# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'publ.cif' #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. Michael Bolte Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; _publ_contact_author_phone '49 69 798 29136' _publ_contact_author_fax '49 69 798 29239' _publ_contact_author_email bolte@chemie.uni-frankfurt.de _publ_requested_coeditor_name ' ' _publ_contact_letter ; Please consider this CIF submission as supplementary material for a manuscript intended to publication in Z. Anorg. Allg. Chemie. ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Reductive Degradatio of Cyclopentadienidoirondicarbonyl complexes ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' F.Dornhaus ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; I.Sanger ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; M.Wagner ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; T.Kuckmann ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; H.-W.Lerner ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; M.Bolte ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; ; _publ_section_references ; Allen, F. H. (2002). Acta Cryst., B58, 380-388. Blessing, R.H. (1995). Acta Cryst. A51, 33-38. Bruno, I.J., Cole, J.C., Edgington, P.R., Kessler, M.K., Macrae, C.F., McCabe, P., Pearson J. & Taylor, R. (2002). Acta Crystallogr., B58, 389-397. Burla, M.C., Camalli, M., Carrozzini, B., Cascarano, G.L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. Sheldrick, G.M. (1990). Acta Cryst. A46, 467 - 473. Sheldrick, G.M. (1997). SHELXL-97. Program for the refinement of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. Spek, A.L. (2003). J. Appl. Cryst. A36, 7-13. Stoe & Cie (2001). X-Area. Area-Detector Control and Integration Software. Stoe & Cie, Darmstadt, Germany. ; _publ_section_figure_captions ; Fig. 1. ; _publ_contact_author_name 'Dr. Michael Bolte' data_wa575 _database_code_depnum_ccdc_archive 'CCDC 832031' #TrackingRef 'publ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H18 Fe O2 Si' _chemical_formula_weight 374.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _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 15.2447(12) _cell_length_b 7.7411(7) _cell_length_c 45.632(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.899(6) _cell_angle_gamma 90.00 _cell_volume 5382.1(8) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16269 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.3 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8170 _exptl_absorpt_correction_T_max 0.9557 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 41050 _diffrn_reflns_av_R_equivalents 0.1304 _diffrn_reflns_av_sigmaI/netI 0.1694 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.11 _reflns_number_total 9479 _reflns_number_gt 5255 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0697P)^2^+179.8729P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0070(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9479 _refine_ls_number_parameters 650 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2237 _refine_ls_R_factor_gt 0.1613 _refine_ls_wR_factor_ref 0.3785 _refine_ls_wR_factor_gt 0.3508 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Fe1 Fe 0.51090(14) 0.2952(3) 0.55009(5) 0.0353(6) Uani 1 1 d . . . Si1 Si 0.5825(3) 0.1381(6) 0.58718(10) 0.0337(10) Uani 1 1 d . . . C1 C 0.6618(10) 0.283(2) 0.6083(4) 0.040(4) Uani 1 1 d . . . H1A H 0.7041 0.3316 0.5949 0.061 Uiso 1 1 calc R . . H1B H 0.6932 0.2150 0.6235 0.061 Uiso 1 1 calc R . . H1C H 0.6294 0.3763 0.6175 0.061 Uiso 1 1 calc R . . C2 C 0.4715(9) 0.0994(18) 0.5358(4) 0.032(4) Uani 1 1 d . . . O2 O 0.4441(7) -0.0286(19) 0.5270(3) 0.054(3) Uani 1 1 d . . . C3 C 0.6124(10) 0.298(2) 0.5332(4) 0.041(4) Uani 1 1 d . . . O3 O 0.6785(8) 0.3085(17) 0.5217(3) 0.050(3) Uani 1 1 d . . . C11 C 0.5035(9) 0.049(2) 0.6142(3) 0.032(3) Uani 1 1 d . . . C12 C 0.4961(10) 0.119(2) 0.6421(3) 0.037(4) Uani 1 1 d . . . H12 H 0.5332 0.2120 0.6481 0.045 Uiso 1 1 calc R . . C13 C 0.4345(11) 0.054(3) 0.6617(4) 0.045(4) Uani 1 1 d . . . H13 H 0.4297 0.1059 0.6804 0.054 Uiso 1 1 calc R . . C14 C 0.3824(11) -0.082(2) 0.6544(4) 0.045(4) Uani 1 1 d . . . H14 H 0.3418 -0.1248 0.6679 0.054 Uiso 1 1 calc R . . C15 C 0.3886(11) -0.160(2) 0.6260(4) 0.043(4) Uani 1 1 d . . . H15 H 0.3513 -0.2534 0.6204 0.052 Uiso 1 1 calc R . . C16 C 0.4505(10) -0.096(2) 0.6065(4) 0.042(4) Uani 1 1 d . . . H16 H 0.4569 -0.1503 0.5881 0.050 Uiso 1 1 calc R . . C21 C 0.6510(9) -0.058(2) 0.5750(4) 0.034(4) Uani 1 1 d . . . C22 C 0.6949(9) -0.148(2) 0.5978(4) 0.044(4) Uani 1 1 d . . . H22 H 0.6869 -0.1131 0.6175 0.053 Uiso 1 1 calc R . . C23 C 0.7495(10) -0.285(2) 0.5922(5) 0.059(6) Uani 1 1 d . . . H23 H 0.7785 -0.3453 0.6079 0.071 Uiso 1 1 calc R . . C24 C 0.7617(10) -0.336(3) 0.5631(5) 0.052(5) Uani 1 1 d . . . H24 H 0.7980 -0.4325 0.5592 0.062 Uiso 1 1 calc R . . C25 C 0.7205(11) -0.245(2) 0.5398(4) 0.046(4) Uani 1 1 d . . . H25 H 0.7309 -0.2753 0.5200 0.055 Uiso 1 1 calc R . . C26 C 0.6621(10) -0.105(2) 0.5466(4) 0.045(4) Uani 1 1 d . . . H26 H 0.6315 -0.0447 0.5312 0.054 Uiso 1 1 calc R . . C31 C 0.4559(11) 0.435(2) 0.5839(4) 0.046(4) Uani 1 1 d . . . H31 H 0.4616 0.4040 0.6040 0.056 Uiso 1 1 calc R . . C32 C 0.5143(13) 0.547(2) 0.5685(4) 0.051(5) Uani 1 1 d . . . H32 H 0.5655 0.6040 0.5760 0.062 Uiso 1 1 calc R . . C33 C 0.4775(12) 0.553(2) 0.5396(4) 0.045(4) Uani 1 1 d . . . H33 H 0.5017 0.6171 0.5241 0.053 Uiso 1 1 calc R . . C34 C 0.4044(9) 0.456(2) 0.5366(4) 0.038(4) Uani 1 1 d . . . H34 H 0.3691 0.4409 0.5192 0.046 Uiso 1 1 calc R . . C35 C 0.3902(11) 0.381(2) 0.5644(5) 0.053(5) Uani 1 1 d . . . H35 H 0.3432 0.3062 0.5689 0.063 Uiso 1 1 calc R . . Fe1A Fe 0.87600(13) 0.2182(3) 0.45079(5) 0.0352(6) Uani 1 1 d . . . Si1A Si 0.9366(3) 0.3667(6) 0.41214(10) 0.0359(11) Uani 1 1 d . . . C1A C 1.0066(12) 0.223(3) 0.3910(4) 0.052(5) Uani 1 1 d . . . H1A1 H 0.9731 0.1204 0.3849 0.077 Uiso 1 1 calc R . . H1A2 H 1.0576 0.1877 0.4033 0.077 Uiso 1 1 calc R . . H1A3 H 1.0266 0.2840 0.3737 0.077 Uiso 1 1 calc R . . C2A C 0.8437(10) 0.415(2) 0.4664(4) 0.037(4) Uani 1 1 d . . . O2A O 0.8199(8) 0.5432(17) 0.4756(3) 0.054(3) Uani 1 1 d . . . C3A C 0.9813(10) 0.214(2) 0.4650(4) 0.049(4) Uani 1 1 d . . . O3A O 1.0546(7) 0.2066(19) 0.4757(3) 0.058(4) Uani 1 1 d . . . C21A C 1.0081(9) 0.558(2) 0.4225(3) 0.032(3) Uani 1 1 d . . . C22A C 1.0442(10) 0.652(2) 0.3985(4) 0.046(4) Uani 1 1 d . . . H22A H 1.0302 0.6178 0.3790 0.055 Uiso 1 1 calc R . . C23A C 1.0999(11) 0.795(2) 0.4037(5) 0.051(5) Uani 1 1 d . . . H23A H 1.1225 0.8565 0.3876 0.062 Uiso 1 1 calc R . . C24A C 1.1217(10) 0.847(2) 0.4318(4) 0.047(4) Uani 1 1 d . . . H24A H 1.1593 0.9433 0.4352 0.057 Uiso 1 1 calc R . . C25A C 1.0872(11) 0.754(3) 0.4556(4) 0.052(5) Uani 1 1 d . . . H25A H 1.1035 0.7869 0.4750 0.063 Uiso 1 1 calc R . . C26A C 1.0309(10) 0.618(2) 0.4511(4) 0.041(4) Uani 1 1 d . . . H26A H 1.0064 0.5633 0.4675 0.049 Uiso 1 1 calc R . . C11A C 0.8522(9) 0.457(2) 0.3853(3) 0.036(4) Uani 1 1 d . . . C12A C 0.8343(11) 0.377(2) 0.3580(4) 0.045(4) Uani 1 1 d . . . H12A H 0.8654 0.2759 0.3527 0.054 Uiso 1 1 calc R . . C13A C 0.7703(11) 0.447(3) 0.3387(4) 0.044(4) Uani 1 1 d . . . H13A H 0.7605 0.3941 0.3201 0.053 Uiso 1 1 calc R . . C14A C 0.7211(11) 0.590(2) 0.3457(4) 0.046(5) Uani 1 1 d . . . H14A H 0.6783 0.6362 0.3322 0.055 Uiso 1 1 calc R . . C15A C 0.7357(12) 0.661(3) 0.3719(4) 0.058(5) Uani 1 1 d . . . H15A H 0.7008 0.7567 0.3772 0.069 Uiso 1 1 calc R . . C16A C 0.8007(9) 0.600(2) 0.3924(4) 0.046(4) Uani 1 1 d . . . H16A H 0.8093 0.6567 0.4107 0.055 Uiso 1 1 calc R . . C31A C 0.8091(10) 0.071(2) 0.4185(4) 0.043(4) Uani 1 1 d . . . H31A H 0.8073 0.0939 0.3981 0.052 Uiso 1 1 calc R . . C32A C 0.8698(11) -0.031(2) 0.4337(4) 0.046(4) Uani 1 1 d . . . H32A H 0.9183 -0.0881 0.4254 0.055 Uiso 1 1 calc R . . C33A C 0.8483(11) -0.037(2) 0.4632(4) 0.044(4) Uani 1 1 d . . . H33A H 0.8789 -0.1001 0.4782 0.052 Uiso 1 1 calc R . . C34A C 0.7716(12) 0.069(2) 0.4669(5) 0.055(5) Uani 1 1 d . . . H34A H 0.7416 0.0896 0.4845 0.066 Uiso 1 1 calc R . . C35A C 0.7510(11) 0.135(2) 0.4389(4) 0.045(4) Uani 1 1 d . . . H35A H 0.7041 0.2130 0.4345 0.054 Uiso 1 1 calc R . . Fe1B Fe 0.37967(16) 0.3454(3) 0.28831(6) 0.0447(7) Uani 1 1 d . . . Si1B Si 0.2386(3) 0.2273(7) 0.28549(11) 0.0462(12) Uani 1 1 d . . . C1B C 0.2226(12) 0.063(3) 0.3148(5) 0.062(6) Uani 1 1 d . . . H1B1 H 0.2373 0.1149 0.3340 0.093 Uiso 1 1 calc R . . H1B2 H 0.2609 -0.0359 0.3116 0.093 Uiso 1 1 calc R . . H1B3 H 0.1613 0.0254 0.3143 0.093 Uiso 1 1 calc R . . C2B C 0.3643(10) 0.398(3) 0.2521(4) 0.047(5) Uani 1 1 d . . . O2B O 0.3523(8) 0.441(2) 0.2277(3) 0.068(4) Uani 1 1 d . . . C3B C 0.4229(13) 0.144(3) 0.2812(5) 0.060(5) Uani 1 1 d . . . O3B O 0.4484(12) 0.003(2) 0.2785(4) 0.093(6) Uani 1 1 d . . . C11B C 0.1552(11) 0.407(2) 0.2894(4) 0.047(5) Uani 1 1 d . . . C12B C 0.0901(14) 0.393(3) 0.3098(5) 0.070(6) Uani 1 1 d . . . H12B H 0.0899 0.2950 0.3224 0.084 Uiso 1 1 calc R . . C13B C 0.0255(12) 0.517(5) 0.3124(5) 0.086(10) Uani 1 1 d . . . H13B H -0.0209 0.5010 0.3255 0.103 Uiso 1 1 calc R . . C14B C 0.0300(13) 0.670(4) 0.2949(6) 0.080(8) Uani 1 1 d . . . H14B H -0.0128 0.7583 0.2966 0.095 Uiso 1 1 calc R . . C15B C 0.0936(12) 0.686(3) 0.2766(6) 0.070(6) Uani 1 1 d . . . H15B H 0.0992 0.7901 0.2657 0.084 Uiso 1 1 calc R . . C16B C 0.1539(13) 0.551(3) 0.2730(4) 0.056(5) Uani 1 1 d . . . H16B H 0.1959 0.5621 0.2582 0.067 Uiso 1 1 calc R . . C21B C 0.2082(12) 0.117(3) 0.2501(4) 0.054(5) Uani 1 1 d . . . C22B C 0.1434(13) 0.167(2) 0.2302(5) 0.066(6) Uani 1 1 d . . . H22B H 0.1119 0.2695 0.2347 0.079 Uiso 1 1 calc R . . C23B C 0.1199(15) 0.085(3) 0.2046(4) 0.062(6) Uani 1 1 d . . . H23B H 0.0715 0.1251 0.1928 0.074 Uiso 1 1 calc R . . C24B C 0.1671(13) -0.054(3) 0.1964(4) 0.061(6) Uani 1 1 d . . . H24B H 0.1531 -0.1136 0.1787 0.073 Uiso 1 1 calc R . . C25B C 0.2365(12) -0.108(3) 0.2147(5) 0.070(7) Uani 1 1 d . . . H25B H 0.2709 -0.2038 0.2088 0.084 Uiso 1 1 calc R . . C26B C 0.2576(13) -0.029(3) 0.2411(5) 0.065(6) Uani 1 1 d . . . H26B H 0.3046 -0.0720 0.2533 0.078 Uiso 1 1 calc R . . C31B C 0.3379(12) 0.457(3) 0.3275(4) 0.055(5) Uani 1 1 d . . . H31B H 0.2821 0.4368 0.3355 0.066 Uiso 1 1 calc R . . C32B C 0.4153(13) 0.358(3) 0.3334(4) 0.060(5) Uani 1 1 d . . . H32B H 0.4205 0.2612 0.3462 0.071 Uiso 1 1 calc R . . C33B C 0.4853(11) 0.433(2) 0.3163(4) 0.046(4) Uani 1 1 d . . . H33B H 0.5443 0.3943 0.3157 0.055 Uiso 1 1 calc R . . C34B C 0.4500(13) 0.569(3) 0.3015(5) 0.060(5) Uani 1 1 d . . . H34B H 0.4819 0.6413 0.2888 0.072 Uiso 1 1 calc R . . C35B C 0.3585(13) 0.593(3) 0.3073(5) 0.062(5) Uani 1 1 d . . . H35B H 0.3200 0.6789 0.2995 0.074 Uiso 1 1 calc R . . 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 Fe1 0.0310(11) 0.0283(12) 0.0464(14) 0.0004(11) -0.0036(10) 0.0016(10) Si1 0.0267(19) 0.027(2) 0.046(3) 0.000(2) -0.0057(18) -0.0005(17) C1 0.030(8) 0.041(9) 0.050(10) -0.004(8) -0.009(7) -0.007(7) C2 0.028(7) 0.014(7) 0.055(10) -0.003(7) -0.008(7) -0.012(6) O2 0.027(6) 0.068(10) 0.066(9) -0.003(7) 0.007(6) 0.002(6) C3 0.036(9) 0.035(9) 0.052(10) 0.000(8) 0.003(8) -0.008(7) O3 0.048(7) 0.046(8) 0.057(8) -0.001(6) 0.006(6) 0.001(6) C11 0.020(7) 0.033(9) 0.042(9) 0.004(7) -0.004(6) 0.010(6) C12 0.046(9) 0.027(9) 0.038(9) 0.006(7) 0.000(7) -0.012(7) C13 0.046(9) 0.056(12) 0.032(9) 0.000(8) 0.003(7) 0.019(9) C14 0.048(10) 0.041(10) 0.047(11) 0.009(8) 0.008(8) 0.001(8) C15 0.045(9) 0.036(9) 0.049(10) 0.012(8) 0.002(8) -0.003(7) C16 0.039(9) 0.037(10) 0.049(10) 0.000(8) -0.010(8) 0.006(7) C21 0.031(7) 0.024(8) 0.048(10) -0.005(7) 0.003(7) 0.006(6) C22 0.020(7) 0.036(9) 0.076(13) -0.014(9) 0.008(7) -0.007(7) C23 0.029(8) 0.032(9) 0.114(18) 0.023(11) -0.016(10) -0.005(8) C24 0.020(7) 0.056(12) 0.081(14) -0.031(11) 0.008(8) -0.001(7) C25 0.043(9) 0.040(11) 0.055(11) 0.002(9) 0.002(8) 0.001(8) C26 0.035(8) 0.044(11) 0.057(12) 0.013(9) 0.001(8) 0.006(8) C31 0.045(10) 0.044(10) 0.051(11) 0.009(9) 0.003(8) 0.007(8) C32 0.064(12) 0.041(11) 0.049(11) -0.001(9) -0.008(9) 0.010(9) C33 0.062(11) 0.016(8) 0.055(11) 0.005(8) 0.001(9) 0.007(8) C34 0.022(7) 0.037(9) 0.054(11) 0.005(8) -0.006(7) 0.013(7) C35 0.032(9) 0.044(11) 0.082(14) 0.006(10) 0.008(9) 0.015(8) Fe1A 0.0281(11) 0.0346(13) 0.0423(13) 0.0026(11) -0.0080(9) 0.0006(10) Si1A 0.028(2) 0.037(2) 0.042(3) 0.001(2) -0.0093(18) 0.0032(18) C1A 0.053(10) 0.055(12) 0.047(11) 0.010(9) 0.009(8) 0.022(9) C2A 0.036(8) 0.026(9) 0.048(10) 0.002(8) -0.005(7) 0.001(7) O2A 0.041(7) 0.040(8) 0.080(10) -0.005(7) 0.007(6) -0.004(6) C3A 0.035(9) 0.040(10) 0.071(13) -0.003(10) -0.002(8) -0.007(8) O3A 0.034(6) 0.066(9) 0.071(9) 0.013(8) -0.020(6) -0.007(6) C21A 0.021(7) 0.030(8) 0.044(9) 0.000(7) -0.003(6) -0.010(6) C22A 0.035(8) 0.041(10) 0.061(12) 0.004(9) 0.001(8) 0.001(8) C23A 0.040(9) 0.030(9) 0.083(14) 0.005(10) -0.010(9) -0.009(8) C24A 0.036(8) 0.033(9) 0.074(13) 0.007(9) 0.001(8) -0.013(7) C25A 0.035(9) 0.060(13) 0.061(12) -0.020(10) -0.009(8) 0.007(8) C26A 0.029(8) 0.045(10) 0.049(10) 0.004(8) 0.004(7) 0.000(7) C11A 0.026(7) 0.043(10) 0.037(9) 0.012(8) 0.003(6) -0.004(7) C12A 0.045(9) 0.035(10) 0.055(11) -0.003(9) -0.006(8) -0.003(8) C13A 0.042(9) 0.057(12) 0.033(9) 0.007(8) -0.011(7) -0.012(9) C14A 0.043(9) 0.052(11) 0.041(10) 0.028(9) -0.020(8) -0.006(8) C15A 0.058(11) 0.054(13) 0.060(13) 0.017(10) -0.018(9) 0.018(9) C16A 0.023(7) 0.043(10) 0.070(12) -0.002(9) -0.011(8) 0.004(7) C31A 0.033(8) 0.047(10) 0.048(10) -0.002(8) -0.014(8) -0.011(8) C32A 0.041(9) 0.033(10) 0.063(12) -0.014(9) -0.011(8) -0.003(7) C33A 0.045(9) 0.017(8) 0.068(13) -0.006(8) -0.008(9) -0.004(7) C34A 0.049(10) 0.037(10) 0.081(15) -0.004(10) 0.019(10) -0.018(8) C35A 0.039(9) 0.027(9) 0.069(12) 0.001(9) 0.003(8) 0.001(7) Fe1B 0.0455(14) 0.0402(15) 0.0478(15) -0.0030(12) -0.0100(11) 0.0048(11) Si1B 0.055(3) 0.039(3) 0.044(3) 0.002(2) 0.000(2) -0.002(2) C1B 0.051(11) 0.061(13) 0.073(14) -0.010(11) -0.011(10) -0.017(10) C2B 0.028(8) 0.056(12) 0.057(12) -0.013(10) -0.005(8) -0.012(8) O2B 0.042(7) 0.115(13) 0.045(8) 0.001(8) -0.005(6) -0.028(8) C3B 0.065(12) 0.048(12) 0.065(13) 0.007(11) -0.022(10) 0.004(10) O3B 0.110(13) 0.072(12) 0.094(13) -0.032(10) -0.033(10) 0.054(10) C11B 0.042(9) 0.052(12) 0.048(11) 0.001(9) -0.005(8) -0.020(8) C12B 0.062(13) 0.077(17) 0.069(15) -0.014(12) -0.008(11) -0.025(12) C13B 0.028(9) 0.18(3) 0.050(13) -0.006(16) 0.004(9) 0.030(14) C14B 0.041(11) 0.10(2) 0.094(18) -0.028(16) -0.017(12) 0.045(12) C15B 0.040(10) 0.067(15) 