# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Robert Wolf' _publ_contact_author_email R.WOLF@UNI-MUENSTER.DE _publ_section_title ; A reactive iron napthalene complex provides convenient access to the Cp*Fe(-) synthon (Cp* = C5Me5) ; loop_ _publ_author_name 'Robert Wolf' 'Eva-Maria Schnockelborg' # Attachment 'subm1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 758967' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H45 Fe K O6' _chemical_formula_weight 620.63 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' 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 P2(1)/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 11.3254(9) _cell_length_b 19.2204(16) _cell_length_c 14.9090(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.0420(10) _cell_angle_gamma 90.00 _cell_volume 3174.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9613 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 30.36 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9092 _exptl_absorpt_correction_T_max 0.9872 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.838256 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31912 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 27.88 _reflns_number_total 7537 _reflns_number_gt 6183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _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^)+(0.0596P)^2^+2.0657P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7537 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.004 _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 -0.10825(17) 0.32673(10) 0.52546(14) 0.0247(4) Uani 1 1 d . . . C2 C -0.02104(18) 0.32407(11) 0.46811(14) 0.0292(4) Uani 1 1 d . . . C3 C 0.0552(2) 0.26500(12) 0.49487(17) 0.0379(5) Uani 1 1 d . . . C4 C 0.0151(2) 0.23198(11) 0.56940(19) 0.0399(6) Uani 1 1 d . . . C5 C -0.08582(18) 0.27017(11) 0.58821(16) 0.0324(5) Uani 1 1 d . . . C6 C -0.20724(19) 0.37927(11) 0.51923(16) 0.0326(5) Uani 1 1 d . . . H6A H -0.2797 0.3625 0.4768 0.049 Uiso 1 1 calc R . . H6B H -0.1815 0.4235 0.4967 0.049 Uiso 1 1 calc R . . H6C H -0.2254 0.3862 0.5801 0.049 Uiso 1 1 calc R . . C7 C -0.0108(2) 0.37420(16) 0.39339(16) 0.0451(6) Uani 1 1 d . . . H7A H 0.0746 0.3819 0.3928 0.068 Uiso 1 1 calc R . . H7B H -0.0483 0.4185 0.4042 0.068 Uiso 1 1 calc R . . H7C H -0.0519 0.3551 0.3342 0.068 Uiso 1 1 calc R . . C8 C 0.1567(3) 0.2424(2) 0.4502(2) 0.0707(11) Uani 1 1 d . . . H8A H 0.2337 0.2588 0.4868 0.106 Uiso 1 1 calc R . . H8B H 0.1445 0.2622 0.3884 0.106 Uiso 1 1 calc R . . H8C H 0.1578 0.1915 0.4463 0.106 Uiso 1 1 calc R . . C9 C 0.0672(3) 0.16701(13) 0.6189(3) 0.0668(10) Uani 1 1 d . . . H9A H 0.0256 0.1262 0.5880 0.100 Uiso 1 1 calc R . . H9B H 0.0565 0.1685 0.6824 0.100 Uiso 1 1 calc R . . H9C H 0.1535 0.1641 0.6184 0.100 Uiso 1 1 calc R . . C10 C -0.1573(2) 0.25319(16) 0.6598(2) 0.0544(8) Uani 1 1 d . . . H10A H -0.1872 0.2963 0.6822 0.082 Uiso 1 1 calc R . . H10B H -0.1056 0.2287 0.7110 0.082 Uiso 1 1 calc R . . H10C H -0.2258 0.2234 0.6328 0.082 Uiso 1 1 calc R . . C11 C 0.15772(17) 0.42495(10) 0.59800(14) 0.0248(4) Uani 1 1 d . . . C12 C 0.09416(19) 0.41965(11) 0.67229(15) 0.0295(4) Uani 1 1 d . . . C13 C 0.1268(2) 0.36188(12) 0.73003(15) 0.0328(5) Uani 1 1 d . . . C14 C 0.21733(19) 0.31645(11) 0.70587(14) 0.0286(4) Uani 1 1 d . . . C20 C 0.31668(17) 0.34597(10) 0.66953(13) 0.0236(4) Uani 1 1 d . . . C19 C 0.28535(17) 0.40546(10) 0.61300(13) 0.0227(4) Uani 1 1 d . . . C15 C 0.43217(18) 0.31832(11) 0.67938(15) 0.0304(4) Uani 1 1 d . . . H17 H 0.4549 0.2794 0.7184 0.036 Uiso 1 1 calc R . . C16 C 0.51581(19) 0.34735(12) 0.63209(17) 0.0353(5) Uani 1 1 d . . . H18 H 0.5929 0.3264 0.6367 0.042 Uiso 1 1 calc R . . C17 C 0.48610(19) 0.40575(12) 0.57942(16) 0.0343(5) Uani 1 1 d . . . H19 H 0.5431 0.4258 0.5485 0.041 Uiso 1 1 calc R . . C18 C 0.37103(18) 0.43594(11) 0.57118(14) 0.0289(4) Uani 1 1 d . . . H20 H 0.3519 0.4775 0.5367 0.035 Uiso 1 1 calc R . . C21 C 0.5564(4) 0.62856(16) 0.7094(3) 0.0787(12) Uani 1 1 d . . . H21A H 0.5878 0.6564 0.7651 0.094 Uiso 1 1 calc R . . H21B H 0.5239 0.6610 0.6586 0.094 Uiso 1 1 calc R . . C22 C 0.6554(4) 0.58659(18) 0.6855(2) 0.0740(11) Uani 1 1 d . . . H22A H 0.6235 0.5581 0.6304 0.089 Uiso 1 1 calc R . . H22B H 0.7185 0.6178 0.6713 0.089 Uiso 1 1 calc R . . C23 C 0.8081(3) 0.50726(19) 0.7445(3) 0.0677(9) Uani 1 1 d . . . H23A H 0.8717 0.5413 0.7385 0.081 Uiso 1 1 calc R . . H23B H 0.7868 0.4806 0.6866 0.081 Uiso 1 1 calc R . . C24 C 0.8534(2) 0.45976(18) 0.8211(3) 0.0668(10) Uani 1 1 d . . . H24A H 0.9287 0.4373 0.8121 0.080 Uiso 1 1 calc R . . H24B H 0.8721 0.4864 0.8792 0.080 Uiso 1 1 calc R . . C25 C 0.8066(3) 0.35449(18) 0.8912(3) 0.0725(11) Uani 1 1 d . . . H25A H 0.8418 0.3753 0.9515 0.087 Uiso 1 1 calc R . . H25B H 0.8700 0.3268 0.8709 0.087 Uiso 1 1 calc R . . C26 C 0.7039(4) 0.30916(15) 0.8991(3) 0.0768(12) Uani 1 1 d . . . H26A H 0.6659 0.2901 0.8382 0.092 Uiso 1 1 calc R . . H26B H 0.7322 0.2698 0.9409 0.092 Uiso 1 1 calc R . . C27 C 0.5251(4) 0.3111(2) 0.9576(3) 0.0879(15) Uani 1 1 d . . . H27A H 0.5589 0.2731 1.0001 0.105 Uiso 1 1 calc R . . H27B H 0.4746 0.2903 0.9018 0.105 Uiso 1 1 calc R . . C28 C 0.4519(4) 0.3586(3) 1.0022(2) 0.0873(15) Uani 1 1 d . . . H28A H 0.3912 0.3316 1.0267 0.105 Uiso 1 1 calc R . . H28B H 0.5045 0.3832 1.0538 0.105 Uiso 1 1 calc R . . C29 C 0.3279(4) 0.4577(2) 0.9729(3) 0.0867(14) Uani 1 1 d . . . H29A H 0.3839 0.4880 1.0158 0.104 Uiso 1 1 calc R . . H29B H 0.2728 0.4348 1.0073 0.104 Uiso 1 1 calc R . . C30 C 0.2579(3) 0.4996(2) 0.8971(3) 0.0793(13) Uani 1 1 d . . . H30A H 0.2049 0.4687 0.8530 0.095 Uiso 1 1 calc R . . H30B H 0.2062 0.5331 0.9216 0.095 Uiso 1 1 calc R . . C31 C 0.2781(3) 0.57204(18) 0.7725(3) 0.0724(11) Uani 1 1 d . . . C32 C 0.3647(3) 0.62138(16) 0.7455(2) 0.0725(11) Uani 1 1 d . . . H32A H 0.3240 0.6482 0.6911 0.087 Uiso 1 1 calc R . . H32B H 0.3931 0.6546 0.7962 0.087 Uiso 1 1 calc R . . Fe1 Fe 0.06675(2) 0.331623(14) 0.602022(19) 0.02172(9) Uani 1 1 d . . . K1 K 0.51665(4) 0.45113(2) 0.79595(3) 0.02940(11) Uani 1 1 d . . . O1 O 0.4655(2) 0.58464(9) 0.72479(14) 0.0595(6) Uani 1 1 d . . . O2 O 0.70663(19) 0.54212(10) 0.76066(13) 0.0528(5) Uani 1 1 d . . . O3 O 0.76477(17) 0.40753(10) 0.82669(15) 0.0559(5) Uani 1 1 d . . . O4 O 0.6183(2) 0.35040(10) 0.93448(15) 0.0645(6) Uani 1 1 d . . . O5 O 0.3926(2) 0.40798(14) 0.93569(13) 0.0664(7) Uani 1 1 d . . . O6 O 0.33833(17) 0.53651(12) 0.85116(14) 0.0587(6) Uani 1 1 d . . . H11 H 0.130(2) 0.4587(12) 0.5550(15) 0.022(5) Uiso 1 1 d . . . H14 H 0.235(2) 0.2727(13) 0.7381(16) 0.026(6) Uiso 1 1 d . . . H12 H 0.029(2) 0.4527(13) 0.6764(17) 0.035(6) Uiso 1 1 d . . . H13 H 0.085(2) 0.3505(15) 0.7807(19) 0.045(7) Uiso 1 1 d . . . 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 0.0193(9) 0.0218(9) 0.0314(10) -0.0007(7) 0.0014(7) -0.0021(7) C2 0.0223(9) 0.0351(11) 0.0282(10) -0.0081(8) 0.0009(8) 0.0003(8) C3 0.0257(10) 0.0379(12) 0.0460(13) -0.0192(10) -0.0019(9) 0.0056(9) C4 0.0283(11) 0.0202(10) 0.0624(16) -0.0036(10) -0.0104(10) 0.0005(8) C5 0.0220(9) 0.0240(10) 0.0474(13) 0.0070(9) -0.0014(9) -0.0065(8) C6 0.0247(10) 0.0319(11) 0.0409(12) 0.0022(9) 0.0060(9) 0.0051(8) C7 0.0379(13) 0.0707(18) 0.0263(11) 0.0031(11) 0.0059(9) -0.0015(12) C8 0.0434(16) 0.091(2) 0.075(2) -0.0448(19) 0.0058(15) 0.0231(16) C9 0.0479(16) 0.0230(12) 0.113(3) 0.0046(14) -0.0204(17) 0.0047(11) C10 0.0336(13) 0.0605(17) 0.0666(18) 0.0333(14) 0.0049(12) -0.0133(12) C11 0.0217(9) 0.0211(9) 0.0307(10) 0.0004(8) 0.0036(8) -0.0003(7) C12 0.0245(10) 0.0308(10) 0.0348(11) -0.0106(8) 0.0096(8) -0.0033(8) C13 0.0327(11) 0.0429(12) 0.0244(10) -0.0037(9) 0.0097(8) -0.0094(9) C14 0.0278(10) 0.0294(10) 0.0263(10) 0.0056(8) 0.0003(8) -0.0044(8) C20 0.0224(9) 0.0224(9) 0.0238(9) -0.0030(7) -0.0003(7) -0.0037(7) C19 0.0210(9) 0.0221(9) 0.0242(9) -0.0027(7) 0.0030(7) -0.0027(7) C15 0.0255(10) 0.0235(9) 0.0374(11) -0.0008(8) -0.0042(8) 0.0012(8) C16 0.0214(10) 0.0350(11) 0.0484(13) -0.0106(10) 0.0048(9) 0.0025(8) C17 0.0255(10) 0.0398(12) 0.0408(12) -0.0061(10) 0.0139(9) -0.0057(9) C18 0.0268(10) 0.0285(10) 0.0317(10) 0.0011(8) 0.0071(8) -0.0033(8) C21 0.142(4) 0.0318(15) 0.062(2) 0.0110(14) 0.021(2) -0.0028(19) C22 0.119(3) 0.0583(19) 0.0534(18) 0.0108(15) 0.037(2) -0.024(2) C23 0.069(2) 0.070(2) 0.077(2) -0.0248(18) 0.0439(18) -0.0174(17) C24 0.0310(13) 0.075(2) 0.099(3) -0.038(2) 0.0229(15) -0.0048(13) C25 0.067(2) 0.0600(19) 0.074(2) -0.0194(17) -0.0228(17) 0.0311(17) C26 0.102(3) 0.0287(13) 0.078(2) 0.0035(14) -0.033(2) 0.0208(16) C27 0.124(4) 0.064(2) 0.057(2) 0.0268(18) -0.023(2) -0.050(2) C28 0.088(3) 0.128(4) 0.0381(16) 0.022(2) -0.0065(17) -0.076(3) C29 0.078(2) 0.135(4) 0.056(2) -0.046(2) 0.0355(19) -0.061(3) C30 0.0413(16) 0.103(3) 0.101(3) -0.063(2) 0.0329(18) -0.0218(17) C31 0.0539(18) 0.0560(18) 0.089(2) -0.0343(17) -0.0280(17) 0.0234(15) C32 0.094(3) 0.0432(16) 0.0618(19) -0.0117(14) -0.0254(18) 0.0374(17) Fe1 0.01818(14) 0.02080(14) 0.02566(15) -0.00077(10) 0.00336(10) -0.00197(10) K1 0.0334(2) 0.0240(2) 0.0298(2) -0.00085(16) 0.00422(18) 0.00146(17) O1 0.0947(16) 0.0274(9) 0.0492(11) -0.0022(8) -0.0019(11) 0.0074(10) O2 0.0685(13) 0.0463(10) 0.0528(11) -0.0130(9) 0.0341(10) -0.0161(9) O3 0.0389(10) 0.0503(11) 0.0715(13) -0.0144(10) -0.0041(9) 0.0123(8) O4 0.0852(16) 0.0363(10) 0.0597(13) 0.0135(9) -0.0132(11) -0.0171(10) O5 0.0631(13) 0.1012(18) 0.0352(10) -0.0149(11) 0.0114(9) -0.0378(12) O6 0.0343(9) 0.0751(14) 0.0614(12) -0.0347(11) -0.0019(9) 0.0032(9) _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 C5 1.422(3) . ? C1 C2 1.436(3) . ? C1 C6 1.497(3) . ? C1 Fe1 2.0727(19) . ? C2 C3 1.432(3) . ? C2 C7 1.496(3) . ? C2 Fe1 2.041(2) . ? C3 C4 1.433(4) . ? C3 C8 1.508(4) . ? C3 Fe1 2.030(2) . ? C4 C5 1.435(3) . ? C4 C9 1.507(3) . ? C4 Fe1 2.032(2) . ? C5 C10 1.504(4) . ? C5 Fe1 2.068(2) . ? C11 C12 1.445(3) . ? C11 C19 1.465(3) . ? C12 C13 1.406(3) . ? C12 Fe1 1.980(2) . ? C13 C14 1.448(3) . ? C13 Fe1 1.975(2) . ? C14 C20 1.461(3) . ? C20 C15 1.391(3) . ? C20 C19 1.421(3) . ? C19 C18 1.388(3) . ? C15 C16 1.409(3) . ? C16 C17 1.371(3) . ? C17 C18 1.408(3) . ? C21 O1 1.387(4) . ? C21 C22 1.483(6) . ? C22 O2 1.432(4) . ? C23 O2 1.394(4) . ? C23 C24 1.469(5) . ? C24 O3 1.434(4) . ? C25 O3 1.413(4) . ? C25 C26 1.478(6) . ? C26 O4 1.435(5) . ? C27 O4 1.398(4) . ? C27 C28 1.481(6) . ? C28 O5 1.434(5) . ? C29 O5 1.389(5) . ? C29 C30 1.477(6) . ? C30 O6 1.436(4) . ? C31 O6 1.405(4) . ? C31 C32 1.478(6) . ? C32 O1 1.430(4) . ? K1 O1 2.7909(19) . ? K1 O6 2.8535(19) . ? K1 O5 2.868(2) . ? K1 O3 2.8760(19) . ? K1 O4 2.889(2) . ? K1 O2 2.9046(19) . ? 