# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Lindoy, Leonard' _publ_contact_author_name 'Lindoy, Leonard' _publ_contact_author_email lindoy@gmail.com _publ_section_title ; An Expanded Neutral M4L6 Cage that Encapsulates Four Tetrahydrofuran Molecules ; # Attachment '- Lindoy LJ102SADx.CIF' data_lj102sad _database_code_depnum_ccdc_archive 'CCDC 815064' #TrackingRef '- Lindoy LJ102SADx.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C156 H168 Fe4 O24, 18(C4 H8 O), 14(C4 H10 O)' _chemical_formula_sum 'C284 H452 Fe4 O84' _chemical_formula_weight 5433.86 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I41/a _symmetry_space_group_name_Hall '-I 4ad' _symmetrry_Inl_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 34.877(3) _cell_length_b 34.877(3) _cell_length_c 23.646(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 28763(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20959 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 24.85 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11728 _exptl_absorpt_coefficient_mu 0.281 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.293876 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.013 0.044 0.551 15345.8 4726.9 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 115 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.02 _diffrn_reflns_number 108221 _diffrn_reflns_av_R_equivalents 0.1206 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.35 _reflns_number_total 13118 _reflns_number_gt 7262 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.1603P)^2^+0.0000P] 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 13118 _refine_ls_number_parameters 484 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2407 _refine_ls_wR_factor_gt 0.2143 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.920 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.23380(15) 0.03388(17) 0.5807(2) 0.1021(17) Uani 1 1 d . . . H1A H 0.2128 0.0159 0.5880 0.153 Uiso 1 1 calc R . . H1B H 0.2236 0.0571 0.5627 0.153 Uiso 1 1 calc R . . H1C H 0.2462 0.0407 0.6164 0.153 Uiso 1 1 calc R . . C2 C 0.24181(18) 0.00523(18) 0.4877(3) 0.126(3) Uani 1 1 d . . . H2A H 0.2597 -0.0042 0.4589 0.190 Uiso 1 1 calc R . . H2B H 0.2288 0.0283 0.4737 0.190 Uiso 1 1 calc R . . H2C H 0.2227 -0.0146 0.4959 0.190 Uiso 1 1 calc R . . C3 C 0.27779(14) -0.02074(14) 0.5687(3) 0.109(2) Uani 1 1 d . . . H3A H 0.2568 -0.0394 0.5714 0.164 Uiso 1 1 calc R . . H3B H 0.2871 -0.0145 0.6067 0.164 Uiso 1 1 calc R . . H3C H 0.2987 -0.0317 0.5463 0.164 Uiso 1 1 calc R . . C4 C 0.26357(10) 0.01479(11) 0.54075(17) 0.0566(10) Uani 1 1 d . . . C5 C 0.29529(9) 0.04444(9) 0.53243(15) 0.0450(8) Uani 1 1 d . . . C6 C 0.29178(10) 0.07257(10) 0.48999(16) 0.0540(9) Uani 1 1 d . . . H6 H 0.2694 0.0721 0.4672 0.065 Uiso 1 1 calc R . . C7 C 0.31898(9) 0.10116(9) 0.47906(15) 0.0449(8) Uani 1 1 d . . . C8 C 0.31521(9) 0.12904(10) 0.43174(16) 0.0509(9) Uani 1 1 d . . . C9 C 0.28759(9) 0.12694(9) 0.39038(15) 0.0477(8) Uani 1 1 d . . . H9 H 0.2697 0.1064 0.3908 0.057 Uiso 1 1 calc R . . C10 C 0.28536(9) 0.15472(10) 0.34751(16) 0.0506(9) Uani 1 1 d . . . H10 H 0.2662 0.1524 0.3191 0.061 Uiso 1 1 calc R . . C11 C 0.31047(11) 0.18527(10) 0.34599(17) 0.0593(10) Uani 1 1 d . . . C12 C 0.33837(12) 0.18712(13) 0.3884(2) 0.0840(16) Uani 1 1 d . . . H12 H 0.3559 0.2080 0.3886 0.101 Uiso 1 1 calc R . . C13 C 0.34107(12) 0.15962(13) 0.42975(19) 0.0794(15) Uani 1 1 d . . . H13 H 0.3608 0.1614 0.4574 0.095 Uiso 1 1 calc R . . C14 C 0.30769(10) 0.21670(10) 0.30252(18) 