# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'G Erker' 'Roland Frohlich' 'Gerald Kehr' 'Jochen Niemeyer' _publ_contact_author_name 'G Erker' _publ_contact_author_email ERKER@UNI-MUENSTER.DE _publ_section_title ; Selective Synthesis of the 2-Hydroxyferrocene-aldimine Enantiomers - Extended Planar-Chiral Analogues of the "Flat" Salicylaldimine Ligand Family ; # Attachment 'S,S,p-R-13.cif' data_erk4324 _database_code_depnum_ccdc_archive 'CCDC 714358' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H19 Fe I O3' _chemical_formula_weight 442.06 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.8132(1) _cell_length_b 20.1279(3) _cell_length_c 16.9731(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.4640(10) _cell_angle_gamma 90.00 _cell_volume 3346.39(7) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6135 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 2.752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4923 _exptl_absorpt_correction_T_max 0.6829 _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'roptating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22945 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.88 _reflns_number_total 13402 _reflns_number_gt 10864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0302P)^2^+4.2658P] 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 riding _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 -0.018(17) _refine_ls_number_reflns 13402 _refine_ls_number_parameters 761 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Fe1A Fe 0.16492(8) 0.21259(4) 0.34423(4) 0.04301(19) Uani 1 1 d . . . I1A I 0.08997(5) 0.35566(3) 0.47250(3) 0.07130(15) Uani 1 1 d . . . C1A C 0.2804(6) 0.2340(3) 0.4434(3) 0.0429(13) Uani 1 1 d . . . C2A C 0.1458(5) 0.2581(3) 0.4483(3) 0.0432(13) Uani 1 1 d . . . C3A C 0.0547(6) 0.2026(4) 0.4418(3) 0.0501(15) Uani 1 1 d . . . H3A H -0.0407 0.2041 0.4440 0.060 Uiso 1 1 calc R . . C4A C 0.1339(7) 0.1455(3) 0.4316(3) 0.0537(16) Uani 1 1 d . . . H4A H 0.1004 0.1020 0.4246 0.064 Uiso 1 1 calc R . . C5A C 0.2758(6) 0.1650(3) 0.4337(3) 0.0464(14) Uani 1 1 d . . . H5A H 0.3510 0.1367 0.4294 0.056 Uiso 1 1 calc R . . C6A C 0.0301(9) 0.2141(6) 0.2477(4) 0.079(2) Uani 1 1 d . . . H6A H -0.0650 0.2092 0.2484 0.095 Uiso 1 1 calc R . . C7A C 0.1023(11) 0.2736(5) 0.2553(4) 0.089(3) Uani 1 1 d . . . H7A H 0.0638 0.3160 0.2609 0.107 Uiso 1 1 calc R . . C8A C 0.2457(9) 0.2592(5) 0.2532(4) 0.074(2) Uani 1 1 d . . . H8A H 0.3184 0.2896 0.2587 0.089 Uiso 1 1 calc R . . C9A C 0.2546(8) 0.1902(4) 0.2411(4) 0.0637(19) Uani 1 1 d . . . H9A H 0.3351 0.1658 0.2354 0.076 Uiso 1 1 calc R . . C10A C 0.1219(8) 0.1644(5) 0.2392(4) 0.071(2) Uani 1 1 d . . . H10A H 0.0996 0.1192 0.2329 0.085 Uiso 1 1 calc R . . C11A C 0.4072(5) 0.2747(3) 0.4546(4) 0.0486(14) Uani 1 1 d . . . H11A H 0.3822 0.3221 0.4594 0.058 Uiso 1 1 calc R . . O12A O 0.4904(4) 0.2667(2) 0.3903(2) 0.0444(9) Uani 1 1 d . . . C13A C 0.6090(6) 0.3081(3) 0.3981(4) 0.0562(17) Uani 1 1 d . . . H13A H 0.5804 0.3551 0.4021 0.067 Uiso 1 1 calc R . . C14A C 0.6890(7) 0.2875(4) 0.4753(5) 0.073(2) Uani 1 1 d . . . H14A H 0.7222 0.2418 0.4707 0.087 Uiso 1 1 calc R . . H14B H 0.7681 0.3167 0.4850 0.087 Uiso 1 1 calc R . . C15A C 0.5973(7) 0.2923(5) 0.5432(5) 0.081(3) Uani 1 1 d . . . H15A H 0.6456 0.2758 0.5915 0.097 Uiso 1 1 calc R . . H15B H 0.5724 0.3388 0.5516 0.097 Uiso 1 1 calc R . . O16A O 0.4757(4) 0.2533(3) 0.5260(3) 0.0701(14) Uani 1 1 d . . . C17A C 0.6896(7) 0.2997(3) 0.3269(4) 0.0610(18) Uani 1 1 d . . . H17A H 0.7752 0.3247 0.3337 0.073 Uiso 1 1 calc R . . H17B H 0.7122 0.2527 0.3202 0.073 Uiso 1 1 calc R . . O18A O 0.6139(5) 0.3226(3) 0.2599(3) 0.0729(14) Uani 1 1 d . . . C19A C 0.6808(9) 0.3138(5) 0.1896(5) 0.086(2) Uani 1 1 d . . . H19A H 0.7711 0.3335 0.1953 0.129 Uiso 1 1 calc R . . H19B H 0.6285 0.3352 0.1464 0.129 Uiso 1 1 calc R . . H19C H 0.6889 0.2667 0.1786 0.129 Uiso 1 1 calc R . . Fe1B Fe 0.41578(10) 0.53369(4) 0.73445(5) 0.0502(2) Uani 1 1 d . . . I1B I 0.06614(6) 0.47118(3) 0.70043(4) 0.08487(18) Uani 1 1 d . . . C1B C 0.2881(6) 0.5745(3) 0.6500(3) 0.0476(14) Uani 1 1 d . . . C2B C 0.2128(7) 0.5467(3) 0.7110(4) 0.0526(16) Uani 1 1 d . . . C3B C 0.2537(7) 0.5781(3) 0.7830(4) 0.0537(16) Uani 1 1 d . . . H3B H 0.2210 0.5684 0.8326 0.064 Uiso 1 1 calc R . . C4B C 0.3525(8) 0.6266(3) 0.7672(4) 0.0561(17) Uani 1 1 d . . . H4B H 0.3958 0.6556 0.8042 0.067 Uiso 1 1 calc R . . C5B C 0.3747(6) 0.6238(3) 0.6850(3) 0.0462(14) Uani 1 1 d . . . H5B H 0.4364 0.6502 0.6586 0.055 Uiso 1 1 calc R . . C6B C 0.6175(11) 0.5128(5) 0.7192(6) 0.099(3) Uani 1 1 d . . . H6B H 0.6799 0.5390 0.6930 0.119 Uiso 1 1 calc R . . C7B C 0.5986(10) 0.5162(5) 0.7964(6) 0.098(3) Uani 1 1 d . . . H7B H 0.6442 0.5456 0.8320 0.117 Uiso 1 1 calc R . . C8B C 0.5034(10) 0.4706(4) 0.8159(5) 0.084(3) Uani 1 1 d . . . H8B H 0.4737 0.4630 0.8667 0.101 Uiso 1 1 calc R . . C9B C 0.4561(9) 0.4359(4) 0.7447(7) 0.100(3) Uani 1 1 d . . . H9B H 0.3903 0.4020 0.7398 0.120 Uiso 1 1 calc R . . C10B C 0.5319(10) 0.4649(5) 0.6827(5) 0.080(3) Uani 1 1 d . . . H10B H 0.5250 0.4537 0.6288 0.096 Uiso 1 1 calc R . . C11B C 0.2745(6) 0.5549(3) 0.5651(3) 0.0484(14) Uani 1 1 d . . . H11B H 0.2330 0.5102 0.5592 0.058 Uiso 1 1 calc R . . O12B O 0.4070(4) 0.5555(2) 0.5351(2) 0.0528(11) Uani 1 1 d . . . C13B C 0.4023(8) 0.5371(4) 0.4544(4) 0.0649(19) Uani 1 1 d . . . H13B H 0.3616 0.4922 0.4493 0.078 Uiso 1 1 calc R . . C14B C 0.3105(10) 0.5851(5) 0.4074(4) 0.091(3) Uani 1 1 d . . . H14C H 0.3516 0.6295 0.4086 0.109 Uiso 1 1 calc R . . H14D H 0.2993 0.5706 0.3523 0.109 Uiso 1 1 calc R . . C15B C 0.1741(10) 0.5874(6) 0.4428(4) 0.097(3) Uani 1 1 d . . . H15C H 0.1166 0.6212 0.4156 0.116 Uiso 1 1 calc R . . H15D H 0.1286 0.5443 0.4357 0.116 Uiso 1 1 calc R . . O16B O 0.1905(6) 0.6029(3) 0.5252(3) 0.0783(16) Uani 1 1 d . . . C17B C 0.5460(9) 0.5332(6) 0.4314(5) 0.089(3) Uani 1 1 d . . . H17C H 0.5479 0.5241 0.3748 0.107 Uiso 1 1 calc R . . H17D H 0.5926 0.5755 0.4426 0.107 Uiso 1 1 calc R . . O18B O 0.6130(7) 0.4814(5) 0.4752(5) 0.120(3) Uani 1 1 d . . . C19B C 0.7479(11) 0.4783(8) 0.4799(10) 0.175(7) Uani 1 1 d . . . H19D H 0.7799 0.4674 0.4285 0.263 Uiso 1 1 calc R . . H19E H 0.7777 0.4443 0.5176 0.263 Uiso 1 1 calc R . . H19F H 0.7850 0.5209 0.4971 0.263 Uiso 1 1 calc R . . Fe1C Fe 0.29026(7) 0.59255(4) 0.08906(4) 0.03379(16) Uani 1 1 d . . . I1CA I 0.40387(4) 0.44814(2) 0.21421(2) 0.04999(10) Uani 1 1 d . . . C1C C 0.1936(5) 0.5651(3) 0.1855(3) 0.0368(12) Uani 1 1 d . . . C2C C 0.3331(5) 0.5446(3) 0.1925(3) 0.0363(12) Uani 1 1 d . . . C3C C 0.4172(5) 0.6018(3) 0.1877(3) 0.0423(13) Uani 1 1 d . . . H3C H 0.5131 0.6026 0.1893 0.051 Uiso 1 1 calc R . . C4C C 0.3292(6) 0.6571(3) 0.1801(3) 0.0434(13) Uani 1 1 d . . . H4C H 0.3577 0.7015 0.1763 0.052 Uiso 1 1 calc R . . C5C C 0.1923(6) 0.6358(3) 0.1792(3) 0.0385(12) Uani 1 1 d . . . H5C H 0.1146 0.6632 0.1751 0.046 Uiso 1 1 calc R . . C6C C 0.3301(6) 0.5301(3) -0.0009(3) 0.0479(14) Uani 1 1 d . . . H6C H 0.3649 0.4867 0.0044 0.057 Uiso 1 1 calc R . . C7C C 0.4080(6) 0.5885(4) -0.0065(3) 0.0500(16) Uani 1 1 d . . . H7C H 0.5037 0.5910 -0.0055 0.060 Uiso 1 1 calc R . . C8C C 0.3167(7) 0.6428(3) -0.0138(3) 0.0498(15) Uani 1 1 d . . . H8C H 0.3409 0.6878 -0.0180 0.060 Uiso 1 1 calc R . . C9C C 0.1817(7) 0.6172(3) -0.0136(3) 0.0453(14) Uani 1 1 d . . . H9C H 0.1006 0.6421 -0.0185 0.054 Uiso 1 1 calc R . . C10C C 0.1912(6) 0.5481(3) -0.0048(3) 0.0437(14) Uani 1 1 d . . . H10C H 0.1173 0.5186 -0.0019 0.052 Uiso 1 1 calc R . . C11C C 0.0739(5) 0.5201(3) 0.1927(3) 0.0411(13) Uani 1 1 d . . . H11C H 0.1002 0.4740 0.1801 0.049 Uiso 1 1 calc R . . O12C O -0.0352(3) 0.53975(18) 0.1421(2) 0.0363(8) Uani 1 1 d . . . C13C C -0.1488(5) 0.4954(3) 0.1476(4) 0.0440(14) Uani 1 1 d . . . H13C H -0.1207 0.4499 0.1334 0.053 Uiso 1 1 calc R . . C14C C -0.1917(6) 0.4955(4) 0.2314(4) 0.066(2) Uani 1 1 d . . . H14E H -0.2272 0.5394 0.2444 0.079 Uiso 1 1 calc R . . H14F H -0.2647 0.4629 0.2369 0.079 Uiso 1 1 calc R . . C15C C -0.0723(7) 0.4787(5) 0.2872(4) 0.082(3) Uani 1 1 d . . . H15E H -0.0981 0.4830 0.3418 0.098 Uiso 1 1 calc R . . H15F H -0.0440 0.4326 0.2788 0.098 Uiso 1 1 calc R . . O16C O 0.0403(4) 0.5237(3) 0.2731(2) 0.0616(13) Uani 1 1 d . . . C17C C -0.2630(6) 0.5186(4) 0.0894(4) 0.0543(16) Uani 1 1 d . . . H17E H -0.3413 0.4888 0.0931 0.065 Uiso 1 1 calc R . . H17F H -0.2919 0.5631 0.1049 0.065 Uiso 1 1 calc R . . O18C O -0.2281(5) 0.5208(2) 0.0103(3) 0.0641(13) Uani 1 1 d . . . C19C C -0.2071(10) 0.4601(4) -0.0250(5) 0.094(3) Uani 1 1 d . . . H19G H -0.1233 0.4404 -0.0024 0.140 Uiso 1 1 calc R . . H19H H -0.2000 0.4664 -0.0813 0.140 Uiso 1 1 calc R . . H19I H -0.2832 0.4308 -0.0162 0.140 Uiso 1 1 calc R . . Fe1D Fe -0.14868(8) 0.77096(4) 0.01252(4) 0.03546(17) Uani 1 1 d . . . I1D I -0.49905(4) 0.81909(2) 0.05438(3) 0.05634(11) Uani 1 1 d . . . C1D C -0.2499(5) 0.7240(3) 0.0970(3) 0.0376(12) Uani 1 1 d . . . C2D C -0.3433(5) 0.7509(3) 0.0371(3) 0.0366(12) Uani 1 1 d . . . C3D C -0.3157(6) 0.7234(3) -0.0371(3) 0.0389(12) Uani 1 1 d . . . H3D H -0.3607 0.7342 -0.0859 0.047 Uiso 1 1 calc R . . C4D C -0.2097(6) 0.6776(3) -0.0247(3) 0.0431(13) Uani 1 1 d . . . H4D H -0.1722 0.6513 -0.0637 0.052 Uiso 1 1 calc R . . C5D C -0.1683(6) 0.6775(3) 0.0571(3) 0.0434(13) Uani 1 1 d . . . H5D H -0.0985 0.6510 0.0810 0.052 Uiso 1 1 calc R . . C6D C -0.0936(8) 0.8437(4) -0.0609(5) 0.076(2) Uani 1 1 d . . . H6D H -0.1386 0.8543 -0.1097 0.091 Uiso 1 1 calc R . . C7D C 0.0125(8) 0.7989(4) -0.0504(4) 0.064(2) Uani 1 1 d . . . H7D H 0.0523 0.7740 -0.0898 0.077 Uiso 1 1 calc R . . C8D C 0.0492(7) 0.7981(3) 0.0308(4) 0.0592(17) Uani 1 1 d . . . H8D H 0.1191 0.7720 0.0552 0.071 Uiso 1 1 calc R . . C9D C -0.0343(8) 0.8421(4) 0.0698(4) 0.064(2) Uani 1 1 d . . . H9D H -0.0320 0.8510 0.1242 0.077 Uiso 1 1 calc R . . C10D C -0.1235(8) 0.8704(3) 0.0096(6) 0.068(2) Uani 1 1 d . . . H10D H -0.1915 0.9022 0.0173 0.082 Uiso 1 1 calc R . . C11D C -0.2454(6) 0.7383(3) 0.1822(3) 0.0419(13) Uani 1 1 d . . . H11D H -0.2924 0.7808 0.1914 0.050 Uiso 1 1 calc R . . O12D O -0.1088(4) 0.7426(2) 0.2114(2) 0.0428(9) Uani 1 1 d . . . C13D C -0.0988(7) 0.7572(3) 0.2948(4) 0.0529(16) Uani 1 1 d . . . H13D H -0.1475 0.7995 0.3028 0.064 Uiso 1 1 calc R . . C14D C -0.1700(9) 0.7042(5) 0.3381(4) 0.083(3) Uani 1 1 d . . . H14G H -0.1698 0.7155 0.3942 0.100 Uiso 1 1 calc R . . H14H H -0.1224 0.6618 0.3330 0.100 Uiso 1 1 calc R . . C15D C -0.3153(9) 0.6984(6) 0.3035(4) 0.102(4) Uani 1 1 d . . . H15G H -0.3617 0.6617 0.3288 0.122 Uiso 1 1 calc R . . H15H H -0.3654 0.7395 0.3130 0.122 Uiso 1 1 calc R . . O16D O -0.3130(5) 0.6863(3) 0.2195(2) 0.0646(14) Uani 1 1 d . . . C17D C 0.0483(8) 0.7677(4) 0.3198(5) 0.080(2) Uani 1 1 d . . . H17G H 0.0597 0.7699 0.3775 0.096 Uiso 1 1 calc R . . H17H H 0.1028 0.7305 0.3018 0.096 Uiso 1 1 calc R . . O18D O 0.0948(6) 0.8293(3) 0.2858(6) 0.135(3) Uani 1 1 d . . . C19D C 0.2152(10) 0.8350(7) 0.2640(7) 0.127(4) Uani 1 1 d . . . H19J H 0.2747 0.8503 0.3079 0.191 Uiso 1 1 calc R . . H19K H 0.2164 0.8668 0.2211 0.191 Uiso 1 1 calc R . . H19L H 0.2467 0.7922 0.2462 0.191 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 Fe1A 0.0385(4) 0.0547(5) 0.0359(4) 0.0049(4) 0.0029(3) 0.0014(4) I1A 0.0457(2) 0.0662(3) 0.1034(4) -0.0176(3) 0.0162(2) 0.0060(2) C1A 0.037(3) 0.053(4) 0.039(3) 0.001(3) 0.002(2) -0.001(3) C2A 0.034(3) 0.055(4) 0.042(3) 0.005(3) 0.006(2) 0.001(3) C3A 0.041(3) 0.070(5) 0.040(3) 0.001(3) 0.008(2) 0.002(3) C4A 0.059(4) 0.056(4) 0.046(4) 0.012(3) 0.002(3) -0.013(3) C5A 0.040(3) 0.053(4) 0.046(3) 0.004(3) 0.003(2) 0.001(3) C6A 0.061(5) 0.118(8) 0.058(5) 0.014(5) -0.005(3) 0.006(5) C7A 0.129(8) 0.094(7) 0.044(4) 0.022(4) 0.002(4) 0.048(6) C8A 0.100(6) 0.087(6) 0.036(4) 0.019(4) 0.001(3) -0.020(5) C9A 0.062(5) 0.083(6) 0.047(4) 0.005(4) 0.008(3) 0.003(4) C10A 0.077(5) 0.094(6) 0.041(4) -0.009(4) -0.005(3) -0.014(5) C11A 0.031(3) 0.058(4) 0.057(4) -0.007(3) 0.008(2) 0.000(3) O12A 0.030(2) 0.048(2) 0.056(2) -0.0080(19) 0.0118(16) -0.0045(17) C13A 0.036(3) 0.046(4) 0.088(5) -0.016(3) 0.012(3) -0.004(3) C14A 0.040(4) 0.087(6) 0.092(5) -0.018(5) 0.003(3) -0.010(4) C15A 0.048(4) 0.122(8) 0.070(5) -0.020(5) -0.004(3) -0.013(4) O16A 0.040(2) 0.113(5) 0.056(3) -0.006(3) -0.0031(19) -0.009(3) C17A 0.042(4) 0.045(4) 0.098(5) -0.009(4) 0.026(3) -0.005(3) O18A 0.061(3) 0.073(3) 0.088(4) 0.018(3) 0.033(3) 0.011(3) C19A 0.102(7) 0.074(6) 0.086(6) 0.000(5) 0.040(5) -0.005(5) Fe1B 0.0698(6) 0.0405(5) 0.0411(5) 0.0107(4) 0.0108(4) 0.0136(4) I1B 0.0859(4) 0.0754(4) 0.0962(4) -0.0044(3) 0.0296(3) -0.0251(3) C1B 0.061(4) 0.043(4) 0.039(3) 0.006(3) 0.005(3) 0.009(3) C2B 0.063(4) 0.042(4) 0.054(4) 0.003(3) 0.018(3) 0.005(3) C3B 0.074(4) 0.046(4) 0.043(4) 0.005(3) 0.023(3) 0.015(3) C4B 0.086(5) 0.038(4) 0.045(4) -0.004(3) 0.007(3) 0.015(3) C5B 0.060(4) 0.037(3) 0.042(3) 0.003(3) 0.005(3) 0.009(3) C6B 0.112(8) 0.091(8) 0.094(8) 0.020(6) 0.017(6) 0.048(6) C7B 0.100(7) 0.088(7) 0.103(8) 0.029(6) -0.010(5) 0.037(6) C8B 0.125(7) 0.062(5) 0.067(5) 0.029(4) 0.021(5) 0.033(5) C9B 0.084(6) 0.038(4) 0.176(11) 0.014(6) -0.004(6) 0.020(4) C10B 0.105(7) 0.072(6) 0.064(5) 0.004(4) 0.008(4) 0.052(5) C11B 0.053(4) 0.044(4) 0.048(3) 0.005(3) 0.001(3) 0.012(3) O12B 0.062(3) 0.059(3) 0.037(2) 0.002(2) 0.0034(18) -0.001(2) C13B 0.076(5) 0.071(5) 0.048(4) -0.018(4) 0.008(3) -0.009(4) C14B 0.137(8) 0.098(7) 0.037(4) 0.002(4) -0.011(4) 0.009(6) C15B 0.115(8) 0.125(8) 0.047(4) -0.008(5) -0.018(4) 0.046(6) O16B 0.093(4) 0.093(4) 0.048(3) -0.002(3) -0.008(2) 0.042(3) C17B 0.082(6) 0.116(8) 0.071(5) -0.033(5) 0.028(4) -0.032(6) O18B 0.067(4) 0.143(7) 0.152(7) -0.024(6) 0.021(4) -0.006(4) C19B 0.080(8) 0.183(16) 0.269(18) -0.063(14) 0.056(9) -0.027(9) Fe1C 0.0324(4) 0.0329(4) 0.0364(4) -0.0049(3) 0.0041(3) -0.0065(3) I1CA 0.03288(18) 0.0506(2) 0.0662(2) 0.0079(2) 0.00041(15) 0.00293(17) C1C 0.033(3) 0.040(3) 0.037(3) -0.005(2) 0.005(2) -0.005(2) C2C 0.029(3) 0.043(3) 0.037(3) -0.002(2) -0.002(2) -0.002(2) C3C 0.028(3) 0.053(4) 0.046(3) -0.004(3) 0.003(2) -0.013(2) C4C 0.050(3) 0.033(3) 0.048(3) -0.012(2) 0.009(2) -0.015(3) C5C 0.038(3) 0.036(3) 0.042(3) -0.007(2) 0.005(2) -0.001(2) C6C 0.058(4) 0.042(3) 0.044(3) -0.013(3) 0.002(3) 0.010(3) C7C 0.041(3) 0.074(5) 0.036(3) -0.006(3) 0.011(2) -0.008(3) C8C 0.065(4) 0.047(4) 0.039(3) 0.000(3) 0.013(3) -0.016(3) C9C 0.059(4) 0.041(3) 0.036(3) -0.003(3) 0.001(3) 0.005(3) C10C 0.048(3) 0.044(3) 0.038(3) -0.009(3) -0.007(2) -0.005(3) C11C 0.026(3) 0.040(3) 0.057(4) 0.012(3) 0.002(2) 0.006(2) O12C 0.0245(17) 0.035(2) 0.049(2) 0.0036(17) -0.0004(14) -0.0027(15) C13C 0.026(3) 0.038(3) 0.068(4) 0.013(3) 0.002(2) -0.006(2) C14C 0.039(4) 0.085(6) 0.074(5) 0.025(4) 0.003(3) -0.014(3) C15C 0.053(4) 0.131(8) 0.062(4) 0.038(5) 0.004(3) -0.029(4) O16C 0.040(2) 0.100(4) 0.046(2) 0.017(2) 0.0047(18) -0.016(2) C17C 0.042(3) 0.059(4) 0.062(4) 0.009(3) -0.004(3) -0.006(3) O18C 0.065(3) 0.046(3) 0.079(3) -0.003(2) -0.012(2) 0.003(2) C19C 0.107(7) 0.069(6) 0.100(6) -0.025(5) -0.023(5) 0.026(5) Fe1D 0.0442(4) 0.0279(4) 0.0341(4) 0.0025(3) 0.0002(3) -0.0019(3) I1D 0.0478(2) 0.0446(2) 0.0760(3) -0.0112(2) -0.00106(19) 0.00798(19) C1D 0.037(3) 0.034(3) 0.042(3) 0.003(2) 0.001(2) -0.001(2) C2D 0.036(3) 0.030(3) 0.043(3) -0.005(2) 0.000(2) -0.005(2) C3D 0.048(3) 0.034(3) 0.034(3) -0.002(2) -0.003(2) -0.008(2) C4D 0.062(4) 0.025(3) 0.043(3) -0.007(2) 0.009(3) -0.005(3) C5D 0.053(4) 0.029(3) 0.048(3) 0.007(2) 0.008(3) 0.005(2) C6D 0.083(5) 0.077(6) 0.065(5) 0.040(4) -0.018(4) -0.031(5) C7D 0.066(5) 0.084(6) 0.045(4) -0.007(3) 0.018(3) -0.027(4) C8D 0.054(4) 0.050(4) 0.072(5) 0.010(3) -0.007(3) -0.007(3) C9D 0.079(5) 0.058(5) 0.055(4) -0.013(3) 0.014(3) -0.037(4) C10D 0.064(5) 0.021(3) 0.121(7) 0.006(4) 