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 C5 C1 C2 108.29(18) . . ? C5 C1 C6 125.81(19) . . ? C2 C1 C6 125.89(18) . . ? C5 C1 Fe1 69.72(11) . . ? C2 C1 Fe1 68.41(11) . . ? C6 C1 Fe1 128.40(14) . . ? C3 C2 C1 108.2(2) . . ? C3 C2 C7 125.6(2) . . ? C1 C2 C7 126.2(2) . . ? C3 C2 Fe1 69.00(12) . . ? C1 C2 Fe1 70.75(11) . . ? C7 C2 Fe1 125.80(16) . . ? C2 C3 C4 107.3(2) . . ? C2 C3 C8 125.2(3) . . ? C4 C3 C8 127.5(3) . . ? C2 C3 Fe1 69.83(12) . . ? C4 C3 Fe1 69.40(13) . . ? C8 C3 Fe1 126.81(18) . . ? C3 C4 C5 108.60(19) . . ? C3 C4 C9 126.3(3) . . ? C5 C4 C9 125.1(3) . . ? C3 C4 Fe1 69.29(12) . . ? C5 C4 Fe1 70.86(12) . . ? C9 C4 Fe1 126.91(18) . . ? C1 C5 C4 107.6(2) . . ? C1 C5 C10 125.7(2) . . ? C4 C5 C10 126.6(2) . . ? C1 C5 Fe1 70.10(11) . . ? C4 C5 Fe1 68.17(12) . . ? C10 C5 Fe1 128.03(18) . . ? C12 C11 C19 119.91(18) . . ? C13 C12 C11 114.54(18) . . ? C13 C12 Fe1 68.98(12) . . ? C11 C12 Fe1 72.71(11) . . ? C12 C13 C14 115.67(19) . . ? C12 C13 Fe1 69.36(12) . . ? C14 C13 Fe1 72.61(12) . . ? C13 C14 C20 119.86(19) . . ? C15 C20 C19 118.88(18) . . ? C15 C20 C14 126.32(19) . . ? C19 C20 C14 114.59(17) . . ? C18 C19 C20 119.65(18) . . ? C18 C19 C11 125.72(18) . . ? C20 C19 C11 114.37(17) . . ? C20 C15 C16 120.8(2) . . ? C17 C16 C15 120.05(19) . . ? C16 C17 C18 120.0(2) . . ? C19 C18 C17 120.5(2) . . ? O1 C21 C22 109.4(3) . . ? O2 C22 C21 109.9(3) . . ? O2 C23 C24 109.3(3) . . ? O3 C24 C23 110.2(3) . . ? O3 C25 C26 108.8(2) . . ? O4 C26 C25 107.9(2) . . ? O4 C27 C28 107.4(3) . . ? O5 C28 C27 108.9(3) . . ? O5 C29 C30 108.2(3) . . ? O6 C30 C29 110.0(3) . . ? O6 C31 C32 107.8(2) . . ? O1 C32 C31 110.3(2) . . ? C13 Fe1 C12 41.66(10) . . ? C13 Fe1 C3 153.99(10) . . ? C12 Fe1 C3 158.84(10) . . ? C13 Fe1 C4 122.19(10) . . ? C12 Fe1 C4 159.66(11) . . ? C3 Fe1 C4 41.31(11) . . ? C13 Fe1 C2 164.83(9) . . ? C12 Fe1 C2 124.67(9) . . ? C3 Fe1 C2 41.17(9) . . ? C4 Fe1 C2 69.01(9) . . ? C13 Fe1 C5 112.12(9) . . ? C12 Fe1 C5 125.19(9) . . ? C3 Fe1 C5 69.26(10) . . ? C4 Fe1 C5 40.97(9) . . ? C2 Fe1 C5 68.63(9) . . ? C13 Fe1 C1 129.97(9) . . ? C12 Fe1 C1 110.88(8) . . ? C3 Fe1 C1 68.94(8) . . ? C4 Fe1 C1 68.35(8) . . ? C2 Fe1 C1 40.85(8) . . ? C5 Fe1 C1 40.18(8) . . ? O1 K1 O6 58.51(7) . . ? O1 K1 O5 116.60(8) . . ? O6 K1 O5 58.22(8) . . ? O1 K1 O3 116.55(7) . . ? O6 K1 O3 148.04(6) . . ? O5 K1 O3 114.24(7) . . ? O1 K1 O4 155.24(6) . . ? O6 K1 O4 112.31(7) . . ? O5 K1 O4 57.95(8) . . ? O3 K1 O4 57.35(7) . . ? O1 K1 O2 58.70(7) . . ? O6 K1 O2 107.55(6) . . ? O5 K1 O2 143.08(6) . . ? O3 K1 O2 57.88(6) . . ? O4 K1 O2 109.47(7) . . ? C21 O1 C32 112.9(3) . . ? C21 O1 K1 121.3(2) . . ? C32 O1 K1 118.9(2) . . ? C23 O2 C22 111.5(3) . . ? C23 O2 K1 114.24(18) . . ? C22 O2 K1 107.84(19) . . ? C25 O3 C24 113.9(3) . . ? C25 O3 K1 119.7(2) . . ? C24 O3 K1 117.33(17) . . ? C27 O4 C26 113.2(3) . . ? C27 O4 K1 109.3(2) . . ? C26 O4 K1 107.82(18) . . ? C29 O5 C28 112.9(3) . . ? C29 O5 K1 118.1(2) . . ? C28 O5 K1 117.6(2) . . ? C31 O6 C30 113.1(3) . . ? C31 O6 K1 106.75(18) . . ? C30 O6 K1 114.27(19) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.631 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.061 data_2 _database_code_depnum_ccdc_archive 'CCDC 758968' #TrackingRef 'subm1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H59 Fe K O6' _chemical_formula_weight 850.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0892(2) _cell_length_b 12.3239(3) _cell_length_c 18.1483(4) _cell_angle_alpha 94.894(2) _cell_angle_beta 102.909(2) _cell_angle_gamma 96.094(2) _cell_volume 2173.19(8) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7311 _cell_measurement_theta_min 0.86 _cell_measurement_theta_max 71.59 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 4.027 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7132 _exptl_absorpt_correction_T_max 0.9238 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.772893 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator goebel-mirror _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12862 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0773 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 71.59 _reflns_number_total 7311 _reflns_number_gt 5028 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; The hydrogens on C8, C112 and C113 were located on the Fourier difference map and refined freely. The data completeness is low due to technical reasons. 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^)+(0.0347P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7311 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.884 _refine_ls_shift/su_max 0.001 _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 0.5424(3) 0.5348(2) 0.17747(15) 0.0242(6) Uani 1 1 d . . . C2 C 0.6089(3) 0.5187(2) 0.25351(15) 0.0244(6) Uani 1 1 d . . . C3 C 0.5076(3) 0.4674(2) 0.28770(15) 0.0269(6) Uani 1 1 d . . . C4 C 0.3787(3) 0.4511(2) 0.23266(16) 0.0268(6) Uani 1 1 d . . . C5 C 0.4011(3) 0.4928(2) 0.16494(15) 0.0255(6) Uani 1 1 d . . . C6 C 0.6076(3) 0.5857(2) 0.11954(16) 0.0317(7) Uani 1 1 d . . . H6A H 0.6883 0.6347 0.1451 0.048 Uiso 1 1 calc R . . H6B H 0.5438 0.6259 0.0890 0.048 Uiso 1 1 calc R . . H6C H 0.6323 0.5289 0.0875 0.048 Uiso 1 1 calc R . . C7 C 0.7593(3) 0.5448(2) 0.29185(17) 0.0358(7) Uani 1 1 d . . . H7A H 0.8059 0.5849 0.2599 0.054 Uiso 1 1 calc R . . H7B H 0.7979 0.4778 0.3003 0.054 Uiso 1 1 calc R . . H7C H 0.7699 0.5885 0.3397 0.054 Uiso 1 1 calc R . . C8 C 0.5389(4) 0.4267(3) 0.3646(2) 0.0406(8) Uani 1 1 d . . . C9 C 0.2445(3) 0.3957(2) 0.24254(18) 0.0409(8) Uani 1 1 d . . . H9A H 0.1702 0.4246 0.2107 0.061 Uiso 1 1 calc R . . H9B H 0.2399 0.4091 0.2947 0.061 Uiso 1 1 calc R . . H9C H 0.2379 0.3181 0.2285 0.061 Uiso 1 1 calc R . . C10 C 0.2941(3) 0.4890(2) 0.09159(16) 0.0355(7) Uani 1 1 d . . . H10A H 0.3133 0.5525 0.0667 0.053 Uiso 1 1 calc R . . H10B H 0.2051 0.4882 0.1024 0.053 Uiso 1 1 calc R . . H10C H 0.2959 0.4238 0.0590 0.053 Uiso 1 1 calc R . . C11 C 0.4912(3) 0.7806(2) 0.25880(15) 0.0236(6) Uani 1 1 d . . . C12 C 0.5050(3) 0.7454(2) 0.33511(15) 0.0227(6) Uani 1 1 d . . . C13 C 0.3561(3) 0.7053(2) 0.31661(15) 0.0247(6) Uani 1 1 d . . . C14 C 0.3437(3) 0.7426(2) 0.24056(15) 0.0226(6) Uani 1 1 d . . . C15 C 0.2554(3) 1.0922(3) 0.04831(17) 0.0412(8) Uani 1 1 d . . . H15A H 0.2919 1.0231 0.0424 0.049 Uiso 1 1 calc R . . H15B H 0.1990 1.1036 -0.0005 0.049 Uiso 1 1 calc R . . C16 C 0.1709(3) 1.0883(3) 0.10612(18) 0.0461(8) Uani 1 1 d . . . H16A H 0.1327 1.1568 0.1114 0.055 Uiso 1 1 calc R . . H16B H 0.0957 1.0290 0.0902 0.055 Uiso 1 1 calc R . . C17 C 0.1811(3) 1.0548(3) 0.23298(19) 0.0433(8) Uani 1 1 d . . . H17A H 0.1016 1.0003 0.2127 0.052 Uiso 1 1 calc R . . H17B H 0.1494 1.1229 0.2483 0.052 Uiso 1 1 calc R . . C18 C 0.2719(3) 1.0167(2) 0.29997(19) 0.0453(9) Uani 1 1 d . . . H18A H 0.2206 1.0022 0.3381 0.054 Uiso 1 1 calc R . . H18B H 0.3043 0.9491 0.2844 0.054 Uiso 1 1 calc R . . C19 C 0.4731(3) 1.0626(3) 0.39562(18) 0.0473(9) Uani 1 1 d . . . H19A H 0.4952 0.9901 0.3817 0.057 Uiso 1 1 calc R . . H19B H 0.4258 1.0579 0.4365 0.057 Uiso 1 1 calc R . . C20 C 0.6013(3) 1.1404(3) 0.42199(17) 0.0467(9) Uani 1 1 d . . . H20A H 0.5800 1.2127 0.4371 0.056 Uiso 1 1 calc R . . H20B H 0.6602 1.1157 0.4656 0.056 Uiso 1 1 calc R . . C21 C 0.8010(3) 1.2071(3) 0.38422(18) 0.0461(9) Uani 1 1 d . . . H21A H 0.8565 1.1751 0.4255 0.055 Uiso 1 1 calc R . . H21B H 0.7927 1.2818 0.4026 0.055 Uiso 1 1 calc R . . C22 C 0.8683(3) 1.2080(3) 0.31920(17) 0.0417(8) Uani 1 1 d . . . H22A H 0.9600 1.2476 0.3357 0.050 Uiso 1 1 calc R . . H22B H 0.8755 1.1333 0.3002 0.050 Uiso 1 1 calc R . . C23 C 0.8588(3) 1.2806(3) 0.20241(18) 0.0411(8) Uani 1 1 d . . . H23A H 0.8850 1.2129 0.1820 0.049 Uiso 1 1 calc R . . H23B H 0.9413 1.3319 0.2231 0.049 Uiso 1 1 calc R . . C24 C 0.7647(3) 1.3284(2) 0.14041(17) 0.0365(7) Uani 1 1 d . . . H24A H 0.7338 1.3936 0.1613 0.044 Uiso 1 1 calc R . . H24B H 0.8126 1.3487 0.1019 0.044 Uiso 1 1 calc R . . C25 C 0.5570(3) 1.2843(2) 0.04733(17) 0.0374(7) Uani 1 1 d . . . H25A H 0.6027 1.3028 0.0075 0.045 Uiso 1 1 calc R . . H25B H 0.5226 1.3493 0.0657 0.045 Uiso 1 1 calc R . . C26 C 0.4414(3) 1.1947(2) 0.01666(16) 0.0382(8) Uani 1 1 d . . . H26A H 0.3830 1.2140 -0.0292 0.046 