# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Patrick Gamez' _publ_contact_author_address ; Leiden Institute of Chemidtry Leiden University PO BOX 9502 Leiden 2300 RA NETHERLANDS ; _publ_contact_author_email P.GAMEZ@CHEM.LEIDENUNIV.NL _publ_section_title ; Spin transition in a triazine-based Fe(II) complex: variable-temperature structural, thermal, magnetic and spectroscopic studies ; loop_ _publ_author_name 'Patrick Gamez' 'Guillem Aromi' "V.A.de la Pena-O'Shea" 'Marti Gich' 'Elizabeth J. MacLean' ; E.Molins ; 'Maria Monrabal' 'Manuel Quesada' 'J. Reedijk' 'Olivier Roubeau' 'S. J. Teat' # Attachment 'Revised_B602903E_200K.cif' data_eu_22_01c _database_code_depnum_ccdc_archive 'CCDC 298835' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H52 Fe N26 O2 S2' _chemical_formula_weight 1385.33 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7151(7) _cell_length_b 12.8256(8) _cell_length_c 13.0725(8) _cell_angle_alpha 95.3500(10) _cell_angle_beta 111.7160(10) _cell_angle_gamma 116.3790(10) _cell_volume 1554.48(16) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5736 _cell_measurement_theta_min 3.118 _cell_measurement_theta_max 29.582 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.382 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9753 _exptl_absorpt_correction_T_max 0.9843 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.69230 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 17729 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 29.59 _reflns_number_total 9158 _reflns_number_gt 7343 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _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 and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.1384P] 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 9158 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1268 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 N1 N 0.27798(13) 0.08396(11) 0.27529(11) 0.0204(2) Uani 1 1 d . . . C1 C 0.24048(15) 0.16462(12) 0.24381(12) 0.0176(3) Uani 1 1 d . . . N2 N 0.10681(13) 0.14382(11) 0.18981(11) 0.0202(2) Uani 1 1 d . . . C2 C 0.00489(15) 0.02695(13) 0.16322(12) 0.0196(3) Uani 1 1 d . . . N3 N 0.02663(13) -0.06589(11) 0.18168(11) 0.0214(2) Uani 1 1 d . . . C3 C 0.16582(15) -0.02998(13) 0.24079(13) 0.0197(3) Uani 1 1 d . . . N4 N 0.35183(12) 0.28400(10) 0.27546(11) 0.0190(2) Uani 1 1 d . . . C4 C 0.32429(15) 0.37723(13) 0.24466(13) 0.0204(3) Uani 1 1 d . . . C5 C 0.24469(17) 0.36272(15) 0.12911(14) 0.0256(3) Uani 1 1 d . . . H5 H 0.2057 0.2900 0.0699 0.031 Uiso 1 1 calc R . . C6 C 0.22349(19) 0.45731(17) 0.10230(16) 0.0312(4) Uani 1 1 d . . . H6 H 0.1664 0.4488 0.0246 0.037 Uiso 1 1 calc R . . C7 C 0.2868(2) 0.56421(16) 0.19051(17) 0.0330(4) Uani 1 1 d . . . H7 H 0.2752 0.6305 0.1741 0.040 Uiso 1 1 calc R . . N5 N 0.38368(14) 0.47916(11) 0.33152(12) 0.0224(3) Uani 1 1 d . . . C8 C 0.36672(19) 0.57223(15) 0.30231(16) 0.0287(3) Uani 1 1 d . . . H8 H 0.4123 0.6465 0.3620 0.034 Uiso 1 1 calc R . . C9 C 0.49844(15) 0.31685(13) 0.33932(13) 0.0204(3) Uani 1 1 d . . . C10 C 0.55113(17) 0.25562(15) 0.29562(15) 0.0271(3) Uani 1 1 d . . . H10 H 0.4909 0.1917 0.2239 0.032 Uiso 1 1 calc R . . C11 C 0.69403(18) 0.29026(17) 0.35941(17) 0.0328(4) Uani 1 1 d . . . H11 H 0.7323 0.2478 0.3339 0.039 Uiso 1 1 calc R . . C12 C 0.78005(17) 0.38807(17) 0.46111(16) 0.0328(4) Uani 1 1 d . . . H12 H 0.8783 0.4141 0.5057 0.039 Uiso 1 1 calc R . . C13 C 0.72070(16) 0.44704(15) 0.49651(15) 0.0287(3) Uani 1 1 d . . . H13A H 0.7812 0.5160 0.5643 0.034 Uiso 1 1 calc R . . N6 N 0.57938(13) 0.41066(11) 0.43846(11) 0.0223(3) Uani 1 1 d . . . N7 N -0.13681(13) -0.00354(11) 0.11200(12) 0.0225(3) Uani 1 1 d . . . C14 C -0.18207(15) 0.08024(13) 0.07954(13) 0.0211(3) Uani 1 1 d . . . C15 C -0.11881(16) 0.16522(15) 0.02953(13) 0.0247(3) Uani 1 1 d . . . H15 H -0.0442 0.1688 0.0141 0.030 Uiso 1 1 calc R . . C16 C -0.16798(18) 0.24442(16) 0.00295(15) 0.0301(3) Uani 1 1 d . . . H16 H -0.1255 0.3051 -0.0292 0.036 Uiso 1 1 calc R . . C17 C -0.28008(19) 0.23427(16) 0.02376(16) 0.0307(3) Uani 1 1 d . . . H17 H -0.3144 0.2884 0.0076 0.037 Uiso 1 1 calc R . . C18 C -0.33995(18) 0.14318(16) 0.06861(16) 0.0305(3) Uani 1 1 d . . . H18 H -0.4194 0.1337 0.0795 0.037 Uiso 1 1 calc R . . N8 N -0.29204(14) 0.06678(12) 0.09784(13) 0.0279(3) Uani 1 1 d . . . C19 C -0.24592(15) -0.12233(13) 0.10250(14) 0.0227(3) Uani 1 1 d . . . C20 C -0.24584(18) -0.15316(16) 0.20168(16) 0.0315(4) Uani 1 1 d . . . H20 H -0.1748 -0.0972 0.2766 0.038 Uiso 1 1 calc R . . C21 C -0.3531(2) -0.26840(18) 0.18742(19) 0.0381(4) Uani 1 1 d . . . H21 H -0.3574 -0.2932 0.2528 0.046 Uiso 1 1 calc R . . C22 C -0.45332(19) -0.34642(16) 0.07674(19) 0.0377(4) Uani 1 1 d . . . H22 H -0.5265 -0.4266 0.0646 0.045 Uiso 1 1 calc R . . C23 C -0.44552(19) -0.30610(15) -0.01591(18) 0.0352(4) Uani 1 1 d . . . H23 H -0.5163 -0.3600 -0.0917 0.042 Uiso 1 1 calc R . . N9 N -0.34307(14) -0.19441(12) -0.00493(13) 0.0288(3) Uani 1 1 d . . . N10 N 0.19602(13) -0.11915(11) 0.26831(12) 0.0228(3) Uani 1 1 d . C . C24 C 0.33770(16) -0.10002(13) 0.30738(13) 0.0218(3) Uani 1 1 d . . . C26 C 0.5483(2) -0.03626(18) 0.2881(2) 0.0420(5) Uani 1 1 d . . . H26 H 0.6036 -0.0029 0.2491 0.050 Uiso 1 1 calc R A 1 C27 C 0.6031(2) -0.06943(18) 0.3830(2) 0.0444(5) Uani 1 1 d . C . H27 H 0.6962 -0.0583 0.4108 0.053 Uiso 1 1 calc R . . C28 C 0.5199(2) -0.11910(17) 0.43711(17) 0.0403(5) Uani 1 1 d . . . H28 H 0.5574 -0.1421 0.5029 0.048 Uiso 1 1 calc R B 1 C25A C 0.41316(18) -0.05093(14) 0.24845(15) 0.0312(3) Uani 0.50 1 d P C 1 H25A H 0.3745 -0.0279 0.1831 0.037 Uiso 0.50 1 calc PR C 1 N12A N 0.38513(18) -0.13653(13) 0.39935(13) 0.0287(3) Uani 0.50 1 d P C 1 N12B N 0.41316(18) -0.05093(14) 0.24845(15) 0.0312(3) Uani 0.50 1 d P C 2 C25B C 0.38513(18) -0.13653(13) 0.39935(13) 0.0287(3) Uani 0.50 1 d P C 2 H25B H 0.3278 -0.1726 0.4362 0.034 Uiso 0.50 1 calc PR C 2 C29 C 0.08852(16) -0.23318(13) 0.26585(14) 0.0228(3) Uani 1 1 d . . . C30 C 0.0103(2) -0.23613(17) 0.32499(17) 0.0335(4) Uani 1 1 d . C . H30 H 0.0242 -0.1628 0.3659 0.040 Uiso 1 1 calc R . . C31 C -0.0884(2) -0.34942(19) 0.32226(19) 0.0410(4) Uani 1 1 d . . . H31 H -0.1451 -0.3554 0.3604 0.049 Uiso 1 1 calc R C . C32 C -0.1036(2) -0.45416(17) 0.26320(18) 0.0389(4) Uani 1 1 d . C . H32 H -0.1710 -0.5329 0.2597 0.047 Uiso 1 1 calc R . . C33 C -0.0187(2) -0.44121(15) 0.20980(16) 0.0347(4) Uani 1 1 d . . . H33 H -0.0275 -0.5130 0.1713 0.042 Uiso 1 1 calc R C . N11 N 0.07617(16) -0.33231(12) 0.20904(12) 0.0281(3) Uani 1 1 d . C . Fe1 Fe 0.5000 0.5000 0.5000 0.01742(8) Uani 1 2 d S . . N13 N 0.34244(15) 0.34423(12) 0.49052(12) 0.0248(3) Uani 1 1 d . . . C34 C 0.24199(17) 0.25613(14) 0.48147(13) 0.0232(3) Uani 1 1 d . . . S1 S 0.10005(5) 0.13201(4) 0.46791(4) 0.03393(11) Uani 1 1 d . . . O1W O -0.0194(3) 0.3006(2) 0.3253(3) 0.1192(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0176(5) 0.0145(5) 0.0263(6) 0.0056(5) 0.0074(5) 0.0084(5) C1 0.0164(6) 0.0144(6) 0.0193(6) 0.0038(5) 0.0069(5) 0.0071(5) N2 0.0161(5) 0.0152(5) 0.0252(6) 0.0053(5) 0.0063(5) 0.0076(5) C2 0.0162(6) 0.0171(6) 0.0223(7) 0.0035(5) 0.0074(5) 0.0079(5) N3 0.0177(5) 0.0148(5) 0.0290(6) 0.0055(5) 0.0088(5) 0.0081(5) C3 0.0198(6) 0.0161(6) 0.0244(7) 0.0064(5) 0.0103(5) 0.0102(5) N4 0.0142(5) 0.0139(5) 0.0243(6) 0.0056(4) 0.0051(4) 0.0069(4) C4 0.0160(6) 0.0162(6) 0.0291(7) 0.0098(5) 0.0100(5) 0.0082(5) C5 0.0213(7) 0.0241(7) 0.0301(8) 0.0114(6) 0.0107(6) 0.0111(6) C6 0.0288(8) 0.0361(9) 0.0357(9) 0.0211(7) 0.0145(7) 0.0205(7) C7 0.0380(9) 0.0317(8) 0.0491(10) 0.0259(8) 0.0260(8) 0.0258(8) N5 0.0216(6) 0.0161(5) 0.0324(7) 0.0102(5) 0.0135(5) 0.0106(5) C8 0.0347(8) 0.0231(7) 0.0402(9) 0.0166(7) 0.0217(7) 0.0193(7) C9 0.0150(6) 0.0173(6) 0.0264(7) 0.0094(5) 0.0075(5) 0.0075(5) C10 0.0223(7) 0.0228(7) 0.0361(9) 0.0081(6) 0.0132(6) 0.0121(6) C11 0.0251(8) 0.0341(9) 0.0484(10) 0.0161(8) 0.0198(7) 0.0195(7) C12 0.0175(7) 0.0382(9) 0.0398(9) 0.0163(8) 0.0103(7) 0.0138(7) C13 0.0161(6) 0.0283(8) 0.0312(8) 0.0098(6) 0.0061(6) 0.0072(6) N6 0.0156(5) 0.0185(6) 0.0267(6) 0.0081(5) 0.0068(5) 0.0064(5) N7 0.0152(5) 0.0166(6) 0.0324(7) 0.0077(5) 0.0085(5) 0.0077(5) C14 0.0171(6) 0.0169(6) 0.0250(7) 0.0034(5) 0.0065(5) 0.0086(5) C15 0.0198(7) 0.0298(8) 0.0252(7) 0.0103(6) 0.0094(6) 0.0137(6) C16 0.0284(8) 0.0301(8) 0.0331(8) 0.0153(7) 0.0125(7) 0.0163(7) C17 0.0291(8) 0.0292(8) 0.0365(9) 0.0116(7) 0.0115(7) 0.0197(7) C18 0.0245(7) 0.0299(8) 0.0425(10) 0.0102(7) 0.0168(7) 0.0175(7) N8 0.0218(6) 0.0255(7) 0.0403(8) 0.0115(6) 0.0160(6) 0.0137(5) C19 0.0165(6) 0.0170(6) 0.0335(8) 0.0067(6) 0.0109(6) 0.0085(5) C20 0.0240(7) 0.0301(8) 0.0360(9) 0.0109(7) 0.0136(7) 0.0107(7) C21 0.0327(9) 0.0365(10) 0.0542(12) 0.0233(9) 0.0269(9) 0.0176(8) C22 0.0275(8) 0.0219(8) 0.0645(13) 0.0138(8) 0.0260(9) 0.0096(7) C23 0.0231(8) 0.0209(8) 0.0470(10) 0.0001(7) 0.0125(7) 0.0052(6) N9 0.0212(6) 0.0215(6) 0.0338(7) 0.0033(5) 0.0098(6) 0.0070(5) N10 0.0200(6) 0.0147(5) 0.0356(7) 0.0099(5) 0.0129(5) 0.0100(5) C24 0.0204(6) 0.0139(6) 0.0293(7) 0.0045(5) 0.0086(6) 0.0101(5) C26 0.0397(10) 0.0291(9) 0.0663(14) 0.0117(9) 0.0334(10) 0.0183(8) C27 0.0243(8) 0.0306(9) 0.0647(13) -0.0024(9) 0.0070(9) 0.0178(7) C28 0.0475(11) 0.0280(9) 0.0315(9) -0.0001(7) -0.0018(8) 0.0270(8) C25A 0.0357(8) 0.0247(7) 0.0415(9) 0.0117(6) 0.0209(7) 0.0193(7) N12A 0.0372(8) 0.0196(6) 0.0296(7) 0.0073(6) 0.0117(6) 0.0181(6) N12B 0.0357(8) 0.0247(7) 0.0415(9) 0.0117(6) 0.0209(7) 0.0193(7) C25B 0.0372(8) 0.0196(6) 0.0296(7) 0.0073(6) 0.0117(6) 0.0181(6) C29 0.0218(7) 0.0172(6) 0.0305(8) 0.0102(6) 0.0121(6) 0.0105(6) C30 0.0407(9) 0.0300(8) 0.0477(10) 0.0191(8) 0.0304(9) 0.0224(8) C31 0.0409(10) 0.0436(11) 0.0589(13) 0.0310(10) 0.0351(10) 0.0248(9) C32 0.0333(9) 0.0275(8) 0.0471(11) 0.0201(8) 0.0179(8) 0.0080(7) C33 0.0391(9) 0.0180(7) 0.0362(9) 0.0082(7) 0.0150(8) 0.0086(7) N11 0.0323(7) 0.0171(6) 0.0326(7) 0.0073(5) 0.0161(6) 0.0101(5) Fe1 0.01527(14) 0.01122(13) 0.02093(15) 0.00360(10) 0.00613(11) 0.00522(10) N13 0.0230(6) 0.0196(6) 0.0258(6) 0.0037(5) 0.0083(5) 0.0095(5) C34 0.0245(7) 0.0208(7) 0.0232(7) 0.0050(5) 0.0106(6) 0.0115(6) S1 0.0290(2) 0.0255(2) 0.0387(2) 0.00988(17) 0.01863(18) 0.00519(17) O1W 0.0822(17) 0.0822(17) 0.124(2) -0.0033(16) -0.0107(16) 0.0434(14) _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 N1 C1 1.3349(18) . ? N1 C3 1.3408(18) . ? C1 N2 