0.013(4) -0.004(3) C11D 0.043(3) 0.043(3) 0.039(3) -0.002(3) 0.004(2) -0.007(3) O12D 0.044(2) 0.043(2) 0.041(2) -0.0003(17) 0.0010(16) -0.0065(17) C13D 0.054(4) 0.055(4) 0.049(4) -0.008(3) -0.001(3) -0.014(3) C14D 0.112(7) 0.100(7) 0.034(4) 0.007(4) -0.014(4) -0.043(5) C15D 0.115(7) 0.158(10) 0.033(4) -0.006(5) 0.011(4) -0.088(7) O16D 0.071(3) 0.085(4) 0.038(2) 0.001(2) 0.0051(19) -0.046(3) C17D 0.065(5) 0.081(6) 0.090(6) -0.032(5) -0.014(4) 0.002(4) O18D 0.065(4) 0.072(5) 0.273(10) -0.024(5) 0.056(5) -0.019(3) C19D 0.085(7) 0.160(12) 0.137(9) 0.052(9) 0.012(6) 0.022(7) _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 Fe1A C2A 2.009(6) . ? Fe1A C8A 2.011(7) . ? Fe1A C7A 2.013(7) . ? Fe1A C1A 2.019(5) . ? Fe1A C6A 2.042(7) . ? Fe1A C3A 2.042(6) . ? Fe1A C4A 2.042(6) . ? Fe1A C5A 2.051(6) . ? Fe1A C10A 2.051(7) . ? Fe1A C9A 2.056(7) . ? I1A C2A 2.086(6) . ? C1A C5A 1.399(9) . ? C1A C2A 1.414(8) . ? C1A C11A 1.492(8) . ? C2A C3A 1.432(9) . ? C3A C4A 1.404(10) . ? C4A C5A 1.445(8) . ? C6A C10A 1.360(12) . ? C6A C7A 1.393(13) . ? C7A C8A 1.439(12) . ? C8A C9A 1.408(11) . ? C9A C10A 1.400(10) . ? C11A O12A 1.411(7) . ? C11A O16A 1.417(8) . ? O12A C13A 1.432(7) . ? C13A C17A 1.494(9) . ? C13A C14A 1.543(10) . ? C14A C15A 1.507(10) . ? C15A O16A 1.442(8) . ? C17A O18A 1.397(9) . ? O18A C19A 1.408(8) . ? Fe1B C9B 2.013(8) . ? Fe1B C1B 2.021(6) . ? Fe1B C2B 2.025(7) . ? Fe1B C10B 2.028(7) . ? Fe1B C8B 2.030(7) . ? Fe1B C5B 2.029(6) . ? Fe1B C3B 2.041(6) . ? Fe1B C7B 2.055(9) . ? Fe1B C6B 2.056(10) . ? Fe1B C4B 2.058(6) . ? I1B C2B 2.093(7) . ? C1B C5B 1.413(9) . ? C1B C2B 1.422(8) . ? C1B C11B 1.493(9) . ? C2B C3B 1.412(9) . ? C3B C4B 1.414(10) . ? C4B C5B 1.426(8) . ? C6B C7B 1.335(13) . ? C6B C10B 1.399(14) . ? C7B C8B 1.365(13) . ? C8B C9B 1.447(13) . ? C9B C10B 1.448(13) . ? C11B O16B 1.415(7) . ? C11B O12B 1.425(7) . ? O12B C13B 1.416(7) . ? C13B C17B 1.488(11) . ? C13B C14B 1.516(11) . ? C14B C15B 1.500(13) . ? C15B O16B 1.433(9) . ? C17B O18B 1.418(12) . ? O18B C19B 1.323(12) . ? Fe1C C1C 2.018(5) . ? Fe1C C10C 2.024(5) . ? Fe1C C2C 2.025(5) . ? Fe1C C6C 2.034(6) . ? Fe1C C3C 2.034(5) . ? Fe1C C4C 2.037(5) . ? Fe1C C9C 2.048(6) . ? Fe1C C8C 2.047(6) . ? Fe1C C7C 2.049(5) . ? Fe1C C5C 2.049(5) . ? I1CA C2C 2.088(6) . ? C1C C5C 1.428(8) . ? C1C C2C 1.428(7) . ? C1C C11C 1.494(8) . ? C2C C3C 1.421(8) . ? C3C C4C 1.409(8) . ? C4C C5C 1.409(8) . ? C6C C10C 1.408(8) . ? C6C C7C 1.408(9) . ? C7C C8C 1.414(9) . ? C8C C9C 1.422(9) . ? C9C C10C 1.402(8) . ? C11C O12C 1.389(6) . ? C11C O16C 1.424(7) . ? O12C C13C 1.436(6) . ? C13C C14C 1.507(9) . ? C13C C17C 1.522(8) . ? C14C C15C 1.500(10) . ? C15C O16C 1.461(8) . ? C17C O18C 1.405(8) . ? O18C C19C 1.382(9) . ? Fe1D C10D 2.017(6) . ? Fe1D C6D 2.018(7) . ? Fe1D C2D 2.020(5) . ? Fe1D C8D 2.023(7) . ? Fe1D C1D 2.027(5) . ? Fe1D C9D 2.030(6) . ? Fe1D C3D 2.036(5) . ? Fe1D C7D 2.041(6) . ? Fe1D C5D 2.041(6) . ? Fe1D C4D 2.060(5) . ? I1D C2D 2.088(5) . ? C1D C5D 1.430(8) . ? C1D C2D 1.433(7) . ? C1D C11D 1.473(8) . ? C2D C3D 1.417(8) . ? C3D C4D 1.397(8) . ? C4D C5D 1.422(8) . ? C6D C10D 1.359(11) . ? C6D C7D 1.381(11) . ? C7D C8D 1.403(9) . ? C8D C9D 1.399(10) . ? C9D C10D 1.423(11) . ? C11D O12D 1.403(6) . ? C11D O16D 1.409(7) . ? O12D C13D 1.443(7) . ? C13D C14D 1.491(10) . ? C13D C17D 1.495(9) . ? C14D C15D 1.514(11) . ? C15D O16D 1.449(8) . ? C17D O18D 1.453(11) . ? O18D C19D 1.264(11) . ? 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 C2A Fe1A C8A 121.7(3) . . ? C2A Fe1A C7A 109.9(3) . . ? C8A Fe1A C7A 41.9(4) . . ? C2A Fe1A C1A 41.1(2) . . ? C8A Fe1A C1A 108.3(3) . . ? C7A Fe1A C1A 128.7(4) . . ? C2A Fe1A C6A 127.5(3) . . ? C8A Fe1A C6A 69.1(3) . . ? C7A Fe1A C6A 40.2(4) . . ? C1A Fe1A C6A 165.8(4) . . ? C2A Fe1A C3A 41.4(2) . . ? C8A Fe1A C3A 157.2(3) . . ? C7A Fe1A C3A 121.0(3) . . ? C1A Fe1A C3A 69.1(2) . . ? C6A Fe1A C3A 107.6(3) . . ? C2A Fe1A C4A 68.7(3) . . ? C8A Fe1A C4A 161.7(3) . . ? C7A Fe1A C4A 153.6(4) . . ? C1A Fe1A C4A 68.7(3) . . ? C6A Fe1A C4A 118.3(3) . . ? C3A Fe1A C4A 40.2(3) . . ? C2A Fe1A C5A 68.6(2) . . ? C8A Fe1A C5A 124.8(3) . . ? C7A Fe1A C5A 164.6(4) . . ? C1A Fe1A C5A 40.2(3) . . ? C6A Fe1A C5A 152.8(4) . . ? C3A Fe1A C5A 68.7(2) . . ? C4A Fe1A C5A 41.3(2) . . ? C2A Fe1A C10A 162.7(3) . . ? C8A Fe1A C10A 67.8(3) . . ? C7A Fe1A C10A 66.4(4) . . ? C1A Fe1A C10A 154.4(3) . . ? C6A Fe1A C10A 38.8(3) . . ? C3A Fe1A C10A 124.6(3) . . ? C4A Fe1A C10A 106.7(3) . . ? C5A Fe1A C10A 119.7(3) . . ? C2A Fe1A C9A 156.4(3) . . ? C8A Fe1A C9A 40.5(3) . . ? C7A Fe1A C9A 67.8(3) . . ? C1A Fe1A C9A 120.6(3) . . ? C6A Fe1A C9A 67.1(3) . . ? C3A Fe1A C9A 160.7(3) . . ? C4A Fe1A C9A 124.3(3) . . ? C5A Fe1A C9A 107.0(3) . . ? C10A Fe1A C9A 39.9(3) . . ? C5A C1A C2A 108.9(5) . . ? C5A C1A C11A 125.4(5) . . ? C2A C1A C11A 125.4(6) . . ? C5A C1A Fe1A 71.2(3) . . ? C2A C1A Fe1A 69.1(3) . . ? C11A C1A Fe1A 130.2(4) . . ? C1A C2A C3A 108.0(5) . . ? C1A C2A Fe1A 69.8(3) . . ? C3A C2A Fe1A 70.6(3) . . ? C1A C2A I1A 126.3(4) . . ? C3A C2A I1A 125.4(4) . . ? Fe1A C2A I1A 130.0(3) . . ? C4A C3A C2A 107.5(5) . . ? C4A C3A Fe1A 69.9(3) . . ? C2A C3A Fe1A 68.0(3) . . ? C3A C4A C5A 108.3(6) . . ? C3A C4A Fe1A 69.9(4) . . ? C5A C4A Fe1A 69.6(3) . . ? C1A C5A C4A 107.3(5) . . ? C1A C5A Fe1A 68.7(3) . . ? C4A C5A Fe1A 69.0(3) . . ? C10A C6A C7A 107.8(8) . . ? C10A C6A Fe1A 70.9(4) . . ? C7A C6A Fe1A 68.8(4) . . ? C6A C7A C8A 108.5(8) . . ? C6A C7A Fe1A 71.1(5) . . ? C8A C7A Fe1A 69.0(4) . . ? C9A C8A C7A 105.7(8) . . ? C9A C8A Fe1A 71.5(4) . . ? C7A C8A Fe1A 69.1(4) . . ? C10A C9A C8A 107.7(7) . . ? C10A C9A Fe1A 69.9(4) . . ? C8A C9A Fe1A 68.0(4) . . ? C6A C10A C9A 110.2(8) . . ? C6A C10A Fe1A 70.3(5) . . ? C9A C10A Fe1A 70.3(4) . . ? O12A C11A O16A 111.1(5) . . ? O12A C11A C1A 110.9(5) . . ? O16A C11A C1A 107.0(5) . . ? C11A O12A C13A 111.5(4) . . ? O12A C13A C17A 109.0(5) . . ? O12A C13A C14A 106.9(5) . . ? C17A C13A C14A 113.0(6) . . ? C15A C14A C13A 109.6(6) . . ? O16A C15A C14A 109.7(6) . . ? C11A O16A C15A 110.6(6) . . ? O18A C17A C13A 109.8(5) . . ? C17A O18A C19A 113.3(6) . . ? C9B Fe1B C1B 124.7(4) . . ? C9B Fe1B C2B 109.2(3) . . ? C1B Fe1B C2B 41.2(2) . . ? C9B Fe1B C10B 42.0(4) . . ? C1B Fe1B C10B 108.1(3) . . ? C2B Fe1B C10B 125.1(4) . . ? C9B Fe1B C8B 41.9(4) . . ? C1B Fe1B C8B 163.0(4) . . ? C2B Fe1B C8B 125.9(3) . . ? C10B Fe1B C8B 69.0(3) . . ? C9B Fe1B C5B 160.5(4) . . ? C1B Fe1B C5B 40.8(3) . . ? C2B Fe1B C5B 68.6(3) . . ? C10B Fe1B C5B 122.3(3) . . ? C8B Fe1B C5B 155.1(4) . . ? C9B Fe1B C3B 123.1(4) . . ? C1B Fe1B C3B 69.1(2) . . ? C2B Fe1B C3B 40.6(3) . . ? C10B Fe1B C3B 161.1(4) . . ? C8B Fe1B C3B 107.9(3) . . ? C5B Fe1B C3B 68.6(3) . . ? C9B Fe1B C7B 68.1(4) . . ? C1B Fe1B C7B 156.6(4) . . ? C2B Fe1B C7B 160.3(4) . . ? C10B Fe1B C7B 66.9(4) . . ? C8B Fe1B C7B 39.1(4) . . ? C5B Fe1B C7B 120.7(4) . . ? C3B Fe1B C7B 123.1(4) . . ? C9B Fe1B C6B 68.0(4) . . ? C1B Fe1B C6B 123.7(3) . . ? C2B Fe1B C6B 161.0(4) . . ? C10B Fe1B C6B 40.1(4) . . ? C8B Fe1B C6B 65.5(4) . . ? C5B Fe1B C6B 107.5(4) . . ? C3B Fe1B C6B 157.0(4) . . ? C7B Fe1B C6B 37.9(4) . . ? C9B Fe1B C4B 157.9(4) . . ? C1B Fe1B C4B 68.7(3) . . ? C2B Fe1B C4B 68.1(3) . . ? C10B Fe1B C4B 157.6(4) . . ? C8B Fe1B C4B 120.5(3) . . ? C5B Fe1B C4B 40.8(2) . . ? C3B Fe1B C4B 40.4(3) . . ? C7B Fe1B C4B 106.6(4) . . ? C6B Fe1B C4B 121.9(4) . . ? C5B C1B C2B 107.2(5) . . ? C5B C1B C11B 127.4(6) . . ? C2B C1B C11B 125.3(6) . . ? C5B C1B Fe1B 69.9(3) . . ? C2B C1B Fe1B 69.6(4) . . ? C11B C1B Fe1B 126.4(4) . . ? C3B C2B C1B 108.7(6) . . ? C3B C2B Fe1B 70.3(4) . . ? C1B C2B Fe1B 69.3(4) . . ? C3B C2B I1B 123.8(4) . . ? C1B C2B I1B 127.5(5) . . ? Fe1B C2B I1B 125.9(3) . . ? C4B C3B C2B 107.9(5) . . ? C4B C3B Fe1B 70.5(4) . . ? C2B C3B Fe1B 69.1(3) . . ? C3B C4B C5B 107.7(6) . . ? C3B C4B Fe1B 69.2(4) . . ? C5B C4B Fe1B 68.5(3) . . ? C1B C5B C4B 108.4(6) . . ? C1B C5B Fe1B 69.3(3) . . ? C4B C5B Fe1B 70.7(3) . . ? C7B C6B C10B 110.8(11) . . ? C7B C6B Fe1B 71.0(6) . . ? C10B C6B Fe1B 68.9(6) . . ? C6B C7B C8B 109.9(11) . . ? C6B C7B Fe1B 71.1(6) . . ? C8B C7B Fe1B 69.5(5) . . ? C7B C8B C9B 108.2(8) . . ? C7B C8B Fe1B 71.5(5) . . ? C9B C8B Fe1B 68.4(4) . . ? C8B C9B C10B 105.1(8) . . ? C8B C9B Fe1B 69.7(5) . . ? C10B C9B Fe1B 69.6(5) . . ? C6B C10B C9B 106.0(8) . . ? C6B C10B Fe1B 71.1(5) . . ? C9B C10B Fe1B 68.4(4) . . ? O16B C11B O12B 110.0(5) . . ? O16B C11B C1B 107.3(5) . . ? O12B C11B C1B 108.2(5) . . ? C13B O12B C11B 111.5(5) . . ? O12B C13B C17B 106.9(6) . . ? O12B C13B C14B 109.0(6) . . ? C17B C13B C14B 116.0(8) . . ? C15B C14B C13B 109.0(7) . . ? O16B C15B C14B 110.3(7) . . ? C11B O16B C15B 110.2(6) . . ? O18B C17B C13B 108.5(8) . . ? C19B O18B C17B 119.7(11) . . ? C1C Fe1C C10C 106.9(2) . . ? C1C Fe1C C2C 41.4(2) . . ? C10C Fe1C C2C 122.4(2) . . ? C1C Fe1C C6C 124.1(2) . . ? C10C Fe1C C6C 40.6(2) . . ? C2C Fe1C C6C 108.5(2) . . ? C1C Fe1C C3C 69.6(2) . . ? C10C Fe1C C3C 158.3(2) . . ? C2C Fe1C C3C 41.0(2) . . ? C6C Fe1C C3C 122.6(2) . . ? C1C Fe1C C4C 68.6(2) . . ? C10C Fe1C C4C 159.8(2) . . ? C2C Fe1C C4C 68.1(2) . . ? C6C Fe1C C4C 158.1(2) . . ? C3C Fe1C C4C 40.5(2) . . ? C1C Fe1C C9C 120.7(2) . . ? C10C Fe1C C9C 40.3(2) . . ? C2C Fe1C C9C 157.4(2) . . ? C6C Fe1C C9C 67.9(2) . . ? C3C Fe1C C9C 160.0(2) . . ? C4C Fe1C C9C 123.7(2) . . ? C1C Fe1C C8C 156.5(2) . . ? C10C Fe1C C8C 68.1(2) . . ? C2C Fe1C C8C 160.8(2) . . ? C6C Fe1C C8C 68.0(3) . . ? C3C Fe1C C8C 123.6(2) . . ? C4C Fe1C C8C 107.7(2) . . ? C9C Fe1C C8C 40.6(2) . . ? C1C Fe1C C7C 161.1(3) . . ? C10C Fe1C C7C 68.1(2) . . ? C2C Fe1C C7C 124.7(2) . . ? C6C Fe1C C7C 40.3(3) . . ? C3C Fe1C C7C 108.0(2) . . ? C4C Fe1C C7C 122.5(2) . . ? C9C Fe1C C7C 68.0(2) . . ? C8C Fe1C C7C 40.4(3) . . ? C1C Fe1C C5C 41.1(2) . . ? C10C Fe1C C5C 123.4(2) . . ? C2C Fe1C C5C 68.8(2) . . ? C6C Fe1C C5C 160.6(2) . . ? C3C Fe1C C5C 68.8(2) . . ? C4C Fe1C C5C 40.3(2) . . ? C9C Fe1C C5C 106.8(2) . . ? C8C Fe1C C5C 121.0(3) . . ? C7C Fe1C C5C 156.9(3) . . ? C5C C1C C2C 107.3(5) . . ? C5C C1C C11C 127.4(5) . . ? C2C C1C C11C 125.0(5) . . ? C5C C1C Fe1C 70.6(3) . . ? C2C C1C Fe1C 69.6(3) . . ? C11C C1C Fe1C 130.0(4) . . ? C3C C2C C1C 108.6(5) . . ? C3C C2C Fe1C 69.9(3) . . ? C1C C2C Fe1C 69.1(3) . . ? C3C C2C I1CA 125.1(4) . . ? C1C C2C I1CA 126.1(4) . . ? Fe1C C2C I1CA 130.2(3) . . ? C4C C3C C2C 106.9(5) . . ? C4C C3C Fe1C 69.9(3) . . ? C2C C3C Fe1C 69.1(3) . . ? C5C C4C C3C 109.9(5) . . ? C5C C4C Fe1C 70.3(3) . . ? C3C C4C Fe1C 69.6(3) . . ? C4C C5C C1C 107.3(5) . . ? C4C C5C Fe1C 69.4(3) . . ? C1C C5C Fe1C 68.3(3) . . ? C10C C6C C7C 108.1(6) . . ? C10C C6C Fe1C 69.3(3) . . ? C7C C6C Fe1C 70.4(3) . . ? C6C C7C C8C 107.9(5) . . ? C6C C7C Fe1C 69.3(3) . . ? C8C C7C Fe1C 69.8(3) . . ? C7C C8C C9C 107.8(6) . . ? C7C C8C Fe1C 69.9(3) . . ? C9C C8C Fe1C 69.7(3) . . ? C10C C9C C8C 107.7(6) . . ? C10C C9C Fe1C 68.9(3) . . ? C8C C9C Fe1C 69.7(3) . . ? C9C C10C C6C 108.5(6) . . ? C9C C10C Fe1C 70.8(3) . . ? C6C C10C Fe1C 70.1(3) . . ? O12C C11C O16C 111.3(4) . . ? O12C C11C C1C 110.9(4) . . ? O16C C11C C1C 106.0(5) . . ? C11C O12C C13C 110.8(4) . . ? O12C C13C C14C 108.9(5) . . ? O12C C13C C17C 108.1(4) . . ? C14C C13C C17C 112.1(5) . . ? C15C C14C C13C 110.0(6) . . ? O16C C15C C14C 109.1(6) . . ? C11C O16C C15C 110.2(5) . . ? O18C C17C C13C 114.7(5) . . ? C19C O18C C17C 116.0(6) . . ? C10D Fe1D C6D 39.4(3) . . ? C10D Fe1D C2D 108.8(3) . . ? C6D Fe1D C2D 124.4(3) . . ? C10D Fe1D C8D 67.5(3) . . ? C6D Fe1D C8D 66.9(3) . . ? C2D Fe1D C8D 158.9(3) . . ? C10D Fe1D C1D 123.1(3) . . ? C6D Fe1D C1D 159.4(3) . . ? C2D Fe1D C1D 41.5(2) . . ? C8D Fe1D C1D 121.6(2) . . ? C10D Fe1D C9D 41.2(3) . . ? C6D Fe1D C9D 67.8(3) . . ? C2D Fe1D C9D 123.0(3) . . ? C8D Fe1D C9D 40.4(3) . . ? C1D Fe1D C9D 105.7(2) . . ? C10D Fe1D C3D 123.6(3) . . ? C6D Fe1D C3D 109.0(3) . . ? C2D Fe1D C3D 40.9(2) . . ? C8D Fe1D C3D 158.7(3) . . ? C1D Fe1D C3D 69.9(2) . . ? C9D Fe1D C3D 159.6(3) . . ? C10D Fe1D C7D 67.2(3) . . ? C6D Fe1D C7D 39.8(3) . . ? C2D Fe1D C7D 159.4(3) . . ? C8D Fe1D C7D 40.4(3) . . ? C1D Fe1D C7D 158.0(3) . . ? C9D Fe1D C7D 68.4(3) . . ? C3D Fe1D C7D 122.9(2) . . ? C10D Fe1D C5D 159.7(3) . . ? C6D Fe1D C5D 158.8(3) . . ? C2D Fe1D C5D 68.2(2) . . ? C8D Fe1D C5D 107.7(3) . . ? C1D Fe1D C5D 41.2(2) . . ? C9D Fe1D C5D 122.3(3) . . ? C3D Fe1D C5D 68.2(2) . . ? C7D Fe1D C5D 122.8(3) . . ? C10D Fe1D C4D 158.6(3) . . ? C6D Fe1D C4D 123.8(3) . . ? C2D Fe1D C4D 67.7(2) . . ? C8D Fe1D C4D 123.5(3) . . ? C1D Fe1D C4D 69.3(2) . . ? C9D Fe1D C4D 158.8(3) . . ? C3D Fe1D C4D 39.9(2) . . ? C7D Fe1D C4D 108.1(3) . . ? C5D Fe1D C4D 40.6(2) . . ? C5D C1D C2D 105.3(5) . . ? C5D C1D C11D 127.5(5) . . ? C2D C1D C11D 127.1(5) . . ? C5D C1D Fe1D 70.0(3) . . ? C2D C1D Fe1D 69.0(3) . . ? C11D C1D Fe1D 128.1(4) . . ? C3D C2D C1D 109.6(5) . . ? C3D C2D Fe1D 70.1(3) . . ? C1D C2D Fe1D 69.5(3) . . ? C3D C2D I1D 124.2(4) . . ? C1D C2D I1D 126.2(4) . . ? Fe1D C2D I1D 127.4(3) . . ? C4D C3D C2D 107.8(5) . . ? C4D C3D Fe1D 71.0(3) . . ? C2D C3D Fe1D 69.0(3) . . ? C3D C4D C5D 108.3(5) . . ? C3D C4D Fe1D 69.1(3) . . ? C5D C4D Fe1D 69.0(3) . . ? C4D C5D C1D 109.1(5) . . ? C4D C5D Fe1D 70.4(3) . . ? C1D C5D Fe1D 68.9(3) . . ? C10D C6D C7D 110.2(6) . . ? C10D C6D Fe1D 70.3(4) . . ? C7D C6D Fe1D 71.0(4) . . ? C6D C7D C8D 106.3(7) . . ? C6D C7D Fe1D 69.2(4) . . ? C8D C7D Fe1D 69.1(4) . . ? C9D C8D C7D 109.5(7) . . ? C9D C8D Fe1D 70.1(4) . . ? C7D C8D Fe1D 70.5(4) . . ? C8D C9D C10D 105.4(6) . . ? C8D C9D Fe1D 69.5(4) . . ? C10D C9D Fe1D 68.9(4) . . ? C6D C10D C9D 108.5(7) . . ? C6D C10D Fe1D 70.3(4) . . ? C9D C10D Fe1D 69.9(4) . . ? O12D C11D O16D 110.7(5) . . ? O12D C11D C1D 109.3(4) . . ? O16D C11D C1D 108.0(4) . . ? C11D O12D C13D 111.4(4) . . ? O12D C13D C14D 109.4(5) . . ? O12D C13D C17D 108.3(6) . . ? C14D C13D C17D 115.8(7) . . ? C13D C14D C15D 108.9(6) . . ? O16D C15D C14D 108.9(7) . . ? C11D O16D C15D 110.7(5) . . ? O18D C17D C13D 109.3(7) . . ? C19D O18D C17D 121.0(8) . . ? 