0.0000 O1 0.072(4) 0.036(3) 0.043(3) 0.001(3) -0.020(3) 0.000(3) O2 0.050(4) 0.030(3) 0.041(3) 0.000(2) -0.010(3) -0.001(3) O3 0.052(4) 0.029(3) 0.032(3) -0.004(2) -0.003(3) -0.005(2) O4 0.041(3) 0.050(4) 0.043(3) -0.006(3) 0.000(3) 0.008(3) N1 0.044(4) 0.029(3) 0.035(3) 0.004(3) 0.000(3) -0.006(3) N2 0.035(4) 0.030(3) 0.031(3) -0.001(3) -0.011(3) -0.003(3) N3 0.038(4) 0.029(3) 0.034(3) 0.001(3) 0.000(3) 0.001(3) C1 0.045(5) 0.030(4) 0.038(4) 0.002(3) 0.003(4) -0.004(4) C2 0.050(5) 0.039(5) 0.036(4) -0.009(4) -0.002(4) -0.007(4) C3 0.054(6) 0.050(5) 0.038(5) 0.000(4) -0.016(4) -0.004(4) C4 0.052(5) 0.034(4) 0.036(4) 0.001(3) -0.012(4) -0.003(4) C5 0.042(4) 0.035(4) 0.032(4) -0.001(3) 0.000(3) 0.001(4) C6 0.042(5) 0.035(5) 0.040(4) 0.002(4) -0.003(4) -0.008(4) C7 0.051(5) 0.031(4) 0.028(4) -0.002(3) 0.000(4) 0.000(4) C8 0.037(4) 0.033(4) 0.035(4) -0.003(3) 0.000(3) -0.003(3) C9 0.039(5) 0.032(4) 0.036(4) -0.005(3) 0.000(4) -0.003(4) C10 0.037(4) 0.044(5) 0.030(4) 0.005(3) -0.005(3) -0.004(4) C11 0.042(5) 0.051(5) 0.031(4) 0.006(4) 0.000(4) -0.004(4) C12 0.048(5) 0.032(4) 0.038(4) 0.006(4) -0.003(4) -0.006(4) C13 0.042(5) 0.047(5) 0.034(4) 0.003(4) -0.004(4) -0.012(4) C14 0.048(5) 0.033(4) 0.044(5) 0.003(4) -0.009(4) -0.001(4) C15 0.033(5) 0.043(5) 0.055(5) -0.003(4) -0.011(4) 0.002(4) C16 0.067(7) 0.051(6) 0.056(6) 0.001(5) -0.021(5) 0.009(5) C17 0.102(9) 0.044(6) 0.051(6) 0.014(5) -0.040(6) -0.010(6) C18 0.065(6) 0.043(5) 0.035(4) 0.005(4) -0.007(4) -0.001(4) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.5894(11) . . no I1 Cu1 3.2043(13) . 7_545 no Cu1 N1 2.012(6) . . no Cu1 N2 1.938(6) . . no Cu1 N3 2.041(6) . . no Fe1 C14 2.029(8) . . no Fe1 C15 2.040(9) . . no Fe1 C16 2.049(11) . . no Fe1 C17 2.050(11) . . no Fe1 C18 2.039(8) . . no Fe1 C14 2.029(8) . 2_655 no Fe1 C15 2.040(9) . 2_655 no Fe1 C16 2.049(11) . 2_655 no Fe1 C17 2.050(11) . 2_655 no Fe1 C18 2.039(8) . 2_655 no O1 C6 1.201(10) . . no O2 C7 1.209(9) . . no O3 C9 1.389(9) . . no O3 C13 1.401(10) . . no O4 C13 1.205(11) . . no N1 C1 1.345(10) . . no N1 C5 1.361(10) . . no N2 C6 1.370(10) . . no N2 C7 1.363(10) . . no N3 C8 1.352(10) . . no N3 C12 1.323(10) . . no C1 C2 1.386(12) . . no C2 C3 1.381(13) . . no C3 C4 1.382(12) . . no C4 C5 1.386(12) . . no C5 C6 1.504(11) . . no C7 