data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H25 B1.82 Cl0.18 F7.27 Fe N6 O2' _chemical_formula_weight 649.64 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' '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 orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 17.0215(3) _cell_length_b 12.70711(18) _cell_length_c 12.66693(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2739.78(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9379 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 26.32 _exptl_crystal_description plate _exptl_crystal_colour "orange-red" _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1322.3 _exptl_absorpt_coefficient_mu 0.653 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 0.968 _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 18464 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 26.24 _reflns_number_total 5214 _reflns_number_gt 4802 _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^)+(0.0572P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(13) _refine_ls_number_reflns 5214 _refine_ls_number_parameters 476 _refine_ls_number_restraints 544 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.024 _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 0.259217(16) 0.84692(2) 0.31832(4) 0.01493(9) Uani 1 1 d . . . C1 C 0.25089(15) 0.95529(19) 0.1092(2) 0.0230(5) Uani 1 1 d . . . H1 H 0.3050 0.9721 0.1167 0.028 Uiso 1 1 calc R . . C2 C 0.21128(18) 0.9869(2) 0.0191(2) 0.0289(6) Uani 1 1 d . . . H2 H 0.2381 1.0243 -0.0350 0.035 Uiso 1 1 calc R . . C3 C 0.13267(18) 0.9636(2) 0.0086(2) 0.0303(6) Uani 1 1 d . . . H3 H 0.1048 0.9849 -0.0528 0.036 Uiso 1 1 calc R . . C4 C 0.09433(16) 0.90861(19) 0.0884(2) 0.0259(6) Uani 1 1 d . . . H4 H 0.0401 0.8918 0.0826 0.031 Uiso 1 1 calc R . . C5 C 0.13683(14) 0.87937(19) 0.17555(19) 0.0190(5) Uani 1 1 d . . . C6 C 0.10696(14) 0.81570(18) 0.2679(2) 0.0175(5) Uani 1 1 d . . . H6 H 0.0483 0.8142 0.2716 0.021 Uiso 1 1 calc R . . C7 C 0.14212(13) 0.70749(18) 0.25377(19) 0.0190(5) Uani 1 1 d . . . C8 C 0.10140(15) 0.61928(19) 0.2230(2) 0.0231(5) Uani 1 1 d . . . H8 H 0.0461 0.6216 0.2126 0.028 Uiso 1 1 calc R . . C9 C 0.14328(17) 0.5266(2) 0.2074(2) 0.0278(6) Uani 1 1 d . . . H9 H 0.1168 0.4645 0.1856 0.033 Uiso 1 1 calc R . . C10 C 0.22347(16) 0.52528(19) 0.2238(2) 0.0263(6) Uani 1 1 d . . . H10 H 0.2527 0.4625 0.2131 0.032 Uiso 1 1 calc R . . C11 C 0.26097(15) 0.6172(2) 0.2562(2) 0.0224(5) Uani 1 1 d . . . H11 H 0.3160 0.6163 0.2684 0.027 Uiso 1 1 calc R . . C12 C 0.34291(15) 0.77466(18) 0.5109(2) 0.0220(5) Uani 1 1 d . . . H12 H 0.3900 0.7858 0.4721 0.026 Uiso 1 1 calc R . . C13 C 0.34750(16) 0.74059(19) 0.6141(2) 0.0273(6) Uani 1 1 d . . . H13 H 0.3971 0.7276 0.6460 0.033 Uiso 1 1 calc R . . C14 C 0.27928(17) 0.72580(19) 0.6701(2) 0.0270(6) Uani 1 1 d . . . H14 H 0.2816 0.7025 0.7413 0.032 Uiso 1 1 calc R . . C15 C 0.20739(16) 0.74467(19) 0.6233(2) 0.0244(5) Uani 1 1 d . . . H15 H 0.1599 0.7351 0.6615 0.029 Uiso 1 1 calc R . . C16 C 0.20639(14) 0.77806(17) 0.51906(19) 0.0190(5) Uani 1 1 d . . . C17 C 0.13009(14) 0.79674(19) 0.46090(19) 0.0199(5) Uani 1 1 d . . . H17A H 0.1067 0.7283 0.4407 0.024 Uiso 1 1 calc R . . H17B H 0.0926 0.8334 0.5080 0.024 Uiso 1 1 calc R . . C18 C 0.12516(14) 0.97520(18) 0.38163(19) 0.0190(5) Uani 1 1 d . . . H18A H 0.0865 0.9825 0.4395 0.023 Uiso 1 1 calc R . . H18B H 0.1018 1.0052 0.3167 0.023 Uiso 1 1 calc R . . C19 C 0.19873(14) 1.03435(18) 0.40923(18) 0.0186(5) Uani 1 1 d . . . C20 C 0.19562(15) 1.1312(2) 0.4606(2) 0.0230(5) Uani 1 1 d . . . H20 H 0.1472 1.1581 0.4863 0.028 Uiso 1 1 calc R . . C21 