data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C35 H28 Fe N5 O), 4(B F4), 3(C2 H3 N)' _chemical_formula_sum 'C76 H65 B4 F16 Fe2 N13 O2' _chemical_formula_weight 1651.35 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' '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' 'B' 'B' 0.0013 0.0007 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9067(3) _cell_length_b 12.4935(4) _cell_length_c 13.4579(4) _cell_angle_alpha 91.551(2) _cell_angle_beta 112.033(2) _cell_angle_gamma 104.801(2) _cell_volume 1777.21(9) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 12073 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 26.31 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.510 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.837 _exptl_absorpt_correction_T_max 0.967 _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 29272 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.25 _reflns_number_total 7168 _reflns_number_gt 6218 _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^)+(0.0506P)^2^+1.0614P] 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 7168 _refine_ls_number_parameters 605 _refine_ls_number_restraints 328 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0997 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.088 _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 0.12224(2) 0.24109(2) 0.250446(19) 0.01533(8) Uani 1 1 d . . . C1 C 0.38186(17) 0.22218(16) 0.34930(15) 0.0212(4) Uani 1 1 d . . . H1 H 0.3897 0.2409 0.2838 0.025 Uiso 1 1 calc R . . C2 C 0.48007(18) 0.19623(17) 0.42850(17) 0.0271(4) Uani 1 1 d . . . H2 H 0.5546 0.1963 0.4179 0.033 Uiso 1 1 calc R . . C3 C 0.46846(18) 0.16993(17) 0.52424(16) 0.0263(4) Uani 1 1 d . . . H3 H 0.5350 0.1512 0.5799 0.032 Uiso 1 1 calc R . . C4 C 0.35967(18) 0.17101(16) 0.53832(15) 0.0238(4) Uani 1 1 d . . . H4 H 0.3510 0.1545 0.6040 0.029 Uiso 1 1 calc R . . C5 C 0.26333(17) 0.19666(15) 0.45491(14) 0.0183(4) Uani 1 1 d . . . C6 C 0.13864(18) 0.19272(16) 0.46162(15) 0.0207(4) Uani 1 1 d . . . H6A H 0.0945 0.1148 0.4644 0.025 Uiso 1 1 calc R . . H6B H 0.1542 0.2391 0.5289 0.025 Uiso 1 1 calc R . . C7 C 0.04218(18) 0.34604(15) 0.39465(15) 0.0211(4) Uani 1 1 d . . . H7A H -0.0469 0.3461 0.3563 0.025 Uiso 1 1 calc R . . H7B H 0.0643 0.3594 0.4734 0.025 Uiso 1 1 calc R . . C8 C 0.12646(17) 0.43691(16) 0.36362(14) 0.0197(4) Uani 1 1 d . . . C9 C 0.15073(18) 0.54896(17) 0.39805(16) 0.0248(4) Uani 1 1 d . . . H9 H 0.1136 0.5711 0.4435 0.030 Uiso 1 1 calc R . . C10 C 0.22935(19) 0.62812(17) 0.36569(17) 0.0270(4) Uani 1 1 d . . . H10 H 0.2450 0.7055 0.3866 0.032 Uiso 1 1 calc R . . C11 C 0.28535(19) 0.59294(17) 0.30194(16) 0.0265(4) Uani 1 1 d . . . H11 H 0.3426 0.6458 0.2811 0.032 Uiso 1 1 calc R . . C12 C 0.25668(17) 0.48043(16) 0.26939(15) 0.0220(4) Uani 1 1 d . . . H12 H 0.2950 0.4566 0.2258 0.026 Uiso 1 1 calc R . . C13 C -0.07041(17) 0.15190(16) 0.30059(15) 0.0208(4) Uani 1 1 d . . . H13 H -0.1259 0.1361 0.3420 0.025 Uiso 1 1 calc R . . C14 C -0.04245(17) 0.04866(15) 0.26831(14) 0.0196(4) Uani 1 1 d . . . C15 C -0.10435(19) -0.05741(16) 0.27713(15) 0.0245(4) Uani 1 1 d . . . H15 H -0.1702 -0.0698 0.3028 0.029 Uiso 1 1 calc R . . C16 C -0.0677(2) -0.14567(17) 0.24742(16) 0.0272(4) Uani 1 1 d . . . H16 H -0.1079 -0.2203 0.2525 0.033 Uiso 1 1 calc R . . C17 C 0.02791(19) -0.12329(16) 0.21041(15) 0.0243(4) Uani 1 1 d . . . H17 H 0.0542 -0.1833 0.1905 0.029 Uiso 1 1 calc R . . C18 C 0.08704(17) -0.01443(15) 0.20157(14) 0.0198(4) Uani 1 1 d . . . C19 C 0.18950(18) 0.00468(15) 0.16070(15) 0.0207(4) Uani 1 1 d . . . C20 C 0.2971(2) -0.02787(17) 0.21768(16) 0.0277(4) Uani 1 1 d . . . H20 H 0.3042 -0.0606 0.2819 0.033 Uiso 1 1 calc R . . C21 C 0.3942(2) -0.0129(2) 0.18138(18) 0.0359(5) Uani 1 1 d . . . H21 H 0.4683 -0.0336 0.2215 0.043 Uiso 1 1 calc R . . C22 C 0.3826(2) 0.03225(19) 0.08650(18) 0.0336(5) Uani 1 1 d . . . H22 H 0.4489 0.0425 0.0615 0.040 Uiso 1 1 calc R . . C23 C 0.2748(2) 0.06253(17) 0.02783(16) 0.0279(4) Uani 1 1 d . . . H23 H 0.2670 0.0928 -0.0377 0.034 Uiso 1 1 calc R . . C24 C 0.17844(18) 0.04877(16) 0.06449(15) 0.0218(4) Uani 1 1 d . . . H24 H 0.1045 0.0694 0.0239 0.026 Uiso 1 1 calc R . . C25 C -0.12858(18) 0.20047(16) 0.19873(16) 0.0227(4) Uani 1 1 d . . . C26 C -0.25428(19) 0.19513(19) 0.14901(18) 