# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address L.V.Zorina ; Institute of Solid State Physics, RAS, Chernogolovka, MD, 142432, Russia ; S.S.Khasanov ; Institute of Solid State Physics, RAS, Chernogolovka, MD, 142432, Russia ; S.V.Simonov ; Institute of Solid State Physics, RAS, Chernogolovka, MD, 142432, Russia ; R.P.Shibaeva ; Institute of Solid State Physics, RAS, Chernogolovka, MD, 142432, Russia ; ; P.O.Bulanchuk ; ; Institute of Solid State Physics, RAS, Chernogolovka, MD, 142432, Russia ; V.N.Zverev ; Institute of Solid State Physics, RAS, Chernogolovka, MD, 142432, Russia ; E.Canadell ; Institut de Ci\`encia de Materials de Barcelona, CSIC, Campus de la UAB, E-08193 Bellaterra, Spain ; T.G.Prokhorova ; Institute of Problems of Chemical Physics, RAS, Chernogolovka, MD, 142432, Russia ; E.B.Yagubskii ; Institute of Problems of Chemical Physics, RAS, Chernogolovka, MD, 142432, Russia ; _publ_contact_author_address ; Institute of Solid State Physics, RAS, Chernogolovka, MD, 142432, Russia ; _publ_contact_author_email zorina@issp.ac.ru #TrackingRef '- P-1_150K.cif' _publ_contact_author_name 'Zorina, Leokadiya V.' _publ_requested_category FA # Attachment '- X.cif' data_beta''-(BEDT-TTF)4H3O[Fe(C2O4)3](BN)0.35(CB)0.65-(X) _database_code_depnum_ccdc_archive 'CCDC 771736' _audit_creation_method ; CrysAlis RED (Oxford Diffraction Ltd.), SHELXL-97 and WinGX routine-INITIALISE ; _chemical_name_systematic ; ? ; _chemical_compound_source 'synthesis as described' _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 S8), C6 Fe O12, 0.35(C7 H5 N), 0.65(C6 H5 Cl), H3 O' _chemical_formula_sum 'C52.35 H40 Cl0.65 Fe N0.35 O13 S32' _chemical_formula_weight 1986.76 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' 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.2763(6) _cell_length_b 20.0670(10) _cell_length_c 35.369(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.915(6) _cell_angle_gamma 90.00 _cell_volume 7284.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_radiation CuK\a _cell_measurement_reflns_used 8138 _cell_measurement_theta_min 3.7509 _cell_measurement_theta_max 70.9421 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4038 _exptl_absorpt_coefficient_mu 1.209 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63728 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Scale3AbsPack program of CrysAlisPro software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 50869 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 31.68 _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.946 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.075 _reflns_number_total 11242 _reflns_number_gt 8874 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997), DIAMOND 3.1 (Crystal Impact GbR 2005)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0482P)^2^+11.7459P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11242 _refine_ls_number_parameters 484 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.006 _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 S11 S 0.42214(5) 0.21374(3) 0.508284(14) 0.02943(11) Uani 1 1 d . . . S12 S 0.66487(5) 0.14324(3) 0.531331(14) 0.02759(10) Uani 1 1 d . . . S13 S 0.54107(5) 0.24611(3) 0.426537(14) 0.02933(11) Uani 1 1 d . . . S14 S 0.78052(5) 0.17409(3) 0.450844(14) 0.02836(10) Uani 1 1 d . . . S15 S 0.29496(5) 0.19242(3) 0.579630(16) 0.03404(12) Uani 1 1 d . . . S16 S 0.58809(5) 0.11043(3) 0.608650(15) 0.03188(11) Uani 1 1 d . . . S17 S 0.61890(6) 0.27495(3) 0.349549(16) 0.04190(14) Uani 1 1 d . . . S18 S 0.91007(5) 0.19420(3) 0.379202(17) 0.03639(12) Uani 1 1 d . . . C11 C 0.57630(18) 0.18791(9) 0.49630(5) 0.0242(4) Uani 1 1 d . . . C12 C 0.62651(18) 0.20127(9) 0.46207(5) 0.0235(3) Uani 1 1 d . . . C13 C 0.43373(18) 0.17948(10) 0.55408(5) 0.0246(4) Uani 1 1 d . . . C14 C 0.54580(18) 0.14730(9) 0.56473(5) 0.0237(3) Uani 1 1 d . . . C15 C 0.6625(2) 0.24055(10) 0.39392(5) 0.0271(4) Uani 1 1 d . . . C16 C 0.77381(19) 0.20856(10) 0.40535(5) 0.0258(4) Uani 1 1 d . . . C17 C 0.3531(2) 0.16908(11) 0.62725(6) 0.0325(4) Uani 1 1 d . . . H17A H 0.4071 0.2048 0.6378 0.039 Uiso 1 1 calc R . . H17B H 0.2788 0.1644 0.6429 0.039 Uiso 1 1 calc R . . C18 C 0.4312(2) 0.10457(10) 0.62908(6) 0.0305(4) Uani 1 1 d . . . H18A H 0.3809 0.0699 0.6160 0.037 Uiso 1 1 calc R . . H18B H 0.4441 0.0912 0.6554 0.037 Uiso 1 1 calc R . . C19 C 0.7643(3) 0.26208(15) 0.32373(7) 0.0492(6) Uani 1 1 d . . . H19A H 0.7411 0.2642 0.2968 0.059 Uiso 1 1 calc R . . H19B H 0.8247 0.2982 0.3296 0.059 Uiso 1 1 calc R . . C20 C 0.8328(3) 0.19632(14) 0.33225(7) 0.0483(6) Uani 1 1 d . . . H20A H 0.8981 0.1890 0.3138 0.058 Uiso 1 1 calc R . . H20B H 0.7698 0.1604 0.3297 0.058 Uiso 1 1 calc R . . S21 S 0.02556(5) 0.08803(3) 0.519382(14) 0.02890(11) Uani 1 1 d . . . S22 S 0.25958(5) 0.01163(3) 0.544125(13) 0.02733(10) Uani 1 1 d . . . S23 S 0.14774(5) 0.11774(3) 0.439426(13) 0.02869(11) Uani 1 1 d . . . S24 S 0.38456(5) 0.04298(3) 0.463499(14) 0.02723(10) Uani 1 1 d . . . S25 S -0.10898(5) 0.07005(3) 0.589642(17) 0.04186(15) Uani 1 1 d . . . S26 S 0.17233(5) -0.01794(3) 0.621030(15) 0.03428(12) Uani 1 1 d . . . S27 S 0.24294(6) 0.15855(3) 0.365091(15) 0.03776(13) Uani 1 1 d . . . S28 S 0.52105(5) 0.07310(3) 0.393450(15) 0.03091(11) Uani 1 1 d . . . C21 C 0.17946(18) 0.05941(10) 0.50900(5) 0.0242(4) Uani 1 1 d . . . C22 C 0.23229(17) 0.07260(9) 0.47497(5) 0.0235(4) Uani 1 1 d . . . C23 C 0.02968(18) 0.05374(10) 0.56491(5) 0.0257(4) Uani 1 1 d . A . C24 C 0.13763(18) 0.01891(10) 0.57664(5) 0.0242(4) Uani 1 1 d . A . C25 C 0.27492(19) 0.11803(10) 0.40833(5) 0.0254(4) Uani 1 1 d . B . C26 C 0.38423(18) 0.08407(9) 0.41982(5) 0.0235(3) Uani 1 1 d . B . C27A C -0.0456(4) 0.0533(2) 0.63837(12) 0.0352(9) Uani 0.74 1 d P A 1 H27A H 0.0170 0.0876 0.6459 0.042 Uiso 0.74 1 calc PR A 1 H27B H -0.1169 0.0556 0.6553 0.042 Uiso 0.74 1 calc PR A 1 C28A C 0.0194(3) -0.01449(15) 0.64254(8) 0.0304(6) Uani 0.74 1 d P A 1 H28A H -0.0380 -0.0481 0.6311 0.036 Uiso 0.74 1 calc PR A 1 H28B H 0.0324 -0.0249 0.6692 0.036 Uiso 0.74 1 calc PR A 1 C27B C -0.0850(11) 0.0311(7) 0.6321(4) 0.036(3) Uani 0.26 1 d P A 2 H27C H -0.1403 0.0516 0.6502 0.043 Uiso 0.26 1 calc PR A 2 H27D H -0.1108 -0.0152 0.6293 0.043 Uiso 0.26 1 calc PR A 2 C28B C 0.0555(9) 0.0342(5) 0.6474(2) 0.0365(18) Uani 0.26 1 d P A 2 H28C H 0.0591 0.0199 0.6737 0.044 Uiso 0.26 1 calc PR A 2 H28D H 0.0843 0.0802 0.6469 0.044 Uiso 0.26 1 calc PR A 2 C29A C 0.3630(4) 0.1276(2) 0.33444(10) 0.0344(7) Uani 0.75 1 d P B 1 H29A H 0.3210 0.1199 0.3096 0.041 Uiso 0.75 1 calc PR B 1 H29B H 0.4280 0.1620 0.3316 0.041 Uiso 0.75 1 calc PR B 1 C30A C 0.4322(3) 0.06416(17) 0.34708(8) 0.0332(6) Uani 0.75 1 d P B 1 H30A H 0.4932 0.0516 0.3283 0.040 Uiso 0.75 1 calc PR B 1 H30B H 0.3687 0.0286 0.3486 0.040 Uiso 0.75 1 calc PR B 1 C29B C 0.3366(11) 0.0977(6) 0.3379(3) 0.038(2) Uani 0.25 1 