C 0.26503(17) 1.1876(2) 0.4734(2) 0.0263(6) Uani 1 1 d . . . H21 H 0.2643 1.2547 0.5064 0.032 Uiso 1 1 calc R . . C22 C 0.33515(17) 1.1454(2) 0.4377(2) 0.0287(6) Uani 1 1 d . . . H22 H 0.3830 1.1830 0.4456 0.034 Uiso 1 1 calc R . . C23 C 0.33403(15) 1.04654(19) 0.3900(2) 0.0237(5) Uani 1 1 d . . . H23 H 0.3821 1.0165 0.3668 0.028 Uiso 1 1 calc R . . N1 N 0.21478(12) 0.90188(14) 0.18552(15) 0.0169(4) Uani 1 1 d . . . N2 N 0.22077(12) 0.70707(14) 0.27043(16) 0.0169(4) Uani 1 1 d . . . N3 N 0.27311(12) 0.79255(15) 0.46360(16) 0.0185(4) Uani 1 1 d . . . N4 N 0.14334(12) 0.86137(15) 0.36448(17) 0.0162(4) Uani 1 1 d . . . N5 N 0.26724(11) 0.99259(16) 0.37591(16) 0.0180(4) Uani 1 1 d . . . N6 N 0.35447(12) 0.83093(16) 0.27294(18) 0.0218(4) Uani 1 1 d . . . O1 O 0.39364(13) 0.78931(19) 0.2111(2) 0.0595(7) Uani 1 1 d . . . B1 B 0.06113(11) 0.95763(15) 0.72287(16) 0.0155(5) Uani 0.923(2) 1 d PU A 1 F1 F 0.09434(12) 0.99236(17) 0.62747(15) 0.0431(5) Uani 0.923(2) 1 d PU A 1 F2 F -0.00993(10) 0.90828(13) 0.70181(16) 0.0389(5) Uani 0.923(2) 1 d PU A 1 F3 F 0.04704(9) 1.04687(11) 0.78622(12) 0.0232(4) Uani 0.923(2) 1 d PU A 1 F4 F 0.11263(10) 0.89158(14) 0.77361(15) 0.0366(4) Uani 0.923(2) 1 d PU A 1 Cl1 Cl 0.06113(11) 0.95763(15) 0.72287(16) 0.0155(5) Uani 0.077(2) 1 d PU B 2 B2 B 0.0368(9) 0.5553(13) 0.5675(12) 0.0323(8) Uani 0.259(3) 1 d PDU C 1 F5 F 0.1019(9) 0.5601(15) 0.4951(17) 0.0281(12) Uani 0.259(3) 1 d PDU C 1 F6 F 0.0097(9) 0.6589(9) 0.5780(12) 0.046(3) Uani 0.259(3) 1 d PDU C 1 F7 F 0.0599(4) 0.5155(7) 0.6585(6) 0.0397(17) Uani 0.259(3) 1 d PDU C 1 F8 F -0.0248(6) 0.5058(11) 0.5179(10) 0.056(2) Uani 0.259(3) 1 d PDU C 1 B2' B 0.0305(7) 0.5594(9) 0.5160(10) 0.0323(8) Uani 0.394(6) 1 d PDU D 2 F5' F 0.1114(7) 0.5401(10) 0.4892(15) 0.0281(12) Uani 0.394(6) 1 d PDU D 2 F6' F 0.0333(9) 0.6288(8) 0.6044(10) 0.050(2) Uani 0.394(6) 1 d PDU D 2 F7' F -0.0039(4) 0.4642(4) 0.5452(5) 0.0421(17) Uani 0.394(6) 1 d PDU D 2 F8' F -0.0057(3) 0.6020(5) 0.4320(4) 0.0364(13) Uani 0.394(6) 1 d PDU D 2 B2C B 0.0417(4) 0.5553(5) 0.5426(5) 0.0323(8) Uani 0.240(6) 1 d PDU E 3 F5C F 0.1155(9) 0.5653(16) 0.489(2) 0.0281(12) Uani 0.240(6) 1 d PDU E 3 F6C F 0.0245(13) 0.6464(13) 0.6010(16) 0.038(3) Uani 0.240(6) 1 d PDU E 3 F7C F 0.0469(5) 0.4626(6) 0.5999(8) 0.041(2) Uani 0.240(6) 1 d PDU E 3 F8C F -0.0157(6) 0.5534(9) 0.4665(11) 0.052(2) Uani 0.240(6) 1 d PDU E 3 Cl2 Cl 0.0417(4) 0.5553(5) 0.5426(5) 0.0323(8) Uani 0.107(3) 1 d PU F 4 O1S O 0.03029(19) 0.2709(3) 0.4722(3) 0.0412(11) Uani 0.781(9) 1 d PDU G 1 H1S H 0.0311 0.3234 0.5125 0.062 Uiso 1 1 calc R G 1 C1S C 0.0418(5) 0.3038(6) 0.3685(8) 0.0516(15) Uani 0.781(9) 1 d PDU G 1 H1S1 H 0.0066 0.3629 0.3529 0.077 Uiso 0.781(9) 1 calc PR G 1 H1S2 H 0.0304 0.2455 0.3202 0.077 Uiso 0.781(9) 1 calc PR G 1 H1S3 H 0.0965 0.3262 0.3593 0.077 Uiso 0.781(9) 1 calc PR G 1 O1' O 0.0181(8) 0.2189(13) 0.4130(14) 0.066(4) Uani 0.219(9) 1 d PDU G 2 C1' C 0.060(2) 0.295(3) 0.359(3) 0.0516(15) Uani 0.219(9) 1 d PDU G 2 H1'1 H 0.0845 0.3431 0.4102 0.077 Uiso 0.219(9) 1 calc PR G 2 H1'2 H 0.0240 0.3353 0.3139 0.077 Uiso 0.219(9) 1 calc PR G 2 H1'3 H 0.1004 0.2620 0.3159 0.077 Uiso 0.219(9) 1 calc PR G 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 0.01467(15) 0.01674(14) 0.01339(15) 0.00015(15) -0.00077(18) 0.00025(11) C1 0.0301(14) 0.0182(12) 0.0207(13) -0.0037(10) 0.0027(11) -0.0019(10) C2 0.0449(17) 0.0238(12) 0.0180(13) 0.0030(10) 0.0013(12) 0.0045(12) C3 0.0470(18) 0.0302(14) 0.0136(12) 0.0014(11) -0.0092(13) 0.0095(12) C4 0.0305(14) 0.0257(12) 0.0215(13) -0.0063(11) -0.0072(11) 0.0070(11) C5 0.0216(12) 0.0194(11) 