0.0316(5) Uani 1 1 d . . . H26 H -0.3124 0.1652 0.1809 0.038 Uiso 1 1 calc R . . C27 C -0.2929(2) 0.2354(2) 0.04977(19) 0.0380(5) Uani 1 1 d . . . H27 H -0.3791 0.2330 0.0126 0.046 Uiso 1 1 calc R . . C28 C -0.2073(2) 0.27849(19) 0.00564(17) 0.0315(5) Uani 1 1 d . . . H28 H -0.2350 0.3045 -0.0626 0.038 Uiso 1 1 calc R . . C29 C -0.07858(18) 0.28468(15) 0.06023(15) 0.0225(4) Uani 1 1 d . . . C30 C 0.01806(19) 0.32763(15) 0.01744(15) 0.0220(4) Uani 1 1 d . . . C31 C -0.0093(2) 0.38779(16) -0.07159(16) 0.0277(4) Uani 1 1 d . . . H31 H -0.0884 0.4037 -0.0993 0.033 Uiso 1 1 calc R . . C32 C 0.0741(2) 0.42420(17) -0.11966(16) 0.0318(5) Uani 1 1 d . . . H32 H 0.0528 0.4654 -0.1789 0.038 Uiso 1 1 calc R . . C33 C 0.1895(2) 0.40073(17) -0.08159(17) 0.0314(5) Uani 1 1 d . . . H33 H 0.2465 0.4240 -0.1160 0.038 Uiso 1 1 calc R . . C34 C 0.2215(2) 0.34337(16) 0.00653(16) 0.0257(4) Uani 1 1 d . . . H34 H 0.3008 0.3276 0.0322 0.031 Uiso 1 1 calc R . . C35 C 0.13887(18) 0.30815(15) 0.05856(14) 0.0199(4) Uani 1 1 d . . . N1 N 0.27495(14) 0.22187(12) 0.36193(12) 0.0171(3) Uani 1 1 d . . . N2 N 0.05661(14) 0.23486(12) 0.36596(12) 0.0175(3) Uani 1 1 d . . . N3 N 0.17613(14) 0.40310(13) 0.29732(12) 0.0180(3) Uani 1 1 d . . . N4 N 0.05101(14) 0.07185(12) 0.23071(12) 0.0175(3) Uani 1 1 d . . . N5 N -0.04341(14) 0.24571(13) 0.15647(12) 0.0192(3) Uani 1 1 d . . . O1 O 0.18336(12) 0.25745(11) 0.14540(10) 0.0191(3) Uani 1 1 d . . . B1 B 0.2113(11) 0.8814(10) 0.5146(9) 0.0260(8) Uani 0.56(2) 1 d PDU A 1 F1 F 0.1412(13) 0.7714(6) 0.5020(10) 0.0497(19) Uani 0.56(2) 1 d PDU A 1 F2 F 0.266(2) 0.897(2) 0.4393(14) 0.030(3) Uani 0.56(2) 1 d PDU A 1 F3 F 0.1316(15) 0.9487(12) 0.5010(15) 0.032(2) Uani 0.56(2) 1 d PDU A 1 F4 F 0.3050(5) 0.9098(11) 0.6191(4) 0.0423(16) Uani 0.56(2) 1 d PDU A 1 B1' B 0.2015(14) 0.8691(13) 0.5094(11) 0.0260(8) Uani 0.44(2) 1 d PDU A 2 F1' F 0.1015(10) 0.7707(9) 0.4674(11) 0.0406(18) Uani 0.44(2) 1 d PDU A 2 F2' F 0.268(3) 0.887(3) 0.4430(18) 0.028(2) Uani 0.44(2) 1 d PDU A 2 F3' F 0.1521(19) 0.9564(14) 0.5171(19) 0.030(2) Uani 0.44(2) 1 d PDU A 2 F4' F 0.2803(12) 0.8554(16) 0.6107(7) 0.047(2) Uani 0.44(2) 1 d PDU A 2 B2 B 0.5540(11) 0.6933(9) 0.1795(10) 0.039(3) Uani 0.369(5) 1 d PDU B 1 F5 F 0.5758(13) 0.7072(11) 0.0866(9) 0.062(3) Uani 0.369(5) 1 d PDU B 1 F6 F 0.6644(11) 0.6907(14) 0.2636(12) 0.042(3) Uani 0.369(5) 1 d PDU B 1 F7 F 0.5073(6) 0.7740(5) 0.2052(4) 0.063(2) Uani 0.369(5) 1 d PDU B 1 F8 F 0.4637(5) 0.5920(5) 0.1657(5) 0.0735(18) Uani 0.369(5) 1 d PDU B 1 B2' B 0.5731(6) 0.7252(6) 0.1699(6) 0.0393(16) Uani 0.631(5) 1 d PDU B 2 F5' F 0.5561(8) 0.6770(7) 0.0707(6) 0.0590(17) Uani 0.631(5) 1 d PDU B 2 F6' F 0.6773(7) 0.7082(8) 0.2517(7) 0.0413(16) Uani 0.631(5) 1 d PDU B 2 F7' F 0.4658(2) 0.6852(4) 0.1868(2) 0.0747(15) Uani 0.631(5) 1 d PDU B 2 F8' F 0.5941(3) 0.8400(3) 0.1696(3) 0.0769(13) Uani 0.631(5) 1 d PDU B 2 C1S C -0.4164(3) 0.4165(5) 0.2018(4) 0.117(2) Uani 1 1 d . C 2 H1S1 H -0.4577 0.4721 0.2116 0.176 Uiso 1 1 calc R C 2 H1S2 H -0.4589 0.3440 0.2158 0.176 Uiso 1 1 calc R C 2 H1S3 H -0.4213 0.4102 0.1274 0.176 Uiso 1 1 calc R C 2 C2S C -0.2837(3) 0.4514(3) 0.2774(2) 0.0539(7) Uani 1 1 d . C 2 N1S N -0.1814(2) 0.4783(2) 0.33470(19) 0.0518(6) Uani 1 1 d . C 2 C3S C 0.575(3) 0.523(4) 0.434(3) 0.075(2) Uani 0.50 1 d PDU D -1 H3S1 H 0.6206 0.4669 0.4416 0.112 Uiso 0.50 1 calc PR D -1 H3S2 H 0.6350 0.5972 0.4642 0.112 Uiso 0.50 1 calc PR D -1 H3S3 H 0.5238 0.5223 0.3574 0.112 Uiso 0.50 1 calc PR D -1 C4S C 0.488(2) 0.496(3) 0.495(2) 0.060(2) Uani 0.50 1 d PDU D -1 N2S N 0.431(2) 0.481(3) 0.545(2) 0.075(2) Uani 0.50 1 d PDU D -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 0.01609(14) 0.01709(14) 0.01398(13) 0.00058(9) 0.00658(10) 0.00590(10) C1 0.0191(9) 0.0234(9) 0.0220(9) -0.0004(7) 0.0094(8) 0.0061(7) C2 0.0189(9) 0.0305(11) 0.0296(11) -0.0014(8) 0.0070(8) 0.0080(8) C3 0.0206(9) 0.0280(10) 0.0244(10) 0.0030(8) 0.0013(8) 0.0085(8) C4 0.0249(10) 0.0243(10) 0.0185(9) 0.0021(7) 0.0052(8) 0.0060(8) C5 0.0213(9) 0.0161(8) 0.0175(9) -0.0002(7) 0.0076(7) 0.0054(7) C6 0.0245(9) 0.0250(9) 0.0162(9) 0.0045(7) 0.0096(7) 0.0105(8) C7 0.0245(9) 0.0215(9) 0.0236(9) 0.0016(7) 0.0141(8) 0.0100(8) C8 0.0191(9) 0.0244(9) 0.0174(9) 0.0004(7) 0.0068(7) 0.0097(7) C9 0.0262(10) 0.0252(10) 0.0255(10) -0.0028(8) 0.0121(8) 