0.0555(10) Uani 1 1 d . . . C15 C 0.29455(11) 0.20969(11) 0.24865(18) 0.0627(10) Uani 1 1 d . . . H15 H 0.2863 0.1846 0.2387 0.075 Uiso 1 1 calc R . . C16 C 0.29325(11) 0.23876(10) 0.20881(17) 0.0596(10) Uani 1 1 d . . . H16 H 0.2842 0.2334 0.1718 0.071 Uiso 1 1 calc R . . C17 C 0.30516(9) 0.27590(9) 0.22235(16) 0.0463(8) Uani 1 1 d . . . C18 C 0.31737(13) 0.28294(11) 0.27617(18) 0.0698(12) Uani 1 1 d . . . H18 H 0.3257 0.3080 0.2862 0.084 Uiso 1 1 calc R . . C19 C 0.31781(15) 0.25403(13) 0.3166(2) 0.0849(15) Uani 1 1 d . . . H19 H 0.3251 0.2599 0.3543 0.102 Uiso 1 1 calc R . . C20 C 0.30644(9) 0.30842(9) 0.17976(16) 0.0467(9) Uani 1 1 d . . . C21 C 0.30473(10) 0.30260(10) 0.12277(15) 0.0487(9) Uani 1 1 d . . . H21 H 0.3033 0.2769 0.1096 0.058 Uiso 1 1 calc R . . C22 C 0.30493(10) 0.33221(10) 0.08186(16) 0.0502(9) Uani 1 1 d . . . C23 C 0.30243(13) 0.32333(11) 0.01835(17) 0.0651(11) Uani 1 1 d . . . C24 C 0.33604(18) 0.29695(18) 0.0034(2) 0.1087(19) Uani 1 1 d . . . H24A H 0.3365 0.2925 -0.0376 0.163 Uiso 1 1 calc R . . H24B H 0.3330 0.2724 0.0230 0.163 Uiso 1 1 calc R . . H24C H 0.3601 0.3090 0.0151 0.163 Uiso 1 1 calc R . . C25 C 0.3017(2) 0.35922(15) -0.0157(2) 0.111(2) Uani 1 1 d . . . H25A H 0.2774 0.3727 -0.0092 0.166 Uiso 1 1 calc R . . H25B H 0.3041 0.3529 -0.0559 0.166 Uiso 1 1 calc R . . H25C H 0.3231 0.3758 -0.0043 0.166 Uiso 1 1 calc R . . C26 C 0.26508(18) 0.30135(17) 0.0074(2) 0.1082(19) Uani 1 1 d . . . H26A H 0.2432 0.3172 0.0188 0.162 Uiso 1 1 calc R . . H26B H 0.2651 0.2775 0.0293 0.162 Uiso 1 1 calc R . . H26C H 0.2631 0.2953 -0.0330 0.162 Uiso 1 1 calc R . . C27 C 0.2514(5) 0.1362(6) 0.6604(9) 0.079(4) Uani 0.33 1 d P A 1 H27A H 0.2286 0.1466 0.6792 0.119 Uiso 0.33 1 calc PR A 1 H27B H 0.2495 0.1082 0.6587 0.119 Uiso 0.33 1 calc PR A 1 H27C H 0.2531 0.1466 0.6220 0.119 Uiso 0.33 1 calc PR A 1 C28 C 0.2880(5) 0.1230(5) 0.7475(7) 0.073(3) Uani 0.33 1 d P A 1 H28A H 0.3054 0.1353 0.7746 0.110 Uiso 0.33 1 calc PR A 1 H28B H 0.2975 0.0972 0.7386 0.110 Uiso 0.33 1 calc PR A 1 H28C H 0.2624 0.1211 0.7642 0.110 Uiso 0.33 1 calc PR A 1 C29 C 0.2812(5) 0.1918(5) 0.7116(9) 0.071(3) Uani 0.33 1 d P A 1 H29A H 0.2726 0.2070 0.6791 0.106 Uiso 0.33 1 calc PR A 1 H29B H 0.3059 0.2017 0.7251 0.106 Uiso 0.33 1 calc PR A 1 H29C H 0.2622 0.1936 0.7420 0.106 Uiso 0.33 1 calc PR A 1 C27A C 0.2525(5) 0.1174(5) 0.6757(9) 0.079(4) Uani 0.33 1 d P A 2 H27D H 0.2286 0.1247 0.6947 0.119 Uiso 0.33 1 calc PR A 2 H27E H 0.2598 0.0914 0.6873 0.119 Uiso 0.33 1 calc PR A 2 H27F H 0.2486 0.1180 0.6346 0.119 Uiso 0.33 1 calc PR A 2 C28A C 0.2953(5) 0.1415(5) 0.7563(7) 0.073(3) Uani 0.33 1 d P A 2 H28D H 0.3042 0.1657 0.7725 0.110 Uiso 0.33 1 calc PR A 2 H28E H 0.3154 0.1220 0.7604 0.110 Uiso 0.33 1 calc PR A 2 H28F H 0.2721 0.1330 0.7762 0.110 Uiso 0.33 1 calc PR A 2 C29A C 0.2730(5) 0.1879(4) 0.6813(7) 0.071(3) Uani 0.33 1 d P A 2 H29D H 0.2489 0.1927 0.7014 0.106 Uiso 0.33 1 calc PR A 2 H29E H 0.2691 0.1914 0.6406 0.106 Uiso 0.33 1 calc PR A 2 H29F H 0.2926 0.2059 0.6946 0.106 Uiso 0.33 1 calc PR A 2 C27B C 0.2900(4) 0.1826(6) 0.7317(8) 0.079(4) Uani 0.33 1 d P A 3 H27G H 0.2959 0.2053 0.7089 0.119 Uiso 0.33 1 calc PR A 3 H27H H 0.3106 0.1783 0.7591 0.119 Uiso 0.33 1 calc PR A 3 H27I H 0.2658 0.1867 0.7520 0.119 Uiso 0.33 1 calc PR A 3 C28B C 0.2772(5) 0.1102(5) 0.7275(7) 0.073(3) Uani 0.33 1 d P A 3 H28G H 0.2541 0.1143 0.7504 0.110 Uiso 0.33 1 calc PR A 3 H28H H 0.2988 0.1043 0.7525 0.110 Uiso 0.33 1 calc PR A 3 H28I H 0.2729 0.0886 0.7016 0.110 Uiso 0.33 1 calc PR A 3 C29B C 