data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 Cl Fe N6 O S, B F4' _chemical_formula_sum 'C32 H34 B Cl F4 Fe N6 O S' _chemical_formula_weight 728.82 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' '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' 'F' 'F' 0.0171 0.0103 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.4707(3) _cell_length_b 9.98637(13) _cell_length_c 25.8674(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.8579(12) _cell_angle_gamma 90.00 _cell_volume 6555.99(14) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 26.31 _exptl_crystal_description 'irregular block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) 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 24531 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.25 _reflns_number_total 6622 _reflns_number_gt 5537 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _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^)+(0.0338P)^2^+7.3328P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6622 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.100505(9) 0.98911(2) 0.344272(10) 0.01602(8) Uani 1 1 d . . . Cl1 Cl 0.093125(17) 0.83045(5) 0.280859(18) 0.02621(11) Uani 1 1 d . . . S1 S 0.113536(17) 0.81540(4) 0.419360(17) 0.01912(10) Uani 1 1 d . . . C1 C 0.10421(7) 1.20921(19) 0.25271(7) 0.0219(4) Uani 1 1 d . . . H1 H 0.1214 1.1438 0.2335 0.026 Uiso 1 1 calc R . . C2 C 0.09311(7) 1.3333(2) 0.23017(7) 0.0239(4) Uani 1 1 d . . . H2 H 0.1028 1.3523 0.1963 0.029 Uiso 1 1 calc R . . C3 C 0.06783(7) 1.42870(19) 0.25766(7) 0.0228(4) Uani 1 1 d . . . H3 H 0.0595 1.5139 0.2428 0.027 Uiso 1 1 calc R . . C4 C 0.05477(7) 1.39803(18) 0.30743(7) 0.0202(4) Uani 1 1 d . . . H4 H 0.0374 1.4618 0.3273 0.024 Uiso 1 1 calc R . . C5 C 0.06756(6) 1.27273(18) 0.32736(7) 0.0177(4) Uani 1 1 d . . . C6 C 0.05454(6) 1.22820(17) 0.38060(7) 0.0172(4) Uani 1 1 d . . . H6 H 0.0472 1.3070 0.4028 0.021 Uiso 1 1 calc R . . C7 C 0.00674(7) 1.13701(18) 0.37320(7) 0.0173(4) Uani 1 1 d . . . C8 C -0.04342(7) 1.17636(19) 0.38291(7) 0.0199(4) Uani 1 1 d . . . H8 H -0.0497 1.2633 0.3960 0.024 Uiso 1 1 calc R . . C9 C -0.08455(7) 1.0857(2) 0.37312(7) 0.0237(4) Uani 1 1 d . . . H9 H -0.1194 1.1096 0.3799 0.028 Uiso 1 1 calc R . . C10 C -0.07416(7) 0.9607(2) 0.35349(7) 0.0236(4) Uani 1 1 d . . . H10 H -0.1017 0.8972 0.3467 0.028 Uiso 1 1 calc R . . C11 C -0.02278(7) 0.92941(19) 0.34386(7) 0.0216(4) Uani 1 1 d . . . H11 H -0.0157 0.8442 0.3297 0.026 Uiso 1 1 calc R . . C12 C 0.08669(7) 1.10851(18) 0.45825(7) 0.0181(4) Uani 1 1 d . . . H12A H 0.0540 1.0545 0.4555 0.022 Uiso 1 1 calc R . . H12B H 0.0797 1.1908 0.4779 0.022 Uiso 1 1 calc R . . C13 C 0.12958(7) 1.02980(18) 0.48832(7) 0.0175(4) Uani 1 1 d . . . C14 C 0.15646(7) 1.08890(19) 0.53175(7) 0.0218(4) Uani 1 1 d . . . H14 H 0.1470 1.1765 0.5419 0.026 Uiso 1 1 calc R . . C15 C 0.19671(8) 1.0218(2) 0.56034(8) 0.0255(4) Uani 1 1 d . . . H15 H 0.2149 1.0642 0.5895 0.031 Uiso 1 1 calc R . . C16 C 0.21044(7) 0.8939(2) 0.54674(8) 0.0258(4) Uani 1 1 d . . . H16 H 0.2380 0.8480 0.5665 0.031 Uiso 1 1 calc R . . C17 C 0.18387(7) 0.83240(19) 0.50419(7) 0.0228(4) Uani 1 1 d . . . H17 H 0.1932 0.7440 0.4949 0.027 Uiso 1 1 calc R . . C18 C 0.14372(7) 0.89914(18) 0.47503(7) 0.0185(4) Uani 1 1 d . . . C19 C 0.05121(7) 0.75935(19) 0.44103(8) 0.0237(4) Uani 1 1 d . . . H19A H 0.0303 0.8386 0.4496 0.028 Uiso 1 1 calc R . . H19B