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 C2A Fe1A C1A C5A 119.8(5) . . . . ? C8A Fe1A C1A C5A -122.7(4) . . . . ? C7A Fe1A C1A C5A -165.0(4) . . . . ? C6A Fe1A C1A C5A 160.4(12) . . . . ? C3A Fe1A C1A C5A 81.4(4) . . . . ? C4A Fe1A C1A C5A 38.1(4) . . . . ? C10A Fe1A C1A C5A -46.0(8) . . . . ? C9A Fe1A C1A C5A -80.0(4) . . . . ? C8A Fe1A C1A C2A 117.5(4) . . . . ? C7A Fe1A C1A C2A 75.2(5) . . . . ? C6A Fe1A C1A C2A 40.6(13) . . . . ? C3A Fe1A C1A C2A -38.4(4) . . . . ? C4A Fe1A C1A C2A -81.7(4) . . . . ? C5A Fe1A C1A C2A -119.8(5) . . . . ? C10A Fe1A C1A C2A -165.8(6) . . . . ? C9A Fe1A C1A C2A 160.2(4) . . . . ? C2A Fe1A C1A C11A -119.3(7) . . . . ? C8A Fe1A C1A C11A -1.8(7) . . . . ? C7A Fe1A C1A C11A -44.1(7) . . . . ? C6A Fe1A C1A C11A -78.7(14) . . . . ? C3A Fe1A C1A C11A -157.7(7) . . . . ? C4A Fe1A C1A C11A 159.0(7) . . . . ? C5A Fe1A C1A C11A 120.9(7) . . . . ? C10A Fe1A C1A C11A 74.9(9) . . . . ? C9A Fe1A C1A C11A 40.9(7) . . . . ? C5A C1A C2A C3A 0.3(6) . . . . ? C11A C1A C2A C3A -174.3(5) . . . . ? Fe1A C1A C2A C3A 60.5(4) . . . . ? C5A C1A C2A Fe1A -60.2(4) . . . . ? C11A C1A C2A Fe1A 125.2(6) . . . . ? C5A C1A C2A I1A 174.4(4) . . . . ? C11A C1A C2A I1A -0.2(8) . . . . ? Fe1A C1A C2A I1A -125.4(4) . . . . ? C8A Fe1A C2A C1A -81.6(5) . . . . ? C7A Fe1A C2A C1A -126.7(5) . . . . ? C6A Fe1A C2A C1A -168.4(5) . . . . ? C3A Fe1A C2A C1A 118.6(5) . . . . ? C4A Fe1A C2A C1A 81.5(4) . . . . ? C5A Fe1A C2A C1A 37.0(4) . . . . ? C10A Fe1A C2A C1A 159.0(10) . . . . ? C9A Fe1A C2A C1A -46.7(8) . . . . ? C8A Fe1A C2A C3A 159.8(4) . . . . ? C7A Fe1A C2A C3A 114.7(5) . . . . ? C1A Fe1A C2A C3A -118.6(5) . . . . ? C6A Fe1A C2A C3A 73.0(5) . . . . ? C4A Fe1A C2A C3A -37.1(4) . . . . ? C5A Fe1A C2A C3A -81.6(4) . . . . ? C10A Fe1A C2A C3A 40.4(12) . . . . ? C9A Fe1A C2A C3A -165.3(7) . . . . ? C8A Fe1A C2A I1A 39.4(5) . . . . ? C7A Fe1A C2A I1A -5.7(5) . . . . ? C1A Fe1A C2A I1A 121.0(5) . . . . ? C6A Fe1A C2A I1A -47.4(6) . . . . ? C3A Fe1A C2A I1A -120.4(5) . . . . ? C4A Fe1A C2A I1A -157.5(4) . . . . ? C5A Fe1A C2A I1A 158.0(4) . . . . ? C10A Fe1A C2A I1A -80.0(11) . . . . ? C9A Fe1A C2A I1A 74.3(8) . . . . ? C1A C2A C3A C4A -1.1(6) . . . . ? Fe1A C2A C3A C4A 59.0(4) . . . . ? I1A C2A C3A C4A -175.2(4) . . . . ? C1A C2A C3A Fe1A -60.1(4) . . . . ? I1A C2A C3A Fe1A 125.8(4) . . . . ? C2A Fe1A C3A C4A -119.5(5) . . . . ? C8A Fe1A C3A C4A -168.9(7) . . . . ? C7A Fe1A C3A C4A 155.2(5) . . . . ? C1A Fe1A C3A C4A -81.4(4) . . . . ? C6A Fe1A C3A C4A 113.3(5) . . . . ? C5A Fe1A C3A C4A -38.1(4) . . . . ? C10A Fe1A C3A C4A 74.0(5) . . . . ? C9A Fe1A C3A C4A 42.5(10) . . . . ? C8A Fe1A C3A C2A -49.3(8) . . . . ? C7A Fe1A C3A C2A -85.3(5) . . . . ? C1A Fe1A C3A C2A 38.2(3) . . . . ? C6A Fe1A C3A C2A -127.2(4) . . . . ? C4A Fe1A C3A C2A 119.5(5) . . . . ? C5A Fe1A C3A C2A 81.4(4) . . . . ? C10A Fe1A C3A C2A -166.5(4) . . . . ? C9A Fe1A C3A C2A 162.1(8) . . . . ? C2A C3A C4A C5A 1.5(6) . . . . ? Fe1A C3A C4A C5A 59.3(4) . . . . ? C2A C3A C4A Fe1A -57.8(4) . . . . ? C2A Fe1A C4A C3A 38.1(4) . . . . ? C8A Fe1A C4A C3A 166.2(9) . . . . ? C7A Fe1A C4A C3A -54.0(9) . . . . ? C1A Fe1A C4A C3A 82.4(4) . . . . ? C6A Fe1A C4A C3A -84.0(5) . . . . ? C5A Fe1A C4A C3A 119.5(5) . . . . ? C10A Fe1A C4A C3A -124.3(4) . . . . ? C9A Fe1A C4A C3A -164.3(4) . . . . ? C2A Fe1A C4A C5A -81.4(4) . . . . ? C8A Fe1A C4A C5A 46.7(11) . . . . ? C7A Fe1A C4A C5A -173.5(7) . . . . ? C1A Fe1A C4A C5A -37.1(4) . . . . ? C6A Fe1A C4A C5A 156.5(4) . . . . ? C3A Fe1A C4A C5A -119.5(5) . . . . ? C10A Fe1A C4A C5A 116.2(4) . . . . ? C9A Fe1A C4A C5A 76.2(5) . . . . ? C2A C1A C5A C4A 0.6(6) . . . . ? C11A C1A C5A C4A 175.2(5) . . . . ? Fe1A C1A C5A C4A -58.4(4) . . . . ? C2A C1A C5A Fe1A 59.0(4) . . . . ? C11A C1A C5A Fe1A -126.5(6) . . . . ? C3A C4A C5A C1A -1.3(6) . . . . ? Fe1A C4A C5A C1A 58.1(4) . . . . ? C3A C4A C5A Fe1A -59.4(4) . . . . ? C2A Fe1A C5A C1A -37.8(3) . . . . ? C8A Fe1A C5A C1A 76.7(5) . . . . ? C7A Fe1A C5A C1A 49.6(13) . . . . ? C6A Fe1A C5A C1A -169.6(6) . . . . ? C3A Fe1A C5A C1A -82.4(4) . . . . ? C4A Fe1A C5A C1A -119.5(5) . . . . ? C10A Fe1A C5A C1A 159.0(4) . . . . ? C9A Fe1A C5A C1A 117.6(4) . . . . ? C2A Fe1A C5A C4A 81.7(4) . . . . ? C8A Fe1A C5A C4A -163.9(4) . . . . ? C7A Fe1A C5A C4A 169.1(11) . . . . ? C1A Fe1A C5A C4A 119.5(5) . . . . ? C6A Fe1A C5A C4A -50.1(8) . . . . ? C3A Fe1A C5A C4A 37.1(4) . . . . ? C10A Fe1A C5A C4A -81.5(5) . . . . ? C9A Fe1A C5A C4A -122.9(4) . . . . ? C2A Fe1A C6A C10A -165.2(4) . . . . ? C8A Fe1A C6A C10A 80.3(6) . . . . ? C7A Fe1A C6A C10A 118.8(8) . . . . ? C1A Fe1A C6A C10A 162.1(10) . . . . ? C3A Fe1A C6A C10A -123.7(5) . . . . ? C4A Fe1A C6A C10A -81.3(6) . . . . ? C5A Fe1A C6A C10A -46.2(9) . . . . ? C9A Fe1A C6A C10A 36.5(5) . . . . ? C2A Fe1A C6A C7A 76.0(6) . . . . ? C8A Fe1A C6A C7A -38.5(5) . . . . ? C1A Fe1A C6A C7A 43.3(14) . . . . ? C3A Fe1A C6A C7A 117.5(5) . . . . ? C4A Fe1A C6A C7A 159.9(5) . . . . ? C5A Fe1A C6A C7A -164.9(6) . . . . ? C10A Fe1A C6A C7A -118.8(8) . . . . ? C9A Fe1A C6A C7A -82.3(6) . . . . ? C10A C6A C7A C8A -1.4(8) . . . . ? Fe1A C6A C7A C8A 59.0(5) . . . . ? C10A C6A C7A Fe1A -60.5(5) . . . . ? C2A Fe1A C7A C6A -125.0(5) . . . . ? C8A Fe1A C7A C6A 119.4(7) . . . . ? C1A Fe1A C7A C6A -167.5(5) . . . . ? C3A Fe1A C7A C6A -80.5(6) . . . . ? C4A Fe1A C7A C6A -43.0(10) . . . . ? C5A Fe1A C7A C6A 153.4(11) . . . . ? C10A Fe1A C7A C6A 36.8(5) . . . . ? C9A Fe1A C7A C6A 80.2(6) . . . . ? C2A Fe1A C7A C8A 115.6(5) . . . . ? C1A Fe1A C7A C8A 73.1(6) . . . . ? C6A Fe1A C7A C8A -119.4(7) . . . . ? C3A Fe1A C7A C8A 160.1(5) . . . . ? C4A Fe1A C7A C8A -162.4(6) . . . . ? C5A Fe1A C7A C8A 34.0(14) . . . . ? C10A Fe1A C7A C8A -82.6(5) . . . . ? C9A Fe1A C7A C8A -39.2(5) . . . . ? C6A C7A C8A C9A 2.2(8) . . . . ? Fe1A C7A C8A C9A 62.5(5) . . . . ? C6A C7A C8A Fe1A -60.3(5) . . . . ? C2A Fe1A C8A C9A 159.3(4) . . . . ? C7A Fe1A C8A C9A -115.7(7) . . . . ? C1A Fe1A C8A C9A 116.1(5) . . . . ? C6A Fe1A C8A C9A -78.7(5) . . . . ? C3A Fe1A C8A C9A -164.6(6) . . . . ? C4A Fe1A C8A C9A 38.8(12) . . . . ? C5A Fe1A C8A C9A 74.7(5) . . . . ? C10A Fe1A C8A C9A -36.9(5) . . . . ? C2A Fe1A C8A C7A -85.0(6) . . . . ? C1A Fe1A C8A C7A -128.2(5) . . . . ? C6A Fe1A C8A C7A 37.0(5) . . . . ? C3A Fe1A C8A C7A -48.9(10) . . . . ? C4A Fe1A C8A C7A 154.6(9) . . . . ? C5A Fe1A C8A C7A -169.6(5) . . . . ? C10A Fe1A C8A C7A 78.8(6) . . . . ? C9A Fe1A C8A C7A 115.7(7) . . . . ? C7A C8A C9A C10A -2.1(8) . . . . ? Fe1A C8A C9A C10A 58.8(5) . . . . ? C7A C8A C9A Fe1A -61.0(4) . . . . ? C2A Fe1A C9A C10A -168.4(6) . . . . ? C8A Fe1A C9A C10A -119.8(7) . . . . ? C7A Fe1A C9A C10A -79.2(6) . . . . ? C1A Fe1A C9A C10A 157.8(5) . . . . ? C6A Fe1A C9A C10A -35.6(5) . . . . ? C3A Fe1A C9A C10A 42.1(11) . . . . ? C4A Fe1A C9A C10A 74.0(6) . . . . ? C5A Fe1A C9A C10A 116.2(5) . . . . ? C2A Fe1A C9A C8A -48.7(9) . . . . ? C7A Fe1A C9A C8A 40.5(5) . . . . ? C1A Fe1A C9A C8A -82.4(5) . . . . ? C6A Fe1A C9A C8A 84.2(6) . . . . ? C3A Fe1A C9A C8A 161.9(7) . . . . ? C4A Fe1A C9A C8A -166.2(4) . . . . ? C5A Fe1A C9A C8A -124.1(5) . . . . ? C10A Fe1A C9A C8A 119.8(7) . . . . ? C7A C6A C10A C9A 0.1(8) . . . . ? Fe1A C6A C10A C9A -59.0(5) . . . . ? C7A C6A C10A Fe1A 59.1(5) . . . . ? C8A C9A C10A C6A 1.4(8) . . . . ? Fe1A C9A C10A C6A 59.0(5) . . . . ? C8A C9A C10A Fe1A -57.7(5) . . . . ? C2A Fe1A C10A C6A 43.0(13) . . . . ? C8A Fe1A C10A C6A -83.8(6) . . . . ? C7A Fe1A C10A C6A -38.1(6) . . . . ? C1A Fe1A C10A C6A -170.0(6) . . . . ? C3A Fe1A C10A C6A 74.4(6) . . . . ? C4A Fe1A C10A C6A 114.7(6) . . . . ? C5A Fe1A C10A C6A 157.7(5) . . . . ? C9A Fe1A C10A C6A -121.3(8) . . . . ? C2A Fe1A C10A C9A 164.3(9) . . . . ? C8A Fe1A C10A C9A 37.5(5) . . . . ? C7A Fe1A C10A C9A 83.2(6) . . . . ? C1A Fe1A C10A C9A -48.7(9) . . . . ? C6A Fe1A C10A C9A 121.3(8) . . . . ? C3A Fe1A C10A C9A -164.4(4) . . . . ? C4A Fe1A C10A C9A -124.0(5) . . . . ? C5A Fe1A C10A C9A -81.0(5) . . . . ? C5A C1A C11A O12A 58.8(8) . . . . ? C2A C1A C11A O12A -127.5(6) . . . . ? Fe1A C1A C11A O12A -36.0(8) . . . . ? C5A C1A C11A O16A -62.5(7) . . . . ? C2A C1A C11A O16A 111.2(6) . . . . ? Fe1A C1A C11A O16A -157.3(5) . . . . ? O16A C11A O12A C13A -64.3(7) . . . . ? C1A C11A O12A C13A 176.8(5) . . . . ? C11A O12A C13A C17A -177.6(5) . . . . ? C11A O12A C13A C14A 60.0(6) . . . . ? O12A C13A C14A C15A -55.5(8) . . . . ? C17A C13A C14A C15A -175.5(6) . . . . ? C13A C14A C15A O16A 54.9(9) . . . . ? O12A C11A O16A C15A 61.3(7) . . . . ? C1A C11A O16A C15A -177.5(5) . . . . ? C14A C15A O16A C11A -57.1(9) . . . . ? O12A C13A C17A O18A 64.5(7) . . . . ? C14A C13A C17A O18A -176.8(6) . . . . ? C13A C17A O18A C19A -177.5(6) . . . . ? C9B Fe1B C1B C5B -162.3(5) . . . . ? C2B Fe1B C1B C5B 118.2(5) . . . . ? C10B Fe1B C1B C5B -118.7(5) . . . . ? C8B Fe1B C1B C5B 164.0(10) . . . . ? C3B Fe1B C1B C5B 81.1(4) . . . . ? C7B Fe1B C1B C5B -45.1(10) . . . . ? C6B Fe1B C1B C5B -77.3(6) . . . . ? C4B Fe1B C1B C5B 37.7(4) . . . . ? C9B Fe1B C1B C2B 79.4(5) . . . . ? C10B Fe1B C1B C2B 123.0(5) . . . . ? C8B Fe1B C1B C2B 45.7(11) . . . . ? C5B Fe1B C1B C2B -118.2(5) . . . . ? C3B Fe1B C1B C2B -37.2(4) . . . . ? C7B Fe1B C1B C2B -163.3(9) . . . . ? C6B Fe1B C1B C2B 164.5(5) . . . . ? C4B Fe1B C1B C2B -80.5(4) . . . . ? C9B Fe1B C1B C11B -40.1(7) . . . . ? C2B Fe1B C1B C11B -119.5(7) . . . . ? C10B Fe1B C1B C11B 3.5(7) . . . . ? C8B Fe1B C1B C11B -73.8(12) . . . . ? C5B Fe1B C1B C11B 122.3(7) . . . . ? C3B Fe1B C1B C11B -156.6(6) . . . . ? C7B Fe1B C1B C11B 77.2(11) . . . . ? C6B Fe1B C1B C11B 45.0(8) . . . . ? C4B Fe1B C1B C11B 160.0(6) . . . . ? C5B C1B C2B C3B -0.6(7) . . . . ? C11B C1B C2B C3B -179.8(6) . . . . ? Fe1B C1B C2B C3B 59.4(5) . . . . ? C5B C1B C2B Fe1B -60.0(4) . . . . ? C11B C1B C2B Fe1B 120.8(6) . . . . ? C5B C1B C2B I1B -180.0(4) . . . . ? C11B C1B C2B I1B 0.8(9) . . . . ? Fe1B C1B C2B I1B -120.0(5) . . . . ? C9B Fe1B C2B C3B 118.9(5) . . . . ? C1B Fe1B C2B C3B -120.0(5) . . . . ? C10B Fe1B C2B C3B 163.1(4) . . . . ? C8B Fe1B C2B C3B 74.9(5) . . . . ? C5B Fe1B C2B C3B -81.8(4) . . . . ? C7B Fe1B C2B C3B 40.3(12) . . . . ? C6B Fe1B C2B C3B -163.1(11) . . . . ? C4B Fe1B C2B C3B -37.6(4) . . . . ? C9B Fe1B C2B C1B -121.1(5) . . . . ? C10B Fe1B C2B C1B -76.9(5) . . . . ? C8B Fe1B C2B C1B -165.1(4) . . . . ? C5B Fe1B C2B C1B 38.2(4) . . . . ? C3B Fe1B C2B C1B 120.0(5) . . . . ? C7B Fe1B C2B C1B 160.3(10) . . . . ? C6B Fe1B C2B C1B -43.1(12) . . . . ? C4B Fe1B C2B C1B 82.4(4) . . . . ? C9B Fe1B C2B I1B 0.8(6) . . . . ? C1B Fe1B C2B I1B 121.9(6) . . . . ? C10B Fe1B C2B I1B 45.0(5) . . . . ? C8B Fe1B C2B I1B -43.1(6) . . . . ? C5B Fe1B C2B I1B 160.2(4) . . . . ? C3B Fe1B C2B I1B -118.1(5) . . . . ? C7B Fe1B C2B I1B -77.8(12) . . . . ? C6B Fe1B C2B I1B 78.8(12) . . . . ? C4B Fe1B C2B I1B -155.7(4) . . . . ? C1B C2B C3B C4B 1.2(7) . . . . ? Fe1B C2B C3B C4B 60.0(4) . . . . ? I1B C2B C3B C4B -179.4(4) . . . . ? C1B C2B C3B Fe1B -58.8(4) . . . . ? I1B C2B C3B Fe1B 120.6(5) . . . . ? C9B Fe1B C3B C4B 160.1(5) . . . . ? C1B Fe1B C3B C4B -81.4(4) . . . . ? C2B Fe1B C3B C4B -119.0(5) . . . . ? C10B Fe1B C3B C4B -166.4(8) . . . . ? C8B Fe1B C3B C4B 116.3(5) . . . . ? C5B Fe1B C3B C4B -37.4(4) . . . . ? C7B Fe1B C3B C4B 76.1(5) . . . . ? C6B Fe1B C3B C4B 47.0(10) . . . . ? C9B Fe1B C3B C2B -81.0(5) . . . . ? C1B Fe1B C3B C2B 37.6(4) . . . . ? C10B Fe1B C3B C2B -47.4(10) . . . . ? C8B Fe1B C3B C2B -124.7(5) . . . . ? C5B Fe1B C3B C2B 81.5(4) . . . . ? C7B Fe1B C3B C2B -164.9(5) . . . . ? C6B Fe1B C3B C2B 166.0(8) . . . . ? C4B Fe1B C3B C2B 119.0(5) . . . . ? C2B C3B C4B C5B -1.4(7) . . . . ? Fe1B C3B C4B C5B 57.7(4) . . . . ? C2B C3B C4B Fe1B -59.1(4) . . . . ? C9B Fe1B C4B C3B -49.3(11) . . . . ? C1B Fe1B C4B C3B 82.3(4) . . . . ? C2B Fe1B C4B C3B 37.9(4) . . . . ? C10B Fe1B C4B C3B 168.5(8) . . . . ? C8B Fe1B C4B C3B -81.8(5) . . . . ? C5B Fe1B C4B C3B 120.0(6) . . . . ? C7B Fe1B C4B C3B -121.9(5) . . . . ? C6B Fe1B C4B C3B -160.3(5) . . . . ? C9B Fe1B C4B C5B -169.3(9) . . . . ? C1B Fe1B C4B C5B -37.7(4) . . . . ? C2B Fe1B C4B C5B -82.1(4) . . . . ? C10B Fe1B C4B C5B 48.4(10) . . . . ? C8B Fe1B C4B C5B 158.1(5) . . . . ? C3B Fe1B C4B C5B -120.0(6) . . . . ? C7B Fe1B C4B C5B 118.0(5) . . . . ? C6B Fe1B C4B C5B 79.6(5) . . . . ? C2B C1B C5B C4B -0.3(7) . . . . ? C11B C1B C5B C4B 178.9(6) . . . . ? Fe1B C1B C5B C4B -60.1(4) . . . . ? C2B C1B C5B Fe1B 59.8(4) . . . . ? C11B C1B C5B Fe1B -121.0(6) . . . . ? C3B C4B C5B C1B 1.1(7) . . . . ? Fe1B C4B C5B C1B 59.2(4) . . . . ? C3B C4B C5B Fe1B -58.2(4) . . . . ? C9B Fe1B C5B C1B 48.6(11) . . . . ? C2B Fe1B C5B C1B -38.5(4) . . . . ? C10B Fe1B C5B C1B 80.3(5) . . . . ? C8B Fe1B C5B C1B -169.0(7) . . . . ? C3B Fe1B C5B C1B -82.4(4) . . . . ? C7B Fe1B C5B C1B 160.9(5) . . . . ? C6B Fe1B C5B C1B 121.7(5) . . . . ? C4B Fe1B C5B C1B -119.4(5) . . . . ? C9B Fe1B C5B C4B 167.9(10) . . . . ? C1B Fe1B C5B C4B 119.4(5) . . . . ? C2B Fe1B C5B C4B 80.8(4) . . . . ? C10B Fe1B C5B C4B -160.3(5) . . . . ? C8B Fe1B C5B C4B -49.6(9) . . . . ? C3B Fe1B C5B C4B 37.0(4) . . . . ? C7B Fe1B C5B C4B -79.7(5) . . . . ? C6B Fe1B C5B C4B -118.9(5) . . . . ? C9B Fe1B C6B C7B -82.2(7) . . . . ? C1B Fe1B C6B C7B 159.8(6) . . . . ? C2B Fe1B C6B C7B -167.4(9) . . . . ? C10B Fe1B C6B C7B -122.4(9) . . . . ? C8B Fe1B C6B C7B -36.5(6) . . . . ? C5B Fe1B C6B C7B 117.9(7) . . . . ? C3B Fe1B C6B C7B 41.5(13) . . . . ? C4B Fe1B C6B C7B 75.5(7) . . . . ? C9B Fe1B C6B C10B 40.2(6) . . . . ? C1B Fe1B C6B C10B -77.8(6) . . . . ? C2B Fe1B C6B C10B -45.0(13) . . . . ? C8B Fe1B C6B C10B 85.9(6) . . . . ? C5B Fe1B C6B C10B -119.7(5) . . . . ? C3B Fe1B C6B C10B 163.9(7) . . . . ? C7B Fe1B C6B C10B 122.4(9) . . . . ? C4B Fe1B C6B C10B -162.1(5) . . . . ? C10B C6B C7B C8B 1.4(10) . . . . ? Fe1B C6B C7B C8B 58.8(6) . . . . ? C10B C6B C7B Fe1B -57.4(6) . . . . ? C9B Fe1B C7B C6B 81.8(7) . . . . ? C1B Fe1B C7B C6B -46.2(13) . . . . ? C2B Fe1B C7B C6B 167.8(9) . . . . ? C10B Fe1B C7B C6B 36.2(7) . . . . ? C8B Fe1B C7B C6B 120.8(10) . . . . ? C5B Fe1B C7B C6B -78.8(8) . . . . ? C3B Fe1B C7B C6B -162.0(6) . . . . ? C4B Fe1B C7B C6B -121.0(7) . . . . ? C9B Fe1B C7B C8B -39.0(6) . . . . ? C1B Fe1B C7B C8B -167.0(7) . . . . ? C2B Fe1B C7B C8B 47.0(14) . . . . ? C10B Fe1B C7B C8B -84.6(6) . . . . ? C5B Fe1B C7B C8B 160.4(5) . . . . ? C3B Fe1B C7B C8B 77.2(7) . . . . ? C6B Fe1B C7B C8B -120.8(10) . . . . ? C4B Fe1B C7B C8B 118.2(6) . . . . ? C6B C7B C8B C9B -1.0(10) . . . . ? Fe1B C7B C8B C9B 58.8(6) . . . . ? C6B C7B C8B Fe1B -59.8(6) . . . . ? C9B Fe1B C8B C7B 119.1(8) . . . . ? C1B Fe1B C8B C7B 162.2(9) . . . . ? C2B Fe1B C8B C7B -162.3(6) . . . . ? C10B Fe1B C8B C7B 78.9(7) . . . . ? C5B Fe1B C8B C7B -43.2(10) . . . . ? C3B Fe1B C8B C7B -120.9(6) . . . . ? C6B Fe1B C8B C7B 35.4(6) . . . . ? C4B Fe1B C8B C7B -78.5(7) . . . . ? C1B Fe1B C8B C9B 43.1(13) . . . . ? C2B Fe1B C8B C9B 78.6(6) . . . . ? C10B Fe1B C8B C9B -40.2(6) . . . . ? C5B Fe1B C8B C9B -162.3(7) . . . . ? C3B Fe1B C8B C9B 120.0(6) . . . . ? C7B Fe1B C8B C9B -119.1(8) . . . . ? C6B Fe1B C8B C9B -83.7(6) . . . . ? C4B Fe1B C8B C9B 162.4(5) . . . . ? C7B C8B C9B C10B 0.3(9) . . . . ? Fe1B C8B C9B C10B 60.9(5) . . . . ? C7B C8B C9B Fe1B -60.7(6) . . . . ? C1B Fe1B C9B C8B -166.0(5) . . . . ? C2B Fe1B C9B C8B -122.7(5) . . . . ? C10B Fe1B C9B C8B 115.7(8) . . . . ? C5B Fe1B C9B C8B 157.4(9) . . . . ? C3B Fe1B C9B C8B -79.8(6) . . . . ? C7B Fe1B C9B C8B 36.4(5) . . . . ? C6B Fe1B C9B C8B 77.4(6) . . . . ? C4B Fe1B C9B C8B -43.9(12) . . . . ? C1B Fe1B C9B C10B 78.3(6) . . . . ? C2B Fe1B C9B C10B 121.5(5) . . . . ? C8B Fe1B C9B C10B -115.7(8) . . . . ? C5B Fe1B C9B C10B 41.7(12) . . . . ? C3B Fe1B C9B C10B 164.5(5) . . . . ? C7B Fe1B C9B C10B -79.3(6) . . . . ? C6B Fe1B C9B C10B -38.3(5) . . . . ? C4B Fe1B C9B C10B -159.6(8) . . . . ? C7B C6B C10B C9B -1.2(9) . . . . ? Fe1B C6B C10B C9B -59.8(5) . . . . ? C7B C6B C10B Fe1B 58.7(6) . . . . ? C8B C9B C10B C6B 0.5(8) . . . . ? Fe1B C9B C10B C6B 61.5(6) . . . . ? C8B C9B C10B Fe1B -61.0(5) . . . . ? C9B Fe1B C10B C6B -116.7(8) . . . . ? C1B Fe1B C10B C6B 121.2(5) . . . . ? C2B Fe1B C10B C6B 163.6(5) . . . . ? C8B Fe1B C10B C6B -76.6(6) . . . . ? C5B Fe1B C10B C6B 78.5(6) . . . . ? C3B Fe1B C10B C6B -160.5(8) . . . . ? C7B Fe1B C10B C6B -34.3(6) . . . . ? C4B Fe1B C10B C6B 43.1(10) . . . . ? C1B Fe1B C10B C9B -122.1(6) . . . . ? C2B Fe1B C10B C9B -79.7(6) . . . . ? C8B Fe1B C10B C9B 40.2(6) . . . . ? C5B Fe1B C10B C9B -164.8(5) . . . . ? C3B Fe1B C10B C9B -43.8(11) . . . . ? C7B Fe1B C10B C9B 82.4(6) . . . . ? C6B Fe1B C10B C9B 116.7(8) . . . . ? C4B Fe1B C10B C9B 159.8(8) . . . . ? C5B C1B C11B O16B -79.3(8) . . . . ? C2B C1B C11B O16B 99.8(7) . . . . ? Fe1B C1B C11B O16B -170.8(5) . . . . ? C5B C1B C11B O12B 39.3(8) . . . . ? C2B C1B C11B O12B -141.6(6) . . . . ? Fe1B C1B C11B O12B -52.2(7) . . . . ? O16B C11B O12B C13B -63.3(7) . . . . ? C1B C11B O12B C13B 179.8(5) . . . . ? C11B O12B C13B C17B -174.8(7) . . . . ? C11B O12B C13B C14B 59.0(8) . . . . ? O12B C13B C14B C15B -54.2(9) . . . . ? C17B C13B C14B C15B -174.9(7) . . . . ? C13B C14B C15B O16B 54.4(11) . . . . ? O12B C11B O16B C15B 62.0(8) . . . . ? C1B C11B O16B C15B 179.5(7) . . . . ? C14B C15B O16B C11B -58.7(10) . . . . ? O12B C13B C17B O18B 64.3(9) . . . . ? C14B C13B C17B O18B -173.9(7) . . . . ? C13B C17B O18B C19B -163.7(9) . . . . ? C10C Fe1C C1C C5C -121.9(3) . . . . ? C2C Fe1C C1C C5C 117.9(4) . . . . ? C6C Fe1C C1C C5C -163.0(3) . . . . ? C3C Fe1C C1C C5C 80.7(4) . . . . ? C4C Fe1C C1C C5C 37.2(3) . . . . ? C9C Fe1C C1C C5C -80.2(4) . . . . ? C8C Fe1C C1C C5C -48.1(7) . . . . ? C7C Fe1C C1C C5C 166.7(6) . . . . ? C10C