# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2007 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Peter Day' _publ_contact_author_address ; Davy-Faraday Research Laboratory The Royal Institution of Great Britain 21 Albemarle Street London W1X 4BS UNITED KINGDOM ; _publ_contact_author_email PDAY@RI.AC.UK _publ_section_title ; Multi-layered molecular charge-transfer salts containing alkali metal ions ; loop_ _publ_author_name 'Peter Day' 'Ann L. Bingham' 'William Clegg' 'Steven Firth' 'Ross W. Harrington' 'Peter Horton' ; M.B.Hursthouse ; 'Lee Martin' 'Paul McMillan' data_I _database_code_depnum_ccdc_archive 'CCDC 637271' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Dr. S. G. Carling/Dr. L. Martin' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C138 H120 Fe8 Na18 O120 S72' _chemical_formula_weight 6867.28 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' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6196(18) _cell_length_b 17.378(2) _cell_length_c 26.551(4) _cell_angle_alpha 90.019(10) _cell_angle_beta 98.764(11) _cell_angle_gamma 92.938(10) _cell_volume 5747.0(14) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 20242 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Sheet _exptl_crystal_colour Brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3466 _exptl_absorpt_coefficient_mu 1.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8016 _exptl_absorpt_correction_T_max 0.9873 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104059 _diffrn_reflns_av_R_equivalents 0.1272 _diffrn_reflns_av_sigmaI/netI 0.1653 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.48 _reflns_number_total 25387 _reflns_number_gt 13019 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' DENZO (Otwinowski and Minor, 1997)' _computing_cell_refinement ' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_data_reduction ' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+39.8012P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25387 _refine_ls_number_parameters 1621 _refine_ls_number_restraints 613 _refine_ls_R_factor_all 0.2117 _refine_ls_R_factor_gt 0.1026 _refine_ls_wR_factor_ref 0.2079 _refine_ls_wR_factor_gt 0.1685 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _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 C1 C 0.1096(7) 0.6391(5) 0.7873(3) 0.029(2) Uani 1 1 d U . . H1A H 0.0709 0.6715 0.7606 0.034 Uiso 1 1 calc R . . H1B H 0.1874 0.6513 0.7885 0.034 Uiso 1 1 calc R . . C2 C 0.0855(7) 0.5551(5) 0.7722(3) 0.0236(19) Uani 1 1 d U . . H2A H 0.0965 0.5485 0.7363 0.028 Uiso 1 1 calc R . . H2B H 0.0090 0.5418 0.7739 0.028 Uiso 1 1 calc R . . C3 C 0.1538(7) 0.5191(5) 0.8715(3) 0.0243(19) Uani 1 1 d U . . C4 C 0.1171(7) 0.5864(5) 0.8860(3) 0.0241(19) Uani 1 1 d U . . C5 C 0.1609(7) 0.5133(5) 0.9705(3) 0.025(2) Uani 1 1 d U . . C6 C 0.1711(8) 0.4901(5) 1.0190(3) 0.029(2) Uani 1 1 d U . . C7 C 0.1707(7) 0.4827(5) 1.1162(3) 0.026(2) Uani 1 1 d U . . C8 C 0.2094(7) 0.4160(5) 1.1029(3) 0.0255(19) Uani 1 1 d U . . C9 C 0.2196(8) 0.3682(6) 1.2036(3) 0.032(2) Uani 1 1 d U . . H9A H 0.1431 0.3538 1.2048 0.039 Uiso 1 1 calc R . . H9B H 0.2630 0.3392 1.2307 0.039 Uiso 1 1 calc R . . C10 C 0.2389(8) 0.4519(6) 1.2150(3) 0.033(2) Uani 1 1 d U . . H10A H 0.3139 0.4669 1.2111 0.040 Uiso 1 1 calc R . . H10B H 0.2315 0.4607 1.2511 0.040 Uiso 1 1 calc R . . S1 S 0.0720(2) 0.66441(14) 0.84874(8) 0.0289(6) Uani 1 1 d U . . S2 S 0.1665(2) 0.48833(14) 0.81116(8) 0.0306(6) Uani 1 1 d U . . S3 S 0.19566(19) 0.45622(14) 0.92160(8) 0.0268(5) Uani 1 1 d U . . S4 S 0.1113(2) 0.60074(14) 0.95034(8) 0.0307(6) Uani 1 1 d U . . S5 S 0.1375(2) 0.54779(14) 1.06671(8) 0.0288(6) Uani 1 1 d U . . S6 S 0.2238(2) 0.40280(14) 1.03989(8) 0.0300(6) Uani 1 1 d U . . S7 S 0.2517(2) 0.33883(15) 1.14244(9) 0.0339(6) Uani 1 1 d U . . S8 S 0.1522(2) 0.51369(14) 1.17641(9) 0.0323(6) Uani 1 1 d U . . C11 C 0.2351(7) 0.3000(5) 0.7880(3) 0.027(2) Uani 1 1 d U . . H11A H 0.1591 0.3088 0.7904 0.032 Uiso 1 1 calc R . . H11B H 0.2560 0.3325 0.7602 0.032 Uiso 1 1 calc R . . C12 C 0.2441(7) 0.2166(5) 0.7744(3) 0.025(2) Uani 1 1 d U . . H12A H 0.3209 0.2064 0.7757 0.030 Uiso 1 1 calc R . . H12B H 0.2083 0.2074 0.7389 0.030 Uiso 1 1 calc R . . C13 C 0.2462(7) 0.1834(5) 0.8749(3) 0.0245(19) Uani 1 1 d U . . C14 C 0.2977(7) 0.2525(5) 0.8868(3) 0.0216(18) Uani 1 1 d U . . C15 C 0.3102(7) 0.1797(5) 0.9718(3) 0.0236(19) Uani 1 1 d U . . C16 C 0.3264(7) 0.1592(5) 1.0214(3) 0.027(2) Uani 1 1 d U . . C17 C 0.3735(7) 0.1553(5) 1.1190(3) 0.0249(19) Uani 1 1 d U . . C18 C 0.3219(7) 0.0872(5) 1.1057(3) 0.0253(19) Uani 1 1 d U . . C19 C 0.3608(8) 0.0421(6) 1.2058(3) 0.032(2) Uani 1 1 d U . . H19A H 0.3344 0.0102 1.2327 0.038 Uiso 1 1 calc R . . H19B H 0.4382 0.0339 1.2072 0.038 Uiso 1 1 calc R . . C20 C 0.3466(7) 0.1258(5) 1.2166(3) 0.026(2) Uani 1 1 d U . . H20A H 0.3701 0.1363 1.2534 0.031 Uiso 1 1 calc R . . H20B H 0.2694 0.1360 1.2088 0.031 Uiso 1 1 calc R . . S11 S 0.31736(19) 0.33035(14) 0.84743(8) 0.0281(6) Uani 1 1 d U . . S12 S 0.18610(19) 0.14938(13) 0.81532(8) 0.0264(5) Uani 1 1 d U . . S13 S 0.24204(19) 0.11831(14) 0.92474(8) 0.0275(5) Uani 1 1 d U . . S14 S 0.3555(2) 0.26746(14) 0.95021(8) 0.0301(6) Uani 1 1 d U . . S15 S 0.3952(2) 0.21694(14) 1.06946(8) 0.0295(6) Uani 1 1 d U . . S16 S 0.2794(2) 0.06951(14) 1.04139(8) 0.0296(6) Uani 1 1 d U . . S17 S 0.2901(2) 0.01101(15) 1.14458(8) 0.0307(6) Uani 1 1 d U . . S18 S 0.42124(19) 0.19093(15) 1.18016(8) 0.0304(6) Uani 1 1 d U . . C21 C 0.9127(8) 0.3027(5) 0.7940(3) 0.029(2) Uani 1 1 d U . . H21A H 0.8374 0.3149 0.7953 0.035 Uiso 1 1 calc R . . H21B H 0.9383 0.3343 0.7668 0.035 Uiso 1 1 calc R . . C22 C 0.9158(7) 0.2195(6) 0.7805(3) 0.030(2) Uani 1 1 d U . . H22A H 0.9918 0.2061 0.7834 0.036 Uiso 1 1 calc R . . H22B H 0.8828 0.2118 0.7445 0.036 Uiso 1 1 calc R . . C23 C 0.9110(8) 0.1839(5) 0.8799(3) 0.029(2) Uani 1 1 d U . . C24 C 0.9662(7) 0.2505(5) 0.8918(3) 0.0248(19) Uani 1 1 d U . . C25 C 0.9725(7) 0.1756(5) 0.9762(3) 0.026(2) Uani 1 1 d U . . C26 C 0.9866(7) 0.1522(5) 1.0252(3) 0.0217(18) Uani 1 1 d U . . C27 C 1.0264(6) 0.1499(5) 1.1233(3) 0.0208(18) Uani 1 1 d U . . C28 C 0.9740(7) 0.0810(5) 1.1088(3) 0.0230(19) Uani 1 1 d U . . C29 C 1.0335(7) 0.0260(5) 1.2041(3) 0.0227(19) Uani 1 1 d U . . H29A H 1.0192 -0.0112 1.2308 0.027 Uiso 1 1 calc R . . H29B H 1.1066 0.0181 1.1964 0.027 Uiso 1 1 calc R . . C30 C 1.0298(7) 0.1065(5) 1.2242(3) 0.0227(19) Uani 1 1 d U . . H30A H 1.0754 0.1104 1.2580 0.027 Uiso 1 1 calc R . . H30B H 0.9552 0.1147 1.2294 0.027 Uiso 1 1 calc R . . S21 S 0.9934(2) 0.32896(14) 0.85429(8) 0.0300(6) Uani 1 1 d U . . S22 S 0.8482(2) 0.15400(14) 0.81934(8) 0.0301(6) Uani 1 1 d U . . S23 S 0.9039(2) 0.11661(14) 0.92776(8) 0.0279(5) Uani 1 1 d U . . S24 S 1.0248(2) 0.26233(14) 0.95618(8) 0.0301(6) Uani 1 1 d U . . S25 S 1.05794(19) 0.20852(14) 1.07443(8) 0.0282(6) Uani 1 1 d U . . S26 S 0.93910(19) 0.06309(14) 1.04386(8) 0.0273(5) Uani 1 1 d U . . S27 S 0.9381(2) 0.00633(14) 1.14763(8) 0.0293(6) Uani 1 1 d U . . S28 S 1.07226(18) 0.18365(13) 1.18490(8) 0.0238(5) Uani 1 1 d U . . C31 C 0.4214(7) 0.7796(5) 0.2225(3) 0.0222(19) Uani 1 1 d U . . H31A H 0.4608 0.7857 0.2576 0.027 Uiso 1 1 calc R . . H31B H 0.3454 0.7903 0.2233 0.027 Uiso 1 1 calc R . . C32 C 0.4276(7) 0.6975(5) 0.2048(3) 0.026(2) Uani 1 1 d U . . H32A H 0.4109 0.6622 0.2321 0.031 Uiso 1 1 calc R . . H32B H 0.5020 0.6894 0.1993 0.031 Uiso 1 1 calc R . . C33 C 0.3619(7) 0.7499(5) 0.1075(3) 0.0256(19) Uani 1 1 d U . . C34 C 0.4170(7) 0.8185(5) 0.1210(3) 0.0239(19) Uani 1 1 d U . . C35 C 0.3565(7) 0.8248(5) 0.0239(3) 0.0240(19) Uani 1 1 d U . . C36 C 0.3413(7) 0.8468(5) -0.0266(3) 0.025(2) Uani 1 1 d U . . C37 C 0.3543(7) 0.9186(5) -0.1102(3) 0.0225(19) Uani 1 1 d U . . C38 C 0.2967(7) 0.8518(5) -0.1239(3) 0.0239(19) Uani 1 1 d U . . C39 C 0.3112(7) 0.8881(5) -0.2243(3) 0.0243(19) Uani 1 1 d U . . H39A H 0.3873 0.8757 -0.2225 0.029 Uiso 1 1 calc R . . H39B H 0.2767 0.8823 -0.2602 0.029 Uiso 1 1 calc R . . C40 C 0.3061(7) 0.9706(5) -0.2078(3) 0.025(2) Uani 1 1 d U . . H40A H 0.2311 0.9807 -0.2042 0.030 Uiso 1 1 calc R . . H40B H 0.3277 1.0051 -0.2345 0.030 Uiso 1 1 calc R . . S31 S 0.4779(2) 0.84926(14) 0.18128(8) 0.0290(6) Uani 1 1 d U . . S32 S 0.33707(19) 0.67265(14) 0.14658(8) 0.0275(5) Uani 1 1 d U . . S33 S 0.30710(19) 0.73716(13) 0.04401(8) 0.0268(5) Uani 1 1 d U . . S34 S 0.4274(2) 0.88307(14) 0.07173(8) 0.0280(6) Uani 1 1 d U . . S35 S 0.39405(19) 0.93494(13) -0.04498(8) 0.0257(5) Uani 1 1 d U . . S36 S 0.26876(19) 0.79136(13) -0.07465(8) 0.0260(5) Uani 1 1 d U . . S37 S 0.24569(19) 0.81930(13) -0.18556(8) 0.0254(5) Uani 1 1 d U . . S38 S 0.3915(2) 0.99313(14) -0.14835(8) 0.0277(6) Uani 1 1 d U . . C41 C 0.5715(13) 0.4437(8) 0.2205(5) 0.020(3) Uani 0.50 1 d PDU . . H41A H 0.6495 0.4530 0.2205 0.025 Uiso 0.50 1 calc PR . . H41B H 0.5579 0.4503 0.2560 0.025 Uiso 0.50 1 calc PR . . C42 C 0.5407(16) 0.3630(9) 0.2041(6) 0.019(4) Uani 0.50 1 d PDU . . H42A H 0.4615 0.3563 0.1967 0.023 Uiso 0.50 1 calc PR . . H42B H 0.5661 0.3278 0.2322 0.023 Uiso 0.50 1 calc PR . . C43 C 0.5535(7) 0.4137(5) 0.1079(3) 0.0208(18) Uani 1 1 d U . . C44 C 0.5177(7) 0.4815(5) 0.1218(3) 0.0198(18) Uani 1 1 d U . . C45 C 0.5069(7) 0.4883(5) 0.0249(3) 0.0228(19) Uani 1 1 d U . . S41 S 0.5052(2) 0.51165(14) 0.18345(8) 0.0293(6) Uani 1 1 d U . . S42 S 0.5999(2) 0.33674(14) 0.14554(8) 0.0285(6) Uani 1 1 d U . . S43 S 0.5572(2) 0.40004(14) 0.04328(8) 0.0285(6) Uani 1 1 d U . . S44 S 0.47481(19) 0.54499(14) 0.07332(8) 0.0268(5) Uani 1 1 d U . . C46 C 0.5090(15) 0.4123(13) 0.2152(8) 0.034(5) Uani 0.50 1 d PDU . . H46A H 0.5078 0.4196 0.2521 0.041 Uiso 0.50 1 calc PR . . H46B H 0.4427 0.3818 0.2010 0.041 Uiso 0.50 1 calc PR . . C47 C 0.6022(12) 0.3670(11) 0.2090(7) 0.025(4) Uani 0.50 1 d PDU . . H47A H 0.6027 0.3212 0.2312 0.030 Uiso 0.50 1 calc PR . . H47B H 0.6691 0.3987 0.2202 0.030 Uiso 0.50 1 calc PR . . C51 C 0.3982(7) 0.4974(5) 0.3436(3) 0.0211(18) Uani 1 1 d U . . C52 C 0.3755(7) 0.5379(5) 0.3923(3) 0.0235(19) Uani 1 1 d U . . C55 C 0.2173(7) 0.2839(5) 0.3843(3) 0.0204(18) Uani 1 1 d U . . C56 C 0.1604(7) 0.2881(5) 0.3280(3) 0.0217(19) Uani 1 1 d U . . C59 C 0.0380(7) 0.5497(5) 0.3327(3) 0.0212(19) Uani 1 1 d U . . C60 C 0.0107(7) 0.5112(5) 0.3827(3) 0.023(2) Uani 1 1 d U . . O51 O 0.3237(4) 0.4470(3) 0.3266(2) 0.0233(13) Uani 1 1 d U . . O52 O 0.2868(4) 0.5195(3) 0.4071(2) 0.0207(13) Uani 1 1 d U . . O53 O 0.4450(5) 0.5839(3) 0.4152(2) 0.0241(13) Uani 1 1 d U . . O54 O 0.4803(5) 0.5128(3) 0.3265(2) 0.0256(14) Uani 1 1 d U . . O55 O 0.2412(4) 0.3513(3) 0.4057(2) 0.0207(13) Uani 1 1 d U . . O56 O 0.1339(5) 0.3551(3) 0.3131(2) 0.0214(13) Uani 1 1 d U . . O57 O 0.1443(5) 0.2294(3) 0.3030(2) 0.0269(14) Uani 1 1 d U . . O58 O 0.2353(5) 0.2219(3) 0.4033(2) 0.0239(14) Uani 1 1 d U . . O59 O 0.1178(5) 0.5189(3) 0.3158(2) 0.0246(14) Uani 1 1 d U . . O60 O 0.0723(4) 0.4584(3) 0.4000(2) 0.0226(13) Uani 1 1 d U . . O61 O -0.0650(5) 0.5316(4) 0.4017(2) 0.0278(15) Uani 1 1 d U . . O62 O -0.0139(5) 0.6017(4) 0.3143(2) 0.0321(16) Uani 1 1 d U . . Fe1 Fe 0.19254(10) 