1.3406(18) . ? C1 N4 1.3874(17) . ? N2 C2 1.3411(18) . ? C2 N3 1.3486(18) . ? C2 N7 1.3815(18) . ? N3 C3 1.3424(18) . ? C3 N10 1.3801(18) . ? N4 C4 1.4257(18) . ? N4 C9 1.4334(18) . ? C4 C5 1.392(2) . ? C4 N5 1.3463(19) . ? C5 C6 1.392(2) . ? C6 C7 1.389(3) . ? C7 C8 1.377(3) . ? N5 C8 1.3601(19) . ? N5 Fe1 2.0310(13) . ? C9 C10 1.390(2) . ? C9 N6 1.3462(19) . ? C10 C11 1.390(2) . ? C11 C12 1.390(3) . ? C12 C13 1.382(3) . ? C13 N6 1.3610(19) . ? N6 Fe1 2.0381(13) . ? N7 C14 1.4285(18) . ? N7 C19 1.4448(18) . ? C14 C15 1.392(2) . ? C14 N8 1.336(2) . ? C15 C16 1.386(2) . ? C16 C17 1.391(2) . ? C17 C18 1.380(2) . ? C18 N8 1.350(2) . ? C19 C20 1.390(2) . ? C19 N9 1.327(2) . ? C20 C21 1.387(2) . ? C21 C22 1.379(3) . ? C22 C23 1.378(3) . ? C23 N9 1.349(2) . ? N10 C24 1.4364(19) . ? N10 C29 1.4320(18) . ? C24 C25A 1.368(2) . ? C24 N12A 1.347(2) . ? C26 C27 1.373(3) . ? C26 C25A 1.385(3) . ? C27 C28 1.377(3) . ? C28 N12A 1.370(3) . ? C29 C30 1.392(2) . ? C29 N11 1.330(2) . ? C30 C31 1.384(2) . ? C31 C32 1.387(3) . ? C32 C33 1.375(3) . ? C33 N11 1.348(2) . ? Fe1 N5 2.0309(13) 2_666 ? Fe1 N6 2.0381(13) 2_666 ? Fe1 N13 1.9802(14) . ? Fe1 N13 1.9802(14) 2_666 ? N13 C34 1.169(2) . ? C34 S1 1.6455(16) . ? 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 C1 N1 C3 113.59(12) . . ? N1 C1 N2 126.91(12) . . ? N1 C1 N4 116.44(12) . . ? N2 C1 N4 116.57(12) . . ? C1 N2 C2 113.27(12) . . ? N2 C2 N3 126.24(13) . . ? N2 C2 N7 118.10(12) . . ? N3 C2 N7 115.67(12) . . ? C2 N3 C3 113.47(12) . . ? N1 C3 N3 126.24(13) . . ? N1 C3 N10 117.04(13) . . ? N3 C3 N10 116.72(12) . . ? C1 N4 C4 121.21(11) . . ? C1 N4 C9 120.76(11) . . ? C4 N4 C9 118.03(11) . . ? N4 C4 C5 120.17(13) . . ? N4 C4 N5 116.65(13) . . ? C5 C4 N5 123.11(13) . . ? C4 C5 C6 118.42(15) . . ? C5 C6 C7 119.19(16) . . ? C6 C7 C8 118.68(15) . . ? C4 N5 C8 117.20(14) . . ? C4 N5 Fe1 122.97(10) . . ? C8 N5 Fe1 119.80(11) . . ? C7 C8 N5 123.29(16) . . ? N4 C9 C10 119.86(13) . . ? N4 C9 N6 116.49(13) . . ? C10 C9 N6 123.60(13) . . ? C9 C10 C11 118.38(15) . . ? C10 C11 C12 118.92(16) . . ? C11 C12 C13 119.10(15) . . ? C12 C13 N6 122.88(16) . . ? C9 N6 C13 116.99(14) . . ? C9 N6 Fe1 122.86(10) . . ? C13 N6 Fe1 120.13(11) . . ? C2 N7 C14 124.02(12) . . ? C2 N7 C19 118.83(12) . . ? C14 N7 C19 116.73(12) . . ? N7 C14 C15 122.05(13) . . ? N7 C14 N8 114.26(13) . . ? C15 C14 N8 123.65(14) . . ? C14 C15 C16 117.97(15) . . ? C15 C16 C17 119.46(15) . . ? C16 C17 C18 118.06(15) . . ? C17 C18 N8 123.71(15) . . ? C14 N8 C18 117.05(14) . . ? N7 C19 C20 120.16(14) . . ? N7 C19 N9 115.17(14) . . ? C20 C19 N9 124.66(14) . . ? C19 C20 C21 117.70(17) . . ? C20 C21 C22 118.89(18) . . ? C21 C22 C23 118.85(16) . . ? C22 C23 N9 123.67(17) . . ? C19 N9 C23 116.19(15) . . ? C3 N10 C24 122.11(12) . . ? C3 N10 C29 121.17(12) . . ? C24 N10 C29 116.62(12) . . ? N10 C24 C25A 119.29(14) . . ? N10 C24 N12A 116.30(14) . . ? C25A C24 N12A 124.37(15) . . ? C27 C26 C25A 120.77(19) . . ? C26 C27 C28 118.50(17) . . ? C27 C28 N12A 122.31(17) . . ? C24 C25A C26 117.21(17) . . ? C24 N12A C28 116.80(16) . . ? N10 C29 C30 120.87(14) . . ? N10 C29 N11 115.06(13) . . ? C30 C29 N11 123.97(14) . . ? C29 C30 C31 117.82(17) . . ? C30 C31 C32 119.24(17) . . ? C31 C32 C33 118.42(16) . . ? C32 C33 N11 123.63(17) . . ? C29 N11 C33 116.88(15) . . ? N5 Fe1 N5 180.000(1) . 2_666 ? N5 Fe1 N6 85.50(5) . . ? N5 Fe1 N6 94.50(5) 2_666 . ? N5 Fe1 N6 85.50(5) 2_666 2_666 ? N5 Fe1 N6 94.50(5) . 2_666 ? N5 Fe1 N13 91.23(5) . . ? N5 Fe1 N13 91.23(5) 2_666 2_666 ? N5 Fe1 N13 88.77(5) 2_666 . ? N5 Fe1 N13 88.77(5) . 2_666 ? N6 Fe1 N6 180.0 . 2_666 ? N6 Fe1 N13 91.59(5) . . ? N6 Fe1 N13 88.41(5) . 2_666 ? N6 Fe1 N13 91.59(5) 2_666 2_666 ? N6 Fe1 N13 88.41(5) 2_666 . ? N13 Fe1 N13 180.0 . 2_666 ? Fe1 N13 C34 174.33(13) . . ? N13 C34 S1 179.66(17) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.537 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.061 # Attachment 'Revised_B602903E_250K.CIF' data_eu_22_01b _database_code_depnum_ccdc_archive 'CCDC 298836' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H52 Fe N26 O2 S2' _chemical_formula_weight 1385.33 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6660(7) _cell_length_b 12.8283(7) _cell_length_c 13.4211(8) _cell_angle_alpha 95.9420(10) _cell_angle_beta 111.8980(10) _cell_angle_gamma 115.8500(10) _cell_volume 1589.67(16) _cell_formula_units_Z 1 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 4944 _cell_measurement_theta_min 3.122 _cell_measurement_theta_max 29.492 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9761 _exptl_absorpt_correction_T_max 0.9843 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 0.69230 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 18217 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 29.62 _reflns_number_total 9385 _reflns_number_gt 7126 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _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 and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^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 9385 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1412 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 N1 N 0.27782(13) 