Fe1C C1C C2C 120.2(3) . . . . ? C6C Fe1C C1C C2C 79.1(4) . . . . ? C3C Fe1C C1C C2C -37.2(3) . . . . ? C4C Fe1C C1C C2C -80.7(3) . . . . ? C9C Fe1C C1C C2C 161.9(3) . . . . ? C8C Fe1C C1C C2C -166.0(5) . . . . ? C7C Fe1C C1C C2C 48.9(8) . . . . ? C5C Fe1C C1C C2C -117.9(4) . . . . ? C10C Fe1C C1C C11C 1.1(6) . . . . ? C2C Fe1C C1C C11C -119.1(6) . . . . ? C6C Fe1C C1C C11C -40.0(6) . . . . ? C3C Fe1C C1C C11C -156.3(6) . . . . ? C4C Fe1C C1C C11C 160.2(6) . . . . ? C9C Fe1C C1C C11C 42.8(6) . . . . ? C8C Fe1C C1C C11C 74.9(8) . . . . ? C7C Fe1C C1C C11C -70.3(9) . . . . ? C5C Fe1C C1C C11C 123.0(6) . . . . ? C5C C1C C2C C3C -2.0(6) . . . . ? C11C C1C C2C C3C -175.9(5) . . . . ? Fe1C C1C C2C C3C 58.8(4) . . . . ? C5C C1C C2C Fe1C -60.8(4) . . . . ? C11C C1C C2C Fe1C 125.2(5) . . . . ? C5C C1C C2C I1CA 173.9(4) . . . . ? C11C C1C C2C I1CA 0.0(8) . . . . ? Fe1C C1C C2C I1CA -125.2(4) . . . . ? C1C Fe1C C2C C3C -120.2(5) . . . . ? C10C Fe1C C2C C3C 161.4(3) . . . . ? C6C Fe1C C2C C3C 118.8(4) . . . . ? C4C Fe1C C2C C3C -38.1(3) . . . . ? C9C Fe1C C2C C3C -164.3(5) . . . . ? C8C Fe1C C2C C3C 42.7(9) . . . . ? C7C Fe1C C2C C3C 77.0(4) . . . . ? C5C Fe1C C2C C3C -81.7(3) . . . . ? C10C Fe1C C2C C1C -78.4(4) . . . . ? C6C Fe1C C2C C1C -121.0(3) . . . . ? C3C Fe1C C2C C1C 120.2(5) . . . . ? C4C Fe1C C2C C1C 82.1(3) . . . . ? C9C Fe1C C2C C1C -44.1(7) . . . . ? C8C Fe1C C2C C1C 162.9(7) . . . . ? C7C Fe1C C2C C1C -162.8(3) . . . . ? C5C Fe1C C2C C1C 38.6(3) . . . . ? C1C Fe1C C2C I1CA 120.2(5) . . . . ? C10C Fe1C C2C I1CA 41.8(4) . . . . ? C6C Fe1C C2C I1CA -0.8(4) . . . . ? C3C Fe1C C2C I1CA -119.5(5) . . . . ? C4C Fe1C C2C I1CA -157.7(4) . . . . ? C9C Fe1C C2C I1CA 76.1(7) . . . . ? C8C Fe1C C2C I1CA -76.8(8) . . . . ? C7C Fe1C C2C I1CA -42.5(4) . . . . ? C5C Fe1C C2C I1CA 158.8(4) . . . . ? C1C C2C C3C C4C 1.6(6) . . . . ? Fe1C C2C C3C C4C 60.0(4) . . . . ? I1CA C2C C3C C4C -174.3(4) . . . . ? C1C C2C C3C Fe1C -58.4(4) . . . . ? I1CA C2C C3C Fe1C 125.7(4) . . . . ? C1C Fe1C C3C C4C -80.6(3) . . . . ? C10C Fe1C C3C C4C -165.0(6) . . . . ? C2C Fe1C C3C C4C -118.1(4) . . . . ? C6C Fe1C C3C C4C 161.2(3) . . . . ? C9C Fe1C C3C C4C 44.3(8) . . . . ? C8C Fe1C C3C C4C 77.5(4) . . . . ? C7C Fe1C C3C C4C 119.3(4) . . . . ? C5C Fe1C C3C C4C -36.4(3) . . . . ? C1C Fe1C C3C C2C 37.5(3) . . . . ? C10C Fe1C C3C C2C -46.9(7) . . . . ? C6C Fe1C C3C C2C -80.7(4) . . . . ? C4C Fe1C C3C C2C 118.1(4) . . . . ? C9C Fe1C C3C C2C 162.4(6) . . . . ? C8C Fe1C C3C C2C -164.4(3) . . . . ? C7C Fe1C C3C C2C -122.7(4) . . . . ? C5C Fe1C C3C C2C 81.6(3) . . . . ? C2C C3C C4C C5C -0.6(6) . . . . ? Fe1C C3C C4C C5C 58.9(4) . . . . ? C2C C3C C4C Fe1C -59.5(4) . . . . ? C1C Fe1C C4C C5C -37.9(3) . . . . ? C10C Fe1C C4C C5C 42.8(8) . . . . ? C2C Fe1C C4C C5C -82.6(3) . . . . ? C6C Fe1C C4C C5C -167.7(6) . . . . ? C3C Fe1C C4C C5C -121.2(5) . . . . ? C9C Fe1C C4C C5C 75.5(4) . . . . ? C8C Fe1C C4C C5C 117.4(4) . . . . ? C7C Fe1C C4C C5C 159.3(4) . . . . ? C1C Fe1C C4C C3C 83.3(3) . . . . ? C10C Fe1C C4C C3C 164.0(6) . . . . ? C2C Fe1C C4C C3C 38.6(3) . . . . ? C6C Fe1C C4C C3C -46.5(8) . . . . ? C9C Fe1C C4C C3C -163.3(3) . . . . ? C8C Fe1C C4C C3C -121.4(4) . . . . ? C7C Fe1C C4C C3C -79.5(4) . . . . ? C5C Fe1C C4C C3C 121.2(5) . . . . ? C3C C4C C5C C1C -0.6(6) . . . . ? Fe1C C4C C5C C1C 57.9(4) . . . . ? C3C C4C C5C Fe1C -58.5(4) . . . . ? C2C C1C C5C C4C 1.6(6) . . . . ? C11C C1C C5C C4C 175.3(5) . . . . ? Fe1C C1C C5C C4C -58.6(4) . . . . ? C2C C1C C5C Fe1C 60.2(4) . . . . ? C11C C1C C5C Fe1C -126.1(6) . . . . ? C1C Fe1C C5C C4C 119.5(5) . . . . ? C10C Fe1C C5C C4C -163.7(4) . . . . ? C2C Fe1C C5C C4C 80.7(4) . . . . ? C6C Fe1C C5C C4C 166.2(7) . . . . ? C3C Fe1C C5C C4C 36.6(3) . . . . ? C9C Fe1C C5C C4C -122.7(4) . . . . ? C8C Fe1C C5C C4C -80.8(4) . . . . ? C7C Fe1C C5C C4C -49.6(7) . . . . ? C10C Fe1C C5C C1C 76.8(4) . . . . ? C2C Fe1C C5C C1C -38.8(3) . . . . ? C6C Fe1C C5C C1C 46.7(8) . . . . ? C3C Fe1C C5C C1C -82.9(3) . . . . ? C4C Fe1C C5C C1C -119.5(5) . . . . ? C9C Fe1C C5C C1C 117.8(3) . . . . ? C8C Fe1C C5C C1C 159.7(3) . . . . ? C7C Fe1C C5C C1C -169.1(5) . . . . ? C1C Fe1C C6C C10C 75.4(4) . . . . ? C2C Fe1C C6C C10C 118.6(4) . . . . ? C3C Fe1C C6C C10C 161.6(3) . . . . ? C4C Fe1C C6C C10C -164.4(6) . . . . ? C9C Fe1C C6C C10C -37.6(4) . . . . ? C8C Fe1C C6C C10C -81.6(4) . . . . ? C7C Fe1C C6C C10C -119.2(5) . . . . ? C5C Fe1C C6C C10C 40.1(9) . . . . ? C1C Fe1C C6C C7C -165.4(4) . . . . ? C10C Fe1C C6C C7C 119.2(5) . . . . ? C2C Fe1C C6C C7C -122.3(4) . . . . ? C3C Fe1C C6C C7C -79.2(4) . . . . ? C4C Fe1C C6C C7C -45.2(8) . . . . ? C9C Fe1C C6C C7C 81.5(4) . . . . ? C8C Fe1C C6C C7C 37.6(4) . . . . ? C5C Fe1C C6C C7C 159.3(7) . . . . ? C10C C6C C7C C8C 0.0(6) . . . . ? Fe1C C6C C7C C8C -59.3(4) . . . . ? C10C C6C C7C Fe1C 59.3(4) . . . . ? C1C Fe1C C7C C6C 40.1(9) . . . . ? C10C Fe1C C7C C6C -37.8(4) . . . . ? C2C Fe1C C7C C6C 77.3(4) . . . . ? C3C Fe1C C7C C6C 119.5(4) . . . . ? C4C Fe1C C7C C6C 161.7(4) . . . . ? C9C Fe1C C7C C6C -81.4(4) . . . . ? C8C Fe1C C7C C6C -119.3(5) . . . . ? C5C Fe1C C7C C6C -162.6(5) . . . . ? C1C Fe1C C7C C8C 159.4(6) . . . . ? C10C Fe1C C7C C8C 81.5(4) . . . . ? C2C Fe1C C7C C8C -163.3(3) . . . . ? C6C Fe1C C7C C8C 119.3(5) . . . . ? C3C Fe1C C7C C8C -121.1(4) . . . . ? C4C Fe1C C7C C8C -79.0(4) . . . . ? C9C Fe1C C7C C8C 38.0(4) . . . . ? C5C Fe1C C7C C8C -43.2(7) . . . . ? C6C C7C C8C C9C -0.7(6) . . . . ? Fe1C C7C C8C C9C -59.6(4) . . . . ? C6C C7C C8C Fe1C 59.0(4) . . . . ? C1C Fe1C C8C C7C -163.4(5) . . . . ? C10C Fe1C C8C C7C -81.4(4) . . . . ? C2C Fe1C C8C C7C 45.6(9) . . . . ? C6C Fe1C C8C C7C -37.5(4) . . . . ? C3C Fe1C C8C C7C 77.9(4) . . . . ? C4C Fe1C C8C C7C 119.6(4) . . . . ? C9C Fe1C C8C C7C -118.8(5) . . . . ? C5C Fe1C C8C C7C 161.7(3) . . . . ? C1C Fe1C C8C C9C -44.6(7) . . . . ? C10C Fe1C C8C C9C 37.4(4) . . . . ? C2C Fe1C C8C C9C 164.5(6) . . . . ? C6C Fe1C C8C C9C 81.3(4) . . . . ? C3C Fe1C C8C C9C -163.3(3) . . . . ? C4C Fe1C C8C C9C -121.5(4) . . . . ? C7C Fe1C C8C C9C 118.8(5) . . . . ? C5C Fe1C C8C C9C -79.4(4) . . . . ? C7C C8C C9C C10C 1.1(6) . . . . ? Fe1C C8C C9C C10C -58.6(4) . . . . ? C7C C8C C9C Fe1C 59.7(4) . . . . ? C1C Fe1C C9C C10C -79.7(4) . . . . ? C2C Fe1C C9C C10C -47.4(7) . . . . ? C6C Fe1C C9C C10C 37.9(4) . . . . ? C3C Fe1C C9C C10C 163.8(6) . . . . ? C4C Fe1C C9C C10C -163.2(3) . . . . ? C8C Fe1C C9C C10C 119.4(5) . . . . ? C7C Fe1C C9C C10C 81.6(4) . . . . ? C5C Fe1C C9C C10C -122.3(4) . . . . ? C1C Fe1C C9C C8C 161.0(4) . . . . ? C10C Fe1C C9C C8C -119.4(5) . . . . ? C2C Fe1C C9C C8C -166.7(5) . . . . ? C6C Fe1C C9C C8C -81.4(4) . . . . ? C3C Fe1C C9C C8C 44.4(8) . . . . ? C4C Fe1C C9C C8C 77.5(4) . . . . ? C7C Fe1C C9C C8C -37.8(4) . . . . ? C5C Fe1C C9C C8C 118.4(4) . . . . ? C8C C9C C10C C6C -1.1(6) . . . . ? Fe1C C9C C10C C6C -60.2(4) . . . . ? C8C C9C C10C Fe1C 59.1(4) . . . . ? C7C C6C C10C C9C 0.7(6) . . . . ? Fe1C C6C C10C C9C 60.6(4) . . . . ? C7C C6C C10C Fe1C -59.9(4) . . . . ? C1C Fe1C C10C C9C 117.9(4) . . . . ? C2C Fe1C C10C C9C 160.4(3) . . . . ? C6C Fe1C C10C C9C -118.9(5) . . . . ? C3C Fe1C C10C C9C -165.0(6) . . . . ? C4C Fe1C C10C C9C 44.1(9) . . . . ? C8C Fe1C C10C C9C -37.7(4) . . . . ? C7C Fe1C C10C C9C -81.4(4) . . . . ? C5C Fe1C C10C C9C 75.9(4) . . . . ? C1C Fe1C C10C C6C -123.2(4) . . . . ? C2C Fe1C C10C C6C -80.6(4) . . . . ? C3C Fe1C C10C C6C -46.0(8) . . . . ? C4C Fe1C C10C C6C 163.1(6) . . . . ? C9C Fe1C C10C C6C 118.9(5) . . . . ? C8C Fe1C C10C C6C 81.2(4) . . . . ? C7C Fe1C C10C C6C 37.5(4) . . . . ? C5C Fe1C C10C C6C -165.2(4) . . . . ? C5C C1C C11C O12C 42.2(8) . . . . ? C2C C1C C11C O12C -145.1(5) . . . . ? Fe1C C1C C11C O12C -53.3(7) . . . . ? C5C C1C C11C O16C -78.8(7) . . . . ? C2C C1C C11C O16C 93.9(6) . . . . ? Fe1C C1C C11C O16C -174.3(4) . . . . ? O16C C11C O12C C13C -63.7(6) . . . . ? C1C C11C O12C C13C 178.5(5) . . . . ? C11C O12C C13C C14C 59.4(6) . . . . ? C11C O12C C13C C17C -178.6(5) . . . . ? O12C C13C C14C C15C -55.0(8) . . . . ? C17C C13C C14C C15C -174.6(6) . . . . ? C13C C14C C15C O16C 53.9(9) . . . . ? O12C C11C O16C C15C 62.0(7) . . . . ? C1C C11C O16C C15C -177.2(5) . . . . ? C14C C15C O16C C11C -56.6(9) . . . . ? O12C C13C C17C O18C 58.8(7) . . . . ? C14C C13C C17C O18C 178.8(6) . . . . ? C13C C17C O18C C19C 68.9(8) . . . . ? C10D Fe1D C1D C5D -162.9(4) . . . . ? C6D Fe1D C1D C5D 170.1(7) . . . . ? C2D Fe1D C1D C5D 116.1(5) . . . . ? C8D Fe1D C1D C5D -80.6(4) . . . . ? C9D Fe1D C1D C5D -121.5(4) . . . . ? C3D Fe1D C1D C5D 79.4(4) . . . . ? C7D Fe1D C1D C5D -50.5(8) . . . . ? C4D Fe1D C1D C5D 36.8(4) . . . . ? C10D Fe1D C1D C2D 81.0(4) . . . . ? C6D Fe1D C1D C2D 53.9(8) . . . . ? C8D Fe1D C1D C2D 163.3(3) . . . . ? C9D Fe1D C1D C2D 122.4(4) . . . . ? C3D Fe1D C1D C2D -36.7(3) . . . . ? C7D Fe1D C1D C2D -166.6(6) . . . . ? C5D Fe1D C1D C2D -116.1(5) . . . . ? C4D Fe1D C1D C2D -79.4(3) . . . . ? C10D Fe1D C1D C11D -40.4(6) . . . . ? C6D Fe1D C1D C11D -67.4(9) . . . . ? C2D Fe1D C1D C11D -121.4(6) . . . . ? C8D Fe1D C1D C11D 41.9(6) . . . . ? C9D Fe1D C1D C11D 1.0(6) . . . . ? C3D Fe1D C1D C11D -158.0(6) . . . . ? C7D Fe1D C1D C11D 72.0(9) . . . . ? C5D Fe1D C1D C11D 122.5(6) . . . . ? C4D Fe1D C1D C11D 159.3(6) . . . . ? C5D C1D C2D C3D -2.1(6) . . . . ? C11D C1D C2D C3D -178.6(5) . . . . ? Fe1D C1D C2D C3D 58.8(4) . . . . ? C5D C1D C2D Fe1D -61.0(4) . . . . ? C11D C1D C2D Fe1D 122.6(6) . . . . ? C5D C1D C2D I1D 177.1(4) . . . . ? C11D C1D C2D I1D 0.6(8) . . . . ? Fe1D C1D C2D I1D -122.0(4) . . . . ? C10D Fe1D C2D C3D 119.9(4) . . . . ? C6D Fe1D C2D C3D 79.1(5) . . . . ? C8D Fe1D C2D C3D -163.9(6) . . . . ? C1D Fe1D C2D C3D -121.0(5) . . . . ? C9D Fe1D C2D C3D 163.3(4) . . . . ? C7D Fe1D C2D C3D 44.8(9) . . . . ? C5D Fe1D C2D C3D -81.5(3) . . . . ? C4D Fe1D C2D C3D -37.5(3) . . . . ? C10D Fe1D C2D C1D -119.1(4) . . . . ? C6D Fe1D C2D C1D -159.9(4) . . . . ? C8D Fe1D C2D C1D -42.9(8) . . . . ? C9D Fe1D C2D C1D -75.7(4) . . . . ? C3D Fe1D C2D C1D 121.0(5) . . . . ? C7D Fe1D C2D C1D 165.8(7) . . . . ? C5D Fe1D C2D C1D 39.5(3) . . . . ? C4D Fe1D C2D C1D 83.5(3) . . . . ? C10D Fe1D C2D I1D 1.5(5) . . . . ? C6D Fe1D C2D I1D -39.3(5) . . . . ? C8D Fe1D C2D I1D 77.6(8) . . . . ? C1D Fe1D C2D I1D 120.6(5) . . . . ? C9D Fe1D C2D I1D 44.9(5) . . . . ? C3D Fe1D C2D I1D -118.4(5) . . . . ? C7D Fe1D C2D I1D -73.7(8) . . . . ? C5D Fe1D C2D I1D 160.1(4) . . . . ? C4D Fe1D C2D I1D -155.9(4) . . . . ? C1D C2D C3D C4D 2.3(6) . . . . ? Fe1D C2D C3D C4D 60.7(4) . . . . ? I1D C2D C3D C4D -177.0(4) . . . . ? C1D C2D C3D Fe1D -58.4(4) . . . . ? I1D C2D C3D Fe1D 122.3(4) . . . . ? C10D Fe1D C3D C4D 161.6(4) . . . . ? C6D Fe1D C3D C4D 120.4(4) . . . . ? C2D Fe1D C3D C4D -118.5(5) . . . . ? C8D Fe1D C3D C4D 45.5(8) . . . . ? C1D Fe1D C3D C4D -81.4(3) . . . . ? C9D Fe1D C3D C4D -162.3(7) . . . . ? C7D Fe1D C3D C4D 78.7(4) . . . . ? C5D Fe1D C3D C4D -37.2(3) . . . . ? C10D Fe1D C3D C2D -79.9(5) . . . . ? C6D Fe1D C3D C2D -121.0(4) . . . . ? C8D Fe1D C3D C2D 164.1(6) . . . . ? C1D Fe1D C3D C2D 37.2(3) . . . . ? C9D Fe1D C3D C2D -43.8(8) . . . . ? C7D Fe1D C3D C2D -162.8(4) . . . . ? C5D Fe1D C3D C2D 81.4(3) . . . . ? C4D Fe1D C3D C2D 118.5(5) . . . . ? C2D C3D C4D C5D -1.5(6) . . . . ? Fe1D C3D C4D C5D 58.0(4) . . . . ? C2D C3D C4D Fe1D -59.4(4) . . . . ? C10D Fe1D C4D C3D -46.2(9) . . . . ? C6D Fe1D C4D C3D -79.0(5) . . . . ? C2D Fe1D C4D C3D 38.4(3) . . . . ? C8D Fe1D C4D C3D -161.9(4) . . . . ? C1D Fe1D C4D C3D 83.1(3) . . . . ? C9D Fe1D C4D C3D 163.0(6) . . . . ? C7D Fe1D C4D C3D -120.0(4) . . . . ? C5D Fe1D C4D C3D 120.4(5) . . . . ? C10D Fe1D C4D C5D -166.7(7) . . . . ? C6D Fe1D C4D C5D 160.6(4) . . . . ? C2D Fe1D C4D C5D -82.0(4) . . . . ? C8D Fe1D C4D C5D 77.7(4) . . . . ? C1D Fe1D C4D C5D -37.3(3) . . . . ? C9D Fe1D C4D C5D 42.6(8) . . . . ? C3D Fe1D C4D C5D -120.4(5) . . . . ? C7D Fe1D C4D C5D 119.6(4) . . . . ? C3D C4D C5D C1D 0.1(6) . . . . ? Fe1D C4D C5D C1D 58.2(4) . . . . ? C3D C4D C5D Fe1D -58.0(4) . . . . ? C2D C1D C5D C4D 1.2(6) . . . . ? C11D C1D C5D C4D 177.6(5) . . . . ? Fe1D C1D C5D C4D -59.1(4) . . . . ? C2D C1D C5D Fe1D 60.3(4) . . . . ? C11D C1D C5D Fe1D -123.3(6) . . . . ? C10D Fe1D C5D C4D 166.0(7) . . . . ? C6D Fe1D C5D C4D -49.7(9) . . . . ? C2D Fe1D C5D C4D 80.8(4) . . . . ? C8D Fe1D C5D C4D -121.2(4) . . . . ? C1D Fe1D C5D C4D 120.6(5) . . . . ? C9D Fe1D C5D C4D -163.1(4) . . . . ? C3D Fe1D C5D C4D 36.6(3) . . . . ? C7D Fe1D C5D C4D -79.5(4) . . . . ? C10D Fe1D C5D C1D 45.4(9) . . . . ? C6D Fe1D C5D C1D -170.3(7) . . . . ? C2D Fe1D C5D C1D -39.8(3) . . . . ? C8D Fe1D C5D C1D 118.2(4) . . . . ? C9D Fe1D C5D C1D 76.3(4) . . . . ? C3D Fe1D C5D C1D -84.0(3) . . . . ? C7D Fe1D C5D C1D 159.9(3) . . . . ? C4D Fe1D C5D C1D -120.6(5) . . . . ? C2D Fe1D C6D C10D 77.4(5) . . . . ? C8D Fe1D C6D C10D -82.2(5) . . . . ? C1D Fe1D C6D C10D 36.9(9) . . . . ? C9D Fe1D C6D C10D -38.3(5) . . . . ? C3D Fe1D C6D C10D 120.2(5) . . . . ? C7D Fe1D C6D C10D -120.7(6) . . . . ? C5D Fe1D C6D C10D -161.4(7) . . . . ? C4D Fe1D C6D C10D 161.9(4) . . . . ? C10D Fe1D C6D C7D 120.7(6) . . . . ? C2D Fe1D C6D C7D -161.9(4) . . . . ? C8D Fe1D C6D C7D 38.5(4) . . . . ? C1D Fe1D C6D C7D 157.7(6) . . . . ? C9D Fe1D C6D C7D 82.4(5) . . . . ? C3D Fe1D C6D C7D -119.1(4) . . . . ? C5D Fe1D C6D C7D -40.7(9) . . . . ? C4D Fe1D C6D C7D -77.4(5) . . . . ? C10D C6D C7D C8D 0.1(8) . . . . ? Fe1D C6D C7D C8D -59.5(5) . . . . ? C10D C6D C7D Fe1D 59.6(5) . . . . ? C10D Fe1D C7D C6D -36.2(5) . . . . ? C2D Fe1D C7D C6D 46.7(10) . . . . ? C8D Fe1D C7D C6D -117.8(7) . . . . ? C1D Fe1D C7D C6D -159.1(6) . . . . ? C9D Fe1D C7D C6D -80.9(5) . . . . ? C3D Fe1D C7D C6D 80.0(5) . . . . ? C5D Fe1D C7D C6D 163.7(4) . . . . ? C4D Fe1D C7D C6D 121.5(5) . . . . ? C10D Fe1D C7D C8D 81.6(5) . . . . ? C6D Fe1D C7D C8D 117.8(7) . . . . ? C2D Fe1D C7D C8D 164.5(6) . . . . ? C1D Fe1D C7D C8D -41.3(9) . . . . ? C9D Fe1D C7D C8D 37.0(4) . . . . ? C3D Fe1D C7D C8D -162.2(4) . . . . ? C5D Fe1D C7D C8D -78.4(5) . . . . ? C4D Fe1D C7D C8D -120.7(4) . . . . ? C6D C7D C8D C9D 0.1(8) . . . . ? Fe1D C7D C8D C9D -59.4(5) . . . . ? C6D C7D C8D Fe1D 59.5(5) . . . . ? C10D Fe1D C8D C9D 39.6(4) . . . . ? C6D Fe1D C8D C9D 82.4(5) . . . . ? C2D Fe1D C8D C9D -44.5(9) . . . . ? C1D Fe1D C8D C9D -76.5(5) . . . . ? C3D Fe1D C8D C9D 165.5(6) . . . . ? C7D Fe1D C8D C9D 120.4(6) . . . . ? C5D Fe1D C8D C9D -119.4(4) . . . . ? C4D Fe1D C8D C9D -161.3(4) . . . . ? C10D Fe1D C8D C7D -80.8(5) . . . . ? C6D Fe1D C8D C7D -38.0(5) . . . . ? C2D Fe1D C8D C7D -164.9(6) . . . . ? C1D Fe1D C8D C7D 163.1(4) . . . . ? C9D Fe1D C8D C7D -120.4(6) . . . . ? C3D Fe1D C8D C7D 45.1(9) . . . . ? C5D Fe1D C8D C7D 120.2(5) . . . . ? C4D Fe1D C8D C7D 78.4(5) . . . . ? C7D C8D C9D C10D -0.3(7) . . . . ? Fe1D C8D C9D C10D -59.9(4) . . . . ? C7D C8D C9D Fe1D 59.6(5) . . . . ? C10D Fe1D C9D C8D -116.6(6) . . . . ? C6D Fe1D C9D C8D -79.9(5) . . . . ? C2D Fe1D C9D C8D 162.5(4) . . . . ? C1D Fe1D C9D C8D 120.7(4) . . . . ? C3D Fe1D C9D C8D -164.8(6) . . . . ? C7D Fe1D C9D C8D -36.9(4) . . . . ? C5D Fe1D C9D C8D 79.1(5) . . . . ? C4D Fe1D C9D C8D 47.7(8) . . . . ? C6D Fe1D C9D C10D 36.7(5) . . . . ? C2D Fe1D C9D C10D -80.9(5) . . . . ? C8D Fe1D C9D C10D 116.6(6) . . . . ? C1D Fe1D C9D C10D -122.7(4) . . . . ? C3D Fe1D C9D C10D -48.2(9) . . . . ? C7D Fe1D C9D C10D 79.7(5) . . . . ? C5D Fe1D C9D C10D -164.3(4) . . . . ? C4D Fe1D C9D C10D 164.3(6) . . . . ? C7D C6D C10D C9D -0.3(8) . . . . ? Fe1D C6D C10D C9D 59.7(5) . . . . ? C7D C6D C10D Fe1D -60.0(5) . . . . ? C8D C9D C10D C6D 0.4(7) . . . . ? Fe1D C9D C10D C6D -60.0(5) . . . . ? C8D C9D C10D Fe1D 60.3(4) . . . . ? C2D Fe1D C10D C6D -121.7(5) . . . . ? C8D Fe1D C10D C6D 80.5(5) . . . . ? C1D Fe1D C10D C6D -165.4(4) . . . . ? C9D Fe1D C10D C6D 