data_1acacOMe _audit_creation_date 2011-08-18 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _publ_requested_journal '?' _chemical_name_common ? _chemical_name_systematic '?' _chemical_formula_moiety 'C22 H32 B Fe N7 O4, C2 H3 N' _chemical_formula_sum 'C24 H35 B Fe N8 O4' _chemical_formula_weight 566.26 _chemical_absolute_configuration unk _chemical_melting_point ? 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' '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' _space_group_crystal_system 'orthorhombic' _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z+1/2' 3 'x+1/2, -y+1/2, -z' 4 '-x, y+1/2, -z+1/2' _cell_length_a 12.62432(13) _cell_length_b 16.70885(18) _cell_length_c 13.70225(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2890.32(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 59038 _cell_measurement_temperature 100 _cell_measurement_theta_max 29.4215 _cell_measurement_theta_min 3.3766 _exptl_absorpt_coefficient_mu 0.565 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.89316 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1192 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_special_details '?' _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_unetI/netI 0.0172 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 89285 _diffrn_reflns_theta_full 29.00 _diffrn_reflns_theta_max 29.49 _diffrn_reflns_theta_min 3.38 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 7.00 51.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 11.5134 37.0000 30.0000 44 #__ type_ start__ end____ width___ exp.time_ 2 omega -15.00 74.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 11.5134 77.0000 -120.0000 89 #__ type_ start__ end____ width___ exp.time_ 3 omega -20.00 53.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 11.5134 -99.0000 96.0000 73 #__ type_ start__ end____ width___ exp.time_ 4 omega 3.00 70.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 11.5134 -127.0000 -98.0000 67 #__ type_ start__ end____ width___ exp.time_ 5 omega -20.00 53.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 11.5134 -99.0000 -22.0000 73 #__ type_ start__ end____ width___ exp.time_ 6 omega -15.00 88.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 11.5134 37.0000 -60.0000 103 #__ type_ start__ end____ width___ exp.time_ 7 omega -22.00 90.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 11.5134 77.0000 90.0000 112 #__ type_ start__ end____ width___ exp.time_ 8 omega -28.00 64.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -11.6697 37.0000 -150.0000 92 #__ type_ start__ end____ width___ exp.time_ 9 omega 3.00 69.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 11.5134 -127.0000 -157.0000 66 #__ type_ start__ end____ width___ exp.time_ 10 omega 3.00 70.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 11.5134 -127.0000 22.0000 67 #__ type_ start__ end____ width___ exp.time_ 11 omega -20.00 53.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 11.5134 -99.0000 157.0000 73 #__ type_ start__ end____ width___ exp.time_ 12 omega -15.00 88.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 11.5134 37.0000 150.0000 103 #__ type_ start__ end____ width___ exp.time_ 13 omega -28.00 64.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -11.6697 37.0000 120.0000 92 #__ type_ start__ end____ width___ exp.time_ 14 omega -28.00 64.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -11.6697 37.0000 0.0000 92 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0457648 _diffrn_orient_matrix_UB_12 0.0132691 _diffrn_orient_matrix_UB_13 -0.0253068 _diffrn_orient_matrix_UB_21 -0.0269016 _diffrn_orient_matrix_UB_22 -0.0048092 _diffrn_orient_matrix_UB_23 -0.0450531 _diffrn_orient_matrix_UB_31 -0.018437 _diffrn_orient_matrix_UB_32 0.0400344 _diffrn_orient_matrix_UB_33 0.0029181 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'fine-focus sealed tube' _reflns_number_gt 7274 _reflns_number_total 7745 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.248 _refine_diff_density_min -0.177 _refine_diff_density_rms 0.040 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 7745 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0226 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.1650P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.0615 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 -0.111039(12) 0.438363(9) 0.514757(12) 0.01399(4) Uani 1 1 d . . . O1 O -0.04887(6) 0.32234(5) 0.51209(7) 0.01983(17) Uani 1 1 d . . . O2 O -0.20949(7) 0.39878(5) 0.62676(6) 0.01926(17) Uani 1 1 d . . . O3 O -0.04079(8) 0.18977(5) 0.53824(7) 0.0267(2) Uani 1 1 d . . . O4 O -0.29611(7) 0.31201(6) 0.72324(7) 0.02597(19) Uani 1 1 d . . . N1 N -0.00632(8) 0.47265(6) 0.39784(7) 0.01625(19) Uani 1 1 d . . . N2 N 0.04437(7) 0.54503(5) 0.40688(7) 0.01557(19) Uani 1 1 d . . . N3 N -0.16810(7) 0.56037(6) 0.51330(7) 0.01599(17) Uani 1 1 d . . . N4 N -0.09253(7) 0.61928(5) 0.50693(7) 0.01479(18) Uani 1 1 d . . . N5 N 0.00716(8) 0.48342(6) 0.61845(7) 0.01609(19) Uani 1 1 d . . . N6 N 0.05970(7) 0.55221(6) 0.59127(7) 0.01471(18) Uani 1 1 d . . . N7 N -0.23480(9) 0.40383(7) 0.40411(8) 0.0221(2) Uani 1 1 d . . . N8 N 0.34857(11) 0.52548(8) 0.49064(10) 0.0391(3) Uani 1 1 d . . . C1 C 0.03889(12) 0.18683(9) 0.46412(12) 0.0351(3) Uani 1 1 d . . . H20A H 0.0088 0.2051 0.4020 0.053 Uiso 1 1 calc R . . H20B H 0.0644 0.1317 0.4571 0.053 Uiso 1 1 calc R . . H20C H 0.0981 0.2217 0.4825 0.053 Uiso 1 1 calc R . . C2 C -0.08523(9) 0.26277(7) 0.55558(9) 0.0188(2) Uani 1 1 d . . . C3 C -0.16845(10) 0.25949(7) 0.62282(9) 0.0209(2) Uani 1 1 d . . . H17 H -0.1891 0.2089 0.6483 0.025 Uiso 1 1 calc R . . C4 C -0.22236(9) 0.32791(7) 0.65392(9) 0.0185(2) Uani 1 1 d . . . C5 C -0.34838(12) 0.37995(9) 0.76569(10) 0.0308(3) Uani 1 1 d . . . H19A H -0.3818 0.4117 0.7140 0.046 Uiso 1 1 calc R . . H19B H -0.2964 0.4129 0.8004 0.046 Uiso 1 1 calc R . . H19C H -0.4026 0.3615 0.8116 0.046 Uiso 1 1 calc R . . C6 C 0.02288(9) 0.44231(8) 0.31143(8) 0.0186(2) Uani 1 1 d . . . C7 C 0.09197(9) 0.49486(7) 0.26410(9) 0.0208(2) Uani 1 1 d . . . H2 H 0.1241 0.4878 0.2020 0.025 Uiso 1 1 calc R . . C8 C 0.10380(9) 0.55954(7) 0.32666(8) 0.0184(2) Uani 1 1 d . . . C9 C -0.01554(12) 0.36212(8) 0.27709(10) 0.0270(3) Uani 1 1 d . . . H11A H 0.0449 0.3299 0.2555 0.041 Uiso 1 1 calc R . . H11B H -0.0649 0.3694 0.2226 0.041 Uiso 1 1 calc R . . H11C H -0.0518 0.3347 0.3308 0.041 Uiso 1 1 calc R . . C10 C 0.16873(11) 0.63333(8) 0.31340(10) 0.0269(3) Uani 1 1 d . . . H10A H 0.2051 0.6311 0.2503 0.040 Uiso 1 1 calc R . . H10B H 0.2213 0.6369 0.3659 0.040 Uiso 1 1 calc R . . H10C H 0.1225 0.6804 0.3154 0.040 Uiso 1 1 calc R . . C11 C -0.26164(9) 0.59756(7) 0.52089(9) 0.0183(2) Uani 1 1 d . . . C12 C -0.24657(9) 0.68065(7) 0.51996(10) 0.0208(2) Uani 1 1 d . . . H5 H -0.2997 0.7208 0.5244 0.025 Uiso 1 1 calc R . . C13 C -0.13823(9) 0.69231(7) 0.51116(9) 0.0180(2) Uani 1 1 d . . . C14 C -0.36313(9) 0.55150(8) 0.52843(11) 0.0253(3) Uani 1 1 d . . . H13A H -0.3803 0.5281 0.4648 0.038 Uiso 1 1 calc R . . H13B H -0.3551 0.5087 0.5768 0.038 Uiso 1 1 calc R . . H13C H -0.4203 0.5876 0.5486 0.038 Uiso 1 1 calc R . . C15 C -0.07621(10) 0.76813(7) 0.50562(10) 0.0246(3) Uani 1 1 d . . . H12A H -0.0441 0.7730 0.4408 0.037 Uiso 1 1 calc R . . H12B H -0.0204 0.7675 0.5553 0.037 Uiso 1 1 calc R . . H12C H -0.1234 0.8137 0.5172 0.037 Uiso 1 1 calc R . . C16 C 0.04765(9) 0.46214(7) 0.70527(9) 0.0192(2) Uani 1 1 d . . . C17 C 0.12566(10) 0.51687(7) 0.73397(9) 0.0203(2) Uani 1 1 d . . . H8 H 0.1664 0.5156 0.7922 0.024 Uiso 1 1 calc R . . C18 C 0.13125(9) 0.57312(7) 0.66035(8) 0.0175(2) Uani 1 1 d . . . C19 C 0.01070(12) 0.38943(8) 0.75914(10) 0.0290(3) Uani 1 1 d . . . H15A H 0.0164 0.3425 0.7166 0.044 Uiso 1 1 calc R . . H15B H -0.0633 0.3967 0.7789 0.044 Uiso 1 1 calc R . . H15C H 0.0548 0.3815 0.8172 0.044 Uiso 1 1 calc R . . C20 C 0.20170(10) 0.64479(8) 0.65162(10) 0.0228(3) Uani 1 1 d . . . H14A H 0.2370 0.6442 0.5879 0.034 Uiso 1 1 calc R . . H14B H 0.2551 0.6435 0.7035 0.034 Uiso 1 1 calc R . . H14C H 0.1591 0.6936 0.6577 0.034 Uiso 1 1 calc R . . C21 C -0.29446(10) 0.39248(8) 0.34328(10) 0.0248(3) Uani 1 1 d . . . C22 C -0.37124(13) 0.37812(12) 0.26602(12) 0.0427(4) Uani 1 1 d . . . H22A H -0.3511 0.3300 0.2296 0.064 Uiso 1 1 calc R . . H22B H -0.3727 0.4242 0.2217 0.064 Uiso 1 1 calc R . . H22C H -0.4416 0.3705 0.2947 0.064 Uiso 1 1 calc R . . C23 C 0.29389(10) 0.47221(8) 0.50040(9) 0.0265(3) Uani 1 1 d . . . C24 C 0.22414(10) 0.40387(8) 0.51379(13) 0.0327(3) Uani 1 1 d . . . H24A H 0.1714 0.4028 0.4613 0.049 Uiso 1 1 calc R . . H24B H 0.2659 0.3544 0.5122 0.049 Uiso 1 1 calc R . . H24C H 0.1881 0.4083 0.5769 0.049 Uiso 1 1 calc R . . B1 B 0.02668(10) 0.59732(7) 0.49834(9) 0.0151(2) Uani 1 1 d . . . H1 H 0.0694 0.6475 0.4925 0.018 Uiso 1 1 calc R . . 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 0.01439(7) 0.01352(7) 0.01407(7) 0.00029(6) 0.00025(6) 0.00066(6) O1 0.0194(4) 0.0173(4) 0.0228(4) 0.0003(3) 0.0044(4) 0.0013(3) O2 0.0193(4) 0.0203(4) 0.0183(4) 0.0014(3) 0.0028(3) 0.0025(3) O3 0.0317(5) 0.0165(4) 0.0319(5) 0.0009(3) 0.0090(4) 0.0047(4) O4 0.0259(4) 0.0296(5) 0.0223(4) 0.0037(4) 0.0101(4) 0.0016(4) N1 0.0172(4) 0.0158(4) 0.0157(5) -0.0014(4) -0.0007(4) 0.0002(4) N2 0.0150(4) 0.0158(5) 0.0159(4) 0.0008(3) 0.0009(4) 0.0005(3) N3 0.0153(4) 0.0170(4) 0.0157(4) 0.0009(4) -0.0003(3) -0.0003(4) N4 0.0175(4) 0.0137(4) 0.0132(4) 0.0007(3) 0.0003(4) 0.0012(3) N5 0.0176(5) 0.0144(5) 0.0162(5) 0.0020(4) -0.0007(4) 0.0002(4) N6 0.0146(4) 0.0135(4) 0.0160(4) 0.0002(3) 0.0001(3) -0.0008(4) N7 0.0206(5) 0.0250(5) 0.0208(5) -0.0009(4) 0.0000(4) -0.0021(4) N8 0.0486(7) 0.0367(7) 0.0320(7) -0.0051(6) 0.0065(6) -0.0032(6) C1 0.0371(7) 0.0265(7) 0.0416(9) 0.0012(6) 0.0152(7) 0.0124(6) C2 0.0193(5) 0.0172(5) 0.0197(5) -0.0025(4) -0.0015(4) 0.0022(4) C3 0.0244(6) 0.0173(5) 0.0211(6) 0.0005(4) 0.0035(5) -0.0037(5) C4 0.0155(5) 0.0256(6) 0.0145(5) 0.0009(4) 0.0000(4) -0.0027(5) C5 0.0303(7) 0.0406(8) 0.0215(6) 0.0009(6) 0.0096(5) 0.0110(6) C6 0.0184(5) 0.0219(5) 0.0156(5) -0.0019(5) 0.0006(4) 0.0023(5) C7 0.0198(6) 0.0258(6) 0.0168(5) -0.0008(5) 0.0043(4) 0.0029(5) C8 0.0165(5) 0.0219(5) 0.0169(5) 0.0025(4) 0.0025(4) 0.0022(5) C9 0.0332(7) 0.0268(6) 0.0210(6) -0.0078(5) 0.0034(5) -0.0026(5) C10 0.0286(7) 0.0262(6) 0.0259(7) 0.0014(5) 0.0102(5) -0.0034(5) C11 0.0175(5) 0.0206(5) 0.0168(5) 0.0006(5) -0.0008(5) 0.0045(4) C12 0.0198(5) 0.0191(5) 0.0234(6) 0.0001(5) -0.0002(5) 0.0056(4) C13 0.0228(5) 0.0163(5) 0.0148(5) 0.0001(4) -0.0013(4) 0.0032(4) C14 0.0173(5) 0.0253(6) 0.0333(7) -0.0012(5) 0.0018(5) 0.0021(4) C15 0.0279(6) 0.0157(5) 0.0302(7) -0.0005(5) -0.0023(5) 0.0022(4) C16 0.0189(5) 0.0229(6) 0.0159(5) 0.0024(4) -0.0015(4) 0.0010(4) C17 0.0203(6) 0.0252(6) 0.0154(5) 0.0003(4) -0.0038(4) 0.0002(5) C18 0.0157(5) 0.0204(5) 0.0164(5) -0.0040(4) -0.0003(4) 0.0023(4) C19 0.0326(7) 0.0302(7) 0.0243(7) 0.0107(5) -0.0093(6) -0.0074(6) C20 0.0226(6) 0.0229(6) 0.0229(6) -0.0038(5) -0.0034(5) -0.0037(5) C21 0.0217(6) 0.0305(7) 0.0221(6) -0.0027(5) 0.0005(5) 0.0045(5) C22 0.0321(8) 0.0643(11) 0.0317(8) -0.0051(8) -0.0131(7) 0.0084(8) C23 0.0307(6) 0.0311(6) 0.0178(6) -0.0053(5) -0.0003(5) 0.0084(5) C24 0.0243(6) 0.0303(6) 0.0435(8) -0.0069(6) 0.0007(6) 0.0056(5) B1 0.0155(5) 0.0148(5) 0.0149(6) -0.0003(5) 0.0006(4) 0.0003(4) _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 2.0918(8) . ? Fe1 O2 2.0826(8) . ? Fe1 N1 2.1546(10) . ? Fe1 N3 2.1623(9) . ? Fe1 N5 2.1937(10) . ? Fe1 N7 2.2522(11) . ? O1 C2 1.2477(15) . ? O2 C4 1.2518(15) . ? O3 C1 1.4304(16) . ? O3 C2 1.3633(14) . ? O4 C4 1.3563(14) . ? O4 C5 1.4362(17) . ? N1 C6 1.3397(15) . ? N2 N1 1.3739(13) . ? N2 C8 1.3527(14) . ? N2 B1 1.5439(15) . ? N3 C11 1.3385(14) . ? N4 N3 1.3734(12) . ? N4 C13 1.3510(14) . ? N4 B1 1.5535(15) . ? N5 C16 1.3427(15) . ? N6 N5 1.3784(13) . ? N6 C18 1.3543(15) . ? N6 B1 1.5372(15) . ? N7 C21 1.1393(17) . ? N8 C23 1.1342(19) . ? C1 H20A 0.9800 . ? C1 H20B 0.9800 . ? C1 H20C 0.9800 . ? C3 C2 1.3984(17) . ? C3 H17 0.9500 . ? C4 C3 1.3971(17) . ? C5 H19A 0.9800 . ? C5 H19B 0.9800 . ? C5 H19C 0.9800 . ? C6 C9 1.5006(18) . ? C7 C6 1.3973(17) . ? C7 H2 0.9500 . ? C8 C7 1.3875(17) . ? C8 C10 1.4917(17) . ? C9 H11A 0.9800 . ? C9 H11B 0.9800 . ? C9 H11C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.4982(16) . ? C12 C11 1.4014(16) . ? C12 H5 0.9500 . ? C13 C12 1.3867(16) . ? C13 C15 1.4912(16) . ? C14 H13A 0.9800 . ? C14 H13B 0.9800 . ? C14 H13C 0.9800 . ? C15 H12A 0.9800 . ? C15 H12B 0.9800 . ? C15 H12C 0.9800 . ? C16 C19 1.4962(17) . ? C17 C16 1.4003(17) . ? C17 H8 0.9500 . ? C18 C17 1.3805(17) . ? C18 C20 1.4964(17) . ? C19 H15A 0.9800 . ? C19 H15B 0.9800 . ? C19 H15C 0.9800 . ? C20 H14A 0.9800 . ? C20 H14B 0.9800 . ? C20 H14C 0.9800 . ? C21 C22 1.4552(19) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.454(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? B1 H1 1.0000 . ? 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 N1 90.18(3) . . ? O1 Fe1 N3 177.00(3) . . ? O1 Fe1 N5 94.25(3) . . ? O1 Fe1 N7 90.64(4) . . ? O2 Fe1 O1 86.70(3) . . ? O2 Fe1 N1 176.86(4) . . ? O2 Fe1 N3 96.17(3) . . ? O2 Fe1 N5 92.16(4) . . ? O2 Fe1 N7 90.04(4) . . ? N1 Fe1 N3 86.95(4) . . ? N1 Fe1 N5 88.45(4) . . ? N1 Fe1 N7 89.61(4) . . ? N3 Fe1 N5 84.78(4) . . ? N3 Fe1 N7 90.24(4) . . ? N5 Fe1 N7 174.75(4) . . ? C2 O1 Fe1 126.37(8) . . ? C4 O2 Fe1 126.65(8) . . ? C2 O3 C1 116.35(10) . . ? C4 O4 C5 116.37(10) . . ? N2 N1 Fe1 116.93(7) . . ? C6 N1 Fe1 136.50(8) . . ? C6 N1 N2 106.54(10) . . ? N1 N2 B1 120.26(9) . . ? C8 N2 N1 110.05(9) . . ? C8 N2 B1 129.67(10) . . ? N4 N3 Fe1 116.42(6) . . ? C11 N3 Fe1 136.96(8) . . ? C11 N3 N4 106.56(9) . . ? N3 N4 B1 120.56(8) . . ? C13 N4 N3 110.36(8) . . ? C13 N4 B1 129.07(9) . . ? N6 N5 Fe1 116.01(7) . . ? C16 N5 Fe1 137.90(8) . . ? C16 N5 N6 106.08(9) . . ? N5 N6 B1 120.14(9) . . ? C18 N6 N5 110.31(9) . . ? C18 N6 B1 129.30(9) . . ? C21 N7 Fe1 173.58(11) . . ? O3 C1 H20A 109.5 . . ? O3 C1 H20B 109.5 . . ? O3 C1 H20C 109.5 . . ? H20A C1 H20B 109.5 . . ? H20C C1 H20A 109.5 . . ? H20C C1 H20B 109.5 . . ? O1 C2 O3 118.62(10) . . ? O1 C2 C3 128.49(11) . . ? O3 C2 C3 112.89(10) . . ? C2 C3 H17 118.8 . . ? C4 C3 C2 122.34(11) . . ? C4 C3 H17 118.8 . . ? O2 C4 O4 118.86(11) . . ? O2 C4 C3 128.33(11) . . ? O4 C4 C3 112.81(10) . . ? O4 C5 H19A 109.5 . . ? O4 C5 H19B 109.5 . . ? O4 C5 H19C 109.5 . . ? H19A C5 H19B 109.5 . . ? H19C C5 H19A 109.5 . . ? H19C C5 H19B 109.5 . . ? N1 C6 C7 110.13(11) . . ? N1 C6 C9 121.74(11) . . ? C7 C6 C9 128.12(11) . . ? C6 C7 H2 127.2 . . ? C8 C7 C6 105.65(10) . . ? C8 C7 H2 127.2 . . ? N2 C8 C7 107.63(10) . . ? N2 C8 C10 123.50(11) . . ? C7 C8 C10 128.88(11) . . ? C6 C9 H11A 109.5 . . ? C6 C9 H11B 109.5 . . ? C6 C9 H11C 109.5 . . ? H11A C9 H11B 109.5 . . ? H11C C9 H11A 109.5 . . ? H11C C9 H11B 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10C C10 H10A 109.5 . . ? H10C C10 H10B 109.5 . . ? N3 C11 C12 109.84(10) . . ? N3 C11 C14 121.43(10) . . ? C12 C11 C14 128.73(10) . . ? C11 C12 H5 127.1 . . ? C13 C12 C11 105.89(10) . . ? C13 C12 H5 127.1 . . ? N4 C13 C12 107.34(10) . . ? N4 C13 C15 122.75(10) . . ? C12 C13 C15 129.91(10) . . ? C11 C14 H13A 109.5 . . ? C11 C14 H13B 109.5 . . ? C11 C14 H13C 109.5 . . ? H13B C14 H13A 109.5 . . ? H13C C14 H13A 109.5 . . ? H13C C14 H13B 109.5 . . ? C13 C15 H12A 109.5 . . ? C13 C15 H12B 109.5 . . ? C13 C15 H12C 109.5 . . ? H12A C15 H12B 109.5 . . ? H12A C15 H12C 109.5 . . ? H12B C15 H12C 109.5 . . ? N5 C16 C17 110.10(11) . . ? N5 C16 C19 122.24(11) . . ? C17 C16 C19 127.66(11) . . ? C16 C17 H8 127.0 . . ? C18 C17 C16 105.98(10) . . ? C18 C17 H8 127.0 . . ? N6 C18 C17 107.52(10) . . ? N6 C18 C20 123.15(11) . . ? C17 C18 C20 129.32(11) . . ? C16 C19 H15A 109.5 . . ? C16 C19 H15B 109.5 . . ? C16 C19 H15C 109.5 . . ? H15B C19 H15A 109.5 . . ? H15B C19 H15C 109.5 . . ? H15C C19 H15A 109.5 . . ? C18 C20 H14A 109.5 . . ? C18 C20 H14B 109.5 . . ? C18 C20 H14C 109.5 . . ? H14A C20 H14B 109.5 . . ? H14C C20 H14A 109.5 . . ? H14C C20 H14B 109.5 . . ? N7 C21 C22 179.62(16) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22C C22 H22A 109.5 . . ? H22C C22 H22B 109.5 . . ? N8 C23 C24 179.50(16) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24C C24 H24B 109.5 . . ? N2 B1 N4 109.59(9) . . ? N2 B1 H1 109.3 . . ? N4 B1 H1 109.3 . . ? N6 B1 N2 110.84(9) . . ? N6 B1 N4 108.41(9) . . ? N6 B1 H1 109.3 . . ? 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 Fe1 O1 C2 O3 173.64(8) . . . . ? Fe1 O1 C2 C3 -6.57(19) . . . . ? Fe1 O2 C4 O4 -174.84(7) . . . . ? Fe1 O2 C4 C3 6.12(18) . . . . ? Fe1 N1 C6 C7 177.20(8) . . . . ? Fe1 N1 C6 C9 -3.81(18) . . . . ? Fe1 N3 C11 C12 176.61(9) . . . . ? Fe1 N3 C11 C14 -3.64(19) . . . . ? Fe1 N5 C16 C17 178.67(9) . . . . ? Fe1 N5 C16 C19 -1.25(19) . . . . ? Fe1 N7 C21 C22 -111(25) . . . . ? O1 Fe1 O2 C4 -10.15(10) . . . . ? O1 Fe1 N1 N2 -135.99(7) . . . . ? O1 Fe1 N1 C6 46.74(12) . . . . ? O1 Fe1 N3 N4 -26.8(8) . . . . ? O1 Fe1 N3 C11 156.5(7) . . . . ? O1 Fe1 N5 N6 128.27(7) . . . . ? O1 Fe1 N5 C16 -50.23(12) . . . . ? O1 Fe1 N7 C21 -128.8(10) . . . . ? O2 Fe1 O1 C2 10.35(10) . . . . ? O2 Fe1 N1 N2 -143.0(6) . . . . ? O2 Fe1 N1 C6 39.8(7) . . . . ? O2 Fe1 N3 N4 136.06(7) . . . . ? O2 Fe1 N3 C11 -40.65(12) . . . . ? O2 Fe1 N5 N6 -144.88(7) . . . . ? O2 Fe1 N5 C16 36.62(12) . . . . ? O2 Fe1 N7 C21 144.5(10) . . . . ? O2 C4 C3 C2 2.6(2) . . . . ? O4 C4 C3 C2 -176.50(11) . . . . ? N1 Fe1 O1 C2 -169.26(10) . . . . ? N1 Fe1 O2 C4 -3.2(7) . . . . ? N1 Fe1 N3 N4 -44.27(8) . . . . ? N1 Fe1 N3 C11 139.02(12) . . . . ? N1 Fe1 N5 N6 38.20(7) . . . . ? N1 Fe1 N5 C16 -140.30(12) . . . . ? N1 Fe1 N7 C21 -38.6(10) . . . . ? N1 N2 C8 C7 -0.31(12) . . . . ? N1 N2 C8 C10 179.89(11) . . . . ? N1 N2 B1 N4 -60.12(12) . . . . ? N1 N2 B1 N6 59.49(12) . . . . ? N2 N1 C6 C7 -0.26(13) . . . . ? N2 N1 C6 C9 178.73(11) . . . . ? N2 C8 C7 C6 0.14(13) . . . . ? N3 Fe1 O1 C2 173.3(7) . . . . ? N3 Fe1 O2 C4 170.73(10) . . . . ? N3 Fe1 N1 N2 43.12(7) . . . . ? N3 Fe1 N1 C6 -134.15(12) . . . . ? N3 Fe1 N5 N6 -48.88(7) . . . . ? N3 Fe1 N5 C16 132.62(12) . . . . ? N3 Fe1 N7 C21 48.4(10) . . . . ? N3 N4 C13 C12 -0.35(13) . . . . ? N3 N4 C13 C15 -179.75(11) . . . . ? N3 N4 B1 N2 58.50(13) . . . . ? N3 N4 B1 N6 -62.58(12) . . . . ? N4 N3 C11 C12 -0.32(14) . . . . ? N4 N3 C11 C14 179.43(11) . . . . ? N4 C13 C12 C11 0.15(15) . . . . ? N5 Fe1 O1 C2 102.28(10) . . . . ? N5 Fe1 O2 C4 -104.29(10) . . . . ? N5 Fe1 N1 N2 -41.74(7) . . . . ? N5 Fe1 N1 C6 140.99(12) . . . . ? N5 Fe1 N3 N4 44.45(8) . . . . ? N5 Fe1 N3 C11 -132.26(12) . . . . ? N5 Fe1 N7 C21 29.7(12) . . . . ? N5 N6 C18 C17 0.16(12) . . . . ? N5 N6 C18 C20 179.34(10) . . . . ? N5 N6 B1 N2 -63.42(12) . . . . ? N5 N6 B1 N4 56.89(12) . . . . ? N6 N5 C16 C17 0.07(13) . . . . ? N6 N5 C16 C19 -179.85(11) . . . . ? N6 C18 C17 C16 -0.11(13) . . . . ? N7 Fe1 O1 C2 -79.65(10) . . . . ? N7 Fe1 O2 C4 80.48(10) . . . . ? N7 Fe1 N1 N2 133.38(8) . . . . ? N7 Fe1 N1 C6 -43.89(12) . . . . ? N7 Fe1 N3 N4 -133.87(8) . . . . ? N7 Fe1 N3 C11 49.42(12) . . . . ? N7 Fe1 N5 N6 -30.2(5) . . . . ? N7 Fe1 N5 C16 151.3(4) . . . . ? C1 O3 C2 O1 -5.33(17) . . . . ? C1 O3 C2 C3 174.85(12) . . . . ? C4 C3 C2 O1 -2.3(2) . . . . ? C4 C3 C2 O3 177.49(11) . . . . ? C5 O4 C4 O2 -4.72(16) . . . . ? C5 O4 C4 C3 174.47(11) . . . . ? C8 N2 N1 Fe1 -177.68(7) . . . . ? C8 N2 N1 C6 0.36(12) . . . . ? C8 N2 B1 N4 118.19(12) . . . . ? C8 N2 B1 N6 -122.21(12) . . . . ? C8 C7 C6 N1 0.08(14) . . . . ? C8 C7 C6 C9 -178.84(12) . . . . ? C10 C8 C7 C6 179.93(12) . . . . ? C13 N4 N3 Fe1 -177.24(7) . . . . ? C13 N4 N3 C11 0.42(12) . . . . ? C13 N4 B1 N2 -122.82(12) . . . . ? C13 N4 B1 N6 116.10(12) . . . . ? C13 C12 C11 N3 0.11(15) . . . . ? C13 C12 C11 C14 -179.62(13) . . . . ? C15 C13 C12 C11 179.49(12) . . . . ? C18 N6 N5 Fe1 -179.10(7) . . . . ? C18 N6 N5 C16 -0.15(12) . . . . ? C18 N6 B1 N2 122.78(12) . . . . ? C18 N6 B1 N4 -116.91(12) . . . . ? C18 C17 C16 N5 0.02(14) . . . . ? C18 C17 C16 C19 179.94(13) . . . . ? C20 C18 C17 C16 -179.22(12) . . . . ? B1 N2 N1 Fe1 0.93(12) . . . . ? B1 N2 N1 C6 178.97(10) . . . . ? B1 N2 C8 C7 -178.76(10) . . . . ? B1 N2 C8 C10 1.45(18) . . . . ? B1 N4 N3 Fe1 1.67(12) . . . . ? B1 N4 N3 C11 179.33(10) . . . . ? B1 N4 C13 C12 -179.14(11) . . . . ? B1 N4 C13 C15 1.46(19) . . . . ? B1 N6 N5 Fe1 6.01(12) . . . . ? B1 N6 N5 C16 -175.03(9) . . . . ? B1 N6 C18 C17 174.45(10) . . . . ? B1 N6 C18 C20 -6.38(18) . . . . ? #===END data_2acacOMe _audit_creation_date 2011-08-18 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C50 H41 B Fe N6 O4, 1.5(C H2 Cl2)' _chemical_formula_sum 'C51.50 H44 B Cl3 Fe N6 O4' _chemical_formula_weight 983.94 _chemical_melting_point ? _chemical_oxdiff_formula 'Fe C52 H55 N6 O4 B Cl2' 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 12.2090(3) _cell_length_b 13.0283(4) _cell_length_c 17.0877(5) _cell_angle_alpha 95.921(3) _cell_angle_beta 103.201(3) _cell_angle_gamma 117.095(3) _cell_volume 2287.47(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 24918 _cell_measurement_temperature 100 _cell_measurement_theta_max 31.0278 _cell_measurement_theta_min 3.4240 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1018 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_unetI/netI 0.0662 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 49672 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 31.0278 _diffrn_reflns_theta_min 3.4240 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.912 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -28.00 50.00 1.0000 26.3600 omega____ theta____ kappa____ phi______ frames - 15.4799 -92.0000 -8.0000 78 #__ type_ start__ end____ width___ exp.time_ 2 omega -61.00 38.00 1.0000 26.3600 omega____ theta____ kappa____ phi______ frames - 15.4799 -37.0000 -150.0000 99 #__ type_ start__ end____ width___ exp.time_ 3 omega -18.00 94.00 1.0000 26.3600 omega____ theta____ kappa____ phi______ frames - 15.4799 77.0000 120.0000 112 #__ type_ start__ end____ width___ exp.time_ 4 omega -27.00 -1.00 1.0000 26.3600 omega____ theta____ kappa____ phi______ frames - -15.6362 -92.0000 -104.0000 26 #__ type_ start__ end____ width___ exp.time_ 5 omega -53.00 -23.00 1.0000 26.3600 omega____ theta____ kappa____ phi______ frames - -15.6362 92.0000 -171.0000 30 #__ type_ start__ end____ width___ exp.time_ 6 omega -28.00 55.00 1.0000 26.3600 omega____ theta____ kappa____ phi______ frames - 15.4799 -92.0000 171.0000 83 #__ type_ start__ end____ width___ exp.time_ 7 omega -28.00 55.00 1.0000 26.3600 omega____ theta____ kappa____ phi______ frames - 15.4799 -92.0000 75.0000 83 #__ type_ start__ end____ width___ exp.time_ 8 omega -11.00 92.00 1.0000 26.3600 omega____ theta____ kappa____ phi______ frames - 15.4799 37.0000 30.0000 103 #__ type_ start__ end____ width___ exp.time_ 9 omega -18.00 94.00 1.0000 26.3600 omega____ theta____ kappa____ phi______ frames - 15.4799 77.0000 -90.0000 112 #__ type_ start__ end____ width___ exp.time_ 10 omega -11.00 25.00 1.0000 26.3600 omega____ theta____ kappa____ phi______ frames - 15.4799 37.0000 120.0000 36 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0007676000 _diffrn_orient_matrix_UB_12 0.0457688000 _diffrn_orient_matrix_UB_13 0.0268838000 _diffrn_orient_matrix_UB_21 -0.0083431000 _diffrn_orient_matrix_UB_22 -0.0340370000 _diffrn_orient_matrix_UB_23 0.0301854000 _diffrn_orient_matrix_UB_31 0.0681496000 _diffrn_orient_matrix_UB_32 0.0267069000 _diffrn_orient_matrix_UB_33 0.0171495000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_number_gt 11414 _reflns_number_total 13415 _reflns_odcompleteness_completeness 99.