C8 1.506(11) . . no C8 C9 1.374(11) . . no C9 C10 1.410(11) . . no C10 C11 1.351(13) . . no C11 C12 1.393(12) . . no C13 C14 1.456(12) . . no C14 C15 1.421(12) . . no C14 C18 1.410(13) . . no C15 C16 1.407(14) . . no C16 C17 1.407(16) . . no C17 C18 1.428(14) . . no C1 H1A 0.9500 . . no C2 H2A 0.9500 . . no C3 H3A 0.9500 . . no C4 H4A 0.9500 . . no C10 H10A 0.9500 . . no C11 H11A 0.9500 . . no C12 H12A 0.9500 . . no C15 H15A 0.9500 . . no C16 H16A 0.9500 . . no C17 H17A 0.9500 . . no C18 H18A 0.9500 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I1 Cu1 85.31(3) . . 7_545 no I1 Cu1 N1 98.47(18) . . . no I1 Cu1 N2 171.2(2) . . . no I1 Cu1 N3 97.63(18) . . . no I1 Cu1 I1 94.69(3) . . 7_545 no N1 Cu1 N2 82.0(3) . . . no N1 Cu1 N3 162.7(2) . . . no I1 Cu1 N1 84.36(18) 7_545 . . no N2 Cu1 N3 81.1(2) . . . no I1 Cu1 N2 94.12(19) 7_545 . . no I1 Cu1 N3 100.66(18) 7_545 . . no C14 Fe1 C15 40.9(4) . . . no C14 Fe1 C16 68.6(4) . . . no C14 Fe1 C17 68.2(4) . . . no C14 Fe1 C18 40.6(4) . . . no C14 Fe1 C14 110.4(3) . . 2_655 no C14 Fe1 C15 124.1(4) . . 2_655 no C14 Fe1 C16 157.4(4) . . 2_655 no C14 Fe1 C17 162.1(4) . . 2_655 no C14 Fe1 C18 126.4(4) . . 2_655 no C15 Fe1 C16 40.3(4) . . . no C15 Fe1 C17 67.4(4) . . . no C15 Fe1 C18 68.2(4) . . . no C14 Fe1 C15 124.1(4) 2_655 . . no C15 Fe1 C15 160.3(4) . . 2_655 no C15 Fe1 C16 158.6(4) . . 2_655 no C15 Fe1 C17 123.9(4) . . 2_655 no C15 Fe1 C18 108.7(4) . . 2_655 no C16 Fe1 C17 40.2(5) . . . no C16 Fe1 C18 68.5(4) . . . no C14 Fe1 C16 157.4(4) 2_655 . . no C15 Fe1 C16 158.6(4) 2_655 . . no C16 Fe1 C16 121.4(4) . . 2_655 no C16 Fe1 C17 105.5(4) . . 2_655 no C16 Fe1 C18 120.6(4) . . 2_655 no C17 Fe1 C18 40.9(4) . . . no C14 Fe1 C17 162.1(4) 2_655 . . no C15 Fe1 C17 123.9(4) 2_655 . . no C16 Fe1 C17 105.5(4) 2_655 . . no C17 Fe1 C17 118.9(4) . . 2_655 no C17 Fe1 C18 154.8(4) . . 2_655 no C14 Fe1 C18 126.4(4) 2_655 . . no C15 Fe1 C18 108.7(4) 2_655 . . no C16 Fe1 C18 120.6(4) 2_655 . . no C17 Fe1 C18 154.8(4) 2_655 . . no C18 Fe1 C18 163.2(4) . . 2_655 no C14 Fe1 C15 40.9(4) 2_655 . 2_655 no C14 Fe1 C16 68.6(4) 2_655 . 2_655 no C14 Fe1 C17 68.2(4) 2_655 . 2_655 no C14 Fe1 C18 40.6(4) 2_655 . 2_655 no C15 Fe1 C16 40.3(4) 2_655 . 2_655 no C15 Fe1 C17 67.4(4) 2_655 . 2_655 no C15 Fe1 C18 68.2(4) 2_655 . 