# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Hiroki OSHIO' _publ_contact_author_address ;Graduate School of Pure and Applied Sciences, University of Tsukuba, Tennodai 1-1-1, Tsukuba 305-8571, Japan ; _publ_contact_author_email oshio@chem.tsukuba.ac.jp _publ_contact_author_phone +81-29-853-4238 _publ_contact_author_fax +81-29-853-4238 loop_ _publ_author_name _publ_author_address C.Krueger ;Leibniz Universitut Hannover, Institat fur Anorganische Chemie, Callinstr. 9, D-30167 Hannover, Germany ; H.Sato ;Graduate School of Pure and Applied Sciences, University of Tsukuba, Tennodai 1-1-1, Tsukuba 305-8571, Japan ; T.Matsumoto ;Graduate School of Pure and Applied Sciences, University of Tsukuba, Tennodai 1-1-1, Tsukuba 305-8571, Japan ; T.Shiga ;Graduate School of Pure and Applied Sciences, University of Tsukuba, Tennodai 1-1-1, Tsukuba 305-8571, Japan ; G.N.Newton ;Graduate School of Pure and Applied Sciences, University of Tsukuba, Tennodai 1-1-1, Tsukuba 305-8571, Japan ; F.Renz ;Leibniz Universitut Hannover, Institat fur Anorganische Chemie, Callinstr. 9, D-30167 Hannover, Germany ; H.Oshio ;Graduate School of Pure and Applied Sciences, University of Tsukuba, Tennodai 1-1-1, Tsukuba 305-8571, Japan ; data_Comp1 _database_code_depnum_ccdc_archive 'CCDC 883725' #TrackingRef '- TetraCN.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H22 Fe2 K4 N16 O, 0.22(C2 O2), 0.57(C O), H0.50, H0.50, H' _chemical_formula_sum 'C36 H26 Fe2 K4 N16 O2' _chemical_formula_weight 982.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.408(4) _cell_length_b 20.572(10) _cell_length_c 24.726(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.789(7) _cell_angle_gamma 90.00 _cell_volume 4215(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5847 _cell_measurement_theta_min 2.648 _cell_measurement_theta_max 25.607 _exptl_crystal_description needles _exptl_crystal_colour purple _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 1.138 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7961 _exptl_absorpt_correction_T_max 0.9045 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 177 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25983 _diffrn_reflns_av_R_equivalents 0.1217 _diffrn_reflns_av_sigmaI/netI 0.1179 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9551 _reflns_number_gt 6054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Methanol molecules in the lattice were treated by DFIX restraints. ; _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^)+(0.1125P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9551 _refine_ls_number_parameters 563 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.2024 _refine_ls_wR_factor_gt 0.1833 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K -0.11751(14) -0.12776(5) 0.17658(4) 0.0336(3) Uani 1 1 d . . . K2 K -0.9723(2) -0.19475(6) 0.02890(5) 0.0561(4) Uani 1 1 d . . . K3 K 0.30716(13) -0.07096(5) 0.13325(4) 0.0274(2) Uani 1 1 d . . . K4 K -0.36418(15) -0.07648(7) 0.00412(5) 0.0454(3) Uani 1 1 d . . . Fe1 Fe -0.53645(9) -0.27632(3) 0.13203(3) 0.0295(2) Uani 1 1 d . . . Fe2 Fe -0.11373(8) 0.06364(3) 0.10587(2) 0.02091(17) Uani 1 1 d . . . C1 C -0.4419(8) -0.2019(3) 0.1053(2) 0.0496(16) Uani 1 1 d . . . C2 C -0.6647(7) -0.2890(2) 0.0604(2) 0.0347(12) Uani 1 1 d . . . C3 C -0.7243(7) -0.2257(2) 0.14733(19) 0.0293(11) Uani 1 1 d . . . C4 C -0.3692(8) -0.3294(3) 0.1083(2) 0.0395(13) Uani 1 1 d . . . C5 C -0.5508(6) -0.3624(2) 0.2212(2) 0.0291(11) Uani 1 1 d . . . C6 C -0.5917(6) -0.4151(2) 0.2516(2) 0.0316(11) Uani 1 1 d . . . H6 H -0.5416 -0.4207 0.2887 0.038 Uiso 1 1 calc R . . C7 C -0.7045(7) -0.4586(2) 0.2274(2) 0.0371(13) Uani 1 1 d . . . H7 H -0.7331 -0.4949 0.2474 0.045 Uiso 1 1 calc R . . C8 C -0.7775(7) -0.4492(2) 0.1728(2) 0.0395(13) Uani 1 1 d . . . H8 H -0.8578 -0.4784 0.1555 0.047 Uiso 1 1 calc R . . C9 C -0.7310(7) -0.3965(2) 0.1444(2) 0.0344(12) Uani 1 1 d . . . H9 H -0.7798 -0.3902 0.1072 0.041 Uiso 1 1 calc R . . C10 C -0.4348(6) -0.3123(2) 0.24126(18) 0.0245(10) Uani 1 1 d . . . C11 C -0.3384(6) -0.2959(2) 0.2897(2) 0.0285(10) Uani 1 1 d . . . H11 H -0.3275 -0.3179 0.3239 0.034 Uiso 1 1 calc R . . C12 C -0.2597(6) -0.2391(2) 0.27741(19) 0.0255(10) Uani 1 1 d . . . C13 C -0.1461(6) -0.1973(2) 0.31425(18) 0.0265(10) Uani 1 1 d . . . C14 C -0.0998(7) -0.2127(2) 0.3690(2) 0.0347(12) Uani 1 1 d . . . H14 H -0.1347 -0.2521 0.3834 0.042 Uiso 1 1 calc R . . C15 C -0.0013(7) -0.1698(3) 0.4028(2) 0.0411(13) Uani 1 1 d . . . H15 H 0.0307 -0.1790 0.4407 0.049 Uiso 1 1 calc R . . C16 C 0.0494(7) -0.1138(3) 0.3806(2) 0.0422(13) Uani 1 1 d . . . H16 H 0.1165 -0.0835 0.4028 0.051 Uiso 1 1 calc R . . C17 C 0.0007(7) -0.1027(2) 0.3255(2) 0.0373(12) Uani 1 1 d . . . H17 H 0.0372 -0.0641 0.3104 0.045 Uiso 1 1 calc R . . C18 C -0.0584(6) -0.0202(2) 0.08145(17) 0.0257(10) Uani 1 1 d . . . C19 C -0.2288(6) 0.0811(2) 0.03261(19) 0.0252(10) Uani 1 1 d . . . C20 C 0.0705(6) 0.1046(2) 0.08187(17) 0.0238(9) Uani 1 1 d . . . C21 C -0.3191(8) 0.0285(2) 0.1178(2) 0.0435(15) Uani 1 1 d . . . C22 C -0.0952(6) 0.1521(2) 0.19552(18) 0.0240(10) Uani 1 1 d . . . C23 C -0.1257(6) 0.2045(2) 0.2276(2) 0.0282(10) Uani 1 1 d . . . H23 H -0.0760 0.2070 0.2651 0.034 Uiso 1 1 calc R . . C24 C -0.2292(6) 0.2530(2) 0.2044(2) 0.0337(12) Uani 1 1 d . . . H24 H -0.2509 0.2894 0.2257 0.040 Uiso 1 1 calc R . . C25 C -0.3005(6) 0.2481(2) 0.1503(2) 0.0342(12) Uani 1 1 d . . . H25 H -0.3724 0.2809 0.1338 0.041 Uiso 1 1 calc R . . C26 C -0.2665(6) 0.1949(2) 0.1200(2) 0.0307(11) Uani 1 1 d . . . H26 H -0.3156 0.1920 0.0826 0.037 Uiso 1 1 calc R . . C27 C 0.0080(6) 0.09779(19) 0.21419(17) 0.0221(9) Uani 1 1 d . . . C28 C 0.1173(6) 0.0820(2) 0.25987(18) 0.0237(9) Uani 1 1 d . . . H28 H 0.1454 0.1064 0.2928 0.028 Uiso 1 1 calc R . . C29 C 0.1783(6) 0.02122(19) 0.24680(17) 0.0226(9) Uani 1 1 d . . . C30 C 0.3061(6) -0.0181(2) 0.27994(18) 0.0239(10) Uani 1 1 d . . . C31 C 0.3548(6) -0.0055(2) 0.33600(19) 0.0313(11) Uani 1 1 d . . . H31 H 0.3085 0.0292 0.3533 0.038 Uiso 1 1 calc R . . C32 C 0.4719(7) -0.0449(3) 0.3654(2) 0.0379(12) Uani 1 1 d . . . H32 H 0.5047 -0.0384 0.4038 0.046 Uiso 1 1 calc R . . C33 C 0.5406(7) -0.0934(2) 0.3391(2) 0.0359(12) Uani 1 1 d . . . H33 H 0.6230 -0.1203 0.3584 0.043 Uiso 1 1 calc R . . C34 C 0.4860(7) -0.1019(2) 0.2832(2) 0.0339(12) Uani 1 1 d . . . H34 H 0.5337 -0.1355 0.2650 0.041 Uiso 1 1 calc R . . N1 N -0.3781(8) -0.1571(3) 0.0910(3) 0.087(2) Uani 1 1 d . . . N2 N -0.7481(7) -0.2926(2) 0.0180(2) 0.0500(13) Uani 1 1 d . . . N3 N -0.8372(6) -0.19698(19) 0.15332(16) 0.0349(10) Uani 1 1 d . . . N4 N -0.2661(7) -0.3595(3) 0.0954(2) 0.0539(14) Uani 1 1 d . . . N5 N -0.6186(5) -0.35414(17) 0.16793(16) 0.0278(9) Uani 1 1 d . . . N6 N -0.4144(5) -0.26693(18) 0.20254(15) 0.0275(9) Uani 1 1 d . . . N7 N -0.3045(5) -0.22185(18) 0.22422(16) 0.0276(9) Uani 1 1 d . . . N8 N -0.0958(5) -0.14300(19) 0.29166(16) 0.0318(9) Uani 1 1 d . . . N9 N -0.0325(5) -0.07311(17) 0.06965(14) 0.0280(9) Uani 1 1 d . . . N10 