d P B 2 H29C H 0.3022 0.0535 0.3422 0.045 Uiso 0.25 1 calc PR B 2 H29D H 0.3226 0.1075 0.3111 0.045 Uiso 0.25 1 calc PR B 2 C30B C 0.4811(10) 0.0970(5) 0.3475(2) 0.0336(18) Uani 0.25 1 d P B 2 H30C H 0.5157 0.1412 0.3434 0.040 Uiso 0.25 1 calc PR B 2 H30D H 0.5224 0.0667 0.3304 0.040 Uiso 0.25 1 calc PR B 2 Fe1 Fe 0.5000 0.08106(2) 0.7500 0.03032(10) Uani 1 2 d S . . O1 O 0.42602(17) 0.15859(8) 0.71907(4) 0.0409(4) Uani 1 1 d . . . O2 O 0.39598(15) 0.01697(8) 0.71657(4) 0.0363(3) Uani 1 1 d . . . O3 O 0.64981(16) 0.06470(8) 0.71693(4) 0.0363(3) Uani 1 1 d . . . O4 O 0.4111(2) 0.27011(9) 0.71862(6) 0.0536(5) Uani 1 1 d . . . O5 O 0.21742(17) -0.04672(9) 0.71476(5) 0.0448(4) Uani 1 1 d . . . O6 O 0.81959(19) -0.00402(10) 0.71150(5) 0.0506(5) Uani 1 1 d . . . C1 C 0.4524(2) 0.21690(12) 0.73197(7) 0.0385(5) Uani 1 1 d . . . C2 C 0.2937(2) -0.00696(11) 0.73044(6) 0.0323(4) Uani 1 1 d . . . C3 C 0.7302(2) 0.01946(11) 0.72875(6) 0.0330(4) Uani 1 1 d . . . Cl31 Cl 0.0238(2) 0.34815(9) 0.75367(6) 0.0409(5) Uiso 0.326(3) 1 d P . 1 C31 C 0.0141(7) 0.2640(2) 0.7485(2) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 C32 C -0.0804(6) 0.2254(3) 0.7648(2) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 H32 H -0.1452 0.2456 0.7782 0.049 Uiso 0.326(3) 1 calc PR . 1 C33 C -0.0782(5) 0.1565(3) 0.76101(18) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 H33 H -0.1414 0.1306 0.7719 0.049 Uiso 0.326(3) 1 calc PR . 1 C34 C 0.0186(5) 0.1262(2) 0.74098(17) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 H34 H 0.0202 0.0801 0.7385 0.049 Uiso 0.326(3) 1 calc PR . 1 C35 C 0.1132(5) 0.1648(3) 0.72473(16) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 H35 H 0.1779 0.1446 0.7113 0.049 Uiso 0.326(3) 1 calc PR . 1 C36 C 0.1109(6) 0.2338(3) 0.7285(2) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 H36 H 0.1741 0.2596 0.7176 0.049 Uiso 0.326(3) 1 calc PR . 1 N41 N 0.0000 0.3726(7) 0.7500 0.0409(5) Uiso 0.348(7) 2 d SP . 2 C45 C 0.0000 0.3230(8) 0.7500 0.0409(5) Uiso 0.348(7) 2 d SP . 2 C41 C 0.0000 0.2489(5) 0.7500 0.0409(5) Uiso 0.348(7) 2 d SP . 2 C42 C 0.0953(8) 0.2151(4) 0.7296(2) 0.0409(5) Uiso 0.348(7) 1 d P . 2 H42 H 0.1573 0.2384 0.7166 0.049 Uiso 0.348(7) 1 calc PR . 2 C43 C 0.0922(8) 0.1474(4) 0.7297(2) 0.0409(5) Uiso 0.348(7) 1 d P . 2 H43 H 0.1519 0.1236 0.7162 0.049 Uiso 0.348(7) 1 calc PR . 2 C44 C 0.0000 0.1135(6) 0.7500 0.0409(5) Uiso 0.348(7) 2 d SP . 2 H44 H 0.0000 0.0672 0.7500 0.049 Uiso 0.348(7) 2 calc SPR . 2 O51 O 0.0101(6) -0.09987(14) 0.75499(15) 0.0464(9) Uiso 0.50 1 d PD . . H51A H 0.046(4) -0.151(2) 0.7674(16) 0.070 Uiso 0.50 1 d PD . . H51B H 0.090(4) -0.059(2) 0.7621(18) 0.070 Uiso 0.50 1 d PD . . H51C H -0.086(5) -0.084(2) 0.7689(18) 0.070 Uiso 0.50 1 d PD . . 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 S11 0.0249(2) 0.0382(3) 0.0253(2) 0.0037(2) 0.00228(18) 0.00720(19) S12 0.0233(2) 0.0363(3) 0.0234(2) 0.00607(19) 0.00412(17) 0.00582(18) S13 0.0259(2) 0.0366(3) 0.0253(2) 0.00447(19) 0.00048(18) 0.00661(19) S14 0.0244(2) 0.0341(2) 0.0268(2) 0.00516(19) 0.00274(17) 0.00553(18) S15 0.0259(2) 0.0443(3) 0.0326(3) 0.0024(2) 0.00790(19) 0.0081(2) S16 0.0282(2) 0.0413(3) 0.0265(2) 0.0099(2) 0.00501(19) 0.0054(2) S17 0.0519(3) 0.0502(3) 0.0231(3) 0.0079(2) -0.0027(2) 0.0039(3) S18 0.0353(3) 0.0363(3) 0.0390(3) 0.0019(2) 0.0163(2) 0.0017(2) C11 0.0232(8) 0.0277(9) 0.0216(9) 0.0003(7) 0.0008(7) 0.0014(7) C12 0.0228(8) 0.0266(9) 0.0210(8) 0.0017(7) 0.0009(7) 0.0024(7) C13 0.0253(9) 0.0280(9) 0.0209(8) 0.0001(7) 0.0050(7) 0.0003(7) C14 0.0251(8) 0.0268(9) 0.0192(8) 0.0024(7) 0.0026(7) 0.0001(7) C15 0.0327(10) 0.0286(9) 0.0200(9) 0.0011(7) 0.0014(7) -0.0005(8) C16 0.0274(9) 0.0261(9) 0.0243(9) 0.0010(7) 0.0058(7) -0.0008(7) C17 0.0341(10) 0.0359(11) 0.0284(10) -0.0006(8) 0.0100(8) 0.0030(8) C18 0.0302(10) 0.0321(10) 0.0300(10) 0.0037(8) 0.0097(8) -0.0012(8) C19 0.0509(14) 0.0734(18) 0.0233(11) 0.0065(11) 0.0025(10) -0.0170(13) C20 0.0563(15) 0.0565(16) 0.0337(13) -0.0147(11) 0.0173(11) -0.0124(12) S21 0.0251(2) 0.0409(3) 0.0209(2) 0.00603(19) 0.00289(17) 0.00969(19) S22 0.0244(2) 0.0357(3) 0.0221(2) 0.00544(18) 0.00335(17) 0.00805(18) S23 0.0248(2) 0.0416(3) 0.0200(2) 0.00504(19) 0.00413(17) 0.01064(19) S24 0.0246(2) 0.0332(2) 0.0241(2) 0.00410(18) 0.00318(17) 0.00781(18) S25 0.0305(3) 0.0645(4) 0.0316(3) 0.0151(3) 0.0117(2) 0.0196(3) S26 0.0264(2) 0.0463(3) 0.0305(3) 0.0182(2) 0.00491(19) 0.0049(2) S27 0.0466(3) 0.0435(3) 0.0240(2) 0.0102(2) 0.0108(2) 0.0174(2) S28 0.0256(2) 0.0339(3) 0.0341(3) 0.0013(2) 0.01074(19) 0.00510(19) C21 0.0233(8) 0.0292(9) 0.0201(8) 0.0020(7) 0.0008(6) 0.0043(7) C22 0.0220(8) 0.0290(9) 0.0196(8) 0.0019(7) 0.0006(6) 0.0049(7) C23 0.0247(8) 0.0321(9) 0.0205(9) 0.0049(7) 0.0042(7) 0.0042(7) C24 0.0230(8) 0.0279(9) 0.0220(9) 0.0056(7) 0.0035(7) 0.0014(7) C25 0.0290(9) 0.0271(9) 0.0207(9) 0.0030(7) 0.0063(7) 0.0060(7) C26 0.0234(8) 0.0256(9) 0.0220(9) 0.0008(7) 0.0050(7) 0.0023(7) C27A 0.038(3) 0.045(2) 0.0226(17) 0.0038(16) 0.0059(16) 0.0108(16) C28A 0.0267(13) 0.0380(15) 0.0271(13) 0.0116(11) 0.0082(10) 0.0039(11) C27B 0.024(5) 0.055(8) 0.028(6) 0.015(5) 0.008(4) 0.009(4) C28B 0.039(5) 0.046(5) 0.025(4) 0.001(3) 0.003(3) 0.000(4) C29A 0.0356(17) 0.043(2) 0.0248(15) 0.0012(15) 0.0079(12) 0.0039(15) C30A 0.0390(16) 0.0340(16) 0.0274(14) -0.0060(12) 0.0081(12) 0.0065(13) C29B 0.050(6) 0.046(6) 0.018(4) -0.004(4) 0.011(4) -0.016(5) C30B 0.041(5) 0.035(5) 0.026(4) -0.002(4) 0.011(4) -0.001(4) Fe1 0.0370(2) 0.0329(2) 0.02130(19) 0.000 0.00394(16) 0.000 O1 0.0561(10) 0.0378(8) 0.0286(8) 0.0028(6) -0.0004(7) 0.0036(7) O2 0.0381(8) 0.0464(9) 0.0250(7) -0.0052(6) 0.0069(6) -0.0047(7) O3 0.0408(8) 0.0426(9) 0.0261(7) 0.0037(6) 0.0076(6) -0.0026(7) O4 0.0621(12) 0.0402(10) 0.0590(12) 0.0117(9) 0.0092(10) 0.0056(8) O5 0.0408(9) 0.0550(11) 0.0386(9) -0.0043(8) 0.0019(7) -0.0090(8) O6 0.0523(11) 0.0609(12) 0.0405(10) 0.0013(8) 0.0207(8) 0.0058(9) C1 0.0434(12) 0.0388(12) 0.0345(12) 0.0046(9) 0.0132(10) 0.0003(10) C2 0.0341(10) 0.0374(11) 0.0255(10) 0.0026(8) 0.0022(8) 0.0048(9) C3 0.0359(11) 0.0378(11) 0.0259(10) -0.0044(8) 0.0077(8) -0.0087(9) _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 S11 C11 1.7396(19) . ? S11 C13 1.7582(19) . ? S12 C14 1.7454(19) . ? S12 C11 1.7471(19) . ? S13 C12 1.7458(19) . ? S13 C15 1.746(2) . ? S14 C12 1.7390(19) . ? S14 C16 1.750(2) . ? S15 C13 1.7460(19) . ? S15 C17 1.819(2) . ? S16 C14 1.7552(19) . ? S16 C18 1.803(2) . ? S17 C15 1.752(2) . ? S17 C19 1.809(3) . ? S18 C16 1.7410(19) . ? S18 C20 1.804(3) . ? C11 C12 1.367(3) . ? C13 C14 1.357(3) . ? C15 C16 1.355(3) . ? C17 C18 1.523(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.518(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? S21 C21 1.7392(19) . ? S21 C23 1.7497(19) . ? S22 C21 1.7427(19) . ? S22 C24 1.7496(19) . ? S23 C22 1.7449(19) . ? S23 C25 1.7504(19) . ? S24 C22 1.7410(18) . ? S24 C26 1.7509(19) . ? S25 C27B 1.700(12) . ? S25 C23 1.7405(19) . ? S25 C27A 1.842(4) . ? S26 C24 1.7554(19) . ? S26 C28A 1.782(3) . ? S26 C28B 1.876(9) . ? S27 C25 1.7485(19) . ? S27 C29A 1.794(3) . ? S27 C29B 1.855(12) . ? S28 C30B 1.724(9) . ? S28 C26 1.7403(18) . ? S28 C30A 1.845(3) . ? C21 C22 1.371(3) . ? C23 C24 1.358(3) . ? C25 C26 1.358(3) . ? C27A C28A 1.519(5) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C27B C28B 1.518(14) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C28B H28C 0.9700 . ? C28B H28D 0.9700 . ? C29A C30A 1.514(5) . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C30A H30A 0.9700 . ? C30A H30B 0.9700 . ? C29B C30B 1.506(15) . ? C29B H29C 0.9700 . ? C29B H29D 0.9700 . ? C30B H30C 0.9700 . ? C30B H30D 0.9700 . ? Fe1 O3 2.0071(15) 2_656 ? Fe1 O3 2.0071(15) . ? Fe1 O2 2.0166(16) . ? Fe1 O2 2.0166(16) 2_656 ? Fe1 O1 2.0275(17) 2_656 ? Fe1 O1 2.0275(17) . ? O1 C1 1.280(3) . ? O2 C2 1.276(3) . ? O3 C3 1.283(3) . ? O4 C1 1.234(3) . ? O5 C2 1.231(3) . ? O6 C3 1.222(3) . ? C1 C1 1.568(5) 2_656 ? C2 C3 1.569(3) 2_656 ? C3 C2 1.569(3) 2_656 ? Cl31 Cl31 0.542(4) 2_556 ? Cl31 C31 1.700(5) . ? Cl31 C31 1.733(5) 2_556 ? C31 C31 0.313(12) 2_556 ? C31 C32 1.149(7) 2_556 ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 C36 1.669(9) 2_556 ? C31 Cl31 1.733(4) 2_556 ? C32 C33 1.3900 . ? C32 H32 0.9300 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 C36 1.3900 . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? N41 C45 1.00(2) . ? C45 C41 1.486(17) . ? C41 C42 1.419(8) 2_556 ? C41 C42 1.419(8) . ? C42 C43 1.359(10) . ? C42 H42 0.9300 . ? C43 C44 1.395(9) . ? C43 H43 0.9300 . ? C44 C43 1.395(9) 2_556 ? C44 H44 0.9300 . ? O51 H51A 1.17(3) . ? O51 H51B 1.17(4) . ? O51 H51C 1.17(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 C11 S11 C13 95.05(9) . . ? C14 S12 C11 95.63(9) . . ? C12 S13 C15 95.31(9) . . ? C12 S14 C16 95.29(9) . . ? C13 S15 C17 101.67(9) . . ? C14 S16 C18 101.30(10) . . ? C15 S17 C19 102.46(11) . . ? C16 S18 C20 99.02(11) . . ? C12 C11 S11 123.16(15) . . ? C12 C11 S12 121.49(15) . . ? S11 C11 S12 115.35(11) . . ? C11 C12 S14 121.99(14) . . ? C11 C12 S13 122.70(14) . . ? S14 C12 S13 115.31(10) . . ? C14 C13 S15 129.14(15) . . ? C14 C13 S11 117.29(14) . . ? S15 C13 S11 113.57(11) . . ? C13 C14 S12 116.67(14) . . ? C13 C14 S16 127.93(15) . . ? S12 C14 S16 115.39(10) . . ? C16 C15 S13 116.99(15) . . ? C16 C15 S17 128.88(16) . . ? S13 C15 S17 114.07(11) . . ? C15 C16 S18 127.53(16) . . ? C15 C16 S14 117.07(15) . . ? S18 C16 S14 115.34(11) . . ? C18 C17 S15 113.94(15) . . ? C18 C17 H17A 108.8 . . ? S15 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? S15 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C17 C18 S16 114.05(14) . . ? C17 C18 H18A 108.7 . . ? S16 C18 H18A 108.7 . . ? C17 C18 H18B 108.7 . . ? S16 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C20 C19 S17 114.22(17) . . ? C20 C19 H19A 108.7 . . ? S17 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? S17 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C19 C20 S18 112.41(17) . . ? C19 C20 H20A 109.1 . . ? S18 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? S18 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? C21 S21 C23 94.87(9) . . ? C21 S22 C24 95.42(9) . . ? C22 S23 C25 95.40(9) . . ? C22 S24 C26 94.78(9) . . ? C27B S25 C23 105.8(4) . . ? C23 S25 C27A 100.15(16) . . ? C24 S26 C28A 102.82(11) . . ? C24 S26 C28B 96.0(3) . . ? C25 S27 C29A 105.24(13) . . ? C25 S27 C29B 93.9(4) . . ? C30B S28 C26 108.1(3) . . ? C26 S28 C30A 96.43(12) . . ? C22 C21 S21 121.78(14) . . ? C22 C21 S22 122.56(14) . . ? S21 C21 S22 115.65(11) . . ? C21 C22 S24 122.64(14) . . ? C21 C22 S23 121.85(14) . . ? S24 C22 S23 115.46(10) . . ? C24 C23 S25 128.33(15) . . ? C24 C23 S21 117.69(14) . . ? S25 C23 S21 113.98(11) . . ? C23 C24 S22 116.32(14) . . ? C23 C24 S26 128.00(15) . . ? S22 C24 S26 115.66(10) . . ? C26 C25 S27 127.65(15) . . ? C26 C25 S23 116.29(14) . . ? S27 C25 S23 115.98(11) . . ? C25 C26 S28 125.55(15) . . ? C25 C26 S24 117.69(14) . . ? S28 C26 S24 116.61(10) . . ? C28A C27A S25 112.8(3) . . ? C28A C27A H27A 109.0 . . ? S25 C27A H27A 109.0 . . ? C28A C27A H27B 109.0 . . ? S25 C27A H27B 109.0 . . ? H27A C27A H27B 107.8 . . ? C27A C28A S26 112.7(2) . . ? C27A C28A H28A 109.0 . . ? S26 C28A H28A 109.0 . . ? C27A C28A H28B 109.0 . . ? S26 C28A H28B 109.0 . . ? H28A C28A H28B 107.8 . . ? C28B C27B S25 112.9(8) . . ? C28B C27B H27C 109.0 . . ? S25 C27B H27C 109.0 . . ? C28B C27B H27D 109.0 . . ? S25 C27B H27D 109.0 . . ? H27C C27B H27D 107.8 . . ? C27B C28B S26 114.9(7) . . ? C27B C28B H28C 108.5 . . ? S26 C28B H28C 108.5 . . ? C27B C28B H28D 108.5 . . ? S26 C28B H28D 108.5 . . ? H28C C28B H28D 107.5 . . ? C30A C29A S27 116.1(2) . . ? C30A C29A H29A 108.3 . . ? S27 C29A H29A 108.3 . . ? C30A C29A H29B 108.3 . . ? S27 C29A H29B 108.3 . . ? H29A C29A H29B 107.4 . . ? C29A C30A S28 112.6(2) . . ? C29A C30A H30A 109.1 . . ? S28 C30A H30A 109.1 . . ? C29A C30A H30B 109.1 . . ? S28 C30A H30B 109.1 . . ? H30A C30A H30B 107.8 . . ? C30B C29B S27 114.8(7) . . ? C30B C29B H29C 108.6 . . ? S27 C29B H29C 108.6 . . ? C30B C29B H29D 108.6 . . ? S27 C29B H29D 108.6 . . ? H29C C29B H29D 107.5 . . ? C29B C30B S28 113.6(7) . . ? C29B C30B H30C 108.8 . . ? S28 C30B H30C 108.8 . . ? C29B C30B H30D 108.8 . . ? S28 C30B H30D 108.8 . . ? H30C C30B H30D 107.7 . . ? O3 Fe1 O3 161.17(10) 2_656 . ? O3 Fe1 O2 80.67(6) 2_656 . ? O3 Fe1 O2 87.33(6) . . ? O3 Fe1 O2 87.33(6) 2_656 2_656 ? O3 Fe1 O2 80.67(6) . 2_656 ? O2 Fe1 O2 100.75(10) . 2_656 ? O3 Fe1 O1 95.09(7) 2_656 2_656 ? O3 Fe1 O1 99.34(7) . 2_656 ? O2 Fe1 O1 168.19(7) . 2_656 ? O2 Fe1 O1 90.00(7) 2_656 2_656 ? O3 Fe1 O1 99.34(7) 2_656 . ? O3 Fe1 O1 95.09(7) . . ? O2 Fe1 O1 90.00(7) . . ? O2 Fe1 O1 168.19(7) 2_656 . ? O1 Fe1 O1 79.77(10) 2_656 . ? C1 O1 Fe1 116.26(15) . . ? C2 O2 Fe1 115.90(14) . . ? C3 O3 Fe1 115.24(13) . . ? O4 C1 O1 126.3(2) . . ? O4 C1 C1 119.99(15) . 2_656 ? O1 C1 C1 113.71(13) . 2_656 ? O5 C2 O2 126.1(2) . . ? O5 C2 C3 120.5(2) . 2_656 ? O2 C2 C3 113.43(19) . 2_656 ? O6 C3 O3 126.7(2) . . ? O6 C3 C2 119.1(2) . 2_656 ? O3 C3 C2 114.20(18) . 2_656 ? Cl31 Cl31 C31 84.4(3) 2_556 . ? Cl31 Cl31 C31 77.5(3) 2_556 2_556 ? C31 C31 C32 135.7(11) 2_556 2_556 ? C32 C31 C32 103.6(3) 2_556 . ? C31 C31 C36 150.3(16) 2_556 . ? C32 C31 C36 120.0 . . ? C32 C31 C36 116.17(19) 2_556 2_556 ? C36 C31 C36 132.63(14) . 2_556 ? C31 C31 Cl31 90.9(4) 2_556 . ? C32 C31 Cl31 132.9(6) 2_556 . ? C32 C31 Cl31 123.3(3) . . ? C36 C31 Cl31 116.7(3) . . ? C36 C31 Cl31 110.6(5) 2_556 . ? C31 C31 Cl31 78.8(5) 2_556 2_556 ? C32 C31 Cl31 140.9(7) 2_556 2_556 ? C32 C31 Cl31 113.7(4) . 2_556 ? C36 C31 Cl31 124.6(4) . 