# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_fempbi _audit_creation_date 2013-03-15T15:21:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C82 H68 F12 Fe2 N18 O13 S4' _chemical_formula_sum 'C82 H68 F12 Fe2 N18 O13 S4' _chemical_formula_weight 1981.48 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 19.5327(3) _cell_length_b 10.9126(1) _cell_length_c 39.6368(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8448.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 55239 _cell_measurement_theta_min 1.03 _cell_measurement_theta_max 28.28 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4056 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.935 _exptl_absorpt_correction_T_max 0.937 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'Omega + Phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0963 _diffrn_reflns_av_unetI/netI 0.1684 _diffrn_reflns_number 14563 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.941 _reflns_number_total 14563 _reflns_number_gt 6144 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SIR2004 (Giacovazzo et al, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0914P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 14563 _refine_ls_number_parameters 1180 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.1967 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1928 _refine_ls_wR_factor_gt 0.151 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.94 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.011 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.40(2) _refine_diff_density_max 0.512 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.067 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C -0.0796(4) 0.6473(9) 0.7331(3) 0.063(3) Uani 1 1 d . . . H1 H -0.0609 0.7223 0.7269 0.076 Uiso 1 1 calc R . . C2 C -0.0693(5) 0.5490(11) 0.7125(3) 0.073(3) Uani 1 1 d . . . H2 H -0.0438 0.5572 0.6928 0.088 Uiso 1 1 calc R . . C3 C -0.0981(6) 0.4340(13) 0.7215(3) 0.088(4) Uani 1 1 d . . . H3 H -0.0924 0.3654 0.7079 0.106 Uiso 1 1 calc R . . C4 C -0.1349(5) 0.4275(10) 0.7513(3) 0.071(3) Uani 1 1 d . . . H4 H -0.1552 0.3542 0.7578 0.085 Uiso 1 1 calc R . . C5 C -0.1411(4) 0.5292(9) 0.7711(3) 0.052(2) Uani 1 1 d . . . C6 C -0.1746(4) 0.5389(8) 0.8040(2) 0.050(2) Uani 1 1 d . . . C7 C -0.1978(4) 0.6171(9) 0.8522(3) 0.057(3) Uani 1 1 d . . . C8 C -0.2035(4) 0.6923(10) 0.8820(2) 0.062(3) Uani 1 1 d . . . H8 H -0.1838 0.7697 0.8831 0.074 Uiso 1 1 calc R . . C9 C -0.2395(5) 0.6441(11) 0.9084(3) 0.076(3) Uani 1 1 d . . . H9 H -0.2442 0.6893 0.9281 0.091 Uiso 1 1 calc R . . C10 C -0.2697(6) 0.5266(12) 0.9062(3) 0.093(4) Uani 1 1 d . . . H10 H -0.2941 0.4979 0.9247 0.112 Uiso 1 1 calc R . . C11 C -0.2650(5) 0.4502(10) 0.8776(3) 0.072(3) Uani 1 1 d . . . H11 H -0.2848 0.3728 0.8764 0.087 Uiso 1 1 calc R . . C12 C -0.2277(4) 0.5027(9) 0.8514(3) 0.054(2) Uani 1 1 d . . . C13 C -0.2388(5) 0.3333(7) 0.8077(3) 0.068(3) Uani 1 1 d . . . H13A H -0.2619 0.291 0.8256 0.102 Uiso 1 1 calc R . . H13B H -0.202 0.2834 0.7993 0.102 Uiso 1 1 calc R . . H13C H -0.2705 0.3496 0.7897 0.102 Uiso 1 1 calc R . . C14 C -0.1334(4) 0.9774(10) 0.7407(3) 0.068(3) Uani 1 1 d . . . H14 H -0.1807 0.9686 0.7411 0.082 Uiso 1 1 calc R . . C15 C -0.1066(6) 1.0581(12) 0.7174(3) 0.086(4) Uani 1 1 d . . . H15 H -0.1346 1.0967 0.7017 0.103 Uiso 1 1 calc R . . C16 C -0.0377(7) 1.0802(11) 0.7180(3) 0.103(4) Uani 1 1 d . . . H16 H -0.0169 1.1322 0.7025 0.124 Uiso 1 1 calc R . . C17 C 0.0007(5) 1.0193(9) 0.7438(3) 0.073(3) Uani 1 1 d . . . H17 H 0.0471 1.0359 0.7464 0.087 Uiso 1 1 calc R . . C18 C -0.0306(4) 0.9369(8) 0.7645(3) 0.055(2) Uani 1 1 d . . . C19 C 0.0024(4) 0.8687(7) 0.7914(2) 0.044(2) Uani 1 1 d . . . C20 C 0.0060(5) 0.7344(8) 0.8316(3) 0.055(3) Uani 1 1 d . . . C21 C -0.0079(4) 0.6403(8) 0.8553(2) 0.059(2) Uani 1 1 d . . . H21 H -0.0505 0.6023 0.8566 0.071 Uiso 1 1 calc R . . C22 C 0.0455(5) 0.6085(9) 0.8763(3) 0.068(3) Uani 1 1 d . . . H22 H 0.0392 0.5481 0.8925 0.081 Uiso 1 1 calc R . . C23 C 0.1091(5) 0.6663(10) 0.8733(3) 0.076(3) Uani 1 1 d . . . H23 H 0.1448 0.6412 0.8873 0.091 Uiso 1 1 calc R . . C24 C 0.1204(6) 0.7560(11) 0.8513(3) 0.074(4) Uani 1 1 d . . . H24 H 0.162 0.7973 0.8508 0.088 Uiso 1 1 calc R . . C25 C 0.0702(4) 0.7847(8) 0.8300(3) 0.052(2) Uani 1 1 d . . . C26 C 0.1245(4) 0.9577(8) 0.7955(3) 0.075(3) Uani 1 1 d . . . H26A H 0.164 0.9387 0.8089 0.112 Uiso 1 1 calc R . . H26B H 0.1102 1.0402 0.8001 0.112 Uiso 1 1 calc R . . H26C H 0.1357 0.9497 0.772 0.112 Uiso 1 1 calc R . . C27 C -0.1214(4) 0.9570(9) 0.8524(3) 0.061(3) Uani 1 1 d . . . H27 H -0.0758 0.9329 0.8534 0.073 Uiso 1 1 calc R . . C28 C -0.1459(6) 1.0385(9) 0.8766(3) 0.078(3) Uani 1 1 d . . . H28 H -0.1168 1.0684 0.8932 0.093 Uiso 1 1 calc R . . C29 C -0.2117(6) 1.0740(8) 0.8758(3) 0.074(3) Uani 1 1 d . . . H29 H -0.2288 1.1271 0.8922 0.089 Uiso 1 1 calc R . . C30 C -0.2537(5) 1.0304(9) 0.8506(3) 0.062(3) Uani 1 1 d . . . H30 H -0.2997 1.052 0.8499 0.074 Uiso 1 1 calc R . . C31 C -0.2265(4) 0.9550(8) 0.8266(3) 0.054(2) Uani 1 1 d . . . C32 C -0.2612(4) 0.8931(7) 0.7967(2) 0.046(2) Uani 1 1 d . . . C33 C -0.2735(5) 0.7704(8) 0.7558(3) 0.051(3) Uani 1 1 d . . . C34 C -0.2672(5) 0.6858(9) 0.7294(2) 0.063(3) Uani 1 1 d . . . H34 H -0.2266 0.6427 0.7262 0.076 Uiso 1 1 calc R . . C35 C -0.3227(5) 0.6681(9) 0.7084(3) 0.078(3) Uani 1 1 d . . . H35 H -0.3204 0.6097 0.6913 0.094 Uiso 1 1 calc R . . C36 C -0.3815(5) 0.7364(11) 0.7126(4) 0.075(4) Uani 1 1 d . . . H36 H -0.4177 0.7232 0.6977 0.09 Uiso 1 1 calc R . . C37 C -0.3892(5) 0.8191(10) 0.7363(3) 0.070(3) Uani 1 1 d . . . H37 H -0.4301 0.8617 0.7386 0.084 Uiso 1 1 calc R . . C38 C -0.3342(4) 0.8415(8) 0.7579(2) 0.047(2) Uani 1 1 d . . . C39 C -0.3727(5) 1.0093(9) 0.7961(3) 0.072(3) Uani 1 1 d . . . H39A H -0.4137 1.003 0.7829 0.108 Uiso 1 1 calc R . . H39B H -0.3528 1.089 0.793 0.108 Uiso 1 1 calc R . . H39C H -0.3835 0.9975 0.8195 0.108 Uiso 1 1 calc R . . C40 C -0.1241(5) 0.5422(10) 0.9842(3) 0.073(3) Uani 1 1 d . . . H40 H -0.1701 0.5641 0.984 0.088 Uiso 1 1 calc R . . C41 C -0.1011(5) 0.4644(9) 0.9589(3) 0.067(3) Uani 1 1 d . . . H41 H -0.1299 0.4387 0.9416 0.081 Uiso 1 1 calc R . . C42 C -0.0331(6) 0.4265(9) 0.9605(3) 0.072(3) Uani 1 1 d . . . H42 H -0.015 0.375 0.9441 0.087 Uiso 1 1 calc R . . C43 C 0.0058(5) 0.4663(8) 0.9864(3) 0.060(3) Uani 1 1 d . . . H43 H 0.0511 0.4407 0.9878 0.072 Uiso 1 1 calc R . . C44 C -0.0194(5) 0.5424(8) 1.0102(2) 0.056(2) Uani 1 1 d . . . C45 C 0.0173(4) 0.5956(7) 1.0379(2) 0.052(2) Uani 1 1 d . . . C46 C 0.0323(4) 0.7171(9) 1.0831(3) 0.053(2) Uani 1 1 d . . . C47 C 0.0256(4) 0.8027(10) 1.1081(3) 0.068(3) Uani 1 1 d . . . H47 H -0.0138 0.8494 1.111 0.081 Uiso 1 1 calc R . . C48 C 0.0828(5) 0.8139(11) 1.1287(3) 0.084(3) Uani 1 1 d . . . H48 H 0.0811 0.8693 1.1466 0.101 Uiso 1 1 calc R . . C49 C 0.1440(6) 0.7445(11) 1.1240(4) 0.084(4) Uani 1 1 d . . . H49 H 0.1812 0.7565 1.1382 0.1 Uiso 1 1 calc R . . C50 C 0.1480(5) 0.6626(10) 1.0991(3) 0.076(3) Uani 1 1 d . . . H50 H 0.1875 0.6165 1.0961 0.091 Uiso 1 1 calc R . . C51 