N -0.2995(6) 0.0863(2) -0.01197(18) 0.0419(11) Uani 1 1 d . . . N11 N 0.1791(6) 0.1296(2) 0.06707(17) 0.0383(11) Uani 1 1 d . . . N12 N -0.4449(9) 0.0093(3) 0.1193(3) 0.094(3) Uani 1 1 d . . . N13 N -0.1671(5) 0.14729(16) 0.14165(15) 0.0226(8) Uani 1 1 d . . . N14 N 0.0047(5) 0.04901(16) 0.17682(14) 0.0250(8) Uani 1 1 d . . . N15 N 0.1102(5) 0.00159(17) 0.19682(14) 0.0270(9) Uani 1 1 d . . . N16 N 0.3705(5) -0.06577(17) 0.25352(16) 0.0289(9) Uani 1 1 d . . . O1SA O 0.0888(12) 0.0377(5) 0.4400(4) 0.064(4) Uani 0.432(11) 1 d PDU A 1 H45 H 0.1941 0.0374 0.4463 0.095 Uiso 0.50 1 d PD B 1 C1SA C 0.039(2) 0.0301(7) 0.4908(5) 0.048(4) Uani 0.432(11) 1 d PDU A 1 H42 H 0.1331 0.0343 0.5202 0.072 Uiso 0.50 1 calc PR A 1 H43 H -0.0093 -0.0129 0.4927 0.072 Uiso 0.50 1 calc PR A 1 H44 H -0.0399 0.0638 0.4952 0.072 Uiso 0.50 1 calc PR A 1 O1SB O 0.313(3) -0.0188(12) 0.5014(7) 0.247(12) Uani 0.568(11) 1 d PDU A 2 H46 H 0.3179 -0.0164 0.4667 0.371 Uiso 0.50 1 d PD C 2 C1SB C 0.184(2) 0.0254(10) 0.5064(8) 0.106(6) Uani 0.568(11) 1 d PDU A 2 H38 H 0.2184 0.0552 0.5370 0.159 Uiso 0.50 1 calc PR A 2 H39 H 0.0893 0.0008 0.5132 0.159 Uiso 0.50 1 calc PR A 2 H40 H 0.1555 0.0504 0.4723 0.159 Uiso 0.50 1 calc PR A 2 O1 O -1.2104(8) -0.2806(4) 0.0027(2) 0.131(3) Uani 1 1 d . . . H1 H -1.1870 -0.3217 0.0196 0.157 Uiso 1 1 calc R . . C35 C -1.3645(9) -0.2780(4) -0.0311(3) 0.074(2) Uani 1 1 d . . . H35 H -1.4365 -0.2505 -0.0136 0.112 Uiso 1 1 calc R . . H36 H -1.4095 -0.3220 -0.0360 0.112 Uiso 1 1 calc R . . H37 H -1.3541 -0.2598 -0.0669 0.112 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0382(7) 0.0380(6) 0.0272(5) 0.0042(4) 0.0132(4) -0.0028(5) K2 0.0876(11) 0.0325(6) 0.0386(7) -0.0111(5) -0.0168(7) 0.0221(7) K3 0.0307(6) 0.0277(5) 0.0257(5) -0.0016(4) 0.0106(4) -0.0070(4) K4 0.0341(7) 0.0701(9) 0.0327(6) -0.0041(6) 0.0082(5) 0.0034(6) Fe1 0.0383(4) 0.0191(3) 0.0293(4) 0.0031(3) 0.0004(3) 0.0015(3) Fe2 0.0292(4) 0.0157(3) 0.0190(3) -0.0007(2) 0.0075(3) 0.0003(3) C1 0.055(4) 0.034(3) 0.052(4) 0.017(3) -0.013(3) -0.007(3) C2 0.045(3) 0.025(2) 0.032(3) 0.000(2) 0.000(2) 0.008(2) C3 0.041(3) 0.017(2) 0.027(2) 0.0007(18) -0.002(2) -0.001(2) C4 0.056(4) 0.035(3) 0.029(3) 0.012(2) 0.012(3) -0.001(3) C5 0.035(3) 0.018(2) 0.037(3) 0.0002(19) 0.014(2) 0.006(2) C6 0.039(3) 0.025(2) 0.035(3) 0.003(2) 0.016(2) 0.009(2) C7 0.042(3) 0.023(2) 0.053(3) 0.001(2) 0.023(3) 0.000(2) C8 0.042(3) 0.026(2) 0.054(4) -0.007(2) 0.019(3) -0.003(2) C9 0.040(3) 0.023(2) 0.042(3) -0.002(2) 0.010(2) 0.000(2) C10 0.029(3) 0.018(2) 0.029(2) 0.0011(17) 0.0116(19) 0.0128(19) C11 0.034(3) 0.023(2) 0.032(3) 0.0042(19) 0.015(2) 0.006(2) C12 0.027(3) 0.023(2) 0.028(2) 0.0020(18) 0.0092(19) 0.0070(19) C13 0.032(3) 0.023(2) 0.025(2) 0.0030(18) 0.0063(19) 0.006(2) C14 0.044(3) 0.031(3) 0.030(3) 0.005(2) 0.008(2) 0.004(2) C15 0.051(4) 0.042(3) 0.028(3) 0.005(2) 0.002(2) 0.006(3) C16 0.046(4) 0.039(3) 0.041(3) -0.002(2) 0.003(2) -0.002(3) C17 0.039(3) 0.034(3) 0.039(3) 0.005(2) 0.006(2) -0.004(2) C18 0.037(3) 0.026(2) 0.015(2) 0.0028(17) 0.0034(18) 0.000(2) C19 0.025(2) 0.025(2) 0.027(2) -0.0006(18) 0.0067(19) 0.0021(19) C20 0.030(3) 0.025(2) 0.017(2) -0.0043(17) 0.0046(18) 0.000(2) C21 0.063(4) 0.031(3) 0.047(3) -0.023(2) 0.038(3) -0.018(3) C22 0.029(3) 0.0159(19) 0.030(2) -0.0056(17) 0.0121(19) -0.0068(18) C23 0.033(3) 0.019(2) 0.034(3) -0.0091(18) 0.010(2) -0.008(2) C24 0.035(3) 0.021(2) 0.048(3) -0.013(2) 0.016(2) -0.004(2) C25 0.031(3) 0.020(2) 0.052(3) -0.007(2) 0.006(2) 0.003(2) C26 0.028(3) 0.026(2) 0.038(3) -0.004(2) 0.005(2) 0.002(2) C27 0.028(2) 0.017(2) 0.024(2) -0.0028(16) 0.0105(18) -0.0037(18) C28 0.028(3) 0.022(2) 0.023(2) -0.0041(17) 0.0095(18) -0.0042(19) C29 0.031(3) 0.0155(19) 0.021(2) 0.0027(16) 0.0056(18) -0.0031(18) C30 0.029(3) 0.017(2) 0.026(2) 0.0008(17) 0.0054(18) -0.0024(19) C31 0.038(3) 0.028(2) 0.029(3) -0.0013(19) 0.009(2) 0.001(2) C32 0.046(3) 0.044(3) 0.023(3) 0.006(2) 0.003(2) -0.001(3) C33 0.037(3) 0.031(3) 0.040(3) 0.006(2) 0.008(2) 0.000(2) C34 0.040(3) 0.022(2) 0.043(3) 0.002(2) 0.013(2) 0.003(2) N1 0.082(5) 0.068(4) 0.092(5) 0.057(3) -0.045(4) -0.037(4) N2 0.056(3) 0.046(3) 0.044(3) -0.009(2) -0.002(2) 0.004(3) N3 0.046(3) 0.025(2) 0.030(2) 0.0015(17) -0.0017(19) 0.003(2) N4 0.054(3) 0.064(3) 0.049(3) 0.017(3) 0.023(3) 0.019(3) N5 0.036(2) 0.0182(18) 0.030(2) -0.0013(15) 0.0070(17) 0.0029(17) N6 0.032(2) 0.0245(19) 0.025(2) 0.0036(15) 0.0024(16) 0.0039(17) N7 0.032(2) 0.0236(19) 0.028(2) 0.0041(15) 0.0063(17) 0.0008(17) N8 0.037(3) 0.030(2) 0.029(2) 0.0015(17) 0.0093(18) 0.0001(19) N9 0.044(3) 0.0204(19) 0.0196(19) -0.0035(15) 0.0062(17) 0.0057(18) N10 0.036(3) 0.055(3) 0.033(3) -0.001(2) 0.003(2) 0.015(2) N11 0.041(3) 0.043(3) 0.034(2) -0.0095(19) 0.015(2) -0.006(2) N12 0.096(5) 0.090(5) 0.119(6) -0.070(4) 0.080(5) -0.066(4) N13 0.028(2) 0.0137(16) 0.028(2) 0.0004(14) 0.0105(16) 0.0006(15) N14 0.041(2) 0.0159(17) 0.0183(18) -0.0021(14) 0.0068(16) 0.0009(17) N15 0.048(3) 0.0157(17) 0.0183(19) -0.0012(14) 0.0076(17) 0.0024(17) N16 0.036(2) 0.0204(18) 0.032(2) 0.0011(16) 0.0083(17) 0.0002(17) O1SA 0.068(5) 0.065(5) 0.059(5) -0.005(4) 0.015(4) -0.005(4) C1SA 0.059(6) 0.046(5) 0.040(5) 0.004(4) 0.012(4) 0.004(4) O1SB 0.250(12) 0.249(12) 0.241(12) -0.006(5) 0.039(5) -0.003(5) C1SB 0.109(8) 0.101(7) 0.108(7) 0.001(5) 0.015(5) -0.002(5) O1 0.082(5) 0.228(9) 0.078(4) 0.070(5) 0.000(3) -0.067(5) C35 0.056(5) 0.111(6) 0.058(5) 0.011(4) 0.016(4) -0.023(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 N8 2.837(4) . ? K1 N1 2.840(6) . ? K1 N7 2.870(4) . ? K1 N3 2.894(5) 1_655 ? K1 N9 3.067(4) . ? K1 N15 3.267(4) . ? K1 C18 3.328(4) . ? K1 C1 3.352(6) . ? K1 K3 4.914(3) 1_455 ? K2 O1 2.665(7) . ? K2 N9 2.776(4) 1_455 ? K2 N2 2.803(5) . ? K2 N11 3.007(5) 3_455 ? K2 N3 3.093(4) . ? K2 N10 3.271(5) 3_455 ? K2 C3 3.355(5) . ? K2 C19 3.394(5) 3_455 ? K2 K1 4.271(2) 1_455 ? K3 N12 2.726(6) 1_655 ? K3 N15 2.885(4) . ? K3 N16 2.933(4) . ? K3 N3 2.940(4) 1_655 ? K3 N10 3.005(5) 3 ? K3 N9 3.018(5) . ? K3 N1 3.489(8) 1_655 ? K3 K2 4.075(2) 1_655 ? K3 K4 4.565(2) 1_655 ? K3 K4 4.639(2) 3 ? K3 K1 4.914(3) 1_655 ? K4 N1 2.732(6) . ? K4 N11 2.765(4) 3 ? K4 N10 2.874(5) 3_455 ? K4 N9 2.978(5) . ? K4 C19 3.390(5) 3_455 ? K4 N10 3.427(5) . ? K4 C19 3.467(5) . ? K4 N12 3.512(5) . ? K4 C21 3.513(5) . ? K4 K2 4.057(2) 1_655 ? K4 K3 4.565(2) 1_455 ? K4 K3 4.639(2) 3 ? Fe1 N6 1.877(4) . ? Fe1 C1 1.895(6) . ? Fe1 C2 1.929(5) . ? Fe1 C4 1.948(6) . ? Fe1 C3 1.981(6) . ? Fe1 N5 2.009(4) . ? Fe2 N14 1.888(4) . ? Fe2 C18 1.910(5) . ? Fe2 C19 1.936(5) . ? Fe2 C21 1.940(6) . ? Fe2 C20 1.943(5) . ? Fe2 N13 2.020(3) . ? C1 N1 1.152(7) . ? C2 N2 1.160(7) . ? C3 N3 1.149(6) . ? C3 K3 3.218(5) 1_455 ? C4 N4 1.154(7) . ? C5 N5 1.355(6) . ? C5 C6 1.395(6) . ? C5 C10 1.448(7) . ? C6 C7 1.365(7) . ? C6 H6 0.9500 . ? C7 C8 1.398(8) . ? C7 H7 0.9500 . ? C8 C9 1.383(7) . ? C8 H8 0.9500 . ? C9 N5 1.344(6) . ? C9 H9 0.9500 . ? C10 N6 1.368(6) . ? C10 C11 1.370(7) . ? C11 C12 1.401(6) . ? C11 H11 0.9500 . ? C12 