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 28.22 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.557 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.058 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 609 _refine_ls_number_reflns 13415 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0364 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+1.4696P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.0925 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.412688(17) 0.716275(16) 0.233439(11) 0.01245(5) Uani 1 1 d . . . Cl1 Cl 0.82589(5) 0.40620(5) 0.38905(3) 0.04379(12) Uani 1 1 d D . . Cl2 Cl 0.77626(6) 0.56116(5) 0.49264(4) 0.05463(14) Uani 1 1 d D . . Cl3 Cl 0.9665(5) 0.9592(4) 0.08295(17) 0.0454(4) Uani 0.50 1 d PDU A -1 Cl4 Cl 1.0383(5) 1.0430(4) -0.05859(17) 0.0454(4) Uani 0.50 1 d PDU A -1 O1 O 0.31082(9) 0.67728(9) 0.31602(6) 0.01752(19) Uani 1 1 d . . . O2 O 0.57222(9) 0.75311(9) 0.32798(6) 0.01709(19) Uani 1 1 d . . . O3 O 0.28086(10) 0.70582(9) 0.43956(6) 0.0214(2) Uani 1 1 d . . . O4 O 0.70285(10) 0.81651(9) 0.45928(6) 0.0204(2) Uani 1 1 d . . . N1 N 0.27559(10) 0.75134(10) 0.15443(6) 0.0130(2) Uani 1 1 d . . . N2 N 0.25910(10) 0.71697(9) 0.07198(6) 0.01221(19) Uani 1 1 d . . . N3 N 0.54045(10) 0.82112(10) 0.16949(6) 0.0132(2) Uani 1 1 d . . . N4 N 0.49177(10) 0.78166(9) 0.08486(6) 0.01248(19) Uani 1 1 d . . . N5 N 0.35096(10) 0.55517(9) 0.14789(6) 0.0126(2) Uani 1 1 d . . . N6 N 0.33179(10) 0.56363(9) 0.06681(6) 0.01198(19) Uani 1 1 d . . . C1 C 0.14465(14) 0.65302(14) 0.39600(9) 0.0228(3) Uani 1 1 d . . . H49A H 0.1126 0.5729 0.3635 0.034 Uiso 1 1 calc R . . H49B H 0.1313 0.7017 0.3589 0.034 Uiso 1 1 calc R . . H49C H 0.0974 0.6486 0.4360 0.034 Uiso 1 1 calc R . . C2 C 0.35926(13) 0.71340(12) 0.39351(8) 0.0173(2) Uani 1 1 d . . . C3 C 0.48916(14) 0.76232(13) 0.44037(8) 0.0197(3) Uani 1 1 d . . . H47 H 0.5130 0.7874 0.4988 0.024 Uiso 1 1 calc R . . C4 C 0.58458(13) 0.77551(11) 0.40426(8) 0.0166(2) Uani 1 1 d . . . C5 C 0.80667(14) 0.83654(13) 0.42607(9) 0.0213(3) Uani 1 1 d . . . H50A H 0.7914 0.7605 0.3962 0.032 Uiso 1 1 calc R . . H50B H 0.8110 0.8886 0.3880 0.032 Uiso 1 1 calc R . . H50C H 0.8886 0.8742 0.4713 0.032 Uiso 1 1 calc R . . C6 C 0.18258(12) 0.77852(11) 0.15810(8) 0.0145(2) Uani 1 1 d . . . C7 C 0.10295(13) 0.75715(12) 0.07814(8) 0.0169(2) Uani 1 1 d . . . H8 H 0.0285 0.7662 0.0634 0.020 Uiso 1 1 calc R . . C8 C 0.15520(12) 0.72003(11) 0.02500(8) 0.0137(2) Uani 1 1 d . . . C9 C 0.17841(13) 0.83590(11) 0.23532(8) 0.0154(2) Uani 1 1 d . . . C10 C 0.28942(14) 0.90222(12) 0.30375(8) 0.0190(3) Uani 1 1 d . . . H41 H 0.3691 0.9084 0.3014 0.023 Uiso 1 1 calc R . . C11 C 0.28484(16) 0.95928(13) 0.37521(9) 0.0245(3) Uani 1 1 d . . . H42 H 0.3607 1.0031 0.4216 0.029 Uiso 1 1 calc R . . C12 C 0.16904(17) 0.95213(14) 0.37870(9) 0.0268(3) Uani 1 1 d . . . H43 H 0.1655 0.9910 0.4275 0.032 Uiso 1 1 calc R . . C13 C 0.05887(16) 0.88829(13) 0.31090(9) 0.0237(3) Uani 1 1 d . . . H44 H -0.0201 0.8839 0.3131 0.028 Uiso 1 1 calc R . . C14 C 0.06311(14) 0.83042(12) 0.23945(9) 0.0186(3) Uani 1 1 d . . . H45 H -0.0130 0.7869 0.1932 0.022 Uiso 1 1 calc R . . C15 C 0.11337(12) 0.69383(11) -0.06641(8) 0.0139(2) Uani 1 1 d . . . C16 C 0.19791(13) 0.75490(11) -0.10905(8) 0.0154(2) Uani 1 1 d . . . H35 H 0.2854 0.8118 -0.0792 0.019 Uiso 1 1 calc R . . C17 C 0.15522(14) 0.73318(12) -0.19488(8) 0.0179(3) Uani 1 1 d . . . H36 H 0.2131 0.7755 -0.2235 0.022 Uiso 1 1 calc R . . C18 C 0.02733(14) 0.64924(13) -0.23856(8) 0.0193(3) Uani 1 1 d . . . H37 H -0.0025 0.6351 -0.2971 0.023 Uiso 1 1 calc R . . C19 C -0.05675(13) 0.58615(13) -0.19680(8) 0.0197(3) Uani 1 1 d . . . H38 H -0.1434 0.5274 -0.2270 0.024 Uiso 1 1 calc R . . C20 C -0.01446(13) 0.60867(12) -0.11085(8) 0.0175(2) Uani 1 1 d . . . H39 H -0.0726 0.5661 -0.0824 0.021 Uiso 1 1 calc R . . C21 C 0.65599(12) 0.91972(11) 0.18599(8) 0.0144(2) Uani 1 1 d . . . C22 C 0.68208(12) 0.94328(12) 0.11236(8) 0.0165(2) Uani 1 1 d . . . H2 H 0.7574 1.0068 0.1068 0.020 Uiso 1 1 calc R . . C23 C 0.57577(12) 0.85502(11) 0.04928(8) 0.0139(2) Uani 1 1 d . . . C24 C 0.73673(12) 0.99545(11) 0.26981(8) 0.0149(2) Uani 1 1 d . . . C25 C 0.87149(13) 1.05399(12) 0.28930(8) 0.0180(3) Uani 1 1 d . . . H21 H 0.9100 1.0405 0.2499 0.022 Uiso 1 1 calc R . . C26 C 0.94949(13) 1.13195(13) 0.36622(9) 0.0215(3) Uani 1 1 d . . . H20 H 1.0410 1.1711 0.3792 0.026 Uiso 1 1 calc R . . C27 C 0.89411(14) 1.15263(13) 0.42384(9) 0.0227(3) Uani 1 1 d . . . H19 H 0.9476 1.2058 0.4763 0.027 Uiso 1 1 calc R . . C28 C 0.75994(14) 1.09553(13) 0.40489(9) 0.0215(3) Uani 1 1 d . . . H18 H 0.7218 1.1096 0.4444 0.026 Uiso 1 1 calc R . . C29 C 0.68216(13) 1.01811(12) 0.32823(8) 0.0175(2) Uani 1 1 d . . . H17 H 0.5907 0.9800 0.3153 0.021 Uiso 1 1 calc R . . C30 C 0.55086(12) 0.84379(11) -0.04077(8) 0.0138(2) Uani 1 1 d . . . C31 C 0.57528(13) 0.94569(12) -0.07038(8) 0.0182(3) Uani 1 1 d . . . H15 H 0.6072 1.0192 -0.0327 0.022 Uiso 1 1 calc R . . C32 C 0.55330(14) 0.94033(13) -0.15447(9) 0.0215(3) Uani 1 1 d . . . H14 H 0.5700 1.0100 -0.1741 0.026 Uiso 1 1 calc R . . C33 C 0.50708(15) 0.83351(14) -0.20981(9) 0.0236(3) Uani 1 1 d . . . H13 H 0.4916 0.8297 -0.2674 0.028 Uiso 1 1 calc R . . C34 C 0.48350(15) 0.73203(13) -0.18083(9) 0.0217(3) Uani 1 1 d . . . H12 H 0.4522 0.6588 -0.2187 0.026 Uiso 1 1 calc R . . C35 C 0.50536(13) 0.73694(12) -0.09688(8) 0.0164(2) Uani 1 1 d . . . H11 H 0.4893 0.6672 -0.0775 0.020 Uiso 1 1 calc R . . C36 C 0.32486(12) 0.44260(11) 0.14706(8) 0.0137(2) Uani 1 1 d . . . C37 C 0.29044(12) 0.37954(11) 0.06590(8) 0.0153(2) Uani 1 1 d . . . H5 H 0.2681 0.2990 0.0483 0.018 Uiso 1 1 calc R . . C38 C 0.29555(12) 0.45844(11) 0.01663(8) 0.0129(2) Uani 1 1 d . . . C39 C 0.32698(13) 0.39312(12) 0.22085(8) 0.0159(2) Uani 1 1 d . . . C40 C 0.40806(14) 0.46178(13) 0.29981(8) 0.0200(3) Uani 1 1 d . . . H29 H 0.4660 0.5440 0.3077 0.024 Uiso 1 1 calc R . . C41 C 0.40443(16) 0.41027(15) 0.36718(9) 0.0263(3) Uani 1 1 d . . . H30 H 0.4587 0.4581 0.4211 0.032 Uiso 1 1 calc R . . C42 C 0.32245(16) 0.28988(15) 0.35656(10) 0.0275(3) Uani 1 1 d . . . H31 H 0.3209 0.2552 0.4028 0.033 Uiso 1 1 calc R . . C43 C 0.24299(16) 0.22089(15) 0.27812(10) 0.0279(3) Uani 1 1 d . . . H32 H 0.1874 0.1382 0.2702 0.033 Uiso 1 1 calc R . . C44 C 0.24426(15) 0.27220(13) 0.21083(9) 0.0240(3) Uani 1 1 d . . . H33 H 0.1881 0.2244 0.1573 0.029 Uiso 1 1 calc R . . C45 C 0.27032(12) 0.43746(11) -0.07391(8) 0.0133(2) Uani 1 1 d . . . C46 C 0.18574(13) 0.46548(12) -0.12463(8) 0.0162(2) Uani 1 1 d . . . H23 H 0.1400 0.4961 -0.1012 0.019 Uiso 1 1 calc R . . C47 C 0.16811(14) 0.44893(12) -0.20903(8) 0.0198(3) Uani 1 1 d . . . H24 H 0.1123 0.4702 -0.2430 0.024 Uiso 1 1 calc R . . C48 C 0.23201(15) 0.40131(12) -0.24391(8) 0.0210(3) Uani 1 1 d . . . H25 H 0.2207 0.3910 -0.3016 0.025 Uiso 1 1 calc R . . C49 C 0.31234(14) 0.36870(13) -0.19481(9) 0.0211(3) Uani 1 1 d . . . H26 H 0.3538 0.3338 -0.2191 0.025 Uiso 1 1 calc R . . C50 C 0.33204(13) 0.38718(12) -0.10986(8) 0.0177(3) Uani 1 1 d . . . H27 H 0.3877 0.3655 -0.0762 0.021 Uiso 1 1 calc R . . C51 C 0.70836(16) 0.42936(15) 0.41698(10) 0.0288(3) Uani 1 1 d D . . H51A H 0.6503 0.4321 0.3673 0.035 Uiso 1 1 calc R . . H51B H 0.6554 0.3617 0.4382 0.035 Uiso 1 1 calc R . . C52 C 0.9228(5) 1.0126(5) -0.0039(4) 0.0620(15) Uani 0.50 1 d PDU A -1 H52A H 0.9205 1.0859 0.0149 0.074 Uiso 0.50 1 calc PR A -1 H52B H 0.8355 0.9524 -0.0410 0.074 Uiso 0.50 1 calc PR A -1 B1 B 0.35068(13) 0.68075(12) 0.04368(8) 0.0112(2) Uani 1 1 d . . . H1 H 0.3297 0.6687 -0.0178 0.013 Uiso 1 1 calc R . . 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 0.01374(8) 0.01359(9) 0.00857(8) 0.00217(6) 0.00266(6) 0.00606(7) Cl1 0.0535(3) 0.0594(3) 0.0391(2) 0.0199(2) 0.0258(2) 0.0376(3) Cl2 0.0731(4) 0.0346(3) 0.0516(3) -0.0013(2) 0.0174(3) 0.0262(3) Cl3 0.0589(5) 0.0426(3) 0.0572(15) 0.0211(13) 0.0307(14) 0.0355(3) Cl4 0.0589(5) 0.0426(3) 0.0572(15) 0.0211(13) 0.0307(14) 0.0355(3) O1 0.0189(4) 0.0199(5) 0.0119(4) 0.0037(3) 0.0053(4) 0.0079(4) O2 0.0182(4) 0.0188(5) 0.0103(4) 0.0027(3) 0.0022(3) 0.0071(4) O3 0.0228(5) 0.0254(5) 0.0141(4) 0.0036(4) 0.0088(4) 0.0093(4) O4 0.0195(5) 0.0243(5) 0.0120(4) 0.0026(4) 0.0014(4) 0.0085(4) N1 0.0161(5) 0.0141(5) 0.0090(4) 0.0021(4) 0.0045(4) 0.0075(4) N2 0.0141(5) 0.0130(5) 0.0091(4) 0.0019(4) 0.0034(4) 0.0066(4) N3 0.0135(5) 0.0137(5) 0.0094(4) 0.0018(4) 0.0013(4) 0.0056(4) N4 0.0132(5) 0.0134(5) 0.0094(4) 0.0028(4) 0.0022(4) 0.0059(4) N5 0.0139(5) 0.0137(5) 0.0099(4) 0.0040(4) 0.0035(4) 0.0063(4) N6 0.0134(5) 0.0130(5) 0.0089(4) 0.0026(4) 0.0032(4) 0.0061(4) C1 0.0226(7) 0.0237(7) 0.0214(7) 0.0052(5) 0.0097(6) 0.0095(6) C2 0.0229(6) 0.0147(6) 0.0138(6) 0.0043(5) 0.0077(5) 0.0078(5) C3 0.0230(6) 0.0207(7) 0.0101(5) 0.0015(5) 0.0040(5) 0.0074(5) C4 0.0207(6) 0.0120(6) 0.0117(5) 0.0023(4) 0.0008(5) 0.0058(5) C5 0.0199(6) 0.0249(7) 0.0169(6) 0.0029(5) 0.0018(5) 0.0117(6) C6 0.0153(5) 0.0135(6) 0.0143(6) 0.0023(4) 0.0053(5) 0.0066(5) C7 0.0166(6) 0.0197(6) 0.0152(6) 0.0011(5) 0.0036(5) 0.0108(5) C8 0.0137(5) 0.0134(6) 0.0134(5) 0.0018(4) 0.0027(4) 0.0071(5) C9 0.0200(6) 0.0130(6) 0.0143(6) 0.0040(4) 0.0077(5) 0.0079(5) C10 0.0215(6) 0.0164(6) 0.0156(6) 0.0019(5) 0.0061(5) 0.0066(5) C11 0.0331(8) 0.0174(7) 0.0159(6) -0.0004(5) 0.0070(6) 0.0080(6) C12 0.0441(9) 0.0194(7) 0.0210(7) 0.0023(5) 0.0179(7) 0.0159(7) C13 0.0333(8) 0.0212(7) 0.0268(7) 0.0078(6) 0.0187(6) 0.0170(6) C14 0.0230(6) 0.0164(6) 0.0193(6) 0.0047(5) 0.0096(5) 0.0106(5) C15 0.0156(5) 0.0155(6) 0.0117(5) 0.0015(4) 0.0019(4) 0.0101(5) C16 0.0161(6) 0.0140(6) 0.0143(6) 0.0022(4) 0.0020(5) 0.0073(5) C17 0.0234(6) 0.0165(6) 0.0155(6) 0.0050(5) 0.0059(5) 0.0109(5) C18 0.0239(6) 0.0229(7) 0.0117(6) 0.0022(5) 0.0013(5) 0.0144(6) C19 0.0158(6) 0.0237(7) 0.0156(6) -0.0004(5) -0.0002(5) 0.0099(5) C20 0.0148(6) 0.0218(7) 0.0156(6) 0.0028(5) 0.0036(5) 0.0097(5) C21 0.0141(5) 0.0131(6) 0.0134(5) 0.0034(4) 0.0020(4) 0.0056(5) C22 0.0144(5) 0.0163(6) 0.0153(6) 0.0058(5) 0.0039(5) 0.0046(5) C23 0.0145(5) 0.0136(6) 0.0139(5) 0.0049(4) 0.0045(5) 0.0068(5) C24 0.0153(5) 0.0128(6) 0.0126(5) 0.0035(4) 0.0005(5) 0.0054(5) C25 0.0156(6) 0.0192(6) 0.0159(6) 0.0047(5) 0.0025(5) 0.0068(5) C26 0.0152(6) 0.0207(7) 0.0200(6) 0.0031(5) -0.0009(5) 0.0052(5) C27 0.0220(7) 0.0194(7) 0.0173(6) -0.0021(5) -0.0022(5) 0.0078(5) C28 0.0225(7) 0.0221(7) 0.0174(6) 0.0004(5) 0.0038(5) 0.0110(6) C29 0.0159(6) 0.0163(6) 0.0172(6) 0.0028(5) 0.0024(5) 0.0070(5) C30 0.0119(5) 0.0159(6) 0.0127(5) 0.0043(4) 0.0045(4) 0.0057(5) C31 0.0191(6) 0.0158(6) 0.0159(6) 0.0045(5) 0.0055(5) 0.0056(5) C32 0.0251(7) 0.0204(7) 0.0184(6) 0.0103(5) 0.0085(5) 0.0089(6) C33 0.0287(7) 0.0286(8) 0.0137(6) 0.0077(5) 0.0092(5) 0.0127(6) C34 0.0288(7) 0.0219(7) 0.0159(6) 0.0019(5) 0.0097(5) 0.0130(6) C35 0.0192(6) 0.0170(6) 0.0171(6) 0.0060(5) 0.0088(5) 0.0104(5) C36 0.0131(5) 0.0142(6) 0.0130(5) 0.0043(4) 0.0031(4) 0.0064(5) C37 0.0170(6) 0.0128(6) 0.0150(6) 0.0033(4) 0.0041(5) 0.0070(5) C38 0.0127(5) 0.0132(6) 0.0121(5) 0.0019(4) 0.0028(4) 0.0065(4) C39 0.0180(6) 0.0180(6) 0.0151(6) 0.0076(5) 0.0063(5) 0.0104(5) C40 0.0243(7) 0.0207(7) 0.0162(6) 0.0064(5) 0.0055(5) 0.0119(6) C41 0.0324(8) 0.0345(8) 0.0160(6) 0.0099(6) 0.0072(6) 0.0192(7) C42 0.0316(8) 0.0372(9) 0.0250(7) 0.0204(7) 0.0140(6) 0.0212(7) C43 0.0308(8) 0.0247(8) 0.0314(8) 0.0176(6) 0.0133(7) 0.0124(6) C44 0.0254(7) 0.0201(7) 0.0213(7) 0.0084(5) 0.0052(6) 0.0073(6) C45 0.0153(5) 0.0109(5) 0.0117(5) 0.0007(4) 0.0038(4) 0.0054(4) C46 0.0184(6) 0.0140(6) 0.0142(6) 0.0001(4) 0.0019(5) 0.0086(5) C47 0.0253(7) 0.0163(6) 0.0144(6) 0.0019(5) 0.0000(5) 0.0107(5) C48 0.0299(7) 0.0172(6) 0.0127(6) 0.0021(5) 0.0074(5) 0.0091(6) C49 0.0252(7) 0.0218(7) 0.0187(6) 0.0022(5) 0.0110(5) 0.0124(6) C50 0.0200(6) 0.0187(6) 0.0169(6) 0.0031(5) 0.0055(5) 0.0119(5) C51 0.0287(8) 0.0294(8) 0.0271(8) 0.0095(6) 0.0106(6) 0.0121(7) C52 0.066(3) 0.074(3) 0.109(4) 0.065(3) 0.065(3) 0.059(3) B1 0.0121(6) 0.0113(6) 0.0098(5) 0.0021(4) 0.0031(5) 0.0057(5) _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 2.0422(9) . ? Fe1 O2 2.0458(9) . ? Fe1 N1 2.1505(11) . ? Fe1 N3 2.1537(11) . ? Fe1 N5 2.1291(11) . ? Cl1 C51 1.7480(17) . ? Cl2 C51 1.7500(18) . ? Cl3 C52 1.778(6) . ? Cl4 C52 1.785(6) . ? O1 C2 1.2589(16) . ? O2 C4 1.2642(15) . ? O3 C1 1.4421(18) . ? O3 C2 1.3487(16) . ? O4 C4 1.3520(16) . ? O4 C5 1.4333(17) . ? N1 C6 1.3465(16) . ? N2 N1 1.3726(14) . ? N2 C8 1.3575(16) . ? N2 B1 1.5452(17) . ? N3 C21 1.3462(16) . ? N4 N3 1.3728(14) . ? N4 C23 1.3590(16) . ? N4 B1 1.5438(17) . ? N5 C36 1.3493(16) . ? N6 N5 1.3760(14) . ? N6 C38 1.3568(16) . ? N6 B1 1.5437(17) . ? C1 H49A 0.9800 . ? C1 H49B 0.9800 . ? C1 H49C 0.9800 . ? C2 C3 1.3987(19) . ? C3 H47 0.9500 . ? C3 C4 1.391(2) . ? C5 H50A 0.9800 . ? C5 H50B 0.9800 . ? C5 H50C 0.9800 . ? C6 C9 1.4711(17) . ? C7 C6 1.3992(18) . ? C7 H8 0.9500 . ? C8 C7 1.3858(17) . ? C8 C15 1.4778(17) . ? C9 C10 1.3971(19) . ? C9 C14 1.3953(19) . ? C10 H41 0.9500 . ? C10 C11 1.3887(19) . ? C11 H42 0.9500 . ? C11 C12 1.389(2) . ? C12 H43 0.9500 . ? C12 C13 1.383(2) . ? C13 H44 0.9500 . ? C13 C14 1.3916(19) . ? C14 H45 0.9500 . ? C15 C16 1.3944(18) . ? C15 C20 1.3967(18) . ? C16 H35 0.9500 . ? C16 C17 1.3905(18) . ? C17 H36 0.9500 . ? C17 C18 1.3910(19) . ? C18 H37 0.9500 . ? C18 C19 1.388(2) . ? C19 H38 0.9500 . ? C19 C20 1.3916(18) . ? C20 H39 0.9500 . ? C21 C24 1.4745(17) . ? C22 C21 1.3973(18) . ? C22 H2 0.9500 . ? C23 C22 1.3836(18) . ? C23 C30 1.4768(17) . ? C24 C25 1.3978(18) . ? C24 C29 1.3963(19) . ? C25 H21 0.9500 . ? C26 C25 1.3921(19) . ? C26 H20 0.9500 . ? C27 C26 1.384(2) . ? C27 H19 0.9500 . ? C28 C27 1.393(2) . ? C28 H18 0.9500 . ? C29 C28 1.3863(19) . ? C29 H17 0.9500 . ? C30 C31 1.3979(18) . ? C30 C35 1.3938(18) . ? C31 H15 0.9500 . ? C32 C31 1.3885(19) . ? C32 H14 0.9500 . ? C33 C32 1.385(2) . ? C33 H13 0.9500 . ? C34 C33 1.389(2) . ? C34 H12 0.9500 . ? C35 C34 1.3869(19) . ? C35 H11 0.9500 . ? C36 C39 1.4745(17) . ? C37 C36 1.3997(17) . ? C37 H5 0.9500 . ? C38 C37 1.3832(18) . ? C38 C45 1.4770(17) . ? C39 C40 1.3910(19) . ? C39 C44 1.395(2) . ? C40 H29 0.9500 . ? C40 C41 1.390(2) . ? C41 H30 0.9500 . ? C41 C42 1.387(2) . ? C42 H31 0.9500 . ? C42 C43 1.382(2) . ? C43 H32 0.9500 . ? C43 C44 1.388(2) . ? C44 H33 0.9500 . ? C45 C46 1.3968(18) . ? C45 C50 1.3973(18) . ? C46 H23 0.9500 . ? C46 C47 1.3872(18) . ? C47 H24 0.9500 . ? C47 C48 1.388(2) . ? C48 H25 0.9500 . ? C48 C49 1.387(2) . ? C49 H26 0.9500 . ? C49 C50 1.3922(19) . ? C50 H27 0.9500 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? B1 H1 1.0000 . ? 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 O2 87.50(4) . . ? O1 Fe1 N1 92.16(4) . . ? O1 Fe1 N3 159.16(4) . . ? O1 Fe1 N5 108.31(4) . . ? O2 Fe1 N1 157.09(4) . . ? O2 Fe1 N3 88.54(4) . . ? O2 Fe1 N5 109.58(4) . . ? N1 Fe1 N3 83.68(4) . . ? N5 Fe1 N1 92.28(4) . . ? N5 Fe1 N3 92.29(4) . . ? C2 O1 Fe1 125.25(9) . . ? C4 O2 Fe1 125.43(9) . . ? C2 O3 C1 117.02(11) . . ? C4 O4 C5 116.91(10) . . ? N2 N1 Fe1 112.69(8) . . ? C6 N1 Fe1 139.58(9) . . ? C6 N1 N2 106.51(10) . . ? N1 N2 B1 121.21(10) . . ? C8 N2 N1 110.00(10) . . ? C8 N2 B1 128.79(10) . . ? N4 N3 Fe1 113.91(8) . . ? C21 N3 Fe1 139.76(9) . . ? C21 N3 N4 106.27(10) . . ? N3 N4 B1 120.02(10) . . ? C23 N4 N3 110.19(10) . . ? C23 N4 B1 128.94(10) . . ? N6 N5 Fe1 113.85(8) . . ? C36 N5 Fe1 139.92(9) . . ? C36 N5 N6 106.22(10) . . ? N5 N6 B1 120.79(10) . . ? C38 N6 N5 110.20(10) . . ? C38 N6 B1 129.01(10) . . ? O3 C1 H49A 109.5 . . ? O3 C1 H49B 109.5 . . ? O3 C1 H49C 109.5 . . ? H49B C1 H49A 109.5 . . ? H49B C1 H49C 109.5 . . ? H49C C1 H49A 109.5 . . ? O1 C2 O3 118.86(12) . . ? O1 C2 C3 127.53(13) . . ? O3 C2 C3 113.61(11) . . ? C2 C3 H47 118.9 . . ? C4 C3 C2 122.23(12) . . ? C4 C3 H47 118.9 . . ? O2 C4 O4 118.22(12) . . ? O2 C4 C3 127.67(12) . . ? O4 C4 C3 114.11(11) . . ? O4 C5 H50A 109.5 . . ? O4 C5 H50B 109.5 . . ? O4 C5 H50C 109.5 . . ? H50A C5 H50C 109.5 . . ? H50B C5 H50A 109.5 . . ? H50B C5 H50C 109.5 . . ? N1 C6 C7 109.99(11) . . ? N1 C6 C9 123.38(11) . . ? C7 C6 C9 126.23(12) . . ? C6 C7 H8 127.1 . . ? C8 C7 C6 105.71(11) . . ? C8 C7 H8 127.1 . . ? N2 C8 C7 107.73(11) . . ? N2 C8 C15 124.36(11) . . ? C7 C8 C15 127.84(12) . . ? C10 C9 C6 121.57(12) . . ? C14 C9 C6 119.75(12) . . ? C14 C9 C10 118.58(12) . . ? C9 C10 H41 119.6 . . ? C11 C10 C9 120.89(14) . . ? C11 C10 H41 119.6 . . ? C10 C11 H42 120.1 . . ? C10 C11 C12 119.88(14) . . ? C12 C11 H42 120.1 . . ? C11 C12 H43 120.1 . . ? C13 C12 C11 119.82(13) . . ? C13 C12 H43 120.1 . . ? C12 C13 H44 119.8 . . ? C12 C13 C14 120.37(14) . . ? C14 C13 H44 119.8 . . ? C9 C14 H45 119.8 . . ? C13 C14 C9 120.45(13) . . ? C13 C14 H45 119.8 . . ? C16 C15 C8 121.31(11) . . ? C16 C15 C20 119.36(12) . . ? C20 C15 C8 119.31(12) . . ? C15 C16 H35 119.7 . . ? C17 C16 C15 120.55(12) . . ? C17 C16 H35 119.7 . . ? C16 C17 H36 120.2 . . ? C16 C17 C18 119.69(13) . . ? C18 C17 H36 120.2 . . ? C17 C18 H37 119.9 . . ? C19 C18 C17 120.17(12) . . ? C19 C18 H37 119.9 . . ? C18 C19 H38 119.9 . . ? C18 C19 C20 120.17(13) . . ? C20 C19 H38 119.9 . . ? C15 C20 H39 120.0 . . ? C19 C20 C15 120.04(13) . . ? C19 C20 H39 120.0 . . ? N3 C21 C22 110.15(11) . . ? N3 C21 C24 123.92(11) . . ? C22 C21 C24 125.77(12) . . ? C21 C22 H2 127.1 . . ? C23 C22 C21 105.86(11) . . ? C23 C22 H2 127.1 . . ? N4 C23 C22 107.52(11) . . ? N4 C23 C30 124.80(11) . . ? C22 C23 C30 127.58(12) . . ? C25 C24 C21 119.33(12) . . ? C29 C24 C21 121.61(12) . . ? C29 C24 C25 118.84(12) . . ? C24 C25 H21 119.8 . . ? C26 C25 C24 120.33(13) . . ? C26 C25 H21 119.8 . . ? C25 C26 H20 119.9 . . ? C27 C26 C25 120.20(13) . . ? C27 C26 H20 119.9 . . ? C26 C27 H19 120.0 . . ? C26 C27 C28 119.99(13) . . ? C28 C27 H19 120.0 . . ? C27 C28 H18 120.1 . . ? C29 C28 C27 119.85(13) . . ? C29 C28 H18 120.1 . . ? C24 C29 H17 119.6 . . ? C28 C29 C24 120.77(13) . . ? C28 C29 H17 119.6 . . ? C31 C30 C23 118.03(12) . . ? C35 C30 C23 122.99(12) . . ? C35 C30 C31 118.98(12) . . ? C30 C31 H15 119.7 . . ? C32 C31 C30 120.53(13) . . ? C32 C31 H15 119.7 . . ? C31 C32 H14 120.0 . . ? C33 C32 C31 120.05(13) . . ? C33 C32 H14 120.0 . . ? C32 C33 H13 120.1 . . ? C32 C33 C34 119.78(13) . . ? C34 C33 H13 120.1 . . ? C33 C34 H12 119.8 . . ? C35 C34 C33 120.39(13) . . ? C35 C34 H12 119.8 . . ? C30 C35 H11 119.9 . . ? C34 C35 C30 120.27(13) . . ? C34 C35 H11 119.9 . . ? N5 C36 C37 109.98(11) . . ? N5 C36 C39 124.42(11) . . ? C37 C36 C39 125.54(12) . . ? C36 C37 H5 127.0 . . ? C38 C37 C36 105.94(11) . . ? C38 C37 H5 127.0 . . ? N6 C38 C37 107.66(11) . . ? N6 C38 C45 124.34(11) . . ? C37 C38 C45 127.98(12) . . ? C40 C39 C36 122.79(12) . . ? C40 C39 C44 118.73(13) . . ? C44 C39 C36 118.48(12) . . ? C39 C40 H29 119.9 . . ? C41 C40 C39 120.12(14) . . ? C41 C40 H29 119.9 . . ? C40 C41 H30 119.6 . . ? C42 C41 C40 120.73(14) . . ? C42 C41 H30 119.6 . . ? C41 C42 H31 120.3 . . ? C43 C42 C41 119.42(14) . . ? C43 C42 H31 120.3 . . ? C42 C43 H32 119.9 . . ? C42 C43 C44 120.14(15) . . ? C44 C43 H32 119.9 . . ? C39 C44 H33 119.6 . . ? C43 C44 C39 120.84(14) . . ? C43 C44 H33 119.6 . . ? C46 C45 C38 121.89(11) . . ? C46 C45 C50 119.10(12) . . ? C50 C45 C38 119.00(12) . . ? C45 C46 H23 119.8 . . ? C47 C46 C45 120.39(12) . . ? C47 C46 H23 119.8 . . ? C46 C47 H24 120.0 . . ? C46 C47 C48 120.03(13) . . ? C48 C47 H24 120.0 . . ? C47 C48 H25 119.9 . . ? C49 C48 C47 120.21(13) . . ? C49 C48 H25 119.9 . . ? C48 C49 H26 120.1 . . ? C48 C49 C50 119.88(13) . . ? C50 C49 H26 120.1 . . ? C45 C50 H27 119.8 . . ? C49 C50 C45 120.32(13) . . ? C49 C50 H27 119.8 . . ? Cl1 C51 Cl2 112.33(9) . . ? Cl1 C51 H51A 109.1 . . ? Cl1 C51 H51B 109.1 . . ? Cl2 C51 H51A 109.1 . . ? Cl2 C51 H51B 109.1 . . ? H51B C51 H51A 107.9 . . ? Cl3 C52 Cl4 109.3(3) . . ? Cl3 C52 H52A 109.8 . . ? Cl3 C52 H52B 109.8 . . ? Cl4 C52 H52A 109.8 . . ? Cl4 C52 H52B 109.8 . . ? H52A C52 H52B 108.3 . . ? N2 B1 H1 109.0 . . ? N4 B1 N2 108.99(10) . . ? N4 B1 H1 109.0 . . ? N6 B1 N2 109.98(10) . . ? N6 B1 N4 110.93(10) . . ? N6 B1 H1 109.0 . . ? 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 Fe1 O1 C2 O3 164.03(9) . . . . ? Fe1 O1 C2 C3 -16.1(2) . . . . ? Fe1 O2 C4 O4 -169.63(9) . . . . ? Fe1 O2 C4 C3 10.9(2) . . . . ? Fe1 N1 C6 C7 -163.21(10) . . . . ? Fe1 N1 C6 C9 23.7(2) . . . . ? Fe1 N3 C21 C22 -177.35(10) . . . . ? Fe1 N3 C21 C24 -1.7(2) . . . . ? Fe1 N5 C36 C37 -178.20(10) . . . . ? Fe1 N5 C36 C39 4.3(2) . . . . ? O1 Fe1 O2 C4 -19.12(11) . . . . ? O1 Fe1 N1 N2 -144.87(8) . . . . ? O1 Fe1 N1 C6 20.12(14) . . . . ? O1 Fe1 N3 N4 -133.46(11) . . . . ? O1 Fe1 N3 C21 43.3(2) . . . . ? O1 Fe1 N5 N6 136.22(8) . . . . ? O1 Fe1 N5 C36 -45.03(14) . . . . ? O1 C2 C3 C4 -1.1(2) . . . . ? O2 Fe1 O1 C2 21.55(11) . . . . ? O2 Fe1 N1 N2 126.45(10) . . . . ? O2 Fe1 N1 C6 -68.56(18) . . . . ? O2 Fe1 N3 N4 147.47(9) . . . . ? O2 Fe1 N3 C21 -35.73(14) . . . . ? O2 Fe1 N5 N6 -129.82(8) . . . . ? O2 Fe1 N5 C36 48.93(14) . . . . ? O3 C2 C3 C4 178.81(13) . . . . ? N1 Fe1 O1 C2 -135.53(11) . . . . ? N1 Fe1 O2 C4 70.50(15) . . . . ? N1 Fe1 N3 N4 -54.10(8) . . . . ? N1 Fe1 N3 C21 122.70(14) . . . . ? N1 Fe1 N5 N6 43.19(8) . . . . ? N1 Fe1 N5 C36 -138.05(13) . . . . ? N1 N2 C8 C7 -0.05(14) . . . . ? N1 N2 C8 C15 177.01(11) . . . . ? N1 N2 B1 N4 -54.20(14) . . . . ? N1 N2 B1 N6 67.60(14) . . . . ? N1 C6 C9 C10 22.4(2) . . . . ? N1 C6 C9 C14 -161.46(13) . . . . ? N2 N1 C6 C7 2.37(14) . . . . ? N2 N1 C6 C9 -170.74(11) . . . . ? N2 C8 C7 C6 1.45(15) . . . . ? N2 C8 C15 C16 -55.32(18) . . . . ? N2 C8 C15 C20 126.60(14) . . . . ? N3 Fe1 O1 C2 -57.70(17) . . . . ? N3 Fe1 O2 C4 140.41(11) . . . . ? N3 Fe1 N1 N2 55.61(8) . . . . ? N3 Fe1 N1 C6 -139.39(14) . . . . ? N3 Fe1 N5 N6 -40.56(8) . . . . ? N3 Fe1 N5 C36 138.19(13) . . . . ? N3 N4 C23 C22 0.73(14) . . . . ? N3 N4 C23 C30 -175.84(12) . . . . ? N3 N4 B1 N2 56.26(14) . . . . ? N3 N4 B1 N6 -64.97(14) . . . . ? N3 C21 C24 C25 147.47(13) . . . . ? N3 C21 C24 C29 -37.9(2) . . . . ? N4 N3 C21 C22 -0.40(14) . . . . ? N4 N3 C21 C24 175.25(12) . . . . ? N4 C23 C22 C21 -0.93(15) . . . . ? N4 C23 C30 C31 131.69(14) . . . . ? N4 C23 C30 C35 -48.82(19) . . . . ? N5 Fe1 O1 C2 131.36(11) . . . . ? N5 Fe1 O2 C4 -127.68(10) . . . . ? N5 Fe1 N1 N2 -36.44(8) . . . . ? N5 Fe1 N1 C6 128.55(14) . . . . ? N5 Fe1 N3 N4 37.93(9) . . . . ? N5 Fe1 N3 C21 -145.27(14) . . . . ? N5 N6 C38 C37 0.23(14) . . . . ? N5 N6 C38 C45 -178.41(11) . . . . ? N5 N6 B1 N2 -58.85(14) . . . . ? N5 N6 B1 N4 61.80(14) . . . . ? N5 C36 C39 C40 -30.3(2) . . . . ? N5 C36 C39 C44 149.80(14) . . . . ? N6 N5 C36 C37 0.61(14) . . . . ? N6 N5 C36 C39 -176.84(11) . . . . ? N6 C38 C37 C36 0.14(14) . . . . ? N6 C38 C45 C46 -52.11(18) . . . . ? N6 C38 C45 C50 128.46(14) . . . . ? C1 O3 C2 O1 1.70(19) . . . . ? C1 O3 C2 C3 -178.21(12) . . . . ? C2 C3 C4 O2 4.0(2) . . . . ? C2 C3 C4 O4 -175.55(13) . . . . ? C5 O4 C4 O2 2.82(18) . . . . ? C5 O4 C4 C3 -177.62(12) . . . . ? C6 C9 C10 C11 177.74(13) . . . . ? C6 C9 C14 C13 -177.38(13) . . . . ? C7 C6 C9 C10 -149.60(14) . . . . ? C7 C6 C9 C14 26.6(2) . . . . ? C7 C8 C15 C16 121.12(15) . . . . ? C7 C8 C15 C20 -56.95(19) . . . . ? C8 N2 N1 Fe1 168.48(8) . . . . ? C8 N2 N1 C6 -1.44(14) . . . . ? C8 N2 B1 N4 126.39(13) . . . . ? C8 N2 B1 N6 -111.81(13) . . . . ? C8 C7 C6 N1 -2.40(15) . . . . ? C8 C7 C6 C9 170.46(12) . . . . ? C8 C15 C16 C17 -176.86(12) . . . . ? C8 C15 C20 C19 177.55(12) . . . . ? C9 C10 C11 C12 -0.9(2) . . . . ? C10 C9 C14 C13 -1.1(2) . . . . ? C10 C11 C12 C13 -0.1(2) . . . . ? C11 C12 C13 C14 0.5(2) . . . . ? C12 C13 C14 C9 0.1(2) . . . . ? C14 C9 C10 C11 1.5(2) . . . . ? C15 C8 C7 C6 -175.47(13) . . . . ? C15 C16 C17 C18 -0.4(2) . . . . ? C16 C15 C20 C19 -0.6(2) . . . . ? C16 C17 C18 C19 -1.0(2) . . . . ? C17 C18 C19 C20 1.6(2) . . . . ? C18 C19 C20 C15 -0.8(2) . . . . ? C20 C15 C16 C17 1.21(19) . . . . ? C21 C24 C25 C26 175.81(13) . . . . ? C21 C24 C29 C28 -175.86(13) . . . . ? C22 C21 C24 C25 -37.6(2) . . . . ? C22 C21 C24 C29 