H 0.0312 0.7112 0.4123 0.028 Uiso 1 1 calc R . . C20 C 0.05770(8) 0.6678(2) 0.48817(8) 0.0287(4) Uani 1 1 d . . . H20A H 0.0737 0.7190 0.5183 0.034 Uiso 1 1 calc R . . H20B H 0.0226 0.6365 0.4967 0.034 Uiso 1 1 calc R . . C21 C 0.09056(10) 0.5527(2) 0.47929(8) 0.0347(5) Uani 1 1 d . . . C22 C 0.15085(6) 1.21611(17) 0.40648(7) 0.0180(4) Uani 1 1 d . . . H22A H 0.1572 1.2642 0.4399 0.022 Uiso 1 1 calc R . . H22B H 0.1497 1.2834 0.3783 0.022 Uiso 1 1 calc R . . C23 C 0.19587(7) 1.12059(17) 0.40041(7) 0.0167(3) Uani 1 1 d . . . C24 C 0.24436(7) 1.14666(18) 0.42642(7) 0.0204(4) Uani 1 1 d . . . H24 H 0.2489 1.2210 0.4493 0.024 Uiso 1 1 calc R . . C25 C 0.28620(7) 1.06283(19) 0.41865(7) 0.0231(4) Uani 1 1 d . . . H25 H 0.3201 1.0803 0.4355 0.028 Uiso 1 1 calc R . . C26 C 0.27847(7) 0.95419(19) 0.38637(7) 0.0205(4) Uani 1 1 d . . . H26 H 0.3068 0.8956 0.3806 0.025 Uiso 1 1 calc R . . C27 C 0.22802(7) 0.93156(17) 0.36210(7) 0.0158(3) Uani 1 1 d . . . C28 C 0.25078(7) 0.72181(18) 0.31658(7) 0.0183(4) Uani 1 1 d . . . C29 C 0.22526(7) 0.59802(18) 0.29012(7) 0.0202(4) Uani 1 1 d . . . C30 C 0.19921(8) 0.6335(2) 0.23588(7) 0.0253(4) Uani 1 1 d . . . H30A H 0.1722 0.7022 0.2392 0.038 Uiso 1 1 calc R . . H30B H 0.1829 0.5533 0.2198 0.038 Uiso 1 1 calc R . . H30C H 0.2260 0.6677 0.2142 0.038 Uiso 1 1 calc R . . C31 C 0.26829(8) 0.4937(2) 0.28381(9) 0.0294(5) Uani 1 1 d . . . H31A H 0.2934 0.5286 0.2605 0.044 Uiso 1 1 calc R . . H31B H 0.2522 0.4113 0.2692 0.044 Uiso 1 1 calc R . . H31C H 0.2868 0.4742 0.3178 0.044 Uiso 1 1 calc R . . C32 C 0.18451(7) 0.53888(19) 0.32418(8) 0.0234(4) Uani 1 1 d . . . H32A H 0.2007 0.5263 0.3596 0.035 Uiso 1 1 calc R . . H32B H 0.1722 0.4523 0.3100 0.035 Uiso 1 1 calc R . . H32C H 0.1545 0.6002 0.3247 0.035 Uiso 1 1 calc R . . N1 N 0.09171(5) 1.17823(15) 0.30044(6) 0.0185(3) Uani 1 1 d . . . N2 N 0.01708(6) 1.01540(15) 0.35384(6) 0.0182(3) Uani 1 1 d . . . N3 N 0.09942(5) 1.14697(14) 0.40504(5) 0.0157(3) Uani 1 1 d . . . N4 N 0.11733(10) 0.4649(2) 0.47215(9) 0.0546(6) Uani 1 1 d . . . N5 N 0.18719(5) 1.01463(14) 0.36828(6) 0.0151(3) Uani 1 1 d . . . N6 N 0.21622(6) 0.81850(15) 0.33129(6) 0.0171(3) Uani 1 1 d . . . H6A H 0.1853(8) 0.810(2) 0.3214(8) 0.016(5) Uiso 1 1 d . . . O1 O 0.29831(5) 0.73256(14) 0.32496(6) 0.0285(3) Uani 1 1 d . . . B1 B -0.06001(9) 0.5631(2) 0.39546(9) 0.0249(5) Uani 1 1 d . . . F1 F -0.04958(7) 0.60895(14) 0.34748(5) 0.0568(4) Uani 1 1 d . . . F2 F -0.01476(5) 0.49651(12) 0.41694(6) 0.0386(3) Uani 1 1 d . . . F3 F -0.10091(4) 0.47179(13) 0.39271(6) 0.0409(3) Uani 1 1 d . . . F4 F -0.07027(5) 0.66965(12) 0.42745(5) 0.0392(3) 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 Fe1 0.01436(13) 0.01624(13) 0.01727(13) -0.00287(10) 0.00021(9) 0.00144(10) Cl1 0.0233(2) 0.0281(2) 0.0260(2) -0.01113(19) -0.00552(18) 0.00560(19) S1 0.0202(2) 0.0176(2) 0.0196(2) -0.00145(17) 0.00196(17) -0.00037(18) C1 0.0183(9) 0.0280(10) 0.0192(9) -0.0025(8) 0.0005(7) -0.0004(8) C2 0.0202(9) 0.0320(11) 0.0190(9) 0.0027(8) -0.0008(7) -0.0058(8) C3 0.0170(9) 0.0244(10) 0.0258(10) 0.0052(8) -0.0038(7) -0.0022(8) C4 0.0143(8) 0.0198(9) 0.0264(10) -0.0007(8) -0.0001(7) -0.0005(7) C5 0.0127(8) 0.0197(9) 0.0204(9) -0.0007(7) -0.0004(7) -0.0006(7) C6 0.0159(8) 0.0157(8) 0.0199(9) -0.0018(7) 0.0014(7) 0.0032(7) C7 0.0175(8) 0.0190(9) 0.0152(8) 0.0031(7) 0.0007(7) 0.0024(7) C8 0.0193(9) 0.0217(9) 0.0187(9) 0.0022(7) 0.0022(7) 