0.44099(7) 0.36015(4) 0.0210(3) Uani 1 1 d U . . C63 C 0.3464(7) 0.7269(5) 0.3359(3) 0.0227(19) Uani 1 1 d U . . C64 C 0.4091(7) 0.7692(5) 0.3831(3) 0.0201(18) Uani 1 1 d U . . C67 C 0.0510(7) 0.7411(5) 0.4007(3) 0.024(2) Uani 1 1 d U . . C68 C -0.0046(7) 0.7761(5) 0.3504(3) 0.0190(18) Uani 1 1 d U . . C71 C 0.2287(6) 0.9848(5) 0.3276(3) 0.0211(18) Uani 1 1 d U . . C72 C 0.2024(7) 0.9943(5) 0.3821(3) 0.0207(18) Uani 1 1 d U . . O63 O 0.2548(5) 0.7528(3) 0.3209(2) 0.0229(13) Uani 1 1 d U . . O64 O 0.3578(4) 0.8217(3) 0.4011(2) 0.0204(13) Uani 1 1 d U . . O65 O 0.4998(5) 0.7502(3) 0.4010(2) 0.0251(13) Uani 1 1 d U . . O66 O 0.3877(5) 0.6742(4) 0.3169(2) 0.0282(14) Uani 1 1 d U . . O67 O 0.1500(5) 0.7625(3) 0.4139(2) 0.0195(12) Uani 1 1 d U . . O68 O 0.0580(4) 0.8243(3) 0.3304(2) 0.0212(13) Uani 1 1 d U . . O69 O -0.0975(5) 0.7591(3) 0.3346(2) 0.0214(13) Uani 1 1 d U . . O70 O -0.0018(4) 0.6978(3) 0.4251(2) 0.0228(14) Uani 1 1 d U . . O71 O 0.2388(5) 0.9158(3) 0.3130(2) 0.0231(13) Uani 1 1 d U . . O72 O 0.1914(4) 0.9294(3) 0.4055(2) 0.0215(13) Uani 1 1 d U . . O73 O 0.1939(5) 1.0578(3) 0.3992(2) 0.0258(15) Uani 1 1 d U . . O74 O 0.2376(5) 1.0432(4) 0.3022(2) 0.0276(15) Uani 1 1 d U . . Fe2 Fe 0.20963(10) 0.83476(7) 0.36296(4) 0.0198(3) Uani 1 1 d U . . C75 C 0.8907(8) 0.9989(5) 0.3377(3) 0.0225(19) Uani 1 1 d U . . C76 C 0.8751(7) 1.0357(5) 0.3881(3) 0.0173(18) Uani 1 1 d U . . C79 C 0.7183(7) 0.7849(6) 0.3871(3) 0.0243(18) Uani 1 1 d U . . C80 C 0.6568(7) 0.7832(5) 0.3327(3) 0.0198(18) Uani 1 1 d U . . C83 C 0.5087(7) 1.0056(5) 0.3843(3) 0.0204(19) Uani 1 1 d U . . C84 C 0.5360(7) 1.0453(5) 0.3351(3) 0.0220(19) Uani 1 1 d U . . O75 O 0.8145(5) 0.9497(3) 0.3200(2) 0.0233(13) Uani 1 1 d U . . O76 O 0.7869(5) 1.0167(3) 0.4045(2) 0.0207(13) Uani 1 1 d U . . O77 O 0.9439(5) 1.0839(3) 0.4094(2) 0.0237(14) Uani 1 1 d U . . O78 O 0.9723(5) 1.0153(3) 0.3193(2) 0.0273(15) Uani 1 1 d U . . O79 O 0.7464(4) 0.8516(3) 0.4058(2) 0.0220(13) Uani 1 1 d U . . O80 O 0.6313(5) 0.8496(3) 0.3155(2) 0.0249(13) Uani 1 1 d U . . O81 O 0.6370(5) 0.7220(4) 0.3090(2) 0.0285(14) Uani 1 1 d U . . O82 O 0.7369(5) 0.7229(3) 0.4092(2) 0.0262(13) Uani 1 1 d U . . O83 O 0.5746(4) 0.9541(3) 0.4010(2) 0.0225(13) Uani 1 1 d U . . O84 O 0.6117(5) 1.0150(3) 0.3161(2) 0.0248(14) Uani 1 1 d U . . O85 O 0.4870(5) 1.1003(4) 0.3183(2) 0.0287(15) Uani 1 1 d U . . O86 O 0.4345(5) 1.0268(3) 0.4042(2) 0.0233(14) Uani 1 1 d U . . Fe3 Fe 0.69210(10) 0.93835(7) 0.35869(4) 0.0192(3) Uani 1 1 d U . . C87 C 0.4513(7) 0.7588(5) 0.6068(3) 0.0174(18) Uani 1 1 d U . . C88 C 0.5039(7) 0.7268(5) 0.6594(3) 0.0180(18) Uani 1 1 d U . . C91 C 0.2648(7) 0.5130(6) 0.6738(3) 0.024(2) Uani 1 1 d U . . C92 C 0.2968(6) 0.5094(5) 0.6205(3) 0.0196(18) Uani 1 1 d U . . C95 C 0.0885(7) 0.7287(5) 0.6232(3) 0.0200(18) Uani 1 1 d U . . C96 C 0.1448(7) 0.7685(5) 0.6742(3) 0.0209(18) Uani 1 1 d U . . O87 O 0.3516(4) 0.7390(3) 0.5948(2) 0.0200(13) Uani 1 1 d U . . O88 O 0.4403(4) 0.6809(3) 0.6799(2) 0.0218(13) Uani 1 1 d U . . O89 O 0.5976(5) 0.7431(4) 0.6754(2) 0.0273(15) Uani 1 1 d U . . O90 O 0.5058(4) 0.7993(3) 0.5818(2) 0.0210(13) Uani 1 1 d U . . O91 O 0.2553(5) 0.5821(3) 0.6897(2) 0.0223(13) Uani 1 1 d U . . O92 O 0.3131(5) 0.5750(3) 0.6001(2) 0.0221(13) Uani 1 1 d U . . O93 O 0.3036(5) 0.4461(3) 0.6006(2) 0.0233(14) Uani 1 1 d U . . O94 O 0.2523(5) 0.4547(3) 0.6981(2) 0.0334(16) Uani 1 1 d U . . O95 O 0.1444(4) 0.6798(3) 0.6046(2) 0.0187(12) Uani 1 1 d U . . O96 O 0.2398(4) 0.7431(3) 0.6895(2) 0.0219(13) Uani 1 1 d U . . O97 O 0.1002(5) 0.8175(4) 0.6947(2) 0.0289(15) Uani 1 1 d U . . O98 O -0.0002(5) 0.7493(3) 0.6044(2) 0.0214(13) Uani 1 1 d U . . Fe4 Fe 0.29107(10) 0.66697(7) 0.64496(4) 0.0195(3) Uani 1 1 d U . . Na1 Na 0.0608(3) 0.13729(19) 0.35335(12) 0.0237(8) Uani 1 1 d U . . Na2 Na 0.3392(3) 0.1395(2) 0.35983(13) 0.0256(8) Uani 1 1 d U . . Na3 Na 0.5597(3) 0.63397(19) 0.35825(12) 0.0234(8) Uani 1 1 d U . . Na4 Na 0.8401(3) 0.63932(19) 0.36162(13) 0.0249(8) Uani 1 1 d U . . Na5 Na 0.2625(3) 0.5445(2) 0.50111(13) 0.0274(8) Uani 1 1 d U . . Na6 Na 0.7419(3) 0.6564(2) 0.49225(14) 0.0284(8) Uani 1 1 d U . . Na7 Na 0.2499(3) 0.7503(2) 0.50396(13) 0.0254(7) Uani 1 1 d U . . Na8 Na 0.7615(3) 0.8472(2) 0.51408(13) 0.0282(8) Uani 1 1 d U . . Na9 Na 0.2385(3) 0.9540(2) 0.50268(13) 0.0252(8) Uani 1 1 d U . . O101 O 0.8893(5) 0.9529(3) 0.5078(2) 0.0242(14) Uani 1 1 d U . . H10C H 0.9345 0.9597 0.5349 0.029 Uiso 1 1 calc R . . H10D H 0.9216 0.9490 0.4822 0.029 Uiso 1 1 calc R . . O102 O 0.6357(4) 0.9421(3) 0.5041(2) 0.0223(13) Uani 1 1 d U . . H10E H 0.6039 0.9462 0.5300 0.027 Uiso 1 1 calc R . . H10F H 0.5899 0.9355 0.4773 0.027 Uiso 1 1 calc R . . O103 O 0.1340(4) 0.4416(3) 0.5041(2) 0.0255(14) Uani 1 1 d U . . H10G H 0.0871 0.4385 0.4775 0.031 Uiso 1 1 calc R . . H10H H 0.1037 0.4432 0.5305 0.031 Uiso 1 1 calc R . . O104 O 0.1326(4) 0.6346(3) 0.5045(2) 0.0247(13) Uani 1 1 d U . . H10I H 0.1045 0.6309 0.5316 0.030 Uiso 1 1 calc R . . H10J H 0.0837 0.6317 0.4786 0.030 Uiso 1 1 calc R . . O105 O 0.6126(5) 0.5506(3) 0.4946(2) 0.0209(13) Uani 1 1 d U . . H10K H 0.5815 0.5517 0.5208 0.025 Uiso 1 1 calc R . . H10L H 0.5663 0.5471 0.4677 0.025 Uiso 1 1 calc R . . O106 O 0.3747(4) 0.6603(3) 0.4919(2) 0.0236(13) Uani 1 1 d U . . H10M H 0.4300 0.6638 0.5146 0.028 Uiso 1 1 calc R . . H10N H 0.3934 0.6634 0.4625 0.028 Uiso 1 1 calc R . . O107 O 0.6179(5) 0.7519(3) 0.4973(2) 0.0258(13) Uani 1 1 d U . . H10O H 0.5821 0.7455 0.5217 0.031 Uiso 1 1 calc R . . H10P H 0.5765 0.7586 0.4694 0.031 Uiso 1 1 calc R . . O108 O 0.8864(5) 0.7516(3) 0.5081(2) 0.0247(13) Uani 1 1 d U . . H10Q H 0.9287 0.7448 0.5357 0.030 Uiso 1 1 calc R . . H10R H 0.9212 0.7579 0.4833 0.030 Uiso 1 1 calc R . . O109 O 0.1252(4) 0.8410(3) 0.5124(2) 0.0223(13) Uani 1 1 d U . . H10S H 0.1047 0.8393 0.5414 0.027 Uiso 1 1 calc R . . H10T H 0.0711 0.8368 0.4890 0.027 Uiso 1 1 calc R . . O110 O 0.3696(5) 0.8640(3) 0.5023(2) 0.0239(13) Uani 1 1 d U . . H11C H 0.4176 0.8678 0.5285 0.029 Uiso 1 1 calc R . . H11D H 0.3987 0.8663 0.4755 0.029 Uiso 1 1 calc R . . O111 O 0.4772(5) 0.3903(3) 0.4261(2) 0.0267(15) Uani 1 1 d D . . H111 H 0.5107 0.4077 0.4027 0.040 Uiso 1 1 d RD . . H112 H 0.4136 0.3770 0.4121 0.040 Uiso 1 1 d RD . . O121 O 0.9746(5) 0.8902(3) 0.4290(2) 0.0280(15) Uani 1 1 d D . . H121 H 1.0182 0.9166 0.4137 0.042 Uiso 1 1 d RD . . H122 H 0.9256 0.8704 0.4067 0.042 Uiso 1 1 d RD . . 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 0.037(6) 0.029(5) 0.019(4) 0.007(4) 0.004(4) 0.002(4) C2 0.025(5) 0.032(5) 0.014(4) -0.006(3) 0.002(3) 0.002(4) C3 0.030(5) 0.020(5) 0.023(4) 0.002(3) 0.006(4) 0.000(4) C4 0.024(5) 0.026(5) 0.022(4) 0.001(3) 0.006(4) 0.003(4) C5 0.027(5) 0.027(5) 0.020(4) 0.003(3) 0.000(4) 0.006(4) C6 0.045(6) 0.025(5) 0.019(4) 0.000(3) 0.007(4) 0.002(4) C7 0.035(6) 0.029(5) 0.017(4) 0.009(3) 0.011(4) 0.001(4) C8 0.031(5) 0.021(5) 0.024(4) 0.002(3) 0.004(4) -0.002(4) C9 0.037(6) 0.040(5) 0.020(4) 0.008(4) 0.001(4) 0.001(5) C10 0.035(6) 0.046(6) 0.019(4) 0.001(4) 0.005(4) -0.002(5) S1 0.0441(16) 0.0232(14) 0.0184(11) 0.0016(10) 0.0014(10) 0.0035(11) S2 0.0416(16) 0.0318(15) 0.0200(11) 0.0007(10) 0.0076(10) 0.0089(12) S3 0.0378(15) 0.0261(14) 0.0172(11) 0.0018(10) 0.0055(10) 0.0054(11) S4 0.0494(16) 0.0242(14) 0.0196(11) -0.0012(10) 0.0076(11) 0.0068(12) S5 0.0443(16) 0.0250(14) 0.0180(11) 0.0012(10) 0.0074(10) 0.0036(11) S6 0.0445(16) 0.0280(14) 0.0186(11) 0.0024(10) 0.0069(10) 0.0078(11) S7 0.0484(17) 0.0310(15) 0.0217(12) 0.0052(11) 0.0022(11) 0.0056(12) S8 0.0495(17) 0.0296(15) 0.0194(11) 0.0008(10) 0.0107(11) 0.0002(12) C11 0.031(5) 0.027(5) 0.019(4) -0.004(4) -0.006(4) 0.004(4) C12 0.034(5) 0.029(5) 0.013(4) -0.004(3) 0.006(4) 0.003(4) C13 0.028(5) 0.027(5) 0.022(4) 0.005(3) 0.009(4) 0.013(4) C14 0.026(5) 0.027(5) 0.015(4) 0.006(3) 0.010(3) 0.009(4) C15 0.016(5) 0.030(5) 0.025(4) 0.005(3) 0.004(3) 0.000(4) C16 0.026(5) 0.034(5) 0.021(4) 0.005(3) -0.002(4) 0.006(4) C17 0.025(5) 0.033(5) 0.018(4) 0.006(3) 0.001(3) 0.015(4) C18 0.023(5) 0.035(5) 0.019(4) 0.008(3) 0.004(4) 0.007(4) C19 0.035(6) 0.039(5) 0.023(4) 0.007(4) 0.008(4) 0.007(5) C20 0.025(5) 0.037(5) 0.016(4) 0.004(4) 0.001(4) 0.010(4) S11 0.0363(15) 0.0273(14) 0.0212(11) 0.0048(10) 0.0059(10) 0.0006(11) S12 0.0351(14) 0.0257(14) 0.0181(11) 0.0022(10) 0.0031(10) 0.0015(11) S13 0.0356(14) 0.0247(14) 0.0211(11) 0.0027(10) 0.0014(10) -0.0006(11) S14 0.0368(15) 0.0329(15) 0.0199(11) 0.0049(10) 0.0027(10) -0.0022(11) S15 0.0375(15) 0.0304(15) 0.0197(11) 0.0037(10) 0.0028(10) -0.0028(11) S16 0.0367(15) 0.0305(15) 0.0214(11) 0.0027(10) 0.0053(10) -0.0013(11) S17 0.0375(15) 0.0343(15) 0.0205(11) 0.0041(10) 0.0050(10) 0.0008(12) S18 0.0335(14) 0.0377(16) 0.0187(11) 0.0032(10) 0.0001(10) 0.0026(11) C21 0.041(6) 0.031(5) 0.015(4) -0.001(4) 0.004(4) 0.001(4) C22 0.025(5) 0.049(6) 0.018(4) -0.005(4) 0.004(4) 0.006(4) C23 0.039(6) 0.027(5) 0.023(4) -0.003(4) 0.006(4) 0.005(4) C24 0.028(5) 0.029(5) 0.020(4) 0.003(3) 0.007(4) 0.008(4) C25 0.034(6) 0.018(5) 0.023(4) -0.007(3) 0.000(4) -0.004(4) C26 0.023(5) 0.019(5) 0.023(4) -0.003(3) 0.003(3) 0.002(4) C27 0.011(4) 0.027(5) 0.024(4) 0.002(3) 0.002(3) 0.002(4) C28 0.017(5) 0.027(5) 0.024(4) 0.004(3) 0.001(3) 0.002(4) C29 0.024(5) 0.022(4) 0.022(4) 0.000(4) 0.003(4) 0.007(4) C30 0.025(5) 0.026(5) 0.017(4) 0.002(3) 0.003(4) 0.004(4) S21 0.0391(15) 0.0313(15) 0.0197(11) 0.0033(10) 0.0049(10) 0.0003(11) S22 0.0388(15) 0.0297(15) 0.0207(11) -0.0001(10) -0.0006(10) 0.0064(11) S23 0.0374(15) 0.0277(14) 0.0177(11) -0.0021(10) 0.0009(10) 0.0009(11) S24 0.0375(15) 0.0336(15) 0.0177(11) 0.0028(10) 0.0013(10) -0.0046(11) S25 0.0348(14) 0.0293(14) 0.0191(11) 0.0013(10) 0.0025(10) -0.0063(11) S26 0.0328(14) 0.0273(14) 0.0207(11) -0.0009(10) 0.0022(10) -0.0044(11) S27 0.0421(15) 0.0283(14) 0.0171(11) 0.0016(10) 0.0055(10) -0.0056(11) S28 0.0322(14) 0.0208(13) 0.0176(11) 0.0008(9) 0.0021(9) 0.0000(10) C31 0.024(5) 0.027(5) 0.016(4) 0.005(3) 0.000(3) 0.003(4) C32 0.031(5) 0.033(5) 0.014(4) 0.006(4) 0.003(3) 0.008(4) C33 0.032(5) 0.020(5) 0.025(4) 0.008(3) 0.004(4) 0.009(4) C34 0.020(5) 0.036(5) 0.016(3) 0.002(3) 0.004(3) -0.001(4) C35 0.025(5) 0.031(5) 0.017(3) 0.001(3) 0.007(3) 0.003(4) C36 0.030(5) 0.021(5) 0.023(4) -0.001(3) 0.004(4) -0.003(4) C37 0.023(5) 0.029(5) 0.019(4) 0.003(3) 0.012(3) 0.003(4) C38 0.027(5) 0.023(5) 0.023(4) 0.002(3) 0.005(4) 0.003(4) C39 0.022(5) 0.033(5) 0.020(4) 0.002(4) 0.005(4) 0.005(4) C40 0.023(5) 0.029(5) 0.023(4) 0.002(4) 0.004(4) 0.003(4) S31 0.0356(15) 0.0290(14) 0.0197(11) 0.0034(10) -0.0019(10) -0.0062(11) S32 0.0348(14) 0.0262(14) 0.0221(11) 0.0040(10) 0.0071(10) -0.0005(11) S33 0.0370(15) 0.0237(14) 0.0186(11) 0.0024(10) 0.0029(10) -0.0041(11) S34 0.0367(15) 0.0263(14) 0.0197(11) 0.0016(10) 0.0011(10) -0.0019(11) S35 0.0346(14) 0.0239(14) 0.0175(11) 0.0007(9) 0.0020(10) -0.0036(11) S36 0.0336(14) 0.0257(14) 0.0176(11) 0.0013(9) 0.0016(10) -0.0032(11) S37 0.0326(14) 0.0238(14) 0.0184(11) 0.0031(9) 0.0005(9) -0.0005(10) S38 0.0387(15) 0.0237(14) 0.0200(11) 0.0042(10) 0.0051(10) -0.0078(11) C41 0.024(10) 0.019(8) 0.022(7) 0.012(6) 0.009(8) 