2_556 ? C36 C31 Cl31 101.5(5) 2_556 2_556 ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? N41 C45 C41 180.000(8) . . ? C42 C41 C42 122.9(10) 2_556 . ? C42 C41 C45 118.6(5) 2_556 . ? C42 C41 C45 118.6(5) . . ? C43 C42 C41 117.3(7) . . ? C43 C42 H42 121.3 . . ? C41 C42 H42 121.3 . . ? C42 C43 C44 120.4(7) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C43 121.6(10) . 2_556 ? C43 C44 H44 119.2 . . ? C43 C44 H44 119.2 2_556 . ? H51A O51 H51B 109(2) . . ? H51A O51 H51C 110(2) . . ? H51B O51 H51C 108(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C20 H20A O4 0.97 2.46 3.332(3) 149.0 7_656 C27A H27B O6 0.97 2.44 3.208(5) 136.1 1_455 C28A H28B O5 0.97 2.47 3.249(3) 137.5 . C27B H27C O6 0.97 2.49 3.102(12) 120.9 1_455 C28B H28C O5 0.97 2.51 3.267(9) 134.6 . C30A H30A O2 0.97 2.43 3.353(3) 159.5 5_656 C29B H29C O6 0.97 2.43 2.978(11) 115.3 5_656 C30B H30D O2 0.97 2.53 3.500(9) 173.3 5_656 C35 H35 O1 0.93 2.57 3.234(5) 129.1 . C36 H36 O4 0.93 2.44 3.206(6) 139.4 . O51 H51B O6 1.17(4) 1.70(4) 2.821(5) 158(5) 2_656 O51 H51C O5 1.17(3) 1.67(4) 2.829(6) 169(4) 2_556 O51 H51A O4 1.17(3) 1.71(3) 2.874(4) 173(5) 4_546 data_beta''-(BEDT-TTF)4H3O[Fe(C2O4)3](BN)0.35(CB)0.65-150K _database_code_depnum_ccdc_archive 'CCDC 833651' _audit_creation_method ; CrysAlis RED (Oxford Diffraction Ltd.), SHELXL-97 and WinGX routine-INITIALISE ; _chemical_compound_source 'synthesis as described' _chemical_melting_point ? _chemical_name_common ? _chemical_formula_moiety '4(C10 H8 S8), C6 Fe O12, 0.35(C7 H5 N), 0.65(C6 H5 Cl), H3 O' _chemical_formula_sum 'C52.35 H40 Cl0.65 Fe N0.35 O13 S32' _chemical_formula_weight 1986.76 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' 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2649(3) _cell_length_b 11.1956(3) _cell_length_c 35.1514(10) _cell_angle_alpha 88.619(2) _cell_angle_beta 86.651(2) _cell_angle_gamma 62.748(3) _cell_volume 3585.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 22669 _cell_measurement_theta_min 2.5499 _cell_measurement_theta_max 33.1050 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2019 _exptl_absorpt_coefficient_mu 1.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83949 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 10.4752 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45485 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 32.99 _reflns_number_total 23141 _reflns_number_gt 19179 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND 3.1 (Crystal Impact GbR 2005)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0688P)^2^+4.7785P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23141 _refine_ls_number_parameters 987 _refine_ls_number_restraints 125 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.002 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 S11 S -0.42388(10) 0.08219(10) -0.03581(3) 0.01911(18) Uani 1 1 d . . . S12 S -0.26201(10) 0.23286(10) -0.05983(3) 0.01938(18) Uani 1 1 d . . . S13 S -0.27145(10) 0.02305(10) 0.04515(3) 0.01862(17) Uani 1 1 d . . . S14 S -0.11208(10) 0.17528(10) 0.02053(3) 0.01972(18) Uani 1 1 d . . . S15 S -0.59145(10) 0.14220(10) -0.10551(3) 0.02267(19) Uani 1 1 d . . . S16 S -0.39949(12) 0.31348(11) -0.13440(3) 0.0257(2) Uani 1 1 d . . . S17 S -0.15957(10) -0.03297(11) 0.12269(3) 0.0233(2) Uani 1 1 d . . . S18 S 0.03784(12) 0.14107(13) 0.09140(3) 0.0282(2) Uani 1 1 d . . . C11 C -0.3026(4) 0.1432(4) -0.02419(10) 0.0168(6) Uani 1 1 d . . . C12 C -0.2374(4) 0.1175(4) 0.00982(10) 0.0167(7) Uani 1 1 d . . . C13 C -0.4648(4) 0.1647(4) -0.07953(10) 0.0163(6) Uani 1 1 d . A . C14 C -0.3898(4) 0.2334(4) -0.09086(11) 0.0172(7) Uani 1 1 d . A . C15 C -0.1582(4) 0.0385(4) 0.07803(11) 0.0158(6) Uani 1 1 d . . . C16 C -0.0840(4) 0.1085(4) 0.06635(11) 0.0184(7) Uani 1 1 d . . . C17A C -0.4893(8) 0.1220(7) -0.15318(19) 0.0224(12) Uani 0.60 1 d P A 1 H17A H -0.3895 0.0512 -0.1517 0.027 Uiso 0.60 1 calc PR A 1 H17B H -0.5365 0.0964 -0.1722 0.027 Uiso 0.60 1 calc PR A 1 C18A C -0.4870(9) 0.2533(9) -0.1649(2) 0.0256(14) Uani 0.60 1 d P A 1 H18A H -0.5876 0.3220 -0.1668 0.031 Uiso 0.60 1 calc PR A 1 H18B H -0.4388 0.2410 -0.1901 0.031 Uiso 0.60 1 calc PR A 1 C17B C -0.5755(11) 0.1892(10) -0.1520(2) 0.0192(16) Uani 0.40 1 d P A 2 H17C H -0.5879 0.1285 -0.1690 0.023 Uiso 0.40 1 calc PR A 2 H17D H -0.6539 0.2788 -0.1560 0.023 Uiso 0.40 1 calc PR A 2 C18B C -0.4298(11) 0.1886(11) -0.1625(3) 0.0203(18) Uani 0.40 1 d P A 2 H18C H -0.4256 0.2085 -0.1894 0.024 Uiso 0.40 1 calc PR A 2 H18D H -0.3511 0.0994 -0.1582 0.024 Uiso 0.40 1 calc PR A 2 C19 C -0.0082(4) -0.0258(5) 0.14381(13) 0.0256(8) Uani 1 1 d . . . H19A H -0.0106 -0.0468 0.1707 0.031 Uiso 1 1 calc R . . H19B H 0.0826 -0.0944 0.1322 0.031 Uiso 1 1 calc R . . C20 C -0.0074(5) 0.1092(5) 0.13973(12) 0.0266(9) Uani 1 1 d . . . H20A H 0.0635 0.1117 0.1564 0.032 Uiso 1 1 calc R . . H20B H -0.1033 0.1798 0.1478 0.032 Uiso 1 1 calc R . . S21 S 0.04467(10) 0.34594(10) -0.04778(3) 0.01902(18) Uani 1 1 d . . . S22 S 0.21404(10) 0.48789(10) -0.07362(3) 0.01987(18) Uani 1 1 d . . . S23 S 0.19045(10) 0.28746(10) 0.03230(3) 0.01898(17) Uani 1 1 d . . . S24 S 0.36617(10) 0.42547(10) 0.00846(3) 0.02025(18) Uani 1 1 d . . . S25 S 0.29613(10) 0.22772(11) 0.11027(3) 0.02211(19) Uani 1 1 d . . . S26 S 0.51170(11) 0.38741(11) 0.08020(3) 0.0240(2) Uani 1 1 d . . . S27 S -0.10710(10) 0.38483(10) -0.11930(3) 0.02146(18) Uani 1 1 d . . . S28 S 0.10680(12) 0.54185(11) -0.15073(3) 0.0256(2) Uani 1 1 d . . . C21 C 0.1726(4) 0.4012(4) -0.03727(11) 0.0177(7) Uani 1 1 d . . . C22 C 0.2357(4) 0.3748(4) -0.00331(11) 0.0165(7) Uani 1 1 d . . . C23 C 0.0159(4) 0.4138(4) -0.09341(11) 0.0173(7) Uani 1 1 d . . . C24 C 0.0958(4) 0.4766(4) -0.10585(10) 0.0165(6) Uani 1 1 d . . . C25 C 0.3043(4) 0.2979(4) 0.06573(10) 0.0166(7) Uani 1 1 d . . . C26 C 0.3864(4) 0.3603(4) 0.05476(11) 0.0174(7) Uani 1 1 d . . . C27 C -0.0267(5) 0.3800(5) -0.16657(12) 0.0286(8) Uani 1 1 d . . . H27A H 0.0723 0.3068 -0.1682 0.034 Uiso 1 1 calc R . . H27B H -0.0832 0.3626 -0.1849 0.034 Uiso 1 1 calc R . . C28 C -0.0220(5) 0.5108(5) -0.17689(12) 0.0282(9) Uani 1 1 d . . . H28A H -0.1194 0.5848 -0.1723 0.034 Uiso 1 1 calc R . . H28B H 0.0037 0.5096 -0.2039 0.034 Uiso 1 1 calc R . . C29 C 0.4619(4) 0.2122(4) 0.12983(12) 0.0209(7) Uani 1 1 d . . . H29A H 0.4635 0.1844 0.1562 0.025 Uiso 1 1 calc R . . H29B H 0.5456 0.1418 0.1161 0.025 Uiso 1 1 calc R . . C30 C 0.4790(5) 0.3403(4) 0.12806(12) 0.0234(8) Uani 1 1 d . . . H30A H 0.5601 0.3282 0.1432 0.028 Uiso 1 1 calc R . . H30B H 0.3907 0.4131 0.1394 0.028 Uiso 1 1 calc R . . S31 S 0.20761(10) 0.42983(10) 0.49291(3) 0.02098(18) Uani 1 1 d . . . S32 S 0.52260(10) 0.28471(10) 0.46998(3) 0.02002(18) Uani 1 1 d . . . S33 S 0.29081(10) 0.50063(10) 0.57449(3) 0.02129(19) Uani 1 1 d . . . S34 S 0.60464(10) 0.35187(10) 0.55084(3) 0.02064(18) Uani 1 1 d . . . S35 S 0.10368(10) 0.37974(11) 0.42192(3) 0.02349(19) Uani 1 1 d . . . S36 S 0.48089(10) 0.21166(11) 0.39285(3) 0.02211(19) Uani 1 1 d . . . S37 S 0.33450(13) 0.56467(13) 0.65158(3) 0.0322(2) Uani 1 1 d . . . S38 