Uiso 1 1 calc R . . H26B H 0.4768 1.1272 0.0039 0.046 Uiso 1 1 calc R . . C111 C 0.5890(3) 0.8442(2) 0.22530(15) 0.0232(6) Uani 1 1 d . . . C112 C 0.5544(3) 0.9329(2) 0.18436(15) 0.0256(6) Uani 1 1 d . . . C113 C 0.6495(3) 0.9919(2) 0.15389(17) 0.0312(7) Uani 1 1 d . . . C114 C 0.7824(3) 0.9669(2) 0.16399(17) 0.0343(7) Uani 1 1 d . . . H114 H 0.8456 1.0067 0.1431 0.041 Uiso 1 1 calc R . . C115 C 0.8196(3) 0.8810(2) 0.20596(17) 0.0336(7) Uani 1 1 d . . . H115 H 0.9088 0.8635 0.2139 0.040 Uiso 1 1 calc R . . C116 C 0.7247(3) 0.8218(2) 0.23575(16) 0.0285(6) Uani 1 1 d . . . H116 H 0.7516 0.7649 0.2638 0.034 Uiso 1 1 calc R . . C121 C 0.6118(3) 0.7736(2) 0.40566(15) 0.0252(6) Uani 1 1 d . . . C122 C 0.6213(3) 0.7121(2) 0.46761(16) 0.0334(7) Uani 1 1 d . . . H122 H 0.5582 0.6501 0.4644 0.040 Uiso 1 1 calc R . . C123 C 0.7228(3) 0.7418(3) 0.53352(17) 0.0402(8) Uani 1 1 d . . . H123 H 0.7275 0.6995 0.5739 0.048 Uiso 1 1 calc R . . C124 C 0.8178(3) 0.8342(3) 0.53997(17) 0.0387(8) Uani 1 1 d . . . H124 H 0.8856 0.8541 0.5845 0.046 Uiso 1 1 calc R . . C125 C 0.8106(3) 0.8957(3) 0.48008(17) 0.0362(7) Uani 1 1 d . . . H125 H 0.8744 0.9575 0.4840 0.043 Uiso 1 1 calc R . . C126 C 0.7093(3) 0.8669(2) 0.41379(16) 0.0293(6) Uani 1 1 d . . . H126 H 0.7056 0.9100 0.3739 0.035 Uiso 1 1 calc R . . C131 C 0.2566(3) 0.6800(2) 0.36265(15) 0.0282(6) Uani 1 1 d . . . C132 C 0.1466(3) 0.7406(2) 0.36049(17) 0.0345(7) Uani 1 1 d . . . H132 H 0.1381 0.7980 0.3304 0.041 Uiso 1 1 calc R . . C133 C 0.0502(3) 0.7169(3) 0.40203(18) 0.0425(8) Uani 1 1 d . . . H133 H -0.0221 0.7584 0.3996 0.051 Uiso 1 1 calc R . . C134 C 0.0602(3) 0.6318(3) 0.44726(18) 0.0466(9) Uani 1 1 d . . . H134 H -0.0053 0.6155 0.4749 0.056 Uiso 1 1 calc R . . C135 C 0.1686(3) 0.5715(3) 0.45085(18) 0.0462(9) Uani 1 1 d . . . H135 H 0.1766 0.5146 0.4815 0.055 Uiso 1 1 calc R . . C136 C 0.2652(3) 0.5947(2) 0.40947(17) 0.0364(7) Uani 1 1 d . . . H136 H 0.3375 0.5531 0.4126 0.044 Uiso 1 1 calc R . . C141 C 0.2307(3) 0.7335(2) 0.17334(16) 0.0269(6) Uani 1 1 d . . . C142 C 0.2454(3) 0.7786(2) 0.10700(16) 0.0351(7) Uani 1 1 d . . . H142 H 0.3301 0.8154 0.1056 0.042 Uiso 1 1 calc R . . C143 C 0.1377(3) 0.7703(3) 0.04324(18) 0.0439(8) Uani 1 1 d . . . H143 H 0.1508 0.8022 0.0003 0.053 Uiso 1 1 calc R . . C144 C 0.0124(3) 0.7157(3) 0.04307(19) 0.0498(9) Uani 1 1 d . . . H144 H -0.0599 0.7105 0.0004 0.060 Uiso 1 1 calc R . . C145 C -0.0055(3) 0.6680(3) 0.1074(2) 0.0501(9) Uani 1 1 d . . . H145 H -0.0899 0.6294 0.1074 0.060 Uiso 1 1 calc R . . C146 C 0.1010(3) 0.6774(3) 0.17154(18) 0.0382(7) Uani 1 1 d . . . H146 H 0.0865 0.6460 0.2143 0.046 Uiso 1 1 calc R . . Fe1 Fe 0.45662(4) 0.61534(3) 0.25672(2) 0.02157(11) Uani 1 1 d . . . K1 K 0.50738(6) 1.20971(5) 0.22717(3) 0.03231(15) Uani 1 1 d . . . O1 O 0.3645(2) 1.17944(16) 0.07268(11) 0.0356(5) Uani 1 1 d . . . O2 O 0.25618(19) 1.07122(17) 0.17643(12) 0.0366(5) Uani 1 1 d . . . O3 O 0.3859(2) 1.09877(16) 0.33141(11) 0.0368(5) Uani 1 1 d . . . O4 O 0.6694(2) 1.14535(18) 0.36088(11) 0.0397(5) Uani 1 1 d . . . O5 O 0.78856(19) 1.25976(16) 0.26035(11) 0.0349(5) Uani 1 1 d . . . O6 O 0.6510(2) 1.24747(15) 0.10792(11) 0.0348(5) Uani 1 1 d . . . H113 H 0.626(3) 1.048(2) 0.1269(17) 0.046(9) Uiso 1 1 d . . . H112 H 0.465(3) 0.953(3) 0.1803(16) 0.046(9) Uiso 1 1 d . . . H8A H 0.583(3) 0.366(3) 0.3668(18) 0.055(11) Uiso 1 1 d . . . H8B H 0.461(3) 0.414(3) 0.3861(18) 0.052(11) Uiso 1 1 d . . . H8C H 0.596(4) 0.475(3) 0.403(2) 0.080(14) Uiso 1 1 d . . . 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 0.0242(15) 0.0221(13) 0.0286(15) 0.0030(12) 0.0104(12) 0.0043(11) C2 0.0199(14) 0.0189(13) 0.0340(16) 0.0018(12) 0.0052(12) 0.0040(11) C3 0.0320(16) 0.0201(13) 0.0288(15) 0.0045(12) 0.0057(13) 0.0059(12) C4 0.0300(16) 0.0173(12) 0.0339(16) -0.0007(12) 0.0123(13) -0.0009(11) C5 0.0268(15) 0.0225(13) 0.0275(15) 0.0008(12) 0.0071(12) 0.0051(12) C6 0.0316(17) 0.0285(15) 0.0368(17) 0.0031(14) 0.0119(14) 0.0042(13) C7 0.0270(16) 0.0309(15) 0.0467(19) 0.0012(15) 0.0018(14) 0.0085(13) C8 0.056(2) 0.0325(18) 0.037(2) 0.0115(17) 0.0105(18) 0.0179(18) C9 0.0391(19) 0.0342(16) 0.052(2) 0.0038(16) 0.0197(16) -0.0039(14) C10 0.0325(17) 0.0368(17) 0.0331(17) -0.0010(14) 0.0015(14) 0.0030(14) C11 0.0232(14) 0.0211(13) 0.0278(15) 0.0039(12) 0.0077(12) 0.0042(11) C12 0.0219(14) 0.0189(12) 0.0288(15) 0.0013(12) 0.0092(12) 0.0027(11) C13 0.0237(15) 0.0242(13) 0.0270(14) 0.0030(12) 0.0070(12) 0.0047(12) C14 0.0223(14) 0.0199(12) 0.0274(14) 0.0025(12) 0.0085(12) 0.0052(11) C15 0.0371(19) 0.0435(18) 0.0377(18) 0.0038(16) 0.0004(15) 0.0003(15) C16 0.0292(18) 0.052(2) 0.051(2) -0.0005(18) 0.0010(16) -0.0012(16) C17 0.0326(18) 0.0391(18) 0.062(2) 0.0016(18) 0.0248(17) -0.0031(15) C18 0.061(2) 0.0299(16) 0.058(2) 0.0100(17) 0.0395(19) 0.0049(16) C19 0.061(2) 0.049(2) 0.049(2) 0.0255(18) 0.0317(19) 0.0290(18) C20 0.064(2) 0.055(2) 0.0317(18) 0.0179(17) 0.0171(17) 0.0310(19) C21 0.046(2) 0.049(2) 0.0369(18) 0.0029(16) -0.0077(16) 0.0175(17) C22 0.0274(17) 0.0469(19) 0.0472(19) 0.0065(17) -0.0017(15) 0.0097(15) C23 0.0293(17) 0.0410(18) 0.057(2) 0.0044(17) 0.0186(16) 0.0027(14) C24 0.0380(18) 0.0318(16) 0.0448(19) 0.0078(15) 0.0198(15) 0.0024(14) C25 0.0459(19) 0.0347(16) 0.0359(17) 0.0127(15) 0.0145(15) 0.0070(15) C26 0.049(2) 0.0360(16) 0.0298(16) 0.0095(14) 0.0059(15) 0.0086(16) C111 0.0243(14) 0.0185(12) 0.0270(15) -0.0006(12) 0.0081(12) 0.0025(11) C112 0.0287(16) 0.0220(13) 0.0260(15) 0.0024(12) 0.0059(12) 0.0046(12) C113 0.0408(18) 0.0227(14) 0.0298(16) 0.0065(13) 0.0084(14) 0.0001(13) C114 0.0362(18) 0.0313(15) 0.0368(17) -0.0004(14) 0.0194(14) -0.0093(13) C115 0.0218(15) 0.0309(15) 0.0482(19) 0.0013(15) 0.0106(14) 0.0020(12) C116 0.0266(15) 0.0230(14) 0.0371(17) 0.0060(13) 0.0084(13) 0.0042(12) C121 0.0278(15) 0.0262(14) 0.0246(14) -0.0002(12) 0.0095(12) 0.0120(12) C122 0.0392(18) 0.0301(15) 0.0326(17) 0.0062(14) 0.0103(14) 0.0058(14) C123 0.051(2) 0.0462(19) 0.0259(16) 0.0079(15) 0.0083(15) 0.0180(17) C124 0.0329(18) 0.053(2) 0.0278(16) -0.0034(15) -0.0013(14) 0.0185(16) C125 0.0235(16) 0.0404(17) 0.0419(18) -0.0046(15) 0.0047(14) 0.0048(14) C126 0.0279(16) 0.0332(15) 0.0288(15) 0.0064(13) 0.0082(13) 0.0067(13) C131 0.0290(16) 0.0289(14) 0.0266(15) -0.0003(13) 0.0097(13) -0.0005(12) C132 0.0284(16) 0.0374(16) 0.0374(17) -0.0007(15) 0.0103(14) 0.0014(13) C133 0.0278(17) 0.056(2) 0.0429(19) -0.0078(18) 0.0122(15) 0.0020(15) C134 0.0332(19) 0.070(2) 0.0346(18) -0.0044(18) 0.0165(15) -0.0130(17) C135 0.043(2) 0.055(2) 0.0402(19) 0.0106(17) 0.0143(16) -0.0088(17) C136 0.0351(18) 0.0384(17) 0.0383(18) 0.0077(15) 0.0132(15) 0.0034(14) C141 0.0255(15) 0.0218(13) 0.0343(16) -0.0003(13) 0.0081(13) 0.0073(12) C142 0.0350(18) 0.0303(15) 0.0365(17) 0.0046(14) 0.0023(14) 0.0013(14) C143 0.052(2) 0.0368(17) 0.0356(18) 0.0044(15) -0.0047(16) 0.0067(17) C144 0.041(2) 0.056(2) 0.043(2) -0.0027(18) -0.0125(16) 0.0151(18) C145 0.0245(18) 0.065(2) 0.056(2) -0.008(2) 0.0066(16) 0.0034(16) C146 0.0246(16) 0.0513(19) 0.0381(18) -0.0016(16) 0.0096(14) 0.0024(14) Fe1 0.0208(2) 0.0189(2) 0.0262(2) 0.00455(19) 0.00690(18) 0.00314(17) K1 0.0282(3) 0.0391(4) 0.0300(3) 0.0044(3) 0.0080(3) 0.0029(3) O1 0.0391(13) 0.0341(11) 0.0318(11) 0.0043(10) 0.0063(10) -0.0002(10) O2 0.0275(11) 0.0410(12) 0.0427(12) 0.0065(11) 0.0122(10) 0.0015(10) O3 0.0459(13) 0.0303(11) 0.0418(12) 0.0139(10) 0.0196(10) 0.0113(10) O4 0.0413(13) 0.0496(13) 0.0304(11) 0.0074(11) 0.0081(10) 0.0138(11) O5 0.0249(11) 0.0389(11) 0.0411(12) 0.0091(10) 0.0047(9) 0.0083(9) O6 0.0398(12) 0.0275(10) 0.0374(12) 0.0086(10) 0.0089(10) 0.0022(9) _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 C5 1.425(4) . ? C1 C2 1.434(4) . ? C1 C6 1.505(4) . ? C1 Fe1 2.073(3) . ? C2 C3 1.429(4) . ? C2 C7 1.509(3) . ? C2 Fe1 2.050(3) . ? C3 C4 1.435(4) . ? C3 C8 1.502(4) . ? C3 Fe1 2.038(3) . ? C3 K1 3.270(3) 1_545 ? C4 C5 1.426(4) . ? C4 C9 1.505(4) . ? C4 Fe1 2.064(3) . ? C4 K1 3.373(3) 1_545 ? C5 C10 1.509(4) . ? C5 Fe1 2.084(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 K1 3.435(4) 1_545 ? C8 H8A 0.91(3) . ? C8 H8B 0.96(3) . ? C8 H8C 0.92(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C111 1.464(3) . ? C11 C14 1.465(3) . ? C11 C12 1.467(4) . ? C11 Fe1 2.025(3) . ? C12 C121 1.466(4) . ? C12 C13 1.484(3) . ? C12 Fe1 1.992(3) . ? C13 C131 1.468(4) . ? C13 C14 1.475(4) . ? C13 Fe1 1.991(3) . ? C14 C141 1.459(4) . ? C14 Fe1 2.037(2) . ? C15 O1 1.419(3) . ? C15 C16 1.493(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O2 1.417(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O2 1.421(3) . ? C17 C18 1.493(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O3 1.425(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O3 1.430(3) . ? C19 C20 1.484(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O4 1.432(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 O4 1.414(4) . ? C21 C22 1.488(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 O5 1.427(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 O5 1.419(3) . ? C23 C24 1.506(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O6 1.418(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O6 1.423(3) . ? C25 C26 1.490(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 O1 1.423(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C111 C116 1.400(3) . ? C111 C112 1.405(4) . ? C112 C113 1.383(4) . ? C112 K1 3.539(3) . ? C112 H112 0.95(3) . ? C113 C114 1.383(4) . ? C113 K1 3.478(3) . ? C113 H113 0.91(3) . ? C114 C115 1.392(4) . ? C114 H114 0.9300 . ? C115 C116 1.375(4) . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? C121 C122 1.400(4) . ? C121 C126 1.406(4) . ? C122 C123 1.383(4) . ? C122 H122 0.9300 . ? C123 C124 1.386(4) . ? C123 H123 0.9300 . ? C124 C125 1.371(4) . ? C124 H124 0.9300 . ? C125 C126 1.385(4) . ? C125 H125 0.9300 . ? C126 H126 0.9300 . ? C131 C132 1.397(4) . ? C131 C136 1.405(4) . ? C132 C133 1.380(4) . ? C132 H132 0.9300 . ? C133 C134 1.384(5) . ? C133 H133 0.9300 . ? C134 C135 1.379(5) . ? C134 H134 0.9300 . ? C135 C136 1.378(4) . ? C135 H135 0.9300 . ? C136 H136 0.9300 . ? C141 C142 1.399(4) . ? C141 C146 1.405(4) . ? C142 C143 1.387(4) . ? C142 H142 0.9300 . ? C143 C144 1.367(4) . ? C143 H143 0.9300 . ? C144 C145 1.389(5) . ? C144 H144 0.9300 . ? C145 C146 1.384(4) . ? C145 H145 0.9300 . ? C146 H146 0.9300 . ? K1 O5 2.7556(19) . ? K1 O2 2.820(2) . ? K1 O1 2.825(2) . ? K1 O4 2.832(2) . ? K1 O3 2.841(2) . ? K1 O6 2.903(2) . ? K1 C3 3.270(3) 1_565 ? K1 C4 3.373(3) 1_565 ? K1 C8 3.435(4) 1_565 ? 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 C5 C1 C2 108.0(2) . . ? C5 C1 C6 124.9(2) . . ? C2 C1 C6 127.1(2) . . ? C5 C1 Fe1 70.39(15) . . ? C2 C1 Fe1 68.79(15) . . ? C6 C1 Fe1 126.92(19) . . ? C3 C2 C1 107.8(2) . . ? C3 C2 C7 124.4(2) . . ? C1 C2 C7 127.8(2) . . ? C3 C2 Fe1 69.08(15) . . ? C1 C2 Fe1 70.51(15) . . ? C7 C2 Fe1 127.89(19) . . ? C2 C3 C4 108.1(2) . . ? C2 C3 C8 124.2(3) . . ? C4 C3 C8 127.4(3) . . ? C2 C3 Fe1 69.99(15) . . ? C4 C3 Fe1 70.51(15) . . ? C8 C3 Fe1 130.6(2) . . ? C2 C3 K1 100.39(16) . 1_545 ? C4 C3 K1 81.58(15) . 1_545 ? C8 C3 K1 83.31(18) . 1_545 ? Fe1 C3 K1 144.93(12) . 1_545 ? C5 C4 C3 107.7(2) . . ? C5 C4 C9 125.5(3) . . ? C3 C4 C9 126.7(3) . . ? C5 C4 Fe1 70.65(15) . . ? C3 C4 Fe1 68.52(15) . . ? C9 C4 Fe1 128.30(19) . . ? C5 C4 K1 102.70(16) . 1_545 ? C3 C4 K1 73.53(15) . 1_545 ? C9 C4 K1 91.34(16) . 1_545 ? Fe1 C4 K1 136.56(11) . 1_545 ? C1 C5 C4 108.4(2) . . ? C1 C5 C10 125.9(3) . . ? C4 C5 C10 125.6(2) . . ? C1 C5 Fe1 69.52(15) . . ? C4 C5 Fe1 69.15(15) . . ? C10 C5 Fe1 128.81(19) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 K1 70.95(17) . 1_545 ? C3 C8 H8A 115(2) . . ? K1 C8 H8A 51(2) 1_545 . ? C3 C8 H8B 115(2) . . ? K1 C8 H8B 105(2) 1_545 . ? H8A C8 H8B 108(3) . . ? C3 C8 H8C 115(2) . . ? K1 C8 H8C 148(2) 1_545 . ? H8A C8 H8C 102(3) . . ? H8B C8 H8C 100(3) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C111 C11 C14 137.9(2) . . ? C111 C11 C12 131.1(2) . . ? C14 C11 C12 90.3(2) . . ? C111 C11 Fe1 127.81(18) . . ? C14 C11 Fe1 69.31(14) . . ? C12 C11 Fe1 67.39(14) . . ? C121 C12 C11 132.4(2) . . ? C121 C12 C13 134.8(2) . . ? C11 C12 C13 90.0(2) . . ? C121 C12 Fe1 133.32(19) . . ? C11 C12 Fe1 69.77(15) . . ? C13 C12 Fe1 68.10(14) . . ? C131 C13 C14 133.2(2) . . ? C131 C13 C12 133.9(2) . . ? C14 C13 C12 89.3(2) . . ? C131 C13 Fe1 134.5(2) . . ? C14 C13 Fe1 70.20(14) . . ? C12 C13 Fe1 68.15(14) . . ? C141 C14 C11 136.0(2) . . ? C141 C14 C13 133.4(2) . . ? C11 C14 C13 90.4(2) . . ? C141 C14 Fe1 118.81(18) . . ? C11 C14 Fe1 68.40(14) . . ? C13 C14 Fe1 66.88(14) . . ? O1 C15 C16 109.0(3) . . ? O1 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? O1 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O2 C16 C15 108.3(2) . . ? O2 C16 H16A 110.0 . . ? C15 C16 H16A 110.0 . . ? O2 C16 H16B 110.0 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? O2 C17 C18 108.9(2) . . ? O2 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? O2 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? O3 C18 C17 109.8(2) . . ? O3 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? O3 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? O3 C19 C20 110.2(3) . . ? O3 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? O3 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? O4 C20 C19 108.5(3) . . ? O4 C20 H20A 110.0 . . ? C19 C20 H20A 110.0 . . ? O4 C20 H20B 110.0 . . ? C19 C20 H20B 110.0 . . ? H20A C20 H20B 108.4 . . ? O4 C21 C22 109.9(2) . . ? O4 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? O4 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? O5 C22 C21 109.0(2) . . ? O5 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? O5 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? O5 C23 C24 108.4(2) . . ? O5 C23 H23A 110.0 . . ? C24 C23 H23A 110.0 . . ? O5 C23 H23B 110.0 . . ? C24 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? O6 C24 C23 107.9(2) . . ? O6 C24 H24A 110.1 . . ? C23 C24 H24A 110.1 . . ? O6 C24 H24B 110.1 . . ? C23 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? O6 C25 C26 108.6(2) . . ? O6 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? O6 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? H25A C25 H25B 108.3 . . ? O1 C26 C25 108.9(2) . . ? O1 C26 H26A 109.9 . . ? C25 C26 H26A 109.9 . . ? O1 C26 H26B 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? C116 C111 C112 116.7(2) . . ? C116 C111 C11 120.9(2) . . ? C112 C111 C11 122.4(2) . . ? C113 C112 C111 121.0(3) . . ? C113 C112 K1 76.15(17) . . ? C111 C112 K1 136.83(18) . . ? C113 C112 H112 121.1(19) . . ? C111 C112 H112 117.9(19) . . ? K1 C112 H112 59.3(19) . . ? C112 C113 C114 121.1(3) . . ? C112 C113 K1 81.14(17) . . ? C114 C113 K1 133.0(2) . . ? C112 C113 H113 121(2) . . ? C114 C113 H113 118(2) . . ? K1 C113 H113 57.9(19) . . ? C113 C114 C115 118.8(3) . . ? C113 C114 H114 120.6 . . ? C115 C114 H114 120.6 . . ? C116 C115 C114 120.1(3) . . ? C116 C115 H115 120.0 . . ? C114 C115 H115 120.0 . . ? C115 C116 C111 122.3(3) . . ? C115 C116 H116 118.8 . . ? C111 C116 H116 118.8 . . ? C122 C121 C126 117.0(3) . . ? C122 C121 C12 122.9(3) . . ? C126 C121 C12 120.1(2) . . ? C123 C122 C121 121.2(3) . . ? C123 C122 H122 119.4 . . ? C121 C122 H122 119.4 . . ? C122 C123 C124 120.5(3) . . ? C122 C123 H123 119.7 . . ? C124 C123 H123 119.7 . . ? C125 C124 C123 119.3(3) . . ? C125 C124 H124 120.3 . . ? C123 C124 H124 120.3 . . ? C124 C125 C126 120.7(3) . . ? C124 C125 H125 119.7 . . ? C126 C125 H125 119.7 . . ? C125 C126 C121 121.2(3) . . ? C125 C126 H126 119.4 . . ? C121 C126 H126 119.4 . . ? C132 C131 C136 117.0(3) . . ? C132 C131 C13 120.3(3) . . ? C136 C131 C13 122.7(3) . . ? C133 C132 C131 121.4(3) . . ? C133 C132 H132 119.3 . . ? C131 C132 H132 119.3 . . ? C132 C133 C134 120.5(3) . . ? C132 C133 H133 119.7 . . ? C134 C133 H133 119.7 . . ? C135 C134 C133 119.1(3) . . ? C135 C134 H134 120.4 . . ? C133 C134 H134 120.4 . . ? C136 C135 C134 120.6(3) . . ? C136 C135 H135 119.7 . . ? C134 C135 H135 119.7 . . ? C135 C136 C131 121.3(3) . . ? C135 C136 H136 119.3 . . ? C131 C136 H136 119.3 . . ? C142 C141 C146 116.3(3) . . ? C142 C141 C14 122.1(2) . . ? C146 C141 C14 121.6(3) . . ? C143 C142 C141 122.1(3) . . ? C143 C142 H142 119.0 . . ? C141 C142 H142 119.0 . . ? C144 C143 C142 120.4(3) . . ? C144 C143 H143 119.8 . . ? C142 C143 H143 119.8 . . ? C143 C144 C145 119.2(3) . . ? C143 C144 H144 120.4 . . ? C145 C144 H144 120.4 . . ? C146 C145 C144 120.6(3) . . ? C146 C145 H145 119.7 . . ? C144 C145 H145 119.7 . . ? C145 C146 C141 121.4(3) . . ? C145 C146 H146 119.3 . . ? C141 C146 H146 119.3 . . ? C13 Fe1 C12 43.75(10) . . ? C13 Fe1 C11 62.60(10) . . ? C12 Fe1 C11 42.85(10) . . ? C13 Fe1 C14 42.92(10) . . ? C12 Fe1 C14 62.12(10) . . ? C11 Fe1 C14 42.29(10) . . ? C13 Fe1 C3 120.71(11) . . ? C12 Fe1 C3 118.66(11) . . ? C11 Fe1 C3 153.63(11) . . ? C14 Fe1 C3 158.46(10) . . ? C13 Fe1 C2 149.66(11) . . ? C12 Fe1 C2 115.73(11) . . ? C11 Fe1 C2 121.61(10) . . ? C14 Fe1 C2 160.54(10) . . ? C3 Fe1 C2 40.93(10) . . ? C13 Fe1 C4 114.83(11) . . ? C12 Fe1 C4 145.98(11) . . ? C11 Fe1 C4 165.31(11) . . ? C14 Fe1 C4 125.10(11) . . ? C3 Fe1 C4 40.96(10) . . ? C2 Fe1 C4 68.60(10) . . ? C13 Fe1 C1 169.43(11) . . ? C12 Fe1 C1 138.90(11) . . ? C11 Fe1 C1 111.90(10) . . ? C14 Fe1 C1 126.72(10) . . ? C3 Fe1 C1 68.49(10) . . ? C2 Fe1 C1 40.71(10) . . ? C4 Fe1 C1 67.97(10) . . ? C13 Fe1 C5 135.45(11) . . ? C12 Fe1 C5 173.00(11) . . ? C11 Fe1 C5 130.27(11) . . ? C14 Fe1 C5 112.23(11) . . ? C3 Fe1 C5 68.18(11) . . ? C2 Fe1 C5 68.02(10) . . ? C4 Fe1 C5 40.19(10) . . ? C1 Fe1 C5 40.09(10) . . ? O5 K1 O2 155.22(6) . . ? O5 K1 O1 118.08(6) . . ? O2 K1 O1 58.28(6) . . ? O5 K1 O4 60.04(6) . . ? O2 K1 O4 111.60(6) . . ? O1 K1 O4 154.62(6) . . ? O5 K1 O3 118.64(6) . . ? O2 K1 O3 59.27(6) . . ? O1 K1 O3 117.53(6) . . ? O4 K1 O3 58.62(6) . . ? O5 K1 O6 58.95(6) . . ? O2 K1 O6 113.71(6) . . ? O1 K1 O6 59.31(6) . . ? O4 K1 O6 114.79(6) . . ? O3 K1 O6 160.34(6) . . ? O5 K1 C3 85.20(7) . 1_565 ? O2 K1 C3 119.57(7) . 1_565 ? O1 K1 C3 106.56(6) . 1_565 ? O4 K1 C3 98.60(7) . 1_565 ? O3 K1 C3 102.04(6) . 1_565 ? O6 K1 C3 97.24(6) . 1_565 ? O5 K1 C4 106.54(6) . 1_565 ? O2 K1 C4 97.71(6) . 1_565 ? O1 K1 C4 85.06(6) . 1_565 ? O4 K1 C4 120.22(7) . 1_565 ? O3 K1 C4 101.94(6) . 1_565 ? O6 K1 C4 97.16(6) . 1_565 ? C3 K1 C4 24.90(6) 1_565 1_565 ? O5 K1 C8 81.90(8) . 1_565 ? O2 K1 C8 119.96(8) . 1_565 ? O1 K1 C8 130.54(7) . 1_565 ? O4 K1 C8 74.82(7) . 1_565 ? O3 K1 C8 81.30(7) . 1_565 ? O6 K1 C8 116.05(8) . 