0.103(18) -0.003(13) -0.002(11) -0.006(10) C16B 0.061(12) 0.052(12) 0.053(12) -0.004(10) -0.007(9) 0.014(10) C21B 0.051(10) 0.070(14) 0.041(10) -0.008(10) -0.005(8) -0.002(10) C22B 0.061(12) 0.031(10) 0.104(18) 0.003(11) -0.022(12) 0.003(9) C23B 0.090(15) 0.055(13) 0.039(11) 0.008(10) -0.017(10) -0.002(12) C24B 0.064(13) 0.078(16) 0.042(11) -0.017(11) 0.003(9) -0.017(12) C25B 0.039(10) 0.093(18) 0.079(16) -0.030(14) 0.018(10) -0.025(11) C26B 0.053(11) 0.054(13) 0.087(16) -0.008(12) 0.001(11) 0.004(10) C31B 0.048(10) 0.074(15) 0.044(11) -0.013(10) 0.006(8) 0.003(10) C32B 0.074(13) 0.046(11) 0.058(12) -0.010(10) -0.017(10) -0.005(10) C33B 0.041(9) 0.052(11) 0.045(10) 0.000(9) -0.005(8) 0.004(8) C34B 0.064(12) 0.051(12) 0.063(13) -0.002(10) -0.011(10) -0.002(10) C35B 0.059(12) 0.061(14) 0.064(13) -0.007(11) -0.011(10) -0.002(10) _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 Fe1 C2 1.748(14) . ? Fe1 C3 1.751(17) . ? Fe1 C35 2.082(17) . ? Fe1 C31 2.083(19) . ? Fe1 C33 2.108(16) . ? Fe1 C34 2.122(14) . ? Fe1 C32 2.124(19) . ? Fe1 Si1 2.326(5) . ? Si1 C11 1.884(16) . ? Si1 C1 1.888(15) . ? Si1 C21 1.938(15) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O2 1.145(18) . ? C3 O3 1.156(19) . ? C11 C12 1.39(2) . ? C11 C16 1.42(2) . ? C12 C13 1.41(2) . ? C12 H12 0.9500 . ? C13 C14 1.35(3) . ? C13 H13 0.9500 . ? C14 C15 1.44(3) . ? C14 H14 0.9500 . ? C15 C16 1.41(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.36(2) . ? C21 C22 1.40(2) . ? C22 C23 1.38(2) . ? C22 H22 0.9500 . ? C23 C24 1.40(3) . ? C23 H23 0.9500 . ? C24 C25 1.41(3) . ? C24 H24 0.9500 . ? C25 C26 1.45(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C35 1.38(3) . ? C31 C32 1.44(3) . ? C31 H31 0.9500 . ? C32 C33 1.42(2) . ? C32 H32 0.9500 . ? C33 C34 1.35(2) . ? C33 H33 0.9500 . ? C34 C35 1.42(3) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? Fe1A C3A 1.711(16) . ? Fe1A C2A 1.756(17) . ? Fe1A C35A 2.066(17) . ? Fe1A C32A 2.082(17) . ? Fe1A C31A 2.097(16) . ? Fe1A C33A 2.103(17) . ? Fe1A C34A 2.118(18) . ? Fe1A Si1A 2.323(5) . ? Si1A C1A 1.836(18) . ? Si1A C11A 1.882(15) . ? Si1A C21A 1.889(15) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A O2A 1.14(2) . ? C3A O3A 1.207(19) . ? C21A C26A 1.42(2) . ? C21A C22A 1.44(2) . ? C22A C23A 1.41(2) . ? C22A H22A 0.9500 . ? C23A C24A 1.37(3) . ? C23A H23A 0.9500 . ? C24A C25A 1.42(3) . ? C24A H24A 0.9500 . ? C25A C26A 1.37(2) . ? C25A H25A 0.9500 . ? C26A H26A 0.9500 . ? C11A C16A 1.40(2) . ? C11A C12A 1.41(2) . ? C12A C13A 1.40(2) . ? C12A H12A 0.9500 . ? C13A C14A 1.38(3) . ? C13A H13A 0.9500 . ? C14A C15A 1.33(3) . ? C14A H14A 0.9500 . ? C15A C16A 1.42(2) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C31A C32A 1.39(2) . ? C31A C35A 1.40(2) . ? C31A H31A 0.9500 . ? C32A C33A 1.40(3) . ? C32A H32A 0.9500 . ? C33A C34A 1.44(3) . ? C33A H33A 0.9500 . ? C34A C35A 1.40(3) . ? C34A H34A 0.9500 . ? C35A H35A 0.9500 . ? Fe1B C2B 1.71(2) . ? Fe1B C3B 1.73(2) . ? Fe1B C31B 2.104(19) . ? Fe1B C32B 2.11(2) . ? Fe1B C34B 2.12(2) . ? Fe1B C35B 2.13(2) . ? Fe1B C33B 2.134(17) . ? Fe1B Si1B 2.337(6) . ? Si1B C1B 1.87(2) . ? Si1B C21B 1.873(19) . ? Si1B C11B 1.90(2) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? C2B O2B 1.17(2) . ? C3B O3B 1.17(2) . ? C11B C16B 1.34(3) . ? C11B C12B 1.39(3) . ? C12B C13B 1.38(3) . ? C12B H12B 0.9500 . ? C13B C14B 1.43(4) . ? C13B H13B 0.9500 . ? C14B C15B 1.31(3) . ? C14B H14B 0.9500 . ? C15B C16B 1.41(3) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? C21B C22B 1.38(3) . ? C21B C26B 1.42(3) . ? C22B C23B 1.37(3) . ? C22B H22B 0.9500 . ? C23B C24B 1.36(3) . ? C23B H23B 0.9500 . ? C24B C25B 1.39(3) . ? C24B H24B 0.9500 . ? C25B C26B 1.38(3) . ? C25B H25B 0.9500 . ? C26B H26B 0.9500 . ? C31B C32B 1.43(3) . ? C31B C35B 1.44(3) . ? C31B H31B 0.9500 . ? C32B C33B 1.47(3) . ? C32B H32B 0.9500 . ? C33B C34B 1.35(3) . ? C33B H33B 0.9500 . ? C34B C35B 1.44(3) . ? C34B H34B 0.9500 . ? C35B H35B 0.9500 . ? 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 Fe1 C3 98.4(8) . . ? C2 Fe1 C35 95.6(8) . . ? C3 Fe1 C35 159.5(8) . . ? C2 Fe1 C31 125.8(8) . . ? C3 Fe1 C31 134.6(8) . . ? C35 Fe1 C31 38.8(7) . . ? C2 Fe1 C33 131.1(7) . . ? C3 Fe1 C33 95.6(8) . . ? C35 Fe1 C33 63.9(8) . . ? C31 Fe1 C33 64.9(7) . . ? C2 Fe1 C34 98.6(7) . . ? C3 Fe1 C34 122.9(8) . . ? C35 Fe1 C34 39.4(7) . . ? C31 Fe1 C34 65.6(7) . . ? C33 Fe1 C34 37.1(7) . . ? C2 Fe1 C32 161.3(7) . . ? C3 Fe1 C32 98.7(8) . . ? C35 Fe1 C32 66.0(8) . . ? C31 Fe1 C32 40.0(7) . . ? C33 Fe1 C32 39.1(7) . . ? C34 Fe1 C32 65.5(7) . . ? C2 Fe1 Si1 88.0(5) . . ? C3 Fe1 Si1 85.8(6) . . ? C35 Fe1 Si1 109.7(6) . . ? C31 Fe1 Si1 85.7(5) . . ? C33 Fe1 Si1 139.8(5) . . ? C34 Fe1 Si1 148.7(5) . . ? C32 Fe1 Si1 100.8(5) . . ? C11 Si1 C1 107.1(8) . . ? C11 Si1 C21 105.3(7) . . ? C1 Si1 C21 105.6(7) . . ? C11 Si1 Fe1 111.9(4) . . ? C1 Si1 Fe1 109.8(6) . . ? C21 Si1 Fe1 116.5(5) . . ? 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 . . ? O2 C2 Fe1 178.4(16) . . ? O3 C3 Fe1 176.6(17) . . ? C12 C11 C16 118.1(15) . . ? C12 C11 Si1 122.1(12) . . ? C16 C11 Si1 119.8(13) . . ? C11 C12 C13 121.1(15) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 121.2(17) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 119.7(17) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 119.1(16) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C11 120.7(17) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C26 C21 C22 120.5(15) . . ? C26 C21 Si1 124.4(12) . . ? C22 C21 Si1 115.0(12) . . ? C23 C22 C21 121.1(18) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 119.4(18) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C23 C24 C25 120.4(17) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 118.5(17) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? C21 C26 C25 119.9(16) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C35 C31 C32 108.4(17) . . ? C35 C31 Fe1 70.6(11) . . ? C32 C31 Fe1 71.5(11) . . ? C35 C31 H31 125.8 . . ? C32 C31 H31 125.8 . . ? Fe1 C31 H31 123.7 . . ? C33 C32 C31 103.8(17) . . ? C33 C32 Fe1 69.8(10) . . ? C31 C32 Fe1 68.5(11) . . ? C33 C32 H32 128.1 . . ? C31 C32 H32 128.1 . . ? Fe1 C32 H32 125.2 . . ? C34 C33 C32 112.4(17) . . ? C34 C33 Fe1 72.0(9) . . ? C32 C33 Fe1 71.1(10) . . ? C34 C33 H33 123.8 . . ? C32 C33 H33 123.8 . . ? Fe1 C33 H33 124.7 . . ? C33 C34 C35 106.5(16) . . ? C33 C34 Fe1 70.9(9) . . ? C35 C34 Fe1 68.8(9) . . ? C33 C34 H34 126.7 . . ? C35 C34 H34 126.7 . . ? Fe1 C34 H34 125.2 . . ? C31 C35 C34 108.8(16) . . ? C31 C35 Fe1 70.7(10) . . ? C34 C35 Fe1 71.8(9) . . ? C31 C35 H35 125.6 . . ? C34 C35 H35 125.6 . . ? Fe1 C35 H35 123.6 . . ? C3A Fe1A C2A 97.7(8) . . ? C3A Fe1A C35A 160.0(8) . . ? C2A Fe1A C35A 96.1(7) . . ? C3A Fe1A C32A 99.0(8) . . ? C2A Fe1A C32A 160.8(7) . . ? C35A Fe1A C32A 65.5(7) . . ? C3A Fe1A C31A 133.2(8) . . ? C2A Fe1A C31A 128.1(7) . . ? C35A Fe1A C31A 39.2(7) . . ? C32A Fe1A C31A 38.8(7) . . ? C3A Fe1A C33A 94.4(8) . . ? C2A Fe1A C33A 130.0(7) . . ? C35A Fe1A C33A 65.7(7) . . ? C32A Fe1A C33A 39.0(7) . . ? C31A Fe1A C33A 65.4(7) . . ? C3A Fe1A C34A 124.5(9) . . ? C2A Fe1A C34A 96.1(8) . . ? C35A Fe1A C34A 39.2(7) . . ? C32A Fe1A C34A 66.4(8) . . ? C31A Fe1A C34A 66.1(8) . . ? C33A Fe1A C34A 40.0(7) . . ? C3A Fe1A Si1A 84.4(7) . . ? C2A Fe1A Si1A 90.2(6) . . ? C35A Fe1A Si1A 110.0(5) . . ? C32A Fe1A Si1A 100.9(6) . . ? C31A Fe1A Si1A 86.1(5) . . ? C33A Fe1A Si1A 139.4(6) . . ? C34A Fe1A Si1A 148.9(6) . . ? C1A Si1A C11A 106.3(8) . . ? C1A Si1A C21A 105.4(8) . . ? C11A Si1A C21A 104.4(7) . . ? C1A Si1A Fe1A 110.6(6) . . ? C11A Si1A Fe1A 113.4(5) . . ? C21A Si1A Fe1A 116.0(5) . . ? Si1A C1A H1A1 109.5 . . ? Si1A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? Si1A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? O2A C2A Fe1A 177.1(16) . . ? O3A C3A Fe1A 177.4(18) . . ? C26A C21A C22A 116.3(14) . . ? C26A C21A Si1A 127.7(12) . . ? C22A C21A Si1A 116.0(12) . . ? C23A C22A C21A 120.9(17) . . ? C23A C22A H22A 119.6 . . ? C21A C22A H22A 119.6 . . ? C24A C23A C22A 120.9(18) . . ? C24A C23A H23A 119.6 . . ? C22A C23A H23A 119.6 . . ? C23A C24A C25A 118.7(16) . . ? C23A C24A H24A 120.6 . . ? C25A C24A H24A 120.6 . . ? C26A C25A C24A 121.5(17) . . ? C26A C25A H25A 119.3 . . ? C24A C25A H25A 119.3 . . ? C25A C26A C21A 121.7(17) . . ? C25A C26A H26A 119.1 . . ? C21A C26A H26A 119.1 . . ? C16A C11A C12A 117.2(15) . . ? C16A C11A Si1A 121.3(13) . . ? C12A C11A Si1A 121.4(13) . . ? C13A C12A C11A 119.7(17) . . ? C13A C12A H12A 120.1 . . ? C11A C12A H12A 120.1 . . ? C14A C13A C12A 122.4(16) . . ? C14A C13A H13A 118.8 . . ? C12A C13A H13A 118.8 . . ? C15A C14A C13A 117.6(15) . . ? C15A C14A H14A 121.2 . . ? C13A C14A H14A 121.2 . . ? C14A C15A C16A 123.4(19) . . ? C14A C15A H15A 118.3 . . ? C16A C15A H15A 118.3 . . ? C11A C16A C15A 119.5(18) . . ? C11A C16A H16A 120.2 . . ? C15A C16A H16A 120.2 . . ? C32A C31A C35A 107.3(17) . . ? C32A C31A Fe1A 70.0(9) . . ? C35A C31A Fe1A 69.2(10) . . ? C32A C31A H31A 126.3 . . ? C35A C31A H31A 126.3 . . ? Fe1A C31A H31A 126.0 . . ? C31A C32A C33A 109.0(16) . . ? C31A C32A Fe1A 71.2(10) . . ? C33A C32A Fe1A 71.3(10) . . ? C31A C32A H32A 125.5 . . ? C33A C32A H32A 125.5 . . ? Fe1A C32A H32A 123.6 . . ? C32A C33A C34A 108.1(17) . . ? C32A C33A Fe1A 69.7(10) . . ? C34A C33A Fe1A 70.6(10) . . ? C32A C33A H33A 125.9 . . ? C34A C33A H33A 125.9 . . ? Fe1A C33A H33A 125.4 . . ? C35A C34A C33A 105.0(17) . . ? C35A C34A Fe1A 68.4(10) . . ? C33A C34A Fe1A 69.4(10) . . ? C35A C34A H34A 127.5 . . ? C33A C34A H34A 127.5 . . ? Fe1A C34A H34A 126.3 . . ? C31A C35A C34A 110.4(16) . . ? C31A C35A Fe1A 71.6(9) . . ? C34A C35A Fe1A 72.4(10) . . ? C31A C35A H35A 124.8 . . ? C34A C35A H35A 124.8 . . ? Fe1A C35A H35A 122.8 . . ? C2B Fe1B C3B 94.3(9) . . ? C2B Fe1B C31B 133.5(9) . . ? C3B Fe1B C31B 131.1(9) . . ? C2B Fe1B C32B 162.3(9) . . ? C3B Fe1B C32B 97.8(9) . . ? C31B Fe1B C32B 39.5(8) . . ? C2B Fe1B C34B 97.7(8) . . ? C3B Fe1B C34B 126.8(9) . . ? C31B Fe1B C34B 65.5(9) . . ? C32B Fe1B C34B 64.7(8) . . ? C2B Fe1B C35B 99.3(9) . . ? C3B Fe1B C35B 162.0(8) . . ? C31B Fe1B C35B 39.7(8) . . ? C32B Fe1B C35B 66.4(8) . . ? C34B Fe1B C35B 39.6(8) . . ? C2B Fe1B C33B 125.4(8) . . ? C3B Fe1B C33B 96.6(8) . . ? C31B Fe1B C33B 66.7(7) . . ? C32B Fe1B C33B 40.3(7) . . ? C34B Fe1B C33B 37.1(7) . . ? C35B Fe1B C33B 65.9(7) . . ? C2B Fe1B Si1B 86.8(5) . . ? C3B Fe1B Si1B 89.6(7) . . ? C31B Fe1B Si1B 84.4(6) . . ? C32B Fe1B Si1B 106.1(6) . . ? C34B Fe1B Si1B 142.5(6) . . ? C35B Fe1B Si1B 102.8(6) . . ? C33B Fe1B Si1B 146.4(5) . . ? C1B Si1B C21B 105.9(9) . . ? C1B Si1B C11B 109.1(9) . . ? C21B Si1B C11B 105.6(8) . . ? C1B Si1B Fe1B 111.6(6) . . ? C21B Si1B Fe1B 115.3(6) . . ? C11B Si1B Fe1B 109.1(5) . . ? Si1B C1B H1B1 109.5 . . ? Si1B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? Si1B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? O2B C2B Fe1B 177.0(19) . . ? O3B C3B Fe1B 174(2) . . ? C16B C11B C12B 116(2) . . ? C16B C11B Si1B 123.6(15) . . ? C12B C11B Si1B 120.1(16) . . ? C13B C12B C11B 122(2) . . ? C13B C12B H12B 119.0 . . ? C11B C12B H12B 119.0 . . ? C12B C13B C14B 119(2) . . ? C12B C13B H13B 120.7 . . ? C14B C13B H13B 120.7 . . ? C15B C14B C13B 119(2) . . ? C15B C14B H14B 120.4 . . ? C13B C14B H14B 120.4 . . ? C14B C15B C16B 120(2) . . ? C14B C15B H15B 119.9 . . ? C16B C15B H15B 119.9 . . ? C11B C16B C15B 123(2) . . ? C11B C16B H16B 118.3 . . ? C15B C16B H16B 118.3 . . ? C22B C21B C26B 114.4(19) . . ? C22B C21B Si1B 126.0(17) . . ? C26B C21B Si1B 119.5(15) . . ? C23B C22B C21B 126(2) . . ? C23B C22B H22B 116.9 . . ? C21B C22B H22B 116.9 . . ? C24B C23B C22B 118.6(19) . . ? C24B C23B H23B 120.7 . . ? C22B C23B H23B 120.7 . . ? C23B C24B C25B 118.4(19) . . ? C23B C24B H24B 120.8 . . ? C25B C24B H24B 120.8 . . ? C26B C25B C24B 123(2) . . ? C26B C25B H25B 118.6 . . ? C24B C25B H25B 118.6 . . ? C25B C26B C21B 119(2) . . ? C25B C26B H26B 120.3 . . ? C21B C26B H26B 120.3 . . ? C32B C31B C35B 108.5(18) . . ? C32B C31B Fe1B 70.7(11) . . ? C35B C31B Fe1B 71.1(11) . . ? C32B C31B H31B 125.7 . . ? C35B C31B H31B 125.7 . . ? Fe1B C31B H31B 124.1 . . ? C31B C32B C33B 107.3(18) . . ? C31B C32B Fe1B 69.8(11) . . ? C33B C32B Fe1B 70.5(11) . . ? C31B C32B H32B 126.4 . . ? C33B C32B H32B 126.4 . . ? Fe1B C32B H32B 124.9 . . ? C34B C33B C32B 106.9(17) . . ? C34B C33B Fe1B 70.7(11) . . ? C32B C33B Fe1B 69.1(10) . . ? C34B C33B H33B 126.5 . . ? C32B C33B H33B 126.5 . . ? Fe1B C33B H33B 125.2 . . ? C33B C34B C35B 112(2) . . ? C33B C34B Fe1B 72.2(12) . . ? C35B C34B Fe1B 70.7(12) . . ? C33B C34B H34B 123.9 . . ? C35B C34B H34B 123.9 . . ? Fe1B C34B H34B 124.8 . . ? C34B C35B C31B 105.0(18) . . ? C34B C35B Fe1B 69.6(12) . . ? C31B C35B Fe1B 69.1(12) . . ? C34B C35B H35B 127.5 . . ? C31B C35B H35B 127.5 . . ? Fe1B C35B H35B 125.