S 0.70991(12) 0.39722(11) 0.62286(3) 0.0291(2) Uani 1 1 d . . . C31 C 0.3874(4) 0.3770(4) 0.50468(11) 0.0186(7) Uani 1 1 d . . . C32 C 0.4233(4) 0.4068(4) 0.53914(11) 0.0173(7) Uani 1 1 d . . . C33 C 0.2552(4) 0.3560(4) 0.44731(11) 0.0181(7) Uani 1 1 d . . . C34 C 0.3999(4) 0.2895(4) 0.43656(11) 0.0165(7) Uani 1 1 d . . . C35 C 0.4160(4) 0.4914(4) 0.60730(11) 0.0201(7) Uani 1 1 d . . . C36 C 0.5606(4) 0.4245(4) 0.59637(11) 0.0202(7) Uani 1 1 d . . . C37 C 0.1871(4) 0.3308(4) 0.37398(12) 0.0230(8) Uani 1 1 d . . . H37A H 0.1177 0.3210 0.3584 0.028 Uiso 1 1 calc R . . H37B H 0.2056 0.4024 0.3631 0.028 Uiso 1 1 calc R . . C38 C 0.3289(4) 0.2018(4) 0.37212(12) 0.0226(8) Uani 1 1 d . . . H38A H 0.3559 0.1750 0.3456 0.027 Uiso 1 1 calc R . . H38B H 0.3124 0.1321 0.3852 0.027 Uiso 1 1 calc R . . C39 C 0.4894(6) 0.5468(5) 0.67719(13) 0.0373(11) Uani 1 1 d . . . H39A H 0.5139 0.6182 0.6696 0.045 Uiso 1 1 calc R . . H39B H 0.4621 0.5568 0.7042 0.045 Uiso 1 1 calc R . . C40 C 0.6254(6) 0.4108(6) 0.67013(14) 0.0419(12) Uani 1 1 d . . . H40A H 0.5972 0.3394 0.6737 0.050 Uiso 1 1 calc R . . H40B H 0.6965 0.3988 0.6887 0.050 Uiso 1 1 calc R . . S41 S 0.93756(9) 0.17562(10) 0.48181(3) 0.02039(18) Uani 1 1 d . . . S42 S 1.24922(9) 0.02112(10) 0.45655(3) 0.01923(18) Uani 1 1 d . . . S43 S 1.02886(10) 0.23971(10) 0.56154(3) 0.02049(19) Uani 1 1 d . . . S44 S 1.34176(9) 0.09047(10) 0.53684(3) 0.01892(17) Uani 1 1 d . . . S45 S 0.82141(10) 0.13323(12) 0.41202(3) 0.0286(2) Uani 1 1 d . . . S46 S 1.19202(11) -0.04467(12) 0.37996(3) 0.0249(2) Uani 1 1 d . . . S47 S 1.07940(11) 0.32564(11) 0.63582(3) 0.0260(2) Uani 1 1 d . . . S48 S 1.44606(10) 0.15450(10) 0.60729(3) 0.02068(18) Uani 1 1 d . . . C41 C 1.1208(4) 0.1185(4) 0.49172(11) 0.0186(7) Uani 1 1 d . . . C42 C 1.1601(4) 0.1471(4) 0.52574(10) 0.0177(7) Uani 1 1 d . . . C43 C 0.9763(4) 0.1033(4) 0.43641(11) 0.0182(7) Uani 1 1 d . B . C44 C 1.1200(4) 0.0323(4) 0.42418(11) 0.0187(7) Uani 1 1 d . B . C45 C 1.1548(4) 0.2429(4) 0.59262(11) 0.0190(7) Uani 1 1 d . . . C46 C 1.2997(4) 0.1743(4) 0.58060(10) 0.0170(7) Uani 1 1 d . . . C47A C 0.9045(8) 0.0992(9) 0.3626(2) 0.0239(15) Uani 0.62 1 d P B 1 H47A H 0.8311 0.1053 0.3455 0.029 Uiso 0.62 1 calc PR B 1 H47B H 0.9338 0.1679 0.3553 0.029 Uiso 0.62 1 calc PR B 1 C48A C 1.0371(6) -0.0379(6) 0.35793(18) 0.0184(11) Uani 0.62 1 d P B 1 H48A H 1.0616 -0.0581 0.3310 0.022 Uiso 0.62 1 calc PR B 1 H48B H 1.0128 -0.1057 0.3691 0.022 Uiso 0.62 1 calc PR B 1 C47B C 0.8866(13) 0.0540(13) 0.3687(3) 0.021(2) Uani 0.38 1 d P B 2 H47C H 0.9100 -0.0401 0.3714 0.026 Uiso 0.38 1 calc PR B 2 H47D H 0.8103 0.0937 0.3506 0.026 Uiso 0.38 1 calc PR B 2 C48B C 1.0221(11) 0.0643(11) 0.3532(3) 0.026(2) Uani 0.38 1 d P B 2 H48C H 1.0036 0.1572 0.3546 0.031 Uiso 0.38 1 calc PR B 2 H48D H 1.0404 0.0379 0.3265 0.031 Uiso 0.38 1 calc PR B 2 C49 C 1.2331(5) 0.2665(5) 0.66638(12) 0.0306(10) Uani 1 1 d . . . H49A H 1.2625 0.3370 0.6684 0.037 Uiso 1 1 calc R . . H49B H 1.1999 0.2521 0.6917 0.037 Uiso 1 1 calc R . . C50 C 1.3670(5) 0.1386(5) 0.65364(13) 0.0305(9) Uani 1 1 d . . . H50A H 1.3397 0.0665 0.6525 0.037 Uiso 1 1 calc R . . H50B H 1.4406 0.1144 0.6724 0.037 Uiso 1 1 calc R . . Fe1 Fe 0.40357(6) 0.15782(5) 0.251137(19) 0.02363(11) Uani 1 1 d . . . O1 O 0.3735(3) 0.0242(3) 0.28447(9) 0.0290(6) Uani 1 1 d . . . O2 O 0.2737(3) 0.1188(3) 0.21820(8) 0.0286(6) Uani 1 1 d . . . O3 O 0.5666(3) 0.1323(3) 0.28468(8) 0.0257(6) Uani 1 1 d . . . O4 O 0.5765(3) 0.0336(3) 0.21740(9) 0.0285(6) Uani 1 1 d . . . O5 O 0.2461(3) 0.3100(3) 0.28273(9) 0.0298(6) Uani 1 1 d . . . O6 O 0.3942(3) 0.3153(3) 0.22047(8) 0.0292(6) Uani 1 1 d . . . O7 O 0.2641(4) -0.1087(4) 0.28695(10) 0.0339(7) Uani 1 1 d . . . O8 O 0.1697(4) -0.0182(4) 0.21459(10) 0.0410(8) Uani 1 1 d . . . O9 O 0.8043(3) -0.0061(3) 0.29131(9) 0.0323(7) Uani 1 1 d . . . O10 O 0.8205(3) -0.0888(4) 0.21628(9) 0.0338(7) Uani 1 1 d . . . O11 O 0.1173(3) 0.5343(3) 0.28466(10) 0.0392(8) Uani 1 1 d . . . O12 O 0.2956(3) 0.5401(3) 0.22240(10) 0.0365(7) Uani 1 1 d . . . C1 C 0.2962(4) -0.0266(5) 0.27106(13) 0.0281(9) Uani 1 1 d . . . C2 C 0.2401(4) 0.0283(5) 0.23101(13) 0.0282(9) Uani 1 1 d . . . C3 C 0.6942(4) 0.0408(4) 0.27338(11) 0.0239(8) Uani 1 1 d . . . C4 C 0.7026(4) -0.0117(4) 0.23165(11) 0.0233(8) Uani 1 1 d . . . C5 C 0.2122(4) 0.4293(5) 0.27051(12) 0.0277(8) Uani 1 1 d . . . C6 C 0.3085(4) 0.4316(4) 0.23462(12) 0.0277(8) Uani 1 1 d . . . O1WA O 1.0849(9) -0.2013(7) 0.2519(5) 0.0342(9) Uiso 0.56(4) 1 d PD C 1 O1WB O 1.0755(12) -0.2080(10) 0.2615(5) 0.0342(9) Uiso 0.44(4) 1 d PD C 2 H1WA H 1.167(5) -0.306(3) 0.246(3) 0.051 Uiso 0.56(4) 1 d PD . . H2WA H 1.128(7) -0.128(5) 0.254(3) 0.051 Uiso 0.56(4) 1 d PD . . H3WA H 0.982(5) -0.165(6) 0.237(2) 0.051 Uiso 0.56(4) 1 d PD . . H1WB H 1.097(9) -0.312(3) 0.267(3) 0.051 Uiso 0.44(4) 1 d PD . . H2WB H 1.160(7) -0.181(8) 0.270(3) 0.051 Uiso 0.44(4) 1 d PD . . H3WB H 0.961(3) -0.131(6) 0.267(3) 0.051 Uiso 0.44(4) 1 d PD . . Cl1 Cl 0.6379(3) 0.6940(2) 0.24914(9) 0.0458(5) Uani 0.65 1 d PU D 1 C11S C 0.7134(7) 0.5240(4) 0.2460(2) 0.0299(14) Uani 0.65 1 d PGU D 1 C12S C 0.6458(6) 0.4632(5) 0.2264(2) 0.0302(13) Uani 0.65 1 d PGU D 1 H12S H 0.5571 0.5156 0.2154 0.036 Uiso 0.65 1 calc PR D 1 C13S C 0.7109(7) 0.3241(5) 0.2232(2) 0.0343(15) Uani 0.65 1 d PGU D 1 H13S H 0.6657 0.2834 0.2101 0.041 Uiso 0.65 1 calc PR D 1 C14S C 0.8436(7) 0.2457(4) 0.2397(2) 0.0394(16) Uani 0.65 1 d PGU D 1 H14S H 0.8871 0.1526 0.2375 0.047 Uiso 0.65 1 calc PR D 1 C15S C 0.9112(6) 0.3065(6) 0.2593(2) 0.0367(15) Uani 0.65 1 d PGU D 1 H15S H 0.9999 0.2541 0.2703 0.044 Uiso 0.65 1 calc PR D 1 C16S C 0.8461(7) 0.4457(6) 0.2625(2) 0.0315(14) Uani 0.65 1 d PGU D 1 H16S H 0.8913 0.4864 0.2756 0.038 Uiso 0.65 1 calc PR D 1 N1S N 0.619(3) 0.7438(12) 0.2503(8) 0.0458(5) Uani 0.35 1 d PU E 2 C7S C 0.666(3) 0.6425(15) 0.2491(9) 0.0458(5) Uani 0.35 1 d PU E 2 C1S C 0.7377(16) 0.4964(8) 0.2474(5) 0.027(2) Uani 0.35 1 d PGU E 2 C2S C 0.6768(12) 0.4306(11) 0.2273(4) 0.026(2) Uani 0.35 1 d PGU E 2 H2S H 0.5922 0.4799 0.2143 0.032 Uiso 0.35 1 calc PR E 2 C3S C 0.7422(14) 0.2910(11) 0.2268(4) 0.034(3) Uani 0.35 1 d PGU E 2 H3S H 0.7014 0.2469 0.2134 0.041 Uiso 0.35 1 calc PR E 2 C4S C 0.8685(15) 0.2173(8) 0.2464(4) 0.038(3) Uani 0.35 1 d PGU E 2 H4S H 0.9123 0.1239 0.2460 0.045 Uiso 0.35 1 calc PR E 2 C5S C 0.9295(14) 0.2831(12) 0.2664(4) 0.038(3) Uani 0.35 1 d PGU E 2 H5S H 1.0141 0.2338 0.2795 0.046 Uiso 0.35 1 calc PR E 2 C6S C 0.8641(16) 0.4227(12) 0.2670(5) 0.036(3) Uani 0.35 1 d PGU E 2 H6S H 0.9049 0.4667 0.2804 0.043 Uiso 0.35 1 calc PR E 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 S11 0.0214(4) 0.0225(4) 0.0200(4) 0.0029(4) -0.0032(3) -0.0156(4) S12 0.0234(4) 0.0267(5) 0.0167(4) 0.0033(4) -0.0036(3) -0.0188(4) S13 0.0209(4) 0.0234(4) 0.0180(4) 0.0038(4) -0.0038(3) -0.0155(4) S14 0.0241(4) 0.0270(5) 0.0167(4) 