data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H21 Fe N5 O S, B F4' _chemical_formula_sum 'C24 H21 B F4 Fe N5 O S' _chemical_formula_weight 570.18 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 11.65041(18) _cell_length_b 14.6344(2) _cell_length_c 28.0712(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4786.05(13) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8657 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 27.62 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.714 _exptl_absorpt_correction_T_max 0.832 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.989 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19130 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5498 _reflns_number_gt 4680 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL v6.10 (Sheldrick, 2008)' _computing_publication_material 'SHELXTL v6.10 (Sheldrick, 2008)' _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^)+(0.0441P)^2^+4.5499P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5498 _refine_ls_number_parameters 390 _refine_ls_number_restraints 163 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.061 _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 0.87174(2) 0.161495(18) 0.128962(10) 0.01840(9) Uani 1 1 d . . . S1 S 0.81112(4) 0.29743(3) 0.161148(18) 0.02382(12) Uani 1 1 d . A . C1 C 0.66615(18) 0.28177(13) 0.17721(7) 0.0245(4) Uani 1 1 d . . . C2 C 0.6280(2) 0.31622(15) 0.22091(8) 0.0329(5) Uani 1 1 d . A . H2 H 0.6814 0.3432 0.2423 0.040 Uiso 1 1 calc R . . C3 C 0.5132(2) 0.31139(16) 0.23331(9) 0.0391(6) Uani 1 1 d . . . H3 H 0.4882 0.3359 0.2629 0.047 Uiso 1 1 calc R A . C4 C 0.4350(2) 0.27111(16) 0.20298(10) 0.0395(6) Uani 1 1 d . A . H4 H 0.3561 0.2687 0.2115 0.047 Uiso 1 1 calc R . . C5 C 0.47171(19) 0.23422(15) 0.16009(9) 0.0316(5) Uani 1 1 d . . . H5 H 0.4180 0.2050 0.1397 0.038 Uiso 1 1 calc R A . C6 C 0.58684(17) 0.23964(14) 0.14668(7) 0.0247(4) Uani 1 1 d . A . C7 C 0.62310(16) 0.20664(14) 0.09841(7) 0.0236(4) Uani 1 1 d . . . H7A H 0.5542 0.1863 0.0807 0.028 Uiso 1 1 calc R A . H7B H 0.6575 0.2583 0.0807 0.028 Uiso 1 1 calc R . . C8 C 0.74716(17) 0.10753(14) 0.05088(7) 0.0223(4) Uani 1 1 d . . . H8 H 0.6822 0.0904 0.0294 0.027 Uiso 1 1 calc R A . C9 C 0.81033(16) 0.19161(13) 0.03368(7) 0.0218(4) Uani 1 1 d . A . C10 C 0.79465(18) 0.23279(16) -0.01022(7) 0.0289(5) Uani 1 1 d . . . H10 H 0.7421 0.2082 -0.0327 0.035 Uiso 1 1 calc R A . C11 C 0.8572(2) 0.31044(17) -0.02056(8) 0.0333(5) Uani 1 1 d . A . H11 H 0.8479 0.3405 -0.0503 0.040 Uiso 1 1 calc R . . C12 C 0.9336(2) 0.34408(15) 0.01296(8) 0.0326(5) Uani 1 1 d . . . H12 H 0.9775 0.3972 0.0062 0.039 Uiso 1 1 calc R A . C13 C 0.94567(18) 0.30004(14) 0.05611(8) 0.0261(4) Uani 1 1 d . A . H13 H 0.9979 0.3235 0.0790 0.031 Uiso 1 1 calc R . . C14 C 0.83504(16) 0.03255(13) 0.05499(7) 0.0207(4) Uani 1 1 d . A . C15 C 0.84807(17) -0.03813(14) 0.02290(7) 0.0246(4) Uani 1 1 d . . . H15 H 0.7977 -0.0445 -0.0035 0.030 Uiso 1 1 calc R A . C16 C 0.93702(18) -0.09956(13) 0.03041(8) 0.0263(4) Uani 1 1 d . A . H16 H 0.9485 -0.1490 0.0090 0.032 Uiso 1 1 calc R . . C17 C 1.00856(18) -0.08850(14) 0.06902(8) 0.0264(4) Uani 1 1 d . . . H17 H 1.0692 -0.1305 0.0747 0.032 Uiso 1 1 calc R A . C18 C 0.99071(17) -0.01499(13) 0.09948(7) 0.0230(4) Uani 1 1 d . A . H18 H 1.0404 -0.0070 0.1260 0.028 Uiso 1 1 calc R . . C19 C 0.66034(17) 0.05095(14) 0.12689(8) 0.0241(4) Uani 1 1 d . . . H19A H 0.6856 -0.0068 0.1118 0.029 Uiso 1 1 calc R A . H19B H 0.5754 0.0528 0.1263 0.029 Uiso 1 1 calc R . . C20 C 0.70187(17) 0.05445(13) 0.17744(7) 0.0234(4) Uani 1 1 d . A . C21 C 0.6398(2) 0.01649(15) 0.21459(8) 0.0320(5) Uani 1 1 d . . . H21 H 0.5666 -0.0101 0.2090 0.038 Uiso 1 1 calc R A . C22 C 0.6858(2) 0.01778(16) 0.25993(9) 0.0395(6) Uani 1 1 d . A . H22 H 0.6445 -0.0078 0.2859 0.047 Uiso 1 1 calc R . . C23 C 0.7921(3) 0.05648(16) 0.26717(8) 0.0389(6) Uani 1 1 d . . . H23 H 0.8252 0.0575 0.2981 0.047 Uiso 1 1 calc R A . C24 C 0.8498(2) 0.09379(15) 0.22891(8) 0.0291(5) Uani 1 1 d . A . H24 H 0.9230 0.1207 0.2340 0.035 Uiso 1 1 calc R . . N1 N 0.70737(13) 0.13001(11) 0.10007(6) 0.0195(3) Uani 1 1 d . A . N2 N 0.88469(14) 0.22444(11) 0.06632(6) 0.0210(3) Uani 1 1 d . A . N3 N 0.90563(13) 0.04472(11) 0.09257(6) 0.0197(3) Uani 1 1 d . A . N4 N 0.80556(14) 0.09320(11) 0.18461(6) 0.0215(3) Uani 1 1 d . A . N5 N 1.01045(15) 0.17981(12) 0.14907(7) 0.0260(4) Uani 0.886(10) 1 d PD A 1 O1 O 1.0908(2) 0.22546(18) 0.14802(17) 0.0639(12) Uani 0.886(10) 1 d PDU A 1 N5' N 1.01045(15) 0.17981(12) 0.14907(7) 0.0260(4) Uani 0.114(10) 1 d PD A 2 O1' O 1.0766(17) 0.196(2) 0.1773(9) 0.062(7) Uani 0.114(10) 1 d PDU A 2 B1 B 0.1749(7) 0.4693(7) 0.1004(3) 0.0351(15) Uani 0.597(6) 1 d PDU B 1 F1 F 0.2482(3) 0.3979(2) 0.10903(16) 0.0667(12) Uani 0.597(6) 1 d PDU B 1 F2 F 0.0870(7) 0.4646(6) 0.1312(3) 0.075(2) Uani 0.597(6) 1 d PDU B 1 F3 F 0.2268(7) 0.5541(5) 0.1033(3) 0.085(2) Uani 0.597(6) 1 d PDU B 1 F4 F 0.1379(3) 0.4654(2) 0.05377(9) 0.0574(13) Uani 0.597(6) 1 d PDU B 1 B1' B 0.1535(11) 0.4808(9) 0.0970(4) 0.0335(18) Uani 0.403(6) 1 d PDU B 2 F1' F 0.2412(5) 0.5433(6) 0.1107(3) 0.0363(14) Uani 0.403(6) 1 d PDU B 2 F2' F 0.0970(9) 0.4511(6) 0.1368(4) 0.0421(17) Uani 0.403(6) 1 d PDU B 2 F3' F 0.0665(4) 0.5131(3) 0.06565(14) 0.0479(15) Uani 0.403(6) 1 d PDU B 2 F4' F 0.2031(4) 0.4095(4) 0.0736(2) 0.068(2) Uani 0.403(6) 1 d PDU B 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 0.01880(14) 0.01570(14) 0.02069(15) -0.00117(11) -0.00045(10) 0.00043(10) S1 0.0296(2) 0.0173(2) 0.0246(2) -0.00269(19) 0.0006(2) 0.00108(19) C1 0.0304(10) 0.0161(9) 0.0270(10) 0.0031(8) 0.0062(8) 0.0068(8) C2 0.0482(13) 0.0202(10) 0.0304(11) -0.0016(9) 0.0079(10) 0.0067(9) C3 0.0563(15) 0.0251(11) 0.0360(13) 0.0011(10) 0.0207(12) 0.0126(11) C4 0.0369(12) 0.0297(12) 0.0520(15) 0.0091(11) 0.0216(11) 0.0115(10) C5 0.0283(10) 0.0260(11) 0.0405(13) 0.0071(10) 0.0066(9) 0.0060(9) C6 