137.06(14) . . . . ? C22 C23 C30 C31 -44.2(2) . . . . ? C22 C23 C30 C35 135.31(15) . . . . ? C23 N4 N3 Fe1 177.64(8) . . . . ? C23 N4 N3 C21 -0.20(14) . . . . ? C23 N4 B1 N2 -112.09(13) . . . . ? C23 N4 B1 N6 126.68(13) . . . . ? C23 C22 C21 N3 0.84(15) . . . . ? C23 C22 C21 C24 -174.71(12) . . . . ? C23 C30 C31 C32 -179.83(12) . . . . ? C23 C30 C35 C34 179.83(12) . . . . ? C24 C29 C28 C27 0.7(2) . . . . ? C25 C24 C29 C28 -1.2(2) . . . . ? C27 C26 C25 C24 -0.4(2) . . . . ? C28 C27 C26 C25 -0.1(2) . . . . ? C29 C24 C25 C26 1.0(2) . . . . ? C29 C28 C27 C26 0.0(2) . . . . ? C30 C23 C22 C21 175.51(13) . . . . ? C30 C35 C34 C33 0.2(2) . . . . ? C31 C30 C35 C34 -0.7(2) . . . . ? C33 C32 C31 C30 -0.1(2) . . . . ? C34 C33 C32 C31 -0.3(2) . . . . ? C35 C30 C31 C32 0.7(2) . . . . ? C35 C34 C33 C32 0.3(2) . . . . ? C36 C39 C40 C41 179.17(13) . . . . ? C36 C39 C44 C43 179.55(14) . . . . ? C37 C36 C39 C40 152.59(14) . . . . ? C37 C36 C39 C44 -27.3(2) . . . . ? C37 C38 C45 C46 129.53(15) . . . . ? C37 C38 C45 C50 -49.90(19) . . . . ? C38 N6 N5 Fe1 178.64(8) . . . . ? C38 N6 N5 C36 -0.53(13) . . . . ? C38 N6 B1 N2 120.56(13) . . . . ? C38 N6 B1 N4 -118.79(13) . . . . ? C38 C37 C36 N5 -0.48(15) . . . . ? C38 C37 C36 C39 176.94(12) . . . . ? C38 C45 C46 C47 177.48(12) . . . . ? C38 C45 C50 C49 -178.62(12) . . . . ? C39 C40 C41 C42 1.4(2) . . . . ? C40 C39 C44 C43 -0.3(2) . . . . ? C40 C41 C42 C43 -0.5(2) . . . . ? C41 C42 C43 C44 -0.8(2) . . . . ? C42 C43 C44 C39 1.2(2) . . . . ? C44 C39 C40 C41 -1.0(2) . . . . ? C45 C38 C37 C36 178.72(12) . . . . ? C45 C46 C47 C48 1.7(2) . . . . ? C46 C45 C50 C49 1.9(2) . . . . ? C46 C47 C48 C49 0.8(2) . . . . ? C47 C48 C49 C50 -2.0(2) . . . . ? C48 C49 C50 C45 0.6(2) . . . . ? C50 C45 C46 C47 -3.09(19) . . . . ? B1 N2 N1 Fe1 -11.03(13) . . . . ? B1 N2 N1 C6 179.05(11) . . . . ? B1 N2 C8 C7 179.41(12) . . . . ? B1 N2 C8 C15 -3.5(2) . . . . ? B1 N4 N3 Fe1 7.28(13) . . . . ? B1 N4 N3 C21 -170.57(11) . . . . ? B1 N4 C23 C22 169.99(12) . . . . ? B1 N4 C23 C30 -6.6(2) . . . . ? B1 N6 N5 Fe1 -1.85(13) . . . . ? B1 N6 N5 C36 178.98(10) . . . . ? B1 N6 C38 C37 -179.22(11) . . . . ? B1 N6 C38 C45 2.1(2) . . . . ? #===END data_2acacPhmal _audit_creation_date 2012-06-08 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C58 H49 B Fe N6 O4, C2 H3 N' _chemical_formula_sum 'C60 H52 B Fe N7 O4' _chemical_formula_weight 1001.75 _chemical_melting_point ? _chemical_oxdiff_formula 'Fe C58 H49 B N6 O4' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 38.1369(8) _cell_length_b 13.5597(3) _cell_length_c 20.5303(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.121(2) _cell_angle_gamma 90.00 _cell_volume 10295.9(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 25638 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 73.8989 _cell_measurement_theta_min 3.2569 _exptl_absorpt_coefficient_mu 2.789 _exptl_absorpt_correction_T_max 0.858 _exptl_absorpt_correction_T_min 0.456 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 4192 _exptl_crystal_size_max 0.5011 _exptl_crystal_size_mid 0.2887 _exptl_crystal_size_min 0.0559 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_unetI/netI 0.0330 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 72082 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 74.06 _diffrn_reflns_theta_min 3.47 _diffrn_ambient_temperature 100.00(10) _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -28.00 24.00 1.0000 16.0000 omega____ theta____ kappa____ phi______ frames - -40.7737 37.0000 120.0000 52 #__ type_ start__ end____ width___ exp.time_ 2 omega -44.00 29.00 1.0000 16.0000 omega____ theta____ kappa____ phi______ frames - -40.7737 37.0000 0.0000 73 #__ type_ start__ end____ width___ exp.time_ 3 omega -38.00 33.00 1.0000 16.0000 omega____ theta____ kappa____ phi______ frames - -40.7737 37.0000 60.0000 71 #__ type_ start__ end____ width___ exp.time_ 4 omega 62.00 98.00 1.0000 16.0000 omega____ theta____ kappa____ phi______ frames - 40.7737 -125.0000 30.0000 36 #__ type_ start__ end____ width___ exp.time_ 5 omega 73.00 108.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 -30.0000 35 #__ type_ start__ end____ width___ exp.time_ 6 omega 39.00 90.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 60.0000 51 #__ type_ start__ end____ width___ exp.time_ 7 omega 132.00 171.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 125.0000 -120.0000 39 #__ type_ start__ end____ width___ exp.time_ 8 omega 95.00 177.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 125.0000 60.0000 82 #__ type_ start__ end____ width___ exp.time_ 9 omega 54.00 95.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -45.0000 -90.0000 41 #__ type_ start__ end____ width___ exp.time_ 10 omega 32.00 90.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 120.0000 58 #__ type_ start__ end____ width___ exp.time_ 11 omega 140.00 165.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 159.0000 -174.0000 25 #__ type_ start__ end____ width___ exp.time_ 12 omega 37.00 71.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 30.0000 34 #__ type_ start__ end____ width___ exp.time_ 13 omega 29.00 88.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 -180.0000 59 #__ type_ start__ end____ width___ exp.time_ 14 omega 42.00 97.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 -180.0000 55 #__ type_ start__ end____ width___ exp.time_ 15 omega -115.00 -11.00 1.0000 16.0000 omega____ theta____ kappa____ phi______ frames - -40.7737 -57.0000 -30.0000 104 #__ type_ start__ end____ width___ exp.time_ 16 omega -115.00 -11.00 1.0000 16.0000 omega____ theta____ kappa____ phi______ frames - -40.7737 -57.0000 -150.0000 104 #__ type_ start__ end____ width___ exp.time_ 17 omega -117.00 -55.00 1.0000 16.0000 omega____ theta____ kappa____ phi______ frames - -40.7737 -152.0000 79.0000 62 #__ type_ start__ end____ width___ exp.time_ 18 omega -115.00 -11.00 1.0000 16.0000 omega____ theta____ kappa____ phi______ frames - -40.7737 -57.0000 90.0000 104 #__ type_ start__ end____ width___ exp.time_ 19 omega 46.00 119.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 15.0000 120.0000 73 #__ type_ start__ end____ width___ exp.time_ 20 omega 77.00 178.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 30.0000 -150.0000 101 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0080355000 _diffrn_orient_matrix_UB_12 0.1107211000 _diffrn_orient_matrix_UB_13 0.0124392000 _diffrn_orient_matrix_UB_21 -0.0406003000 _diffrn_orient_matrix_UB_22 0.0201670000 _diffrn_orient_matrix_UB_23 -0.0082717000 _diffrn_orient_matrix_UB_31 0.0045779000 _diffrn_orient_matrix_UB_32 -0.0160970000 _diffrn_orient_matrix_UB_33 0.0758807000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_number_gt 18607 _reflns_number_total 20374 _reflns_odcompleteness_completeness 99.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 1.007 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.066 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1321 _refine_ls_number_reflns 20374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0525 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+10.0109P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1393 _refine_ls_wR_factor_ref 0.1430 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.357577(9) 0.69847(3) 0.838682(18) 0.01979(9) Uani 1 1 d . . . O1 O 0.39571(4) 0.59947(12) 0.83796(9) 0.0272(4) Uani 1 1 d . . . O2 O 0.38239(4) 0.78440(11) 0.77996(8) 0.0232(3) Uani 1 1 d . . . O3 O 0.44402(4) 0.52365(12) 0.81676(9) 0.0303(4) Uani 1 1 d . . . O4 O 0.42818(4) 0.84677(12) 0.74255(9) 0.0297(4) Uani 1 1 d . . . N1 N 0.33397(5) 0.62436(14) 0.91414(9) 0.0217(4) Uani 1 1 d . . . N2 N 0.29967(5) 0.65437(14) 0.91433(9) 0.0203(4) Uani 1 1 d . . . N3 N 0.34224(5) 0.82647(14) 0.88279(9) 0.0202(4) Uani 1 1 d . . . N4 N 0.30636(5) 0.83038(13) 0.88262(9) 0.0189(4) Uani 1 1 d . . . N5 N 0.30793(5) 0.69074(13) 0.76924(10) 0.0199(4) Uani 1 1 d . . . N6 N 0.27742(5) 0.70375(13) 0.79237(10) 0.0194(4) Uani 1 1 d . . . C1 C 0.29963(6) 0.91683(16) 0.91109(11) 0.0196(4) Uani 1 1 d . . . C2 C 0.33175(6) 0.96851(16) 0.92959(12) 0.0222(4) Uani 1 1 d . . . H2 H 0.3354 1.0313 0.9507 0.027 Uiso 1 1 calc R . . C3 C 0.35776(6) 0.90933(17) 0.91093(11) 0.0214(4) Uani 1 1 d . . . C4 C 0.28711(6) 0.60193(16) 0.96044(11) 0.0222(4) Uani 1 1 d . . . C5 C 0.31376(7) 0.53545(17) 0.99001(12) 0.0266(5) Uani 1 1 d . . . H5 H 0.3126 0.4876 1.0232 0.032 Uiso 1 1 calc R . . C6 C 0.34274(6) 0.55332(18) 0.96086(12) 0.0259(5) Uani 1 1 d . . . C7 C 0.24766(6) 0.69732(15) 0.74018(11) 0.0203(4) Uani 1 1 d . . . C8 C 0.25937(6) 0.68218(16) 0.68236(12) 0.0226(4) Uani 1 1 d . . . H8 H 0.2447 0.6759 0.6379 0.027 Uiso 1 1 calc R . . C9 C 0.29702(6) 0.67789(16) 0.70241(11) 0.0213(4) Uani 1 1 d . . . C10 C 0.26371(6) 0.94676(16) 0.91853(12) 0.0211(4) Uani 1 1 d . . . C11 C 0.25955(6) 0.97514(16) 0.98135(12) 0.0250(5) Uani 1 1 d . . . H11 H 0.2796 0.9729 1.0193 0.030 Uiso 1 1 calc R . . C12 C 0.22596(7) 1.00687(18) 0.98881(14) 0.0305(5) Uani 1 1 d . . . H12 H 0.2233 1.0266 1.0317 0.037 Uiso 1 1 calc R . . C13 C 0.19648(7) 1.0097(2) 0.93369(15) 0.0351(6) Uani 1 1 d . . . H13 H 0.1736 1.0316 0.9387 0.042 Uiso 1 1 calc R . . C14 C 0.20060(7) 0.9805(2) 0.87141(14) 0.0344(6) Uani 1 1 d . . . H14 H 0.1804 0.9818 0.8338 0.041 Uiso 1 1 calc R . . C15 C 0.23393(6) 0.94933(18) 0.86316(12) 0.0267(5) Uani 1 1 d . . . H15 H 0.2365 0.9298 0.8201 0.032 Uiso 1 1 calc R . . C16 C 0.39625(6) 0.93202(19) 0.91828(11) 0.0263(5) Uani 1 1 d . . . C17 C 0.40767(7) 1.0301(2) 0.92210(14) 0.0357(6) Uani 1 1 d . . . H17 H 0.3906 1.0814 0.9209 0.043 Uiso 1 1 calc R . . C18 C 0.44368(8) 1.0535(3) 0.92767(16) 0.0474(8) Uani 1 1 d . . . H18 H 0.4512 1.1205 0.9310 0.057 Uiso 1 1 calc R . . C19 C 0.46867(7) 0.9797(3) 0.92841(15) 0.0466(8) Uani 1 1 d . . . H19 H 0.4932 0.9959 0.9307 0.056 Uiso 1 1 calc R . . C20 C 0.45803(7) 0.8824(3) 0.92583(14) 0.0426(7) Uani 1 1 d . . . H20 H 0.4753 0.8314 0.9271 0.051 Uiso 1 1 calc R . . C21 C 0.42203(6) 0.8587(2) 0.92133(13) 0.0318(5) Uani 1 1 d . . . H21 H 0.4150 0.7914 0.9203 0.038 Uiso 1 1 calc R . . C22 C 0.25150(6) 0.61801(16) 0.97551(11) 0.0221(4) Uani 1 1 d . . . C23 C 0.22974(6) 0.53659(17) 0.98021(12) 0.0250(5) Uani 1 1 d . . . H23 H 0.2378 0.4721 0.9729 0.030 Uiso 1 1 calc R . . C24 C 0.19639(6) 0.54929(18) 0.99549(12) 0.0274(5) Uani 1 1 d . . . H24 H 0.1817 0.4937 0.9987 0.033 Uiso 1 1 calc R . . C25 C 0.18461(6) 0.64355(19) 1.00609(12) 0.0283(5) Uani 1 1 d . . . H25 H 0.1618 0.6525 1.0161 0.034 Uiso 1 1 calc R . . C26 C 0.20623(7) 0.72485(18) 1.00212(12) 0.0269(5) Uani 1 1 d . . . H26 H 0.1982 0.7892 1.0096 0.032 Uiso 1 1 calc R . . C27 C 0.23951(6) 0.71209(17) 0.98730(12) 0.0237(5) Uani 1 1 d . . . H27 H 0.2543 0.7678 0.9852 0.028 Uiso 1 1 calc R . . C28 C 0.37943(8) 0.5104(2) 0.98102(14) 0.0384(6) Uani 1 1 d . . . C29 C 0.38398(10) 0.4103(3) 0.99456(17) 0.0582(10) Uani 1 1 d . . . H29 H 0.3635 0.3680 0.9878 0.070 Uiso 1 1 calc R . . C30 C 0.41891(14) 0.3719(4) 1.0183(2) 0.0921(19) Uani 1 1 d . . . H30 H 0.4221 0.3035 1.0279 0.111 Uiso 1 1 calc R . . C31 C 0.44825(12) 0.4322(5) 1.0276(2) 0.103(2) Uani 1 1 d . . . H31 H 0.4718 0.4051 1.0422 0.124 Uiso 1 1 calc R . . C32 C 0.44405(9) 0.5327(4) 1.01581(19) 0.0812(16) Uani 1 1 d . . . H32 H 0.4646 0.5745 1.0236 0.097 Uiso 1 1 calc R . . C33 C 0.40964(8) 0.5718(3) 0.99267(15) 0.0517(9) Uani 1 1 d . . . H33 H 0.4067 0.6406 0.9847 0.062 Uiso 1 1 calc R . . C34 C 0.21023(6) 0.69688(15) 0.74764(12) 0.0214(4) Uani 1 1 d . . . C35 C 0.18251(7) 0.73426(18) 0.69587(14) 0.0295(5) Uani 1 1 d . . . H35 H 0.1882 0.7655 0.6583 0.035 Uiso 1 1 calc R . . C36 C 0.14659(7) 0.7258(2) 0.69908(16) 0.0405(7) Uani 1 1 d . . . H36 H 0.1279 0.7492 0.6629 0.049 Uiso 1 1 calc R . . C37 C 0.13799(7) 0.6835(2) 0.75481(16) 0.0403(7) Uani 1 1 d . . . H37 H 0.1135 0.6796 0.7575 0.048 Uiso 1 1 calc R . . C38 C 0.16538(7) 0.64711(19) 0.80651(14) 0.0314(5) Uani 1 1 d . . . H38 H 0.1597 0.6186 0.8449 0.038 Uiso 1 1 calc R . . C39 C 0.20103(6) 0.65212(17) 0.80240(12) 0.0250(5) Uani 1 1 d . . . H39 H 0.2195 0.6247 0.8374 0.030 Uiso 1 1 calc R . . C40 C 0.32327(6) 0.66196(16) 0.66122(11) 0.0220(4) Uani 1 1 d . . . C41 C 0.32133(7) 0.71771(19) 0.60358(12) 0.0278(5) Uani 1 1 d . . . H41 H 0.3029 0.7661 0.5907 0.033 Uiso 1 1 calc R . . C42 C 0.34598(7) 0.7035(2) 0.56471(13) 0.0336(6) Uani 1 1 d . . . H42 H 0.3444 0.7419 0.5254 0.040 Uiso 1 1 calc R . . C43 C 0.37301(7) 0.6332(2) 0.58318(13) 0.0330(6) Uani 1 1 d . . . H43 H 0.3899 0.6234 0.5566 0.040 Uiso 1 1 calc R . . C44 C 0.37522(7) 0.5773(2) 0.64036(13) 0.0318(5) Uani 1 1 d . . . H44 H 0.3937 0.5290 0.6531 0.038 Uiso 1 1 calc R . . C45 C 0.35051(7) 0.59145(18) 0.67919(12) 0.0271(5) Uani 1 1 d . . . H45 H 0.3522 0.5527 0.7184 0.033 Uiso 1 1 calc R . . C46 C 0.42307(6) 0.60508(17) 0.81305(12) 0.0245(5) Uani 1 1 d . . . C47 C 0.43459(6) 0.68568(17) 0.78151(12) 0.0231(5) Uani 1 1 d . . . C48 C 0.41280(6) 0.77196(17) 0.76892(12) 0.0227(5) Uani 1 1 d . . . C49 C 0.43331(7) 0.43614(19) 0.84708(15) 0.0378(6) Uani 1 1 d . . . H49A H 0.4233 0.4553 0.8854 0.045 Uiso 1 1 calc R . . H49B H 0.4548 0.3942 0.8645 0.045 Uiso 1 1 calc R . . C50 C 0.40547(8) 0.3782(2) 0.7974(2) 0.0527(9) Uani 1 1 d . . . H50A H 0.3994 0.3182 0.8190 0.079 Uiso 1 1 calc R . . H50B H 0.4152 0.3602 0.7590 0.079 Uiso 1 1 calc R . . H50C H 0.3837 0.4184 0.7819 0.079 Uiso 1 1 calc R . . C51 C 0.46874(6) 0.68124(17) 0.75847(13) 0.0252(5) Uani 1 1 d . . . C52 C 0.50196(6) 0.66483(18) 0.80409(14) 0.0302(5) Uani 1 1 d . . . H52 H 0.5027 0.6561 0.8503 0.036 Uiso 1 1 calc R . . C53 C 0.53395(7) 0.66109(19) 0.78282(16) 0.0364(6) Uani 1 1 d . . . H53 H 0.5563 0.6496 0.8145 0.044 Uiso 1 1 calc R . . C54 C 0.53331(7) 0.6739(2) 0.71609(17) 0.0390(7) Uani 1 1 d . . . H54 H 0.5551 0.6710 0.7016 0.047 Uiso 1 1 calc R . . C55 C 0.50068(8) 0.6912(2) 0.67013(16) 0.0374(6) Uani 1 1 d . . . H55 H 0.5002 0.7009 0.6241 0.045 Uiso 1 1 calc R . . C56 C 0.46865(7) 0.69447(18) 0.69126(14) 0.0297(5) Uani 1 1 d . . . H56 H 0.4464 0.7059 0.6593 0.036 Uiso 1 1 calc R . . C57 C 0.40800(7) 0.93757(18) 0.72805(15) 0.0341(6) Uani 1 1 d . . . H57A H 0.4250 0.9940 0.7338 0.041 Uiso 1 1 calc R . . H57B H 0.3925 0.9459 0.7600 0.041 Uiso 1 1 calc R . . C58 C 0.38547(12) 0.9368(3) 0.65954(18) 0.0656(11) Uani 1 1 d . . . H58A H 0.3676 0.8836 0.6547 0.098 Uiso 1 1 calc R . . H58B H 0.4007 0.9261 0.6280 0.098 Uiso 1 1 calc R . . H58C H 0.3730 1.0002 0.6498 0.098 Uiso 1 1 calc R . . B1 B 0.28163(6) 0.73773(18) 0.86585(13) 0.0195(5) Uani 1 1 d . . . H1 H 0.2573 0.7530 0.8734 0.023 Uiso 1 1 calc R . . Fe1A Fe 0.138110(9) 0.22979(3) 0.488215(18) 0.02150(9) Uani 1 1 d . . . O1A O 0.11703(4) 0.32187(12) 0.40894(8) 0.0257(3) Uani 1 1 d . . . O2A O 0.09919(4) 0.13553(12) 0.44514(8) 0.0261(3) Uani 1 1 d . . . O3A O 0.07728(5) 0.38727(14) 0.32094(10) 0.0380(4) Uani 1 1 d . . . O4A O 0.05227(4) 0.06711(12) 0.37125(9) 0.0289(4) Uani 1 1 d . . . N1A N 0.15913(5) 0.34421(14) 0.55632(10) 0.0228(4) Uani 1 1 d . . . N2A N 0.19285(5) 0.32774(13) 0.59763(9) 0.0202(4) Uani 1 1 d . . . N3A N 0.15510(5) 0.13351(13) 0.57714(9) 0.0193(4) Uani 1 1 d . . . N4A N 0.19116(5) 0.14237(13) 0.60825(9) 0.0190(4) Uani 1 1 d . . . N5A N 0.18931(5) 0.21007(13) 0.46841(9) 0.0192(4) Uani 1 1 d . . . N6A N 0.21925(5) 0.21902(13) 0.52095(9) 0.0189(4) Uani 1 1 d . . . C1A C 0.20216(6) 0.40449(16) 0.64112(12) 0.0229(4) Uani 1 1 d . . . C2A C 0.17389(7) 0.47168(17) 0.62679(13) 0.0296(5) Uani 1 1 d . . . H2A H 0.1726 0.5328 0.6488 0.035 Uiso 1 1 calc R . . C3A C 0.14775(7) 0.43175(18) 0.57374(13) 0.0279(5) Uani 1 1 d . . . C4A C 0.20185(6) 0.06674(16) 0.65161(11) 0.0205(4) Uani 1 1 d . . . C5A C 0.17200(6) 0.00751(16) 0.64952(12) 0.0222(4) Uani 1 1 d . . . H5A H 0.1711 -0.0511 0.6744 0.027 Uiso 1 1 calc R . . C6A C 0.14346(6) 0.05213(16) 0.60308(11) 0.0206(4) Uani 1 1 d . . . C7A C 0.24917(6) 0.23119(15) 0.49683(12) 0.0207(4) Uani 1 1 d . . . C8A C 0.23812(6) 0.23095(16) 0.42736(12) 0.0226(4) Uani 1 1 d . . . H8A H 0.2529 0.2390 0.3966 0.027 Uiso 1 1 calc R . . C9A C 0.20075(6) 0.21642(16) 0.41175(12) 0.0218(4) Uani 1 1 d . . . C10A C 0.23627(6) 0.40926(16) 0.69338(12) 0.0248(5) Uani 1 1 d . . . C11A C 0.23489(7) 0.43111(17) 0.75921(13) 0.0293(5) Uani 1 1 d . . . H11A H 0.2122 0.4417 0.7696 0.035 Uiso 1 1 calc R . . C12A C 0.26659(8) 0.4373(2) 0.80939(14) 0.0382(6) Uani 1 1 d . . . H12A H 0.2656 0.4531 0.8540 0.046 Uiso 1 1 calc R . . C13A C 0.29982(8) 0.4205(2) 0.79503(15) 0.0395(6) Uani 1 1 d . . . H13A H 0.3214 0.4239 0.8297 0.047 Uiso 1 1 calc R . . C14A C 0.30129(7) 0.3989(2) 0.73009(15) 0.0362(6) Uani 1 1 d . . . H14A H 0.3240 0.3866 0.7202 0.043 Uiso 1 1 calc R . . C15A C 0.26989(7) 0.39506(18) 0.67918(13) 0.0282(5) Uani 1 1 d . . . H15A H 0.2712 0.3827 0.6343 0.034 Uiso 1 1 calc R . . C16A C 0.11194(7) 0.4714(2) 0.53813(14) 0.0349(6) Uani 1 1 d . . . C17A C 0.10797(9) 0.5723(2) 0.52571(17) 0.0469(7) Uani 1 1 d . . . H17A H 0.1281 0.6150 0.5402 0.056 Uiso 1 1 calc R . . C18A C 0.07448(11) 0.6110(3) 0.49206(19) 0.0610(10) Uani 1 1 d . . . H18A H 0.0719 0.6799 0.4842 0.073 Uiso 1 1 calc R . . C19A C 0.04514(10) 0.5495(3) 0.4703(2) 0.0645(10) Uani 1 1 d . . . H19A H 0.0226 0.5761 0.4467 0.077 Uiso 1 1 calc R . . C20A C 0.04844(9) 0.4489(3) 0.48259(18) 0.0540(8) Uani 1 1 d . . . H20A H 0.0282 0.4067 0.4679 0.065 Uiso 1 1 calc R . . C21A C 0.08165(7) 0.4103(2) 0.51662(15) 0.0410(6) Uani 1 1 d . . . H21A H 0.0839 0.3415 0.5254 0.049 Uiso 1 1 calc R . . C22A C 0.23943(6) 0.05214(17) 0.69118(12) 0.0223(4) Uani 1 1 d . . . C23A C 0.25701(6) -0.03574(17) 0.68257(13) 0.0268(5) Uani 1 1 d . . . H23A H 0.2447 -0.0846 0.6523 0.032 Uiso 1 1 calc R . . C24A C 0.29263(7) -0.05151(19) 0.71847(14) 0.0324(6) Uani 1 1 d . . . H24A H 0.3046 -0.1110 0.7125 0.039 Uiso 1 1 calc R . . C25A C 0.31049(7) 0.0189(2) 0.76257(13) 0.0336(6) Uani 1 1 d . . . H25A H 0.3348 0.0080 0.7865 0.040 Uiso 1 1 calc R . . C26A C 0.29313(7) 0.1059(2) 0.77225(13) 0.0307(5) Uani 1 1 d . . . H26A H 0.3055 0.1540 0.8031 0.037 Uiso 1 1 calc R . . C27A C 0.25767(6) 0.12235(18) 0.73677(12) 0.0257(5) Uani 1 1 d . . . H27A H 0.2458 0.1816 0.7435 0.031 Uiso 1 1 calc R . . C28A C 0.10523(6) 0.02159(17) 0.58867(12) 0.0234(5) Uani 1 1 d . . . C29A C 0.09653(6) -0.07840(18) 0.58594(12) 0.0272(5) Uani 1 1 d . . . H29A H 0.1151 -0.1260 0.5886 0.033 Uiso 1 1 calc R . . C30A C 0.06104(7) -0.10963(19) 0.57936(13) 0.0322(5) Uani 1 1 d . . . H30A H 0.0556 -0.1781 0.5782 0.039 Uiso 1 1 calc R . . C31A C 0.03389(7) -0.0413(2) 0.57448(14) 0.0353(6) Uani 1 1 d . . . H31A H 0.0097 -0.0625 0.5702 0.042 Uiso 1 1 calc R . . C32A C 0.04197(7) 0.0593(2) 0.57577(14) 0.0345(6) Uani 1 1 d . . . H32A H 0.0232 0.1065 0.5716 0.041 Uiso 1 1 calc R . . C33A C 0.07726(6) 0.09016(19) 0.58314(13) 0.0282(5) Uani 1 1 d . . . H33A H 0.0826 0.1587 0.5845 0.034 Uiso 1 1 calc R . . C34A C 0.28640(6) 0.23926(16) 0.53900(12) 0.0209(4) Uani 1 1 d . . . C35A C 0.30982(6) 0.30663(17) 0.52013(13) 0.0248(5) Uani 1 1 d . . . H35A H 0.3015 0.3458 0.4810 0.030 Uiso 1 1 calc R . . C36A C 0.34528(6) 0.31698(19) 0.55809(14) 0.0307(5) Uani 1 1 d . . . H36A H 0.3609 0.3633 0.5450 0.037 Uiso 1 1 calc R . . C37A C 0.35771(6) 0.25984(19) 0.61491(13) 0.0297(5) Uani 1 1 d . . . H37A H 0.3818 0.2671 0.6410 0.036 Uiso 1 1 calc R . . C38A C 0.33484(6) 0.19197(18) 0.63368(13) 0.0273(5) Uani 1 1 d . . . H38A H 0.3433 0.1529 0.6728 0.033 Uiso 1 1 calc R . . C39A C 0.29945(6) 0.18072(17) 0.59551(12) 0.0235(5) Uani 1 1 d . . . H39A H 0.2841 0.1329 0.6081 0.028 Uiso 1 1 calc R . . C40A C 0.17547(6) 0.20280(16) 0.34558(11) 0.0215(4) Uani 1 1 d . . . C41A C 0.17581(7) 0.26653(18) 0.29248(12) 0.0263(5) Uani 1 1 d . . . H41A H 0.1921 0.3206 0.2989 0.032 Uiso 1 1 calc R . . C42A C 0.15230(7) 0.2509(2) 0.23023(13) 0.0312(5) Uani 1 1 d . . . H42A H 0.1525 0.2949 0.1943 0.037 Uiso 1 1 calc R . . C43A C 0.12871(7) 0.1723(2) 0.21996(13) 0.0316(5) Uani 1 1 d . . . H43A H 0.1129 0.1619 0.1770 0.038 Uiso 1 1 calc R . . C44A C 0.12812(7) 0.10834(19) 0.27238(13) 0.0309(5) Uani 1 1 d . . . H44A H 0.1117 0.0544 0.2656 0.037 Uiso 1 1 calc R . . C45A C 0.15151(6) 0.12354(18) 0.33466(12) 0.0268(5) Uani 1 1 d . . . H45A H 0.1512 0.0793 0.3704 0.032 Uiso 1 1 calc R . . C46A C 0.07372(6) 0.14617(17) 0.39239(12) 0.0240(5) Uani 1 1 d . . . C47A C 0.06502(6) 0.22977(17) 0.35234(13) 0.0258(5) Uani 1 1 d . . . C48A C 0.08823(6) 0.31261(18) 0.36415(12) 0.0258(5) Uani 1 1 d . . . C49A C 0.06004(6) -0.02337(17) 0.40925(13) 0.0274(5) Uani 1 1 d . . . H49C H 0.0382 -0.0657 0.3992 0.033 Uiso 1 1 calc R . . H49D H 0.0659 -0.0078 0.4578 0.033 Uiso 1 1 calc R . . C50A C 0.09093(7) -0.0787(2) 0.39332(16) 0.0371(6) Uani 1 1 d . . . H50D H 0.0936 -0.1426 0.4163 0.056 Uiso 1 1 calc R . . H50E H 0.1132 -0.0405 0.4085 0.056 Uiso 1 1 calc R . . H50F H 0.0861 -0.0892 0.3447 0.056 Uiso 1 1 calc R . . C51A C 0.03217(7) 0.22953(17) 0.29481(14) 0.0294(5) Uani 1 1 d . . . C52A C -0.00196(7) 0.2191(2) 0.30703(18) 0.0424(7) Uani 1 1 d . . . H52A H -0.0043 0.2136 0.3519 0.051 Uiso 1 1 calc R . . C53A C -0.03291(8) 0.2167(2) 0.2539(2) 0.0572(10) Uani 1 1 d . . . H53A H -0.0561 0.2097 0.2628 0.069 Uiso 1 1 calc R . . C54A C -0.02985(9) 0.2245(2) 0.1884(2) 0.0571(10) Uani 1 1 d . . . H54A H -0.0508 0.2223 0.1522 0.069 Uiso 1 1 calc R . . C55A C 0.00379(9) 0.2356(2) 0.17576(17) 0.0487(8) Uani 1 1 d . . . H55A H 0.0059 0.2415 0.1308 0.058 Uiso 1 1 calc R . . C56A C 0.03470(8) 0.2383(2) 0.22865(14) 0.0369(6) Uani 1 1 d . . . H56A H 0.0578 0.2461 0.2194 0.044 Uiso 1 1 calc R . . C57A C 0.09982(10) 0.4741(3) 0.32698(17) 0.0583(10) Uani 1 1 d . . . H57C H 0.0910 0.5247 0.3539 0.070 Uiso 1 1 calc R . . H57D H 0.1250 0.4570 0.3503 0.070 Uiso 1 1 calc R . . C58A C 0.09891(10) 0.5129(2) 0.26107(17) 0.0492(8) Uani 1 1 d . . . H58D H 0.1130 0.5741 0.2655 0.074 Uiso 1 1 calc R . . H58E H 0.0738 0.5264 0.2372 0.074 Uiso 1 1 calc R . . H58F H 0.1093 0.4645 0.2357 0.074 Uiso 1 1 calc R . . B1A B 0.21353(7) 0.23049(17) 0.59235(13) 0.0191(5) Uani 1 1 d . . . H1A H 0.2376 0.2319 0.6256 0.023 Uiso 1 1 calc R . . N1S N 0.43875(7) 0.3770(2) 0.59861(16) 0.0546(7) Uani 1 1 d . . . C1S C 0.45976(7) 0.39806(19) 0.64638(16) 0.0353(6) Uani 1 1 d . . . C2S C 0.48667(7) 0.4240(2) 0.70693(15) 0.0350(6) Uani 1 1 d . . . H2SA H 0.4928 0.3656 0.7356 0.053 Uiso 1 1 calc R . . H2SB H 0.4770 0.4755 0.7312 0.053 Uiso 1 1 calc R . . H2SC H 0.5084 0.4486 0.6949 0.053 Uiso 1 1 calc R . . N2S N 0.05719(14) 0.5634(7) 0.6583(3) 0.175(4) Uani 1 1 d . . . C3S C 0.03573(13) 0.5446(4) 0.6855(3) 0.0918(17) Uani 1 1 d . . . C4S C 0.00819(11) 0.5246(3) 0.7193(2) 0.0665(11) Uani 1 1 d . . . H4SA H 0.0153 0.4682 0.7494 0.100 Uiso 1 1 calc R . . H4SB H -0.0144 0.5093 0.6862 0.100 Uiso 1 1 calc R . . H4SC H 0.0046 0.5825 0.7455 0.100 Uiso 1 1 calc R . . 