C 0.0914(4) 0.6466(9) 1.0774(3) 0.059(2) Uani 1 1 d . . . C52 C 0.1315(4) 0.4771(9) 1.0408(3) 0.090(4) Uani 1 1 d . . . H52A H 0.1145 0.4327 1.0216 0.135 Uiso 1 1 calc R . . H52B H 0.1395 0.4212 1.0591 0.135 Uiso 1 1 calc R . . H52C H 0.1736 0.5171 1.0349 0.135 Uiso 1 1 calc R . . C53 C -0.1591(4) 0.8429(9) 1.1065(2) 0.062(3) Uani 1 1 d . . . H53 H -0.1739 0.7665 1.114 0.074 Uiso 1 1 calc R . . C54 C -0.1716(5) 0.9414(10) 1.1269(3) 0.077(3) Uani 1 1 d . . . H54 H -0.1956 0.9329 1.1471 0.092 Uiso 1 1 calc R . . C55 C -0.1476(6) 1.0522(10) 1.1167(3) 0.086(4) Uani 1 1 d . . . H55 H -0.153 1.1203 1.1305 0.103 Uiso 1 1 calc R . . C56 C -0.1155(5) 1.0642(9) 1.0862(3) 0.075(3) Uani 1 1 d . . . H56 H -0.1013 1.1408 1.0786 0.09 Uiso 1 1 calc R . . C57 C -0.1046(4) 0.9624(8) 1.0670(2) 0.055(2) Uani 1 1 d . . . C58 C -0.0730(4) 0.9592(8) 1.0335(2) 0.043(2) Uani 1 1 d . . . C59 C -0.0468(4) 0.8823(8) 0.9847(2) 0.051(2) Uani 1 1 d . . . C60 C -0.0416(4) 0.8114(9) 0.9563(3) 0.064(3) Uani 1 1 d . . . H60 H -0.0609 0.7337 0.9546 0.077 Uiso 1 1 calc R . . C61 C -0.0048(6) 0.8660(12) 0.9300(3) 0.080(3) Uani 1 1 d . . . H61 H 0.0007 0.8215 0.9102 0.096 Uiso 1 1 calc R . . C62 C 0.0228(5) 0.9769(11) 0.9315(3) 0.077(3) Uani 1 1 d . . . H62 H 0.0464 1.0073 0.9129 0.092 Uiso 1 1 calc R . . C63 C 0.0172(5) 1.0469(10) 0.9597(3) 0.073(3) Uani 1 1 d . . . H63 H 0.0381 1.1233 0.9609 0.088 Uiso 1 1 calc R . . C64 C -0.0204(4) 1.0017(9) 0.9864(3) 0.055(3) Uani 1 1 d . . . C65 C -0.0132(5) 1.1654(8) 1.0298(3) 0.074(3) Uani 1 1 d . . . H65A H 0.0128 1.2063 1.0126 0.111 Uiso 1 1 calc R . . H65B H 0.0146 1.1547 1.0495 0.111 Uiso 1 1 calc R . . H65C H -0.0527 1.2138 1.0354 0.111 Uiso 1 1 calc R . . C66 C -0.1071(5) 0.5156(10) 1.0980(3) 0.069(3) Uani 1 1 d . . . H66 H -0.0601 0.5285 1.0986 0.082 Uiso 1 1 calc R . . C67 C -0.1357(6) 0.4347(10) 1.1206(3) 0.075(4) Uani 1 1 d . . . H67 H -0.1086 0.3925 1.136 0.09 Uiso 1 1 calc R . . C68 C -0.2058(6) 0.4178(9) 1.1199(3) 0.091(4) Uani 1 1 d . . . H68 H -0.2266 0.3642 1.135 0.11 Uiso 1 1 calc R . . C69 C -0.2452(5) 0.4818(9) 1.0964(3) 0.071(3) Uani 1 1 d . . . H69 H -0.2926 0.4735 1.0961 0.085 Uiso 1 1 calc R . . C70 C -0.2132(5) 0.5566(8) 1.0738(2) 0.063(3) Uani 1 1 d . . . C71 C -0.2458(4) 0.6293(7) 1.0472(2) 0.046(2) Uani 1 1 d . . . C72 C -0.2498(5) 0.7628(8) 1.0071(3) 0.051(3) Uani 1 1 d . . . C73 C -0.2366(5) 0.8549(8) 0.9844(3) 0.063(3) Uani 1 1 d . . . H73 H -0.1943 0.8939 0.9834 0.075 Uiso 1 1 calc R . . C74 C -0.2905(5) 0.8866(11) 0.9629(3) 0.078(3) Uani 1 1 d . . . H74 H -0.2833 0.9478 0.947 0.093 Uiso 1 1 calc R . . C75 C -0.3538(6) 0.8311(12) 0.9644(3) 0.085(3) Uani 1 1 d . . . H75 H -0.3871 0.8549 0.9489 0.102 Uiso 1 1 calc R . . C76 C -0.3699(5) 0.7428(10) 0.9874(4) 0.076(4) Uani 1 1 d . . . H76 H -0.4133 0.7082 0.9889 0.091 Uiso 1 1 calc R . . C77 C -0.3144(4) 0.7073(9) 1.0093(2) 0.051(2) Uani 1 1 d . . . C78 C -0.3649(4) 0.5402(10) 1.0448(3) 0.077(3) Uani 1 1 d . . . H78A H -0.4062 0.5603 1.0329 0.116 Uiso 1 1 calc R . . H78B H -0.373 0.5461 1.0687 0.116 Uiso 1 1 calc R . . H78C H -0.3513 0.4582 1.0393 0.116 Uiso 1 1 calc R . . C79 C -0.0193(6) 1.2702(10) 0.8222(3) 0.076(3) Uani 1 1 d U . . C80 C 0.1326(10) 1.3212(14) 0.7018(3) 0.140(5) Uani 1 1 d DU . . C81 C -0.2245(8) 0.2236(13) 1.0116(5) 0.142(6) Uani 1 1 d U . . C82 C -0.3738(8) 0.2135(16) 1.1306(6) 0.164(7) Uani 1 1 d U . . N1 N -0.1150(3) 0.6408(7) 0.7614(2) 0.055(2) Uani 1 1 d . . . N2 N -0.1646(3) 0.6400(7) 0.8222(2) 0.054(2) Uani 1 1 d . . . N3 N -0.2108(3) 0.4507(6) 0.8206(2) 0.056(2) Uani 1 1 d . . . N4 N -0.0973(3) 0.9111(7) 0.7624(2) 0.058(2) Uani 1 1 d . . . N5 N -0.0367(4) 0.7845(7) 0.8075(2) 0.055(2) Uani 1 1 d . . . N6 N 0.0676(3) 0.8709(7) 0.80417(19) 0.058(2) Uani 1 1 d . . . N7 N -0.1607(3) 0.9122(6) 0.82781(19) 0.0494(19) Uani 1 1 d . . . N8 N -0.2293(3) 0.8063(6) 0.77954(19) 0.053(2) Uani 1 1 d . . . N9 N -0.3246(3) 0.9168(6) 0.7854(2) 0.055(2) Uani 1 1 d . . . N10 N -0.0850(4) 0.5878(6) 1.0087(2) 0.055(2) Uani 1 1 d . . . N11 N -0.0133(3) 0.6830(6) 1.05657(16) 0.0467(17) Uani 1 1 d . . . N12 N 0.0810(3) 0.5690(7) 1.0511(2) 0.0554(19) Uani 1 1 d . . . N13 N -0.1275(3) 0.8477(6) 1.0766(2) 0.0495(19) Uani 1 1 d . . . N14 N -0.0794(3) 0.8577(6) 1.01536(19) 0.0457(19) Uani 1 1 d . . . N15 N -0.0348(3) 1.0488(7) 1.0176(2) 0.055(2) Uani 1 1 d . . . N16 N -0.1449(4) 0.5770(7) 1.0749(2) 0.057(2) Uani 1 1 d . . . N17 N -0.2093(3) 0.7120(7) 1.0311(2) 0.056(2) Uani 1 1 d . . . N18 N -0.3114(3) 0.6247(7) 1.0353(2) 0.062(2) Uani 1 1 d . . . O1 O 0.0311(4) 1.0820(6) 0.85124(19) 0.089(2) Uani 1 1 d . . . O2 O 0.0073(7) 1.2579(8) 0.8856(3) 0.147(5) Uani 1 1 d . . . O1W O 0.1301(6) 1.3951(7) 0.9178(3) 0.139(3) Uani 1 1 d . . . H1W1 H 0.1223 1.3584 0.8978 0.208 Uiso 1 1 d R . . H2W1 H 0.1652 1.3554 0.9277 0.208 Uiso 1 1 d R . . O3 O 0.1007(4) 1.2673(8) 0.8492(3) 0.125(4) Uani 1 1 d . . . O4 O 0.1797(8) 1.1424(10) 0.7218(4) 0.247(8) Uani 1 1 d . . . O5 O 0.2390(7) 1.2584(14) 0.6838(4) 0.223(9) Uani 1 1 d . . . O6 O 0.2302(4) 1.3331(9) 0.7401(3) 0.120(3) Uani 1 1 d . . . O7 O -0.3421(5) 0.2405(8) 0.9920(4) 0.199(8) Uani 1 1 d . . . O8 O -0.2478(9) 0.2435(10) 0.9528(4) 0.217(8) Uani 1 1 d . . . O9 O -0.2733(4) 0.4209(6) 0.9859(2) 0.093(2) Uani 1 1 d . . . O10 O -0.4472(7) 0.3817(9) 1.1111(3) 0.177(5) Uani 1 1 d . . . O11 O -0.4911(5) 0.2462(12) 1.1550(3) 0.185(7) Uani 1 1 d . . . O12 O -0.4711(6) 0.1608(11) 1.0962(3) 0.192(6) Uani 1 1 d . . . Fe1 Fe -0.13258(5) 0.78099(11) 0.79460(3) 0.0499(3) Uani 1 1 d . . . Fe2 Fe -0.11038(5) 0.71257(11) 1.04391(3) 0.0477(3) Uani 1 1 d . . . S1 S 0.03635(14) 1.2124(3) 0.85483(8) 0.0742(8) Uani 1 1 d . . . S2 S 0.2052(2) 1.2574(4) 0.71504(13) 0.1009(13) Uani 1 1 d . . . S3 S -0.28070(15) 0.2931(3) 0.98323(9) 0.0871(9) Uani 1 1 d . . . S4 S -0.4541(3) 0.2612(5) 1.12623(17) 0.156(2) Uani 1 1 d . . . F1 F -0.0749(4) 1.2219(8) 0.8198(3) 0.184(4) Uani 1 1 d U . . F2 F 0.0142(6) 1.2485(7) 0.7933(2) 0.156(3) Uani 1 1 d U . . F3 F -0.0245(4) 1.3896(6) 0.8213(2) 0.124(2) Uani 1 1 d U . . F4 F 0.0954(5) 1.2589(9) 0.6786(2) 0.153(3) Uani 1 1 d U . . F5 F 0.0854(5) 1.3358(14) 0.7241(3) 0.218(5) Uani 1 1 d U . . F6 F 0.1396(10) 1.4353(11) 0.6915(4) 0.312(8) Uani 1 1 d DU . . F7 F -0.1617(6) 0.2602(16) 1.0046(8) 0.545(19) Uani 1 1 d U . . F8 F -0.2207(4) 0.1145(7) 1.0152(2) 0.142(3) Uani 1 1 d U . . F9 F -0.2200(15) 0.2696(13) 1.0368(5) 0.452(14) Uani 1 1 d U . . F10 F -0.3670(5) 0.1007(13) 1.1424(3) 0.223(5) Uani 1 1 d U . . F11 F -0.3533(7) 0.303(2) 1.1582(4) 0.321(9) Uani 1 1 d U . . F12 F -0.3336(5) 0.2210(10) 1.1057(3) 0.195(5) Uani 1 1 d U . . 