N7 1.352(6) . ? C12 C13 1.478(7) . ? C13 N8 1.349(6) . ? C13 C14 1.381(7) . ? C14 C15 1.389(8) . ? C14 H14 0.9500 . ? C15 C16 1.374(8) . ? C15 H15 0.9500 . ? C16 C17 1.373(7) . ? C16 H16 0.9500 . ? C17 N8 1.348(7) . ? C17 H17 0.9500 . ? C18 N9 1.158(5) . ? C19 N10 1.165(6) . ? C19 K4 3.390(5) 3_455 ? C19 K2 3.394(5) 3_455 ? C20 N11 1.160(6) . ? C21 N12 1.136(8) . ? C22 N13 1.369(6) . ? C22 C23 1.388(6) . ? C22 C27 1.441(6) . ? C23 C24 1.383(7) . ? C23 H23 0.9500 . ? C24 C25 1.375(7) . ? C24 H24 0.9500 . ? C25 C26 1.382(6) . ? C25 H25 0.9500 . ? C26 N13 1.339(6) . ? C26 H26 0.9500 . ? C27 N14 1.361(5) . ? C27 C28 1.368(6) . ? C28 C29 1.410(6) . ? C28 H28 0.9500 . ? C29 N15 1.333(6) . ? C29 C30 1.477(6) . ? C30 N16 1.342(6) . ? C30 C31 1.401(6) . ? C31 C32 1.383(7) . ? C31 H31 0.9500 . ? C32 C33 1.372(7) . ? C32 H32 0.9500 . ? C33 C34 1.391(7) . ? C33 H33 0.9500 . ? C34 N16 1.339(6) . ? C34 H34 0.9500 . ? N1 K3 14.142(10) 1_655 ? N3 K1 2.894(5) 1_455 ? N3 K3 2.940(4) 1_455 ? N6 N7 1.354(5) . ? N9 K2 2.776(4) 1_655 ? N10 K4 2.874(5) 3_455 ? N10 K3 3.005(5) 3 ? N10 K2 3.271(5) 3_455 ? N11 K4 2.766(4) 3 ? N11 K2 3.007(5) 3_455 ? N12 K3 2.726(6) 1_455 ? N14 N15 1.354(5) . ? O1SA C1SA 1.399(13) . ? O1SA H45 0.873(10) . ? C1SA H42 0.9800 . ? C1SA H43 0.9800 . ? C1SA H44 0.9800 . ? O1SB C1SB 1.436(10) . ? O1SB H46 0.868(15) . ? C1SB H45 1.522(18) . ? C1SB H38 0.9800 . ? C1SB H39 0.9800 . ? C1SB H40 0.9800 . ? O1 C35 1.418(9) . ? O1 H1 0.9500 . ? C35 H35 0.9800 . ? C35 H36 0.9800 . ? C35 H37 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 K1 N1 129.31(17) . . ? N8 K1 N7 57.32(12) . . ? N1 K1 N7 75.84(15) . . ? N8 K1 N3 103.26(12) . 1_655 ? N1 K1 N3 107.38(19) . 1_655 ? N7 K1 N3 105.73(12) . 1_655 ? N8 K1 N9 156.97(12) . . ? N1 K1 N9 72.48(16) . . ? N7 K1 N9 145.61(12) . . ? N3 K1 N9 72.06(11) 1_655 . ? N8 K1 N15 90.02(11) . . ? N1 K1 N15 130.17(13) . . ? N7 K1 N15 146.55(11) . . ? N3 K1 N15 87.44(12) 1_655 . ? N9 K1 N15 67.48(10) . . ? N8 K1 C18 142.22(12) . . ? N1 K1 C18 78.68(14) . . ? N7 K1 C18 153.74(12) . . ? N3 K1 C18 87.83(12) 1_655 . ? N9 K1 C18 20.33(10) . . ? N15 K1 C18 54.01(10) . . ? N8 K1 C1 112.63(14) . . ? N1 K1 C1 19.24(13) . . ? N7 K1 C1 57.01(13) . . ? N3 K1 C1 106.79(15) 1_655 . ? N9 K1 C1 90.08(14) . . ? N15 K1 C1 148.70(12) . . ? C18 K1 C1 97.87(13) . . ? N8 K1 K3 97.93(9) . 1_455 ? N1 K1 K3 44.10(17) . 1_455 ? N7 K1 K3 70.26(9) . 1_455 ? N3 K1 K3 151.45(9) 1_655 1_455 ? N9 K1 K3 95.16(9) . 1_455 ? N15 K1 K3 111.68(8) . 1_455 ? C18 K1 K3 87.00(9) . 1_455 ? C1 K1 K3 46.44(11) . 1_455 ? O1 K2 N9 120.6(2) . 1_455 ? O1 K2 N2 89.5(2) . . ? N9 K2 N2 148.17(15) 1_455 . ? O1 K2 N11 78.11(17) . 3_455 ? N9 K2 N11 76.60(12) 1_455 3_455 ? N2 K2 N11 123.51(14) . 3_455 ? O1 K2 N3 111.43(15) . . ? N9 K2 N3 73.21(11) 1_455 . ? N2 K2 N3 86.89(14) . . ? N11 K2 N3 148.94(12) 3_455 . ? O1 K2 N10 158.90(15) . 3_455 ? N9 K2 N10 66.82(12) 1_455 3_455 ? N2 K2 N10 88.92(15) . 3_455 ? N11 K2 N10 85.30(12) 3_455 3_455 ? N3 K2 N10 89.48(12) . 3_455 ? O1 K2 C3 114.59(16) . . ? N9 K2 C3 88.79(12) 1_455 . ? N2 K2 C3 67.61(14) . . ? N11 K2 C3 164.47(12) 3_455 . ? N3 K2 C3 20.01(11) . . ? N10 K2 C3 84.08(12) 3_455 . ? O1 K2 C19 139.34(15) . 3_455 ? N9 K2 C19 71.15(12) 1_455 3_455 ? N2 K2 C19 93.29(14) . 3_455 ? N11 K2 C19 66.71(12) 3_455 3_455 ? N3 K2 C19 109.22(12) . 3_455 ? N10 K2 C19 20.03(11) 3_455 3_455 ? C3 K2 C19 103.81(13) . 3_455 ? O1 K2 K1 96.28(16) . 1_455 ? N9 K2 K1 45.78(8) 1_455 1_455 ? N2 K2 K1 127.51(11) . 1_455 ? N11 K2 K1 108.67(9) 3_455 1_455 ? N3 K2 K1 42.65(9) . 1_455 ? N10 K2 K1 101.36(9) 3_455 1_455 ? C3 K2 K1 62.65(10) . 1_455 ? C19 K2 K1 113.41(9) 3_455 1_455 ? N12 K3 N15 106.13(15) 1_655 . ? N12 K3 N16 95.48(17) 1_655 . ? N15 K3 N16 56.69(11) . . ? N12 K3 N3 154.4(2) 1_655 1_655 ? N15 K3 N3 94.16(12) . 1_655 ? N16 K3 N3 82.53(11) . 1_655 ? N12 K3 N10 79.88(17) 1_655 3 ? N15 K3 N10 132.93(12) . 3 ? N16 K3 N10 170.10(12) . 3 ? N3 K3 N10 97.83(13) 1_655 3 ? N12 K3 N9 128.3(2) 1_655 . ? N15 K3 N9 73.23(11) . . ? N16 K3 N9 121.44(11) . . ? N3 K3 N9 72.16(11) 1_655 . ? N10 K3 N9 67.71(12) 3 . ? N12 K3 N1 68.54(17) 1_655 1_655 ? N15 K3 N1 163.84(13) . 1_655 ? N16 K3 N1 107.81(13) . 1_655 ? N3 K3 N1 87.64(13) 1_655 1_655 ? N10 K3 N1 62.39(13) 3 1_655 ? N9 K3 N1 122.38(13) . 1_655 ? N12 K3 K2 132.00(13) 1_655 1_655 ? N15 K3 K2 110.22(10) . 1_655 ? N16 K3 K2 130.59(8) . 1_655 ? N3 K3 K2 49.13(8) 1_655 1_655 ? N10 K3 K2 52.43(10) 3 1_655 ? N9 K3 K2 42.94(7) . 1_655 ? N1 K3 K2 83.01(11) 1_655 1_655 ? N12 K3 K4 50.19(11) 1_655 1_655 ? N15 K3 K4 149.94(8) . 1_655 ? N16 K3 K4 133.08(9) . 1_655 ? N3 K3 K4 114.36(9) 1_655 1_655 ? N10 K3 K4 38.03(9) 3 1_655 ? N9 K3 K4 105.49(8) . 1_655 ? N1 K3 K4 36.67(9) 1_655 1_655 ? K2 K3 K4 83.92(5) 1_655 1_655 ? N12 K3 K4 48.32(19) 1_655 3 ? N15 K3 K4 101.59(8) . 3 ? N16 K3 K4 134.03(8) . 3 ? N3 K3 K4 142.85(9) 1_655 3 ? N10 K3 K4 47.59(10) 3 3 ? N9 K3 K4 80.47(8) . 3 ? N1 K3 K4 86.26(9) 1_655 3 ? K2 K3 K4 93.74(5) 1_655 3 ? K4 K3 K4 49.76(4) 1_655 3 ? N12 K3 K1 54.97(19) 1_655 1_655 ? N15 K3 K1 129.72(9) . 1_655 ? N16 K3 K1 77.61(9) . 1_655 ? N3 K3 K1 99.96(10) 1_655 1_655 ? N10 K3 K1 92.62(9) 3 1_655 ? N9 K3 K1 156.86(7) . 1_655 ? N1 K3 K1 34.50(10) 1_655 1_655 ? K2 K3 K1 115.46(4) 1_655 1_655 ? K4 K3 K1 57.05(3) 1_655 1_655 ? K4 K3 K1 95.43(3) 3 1_655 ? N1 K4 N11 111.4(2) . 3 ? N1 K4 N10 74.33(17) . 3_455 ? N11 K4 N10 132.98(14) 3 3_455 ? N1 K4 N9 75.38(15) . . ? N11 K4 N9 77.24(13) 3 . ? N10 K4 N9 143.69(12) 3_455 . ? N1 K4 C19 91.01(16) . 3_455 ? N11 K4 C19 118.06(13) 3 3_455 ? N10 K4 C19 19.27(11) 3_455 3_455 ? N9 K4 C19 162.89(11) . 3_455 ? N1 K4 N10 135.50(18) . . ? N11 K4 N10 101.24(13) 3 . ? N10 K4 N10 104.72(12) 3_455 . ? N9 K4 N10 83.57(11) . . ? C19 K4 N10 99.72(11) 3_455 . ? N1 K4 C19 117.64(17) . . ? N11 K4 C19 107.33(13) 3 . ? N10 K4 C19 110.19(13) 3_455 . ? N9 K4 C19 67.85(11) . . ? C19 K4 C19 111.23(10) 3_455 . ? N10 K4 C19 19.45(10) . . ? N1 K4 N12 68.1(2) . . ? N11 K4 N12 157.19(16) 3 . ? N10 K4 N12 69.68(15) 3_455 . ? N9 K4 N12 80.76(16) . . ? C19 K4 N12 84.58(15) 3_455 . ? N10 K4 N12 70.10(14) . . ? C19 K4 N12 57.86(12) . . ? N1 K4 C21 75.94(19) . . ? N11 K4 C21 139.14(15) 3 . ? N10 K4 C21 87.88(14) 3_455 . ? N9 K4 C21 65.59(13) . . ? C19 K4 C21 101.43(13) 3_455 . ? N10 K4 C21 59.64(12) . . ? C19 K4 C21 43.62(11) . . ? N12 K4 C21 18.61(13) . . ? N1 K4 K2 70.10(17) . 1_655 ? N11 K4 K2 47.83(10) 3 1_655 ? N10 K4 K2 136.92(11) 3_455 1_655 ? N9 K4 K2 43.17(7) . 1_655 ? C19 K4 K2 141.33(9) 3_455 1_655 ? N10 K4 K2 117.57(9) . 1_655 ? C19 K4 K2 107.43(9) . 1_655 ? N12 K4 K2 116.27(15) . 1_655 ? C21 K4 K2 105.86(12) . 1_655 ? N1 K4 K3 49.70(18) . 1_455 ? N11 K4 K3 158.13(10) 3 1_455 ? N10 K4 K3 40.10(9) 3_455 1_455 ? N9 K4 K3 103.95(9) . 1_455 ? C19 K4 K3 58.96(8) 3_455 1_455 ? N10 K4 K3 100.58(8) . 1_455 ? C19 K4 K3 92.96(8) . 1_455 ? N12 K4 K3 36.60(9) . 1_455 ? C21 K4 K3 54.63(9) . 1_455 ? K2 K4 K3 118.80(4) 1_655 1_455 ? N1 K4 K3 174.97(13) . 3 ? N11 K4 K3 69.70(10) 3 3 ? N10 K4 K3 108.72(10) 3_455 3 ? N9 K4 K3 100.33(8) . 