0.0094(8) C10 0.0293(10) 0.0204(10) 0.0298(11) -0.0043(8) 0.0114(9) 0.0057(8) C11 0.0262(10) 0.0228(10) 0.0294(11) -0.0003(8) 0.0136(9) 0.0016(8) C12 0.0206(9) 0.0248(10) 0.0206(9) -0.0004(7) 0.0094(8) 0.0051(8) C13 0.0173(9) 0.0232(9) 0.0228(9) 0.0017(7) 0.0100(7) 0.0040(7) C14 0.0195(9) 0.0219(9) 0.0158(8) 0.0013(7) 0.0060(7) 0.0049(7) C15 0.0247(10) 0.0248(10) 0.0210(9) 0.0012(8) 0.0094(8) 0.0015(8) C16 0.0350(11) 0.0204(10) 0.0210(10) 0.0005(8) 0.0100(9) 0.0013(8) C17 0.0338(11) 0.0199(9) 0.0175(9) -0.0008(7) 0.0089(8) 0.0074(8) C18 0.0237(9) 0.0206(9) 0.0133(8) -0.0005(7) 0.0046(7) 0.0076(7) C19 0.0250(9) 0.0181(9) 0.0172(9) -0.0037(7) 0.0066(8) 0.0067(7) C20 0.0331(11) 0.0310(11) 0.0224(10) 0.0015(8) 0.0098(9) 0.0169(9) C21 0.0322(11) 0.0456(13) 0.0331(12) -0.0027(10) 0.0105(10) 0.0212(10) C22 0.0305(11) 0.0404(12) 0.0338(12) -0.0066(9) 0.0181(10) 0.0094(9) C23 0.0342(11) 0.0297(11) 0.0206(10) -0.0027(8) 0.0136(9) 0.0067(9) C24 0.0244(9) 0.0211(9) 0.0179(9) -0.0022(7) 0.0072(8) 0.0056(8) C25 0.0209(9) 0.0224(9) 0.0252(10) 0.0012(8) 0.0093(8) 0.0071(8) C26 0.0206(10) 0.0376(12) 0.0356(12) 0.0048(9) 0.0094(9) 0.0089(9) C27 0.0201(10) 0.0475(14) 0.0389(13) 0.0067(11) 0.0017(9) 0.0123(10) C28 0.0291(11) 0.0350(12) 0.0244(10) 0.0052(9) 0.0012(9) 0.0133(9) C29 0.0261(10) 0.0190(9) 0.0195(9) -0.0012(7) 0.0049(8) 0.0083(8) C30 0.0302(10) 0.0174(9) 0.0163(9) -0.0008(7) 0.0066(8) 0.0079(8) C31 0.0404(12) 0.0223(10) 0.0194(9) 0.0014(8) 0.0076(9) 0.0141(9) C32 0.0539(14) 0.0215(10) 0.0209(10) 0.0066(8) 0.0146(10) 0.0125(10) C33 0.0482(13) 0.0245(10) 0.0250(10) 0.0037(8) 0.0213(10) 0.0058(9) C34 0.0331(11) 0.0236(10) 0.0225(10) 0.0017(8) 0.0142(9) 0.0072(8) C35 0.0295(10) 0.0150(8) 0.0155(8) -0.0004(7) 0.0097(8) 0.0060(7) N1 0.0173(7) 0.0170(7) 0.0171(7) -0.0012(6) 0.0066(6) 0.0054(6) N2 0.0178(7) 0.0188(8) 0.0182(7) 0.0015(6) 0.0080(6) 0.0077(6) N3 0.0170(7) 0.0205(8) 0.0164(7) -0.0005(6) 0.0064(6) 0.0060(6) N4 0.0176(7) 0.0193(8) 0.0132(7) 0.0006(6) 0.0041(6) 0.0045(6) N5 0.0202(8) 0.0188(8) 0.0184(8) 0.0001(6) 0.0063(6) 0.0076(6) O1 0.0226(6) 0.0213(6) 0.0169(6) 0.0029(5) 0.0098(5) 0.0089(5) B1 0.0341(17) 0.027(2) 0.0282(14) 0.0077(14) 0.0198(12) 0.0154(15) F1 0.085(5) 0.0218(16) 0.067(4) 0.002(2) 0.061(4) 0.009(3) F2 0.041(4) 0.032(5) 0.027(3) 0.004(3) 0.023(3) 0.013(3) F3 0.030(4) 0.036(4) 0.037(4) 0.006(2) 0.013(3) 0.018(3) F4 0.0279(17) 0.078(5) 0.0239(14) 0.011(2) 0.0105(12) 0.020(2) B1' 0.0341(17) 0.027(2) 0.0282(14) 0.0077(14) 0.0198(12) 0.0154(15) F1' 0.050(4) 0.025(2) 0.062(5) 0.007(3) 0.040(3) 0.007(2) F2' 0.038(4) 0.025(4) 0.033(4) 0.010(3) 0.025(3) 0.013(3) F3' 0.033(6) 0.022(3) 0.044(6) 0.005(3) 0.023(5) 0.013(3) F4' 0.045(3) 0.086(6) 0.035(2) 0.025(3) 0.025(2) 0.043(4) B2 0.042(5) 0.062(5) 0.024(4) 0.003(4) 0.016(3) 0.030(4) F5 0.040(4) 0.120(8) 0.026(4) 0.009(4) 0.017(3) 0.016(5) F6 0.035(4) 0.063(5) 0.037(4) 0.018(3) 0.017(3) 0.026(4) F7 0.080(4) 0.071(3) 0.036(2) -0.006(2) -0.002(2) 0.059(3) F8 0.050(3) 0.064(4) 0.097(4) -0.007(3) 0.036(3) -0.009(3) B2' 0.026(2) 0.072(4) 0.024(2) 0.004(3) 0.0091(18) 0.023(3) F5' 0.054(3) 0.096(3) 0.028(2) -0.0116(19) 0.010(2) 0.034(3) F6' 0.0238(17) 0.063(3) 0.034(2) 0.010(2) 0.0082(17) 0.0119(16) F7' 0.0258(14) 0.161(5) 0.0418(16) 0.029(2) 0.0206(12) 0.021(2) F8' 0.0417(16) 0.062(2) 0.108(3) -0.0021(17) 0.0029(16) 0.0265(14) C1S 0.0366(18) 0.164(5) 0.131(4) 0.087(4) 0.024(2) 0.005(2) C2S 0.0455(16) 0.079(2) 0.0577(17) 0.0388(16) 0.0339(15) 0.0284(15) N1S 0.0540(15) 0.0726(17) 0.0448(13) 0.0216(12) 0.0231(12) 0.0379(13) C3S 0.074(3) 0.078(3) 0.086(9) 0.025(6) 0.042(3) 0.029(2) C4S 0.068(5) 0.055(3) 0.059(4) 0.011(3) 0.024(4) 0.023(4) N2S 0.074(3) 0.078(3) 0.086(9) 0.025(6) 0.042(3) 0.029(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 O1 1.8114(12) . ? Fe1 N5 1.9193(15) . ? Fe1 N1 1.9520(15) . ? Fe1 N3 1.9674(15) . ? Fe1 N2 1.9800(15) . ? Fe1 N4 2.0358(15) . ? C1 N1 1.345(2) . ? C1 C2 1.373(3) . ? C1 H1 0.9500 . ? C2 C3 1.386(3) . ? C2 H2 0.9500 . ? C3 C4 1.381(3) . ? C3 H3 0.9500 . ? C4 C5 1.386(3) . ? C4 H4 0.9500 . ? C5 N1 1.347(2) . ? C5 C6 1.509(3) . ? C6 N2 1.498(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.493(3) . ? C7 N2 1.500(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N3 1.352(2) . ? C8 C9 1.384(3) . ? C9 C10 1.379(3) . ? C9 H9 0.9500 . ? C10 C11 1.390(3) . ? C10 H10 0.9500 . ? C11 C12 1.376(3) . ? C11 H11 0.9500 . ? C12 N3 1.346(2) . ? C12 H12 0.9500 . ? C13 C14 1.504(3) . ? C13 C25 1.508(3) . ? C13 N2 1.512(2) . ? C13 H13 1.0000 . ? C14 N4 1.358(2) . ? C14 C15 1.374(3) . ? C15 C16 1.385(3) . ? C15 H15 0.9500 . ? C16 C17 1.376(3) . ? C16 H16 0.9500 . ? C17 C18 1.394(3) . ? C17 H17 0.9500 . ? C18 N4 1.356(2) . ? C18 C19 1.486(3) . ? C19 C20 1.394(3) . ? C19 C24 1.395(3) . ? C20 C21 1.388(3) . ? C20 H20 0.9500 . ? C21 C22 1.384(3) . ? C21 H21 0.9500 . ? C22 C23 1.385(3) . ? C22 H22 0.9500 . ? C23 C24 1.385(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 N5 1.352(3) . ? C25 C26 1.374(3) . ? C26 C27 1.394(3) . ? C26 H26 0.9500 . ? C27 C28 1.368(3) . ? C27 H27 0.9500 . ? C28 C29 1.410(3) . ? C28 H28 0.9500 . ? C29 N5 1.350(2) . ? C29 C30 1.464(3) . ? C30 C31 1.410(3) . ? C30 C35 1.422(3) . ? C31 C32 1.370(3) . ? C31 H31 0.9500 . ? C32 C33 1.387(3) . ? C32 H32 0.9500 . ? C33 C34 1.383(3) . ? C33 H33 0.9500 . ? C34 C35 1.402(3) . ? C34 H34 0.9500 . ? C35 O1 1.340(2) . ? B1 F1 1.382(9) . ? B1 F3 1.388(9) . ? B1 F2 1.390(9) . ? B1 F4 1.394(9) . ? B1' F4' 1.380(12) . ? B1' F3' 1.384(11) . ? B1' F2' 1.389(11) . ? B1' F1' 1.398(11) . ? B2 F7 1.363(11) . ? B2 F5 1.377(11) . ? B2 F6 1.385(11) . ? B2 F8 1.390(11) . ? B2' F7' 1.354(7) . ? B2' F5' 1.370(8) . ? B2' F6' 1.385(7) . ? B2' F8' 1.392(7) . ? C1S C2S 1.463(5) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S N1S 1.123(4) . ? C3S C4S 1.53(2) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C4S N2S 1.10(2) . ? 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 O1 Fe1 N5 93.87(6) . . ? O1 Fe1 N1 95.84(6) . . ? N5 Fe1 N1 169.45(7) . . ? O1 Fe1 N3 92.88(6) . . ? N5 Fe1 N3 91.46(6) . . ? N1 Fe1 N3 92.14(6) . . ? O1 Fe1 N2 175.87(6) . . ? N5 Fe1 N2 85.21(6) . . ? N1 Fe1 N2 85.38(6) . . ? N3 Fe1 N2 83.13(6) . . ? O1 Fe1 N4 100.84(6) . . ? N5 Fe1 N4 87.61(6) . . ? N1 Fe1 N4 86.54(6) . . ? N3 Fe1 N4 166.29(6) . . ? N2 Fe1 N4 83.16(6) . . ? N1 C1 C2 121.84(18) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C1 C2 C3 118.76(18) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 119.68(18) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 118.82(18) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.26(17) . . ? N1 C5 C6 116.81(15) . . ? C4 C5 C6 121.87(17) . . ? N2 C6 C5 110.95(15) . . ? N2 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 N2 110.07(14) . . ? C8 C7 H7A 109.6 . . ? N2 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? N2 C7 H7B 109.6 . . ? H7A C7 H7B 108.2 . . ? N3 C8 C9 121.63(18) . . ? N3 C8 C7 115.68(16) . . ? C9 C8 C7 122.67(17) . . ? C10 C9 C8 119.31(18) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 118.95(18) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 119.05(19) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? N3 C12 C11 122.15(17) . . ? N3 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C14 C13 C25 107.45(15) . . ? C14 C13 N2 105.98(14) . . ? C25 C13 N2 106.43(15) . . ? C14 C13 H13 112.2 . . ? C25 C13 H13 112.2 . . ? N2 C13 H13 112.2 . . ? N4 C14 C15 123.92(17) . . ? N4 C14 C13 112.73(16) . . ? C15 C14 C13 123.35(17) . . ? C14 C15 C16 117.94(19) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? C17 C16 C15 118.77(18) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C16 C17 C18 121.32(18) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? N4 C18 C17 119.79(17) . . ? N4 C18 C19 121.25(16) . . ? C17 C18 C19 118.96(16) . . ? C20 C19 C24 119.09(18) . . ? C20 C19 C18 118.74(17) . . ? C24 C19 C18 122.09(17) . . ? C21 C20 C19 120.5(2) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 119.7(2) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.3(2) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C24 120.09(19) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.25(18) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? N5 C25 C26 122.46(19) . . ? N5 C25 C13 112.09(16) . . ? C26 C25 C13 125.34(19) . . ? C25 C26 C27 117.2(2) . . ? C25 C26 H26 121.4 . . ? C27 C26 H26 121.4 . . ? C28 C27 C26 120.37(19) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.8(2) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? N5 C29 C28 117.72(19) . . ? N5 C29 C30 118.24(17) . . ? C28 C29 C30 124.01(18) . . ? C31 C30 C35 117.17(18) . . ? C31 