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 C1 0.042(5) 0.079(7) 0.070(8) -0.008(6) -0.004(5) 0.003(5) C2 0.065(6) 0.104(9) 0.051(7) -0.019(6) 0.017(5) -0.003(6) C3 0.104(9) 0.103(10) 0.056(10) -0.011(7) 0.010(7) 0.005(7) C4 0.084(7) 0.059(7) 0.070(9) -0.014(6) 0.002(6) 0.003(5) C5 0.048(5) 0.051(6) 0.055(7) 0.010(5) -0.013(5) -0.002(4) C6 0.043(5) 0.062(6) 0.047(7) 0.004(5) -0.002(4) 0.004(4) C7 0.038(5) 0.089(8) 0.043(7) 0.002(6) -0.006(5) 0.009(5) C8 0.059(6) 0.092(8) 0.035(7) 0.024(6) -0.011(5) 0.007(5) C9 0.078(7) 0.091(9) 0.059(8) 0.004(7) -0.014(6) 0.014(6) C10 0.107(9) 0.113(11) 0.060(9) 0.038(8) 0.024(7) 0.015(8) C11 0.061(6) 0.070(7) 0.086(10) 0.015(7) 0.011(6) 0.013(5) C12 0.049(5) 0.054(6) 0.060(8) 0.002(6) 0.005(5) 0.000(5) C13 0.083(6) 0.035(5) 0.087(8) -0.005(5) -0.003(6) -0.012(4) C14 0.051(6) 0.067(7) 0.086(10) 0.006(6) 0.003(6) 0.013(5) C15 0.072(8) 0.121(10) 0.064(9) 0.042(8) -0.004(6) -0.006(7) C16 0.108(10) 0.097(9) 0.104(11) 0.048(8) 0.027(8) -0.002(7) C17 0.068(6) 0.059(6) 0.090(9) 0.012(6) 0.002(6) -0.002(5) C18 0.053(6) 0.041(5) 0.070(8) -0.010(5) 0.013(5) 0.001(4) C19 0.037(4) 0.056(5) 0.038(6) -0.006(5) -0.006(4) 0.001(4) C20 0.061(6) 0.052(6) 0.052(9) -0.003(5) -0.005(6) 0.017(5) C21 0.051(5) 0.072(7) 0.055(7) 0.002(5) -0.010(5) 0.006(5) C22 0.067(6) 0.074(7) 0.063(7) 0.011(5) -0.004(5) -0.009(5) C23 0.072(7) 0.084(8) 0.072(9) -0.023(7) 0.001(6) 0.020(6) C24 0.071(7) 0.115(10) 0.035(9) -0.006(6) 0.003(6) 0.015(6) C25 0.041(5) 0.050(5) 0.064(8) 0.003(5) -0.007(5) 0.002(4) C26 0.032(4) 0.087(7) 0.105(9) 0.005(7) 0.016(6) -0.016(5) C27 0.053(5) 0.065(7) 0.064(8) -0.011(6) -0.012(5) 0.004(5) C28 0.095(9) 0.065(7) 0.073(9) -0.012(6) -0.012(6) -0.008(6) C29 0.080(8) 0.048(6) 0.095(10) -0.019(6) 0.023(7) -0.011(5) C30 0.055(6) 0.061(7) 0.070(8) -0.003(6) 0.028(6) -0.001(5) C31 0.038(5) 0.066(6) 0.057(7) 0.014(5) -0.003(5) -0.005(4) C32 0.045(5) 0.045(5) 0.047(6) 0.013(4) -0.006(5) -0.012(4) C33 0.057(6) 0.052(5) 0.045(7) -0.016(5) -0.009(5) -0.019(5) C34 0.075(6) 0.081(7) 0.033(6) -0.001(5) -0.021(5) 0.020(5) C35 0.080(7) 0.079(7) 0.075(9) -0.003(6) -0.018(6) -0.007(6) C36 0.052(7) 0.113(10) 0.060(10) 0.005(7) -0.022(6) 0.003(6) C37 0.049(6) 0.094(8) 0.065(8) 0.018(6) -0.005(5) 0.016(5) C38 0.044(5) 0.046(5) 0.052(6) 0.012(5) -0.003(4) 0.003(4) C39 0.064(5) 0.079(7) 0.073(8) 0.018(6) 0.021(6) 0.012(5) C40 0.049(6) 0.090(8) 0.081(9) -0.013(7) -0.004(6) -0.022(5) C41 0.073(7) 0.065(7) 0.064(8) -0.027(6) -0.015(5) -0.012(5) C42 0.092(8) 0.071(7) 0.055(8) -0.007(6) 0.017(6) 0.007(6) C43 0.061(6) 0.054(6) 0.063(8) -0.005(6) 0.011(6) 0.006(5) C44 0.064(6) 0.059(6) 0.045(7) -0.015(5) 0.017(5) -0.011(5) C45 0.049(5) 0.051(5) 0.056(7) -0.002(5) 0.018(5) 0.001(4) C46 0.055(6) 0.074(6) 0.031(6) 0.015(5) -0.011(4) 0.012(5) C47 0.048(5) 0.091(8) 0.064(8) -0.013(6) -0.005(5) -0.007(5) C48 0.074(7) 0.136(10) 0.042(7) -0.020(6) -0.019(6) -0.020(7) C49 0.055(7) 0.124(12) 0.072(12) 0.006(7) -0.018(6) 0.003(6) C50 0.049(6) 0.109(9) 0.070(9) 0.000(7) -0.016(5) -0.013(5) C51 0.046(5) 0.063(6) 0.068(8) 0.014(5) -0.004(5) 0.000(4) C52 0.061(6) 0.091(7) 0.118(10) -0.012(7) 0.005(7) 0.047(5) C53 0.064(6) 0.072(7) 0.048(7) 0.014(5) 0.013(5) -0.013(5) C54 0.099(8) 0.076(8) 0.055(8) -0.010(6) 0.021(6) 0.016(6) C55 0.144(11) 0.039(6) 0.075(10) -0.012(6) 0.037(8) -0.008(6) C56 0.109(8) 0.055(7) 0.061(9) -0.012(6) 0.005(6) -0.009(5) C57 0.070(6) 0.050(6) 0.045(7) -0.010(5) 0.001(5) 0.009(4) C58 0.040(4) 0.059(6) 0.029(6) 0.009(4) -0.009(4) 0.006(4) C59 0.039(5) 0.061(6) 0.051(7) 0.002(5) 0.007(4) 0.003(4) C60 0.059(6) 0.073(7) 0.059(8) -0.034(6) -0.002(5) 0.001(5) C61 0.103(8) 0.102(10) 0.035(7) 0.011(6) 0.012(6) 0.003(7) C62 0.089(8) 0.090(9) 0.051(9) 0.023(7) 0.016(6) 0.001(6) C63 0.083(7) 0.080(8) 0.057(9) 0.013(6) -0.005(6) -0.009(6) C64 0.052(6) 0.068(7) 0.043(7) 0.015(5) -0.001(5) -0.003(5) C65 0.074(6) 0.053(6) 0.095(9) 0.007(5) -0.001(6) -0.023(5) C66 0.076(7) 0.074(7) 0.056(8) 0.026(6) -0.017(5) 0.007(5) C67 0.073(8) 0.065(7) 0.088(11) 0.011(7) -0.004(6) -0.012(6) C68 0.098(9) 0.063(7) 0.113(12) 0.028(7) -0.007(7) -0.007(6) C69 0.054(6) 0.073(7) 0.086(9) 0.017(6) -0.009(6) 0.001(5) C70 0.092(8) 0.051(6) 0.045(7) -0.001(5) -0.001(5) 0.007(5) C71 0.041(5) 0.045(5) 0.053(6) -0.005(5) 0.004(4) 0.000(4) C72 0.046(6) 0.066(7) 0.041(8) -0.006(5) -0.014(5) 0.014(5) C73 0.077(7) 0.053(6) 0.057(7) -0.009(5) 0.000(5) 0.016(5) C74 0.059(7) 0.118(9) 0.056(7) -0.002(6) -0.011(5) 0.029(6) C75 0.073(8) 0.133(11) 0.048(7) -0.004(7) -0.025(6) 0.028(7) C76 0.050(6) 0.088(9) 0.091(13) -0.021(7) -0.019(7) 0.022(5) C77 0.056(6) 0.059(6) 0.039(6) -0.024(5) -0.007(4) 0.004(5) C78 0.049(5) 0.110(8) 0.073(8) -0.008(7) -0.006(6) -0.022(5) C79 0.084(6) 0.074(5) 0.069(7) 0.003(6) -0.024(5) -0.011(5) C80 0.246(18) 0.137(9) 0.036(9) -0.021(7) -0.017(7) 0.008(12) C81 0.122(9) 0.070(5) 0.233(16) -0.040(11) -0.102(9) -0.036(8) C82 0.120(13) 0.148(12) 0.222(18) -0.038(10) 0.137(13) -0.051(9) N1 0.036(4) 0.066(6) 0.061(6) -0.008(4) -0.001(4) 0.010(4) N2 0.041(4) 0.074(6) 0.047(6) -0.004(4) -0.002(4) -0.003(4) N3 0.053(4) 0.052(5) 0.064(6) 0.007(4) 0.002(4) 0.000(4) N4 0.035(4) 0.057(5) 0.082(7) 0.000(4) -0.010(4) 0.006(3) N5 0.059(4) 0.055(4) 0.051(6) -0.024(4) 0.016(4) -0.013(4) N6 0.046(4) 0.069(5) 0.059(6) -0.013(4) 0.002(4) 0.006(4) N7 0.050(5) 0.044(4) 0.054(6) -0.006(4) -0.012(4) -0.011(3) N8 0.051(4) 0.044(4) 0.063(6) 0.002(4) 0.018(4) 0.006(3) N9 0.048(4) 0.042(4) 0.074(7) 0.013(4) 0.004(4) 0.000(3) N10 0.035(4) 0.054(5) 0.076(7) 0.011(4) -0.002(4) 0.004(4) N11 0.048(4) 0.056(5) 0.036(5) -0.011(3) -0.012(3) -0.002(3) N12 0.040(4) 0.068(5) 0.059(6) 0.000(4) 0.008(4) 0.008(3) N13 0.052(4) 0.045(5) 0.052(6) 0.004(4) -0.007(4) 0.005(3) N14 0.040(4) 0.048(5) 0.049(5) -0.016(4) -0.009(3) -0.001(3) N15 0.055(4) 0.057(5) 0.053(6) 0.000(4) -0.009(4) -0.006(4) N16 0.053(5) 0.056(5) 0.061(6) -0.010(4) -0.011(4) 0.000(4) N17 0.050(4) 0.055(4) 0.064(6) 0.002(4) -0.013(4) 0.005(4) N18 0.036(4) 0.072(5) 0.077(7) -0.017(5) -0.005(4) -0.005(4) O1 0.145(6) 0.045(4) 0.078(6) 0.009(3) 0.011(5) 0.018(4) O2 0.274(14) 0.104(8) 0.062(8) -0.029(5) -0.033(8) 0.048(7) O1W 0.174(7) 0.116(6) 0.126(7) -0.012(6) -0.062(6) 0.006(7) O3 0.075(5) 0.132(7) 0.167(10) 0.076(6) -0.043(6) -0.040(5) O4 0.323(18) 0.072(8) 0.35(2) 0.045(10) -0.123(15) -0.029(9) O5 0.154(10) 0.31(2) 0.205(17) -0.141(13) 0.097(11) -0.058(10) O6 0.093(6) 0.159(9) 0.109(8) -0.012(6) -0.022(5) -0.015(5) O7 0.074(6) 0.108(8) 0.42(2) 0.117(10) -0.003(9) -0.012(5) O8 0.36(2) 0.155(12) 0.135(13) -0.059(8) 0.143(13) -0.004(10) O9 0.117(6) 0.059(5) 0.103(7) 0.008(4) -0.018(5) -0.009(4) O10 0.279(14) 0.105(7) 0.147(10) 0.057(7) -0.062(9) -0.008(7) O11 0.067(6) 0.38(2) 0.111(10) 0.054(9) 0.046(6) 0.028(7) O12 0.225(12) 0.171(11) 0.180(13) -0.065(9) -0.011(9) -0.091(9) Fe1 0.0391(6) 0.0541(7) 0.0564(10) -0.0087(9) -0.0011(6) -0.0012(6) Fe2 0.0399(6) 0.0496(7) 0.0535(9) -0.0008(8) -0.0027(6) -0.0025(6) S1 0.0758(18) 0.0689(18) 0.078(2) 0.0074(19) -0.0036(15) -0.0091(15) S2 0.083(2) 0.129(3) 0.091(3) -0.027(2) -0.007(2) 0.0098(19) S3 0.090(2) 0.071(2) 0.101(3) 0.009(2) -0.0143(19) -0.0047(17) S4 0.114(4) 0.212(6) 0.142(6) 0.087(4) 0.017(3) 0.028(3) F1 0.103(5) 0.194(7) 0.254(11) 0.137(8) -0.100(5) -0.074(5) F2 0.278(9) 0.136(6) 0.055(5) 0.006(4) 0.034(6) 0.008(5) F3 0.139(5) 0.079(4) 0.154(7) 0.017(4) -0.037(5) 0.027(3) F4 0.148(6) 0.214(8) 0.095(7) -0.059(6) -0.035(5) 0.035(5) F5 0.146(8) 0.362(14) 0.148(9) -0.139(9) -0.040(6) 0.067(8) F6 0.52(2) 0.123(8) 0.295(17) 0.019(8) -0.097(13) 0.017(10) F7 0.106(7) 0.37(2) 1.16(5) 0.44(3) -0.222(15) -0.119(10) F8 0.146(6) 0.069(4) 0.211(9) -0.002(5) -0.040(6) 0.006(4) F9 0.87(4) 0.173(12) 0.319(18) -0.128(13) -0.43(2) 0.159(18) F10 0.147(8) 0.294(11) 0.227(12) 0.103(9) 0.064(7) 0.099(9) F11 0.230(13) 0.54(2) 0.196(14) -0.163(16) 0.042(11) -0.151(16) F12 0.172(8) 0.285(11) 0.128(8) -0.032(7) 0.092(7) -0.103(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.320(12) . ? C1 C2 1.362(13) . ? C1 H1 0.93 . ? C2 C3 1.421(15) . ? C2 H2 0.93 . ? C3 C4 1.384(15) . ? C3 H3 0.93 . ? C4 C5 1.365(13) . ? C4 H4 0.93 . ? C5 N1 1.375(11) . ? C5 C6 1.463(13) . ? C6 N2 1.333(10) . ? C6 N3 1.364(10) . ? C7 N2 1.378(11) . ? C7 C12 1.378(12) . ? C7 C8 1.440(13) . ? C8 C9 1.366(13) . ? C8 H8 0.93 . ? C9 C10 1.415(15) . ? C9 H9 0.93 . ? C10 C11 1.409(16) . ? C10 H10 0.93 . ? C11 C12 1.391(13) . ? C11 H11 0.93 . ? C12 N3 1.387(12) . ? C13 N3 1.484(10) . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? C14 N4 1.328(12) . ? C14 C15 1.377(15) . ? C14 H14 0.93 . ? C15 C16 1.366(15) . ? C15 H15 0.93 . ? C16 C17 1.431(14) . ? C16 H16 0.93 . ? C17 C18 1.363(13) . ? C17 H17 0.93 . ? C18 N4 1.336(10) . ? C18 C19 1.451(12) . ? C19 N5 1.353(11) . ? C19 N6 1.371(9) . ? C20 C25 1.370(13) . ? C20 N5 1.382(12) . ? C20 C21 1.417(13) . ? C21 C22 1.380(12) . ? C21 H21 0.93 . ? C22 C23 1.398(13) . ? C22 H22 0.93 . ? C23 C24 1.329(15) . ? C23 H23 0.93 . ? C24 C25 1.331(14) . ? C24 H24 0.93 . ? C25 N6 1.392(11) . ? C26 N6 1.499(10) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C27 N7 1.332(11) . ? C27 C28 1.393(13) . ? C27 H27 0.93 . ? C28 C29 1.342(14) . ? C28 H28 0.93 . ? C29 C30 1.379(14) . ? C29 H29 0.93 . ? C30 C31 1.364(13) . ? C30 H30 0.93 . ? C31 N7 1.369(10) . ? C31 C32 1.524(12) . ? C32 N8 1.323(10) . ? C32 N9 1.340(10) . ? C33 N8 1.336(11) . ? C33 C34 1.399(12) . ? C33 C38 1.419(12) . ? C34 C35 1.383(12) . ? C34 H34 0.93 . ? C35 C36 1.379(14) . ? C35 H35 0.93 . ? C36 C37 1.311(15) . ? C36 H36 0.93 . ? C37 C38 1.396(12) . ? C37 H37 0.93 . ? C38 N9 1.379(11) . ? C39 N9 1.443(11) . ? C39 H39A 0.96 . ? C39 H39B 0.96 . ? C39 H39C 0.96 . ? C40 N10 1.334(12) . ? C40 C41 1.389(13) . ? C40 H40 0.93 . ? C41 C42 1.391(13) . ? C41 H41 0.93 . ? C42 C43 1.349(14) . ? C42 H42 0.93 . ? C43 C44 1.350(12) . ? C43 H43 0.93 . ? C44 N10 1.375(11) . ? C44 C45 1.435(12) . ? C45 N11 1.346(10) . ? C45 N12 1.379(10) . ? C46 C47 1.367(13) . ? C46 C51 1.405(12) . ? C46 N11 1.428(11) . ? C47 C48 1.392(12) . ? C47 H47 0.93 . ? C48 C49 1.427(15) . ? C48 H48 0.93 . ? C49 C50 1.332(15) . ? C49 H49 0.93 . ? C50 C51 1.413(13) . ? C50 H50 0.93 . ? C51 N12 1.357(11) . ? C52 N12 1.466(10) . ? C52 H52A 0.96 . ? C52 H52B 0.96 . ? C52 H52C 0.96 . ? C53 N13 1.336(11) . ? C53 C54 1.368(13) . ? C53 H53 0.93 . ? C54 C55 1.358(13) . ? C54 H54 0.93 . ? C55 C56 1.370(14) . ? C55 H55 0.93 . ? C56 C57 1.362(12) . ? C56 H56 0.93 . ? C57 N13 1.383(11) . ? C57 C58 1.466(12) . ? C58 N14 1.326(10) . ? C58 N15 1.382(10) . ? C59 C60 1.370(12) . ? C59 N14 1.398(11) . ? C59 C64 1.403(12) . ? C60 C61 1.399(14) . ? C60 H60 0.93 . ? C61 C62 1.326(14) . ? C61 H61 0.93 . ? C62 C63 1.358(14) . ? C62 H62 0.93 . ? C63 C64 1.379(13) . ? C63 H63 0.93 . ? C64 N15 1.371(12) . ? C65 N15 1.423(11) . ? C65 H65A 0.96 . ? C65 H65B 0.96 . ? C65 H65C 0.96 . ? C66 N16 1.352(11) . ? C66 C67 1.378(14) . ? C66 H66 0.93 . ? C67 C68 1.380(14) . ? C67 H67 0.93 . ? C68 C69 1.396(13) . ? C68 H68 0.93 . ? C69 C70 1.363(13) . ? C69 H69 0.93 . ? C70 N16 1.354(11) . ? C70 C71 1.465(12) . ? C71 N17 1.315(10) . ? C71 N18 1.366(10) . ? C72 N17 1.357(11) . ? C72 C73 1.373(13) . ? C72 C77 1.403(13) . ? C73 C74 1.397(13) . ? C73 H73 0.93 . ? C74 C75 1.378(14) . ? C74 H74 0.93 . ? C75 C76 1.364(16) . ? C75 H75 0.93 . ? C76 C77 1.441(15) . ? C76 H76 0.93 . ? C77 N18 1.369(12) . ? C78 N18 1.444(11) . ? C78 H78A 0.96 . ? C78 H78B 0.96 . ? C78 H78C 0.96 . ? C79 F1 1.210(12) . ? C79 F3 1.308(11) . ? C79 F2 1.341(13) . ? C79 S1 1.803(12) . ? C80 F5 1.287(17) . ? C80 F6 1.317(14) . ? C80 F4 1.354(16) . ? C80 S2 1.665(19) . ? C81 F9 1.12(2) . ? C81 F8 1.201(14) . ? C81 F7 1.32(2) . ? C81 S3 1.746(17) . ? C82 F12 1.263(15) . ? C82 F10 1.323(19) . ? C82 F11 1.52(2) . ? C82 S4 1.66(2) . ? N1 Fe1 2.047(8) . ? N2 Fe1 1.989(8) . ? N4 Fe1 2.029(8) . ? N5 Fe1 1.941(8) . ? N7 Fe1 2.021(7) . ? N8 Fe1 2.000(7) . ? N10 Fe2 2.011(8) . ? N11 Fe2 1.988(6) . ? N13 Fe2 1.992(7) . ? N14 Fe2 2.038(7) . ? N16 Fe2 2.038(8) . ? N17 Fe2 1.997(7) . ? O1 S1 1.433(7) . ? O2 S1 1.436(11) . ? O1W H1W1 0.9007 . ? O1W H2W1 0.9006 . ? O3 S1 1.410(8) . ? O4 S2 1.376(11) . ? O5 S2 1.404(15) . ? O6 S2 1.380(9) . ? O7 S3 1.375(10) . ? O8 S3 1.470(11) . ? O9 S3 1.407(7) . ? O10 S4 1.451(9) . ? O11 S4 1.359(11) . ? O12 S4 1.651(12) . ? F7 F9 1.71(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.0(10) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 119.1(10) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 117.7(11) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C5 C4 C3 119.7(11) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 N1 121.8(10) . . ? C4 C5 C6 127.7(9) . . ? N1 C5 C6 110.6(8) . . ? N2 C6 N3 113.5(9) . . ? N2 C6 C5 118.5(8) . . ? N3 C6 C5 127.7(9) . . ? N2 C7 C12 110.1(9) . . ? N2 C7 C8 129.7(9) . . ? C12 C7 C8 120.2(9) . . ? C9 C8 C7 116.6(10) . . ? C9 C8 H8 121.7 . . ? C7 C8 H8 121.7 . . ? C8 C9 C10 121.1(11) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 123.9(10) . . ? C11 C10 H10 118 . . ? C9 C10 H10 118 . . ? C12 C11 C10 113.0(10) . . ? C12 C11 H11 123.5 . . ? C10 C11 H11 123.5 . . ? C7 C12 N3 106.8(9) . . ? C7 C12 C11 125.3(10) . . ? N3 C12 C11 127.8(10) . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C15 125.6(9) . . ? N4 C14 H14 117.2 . . ? C15 C14 H14 117.2 . . ? C16 C15 C14 118.4(11) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C15 C16 C17 116.5(10) . . ? C15 C16 H16 121.8 . . ? C17 C16 H16 121.8 . . ? C18 C17 C16 120.2(10) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? N4 C18 C17 122.6(9) . . ? N4 C18 C19 111.8(8) . . ? C17 C18 C19 125.7(8) . . ? N5 C19 N6 111.3(8) . . ? N5 C19 C18 116.3(7) . . ? N6 C19 C18 132.4(8) . . ? C25 C20 N5 111.3(9) . . ? C25 C20 C21 119.8(9) . . ? N5 C20 C21 128.9(9) . . ? C22 C21 C20 115.8(9) . . ? C22 C21 H21 122.1 . . ? C20 C21 H21 122.1 . . ? C21 C22 C23 120.6(10) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 122.3(11) . . ? C24 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? C23 C24 C25 117.9(12) . . ? C23 C24 H24 121.1 . . ? C25 C24 H24 121.1 . . ? C24 C25 C20 123.4(11) . . ? C24 C25 N6 130.7(10) . . ? C20 C25 N6 105.7(8) . . ? N6 C26 H26A 109.5 . . ? N6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N7 C27 C28 122.7(9) . . ? N7 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C29 C28 C27 119.9(10) . . ? C29 C28 H28 120 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 119.0(10) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C31 C30 C29 118.8(9) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? C30 C31 N7 123.2(9) . . ? C30 C31 C32 129.5(8) . . ? N7 