0.07922(11) 0.27681(11) 0.0266(3) Uani 1 1 d . . . C1 C 0.23840(15) 0.15863(12) 0.24477(12) 0.0222(3) Uani 1 1 d . . . N2 N 0.10401(13) 0.13755(11) 0.19313(11) 0.0253(2) Uani 1 1 d . . . C2 C 0.00312(15) 0.02112(13) 0.16928(12) 0.0247(3) Uani 1 1 d . . . N3 N 0.02610(13) -0.07046(11) 0.18818(11) 0.0275(3) Uani 1 1 d . . . C3 C 0.16617(16) -0.03379(13) 0.24524(13) 0.0251(3) Uani 1 1 d . . . N4 N 0.34901(13) 0.27691(10) 0.27233(11) 0.0243(2) Uani 1 1 d . . . C4 C 0.31753(15) 0.36706(13) 0.23748(13) 0.0247(3) Uani 1 1 d . . . C5 C 0.23909(17) 0.34768(15) 0.12288(14) 0.0310(3) Uani 1 1 d . . . H5 H 0.2053 0.2756 0.0676 0.037 Uiso 1 1 calc R . . C6 C 0.2123(2) 0.43810(18) 0.09290(16) 0.0399(4) Uani 1 1 d . . . H6 H 0.1574 0.4270 0.0165 0.048 Uiso 1 1 calc R . . C7 C 0.2666(2) 0.54412(18) 0.17559(18) 0.0432(4) Uani 1 1 d . . . H7 H 0.2499 0.6064 0.1566 0.052 Uiso 1 1 calc R . . N5 N 0.37018(15) 0.46899(11) 0.31894(12) 0.0303(3) Uani 1 1 d . . . C8 C 0.3456(2) 0.55693(16) 0.28626(17) 0.0399(4) Uani 1 1 d . . . H8 H 0.3846 0.6303 0.3423 0.048 Uiso 1 1 calc R . . C9 C 0.49654(15) 0.30829(13) 0.33127(13) 0.0247(3) Uani 1 1 d . . . C10 C 0.54689(18) 0.24848(16) 0.28313(15) 0.0343(3) Uani 1 1 d . . . H10 H 0.4860 0.1881 0.2116 0.041 Uiso 1 1 calc R . . C11 C 0.68931(19) 0.28002(17) 0.34317(17) 0.0410(4) Uani 1 1 d . . . H11 H 0.7258 0.2390 0.3143 0.049 Uiso 1 1 calc R . . C12 C 0.77701(18) 0.37274(18) 0.44621(17) 0.0411(4) Uani 1 1 d . . . H12 H 0.8741 0.3960 0.4882 0.049 Uiso 1 1 calc R . . C13 C 0.71985(18) 0.43033(17) 0.48614(15) 0.0380(4) Uani 1 1 d . . . H13A H 0.7807 0.4949 0.5550 0.046 Uiso 1 1 calc R . . N6 N 0.57973(14) 0.39817(12) 0.43070(11) 0.0294(3) Uani 1 1 d . . . N7 N -0.13941(13) -0.00934(12) 0.11901(12) 0.0290(3) Uani 1 1 d . . . C14 C -0.18531(16) 0.07274(14) 0.08184(13) 0.0272(3) Uani 1 1 d . . . C15 C -0.12558(18) 0.14917(16) 0.02669(14) 0.0334(3) Uani 1 1 d . . . H15 H -0.0537 0.1481 0.0113 0.040 Uiso 1 1 calc R . . C16 C -0.1754(2) 0.22691(18) -0.00481(16) 0.0410(4) Uani 1 1 d . . . H16 H -0.1356 0.2817 -0.0402 0.049 Uiso 1 1 calc R . . C17 C -0.2841(2) 0.22312(18) 0.01635(17) 0.0421(4) Uani 1 1 d . . . H17 H -0.3189 0.2755 -0.0036 0.051 Uiso 1 1 calc R . . C18 C -0.33999(19) 0.14099(17) 0.06721(16) 0.0388(4) Uani 1 1 d . . . H18 H -0.4166 0.1365 0.0786 0.047 Uiso 1 1 calc R . . N8 N -0.29158(15) 0.06624(13) 0.10185(13) 0.0349(3) Uani 1 1 d . . . C19 C -0.24863(16) -0.12672(14) 0.10952(14) 0.0292(3) Uani 1 1 d . . . C20 C -0.2477(2) -0.15807(18) 0.20554(17) 0.0403(4) Uani 1 1 d . . . H20 H -0.1764 -0.1033 0.2785 0.048 Uiso 1 1 calc R . . C21 C -0.3550(2) -0.27250(19) 0.1904(2) 0.0501(5) Uani 1 1 d . . . H21 H -0.3584 -0.2973 0.2532 0.060 Uiso 1 1 calc R . . C22 C -0.4566(2) -0.34949(17) 0.0824(2) 0.0516(5) Uani 1 1 d . . . H22 H -0.5291 -0.4285 0.0701 0.062 Uiso 1 1 calc R . . C23 C -0.4505(2) -0.30946(17) -0.00715(19) 0.0465(5) Uani 1 1 d . . . H23 H -0.5221 -0.3623 -0.0807 0.056 Uiso 1 1 calc R . . N9 N -0.34760(15) -0.19836(13) 0.00423(13) 0.0369(3) Uani 1 1 d . . . N10 N 0.19792(14) -0.12210(11) 0.27335(12) 0.0304(3) Uani 1 1 d . C . C24 C 0.34019(17) -0.10323(13) 0.31313(14) 0.0290(3) Uani 1 1 d . . . C26 C 0.5528(3) -0.0404(2) 0.2985(2) 0.0572(6) Uani 1 1 d . . . H26 H 0.6094 -0.0066 0.2627 0.069 Uiso 1 1 calc R A 1 C27 C 0.6052(2) -0.0751(2) 0.3898(2) 0.0601(7) Uani 1 1 d . C . H27 H 0.6975 -0.0649 0.4177 0.072 Uiso 1 1 calc R . . C28 C 0.5202(2) -0.12514(18) 0.44003(18) 0.0530(6) Uani 1 1 d . . . H28 H 0.5556 -0.1495 0.5027 0.064 Uiso 1 1 calc R B 1 C25A C 0.4177(2) -0.05422(16) 0.25793(16) 0.0429(4) Uani 0.50 1 d P C 1 H25A H 0.3807 -0.0308 0.1950 0.052 Uiso 0.50 1 calc PR C 1 N12A N 0.38581(19) -0.14073(14) 0.40209(14) 0.0380(4) Uani 0.50 1 d P C 1 N12B N 0.4177(2) -0.05422(16) 0.25793(16) 0.0429(4) Uani 0.50 1 d P C 2 C25B C 0.38581(19) -0.14073(14) 0.40209(14) 0.0380(4) Uani 0.50 1 d P C 2 H25B H 0.3280 -0.1760 0.4366 0.046 Uiso 0.50 1 calc PR C 2 C29 C 0.08929(17) -0.23657(14) 0.26822(14) 0.0305(3) Uani 1 1 d . . . C30 C 0.0129(2) -0.24039(18) 0.32702(18) 0.0443(4) Uani 1 1 d . C . H30 H 0.0281 -0.1682 0.3693 0.053 Uiso 1 1 calc R . . C31 C -0.0866(2) -0.3538(2) 0.3215(2) 0.0555(6) Uani 1 1 d . . . H31 H -0.1418 -0.3601 0.3592 0.067 Uiso 1 1 calc R C . C32 C -0.1041(2) -0.45733(19) 0.2603(2) 0.0531(5) Uani 1 1 d . C . H32 H -0.1715 -0.5353 0.2553 0.064 Uiso 1 1 calc R . . C33 C -0.0211(2) -0.44441(16) 0.20666(17) 0.0470(5) Uani 1 1 d . . . H33 H -0.0315 -0.5153 0.1666 0.056 Uiso 1 1 calc R C . N11 N 0.07471(17) -0.33477(12) 0.20859(13) 0.0373(3) Uani 1 1 d . C . Fe1 Fe 0.5000 0.5000 0.5000 0.02629(9) Uani 1 2 d S . . N13 N 0.33523(17) 0.33775(13) 0.49415(13) 0.0379(3) Uani 1 1 d . . . C34 C 0.23172(18) 0.25183(14) 0.48110(14) 0.0313(3) Uani 1 1 d . . . S1 S 0.08665(6) 0.13049(5) 0.46376(5) 0.04970(14) Uani 1 1 d . . . O1W O -0.0049(3) 0.3104(2) 0.3131(3) 0.1414(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0223(6) 0.0196(6) 0.0330(6) 0.0070(5) 0.0081(5) 0.0112(5) C1 0.0211(6) 0.0181(6) 0.0243(6) 0.0051(5) 0.0086(5) 0.0095(5) N2 0.0204(6) 0.0196(5) 0.0316(6) 0.0073(5) 0.0084(5) 0.0102(5) C2 0.0212(6) 0.0208(6) 0.0281(7) 0.0051(5) 0.0093(5) 