0.2557(4) 0.1543(4) 0.6474(7) 0.071(3) Uani 0.33 1 d P A 3 H29G H 0.2301 0.1517 0.6641 0.106 Uiso 0.33 1 calc PR A 3 H29H H 0.2588 0.1355 0.6169 0.106 Uiso 0.33 1 calc PR A 3 H29I H 0.2587 0.1802 0.6321 0.106 Uiso 0.33 1 calc PR A 3 C30 C 0.28610(10) 0.14719(11) 0.69274(17) 0.0583(10) Uani 1 1 d . . . C31 C 0.32249(9) 0.13828(10) 0.65883(15) 0.0464(8) Uani 1 1 d . A . C32 C 0.35528(10) 0.16202(10) 0.66362(17) 0.0556(9) Uani 1 1 d . . . H32 H 0.3544 0.1827 0.6897 0.067 Uiso 1 1 calc R A . C33 C 0.38858(9) 0.15696(9) 0.63262(15) 0.0438(8) Uani 1 1 d . A . C34 C 0.42174(9) 0.18442(9) 0.63856(16) 0.0495(9) Uani 1 1 d . . . C35 C 0.41564(11) 0.22316(11) 0.6542(2) 0.0694(12) Uani 1 1 d . A . H35 H 0.3906 0.2318 0.6634 0.083 Uiso 1 1 calc R . . C36 C 0.44611(11) 0.24830(11) 0.65618(19) 0.0660(11) Uani 1 1 d . . . H36 H 0.4418 0.2743 0.6663 0.079 Uiso 1 1 calc R A . C37 C 0.48351(10) 0.23608(10) 0.64338(18) 0.0575(10) Uani 1 1 d . . . C38 C 0.48922(10) 0.19782(10) 0.62906(18) 0.0589(10) Uani 1 1 d . . . H38 H 0.5143 0.1888 0.6210 0.071 Uiso 1 1 calc R A . C39 C 0.45826(10) 0.17288(11) 0.62654(18) 0.0584(10) Uani 1 1 d . A . H39 H 0.4626 0.1469 0.6161 0.070 Uiso 1 1 calc R . . O7 O 0.4224(7) 0.2243(6) 0.4441(10) 0.289(5) Uani 0.50 1 d PD B 1 C41 C 0.4367(12) 0.2026(10) 0.3839(12) 0.289(5) Uani 0.50 1 d PD B 1 H41A H 0.4620 0.2116 0.3703 0.347 Uiso 0.50 1 calc PR B 1 H41B H 0.4174 0.2039 0.3533 0.347 Uiso 0.50 1 calc PR B 1 C42 C 0.4386(10) 0.1586(10) 0.4163(14) 0.289(5) Uani 0.50 1 d P B 1 H42A H 0.4138 0.1449 0.4134 0.347 Uiso 0.50 1 calc PR B 1 H42B H 0.4591 0.1424 0.4001 0.347 Uiso 0.50 1 calc PR B 1 C40 C 0.4537(9) 0.2126(10) 0.4802(11) 0.289(5) Uani 0.50 1 d PD B 1 H40A H 0.4496 0.2186 0.5207 0.347 Uiso 0.50 1 calc PR B 1 H40B H 0.4791 0.2220 0.4674 0.347 Uiso 0.50 1 calc PR B 1 C43 C 0.4455(10) 0.1674(10) 0.4640(15) 0.289(5) Uani 0.50 1 d P B 1 H43A H 0.4682 0.1524 0.4760 0.347 Uiso 0.50 1 calc PR B 1 H43B H 0.4237 0.1586 0.4875 0.347 Uiso 0.50 1 calc PR B 1 O7A O 0.4379(7) 0.2020(7) 0.4190(9) 0.289(5) Uani 0.50 1 d PD C 2 C40A C 0.4524(9) 0.1702(8) 0.4942(8) 0.289(5) Uani 0.50 1 d PD C 2 H40C H 0.4589 0.1694 0.5350 0.347 Uiso 0.50 1 calc PR C 2 H40D H 0.4376 0.1470 0.4840 0.347 Uiso 0.50 1 calc PR C 2 C41A C 0.4316(8) 0.2052(8) 0.4797(11) 0.289(5) Uani 0.50 1 d PD C 2 H41C H 0.4041 0.2040 0.4900 0.347 Uiso 0.50 1 calc PR C 2 H41D H 0.4435 0.2285 0.4960 0.347 Uiso 0.50 1 calc PR C 2 C42A C 0.4866(6) 0.1744(8) 0.4593(12) 0.289(5) Uani 0.50 1 d PD C 2 H42C H 0.5006 0.1985 0.4675 0.347 Uiso 0.50 1 calc PR C 2 H42D H 0.5041 0.1522 0.4628 0.347 Uiso 0.50 1 calc PR C 2 C43A C 0.4678(9) 0.1755(10) 0.4052(9) 0.289(5) Uani 0.50 1 d PD C 2 H43C H 0.4849 0.1855 0.3751 0.347 Uiso 0.50 1 calc PR C 2 H43D H 0.4576 0.1501 0.3941 0.347 Uiso 0.50 1 calc PR C 2 O1 O 0.32423(6) 0.04185(6) 0.56543(10) 0.0465(6) Uani 1 1 d . . . O2 O 0.34885(6) 0.10560(6) 0.50983(10) 0.0505(6) Uani 1 1 d . . . O3 O 0.30855(6) 0.34207(6) 0.20288(9) 0.0463(6) Uani 1 1 d . . . O4 O 0.30748(6) 0.36745(6) 0.09524(9) 0.0458(6) Uani 1 1 d . . . O5 O 0.32157(6) 0.10847(7) 0.62755(10) 0.0495(6) Uani 1 1 d . . . O6 O 0.39490(6) 0.12856(6) 0.60003(11) 0.0524(6) Uani 1 1 d . . . Fe1 Fe 0.362617(13) 0.082365(13) 0.58358(2) 0.04651(19) Uani 1 1 d . A . 