0.0042(8) C9 0.0163(9) 0.0304(10) 0.0249(10) 0.0050(8) 0.0040(7) 0.0026(8) C10 0.0179(9) 0.0268(10) 0.0255(10) 0.0049(8) -0.0017(7) -0.0026(8) C11 0.0197(9) 0.0209(9) 0.0236(9) 0.0001(8) -0.0016(7) -0.0003(8) C12 0.0182(8) 0.0185(9) 0.0179(9) -0.0016(7) 0.0038(7) 0.0003(7) C13 0.0179(8) 0.0200(9) 0.0149(8) 0.0016(7) 0.0040(7) -0.0007(7) C14 0.0240(9) 0.0207(9) 0.0212(9) -0.0012(7) 0.0039(7) -0.0019(8) C15 0.0255(10) 0.0315(11) 0.0191(9) 0.0011(8) -0.0011(7) -0.0055(8) C16 0.0208(9) 0.0313(11) 0.0249(10) 0.0049(8) -0.0006(8) 0.0024(8) C17 0.0222(9) 0.0221(9) 0.0243(10) 0.0021(8) 0.0030(7) 0.0026(8) C18 0.0167(8) 0.0210(9) 0.0179(9) 0.0002(7) 0.0030(7) -0.0021(7) C19 0.0224(9) 0.0221(10) 0.0269(10) 0.0006(8) 0.0036(8) -0.0049(8) C20 0.0394(11) 0.0236(10) 0.0237(10) -0.0016(8) 0.0062(8) -0.0080(9) C21 0.0582(14) 0.0218(10) 0.0232(11) 0.0010(9) -0.0025(10) -0.0048(11) C22 0.0180(9) 0.0160(8) 0.0200(9) -0.0024(7) 0.0015(7) -0.0016(7) C23 0.0180(8) 0.0158(8) 0.0166(8) 0.0014(7) 0.0037(7) -0.0016(7) C24 0.0196(9) 0.0196(9) 0.0218(9) -0.0052(7) 0.0010(7) -0.0034(7) C25 0.0152(8) 0.0266(10) 0.0269(10) -0.0049(8) -0.0015(7) -0.0018(8) C26 0.0160(8) 0.0215(9) 0.0235(9) -0.0013(8) -0.0001(7) 0.0014(7) C27 0.0159(8) 0.0158(8) 0.0158(8) 0.0004(7) 0.0024(6) -0.0017(7) C28 0.0192(9) 0.0184(9) 0.0178(9) 0.0006(7) 0.0045(7) 0.0005(7) C29 0.0202(9) 0.0187(9) 0.0218(9) -0.0022(7) 0.0028(7) -0.0002(7) C30 0.0317(10) 0.0240(10) 0.0207(9) -0.0039(8) 0.0039(8) -0.0023(8) C31 0.0286(11) 0.0235(10) 0.0363(12) -0.0079(9) 0.0045(9) 0.0035(8) C32 0.0247(10) 0.0198(9) 0.0257(10) 0.0002(8) 0.0018(8) -0.0042(8) N1 0.0150(7) 0.0207(8) 0.0195(8) -0.0005(6) -0.0005(6) -0.0002(6) N2 0.0156(7) 0.0183(8) 0.0201(8) -0.0001(6) -0.0009(6) 0.0009(6) N3 0.0152(7) 0.0162(7) 0.0157(7) 0.0007(6) 0.0018(5) 0.0010(6) N4 0.0872(18) 0.0323(11) 0.0428(13) -0.0044(10) -0.0028(12) 0.0186(12) N5 0.0131(7) 0.0169(7) 0.0153(7) -0.0005(6) 0.0015(5) -0.0010(6) N6 0.0113(7) 0.0184(8) 0.0212(8) -0.0033(6) -0.0002(6) -0.0003(6) O1 0.0157(7) 0.0301(7) 0.0397(8) -0.0133(6) 0.0028(6) 0.0007(6) B1 0.0240(11) 0.0221(11) 0.0292(12) -0.0042(9) 0.0059(9) -0.0013(9) F1 0.1029(12) 0.0378(8) 0.0306(7) 0.0031(6) 0.0106(8) -0.0077(8) F2 0.0264(6) 0.0283(6) 0.0593(9) -0.0071(6) -0.0063(6) 0.0007(5) F3 0.0195(6) 0.0340(7) 0.0697(10) -0.0165(6) 0.0063(6) -0.0041(5) F4 0.0412(7) 0.0276(6) 0.0508(8) -0.0145(6) 0.0156(6) -0.0003(6) _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 N2 2.1757(15) . ? Fe1 N1 2.2044(15) . ? Fe1 N3 2.2281(14) . ? Fe1 N5 2.2568(14) . ? Fe1 Cl1 2.2769(5) . ? Fe1 S1 2.6044(5) . ? S1 C18 1.7823(18) . ? S1 C19 1.8161(18) . ? C1 N1 1.337(2) . ? C1 C2 1.388(3) . ? C1 H1 0.9500 . ? C2 C3 1.381(3) . ? C2 H2 0.9500 . ? C3 C4 1.391(3) . ? C3 H3 0.9500 . ? C4 C5 1.382(3) . ? C4 H4 0.9500 . ? C5 N1 1.351(2) . ? C5 C6 1.511(2) . ? C6 N3 1.497(2) . ? C6 C7 1.520(2) . ? C6 H6 1.0000 . ? C7 N2 1.348(2) . ? C7 C8 1.380(2) . ? C8 C9 1.391(3) . ? C8 H8 0.9500 . ? C9 C10 1.382(3) . ? C9 H9 0.9500 . ? C10 C11 1.388(3) . ? C10 H10 0.9500 . ? C11 N2 1.338(2) . ? C11 H11 0.9500 . ? C12 N3 1.491(2) . ? C12 C13 1.507(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.396(2) . ? C13 C18 1.404(2) . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.378(3) . ? C15 H15 0.9500 . ? C16 C17 1.386(3) . ? C16 H16 0.9500 . ? C17 C18 1.389(3) . ? C17 H17 0.9500 . ? C19 C20 1.522(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.451(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 N4 1.135(3) . ? C22 N3 1.479(2) . ? C22 C23 1.510(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N5 1.352(2) . ? C23 C24 1.380(2) . ? C24 C25 1.383(3) . ? C24 H24 0.9500 . ? C25 C26 1.373(3) . ? C25 H25 0.9500 . ? C26 C27 1.400(2) . ? C26 H26 0.9500 . ? C27 N5 1.350(2) . ? C27 N6 1.400(2) . ? C28 O1 1.216(2) . ? C28 N6 1.382(2) . ? C28 C29 1.531(2) . ? C29 C31 1.531(3) . ? C29 C32 1.536(3) . ? C29 C30 1.542(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N6 H6A 0.81(2) . ? B1 F1 1.370(3) . ? B1 F3 1.382(2) . ? B1 F4 1.386(2) . ? B1 F2 1.404(3) . ? 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 N2 Fe1 N1 84.11(5) . . ? N2 Fe1 N3 76.33(5) . . ? N1 Fe1 N3 75.52(5) . . ? N2 Fe1 N5 153.79(6) . . ? N1 Fe1 N5 95.69(5) . . ? N3 Fe1 N5 78.25(5) . . ? N2 Fe1 Cl1 98.28(4) . . ? N1 Fe1 Cl1 103.12(4) . . ? N3 Fe1 Cl1 174.52(4) . . ? N5 Fe1 Cl1 107.22(4) . . ? N2 Fe1 S1 93.41(4) . . ? N1 Fe1 S1 162.79(4) . . ? N3 Fe1 S1 87.33(4) . . ? N5 Fe1 S1 79.05(4) . . ? Cl1 Fe1 S1 94.089(18) . . ? C18 S1 C19 102.93(9) . . ? C18 S1 Fe1 108.00(6) . . ? C19 S1 Fe1 112.08(6) . . ? N1 C1 C2 122.57(17) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.15(18) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 118.90(18) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 118.52(17) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 122.91(17) . . ? N1 C5 C6 114.13(15) . . ? C4 C5 C6 122.94(16) . . ? N3 C6 C5 109.02(13) . . ? N3 C6 C7 107.66(13) . . ? C5 C6 C7 107.28(14) . . ? N3 C6 H6 110.9 . . ? C5 C6 H6 110.9 . . ? C7 C6 H6 110.9 . . ? N2 C7 C8 122.50(16) . . ? N2 C7 C6 114.00(14) . . ? C8 C7 C6 123.42(16) . . ? C7 C8 C9 118.43(17) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? C10 C9 C8 119.34(17) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 118.80(18) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? N2 C11 C10 122.18(17) . . ? N2 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? N3 C12 C13 113.96(14) . . ? N3 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? N3 C12 H12B 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C14 C13 C18 118.13(16) . . ? C14 C13 C12 118.65(16) . . ? C18 C13 C12 123.22(16) . . ? C15 C14 C13 121.03(17) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 120.30(18) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.75(18) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 120.43(17) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.36(17) . . ? C17 C18 S1 117.46(14) . . ? C13 C18 S1 122.13(14) . . ? C20 C19 S1 113.20(14) . . ? C20 C19 H19A 108.9 . . ? S1 C19 H19A 108.9 . . ? C20 C19 H19B 108.9 . . ? S1 C19 H19B 108.9 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C19 111.94(17) . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20B 109.2 . . ? C19 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? N4 C21 C20 178.2(3) . . ? N3 C22 C23 112.42(14) . . ? N3 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? N3 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? N5 C23 C24 122.69(16) . . ? N5 C23 C22 118.18(15) . . ? C24 C23 C22 119.10(16) . . ? C23 C24 C25 118.92(17) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 119.62(17) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 118.63(17) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? N5 C27 N6 115.62(15) . . ? N5 C27 