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Fe1 Si1 C11 -72.5(8) . . . . ? C3 Fe1 Si1 C11 -171.0(8) . . . . ? C35 Fe1 Si1 C11 22.7(8) . . . . ? C31 Fe1 Si1 C11 53.6(8) . . . . ? C33 Fe1 Si1 C11 95.2(10) . . . . ? C34 Fe1 Si1 C11 30.9(11) . . . . ? C32 Fe1 Si1 C11 90.9(8) . . . . ? C2 Fe1 Si1 C1 168.7(8) . . . . ? C3 Fe1 Si1 C1 70.1(8) . . . . ? C35 Fe1 Si1 C1 -96.1(8) . . . . ? C31 Fe1 Si1 C1 -65.2(8) . . . . ? C33 Fe1 Si1 C1 -23.6(10) . . . . ? C34 Fe1 Si1 C1 -88.0(11) . . . . ? C32 Fe1 Si1 C1 -28.0(8) . . . . ? C2 Fe1 Si1 C21 48.8(8) . . . . ? C3 Fe1 Si1 C21 -49.8(8) . . . . ? C35 Fe1 Si1 C21 143.9(8) . . . . ? C31 Fe1 Si1 C21 174.9(7) . . . . ? C33 Fe1 Si1 C21 -143.6(10) . . . . ? C34 Fe1 Si1 C21 152.1(10) . . . . ? C32 Fe1 Si1 C21 -147.9(8) . . . . ? C3 Fe1 C2 O2 171(100) . . . . ? C35 Fe1 C2 O2 -24(64) . . . . ? C31 Fe1 C2 O2 2(64) . . . . ? C33 Fe1 C2 O2 -84(64) . . . . ? C34 Fe1 C2 O2 -64(64) . . . . ? C32 Fe1 C2 O2 -33(65) . . . . ? Si1 Fe1 C2 O2 86(64) . . . . ? C2 Fe1 C3 O3 132(27) . . . . ? C35 Fe1 C3 O3 0(28) . . . . ? C31 Fe1 C3 O3 -61(27) . . . . ? C33 Fe1 C3 O3 -1(27) . . . . ? C34 Fe1 C3 O3 26(27) . . . . ? C32 Fe1 C3 O3 -40(27) . . . . ? Si1 Fe1 C3 O3 -140(27) . . . . ? C1 Si1 C11 C12 14.5(14) . . . . ? C21 Si1 C11 C12 126.7(13) . . . . ? Fe1 Si1 C11 C12 -105.9(12) . . . . ? C1 Si1 C11 C16 -164.1(12) . . . . ? C21 Si1 C11 C16 -52.0(13) . . . . ? Fe1 Si1 C11 C16 75.5(12) . . . . ? C16 C11 C12 C13 -3(2) . . . . ? Si1 C11 C12 C13 178.0(12) . . . . ? C11 C12 C13 C14 2(2) . . . . ? C12 C13 C14 C15 -1(3) . . . . ? C13 C14 C15 C16 1(2) . . . . ? C14 C15 C16 C11 -3(2) . . . . ? C12 C11 C16 C15 4(2) . . . . ? Si1 C11 C16 C15 -177.4(12) . . . . ? C11 Si1 C21 C26 127.2(14) . . . . ? C1 Si1 C21 C26 -119.6(15) . . . . ? Fe1 Si1 C21 C26 2.6(16) . . . . ? C11 Si1 C21 C22 -56.7(13) . . . . ? C1 Si1 C21 C22 56.5(13) . . . . ? Fe1 Si1 C21 C22 178.6(10) . . . . ? C26 C21 C22 C23 -1(2) . . . . ? Si1 C21 C22 C23 -176.9(12) . . . . ? C21 C22 C23 C24 0(2) . . . . ? C22 C23 C24 C25 2(2) . . . . ? C23 C24 C25 C26 -3(2) . . . . ? C22 C21 C26 C25 -1(2) . . . . ? Si1 C21 C26 C25 174.9(12) . . . . ? C24 C25 C26 C21 3(2) . . . . ? C2 Fe1 C31 C35 -45.0(14) . . . . ? C3 Fe1 C31 C35 150.8(12) . . . . ? C33 Fe1 C31 C35 78.9(12) . . . . ? C34 Fe1 C31 C35 37.9(11) . . . . ? C32 Fe1 C31 C35 118.1(16) . . . . ? Si1 Fe1 C31 C35 -129.4(11) . . . . ? C2 Fe1 C31 C32 -163.2(10) . . . . ? C3 Fe1 C31 C32 32.7(15) . . . . ? C35 Fe1 C31 C32 -118.1(16) . . . . ? C33 Fe1 C31 C32 -39.3(10) . . . . ? C34 Fe1 C31 C32 -80.3(11) . . . . ? Si1 Fe1 C31 C32 112.5(10) . . . . ? C35 C31 C32 C33 0(2) . . . . ? Fe1 C31 C32 C33 61.4(12) . . . . ? C35 C31 C32 Fe1 -61.3(13) . . . . ? C2 Fe1 C32 C33 -68(3) . . . . ? C3 Fe1 C32 C33 88.2(12) . . . . ? C35 Fe1 C32 C33 -77.5(12) . . . . ? C31 Fe1 C32 C33 -114.7(16) . . . . ? C34 Fe1 C32 C33 -34.1(11) . . . . ? Si1 Fe1 C32 C33 175.6(10) . . . . ? C2 Fe1 C32 C31 47(3) . . . . ? C3 Fe1 C32 C31 -157.1(11) . . . . ? C35 Fe1 C32 C31 37.2(10) . . . . ? C33 Fe1 C32 C31 114.7(16) . . . . ? C34 Fe1 C32 C31 80.6(11) . . . . ? Si1 Fe1 C32 C31 -69.7(10) . . . . ? C31 C32 C33 C34 0(2) . . . . ? Fe1 C32 C33 C34 60.4(13) . . . . ? C31 C32 C33 Fe1 -60.5(12) . . . . ? C2 Fe1 C33 C34 34.5(15) . . . . ? C3 Fe1 C33 C34 140.8(12) . . . . ? C35 Fe1 C33 C34 -39.0(11) . . . . ? C31 Fe1 C33 C34 -82.1(12) . . . . ? C32 Fe1 C33 C34 -122.3(17) . . . . ? Si1 Fe1 C33 C34 -129.1(10) . . . . ? C2 Fe1 C33 C32 156.8(12) . . . . ? C3 Fe1 C33 C32 -96.9(12) . . . . ? C35 Fe1 C33 C32 83.3(13) . . . . ? C31 Fe1 C33 C32 40.2(11) . . . . ? C34 Fe1 C33 C32 122.3(17) . . . . ? Si1 Fe1 C33 C32 -6.8(16) . . . . ? C32 C33 C34 C35 0(2) . . . . ? Fe1 C33 C34 C35 59.8(11) . . . . ? C32 C33 C34 Fe1 -59.8(13) . . . . ? C2 Fe1 C34 C33 -154.5(12) . . . . ? C3 Fe1 C34 C33 -48.6(14) . . . . ? C35 Fe1 C34 C33 117.3(16) . . . . ? C31 Fe1 C34 C33 80.1(12) . . . . ? C32 Fe1 C34 C33 35.9(11) . . . . ? Si1 Fe1 C34 C33 105.1(12) . . . . ? C2 Fe1 C34 C35 88.3(12) . . . . ? C3 Fe1 C34 C35 -165.8(12) . . . . ? C31 Fe1 C34 C35 -37.2(11) . . . . ? C33 Fe1 C34 C35 -117.3(16) . . . . ? C32 Fe1 C34 C35 -81.4(12) . . . . ? Si1 Fe1 C34 C35 -12.1(16) . . . . ? C32 C31 C35 C34 0(2) . . . . ? Fe1 C31 C35 C34 -62.0(12) . . . . ? C32 C31 C35 Fe1 61.8(13) . . . . ? C33 C34 C35 C31 0.1(19) . . . . ? Fe1 C34 C35 C31 61.3(12) . . . . ? C33 C34 C35 Fe1 -61.2(11) . . . . ? C2 Fe1 C35 C31 144.8(12) . . . . ? C3 Fe1 C35 C31 -82(3) . . . . ? C33 Fe1 C35 C31 -81.7(12) . . . . ? C34 Fe1 C35 C31 -118.4(16) . . . . ? C32 Fe1 C35 C31 -38.4(11) . . . . ? Si1 Fe1 C35 C31 54.9(12) . . . . ? C2 Fe1 C35 C34 -96.8(11) . . . . ? C3 Fe1 C35 C34 36(3) . . . . ? C31 Fe1 C35 C34 118.4(16) . . . . ? C33 Fe1 C35 C34 36.7(10) . . . . ? C32 Fe1 C35 C34 80.0(11) . . . . ? Si1 Fe1 C35 C34 173.3(9) . . . . ? C3A Fe1A Si1A C1A 69.1(9) . . . . ? C2A Fe1A Si1A C1A 166.8(8) . . . . ? C35A Fe1A Si1A C1A -96.7(9) . . . . ? C32A Fe1A Si1A C1A -29.0(8) . . . . ? C31A Fe1A Si1A C1A -65.0(8) . . . . ? C33A Fe1A Si1A C1A -21.1(10) . . . . ? C34A Fe1A Si1A C1A -91.0(13) . . . . ? C3A Fe1A Si1A C11A -171.6(9) . . . . ? C2A Fe1A Si1A C11A -73.9(8) . . . . ? C35A Fe1A Si1A C11A 22.6(8) . . . . ? C32A Fe1A Si1A C11A 90.3(8) . . . . ? C31A Fe1A Si1A C11A 54.2(8) . . . . ? C33A Fe1A Si1A C11A 98.1(10) . . . . ? C34A Fe1A Si1A C11A 28.3(13) . . . . ? C3A Fe1A Si1A C21A -50.8(8) . . . . ? C2A Fe1A Si1A C21A 46.9(7) . . . . ? C35A Fe1A Si1A C21A 143.4(7) . . . . ? C32A Fe1A Si1A C21A -148.9(7) . . . . ? C31A Fe1A Si1A C21A 175.1(7) . . . . ? C33A Fe1A Si1A C21A -141.0(9) . . . . ? C34A Fe1A Si1A C21A 149.1(12) . . . . ? C3A Fe1A C2A O2A 156(34) . . . . ? C35A Fe1A C2A O2A -39(34) . . . . ? C32A Fe1A C2A O2A -54(35) . . . . ? C31A Fe1A C2A O2A -14(34) . . . . ? C33A Fe1A C2A O2A -102(34) . . . . ? C34A Fe1A C2A O2A -78(34) . . . . ? Si1A Fe1A C2A O2A 71(34) . . . . ? C2A Fe1A C3A O3A 108(43) . . . . ? C35A Fe1A C3A O3A -25(45) . . . . ? C32A Fe1A C3A O3A -62(43) . . . . ? C31A Fe1A C3A O3A -83(43) . . . . ? C33A Fe1A C3A O3A -23(43) . . . . ? C34A Fe1A C3A O3A 5(43) . . . . ? Si1A Fe1A C3A O3A -162(43) . . . . ? C1A Si1A C21A C26A -120.9(15) . . . . ? C11A Si1A C21A C26A 127.4(14) . . . . ? Fe1A Si1A C21A C26A 1.8(16) . . . . ? C1A Si1A C21A C22A 58.7(13) . . . . ? C11A Si1A C21A C22A -53.1(13) . . . . ? Fe1A Si1A C21A C22A -178.7(10) . . . . ? C26A C21A C22A C23A 1(2) . . . . ? Si1A C21A C22A C23A -178.7(13) . . . . ? C21A C22A C23A C24A 1(3) . . . . ? C22A C23A C24A C25A 0(3) . . . . ? C23A C24A C25A C26A -2(3) . . . . ? C24A C25A C26A C21A 4(3) . . . . ? C22A C21A C26A C25A -3(2) . . . . ? Si1A C21A C26A C25A 176.7(13) . . . . ? C1A Si1A C11A C16A -165.4(14) . . . . ? C21A Si1A C11A C16A -54.2(15) . . . . ? Fe1A Si1A C11A C16A 72.9(14) . . . . ? C1A Si1A C11A C12A 18.7(16) . . . . ? C21A Si1A C11A C12A 129.9(14) . . . . ? Fe1A Si1A C11A C12A -103.0(13) . . . . ? C16A C11A C12A C13A 3(2) . . . . ? Si1A C11A C12A C13A 179.3(13) . . . . ? C11A C12A C13A C14A -2(3) . . . . ? C12A C13A C14A C15A 0(3) . . . . ? C13A C14A C15A C16A 2(3) . . . . ? C12A C11A C16A C15A -2(2) . . . . ? Si1A C11A C16A C15A -177.8(14) . . . . ? C14A C15A C16A C11A -1(3) . . . . ? C3A Fe1A C31A C32A 34.2(16) . . . . ? C2A Fe1A C31A C32A -160.1(12) . . . . ? C35A Fe1A C31A C32A -118.5(16) . . . . ? C33A Fe1A C31A C32A -37.4(11) . . . . ? C34A Fe1A C31A C32A -81.5(12) . . . . ? Si1A Fe1A C31A C32A 112.8(11) . . . . ? C3A Fe1A C31A C35A 152.7(12) . . . . ? C2A Fe1A C31A C35A -41.6(14) . . . . ? C32A Fe1A C31A C35A 118.5(16) . . . . ? C33A Fe1A C31A C35A 81.1(12) . . . . ? C34A Fe1A C31A C35A 37.0(11) . . . . ? Si1A Fe1A C31A C35A -128.7(10) . . . . ? C35A C31A C32A C33A 2.2(19) . . . . ? Fe1A C31A C32A C33A 61.6(12) . . . . ? C35A C31A C32A Fe1A -59.4(12) . . . . ? C3A Fe1A C32A C31A -155.5(12) . . . . ? C2A Fe1A C32A C31A 55(3) . . . . ? C35A Fe1A C32A C31A 37.6(11) . . . . ? C33A Fe1A C32A C31A 118.6(15) . . . . ? C34A Fe1A C32A C31A 80.7(12) . . . . ? Si1A Fe1A C32A C31A -69.5(11) . . . . ? C3A Fe1A C32A C33A 85.9(11) . . . . ? C2A Fe1A C32A C33A -64(3) . . . . ? C35A Fe1A C32A C33A -81.0(11) . . . . ? C31A Fe1A C32A C33A -118.6(15) . . . . ? C34A Fe1A C32A C33A -37.9(11) . . . . ? Si1A Fe1A C32A C33A 171.9(9) . . . . ? C31A C32A C33A C34A -1.1(19) . . . . ? Fe1A C32A C33A C34A 60.4(11) . . . . ? C31A C32A C33A Fe1A -61.5(12) . . . . ? C3A Fe1A C33A C32A -98.9(11) . . . . ? C2A Fe1A C33A C32A 157.3(10) . . . . ? C35A Fe1A C33A C32A 80.5(11) . . . . ? C31A Fe1A C33A C32A 37.2(10) . . . . ? C34A Fe1A C33A C32A 118.8(16) . . . . ? Si1A Fe1A C33A C32A -12.3(13) . . . . ? C3A Fe1A C33A C34A 142.3(13) . . . . ? C2A Fe1A C33A C34A 38.5(15) . . . . ? C35A Fe1A C33A C34A -38.3(11) . . . . ? C32A Fe1A C33A C34A -118.8(16) . . . . ? C31A Fe1A C33A C34A -81.6(12) . . . . ? Si1A Fe1A C33A C34A -131.1(11) . . . . ? C32A C33A C34A C35A -0.4(18) . . . . ? Fe1A C33A C34A C35A 59.5(11) . . . . ? C32A C33A C34A Fe1A -59.8(12) . . . . ? C3A Fe1A C34A C35A -164.2(12) . . . . ? C2A Fe1A C34A C35A 92.1(12) . . . . ? C32A Fe1A C34A C35A -79.6(12) . . . . ? C31A Fe1A C34A C35A -37.0(11) . . . . ? C33A Fe1A C34A C35A -116.5(16) . . . . ? Si1A Fe1A C34A C35A -8.5(18) . . . . ? C3A Fe1A C34A C33A -47.7(15) . . . . ? C2A Fe1A C34A C33A -151.4(11) . . . . ? C35A Fe1A C34A C33A 116.5(16) . . . . ? C32A Fe1A C34A C33A 37.0(11) . . . . ? C31A Fe1A C34A C33A 79.5(12) . . . . ? Si1A Fe1A C34A C33A 108.1(13) . . . . ? C32A C31A C35A C34A -2(2) . . . . ? Fe1A C31A C35A C34A -62.4(12) . . . . ? C32A C31A C35A Fe1A 59.9(11) . . . . ? C33A C34A C35A C31A 1.8(19) . . . . ? Fe1A C34A C35A C31A 61.9(12) . . . . ? C33A C34A C35A Fe1A -60.1(11) . . . . ? C3A Fe1A C35A C31A -78(3) . . . . ? C2A Fe1A C35A C31A 148.3(11) . . . . ? C32A Fe1A C35A C31A -37.2(11) . . . . ? C33A Fe1A C35A C31A -80.3(12) . . . . ? C34A Fe1A C35A C31A -119.4(16) . . . . ? Si1A Fe1A C35A C31A 55.9(11) . . . . ? C3A Fe1A C35A C34A 41(3) . . . . ? C2A Fe1A C35A C34A -92.3(12) . . . . ? C32A Fe1A C35A C34A 82.2(12) . . . . ? C31A Fe1A C35A C34A 119.4(16) . . . . ? C33A Fe1A C35A C34A 39.2(11) . . . . ? Si1A Fe1A C35A C34A 175.4(10) . . . . ? C2B Fe1B Si1B C1B 157.6(10) . . . . ? C3B Fe1B Si1B C1B 63.3(10) . . . . ? C31B Fe1B Si1B C1B -68.1(10) . . . . ? C32B Fe1B Si1B C1B -34.7(10) . . . . ? C34B Fe1B Si1B C1B -104.0(13) . . . . ? C35B Fe1B Si1B C1B -103.5(10) . . . . ? C33B Fe1B Si1B C1B -38.0(13) . . . . ? C2B Fe1B Si1B C21B 36.8(10) . . . . ? C3B Fe1B Si1B C21B -57.5(10) . . . . ? C31B Fe1B Si1B C21B 171.1(10) . . . . ? C32B Fe1B Si1B C21B -155.5(10) . . . . ? C34B Fe1B Si1B C21B 135.2(12) . . . . ? C35B Fe1B Si1B C21B 135.7(10) . . . . ? C33B Fe1B Si1B C21B -158.8(12) . . . . ? C2B Fe1B Si1B C11B -81.8(9) . . . . ? C3B Fe1B Si1B C11B -176.0(9) . . . . ? C31B Fe1B Si1B C11B 52.5(9) . . . . ? C32B Fe1B Si1B C11B 85.9(9) . . . . ? C34B Fe1B Si1B C11B 16.6(12) . . . . ? C35B Fe1B Si1B C11B 17.1(9) . . . . ? C33B Fe1B Si1B C11B 82.6(12) . . . . ? C3B Fe1B C2B O2B 180(100) . . . . ? C31B Fe1B C2B O2B 11(28) . . . . ? C32B Fe1B C2B O2B -47(29) . . . . ? C34B Fe1B C2B O2B -52(28) . . . . ? C35B Fe1B C2B O2B -12(28) . . . . ? C33B Fe1B C2B O2B -79(28) . . . . ? Si1B Fe1B C2B O2B 91(28) . . . . ? C2B Fe1B C3B O3B -142(19) . . . . ? C31B Fe1B C3B O3B 27(19) . . . . ? C32B Fe1B C3B O3B 51(19) . . . . ? C34B Fe1B C3B O3B 115(19) . . . . ? C35B Fe1B C3B O3B 79(20) . . . . ? C33B Fe1B C3B O3B 92(19) . . . . ? Si1B Fe1B C3B O3B -55(19) . . . . ? C1B Si1B C11B C16B 174.6(15) . . . . ? C21B Si1B C11B C16B -72.0(17) . . . . ? Fe1B Si1B C11B C16B 52.5(17) . . . . ? C1B Si1B C11B C12B -6.2(17) . . . . ? C21B Si1B C11B C12B 107.2(16) . . . . ? Fe1B Si1B C11B C12B -128.4(14) . . . . ? C16B C11B C12B C13B 2(3) . . . . ? Si1B C11B C12B C13B -176.8(17) . . . . ? C11B C12B C13B C14B -5(3) . . . . ? C12B C13B C14B C15B 1(4) . . . . ? C13B C14B C15B C16B 4(3) . . . . ? C12B C11B C16B C15B 3(3) . . . . ? Si1B C11B C16B C15B -177.9(15) . . . . ? C14B C15B C16B C11B -6(3) . . . . ? C1B Si1B C21B C22B 121(2) . . . . ? C11B Si1B C21B C22B 5(2) . . . . ? Fe1B Si1B C21B C22B -115.3(18) . . . . ? C1B Si1B C21B C26B -62.6(19) . . . . ? C11B Si1B C21B C26B -178.3(16) . . . . ? Fe1B Si1B C21B C26B 61.2(19) . . . . ? C26B C21B C22B C23B 5(3) . . . . ? Si1B C21B C22B C23B -178.7(18) . . . . ? C21B C22B C23B C24B -4(4) . . . . ? C22B C23B C24B C25B 1(3) . . . . ? C23B C24B C25B C26B 2(3) . . . . ? C24B C25B C26B C21B -2(3) . . . . ? C22B C21B C26B C25B -2(3) . . . . ? Si1B C21B C26B C25B -178.4(17) . . . . ? C2B Fe1B C31B C32B -156.0(12) . . . . ? C3B Fe1B C31B C32B 39.2(17) . . . . ? C34B Fe1B C31B C32B -79.3(13) . . . . ? C35B Fe1B C31B C32B -118.4(17) . . . . ? C33B Fe1B C31B C32B -38.6(12) . . . . ? Si1B Fe1B C31B C32B 123.8(12) . . . . ? C2B Fe1B C31B C35B -37.6(16) . . . . ? C3B Fe1B C31B C35B 157.6(13) . . . . ? C32B Fe1B C31B C35B 118.4(17) . . . . ? C34B Fe1B C31B C35B 39.1(11) . . . . ? C33B Fe1B C31B C35B 79.8(12) . . . . ? Si1B Fe1B C31B C35B -117.8(11) . . . . ? C35B C31B C32B C33B 0(2) . . . . ? Fe1B C31B C32B C33B 60.9(13) . . . . ? C35B C31B C32B Fe1B -61.4(14) . . . . ? C2B Fe1B C32B C31B 76(3) . . . . ? C3B Fe1B C32B C31B -151.3(14) . . . . ? C34B Fe1B C32B C31B 81.6(14) . . . . ? C35B Fe1B C32B C31B 37.9(12) . . . . ? C33B Fe1B C32B C31B 117.8(17) . . . . ? Si1B Fe1B C32B C31B -59.4(13) . . . . ? C2B Fe1B C32B C33B -42(3) . . . . ? C3B Fe1B C32B C33B 91.0(13) . . . . ? C31B Fe1B C32B C33B -117.8(17) . . . . ? C34B Fe1B C32B C33B -36.2(11) . . . . ? C35B Fe1B C32B C33B -79.9(12) . . . . ? Si1B Fe1B C32B C33B -177.1(10) . . . . ? C31B C32B C33B C34B 1(2) . . . . ? Fe1B C32B C33B C34B 61.0(13) . . . . ? C31B C32B C33B Fe1B -60.4(13) . . . . ? C2B Fe1B C33B C34B 48.0(16) . . . . ? C3B Fe1B C33B C34B 148.0(14) . . . . ? C31B Fe1B C33B C34B -79.8(14) . . . . ? C32B Fe1B C33B C34B -117.6(18) . . . . ? C35B Fe1B C33B C34B -36.2(13) . . . . ? Si1B Fe1B C33B C34B -112.7(13) . . . . ? C2B Fe1B C33B C32B 165.6(12) . . . . ? C3B Fe1B C33B C32B -94.4(13) . . . . ? C31B Fe1B C33B C32B 37.8(12) . . . . ? C34B Fe1B C33B C32B 117.6(18) . . . . ? C35B Fe1B C33B C32B 81.4(13) . . . . ? Si1B Fe1B C33B C32B 5.0(17) . . . . ? C32B C33B C34B C35B 0(2) . . . . ? Fe1B C33B C34B C35B 59.6(15) . . . . ? C32B C33B C34B Fe1B -59.9(13) . . . . ? C2B Fe1B C34B C33B -142.3(13) . . . . ? C3B Fe1B C34B C33B -41.1(17) . . . . ? C31B Fe1B C34B C33B 83.1(13) . . . . ? C32B Fe1B C34B C33B 39.4(12) . . . . ? C35B Fe1B C34B C33B 122.3(19) . . . . ? Si1B Fe1B C34B C33B 123.0(11) . . . . ? C2B Fe1B C34B C35B 95.4(13) . . . . ? C3B Fe1B C34B C35B -163.4(13) . . . . ? C31B Fe1B C34B C35B -39.2(12) . . . . ? C32B Fe1B C34B C35B -82.9(14) . . . . ? C33B Fe1B C34B C35B -122.3(19) . . . . ? Si1B Fe1B C34B C35B 0.7(18) . . . . ? C33B C34B C35B C31B 0(2) . . . . ? Fe1B C34B C35B C31B 60.5(13) . . . . ? C33B C34B C35B Fe1B -60.4(15) . . . . ? C32B C31B C35B C34B 0(2) . . . . ? Fe1B C31B C35B C34B -60.8(14) . . . . ? C32B C31B C35B Fe1B 61.1(13) . . . . ? C2B Fe1B C35B C34B -90.8(13) . . . . ? C3B Fe1B C35B C34B 48(4) . . . . ? C31B Fe1B C35B C34B 115.9(17) . . . . ? C32B Fe1B C35B C34B 78.2(13) . . . . ? C33B Fe1B C35B C34B 33.9(12) . . . . ? Si1B Fe1B C35B C34B -179.5(11) . . . . ? C2B Fe1B C35B C31B 153.4(11) . . . . ? C3B Fe1B C35B C31B -68(3) . . . . ? C32B Fe1B C35B C31B -37.6(11) . . . . ? C34B Fe1B C35B C31B -115.9(17) . . . . ? C33B Fe1B C35B C31B -81.9(12) . . . . ? Si1B Fe1B C35B C31B 64.6(11) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.848 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.154 data_wa622 _database_code_depnum_ccdc_archive 'CCDC 832033' #TrackingRef 'publ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H32 Fe0.50 K O7' _chemical_formula_weight 463.49 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' 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' O O 0.0106 0.0060 '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 mc21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' _cell_length_a 11.4260(13) _cell_length_b 9.8741(8) _cell_length_c 21.0967(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2380.