2_655 no C16 Fe1 C17 40.2(5) 2_655 . 2_655 no C16 Fe1 C18 68.5(4) 2_655 . 2_655 no C17 Fe1 C18 40.9(4) 2_655 . 2_655 no C9 O3 C13 116.9(6) . . . no Cu1 N1 C1 129.6(5) . . . no Cu1 N1 C5 112.5(5) . . . no C1 N1 C5 117.9(7) . . . no Cu1 N2 C6 117.7(5) . . . no Cu1 N2 C7 119.2(5) . . . no C6 N2 C7 123.1(6) . . . no Cu1 N3 C8 112.4(5) . . . no Cu1 N3 C12 127.4(5) . . . no C8 N3 C12 120.2(7) . . . no N1 C1 C2 123.5(7) . . . no C1 C2 C3 117.5(8) . . . no C2 C3 C4 120.6(8) . . . no C3 C4 C5 118.5(7) . . . no N1 C5 C4 122.0(7) . . . no N1 C5 C6 116.4(7) . . . no C4 C5 C6 121.6(7) . . . no O1 C6 N2 128.4(7) . . . no O1 C6 C5 120.9(8) . . . no N2 C6 C5 110.7(6) . . . no O2 C7 N2 127.4(7) . . . no O2 C7 C8 122.3(7) . . . no N2 C7 C8 110.3(6) . . . no N3 C8 C7 116.7(7) . . . no N3 C8 C9 120.1(7) . . . no C7 C8 C9 123.2(7) . . . no O3 C9 C8 123.0(7) . . . no O3 C9 C10 117.1(7) . . . no C8 C9 C10 119.8(7) . . . no C9 C10 C11 118.5(7) . . . no C10 C11 C12 119.4(8) . . . no N3 C12 C11 121.8(7) . . . no O3 C13 O4 122.8(8) . . . no O3 C13 C14 111.0(7) . . . no O4 C13 C14 126.2(8) . . . no Fe1 C14 C13 125.4(6) . . . no Fe1 C14 C15 70.0(5) . . . no Fe1 C14 C18 70.1(5) . . . no C13 C14 C15 128.3(8) . . . no C13 C14 C18 123.9(8) . . . no C15 C14 C18 107.8(7) . . . no Fe1 C15 C14 69.1(5) . . . no Fe1 C15 C16 70.2(6) . . . no C14 C15 C16 108.7(8) . . . no Fe1 C16 C15 69.5(6) . . . no Fe1 C16 C17 69.9(6) . . . no C15 C16 C17 107.6(9) . . . no Fe1 C17 C16 69.9(6) . . . no Fe1 C17 C18 69.2(5) . . . no C16 C17 C18 108.6(9) . . . no Fe1 C18 C14 69.3(5) . . . no Fe1 C18 C17 70.0(6) . . . no C14 C18 C17 107.4(9) . . . no N1 C1 H1A 118.00 . . . no C2 C1 H1A 118.00 . . . no C1 C2 H2A 121.00 . . . no C3 C2 H2A 121.00 . . . no C2 C3 H3A 120.00 . . . no C4 C3 H3A 120.00 . . . no C3 C4 H4A 121.00 . . . no C5 C4 H4A 121.00 . . . no C9 C10 H10A 121.00 . . . no C11 C10 H10A 121.00 . . . no C10 C11 H11A 120.00 . . . no C12 C11 H11A 120.00 . . . no N3 C12 H12A 119.00 . . . no C11 C12 H12A 119.00 . . . no Fe1 C15 H15A 127.00 . . . no C14 C15 H15A 126.00 . . . no C16 C15 H15A 126.00 . . . no Fe1 C16 H16A 126.00 . . . no C15 C16 H16A 126.00 . . . no C17 C16 H16A 126.00 . . . no Fe1 C17 H17A 127.00 . . . no C16 C17 H17A 126.00 . . . no C18 C17 H17A 126.00 . . . no Fe1 C18 H18A 126.00 . . . no C14 C18 H18A 126.00 . . . no C17 C18 H18A 126.00 . . . no 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 Cu1 I1 Cu1 N1 -84.98(19) 7_545 . . . no Cu1 I1 Cu1 N3 101.44(18) 7_545 . . . no Cu1 I1 Cu1 I1 -0.02(9) 7_545 . . 