C30 C29 119.57(18) . . ? C35 C30 C29 123.21(17) . . ? C32 C31 C30 122.4(2) . . ? C32 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? C31 C32 C33 119.84(19) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 119.9(2) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 121.0(2) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? O1 C35 C34 115.02(17) . . ? O1 C35 C30 125.44(17) . . ? C34 C35 C30 119.54(17) . . ? C1 N1 C5 119.63(16) . . ? C1 N1 Fe1 125.73(13) . . ? C5 N1 Fe1 114.37(12) . . ? C6 N2 C7 112.86(14) . . ? C6 N2 C13 114.30(14) . . ? C7 N2 C13 111.25(14) . . ? C6 N2 Fe1 110.23(11) . . ? C7 N2 Fe1 110.83(11) . . ? C13 N2 Fe1 96.21(10) . . ? C12 N3 C8 118.77(16) . . ? C12 N3 Fe1 125.75(12) . . ? C8 N3 Fe1 115.48(13) . . ? C18 N4 C14 118.25(16) . . ? C18 N4 Fe1 133.64(13) . . ? C14 N4 Fe1 107.58(12) . . ? C29 N5 C25 121.45(16) . . ? C29 N5 Fe1 128.30(13) . . ? C25 N5 Fe1 110.24(12) . . ? C35 O1 Fe1 124.52(11) . . ? F1 B1 F3 108.4(10) . . ? F1 B1 F2 110.8(11) . . ? F3 B1 F2 109.9(12) . . ? F1 B1 F4 108.9(8) . . ? F3 B1 F4 108.8(10) . . ? F2 B1 F4 110.0(11) . . ? F4' B1' F3' 110.2(13) . . ? F4' B1' F2' 109.3(15) . . ? F3' B1' F2' 111.6(15) . . ? F4' B1' F1' 107.6(10) . . ? F3' B1' F1' 108.4(13) . . ? F2' B1' F1' 109.6(14) . . ? F7 B2 F5 112.1(10) . . ? F7 B2 F6 111.1(10) . . ? F5 B2 F6 109.5(10) . . ? F7 B2 F8 106.2(8) . . ? F5 B2 F8 110.3(9) . . ? F6 B2 F8 107.6(9) . . ? F7' B2' F5' 109.0(6) . . ? F7' B2' F6' 112.0(6) . . ? F5' B2' F6' 111.6(7) . . ? F7' B2' F8' 107.6(5) . . ? F5' B2' F8' 108.9(6) . . ? F6' B2' F8' 107.6(6) . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? N1S C2S C1S 179.4(3) . . ? N2S C4S C3S 175(4) . . ? 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 N1 C1 C2 C3 -0.5(3) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 C5 1.1(3) . . . . ? C3 C4 C5 N1 -1.0(3) . . . . ? C3 C4 C5 C6 176.24(17) . . . . ? N1 C5 C6 N2 -8.3(2) . . . . ? C4 C5 C6 N2 174.41(16) . . . . ? N2 C7 C8 N3 13.7(2) . . . . ? N2 C7 C8 C9 -167.69(17) . . . . ? N3 C8 C9 C10 -1.2(3) . . . . ? C7 C8 C9 C10 -179.80(18) . . . . ? C8 C9 C10 C11 -2.0(3) . . . . ? C9 C10 C11 C12 2.6(3) . . . . ? C10 C11 C12 N3 0.0(3) . . . . ? C25 C13 C14 N4 68.01(19) . . . . ? N2 C13 C14 N4 -45.46(19) . . . . ? C25 C13 C14 C15 -112.6(2) . . . . ? N2 C13 C14 C15 133.94(18) . . . . ? N4 C14 C15 C16 1.0(3) . . . . ? C13 C14 C15 C16 -178.30(17) . . . . ? C14 C15 C16 C17 -0.2(3) . . . . ? C15 C16 C17 C18 -0.6(3) . . . . ? C16 C17 C18 N4 0.6(3) . . . . ? C16 C17 C18 C19 -179.78(17) . . . . ? N4 C18 C19 C20 119.5(2) . . . . ? C17 C18 C19 C20 -60.2(2) . . . . ? N4 C18 C19 C24 -63.9(2) . . . . ? C17 C18 C19 C24 116.5(2) . . . . ? C24 C19 C20 C21 2.3(3) . . . . ? C18 C19 C20 C21 179.10(18) . . . . ? C19 C20 C21 C22 -1.5(3) . . . . ? C20 C21 C22 C23 0.0(3) . . . . ? C21 C22 C23 C24 0.7(3) . . . . ? C22 C23 C24 C19 0.2(3) . . . . ? C20 C19 C24 C23 -1.6(3) . . . . ? C18 C19 C24 C23 -178.31(17) . . . . ? C14 C13 C25 N5 -70.69(19) . . . . ? N2 C13 C25 N5 42.5(2) . . . . ? C14 C13 C25 C26 105.7(2) . . . . ? N2 C13 C25 C26 -141.12(19) . . . . ? N5 C25 C26 C27 2.0(3) . . . . ? C13 C25 C26 C27 -174.0(2) . . . . ? C25 C26 C27 C28 -0.2(3) . . . . ? C26 C27 C28 C29 -1.1(4) . . . . ? C27 C28 C29 N5 0.7(3) . . . . ? C27 C28 C29 C30 178.8(2) . . . . ? N5 C29 C30 C31 -168.09(17) . . . . ? C28 C29 C30 C31 13.8(3) . . . . ? N5 C29 C30 C35 14.5(3) . . . . ? C28 C29 C30 C35 -163.65(18) . . . . ? C35 C30 C31 C32 1.7(3) . . . . ? C29 C30 C31 C32 -175.87(18) . . . . ? C30 C31 C32 C33 0.9(3) . . . . ? C31 C32 C33 C34 -1.8(3) . . . . ? C32 C33 C34 C35 0.0(3) . . . . ? C33 C34 C35 O1 -177.44(17) . . . . ? C33 C34 C35 C30 2.6(3) . . . . ? C31 C30 C35 O1 176.66(17) . . . . ? C29 C30 C35 O1 -5.8(3) . . . . ? C31 C30 C35 C34 -3.4(3) . . . . ? C29 C30 C35 C34 174.10(17) . . . . ? C2 C1 N1 C5 0.7(3) . . . . ? C2 C1 N1 Fe1 -172.92(14) . . . . ? C4 C5 N1 C1 0.1(3) . . . . ? C6 C5 N1 C1 -177.28(16) . . . . ? C4 C5 N1 Fe1 174.38(14) . . . . ? C6 C5 N1 Fe1 -3.0(2) . . . . ? O1 Fe1 N1 C1 -0.49(15) . . . . ? N5 Fe1 N1 C1 156.5(3) . . . . ? N3 Fe1 N1 C1 -93.61(15) . . . . ? N2 Fe1 N1 C1 -176.54(15) . . . . ? N4 Fe1 N1 C1 100.06(15) . . . . ? O1 Fe1 N1 C5 -174.40(12) . . . . ? N5 Fe1 N1 C5 -17.4(4) . . . . ? N3 Fe1 N1 C5 92.48(13) . . . . ? N2 Fe1 N1 C5 