data_a13195 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H52 Fe K N4 O9' _chemical_formula_sum 'C40 H52 Fe K N4 O9' _chemical_formula_weight 827.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.256(3) _cell_length_b 13.064(3) _cell_length_c 24.449(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.777(4) _cell_angle_gamma 90.00 _cell_volume 4530.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7563 _exptl_absorpt_correction_T_max 0.9719 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26327 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.0885 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.04 _reflns_number_total 7925 _reflns_number_gt 4489 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0892P)^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 7925 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1540 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.003 _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 0.9580(2) 0.2244(3) 0.11068(17) 0.0376(9) Uani 1 1 d . . . C2 C 1.0178(3) 0.2405(3) 0.15822(18) 0.0454(10) Uani 1 1 d . . . H2 H 0.9958 0.2272 0.1930 0.054 Uiso 1 1 calc R . . C3 C 1.1094(3) 0.2758(3) 0.1558(2) 0.0591(13) Uani 1 1 d . . . H3 H 1.1496 0.2854 0.1889 0.071 Uiso 1 1 calc R . . C4 C 1.1423(3) 0.2967(3) 0.1062(2) 0.0619(13) Uani 1 1 d . . . H4 H 1.2050 0.3204 0.1047 0.074 Uiso 1 1 calc R . . C5 C 1.0834(3) 0.2830(3) 0.0583(2) 0.0582(13) Uani 1 1 d . . . H5 H 1.1056 0.2978 0.0238 0.070 Uiso 1 1 calc R . . C6 C 0.9925(3) 0.2480(3) 0.06036(18) 0.0463(10) Uani 1 1 d . . . H6 H 0.9525 0.2397 0.0271 0.056 Uiso 1 1 calc R . . C7 C 0.8400(2) 0.0979(3) 0.08618(15) 0.0384(9) Uani 1 1 d . . . C8 C 0.9041(3) 0.0319(3) 0.06474(16) 0.0405(9) Uani 1 1 d . . . H8 H 0.9690 0.0501 0.0678 0.049 Uiso 1 1 calc R . . C9 C 0.8762(3) -0.0591(3) 0.03929(17) 0.0489(11) Uani 1 1 d . . . H9 H 0.9217 -0.1015 0.0247 0.059 Uiso 1 1 calc R . . C10 C 0.7826(3) -0.0893(3) 0.0348(2) 0.0619(13) Uani 1 1 d . . . H10 H 0.7633 -0.1522 0.0177 0.074 Uiso 1 1 calc R . . C11 C 0.7183(3) -0.0250(4) 0.0559(2) 0.0657(14) Uani 1 1 d . . . H11 H 0.6538 -0.0444 0.0532 0.079 Uiso 1 1 calc R . . C12 C 0.7450(3) 0.0661(3) 0.08054(17) 0.0491(11) Uani 1 1 d . . . H12 H 0.6985 0.1087 0.0941 0.059 Uiso 1 1 calc R . . C13 C 0.6789(2) 0.4024(3) 0.07404(15) 0.0338(9) Uani 1 1 d . . . C14 C 0.7667(2) 0.4248(3) 0.05550(17) 0.0452(10) Uani 1 1 d . . . H14 H 0.8187 0.3806 0.0649 0.054 Uiso 1 1 calc R . . C15 C 0.7781(3) 0.5103(3) 0.02382(18) 0.0533(12) Uani 1 1 d . . . H15 H 0.8384 0.5240 0.0121 0.064 Uiso 1 1 calc R . . C16 C 0.7056(3) 0.5761(3) 0.00877(17) 0.0500(11) Uani 1 1 d . . . H16 H 0.7149 0.6347 -0.0130 0.060 Uiso 1 1 calc R . . C17 C 0.6181(3) 0.5551(3) 0.02613(16) 0.0465(10) Uani 1 1 d . . . H17 H 0.5668 0.6001 0.0163 0.056 Uiso 1 1 calc R . . C18 C 0.6046(2) 0.4703(3) 0.05739(15) 0.0397(10) Uani 1 1 d . . . H18 H 0.5435 0.4569 0.0681 0.048 Uiso 1 1 calc R . . C19 C 0.5774(2) 0.2811(3) 0.11134(17) 0.0402(10) Uani 1 1 d . . . C20 C 0.5252(3) 0.2412(3) 0.0653(2) 0.0589(12) Uani 1 1 d . . . H20 H 0.5505 0.2425 0.0308 0.071 Uiso 1 1 calc R . . C21 C 0.4365(3) 0.1995(4) 0.0687(3) 0.0776(16) Uani 1 1 d . . . H21 H 0.4016 0.1730 0.0367 0.093 Uiso 1 1 calc R . . C22 C 0.3988(3) 0.1963(4) 0.1185(3) 0.0812(18) Uani 1 1 d . . . H22 H 0.3384 0.1669 0.1209 0.097 Uiso 1 1 calc R . . C23 C 0.4483(3) 0.2352(4) 0.1637(3) 0.0687(15) Uani 1 1 d . . . H23 H 0.4219 0.2341 0.1978 0.082 Uiso 1 1 calc R . . C24 C 0.5373(3) 0.2767(3) 0.16093(19) 0.0500(11) Uani 1 1 d . . . H24 H 0.5713 0.3027 0.1934 0.060 Uiso 1 1 calc R . . C25 C 0.8515(6) 0.8746(5) 0.1916(3) 0.136(3) Uani 1 1 d . . . H25A H 0.9149 0.8429 0.1936 0.163 Uiso 1 1 calc R . . H25B H 0.8397 0.9068 0.1549 0.163 Uiso 1 1 calc R . . C26 C 0.8546(5) 0.9499(4) 0.2296(3) 0.0938(18) Uani 1 1 d . . . H26A H 0.9154 0.9861 0.2287 0.113 Uiso 1 1 calc R . . H26B H 0.8041 0.9994 0.2176 0.113 Uiso 1 1 calc R . . C27 C 0.8500(5) 0.9994(5) 0.3233(3) 0.120(3) Uani 1 1 d . . . H27A H 0.8014 1.0518 0.3128 0.144 Uiso 1 1 calc R . . H27B H 0.9122 1.0336 0.3247 0.144 Uiso 1 1 calc R . . C28 C 0.8373(5) 0.9647(6) 0.3768(3) 0.117(2) Uani 1 1 d . . . H28A H 0.8991 0.9393 0.3934 0.140 Uiso 1 1 calc R . . H28B H 0.8213 1.0251 0.3984 0.140 Uiso 1 1 calc R . . C29 C 0.7603(6) 0.8629(8) 0.4370(3) 0.164(4) Uani 1 1 d . . . H29A H 0.7399 0.9227 0.4577 0.197 Uiso 1 1 calc R . . H29B H 0.8208 0.8384 0.4560 0.197 Uiso 1 1 calc R . . C30 C 0.6920(6) 0.7843(7) 0.4385(3) 0.130(3) Uani 1 1 d . . . H30A H 0.7004 0.7544 0.4759 0.156 Uiso 1 1 calc R . . H30B H 0.6294 0.8178 0.4346 0.156 Uiso 1 1 calc R . . C31 C 0.6227(5) 0.6277(5) 0.4070(3) 0.107(2) Uani 1 1 d . . . H31A H 0.5581 0.6562 0.4008 0.128 Uiso 1 1 calc R . . H31B H 0.6308 0.5991 0.4447 0.128 Uiso 1 1 calc R . . C32 C 0.6318(5) 0.5476(6) 0.3689(3) 0.113(2) Uani 1 1 d . . . H32A H 0.6902 0.5093 0.3809 0.136 Uiso 1 1 calc R . . H32B H 0.5783 0.4999 0.3710 0.136 Uiso 1 1 calc R . . C33 C 0.6438(5) 0.4979(5) 0.2783(3) 0.108(2) Uani 1 1 d . . . H33A H 0.5919 0.4480 0.2799 0.129 Uiso 1 1 calc R . . H33B H 0.7038 0.4612 0.2881 0.129 Uiso 1 1 calc R . . C34 C 0.6425(4) 0.5344(5) 0.2232(3) 0.101(2) Uani 1 1 d . . . H34A H 0.6596 0.4771 0.1997 0.121 Uiso 1 1 calc R . . H34B H 0.5772 0.5551 0.2103 0.121 Uiso 1 1 calc R . . C35 C 0.7111(5) 0.6444(5) 0.1633(2) 0.0918(18) Uani 1 1 d . . . H35A H 0.6504 0.6718 0.1462 0.110 Uiso 1 1 calc R . . H35B H 0.7271 0.5842 0.1415 0.110 Uiso 1 1 calc R . . C36 C 0.7805(7) 0.7188(6) 0.1597(3) 0.169(4) Uani 1 1 d . . . H36A H 0.8423 0.6836 0.1635 0.203 Uiso 1 1 calc R . . H36B H 0.7717 0.7477 0.1221 0.203 Uiso 1 1 calc R . . N1 N 0.7338(2) 0.1935(3) 0.20487(15) 0.0490(9) Uani 1 1 d . . . N2 N 0.8416(2) 0.3652(3) 0.18615(15) 0.0494(9) Uani 1 1 d . . . N3 N 0.86392(18) 0.1894(2) 0.11234(12) 0.0360(7) Uani 1 1 d . . . N4 N 0.66996(18) 0.3191(2) 0.10837(13) 0.0376(8) Uani 1 1 d . . . O1 O 0.7093(2) 0.1659(3) 0.24705(15) 0.0813(11) Uani 1 1 d . . . O2 O 0.8793(2) 0.4222(3) 0.21762(16) 0.0876(11) Uani 1 1 d . . . O3 O 0.7862(2) 0.7966(3) 0.19457(13) 0.0687(9) Uani 1 1 d . . . O4 O 0.8458(3) 0.9261(3) 0.28199(18) 0.0920(12) Uani 1 1 d . . . O5 O 0.7756(3) 0.8947(3) 0.38374(15) 0.0883(11) Uani 1 1 d . . . O6 O 0.6876(3) 0.7067(4) 0.40323(17) 0.1119(15) Uani 1 1 d . . . O7 O 0.6346(3) 0.5731(3) 0.31644(19) 0.0958(13) Uani 1 1 d . . . O8 O 0.6988(3) 0.6119(3) 0.21606(16) 0.0959(12) Uani 1 1 d . . . Fe1 Fe 0.77846(3) 0.26632(4) 0.15665(2) 0.03742(19) Uani 1 1 d . . . K1 K 0.74510(7) 0.75094(7) 0.30074(4) 0.0544(3) 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 0.0322(19) 0.032(2) 0.049(3) -0.0035(19) 0.0087(18) 0.0029(17) C2 0.040(2) 0.048(3) 0.048(3) 0.001(2) 0.0007(19) 0.0035(19) C3 0.037(2) 0.056(3) 0.081(4) -0.004(3) -0.013(2) 0.009(2) C4 0.035(2) 0.051(3) 0.100(4) -0.005(3) 0.009(3) -0.003(2) C5 0.053(3) 0.044(3) 0.082(4) -0.001(3) 0.027(3) -0.006(2) C6 0.045(2) 0.046(3) 0.048(3) -0.001(2) 0.007(2) -0.0031(19) C7 0.042(2) 0.040(2) 0.034(2) -0.0003(19) 0.0058(18) -0.0004(18) C8 0.043(2) 0.040(2) 0.039(2) 0.0041(19) 0.0050(18) -0.0014(18) C9 0.057(3) 0.041(2) 0.049(3) -0.004(2) 0.008(2) 0.006(2) C10 0.069(3) 0.046(3) 0.071(4) -0.017(2) 0.009(3) -0.008(2) C11 0.053(3) 0.067(3) 0.078(4) -0.024(3) 0.008(2) -0.018(2) C12 0.037(2) 0.051(3) 0.060(3) -0.012(2) 0.008(2) -0.004(2) C13 0.0350(19) 0.040(2) 0.027(2) -0.0045(18) 0.0039(16) -0.0047(17) C14 0.035(2) 0.050(2) 0.052(3) 0.009(2) 0.0092(19) -0.0010(18) C15 0.041(2) 0.060(3) 0.061(3) 0.010(2) 0.013(2) -0.008(2) C16 0.054(2) 0.049(3) 0.045(3) 0.007(2) 0.000(2) -0.009(2) C17 0.049(2) 0.044(2) 0.046(3) 0.005(2) -0.001(2) 0.002(2) C18 0.0316(19) 0.046(2) 0.042(3) -0.002(2) 0.0061(17) 0.0003(18) C19 0.0276(19) 0.039(2) 0.055(3) 0.005(2) 0.0079(19) 0.0047(17) C20 0.047(2) 0.074(3) 0.055(3) -0.004(3) 0.003(2) -0.009(2) C21 0.057(3) 0.074(4) 0.095(5) -0.003(3) -0.022(3) -0.014(3) C22 0.042(3) 0.068(4) 0.135(6) 0.018(4) 0.016(3) -0.013(3) C23 0.044(3) 0.074(3) 0.094(4) 0.016(3) 0.031(3) 0.004(2) C24 0.045(2) 0.045(2) 0.062(3) 0.007(2) 0.019(2) 0.0058(19) C25 0.231(8) 0.093(5) 0.097(5) -0.017(4) 0.084(6) -0.082(5) C26 0.136(5) 0.067(4) 0.077(5) 0.025(4) 0.003(4) -0.006(4) C27 0.189(7) 0.063(4) 0.098(6) 0.002(4) -0.028(5) -0.051(4) C28 0.119(5) 0.126(6) 0.105(6) -0.023(5) 0.013(5) -0.041(5) C29 0.172(7) 0.277(11) 0.048(5) -0.054(6) 0.040(5) -0.089(8) C30 0.147(7) 0.168(7) 0.083(6) -0.028(5) 0.045(5) -0.011(6) C31 0.130(5) 0.091(5) 0.112(6) 0.042(4) 0.076(5) 0.021(4) C32 0.124(5) 0.144(7) 0.075(5) 0.025(5) 0.031(4) -0.001(5) C33 0.136(5) 0.082(4) 0.108(6) -0.002(4) 0.025(5) -0.029(4) C34 0.117(5) 0.078(4) 0.114(6) 0.000(4) 0.040(4) -0.015(4) C35 0.136(5) 0.092(4) 0.050(4) -0.017(3) 0.023(3) -0.025(4) C36 0.322(13) 0.115(6) 0.076(5) -0.033(5) 0.038(7) -0.092(7) N1 0.0463(19) 0.057(2) 0.046(2) 0.0062(18) 0.0137(17) 0.0058(17) N2 0.0441(19) 0.052(2) 0.051(2) -0.0163(19) 0.0002(17) 0.0018(17) N3 0.0301(15) 0.0372(18) 0.041(2) -0.0030(15) 0.0067(14) -0.0041(14) N4 0.0295(15) 0.0453(19) 0.038(2) 0.0026(16) 0.0064(14) -0.0028(14) O1 0.078(2) 0.108(3) 0.063(2) 0.031(2) 0.0330(19) 0.015(2) O2 0.088(2) 0.084(3) 0.088(3) -0.035(2) -0.003(2) -0.015(2) O3 0.091(2) 0.069(2) 0.048(2) -0.0034(18) 0.0146(17) -0.0030(19) O4 0.125(3) 0.071(2) 0.085(3) -0.015(2) 0.037(2) -0.031(2) O5 0.103(3) 0.100(3) 0.061(3) -0.016(2) 0.004(2) 0.003(2) O6 0.094(3) 0.188(5) 0.057(3) -0.004(3) 0.025(2) -0.037(3) O7 0.124(3) 0.070(2) 0.102(3) 0.016(2) 0.055(3) 0.006(2) O8 0.135(3) 0.075(3) 0.077(3) -0.005(2) 0.005(2) -0.039(2) Fe1 0.0344(3) 0.0434(3) 0.0353(3) -0.0011(3) 0.0075(2) 0.0013(3) K1 0.0678(6) 0.0559(6) 0.0402(6) 0.0018(5) 0.0084(5) -0.0078(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.386(5) . ? C1 C6 1.404(5) . ? C1 N3 1.422(4) . ? C2 C3 1.393(5) . ? C2 H2 0.9500 . ? C3 C4 1.373(6) . ? C3 H3 0.9500 . ? C4 C5 1.381(6) . ? C4 H4 0.9500 . ? C5 C6 1.380(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N3 1.381(4) . ? C7 C8 1.396(5) . ? C7 C12 1.411(5) . ? C8 C9 1.382(5) . ? C8 H8 0.9500 . ? C9 C10 1.384(5) . ? C9 H9 0.9500 . ? C10 C11 1.381(6) . ? C10 H10 0.9500 . ? C11 C12 1.371(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 N4 1.388(4) . ? C13 C14 1.403(4) . ? C13 C18 1.410(5) . ? C14 C15 1.379(5) . ? C14 H14 0.9500 . ? C15 C16 1.366(5) . ? C15 H15 0.9500 . ? C16 C17 1.384(5) . ? C16 H16 0.9500 . ? C17 C18 1.371(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.388(6) . ? C19 C24 1.393(5) . ? C19 N4 1.418(4) . ? C20 C21 1.386(6) . ? C20 H20 0.9500 . ? C21 C22 1.378(7) . ? C21 H21 0.9500 . ? C22 C23 1.349(7) . ? C22 H22 0.9500 . ? C23 C24 1.388(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.350(7) . ? C25 O3 1.387(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O4 1.336(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O4 1.388(7) . ? C27 C28 1.412(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O5 1.293(7) . ? C28 K1 3.534(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O5 1.404(7) . ? C29 C30 1.418(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O6 1.328(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 O6 1.396(7) . ? C31 C32 1.416(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O7 1.329(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O7 1.371(7) . ? C33 C34 1.425(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O8 1.315(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O8 1.386(6) . ? C35 C36 1.396(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O3 1.323(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N1 O1 1.178(4) . ? N1 Fe1 1.689(3) . ? N2 O2 1.163(4) . ? N2 Fe1 1.693(4) . ? N3 Fe1 1.983(3) . ? N4 Fe1 1.973(3) . ? O3 K1 2.783(3) . ? O4 K1 2.764(4) . ? O5 K1 2.767(4) . ? O6 K1 2.775(4) . ? O7 K1 2.855(4) . ? O8 K1 2.783(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.5(3) . . ? C2 C1 N3 121.8(3) . . ? C6 C1 N3 120.7(4) . . ? C1 C2 C3 121.0(4) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 120.5(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 121.2(4) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? N3 C7 C8 124.6(3) . . ? N3 C7 C12 119.3(3) . . ? C8 C7 C12 116.1(4) . . ? C9 C8 C7 122.1(3) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C10 120.9(4) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C11 C10 C9 117.8(4) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? C12 C11 C10 121.9(4) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C7 121.3(4) . . ? C11 C12 H12 119.3 . . ? C7 C12 H12 119.3 . . ? N4 C13 C14 119.9(3) . . ? N4 C13 C18 123.7(3) . . ? C14 C13 C18 116.4(3) . . ? C15 C14 C13 120.7(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 122.1(4) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C17 118.3(4) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C18 C17 C16 120.8(4) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C13 121.7(3) . . ? C17 C18 H18 119.2 . . ? C13 C18 H18 119.2 . . ? C20 C19 C24 117.2(3) . . ? C20 C19 N4 121.1(4) . . ? C24 C19 N4 121.7(4) . . ? C19 C20 C21 121.1(5) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C20 120.3(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.5(4) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 120.8(5) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C19 121.1(5) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? C26 C25 O3 118.3(5) . . ? C26 C25 H25A 107.7 . . ? O3 C25 H25A 107.7 . . ? C26 C25 H25B 107.7 . . ? O3 C25 H25B 107.7 . . ? H25A C25 H25B 107.1 . . ? O4 C26 C25 119.4(5) . . ? O4 C26 H26A 107.5 . . ? C25 C26 H26A 107.5 . . ? O4 C26 H26B 107.5 . . ? C25 C26 H26B 107.5 . . ? H26A C26 H26B 107.0 . . ? O4 C27 C28 116.9(5) . . ? O4 C27 H27A 108.1 . . ? C28 C27 H27A 108.1 . . ? O4 C27 H27B 108.1 . . ? C28 C27 H27B 108.1 . . ? H27A C27 H27B 107.3 . . ? O5 C28 C27 120.1(6) . . ? O5 C28 K1 44.6(3) . . ? C27 C28 K1 80.9(4) . . ? O5 C28 H28A 107.3 . . ? C27 C28 H28A 107.3 . . ? K1 C28 H28A 102.7 . . ? O5 C28 H28B 107.3 . . ? C27 C28 H28B 107.3 . . ? K1 C28 H28B 144.9 . . ? H28A C28 H28B 106.9 . . ? O5 C29 C30 114.1(6) . . ? O5 C29 H29A 108.7 . . ? C30 C29 H29A 108.7 . . ? O5 C29 H29B 108.7 . . ? C30 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? O6 C30 C29 121.6(7) . . ? O6 C30 H30A 106.9 . . ? C29 C30 H30A 106.9 . . ? O6 C30 H30B 106.9 . . ? C29 C30 H30B 106.9 . . ? H30A C30 H30B 106.7 . . ? O6 C31 C32 113.5(5) . . ? O6 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? O6 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? O7 C32 C31 117.5(6) . . ? O7 C32 H32A 107.9 . . ? C31 C32 H32A 107.9 . . ? O7 C32 H32B 107.9 . . ? C31 C32 H32B 107.9 . . ? H32A C32 H32B 107.2 . . ? O7 C33 C34 114.2(6) . . ? O7 C33 H33A 108.7 . . ? C34 C33 H33A 108.7 . . ? O7 C33 H33B 108.7 . . ? C34 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? O8 C34 C33 115.7(6) . . ? O8 C34 H34A 108.4 . . ? C33 C34 H34A 108.4 . . ? O8 C34 H34B 108.4 . . ? C33 C34 H34B 108.4 . . ? H34A C34 H34B 107.4 . . ? O8 C35 C36 115.4(5) . . ? O8 C35 H35A 108.4 . . ? C36 C35 H35A 108.4 . . ? O8 C35 H35B 108.4 . . ? C36 C35 H35B 108.4 . . ? H35A C35 H35B 107.5 . . ? O3 C36 C35 119.5(7) . . ? O3 C36 H36A 107.4 . . ? C35 C36 H36A 107.4 . . ? O3 C36 H36B 107.4 . . ? C35 C36 H36B 107.4 . . ? H36A C36 H36B 107.0 . . ? O1 N1 Fe1 161.7(3) . . ? O2 N2 Fe1 163.9(4) . . ? C7 N3 C1 117.0(3) . . ? C7 N3 Fe1 123.7(2) . . ? C1 N3 Fe1 119.1(2) . . ? C13 N4 C19 116.6(3) . . ? C13 N4 Fe1 121.4(2) . . ? C19 N4 Fe1 121.6(2) . . ? C36 O3 C25 121.9(5) . . ? C36 O3 K1 115.5(4) . . ? C25 O3 K1 114.3(3) . . ? C26 O4 C27 122.4(5) . . ? C26 O4 K1 116.9(3) . . ? C27 O4 K1 115.8(3) . . ? C28 O5 C29 120.2(6) . . ? C28 O5 K1 116.2(4) . . ? C29 O5 K1 116.9(4) . . ? C30 O6 C31 120.7(5) . . ? C30 O6 K1 115.4(4) . . ? C31 O6 K1 118.1(4) . . ? C32 O7 C33 119.4(5) . . ? C32 O7 K1 113.9(4) . . ? C33 O7 K1 113.6(3) . . ? C34 O8 C35 119.8(5) . . ? C34 O8 K1 120.4(4) . . ? C35 O8 K1 116.7(3) . . ? N1 Fe1 N2 110.73(17) . . ? N1 Fe1 N4 106.64(14) . . ? N2 Fe1 N4 109.83(15) . . ? N1 Fe1 N3 113.05(14) . . ? N2 Fe1 N3 106.84(13) . . ? N4 Fe1 N3 109.75(12) . . ? O4 K1 O5 60.92(12) . . ? O4 K1 O6 121.85(14) . . ? O5 K1 O6 61.16(15) . . ? O4 K1 O3 60.41(11) . . ? O5 K1 O3 120.43(12) . . ? O6 K1 O3 174.99(12) . . ? O4 K1 O8 120.34(12) . . ? O5 K1 O8 175.20(12) . . ? O6 K1 O8 117.81(14) . . ? O3 K1 O8 60.16(11) . . ? O4 K1 O7 177.40(13) . . ? O5 K1 O7 120.11(13) . . ? O6 K1 O7 59.46(14) . . ? O3 K1 O7 118.09(12) . . ? O8 K1 O7 58.41(12) . . ? O4 K1 C28 42.36(15) . . ? O5 K1 C28 19.16(13) . . ? O6 K1 C28 79.49(17) . . ? O3 K1 C28 102.65(15) . . ? O8 K1 C28 162.69(15) . . ? O7 K1 C28 138.90(16) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.518 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.059 ************************************************* data_a13328 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H60 Fe K N4 O8 Si4' _chemical_formula_sum 'C24 H60 Fe K N4 O8 Si4' _chemical_formula_weight 740.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 'P 21/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 23.2705(8) _cell_length_b 15.7542(6) _cell_length_c 24.0988(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.731(2) _cell_angle_gamma 90.00 _cell_volume 8206.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown(dark) _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3176 _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6472 _exptl_absorpt_correction_T_max 0.9754 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54135 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.1036 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 25.03 _reflns_number_total 14412 _reflns_number_gt 8662 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0665P)^2^+38.1418P] 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 14412 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1374 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.2275 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.6373(5) 0.3203(7) 1.2660(5) 0.081(3) Uani 1 1 d . . . H1A H 0.5952 0.2964 1.2550 0.097 Uiso 1 1 calc R . . H1B H 0.6408 0.3701 1.2922 0.097 Uiso 1 1 calc R . . C2 C 0.6837(5) 0.2560(7) 1.2979(4) 0.077(3) Uani 1 1 d . . . H2A H 0.7259 0.2779 1.3057 0.093 Uiso 1 1 calc R . . H2B H 0.6804 0.2424 1.3367 0.093 Uiso 1 1 calc R . . C3 C 0.7117(4) 0.1140(7) 1.2905(4) 0.076(3) Uani 1 1 d . . . H3A H 0.7055 0.0992 1.3278 0.091 Uiso 1 1 calc R . . H3B H 0.7555 0.1305 1.3009 0.091 Uiso 1 1 calc R . . C4 C 0.6968(4) 0.0404(6) 1.2498(4) 0.071(3) Uani 1 1 d . . . H4A H 0.7201 -0.0101 1.2708 0.085 Uiso 1 1 calc R . . H4B H 0.6521 0.0275 1.2361 0.085 Uiso 1 1 calc R . . C5 C 0.7039(5) -0.0076(6) 1.1586(5) 0.077(3) Uani 1 1 d . . . H5A H 0.6594 -0.0224 1.1411 0.092 Uiso 1 1 calc R . . H5B H 0.7271 -0.0582 1.1795 0.092 Uiso 1 1 calc R . . C6 C 0.7258(5) 0.0182(6) 1.1104(5) 0.077(3) Uani 1 1 d . . . H6A H 0.7690 0.0385 1.1280 0.092 Uiso 1 1 calc R . . H6B H 0.7243 -0.0309 1.0842 0.092 Uiso 1 1 calc R . . C7 C 0.7032(4) 0.1104(6) 1.0280(4) 0.059(2) Uani 1 1 d . . . H7A H 0.7012 0.0616 1.0014 0.071 Uiso 1 1 calc R . . H7B H 0.7460 0.1328 1.0430 0.071 Uiso 1 1 calc R . . C8 C 0.6596(4) 0.1771(7) 0.9946(4) 0.063(3) Uani 1 1 d . . . H8A H 0.6692 0.1945 0.9595 0.076 Uiso 1 1 calc R . . H8B H 0.6169 0.1547 0.9800 0.076 Uiso 1 1 calc R . . C9 C 0.6277(4) 0.3171(6) 1.0006(4) 0.062(3) Uani 1 1 d . . . H9A H 0.5834 0.3012 0.9848 0.074 Uiso 1 1 calc R . . H9B H 0.6393 0.3334 0.9665 0.074 Uiso 1 1 calc R . . C10 C 0.6380(4) 0.3903(6) 1.0427(4) 0.071(3) Uani 1 1 d . . . H10A H 0.6824 0.4057 1.0592 0.085 Uiso 1 1 calc R . . H10B H 0.6141 0.4403 1.0214 0.085 Uiso 1 1 calc R . . C11 C 0.6209(6) 0.4342(7) 1.1281(6) 0.096(4) Uani 1 1 d . . . H11A H 0.5931 0.4803 1.1057 0.116 Uiso 1 1 calc R . . H11B H 0.6636 0.4570 1.1450 0.116 Uiso 1 1 calc R . . C12 C 0.6018(6) 0.4047(7) 1.1771(6) 0.092(4) Uani 1 1 d . . . H12A H 0.5985 0.4536 1.2015 0.110 Uiso 1 1 calc R . . H12B H 0.5609 0.3766 1.1603 0.110 Uiso 1 1 calc R . . C13 C 0.9751(5) 0.0722(6) 1.2307(4) 0.079(3) Uani 1 1 d . . . H13A H 