0.0160(12) -0.0066(10) -0.0035(10) 0.0028(10) C6 0.0161(11) 0.0204(11) 0.0158(12) -0.0036(10) -0.0038(10) -0.0008(9) C7 0.0216(12) 0.0207(11) 0.0146(11) 0.0008(9) 0.0014(10) -0.0009(9) C8 0.0226(13) 0.0251(12) 0.0215(13) -0.0027(10) -0.0015(11) -0.0027(10) C9 0.0351(15) 0.0227(12) 0.0256(14) -0.0030(11) 0.0036(12) -0.0061(11) C10 0.0336(14) 0.0165(12) 0.0288(15) -0.0003(10) 0.0011(12) 0.0013(10) C11 0.0237(13) 0.0228(12) 0.0207(14) 0.0021(11) 0.0011(10) 0.0042(9) C12 0.0217(12) 0.0195(11) 0.0248(13) -0.0002(10) -0.0028(11) 0.0021(9) C13 0.0329(14) 0.0217(12) 0.0274(14) -0.0014(11) -0.0141(12) 0.0048(11) C14 0.0441(16) 0.0207(12) 0.0161(13) 0.0024(10) -0.0073(12) -0.0003(12) C15 0.0344(14) 0.0191(12) 0.0198(13) -0.0004(10) 0.0014(12) -0.0012(10) C16 0.0222(12) 0.0140(10) 0.0209(12) -0.0020(9) 0.0011(10) 0.0000(9) C17 0.0218(13) 0.0214(12) 0.0167(12) 0.0007(10) 0.0004(10) -0.0023(10) C18 0.0179(12) 0.0189(11) 0.0201(13) -0.0026(10) -0.0010(10) 0.0030(9) C19 0.0223(13) 0.0197(11) 0.0137(11) 0.0002(9) -0.0024(10) 0.0014(9) C20 0.0272(14) 0.0245(12) 0.0174(12) -0.0014(10) -0.0002(11) 0.0010(10) C21 0.0344(15) 0.0210(13) 0.0236(14) -0.0053(11) -0.0062(12) -0.0043(11) C22 0.0267(14) 0.0273(13) 0.0321(16) -0.0019(12) -0.0044(12) -0.0073(11) C23 0.0201(12) 0.0243(12) 0.0268(14) -0.0016(10) -0.0007(11) -0.0045(10) N1 0.0210(10) 0.0157(9) 0.0141(10) -0.0014(8) -0.0016(8) 0.0016(8) N2 0.0207(10) 0.0169(9) 0.0130(9) 0.0015(8) -0.0004(9) 0.0003(8) N3 0.0206(11) 0.0178(10) 0.0172(11) -0.0005(8) -0.0046(9) 0.0017(8) N4 0.0169(10) 0.0164(9) 0.0152(9) 0.0007(8) -0.0008(8) 0.0008(8) N5 0.0202(10) 0.0190(10) 0.0147(11) 0.0015(8) -0.0026(9) -0.0014(8) N6 0.0190(10) 0.0238(10) 0.0227(11) 0.0026(9) 0.0049(9) 0.0021(8) O1 0.0357(13) 0.0581(15) 0.085(2) -0.0239(15) 0.0312(13) -0.0049(11) B1 0.0114(10) 0.0226(10) 0.0125(10) -0.0060(8) -0.0007(8) 0.0014(7) F1 0.0464(12) 0.0643(12) 0.0185(9) -0.0032(9) 0.0112(9) -0.0032(10) F2 0.0294(10) 0.0345(9) 0.0526(12) -0.0089(9) -0.0081(9) -0.0076(7) F3 0.0227(8) 0.0250(8) 0.0219(8) -0.0048(6) -0.0006(6) 0.0037(6) F4 0.0367(10) 0.0380(9) 0.0351(10) -0.0102(8) -0.0060(9) 0.0162(8) Cl1 0.0114(10) 0.0226(10) 0.0125(10) -0.0060(8) -0.0007(8) 0.0014(7) B2 0.0194(15) 0.0257(11) 0.052(2) 0.0080(15) 0.0014(15) -0.0062(10) F5 0.0251(19) 0.019(4) 0.0408(14) 0.007(3) -0.0008(13) 0.003(2) F6 0.030(5) 0.042(3) 0.067(6) 0.009(3) 0.011(4) 0.021(3) F7 0.022(3) 0.061(4) 0.036(3) 0.012(3) 0.006(3) 0.012(3) F8 0.037(4) 0.074(5) 0.056(5) -0.004(5) -0.003(3) -0.028(4) B2' 0.0194(15) 0.0257(11) 0.052(2) 0.0080(15) 0.0014(15) -0.0062(10) F5' 0.0251(19) 0.019(4) 0.0408(14) 0.007(3) -0.0008(13) 0.003(2) F6' 0.049(5) 0.053(5) 0.048(3) -0.010(4) 0.012(3) -0.002(4) F7' 0.052(4) 0.024(2) 0.051(3) 0.016(2) 0.017(3) -0.006(2) F8' 0.024(2) 0.039(3) 0.046(3) 0.014(2) -0.001(2) -0.0006(19) B2C 0.0194(15) 0.0257(11) 0.052(2) 0.0080(15) 0.0014(15) -0.0062(10) F5C 0.0251(19) 0.019(4) 0.0408(14) 0.007(3) -0.0008(13) 0.003(2) F6C 0.029(6) 0.034(4) 0.050(6) 0.007(4) -0.003(4) 0.023(4) F7C 0.034(4) 0.034(3) 0.055(5) 0.020(3) 0.019(4) 0.005(3) F8C 0.037(4) 0.044(5) 0.073(5) 0.005(4) -0.020(4) 0.007(4) Cl2 0.0194(15) 0.0257(11) 0.052(2) 0.0080(15) 0.0014(15) -0.0062(10) O1S 0.0464(18) 0.0418(18) 0.0355(19) 0.0059(15) 0.0103(14) 0.0067(14) C1S 0.044(4) 0.066(3) 0.045(3) 0.005(3) 0.023(3) 0.018(3) O1' 0.066(7) 0.064(7) 0.067(8) 0.007(7) 0.011(6) 0.003(6) C1' 0.044(4) 0.066(3) 0.045(3) 0.005(3) 0.023(3) 0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N6 1.732(2) . ? Fe1 N1 1.972(2) . ? Fe1 N3 1.980(2) . ? Fe1 N2 1.9886(19) . ? Fe1 N5 1.994(2) . ? Fe1 N4 2.065(2) . ? C1 N1 