0.0035(4) -0.0032(3) -0.0191(4) S15 0.0222(4) 0.0233(4) 0.0286(5) 0.0022(4) -0.0086(4) -0.0150(4) S16 0.0375(5) 0.0292(5) 0.0198(5) 0.0077(4) -0.0093(4) -0.0229(5) S17 0.0213(4) 0.0314(5) 0.0242(5) 0.0120(4) -0.0077(3) -0.0179(4) S18 0.0350(5) 0.0435(6) 0.0233(5) 0.0082(4) -0.0091(4) -0.0321(5) C11 0.0179(15) 0.0188(16) 0.0173(16) -0.0003(14) 0.0001(12) -0.0116(14) C12 0.0184(15) 0.0180(16) 0.0173(16) 0.0014(13) -0.0003(12) -0.0115(14) C13 0.0138(14) 0.0167(15) 0.0193(16) 0.0007(14) -0.0026(12) -0.0076(13) C14 0.0219(16) 0.0167(16) 0.0172(16) 0.0023(13) -0.0051(13) -0.0121(14) C15 0.0149(15) 0.0151(15) 0.0184(16) 0.0060(13) -0.0037(12) -0.0076(13) C16 0.0200(16) 0.0212(17) 0.0191(17) 0.0037(14) -0.0031(13) -0.0137(14) C17A 0.028(3) 0.020(3) 0.022(3) -0.006(2) 0.001(2) -0.013(3) C18A 0.029(4) 0.026(4) 0.028(4) 0.004(3) -0.006(3) -0.017(3) C17B 0.030(5) 0.028(5) 0.008(3) 0.000(3) -0.002(3) -0.020(4) C18B 0.017(4) 0.025(5) 0.014(4) -0.005(4) -0.001(3) -0.005(4) C19 0.0269(19) 0.032(2) 0.026(2) 0.0046(17) -0.0058(15) -0.0206(18) C20 0.040(2) 0.031(2) 0.0190(18) 0.0039(16) -0.0068(16) -0.0244(19) S21 0.0196(4) 0.0220(4) 0.0207(4) 0.0043(4) -0.0027(3) -0.0140(4) S22 0.0216(4) 0.0231(4) 0.0208(4) 0.0031(4) -0.0023(3) -0.0152(4) S23 0.0201(4) 0.0247(4) 0.0181(4) 0.0036(4) -0.0038(3) -0.0153(4) S24 0.0208(4) 0.0257(4) 0.0203(4) 0.0016(4) -0.0023(3) -0.0158(4) S25 0.0221(4) 0.0286(5) 0.0214(4) 0.0049(4) -0.0041(3) -0.0165(4) S26 0.0241(5) 0.0324(5) 0.0241(5) 0.0026(4) -0.0057(4) -0.0201(4) S27 0.0209(4) 0.0244(4) 0.0231(4) 0.0016(4) -0.0052(3) -0.0135(4) S28 0.0319(5) 0.0298(5) 0.0206(4) 0.0057(4) -0.0006(4) -0.0192(4) C21 0.0166(15) 0.0207(17) 0.0184(16) 0.0010(14) 0.0008(13) -0.0108(14) C22 0.0132(14) 0.0183(16) 0.0210(17) -0.0005(14) -0.0007(12) -0.0099(13) C23 0.0166(15) 0.0194(16) 0.0182(16) 0.0031(13) -0.0012(12) -0.0102(13) C24 0.0181(15) 0.0158(15) 0.0158(16) 0.0024(13) -0.0032(12) -0.0078(13) C25 0.0169(15) 0.0210(17) 0.0151(16) 0.0023(13) -0.0023(12) -0.0113(14) C26 0.0178(16) 0.0184(16) 0.0171(16) 0.0011(14) -0.0030(13) -0.0090(14) C27 0.031(2) 0.034(2) 0.0218(18) -0.0074(16) -0.0010(15) -0.0159(18) C28 0.0288(19) 0.035(2) 0.0205(18) 0.0059(16) -0.0059(15) -0.0141(17) C29 0.0207(17) 0.0218(17) 0.0223(18) 0.0020(15) -0.0069(14) -0.0108(14) C30 0.0273(19) 0.027(2) 0.0207(18) -0.0014(16) -0.0053(15) -0.0157(16) S31 0.0146(4) 0.0266(5) 0.0205(4) -0.0029(4) 0.0001(3) -0.0083(4) S32 0.0138(4) 0.0252(5) 0.0210(4) -0.0045(4) 0.0000(3) -0.0088(3) S33 0.0156(4) 0.0260(5) 0.0210(4) -0.0040(4) 0.0015(3) -0.0085(4) S34 0.0145(4) 0.0233(4) 0.0234(5) -0.0038(4) -0.0002(3) -0.0080(3) S35 0.0141(4) 0.0290(5) 0.0267(5) -0.0013(4) -0.0032(3) -0.0090(4) S36 0.0168(4) 0.0272(5) 0.0217(4) -0.0074(4) 0.0003(3) -0.0093(4) S37 0.0380(6) 0.0395(6) 0.0180(5) -0.0075(4) 0.0048(4) -0.0172(5) S38 0.0249(5) 0.0263(5) 0.0373(6) -0.0018(4) -0.0133(4) -0.0115(4) C31 0.0165(16) 0.0191(17) 0.0222(18) -0.0006(14) -0.0012(13) -0.0098(14) C32 0.0147(15) 0.0204(17) 0.0181(16) -0.0015(14) -0.0001(12) -0.0090(13) C33 0.0165(16) 0.0205(17) 0.0198(17) -0.0014(14) -0.0022(13) -0.0103(14) C34 0.0178(15) 0.0156(16) 0.0178(16) -0.0028(13) -0.0008(12) -0.0090(13) C35 0.0233(17) 0.0232(18) 0.0156(16) 0.0013(14) -0.0031(13) -0.0118(15) C36 0.0206(16) 0.0198(17) 0.0224(18) -0.0010(14) -0.0051(13) -0.0106(14) C37 0.0197(17) 0.027(2) 0.0222(18) -0.0027(16) -0.0056(14) -0.0104(15) C38 0.0220(17) 0.0253(19) 0.0240(19) -0.0004(16) -0.0046(14) -0.0135(15) C39 0.056(3) 0.052(3) 0.0196(19) -0.0055(19) 0.0029(19) -0.038(3) C40 0.060(3) 0.051(3) 0.031(2) 0.015(2) -0.021(2) -0.038(3) S41 0.0130(4) 0.0270(5) 0.0191(4) -0.0041(4) 0.0009(3) -0.0073(4) S42 0.0125(4) 0.0248(4) 0.0184(4) -0.0037(4) 0.0002(3) -0.0067(3) S43 0.0134(4) 0.0280(5) 0.0183(4) -0.0044(4) -0.0001(3) -0.0077(4) S44 0.0124(4) 0.0210(4) 0.0211(4) -0.0037(4) 0.0004(3) -0.0057(3) S45 0.0143(4) 0.0409(6) 0.0279(5) -0.0084(5) -0.0035(3) -0.0098(4) S46 0.0193(4) 0.0337(5) 0.0235(5) -0.0113(4) 0.0028(3) -0.0136(4) S47 0.0192(4) 0.0296(5) 0.0200(5) -0.0087(4) -0.0015(3) -0.0027(4) S48 0.0135(4) 0.0228(4) 0.0260(5) -0.0011(4) -0.0041(3) -0.0081(3) C41 0.0145(15) 0.0241(18) 0.0187(17) -0.0015(14) 0.0007(12) -0.0103(14) C42 0.0136(15) 0.0218(17) 0.0175(16) -0.0034(14) 0.0018(12) -0.0080(14) C43 0.0156(15) 0.0238(18) 0.0166(16) -0.0037(14) -0.0016(12) -0.0100(14) C44 0.0165(15) 0.0207(17) 0.0194(17) -0.0040(14) 0.0002(13) -0.0089(14) C45 0.0141(15) 0.0227(17) 0.0186(17) -0.0018(14) -0.0022(13) -0.0069(14) C46 0.0139(15) 0.0169(16) 0.0175(16) -0.0017(13) -0.0004(12) -0.0046(13) C47A 0.020(3) 0.033(4) 0.017(3) -0.001(3) -0.003(2) -0.011(3) C48A 0.017(2) 0.019(3) 0.022(3) -0.007(2) 0.002(2) -0.010(2) C47B 0.019(5) 0.027(6) 0.014(5) -0.006(4) -0.002(3) -0.007(4) C48B 0.022(4) 0.030(5) 0.022(5) 0.001(4) -0.004(4) -0.008(4) C49 0.027(2) 0.047(3) 0.0186(19) -0.0038(18) -0.0039(15) -0.017(2) C50 0.0253(19) 0.036(2) 0.026(2) 0.0020(18) -0.0037(16) -0.0100(18) Fe1 0.0224(3) 0.0273(2) 0.0189(2) -0.0015(2) -0.0004(2) -0.0095(2) O1 0.0284(14) 0.0423(17) 0.0219(14) 0.0009(13) -0.0054(11) -0.0206(14) O2 0.0263(14) 0.0375(16) 0.0209(13) 0.0025(12) -0.0057(11) -0.0134(13) O3 0.0265(13) 0.0298(14) 0.0230(13) -0.0026(11) -0.0001(10) -0.0147(12) O4 0.0269(14) 0.0349(16) 0.0215(14) -0.0057(12) -0.0008(11) -0.0120(12) O5 0.0257(14) 0.0314(15) 0.0259(14) -0.0031(12) 0.0025(11) -0.0077(12) O6 0.0311(15) 0.0311(15) 0.0231(14) -0.0016(12) 0.0016(11) -0.0126(12) O7 0.0355(16) 0.0395(17) 0.0342(17) 0.0015(14) -0.0036(13) -0.0235(15) O8 0.0472(19) 0.050(2) 0.0342(18) 0.0029(15) -0.0194(15) -0.0282(17) O9 0.0263(14) 0.0418(18) 0.0295(15) 0.0001(13) -0.0072(12) -0.0154(13) O10 0.0226(14) 0.0424(18) 0.0322(17) -0.0042(14) 0.0033(12) -0.0116(13) O11 0.0313(16) 0.0361(17) 0.0453(19) -0.0131(15) 0.0025(14) -0.0111(14) O12 0.0333(16) 0.0310(16) 0.0412(18) 0.0044(14) -0.0065(14) -0.0108(13) C1 0.0197(17) 0.033(2) 0.027(2) -0.0061(17) -0.0005(15) -0.0081(16) C2 0.0207(17) 0.030(2) 0.031(2) -0.0056(17) -0.0032(15) -0.0079(16) C3 0.0310(19) 0.030(2) 0.0190(17) 0.0013(15) -0.0038(14) -0.0206(17) C4 0.0281(18) 0.0287(19) 0.0153(16) -0.0012(14) 0.0020(13) -0.0151(16) C5 0.0238(18) 0.036(2) 0.0238(18) -0.0068(16) -0.0041(14) -0.0134(17) C6 0.0259(18) 0.032(2) 0.0232(18) -0.0022(16) -0.0068(14) -0.0113(16) Cl1 0.0563(15) 0.0324(9) 0.0418(8) -0.0028(18) -0.0203(10) -0.0123(15) C11S 0.030(3) 0.0320(17) 0.026(3) 0.002(3) -0.001(2) -0.013(2) C12S 0.030(3) 0.036(2) 0.026(3) 0.001(3) 0.005(2) -0.017(2) C13S 0.035(3) 0.037(3) 0.036(3) 0.001(3) 0.005(2) -0.021(2) C14S 0.043(3) 0.035(3) 0.040(4) 0.010(3) 0.001(3) -0.018(2) C15S 0.026(3) 0.040(2) 0.038(4) 0.007(3) 0.002(2) -0.011(2) C16S 0.026(3) 0.041(2) 0.027(3) 0.004(2) 0.005(2) -0.015(2) N1S 0.0563(15) 0.0324(9) 0.0418(8) -0.0028(18) -0.0203(10) -0.0123(15) C7S 0.0563(15) 0.0324(9) 0.0418(8) -0.0028(18) -0.0203(10) -0.0123(15) C1S 0.026(4) 0.0313(17) 