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 0.01746(17) 0.02065(17) 0.02320(18) 0.00023(14) 0.00870(14) 0.00255(13) O1 0.0255(8) 0.0277(8) 0.0325(9) 0.0075(7) 0.0152(7) 0.0076(7) O2 0.0196(7) 0.0233(7) 0.0292(8) 0.0036(7) 0.0106(6) 0.0031(6) O3 0.0267(8) 0.0260(8) 0.0423(10) 0.0072(8) 0.0164(8) 0.0083(7) O4 0.0253(8) 0.0235(8) 0.0452(10) 0.0069(7) 0.0177(8) 0.0024(7) N1 0.0207(9) 0.0242(9) 0.0220(9) 0.0038(8) 0.0089(7) 0.0030(7) N2 0.0184(8) 0.0211(9) 0.0231(9) 0.0000(7) 0.0083(7) -0.0003(7) N3 0.0159(8) 0.0234(9) 0.0227(9) -0.0014(8) 0.0073(7) 0.0000(7) N4 0.0160(8) 0.0193(8) 0.0230(9) -0.0002(7) 0.0079(7) 0.0013(7) N5 0.0187(9) 0.0195(9) 0.0243(9) 0.0003(7) 0.0108(7) 0.0010(7) N6 0.0165(8) 0.0187(8) 0.0250(10) 0.0001(7) 0.0090(7) 0.0000(7) C1 0.0200(10) 0.0202(10) 0.0204(10) 0.0004(8) 0.0084(8) 0.0015(8) C2 0.0229(11) 0.0199(10) 0.0251(11) -0.0031(9) 0.0084(9) -0.0025(8) C3 0.0202(10) 0.0246(11) 0.0208(10) -0.0007(9) 0.0076(8) -0.0013(8) C4 0.0241(11) 0.0207(10) 0.0236(11) -0.0016(9) 0.0098(9) -0.0026(8) C5 0.0317(12) 0.0241(11) 0.0260(12) 0.0055(9) 0.0114(10) 0.0023(9) C6 0.0284(12) 0.0271(11) 0.0244(11) 0.0035(9) 0.0106(9) 0.0048(9) C7 0.0195(10) 0.0164(10) 0.0249(11) 0.0003(8) 0.0055(9) 0.0004(8) C8 0.0245(11) 0.0209(10) 0.0229(11) 0.0001(9) 0.0066(9) -0.0010(9) C9 0.0243(11) 0.0174(10) 0.0239(11) -0.0014(9) 0.0088(9) -0.0016(8) C10 0.0209(10) 0.0171(10) 0.0266(11) -0.0001(9) 0.0084(9) 0.0004(8) C11 0.0238(11) 0.0213(10) 0.0310(12) -0.0034(9) 0.0092(9) -0.0015(9) C12 0.0296(12) 0.0274(12) 0.0380(14) -0.0084(11) 0.0151(11) 0.0002(10) C13 0.0232(12) 0.0355(13) 0.0492(16) -0.0048(12) 0.0141(11) 0.0058(10) C14 0.0239(12) 0.0381(14) 0.0393(15) -0.0001(12) 0.0038(11) 0.0068(10) C15 0.0253(11) 0.0288(12) 0.0263(12) 0.0002(10) 0.0064(9) 0.0031(9) C16 0.0220(11) 0.0382(13) 0.0200(11) -0.0049(10) 0.0075(9) -0.0066(10) C17 0.0318(13) 0.0415(15) 0.0378(14) -0.0090(12) 0.0160(11) -0.0124(11) C18 0.0387(16) 0.0602(19) 0.0487(17) -0.0181(15) 0.0214(14) -0.0277(14) C19 0.0246(13) 0.080(2) 0.0376(15) -0.0163(15) 0.0124(12) -0.0196(14) C20 0.0233(12) 0.070(2) 0.0349(15) -0.0065(14) 0.0077(11) 0.0012(13) C21 0.0222(11) 0.0435(14) 0.0289(13) -0.0042(11) 0.0048(10) -0.0006(10) C22 0.0246(11) 0.0223(10) 0.0211(11) -0.0012(9) 0.0087(9) -0.0035(9) C23 0.0287(12) 0.0227(11) 0.0248(11) 0.0021(9) 0.0088(9) -0.0031(9) C24 0.0267(12) 0.0288(12) 0.0276(12) 0.0021(10) 0.0087(10) -0.0086(10) C25 0.0224(11) 0.0366(13) 0.0284(12) 0.0014(10) 0.0109(9) -0.0020(10) C26 0.0289(12) 0.0274(12) 0.0264(12) -0.0012(10) 0.0102(10) 0.0007(9) C27 0.0278(12) 0.0222(11) 0.0231(11) -0.0008(9) 0.0099(9) -0.0038(9) C28 0.0359(14) 0.0542(17) 0.0291(13) 0.0177(12) 0.0159(11) 0.0191(13) C29 0.069(2) 0.064(2) 0.0536(19) 0.0350(17) 0.0374(18) 0.0405(18) C30 0.103(4) 0.115(4) 0.079(3) 0.071(3) 0.062(3) 0.083(3) C31 0.058(3) 0.192(6) 0.069(3) 0.077(4) 0.035(2) 0.074(3) C32 0.0326(17) 0.163(5) 0.049(2) 0.042(3) 0.0115(15) 0.028(2) C33 0.0270(14) 0.093(3) 0.0355(15) 0.0204(17) 0.0088(12) 0.0119(15) C34 0.0211(11) 0.0165(10) 0.0273(12) -0.0015(9) 0.0069(9) -0.0006(8) C35 0.0246(12) 0.0275(12) 0.0366(14) 0.0096(10) 0.0079(10) 0.0053(9) C36 0.0250(13) 0.0418(15) 0.0526(18) 0.0186(13) 0.0055(12) 0.0093(11) C37 0.0222(12) 0.0426(15) 0.0586(18) 0.0154(14) 0.0149(12) 0.0059(11) C38 0.0255(12) 0.0323(13) 0.0382(14) 0.0041(11) 0.0112(10) -0.0039(10) C39 0.0229(11) 0.0226(11) 0.0291(12) 0.0006(9) 0.0058(9) -0.0030(9) C40 0.0226(10) 0.0224(10) 0.0220(11) -0.0046(9) 0.0070(9) -0.0037(8) C41 0.0266(12) 0.0348(12) 0.0220(11) -0.0003(10) 0.0059(9) 0.0003(10) C42 0.0310(13) 0.0490(15) 0.0232(12) 0.0019(11) 0.0108(10) -0.0035(11) C43 0.0261(12) 0.0497(16) 0.0258(12) -0.0107(11) 0.0114(10) -0.0043(11) C44 0.0280(12) 0.0383(14) 0.0307(13) -0.0080(11) 0.0101(10) 0.0048(10) C45 0.0300(12) 0.0263(11) 0.0265(12) -0.0015(10) 0.0098(10) 0.0022(9) C46 0.0217(11) 0.0263(11) 0.0268(12) 0.0023(9) 0.0085(9) 0.0065(9) C47 0.0206(11) 0.0237(11) 0.0265(11) 0.0009(9) 0.0086(9) 0.0028(9) C48 0.0209(11) 0.0239(11) 0.0253(11) -0.0011(9) 0.0093(9) -0.0018(8) C49 0.0378(14) 0.0294(13) 0.0520(17) 0.0185(12) 0.0222(13) 0.0136(11) C50 0.0340(15) 0.0289(14) 0.096(3) 0.0112(16) 0.0176(16) 0.0037(12) C51 0.0205(11) 0.0222(11) 0.0350(13) -0.0030(10) 0.0107(10) 0.0002(9) C52 0.0231(11) 0.0282(12) 0.0391(14) -0.0042(11) 0.0070(10) 0.0016(9) C53 0.0198(11) 0.0286(12) 0.0608(18) -0.0081(12) 0.0096(12) 0.0012(10) C54 0.0262(13) 0.0296(13) 0.069(2) -0.0055(13) 0.0271(13) -0.0015(10) C55 0.0383(15) 0.0339(13) 0.0489(17) 0.0007(12) 0.0275(13) 0.0020(11) C56 0.0261(12) 0.0285(12) 0.0372(14) -0.0002(10) 0.0132(11) 0.0015(9) C57 0.0343(13) 0.0235(12) 0.0499(16) 0.0068(11) 0.0210(12) 0.0044(10) C58 0.088(3) 0.052(2) 0.049(2) 0.0029(16) 0.0036(19) 0.031(2) B1 0.0168(11) 0.0206(11) 0.0233(12) -0.0006(10) 0.0092(9) -0.0006(9) Fe1A 0.01710(17) 0.02313(18) 0.02392(19) 0.00389(14) 0.00432(14) -0.00205(13) O1A 0.0224(8) 0.0265(8) 0.0264(8) 0.0042(7) 0.0024(7) -0.0024(6) O2A 0.0259(8) 0.0260(8) 0.0252(8) 0.0028(7) 0.0041(7) -0.0041(7) O3A 0.0365(10) 0.0296(9) 0.0390(10) 0.0130(8) -0.0078(8) -0.0116(8) O4A 0.0261(8) 0.0223(8) 0.0354(9) 0.0018(7) 0.0021(7) -0.0043(7) N1A 0.0213(9) 0.0233(9) 0.0247(10) 0.0042(8) 0.0073(8) 0.0065(7) N2A 0.0199(9) 0.0185(8) 0.0228(9) 0.0015(7) 0.0065(7) 0.0014(7) N3A 0.0147(8) 0.0207(9) 0.0231(9) 0.0018(7) 0.0057(7) 0.0005(7) N4A 0.0153(8) 0.0196(9) 0.0229(9) 0.0020(7) 0.0060(7) 0.0002(7) N5A 0.0171(8) 0.0208(8) 0.0199(9) 0.0004(7) 0.0049(7) -0.0019(7) N6A 0.0168(8) 0.0186(8) 0.0216(9) -0.0004(7) 0.0053(7) -0.0018(7) C1A 0.0287(11) 0.0192(10) 0.0244(11) 0.0001(9) 0.0135(9) -0.0015(9) C2A 0.0389(13) 0.0191(11) 0.0360(13) 0.0020(10) 0.0193(11) 0.0054(10) C3A 0.0306(12) 0.0260(11) 0.0307(12) 0.0051(10) 0.0145(10) 0.0058(10) C4A 0.0196(10) 0.0204(10) 0.0231(11) 0.0012(9) 0.0081(9) 0.0015(8) C5A 0.0228(11) 0.0195(10) 0.0267(11) 0.0033(9) 0.0105(9) 0.0001(8) C6A 0.0214(10) 0.0196(10) 0.0227(11) 0.0009(8) 0.0090(9) -0.0001(8) C7A 0.0197(10) 0.0159(10) 0.0284(12) 0.0008(9) 0.0095(9) -0.0011(8) C8A 0.0239(11) 0.0225(11) 0.0244(11) 0.0015(9) 0.0116(9) -0.0018(9) C9A 0.0254(11) 0.0184(10) 0.0227(11) 0.0015(8) 0.0081(9) -0.0018(8) C10A 0.0311(12) 0.0157(10) 0.0295(12) -0.0035(9) 0.0110(10) -0.0048(9) C11A 0.0379(13) 0.0234(11) 0.0295(12) -0.0046(10) 0.0138(11) -0.0053(10) C12A 0.0546(17) 0.0303(13) 0.0309(14) -0.0067(11) 0.0128(12) -0.0072(12) C13A 0.0406(15) 0.0341(14) 0.0390(15) -0.0080(12) 0.0005(12) -0.0098(12) C14A 0.0285(13) 0.0324(13) 0.0485(16) -0.0101(12) 0.0106(12) -0.0067(10) C15A 0.0300(12) 0.0246(11) 0.0323(13) -0.0065(10) 0.0118(10) -0.0058(9) C16A 0.0350(14) 0.0373(14) 0.0350(14) 0.0065(11) 0.0134(11) 0.0150(11) C17A 0.0521(18) 0.0387(16) 0.0494(18) 0.0054(14) 0.0111(15) 0.0151(14) C18A 0.065(2) 0.053(2) 0.059(2) 0.0150(17) 0.0039(18) 0.0285(18) C19A 0.051(2) 0.078(3) 0.062(2) 0.015(2) 0.0090(17) 0.033(2) C20A 0.0353(16) 0.072(2) 0.0536(19) 0.0012(17) 0.0084(14) 0.0127(16) C21A 0.0323(14) 0.0479(16) 0.0435(16) 0.0035(13) 0.0109(12) 0.0094(12) C22A 0.0207(10) 0.0227(10) 0.0253(11) 0.0079(9) 0.0088(9) 0.0006(8) C23A 0.0258(11) 0.0225(11) 0.0335(13) 0.0057(10) 0.0102(10) 0.0021(9) C24A 0.0280(12) 0.0320(13) 0.0400(14) 0.0133(11) 0.0137(11) 0.0105(10) C25A 0.0229(11) 0.0450(15) 0.0332(13) 0.0160(12) 0.0072(10) 0.0063(11) C26A 0.0258(12) 0.0407(14) 0.0249(12) 0.0038(11) 0.0049(10) -0.0029(10) C27A 0.0244(11) 0.0280(11) 0.0256(12) 0.0047(9) 0.0079(9) 0.0020(9) C28A 0.0219(11) 0.0260(11) 0.0246(11) 0.0023(9) 0.0096(9) -0.0019(9) C29A 0.0259(11) 0.0266(12) 0.0307(12) 0.0024(10) 0.0099(10) -0.0016(9) C30A 0.0321(13) 0.0294(12) 0.0369(14) 0.0006(11) 0.0119(11) -0.0085(10) C31A 0.0233(12) 0.0431(15) 0.0402(15) 0.0003(12) 0.0093(11) -0.0100(11) C32A 0.0230(12) 0.0398(14) 0.0427(15) 0.0015(12) 0.0116(11) 0.0024(10) C33A 0.0256(12) 0.0282(12) 0.0322(13) 0.0012(10) 0.0100(10) -0.0013(9) C34A 0.0189(10) 0.0177(10) 0.0277(11) -0.0016(9) 0.0089(9) 0.0006(8) C35A 0.0213(11) 0.0223(11) 0.0310(12) 0.0040(9) 0.0069(9) -0.0019(9) C36A 0.0210(11) 0.0288(12) 0.0422(15) 0.0037(11) 0.0077(10) -0.0040(9) C37A 0.0194(11) 0.0337(13) 0.0343(13) -0.0006(11) 0.0035(10) 0.0017(9) C38A 0.0257(12) 0.0281(12) 0.0288(12) 0.0026(10) 0.0078(10) 0.0064(9) C39A 0.0217(11) 0.0214(10) 0.0300(12) 0.0008(9) 0.0115(9) 0.0016(8) C40A 0.0214(10) 0.0238(11) 0.0209(11) -0.0005(9) 0.0081(9) 0.0014(8) C41A 0.0269(12) 0.0286(12) 0.0258(12) 0.0021(10) 0.0112(10) 0.0000(9) C42A 0.0318(13) 0.0406(14) 0.0235(12) 0.0073(11) 0.0113(10) 0.0057(11) C43A 0.0288(12) 0.0427(14) 0.0230(12) -0.0043(11) 0.0057(10) 0.0051(11) C44A 0.0293(12) 0.0340(13) 0.0290(13) -0.0044(10) 0.0061(10) -0.0052(10) C45A 0.0290(12) 0.0273(11) 0.0251(12) 0.0003(9) 0.0086(10) -0.0026(9) C46A 0.0214(11) 0.0241(11) 0.0270(12) -0.0016(9) 0.0067(9) -0.0031(9) C47A 0.0224(11) 0.0245(11) 0.0300(12) 0.0020(10) 0.0053(10) -0.0019(9) C48A 0.0251(11) 0.0265(11) 0.0252(12) 0.0046(9) 0.0048(9) -0.0014(9) C49A 0.0271(12) 0.0227(11) 0.0319(13) 0.0028(10) 0.0065(10) -0.0034(9) C50A 0.0287(13) 0.0281(12) 0.0539(17) 0.0004(12) 0.0090(12) 0.0006(10) C51A 0.0249(12) 0.0212(11) 0.0380(14) 0.0018(10) -0.0003(10) -0.0012(9) C52A 0.0255(13) 0.0358(14) 0.063(2) 0.0158(14) 0.0043(13) 0.0009(11) C53A 0.0240(14) 0.0430(17) 0.093(3) 0.0205(18) -0.0072(16) -0.0020(12) C54A 0.0468(19) 0.0312(15) 0.072(2) 0.0100(15) -0.0267(17) -0.0040(13) C55A 0.0554(19) 0.0351(15) 0.0420(17) 0.0013(13) -0.0141(14) -0.0036(13) C56A 0.0367(14) 0.0318(13) 0.0368(15) 0.0006(11) -0.0013(12) -0.0028(11) C57A 0.071(2) 0.0443(17) 0.0453(18) 0.0164(14) -0.0128(16) -0.0356(17) C58A 0.0582(19) 0.0421(16) 0.0495(18) 0.0053(14) 0.0176(15) -0.0132(14) B1A 0.0176(11) 0.0184(11) 0.0223(12) -0.0001(9) 0.0071(9) 0.0000(9) N1S 0.0405(14) 0.0596(17) 0.0604(18) 0.0048(14) 0.0061(13) -0.0102(13) C1S 0.0285(13) 0.0290(13) 0.0523(17) 0.0021(12) 0.0177(13) -0.0013(10) C2S 0.0326(13) 0.0295(13) 0.0464(16) -0.0032(11) 0.0163(12) -0.0004(10) N2S 0.068(3) 0.328(11) 0.137(5) -0.108(6) 0.040(3) -0.019(4) C3S 0.054(2) 0.122(4) 0.091(3) -0.050(3) 0.000(2) 0.013(3) C4S 0.075(3) 0.0342(16) 0.073(3) -0.0003(17) -0.014(2) 0.0055(16) _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 1.9819(16) . ? Fe1 O2 2.0647(16) . ? Fe1 N1 2.2138(18) . ? Fe1 N3 2.1054(19) . ? Fe1 N5 2.0763(19) . ? O1 C46 1.271(3) . ? O2 C48 1.246(3) . ? O3 C46 1.354(3) . ? O3 C49 1.444(3) . ? O4 C48 1.349(3) . ? O4 C57 1.444(3) . ? N1 C6 1.343(3) . ? N2 N1 1.371(2) . ? N2 C4 1.361(3) . ? N2 B1 1.552(3) . ? N3 C3 1.334(3) . ? N4 N3 1.369(2) . ? N4 C1 1.362(3) . ? N4 B1 1.558(3) . ? N5 C9 1.344(3) . ? N6 N5 1.371(2) . ? N6 C7 1.361(3) . ? N6 B1 1.548(3) . ? C1 C2 1.382(3) . ? C1 C10 1.472(3) . ? C2 H2 0.9500 . ? C2 C3 1.400(3) . ? C3 C16 1.471(3) . ? C4 C5 1.383(3) . ? C4 C22 1.481(3) . ? C5 H5 0.9500 . ? C5 C6 1.401(3) . ? C6 C28 1.478(3) . ? C7 C8 1.382(3) . ? C7 C34 1.472(3) . ? C8 H8 0.9500 . ? C8 C9 1.395(3) . ? C9 C40 1.475(3) . ? C10 C11 1.392(3) . ? C10 C15 1.398(3) . ? C11 H11 0.9500 . ? C11 C12 1.395(3) . ? C12 H12 0.9500 . ? C12 C13 1.387(4) . ? C13 H13 0.9500 . ? C13 C14 1.384(4) . ? C14 H14 0.9500 . ? C14 C15 1.388(3) . ? C15 H15 0.9500 . ? C16 C17 1.396(4) . ? C16 C21 1.389(4) . ? C17 H17 0.9500 . ? C17 C18 1.387(4) . ? C18 H18 0.9500 . ? C18 C19 1.379(5) . ? C19 H19 0.9500 . ? C19 C20 1.378(5) . ? C20 H20 0.9500 . ? C20 C21 1.391(4) . ? C21 H21 0.9500 . ? C22 C23 1.398(3) . ? C22 C27 1.396(3) . ? C23 H23 0.9500 . ? C23 C24 1.393(3) . ? C24 H24 0.9500 . ? C24 C25 1.389(4) . ? C25 H25 0.9500 . ? C25 C26 1.391(3) . ? C26 H26 0.9500 . ? C26 C27 1.386(3) . ? C27 H27 0.9500 . ? C28 C29 1.388(5) . ? C28 C33 1.394(5) . ? C29 H29 0.9500 . ? C29 C30 1.402(5) . ? C30 H30 0.9500 . ? C30 C31 1.361(8) . ? C31 H31 0.9500 . ? C31 C32 1.387(8) . ? C32 H32 0.9500 . ? C32 C33 1.388(4) . ? C33 H33 0.9500 . ? C34 C35 1.399(3) . ? C34 C39 1.396(3) . ? C35 H35 0.9500 . ? C35 C36 1.392(4) . ? C36 H36 0.9500 . ? C36 C37 1.389(4) . ? C37 H37 0.9500 . ? C37 C38 1.386(4) . ? C38 H38 0.9500 . ? C38 C39 1.384(3) . ? C39 H39 0.9500 . ? C40 C41 1.391(3) . ? C40 C45 1.394(3) . ? C41 H41 0.9500 . ? C41 C42 1.387(3) . ? C42 H42 0.9500 . ? C42 C43 1.388(4) . ? C43 H43 0.9500 . ? C43 C44 1.382(4) . ? C44 H44 0.9500 . ? C44 C45 1.388(3) . ? C45 H45 0.9500 . ? C46 C47 1.395(3) . ? C47 C48 1.422(3) . ? C47 C51 1.491(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C49 C50 1.502(5) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.397(3) . ? C51 C56 1.391(4) . ? C52 H52 0.9500 . ? C52 C53 1.393(3) . ? C53 H53 0.9500 . ? C53 C54 1.376(4) . ? C54 H54 0.9500 . ? C54 C55 1.386(4) . ? C55 H55 0.9500 . ? C55 C56 1.393(3) . ? C56 H56 0.9500 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C57 C58 1.458(5) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? B1 H1 1.0000 . ? Fe1A O1A 2.0532(16) . ? Fe1A O2A 1.9945(16) . ? Fe1A N1A 2.111(2) . ? Fe1A N3A 2.2090(18) . ? Fe1A N5A 2.1064(18) . ? O1A C48A 1.255(3) . ? O2A C46A 1.274(3) . ? O3A C48A 1.344(3) . ? O3A C57A 1.446(3) . ? O4A C46A 1.354(3) . ? O4A C49A 1.445(3) . ? N1A C3A 1.342(3) . ? N2A N1A 1.375(3) . ? N2A C1A 1.361(3) . ? N2A B1A 1.554(3) . ? N3A C6A 1.347(3) . ? N4A N3A 1.373(2) . ? N4A C4A 1.354(3) . ? N4A B1A 1.549(3) . ? N5A C9A 1.341(3) . ? N6A N5A 1.372(3) . ? N6A C7A 1.360(3) . ? N6A B1A 1.542(3) . ? C1A C2A 1.387(3) . ? C1A C10A 1.472(3) . ? C2A H2A 0.9500 . ? C2A C3A 1.394(4) . ? C3A C16A 1.484(3) . ? C4A C5A 1.385(3) . ? C4A C22A 1.478(3) . ? C5A H5A 0.9500 . ? C5A C6A 1.398(3) . ? C6A C28A 1.474(3) . ? C7A C8A 1.385(3) . ? C7A C34A 1.476(3) . ? C8A H8A 0.9500 . ? C8A C9A 1.396(3) . ? C9A C40A 1.473(3) . ? C10A C11A 1.397(3) . ? C10A C15A 1.396(3) . ? C11A H11A 0.9500 . ? C11A C12A 1.386(4) . ? C12A H12A 0.9500 . ? C12A C13A 1.388(4) . ? C13A H13A 0.9500 . ? C13A C14A 1.380(4) . ? C14A H14A 0.9500 . ? C14A C15A 1.385(4) . ? C15A H15A 0.9500 . ? C16A C17A 1.392(4) . ? C16A C21A 1.403(4) . ? C17A H17A 0.9500 . ? C17A C18A 1.398(4) . ? C18A H18A 0.9500 . ? C18A C19A 1.379(6) . ? C19A H19A 0.9500 . ? C19A C20A 1.388(6) . ? C20A H20A 0.9500 . ? C20A C21A 1.391(4) . ? C21A H21A 0.9500 . ? C22A C23A 1.400(3) . ? C22A C27A 1.396(3) . ? C23A H23A 0.9500 . ? C23A C24A 1.395(3) . ? C24A H24A 0.9500 . ? C24A C25A 1.376(4) . ? C25A H25A 0.9500 . ? C25A C26A 1.391(4) . ? C26A H26A 0.9500 . ? C26A C27A 1.389(3) . ? C27A H27A 0.9500 . ? C28A C29A 1.394(3) . ? C28A C33A 1.399(3) . ? C29A H29A 0.9500 . ? C29A C30A 1.393(3) . ? C30A H30A 0.9500 . ? C30A C31A 1.375(4) . ? C31A H31A 0.9500 . ? C31A C32A 1.397(4) . ? C32A H32A 0.9500 . ? C32A C33A 1.382(3) . ? C33A H33A 0.9500 . ? C34A C35A 1.397(3) . ? C34A C39A 1.394(3) . ? C35A H35A 0.9500 . ? C35A C36A 1.394(3) . ? C36A H36A 0.9500 . ? C36A C37A 1.384(4) . ? C37A H37A 0.9500 . ? C37A C38A 1.386(4) . ? C38A H38A 0.9500 . ? C38A C39A 1.394(3) . ? C39A H39A 0.9500 . ? C40A C41A 1.394(3) . ? C40A C45A 1.393(3) . ? C41A H41A 0.9500 . ? C41A C42A 1.387(4) . ? C42A H42A 0.9500 . ? C42A C43A 1.378(4) . ? C43A H43A 0.9500 . ? C43A C44A 1.387(4) . ? C44A H44A 0.9500 . ? C44A C45A 1.384(3) . ? C45A H45A 0.9500 . ? C46A C47A 1.392(3) . ? C47A C48A 1.414(3) . ? C47A C51A 1.497(3) . ? C49A H49C 0.9900 . ? C49A H49D 0.9900 . ? C49A C50A 1.499(3) . ? C50A H50D 0.9800 . ? C50A H50E 0.9800 . ? C50A H50F 0.9800 . ? C51A C52A 1.391(4) . ? C51A C56A 1.390(4) . ? C52A H52A 0.9500 . ? C52A C53A 1.399(4) . ? C53A H53A 0.9500 . ? C53A C54A 1.382(6) . ? C54A H54A 0.9500 . ? C54A C55A 1.377(5) . ? C55A H55A 0.9500 . ? C55A C56A 1.395(4) . ? C56A H56A 0.9500 . ? C57A H57C 0.9900 . ? C57A H57D 0.9900 . ? C57A C58A 1.444(4) . ? C58A H58D 0.9800 . ? C58A H58E 0.9800 . ? C58A H58F 0.9800 . ? B1A H1A 1.0000 . ? N1S C1S 1.141(4) . ? C1S C2S 1.449(4) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? N2S C3S 1.127(8) . ? C3S C4S 1.418(7) . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 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 O1 Fe1 O2 86.34(6) . . ? O1 Fe1 N1 97.02(7) . . ? O1 Fe1 N3 147.45(7) . . ? O1 Fe1 N5 120.57(7) . . ? O2 Fe1 N1 170.87(7) . . ? O2 Fe1 N3 90.05(7) . . ? O2 Fe1 N5 95.66(7) . . ? N3 Fe1 N1 82.54(7) . . ? N5 Fe1 N1 89.95(7) . . ? N5 Fe1 N3 91.98(7) . . ? C46 O1 Fe1 129.66(15) . . ? C48 O2 Fe1 127.54(15) . . ? C46 O3 C49 117.97(18) . . ? C48 O4 C57 117.49(18) . . ? N2 N1 Fe1 114.74(13) . . ? C6 N1 Fe1 138.81(15) . . ? C6 N1 N2 106.41(18) . . ? N1 N2 B1 119.23(17) . . ? C4 N2 N1 110.17(18) . . ? C4 N2 B1 130.60(18) . . ? N4 N3 Fe1 114.41(13) . . ? C3 N3 Fe1 137.74(15) . . ? C3 N3 N4 107.83(17) . . ? N3 N4 B1 121.35(17) . . ? C1 N4 N3 108.97(17) . . ? C1 N4 B1 128.44(17) . . ? N6 N5 Fe1 117.67(14) . . ? C9 N5 Fe1 135.29(15) . . ? C9 N5 N6 107.02(18) . . ? N5 N6 B1 118.74(17) . . ? C7 N6 N5 109.54(18) . . ? C7 N6 B1 130.91(18) . . ? N4 C1 C2 107.90(18) . . ? N4 C1 C10 124.01(19) . . ? C2 C1 C10 128.1(2) . . ? C1 C2 H2 127.1 . . ? C1 C2 C3 105.89(19) . . ? C3 C2 H2 127.1 . . ? N3 C3 C2 109.40(19) . . ? N3 C3 C16 123.2(2) . . ? C2 C3 C16 127.4(2) . . ? N2 C4 C5 107.48(19) . . ? N2 C4 C22 124.4(2) . . ? C5 C4 C22 128.1(2) . . ? C4 C5 H5 127.1 . . ? C4 C5 C6 105.8(2) . . ? C6 C5 H5 127.1 . . ? N1 C6 C5 110.1(2) . . ? N1 C6 C28 122.4(2) . . ? C5 C6 C28 127.2(2) . . ? N6 C7 C8 107.67(19) . . ? N6 C7 C34 124.2(2) . . ? C8 C7 C34 127.8(2) . . ? C7 C8 H8 126.9 . . ? C7 C8 C9 106.1(2) . . ? C9 C8 H8 126.9 . . ? N5 C9 C8 109.61(19) . . ? N5 C9 C40 121.3(2) . . ? C8 C9 C40 129.1(2) . . ? C11 C10 C1 119.5(2) . . ? C11 C10 C15 119.5(2) . . ? C15 C10 C1 121.0(2) . . ? C10 C11 H11 119.9 . . ? C10 C11 C12 120.2(2) . . ? C12 C11 H11 119.9 . . ? C11 C12 H12 119.9 . . ? C13 C12 C11 120.1(2) . . ? C13 C12 H12 119.9 . . ? C12 C13 H13 120.2 . . ? C14 C13 C12 119.6(2) . . ? C14 C13 H13 120.2 . . ? C13 C14 H14 119.6 . . ? C13 C14 C15 120.9(2) . . ? C15 C14 H14 119.6 . . ? C10 C15 H15 120.2 . . ? C14 C15 C10 119.7(2) . . ? C14 C15 H15 120.2 . . ? C17 C16 C3 119.7(2) . . ? C21 C16 C3 122.2(2) . . ? C21 C16 C17 118.1(2) . . ? C16 C17 H17 119.6 . . ? C18 C17 C16 120.8(3) . . ? C18 C17 H17 119.6 . . ? C17 C18 H18 119.9 . . ? C19 C18 C17 120.2(3) . . ? C19 C18 H18 119.9 . . ? C18 C19 H19 120.1 . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.1 . . ? C19 C20 H20 120.0 . . ? C19 C20 C21 120.0(3) . . ? C21 C20 H20 120.0 . . ? C16 C21 C20 120.9(3) . . ? C16 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C23 C22 C4 119.2(2) . . ? C27 C22 C4 121.8(2) . . ? C27 C22 C23 119.0(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 C22 120.5(2) . . ? C24 C23 H23 119.7 . . ? C23 C24 H24 120.1 . . ? C25 C24 C23 119.8(2) . . ? C25 C24 H24 120.1 . . ? C24 C25 H25 120.0 . . ? C24 C25 C26 120.1(2) . . ? C26 C25 H25 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H26 120.0 . . ? C22 C27 H27 119.7 . . ? C26 C27 C22 120.5(2) . . ? C26 C27 H27 119.7 . . ? C29 C28 C6 120.3(3) . . ? C29 C28 C33 119.5(3) . . ? C33 C28 C6 120.0(3) . . ? C28 C29 H29 120.2 . . ? C28 C29 C30 119.7(4) . . ? C30 C29 H29 120.2 . . ? C29 C30 H30 119.9 . . ? C31 C30 C29 120.3(4) . . ? C31 C30 H30 119.9 . . ? C30 C31 H31 119.7 . . ? C30 C31 C32 120.7(4) . . ? C32 C31 H31 119.7 . . ? C31 C32 H32 120.2 . . ? C31 C32 C33 119.6(5) . . ? C33 C32 H32 120.2 . . ? C28 C33 H33 119.9 . . ? C32 C33 C28 120.3(4) . . ? C32 C33 H33 119.9 . . ? C35 C34 C7 119.5(2) . . ? C39 C34 C7 121.8(2) . . ? C39 C34 C35 118.5(2) . . ? C34 C35 H35 119.8 . . ? C36 C35 C34 120.3(2) . . ? C36 C35 H35 119.8 . . ? C35 C36 H36 119.8 . . ? C37 C36 C35 120.4(3) . . ? C37 C36 H36 119.8 . . ? C36 C37 H37 120.3 . . ? C38 C37 C36 119.5(2) . . ? C38 C37 H37 120.3 . . ? C37 C38 H38 119.9 . . ? C39 C38 C37 120.3(2) . . ? C39 C38 H38 119.9 . . ? C34 C39 H39 119.5 . . ? C38 C39 C34 120.9(2) . . ? C38 C39 H39 119.5 . . ? C41 C40 C9 120.4(2) . . ? C41 C40 C45 118.7(2) . . ? C45 C40 C9 121.0(2) . . ? C40 C41 H41 119.6 . . ? C42 C41 C40 120.8(2) . . ? C42 C41 H41 119.6 . . ? C41 C42 H42 120.0 . . ? C41 C42 C43 120.1(2) . . ? C43 C42 H42 120.0 . . ? C42 C43 H43 120.1 . . ? C44 C43 C42 119.8(2) . . ? C44 C43 H43 120.1 . . ? C43 C44 H44 119.9 . . ? C43 C44 C45 120.1(2) . . ? C45 C44 H44 119.9 . . ? C40 C45 H45 119.7 . . ? C44 C45 C40 120.6(2) . . ? C44 C45 H45 119.7 . . ? O1 C46 O3 117.4(2) . . ? O1 C46 C47 128.0(2) . . ? O3 C46 C47 114.62(19) . . ? C46 C47 C48 119.5(2) . . ? C46 C47 C51 120.9(2) . . ? C48 C47 C51 119.5(2) . . ? O2 C48 O4 119.1(2) . . ? O2 C48 C47 127.4(2) . . ? O4 C48 C47 113.54(19) . . ? O3 C49 H49A 109.3 . . ? O3 C49 H49B 109.3 . . ? O3 C49 C50 111.4(2) . . ? H49A C49 H49B 108.0 . . ? C50 C49 H49A 109.3 . . ? C50 C49 H49B 109.3 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C47 120.9(2) . . ? C56 C51 C47 121.2(2) . . ? C56 C51 C52 117.9(2) . . ? C51 C52 H52 119.5 . . ? C53 C52 C51 121.0(3) . . ? C53 C52 H52 119.5 . . ? C52 C53 H53 119.9 . . ? C54 C53 C52 120.2(3) . . ? C54 C53 H53 119.9 . . ? C53 C54 H54 120.2 . . ? C53 C54 C55 119.6(2) . . ? C55 C54 H54 120.2 . . ? C54 C55 H55 119.9 . . ? C54 C55 C56 120.2(3) . . ? C56 C55 H55 119.9 . . ? C51 C56 C55 121.0(3) . . ? C51 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? O4 C57 H57A 109.5 . . ? O4 C57 H57B 109.5 . . ? O4 C57 C58 110.6(2) . . ? H57A C57 H57B 108.1 . . ? C58 C57 H57A 109.5 . . ? C58 C57 H57B 109.5 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58B 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N2 B1 N4 107.22(18) . . ? N2 B1 H1 109.5 . . ? N4 B1 H1 109.5 . . ? N6 B1 N2 109.43(17) . . ? N6 B1 N4 111.64(17) . . ? N6 B1 H1 109.5 . . ? O1A Fe1A N1A 95.17(7) . . ? O1A Fe1A N3A 173.54(7) . . ? O1A Fe1A N5A 97.25(7) . . ? O2A Fe1A O1A 86.17(7) . . ? O2A Fe1A N1A 152.35(7) . . ? O2A Fe1A N3A 91.39(7) . . ? O2A Fe1A N5A 117.23(7) . . ? N1A Fe1A N3A 84.24(7) . . ? N5A Fe1A N1A 90.06(7) . . ? N5A Fe1A N3A 89.18(7) . . ? C48A O1A Fe1A 128.55(15) . . ? C46A O2A Fe1A 129.40(15) . . ? C48A O3A C57A 118.3(2) . . ? C46A O4A C49A 118.09(18) . . ? N2A N1A Fe1A 115.85(13) . . ? C3A N1A Fe1A 136.99(17) . . ? C3A N1A N2A 107.09(19) . . ? N1A N2A B1A 120.60(18) . . ? C1A N2A N1A 109.60(18) . . ? C1A N2A B1A 129.73(19) . . ? N4A N3A Fe1A 113.03(13) . . ? C6A N3A Fe1A 138.82(15) . . ? C6A N3A N4A 106.08(17) . . ? N3A N4A B1A 120.69(17) . . ? C4A N4A N3A 110.27(17) . . ? C4A N4A B1A 129.04(18) . . ? N6A N5A Fe1A 118.04(13) . . ? C9A N5A Fe1A 132.25(15) . . ? C9A N5A N6A 106.97(17) . . ? N5A N6A B1A 118.22(17) . . ? C7A N6A N5A 109.63(18) . . ? C7A N6A B1A 131.29(19) . . ? N2A C1A C2A 107.4(2) . . ? N2A C1A C10A 123.7(2) . . ? C2A C1A C10A 129.0(2) . . ? C1A C2A H2A 126.8 . . ? C1A C2A C3A 106.3(2) . . ? C3A C2A H2A 126.8 . . ? N1A C3A C2A 109.6(2) . . ? N1A C3A C16A 120.5(2) . . ? C2A C3A C16A 129.8(2) . . ? N4A C4A C5A 107.77(19) . . ? N4A C4A C22A 123.98(19) . . ? C5A C4A C22A 128.2(2) . . ? C4A C5A H5A 127.2 . . ? C4A C5A C6A 105.52(19) . . ? C6A C5A H5A 127.2 . . ? N3A C6A C5A 110.33(19) . . ? N3A C6A C28A 123.8(2) . . ? C5A C6A C28A 125.6(2) . . ? N6A C7A C8A 107.64(19) . . ? N6A C7A C34A 124.6(2) . . ? C8A C7A C34A 127.7(2) . . ? C7A C8A H8A 127.1 . . ? C7A C8A C9A 105.89(19) . . ? C9A C8A H8A 127.1 . . ? N5A C9A C8A 109.9(2) . . ? N5A C9A C40A 120.9(2) . . ? C8A C9A C40A 129.1(2) . . ? C11A C10A C1A 118.6(2) . . ? C15A C10A C1A 122.4(2) . . ? C15A C10A C11A 119.0(2) . . ? C10A C11A H11A 120.0 . . ? C12A C11A C10A 120.0(2) . . ? C12A C11A H11A 120.0 . . ? C11A C12A H12A 119.7 . . ? C11A C12A C13A 120.5(3) . . ? C13A C12A H12A 119.7 . . ? C12A C13A H13A 120.2 . . ? C14A C13A C12A 119.6(3) . . ? C14A C13A H13A 120.2 . . ? C13A C14A H14A 119.8 . . ? C13A C14A C15A 120.4(3) . . ? C15A C14A H14A 119.8 . . ? C10A C15A H15A 119.8 . . ? C14A C15A C10A 120.4(2) . . ? C14A C15A H15A 119.8 . . ? C17A C16A C3A 119.5(3) . . ? C17A C16A C21A 118.6(3) . . ? C21A C16A C3A 121.9(2) . . ? C16A C17A H17A 119.9 . . ? C16A C17A C18A 120.3(3) . . ? C18A C17A H17A 119.9 . . ? C17A C18A H18A 119.8 . . ? C19A C18A C17A 120.3(3) . . ? C19A C18A H18A 119.8 . . ? C18A C19A H19A 119.8 . . ? C18A C19A C20A 120.3(3) . . ? C20A C19A H19A 119.8 . . ? C19A C20A H20A 120.3 . . ? C19A C20A C21A 119.5(4) . . ? C21A C20A H20A 120.3 . . ? C16A C21A H21A 119.5 . . ? C20A C21A C16A 121.0(3) . . ? C20A C21A H21A 119.5 . . ? C23A C22A C4A 118.3(2) . . ? C27A C22A C4A 122.3(2) . . ? C27A C22A C23A 119.3(2) . . ? C22A C23A H23A 120.0 . . ? C24A C23A C22A 119.9(2) . . ? C24A C23A H23A 120.0 . . ? C23A C24A H24A 119.9 . . ? C25A C24A C23A 120.2(2) . . ? C25A C24A H24A 119.9 . . ? C24A C25A H25A 119.8 . . ? C24A C25A C26A 120.4(2) . . ? C26A C25A H25A 119.8 . . ? C25A C26A H26A 120.1 . . ? C27A C26A C25A 119.9(2) . . ? C27A C26A H26A 120.1 . . ? C22A C27A H27A 119.9 . . ? C26A C27A C22A 120.3(2) . . ? C26A C27A H27A 119.9 . . ? C29A C28A C6A 119.7(2) . . ? C29A C28A C33A 118.3(2) . . ? C33A C28A C6A 121.8(2) . . ? C28A