1_565 ? C3 K1 C8 25.74(7) 1_565 1_565 ? C4 K1 C8 45.51(7) 1_565 1_565 ? O5 K1 C113 70.59(7) . . ? O2 K1 C113 85.05(7) . . ? O1 K1 C113 77.69(7) . . ? O4 K1 C113 78.24(7) . . ? O3 K1 C113 98.36(6) . . ? O6 K1 C113 62.06(6) . . ? C3 K1 C113 153.81(7) 1_565 . ? C4 K1 C113 157.84(7) 1_565 . ? C8 K1 C113 148.51(8) 1_565 . ? O5 K1 C112 87.55(6) . . ? O2 K1 C112 67.75(6) . . ? O1 K1 C112 81.55(6) . . ? O4 K1 C112 73.13(6) . . ? O3 K1 C112 76.87(6) . . ? O6 K1 C112 83.49(6) . . ? C3 K1 C112 171.03(7) 1_565 . ? C4 K1 C112 164.01(7) 1_565 . ? C8 K1 C112 147.34(7) 1_565 . ? C113 K1 C112 22.71(6) . . ? C15 O1 C26 112.0(2) . . ? C15 O1 K1 118.57(17) . . ? C26 O1 K1 118.08(16) . . ? C16 O2 C17 112.2(2) . . ? C16 O2 K1 117.25(17) . . ? C17 O2 K1 114.91(17) . . ? C18 O3 C19 110.0(2) . . ? C18 O3 K1 117.03(17) . . ? C19 O3 K1 118.84(17) . . ? C21 O4 C20 112.0(2) . . ? C21 O4 K1 113.10(17) . . ? C20 O4 K1 113.60(16) . . ? C23 O5 C22 111.8(2) . . ? C23 O5 K1 121.19(16) . . ? C22 O5 K1 118.27(17) . . ? C24 O6 C25 112.2(2) . . ? C24 O6 K1 106.43(16) . . ? C25 O6 K1 107.15(16) . . ? _diffrn_measured_fraction_theta_max 0.860 _diffrn_reflns_theta_full 71.59 _diffrn_measured_fraction_theta_full 0.860 _refine_diff_density_max 0.298 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.048 data_3 _database_code_depnum_ccdc_archive 'CCDC 758969' #TrackingRef 'subm1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H73 Fe K O8 P2' _chemical_formula_weight 838.87 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' P P 0.1023 0.0942 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.1729(6) _cell_length_b 17.1904(6) _cell_length_c 32.8716(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.5490(10) _cell_angle_gamma 90.00 _cell_volume 9110.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9944 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 24.32 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3616 _exptl_absorpt_coefficient_mu 0.538 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8553 _exptl_absorpt_correction_T_max 0.9633 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68573 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 24.37 _reflns_number_total 14910 _reflns_number_gt 11202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ? ; _computing_publication_material ? _refine_special_details ; Some carbon atoms of one crown ether ligands show comparatively high adp's due to slight disorder. Attempts at modeling this disorder did not lead to an improved refinement. 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^)+(0.0532P)^2^+10.4592P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14910 _refine_ls_number_parameters 959 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _refine_ls_shift/su_max 0.001 _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 0.05776(17) 0.20200(16) 0.14215(9) 0.0302(7) Uani 1 1 d . . . C2 C 0.12042(17) 0.21048(15) 0.17478(9) 0.0291(6) Uani 1 1 d . . . C3 C 0.19884(16) 0.20248(15) 0.15835(8) 0.0251(6) Uani 1 1 d . . . C4 C 0.18465(17) 0.18653(15) 0.11559(8) 0.0262(6) Uani 1 1 d . . . C5 C 0.09725(18) 0.18532(15) 0.10582(9) 0.0292(7) Uani 1 1 d . . . C6 C -0.03406(19) 0.20492(19) 0.14651(12) 0.0512(9) Uani 1 1 d . . . H6A H -0.0537 0.1531 0.1537 0.077 Uiso 1 1 calc R . . H6B H -0.0629 0.2216 0.1206 0.077 Uiso 1 1 calc R . . H6C H -0.0454 0.2419 0.1680 0.077 Uiso 1 1 calc R . . C7 C 0.1057(2) 0.21338(19) 0.21914(10) 0.0490(9) Uani 1 1 d . . . H7A H 0.0520 0.2381 0.2224 0.074 Uiso 1 1 calc R . . H7B H 0.1499 0.2436 0.2339 0.074 Uiso 1 1 calc R . . H7C H 0.1055 0.1604 0.2301 0.074 Uiso 1 1 calc R . . C8 C 0.28175(18) 0.19872(17) 0.18200(10) 0.0385(7) Uani 1 1 d . . . H8A H 0.3040 0.1459 0.1806 0.058 Uiso 1 1 calc R . . H8B H 0.2757 0.2125 0.2105 0.058 Uiso 1 1 calc R . . H8C H 0.3198 0.2354 0.1703 0.058 Uiso 1 1 calc R . . C9 C 0.25070(18) 0.16453(17) 0.08817(10) 0.0362(7) Uani 1 1 d . . . H9A H 0.2943 0.2043 0.0898 0.054 Uiso 1 1 calc R . . H9B H 0.2263 0.1607 0.0600 0.054 Uiso 1 1 calc R . . H9C H 0.2747 0.1142 0.0968 0.054 Uiso 1 1 calc R . . C10 C 0.0530(2) 0.15674(18) 0.06674(10) 0.0456(8) Uani 1 1 d . . . H10A H 0.0493 0.0999 0.0674 0.068 Uiso 1 1 calc R . . H10B H 0.0838 0.1728 0.0436 0.068 Uiso 1 1 calc R . . H10C H -0.0030 0.1789 0.0637 0.068 Uiso 1 1 calc R . . C11 C 0.15190(16) 0.40522(15) 0.15410(8) 0.0245(6) Uani 1 1 d . . . C12 C 0.12938(16) 0.37938(15) 0.08445(8) 0.0245(6) Uani 1 1 d . . . C13 C 0.16731(18) 0.43595(16) 0.19710(8) 0.0284(6) Uani 1 1 d . . . C14 C 0.24064(18) 0.39385(17) 0.21952(9) 0.0325(7) Uani 1 1 d . . . H14A H 0.2264 0.3390 0.2231 0.049 Uiso 1 1 calc R . . H14B H 0.2534 0.4180 0.2463 0.049 Uiso 1 1 calc R . . H14C H 0.2891 0.3976 0.2035 0.049 Uiso 1 1 calc R . . C15 C 0.08933(19) 0.4263(2) 0.22013(9) 0.0416(8) Uani 1 1 d . . . H15A H 0.0435 0.4556 0.2061 0.062 Uiso 1 1 calc R . . H15B H 0.1001 0.4460 0.2480 0.062 Uiso 1 1 calc R . . H15C H 0.0744 0.3711 0.2210 0.062 Uiso 1 1 calc R . . C16 C 0.1890(2) 0.52274(17) 0.19555(10) 0.0456(9) Uani 1 1 d . . . H16A H 0.2404 0.5294 0.1820 0.068 Uiso 1 1 calc R . . H16B H 0.1965 0.5434 0.2234 0.068 Uiso 1 1 calc R . . H16C H 0.1439 0.5508 0.1802 0.068 Uiso 1 1 calc R . . C17 C 0.11507(17) 0.37676(16) 0.03823(8) 0.0268(6) Uani 1 1 d . . . C18 C 0.02620(18) 0.35123(18) 0.02572(9) 0.0361(7) Uani 1 1 d . . . H18A H 0.0169 0.2991 0.0365 0.054 Uiso 1 1 calc R . . H18B H 0.0174 0.3503 -0.0041 0.054 Uiso 1 1 calc R . . H18C H -0.0127 0.3880 0.0367 0.054 Uiso 1 1 calc R . . C19 C 0.17807(18) 0.32296(17) 0.02063(9) 0.0338(7) Uani 1 1 d . . . H19A H 0.2342 0.3391 0.0305 0.051 Uiso 1 1 calc R . . H19B H 0.1720 0.3258 -0.0092 0.051 Uiso 1 1 calc R . . H19C H 0.1684 0.2694 0.0293 0.051 Uiso 1 1 calc R . . C20 C 0.1274(2) 0.45854(17) 0.02089(9) 0.0399(8) Uani 1 1 d . . . H20A H 0.0865 0.4941 0.0311 0.060 Uiso 1 1 calc R . . H20B H 0.1203 0.4567 -0.0090 0.060 Uiso 1 1 calc R . . H20C H 0.1834 0.4770 0.0295 0.060 Uiso 1 1 calc R . . C21 C 0.1781(2) 1.00097(18) 0.16375(11) 0.0501(9) Uani 1 1 d . . . H21A H 0.1964 1.0279 0.1394 0.060 Uiso 1 1 calc R . . H21B H 0.1994 1.0304 0.1883 0.060 Uiso 1 1 calc R . . C22 C 0.0863(2) 0.99835(18) 0.16155(10) 0.0469(9) Uani 1 1 d . . . H22A H 0.0681 0.9680 0.1848 0.056 Uiso 1 1 calc R . . H22B H 0.0640 1.0518 0.1633 0.056 Uiso 1 1 calc R . . C23 C -0.03266(19) 0.96668(18) 0.11951(11) 0.0426(8) Uani 1 1 d . . . H23A H -0.0510 1.0209 0.1142 0.051 Uiso 1 1 calc R . . H23B H -0.0560 0.9488 0.1448 0.051 Uiso 1 1 calc R . . C24 C -0.06307(19) 0.91616(18) 0.08485(10) 0.0405(8) Uani 1 1 d . . . H24A H -0.1242 0.9201 0.0801 0.049 Uiso 1 1 calc R . . H24B H -0.0382 0.9324 0.0596 0.049 Uiso 1 1 calc R . . C25 C -0.08097(18) 0.78151(18) 0.06955(9) 0.0351(7) Uani 1 1 d . . . H25A H -0.0646 0.7865 0.0413 0.042 Uiso 1 1 calc R . . H25B H -0.1418 0.7882 0.0692 0.042 Uiso 1 1 calc R . . C26 C -0.05629(18) 0.70386(17) 0.08649(9) 0.0339(7) Uani 1 1 d . . . H26A H -0.0692 0.7006 0.1154 0.041 Uiso 1 1 calc R . . H26B H -0.0877 0.6625 0.0710 0.041 Uiso 1 1 calc R . . C27 C 0.0570(2) 0.61920(17) 0.09914(10) 0.0399(8) Uani 1 1 d . . . H27A H 0.0258 0.5772 0.0841 0.048 Uiso 1 1 calc R . . H27B H 0.0469 0.6150 0.1284 0.048 Uiso 1 1 calc R . . C28 C 0.1472(2) 0.61107(18) 0.09406(10) 0.0438(8) Uani 1 1 d . . . H28A H 0.1655 0.5573 0.1007 0.053 Uiso 1 1 calc R . . H28B H 0.1582 0.6220 0.0654 0.053 Uiso 1 1 calc R . . C29 C 0.2783(2) 0.6630(2) 0.11604(11) 0.0541(10) Uani 1 1 d . . . H29A H 0.2895 0.6824 0.0887 0.065 Uiso 1 1 calc R . . H29B H 0.2994 0.6090 0.1188 0.065 Uiso 1 1 calc R . . C30 C 0.3211(2) 0.7136(2) 0.14844(11) 0.0558(10) Uani 1 1 d . . . H30A H 0.3080 0.6954 0.1758 0.067 Uiso 1 1 calc R . . H30B H 0.3819 0.7109 0.1470 0.067 Uiso 1 1 calc R . . C31 C 0.32848(19) 0.8419(2) 0.17344(10) 0.0495(9) Uani 1 1 d . . . H31A H 0.3898 0.8410 0.1739 0.059 Uiso 1 1 calc R . . H31B H 0.3126 0.8243 0.2004 0.059 Uiso 1 1 calc R . . C32 C 0.2975(2) 0.9221(2) 0.16523(10) 0.0478(9) Uani 1 1 d . . . H32A H 0.3226 0.9580 0.1863 0.057 Uiso 1 1 calc R . . H32B H 0.3136 0.9397 0.1383 0.057 Uiso 1 1 calc R . . C33 C -0.0316(2) 0.7911(2) 0.19939(10) 0.0441(8) Uani 1 1 d . . . H33A H -0.0721 0.7989 0.1755 0.053 Uiso 1 1 calc R . . H33B H -0.0350 0.8357 0.2182 0.053 Uiso 1 1 calc R . . C34 C -0.0478(2) 0.7162(2) 0.22058(11) 0.0542(9) Uani 1 1 d . . . H34A H -0.0705 0.6765 0.2010 0.065 Uiso 1 1 calc R . . H34B H -0.0870 0.7239 0.2419 0.065 Uiso 1 1 calc R . . C35 C 0.0376(2) 0.6929(3) 0.23936(13) 0.0718(13) Uani 1 1 d . . . H35A H 0.0424 0.7027 0.2691 0.086 Uiso 1 1 calc R . . H35B H 0.0481 0.6370 0.2346 0.086 Uiso 1 1 calc R . . C36 C 0.0969(2) 0.7421(3) 0.21862(11) 0.0615(11) Uani 1 1 d . . . H36A H 0.1250 0.7791 0.2382 0.074 Uiso 1 1 calc R . . H36B H 0.1395 0.7093 0.2070 0.074 Uiso 1 1 calc R . . C37 C 0.2441(3) 0.8956(4) 0.04366(14) 0.109(2) Uani 1 1 d . . . H37A H 0.2829 0.8890 0.0220 0.131 Uiso 1 1 calc R . . H37B H 0.2762 0.8986 0.0705 0.131 Uiso 1 1 calc R . . C38 C 0.1887(6) 0.9676(4) 0.0358(2) 0.155(4) Uani 1 1 d . . . H38A H 0.1655 0.9855 0.0611 0.186 Uiso 1 1 calc R . . H38B H 0.2196 1.0108 0.0241 0.186 Uiso 1 1 calc R . . C39 C 0.1232(4) 0.9375(4) 0.0061(2) 0.132(3) Uani 1 1 d . . . H39A H 0.0693 0.9624 0.0102 0.159 Uiso 1 1 calc R . . H39B H 0.1373 0.9474 -0.0222 0.159 Uiso 1 1 calc R . . C40 C 0.1197(2) 0.8553(3) 0.01397(12) 0.0689(12) Uani 1 1 d . . . H40A H 0.0659 0.8419 0.0246 0.083 Uiso 1 1 calc R . . H40B H 0.1245 0.8260 -0.0117 0.083 Uiso 1 1 calc R . . Fe1 Fe 0.13594(2) 0.29345(2) 0.129356(11) 0.02100(10) Uani 1 1 d . . . K1 K 0.12578(4) 0.81270(3) 0.119072(18) 0.02683(14) Uani 1 1 d . . . O1 O 0.21073(13) 0.92347(12) 0.16561(6) 0.0382(5) Uani 1 1 d . . . O2 O 0.05557(13) 0.96358(11) 0.12446(6) 0.0363(5) Uani 1 1 d . . . O3 