0.0276(10) 0.0198(9) 0.0265(10) 0.0048(8) 0.0049(8) 0.0075(8) C7 0.0205(9) 0.0264(10) 0.0238(9) -0.0001(8) -0.0019(8) 0.0061(8) C8 0.0207(8) 0.0258(10) 0.0206(9) -0.0071(8) -0.0032(7) 0.0011(8) C9 0.0219(9) 0.0222(9) 0.0213(9) -0.0036(8) 0.0014(7) 0.0066(8) C10 0.0304(10) 0.0348(12) 0.0214(10) -0.0022(9) 0.0039(8) 0.0123(9) C11 0.0398(12) 0.0355(12) 0.0246(10) 0.0070(9) 0.0147(9) 0.0169(10) C12 0.0361(11) 0.0244(10) 0.0374(12) 0.0035(9) 0.0188(10) 0.0042(9) C13 0.0259(9) 0.0211(10) 0.0314(11) -0.0033(8) 0.0084(8) 0.0006(8) C14 0.0203(8) 0.0184(9) 0.0234(9) -0.0032(8) 0.0012(7) -0.0031(7) C15 0.0270(10) 0.0205(9) 0.0262(10) -0.0053(8) 0.0044(8) -0.0080(8) C16 0.0337(10) 0.0155(9) 0.0296(10) -0.0037(8) 0.0125(9) -0.0031(8) C17 0.0300(10) 0.0174(9) 0.0318(11) 0.0019(8) 0.0093(9) 0.0032(8) C18 0.0232(9) 0.0203(9) 0.0256(10) 0.0015(8) 0.0027(8) 0.0010(8) C19 0.0193(8) 0.0201(9) 0.0330(11) -0.0031(8) 0.0020(8) -0.0033(7) C20 0.0276(9) 0.0137(9) 0.0288(10) -0.0019(8) 0.0050(8) 0.0033(7) C21 0.0389(12) 0.0191(10) 0.0382(12) -0.0002(9) 0.0133(10) -0.0018(9) C22 0.0619(16) 0.0246(11) 0.0320(12) 0.0044(9) 0.0158(12) -0.0010(11) C23 0.0658(16) 0.0269(11) 0.0241(11) 0.0024(9) -0.0002(11) 0.0056(11) C24 0.0381(11) 0.0225(10) 0.0267(10) -0.0019(8) -0.0036(9) 0.0050(9) N1 0.0188(7) 0.0188(7) 0.0209(8) -0.0023(6) 0.0001(6) 0.0016(6) N2 0.0212(7) 0.0184(8) 0.0233(8) -0.0029(6) 0.0024(6) 0.0019(6) N3 0.0191(7) 0.0167(7) 0.0231(8) -0.0016(6) 0.0019(6) -0.0015(6) N4 0.0259(8) 0.0160(7) 0.0227(8) -0.0009(6) -0.0001(7) 0.0029(6) N5 0.0239(8) 0.0247(9) 0.0295(9) -0.0063(7) -0.0036(7) -0.0022(7) O1 0.0374(13) 0.0536(16) 0.101(3) 0.0209(16) -0.0211(14) -0.0192(11) N5' 0.0239(8) 0.0247(9) 0.0295(9) -0.0063(7) -0.0036(7) -0.0022(7) O1' 0.058(11) 0.068(14) 0.061(13) -0.014(11) -0.001(10) -0.006(10) B1 0.045(3) 0.032(3) 0.028(2) -0.008(2) -0.001(2) 0.003(2) F1 0.0512(18) 0.0600(19) 0.089(3) 0.0249(18) 0.0290(18) 0.0248(15) F2 0.038(2) 0.138(5) 0.049(3) -0.011(3) 0.010(2) 0.038(2) F3 0.143(5) 0.035(2) 0.076(3) 0.0156(19) -0.071(3) -0.023(3) F4 0.091(3) 0.055(2) 0.0258(13) -0.0045(12) -0.0061(14) -0.025(2) B1' 0.045(4) 0.024(4) 0.032(4) -0.004(3) 0.008(3) -0.004(3) F1' 0.032(2) 0.035(3) 0.042(3) 0.003(2) -0.009(2) -0.0062(18) F2' 0.048(4) 0.048(3) 0.031(3) 0.018(2) 0.007(2) -0.002(3) F3' 0.057(3) 0.054(3) 0.033(2) 0.0174(19) -0.0122(19) -0.015(2) F4' 0.057(3) 0.056(3) 0.091(5) -0.038(3) 0.025(3) 0.002(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 N5 1.7327(18) . ? Fe1 N2 1.9909(17) . ? Fe1 N4 2.0085(17) . ? Fe1 N3 2.0297(16) . ? Fe1 N1 2.1300(16) . ? Fe1 S1 2.2962(5) . ? S1 C1 1.763(2) . ? C1 C2 1.399(3) . ? C1 C6 1.403(3) . ? C2 C3 1.383(4) . ? C2 H2 0.9500 . ? C3 C4 1.380(4) . ? C3 H3 0.9500 . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 C7 1.499(3) . ? C7 N1 1.491(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N1 1.493(2) . ? C8 C14 1.505(3) . ? C8 C9 1.513(3) . ? C8 H8 1.0000 . ? C9 N2 1.349(3) . ? C9 C10 1.384(3) . ? C10 C11 1.381(3) . ? C10 H10 0.9500 . ? C11 C12 1.386(4) . ? C11 H11 0.9500 . ? C12 C13 1.379(3) . ? C12 H12 0.9500 . ? C13 N2 1.346(3) . ? C13 H13 0.9500 . ? C14 N3 1.350(2) . ? C14 C15 1.380(3) . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 C17 1.377(3) . ? C16 H16 0.9500 . ? C17 C18 1.390(3) . ? C17 H17 0.9500 . ? C18 N3 1.336(3) . ? C18 H18 0.9500 . ? C19 N1 1.485(3) . ? C19 C20 1.500(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N4 1.350(3) . ? C20 C21 1.385(3) . ? C21 C22 1.381(4) . ? C21 H21 0.9500 . ? C22 C23 1.377(4) . ? C22 H22 0.9500 . ? C23 C24 1.380(3) . ? C23 H23 0.9500 . ? C24 N4 1.346(3) . ? C24 H24 0.9500 . ? N5 O1 1.150(3) . ? B1 F2 1.343(8) . ? B1 F1 1.372(8) . ? B1 F4 1.378(8) . ? B1 F3 1.383(12) . ? B1' F4' 1.363(11) . ? B1' F2' 1.368(11) . ? B1' F3' 1.423(12) . ? B1' F1' 1.424(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 N5 Fe1 N2 98.37(8) . . ? N5 Fe1 N4 100.46(8) . . ? N2 Fe1 N4 161.15(7) . . ? N5 Fe1 N3 96.47(7) . . ? N2 Fe1 N3 86.00(7) . . ? N4 Fe1 N3 92.70(6) . . ? N5 Fe1 N1 174.89(7) . . ? N2 Fe1 N1 80.32(6) . . ? N4 Fe1 N1 80.99(7) . . ? N3 Fe1 N1 78.53(6) . . ? N5 Fe1 S1 91.41(6) . . ? N2 Fe1 S1 88.28(5) . . ? N4 Fe1 S1 90.40(5) . . ? N3 Fe1 S1 170.86(5) . . ? N1 Fe1 S1 93.48(5) . . ? C1 S1 Fe1 106.42(7) . . ? C2 C1 C6 119.0(2) . . ? C2 C1 S1 118.81(18) . . ? C6 C1 S1 122.13(16) . . ? C3 C2 C1 120.6(2) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 120.4(2) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.8(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 119.6(2) . . ? C5 C6 C7 119.8(2) . . ? C1 C6 C7 120.53(18) . . ? N1 C7 C6 113.55(16) . . ? N1 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C14 107.51(15) . . ? N1 C8 C9 105.48(15) . . ? C14 C8 C9 106.64(16) . . ? N1 C8 H8 112.3 . . ? C14 C8 H8 112.3 . . ? C9 C8 H8 112.3 . . ? N2 C9 C10 122.30(19) . . ? N2 C9 C8 112.66(17) . . ? C10 C9 C8 125.03(19) . . ? C11 C10 C9 118.4(2) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C10 C11 C12 119.3(2) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 119.7(2) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? N2 C13 C12 121.2(2) . . ? N2 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? N3 C14 C15 122.83(18) . . ? N3 C14 C8 112.22(16) . . ? C15 C14 C8 124.84(18) . . ? C14 C15 C16 117.93(19) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? C17 C16 C15 119.70(19) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 119.00(19) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? N3 C18 C17 121.88(19) . . ? N3 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? N1 C19 C20 109.50(16) . . ? N1 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? N1 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? N4 C20 C21 121.6(2) . . ? N4 C20 C19 116.37(17) . . ? C21 C20 C19 122.01(19) . . ? C22 C21 C20 119.1(2) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C23 C22 C21 