C29A H29A 119.5 . . ? C30A C29A C28A 121.1(2) . . ? C30A C29A H29A 119.5 . . ? C29A C30A H30A 120.0 . . ? C31A C30A C29A 119.9(2) . . ? C31A C30A H30A 120.0 . . ? C30A C31A H31A 120.1 . . ? C30A C31A C32A 119.8(2) . . ? C32A C31A H31A 120.1 . . ? C31A C32A H32A 119.9 . . ? C33A C32A C31A 120.2(2) . . ? C33A C32A H32A 119.9 . . ? C28A C33A H33A 119.7 . . ? C32A C33A C28A 120.7(2) . . ? C32A C33A H33A 119.7 . . ? C35A C34A C7A 118.3(2) . . ? C39A C34A C7A 122.9(2) . . ? C39A C34A C35A 118.7(2) . . ? C34A C35A H35A 119.7 . . ? C36A C35A C34A 120.6(2) . . ? C36A C35A H35A 119.7 . . ? C35A C36A H36A 120.0 . . ? C37A C36A C35A 120.1(2) . . ? C37A C36A H36A 120.0 . . ? C36A C37A H37A 120.1 . . ? C36A C37A C38A 119.8(2) . . ? C38A C37A H37A 120.1 . . ? C37A C38A H38A 119.8 . . ? C37A C38A C39A 120.3(2) . . ? C39A C38A H38A 119.8 . . ? C34A C39A C38A 120.4(2) . . ? C34A C39A H39A 119.8 . . ? C38A C39A H39A 119.8 . . ? C41A C40A C9A 121.0(2) . . ? C45A C40A C9A 120.1(2) . . ? C45A C40A C41A 118.9(2) . . ? C40A C41A H41A 120.0 . . ? C42A C41A C40A 119.9(2) . . ? C42A C41A H41A 120.0 . . ? C41A C42A H42A 119.7 . . ? C43A C42A C41A 120.7(2) . . ? C43A C42A H42A 119.7 . . ? C42A C43A H43A 120.0 . . ? C42A C43A C44A 119.9(2) . . ? C44A C43A H43A 120.0 . . ? C43A C44A H44A 120.2 . . ? C45A C44A C43A 119.7(2) . . ? C45A C44A H44A 120.2 . . ? C40A C45A H45A 119.6 . . ? C44A C45A C40A 120.9(2) . . ? C44A C45A H45A 119.6 . . ? O2A C46A O4A 117.3(2) . . ? O2A C46A C47A 128.1(2) . . ? O4A C46A C47A 114.7(2) . . ? C46A C47A C48A 119.8(2) . . ? C46A C47A C51A 119.8(2) . . ? C48A C47A C51A 120.3(2) . . ? O1A C48A O3A 118.9(2) . . ? O1A C48A C47A 127.2(2) . . ? O3A C48A C47A 113.9(2) . . ? O4A C49A H49C 109.2 . . ? O4A C49A H49D 109.2 . . ? O4A C49A C50A 112.1(2) . . ? H49C C49A H49D 107.9 . . ? C50A C49A H49C 109.2 . . ? C50A C49A H49D 109.2 . . ? C49A C50A H50D 109.5 . . ? C49A C50A H50E 109.5 . . ? C49A C50A H50F 109.5 . . ? H50D C50A H50E 109.5 . . ? H50D C50A H50F 109.5 . . ? H50E C50A H50F 109.5 . . ? C52A C51A C47A 119.8(3) . . ? C56A C51A C47A 121.8(2) . . ? C56A C51A C52A 118.4(3) . . ? C51A C52A H52A 119.7 . . ? C51A C52A C53A 120.7(3) . . ? C53A C52A H52A 119.7 . . ? C52A C53A H53A 119.9 . . ? C54A C53A C52A 120.1(3) . . ? C54A C53A H53A 119.9 . . ? C53A C54A H54A 120.2 . . ? C55A C54A C53A 119.7(3) . . ? C55A C54A H54A 120.2 . . ? C54A C55A H55A 119.8 . . ? C54A C55A C56A 120.4(3) . . ? C56A C55A H55A 119.8 . . ? C51A C56A C55A 120.8(3) . . ? C51A C56A H56A 119.6 . . ? C55A C56A H56A 119.6 . . ? O3A C57A H57C 109.7 . . ? O3A C57A H57D 109.7 . . ? H57C C57A H57D 108.2 . . ? C58A C57A O3A 109.8(3) . . ? C58A C57A H57C 109.7 . . ? C58A C57A H57D 109.7 . . ? C57A C58A H58D 109.5 . . ? C57A C58A H58E 109.5 . . ? C57A C58A H58F 109.5 . . ? H58D C58A H58E 109.5 . . ? H58D C58A H58F 109.5 . . ? H58E C58A H58F 109.5 . . ? N2A B1A H1A 109.4 . . ? N4A B1A N2A 108.96(17) . . ? N4A B1A H1A 109.4 . . ? N6A B1A N2A 110.12(18) . . ? N6A B1A N4A 109.61(18) . . ? N6A B1A H1A 109.4 . . ? N1S C1S C2S 179.4(3) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SB 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? N2S C3S C4S 177.9(8) . . ? C3S C4S H4SA 109.5 . . ? C3S C4S H4SB 109.5 . . ? C3S C4S H4SC 109.5 . . ? H4SA C4S H4SB 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 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 Fe1 O1 C46 O3 -176.67(15) . . . . ? Fe1 O1 C46 C47 3.1(4) . . . . ? Fe1 O2 C48 O4 -164.66(16) . . . . ? Fe1 O2 C48 C47 14.8(4) . . . . ? Fe1 N1 C6 C5 -175.71(18) . . . . ? Fe1 N1 C6 C28 9.9(4) . . . . ? Fe1 N3 C3 C2 178.43(17) . . . . ? Fe1 N3 C3 C16 -0.2(4) . . . . ? Fe1 N5 C9 C8 -178.19(16) . . . . ? Fe1 N5 C9 C40 1.9(3) . . . . ? O1 Fe1 O2 C48 -12.93(19) . . . . ? O1 Fe1 N1 N2 -161.02(15) . . . . ? O1 Fe1 N1 C6 16.1(3) . . . . ? O1 Fe1 N3 N4 -147.43(14) . . . . ? O1 Fe1 N3 C3 34.3(3) . . . . ? O1 Fe1 N5 N6 135.07(14) . . . . ? O1 Fe1 N5 C9 -47.2(2) . . . . ? O1 C46 C47 C48 -5.9(4) . . . . ? O1 C46 C47 C51 176.5(2) . . . . ? O2 Fe1 O1 C46 4.5(2) . . . . ? O2 Fe1 N1 N2 87.8(4) . . . . ? O2 Fe1 N1 C6 -95.0(5) . . . . ? O2 Fe1 N3 N4 129.30(15) . . . . ? O2 Fe1 N3 C3 -49.0(2) . . . . ? O2 Fe1 N5 N6 -135.85(14) . . . . ? O2 Fe1 N5 C9 41.9(2) . . . . ? O3 C46 C47 C48 173.9(2) . . . . ? O3 C46 C47 C51 -3.7(3) . . . . ? N1 Fe1 O1 C46 -167.0(2) . . . . ? N1 Fe1 O2 C48 99.0(4) . . . . ? N1 Fe1 N3 N4 -56.06(15) . . . . ? N1 Fe1 N3 C3 125.6(2) . . . . ? N1 Fe1 N5 N6 36.93(15) . . . . ? N1 Fe1 N5 C9 -145.3(2) . . . . ? N1 N2 C4 C5 -0.9(3) . . . . ? N1 N2 C4 C22 177.6(2) . . . . ? N1 N2 B1 N4 -58.9(2) . . . . ? N1 N2 B1 N6 62.4(2) . . . . ? N1 C6 C28 C29 -141.6(3) . . . . ? N1 C6 C28 C33 44.4(4) . . . . ? N2 N1 C6 C5 1.6(3) . . . . ? N2 N1 C6 C28 -172.8(2) . . . . ? N2 C4 C5 C6 1.8(3) . . . . ? N2 C4 C22 C23 134.0(2) . . . . ? N2 C4 C22 C27 -48.1(3) . . . . ? N3 Fe1 O1 C46 -79.9(2) . . . . ? N3 Fe1 O2 C48 134.7(2) . . . . ? N3 Fe1 N1 N2 51.79(15) . . . . ? N3 Fe1 N1 C6 -131.0(3) . . . . ? N3 Fe1 N5 N6 -45.60(15) . . . . ? N3 Fe1 N5 C9 132.2(2) . . . . ? N3 N4 C1 C2 0.0(2) . . . . ? N3 N4 C1 C10 179.1(2) . . . . ? N3 N4 B1 N2 54.8(2) . . . . ? N3 N4 B1 N6 -65.0(3) . . . . ? N3 C3 C16 C17 154.3(2) . . . . ? N3 C3 C16 C21 -25.4(4) . . . . ? N4 N3 C3 C2 0.1(2) . . . . ? N4 N3 C3 C16 -178.5(2) . . . . ? N4 C1 C2 C3 0.0(3) . . . . ? N4 C1 C10 C11 127.2(2) . . . . ? N4 C1 C10 C15 -54.3(3) . . . . ? N5 Fe1 O1 C46 98.9(2) . . . . ? N5 Fe1 O2 C48 -133.31(19) . . . . ? N5 Fe1 N1 N2 -40.21(15) . . . . ? N5 Fe1 N1 C6 137.0(2) . . . . ? N5 Fe1 N3 N4 33.63(15) . . . . ? N5 Fe1 N3 C3 -144.7(2) . . . . ? N5 N6 C7 C8 -1.4(2) . . . . ? N5 N6 C7 C34 173.04(19) . . . . ? N5 N6 B1 N2 -67.8(2) . . . . ? N5 N6 B1 N4 50.7(2) . . . . ? N5 C9 C40 C41 -130.0(2) . . . . ? N5 C9 C40 C45 49.7(3) . . . . ? N6 N5 C9 C8 -0.3(2) . . . . ? N6 N5 C9 C40 179.86(19) . . . . ? N6 C7 C8 C9 1.2(2) . . . . ? N6 C7 C34 C35 151.0(2) . . . . ? N6 C7 C34 C39 -34.9(3) . . . . ? C1 N4 N3 Fe1 -178.83(14) . . . . ? C1 N4 N3 C3 0.0(2) . . . . ? C1 N4 B1 N2 -111.0(2) . . . . ? C1 N4 B1 N6 129.2(2) . . . . ? C1 C2 C3 N3 -0.1(3) . . . . ? C1 C2 C3 C16 178.5(2) . . . . ? C1 C10 C11 C12 177.8(2) . . . . ? C1 C10 C15 C14 -178.2(2) . . . . ? C2 C1 C10 C11 -53.8(3) . . . . ? C2 C1 C10 C15 124.6(3) . . . . ? C2 C3 C16 C17 -24.0(4) . . . . ? C2 C3 C16 C21 156.3(2) . . . . ? C3 C16 C17 C18 -178.7(2) . . . . ? C3 C16 C21 C20 177.6(2) . . . . ? C4 N2 N1 Fe1 177.62(14) . . . . ? C4 N2 N1 C6 -0.4(2) . . . . ? C4 N2 B1 N4 120.8(2) . . . . ? C4 N2 B1 N6 -117.9(2) . . . . ? C4 C5 C6 N1 -2.1(3) . . . . ? C4 C5 C6 C28 171.9(3) . . . . ? C4 C22 C23 C24 178.9(2) . . . . ? C4 C22 C27 C26 -179.2(2) . . . . ? C5 C4 C22 C23 -47.8(3) . . . . ? C5 C4 C22 C27 130.1(3) . . . . ? C5 C6 C28 C29 45.0(4) . . . . ? C5 C6 C28 C33 -128.9(3) . . . . ? C6 C28 C29 C30 -175.4(3) . . . . ? C6 C28 C33 C32 175.8(3) . . . . ? C7 N6 N5 Fe1 179.37(13) . . . . ? C7 N6 N5 C9 1.0(2) . . . . ? C7 N6 B1 N2 123.6(2) . . . . ? C7 N6 B1 N4 -117.8(2) . . . . ? C7 C8 C9 N5 -0.6(2) . . . . ? C7 C8 C9 C40 179.3(2) . . . . ? C7 C34 C35 C36 173.8(2) . . . . ? C7 C34 C39 C38 -176.0(2) . . . . ? C8 C7 C34 C35 -35.8(3) . . . . ? C8 C7 C34 C39 138.4(2) . . . . ? C8 C9 C40 C41 50.1(3) . . . . ? C8 C9 C40 C45 -130.2(3) . . . . ? C9 C40 C41 C42 179.7(2) . . . . ? C9 C40 C45 C44 -179.7(2) . . . . ? C10 C1 C2 C3 -179.0(2) . . . . ? C10 C11 C12 C13 0.4(4) . . . . ? C11 C10 C15 C14 0.3(4) . . . . ? C11 C12 C13 C14 0.3(4) . . . . ? C12 C13 C14 C15 -0.7(4) . . . . ? C13 C14 C15 C10 0.4(4) . . . . ? C15 C10 C11 C12 -0.7(3) . . . . ? C16 C17 C18 C19 1.0(5) . . . . ? C17 C16 C21 C20 -2.1(4) . . . . ? C17 C18 C19 C20 -2.1(5) . . . . ? C18 C19 C20 C21 1.1(4) . . . . ? C19 C20 C21 C16 1.0(4) . . . . ? C21 C16 C17 C18 1.0(4) . . . . ? C22 C4 C5 C6 -176.7(2) . . . . ? C22 C23 C24 C25 0.1(4) . . . . ? C23 C22 C27 C26 -1.3(3) . . . . ? C23 C24 C25 C26 -0.7(4) . . . . ? C24 C25 C26 C27 0.3(4) . . . . ? C25 C26 C27 C22 0.7(4) . . . . ? C27 C22 C23 C24 0.9(3) . . . . ? C28 C29 C30 C31 -0.5(6) . . . . ? C29 C28 C33 C32 1.8(5) . . . . ? C29 C30 C31 C32 2.1(7) . . . . ? C30 C31 C32 C33 -1.7(7) . . . . ? C31 C32 C33 C28 -0.3(6) . . . . ? C33 C28 C29 C30 -1.5(5) . . . . ? C34 C7 C8 C9 -173.0(2) . . . . ? C34 C35 C36 C37 2.4(4) . . . . ? C35 C34 C39 C38 -1.8(3) . . . . ? C35 C36 C37 C38 -1.8(5) . . . . ? C36 C37 C38 C39 -0.5(4) . . . . ? C37 C38 C39 C34 2.3(4) . . . . ? C39 C34 C35 C36 -0.6(4) . . . . ? C40 C41 C42 C43 -0.1(4) . . . . ? C41 C40 C45 C44 0.1(4) . . . . ? C41 C42 C43 C44 0.1(4) . . . . ? C42 C43 C44 C45 0.0(4) . . . . ? C43 C44 C45 C40 -0.1(4) . . . . ? C45 C40 C41 C42 0.0(4) . . . . ? C46 O3 C49 C50 83.6(3) . . . . ? C46 C47 C48 O2 -3.9(4) . . . . ? C46 C47 C48 O4 175.6(2) . . . . ? C46 C47 C51 C52 -60.5(3) . . . . ? C46 C47 C51 C56 120.3(3) . . . . ? C47 C51 C52 C53 -179.7(2) . . . . ? C47 C51 C56 C55 179.4(2) . . . . ? C48 O4 C57 C58 -90.5(3) . . . . ? C48 C47 C51 C52 121.9(3) . . . . ? C48 C47 C51 C56 -57.3(3) . . . . ? C49 O3 C46 O1 1.5(3) . . . . ? C49 O3 C46 C47 -178.3(2) . . . . ? C51 C47 C48 O2 173.8(2) . . . . ? C51 C47 C48 O4 -6.7(3) . . . . ? C51 C52 C53 C54 0.2(4) . . . . ? C52 C51 C56 C55 0.1(4) . . . . ? C52 C53 C54 C55 0.4(4) . . . . ? C53 C54 C55 C56 -0.7(4) . . . . ? C54 C55 C56 C51 0.5(4) . . . . ? C56 C51 C52 C53 -0.5(4) . . . . ? C57 O4 C48 O2 -0.5(3) . . . . ? C57 O4 C48 C47 180.0(2) . . . . ? B1 N2 N1 Fe1 -2.6(2) . . . . ? B1 N2 N1 C6 179.30(19) . . . . ? B1 N2 C4 C5 179.4(2) . . . . ? B1 N2 C4 C22 -2.1(4) . . . . ? B1 N4 N3 Fe1 12.9(2) . . . . ? B1 N4 N3 C3 -168.32(19) . . . . ? B1 N4 C1 C2 167.2(2) . . . . ? B1 N4 C1 C10 -13.7(3) . . . . ? B1 N6 N5 Fe1 8.5(2) . . . . ? B1 N6 N5 C9 -169.83(18) . . . . ? B1 N6 C7 C8 168.0(2) . . . . ? B1 N6 C7 C34 -17.6(3) . . . . ? Fe1A O1A C48A O3A 172.47(17) . . . . ? Fe1A O1A C48A C47A -8.3(4) . . . . ? Fe1A O2A C46A O4A 175.36(14) . . . . ? Fe1A O2A C46A C47A -4.0(4) . . . . ? Fe1A N1A C3A C2A 175.96(17) . . . . ? Fe1A N1A C3A C16A -3.6(4) . . . . ? Fe1A N3A C6A C5A 160.10(17) . . . . ? Fe1A N3A C6A C28A -25.4(4) . . . . ? Fe1A N5A C9A C8A 159.38(16) . . . . ? Fe1A N5A C9A C40A -24.0(3) . . . . ? O1A Fe1A O2A C46A -3.0(2) . . . . ? O1A Fe1A N1A N2A -138.83(14) . . . . ? O1A Fe1A N1A C3A 44.8(2) . . . . ? O1A Fe1A N3A N4A -141.3(6) . . . . ? O1A Fe1A N3A C6A 58.1(7) . . . . ? O1A Fe1A N5A N6A 133.26(14) . . . . ? O1A Fe1A N5A C9A -25.2(2) . . . . ? O2A Fe1A O1A C48A 8.8(2) . . . . ? O2A Fe1A N1A N2A 129.56(16) . . . . ? O2A Fe1A N1A C3A -46.8(3) . . . . ? O2A Fe1A N3A N4A 151.10(14) . . . . ? O2A Fe1A N3A C6A -9.5(2) . . . . ? O2A Fe1A N5A N6A -137.33(14) . . . . ? O2A Fe1A N5A C9A 64.2(2) . . . . ? O2A C46A C47A C48A 7.6(4) . . . . ? O2A C46A C47A C51A -175.6(2) . . . . ? O4A C46A C47A C48A -171.8(2) . . . . ? O4A C46A C47A C51A 5.1(3) . . . . ? N1A Fe1A O1A C48A -143.4(2) . . . . ? N1A Fe1A O2A C46A 90.8(2) . . . . ? N1A Fe1A N3A N4A -56.27(14) . . . . ? N1A Fe1A N3A C6A 143.2(2) . . . . ? N1A Fe1A N5A N6A 38.04(15) . . . . ? N1A Fe1A N5A C9A -120.5(2) . . . . ? N1A N2A C1A C2A -0.5(2) . . . . ? N1A N2A C1A C10A 178.49(19) . . . . ? N1A N2A B1A N4A -61.3(2) . . . . ? N1A N2A B1A N6A 58.9(2) . . . . ? N1A C3A C16A C17A -142.8(3) . . . . ? N1A C3A C16A C21A 37.4(4) . . . . ? N2A N1A C3A C2A -0.6(3) . . . . ? N2A N1A C3A C16A 179.8(2) . . . . ? N2A C1A C2A C3A 0.2(3) . . . . ? N2A C1A C10A C11A -129.6(2) . . . . ? N2A C1A C10A C15A 51.9(3) . . . . ? N3A Fe1A O1A C48A -59.0(7) . . . . ? N3A Fe1A O2A C46A 171.0(2) . . . . ? N3A Fe1A N1A N2A 47.62(14) . . . . ? N3A Fe1A N1A C3A -128.7(2) . . . . ? N3A Fe1A N5A N6A -46.19(15) . . . . ? N3A Fe1A N5A C9A 155.3(2) . . . . ? N3A N4A C4A C5A -0.7(2) . . . . ? N3A N4A C4A C22A 177.5(2) . . . . ? N3A N4A B1A N2A 49.6(3) . . . . ? N3A N4A B1A N6A -71.0(2) . . . . ? N3A C6A C28A C29A 146.8(2) . . . . ? N3A C6A C28A C33A -38.7(3) . . . . ? N4A N3A C6A C5A -1.3(2) . . . . ? N4A N3A C6A C28A 173.2(2) . . . . ? N4A C4A C5A C6A -0.1(2) . . . . ? N4A C4A C22A C23A -120.8(2) . . . . ? N4A C4A C22A C27A 59.7(3) . . . . ? N5A Fe1A O1A C48A 125.8(2) . . . . ? N5A Fe1A O2A C46A -99.2(2) . . . . ? N5A Fe1A N1A N2A -41.55(15) . . . . ? N5A Fe1A N1A C3A 142.1(2) . . . . ? N5A Fe1A N3A N4A 33.87(14) . . . . ? N5A Fe1A N3A C6A -126.7(2) . . . . ? N5A N6A C7A C8A 0.6(2) . . . . ? N5A N6A C7A C34A -177.43(19) . . . . ? N5A N6A B1A N2A -63.3(2) . . . . ? N5A N6A B1A N4A 56.6(2) . . . . ? N5A C9A C40A C41A 135.1(2) . . . . ? N5A C9A C40A C45A -47.0(3) . . . . ? N6A N5A C9A C8A -0.9(2) . . . . ? N6A N5A C9A C40A 175.79(19) . . . . ? N6A C7A C8A C9A -1.0(2) . . . . ? N6A C7A C34A C35A -140.7(2) . . . . ? N6A C7A C34A C39A 41.2(3) . . . . ? C1A N2A N1A Fe1A -176.68(14) . . . . ? C1A N2A N1A C3A 0.7(2) . . . . ? C1A N2A B1A N4A 115.5(2) . . . . ? C1A N2A B1A N6A -124.3(2) . . . . ? C1A C2A C3A N1A 0.3(3) . . . . ? C1A C2A C3A C16A 179.8(2) . . . . ? C1A C10A C11A C12A -179.2(2) . . . . ? C1A C10A C15A C14A -179.1(2) . . . . ? C2A C1A C10A C11A 49.2(3) . . . . ? C2A C1A C10A C15A -129.3(3) . . . . ? C2A C3A C16A C17A 37.7(4) . . . . ? C2A C3A C16A C21A -142.0(3) . . . . ? C3A C16A C17A C18A 179.8(3) . . . . ? C3A C16A C21A C20A -179.2(3) . . . . ? C4A N4A N3A Fe1A -165.56(14) . . . . ? C4A N4A N3A C6A 1.3(2) . . . . ? C4A N4A B1A N2A -129.7(2) . . . . ? C4A N4A B1A N6A 109.8(2) . . . . ? C4A C5A C6A N3A 0.9(3) . . . . ? C4A C5A C6A C28A -173.5(2) . . . . ? C4A C22A C23A C24A 179.2(2) . . . . ? C4A C22A C27A C26A -179.2(2) . . . . ? C5A C4A C22A C23A 57.1(3) . . . . ? C5A C4A C22A C27A -122.5(3) . . . . ? C5A C6A C28A C29A -39.6(3) . . . . ? C5A C6A C28A C33A 134.9(3) . . . . ? C6A C28A C29A C30A 173.3(2) . . . . ? C6A C28A C33A C32A -174.0(2) . . . . ? C7A N6A N5A Fe1A -163.34(14) . . . . ? C7A N6A N5A C9A 0.2(2) . . . . ? C7A N6A B1A N2A 104.8(2) . . . . ? C7A N6A B1A N4A -135.3(2) . . . . ? C7A C8A C9A N5A 1.2(3) . . . . ? C7A C8A C9A C40A -175.1(2) . . . . ? C7A C34A C35A C36A -179.8(2) . . . . ? C7A C34A C39A C38A -179.7(2) . . . . ? C8A C7A C34A C35A 41.7(3) . . . . ? C8A C7A C34A C39A -136.4(2) . . . . ? C8A C9A C40A C41A -49.0(3) . . . . ? C8A C9A C40A C45A 129.0(3) . . . . ? C9A C40A C41A C42A 178.6(2) . . . . ? C9A C40A C45A C44A -178.6(2) . . . . ? C10A C1A C2A C3A -178.8(2) . . . . ? C10A C11A C12A C13A -0.9(4) . . . . ? C11A C10A C15A C14A 2.4(4) . . . . ? C11A C12A C13A C14A 0.9(4) . . . . ? C12A C13A C14A C15A 0.8(4) . . . . ? C13A C14A C15A C10A -2.5(4) . . . . ? C15A C10A C11A C12A -0.7(4) . . . . ? C16A C17A C18A C19A -0.7(6) . . . . ? C17A C16A C21A C20A 1.1(4) . . . . ? C17A C18A C19A C20A 1.2(6) . . . . ? C18A C19A C20A C21A -0.5(6) . . . . ? C19A C20A C21A C16A -0.6(5) . . . . ? C21A C16A C17A C18A -0.4(5) . . . . ? C22A C4A C5A C6A -178.2(2) . . . . ? C22A C23A C24A C25A 0.3(4) . . . . ? C23A C22A C27A C26A 1.2(3) . . . . ? C23A C24A C25A C26A 0.6(4) . . . . ? C24A C25A C26A C27A -0.6(4) . . . . ? C25A C26A C27A C22A -0.3(4) . . . . ? C27A C22A C23A C24A -1.2(3) . . . . ? C28A C29A C30A C31A 0.9(4) . . . . ? C29A C28A C33A C32A 0.6(4) . . . . ? C29A C30A C31A C32A 0.3(4) . . . . ? C30A C31A C32A C33A -1.2(4) . . . . ? C31A C32A C33A C28A 0.7(4) . . . . ? C33A C28A C29A C30A -1.4(4) . . . . ? C34A C7A C8A C9A 176.9(2) . . . . ? C34A C35A C36A C37A 0.4(4) . . . . ? C35A C34A C39A C38A 2.2(3) . . . . ? C35A C36A C37A C38A 0.4(4) . . . . ? C36A C37A C38A C39A 0.2(4) . . . . ? C37A C38A C39A C34A -1.6(4) . . . . ? C39A C34A C35A C36A -1.7(3) . . . . ? C40A C41A C42A C43A -0.6(4) . . . . ? C41A C40A C45A C44A -0.6(3) . . . . ? C41A C42A C43A C44A 0.6(4) . . . . ? C42A C43A C44A C45A -0.6(4) . . . . ? C43A C44A C45A C40A 0.6(4) . . . . ? C45A C40A C41A C42A 0.6(3) . . . . ? C46A O4A C49A C50A -79.0(3) . . . . ? C46A C47A C48A O1A -1.0(4) . . . . ? C46A C47A C48A O3A 178.3(2) . . . . ? C46A C47A C51A C52A 63.4(3) . . . . ? C46A C47A C51A C56A -115.8(3) . . . . ? C47A C51A C52A C53A -178.7(3) . . . . ? C47A C51A C56A C55A 178.5(2) . . . . ? C48A O3A C57A C58A 143.4(3) . . . . ? C48A C47A C51A C52A -119.8(3) . . . . ? C48A C47A C51A C56A 61.0(3) . . . . ? C49A O4A C46A O2A -0.8(3) . . . . ? C49A O4A C46A C47A 178.6(2) . . . . ? C51A C47A C48A O1A -177.8(2) . . . . ? C51A C47A C48A O3A 1.5(3) . . . . ? C51A C52A C53A C54A 0.1(5) . . . . ? C52A C51A C56A C55A -0.7(4) . . . . ? C52A C53A C54A C55A -0.6(5) . . . . ? C53A C54A C55A C56A 0.5(5) . . . . ? C54A C55A C56A C51A 0.2(4) . . . . ? C56A C51A C52A C53A 0.5(4) . . . . ? C57A O3A C48A O1A 1.7(4) . . . . ? C57A O3A C48A C47A -177.7(3) . . . . ? B1A N2A N1A Fe1A 0.7(2) . . . . ? B1A N2A N1A C3A 178.12(19) . . . . ? B1A N2A C1A C2A -177.6(2) . . . . ? B1A N2A C1A C10A 1.4(3) . . . . ? B1A N4A N3A Fe1A 15.1(2) . . . . ? B1A N4A N3A C6A -178.12(18) . . . . ? B1A N4A C4A C5A 178.6(2) . . . . ? B1A N4A C4A C22A -3.2(3) . . . . ? B1A N6A N5A Fe1A 7.2(2) . . . . ? B1A N6A N5A C9A 170.72(18) . . . . ? B1A N6A C7A C8A -168.3(2) . . . . ? B1A N6A C7A C34A 13.7(3) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -24 0 0 0.0395 -23.9972 -0.0002 -0.0007 -0.1929 0.9743 -0.1099 24 0 0 0.0165 23.9972 0.0002 0.0007 0.1929 -0.9743 0.1099 -3 -4 11 0.2128 -2.9954 -4.0009 10.9988 -0.3302 -0.0501 0.8853 2 -7 -7 0.1152 2.0020 -7.0007 -7.0010 -0.8461 -0.1646 -0.4094 2 8 -7 0.1925 1.9942 8.0013 -6.9982 0.8149 0.1383 -0.6507 -2 7 8 0.1645 -2.0018 7.0007 8.0010 0.8586 0.1563 0.4853 #===END data_1acacPhF3(NO) _audit_creation_date 2011-12-30 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H28 B F3 Fe N7 O3, Cl0.69, C2 H3 N' _chemical_formula_sum 'C27 H31 B Cl0.69 F3 Fe N8 O3' _chemical_formula_weight 663.78 _chemical_melting_point ? _chemical_oxdiff_formula 'Fe C25 H28 N7 O3 B F3' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.93066(19) _cell_length_b 19.6395(3) _cell_length_c 20.7317(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.126(2) _cell_angle_gamma 90.00 _cell_volume 3228.42(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 11394 _cell_measurement_temperature 100(1) _cell_measurement_theta_max 73.7234 _cell_measurement_theta_min 4.2624 _exptl_absorpt_coefficient_mu 4.782 _exptl_absorpt_correction_T_max 0.815 _exptl_absorpt_correction_T_min 0.414 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour brown _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1371 _exptl_crystal_size_max 0.3187 _exptl_crystal_size_mid 0.1704 _exptl_crystal_size_min 0.0496 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_unetI/netI 0.0292 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 28399 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 73.89 _diffrn_reflns_theta_min 4.27 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -107.00 -38.00 1.0000 6.5200 omega____ theta____ kappa____ phi______ frames - -40.6746 -57.0000 0.0000 69 #__ type_ start__ end____ width___ exp.time_ 2 omega -45.00 34.00 1.0000 6.5200 omega____ theta____ kappa____ phi______ frames - -40.6746 37.0000 -30.0000 79 #__ type_ start__ end____ width___ exp.time_ 3 omega -112.00 -53.00 1.0000 6.5200 omega____ theta____ kappa____ phi______ frames - -40.6746 -158.0000 -4.0000 59 #__ type_ start__ end____ width___ exp.time_ 4 omega 53.00 88.00 1.0000 6.5200 omega____ theta____ kappa____ phi______ frames - 40.6746 -125.0000 60.0000 35 #__ type_ start__ end____ width___ exp.time_ 5 omega 53.00 79.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 -94.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 6 omega 94.00 166.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 125.0000 -150.0000 72 #__ type_ start__ end____ width___ exp.time_ 7 omega 26.00 108.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 -94.0000 -60.0000 82 #__ type_ start__ end____ width___ exp.time_ 8 omega 34.00 79.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 -30.0000 -90.0000 45 #__ type_ start__ end____ width___ exp.time_ 9 omega 80.00 178.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 45.0000 30.0000 98 #__ type_ start__ end____ width___ exp.time_ 10 omega 50.00 105.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 -94.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 11 omega 43.00 89.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 -30.0000 90.0000 46 #__ type_ start__ end____ width___ exp.time_ 12 omega 31.00 71.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 -30.0000 150.0000 40 #__ type_ start__ end____ width___ exp.time_ 13 omega -115.00 -11.00 1.0000 6.5200 omega____ theta____ kappa____ phi______ frames - -40.6746 -57.0000 -150.0000 104 #__ type_ start__ end____ width___ exp.time_ 14 omega -115.00 -11.00 1.0000 6.5200 omega____ theta____ kappa____ phi______ frames - -40.6746 -57.0000 90.0000 104 #__ type_ start__ end____ width___ exp.time_ 15 omega 1.00 83.00 1.0000 6.5200 omega____ theta____ kappa____ phi______ frames - 40.6746 -99.0000 -150.0000 82 #__ type_ start__ end____ width___ exp.time_ 16 omega 79.00 178.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 45.0000 90.0000 99 #__ type_ start__ end____ width___ exp.time_ 17 omega 79.00 178.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 45.0000 -90.0000 99 #__ type_ start__ end____ width___ exp.time_ 18 omega 23.00 109.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 -94.0000 -150.0000 86 #__ type_ start__ end____ width___ exp.time_ 19 omega 73.00 98.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 77.0000 120.0000 25 #__ type_ start__ end____ width___ exp.time_ 20 omega 79.00 178.