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3761 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 25.4 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8303 _exptl_absorpt_correction_T_max 0.8432 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 8991 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 25.57 _reflns_number_total 4207 _reflns_number_gt 3860 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0874P)^2^+1.4611P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.64(3) _refine_ls_number_reflns 4207 _refine_ls_number_parameters 272 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.040 _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 K1 K 0.5000 0.88664(11) 0.5671(5) 0.0279(3) Uani 1 2 d S . . K2 K 0.5000 0.61409(12) 0.3295(5) 0.0280(3) Uani 1 2 d S . . O11 O 0.5000 1.1709(4) 0.5316(5) 0.0371(9) Uani 1 2 d S . . C12 C 0.6037(4) 1.2483(4) 0.5436(5) 0.0504(12) Uani 1 1 d . . . H12A H 0.6026 1.2824 0.5877 0.060 Uiso 1 1 calc R . . H12B H 0.6067 1.3271 0.5147 0.060 Uiso 1 1 calc R . . C13 C 0.7095(4) 1.1606(5) 0.5336(6) 0.0614(16) Uani 1 1 d . . . H13A H 0.7079 1.1213 0.4905 0.074 Uiso 1 1 calc R . . H13B H 0.7815 1.2156 0.5379 0.074 Uiso 1 1 calc R . . O14 O 0.7094(2) 1.0557(3) 0.5794(5) 0.0388(7) Uani 1 1 d . . . C15 C 0.8110(3) 0.9722(5) 0.5733(5) 0.0451(12) Uani 1 1 d . . . H15A H 0.8825 1.0288 0.5749 0.054 Uiso 1 1 calc R . . H15B H 0.8095 0.9240 0.5321 0.054 Uiso 1 1 calc R . . C16 C 0.8116(3) 0.8716(5) 0.6270(5) 0.0405(10) Uani 1 1 d . . . H16A H 0.8833 0.8154 0.6250 0.049 Uiso 1 1 calc R . . H16B H 0.8106 0.9197 0.6681 0.049 Uiso 1 1 calc R . . O17 O 0.7110(2) 0.7882(3) 0.6214(5) 0.0377(7) Uani 1 1 d . . . C18 C 0.7086(4) 0.6847(6) 0.6684(5) 0.0515(13) Uani 1 1 d . . . H18A H 0.7047 0.7260 0.7111 0.062 Uiso 1 1 calc R . . H18B H 0.7808 0.6297 0.6658 0.062 Uiso 1 1 calc R . . C19 C 0.6028(4) 0.5958(5) 0.6577(5) 0.0485(12) Uani 1 1 d . . . H19A H 0.6035 0.5595 0.6140 0.058 Uiso 1 1 calc R . . H19B H 0.6039 0.5186 0.6877 0.058 Uiso 1 1 calc R . . O20 O 0.5000 0.6762(5) 0.6676(5) 0.0393(10) Uani 1 2 d S . . O21 O 0.5000 0.3311(4) 0.3648(5) 0.0385(9) Uani 1 2 d S . . C22 C 0.3968(4) 0.2531(4) 0.3544(5) 0.0521(13) Uani 1 1 d . . . H22A H 0.3956 0.1739 0.3832 0.062 Uiso 1 1 calc R . . H22B H 0.3947 0.2199 0.3102 0.062 Uiso 1 1 calc R . . C23 C 0.2931(5) 0.3423(5) 0.3671(5) 0.0554(13) Uani 1 1 d . . . H23A H 0.2203 0.2880 0.3661 0.066 Uiso 1 1 calc R . . H23B H 0.3002 0.3840 0.4096 0.066 Uiso 1 1 calc R . . O24 O 0.2889(2) 0.4453(3) 0.3196(5) 0.0379(7) Uani 1 1 d . . . C25 C 0.1882(3) 0.5305(5) 0.3258(5) 0.0430(11) Uani 1 1 d . . . H25A H 0.1910 0.5794 0.3667 0.052 Uiso 1 1 calc R . . H25B H 0.1162 0.4748 0.3249 0.052 Uiso 1 1 calc R . . C26 C 0.1868(3) 0.6290(5) 0.2726(5) 0.0398(10) Uani 1 1 d . . . H26A H 0.1879 0.5801 0.2316 0.048 Uiso 1 1 calc R . . H26B H 0.1145 0.6842 0.2744 0.048 Uiso 1 1 calc R . . O27 O 0.2867(2) 0.7147(3) 0.2773(5) 0.0348(6) Uani 1 1 d . . . C28 C 0.2910(4) 0.8113(5) 0.2268(5) 0.0453(11) Uani 1 1 d . . . H28A H 0.2191 0.8673 0.2270 0.054 Uiso 1 1 calc R . . H28B H 0.2958 0.7639 0.1855 0.054 Uiso 1 1 calc R . . C29 C 0.3960(4) 0.8992(5) 0.2357(5) 0.0449(11) Uani 1 1 d . . . H29A H 0.3955 0.9729 0.2039 0.054 Uiso 1 1 calc R . . H29B H 0.3942 0.9407 0.2784 0.054 Uiso 1 1 calc R . . O30 O 0.5000 0.8198(4) 0.2287(5) 0.0362(9) Uani 1 2 d S . . Fe1 Fe 0.0000 0.53713(8) 0.0859(4) 0.0334(2) Uani 1 2 d S . . C1 C 0.0000 0.6916(7) 0.1251(5) 0.0417(14) Uani 1 2 d S . . O1 O 0.0000 0.7961(5) 0.1529(5) 0.0569(12) Uani 1 2 d S . . C2 C 0.0000 0.4553(6) 0.1583(5) 0.0327(12) Uani 1 2 d S . . O2 O 0.0000 0.4011(5) 0.2085(5) 0.0445(10) Uani 1 2 d S . . C31 C 0.5000 0.6496(14) 0.4734(7) 0.034(3) Uiso 0.50 2 d SP . 1 H31 H 0.5000 0.5643 0.4942 0.041 Uiso 0.50 2 calc SPR . 1 C32 C 0.4052(9) 0.7112(12) 0.4583(6) 0.0363(18) Uiso 0.50 1 d P . 1 H32 H 0.3281 0.6794 0.4663 0.044 Uiso 0.50 1 calc PR . 1 C33 C 0.4348(6) 0.8364(8) 0.4274(6) 0.0286(16) Uiso 0.50 1 d P . 1 H33 H 0.3834 0.9033 0.4108 0.034 Uiso 0.50 1 calc PR . 1 C31' C 0.5000 0.8558(12) 0.4218(7) 0.031(2) Uiso 0.50 2 d SP . 2 H31' H 0.5000 0.9417 0.4015 0.037 Uiso 0.50 2 calc SPR . 2 C32' C 0.3959(6) 0.7713(9) 0.4419(6) 0.0265(16) Uiso 0.50 1 d P . 2 H32' H 0.3153 0.7910 0.4359 0.032 Uiso 0.50 1 calc PR . 2 C33' C 0.4446(8) 0.6579(9) 0.4710(6) 0.0277(15) Uiso 0.50 1 d P . 2 H33' H 0.3990 0.5874 0.4892 0.033 Uiso 0.50 1 calc PR . 2 C41 C 0.0000 0.3699(14) 0.0229(8) 0.056(4) Uiso 0.50 2 d SPD . 1 H41 H 0.0000 0.2780 0.0363 0.067 Uiso 0.50 2 calc SPR . 1 C42 C -0.0976(8) 0.4454(11) 0.0119(7) 0.070(3) Uiso 0.50 1 d PD . 1 H42 H -0.1765 0.4171 0.0171 0.084 Uiso 0.50 1 calc PR . 1 C43 C -0.0596(6) 0.5720(10) -0.0084(7) 0.047(2) Uiso 0.50 1 d PD . 1 H43 H -0.1083 0.6458 -0.0202 0.057 Uiso 0.50 1 calc PR . 1 C41' C 0.0000 0.6104(11) -0.0069(7) 0.045(3) Uiso 0.50 2 d SPD . 2 H41' H 0.0000 0.7039 -0.0175 0.054 Uiso 0.50 2 calc SPR . 2 C42' C -0.1025(6) 0.5272(8) 0.0025(6) 0.0342(17) Uiso 0.50 1 d PD . 2 H42' H -0.1815 0.5554 -0.0021 0.041 Uiso 0.50 1 calc PR . 2 C43' C -0.0638(5) 0.3956(7) 0.0199(6) 0.0301(15) Uiso 0.50 1 d PD . 2 H43' H -0.1126 0.3207 0.0298 0.036 Uiso 0.50 1 calc PR . 2 C51 C 0.0000 1.0573(7) 0.3025(5) 0.081(3) Uiso 1 2 d SD . . H51 H 0.0000 1.1042 0.2632 0.098 Uiso 1 2 calc SR . . C52 C 0.0936(9) 1.0302(8) 0.32518(13) 0.244(9) Uiso 1 1 d D . . H52 H 0.1647 1.0545 0.3048 0.293 Uiso 1 1 calc R . . C53 C 0.0928(10) 0.9692(15) 0.3762(6) 0.43(2) Uiso 1 1 d D . . H53 H 0.1640 0.9449 0.3965 0.510 Uiso 1 1 calc R . . C54 C 0.0000 0.9410(19) 0.3998(9) 0.273(15) Uiso 1 2 d SD . . H54 H 0.0000 0.8940 0.4391 0.328 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0312(5) 0.0278(6) 0.0247(6) -0.0006(4) 0.000 0.000 K2 0.0309(5) 0.0280(6) 0.0252(6) -0.0010(4) 0.000 0.000 O11 0.047(2) 0.030(2) 0.034(2) 0.0018(19) 0.000 0.000 C12 0.054(3) 0.030(2) 0.067(3) 0.009(2) -0.001(2) -0.009(2) C13 0.038(2) 0.053(3) 0.094(4) 0.032(3) 0.012(2) -0.009(2) O14 0.0326(12) 0.0332(14) 0.0504(18) 0.0037(16) 0.0034(13) -0.0025(11) C15 0.0273(16) 0.044(2) 0.064(4) -0.004(3) 0.0072(18) -0.0012(17) C16 0.0284(19) 0.047(3) 0.047(3) -0.008(2) -0.0042(17) 0.0063(18) O17 0.0345(14) 0.0403(16) 0.0383(16) 0.0065(14) -0.0039(12) 0.0036(12) C18 0.038(2) 0.066(3) 0.051(3) 0.030(3) 0.0025(19) 0.018(2) C19 0.054(3) 0.039(2) 0.053(3) 0.020(2) 0.007(2) 0.013(2) O20 0.033(2) 0.045(2) 0.040(2) 0.007(2) 0.000 0.000 O21 0.048(2) 0.033(2) 0.035(2) -0.005(2) 0.000 0.000 C22 0.056(3) 0.026(2) 0.074(4) 0.014(2) 0.005(2) -0.0060(19) C23 0.056(3) 0.040(3) 0.070(4) 0.019(3) 0.017(3) -0.006(2) O24 0.0359(14) 0.0383(15) 0.0395(17) -0.0011(15) 0.0058(12) -0.0039(11) C25 0.0289(17) 0.050(3) 0.050(3) -0.001(2) 0.0065(17) -0.0043(18) C26 0.0250(19) 0.047(2) 0.047(3) -0.007(2) -0.0028(17) -0.0019(17) O27 0.0328(14) 0.0381(15) 0.0335(15) 0.0052(13) -0.0057(11) -0.0008(12) C28 0.041(2) 0.052(3) 0.043(3) 0.013(2) -0.0090(18) 0.006(2) C29 0.043(2) 0.039(2) 0.053(3) 0.014(2) -0.001(2) 0.0065(19) O30 0.036(2) 0.031(2) 0.042(2) 0.003(2) 0.000 0.000 Fe1 0.0308(3) 0.0377(4) 0.0318(4) -0.0016(4) 0.000 0.000 C1 0.045(3) 0.047(4) 0.033(3) 0.005(3) 0.000 0.000 O1 0.069(3) 0.041(3) 0.061(3) -0.006(2) 0.000 0.000 C2 0.030(3) 0.035(3) 0.033(3) -0.006(2) 0.000 0.000 O2 0.041(2) 0.054(3) 0.039(2) 0.006(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 K1 O17 2.840(3) 4_655 ? K1 O17 2.840(3) . ? K1 O11 2.906(4) . ? K1 O14 2.929(3) . ? K1 O14 2.929(3) 4_655 ? K1 O20 2.969(4) . ? K1 C31 3.064(13) . ? K1 C32 3.073(8) 4_655 ? K1 C32 3.073(8) . ? K1 C31' 3.080(12) . ? K1 C33 3.081(7) . ? K1 C33 3.081(7) 4_655 ? K2 O27 2.853(3) 4_655 ? K2 O27 2.853(3) . ? K2 O21 2.892(5) . ? K2 O24 2.939(3) . ? K2 O24 2.939(3) 4_655 ? K2 O30 2.941(4) . ? K2 C31 3.055(13) . ? K2 C32' 3.073(8) 4_655 ? K2 C32' 3.073(8) . ? K2 C32 3.078(8) . ? K2 C32 3.079(8) 4_655 ? K2 C31' 3.081(12) . ? O11 C12 1.432(5) . ? O11 C12 1.432(5) 4_655 ? C12 C13 1.502(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O14 1.416(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O14 C15 1.429(5) . ? C15 C16 1.507(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O17 1.419(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O17 C18 1.424(6) . ? C18 C19 1.511(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 O20 1.433(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? O20 C19 1.433(5) 4_655 ? O21 C22 1.425(5) . ? O21 C22 1.425(5) 4_655 ? C22 C23 1.500(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O24 1.429(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? O24 C25 1.431(5) . ? C25 C26 1.486(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O27 1.424(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O27 C28 1.431(5) . ? C28 C29 1.493(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O30 1.431(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O30 C29 1.431(5) 4_655 ? Fe1 C2 1.727(6) . ? Fe1 C1 1.735(7) . ? Fe1 C41' 2.089(12) . ? Fe1 C43' 2.104(7) . ? Fe1 C43' 2.104(7) 4 ? Fe1 C42' 2.117(7) . ? Fe1 C42' 2.117(7) 4 ? Fe1 C41 2.120(14) . ? Fe1 C42 2.122(11) . ? Fe1 C42 2.122(11) 4 ? Fe1 C43 2.131(10) . ? Fe1 C43 2.131(10) 4 ? C1 O1 1.187(8) . ? C2 O2 1.188(7) . ? C31 C32 1.283(15) . ? C31 C32 1.283(15) 4_655 ? C31 H31 0.9500 . ? C32 C33 1.439(14) . ? C32 H32 0.9500 . ? C33 C33 1.490(15) 4_655 ? C33 H33 0.9500 . ? C31' C32' 1.514(11) 4_655 ? C31' C32' 1.514(11) . ? C31' H31' 0.9500 . ? C32' C33' 1.393(11) . ? C32' H32' 0.9500 . ? C33' C33' 1.266(19) 4_655 ? C33' H33' 0.9500 . ? C41 C42 1.362(11) 4 ? C41 C42 1.362(11) . ? C41 H41 0.9500 . ? C42 C43 1.391(12) . ? C42 H42 0.9500 . ? C43 C43 1.361(14) 4 ? C43 H43 0.9500 . ? C41' C42' 1.444(9) . ? C41' C42' 1.444(9) 4 ? C41' H41' 0.9500 . ? C42' C43' 1.421(9) . ? C42' H42' 0.9500 . ? C43' C43' 1.459(11) 4 ? C43' H43' 0.9500 . ? C51 C52 1.202(11) . ? C51 C52 1.202(11) 4 ? C51 H51 0.9500 . ? C52 C53 1.234(15) . ? C52 H52 0.9500 . ? C53 C54 1.204(12) . ? C53 H53 0.9500 . ? C54 C53 1.204(12) 4 ? C54 H54 0.9500 . ? 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 O17 K1 O17 116.16(13) 4_655 . ? O17 K1 O11 115.76(7) 4_655 . ? O17 K1 O11 115.76(7) . . ? O17 K1 O14 148.52(10) 4_655 . ? O17 K1 O14 57.71(8) . . ? O11 K1 O14 58.15(6) . . ? O17 K1 O14 57.71(8) 4_655 4_655 ? O17 K1 O14 148.52(10) . 4_655 ? O11 K1 O14 58.15(6) . 4_655 ? O14 K1 O14 109.58(11) . 4_655 ? O17 K1 O20 58.17(6) 4_655 . ? O17 K1 O20 58.17(6) . . ? O11 K1 O20 149.38(13) . . ? O14 K1 O20 109.62(8) . . ? O14 K1 O20 109.62(8) 4_655 . ? O17 K1 C31 89.93(15) 4_655 . ? O17 K1 C31 89.93(15) . . ? O11 K1 C31 124.9(3) . . ? O14 K1 C31 119.49(11) . . ? O14 K1 C31 119.49(11) 4_655 . ? O20 K1 C31 85.8(3) . . ? O17 K1 C32 114.0(2) 4_655 4_655 ? O17 K1 C32 78.98(19) . 4_655 ? O11 K1 C32 110.6(3) . 4_655 ? O14 K1 C32 95.7(2) . 4_655 ? O14 K1 C32 132.5(2) 4_655 4_655 ? O20 K1 C32 98.0(3) . 4_655 ? C31 K1 C32 24.1(3) . 4_655 ? O17 K1 C32 78.98(19) 4_655 . ? O17 K1 C32 114.0(2) . . ? O11 K1 C32 110.6(3) . . ? O14 K1 C32 132.5(2) . . ? O14 K1 C32 95.7(2) 4_655 . ? O20 K1 C32 98.0(3) . . ? C31 K1 C32 24.1(3) . . ? C32 K1 C32 41.3(4) 4_655 . ? O17 K1 C31' 111.55(12) 4_655 . ? O17 K1 C31' 111.55(12) . . ? O11 K1 C31' 80.7(2) . . ? O14 K1 C31' 98.30(15) . . ? O14 K1 C31' 98.29(15) 4_655 . ? O20 K1 C31' 129.9(2) . . ? C31 K1 C31' 44.1(3) . . ? C32 K1 C31' 37.0(3) 4_655 . ? C32 K1 C31' 37.0(3) . . ? O17 K1 C33 97.20(16) 4_655 . ? O17 K1 C33 122.40(15) . . ? O11 K1 C33 84.75(17) . . ? O14 K1 C33 111.95(17) . . ? O14 K1 C33 88.78(16) 4_655 . ? O20 K1 C33 124.80(18) . . ? C31 K1 C33 42.2(3) . . ? C32 K1 C33 43.9(2) 4_655 . ? C32 K1 C33 27.0(3) . . ? C31' K1 C33 14.51(14) . . ? O17 K1 C33 122.40(15) 4_655 4_655 ? O17 K1 C33 97.20(16) . 4_655 ? O11 K1 C33 84.76(17) . 4_655 ? O14 K1 C33 88.78(16) . 4_655 ? O14 K1 C33 111.95(16) 4_655 4_655 ? O20 K1 C33 124.80(18) . 4_655 ? C31 K1 C33 42.2(3) . 4_655 ? C32 K1 C33 27.0(3) 4_655 4_655 ? C32 K1 C33 43.9(2) . 4_655 ? C31' K1 C33 14.51(14) . 4_655 ? C33 K1 C33 28.0(3) . 4_655 ? O27 K2 O27 117.33(12) 4_655 . ? O27 K2 O21 115.83(7) 4_655 . ? O27 K2 O21 115.83(7) . . ? O27 K2 O24 150.57(10) 4_655 . ? O27 K2 O24 57.92(8) . . ? O21 K2 O24 58.02(6) . . ? O27 K2 O24 57.92(8) 4_655 4_655 ? O27 K2 O24 150.57(10) . 4_655 ? O21 K2 O24 58.02(6) . 4_655 ? O24 K2 O24 110.31(12) . 4_655 ? O27 K2 O30 58.68(6) 4_655 . ? O27 K2 O30 58.68(6) . . ? O21 K2 O30 148.58(13) . . ? O24 K2 O30 109.89(8) . . ? O24 K2 O30 109.89(8) 4_655 . ? O27 K2 C31 110.11(13) 4_655 . ? O27 K2 C31 110.11(13) . . ? O21 K2 C31 81.7(3) . . ? O24 K2 C31 97.79(16) . . ? O24 K2 C31 97.79(16) 4_655 . ? O30 K2 C31 129.7(3) . . ? O27 K2 C32' 77.97(17) 4_655 4_655 ? O27 K2 C32' 116.93(17) . 4_655 ? O21 K2 C32' 106.8(2) . 4_655 ? O24 K2 C32' 131.21(17) . 4_655 ? O24 K2 C32' 91.34(16) 4_655 4_655 ? O30 K2 C32' 102.1(2) . 4_655 ? C31 K2 C32' 34.5(2) . 4_655 ? O27 K2 C32' 116.93(17) 4_655 . ? O27 K2 C32' 77.97(17) . . ? O21 K2 C32' 106.8(2) . . ? O24 K2 C32' 91.34(16) . . ? O24 K2 C32' 131.21(17) 4_655 . ? O30 K2 C32' 102.1(2) . . ? C31 K2 C32' 34.5(2) . . ? C32' K2 C32' 45.6(3) 4_655 . ? O27 K2 C32 122.22(19) 4_655 . ? O27 K2 C32 86.1(2) . . ? O21 K2 C32 94.2(3) . . ? O24 K2 C32 87.16(18) . . ? O24 K2 C32 121.9(2) 4_655 . ? O30 K2 C32 115.0(3) . . ? C31 K2 C32 24.1(3) . . ? C32' K2 C32 45.41(18) 4_655 . ? C32' K2 C32 12.97(18) . . ? O27 K2 C32 86.1(2) 4_655 4_655 ? O27 K2 C32 122.22(19) . 4_655 ? O21 K2 C32 94.2(3) . 4_655 ? O24 K2 C32 121.9(2) . 4_655 ? O24 K2 C32 87.16(18) 4_655 4_655 ? O30 K2 C32 115.0(3) . 4_655 ? C31 K2 C32 24.1(3) . 4_655 ? C32' K2 C32 12.97(18) 4_655 4_655 ? C32' K2 C32 45.41(18) . 4_655 ? C32 K2 C32 41.2(4) . 4_655 ? O27 K2 C31' 88.54(14) 4_655 . ? O27 K2 C31' 88.54(14) . . ? O21 K2 C31' 125.9(3) . . ? O24 K2 C31' 118.95(10) . . ? O24 K2 C31' 118.95(10) 4_655 . ? O30 K2 C31' 85.5(2) . . ? C31 K2 C31' 44.2(3) . . ? C32' K2 C31' 28.5(2) 4_655 . ? C32' K2 C31' 28.5(2) . . ? C32 K2 C31' 36.9(3) . . ? C32 K2 C31' 36.9(3) 4_655 . ? C12 O11 C12 111.6(5) . 