0.9483 0.0724 1.1884 0.119 Uiso 1 1 calc R . . H13B H 0.9693 0.0191 1.2492 0.119 Uiso 1 1 calc R . . H13C H 1.0184 0.0771 1.2346 0.119 Uiso 1 1 calc R . . C14 C 0.8762(4) 0.1439(6) 1.2723(5) 0.080(3) Uani 1 1 d . . . H14A H 0.8444 0.1502 1.2323 0.119 Uiso 1 1 calc R . . H14B H 0.8687 0.1849 1.2995 0.119 Uiso 1 1 calc R . . H14C H 0.8747 0.0862 1.2869 0.119 Uiso 1 1 calc R . . C15 C 1.0107(5) 0.1510(7) 1.3481(4) 0.086(3) Uani 1 1 d . . . H15A H 1.0529 0.1604 1.3498 0.129 Uiso 1 1 calc R . . H15B H 1.0073 0.0934 1.3620 0.129 Uiso 1 1 calc R . . H15C H 1.0010 0.1924 1.3737 0.129 Uiso 1 1 calc R . . C16 C 0.9530(5) 0.3694(6) 1.3354(4) 0.071(3) Uani 1 1 d . . . H16A H 0.9604 0.3201 1.3619 0.107 Uiso 1 1 calc R . . H16B H 0.9084 0.3794 1.3163 0.107 Uiso 1 1 calc R . . H16C H 0.9729 0.4195 1.3587 0.107 Uiso 1 1 calc R . . C17 C 1.0726(4) 0.3433(7) 1.3141(5) 0.092(4) Uani 1 1 d . . . H17A H 1.0841 0.2927 1.3395 0.137 Uiso 1 1 calc R . . H17B H 1.0876 0.3941 1.3387 0.137 Uiso 1 1 calc R . . H17C H 1.0913 0.3403 1.2838 0.137 Uiso 1 1 calc R . . C18 C 0.9689(5) 0.4467(5) 1.2302(4) 0.070(3) Uani 1 1 d . . . H18A H 0.9240 0.4522 1.2095 0.106 Uiso 1 1 calc R . . H18B H 0.9887 0.4434 1.2008 0.106 Uiso 1 1 calc R . . H18C H 0.9848 0.4962 1.2560 0.106 Uiso 1 1 calc R . . C19 C 1.0332(4) 0.2414(6) 1.1394(4) 0.056(2) Uani 1 1 d . . . H19A H 1.0101 0.1900 1.1408 0.084 Uiso 1 1 calc R . . H19B H 1.0492 0.2679 1.1790 0.084 Uiso 1 1 calc R . . H19C H 1.0678 0.2266 1.1274 0.084 Uiso 1 1 calc R . . C20 C 1.0293(3) 0.4139(5) 1.0849(4) 0.058(2) Uani 1 1 d . . . H20A H 1.0040 0.4564 1.0566 0.087 Uiso 1 1 calc R . . H20B H 1.0639 0.3972 1.0733 0.087 Uiso 1 1 calc R . . H20C H 1.0455 0.4382 1.1252 0.087 Uiso 1 1 calc R . . C21 C 0.9598(4) 0.2643(6) 1.0093(4) 0.066(3) Uani 1 1 d . . . H21A H 0.9326 0.3010 0.9776 0.099 Uiso 1 1 d R . . H21B H 0.9385 0.2109 1.0099 0.099 Uiso 1 1 d R . . H21C H 0.9976 0.2524 1.0018 0.099 Uiso 1 1 d R . . C22 C 0.8786(4) 0.4670(6) 0.9953(4) 0.069(3) Uani 1 1 d . . . H22A H 0.8938 0.4285 0.9718 0.103 Uiso 1 1 calc R . . H22B H 0.9111 0.5078 1.0165 0.103 Uiso 1 1 calc R . . H22C H 0.8422 0.4975 0.9686 0.103 Uiso 1 1 calc R . . C23 C 0.7896(3) 0.3357(6) 1.0054(4) 0.058(2) Uani 1 1 d . . . H23A H 0.8039 0.2917 0.9848 0.086 Uiso 1 1 calc R . . H23B H 0.7583 0.3710 0.9759 0.086 Uiso 1 1 calc R . . H23C H 0.7715 0.3089 1.0319 0.086 Uiso 1 1 calc R . . C24 C 0.8283(4) 0.4866(6) 1.0902(4) 0.067(3) Uani 1 1 d . . . H24A H 0.8628 0.5228 1.1140 0.101 Uiso 1 1 calc R . . H24B H 0.8103 0.4589 1.1164 0.101 Uiso 1 1 calc R . . H24C H 0.7967 0.5214 1.0606 0.101 Uiso 1 1 calc R . . C25 C 0.9406(7) -0.0176(8) 0.9172(6) 0.133(7) Uani 1 1 d . . . H25A H 0.9675 -0.0637 0.9410 0.159 Uiso 1 1 calc R . . H25B H 0.9231 -0.0359 0.8749 0.159 Uiso 1 1 calc R . . C26 C 0.8906(7) -0.0002(8) 0.9389(6) 0.133(7) Uani 1 1 d . . . H26A H 0.8702 -0.0540 0.9423 0.160 Uiso 1 1 calc R . . H26B H 0.9079 0.0262 0.9789 0.160 Uiso 1 1 calc R . . C27 C 0.7960(7) 0.0710(9) 0.9173(5) 0.107(5) Uani 1 1 d . . . H27A H 0.7753 0.0174 0.9206 0.128 Uiso 1 1 calc R . . H27B H 0.8103 0.1000 0.9566 0.128 Uiso 1 1 calc R . . C28 C 0.7542(6) 0.1243(9) 0.8723(6) 0.106(4) Uani 1 1 d . . . H28A H 0.7425 0.0958 0.8331 0.127 Uiso 1 1 calc R . . H28B H 0.7161 0.1324 0.8809 0.127 Uiso 1 1 calc R . . C29 C 0.7398(5) 0.2615(9) 0.8274(5) 0.089(4) Uani 1 1 d . . . H29A H 0.7022 0.2707 0.8368 0.106 Uiso 1 1 calc R . . H29B H 0.7268 0.2371 0.7867 0.106 Uiso 1 1 calc R . . C30 C 0.7718(5) 0.3435(7) 0.8296(4) 0.079(3) Uani 1 1 d . . . H30A H 0.7433 0.3840 0.8011 0.094 Uiso 1 1 calc R . . H30B H 0.7846 0.3681 0.8702 0.094 Uiso 1 1 calc R . . C31 C 0.8521(5) 0.4059(6) 0.8096(4) 0.077(3) Uani 1 1 d . . . H31A H 0.8654 0.4372 0.8479 0.092 Uiso 1 1 calc R . . H31B H 0.8225 0.4419 0.7784 0.092 Uiso 1 1 calc R . . C32 C 0.9064(5) 0.3881(6) 0.7938(5) 0.078(3) Uani 1 1 d . . . H32A H 0.8941 0.3530 0.7572 0.093 Uiso 1 1 calc R . . H32B H 0.9243 0.4419 0.7862 0.093 Uiso 1 1 calc R . . C33 C 1.0079(5) 0.3350(9) 0.8345(5) 0.111(5) Uani 1 1 d . . . H33A H 1.0280 0.3911 0.8373 0.134 Uiso 1 1 calc R . . H33B H 1.0010 0.3106 0.7947 0.134 Uiso 1 1 calc R . . C34 C 1.0481(5) 0.2776(11) 0.8823(5) 0.110(5) Uani 1 1 d . . . H34A H 1.0898 0.2743 0.8803 0.132 Uiso 1 1 calc R . . H34B H 1.0524 0.3001 0.9220 0.132 Uiso 1 1 calc R . . C35 C 1.0593(5) 0.1316(12) 0.9108(5) 0.120(6) Uani 1 1 d . . . H35A H 1.0727 0.1476 0.9534 0.144 Uiso 1 1 calc R . . H35B H 1.0966 0.1234 0.9009 0.144 Uiso 1 1 calc R . . C36 C 1.0234(8) 0.0536(9) 0.8999(5) 0.121(6) Uani 1 1 d . . . H36A H 1.0050 0.0426 0.8563 0.145 Uiso 1 1 calc R . . H36B H 1.0510 0.0054 0.9190 0.145 Uiso 1 1 calc R . . C37 C 0.8707(4) 0.1299(7) 0.7414(4) 0.075(3) Uani 1 1 d . . . H37A H 0.8314 0.1247 0.7475 0.112 Uiso 1 1 d R . . H37B H 0.8903 0.1841 0.7579 0.112 Uiso 1 1 d R . . H37C H 0.8981 0.0831 0.7617 0.112 Uiso 1 1 d R . . C38 C 0.8302(5) 0.0154(6) 0.6332(5) 0.081(3) Uani 1 1 d . . . H38A H 0.7888 0.0059 0.6337 0.121 Uiso 1 1 calc R . . H38B H 0.8592 -0.0256 0.6597 0.121 Uiso 1 1 calc R . . H38C H 0.8291 0.0082 0.5924 0.121 Uiso 1 1 calc R . . C39 C 0.9342(4) 0.1355(7) 0.6564(5) 0.088(4) Uani 1 1 d . . . H39A H 0.9306 0.1343 0.6146 0.132 Uiso 1 1 calc R . . H39B H 0.9597 0.0877 0.6779 0.132 Uiso 1 1 calc R . . H39C H 0.9535 0.1889 0.6748 0.132 Uiso 1 1 calc R . . C40 C 0.6714(4) 0.2105(6) 0.5430(4) 0.068(3) Uani 1 1 d . . . H40A H 0.6751 0.1574 0.5234 0.102 Uiso 1 1 calc R . . H40B H 0.6765 0.2588 0.5196 0.102 Uiso 1 1 calc R . . H40C H 0.6305 0.2134 0.5458 0.102 Uiso 1 1 calc R . . C41 C 0.7231(4) 0.3157(6) 0.6542(4) 0.062(2) Uani 1 1 d . . . H41A H 0.7542 0.3199 0.6947 0.093 Uiso 1 1 calc R . . H41B H 0.6816 0.3178 0.6557 0.093 Uiso 1 1 calc R . . H41C H 0.7282 0.3630 0.6300 0.093 Uiso 1 1 calc R . . C42 C 0.7090(4) 0.1290(6) 0.6622(4) 0.061(2) Uani 1 1 d . . . H42A H 0.7128 0.0733 0.6458 0.091 Uiso 1 1 calc R . . H42B H 0.6659 0.1382 0.6580 0.091 Uiso 1 1 calc R . . H42C H 0.7357 0.1311 0.7045 0.091 Uiso 1 1 calc R . . C43 C 0.8079(4) 0.1494(6) 0.4785(4) 0.068(3) Uani 1 1 d . . . H43A H 0.7731 0.1845 0.4784 0.102 Uiso 1 1 calc R . . H43B H 0.8186 0.1088 0.5116 0.102 Uiso 1 1 calc R . . H43C H 0.7963 0.1186 0.4406 0.102 Uiso 1 1 calc R . . C44 C 0.8514(5) 0.2851(7) 0.4183(4) 0.078(3) Uani 1 1 d . . . H44A H 0.8851 0.3237 0.4200 0.116 Uiso 1 1 calc R . . H44B H 0.8147 0.3182 0.4150 0.116 Uiso 1 1 calc R . . H44C H 0.8418 0.2480 0.3833 0.116 Uiso 1 1 calc R . . C45 C 0.9385(4) 0.1443(6) 0.4863(5) 0.084(3) Uani 1 1 d . . . H45A H 0.9759 0.1768 0.4911 0.126 Uiso 1 1 calc R . . H45B H 0.9245 0.1143 0.4479 0.126 Uiso 1 1 calc R . . H45C H 0.9475 0.1031 0.5188 0.126 Uiso 1 1 calc R . . C46 C 0.9288(4) 0.4622(5) 0.5455(4) 0.051(2) Uani 1 1 d . . . H46A H 0.9046 0.4624 0.5024 0.077 Uiso 1 1 calc R . . H46B H 0.9643 0.5003 0.5542 0.077 Uiso 1 1 calc R . . H46C H 0.9027 0.4817 0.5669 0.077 Uiso 1 1 calc R . . C47 C 1.0158(3) 0.3309(6) 0.5362(4) 0.056(2) Uani 1 1 d . . . H47A H 0.9955 0.3278 0.4926 0.084 Uiso 1 1 calc R . . H47B H 1.0365 0.2768 0.5514 0.084 Uiso 1 1 calc R . . H47C H 1.0465 0.3767 0.5469 0.084 Uiso 1 1 calc R . . C48 C 1.0022(4) 0.3554(5) 0.6516(3) 0.053(2) Uani 1 1 d . . . H48A H 1.0171 0.2983 0.6656 0.080 Uiso 1 1 calc R . . H48B H 0.9760 0.3759 0.6726 0.080 Uiso 1 1 calc R . . H48C H 1.0375 0.3937 0.6596 0.080 Uiso 1 1 calc R . . N1 N 0.8297(3) 0.3102(5) 1.1618(3) 0.0516(18) Uani 1 1 d . . . N2 N 0.8799(3) 0.1753(4) 1.1204(3) 0.0467(17) Uani 1 1 d . . . N3 N 0.9579(2) 0.2578(4) 1.2371(2) 0.0330(14) Uani 1 1 d . . . N4 N 0.9161(2) 0.3437(4) 1.0982(2) 0.0327(14) Uani 1 1 d . . . N5 N 0.8558(3) 0.3832(4) 0.6341(3) 0.0501(17) Uani 1 1 d . . . N6 N 0.7699(3) 0.3426(5) 0.5274(3) 0.0520(18) Uani 1 1 d . . . N7 N 0.8059(2) 0.2025(4) 0.6197(2) 0.0350(14) Uani 1 1 d . . . N8 N 0.8972(2) 0.2805(4) 0.5505(2) 0.0308(13) Uani 1 1 d . . . O1 O 0.7776(3) 0.3038(5) 1.1585(3) 0.077(2) Uani 1 1 d . . . O2 O 0.8660(3) 0.1166(4) 1.0898(3) 0.081(2) Uani 1 1 d . . . O3 O 0.6474(3) 0.3459(4) 1.2136(3) 0.0654(17) Uani 1 1 d . . . O4 O 0.6726(3) 0.1820(4) 1.2616(2) 0.0611(16) Uani 1 1 d . . . O5 O 0.7131(3) 0.0601(4) 1.1998(3) 0.0605(16) Uani 1 1 d . . . O6 O 0.6871(2) 0.0833(4) 1.0771(2) 0.0534(15) Uani 1 1 d . . . O7 O 0.6641(2) 0.2472(4) 1.0313(2) 0.0485(14) Uani 1 1 d . . . O8 O 0.6184(3) 0.3661(4) 1.0892(3) 0.0604(16) Uani 1 1 d . . . O9 O 0.9764(4) 0.0597(4) 0.9228(3) 0.084(2) Uani 1 1 d . . . O10 O 0.8479(4) 0.0536(4) 0.8997(3) 0.084(2) Uani 1 1 d . . . O11 O 0.7800(3) 0.2041(4) 0.8694(3) 0.0691(18) Uani 1 1 d . . . O12 O 0.8233(3) 0.3300(4) 0.8149(2) 0.0591(15) Uani 1 1 d . . . O13 O 0.9505(3) 0.3442(4) 0.8422(3) 0.0698(18) Uani 1 1 d . . . O14 O 1.0213(3) 0.1967(6) 0.8742(3) 0.086(2) Uani 1 1 d . . . O15 O 0.8501(3) 0.4528(4) 0.6498(3) 0.0728(19) Uani 1 1 d . . . O16 O 0.7333(3) 0.3893(5) 0.4952(3) 0.087(2) Uani 1 1 d . . . Si1 Si 0.95476(10) 0.16379(14) 1.26907(9) 0.0446(6) Uani 1 1 d . . . Si2 Si 0.98625(9) 0.34869(15) 1.27646(9) 0.0415(5) Uani 1 1 d . . . Si3 Si 0.98056(9) 0.31791(14) 1.08389(9) 0.0376(5) Uani 1 1 d . . . Si4 Si 0.85693(9) 0.40393(14) 1.05080(9) 0.0394(5) Uani 1 1 d . . . Si5 Si 0.85652(9) 0.12706(14) 0.65988(9) 0.0399(5) Uani 1 1 d . . . Si6 Si 0.73300(9) 0.21440(15) 0.62024(9) 0.0411(5) Uani 1 1 d . . . Si7 Si 0.87590(10) 0.21874(15) 0.48806(9) 0.0429(5) Uani 1 1 d . . . Si8 Si 0.95653(9) 0.35246(13) 0.56996(9) 0.0344(5) Uani 1 1 d . . . Fe1 Fe 0.89443(4) 0.27099(7) 1.15409(4) 0.0309(3) Uani 1 1 d . . . Fe2 Fe 0.83241(4) 0.30263(7) 0.58330(4) 0.0335(3) Uani 1 1 d . . . K1 K 0.67014(8) 0.21527(11) 1.14544(7) 0.0461(4) Uani 1 1 d . . . K2 K 0.90105(8) 0.19879(11) 0.87389(7) 0.0480(5) 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 0.093(8) 0.092(9) 0.076(7) -0.032(6) 0.052(6) -0.016(7) C2 0.077(7) 0.107(9) 0.044(5) -0.018(6) 0.019(5) -0.015(7) C3 0.060(6) 0.105(9) 0.051(6) 0.029(6) 0.009(5) -0.006(6) C4 0.071(6) 0.061(7) 0.076(7) 0.035(6) 0.023(5) 0.004(5) C5 0.086(7) 0.043(6) 0.111(8) 0.007(6) 0.048(7) 0.011(5) C6 0.084(7) 