C26 122.33(16) . . ? N6 C27 C26 122.02(16) . . ? O1 C28 N6 122.47(17) . . ? O1 C28 C29 121.96(16) . . ? N6 C28 C29 115.55(15) . . ? C28 C29 C31 108.47(15) . . ? C28 C29 C32 109.64(15) . . ? C31 C29 C32 108.92(16) . . ? C28 C29 C30 110.78(15) . . ? C31 C29 C30 108.44(16) . . ? C32 C29 C30 110.54(15) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C1 N1 C5 117.94(16) . . ? C1 N1 Fe1 130.64(13) . . ? C5 N1 Fe1 111.35(12) . . ? C11 N2 C7 118.73(15) . . ? C11 N2 Fe1 129.27(12) . . ? C7 N2 Fe1 111.99(11) . . ? C22 N3 C12 111.01(13) . . ? C22 N3 C6 113.62(13) . . ? C12 N3 C6 108.15(13) . . ? C22 N3 Fe1 106.51(10) . . ? C12 N3 Fe1 119.07(10) . . ? C6 N3 Fe1 98.05(10) . . ? C27 N5 C23 117.77(14) . . ? C27 N5 Fe1 130.05(11) . . ? C23 N5 Fe1 111.26(11) . . ? C28 N6 C27 127.55(15) . . ? C28 N6 H6A 117.3(14) . . ? C27 N6 H6A 115.1(14) . . ? F1 B1 F3 112.16(18) . . ? F1 B1 F4 110.20(18) . . ? F3 B1 F4 110.96(16) . . ? F1 B1 F2 107.53(17) . . ? F3 B1 F2 107.32(17) . . ? F4 B1 F2 108.50(17) . . ? 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 N2 Fe1 S1 C18 -101.64(7) . . . . ? N1 Fe1 S1 C18 -20.54(15) . . . . ? N3 Fe1 S1 C18 -25.51(7) . . . . ? N5 Fe1 S1 C18 53.03(7) . . . . ? Cl1 Fe1 S1 C18 159.79(6) . . . . ? N2 Fe1 S1 C19 11.04(8) . . . . ? N1 Fe1 S1 C19 92.14(15) . . . . ? N3 Fe1 S1 C19 87.17(8) . . . . ? N5 Fe1 S1 C19 165.71(8) . . . . ? Cl1 Fe1 S1 C19 -87.53(7) . . . . ? N1 C1 C2 C3 -0.5(3) . . . . ? C1 C2 C3 C4 0.7(3) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C3 C4 C5 N1 -0.7(3) . . . . ? C3 C4 C5 C6 -179.10(16) . . . . ? N1 C5 C6 N3 40.25(19) . . . . ? C4 C5 C6 N3 -141.21(16) . . . . ? N1 C5 C6 C7 -76.06(17) . . . . ? C4 C5 C6 C7 102.48(19) . . . . ? N3 C6 C7 N2 -44.50(19) . . . . ? C5 C6 C7 N2 72.70(18) . . . . ? N3 C6 C7 C8 138.51(17) . . . . ? C5 C6 C7 C8 -104.29(19) . . . . ? N2 C7 C8 C9 1.2(3) . . . . ? C6 C7 C8 C9 177.90(16) . . . . ? C7 C8 C9 C10 -0.8(3) . . . . ? C8 C9 C10 C11 -0.3(3) . . . . ? C9 C10 C11 N2 1.2(3) . . . . ? N3 C12 C13 C14 112.68(18) . . . . ? N3 C12 C13 C18 -67.7(2) . . . . ? C18 C13 C14 C15 1.4(3) . . . . ? C12 C13 C14 C15 -179.06(16) . . . . ? C13 C14 C15 C16 -1.0(3) . . . . ? C14 C15 C16 C17 0.2(3) . . . . ? C15 C16 C17 C18 0.3(3) . . . . ? C16 C17 C18 C13 0.0(3) . . . . ? C16 C17 C18 S1 177.41(14) . . . . ? C14 C13 C18 C17 -0.9(3) . . . . ? C12 C13 C18 C17 179.57(16) . . . . ? C14 C13 C18 S1 -178.11(13) . . . . ? C12 C13 C18 S1 2.3(2) . . . . ? C19 S1 C18 C17 103.65(15) . . . . ? Fe1 S1 C18 C17 -137.65(13) . . . . ? C19 S1 C18 C13 -79.02(16) . . . . ? Fe1 S1 C18 C13 39.67(15) . . . . ? C18 S1 C19 C20 -58.81(16) . . . . ? Fe1 S1 C19 C20 -174.62(12) . . . . ? S1 C19 C20 C21 -55.5(2) . . . . ? N3 C22 C23 N5 36.0(2) . . . . ? N3 C22 C23 C24 -145.94(16) . . . . ? N5 C23 C24 C25 1.3(3) . . . . ? C22 C23 C24 C25 -176.65(17) . . . . ? C23 C24 C25 C26 -1.5(3) . . . . ? C24 C25 C26 C27 0.0(3) . . . . ? C25 C26 C27 N5 1.8(3) . . . . ? C25 C26 C27 N6 -175.88(17) . . . . ? O1 C28 C29 C31 6.7(2) . . . . ? N6 C28 C29 C31 -171.79(16) . . . . ? O1 C28 C29 C32 125.56(19) . . . . ? N6 C28 C29 C32 -53.0(2) . . . . ? O1 C28 C29 C30 -112.2(2) . . . . ? N6 C28 C29 C30 69.3(2) . . . . ? C2 C1 N1 C5 -0.3(3) . . . . ? C2 C1 N1 Fe1 176.48(13) . . . . ? C4 C5 N1 C1 0.9(3) . . . . ? C6 C5 N1 C1 179.46(15) . . . . ? C4 C5 N1 Fe1 -176.47(13) . . . . ? C6 C5 N1 Fe1 2.07(17) . . . . ? N2 Fe1 N1 C1 -127.08(16) . . . . ? N3 Fe1 