4_655 ? C12 O11 K1 118.0(2) . . ? C12 O11 K1 118.0(2) 4_655 . ? O11 C12 C13 109.5(4) . . ? O11 C12 H12A 109.8 . . ? C13 C12 H12A 109.8 . . ? O11 C12 H12B 109.8 . . ? C13 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? O14 C13 C12 109.0(4) . . ? O14 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? O14 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C13 O14 C15 111.1(3) . . ? C13 O14 K1 110.9(3) . . ? C15 O14 K1 109.1(2) . . ? O14 C15 C16 108.4(3) . . ? O14 C15 H15A 110.0 . . ? C16 C15 H15A 110.0 . . ? O14 C15 H15B 110.0 . . ? C16 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? O17 C16 C15 108.4(3) . . ? O17 C16 H16A 110.0 . . ? C15 C16 H16A 110.0 . . ? O17 C16 H16B 110.0 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? C16 O17 C18 111.9(3) . . ? C16 O17 K1 121.5(2) . . ? C18 O17 K1 120.7(2) . . ? O17 C18 C19 109.2(4) . . ? O17 C18 H18A 109.8 . . ? C19 C18 H18A 109.8 . . ? O17 C18 H18B 109.8 . . ? C19 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? O20 C19 C18 108.2(4) . . ? O20 C19 H19A 110.1 . . ? C18 C19 H19A 110.1 . . ? O20 C19 H19B 110.1 . . ? C18 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? C19 O20 C19 110.1(5) . 4_655 ? C19 O20 K1 106.5(2) . . ? C19 O20 K1 106.5(2) 4_655 . ? C22 O21 C22 111.7(5) . 4_655 ? C22 O21 K2 118.8(2) . . ? C22 O21 K2 118.8(2) 4_655 . ? O21 C22 C23 108.0(4) . . ? O21 C22 H22A 110.1 . . ? C23 C22 H22A 110.1 . . ? O21 C22 H22B 110.1 . . ? C23 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? O24 C23 C22 108.6(4) . . ? O24 C23 H23A 110.0 . . ? C22 C23 H23A 110.0 . . ? O24 C23 H23B 110.0 . . ? C22 C23 H23B 110.0 . . ? H23A C23 H23B 108.3 . . ? C23 O24 C25 112.5(3) . . ? C23 O24 K2 109.0(3) . . ? C25 O24 K2 108.7(2) . . ? O24 C25 C26 109.0(3) . . ? O24 C25 H25A 109.9 . . ? C26 C25 H25A 109.9 . . ? O24 C25 H25B 109.9 . . ? C26 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? O27 C26 C25 109.1(4) . . ? O27 C26 H26A 109.9 . . ? C25 C26 H26A 109.9 . . ? O27 C26 H26B 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? C26 O27 C28 111.8(3) . . ? C26 O27 K2 120.3(2) . . ? C28 O27 K2 119.4(2) . . ? O27 C28 C29 108.8(3) . . ? O27 C28 H28A 109.9 . . ? C29 C28 H28A 109.9 . . ? O27 C28 H28B 109.9 . . ? C29 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? O30 C29 C28 109.6(4) . . ? O30 C29 H29A 109.7 . . ? C28 C29 H29A 109.7 . . ? O30 C29 H29B 109.7 . . ? C28 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C29 O30 C29 112.2(5) . 4_655 ? C29 O30 K2 107.7(3) . . ? C29 O30 K2 107.7(3) 4_655 . ? C2 Fe1 C1 89.5(3) . . ? C2 Fe1 C41' 172.3(4) . . ? C1 Fe1 C41' 98.2(4) . . ? C2 Fe1 C43' 105.9(3) . . ? C1 Fe1 C43' 154.1(2) . . ? C41' Fe1 C43' 67.0(3) . . ? C2 Fe1 C43' 105.9(3) . 4 ? C1 Fe1 C43' 154.1(2) . 4 ? C41' Fe1 C43' 67.0(3) . 4 ? C43' Fe1 C43' 40.6(3) . 4 ? C2 Fe1 C42' 135.5(2) . . ? C1 Fe1 C42' 115.9(3) . . ? C41' Fe1 C42' 40.2(2) . . ? C43' Fe1 C42' 39.3(2) . . ? C43' Fe1 C42' 67.1(3) 4 . ? C2 Fe1 C42' 135.5(2) . 4 ? C1 Fe1 C42' 115.9(3) . 4 ? C41' Fe1 C42' 40.2(2) . 4 ? C43' Fe1 C42' 67.1(3) . 4 ? C43' Fe1 C42' 39.3(2) 4 4 ? C42' Fe1 C42' 67.2(4) . 4 ? C2 Fe1 C41 100.9(4) . . ? C1 Fe1 C41 169.6(4) . . ? C41' Fe1 C41 71.4(5) . . ? C43' Fe1 C41 21.15(17) . . ? C43' Fe1 C41 21.15(17) 4 . ? C42' Fe1 C41 56.1(3) . . ? C42' Fe1 C41 56.1(3) 4 . ? C2 Fe1 C42 116.8(3) . . ? C1 Fe1 C42 136.5(3) . . ? C41' Fe1 C42 57.1(4) . . ? C43' Fe1 C42 17.6(3) . . ? C43' Fe1 C42 53.9(3) 4 . ? C42' Fe1 C42 22.7(3) . . ? C42' Fe1 C42 70.1(3) 4 . ? C41 Fe1 C42 37.5(3) . . ? C2 Fe1 C42 116.8(3) . 4 ? C1 Fe1 C42 136.5(3) . 4 ? C41' Fe1 C42 57.1(4) . 4 ? C43' Fe1 C42 53.9(3) . 4 ? C43' Fe1 C42 17.6(3) 4 4 ? C42' Fe1 C42 70.1(3) . 4 ? C42' Fe1 C42 22.7(3) 4 4 ? C41 Fe1 C42 37.5(3) . 4 ? C42 Fe1 C42 63.4(5) . 4 ? C2 Fe1 C43 154.3(2) . . ? C1 Fe1 C43 107.6(3) . . ? C41' Fe1 C43 21.3(2) . . ? C43' Fe1 C43 51.6(3) . . ? C43' Fe1 C43 66.4(3) 4 . ? C42' Fe1 C43 18.9(2) . . ? C42' Fe1 C43 53.7(3) 4 . ? C41 Fe1 C43 62.7(4) . . ? C42 Fe1 C43 38.2(3) . . ? C42 Fe1 C43 63.2(4) 4 . ? C2 Fe1 C43 154.3(2) . 4 ? C1 Fe1 C43 107.6(3) . 4 ? C41' Fe1 C43 21.3(2) . 4 ? C43' Fe1 C43 66.4(3) . 4 ? C43' Fe1 C43 51.6(3) 4 4 ? C42' Fe1 C43 53.7(3) . 4 ? C42' Fe1 C43 18.9(2) 4 4 ? C41 Fe1 C43 62.7(4) . 4 ? C42 Fe1 C43 63.2(4) . 4 ? C42 Fe1 C43 38.2(3) 4 4 ? C43 Fe1 C43 37.3(4) . 4 ? O1 C1 Fe1 178.8(6) . . ? O2 C2 Fe1 178.9(5) . . ? C32 C31 C32 115.3(14) . 4_655 ? C32 C31 K2 79.0(7) . . ? C32 C31 K2 79.0(7) 4_655 . ? C32 C31 K1 78.3(7) . . ? C32 C31 K1 78.3(7) 4_655 . ? K2 C31 K1 136.8(5) . . ? C32 C31 H31 122.4 . . ? C32 C31 H31 122.4 4_655 . ? K2 C31 H31 111.0 . . ? K1 C31 H31 112.2 . . ? C31 C32 C33 108.8(8) . . ? C31 C32 K1 77.6(7) . . ? C33 C32 K1 76.8(4) . . ? C31 C32 K2 76.9(6) . . ? C33 C32 K2 77.5(5) . . ? K1 C32 K2 135.3(3) . . ? C31 C32 H32 125.6 . . ? C33 C32 H32 125.6 . . ? K1 C32 H32 112.4 . . ? K2 C32 H32 112.3 . . ? C32 C33 C33 103.6(5) . 4_655 ? C32 C33 K1 76.2(4) . . ? C33 C33 K1 76.01(14) 4_655 . ? C32 C33 K2 75.6(4) . . ? C33 C33 K2 76.11(14) 4_655 . ? K1 C33 K2 133.8(3) . . ? C32 C33 H33 128.2 . . ? C33 C33 H33 128.2 4_655 . ? K1 C33 H33 112.9 . . ? K2 C33 H33 113.3 . . ? C32' C31' C32' 103.6(10) 4_655 . ? C32' C31' K1 77.1(5) 4_655 . ? C32' C31' K1 77.1(5) . . ? C32' C31' K2 75.5(5) 4_655 . ? C32' C31' K2 75.5(5) . . ? K1 C31' K2 134.9(4) . . ? C32' C31' H31' 128.2 4_655 . ? C32' C31' H31' 128.2 . . ? K1 C31' H31' 111.2 . . ? K2 C31' H31' 114.0 . . ? C33' C32' C31' 104.6(7) . . ? C33' C32' K2 77.3(5) . . ? C31' C32' K2 76.1(5) . . ? C33' C32' K1 76.5(5) . . ? C31' C32' K1 74.6(5) . . ? K2 C32' K1 133.8(2) . . ? C33' C32' H32' 127.7 . . ? C31' C32' H32' 127.7 . . ? K2 C32' H32' 112.1 . . ? K1 C32' H32' 114.1 . . ? C33' C33' C32' 113.5(5) 4_655 . ? C33' C33' K2 78.15(17) 4_655 . ? C32' C33' K2 76.5(5) . . ? C33' C33' K1 78.22(17) 4_655 . ? C32' C33' K1 77.6(5) . . ? K2 C33' K1 133.9(3) . . ? C33' C33' H33' 123.2 4_655 . ? C32' C33' H33' 123.2 . . ? K2 C33' H33' 113.6 . . ? K1 C33' H33' 112.5 . . ? C42 C41 C42 110.0(8) 4 . ? C42 C41 Fe1 71.4(6) 4 . ? C42 C41 Fe1 71.4(6) . . ? C42 C41 H41 125.0 4 . ? C42 C41 H41 125.0 . . ? Fe1 C41 H41 123.9 . . ? C41 C42 C43 106.8(5) . . ? C41 C42 Fe1 71.2(6) . . ? C43 C42 Fe1 71.2(6) . . ? C41 C42 H42 126.6 . . ? C43 C42 H42 126.6 . . ? Fe1 C42 H42 122.7 . . ? C43 C43 C42 108.2(3) 4 . ? C43 C43 Fe1 71.37(19) 4 . ? C42 C43 Fe1 70.6(6) . . ? C43 C43 H43 125.9 4 . ? C42 C43 H43 125.9 . . ? Fe1 C43 H43 123.8 . . ? C42' C41' C42' 108.4(7) . 4 ? C42' C41' Fe1 71.0(5) . . ? C42' C41' Fe1 71.0(5) 4 . ? C42' C41' H41' 125.8 . . ? C42' C41' H41' 125.8 4 . ? Fe1 C41' H41' 123.9 . . ? C43' C42' C41' 107.7(5) . . ? C43' C42' Fe1 69.8(4) . . ? C41' C42' Fe1 68.9(5) . . ? C43' C42' H42' 126.2 . . ? C41' C42' H42' 126.2 . . ? Fe1 C42' H42' 126.7 . . ? C42' C43' C43' 108.1(3) . 4 ? C42' C43' Fe1 70.8(4) . . ? C43' C43' Fe1 69.72(16) 4 . ? C42' C43' H43' 125.9 . . ? C43' C43' H43' 125.9 4 . ? Fe1 C43' H43' 125.1 . . ? C52 C51 C52 125.7(12) . 4 ? C52 C51 H51 117.2 . . ? C52 C51 H51 117.2 4 . ? C51 C52 C53 116.7(7) . . ? C51 C52 H52 121.6 . . ? C53 C52 H52 121.6 . . ? C54 C53 C52 118.7(8) . . ? C54 C53 H53 120.6 . . ? C52 C53 H53 120.6 . . ? C53 C54 C53 123.4(13) 4 . ? C53 C54 H54 118.3 4 . ? C53 C54 H54 118.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O17 K1 O11 C12 140.0(3) 4_655 . . . ? O17 K1 O11 C12 -0.9(4) . . . . ? O14 K1 O11 C12 -4.6(3) . . . . ? O14 K1 O11 C12 143.6(4) 4_655 . . . ? O20 K1 O11 C12 69.5(3) . . . . ? C31 K1 O11 C12 -110.5(3) . . . . ? C32 K1 O11 C12 -88.3(4) 4_655 . . . ? C32 K1 O11 C12 -132.6(4) . . . . ? C31' K1 O11 C12 -110.5(3) . . . . ? C33 K1 O11 C12 -124.5(4) . . . . ? C33 K1 O11 C12 -96.4(4) 4_655 . . . ? O17 K1 O11 C12 0.9(4) 4_655 . . 4_655 ? O17 K1 O11 C12 -140.0(3) . . . 4_655 ? O14 K1 O11 C12 -143.6(4) . . . 4_655 ? O14 K1 O11 C12 4.6(3) 4_655 . . 4_655 ? O20 K1 O11 C12 -69.5(3) . . . 4_655 ? C31 K1 O11 C12 110.5(3) . . . 4_655 ? C32 K1 O11 C12 132.6(4) 4_655 . . 4_655 ? C32 K1 O11 C12 88.4(4) . . . 4_655 ? C31' K1 O11 C12 110.5(3) . . . 4_655 ? C33 K1 O11 C12 96.4(4) . . . 4_655 ? C33 K1 O11 C12 124.5(4) 4_655 . . 4_655 ? C12 O11 C12 C13 177.0(3) 4_655 . . . ? K1 O11 C12 C13 35.5(5) . . . . ? O11 C12 C13 O14 -64.9(6) . . . . ? C12 C13 O14 C15 -177.9(4) . . . . ? C12 C13 O14 K1 60.6(5) . . . . ? O17 K1 O14 C13 -116.9(3) 4_655 . . . ? O17 K1 O14 C13 155.0(3) . . . . ? O11 K1 O14 C13 -28.9(3) . . . . ? O14 K1 O14 C13 -57.3(4) 4_655 . . . ? O20 K1 O14 C13 -177.6(3) . . . . ? C31 K1 O14 C13 86.0(4) . . . . ? C32 K1 O14 C13 81.8(4) 4_655 . . . ? C32 K1 O14 C13 60.7(5) . . . . ? C31' K1 O14 C13 44.7(4) . . . . ? C33 K1 O14 C13 39.6(4) . . . . ? C33 K1 O14 C13 55.7(3) 4_655 . . . ? O17 K1 O14 C15 120.4(3) 4_655 . . . ? O17 K1 O14 C15 32.3(3) . . . . ? O11 K1 O14 C15 -151.6(3) . . . . ? O14 K1 O14 C15 -180.0(2) 4_655 . . . ? O20 K1 O14 C15 59.7(3) . . . . ? C31 K1 O14 C15 -36.7(4) . . . . ? C32 K1 O14 C15 -40.9(4) 4_655 . . . ? C32 K1 O14 C15 -62.0(5) . . . . ? C31' K1 O14 C15 -78.0(3) . . . . ? C33 K1 O14 C15 -83.1(3) . . . . ? C33 K1 O14 C15 -67.0(3) 4_655 . . . ? C13 O14 C15 C16 174.6(4) . . . . ? K1 O14 C15 C16 -62.9(4) . . . . ? O14 C15 C16 O17 62.5(4) . . . . ? C15 C16 O17 C18 176.5(4) . . . . ? C15 C16 O17 K1 -30.3(4) . . . . ? O17 K1 O17 C16 -144.4(3) 4_655 . . . ? O11 K1 O17 C16 -3.6(3) . . . . ? O14 K1 O17 C16 0.0(3) . . . . ? O14 K1 O17 C16 -74.1(4) 4_655 . . . ? O20 K1 O17 C16 -149.2(3) . . . . ? C31 K1 O17 C16 125.7(4) . . . . ? C32 K1 O17 C16 104.1(4) 4_655 . . . ? C32 K1 O17 C16 126.4(4) . . . . ? C31' K1 O17 C16 86.3(4) . . . . ? C33 K1 O17 C16 97.1(4) . . . . ? C33 K1 O17 C16 84.0(3) 4_655 . . . ? O17 K1 O17 C18 6.4(4) 4_655 . . . ? O11 K1 O17 C18 147.2(3) . . . . ? O14 K1 O17 C18 150.9(4) . . . . ? O14 K1 O17 C18 76.7(4) 4_655 . . . ? O20 K1 O17 C18 1.6(3) . . . . ? C31 K1 O17 C18 -83.5(4) . . . . ? C32 K1 O17 C18 -105.1(4) 4_655 . . . ? C32 K1 O17 C18 -82.8(4) . . . . ? C31' K1 O17 C18 -122.9(4) . . . . ? C33 K1 O17 C18 -112.1(4) . . . . ? C33 K1 O17 C18 -125.2(4) 4_655 . . . ? C16 O17 C18 C19 -177.2(4) . . . . ? K1 O17 C18 C19 29.4(5) . . . . ? O17 C18 C19 O20 -64.8(5) . . . . ? C18 C19 O20 C19 179.8(3) . . . 4_655 ? C18 C19 O20 K1 64.7(4) . . . . ? O17 K1 O20 C19 151.3(3) 4_655 . . . ? O17 K1 O20 C19 -33.8(3) . . . . ? O11 K1 O20 C19 -121.3(3) . . . . ? O14 K1 O20 C19 -61.1(3) . . . . ? O14 K1 O20 C19 178.6(3) 4_655 . . . ? C31 K1 O20 C19 58.7(3) . . . . ? C32 K1 O20 C19 37.9(3) 4_655 . . . ? C32 K1 O20 C19 79.6(3) . . . . ? C31' K1 O20 C19 58.7(3) . . . . ? C33 K1 O20 C19 75.9(3) . . . . ? C33 K1 O20 C19 41.6(3) 4_655 . . . ? O17 K1 O20 C19 33.8(3) 4_655 . . 4_655 ? O17 K1 O20 C19 -151.3(3) . . . 4_655 ? O11 K1 O20 C19 121.3(3) . . . 4_655 ? O14 K1 O20 C19 -178.6(3) . . . 4_655 ? O14 K1 O20 C19 61.1(3) 4_655 . . 4_655 ? C31 K1 O20 C19 -58.7(3) . . . 4_655 ? C32 K1 O20 C19 -79.6(3) 4_655 . . 4_655 ? C32 K1 O20 C19 -37.9(3) . . . 4_655 ? C31' K1 O20 C19 -58.7(3) . . . 4_655 ? C33 K1 O20 C19 -41.6(3) . . . 4_655 ? C33 K1 O20 C19 -75.9(3) 4_655 . . 4_655 ? O27 K2 O21 C22 -142.5(3) 4_655 . . . ? O27 K2 O21 C22 0.8(4) . . . . ? O24 K2 O21 C22 4.5(3) . . . . ? O24 K2 O21 C22 -146.2(4) 4_655 . . . ? O30 K2 O21 C22 -70.9(3) . . . . ? C31 K2 O21 C22 109.1(3) . . . . ? C32' K2 O21 C22 133.0(4) 4_655 . . . ? C32' K2 O21 C22 85.3(4) . . . . ? C32 K2 O21 C22 88.5(4) . . . . ? C32 K2 O21 C22 129.8(4) 4_655 . . . ? C31' K2 O21 C22 109.1(3) . . . . ? O27 K2 O21 C22 -0.8(4) 4_655 . . 4_655 ? O27 K2 O21 C22 142.5(3) . . . 4_655 ? O24 K2 O21 C22 146.2(4) . . . 4_655 ? O24 K2 O21 C22 -4.5(3) 4_655 . . 4_655 ? O30 K2 O21 C22 70.9(3) . . . 4_655 ? C31 K2 O21 C22 -109.1(3) . . . 4_655 ? C32' K2 O21 C22 -85.3(4) 4_655 . . 4_655 ? C32' K2 O21 C22 -133.0(4) . . . 4_655 ? C32 K2 O21 C22 -129.8(4) . . . 4_655 ? C32 K2 O21 C22 -88.5(4) 4_655 . . 4_655 ? C31' K2 O21 C22 -109.1(3) . . . 4_655 ? C22 O21 C22 C23 179.3(3) 4_655 . . . ? K2 O21 C22 C23 -36.4(5) . . . . ? O21 C22 C23 O24 67.3(6) . . . . ? C22 C23 O24 C25 176.4(4) . . . . ? C22 C23 O24 K2 -63.0(4) . . . . ? O27 K2 O24 C23 116.3(3) 4_655 . . . ? O27 K2 O24 C23 -154.2(3) . . . . ? O21 K2 O24 C23 29.8(3) . . . . ? O24 K2 O24 C23 56.1(3) 4_655 . . . ? O30 K2 O24 C23 177.4(3) . . . . ? C31 K2 O24 C23 -45.3(4) . . . . ? C32' K2 O24 C23 -54.9(4) 4_655 . . . ? C32' K2 O24 C23 -79.3(3) . . . . ? C32 K2 O24 C23 -67.0(4) . . . . ? C32 K2 O24 C23 -43.6(4) 4_655 . . . ? C31' K2 O24 C23 -86.6(4) . . . . ? O27 K2 O24 C25 -120.8(3) 4_655 . . . ? O27 K2 O24 C25 -31.3(2) . . . . ? O21 K2 O24 C25 152.7(3) . . . . ? O24 K2 O24 C25 179.0(2) 4_655 . . . ? O30 K2 O24 C25 -59.7(3) . . . . ? C31 K2 O24 C25 77.6(3) . . . . ? C32' K2 O24 C25 68.0(4) 4_655 . . . ? C32' K2 O24 C25 43.6(3) . . . . ? C32 K2 O24 C25 55.9(4) . . . . ? C32 K2 O24 C25 79.3(3) 4_655 . . . ? C31' K2 O24 C25 36.3(4) . . . . ? C23 O24 C25 C26 -176.6(4) . . . . ? K2 O24 C25 C26 62.6(4) . . . . ? O24 C25 C26 O27 -63.7(5) . . . . ? C25 C26 O27 C28 179.4(4) . . . . ? C25 C26 O27 K2 31.6(4) . . . . ? O27 K2 O27 C26 145.6(3) 4_655 . . . ? O21 K2 O27 C26 2.9(3) . . . . ? O24 K2 O27 C26 -0.8(3) . . . . ? O24 K2 O27 C26 73.1(4) 4_655 . . . ? O30 K2 O27 C26 147.5(3) . . . . ? C31 K2 O27 C26 -87.4(4) . . . . ? C32' K2 O27 C26 -124.4(3) 4_655 . . . ? C32' K2 O27 C26 -100.1(3) . . . . ? C32 K2 O27 C26 -89.9(4) . . . . ? C32 K2 O27 C26 -110.8(4) 4_655 . . . ? C31' K2 O27 C26 -126.8(3) . . . . ? O27 K2 O27 C28 0.2(4) 4_655 . . . ? O21 K2 O27 C28 -142.5(3) . . . . ? O24 K2 O27 C28 -146.2(3) . . . . ? O24 K2 O27 C28 -72.3(4) 4_655 . . . ? O30 K2 O27 C28 2.1(3) . . . . ? C31 K2 O27 C28 127.2(4) . . . . ? C32' K2 O27 C28 90.2(4) 4_655 . . . ? C32' K2 O27 C28 114.5(3) . . . . ? C32 K2 O27 C28 124.7(4) . . . . ? C32 K2 O27 C28 103.8(4) 4_655 . . . ? C31' K2 O27 C28 87.8(3) . . . . ? C26 O27 C28 C29 178.7(4) . . . . ? K2 O27 C28 C29 -33.2(5) . . . . ? O27 C28 C29 O30 65.6(5) . . . . ? C28 C29 O30 C29 179.0(3) . . . 4_655 ? C28 C29 O30 K2 -62.6(4) . . . . ? O27 K2 O30 C29 -151.6(3) 4_655 . . . ? O27 K2 O30 C29 30.4(3) . . . . ? O21 K2 O30 C29 119.4(3) . . . . ? O24 K2 O30 C29 58.6(3) . . . . ? O24 K2 O30 C29 -179.8(3) 4_655 . . . ? C31 K2 O30 C29 -60.6(3) . . . . ? C32' K2 O30 C29 -83.9(3) 4_655 . . . ? C32' K2 O30 C29 -37.3(3) . . . . ? C32 K2 O30 C29 -37.8(3) . . . . ? C32 K2 O30 C29 -83.5(3) 4_655 . . . ? C31' K2 O30 C29 -60.6(3) . . . . ? O27 K2 O30 C29 -30.4(3) 4_655 . . 4_655 ? O27 K2 O30 C29 151.6(3) . . . 4_655 ? O21 K2 O30 C29 -119.4(3) . . . 4_655 ? O24 K2 O30 C29 179.8(3) . . . 4_655 ? O24 K2 O30 C29 -58.6(3) 4_655 . . 4_655 ? C31 K2 O30 C29 60.6(3) . . . 4_655 ? C32' K2 O30 C29 37.3(3) 4_655 . . 4_655 ? C32' K2 O30 C29 83.9(3) . . . 4_655 ? C32 K2 O30 C29 83.5(3) . . . 4_655 ? C32 K2 O30 C29 37.8(3) 4_655 . . 4_655 ? C31' K2 O30 C29 60.6(3) . . . 