0.048(6) 0.110(8) 0.000(6) 0.048(7) 0.016(6) C7 0.053(5) 0.065(7) 0.069(6) -0.027(5) 0.033(5) -0.023(5) C8 0.050(5) 0.099(8) 0.041(5) -0.013(5) 0.018(4) -0.018(5) C9 0.038(5) 0.089(8) 0.051(5) 0.025(5) 0.007(4) -0.006(5) C10 0.053(6) 0.071(7) 0.084(7) 0.039(6) 0.019(5) 0.007(5) C11 0.111(9) 0.044(7) 0.141(11) 0.011(7) 0.055(9) 0.019(6) C12 0.106(9) 0.063(8) 0.120(10) -0.018(7) 0.058(8) 0.016(7) C13 0.121(9) 0.057(7) 0.057(6) 0.020(5) 0.030(6) 0.032(6) C14 0.085(7) 0.073(7) 0.095(8) 0.029(6) 0.049(6) -0.006(6) C15 0.112(9) 0.083(8) 0.045(5) 0.019(5) 0.008(5) 0.028(7) C16 0.098(7) 0.070(7) 0.056(6) -0.013(5) 0.041(5) -0.009(6) C17 0.050(6) 0.111(9) 0.093(8) -0.041(7) 0.004(5) -0.028(6) C18 0.111(8) 0.043(6) 0.064(6) -0.015(5) 0.040(6) -0.027(5) C19 0.040(5) 0.067(6) 0.062(5) -0.001(5) 0.021(4) 0.013(4) C20 0.037(5) 0.055(6) 0.084(6) 0.007(5) 0.025(4) -0.002(4) C21 0.069(6) 0.076(7) 0.059(6) -0.016(5) 0.031(5) 0.005(5) C22 0.057(6) 0.087(8) 0.056(5) 0.036(5) 0.015(4) 0.004(5) C23 0.039(5) 0.078(7) 0.051(5) 0.008(5) 0.012(4) -0.002(4) C24 0.058(6) 0.067(7) 0.070(6) 0.005(5) 0.016(5) 0.030(5) C25 0.145(13) 0.043(8) 0.113(11) -0.017(7) -0.065(10) 0.031(9) C26 0.153(14) 0.056(9) 0.114(11) 0.041(8) -0.040(10) -0.024(9) C27 0.135(12) 0.119(11) 0.064(8) 0.001(7) 0.034(8) -0.060(9) C28 0.092(9) 0.157(13) 0.086(9) -0.029(9) 0.054(8) -0.058(9) C29 0.051(6) 0.151(12) 0.067(7) 0.002(7) 0.025(5) 0.014(7) C30 0.068(7) 0.094(9) 0.066(7) -0.006(6) 0.015(5) 0.019(6) C31 0.111(9) 0.038(6) 0.063(6) 0.004(5) 0.013(6) -0.001(6) C32 0.094(8) 0.053(7) 0.079(7) 0.017(5) 0.023(6) -0.018(6) C33 0.071(8) 0.176(14) 0.093(9) 0.022(9) 0.036(7) -0.039(8) C34 0.041(6) 0.207(17) 0.076(8) 0.032(10) 0.014(6) -0.001(8) C35 0.066(8) 0.238(19) 0.054(7) 0.013(10) 0.022(6) 0.079(10) C36 0.156(15) 0.106(12) 0.062(8) -0.020(8) -0.004(8) 0.082(11) C37 0.073(6) 0.087(8) 0.045(5) 0.010(5) -0.001(5) 0.008(6) C38 0.100(8) 0.044(6) 0.092(8) 0.003(5) 0.028(6) 0.014(6) C39 0.056(6) 0.081(8) 0.133(9) 0.073(7) 0.041(6) 0.034(5) C40 0.039(5) 0.091(8) 0.063(6) 0.011(5) 0.007(4) -0.019(5) C41 0.046(5) 0.064(6) 0.079(6) 0.005(5) 0.027(5) 0.008(4) C42 0.049(5) 0.065(6) 0.072(6) 0.020(5) 0.027(4) -0.006(4) C43 0.082(7) 0.073(7) 0.052(5) -0.028(5) 0.028(5) -0.039(5) C44 0.092(7) 0.095(8) 0.040(5) -0.004(5) 0.017(5) -0.034(6) C45 0.077(7) 0.058(7) 0.111(8) -0.043(6) 0.029(6) -0.005(5) C46 0.049(5) 0.036(5) 0.062(5) 0.013(4) 0.012(4) -0.001(4) C47 0.037(5) 0.065(6) 0.069(6) -0.007(5) 0.023(4) -0.007(4) C48 0.046(5) 0.037(5) 0.055(5) -0.004(4) -0.007(4) -0.009(4) N1 0.038(4) 0.079(5) 0.042(4) 0.014(4) 0.018(3) 0.004(4) N2 0.047(4) 0.041(4) 0.040(4) -0.003(3) 0.003(3) -0.016(3) N3 0.031(3) 0.036(4) 0.028(3) 0.002(3) 0.006(2) 0.000(3) N4 0.028(3) 0.040(4) 0.031(3) 0.003(3) 0.013(2) 0.001(3) N5 0.054(4) 0.041(5) 0.063(4) -0.012(4) 0.030(4) -0.012(3) N6 0.038(4) 0.061(5) 0.058(4) 0.015(4) 0.019(3) -0.006(3) N7 0.035(3) 0.032(4) 0.041(3) 0.003(3) 0.017(3) 0.000(3) N8 0.025(3) 0.036(4) 0.029(3) -0.005(3) 0.008(2) -0.006(3) O1 0.038(3) 0.125(6) 0.078(4) 0.015(4) 0.032(3) 0.000(4) O2 0.066(4) 0.062(5) 0.086(5) -0.032(4) -0.004(4) -0.003(3) O3 0.067(4) 0.060(4) 0.078(4) -0.025(3) 0.037(4) -0.014(3) O4 0.050(3) 0.088(5) 0.040(3) -0.005(3) 0.011(3) -0.019(3) O5 0.059(4) 0.050(4) 0.069(4) 0.011(3) 0.021(3) -0.006(3) O6 0.052(3) 0.051(4) 0.063(4) -0.020(3) 0.028(3) -0.012(3) O7 0.041(3) 0.064(4) 0.036(3) 0.005(3) 0.008(2) -0.004(3) O8 0.055(4) 0.047(4) 0.078(4) 0.014(3) 0.023(3) 0.007(3) O9 0.105(6) 0.054(5) 0.062(4) -0.017(3) -0.007(4) 0.029(4) O10 0.113(6) 0.058(5) 0.057(4) 0.004(3) 0.004(4) -0.032(4) O11 0.065(4) 0.080(5) 0.071(4) -0.012(4) 0.036(4) -0.018(4) O12 0.063(4) 0.050(4) 0.062(4) -0.006(3) 0.020(3) 0.004(3) O13 0.070(4) 0.075(5) 0.056(4) 0.018(3) 0.013(3) -0.013(4) O14 0.066(5) 0.132(7) 0.054(4) 0.008(4) 0.016(4) 0.027(5) O15 0.097(5) 0.038(4) 0.095(5) -0.022(4) 0.050(4) -0.011(4) O16 0.050(4) 0.096(6) 0.097(5) 0.052(4) 0.007(4) 0.019(4) Si1 0.0538(14) 0.0427(14) 0.0325(11) 0.0069(10) 0.0104(10) 0.0067(11) Si2 0.0383(12) 0.0494(15) 0.0346(11) -0.0087(10) 0.0108(9) -0.0097(10) Si3 0.0348(11) 0.0456(14) 0.0379(11) 0.0001(10) 0.0197(9) 0.0027(10) Si4 0.0345(11) 0.0444(14) 0.0397(12) 0.0120(10) 0.0141(9) 0.0083(10) Si5 0.0374(12) 0.0374(13) 0.0420(12) 0.0099(10) 0.0111(9) 0.0011(10) Si6 0.0282(11) 0.0512(15) 0.0400(12) 0.0083(10) 0.0083(9) -0.0053(10) Si7 0.0432(12) 0.0473(15) 0.0383(12) -0.0133(10) 0.0152(9) -0.0171(10) Si8 0.0289(10) 0.0310(12) 0.0384(11) 0.0005(9) 0.0069(8) -0.0042(9) Fe1 0.0247(5) 0.0378(6) 0.0279(5) 0.0039(4) 0.0068(4) -0.0014(4) Fe2 0.0288(5) 0.0351(6) 0.0352(6) 0.0021(5) 0.0102(4) -0.0020(5) K1 0.0538(11) 0.0438(11) 0.0420(9) 0.0011(8) 0.0194(8) 0.0004(8) K2 0.0531(11) 0.0477(12) 0.0415(10) 0.0008(8) 0.0155(8) 0.0026(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 O3 1.427(11) . ? C1 C2 1.473(14) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O4 1.424(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O4 1.411(11) . ? C3 C4 1.475(13) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O5 1.425(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O5 1.418(11) . ? C5 C6 1.486(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O6 1.404(10) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O6 1.432(9) . ? C7 C8 1.476(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O7 1.394(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O7 1.420(10) . ? C9 C10 1.495(13) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O8 1.411(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O8 1.411(12) . ? C11 C12 1.482(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O3 1.437(12) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 Si1 1.866(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si1 1.884(9) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si1 1.878(9) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si2 1.880(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.876(9) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 Si2 1.859(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 Si3 1.879(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 Si3 1.886(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 Si3 1.881(8) . ? C21 K2 3.205(8) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 Si4 1.878(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 Si4 1.880(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 Si4 1.873(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 O9 1.453(15) . ? C25 C26 1.47(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O10 1.380(13) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.430(16) . ? C27 O10 1.445(14) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O11 1.406(13) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O11 1.419(12) . ? C29 C30 1.483(15) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O12 1.389(11) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 O12 1.399(10) . ? C31 C32 1.475(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O13 1.417(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O13 1.422(12) . ? C33 C34 1.490(16) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O14 1.400(15) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O14 1.427(14) . ? C35 C36 1.452(18) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O9 1.401(16) . ? C36 K2 3.523(13) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 Si5 1.868(8) . ? C37 K2 3.194(9) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 Si5 1.895(9) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 Si5 1.845(9) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 Si6 1.884(8) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 Si6 1.845(9) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 Si6 1.887(8) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 Si7 1.866(8) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 Si7 1.881(9) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 Si7 1.883(9) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 Si8 1.864(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 Si8 1.875(8) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 Si8 1.858(7) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? N1 O1 1.190(7) . ? N1 Fe1 1.700(6) . ? N2 O2 1.152(8) . ? N2 Fe1 1.686(7) . ? N3 Si1 1.683(6) . ? N3 Si2 1.709(6) . ? N3 Fe1 2.010(5) . ? N4 Si3 1.708(5) . ? N4 Si4 1.713(6) . ? N4 Fe1 1.971(5) . ? N5 O15 1.184(8) . ? N5 Fe2 1.706(7) . ? N6 O16 1.175(8) . ? N6 Fe2 1.695(7) . ? N7 Si5 1.701(6) . ? N7 Si6 1.712(6) . ? N7 Fe2 2.009(6) . ? N8 Si7 1.704(5) . ? N8 Si8 1.712(5) . ? N8 Fe2 1.976(5) . ? O1 K1 2.778(6) . ? O3 K1 2.803(6) . ? O4 K1 2.828(6) . ? O5 K1 2.778(6) . ? O6 K1 2.769(5) . ? O7 K1 2.748(5) . ? O8 K1 2.779(6) . ? O9 K2 2.781(7) . ? O10 K2 2.778(7) . ? O11 K2 2.779(6) . ? O12 K2 2.768(6) . ? O13 K2 2.794(6) . ? O14 K2 2.795(7) . ? K2 H21A 2.8309 . ? K2 H21B 3.0691 . ? K2 H37B 2.7232 . ? 