119.3(6) . . . . ? C3D Fe1D C10D C6D -78.8(5) . . . . ? C7D Fe1D C10D C6D 36.6(4) . . . . ? C5D Fe1D C10D C6D 160.6(7) . . . . ? C4D Fe1D C10D C6D -45.0(9) . . . . ? C6D Fe1D C10D C9D -119.3(6) . . . . ? C2D Fe1D C10D C9D 118.9(4) . . . . ? C8D Fe1D C10D C9D -38.8(4) . . . . ? C1D Fe1D C10D C9D 75.2(5) . . . . ? C3D Fe1D C10D C9D 161.8(4) . . . . ? C7D Fe1D C10D C9D -82.7(5) . . . . ? C5D Fe1D C10D C9D 41.3(10) . . . . ? C4D Fe1D C10D C9D -164.4(6) . . . . ? C5D C1D C11D O12D 43.5(8) . . . . ? C2D C1D C11D O12D -140.9(5) . . . . ? Fe1D C1D C11D O12D -49.6(7) . . . . ? C5D C1D C11D O16D -77.0(7) . . . . ? C2D C1D C11D O16D 98.6(7) . . . . ? Fe1D C1D C11D O16D -170.1(4) . . . . ? O16D C11D O12D C13D -61.7(6) . . . . ? C1D C11D O12D C13D 179.4(5) . . . . ? C11D O12D C13D C14D 58.6(7) . . . . ? C11D O12D C13D C17D -174.4(6) . . . . ? O12D C13D C14D C15D -55.2(9) . . . . ? C17D C13D C14D C15D -177.9(7) . . . . ? C13D C14D C15D O16D 55.6(10) . . . . ? O12D C11D O16D C15D 62.0(8) . . . . ? C1D C11D O16D C15D -178.4(6) . . . . ? C14D C15D O16D C11D -58.9(10) . . . . ? O12D C13D C17D O18D 69.4(8) . . . . ? C14D C13D C17D O18D -167.4(7) . . . . ? C13D C17D O18D C19D -145.0(10) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.901 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.082 # Attachment 'SSpR14.cif' data_erk4262 _database_code_depnum_ccdc_archive 'CCDC 714359' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 Fe O5' _chemical_formula_weight 374.21 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.5104(1) _cell_length_b 8.8078(2) _cell_length_c 23.3727(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1751.97(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3909 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6917 _exptl_absorpt_correction_T_max 0.9571 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13367 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.86 _reflns_number_total 4124 _reflns_number_gt 3344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0333P)^2^+0.1867P] 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 riding _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 -0.013(15) _refine_ls_number_reflns 4124 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Fe Fe 0.06635(4) 0.96427(4) 0.935767(14) 0.02761(10) Uani 1 1 d . . . C1 C 0.1275(3) 1.1430(3) 0.88528(13) 0.0422(7) Uani 1 1 d . . . H1 H 0.0582 1.2024 0.8634 0.051 Uiso 1 1 calc R . . C2 C 0.1738(3) 1.1703(3) 0.94275(14) 0.0440(7) Uani 1 1 d . . . H2 H 0.1407 1.2518 0.9657 0.053 Uiso 1 1 calc R . . C3 C 0.2779(3) 1.0542(4) 0.95933(13) 0.0502(8) Uani 1 1 d . . . H3 H 0.3259 1.0442 0.9954 0.060 Uiso 1 1 calc R . . C4 C 0.2974(3) 0.9565(4) 0.91288(14) 0.0496(8) Uani 1 1 d . . . H4 H 0.3616 0.8697 0.9123 0.060 Uiso 1 1 calc R . . C5 C 0.2055(3) 1.0093(3) 0.86729(12) 0.0409(7) Uani 1 1 d . . . H5 H 0.1972 0.9638 0.8310 0.049 Uiso 1 1 calc R . . C10 C -0.1713(2) 0.9496(3) 0.92963(10) 0.0269(5) Uani 1 1 d . . . C11 C -0.1246(3) 0.9659(3) 0.98855(10) 0.0320(5) Uani 1 1 d . . . H11 H -0.1559 1.0442 1.0134 0.038 Uiso 1 1 calc R . . C12 C -0.0236(3) 0.8438(3) 1.00247(11) 0.0355(6) Uani 1 1 d . . . H12 H 0.0248 0.8281 1.0381 0.043 Uiso 1 1 calc R . . C13 C -0.0074(3) 0.7489(3) 0.95393(11) 0.0339(6) Uani 1 1 d . . . H13 H 0.0526 0.6596 0.9515 0.041 Uiso 1 1 calc R . . C14 C -0.0987(3) 0.8143(3) 0.90977(10) 0.0280(5) Uani 1 1 d . . . C15 C -0.2807(3) 1.0534(3) 0.89824(10) 0.0296(5) Uani 1 1 d . . . H15 H -0.3886 1.0118 0.9004 0.035 Uiso 1 1 calc R . . O16 O -0.23484(18) 1.06296(18) 0.83979(7) 0.0290(4) Uani 1 1 d . . . C17 C -0.3450(3) 1.1545(3) 0.80843(11) 0.0332(6) Uani 1 1 d . . . H17 H -0.4496 1.1056 0.8097 0.040 Uiso 1 1 calc R . . C18 C -0.3558(3) 1.3115(4) 0.83587(13) 0.0457(7) Uani 1 1 d . . . H18A H -0.2564 1.3658 0.8305 0.055 Uiso 1 1 calc R . . H18B H -0.4393 1.3702 0.8173 0.055 Uiso 1 1 calc R . . C19 C -0.3902(3) 1.2966(3) 0.89876(13) 0.0489(8) Uani 1 1 d . . . H19A H -0.3850 1.3967 0.9170 0.059 Uiso 1 1 calc R . . H19B H -0.4966 1.2564 0.9041 0.059 Uiso 1 1 calc R . . O20 O -0.2774(2) 1.1958(2) 0.92513(8) 0.0411(5) Uani 1 1 d . . . C21 C -0.2915(3) 1.1645(3) 0.74719(11) 0.0378(6) Uani 1 1 d . . . H21A H -0.3547 1.2403 0.7269 0.045 Uiso 1 1 calc R . . H21B H -0.1815 1.1973 0.7460 0.045 Uiso 1 1 calc R . . O22 O -0.3063(2) 1.0225(2) 0.71957(8) 0.0447(5) Uani 1 1 d . . . C23 C -0.2599(4) 1.0296(4) 0.66137(12) 0.0528(7) Uani 1 1 d . . . H23A H -0.3250 1.1027 0.6413 0.079 Uiso 1 1 calc R . . H23B H -0.2722 0.9304 0.6439 0.079 Uiso 1 1 calc R . . H23C H -0.1507 1.0606 0.6590 0.079 Uiso 1 1 calc R . . O24 O -0.10534(17) 0.7542(2) 0.85412(7) 0.0314(4) Uani 1 1 d . . . C25 C -0.2506(3) 0.7183(3) 0.83309(11) 0.0328(6) Uani 1 1 d . . . O26 O -0.3680(2) 0.7224(3) 0.86121(9) 0.0491(5) Uani 1 1 d . . . C27 C -0.2383(4) 0.6775(3) 0.77156(11) 0.0456(7) Uani 1 1 d . . . H27A H -0.3315 0.6220 0.7600 0.068 Uiso 1 1 calc R . . H27B H -0.1462 0.6146 0.7656 0.068 Uiso 1 1 calc R . . H27C H -0.2292 0.7693 0.7489 0.068 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 Fe 0.02786(16) 0.03072(19) 0.02423(17) 0.00397(17) -0.00252(15) -0.00323(15) C1 0.0368(14) 0.0402(18) 0.0495(19) 0.0177(15) -0.0043(12) -0.0085(13) C2 0.0474(16) 0.0361(17) 0.0485(19) -0.0098(15) 0.0042(14) -0.0175(13) C3 0.0353(14) 0.067(2) 0.0483(17) 0.0114(17) -0.0144(12) -0.0180(16) C4 0.0302(13) 0.0512(19) 0.067(2) 0.0112(18) 0.0048(13) 0.0029(14) C5 0.0477(15) 0.0426(19) 0.0325(14) 0.0004(12) 0.0079(12) -0.0124(13) C10 0.0285(11) 0.0277(14) 0.0246(12) 0.0009(13) 0.0035(9) -0.0034(10) C11 0.0363(12) 0.0368(14) 0.0231(12) -0.0001(13) 0.0025(9) -0.0038(12) C12 0.0423(15) 0.0401(16) 0.0241(14) 0.0084(12) -0.0038(10) -0.0065(12) C13 0.0381(13) 0.0284(14) 0.0351(15) 0.0100(12) -0.0033(11) -0.0005(11) C14 0.0300(13) 0.0286(14) 0.0253(13) -0.0009(10) -0.0023(9) -0.0035(10) C15 0.0255(11) 0.0332(15) 0.0300(13) -0.0008(12) 0.0000(9) 0.0028(11) O16 0.0292(8) 0.0326(10) 0.0252(9) 0.0010(7) -0.0028(6) 0.0027(7) C17 0.0312(13) 0.0333(15) 0.0352(15) 0.0052(12) -0.0035(11) 0.0024(11) C18 0.0457(16) 0.0391(18) 0.052(2) 0.0080(15) -0.0011(13) 0.0124(13) C19 0.0537(18) 0.0413(18) 0.0517(19) -0.0007(15) 0.0040(14) 0.0221(14) O20 0.0503(10) 0.0359(11) 0.0370(12) -0.0069(9) -0.0002(8) 0.0140(9) C21 0.0431(15) 0.0365(17) 0.0339(16) 0.0082(12) -0.0044(12) -0.0029(12) O22 0.0632(12) 0.0382(12) 0.0326(10) 0.0027(10) -0.0027(8) -0.0067(10) C23 0.0619(18) 0.059(2) 0.0372(16) 0.0007(16) 0.0034(13) -0.0034(17) O24 0.0333(9) 0.0335(11) 0.0275(9) -0.0060(8) -0.0021(7) 0.0009(7) C25 0.0418(15) 0.0243(14) 0.0323(14) 0.0000(11) -0.0047(11) -0.0062(11) O26 0.0396(10) 0.0631(15) 0.0446(13) -0.0094(11) 0.0030(9) -0.0164(10) C27 0.0606(19) 0.0448(18) 0.0314(16) -0.0066(14) -0.0060(13) -0.0033(15) _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 Fe C14 2.022(2) . ? Fe C5 2.030(3) . ? Fe C10 2.032(2) . ? Fe C1 2.035(3) . ? Fe C12 2.036(3) . ? Fe C2 2.038(3) . ? Fe C4 2.039(3) . ? Fe C11 2.041(2) . ? Fe C13 2.042(3) . ? Fe C3 2.043(3) . ? C1 C5 1.416(4) . ? C1 C2 1.420(4) . ? C2 C3 1.407(4) . ? C3 C4 1.395(4) . ? C4 C5 1.401(4) . ? C10 C14 1.421(3) . ? C10 C11 1.440(3) . ? C10 C15 1.497(3) . ? C11 C12 1.415(4) . ? C12 C13 1.416(4) . ? C13 C14 1.414(3) . ? C14 O24 1.405(3) . ? C15 O20 1.403(3) . ? C15 O16 1.423(3) . ? O16 C17 1.437(3) . ? C17 C21 1.505(4) . ? C17 C18 1.527(4) . ? C18 C19 1.505(4) . ? C19 O20 1.446(3) . ? C21 O22 1.413(3) . ? O22 C23 1.418(3) . ? O24 C25 1.368(3) . ? C25 O26 1.197(3) . ? C25 C27 1.486(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Fe C5 107.23(10) . . ? C14 Fe C10 41.03(10) . . ? C5 Fe C10 122.52(11) . . ? C14 Fe C1 120.59(11) . . ? C5 Fe C1 40.77(11) . . ? C10 Fe C1 105.23(11) . . ? C14 Fe C12 68.16(10) . . ? C5 Fe C12 157.69(11) . . ? C10 Fe C12 69.29(10) . . ? C1 Fe C12 160.67(12) . . ? C14 Fe C2 156.55(11) . . ? C5 Fe C2 68.13(12) . . ? C10 Fe C2 120.59(11) . . ? C1 Fe C2 40.81(12) . . ? C12 Fe C2 124.86(12) . . ? C14 Fe C4 124.71(12) . . ? C5 Fe C4 40.27(11) . . ? C10 Fe C4 159.95(12) . . ? C1 Fe C4 68.11(12) . . ? C12 Fe C4 123.12(12) . . ? C2 Fe C4 67.54(13) . . ? C14 Fe C11 68.46(10) . . ? C5 Fe C11 160.04(11) . . ? C10 Fe C11 41.43(9) . . ? C1 Fe C11 123.27(12) . . ? C12 Fe C11 40.63(10) . . ? C2 Fe C11 107.61(12) . . ? C4 Fe C11 157.98(11) . . ? C14 Fe C13 40.73(10) . . ? C5 Fe C13 121.64(11) . . ? C10 Fe C13 69.50(10) . . ? C1 Fe C13 156.56(12) . . ? C12 Fe C13 40.62(10) . . ? C2 Fe C13 161.41(12) . . ? C4 Fe C13 108.66(13) . . ? C11 Fe C13 68.67(11) . . ? C14 Fe C3 161.23(12) . . ? C5 Fe C3 67.82(12) . . ? C10 Fe C3 157.09(12) . . ? C1 Fe C3 68.36(11) . . ? C12 Fe C3 109.10(11) . . ? C2 Fe C3 40.35(12) . . ? C4 Fe C3 39.97(13) . . ? C11 Fe C3 122.43(12) . . ? C13 Fe C3 125.09(12) . . ? C5 C1 C2 106.9(3) . . ? C5 C1 Fe 69.43(15) . . ? C2 C1 Fe 69.72(16) . . ? C3 C2 C1 108.2(3) . . ? C3 C2 Fe 69.99(16) . . ? C1 C2 Fe 69.47(15) . . ? C4 C3 C2 108.0(3) . . ? C4 C3 Fe 69.88(16) . . ? C2 C3 Fe 69.66(14) . . ? C3 C4 C5 108.7(3) . . ? C3 C4 Fe 70.15(16) . . ? C5 C4 Fe 69.52(15) . . ? C4 C5 C1 108.2(3) . . ? C4 C5 Fe 70.20(16) . . ? C1 C5 Fe 69.80(15) . . ? C14 C10 C11 106.0(2) . . ? C14 C10 C15 128.5(2) . . ? C11 C10 C15 125.4(2) . . ? C14 C10 Fe 69.12(13) . . ? C11 C10 Fe 69.62(13) . . ? C15 C10 Fe 127.95(17) . . ? C12 C11 C10 108.1(2) . . ? C12 C11 Fe 69.50(14) . . ? C10 C11 Fe 68.95(12) . . ? C11 C12 C13 108.9(2) . . ? C11 C12 Fe 69.88(14) . . ? C13 C12 Fe 69.95(14) . . ? C14 C13 C12 106.9(2) . . ? C14 C13 Fe 68.86(14) . . ? C12 C13 Fe 69.43(15) . . ? O24 C14 C13 123.0(2) . . ? O24 C14 C10 126.9(2) . . ? C13 C14 C10 110.0(2) . . ? O24 C14 Fe 123.49(15) . . ? C13 C14 Fe 70.42(14) . . ? C10 C14 Fe 69.85(13) . . ? O20 C15 O16 111.8(2) . . ? O20 C15 C10 108.3(2) . . ? O16 C15 C10 109.65(18) . . ? C15 O16 C17 110.12(17) . . ? O16 C17 C21 108.7(2) . . ? O16 C17 C18 109.5(2) . . ? C21 C17 C18 111.4(2) . . ? C19 C18 C17 110.1(2) . . ? O20 C19 C18 109.9(2) . . ? C15 O20 C19 110.2(2) . . ? O22 C21 C17 110.8(2) . . ? C21 O22 C23 112.0(2) . . ? C25 O24 C14 117.12(19) . . ? O26 C25 O24 123.4(2) . . ? O26 C25 C27 126.7(2) . . ? O24 C25 C27 109.9(2) . . ? 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 C14 Fe C1 C5 -80.87(18) . . . . ? C10 Fe C1 C5 -122.52(17) . . . . ? C12 Fe C1 C5 166.8(3) . . . . ? C2 Fe C1 C5 118.0(2) . . . . ? C4 Fe C1 C5 37.51(17) . . . . ? C11 Fe C1 C5 -163.85(15) . . . . ? C13 Fe C1 C5 -49.1(3) . . . . ? C3 Fe C1 C5 80.70(19) . . . . ? C14 Fe C1 C2 161.09(15) . . . . ? C5 Fe C1 C2 -118.0(2) . . . . ? C10 Fe C1 C2 119.45(17) . . . . ? C12 Fe C1 C2 48.8(4) . . . . ? C4 Fe C1 C2 -80.52(18) . . . . ? C11 Fe C1 C2 78.11(19) . . . . ? C13 Fe C1 C2 -167.1(2) . . . . ? C3 Fe C1 C2 -37.34(17) . . . . ? C5 C1 C2 C3 -0.3(3) . . . . ? Fe C1 C2 C3 59.48(18) . . . . ? C5 C1 C2 Fe -59.74(18) . . . . ? C14 Fe C2 C3 -163.9(2) . . . . ? C5 Fe C2 C3 -81.05(19) . . . . ? C10 Fe C2 C3 163.13(17) . . . . ? C1 Fe C2 C3 -119.4(3) . . . . ? C12 Fe C2 C3 78.2(2) . . . . ? C4 Fe C2 C3 -37.41(18) . . . . ? C11 Fe C2 C3 119.70(18) . . . . ? C13 Fe C2 C3 44.4(4) . . . . ? C14 Fe C2 C1 -44.5(3) . . . . ? C5 Fe C2 C1 38.40(17) . . . . ? C10 Fe C2 C1 -77.43(19) . . . . ? C12 Fe C2 C1 -162.33(16) . . . . ? C4 Fe C2 C1 82.04(18) . . . . ? C11 Fe C2 C1 -120.86(17) . . . . ? C13 Fe C2 C1 163.8(3) . . . . ? C3 Fe C2 C1 119.4(3) . . . . ? C1 C2 C3 C4 0.5(3) . . . . ? Fe C2 C3 C4 59.6(2) . . . . ? C1 C2 C3 Fe -59.16(18) . . . . ? C14 Fe C3 C4 40.9(4) . . . . ? C5 Fe C3 C4 -37.22(18) . . . . ? C10 Fe C3 C4 -159.0(3) . . . . ? C1 Fe C3 C4 -81.3(2) . . . . ? C12 Fe C3 C4 119.14(19) . . . . ? C2 Fe C3 C4 -119.1(3) . . . . ? C11 Fe C3 C4 162.12(18) . . . . ? C13 Fe C3 C4 76.7(2) . . . . ? C14 Fe C3 C2 160.0(3) . . . . ? C5 Fe C3 C2 81.86(19) . . . . ? C10 Fe C3 C2 -39.9(4) . . . . ? C1 Fe C3 C2 37.76(18) . . . . ? C12 Fe C3 C2 -121.78(19) . . . . ? C4 Fe C3 C2 119.1(3) . . . . ? C11 Fe C3 C2 -78.8(2) . . . . ? C13 Fe C3 C2 -164.19(18) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? Fe C3 C4 C5 59.00(19) . . . . ? C2 C3 C4 Fe -59.48(19) . . . . ? C14 Fe C4 C3 -165.14(17) . . . . ? C5 Fe C4 C3 119.9(3) . . . . ? C10 Fe C4 C3 156.0(3) . . . . ? C1 Fe C4 C3 82.0(2) . . . . ? C12 Fe C4 C3 -80.2(2) . . . . ? C2 Fe C4 C3 37.75(18) . . . . ? C11 Fe C4 C3 -43.7(4) . . . . ? C13 Fe C4 C3 -122.80(18) . . . . ? C14 Fe C4 C5 74.9(2) . . . . ? C10 Fe C4 C5 36.1(4) . . . . ? C1 Fe C4 C5 -37.96(17) . . . . ? C12 Fe C4 C5 159.85(17) . . . . ? C2 Fe C4 C5 -82.19(19) . . . . ? C11 Fe C4 C5 -163.6(3) . . . . ? C13 Fe C4 C5 117.26(18) . . . . ? C3 Fe C4 C5 -119.9(3) . . . . ? C3 C4 C5 C1 0.3(3) . . . . ? Fe C4 C5 C1 59.70(18) . . . . ? C3 C4 C5 Fe -59.4(2) . . . . ? C2 C1 C5 C4 0.0(3) . . . . ? Fe C1 C5 C4 -59.96(19) . . . . ? C2 C1 C5 Fe 59.92(18) . . . . ? C14 Fe C5 C4 -123.8(2) . . . . ? C10 Fe C5 C4 -166.15(18) . . . . ? C1 Fe C5 C4 119.1(3) . . . . ? C12 Fe C5 C4 -49.5(4) . . . . ? C2 Fe C5 C4 80.6(2) . . . . ? C11 Fe C5 C4 162.0(3) . . . . ? C13 Fe C5 C4 -81.6(2) . . . . ? C3 Fe C5 C4 36.95(19) . . . . ? C14 Fe C5 C1 117.14(17) . . . . ? C10 Fe C5 C1 74.78(19) . . . . ? C12 Fe C5 C1 -168.5(3) . . . . ? C2 Fe C5 C1 -38.44(17) . . . . ? C4 Fe C5 C1 -119.1(3) . . . . ? C11 Fe C5 C1 42.9(4) . . . . ? C13 Fe C5 C1 159.33(16) . . . . ? C3 Fe C5 C1 -82.11(18) . . . . ? C5 Fe C10 C14 78.60(17) . . . . ? C1 Fe C10 C14 119.38(16) . . . . ? C12 Fe C10 C14 -80.13(15) . . . . ? C2 Fe C10 C14 160.76(15) . . . . ? C4 Fe C10 C14 51.8(4) . . . . ? C11 Fe C10 C14 -117.2(2) . . . . ? C13 Fe C10 C14 -36.60(14) . . . . ? C3 Fe C10 C14 -170.4(3) . . . . ? C14 Fe C10 C11 117.2(2) . . . . ? C5 Fe C10 C11 -164.19(17) . . . . ? C1 Fe C10 C11 -123.42(17) . . . . ? C12 Fe C10 C11 37.07(16) . . . . ? C2 Fe C10 C11 -82.04(19) . . . . ? C4 Fe C10 C11 169.0(3) . . . . ? C13 Fe C10 C11 80.60(17) . . . . ? C3 Fe C10 C11 -53.2(3) . . . . ? C14 Fe C10 C15 -123.2(3) . . . . ? C5 Fe C10 C15 -44.6(3) . . . . ? C1 Fe C10 C15 -3.8(3) . . . . ? C12 Fe C10 C15 156.7(3) . . . . ? C2 Fe C10 C15 37.6(3) . . . . ? C4 Fe C10 C15 -71.4(4) . . . . ? C11 Fe C10 C15 119.6(3) . . . . ? C13 Fe C10 C15 -159.8(2) . . . . ? C3 Fe C10 C15 66.4(4) . . . . ? C14 C10 C11 C12 1.2(3) . . . . ? C15 C10 C11 C12 178.7(2) . . . . ? Fe C10 C11 C12 -58.59(16) . . . . ? C14 C10 C11 Fe 59.84(15) . . . . ? C15 C10 C11 Fe -122.7(2) . . . . ? C14 Fe C11 C12 81.14(16) . . . . ? C5 Fe C11 C12 162.3(3) . . . . ? C10 Fe C11 C12 120.0(2) . . . . ? C1 Fe C11 C12 -165.58(16) . . . . ? C2 Fe C11 C12 -123.43(17) . . . . ? C4 Fe C11 C12 -49.9(4) . . . . ? C13 Fe C11 C12 37.23(15) . . . . ? C3 Fe C11 C12 -81.65(19) . . . . ? C14 Fe C11 C10 -38.88(15) . . . . ? C5 Fe C11 C10 42.3(4) . . . . ? C1 Fe C11 C10 74.41(19) . . . . ? C12 Fe C11 C10 -120.0(2) . . . . ? C2 Fe C11 C10 116.55(17) . . . . ? C4 Fe C11 C10 -169.9(3) . . . . ? C13 Fe C11 C10 -82.78(16) . . . . ? C3 Fe C11 C10 158.34(16) . . . . ? C10 C11 C12 C13 -1.0(3) . . . . ? Fe C11 C12 C13 -59.25(18) . . . . ? C10 C11 C12 Fe 58.26(16) . . . . ? C14 Fe C12 C11 -81.93(16) . . . . ? C5 Fe C12 C11 -164.1(3) . . . . ? C10 Fe C12 C11 -37.77(15) . . . . ? C1 Fe C12 C11 39.0(4) . . . . ? C2 Fe C12 C11 75.78(18) . . . . ? C4 Fe C12 C11 159.96(17) . . . . ? C13 Fe C12 C11 -120.0(2) . . . . ? C3 Fe C12 C11 117.91(17) . . . . ? C14 Fe C12 C13 38.11(14) . . . . ? C5 Fe C12 C13 -44.1(3) . . . . ? C10 Fe C12 C13 82.28(16) . . . . ? C1 Fe C12 C13 159.0(3) . . . . ? C2 Fe C12 C13 -164.17(15) . . . . ? C4 Fe C12 C13 -79.99(19) . . . . ? C11 Fe C12 C13 120.0(2) . . . . ? C3 Fe C12 C13 -122.05(17) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? Fe C12 C13 C14 -58.87(17) . . . . ? C11 C12 C13 Fe 59.21(17) . . . . ? C5 Fe C13 C14 -79.48(17) . . . . ? C10 Fe C13 C14 36.86(14) . . . . ? C1 Fe