9.55(12) . . . . ? N4 Fe1 N1 C5 -73.85(13) . . . . ? C5 C6 N2 C7 -109.48(16) . . . . ? C5 C6 N2 C13 122.07(16) . . . . ? C5 C6 N2 Fe1 15.04(18) . . . . ? C8 C7 N2 C6 101.40(17) . . . . ? C8 C7 N2 C13 -128.58(16) . . . . ? C8 C7 N2 Fe1 -22.79(17) . . . . ? C14 C13 N2 C6 -55.99(18) . . . . ? C25 C13 N2 C6 -170.17(14) . . . . ? C14 C13 N2 C7 174.74(14) . . . . ? C25 C13 N2 C7 60.56(18) . . . . ? C14 C13 N2 Fe1 59.53(14) . . . . ? C25 C13 N2 Fe1 -54.65(14) . . . . ? N5 Fe1 N2 C6 161.65(12) . . . . ? N1 Fe1 N2 C6 -13.57(12) . . . . ? N3 Fe1 N2 C6 -106.29(12) . . . . ? N4 Fe1 N2 C6 73.49(12) . . . . ? N5 Fe1 N2 C7 -72.67(12) . . . . ? N1 Fe1 N2 C7 112.10(12) . . . . ? N3 Fe1 N2 C7 19.39(12) . . . . ? N4 Fe1 N2 C7 -160.83(12) . . . . ? N5 Fe1 N2 C13 42.88(10) . . . . ? N1 Fe1 N2 C13 -132.34(10) . . . . ? N3 Fe1 N2 C13 134.94(10) . . . . ? N4 Fe1 N2 C13 -45.28(10) . . . . ? C11 C12 N3 C8 -3.1(3) . . . . ? C11 C12 N3 Fe1 177.10(14) . . . . ? C9 C8 N3 C12 3.8(3) . . . . ? C7 C8 N3 C12 -177.56(16) . . . . ? C9 C8 N3 Fe1 -176.43(14) . . . . ? C7 C8 N3 Fe1 2.2(2) . . . . ? O1 Fe1 N3 C12 -13.80(15) . . . . ? N5 Fe1 N3 C12 -107.75(15) . . . . ? N1 Fe1 N3 C12 82.17(15) . . . . ? N2 Fe1 N3 C12 167.26(15) . . . . ? N4 Fe1 N3 C12 166.3(2) . . . . ? O1 Fe1 N3 C8 166.43(13) . . . . ? N5 Fe1 N3 C8 72.47(13) . . . . ? N1 Fe1 N3 C8 -97.61(13) . . . . ? N2 Fe1 N3 C8 -12.52(13) . . . . ? N4 Fe1 N3 C8 -13.4(3) . . . . ? C17 C18 N4 C14 0.2(2) . . . . ? C19 C18 N4 C14 -179.42(16) . . . . ? C17 C18 N4 Fe1 170.66(13) . . . . ? C19 C18 N4 Fe1 -9.0(3) . . . . ? C15 C14 N4 C18 -1.0(3) . . . . ? C13 C14 N4 C18 178.35(15) . . . . ? C15 C14 N4 Fe1 -173.80(15) . . . . ? C13 C14 N4 Fe1 5.59(17) . . . . ? O1 Fe1 N4 C18 34.55(17) . . . . ? N5 Fe1 N4 C18 128.04(17) . . . . ? N1 Fe1 N4 C18 -60.75(16) . . . . ? N3 Fe1 N4 C18 -145.6(2) . . . . ? N2 Fe1 N4 C18 -146.51(17) . . . . ? O1 Fe1 N4 C14 -154.28(11) . . . . ? N5 Fe1 N4 C14 -60.79(12) . . . . ? N1 Fe1 N4 C14 110.43(12) . . . . ? N3 Fe1 N4 C14 25.6(3) . . . . ? N2 Fe1 N4 C14 24.67(12) . . . . ? C28 C29 N5 C25 1.1(3) . . . . ? C30 C29 N5 C25 -177.17(16) . . . . ? C28 C29 N5 Fe1 179.70(14) . . . . ? C30 C29 N5 Fe1 1.5(2) . . . . ? C26 C25 N5 C29 -2.5(3) . . . . ? C13 C25 N5 C29 174.01(16) . . . . ? C26 C25 N5 Fe1 178.65(16) . . . . ? C13 C25 N5 Fe1 -4.83(19) . . . . ? O1 Fe1 N5 C29 -18.35(16) . . . . ? N1 Fe1 N5 C29 -175.4(3) . . . . ? N3 Fe1 N5 C29 74.63(16) . . . . ? N2 Fe1 N5 C29 157.61(16) . . . . ? N4 Fe1 N5 C29 -119.06(16) . . . . ? O1 Fe1 N5 C25 160.40(12) . . . . ? N1 Fe1 N5 C25 3.3(4) . . . . ? N3 Fe1 N5 C25 -106.62(13) . . . . ? N2 Fe1 N5 C25 -23.64(13) . . . . ? N4 Fe1 N5 C25 59.69(13) . . . . ? C34 C35 O1 Fe1 160.58(13) . . . . ? C30 C35 O1 Fe1 -19.5(2) . . . . ? N5 Fe1 O1 C35 26.47(14) . . . . ? N1 Fe1 O1 C35 -157.64(14) . . . . ? N3 Fe1 O1 C35 -65.20(14) . . . . ? N4 Fe1 O1 C35 114.77(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.456 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.063 _iucr_refine_instructions_details ; TITL x0959a - SHELXL CELL 0.71073 11.9067 12.4935 13.4579 91.551 112.033 104.801 ZERR 1 0.0003 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H F FE N O B UNIT 76 65 16 2 13 2 4 TEMP -163 ACTA HTAB BOND BOND $H CONF WPDB L.S. 6 FMAP 2 PLAN 10 OMIT -2 52.5 OMIT 1 0 0 OMIT 0 1 0 OMIT -1 0 1 WGHT 0.050600 1.061400 FVAR 4.30606 0.56169 0.36891 PART 0 rem Fe complex FE1 4 0.122245 0.241086 0.250446 11.00000 0.01609 0.01709 = 0.01398 0.00058 0.00658 0.00590 C1 1 0.381861 0.222182 0.349302 11.00000 0.01912 0.02342 = 0.02195 -0.00035 0.00936 0.00611 AFIX 43 H1 2 0.389651 0.240876 0.283765 11.00000 -1.20000 AFIX 0 C2 1 0.480072 0.196233 0.428503 11.00000 0.01893 0.03051 = 0.02965 -0.00137 0.00702 0.00797 AFIX 43 H2 2 0.554583 0.196310 0.417861 11.00000 -1.20000 AFIX 0 C3 1 0.468463 0.169931 0.524240 11.00000 0.02056 0.02798 = 0.02438 0.00295 0.00126 0.00853 AFIX 43 H3 2 0.535029 0.151249 0.579917 11.00000 -1.20000 AFIX 0 C4 1 0.359670 0.171007 0.538321 11.00000 0.02488 0.02431 = 0.01846 0.00209 0.00518 0.00597 AFIX 43 H4 2 0.351034 0.154455 0.604027 11.00000 -1.20000 AFIX 0 C5 1 0.263331 0.196660 0.454909 11.00000 0.02125 0.01607 = 0.01748 -0.00020 0.00762 0.00544 C6 1 0.138642 0.192722 0.461619 11.00000 0.02450 0.02504 = 0.01622 0.00448 0.00961 0.01050 AFIX 23 H6A 2 0.094480 