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 O3 C1 C2 109.1(8) . . ? O3 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? O3 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? O4 C2 C1 108.1(8) . . ? O4 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? O4 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? O4 C3 C4 108.6(7) . . ? O4 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? O4 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? O5 C4 C3 108.7(8) . . ? O5 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? O5 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.3 . . ? O5 C5 C6 109.6(8) . . ? O5 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? O5 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? O6 C6 C5 108.3(8) . . ? O6 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O6 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? O6 C7 C8 109.0(7) . . ? O6 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O6 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O7 C8 C7 110.0(7) . . ? O7 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? O7 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O7 C9 C10 109.3(7) . . ? O7 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? O7 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? O8 C10 C9 108.2(8) . . ? O8 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O8 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? O8 C11 C12 109.8(9) . . ? O8 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? O8 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O3 C12 C11 108.6(9) . . ? O3 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? O3 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 K2 168.3(5) . . ? Si3 C21 H21A 110.1 . . ? K2 C21 H21A 59.2 . . ? Si3 C21 H21B 108.9 . . ? K2 C21 H21B 73.2 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.4 . . ? K2 C21 H21C 79.9 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si4 C22 H22A 109.5 . . ? Si4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O9 C25 C26 108.1(11) . . ? O9 C25 H25A 110.1 . . ? C26 C25 H25A 110.1 . . ? O9 C25 H25B 110.1 . . ? C26 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? O10 C26 C25 109.7(13) . . ? O10 C26 H26A 109.7 . . ? C25 C26 H26A 109.7 . . ? O10 C26 H26B 109.7 . . ? C25 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C28 C27 O10 107.2(9) . . ? C28 C27 H27A 110.3 . . ? O10 C27 H27A 110.3 . . ? C28 C27 H27B 110.3 . . ? O10 C27 H27B 110.3 . . ? H27A C27 H27B 108.5 . . ? O11 C28 C27 112.3(10) . . ? O11 C28 H28A 109.1 . . ? C27 C28 H28A 109.1 . . ? O11 C28 H28B 109.1 . . ? C27 C28 H28B 109.1 . . ? H28A C28 H28B 107.9 . . ? O11 C29 C30 109.9(9) . . ? O11 C29 H29A 109.7 . . ? C30 C29 H29A 109.7 . . ? O11 C29 H29B 109.7 . . ? C30 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? O12 C30 C29 109.1(8) . . ? O12 C30 H30A 109.9 . . ? C29 C30 H30A 109.9 . . ? O12 C30 H30B 109.9 . . ? C29 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? O12 C31 C32 110.2(8) . . ? O12 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? O12 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? O13 C32 C31 108.0(8) . . ? O13 C32 H32A 110.1 . . ? C31 C32 H32A 110.1 . . ? O13 C32 H32B 110.1 . . ? C31 C32 H32B 110.1 . . ? H32A C32 H32B 108.4 . . ? O13 C33 C34 108.1(8) . . ? O13 C33 H33A 110.1 . . ? C34 C33 H33A 110.1 . . ? O13 C33 H33B 110.1 . . ? C34 C33 H33B 110.1 . . ? H33A C33 H33B 108.4 . . ? O14 C34 C33 109.0(10) . . ? O14 C34 H34A 109.9 . . ? C33 C34 H34A 109.9 . . ? O14 C34 H34B 109.9 . . ? C33 C34 H34B 109.9 . . ? H34A C34 H34B 108.3 . . ? O14 C35 C36 108.3(10) . . ? O14 C35 H35A 110.0 . . ? C36 C35 H35A 110.0 . . ? O14 C35 H35B 110.0 . . ? C36 C35 H35B 110.0 . . ? H35A C35 H35B 108.4 . . ? O9 C36 C35 110.5(10) . . ? O9 C36 K2 47.7(5) . . ? C35 C36 K2 81.7(7) . . ? O9 C36 H36A 109.5 . . ? C35 C36 H36A 109.5 . . ? K2 C36 H36A 85.4 . . ? O9 C36 H36B 109.5 . . ? C35 C36 H36B 109.5 . . ? K2 C36 H36B 157.2 . . ? H36A C36 H36B 108.1 . . ? Si5 C37 K2 161.3(5) . . ? Si5 C37 H37A 110.1 . . ? K2 C37 H37A 75.7 . . ? Si5 C37 H37B 108.7 . . ? K2 C37 H37B 53.3 . . ? H37A C37 H37B 109.5 . . ? Si5 C37 H37C 109.6 . . ? K2 C37 H37C 83.9 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si5 C38 H38A 109.5 . . ? Si5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si5 C39 H39A 109.5 . . ? Si5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si6 C40 H40A 109.5 . . ? Si6 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si6 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si6 C41 H41A 109.5 . . ? Si6 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si6 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si6 C42 H42A 109.5 . . ? Si6 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si6 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si7 C43 H43A 109.5 . . ? Si7 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si7 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si7 C44 H44A 109.5 . . ? Si7 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si7 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si7 C45 H45A 109.5 . . ? Si7 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si7 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si8 C46 H46A 109.5 . . ? Si8 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si8 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si8 C47 H47A 109.5 . . ? Si8 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si8 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si8 C48 H48A 109.5 . . ? Si8 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si8 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O1 N1 Fe1 152.1(7) . . ? O2 N2 Fe1 170.0(6) . . ? Si1 N3 Si2 123.8(3) . . ? Si1 N3 Fe1 114.0(3) . . ? Si2 N3 Fe1 117.1(3) . . ? Si3 N4 Si4 123.2(3) . . ? Si3 N4 Fe1 117.7(3) . . ? Si4 N4 Fe1 115.6(3) . . ? O15 N5 Fe2 150.9(7) . . ? O16 N6 Fe2 163.0(7) . . ? Si5 N7 Si6 123.4(3) . . ? Si5 N7 Fe2 122.5(3) . . ? Si6 N7 Fe2 112.5(3) . . ? Si7 N8 Si8 124.2(3) . . ? Si7 N8 Fe2 116.0(3) . . ? Si8 N8 Fe2 115.5(3) . . ? N1 O1 K1 154.5(6) . . ? C1 O3 C12 113.4(8) . . ? C1 O3 K1 116.2(6) . . ? C12 O3 K1 111.8(5) . . ? C3 O4 C2 112.4(7) . . ? C3 O4 K1 113.7(5) . . ? C2 O4 K1 112.9(5) . . ? C5 O5 C4 114.2(7) . . ? C5 O5 K1 113.4(5) . . ? C4 O5 K1 115.4(5) . . ? C6 O6 C7 112.4(7) . . ? C6 O6 K1 114.3(5) . . ? C7 O6 K1 114.0(5) . . ? C8 O7 C9 113.2(7) . . ? C8 O7 K1 117.1(5) . . ? C9 O7 K1 117.6(5) . . ? C11 O8 C10 112.1(8) . . ? C11 O8 K1 115.0(6) . . ? C10 O8 K1 114.2(5) . . ? C36 O9 C25 114.2(11) . . ? C36 O9 K2 110.4(7) . . ? C25 O9 K2 111.8(6) . . ? C26 O10 C27 112.6(11) . . ? C26 O10 K2 113.0(7) . . ? C27 O10 K2 113.5(7) . . ? C28 O11 C29 115.1(9) . . ? C28 O11 K2 114.6(7) . . ? C29 O11 K2 116.0(5) . . ? C30 O12 C31 112.4(8) . . ? C30 O12 K2 116.4(6) . . ? C31 O12 K2 116.2(5) . . ? C32 O13 C33 111.7(8) . . ? C32 O13 K2 112.3(5) . . ? C33 O13 K2 117.0(7) . . ? C34 O14 C35 115.3(10) . . ? C34 O14 K2 112.6(6) . . ? C35 O14 K2 113.6(7) . . ? N3 Si1 C13 113.1(4) . . ? N3 Si1 C15 115.3(4) . . ? C13 Si1 C15 102.2(4) . . ? N3 Si1 C14 111.9(4) . . ? C13 Si1 C14 108.6(5) . . ? C15 Si1 C14 105.0(5) . . ? N3 Si2 C18 114.2(3) . . ? N3 Si2 C17 110.8(4) . . ? C18 Si2 C17 106.5(5) . . ? N3 Si2 C16 112.5(4) . . ? C18 Si2 C16 104.5(4) . . ? C17 Si2 C16 108.0(5) . . ? N4 Si3 C19 113.5(3) . . ? N4 Si3 C21 111.5(3) . . ? C19 Si3 C21 105.2(4) . . ? N4 Si3 C20 112.1(3) . . ? C19 Si3 C20 105.9(4) . . ? C21 Si3 C20 108.2(4) . . ? N4 Si4 C24 113.4(3) . . ? N4 Si4 C22 114.0(3) . . ? C24 Si4 C22 103.4(4) . . ? N4 Si4 C23 111.2(4) . . ? C24 Si4 C23 108.4(4) . . ? C22 Si4 C23 105.8(4) . . ? N7 Si5 C39 114.0(3) . . ? N7 Si5 C37 113.4(4) . . ? C39 Si5 C37 104.6(5) . . ? N7 Si5 C38 112.8(4) . . ? C39 Si5 C38 104.5(5) . . ? C37 Si5 C38 106.8(5) . . ? N7 Si6 C41 112.6(3) . . ? N7 Si6 C40 112.5(3) . . ? C41 Si6 C40 106.9(4) . . ? N7 Si6 C42 114.7(3) . . ? C41 Si6 C42 105.6(4) . . ? C40 Si6 C42 103.8(4) . . ? N8 Si7 C43 113.5(3) . . ? N8 Si7 C44 111.4(4) . . ? C43 Si7 C44 104.7(4) . . ? N8 Si7 C45 113.7(4) . . ? C43 Si7 C45 105.1(4) . . ? C44 Si7 C45 107.8(5) . . ? N8 Si8 C48 113.2(3) . . ? N8 Si8 C46 112.2(3) . . ? C48 Si8 C46 107.9(4) . . ? N8 Si8 C47 114.2(3) . . ? C48 Si8 C47 103.9(4) . . ? C46 Si8 C47 104.8(4) . . ? N2 Fe1 N1 110.5(3) . . ? N2 Fe1 N4 104.3(3) . . ? N1 Fe1 N4 108.9(3) . . ? N2 Fe1 N3 109.2(3) . . ? N1 Fe1 N3 106.4(3) . . ? N4 Fe1 N3 117.5(2) . . ? N6 Fe2 N5 104.2(3) . . ? N6 Fe2 N8 107.7(3) . . ? N5 Fe2 N8 109.3(3) . . ? N6 Fe2 N7 109.0(3) . . ? N5 Fe2 N7 109.8(3) . . ? N8 Fe2 N7 116.1(2) . . ? O7 K1 O6 60.53(18) . . ? O7 K1 O1 74.46(17) . . ? O6 K1 O1 97.12(18) . . ? O7 K1 O5 120.58(19) . . ? O6 K1 O5 60.92(18) . . ? O1 K1 O5 103.70(19) . . ? O7 K1 O8 60.23(18) . . ? O6 K1 O8 118.93(19) . . ? O1 K1 O8 80.51(19) . . ? O5 K1 O8 175.79(18) . . ? O7 K1 O3 120.1(2) . . ? O6 K1 O3 177.32(17) . . ? O1 K1 O3 85.54(19) . . ? O5 K1 O3 118.9(2) . . ? O8 K1 O3 61.0(2) . . ? O7 K1 O4 178.32(16) . . ? O6 K1 O4 119.6(2) . . ? O1 K1 O4 107.08(18) . . ? O5 K1 O4 59.90(19) . . ? O8 K1 O4 119.2(2) . . ? O3 K1 O4 59.7(2) . . ? O12 K2 O10 118.0(2) . . ? O12 K2 O11 59.8(2) . . ? O10 K2 O11 60.3(2) . . ? O12 K2 O9 174.63(19) . . ? O10 K2 O9 61.3(3) . . ? O11 K2 O9 120.7(3) . . ? O12 K2 O13 60.28(19) . . ? O10 K2 O13 177.25(19) . . ? O11 K2 O13 118.6(2) . . ? O9 K2 O13 120.2(2) . . ? O12 K2 O14 118.2(2) . . ? O10 K2 O14 121.2(3) . . ? O11 K2 O14 177.8(2) . . ? O9 K2 O14 61.1(3) . . ? O13 K2 O14 59.8(2) . . ? O12 K2 C37 83.1(2) . . ? O10 K2 C37 89.6(2) . . ? O11 K2 C37 97.2(2) . . ? O9 K2 C37 91.6(2) . . ? O13 K2 C37 88.1(2) . . ? O14 K2 C37 81.4(2) . . ? O12 K2 C21 103.5(2) . . ? O10 K2 C21 95.4(2) . . ? O11 K2 C21 94.3(2) . . ? O9 K2 C21 81.8(2) . . ? O13 K2 C21 87.2(2) . . ? O14 K2 C21 87.2(2) . . ? C37 K2 C21 168.5(2) . . ? O12 K2 C36 155.1(3) . . ? O10 K2 C36 79.8(4) . . ? O11 K2 C36 140.1(4) . . ? O9 K2 C36 21.9(3) . . ? O13 K2 C36 101.1(4) . . ? O14 K2 C36 41.4(4) . . ? C37 K2 C36 79.8(3) . . ? C21 K2 C36 90.9(3) . . ? O12 K2 H21A 86.3 . . ? O10 K2 H21A 105.2 . . ? O11 K2 H21A 86.9 . . ? O9 K2 H21A 99.0 . . ? O13 K2 H21A 77.1 . . ? O14 K2 H21A 94.1 . . ? C37 K2 H21A 164.7 . . ? C21 K2 H21A 17.3 . . ? C36 K2 H21A 106.5 . . ? O12 K2 H21B 112.1 . . ? O10 K2 H21B 77.6 . . ? O11 K2 H21B 85.6 . . ? O9 K2 H21B 73.2 . . ? O13 K2 H21B 105.0 . . ? O14 K2 H21B 96.3 . . ? C37 K2 H21B 163.5 . . ? C21 K2 H21B 17.8 . . ? C36 K2 H21B 87.7 . . ? H21A K2 H21B 31.1 . . ? O12 K2 H37B 75.0 . . ? O10 K2 H37B 106.3 . . ? O11 K2 H37B 104.8 . . ? O9 K2 H37B 99.9 . . ? O13 K2 H37B 71.3 . . ? O14 K2 H37B 73.3 . . ? C37 K2 H37B 16.8 . . ? C21 K2 H37B 156.2 . . ? C36 K2 H37B 83.6 . . ? H21A K2 H37B 148.2 . . ? H21B K2 H37B 169.6 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.994 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.090 ********************************************** data_a12838 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H80 Fe K N4 O10 Si2' _chemical_formula_sum 'C44 H80 Fe K N4 O10 Si2' _chemical_formula_weight 976.