C31 C32 107.1(8) . . ? N8 C32 N9 113.7(8) . . ? N8 C32 C31 120.5(7) . . ? N9 C32 C31 125.8(8) . . ? N8 C33 C34 131.4(9) . . ? N8 C33 C38 109.8(8) . . ? C34 C33 C38 118.6(8) . . ? C35 C34 C33 118.3(9) . . ? C35 C34 H34 120.9 . . ? C33 C34 H34 120.9 . . ? C36 C35 C34 120.3(10) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 123.6(11) . . ? C37 C36 H36 118.2 . . ? C35 C36 H36 118.2 . . ? C36 C37 C38 118.2(9) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? N9 C38 C37 134.0(8) . . ? N9 C38 C33 105.0(7) . . ? C37 C38 C33 120.7(9) . . ? N9 C39 H39A 109.5 . . ? N9 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N9 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N10 C40 C41 124.7(9) . . ? N10 C40 H40 117.7 . . ? C41 C40 H40 117.7 . . ? C40 C41 C42 117.3(9) . . ? C40 C41 H41 121.4 . . ? C42 C41 H41 121.4 . . ? C43 C42 C41 118.4(9) . . ? C43 C42 H42 120.8 . . ? C41 C42 H42 120.8 . . ? C42 C43 C44 121.7(10) . . ? C42 C43 H43 119.2 . . ? C44 C43 H43 119.2 . . ? C43 C44 N10 122.1(9) . . ? C43 C44 C45 127.1(9) . . ? N10 C44 C45 110.5(8) . . ? N11 C45 N12 110.0(8) . . ? N11 C45 C44 119.1(8) . . ? N12 C45 C44 130.8(8) . . ? C47 C46 C51 124.8(9) . . ? C47 C46 N11 130.6(8) . . ? C51 C46 N11 104.5(8) . . ? C46 C47 C48 114.1(9) . . ? C46 C47 H47 122.9 . . ? C48 C47 H47 122.9 . . ? C47 C48 C49 123.2(10) . . ? C47 C48 H48 118.4 . . ? C49 C48 H48 118.4 . . ? C50 C49 C48 120.2(11) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C49 C50 C51 119.3(10) . . ? C49 C50 H50 120.4 . . ? C51 C50 H50 120.4 . . ? N12 C51 C46 110.1(8) . . ? N12 C51 C50 131.5(9) . . ? C46 C51 C50 118.4(10) . . ? N12 C52 H52A 109.5 . . ? N12 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N12 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N13 C53 C54 125.1(9) . . ? N13 C53 H53 117.4 . . ? C54 C53 H53 117.4 . . ? C55 C54 C53 117.5(10) . . ? C55 C54 H54 121.2 . . ? C53 C54 H54 121.2 . . ? C54 C55 C56 120.5(10) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C57 C56 C55 119.0(10) . . ? C57 C56 H56 120.5 . . ? C55 C56 H56 120.5 . . ? C56 C57 N13 122.3(9) . . ? C56 C57 C58 126.2(9) . . ? N13 C57 C58 111.4(8) . . ? N14 C58 N15 113.3(8) . . ? N14 C58 C57 118.1(8) . . ? N15 C58 C57 128.5(8) . . ? C60 C59 N14 129.8(9) . . ? C60 C59 C64 122.4(9) . . ? N14 C59 C64 107.7(8) . . ? C59 C60 C61 114.2(10) . . ? C59 C60 H60 122.9 . . ? C61 C60 H60 122.9 . . ? C62 C61 C60 124.4(10) . . ? C62 C61 H61 117.8 . . ? C60 C61 H61 117.8 . . ? C61 C62 C63 121.1(10) . . ? C61 C62 H62 119.5 . . ? C63 C62 H62 119.5 . . ? C62 C63 C64 118.3(11) . . ? C62 C63 H63 120.9 . . ? C64 C63 H63 120.9 . . ? N15 C64 C63 132.0(10) . . ? N15 C64 C59 108.4(8) . . ? C63 C64 C59 119.4(10) . . ? N15 C65 H65A 109.5 . . ? N15 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N15 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N16 C66 C67 122.5(10) . . ? N16 C66 H66 118.8 . . ? C67 C66 H66 118.8 . . ? C66 C67 C68 118.2(11) . . ? C66 C67 H67 120.9 . . ? C68 C67 H67 120.9 . . ? C67 C68 C69 119.6(11) . . ? C67 C68 H68 120.2 . . ? C69 C68 H68 120.2 . . ? C70 C69 C68 119.0(10) . . ? C70 C69 H69 120.5 . . ? C68 C69 H69 120.5 . . ? N16 C70 C69 121.9(9) . . ? N16 C70 C71 111.3(8) . . ? C69 C70 C71 126.7(10) . . ? N17 C71 N18 111.6(8) . . ? N17 C71 C70 118.9(8) . . ? N18 C71 C70 129.5(8) . . ? N17 C72 C73 130.4(9) . . ? N17 C72 C77 107.8(9) . . ? C73 C72 C77 121.7(9) . . ? C72 C73 C74 116.0(10) . . ? C72 C73 H73 122 . . ? C74 C73 H73 122 . . ? C75 C74 C73 122.8(11) . . ? C75 C74 H74 118.6 . . ? C73 C74 H74 118.6 . . ? C76 C75 C74 123.0(10) . . ? C76 C75 H75 118.5 . . ? C74 C75 H75 118.5 . . ? C75 C76 C77 114.9(11) . . ? C75 C76 H76 122.6 . . ? C77 C76 H76 122.6 . . ? N18 C77 C72 107.0(8) . . ? N18 C77 C76 131.5(10) . . ? C72 C77 C76 121.5(11) . . ? N18 C78 H78A 109.5 . . ? N18 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? N18 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? F1 C79 F3 111.2(11) . . ? F1 C79 F2 107.1(12) . . ? F3 C79 F2 101.0(9) . . ? F1 C79 S1 116.4(9) . . ? F3 C79 S1 114.5(8) . . ? F2 C79 S1 104.9(9) . . ? F5 C80 F6 99.8(16) . . ? F5 C80 F4 98.2(15) . . ? F6 C80 F4 108.8(14) . . ? F5 C80 S2 116.4(11) . . ? F6 C80 S2 113.8(16) . . ? F4 C80 S2 117.5(11) . . ? F9 C81 F8 110(2) . . ? F9 C81 F7 88.8(19) . . ? F8 C81 F7 105.5(16) . . ? F9 C81 S3 115.4(16) . . ? F8 C81 S3 123.0(9) . . ? F7 C81 S3 108.5(16) . . ? F12 C82 F10 105.9(14) . . ? F12 C82 F11 110.8(12) . . ? F10 C82 F11 109(2) . . ? F12 C82 S4 119.0(19) . . ? F10 C82 S4 115.0(10) . . ? F11 C82 S4 97.0(12) . . ? C1 N1 C5 118.6(8) . . ? C1 N1 Fe1 126.5(7) . . ? C5 N1 Fe1 114.8(7) . . ? C6 N2 C7 104.4(8) . . ? C6 N2 Fe1 112.8(7) . . ? C7 N2 Fe1 139.8(7) . . ? C6 N3 C12 105.1(8) . . ? C6 N3 C13 129.3(8) . . ? C12 N3 C13 124.7(8) . . ? C14 N4 C18 116.3(9) . . ? C14 N4 Fe1 127.6(6) . . ? C18 N4 Fe1 116.1(6) . . ? C19 N5 C20 104.6(8) . . ? C19 N5 Fe1 115.7(7) . . ? C20 N5 Fe1 139.2(7) . . ? C19 N6 C25 107.0(7) . . ? C19 N6 C26 128.0(8) . . ? C25 N6 C26 124.6(8) . . ? C27 N7 C31 116.2(8) . . ? C27 N7 Fe1 125.4(6) . . ? C31 N7 Fe1 118.3(6) . . ? C32 N8 C33 105.5(7) . . ? C32 N8 Fe1 113.0(6) . . ? C33 N8 Fe1 141.3(6) . . ? C32 N9 C38 105.9(7) . . ? C32 N9 C39 129.7(9) . . ? C38 N9 C39 124.1(8) . . ? C40 N10 C44 115.5(8) . . ? C40 N10 Fe2 128.1(7) . . ? C44 N10 Fe2 116.4(6) . . ? C45 N11 C46 108.2(7) . . ? C45 N11 Fe2 113.6(5) . . ? C46 N11 Fe2 137.6(6) . . ? C51 N12 C45 107.1(7) . . ? C51 N12 C52 122.7(8) . . ? C45 N12 C52 130.2(9) . . ? C53 N13 C57 115.4(8) . . ? C53 N13 Fe2 128.7(6) . . ? C57 N13 Fe2 115.9(6) . . ? C58 N14 C59 105.6(7) . . ? C58 N14 Fe2 112.1(6) . . ? C59 N14 Fe2 140.0(6) . . ? C64 N15 C58 104.9(7) . . ? C64 N15 C65 125.5(8) . . ? C58 N15 C65 129.7(8) . . ? C66 N16 C70 118.6(9) . . ? C66 N16 Fe2 125.9(7) . . ? C70 N16 Fe2 115.2(6) . . ? C71 N17 C72 107.6(8) . . ? C71 N17 Fe2 113.9(6) . . ? C72 N17 Fe2 137.9(7) . . ? C71 N18 C77 106.0(7) . . ? C71 N18 C78 127.8(9) . . ? C77 N18 C78 125.8(8) . . ? H1W1 O1W H2W1 107.4 . . ? N5 Fe1 N2 100.0(3) . . ? N5 Fe1 N8 170.7(3) . . ? N2 Fe1 N8 88.5(3) . . ? N5 Fe1 N7 94.4(3) . . ? N2 Fe1 N7 96.0(3) . . ? N8 Fe1 N7 80.8(3) . . ? N5 Fe1 N4 79.9(3) . . ? N2 Fe1 N4 173.7(3) . . ? N8 Fe1 N4 92.1(3) . . ? N7 Fe1 N4 90.3(3) . . ? N5 Fe1 N1 91.3(3) . . ? N2 Fe1 N1 80.1(3) . . ? N8 Fe1 N1 94.0(3) . . ? N7 Fe1 N1 173.6(3) . . ? N4 Fe1 N1 93.6(3) . . ? N11 Fe2 N13 96.7(3) . . ? N11 Fe2 N17 170.5(3) . . ? N13 Fe2 N17 90.3(3) . . ? N11 Fe2 N10 80.2(3) . . ? N13 Fe2 N10 173.7(3) . . ? N17 Fe2 N10 93.5(3) . . ? N11 Fe2 N14 89.0(3) . . ? N13 Fe2 N14 80.6(3) . . ? N17 Fe2 N14 98.5(3) . . ? N10 Fe2 N14 93.9(3) . . ? N11 Fe2 N16 92.6(3) . . ? N13 Fe2 N16 95.1(3) . . ? N17 Fe2 N16 80.3(3) . . ? N10 Fe2 N16 90.5(3) . . ? N14 Fe2 N16 175.5(3) . . ? O3 S1 O1 118.0(5) . . ? O3 S1 O2 109.9(7) . . ? O1 S1 O2 113.5(5) . . ? O3 S1 C79 106.0(5) . . ? O1 S1 C79 103.5(5) . . ? O2 S1 C79 104.5(6) . . ? O4 S2 O6 122.3(9) . . ? O4 S2 O5 110.3(10) . . ? O6 S2 O5 117.6(7) . . ? O4 S2 C80 97.7(9) . . ? O6 S2 C80 106.2(6) . . ? O5 S2 C80 96.8(10) . . ? O7 S3 O9 119.0(6) . . ? O7 S3 O8 115.8(10) . . ? O9 S3 O8 112.5(6) . . ? O7 S3 C81 101.8(8) . . ? O9 S3 C81 108.5(5) . . ? O8 S3 C81 95.4(10) . . ? O11 S4 O10 120.3(10) . . ? O11 S4 O12 114.6(9) . . ? O10 S4 O12 108.9(8) . . ? O11 S4 C82 112.1(9) . . ? O10 S4 C82 103.8(9) . . ? O12 S4 C82 93.2(8) . . ? C81 F7 F9 40.9(10) . . ? C81 F9 F7 50.4(16) . . ? # END of CIF _database_code_depnum_ccdc_archive 'CCDC 955599' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_fepbo _audit_creation_date 2011-10-20T16:21:19-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C39 H24 F9 Fe1.5 N6 O12 S3' _chemical_formula_sum 'C39 H24 F9 Fe1.5 N6 O12 S3' _chemical_formula_weight 1119.6 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.061(1) _cell_length_b 13.4974(6) _cell_length_c 19.732(1) _cell_angle_alpha 90 _cell_angle_beta 95.911(4) _cell_angle_gamma 90 _cell_volume 8758.