3 ? C19 K4 K3 92.71(8) 3_455 3 ? N10 K4 K3 40.34(8) . 3 ? C19 K4 K3 57.75(8) . 3 ? N12 K4 K3 108.87(13) . 3 ? C21 K4 K3 99.98(10) . 3 ? K2 K4 K3 108.68(4) 1_655 3 ? K3 K4 K3 130.24(4) 1_455 3 ? N6 Fe1 C1 92.6(2) . . ? N6 Fe1 C2 177.92(19) . . ? C1 Fe1 C2 89.5(2) . . ? N6 Fe1 C4 91.6(2) . . ? C1 Fe1 C4 88.9(3) . . ? C2 Fe1 C4 88.1(2) . . ? N6 Fe1 C3 95.53(18) . . ? C1 Fe1 C3 92.1(2) . . ? C2 Fe1 C3 84.7(2) . . ? C4 Fe1 C3 172.7(2) . . ? N6 Fe1 N5 81.17(16) . . ? C1 Fe1 N5 173.7(2) . . ? C2 Fe1 N5 96.76(19) . . ? C4 Fe1 N5 90.39(18) . . ? C3 Fe1 N5 89.38(18) . . ? N14 Fe2 C18 91.81(17) . . ? N14 Fe2 C19 177.76(19) . . ? C18 Fe2 C19 88.92(18) . . ? N14 Fe2 C21 98.1(2) . . ? C18 Fe2 C21 89.0(2) . . ? C19 Fe2 C21 84.0(2) . . ? N14 Fe2 C20 91.79(18) . . ? C18 Fe2 C20 92.61(19) . . ? C19 Fe2 C20 86.06(19) . . ? C21 Fe2 C20 169.9(2) . . ? N14 Fe2 N13 81.38(15) . . ? C18 Fe2 N13 172.52(16) . . ? C19 Fe2 N13 98.01(17) . . ? C21 Fe2 N13 88.94(18) . . ? C20 Fe2 N13 90.67(16) . . ? N1 C1 Fe1 176.7(5) . . ? N1 C1 K1 54.3(4) . . ? Fe1 C1 K1 122.4(2) . . ? N2 C2 Fe1 175.1(5) . . ? N3 C3 Fe1 176.3(4) . . ? N3 C3 K3 65.8(3) . 1_455 ? Fe1 C3 K3 114.6(2) . 1_455 ? N3 C3 K2 67.0(3) . . ? Fe1 C3 K2 109.31(18) . . ? K3 C3 K2 76.59(10) 1_455 . ? N4 C4 Fe1 177.6(6) . . ? N5 C5 C6 121.3(5) . . ? N5 C5 C10 113.0(4) . . ? C6 C5 C10 125.7(5) . . ? C7 C6 C5 119.3(5) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 119.4(5) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 118.9(5) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? N5 C9 C8 121.8(5) . . ? N5 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? N6 C10 C11 108.5(4) . . ? N6 C10 C5 113.8(4) . . ? C11 C10 C5 137.6(4) . . ? C10 C11 C12 104.3(4) . . ? C10 C11 H11 127.9 . . ? C12 C11 H11 127.9 . . ? N7 C12 C11 111.5(4) . . ? N7 C12 C13 119.4(4) . . ? C11 C12 C13 129.1(4) . . ? N8 C13 C14 122.7(5) . . ? N8 C13 C12 116.2(4) . . ? C14 C13 C12 121.1(4) . . ? C13 C14 C15 118.9(5) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 119.1(5) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 118.4(5) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? N8 C17 C16 124.1(5) . . ? N8 C17 H17 118.0 . . ? C16 C17 H17 118.0 . . ? N9 C18 Fe2 174.3(4) . . ? N9 C18 K1 67.0(3) . . ? Fe2 C18 K1 107.65(17) . . ? N10 C19 Fe2 174.7(4) . . ? N10 C19 K4 54.5(3) . 3_455 ? Fe2 C19 K4 124.51(19) . 3_455 ? N10 C19 K2 74.0(3) . 3_455 ? Fe2 C19 K2 109.82(19) . 3_455 ? K4 C19 K2 117.15(14) 3_455 3_455 ? N10 C19 K4 78.3(3) . . ? Fe2 C19 K4 96.41(16) . . ? K4 C19 K4 68.77(10) 3_455 . ? K2 C19 K4 136.43(14) 3_455 . ? N11 C20 Fe2 179.1(5) . . ? N12 C21 Fe2 173.0(7) . . ? N12 C21 K4 80.7(4) . . ? Fe2 C21 K4 94.90(16) . . ? N13 C22 C23 121.2(4) . . ? N13 C22 C27 113.4(4) . . ? C23 C22 C27 125.3(4) . . ? C24 C23 C22 119.2(5) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 C23 119.3(4) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 119.3(5) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? N13 C26 C25 122.4(5) . . ? N13 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? N14 C27 C28 108.6(4) . . ? N14 C27 C22 114.3(4) . . ? C28 C27 C22 137.0(4) . . ? C27 C28 C29 103.9(4) . . ? C27 C28 H28 128.0 . . ? C29 C28 H28 128.0 . . ? N15 C29 C28 111.4(4) . . ? N15 C29 C30 120.4(4) . . ? C28 C29 C30 128.2(4) . . ? N16 C30 C31 122.9(4) . . ? N16 C30 C29 116.5(4) . . ? C31 C30 C29 120.7(4) . . ? C32 C31 C30 118.3(4) . . ? C32 C31 H31 120.8 . . ? C30 C31 H31 120.8 . . ? C33 C32 C31 119.7(5) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 118.0(5) . . ? C32 C33 H33 121.0 . . ? C34 C33 H33 121.0 . . ? N16 C34 C33 124.1(5) . . ? N16 C34 H34 118.0 . . ? C33 C34 H34 118.0 . . ? C1 N1 K4 144.2(5) . . ? C1 N1 K1 106.4(4) . . ? K4 N1 K1 109.0(2) . . ? C1 N1 K3 126.2(5) . 1_655 ? K4 N1 K3 78.80(14) . 1_655 ? K1 N1 K3 44.10(14) . 1_655 ? C2 N2 K2 100.3(4) . . ? C3 N3 K1 175.8(4) . 1_455 ? C3 N3 K3 93.3(3) . 1_455 ? K1 N3 K3 88.47(12) 1_455 1_455 ? C3 N3 K2 92.9(3) . . ? K1 N3 K2 90.95(13) 1_455 . ? K3 N3 K2 84.92(11) 1_455 . ? C9 N5 C5 119.2(4) . . ? C9 N5 Fe1 126.5(3) . . ? C5 N5 Fe1 114.2(3) . . ? N7 N6 C10 110.4(4) . . ? N7 N6 Fe1 131.8(3) . . ? C10 N6 Fe1 117.8(3) . . ? C12 N7 N6 105.3(4) . . ? C12 N7 K1 119.6(3) . . ? N6 N7 K1 133.2(3) . . ? C17 N8 C13 116.8(4) . . ? C17 N8 K1 119.0(3) . . ? C13 N8 K1 122.4(3) . . ? C18 N9 K2 173.3(3) . 1_655 ? C18 N9 K4 87.7(3) . . ? K2 N9 K4 89.61(11) 1_655 . ? C18 N9 K3 93.2(3) . . ? K2 N9 K3 89.28(12) 1_655 . ? K4 N9 K3 178.40(14) . . ? C18 N9 K1 92.6(3) . . ? K2 N9 K1 93.79(11) 1_655 . ? K4 N9 K1 97.27(13) . . ? K3 N9 K1 83.95(10) . . ? C19 N10 K4 106.2(4) . 3_455 ? C19 N10 K3 148.7(4) . 3 ? K4 N10 K3 101.87(14) 3_455 3 ? C19 N10 K2 85.9(3) . 3_455 ? K4 N10 K2 140.69(17) 3_455 3_455 ? K3 N10 K2 80.84(12) 3 3_455 ? C19 N10 K4 82.2(3) . . ? K4 N10 K4 75.28(12) 3_455 . ? K3 N10 K4 92.07(12) 3 . ? K2 N10 K4 144.02(15) 3_455 . ? C20 N11 K4 125.7(3) . 3 ? C20 N11 K2 93.8(4) . 3_455 ? K4 N11 K2 89.21(13) 3 3_455 ? C21 N12 K3 162.0(7) . 1_455 ? C21 N12 K4 80.7(4) . . ? K3 N12 K4 93.22(15) 1_455 . ? C26 N13 C22 118.6(4) . . ? C26 N13 Fe2 128.2(3) . . ? C22 N13 Fe2 113.2(3) . . ? N15 N14 C27 110.3(4) . . ? N15 N14 Fe2 131.5(3) . . ? C27 N14 Fe2 117.4(3) . . ? C29 N15 N14 105.8(3) . . ? C29 N15 K3 117.8(3) . . ? N14 N15 K3 125.1(3) . . ? C29 N15 K1 122.5(3) . . ? N14 N15 K1 101.5(3) . . ? K3 N15 K1 82.59(9) . . ? C34 N16 C30 117.0(4) . . ? C34 N16 K3 121.7(3) . . ? C30 N16 K3 120.1(3) . . ? C1SA O1SA H45 106.5(12) . . ? C1SB O1SB H46 102.5(19) . . ? O1SB C1SB H45 81.3(12) . . ? O1SB C1SB H38 109.5 . . ? O1SB C1SB H39 109.5 . . ? H38 C1SB H39 109.5 . . ? O1SB C1SB H40 109.5 . . ? H38 C1SB H40 109.5 . . ? H39 C1SB H40 109.5 . . ? C35 O1 K2 133.8(6) . . ? C35 O1 H1 113.1 . . ? K2 O1 H1 113.1 . . ? O1 C35 H35 109.5 . . ? O1 C35 H36 109.5 . . ? H35 C35 H36 109.5 . . ? O1 C35 H37 109.5 . . ? H35 C35 H37 109.5 . . ? H36 C35 H37 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.045 _refine_diff_density_min -1.210 _refine_diff_density_rms 0.147 data_Comp2 _database_code_depnum_ccdc_archive 'CCDC 883726' #TrackingRef '- TetraCN.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H46 Fe2 N20 Ni2, C2 O3, 5(O)' _chemical_formula_sum 'C64 H46 Fe2 N20 Ni2 O8' _chemical_formula_weight 1452.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 13.334(2) _cell_length_b 20.437(3) _cell_length_c 11.9421(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3254.