0.0101(5) N3 0.0238(6) 0.0205(6) 0.0364(7) 0.0078(5) 0.0120(5) 0.0120(5) C3 0.0246(7) 0.0206(6) 0.0308(7) 0.0074(5) 0.0120(6) 0.0131(6) N4 0.0192(5) 0.0167(5) 0.0307(6) 0.0061(5) 0.0066(5) 0.0090(5) C4 0.0217(6) 0.0195(6) 0.0319(7) 0.0093(5) 0.0119(6) 0.0100(5) C5 0.0286(7) 0.0312(8) 0.0328(8) 0.0124(6) 0.0131(6) 0.0156(7) C6 0.0391(9) 0.0461(10) 0.0426(10) 0.0262(8) 0.0189(8) 0.0258(8) C7 0.0508(11) 0.0422(10) 0.0587(12) 0.0321(9) 0.0297(10) 0.0343(9) N5 0.0338(7) 0.0197(6) 0.0363(7) 0.0092(5) 0.0147(6) 0.0142(5) C8 0.0521(11) 0.0267(8) 0.0508(10) 0.0165(7) 0.0258(9) 0.0255(8) C9 0.0201(6) 0.0210(6) 0.0308(7) 0.0097(5) 0.0095(6) 0.0105(5) C10 0.0279(8) 0.0316(8) 0.0388(9) 0.0057(7) 0.0133(7) 0.0149(7) C11 0.0309(8) 0.0409(9) 0.0551(11) 0.0129(8) 0.0212(8) 0.0212(8) C12 0.0226(7) 0.0461(10) 0.0506(10) 0.0176(8) 0.0127(7) 0.0177(7) C13 0.0231(7) 0.0382(9) 0.0364(9) 0.0055(7) 0.0059(7) 0.0109(7) N6 0.0210(6) 0.0247(6) 0.0325(7) 0.0054(5) 0.0080(5) 0.0087(5) N7 0.0201(6) 0.0234(6) 0.0391(7) 0.0095(5) 0.0105(5) 0.0108(5) C14 0.0213(6) 0.0242(7) 0.0300(7) 0.0048(6) 0.0072(6) 0.0119(6) C15 0.0280(7) 0.0415(9) 0.0333(8) 0.0153(7) 0.0133(6) 0.0200(7) C16 0.0390(9) 0.0446(10) 0.0441(10) 0.0248(8) 0.0177(8) 0.0241(8) C17 0.0399(10) 0.0394(9) 0.0482(10) 0.0154(8) 0.0134(8) 0.0268(8) C18 0.0312(8) 0.0399(9) 0.0498(10) 0.0108(8) 0.0177(8) 0.0234(8) N8 0.0293(7) 0.0338(7) 0.0455(8) 0.0128(6) 0.0183(6) 0.0185(6) C19 0.0214(7) 0.0234(7) 0.0406(8) 0.0082(6) 0.0130(6) 0.0115(6) C20 0.0331(9) 0.0392(9) 0.0453(10) 0.0153(8) 0.0192(8) 0.0149(8) C21 0.0448(11) 0.0463(11) 0.0708(14) 0.0302(11) 0.0361(11) 0.0224(10) C22 0.0389(10) 0.0269(9) 0.0908(16) 0.0178(10) 0.0372(11) 0.0129(8) C23 0.0319(9) 0.0282(8) 0.0608(12) -0.0006(8) 0.0167(9) 0.0080(7) N9 0.0273(7) 0.0276(7) 0.0433(8) 0.0031(6) 0.0125(6) 0.0095(6) N10 0.0279(6) 0.0194(6) 0.0456(8) 0.0121(5) 0.0162(6) 0.0140(5) C24 0.0275(7) 0.0189(6) 0.0369(8) 0.0056(6) 0.0102(6) 0.0137(6) C26 0.0549(13) 0.0422(11) 0.0941(18) 0.0231(11) 0.0455(13) 0.0310(10) C27 0.0320(10) 0.0398(11) 0.0881(17) -0.0004(11) 0.0094(11) 0.0224(9) C28 0.0598(13) 0.0393(10) 0.0425(10) 0.0027(8) -0.0016(9) 0.0352(10) C25A 0.0508(10) 0.0383(9) 0.0578(11) 0.0204(8) 0.0315(9) 0.0308(8) N12A 0.0476(9) 0.0284(7) 0.0398(8) 0.0119(6) 0.0157(7) 0.0246(7) N12B 0.0508(10) 0.0383(9) 0.0578(11) 0.0204(8) 0.0315(9) 0.0308(8) C25B 0.0476(9) 0.0284(7) 0.0398(8) 0.0119(6) 0.0157(7) 0.0246(7) C29 0.0289(7) 0.0243(7) 0.0393(8) 0.0140(6) 0.0153(7) 0.0142(6) C30 0.0521(11) 0.0399(10) 0.0626(12) 0.0260(9) 0.0371(10) 0.0300(9) C31 0.0572(13) 0.0593(13) 0.0813(16) 0.0447(13) 0.0495(13) 0.0354(11) C32 0.0442(11) 0.0364(10) 0.0666(14) 0.0297(10) 0.0231(10) 0.0108(9) C33 0.0523(12) 0.0226(8) 0.0503(11) 0.0115(8) 0.0195(9) 0.0106(8) N11 0.0431(8) 0.0220(6) 0.0440(8) 0.0109(6) 0.0209(7) 0.0140(6) Fe1 0.02487(16) 0.01741(14) 0.02939(16) 0.00461(11) 0.01040(12) 0.00775(12) N13 0.0369(8) 0.0265(7) 0.0418(8) 0.0074(6) 0.0177(6) 0.0110(6) C34 0.0322(8) 0.0267(7) 0.0319(8) 0.0068(6) 0.0157(6) 0.0126(6) S1 0.0391(3) 0.0390(3) 0.0539(3) 0.0127(2) 0.0255(2) 0.0041(2) O1W 0.106(2) 0.0918(18) 0.136(2) -0.0088(17) -0.0174(18) 0.0510(17) _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 N1 C1 1.3364(18) . ? N1 C3 1.3387(19) . ? C1 N2 1.3388(18) . ? C1 N4 1.3873(18) . ? N2 C2 1.3437(18) . ? C2 N3 1.3424(18) . ? C2 N7 1.3837(18) . ? N3 C3 1.3415(19) . ? C3 N10 1.3832(18) . ? N4 C4 1.4301(18) . ? N4 C9 1.4369(18) . ? C4 C5 1.392(2) . ? C4 N5 1.3360(19) . ? C5 C6 1.387(2) . ? C6 C7 1.377(3) . ? C7 C8 1.371(3) . ? N5 C8 1.356(2) . ? N5 Fe1 2.2105(14) . ? C9 C10 1.387(2) . ? C9 N6 1.3386(19) . ? C10 C11 1.386(2) . ? C11 C12 1.384(3) . ? C12 C13 1.376(3) . ? C13 N6 1.355(2) . ? N6 Fe1 2.2112(13) . ? N7 C14 1.4302(19) . ? N7 C19 1.4399(19) . ? C14 C15 1.391(2) . ? C14 N8 1.334(2) . ? C15 C16 1.386(2) . ? C16 C17 1.382(3) . ? C17 C18 1.372(3) . ? C18 N8 1.350(2) . ? C19 C20 1.387(2) . ? C19 N9 1.328(2) . ? C20 C21 1.382(3) . ? C21 C22 1.372(3) . ? C22 C23 1.368(3) . ? C23 N9 1.350(2) . ? N10 C24 1.435(2) . ? N10 C29 1.4346(19) . ? C24 C25A 1.365(2) . ? C24 N12A 1.345(2) . ? C26 C27 1.367(4) . ? C26 C25A 1.382(3) . ? C27 C28 1.372(4) . ? C28 N12A 1.367(3) . ? C29 C30 1.384(2) . ? C29 N11 1.326(2) . ? C30 C31 1.382(3) . ? C31 C32 1.376(3) . ? C32 C33 1.374(3) . ? C33 N11 1.352(2) . ? Fe1 N5 2.2105(14) 2_666 ? Fe1 N6 2.2113(13) 2_666 ? Fe1 N13 2.0971(15) . ? Fe1 N13 2.0971(15) 2_666 ? N13 C34 1.160(2) . ? C34 S1 1.6357(17) . ? 