1.331(3) . ? C1 C2 1.386(4) . ? C1 H1 0.9500 . ? C2 C3 1.377(4) . ? C2 H2 0.9500 . ? C3 C4 1.392(4) . ? C3 H3 0.9500 . ? C4 C5 1.371(4) . ? C4 H4 0.9500 . ? C5 N1 1.363(3) . ? C5 C6 1.510(4) . ? C6 N4 1.489(3) . ? C6 C7 1.510(3) . ? C6 H6 1.0000 . ? C7 N2 1.355(3) . ? C7 C8 1.374(3) . ? C8 C9 1.391(4) . ? C8 H8 0.9500 . ? C9 C10 1.381(4) . ? C9 H9 0.9500 . ? C10 C11 1.393(4) . ? C10 H10 0.9500 . ? C11 N2 1.343(3) . ? C11 H11 0.9500 . ? C12 N3 1.350(3) . ? C12 C13 1.380(4) . ? C12 H12 0.9500 . ? C13 C14 1.373(4) . ? C13 H13 0.9500 . ? C14 C15 1.380(4) . ? C14 H14 0.9500 . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 N3 1.348(3) . ? C16 C17 1.512(3) . ? C17 N4 1.489(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N4 1.495(3) . ? C18 C19 1.502(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N5 1.349(3) . ? C19 C20 1.392(3) . ? C20 C21 1.392(4) . ? C20 H20 0.9500 . ? C21 C22 1.384(4) . ? C21 H21 0.9500 . ? C22 C23 1.394(4) . ? C22 H22 0.9500 . ? C23 N5 1.339(3) . ? C23 H23 0.9500 . ? N6 O1 1.157(3) . ? B1 F4 1.373(3) . ? B1 F2 1.388(3) . ? B1 F1 1.405(3) . ? B1 F3 1.410(2) . ? B2 F7 1.319(13) . ? B2 F8 1.375(14) . ? B2 F6 1.402(14) . ? B2 F5 1.439(14) . ? B2' F8' 1.342(12) . ? B2' F7' 1.394(11) . ? B2' F6' 1.426(12) . ? B2' F5' 1.438(12) . ? B2C F8C 1.373(9) . ? B2C F7C 1.386(8) . ? B2C F6C 1.405(11) . ? B2C F5C 1.432(11) . ? O1S C1S 1.392(8) . ? O1S H1S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O1' C1' 1.381(18) . ? C1' H1'1 0.9800 . ? C1' H1'2 0.9800 . ? C1' H1'3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Fe1 N1 96.75(10) . . ? N6 Fe1 N3 98.96(10) . . ? N1 Fe1 N3 164.19(9) . . ? N6 Fe1 N2 95.86(9) . . ? N1 Fe1 N2 85.99(8) . . ? N3 Fe1 N2 90.63(8) . . ? N6 Fe1 N5 99.56(9) . . ? N1 Fe1 N5 90.55(8) . . ? N3 Fe1 N5 88.61(9) . . ? N2 Fe1 N5 164.49(8) . . ? N6 Fe1 N4 176.59(10) . . ? N1 Fe1 N4 81.01(8) . . ? N3 Fe1 N4 83.22(8) . . ? N2 Fe1 N4 81.46(8) . . ? N5 Fe1 N4 83.07(8) . . ? N1 C1 C2 121.4(2) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 119.3(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.6(2) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 118.3(2) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? N1 C5 C4 122.1(2) . . ? N1 C5 C6 111.6(2) . . ? C4 C5 C6 126.2(2) . . ? N4 C6 C5 106.71(17) . . ? N4 C6 C7 106.69(18) . . ? C5 C6 C7 105.24(19) . . ? N4 C6 H6 112.6 . . ? C5 C6 H6 112.6 . . ? C7 C6 H6 112.6 . . ? N2 C7 C8 122.6(2) . . ? N2 C7 C6 112.12(19) . . ? C8 C7 C6 125.2(2) . . ? C7 C8 C9 118.2(2) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C10 C9 C8 119.7(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 119.1(2) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N2 C11 C10 121.3(2) . . ? N2 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? N3 C12 C13 121.5(2) . . ? N3 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C14 C13 C12 119.0(2) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 120.3(2) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 118.2(2) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? N3 C16 C15 121.8(2) . . ? N3 C16 C17 116.6(2) . . ? C15 C16 C17 121.5(2) . . ? N4 C17 C16 110.86(19) . . ? N4 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? N4 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? N4 C18 C19 110.21(19) . . ? N4 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? N4 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? N5 C19 C20 121.8(2) . . ? N5 C19 C18 116.8(2) . . ? C20 C19 C18 121.3(2) . . ? C21 C20 C19 118.5(2) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C22 C21 C20 119.6(2) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 