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 0.077(3) 0.103(4) 0.126(4) 0.020(3) 0.021(3) -0.015(3) C2 0.132(5) 0.123(5) 0.124(5) 0.049(4) -0.045(4) -0.086(4) C3 0.064(3) 0.068(3) 0.196(6) 0.041(4) -0.021(3) -0.029(2) C4 0.048(2) 0.051(2) 0.071(3) 0.0098(18) -0.0080(19) -0.0214(17) C5 0.0380(18) 0.0369(18) 0.060(2) 0.0002(16) 0.0039(16) -0.0084(14) C6 0.0397(19) 0.048(2) 0.075(2) 0.0152(18) -0.0100(17) -0.0170(15) C7 0.0309(17) 0.0393(18) 0.064(2) 0.0072(16) -0.0050(15) -0.0049(13) C8 0.0361(18) 0.046(2) 0.071(2) 0.0126(17) -0.0048(17) -0.0054(15) C9 0.0368(18) 0.0353(18) 0.071(2) 0.0091(16) -0.0003(16) -0.0098(14) C10 0.0305(17) 0.050(2) 0.071(2) 0.0038(18) -0.0097(16) -0.0015(14) C11 0.052(2) 0.045(2) 0.081(3) 0.0189(19) -0.0143(19) -0.0050(17) C12 0.064(3) 0.071(3) 0.117(4) 0.049(3) -0.045(3) -0.037(2) C13 0.067(3) 0.075(3) 0.096(3) 0.036(2) -0.046(2) -0.035(2) C14 0.043(2) 0.042(2) 0.082(3) 0.0107(18) -0.0114(19) -0.0059(15) C15 0.060(2) 0.041(2) 0.086(3) 0.011(2) -0.007(2) 0.0016(17) C16 0.067(3) 0.040(2) 0.071(3) 0.0015(18) -0.017(2) 0.0022(17) C17 0.0388(18) 0.0330(17) 0.067(2) 0.0039(16) -0.0072(16) 0.0050(13) C18 0.086(3) 0.046(2) 0.077(3) 0.012(2) -0.032(2) -0.020(2) C19 0.112(4) 0.063(3) 0.079(3) 0.017(2) -0.043(3) -0.030(3) C20 0.0316(17) 0.0318(17) 0.077(3) 0.0020(16) -0.0100(16) 0.0087(13) C21 0.054(2) 0.0346(18) 0.057(2) -0.0050(16) -0.0121(17) 0.0124(15) C22 0.045(2) 0.041(2) 0.064(2) -0.0065(17) -0.0110(17) 0.0126(15) C23 0.080(3) 0.051(2) 0.064(3) -0.0055(19) -0.018(2) 0.012(2) C24 0.133(5) 0.130(5) 0.063(3) -0.002(3) 0.000(3) 0.047(4) C25 0.197(7) 0.073(3) 0.063(3) 0.003(3) -0.019(3) 0.016(4) C26 0.128(5) 0.106(4) 0.090(4) -0.032(3) -0.036(3) 0.000(4) C27 0.043(4) 0.091(10) 0.103(10) -0.015(8) 0.008(5) -0.015(6) C28 0.070(7) 0.078(10) 0.071(7) -0.003(6) 0.013(5) -0.017(6) C29 0.057(5) 0.063(5) 0.093(9) -0.015(6) 0.007(5) -0.006(4) C27A 0.043(4) 0.091(10) 0.103(10) -0.015(8) 0.008(5) -0.015(6) C28A 0.070(7) 0.078(10) 0.071(7) -0.003(6) 0.013(5) -0.017(6) C29A 0.057(5) 0.063(5) 0.093(9) -0.015(6) 0.007(5) -0.006(4) C27B 0.043(4) 0.091(10) 0.103(10) -0.015(8) 0.008(5) -0.015(6) C28B 0.070(7) 0.078(10) 0.071(7) -0.003(6) 0.013(5) -0.017(6) C29B 0.057(5) 0.063(5) 0.093(9) -0.015(6) 0.007(5) -0.006(4) C30 0.039(2) 0.064(2) 0.072(3) 0.004(2) 0.0107(18) -0.0125(17) C31 0.0330(17) 0.048(2) 0.058(2) 0.0095(17) -0.0061(15) -0.0068(14) C32 0.046(2) 0.044(2) 0.078(3) -0.0079(18) 0.0017(18) -0.0177(16) C33 0.0336(17) 0.0353(18) 0.062(2) 0.0065(16) -0.0070(15) -0.0093(13) C34 0.0344(18) 0.0373(18) 0.077(2) 0.0048(17) 0.0018(17) -0.0116(14) C35 0.035(2) 0.051(2) 0.122(4) -0.007(2) 0.005(2) -0.0120(16) C36 0.046(2) 0.039(2) 0.114(3) -0.009(2) 0.008(2) -0.0114(16) C37 0.0375(19) 0.041(2) 0.094(3) 0.0011(19) 0.0023(19) -0.0164(15) C38 0.0372(19) 0.0334(18) 0.106(3) -0.0007(19) 0.0067(19) -0.0076(14) C39 0.042(2) 0.042(2) 0.091(3) -0.0019(19) 0.0014(19) -0.0109(15) O7 0.304(11) 0.291(11) 0.274(11) 0.008(11) -0.085(11) 0.085(9) C41 0.304(11) 0.291(11) 0.274(11) 0.008(11) -0.085(11) 0.085(9) C42 0.304(11) 0.291(11) 0.274(11) 0.008(11) -0.085(11) 0.085(9) C40 0.304(11) 0.291(11) 0.274(11) 0.008(11) -0.085(11) 0.085(9) C43 0.304(11) 0.291(11) 0.274(11) 0.008(11) -0.085(11) 0.085(9) O7A 0.304(11) 0.291(11) 0.274(11) 0.008(11) -0.085(11) 0.085(9) C40A 0.304(11) 0.291(11) 0.274(11) 0.008(11) -0.085(11) 0.085(9) C41A 0.304(11) 0.291(11) 0.274(11) 0.008(11) -0.085(11) 0.085(9) C42A 0.304(11) 0.291(11) 0.274(11) 0.008(11) -0.085(11) 0.085(9) C43A 0.304(11) 0.291(11) 0.274(11) 0.008(11) -0.085(11) 0.085(9) O1 0.0413(13) 0.0388(12) 0.0593(14) 0.0074(10) -0.0097(11) -0.0123(10) O2 0.0394(13) 0.0443(13) 0.0678(16) 0.0142(11) -0.0086(11) -0.0168(10) O3 0.0447(13) 0.0384(13) 0.0559(14) 0.0016(10) -0.0021(11) 0.0111(10) O4 0.0424(13) 0.0356(12) 