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 C1 N1 C3 113.35(12) . . ? N1 C1 N2 126.98(13) . . ? N1 C1 N4 116.37(12) . . ? N2 C1 N4 116.59(12) . . ? C1 N2 C2 113.03(12) . . ? N2 C2 N3 126.52(13) . . ? N2 C2 N7 117.60(13) . . ? N3 C2 N7 115.88(12) . . ? C2 N3 C3 113.26(12) . . ? N1 C3 N3 126.53(13) . . ? N1 C3 N10 116.96(13) . . ? N3 C3 N10 116.50(13) . . ? C1 N4 C4 120.44(12) . . ? C1 N4 C9 120.15(11) . . ? C4 N4 C9 119.33(11) . . ? N4 C4 C5 119.86(13) . . ? N4 C4 N5 116.89(13) . . ? C5 C4 N5 123.21(14) . . ? C4 C5 C6 117.89(16) . . ? C5 C6 C7 119.70(16) . . ? C6 C7 C8 118.60(16) . . ? C4 N5 C8 117.27(14) . . ? C4 N5 Fe1 122.55(10) . . ? C8 N5 Fe1 120.14(11) . . ? C7 C8 N5 123.27(17) . . ? N4 C9 C10 119.95(13) . . ? N4 C9 N6 116.60(13) . . ? C10 C9 N6 123.43(14) . . ? C9 C10 C11 118.31(16) . . ? C10 C11 C12 119.05(16) . . ? C11 C12 C13 118.94(16) . . ? C12 C13 N6 122.97(16) . . ? C9 N6 C13 117.22(14) . . ? C9 N6 Fe1 122.59(10) . . ? C13 N6 Fe1 120.09(11) . . ? C2 N7 C14 123.66(12) . . ? C2 N7 C19 119.27(12) . . ? C14 N7 C19 116.93(12) . . ? N7 C14 C15 121.88(14) . . ? N7 C14 N8 114.18(14) . . ? C15 C14 N8 123.91(14) . . ? C14 C15 C16 117.85(15) . . ? C15 C16 C17 119.32(17) . . ? C16 C17 C18 118.40(16) . . ? C17 C18 N8 123.92(16) . . ? C14 N8 C18 116.52(15) . . ? N7 C19 C20 120.70(15) . . ? N7 C19 N9 114.99(14) . . ? C20 C19 N9 124.30(16) . . ? C19 C20 C21 117.72(19) . . ? C20 C21 C22 119.2(2) . . ? C21 C22 C23 118.92(18) . . ? C22 C23 N9 123.65(19) . . ? C19 N9 C23 116.21(17) . . ? C3 N10 C24 122.56(12) . . ? C3 N10 C29 120.82(13) . . ? C24 N10 C29 116.58(12) . . ? N10 C24 C25A 119.66(15) . . ? N10 C24 N12A 116.06(15) . . ? C25A C24 N12A 124.23(16) . . ? C27 C26 C25A 120.8(2) . . ? C26 C27 C28 118.59(19) . . ? C27 C28 N12A 122.26(19) . . ? C24 C25A C26 117.21(18) . . ? C24 N12A C28 116.85(18) . . ? N10 C29 C30 120.89(15) . . ? N10 C29 N11 114.94(14) . . ? C30 C29 N11 124.09(15) . . ? C29 C30 C31 117.85(18) . . ? C30 C31 C32 119.38(19) . . ? C31 C32 C33 118.63(18) . . ? C32 C33 N11 123.21(18) . . ? C29 N11 C33 116.81(16) . . ? N5 Fe1 N5 180.0 . 2_666 ? N5 Fe1 N6 82.71(5) . . ? N5 Fe1 N6 97.29(5) 2_666 . ? N5 Fe1 N6 97.29(5) . 2_666 ? N5 Fe1 N6 82.71(5) 2_666 2_666 ? N5 Fe1 N13 91.13(6) . . ? N5 Fe1 N13 88.87(5) . 2_666 ? N5 Fe1 N13 91.13(6) 2_666 2_666 ? N5 Fe1 N13 88.87(6) 2_666 . ? N6 Fe1 N6 180.00(7) . 2_666 ? N6 Fe1 N13 91.20(5) . . ? N6 Fe1 N13 88.80(5) . 2_666 ? N6 Fe1 N13 91.20(5) 2_666 2_666 ? N6 Fe1 N13 88.80(5) 2_666 . ? N13 Fe1 N13 180.0 . 2_666 ? Fe1 N13 C34 170.89(15) . . ? N13 C34 S1 179.46(19) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.564 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.057 data_eu_22_01a _database_code_depnum_ccdc_archive 'CCDC 298837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H52 Fe N26 O2 S2' _chemical_formula_weight 1385.33 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7103(5) _cell_length_b 12.8096(6) _cell_length_c 12.9408(6) _cell_angle_alpha 95.223(2) _cell_angle_beta 111.650(2) _cell_angle_gamma 116.420(2) _cell_volume 1537.98(12) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6872 _cell_measurement_theta_min 2.319 _cell_measurement_theta_max 29.548 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9753 _exptl_absorpt_correction_T_max 0.9843 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69230 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 17506 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 29.59 _reflns_number_total 9033 _reflns_number_gt 7565 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _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 and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.4509P] 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 9033 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1206 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 N1 N 0.27815(13) 0.08506(10) 0.27450(10) 0.0156(2) Uani 1 1 d . . . C1 C 0.24050(14) 0.16595(12) 0.24268(11) 0.0130(2) Uani 1 1 d . . . N2 N 0.10747(12) 0.14556(10) 0.18822(10) 0.0149(2) Uani 1 1 d . . . C2 C 0.00543(15) 0.02846(12) 0.16119(12) 0.0142(2) Uani 1 1 d . . . N3 N 0.02664(13) -0.06476(10) 0.17924(11) 0.0158(2) Uani 1 1 d . . . C3 C 0.16567(15) -0.02905(12) 0.23925(12) 0.0145(2) Uani 1 1 d . . . N4 N 0.35272(12) 0.28573(10) 0.27561(10) 0.0137(2) Uani 1 1 d . . . C4 C 0.32586(14) 0.37972(12) 0.24553(12) 0.0141(2) Uani 1 1 d . . . C5 C 0.24582(15) 0.36633(13) 0.12927(12) 0.0167(3) Uani 1 1 d . . . H5 H 0.2056 0.2934 0.0693 0.020 Uiso 1 1 calc R . . C6 C 0.22598(16) 0.46138(14) 0.10261(13) 0.0203(3) Uani 1 1 d . . . H6 H 0.1689 0.4535 0.0244 0.024 Uiso 1 1 calc R . . C7 C 0.29109(17) 0.56874(14) 0.19239(14) 0.0210(3) Uani 1 1 d . . . H7 H 0.2806 0.6357 0.1763 0.025 Uiso 1 1 calc R . . N5 N 0.38680(13) 0.48169(10) 0.33368(10) 0.0144(2) Uani 1 1 d . . . C8 C 0.37105(16) 0.57574(13) 0.30491(13) 0.0183(3) Uani 1 1 d . . . H8 H 0.4175 0.6499 0.3654 0.022 Uiso 1 1 calc R . . C9 C 0.49857(14) 0.31854(12) 0.34055(12) 0.0139(2) Uani 1 1 d . . . C10 C 0.55212(16) 0.25699(13) 0.29775(13) 0.0185(3) Uani 1 1 d . . . H10 H 0.4921 0.1924 0.2260 0.022 Uiso 1 1 calc R . . C11 C 0.69489(17) 0.29174(14) 0.36195(14) 0.0219(3) Uani 1 1 d . . . H11 H 0.7331 0.2487 0.3370 0.026 Uiso 1 1 calc R . . C12 C 0.78091(16) 0.39097(14) 0.46377(14) 0.0213(3) Uani 1 1 d . . . H12 H 0.8794 0.4177 0.5086 0.026 Uiso 1 1 calc R . . C13 C 0.72092(15) 0.45004(13) 0.49867(13) 0.0182(3) Uani 1 1 d . . . H13 H 0.7811 0.5195 0.5665 0.022 Uiso 1 1 calc R . . N6 N 0.57949(12) 0.41309(10) 0.44010(10) 0.0146(2) Uani 1 1 d . . . N7 N -0.13635(13) -0.00196(11) 0.10961(11) 0.0165(2) Uani 1 1 d . . . C14 C -0.18184(15) 0.08205(12) 0.07830(12) 0.0158(3) Uani 1 1 d . . . C15 C -0.11693(15) 0.16998(14) 0.03008(12) 0.0180(3) Uani 1 1 d . . . H15 H -0.0417 0.1749 0.0147 0.022 Uiso 1 1 calc R . . C16 C -0.16593(17) 