118.6(2) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? N5 C23 C22 122.0(2) . . ? N5 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C1 N1 C5 119.3(2) . . ? C1 N1 Fe1 128.52(18) . . ? C5 N1 Fe1 112.21(16) . . ? C11 N2 C7 119.0(2) . . ? C11 N2 Fe1 129.27(18) . . ? C7 N2 Fe1 111.66(15) . . ? C16 N3 C12 119.2(2) . . ? C16 N3 Fe1 115.56(16) . . ? C12 N3 Fe1 125.18(17) . . ? C17 N4 C6 113.33(17) . . ? C17 N4 C18 112.5(2) . . ? C6 N4 C18 114.23(18) . . ? C17 N4 Fe1 109.14(14) . . ? C6 N4 Fe1 97.46(14) . . ? C18 N4 Fe1 108.95(14) . . ? C23 N5 C19 119.4(2) . . ? C23 N5 Fe1 125.59(17) . . ? C19 N5 Fe1 114.86(16) . . ? O1 N6 Fe1 144.9(2) . . ? F4 B1 F2 111.72(18) . . ? F4 B1 F1 109.73(17) . . ? F2 B1 F1 109.09(18) . . ? F4 B1 F3 109.51(16) . . ? F2 B1 F3 108.94(16) . . ? F1 B1 F3 107.78(17) . . ? F7 B2 F8 116.8(13) . . ? F7 B2 F6 112.0(13) . . ? F8 B2 F6 102.8(13) . . ? F7 B2 F5 110.1(14) . . ? F8 B2 F5 108.4(14) . . ? F6 B2 F5 105.9(12) . . ? F8' B2' F7' 111.5(9) . . ? F8' B2' F6' 112.9(10) . . ? F7' B2' F6' 110.0(10) . . ? F8' B2' F5' 108.8(11) . . ? F7' B2' F5' 108.4(10) . . ? F6' B2' F5' 105.0(10) . . ? F8C B2C F7C 113.5(8) . . ? F8C B2C F6C 103.6(10) . . ? F7C B2C F6C 116.0(10) . . ? F8C B2C F5C 107.1(12) . . ? F7C B2C F5C 105.4(9) . . ? F6C B2C F5C 111.0(12) . . ? O1' C1' H1'1 109.5 . . ? O1' C1' H1'2 109.5 . . ? H1'1 C1' H1'2 109.5 . . ? O1' C1' H1'3 109.5 . . ? H1'1 C1' H1'3 109.5 . . ? H1'2 C1' H1'3 109.5 . . ? 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 0.7(4) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C2 C3 C4 C5 0.0(4) . . . . ? C3 C4 C5 N1 -0.4(4) . . . . ? C3 C4 C5 C6 -177.2(2) . . . . ? N1 C5 C6 N4 41.3(2) . . . . ? C4 C5 C6 N4 -141.6(2) . . . . ? N1 C5 C6 C7 -71.8(2) . . . . ? C4 C5 C6 C7 105.3(3) . . . . ? N4 C6 C7 N2 -43.3(3) . . . . ? C5 C6 C7 N2 69.8(2) . . . . ? N4 C6 C7 C8 139.5(2) . . . . ? C5 C6 C7 C8 -107.4(3) . . . . ? N2 C7 C8 C9 -0.7(4) . . . . ? C6 C7 C8 C9 176.2(2) . . . . ? C7 C8 C9 C10 0.5(4) . . . . ? C8 C9 C10 C11 0.3(4) . . . . ? C9 C10 C11 N2 -0.8(4) . . . . ? N3 C12 C13 C14 -0.7(4) . . . . ? C12 C13 C14 C15 0.1(4) . . . . ? C13 C14 C15 C16 0.4(4) . . . . ? C14 C15 C16 N3 -0.3(3) . . . . ? C14 C15 C16 C17 177.8(2) . . . . ? N3 C16 C17 N4 -18.9(3) . . . . ? C15 C16 C17 N4 162.9(2) . . . . ? N4 C18 C19 N5 24.7(3) . . . . ? N4 C18 C19 C20 -159.5(2) . . . . ? N5 C19 C20 C21 2.8(4) . . . . ? C18 C19 C20 C21 -172.8(2) . . . . ? C19 C20 C21 C22 -1.8(4) . . . . ? C20 C21 C22 C23 -0.2(4) . . . . ? C21 C22 C23 N5 1.4(4) . . . . ? C2 C1 N1 C5 -1.1(3) . . . . ? C2 C1 N1 Fe1 178.75(18) . . . . ? C4 C5 N1 C1 1.0(3) . . . . ? C6 C5 N1 C1 178.2(2) . . . . ? C4 C5 N1 Fe1 -178.89(18) . . . . ? C6 C5 N1 Fe1 -1.7(2) . . . . ? N6 Fe1 N1 C1 -27.9(2) . . . . ? N3 Fe1 N1 C1 158.6(3) . . . . ? N2 Fe1 N1 C1 -123.4(2) . . . . ? N5 Fe1 N1 C1 71.7(2) . . . . ? N4 Fe1 N1 C1 154.6(2) . . . . ? N6 Fe1 N1 C5 151.93(16) . . . . ? N3 Fe1 N1 C5 -21.6(4) . . . . ? N2 Fe1 N1 C5 56.50(16) . . . . ? N5 Fe1 N1 C5 -108.37(16) . . . . ? N4 Fe1 N1 C5 -25.48(15) . . . . ? C10 C11 N2 C7 0.6(4) . . . . ? C10 C11 N2 Fe1 178.71(19) . . . . ? C8 C7 N2 C11 0.2(4) . . . . ? C6 C7 N2 C11 -177.1(2) . . . . ? C8 C7 N2 Fe1 -178.25(19) . . . . ? C6 C7 N2 Fe1 4.5(2) . . . . ? N6 Fe1 N2 C11 27.1(2) . . . . ? N1 Fe1 N2 C11 123.5(2) . . . . ? N3 Fe1 N2 C11 -72.0(2) . . . . ? N5 Fe1 N2 C11 -159.1(3) . . . . ? N4 Fe1 N2 C11 -155.0(2) . . . . ? N6 Fe1 N2 C7 -154.68(17) . . . . ? N1 Fe1 N2 C7 -58.30(17) . . . . ? N3 Fe1 N2 C7 106.25(17) . . . . ? N5 Fe1 N2 C7 19.2(4) . . . . ? N4 Fe1 N2 C7 23.20(17) . . . . ? C15 C16 N3 