C13 C14 -44.1(3) . . . . ? C12 Fe C13 C14 118.6(2) . . . . ? C2 Fe C13 C14 163.2(3) . . . . ? C4 Fe C13 C14 -121.94(16) . . . . ? C11 Fe C13 C14 81.35(15) . . . . ? C3 Fe C13 C14 -163.23(16) . . . . ? C14 Fe C13 C12 -118.6(2) . . . . ? C5 Fe C13 C12 161.93(15) . . . . ? C10 Fe C13 C12 -81.73(16) . . . . ? C1 Fe C13 C12 -162.7(2) . . . . ? C2 Fe C13 C12 44.6(4) . . . . ? C4 Fe C13 C12 119.48(16) . . . . ? C11 Fe C13 C12 -37.24(14) . . . . ? C3 Fe C13 C12 78.18(19) . . . . ? C12 C13 C14 O24 177.1(2) . . . . ? Fe C13 C14 O24 117.9(2) . . . . ? C12 C13 C14 C10 0.5(3) . . . . ? Fe C13 C14 C10 -58.77(16) . . . . ? C12 C13 C14 Fe 59.24(17) . . . . ? C11 C10 C14 O24 -177.5(2) . . . . ? C15 C10 C14 O24 5.2(4) . . . . ? Fe C10 C14 O24 -117.4(2) . . . . ? C11 C10 C14 C13 -1.1(3) . . . . ? C15 C10 C14 C13 -178.4(2) . . . . ? Fe C10 C14 C13 59.11(17) . . . . ? C11 C10 C14 Fe -60.17(15) . . . . ? C15 C10 C14 Fe 122.5(2) . . . . ? C5 Fe C14 O24 1.6(2) . . . . ? C10 Fe C14 O24 121.7(3) . . . . ? C1 Fe C14 O24 44.0(2) . . . . ? C12 Fe C14 O24 -155.2(2) . . . . ? C2 Fe C14 O24 76.2(3) . . . . ? C4 Fe C14 O24 -39.2(2) . . . . ? C11 Fe C14 O24 160.9(2) . . . . ? C13 Fe C14 O24 -117.2(3) . . . . ? C3 Fe C14 O24 -70.0(4) . . . . ? C5 Fe C14 C13 118.79(16) . . . . ? C10 Fe C14 C13 -121.1(2) . . . . ? C1 Fe C14 C13 161.25(16) . . . . ? C12 Fe C14 C13 -38.01(15) . . . . ? C2 Fe C14 C13 -166.6(3) . . . . ? C4 Fe C14 C13 77.99(19) . . . . ? C11 Fe C14 C13 -81.89(16) . . . . ? C3 Fe C14 C13 47.2(4) . . . . ? C5 Fe C14 C10 -120.07(15) . . . . ? C1 Fe C14 C10 -77.61(17) . . . . ? C12 Fe C14 C10 83.12(15) . . . . ? C2 Fe C14 C10 -45.5(3) . . . . ? C4 Fe C14 C10 -160.87(16) . . . . ? C11 Fe C14 C10 39.25(14) . . . . ? C13 Fe C14 C10 121.1(2) . . . . ? C3 Fe C14 C10 168.3(3) . . . . ? C14 C10 C15 O20 -158.7(2) . . . . ? C11 C10 C15 O20 24.4(3) . . . . ? Fe C10 C15 O20 -66.3(3) . . . . ? C14 C10 C15 O16 -36.5(3) . . . . ? C11 C10 C15 O16 146.7(2) . . . . ? Fe C10 C15 O16 56.0(3) . . . . ? O20 C15 O16 C17 -63.6(2) . . . . ? C10 C15 O16 C17 176.30(19) . . . . ? C15 O16 C17 C21 179.0(2) . . . . ? C15 O16 C17 C18 57.1(3) . . . . ? O16 C17 C18 C19 -52.9(3) . . . . ? C21 C17 C18 C19 -173.1(2) . . . . ? C17 C18 C19 O20 52.8(3) . . . . ? O16 C15 O20 C19 63.3(2) . . . . ? C10 C15 O20 C19 -175.8(2) . . . . ? C18 C19 O20 C15 -57.6(3) . . . . ? O16 C17 C21 O22 68.8(3) . . . . ? C18 C17 C21 O22 -170.5(2) . . . . ? C17 C21 O22 C23 178.7(2) . . . . ? C13 C14 O24 C25 123.9(2) . . . . ? C10 C14 O24 C25 -60.0(3) . . . . ? Fe C14 O24 C25 -148.91(18) . . . . ? C14 O24 C25 O26 -7.1(4) . . . . ? C14 O24 C25 C27 172.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.417 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.053 # Attachment 'SSpR17.cif' data_erk4239 _database_code_depnum_ccdc_archive 'CCDC 714360' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H27 Fe I O3 Si' _chemical_formula_weight 514.25 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.6461(2) _cell_length_b 10.4222(2) _cell_length_c 12.2221(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.712(1) _cell_angle_gamma 90.00 _cell_volume 1093.80(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2113 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 2.169 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5173 _exptl_absorpt_correction_T_max 0.8993 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7850 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.86 _reflns_number_total 4845 _reflns_number_gt 4188 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0330P)^2^+0.3261P] 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 riding _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 0.020(18) _refine_ls_number_reflns 4845 _refine_ls_number_parameters 230 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Fe Fe -0.36530(6) 0.18730(4) 0.15190(4) 0.03459(13) Uani 1 1 d . . . C1 C -0.2055(6) 0.1262(4) 0.2768(5) 0.0632(15) Uani 1 1 d . . . H1 H -0.1489 0.1795 0.3292 0.076 Uiso 1 1 calc R . . C2 C -0.3521(6) 0.0683(4) 0.2875(4) 0.0613(13) Uani 1 1 d . . . H2 H -0.4089 0.0750 0.3483 0.074 Uiso 1 1 calc R . . C3 C -0.3961(6) -0.0008(4) 0.1897(4) 0.0577(12) Uani 1 1 d . . . H3 H -0.4891 -0.0473 0.1732 0.069 Uiso 1 1 calc R . . C4 C -0.2767(6) 0.0116(4) 0.1208(5) 0.0602(12) Uani 1 1 d . . . H4 H -0.2751 -0.0259 0.0510 0.072 Uiso 1 1 calc R . . C5 C -0.1604(6) 0.0904(4) 0.1759(5) 0.0629(14) Uani 1 1 d . . . H5 H -0.0674 0.1147 0.1487 0.075 Uiso 1 1 calc R . . C10 C -0.3622(4) 0.3824(3) 0.1464(2) 0.0282(7) Uani 1 1 d . . . C11 C -0.5121(4) 0.3401(3) 0.1742(3) 0.0330(7) Uani 1 1 d . . . C12 C -0.5741(5) 0.2590(4) 0.0839(3) 0.0439(10) Uani 1 1 d . . . H12 H -0.6707 0.2167 0.0793 0.053 Uiso 1 1 calc R . . C13 C -0.4698(5) 0.2518(4) 0.0035(4) 0.0468(10) Uani 1 1 d . . . H13 H -0.4841 0.2054 -0.0629 0.056 Uiso 1 1 calc R . . C14 C -0.3388(4) 0.3287(3) 0.0426(3) 0.0377(9) Uani 1 1 d . . . I1 I -0.14748(3) 0.36361(4) -0.043186(19) 0.06119(11) Uani 1 1 d . . . C15 C -0.2481(4) 0.4714(3) 0.2092(3) 0.0265(7) Uani 1 1 d . . . H15 H -0.1411 0.4465 0.1967 0.032 Uiso 1 1 calc R . . O16 O -0.2626(3) 0.4645(2) 0.32185(19) 0.0330(5) Uani 1 1 d . . . C17 C -0.1512(4) 0.5462(4) 0.3845(3) 0.0363(8) Uani 1 1 d . . . H17 H -0.0446 0.5167 0.3755 0.044 Uiso 1 1 calc R . . C18 C -0.1719(5) 0.6828(4) 0.3436(4) 0.0514(10) Uani 1 1 d . . . H18A H -0.2722 0.7165 0.3608 0.062 Uiso 1 1 calc R . . H18B H -0.0889 0.7371 0.3803 0.062 Uiso 1 1 calc R . . C19 C -0.1663(5) 0.6847(4) 0.2205(4) 0.0495(10) Uani 1 1 d . . . H19A H -0.1883 0.7716 0.1922 0.059 Uiso 1 1 calc R . . H19B H -0.0619 0.6604 0.2042 0.059 Uiso 1 1 calc R . . O20 O -0.2799(3) 0.5962(2) 0.1672(2) 0.0411(6) Uani 1 1 d . . . C21 C -0.1781(6) 0.5345(4) 0.5041(3) 0.0516(11) Uani 1 1 d . . . H21A H -0.1107 0.5952 0.5486 0.062 Uiso 1 1 calc R . . H21B H -0.2866 0.5557 0.5122 0.062 Uiso 1 1 calc R . . O22 O -0.1458(4) 0.4110(3) 0.5408(2) 0.0542(8) Uani 1 1 d . . . C23 C -0.1808(6) 0.3971(5) 0.6515(3) 0.0640(14) Uani 1 1 d . . . H23A H -0.1104 0.4500 0.6999 0.096 Uiso 1 1 calc R . . H23B H -0.1684 0.3080 0.6737 0.096 Uiso 1 1 calc R . . H23C H -0.2873 0.4239 0.6561 0.096 Uiso 1 1 calc R . . Si1 Si -0.62030(12) 0.38189(10) 0.29320(9) 0.0421(2) Uani 1 1 d . . . C24 C -0.8145(5) 0.3005(5) 0.2644(5) 0.0639(13) Uani 1 1 d . . . H24A H -0.7991 0.2088 0.2572 0.096 Uiso 1 1 calc R . . H24B H -0.8690 0.3338 0.1965 0.096 Uiso 1 1 calc R . . H24C H -0.8756 0.3167 0.3247 0.096 Uiso 1 1 calc R . . C25 C -0.5320(6) 0.3270(5) 0.4317(4) 0.0579(12) Uani 1 1 d . . . H25A H -0.5478 0.2353 0.4384 0.087 Uiso 1 1 calc R . . H25B H -0.5809 0.3715 0.4882 0.087 Uiso 1 1 calc R . . H25C H -0.4213 0.3454 0.4404 0.087 Uiso 1 1 calc R . . C26 C -0.6520(6) 0.5597(5) 0.2945(5) 0.0720(15) Uani 1 1 d . . . H26A H -0.6961 0.5836 0.3610 0.108 Uiso 1 1 calc R . . H26B H -0.7230 0.5842 0.2306 0.108 Uiso 1 1 calc R . . H26C H -0.5532 0.6033 0.2926 0.108 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 Fe 0.0346(3) 0.0277(2) 0.0389(3) -0.0028(2) -0.0066(2) 0.0004(2) C1 0.064(3) 0.039(2) 0.077(4) 0.011(2) -0.031(3) 0.003(2) C2 0.079(4) 0.045(2) 0.058(3) 0.020(2) 0.002(2) 0.014(2) C3 0.058(3) 0.035(2) 0.078(4) 0.003(2) -0.004(3) -0.0022(19) C4 0.070(3) 0.036(2) 0.075(3) -0.010(2) 0.009(3) 0.011(2) C5 0.041(3) 0.045(2) 0.102(4) 0.009(3) 0.003(3) 0.014(2) C10 0.0301(17) 0.0261(16) 0.0270(15) 0.0026(14) -0.0029(13) 0.0024(14) C11 0.0292(17) 0.0311(17) 0.0369(17) 0.0038(15) -0.0040(14) 0.0023(14) C12 0.035(2) 0.042(2) 0.050(2) -0.0016(18) -0.0132(19) 0.0001(16) C13 0.046(2) 0.049(2) 0.041(2) -0.0040(18) -0.0145(19) 0.0017(18) C14 0.043(2) 0.043(2) 0.0262(16) 0.0016(15) -0.0001(15) -0.0003(15) I1 0.06144(19) 0.0919(2) 0.03265(13) -0.00480(16) 0.01574(11) -0.00204(18) C15 0.0264(17) 0.0265(15) 0.0262(17) 0.0029(13) 0.0008(13) 0.0032(13) O16 0.0399(15) 0.0323(12) 0.0266(12) -0.0015(10) 0.0032(11) -0.0093(10) C17 0.041(2) 0.0366(18) 0.0312(18) -0.0038(16) 0.0027(15) -0.0091(16) C18 0.057(3) 0.0337(17) 0.063(3) -0.012(2) 0.008(2) -0.010(2) C19 0.062(3) 0.0294(16) 0.056(3) 0.012(2) 0.002(2) -0.010(2) O20 0.0447(16) 0.0295(12) 0.0471(16) 0.0110(12) -0.0039(12) -0.0041(11) C21 0.064(3) 0.048(2) 0.040(2) -0.015(2) -0.006(2) -0.009(2) O22 0.068(2) 0.0574(18) 0.0357(14) -0.0005(13) -0.0008(14) 0.0078(14) C23 0.076(3) 0.087(4) 0.0283(19) 0.005(2) 0.004(2) -0.012(3) Si1 0.0324(5) 0.0405(6) 0.0551(6) 0.0019(5) 0.0119(4) 0.0000(5) C24 0.034(2) 0.069(3) 0.089(4) 0.011(3) 0.007(2) -0.008(2) C25 0.057(3) 0.069(3) 0.049(2) 0.006(2) 0.013(2) -0.013(2) C26 0.068(3) 0.054(3) 0.101(4) -0.001(3) 0.036(3) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C14 2.020(3) . ? Fe C5 2.031(4) . ? Fe C10 2.035(3) . ? Fe C4 2.038(4) . ? Fe C1 2.038(4) . ? Fe C3 2.039(4) . ? Fe C12 2.039(4) . ? Fe C13 2.043(4) . ? Fe C2 2.062(4) . ? Fe C11 2.075(3) . ? C1 C5 1.387(8) . ? C1 C2 1.424(7) . ? C2 C3 1.409(7) . ? C3 C4 1.413(8) . ? C4 C5 1.407(7) . ? C10 C14 1.423(4) . ? C10 C11 1.446(5) . ? C10 C15 1.498(4) . ? C11 C12 1.443(5) . ? C11 Si1 1.870(4) . ? C12 C13 1.411(6) . ? C13 C14 1.424(5) . ? C14 I1 2.091(4) . ? C15 O16 1.399(4) . ? C15 O20 1.414(4) . ? O16 C17 1.437(4) . ? C17 C21 1.512(6) . ? C17 C18 1.513(6) . ? C18 C19 1.511(6) . ? C19 O20 1.446(5) . ? C21 O22 1.381(5) . ? O22 C23 1.427(5) . ? Si1 C25 1.864(5) . ? Si1 C26 1.874(5) . ? Si1 C24 1.877(5) . ? 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 C14 Fe C5 107.09(19) . . ? C14 Fe C10 41.09(13) . . ? C5 Fe C10 119.18(17) . . ? C14 Fe C4 117.26(19) . . ? C5 Fe C4 40.5(2) . . ? C10 Fe C4 152.29(18) . . ? C14 Fe C1 127.16(18) . . ? C5 Fe C1 39.9(2) . . ? C10 Fe C1 109.07(15) . . ? C4 Fe C1 67.8(2) . . ? C14 Fe C3 151.57(18) . . ? C5 Fe C3 67.9(2) . . ? C10 Fe C3 166.14(19) . . ? C4 Fe C3 40.5(2) . . ? C1 Fe C3 67.95(19) . . ? C14 Fe C12 68.08(16) . . ? C5 Fe C12 163.2(2) . . ? C10 Fe C12 68.57(14) . . ? C4 Fe C12 125.99(19) . . ? C1 Fe C12 155.6(2) . . ? C3 Fe C12 108.17(19) . . ? C14 Fe C13 41.02(15) . . ? C5 Fe C13 125.4(2) . . ? C10 Fe C13 69.39(14) . . ? C4 Fe C13 105.50(19) . . ? C1 Fe C13 163.5(2) . . ? C3 Fe C13 117.50(19) . . ? C12 Fe C13 40.44(18) . . ? C14 Fe C2 165.98(18) . . ? C5 Fe C2 67.6(2) . . ? C10 Fe C2 128.87(17) . . ? C4 Fe C2 67.8(2) . . ? C1 Fe C2 40.6(2) . . ? C3 Fe C2 40.2(2) . . ? C12 Fe C2 120.7(2) . . ? C13 Fe C2 152.66(19) . . ? C14 Fe C11 69.22(14) . . ? C5 Fe C11 154.15(18) . . ? C10 Fe C11 41.19(13) . . ? C4 Fe C11 164.50(18) . . ? C1 Fe C11 120.89(19) . . ? C3 Fe C11 127.62(18) . . ? C12 Fe C11 41.06(15) . . ? C13 Fe C11 69.51(16) . . ? C2 Fe C11 109.48(18) . . ? C5 C1 C2 108.2(4) . . ? C5 C1 Fe 69.8(3) . . ? C2 C1 Fe 70.6(2) . . ? C3 C2 C1 107.1(5) . . ? C3 C2 Fe 69.0(3) . . ? C1 C2 Fe 68.8(3) . . ? C2 C3 C4 108.4(5) . . ? C2 C3 Fe 70.8(2) . . ? C4 C3 Fe 69.7(3) . . ? C5 C4 C3 107.4(5) . . ? C5 C4 Fe 69.5(2) . . ? C3 C4 Fe 69.8(2) . . ? C1 C5 C4 108.9(5) . . ? C1 C5 Fe 70.4(3) . . ? C4 C5 Fe 70.1(3) . . ? C14 C10 C11 108.3(3) . . ? C14 C10 C15 123.1(3) . . ? C11 C10 C15 128.5(3) . . ? C14 C10 Fe 68.88(19) . . ? C11 C10 Fe 70.87(19) . . ? C15 C10 Fe 127.7(2) . . ? C12 C11 C10 105.2(3) . . ? C12 C11 Si1 123.8(3) . . ? C10 C11 Si1 130.9(3) . . ? C12 C11 Fe 68.1(2) . . ? C10 C11 Fe 67.94(19) . . ? Si1 C11 Fe 130.54(18) . . ? C13 C12 C11 110.7(4) . . ? C13 C12 Fe 69.9(2) . . ? C11 C12 Fe 70.8(2) . . ? C12 C13 C14 106.5(3) . . ? C12 C13 Fe 69.6(2) . . ? C14 C13 Fe 68.6(2) . . ? C10 C14 C13 109.3(3) . . ? C10 C14 Fe 70.03(19) . . ? C13 C14 Fe 70.4(2) . . ? C10 C14 I1 125.6(2) . . ? C13 C14 I1 125.1(3) . . ? Fe C14 I1 128.05(18) . . ? O16 C15 O20 111.6(3) . . ? O16 C15 C10 110.1(3) . . ? O20 C15 C10 107.2(3) . . ? C15 O16 C17 111.2(3) . . ? O16 C17 C21 107.3(3) . . ? O16 C17 C18 109.6(3) . . ? C21 C17 C18 111.7(3) . . ? C19 C18 C17 108.9(3) . . ? O20 C19 C18 109.9(3) . . ? C15 O20 C19 109.3(3) . . ? O22 C21 C17 110.0(3) . . ? C21 O22 C23 110.2(3) . . ? C25 Si1 C11 116.47(19) . . ? C25 Si1 C26 109.9(3) . . ? C11 Si1 C26 108.9(2) . . ? C25 Si1 C24 107.1(2) . . ? C11 Si1 C24 105.5(2) . . ? C26 Si1 C24 108.7(2) . . ? 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 C14 Fe C1 C5 -70.6(3) . . . . ? C10 Fe C1 C5 -113.0(3) . . . . ? C4 Fe C1 C5 37.5(3) . . . . ? C3 Fe C1 C5 81.5(3) . . . . ? C12 Fe C1 C5 167.0(4) . . . . ? C13 Fe C1 C5 -31.3(8) . . . . ? C2 Fe C1 C5 118.9(4) . . . . ? C11 Fe C1 C5 -156.9(3) . . . . ? C14 Fe C1 C2 170.5(3) . . . . ? C5 Fe C1 C2 -118.9(4) . . . . ? C10 Fe C1 C2 128.1(3) . . . . ? C4 Fe C1 C2 -81.4(3) . . . . ? C3 Fe C1 C2 -37.4(3) . . . . ? C12 Fe C1 C2 48.1(5) . . . . ? C13 Fe C1 C2 -150.2(6) . . . . ? C11 Fe C1 C2 84.2(3) . . . . ? C5 C1 C2 C3 -1.3(5) . . . . ? Fe C1 C2 C3 58.6(3) . . . . ? C5 C1 C2 Fe -59.9(3) . . . . ? C14 Fe C2 C3 -152.1(7) . . . . ? C5 Fe C2 C3 -81.8(3) . . . . ? C10 Fe C2 C3 168.0(3) . . . . ? C4 Fe C2 C3 -37.9(3) . . . . ? C1 Fe C2 C3 -119.1(5) . . . . ? C12 Fe C2 C3 81.9(3) . . . . ? C13 Fe C2 C3 42.9(6) . . . . ? C11 Fe C2 C3 125.8(3) . . . . ? C14 Fe C2 C1 -33.0(9) . . . . ? C5 Fe C2 C1 37.4(3) . . . . ? C10 Fe C2 C1 -72.8(4) . . . . ? C4 Fe C2 C1 81.2(3) . . . . ? C3 Fe C2 C1 119.1(5) . . . . ? C12 Fe C2 C1 -159.0(3) . . . . ? C13 Fe C2 C1 162.1(4) . . . . ? C11 Fe C2 C1 -115.1(3) . . . . ? C1 C2 C3 C4 1.4(5) . . . . ? Fe C2 C3 C4 59.8(3) . . . . ? C1 C2 C3 Fe -58.4(3) . . . . ? C14 Fe C3 C2 166.2(3) . . . . ? C5 Fe C3 C2 81.0(4) . . . . ? C10 Fe C3 C2 -42.4(8) . . . . ? C4 Fe C3 C2 119.0(4) . . . . ? C1 Fe C3 C2 37.9(3) . . . . ? C12 Fe C3 C2 -116.4(3) . . . . ? C13 Fe C3 C2 -159.4(3) . . . . ? C11 Fe C3 C2 -74.9(4) . . . . ? C14 Fe C3 C4 47.2(5) . . . . ? C5 Fe C3 C4 -37.9(3) . . . . ? C10 Fe C3 C4 -161.4(6) . . . . ? C1 Fe C3 C4 -81.1(3) . . . . ? C12 Fe C3 C4 124.6(3) . . . . ? C13 Fe C3 C4 81.7(3) . . . . ? C2 Fe C3 C4 -119.0(4) . . . . ? C11 Fe C3 C4 166.1(3) . . . . ? C2 C3 C4 C5 -1.0(5) . . . . ? Fe C3 C4 C5 59.5(3) . . . . ? C2 C3 C4 Fe -60.5(3) . . . . ? C14 Fe C4 C5 84.6(4) . . . . ? C10 Fe C4 C5 51.9(5) . . . . ? C1 Fe C4 C5 -37.0(3) . . . . ? C3 Fe C4 C5 -118.6(5) . . . . ? C12 Fe C4 C5 166.2(3) . . . . ? C13 Fe C4 C5 127.0(4) . . . . ? C2 Fe C4 C5 -81.0(4) . . . . ? C11 Fe C4 C5 -164.0(6) . . . . ? C14 Fe C4 C3 -156.8(3) . . . . ? C5 Fe C4 C3 118.6(5) . . . . ? C10 Fe C4 C3 170.5(3) . . . . ? C1 Fe C4 C3 81.6(3) . . . . ? C12 Fe C4 C3 -75.2(4) . . . . ? C13 Fe C4 C3 -114.4(3) . . . . ? C2 Fe C4 C3 37.5(3) . . . . ? C11 Fe C4 C3 -45.4(8) . . . . ? C2 C1 C5 C4 0.7(5) . . . . ? Fe C1 C5 C4 -59.7(3) . . . . ? C2 C1 C5 Fe 60.4(3) . . . . ? C3 C4 C5 C1 0.2(5) . . . . ? Fe C4 C5 C1 59.9(3) . . . . ? C3 C4 C5 Fe -59.7(3) . . . . ? C14 Fe C5 C1 128.1(3) . . . . ? C10 Fe C5 C1 85.1(3) . . . . ? C4 Fe C5 C1 -119.6(5) . . . . ? C3 Fe C5 C1 -81.6(3) . . . . ? C12 Fe C5 C1 -161.3(6) . . . . ? C13 Fe C5 C1 169.6(3) . . . . ? C2 Fe C5 C1 -38.1(3) . . . . ? C11 Fe C5 C1 50.6(6) . . . . ? C14 Fe C5 C4 -112.2(3) . . . . ? C10 Fe C5 C4 -155.2(3) . . . . ? C1 Fe C5 C4 119.6(5) . . . . ? C3 Fe C5 C4 38.0(3) . . . . ? C12 Fe C5 C4 -41.6(8) . . . . ? C13 Fe C5 C4 -70.8(4) . . . . ? C2 Fe C5 C4 81.6(3) . . . . ? C11 Fe C5 C4 170.3(4) . . . . ? C5 Fe C10 C14 82.6(3) . . . . ? C4 Fe C10 C14 46.8(4) . . . . ? C1 Fe C10 C14 125.2(3) . . . . ? C3 Fe C10 C14 -159.7(6) . . . . ? C12 Fe C10 C14 -80.8(2) . . . . ? C13 Fe C10 C14 -37.3(2) . . . . ? C2 Fe C10 C14 166.3(3) . . . . ? C11 Fe C10 C14 -119.4(3) . . . . ? C14 Fe C10 C11 119.4(3) . . . . ? C5 Fe C10 C11 -158.0(3) . . . . ? C4 Fe C10 C11 166.2(4) . . . . ? C1 Fe C10 C11 -115.5(3) . . . . ? C3 Fe C10 C11 -40.3(7) . . . . ? C12 Fe C10 C11 38.6(2) . . . . ? C13 Fe C10 C11 82.1(2) . . . . ? C2 Fe C10 C11 -74.3(3) . . . . ? C14 Fe C10 C15 -116.2(4) . . . . ? C5 Fe C10 C15 -33.6(4) . . . . ? C4 Fe C10 C15 -69.4(5) . . . . ? C1 