7_545 no Cu1 I1 Cu1 I1 0.00(6) . . 7_545 7_545 no Cu1 I1 Cu1 N1 -98.07(18) . . 7_545 7_545 no Cu1 I1 Cu1 N2 -179.63(18) . . 7_545 7_545 no Cu1 I1 Cu1 N3 98.68(18) . . 7_545 7_545 no I1 Cu1 N1 C1 6.0(7) . . . . no I1 Cu1 N1 C5 -177.8(5) . . . . no N2 Cu1 N1 C1 177.2(7) . . . . no N2 Cu1 N1 C5 -6.7(5) . . . . no I1 Cu1 N1 C1 -87.9(7) 7_545 . . . no I1 Cu1 N1 C5 88.3(5) 7_545 . . . no N1 Cu1 N2 C6 8.4(6) . . . . no N1 Cu1 N2 C7 -172.1(6) . . . . no N3 Cu1 N2 C6 -175.5(6) . . . . no N3 Cu1 N2 C7 4.0(6) . . . . no I1 Cu1 N2 C6 -75.3(6) 7_545 . . . no I1 Cu1 N2 C7 104.2(6) 7_545 . . . no I1 Cu1 N3 C8 166.0(5) . . . . no I1 Cu1 N3 C12 -13.6(7) . . . . no N2 Cu1 N3 C8 -5.2(5) . . . . no N2 Cu1 N3 C12 175.2(7) . . . . no I1 Cu1 N3 C8 -97.8(5) 7_545 . . . no I1 Cu1 N3 C12 82.6(7) 7_545 . . . no C15 Fe1 C14 C13 -123.4(9) . . . . no C15 Fe1 C14 C18 118.5(7) . . . . no C16 Fe1 C14 C13 -160.3(8) . . . . no C16 Fe1 C14 C15 -36.9(5) . . . . no C16 Fe1 C14 C18 81.6(6) . . . . no C17 Fe1 C14 C13 156.3(9) . . . . no C17 Fe1 C14 C15 -80.3(6) . . . . no C17 Fe1 C14 C18 38.3(6) . . . . no C18 Fe1 C14 C13 118.1(10) . . . . no C18 Fe1 C14 C15 -118.5(7) . . . . no C14 Fe1 C14 C13 -4.5(8) 2_655 . . . no C14 Fe1 C14 C15 118.9(5) 2_655 . . . no C14 Fe1 C14 C18 -122.6(5) 2_655 . . . no C15 Fe1 C14 C13 39.3(9) 2_655 . . . no C15 Fe1 C14 C15 162.7(5) 2_655 . . . no C15 Fe1 C14 C18 -78.8(6) 2_655 . . . no C16 Fe1 C14 C13 78.7(12) 2_655 . . . no C16 Fe1 C14 C15 -157.9(10) 2_655 . . . no C16 Fe1 C14 C18 -39.4(12) 2_655 . . . no C18 Fe1 C14 C13 -47.4(9) 2_655 . . . no C18 Fe1 C14 C15 76.0(6) 2_655 . . . no C18 Fe1 C14 C18 -165.5(6) 2_655 . . . no C14 Fe1 C15 C16 -120.1(8) . . . . no C16 Fe1 C15 C14 120.1(8) . . . . no C17 Fe1 C15 C14 82.3(6) . . . . no C17 Fe1 C15 C16 -37.8(6) . . . . no C18 Fe1 C15 C14 38.0(5) . . . . no C18 Fe1 C15 C16 -82.1(6) . . . . no C14 Fe1 C15 C14 -82.1(6) 2_655 . . . no C14 Fe1 C15 C16 157.9(6) 2_655 . . . no C16 Fe1 C15 C14 156.7(10) 2_655 . . . no C16 Fe1 C15 C16 36.7(13) 2_655 . . . no C17 Fe1 C15 C14 -167.2(5) 2_655 . . . no C17 Fe1 C15 C16 