N1 C1 155.55(16) . . . . ? N5 Fe1 N1 C1 79.27(16) . . . . ? Cl1 Fe1 N1 C1 -29.92(16) . . . . ? S1 Fe1 N1 C1 150.42(13) . . . . ? N2 Fe1 N1 C5 49.88(12) . . . . ? N3 Fe1 N1 C5 -27.49(11) . . . . ? N5 Fe1 N1 C5 -103.77(12) . . . . ? Cl1 Fe1 N1 C5 147.04(11) . . . . ? S1 Fe1 N1 C5 -32.6(2) . . . . ? C10 C11 N2 C7 -0.9(3) . . . . ? C10 C11 N2 Fe1 178.24(13) . . . . ? C8 C7 N2 C11 -0.3(3) . . . . ? C6 C7 N2 C11 -177.30(15) . . . . ? C8 C7 N2 Fe1 -179.60(13) . . . . ? C6 C7 N2 Fe1 3.38(18) . . . . ? N1 Fe1 N2 C11 127.90(16) . . . . ? N3 Fe1 N2 C11 -155.61(17) . . . . ? N5 Fe1 N2 C11 -141.16(15) . . . . ? Cl1 Fe1 N2 C11 25.45(16) . . . . ? S1 Fe1 N2 C11 -69.19(16) . . . . ? N1 Fe1 N2 C7 -52.87(12) . . . . ? N3 Fe1 N2 C7 23.62(11) . . . . ? N5 Fe1 N2 C7 38.07(19) . . . . ? Cl1 Fe1 N2 C7 -155.32(11) . . . . ? S1 Fe1 N2 C7 110.04(11) . . . . ? C23 C22 N3 C12 91.51(17) . . . . ? C23 C22 N3 C6 -146.33(14) . . . . ? C23 C22 N3 Fe1 -39.53(16) . . . . ? C13 C12 N3 C22 -52.71(19) . . . . ? C13 C12 N3 C6 -177.99(14) . . . . ? C13 C12 N3 Fe1 71.47(16) . . . . ? C5 C6 N3 C22 54.13(18) . . . . ? C7 C6 N3 C22 170.20(14) . . . . ? C5 C6 N3 C12 177.86(14) . . . . ? C7 C6 N3 C12 -66.08(16) . . . . ? C5 C6 N3 Fe1 -57.90(13) . . . . ? C7 C6 N3 Fe1 58.17(13) . . . . ? N2 Fe1 N3 C22 -160.77(11) . . . . ? N1 Fe1 N3 C22 -73.42(10) . . . . ? N5 Fe1 N3 C22 25.69(10) . . . . ? S1 Fe1 N3 C22 105.06(10) . . . . ? N2 Fe1 N3 C12 72.89(12) . . . . ? N1 Fe1 N3 C12 160.24(12) . . . . ? N5 Fe1 N3 C12 -100.65(12) . . . . ? S1 Fe1 N3 C12 -21.28(11) . . . . ? N2 Fe1 N3 C6 -43.13(9) . . . . ? N1 Fe1 N3 C6 44.22(9) . . . . ? N5 Fe1 N3 C6 143.34(10) . . . . ? S1 Fe1 N3 C6 -137.30(9) . . . . ? N6 C27 N5 C23 175.82(15) . . . . ? C26 C27 N5 C23 -2.0(2) . . . . ? N6 C27 N5 Fe1 7.8(2) . . . . ? C26 C27 N5 Fe1 -170.00(13) . . . . ? C24 C23 N5 C27 0.4(2) . . . . ? C22 C23 N5 C27 178.40(15) . . . . ? C24 C23 N5 Fe1 170.59(14) . . . . ? C22 C23 N5 Fe1 -11.41(18) . . . . ? N2 Fe1 N5 C27 145.80(15) . . . . ? N1 Fe1 N5 C27 -125.96(15) . . . . ? N3 Fe1 N5 C27 160.14(15) . . . . ? Cl1 Fe1 N5 C27 -20.31(15) . . . . ? S1 Fe1 N5 C27 70.61(14) . . . . ? N2 Fe1 N5 C23 -22.83(19) . . . . ? N1 Fe1 N5 C23 65.40(12) . . . . ? N3 Fe1 N5 C23 -8.49(11) . . . . ? Cl1 Fe1 N5 C23 171.05(10) . . . . ? S1 Fe1 N5 C23 -98.03(11) . . . . ? O1 C28 N6 C27 -8.0(3) . . . . ? C29 C28 N6 C27 170.50(16) . . . . ? N5 C27 N6 C28 176.38(16) . . . . ? C26 C27 N6 C28 -5.8(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.471 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.060 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6A Cl1 0.81(2) 2.50(2) 3.2945(16) 167.2(19) . _iucr_refine_instructions_details ; TITL x1065a CELL 0.71073 25.4707 9.98637 25.8674 90.0000 94.8579 90.0000 ZERR 8 0.0003 0.00013 0.0003 0.0000 0.0012 0.0000 LATT 7 SYMM -X,Y,1/2-Z SFAC C H B N O F S FE Cl UNIT 256 272 8 48 8 32 8 8 8 TEMP -163 ACTA HTAB BOND BOND $H CONF WPDB L.S. 6 FMAP 2 PLAN 10 OMIT -2 52.5 WGHT 0.033800 7.332800 FVAR 0.99291 PART 0 rem Fe complex FE1 8 0.100505 0.989112 0.344272 11.00000 0.01436 0.01624 = 0.01727 -0.00287 0.00021 0.00144 CL1 9 0.093125 0.830451 0.280859 11.00000 0.02329 0.02809 = 0.02597 -0.01113 -0.00552 0.00560 S1 7 0.113536 0.815403 0.419360 11.00000 0.02018 0.01764 = 0.01959 -0.00145 0.00196 -0.00037 C1 1 0.104208 1.209206 0.252714 11.00000 0.01833 0.02805 = 0.01922 -0.00252 0.00048 -0.00036 AFIX 43 H1 2 