0.015(7) C42 0.018(10) 0.030(7) 0.007(7) 0.003(7) -0.006(8) 0.014(9) C43 0.020(5) 0.026(5) 0.017(4) 0.007(3) 0.004(3) 0.002(4) C44 0.027(5) 0.017(4) 0.013(3) 0.001(3) 0.000(3) -0.002(4) C45 0.027(5) 0.026(5) 0.015(4) 0.003(3) 0.003(4) 0.002(4) S41 0.0403(15) 0.0282(14) 0.0207(11) -0.0010(10) 0.0079(10) 0.0043(11) S42 0.0410(15) 0.0240(14) 0.0196(11) 0.0045(10) 0.0007(10) 0.0045(11) S43 0.0407(15) 0.0259(14) 0.0188(11) 0.0029(10) 0.0027(10) 0.0061(11) S44 0.0382(15) 0.0256(14) 0.0165(11) 0.0025(10) 0.0016(10) 0.0083(11) C46 0.032(11) 0.045(11) 0.032(10) 0.023(8) 0.024(10) 0.007(8) C47 0.029(11) 0.018(9) 0.024(6) 0.001(7) -0.014(10) -0.002(8) C51 0.015(4) 0.032(5) 0.015(4) -0.002(3) -0.003(3) 0.007(4) C52 0.024(5) 0.024(6) 0.023(4) -0.002(4) 0.005(3) -0.001(4) C55 0.016(5) 0.023(4) 0.026(4) 0.004(3) 0.013(3) 0.001(3) C56 0.034(6) 0.008(4) 0.024(4) -0.004(3) 0.007(4) 0.002(4) C59 0.024(5) 0.020(5) 0.021(4) 0.000(3) 0.004(4) 0.007(4) C60 0.022(5) 0.023(5) 0.024(4) 0.005(4) 0.004(4) 0.001(4) O51 0.018(3) 0.025(4) 0.025(3) -0.002(3) -0.001(2) 0.002(2) O52 0.019(3) 0.016(3) 0.028(3) -0.006(2) 0.006(2) 0.002(2) O53 0.028(3) 0.023(4) 0.022(3) 0.001(2) 0.005(3) 0.001(3) O54 0.023(3) 0.027(3) 0.028(3) -0.001(3) 0.010(3) 0.001(3) O55 0.019(3) 0.019(3) 0.024(3) -0.001(2) 0.000(2) 0.005(2) O56 0.029(3) 0.017(3) 0.018(3) -0.001(2) 0.004(2) 0.002(3) O57 0.034(4) 0.018(3) 0.030(3) -0.005(3) 0.010(3) -0.004(3) O58 0.027(4) 0.020(3) 0.028(3) 0.003(3) 0.011(3) 0.006(3) O59 0.024(3) 0.030(4) 0.022(3) 0.003(3) 0.008(2) 0.011(3) O60 0.023(3) 0.024(4) 0.022(3) 0.001(3) 0.005(2) 0.006(3) O61 0.024(4) 0.034(4) 0.027(3) 0.005(3) 0.007(3) 0.009(3) O62 0.040(4) 0.025(4) 0.033(4) 0.013(3) 0.008(3) 0.014(3) Fe1 0.0231(7) 0.0214(8) 0.0187(6) -0.0001(5) 0.0034(5) 0.0025(6) C63 0.029(5) 0.028(5) 0.013(4) 0.003(3) 0.005(3) 0.008(4) C64 0.026(5) 0.020(5) 0.017(4) 0.007(3) 0.008(3) 0.006(4) C67 0.025(5) 0.024(6) 0.021(4) 0.002(4) -0.001(3) -0.002(4) C68 0.026(4) 0.014(5) 0.018(4) -0.006(3) 0.005(3) 0.002(4) C71 0.010(4) 0.024(5) 0.028(4) 0.006(4) -0.002(4) 0.004(4) C72 0.014(5) 0.023(4) 0.026(4) 0.002(4) 0.004(4) 0.007(4) O63 0.022(3) 0.028(3) 0.019(3) -0.001(2) 0.000(2) 0.009(3) O64 0.023(3) 0.018(3) 0.022(3) -0.003(2) 0.003(2) 0.007(2) O65 0.019(3) 0.028(3) 0.030(3) 0.006(3) 0.005(2) 0.010(3) O66 0.034(3) 0.035(4) 0.019(3) 0.003(3) 0.009(3) 0.013(3) O67 0.024(3) 0.013(3) 0.023(3) -0.003(2) 0.006(2) 0.003(2) O68 0.017(3) 0.025(4) 0.022(3) 0.002(2) 0.003(2) 0.004(2) O69 0.020(3) 0.019(3) 0.024(3) 0.002(3) -0.002(3) -0.001(3) O70 0.021(3) 0.022(4) 0.026(3) 0.003(3) 0.007(3) 0.002(3) O71 0.031(4) 0.022(3) 0.018(3) 0.006(2) 0.008(3) 0.005(3) O72 0.023(3) 0.022(3) 0.020(3) 0.003(2) 0.003(2) 0.008(3) O73 0.033(4) 0.017(3) 0.030(3) 0.000(3) 0.007(3) 0.011(3) O74 0.036(4) 0.027(4) 0.020(3) 0.002(3) 0.007(3) -0.002(3) Fe2 0.0203(7) 0.0220(8) 0.0178(6) 0.0020(5) 0.0037(5) 0.0047(6) C75 0.034(5) 0.018(5) 0.018(4) 0.007(3) 0.008(4) 0.006(4) C76 0.018(4) 0.018(5) 0.014(4) 0.004(3) -0.006(3) 0.009(3) C79 0.020(5) 0.025(4) 0.029(4) 0.001(3) 0.006(4) 0.000(4) C80 0.018(5) 0.023(4) 0.022(4) 0.002(3) 0.012(3) -0.001(4) C83 0.011(4) 0.026(5) 0.023(4) -0.002(4) -0.001(3) -0.002(4) C84 0.019(5) 0.020(5) 0.028(5) 0.002(4) 0.005(4) 0.002(4) O75 0.028(3) 0.023(4) 0.019(3) -0.002(2) 0.004(2) -0.003(3) O76 0.026(3) 0.018(3) 0.018(3) 0.001(2) 0.007(2) 0.000(3) O77 0.021(3) 0.026(4) 0.025(3) -0.004(3) 0.006(3) 0.001(3) O78 0.027(4) 0.028(4) 0.030(3) -0.001(3) 0.014(3) 0.000(3) O79 0.023(3) 0.016(3) 0.027(3) 0.001(2) 0.003(2) 0.004(2) O80 0.029(4) 0.022(3) 0.023(3) 0.000(2) 0.002(3) -0.002(3) O81 0.038(4) 0.023(3) 0.027(3) -0.002(3) 0.013(3) -0.003(3) O82 0.031(3) 0.021(3) 0.028(3) 0.000(3) 0.008(2) 0.004(3) O83 0.022(3) 0.024(4) 0.023(3) 0.006(3) 0.008(2) 0.005(3) O84 0.028(3) 0.026(4) 0.023(3) 0.003(3) 0.009(3) 0.010(3) O85 0.032(4) 0.034(4) 0.024(3) 0.005(3) 0.009(3) 0.018(3) O86 0.019(3) 0.033(4) 0.021(3) 0.000(3) 0.007(2) 0.010(3) Fe3 0.0208(7) 0.0196(7) 0.0175(6) 0.0010(5) 0.0026(5) 0.0041(5) C87 0.014(4) 0.020(5) 0.019(4) -0.001(3) 0.005(3) 0.007(3) C88 0.021(4) 0.019(5) 0.015(4) 0.004(3) 0.008(3) 0.004(4) C91 0.026(5) 0.027(5) 0.018(4) 0.006(3) -0.001(4) 0.001(4) C92 0.013(5) 0.021(4) 0.023(4) 0.004(3) -0.004(3) 0.000(4) C95 0.018(4) 0.023(5) 0.019(4) 0.001(3) 0.005(3) 0.003(4) C96 0.021(5) 0.024(5) 0.017(4) 0.001(3) 0.000(3) -0.001(4) O87 0.019(3) 0.023(3) 0.019(3) 0.006(2) 0.006(2) 0.000(2) O88 0.021(3) 0.021(4) 0.022(3) 0.008(2) -0.001(2) 0.000(2) O89 0.017(3) 0.035(4) 0.031(3) 0.008(3) 0.006(3) 0.005(3) O90 0.023(3) 0.023(4) 0.017(3) 0.000(3) 0.004(2) 0.002(3) O91 0.029(3) 0.017(3) 0.023(3) 0.003(2) 0.011(3) 0.001(3) O92 0.031(4) 0.016(3) 0.020(3) 0.002(2) 0.005(2) 0.004(3) O93 0.022(3) 0.019(3) 0.029(3) 0.005(3) 0.005(3) 0.000(3) O94 0.053(5) 0.018(4) 0.028(3) 0.003(3) 0.004(3) -0.005(3) O95 0.019(3) 0.022(4) 0.016(3) 0.000(2) 0.003(2) 0.004(2) O96 0.023(3) 0.024(3) 0.020(3) -0.004(2) 0.005(2) 0.008(3) O97 0.027(4) 0.036(4) 0.025(3) -0.007(3) 0.003(3) 0.010(3) O98 0.021(3) 0.024(4) 0.018(3) -0.003(3) -0.002(2) 0.001(3) Fe4 0.0202(7) 0.0206(8) 0.0186(6) 0.0031(5) 0.0041(5) 0.0048(6) Na1 0.027(2) 0.019(2) 0.0258(18) 0.0032(15) 0.0057(15) 0.0028(15) Na2 0.027(2) 0.023(2) 0.0268(19) 0.0001(16) 0.0048(15) 0.0020(16) Na3 0.0259(19) 0.0203(19) 0.0248(18) 0.0030(15) 0.0062(15) 0.0026(15) Na4 0.026(2) 0.019(2) 0.0290(19) 0.0012(15) 0.0029(15) 0.0008(15) Na5 0.028(2) 0.023(2) 0.0312(18) 0.0012(16) 0.0039(16) 0.0046(16) Na6 0.022(2) 0.024(2) 0.039(2) 0.0086(16) 0.0044(16) 0.0028(15) Na7 0.0232(17) 0.0240(17) 0.0296(17) -0.0004(14) 0.0047(14) 0.0044(14) Na8 0.024(2) 0.022(2) 0.038(2) 0.0067(16) 0.0040(16) 0.0041(15) Na9 0.029(2) 0.021(2) 0.0283(18) -0.0006(15) 0.0094(16) 0.0057(16) O101 0.025(3) 0.030(4) 0.018(3) 0.005(3) 0.001(3) 0.004(3) O102 0.024(3) 0.027(3) 0.015(3) -0.001(3) 0.000(2) 0.001(3) O103 0.025(3) 0.036(4) 0.016(3) 0.007(3) 0.001(2) 0.006(3) O104 0.023(3) 0.031(3) 0.020(3) 0.000(3) 0.004(2) 0.006(2) O105 0.028(3) 0.022(3) 0.013(3) -0.004(2) 0.005(2) 0.004(3) O106 0.019(3) 0.031(3) 0.021(3) 0.001(3) 0.003(2) 0.005(2) O107 0.025(3) 0.031(3) 0.022(3) 0.006(3) 0.005(3) 0.006(3) O108 0.024(3) 0.028(3) 0.022(3) 0.000(3) 0.001(3) 0.005(2) O109 0.028(3) 0.027(3) 0.011(3) -0.004(2) 0.002(2) 0.004(3) O110 0.029(3) 0.026(3) 0.016(3) 0.003(3) 0.001(2) 0.003(2) O111 0.019(3) 0.032(4) 0.030(3) 0.009(3) 0.004(3) 0.006(3) O121 0.034(4) 0.028(4) 0.022(3) -0.006(3) 0.003(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.516(12) . ? C1 S1 1.827(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 S2 1.806(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.357(12) . ? C3 S2 1.722(9) . ? C3 S3 1.757(9) . ? C4 S4 1.739(9) . ? C4 S1 1.747(9) . ? C5 C6 1.339(11) . ? C5 S4 1.727(9) . ? C5 S3 1.755(9) . ? C6 S5 1.730(9) . ? C6 S6 1.745(10) . ? C7 C8 1.347(12) . ? C7 S8 1.739(9) . ? C7 S5 1.751(8) . ? C8 S6 1.727(9) . ? C8 S7 1.758(9) . ? C9 C10 1.486(13) . ? C9 S7 1.812(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 S8 1.783(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.508(12) . ? C11 S11 1.814(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 S12 1.798(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.349(12) . ? C13 S12 1.736(9) . ? C13 S13 1.747(8) . ? C14 S11 1.740(8) . ? C14 S14 1.744(8) . ? C15 C16 1.353(11) . ? C15 S14 1.731(9) . ? C15 S13 1.737(9) . ? C16 S15 1.720(9) . ? C16 S16 1.750(9) . ? C17 C18 1.342(13) . ? C17 S15 1.743(9) . ? C17 S18 1.745(9) . ? C18 S16 1.733(9) . ? C18 S17 1.746(9) . ? C19 C20 1.508(13) . ? C19 S17 1.800(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 S18 1.810(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.494(13) . ? C21 S21 1.807(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 S22 1.805(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.333(13) . ? C23 S23 1.737(9) . ? C23 S22 1.747(9) . ? C24 S21 1.739(9) . ? C24 S24 1.763(9) . ? C25 C26 1.349(11) . ? C25 S24 1.731(9) . ? C25 S23 1.739(9) . ? C26 S26 1.733(9) . ? C26 S25 1.740(9) . ? C27 C28 1.364(12) . ? C27 S25 1.732(8) . ? C27 S28 1.740(9) . ? C28 S26 1.738(9) . ? C28 S27 1.741(9) . ? C29 C30 1.504(12) . ? C29 S27 1.795(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 S28 1.808(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.511(12) . ? C31 S31 1.823(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 S32 1.814(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.367(12) . ? C33 S33 1.731(9) . ? C33 S32 1.743(9) . ? C34 S31 1.739(9) . ? C34 S34 1.739(9) . ? C35 C36 1.381(11) . ? C35 S33 1.731(9) . ? C35 S34 1.731(9) . ? C36 S36 1.718(9) . ? C36 S35 1.739(9) . ? C37 C38 1.356(12) . ? C37 S38 1.735(8) . ? C37 S35 1.747(8) . ? C38 S36 1.744(8) . ? C38 S37 1.748(9) . ? C39 C40 1.508(12) . ? C39 S37 1.824(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 S38 1.800(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.483(15) . ? C41 S41 1.707(14) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 S42 1.891(19) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.353(12) . ? C43 S43 1.740(8) . ? C43 S42 1.742(8) . ? C44 S44 1.737(8) . ? C44 S41 1.750(8) . ? C45 C45 1.371(15) 2_665 ? C45 S44 1.728(9) . ? C45 S43 1.732(9) . ? S41 C46 1.921(19) . ? S42 C47 1.760(19) . ? C46 C47 1.478(14) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C51 O54 1.212(10) . ? C51 O51 1.280(10) . ? C51 C52 1.545(12) . ? C52 O53 1.242(10) . ? C52 O52 1.267(10) . ? C55 O58 1.208(10) . ? C55 O55 1.302(10) . ? C55 C56 1.561(12) . ? C56 O57 1.207(9) . ? C56 O56 1.274(10) . ? C59 O62 1.203(10) . ? C59 O59 1.302(10) . ? C59 C60 1.562(11) . ? C60 O61 1.214(10) . ? C60 O60 1.273(10) . ? O51 Fe1 1.993(6) . ? O52 Fe1 2.052(6) . ? O52 Na5 2.599(7) . ? O53 Na3 2.384(6) . ? O54 Na3 2.382(7) . ? O55 Fe1 2.036(6) . ? O55 Na6 2.688(6) 2_666 ? O56 Fe1 1.985(6) . ? O57 Na1 2.390(6) . ? O58 Na2 2.398(7) . ? O58 Na8 2.497(7) 2_666 ? O58 Na1 2.746(7) . ? O59 Fe1 1.976(6) . ? O60 Fe1 2.013(6) . ? O61 Na4 2.431(7) 1_455 ? O62 Na4 2.496(7) 1_455 ? C63 O66 1.222(10) . ? C63 O63 1.270(10) . ? C63 C64 1.540(12) . ? C64 O65 1.232(10) . ? C64 O64 1.279(10) . ? C67 O70 1.229(10) . ? C67 O67 1.280(10) . ? C67 C68 1.551(11) . ? C68 O69 1.206(10) . ? C68 O68 1.291(10) . ? C71 O74 1.228(10) . ? C71 O71 1.279(10) . ? C71 C72 1.542(12) . ? C72 O73 1.209(10) . ? C72 O72 1.299(10) . ? O63 Fe2 1.969(6) . ? O64 Fe2 2.010(6) . ? O65 Na3 2.522(7) . ? O66 Na3 2.416(7) . ? O67 Fe2 2.045(6) . ? O67 Na7 2.543(7) . ? O68 Fe2 1.975(6) . ? O69 Na4 2.339(6) 1_455 ? O70 Na4 2.572(7) 1_455 ? O71 Fe2 1.995(5) . ? O72 Fe2 2.036(6) . ? O72 Na9 2.590(6) . ? O73 Na1 2.414(7) 1_565 ? O73 Na2 2.606(7) 1_565 ? O73 Na8 2.802(7) 2_676 ? O74 Na2 2.443(7) 1_565 ? C75 O78 1.225(10) . ? C75 O75 1.287(10) . ? C75 C76 1.525(11) . ? C76 O77 1.246(10) . ? C76 O76 1.284(10) . ? C79 O82 1.242(10) . ? C79 O79 1.274(10) . ? C79 C80 1.530(12) . ? C80 O81 1.231(10) . ? C80 O80 1.279(10) . ? C83 O86 1.215(10) . ? C83 O83 1.286(10) . ? C83 C84 1.555(11) . ? C84 O85 1.213(10) . ? C84 O84 1.281(10) . ? O75 Fe3 1.984(6) . ? O76 Fe3 2.037(6) . ? O76 