0.0593(14) 0.0006(10) -0.0122(10) 0.0100(9) O5 0.0332(12) 0.0440(14) 0.0714(16) -0.0015(12) 0.0023(11) -0.0143(10) O6 0.0317(12) 0.0395(13) 0.0859(18) -0.0015(12) -0.0050(12) -0.0149(10) Fe1 0.0344(3) 0.0391(3) 0.0660(4) 0.0072(2) -0.0039(2) -0.0115(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 C1 C4 1.553(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.504(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.489(6) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.527(4) . ? C5 O1 1.279(4) . ? C5 C6 1.409(5) . ? C6 C7 1.400(4) . ? C6 H6 0.9500 . ? C7 O2 1.280(4) . ? C7 C8 1.488(5) . ? C8 C9 1.375(5) . ? C8 C13 1.398(5) . ? C9 C10 1.404(5) . ? C9 H9 0.9500 . ? C10 C11 1.379(5) . ? C10 H10 0.9500 . ? C11 C12 1.399(5) . ? C11 C14 1.506(5) . ? C12 C13 1.373(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.376(5) . ? C14 C19 1.389(5) . ? C15 C16 1.385(5) . ? C15 H15 0.9500 . ? C16 C17 1.398(5) . ? C16 H16 0.9500 . ? C17 C18 1.364(5) . ? C17 C20 1.517(5) . ? C18 C19 1.389(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 O3 1.297(4) . ? C20 C21 1.364(5) . ? C21 C22 1.415(5) . ? C21 H21 0.9500 . ? C22 O4 1.272(4) . ? C22 C23 1.536(5) . ? C23 C25 1.488(6) . ? C23 C24 1.532(6) . ? C23 C26 1.533(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C30 1.482(19) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.548(17) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.629(19) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C27A C30 1.618(17) . ? C27A H27D 0.9800 . ? C27A H27E 0.9800 . ? C27A H27F 0.9800 . ? C28A C30 1.549(17) . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A C30 1.515(16) . ? C29A H29D 0.9800 . ? C29A H29E 0.9800 . ? C29A H29F 0.9800 . ? C27B C30 1.548(18) . ? C27B H27G 0.9800 . ? C27B H27H 0.9800 . ? C27B H27I 0.9800 . ? C28B C30 1.563(16) . ? C28B H28G 0.9800 . ? C28B H28H 0.9800 . ? C28B H28I 0.9800 . ? C29B C30 1.528(16) . ? C29B H29G 0.9800 . ? C29B H29H 0.9800 . ? C29B H29I 0.9800 . ? C30 C31 1.533(5) . ? C31 O5 1.276(4) . ? C31 C32 1.417(4) . ? C32 C33 1.385(5) . ? C32 H32 0.9500 . ? C33 O6 1.274(4) . ? C33 C34 1.508(4) . ? C34 C39 1.366(5) . ? C34 C35 1.417(5) . ? C35 C36 1.378(5) . ? C35 H35 0.9500 . ? C36 C37 1.405(5) . ? C36 H36 0.9500 . ? C37 C38 1.391(5) . ? C37 C37 1.505(6) 2_655 ? C38 C39 1.388(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? O7 C40 1.445(10) . ? O7 C41 1.69(3) . ? C41 C42 1.72(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.19(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C40 C43 1.65(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? O7A C43A 1.43(2) . ? O7A C41A 1.456(10) . ? C40A C42A 1.459(10) . ? C40A C41A 1.460(10) . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ? C41A H41C 0.9900 . ? C41A H41D 0.9900 . ? C42A C43A 1.436(10) . ? C42A H42C 0.9900 . ? C42A H42D 0.9900 . ? C43A H43C 0.9900 . ? C43A H43D 0.9900 . ? O1 Fe1 1.993(2) . ? O2 Fe1 1.982(2) . ? O3 Fe1 1.982(2) 11_666 ? O4 Fe1 2.017(2) 11_666 ? O5 Fe1 1.990(2) . ? O6 Fe1 2.004(2) . ? Fe1 O3 1.982(2) 12_656 ? Fe1 O4 2.017(2) 12_656 ? 