119.4(2) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 119.1(2) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? N4 C24 C23 122.0(2) . . ? N4 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C19 N1 C7 111.03(15) . . ? C19 N1 C8 114.30(15) . . ? C7 N1 C8 109.95(15) . . ? C19 N1 Fe1 107.89(12) . . ? C7 N1 Fe1 116.18(12) . . ? C8 N1 Fe1 96.93(11) . . ? C13 N2 C9 119.16(18) . . ? C13 N2 Fe1 127.47(14) . . ? C9 N2 Fe1 112.72(13) . . ? C18 N3 C14 118.65(17) . . ? C18 N3 Fe1 128.48(14) . . ? C14 N3 Fe1 112.71(13) . . ? C24 N4 C20 118.89(18) . . ? C24 N4 Fe1 124.65(14) . . ? C20 N4 Fe1 115.89(13) . . ? O1 N5 Fe1 147.2(2) . . ? F2 B1 F1 108.7(7) . . ? F2 B1 F4 111.8(7) . . ? F1 B1 F4 109.4(7) . . ? F2 B1 F3 109.9(8) . . ? F1 B1 F3 113.7(7) . . ? F4 B1 F3 103.3(7) . . ? F4' B1' F2' 110.8(10) . . ? F4' B1' F3' 104.9(9) . . ? F2' B1' F3' 105.6(9) . . ? F4' B1' F1' 108.5(9) . . ? F2' B1' F1' 109.3(10) . . ? F3' B1' F1' 117.6(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Fe1 S1 C1 -149.16(10) . . . . ? N2 Fe1 S1 C1 112.51(9) . . . . ? N4 Fe1 S1 C1 -48.68(9) . . . . ? N1 Fe1 S1 C1 32.31(9) . . . . ? Fe1 S1 C1 C2 137.41(16) . . . . ? Fe1 S1 C1 C6 -45.55(18) . . . . ? C6 C1 C2 C3 -1.9(3) . . . . ? S1 C1 C2 C3 175.19(17) . . . . ? C1 C2 C3 C4 1.0(3) . . . . ? C2 C3 C4 C5 0.8(4) . . . . ? C3 C4 C5 C6 -1.7(3) . . . . ? C4 C5 C6 C1 0.8(3) . . . . ? C4 C5 C6 C7 -174.7(2) . . . . ? C2 C1 C6 C5 1.0(3) . . . . ? S1 C1 C6 C5 -176.02(16) . . . . ? C2 C1 C6 C7 176.53(19) . . . . ? S1 C1 C6 C7 -0.5(3) . . . . ? C5 C6 C7 N1 -118.8(2) . . . . ? C1 C6 C7 N1 65.7(2) . . . . ? N1 C8 C9 N2 46.7(2) . . . . ? C14 C8 C9 N2 -67.4(2) . . . . ? N1 C8 C9 C10 -132.52(19) . . . . ? C14 C8 C9 C10 113.4(2) . . . . ? N2 C9 C10 C11 -0.4(3) . . . . ? C8 C9 C10 C11 178.79(18) . . . . ? C9 C10 C11 C12 0.4(3) . . . . ? C10 C11 C12 C13 -0.4(3) . . . . ? C11 C12 C13 N2 0.3(3) . . . . ? N1 C8 C14 N3 -40.0(2) . . . . ? C9 C8 C14 N3 72.8(2) . . . . ? N1 C8 C14 C15 143.72(19) . . . . ? C9 C8 C14 C15 -103.5(2) . . . . ? N3 C14 C15 C16 0.9(3) . . . . ? C8 C14 C15 C16 176.85(18) . . . . ? C14 C15 C16 C17 0.0(3) . . . . ? C15 C16 C17 C18 -0.7(3) . . . . ? C16 C17 C18 N3 0.5(3) . . . . ? N1 C19 C20 N4 -30.2(2) . . . . ? N1 C19 C20 C21 152.60(18) . . . . ? N4 C20 C21 C22 -0.5(3) . . . . ? C19 C20 C21 C22 176.6(2) . . . . ? C20 C21 C22 C23 -0.1(3) . . . . ? C21 C22 C23 C24 0.5(3) . . . . ? C22 C23 C24 N4 -0.3(3) . . . . ? C20 C19 N1 C7 -96.29(18) . . . . ? C20 C19 N1 C8 138.63(16) . . . . ? C20 C19 N1 Fe1 32.08(17) . . . . ? C6 C7 N1 C19 57.9(2) . . . . ? C6 C7 N1 C8 -174.59(16) . . . . ? C6 C7 N1 Fe1 -65.84(19) . . . . ? C14 C8 N1 C19 -56.5(2) . . . . ? C9 C8 N1 C19 -170.02(15) . . . . ? C14 C8 N1 C7 177.85(15) . . . . ? C9 C8 N1 C7 64.34(19) . . . . ? C14 C8 N1 Fe1 56.73(15) . . . . ? C9 C8 N1 Fe1 -56.79(14) . . . . ? N2 Fe1 N1 C19 161.15(13) . . . . ? N4 Fe1 N1 C19 -21.34(12) . . . . ? N3 Fe1 N1 C19 73.30(12) . . . . ? S1 Fe1 N1 C19 -111.19(11) . . . . ? N2 Fe1 N1 C7 -73.48(13) . . . . ? N4 Fe1 N1 C7 104.03(14) . . . . ? N3 Fe1 N1 C7 -161.33(14) . . . . ? S1 Fe1 N1 C7 14.18(13) . . . . ? N2 Fe1 N1 C8 42.79(11) . . . . ? N4 Fe1 N1 C8 -139.69(12) . . . . ? N3 Fe1 N1 C8 -45.05(11) . . . . ? S1 Fe1 N1 C8 130.45(10) . . . . ? C12 C13 N2 C9 -0.2(3) . . . . ? C12 C13 N2 Fe1 -170.30(15) . . . . ? C10 C9 N2 C13 0.3(3) . . . . ? C8 C9 N2 C13 -178.99(16) . . . . ? C10 C9 N2 Fe1 171.75(15) . . . . ? C8 C9 N2 Fe1 -7.50(19) . . . . ? N5 Fe1 N2 C13 -35.56(17) . . . . ? N4 Fe1 N2 C13 141.8(2) . . . . ? N3 Fe1 N2 C13 -131.52(17) . . . . ? N1 Fe1 N2 C13 149.45(17) . . . . ? S1 Fe1 N2 C13 55.62(16) . . . . ? N5 Fe1 N2 C9 153.82(14) . . . . ? N4 Fe1 N2 C9 -28.8(3) . . . . ? N3 Fe1 N2 C9 57.85(13) . . . . ? N1 Fe1 N2 C9 -21.18(13) . . . . ? S1 Fe1 N2 C9 -115.01(13) . . . . ? C17 C18 N3 C14 0.3(3) . . . . ? C17 C18 N3 Fe1 -174.59(14) . . . . ? C15 C14 N3 C18 -1.1(3) . . . . ? C8 C14 N3 C18 -177.50(16) . . . . ? C15 C14 N3 Fe1 174.60(15) . . . . ? C8 C14 N3 Fe1 -1.8(2) . . . . ? N5 Fe1 N3 C18 24.39(18) . . . . ? N2 Fe1 N3 C18 122.37(17) . . . . ? N4 Fe1 N3 C18 -76.46(17) . . . . ? N1 Fe1 N3 C18 -156.70(17) . . . . ? N5 Fe1 N3 C14 -150.79(14) . . . . ? N2 Fe1 N3 C14 -52.81(13) . . . . ? N4 Fe1 N3 C14 108.36(14) . . . . ? N1 Fe1 N3 C14 28.12(13) . . . . ? C23 C24 N4 C20 -0.4(3) . . . . ? C23 C24 N4 Fe1 170.54(16) . . . . ? C21 C20 N4 C24 0.8(3) . . . . ? C19 C20 N4 C24 -176.49(17) . . . . ? C21 C20 N4 Fe1 -170.91(15) . . . . ? C19 C20 N4 Fe1 11.8(2) . . . . ? N5 Fe1 N4 C24 19.60(17) . . . . ? N2 Fe1 N4 C24 -157.77(19) . . . . ? N3 Fe1 N4 C24 116.69(16) . . . . ? N1 Fe1 N4 C24 -165.37(17) . . . . ? S1 Fe1 N4 C24 -71.91(16) . . . . ? N5 Fe1 N4 C20 -169.26(14) . . . . ? N2 Fe1 N4 C20 13.4(3) . . . . ? N3 Fe1 N4 C20 -72.16(14) . . . . ? N1 Fe1 N4 C20 5.77(13) . . . . ? S1 Fe1 N4 C20 99.23(13) . . . . ? N2 Fe1 N5 O1 27.6(5) . . . . ? N4 Fe1 N5 O1 -151.6(5) . . . . ? N3 Fe1 N5 O1 114.5(5) . . . . ? S1 Fe1 N5 O1 -60.9(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.746 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.065 _iucr_refine_instructions_details ; TITL x0920a - SHELXL CELL 0.71073 11.65041 14.6344 28.0712 90.000 90.000 90.000 ZERR 8 0.00018 0.0002 0.0005 0.000 0.000 0.000 LATT 1 SYMM 0.50000 - X , - Y , 0.50000 + Z SYMM 0.50000 + X , 0.50000 - Y , - Z SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H B F FE N O S UNIT 192 168 8 32 8 40 8 8 TEMP -163 ACTA HTAB BOND BOND $H CONF WPDB L.S. 6 FMAP 2 PLAN 10 OMIT -2 55 WGHT 0.044100 4.549900 FVAR 2.57901 0.59738 0.88557 PART 0 rem Fe complex FE1 5 0.871737 0.161495 0.128962 11.00000 0.01880 0.01570 = 0.02069 -0.00117 -0.00045 0.00043 S1 8 0.811124 0.297433 0.161148 11.00000 0.02958 0.01731 = 0.02456 -0.00269 0.00059 0.00108 C1 1 0.666152 0.281774 0.177207 11.00000 0.03043 0.01610 = 0.02702 0.00307 0.00621 0.00682 C2 1 0.627986 0.316218 0.220911 11.00000 0.04816 0.02017 = 0.03045 -0.00156 0.00788 0.00674 AFIX 43 H2 2 