Na9 2.588(6) 2_676 ? O77 Na1 2.404(6) 1_665 ? O78 Na1 2.451(7) 1_665 ? O79 Fe3 2.038(6) . ? O79 Na8 2.853(7) . ? O80 Fe3 1.972(6) . ? O81 Na3 2.289(6) . ? O82 Na4 2.470(7) . ? O82 Na6 2.484(7) . ? O82 Na3 2.818(7) . ? O83 Fe3 2.021(6) . ? O84 Fe3 1.968(6) . ? O85 Na2 2.432(7) 1_565 ? O86 Na2 2.546(7) 1_565 ? C87 O90 1.225(9) . ? C87 O87 1.280(9) . ? C87 C88 1.565(11) . ? C88 O89 1.212(10) . ? C88 O88 1.283(9) . ? C91 O94 1.217(10) . ? C91 O91 1.291(10) . ? C91 C92 1.532(12) . ? C92 O93 1.233(10) . ? C92 O92 1.282(10) . ? C95 O98 1.226(10) . ? C95 O95 1.277(10) . ? C95 C96 1.573(12) . ? C96 O97 1.217(10) . ? C96 O96 1.304(10) . ? O87 Fe4 2.035(5) . ? O87 Na7 2.565(6) . ? O88 Fe4 1.972(6) . ? O89 Na2 2.395(7) 2_666 ? O90 Na2 2.494(6) 2_666 ? O91 Fe4 1.970(5) . ? O92 Fe4 2.047(6) . ? O92 Na5 2.656(6) . ? O93 Na3 2.403(7) 2_666 ? O93 Na4 2.604(6) 2_666 ? O93 Na6 3.007(7) 2_666 ? O94 Na4 2.404(7) 2_666 ? O95 Fe4 2.015(5) . ? O96 Fe4 1.972(6) . ? O97 Na1 2.398(7) 2_566 ? O98 Na1 2.478(7) 2_566 ? Na1 O97 2.398(7) 2_566 ? Na1 O77 2.404(6) 1_445 ? Na1 O73 2.414(7) 1_545 ? Na1 O78 2.451(7) 1_445 ? Na1 O98 2.478(7) 2_566 ? Na2 O89 2.395(7) 2_666 ? Na2 O85 2.432(7) 1_545 ? Na2 O74 2.443(7) 1_545 ? Na2 O90 2.494(6) 2_666 ? Na2 O86 2.546(7) 1_545 ? Na2 O73 2.606(7) 1_545 ? Na3 O93 2.403(7) 2_666 ? Na4 O69 2.339(6) 1_655 ? Na4 O94 2.404(7) 2_666 ? Na4 O61 2.431(7) 1_655 ? Na4 O62 2.496(7) 1_655 ? Na4 O70 2.572(7) 1_655 ? Na4 O93 2.604(6) 2_666 ? Na4 C91 2.984(10) 2_666 ? Na5 O105 2.333(6) 2_666 ? Na5 O104 2.336(7) . ? Na5 O103 2.362(7) . ? Na5 O106 2.434(7) . ? Na6 O107 2.355(7) . ? Na6 O103 2.365(7) 2_666 ? Na6 O108 2.386(7) . ? Na6 O105 2.402(6) . ? Na6 O55 2.688(6) 2_666 ? Na6 O93 3.007(7) 2_666 ? Na7 O109 2.317(7) . ? Na7 O106 2.332(7) . ? Na7 O110 2.430(7) . ? Na7 O104 2.435(7) . ? Na8 O102 2.335(7) . ? Na8 O108 2.370(7) . ? Na8 O107 2.382(7) . ? Na8 O101 2.404(7) . ? Na8 O58 2.497(7) 2_666 ? Na8 O73 2.802(7) 2_676 ? Na9 O101 2.330(6) 2_676 ? Na9 O110 2.335(7) . ? Na9 O102 2.369(6) 2_676 ? Na9 O109 2.406(7) . ? Na9 O76 2.588(6) 2_676 ? O101 Na9 2.330(6) 2_676 ? O101 H10C 0.8500 . ? O101 H10D 0.8500 . ? O102 Na9 2.369(6) 2_676 ? O102 H10E 0.8500 . ? O102 H10F 0.8500 . ? O103 Na6 2.365(7) 2_666 ? O103 H10G 0.8500 . ? O103 H10H 0.8500 . ? O104 H10I 0.8500 . ? O104 H10J 0.8500 . ? O105 Na5 2.333(6) 2_666 ? O105 H10K 0.8500 . ? O105 H10L 0.8500 . ? O106 H10M 0.8500 . ? O106 H10N 0.8500 . ? O107 H10O 0.8500 . ? O107 H10P 0.8500 . ? O108 H10Q 0.8500 . ? O108 H10R 0.8500 . ? O109 H10S 0.8500 . ? O109 H10T 0.8500 . ? O110 H11C 0.8500 . ? O110 H11D 0.8500 . ? O111 H111 0.8498 . ? O111 H112 0.8509 . ? O121 H121 0.8477 . ? O121 H122 0.8470 . ? 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 C2 C1 S1 114.2(6) . . ? C2 C1 H1A 108.7 . . ? S1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? S1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C1 C2 S2 114.5(6) . . ? C1 C2 H2A 108.6 . . ? S2 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? S2 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C4 C3 S2 128.7(7) . . ? C4 C3 S3 114.9(7) . . ? S2 C3 S3 116.4(5) . . ? C3 C4 S4 118.3(7) . . ? C3 C4 S1 129.2(7) . . ? S4 C4 S1 112.5(5) . . ? C6 C5 S4 123.4(7) . . ? C6 C5 S3 122.5(7) . . ? S4 C5 S3 114.2(5) . . ? C5 C6 S5 121.7(7) . . ? C5 C6 S6 123.6(7) . . ? S5 C6 S6 114.6(5) . . ? C8 C7 S8 128.6(7) . . ? C8 C7 S5 115.9(7) . . ? S8 C7 S5 115.5(5) . . ? C7 C8 S6 118.1(7) . . ? C7 C8 S7 128.1(7) . . ? S6 C8 S7 113.8(5) . . ? C10 C9 S7 114.5(6) . . ? C10 C9 H9A 108.6 . . ? S7 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? S7 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C9 C10 S8 115.6(7) . . ? C9 C10 H10A 108.4 . . ? S8 C10 H10A 108.4 . . ? C9 C10 H10B 108.4 . . ? S8 C10 H10B 108.4 . . ? H10A C10 H10B 107.4 . . ? C4 S1 C1 101.5(4) . . ? C3 S2 C2 101.4(4) . . ? C5 S3 C3 96.4(4) . . ? C5 S4 C4 96.1(4) . . ? C6 S5 C7 95.9(4) . . ? C8 S6 C6 95.4(4) . . ? C8 S7 C9 102.6(4) . . ? C7 S8 C10 99.8(4) . . ? C12 C11 S11 114.0(6) . . ? C12 C11 H11A 108.8 . . ? S11 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? S11 C11 H11B 108.8 . . ? H11A C11 H11B 107.6 . . ? C11 C12 S12 114.2(6) . . ? C11 C12 H12A 108.7 . . ? S12 C12 H12A 108.7 . . ? C11 C12 H12B 108.7 . . ? S12 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C14 C13 S12 128.0(7) . . ? C14 C13 S13 116.8(7) . . ? S12 C13 S13 115.2(5) . . ? C13 C14 S11 129.3(7) . . ? C13 C14 S14 116.8(6) . . ? S11 C14 S14 113.9(5) . . ? C16 C15 S14 123.3(7) . . ? C16 C15 S13 121.8(7) . . ? S14 C15 S13 115.0(5) . . ? C15 C16 S15 123.7(7) . . ? C15 C16 S16 121.6(7) . . ? S15 C16 S16 114.7(5) . . ? C18 C17 S15 116.6(6) . . ? C18 C17 S18 128.2(7) . . ? S15 C17 S18 115.2(6) . . ? C17 C18 S16 117.5(6) . . ? C17 C18 S17 129.0(7) . . ? S16 C18 S17 113.5(5) . . ? C20 C19 S17 112.4(6) . . ? C20 C19 H19A 109.1 . . ? S17 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? S17 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C19 C20 S18 113.2(6) . . ? C19 C20 H20A 108.9 . . ? S18 C20 H20A 108.9 . . ? C19 C20 H20B 108.9 . . ? S18 C20 H20B 108.9 . . ? H20A C20 H20B 107.8 . . ? C14 S11 C11 101.9(4) . . ? C13 S12 C12 100.9(4) . . ? C15 S13 C13 95.5(4) . . ? C15 S14 C14 95.8(4) . . ? C16 S15 C17 95.8(4) . . ? C18 S16 C16 95.1(4) . . ? C18 S17 C19 101.7(4) . . ? C17 S18 C20 99.3(4) . . ? C22 C21 S21 113.4(6) . . ? C22 C21 H21A 108.9 . . ? S21 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? S21 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 S22 114.8(6) . . ? C21 C22 H22A 108.6 . . ? S22 C22 H22A 108.6 . . ? C21 C22 H22B 108.6 . . ? S22 C22 H22B 108.6 . . ? H22A C22 H22B 107.5 . . ? C24 C23 S23 118.3(7) . . ? C24 C23 S22 126.6(7) . . ? S23 C23 S22 115.1(5) . . ? C23 C24 S21 131.0(7) . . ? C23 C24 S24 115.9(7) . . ? S21 C24 S24 113.1(5) . . ? C26 C25 S24 123.9(7) . . ? C26 C25 S23 121.1(7) . . ? S24 C25 S23 114.9(5) . . ? C25 C26 S26 123.0(7) . . ? C25 C26 S25 122.4(7) . . ? S26 C26 S25 114.5(5) . . ? C28 C27 S25 115.9(6) . . ? C28 C27 S28 128.0(7) . . ? S25 C27 S28 116.0(5) . . ? C27 C28 S26 117.3(6) . . ? C27 C28 S27 128.0(7) . . ? S26 C28 S27 114.7(5) . . ? C30 C29 S27 112.8(6) . . ? C30 C29 H29A 109.0 . . ? S27 C29 H29A 109.0 . . ? C30 C29 H29B 109.0 . . ? S27 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C29 C30 S28 116.4(6) . . ? C29 C30 H30A 108.2 . . ? S28 C30 H30A 108.2 . . ? C29 C30 H30B 108.2 . . ? S28 C30 H30B 108.2 . . ? H30A C30 H30B 107.3 . . ? C24 S21 C21 101.6(4) . . ? C23 S22 C22 99.9(4) . . ? C23 S23 C25 95.1(4) . . ? C25 S24 C24 95.5(4) . . ? C27 S25 C26 95.9(4) . . ? C26 S26 C28 95.4(4) . . ? C28 S27 C29 100.3(4) . . ? C27 S28 C30 103.0(4) . . ? C32 C31 S31 112.3(6) . . ? C32 C31 H31A 109.1 . . ? S31 C31 H31A 109.1 . . ? C32 C31 H31B 109.1 . . ? S31 C31 H31B 109.1 . . ? H31A C31 H31B 107.9 . . ? C31 C32 S32 113.9(6) . . ? C31 C32 H32A 108.8 . . ? S32 C32 H32A 108.8 . . ? C31 C32 H32B 108.8 . . ? S32 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C34 C33 S33 117.2(6) . . ? C34 C33 S32 128.2(7) . . ? S33 C33 S32 114.6(5) . . ? C33 C34 S31 128.1(7) . . ? C33 C34 S34 116.0(6) . . ? S31 C34 S34 115.9(5) . . ? C36 C35 S33 122.7(7) . . ? C36 C35 S34 122.2(7) . . ? S33 C35 S34 115.1(5) . . ? C35 C36 S36 123.3(7) . . ? C35 C36 S35 121.0(7) . . ? S36 C36 S35 115.7(5) . . ? C38 C37 S38 129.2(7) . . ? C38 C37 S35 116.7(6) . . ? S38 C37 S35 114.1(5) . . ? C37 C38 S36 116.7(6) . . ? C37 C38 S37 127.5(7) . . ? S36 C38 S37 115.8(5) . . ? C40 C39 S37 113.3(6) . . ? C40 C39 H39A 108.9 . . ? S37 C39 H39A 108.9 . . ? C40 C39 H39B 108.9 . . ? S37 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? C39 C40 S38 112.7(6) . . ? C39 C40 H40A 109.0 . . ? S38 C40 H40A 109.0 . . ? C39 C40 H40B 109.0 . . ? S38 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? C34 S31 C31 102.2(4) . . ? C33 S32 C32 101.8(4) . . ? C33 S33 C35 95.7(4) . . ? C35 S34 C34 95.9(4) . . ? C36 S35 C37 95.0(4) . . ? C36 S36 C38 95.5(4) . . ? C38 S37 C39 101.7(4) . . ? C37 S38 C40 101.3(4) . . ? C42 C41 S41 114.6(10) . . ? C42 C41 H41A 108.6 . . ? S41 C41 H41A 108.6 . . ? C42 C41 H41B 108.6 . . ? S41 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? C41 C42 S42 111.5(13) . . ? C41 C42 H42A 109.3 . . ? S42 C42 H42A 109.3 . . ? C41 C42 H42B 109.3 . . ? S42 C42 H42B 109.3 . . ? H42A C42 H42B 108.0 . . ? C44 C43 S43 116.9(6) . . ? C44 C43 S42 129.5(6) . . ? S43 C43 S42 113.6(5) . . ? C43 C44 S44 117.0(6) . . ? C43 C44 S41 127.3(6) . . ? S44 C44 S41 115.6(5) . . ? C45 C45 S44 122.1(9) 2_665 . ? C45 C45 S43 122.2(9) 2_665 . ? S44 C45 S43 115.7(4) . . ? C41 S41 C44 102.4(6) . . ? C44 S41 C46 97.8(7) . . ? C43 S42 C47 105.7(6) . . ? C43 S42 C42 97.3(6) . . ? C45 S43 C43 95.1(4) . . ? C45 S44 C44 95.2(4) . . ? C47 C46 S41 115.8(13) . . ? C47 C46 H46A 108.3 . . ? S41 C46 H46A 108.3 . . ? C47 C46 H46B 108.3 . . ? S41 C46 H46B 108.3 . . ? H46A C46 H46B 107.4 . . ? C46 C47 S42 112.3(14) . . ? C46 C47 H47A 109.2 . . ? S42 C47 H47A 109.2 . . ? C46 C47 H47B 109.2 . . ? S42 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? O54 C51 O51 127.3(8) . . ? O54 C51 C52 120.6(8) . . ? O51 C51 C52 112.0(7) . . ? O53 C52 O52 124.3(8) . . ? O53 C52 C51 119.0(8) . . ? O52 C52 C51 116.6(8) . . ? O58 C55 O55 127.0(8) . . ? O58 C55 C56 119.5(8) . . ? O55 C55 C56 113.5(7) . . ? O57 C56 O56 126.3(8) . . ? O57 C56 C55 118.7(8) . . ? O56 C56 C55 115.0(7) . . ? O62 C59 O59 127.6(8) . . ? O62 C59 C60 119.6(8) . . ? O59 C59 C60 112.8(7) . . ? O61 C60 O60 125.1(8) . . ? O61 C60 C59 120.2(8) . . ? O60 C60 C59 114.8(8) . . ? C51 O51 Fe1 117.6(5) . . ? C52 O52 Fe1 113.5(5) . . ? C52 O52 Na5 120.0(5) . . ? Fe1 O52 Na5 123.5(3) . . ? C52 O53 Na3 110.1(5) . . ? C51 O54 Na3 110.9(6) . . ? C55 O55 Fe1 113.8(5) . . ? C55 O55 Na6 111.7(5) . 2_666 ? Fe1 O55 Na6 127.7(3) . 2_666 ? C56 O56 Fe1 115.4(5) . . ? C56 O57 Na1 106.7(5) . . ? C55 O58 Na2 116.4(5) . . ? C55 O58 Na8 141.1(6) . 2_666 ? Na2 O58 Na8 100.7(2) . 2_666 ? C55 O58 Na1 99.1(5) . . ? Na2 O58 Na1 85.1(2) . . ? Na8 O58 Na1 95.2(2) 2_666 . ? C59 O59 Fe1 115.9(5) . . ? C60 O60 Fe1 114.8(5) . . ? C60 O61 Na4 116.6(6) . 1_455 ? C59 O62 Na4 115.1(6) . 1_455 ? O59 Fe1 O56 92.7(2) . . ? O59 Fe1 O51 94.5(2) . . ? O56 Fe1 O51 88.9(2) . . ? O59 Fe1 O60 81.4(2) . . ? O56 Fe1 O60 103.4(2) . . ? O51 Fe1 O60 167.2(2) . . ? O59 Fe1 O55 169.1(2) . . ? O56 Fe1 O55 81.4(2) . . ? O51 Fe1 O55 94.5(2) . . ? O60 Fe1 O55 91.0(2) . . ? O59 Fe1 O52 95.2(2) . . ? O56 Fe1 O52 166.6(2) . . ? O51 Fe1 O52 79.8(2) . . ? O60 Fe1 O52 88.5(2) . . ? O55 Fe1 O52 92.3(2) . . ? O66 C63 O63 127.1(8) . . ? O66 C63 C64 119.0(8) . . ? O63 C63 C64 113.9(8) . . ? O65 C64 O64 125.5(8) . . ? O65 C64 C63 120.2(8) . . ? O64 C64 C63 114.3(8) . . ? O70 C67 O67 125.5(8) . . ? O70 C67 C68 119.1(8) . . ? O67 C67 C68 115.3(7) . . ? O69 C68 O68 126.8(8) . . ? O69 C68 C67 120.4(8) . . ? O68 C68 C67 112.8(7) . . ? O74 C71 O71 125.8(8) . . ? O74 C71 C72 118.0(8) . . ? O71 C71 C72 116.2(8) . . ? O73 C72 O72 126.1(8) . . ? O73 C72 C71 120.3(8) . . ? O72 C72 C71 113.6(8) . . ? C63 O63 Fe2 116.4(5) . . ? C64 O64 Fe2 114.4(5) . . ? C64 O65 Na3 114.0(6) . . ? C63 O66 Na3 118.7(6) . . ? C67 O67 Fe2 113.8(5) . . ? C67 O67 Na7 123.5(5) . . ? Fe2 O67 Na7 120.5(3) . . ? C68 O68 Fe2 117.2(5) . . ? C68 O69 Na4 114.7(5) . 