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 C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C3 C4 C2 110.7(4) . . ? C3 C4 C5 112.3(3) . . ? C2 C4 C5 114.1(3) . . ? C3 C4 C1 108.1(4) . . ? C2 C4 C1 105.4(4) . . ? C5 C4 C1 105.8(3) . . ? O1 C5 C6 123.5(3) . . ? O1 C5 C4 116.4(3) . . ? C6 C5 C4 120.0(3) . . ? C7 C6 C5 124.7(3) . . ? C7 C6 H6 117.7 . . ? C5 C6 H6 117.7 . . ? O2 C7 C6 122.2(3) . . ? O2 C7 C8 114.8(3) . . ? C6 C7 C8 123.0(3) . . ? C9 C8 C13 118.0(3) . . ? C9 C8 C7 124.2(3) . . ? C13 C8 C7 117.8(3) . . ? C8 C9 C10 121.0(3) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 121.1(3) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 117.3(3) . . ? C10 C11 C14 122.6(3) . . ? C12 C11 C14 120.0(3) . . ? C13 C12 C11 121.7(3) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C8 120.8(3) . . ? C12 C13 H13 119.6 . . ? C8 C13 H13 119.6 . . ? C15 C14 C19 118.2(4) . . ? C15 C14 C11 121.6(3) . . ? C19 C14 C11 120.2(4) . . ? C14 C15 C16 120.7(4) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C17 120.9(4) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 118.2(3) . . ? C18 C17 C20 118.4(3) . . ? C16 C17 C20 123.3(3) . . ? C17 C18 C19 121.0(4) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C14 120.8(4) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? O3 C20 C21 123.6(3) . . ? O3 C20 C17 113.5(3) . . ? C21 C20 C17 122.9(3) . . ? C20 C21 C22 124.5(3) . . ? C20 C21 H21 117.7 . . ? C22 C21 H21 117.7 . . ? O4 C22 C21 122.4(3) . . ? O4 C22 C23 116.2(3) . . ? C21 C22 C23 121.4(3) . . ? C25 C23 C24 113.2(4) . . ? C25 C23 C26 108.3(4) . . ? C24 C23 C26 108.1(4) . . ? C25 C23 C22 111.1(3) . . ? C24 C23 C22 107.7(3) . . ? C26 C23 C22 108.3(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C30 C27 H27A 109.5 . . ? C30 C27 H27B 109.5 . . ? C30 C27 H27C 109.5 . . ? C30 C28 H28A 109.5 . . ? C30 C28 H28B 109.5 . . ? C30 C28 H28C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? C30 C27A H27D 109.5 . . ? C30 C27A H27E 109.5 . . ? H27D C27A H27E 109.5 . . ? C30 C27A H27F 109.5 . . ? H27D C27A H27F 109.5 . . ? H27E C27A H27F 109.5 . . ? C30 C28A H28D 109.5 . . ? C30 C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C30 C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C30 C29A H29D 109.5 . . ? C30 C29A H29E 109.5 . . ? H29D C29A H29E 109.5 . . ? C30 C29A H29F 109.5 . . ? H29D C29A H29F 109.5 . . ? H29E C29A H29F 109.5 . . ? C30 C27B H27G 109.5 . . ? C30 C27B H27H 109.5 . . ? C30 C27B H27I 109.5 . . ? C30 C28B H28G 109.5 . . ? C30 C28B H28H 109.5 . . ? C30 C28B H28I 109.5 . . ? C30 C29B H29G 109.5 . . ? C30 C29B H29H 109.5 . . ? C30 C29B H29I 109.5 . . ? C27 C30 C29A 84.5(10) . . ? C27 C30 C29B 27.5(7) . . ? C29A C30 C29B 61.0(8) . . ? C27 C30 C31 110.7(9) . . ? C29A C30 C31 110.3(7) . . ? C29B C30 C31 103.9(6) . . ? C27 C30 C27B 125.8(11) . . ? C29A C30 C27B 52.0(8) . . ? C29B C30 C27B 110.4(9) . . ? C31 C30 C27B 113.7(7) . . ? C27 C30 C28 109.0(11) . . ? C29A C30 C28 132.3(9) . . ? C29B C30 C28 134.9(9) . . ? C31 C30 C28 106.9(7) . . ? C27B C30 C28 86.2(10) . . ? C27 C30 C28A 129.5(10) . . ? C29A C30 C28A 110.8(9) . . ? C29B C30 C28A 147.7(9) . . ? C31 C30 C28A 108.0(7) . . ? C27B C30 C28A 60.5(9) . . ? C28 C30 C28A 27.0(6) . . ? C27 C30 C28B 84.0(10) . . ? C29A C30 C28B 143.9(9) . . ? C29B C30 C28B 111.4(9) . . ? C31 C30 C28B 105.9(7) . . ? C27B C30 C28B 111.3(10) . . ? C28 C30 C28B 28.0(6) . . ? C28A C30 C28B 54.8(7) . . ? C27 C30 C27A 27.6(9) . . ? C29A C30 C27A 109.9(10) . . ? C29B C30 C27A 55.0(8) . . ? C31 C30 C27A 109.8(8) . . ? C27B C30 C27A 136.4(10) . . ? C28 C30 C27A 83.7(10) . . ? C28A C30 C27A 108.0(10) . . ? C28B C30 C27A 57.0(9) . . ? C27 C30 C29 107.6(11) . . ? C29A C30 C29 28.5(7) . . ? C29B C30 C29 88.0(9) . . ? C31 C30 C29 115.1(7) . . ? C27B C30 C29 23.5(8) . . ? C28 C30 C29 107.3(10) . . ? C28A C30 C29 83.1(10) . . ? C28B C30 C29 128.7(10) . . ? C27A C30 C29 127.3(9) . . ? O5 C31 C32 122.9(3) . . ? O5 C31 C30 116.6(3) . . ? C32 C31 C30 120.5(3) . . ? C33 C32 C31 124.1(3) . . ? C33 C32 H32 118.0 . . ? C31 C32 H32 118.0 . . ? O6 C33 C32 124.4(3) . . ? O6 C33 C34 114.7(3) . . ? C32 C33 C34 120.9(3) . . ? C39 C34 C35 118.4(3) . . ? C39 C34 C33 120.6(3) . . ? C35 C34 C33 121.0(3) . . ? C36 C35 C34 120.0(4) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 121.0(4) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C38 C37 C36 118.4(3) . . ? C38 C37 C37 120.6(4) . 