C12 -0.4(3) . . . . ? C17 C16 N3 C12 -178.5(2) . . . . ? C15 C16 N3 Fe1 -177.19(17) . . . . ? C17 C16 N3 Fe1 4.7(2) . . . . ? C13 C12 N3 C16 0.9(3) . . . . ? C13 C12 N3 Fe1 177.36(17) . . . . ? N6 Fe1 N3 C16 -170.26(16) . . . . ? N1 Fe1 N3 C16 3.2(4) . . . . ? N2 Fe1 N3 C16 -74.23(16) . . . . ? N5 Fe1 N3 C16 90.28(16) . . . . ? N4 Fe1 N3 C16 7.09(15) . . . . ? N6 Fe1 N3 C12 13.1(2) . . . . ? N1 Fe1 N3 C12 -173.4(2) . . . . ? N2 Fe1 N3 C12 109.15(19) . . . . ? N5 Fe1 N3 C12 -86.34(19) . . . . ? N4 Fe1 N3 C12 -169.5(2) . . . . ? C16 C17 N4 C6 130.3(2) . . . . ? C16 C17 N4 C18 -98.2(2) . . . . ? C16 C17 N4 Fe1 22.9(2) . . . . ? C5 C6 N4 C17 -170.67(19) . . . . ? C7 C6 N4 C17 -58.6(2) . . . . ? C5 C6 N4 C18 58.7(2) . . . . ? C7 C6 N4 C18 170.79(19) . . . . ? C5 C6 N4 Fe1 -56.05(17) . . . . ? C7 C6 N4 Fe1 56.07(17) . . . . ? C19 C18 N4 C17 95.2(2) . . . . ? C19 C18 N4 C6 -133.7(2) . . . . ? C19 C18 N4 Fe1 -25.9(2) . . . . ? N1 Fe1 N4 C17 162.13(16) . . . . ? N3 Fe1 N4 C17 -16.80(15) . . . . ? N2 Fe1 N4 C17 74.87(15) . . . . ? N5 Fe1 N4 C17 -106.21(16) . . . . ? N1 Fe1 N4 C6 44.21(13) . . . . ? N3 Fe1 N4 C6 -134.72(13) . . . . ? N2 Fe1 N4 C6 -43.05(13) . . . . ? N5 Fe1 N4 C6 135.87(14) . . . . ? N1 Fe1 N4 C18 -74.65(15) . . . . ? N3 Fe1 N4 C18 106.43(16) . . . . ? N2 Fe1 N4 C18 -161.91(16) . . . . ? N5 Fe1 N4 C18 17.01(15) . . . . ? C22 C23 N5 C19 -0.4(4) . . . . ? C22 C23 N5 Fe1 -175.4(2) . . . . ? C20 C19 N5 C23 -1.7(4) . . . . ? C18 C19 N5 C23 174.1(2) . . . . ? C20 C19 N5 Fe1 173.78(18) . . . . ? C18 C19 N5 Fe1 -10.4(3) . . . . ? N6 Fe1 N5 C23 -11.1(2) . . . . ? N1 Fe1 N5 C23 -108.1(2) . . . . ? N3 Fe1 N5 C23 87.7(2) . . . . ? N2 Fe1 N5 C23 175.0(3) . . . . ? N4 Fe1 N5 C23 171.0(2) . . . . ? N6 Fe1 N5 C19 173.68(17) . . . . ? N1 Fe1 N5 C19 76.75(17) . . . . ? N3 Fe1 N5 C19 -87.47(17) . . . . ? N2 Fe1 N5 C19 -0.1(4) . . . . ? N4 Fe1 N5 C19 -4.13(17) . . . . ? N1 Fe1 N6 O1 -59.4(4) . . . . ? N3 Fe1 N6 O1 118.8(4) . . . . ? N2 Fe1 N6 O1 27.3(4) . . . . ? N5 Fe1 N6 O1 -151.1(4) . . . . ? 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 O1S H1S F8 0.84 2.51 3.181(15) 138.1 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.24 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.472 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.093 _iucr_refine_instructions_details ; TITL x1005a CELL 0.71073 17.0215 12.70711 12.66693 90.000 90.000 90.000 ZERR 4 0.0003 0.00018 0.00019 0.000 0.000 0.000 LATT -1 SYMM -X,-Y,1/2+Z SYMM 1/2-X,1/2+Y,1/2+Z SYMM 1/2+X,1/2-Y,Z SFAC C H B N O F FE cL UNIT 96 100 7.27 24 8 29.09 4 0.73 TEMP -163 ACTA HTAB BOND BOND $H CONF WPDB L.S. 6 FMAP 2 PLAN 10 OMIT -2 52.5 OMIT 1 1 0 OMIT 0 2 0 HTAB O1S F8 WGHT 0.057200 FVAR 1.97317 0.92313 0.07691 0.25853 0.39412 0.24024 0.10714 FVAR 0.78137 FE1 7 0.259217 0.846919 0.318316 11.00000 0.01467 0.01674 = 0.01339 0.00015 -0.00077 0.00025 C1 1 0.250890 0.955286 0.109213 11.00000 0.03013 0.01820 = 0.02065 -0.00367 0.00273 -0.00189 AFIX 43 H1 2 0.304986 0.972078 0.116736 11.00000 -1.20000 AFIX 0 C2 1 0.211285 0.986907 0.019053 11.00000 0.04490 0.02377 = 0.01796 0.00295 0.00130 0.00453 AFIX 43 H2 2 0.238101 1.024306 -0.034972 11.00000 -1.20000 AFIX 0 C3 1 0.132675 0.963579 0.008551 11.00000 0.04703 0.03019 = 0.01362 0.00141 -0.00924 0.00949 AFIX 43 H3 2 0.104792 0.984875 -0.052805 11.00000 -1.20000 AFIX 0 C4 1 0.094333 0.908614 0.088382 11.00000 0.03046 0.02573 = 0.02151 -0.00627 -0.00720 0.00695 AFIX 43 H4 2 0.040121 0.891788 0.082646 11.00000 -1.20000 AFIX 0 C5 1 0.136826 0.879365 0.175545 11.00000 0.02162 0.01943 = 0.01598 -0.00662 -0.00354 0.00283 C6 1 0.106963 0.815698 0.267875 