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 45.0000 -30.0000 99 #__ type_ start__ end____ width___ exp.time_ 21 omega 79.00 178.00 1.0000 26.1000 omega____ theta____ kappa____ phi______ frames - 107.0119 45.0000 -180.0000 99 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0408882000 _diffrn_orient_matrix_UB_12 0.0762220000 _diffrn_orient_matrix_UB_13 -0.0076537000 _diffrn_orient_matrix_UB_21 0.1889804000 _diffrn_orient_matrix_UB_22 -0.0154401000 _diffrn_orient_matrix_UB_23 0.0107340000 _diffrn_orient_matrix_UB_31 0.0197654000 _diffrn_orient_matrix_UB_32 -0.0101630000 _diffrn_orient_matrix_UB_33 -0.0731274000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_number_gt 5745 _reflns_number_total 6454 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.617 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.068 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 445 _refine_ls_number_reflns 6454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0478 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+5.3052P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1268 _refine_ls_wR_factor_ref 0.1303 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.59953(5) 0.63587(2) 0.73378(2) 0.01648(12) Uani 1 1 d . A . Cl1 Cl 0.622(3) 0.5302(8) 1.0050(6) 0.217(9) Uani 0.274(13) 1 d P . . Cl2 Cl 0.733(4) 0.5358(8) 0.9763(14) 0.206(14) Uani 0.195(15) 1 d P . . Cl3 Cl 0.991(7) 0.490(2) 0.9620(12) 0.175(18) Uani 0.151(16) 1 d P . . Cl4 Cl 0.885(4) 0.5133(13) 0.9589(14) 0.083(13) Uani 0.072(16) 1 d P . . F1 F 0.2275(3) 0.71638(10) 0.89742(10) 0.0435(5) Uani 1 1 d . . . F2 F 0.4608(3) 0.68467(12) 0.94154(9) 0.0446(5) Uani 1 1 d . . . F3 F 0.2413(3) 0.62159(11) 0.94890(10) 0.0456(5) Uani 1 1 d . . . O1 O 0.4535(2) 0.66827(9) 0.80914(9) 0.0217(4) Uani 1 1 d . . . O2 O 0.4407(2) 0.55231(9) 0.73134(9) 0.0204(4) Uani 1 1 d . . . O3 O 0.8891(4) 0.5857(2) 0.80212(18) 0.0464(12) Uani 0.716(8) 1 d P A 1 O3A O 0.7522(14) 0.5638(7) 0.8385(5) 0.064(4) Uani 0.284(8) 1 d P A 2 N1 N 0.7310(3) 0.72859(11) 0.72469(11) 0.0180(4) Uani 1 1 d . . . N1S N 0.4576(5) 0.60631(16) 0.44878(16) 0.0466(8) Uani 1 1 d . . . N2 N 0.7526(3) 0.75506(11) 0.66404(11) 0.0181(4) Uani 1 1 d . . . N3 N 0.7260(3) 0.59993(11) 0.65182(11) 0.0179(4) Uani 1 1 d . . . N4 N 0.7522(3) 0.64420(11) 0.60144(11) 0.0180(4) Uani 1 1 d . . . N5 N 0.4216(3) 0.68323(11) 0.66429(11) 0.0177(4) Uani 1 1 d . . . N6 N 0.4881(3) 0.71366(11) 0.61073(11) 0.0184(5) Uani 1 1 d . . . N7 N 0.7504(3) 0.59741(12) 0.78958(12) 0.0253(5) Uani 1 1 d . . . C1 C 0.8340(3) 0.81564(13) 0.66902(14) 0.0222(6) Uani 1 1 d . . . C1S C 0.4095(4) 0.58483(16) 0.49626(17) 0.0326(7) Uani 1 1 d . . . C2 C 0.8668(4) 0.82781(14) 0.73376(15) 0.0261(6) Uani 1 1 d . . . H2 H 0.9232 0.8662 0.7519 0.031 Uiso 1 1 calc R . . C2S C 0.3489(4) 0.55647(16) 0.55631(16) 0.0334(7) Uani 1 1 d . . . H2SA H 0.3204 0.5083 0.5499 0.050 Uiso 1 1 calc R . . H2SB H 0.2483 0.5814 0.5696 0.050 Uiso 1 1 calc R . . H2SC H 0.4371 0.5605 0.5899 0.050 Uiso 1 1 calc R . . C3 C 0.8003(3) 0.77236(14) 0.76729(14) 0.0217(6) Uani 1 1 d . . . C4 C 0.3625(4) 0.74004(14) 0.57302(14) 0.0222(6) Uani 1 1 d . . . C5 C 0.2132(4) 0.72603(15) 0.60262(14) 0.0244(6) Uani 1 1 d . . . H5 H 0.1033 0.7380 0.5875 0.029 Uiso 1 1 calc R . . C6 C 0.2542(3) 0.69085(14) 0.65928(14) 0.0220(6) Uani 1 1 d . . . C7 C 0.8392(3) 0.61223(14) 0.55486(13) 0.0204(5) Uani 1 1 d . . . C8 C 0.8707(4) 0.54629(14) 0.57551(14) 0.0233(6) Uani 1 1 d . . . H8 H 0.9294 0.5119 0.5528 0.028 Uiso 1 1 calc R . . C9 C 0.7990(3) 0.54039(13) 0.63621(14) 0.0209(5) Uani 1 1 d . . . C10 C 0.8713(4) 0.85998(15) 0.61239(16) 0.0304(7) Uani 1 1 d . . . H10A H 0.9340 0.8338 0.5806 0.046 Uiso 1 1 calc R . . H10B H 0.9391 0.8991 0.6267 0.046 Uiso 1 1 calc R . . H10C H 0.7652 0.8762 0.5928 0.046 Uiso 1 1 calc R . . C11 C 0.8033(4) 0.75951(16) 0.83810(15) 0.0306(7) Uani 1 1 d . . . H11A H 0.6905 0.7461 0.8518 0.046 Uiso 1 1 calc R . . H11B H 0.8381 0.8011 0.8609 0.046 Uiso 1 1 calc R . . H11C H 0.8834 0.7229 0.8482 0.046 Uiso 1 1 calc R . . C12 C 0.1349(4) 0.66415(17) 0.70790(16) 0.0298(7) Uani 1 1 d . . . H12A H 0.1492 0.6148 0.7120 0.045 Uiso 1 1 calc R . . H12B H 0.0189 0.6743 0.6939 0.045 Uiso 1 1 calc R . . H12C H 0.1583 0.6859 0.7497 0.045 Uiso 1 1 calc R . . C13 C 0.3938(4) 0.77718(16) 0.51160(15) 0.0301(7) Uani 1 1 d . . . H13A H 0.4586 0.8186 0.5209 0.045 Uiso 1 1 calc R . . H13B H 0.2858 0.7894 0.4910 0.045 Uiso 1 1 calc R . . H13C H 0.4576 0.7479 0.4826 0.045 Uiso 1 1 calc R . . C14 C 0.8851(4) 0.64500(16) 0.49274(14) 0.0279(6) Uani 1 1 d . . . H14A H 0.7835 0.6636 0.4717 0.042 Uiso 1 1 calc R . . H14B H 0.9362 0.6111 0.4645 0.042 Uiso 1 1 calc R . . H14C H 0.9659 0.6818 0.5012 0.042 Uiso 1 1 calc R . . C15 C 0.7963(4) 0.47957(14) 0.67945(15) 0.0271(6) Uani 1 1 d . . . H15A H 0.9029 0.4768 0.7040 0.041 Uiso 1 1 calc R . . H15B H 0.7816 0.4383 0.6534 0.041 Uiso 1 1 calc R . . H15C H 0.7026 0.4837 0.7093 0.041 Uiso 1 1 calc R . . C16 C 0.3533(3) 0.52724(13) 0.77556(14) 0.0203(5) Uani 1 1 d . . . C17 C 0.3267(4) 0.56145(14) 0.83517(14) 0.0236(6) Uani 1 1 d . . . H17 H 0.2737 0.5374 0.8690 0.028 Uiso 1 1 calc R . . C18 C 0.3746(4) 0.62797(14) 0.84568(14) 0.0221(6) Uani 1 1 d . . . C19 C 0.2735(3) 0.45979(13) 0.76193(14) 0.0213(6) Uani 1 1 d . . . C20 C 0.2969(4) 0.43061(14) 0.70137(15) 0.0254(6) Uani 1 1 d . . . H20 H 0.3600 0.4543 0.6700 0.031 Uiso 1 1 calc R . . C21 C 0.2288(4) 0.36752(15) 0.68672(16) 0.0300(7) Uani 1 1 d . . . H21 H 0.2459 0.3480 0.6454 0.036 Uiso 1 1 calc R . . C22 C 0.1358(4) 0.33247(15) 0.73197(16) 0.0305(7) Uani 1 1 d . . . H22 H 0.0892 0.2891 0.7218 0.037 Uiso 1 1 calc R . . C23 C 0.1114(4) 0.36098(16) 0.79193(17) 0.0338(7) Uani 1 1 d . . . H23 H 0.0475 0.3371 0.8229 0.041 Uiso 1 1 calc R . . C24 C 0.1795(4) 0.42439(15) 0.80751(16) 0.0296(7) Uani 1 1 d . . . H24 H 0.1622 0.4436 0.8489 0.035 Uiso 1 1 calc R . . C25 C 0.3248(4) 0.66248(16) 0.90873(15) 0.0289(6) Uani 1 1 d . . . B1 B 0.6800(4) 0.71736(15) 0.60410(14) 0.0181(6) Uani 1 1 d . . . H1 H 0.7089 0.7427 0.5640 0.022 Uiso 1 1 calc R . . 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 0.0188(2) 0.01285(19) 0.0178(2) -0.00010(15) 0.00233(15) -0.00013(15) Cl1 0.31(2) 0.194(13) 0.149(9) 0.048(10) 0.083(13) 0.168(13) Cl2 0.27(3) 0.089(9) 0.26(2) -0.042(12) 0.10(2) -0.042(13) Cl3 0.18(4) 0.15(2) 0.19(2) 0.011(18) 0.03(2) -0.06(3) Cl4 0.07(2) 0.070(15) 0.11(2) -0.024(12) -0.011(13) 0.004(11) F1 0.0572(13) 0.0344(10) 0.0392(11) -0.0063(9) 0.0135(10) 0.0164(9) F2 0.0488(12) 0.0543(13) 0.0306(10) -0.0164(9) 0.0014(9) -0.0087(10) F3 0.0692(15) 0.0370(11) 0.0315(10) -0.0043(8) 0.0257(10) -0.0118(10) O1 0.0272(10) 0.0167(9) 0.0213(10) -0.0011(7) 0.0052(8) -0.0009(7) O2 0.0243(10) 0.0141(8) 0.0232(10) -0.0006(7) 0.0054(8) -0.0024(7) O3 0.028(2) 0.060(2) 0.051(2) 0.0159(18) -0.0056(15) 0.0044(16) O3A 0.055(7) 0.092(9) 0.044(6) 0.036(6) 0.000(5) 0.022(6) N1 0.0195(11) 0.0153(10) 0.0191(11) -0.0018(9) 0.0007(9) 0.0001(8) N1S 0.061(2) 0.0372(16) 0.0410(18) 0.0011(14) -0.0010(16) 0.0020(15) N2 0.0201(11) 0.0123(10) 0.0218(11) -0.0010(8) 0.0017(9) -0.0009(8) N3 0.0205(11) 0.0139(10) 0.0194(11) 0.0009(8) 0.0008(9) -0.0001(8) N4 0.0181(11) 0.0171(11) 0.0188(11) 0.0011(9) 0.0027(9) 0.0002(8) N5 0.0178(11) 0.0154(10) 0.0199(11) -0.0003(8) 0.0022(8) -0.0001(8) N6 0.0224(11) 0.0155(10) 0.0172(11) -0.0001(8) 0.0002(9) 0.0009(8) N7 0.0272(14) 0.0214(11) 0.0274(13) 0.0006(10) 0.0033(10) -0.0005(10) C1 0.0225(13) 0.0132(12) 0.0308(15) -0.0003(11) 0.0028(11) -0.0009(10) C1S 0.0338(17) 0.0244(15) 0.0393(19) -0.0077(14) -0.0066(14) 0.0046(12) C2 0.0281(15) 0.0184(13) 0.0317(16) -0.0051(11) -0.0005(12) -0.0030(11) C2S 0.0381(18) 0.0266(15) 0.0353(17) -0.0075(13) -0.0015(14) 0.0010(13) C3 0.0205(13) 0.0186(12) 0.0259(14) -0.0063(11) -0.0010(11) -0.0013(10) C4 0.0251(14) 0.0188(12) 0.0227(14) -0.0025(11) -0.0023(11) 0.0051(11) C5 0.0197(13) 0.0251(14) 0.0283(15) -0.0011(12) -0.0024(11) 0.0046(11) C6 0.0204(13) 0.0195(13) 0.0262(14) -0.0044(11) 0.0006(11) 0.0016(10) C7 0.0211(13) 0.0201(13) 0.0201(13) -0.0040(10) 0.0022(10) 0.0012(10) C8 0.0264(14) 0.0186(13) 0.0250(14) -0.0040(11) 0.0038(11) 0.0056(11) C9 0.0221(13) 0.0147(12) 0.0258(14) -0.0005(11) 0.0008(11) 0.0019(10) C10 0.0383(17) 0.0179(14) 0.0350(17) 0.0036(12) 0.0023(14) -0.0055(12) C11 0.0359(17) 0.0298(16) 0.0259(15) -0.0051(12) -0.0025(13) -0.0035(13) C12 0.0180(14) 0.0377(17) 0.0337(16) 0.0035(13) 0.0044(12) 0.0010(12) C13 0.0330(17) 0.0302(15) 0.0271(15) 0.0062(13) -0.0024(13) 0.0062(12) C14 0.0355(17) 0.0264(14) 0.0221(14) -0.0016(12) 0.0086(12) 0.0038(12) C15 0.0342(16) 0.0158(13) 0.0313(16) 0.0038(11) 0.0046(13) 0.0048(11) C16 0.0197(13) 0.0165(12) 0.0249(14) 0.0029(11) 0.0018(11) 0.0006(10) C17 0.0287(15) 0.0199(13) 0.0225(14) 0.0021(11) 0.0055(11) -0.0031(11) C18 0.0243(14) 0.0210(13) 0.0212(14) -0.0012(11) 0.0028(11) 0.0017(11) C19 0.0210(13) 0.0154(12) 0.0273(14) 0.0043(11) -0.0002(11) -0.0001(10) C20 0.0308(15) 0.0185(13) 0.0269(15) 0.0036(11) -0.0019(12) -0.0025(11) C21 0.0393(18) 0.0193(14) 0.0312(16) -0.0010(12) -0.0050(13) -0.0033(12) C22 0.0321(16) 0.0176(13) 0.0414(18) 0.0036(12) -0.0065(13) -0.0047(12) C23 0.0376(18) 0.0216(15) 0.0423(19) 0.0070(13) 0.0059(15) -0.0092(13) C24 0.0363(17) 0.0199(14) 0.0327(16) 0.0015(12) 0.0068(13) -0.0034(12) C25 0.0359(17) 0.0262(15) 0.0248(15) -0.0015(12) 0.0081(13) -0.0027(12) B1 0.0224(15) 0.0161(13) 0.0161(14) -0.0001(11) 0.0031(11) 0.0001(11) _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 2.0637(19) . ? Fe1 O2 2.0689(19) . ? Fe1 N1 2.109(2) . ? Fe1 N3 2.112(2) . ? Fe1 N5 2.203(2) . ? Fe1 N7 1.813(3) . ? Cl1 Cl1 2.28(5) 3_667 ? Cl1 Cl2 1.08(2) . ? Cl1 Cl4 2.34(4) . ? Cl2 Cl3 2.26(7) . ? Cl2 Cl4 1.34(5) . ? Cl3 Cl3 1.63(5) 3_767 ? Cl3 Cl4 1.90(6) 3_767 ? Cl3 Cl4 0.95(4) . ? Cl4 Cl3 1.90(6) 3_767 ? F1 C25 1.328(4) . ? F2 C25 1.337(4) . ? F3 C25 1.341(4) . ? O1 C18 1.269(3) . ? O2 C16 1.260(3) . ? O3 N7 1.148(4) . ? O3A N7 1.210(10) . ? N1 C3 1.342(3) . ? N1S C1S 1.143(5) . ? N2 N1 1.374(3) . ? N2 C1 1.357(3) . ? N2 B1 1.548(4) . ? N3 C9 1.347(3) . ? N4 N3 1.378(3) . ? N4 C7 1.353(3) . ? N4 B1 1.548(4) . ? N5 C6 1.338(4) . ? N6 N5 1.375(3) . ? N6 C4 1.357(4) . ? N6 B1 1.533(4) . ? C1 C2 1.383(4) . ? C1 C10 1.496(4) . ? C1S C2S 1.454(5) . ? C2 H2 0.9500 . ? C2 C3 1.401(4) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3 C11 1.489(4) . ? C4 C5 1.372(4) . ? C4 C13 1.492(4) . ? C5 H5 0.9500 . ? C5 C6 1.396(4) . ? C6 C12 1.491(4) . ? C7 C8 1.385(4) . ? C7 C14 1.491(4) . ? C8 H8 0.9500 . ? C8 C9 1.396(4) . ? C9 C15 1.494(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.426(4) . ? C16 C19 1.493(4) . ? C17 H17 0.9500 . ? C17 C18 1.377(4) . ? C18 C25 1.531(4) . ? C19 C20 1.396(4) . ? C19 C24 1.400(4) . ? C20 H20 0.9500 . ? C20 C21 1.383(4) . ? C21 H21 0.9500 . ? C21 C22 1.388(5) . ? C22 H22 0.9500 . ? C22 C23 1.380(5) . ? C23 H23 0.9500 . ? C23 C24 1.393(4) . ? C24 H24 0.9500 . ? B1 H1 1.0000 . ? 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 O2 84.98(8) . . ? O1 Fe1 N1 95.01(8) . . ? O1 Fe1 N3 174.21(9) . . ? O1 Fe1 N5 90.18(8) . . ? O2 Fe1 N1 169.98(8) . . ? O2 Fe1 N3 90.79(8) . . ? O2 Fe1 N5 86.39(8) . . ? N1 Fe1 N3 88.47(9) . . ? N1 Fe1 N5 83.59(8) . . ? N3 Fe1 N5 85.60(8) . . ? N7 Fe1 O1 91.07(10) . . ? N7 Fe1 O2 94.53(10) . . ? N7 Fe1 N1 95.49(10) . . ? N7 Fe1 N3 93.21(10) . . ? N7 Fe1 N5 178.51(10) . . ? Cl1 Cl1 Cl4 130.8(10) 3_667 . ? Cl2 Cl1 Cl1 135(2) . 3_667 ? Cl2 Cl1 Cl4 16.8(14) . . ? Cl1 Cl2 Cl3 141(2) . . ? Cl1 Cl2 Cl4 150(2) . . ? Cl4 Cl2 Cl3 8.9(16) . . ? Cl3 Cl3 Cl2 81(4) 3_767 . ? Cl3 Cl3 Cl4 30(2) 3_767 3_767 ? Cl4 Cl3 Cl2 111(2) 3_767 . ? Cl4 Cl3 Cl2 13(2) . . ? Cl4 Cl3 Cl3 91(5) . 3_767 ? Cl4 Cl3 Cl4 121(3) . 3_767 ? Cl2 Cl4 Cl1 13.4(11) . . ? Cl2 Cl4 Cl3 103(3) . 3_767 ? Cl3 Cl4 Cl1 146(3) . . ? Cl3 Cl4 Cl1 96(2) 3_767 . ? Cl3 Cl4 Cl2 159(4) . . ? Cl3 Cl4 Cl3 59(3) . 3_767 ? C18 O1 Fe1 123.38(17) . . ? C16 O2 Fe1 129.45(18) . . ? N2 N1 Fe1 118.63(16) . . ? C3 N1 Fe1 133.71(19) . . ? C3 N1 N2 107.6(2) . . ? N1 N2 B1 120.2(2) . . ? C1 N2 N1 109.3(2) . . ? C1 N2 B1 130.5(2) . . ? N4 N3 Fe1 118.69(16) . . ? C9 N3 Fe1 134.16(19) . . ? C9 N3 N4 107.1(2) . . ? N3 N4 B1 119.8(2) . . ? C7 N4 N3 109.6(2) . . ? C7 N4 B1 130.6(2) . . ? N6 N5 Fe1 117.42(16) . . ? C6 N5 Fe1 136.04(19) . . ? C6 N5 N6 106.5(2) . . ? N5 N6 B1 119.4(2) . . ? C4 N6 N5 110.0(2) . . ? C4 N6 B1 130.5(2) . . ? O3 N7 Fe1 147.7(3) . . ? O3 N7 O3A 72.9(6) . . ? O3A N7 Fe1 139.4(6) . . ? N2 C1 C2 107.8(2) . . ? N2 C1 C10 123.5(3) . . ? C2 C1 C10 128.7(3) . . ? N1S C1S C2S 179.1(4) . . ? C1 C2 H2 126.8 . . ? C1 C2 C3 106.4(2) . . ? C3 C2 H2 126.8 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SB 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? N1 C3 C2 108.9(2) . . ? N1 C3 C11 122.6(3) . . ? C2 C3 C11 128.5(3) . . ? N6 C4 C5 107.2(2) . . ? N6 C4 C13 123.0(3) . . ? C5 C4 C13 129.7(3) . . ? C4 C5 H5 126.7 . . ? C4 C5 C6 106.7(3) . . ? C6 C5 H5 126.7 . . ? N5 C6 C5 109.6(3) . . ? N5 C6 C12 123.4(3) . . ? C5 C6 C12 127.1(3) . . ? N4 C7 C8 107.7(2) . . ? N4 C7 C14 123.6(2) . . ? C8 C7 C14 128.7(3) . . ? C7 C8 H8 126.8 . . ? C7 C8 C9 106.4(2) . . ? C9 C8 H8 126.8 . . ? N3 C9 C8 109.2(2) . . ? N3 C9 C15 122.6(3) . . ? C8 C9 C15 128.2(3) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C4 C13 H13A 109.5 . . ? C4 C13 H13B 109.5 . . ? C4 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 C17 122.6(2) . . ? O2 C16 C19 116.5(2) . . ? C17 C16 C19 120.9(2) . . ? C16 C17 H17 118.7 . . ? C18 C17 C16 122.6(3) . . ? C18 C17 H17 118.7 . . ? O1 C18 C17 129.4(3) . . ? O1 C18 C25 111.8(2) . . ? C17 C18 C25 118.7(3) . . ? C20 C19 C16 118.1(2) . . ? C20 C19 C24 119.0(3) . . ? C24 C19 C16 122.8(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20 119.8 . . ? C20 C21 H21 119.8 . . ? C20 C21 C22 120.4(3) . . ? C22 C21 H21 119.8 . . ? C21 C22 H22 120.2 . . ? C23 C22 C21 119.6(3) . . ? C23 C22 H22 120.2 . . ? C22 C23 H23 119.6 . . ? C22 C23 C24 120.7(3) . . ? C24 C23 H23 119.6 . . ? C19 C24 H24 120.1 . . ? C23 C24 C19 119.8(3) . . ? C23 C24 H24 120.1 . . ? F1 C25 F2 106.9(3) . . ? F1 C25 F3 107.1(3) . . ? F1 C25 C18 111.2(2) . . ? F2 C25 F3 106.4(3) . . ? F2 C25 C18 111.1(3) . . ? F3 C25 C18 113.8(2) . . ? N2 B1 N4 109.9(2) . . ? N2 B1 H1 110.0 . . ? N4 B1 H1 110.0 . . ? N6 B1 N2 107.8(2) . . ? N6 B1 N4 109.1(2) . . ? N6 B1 H1 110.0 . . ? 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 Fe1 O1 C18 C17 -20.4(4) . . . . ? Fe1 O1 C18 C25 161.77(19) . . . . ? Fe1 O2 C16 C17 11.5(4) . . . . ? Fe1 O2 C16 C19 -170.10(17) . . . . ? Fe1 N1 C3 C2 -177.7(2) . . . . ? Fe1 N1 C3 C11 3.3(4) . . . . ? Fe1 N3 C9 C8 -177.6(2) . . . . ? Fe1 N3 C9 C15 3.1(4) . . . . ? Fe1 N5 C6 C5 -179.6(2) . . . . ? Fe1 N5 C6 C12 -0.2(4) . . . . ? Cl1 Cl1 Cl2 Cl3 -90(4) 3_667 . . . ? Cl1 Cl1 Cl2 Cl4 -84(6) 3_667 . . . ? Cl1 Cl1 Cl4 Cl2 111(6) 3_667 . . . ? Cl1 Cl1 Cl4 Cl3 -84(5) 3_667 . . . ? Cl1 Cl1 Cl4 Cl3 -124.0(15) 3_667 . . 3_767 ? Cl1 Cl2 Cl3 Cl3 -58(4) . . . 3_767 ? Cl1 Cl2 Cl3 Cl4 -54(4) . . . 3_767 ? Cl1 Cl2 Cl3 Cl4 161(9) . . . . ? Cl1 Cl2 Cl4 Cl3 -23(12) . . . . ? Cl1 Cl2 Cl4 Cl3 -57(6) . . . 3_767 ? Cl2 Cl1 Cl4 Cl3 165(8) . . . . ? Cl2 Cl1 Cl4 Cl3 125(6) . . . 3_767 ? Cl2 Cl3 Cl4 Cl1 -9(5) . . . . ? Cl2 Cl3 Cl4 Cl3 39(9) . . . 3_767 ? Cl3 Cl2 Cl4 Cl1 23(12) . . . . ? Cl3 Cl2 Cl4 Cl3 -34(8) . . . 3_767 ? Cl3 Cl3 Cl4 Cl1 -48(5) 3_767 . . . ? Cl3 Cl3 Cl4 Cl2 -39(9) 3_767 . . . ? Cl4 Cl1 Cl2 Cl3 -6(3) . . . . ? Cl4 Cl2 Cl3 Cl3 140(9) . . . 3_767 ? Cl4 Cl2 Cl3 Cl4 145(8) . . . 3_767 ? Cl4 Cl3 Cl4 Cl1 -48(5) 3_767 . . . ? Cl4 Cl3 Cl4 Cl2 -39(9) 3_767 . . . ? Cl4 Cl3 Cl4 Cl3 0.001(7) 3_767 . . 3_767 ? O1 Fe1 O2 C16 -24.5(2) . . . . ? O1 Fe1 N1 N2 -134.80(18) . . . . ? O1 Fe1 N1 C3 42.9(3) . . . . ? O1 Fe1 N3 N4 88.0(8) . . . . ? O1 Fe1 N3 C9 -95.2(8) . . . . ? O1 Fe1 N5 N6 142.67(17) . . . . ? O1 Fe1 N5 C6 -37.7(3) . . . . ? O1 Fe1 N7 O3 -142.4(5) . . . . ? O1 Fe1 N7 O3A 42.0(10) . . . . ? O1 C18 C25 F1 59.0(3) . . . . ? O1 C18 C25 F2 -59.8(3) . . . . ? O1 C18 C25 F3 -179.9(3) . . . . ? O2 Fe1 O1 C18 27.3(2) . . . . ? O2 Fe1 N1 N2 -45.3(6) . . . . ? O2 Fe1 N1 C3 132.5(4) . . . . ? O2 Fe1 N3 N4 131.05(18) . . . . ? O2 Fe1 N3 C9 -52.2(3) . . . . ? O2 Fe1 N5 N6 -132.37(17) . . . . ? O2 Fe1 N5 C6 47.2(3) . . . . ? O2 Fe1 N7 O3 132.5(5) . . . . ? O2 Fe1 N7 O3A -43.0(10) . . . . ? O2 C16 C17 C18 9.1(4) . . . . ? O2 C16 C19 C20 -1.9(4) . . . . ? O2 C16 C19 C24 177.0(3) . . . . ? N1 Fe1 O1 C18 -162.7(2) . . . . ? N1 Fe1 O2 C16 -114.9(5) . . . . ? N1 Fe1 N3 N4 -38.95(19) . . . . ? N1 Fe1 N3 C9 137.8(3) . . . . ? N1 Fe1 N5 N6 47.64(17) . . . . ? N1 Fe1 N5 C6 -132.8(3) . . . . ? N1 Fe1 N7 O3 -47.3(5) . . . . ? N1 Fe1 N7 O3A 137.2(10) . . . . ? N1 N2 C1 C2 0.7(3) . . . . ? N1 N2 C1 C10 -177.1(3) . . . . ? N1 N2 B1 N4 -57.5(3) . . . . ? N1 N2 B1 N6 61.3(3) . . . . ? N2 N1 C3 C2 0.2(3) . . . . ? N2 N1 C3 C11 -178.8(3) . . . . ? N2 C1 C2 C3 -0.5(3) . . . . ? N3 Fe1 O1 C18 70.6(9) . . . . ? N3 Fe1 O2 C16 159.4(2) . . . . ? N3 Fe1 N1 N2 40.56(18) . . . . ? N3 Fe1 N1 C3 -141.7(3) . . . . ? N3 Fe1 N5 N6 -41.30(17) . . . . ? N3 Fe1 N5 C6 138.3(3) . . . . ? N3 Fe1 N7 O3 41.5(5) . . . . ? N3 Fe1 N7 O3A -134.1(10) . . . . ? N3 N4 C7 C8 -0.3(3) . . . . ? N3 N4 C7 C14 178.4(3) . . . . ? N3 N4 B1 N2 59.2(3) . . . . ? N3 N4 B1 N6 -58.7(3) . . . . ? N4 N3 C9 C8 -0.6(3) . . . . ? N4 N3 C9 C15 -179.9(3) . . . . ? N4 C7 C8 C9 -0.1(3) . . . . ? N5 Fe1 O1 C18 113.7(2) . . . . ? N5 Fe1 O2 C16 -115.0(2) . . . . ? N5 Fe1 N1 N2 -45.18(18) . . . . ? N5 Fe1 N1 C3 132.6(3) . . . . ? N5 Fe1 N3 N4 44.74(18) . . . . ? N5 Fe1 N3 C9 -138.5(3) . . . . ? N5 Fe1 N7 O3 4(4) . . . . ? N5 Fe1 N7 O3A -171(4) . . . . ? N5 N6 C4 C5 -0.3(3) . . . . ? N5 N6 C4 C13 179.3(2) . . . . ? N5 N6 B1 N2 -57.4(3) . . . . ? N5 N6 B1 N4 61.9(3) . . . . ? N6 N5 C6 C5 0.1(3) . . . . ? N6 N5 C6 C12 179.5(3) . . . . ? N6 C4 C5 C6 0.3(3) . . . . ? N7 Fe1 O1 C18 -67.1(2) . . . . ? N7 Fe1 O2 C16 66.1(2) . . . . ? N7 Fe1 N1 N2 133.64(19) . . . . ? N7 Fe1 N1 C3 -48.6(3) . . . . ? N7 Fe1 N3 N4 -134.36(19) . . . . ? N7 Fe1 N3 C9 42.4(3) . . . . ? N7 Fe1 N5 N6 -4(4) . . . . ? N7 Fe1 N5 C6 175(100) . . . . ? C1 N2 N1 Fe1 177.72(17) . . . . ? C1 N2 N1 C3 -0.6(3) . . . . ? C1 N2 B1 N4 125.9(3) . . . . ? C1 N2 B1 N6 -115.2(3) . . . . ? C1 C2 C3 N1 0.2(3) . . . . ? C1 C2 C3 C11 179.1(3) . . . . ? C4 N6 N5 Fe1 179.86(17) . . . . ? C4 N6 N5 C6 0.2(3) . . . . ? C4 N6 B1 N2 117.9(3) . . . . ? C4 N6 B1 N4 -122.8(3) . . . . ? C4 C5 C6 N5 -0.2(3) . . . . ? C4 C5 C6 C12 -179.6(3) . . . . ? C7 N4 N3 Fe1 178.09(17) . . . . ? C7 N4 N3 C9 0.5(3) . . . . ? C7 N4 B1 N2 -122.8(3) . . . . ? C7 N4 B1 N6 119.2(3) . . . . ? C7 C8 C9 N3 0.4(3) . . . . ? C7 C8 C9 C15 179.6(3) . . . . ? C10 C1 C2 C3 177.2(3) . . . . ? C13 C4 C5 C6 -179.2(3) . . . . ? C14 C7 C8 C9 -178.6(3) . . . . ? C16 C17 C18 O1 -3.8(5) . . . . ? C16 C17 C18 C25 173.9(3) . . . . ? C16 C19 C20 C21 178.6(3) . . . . ? C16 C19 C24 C23 -178.7(3) . . . . ? C17 C16 C19 C20 176.6(3) . . . . ? C17 C16 C19 C24 -4.6(4) . . . . ? C17 C18 C25 F1 -119.1(3) . . . . ? C17 C18 C25 F2 122.1(3) . . . . ? C17 C18 C25 F3 2.0(4) . . . . ? C19 C16 C17 C18 -169.3(3) . . . . ? C19 C20 C21 C22 0.3(5) . . . . ? C20 C19 C24 C23 0.1(5) . . . . ? C20 C21 C22 C23 0.0(5) . . . . ? C21 C22 C23 C24 -0.2(5) . . . . ? C22 C23 C24 C19 0.1(5) . . . . ? C24 C19 C20 C21 -0.3(4) . . . . ? B1 N2 N1 Fe1 0.5(3) . . . . ? B1 N2 N1 C3 -177.8(2) . . . . ? B1 N2 C1 C2 177.5(3) . . . . ? B1 N2 C1 C10 -0.3(5) . . . . ? B1 N4 N3 Fe1 -3.5(3) . . . . ? B1 N4 N3 C9 178.9(2) . . . . ? B1 N4 C7 C8 -178.4(3) . . . . ? B1 N4 C7 C14 0.3(5) . . . . ? B1 N6 N5 Fe1 -3.9(3) . . . . ? B1 N6 N5 C6 176.4(2) . . . . ? B1 N6 C4 C5 -176.0(3) . . . . ? B1 N6 C4 C13 3.6(4) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 1 -13 0.0248 0.0000 1.0002 -12.9996 0.1757 -0.1550 0.9405 0 -1 13 0.0248 -0.0000 -1.0002 12.9996 -0.1757 0.1550 -0.9405 5 -1 -1 0.1499 5.0000 -1.0001 -1.0002 0.1359 0.9496 0.1821 -5 1 1 0.1499 -5.0000 1.0001 1.0002 -0.1359 -0.9496 -0.1821 0 13 0 0.0852 0.0000 13.0002 0.0003 0.9909 -0.2007 -0.1321 0 -13 0 0.0852 -0.0000 -13.0002 -0.0003 -0.9909 0.2007 0.1321 #===END data_5acacPhF3 _audit_creation_date 2012-04-11 _audit_creation_method ; Olex2 1.1-beta (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.5(C116 H128 B4 Fe6 N24 O20), 1.49(C4 H6 N2)' _chemical_formula_sum 'C63.96 H72.94 B2 Fe3 N14.98 O10' _chemical_formula_weight 1400.78 _chemical_melting_point ? _chemical_oxdiff_formula 'Fe3 (C7 H5 O2)4 (C15 H22 N6 B)2 O2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'orthorhombic' _space_group_IT_number 62 _space_group_name_H-M_alt 'P n m a' _space_group_name_Hall '-P 2ac 2n' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z+1/2' 3 'x+1/2, -y+1/2, -z+1/2' 4 '-x, y+1/2, -z' 5 '-x, -y, -z' 6 'x-1/2, y, -z-1/2' 7 '-x-1/2, y-1/2, z-1/2' 8 'x, -y-1/2, z' _cell_length_a 15.8198(10) _cell_length_b 22.6357(16) _cell_length_c 19.1610(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6861.4(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4277 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 74.0111 _cell_measurement_theta_min 3.4057 _exptl_absorpt_coefficient_mu 5.568 _exptl_absorpt_correction_T_max 0.821 _exptl_absorpt_correction_T_min 0.606 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 2918 _exptl_crystal_size_max 0.1452 _exptl_crystal_size_mid 0.0865 _exptl_crystal_size_min 0.0374 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_unetI/netI 0.0510 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 22926 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 74.18 _diffrn_reflns_theta_min 3.62 _diffrn_ambient_temperature 100.00(10) _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -49.00 -7.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 37.0000 -60.0000 42 #__ type_ start__ end____ width___ exp.time_ 2 omega -81.00 40.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 19.0000 -150.0000 121 #__ type_ start__ end____ width___ exp.time_ 3 omega 63.00 90.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 150.0000 27 #__ type_ start__ end____ width___ exp.time_ 4 omega 32.00 86.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -45.0000 150.0000 54 #__ type_ start__ end____ width___ exp.time_ 5 omega 102.00 160.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 98.0000 -145.0000 58 #__ type_ start__ end____ width___ exp.time_ 6 omega 39.00 94.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -45.0000 -90.0000 55 #__ type_ start__ end____ width___ exp.time_ 7 omega 30.00 88.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 -30.0000 58 #__ type_ start__ end____ width___ exp.time_ 8 omega 42.00 94.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -45.0000 90.0000 52 #__ type_ start__ end____ width___ exp.time_ 9 omega -115.00 -62.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -57.0000 -120.0000 53 #__ type_ start__ end____ width___ exp.time_ 10 omega -117.00 -14.