0.114842 0.464422 11.00000 -1.20000 H6B 2 0.154222 0.239060 0.528898 11.00000 -1.20000 AFIX 0 C7 1 0.042182 0.346039 0.394655 11.00000 0.02448 0.02147 = 0.02365 0.00156 0.01413 0.01001 AFIX 23 H7A 2 -0.046867 0.346061 0.356326 11.00000 -1.20000 H7B 2 0.064266 0.359431 0.473441 11.00000 -1.20000 AFIX 0 C8 1 0.126459 0.436907 0.363616 11.00000 0.01907 0.02439 = 0.01739 0.00036 0.00683 0.00973 C9 1 0.150734 0.548957 0.398054 11.00000 0.02621 0.02521 = 0.02550 -0.00280 0.01211 0.00936 AFIX 43 H9 2 0.113603 0.571079 0.443522 11.00000 -1.20000 AFIX 0 C10 1 0.229352 0.628124 0.365692 11.00000 0.02927 0.02037 = 0.02982 -0.00425 0.01136 0.00574 AFIX 43 H10 2 0.245014 0.705505 0.386628 11.00000 -1.20000 AFIX 0 C11 1 0.285351 0.592940 0.301939 11.00000 0.02617 0.02277 = 0.02938 -0.00031 0.01363 0.00157 AFIX 43 H11 2 0.342597 0.645816 0.281136 11.00000 -1.20000 AFIX 0 C12 1 0.256680 0.480431 0.269394 11.00000 0.02062 0.02476 = 0.02060 -0.00040 0.00938 0.00512 AFIX 43 H12 2 0.295000 0.456560 0.225785 11.00000 -1.20000 AFIX 0 C13 1 -0.070406 0.151897 0.300595 11.00000 0.01727 0.02323 = 0.02280 0.00175 0.01005 0.00403 AFIX 13 H13 2 -0.125857 0.136097 0.341964 11.00000 -1.20000 AFIX 0 C14 1 -0.042449 0.048664 0.268311 11.00000 0.01952 0.02194 = 0.01581 0.00128 0.00600 0.00493 C15 1 -0.104346 -0.057408 0.277131 11.00000 0.02469 0.02483 = 0.02096 0.00125 0.00937 0.00154 AFIX 43 H15 2 -0.170204 -0.069812 0.302812 11.00000 -1.20000 AFIX 0 C16 1 -0.067734 -0.145671 0.247418 11.00000 0.03495 0.02037 = 0.02103 0.00052 0.00999 0.00132 AFIX 43 H16 2 -0.107912 -0.220279 0.252493 11.00000 -1.20000 AFIX 0 C17 1 0.027908 -0.123293 0.210414 11.00000 0.03385 0.01991 = 0.01749 -0.00078 0.00892 0.00741 AFIX 43 H17 2 0.054156 -0.183261 0.190491 11.00000 -1.20000 AFIX 0 C18 1 0.087041 -0.014430 0.201574 11.00000 0.02366 0.02058 = 0.01328 -0.00052 0.00456 0.00762 C19 1 0.189499 0.004677 0.160704 11.00000 0.02503 0.01807 = 0.01719 -0.00372 0.00659 0.00670 C20 1 0.297145 -0.027874 0.217683 11.00000 0.03309 0.03101 = 0.02240 0.00146 0.00982 0.01691 AFIX 43 H20 2 0.304167 -0.060559 0.281879 11.00000 -1.20000 AFIX 0 C21 1 0.394217 -0.012920 0.181379 11.00000 0.03220 0.04561 = 0.03315 -0.00272 0.01046 0.02122 AFIX 43 H21 2 0.468265 -0.033608 0.221501 11.00000 -1.20000 AFIX 0 C22 1 0.382615 0.032255 0.086495 11.00000 0.03047 0.04035 = 0.03383 -0.00662 0.01808 0.00940 AFIX 43 H22 2 0.448903 0.042546 0.061489 11.00000 -1.20000 AFIX 0 C23 1 0.274840 0.062529 0.027828 11.00000 0.03415 0.02968 = 0.02065 -0.00268 0.01359 0.00666 AFIX 43 H23 2 0.266992 0.092780 -0.037655 11.00000 -1.20000 AFIX 0 C24 1 0.178440 0.048767 0.064487 11.00000 0.02439 0.02111 = 0.01786 -0.00219 0.00716 0.00562 AFIX 43 H24 2 0.104523 0.069439 0.023937 11.00000 -1.20000 AFIX 0 C25 1 -0.128580 0.200471 0.198729 11.00000 0.02094 0.02240 = 0.02518 0.00122 0.00932 0.00706 C26 1 -0.254281 0.195126 0.149005 11.00000 0.02058 0.03756 = 0.03555 0.00478 0.00945 0.00890 AFIX 43 H26 2 -0.312424 0.165226 0.180897 11.00000 -1.20000 AFIX 0 C27 1 -0.292860 0.235444 0.049774 11.00000 0.02013 0.04750 = 0.03886 0.00672 0.00167 0.01231 AFIX 43 H27 2 -0.379053 0.233009 0.012583 11.00000 -1.20000 AFIX 0 C28 1 -0.207323 0.278493 0.005639 11.00000 0.02908 0.03502 = 0.02441 0.00521 0.00122 0.01327 AFIX 43 H28 2 -0.235011 0.304543 -0.062631 11.00000 -1.20000 AFIX 0 C29 1 -0.078576 0.284678 0.060228 11.00000 0.02610 0.01905 = 0.01951 -0.00118 0.00490 0.00831 C30 1 0.018062 0.327625 0.017436 11.00000 0.03022 0.01741 = 0.01626 -0.00077 0.00656 0.00789 C31 1 -0.009280 0.387786 -0.071594 11.00000 0.04045 0.02226 = 0.01935 0.00144 0.00756 0.01408 AFIX 43 H31 2 -0.088433 0.403668 -0.099286 11.00000 -1.20000 AFIX 0 C32 1 0.074074 0.424198 -0.119660 11.00000 0.05392 0.02154 = 0.02091 0.00657 0.01456 0.01254 AFIX 43 H32 2 0.052840 0.465416 -0.178915 11.00000 -1.20000 AFIX 0 C33 1 0.189543 0.400731 -0.081594 11.00000 0.04821 0.02445 = 0.02495 0.00371 0.02133 0.00577 AFIX 43 H33 2 0.246549 0.424038 -0.116024 11.00000 -1.20000 AFIX 0 C34 1 0.221547 0.343374 0.006526 11.00000 0.03309 0.02363 = 0.02249 0.00173 0.01417 0.00715 AFIX 43 H34 2 0.300782 0.327590 0.032214 11.00000 -1.20000 AFIX 0 C35 1 0.138872 0.308148 0.058555 11.00000 0.02955 0.01497 = 0.01555 -0.00039 0.00971 0.00604 N1 5 0.274950 0.221870 0.361926 11.00000 0.01725 