Fe C10 C15 9.0(4) . . . . ? C3 Fe C10 C15 84.1(7) . . . . ? C12 Fe C10 C15 163.0(3) . . . . ? C13 Fe C10 C15 -153.5(3) . . . . ? C2 Fe C10 C15 50.1(4) . . . . ? C11 Fe C10 C15 124.4(4) . . . . ? C14 C10 C11 C12 0.6(4) . . . . ? C15 C10 C11 C12 178.3(3) . . . . ? Fe C10 C11 C12 -58.3(2) . . . . ? C14 C10 C11 Si1 -175.9(3) . . . . ? C15 C10 C11 Si1 1.8(5) . . . . ? Fe C10 C11 Si1 125.2(3) . . . . ? C14 C10 C11 Fe 58.9(2) . . . . ? C15 C10 C11 Fe -123.5(3) . . . . ? C14 Fe C11 C12 80.1(2) . . . . ? C5 Fe C11 C12 166.5(5) . . . . ? C10 Fe C11 C12 117.9(3) . . . . ? C4 Fe C11 C12 -37.6(8) . . . . ? C1 Fe C11 C12 -158.2(3) . . . . ? C3 Fe C11 C12 -73.4(3) . . . . ? C13 Fe C11 C12 36.1(2) . . . . ? C2 Fe C11 C12 -114.8(3) . . . . ? C14 Fe C11 C10 -37.78(18) . . . . ? C5 Fe C11 C10 48.7(5) . . . . ? C4 Fe C11 C10 -155.5(7) . . . . ? C1 Fe C11 C10 83.9(3) . . . . ? C3 Fe C11 C10 168.7(2) . . . . ? C12 Fe C11 C10 -117.9(3) . . . . ? C13 Fe C11 C10 -81.8(2) . . . . ? C2 Fe C11 C10 127.4(2) . . . . ? C14 Fe C11 Si1 -163.4(3) . . . . ? C5 Fe C11 Si1 -77.0(5) . . . . ? C10 Fe C11 Si1 -125.7(3) . . . . ? C4 Fe C11 Si1 78.8(7) . . . . ? C1 Fe C11 Si1 -41.7(3) . . . . ? C3 Fe C11 Si1 43.0(3) . . . . ? C12 Fe C11 Si1 116.5(4) . . . . ? C13 Fe C11 Si1 152.6(3) . . . . ? C2 Fe C11 Si1 1.7(3) . . . . ? C10 C11 C12 C13 -0.6(4) . . . . ? Si1 C11 C12 C13 176.3(3) . . . . ? Fe C11 C12 C13 -58.7(3) . . . . ? C10 C11 C12 Fe 58.1(2) . . . . ? Si1 C11 C12 Fe -125.1(3) . . . . ? C14 Fe C12 C13 38.6(2) . . . . ? C5 Fe C12 C13 -37.8(7) . . . . ? C10 Fe C12 C13 83.0(2) . . . . ? C4 Fe C12 C13 -69.9(3) . . . . ? C1 Fe C12 C13 172.1(4) . . . . ? C3 Fe C12 C13 -111.4(3) . . . . ? C2 Fe C12 C13 -153.6(3) . . . . ? C11 Fe C12 C13 121.7(3) . . . . ? C14 Fe C12 C11 -83.1(2) . . . . ? C5 Fe C12 C11 -159.5(6) . . . . ? C10 Fe C12 C11 -38.7(2) . . . . ? C4 Fe C12 C11 168.4(3) . . . . ? C1 Fe C12 C11 50.4(5) . . . . ? C3 Fe C12 C11 127.0(3) . . . . ? C13 Fe C12 C11 -121.7(3) . . . . ? C2 Fe C12 C11 84.7(3) . . . . ? C11 C12 C13 C14 0.3(4) . . . . ? Fe C12 C13 C14 -58.9(2) . . . . ? C11 C12 C13 Fe 59.2(3) . . . . ? C14 Fe C13 C12 -118.2(3) . . . . ? C5 Fe C13 C12 167.4(3) . . . . ? C10 Fe C13 C12 -80.8(2) . . . . ? C4 Fe C13 C12 127.9(3) . . . . ? C1 Fe C13 C12 -168.5(6) . . . . ? C3 Fe C13 C12 86.1(3) . . . . ? C2 Fe C13 C12 56.4(5) . . . . ? C11 Fe C13 C12 -36.6(2) . . . . ? C5 Fe C13 C14 -74.4(3) . . . . ? C10 Fe C13 C14 37.4(2) . . . . ? C4 Fe C13 C14 -113.9(3) . . . . ? C1 Fe C13 C14 -50.3(7) . . . . ? C3 Fe C13 C14 -155.8(3) . . . . ? C12 Fe C13 C14 118.2(3) . . . . ? C2 Fe C13 C14 174.5(4) . . . . ? C11 Fe C13 C14 81.5(2) . . . . ? C11 C10 C14 C13 -0.5(4) . . . . ? C15 C10 C14 C13 -178.3(3) . . . . ? Fe C10 C14 C13 59.6(3) . . . . ? C11 C10 C14 Fe -60.1(2) . . . . ? C15 C10 C14 Fe 122.1(3) . . . . ? C11 C10 C14 I1 176.8(2) . . . . ? C15 C10 C14 I1 -1.0(5) . . . . ? Fe C10 C14 I1 -123.1(3) . . . . ? C12 C13 C14 C10 0.1(4) . . . . ? Fe C13 C14 C10 -59.4(2) . . . . ? C12 C13 C14 Fe 59.6(3) . . . . ? C12 C13 C14 I1 -177.1(3) . . . . ? Fe C13 C14 I1 123.3(3) . . . . ? C5 Fe C14 C10 -115.1(2) . . . . ? C4 Fe C14 C10 -157.6(2) . . . . ? C1 Fe C14 C10 -75.8(3) . . . . ? C3 Fe C14 C10 170.0(3) . . . . ? C12 Fe C14 C10 82.1(2) . . . . ? C13 Fe C14 C10 120.1(3) . . . . ? C2 Fe C14 C10 -49.4(8) . . . . ? C11 Fe C14 C10 37.86(18) . . . . ? C5 Fe C14 C13 124.8(3) . . . . ? C10 Fe C14 C13 -120.1(3) . . . . ? C4 Fe C14 C13 82.3(3) . . . . ? C1 Fe C14 C13 164.1(3) . . . . ? C3 Fe C14 C13 49.8(5) . . . . ? C12 Fe C14 C13 -38.1(2) . . . . ? C2 Fe C14 C13 -169.6(7) . . . . ? C11 Fe C14 C13 -82.3(2) . . . . ? C5 Fe C14 I1 5.1(3) . . . . ? C10 Fe C14 I1 120.1(3) . . . . ? C4 Fe C14 I1 -37.4(3) . . . . ? C1 Fe C14 I1 44.3(3) . . . . ? C3 Fe C14 I1 -69.9(4) . . . . ? C12 Fe C14 I1 -157.8(3) . . . . ? C13 Fe C14 I1 -119.7(3) . . . . ? C2 Fe C14 I1 70.7(8) . . . . ? C11 Fe C14 I1 158.0(2) . . . . ? C14 C10 C15 O16 -154.2(3) . . . . ? C11 C10 C15 O16 28.5(4) . . . . ? Fe C10 C15 O16 -66.5(4) . . . . ? C14 C10 C15 O20 84.2(4) . . . . ? C11 C10 C15 O20 -93.1(4) . . . . ? Fe C10 C15 O20 171.9(2) . . . . ? O20 C15 O16 C17 -62.8(4) . . . . ? C10 C15 O16 C17 178.3(3) . . . . ? C15 O16 C17 C21 178.8(3) . . . . ? C15 O16 C17 C18 57.3(4) . . . . ? O16 C17 C18 C19 -53.2(4) . . . . ? C21 C17 C18 C19 -172.0(4) . . . . ? C17 C18 C19 O20 54.6(5) . . . . ? O16 C15 O20 C19 63.0(4) . . . . ? C10 C15 O20 C19 -176.4(3) . . . . ? C18 C19 O20 C15 -58.9(4) . . . . ? O16 C17 C21 O22 64.7(4) . . . . ? C18 C17 C21 O22 -175.2(3) . . . . ? C17 C21 O22 C23 -176.2(4) . . . . ? C12 C11 Si1 C25 117.4(3) . . . . ? C10 C11 Si1 C25 -66.6(4) . . . . ? Fe C11 Si1 C25 28.4(3) . . . . ? C12 C11 Si1 C26 -117.6(4) . . . . ? C10 C11 Si1 C26 58.3(4) . . . . ? Fe C11 Si1 C26 153.3(3) . . . . ? C12 C11 Si1 C24 -1.1(4) . . . . ? C10 C11 Si1 C24 174.8(3) . . . . ? Fe C11 Si1 C24 -90.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.407 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.068 # Attachment 'SSpS16.cif' data_erk4247 _database_code_depnum_ccdc_archive 'CCDC 714361' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H28 Fe O3 Si' _chemical_formula_weight 388.35 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.4036(2) _cell_length_b 10.1503(2) _cell_length_c 11.0179(3) _cell_angle_alpha 102.777(1) _cell_angle_beta 104.675(1) _cell_angle_gamma 91.046(1) _cell_volume 989.07(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1841 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8183 _exptl_absorpt_correction_T_max 0.8506 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9259 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.25 _reflns_number_total 6913 _reflns_number_gt 6087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0500P)^2^+0.4365P] 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 riding _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 -0.004(13) _refine_ls_number_reflns 6913 _refine_ls_number_parameters 441 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0979 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Fe1A Fe 0.47712(5) 0.53740(4) 0.16327(4) 0.03119(13) Uani 1 1 d . . . Si1A Si 0.83819(12) 0.49933(11) 0.13295(11) 0.0365(3) Uani 1 1 d . . . C1A C 0.4649(6) 0.7419(4) 0.1970(5) 0.0533(12) Uani 1 1 d . . . H1A H 0.4838 0.7983 0.1448 0.064 Uiso 1 1 calc R . . C2A C 0.3279(6) 0.6777(5) 0.1867(5) 0.0607(14) Uani 1 1 d . . . H2A H 0.2390 0.6828 0.1260 0.073 Uiso 1 1 calc R . . C3A C 0.3468(6) 0.6036(5) 0.2834(5) 0.0547(13) Uani 1 1 d . . . H3A H 0.2727 0.5511 0.2987 0.066 Uiso 1 1 calc R . . C4A C 0.4976(6) 0.6227(4) 0.3533(4) 0.0504(12) Uani 1 1 d . . . H4A H 0.5415 0.5853 0.4233 0.060 Uiso 1 1 calc R . . C5A C 0.5695(5) 0.7076(4) 0.2992(5) 0.0478(11) Uani 1 1 d . . . H5A H 0.6704 0.7366 0.3265 0.057 Uiso 1 1 calc R . . C10A C 0.5636(4) 0.3540(3) 0.1469(4) 0.0305(8) Uani 1 1 d . . . C11A C 0.6394(4) 0.4396(3) 0.0917(4) 0.0324(8) Uani 1 1 d . . . C12A C 0.5259(5) 0.4743(4) -0.0087(4) 0.0385(10) Uani 1 1 d . . . H12A H 0.5413 0.5300 -0.0627 0.046 Uiso 1 1 calc R . . C13A C 0.3882(5) 0.4125(4) -0.0139(4) 0.0418(9) Uani 1 1 d . . . H13A H 0.2973 0.4195 -0.0713 0.050 Uiso 1 1 calc R . . C14A C 0.4119(4) 0.3377(4) 0.0831(4) 0.0378(9) Uani 1 1 d . . . H14A H 0.3393 0.2863 0.1016 0.045 Uiso 1 1 calc R . . C15A C 0.6365(4) 0.2893(4) 0.2560(4) 0.0352(8) Uani 1 1 d . . . H15A H 0.6787 0.3606 0.3354 0.042 Uiso 1 1 calc R . . O16A O 0.7506(3) 0.2142(2) 0.2196(3) 0.0360(6) Uani 1 1 d . . . C17A C 0.8284(5) 0.1542(4) 0.3217(4) 0.0443(10) Uani 1 1 d . . . H17A H 0.8720 0.2270 0.3995 0.053 Uiso 1 1 calc R . . C18A C 0.7205(6) 0.0632(5) 0.3521(6) 0.0611(14) Uani 1 1 d . . . H18A H 0.7699 0.0281 0.4267 0.073 Uiso 1 1 calc R . . H18B H 0.6832 -0.0139 0.2783 0.073 Uiso 1 1 calc R . . C19A C 0.5941(6) 0.1425(6) 0.3811(7) 0.0761(18) Uani 1 1 d . . . H19A H 0.5188 0.0817 0.3924 0.091 Uiso 1 1 calc R . . H19B H 0.6296 0.2121 0.4616 0.091 Uiso 1 1 calc R . . O20A O 0.5304(3) 0.2058(3) 0.2768(3) 0.0537(8) Uani 1 1 d . . . C21A C 0.9500(6) 0.0787(5) 0.2796(6) 0.0592(14) Uani 1 1 d . . . H21A H 0.9818 0.0130 0.3321 0.071 Uiso 1 1 calc R . . H21B H 0.9145 0.0293 0.1892 0.071 Uiso 1 1 calc R . . O22A O 1.0664(4) 0.1694(4) 0.2936(4) 0.0790(11) Uani 1 1 d . . . C23A C 1.1848(8) 0.1043(10) 0.2542(9) 0.123(3) Uani 1 1 d . . . H23A H 1.2061 0.0275 0.2931 0.185 Uiso 1 1 calc R . . H23B H 1.2715 0.1678 0.2815 0.185 Uiso 1 1 calc R . . H23C H 1.1579 0.0731 0.1609 0.185 Uiso 1 1 calc R . . C24A C 0.9312(5) 0.5205(5) 0.3079(4) 0.0483(10) Uani 1 1 d . . . H24A H 0.9606 0.4336 0.3242 0.072 Uiso 1 1 calc R . . H24B H 0.8636 0.5552 0.3586 0.072 Uiso 1 1 calc R . . H24C H 1.0177 0.5838 0.3319 0.072 Uiso 1 1 calc R . . C25A C 0.8513(5) 0.6668(5) 0.0905(5) 0.0540(12) Uani 1 1 d . . . H25A H 0.9538 0.7017 0.1152 0.081 Uiso 1 1 calc R . . H25B H 0.7956 0.7300 0.1361 0.081 Uiso 1 1 calc R . . H25C H 0.8113 0.6556 -0.0017 0.081 Uiso 1 1 calc R . . C26A C 0.9351(6) 0.3729(5) 0.0384(5) 0.0619(13) Uani 1 1 d . . . H26A H 0.9237 0.2855 0.0582 0.093 Uiso 1 1 calc R . . H26B H 1.0391 0.4025 0.0610 0.093 Uiso 1 1 calc R . . H26C H 0.8928 0.3652 -0.0531 0.093 Uiso 1 1 calc R . . Fe1B Fe 0.48529(5) 0.94322(4) 0.76119(4) 0.03030(13) Uani 1 1 d . . . Si1B Si 0.11765(12) 0.91638(11) 0.77905(11) 0.0359(3) Uani 1 1 d . . . C1B C 0.4018(5) 1.0491(4) 0.6255(4) 0.0413(10) Uani 1 1 d . . . H1B H 0.3036 1.0711 0.6006 0.050 Uiso 1 1 calc R . . C2B C 0.5166(5) 1.1293(4) 0.7260(5) 0.0492(11) Uani 1 1 d . . . H2B H 0.5081 1.2133 0.7795 0.059 Uiso 1 1 calc R . . C3B C 0.6460(5) 1.0595(5) 0.7309(6) 0.0567(13) Uani 1 1 d . . . H3B H 0.7391 1.0887 0.7885 0.068 Uiso 1 1 calc R . . C4B C 0.6106(5) 0.9384(5) 0.6339(5) 0.0507(12) Uani 1 1 d . . . H4B H 0.6767 0.8733 0.6154 0.061 Uiso 1 1 calc R . . C5B C 0.4598(5) 0.9307(4) 0.5693(4) 0.0443(10) Uani 1 1 d . . . H5B H 0.4075 0.8598 0.5013 0.053 Uiso 1 1 calc R . . C10B C 0.3929(4) 0.7694(3) 0.7844(4) 0.0304(8) Uani 1 1 d . . . C11B C 0.3170(4) 0.8837(3) 0.8307(4) 0.0324(8) Uani 1 1 d . . . C12B C 0.4264(5) 0.9737(4) 0.9312(4) 0.0396(10) Uani 1 1 d . . . H12B H 0.4090 1.0570 0.9804 0.048 Uiso 1 1 calc R . . C13B C 0.5649(5) 0.9173(4) 0.9448(4) 0.0441(10) Uani 1 1 d . . . H13B H 0.6544 0.9567 1.0034 0.053 Uiso 1 1 calc R . . C14B C 0.5439(4) 0.7913(4) 0.8544(4) 0.0379(9) Uani 1 1 d . . . H14B H 0.6174 0.7320 0.8426 0.045 Uiso 1 1 calc R . . C15B C 0.3212(4) 0.6456(3) 0.6840(4) 0.0310(8) Uani 1 1 d . . . H15B H 0.2808 0.6695 0.6002 0.037 Uiso 1 1 calc R . . O16B O 0.2059(3) 0.5934(2) 0.7254(2) 0.0301(5) Uani 1 1 d . . . C17B C 0.1279(4) 0.4742(3) 0.6312(4) 0.0320(8) Uani 1 1 d . . . H17B H 0.0868 0.4991 0.5480 0.038 Uiso 1 1 calc R . . C18B C 0.2359(4) 0.3675(3) 0.6126(4) 0.0360(9) Uani 1 1 d . . . H18C H 0.2706 0.3356 0.6919 0.043 Uiso 1 1 calc R . . H18D H 0.1870 0.2899 0.5430 0.043 Uiso 1 1 calc R . . C19B C 0.3648(5) 0.4273(4) 0.5793(4) 0.0443(10) Uani 1 1 d . . . H19C H 0.4398 0.3617 0.5767 0.053 Uiso 1 1 calc R . . H19D H 0.3319 0.4465 0.4936 0.053 Uiso 1 1 calc R . . O20B O 0.4278(3) 0.5499(2) 0.6726(3) 0.0388(6) Uani 1 1 d . . . C21B C 0.0029(5) 0.4294(4) 0.6783(5) 0.0448(10) Uani 1 1 d . . . H21C H -0.0279 0.3335 0.6386 0.054 Uiso 1 1 calc R . . H21D H 0.0338 0.4411 0.7722 0.054 Uiso 1 1 calc R . . O22B O -0.1152(3) 0.5102(4) 0.6439(4) 0.0655(9) Uani 1 1 d . . . C23B C -0.2314(6) 0.4887(7) 0.6936(7) 0.085(2) Uani 1 1 d . . . H23D H -0.2674 0.3939 0.6647 0.128 Uiso 1 1 calc R . . H23E H -0.3100 0.5440 0.6641 0.128 Uiso 1 1 calc R . . H23F H -0.1989 0.5132 0.7871 0.128 Uiso 1 1 calc R . . C24B C 0.0348(5) 0.8483(5) 0.6031(4) 0.0477(10) Uani 1 1 d . . . H24D H 0.0170 0.7507 0.5853 0.072 Uiso 1 1 calc R . . H24E H 0.1020 0.8708 0.5555 0.072 Uiso 1 1 calc R . . H24F H -0.0577 0.8881 0.5766 0.072 Uiso 1 1 calc R . . C25B C 0.0129(6) 0.8393(5) 0.8729(5) 0.0597(13) Uani 1 1 d . . . H25D H -0.0908 0.8540 0.8449 0.090 Uiso 1 1 calc R . . H25E H 0.0506 0.8811 0.9641 0.090 Uiso 1 1 calc R . . H25F H 0.0245 0.7428 0.8583 0.090 Uiso 1 1 calc R . . C26B C 0.1046(5) 1.1045(4) 0.8167(5) 0.0558(13) Uani 1 1 d . . . H26D H 0.0037 1.1243 0.7827 0.084 Uiso 1 1 calc R . . H26E H 0.1690 1.1465 0.7775 0.084 Uiso 1 1 calc R . . H26F H 0.1343 1.1399 0.9095 0.084 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 Fe1A 0.0339(3) 0.0278(3) 0.0327(3) 0.0082(2) 0.0092(2) 0.0024(2) Si1A 0.0335(6) 0.0459(6) 0.0342(6) 0.0145(5) 0.0117(5) 0.0016(5) C1A 0.081(4) 0.030(2) 0.056(3) 0.0113(19) 0.030(3) 0.012(2) C2A 0.055(3) 0.054(3) 0.072(4) 0.008(2) 0.018(3) 0.024(2) C3A 0.054(3) 0.057(3) 0.064(3) 0.012(2) 0.038(3) 0.008(2) C4A 0.073(3) 0.041(2) 0.037(3) 0.0024(19) 0.021(2) 0.013(2) C5A 0.055(3) 0.032(2) 0.053(3) -0.0028(18) 0.020(2) -0.0006(18) C10A 0.0327(19) 0.0227(16) 0.034(2) 0.0049(14) 0.0069(16) 0.0014(14) C11A 0.039(2) 0.0308(17) 0.0256(19) 0.0071(14) 0.0052(16) 0.0032(15) C12A 0.050(3) 0.042(2) 0.023(2) 0.0093(16) 0.0061(19) 0.0063(19) C13A 0.038(2) 0.042(2) 0.034(2) 0.0034(17) -0.0062(18) -0.0012(17) C14A 0.035(2) 0.0304(18) 0.042(2) 0.0067(16) 0.0022(18) -0.0027(15) C15A 0.038(2) 0.0293(18) 0.041(2) 0.0130(16) 0.0108(18) 0.0013(15) O16A 0.0336(14) 0.0329(13) 0.0419(16) 0.0127(11) 0.0072(12) 0.0040(10) C17A 0.038(2) 0.039(2) 0.051(3) 0.0145(18) -0.001(2) 0.0022(17) C18A 0.056(3) 0.052(3) 0.081(4) 0.044(3) 0.003(3) 0.003(2) C19A 0.068(4) 0.092(4) 0.100(5) 0.073(4) 0.036(3) 0.018(3) O20A 0.0430(17) 0.0615(18) 0.073(2) 0.0455(17) 0.0196(16) 0.0036(14) C21A 0.045(3) 0.050(3) 0.075(4) 0.015(2) 0.003(3) 0.008(2) O22A 0.051(2) 0.096(3) 0.091(3) 0.025(2) 0.017(2) 0.004(2) C23A 0.064(4) 0.195(10) 0.113(7) 0.020(6) 0.041(5) 0.017(5) C24A 0.042(2) 0.056(3) 0.041(3) 0.012(2) 0.001(2) -0.011(2) C25A 0.052(3) 0.057(3) 0.060(3) 0.030(2) 0.014(2) -0.006(2) C26A 0.056(3) 0.076(3) 0.067(4) 0.019(3) 0.037(3) 0.018(3) Fe1B 0.0297(3) 0.0257(2) 0.0379(3) 0.0093(2) 0.0116(2) 0.0014(2) Si1B 0.0333(6) 0.0327(5) 0.0459(7) 0.0079(5) 0.0190(5) 0.0016(4) C1B 0.048(2) 0.036(2) 0.049(3) 0.0196(18) 0.022(2) 0.0106(18) C2B 0.063(3) 0.0238(18) 0.068(3) 0.0152(18) 0.027(3) 0.0014(18) C3B 0.042(3) 0.056(3) 0.078(4) 0.029(3) 0.017(3) -0.013(2) C4B 0.050(3) 0.051(3) 0.067(3) 0.023(2) 0.036(3) 0.010(2) C5B 0.059(3) 0.039(2) 0.042(3) 0.0125(18) 0.024(2) 0.001(2) C10B 0.0312(19) 0.0268(16) 0.035(2) 0.0133(15) 0.0072(16) -0.0015(14) C11B 0.040(2) 0.0279(17) 0.032(2) 0.0077(15) 0.0132(17) -0.0026(15) C12B 0.050(3) 0.035(2) 0.032(2) 0.0052(16) 0.010(2) -0.0048(18) C13B 0.044(2) 0.043(2) 0.038(2) 0.0126(18) -0.0046(19) -0.0075(18) C14B 0.034(2) 0.0343(19) 0.045(2) 0.0163(17) 0.0046(18) 0.0023(16) C15B 0.0303(19) 0.0291(17) 0.037(2) 0.0121(15) 0.0097(16) 0.0062(14) O16B 0.0253(12) 0.0269(11) 0.0362(14) 0.0056(10) 0.0065(11) -0.0012(9) C17B 0.0285(18) 0.0286(17) 0.037(2) 0.0106(15) 0.0025(16) 0.0012(14) C18B 0.042(2) 0.0249(17) 0.040(2) 0.0058(15) 0.0093(18) 0.0028(15) C19B 0.049(3) 0.033(2) 0.050(3) 0.0011(18) 0.020(2) 0.0026(18) O20B 0.0311(14) 0.0288(12) 0.0568(18) 0.0053(12) 0.0163(13) 0.0032(11) C21B 0.032(2) 0.044(2) 0.054(3) 0.009(2) 0.005(2) -0.0026(17) O22B 0.0374(18) 0.077(2) 0.083(3) 0.023(2) 0.0137(18) 0.0120(16) C23B 0.031(3) 0.112(5) 0.102(5) -0.003(4) 0.021(3) 0.003(3) C24B 0.045(3) 0.050(2) 0.048(3) 0.015(2) 0.009(2) 0.0089(19) C25B 0.056(3) 0.059(3) 0.076(4) 0.016(3) 0.039(3) 0.001(2) C26B 0.053(3) 0.033(2) 0.090(4) 0.010(2) 0.038(3) 0.0116(19) _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 Fe1A C5A 2.030(4) . ? Fe1A C10A 2.035(3) . ? Fe1A C12A 2.031(4) . ? Fe1A C1A 2.037(4) . ? Fe1A C14A 2.038(4) . ? Fe1A C3A 2.040(4) . ? Fe1A C4A 2.040(4) . ? Fe1A C2A 2.038(4) . ? Fe1A C13A 2.039(4) . ? Fe1A C11A 2.063(4) . ? Si1A C11A 1.864(4) . ? Si1A C24A 1.866(5) . ? Si1A C26A 1.869(4) . ? Si1A C25A 1.870(4) . ? C1A C2A 1.400(7) . ? C1A C5A 1.407(7) . ? C2A C3A 1.412(7) . ? C3A C4A 1.419(7) . ? C4A C5A 1.401(6) . ? C10A C14A 1.410(5) . ? C10A C11A 1.437(5) . ? C10A C15A 1.515(5) . ? C11A C12A 1.441(5) . ? C12A C13A 1.411(6) . ? C13A C14A 1.419(6) . ? C15A O20A 1.392(5) . ? C15A O16A 1.416(4) . ? O16A C17A 1.440(5) . ? C17A C21A 1.501(6) . ? C17A C18A 1.506(6) . ? C18A C19A 1.509(7) . ? C19A O20A 1.444(6) . ? C21A O22A 1.373(6) . ? O22A C23A 1.418(8) . ? Fe1B C3B 2.038(4) . ? Fe1B C1B 2.038(4) . ? Fe1B C5B 2.041(4) . ? Fe1B C2B 2.041(4) . ? Fe1B C4B 2.041(4) . ? Fe1B C14B 2.045(4) . ? Fe1B C12B 2.046(4) . ? Fe1B C10B 2.047(3) . ? Fe1B C13B 2.049(4) . ? Fe1B C11B 2.059(4) . ? Si1B C24B 1.862(5) . ? Si1B C25B 1.870(5) . ? Si1B C26B 1.875(4) . ? Si1B C11B 1.875(4) . ? C1B C5B 1.411(6) . ? C1B C2B 1.421(6) . ? C2B C3B 1.415(6) . ? C3B C4B 1.410(7) . ? C4B C5B 1.408(7) . ? C10B C14B 1.421(5) . ? C10B C11B 1.438(5) . ? C10B C15B 1.494(5) . ? C11B C12B 1.435(6) . ? C12B C13B 1.418(6) . ? C13B C14B 1.412(6) . ? C15B O16B 1.414(4) . ? C15B O20B 1.418(4) . ? O16B C17B 1.452(4) . ? C17B C21B 1.500(6) . ? C17B C18B 1.514(5) . ? C18B C19B 1.506(6) . ? C19B O20B 1.433(5) . ? C21B O22B 1.417(5) . ? O22B C23B 1.375(6) . ? 