O -0.03963(12) 0.83886(11) 0.09517(6) 0.0332(5) Uani 1 1 d . . . O4 O 0.02952(12) 0.69317(11) 0.08361(6) 0.0310(5) Uani 1 1 d . . . O5 O 0.19145(13) 0.66447(12) 0.12056(6) 0.0382(5) Uani 1 1 d . . . O6 O 0.29369(12) 0.79088(14) 0.14233(6) 0.0427(5) Uani 1 1 d . . . O7 O 0.04969(14) 0.78303(16) 0.18695(7) 0.0602(7) Uani 1 1 d . . . O8 O 0.18519(14) 0.83498(15) 0.04271(7) 0.0540(6) Uani 1 1 d . . . P1 P 0.22479(4) 0.39065(4) 0.11599(2) 0.02406(16) Uani 1 1 d . . . P2 P 0.05747(4) 0.40304(4) 0.12145(2) 0.02515(17) Uani 1 1 d . . . C101 C 0.62586(17) 1.03001(15) 0.18456(8) 0.0278(6) Uani 1 1 d . . . C102 C 0.70272(16) 1.03769(15) 0.16696(8) 0.0264(6) Uani 1 1 d . . . C103 C 0.68620(17) 1.05660(15) 0.12495(8) 0.0270(6) Uani 1 1 d . . . C104 C 0.59825(17) 1.06130(15) 0.11662(8) 0.0275(6) Uani 1 1 d . . . C105 C 0.56153(16) 1.04258(15) 0.15310(9) 0.0285(6) Uani 1 1 d . . . C106 C 0.6144(2) 1.02328(19) 0.22930(9) 0.0453(8) Uani 1 1 d . . . H10D H 0.6592 0.9917 0.2425 0.068 Uiso 1 1 calc R . . H10E H 0.5609 0.9985 0.2330 0.068 Uiso 1 1 calc R . . H10F H 0.6155 1.0753 0.2416 0.068 Uiso 1 1 calc R . . C107 C 0.78752(18) 1.03837(19) 0.18944(10) 0.0426(8) Uani 1 1 d . . . H10G H 0.8258 1.0076 0.1743 0.064 Uiso 1 1 calc R . . H10H H 0.7843 1.0159 0.2167 0.064 Uiso 1 1 calc R . . H10I H 0.8077 1.0920 0.1920 0.064 Uiso 1 1 calc R . . C108 C 0.75051(19) 1.07870(17) 0.09650(10) 0.0384(8) Uani 1 1 d . . . H10J H 0.7783 1.1267 0.1062 0.058 Uiso 1 1 calc R . . H10K H 0.7238 1.0870 0.0690 0.058 Uiso 1 1 calc R . . H10L H 0.7915 1.0368 0.0957 0.058 Uiso 1 1 calc R . . C109 C 0.5533(2) 1.09391(18) 0.07859(10) 0.0439(8) Uani 1 1 d . . . H10M H 0.4961 1.0747 0.0762 0.066 Uiso 1 1 calc R . . H10N H 0.5815 1.0775 0.0547 0.066 Uiso 1 1 calc R . . H10O H 0.5530 1.1508 0.0801 0.066 Uiso 1 1 calc R . . C110 C 0.47017(18) 1.04264(19) 0.15863(11) 0.0465(8) Uani 1 1 d . . . H11A H 0.4528 1.0952 0.1658 0.070 Uiso 1 1 calc R . . H11B H 0.4587 1.0065 0.1806 0.070 Uiso 1 1 calc R . . H11C H 0.4394 1.0263 0.1332 0.070 Uiso 1 1 calc R . . C111 C 0.65182(17) 0.83649(15) 0.15873(8) 0.0274(6) Uani 1 1 d . . . C112 C 0.62193(19) 0.86811(16) 0.09026(9) 0.0331(7) Uani 1 1 d . . . C113 C 0.67070(18) 0.80123(16) 0.20064(9) 0.0321(7) Uani 1 1 d . . . C114 C 0.74625(18) 0.83964(18) 0.22292(9) 0.0385(7) Uani 1 1 d . . . H11D H 0.7929 0.8378 0.2057 0.058 Uiso 1 1 calc R . . H11E H 0.7611 0.8119 0.2485 0.058 Uiso 1 1 calc R . . H11F H 0.7333 0.8939 0.2289 0.058 Uiso 1 1 calc R . . C115 C 0.6902(3) 0.71402(18) 0.19558(11) 0.0568(10) Uani 1 1 d . . . H11G H 0.6430 0.6884 0.1806 0.085 Uiso 1 1 calc R . . H11H H 0.7004 0.6900 0.2225 0.085 Uiso 1 1 calc R . . H11I H 0.7396 0.7083 0.1804 0.085 Uiso 1 1 calc R . . C116 C 0.5951(2) 0.8079(2) 0.22558(9) 0.0455(8) Uani 1 1 d . . . H11J H 0.5810 0.8629 0.2289 0.068 Uiso 1 1 calc R . . H11K H 0.6078 0.7844 0.2525 0.068 Uiso 1 1 calc R . . H11L H 0.5479 0.7808 0.2114 0.068 Uiso 1 1 calc R . . C117 C 0.6006(2) 0.87597(18) 0.04462(9) 0.0460(9) Uani 1 1 d . . . C118 C 0.6101(3) 0.7964(2) 0.02371(11) 0.0782(15) Uani 1 1 d . . . H11M H 0.6667 0.7771 0.0298 0.117 Uiso 1 1 calc R . . H11N H 0.5990 0.8023 -0.0059 0.117 Uiso 1 1 calc R . . H11O H 0.5706 0.7594 0.0339 0.117 Uiso 1 1 calc R . . C119 C 0.5113(3) 0.9029(2) 0.03675(11) 0.0654(12) Uani 1 1 d . . . H11P H 0.4743 0.8651 0.0483 0.098 Uiso 1 1 calc R . . H11Q H 0.4973 0.9074 0.0073 0.098 Uiso 1 1 calc R . . H11R H 0.5047 0.9537 0.0496 0.098 Uiso 1 1 calc R . . C120 C 0.6597(3) 0.9321(2) 0.02588(10) 0.0558(10) Uani 1 1 d . . . H12A H 0.6544 0.9838 0.0380 0.084 Uiso 1 1 calc R . . H12B H 0.6459 0.9351 -0.0036 0.084 Uiso 1 1 calc R . . H12C H 0.7168 0.9136 0.0313 0.084 Uiso 1 1 calc R . . C121 C 0.5507(2) 0.62200(19) 0.08891(13) 0.0604(11) Uani 1 1 d . . . H12D H 0.5350 0.6203 0.1174 0.072 Uiso 1 1 calc R . . H12E H 0.5196 0.6648 0.0745 0.072 Uiso 1 1 calc R . . C122 C 0.6415(2) 0.6355(2) 0.08842(12) 0.0588(10) Uani 1 1 d . . . H12F H 0.6581 0.6316 0.0601 0.071 Uiso 1 1 calc R . . H12G H 0.6556 0.6883 0.0988 0.071 Uiso 1 1 calc R . . C123 C 0.7714(2) 0.5841(2) 0.11243(12) 0.0575(10) Uani 1 1 d . . . H12H H 0.7894 0.6386 0.1174 0.069 Uiso 1 1 calc R . . H12I H 0.7876 0.5682 0.0852 0.069 Uiso 1 1 calc R . . C124 C 0.8121(2) 0.5326(2) 0.14437(12) 0.0563(10) Uani 1 1 d . . . H12J H 0.8731 0.5368 0.1442 0.068 Uiso 1 1 calc R . . H12K H 0.7963 0.5489 0.1716 0.068 Uiso 1 1 calc R . . C125 C 0.8231(2) 0.4026(2) 0.16681(10) 0.0508(9) Uani 1 1 d . . . H12L H 0.8102 0.4202 0.1943 0.061 Uiso 1 1 calc R . . H12M H 0.8841 0.4022 0.1659 0.061 Uiso 1 1 calc R . . C126 C 0.78949(19) 0.3229(2) 0.15895(10) 0.0453(9) Uani 1 1 d . . . H12N H 0.8010 0.3059 0.1312 0.054 Uiso 1 1 calc R . . H12O H 0.8165 0.2859 0.1789 0.054 Uiso 1 1 calc R . . C127 C 0.6686(2) 0.24734(18) 0.16177(11) 0.0475(9) Uani 1 1 d . . . H12P H 0.6896 0.2184 0.1865 0.057 Uiso 1 1 calc R . . H12Q H 0.6852 0.2188 0.1376 0.057 Uiso 1 1 calc R . . C128 C 0.5768(2) 0.25335(18) 0.16017(11) 0.0459(8) Uani 1 1 d . . . H12R H 0.5522 0.2012 0.1633 0.055 Uiso 1 1 calc R . . H12S H 0.5603 0.2868 0.1827 0.055 Uiso 1 1 calc R . . C129 C 0.45973(19) 0.28528(19) 0.11585(12) 0.0491(9) Uani 1 1 d . . . H12T H 0.4355 0.3106 0.1392 0.059 Uiso 1 1 calc R . . H12U H 0.4394 0.2310 0.1139 0.059 Uiso 1 1 calc R . . C130 C 0.43392(19) 0.32761(19) 0.07763(11) 0.0483(9) Uani 1 1 d . . . H13A H 0.4619 0.3053 0.0546 0.058 Uiso 1 1 calc R . . H13B H 0.3732 0.3230 0.0714 0.058 Uiso 1 1 calc R . . C131 C 0.4280(2) 0.4552(2) 0.05036(12) 0.0610(11) Uani 1 1 d . . . H13C H 0.3680 0.4470 0.0434 0.073 Uiso 1 1 calc R . . H13D H 0.4579 0.4431 0.0260 0.073 Uiso 1 1 calc R . . C132 C 0.4441(2) 0.5374(2) 0.06344(14) 0.0703(12) Uani 1 1 d . . . H13E H 0.4193 0.5735 0.0424 0.084 Uiso 1 1 calc R . . H13F H 0.4185 0.5476 0.0893 0.084 Uiso 1 1 calc R . . C133 C 0.4562(2) 0.4709(3) 0.18646(13) 0.0869(17) Uani 1 1 d . . . H13G H 0.4397 0.4185 0.1953 0.104 Uiso 1 1 calc R . . H13H H 0.4203 0.4850 0.1618 0.104 Uiso 1 1 calc R . . C134 C 0.4450(2) 0.5243(3) 0.21722(15) 0.0948(18) Uani 1 1 d . . . H13I H 0.4091 0.5022 0.2374 0.114 Uiso 1 1 calc R . . H13J H 0.4187 0.5724 0.2057 0.114 Uiso 1 1 calc R . . C135 C 0.5300(2) 0.5417(3) 0.23705(13) 0.0786(14) Uani 1 1 d . . . H13K H 0.5415 0.5983 0.2367 0.094 Uiso 1 1 calc R . . H13L H 0.5355 0.5231 0.2656 0.094 Uiso 1 1 calc R . . C136 C 0.5874(2) 0.4986(2) 0.21163(11) 0.0560(10) Uani 1 1 d . . . H13M H 0.6311 0.5337 0.2028 0.067 Uiso 1 1 calc R . . H13N H 0.6144 0.4552 0.2274 0.067 Uiso 1 1 calc R . . C137 C 0.6510(3) 0.2990(3) 0.02729(16) 0.0889(16) Uani 1 1 d . . . H13O H 0.6276 0.2869 -0.0007 0.107 Uiso 1 1 calc R . . H13P H 0.6192 0.2703 0.0470 0.107 Uiso 1 1 calc R . . C138 C 0.7387(6) 0.2786(4) 0.0325(2) 0.164(3) Uani 1 1 d . . . H13Q H 0.7539 0.2454 0.0096 0.197 Uiso 1 1 calc R . . H13R H 0.7510 0.2499 0.0583 0.197 Uiso 1 1 calc R . . C139 C 0.7858(3) 0.3534(5) 0.03309(17) 0.133(3) Uani 1 1 d . . . H13S H 0.8130 0.3641 0.0606 0.160 Uiso 1 1 calc R . . H13T H 0.8284 0.3527 0.0130 0.160 Uiso 1 1 calc R . . C140 C 0.7228(3) 0.4094(3) 0.02216(14) 0.0814(14) Uani 1 1 d . . . H14D H 0.7358 0.4595 0.0360 0.098 Uiso 1 1 calc R . . H14E H 0.7181 0.4181 -0.0077 0.098 Uiso 1 1 calc R . . Fe2 Fe 0.63541(2) 0.95015(2) 0.137189(11) 0.02263(10) Uani 1 1 d . . . K2 K 0.61818(4) 0.43126(3) 0.111745(19) 0.02921(15) Uani 1 1 d . . . O101 O 0.53086(14) 0.54957(13) 0.06903(7) 0.0501(6) Uani 1 1 d . . . O102 O 0.68422(14) 0.57873(12) 0.11346(7) 0.0478(6) Uani 1 1 d . . . O103 O 0.78701(12) 0.45469(13) 0.13666(6) 0.0422(5) Uani 1 1 d . . . O104 O 0.70284(12) 0.32385(11) 0.16252(6) 0.0378(5) Uani 1 1 d . . . O105 O 0.54793(12) 0.28579(12) 0.12211(6) 0.0376(5) Uani 1 1 d . . . O106 O 0.45647(12) 0.40673(12) 0.08334(6) 0.0394(5) Uani 1 1 d . . . O107 O 0.53830(14) 0.46950(18) 0.17720(7) 0.0655(8) Uani 1 1 d . . . O108 O 0.64897(17) 0.37869(15) 0.03468(9) 0.0687(8) Uani 1 1 d . . . P3 P 0.71983(5) 0.85338(4) 0.11895(2) 0.03164(18) Uani 1 1 d . . . P4 P 0.55435(5) 0.84200(4) 0.12883(2) 0.03038(18) Uani 1 1 d . . . 