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.8975(9) _cell_length_b 22.4576(12) _cell_length_c 30.9214(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11039.5(11) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown(dark) _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4200 _exptl_absorpt_coefficient_mu 0.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8972 _exptl_absorpt_correction_T_max 0.9528 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62208 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9717 _reflns_number_gt 6474 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0584P)^2^+8.5360P] 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 9717 _refine_ls_number_parameters 557 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.9406(2) 0.23976(17) 0.44427(12) 0.0590(10) Uani 1 1 d . . . H1A H 0.9355 0.2668 0.4195 0.089 Uiso 1 1 calc R . . H1B H 0.9994 0.2275 0.4475 0.089 Uiso 1 1 calc R . . H1C H 0.9221 0.2602 0.4706 0.089 Uiso 1 1 calc R . . C2 C 0.9219(2) 0.13119(19) 0.38820(13) 0.0638(11) Uani 1 1 d . . . H2A H 0.8888 0.0954 0.3819 0.096 Uiso 1 1 calc R . . H2B H 0.9796 0.1197 0.3957 0.096 Uiso 1 1 calc R . . H2C H 0.9228 0.1571 0.3627 0.096 Uiso 1 1 calc R . . C3 C 0.8842(2) 0.12208(19) 0.48317(12) 0.0658(11) Uani 1 1 d . . . H3A H 0.8495 0.0865 0.4790 0.099 Uiso 1 1 calc R . . H3B H 0.8657 0.1432 0.5092 0.099 Uiso 1 1 calc R . . H3C H 0.9433 0.1104 0.4865 0.099 Uiso 1 1 calc R . . C4 C 0.70793(19) 0.16220(13) 0.45348(10) 0.0341(7) Uani 1 1 d . . . C5 C 0.67467(19) 0.10571(14) 0.44377(10) 0.0370(7) Uani 1 1 d . . . C6 C 0.7019(2) 0.07207(16) 0.40378(12) 0.0557(10) Uani 1 1 d . . . H6A H 0.6722 0.0338 0.4025 0.083 Uiso 1 1 calc R . . H6B H 0.7626 0.0650 0.4049 0.083 Uiso 1 1 calc R . . H6C H 0.6883 0.0956 0.3780 0.083 Uiso 1 1 calc R . . C7 C 0.6174(2) 0.07874(15) 0.47178(11) 0.0438(8) Uani 1 1 d . . . H7 H 0.5962 0.0404 0.4647 0.053 Uiso 1 1 calc R . . C8 C 0.5901(2) 0.10604(17) 0.50980(11) 0.0462(9) Uani 1 1 d . . . C9 C 0.5286(2) 0.0750(2) 0.53981(13) 0.0698(12) Uani 1 1 d . . . H9A H 0.5130 0.0363 0.5276 0.105 Uiso 1 1 calc R . . H9B H 0.4781 0.0996 0.5431 0.105 Uiso 1 1 calc R . . H9C H 0.5550 0.0691 0.5681 0.105 Uiso 1 1 calc R . . C10 C 0.6232(2) 0.16151(16) 0.51899(11) 0.0469(9) Uani 1 1 d . . . H10 H 0.6061 0.1809 0.5449 0.056 Uiso 1 1 calc R . . C11 C 0.6804(2) 0.19030(14) 0.49208(10) 0.0413(8) Uani 1 1 d . . . C12 C 0.7148(3) 0.25036(17) 0.50429(12) 0.0629(11) Uani 1 1 d . . . H12A H 0.7538 0.2640 0.4819 0.094 Uiso 1 1 calc R . . H12B H 0.7445 0.2474 0.5320 0.094 Uiso 1 1 calc R . . H12C H 0.6683 0.2788 0.5070 0.094 Uiso 1 1 calc R . . C13 C 0.5783(2) 0.30291(13) 0.36310(10) 0.0374(8) Uani 1 1 d . . . C14 C 0.5049(2) 0.29137(15) 0.38707(11) 0.0458(9) Uani 1 1 d . . . C15 C 0.5108(3) 0.27528(18) 0.43449(12) 0.0635(11) Uani 1 1 d . . . H15A H 0.5699 0.2756 0.4435 0.095 Uiso 1 1 calc R . . H15B H 0.4872 0.2355 0.4391 0.095 Uiso 1 1 calc R . . H15C H 0.4792 0.3044 0.4516 0.095 Uiso 1 1 calc R . . C16 C 0.4263(2) 0.29327(16) 0.36646(14) 0.0569(10) Uani 1 1 d . . . H16 H 0.3771 0.2862 0.3831 0.068 Uiso 1 1 calc R . . C17 C 0.4177(2) 0.30517(16) 0.32245(15) 0.0572(10) Uani 1 1 d . . . C18 C 0.3310(3) 0.3080(2) 0.30121(17) 0.0866(15) Uani 1 1 d . . . H18A H 0.3374 0.3168 0.2703 0.130 Uiso 1 1 calc R . . H18B H 0.2975 0.3395 0.3149 0.130 Uiso 1 1 calc R . . H18C H 0.3024 0.2697 0.3048 0.130 Uiso 1 1 calc R . . C19 C 0.4901(2) 0.31328(15) 0.29915(12) 0.0504(9) Uani 1 1 d . . . H19 H 0.4857 0.3197 0.2689 0.060 Uiso 1 1 calc R . . C20 C 0.5700(2) 0.31256(14) 0.31794(11) 0.0421(8) Uani 1 1 d . . . C21 C 0.6455(2) 0.32116(18) 0.28887(11) 0.0559(10) Uani 1 1 d . . . H21A H 0.6970 0.3199 0.3063 0.084 Uiso 1 1 calc R . . H21B H 0.6414 0.3598 0.2743 0.084 Uiso 1 1 calc R . . H21C H 0.6471 0.2894 0.2672 0.084 Uiso 1 1 calc R . . C22 C 0.6243(3) 0.40512(19) 0.44663(15) 0.0782(13) Uani 1 1 d . . . H22A H 0.5652 0.4066 0.4376 0.117 Uiso 1 1 calc R . . H22B H 0.6437 0.4454 0.4537 0.117 Uiso 1 1 calc R . . H22C H 0.6297 0.3796 0.4722 0.117 Uiso 1 1 calc R . . C23 C 0.6810(4) 0.43314(19) 0.35879(15) 0.1003(19) Uani 1 1 d . . . H23A H 0.6229 0.4349 0.3483 0.150 Uiso 1 1 calc R . . H23B H 0.7187 0.4238 0.3346 0.150 Uiso 1 1 calc R . . H23C H 0.6967 0.4717 0.3712 0.150 Uiso 1 1 calc R . . C24 C 0.8004(2) 0.37231(18) 0.42052(13) 0.0625(11) Uani 1 1 d . . . H24A H 0.8064 0.3418 0.4429 0.094 Uiso 1 1 calc R . . H24B H 0.8153 0.4113 0.4326 0.094 Uiso 1 1 calc R . . H24C H 0.8379 0.3630 0.3963 0.094 Uiso 1 1 calc R . . C25 C 0.4733(2) 0.14400(18) 0.32820(14) 0.0665(12) Uani 1 1 d . . . H25A H 0.5144 0.1113 0.3244 0.080 Uiso 1 1 calc R . . H25B H 0.5045 0.1807 0.3358 0.080 Uiso 1 1 calc R . . C26 C 0.4262(3) 0.15326(17) 0.28767(14) 0.0651(11) Uani 1 1 d . . . H26A H 0.3818 0.1835 0.2922 0.078 Uiso 1 1 calc R . . H26B H 0.4647 0.1679 0.2648 0.078 Uiso 1 1 calc R . . C27 C 0.3410(3) 0.10450(19) 0.23604(12) 0.0717(12) Uani 1 1 d . . . H27A H 0.3784 0.1156 0.2118 0.086 Uiso 1 1 calc R . . H27B H 0.2988 0.1365 0.2398 0.086 Uiso 1 1 calc R . . C28 C 0.2981(3) 0.0476(2) 0.22615(12) 0.0731(13) Uani 1 1 d . . . H28A H 0.2716 0.0499 0.1972 0.088 Uiso 1 1 calc R . . H28B H 0.3396 0.0148 0.2258 0.088 Uiso 1 1 calc R . . C29 C 0.1906(3) -0.0175(2) 0.25086(14) 0.0812(14) Uani 1 1 d . . . H29A H 0.2293 -0.0519 0.2533 0.097 Uiso 1 1 calc R . . H29B H 0.1664 -0.0175 0.2214 0.097 Uiso 1 1 calc R . . C30 C 0.1215(3) -0.0229(2) 0.28376(14) 0.0813(14) Uani 1 1 d . . . H30A H 0.0861 0.0134 0.2832 0.098 Uiso 1 1 calc R . . H30B H 0.0855 -0.0575 0.2768 0.098 Uiso 1 1 calc R . . C31 C 0.0953(3) -0.0341(2) 0.35857(15) 0.0743(13) Uani 1 1 d . . . H31A H 0.0560 -0.0671 0.3523 0.089 Uiso 1 1 calc R . . H31B H 0.0626 0.0034 0.3600 0.089 Uiso 1 1 calc R . . C32 C 0.1386(3) -0.0448(2) 0.40059(14) 0.0756(13) Uani 1 1 d . . . H32A H 0.0965 -0.0515 0.4237 0.091 Uiso 1 1 calc R . . H32B H 0.1746 -0.0807 0.3985 0.091 Uiso 1 1 calc R . . C33 C 0.2311(3) -0.0006(2) 0.45108(13) 0.0780(13) Uani 1 1 d . . . H33A H 0.2698 -0.0351 0.4499 0.094 Uiso 1 1 calc R . . H33B H 0.1896 -0.0079 0.4744 0.094 Uiso 1 1 calc R . . C34 C 0.2794(3) 0.0545(2) 0.46055(13) 0.0766(13) Uani 1 1 d . . . H34A H 0.2409 0.0892 0.4608 0.092 Uiso 1 1 calc R . . H34B H 0.3059 0.0514 0.4894 0.092 Uiso 1 1 calc R . . C35 C 0.3928(3) 0.1142(2) 0.43642(14) 0.0759(13) Uani 1 1 d . . . H35A H 0.4206 0.1110 0.4650 0.091 Uiso 1 1 calc R . . H35B H 0.3573 0.1504 0.4364 0.091 Uiso 1 1 calc R . . C36 C 0.4572(3) 0.1183(2) 0.40163(14) 0.0738(13) Uani 1 1 d . . . H36A H 0.4971 0.1510 0.4080 0.089 Uiso 1 1 calc R . . H36B H 0.4893 0.0806 0.3998 0.089 Uiso 1 1 calc R . . C37 C 0.1218(3) 0.1516(2) 0.30777(15) 0.0942(17) Uani 1 1 d . . . H37A H 0.0681 0.1298 0.3041 0.113 Uiso 1 1 calc R A 3 H37B H 0.1543 0.1473 0.2806 0.113 Uiso 1 1 calc R A 3 C38 C 0.1037(3) 0.2140(2) 0.31478(18) 0.0930(16) Uani 1 1 d . . . H38A H 0.0429 0.2220 0.3110 0.112 Uiso 1 1 calc R . . H38B H 0.1356 0.2390 0.2941 0.112 Uiso 1 1 calc R . . C39 C 0.1304(3) 0.2268(2) 0.36041(17) 0.0871(15) Uani 1 1 d . . . H39A H 0.1637 0.2640 0.3620 0.105 Uiso 1 1 calc R B . H39B H 0.0811 0.2304 0.3797 0.105 Uiso 1 1 calc R . . C40 C 0.1821(4) 0.1749(2) 0.37207(15) 0.1007(19) Uani 1 1 d . B . H40A H 0.2394 0.1878 0.3805 0.121 Uiso 1 1 d R . . H40B H 0.1566 0.1535 0.3968 0.121 Uiso 1 1 d R . . C41' C 0.4873(8) -0.0318(5) 0.3300(4) 0.080(3) Uiso 0.40 1 d P B 1 H41A H 0.5041 -0.0045 0.3064 0.096 Uiso 0.40 1 d PR B 1 H41B H 0.5007 -0.0130 0.3581 0.096 Uiso 0.40 1 d PR B 1 C41 C 0.4650(5) -0.0455(3) 0.3007(3) 0.071(2) Uiso 0.60 1 d P B 2 H41C H 0.4864 -0.0043 0.2973 0.085 Uiso 0.60 1 calc PR B 2 H41D H 0.4537 -0.0627 0.2718 0.085 Uiso 0.60 1 calc PR B 2 C42 C 0.5258(3) -0.0838(2) 0.3262(2) 0.1032(19) Uani 1 1 d . B 2 H42A H 0.5718 -0.0991 0.3078 0.124 Uiso 1 1 calc R B 2 H42B H 0.5501 -0.0616 0.3509 0.124 Uiso 1 1 calc R B 2 C43 C 0.4697(3) -0.1324(2) 0.34110(16) 0.0815(14) Uani 1 1 d . . . H43A H 0.4866 -0.1468 0.3701 0.098 Uiso 1 1 calc R B 2 H43B H 0.4708 -0.1663 0.3206 0.098 Uiso 1 1 calc R B 2 C44 C 0.3843(3) -0.1045(2) 0.34250(17) 0.0831(14) Uani 1 1 d . B . H44A H 0.3446 -0.1273 0.3242 0.100 Uiso 1 1 calc R . . H44B H 0.3627 -0.1042 0.3725 0.100 Uiso 1 1 calc R . . N1 N 0.82295(18) 0.25582(13) 0.34822(9) 0.0469(7) Uani 1 1 d . . . N2 N 0.67986(17) 0.19130(13) 0.33956(9) 0.0450(7) Uani 1 1 d . . . N3 N 0.76934(15) 0.19034(11) 0.42695(8) 0.0345(6) Uani 1 1 d . . . N4 N 0.65867(16) 0.30480(11) 0.38383(8) 0.0363(6) Uani 1 1 d . . . O1 O 0.87322(18) 0.26373(15) 0.32072(9) 0.0832(10) Uani 1 1 d . . . O2 O 0.66652(17) 0.16871(13) 0.30539(8) 0.0700(8) Uani 1 1 d . . . O3 O 0.41548(15) 0.12940(11) 0.36188(9) 0.0602(7) Uani 1 1 d . . . O4 O 0.38906(16) 0.09807(11) 0.27454(8) 0.0560(7) Uani 1 1 d . . . O5 O 0.23532(17) 0.03610(12) 0.25804(8) 0.0624(7) Uani 1 1 d . . . O6 O 0.15742(16) -0.03013(12) 0.32529(9) 0.0642(7) Uani 1 1 d . . . O7 O 0.18870(16) 0.00567(12) 0.41077(8) 0.0614(7) Uani 1 1 d . . . O8 O 0.34183(17) 0.06262(12) 0.42871(8) 0.0632(7) Uani 1 1 d . . . O9 O 0.1652(4) 0.1266(3) 0.34020(19) 0.0696(16) Uiso 0.50 1 d P B 3 O9' O 0.2043(4) 0.1476(3) 0.33260(18) 0.0616(15) Uiso 0.50 1 d P B 4 O10 O 0.3923(2) -0.04721(15) 0.32730(12) 0.1064(10) Uani 1 1 d . . . Si1 Si 0.87318(6) 0.17226(4) 0.43498(3) 0.0434(2) Uani 1 1 d . . . Si2 Si 0.69015(7) 0.37393(4) 0.40119(3) 0.0482(3) Uani 1 1 d . . . Fe1 Fe 0.73411(3) 0.23511(2) 0.374723(13) 0.03514(14) Uani 1 1 d . . . K1 K 0.29129(4) 0.04665(3) 0.34264(2) 0.04116(19) Uani 1 1 d . B . 