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -37.0000 120.0000 103 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0426956000 _diffrn_orient_matrix_UB_12 -0.0607129000 _diffrn_orient_matrix_UB_13 -0.0089184000 _diffrn_orient_matrix_UB_21 -0.0400755000 _diffrn_orient_matrix_UB_22 0.0210446000 _diffrn_orient_matrix_UB_23 -0.0689116000 _diffrn_orient_matrix_UB_31 0.0778123000 _diffrn_orient_matrix_UB_32 -0.0224688000 _diffrn_orient_matrix_UB_33 -0.0404303000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_number_gt 5088 _reflns_number_total 6955 _reflns_odcompleteness_completeness 99.93 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 2.137 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.111 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 467 _refine_ls_number_reflns 6955 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0781 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1247P)^2^+8.1178P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2048 _refine_ls_wR_factor_ref 0.2255 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.56231(6) 0.2500 0.16106(4) 0.0258(2) Uani 1 2 d S . . Fe2 Fe 0.69058(6) 0.2500 -0.17613(5) 0.0270(2) Uani 1 2 d S . . Fe3 Fe 0.62858(6) 0.2500 -0.00639(6) 0.0378(3) Uani 1 2 d S . . O1 O 0.49500(18) 0.31484(14) 0.11413(15) 0.0326(7) Uani 1 1 d . E . O2 O 0.5380(2) 0.31541(15) 0.00231(15) 0.0360(7) Uani 1 1 d . E . O3 O 0.75868(18) 0.31513(13) -0.12933(15) 0.0318(7) Uani 1 1 d . . . O4 O 0.7207(2) 0.31405(16) -0.01623(15) 0.0390(8) Uani 1 1 d . . . O5 O 0.6463(2) 0.2500 0.0932(2) 0.0269(8) Uani 1 2 d S . . O6 O 0.6085(2) 0.2500 -0.1063(2) 0.0291(9) Uani 1 2 d S . . N1 N 0.4790(3) 0.2500 0.3073(3) 0.0310(11) Uani 1 2 d S . . N2 N 0.4594(3) 0.2500 0.2385(3) 0.0283(11) Uani 1 2 d S . . N3 N 0.6154(2) 0.30511(17) 0.29930(18) 0.0316(8) Uani 1 1 d . . . N4 N 0.6183(2) 0.31385(17) 0.22836(17) 0.0295(8) Uani 1 1 d . . . N5 N 0.7662(3) 0.2500 -0.3257(3) 0.0345(12) Uani 1 2 d S . . N6 N 0.7899(3) 0.2500 -0.2559(3) 0.0302(11) Uani 1 2 d S . . N7 N 0.6302(2) 0.3054(2) -0.31295(18) 0.0365(9) Uani 1 1 d . . . N8 N 0.6323(2) 0.31378(18) -0.24234(18) 0.0320(8) Uani 1 1 d . . . C1 C 0.4073(4) 0.2500 0.3460(3) 0.0393(15) Uani 1 2 d S . . C2 C 0.3403(4) 0.2500 0.3011(4) 0.0428(16) Uani 1 2 d S . . H2 H 0.2820 0.2500 0.3132 0.051 Uiso 1 2 calc SR . . C3 C 0.3746(4) 0.2500 0.2335(4) 0.0346(14) Uani 1 2 d S . . C4 C 0.6549(3) 0.3507(2) 0.3316(2) 0.0392(11) Uani 1 1 d . . . C5 C 0.6835(3) 0.3886(2) 0.2813(3) 0.0415(11) Uani 1 1 d . . . H5 H 0.7141 0.4242 0.2885 0.050 Uiso 1 1 calc R . . C6 C 0.6587(3) 0.3646(2) 0.2172(2) 0.0342(10) Uani 1 1 d . . . C7 C 0.4079(5) 0.2500 0.4249(4) 0.059(2) Uani 1 2 d S . . H7A H 0.4372 0.2147 0.4418 0.088 Uiso 0.50 1 calc PR A -1 H7B H 0.3496 0.2500 0.4422 0.088 Uiso 0.50 1 calc PR A -1 H7C H 0.4372 0.2854 0.4418 0.088 Uiso 0.50 1 calc PR A -1 C8 C 0.3294(4) 0.2500 0.1658(4) 0.0476(18) Uani 1 2 d S . . H8A H 0.3450 0.2854 0.1392 0.071 Uiso 0.50 1 calc PR B -1 H8B H 0.2683 0.2500 0.1741 0.071 Uiso 0.50 1 calc PR B -1 H8C H 0.3450 0.2147 0.1392 0.071 Uiso 0.50 1 calc PR B -1 C9 C 0.6625(4) 0.3545(3) 0.4094(2) 0.0487(13) Uani 1 1 d . . . H9A H 0.6059 0.3555 0.4302 0.073 Uiso 1 1 calc R . . H9B H 0.6932 0.3905 0.4220 0.073 Uiso 1 1 calc R . . H9C H 0.6932 0.3200 0.4269 0.073 Uiso 1 1 calc R . . C10 C 0.6712(4) 0.3891(2) 0.1457(3) 0.0503(14) Uani 1 1 d . . . H10A H 0.7036 0.3609 0.1175 0.076 Uiso 1 1 calc R . . H10B H 0.7021 0.4265 0.1487 0.076 Uiso 1 1 calc R . . H10C H 0.6160 0.3960 0.1238 0.076 Uiso 1 1 calc R . . C11 C 0.8359(4) 0.2500 -0.3656(4) 0.0441(17) Uani 1 2 d S . . C12 C 0.9050(4) 0.2500 -0.3219(4) 0.054(2) Uani 1 2 d S . . H12 H 0.9628 0.2500 -0.3353 0.065 Uiso 1 2 calc SR . . C13 C 0.8735(4) 0.2500 -0.2549(4) 0.0411(16) Uani 1 2 d S . . C14 C 0.5877(3) 0.3500(3) -0.3433(2) 0.0467(13) Uani 1 1 d . . . C15 C 0.5603(4) 0.3882(3) -0.2921(3) 0.0529(15) Uani 1 1 d . . . H15 H 0.5276 0.4230 -0.2981 0.063 Uiso 1 1 calc R . . C16 C 0.5913(3) 0.3646(2) -0.2292(2) 0.0413(12) Uani 1 1 d . . . C17 C 0.8333(5) 0.2500 -0.4439(4) 0.063(2) Uani 1 2 d S . . H17A H 0.8035 0.2147 -0.4602 0.094 Uiso 0.50 1 calc PR C -1 H17B H 0.8911 0.2500 -0.4623 0.094 Uiso 0.50 1 calc PR C -1 H17C H 0.8035 0.2854 -0.4602 0.094 Uiso 0.50 1 calc PR C -1 C18 C 0.9215(5) 0.2500 -0.1879(4) 0.058(2) Uani 1 2 d S . . H18A H 0.9068 0.2853 -0.1610 0.086 Uiso 0.50 1 calc PR D -1 H18B H 0.9823 0.2500 -0.1978 0.086 Uiso 0.50 1 calc PR D -1 H18C H 0.9068 0.2146 -0.1610 0.086 Uiso 0.50 1 calc PR D -1 C19 C 0.5730(4) 0.3535(3) -0.4210(3) 0.0648(18) Uani 1 1 d . . . H19A H 0.6276 0.3548 -0.4452 0.097 Uiso 1 1 calc R . . H19B H 0.5409 0.3894 -0.4318 0.097 Uiso 1 1 calc R . . H19C H 0.5412 0.3188 -0.4364 0.097 Uiso 1 1 calc R . . C20 C 0.5828(4) 0.3895(3) -0.1575(3) 0.0586(16) Uani 1 1 d . . . H20A H 0.5528 0.3612 -0.1277 0.088 Uiso 1 1 calc R . . H20B H 0.5508 0.4266 -0.1596 0.088 Uiso 1 1 calc R . . H20C H 0.6390 0.3972 -0.1382 0.088 Uiso 1 1 calc R . . C21 C 0.4964(3) 0.33549(19) 0.0527(2) 0.0291(9) Uani 1 1 d . . . C22A C 0.4497(9) 0.3928(6) 0.0392(6) 0.037(4) Uiso 0.50 1 d PD E 1 C23A C 0.3821(7) 0.4085(5) 0.0803(7) 0.054(3) Uiso 0.50 1 d PD E 1 H23A H 0.3656 0.3833 0.1176 0.064 Uiso 0.50 1 calc PR E 1 C24A C 0.3369(8) 0.4611(6) 0.0685(8) 0.063(4) Uiso 0.50 1 d PD E 1 H24A H 0.2891 0.4704 0.0965 0.075 Uiso 0.50 1 calc PR E 1 C25A C 0.3619(9) 0.4992(6) 0.0162(6) 0.059(3) Uiso 0.50 1 d PD E 1 H25A H 0.3346 0.5362 0.0099 0.070 Uiso 0.50 1 calc PR E 1 C26A C 0.4253(9) 0.4829(6) -0.0254(7) 0.072(4) Uiso 0.50 1 d PD E 1 H26A H 0.4396 0.5076 -0.0638 0.086 Uiso 0.50 1 calc PR E 1 C27A C 0.4729(8) 0.4297(5) -0.0147(6) 0.060(3) Uiso 0.50 1 d PD E 1 H27A H 0.5193 0.4201 -0.0441 0.072 Uiso 0.50 1 calc PR E 1 C22B C 0.4349(9) 0.3858(6) 0.0440(6) 0.041(4) Uiso 0.50 1 d PD E 2 C23B C 0.4049(6) 0.4166(4) 0.1017(5) 0.033(2) Uiso 0.50 1 d PD E 2 H23B H 0.4192 0.4033 0.1473 0.039 Uiso 0.50 1 calc PR E 2 C24B C 0.3545(7) 0.4664(5) 0.0941(6) 0.048(3) Uiso 0.50 1 d PD E 2 H24B H 0.3345 0.4874 0.1338 0.058 Uiso 0.50 1 calc PR E 2 C25B C 0.3340(8) 0.4850(6) 0.0266(6) 0.050(3) Uiso 0.50 1 d PD E 2 H25B H 0.2976 0.5180 0.0201 0.060 Uiso 0.50 1 calc PR E 2 C26B C 0.3655(7) 0.4564(5) -0.0292(6) 0.058(3) Uiso 0.50 1 d PD E 2 H26B H 0.3520 0.4707 -0.0745 0.070 Uiso 0.50 1 calc PR E 2 C27B C 0.4183(7) 0.4054(5) -0.0234(5) 0.046(2) Uiso 0.50 1 d PD E 2 H27B H 0.4407 0.3859 -0.0633 0.055 Uiso 0.50 1 calc PR E 2 C28 C 0.7605(2) 0.33471(19) -0.0673(2) 0.0286(9) Uani 1 1 d . . . C29 C 0.8143(3) 0.3883(2) -0.0552(3) 0.0388(11) Uani 1 1 d . . . C30 C 0.8412(4) 0.4221(2) -0.1119(3) 0.0521(13) Uani 1 1 d . . . H30 H 0.8282 0.4095 -0.1579 0.063 Uiso 1 1 calc R . . C31 C 0.8863(4) 0.4733(3) -0.1020(4) 0.0625(16) Uani 1 1 d . . . H31 H 0.9055 0.4957 -0.1408 0.075 Uiso 1 1 calc R . . C32 C 0.9032(4) 0.4917(3) -0.0345(4) 0.0657(17) Uani 1 1 d . . . H32 H 0.9329 0.5276 -0.0271 0.079 Uiso 1 1 calc R . . C33 C 0.8779(4) 0.4588(4) 0.0216(4) 0.071(2) Uani 1 1 d . . . H33 H 0.8917 0.4710 0.0676 0.085 Uiso 1 1 calc R . . C34 C 0.8314(4) 0.4072(3) 0.0107(3) 0.0566(15) Uani 1 1 d . . . H34 H 0.8116 0.3851 0.0495 0.068 Uiso 1 1 calc R . . B1 B 0.5697(4) 0.2500 0.3285(3) 0.0202(12) Uani 1 2 d S . . H1 H 0.5737 0.2500 0.3806 0.024 Uiso 1 2 calc SR . . B2 B 0.6762(4) 0.2500 -0.3441(3) 0.0258(13) Uani 1 2 d S . . H2A H 0.6700 0.2500 -0.3960 0.031 Uiso 1 2 calc SR . . N1S N 0.8408(5) 0.4820(4) 0.2221(5) 0.085(3) Uani 0.756(11) 1 d P . . C1S C 0.8943(6) 0.4459(4) 0.2202(5) 0.066(3) Uani 0.756(11) 1 d P . . C2S C 0.9526(6) 0.4029(4) 0.2175(7) 0.097(5) Uani 0.756(11) 1 d P . . H2SA H 0.9662 0.3942 0.1686 0.146 Uiso 0.756(11) 1 calc PR . . H2SB H 0.9305 0.3673 0.2400 0.146 Uiso 0.756(11) 1 calc PR . . H2SC H 1.0039 0.4159 0.2418 0.146 Uiso 0.756(11) 1 calc PR . . N2S N 0.9064(4) 0.4805(3) -0.2811(3) 0.056(2) Uani 0.735(10) 1 d P . . C3S C 0.8584(5) 0.4468(3) -0.2951(4) 0.050(2) Uani 0.735(10) 1 d P . . C4S C 0.7954(6) 0.4022(4) -0.3127(6) 0.075(3) Uani 0.735(10) 1 d P . . H4SA H 0.8020 0.3906 -0.3617 0.112 Uiso 0.735(10) 1 calc PR . . H4SB H 0.7387 0.4184 -0.3054 0.112 Uiso 0.735(10) 1 calc PR . . H4SC H 0.8032 0.3675 -0.2828 0.112 Uiso 0.735(10) 1 calc PR . . 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 0.0299(5) 0.0250(5) 0.0226(4) 0.000 -0.0012(3) 0.000 Fe2 0.0270(4) 0.0308(5) 0.0234(4) 0.000 -0.0019(3) 0.000 Fe3 0.0287(5) 0.0290(5) 0.0558(7) 0.000 0.0133(4) 0.000 O1 0.0312(15) 0.0334(16) 0.0332(15) 0.0065(13) 0.0048(12) 0.0065(13) O2 0.0403(17) 0.0399(18) 0.0279(15) 0.0005(13) -0.0026(13) 0.0109(14) O3 0.0314(15) 0.0327(16) 0.0312(15) -0.0033(13) 0.0029(12) -0.0063(13) O4 0.0378(17) 0.051(2) 0.0278(15) 0.0028(14) -0.0031(13) -0.0150(15) O5 0.0251(19) 0.027(2) 0.029(2) 0.000 -0.0001(16) 0.000 O6 0.0264(19) 0.036(2) 0.0251(19) 0.000 -0.0020(16) 0.000 N1 0.029(2) 0.037(3) 0.028(2) 0.000 0.009(2) 0.000 N2 0.023(2) 0.028(3) 0.034(3) 0.000 0.002(2) 0.000 N3 0.0311(18) 0.039(2) 0.0253(17) -0.0074(15) 0.0018(14) -0.0005(16) N4 0.0325(18) 0.0307(19) 0.0254(17) -0.0024(15) 0.0033(14) -0.0041(15) N5 0.030(3) 0.045(3) 0.029(2) 0.000 0.012(2) 0.000 N6 0.022(2) 0.040(3) 0.028(2) 0.000 0.0004(19) 0.000 N7 0.0266(18) 0.058(3) 0.0244(17) 0.0086(17) 0.0037(14) 0.0049(17) N8 0.0278(18) 0.041(2) 0.0271(17) 0.0059(16) 0.0018(14) 0.0094(17) C1 0.037(3) 0.042(4) 0.039(3) 0.000 0.017(3) 0.000 C2 0.023(3) 0.046(4) 0.059(4) 0.000 0.012(3) 0.000 C3 0.024(3) 0.037(4) 0.043(3) 0.000 0.003(3) 0.000 C4 0.041(2) 0.042(3) 0.035(2) -0.012(2) 0.000(2) -0.006(2) C5 0.044(3) 0.040(3) 0.040(2) -0.012(2) 0.002(2) -0.007(2) C6 0.040(2) 0.033(2) 0.030(2) -0.0056(18) 0.0063(18) -0.005(2) C7 0.048(4) 0.084(6) 0.045(4) 0.000 0.022(4) 0.000 C8 0.027(3) 0.060(5) 0.057(4) 0.000 -0.001(3) 0.000 C9 0.060(3) 0.057(3) 0.030(2) -0.013(2) -0.001(2) -0.003(3) C10 0.070(4) 0.045(3) 0.036(2) -0.008(2) 0.013(2) -0.020(3) C11 0.034(3) 0.057(5) 0.041(4) 0.000 0.017(3) 0.000 C12 0.025(3) 0.084(6) 0.054(4) 0.000 0.009(3) 0.000 C13 0.025(3) 0.053(5) 0.045(4) 0.000 0.004(3) 0.000 C14 0.044(3) 0.065(4) 0.031(2) 0.011(2) 0.004(2) 0.010(3) C15 0.057(3) 0.061(4) 0.041(3) 0.018(3) 0.012(2) 0.025(3) C16 0.041(3) 0.052(3) 0.031(2) 0.008(2) 0.0048(19) 0.013(2) C17 0.046(4) 0.100(7) 0.042(4) 0.000 0.023(3) 0.000 C18 0.029(3) 0.088(7) 0.057(5) 0.000 -0.008(3) 0.000 C19 0.070(4) 0.092(5) 0.032(3) 0.017(3) 0.002(3) 0.024(4) C20 0.080(4) 0.059(4) 0.036(3) 0.005(3) 0.009(3) 0.031(3) C21 0.0266(19) 0.030(2) 0.031(2) 0.0021(17) -0.0027(16) 0.0010(17) C28 0.0245(19) 0.031(2) 0.030(2) 0.0015(17) -0.0029(16) 0.0001(17) C29 0.034(2) 0.038(3) 0.044(3) 0.000(2) 0.002(2) -0.006(2) C30 0.057(3) 0.043(3) 0.057(3) -0.001(3) 0.004(3) -0.009(3) C31 0.069(4) 0.044(3) 0.074(4) -0.002(3) 0.015(3) -0.008(3) C32 0.068(4) 0.049(3) 0.080(4) -0.016(3) 0.004(4) -0.012(3) C33 0.064(4) 0.081(5) 0.069(4) -0.019(4) 0.007(3) -0.028(4) C34 0.058(3) 0.061(4) 0.050(3) -0.006(3) 0.002(3) -0.017(3) B1 0.029(3) 0.018(3) 0.013(2) 0.000 0.009(2) 0.000 B2 0.033(3) 0.032(3) 0.013(3) 0.000 0.010(2) 0.000 N1S 0.067(5) 0.056(5) 0.133(8) 0.013(5) -0.003(5) 0.002(4) C1S 0.057(5) 0.047(5) 0.094(7) 0.009(4) -0.017(5) -0.011(4) C2S 0.055(5) 0.030(4) 0.207(14) 0.013(6) -0.035(7) 0.004(4) N2S 0.060(4) 0.052(4) 0.057(4) 0.004(3) 0.001(3) 0.000(4) C3S 0.056(4) 0.037(4) 0.058(5) -0.002(3) 0.005(4) 0.007(4) C4S 0.081(6) 0.047(5) 0.096(7) -0.012(5) -0.007(6) -0.006(5) _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 2.024(3) 8_565 ? Fe1 O1 2.024(3) . ? Fe1 O5 1.859(4) . ? Fe1 N2 2.203(5) . ? Fe1 N4 2.130(4) 8_565 ? Fe1 N4 2.130(4) . ? Fe2 O3 2.034(3) 8_565 ? Fe2 O3 2.034(3) . ? Fe2 O6 1.864(4) . ? Fe2 N6 2.192(5) . ? Fe2 N8 2.132(4) . ? Fe2 N8 2.132(4) 8_565 ? Fe3 O2 2.067(3) 8_565 ? Fe3 O2 2.067(3) . ? Fe3 O4 2.065(3) . ? Fe3 O4 2.065(3) 8_565 ? Fe3 O5 1.929(4) . ? Fe3 O6 1.940(4) . ? O1 C21 1.266(5) . ? O2 C21 1.254(5) . ? O3 C28 1.270(5) . ? O4 C28 1.253(5) . ? N1 N2 1.354(7) . ? N1 C1 1.355(8) . ? N1 B1 1.491(8) . ? N2 C3 1.345(7) . ? N3 N4 1.374(5) . ? N3 C4 1.355(6) . ? N3 B1 1.546(5) . ? N4 C6 1.333(6) . ? N5 N6 1.389(7) . ? N5 C11 1.342(8) . ? N5 B2 1.467(8) . ? N6 C13 1.323(8) . ? N7 N8 1.366(5) . ? N7 C14 1.345(6) . ? N7 B2 1.568(5) . ? N8 C16 1.344(6) . ? C1 C2 1.365(10) . ? C1 C7 1.512(10) . ? C2 H2 0.9500 . ? C2 C3 1.404(9) . ? C3 C8 1.482(9) . ? C4 C5 1.368(7) . ? C4 C9 1.499(6) . ? C5 H5 0.9500 . ? C5 C6 1.399(6) . ? C6 C10 1.491(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.376(11) . ? C11 C17 1.501(10) . ? C12 H12 0.9500 . ? C12 C13 1.378(10) . ? C13 C18 1.490(10) . ? C14 C15 1.377(8) . ? C14 C19 1.509(6) . ? C15 H15 0.9500 . ? C15 C16 1.407(7) . ? C16 C20 1.491(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22A 1.515(11) . ? C21 C22B 1.507(12) . ? C22A C23A 1.375(12) . ? C22A C27A 1.379(14) . ? C23A H23A 0.9500 . ? C23A C24A 1.408(13) . ? C24A H24A 0.9500 . ? C24A C25A 1.381(14) . ? C25A H25A 0.9500 . ? C25A C26A 1.334(15) . ? C26A H26A 0.9500 . ? C26A C27A 1.436(15) . ? C27A H27A 0.9500 . ? C22B C23B 1.391(12) . ? C22B C27B 1.391(13) . ? C23B H23B 0.9500 . ? C23B C24B 1.388(12) . ? C24B H24B 0.9500 . ? C24B C25B 1.399(13) . ? C25B H25B 0.9500 . ? C25B C26B 1.346(14) . ? C26B H26B 0.9500 . ? C26B C27B 1.430(14) . ? C27B H27B 0.9500 . ? C28 C29 1.501(6) . ? C29 C30 1.394(7) . ? C29 C34 1.359(7) . ? C30 H30 0.9500 . ? C30 C31 1.373(8) . ? C31 H31 0.9500 . ? C31 C32 1.384(9) . ? C32 H32 0.9500 . ? C32 C33 1.368(10) . ? C33 H33 0.9500 . ? C33 C34 1.397(9) . ? C34 H34 0.9500 . ? B1 N3 1.546(5) 8_565 ? B1 H1 1.0000 . ? B2 N7 1.568(5) 8_565 ? B2 H2A 1.0000 . ? N1S C1S 1.177(11) . ? C1S C2S 1.342(12) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? N2S C3S 1.110(10) . ? C3S C4S 1.459(12) . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 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 O1 Fe1 O1 92.96(18) . 8_565 ? O1 Fe1 N2 84.88(12) . . ? O1 Fe1 N2 84.88(12) 8_565 . ? O1 Fe1 N4 89.76(14) 8_565 8_565 ? O1 Fe1 N4 168.48(13) . 8_565 ? O1 Fe1 N4 168.48(13) 8_565 . ? O1 Fe1 N4 89.76(14) . . ? O5 Fe1 O1 93.75(12) . . ? O5 Fe1 O1 93.75(12) . 8_565 ? O5 Fe1 N2 178.00(18) . . ? O5 Fe1 N4 97.24(13) . . ? O5 Fe1 N4 97.24(13) . 8_565 ? N4 Fe1 N2 84.22(13) 8_565 . ? N4 Fe1 N2 84.22(13) . . ? N4 Fe1 N4 85.5(2) . 8_565 ? O3 Fe2 O3 92.89(18) . 8_565 ? O3 Fe2 N6 85.86(12) . . ? O3 Fe2 N6 85.86(12) 8_565 . ? O3 Fe2 N8 169.20(13) . 8_565 ? O3 Fe2 N8 90.04(14) 8_565 8_565 ? O3 Fe2 N8 169.20(13) 8_565 . ? O3 Fe2 N8 90.04(14) . . ? O6 Fe2 O3 93.00(12) . 8_565 ? O6 Fe2 O3 92.99(12) . . ? O6 Fe2 N6 178.34(18) . . ? O6 Fe2 N8 97.24(13) . 8_565 ? O6 Fe2 N8 97.23(13) . . ? N8 Fe2 N6 83.98(14) 8_565 . ? N8 Fe2 N6 83.98(14) . . ? N8 Fe2 N8 85.3(2) . 8_565 ? O2 Fe3 O2 91.51(19) 8_565 . ? O4 Fe3 O2 178.74(14) 8_565 . ? O4 Fe3 O2 89.64(14) 8_565 8_565 ? O4 Fe3 O2 89.64(14) . . ? O4 Fe3 O2 178.74(14) . 8_565 ? O4 Fe3 O4 89.2(2) 8_565 . ? O5 Fe3 O2 91.20(12) . . ? O5 Fe3 O2 91.20(12) . 8_565 ? O5 Fe3 O4 89.29(12) . 8_565 ? O5 Fe3 O4 89.29(12) . . ? O5 Fe3 O6 178.96(17) . . ? O6 Fe3 O2 88.07(12) . . ? O6 Fe3 O2 88.07(12) . 8_565 ? O6 Fe3 O4 91.45(12) . 8_565 ? O6 Fe3 O4 91.45(12) . . ? C21 O1 Fe1 132.2(3) . . ? C21 O2 Fe3 133.3(3) . . ? C28 O3 Fe2 132.7(3) . . ? C28 O4 Fe3 133.4(3) . . ? Fe1 O5 Fe3 126.0(2) . . ? Fe2 O6 Fe3 126.5(2) . . ? N2 N1 C1 109.9(5) . . ? N2 N1 B1 119.0(4) . . ? C1 N1 B1 131.1(5) . . ? N1 N2 Fe1 119.1(4) . . ? C3 N2 Fe1 133.5(4) . . ? C3 N2 N1 107.3(5) . . ? N4 N3 B1 119.3(4) . . ? C4 N3 N4 109.0(4) . . ? C4 N3 B1 131.7(4) . . ? N3 N4 Fe1 119.1(3) . . ? C6 N4 Fe1 133.4(3) . . ? C6 N4 N3 107.4(3) . . ? N6 N5 B2 119.6(4) . . ? C11 N5 N6 109.0(5) . . ? C11 N5 B2 131.4(6) . . ? N5 N6 Fe2 118.6(4) . . ? C13 N6 Fe2 134.9(5) . . ? C13 N6 N5 106.5(5) . . ? N8 N7 B2 118.5(4) . . ? C14 N7 N8 109.6(4) . . ? C14 N7 B2 131.9(4) . . ? N7 N8 Fe2 120.4(3) . . ? C16 N8 Fe2 132.6(3) . . ? C16 N8 N7 107.0(4) . . ? N1 C1 C2 107.8(6) . . ? N1 C1 C7 122.8(6) . . ? C2 C1 C7 129.4(6) . . ? C1 C2 H2 126.9 . . ? C1 C2 C3 106.3(6) . . ? C3 C2 H2 126.9 . . ? N2 C3 C2 108.7(6) . . ? N2 C3 C8 123.0(6) . . ? C2 C3 C8 128.4(6) . . ? N3 C4 C5 108.0(4) . . ? N3 C4 C9 122.3(5) . . ? C5 C4 C9 129.7(5) . . ? C4 C5 H5 126.8 . . ? C4 C5 C6 106.4(4) . . ? C6 C5 H5 126.8 . . ? N4 C6 C5 109.2(4) . . ? N4 C6 C10 122.1(4) . . ? C5 C6 C10 128.7(5) . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C12 107.9(6) . . ? N5 C11 C17 123.1(7) . . ? C12 C11 C17 129.1(6) . . ? C11 C12 H12 126.9 . . ? C11 C12 C13 106.3(6) . . ? C13 C12 H12 126.9 . . ? N6 C13 C12 110.3(6) . . ? N6 C13 C18 121.5(6) . . ? C12 C13 C18 128.2(6) . . ? N7 C14 C15 108.8(4) . . ? N7 C14 C19 122.9(5) . . ? C15 C14 C19 128.3(5) . . ? C14 C15 H15 127.4 . . ? C14 C15 C16 105.1(5) . . ? C16 C15 H15 127.4 . . ? N8 C16 C15 109.5(4) . . ? N8 C16 C20 122.6(4) . . ? C15 C16 C20 127.9(5) . . ? C11 C17 H17A 109.5 . . ? C11 C17 H17B 109.5 . . ? C11 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O1 C21 C22A 117.8(5) . . ? O1 C21 C22B 111.7(6) . . ? O2 C21 O1 126.2(4) . . ? O2 C21 C22A 115.8(5) . . ? O2 C21 C22B 121.9(6) . . ? C22B C21 C22A 11.3(8) . . ? C23A C22A C21 120.2(10) . . ? C23A C22A C27A 118.7(10) . . ? C27A C22A C21 121.1(9) . . ? C22A C23A H23A 119.2 . . ? C22A C23A C24A 121.5(11) . . ? C24A C23A H23A 119.2 . . ? C23A C24A H24A 120.0 . . ? C25A C24A C23A 120.0(11) . . ? C25A C24A H24A 120.0 . . ? C24A C25A H25A 120.8 . . ? C26A C25A C24A 118.5(12) . . ? C26A C25A H25A 120.8 . . ? C25A C26A H26A 118.6 . . ? C25A C26A C27A 122.8(12) . . ? C27A C26A H26A 118.6 . . ? C22A C27A C26A 118.4(11) . . ? C22A C27A H27A 120.8 . . ? C26A C27A H27A 120.8 . . ? C23B C22B C21 120.7(9) . . ? C27B C22B C21 117.7(9) . . ? C27B C22B C23B 121.0(10) . . ? C22B C23B H23B 119.4 . . ? C24B C23B C22B 121.3(10) . . ? C24B C23B H23B 119.4 . . ? C23B C24B H24B 120.8 . . ? C23B C24B C25B 118.3(10) . . ? C25B C24B H24B 120.8 . . ? C24B C25B H25B 119.9 . . ? C26B C25B C24B 120.3(11) . . ? C26B C25B H25B 119.9 . . ? C25B C26B H26B 118.6 . . ? C25B C26B C27B 122.9(11) . . ? C27B C26B H26B 118.6 . . ? C22B C27B C26B 116.1(10) . . ? C22B C27B H27B 121.9 . . ? C26B C27B H27B 121.9 . . ? O3 C28 C29 116.1(4) . . ? O4 C28 O3 126.1(4) . . ? O4 C28 C29 117.8(4) . . ? C30 C29 C28 119.8(4) . . ? C34 C29 C28 120.6(5) . . ? C34 C29 C30 119.4(5) . . ? C29 C30 H30 119.6 . . ? C31 C30 C29 120.9(6) . . ? C31 C30 H30 119.6 . . ? C30 C31 H31 120.5 . . ? C30 C31 C32 118.9(6) . . ? C32 C31 H31 120.5 . . ? C31 C32 H32 119.6 . . ? C33 C32 C31 120.9(6) . . ? C33 C32 H32 119.6 . . ? C32 C33 H33 120.3 . . ? C32 C33 C34 119.5(6) . . ? C34 C33 H33 120.3 . . ? C29 C34 C33 120.4(6) . . ? C29 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? N1 B1 N3 110.6(3) . . ? N1 B1 N3 110.6(3) . 8_565 ? N1 B1 H1 109.4 . . ? N3 B1 N3 107.6(4) 8_565 . ? N3 B1 H1 109.4 . . ? N3 B1 H1 109.4 8_565 . ? N5 B2 N7 111.0(3) . . ? N5 B2 N7 111.0(3) . 8_565 ? N5 B2 H2A 109.5 . . ? N7 B2 N7 106.3(4) 8_565 . ? N7 B2 H2A 109.5 . . ? N7 B2 H2A 109.5 8_565 . ? N1S C1S C2S 177.5(9) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SB 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? N2S C3S C4S 179.3(10) . . ? C3S C4S H4SA 109.5 . . ? C3S C4S H4SB 109.5 . . ? C3S C4S H4SC 109.5 . . ? H4SA C4S H4SB 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 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 Fe1 O1 C21 O2 6.9(7) . . . . ? Fe1 O1 C21 C22A -167.5(7) . . . . ? Fe1 O1 C21 C22B -178.1(7) . . . . ? Fe1 N2 C3 C2 180.0 . . . . ? Fe1 N2 C3 C8 0.0 . . . . ? Fe1 N4 C6 C5 -179.2(3) . . . . ? Fe1 N4 C6 C10 1.7(7) . . . . ? Fe2 O3 C28 O4 4.8(7) . . . . ? Fe2 O3 C28 C29 -174.0(3) . . . . ? Fe2 N6 C13 C12 180.0 . . . . ? Fe2 N6 C13 C18 0.0 . . . . ? Fe2 N8 C16 C15 -176.3(4) . . . . ? Fe2 N8 C16 C20 3.8(8) . . . . ? Fe3 O2 C21 O1 -7.3(7) . . . . ? Fe3 O2 C21 C22A 167.2(7) . . . . ? Fe3 O2 C21 C22B 178.1(7) . . . . ? Fe3 O4 C28 O3 -8.0(7) . . . . ? Fe3 O4 C28 C29 170.7(3) . . . . ? O1 Fe1 O1 C21 -76.7(4) 8_565 . . . ? O1 Fe1 O5 Fe3 46.61(9) 8_565 . . . ? O1 Fe1 O5 Fe3 -46.61(9) . . . . ? O1 Fe1 N2 N1 -133.28(9) . . . . ? O1 Fe1 N2 N1 133.28(9) 8_565 . . . ? O1 Fe1 N2 C3 -46.72(9) 8_565 . . . ? O1 Fe1 N2 C3 46.72(9) . . . . ? O1 Fe1 N4 N3 127.2(3) . . . . ? O1 Fe1 N4 N3 23.5(9) 8_565 . . . ? O1 Fe1 N4 C6 -156.3(6) 8_565 . . . ? O1 Fe1 N4 C6 -52.5(4) . . . . ? O1 C21 C22A C23A -26.4(15) . . . . ? O1 C21 C22A C27A 154.6(10) . . . . ? O1 C21 C22B C23B 20.2(15) . . . . ? O1 C21 C22B C27B -168.3(10) . . . . ? O2 Fe3 O2 C21 75.3(4) 8_565 . . . ? O2 Fe3 O4 C28 54(6) 8_565 . . . ? O2 Fe3 O4 C28 -101.7(4) . . . . ? O2 Fe3 O5 Fe1 -45.77(10) 8_565 . . . ? O2 Fe3 O5 Fe1 45.77(10) . . . . ? O2 Fe3 O6 Fe2 134.21(10) . . . . ? O2 Fe3 O6 Fe2 -134.21(10) 8_565 . . . ? O2 C21 C22A C23A 158.6(10) . . . . ? O2 C21 C22A C27A -20.4(15) . . . . ? O2 C21 C22B C23B -164.4(10) . . . . ? O2 C21 C22B C27B 7.1(16) . . . . ? O3 Fe2 O3 C28 -73.7(4) 8_565 . . . ? O3 Fe2 O6 Fe3 46.53(9) 8_565 . . . ? O3 Fe2 O6 Fe3 -46.53(9) . . . . ? O3 Fe2 N6 N5 133.40(9) 8_565 . . . ? O3 Fe2 N6 N5 -133.40(9) . . . . ? O3 Fe2 N6 C13 -46.60(9) 8_565 . . . ? O3 Fe2 N6 C13 46.60(9) . . . . ? O3 Fe2 N8 N7 23.7(10) 8_565 . . . ? O3 Fe2 N8 N7 129.5(3) . . . . ? O3 Fe2 N8 C16 -52.5(5) . . . . ? O3 Fe2 N8 C16 -158.4(7) 8_565 . . . ? O3 C28 C29 C30 16.0(7) . . . . ? O3 C28 C29 C34 -169.5(5) . . . . ? O4 Fe3 O2 C21 -105.2(4) . . . . ? O4 Fe3 O2 C21 -129(6) 8_565 . . . ? O4 Fe3 O4 C28 77.8(4) 8_565 . . . ? O4 Fe3 O5 Fe1 -135.40(10) 8_565 . . . ? O4 Fe3 O5 Fe1 135.40(10) . . . . ? O4 Fe3 O6 Fe2 -44.62(10) 8_565 . . . ? O4 Fe3 O6 Fe2 44.62(10) . . . . ? O4 C28 C29 C30 -162.9(5) . . . . ? O4 C28 C29 C34 11.7(7) . . . . ? O5 Fe1 O1 C21 17.3(4) . . . . ? O5 Fe1 N2 N1 180.000(4) . . . . ? O5 Fe1 N2 C3 0.000(5) . . . . ? O5 Fe1 N4 N3 -139.0(3) . . . . ? O5 Fe1 N4 C6 41.2(4) . . . . ? O5 Fe3 O2 C21 -15.9(4) . . . . ? O5 Fe3 O4 C28 167.1(4) . . . . ? O5 Fe3 O6 Fe2 180.000(3) . . . . ? O6 Fe2 O3 C28 19.5(4) . . . . ? O6 Fe2 N6 N5 180.000(6) . . . . ? O6 Fe2 N6 C13 0.000(7) . . . . ? O6 Fe2 N8 N7 -137.5(3) . . . . ? O6 Fe2 N8 C16 40.5(5) . . . . ? O6 Fe3 O2 C21 163.3(4) . . . . ? O6 Fe3 O4 C28 -13.7(4) . . . . ? O6 Fe3 O5 Fe1 0.000(4) . . . . ? N1 N2 C3 C2 0.0 . . . . ? N1 N2 C3 C8 180.0 . . . . ? N1 C1 C2 C3 0.0 . . . . ? N2 Fe1 O1 C21 -161.2(4) . . . . ? N2 Fe1 O5 Fe3 0.000(2) . . . . ? N2 Fe1 N4 N3 42.3(3) . . . . ? N2 Fe1 N4 C6 -137.4(4) . . . . ? N2 N1 C1 C2 0.0 . . . . ? N2 N1 C1 C7 180.0 . . . . ? N2 N1 B1 N3 59.5(3) . . . . ? N2 N1 B1 N3 -59.5(3) . . . 8_565 ? N3 N4 C6 C5 1.0(5) . . . . ? N3 N4 C6 C10 -178.0(5) . . . . ? N3 C4 C5 C6 0.7(6) . . . . ? N4 Fe1 O1 C21 179.9(6) 8_565 . . . ? N4 Fe1 O1 C21 114.5(4) . . . . ? N4 Fe1 O5 Fe3 -136.84(10) . . . . ? N4 Fe1 O5 Fe3 136.84(10) 8_565 . . . ? N4 Fe1 N2 N1 43.00(10) 8_565 . . . ? N4 Fe1 N2 N1 -43.00(10) . . . . ? N4 Fe1 N2 C3 -137.00(10) 8_565 . . . ? N4 Fe1 N2 C3 137.00(10) . . . . ? N4 Fe1 N4 N3 -42.3(4) 8_565 . . . ? N4 Fe1 N4 C6 138.0(4) 8_565 . . . ? N4 N3 C4 C5 -0.2(5) . . . . ? N4 N3 C4 C9 179.8(4) . . . . ? N4 N3 B1 N1 -60.0(5) . . . . ? N4 N3 B1 N3 60.8(6) . . . 8_565 ? N5 N6 C13 C12 0.0 . . . . ? N5 N6 C13 C18 180.0 . . . . ? N5 C11 C12 C13 0.0 . . . . ? N6 Fe2 O3 C28 -159.3(4) . . . . ? N6 Fe2 O6 Fe3 0.000(3) . . . . ? N6 Fe2 N8 N7 43.7(3) . . . . ? N6 Fe2 N8 C16 -138.4(5) . . . . ? N6 N5 C11 C12 0.0 . . . . ? N6 N5 C11 C17 180.0 . . . . ? N6 N5 B2 N7 -59.0(3) . . . 8_565 ? N6 N5 B2 N7 59.0(3) . . . . ? N7 N8 C16 C15 1.8(6) . . . . ? N7 N8 C16 C20 -178.0(5) . . . . ? N7 C14 C15 C16 1.6(7) . . . . ? N8 Fe2 O3 C28 116.7(4) . . . . ? N8 Fe2 O3 C28 -179.3(7) 8_565 . . . ? N8 Fe2 O6 Fe3 -136.95(11) . . . . ? N8 Fe2 O6 Fe3 136.95(11) 8_565 . . . ? N8 Fe2 N6 N5 -42.92(11) . . . . ? N8 Fe2 N6 N5 42.92(11) 8_565 . . . ? N8 Fe2 N6 C13 137.08(11) . . . . ? N8 Fe2 N6 C13 -137.08(11) 8_565 . . . ? N8 Fe2 N8 N7 -40.7(4) 8_565 . . . ? N8 Fe2 N8 C16 137.2(4) 8_565 . . . ? N8 N7 C14 C15 -0.6(6) . . . . ? N8 N7 C14 C19 -179.2(5) . . . . ? N8 N7 B2 N5 -58.2(5) . . . . ? N8 N7 B2 N7 62.6(6) . . . 8_565 ? C1 N1 N2 Fe1 180.0 . . . . ? C1 N1 N2 C3 0.0 . . . . ? C1 N1 B1 N3 120.5(3) . . . 8_565 ? C1 N1 B1 N3 -120.5(3) . . . . ? C1 C2 C3 N2 0.0 . . . . ? C1 C2 C3 C8 180.0 . . . . ? C4 N3 N4 Fe1 179.7(3) . . . . ? C4 N3 N4 C6 -0.5(5) . . . . ? C4 N3 B1 N1 118.6(5) . . . . ? C4 N3 B1 N3 -120.6(5) . . . 8_565 ? C4 C5 C6 N4 -1.1(6) . . . . ? C4 C5 C6 C10 177.9(5) . . . . ? C7 C1 C2 C3 180.0 . . . . ? C9 C4 C5 C6 -179.2(5) . . . . ? C11 N5 N6 Fe2 180.0 . . . . ? C11 N5 N6 C13 0.0 . . . . ? C11 N5 B2 N7 -121.0(3) . . . . ? C11 N5 B2 N7 121.0(3) . . . 8_565 ? C11 C12 C13 N6 0.0 . . . . ? C11 C12 C13 C18 180.0 . . . . ? C14 N7 N8 Fe2 177.7(3) . . . . ? C14 N7 N8 C16 -0.8(5) . . . . ? C14 N7 B2 N5 120.3(6) . . . . ? C14 N7 B2 N7 -118.9(5) . . . 8_565 ? C14 C15 C16 N8 -2.1(7) . . . . ? C14 C15 C16 C20 177.7(6) . . . . ? C17 C11 C12 C13 180.0 . . . . ? C19 C14 C15 C16 -179.9(6) . . . . ? C21 C22A C23A C24A -179.1(12) . . . . ? C21 C22A C27A C26A 179.0(11) . . . . ? C21 C22B C23B C24B 174.0(10) . . . . ? C21 C22B C27B C26B -174.8(10) . . . . ? C22A C21 C22B C23B -104(5) . . . . ? C22A C21 C22B C27B 67(4) . . . . ? C22A C23A C24A C25A -2(2) . . . . ? C23A C22A C27A C26A 0(2) . . . . ? C23A C24A C25A C26A 5(2) . . . . ? C24A C25A C26A C27A -5(2) . . . . ? C25A C26A C27A C22A 3(2) . . . . ? C27A C22A C23A C24A 0(2) . . . . ? C22B C21 C22A C23A 34(3) . . . . ? C22B C21 C22A C27A -145(5) . . . . ? C22B C23B C24B C25B 0.3(19) . . . . ? C23B C22B C27B C26B -3.3(19) . . . . ? C23B C24B C25B C26B -3(2) . . . . ? C24B C25B C26B C27B 2(2) . . . . ? C25B C26B C27B C22B 0.9(19) . . . . ? C27B C22B C23B C24B 3(2) . . . . ? C28 C29 C30 C31 176.1(5) . . . . ? C28 C29 C34 C33 -176.7(6) . . . . ? C29 C30 C31 C32 -1.3(10) . . . . ? C30 C29 C34 C33 -2.1(9) . . . . ? C30 C31 C32 C33 1.9(11) . . . . ? C31 C32 C33 C34 -2.5(11) . . . . ? C32 C33 C34 C29 2.7(11) . . . . ? C34 C29 C30 C31 1.5(9) . . . . ? B1 N1 N2 Fe1 0.0 . . . . ? B1 N1 N2 C3 180.0 . . . . ? B1 N1 C1 C2 180.0 . . . . ? B1 N1 C1 C7 0.000(1) . . . . ? B1 N3 N4 Fe1 -1.4(5) . . . . ? B1 N3 N4 C6 178.4(4) . . . . ? B1 N3 C4 C5 -178.9(4) . . . . ? B1 N3 C4 C9 1.1(8) . . . . ? B2 N5 N6 Fe2 0.0 . . . . ? B2 N5 N6 C13 180.0 . . . . ? B2 N5 C11 C12 180.0 . . . . ? B2 N5 C11 C17 0.000(1) . . . . ? B2 N7 N8 Fe2 -3.5(5) . . . . ? B2 N7 N8 C16 178.1(4) . . . . ? B2 N7 C14 C15 -179.2(5) . . . . ? B2 N7 C14 C19 2.2(9) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 1 15 0 0.0187 1.0012 14.9985 -0.0002 -0.9533 0.2755 -0.2591 -1 -15 0 0.0187 -1.0012 -14.9985 0.0002 0.9533 -0.2755 0.2591 -7 -2 -9 0.0512 -7.0010 -1.9982 -9.0001 0.5005 0.8587 -0.1360 7 2 9 0.0512 7.0010 1.9982 9.0001 -0.5005 -0.8587 0.1360 -1 1 -12 0.0433 -1.0012 1.0015 -11.9999 0.0890 0.8881 0.3848 1 -1 12 0.0433 1.0012 -1.0015 11.9999 -0.0890 -0.8881 -0.3848 8 -5 -6 0.0558 7.9989 -4.9993 -5.9997 0.0155 -0.0123 0.9773 -8 5 6 0.0558 -7.9989 4.9993 5.9997 -0.0155 0.0123 -0.9773 #===END data_Fe(Ph2Tp)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H68 B2 Fe N12' _chemical_formula_weight 1395.