0.121356 1.143750 0.233476 11.00000 -1.20000 AFIX 0 C2 1 0.093107 1.333272 0.230173 11.00000 0.02024 0.03204 = 0.01896 0.00269 -0.00084 -0.00580 AFIX 43 H2 2 0.102781 1.352263 0.196268 11.00000 -1.20000 AFIX 0 C3 1 0.067828 1.428702 0.257660 11.00000 0.01704 0.02444 = 0.02584 0.00522 -0.00383 -0.00216 AFIX 43 H3 2 0.059493 1.513906 0.242827 11.00000 -1.20000 AFIX 0 C4 1 0.054768 1.398030 0.307429 11.00000 0.01425 0.01976 = 0.02640 -0.00069 -0.00013 -0.00051 AFIX 43 H4 2 0.037440 1.461809 0.327279 11.00000 -1.20000 AFIX 0 C5 1 0.067557 1.272726 0.327358 11.00000 0.01269 0.01972 = 0.02035 -0.00068 -0.00045 -0.00059 C6 1 0.054540 1.228199 0.380601 11.00000 0.01591 0.01571 = 0.01987 -0.00176 0.00138 0.00323 AFIX 13 H6 2 0.047210 1.306958 0.402756 11.00000 -1.20000 AFIX 0 C7 1 0.006736 1.137013 0.373204 11.00000 0.01754 0.01898 = 0.01523 0.00305 0.00075 0.00242 C8 1 -0.043416 1.176363 0.382914 11.00000 0.01935 0.02172 = 0.01872 0.00215 0.00219 0.00422 AFIX 43 H8 2 -0.049715 1.263278 0.395978 11.00000 -1.20000 AFIX 0 C9 1 -0.084551 1.085728 0.373119 11.00000 0.01625 0.03041 = 0.02486 0.00503 0.00398 0.00262 AFIX 43 H9 2 -0.119429 1.109570 0.379857 11.00000 -1.20000 AFIX 0 C10 1 -0.074161 0.960658 0.353488 11.00000 0.01788 0.02682 = 0.02545 0.00494 -0.00171 -0.00257 AFIX 43 H10 2 -0.101682 0.897232 0.346707 11.00000 -1.20000 AFIX 0 C11 1 -0.022782 0.929409 0.343859 11.00000 0.01965 0.02092 = 0.02357 0.00009 -0.00159 -0.00025 AFIX 43 H11 2 -0.015689 0.844155 0.329718 11.00000 -1.20000 AFIX 0 C12 1 0.086693 1.108513 0.458250 11.00000 0.01824 0.01845 = 0.01788 -0.00159 0.00382 0.00034 AFIX 23 H12A 2 0.053980 1.054511 0.455509 11.00000 -1.20000 H12B 2 0.079747 1.190844 0.477871 11.00000 -1.20000 AFIX 0 C13 1 0.129580 1.029802 0.488323 11.00000 0.01792 0.02004 = 0.01489 0.00165 0.00401 -0.00072 C14 1 0.156460 1.088901 0.531755 11.00000 0.02398 0.02069 = 0.02116 -0.00124 0.00388 -0.00189 AFIX 43 H14 2 0.146994 1.176504 0.541863 11.00000 -1.20000 AFIX 0 C15 1 0.196714 1.021804 0.560339 11.00000 0.02547 0.03146 = 0.01907 0.00114 -0.00114 -0.00551 AFIX 43 H15 2 0.214946 1.064171 0.589450 11.00000 -1.20000 AFIX 0 C16 1 0.210436 0.893856 0.546737 11.00000 0.02079 0.03133 = 0.02487 0.00487 -0.00064 0.00236 AFIX 43 H16 2 0.238003 0.847977 0.566458 11.00000 -1.20000 AFIX 0 C17 1 0.183872 0.832397 0.504190 11.00000 0.02218 0.02207 = 0.02429 0.00209 0.00296 0.00259 AFIX 43 H17 2 0.193188 0.744024 0.494903 11.00000 -1.20000 AFIX 0 C18 1 0.143717 0.899140 0.475031 11.00000 0.01673 0.02104 = 0.01793 0.00018 0.00300 -0.00215 C19 1 0.051213 0.759355 0.441031 11.00000 0.02236 0.02208 = 0.02692 0.00061 0.00357 -0.00493 AFIX 23 H19A 2 0.030270 0.838596 0.449614 11.00000 -1.20000 H19B 2 0.031246 0.711172 0.412255 11.00000 -1.20000 AFIX 0 C20 1 0.057705 0.667804 0.488175 11.00000 0.03938 0.02359 = 0.02371 -0.00158 0.00621 -0.00801 AFIX 23 H20A 2 0.073700 0.719031 0.518272 11.00000 -1.20000 H20B 2 0.022582 0.636491 0.496697 11.00000 -1.20000 AFIX 0 C21 1 0.090565 0.552729 0.479287 11.00000 0.05817 0.02181 = 0.02324 0.00096 -0.00252 -0.00476 C22 1 0.150854 1.216108 0.406477 11.00000 0.01805 0.01596 = 0.02002 -0.00238 0.00151 -0.00155 AFIX 23 H22A 2 0.157215 1.264178 0.439893 11.00000 -1.20000 H22B 2 0.149704 1.283368 0.378288 11.00000 -1.20000 AFIX 0 C23 1 0.195866 1.120595 0.400414 11.00000 0.01801 0.01576 = 0.01658 0.00140 0.00373 -0.00156 C24 1 0.244362 1.146662 