4_655 ? C2 Fe1 C1 O1 0.00(10) . . . . ? C41' Fe1 C1 O1 180.00(10) . . . . ? C43' Fe1 C1 O1 127.5(6) . . . . ? C43' Fe1 C1 O1 -127.5(6) 4 . . . ? C42' Fe1 C1 O1 142.0(2) . . . . ? C42' Fe1 C1 O1 -142.0(2) 4 . . . ? C41 Fe1 C1 O1 180.00(9) . . . . ? C42 Fe1 C1 O1 130.2(5) . . . . ? C42 Fe1 C1 O1 -130.2(5) 4 . . . ? C43 Fe1 C1 O1 160.4(2) . . . . ? C43 Fe1 C1 O1 -160.4(2) 4 . . . ? C1 Fe1 C2 O2 0.00(8) . . . . ? C41' Fe1 C2 O2 180.00(7) . . . . ? C43' Fe1 C2 O2 -158.87(19) . . . . ? C43' Fe1 C2 O2 158.87(17) 4 . . . ? C42' Fe1 C2 O2 -127.9(3) . . . . ? C42' Fe1 C2 O2 127.9(3) 4 . . . ? C41 Fe1 C2 O2 180.00(8) . . . . ? C42 Fe1 C2 O2 -143.9(3) . . . . ? C42 Fe1 C2 O2 143.9(3) 4 . . . ? C43 Fe1 C2 O2 -132.6(6) . . . . ? C43 Fe1 C2 O2 132.6(6) 4 . . . ? O27 K2 C31 C32 124.8(6) 4_655 . . . ? O27 K2 C31 C32 -6.1(7) . . . . ? O21 K2 C31 C32 -120.6(7) . . . . ? O24 K2 C31 C32 -64.7(7) . . . . ? O24 K2 C31 C32 -176.5(7) 4_655 . . . ? O30 K2 C31 C32 59.4(7) . . . . ? C32' K2 C31 C32 102.5(10) 4_655 . . . ? C32' K2 C31 C32 16.3(5) . . . . ? C32 K2 C31 C32 118.8(14) 4_655 . . . ? C31' K2 C31 C32 59.4(7) . . . . ? O27 K2 C31 C32 6.1(7) 4_655 . . 4_655 ? O27 K2 C31 C32 -124.8(6) . . . 4_655 ? O21 K2 C31 C32 120.6(7) . . . 4_655 ? O24 K2 C31 C32 176.5(7) . . . 4_655 ? O24 K2 C31 C32 64.7(7) 4_655 . . 4_655 ? O30 K2 C31 C32 -59.4(7) . . . 4_655 ? C32' K2 C31 C32 -16.3(5) 4_655 . . 4_655 ? C32' K2 C31 C32 -102.5(10) . . . 4_655 ? C32 K2 C31 C32 -118.8(14) . . . 4_655 ? C31' K2 C31 C32 -59.4(7) . . . 4_655 ? O27 K2 C31 K1 65.45(11) 4_655 . . . ? O27 K2 C31 K1 -65.45(11) . . . . ? O21 K2 C31 K1 180.000(1) . . . . ? O24 K2 C31 K1 -124.07(7) . . . . ? O24 K2 C31 K1 124.07(7) 4_655 . . . ? O30 K2 C31 K1 0.000(2) . . . . ? C32' K2 C31 K1 43.1(4) 4_655 . . . ? C32' K2 C31 K1 -43.1(4) . . . . ? C32 K2 C31 K1 -59.4(7) . . . . ? C32 K2 C31 K1 59.4(7) 4_655 . . . ? C31' K2 C31 K1 0.000(2) . . . . ? O17 K1 C31 C32 62.3(7) 4_655 . . . ? O17 K1 C31 C32 178.5(7) . . . . ? O11 K1 C31 C32 -59.6(7) . . . . ? O14 K1 C31 C32 -129.4(6) . . . . ? O14 K1 C31 C32 10.2(8) 4_655 . . . ? O20 K1 C31 C32 120.4(7) . . . . ? C32 K1 C31 C32 -119.2(14) 4_655 . . . ? C31' K1 C31 C32 -59.6(7) . . . . ? C33 K1 C31 C32 -38.5(6) . . . . ? C33 K1 C31 C32 -80.7(8) 4_655 . . . ? O17 K1 C31 C32 -178.5(7) 4_655 . . 4_655 ? O17 K1 C31 C32 -62.3(7) . . . 4_655 ? O11 K1 C31 C32 59.6(7) . . . 4_655 ? O14 K1 C31 C32 -10.2(8) . . . 4_655 ? O14 K1 C31 C32 129.4(6) 4_655 . . 4_655 ? O20 K1 C31 C32 -120.4(7) . . . 4_655 ? C32 K1 C31 C32 119.2(14) . . . 4_655 ? C31' K1 C31 C32 59.6(7) . . . 4_655 ? C33 K1 C31 C32 80.7(8) . . . 4_655 ? C33 K1 C31 C32 38.5(6) 4_655 . . 4_655 ? O17 K1 C31 K2 121.92(6) 4_655 . . . ? O17 K1 C31 K2 -121.92(6) . . . . ? O11 K1 C31 K2 0.000(3) . . . . ? O14 K1 C31 K2 -69.83(16) . . . . ? O14 K1 C31 K2 69.83(16) 4_655 . . . ? O20 K1 C31 K2 180.000(2) . . . . ? C32 K1 C31 K2 -59.6(7) 4_655 . . . ? C32 K1 C31 K2 59.6(7) . . . . ? C31' K1 C31 K2 0.000(1) . . . . ? C33 K1 C31 K2 21.1(2) . . . . ? C33 K1 C31 K2 -21.1(2) 4_655 . . . ? C32 C31 C32 C33 0.3(14) 4_655 . . . ? K2 C31 C32 C33 -71.8(6) . . . . ? K1 C31 C32 C33 71.2(6) . . . . ? C32 C31 C32 K1 -70.9(10) 4_655 . . . ? K2 C31 C32 K1 -143.0(3) . . . . ? C32 C31 C32 K2 72.1(10) 4_655 . . . ? K1 C31 C32 K2 143.0(3) . . . . ? O17 K1 C32 C31 -115.6(7) 4_655 . . . ? O17 K1 C32 C31 -1.7(7) . . . . ? O11 K1 C32 C31 130.9(7) . . . . ? O14 K1 C32 C31 65.7(8) . . . . ? O14 K1 C32 C31 -171.1(7) 4_655 . . . ? O20 K1 C32 C31 -60.3(7) . . . . ? C32 K1 C32 C31 32.7(7) 4_655 . . . ? C31' K1 C32 C31 92.7(7) . . . . ? C33 K1 C32 C31 113.0(8) . . . . ? C33 K1 C32 C31 72.9(7) 4_655 . . . ? O17 K1 C32 C33 131.5(5) 4_655 . . . ? O17 K1 C32 C33 -114.6(5) . . . . ? O11 K1 C32 C33 17.9(6) . . . . ? O14 K1 C32 C33 -47.2(7) . . . . ? O14 K1 C32 C33 76.0(5) 4_655 . . . ? O20 K1 C32 C33 -173.3(5) . . . . ? C31 K1 C32 C33 -113.0(8) . . . . ? C32 K1 C32 C33 -80.2(5) 4_655 . . . ? C31' K1 C32 C33 -20.3(4) . . . . ? C33 K1 C32 C33 -40.0(5) 4_655 . . . ? O17 K1 C32 K2 -172.0(7) 4_655 . . . ? O17 K1 C32 K2 -58.1(7) . . . . ? O11 K1 C32 K2 74.4(7) . . . . ? O14 K1 C32 K2 9.3(9) . . . . ? O14 K1 C32 K2 132.5(6) 4_655 . . . ? O20 K1 C32 K2 -116.7(6) . . . . ? C31 K1 C32 K2 -56.4(6) . . . . ? C32 K1 C32 K2 -23.7(7) 4_655 . . . ? C31' K1 C32 K2 36.2(5) . . . . ? C33 K1 C32 K2 56.5(5) . . . . ? C33 K1 C32 K2 16.5(5) 4_655 . . . ? O27 K2 C32 C31 -65.6(8) 4_655 . . . ? O27 K2 C32 C31 174.3(7) . . . . ? O21 K2 C32 C31 58.6(7) . . . . ? O24 K2 C32 C31 116.3(7) . . . . ? O24 K2 C32 C31 4.0(8) 4_655 . . . ? O30 K2 C32 C31 -133.1(7) . . . . ? C32' K2 C32 C31 -50.9(7) 4_655 . . . ? C32' K2 C32 C31 -135.1(14) . . . . ? C32 K2 C32 C31 -33.0(7) 4_655 . . . ? C31' K2 C32 C31 -92.9(7) . . . . ? O27 K2 C32 C33 47.3(6) 4_655 . . . ? O27 K2 C32 C33 -72.8(5) . . . . ? O21 K2 C32 C33 171.6(5) . . . . ? O24 K2 C32 C33 -130.8(5) . . . . ? O24 K2 C32 C33 117.0(5) 4_655 . . . ? O30 K2 C32 C33 -20.1(6) . . . . ? C31 K2 C32 C33 112.9(8) . . . . ? C32' K2 C32 C33 62.0(5) 4_655 . . . ? C32' K2 C32 C33 -22.2(9) . . . . ? C32 K2 C32 C33 80.0(6) 4_655 . . . ? C31' K2 C32 C33 20.0(4) . . . . ? O27 K2 C32 K1 -9.0(8) 4_655 . . . ? O27 K2 C32 K1 -129.0(6) . . . . ? O21 K2 C32 K1 115.3(6) . . . . ? O24 K2 C32 K1 172.9(6) . . . . ? O24 K2 C32 K1 60.7(7) 4_655 . . . ? O30 K2 C32 K1 -76.4(7) . . . . ? C31 K2 C32 K1 56.7(7) . . . . ? C32' K2 C32 K1 5.8(6) 4_655 . . . ? C32' K2 C32 K1 -78.4(11) . . . . ? C32 K2 C32 K1 23.7(7) 4_655 . . . ? C31' K2 C32 K1 -36.3(5) . . . . ? C31 C32 C33 C33 -0.2(8) . . . 4_655 ? K1 C32 C33 C33 71.59(17) . . . 4_655 ? K2 C32 C33 C33 -71.49(16) . . . 4_655 ? C31 C32 C33 K1 -71.7(7) . . . . ? K2 C32 C33 K1 -143.1(2) . . . . ? C31 C32 C33 K2 71.3(7) . . . . ? K1 C32 C33 K2 143.1(2) . . . . ? O17 K1 C33 C32 -47.8(5) 4_655 . . . ? O17 K1 C33 C32 79.5(6) . . . . ? O11 K1 C33 C32 -163.2(5) . . . . ? O14 K1 C33 C32 144.3(5) . . . . ? O14 K1 C33 C32 -105.1(5) 4_655 . . . ? O20 K1 C33 C32 8.1(6) . . . . ? C31 K1 C33 C32 34.1(5) . . . . ? C32 K1 C33 C32 69.6(8) 4_655 . . . ? C31' K1 C33 C32 123.8(13) . . . . ? C33 K1 C33 C32 108.1(5) 4_655 . . . ? O17 K1 C33 C33 -155.95(9) 4_655 . . 4_655 ? O17 K1 C33 C33 -28.61(10) . . . 4_655 ? O11 K1 C33 C33 88.69(5) . . . 4_655 ? O14 K1 C33 C33 36.16(7) . . . 4_655 ? O14 K1 C33 C33 146.82(7) 4_655 . . 4_655 ? O20 K1 C33 C33 -99.97(11) . . . 4_655 ? C31 K1 C33 C33 -74.1(2) . . . 4_655 ? C32 K1 C33 C33 -38.5(4) 4_655 . . 4_655 ? C32 K1 C33 C33 -108.1(5) . . . 4_655 ? C31' K1 C33 C33 15.6(11) . . . 4_655 ? O17 K1 C33 K2 -101.5(3) 4_655 . . . ? O17 K1 C33 K2 25.8(4) . . . . ? O11 K1 C33 K2 143.1(4) . . . . ? O14 K1 C33 K2 90.6(4) . . . . ? O14 K1 C33 K2 -158.7(4) 4_655 . . . ? O20 K1 C33 K2 -45.5(4) . . . . ? C31 K1 C33 K2 -19.6(2) . . . . ? C32 K1 C33 K2 15.9(4) 4_655 . . . ? C32 K1 C33 K2 -53.7(5) . . . . ? C31' K1 C33 K2 70.1(11) . . . . ? C33 K1 C33 K2 54.4(4) 4_655 . . . ? O27 K2 C33 C32 -140.5(5) 4_655 . . . ? O27 K2 C33 C32 103.7(5) . . . . ? O21 K2 C33 C32 -9.8(6) . . . . ? O24 K2 C33 C32 51.4(5) . . . . ? O24 K2 C33 C32 -82.2(6) 4_655 . . . ? O30 K2 C33 C32 161.8(5) . . . . ? C31 K2 C33 C32 -34.2(5) . . . . ? C32' K2 C33 C32 -88.2(7) 4_655 . . . ? C32' K2 C33 C32 18.3(8) . . . . ? C32 K2 C33 C32 -69.8(8) 4_655 . . . ? C31' K2 C33 C32 -124.6(13) . . . . ? O27 K2 C33 C33 -32.17(7) 4_655 . . 4_655 ? O27 K2 C33 C33 -148.00(7) . . . 4_655 ? O21 K2 C33 C33 98.48(10) . . . 4_655 ? O24 K2 C33 C33 159.65(10) . . . 4_655 ? O24 K2 C33 C33 26.14(13) 4_655 . . 4_655 ? O30 K2 C33 C33 -89.89(4) . . . 4_655 ? C31 K2 C33 C33 74.1(2) . . . 4_655 ? C32' K2 C33 C33 20.1(3) 4_655 . . 4_655 ? C32' K2 C33 C33 126.6(8) . . . 4_655 ? C32 K2 C33 C33 108.3(5) . . . 4_655 ? C32 K2 C33 C33 38.4(4) 4_655 . . 4_655 ? C31' K2 C33 C33 -16.3(11) . . . 4_655 ? O27 K2 C33 K1 -86.6(4) 4_655 . . . ? O27 K2 C33 K1 157.6(4) . . . . ? O21 K2 C33 K1 44.1(4) . . . . ? O24 K2 C33 K1 105.2(3) . . . . ? O24 K2 C33 K1 -28.3(5) 4_655 . . . ? O30 K2 C33 K1 -144.3(3) . . . . ? C31 K2 C33 K1 19.7(2) . . . . ? C32' K2 C33 K1 -34.3(4) 4_655 . . . ? C32' K2 C33 K1 72.2(8) . . . . ? C32 K2 C33 K1 53.9(5) . . . . ? C32 K2 C33 K1 -16.0(5) 4_655 . . . ? C31' K2 C33 K1 -70.7(11) . . . . ? O17 K1 C31' C32' -119.6(4) 4_655 . . 4_655 ? O17 K1 C31' C32' 12.1(5) . . . 4_655 ? O11 K1 C31' C32' 126.3(5) . . . 4_655 ? O14 K1 C31' C32' 70.6(5) . . . 4_655 ? O14 K1 C31' C32' -178.1(4) 4_655 . . 4_655 ? O20 K1 C31' C32' -53.7(5) . . . 4_655 ? C31 K1 C31' C32' -53.7(5) . . . 4_655 ? C32 K1 C31' C32' -17.8(4) 4_655 . . 4_655 ? C32 K1 C31' C32' -89.6(7) . . . 4_655 ? C33 K1 C31' C32' -128.6(14) . . . 4_655 ? C33 K1 C31' C32' 21.1(9) 4_655 . . 4_655 ? O17 K1 C31' C32' -12.1(5) 4_655 . . . ? O17 K1 C31' C32' 119.6(4) . . . . ? O11 K1 C31' C32' -126.3(5) . . . . ? O14 K1 C31' C32' 178.1(4) . . . . ? O14 K1 C31' C32' -70.6(5) 4_655 . . . ? O20 K1 C31' C32' 53.7(5) . . . . ? C31 K1 C31' C32' 53.7(5) . . . . ? C32 K1 C31' C32' 89.6(7) 4_655 . . . ? C32 K1 C31' C32' 17.8(4) . . . . ? C33 K1 C31' C32' -21.1(9) . . . . ? C33 K1 C31' C32' 128.6(14) 4_655 . . . ? O17 K1 C31' K2 -65.86(11) 4_655 . . . ? O17 K1 C31' K2 65.86(11) . . . . ? O11 K1 C31' K2 180.000(3) . . . . ? O14 K1 C31' K2 124.34(6) . . . . ? O14 K1 C31' K2 -124.34(6) 4_655 . . . ? O20 K1 C31' K2 0.000(3) . . . . ? C31 K1 C31' K2 0.000(1) . . . . ? C32 K1 C31' K2 35.9(4) 4_655 . . . ? C32 K1 C31' K2 -35.9(4) . . . . ? C33 K1 C31' K2 -74.8(11) . . . . ? C33 K1 C31' K2 74.8(11) 4_655 . . . ? O27 K2 C31' C32' -67.0(5) 4_655 . . 4_655 ? O27 K2 C31' C32' 175.6(5) . . . 4_655 ? O21 K2 C31' C32' 54.3(5) . . . 4_655 ? O24 K2 C31' C32' 124.0(4) . . . 4_655 ? O24 K2 C31' C32' -15.4(6) 4_655 . . 4_655 ? O30 K2 C31' C32' -125.7(5) . . . 4_655 ? C31 K2 C31' C32' 54.3(5) . . . 4_655 ? C32' K2 C31' C32' 108.6(9) . . . 4_655 ? C32 K2 C31' C32' 90.1(8) . . . 4_655 ? C32 K2 C31' C32' 18.4(4) 4_655 . . 4_655 ? O27 K2 C31' C32' -175.6(5) 4_655 . . . ? O27 K2 C31' C32' 67.0(5) . . . . ? O21 K2 C31' C32' -54.3(5) . . . . ? O24 K2 C31' C32' 15.4(6) . . . . ? O24 K2 C31' C32' -124.0(4) 4_655 . . . ? O30 K2 C31' C32' 125.7(5) . . . . ? C31 K2 C31' C32' -54.3(5) . . . . ? C32' K2 C31' C32' -108.6(9) 4_655 . . . ? C32 K2 C31' C32' -18.4(4) . . . . ? C32 K2 C31' C32' -90.1(8) 4_655 . . . ? O27 K2 C31' K1 -121.30(6) 4_655 . . . ? O27 K2 C31' K1 121.30(6) . . . . ? O21 K2 C31' K1 0.000(3) . . . . ? O24 K2 C31' K1 69.71(14) . . . . ? O24 K2 C31' K1 -69.71(14) 4_655 . . . ? O30 K2 C31' K1 180.000(1) . . . . ? C31 K2 C31' K1 0.000(2) . . . . ? C32' K2 C31' K1 -54.3(5) 4_655 . . . ? C32' K2 C31' K1 54.3(5) . . . . ? C32 K2 C31' K1 35.9(4) . . . . ? C32 K2 C31' K1 -35.9(4) 4_655 . . . ? C32' C31' C32' C33' 1.9(11) 4_655 . . . ? K1 C31' C32' C33' -71.2(6) . . . . ? K2 C31' C32' C33' 72.6(5) . . . . ? C32' C31' C32' K2 -70.8(7) 4_655 . . . ? K1 C31' C32' K2 -143.8(3) . . . . ? C32' C31' C32' K1 73.1(7) 4_655 . . . ? K2 C31' C32' K1 143.8(3) . . . . ? O27 K2 C32' C33' -103.9(5) 4_655 . . . ? O27 K2 C32' C33' 141.4(5) . . . . ? O21 K2 C32' C33' 27.8(5) . . . . ? O24 K2 C32' C33' 84.6(5) . . . . ? O24 K2 C32' C33' -34.2(6) 4_655 . . . ? O30 K2 C32' C33' -164.7(5) . . . . ? C31 K2 C32' C33' -17.2(5) . . . . ? C32' K2 C32' C33' -69.5(5) 4_655 . . . ? C32 K2 C32' C33' 13.4(10) . . . . ? C32 K2 C32' C33' -51.3(6) 4_655 . . . ? C31' K2 C32' C33' -108.8(7) . . . . ? O27 K2 C32' C31' 5.0(5) 4_655 . . . ? O27 K2 C32' C31' -109.8(5) . . . . ? O21 K2 C32' C31' 136.6(5) . . . . ? O24 K2 C32' C31' -166.5(5) . . . . ? O24 K2 C32' C31' 74.6(5) 4_655 . . . ? O30 K2 C32' C31' -55.9(5) . . . . ? C31 K2 C32' C31' 91.6(6) . . . . ? C32' K2 C32' C31' 39.3(5) 4_655 . . . ? C32 K2 C32' C31' 122.3(13) . . . . ? C32 K2 C32' C31' 57.5(6) 4_655 . . . ? O27 K2 C32' K1 -47.0(5) 4_655 . . . ? O27 K2 C32' K1 -161.8(5) . . . . ? O21 K2 C32' K1 84.6(4) . . . . ? O24 K2 C32' K1 141.5(4) . . . . ? O24 K2 C32' K1 22.7(6) 4_655 . . . ? O30 K2 C32' K1 -107.8(4) . . . . ? C31 K2 C32' K1 39.6(4) . . . . ? C32' K2 C32' K1 -12.7(5) 4_655 . . . ? C32 K2 C32' K1 70.3(11) . . . . ? C32 K2 C32' K1 5.5(6) 4_655 . . . ? C31' K2 C32' K1 -52.0(5) . . . . ? O17 K1 C32' C33' -81.7(5) 4_655 . . . ? O17 K1 C32' C33' 35.5(6) . . . . ? O11 K1 C32' C33' 163.0(5) . . . . ? O14 K1 C32' C33' 107.2(5) . . . . ? O14 K1 C32' C33' -139.4(5) 4_655 . . . ? O20 K1 C32' C33' -29.1(5) . . . . ? C31 K1 C32' C33' 17.3(5) . . . . ? C32 K1 C32' C33' 51.6(6) 4_655 . . . ? C32 K1 C32' C33' -14.7(10) . . . . ? C31' K1 C32' C33' 109.6(7) . . . . ? C33 K1 C32' C33' 129.2(9) . . . . ? C33 K1 C32' C33' 91.4(5) 4_655 . . . ? O17 K1 C32' C31' 168.7(5) 4_655 . . . ? O17 K1 C32' C31' -74.1(5) . . . . ? O11 K1 C32' C31' 53.4(5) . . . . ? O14 K1 C32' C31' -2.4(5) . . . . ? O14 K1 C32' C31' 111.0(5) 4_655 . . . ? O20 K1 C32' C31' -138.7(4) . . . . ? C31 K1 C32' C31' -92.3(5) . . . . ? C32 K1 C32' C31' -58.0(6) 4_655 . . . ? C32 K1 C32' C31' -124.3(13) . . . . ? C33 K1 C32' C31' 19.6(7) . . . . ? C33 K1 C32' C31' -18.2(5) 4_655 . . . ? O17 K1 C32' K2 -138.9(4) 4_655 . . . ? O17 K1 C32' K2 -21.6(5) . . . . ? O11 K1 C32' K2 105.9(4) . . . . ? O14 K1 C32' K2 50.1(5) . . . . ? O14 K1 C32' K2 163.4(4) 4_655 . . . ? O20 K1 C32' K2 -86.2(4) . . . . ? C31 K1 C32' K2 -39.9(4) . . . . ? C32 K1 C32' K2 -5.6(6) 4_655 . . . ? C32 K1 C32' K2 -71.8(11) . . . . ? C31' K1 C32' K2 52.5(5) . . . . ? C33 K1 C32' K2 72.1(7) . . . . ? C33 K1 C32' K2 34.3(4) 4_655 . . . ? C31' C32' C33' C33' -1.3(7) . . . 4_655 ? K2 C32' C33' C33' 70.4(2) . . . 4_655 ? K1 C32' C33' C33' -71.1(2) . . . 4_655 ? C31' C32' C33' K2 -71.7(6) . . . . ? K1 C32' C33' K2 -141.5(2) . . . . ? C31' C32' C33' K1 69.8(6) . . . . ? K2 C32' C33' K1 141.5(2) . . . . ? O27 K2 C33' C33' -27.51(10) 4_655 . . 4_655 ? O27 K2 C33' C33' -156.14(9) . . . 4_655 ? O21 K2 C33' C33' 88.63(4) . . . 4_655 ? O24 K2 C33' C33' 146.56(7) . . . 4_655 ? O24 K2 C33' C33' 35.51(7) 4_655 . . 4_655 ? O30 K2 C33' C33' -99.14(13) . . . 4_655 ? C31 K2 C33' C33' 8.0(17) . . . 4_655 ? C32' K2 C33' C33' -35.3(3) 4_655 . . 4_655 ? C32' K2 C33' C33' -118.0(5) . . . 4_655 ? C32 K2 C33' C33' -130.6(10) . . . 4_655 ? C32 K2 C33' C33' -18.8(4) 4_655 . . 4_655 ? C31' K2 C33' C33' -77.4(2) . . . 4_655 ? O27 K2 C33' C32' 90.5(5) 4_655 . . . ? O27 K2 C33' C32' -38.1(5) . . . . ? O21 K2 C33' C32' -153.3(5) . . . . ? O24 K2 C33' C32' -95.4(5) . . . . ? O24 K2 C33' C32' 153.5(4) 4_655 . . . ? O30 K2 C33' C32' 18.9(6) . . . . ? C31 K2 C33' C32' 126.0(18) . . . . ? C32' K2 C33' C32' 82.8(6) 4_655 . . . ? C32 K2 C33' C32' -12.6(9) . . . . ? C32 K2 C33' C32' 99.2(6) 4_655 . . . ? C31' K2 C33' C32' 40.6(4) . . . . ? O27 K2 C33' K1 33.0(5) 4_655 . . . ? O27 K2 C33' K1 -95.6(4) . . . . ? O21 K2 C33' K1 149.2(5) . . . . ? O24 K2 C33' K1 -152.9(5) . . . . ? O24 K2 C33' K1 96.1(4) 4_655 . . . ? O30 K2 C33' K1 -38.6(6) . . . . ? C31 K2 C33' K1 68.6(16) . . . . ? C32' K2 C33' K1 25.3(4) 4_655 . . . ? C32' K2 C33' K1 -57.5(4) . . . . ? C32 K2 C33' K1 -70.1(10) . . . . ? C32 K2 C33' K1 41.7(6) 4_655 . . . ? C31' K2 C33' K1 -16.8(3) . . . . ? O17 K1 C33' C33' -147.63(7) 4_655 . . 