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 0.0221(15) 0.0178(14) 0.0512(19) -0.0010(13) 0.0071(13) -0.0015(12) C2 0.0310(16) 0.0166(14) 0.0408(17) 0.0022(12) 0.0104(13) -0.0035(12) C3 0.0250(15) 0.0160(13) 0.0342(16) 0.0024(12) 0.0015(12) -0.0020(11) C4 0.0268(15) 0.0174(14) 0.0350(16) 0.0002(12) 0.0059(12) 0.0029(12) C5 0.0321(16) 0.0160(14) 0.0388(17) -0.0002(12) -0.0018(13) -0.0023(12) C6 0.0280(18) 0.0304(18) 0.097(3) -0.0015(18) 0.0171(18) -0.0031(14) C7 0.071(2) 0.0326(18) 0.047(2) 0.0026(15) 0.0238(18) -0.0101(17) C8 0.0344(17) 0.0278(16) 0.052(2) 0.0025(15) -0.0061(15) 0.0012(14) C9 0.0368(17) 0.0232(15) 0.0505(19) -0.0033(14) 0.0154(14) 0.0002(13) C10 0.055(2) 0.0255(17) 0.054(2) -0.0037(15) -0.0116(17) -0.0099(15) C11 0.0275(15) 0.0172(14) 0.0289(15) 0.0007(11) 0.0029(12) 0.0009(12) C12 0.0266(15) 0.0187(14) 0.0284(15) -0.0026(11) 0.0038(12) -0.0004(12) C13 0.0344(16) 0.0228(15) 0.0280(15) -0.0035(12) 0.0023(12) 0.0018(12) C14 0.0369(17) 0.0305(16) 0.0298(16) -0.0011(13) 0.0002(13) -0.0005(13) C15 0.0409(19) 0.054(2) 0.0310(17) -0.0067(15) 0.0072(14) 0.0129(16) C16 0.071(2) 0.0277(17) 0.0360(18) -0.0092(14) -0.0082(16) 0.0032(16) C17 0.0299(16) 0.0250(15) 0.0256(15) -0.0011(12) 0.0017(12) -0.0001(12) C18 0.0361(17) 0.0395(18) 0.0320(17) -0.0018(14) -0.0015(13) 0.0022(14) C19 0.0356(17) 0.0370(17) 0.0285(16) -0.0059(13) 0.0014(13) 0.0001(14) C20 0.059(2) 0.0339(17) 0.0267(16) 0.0054(14) 0.0022(14) -0.0041(16) C21 0.078(3) 0.0214(17) 0.049(2) -0.0003(15) -0.0056(18) -0.0161(17) C22 0.069(2) 0.0243(17) 0.048(2) -0.0055(15) 0.0037(17) 0.0027(17) C23 0.0396(19) 0.0270(17) 0.063(2) 0.0028(15) 0.0160(16) 0.0109(14) C24 0.0323(17) 0.0348(18) 0.055(2) 0.0110(16) 0.0051(15) 0.0090(14) C25 0.0234(15) 0.0467(19) 0.0343(17) -0.0065(14) -0.0021(13) -0.0017(14) C26 0.0314(17) 0.0380(17) 0.0322(16) -0.0030(14) 0.0015(13) -0.0121(14) C27 0.059(2) 0.0185(15) 0.0412(19) 0.0027(13) -0.0008(16) -0.0040(15) C28 0.058(2) 0.0255(17) 0.048(2) -0.0033(15) 0.0049(16) 0.0087(16) C29 0.043(2) 0.056(2) 0.065(2) -0.0025(19) 0.0133(18) 0.0225(18) C30 0.0296(18) 0.079(3) 0.059(2) -0.003(2) 0.0000(16) 0.0157(19) C31 0.0258(17) 0.088(3) 0.0340(18) -0.0083(18) -0.0040(14) -0.0098(18) C32 0.045(2) 0.062(2) 0.0361(19) -0.0006(17) 0.0007(15) -0.0249(18) C33 0.0405(19) 0.048(2) 0.0444(19) 0.0041(16) 0.0090(15) 0.0049(16) C34 0.053(2) 0.056(2) 0.054(2) 0.0139(18) 0.0126(18) -0.0042(19) C35 0.061(3) 0.085(3) 0.071(3) 0.035(2) 0.019(2) 0.020(2) C36 0.045(2) 0.088(3) 0.051(2) 0.023(2) -0.0005(18) 0.001(2) C37 0.098(4) 0.184(7) 0.046(3) -0.004(3) 0.014(3) -0.090(4) C38 0.268(11) 0.072(4) 0.144(6) -0.042(4) 0.132(7) -0.084(6) C39 0.160(7) 0.104(5) 0.148(6) 0.058(4) 0.107(5) 0.060(5) C40 0.056(3) 0.093(3) 0.057(2) -0.006(2) -0.003(2) 0.019(2) Fe1 0.0199(2) 0.01572(19) 0.0276(2) -0.00052(16) 0.00305(16) -0.00014(16) K1 0.0248(3) 0.0223(3) 0.0334(3) -0.0009(3) 0.0023(3) -0.0020(3) O1 0.0397(13) 0.0330(12) 0.0412(12) 0.0032(10) -0.0008(10) -0.0150(10) O2 0.0459(13) 0.0243(11) 0.0391(12) -0.0025(9) 0.0067(10) 0.0001(10) O3 0.0303(11) 0.0280(11) 0.0406(12) 0.0006(9) -0.0020(9) 0.0068(9) O4 0.0325(11) 0.0223(10) 0.0382(11) 0.0015(9) 0.0028(9) -0.0037(8) O5 0.0399(12) 0.0300(11) 0.0448(13) -0.0027(10) 0.0043(10) 0.0122(10) O6 0.0270(11) 0.0606(15) 0.0400(13) 0.0001(11) -0.0014(9) 0.0014(11) O7 0.0395(14) 0.091(2) 0.0514(15) 0.0333(14) 0.0112(11) 0.0038(13) O8 0.0477(14) 0.0731(17) 0.0408(13) 0.0076(12) 0.0015(11) -0.0151(13) P1 0.0245(4) 0.0204(4) 0.0274(4) -0.0013(3) 0.0030(3) -0.0029(3) P2 0.0246(4) 0.0218(4) 0.0291(4) -0.0006(3) 0.0028(3) 0.0042(3) C101 0.0343(16) 0.0188(14) 0.0307(16) -0.0016(12) 0.0057(13) 0.0024(12) C102 0.0270(15) 0.0190(14) 0.0328(16) -0.0056(12) 0.0000(12) 0.0008(12) C103 0.0291(16) 0.0181(14) 0.0349(16) -0.0024(12) 0.0099(12) -0.0018(12) C104 0.0317(16) 0.0178(14) 0.0324(16) -0.0010(12) -0.0021(12) 0.0002(12) C105 0.0235(15) 0.0185(14) 0.0435(18) -0.0007(13) 0.0034(13) -0.0016(12) C106 0.065(2) 0.0364(18) 0.0362(18) -0.0016(15) 0.0138(16) 0.0109(17) C107 0.0351(18) 0.0356(18) 0.056(2) -0.0046(16) -0.0053(15) -0.0012(15) C108 0.0391(18) 0.0284(16) 0.050(2) -0.0035(14) 0.0176(15) -0.0041(14) C109 0.059(2) 0.0313(18) 0.0400(19) 0.0020(15) -0.0084(16) 0.0046(16) C110 0.0314(18) 0.0365(19) 0.073(2) -0.0021(17) 0.0118(16) -0.0022(15) C111 0.0343(16) 0.0194(14) 0.0290(15) 0.0001(12) 0.0056(12) 0.0001(12) C112 0.0487(19) 0.0213(15) 0.0294(16) 0.0000(12) 0.0042(14) -0.0053(14) C113 0.0391(17) 0.0255(15) 0.0319(16) 0.0051(13) 0.0030(13) 0.0007(13) C114 0.0404(18) 0.0402(18) 0.0344(17) 0.0048(14) -0.0009(14) 0.0051(15) C115 0.093(3) 0.0261(18) 0.050(2) 0.0100(16) -0.004(2) 0.0092(19) C116 0.049(2) 0.054(2) 0.0343(18) 0.0112(16) 0.0077(15) -0.0092(17) C117 0.081(3) 0.0312(18) 0.0250(17) -0.0019(14) -0.0005(16) -0.0134(17) C118 0.164(5) 0.037(2) 0.034(2) -0.0110(17) 0.007(2) -0.021(3) C119 0.087(3) 0.061(3) 0.042(2) 0.0126(19) -0.029(2) -0.024(2) C120 0.102(3) 0.040(2) 0.0270(18) 0.0039(15) 0.0119(18) -0.010(2) C121 0.076(3) 0.0242(18) 0.082(3) 0.0056(18) 0.015(2) 0.0075(18) C122 0.077(3) 0.0268(18) 0.074(3) 0.0018(18) 0.016(2) -0.0084(19) C123 0.055(2) 0.047(2) 0.073(3) -0.014(2) 0.024(2) -0.0289(19) C124 0.039(2) 0.067(3) 0.063(2) -0.018(2) 0.0079(18) -0.0270(19) C125 0.0267(17) 0.083(3) 0.042(2) -0.0037(19) -0.0013(15) 0.0024(18) C126 0.0372(19) 0.058(2) 0.0398(19) -0.0059(16) -0.0012(15) 0.0188(17) C127 0.064(2) 0.0253(17) 0.052(2) 0.0017(15) -0.0017(17) 0.0091(16) C128 0.059(2) 0.0250(17) 0.055(2) 0.0031(15) 0.0145(17) -0.0087(16) C129 0.0356(19) 0.0299(18) 0.084(3) -0.0082(18) 0.0176(18) -0.0140(15) C130 0.0273(17) 0.045(2) 0.072(2) -0.0250(19) -0.0006(16) -0.0101(15) C131 0.044(2) 0.072(3) 0.064(3) 0.011(2) -0.0173(18) -0.005(2) C132 0.047(2) 0.057(3) 0.103(3) 0.022(2) -0.014(2) 0.011(2) C133 0.038(2) 0.149(5) 0.075(3) -0.059(3) 0.015(2) -0.014(3) C134 0.046(2) 0.141(5) 0.096(4) -0.070(3) -0.004(2) 0.010(3) C135 0.051(2) 0.113(4) 0.073(3) -0.048(3) 0.011(2) -0.016(2) C136 0.040(2) 0.073(3) 0.054(2) -0.013(2) -0.0007(17) -0.0055(19) C137 0.116(4) 0.047(3) 0.109(4) -0.017(3) 0.045(3) -0.018(3) C138 0.221(9) 0.100(5) 0.177(7) 0.028(5) 0.053(7) 0.095(6) C139 0.055(3) 0.260(9) 0.086(4) 0.076(5) 0.013(3) 0.029(5) C140 0.081(3) 0.091(4) 0.075(3) -0.011(3) 0.027(3) -0.039(3) Fe2 0.0254(2) 0.0180(2) 0.0247(2) 0.00000(16) 0.00310(16) -0.00123(16) K2 0.0251(3) 0.0235(3) 0.0396(4) -0.0018(3) 0.0054(3) -0.0038(3) O101 0.0476(14) 0.0386(13) 0.0635(16) 0.0082(12) 0.0011(12) 0.0017(11) O102 0.0492(14) 0.0291(12) 0.0665(16) 0.0015(11) 0.0138(12) -0.0129(11) O103 0.0293(11) 0.0511(14) 0.0461(13) -0.0110(11) 0.0031(10) -0.0082(10) O104 0.0360(12) 0.0292(11) 0.0479(13) -0.0036(10) 0.0018(10) 0.0094(9) O105 0.0329(12) 0.0294(11) 0.0515(14) -0.0023(10) 0.0100(10) -0.0081(9) O106 0.0313(12) 0.0384(12) 0.0480(13) -0.0038(10) 0.0001(10) -0.0078(10) O107 0.0386(14) 0.104(2) 0.0551(16) -0.0337(15) 0.0120(12) -0.0046(14) O108 0.0746(19) 0.0540(17) 0.083(2) -0.0097(15) 0.0420(16) -0.0062(14) P3 0.0386(5) 0.0231(4) 0.0349(4) -0.0013(3) 0.0138(3) 0.0017(3) P4 0.0333(4) 0.0239(4) 0.0336(4) 0.0014(3) 0.0006(3) -0.0068(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 C5 1.427(4) . ? C1 C2 1.423(4) . ? C1 C6 1.504(4) . ? C1 Fe1 2.081(3) . ? C2 C3 1.424(4) . ? C2 C7 1.497(4) . ? C2 Fe1 2.094(3) . ? C3 C4 1.432(4) . ? C3 C8 1.497(4) . ? C3 Fe1 2.058(3) . ? C4 C5 1.425(4) . ? C4 C9 1.500(4) . ? C4 Fe1 2.064(3) . ? C5 C10 1.503(4) . ? C5 Fe1 2.090(3) . ? C11 C13 1.511(4) . ? C11 P2 1.796(3) . ? C11 P1 1.804(3) . ? C11 Fe1 2.094(3) . ? C12 C17 1.519(4) . ? C12 P2 1.795(3) . ? C12 P1 1.800(3) . ? C12 Fe1 2.085(3) . ? C13 C14 1.528(4) . ? C13 C15 1.531(4) . ? C13 C16 1.534(4) . ? C17 C18 1.528(4) . ? C17 C19 1.524(4) . ? C17 C20 1.536(4) . ? C21 O1 1.432(4) . ? C21 C22 1.482(5) . ? C22 O2 1.412(4) . ? C23 O2 1.424(4) . ? C23 C24 1.485(4) . ? C24 O3 1.416(3) . ? C25 O3 1.428(3) . ? C25 C26 1.489(4) . ? C26 O4 1.410(3) . ? C27 O4 1.428(3) . ? C27 C28 1.488(4) . ? C28 O5 1.419(4) . ? C29 O5 1.425(4) . ? C29 C30 1.501(5) . ? C30 O6 1.409(4) . ? C31 O6 1.428(4) . ? C31 C32 1.485(5) . ? C32 O1 1.404(4) . ? C33 O7 1.415(4) . ? C33 C34 1.496(5) . ? C34 C35 1.521(5) . ? C35 C36 1.485(5) . ? C36 O7 1.427(4) . ? C37 O8 1.410(5) . ? C37 C38 1.538(9) . ? C38 C39 1.475(9) . ? C39 C40 1.438(7) . ? C40 O8 1.406(4) . ? C40 K1 3.525(4) . ? Fe1 P1 2.2692(8) . ? Fe1 P2 2.2748(8) . ? K1 O7 2.681(2) . ? K1 O1 2.742(2) . ? K1 O5 2.760(2) . ? K1 O3 2.7646(19) . ? K1 O4 2.7778(19) . ? K1 O6 2.788(2) . ? K1 O2 2.843(2) . ? C101 C102 1.418(4) . ? C101 C105 1.424(4) . ? C101 C106 1.501(4) . ? C101 Fe2 2.091(3) . ? C102 C103 1.423(4) . ? C102 C107 1.506(4) . ? C102 Fe2 2.059(3) . ? C103 C104 1.429(4) . ? C103 C108 1.502(4) . ? C103 Fe2 2.059(3) . ? C104 C105 1.417(4) . ? C104 C109 1.504(4) . ? C104 Fe2 2.099(3) . ? C105 C110 1.503(4) . ? C105 Fe2 2.080(3) . ? C111 C113 1.514(4) . ? C111 P4 1.793(3) . ? C111 P3 1.798(3) . ? C111 Fe2 2.088(3) . ? C112 C117 1.518(4) . ? C112 P3 1.795(3) . ? C112 P4 1.796(3) . ? C112 Fe2 2.089(3) . ? C113 C114 1.524(4) . ? C113 C116 1.530(4) . ? C113 C115 1.544(4) . ? C117 C119 1.520(5) . ? C117 C120 1.522(5) . ? C117 C118 1.544(5) . ? C121 O101 1.431(4) . ? C121 C122 1.488(5) . ? C121 K2 3.518(3) . ? C122 O102 1.421(4) . ? C123 O102 1.415(4) . ? C123 C124 1.487(5) . ? C124 O103 1.417(4) . ? C125 O103 1.426(4) . ? C125 C126 1.489(5) . ? C126 O104 1.416(4) . ? C127 O104 1.427(4) . ? C127 C128 1.485(5) . ? C128 O105 1.415(4) . ? C128 K2 3.536(3) . ? C129 O105 1.425(4) . ? C129 C130 1.483(5) . ? C130 O106 1.417(4) . ? C131 O106 1.415(4) . ? C131 C132 1.493(5) . ? C132 O101 1.416(4) . ? C133 O107 1.386(4) . ? C133 C134 1.389(5) . ? C134 C135 1.505(5) . ? C135 C136 1.495(5) . ? C136 O107 1.421(4) . ? C137 O108 1.393(5) . ? C137 C138 1.457(8) . ? C138 C139 1.495(9) . ? C139 C140 1.427(7) . ? C140 O108 1.396(5) . ? Fe2 P3 2.2628(8) . ? Fe2 P4 2.2789(8) . ? K2 O107 2.678(2) . ? K2 O106 2.739(2) . ? K2 O102 2.750(2) . ? K2 O108 2.772(3) . ? K2 O104 2.776(2) . ? K2 O105 2.779(2) . ? K2 O101 2.791(2) . ? K2 O103 2.817(2) . ? 