0.426424 11.00000 0.01961 0.01965 = 0.02177 -0.00521 0.00103 -0.00340 AFIX 43 H24 2 0.248929 1.220972 0.449293 11.00000 -1.20000 AFIX 0 C25 1 0.286200 1.062828 0.418650 11.00000 0.01521 0.02660 = 0.02690 -0.00495 -0.00151 -0.00179 AFIX 43 H25 2 0.320084 1.080318 0.435547 11.00000 -1.20000 AFIX 0 C26 1 0.278475 0.954192 0.386372 11.00000 0.01600 0.02152 = 0.02353 -0.00133 -0.00015 0.00138 AFIX 43 H26 2 0.306780 0.895590 0.380626 11.00000 -1.20000 AFIX 0 C27 1 0.228023 0.931565 0.362102 11.00000 0.01586 0.01584 = 0.01578 0.00036 0.00243 -0.00169 C28 1 0.250779 0.721812 0.316576 11.00000 0.01919 0.01837 = 0.01777 0.00063 0.00448 0.00052 C29 1 0.225264 0.598019 0.290121 11.00000 0.02024 0.01873 = 0.02179 -0.00220 0.00278 -0.00016 C30 1 0.199212 0.633530 0.235878 11.00000 0.03170 0.02397 = 0.02066 -0.00386 0.00386 -0.00232 AFIX 137 H30A 2 0.172223 0.702237 0.239154 11.00000 -1.50000 H30B 2 0.182851 0.553252 0.219778 11.00000 -1.50000 H30C 2 0.226003 0.667672 0.214223 11.00000 -1.50000 AFIX 0 C31 1 0.268291 0.493659 0.283810 11.00000 0.02861 0.02353 = 0.03635 -0.00786 0.00447 0.00350 AFIX 137 H31A 2 0.293395 0.528631 0.260479 11.00000 -1.50000 H31B 2 0.252241 0.411337 0.269157 11.00000 -1.50000 H31C 2 0.286779 0.474211 0.317755 11.00000 -1.50000 AFIX 0 C32 1 0.184506 0.538878 0.324184 11.00000 0.02473 0.01982 = 0.02566 0.00019 0.00184 -0.00418 AFIX 137 H32A 2 0.200722 0.526319 0.359575 11.00000 -1.50000 H32B 2 0.172247 0.452323 0.309968 11.00000 -1.50000 H32C 2 0.154536 0.600248 0.324748 11.00000 -1.50000 AFIX 0 N1 4 0.091709 1.178229 0.300438 11.00000 0.01503 0.02066 = 0.01947 -0.00054 -0.00047 -0.00021 N2 4 0.017085 1.015404 0.353839 11.00000 0.01564 0.01829 = 0.02013 -0.00008 -0.00095 0.00093 N3 4 0.099415 1.146966 0.405044 11.00000 0.01524 0.01616 = 0.01572 0.00071 0.00180 0.00099 N4 4 0.117327 0.464928 0.472154 11.00000 0.08720 0.03229 = 0.04282 -0.00445 -0.00282 0.01864 N5 4 0.187189 1.014630 0.368277 11.00000 0.01313 0.01694 = 0.01531 -0.00049 0.00147 -0.00101 N6 4 0.216221 0.818501 0.331293 11.00000 0.01135 0.01842 = 0.02117 -0.00335 -0.00023 -0.00026 H6A 2 0.185265 0.809522 0.321371 11.00000 0.01629 O1 5 0.298310 0.732563 0.324963 11.00000 0.01571 0.03006 = 0.03971 -0.01331 0.00280 0.00066 rem counterion B1 3 -0.060010 0.563118 0.395456 11.00000 0.02403 0.02213 = 0.02925 -0.00415 0.00588 -0.00132 F1 6 -0.049582 0.608948 0.347476 11.00000 0.10294 0.03782 = 0.03056 0.00306 0.01058 -0.00768 F2 6 -0.014761 0.496513 0.416938 11.00000 0.02642 0.02827 = 0.05931 -0.00713 -0.00626 0.00070 F3 6 -0.100911 0.471785 0.392715 11.00000 0.01948 0.03397 = 0.06971 -0.01654 0.00635 -0.00405 F4 6 -0.070268 0.669651 0.427447 11.00000 0.04115 0.02762 = 0.05076 -0.01455 0.01560 -0.00030 HKLF 4 REM x1065a REM R1 = 0.0317 for 5537 Fo > 4sig(Fo) and 0.0418 for all 6622 data REM 431 parameters refined using 0 restraints END WGHT 0.0334 7.3996 REM Highest difference peak 0.471, deepest hole -0.392, 1-sigma level 0.060 Q1 1 -0.0870 0.6218 0.3462 11.00000 0.05 0.47 Q2 1 0.1530 0.4907 0.4672 11.00000 0.05 0.46 Q3 1 -0.0171 0.5320 0.3846 11.00000 0.05 0.43 Q4 1 0.2524 0.9192 0.3822 11.00000 0.05 0.30 Q5 1 0.1105 1.0674 0.4723 11.00000 0.05 0.29 Q6 1 0.2433 0.5512 0.2882 11.00000 0.05 0.29 Q7 1 0.1230 0.5595 0.4782 11.00000 0.05 0.29 Q8 1 0.2099 0.6068 0.2685 11.00000 0.05 0.29 Q9 1 0.2360 0.6581 0.3012 11.00000 0.05 0.27 Q10 1 0.1326 1.0437 0.5161 11.00000 0.05 0.27 ;