1_455 ? C67 O70 Na4 106.9(5) . 1_455 ? C71 O71 Fe2 114.7(5) . . ? C72 O72 Fe2 114.1(5) . . ? C72 O72 Na9 108.6(5) . . ? Fe2 O72 Na9 130.4(3) . . ? C72 O73 Na1 117.6(6) . 1_565 ? C72 O73 Na2 102.0(5) . 1_565 ? Na1 O73 Na2 88.0(2) 1_565 1_565 ? C72 O73 Na8 145.2(6) . 2_676 ? Na1 O73 Na8 95.7(2) 1_565 2_676 ? Na2 O73 Na8 88.3(2) 1_565 2_676 ? C71 O74 Na2 106.2(5) . 1_565 ? O63 Fe2 O68 93.7(2) . . ? O63 Fe2 O71 92.2(2) . . ? O68 Fe2 O71 90.1(2) . . ? O63 Fe2 O64 80.8(2) . . ? O68 Fe2 O64 167.4(2) . . ? O71 Fe2 O64 101.3(2) . . ? O63 Fe2 O72 168.9(2) . . ? O68 Fe2 O72 95.3(2) . . ? O71 Fe2 O72 81.4(2) . . ? O64 Fe2 O72 91.5(2) . . ? O63 Fe2 O67 95.9(2) . . ? O68 Fe2 O67 80.5(2) . . ? O71 Fe2 O67 168.0(2) . . ? O64 Fe2 O67 88.7(2) . . ? O72 Fe2 O67 92.0(2) . . ? O78 C75 O75 126.7(8) . . ? O78 C75 C76 119.8(8) . . ? O75 C75 C76 113.5(7) . . ? O77 C76 O76 124.1(8) . . ? O77 C76 C75 119.7(8) . . ? O76 C76 C75 116.2(7) . . ? O82 C79 O79 125.4(8) . . ? O82 C79 C80 118.9(8) . . ? O79 C79 C80 115.7(8) . . ? O81 C80 O80 125.2(8) . . ? O81 C80 C79 120.7(8) . . ? O80 C80 C79 114.0(8) . . ? O86 C83 O83 126.8(8) . . ? O86 C83 C84 120.1(8) . . ? O83 C83 C84 113.0(7) . . ? O85 C84 O84 126.1(8) . . ? O85 C84 C83 119.6(8) . . ? O84 C84 C83 114.2(8) . . ? C75 O75 Fe3 116.4(5) . . ? C76 O76 Fe3 113.1(5) . . ? C76 O76 Na9 121.3(5) . 2_676 ? Fe3 O76 Na9 123.5(3) . 2_676 ? C76 O77 Na1 113.2(5) . 1_665 ? C75 O78 Na1 112.0(6) . 1_665 ? C79 O79 Fe3 113.0(5) . . ? C79 O79 Na8 109.8(5) . . ? Fe3 O79 Na8 127.4(3) . . ? C80 O80 Fe3 115.8(5) . . ? C80 O81 Na3 109.2(5) . . ? C79 O82 Na4 112.0(5) . . ? C79 O82 Na6 143.7(6) . . ? Na4 O82 Na6 102.9(2) . . ? C79 O82 Na3 98.0(5) . . ? Na4 O82 Na3 83.3(2) . . ? Na6 O82 Na3 95.7(2) . . ? C83 O83 Fe3 115.1(5) . . ? C84 O84 Fe3 116.0(5) . . ? C84 O85 Na2 118.4(6) . 1_565 ? C83 O86 Na2 114.2(5) . 1_565 ? O84 Fe3 O80 94.7(3) . . ? O84 Fe3 O75 91.9(2) . . ? O80 Fe3 O75 90.5(2) . . ? O84 Fe3 O83 80.9(2) . . ? O80 Fe3 O83 101.7(2) . . ? O75 Fe3 O83 166.3(2) . . ? O84 Fe3 O76 95.6(2) . . ? O80 Fe3 O76 166.7(2) . . ? O75 Fe3 O76 80.8(2) . . ? O83 Fe3 O76 88.3(2) . . ? O84 Fe3 O79 168.7(2) . . ? O80 Fe3 O79 81.1(2) . . ? O75 Fe3 O79 98.6(2) . . ? O83 Fe3 O79 89.8(2) . . ? O76 Fe3 O79 90.3(2) . . ? O90 C87 O87 126.4(7) . . ? O90 C87 C88 119.6(7) . . ? O87 C87 C88 114.1(7) . . ? O89 C88 O88 126.6(7) . . ? O89 C88 C87 120.1(7) . . ? O88 C88 C87 113.2(7) . . ? O94 C91 O91 125.0(8) . . ? O94 C91 C92 121.2(9) . . ? O91 C91 C92 113.7(8) . . ? O93 C92 O92 125.6(8) . . ? O93 C92 C91 119.3(8) . . ? O92 C92 C91 115.0(8) . . ? O98 C95 O95 126.9(8) . . ? O98 C95 C96 118.3(8) . . ? O95 C95 C96 114.8(7) . . ? O97 C96 O96 127.2(8) . . ? O97 C96 C95 120.5(8) . . ? O96 C96 C95 112.3(8) . . ? C87 O87 Fe4 114.7(5) . . ? C87 O87 Na7 123.0(5) . . ? Fe4 O87 Na7 119.5(3) . . ? C88 O88 Fe4 117.2(5) . . ? C88 O89 Na2 112.3(5) . 2_666 ? C87 O90 Na2 108.9(5) . 2_666 ? C91 O91 Fe4 116.8(5) . . ? C92 O92 Fe4 113.8(5) . . ? C92 O92 Na5 102.9(5) . . ? Fe4 O92 Na5 133.6(3) . . ? C92 O93 Na3 116.6(5) . 2_666 ? C92 O93 Na4 102.5(5) . 2_666 ? Na3 O93 Na4 89.3(2) 2_666 2_666 ? C92 O93 Na6 148.9(5) . 2_666 ? Na3 O93 Na6 92.7(2) 2_666 2_666 ? Na4 O93 Na6 87.0(2) 2_666 2_666 ? C91 O94 Na4 106.3(5) . 2_666 ? C95 O95 Fe4 114.8(5) . . ? C96 O96 Fe4 116.5(5) . . ? C96 O97 Na1 116.3(5) . 2_566 ? C95 O98 Na1 114.6(5) . 2_566 ? O91 Fe4 O88 93.5(2) . . ? O91 Fe4 O96 91.1(2) . . ? O88 Fe4 O96 92.5(2) . . ? O91 Fe4 O95 99.3(2) . . ? O88 Fe4 O95 166.0(2) . . ? O96 Fe4 O95 81.5(2) . . ? O91 Fe4 O87 167.7(2) . . ? O88 Fe4 O87 80.7(2) . . ? O96 Fe4 O87 100.0(2) . . ? O95 Fe4 O87 87.8(2) . . ? O91 Fe4 O92 80.4(2) . . ? O88 Fe4 O92 97.3(2) . . ? O96 Fe4 O92 167.4(2) . . ? O95 Fe4 O92 90.6(2) . . ? O87 Fe4 O92 89.5(2) . . ? O57 Na1 O97 82.6(2) . 2_566 ? O57 Na1 O77 159.9(3) . 1_445 ? O97 Na1 O77 85.0(2) 2_566 1_445 ? O57 Na1 O73 110.1(2) . 1_545 ? O97 Na1 O73 163.9(3) 2_566 1_545 ? O77 Na1 O73 85.2(2) 1_445 1_545 ? O57 Na1 O78 123.6(2) . 1_445 ? O97 Na1 O78 79.4(2) 2_566 1_445 ? O77 Na1 O78 69.0(2) 1_445 1_445 ? O73 Na1 O78 85.2(2) 1_545 1_445 ? O57 Na1 O98 85.4(2) . 2_566 ? O97 Na1 O98 69.2(2) 2_566 2_566 ? O77 Na1 O98 75.4(2) 1_445 2_566 ? O73 Na1 O98 120.2(2) 1_545 2_566 ? O78 Na1 O98 134.0(2) 1_445 2_566 ? O57 Na1 O58 64.0(2) . . ? O97 Na1 O58 128.6(2) 2_566 . ? O77 Na1 O58 113.4(2) 1_445 . ? O73 Na1 O58 67.3(2) 1_545 . ? O78 Na1 O58 151.6(2) 1_445 . ? O98 Na1 O58 70.1(2) 2_566 . ? O89 Na2 O58 84.6(2) 2_666 . ? O89 Na2 O85 76.5(2) 2_666 1_545 ? O58 Na2 O85 158.4(3) . 1_545 ? O89 Na2 O74 118.6(2) 2_666 1_545 ? O58 Na2 O74 116.1(2) . 1_545 ? O85 Na2 O74 82.5(2) 1_545 1_545 ? O89 Na2 O90 69.2(2) 2_666 2_666 ? O58 Na2 O90 83.9(2) . 2_666 ? O85 Na2 O90 79.9(2) 1_545 2_666 ? O74 Na2 O90 158.3(3) 1_545 2_666 ? O89 Na2 O86 133.0(2) 2_666 1_545 ? O58 Na2 O86 121.8(2) . 1_545 ? O85 Na2 O86 67.5(2) 1_545 1_545 ? O74 Na2 O86 86.1(2) 1_545 1_545 ? O90 Na2 O86 75.5(2) 2_666 1_545 ? O89 Na2 O73 151.4(2) 2_666 1_545 ? O58 Na2 O73 69.9(2) . 1_545 ? O85 Na2 O73 130.8(2) 1_545 1_545 ? O74 Na2 O73 65.3(2) 1_545 1_545 ? O90 Na2 O73 118.6(2) 2_666 1_545 ? O86 Na2 O73 73.8(2) 1_545 1_545 ? O81 Na3 O54 123.2(3) . . ? O81 Na3 O53 158.6(3) . . ? O54 Na3 O53 71.0(2) . . ? O81 Na3 O93 108.7(2) . 2_666 ? O54 Na3 O93 82.1(2) . 2_666 ? O53 Na3 O93 88.2(2) . 2_666 ? O81 Na3 O66 87.4(2) . . ? O54 Na3 O66 80.2(2) . . ? O53 Na3 O66 79.1(2) . . ? O93 Na3 O66 160.8(3) 2_666 . ? O81 Na3 O65 85.0(2) . . ? O54 Na3 O65 136.5(2) . . ? O53 Na3 O65 74.6(2) . . ? O93 Na3 O65 122.8(2) 2_666 . ? O66 Na3 O65 67.7(2) . . ? O81 Na3 O82 64.6(2) . . ? O54 Na3 O82 150.1(2) . . ? O53 Na3 O82 112.2(2) . . ? O93 Na3 O82 68.6(2) 2_666 . ? O66 Na3 O82 129.6(2) . . ? O65 Na3 O82 68.9(2) . . ? O69 Na4 O94 121.4(2) 1_655 2_666 ? O69 Na4 O61 131.5(2) 1_655 1_655 ? O94 Na4 O61 85.7(2) 2_666 1_655 ? O69 Na4 O82 81.2(2) 1_655 . ? O94 Na4 O82 120.0(3) 2_666 . ? O61 Na4 O82 121.9(2) 1_655 . ? O69 Na4 O62 78.4(2) 1_655 1_655 ? O94 Na4 O62 78.0(2) 2_666 1_655 ? O61 Na4 O62 68.3(2) 1_655 1_655 ? O82 Na4 O62 158.2(3) . 1_655 ? O69 Na4 O70 68.2(2) 1_655 1_655 ? O94 Na4 O70 155.9(3) 2_666 1_655 ? O61 Na4 O70 73.5(2) 1_655 1_655 ? O82 Na4 O70 82.1(2) . 1_655 ? O62 Na4 O70 83.1(2) 1_655 1_655 ? O69 Na4 O93 150.5(3) 1_655 2_666 ? O94 Na4 O93 66.9(2) 2_666 2_666 ? O61 Na4 O93 74.4(2) 1_655 2_666 ? O82 Na4 O93 71.3(2) . 2_666 ? O62 Na4 O93 130.0(2) 1_655 2_666 ? O70 Na4 O93 116.9(2) 1_655 2_666 ? O69 Na4 C91 144.2(2) 1_655 2_666 ? O94 Na4 C91 23.0(2) 2_666 2_666 ? O61 Na4 C91 67.4(2) 1_655 2_666 ? O82 Na4 C91 116.7(3) . 2_666 ? O62 Na4 C91 84.7(3) 1_655 2_666 ? O70 Na4 C91 140.8(2) 1_655 2_666 ? O93 Na4 C91 50.1(2) 2_666 2_666 ? O105 Na5 O104 174.1(2) 2_666 . ? O105 Na5 O103 85.6(2) 2_666 . ? O104 Na5 O103 91.2(2) . . ? O105 Na5 O106 101.5(2) 2_666 . ? O104 Na5 O106 82.1(2) . . ? O103 Na5 O106 172.1(2) . . ? O105 Na5 O52 75.0(2) 2_666 . ? O104 Na5 O52 110.2(2) . . ? O103 Na5 O52 95.1(2) . . ? O106 Na5 O52 83.5(2) . . ? O105 Na5 O92 91.8(2) 2_666 . ? O104 Na5 O92 83.9(2) . . ? O103 Na5 O92 99.4(2) . . ? O106 Na5 O92 84.0(2) . . ? O52 Na5 O92 159.6(2) . . ? O107 Na6 O103 174.3(3) . 2_666 ? O107 Na6 O108 90.2(2) . . ? O103 Na6 O108 90.2(2) 2_666 . ? O107 Na6 O105 94.6(2) . . ? O103 Na6 O105 83.9(2) 2_666 . ? O108 Na6 O105 167.3(2) . . ? O107 Na6 O82 77.2(2) . . ? O103 Na6 O82 108.4(2) 2_666 . ? O108 Na6 O82 76.5(2) . . ? O105 Na6 O82 116.0(2) . . ? O107 Na6 O55 86.2(2) . 2_666 ? O103 Na6 O55 88.2(2) 2_666 2_666 ? O108 Na6 O55 85.2(2) . 2_666 ? O105 Na6 O55 83.4(2) . 2_666 ? O82 Na6 O55 155.1(2) . 2_666 ? O107 Na6 O93 115.5(2) . 2_666 ? O103 Na6 O93 68.7(2) 2_666 2_666 ? O108 Na6 O93 124.7(2) . 2_666 ? O105 Na6 O93 63.26(18) . 2_666 ? O82 Na6 O93 64.42(19) . 2_666 ? O55 Na6 O93 140.4(2) 2_666 2_666 ? O109 Na7 O106 177.6(3) . . ? O109 Na7 O110 82.8(2) . . ? O106 Na7 O110 96.6(2) . . ? O109 Na7 O104 98.4(2) . . ? O106 Na7 O104 82.2(2) . . ? O110 Na7 O104 178.6(3) . . ? O109 Na7 O67 76.5(2) . . ? O106 Na7 O67 101.3(2) . . ? O110 Na7 O67 96.7(2) . . ? O104 Na7 O67 83.0(2) . . ? O109 Na7 O87 103.4(2) . . ? O106 Na7 O87 78.8(2) . . ? O110 Na7 O87 82.8(2) . . ? O104 Na7 O87 97.5(2) . . ? O67 Na7 O87 179.5(3) . . ? O102 Na8 O108 169.8(3) . . ? O102 Na8 O107 88.9(2) . . ? O108 Na8 O107 89.9(2) . . ? O102 Na8 O101 84.4(2) . . ? O108 Na8 O101 94.2(2) . . ? O107 Na8 O101 164.5(2) . . ? O102 Na8 O58 112.1(2) . 2_666 ? O108 Na8 O58 77.5(2) . 2_666 ? O107 Na8 O58 76.0(2) . 2_666 ? O101 Na8 O58 119.4(2) . 2_666 ? O102 Na8 O73 73.2(2) . 2_676 ? O108 Na8 O73 115.4(2) . 2_676 ? O107 Na8 O73 125.8(2) . 2_676 ? O101 Na8 O73 65.3(2) . 2_676 ? O58 Na8 O73 65.3(2) 2_666 2_676 ? O102 Na8 O79 85.6(2) . . ? O108 Na8 O79 84.1(2) . . ? O107 Na8 O79 84.2(2) . . ? O101 Na8 O79 81.4(2) . . ? O58 Na8 O79 152.9(2) 2_666 . ? O73 Na8 O79 141.6(2) 2_676 . ? O101 Na9 O110 172.6(2) 2_676 . ? O101 Na9 O102 85.2(2) 2_676 2_676 ? O110 Na9 O102 91.8(2) . 2_676 ? O101 Na9 O109 100.1(2) 2_676 . ? O110 Na9 O109 83.0(2) . . ? O102 Na9 O109 174.5(3) 2_676 . ? O101 Na9 O76 77.4(2) 2_676 2_676 ? O110 Na9 O76 109.8(2) . 2_676 ? O102 Na9 O76 96.1(2) 2_676 2_676 ? O109 Na9 O76 84.0(2) . 2_676 ? O101 Na9 O72 86.7(2) 2_676 . ? O110 Na9 O72 86.7(2) . . ? O102 Na9 O72 95.1(2) 2_676 . ? O109 Na9 O72 86.4(2) . . ? O76 Na9 O72 159.7(2) 2_676 . ? Na9 O101 Na8 94.8(2) 2_676 . ? Na9 O101 H10C 112.8 2_676 . ? Na8 O101 H10C 112.8 . . ? Na9 O101 H10D 112.8 2_676 . ? Na8 O101 H10D 112.8 . . ? H10C O101 H10D 110.2 . . ? Na8 O102 Na9 95.6(2) . 2_676 ? Na8 O102 H10E 112.6 . . ? Na9 O102 H10E 112.6 2_676 . ? Na8 O102 H10F 112.6 . . ? Na9 O102 H10F 112.6 2_676 . ? H10E O102 H10F 110.1 . . ? Na5 O103 Na6 95.4(2) . 2_666 ? Na5 O103 H10G 112.7 . . ? Na6 O103 H10G 112.7 2_666 . ? Na5 O103 H10H 112.7 . . ? Na6 O103 H10H 112.7 2_666 . ? H10G O103 H10H 110.2 . . ? Na5 O104 Na7 97.5(2) . . ? Na5 O104 H10I 112.3 . . ? Na7 O104 H10I 112.3 . . ? Na5 O104 H10J 112.3 . . ? Na7 O104 H10J 112.3 . . ? H10I O104 H10J 109.9 . . ? Na5 O105 Na6 95.1(2) 2_666 . ? Na5 O105 H10K 112.7 2_666 . ? Na6 O105 H10K 112.7 . . ? Na5 O105 H10L 112.7 2_666 . ? Na6 O105 H10L 112.7 . . ? H10K O105 H10L 110.2 . . ? Na7 O106 Na5 97.7(2) . . ? Na7 O106 H10M 112.2 . . ? Na5 O106 H10M 112.2 . . ? Na7 O106 H10N 112.2 . . ? Na5 O106 H10N 112.2 . . ? H10M O106 H10N 109.8 . . ? Na6 O107 Na8 90.2(2) . . ? Na6 O107 H10O 113.6 . . ? Na8 O107 H10O 113.6 . . ? Na6 O107 H10P 113.6 . . ? Na8 O107 H10P 113.6 . . ? H10O O107 H10P 110.9 . . ? Na8 O108 Na6 89.7(2) . . ? Na8 O108 H10Q 113.7 . . ? Na6 O108 H10Q 113.7 . . ? Na8 O108 H10R 113.7 . . ? Na6 O108 H10R 113.7 . . ? H10Q O108 H10R 110.9 . . ? Na7 O109 Na9 97.4(2) . . ? Na7 O109 H10S 112.3 . . ? Na9 O109 H10S 112.3 . . ? Na7 O109 H10T 112.3 . . ? Na9 O109 H10T 112.3 . . ? H10S O109 H10T 109.9 . . ? Na9 O110 Na7 96.3(2) . . ? Na9 O110 H11C 112.5 . . ? Na7 O110 H11C 112.5 . . ? Na9 O110 H11D 112.5 . . ? Na7 O110 H11D 112.5 . . ? H11C O110 H11D 110.0 . . ? H111 O111 H112 107.2 . . ? H121 O121 H122 108.0 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.718 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.149 data_II _database_code_depnum_ccdc_archive 'CCDC 637272' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2.5 C 10 H 8 S 8 0.6+, 1.5 C 12 H 24 O 6, 1.5 K +, C 6 Fe O 12 3-, 6 H 2 O' _chemical_formula_sum 'C49 H68 Fe K1.50 O27 S20' _chemical_formula_weight 1844.73 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' 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' K K 0.2009 0.2494 '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 32.9933(11) _cell_length_b 11.0441(4) _cell_length_c 20.7262(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.622(1) _cell_angle_gamma 90.00 _cell_volume 7307.