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 225(2) _cell_measurement_reflns_used 46858 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 28.56 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4512 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.755 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 225(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'Omega + Phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_unetI/netI 0.0392 _diffrn_reflns_number 46858 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 28.56 _diffrn_reflns_theta_full 28.56 _diffrn_measured_fraction_theta_full 0.943 _diffrn_measured_fraction_theta_max 0.943 _reflns_number_total 10531 _reflns_number_gt 7522 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1080P)^2^+13.1936P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10531 _refine_ls_number_parameters 690 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.2074 _refine_ls_wR_factor_gt 0.1766 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.563 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.216 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.73298(12) 0.0601(3) 0.3377(2) 0.0519(9) Uani 1 1 d . . . C2 C 0.76457(13) 0.1022(4) 0.3065(3) 0.0690(13) Uani 1 1 d . . . H2 H 0.7616 0.1198 0.2607 0.083 Uiso 1 1 calc R . . C3 C 0.80025(15) 0.1166(4) 0.3468(3) 0.0875(17) Uani 1 1 d . . . H3 H 0.8222 0.1436 0.3274 0.105 Uiso 1 1 calc R . . C4 C 0.80510(17) 0.0922(5) 0.4164(3) 0.0930(19) Uani 1 1 d . . . H4 H 0.8298 0.1051 0.442 0.112 Uiso 1 1 calc R . . C5 C 0.77399(17) 0.0496(4) 0.4473(3) 0.0799(16) Uani 1 1 d . . . H5 H 0.7767 0.033 0.4933 0.096 Uiso 1 1 calc R . . C6 C 0.73825(13) 0.0329(3) 0.4055(2) 0.0583(10) Uani 1 1 d . . . C7 C 0.67808(11) -0.0076(3) 0.36355(17) 0.0433(8) Uani 1 1 d . . . C8 C 0.63734(11) -0.0476(3) 0.36010(17) 0.0426(8) Uani 1 1 d . . . C9 C 0.62215(14) -0.1007(3) 0.41145(19) 0.0549(10) Uani 1 1 d . . . H9 H 0.6379 -0.1131 0.4524 0.066 Uiso 1 1 calc R . . C10 C 0.58237(16) -0.1354(4) 0.3999(2) 0.0705(13) Uani 1 1 d . . . H10 H 0.5709 -0.1708 0.4335 0.085 Uiso 1 1 calc R . . C11 C 0.56052(15) -0.1170(4) 0.3392(2) 0.0724(13) Uani 1 1 d . . . H11 H 0.5339 -0.1397 0.3307 0.087 Uiso 1 1 calc R . . C12 C 0.57818(13) -0.0642(3) 0.2901(2) 0.0605(11) Uani 1 1 d . . . H12 H 0.563 -0.0527 0.2485 0.073 Uiso 1 1 calc R . . C13 C 0.55579(11) 0.1049(3) 0.13981(18) 0.0444(8) Uani 1 1 d . . . C14 C 0.53107(13) 0.1598(3) 0.1777(2) 0.0573(10) Uani 1 1 d . . . H14 H 0.5393 0.1771 0.2226 0.069 Uiso 1 1 calc R . . C15 C 0.49392(13) 0.1879(4) 0.1465(2) 0.0639(11) Uani 1 1 d . . . H15 H 0.4763 0.2232 0.1711 0.077 Uiso 1 1 calc R . . C16 C 0.48190(13) 0.1644(3) 0.0781(2) 0.0625(11) Uani 1 1 d . . . H16 H 0.4567 0.1859 0.0583 0.075 Uiso 1 1 calc R . . C17 C 0.50638(12) 0.1105(3) 0.0395(2) 0.0538(10) Uani 1 1 d . . . H17 H 0.4988 0.0956 -0.0061 0.065 Uiso 1 1 calc R . . C18 C 0.54267(11) 0.0802(3) 0.07278(18) 0.0440(8) Uani 1 1 d . . . C19 C 0.60165(11) 0.0141(3) 0.10174(16) 0.0401(7) Uani 1 1 d . . . C20 C 0.63823(11) -0.0448(3) 0.09731(17) 0.0406(7) Uani 1 1 d . . . C21 C 0.64686(12) -0.0958(3) 0.03998(19) 0.0482(9) Uani 1 1 d . . . H21 H 0.6288 -0.0954 0.0006 0.058 Uiso 1 1 calc R . . C22 C 0.68299(14) -0.1473(3) 0.0425(2) 0.0593(10) Uani 1 1 d . . . H22 H 0.6898 -0.1824 0.0047 0.071 Uiso 1 1 calc R . . C23 C 0.70860(13) -0.1461(4) 0.1011(2) 0.0628(11) Uani 1 1 d . . . H23 H 0.7331 -0.1803 0.1035 0.075 Uiso 1 1 calc R . . C24 C 0.69819(13) -0.0940(3) 0.1571(2) 0.0572(10) Uani 1 1 d . . . H24 H 0.7161 -0.094 0.1967 0.069 Uiso 1 1 calc R . . C25 C 0.66675(14) 0.3367(4) 0.3309(3) 0.0733(14) Uani 1 1 d . . . C27 C 0.41169(13) 0.5906(3) 0.1503(2) 0.0581(11) Uani 1 1 d . . . C28 C 0.38448(14) 0.6449(4) 0.1823(2) 0.0689(12) Uani 1 1 d . . . H28 H 0.3903 0.6657 0.2272 0.083 Uiso 1 1 calc R . . C29 C 0.34807(16) 0.6675(5) 0.1451(3) 0.0873(17) Uani 1 1 d . . . H29 H 0.3286 0.7027 0.1659 0.105 Uiso 1 1 calc R . . C30 C 0.33965(19) 0.6392(5) 0.0773(3) 0.097(2) Uani 1 1 d . . . H30 H 0.3151 0.6577 0.0535 0.116 Uiso 1 1 calc R . . C31 C 0.36660(18) 0.5849(5) 0.0452(3) 0.0832(17) Uani 1 1 d . . . H31 H 0.361 0.5654 0 0.1 Uiso 1 1 calc R . . C32 C 0.40244(16) 0.5604(4) 0.0826(2) 0.0678(13) Uani 1 1 d . . . C33 C 0.46188(13) 0.5051(3) 0.12036(17) 0.0530(10) Uani 1 1 d . . . C34 C 0.50051(14) 0.4547(3) 0.12045(18) 0.0536(10) Uani 1 1 d . . . C35 C 0.51321(19) 0.4035(3) 0.0662(2) 0.0671(14) Uani 1 1 d . . . H35 H 0.4964 0.3986 0.0256 0.081 Uiso 1 1 calc R . . C36 C 0.5513(2) 0.3592(4) 0.0725(2) 0.0758(15) Uani 1 1 d . . . H36 H 0.5605 0.3248 0.0362 0.091 Uiso 1 1 calc R . . C37 C 0.57542(18) 0.3675(3) 0.1343(3) 0.0716(13) Uani 1 1 d . . . H37 H 0.601 0.3382 0.1402 0.086 Uiso 1 1 calc R . . C38 C 0.56076(15) 0.4202(3) 0.1869(2) 0.0581(10) Uani 1 1 d . . . H38 H 0.577 0.4254 0.2281 0.07 Uiso 1 1 calc R . . C39 C 0.58055(13) 0.6961(3) 0.1070(2) 0.0566(10) Uani 1 1 d . . . N1 N 0.69348(9) 0.0333(2) 0.31258(14) 0.0429(7) Uani 1 1 d . . . N2 N 0.61564(9) -0.0292(2) 0.29937(14) 0.0441(7) Uani 1 1 d . . . N3 N 0.59425(8) 0.0622(2) 0.15567(14) 0.0402(6) Uani 1 1 d . . . N4 N 0.66318(9) -0.0436(2) 0.15658(14) 0.0437(7) Uani 1 1 d . . . N5 N 0.45052(10) 0.5540(2) 0.17162(14) 0.0484(8) Uani 1 1 d . . . N6 N 0.52371(11) 0.4646(2) 0.18071(15) 0.0500(8) Uani 1 1 d . . . O1 O 0.70317(9) -0.0108(2) 0.42201(12) 0.0556(7) Uani 1 1 d . . . O2 O 0.57291(8) 0.02129(19) 0.04830(12) 0.0452(6) Uani 1 1 d . . . O3 O 0.43468(11) 0.5056(2) 0.06397(13) 0.0663(9) Uani 1 1 d . . . O4 O 0.62137(8) 0.1986(2) 0.27406(13) 0.0510(6) Uani 1 1 d . . . O5 O 0.63801(14) 0.1907(3) 0.39478(16) 0.0905(12) Uani 1 1 d . . . O6 O 0.59110(9) 0.3167(2) 0.34507(16) 0.0665(8) Uani 1 1 d . . . O7 O 0.68410(9) 0.1668(2) 0.18487(13) 0.0597(8) Uani 1 1 d . . . O8 O 0.66368(15) 0.1782(3) 0.06514(17) 0.1141(17) Uani 1 1 d . . . O10 O 0.53258(8) 0.6884(2) 0.20181(12) 0.0462(6) Uani 1 1 d . . . O11 O 0.50200(8) 0.6958(2) 0.08504(13) 0.0536(7) Uani 1 1 d . . . O12 O 0.53582(9) 0.8401(2) 0.13767(15) 0.0560(7) Uani 1 1 d . . . F1 F 0.70008(8) 0.2879(3) 0.3179(2) 0.1068(12) Uani 1 1 d . . . F2 F 0.67507(11) 0.3871(3) 0.3872(2) 0.1211(14) Uani 1 1 d . . . F3 F 0.65777(11) 0.3998(3) 