72.8(7) 2_655 . . . no C18 Fe1 C15 C14 -124.4(5) 2_655 . . . no C18 Fe1 C15 C16 115.5(6) 2_655 . . . no C14 Fe1 C16 C15 37.5(6) . . . . no C14 Fe1 C16 C17 -81.2(6) . . . . no C15 Fe1 C16 C17 -118.6(9) . . . . no C17 Fe1 C16 C15 118.6(9) . . . . no C18 Fe1 C16 C15 81.2(6) . . . . no C18 Fe1 C16 C17 -37.5(6) . . . . no C14 Fe1 C16 C15 -54.4(12) 2_655 . . . no C14 Fe1 C16 C17 -173.1(9) 2_655 . . . no C15 Fe1 C16 C15 167.9(9) 2_655 . . . no C15 Fe1 C16 C17 49.3(13) 2_655 . . . no C16 Fe1 C16 C15 -165.2(6) 2_655 . . . no C16 Fe1 C16 C17 76.2(7) 2_655 . . . no C17 Fe1 C16 C15 -124.7(6) 2_655 . . . no C17 Fe1 C16 C17 116.7(7) 2_655 . . . no C18 Fe1 C16 C15 -83.1(7) 2_655 . . . no C18 Fe1 C16 C17 158.3(6) 2_655 . . . no C14 Fe1 C17 C16 82.2(7) . . . . no C14 Fe1 C17 C18 -38.0(6) . . . . no C15 Fe1 C17 C16 37.9(6) . . . . no C15 Fe1 C17 C18 -82.3(7) . . . . no C16 Fe1 C17 C18 -120.2(9) . . . . no C18 Fe1 C17 C16 120.2(9) . . . . no C15 Fe1 C17 C16 -160.5(6) 2_655 . . . no C15 Fe1 C17 C18 79.3(7) 2_655 . . . no C16 Fe1 C17 C16 -120.7(7) 2_655 . . . no C16 Fe1 C17 C18 119.2(7) 2_655 . . . no C17 Fe1 C17 C16 -79.6(8) 2_655 . . . no C17 Fe1 C17 C18 160.3(6) 2_655 . . . no C18 Fe1 C17 C16 -48.4(13) 2_655 . . . no C18 Fe1 C17 C18 -168.5(9) 2_655 . . . no C14 Fe1 C18 C17 118.5(9) . . . . no C15 Fe1 C18 C14 -38.3(5) . . . . no C15 Fe1 C18 C17 80.3(7) . . . . no C16 Fe1 C18 C14 -81.7(6) . . . . no C16 Fe1 C18 C17 36.8(7) . . . . no C17 Fe1 C18 C14 -118.5(9) . . . . no C14 Fe1 C18 C14 78.8(6) 2_655 . . . no C14 Fe1 C18 C17 -162.7(6) 2_655 . . . no C15 Fe1 C18 C14 120.9(5) 2_655 . . . no C15 Fe1 C18 C17 -120.5(7) 2_655 . . . no C16 Fe1 C18 C14 163.6(5) 2_655 . . . no C16 Fe1 C18 C17 -77.9(8) 2_655 . . . no C17 Fe1 C18 C14 -162.4(9) 2_655 . . . no C17 Fe1 C18 C17 -43.9(13) 2_655 . . . no C13 O3 C9 C8 -63.1(11) . . . . no C13 O3 C9 C10 121.3(8) . . . . no C9 O3 C13 O4 -12.6(11) . . . . no C9 O3 C13 C14 169.0(7) . . . . no Cu1 N1 C1 C2 176.3(6) . . . . no C5 N1 C1 C2 0.3(12) . . . . no Cu1 N1 C5 C4 -177.0(7) . . . . no Cu1 N1 C5 C6 4.3(9) . . . . no C1 N1 C5 C4 -0.3(12) . . . . no C1 N1 C5 C6 -179.0(7) . . . . no Cu1 N2 C6 O1 169.7(7) . . . . no Cu1 N2 C6 C5 -8.0(9) . . . . no C7 N2 C6 O1 -9.7(14) . . . . no C7 N2 C6 C5 172.6(7) . . . . no Cu1 N2 C7 O2 177.9(7) . . . . no