0.021(4) 0.001(3) 0.007(3) -0.011(3) C2S 0.027(4) 0.030(3) 0.018(4) 0.002(3) 0.006(3) -0.010(3) C3S 0.035(4) 0.030(3) 0.033(5) 0.004(3) 0.005(3) -0.013(3) C4S 0.035(4) 0.031(4) 0.045(5) 0.013(3) 0.002(3) -0.015(3) C5S 0.033(4) 0.039(3) 0.035(5) 0.009(4) 0.001(3) -0.011(3) C6S 0.029(4) 0.040(3) 0.035(5) 0.003(4) -0.001(3) -0.014(3) _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 S11 C11 1.743(3) . ? S11 C13 1.745(4) . ? S12 C11 1.735(4) . ? S12 C14 1.752(4) . ? S13 C12 1.734(4) . ? S13 C15 1.752(4) . ? S14 C16 1.742(4) . ? S14 C12 1.745(3) . ? S15 C17B 1.728(8) . ? S15 C13 1.742(3) . ? S15 C17A 1.885(7) . ? S16 C14 1.739(4) . ? S16 C18A 1.764(7) . ? S16 C18B 1.878(10) . ? S17 C15 1.747(4) . ? S17 C19 1.796(4) . ? S18 C16 1.742(4) . ? S18 C20 1.805(4) . ? C11 C12 1.364(5) . ? C13 C14 1.355(5) . ? C15 C16 1.362(5) . ? C17A C18A 1.526(10) . ? C17A H17A 0.9700 . ? C17A H17B 0.9700 . ? C18A H18A 0.9700 . ? C18A H18B 0.9700 . ? C17B C18B 1.515(13) . ? C17B H17C 0.9700 . ? C17B H17D 0.9700 . ? C18B H18C 0.9700 . ? C18B H18D 0.9700 . ? C19 C20 1.519(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? S21 C23 1.740(4) . ? S21 C21 1.747(4) . ? S22 C21 1.735(4) . ? S22 C24 1.755(4) . ? S23 C22 1.740(4) . ? S23 C25 1.747(4) . ? S24 C22 1.749(3) . ? S24 C26 1.752(4) . ? S25 C25 1.750(4) . ? S25 C29 1.805(4) . ? S26 C26 1.747(4) . ? S26 C30 1.810(4) . ? S27 C23 1.747(4) . ? S27 C27 1.802(5) . ? S28 C24 1.742(4) . ? S28 C28 1.815(4) . ? C21 C22 1.353(5) . ? C23 C24 1.353(5) . ? C25 C26 1.354(5) . ? C27 C28 1.521(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.522(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? S31 C31 1.734(4) . ? S31 C33 1.759(4) . ? S32 C31 1.741(4) . ? S32 C34 1.754(4) . ? S33 C35 1.743(4) . ? S33 C32 1.748(4) . ? S34 C32 1.744(4) . ? S34 C36 1.752(4) . ? S35 C33 1.749(4) . ? S35 C37 1.822(4) . ? S36 C34 1.750(4) . ? S36 C38 1.809(4) . ? S37 C35 1.754(4) . ? S37 C39 1.801(5) . ? S38 C36 1.742(4) . ? S38 C40 1.806(6) . ? C31 C32 1.377(5) . ? C33 C34 1.355(5) . ? C35 C36 1.357(5) . ? C37 C38 1.509(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.536(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? S41 C41 1.741(4) . ? S41 C43 1.748(4) . ? S42 C41 1.736(4) . ? S42 C44 1.757(4) . ? S43 C42 1.749(4) . ? S43 C45 1.754(4) . ? S44 C42 1.738(4) . ? S44 C46 1.748(4) . ? S45 C47B 1.721(11) . ? S45 C43 1.742(4) . ? S45 C47A 1.858(8) . ? S46 C44 1.747(4) . ? S46 C48A 1.778(6) . ? S46 C48B 1.899(10) . ? S47 C45 1.743(4) . ? S47 C49 1.814(4) . ? S48 C46 1.742(4) . ? S48 C50 1.819(5) . ? C41 C42 1.375(5) . ? C43 C44 1.364(5) . ? C45 C46 1.370(5) . ? C47A C48A 1.519(10) . ? C47A H47A 0.9700 . ? C47A H47B 0.9700 . ? C48A H48A 0.9700 . ? C48A H48B 0.9700 . ? C47B C48B 1.517(16) . ? C47B H47C 0.9700 . ? C47B H47D 0.9700 . ? C48B H48C 0.9700 . ? C48B H48D 0.9700 . ? C49 C50 1.515(6) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? Fe1 O1 2.001(3) . ? Fe1 O6 2.011(3) . ? Fe1 O2 2.012(3) . ? Fe1 O3 2.012(3) . ? Fe1 O4 2.016(3) . ? Fe1 O5 2.027(3) . ? O1 C1 1.283(5) . ? O2 C2 1.276(5) . ? O3 C3 1.285(5) . ? O4 C4 1.283(5) . ? O5 C5 1.286(5) . ? O6 C6 1.284(5) . ? O7 C1 1.223(6) . ? O8 C2 1.239(5) . ? O9 C3 1.215(5) . ? O10 C4 1.221(5) . ? O11 C5 1.225(5) . ? O12 C6 1.230(5) . ? C1 C2 1.556(6) . ? C3 C4 1.576(6) . ? C5 C6 1.564(6) . ? O1WA H1WA 1.099(10) . ? O1WA H2WA 1.101(10) . ? O1WA H3WA 1.104(10) . ? O1WA H1WB 1.29(3) . ? O1WA H2WB 1.13(4) . ? O1WA H3WB 1.24(4) . ? O1WB H1WA 1.19(4) . ? O1WB H2WA 1.25(3) . ? O1WB H3WA 1.24(3) . ? O1WB H1WB 1.099(10) . ? O1WB H2WB 1.102(10) . ? O1WB H3WB 1.101(10) . ? Cl1 C11S 1.698(5) . ? C11S C12S 1.3900 . ? C11S C16S 1.3900 . ? C12S C13S 1.3900 . ? C12S H12S 0.9300 . ? C13S C14S 1.3900 . ? C13S H13S 0.9300 . ? C14S C15S 1.3900 . ? C14S H14S 0.9300 . ? C15S C16S 1.3900 . ? C15S H15S 0.9300 . ? C16S H16S 0.9300 . ? N1S C7S 1.010(19) . ? C7S C1S 1.455(17) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C2S H2S 0.9300 . ? C3S C4S 1.3900 . ? C3S H3S 0.9300 . ? C4S C5S 1.3900 . ? C4S H4S 0.9300 . ? C5S C6S 1.3900 . ? C5S H5S 0.9300 . ? C6S H6S 0.9300 . ? 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 C11 S11 C13 94.97(17) . . ? C11 S12 C14 95.06(17) . . ? C12 S13 C15 95.51(17) . . ? C16 S14 C12 95.36(17) . . ? C17B S15 C13 108.0(3) . . ? C13 S15 C17A 95.7(2) . . ? C14 S16 C18A 106.6(3) . . ? C14 S16 C18B 95.1(4) . . ? C15 S17 C19 101.76(18) . . ? C16 S18 C20 101.21(18) . . ? C12 C11 S12 121.5(3) . . ? C12 C11 S11 122.9(3) . . ? S12 C11 S11 115.5(2) . . ? C11 C12 S13 122.3(3) . . ? C11 C12 S14 122.4(3) . . ? S13 C12 S14 115.4(2) . . ? C14 C13 S15 126.5(3) . . ? C14 C13 S11 117.2(3) . . ? S15 C13 S11 116.3(2) . . ? C13 C14 S16 126.4(3) . . ? C13 C14 S12 116.8(3) . . ? S16 C14 S12 116.6(2) . . ? C16 C15 S17 127.8(3) . . ? C16 C15 S13 116.6(3) . . ? S17 C15 S13 115.59(19) . . ? C15 C16 S18 128.4(3) . . ? C15 C16 S14 117.1(3) . . ? S18 C16 S14 114.5(2) . . ? C18A C17A S15 110.3(5) . . ? C18A C17A H17A 109.6 . . ? S15 C17A H17A 109.6 . . ? C18A C17A H17B 109.6 . . ? S15 C17A H17B 109.6 . . ? H17A C17A H17B 108.1 . . ? C17A C18A S16 116.3(6) . . ? C17A C18A H18A 108.2 . . ? S16 C18A H18A 108.2 . . ? C17A C18A H18B 108.2 . . ? S16 C18A H18B 108.2 . . ? H18A C18A H18B 107.4 . . ? C18B C17B S15 113.7(7) . . ? C18B C17B H17C 108.8 . . ? S15 C17B H17C 108.8 . . ? C18B C17B H17D 108.8 . . ? S15 C17B H17D 108.8 . . ? H17C C17B H17D 107.7 . . ? C17B C18B S16 113.1(7) . . ? C17B C18B H18C 109.0 . . ? S16 C18B H18C 109.0 . . ? C17B C18B H18D 109.0 . . ? S16 C18B H18D 109.0 . . ? H18C C18B H18D 107.8 . . ? C20 C19 S17 114.2(3) . . ? C20 C19 H19A 108.7 . . ? S17 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? S17 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C19 C20 S18 112.3(3) . . ? C19 C20 H20A 109.1 . . ? S18 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? S18 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? C23 S21 C21 95.35(17) . . ? C21 S22 C24 95.36(17) . . ? C22 S23 C25 95.57(17) . . ? C22 S24 C26 95.46(17) . . ? C25 S25 C29 100.91(17) . . ? C26 S26 C30 102.13(18) . . ? C23 S27 C27 98.93(18) . . ? C24 S28 C28 102.81(18) . . ? C22 C21 S22 123.2(3) . . ? C22 C21 S21 121.5(3) . . ? S22 C21 S21 115.2(2) . . ? C21 C22 S23 121.6(3) . . ? C21 C22 S24 123.5(3) . . ? S23 C22 S24 115.0(2) . . ? C24 C23 S21 117.3(3) . . ? C24 C23 S27 126.9(3) . . ? S21 C23 S27 115.7(2) . . ? C23 C24 S28 129.3(3) . . ? C23 C24 S22 116.7(3) . . ? S28 C24 S22 113.84(19) . . ? C26 C25 S23 117.2(3) . . ? C26 C25 S25 127.4(3) . . ? S23 C25 S25 115.34(19) . . ? C25 C26 S26 129.6(3) . . ? C25 C26 S24 116.7(3) . . ? S26 C26 S24 113.7(2) . . ? C28 C27 S27 112.2(3) . . ? C28 C27 H27A 109.2 . . ? S27 C27 H27A 109.2 . . ? C28 C27 H27B 109.2 . . ? S27 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C27 C28 S28 114.3(3) . . ? C27 C28 H28A 108.7 . . ? S28 C28 H28A 108.7 . . ? C27 