0.25000(14) 0.00531(13) 0.0213(3) Uani 1 1 d . . . H16 H -0.1225 0.3125 -0.0254 0.026 Uiso 1 1 calc R . . C17 C -0.27928(17) 0.23774(14) 0.02586(14) 0.0225(3) Uani 1 1 d . . . H17 H -0.3135 0.2923 0.0110 0.027 Uiso 1 1 calc R . . C18 C -0.34043(17) 0.14373(14) 0.06857(14) 0.0224(3) Uani 1 1 d . . . H18 H -0.4206 0.1329 0.0793 0.027 Uiso 1 1 calc R . . N8 N -0.29292(14) 0.06674(12) 0.09583(12) 0.0211(3) Uani 1 1 d . . . C19 C -0.24505(15) -0.12086(12) 0.10045(13) 0.0162(3) Uani 1 1 d . . . C20 C -0.24455(17) -0.15108(15) 0.20139(14) 0.0223(3) Uani 1 1 d . . . H20 H -0.1738 -0.0946 0.2767 0.027 Uiso 1 1 calc R . . C21 C -0.35127(19) -0.26684(16) 0.18788(16) 0.0275(3) Uani 1 1 d . . . H21 H -0.3551 -0.2914 0.2542 0.033 Uiso 1 1 calc R . . C22 C -0.45184(18) -0.34563(15) 0.07613(16) 0.0268(3) Uani 1 1 d . . . H22 H -0.5247 -0.4259 0.0644 0.032 Uiso 1 1 calc R . . C23 C -0.44427(17) -0.30533(14) -0.01815(15) 0.0250(3) Uani 1 1 d . . . H23 H -0.5149 -0.3594 -0.0945 0.030 Uiso 1 1 calc R . . N9 N -0.34217(14) -0.19358(12) -0.00769(11) 0.0208(3) Uani 1 1 d . . . N10 N 0.19607(13) -0.11850(11) 0.26698(11) 0.0171(2) Uani 1 1 d . C . C24 C 0.33756(15) -0.09916(12) 0.30555(12) 0.0156(3) Uani 1 1 d . . . C26 C 0.5472(2) -0.03534(16) 0.28453(18) 0.0317(4) Uani 1 1 d . . . H26 H 0.6020 -0.0020 0.2446 0.038 Uiso 1 1 calc R A 1 C27 C 0.60315(18) -0.06816(16) 0.38116(18) 0.0340(4) Uani 1 1 d . C . H27 H 0.6964 -0.0568 0.4088 0.041 Uiso 1 1 calc R . . C28 C 0.5206(2) -0.11782(15) 0.43671(15) 0.0304(4) Uani 1 1 d . . . H28 H 0.5586 -0.1404 0.5034 0.036 Uiso 1 1 calc R B 1 C25A C 0.41228(17) -0.05051(13) 0.24530(14) 0.0234(3) Uani 0.50 1 d P C 1 H25A H 0.3730 -0.0280 0.1790 0.028 Uiso 0.50 1 calc PR C 1 N12A N 0.38584(16) -0.13559(12) 0.39898(12) 0.0212(3) Uani 0.50 1 d P C 1 N12B N 0.41228(17) -0.05051(13) 0.24530(14) 0.0234(3) Uani 0.50 1 d P C 2 C25B C 0.38584(16) -0.13559(12) 0.39898(12) 0.0212(3) Uani 0.50 1 d P C 2 H25B H 0.3288 -0.1718 0.4366 0.025 Uiso 0.50 1 calc PR C 2 C29 C 0.08861(15) -0.23235(13) 0.26519(13) 0.0168(3) Uani 1 1 d . . . C30 C 0.00987(19) -0.23500(15) 0.32470(15) 0.0249(3) Uani 1 1 d . C . H30 H 0.0235 -0.1615 0.3653 0.030 Uiso 1 1 calc R . . C31 C -0.0891(2) -0.34859(17) 0.32265(17) 0.0303(4) Uani 1 1 d . . . H31 H -0.1464 -0.3544 0.3606 0.036 Uiso 1 1 calc R C . C32 C -0.10324(19) -0.45357(16) 0.26428(16) 0.0288(4) Uani 1 1 d . C . H32 H -0.1707 -0.5324 0.2610 0.035 Uiso 1 1 calc R . . C33 C -0.01678(19) -0.44040(14) 0.21121(14) 0.0252(3) Uani 1 1 d . . . H33 H -0.0244 -0.5121 0.1737 0.030 Uiso 1 1 calc R C . N11 N 0.07770(14) -0.33170(11) 0.20955(11) 0.0203(3) Uani 1 1 d . C . Fe1 Fe 0.5000 0.5000 0.5000 0.01254(8) Uani 1 2 d S . . N13 N 0.34365(13) 0.34559(11) 0.48966(10) 0.0167(2) Uani 1 1 d . . . C34 C 0.24420(15) 0.25725(13) 0.48133(12) 0.0162(3) Uani 1 1 d . . . S1 S 0.10249(4) 0.13246(3) 0.46833(3) 0.02366(10) Uani 1 1 d . . . O1W O -0.0224(2) 0.2996(2) 0.3285(2) 0.0886(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0134(5) 0.0116(5) 0.0189(5) 0.0038(4) 0.0052(4) 0.0061(4) C1 0.0134(6) 0.0108(5) 0.0132(6) 0.0027(4) 0.0052(5) 0.0058(5) N2 0.0119(5) 0.0116(5) 0.0172(5) 0.0029(4) 0.0041(4) 0.0054(4) C2 0.0133(6) 0.0130(6) 0.0160(6) 0.0032(5) 0.0061(5) 0.0071(5) N3 0.0136(5) 0.0114(5) 0.0206(6) 0.0033(4) 0.0067(5) 0.0063(4) C3 0.0148(6) 0.0121(6) 0.0176(6) 0.0042(5) 0.0075(5) 0.0077(5) N4 0.0115(5) 0.0101(5) 0.0161(5) 0.0031(4) 0.0035(4) 0.0055(4) C4 0.0124(6) 0.0114(6) 0.0182(6) 0.0052(5) 0.0065(5) 0.0062(5) C5 0.0151(6) 0.0158(6) 0.0177(6) 0.0052(5) 0.0068(5) 0.0073(5) C6 0.0192(7) 0.0223(7) 0.0202(7) 0.0100(6) 0.0079(6) 0.0117(6) C7 0.0237(7) 0.0194(7) 0.0264(7) 0.0125(6) 0.0126(6) 0.0142(6) N5 0.0137(5) 0.0103(5) 0.0178(5) 0.0042(4) 0.0068(4) 0.0055(4) C8 0.0206(7) 0.0137(6) 0.0224(7) 0.0068(5) 0.0094(6) 0.0105(5) C9 0.0115(6) 0.0115(6) 0.0163(6) 0.0048(5) 0.0050(5) 0.0050(5) C10 0.0168(6) 0.0160(6) 0.0209(7) 0.0034(5) 0.0079(5) 0.0081(5) C11 0.0184(7) 0.0220(7) 0.0288(8) 0.0069(6) 0.0115(6) 0.0126(6) C12 0.0135(6) 0.0239(7) 0.0252(7) 0.0076(6) 0.0072(6) 0.0100(6) C13 0.0128(6) 0.0165(6) 0.0191(6) 0.0041(5) 0.0042(5) 0.0055(5) N6 0.0115(5) 0.0127(5) 0.0163(5) 0.0041(4) 0.0046(4) 0.0052(4) N7 0.0117(5) 0.0124(5) 0.0230(6) 0.0056(4) 0.0061(5) 0.0058(4) C14 0.0131(6) 0.0130(6) 0.0180(6) 0.0027(5) 0.0044(5) 0.0069(5) C15 0.0145(6) 0.0217(7) 0.0177(6) 0.0066(5) 0.0066(5) 0.0098(5) C16 0.0208(7) 0.0212(7) 0.0222(7) 0.0097(6) 0.0085(6) 0.0115(6) C17 0.0213(7) 0.0204(7) 0.0266(7) 0.0071(6) 0.0080(6) 0.0137(6) C18 0.0189(7) 0.0225(7) 0.0298(8) 0.0074(6) 0.0124(6) 0.0128(6) N8 0.0176(6) 0.0187(6) 0.0290(7) 0.0077(5) 0.0114(5) 0.0102(5) C19 0.0122(6) 0.0131(6) 0.0231(7) 0.0048(5) 0.0079(5) 0.0065(5) C20 0.0169(7) 0.0229(7) 0.0236(7) 0.0066(6) 0.0088(6) 0.0081(6) C21 0.0251(8) 0.0282(8) 0.0353(9) 0.0165(7) 0.0188(7) 0.0133(7) C22 0.0212(7) 0.0169(7) 0.0441(10) 0.0105(7) 0.0189(7) 0.0078(6) C23 0.0181(7) 0.0164(7) 0.0310(8) -0.0001(6) 0.0095(6) 0.0043(6) N9 0.0167(6) 0.0164(6) 0.0232(6) 0.0024(5) 0.0078(5) 0.0058(5) N10 0.0149(5) 0.0115(5) 0.0259(6) 0.0071(4) 0.0095(5) 0.0073(4) C24 0.0149(6) 0.0105(6) 0.0194(6) 0.0026(5) 0.0052(5) 0.0076(5) C26 0.0315(9) 0.0215(8) 