0.681386 0.343182 0.242278 11.00000 -1.20000 AFIX 0 C3 1 0.513249 0.311391 0.233311 11.00000 0.05627 0.02508 = 0.03604 0.00110 0.02074 0.01257 AFIX 43 H3 2 0.488208 0.335938 0.262867 11.00000 -1.20000 AFIX 0 C4 1 0.434951 0.271114 0.202985 11.00000 0.03692 0.02969 = 0.05201 0.00907 0.02159 0.01153 AFIX 43 H4 2 0.356067 0.268651 0.211460 11.00000 -1.20000 AFIX 0 C5 1 0.471709 0.234224 0.160087 11.00000 0.02829 0.02599 = 0.04049 0.00710 0.00663 0.00596 AFIX 43 H5 2 0.418025 0.205022 0.139663 11.00000 -1.20000 AFIX 0 C6 1 0.586837 0.239639 0.146680 11.00000 0.02762 0.01983 = 0.02654 0.00479 0.00493 0.00753 C7 1 0.623100 0.206639 0.098409 11.00000 0.02050 0.02637 = 0.02382 -0.00009 -0.00189 0.00608 AFIX 23 H7A 2 0.554248 0.186307 0.080664 11.00000 -1.20000 H7B 2 0.657503 0.258276 0.080653 11.00000 -1.20000 AFIX 0 C8 1 0.747157 0.107528 0.050881 11.00000 0.02073 0.02575 = 0.02056 -0.00710 -0.00318 0.00109 AFIX 13 H8 2 0.682203 0.090443 0.029364 11.00000 -1.20000 AFIX 0 C9 1 0.810333 0.191609 0.033684 11.00000 0.02189 0.02225 = 0.02129 -0.00360 0.00142 0.00656 C10 1 0.794650 0.232789 -0.010223 11.00000 0.03038 0.03477 = 0.02144 -0.00217 0.00394 0.01231 AFIX 43 H10 2 0.742104 0.208218 -0.032708 11.00000 -1.20000 AFIX 0 C11 1 0.857200 0.310437 -0.020563 11.00000 0.03976 0.03554 = 0.02459 0.00699 0.01469 0.01686 AFIX 43 H11 2 0.847948 0.340460 -0.050322 11.00000 -1.20000 AFIX 0 C12 1 0.933628 0.344083 0.012955 11.00000 0.03606 0.02441 = 0.03742 0.00350 0.01881 0.00418 AFIX 43 H12 2 0.977533 0.397246 0.006239 11.00000 -1.20000 AFIX 0 C13 1 0.945670 0.300041 0.056115 11.00000 0.02587 0.02106 = 0.03138 -0.00332 0.00840 0.00060 AFIX 43 H13 2 0.997929 0.323493 0.079037 11.00000 -1.20000 AFIX 0 C14 1 0.835035 0.032553 0.054989 11.00000 0.02031 0.01843 = 0.02338 -0.00323 0.00118 -0.00311 C15 1 0.848065 -0.038129 0.022899 11.00000 0.02700 0.02052 = 0.02625 -0.00531 0.00439 -0.00804 AFIX 43 H15 2 0.797718 -0.044542 -0.003511 11.00000 -1.20000 AFIX 0 C16 1 0.937023 -0.099563 0.030410 11.00000 0.03368 0.01554 = 0.02958 -0.00366 0.01252 -0.00310 AFIX 43 H16 2 0.948487 -0.149013 0.009008 11.00000 -1.20000 AFIX 0 C17 1 1.008562 -0.088500 0.069017 11.00000 0.03002 0.01739 = 0.03179 0.00191 0.00934 0.00319 AFIX 43 H17 2 1.069211 -0.130476 0.074749 11.00000 -1.20000 AFIX 0 C18 1 0.990714 -0.014993 0.099482 11.00000 0.02321 0.02028 = 0.02559 0.00153 0.00268 0.00099 AFIX 43 H18 2 1.040448 -0.006998 0.125975 11.00000 -1.20000 AFIX 0 C19 1 0.660341 0.050947 0.126888 11.00000 0.01934 0.02006 = 0.03303 -0.00310 0.00202 -0.00329 AFIX 23 H19A 2 0.685595 -0.006789 0.111790 11.00000 -1.20000 H19B 2 0.575411 0.052806 0.126259 11.00000 -1.20000 AFIX 0 C20 1 0.701870 0.054450 0.177442 11.00000 0.02762 0.01367 = 0.02876 -0.00191 0.00502 0.00331 C21 1 0.639804 0.016493 0.214588 11.00000 0.03888 0.01910 = 0.03815 -0.00017 0.01333 -0.00185 AFIX 43 H21 2 0.566639 -0.010052 0.208954 11.00000 -1.20000 AFIX 0 C22 1 0.685787 0.017783 0.259934 11.00000 