0.2799(2) 0.1096(12) Uani 1 1 d . . . F7 F 0.58431(11) 0.6002(2) 0.1070(2) 0.1053(13) Uani 1 1 d . . . F8 F 0.61122(7) 0.7335(2) 0.14740(15) 0.0800(8) Uani 1 1 d . . . F9 F 0.58438(9) 0.7290(2) 0.04471(14) 0.0775(8) Uani 1 1 d . . . S1 S 0.62451(3) 0.25133(7) 0.33845(5) 0.0504(2) Uani 1 1 d . . . S3 S 0.53202(3) 0.73514(7) 0.13536(4) 0.0392(2) Uani 1 1 d . . . Fe1 Fe 0.646146(15) 0.06850(4) 0.23112(2) 0.03896(16) Uani 1 1 d . A . Fe2 Fe 0.5 0.57270(5) 0.25 0.04059(19) Uani 1 2 d S . . S2 S 0.69921(7) 0.17042(15) 0.11667(10) 0.0408(4) Uani 0.5 1 d PD A 1 O9 O 0.7332(3) 0.1046(7) 0.1038(9) 0.094(4) Uani 0.5 1 d PD A 1 C26 C 0.7188(2) 0.2997(6) 0.1206(4) 0.0464(19) Uani 0.5 1 d PD A 1 F4 F 0.7478(6) 0.3071(14) 0.1719(10) 0.111(6) Uani 0.5 1 d PD A 1 F5 F 0.7325(4) 0.3207(8) 0.0610(4) 0.085(3) Uani 0.5 1 d PD A 1 F6 F 0.6914(3) 0.3694(4) 0.1319(6) 0.086(2) Uani 0.5 1 d PD A 1 S22 S 0.68177(11) 0.2220(3) 0.12081(16) 0.0978(12) Uani 0.5 1 d PD A 2 O99 O 0.6801(6) 0.3330(5) 0.1269(9) 0.138(7) Uani 0.5 1 d PD A 2 C226 C 0.7341(7) 0.2342(9) 0.1125(7) 0.175(12) Uani 0.5 1 d PD A 2 F44 F 0.7530(6) 0.2864(18) 0.1630(11) 0.129(8) Uani 0.5 1 d PD A 2 F55 F 0.7402(6) 0.2911(13) 0.0602(8) 0.171(8) Uani 0.5 1 d PD A 2 F66 F 0.7363(8) 0.1367(8) 0.1038(12) 0.215(10) Uani 0.5 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.043(2) 0.052(2) 0.058(2) 0.0030(17) -0.0115(17) 0.0001(17) C2 0.042(2) 0.073(3) 0.089(3) 0.013(3) -0.010(2) -0.012(2) C3 0.050(3) 0.086(4) 0.121(5) 0.015(3) -0.019(3) -0.018(3) C4 0.064(3) 0.085(4) 0.119(5) 0.000(3) -0.046(3) -0.011(3) C5 0.076(3) 0.079(3) 0.075(3) -0.003(3) -0.039(3) -0.001(3) C6 0.051(2) 0.058(2) 0.060(2) -0.0010(19) -0.0194(19) 0.0006(19) C7 0.052(2) 0.0436(19) 0.0325(17) -0.0001(14) -0.0044(14) 0.0006(16) C8 0.050(2) 0.0450(19) 0.0328(17) 0.0010(14) 0.0059(14) -0.0051(15) C9 0.078(3) 0.049(2) 0.0378(19) 0.0050(16) 0.0091(18) -0.005(2) C10 0.089(3) 0.066(3) 0.062(3) 0.008(2) 0.033(3) -0.019(3) C11 0.059(3) 0.086(3) 0.072(3) 0.008(3) 0.012(2) -0.033(3) C12 0.051(2) 0.076(3) 0.054(2) 0.007(2) 0.0026(18) -0.023(2) C13 0.0422(19) 0.053(2) 0.0371(18) 0.0043(15) -0.0019(14) -0.0038(16) C14 0.053(2) 0.074(3) 0.045(2) 0.0031(19) 0.0033(17) 0.004(2) C15 0.050(2) 0.076(3) 0.067(3) 0.012(2) 0.012(2) 0.013(2) C16 0.042(2) 0.066(3) 0.076(3) 0.016(2) -0.008(2) 0.0009(19) C17 0.050(2) 0.054(2) 0.054(2) 0.0042(18) -0.0118(17) -0.0054(18) C18 0.0401(19) 0.048(2) 0.0425(19) 0.0036(15) -0.0051(14) -0.0050(15) C19 0.0428(18) 0.0424(18) 0.0336(17) 0.0022(14) -0.0034(13) -0.0073(15) C20 0.0436(19) 0.0444(18) 0.0330(17) 0.0027(14) -0.0008(13) -0.0046(15) C21 0.053(2) 0.050(2) 0.0396(19) 0.0015(15) -0.0012(16) -0.0006(17) C22 0.070(3) 0.062(3) 0.047(2) -0.0042(18) 0.0110(19) 0.006(2) C23 0.049(2) 0.075(3) 0.064(3) 0.000(2) 0.0040(19) 0.016(2) C24 0.047(2) 0.072(3) 0.050(2) 0.003(2) -0.0055(17) 0.004(2) C25 0.048(3) 0.077(3) 0.090(4) -0.025(3) -0.013(2) -0.003(2) C27 0.054(2) 0.069(3) 0.047(2) 0.0211(19) -0.0144(18) -0.018(2) C28 0.057(3) 0.084(3) 0.063(3) 0.017(2) -0.009(2) -0.003(2) C29 0.057(3) 0.101(4) 0.098(4) 0.025(3) -0.019(3) -0.002(3) C30 0.072(4) 0.115(5) 0.094(4) 0.033(4) -0.040(3) -0.014(4) C31 0.081(4) 0.095(4) 0.065(3) 0.020(3) -0.033(3) -0.025(3) C32 0.068(3) 0.074(3) 0.055(3) 0.020(2) -0.020(2) -0.025(3) C33 0.073(3) 0.053(2) 0.0297(18) 0.0063(15) -0.0085(17) -0.023(2) C34 0.081(3) 0.045(2) 0.0336(19) 0.0011(15) 0.0018(18) -0.015(2) C35 0.121(4) 0.045(2) 0.035(2) -0.0046(16) 0.009(2) -0.018(3) C36 0.126(5) 0.052(3) 0.054(3) -0.003(2) 0.026(3) -0.006(3) C37 0.094(4) 0.051(3) 0.073(3) 0.001(2) 0.026(3) 0.006(2) C38 0.077(3) 0.049(2) 0.049(2) 0.0005(17) 0.010(2) 0.002(2) C39 0.049(2) 0.054(2) 0.070(3) 0.0108(19) 0.022(2) 0.0016(18) N1 0.0391(15) 0.0512(17) 0.0368(15) 0.0045(13) -0.0043(12) -0.0066(13) N2 0.0465(17) 0.0500(17) 0.0353(15) 0.0026(13) 0.0019(12) -0.0135(14) N3 0.0339(14) 0.0523(17) 0.0326(14) 0.0015(12) -0.0050(11) -0.0042(12) N4 0.0394(16) 0.0528(18) 0.0375(15) 0.0029(13) -0.0028(12) -0.0038(13) N5 0.0518(19) 0.061(2) 0.0297(15) 0.0048(13) -0.0084(13) -0.0150(15) N6 0.069(2) 0.0483(17) 0.0319(15) -0.0012(13) 0.0021(14) -0.0019(16) O1 0.0636(18) 0.0623(17) 0.0367(13) 0.0029(12) -0.0146(12) 0.0026(14) O2 0.0492(14) 0.0496(14) 0.0339(12) -0.0025(10) -0.0097(10) -0.0004(11) O3 0.090(2) 0.0677(19) 0.0360(14) 0.0059(13) -0.0173(14) -0.0250(18) O4 0.0547(15) 0.0542(15) 0.0419(14) -0.0079(11) -0.0051(11) -0.0027(12) O5 0.154(4) 0.070(2) 0.0442(17) 0.0093(15) -0.0050(19) 0.018(2) O6 0.0616(19) 0.0659(19) 0.074(2) -0.0124(15) 0.0147(15) 0.0006(15) O7 0.0694(18) 0.0704(19) 0.0405(14) 0.0063(12) 0.0104(12) -0.0277(15) O8 0.156(4) 0.125(3) 0.052(2) 0.023(2) -0.032(2) -0.077(3) O10 0.0451(14) 0.0563(15) 0.0369(13) 0.0012(11) 0.0026(10) -0.0044(12) O11 0.0502(15) 0.0689(18) 0.0397(14) -0.0001(12) -0.0050(11) -0.0130(13) O12 0.0567(17) 0.0437(14) 0.0678(18) -0.0030(13) 0.0069(13) 0.0030(12) F1 0.0451(16) 0.109(3) 0.163(3) -0.050(2) -0.0040(18) -0.0038(16) F2 0.094(2) 0.116(3) 0.147(3) -0.077(3) -0.019(2) -0.016(2) F3 0.092(2) 0.085(2) 0.153(3) 0.025(2) 0.020(2) -0.0221(19) F7 0.109(3) 0.0554(16) 0.167(3) 0.0112(18) 0.085(2) 0.0228(16) F8 0.0360(13) 0.114(2) 0.0893(19) 0.0269(17) 0.0023(12) 0.0027(14) F9 0.0753(18) 0.096(2) 0.0665(16) 0.0102(14) 0.0328(13) -0.0018(15) S1 0.0597(6) 0.0518(5) 0.0381(5) -0.0022(4) -0.0021(4) -0.0011(4) S3 0.0354(4) 0.0440(5) 0.0379(4) -0.0013(3) 0.0029(3) 0.0005(3) Fe1 0.0370(3) 0.0484(3) 0.0303(3) 0.00360(19) -0.00214(19) -0.0090(2) Fe2 0.0437(4) 0.0501(4) 0.0266(3) 0 -0.0028(3) 0 S2 0.0512(12) 0.0345(10) 0.0385(9) 0.0011(7) 0.0139(8) -0.0073(8) O9 0.115(7) 0.030(5) 0.152(9) 0.003(5) 0.082(6) 0.014(4) C26 0.055(5) 0.038(4) 0.046(4) 0.011(3) 0.001(3) -0.013(4) F4 0.128(15) 0.093(6) 0.103(8) 0.006(6) -0.021(8) -0.067(8) F5 0.123(9) 0.074(4) 0.059(4) 0.016(3) 0.017(4) -0.050(5) F6 0.120(5) 0.019(3) 0.124(6) 0.006(4) 0.038(4) 0.001(4) S22 0.087(2) 0.144(4) 0.0615(17) 0.028(2) 0.0018(16) -0.053(2) O99 0.27(2) 0.024(5) 0.131(9) 0.022(6) 0.053(12) 0.035(7) C226 0.143(18) 0.23(3) 0.154(18) 0.11(2) 0.030(16) -0.09(2) F44 0.052(5) 0.190(19) 0.138(14) 0.051(11) -0.027(7) -0.044(8) F55 0.132(9) 0.229(18) 0.168(11) 0.118(10) 0.089(8) 0.015(10) F66 0.39(3) 0.050(7) 0.217(15) 0.022(9) 0.109(15) 0.062(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C6 1.381(6) . ? C1 C2 1.388(6) . ? C1 N1 1.396(5) . ? C2 C3 1.367(6) . ? C2 H2 0.93 . ? C3 C4 1.405(8) . ? C3 H3 0.93 . ? C4 C5 1.375(9) . ? C4 H4 0.93 . ? C5 C6 1.388(6) . ? C5 H5 0.93 . ? C6 O1 1.370(5) . ? C7 N1 1.296(5) . ? C7 O1 1.350(4) . ? C7 C8 1.447(5) . ? C8 N2 1.355(5) . ? C8 C9 1.377(5) . ? C9 C10 1.392(7) . ? C9 H9 0.93 . ? C10 C11 1.356(7) . ? C10 H10 0.93 . ? C11 C12 1.379(6) . ? C11 H11 0.93 . ? C12 N2 1.321(5) . ? C12 H12 0.93 . ? C13 C14 1.379(6) . ? C13 C18 1.389(5) . ? C13 N3 1.402(5) . ? C14 C15 1.370(6) . ? C14 H14 0.93 . ? C15 C16 1.402(6) . ? C15 H15 0.93 . ? C16 C17 1.376(6) . ? C16 H16 0.93 . ? C17 C18 1.369(5) . ? C17 H17 0.93 . ? C18 O2 1.402(5) . ? C19 N3 1.291(4) . ? C19 O2 1.348(4) . ? C19 C20 