C28 H28B 108.7 . . ? S28 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C30 C29 S25 114.4(3) . . ? C30 C29 H29A 108.7 . . ? S25 C29 H29A 108.7 . . ? C30 C29 H29B 108.7 . . ? S25 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C29 C30 S26 113.7(3) . . ? C29 C30 H30A 108.8 . . ? S26 C30 H30A 108.8 . . ? C29 C30 H30B 108.8 . . ? S26 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C31 S31 C33 94.69(17) . . ? C31 S32 C34 95.29(17) . . ? C35 S33 C32 95.41(18) . . ? C32 S34 C36 95.35(18) . . ? C33 S35 C37 101.42(18) . . ? C34 S36 C38 101.34(18) . . ? C35 S37 C39 102.6(2) . . ? C36 S38 C40 99.0(2) . . ? C32 C31 S31 122.7(3) . . ? C32 C31 S32 121.2(3) . . ? S31 C31 S32 116.1(2) . . ? C31 C32 S34 122.3(3) . . ? C31 C32 S33 122.5(3) . . ? S34 C32 S33 115.1(2) . . ? C34 C33 S35 128.9(3) . . ? C34 C33 S31 117.6(3) . . ? S35 C33 S31 113.5(2) . . ? C33 C34 S36 128.4(3) . . ? C33 C34 S32 116.3(3) . . ? S36 C34 S32 115.3(2) . . ? C36 C35 S33 117.2(3) . . ? C36 C35 S37 128.8(3) . . ? S33 C35 S37 113.9(2) . . ? C35 C36 S38 127.7(3) . . ? C35 C36 S34 116.9(3) . . ? S38 C36 S34 115.4(2) . . ? C38 C37 S35 114.2(3) . . ? C38 C37 H37A 108.7 . . ? S35 C37 H37A 108.7 . . ? C38 C37 H37B 108.7 . . ? S35 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? C37 C38 S36 114.6(3) . . ? C37 C38 H38A 108.6 . . ? S36 C38 H38A 108.6 . . ? C37 C38 H38B 108.6 . . ? S36 C38 H38B 108.6 . . ? H38A C38 H38B 107.6 . . ? C40 C39 S37 113.1(3) . . ? C40 C39 H39A 109.0 . . ? S37 C39 H39A 109.0 . . ? C40 C39 H39B 109.0 . . ? S37 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C39 C40 S38 112.6(3) . . ? C39 C40 H40A 109.1 . . ? S38 C40 H40A 109.1 . . ? C39 C40 H40B 109.1 . . ? S38 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? C41 S41 C43 94.76(17) . . ? C41 S42 C44 95.50(17) . . ? C42 S43 C45 95.59(17) . . ? C42 S44 C46 95.12(17) . . ? C47B S45 C43 105.7(4) . . ? C43 S45 C47A 99.3(3) . . ? C44 S46 C48A 103.8(2) . . ? C44 S46 C48B 95.5(3) . . ? C45 S47 C49 104.50(19) . . ? C46 S48 C50 97.15(19) . . ? C42 C41 S42 122.5(3) . . ? C42 C41 S41 121.6(3) . . ? S42 C41 S41 116.0(2) . . ? C41 C42 S44 122.9(3) . . ? C41 C42 S43 121.7(3) . . ? S44 C42 S43 115.4(2) . . ? C44 C43 S45 127.9(3) . . ? C44 C43 S41 117.9(3) . . ? S45 C43 S41 114.2(2) . . ? C43 C44 S46 128.4(3) . . ? C43 C44 S42 115.8(3) . . ? S46 C44 S42 115.8(2) . . ? C46 C45 S47 128.5(3) . . ? C46 C45 S43 115.8(3) . . ? S47 C45 S43 115.5(2) . . ? C45 C46 S48 124.7(3) . . ? C45 C46 S44 117.7(3) . . ? S48 C46 S44 117.4(2) . . ? C48A C47A S45 113.2(5) . . ? C48A C47A H47A 108.9 . . ? S45 C47A H47A 108.9 . . ? C48A C47A H47B 108.9 . . ? S45 C47A H47B 108.9 . . ? H47A C47A H47B 107.7 . . ? C47A C48A S46 111.9(5) . . ? C47A C48A H48A 109.2 . . ? S46 C48A H48A 109.2 . . ? C47A C48A H48B 109.2 . . ? S46 C48A H48B 109.2 . . ? H48A C48A H48B 107.9 . . ? C48B C47B S45 112.3(8) . . ? C48B C47B H47C 109.1 . . ? S45 C47B H47C 109.1 . . ? C48B C47B H47D 109.1 . . ? S45 C47B H47D 109.1 . . ? H47C C47B H47D 107.9 . . ? C47B C48B S46 113.0(8) . . ? C47B C48B H48C 109.0 . . ? S46 C48B H48C 109.0 . . ? C47B C48B H48D 109.0 . . ? S46 C48B H48D 109.0 . . ? H48C C48B H48D 107.8 . . ? C50 C49 S47 115.9(3) . . ? C50 C49 H49A 108.3 . . ? S47 C49 H49A 108.3 . . ? C50 C49 H49B 108.3 . . ? S47 C49 H49B 108.3 . . ? H49A C49 H49B 107.4 . . ? C49 C50 S48 112.9(3) . . ? C49 C50 H50A 109.0 . . ? S48 C50 H50A 109.0 . . ? C49 C50 H50B 109.0 . . ? S48 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? O1 Fe1 O6 169.23(13) . . ? O1 Fe1 O2 80.82(12) . . ? O6 Fe1 O2 95.65(13) . . ? O1 Fe1 O3 86.73(12) . . ? O6 Fe1 O3 98.92(12) . . ? O2 Fe1 O3 161.59(11) . . ? O1 Fe1 O4 100.44(11) . . ? O6 Fe1 O4 89.56(13) . . ? O2 Fe1 O4 88.14(12) . . ? O3 Fe1 O4 80.81(12) . . ? O1 Fe1 O5 90.06(13) . . ? O6 Fe1 O5 80.39(12) . . ? O2 Fe1 O5 98.88(12) . . ? O3 Fe1 O5 94.61(12) . . ? O4 Fe1 O5 168.22(13) . . ? C1 O1 Fe1 115.9(3) . . ? C2 O2 Fe1 114.9(3) . . ? C3 O3 Fe1 114.8(2) . . ? C4 O4 Fe1 116.0(3) . . ? C5 O5 Fe1 115.9(3) . . ? C6 O6 Fe1 115.6(3) . . ? O7 C1 O1 126.2(4) . . ? O7 C1 C2 120.5(4) . . ? O1 C1 C2 113.3(4) . . ? O8 C2 O2 126.3(4) . . ? O8 C2 C1 118.8(4) . . ? O2 C2 C1 114.9(4) . . ? O9 C3 O3 126.8(4) . . ? O9 C3 C4 119.0(4) . . ? O3 C3 C4 114.3(3) . . ? O10 C4 O4 126.5(4) . . ? O10 C4 C3 120.5(4) . . ? O4 C4 C3 113.0(3) . . ? O11 C5 O5 126.2(4) . . ? O11 C5 C6 120.6(4) . . ? O5 C5 C6 113.2(4) . . ? O12 C6 O6 126.4(4) . . ? O12 C6 C5 119.2(4) . . ? O6 C6 C5 114.4(4) . . ? H1WA O1WA H2WA 116(2) . . ? H1WA O1WA H3WA 116(2) . . ? H2WA O1WA H3WA 115(2) . . ? H2WA O1WA H1WB 141(5) . . ? H3WA O1WA H1WB 102(5) . . ? H1WA O1WA H2WB 93(5) . . ? H3WA O1WA H2WB 150(5) . . ? H1WB O1WA H2WB 100(4) . . ? H1WA O1WA H3WB 144(5) . . ? H2WA O1WA H3WB 97(6) . . ? H1WB O1WA H3WB 95(3) . . ? H2WB O1WA H3WB 104(4) . . ? H1WA O1WB H2WA 100(4) . . ? H1WA O1WB H3WA 100(3) . . ? H2WA O1WB H3WA 97(3) . . ? H2WA O1WB H1WB 147(5) . . ? H3WA O1WB H1WB 106(6) . . ? H1WA O1WB H2WB 90(6) . . ? H3WA O1WB H2WB 134(6) . . ? H1WB O1WB H2WB 116(2) . . ? H1WA O1WB H3WB 152(5) . . ? H2WA O1WB H3WB 96(5) . . ? H3WA O1WB H3WB 55(7) . . ? H1WB O1WB H3WB 116(2) . . ? H2WB O1WB H3WB 116(2) . . ? C12S C11S C16S 120.0 . . ? C12S C11S Cl1 120.7(4) . . ? C16S C11S Cl1 119.3(4) . . ? C11S C12S C13S 120.0 . . ? C11S C12S H12S 120.0 . . ? C13S C12S H12S 120.0 . . ? C14S C13S C12S 120.0 . . ? C14S C13S H13S 120.0 . . ? C12S C13S H13S 120.0 . . ? C15S C14S C13S 120.0 . . ? C15S C14S H14S 120.0 . . ? C13S C14S H14S 120.0 . . ? C14S C15S C16S 120.0 . . ? C14S C15S H15S 120.0 . . ? C16S C15S H15S 120.0 . . ? C15S C16S C11S 120.0 . . ? C15S C16S H16S 120.0 . . ? C11S C16S H16S 120.0 . . ? N1S C7S C1S 178(3) . . ? C2S C1S C6S 120.0 . . ? C2S C1S C7S 119.9(12) . . ? C6S C1S C7S 120.1(12) . . ? C3S C2S C1S 120.0 . . ? C3S C2S H2S 120.0 . . ? C1S C2S H2S 120.0 . . ? C4S C3S C2S 120.0 . . ? C4S C3S H3S 120.0 . . ? C2S C3S H3S 120.0 . . ? C5S C4S C3S 120.0 . . ? C5S C4S H4S 120.0 . . ? C3S C4S H4S 120.0 . . ? C4S C5S C6S 120.0 . . ? C4S C5S H5S 120.0 . . ? C6S C5S H5S 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6S 120.0 . . ? C1S C6S H6S 120.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C17A H17B O4 0.97 2.35 3.285(7) 160.5 2 C17B H17C O4 0.97 2.48 3.436(9) 169.9 2 C18B H18D O8 0.97 2.51 3.009(10) 111.5 2 C19 H19A O10 0.97 2.49 3.257(5) 136.2 1_455 C20 H20A O8 0.97 2.48 3.204(5) 131.1 . C27 H27B O12 0.97 2.40 3.249(5) 145.5 2_565 C29 H29A O6 0.97 2.60 3.339(5) 133.0 . C40 H40B O11 0.97 2.58 3.451(6) 149.8 2_666 C47A H47A O9 0.97 2.40 3.207(9) 140.8 . C48A H48A O7 0.97 2.37 3.164(7) 138.4 1_655 C47B H47D O9 0.97 2.40 3.071(11) 125.5 . C48B H48D O7 0.97 2.49 3.237(11) 133.9 1_655 C50 H50B O1 0.97 2.42 3.345(5) 159.1 2_756 C12S H12S O12 0.93 2.57 3.302(7) 136.2 . _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.201 _refine_diff_density_min -1.021 _refine_diff_density_rms 0.121