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9182 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.62 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3810 _exptl_absorpt_coefficient_mu 0.941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6712 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX2 CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_reflns_number 79494 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.64 _reflns_number_total 22106 _reflns_number_gt 16946 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+5.4225P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22106 _refine_ls_number_parameters 1046 _refine_ls_number_restraints 1448 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _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 K1 K -0.15044(3) 0.27781(6) 0.90542(3) 0.0585(2) Uani 1 1 d . A . K2 K 0.00869(3) 0.19677(10) 0.77609(5) 0.0287(2) Uani 0.50 1 d P . . O1 O -0.12263(6) 0.47656(19) 0.98980(10) 0.0451(5) Uani 1 1 d DU . . C1 C -0.09391(10) 0.4459(3) 1.04892(17) 0.0612(9) Uani 1 1 d DU A . H1A H -0.0887 0.5168 1.0791 0.073 Uiso 1 1 calc R . . H1B H -0.0670 0.4220 1.0396 0.073 Uiso 1 1 calc R . . C2 C -0.11043(11) 0.3445(3) 1.08132(14) 0.0616(10) Uani 1 1 d DU . . H2A H -0.0911 0.3279 1.1254 0.074 Uiso 1 1 calc R A . H2B H -0.1380 0.3670 1.0884 0.074 Uiso 1 1 calc R . . O2 O -0.11474(6) 0.2372(2) 1.04044(9) 0.0456(5) Uani 1 1 d DU A . C3 C -0.13666(11) 0.1430(3) 1.06293(15) 0.0599(9) Uani 1 1 d DU . . H3A H -0.1661 0.1675 1.0582 0.072 Uiso 1 1 calc R A . H3B H -0.1237 0.1266 1.1107 0.072 Uiso 1 1 calc R . . C4 C -0.13533(10) 0.0320(3) 1.02324(16) 0.0558(9) Uani 1 1 d DU A . H4A H -0.1059 0.0115 1.0248 0.067 Uiso 1 1 calc R . . H4B H -0.1477 -0.0366 1.0424 0.067 Uiso 1 1 calc R . . O3 O -0.15841(6) 0.05125(18) 0.95517(11) 0.0456(5) Uani 1 1 d DU . . C5 C -0.15761(11) -0.0520(3) 0.91536(19) 0.0571(9) Uani 1 1 d DU A . H5A H -0.1720 -0.1203 0.9312 0.069 Uiso 1 1 calc R . . H5B H -0.1283 -0.0761 0.9186 0.069 Uiso 1 1 calc R . . C6 C -0.17919(11) -0.0229(3) 0.84469(18) 0.0563(8) Uani 1 1 d DU . . H6A H -0.1803 -0.0960 0.8166 0.068 Uiso 1 1 calc R A . H6B H -0.2082 0.0037 0.8417 0.068 Uiso 1 1 calc R . . O4 O -0.15665(6) 0.07139(18) 0.82133(11) 0.0445(5) Uani 1 1 d DU A . C7 C -0.1729(7) 0.0888(12) 0.7528(6) 0.053(4) Uani 0.40(2) 1 d PDU A 1 H7A H -0.2037 0.0984 0.7423 0.063 Uiso 0.40(2) 1 calc PR A 1 H7B H -0.1663 0.0185 0.7277 0.063 Uiso 0.40(2) 1 calc PR A 1 C8 C -0.1532(6) 0.1997(9) 0.7347(8) 0.058(4) Uani 0.40(2) 1 d PDU A 1 H8A H -0.1225 0.1885 0.7462 0.070 Uiso 0.40(2) 1 calc PR A 1 H8B H -0.1628 0.2118 0.6859 0.070 Uiso 0.40(2) 1 calc PR A 1 O5 O -0.16311(6) 0.3083(2) 0.76843(9) 0.0446(5) Uani 1 1 d DU . . C9 C -0.1546(4) 0.4162(8) 0.7388(5) 0.025(2) Uani 0.40(2) 1 d PDU A 1 H9A H -0.1729 0.4246 0.6931 0.029 Uiso 0.40(2) 1 calc PR A 1 H9B H -0.1250 0.4193 0.7367 0.029 Uiso 0.40(2) 1 calc PR A 1 C10 C -0.1637(4) 0.5126(11) 0.7836(4) 0.029(2) Uani 0.40(2) 1 d PDU A 1 H10A H -0.1609 0.5930 0.7641 0.035 Uiso 0.40(2) 1 calc PR A 1 H10B H -0.1930 0.5041 0.7870 0.035 Uiso 0.40(2) 1 calc PR A 1 O6 O -0.13479(6) 0.50517(17) 0.85167(10) 0.0434(5) Uani 1 1 d DU . . C11 C -0.1447(4) 0.6033(10) 0.8885(4) 0.025(2) Uani 0.40(2) 1 d PDU A 1 H11A H -0.1742 0.5995 0.8907 0.030 Uiso 0.40(2) 1 calc PR A 1 H11B H -0.1397 0.6815 0.8684 0.030 Uiso 0.40(2) 1 calc PR A 1 C12 C -0.1160(4) 0.5883(11) 0.9552(5) 0.032(2) Uani 0.40(2) 1 d PDU A 1 H12A H -0.0868 0.5891 0.9508 0.038 Uiso 0.40(2) 1 calc PR A 1 H12B H -0.1194 0.6585 0.9831 0.038 Uiso 0.40(2) 1 calc PR A 1 C7A C -0.1747(4) 0.1033(11) 0.7536(4) 0.065(3) Uani 0.60(2) 1 d PDU A 2 H7AA H -0.2047 0.1221 0.7477 0.077 Uiso 0.60(2) 1 calc PR A 2 H7AB H -0.1726 0.0336 0.7246 0.077 Uiso 0.60(2) 1 calc PR A 2 C8A C -0.1534(3) 0.2097(8) 0.7329(5) 0.056(2) Uani 0.60(2) 1 d PDU A 2 H8AA H -0.1227 0.1968 0.7438 0.067 Uiso 0.60(2) 1 calc PR A 2 H8AB H -0.1636 0.2236 0.6843 0.067 Uiso 0.60(2) 1 calc PR A 2 C9A C -0.1480(4) 0.4220(9) 0.7488(6) 0.067(3) Uani 0.60(2) 1 d PDU A 2 H9AA H -0.1609 0.4360 0.7008 0.081 Uiso 0.60(2) 1 calc PR A 2 H9AB H -0.1173 0.4167 0.7550 0.081 Uiso 0.60(2) 1 calc PR A 2 C10A C -0.1575(4) 0.5257(10) 0.7874(5) 0.076(3) Uani 0.60(2) 1 d PDU A 2 H10C H -0.1490 0.6028 0.7703 0.091 Uiso 0.60(2) 1 calc PR A 2 H10D H -0.1879 0.5293 0.7849 0.091 Uiso 0.60(2) 1 calc PR A 2 C11A C -0.1336(5) 0.5998(9) 0.8985(6) 0.071(3) Uani 0.60(2) 1 d PDU A 2 H11C H -0.1621 0.6120 0.9045 0.085 Uiso 0.60(2) 1 calc PR A 2 H11D H -0.1251 0.6757 0.8801 0.085 Uiso 0.60(2) 1 calc PR A 2 C12A C -0.1051(4) 0.5771(10) 0.9629(6) 0.067(3) Uani 0.60(2) 1 d PDU A 2 H12C H -0.0768 0.5573 0.9581 0.080 Uiso 0.60(2) 1 calc PR A 2 H12D H -0.1032 0.6488 0.9922 0.080 Uiso 0.60(2) 1 calc PR A 2 O7 O -0.02604(11) 0.2525(3) 0.88482(18) 0.0368(8) Uani 0.50 1 d PDU A -1 C13 C -0.03772(19) 0.1545(5) 0.9202(3) 0.0392(12) Uani 0.50 1 d PDU A -1 H13A H -0.0651 0.1216 0.8952 0.047 Uiso 0.50 1 calc PR A -1 H13B H -0.0404 0.1823 0.9643 0.047 Uiso 0.50 1 calc PR A -1 C14 C -0.00533(18) 0.0602(5) 0.9286(2) 0.0383(11) Uani 0.50 1 d PDU A -1 H14A H 0.0228 0.0964 0.9451 0.046 Uiso 0.50 1 calc PR A -1 H14B H -0.0094 -0.0010 0.9614 0.046 Uiso 0.50 1 calc PR A -1 O8 O -0.00895(11) 0.0042(3) 0.86467(17) 0.0356(8) Uani 0.50 1 d PDU A -1 C15 C 0.02454(18) -0.0795(5) 0.8657(3) 0.0419(12) Uani 0.50 1 d PDU A -1 H15A H 0.0252 -0.1430 0.8997 0.050 Uiso 0.50 1 calc PR A -1 H15B H 0.0518 -0.0366 0.8769 0.050 Uiso 0.50 1 calc PR A -1 C16 C 0.01684(19) -0.1354(5) 0.7978(3) 0.0413(12) Uani 0.50 1 d PDU . -1 H16A H 0.0360 -0.2048 0.7988 0.050 Uiso 0.50 1 calc PR . -1 H16B H -0.0123 -0.1655 0.7834 0.050 Uiso 0.50 1 calc PR . -1 O9 O 0.02391(14) -0.0455(4) 0.7519(2) 0.0376(9) Uani 0.50 1 d PDU . -1 C17 C 0.0107(2) -0.0854(5) 0.6847(3) 0.0427(12) Uani 0.50 1 d PDU . -1 H17A H -0.0202 -0.0954 0.6719 0.051 Uiso 0.50 1 calc PR . -1 H17B H 0.0235 -0.1649 0.6800 0.051 Uiso 0.50 1 calc PR . -1 C18 C 0.0232(2) 0.0046(6) 0.6399(3) 0.0454(15) Uani 0.50 1 d PDU A -1 H18A H 0.0539 0.0174 0.6541 0.054 Uiso 0.50 1 calc PR A -1 H18B H 0.0162 -0.0268 0.5937 0.054 Uiso 0.50 1 calc PR A -1 O10 O 0.00214(11) 0.1172(3) 0.64185(17) 0.0361(8) Uani 0.50 1 d PDU A -1 C19 C 0.01835(17) 0.2106(5) 0.6081(2) 0.0387(11) Uani 0.50 1 d PDU A -1 H19A H 0.0169 0.1849 0.5618 0.046 Uiso 0.50 1 calc PR A -1 H19B H 0.0481 0.2255 0.6309 0.046 Uiso 0.50 1 calc PR A -1 C20 C -0.00598(17) 0.3234(5) 0.6072(2) 0.0386(11) Uani 0.50 1 d PDU A -1 H20A H 0.0046 0.3868 0.5819 0.046 Uiso 0.50 1 calc PR A -1 H20B H -0.0358 0.3086 0.5850 0.046 Uiso 0.50 1 calc PR A -1 O11 O -0.00199(12) 0.3629(3) 0.67375(17) 0.0345(8) Uani 0.50 1 d PDU A -1 C21 C -0.02251(17) 0.4754(5) 0.6764(3) 0.0388(12) Uani 0.50 1 d PDU . -1 H21A H -0.0528 0.4674 0.6552 0.047 Uiso 0.50 1 calc PR . -1 H21B H -0.0108 0.5382 0.6521 0.047 Uiso 0.50 1 calc PR . -1 C22 C -0.0160(2) 0.5109(6) 0.7474(3) 0.0361(13) Uani 0.50 1 d PDU . -1 H22A H 0.0144 0.5168 0.7690 0.043 Uiso 0.50 1 calc PR . -1 H22B H -0.0289 0.5907 0.7505 0.043 Uiso 0.50 1 calc PR . -1 O12 O -0.03489(12) 0.4203(3) 0.7799(2) 0.0351(8) Uani 0.50 1 d PDU A -1 C23 C -0.0357(2) 0.4555(6) 0.8457(3) 0.0397(13) Uani 0.50 1 d PDU A -1 H23A H -0.0531 0.5290 0.8442 0.048 Uiso 0.50 1 calc PR A -1 H23B H -0.0069 0.4738 0.8723 0.048 Uiso 0.50 1 calc PR A -1 C24 C -0.05380(17) 0.3523(5) 0.8767(3) 0.0389(11) Uani 0.50 1 d PDU A -1 H24A H -0.0578 0.3773 0.9206 0.047 Uiso 0.50 1 calc PR A -1 H24B H -0.0814 0.3292 0.8477 0.047 Uiso 0.50 1 calc PR A -1 S1 S 0.634442(16) 0.34987(5) 0.97987(3) 0.02067(10) Uani 1 1 d . . . S2 S 0.644469(15) 0.63910(5) 1.05461(3) 0.01990(10) Uani 1 1 d . . . S3 S 0.545319(15) 0.38059(4) 0.97220(3) 0.01967(10) Uani 1 1 d . . . S4 S 0.553338(15) 0.61972(4) 1.03674(3) 0.01916(10) Uani 1 1 d . . . C25 C 0.68149(6) 0.42549(18) 1.02516(11) 0.0212(4) Uani 1 1 d U . . H25A H 0.6861 0.4069 1.0732 0.025 Uiso 1 1 calc R . . H25B H 0.7056 0.3924 1.0104 0.025 Uiso 1 1 calc R . . C26 C 0.68068(6) 0.56149(18) 1.01641(11) 0.0206(4) Uani 1 1 d U . . H26A H 0.6732 0.5801 0.9681 0.025 Uiso 1 1 calc R . . H26B H 0.7092 0.5935 1.0357 0.025 Uiso 1 1 calc R . . C27 C 0.59581(6) 0.44118(17) 0.99823(9) 0.0161(3) Uani 1 1 d U . . C28 C 0.59941(6) 0.55203(17) 1.02691(9) 0.0158(3) Uani 1 1 d U . . C29 C 0.52098(6) 0.50013(17) 1.00165(9) 0.0162(3) Uani 1 1 d . . . S5 S 0.614721(16) 0.35796(5) 0.77666(3) 0.02060(10) Uani 1 1 d . . . S6 S 0.623796(15) 0.65264(5) 0.84492(3) 0.01959(10) Uani 1 1 d . . . S7 S 0.526061(15) 0.38284(4) 0.77602(3) 0.01938(10) Uani 1 1 d . . . S8 S 0.533988(15) 0.62540(4) 0.83565(3) 0.01962(10) Uani 1 1 d . . . S9 S 0.426661(15) 0.38744(4) 0.76211(2) 0.01766(9) Uani 1 1 d . . . S10 S 0.434750(15) 0.62368(4) 0.82888(3) 0.01871(10) Uani 1 1 d . . . S11 S 0.334713(15) 0.37219(4) 0.73756(3) 0.02013(10) Uani 1 1 d . . . S12 S 0.344928(16) 0.65655(5) 0.81752(3) 0.02226(11) Uani 1 1 d . . . C30 C 0.66124(6) 0.43427(18) 0.82370(10) 0.0192(4) Uani 1 1 d U . . H30A H 0.6641 0.4198 0.8718 0.023 Uiso 1 1 calc R . . H30B H 0.6860 0.3982 0.8121 0.023 Uiso 1 1 calc R . . C31 C 0.66128(6) 0.56959(18) 0.81162(10) 0.0191(4) Uani 1 1 d U . . H31A H 0.6551 0.5843 0.7630 0.023 Uiso 1 1 calc R . . H31B H 0.6897 0.6015 0.8319 0.023 Uiso 1 1 calc R . . C32 C 0.57577(6) 0.44867(17) 0.79478(9) 0.0165(3) Uani 1 1 d U . . C33 C 0.57943(6) 0.56126(17) 0.82140(9) 0.0160(3) Uani 1 1 d U . . C34 C 0.50132(6) 0.50526(17) 0.80229(9) 0.0167(3) Uani 1 1 d U . . C35 C 0.45914(6) 0.50584(17) 0.79804(9) 0.0168(3) Uani 1 1 d U . . C36 C 0.38022(6) 0.45496(17) 0.77046(9) 0.0161(3) Uani 1 1 d U . . C37 C 0.38408(6) 0.56482(17) 0.80104(10) 0.0169(3) Uani 1 1 d U . . C38 C 0.29794(6) 0.44877(18) 0.77535(10) 0.0191(4) Uani 1 1 d U . . H38A H 0.2694 0.4182 0.7546 0.023 Uiso 1 1 calc R . . H38B H 0.3046 0.4278 0.8233 0.023 Uiso 1 1 calc R . . C39 C 0.29790(6) 0.58508(18) 0.76860(10) 0.0195(4) Uani 1 1 d U . . H39A H 0.2735 0.6182 0.7824 0.023 Uiso 1 1 calc R . . H39B H 0.2945 0.6061 0.7211 0.023 Uiso 1 1 calc R . . S13 S 0.593233(16) 0.36667(5) 0.56553(3) 0.02033(10) Uani 1 1 d . . . S14 S 0.602125(16) 0.65245(5) 0.64430(3) 0.02031(10) Uani 1 1 d . . . S15 S 0.505135(15) 0.38176(4) 0.57187(3) 0.01891(10) Uani 1 1 d . . . S16 S 0.512746(15) 0.61983(4) 0.63661(3) 0.01909(10) Uani 1 1 d . . . S17 S 0.406467(15) 0.37671(4) 0.56628(2) 