0.06194 0.02462 = 0.03202 0.00441 0.01578 -0.00096 AFIX 43 H22 2 0.644467 -0.007793 0.285885 11.00000 -1.20000 AFIX 0 C23 1 0.792065 0.056483 0.267169 11.00000 0.06579 0.02694 = 0.02409 0.00241 -0.00020 0.00559 AFIX 43 H23 2 0.825218 0.057485 0.298083 11.00000 -1.20000 AFIX 0 C24 1 0.849775 0.093792 0.228913 11.00000 0.03806 0.02246 = 0.02666 -0.00194 -0.00358 0.00499 AFIX 43 H24 2 0.922953 0.120724 0.233991 11.00000 -1.20000 AFIX 0 N1 6 0.707372 0.130012 0.100071 11.00000 0.01881 0.01881 = 0.02090 -0.00231 0.00005 0.00164 N2 6 0.884691 0.224439 0.066317 11.00000 0.02119 0.01836 = 0.02333 -0.00290 0.00244 0.00187 N3 6 0.905632 0.044725 0.092572 11.00000 0.01914 0.01670 = 0.02314 -0.00158 0.00187 -0.00153 N4 6 0.805562 0.093199 0.184615 11.00000 0.02588 0.01600 = 0.02268 -0.00092 -0.00005 0.00292 EADP N5 N5' EXYZ N5 N5' SIMU 0.01 O1 O1' PART 1 N5 6 1.010455 0.179809 0.149074 31.00000 0.02390 0.02474 = 0.02950 -0.00631 -0.00362 -0.00216 O1 7 1.090759 0.225456 0.148021 31.00000 0.03738 0.05362 = 0.10083 0.02095 -0.02115 -0.01921 PART 2 SAME N5 > O1 N5' 6 1.010455 0.179809 0.149074 -31.00000 0.02390 0.02474 = 0.02950 -0.00631 -0.00362 -0.00216 O1' 7 1.076623 0.195646 0.177288 -31.00000 0.05784 0.06819 = 0.06094 -0.01366 -0.00105 -0.00628 DELU 0.005 B1 > F4' SIMU 0.01 B1 > F4' PART 1 B1 3 0.174911 0.469288 0.100365 21.00000 0.04537 0.03233 = 0.02773 -0.00803 -0.00136 0.00257 F1 4 0.248217 0.397851 0.109029 21.00000 0.05124 0.05998 = 0.08876 0.02487 0.02898 0.02477 F2 4 0.086987 0.464553 0.131208 21.00000 0.03834 0.13840 = 0.04923 -0.01144 0.00984 0.03844 F3 4 0.226787 0.554095 0.103343 21.00000 0.14338 0.03546 = 0.07626 0.01560 -0.07053 -0.02310 F4 4 0.137907 0.465444 0.053770 21.00000 0.09110 0.05520 = 0.02582 -0.00454 -0.00608 -0.02455 PART 2 SAME B1 > F4 B1' 3 0.153467 0.480809 0.097044 -21.00000 0.04519 0.02352 = 0.03166 -0.00377 0.00755 -0.00416 F1' 4 0.241217 0.543308 0.110687 -21.00000 0.03169 0.03542 = 0.04185 0.00279 -0.00948 -0.00619 F2' 4 0.096997 0.451096 0.136844 -21.00000 0.04763 0.04793 = 0.03066 0.01815 0.00670 -0.00203 F3' 4 0.066541 0.513103 0.065649 -21.00000 0.05662 0.05396 = 0.03307 0.01745 -0.01221 -0.01494 F4' 4 0.203125 0.409473 0.073615 -21.00000 0.05685 0.05563 = 0.09110 -0.03825 0.02457 0.00213 HKLF 4 REM x0920a - SHELXL REM R1 = 0.0364 for 4680 Fo > 4sig(Fo) and 0.0447 for all 5498 data REM 390 parameters refined using 163 restraints END WGHT 0.0441 4.5501 REM Highest difference peak 0.746, deepest hole -0.480, 1-sigma level 0.065 Q1 1 0.1235 0.5536 0.1128 11.00000 0.05 0.75 Q2 1 0.8354 0.3186 0.2007 11.00000 0.05 0.66 Q3 1 0.7678 0.3641 0.1202 11.00000 0.05 0.65 Q4 1 0.7456 0.2904 0.1590 11.00000 0.05 0.61 Q5 1 0.2547 0.4424 0.1308 11.00000 0.05 0.46 Q6 1 0.1941 0.3850 0.0992 11.00000 0.05 0.35 Q7 1 0.8789 0.3382 0.0010 11.00000 0.05 0.28 Q8 1 0.8145 0.2049 0.0090 11.00000 0.05 0.26 Q9 1 0.6157 0.2581 0.1701 11.00000 0.05 0.25 Q10 1 0.5351 0.2264 0.1512 11.00000 0.05 0.25 ;