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 0.048(2) 0.074(3) 0.055(2) 0.009(2) -0.0102(18) -0.020(2) C2 0.044(2) 0.075(3) 0.073(3) -0.002(2) 0.011(2) 0.003(2) C3 0.056(2) 0.077(3) 0.064(3) 0.026(2) -0.009(2) -0.007(2) C4 0.0334(17) 0.0342(18) 0.0347(17) 0.0026(14) -0.0006(14) 0.0011(14) C5 0.0330(17) 0.0381(19) 0.0400(18) -0.0012(15) 0.0032(14) 0.0000(15) C6 0.064(2) 0.042(2) 0.060(2) -0.0093(18) 0.014(2) -0.0093(18) C7 0.0376(19) 0.041(2) 0.053(2) 0.0076(17) 0.0006(16) -0.0054(16) C8 0.0352(19) 0.058(2) 0.045(2) 0.0114(17) 0.0077(16) 0.0023(17) C9 0.059(3) 0.085(3) 0.065(3) 0.023(2) 0.017(2) -0.014(2) C10 0.053(2) 0.051(2) 0.0364(19) 0.0033(16) 0.0116(16) 0.0083(18) C11 0.048(2) 0.0391(19) 0.0371(18) 0.0018(15) 0.0049(16) 0.0004(16) C12 0.095(3) 0.052(2) 0.042(2) -0.0118(18) 0.013(2) -0.009(2) C13 0.0408(19) 0.0274(17) 0.0438(19) -0.0056(14) -0.0021(15) -0.0047(15) C14 0.045(2) 0.038(2) 0.054(2) -0.0059(16) 0.0089(17) -0.0042(16) C15 0.065(3) 0.066(3) 0.059(3) -0.003(2) 0.022(2) -0.012(2) C16 0.034(2) 0.047(2) 0.089(3) -0.009(2) 0.012(2) -0.0023(17) C17 0.044(2) 0.041(2) 0.087(3) -0.008(2) -0.016(2) 0.0030(18) C18 0.050(3) 0.080(3) 0.129(4) -0.003(3) -0.029(3) 0.005(2) C19 0.050(2) 0.045(2) 0.057(2) -0.0024(17) -0.0154(19) 0.0012(17) C20 0.046(2) 0.0359(19) 0.045(2) -0.0026(15) -0.0059(16) -0.0028(16) C21 0.062(2) 0.068(3) 0.0375(19) 0.0048(18) 0.0022(18) -0.006(2) C22 0.073(3) 0.065(3) 0.096(3) -0.033(3) -0.007(3) 0.000(2) C23 0.158(5) 0.052(3) 0.090(3) 0.020(3) -0.053(3) -0.039(3) C24 0.060(3) 0.060(3) 0.068(3) -0.007(2) -0.006(2) -0.018(2) C25 0.040(2) 0.058(3) 0.101(3) -0.008(2) 0.010(2) -0.0139(19) C26 0.067(3) 0.048(2) 0.081(3) 0.006(2) 0.017(2) -0.014(2) C27 0.095(3) 0.073(3) 0.047(2) 0.008(2) 0.009(2) -0.009(3) C28 0.100(3) 0.086(3) 0.034(2) -0.009(2) 0.001(2) 0.003(3) C29 0.096(4) 0.089(3) 0.058(3) -0.029(3) -0.013(3) -0.021(3) C30 0.071(3) 0.095(4) 0.078(3) -0.017(3) -0.017(3) -0.026(3) C31 0.053(3) 0.075(3) 0.094(3) -0.005(3) 0.010(3) -0.024(2) C32 0.075(3) 0.077(3) 0.075(3) 0.010(2) 0.019(3) -0.023(3) C33 0.100(4) 0.087(3) 0.047(2) 0.022(2) 0.003(2) -0.006(3) C34 0.100(4) 0.094(4) 0.037(2) 0.002(2) -0.005(2) -0.004(3) C35 0.077(3) 0.086(3) 0.065(3) -0.014(2) -0.031(3) -0.007(3) C36 0.056(3) 0.078(3) 0.087(3) -0.011(3) -0.029(3) -0.012(2) C37 0.107(4) 0.106(4) 0.069(3) -0.006(3) -0.014(3) 0.050(3) C38 0.089(4) 0.083(4) 0.107(4) 0.026(3) -0.008(3) 0.018(3) C39 0.100(4) 0.073(3) 0.089(4) 0.003(3) 0.024(3) 0.012(3) C40 0.139(5) 0.096(4) 0.067(3) -0.014(3) -0.027(3) 0.054(4) C42 0.068(3) 0.087(4) 0.155(5) 0.048(4) 0.029(3) 0.003(3) C43 0.080(3) 0.064(3) 0.100(4) 0.009(3) 0.018(3) 0.006(3) C44 0.072(3) 0.076(3) 0.102(4) 0.022(3) -0.001(3) -0.009(3) N1 0.0409(17) 0.0576(19) 0.0422(17) 0.0053(14) 0.0035(14) -0.0065(14) N2 0.0409(16) 0.0507(18) 0.0434(17) -0.0080(14) -0.0006(13) -0.0024(14) N3 0.0346(14) 0.0368(15) 0.0319(14) 0.0025(11) 0.0051(11) -0.0072(12) N4 0.0363(15) 0.0395(16) 0.0331(14) -0.0023(12) -0.0018(11) -0.0084(12) O1 0.0594(18) 0.122(3) 0.0681(19) 0.0237(18) 0.0282(16) -0.0120(17) O2 0.0676(18) 0.093(2) 0.0500(16) -0.0320(15) 0.0017(14) -0.0138(16) O3 0.0444(15) 0.0655(18) 0.0707(17) 0.0018(14) -0.0101(13) -0.0135(13) O4 0.0634(17) 0.0490(16) 0.0555(16) 0.0050(12) 0.0071(13) -0.0027(13) O5 0.0760(18) 0.0675(18) 0.0439(15) -0.0143(13) -0.0035(14) -0.0064(15) O6 0.0571(17) 0.0717(19) 0.0637(17) -0.0112(14) -0.0028(14) -0.0200(14) O7 0.0662(17) 0.0655(18) 0.0525(16) 0.0093(13) 0.0066(14) -0.0134(14) O8 0.0729(18) 0.0707(19) 0.0459(15) -0.0002(13) -0.0111(14) -0.0041(15) O10 0.097(3) 0.084(2) 0.139 0.033(2) 0.051(2) 0.031(2) Si1 0.0383(5) 0.0519(6) 0.0401(5) 0.0069(4) -0.0013(4) -0.0085(4) Si2 0.0576(6) 0.0383(6) 0.0486(6) -0.0012(5) -0.0113(5) -0.0105(5) Fe1 0.0340(3) 0.0410(3) 0.0305(2) -0.0004(2) 0.0017(2) -0.0069(2) K1 0.0410(4) 0.0426(4) 0.0399(4) -0.0011(3) -0.0007(3) -0.0012(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 Si1 1.879(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 Si1 1.883(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 Si1 1.876(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.407(4) . ? C4 C11 1.419(4) . ? C4 N3 1.423(4) . ? C5 C7 1.395(4) . ? C5 C6 1.512(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.395(5) . ? C7 H7 0.9500 . ? C8 C10 1.382(5) . ? C8 C9 1.517(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.392(4) . ? C10 H10 0.9500 . ? C11 C12 1.503(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.406(4) . ? C13 C20 1.419(4) . ? C13 N4 1.430(4) . ? C14 C16 1.404(5) . ? C14 C15 1.513(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.393(5) . ? C16 H16 0.9500 . ? C17 C19 1.370(5) . ? C17 C18 1.529(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.397(5) . ? C19 H19 0.9500 . ? C20 C21 1.512(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 Si2 1.887(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 Si2 1.873(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 Si2 1.852(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 O3 1.427(4) . ? C25 C26 1.474(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O4 1.432(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O4 1.422(5) . ? C27 C28 1.480(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O5 1.426(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O5 1.415(5) . ? C29 C30 1.502(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O6 1.415(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 O6 1.429(5) . ? C31 C32 1.490(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O7 1.420(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O7 1.424(5) . ? C33 C34 1.485(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O8 1.410(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O8 1.434(5) . ? C35 C36 1.488(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O3 1.419(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O9 1.341(7) . ? C37 C38 1.447(6) . ? C37 O9' 1.523(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.501(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.473(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 O9' 1.410(7) . ? C40 O9 1.489(7) . ? C40 K1 3.483(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41' O10 1.551(12) . ? C41' H41A 0.9900 . ? C41' H41B 0.9900 . ? C41 O10 1.420(7) . ? C41 C42 1.515(8) . ? C41 H41A 1.1258 . ? C41 H41C 0.9900 . ? C41 H41D 0.9900 . ? C42 C43 1.483(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.495(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O10 1.376(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? N1 O1 1.180(3) . ? N1 Fe1 1.698(3) . ? N2 O2 1.191(3) . ? N2 Fe1 1.701(3) . ? N3 Si1 1.718(3) . ? N3 Fe1 1.983(2) . ? N4 Si2 1.717(3) . ? N4 Fe1 1.992(3) . ? O3 K1 2.776(2) . ? O4 K1 2.861(2) . ? O5 K1 2.773(2) . ? O6 K1 2.791(3) . ? O7 K1 2.819(2) . ? O8 K1 2.803(2) . ? O9 K1 2.692(6) . ? O9' K1 2.673(5) . ? O10 K1 2.692(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C11 117.7(3) . . ? C5 C4 N3 122.4(3) . . ? C11 C4 N3 119.9(3) . . ? C7 C5 C4 120.3(3) . . ? C7 C5 C6 118.5(3) . . ? C4 C5 C6 121.2(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C5 122.4(3) . . ? C8 C7 H7 118.8 . . ? C5 C7 H7 118.8 . . ? C10 C8 C7 116.8(3) . . ? C10 C8 C9 122.2(3) . . ? C7 C8 C9 120.9(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 C11 123.0(3) . . ? C8 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C10 C11 C4 119.8(3) . . ? C10 C11 C12 120.3(3) . . ? C4 C11 C12 119.9(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C20 118.0(3) . . ? C14 C13 N4 120.7(3) . . ? C20 C13 N4 121.3(3) . . ? C16 C14 C13 119.6(3) . . ? C16 C14 C15 120.1(3) . . ? C13 C14 C15 120.2(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C14 122.4(3) . . ? C17 C16 H16 118.8 . . ? C14 C16 H16 118.8 . . ? C19 C17 C16 117.2(3) . . ? C19 C17 C18 121.7(4) . . ? C16 C17 C18 121.1(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 C20 122.9(3) . . ? C17 C19 H19 118.5 . . ? C20 C19 H19 118.5 . . ? C19 C20 C13 119.7(3) . . ? C19 C20 C21 118.3(3) . . ? C13 C20 C21 122.0(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 C25 C26 109.0(3) . . ? O3 C25 H25A 109.9 . . ? C26 C25 H25A 109.9 . . ? O3 C25 H25B 109.9 . . ? C26 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? O4 C26 C25 109.2(3) . . ? O4 C26 H26A 109.8 . . ? C25 C26 H26A 109.8 . . ? O4 C26 H26B 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? O4 C27 C28 109.5(3) . . ? O4 C27 H27A 109.8 . . ? C28 C27 H27A 109.8 . . ? O4 C27 H27B 109.8 . . ? C28 C27 H27B 109.8 . . ? H27A C27 H27B 108.2 . . ? O5 C28 C27 109.6(3) . . ? O5 C28 H28A 109.7 . . ? C27 C28 H28A 109.7 . . ? O5 C28 H28B 109.7 . . ? C27 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? O5 C29 C30 109.2(3) . . ? O5 C29 H29A 109.8 . . ? C30 C29 H29A 109.8 . . ? O5 C29 H29B 109.8 . . ? C30 C29 H29B 109.8 . . ? H29A C29 H29B 108.3 . . ? O6 C30 C29 109.2(4) . . ? O6 C30 H30A 109.8 . . ? C29 C30 H30A 109.8 . . ? O6 C30 H30B 109.8 . . ? C29 C30 H30B 109.8 . . ? H30A C30 H30B 108.3 . . ? O6 C31 C32 108.6(3) . . ? O6 C31 H31A 110.0 . . ? C32 C31 H31A 110.0 . . ? O6 C31 H31B 110.0 . . ? C32 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? O7 C32 C31 108.9(3) . . ? O7 C32 H32A 109.9 . . ? C31 C32 H32A 109.9 . . ? O7 C32 H32B 109.9 . . ? C31 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? O7 C33 C34 109.6(3) . . ? O7 C33 H33A 109.8 . . ? C34 C33 H33A 109.8 . . ? O7 C33 H33B 109.8 . . ? C34 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? O8 C34 C33 109.5(4) . . ? O8 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? O8 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? O8 C35 C36 108.6(3) . . ? O8 C35 H35A 110.0 . . ? C36 C35 H35A 110.0 . . ? O8 C35 H35B 110.0 . . ? C36 C35 H35B 110.0 . . ? H35A C35 H35B 108.4 . . ? O3 C36 C35 108.4(3) . . ? O3 C36 H36A 110.0 . . ? C35 C36 H36A 110.0 . . ? O3 C36 H36B 110.0 . . ? C35 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? O9 C37 C38 113.3(5) . . ? O9 C37 O9' 32.2(3) . . ? C38 C37 O9' 98.8(5) . . ? O9 C37 H37A 108.9 . . ? C38 C37 H37A 108.9 . . ? O9' C37 H37A 140.5 . . ? O9 C37 H37B 108.9 . . ? C38 C37 H37B 108.9 . . ? O9' C37 H37B 88.4 . . ? H37A C37 H37B 107.7 . . ? C37 C38 C39 105.7(4) . . ? C37 C38 H38A 110.6 . . ? C39 C38 H38A 110.6 . . ? C37 C38 H38B 110.6 . . ? C39 C38 H38B 110.6 . . ? H38A C38 H38B 108.7 . . ? C40 C39 C38 103.6(4) . . ? C40 C39 H39A 111.0 . . ? C38 C39 H39A 111.0 . . ? C40 C39 H39B 111.0 . . ? C38 C39 H39B 111.0 . . ? H39A C39 H39B 109.0 . . ? O9' C40 C39 105.8(4) . . ? O9' C40 O9 32.5(3) . . ? C39 C40 O9 108.3(4) . . ? O9' C40 K1 44.8(3) . . ? C39 C40 K1 150.4(3) . . ? O9 C40 K1 46.8(3) . . ? O9' C40 H40A 97.1 . . ? C39 C40 H40A 110.2 . . ? O9 C40 H40A 123.5 . . ? K1 C40 H40A 81.5 . . ? O9' C40 H40B 124.1 . . ? C39 C40 H40B 110.1 . . ? O9 C40 H40B 94.9 . . ? K1 C40 H40B 90.3 . . ? H40A C40 H40B 108.4 . . ? O10 C41' H41A 111.3 . . ? O10 C41' H41B 110.6 . . ? H41A C41' H41B 108.9 . . ? O10 C41 C42 101.6(5) . . ? O10 C41 H41A 112.4 . . ? C42 C41 H41A 91.7 . . ? O10 C41 H41C 111.5 . . ? C42 C41 H41C 111.5 . . ? H41A C41 H41C 20.5 . . ? O10 C41 H41D 111.5 . . ? C42 C41 H41D 111.5 . . ? H41A C41 H41D 124.1 . . ? H41C C41 H41D 109.3 . . ? C43 C42 C41 101.3(4) . . ? 