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5092 _cell_measurement_theta_min 2.2895 _cell_measurement_theta_max 26.5815 _exptl_crystal_description plates _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7744 _exptl_absorpt_correction_T_max 0.9481 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18523 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.42 _reflns_number_total 7251 _reflns_number_gt 6389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Methanol molecules in the lattice were treated by DFIX restraints. ; _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^)+(0.0543P)^2^+0.3847P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(14) _chemical_absolute_configuration rmad _refine_ls_number_reflns 7251 _refine_ls_number_parameters 444 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.66332(3) 0.11487(2) 0.82986(4) 0.01800(12) Uani 1 1 d . . . Ni1 Ni 0.36348(3) 0.130938(19) 0.78714(3) 0.01586(10) Uani 1 1 d . . . C1 C 0.5441(2) 0.13237(16) 0.9129(3) 0.0194(7) Uani 1 1 d . . . C2 C 0.6506(2) 0.01994(16) 0.8411(3) 0.0188(7) Uani 1 1 d . . . C3 C 0.7527(3) 0.10767(18) 0.9574(3) 0.0300(9) Uani 1 1 d . . . C4 C 0.6965(2) 0.20817(16) 0.8273(3) 0.0204(7) Uani 1 1 d . . . C5 C 0.7342(3) 0.08521(16) 0.6096(3) 0.0217(8) Uani 1 1 d . . . C6 C 0.7978(3) 0.06796(17) 0.5210(3) 0.0249(8) Uani 1 1 d . . . H1 H 0.7716 0.0610 0.4481 0.030 Uiso 1 1 calc R . . C7 C 0.8985(3) 0.06127(18) 0.5411(4) 0.0316(9) Uani 1 1 d . . . H2 H 0.9426 0.0485 0.4827 0.038 Uiso 1 1 calc R . . C8 C 0.9350(3) 0.07331(18) 0.6474(4) 0.0316(9) Uani 1 1 d . . . H3 H 1.0048 0.0696 0.6623 0.038 Uiso 1 1 calc R . . C9 C 0.8698(3) 0.09074(17) 0.7317(3) 0.0269(8) Uani 1 1 d . . . H4 H 0.8959 0.0993 0.8042 0.032 Uiso 1 1 calc R . . C10 C 0.6260(3) 0.09120(15) 0.6023(3) 0.0187(7) Uani 1 1 d . . . C11 C 0.5531(3) 0.08015(15) 0.5239(3) 0.0200(7) Uani 1 1 d . . . H5 H 0.5613 0.0660 0.4487 0.024 Uiso 1 1 calc R . . C12 C 0.4637(2) 0.09454(15) 0.5800(3) 0.0173(7) Uani 1 1 d . . . C13 C 0.3593(3) 0.09707(14) 0.5463(3) 0.0178(7) Uani 1 1 d . . . C14 C 0.3273(3) 0.08476(16) 0.4368(3) 0.0222(7) Uani 1 1 d . . . H6 H 0.3736 0.0711 0.3810 0.027 Uiso 1 1 calc R . . C15 C 0.2260(3) 0.09287(17) 0.4111(3) 0.0255(8) Uani 1 1 d . . . H7 H 0.2022 0.0850 0.3373 0.031 Uiso 1 1 calc R . . C16 C 0.1608(3) 0.11256(17) 0.4944(3) 0.0253(7) Uani 1 1 d . . . H8 H 0.0917 0.1189 0.4788 0.030 Uiso 1 1 calc R . . C17 C 0.1983(2) 0.12284(16) 0.6013(3) 0.0195(7) Uani 1 1 d . . . H9 H 0.1529 0.1361 0.6583 0.023 Uiso 1 1 calc R . . C18 C 0.2113(3) 0.22176(18) 0.8617(3) 0.0210(7) Uani 1 1 d . . . C19 C 0.1217(3) 0.24822(19) 0.8993(3) 0.0299(8) Uani 1 1 d . . . H10 H 0.1099 0.2940 0.8948 0.036 Uiso 1 1 calc R . . C20 C 0.0496(3) 0.2068(2) 0.9437(3) 0.0339(10) Uani 1 1 d . . . H11 H -0.0122 0.2238 0.9708 0.041 Uiso 1 1 calc R . . C21 C 0.0688(3) 0.1412(2) 0.9479(3) 0.0328(9) Uani 1 1 d . . . H12 H 0.0201 0.1119 0.9772 0.039 Uiso 1 1 calc R . . C22 C 0.1600(3) 0.11756(19) 0.9091(3) 0.0257(7) Uani 1 1 d . . . H13 H 0.1731 0.0719 0.9136 0.031 Uiso 1 1 calc R . . C23 C 0.2916(3) 0.26086(16) 0.8123(3) 0.0202(7) Uani 1 1 d . . . H14 H 0.2879 0.3073 0.8124 0.024 Uiso 1 1 calc R . . C24 C 0.4496(2) 0.26867(16) 0.7168(3) 0.0202(7) Uani 1 1 d . . . H15 H 0.5134 0.2486 0.7440 0.024 Uiso 1 1 calc R . . C25 C 0.4538(3) 0.34113(17) 0.7465(3) 0.0290(9) Uani 1 1 d . . . H16 H 0.3948 0.3634 0.7159 0.044 Uiso 1 1 calc R . . H17 H 0.5147 0.3605 0.7147 0.044 Uiso 1 1 calc R . . H18 H 0.4547 0.3461 0.8282 0.044 Uiso 1 1 calc R . . C26 C 0.4459(3) 0.25838(15) 0.5909(3) 0.0196(7) Uani 1 1 d . . . C27 C 0.5332(3) 0.24431(17) 0.5309(3) 0.0263(8) Uani 1 1 d . . . H19 H 0.5953 0.2396 0.5691 0.032 Uiso 1 1 calc R . . C28 C 0.5291(3) 0.23715(18) 0.4154(3) 0.0305(9) Uani 1 1 d . . . H20 H 0.5888 0.2283 0.3747 0.037 Uiso 1 1 calc R . . C29 C 0.4393(3) 0.24273(18) 0.3592(3) 0.0320(9) Uani 1 1 d . . . H21 H 0.4370 0.2365 0.2804 0.038 Uiso 1 1 calc R . . C30 C 0.3530(3) 0.25732(17) 0.4168(3) 0.0297(8) Uani 1 1 d . . . H22 H 0.2914 0.2619 0.3777 0.036 Uiso 1 1 calc R . . C31 C 0.3557(3) 0.26552(16) 0.5328(3) 0.0249(7) Uani 1 1 d . . . H23 H 0.2960 0.2760 0.5723 0.030 Uiso 1 1 calc R . . N1 N 0.4632(2) 0.14390(15) 0.9434(3) 0.0243(7) Uani 1 1 d . . . N2 N 0.6477(2) -0.03579(13) 0.8318(2) 0.0199(6) Uani 1 1 d . . . N3 N 0.8090(3) 0.10081(18) 1.0272(4) 0.0532(12) Uani 1 1 d . . . N4 N 0.7173(2) 0.26259(15) 0.8274(3) 0.0303(7) Uani 1 1 d . . . N5 N 0.7705(2) 0.09609(13) 0.7149(3) 0.0203(6) Uani 1 1 d . . . N6 N 0.58248(18) 0.11129(12) 0.7001(2) 0.0167(5) Uani 1 1 d . . . N7 N 0.48309(19) 0.11263(12) 0.6858(2) 0.0165(6) Uani 1 1 d . . . N8 N 0.2946(2) 0.11517(13) 0.6284(2) 0.0188(6) Uani 1 1 d . . . N9 N 0.2301(2) 0.15708(14) 0.8655(2) 0.0201(6) Uani 1 1 d . . . N10 N 0.3666(2) 0.23192(13) 0.7692(2) 0.0196(6) Uani 1 1 d . . . O1SA O 0.6775(4) 0.0888(3) 0.2736(4) 0.0980(15) Uani 1 1 d DU . . O1SB O 0.4755(7) 0.0481(5) 0.2130(7) 0.093(3) Uani 0.50 1 d PDU A 2 O2S O 0.1789(4) 0.0106(2) 0.1659(4) 0.0918(17) Uani 1 1 d . . . O3S O 0.3132(2) 0.11419(14) 0.1287(2) 0.0370(7) Uani 1 1 d . . . O4S O 1.0000 0.0000 0.3041(3) 0.0378(10) Uani 1 2 d S B 1 C1SB C 0.5000 0.0000 0.1267(11) 0.147(6) Uani 1 2 d SDU . 2 C1SA C 0.5885(10) 0.0808(10) 0.2009(16) 0.124(6) Uani 0.50 1 d PDU C 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0136(2) 0.0167(2) 0.0237(2) -0.00447(19) -0.00240(18) -0.00025(17) Ni1 0.01322(19) 0.01638(19) 0.0180(2) -0.00070(16) 0.00117(16) -0.00011(15) C1 0.0230(17) 0.0159(15) 0.0192(17) -0.0057(14) -0.0046(13) -0.0005(14) C2 0.0116(16) 0.0255(17) 0.0193(17) -0.0021(14) 0.0003(13) 0.0027(13) C3 0.029(2) 0.0202(18) 0.040(2) -0.0053(17) -0.0106(17) 0.0001(15) C4 0.0167(15) 0.0211(16) 0.0235(18) -0.0024(15) 0.0023(14) -0.0007(13) C5 0.0187(17) 0.0146(15) 0.032(2) -0.0033(15) 0.0023(15) -0.0022(13) C6 0.0234(18) 0.0211(17) 0.030(2) -0.0012(16) 0.0090(15) 0.0001(14) C7 0.0229(19) 0.0234(18) 0.049(3) -0.0090(18) 0.0129(18) 0.0009(15) C8 0.0119(16) 0.0256(18) 0.057(3) -0.0044(18) 0.0015(17) 0.0012(14) C9 0.0173(16) 0.0243(16) 0.039(2) -0.0058(15) -0.0026(16) -0.0017(14) C10 0.0189(17) 0.0148(14) 0.0223(17) -0.0020(13) 0.0040(14) -0.0005(13) C11 0.0222(17) 0.0162(16) 0.0217(18) -0.0045(14) 0.0015(14) 0.0005(13) C12 0.0186(17) 0.0141(15) 0.0192(18) -0.0022(13) -0.0014(13) -0.0018(12) C13 0.0176(16) 0.0142(14) 0.0215(17) 0.0011(12) -0.0011(14) -0.0001(13) C14 0.0231(18) 0.0220(16) 0.0214(18) -0.0014(14) 0.0004(14) 0.0019(14) C15 0.029(2) 0.0273(18) 0.0199(19) -0.0011(15) -0.0071(16) -0.0029(15) C16 0.0204(17) 0.0268(17) 0.0285(19) 0.0018(15) -0.0048(14) -0.0050(15) C17 0.0150(15) 0.0218(16) 0.0217(17) 0.0004(15) 0.0014(12) 0.0011(13) C18 0.0196(17) 0.0288(18) 0.0147(16) -0.0051(14) 0.0000(13) 0.0045(14) C19 0.027(2) 0.034(2) 0.029(2) -0.0096(16) 0.0010(16) 0.0077(16) C20 0.0155(18) 0.058(3) 0.029(2) -0.0154(19) 0.0034(15) 0.0048(18) C21 0.0165(17) 0.054(3) 0.028(2) -0.0097(19) 0.0047(15) -0.0080(18) C22 0.0193(17) 0.0351(19) 0.0226(18) -0.0003(16) 0.0007(14) -0.0032(16) C23 0.0224(17) 0.0177(15) 0.0207(19) -0.0037(14) -0.0005(13) 0.0018(13) C24 0.0188(16) 0.0202(15) 0.0216(17) -0.0019(15) 0.0010(14) -0.0022(12) C25 0.036(2) 0.0204(17) 0.030(2) -0.0038(15) 0.0047(17) -0.0058(16) C26 0.0270(18) 0.0131(15) 0.0188(17) 0.0012(13) 0.0023(14) -0.0021(13) C27 0.025(2) 0.0228(18) 0.031(2) -0.0008(16) 0.0046(16) -0.0027(15) C28 0.036(2) 0.0266(19) 0.029(2) -0.0041(17) 0.0130(17) -0.0029(17) C29 0.048(2) 0.0263(19) 0.022(2) 0.0002(15) 0.0030(17) -0.0042(18) C30 