Cu1 N2 C7 C8 -2.0(9) . . . . no C6 N2 C7 O2 -2.7(13) . . . . no C6 N2 C7 C8 177.5(7) . . . . no Cu1 N3 C8 C7 5.8(9) . . . . no Cu1 N3 C8 C9 -176.7(6) . . . . no C12 N3 C8 C7 -174.6(7) . . . . no C12 N3 C8 C9 2.9(12) . . . . no Cu1 N3 C12 C11 -179.6(6) . . . . no C8 N3 C12 C11 0.8(12) . . . . no N1 C1 C2 C3 0.1(13) . . . . no C1 C2 C3 C4 -0.6(14) . . . . no C2 C3 C4 C5 0.6(14) . . . . no C3 C4 C5 N1 -0.1(13) . . . . no C3 C4 C5 C6 178.5(8) . . . . no N1 C5 C6 O1 -175.9(8) . . . . no N1 C5 C6 N2 2.1(10) . . . . no C4 C5 C6 O1 5.4(13) . . . . no C4 C5 C6 N2 -176.7(8) . . . . no O2 C7 C8 N3 177.4(8) . . . . no O2 C7 C8 C9 -0.1(13) . . . . no N2 C7 C8 N3 -2.7(10) . . . . no N2 C7 C8 C9 179.8(8) . . . . no N3 C8 C9 O3 -179.4(7) . . . . no N3 C8 C9 C10 -3.9(12) . . . . no C7 C8 C9 O3 -2.1(13) . . . . no C7 C8 C9 C10 173.5(8) . . . . no O3 C9 C10 C11 176.9(7) . . . . no C8 C9 C10 C11 1.1(12) . . . . no C9 C10 C11 C12 2.5(12) . . . . no C10 C11 C12 N3 -3.6(13) . . . . no O3 C13 C14 Fe1 80.8(9) . . . . no O3 C13 C14 C15 -10.7(12) . . . . no O3 C13 C14 C18 169.3(8) . . . . no O4 C13 C14 Fe1 -97.6(10) . . . . no O4 C13 C14 C15 170.9(9) . . . . no O4 C13 C14 C18 -9.1(14) . . . . no Fe1 C14 C15 C16 59.3(7) . . . . no C13 C14 C15 Fe1 119.8(9) . . . . no C13 C14 C15 C16 179.1(9) . . . . no C18 C14 C15 Fe1 -60.2(6) . . . . no C18 C14 C15 C16 -0.9(11) . . . . no Fe1 C14 C18 C17 -59.9(7) . . . . no C13 C14 C18 Fe1 -119.9(8) . . . . no C13 C14 C18 C17 -179.8(9) . . . . no C15 C14 C18 Fe1 60.1(6) . . . . no C15 C14 C18 C17 0.3(10) . . . . no Fe1 C15 C16 C17 59.9(8) . . . . no C14 C15 C16 Fe1 -58.6(6) . . . . no C14 C15 C16 C17 1.2(11) . . . . no Fe1 C16 C17 C18 58.5(7) . . . . no C15 C16 C17 Fe1 -59.6(7) . . . . no C15 C16 C17 C18 -1.1(12) . . . . no Fe1 C17 C18 C14 59.5(6) . . . . no C16 C17 C18 Fe1 -59.0(8) . . . . no C16 C17 C18 C14 0.5(12) . . . . no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C1 H1A I1 0.9500 2.9700 3.594(8) 124.00 . yes C1 H1A O1 0.9500 2.3000 3.071(10) 138.00 6_544 yes C2 H2A O2 0.9500 2.3000 3.238(10) 168.00 6_544 yes C10 H10A O4 0.9500 2.4000 3.237(10) 146.00 2_655 yes C12 H12A I1 0.9500 2.9300 3.552(8) 124.00 . yes _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.909 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.142