4_655 ? O17 K1 C33' C33' -32.55(7) . . . 4_655 ? O11 K1 C33' C33' 97.59(11) . . . 4_655 ? O14 K1 C33' C33' 24.17(15) . . . 4_655 ? O14 K1 C33' C33' 160.69(11) 4_655 . . 4_655 ? O20 K1 C33' C33' -89.49(4) . . . 4_655 ? C31 K1 C33' C33' -8.3(16) . . . 4_655 ? C32 K1 C33' C33' 18.6(4) 4_655 . . 4_655 ? C32 K1 C33' C33' 131.3(11) . . . 4_655 ? C31' K1 C33' C33' 77.4(2) . . . 4_655 ? C33 K1 C33' C33' 97.7(4) . . . 4_655 ? C33 K1 C33' C33' 57.1(2) 4_655 . . 4_655 ? O17 K1 C33' C32' 94.7(5) 4_655 . . . ? O17 K1 C33' C32' -150.2(5) . . . . ? O11 K1 C33' C32' -20.0(6) . . . . ? O14 K1 C33' C32' -93.5(5) . . . . ? O14 K1 C33' C32' 43.1(5) 4_655 . . . ? O20 K1 C33' C32' 152.9(5) . . . . ? C31 K1 C33' C32' -125.9(17) . . . . ? C32 K1 C33' C32' -99.0(7) 4_655 . . . ? C32 K1 C33' C32' 13.7(10) . . . . ? C31' K1 C33' C32' -40.2(4) . . . . ? C33 K1 C33' C32' -19.9(4) . . . . ? C33 K1 C33' C32' -60.6(5) 4_655 . . . ? O17 K1 C33' K2 151.8(5) 4_655 . . . ? O17 K1 C33' K2 -93.1(5) . . . . ? O11 K1 C33' K2 37.1(5) . . . . ? O14 K1 C33' K2 -36.4(6) . . . . ? O14 K1 C33' K2 100.2(4) 4_655 . . . ? O20 K1 C33' K2 -150.0(5) . . . . ? C31 K1 C33' K2 -68.8(16) . . . . ? C32 K1 C33' K2 -41.9(6) 4_655 . . . ? C32 K1 C33' K2 70.8(10) . . . . ? C31' K1 C33' K2 16.9(3) . . . . ? C33 K1 C33' K2 37.2(3) . . . . ? C33 K1 C33' K2 -3.5(4) 4_655 . . . ? C2 Fe1 C41 C42 -120.2(5) . . . 4 ? C1 Fe1 C41 C42 59.8(5) . . . 4 ? C41' Fe1 C41 C42 59.8(5) . . . 4 ? C43' Fe1 C41 C42 133.8(13) . . . 4 ? C43' Fe1 C41 C42 -14.1(11) 4 . . 4 ? C42' Fe1 C41 C42 101.6(6) . . . 4 ? C42' Fe1 C41 C42 18.0(5) 4 . . 4 ? C42 Fe1 C41 C42 119.6(9) . . . 4 ? C43 Fe1 C41 C42 80.9(5) . . . 4 ? C43 Fe1 C41 C42 38.7(5) 4 . . 4 ? C2 Fe1 C41 C42 120.2(5) . . . . ? C1 Fe1 C41 C42 -59.8(5) . . . . ? C41' Fe1 C41 C42 -59.8(5) . . . . ? C43' Fe1 C41 C42 14.1(11) . . . . ? C43' Fe1 C41 C42 -133.8(13) 4 . . . ? C42' Fe1 C41 C42 -18.0(5) . . . . ? C42' Fe1 C41 C42 -101.6(6) 4 . . . ? C42 Fe1 C41 C42 -119.6(9) 4 . . . ? C43 Fe1 C41 C42 -38.7(5) . . . . ? C43 Fe1 C41 C42 -80.9(5) 4 . . . ? C42 C41 C42 C43 1.6(15) 4 . . . ? Fe1 C41 C42 C43 62.8(7) . . . . ? C42 C41 C42 Fe1 -61.2(10) 4 . . . ? C2 Fe1 C42 C41 -71.9(5) . . . . ? C1 Fe1 C42 C41 166.9(5) . . . . ? C41' Fe1 C42 C41 102.7(5) . . . . ? C43' Fe1 C42 C41 -16.9(12) . . . . ? C43' Fe1 C42 C41 18.8(5) 4 . . . ? C42' Fe1 C42 C41 138.2(10) . . . . ? C42' Fe1 C42 C41 59.9(5) 4 . . . ? C42 Fe1 C42 C41 36.2(5) 4 . . . ? C43 Fe1 C42 C41 116.0(6) . . . . ? C43 Fe1 C42 C41 79.2(5) 4 . . . ? C2 Fe1 C42 C43 172.1(4) . . . . ? C1 Fe1 C42 C43 51.0(6) . . . . ? C41' Fe1 C42 C43 -13.3(4) . . . . ? C43' Fe1 C42 C43 -132.9(14) . . . . ? C43' Fe1 C42 C43 -97.2(5) 4 . . . ? C42' Fe1 C42 C43 22.3(8) . . . . ? C42' Fe1 C42 C43 -56.1(4) 4 . . . ? C41 Fe1 C42 C43 -116.0(6) . . . . ? C42 Fe1 C42 C43 -79.7(4) 4 . . . ? C43 Fe1 C42 C43 -36.8(4) 4 . . . ? C41 C42 C43 C43 -0.9(9) . . . 4 ? Fe1 C42 C43 C43 61.8(3) . . . 4 ? C41 C42 C43 Fe1 -62.7(7) . . . . ? C2 Fe1 C43 C43 -134.4(6) . . . 4 ? C1 Fe1 C43 C43 96.14(13) . . . 4 ? C41' Fe1 C43 C43 30.0(11) . . . 4 ? C43' Fe1 C43 C43 -101.5(3) . . . 4 ? C43' Fe1 C43 C43 -56.9(2) 4 . . 4 ? C42' Fe1 C43 C43 -144.7(9) . . . 4 ? C42' Fe1 C43 C43 -13.5(3) 4 . . 4 ? C41 Fe1 C43 C43 -79.96(17) . . . 4 ? C42 Fe1 C43 C43 -118.0(4) . . . 4 ? C42 Fe1 C43 C43 -37.7(3) 4 . . 4 ? C2 Fe1 C43 C42 -16.4(8) . . . . ? C1 Fe1 C43 C42 -145.9(4) . . . . ? C41' Fe1 C43 C42 147.9(12) . . . . ? C43' Fe1 C43 C42 16.5(5) . . . . ? C43' Fe1 C43 C42 61.1(5) 4 . . . ? C42' Fe1 C43 C42 -26.8(10) . . . . ? C42' Fe1 C43 C42 104.5(5) 4 . . . ? C41 Fe1 C43 C42 38.0(4) . . . . ? C42 Fe1 C43 C42 80.3(6) 4 . . . ? C43 Fe1 C43 C42 118.0(4) 4 . . . ? C2 Fe1 C41' C42' 59.1(4) . . . . ? C1 Fe1 C41' C42' -120.9(4) . . . . ? C43' Fe1 C41' C42' 36.9(4) . . . . ? C43' Fe1 C41' C42' 81.2(4) 4 . . . ? C42' Fe1 C41' C42' 118.2(7) 4 . . . ? C41 Fe1 C41' C42' 59.1(4) . . . . ? C42 Fe1 C41' C42' 20.3(4) . . . . ? C42 Fe1 C41' C42' 97.8(5) 4 . . . ? C43 Fe1 C41' C42' -2.7(9) . . . . ? C43 Fe1 C41' C42' 120.8(12) 4 . . . ? C2 Fe1 C41' C42' -59.1(4) . . . 4 ? C1 Fe1 C41' C42' 120.9(4) . . . 4 ? C43' Fe1 C41' C42' -81.2(4) . . . 4 ? C43' Fe1 C41' C42' -36.9(4) 4 . . 4 ? C42' Fe1 C41' C42' -118.2(7) . . . 4 ? C41 Fe1 C41' C42' -59.1(4) . . . 4 ? C42 Fe1 C41' C42' -97.8(5) . . . 4 ? C42 Fe1 C41' C42' -20.3(4) 4 . . 4 ? C43 Fe1 C41' C42' -120.8(12) . . . 4 ? C43 Fe1 C41' C42' 2.7(9) 4 . . 4 ? C42' C41' C42' C43' 2.2(11) 4 . . . ? Fe1 C41' C42' C43' -59.3(5) . . . . ? C42' C41' C42' Fe1 61.4(7) 4 . . . ? C2 Fe1 C42' C43' -51.4(5) . . . . ? C1 Fe1 C42' C43' -170.0(3) . . . . ? C41' Fe1 C42' C43' 119.2(5) . . . . ? C43' Fe1 C42' C43' 38.3(3) 4 . . . ? C42' Fe1 C42' C43' 81.1(4) 4 . . . ? C41 Fe1 C42' C43' 17.6(4) . . . . ? C42 Fe1 C42' C43' -11.6(9) . . . . ? C42 Fe1 C42' C43' 57.0(4) 4 . . . ? C43 Fe1 C42' C43' 122.2(11) . . . . ? C43 Fe1 C42' C43' 96.5(5) 4 . . . ? C2 Fe1 C42' C41' -170.6(5) . . . . ? C1 Fe1 C42' C41' 70.7(4) . . . . ? C43' Fe1 C42' C41' -119.2(5) . . . . ? C43' Fe1 C42' C41' -80.9(4) 4 . . . ? C42' Fe1 C42' C41' -38.1(4) 4 . . . ? C41 Fe1 C42' C41' -101.6(5) . . . . ? C42 Fe1 C42' C41' -130.8(10) . . . . ? C42 Fe1 C42' C41' -62.3(5) 4 . . . ? C43 Fe1 C42' C41' 3.0(10) . . . . ? C43 Fe1 C42' C41' -22.7(5) 4 . . . ? C41' C42' C43' C43' -1.3(7) . . . 4 ? Fe1 C42' C43' C43' -60.0(2) . . . 4 ? C41' C42' C43' Fe1 58.7(6) . . . . ? C2 Fe1 C43' C42' 145.3(3) . . . . ? C1 Fe1 C43' C42' 20.9(7) . . . . ? C41' Fe1 C43' C42' -37.7(3) . . . . ? C43' Fe1 C43' C42' -118.7(3) 4 . . . ? C42' Fe1 C43' C42' -81.5(5) 4 . . . ? C41 Fe1 C43' C42' -135.8(13) . . . . ? C42 Fe1 C43' C42' 14.8(12) . . . . ? C42 Fe1 C43' C42' -102.9(6) 4 . . . ? C43 Fe1 C43' C42' -20.5(4) . . . . ? C43 Fe1 C43' C42' -60.9(4) 4 . . . ? C2 Fe1 C43' C43' -96.06(11) . . . 4 ? C1 Fe1 C43' C43' 139.5(6) . . . 4 ? C41' Fe1 C43' C43' 80.95(15) . . . 4 ? C42' Fe1 C43' C43' 118.7(3) . . . 4 ? C42' Fe1 C43' C43' 37.2(2) 4 . . 4 ? C41 Fe1 C43' C43' -17.1(12) . . . 4 ? C42 Fe1 C43' C43' 133.5(12) . . . 4 ? C42 Fe1 C43' C43' 15.8(4) 4 . . 4 ? C43 Fe1 C43' C43' 98.1(3) . . . 4 ? C43 Fe1 C43' C43' 57.8(2) 4 . . 4 ? C52 C51 C52 C53 0.01(3) 4 . . . ? C51 C52 C53 C54 0.01(4) . . . . ? C52 C53 C54 C53 -0.02(10) . . . 4 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.555 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.072 data_wa1065 _database_code_depnum_ccdc_archive 'CCDC 832034' #TrackingRef 'publ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 K O6, C7 H5 Fe O2' _chemical_formula_sum 'C19 H29 Fe K O8' _chemical_formula_weight 480.37 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 14.9080(5) _cell_length_b 10.4189(4) _cell_length_c 14.3622(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2230.81(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22927 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 26.0 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7861 _exptl_absorpt_correction_T_max 0.8192 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 26783 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 25.67 _reflns_number_total 4176 _reflns_number_gt 3843 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.0272P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.0045(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.068(14) _refine_ls_number_reflns 4176 _refine_ls_number_parameters 263 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0554 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _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 Fe1 Fe 0.262786(16) 0.49599(3) 0.50830(3) 0.02831(8) Uani 1 1 d . . . K1 K 0.43705(3) 0.72976(4) 0.48530(3) 0.03177(11) Uani 1 1 d . . . C1 C 0.35577(15) 0.4024(2) 0.52632(17) 0.0351(5) Uani 1 1 d . . . O1 O 0.41990(12) 0.33772(17) 0.53667(15) 0.0531(5) Uani 1 1 d . . . C2 C 0.28446(14) 0.5790(2) 0.60926(17) 0.0326(5) Uani 1 1 d . . . O2 O 0.30135(12) 0.63743(18) 0.67775(13) 0.0469(4) Uani 1 1 d . . . C11 C 0.21317(18) 0.4043(2) 0.38988(17) 0.0415(6) Uani 1 1 d . . . H11 H 0.2388 0.3285 0.3646 0.050 Uiso 1 1 calc R . . C12 C 0.14429(18) 0.4087(3) 0.4571(2) 0.0494(7) Uani 1 1 d . . . H12 H 0.1144 0.3371 0.4837 0.059 Uiso 1 1 calc R . . C13 C 0.12806(18) 0.5383(3) 0.4772(2) 0.0540(7) Uani 1 1 d . . . H13 H 0.0862 0.5700 0.5214 0.065 Uiso 1 1 calc R . . C14 C 0.1852(2) 0.6141(3) 0.41990(19) 0.0494(7) Uani 1 1 d . . . H14 H 0.1872 0.7052 0.4183 0.059 Uiso 1 1 calc R . . C15 C 0.2379(2) 0.5310(3) 0.36633(18) 0.0450(6) Uani 1 1 d . . . H15 H 0.2822 0.5554 0.3222 0.054 Uiso 1 1 calc R . . O21 O 0.46835(11) 0.65198(16) 0.29748(11) 0.0379(4) Uani 1 1 d . . . C22 C 0.4542(2) 0.7456(3) 0.22655(17) 0.0489(7) Uani 1 1 d . . . H22A H 0.4465 0.7024 0.1657 0.059 Uiso 1 1 calc R . . H22B H 0.5071 0.8028 0.2224 0.059 Uiso 1 1 calc R . . C23 C 0.3729(2) 0.8226(3) 0.24853(17) 0.0493(7) Uani 1 1 d . . . H23A H 0.3601 0.8835 0.1973 0.059 Uiso 1 1 calc R . . H23B H 0.3204 0.7655 0.2563 0.059 Uiso 1 1 calc R . . O24 O 0.38967(11) 0.89069(17) 0.33235(11) 0.0389(4) Uani 1 1 d . . . C25 C 0.32075(19) 0.9804(2) 0.35373(18) 0.0420(6) Uani 1 1 d . . . H25A H 0.2641 0.9346 0.3675 0.050 Uiso 1 1 calc R . . H25B H 0.3104 1.0380 0.2999 0.050 Uiso 1 1 calc R . . C26 C 0.34921(19) 1.0568(2) 0.43634(19) 0.0413(6) Uani 1 1 d . . . H26A H 0.4092 1.0945 0.4252 0.050 Uiso 1 1 calc R . . H26B H 0.3063 1.1277 0.4473 0.050 Uiso 1 1 calc R . . O27 O 0.35198(10) 0.97492(13) 0.51534(14) 0.0353(3) Uani 1 1 d . . . C28 C 0.37610(19) 1.0453(2) 0.59716(18) 0.0404(6) Uani 1 1 d . . . H28A H 0.3274 1.1054 0.6141 0.049 Uiso 1 1 calc R . . H28B H 0.4312 1.0957 0.5855 0.049 Uiso 1 1 calc R . . C29 C 0.39169(17) 0.9518(2) 0.67492(17) 0.0380(6) Uani 1 1 d . . . H29A H 0.3998 0.9984 0.7344 0.046 Uiso 1 1 calc R . . H29B H 0.3395 0.8937 0.6813 0.046 Uiso 1 1 calc R . . O30 O 0.46994(11) 0.88009(16) 0.65357(11) 0.0370(4) Uani 1 1 d . . . C31 C 0.49539(16) 0.7993(3) 0.72953(15) 0.0402(6) Uani 1 1 d . . . H31A H 0.4471 0.7367 0.7429 0.048 Uiso 1 1 calc R . . H31B H 0.5056 0.8516 0.7861 0.048 Uiso 1 1 calc R . . C32 C 0.57921(15) 0.7308(3) 0.70320(16) 0.0429(6) Uani 1 1 d . . . H32A H 0.6262 0.7936 0.6861 0.052 Uiso 1 1 calc R . . H32B H 0.6012 0.6795 0.7566 0.052 Uiso 1 1 calc R . . O33 O 0.56092(10) 0.64894(16) 0.62656(11) 0.0366(4) Uani 1 1 d . . . C34 C 0.63926(16) 0.5823(3) 0.59582(18) 0.0400(6) Uani 1 1 d . . . H34A H 0.6651 0.5321 0.6478 0.048 Uiso 1 1 calc R . . H34B H 0.6850 0.6445 0.5742 0.048 Uiso 1 1 calc R . . C35 C 0.61365(15) 0.4949(2) 0.5182(2) 0.0410(5) Uani 1 1 d . . . H35A H 0.6648 0.4386 0.5019 0.049 Uiso 1 1 calc R . . H35B H 0.5627 0.4401 0.5373 0.049 Uiso 1 1 calc R . . O36 O 0.58897(12) 0.57065(15) 0.43976(11) 0.0366(4) Uani 1 1 d . . . C37 C 0.56426(18) 0.4925(2) 0.36247(17) 0.0417(6) Uani 1 1 d . . . H37A H 0.5097 0.4425 0.3776 0.050 Uiso 1 1 calc R . . H37B H 0.6132 0.4315 0.3479 0.050 Uiso 1 1 calc R . . C38 C 0.54676(17) 0.5776(2) 0.28031(18) 0.0419(6) Uani 1 1 d . . . H38A H 0.5987 0.6350 0.2699 0.050 Uiso 1 1 calc R . . H38B H 0.5382 0.5247 0.2237 0.050 Uiso 1 1 calc R . . 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 Fe1 0.02794(13) 0.03163(13) 0.02536(13) 0.00336(13) -0.00225(16) -0.00090(12) K1 0.0334(2) 0.0369(2) 0.0250(2) -0.0003(2) 0.0000(2) -0.00201(19) C1 0.0375(12) 0.0315(10) 0.0362(13) 0.0019(10) -0.0076(10) -0.0045(9) O1 0.0418(10) 0.0404(9) 0.0770(14) 0.0005(9) -0.0149(9) 0.0070(8) C2 0.0257(11) 0.0374(12) 0.0346(13) 0.0040(10) 0.0002(9) 0.0023(9) O2 0.0442(10) 0.0552(11) 0.0414(10) -0.0121(9) -0.0087(8) 0.0006(8) C11 0.0477(15) 0.0409(13) 0.0358(13) -0.0052(10) -0.0099(11) 0.0069(11) C12 0.0415(14) 0.0565(16) 0.0504(16) 0.0071(12) -0.0169(12) -0.0117(12) C13 0.0363(13) 0.0828(19) 0.0428(15) -0.0088(14) -0.0104(11) 0.0177(12) C14 0.0659(18) 0.0369(14) 0.0455(15) 0.0004(12) -0.0241(13) 0.0115(12) C15 0.0556(16) 0.0534(16) 0.0259(12) 0.0065(10) -0.0073(11) -0.0005(12) O21 0.0455(9) 0.0410(9) 0.0272(8) 0.0000(7) 0.0074(7) -0.0036(7) C22 0.0762(19) 0.0485(15) 0.0219(10) -0.0027(11) 0.0085(12) -0.0073(13) C23 0.0732(19) 0.0489(15) 0.0257(12) -0.0005(11) -0.0088(12) -0.0014(14) O24 0.0443(10) 0.0466(10) 0.0258(8) -0.0007(7) -0.0007(7) 0.0030(7) C25 0.0457(15) 0.0440(14) 0.0363(13) 0.0096(11) -0.0021(10) 0.0024(11) C26 0.0474(15) 0.0333(13) 0.0431(15) 0.0060(11) 0.0089(12) -0.0009(11) O27 0.0461(8) 0.0291(7) 0.0306(8) 0.0031(7) 0.0038(9) -0.0045(6) C28 0.0534(16) 0.0308(12) 0.0371(13) -0.0042(10) 0.0094(11) -0.0054(11) C29 0.0462(15) 0.0400(13) 0.0277(12) -0.0054(10) 0.0102(10) -0.0050(11) O30 0.0382(9) 0.0475(10) 0.0252(8) -0.0010(7) 0.0065(6) -0.0051(7) C31 0.0398(13) 0.0610(16) 0.0198(12) -0.0016(10) -0.0034(11) -0.0084(11) C32 0.0300(12) 0.0702(17) 0.0286(12) -0.0029(12) -0.0051(9) -0.0071(11) O33 0.0267(8) 0.0528(10) 0.0302(8) -0.0020(7) -0.0025(7) -0.0022(7) C34 0.0312(13) 0.0499(15) 0.0390(14) 0.0045(11) -0.0025(10) 0.0018(11) C35 0.0388(10) 0.0387(11) 0.0454(15) 0.0054(12) 0.0003(13) 0.0018(11) O36 0.0401(9) 0.0355(9) 0.0341(9) -0.0053(7) 0.0022(7) -0.0035(7) C37 0.0446(14) 0.0387(13) 0.0418(13) -0.0123(11) 0.0055(10) -0.0044(12) C38 0.0448(14) 0.0462(14) 0.0348(13) -0.0119(11) 0.0080(11) -0.0050(11) _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 Fe1 C1 1.714(2) . ? Fe1 C2 1.719(2) . ? Fe1 C11 2.086(2) . ? Fe1 C13 2.104(3) . ? Fe1 C15 2.104(2) . ? Fe1 C14 2.113(2) . ? Fe1 C12 2.119(2) . ? K1 O24 2.8523(17) . ? K1 O21 2.8549(17) . ? K1 O33 2.8697(16) . ? K1 O36 2.8819(17) . ? K1 O27 2.8843(15) . ? K1 O30 2.9214(17) . ? K1 C2 3.288(2) . ? C1 O1 1.179(3) . ? C2 O2 1.184(3) . ? C11 C12 1.410(4) . ? C11 C15 1.411(4) . ? C11 H11 0.9500 . ? C12 C13 1.402(4) . ? C12 H12 0.9500 . ? C13 C14 1.423(4) . ? C13 H13 0.9500 . ? C14 C15 1.399(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? O21 C38 1.424(3) . ? O21 C22 1.426(3) . ? C22 C23 1.488(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O24 1.420(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? O24 C25 1.423(3) . ? C25 C26 1.490(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O27 1.420(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O27 C28 1.431(3) . ? C28 C29 1.499(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O30 1.419(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O30 C31 1.429(3) . ? C31 C32 1.488(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O33 1.419(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? O33 C34 1.429(3) . ? C34 C35 1.489(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O36 1.424(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? O36 C37 1.425(3) . ? C37 C38 1.499(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? 