0.01748(9) Uani 1 1 d . . . S18 S 0.412921(15) 0.61793(4) 0.62662(2) 0.01819(9) Uani 1 1 d . . . S19 S 0.314461(15) 0.35767(4) 0.53927(3) 0.01914(10) Uani 1 1 d . . . S20 S 0.321491(15) 0.65216(4) 0.60681(3) 0.01877(10) Uani 1 1 d . . . C40 C 0.63979(6) 0.43747(18) 0.61715(10) 0.0196(4) Uani 1 1 d U . . H40A H 0.6420 0.4163 0.6643 0.024 Uiso 1 1 calc R . . H40B H 0.6647 0.4039 0.6050 0.024 Uiso 1 1 calc R . . C41 C 0.64030(6) 0.57378(18) 0.61074(10) 0.0196(4) Uani 1 1 d U . . H41A H 0.6354 0.5947 0.5629 0.024 Uiso 1 1 calc R . . H41B H 0.6686 0.6035 0.6338 0.024 Uiso 1 1 calc R . . C42 C 0.55438(6) 0.45061(17) 0.58885(9) 0.0167(3) Uani 1 1 d U . . C43 C 0.55785(6) 0.56085(17) 0.61853(9) 0.0166(3) Uani 1 1 d U . . C44 C 0.48024(6) 0.50043(17) 0.60166(9) 0.0162(3) Uani 1 1 d U . . C45 C 0.43830(6) 0.49862(17) 0.59870(9) 0.0169(3) Uani 1 1 d U . . C46 C 0.35913(6) 0.44540(17) 0.57058(9) 0.0160(3) Uani 1 1 d U . . C47 C 0.36232(6) 0.55834(17) 0.59754(9) 0.0162(3) Uani 1 1 d U . . C48 C 0.27393(6) 0.44720(18) 0.56136(10) 0.0197(4) Uani 1 1 d U . . H48A H 0.2462 0.4181 0.5353 0.024 Uiso 1 1 calc R . . H48B H 0.2754 0.4345 0.6092 0.024 Uiso 1 1 calc R . . C49 C 0.27743(6) 0.58154(19) 0.54879(10) 0.0210(4) Uani 1 1 d U . . H49A H 0.2513 0.6221 0.5522 0.025 Uiso 1 1 calc R . . H49B H 0.2803 0.5934 0.5028 0.025 Uiso 1 1 calc R . . Fe Fe 0.192330(10) 0.29447(3) 0.899400(15) 0.02142(7) Uani 1 1 d . A . O51 O 0.19530(5) 0.47500(14) 0.90651(8) 0.0272(3) Uani 1 1 d U . . O52 O 0.22326(5) 0.31126(14) 0.99643(7) 0.0250(3) Uani 1 1 d U . . O53 O 0.24433(5) 0.44971(15) 1.07634(8) 0.0303(4) Uani 1 1 d U . . O54 O 0.21885(6) 0.62514(15) 0.97838(9) 0.0330(4) Uani 1 1 d U . . O55 O 0.13913(5) 0.26207(15) 0.92440(8) 0.0279(3) Uani 1 1 d U . . O56 O 0.15299(5) 0.29280(16) 0.80823(8) 0.0299(4) Uani 1 1 d U . . O57 O 0.07199(6) 0.21604(19) 0.88112(10) 0.0410(4) Uani 1 1 d U A . O58 O 0.08650(6) 0.2527(2) 0.75583(10) 0.0553(6) Uani 1 1 d U A . O59 O 0.20683(5) 0.11619(14) 0.90739(8) 0.0263(3) Uani 1 1 d U . . O60 O 0.23982(5) 0.29228(14) 0.85387(8) 0.0259(3) Uani 1 1 d U . . O61 O 0.25255(6) -0.01526(16) 0.88369(9) 0.0386(4) Uani 1 1 d U . . O62 O 0.26883(5) 0.15862(16) 0.79707(8) 0.0305(4) Uani 1 1 d U . . C50 C 0.21263(7) 0.5180(2) 0.96416(11) 0.0242(4) Uani 1 1 d U . . C51 C 0.22816(6) 0.4197(2) 1.01864(11) 0.0225(4) Uani 1 1 d U . . C52 C 0.10669(7) 0.2446(2) 0.87595(12) 0.0270(4) Uani 1 1 d U A . C53 C 0.11516(8) 0.2644(2) 0.80632(12) 0.0320(5) Uani 1 1 d U A . C54 C 0.23569(7) 0.0844(2) 0.87996(11) 0.0255(4) Uani 1 1 d U A . C55 C 0.24962(7) 0.1858(2) 0.83921(11) 0.0240(4) Uani 1 1 d U A . O63 O 0.26692(6) -0.10683(18) 0.75828(10) 0.0418(5) Uani 1 1 d . . . O64 O 0.24910(7) -0.25873(17) 0.87332(9) 0.0406(4) Uani 1 1 d . . . O65 O 0.24622(5) 0.25433(15) 0.66526(8) 0.0306(4) Uani 1 1 d . . . O66 O -0.23685(7) 0.30331(17) 0.87483(10) 0.0437(5) Uani 1 1 d . . . O67 O 0.06651(14) 0.3135(4) 0.62020(19) 0.0475(10) Uani 0.50 1 d PU . . O68 O 0.02637(15) 0.2132(5) 0.9793(2) 0.0668(15) Uani 0.50 1 d P . . O69 O -0.07755(16) 0.0000(7) 0.8156(4) 0.125(3) Uani 0.50 1 d P . . O70 O -0.06026(16) 0.1945(5) 0.9079(3) 0.0662(13) Uani 0.50 1 d PU . . 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 K1 0.1085(6) 0.0356(3) 0.0236(3) 0.0048(2) 0.0021(3) -0.0264(4) K2 0.0256(5) 0.0347(5) 0.0257(5) -0.0011(4) 0.0064(4) 0.0000(4) O1 0.0374(10) 0.0490(12) 0.0518(12) -0.0171(9) 0.0163(9) -0.0055(9) C1 0.0391(16) 0.080(2) 0.060(2) -0.0387(18) 0.0042(15) 0.0068(16) C2 0.056(2) 0.098(3) 0.0225(13) -0.0141(14) -0.0046(12) 0.0454(18) O2 0.0396(11) 0.0721(14) 0.0264(9) 0.0015(9) 0.0107(8) 0.0182(10) C3 0.057(2) 0.092(3) 0.0389(16) 0.0311(16) 0.0273(15) 0.0348(18) C4 0.0455(17) 0.062(2) 0.066(2) 0.0448(16) 0.0251(15) 0.0189(15) O3 0.0430(11) 0.0352(10) 0.0623(13) 0.0179(9) 0.0201(10) 0.0067(8) C5 0.0496(18) 0.0311(15) 0.095(3) 0.0087(16) 0.0268(18) 0.0005(13) C6 0.0541(19) 0.0348(16) 0.087(2) -0.0152(15) 0.0310(18) -0.0144(14) O4 0.0379(10) 0.0406(11) 0.0592(12) -0.0131(9) 0.0201(9) -0.0058(8) C7 0.070(9) 0.038(5) 0.051(6) -0.022(4) 0.017(6) -0.002(5) C8 0.092(10) 0.044(5) 0.036(8) -0.006(5) 0.013(7) 0.015(6) O5 0.0388(10) 0.0680(14) 0.0294(9) 0.0058(9) 0.0130(8) -0.0078(10) C9 0.017(4) 0.042(4) 0.016(3) 0.008(3) 0.006(3) 0.001(3) C10 0.025(4) 0.037(4) 0.029(4) 0.004(4) 0.014(3) -0.003(3) O6 0.0471(11) 0.0308(10) 0.0614(13) 0.0056(9) 0.0307(10) 0.0027(8) C11 0.026(4) 0.019(3) 0.040(4) 0.002(2) 0.025(3) 0.007(3) C12 0.020(5) 0.033(4) 0.051(4) -0.011(3) 0.024(3) -0.004(3) C7A 0.052(5) 0.106(7) 0.042(4) -0.037(4) 0.023(4) -0.043(5) C8A 0.034(4) 0.118(6) 0.021(4) -0.018(4) 0.015(3) -0.030(4) C9A 0.047(6) 0.108(5) 0.041(4) 0.045(4) -0.001(4) 0.005(4) C10A 0.062(6) 0.068(4) 0.099(5) 0.069(4) 0.024(4) 0.019(4) C11A 0.068(8) 0.039(4) 0.130(6) 0.003(4) 0.067(5) -0.004(4) C12A 0.053(6) 0.060(5) 0.110(5) -0.056(4) 0.064(4) -0.033(4) O7 0.0363(19) 0.043(2) 0.0352(19) 0.0030(15) 0.0161(16) 0.0066(15) C13 0.037(3) 0.052(3) 0.030(3) 0.006(2) 0.010(2) 0.003(2) C14 0.050(3) 0.040(3) 0.026(2) 0.003(2) 0.011(2) -0.002(2) O8 0.0355(19) 0.037(2) 0.0348(19) 0.0010(15) 0.0104(15) 0.0008(15) C15 0.042(3) 0.041(3) 0.042(3) 0.007(2) 0.008(2) 0.005(2) C16 0.041(3) 0.032(3) 0.054(3) 0.000(2) 0.017(3) 0.004(2) O9 0.033(2) 0.040(3) 0.041(2) -0.007(2) 0.0126(18) -0.001(2) C17 0.043(3) 0.041(3) 0.042(3) -0.015(2) 0.006(3) 0.001(2) C18 0.044(4) 0.059(4) 0.032(3) -0.010(3) 0.008(3) 0.014(3) O10 0.0294(18) 0.050(2) 0.0294(17) -0.0053(15) 0.0084(14) 0.0033(15) C19 0.035(3) 0.058(3) 0.024(2) -0.002(2) 0.008(2) 0.003(2) C20 0.035(3) 0.055(3) 0.025(2) 0.003(2) 0.006(2) -0.001(2) O11 0.034(2) 0.043(2) 0.0258(17) 0.0062(15) 0.0069(15) 0.0057(16) C21 0.035(3) 0.044(3) 0.038(3) 0.012(2) 0.011(2) 0.006(2) C22 0.030(3) 0.037(3) 0.044(3) 0.005(3) 0.015(2) 0.002(3) O12 0.036(2) 0.038(2) 0.035(2) -0.0042(16) 0.0160(18) 0.0044(16) C23 0.043(4) 0.042(3) 0.038(3) -0.007(2) 0.017(3) 0.006(3) C24 0.038(3) 0.047(3) 0.036(3) -0.004(2) 0.019(2) 0.007(2) S1 0.0183(2) 0.0169(2) 0.0298(3) -0.00568(19) 0.0117(2) -0.00176(17) S2 0.0157(2) 0.0181(2) 0.0270(2) -0.00656(18) 0.00751(19) -0.00278(17) S3 0.0153(2) 0.0164(2) 0.0271(2) -0.00428(18) 0.00478(18) -0.00109(17) S4 0.0146(2) 0.0157(2) 0.0272(2) -0.00382(18) 0.00537(18) 0.00005(16) C25 0.0182(9) 0.0196(9) 0.0257(10) -0.0003(8) 0.0056(8) 0.0003(7) C26 0.0174(9) 0.0202(9) 0.0264(10) -0.0016(8) 0.0096(8) -0.0018(7) C27 0.0157(8) 0.0155(8) 0.0182(8) -0.0007(7) 0.0067(7) -0.0005(7) C28 0.0141(8) 0.0167(9) 0.0176(8) -0.0008(7) 0.0057(7) -0.0007(7) C29 0.0145(9) 0.0164(9) 0.0173(8) 0.0000(7) 0.0032(7) 0.0001(7) S5 0.0195(2) 0.0184(2) 0.0260(2) -0.00424(18) 0.00973(19) -0.00011(17) S6 0.0162(2) 0.0176(2) 0.0250(2) -0.00400(18) 0.00548(18) -0.00244(17) S7 0.0169(2) 0.0160(2) 0.0257(2) -0.00364(18) 0.00620(18) -0.00218(17) S8 0.0161(2) 0.0166(2) 0.0271(2) -0.00406(18) 0.00720(19) -0.00095(17) S9 0.0156(2) 0.0154(2) 0.0225(2) -0.00235(17) 0.00582(18) -0.00101(16) S10 0.0162(2) 0.0165(2) 0.0237(2) -0.00366(17) 0.00552(18) -0.00166(17) S11 0.0158(2) 0.0170(2) 0.0277(2) -0.00625(18) 0.00582(19) -0.00186(17) S12 0.0182(2) 0.0173(2) 0.0338(3) -0.00808(19) 0.0111(2) -0.00267(17) C30 0.0171(9) 0.0180(9) 0.0226(9) 0.0042(7) 0.0049(7) 0.0007(7) C31 0.0181(9) 0.0183(9) 0.0220(9) 0.0031(7) 0.0074(7) -0.0003(7) C32 0.0152(8) 0.0173(9) 0.0177(8) -0.0007(7) 0.0054(7) -0.0009(7) C33 0.0141(8) 0.0164(9) 0.0176(8) -0.0007(7) 0.0044(7) -0.0010(6) C34 0.0158(9) 0.0160(9) 0.0183(9) -0.0011(7) 0.0042(7) -0.0012(7) C35 0.0178(9) 0.0161(9) 0.0165(8) 0.0009(7) 0.0047(7) -0.0002(7) C36 0.0149(8) 0.0157(8) 0.0179(8) 0.0000(7) 0.0045(7) 0.0001(6) C37 0.0153(8) 0.0166(9) 0.0199(9) -0.0004(7) 0.0067(7) -0.0011(7) C38 0.0178(9) 0.0187(9) 0.0229(9) -0.0017(7) 0.0089(7) -0.0020(7) C39 0.0185(9) 0.0179(9) 0.0222(9) -0.0016(7) 0.0055(7) 0.0011(7) S13 0.0183(2) 0.0189(2) 0.0250(2) -0.00535(18) 0.00762(19) 0.00097(17) S14 0.0173(2) 0.0177(2) 0.0255(2) -0.00513(18) 0.00466(19) -0.00126(17) S15 0.0164(2) 0.0159(2) 0.0252(2) -0.00375(17) 0.00681(18) -0.00128(16) S16 0.0172(2) 0.0175(2) 0.0237(2) -0.00422(17) 0.00723(18) 0.00024(17) S17 0.0166(2) 0.0153(2) 0.0214(2) -0.00134(17) 0.00636(17) 0.00042(16) S18 0.0177(2) 0.0161(2) 0.0220(2) -0.00165(17) 0.00727(18) 0.00009(17) S19 0.0166(2) 0.0157(2) 0.0251(2) -0.00364(17) 0.00544(18) 0.00000(17) S20 0.0185(2) 0.0150(2) 0.0249(2) -0.00274(17) 0.00920(19) -0.00009(17) C40 0.0169(9) 0.0179(9) 0.0242(9) 0.0022(7) 0.0054(7) 0.0003(7) C41 0.0201(9) 0.0182(9) 0.0226(9) 0.0017(7) 0.0092(8) -0.0003(7) C42 0.0165(9) 0.0157(9) 0.0182(8) -0.0002(7) 0.0049(7) -0.0006(7) C43 0.0152(8) 0.0163(9) 0.0180(8) -0.0003(7) 0.0038(7) 0.0017(7) C44 0.0168(9) 0.0156(9) 0.0165(8) -0.0011(7) 0.0048(7) -0.0002(7) C45 0.0183(9) 0.0174(9) 0.0156(8) 0.0003(7) 0.0055(7) 0.0006(7) C46 0.0147(8) 0.0160(9) 0.0177(8) 0.0006(7) 0.0053(7) 0.0011(6) C47 0.0174(9) 0.0153(8) 0.0173(8) 0.0014(7) 0.0071(7) 0.0005(7) C48 0.0170(9) 0.0202(9) 0.0229(9) -0.0046(7) 0.0070(7) -0.0003(7) C49 0.0217(10) 0.0207(10) 0.0195(9) -0.0009(7) 0.0034(8) 0.0043(7) Fe 0.02235(15) 0.02238(15) 0.02079(14) 0.00195(11) 0.00779(11) 0.00173(11) O51 0.0327(9) 0.0238(8) 0.0252(8) 0.0043(6) 0.0076(7) 0.0045(6) O52 0.0291(8) 0.0223(7) 0.0233(7) 0.0032(6) 0.0064(6) 0.0002(6) O53 0.0342(9) 0.0287(9) 0.0255(8) -0.0002(6) 0.0024(7) -0.0005(7) O54 0.0377(10) 0.0219(8) 0.0379(9) 0.0029(7) 0.0071(8) -0.0023(7) O55 0.0277(8) 0.0325(9) 0.0250(8) -0.0002(6) 0.0097(6) 0.0004(7) O56 0.0265(8) 0.0414(10) 0.0224(8) 0.0045(7) 0.0073(6) -0.0008(7) O57 0.0318(9) 0.0546(12) 0.0392(10) -0.0031(9) 0.0138(8) -0.0104(8) O58 0.0307(10) 0.0972(18) 0.0325(10) 0.0180(11) -0.0020(8) -0.0108(11) O59 0.0322(8) 0.0218(8) 0.0279(8) 0.0012(6) 0.0129(7) -0.0012(6) O60 0.0269(8) 0.0237(8) 0.0302(8) 0.0019(6) 0.0129(6) 0.0005(6) O61 0.0571(12) 0.0238(8) 0.0396(10) 0.0003(7) 0.0207(9) 0.0082(8) O62 0.0293(9) 0.0397(10) 0.0252(8) 0.0014(7) 0.0116(7) 0.0081(7) C50 0.0222(10) 0.0241(10) 0.0282(11) 0.0038(8) 0.0099(8) 0.0016(8) C51 0.0201(10) 0.0238(10) 0.0250(10) 0.0030(8) 0.0085(8) 0.0005(8) C52 0.0278(11) 0.0261(11) 0.0291(11) 0.0013(9) 0.0111(9) 0.0026(9) C53 0.0256(11) 0.0417(14) 0.0277(11) 0.0077(10) 0.0048(9) 0.0015(10) C54 0.0310(11) 0.0235(10) 0.0215(10) -0.0019(8) 0.0056(8) -0.0003(8) C55 0.0200(10) 0.0294(11) 0.0215(10) 0.0010(8) 0.0031(8) 0.0009(8) O63 0.0447(11) 0.0474(11) 0.0405(10) -0.0105(9) 0.0239(9) -0.0002(9) O64 0.0584(12) 0.0308(9) 0.0370(10) 0.0061(8) 0.0204(9) 0.0060(9) O65 0.0369(9) 0.0258(8) 0.0280(8) -0.0030(6) 0.0062(7) -0.0010(7) O66 0.0621(13) 0.0347(10) 0.0407(10) -0.0046(8) 0.0248(10) -0.0113(9) O67 0.057(2) 0.055(3) 0.034(2) 0.0038(18) 0.0180(18) 0.015(2) O68 0.051(3) 0.108(4) 0.041(2) 0.004(3) 0.011(2) -0.028(3) O69 0.034(3) 0.135(6) 0.194(8) -0.109(6) 0.006(4) 0.014(3) O70 0.046(3) 0.068(3) 0.085(4) -0.017(3) 0.015(3) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O1 2.812(2) . ? K1 O2 2.7848(19) . ? K1 O3 2.744(2) . ? K1 O4 2.846(2) . ? K1 O5 2.7841(19) . ? K1 O6 2.8467(19) . ? K1 O66 2.774(2) . ? K1 O70 3.102(5) . ? K2 O7 2.842(3) . ? K2 O8 2.962(4) . ? K2 O9 2.791(5) . ? K2 