2_655 ? C36 C37 C37 120.9(4) . 2_655 ? C39 C38 C37 120.0(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C34 C39 C38 122.1(3) . . ? C34 C39 H39 118.9 . . ? C38 C39 H39 118.9 . . ? C40 O7 C41 98.5(17) . . ? O7 C41 C42 92(2) . . ? O7 C41 H41A 113.3 . . ? C42 C41 H41A 113.3 . . ? O7 C41 H41B 113.3 . . ? C42 C41 H41B 113.3 . . ? H41A C41 H41B 110.6 . . ? C43 C42 C41 102(3) . . ? C43 C42 H42A 111.5 . . ? C41 C42 H42A 111.5 . . ? C43 C42 H42B 111.5 . . ? C41 C42 H42B 111.5 . . ? H42A C42 H42B 109.3 . . ? O7 C40 C43 90.1(19) . . ? O7 C40 H40A 113.6 . . ? C43 C40 H40A 113.6 . . ? O7 C40 H40B 113.6 . . ? C43 C40 H40B 113.6 . . ? H40A C40 H40B 110.9 . . ? C42 C43 C40 120(3) . . ? C42 C43 H43A 107.3 . . ? C40 C43 H43A 107.3 . . ? C42 C43 H43B 107.3 . . ? C40 C43 H43B 107.3 . . ? H43A C43 H43B 106.9 . . ? C43A O7A C41A 112.6(9) . . ? C42A C40A C41A 100.8(12) . . ? C42A C40A H40C 111.6 . . ? C41A C40A H40C 111.6 . . ? C42A C40A H40D 111.6 . . ? C41A C40A H40D 111.6 . . ? H40C C40A H40D 109.4 . . ? O7A C41A C40A 95.4(8) . . ? O7A C41A H41C 112.7 . . ? C40A C41A H41C 112.7 . . ? O7A C41A H41D 112.7 . . ? C40A C41A H41D 112.7 . . ? H41C C41A H41D 110.2 . . ? C43A C42A C40A 97.8(11) . . ? C43A C42A H42C 112.2 . . ? C40A C42A H42C 112.2 . . ? C43A C42A H42D 112.2 . . ? C40A C42A H42D 112.2 . . ? H42C C42A H42D 109.8 . . ? O7A C43A C42A 98.4(12) . . ? O7A C43A H43C 112.1 . . ? C42A C43A H43C 112.1 . . ? O7A C43A H43D 112.1 . . ? C42A C43A H43D 112.1 . . ? H43C C43A H43D 109.7 . . ? C5 O1 Fe1 127.7(2) . . ? C7 O2 Fe1 130.4(2) . . ? C20 O3 Fe1 124.2(2) . 11_666 ? C22 O4 Fe1 124.8(2) . 11_666 ? C31 O5 Fe1 131.1(2) . . ? C33 O6 Fe1 130.2(2) . . ? O2 Fe1 O3 88.96(10) . 12_656 ? O2 Fe1 O5 95.65(10) . . ? O3 Fe1 O5 172.93(10) 12_656 . ? O2 Fe1 O1 86.43(9) . . ? O3 Fe1 O1 98.32(9) 12_656 . ? O5 Fe1 O1 87.34(9) . . ? O2 Fe1 O6 88.76(10) . . ? O3 Fe1 O6 88.48(9) 12_656 . ? O5 Fe1 O6 86.27(9) . . ? O1 Fe1 O6 171.58(10) . . ? O2 Fe1 O4 173.46(10) . 12_656 ? O3 Fe1 O4 84.71(9) 12_656 12_656 ? O5 Fe1 O4 90.51(10) . 12_656 ? O1 Fe1 O4 96.10(9) . 12_656 ? O6 Fe1 O4 89.44(9) . 12_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C4 C5 O1 -23.3(5) . . . . ? C2 C4 C5 O1 -150.3(4) . . . . ? C1 C4 C5 O1 94.4(4) . . . . ? C3 C4 C5 C6 156.5(4) . . . . ? C2 C4 C5 C6 29.5(6) . . . . ? C1 C4 C5 C6 -85.8(4) . . . . ? O1 C5 C6 C7 -0.7(6) . . . . ? C4 C5 C6 C7 179.5(4) . . . . ? C5 C6 C7 O2 -4.6(6) . . . . ? C5 C6 C7 C8 176.5(3) . . . . ? O2 C7 C8 C9 173.0(3) . . . . ? C6 C7 C8 C9 -8.0(6) . . . . ? O2 C7 C8 C13 -8.0(5) . . . . ? C6 C7 C8 C13 171.0(4) . . . . ? C13 C8 C9 C10 -0.2(6) . . . . ? C7 C8 C9 C10 178.8(3) . . . . ? C8 C9 C10 C11 -0.9(6) . . . . ? C9 C10 C11 C12 0.7(6) . . . . ? C9 C10 C11 C14 -176.7(4) . . . . ? C10 C11 C12 C13 0.5(8) . . . . ? C14 C11 C12 C13 178.0(5) . . . . ? C11 C12 C13 C8 -1.6(8) . . . . ? C9 C8 C13 C12 1.4(7) . . . . ? C7 C8 C13 C12 -177.7(4) . . . . ? C10 C11 C14 C15 -32.2(6) . . . . ? C12 C11 C14 C15 150.5(4) . . . . ? C10 C11 C14 C19 146.6(4) . . . . ? C12 C11 C14 C19 -30.8(6) . . . . ? C19 C14 C15 C16 3.1(6) . . . . ? C11 C14 C15 C16 -178.1(4) . . . . ? C14 C15 C16 C17 -0.2(6) . . . . ? C15 