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 C1 Fe1 C2 90.40(11) . . ? C1 Fe1 C11 98.59(10) . . ? C2 Fe1 C11 169.96(10) . . ? C1 Fe1 C13 157.35(11) . . ? C2 Fe1 C13 104.66(11) . . ? C11 Fe1 C13 65.44(11) . . ? C1 Fe1 C15 112.80(12) . . ? C2 Fe1 C15 139.74(11) . . ? C11 Fe1 C15 39.36(10) . . ? C13 Fe1 C15 65.76(12) . . ? C1 Fe1 C14 149.84(12) . . ? C2 Fe1 C14 108.46(11) . . ? C11 Fe1 C14 65.32(10) . . ? C13 Fe1 C14 39.45(12) . . ? C15 Fe1 C14 38.76(11) . . ? C1 Fe1 C12 118.84(11) . . ? C2 Fe1 C12 131.74(11) . . ? C11 Fe1 C12 39.17(11) . . ? C13 Fe1 C12 38.77(12) . . ? C15 Fe1 C12 65.84(11) . . ? C14 Fe1 C12 65.46(11) . . ? C1 Fe1 K1 79.28(7) . . ? C2 Fe1 K1 66.33(8) . . ? C11 Fe1 K1 119.60(8) . . ? C13 Fe1 K1 122.08(9) . . ? C15 Fe1 K1 85.45(8) . . ? C14 Fe1 K1 86.88(8) . . ? C12 Fe1 K1 149.98(8) . . ? O24 K1 O21 58.65(5) . . ? O24 K1 O33 151.20(5) . . ? O21 K1 O33 118.65(5) . . ? O24 K1 O36 110.98(5) . . ? O21 K1 O36 59.59(5) . . ? O33 K1 O36 59.07(5) . . ? O24 K1 O27 59.05(5) . . ? O21 K1 O27 117.69(5) . . ? O33 K1 O27 115.91(5) . . ? O36 K1 O27 152.74(5) . . ? O24 K1 O30 111.31(5) . . ? O21 K1 O30 155.01(5) . . ? O33 K1 O30 57.62(5) . . ? O36 K1 O30 111.36(5) . . ? O27 K1 O30 58.34(5) . . ? O24 K1 C2 121.77(5) . . ? O21 K1 C2 119.29(5) . . ? O33 K1 C2 85.54(5) . . ? O36 K1 C2 113.07(5) . . ? O27 K1 C2 92.16(5) . . ? O30 K1 C2 85.65(5) . . ? O24 K1 Fe1 106.96(4) . . ? O21 K1 Fe1 90.73(3) . . ? O33 K1 Fe1 101.67(4) . . ? O36 K1 Fe1 101.54(3) . . ? O27 K1 Fe1 105.66(3) . . ? O30 K1 Fe1 114.24(3) . . ? C2 K1 Fe1 28.62(4) . . ? O1 C1 Fe1 178.6(2) . . ? O2 C2 Fe1 178.3(2) . . ? O2 C2 K1 93.29(15) . . ? Fe1 C2 K1 85.05(9) . . ? C12 C11 C15 108.9(2) . . ? C12 C11 Fe1 71.67(15) . . ? C15 C11 Fe1 71.02(14) . . ? C12 C11 H11 125.6 . . ? C15 C11 H11 125.6 . . ? Fe1 C11 H11 123.4 . . ? C13 C12 C11 107.3(2) . . ? C13 C12 Fe1 70.05(15) . . ? C11 C12 Fe1 69.16(14) . . ? C13 C12 H12 126.3 . . ? C11 C12 H12 126.3 . . ? Fe1 C12 H12 126.0 . . ? C12 C13 C14 108.2(2) . . ? C12 C13 Fe1 71.18(15) . . ? C14 C13 Fe1 70.60(15) . . ? C12 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? Fe1 C13 H13 123.9 . . ? C15 C14 C13 108.1(2) . . ? C15 C14 Fe1 70.30(14) . . ? C13 C14 Fe1 69.95(14) . . ? C15 C14 H14 126.0 . . ? C13 C14 H14 126.0 . . ? Fe1 C14 H14 125.4 . . ? C14 C15 C11 107.5(3) . . ? C14 C15 Fe1 70.95(15) . . ? C11 C15 Fe1 69.62(14) . . ? C14 C15 H15 126.3 . . ? C11 C15 H15 126.3 . . ? Fe1 C15 H15 124.8 . . ? C38 O21 C22 111.70(19) . . ? C38 O21 K1 116.89(14) . . ? C22 O21 K1 117.17(14) . . ? O21 C22 C23 109.7(2) . . ? O21 C22 H22A 109.7 . . ? C23 C22 H22A 109.7 . . ? O21 C22 H22B 109.7 . . ? C23 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? O24 C23 C22 107.8(2) . . ? O24 C23 H23A 110.1 . . ? C22 C23 H23A 110.1 . . ? O24 C23 H23B 110.1 . . ? C22 C23 H23B 110.1 . . ? H23A C23 H23B 108.5 . . ? C23 O24 C25 112.6(2) . . ? C23 O24 K1 113.76(15) . . ? C25 O24 K1 113.52(13) . . ? O24 C25 C26 108.5(2) . . ? O24 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? O24 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? O27 C26 C25 108.9(2) . . ? O27 C26 H26A 109.9 . . ? C25 C26 H26A 109.9 . . ? O27 C26 H26B 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? C26 O27 C28 110.84(16) . . ? C26 O27 K1 115.17(15) . . ? C28 O27 K1 117.77(14) . . ? O27 C28 C29 108.6(2) . . ? O27 C28 H28A 110.0 . . ? C29 C28 H28A 110.0 . . ? O27 C28 H28B 110.0 . . ? C29 C28 H28B 110.0 . . ? H28A C28 H28B 108.4 . . ? O30 C29 C28 107.96(19) . . ? O30 C29 H29A 110.1 . . ? C28 C29 H29A 110.1 . . ? O30 C29 H29B 110.1 . . ? C28 C29 H29B 110.1 . . ? H29A C29 H29B 108.4 . . ? C29 O30 C31 111.32(17) . . ? C29 O30 K1 108.86(13) . . ? C31 O30 K1 111.12(14) . . ? O30 C31 C32 108.16(18) . . ? O30 C31 H31A 110.1 . . ? C32 C31 H31A 110.1 . . ? O30 C31 H31B 110.1 . . ? C32 C31 H31B 110.1 . . ? H31A C31 H31B 108.4 . . ? O33 C32 C31 108.91(18) . . ? O33 C32 H32A 109.9 . . ? C31 C32 H32A 109.9 . . ? O33 C32 H32B 109.9 . . ? C31 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? C32 O33 C34 112.00(17) . . ? C32 O33 K1 119.73(14) . . ? C34 O33 K1 116.76(13) . . ? O33 C34 C35 108.59(19) . . ? O33 C34 H34A 110.0 . . ? C35 C34 H34A 110.0 . . ? O33 C34 H34B 110.0 . . ? C35 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? O36 C35 C34 108.65(19) . . ? O36 C35 H35A 110.0 . . ? C34 C35 H35A 110.0 . . ? O36 C35 H35B 110.0 . . ? C34 C35 H35B 110.0 . . ? H35A C35 H35B 108.3 . . ? C35 O36 C37 111.47(18) . . ? C35 O36 K1 110.03(14) . . ? C37 O36 K1 107.61(14) . . ? O36 C37 C38 108.66(19) . . ? O36 C37 H37A 110.0 . . ? C38 C37 H37A 110.0 . . ? O36 C37 H37B 110.0 . . ? C38 C37 H37B 110.0 . . ? H37A C37 H37B 108.3 . . ? O21 C38 C37 109.2(2) . . ? O21 C38 H38A 109.8 . . ? C37 C38 H38A 109.8 . . ? O21 C38 H38B 109.8 . . ? C37 C38 H38B 109.8 . . ? H38A C38 H38B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Fe1 K1 O24 138.61(9) . . . . ? C2 Fe1 K1 O24 -126.18(9) . . . . ? C11 Fe1 K1 O24 44.75(9) . . . . ? C13 Fe1 K1 O24 -33.23(10) . . . . ? C15 Fe1 K1 O24 24.36(9) . . . . ? C14 Fe1 K1 O24 -14.47(9) . . . . ? C12 Fe1 K1 O24 7.79(17) . . . . ? C1 Fe1 K1 O21 81.30(9) . . . . ? C2 Fe1 K1 O21 176.51(9) . . . . ? C11 Fe1 K1 O21 -12.56(9) . . . . ? C13 Fe1 K1 O21 -90.54(10) . . . . ? C15 Fe1 K1 O21 -32.95(9) . . . . ? C14 Fe1 K1 O21 -71.78(9) . . . . ? C12 Fe1 K1 O21 -49.52(17) . . . . ? C1 Fe1 K1 O33 -38.19(9) . . . . ? C2 Fe1 K1 O33 57.01(9) . . . . ? C11 Fe1 K1 O33 -132.05(9) . . . . ? C13 Fe1 K1 O33 149.96(10) . . . . ? C15 Fe1 K1 O33 -152.45(9) . . . . ? C14 Fe1 K1 O33 168.73(9) . . . . ? C12 Fe1 K1 O33 -169.01(17) . . . . ? C1 Fe1 K1 O36 22.23(9) . . . . ? C2 Fe1 K1 O36 117.44(9) . . . . ? C11 Fe1 K1 O36 -71.62(9) . . . . ? C13 Fe1 K1 O36 -149.61(10) . . . . ? C15 Fe1 K1 O36 -92.02(9) . . . . ? C14 Fe1 K1 O36 -130.84(9) . . . . ? C12 Fe1 K1 O36 -108.58(17) . . . . ? C1 Fe1 K1 O27 -159.61(9) . . . . ? C2 Fe1 K1 O27 -64.41(9) . . . . ? C11 Fe1 K1 O27 106.53(9) . . . . ? C13 Fe1 K1 O27 28.54(10) . . . . ? C15 Fe1 K1 O27 86.13(9) . . . . ? C14 Fe1 K1 O27 47.31(9) . . . . ? C12 Fe1 K1 O27 69.57(18) . . . . ? C1 Fe1 K1 O30 -97.75(9) . . . . ? C2 Fe1 K1 O30 -2.54(9) . . . . ? C11 Fe1 K1 O30 168.39(9) . . . . ? C13 Fe1 K1 O30 90.41(10) . . . . ? C15 Fe1 K1 O30 148.00(9) . . . . ? C14 Fe1 K1 O30 109.18(9) . . . . ? C12 Fe1 K1 O30 131.44(17) . . . . ? C1 Fe1 K1 C2 -95.21(12) . . . . ? C11 Fe1 K1 C2 170.93(11) . . . . ? C13 Fe1 K1 C2 92.95(12) . . . . ? C15 Fe1 K1 C2 150.54(11) . . . . ? C14 Fe1 K1 C2 111.72(11) . . . . ? C12 Fe1 K1 C2 133.98(19) . . . . ? C1 Fe1 C2 K1 78.11(8) . . . . ? C11 Fe1 C2 K1 -128.2(6) . . . . ? C13 Fe1 C2 K1 -118.99(10) . . . . ? C15 Fe1 C2 K1 -49.34(17) . . . . ? C14 Fe1 C2 K1 -77.95(10) . . . . ? C12 Fe1 C2 K1 -151.15(11) . . . . ? O24 K1 C2 O2 -115.12(14) . . . . ? O21 K1 C2 O2 175.63(13) . . . . ? O33 K1 C2 O2 55.12(14) . . . . ? O36 K1 C2 O2 108.71(14) . . . . ? O27 K1 C2 O2 -60.71(15) . . . . ? O30 K1 C2 O2 -2.68(14) . . . . ? Fe1 K1 C2 O2 179.6(2) . . . . ? O24 K1 C2 Fe1 65.24(9) . . . . ? O21 K1 C2 Fe1 -4.01(10) . . . . ? O33 K1 C2 Fe1 -124.52(8) . . . . ? O36 K1 C2 Fe1 -70.93(9) . . . . ? O27 K1 C2 Fe1 119.65(8) . . . . ? O30 K1 C2 Fe1 177.68(8) . . . . ? C1 Fe1 C11 C12 125.94(16) . . . . ? C2 Fe1 C11 C12 -27.4(7) . . . . ? C13 Fe1 C11 C12 -37.23(17) . . . . ? C15 Fe1 C11 C12 -118.3(2) . . . . ? C14 Fe1 C11 C12 -80.82(18) . . . . ? K1 Fe1 C11 C12 -151.56(13) . . . . ? C1 Fe1 C11 C15 -115.72(17) . . . . ? C2 Fe1 C11 C15 90.9(7) . . . . ? C13 Fe1 C11 C15 81.11(18) . . . . ? C14 Fe1 C11 C15 37.53(17) . . . . ? C12 Fe1 C11 C15 118.3(2) . . . . ? K1 Fe1 C11 C15 -33.22(18) . . . . ? C15 C11 C12 C13 -1.7(3) . . . . ? Fe1 C11 C12 C13 59.92(17) . . . . ? C15 C11 C12 Fe1 -61.61(17) . . . . ? C1 Fe1 C12 C13 175.45(17) . . . . ? C2 Fe1 C12 C13 55.3(2) . . . . ? C11 Fe1 C12 C13 -118.5(2) . . . . ? C15 Fe1 C12 C13 -80.79(18) . . . . ? C14 Fe1 C12 C13 -38.08(17) . . . . ? K1 Fe1 C12 C13 -62.6(2) . . . . ? C1 Fe1 C12 C11 -66.05(18) . . . . ? C2 Fe1 C12 C11 173.82(16) . . . . ? C13 Fe1 C12 C11 118.5(2) . . . . ? C15 Fe1 C12 C11 37.72(16) . . . . ? C14 Fe1 C12 C11 80.43(17) . . . . ? K1 Fe1 C12 C11 55.9(2) . . . . ? C11 C12 C13 C14 1.9(3) . . . . ? Fe1 C12 C13 C14 61.23(18) . . . . ? C11 C12 C13 Fe1 -59.35(17) . . . . ? C1 Fe1 C13 C12 -10.4(4) . . . . ? C2 Fe1 C13 C12 -140.64(17) . . . . ? C11 Fe1 C13 C12 37.61(16) . . . . ? C15 Fe1 C13 C12 81.01(18) . . . . ? C14 Fe1 C13 C12 118.0(2) . . . . ? K1 Fe1 C13 C12 148.37(14) . . . . ? C1 Fe1 C13 C14 -128.4(3) . . . . ? C2 Fe1 C13 C14 101.36(17) . . . . ? C11 Fe1 C13 C14 -80.39(17) . . . . ? C15 Fe1 C13 C14 -36.99(16) . . . . ? C12 Fe1 C13 C14 -118.0(2) . . . . ? K1 Fe1 C13 C14 30.37(18) . . . . ? C12 C13 C14 C15 -1.4(3) . . . . ? Fe1 C13 C14 C15 60.22(18) . . . . ? C12 C13 C14 Fe1 -61.60(17) . . . . ? C1 Fe1 C14 C15 24.3(3) . . . . ? C2 Fe1 C14 C15 150.38(17) . . . . ? C11 Fe1 C14 C15 -38.10(16) . . . . ? C13 Fe1 C14 C15 -118.8(2) . . . . ? C12 Fe1 C14 C15 -81.36(19) . . . . ? K1 Fe1 C14 C15 86.61(16) . . . . ? C1 Fe1 C14 C13 143.1(2) . . . . ? C2 Fe1 C14 C13 -90.82(17) . . . . ? C11 Fe1 C14 C13 80.70(18) . . . . ? C15 Fe1 C14 C13 118.8(2) . . . . ? C12 Fe1 C14 C13 37.43(16) . . . . ? K1 Fe1 C14 C13 -154.59(15) . . . . ? C13 C14 C15 C11 0.3(3) . . . . ? Fe1 C14 C15 C11 60.33(17) . . . . ? C13 C14 C15 Fe1 -60.00(18) . . . . ? C12 C11 C15 C14 0.8(3) . . . . ? Fe1 C11 C15 C14 -61.18(18) . . . . ? C12 C11 C15 Fe1 62.02(17) . . . . ? C1 Fe1 C15 C14 -167.05(17) . . . . ? C2 Fe1 C15 C14 -46.5(3) . . . . ? C11 Fe1 C15 C14 117.9(2) . . . . ? C13 Fe1 C15 C14 37.64(18) . . . . ? C12 Fe1 C15 C14 80.32(19) . . . . ? K1 Fe1 C15 C14 -90.69(16) . . . . ? C1 Fe1 C15 C11 75.10(17) . . . . ? C2 Fe1 C15 C11 -164.36(16) . . . . ? C13 Fe1 C15 C11 -80.22(18) . . . . ? C14 Fe1 C15 C11 -117.9(2) . . . . ? C12 Fe1 C15 C11 -37.54(16) . . . . ? K1 Fe1 C15 C11 151.46(16) . . . . ? O24 K1 O21 C38 145.18(16) . . . . ? O33 K1 O21 C38 -1.58(16) . . . . ? O36 K1 O21 C38 -2.35(14) . . . . ? O27 K1 O21 C38 146.53(14) . . . . ? O30 K1 O21 C38 72.6(2) . . . . ? C2 K1 O21 C38 -103.41(15) . . . . ? Fe1 K1 O21 C38 -105.32(15) . . . . ? O24 K1 O21 C22 8.59(16) . . . . ? O33 K1 O21 C22 -138.17(16) . . . . ? O36 K1 O21 C22 -138.93(18) . . . . ? O27 K1 O21 C22 9.94(18) . . . . ? O30 K1 O21 C22 -64.0(2) . . . . ? C2 K1 O21 C22 120.01(17) . . . . ? Fe1 K1 O21 C22 118.09(17) . . . . ? C38 O21 C22 C23 -178.8(2) . . . . ? K1 O21 C22 C23 -40.1(3) . . . . ? O21 C22 C23 O24 64.0(3) . . . . ? C22 C23 O24 C25 172.4(2) . . . . ? C22 C23 O24 K1 -56.7(2) . . . . ? O21 K1 O24 C23 25.62(16) . . . . ? O33 K1 O24 C23 118.91(17) . . . . ? O36 K1 O24 C23 55.35(17) . . . . ? O27 K1 O24 C23 -152.99(18) . . . . ? O30 K1 O24 C23 179.99(16) . . . . ? C2 K1 O24 C23 -81.62(18) . . . . ? Fe1 K1 O24 C23 -54.58(17) . . . . ? O21 K1 O24 C25 156.13(17) . . . . ? O33 K1 O24 C25 -110.59(16) . . . . ? O36 K1 O24 C25 -174.14(15) . . . . ? O27 K1 O24 C25 -22.48(15) . . . . ? O30 K1 O24 C25 -49.51(16) . . . . ? C2 K1 O24 C25 48.88(17) . . . . ? Fe1 K1 O24 C25 75.92(15) . . . . ? C23 O24 C25 C26 -173.7(2) . . . . ? K1 O24 C25 C26 55.2(2) . . . . ? O24 C25 C26 O27 -67.3(3) . . . . ? C25 C26 O27 C28 -178.0(2) . . . . ? C25 C26 O27 K1 45.1(2) . . . . ? O24 K1 O27 C26 -12.80(15) . . . . ? O21 K1 O27 C26 -14.15(16) . . . . ? O33 K1 O27 C26 134.83(15) . . . . ? O36 K1 O27 C26 62.6(2) . . . . ? O30 K1 O27 C26 137.38(16) . . . . ? C2 K1 O27 C26 -139.08(15) . . . . ? Fe1 K1 O27 C26 -113.47(15) . . . . ? O24 K1 O27 C28 -146.57(16) . . . . ? O21 K1 O27 C28 -147.91(14) . . . . ? O33 K1 O27 C28 1.07(16) . . . . ? O36 K1 O27 C28 -71.19(19) . . . . ? O30 K1 O27 C28 3.61(14) . . . . ? C2 K1 O27 C28 87.16(15) . . . . ? Fe1 K1 O27 C28 112.77(14) . . . . ? C26 O27 C28 C29 -171.5(2) . . . . ? K1 O27 C28 C29 -35.9(2) . . . . ? O27 C28 C29 O30 67.9(2) . . . . ? C28 C29 O30 C31 173.1(2) . . . . ? C28 C29 O30 K1 -64.1(2) . . . . ? O24 K1 O30 C29 58.21(14) . . . . ? O21 K1 O30 C29 119.21(15) . . . . ? O33 K1 O30 C29 -151.74(15) . . . . ? O36 K1 O30 C29 -177.37(13) . . . . ? O27 K1 O30 C29 30.97(13) . . . . ? C2 K1 O30 C29 -64.27(14) . . . . ? Fe1 K1 O30 C29 -63.05(14) . . . . ? O24 K1 O30 C31 -178.84(13) . . . . ? O21 K1 O30 C31 -117.85(16) . . . . ? O33 K1 O30 C31 -28.80(13) . . . . ? O36 K1 O30 C31 -54.42(14) . . . . ? O27 K1 O30 C31 153.91(15) . . . . ? C2 K1 O30 C31 58.67(14) . . . . ? Fe1 K1 O30 C31 59.89(14) . . . . ? C29 O30 C31 C32 -178.2(2) . . . . ? K1 O30 C31 C32 60.3(2) . . . . ? O30 C31 C32 O33 -64.3(3) . . . . ? C31 C32 O33 C34 178.5(2) . . . . ? C31 C32 O33 K1 36.3(2) . . . . ? O24 K1 O33 C32 70.06(18) . . . . ? O21 K1 O33 C32 146.36(14) . . . . ? O36 K1 O33 C32 147.13(16) . . . . ? O27 K1 O33 C32 -2.30(16) . . . . ? O30 K1 O33 C32 -4.87(14) . . . . ? C2 K1 O33 C32 -92.54(15) . . . . ? Fe1 K1 O33 C32 -116.30(14) . . . . ? O24 K1 O33 C34 -70.40(19) . . . . ? O21 K1 O33 C34 5.91(17) . . . . ? O36 K1 O33 C34 6.67(15) . . . . ? O27 K1 O33 C34 -142.76(15) . . . . ? O30 K1 O33 C34 -145.32(17) . . . . ? C2 K1 O33 C34 127.00(16) . . . . ? Fe1 K1 O33 C34 103.24(15) . . . . ? C32 O33 C34 C35 177.7(2) . . . . ? K1 O33 C34 C35 -38.9(2) . . . . ? O33 C34 C35 O36 67.9(3) . . . . ? C34 C35 O36 C37 179.56(18) . . . . ? C34 C35 O36 K1 -61.1(2) . . . . ? O24 K1 O36 C35 177.70(13) . . . . ? O21 K1 O36 C35 -152.89(15) . . . . ? O33 K1 O36 C35 27.89(13) . . . . ? O27 K1 O36 C35 114.98(16) . . . . ? O30 K1 O36 C35 53.09(14) . . . . ? C2 K1 O36 C35 -41.39(15) . . . . ? Fe1 K1 O36 C35 -68.90(14) . . . . ? O24 K1 O36 C37 -60.67(14) . . . . ? O21 K1 O36 C37 -31.25(13) . . . . ? O33 K1 O36 C37 149.53(15) . . . . ? O27 K1 O36 C37 -123.38(15) . . . . ? O30 K1 O36 C37 174.73(13) . . . . ? C2 K1 O36 C37 80.25(15) . . . . ? Fe1 K1 O36 C37 52.73(14) . . . . ? C35 O36 C37 C38 -175.23(19) . . . . ? K1 O36 C37 C38 64.0(2) . . . . ? C22 O21 C38 C37 173.1(2) . . . . ? K1 O21 C38 C37 34.3(2) . . . . ? O36 C37 C38 O21 -67.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.172 _refine_diff_density_min -0.162 _refine_diff_density_rms 0.039