0.036(2) 0.0281(18) 0.0251(19) 0.0023(15) -0.0068(17) -0.0049(17) C31 0.0238(19) 0.0239(16) 0.0270(19) -0.0009(14) 0.0003(15) -0.0011(15) N1 0.0214(16) 0.0263(16) 0.0253(16) -0.0062(13) -0.0040(12) -0.0037(13) N2 0.0157(14) 0.0215(14) 0.0224(14) -0.0016(12) -0.0018(12) -0.0005(11) N3 0.064(3) 0.033(2) 0.063(3) -0.0049(18) -0.041(2) 0.0055(18) N4 0.0291(17) 0.0285(17) 0.0334(18) -0.0046(15) 0.0085(15) -0.0018(13) N5 0.0154(13) 0.0174(13) 0.0281(16) -0.0044(13) 0.0003(13) 0.0000(10) N6 0.0131(12) 0.0160(12) 0.0209(15) -0.0007(12) 0.0007(10) 0.0012(10) N7 0.0135(12) 0.0152(13) 0.0207(15) 0.0010(12) 0.0003(10) 0.0006(10) N8 0.0166(13) 0.0163(13) 0.0236(15) 0.0019(12) 0.0021(11) -0.0022(11) N9 0.0159(14) 0.0268(15) 0.0175(15) -0.0038(12) -0.0005(11) -0.0001(12) N10 0.0195(14) 0.0196(13) 0.0198(15) -0.0024(11) 0.0012(12) -0.0006(11) O1SA 0.105(4) 0.133(4) 0.055(3) -0.001(3) 0.019(3) -0.002(3) O1SB 0.100(7) 0.115(7) 0.066(6) -0.002(5) -0.002(5) 0.061(6) O2S 0.095(3) 0.100(3) 0.081(3) -0.059(3) 0.052(3) -0.049(3) O3S 0.0434(17) 0.0345(15) 0.0332(15) -0.0044(12) -0.0006(12) 0.0099(13) O4S 0.053(3) 0.0283(19) 0.032(3) 0.000 0.000 0.0120(18) C1SB 0.194(15) 0.152(12) 0.095(9) 0.000 0.000 0.106(12) C1SA 0.053(8) 0.156(16) 0.164(16) 0.008(14) 0.022(8) -0.019(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N6 1.889(3) . ? Fe1 C1 1.908(3) . ? Fe1 C3 1.940(4) . ? Fe1 C2 1.952(3) . ? Fe1 C4 1.958(3) . ? Fe1 N5 2.019(3) . ? Ni1 N2 2.022(3) 2_655 ? Ni1 N7 2.037(3) . ? Ni1 N10 2.075(3) . ? Ni1 N9 2.080(3) . ? Ni1 N8 2.132(3) . ? Ni1 N1 2.306(3) . ? C1 N1 1.162(4) . ? C2 N2 1.145(4) . ? C3 N3 1.131(5) . ? C4 N4 1.146(4) . ? C5 N5 1.365(5) . ? C5 C6 1.401(5) . ? C5 C10 1.450(5) . ? C6 C7 1.370(5) . ? C6 H1 0.9500 . ? C7 C8 1.381(6) . ? C7 H2 0.9500 . ? C8 C9 1.377(5) . ? C8 H3 0.9500 . ? C9 N5 1.343(4) . ? C9 H4 0.9500 . ? C10 C11 1.369(5) . ? C10 N6 1.367(4) . ? C11 C12 1.399(5) . ? C11 H5 0.9500 . ? C12 N7 1.341(4) . ? C12 C13 1.450(5) . ? C13 N8 1.357(4) . ? C13 C14 1.398(5) . ? C14 C15 1.395(5) . ? C14 H6 0.9500 . ? C15 C16 1.381(5) . ? C15 H7 0.9500 . ? C16 C17 1.387(5) . ? C16 H8 0.9500 . ? C17 N8 1.333(4) . ? C17 H9 0.9500 . ? C18 N9 1.346(5) . ? C18 C19 1.387(5) . ? C18 C23 1.460(5) . ? C19 C20 1.386(6) . ? C19 H10 0.9500 . ? C20 C21 1.367(6) . ? C20 H11 0.9500 . ? C21 C22 1.387(5) . ? C21 H12 0.9500 . ? C22 N9 1.341(4) . ? C22 H13 0.9500 . ? C23 N10 1.270(4) . ? C23 H14 0.9500 . ? C24 N10 1.476(4) . ? C24 C26 1.519(5) . ? C24 C25 1.524(4) . ? C24 H15 1.0000 . ? C25 H16 0.9800 . ? C25 H17 0.9800 . ? C25 H18 0.9800 . ? C26 C31 1.397(5) . ? C26 C27 1.397(5) . ? C27 C28 1.389(5) . ? C27 H19 0.9500 . ? C28 C29 1.377(6) . ? C28 H20 0.9500 . ? C29 C30 1.373(6) . ? C29 H21 0.9500 . ? C30 C31 1.396(5) . ? C30 H22 0.9500 . ? C31 H23 0.9500 . ? N2 Ni1 2.022(3) 2_655 ? N6 N7 1.337(4) . ? O1SA C1SA 1.480(14) . ? O1SB C1SB 1.462(11) . ? C1SB O1SB 1.462(11) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Fe1 C1 87.59(13) . . ? N6 Fe1 C3 172.70(14) . . ? C1 Fe1 C3 96.77(16) . . ? N6 Fe1 C2 88.19(12) . . ? C1 Fe1 C2 94.46(14) . . ? C3 Fe1 C2 85.64(14) . . ? N6 Fe1 C4 98.83(13) . . ? C1 Fe1 C4 90.80(14) . . ? C3 Fe1 C4 86.99(15) . . ? C2 Fe1 C4 171.41(14) . . ? N6 Fe1 N5 80.73(12) . . ? C1 Fe1 N5 168.32(13) . . ? C3 Fe1 N5 94.87(15) . . ? C2 Fe1 N5 85.40(12) . . ? C4 Fe1 N5 90.82(12) . . ? N2 Ni1 N7 92.18(11) 2_655 . ? N2 Ni1 N10 170.09(11) 2_655 . ? N7 Ni1 N10 96.07(10) . . ? N2 Ni1 N9 93.73(11) 2_655 . ? N7 Ni1 N9 169.85(11) . . ? N10 Ni1 N9 78.93(11) . . ? N2 Ni1 N8 93.30(11) 2_655 . ? N7 Ni1 N8 77.35(11) . . ? N10 Ni1 N8 93.85(11) . . ? N9 Ni1 N8 94.05(10) . . ? N2 Ni1 N1 86.54(11) 2_655 . ? N7 Ni1 N1 92.88(11) . . ? N10 Ni1 N1 87.57(11) . . ? N9 Ni1 N1 95.71(11) . . ? N8 Ni1 N1 170.22(11) . . ? N1 C1 Fe1 166.9(3) . . ? N2 C2 Fe1 170.0(3) . . ? N3 C3 Fe1 175.1(4) . . ? N4 C4 Fe1 178.6(4) . . ? N5 C5 C6 121.4(3) . . ? N5 C5 C10 113.2(3) . . ? C6 C5 C10 125.3(3) . . ? C7 C6 C5 119.1(4) . . ? C7 C6 H1 120.5 . . ? C5 C6 H1 120.5 . . ? C6 C7 C8 119.2(4) . . ? C6 C7 H2 120.4 . . ? C8 C7 H2 120.4 . . ? C9 C8 C7 119.7(3) . . ? C9 C8 H3 120.2 . . ? C7 C8 H3 120.2 . . ? N5 C9 C8 122.3(4) . . ? N5 C9 H4 118.9 . . ? C8 C9 H4 118.9 . . ? C11 C10 N6 109.4(3) . . ? C11 C10 C5 137.2(3) . . ? N6 C10 C5 113.3(3) . . ? C10 C11 C12 104.1(3) . . ? C10 C11 H5 128.0 . . ? C12 C11 H5 128.0 . . ? N7 C12 C11 110.2(3) . . ? N7 C12 C13 115.9(3) . . ? C11 C12 C13 133.8(3) . . ? N8 C13 C14 122.0(3) . . ? N8 C13 C12 114.8(3) . . ? C14 C13 C12 123.1(3) . . ? C15 C14 C13 118.7(3) . . ? C15 C14 H6 120.7 . . ? C13 C14 H6 120.7 . . ? C16 C15 C14 119.0(3) . . ? C16 C15 H7 120.5 . . ? C14 C15 H7 120.5 . . ? C15 C16 C17 118.7(3) . . ? C15 C16 H8 120.6 . . ? C17 C16 H8 120.6 . . ? N8 C17 C16 123.5(3) . . ? N8 C17 H9 118.2 . . ? C16 C17 H9 118.2 . . ? N9 C18 C19 122.1(3) . . ? N9 C18 C23 114.5(3) . . ? C19 C18 C23 123.3(3) . . ? C20 C19 C18 118.9(4) . . ? C20 C19 H10 120.5 . . ? C18 C19 H10 120.5 . . ? C21 C20 C19 118.9(3) . . ? C21 C20 H11 120.6 . . ? C19 C20 H11 120.6 . . ? C20 C21 C22 119.6(4) . . ? C20 C21 H12 120.2 . . ? C22 C21 H12 120.2 . . ? N9 C22 C21 122.1(4) . . ? N9 C22 H13 119.0 . . ? C21 C22 H13 119.0 . . ? N10 C23 C18 119.1(3) . . ? N10 C23 H14 120.5 . . ? C18 C23 H14 120.5 . . ? N10 C24 C26 109.0(3) . . ? N10 C24 C25 115.1(3) . . ? C26 C24 C25 111.5(3) . . ? N10 C24 H15 107.0 . . ? C26 C24 H15 107.0 . . ? C25 C24 H15 107.0 . . ? C24 C25 H16 109.5 . . ? C24 C25 H17 109.5 . . ? H16 C25 H17 109.5 . . ? C24 C25 H18 109.5 . . ? H16 C25 H18 109.5 . . ? H17 C25 H18 109.5 . . ? C31 C26 C27 119.0(3) . . ? C31 C26 C24 120.3(3) . . ? C27 C26 C24 120.7(3) . . ? C28 C27 C26 120.0(4) . . ? C28 C27 H19 120.0 . . ? C26 C27 H19 120.0 . . ? C29 C28 C27 120.6(4) . . ? C29 C28 H20 119.7 . . ? C27 C28 H20 119.7 . . ? C30 C29 C28 120.2(4) . . ? C30 C29 H21 119.9 . . ? C28 C29 H21 119.9 . . ? C29 C30 C31 120.1(4) . . ? C29 C30 H22 119.9 . . ? C31 C30 H22 119.9 . . ? C26 C31 C30 120.2(4) . . ? C26 C31 H23 119.9 . . ? C30 C31 H23 119.9 . . ? C1 N1 Ni1 105.0(3) . . ? C2 N2 Ni1 170.0(3) . 2_655 ? C9 N5 C5 118.3(3) . . ? C9 N5 Fe1 127.7(3) . . ? C5 N5 Fe1 114.0(2) . . ? N7 N6 C10 108.5(3) . . ? N7 N6 Fe1 132.1(2) . . ? C10 N6 Fe1 118.0(2) . . ? N6 N7 C12 107.8(3) . . ? N6 N7 Ni1 134.8(2) . . ? C12 N7 Ni1 117.3(2) . . ? C17 N8 C13 118.0(3) . . ? C17 N8 Ni1 127.8(2) . . ? C13 N8 Ni1 114.2(2) . . ? C22 N9 C18 118.4(3) . . ? C22 N9 Ni1 128.1(2) . . ? C18 N9 Ni1 113.3(2) . . ? C23 N10 C24 121.6(3) . . ? C23 N10 Ni1 113.9(2) . . ? C24 N10 Ni1 124.4(2) . . ? O1SB C1SB O1SB 90.2(10) 2_655 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.386 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.080 data_Comp3 _database_code_depnum_ccdc_archive 'CCDC 883727' #TrackingRef '- TetraCN.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H44 Fe2 N20 Ni2, C2 O3, 5(O)' _chemical_formula_sum 'C64 H44 Fe2 N20 Ni2 O8' _chemical_formula_weight 1450.