C16 C17 C18 -1.3(6) . . . . ? C15 C16 C17 C20 176.6(3) . . . . ? C16 C17 C18 C19 -0.3(6) . . . . ? C20 C17 C18 C19 -178.3(4) . . . . ? C17 C18 C19 C14 3.3(8) . . . . ? C15 C14 C19 C18 -4.7(7) . . . . ? C11 C14 C19 C18 176.5(4) . . . . ? C18 C17 C20 O3 -18.9(5) . . . . ? C16 C17 C20 O3 163.2(3) . . . . ? C18 C17 C20 C21 162.3(4) . . . . ? C16 C17 C20 C21 -15.6(5) . . . . ? O3 C20 C21 C22 -0.2(5) . . . . ? C17 C20 C21 C22 178.4(3) . . . . ? C20 C21 C22 O4 1.4(6) . . . . ? C20 C21 C22 C23 -179.2(3) . . . . ? O4 C22 C23 C25 -2.7(5) . . . . ? C21 C22 C23 C25 177.9(4) . . . . ? O4 C22 C23 C24 121.8(4) . . . . ? C21 C22 C23 C24 -57.7(5) . . . . ? O4 C22 C23 C26 -121.6(4) . . . . ? C21 C22 C23 C26 59.0(5) . . . . ? C27 C30 C31 O5 -34.6(10) . . . . ? C29A C30 C31 O5 -126.4(7) . . . . ? C29B C30 C31 O5 -62.6(7) . . . . ? C27B C30 C31 O5 177.3(8) . . . . ? C28 C30 C31 O5 84.0(8) . . . . ? C28A C30 C31 O5 112.3(7) . . . . ? C28B C30 C31 O5 54.9(7) . . . . ? C27A C30 C31 O5 -5.2(9) . . . . ? C29 C30 C31 O5 -156.9(8) . . . . ? C27 C30 C31 C32 146.5(9) . . . . ? C29A C30 C31 C32 54.8(8) . . . . ? C29B C30 C31 C32 118.5(7) . . . . ? C27B C30 C31 C32 -1.5(9) . . . . ? C28 C30 C31 C32 -94.8(8) . . . . ? C28A C30 C31 C32 -66.5(8) . . . . ? C28B C30 C31 C32 -124.0(7) . . . . ? C27A C30 C31 C32 175.9(8) . . . . ? C29 C30 C31 C32 24.2(9) . . . . ? O5 C31 C32 C33 4.3(6) . . . . ? C30 C31 C32 C33 -177.0(3) . . . . ? C31 C32 C33 O6 -6.5(6) . . . . ? C31 C32 C33 C34 177.6(3) . . . . ? O6 C33 C34 C39 -21.4(5) . . . . ? C32 C33 C34 C39 154.9(4) . . . . ? O6 C33 C34 C35 155.8(4) . . . . ? C32 C33 C34 C35 -28.0(6) . . . . ? C39 C34 C35 C36 1.0(7) . . . . ? C33 C34 C35 C36 -176.2(4) . . . . ? C34 C35 C36 C37 -0.6(7) . . . . ? C35 C36 C37 C38 -0.5(7) . . . . ? C35 C36 C37 C37 177.6(3) . . . 2_655 ? C36 C37 C38 C39 1.3(6) . . . . ? C37 C37 C38 C39 -176.8(3) 2_655 . . . ? C35 C34 C39 C38 -0.2(6) . . . . ? C33 C34 C39 C38 177.0(4) . . . . ? C37 C38 C39 C34 -1.0(7) . . . . ? C40 O7 C41 C42 56(3) . . . . ? O7 C41 C42 C43 -29(3) . . . . ? C41 O7 C40 C43 -54(3) . . . . ? C41 C42 C43 C40 -5(4) . . . . ? O7 C40 C43 C42 42(4) . . . . ? C43A O7A C41A C40A -16(3) . . . . ? C42A C40A C41A O7A 45(2) . . . . ? C41A C40A C42A C43A -60(2) . . . . ? C41A O7A C43A C42A -19(3) . . . . ? C40A C42A C43A O7A 46(2) . . . . ? C6 C5 O1 Fe1 20.1(5) . . . . ? C4 C5 O1 Fe1 -160.2(2) . . . . ? C6 C7 O2 Fe1 -10.3(5) . . . . ? C8 C7 O2 Fe1 168.7(2) . . . . ? C21 C20 O3 Fe1 -28.8(4) . . . 11_666 ? C17 C20 O3 Fe1 152.5(2) . . . 11_666 ? C21 C22 O4 Fe1 26.2(5) . . . 11_666 ? C23 C22 O4 Fe1 -153.2(3) . . . 11_666 ? C32 C31 O5 Fe1 6.7(5) . . . . ? C30 C31 O5 Fe1 -172.1(2) . . . . ? C32 C33 O6 Fe1 -2.2(5) . . . . ? C34 C33 O6 Fe1 173.9(2) . . . . ? C7 O2 Fe1 O3 118.4(3) . . . 12_656 ? C7 O2 Fe1 O5 -66.9(3) . . . . ? C7 O2 Fe1 O1 20.0(3) . . . . ? C7 O2 Fe1 O6 -153.1(3) . . . . ? C7 O2 Fe1 O4 133.0(8) . . . 12_656 ? C31 O5 Fe1 O2 -99.1(3) . . . . ? C31 O5 Fe1 O3 31.4(9) . . . 12_656 ? C31 O5 Fe1 O1 174.8(3) . . . . ? C31 O5 Fe1 O6 -10.7(3) . . . . ? C31 O5 Fe1 O4 78.7(3) . . . 12_656 ? C5 O1 Fe1 O2 -24.5(3) . . . . ? C5 O1 Fe1 O3 -112.9(3) . . . 12_656 ? C5 O1 Fe1 O5 71.3(3) . . . . ? C5 O1 Fe1 O6 30.7(8) . . . . ? C5 O1 Fe1 O4 161.6(3) . . . 12_656 ? C33 O6 Fe1 O2 104.1(3) . . . . ? C33 O6 Fe1 O3 -166.9(3) . . . 12_656 ? C33 O6 Fe1 O5 8.4(3) . . . . ? C33 O6 Fe1 O1 49.1(8) . . . . ? C33 O6 Fe1 O4 -82.2(3) . . . 12_656 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.901 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.069