11.00000 0.01610 0.02044 = 0.01585 -0.00357 -0.00381 -0.00075 AFIX 13 H6 2 0.048292 0.814162 0.271647 11.00000 -1.20000 AFIX 0 C7 1 0.142120 0.707487 0.253772 11.00000 0.02156 0.02073 = 0.01465 0.00075 0.00144 -0.00090 C8 1 0.101395 0.619283 0.222993 11.00000 0.02265 0.02513 = 0.02148 -0.00271 -0.00151 -0.00267 AFIX 43 H8 2 0.046145 0.621560 0.212631 11.00000 -1.20000 AFIX 0 C9 1 0.143281 0.526596 0.207429 11.00000 0.03512 0.02268 = 0.02562 -0.00298 0.00359 -0.00606 AFIX 43 H9 2 0.116827 0.464455 0.185630 11.00000 -1.20000 AFIX 0 C10 1 0.223468 0.525276 0.223793 11.00000 0.03356 0.01649 = 0.02876 -0.00032 0.00110 0.00130 AFIX 43 H10 2 0.252688 0.462475 0.213121 11.00000 -1.20000 AFIX 0 C11 1 0.260972 0.617208 0.256152 11.00000 0.02371 0.02280 = 0.02072 0.00207 0.00110 0.00418 AFIX 43 H11 2 0.316036 0.616349 0.268359 11.00000 -1.20000 AFIX 0 C12 1 0.342911 0.774663 0.510860 11.00000 0.02171 0.01954 = 0.02483 -0.00023 -0.00285 0.00208 AFIX 43 H12 2 0.389981 0.785789 0.472136 11.00000 -1.20000 AFIX 0 C13 1 0.347501 0.740592 0.614105 11.00000 0.03291 0.02171 = 0.02742 -0.00139 -0.01410 0.00481 AFIX 43 H13 2 0.397077 0.727567 0.645979 11.00000 -1.20000 AFIX 0 C14 1 0.279283 0.725801 0.670074 11.00000 0.04414 0.02066 = 0.01613 0.00244 -0.00730 -0.00032 AFIX 43 H14 2 0.281586 0.702479 0.741263 11.00000 -1.20000 AFIX 0 C15 1 0.207389 0.744673 0.623349 11.00000 0.03435 0.01914 = 0.01980 -0.00038 0.00138 -0.00122 AFIX 43 H15 2 0.159896 0.735066 0.661544 11.00000 -1.20000 AFIX 0 C16 1 0.206388 0.778062 0.519055 11.00000 0.02221 0.01397 = 0.02093 -0.00201 0.00109 -0.00004 C17 1 0.130086 0.796743 0.460896 11.00000 0.02175 0.02136 = 0.01666 0.00071 0.00043 -0.00225 AFIX 23 H17A 2 0.106711 0.728305 0.440688 11.00000 -1.20000 H17B 2 0.092612 0.833359 0.508048 11.00000 -1.20000 AFIX 0 C18 1 0.125161 0.975200 0.381626 11.00000 0.01791 0.01895 = 0.02010 -0.00264 -0.00098 0.00297 AFIX 23 H18A 2 0.086459 0.982475 0.439509 11.00000 -1.20000 H18B 2 0.101767 1.005244 0.316728 11.00000 -1.20000 AFIX 0 C19 1 0.198727 1.034354 0.409228 11.00000 0.02235 0.01974 = 0.01370 0.00016 -0.00243 0.00143 C20 1 0.195615 1.131155 0.460577 11.00000 0.02718 0.02446 = 0.01736 -0.00144 -0.00021 0.00099 AFIX 43 H20 2 0.147192 1.158058 0.486311 11.00000 -1.20000 AFIX 0 C21 1 0.265033 1.187614 0.473359 11.00000 0.03443 0.02096 = 0.02356 -0.00526 -0.00621 -0.00431 AFIX 43 H21 2 0.264297 1.254743 0.506357 11.00000 -1.20000 AFIX 0 C22 1 0.335147 1.145399 0.437719 11.00000 0.02672 0.02734 = 0.03209 -0.00189 -0.00440 -0.00729 AFIX 43 H22 2 0.383027 1.183002 0.445603 11.00000 -1.20000 AFIX 0 C23 1 0.334028 1.046540 0.390009 11.00000 0.02015 0.02429 = 0.02678 -0.00162 -0.00070 -0.00452 AFIX 43 H23 2 0.382126 1.016505 0.366781 11.00000 -1.20000 AFIX 0 N1 4 0.214784 0.901885 0.185525 11.00000 0.02104 0.01565 = 0.01415 -0.00145 -0.00160 0.00159 N2 4 0.220768 0.707067 0.270430 11.00000 0.02072 0.01688 = 0.01298 0.00149 -0.00041 0.00034 N3 4 0.273110 0.792553 0.463598 11.00000 0.02057 0.01783 = 0.01723 -0.00055 -0.00462 0.00167 N4 4 0.143342 0.861369 0.364476 11.00000 0.01687 0.01637 = 0.01525 0.00072 -0.00084 0.00075 N5 4 0.267242 0.992593 0.375905 11.00000 0.02022 0.01899 = 0.01471 0.00145 -0.00261 -0.00137 N6 4 0.354470 0.830931 0.272943 11.00000 0.01900 0.02379 = 0.02270 0.00260 0.00486 0.00210 O1 5 0.393636 0.789306 0.211057 11.00000 0.03571 0.05810 = 0.08469 -0.02393 0.03124 -0.00492 SIMU 0.01 B1 > CL1 SUMP 1 0 1 2 1 3 EADP B1 CL1 EXYZ B1 CL1 PART 1 B1 3 0.061131 0.957630 0.722873 21.00000 0.01143 0.02264 = 0.01251 -0.00602 -0.00071 0.00137 F1 6 0.094338 0.992355 0.627466 21.00000 0.04636 