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 . . ? C42 C43 C44 104.2(4) . . ? C42 C43 H43A 110.9 . . ? C44 C43 H43A 110.9 . . ? C42 C43 H43B 110.9 . . ? C44 C43 H43B 110.9 . . ? H43A C43 H43B 108.9 . . ? O10 C44 C43 107.4(4) . . ? O10 C44 H44A 110.2 . . ? C43 C44 H44A 110.2 . . ? O10 C44 H44B 110.2 . . ? C43 C44 H44B 110.2 . . ? H44A C44 H44B 108.5 . . ? O1 N1 Fe1 162.2(3) . . ? O2 N2 Fe1 154.6(3) . . ? C4 N3 Si1 118.1(2) . . ? C4 N3 Fe1 120.06(19) . . ? Si1 N3 Fe1 120.60(13) . . ? C13 N4 Si2 115.3(2) . . ? C13 N4 Fe1 116.82(19) . . ? Si2 N4 Fe1 125.39(14) . . ? C36 O3 C25 111.8(3) . . ? C36 O3 K1 113.6(2) . . ? C25 O3 K1 117.1(2) . . ? C27 O4 C26 111.8(3) . . ? C27 O4 K1 111.4(2) . . ? C26 O4 K1 111.4(2) . . ? C29 O5 C28 113.4(3) . . ? C29 O5 K1 112.4(2) . . ? C28 O5 K1 114.4(2) . . ? C30 O6 C31 112.5(3) . . ? C30 O6 K1 114.2(2) . . ? C31 O6 K1 115.3(2) . . ? C32 O7 C33 112.4(3) . . ? C32 O7 K1 114.8(2) . . ? C33 O7 K1 114.4(2) . . ? C34 O8 C35 112.7(3) . . ? C34 O8 K1 116.4(2) . . ? C35 O8 K1 115.0(2) . . ? C37 O9 C40 106.5(5) . . ? C37 O9 K1 133.1(4) . . ? C40 O9 K1 109.4(4) . . ? C40 O9' C37 101.3(4) . . ? C40 O9' K1 113.4(3) . . ? C37 O9' K1 123.7(4) . . ? C44 O10 C41 107.4(4) . . ? C44 O10 C41' 106.3(5) . . ? C41 O10 C41' 39.9(5) . . ? C44 O10 K1 128.1(3) . . ? C41 O10 K1 124.5(4) . . ? C41' O10 K1 113.4(5) . . ? N3 Si1 C3 110.29(15) . . ? N3 Si1 C1 112.31(16) . . ? C3 Si1 C1 108.05(18) . . ? N3 Si1 C2 113.60(15) . . ? C3 Si1 C2 106.11(19) . . ? C1 Si1 C2 106.12(18) . . ? N4 Si2 C24 111.04(16) . . ? N4 Si2 C23 113.60(16) . . ? C24 Si2 C23 108.2(2) . . ? N4 Si2 C22 114.00(17) . . ? C24 Si2 C22 106.99(19) . . ? C23 Si2 C22 102.4(2) . . ? N1 Fe1 N2 105.76(13) . . ? N1 Fe1 N3 107.28(12) . . ? N2 Fe1 N3 111.74(12) . . ? N1 Fe1 N4 110.73(12) . . ? N2 Fe1 N4 103.86(12) . . ? N3 Fe1 N4 116.96(10) . . ? O9' K1 O10 162.18(14) . . ? O9' K1 O9 17.44(14) . . ? O10 K1 O9 164.04(16) . . ? O9' K1 O5 78.28(13) . . ? O10 K1 O5 87.61(10) . . ? O9 K1 O5 77.98(14) . . ? O9' K1 O3 79.94(14) . . ? O10 K1 O3 97.92(10) . . ? O9 K1 O3 95.10(15) . . ? O5 K1 O3 119.18(8) . . ? O9' K1 O6 96.14(14) . . ? O10 K1 O6 86.40(10) . . ? O9 K1 O6 80.74(15) . . ? O5 K1 O6 61.39(8) . . ? O3 K1 O6 175.65(8) . . ? O9' K1 O8 98.63(13) . . ? O10 K1 O8 95.54(10) . . ? O9 K1 O8 98.89(14) . . ? O5 K1 O8 176.85(8) . . ? O3 K1 O8 60.46(8) . . ? O6 K1 O8 118.69(8) . . ? O9' K1 O7 93.69(14) . . ? O10 K1 O7 102.78(9) . . ? O9 K1 O7 78.93(15) . . ? O5 K1 O7 119.44(8) . . ? O3 K1 O7 118.03(8) . . ? O6 K1 O7 60.05(8) . . ? O8 K1 O7 59.87(8) . . ? O9' K1 O4 81.57(14) . . ? O10 K1 O4 82.08(9) . . ? O9 K1 O4 96.58(14) . . ? O5 K1 O4 60.95(8) . . ? O3 K1 O4 60.07(8) . . ? O6 K1 O4 121.47(8) . . ? O8 K1 O4 119.44(8) . . ? O7 K1 O4 175.10(8) . . ? O9' K1 C40 21.82(13) . . ? O10 K1 C40 172.14(13) . . ? O9 K1 C40 23.78(15) . . ? O5 K1 C40 99.04(9) . . ? O3 K1 C40 75.22(12) . . ? O6 K1 C40 100.43(12) . . ? O8 K1 C40 77.82(9) . . ? O7 K1 C40 77.67(11) . . ? O4 K1 C40 97.43(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.744 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.053 ***************************************************** data_a12109 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 Fe N4 O2 Si2' _chemical_formula_sum 'C24 H40 Fe N4 O2 Si2' _chemical_formula_weight 528.63 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 orthorhombic _symmetry_space_group_name_H-M 'P n n a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 13.1256(10) _cell_length_b 11.3614(9) _cell_length_c 19.5259(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2911.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour blue(dark) _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.57 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6829 _exptl_absorpt_correction_T_max 0.7450 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14571 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2570 _reflns_number_gt 2017 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0586P)^2^+4.0190P] 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 2570 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.5225(2) 0.2305(2) 0.11415(15) 0.0312(7) Uani 1 1 d . . . C2 C 0.4472(2) 0.2367(3) 0.06310(16) 0.0360(7) Uani 1 1 d . . . C3 C 0.3448(3) 0.1787(3) 0.07156(17) 0.0461(9) Uani 1 1 d . . . H3A H 0.3417 0.1396 0.1162 0.069 Uiso 1 1 calc R . . H3B H 0.3350 0.1204 0.0352 0.069 Uiso 1 1 calc R . . H3C H 0.2911 0.2384 0.0688 0.069 Uiso 1 1 calc R . . C4 C 0.4688(3) 0.2975(3) 0.00290(17) 0.0463(9) Uani 1 1 d . . . H4 H 0.4172 0.3029 -0.0311 0.056 Uiso 1 1 calc R . . C5 C 0.5620(3) 0.3504(3) -0.00953(18) 0.0492(9) Uani 1 1 d . . . C6 C 0.5830(4) 0.4128(4) -0.0762(2) 0.0731(13) Uani 1 1 d . . . H6A H 0.5226 0.4083 -0.1056 0.110 Uiso 1 1 calc R . . H6B H 0.6408 0.3752 -0.0993 0.110 Uiso 1 1 calc R . . H6C H 0.5993 0.4955 -0.0671 0.110 Uiso 1 1 calc R . . C7 C 0.6342(3) 0.3442(3) 0.04137(19) 0.0491(9) Uani 1 1 d . . . H7 H 0.6982 0.3812 0.0341 0.059 Uiso 1 1 calc R . . C8 C 0.6176(2) 0.2861(3) 0.10308(17) 0.0394(8) Uani 1 1 d . . . C9 C 0.7009(3) 0.2785(4) 0.15562(19) 0.0533(10) Uani 1 1 d . . . H9A H 0.6764 0.2343 0.1955 0.080 Uiso 1 1 calc R . . H9B H 0.7206 0.3580 0.1699 0.080 Uiso 1 1 calc R . . H9C H 0.7600 0.2382 0.1358 0.080 Uiso 1 1 calc R . . C10 C 0.5907(3) -0.0272(3) 0.0982(2) 0.0632(11) Uani 1 1 d . . . H10A H 0.6553 0.0160 0.0971 0.095 Uiso 1 1 calc R . . H10B H 0.5504 -0.0072 0.0576 0.095 Uiso 1 1 calc R . . H10C H 0.6045 -0.1120 0.0985 0.095 Uiso 1 1 calc R . . C11 C 0.5905(3) -0.0338(3) 0.25346(19) 0.0586(10) Uani 1 1 d . . . H11A H 0.5526 -0.0113 0.2947 0.088 Uiso 1 1 calc R . . H11B H 0.6574 0.0044 0.2539 0.088 Uiso 1 1 calc R . . H11C H 0.5993 -0.1194 0.2526 0.088 Uiso 1 1 calc R . . C12 C 0.3960(3) -0.0693(3) 0.1780(2) 0.0669(12) Uani 1 1 d . . . H12A H 0.3574 -0.0477 0.2190 0.100 Uiso 1 1 calc R . . H12B H 0.4100 -0.1540 0.1786 0.100 Uiso 1 1 calc R . . H12C H 0.3561 -0.0497 0.1371 0.100 Uiso 1 1 calc R . . N1 N 0.37445(19) 0.1509(2) 0.29073(13) 0.0346(6) Uani 1 1 d . . . N2 N 0.50736(17) 0.1678(2) 0.17675(12) 0.0290(6) Uani 1 1 d . . . O1 O 0.3051(2) 0.1029(2) 0.31510(13) 0.0611(8) Uani 1 1 d . . . Si1 Si 0.51879(7) 0.01353(8) 0.17640(5) 0.0363(3) Uani 1 1 d . . . Fe1 Fe 0.44519(4) 0.2500 0.2500 0.0247(2) Uani 1 2 d S . . 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 0.0354(16) 0.0304(15) 0.0279(16) -0.0078(13) 0.0060(13) 0.0053(12) C2 0.0417(17) 0.0364(18) 0.0300(17) -0.0085(14) 0.0006(14) 0.0054(14) C3 0.0460(19) 0.055(2) 0.0370(18) -0.0040(17) -0.0115(16) 0.0040(17) C4 0.064(2) 0.0432(19) 0.0319(18) -0.0063(16) -0.0004(17) 0.0133(18) C5 0.073(3) 0.0371(19) 0.037(2) -0.0029(16) 0.0207(19) 0.0094(18) C6 0.110(4) 0.062(3) 0.048(2) 0.010(2) 0.030(2) 0.014(3) C7 0.052(2) 0.0431(19) 0.052(2) -0.0091(17) 0.0237(19) -0.0016(16) C8 0.0401(18) 0.0391(18) 0.0390(19) -0.0112(15) 0.0133(15) 0.0026(14) C9 0.0347(18) 0.071(3) 0.054(2) -0.013(2) 0.0050(17) -0.0079(17) C10 0.078(3) 0.054(2) 0.058(2) -0.020(2) 0.003(2) 0.025(2) C11 0.071(2) 0.046(2) 0.059(2) 0.0000(18) -0.018(2) 0.016(2) C12 0.057(2) 0.036(2) 0.108(4) -0.010(2) -0.012(2) -0.0045(18) N1 0.0427(15) 0.0309(14) 0.0302(14) -0.0025(11) -0.0025(12) -0.0093(12) N2 0.0281(12) 0.0297(13) 0.0291(13) -0.0078(11) 0.0008(10) 0.0031(10) O1 0.0693(17) 0.0596(16) 0.0544(16) -0.0009(13) 0.0159(14) -0.0359(14) Si1 0.0363(5) 0.0308(5) 0.0418(5) -0.0080(4) -0.0073(4) 0.0081(4) Fe1 0.0252(3) 0.0249(3) 0.0241(3) -0.0026(2) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.405(4) . ? C1 C8 1.415(4) . ? C1 N2 1.429(4) . ? C2 C4 1.392(5) . ? C2 C3 1.506(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C7 1.375(5) . ? C5 C6 1.508(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.391(5) . ? C7 H7 0.9500 . ? C8 C9 1.501(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Si1 1.855(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.854(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si1 1.867(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N1 O1 1.163(3) . ? N1 Fe1 1.662(3) . ? N2 Si1 1.759(3) . ? N2 Fe1 1.893(2) . ? Fe1 N1 1.662(3) 4 ? Fe1 N2 1.893(2) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C8 119.3(3) . . ? C2 C1 N2 122.3(3) . . ? C8 C1 N2 118.4(3) . . ? C4 C2 C1 118.8(3) . . ? C4 C2 C3 119.4(3) . . ? C1 C2 C3 121.8(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C2 122.9(3) . . ? C5 C4 H4 118.6 . . ? C2 C4 H4 118.6 . . ? C7 C5 C4 117.4(3) . . ? C7 C5 C6 121.5(4) . . ? C4 C5 C6 121.1(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 C8 122.9(3) . . ? C5 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C7 C8 C1 118.8(3) . . ? C7 C8 C9 120.4(3) . . ? C1 C8 C9 120.8(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 N1 Fe1 161.9(3) . . ? C1 N2 Si1 118.78(18) . . ? C1 N2 Fe1 117.43(18) . . ? Si1 N2 Fe1 122.08(14) . . ? N2 Si1 C11 109.20(15) . . ? N2 Si1 C10 107.18(16) . . ? C11 Si1 C10 109.73(19) . . ? N2 Si1 C12 115.38(15) . . ? C11 Si1 C12 106.2(2) . . ? C10 Si1 C12 109.1(2) . . ? N1 Fe1 N1 112.07(18) . 4 ? N1 Fe1 N2 102.32(11) . 4 ? N1 Fe1 N2 105.56(11) 4 4 ? N1 Fe1 N2 105.56(11) . . ? N1 Fe1 N2 102.32(11) 4 . ? N2 Fe1 N2 128.93(14) 4 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.408 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.064