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8870(3) _cell_length_b 12.6456(3) _cell_length_c 14.2454(3) _cell_angle_alpha 70.4240(10) _cell_angle_beta 71.3970(10) _cell_angle_gamma 74.6550(10) _cell_volume 1723.75(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6334 _cell_measurement_theta_min 3 _cell_measurement_theta_max 68 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 2.222 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5781 _exptl_absorpt_correction_T_max 0.8167 _exptl_absorpt_process_details ; Numerical (based on real shape of the crystal) absorption correction followed by: SADABS. Program for empirical absorption correction of area-detector data. University of Goetingen. Germany. Sheldrick, G. M. 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14604 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 68.02 _reflns_number_total 5923 _reflns_number_gt 5522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2-2009.5-1 (Bruker, 2009)' _computing_cell_refinement 'SAINT v7.60A (Bruker, 2009)' _computing_data_reduction 'SADABS-2008/1 (Bruker, 2008)' _computing_structure_solution 'XS/SHELXTL-2008/4 (Bruker, 2008)' _computing_structure_refinement 'SHELXL-2008/4(Bruker, 2008)' _computing_molecular_graphics 'XP v5.1 (Bruker, 1998)' _computing_publication_material 'XCIF-2008/2 (Bruker, 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^)+(0.0453P)^2^+0.6155P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00087(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5923 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _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 0.5000 0.5000 0.5000 0.01360(10) Uani 1 2 d S . . N1 N 0.47728(12) 0.51017(11) 0.35045(9) 0.0159(3) Uani 1 1 d . . . N2 N 0.55183(12) 0.58221(10) 0.27090(9) 0.0156(3) Uani 1 1 d . . . N3 N 0.70924(12) 0.45947(11) 0.43590(9) 0.0158(3) Uani 1 1 d . . . N4 N 0.75203(12) 0.53439(11) 0.34238(9) 0.0154(3) Uani 1 1 d . . . N5 N 0.50516(12) 0.68937(11) 0.45162(9) 0.0149(3) Uani 1 1 d . . . N6 N 0.58661(12) 0.71926(11) 0.35425(9) 0.0152(3) Uani 1 1 d . . . B1 B 0.65444(17) 0.63312(15) 0.29007(13) 0.0162(4) Uani 1 1 d . . . H1 H 0.7057 0.6745 0.2217 0.019 Uiso 1 1 calc R . . C11 C 0.42239(15) 0.46051(13) 0.30697(12) 0.0176(3) Uani 1 1 d . . . C12 C 0.46073(16) 0.50152(13) 0.20003(12) 0.0191(3) Uani 1 1 d . . . H12A H 0.4360 0.4807 0.1513 0.023 Uiso 1 1 calc R . . C13 C 0.54198(15) 0.57853(13) 0.17903(12) 0.0170(3) Uani 1 1 d . . . C21 C 0.81533(15) 0.37957(13) 0.45558(12) 0.0174(3) Uani 1 1 d . . . C22 C 0.92655(16) 0.40523(13) 0.37579(12) 0.0197(3) Uani 1 1 d . . . H22A H 1.0139 0.3637 0.3708 0.024 Uiso 1 1 calc R . . C23 C 0.88415(15) 0.50301(13) 0.30564(12) 0.0176(3) Uani 1 1 d . . . C31 C 0.45710(15) 0.78758(13) 0.48089(12) 0.0168(3) Uani 1 1 d . . . C32 C 0.50824(15) 0.87779(13) 0.40131(12) 0.0189(3) Uani 1 1 d . . . H32A H 0.4902 0.9554 0.4015 0.023 Uiso 1 1 calc R . . C33 C 0.58896(15) 0.83286(13) 0.32337(12) 0.0171(3) Uani 1 1 d . . . C41 C 0.34171(15) 0.37017(14) 0.36475(12) 0.0191(3) Uani 1 1 d . . . C42 C 0.24414(16) 0.37332(14) 0.45551(12) 0.0212(3) Uani 1 1 d . . . H42A H 0.2254 0.4370 0.4822 0.025 Uiso 1 1 calc R . . C43 C 0.17362(17) 0.28432(15) 0.50772(13) 0.0245(4) Uani 1 1 d . . . H43A H 0.1085 0.2866 0.5704 0.029 Uiso 1 1 calc R . . C44 C 0.19868(17) 0.19262(15) 0.46805(13) 0.0254(4) Uani 1 1 d . . . H44A H 0.1509 0.1317 0.5035 0.030 Uiso 1 1 calc R . . C45 C 0.29347(17) 0.18971(14) 0.37666(13) 0.0247(4) Uani 1 1 d . . . H45A H 0.3096 0.1273 0.3488 0.030 Uiso 1 1 calc R . . C46 C 0.36480(16) 0.27741(14) 0.32570(13) 0.0218(3) Uani 1 1 d . . . H46A H 0.4303 0.2743 0.2634 0.026 Uiso 1 1 calc R . . C51 C 0.60893(15) 0.64512(14) 0.07705(12) 0.0183(3) Uani 1 1 d . . . C52 C 0.61124(16) 0.76084(14) 0.05450(12) 0.0211(3) Uani 1 1 d . . . H52A H 0.5670 0.8003 0.1056 0.025 Uiso 1 1 calc R . . C53 C 0.67773(18) 0.81858(15) -0.04200(13) 0.0265(4) Uani 1 1 d . . . H53A H 0.6792 0.8973 -0.0566 0.032 Uiso 1 1 calc R . . C54 C 0.74205(18) 0.76220(16) -0.11726(13) 0.0281(4) Uani 1 1 d . . . H54A H 0.7886 0.8020 -0.1830 0.034 Uiso 1 1 calc R . . C55 C 0.73859(17) 0.64785(16) -0.09672(13) 0.0271(4) Uani 1 1 d . . . H55A H 0.7816 0.6093 -0.1486 0.033 Uiso 1 1 calc R . . C56 C 0.67196(16) 0.58952(14) 0.00002(12) 0.0218(3) Uani 1 1 d . . . H56A H 0.6693 0.5112 0.0138 0.026 Uiso 1 1 calc R . . C61 C 0.81212(15) 0.27595(13) 0.54480(12) 0.0185(3) Uani 1 1 d . . . C62 C 0.75853(16) 0.27806(14) 0.64689(12) 0.0229(3) Uani 1 1 d . . . H62A H 0.7197 0.3489 0.6624 0.027 Uiso 1 1 calc R . . C63 C 0.76100(18) 0.17794(15) 0.72651(13) 0.0285(4) Uani 1 1 d . . . H63A H 0.7222 0.1805 0.7958 0.034 Uiso 1 1 calc R . . C64 C 0.81991(18) 0.07422(15) 0.70510(14) 0.0285(4) Uani 1 1 d . . . H64A H 0.8225 0.0060 0.7597 0.034 Uiso 1 1 calc R . . C65 C 0.87472(17) 0.07024(15) 0.60432(14) 0.0257(4) Uani 1 1 d . . . H65A H 0.9150 -0.0007 0.5894 0.031 Uiso 1 1 calc R . . C66 C 0.87082(16) 0.17091(14) 0.52430(13) 0.0213(3) Uani 1 1 d . . . H66A H 0.9086 0.1679 0.4550 0.026 Uiso 1 1 calc R . . C71 C 0.96635(15) 0.56578(13) 0.20886(12) 0.0183(3) Uani 1 1 d . . . C72 C 0.94253(16) 0.58717(14) 0.11304(12) 0.0205(3) Uani 1 1 d . . . H72A H 0.8701 0.5623 0.1085 0.025 Uiso 1 1 calc R . . C73 C 1.02411(17) 0.64449(14) 0.02447(13) 0.0239(4) Uani 1 1 d . . . H73A H 1.0069 0.6593 -0.0405 0.029 Uiso 1 1 calc R . . C74 C 1.13087(16) 0.68049(14) 0.03013(13) 0.0238(4) Uani 1 1 d . . . H74A H 1.1858 0.7207 -0.0307 0.029 Uiso 1 1 calc R . . C75 C 1.15709(16) 0.65771(14) 0.12447(13) 0.0236(4) Uani 1 1 d . . . H75A H 1.2311 0.6810 0.1283 0.028 Uiso 1 1 calc R . . C76 C 1.07485(16) 0.60054(14) 0.21404(13) 0.0214(3) Uani 1 1 d . . . H76A H 1.0928 0.5852 0.2788 0.026 Uiso 1 1 calc R . . C81 C 0.36245(15) 0.80227(13) 0.57889(12) 0.0188(3) Uani 1 1 d . . . C82 C 0.31339(15) 0.71440(14) 0.66160(12) 0.0193(3) Uani 1 1 d . . . H82A H 0.3450 0.6378 0.6583 0.023 Uiso 1 1 calc R . . C83 C 0.21957(17) 0.73604(15) 0.74857(12) 0.0246(4) Uani 1 1 d . . . H83A H 0.1873 0.6745 0.8035 0.029 Uiso 1 1 calc R . . C84 C 0.17268(18) 0.84695(15) 0.75575(13) 0.0275(4) Uani 1 1 d . . . H84A H 0.1075 0.8620 0.8148 0.033 Uiso 1 1 calc R . . C85 C 0.22217(18) 0.93519(15) 0.67585(13) 0.0279(4) Uani 1 1 d . . . H85A H 0.1920 1.0114 0.6804 0.034 Uiso 1 1 calc R . . C86 C 0.31534(17) 0.91320(14) 0.58936(13) 0.0227(3) Uani 1 1 d . . . H86A H 0.3485 0.9751 0.5354 0.027 Uiso 1 1 calc R . . C91 C 0.66100(16) 0.89733(13) 0.22172(12) 0.0185(3) Uani 1 1 d . . . C92 C 0.79467(16) 0.86517(14) 0.17835(13) 0.0211(3) Uani 1 1 d . . . H92A H 0.8436 0.7982 0.2138 0.025 Uiso 1 1 calc R . . C93 C 0.85638(17) 0.93079(15) 0.08359(13) 0.0256(4) Uani 1 1 d . . . H93A H 0.9469 0.9073 0.0537 0.031 Uiso 1 1 calc R . . C94 C 0.78689(18) 1.03033(15) 0.03218(13) 0.0280(4) Uani 1 1 d . . . H94A H 0.8295 1.0748 -0.0327 0.034 Uiso 1 1 calc R . . C95 C 0.65552(17) 1.06426(15) 0.07592(14) 0.0280(4) Uani 1 1 d . . . H95A H 0.6080 1.1332 0.0417 0.034 Uiso 1 1 calc R . . C96 C 0.59271(17) 0.99814(14) 0.16954(13) 0.0238(4) Uani 1 1 d . . . H96A H 0.5019 1.0217 0.1986 0.029 Uiso 1 1 calc R . . 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 0.01532(18) 0.01229(18) 0.01242(17) -0.00172(13) -0.00255(13) -0.00456(12) N1 0.0169(6) 0.0144(7) 0.0154(6) -0.0019(5) -0.0026(5) -0.0056(5) N2 0.0184(7) 0.0134(7) 0.0135(6) -0.0009(5) -0.0031(5) -0.0053(5) N3 0.0176(7) 0.0148(7) 0.0138(6) -0.0013(5) -0.0028(5) -0.0055(5) N4 0.0170(7) 0.0144(7) 0.0143(6) -0.0027(5) -0.0026(5) -0.0054(5) N5 0.0163(6) 0.0150(7) 0.0129(6) -0.0023(5) -0.0022(5) -0.0057(5) N6 0.0152(6) 0.0148(7) 0.0144(6) -0.0004(5) -0.0032(5) -0.0063(5) B1 0.0180(9) 0.0174(9) 0.0130(8) -0.0018(7) -0.0028(7) -0.0074(7) C11 0.0181(8) 0.0156(8) 0.0201(8) -0.0036(6) -0.0071(6) -0.0036(6) C12 0.0228(8) 0.0177(8) 0.0191(8) -0.0042(6) -0.0080(6) -0.0052(6) C13 0.0181(8) 0.0173(8) 0.0156(7) -0.0041(6) -0.0055(6) -0.0022(6) C21 0.0199(8) 0.0171(8) 0.0167(7) -0.0022(6) -0.0073(6) -0.0055(6) C22 0.0173(8) 0.0193(8) 0.0209(8) -0.0028(6) -0.0055(6) -0.0035(6) C23 0.0170(8) 0.0190(8) 0.0176(8) -0.0050(6) -0.0041(6) -0.0048(6) C31 0.0171(8) 0.0161(8) 0.0189(8) -0.0049(6) -0.0067(6) -0.0032(6) C32 0.0202(8) 0.0143(8) 0.0217(8) -0.0038(6) -0.0041(6) -0.0051(6) C33 0.0163(8) 0.0142(8) 0.0205(8) -0.0011(6) -0.0061(6) -0.0049(6) C41 0.0195(8) 0.0193(9) 0.0199(8) -0.0005(6) -0.0101(6) -0.0060(6) C42 0.0225(8) 0.0232(9) 0.0211(8) -0.0050(7) -0.0075(7) -0.0081(6) C43 0.0215(9) 0.0281(10) 0.0250(9) -0.0034(7) -0.0083(7) -0.0082(7) C44 0.0244(9) 0.0215(9) 0.0315(9) 0.0021(7) -0.0128(7) -0.0112(7) C45 0.0288(9) 0.0199(9) 0.0295(9) -0.0045(7) -0.0133(7) -0.0065(7) C46 0.0250(9) 0.0205(9) 0.0215(8) -0.0036(7) -0.0090(7) -0.0057(7) C51 0.0174(8) 0.0214(9) 0.0169(8) -0.0023(6) -0.0072(6) -0.0048(6) C52 0.0248(9) 0.0200(9) 0.0191(8) -0.0027(6) -0.0094(7) -0.0038(6) C53 0.0343(10) 0.0238(9) 0.0232(9) 0.0010(7) -0.0121(7) -0.0118(7) C54 0.0318(10) 0.0349(11) 0.0160(8) 0.0020(7) -0.0057(7) -0.0155(8) C55 0.0287(9) 0.0356(11) 0.0182(8) -0.0089(7) -0.0042(7) -0.0076(7) C56 0.0254(9) 0.0216(9) 0.0197(8) -0.0044(7) -0.0075(7) -0.0057(6) C61 0.0168(8) 0.0179(8) 0.0211(8) -0.0008(6) -0.0079(6) -0.0053(6) C62 0.0251(9) 0.0202(9) 0.0218(8) -0.0043(7) -0.0070(7) -0.0020(6) C63 0.0352(10) 0.0278(10) 0.0180(8) -0.0016(7) -0.0072(7) -0.0038(7) C64 0.0324(10) 0.0206(9) 0.0263(9) 0.0038(7) -0.0087(7) -0.0062(7) C65 0.0258(9) 0.0195(9) 0.0307(9) -0.0067(7) -0.0071(7) -0.0025(7) C66 0.0210(8) 0.0203(9) 0.0210(8) -0.0035(7) -0.0049(7) -0.0043(6) C71 0.0164(8) 0.0153(8) 0.0192(8) -0.0032(6) -0.0023(6) -0.0008(6) C72 0.0176(8) 0.0217(9) 0.0212(8) -0.0060(7) -0.0040(6) -0.0027(6) C73 0.0249(9) 0.0251(9) 0.0177(8) -0.0049(7) -0.0033(7) -0.0014(7) C74 0.0221(9) 0.0194(9) 0.0220(8) -0.0011(7) 0.0014(7) -0.0048(6) C75 0.0209(8) 0.0202(9) 0.0287(9) -0.0048(7) -0.0050(7) -0.0062(6) C76 0.0197(8) 0.0208(9) 0.0220(8) -0.0032(7) -0.0055(7) -0.0038(6) C81 0.0185(8) 0.0203(9) 0.0195(8) -0.0055(6) -0.0074(6) -0.0033(6) C82 0.0209(8) 0.0189(9) 0.0198(8) -0.0058(6) -0.0066(6) -0.0037(6) C83 0.0287(9) 0.0256(9) 0.0172(8) -0.0040(7) -0.0031(7) -0.0069(7) C84 0.0327(10) 0.0280(10) 0.0198(8) -0.0110(7) -0.0028(7) -0.0010(7) C85 0.0366(10) 0.0219(9) 0.0260(9) -0.0097(7) -0.0084(8) -0.0018(7) C86 0.0269(9) 0.0190(9) 0.0227(8) -0.0057(7) -0.0058(7) -0.0055(7) C91 0.0207(8) 0.0148(8) 0.0201(8) -0.0024(6) -0.0038(6) -0.0079(6) C92 0.0204(8) 0.0170(9) 0.0251(8) -0.0040(7) -0.0046(7) -0.0057(6) C93 0.0203(8) 0.0245(9) 0.0295(9) -0.0075(7) 0.0012(7) -0.0089(7) C94 0.0326(10) 0.0243(10) 0.0232(9) 0.0023(7) -0.0022(7) -0.0160(7) C95 0.0285(10) 0.0188(9) 0.0306(9) 0.0044(7) -0.0097(8) -0.0061(7) C96 0.0206(8) 0.0193(9) 0.0274(9) -0.0019(7) -0.0045(7) -0.0042(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 N3 2.1574(13) . ? Fe1 N3 2.1574(13) 2_666 ? Fe1 N1 2.1798(12) 2_666 ? Fe1 N1 2.1799(12) . ? Fe1 N5 2.2700(12) . ? Fe1 N5 2.2701(12) 2_666 ? N1 C11 1.353(2) . ? N1 N2 1.3732(17) . ? N2 C13 1.3637(19) . ? N2 B1 1.559(2) . ? N3 C21 1.354(2) . ? N3 N4 1.3716(17) . ? N4 C23 1.363(2) . ? N4 B1 1.556(2) . ? N5 C31 1.3616(19) . ? N5 N6 1.3765(17) . ? N6 C33 1.359(2) . ? N6 B1 1.542(2) . ? B1 H1 1.0000 . ? C11 C12 1.394(2) . ? C11 C41 1.481(2) . ? C12 C13 1.383(2) . ? C12 H12A 0.9500 . ? C13 C51 1.477(2) . ? C21 C22 1.395(2) . ? C21 C61 1.488(2) . ? C22 C23 1.380(2) . ? C22 H22A 0.9500 . ? C23 C71 1.479(2) . ? C31 C32 1.401(2) . ? C31 C81 1.483(2) . ? C32 C33 1.365(2) . ? C32 H32A 0.9500 . ? C33 C91 1.483(2) . ? C41 C42 1.392(2) . ? C41 C46 1.393(2) . ? C42 C43 1.393(2) . ? C42 H42A 0.9500 . ? C43 C44 1.383(2) . ? C43 H43A 0.9500 . ? C44 C45 1.384(3) . ? C44 H44A 0.9500 . ? C45 C46 1.384(2) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C51 C52 1.395(2) . ? C51 C56 1.397(2) . ? C52 C53 1.385(2) . ? C52 H52A 0.9500 . ? C53 C54 1.384(3) . ? C53 H53A 0.9500 . ? C54 C55 1.384(3) . ? C54 H54A 0.9500 . ? C55 C56 1.391(2) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C61 C62 1.390(2) . ? C61 C66 1.396(2) . ? C62 C63 1.389(2) . ? C62 H62A 0.9500 . ? C63 C64 1.387(3) . ? C63 H63A 0.9500 . ? C64 C65 1.380(3) . ? C64 H64A 0.9500 . ? C65 C66 1.397(2) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C71 C72 1.395(2) . ? C71 C76 1.395(2) . ? C72 C73 1.385(2) . ? C72 H72A 0.9500 . ? C73 C74 1.389(2) . ? C73 H73A 0.9500 . ? C74 C75 1.383(2) . ? C74 H74A 0.9500 . ? C75 C76 1.396(2) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C81 C82 1.394(2) . ? C81 C86 1.401(2) . ? C82 C83 1.387(2) . ? C82 H82A 0.9500 . ? C83 C84 1.386(2) . ? C83 H83A 0.9500 . ? C84 C85 1.381(2) . ? C84 H84A 0.9500 . ? C85 C86 1.381(2) . ? C85 H85A 0.9500 . ? C86 H86A 0.9500 . ? C91 C92 1.395(2) . ? C91 C96 1.395(2) . ? C92 C93 1.388(2) . ? C92 H92A 0.9500 . ? C93 C94 1.387(3) . ? C93 H93A 0.9500 . ? C94 C95 1.380(3) . ? C94 H94A 0.9500 . ? C95 C96 1.385(2) . ? C95 H95A 0.9500 . ? C96 H96A 0.9500 . ? 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 N3 Fe1 N3 180.0 . 2_666 ? N3 Fe1 N1 93.38(5) . 2_666 ? N3 Fe1 N1 86.62(5) 2_666 2_666 ? N3 Fe1 N1 86.62(5) . . ? N3 Fe1 N1 93.38(5) 2_666 . ? N1 Fe1 N1 179.999(7) 2_666 . ? N3 Fe1 N5 91.94(5) . . ? N3 Fe1 N5 88.06(4) 2_666 . ? N1 Fe1 N5 88.66(4) 2_666 . ? N1 Fe1 N5 91.34(4) . . ? N3 Fe1 N5 88.06(5) . 2_666 ? N3 Fe1 N5 91.94(5) 2_666 2_666 ? N1 Fe1 N5 91.34(4) 2_666 2_666 ? N1 Fe1 N5 88.66(4) . 2_666 ? N5 Fe1 N5 180.000(1) . 2_666 ? C11 N1 N2 106.55(12) . . ? C11 N1 Fe1 140.75(10) . . ? N2 N1 Fe1 112.33(9) . . ? C13 N2 N1 109.85(12) . . ? C13 N2 B1 127.75(13) . . ? N1 N2 B1 120.83(12) . . ? C21 N3 N4 106.81(12) . . ? C21 N3 Fe1 140.56(10) . . ? N4 N3 Fe1 112.56(9) . . ? C23 N4 N3 109.53(12) . . ? C23 N4 B1 128.88(13) . . ? N3 N4 B1 121.49(12) . . ? C31 N5 N6 105.75(12) . . ? C31 N5 Fe1 144.44(10) . . ? N6 N5 Fe1 109.80(9) . . ? C33 N6 N5 110.54(12) . . ? C33 N6 B1 126.99(13) . . ? N5 N6 B1 122.31(12) . . ? N6 B1 N4 111.75(12) . . ? N6 B1 N2 111.48(12) . . ? N4 B1 N2 109.33(12) . . ? N6 B1 H1 108.0 . . ? N4 B1 H1 108.0 . . ? N2 B1 H1 108.0 . . ? N1 C11 C12 109.77(13) . . ? N1 C11 C41 124.66(14) . . ? C12 C11 C41 125.44(14) . . ? C13 C12 C11 106.28(14) . . ? C13 C12 H12A 126.9 . . ? C11 C12 H12A 126.9 . . ? N2 C13 C12 107.55(13) . . ? N2 C13 C51 124.83(14) . . ? C12 C13 C51 127.62(14) . . ? N3 C21 C22 109.56(13) . . ? N3 C21 C61 125.19(14) . . ? C22 C21 C61 125.13(14) . . ? C23 C22 C21 106.18(14) . . ? C23 C22 H22A 126.9 . . ? C21 C22 H22A 126.9 . . ? N4 C23 C22 107.89(13) . . ? N4 C23 C71 125.28(14) . . ? C22 C23 C71 126.81(14) . . ? N5 C31 C32 109.24(13) . . ? N5 C31 C81 127.32(14) . . ? C32 C31 C81 123.42(14) . . ? C33 C32 C31 106.95(14) . . ? C33 C32 H32A 126.5 . . ? C31 C32 H32A 126.5 . . ? N6 C33 C32 107.51(13) . . ? N6 C33 C91 126.29(14) . . ? C32 C33 C91 126.14(14) . . ? C42 C41 C46 118.46(14) . . ? C42 C41 C11 123.51(15) . . ? C46 C41 C11 118.02(14) . . ? C41 C42 C43 120.84(15) . . ? C41 C42 H42A 119.6 . . ? C43 C42 H42A 119.6 . . ? C44 C43 C42 119.78(16) . . ? C44 C43 H43A 120.1 . . ? C42 C43 H43A 120.1 . . ? C43 C44 C45 119.90(15) . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C44 C45 C46 120.23(16) . . ? C44 C45 H45A 119.9 . . ? C46 C45 H45A 119.9 . . ? C45 C46 C41 120.76(16) . . ? C45 C46 H46A 119.6 . . ? C41 C46 H46A 119.6 . . ? C52 C51 C56 118.84(15) . . ? C52 C51 C13 122.81(14) . . ? C56 C51 C13 118.35(14) . . ? C53 C52 C51 120.34(16) . . ? C53 C52 H52A 119.8 . . ? C51 C52 H52A 119.8 . . ? C54 C53 C52 120.39(16) . . ? C54 C53 H53A 119.8 . . ? C52 C53 H53A 119.8 . . ? C55 C54 C53 119.98(16) . . ? C55 C54 H54A 120.0 . . ? C53 C54 H54A 120.0 . . ? C54 C55 C56 119.84(16) . . ? C54 C55 H55A 120.1 . . ? C56 C55 H55A 120.1 . . ? C55 C56 C51 120.59(16) . . ? C55 C56 H56A 119.7 . . ? C51 C56 H56A 119.7 . . ? C62 C61 C66 118.37(14) . . ? C62 C61 C21 123.98(14) . . ? C66 C61 C21 117.61(14) . . ? C63 C62 C61 120.85(16) . . ? C63 C62 H62A 119.6 . . ? C61 C62 H62A 119.6 . . ? C64 C63 C62 120.18(16) . . ? C64 C63 H63A 119.9 . . ? C62 C63 H63A 119.9 . . ? C65 C64 C63 119.93(16) . . ? C65 C64 H64A 120.0 . . ? C63 C64 H64A 120.0 . . ? C64 C65 C66 119.79(16) . . ? C64 C65 H65A 120.1 . . ? C66 C65 H65A 120.1 . . ? C61 C66 C65 120.86(15) . . ? C61 C66 H66A 119.6 . . ? C65 C66 H66A 119.6 . . ? C72 C71 C76 119.18(15) . . ? C72 C71 C23 122.58(14) . . ? C76 C71 C23 118.19(14) . . ? C73 C72 C71 120.27(15) . . ? C73 C72 H72A 119.9 . . ? C71 C72 H72A 119.9 . . ? C72 C73 C74 120.36(15) . . ? C72 C73 H73A 119.8 . . ? C74 C73 H73A 119.8 . . ? C75 C74 C73 119.91(15) . . ? C75 C74 H74A 120.0 . . ? C73 C74 H74A 120.0 . . ? C74 C75 C76 119.99(15) . . ? C74 C75 H75A 120.0 . . ? C76 C75 H75A 120.0 . . ? C71 C76 C75 120.27(15) . . ? C71 C76 H76A 119.9 . . ? C75 C76 H76A 119.9 . . ? C82 C81 C86 116.66(15) . . ? C82 C81 C31 125.27(14) . . ? C86 C81 C31 118.05(14) . . ? C83 C82 C81 121.64(15) . . ? C83 C82 H82A 119.2 . . ? C81 C82 H82A 119.2 . . ? C84 C83 C82 120.37(16) . . ? C84 C83 H83A 119.8 . . ? C82 C83 H83A 119.8 . . ? C85 C84 C83 119.03(16) . . ? C85 C84 H84A 120.5 . . ? C83 C84 H84A 120.5 . . ? C84 C85 C86 120.36(16) . . ? C84 C85 H85A 119.8 . . ? C86 C85 H85A 119.8 . . ? C85 C86 C81 121.91(16) . . ? C85 C86 H86A 119.0 . . ? C81 C86 H86A 119.0 . . ? C92 C91 C96 118.59(15) . . ? C92 C91 C33 123.29(14) . . ? C96 C91 C33 118.04(14) . . ? C93 C92 C91 120.21(16) . . ? C93 C92 H92A 119.9 . . ? C91 C92 H92A 119.9 . . ? C94 C93 C92 120.52(16) . . ? C94 C93 H93A 119.7 . . ? C92 C93 H93A 119.7 . . ? C95 C94 C93 119.57(15) . . ? C95 C94 H94A 120.2 . . ? C93 C94 H94A 120.2 . . ? C94 C95 C96 120.22(16) . . ? C94 C95 H95A 119.9 . . ? C96 C95 H95A 119.9 . . ? C95 C96 C91 120.85(16) . . ? C95 C96 H96A 119.6 . . ? C91 C96 H96A 119.6 . . ? 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 N3 Fe1 N1 C11 118.59(17) . . . . ? N3 Fe1 N1 C11 -61.41(17) 2_666 . . . ? N1 Fe1 N1 C11 0(26) 2_666 . . . ? N5 Fe1 N1 C11 -149.54(17) . . . . ? N5 Fe1 N1 C11 30.46(17) 2_666 . . . ? N3 Fe1 N1 N2 -53.03(10) . . . . ? N3 Fe1 N1 N2 126.97(10) 2_666 . . . ? N1 Fe1 N1 N2 -172(26) 2_666 . . . ? N5 Fe1 N1 N2 38.84(10) . . . . ? N5 Fe1 N1 N2 -141.16(10) 2_666 . . . ? C11 N1 N2 C13 0.80(16) . . . . ? Fe1 N1 N2 C13 175.28(9) . . . . ? C11 N1 N2 B1 -166.00(13) . . . . ? Fe1 N1 N2 B1 8.48(16) . . . . ? N3 Fe1 N3 C21 143(40) 2_666 . . . ? N1 Fe1 N3 C21 53.40(16) 2_666 . . . ? N1 Fe1 N3 C21 -126.60(16) . . . . ? N5 Fe1 N3 C21 142.18(16) . . . . ? N5 Fe1 N3 C21 -37.82(16) 2_666 . . . ? N3 Fe1 N3 N4 -40(40) 2_666 . . . ? N1 Fe1 N3 N4 -130.38(9) 2_666 . . . ? N1 Fe1 N3 N4 49.62(9) . . . . ? N5 Fe1 N3 N4 -41.60(9) . . . . ? N5 Fe1 N3 N4 138.40(9) 2_666 . . . ? C21 N3 N4 C23 -1.60(16) . . . . ? Fe1 N3 N4 C23 -179.09(9) . . . . ? C21 N3 N4 B1 175.09(12) . . . . ? Fe1 N3 N4 B1 -2.40(16) . . . . ? N3 Fe1 N5 C31 -139.84(17) . . . . ? N3 Fe1 N5 C31 40.16(17) 2_666 . . . ? N1 Fe1 N5 C31 -46.50(17) 2_666 . . . ? N1 Fe1 N5 C31 133.50(17) . . . . ? N5 Fe1 N5 C31 94(100) 2_666 . . . ? N3 Fe1 N5 N6 41.52(9) . . . . ? N3 Fe1 N5 N6 -138.48(9) 2_666 . . . ? N1 Fe1 N5 N6 134.86(9) 2_666 . . . ? N1 Fe1 N5 N6 -45.14(9) . . . . ? N5 Fe1 N5 N6 -85(100) 2_666 . . . ? C31 N5 N6 C33 -0.25(16) . . . . ? Fe1 N5 N6 C33 178.92(9) . . . . ? C31 N5 N6 B1 -176.00(13) . . . . ? Fe1 N5 N6 B1 3.18(15) . . . . ? C33 N6 B1 N4 121.82(15) . . . . ? N5 N6 B1 N4 -63.17(17) . . . . ? C33 N6 B1 N2 -115.50(16) . . . . ? N5 N6 B1 N2 59.51(17) . . . . ? C23 N4 B1 N6 -120.09(16) . . . . ? N3 N4 B1 N6 63.92(17) . . . . ? C23 N4 B1 N2 116.02(16) . . . . ? N3 N4 B1 N2 -59.98(17) . . . . ? C13 N2 B1 N6 127.09(15) . . . . ? N1 N2 B1 N6 -68.67(17) . . . . ? C13 N2 B1 N4 -108.86(16) . . . . ? N1 N2 B1 N4 55.38(17) . . . . ? N2 N1 C11 C12 -0.56(17) . . . . ? Fe1 N1 C11 C12 -172.48(12) . . . . ? N2 N1 C11 C41 175.38(14) . . . . ? Fe1 N1 C11 C41 3.5(3) . . . . ? N1 C11 C12 C13 0.13(18) . . . . ? C41 C11 C12 C13 -175.78(15) . . . . ? N1 N2 C13 C12 -0.73(17) . . . . ? B1 N2 C13 C12 164.91(14) . . . . ? N1 N2 C13 C51 179.95(14) . . . . ? B1 N2 C13 C51 -14.4(2) . . . . ? C11 C12 C13 N2 0.36(17) . . . . ? C11 C12 C13 C51 179.66(15) . . . . ? N4 N3 C21 C22 1.53(16) . . . . ? Fe1 N3 C21 C22 177.88(12) . . . . ? N4 N3 C21 C61 -174.49(14) . . . . ? Fe1 N3 C21 C61 1.9(3) . . . . ? N3 C21 C22 C23 -0.90(17) . . . . ? C61 C21 C22 C23 175.13(14) . . . . ? N3 N4 C23 C22 1.06(17) . . . . ? B1 N4 C23 C22 -175.32(14) . . . . ? N3 N4 C23 C71 -177.38(14) . . . . ? B1 N4 C23 C71 6.2(2) . . . . ? C21 C22 C23 N4 -0.10(17) . . . . ? C21 C22 C23 C71 178.30(15) . . . . ? N6 N5 C31 C32 0.41(16) . . . . ? Fe1 N5 C31 C32 -178.26(13) . . . . ? N6 N5 C31 C81 178.63(14) . . . . ? Fe1 N5 C31 C81 0.0(3) . . . . ? N5 C31 C32 C33 -0.43(17) . . . . ? C81 C31 C32 C33 -178.73(14) . . . . ? N5 N6 C33 C32 -0.01(17) . . . . ? B1 N6 C33 C32 175.49(14) . . . . ? N5 N6 C33 C91 -177.37(14) . . . . ? B1 N6 C33 C91 -1.9(2) . . . . ? C31 C32 C33 N6 0.26(17) . . . . ? C31 C32 C33 C91 177.63(15) . . . . ? N1 C11 C41 C42 44.0(2) . . . . ? C12 C11 C41 C42 -140.69(17) . . . . ? N1 C11 C41 C46 -136.21(16) . . . . ? C12 C11 C41 C46 39.1(2) . . . . ? C46 C41 C42 C43 1.8(2) . . . . ? C11 C41 C42 C43 -178.45(15) . . . . ? C41 C42 C43 C44 -1.3(2) . . . . ? C42 C43 C44 C45 -0.1(2) . . . . ? C43 C44 C45 C46 1.1(2) . . . . ? C44 C45 C46 C41 -0.6(2) . . . . ? C42 C41 C46 C45 -0.8(2) . . . . ? C11 C41 C46 C45 179.41(14) . . . . ? N2 C13 C51 C52 -45.7(2) . . . . ? C12 C13 C51 C52 135.15(18) . . . . ? N2 C13 C51 C56 134.64(16) . . . . ? C12 C13 C51 C56 -44.5(2) . . . . ? C56 C51 C52 C53 -1.5(2) . . . . ? C13 C51 C52 C53 178.77(15) . . . . ? C51 C52 C53 C54 0.3(3) . . . . ? C52 C53 C54 C55 0.9(3) . . . . ? C53 C54 C55 C56 -0.9(3) . . . . ? C54 C55 C56 C51 -0.3(3) . . . . ? C52 C51 C56 C55 1.5(2) . . . . ? C13 C51 C56 C55 -178.75(15) . . . . ? N3 C21 C61 C62 -54.5(2) . . . . ? C22 C21 C61 C62 130.11(18) . . . . ? N3 C21 C61 C66 127.87(16) . . . . ? C22 C21 C61 C66 -47.5(2) . . . . ? C66 C61 C62 C63 -1.2(2) . . . . ? C21 C61 C62 C63 -178.87(16) . . . . ? C61 C62 C63 C64 1.4(3) . . . . ? C62 C63 C64 C65 -0.9(3) . . . . ? C63 C64 C65 C66 0.1(3) . . . . ? C62 C61 C66 C65 0.5(2) . . . . ? C21 C61 C66 C65 178.30(15) . . . . ? C64 C65 C66 C61 0.0(3) . . . . ? N4 C23 C71 C72 -58.9(2) . . . . ? C22 C23 C71 C72 122.99(18) . . . . ? N4 C23 C71 C76 123.77(17) . . . . ? C22 C23 C71 C76 -54.4(2) . . . . ? C76 C71 C72 C73 -1.4(2) . . . . ? C23 C71 C72 C73 -178.75(15) . . . . ? C71 C72 C73 C74 0.5(2) . . . . ? C72 C73 C74 C75 0.9(3) . . . . ? C73 C74 C75 C76 -1.2(3) . . . . ? C72 C71 C76 C75 1.1(2) . . . . ? C23 C71 C76 C75 178.52(15) . . . . ? C74 C75 C76 C71 0.2(3) . . . . ? N5 C31 C81 C82 4.8(3) . . . . ? C32 C31 C81 C82 -177.21(15) . . . . ? N5 C31 C81 C86 -173.61(15) . . . . ? C32 C31 C81 C86 4.4(2) . . . . ? C86 C81 C82 C83 1.9(2) . . . . ? C31 C81 C82 C83 -176.50(15) . . . . ? C81 C82 C83 C84 -0.6(3) . . . . ? C82 C83 C84 C85 -1.0(3) . . . . ? C83 C84 C85 C86 1.1(3) . . . . ? C84 C85 C86 C81 0.3(3) . . . . ? C82 C81 C86 C85 -1.8(2) . . . . ? C31 C81 C86 C85 176.76(15) . . . . ? N6 C33 C91 C92 -51.9(2) . . . . ? C32 C33 C91 C92 131.16(18) . . . . ? N6 C33 C91 C96 131.30(17) . . . . ? C32 C33 C91 C96 -45.6(2) . . . . ? C96 C91 C92 C93 -2.1(2) . . . . ? C33 C91 C92 C93 -178.81(15) . . . . ? C91 C92 C93 C94 1.6(3) . . . . ? C92 C93 C94 C95 0.2(3) . . . . ? C93 C94 C95 C96 -1.3(3) . . . . ? C94 C95 C96 C91 0.8(3) . . . . ? C92 C91 C96 C95 0.9(2) . . . . ? C33 C91 C96 C95 177.82(15) . . . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 68.0 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.280 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.037