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 C5 C1 C2 108.2(2) . . ? C5 C1 C6 126.7(3) . . ? C2 C1 C6 125.0(3) . . ? C5 C1 Fe1 70.33(15) . . ? C2 C1 Fe1 70.57(15) . . ? C6 C1 Fe1 127.9(2) . . ? C3 C2 C1 107.8(2) . . ? C3 C2 C7 126.0(3) . . ? C1 C2 C7 125.4(3) . . ? C3 C2 Fe1 68.57(15) . . ? C1 C2 Fe1 69.57(16) . . ? C7 C2 Fe1 135.2(2) . . ? C2 C3 C4 108.2(2) . . ? C2 C3 C8 126.5(3) . . ? C4 C3 C8 124.6(3) . . ? C2 C3 Fe1 71.33(15) . . ? C4 C3 Fe1 69.89(15) . . ? C8 C3 Fe1 131.51(19) . . ? C5 C4 C3 107.6(2) . . ? C5 C4 C9 127.0(3) . . ? C3 C4 C9 124.9(2) . . ? C5 C4 Fe1 70.93(15) . . ? C3 C4 Fe1 69.44(15) . . ? C9 C4 Fe1 131.2(2) . . ? C4 C5 C1 108.1(2) . . ? C4 C5 C10 126.5(3) . . ? C1 C5 C10 124.5(3) . . ? C4 C5 Fe1 68.96(15) . . ? C1 C5 Fe1 69.65(15) . . ? C10 C5 Fe1 135.7(2) . . ? C13 C11 P2 129.5(2) . . ? C13 C11 P1 129.0(2) . . ? P2 C11 P1 98.83(13) . . ? C13 C11 Fe1 133.64(19) . . ? P2 C11 Fe1 71.09(9) . . ? P1 C11 Fe1 70.74(9) . . ? C17 C12 P2 129.0(2) . . ? C17 C12 P1 129.4(2) . . ? P2 C12 P1 99.04(13) . . ? C17 C12 Fe1 133.01(18) . . ? P2 C12 Fe1 71.34(10) . . ? P1 C12 Fe1 71.04(9) . . ? C11 C13 C14 110.5(2) . . ? C11 C13 C15 110.1(2) . . ? C14 C13 C15 110.4(2) . . ? C11 C13 C16 109.3(2) . . ? C14 C13 C16 107.8(2) . . ? C15 C13 C16 108.8(3) . . ? C12 C17 C18 110.1(2) . . ? C12 C17 C19 110.1(2) . . ? C18 C17 C19 111.5(2) . . ? C12 C17 C20 109.3(2) . . ? C18 C17 C20 108.1(2) . . ? C19 C17 C20 107.7(2) . . ? O1 C21 C22 109.7(3) . . ? O2 C22 C21 109.7(3) . . ? O2 C23 C24 109.5(2) . . ? O3 C24 C23 107.4(2) . . ? O3 C25 C26 107.4(2) . . ? O4 C26 C25 109.1(2) . . ? O4 C27 C28 108.9(2) . . ? O5 C28 C27 108.8(3) . . ? O5 C29 C30 108.6(3) . . ? O6 C30 C29 108.9(3) . . ? O6 C31 C32 109.4(3) . . ? O1 C32 C31 109.7(3) . . ? O7 C33 C34 104.6(3) . . ? C33 C34 C35 103.2(3) . . ? C36 C35 C34 105.2(3) . . ? O7 C36 C35 106.7(3) . . ? O8 C37 C38 101.9(4) . . ? C39 C38 C37 101.9(4) . . ? C40 C39 C38 105.2(5) . . ? O8 C40 C39 109.0(5) . . ? O8 C40 K1 47.87(17) . . ? C39 C40 K1 112.4(4) . . ? C3 Fe1 C4 40.67(11) . . ? C3 Fe1 C1 67.56(11) . . ? C4 Fe1 C1 67.68(11) . . ? C3 Fe1 C12 149.51(11) . . ? C4 Fe1 C12 118.33(11) . . ? C1 Fe1 C12 132.89(11) . . ? C3 Fe1 C11 118.43(10) . . ? C4 Fe1 C11 149.84(11) . . ? C1 Fe1 C11 132.27(11) . . ? C12 Fe1 C11 67.85(10) . . ? C3 Fe1 C2 40.11(10) . . ? C4 Fe1 C2 67.62(11) . . ? C1 Fe1 C2 39.86(11) . . ? C12 Fe1 C2 170.05(11) . . ? C11 Fe1 C2 111.46(11) . . ? C3 Fe1 C5 67.55(11) . . ? C4 Fe1 C5 40.11(11) . . ? C1 Fe1 C5 40.02(11) . . ? C12 Fe1 C5 111.78(11) . . ? C11 Fe1 C5 169.63(11) . . ? C2 Fe1 C5 66.98(11) . . ? C3 Fe1 P1 110.60(8) . . ? C4 Fe1 P1 110.77(8) . . ? C1 Fe1 P1 178.13(8) . . ? C12 Fe1 P1 48.61(7) . . ? C11 Fe1 P1 48.65(7) . . ? C2 Fe1 P1 138.85(8) . . ? C5 Fe1 P1 139.35(9) . . ? C3 Fe1 P2 158.91(8) . . ? C4 Fe1 P2 158.69(8) . . ? C1 Fe1 P2 107.84(8) . . ? C12 Fe1 P2 48.38(7) . . ? C11 Fe1 P2 48.33(7) . . ? C2 Fe1 P2 123.23(8) . . ? C5 Fe1 P2 123.11(8) . . ? P1 Fe1 P2 73.99(3) . . ? O7 K1 O1 84.86(8) . . ? O7 K1 O5 90.64(7) . . ? O1 K1 O5 117.14(7) . . ? O7 K1 O3 76.70(7) . . ? O1 K1 O3 118.44(6) . . ? O5 K1 O3 121.18(6) . . ? O7 K1 O4 85.96(7) . . ? O1 K1 O4 170.75(6) . . ? O5 K1 O4 61.74(6) . . ? O3 K1 O4 60.24(6) . . ? O7 K1 O6 104.33(7) . . ? O1 K1 O6 60.42(7) . . ? O5 K1 O6 60.38(7) . . ? O3 K1 O6 178.24(7) . . ? O4 K1 O6 121.13(7) . . ? O7 K1 O2 84.83(7) . . ? O1 K1 O2 61.09(6) . . ? O5 K1 O2 175.24(6) . . ? O3 K1 O2 59.13(6) . . ? O4 K1 O2 119.19(6) . . ? O6 K1 O2 119.40(7) . . ? O7 K1 C40 151.18(8) . . ? O1 K1 C40 112.11(9) . . ? O5 K1 C40 100.94(8) . . ? O3 K1 C40 74.72(8) . . ? O4 K1 C40 76.77(9) . . ? O6 K1 C40 104.34(8) . . ? O2 K1 C40 83.76(8) . . ? C32 O1 C21 112.3(2) . . ? C32 O1 K1 116.11(19) . . ? C21 O1 K1 117.10(17) . . ? C22 O2 C23 111.3(2) . . ? C22 O2 K1 108.96(17) . . ? C23 O2 K1 115.37(16) . . ? C24 O3 C25 113.8(2) . . ? C24 O3 K1 117.10(17) . . ? C25 O3 K1 116.91(15) . . ? C26 O4 C27 111.8(2) . . ? C26 O4 K1 113.40(16) . . ? C27 O4 K1 111.14(16) . . ? C28 O5 C29 112.2(2) . . ? C28 O5 K1 114.31(16) . . ? C29 O5 K1 113.34(19) . . ? C30 O6 C31 112.0(3) . . ? C30 O6 K1 117.02(19) . . ? C31 O6 K1 115.72(18) . . ? C33 O7 C36 107.1(2) . . ? C33 O7 K1 136.10(19) . . ? C36 O7 K1 116.5(2) . . ? C40 O8 C37 107.7(4) . . ? C12 P1 C11 80.65(12) . . ? C12 P1 Fe1 60.35(9) . . ? C11 P1 Fe1 60.61(8) . . ? C11 P2 C12 81.01(12) . . ? C11 P2 Fe1 60.58(8) . . ? C12 P2 Fe1 60.28(9) . . ? C102 C101 C105 107.6(2) . . ? C102 C101 C106 126.0(3) . . ? C105 C101 C106 125.7(3) . . ? C102 C101 Fe2 68.79(15) . . ? C105 C101 Fe2 69.61(16) . . ? C106 C101 Fe2 134.5(2) . . ? C103 C102 C101 108.3(2) . . ? C103 C102 C107 124.6(3) . . ? C101 C102 C107 126.5(3) . . ? C103 C102 Fe2 69.77(15) . . ? C101 C102 Fe2 71.24(15) . . ? C107 C102 Fe2 131.7(2) . . ? C102 C103 C104 107.8(2) . . ? C102 C103 C108 125.2(3) . . ? C104 C103 C108 126.5(3) . . ? C102 C103 Fe2 69.79(15) . . ? C104 C103 Fe2 71.41(15) . . ? C108 C103 Fe2 130.8(2) . . ? C105 C104 C103 107.6(2) . . ? C105 C104 C109 125.5(3) . . ? C103 C104 C109 126.1(3) . . ? C105 C104 Fe2 69.46(15) . . ? C103 C104 Fe2 68.38(15) . . ? C109 C104 Fe2 135.6(2) . . ? C104 C105 C101 108.5(2) . . ? C104 C105 C110 125.8(3) . . ? C101 C105 C110 125.5(3) . . ? C104 C105 Fe2 70.91(16) . . ? C101 C105 Fe2 70.46(15) . . ? C110 C105 Fe2 128.4(2) . . ? C113 C111 P4 128.7(2) . . ? C113 C111 P3 129.5(2) . . ? P4 C111 P3 98.91(14) . . ? C113 C111 Fe2 134.0(2) . . ? P4 C111 Fe2 71.46(10) . . ? P3 C111 Fe2 70.78(10) . . ? C117 C112 P3 130.8(2) . . ? C117 C112 P4 128.1(2) . . ? P3 C112 P4 98.90(14) . . ? C117 C112 Fe2 132.2(2) . . ? P3 C112 Fe2 70.80(10) . . ? P4 C112 Fe2 71.39(10) . . ? C111 C113 C114 111.1(2) . . ? C111 C113 C116 110.2(2) . . ? C114 C113 C116 110.8(3) . . ? C111 C113 C115 108.6(2) . . ? C114 C113 C115 108.0(3) . . ? C116 C113 C115 108.0(3) . . ? C112 C117 C119 109.5(3) . . ? C112 C117 C120 110.8(3) . . ? C119 C117 C120 110.9(3) . . ? C112 C117 C118 109.8(3) . . ? C119 C117 C118 108.7(3) . . ? C120 C117 C118 107.1(3) . . ? O101 C121 C122 108.5(3) . . ? O101 C121 K2 48.77(15) . . ? C122 C121 K2 81.86(19) . . ? O102 C122 C121 108.7(3) . . ? O102 C123 C124 109.3(3) . . ? O103 C124 C123 109.4(3) . . ? O103 C125 C126 109.5(3) . . ? O104 C126 C125 109.0(3) . . ? O104 C127 C128 108.8(2) . . ? O105 C128 C127 108.5(3) . . ? O105 C128 K2 47.30(13) . . ? C127 C128 K2 81.46(17) . . ? O105 C129 C130 109.3(3) . . ? O106 C130 C129 107.9(3) . . ? O106 C131 C132 107.3(3) . . ? O101 C132 C131 109.0(3) . . ? O107 C133 C134 110.8(3) . . ? C133 C134 C135 106.2(3) . . ? C136 C135 C134 104.2(3) . . ? O107 C136 C135 106.7(3) . . ? O108 C137 C138 104.6(5) . . ? C137 C138 C139 106.6(5) . . ? C140 C139 C138 102.9(5) . . ? O108 C140 C139 106.4(4) . . ? C103 Fe2 C102 40.44(11) . . ? C103 Fe2 C105 67.42(10) . . ? C102 Fe2 C105 67.33(10) . . ? C103 Fe2 C111 148.89(11) . . ? C102 Fe2 C111 118.34(11) . . ? C105 Fe2 C111 133.61(11) . . ? C103 Fe2 C101 67.42(11) . . ? C102 Fe2 C101 39.96(11) . . ? C105 Fe2 C101 39.93(11) . . ? C111 Fe2 C101 112.14(11) . . ? C103 Fe2 C112 118.41(11) . . ? C102 Fe2 C112 149.87(12) . . ? C105 Fe2 C112 132.31(12) . . ? C111 Fe2 C112 67.77(11) . . ? C101 Fe2 C112 169.68(12) . . ? C103 Fe2 C104 40.21(11) . . ? C102 Fe2 C104 67.34(10) . . ? C105 Fe2 C104 39.64(11) . . ? C111 Fe2 C104 170.62(11) . . ? C101 Fe2 C104 66.80(11) . . ? C112 Fe2 C104 111.48(11) . . ? C103 Fe2 P3 110.07(8) . . ? C102 Fe2 P3 110.85(8) . . ? C105 Fe2 P3 177.50(8) . . ? C111 Fe2 P3 48.61(8) . . ? C101 Fe2 P3 139.63(8) . . ? C112 Fe2 P3 48.53(9) . . ? C104 Fe2 P3 138.35(8) . . ? C103 Fe2 P4 159.44(8) . . ? C102 Fe2 P4 158.60(8) . . ? C105 Fe2 P4 108.49(8) . . ? C111 Fe2 P4 48.23(8) . . ? C101 Fe2 P4 123.34(8) . . ? C112 Fe2 P4 48.30(8) . . ? C104 Fe2 P4 123.81(8) . . ? P3 Fe2 P4 73.85(3) . . ? O107 K2 O106 78.65(7) . . ? O107 K2 O102 88.20(8) . . ? O106 K2 O102 120.51(7) . . ? O107 K2 O108 161.35(8) . . ? O106 K2 O108 82.77(8) . . ? O102 K2 O108 102.81(8) . . ? O107 K2 O104 85.79(8) . . ? O106 K2 O104 120.98(7) . . ? O102 K2 O104 115.38(7) . . ? O108 K2 O104 102.53(8) . . ? O107 K2 O105 83.94(8) . . ? O106 K2 O105 60.96(6) . . ? O102 K2 O105 171.52(7) . . ? O108 K2 O105 85.61(7) . . ? O104 K2 O105 60.97(6) . . ? O107 K2 O101 88.18(8) . . ? O106 K2 O101 60.61(7) . . ? O102 K2 O101 61.23(7) . . ? O108 K2 O101 84.15(8) . . ? O104 K2 O101 173.21(7) . . ? O105 K2 O101 121.47(7) . . ? O107 K2 O103 104.45(7) . . ? O106 K2 O103 176.88(7) . . ? O102 K2 O103 59.75(7) . . ? O108 K2 O103 94.13(7) . . ? O104 K2 O103 59.98(6) . . ? O105 K2 O103 119.30(7) . . ? O101 K2 O103 118.84(7) . . ? O107 K2 C121 77.37(10) . . ? O106 K2 C121 78.41(8) . . ? O102 K2 C121 42.14(8) . . ? O108 K2 C121 100.61(9) . . ? O104 K2 C121 151.40(8) . . ? O105 K2 C121 137.90(8) . . ? O101 K2 C121 22.68(8) . . ? O103 K2 C121 101.89(8) . . ? O107 K2 C128 74.34(9) . . ? O106 K2 C128 79.08(7) . . ? O102 K2 C128 151.07(8) . . ? O108 K2 C128 100.58(8) . . ? O104 K2 C128 41.94(7) . . ? O105 K2 C128 21.97(7) . . ? O101 K2 C128 138.63(8) . . ? O103 K2 C128 101.92(8) . . ? C121 K2 C128 146.67(9) . . ? C132 O101 C121 111.8(3) . . ? C132 O101 K2 114.5(2) . . ? C121 O101 K2 108.6(2) . . ? C123 O102 C122 112.4(3) . . ? C123 O102 K2 116.49(19) . . ? C122 O102 K2 116.84(19) . . ? C124 O103 C125 112.0(3) . . ? C124 O103 K2 116.37(19) . . ? C125 O103 K2 116.51(18) . . ? C126 O104 C127 112.0(2) . . ? C126 O104 K2 113.69(18) . . ? C127 O104 K2 115.48(17) . . ? C128 O105 C129 112.4(2) . . ? C128 O105 K2 110.73(16) . . ? C129 O105 K2 113.72(17) . . ? C131 O106 C130 113.5(3) . . ? C131 O106 K2 114.47(19) . . ? C130 O106 K2 114.95(17) . . ? C133 O107 C136 107.7(3) . . ? C133 O107 K2 135.4(2) . . ? C136 O107 K2 116.83(19) . . ? C140 O108 C137 106.7(3) . . ? C140 O108 K2 111.5(2) . . ? C137 O108 K2 119.3(3) . . ? C112 P3 C111 80.79(13) . . ? C112 P3 Fe2 60.67(9) . . ? C111 P3 Fe2 60.61(9) . . ? C111 P4 C112 80.92(13) . . ? C111 P4 Fe2 60.30(9) . . ? C112 P4 Fe2 60.30(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.542 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.052