O10 2.873(3) . ? K2 O11 2.759(4) . ? K2 O12 2.868(4) . ? K2 O57 2.617(2) . ? K2 O58 2.773(2) . ? O1 C1 1.388(4) . ? O1 C12 1.471(9) . ? O1 C12A 1.428(9) . ? C1 C2 1.479(5) . ? C2 O2 1.442(4) . ? O2 C3 1.412(4) . ? C3 C4 1.483(5) . ? C4 O3 1.440(4) . ? O3 C5 1.411(4) . ? C5 C6 1.493(5) . ? C6 O4 1.433(3) . ? O4 C7 1.398(11) . ? O4 C7A 1.424(8) . ? C7 C8 1.477(12) . ? C8 O5 1.466(10) . ? O5 C9 1.401(9) . ? O5 C8A 1.397(8) . ? O5 C9A 1.447(9) . ? C9 C10 1.494(9) . ? C10 O6 1.492(9) . ? O6 C11 1.410(8) . ? O6 C10A 1.373(9) . ? O6 C11A 1.420(9) . ? C11 C12 1.474(10) . ? C7A C8A 1.487(8) . ? C9A C10A 1.476(10) . ? C11A C12A 1.447(10) . ? O7 C13 1.414(6) . ? O7 C24 1.415(6) . ? O7 O70 1.479(6) . ? C13 C14 1.471(7) . ? C14 O8 1.440(6) . ? O8 C15 1.437(6) . ? C15 C16 1.500(7) . ? C16 K2 2.416(6) 2_546 ? C16 O9 1.434(7) . ? O9 K2 3.046(5) 2_546 ? O9 C17 1.421(6) . ? C17 K2 2.668(6) 2_546 ? C17 C18 1.489(8) . ? C18 O10 1.431(6) . ? O10 C19 1.424(6) . ? C19 C20 1.480(7) . ? C19 O67 1.918(7) . ? C20 O11 1.421(6) . ? O11 C21 1.423(6) . ? C21 K2 2.632(6) 2_556 ? C21 C22 1.484(7) . ? C22 K2 2.138(6) 2_556 ? C22 O12 1.434(6) . ? O12 C23 1.423(6) . ? C23 C24 1.505(7) . ? C24 O70 1.890(8) . ? S1 C25 1.804(2) . ? S1 C27 1.7410(19) . ? S2 C26 1.807(2) . ? S2 C28 1.7416(19) . ? S3 C27 1.749(2) . ? S3 C29 1.734(2) . ? S4 C28 1.7514(19) . ? S4 C29 1.738(2) . ? C25 C26 1.512(3) . ? C27 C28 1.353(3) . ? C29 C29 1.369(4) 3_667 ? S5 C30 1.806(2) . ? S5 C32 1.7436(19) . ? S6 C31 1.811(2) . ? S6 C33 1.7431(19) . ? S7 C32 1.7456(19) . ? S7 C34 1.736(2) . ? S8 C33 1.7495(19) . ? S8 C34 1.739(2) . ? S9 C35 1.735(2) . ? S9 C36 1.7515(19) . ? S10 C35 1.735(2) . ? S10 C37 1.750(2) . ? S11 C36 1.743(2) . ? S11 C38 1.811(2) . ? S12 C37 1.742(2) . ? S12 C39 1.807(2) . ? C30 C31 1.515(3) . ? C32 C33 1.353(3) . ? C34 C35 1.372(3) . ? C36 C37 1.360(3) . ? C38 C39 1.512(3) . ? S13 C40 1.813(2) . ? S13 C42 1.7462(19) . ? S14 C41 1.808(2) . ? S14 C43 1.746(2) . ? S15 C42 1.747(2) . ? S15 C44 1.7406(19) . ? S16 C43 1.7495(19) . ? S16 C44 1.738(2) . ? S17 C45 1.735(2) . ? S17 C46 1.7588(19) . ? S18 C45 1.737(2) . ? S18 C47 1.754(2) . ? S19 C46 1.746(2) . ? S19 C48 1.812(2) . ? S20 C47 1.7481(19) . ? S20 C49 1.812(2) . ? C40 C41 1.512(3) . ? C42 C43 1.356(3) . ? C44 C45 1.370(3) . ? C46 C47 1.360(3) . ? C48 C49 1.516(3) . ? Fe O51 1.9998(16) . ? Fe O52 2.0209(16) . ? Fe O55 1.9839(16) . ? Fe O56 2.0044(16) . ? Fe O59 2.0232(16) . ? Fe O60 2.0231(15) . ? O51 C50 1.279(3) . ? O52 C51 1.278(3) . ? O53 C51 1.226(3) . ? O54 C50 1.224(3) . ? O55 C52 1.284(3) . ? O56 C53 1.278(3) . ? O57 C52 1.218(3) . ? O58 C53 1.227(3) . ? O59 C54 1.275(3) . ? O60 C55 1.277(3) . ? O61 C54 1.227(3) . ? O62 C55 1.238(3) . ? C50 C51 1.557(3) . ? C52 C53 1.553(3) . ? C54 C55 1.541(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 O1 K1 O2 60.78(7) . . ? O1 K1 O3 121.69(7) . . ? O1 K1 O4 165.46(7) . . ? O1 K1 O5 118.76(7) . . ? O1 K1 O6 59.46(6) . . ? O1 K1 O66 102.60(6) . . ? O1 K1 O70 93.44(11) . . ? O2 K1 O3 62.10(7) . . ? O2 K1 O4 115.68(7) . . ? O2 K1 O5 163.91(7) . . ? O2 K1 O6 117.56(7) . . ? O2 K1 O66 113.30(6) . . ? O2 K1 O70 76.99(12) . . ? O3 K1 O4 60.05(6) . . ? O3 K1 O5 119.31(7) . . ? O3 K1 O6 174.52(7) . . ? O3 K1 O66 89.32(6) . . ? O3 K1 O70 84.59(12) . . ? O4 K1 O5 60.21(6) . . ? O4 K1 O6 117.33(6) . . ? O4 K1 O66 91.75(6) . . ? O4 K1 O70 72.13(11) . . ? O5 K1 O6 59.31(6) . . ? O5 K1 O66 82.73(6) . . ? O5 K1 O70 87.11(12) . . ? O6 K1 O66 95.65(6) . . ? O6 K1 O70 90.01(12) . . ? O66 K1 O70 163.72(11) . . ? O7 K2 O8 58.82(10) . . ? O7 K2 O9 118.49(12) . . ? O7 K2 O10 152.55(11) . . ? O7 K2 O11 117.82(11) . . ? O7 K2 O12 59.08(11) . . ? O7 K2 O57 73.72(9) . . ? O7 K2 O58 130.22(10) . . ? O7 K2 C52 89.74(9) . . ? O7 K2 C53 113.60(9) . . ? O8 K2 O9 59.69(11) . . ? O8 K2 O10 113.71(11) . . ? O8 K2 O11 161.28(11) . . ? O8 K2 O12 115.00(11) . . ? O8 K2 O57 77.48(9) . . ? O8 K2 O58 126.03(9) . . ? O8 K2 C52 92.27(8) . . ? O8 K2 C53 112.89(9) . . ? O9 K2 O10 60.39(11) . . ? O9 K2 O11 119.56(12) . . ? O9 K2 O12 160.79(13) . . ? O9 K2 O57 94.90(11) . . ? O9 K2 O58 88.35(11) . . ? O9 K2 C52 94.10(10) . . ? O9 K2 C53 91.09(11) . . ? O10 K2 O11 59.68(11) . . ? O10 K2 O12 111.99(11) . . ? O10 K2 O57 132.80(9) . . ? O10 K2 O58 76.57(9) . . ? O10 K2 C52 117.57(8) . . ? O10 K2 C53 93.76(9) . . ? O11 K2 O12 58.75(11) . . ? O11 K2 O57 120.37(10) . . ? O11 K2 O58 71.27(9) . . ? O11 K2 C52 106.32(9) . . ? O11 K2 C53 85.59(9) . . ? O12 K2 O57 101.97(10) . . ? O12 K2 O58 107.58(10) . . ? O12 K2 C52 104.77(9) . . ? O12 K2 C53 107.43(10) . . ? O57 K2 O58 62.17(6) . . ? O57 K2 C52 17.78(5) . . ? O57 K2 C53 43.75(6) . . ? O58 K2 C52 44.41(6) . . ? O58 K2 C53 18.43(6) . . ? C52 K2 C53 25.98(5) . . ? K1 O1 C1 113.68(18) . . ? K1 O1 C12 114.6(5) . . ? K1 O1 C12A 117.7(5) . . ? C1 O1 C12 118.8(5) . . ? C1 O1 C12A 106.3(6) . . ? C12 O1 C12A 14.8(7) . . ? O1 C1 C2 109.7(3) . . ? C1 C2 O2 110.4(2) . . ? K1 O2 C2 114.33(17) . . ? K1 O2 C3 109.17(17) . . ? C2 O2 C3 113.2(2) . . ? O2 C3 C4 109.7(2) . . ? C3 C4 O3 109.8(2) . . ? K1 O3 C4 115.21(18) . . ? K1 O3 C5 119.95(18) . . ? C4 O3 C5 111.7(2) . . ? O3 C5 C6 109.0(2) . . ? C5 C6 O4 109.1(3) . . ? K1 O4 C6 109.79(17) . . ? K1 O4 C7 117.5(6) . . ? K1 O4 C7A 110.7(5) . . ? C6 O4 C7 110.2(7) . . ? C6 O4 C7A 113.0(4) . . ? C7 O4 C7A 6.9(11) . . ? O4 C7 C8 107.0(12) . . ? C7 C8 O5 113.1(11) . . ? K1 O5 C8 113.1(6) . . ? K1 O5 C9 123.7(4) . . ? K1 O5 C8A 116.6(4) . . ? K1 O5 C9A 114.7(5) . . ? C8 O5 C9 113.2(6) . . ? C8 O5 C8A 3.8(8) . . ? C8 O5 C9A 116.2(7) . . ? C9 O5 C8A 109.5(5) . . ? C9 O5 C9A 10.7(9) . . ? C8A O5 C9A 112.7(5) . . ? O5 C9 C10 103.8(8) . . ? C9 C10 O6 111.6(9) . . ? K1 O6 C10 106.4(5) . . ? K1 O6 C11 112.1(5) . . ? K1 O6 C10A 114.6(6) . . ? K1 O6 C11A 111.0(5) . . ? C10 O6 C11 106.8(6) . . ? C10 O6 C10A 8.7(10) . . ? C10 O6 C11A 120.4(7) . . ? C11 O6 C10A 104.7(6) . . ? C11 O6 C11A 15.2(8) . . ? C10A O6 C11A 117.1(7) . . ? O6 C11 C12 103.9(8) . . ? O1 C12 C11 114.4(9) . . ? O4 C7A C8A 111.7(7) . . ? O5 C8A C7A 106.0(7) . . ? O5 C9A C10A 112.6(9) . . ? O6 C10A C9A 105.0(8) . . ? O6 C11A C12A 113.8(9) . . ? O1 C12A C11A 105.3(8) . . ? K2 O7 C13 117.5(3) . . ? K2 O7 C24 116.9(3) . . ? K2 O7 O70 131.0(3) . . ? C13 O7 C24 113.9(4) . . ? C13 O7 O70 33.9(3) . . ? C24 O7 O70 81.5(4) . . ? O7 C13 C14 108.6(4) . . ? C13 C14 O8 107.8(4) . . ? K2 O8 C14 106.2(3) . . ? K2 O8 C15 101.6(3) . . ? C14 O8 C15 112.2(4) . . ? O8 C15 C16 107.7(4) . . ? K2 C16 C15 149.3(4) 2_546 . ? K2 C16 O9 101.6(3) 2_546 . ? C15 C16 O9 108.7(5) . . ? K2 O9 K2 149.21(17) . 2_546 ? K2 O9 C16 118.6(3) . . ? K2 O9 C16 51.0(3) 2_546 . ? K2 O9 C17 116.7(3) . . ? K2 O9 C17 61.1(3) 2_546 . ? C16 O9 C17 111.9(4) . . ? K2 C17 O9 91.1(3) 2_546 . ? K2 C17 C18 156.6(4) 2_546 . ? O9 C17 C18 109.8(5) . . ? C17 C18 O10 110.4(5) . . ? K2 O10 C18 112.0(3) . . ? K2 O10 C19 108.0(3) . . ? C18 O10 C19 111.7(4) . . ? O10 C19 C20 110.3(4) . . ? O10 C19 O67 140.0(4) . . ? C20 C19 O67 86.1(4) . . ? C19 C20 O11 109.2(4) . . ? K2 O11 C20 120.3(3) . . ? K2 O11 C21 121.4(3) . . ? C20 O11 C21 112.2(4) . . ? K2 C21 O11 141.9(4) 2_556 . ? K2 C21 C22 54.3(3) 2_556 . ? O11 C21 C22 108.5(4) . . ? K2 C22 C21 91.4(4) 2_556 . ? K2 C22 O12 149.7(4) 2_556 . ? C21 C22 O12 108.1(5) . . ? K2 O12 C22 107.8(3) . . ? K2 O12 C23 113.1(3) . . ? C22 O12 C23 112.0(4) . . ? O12 C23 C24 107.9(5) . . ? O7 C24 C23 109.0(4) . . ? O7 C24 O70 50.7(3) . . ? C23 C24 O70 159.4(4) . . ? C25 S1 C27 101.50(9) . . ? C26 S2 C28 101.39(9) . . ? C27 S3 C29 95.15(9) . . ? C28 S4 C29 94.96(9) . . ? S1 C25 C26 114.24(15) . . ? S2 C26 C25 114.35(14) . . ? S1 C27 S3 113.81(11) . . ? S1 C27 C28 129.22(15) . . ? S3 C27 C28 116.92(14) . . ? S2 C28 S4 114.82(11) . . ? S2 C28 C27 128.12(15) . . ? S4 C28 C27 117.06(15) . . ? S3 C29 S4 115.83(10) . . ? S3 C29 C29 122.2(2) . 3_667 ? S4 C29 C29 122.0(2) . 3_667 ? C30 S5 C32 100.83(9) . . ? C31 S6 C33 101.90(9) . . ? C32 S7 C34 95.47(9) . . ? C33 S8 C34 95.48(9) . . ? C35 S9 C36 95.60(9) . . ? C35 S10 C37 95.34(9) . . ? C36 S11 C38 101.00(9) . . ? C37 S12 C39 102.14(9) . . ? S5 C30 C31 114.02(14) . . ? S6 C31 C30 114.05(14) . . ? S5 C32 S7 114.51(11) . . ? S5 C32 C33 128.37(15) . . ? S7 C32 C33 117.12(14) . . ? S6 C33 S8 114.41(11) . . ? S6 C33 C32 128.93(15) . . ? S8 C33 C32 116.66(14) . . ? S7 C34 S8 115.19(11) . . ? S7 C34 C35 122.20(15) . . ? S8 C34 C35 122.60(15) . . ? S9 C35 S10 115.47(11) . . ? S9 C35 C34 122.04(15) . . ? S10 C35 C34 122.49(15) . . ? S9 C36 S11 115.26(11) . . ? S9 C36 C37 116.39(14) . . ? S11 C36 C37 128.35(15) . . ? S10 C37 S12 114.41(11) . . ? S10 C37 C36 117.03(14) . . ? S12 C37 C36 128.56(15) . . ? S11 C38 C39 114.21(14) . . ? S12 C39 C38 113.73(14) . . ? C40 S13 C42 100.34(9) . . ? C41 S14 C43 102.37(9) . . ? C42 S15 C44 95.68(9) . . ? C43 S16 C44 95.56(9) . . ? C45 S17 C46 95.98(9) . . ? C45 S18 C47 95.62(9) . . ? C46 S19 C48 102.16(9) . . ? C47 S20 C49 100.55(9) . . ? S13 C40 C41 113.84(14) . . ? S14 C41 C40 114.87(14) . . ? S13 C42 S15 115.05(11) . . ? S13 C42 C43 128.21(15) . . ? S15 C42 C43 116.74(15) . . ? S14 C43 S16 114.20(11) . . ? S14 C43 C42 128.86(15) . . ? S16 C43 C42 116.91(15) . . ? S15 C44 S16 114.98(11) . . ? S15 C44 C45 122.34(15) . . ? S16 C44 C45 122.67(15) . . ? S17 C45 S18 114.97(11) . . ? S17 C45 C44 122.31(15) . . ? S18 C45 C44 122.72(15) . . ? S17 C46 S19 114.76(11) . . ? S17 C46 C47 116.03(14) . . ? S19 C46 C47 129.21(15) . . ? S18 C47 S20 115.65(11) . . ? S18 C47 C46 116.98(14) . . ? S20 C47 C46 127.37(15) . . ? S19 C48 C49 113.42(14) . . ? S20 C49 C48 112.98(14) . . ? O51 Fe O52 80.33(6) . . ? O51 Fe O55 101.00(7) . . ? O51 Fe O56 94.98(7) . . ? O51 Fe O59 163.35(7) . . ? O51 Fe O60 90.97(7) . . ? O52 Fe O55 90.83(6) . . ? O52 Fe O56 169.48(7) . . ? O52 Fe O59 87.60(6) . . ? O52 Fe O60 102.08(7) . . ? O55 Fe O56 80.77(7) . . ? O55 Fe O59 90.55(7) . . ? O55 Fe O60 163.76(7) . . ? O56 Fe O59 98.73(7) . . ? O56 Fe O60 87.34(7) . . ? O59 Fe O60 80.30(6) . . ? Fe O51 C50 116.20(14) . . ? Fe O52 C51 115.49(13) . . ? Fe O55 C52 116.15(14) . . ? Fe O56 C53 115.24(15) . . ? K2 O57 C52 121.22(16) . . ? K2 O58 C53 115.97(17) . . ? Fe O59 C54 114.78(14) . . ? Fe O60 C55 113.23(14) . . ? O51 C50 O54 126.3(2) . . ? O51 C50 C51 113.94(19) . . ? O54 C50 C51 119.7(2) . . ? O52 C51 O53 126.1(2) . . ? O52 C51 C50 113.81(18) . . ? O53 C51 C50 120.1(2) . . ? K2 C52 O55 166.67(15) . . ? K2 C52 O57 41.00(13) . . ? K2 C52 C53 79.84(13) . . ? O55 C52 O57 125.9(2) . . ? O55 C52 C53 113.28(19) . . ? O57 C52 C53 120.8(2) . . ? K2 C53 O56 171.55(16) . . ? K2 C53 O58 45.60(13) . . ? K2 C53 C52 74.18(13) . . ? O56 C53 O58 126.1(2) . . ? O56 C53 C52 114.2(2) . . ? O58 C53 C52 119.8(2) . . ? O59 C54 O61 126.6(2) . . ? O59 C54 C55 113.83(19) . . ? O61 C54 C55 119.6(2) . . ? O60 C55 O62 126.6(2) . . ? O60 C55 C54 114.24(18) . . ? O62 C55 C54 119.2(2) . . ? K1 O70 O7 132.3(3) . . ? K1 O70 C24 84.9(2) . . ? O7 O70 C24 47.8(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.64 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.164 _refine_diff_density_min -2.296 _refine_diff_density_rms 0.080 #===END