0.01704 = 0.01706 -0.00115 0.00663 0.00535 N2 5 0.056611 0.234865 0.365961 11.00000 0.01779 0.01882 = 0.01817 0.00152 0.00796 0.00770 N3 5 0.176125 0.403104 0.297323 11.00000 0.01695 0.02047 = 0.01645 -0.00050 0.00637 0.00600 N4 5 0.051014 0.071851 0.230707 11.00000 0.01755 0.01925 = 0.01321 0.00062 0.00413 0.00446 N5 5 -0.043408 0.245708 0.156471 11.00000 0.02021 0.01875 = 0.01838 0.00006 0.00625 0.00758 O1 6 0.183359 0.257450 0.145404 11.00000 0.02261 0.02135 = 0.01689 0.00293 0.00979 0.00891 rem counterions EADP B1 B1' SIMU 0.01 B1 > F4' PART 1 B1 7 0.211337 0.881406 0.514567 21.00000 0.03406 0.02698 = 0.02816 0.00773 0.01983 0.01540 F1 3 0.141202 0.771389 0.502033 21.00000 0.08508 0.02184 = 0.06659 0.00233 0.06064 0.00919 F2 3 0.266186 0.896928 0.439342 21.00000 0.04145 0.03189 = 0.02695 0.00436 0.02261 0.01286 F3 3 0.131607 0.948654 0.501025 21.00000 0.02957 0.03611 = 0.03699 0.00623 0.01314 0.01832 F4 3 0.304978 0.909777 0.619147 21.00000 0.02789 0.07837 = 0.02385 0.01130 0.01047 0.01978 PART 2 SAME B1 > F4 B1' 7 0.201481 0.869062 0.509354 -21.00000 0.03406 0.02698 = 0.02816 0.00773 0.01983 0.01540 F1' 3 0.101525 0.770737 0.467409 -21.00000 0.04962 0.02453 = 0.06191 0.00741 0.04002 0.00688 F2' 3 0.268055 0.886814 0.442956 -21.00000 0.03764 0.02466 = 0.03343 0.01049 0.02514 0.01327 F3' 3 0.152114 0.956432 0.517110 -21.00000 0.03346 0.02167 = 0.04369 0.00534 0.02267 0.01277 F4' 3 0.280299 0.855393 0.610700 -21.00000 0.04495 0.08565 = 0.03512 0.02531 0.02541 0.04251 SADI 0.02 B2 F5 B2 F6 B2 F7 B2 F8 SADI 0.02 F5 F6 F6 F7 F7 F8 F8 F5 F5 F7 F6 F8 SIMU 0.01 B2 > F8' PART 1 B2 7 0.553956 0.693268 0.179517 31.00000 0.04221 0.06151 = 0.02404 0.00253 0.01560 0.03016 F5 3 0.575800 0.707225 0.086551 31.00000 0.04028 0.12023 = 0.02550 0.00876 0.01747 0.01601 F6 3 0.664416 0.690717 0.263604 31.00000 0.03517 0.06332 = 0.03695 0.01775 0.01710 0.02597 F7 3 0.507273 0.774010 0.205215 31.00000 0.08036 0.07056 = 0.03579 -0.00629 -0.00219 0.05882 F8 3 0.463662 0.592004 0.165671 31.00000 0.04973 0.06412 = 0.09679 -0.00662 0.03555 -0.00856 PART 2 SAME B2 > F8 B2' 7 0.573094 0.725160 0.169906 -31.00000 0.02612 0.07168 = 0.02435 0.00372 0.00910 0.02262 F5' 3 0.556113 0.677039 0.070691 -31.00000 0.05386 0.09564 = 0.02818 -0.01162 0.01028 0.03351 F6' 3 0.677286 0.708231 0.251664 -31.00000 0.02378 0.06348 = 0.03371 0.01007 0.00822 0.01188 F7' 3 0.465752 0.685203 0.186795 -31.00000 0.02580 0.16064 = 0.04180 0.02861 0.02056 0.02107 F8' 3 0.594136 0.839997 0.169645 -31.00000 0.04167 0.06244 = 0.10815 -0.00211 0.00290 0.02646 rem solvent molecules C1S 1 -0.416362 0.416542 0.201820 11.00000 0.03664 0.16441 = 0.13147 0.08686 0.02384 0.00528 AFIX 137 H1S1 2 -0.457732 0.472117 0.211589 11.00000 -1.50000 H1S2 2 -0.458925 0.343955 0.215782 11.00000 -1.50000 H1S3 2 -0.421339 0.410169 0.127448 11.00000 -1.50000 AFIX 0 C2S 1 -0.283672 0.451443 0.277395 11.00000 0.04548 0.07917 = 0.05770 0.03877 0.03386 0.02838 N1S 5 -0.181434 0.478311 0.334700 11.00000 0.05399 0.07262 = 0.04475 0.02160 0.02310 0.03788 DELU 0.005 C3S > N2S DFIX 1.50 0.03 C3S C4S DFIX 1.15 0.03 C4S N2S EADP C3S N2S ISOR 0.005 C4S SIMU 0.01 C3S > N2S PART -1 C3S 1 0.574553 0.523028 0.434150 10.50000 0.07393 0.07813 = 0.08622 0.02550 0.04183 0.02921 AFIX 137 H3S1 2 0.620583 0.466930 0.441619 10.50000 -1.50000 H3S2 2 0.634999 0.597175 0.464211 10.50000 -1.50000 H3S3 2 0.523771 0.522290 0.357410 10.50000 -1.50000 AFIX 0 C4S 1 0.487788 0.496056 0.495238 10.50000 0.06786 0.05501 = 0.05863 0.01075 0.02411 0.02342 N2S 5 0.430909 0.481470 0.544675 10.50000 0.07393 0.07813 = 0.08622 0.02550 0.04183 0.02921 HKLF 4 REM x0959a - SHELXL REM R1 = 0.0358 for 6218 Fo > 4sig(Fo) and 0.0429 for all 7168 data REM 605 parameters refined using 328 restraints END WGHT 0.0506 1.0608 REM Highest difference peak 0.456, deepest hole -0.580, 1-sigma level 0.063 Q1 1 0.5963 0.8042 0.1209 11.00000 0.05 0.36 Q2 1 0.5645 0.8043 0.1917 11.00000 0.05 0.33 Q3 1 0.0979 0.3956 0.3866 11.00000 0.05 0.32 Q4 1 0.1786 0.0218 0.1150 11.00000 0.05 0.30 Q5 1 0.1987 0.2965 0.2650 11.00000 0.05 0.29 Q6 1 0.2465 0.0160 0.1934 11.00000 0.05 0.28 Q7 1 0.2019 0.1946 0.4588 11.00000 0.05 0.27 Q8 1 0.1396 -0.0033 0.1778 11.00000 0.05 0.27 Q9 1 -0.0007 0.1969 0.3391 11.00000 0.05 0.27 Q10 1 0.3399 0.0723 0.0798 11.00000 0.05 0.26 ;