0.0492(11) 0.0086(7) 0.0266(8) 0.0131(7) C27 0.0173(7) 0.0234(8) 0.0489(11) -0.0041(7) 0.0038(7) 0.0129(7) C28 0.0382(9) 0.0209(7) 0.0221(7) -0.0004(6) -0.0017(7) 0.0215(7) C25A 0.0280(7) 0.0177(6) 0.0297(7) 0.0081(5) 0.0155(6) 0.0139(6) N12A 0.0283(7) 0.0139(6) 0.0208(6) 0.0051(5) 0.0086(6) 0.0127(5) N12B 0.0280(7) 0.0177(6) 0.0297(7) 0.0081(5) 0.0155(6) 0.0139(6) C25B 0.0283(7) 0.0139(6) 0.0208(6) 0.0051(5) 0.0086(6) 0.0127(5) C29 0.0161(6) 0.0137(6) 0.0216(6) 0.0078(5) 0.0090(5) 0.0077(5) C30 0.0311(8) 0.0230(7) 0.0331(8) 0.0137(6) 0.0212(7) 0.0174(7) C31 0.0310(9) 0.0316(9) 0.0427(10) 0.0221(8) 0.0254(8) 0.0183(8) C32 0.0235(8) 0.0213(7) 0.0334(9) 0.0142(7) 0.0117(7) 0.0053(6) C33 0.0291(8) 0.0130(6) 0.0244(7) 0.0044(6) 0.0100(6) 0.0061(6) N11 0.0234(6) 0.0131(5) 0.0226(6) 0.0054(5) 0.0113(5) 0.0075(5) Fe1 0.01090(13) 0.00830(12) 0.01465(13) 0.00235(9) 0.00415(10) 0.00368(10) N13 0.0162(5) 0.0140(5) 0.0171(5) 0.0033(4) 0.0062(4) 0.0072(5) C34 0.0168(6) 0.0148(6) 0.0156(6) 0.0035(5) 0.0069(5) 0.0078(5) S1 0.01913(18) 0.01752(18) 0.02611(19) 0.00592(14) 0.01211(15) 0.00198(14) O1W 0.0630(14) 0.0653(14) 0.0910(17) 0.0009(12) -0.0022(12) 0.0321(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.3372(17) . ? N1 C3 1.3422(17) . ? C1 N2 1.3364(17) . ? C1 N4 1.3915(17) . ? N2 C2 1.3421(17) . ? C2 N3 1.3468(17) . ? C2 N7 1.3832(18) . ? N3 C3 1.3426(18) . ? C3 N10 1.3828(17) . ? N4 C4 1.4256(17) . ? N4 C9 1.4274(17) . ? C4 C5 1.3931(19) . ? C4 N5 1.3473(17) . ? C5 C6 1.387(2) . ? C6 C7 1.395(2) . ? C7 C8 1.379(2) . ? N5 C8 1.3612(17) . ? N5 Fe1 1.9927(12) . ? C9 C10 1.3923(19) . ? C9 N6 1.3484(17) . ? C10 C11 1.389(2) . ? C11 C12 1.394(2) . ? C12 C13 1.384(2) . ? C13 N6 1.3609(18) . ? N6 Fe1 2.0011(12) . ? N7 C14 1.4270(17) . ? N7 C19 1.4438(17) . ? C14 C15 1.397(2) . ? C14 N8 1.3345(19) . ? C15 C16 1.389(2) . ? C16 C17 1.393(2) . ? C17 C18 1.384(2) . ? C18 N8 1.347(2) . ? C19 C20 1.394(2) . ? C19 N9 1.3286(19) . ? C20 C21 1.391(2) . ? C21 C22 1.384(3) . ? C22 C23 1.384(2) . ? C23 N9 1.349(2) . ? N10 C24 1.4345(18) . ? N10 C29 1.4318(17) . ? C24 C25A 1.367(2) . ? C24 N12A 1.3536(19) . ? C26 C27 1.381(3) . ? C26 C25A 1.381(2) . ? C27 C28 1.380(3) . ? C28 N12A 1.368(2) . ? C29 C30 1.395(2) . ? C29 N11 1.3322(19) . ? C30 C31 1.390(2) . ? C31 C32 1.390(3) . ? C32 C33 1.381(3) . ? C33 N11 1.3474(19) . ? Fe1 N5 1.9927(12) 2_666 ? Fe1 N6 2.0012(12) 2_666 ? Fe1 N13 1.9572(13) . ? Fe1 N13 1.9572(13) 2_666 ? N13 C34 1.1665(19) . ? C34 S1 1.6498(15) . ? 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 C1 N1 C3 113.35(12) . . ? N1 C1 N2 127.14(12) . . ? N1 C1 N4 116.02(12) . . ? N2 C1 N4 116.75(11) . . ? C1 N2 C2 113.14(11) . . ? N2 C2 N3 126.39(13) . . ? N2 C2 N7 118.11(12) . . ? N3 C2 N7 115.50(12) . . ? C2 N3 C3 113.37(11) . . ? N1 C3 N3 126.30(12) . . ? N1 C3 N10 116.80(12) . . ? N3 C3 N10 116.91(12) . . ? C1 N4 C4 121.10(11) . . ? C1 N4 C9 121.11(11) . . ? C4 N4 C9 117.79(11) . . ? N4 C4 C5 120.29(12) . . ? N4 C4 N5 116.63(12) . . ? C5 C4 N5 123.02(12) . . ? C4 C5 C6 118.80(13) . . ? C5 C6 C7 118.96(13) . . ? C6 C7 C8 118.68(13) . . ? C4 N5 C8 117.14(12) . . ? C4 N5 Fe1 122.89(9) . . ? C8 N5 Fe1 119.95(9) . . ? C7 C8 N5 123.31(13) . . ? N4 C9 C10 119.95(12) . . ? N4 C9 N6 116.71(12) . . ? C10 C9 N6 123.29(13) . . ? C9 C10 C11 118.79(13) . . ? C10 C11 C12 118.66(14) . . ? C11 C12 C13 119.10(14) . . ? C12 C13 N6 122.92(13) . . ? C9 N6 C13 117.10(12) . . ? C9 N6 Fe1 122.56(9) . . ? C13 N6 Fe1 120.32(9) . . ? C2 N7 C14 124.21(11) . . ? C2 N7 C19 118.64(11) . . ? C14 N7 C19 116.60(11) . . ? N7 C14 C15 122.01(13) . . ? N7 C14 N8 114.41(12) . . ? C15 C14 N8 123.55(13) . . ? C14 C15 C16 117.89(14) . . ? C15 C16 C17 119.43(14) . . ? C16 C17 C18 117.95(14) . . ? C17 C18 N8 123.79(14) . . ? C14 N8 C18 117.26(13) . . ? N7 C19 C20 119.87(13) . . ? N7 C19 N9 115.40(12) . . ? C20 C19 N9 124.71(13) . . ? C19 C20 C21 117.65(15) . . ? C20 C21 C22 118.86(15) . . ? C21 C22 C23 118.76(15) . . ? C22 C23 N9 123.67(15) . . ? C19 N9 C23 116.32(14) . . ? C3 N10 C24 121.95(11) . . ? C3 N10 C29 120.98(12) . . ? C24 N10 C29 116.97(11) . . ? N10 C24 C25A 119.45(13) . . ? N10 C24 N12A 116.19(13) . . ? C25A C24 N12A 124.32(14) . . ? C27 C26 C25A 120.69(17) . . ? C26 C27 C28 118.49(16) . . ? C27 C28 N12A 122.19(16) . . ? C24 C25A C26 117.42(15) . . ? C24 N12A C28 116.86(15) . . ? N10 C29 C30 120.93(13) . . ? N10 C29 N11 114.94(12) . . ? C30 C29 N11 124.00(14) . . ? C29 C30 C31 117.87(15) . . ? C30 C31 C32 119.11(16) . . ? C31 C32 C33 118.32(15) . . ? C32 C33 N11 123.81(15) . . ? C29 N11 C33 116.84(14) . . ? N5 Fe1 N5 180.0 . 2_666 ? N5 Fe1 N6 86.24(5) . . ? N5 Fe1 N6 93.76(5) 2_666 . ? N5 Fe1 N6 86.24(5) 2_666 2_666 ? N5 Fe1 N6 93.76(5) . 2_666 ? N5 Fe1 N13 91.30(5) . . ? N5 Fe1 N13 88.70(5) 2_666 . ? N5 Fe1 N13 91.29(5) 2_666 2_666 ? N5 Fe1 N13 88.71(5) . 2_666 ? N6 Fe1 N6 180.00(6) . 2_666 ? N6 Fe1 N13 91.71(5) . . ? N6 Fe1 N13 88.29(5) . 2_666 ? N6 Fe1 N13 88.29(5) 2_666 . ? N6 Fe1 N13 91.71(5) 2_666 2_666 ? N13 Fe1 N13 180.0 . 2_666 ? Fe1 N13 C34 175.04(12) . . ? N13 C34 S1 179.41(15) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.559 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.064