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 13.319(2) _cell_length_b 20.390(3) _cell_length_c 11.9344(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3241.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 979 _cell_measurement_theta_min 2.500 _cell_measurement_theta_max 27.09 _exptl_crystal_description plates _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 1.082 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8545 _exptl_absorpt_correction_T_max 0.8995 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20217 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7363 _reflns_number_gt 6105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Methanol molecules in the lattice were treated by DFIX restraints. ; _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^)+(0.0454P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(15) _chemical_absolute_configuration rmad _refine_ls_number_reflns 7363 _refine_ls_number_parameters 444 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.1003 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.66302(4) 0.38449(3) 0.32950(5) 0.01808(14) Uani 1 1 d . . . Ni1 Ni 0.36308(3) 0.36915(2) 0.28738(4) 0.01617(12) Uani 1 1 d . . . C1 C 0.5438(3) 0.3672(2) 0.4126(3) 0.0177(8) Uani 1 1 d . . . C2 C 0.6501(3) 0.47920(19) 0.3407(3) 0.0181(8) Uani 1 1 d . . . C3 C 0.7531(3) 0.3917(2) 0.4557(4) 0.0281(10) Uani 1 1 d . . . C4 C 0.6960(3) 0.2910(2) 0.3267(4) 0.0202(9) Uani 1 1 d . . . C5 C 0.7342(3) 0.41495(19) 0.1091(4) 0.0211(9) Uani 1 1 d . . . C6 C 0.7965(3) 0.4319(2) 0.0207(4) 0.0243(10) Uani 1 1 d . . . H1 H 0.7701 0.4387 -0.0524 0.029 Uiso 1 1 calc R . . C7 C 0.8976(3) 0.4387(2) 0.0413(4) 0.0308(11) Uani 1 1 d . . . H2 H 0.9415 0.4518 -0.0173 0.037 Uiso 1 1 calc R . . C8 C 0.9349(3) 0.4267(2) 0.1462(4) 0.0291(11) Uani 1 1 d . . . C9 C 0.8686(3) 0.40914(19) 0.2300(4) 0.0255(9) Uani 1 1 d . . . H3 H 0.8946 0.4008 0.3027 0.031 Uiso 1 1 calc R . . C10 C 0.6259(3) 0.40876(18) 0.1023(3) 0.0176(8) Uani 1 1 d . . . C11 C 0.5516(3) 0.41975(19) 0.0243(3) 0.0189(9) Uani 1 1 d . . . H4 H 0.5593 0.4339 -0.0511 0.023 Uiso 1 1 calc R . . C12 C 0.4628(3) 0.40558(18) 0.0805(3) 0.0183(9) Uani 1 1 d . . . C13 C 0.3591(3) 0.40282(18) 0.0460(3) 0.0181(8) Uani 1 1 d . . . C14 C 0.3259(3) 0.41495(19) -0.0631(3) 0.0222(9) Uani 1 1 d . . . H5 H 0.3721 0.4285 -0.1191 0.027 Uiso 1 1 calc R . . C15 C 0.2256(3) 0.4071(2) -0.0888(4) 0.0254(10) Uani 1 1 d . . . H6 H 0.2017 0.4151 -0.1626 0.030 Uiso 1 1 calc R . . C16 C 0.1602(3) 0.3874(2) -0.0046(3) 0.0242(9) Uani 1 1 d . . . H7 H 0.0910 0.3808 -0.0201 0.029 Uiso 1 1 calc R . . C17 C 0.1976(3) 0.3776(2) 0.1022(3) 0.0204(9) Uani 1 1 d . . . H8 H 0.1521 0.3648 0.1594 0.024 Uiso 1 1 calc R . . C18 C 0.2101(3) 0.2788(2) 0.3621(3) 0.0208(9) Uani 1 1 d . . . C19 C 0.1207(3) 0.2523(2) 0.4002(3) 0.0289(10) Uani 1 1 d . . . H9 H 0.1087 0.2065 0.3963 0.035 Uiso 1 1 calc R . . C20 C 0.0492(3) 0.2944(3) 0.4441(4) 0.0314(11) Uani 1 1 d . . . H10 H -0.0131 0.2776 0.4704 0.038 Uiso 1 1 calc R . . C21 C 0.0684(3) 0.3603(2) 0.4494(4) 0.0309(11) Uani 1 1 d . . . H11 H 0.0201 0.3898 0.4792 0.037 Uiso 1 1 calc R . . C22 C 0.1602(3) 0.3831(2) 0.4103(3) 0.0247(9) Uani 1 1 d . . . H12 H 0.1739 0.4287 0.4153 0.030 Uiso 1 1 calc R . . C23 C 0.2902(3) 0.23942(19) 0.3119(3) 0.0205(9) Uani 1 1 d . . . H13 H 0.2859 0.1929 0.3113 0.025 Uiso 1 1 calc R . . C24 C 0.4480(3) 0.23098(19) 0.2170(4) 0.0219(9) Uani 1 1 d . . . H14 H 0.5122 0.2508 0.2441 0.026 Uiso 1 1 calc R . . C25 C 0.4517(3) 0.1582(2) 0.2460(4) 0.0275(10) Uani 1 1 d . . . H15 H 0.4559 0.1530 0.3275 0.041 Uiso 1 1 calc R . . H16 H 0.5108 0.1383 0.2108 0.041 Uiso 1 1 calc R . . H17 H 0.3908 0.1367 0.2182 0.041 Uiso 1 1 calc R . . C26 C 0.4441(3) 0.24123(19) 0.0897(3) 0.0208(9) Uani 1 1 d . . . C27 C 0.5307(3) 0.2556(2) 0.0302(4) 0.0281(10) Uani 1 1 d . . . H18 H 0.5926 0.2605 0.0689 0.034 Uiso 1 1 calc R . . C28 C 0.5278(3) 0.2628(2) -0.0846(4) 0.0307(11) Uani 1 1 d . . . H19 H 0.5879 0.2714 -0.1248 0.037 Uiso 1 1 calc R . . C29 C 0.4375(3) 0.2576(2) -0.1415(4) 0.0299(11) Uani 1 1 d . . . H20 H 0.4351 0.2640 -0.2203 0.036 Uiso 1 1 calc R . . C30 C 0.3516(4) 0.2430(2) -0.0834(4) 0.0296(10) Uani 1 1 d . . . H21 H 0.2899 0.2383 -0.1225 0.036 Uiso 1 1 calc R . . C31 C 0.3539(3) 0.23492(19) 0.0325(3) 0.0254(9) Uani 1 1 d . . . H22 H 0.2939 0.2251 0.0722 0.030 Uiso 1 1 calc R . . N1 N 0.4626(2) 0.35611(16) 0.4437(3) 0.0220(8) Uani 1 1 d . . . N2 N 0.6471(2) 0.53560(16) 0.3315(3) 0.0191(7) Uani 1 1 d . . . N3 N 0.8108(3) 0.3985(2) 0.5268(4) 0.0464(12) Uani 1 1 d . . . N4 N 0.7162(3) 0.23638(17) 0.3263(3) 0.0285(8) Uani 1 1 d . . . N5 N 0.7702(2) 0.40333(14) 0.2137(3) 0.0185(7) Uani 1 1 d . . . N6 N 0.5821(2) 0.38868(15) 0.1997(3) 0.0173(7) Uani 1 1 d . . . N7 N 0.4825(2) 0.38753(15) 0.1856(3) 0.0164(7) Uani 1 1 d . . . N8 N 0.2940(2) 0.38509(16) 0.1293(3) 0.0192(7) Uani 1 1 d . . . N9 N 0.2299(2) 0.34385(17) 0.3662(3) 0.0213(8) Uani 1 1 d . . . N10 N 0.3653(2) 0.26817(15) 0.2693(2) 0.0178(7) Uani 1 1 d . . . C1SA C 0.0890(9) 0.0769(8) 0.2972(14) 0.087(5) Uani 0.50 1 d PDU A 1 C1SB C 0.0000 0.0000 0.3725(14) 0.193(9) Uani 1 2 d SDU . 2 O1SA O 0.1769(4) 0.0880(3) 0.2263(4) 0.0992(17) Uani 1 1 d DU . . O1SB O -0.0250(9) 0.0482(7) 0.2871(9) 0.123(4) Uani 0.50 1 d PDU B 2 O2S O 0.8131(2) 0.11305(16) 0.3705(2) 0.0378(8) Uani 1 1 d . . . O3S O 0.6806(3) 0.0082(2) 0.3315(4) 0.0808(15) Uani 1 1 d . . . O4S O 0.5000 0.0000 0.1963(4) 0.0367(12) Uani 1 2 d S C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0144(3) 0.0165(3) 0.0233(3) 0.0035(2) -0.0022(2) 0.0005(2) Ni1 0.0137(2) 0.0163(2) 0.0185(2) 0.0006(2) 0.0007(2) -0.00028(19) C1 0.023(2) 0.0133(19) 0.0173(19) 0.0023(18) -0.0043(17) 0.0038(18) C2 0.011(2) 0.026(2) 0.0179(19) 0.0002(17) 0.0002(17) -0.0029(16) C3 0.034(3) 0.016(2) 0.034(2) 0.003(2) -0.009(2) 0.0001(19) C4 0.017(2) 0.022(2) 0.021(2) 0.0011(19) 0.0032(17) -0.0023(16) C5 0.018(2) 0.0121(19) 0.033(3) 0.0037(18) -0.0009(19) 0.0046(16) C6 0.022(2) 0.021(2) 0.030(2) 0.001(2) 0.0092(19) -0.0010(18) C7 0.028(3) 0.021(2) 0.044(3) 0.006(2) 0.011(2) 0.0028(19) C8 0.018(2) 0.022(2) 0.047(3) 0.003(2) 0.003(2) 0.0000(17) C9 0.019(2) 0.019(2) 0.039(3) 0.0021(19) -0.002(2) -0.0013(17) C10 0.018(2) 0.0123(18) 0.022(2) -0.0001(16) 0.0014(18) -0.0024(16) C11 0.024(2) 0.013(2) 0.020(2) 0.0058(17) 0.0015(18) -0.0002(17) C12 0.025(2) 0.0103(19) 0.019(2) 0.0016(17) -0.0014(18) 0.0018(17) C13 0.019(2) 0.0134(18) 0.022(2) -0.0027(16) 0.0004(18) 0.0003(17) C14 0.024(2) 0.020(2) 0.023(2) 0.0031(17) 0.0023(18) 0.0009(18) C15 0.029(2) 0.026(2) 0.022(2) 0.0007(19) -0.007(2) 0.0039(19) C16 0.016(2) 0.024(2) 0.032(2) -0.0058(19) -0.0041(18) 0.0029(18) C17 0.0158(19) 0.021(2) 0.024(2) -0.0032(19) 0.0029(16) -0.0004(17) C18 0.020(2) 0.026(2) 0.016(2) 0.0043(17) -0.0025(16) -0.0035(17) C19 0.026(2) 0.035(3) 0.026(2) 0.006(2) -0.001(2) -0.005(2) C20 0.018(2) 0.053(3) 0.023(2) 0.009(2) 0.0008(19) -0.006(2) C21 0.021(2) 0.046(3) 0.026(2) 0.004(2) 0.0064(19) 0.012(2) C22 0.020(2) 0.031(2) 0.022(2) 0.0040(19) -0.0011(17) 0.003(2) C23 