1.458(5) . ? C20 N4 1.360(4) . ? C20 C21 1.379(5) . ? C21 C22 1.379(6) . ? C21 H21 0.93 . ? C22 C23 1.361(6) . ? C22 H22 0.93 . ? C23 C24 1.384(6) . ? C23 H23 0.93 . ? C24 N4 1.342(5) . ? C24 H24 0.93 . ? C25 F2 1.307(5) . ? C25 F3 1.328(6) . ? C25 F1 1.331(6) . ? C25 S1 1.829(5) . ? C27 C28 1.364(7) . ? C27 N5 1.399(5) . ? C27 C32 1.400(6) . ? C28 C29 1.378(7) . ? C28 H28 0.93 . ? C29 C30 1.392(9) . ? C29 H29 0.93 . ? C30 C31 1.359(9) . ? C30 H30 0.93 . ? C31 C32 1.370(7) . ? C31 H31 0.93 . ? C32 O3 1.378(6) . ? C33 N5 1.295(5) . ? C33 O3 1.357(4) . ? C33 C34 1.447(6) . ? C34 N6 1.354(5) . ? C34 C35 1.375(6) . ? C35 C36 1.389(8) . ? C35 H35 0.93 . ? C36 C37 1.390(7) . ? C36 H36 0.93 . ? C37 C38 1.387(6) . ? C37 H37 0.93 . ? C38 N6 1.358(6) . ? C38 H38 0.93 . ? C39 F7 1.300(5) . ? C39 F8 1.324(5) . ? C39 F9 1.326(5) . ? C39 S3 1.830(4) . ? N1 Fe1 2.177(3) . ? N2 Fe1 2.202(3) . ? N3 Fe1 2.154(3) . ? N4 Fe1 2.223(3) . ? N5 Fe2 2.147(3) . ? N6 Fe2 2.198(3) . ? O4 S1 1.451(3) . ? O4 Fe1 2.148(3) . ? O5 S1 1.415(3) . ? O6 S1 1.430(3) . ? O7 S22 1.463(4) . ? O7 S2 1.484(3) . ? O7 Fe1 2.098(3) . ? O8 S22 1.334(5) . ? O8 S2 1.476(5) . ? O10 S3 1.454(3) . ? O10 Fe2 2.171(3) . ? O11 S3 1.432(3) . ? O12 S3 1.423(3) . ? Fe2 N5 2.147(3) 2_655 ? Fe2 O10 2.171(3) 2_655 ? Fe2 N6 2.198(3) 2_655 ? S2 O9 1.476(7) . ? S2 C26 1.859(8) . ? C26 F4 1.323(9) . ? C26 F5 1.335(8) . ? C26 F6 1.339(8) . ? S22 O99 1.504(7) . ? S22 C226 1.76(2) . ? C226 F55 1.318(9) . ? C226 F44 1.323(10) . ? C226 F66 1.330(10) . ? 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 C6 C1 C2 120.9(4) . . ? C6 C1 N1 107.1(4) . . ? C2 C1 N1 131.9(4) . . ? C3 C2 C1 116.3(5) . . ? C3 C2 H2 121.8 . . ? C1 C2 H2 121.8 . . ? C2 C3 C4 122.7(5) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C5 C4 C3 121.1(4) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 115.8(5) . . ? C4 C5 H5 122.1 . . ? C6 C5 H5 122.1 . . ? O1 C6 C1 108.7(3) . . ? O1 C6 C5 128.2(4) . . ? C1 C6 C5 123.2(5) . . ? N1 C7 O1 114.9(3) . . ? N1 C7 C8 124.1(3) . . ? O1 C7 C8 121.0(3) . . ? N2 C8 C9 123.1(4) . . ? N2 C8 C7 112.2(3) . . ? C9 C8 C7 124.6(3) . . ? C8 C9 C10 117.6(4) . . ? C8 C9 H9 121.2 . . ? C10 C9 H9 121.2 . . ? C11 C10 C9 119.4(4) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 119.3(4) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? N2 C12 C11 123.2(4) . . ? N2 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? C14 C13 C18 120.0(4) . . ? C14 C13 N3 132.4(3) . . ? C18 C13 N3 107.5(3) . . ? C15 C14 C13 117.3(4) . . ? C15 C14 H14 121.4 . . ? C13 C14 H14 121.4 . . ? C14 C15 C16 121.5(4) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C17 C16 C15 121.8(4) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C18 C17 C16 115.3(4) . . ? C18 C17 H17 122.3 . . ? C16 C17 H17 122.3 . . ? C17 C18 C13 123.9(4) . . ? C17 C18 O2 128.6(3) . . ? C13 C18 O2 107.5(3) . . ? N3 C19 O2 115.5(3) . . ? N3 C19 C20 123.5(3) . . ? O2 C19 C20 120.9(3) . . ? N4 C20 C21 123.6(3) . . ? N4 C20 C19 112.1(3) . . ? C21 C20 C19 124.4(3) . . ? C20 C21 C22 118.3(4) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? C23 C22 C21 119.0(4) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 C24 120.1(4) . . ? C22 C23 H23 120 . . ? C24 C23 H23 120 . . ? N4 C24 C23 122.5(4) . . ? N4 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? F2 C25 F3 108.8(5) . . ? F2 C25 F1 108.4(4) . . ? F3 C25 F1 107.2(5) . . ? F2 C25 S1 110.7(4) . . ? F3 C25 S1 110.6(3) . . ? F1 C25 S1 111.0(4) . . ? C28 C27 N5 132.8(4) . . ? C28 C27 C32 120.5(4) . . ? N5 C27 C32 106.7(4) . . ? C27 C28 C29 117.0(5) . . ? C27 C28 H28 121.5 . . ? C29 C28 H28 121.5 . . ? C28 C29 C30 121.9(6) . . ? C28 C29 H29 119 . . ? C30 C29 H29 119 . . ? C31 C30 C29 121.3(5) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 116.8(5) . . ? C30 C31 H31 121.6 . . ? C32 C31 H31 121.6 . . ? C31 C32 O3 129.4(5) . . ? C31 C32 C27 122.4(6) . . ? O3 C32 C27 108.2(4) . . ? N5 C33 O3 114.7(4) . . ? N5 C33 C34 124.4(3) . . ? O3 C33 C34 120.9(4) . . ? N6 C34 C35 122.9(5) . . ? N6 C34 C33 112.0(3) . . ? C35 C34 C33 125.1(4) . . ? C34 C35 C36 119.6(4) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C37 118.4(4) . . ? C35 C36 H36 120.8 . . ? C37 C36 H36 120.8 . . ? C38 C37 C36 119.0(5) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? N6 C38 C37 122.7(4) . . ? N6 C38 H38 118.6 . . ? C37 C38 H38 118.6 . . ? F7 C39 F8 108.2(4) . . ? F7 C39 F9 108.4(4) . . ? F8 C39 F9 106.8(3) . . ? F7 C39 S3 112.0(3) . . ? F8 C39 S3 110.3(3) . . ? F9 C39 S3 110.9(3) . . ? C7 N1 C1 105.2(3) . . ? C7 N1 Fe1 110.8(2) . . ? C1 N1 Fe1 141.3(3) . . ? C12 N2 C8 117.4(3) . . ? C12 N2 Fe1 127.7(3) . . ? C8 N2 Fe1 114.6(2) . . ? C19 N3 C13 105.5(3) . . ? C19 N3 Fe1 112.6(2) . . ? C13 N3 Fe1 141.1(2) . . ? C24 N4 C20 116.6(3) . . ? C24 N4 Fe1 128.1(3) . . ? C20 N4 Fe1 113.9(2) . . ? C33 N5 C27 106.0(3) . . ? C33 N5 Fe2 111.2(3) . . ? C27 N5 Fe2 141.5(3) . . ? C34 N6 C38 117.3(4) . . ? C34 N6 Fe2 114.0(3) . . ? C38 N6 Fe2 127.8(3) . . ? C7 O1 C6 104.1(3) . . ? C19 O2 C18 104.0(3) . . ? C33 O3 C32 104.4(3) . . ? S1 O4 Fe1 138.66(17) . . ? S22 O7 S2 36.11(18) . . ? S22 O7 Fe1 135.8(2) . . ? S2 O7 Fe1 133.45(19) . . ? S22 O8 S2 37.5(2) . . ? S3 O10 Fe2 138.30(16) . . ? O5 S1 O6 118.0(2) . . ? O5 S1 O4 113.1(2) . . ? O6 S1 O4 113.36(18) . . ? O5 S1 C25 104.3(3) . . ? O6 S1 C25 102.8(2) . . ? O4 S1 C25 103.0(2) . . ? O12 S3 O11 116.35(18) . . ? O12 S3 O10 114.24(17) . . ? O11 S3 O10 114.09(16) . . ? O12 S3 C39 102.68(19) . . ? O11 S3 C39 104.4(2) . . ? O10 S3 C39 102.75(17) . . ? O7 Fe1 O4 85.66(12) . . ? O7 Fe1 N3 101.16(11) . . ? O4 Fe1 N3 89.76(11) . . ? O7 Fe1 N1 92.44(11) . . ? O4 Fe1 N1 99.30(11) . . ? N3 Fe1 N1 164.22(12) . . ? O7 Fe1 N2 167.58(11) . . ? O4 Fe1 N2 91.77(11) . . ? N3 Fe1 N2 90.97(11) . . ? N1 Fe1 N2 75.96(11) . . ? O7 Fe1 N4 86.49(11) . . ? O4 Fe1 N4 161.86(10) . . ? N3 Fe1 N4 75.76(11) . . ? N1 Fe1 N4 97.35(11) . . ? N2 Fe1 N4 99.23(12) . . ? N5 Fe2 N5 166.51(18) . 2_655 ? N5 Fe2 O10 98.31(10) . . ? N5 Fe2 O10 91.40(11) 2_655 . ? N5 Fe2 O10 91.40(11) . 2_655 ? N5 Fe2 O10 98.31(10) 2_655 2_655 ? O10 Fe2 O10 88.02(14) . 2_655 ? N5 Fe2 N6 76.59(13) . . ? N5 Fe2 N6 94.36(12) 2_655 . ? O10 Fe2 N6 88.86(11) . . ? O10 Fe2 N6 167.02(11) 2_655 . ? N5 Fe2 N6 94.36(12) . 2_655 ? N5 Fe2 N6 76.59(13) 2_655 2_655 ? O10 Fe2 N6 167.02(11) . 2_655 ? O10 Fe2 N6 88.86(11) 2_655 2_655 ? N6 Fe2 N6 96.85(17) . 2_655 ? O9 S2 O8 119.4(8) . . ? O9 S2 O7 118.0(6) . . ? O8 S2 O7 108.0(3) . . ? O9 S2 C26 107.7(5) . . ? O8 S2 C26 102.2(3) . . ? O7 S2 C26 98.1(3) . . ? F4 C26 F5 111.8(14) . . ? F4 C26 F6 105.6(13) . . ? F5 C26 F6 107.1(10) . . ? F4 C26 S2 108.9(9) . . ? F5 C26 S2 108.1(6) . . ? F6 C26 S2 115.4(6) . . ? O8 S22 O7 117.7(3) . . ? O8 S22 O99 119.4(8) . . ? O7 S22 O99 116.0(7) . . ? O8 S22 C226 109.0(6) . . ? O7 S22 C226 99.4(5) . . ? O99 S22 C226 87.6(9) . . ? F55 C226 F44 100.5(16) . . ? F55 C226 F66 117.4(16) . . ? F44 C226 F66 127(2) . . ? F55 C226 S22 111.0(15) . . ? F44 C226 S22 111.8(14) . . ? F66 C226 S22 89.2(13) . . ? # END of CIF _database_code_depnum_ccdc_archive 'CCDC 955600'