0.06433 = 0.01851 -0.00323 0.01118 -0.00316 F2 6 -0.009926 0.908284 0.701810 21.00000 0.02945 0.03454 = 0.05258 -0.00888 -0.00813 -0.00763 F3 6 0.047042 1.046866 0.786216 21.00000 0.02268 0.02498 = 0.02186 -0.00476 -0.00062 0.00369 F4 6 0.112631 0.891575 0.773605 21.00000 0.03671 0.03797 = 0.03507 -0.01022 -0.00604 0.01624 PART 2 CL1 8 0.061131 0.957630 0.722873 31.00000 0.01143 0.02264 = 0.01251 -0.00602 -0.00071 0.00137 EADP B2 B2' B2C CL2 EXYZ B2C CL2 EADP F5 F5' F5C DELU 0.005 B2 > CL2 SIMU 0.01 B2 > CL2 SUMP 1 0 1 4 1 5 1 6 1 7 PART 1 B2 3 0.036808 0.555260 0.567492 41.00000 0.01942 0.02575 = 0.05178 0.00800 0.00143 -0.00618 F5 6 0.101884 0.560134 0.495141 41.00000 0.02507 0.01853 = 0.04075 0.00742 -0.00077 0.00296 F6 6 0.009659 0.658863 0.578049 41.00000 0.02998 0.04160 = 0.06745 0.00927 0.01121 0.02079 F7 6 0.059897 0.515488 0.658519 41.00000 0.02231 0.06115 = 0.03553 0.01198 0.00603 0.01153 F8 6 -0.024802 0.505783 0.517922 41.00000 0.03744 0.07369 = 0.05571 -0.00371 -0.00255 -0.02805 PART 2 SAME B2 > F8 B2' 3 0.030526 0.559427 0.515950 51.00000 0.01942 0.02575 = 0.05178 0.00800 0.00143 -0.00618 F5' 6 0.111363 0.540054 0.489233 51.00000 0.02507 0.01853 = 0.04075 0.00742 -0.00077 0.00296 F6' 6 0.033311 0.628801 0.604382 51.00000 0.04924 0.05293 = 0.04781 -0.01017 0.01220 -0.00196 F7' 6 -0.003888 0.464212 0.545182 51.00000 0.05167 0.02360 = 0.05117 0.01647 0.01737 -0.00599 F8' 6 -0.005659 0.601959 0.432021 51.00000 0.02401 0.03919 = 0.04614 0.01368 -0.00086 -0.00060 PART 3 SAME B2 > F8 B2C 3 0.041722 0.555292 0.542599 61.00000 0.01942 0.02575 = 0.05178 0.00800 0.00143 -0.00618 F5C 6 0.115504 0.565311 0.489286 61.00000 0.02507 0.01853 = 0.04075 0.00742 -0.00077 0.00296 F6C 6 0.024458 0.646403 0.601031 61.00000 0.02906 0.03379 = 0.05015 0.00661 -0.00301 0.02339 F7C 6 0.046947 0.462593 0.599855 61.00000 0.03405 0.03371 = 0.05544 0.01975 0.01907 0.00525 F8C 6 -0.015687 0.553386 0.466497 61.00000 0.03713 0.04435 = 0.07307 0.00525 -0.01961 0.00680 PART 4 CL2 8 0.041722 0.555292 0.542599 71.00000 0.01942 0.02575 = 0.05178 0.00800 0.00143 -0.00618 EADP C1S C1' SIMU 0.01 O1S > C1' PART 1 O1S 5 0.030287 0.270930 0.472175 81.00000 0.04635 0.04184 = 0.03552 0.00587 0.01033 0.00667 AFIX 147 H1S 2 0.031089 0.323391 0.512507 11.00000 -1.50000 AFIX 0 C1S 1 0.041814 0.303817 0.368466 81.00000 0.04387 0.06627 = 0.04468 0.00475 0.02256 0.01756 AFIX 137 H1S1 2 0.006640 0.362873 0.352917 81.00000 -1.50000 H1S2 2 0.030444 0.245474 0.320230 81.00000 -1.50000 H1S3 2 0.096472 0.326250 0.359260 81.00000 -1.50000 AFIX 0 PART 2 SAME O1S > C1S O1' 5 0.018062 0.218946 0.412950 -81.00000 0.06638 0.06363 = 0.06657 0.00730 0.01117 0.00320 C1' 1 0.059759 0.295404 0.359359 -81.00000 0.04387 0.06627 = 0.04468 0.00475 0.02256 0.01756 AFIX 137 H1'1 2 0.084541 0.343121 0.410204 -81.00000 -1.50000 H1'2 2 0.023953 0.335341 0.313912 -81.00000 -1.50000 H1'3 2 0.100362 0.261987 0.315944 -81.00000 -1.50000 HKLF 4 REM x1005a REM R1 = 0.0319 for 4802 Fo > 4sig(Fo) and 0.0369 for all 5214 data REM 476 parameters refined using 544 restraints END WGHT 0.0572 0.0000 REM Highest difference peak 0.472, deepest hole -0.476, 1-sigma level 0.093 Q1 1 0.0194 0.4154 0.4946 11.00000 0.05 0.47 Q2 1 0.0285 0.5371 0.5925 11.00000 0.05 0.39 Q3 1 -0.0006 0.6187 0.5090 11.00000 0.05 0.39 Q4 1 0.0387 0.9218 0.7323 11.00000 0.05 0.38 Q5 1 0.0234 0.9346 0.7226 11.00000 0.05 0.37 Q6 1 0.0410 0.5076 0.5146 11.00000 0.05 0.36 Q7 1 -0.0095 0.8774 0.7698 11.00000 0.05 0.36 Q8 1 0.0231 0.4585 0.5739 11.00000 0.05 0.36 Q9 1 0.0529 0.9858 0.7533 11.00000 0.05 0.32 Q10 1 0.0553 0.9708 0.7013 11.00000 0.05 0.31 ;