0.021(2) 0.018(2) 0.023(2) 0.0046(18) -0.0030(17) -0.0039(16) C24 0.019(2) 0.021(2) 0.026(2) 0.001(2) -0.0013(19) -0.0022(16) C25 0.036(3) 0.020(2) 0.026(2) 0.0013(18) 0.007(2) 0.0062(19) C26 0.032(2) 0.010(2) 0.020(2) -0.0008(17) 0.0026(19) 0.0030(17) C27 0.029(3) 0.022(2) 0.034(3) -0.004(2) 0.002(2) 0.0003(19) C28 0.035(3) 0.027(2) 0.030(3) 0.003(2) 0.012(2) 0.005(2) C29 0.042(3) 0.025(2) 0.022(2) -0.0018(19) 0.003(2) 0.009(2) C30 0.035(3) 0.024(2) 0.030(2) -0.0052(19) -0.007(2) 0.005(2) C31 0.024(2) 0.020(2) 0.032(2) 0.0016(18) 0.000(2) -0.0008(19) N1 0.0192(19) 0.0200(19) 0.0268(19) 0.0035(16) -0.0032(15) 0.0019(15) N2 0.0148(17) 0.0218(18) 0.0207(16) -0.0001(15) -0.0022(15) 0.0007(14) N3 0.055(3) 0.030(2) 0.055(3) 0.004(2) -0.030(2) -0.002(2) N4 0.030(2) 0.024(2) 0.032(2) 0.0027(18) 0.0058(18) 0.0002(16) N5 0.0133(16) 0.0136(16) 0.0285(18) 0.0015(16) -0.0002(16) 0.0029(12) N6 0.0154(16) 0.0180(17) 0.0185(17) 0.0003(15) -0.0024(13) -0.0021(13) N7 0.0139(15) 0.0129(16) 0.0225(18) -0.0002(15) -0.0035(13) 0.0009(13) N8 0.0177(17) 0.0160(17) 0.0239(17) -0.0011(15) 0.0039(14) 0.0034(14) N9 0.0174(18) 0.030(2) 0.0164(17) 0.0033(15) -0.0006(14) 0.0011(15) N10 0.0186(17) 0.0194(16) 0.0154(16) 0.0002(13) -0.0004(15) 0.0016(14) C1SA 0.041(7) 0.096(11) 0.123(13) -0.005(11) -0.014(7) -0.013(7) C1SB 0.28(2) 0.181(18) 0.116(13) 0.000 0.000 0.135(17) O1SA 0.107(4) 0.133(5) 0.058(3) 0.002(3) -0.008(3) -0.003(3) O1SB 0.121(10) 0.165(12) 0.081(8) 0.010(7) -0.002(7) 0.059(8) O2S 0.047(2) 0.0346(19) 0.0315(17) 0.0034(15) 0.0016(15) 0.0097(16) O3S 0.079(3) 0.088(3) 0.075(3) 0.050(3) -0.032(3) -0.033(3) O4S 0.053(3) 0.022(2) 0.035(3) 0.000 0.000 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N6 1.889(3) . ? Fe1 C1 1.905(4) . ? Fe1 C3 1.931(4) . ? Fe1 C2 1.943(4) . ? Fe1 C4 1.956(4) . ? Fe1 N5 2.023(3) . ? Ni1 N2 2.017(3) 2_665 ? Ni1 N7 2.036(3) . ? Ni1 N10 2.070(3) . ? Ni1 N9 2.073(3) . ? Ni1 N8 2.125(3) . ? Ni1 N1 2.304(3) . ? C1 N1 1.165(5) . ? C2 N2 1.156(5) . ? C3 N3 1.153(5) . ? C4 N4 1.146(5) . ? C5 N5 1.358(5) . ? C5 C6 1.387(6) . ? C5 C10 1.450(6) . ? C6 C7 1.375(6) . ? C6 H1 0.9500 . ? C7 C8 1.369(7) . ? C7 H2 0.9500 . ? C8 C9 1.381(6) . ? C9 N5 1.331(5) . ? C9 H3 0.9500 . ? C10 N6 1.364(5) . ? C10 C11 1.377(5) . ? C11 C12 1.390(5) . ? C11 H4 0.9500 . ? C12 N7 1.334(5) . ? C12 C13 1.443(6) . ? C13 N8 1.367(5) . ? C13 C14 1.397(5) . ? C14 C15 1.380(6) . ? C14 H5 0.9500 . ? C15 C16 1.389(6) . ? C15 H6 0.9500 . ? C16 C17 1.383(5) . ? C16 H7 0.9500 . ? C17 N8 1.332(5) . ? C17 H8 0.9500 . ? C18 N9 1.354(5) . ? C18 C19 1.384(5) . ? C18 C23 1.463(6) . ? C19 C20 1.385(6) . ? C19 H9 0.9500 . ? C20 C21 1.369(7) . ? C20 H10 0.9500 . ? C21 C22 1.388(6) . ? C21 H11 0.9500 . ? C22 N9 1.335(5) . ? C22 H12 0.9500 . ? C23 N10 1.266(5) . ? C23 H13 0.9500 . ? C24 N10 1.476(5) . ? C24 C25 1.524(5) . ? C24 C26 1.535(6) . ? C24 H14 1.0000 . ? C25 H15 0.9800 . ? C25 H16 0.9800 . ? C25 H17 0.9800 . ? C26 C27 1.386(6) . ? C26 C31 1.389(6) . ? C27 C28 1.379(6) . ? C27 H18 0.9500 . ? C28 C29 1.385(6) . ? C28 H19 0.9500 . ? C29 C30 1.370(6) . ? C29 H20 0.9500 . ? C30 C31 1.393(6) . ? C30 H21 0.9500 . ? C31 H22 0.9500 . ? N2 Ni1 2.017(3) 2_665 ? N6 N7 1.337(4) . ? C1SA O1SA 1.463(12) . ? C1SB O1SB 1.454(12) 2 ? C1SB O1SB 1.454(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Fe1 C1 87.71(15) . . ? N6 Fe1 C3 172.10(16) . . ? C1 Fe1 C3 97.22(17) . . ? N6 Fe1 C2 87.78(14) . . ? C1 Fe1 C2 94.29(17) . . ? C3 Fe1 C2 85.71(17) . . ? N6 Fe1 C4 99.10(15) . . ? C1 Fe1 C4 90.86(16) . . ? C3 Fe1 C4 87.03(17) . . ? C2 Fe1 C4 171.57(16) . . ? N6 Fe1 N5 80.44(13) . . ? C1 Fe1 N5 168.15(15) . . ? C3 Fe1 N5 94.57(16) . . ? C2 Fe1 N5 85.45(14) . . ? C4 Fe1 N5 90.87(14) . . ? N2 Ni1 N7 91.79(12) 2_665 . ? N2 Ni1 N10 170.33(13) 2_665 . ? N7 Ni1 N10 96.29(12) . . ? N2 Ni1 N9 93.64(13) 2_665 . ? N7 Ni1 N9 170.05(13) . . ? N10 Ni1 N9 79.17(13) . . ? N2 Ni1 N8 93.17(13) 2_665 . ? N7 Ni1 N8 77.33(12) . . ? N10 Ni1 N8 93.78(12) . . ? N9 Ni1 N8 94.03(12) . . ? N2 Ni1 N1 86.49(12) 2_665 . ? N7 Ni1 N1 93.12(12) . . ? N10 Ni1 N1 87.77(12) . . ? N9 Ni1 N1 95.53(12) . . ? N8 Ni1 N1 170.44(12) . . ? N1 C1 Fe1 167.1(3) . . ? N2 C2 Fe1 170.1(4) . . ? N3 C3 Fe1 175.6(4) . . ? N4 C4 Fe1 179.1(4) . . ? N5 C5 C6 122.1(4) . . ? N5 C5 C10 112.8(4) . . ? C6 C5 C10 125.0(4) . . ? C7 C6 C5 118.3(4) . . ? C7 C6 H1 120.8 . . ? C5 C6 H1 120.8 . . ? C8 C7 C6 120.1(4) . . ? C8 C7 H2 120.0 . . ? C6 C7 H2 120.0 . . ? C7 C8 C9 118.4(4) . . ? N5 C9 C8 123.2(4) . . ? N5 C9 H3 118.4 . . ? C8 C9 H3 118.4 . . ? N6 C10 C11 108.5(3) . . ? N6 C10 C5 113.8(3) . . ? C11 C10 C5 137.6(4) . . ? C10 C11 C12 104.6(3) . . ? C10 C11 H4 127.7 . . ? C12 C11 H4 127.7 . . ? N7 C12 C11 110.1(3) . . ? N7 C12 C13 116.5(3) . . ? C11 C12 C13 133.3(4) . . ? N8 C13 C14 121.6(4) . . ? N8 C13 C12 114.3(3) . . ? C14 C13 C12 124.1(4) . . ? C15 C14 C13 119.5(4) . . ? C15 C14 H5 120.2 . . ? C13 C14 H5 120.2 . . ? C14 C15 C16 118.6(4) . . ? C14 C15 H6 120.7 . . ? C16 C15 H6 120.7 . . ? C17 C16 C15 118.9(4) . . ? C17 C16 H7 120.6 . . ? C15 C16 H7 120.6 . . ? N8 C17 C16 123.6(4) . . ? N8 C17 H8 118.2 . . ? C16 C17 H8 118.2 . . ? N9 C18 C19 122.5(4) . . ? N9 C18 C23 114.2(3) . . ? C19 C18 C23 123.2(4) . . ? C18 C19 C20 118.3(4) . . ? C18 C19 H9 120.8 . . ? C20 C19 H9 120.8 . . ? C21 C20 C19 119.8(4) . . ? C21 C20 H10 120.1 . . ? C19 C20 H10 120.1 . . ? C20 C21 C22 118.6(4) . . ? C20 C21 H11 120.7 . . ? C22 C21 H11 120.7 . . ? N9 C22 C21 123.0(4) . . ? N9 C22 H12 118.5 . . ? C21 C22 H12 118.5 . . ? N10 C23 C18 119.1(4) . . ? N10 C23 H13 120.4 . . ? C18 C23 H13 120.4 . . ? N10 C24 C25 115.4(3) . . ? N10 C24 C26 108.9(3) . . ? C25 C24 C26 111.0(3) . . ? N10 C24 H14 107.1 . . ? C25 C24 H14 107.1 . . ? C26 C24 H14 107.1 . . ? C24 C25 H15 109.5 . . ? C24 C25 H16 109.5 . . ? H15 C25 H16 109.5 . . ? C24 C25 H17 109.5 . . ? H15 C25 H17 109.5 . . ? H16 C25 H17 109.5 . . ? C27 C26 C31 119.2(4) . . ? C27 C26 C24 120.5(4) . . ? C31 C26 C24 120.2(4) . . ? C28 C27 C26 120.5(4) . . ? C28 C27 H18 119.7 . . ? C26 C27 H18 119.7 . . ? C27 C28 C29 120.3(4) . . ? C27 C28 H19 119.9 . . ? C29 C28 H19 119.9 . . ? C30 C29 C28 119.5(4) . . ? C30 C29 H20 120.2 . . ? C28 C29 H20 120.2 . . ? C29 C30 C31 120.7(4) . . ? C29 C30 H21 119.7 . . ? C31 C30 H21 119.7 . . ? C26 C31 C30 119.7(4) . . ? C26 C31 H22 120.1 . . ? C30 C31 H22 120.1 . . ? C1 N1 Ni1 104.8(3) . . ? C2 N2 Ni1 170.2(3) . 2_665 ? C9 N5 C5 117.8(4) . . ? C9 N5 Fe1 127.8(3) . . ? C5 N5 Fe1 114.3(2) . . ? N7 N6 C10 108.8(3) . . ? N7 N6 Fe1 131.9(3) . . ? C10 N6 Fe1 117.9(2) . . ? C12 N7 N6 108.0(3) . . ? C12 N7 Ni1 117.3(2) . . ? N6 N7 Ni1 134.7(3) . . ? C17 N8 C13 117.7(3) . . ? C17 N8 Ni1 128.0(3) . . ? C13 N8 Ni1 114.3(2) . . ? C22 N9 C18 117.8(4) . . ? C22 N9 Ni1 128.7(3) . . ? C18 N9 Ni1 113.2(3) . . ? C23 N10 C24 121.4(3) . . ? C23 N10 Ni1 114.0(3) . . ? C24 N10 Ni1 124.5(2) . . ? O1SB C1SB O1SB 91.0(14) 2 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.826 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.097