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 C5A Fe1A C10A 124.82(17) . . ? C5A Fe1A C12A 125.09(18) . . ? C10A Fe1A C12A 68.17(15) . . ? C5A Fe1A C1A 40.49(19) . . ? C10A Fe1A C1A 160.43(18) . . ? C12A Fe1A C1A 108.03(18) . . ? C5A Fe1A C14A 159.25(17) . . ? C10A Fe1A C14A 40.50(15) . . ? C12A Fe1A C14A 68.25(17) . . ? C1A Fe1A C14A 157.77(19) . . ? C5A Fe1A C3A 68.0(2) . . ? C10A Fe1A C3A 123.56(18) . . ? C12A Fe1A C3A 156.2(2) . . ? C1A Fe1A C3A 67.8(2) . . ? C14A Fe1A C3A 106.24(19) . . ? C5A Fe1A C4A 40.28(18) . . ? C10A Fe1A C4A 109.20(17) . . ? C12A Fe1A C4A 161.58(19) . . ? C1A Fe1A C4A 67.96(19) . . ? C14A Fe1A C4A 122.46(18) . . ? C3A Fe1A C4A 40.7(2) . . ? C5A Fe1A C2A 67.9(2) . . ? C10A Fe1A C2A 158.56(18) . . ? C12A Fe1A C2A 121.15(19) . . ? C1A Fe1A C2A 40.2(2) . . ? C14A Fe1A C2A 121.49(19) . . ? C3A Fe1A C2A 40.5(2) . . ? C4A Fe1A C2A 68.2(2) . . ? C5A Fe1A C13A 159.62(17) . . ? C10A Fe1A C13A 68.32(15) . . ? C12A Fe1A C13A 40.56(18) . . ? C1A Fe1A C13A 122.15(18) . . ? C14A Fe1A C13A 40.73(16) . . ? C3A Fe1A C13A 120.2(2) . . ? C4A Fe1A C13A 157.08(19) . . ? C2A Fe1A C13A 105.3(2) . . ? C5A Fe1A C11A 109.22(17) . . ? C10A Fe1A C11A 41.04(14) . . ? C12A Fe1A C11A 41.20(15) . . ? C1A Fe1A C11A 123.39(17) . . ? C14A Fe1A C11A 69.23(15) . . ? C3A Fe1A C11A 160.62(18) . . ? C4A Fe1A C11A 124.74(17) . . ? C2A Fe1A C11A 157.97(18) . . ? C13A Fe1A C11A 69.38(16) . . ? C11A Si1A C24A 112.48(19) . . ? C11A Si1A C26A 109.1(2) . . ? C24A Si1A C26A 108.2(2) . . ? C11A Si1A C25A 108.20(19) . . ? C24A Si1A C25A 108.6(2) . . ? C26A Si1A C25A 110.2(2) . . ? C2A C1A C5A 108.2(4) . . ? C2A C1A Fe1A 70.0(2) . . ? C5A C1A Fe1A 69.5(2) . . ? C1A C2A C3A 108.0(5) . . ? C1A C2A Fe1A 69.9(2) . . ? C3A C2A Fe1A 69.8(3) . . ? C2A C3A C4A 107.8(4) . . ? C2A C3A Fe1A 69.7(3) . . ? C4A C3A Fe1A 69.6(2) . . ? C5A C4A C3A 107.6(4) . . ? C5A C4A Fe1A 69.5(2) . . ? C3A C4A Fe1A 69.7(3) . . ? C4A C5A C1A 108.4(4) . . ? C4A C5A Fe1A 70.2(2) . . ? C1A C5A Fe1A 70.0(3) . . ? C14A C10A C11A 109.8(3) . . ? C14A C10A C15A 125.2(3) . . ? C11A C10A C15A 124.9(3) . . ? C14A C10A Fe1A 69.9(2) . . ? C11A C10A Fe1A 70.51(19) . . ? C15A C10A Fe1A 126.9(3) . . ? C10A C11A C12A 104.7(3) . . ? C10A C11A Si1A 130.7(3) . . ? C12A C11A Si1A 124.6(3) . . ? C10A C11A Fe1A 68.4(2) . . ? C12A C11A Fe1A 68.2(2) . . ? Si1A C11A Fe1A 126.97(19) . . ? C13A C12A C11A 109.9(4) . . ? C13A C12A Fe1A 70.0(2) . . ? C11A C12A Fe1A 70.6(2) . . ? C12A C13A C14A 107.6(3) . . ? C12A C13A Fe1A 69.4(2) . . ? C14A C13A Fe1A 69.6(2) . . ? C10A C14A C13A 107.9(3) . . ? C10A C14A Fe1A 69.6(2) . . ? C13A C14A Fe1A 69.7(2) . . ? O20A C15A O16A 111.3(3) . . ? O20A C15A C10A 108.5(3) . . ? O16A C15A C10A 108.0(3) . . ? C15A O16A C17A 110.8(3) . . ? O16A C17A C21A 108.7(4) . . ? O16A C17A C18A 108.8(3) . . ? C21A C17A C18A 112.3(4) . . ? C17A C18A C19A 109.4(4) . . ? O20A C19A C18A 110.0(4) . . ? C15A O20A C19A 110.7(4) . . ? O22A C21A C17A 109.1(4) . . ? C21A O22A C23A 111.9(5) . . ? C3B Fe1B C1B 68.19(19) . . ? C3B Fe1B C5B 68.4(2) . . ? C1B Fe1B C5B 40.47(16) . . ? C3B Fe1B C2B 40.59(18) . . ? C1B Fe1B C2B 40.77(18) . . ? C5B Fe1B C2B 68.55(19) . . ? C3B Fe1B C4B 40.4(2) . . ? C1B Fe1B C4B 67.70(18) . . ? C5B Fe1B C4B 40.4(2) . . ? C2B Fe1B C4B 68.05(18) . . ? C3B Fe1B C14B 119.11(18) . . ? C1B Fe1B C14B 163.69(16) . . ? C5B Fe1B C14B 125.92(17) . . ? C2B Fe1B C14B 153.73(19) . . ? C4B Fe1B C14B 107.56(18) . . ? C3B Fe1B C12B 123.9(2) . . ? C1B Fe1B C12B 121.82(17) . . ? C5B Fe1B C12B 157.28(18) . . ? C2B Fe1B C12B 107.23(18) . . ? C4B Fe1B C12B 160.7(2) . . ? C14B Fe1B C12B 67.88(17) . . ? C3B Fe1B C10B 155.04(17) . . ? C1B Fe1B C10B 127.27(17) . . ? C5B Fe1B C10B 109.36(16) . . ? C2B Fe1B C10B 163.73(16) . . ? C4B Fe1B C10B 121.56(17) . . ? C14B Fe1B C10B 40.64(15) . . ? C12B Fe1B C10B 68.09(15) . . ? C3B Fe1B C13B 105.6(2) . . ? C1B Fe1B C13B 155.36(16) . . ? C5B Fe1B C13B 161.46(17) . . ? C2B Fe1B C13B 119.03(19) . . ? C4B Fe1B C13B 123.92(19) . . ? C14B Fe1B C13B 40.36(17) . . ? C12B Fe1B C13B 40.52(17) . . ? C10B Fe1B C13B 68.29(16) . . ? C3B Fe1B C11B 161.59(18) . . ? C1B Fe1B C11B 108.88(16) . . ? C5B Fe1B C11B 122.06(17) . . ? C2B Fe1B C11B 125.32(16) . . ? C4B Fe1B C11B 156.93(18) . . ? C14B Fe1B C11B 68.97(15) . . ? C12B Fe1B C11B 40.94(16) . . ? C10B Fe1B C11B 41.00(14) . . ? C13B Fe1B C11B 69.10(17) . . ? C24B Si1B C25B 109.8(2) . . ? C24B Si1B C26B 108.3(2) . . ? C25B Si1B C26B 109.0(2) . . ? C24B Si1B C11B 112.53(18) . . ? C25B Si1B C11B 109.2(2) . . ? C26B Si1B C11B 107.95(19) . . ? C5B C1B C2B 108.6(4) . . ? C5B C1B Fe1B 69.9(2) . . ? C2B C1B Fe1B 69.7(2) . . ? C3B C2B C1B 107.3(4) . . ? C3B C2B Fe1B 69.6(2) . . ? C1B C2B Fe1B 69.5(2) . . ? C4B C3B C2B 107.9(4) . . ? C4B C3B Fe1B 69.9(2) . . ? C2B C3B Fe1B 69.8(2) . . ? C5B C4B C3B 108.8(4) . . ? C5B C4B Fe1B 69.8(2) . . ? C3B C4B Fe1B 69.7(3) . . ? C4B C5B C1B 107.4(4) . . ? C4B C5B Fe1B 69.8(3) . . ? C1B C5B Fe1B 69.6(2) . . ? C14B C10B C11B 108.7(3) . . ? C14B C10B C15B 126.3(3) . . ? C11B C10B C15B 124.9(3) . . ? C14B C10B Fe1B 69.6(2) . . ? C11B C10B Fe1B 69.94(19) . . ? C15B C10B Fe1B 128.8(3) . . ? C12B C11B C10B 105.8(3) . . ? C12B C11B Si1B 124.5(3) . . ? C10B C11B Si1B 129.8(3) . . ? C12B C11B Fe1B 69.1(2) . . ? C10B C11B Fe1B 69.1(2) . . ? Si1B C11B Fe1B 127.01(19) . . ? C13B C12B C11B 109.5(4) . . ? C13B C12B Fe1B 69.9(3) . . ? C11B C12B Fe1B 70.0(2) . . ? C14B C13B C12B 107.6(4) . . ? C14B C13B Fe1B 69.7(2) . . ? C12B C13B Fe1B 69.6(2) . . ? C13B C14B C10B 108.5(3) . . ? C13B C14B Fe1B 70.0(2) . . ? C10B C14B Fe1B 69.8(2) . . ? O16B C15B O20B 110.6(3) . . ? O16B C15B C10B 107.4(3) . . ? O20B C15B C10B 108.8(3) . . ? C15B O16B C17B 110.9(3) . . ? O16B C17B C21B 107.7(3) . . ? O16B C17B C18B 108.9(3) . . ? C21B C17B C18B 113.7(3) . . ? C19B C18B C17B 109.4(3) . . ? O20B C19B C18B 110.8(3) . . ? C15B O20B C19B 111.5(3) . . ? O22B C21B C17B 107.7(4) . . ? C23B O22B C21B 113.3(4) . . ? 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 C5A Fe1A C1A C2A -119.4(4) . . . . ? C10A Fe1A C1A C2A -167.4(5) . . . . ? C12A Fe1A C1A C2A 117.2(3) . . . . ? C14A Fe1A C1A C2A 40.8(6) . . . . ? C3A Fe1A C1A C2A -37.8(3) . . . . ? C4A Fe1A C1A C2A -81.9(3) . . . . ? C13A Fe1A C1A C2A 74.9(4) . . . . ? C11A Fe1A C1A C2A 160.1(3) . . . . ? C10A Fe1A C1A C5A -48.0(6) . . . . ? C12A Fe1A C1A C5A -123.4(3) . . . . ? C14A Fe1A C1A C5A 160.2(4) . . . . ? C3A Fe1A C1A C5A 81.6(3) . . . . ? C4A Fe1A C1A C5A 37.5(3) . . . . ? C2A Fe1A C1A C5A 119.4(4) . . . . ? C13A Fe1A C1A C5A -165.7(3) . . . . ? C11A Fe1A C1A C5A -80.5(3) . . . . ? C5A C1A C2A C3A 0.4(5) . . . . ? Fe1A C1A C2A C3A 59.6(3) . . . . ? C5A C1A C2A Fe1A -59.2(3) . . . . ? C5A Fe1A C2A C1A 37.6(3) . . . . ? C10A Fe1A C2A C1A 168.4(4) . . . . ? C12A Fe1A C2A C1A -81.1(4) . . . . ? C14A Fe1A C2A C1A -163.2(3) . . . . ? C3A Fe1A C2A C1A 119.1(5) . . . . ? C4A Fe1A C2A C1A 81.2(3) . . . . ? C13A Fe1A C2A C1A -122.0(3) . . . . ? C11A Fe1A C2A C1A -49.3(7) . . . . ? C5A Fe1A C2A C3A -81.5(3) . . . . ? C10A Fe1A C2A C3A 49.3(7) . . . . ? C12A Fe1A C2A C3A 159.9(3) . . . . ? C1A Fe1A C2A C3A -119.1(5) . . . . ? C14A Fe1A C2A C3A 77.8(4) . . . . ? C4A Fe1A C2A C3A -37.9(3) . . . . ? C13A Fe1A C2A C3A 118.9(3) . . . . ? C11A Fe1A C2A C3A -168.3(4) . . . . ? C1A C2A C3A C4A -0.2(5) . . . . ? Fe1A C2A C3A C4A 59.4(3) . . . . ? C1A C2A C3A Fe1A -59.6(3) . . . . ? C5A Fe1A C3A C2A 81.4(3) . . . . ? C10A Fe1A C3A C2A -160.6(3) . . . . ? C12A Fe1A C3A C2A -47.0(6) . . . . ? C1A Fe1A C3A C2A 37.5(3) . . . . ? C14A Fe1A C3A C2A -119.8(3) . . . . ? C4A Fe1A C3A C2A 119.0(4) . . . . ? C13A Fe1A C3A C2A -77.8(4) . . . . ? C11A Fe1A C3A C2A 166.8(5) . . . . ? C5A Fe1A C3A C4A -37.6(3) . . . . ? C10A Fe1A C3A C4A 80.5(3) . . . . ? C12A Fe1A C3A C4A -166.0(4) . . . . ? C1A Fe1A C3A C4A -81.5(3) . . . . ? C14A Fe1A C3A C4A 121.2(3) . . . . ? C2A Fe1A C3A C4A -119.0(4) . . . . ? C13A Fe1A C3A C4A 163.2(2) . . . . ? C11A Fe1A C3A C4A 47.8(7) . . . . ? C2A C3A C4A C5A -0.1(5) . . . . ? Fe1A C3A C4A C5A 59.4(3) . . . . ? C2A C3A C4A Fe1A -59.4(3) . . . . ? C10A Fe1A C4A C5A 121.6(3) . . . . ? C12A Fe1A C4A C5A 43.2(7) . . . . ? C1A Fe1A C4A C5A -37.7(3) . . . . ? C14A Fe1A C4A C5A 164.5(3) . . . . ? C3A Fe1A C4A C5A -118.9(4) . . . . ? C2A Fe1A C4A C5A -81.1(3) . . . . ? C13A Fe1A C4A C5A -158.8(4) . . . . ? C11A Fe1A C4A C5A 78.5(3) . . . . ? C5A Fe1A C4A C3A 118.9(4) . . . . ? C10A Fe1A C4A C3A -119.5(3) . . . . ? C12A Fe1A C4A C3A 162.0(5) . . . . ? C1A Fe1A C4A C3A 81.2(3) . . . . ? C14A Fe1A C4A C3A -76.6(3) . . . . ? C2A Fe1A C4A C3A 37.7(3) . . . . ? C13A Fe1A C4A C3A -39.9(6) . . . . ? C11A Fe1A C4A C3A -162.6(3) . . . . ? C3A C4A C5A C1A 0.3(5) . . . . ? Fe1A C4A C5A C1A 59.8(3) . . . . ? C3A C4A C5A Fe1A -59.5(3) . . . . ? C2A C1A C5A C4A -0.5(5) . . . . ? Fe1A C1A C5A C4A -59.9(3) . . . . ? C2A C1A C5A Fe1A 59.5(3) . . . . ? C10A Fe1A C5A C4A -78.4(3) . . . . ? C12A Fe1A C5A C4A -164.7(3) . . . . ? C1A Fe1A C5A C4A 119.2(4) . . . . ? C14A Fe1A C5A C4A -39.5(6) . . . . ? C3A Fe1A C5A C4A 38.0(3) . . . . ? C2A Fe1A C5A C4A 81.9(3) . . . . ? C13A Fe1A C5A C4A 156.2(5) . . . . ? C11A Fe1A C5A C4A -121.5(3) . . . . ? C10A Fe1A C5A C1A 162.4(3) . . . . ? C12A Fe1A C5A C1A 76.1(3) . . . . ? C14A Fe1A C5A C1A -158.8(4) . . . . ? C3A Fe1A C5A C1A -81.2(3) . . . . ? C4A Fe1A C5A C1A -119.2(4) . . . . ? C2A Fe1A C5A C1A -37.3(3) . . . . ? C13A Fe1A C5A C1A 36.9(6) . . . . ? C11A Fe1A C5A C1A 119.3(3) . . . . ? C5A Fe1A C10A C14A 160.0(3) . . . . ? C12A Fe1A C10A C14A -81.6(3) . . . . ? C1A Fe1A C10A C14A -164.1(5) . . . . ? C3A Fe1A C10A C14A 74.9(3) . . . . ? C4A Fe1A C10A C14A 117.9(3) . . . . ? C2A Fe1A C10A C14A 38.7(6) . . . . ? C13A Fe1A C10A C14A -37.8(2) . . . . ? C11A Fe1A C10A C14A -120.9(3) . . . . ? C5A Fe1A C10A C11A -79.1(3) . . . . ? C12A Fe1A C10A C11A 39.3(2) . . . . ? C1A Fe1A C10A C11A -43.2(6) . . . . ? C14A Fe1A C10A C11A 120.9(3) . . . . ? C3A Fe1A C10A C11A -164.2(3) . . . . ? C4A Fe1A C10A C11A -121.3(2) . . . . ? C2A Fe1A C10A C11A 159.6(5) . . . . ? C13A Fe1A C10A C11A 83.1(2) . . . . ? C5A Fe1A C10A C15A 40.5(4) . . . . ? C12A Fe1A C10A C15A 158.9(4) . . . . ? C1A Fe1A C10A C15A 76.4(6) . . . . ? C14A Fe1A C10A C15A -119.5(4) . . . . ? C3A Fe1A C10A C15A -44.6(4) . . . . ? C4A Fe1A C10A C15A -1.7(4) . . . . ? C2A Fe1A C10A C15A -80.8(6) . . . . ? C13A Fe1A C10A C15A -157.3(4) . . . . ? C11A Fe1A C10A C15A 119.6(4) . . . . ? C14A C10A C11A C12A 0.0(4) . . . . ? C15A C10A C11A C12A 179.2(3) . . . . ? Fe1A C10A C11A C12A -58.9(2) . . . . ? C14A C10A C11A Si1A 179.8(3) . . . . ? C15A C10A C11A Si1A -1.1(5) . . . . ? Fe1A C10A C11A Si1A 120.9(3) . . . . ? C14A C10A C11A Fe1A 58.9(3) . . . . ? C15A C10A C11A Fe1A -121.9(3) . . . . ? C24A Si1A C11A C10A -31.5(4) . . . . ? C26A Si1A C11A C10A 88.6(4) . . . . ? C25A Si1A C11A C10A -151.5(3) . . . . ? C24A Si1A C11A C12A 148.3(3) . . . . ? C26A Si1A C11A C12A -91.7(4) . . . . ? C25A Si1A C11A C12A 28.3(4) . . . . ? C24A Si1A C11A Fe1A 60.8(3) . . . . ? C26A Si1A C11A Fe1A -179.1(2) . . . . ? C25A Si1A C11A Fe1A -59.2(3) . . . . ? C5A Fe1A C11A C10A 121.4(2) . . . . ? C12A Fe1A C11A C10A -116.9(3) . . . . ? C1A Fe1A C11A C10A 164.1(2) . . . . ? C14A Fe1A C11A C10A -36.6(2) . . . . ? C3A Fe1A C11A C10A 43.2(6) . . . . ? C4A Fe1A C11A C10A 79.2(3) . . . . ? C2A Fe1A C11A C10A -160.1(5) . . . . ? C13A Fe1A C11A C10A -80.3(2) . . . . ? C5A Fe1A C11A C12A -121.7(3) . . . . ? C10A Fe1A C11A C12A 116.9(3) . . . . ? C1A Fe1A C11A C12A -79.0(3) . . . . ? C14A Fe1A C11A C12A 80.3(3) . . . . ? C3A Fe1A C11A C12A 160.1(5) . . . . ? C4A Fe1A C11A C12A -163.9(3) . . . . ? C2A Fe1A C11A C12A -43.2(6) . . . . ? C13A Fe1A C11A C12A 36.6(2) . . . . ? C5A Fe1A C11A Si1A -4.1(3) . . . . ? C10A Fe1A C11A Si1A -125.4(3) . . . . ? C12A Fe1A C11A Si1A 117.7(3) . . . . ? C1A Fe1A C11A Si1A 38.6(3) . . . . ? C14A Fe1A C11A Si1A -162.0(3) . . . . ? C3A Fe1A C11A Si1A -82.2(6) . . . . ? C4A Fe1A C11A Si1A -46.2(3) . . . . ? C2A Fe1A C11A Si1A 74.5(6) . . . . ? C13A Fe1A C11A Si1A 154.3(3) . . . . ? C10A C11A C12A C13A -0.1(4) . . . . ? Si1A C11A C12A C13A -179.9(3) . . . . ? Fe1A C11A C12A C13A -59.1(3) . . . . ? C10A C11A C12A Fe1A 59.1(2) . . . . ? Si1A C11A C12A Fe1A -120.7(3) . . . . ? C5A Fe1A C12A C13A -160.2(2) . . . . ? C10A Fe1A C12A C13A 81.7(2) . . . . ? C1A Fe1A C12A C13A -118.7(3) . . . . ? C14A Fe1A C12A C13A 37.9(2) . . . . ? C3A Fe1A C12A C13A -42.9(6) . . . . ? C4A Fe1A C12A C13A 167.0(5) . . . . ? C2A Fe1A C12A C13A -76.6(3) . . . . ? C11A Fe1A C12A C13A 120.8(3) . . . . ? C5A Fe1A C12A C11A 78.9(3) . . . . ? C10A Fe1A C12A C11A -39.1(2) . . . . ? C1A Fe1A C12A C11A 120.5(3) . . . . ? C14A Fe1A C12A C11A -82.9(2) . . . . ? C3A Fe1A C12A C11A -163.7(4) . . . . ? C4A Fe1A C12A C11A 46.2(6) . . . . ? C2A Fe1A C12A C11A 162.5(3) . . . . ? C13A Fe1A C12A C11A -120.8(3) . . . . ? C11A C12A C13A C14A 0.1(5) . . . . ? Fe1A C12A C13A C14A -59.4(3) . . . . ? C11A C12A C13A Fe1A 59.5(3) . . . . ? C5A Fe1A C13A C12A 52.6(6) . . . . ? C10A Fe1A C13A C12A -81.3(2) . . . . ? C1A Fe1A C13A C12A 80.1(3) . . . . ? C14A Fe1A C13A C12A -118.9(3) . . . . ? C3A Fe1A C13A C12A 161.5(3) . . . . ? C4A Fe1A C13A C12A -169.5(4) . . . . ? C2A Fe1A C13A C12A 120.3(3) . . . . ? C11A Fe1A C13A C12A -37.2(2) . . . . ? C5A Fe1A C13A C14A 171.6(4) . . . . ? C10A Fe1A C13A C14A 37.6(2) . . . . ? C12A Fe1A C13A C14A 118.9(3) . . . . ? C1A Fe1A C13A C14A -161.0(3) . . . . ? C3A Fe1A C13A C14A -79.6(3) . . . . ? C4A Fe1A C13A C14A -50.6(5) . . . . ? C2A Fe1A C13A C14A -120.8(3) . . . . ? C11A Fe1A C13A C14A 81.7(2) . . . . ? C11A C10A C14A C13A 0.0(4) . . . . ? C15A C10A C14A C13A -179.1(3) . . . . ? Fe1A C10A C14A C13A 59.4(3) . . . . ? C11A C10A C14A Fe1A -59.3(2) . . . . ? C15A C10A C14A Fe1A 121.5(4) . . . . ? C12A C13A C14A C10A -0.1(4) . . . . ? Fe1A C13A C14A C10A -59.3(3) . . . . ? C12A C13A C14A Fe1A 59.3(3) . . . . ? C5A Fe1A C14A C10A -52.5(6) . . . . ? C12A Fe1A C14A C10A 81.4(2) . . . . ? C1A Fe1A C14A C10A 165.9(4) . . . . ? C3A Fe1A C14A C10A -123.1(3) . . . . ? C4A Fe1A C14A C10A -81.7(3) . . . . ? C2A Fe1A C14A C10A -164.5(3) . . . . ? C13A Fe1A C14A C10A 119.2(3) . . . . ? C11A Fe1A C14A C10A 37.1(2) . . . . ? C5A Fe1A C14A C13A -171.7(4) . . . . ? C10A Fe1A C14A C13A -119.2(3) . . . . ? C12A Fe1A C14A C13A -37.8(2) . . . . ? C1A Fe1A C14A C13A 46.7(6) . . . . ? C3A Fe1A C14A C13A 117.7(3) . . . . ? C4A Fe1A C14A C13A 159.1(3) . . . . ? C2A Fe1A C14A C13A 76.3(3) . . . . ? C11A Fe1A C14A C13A -82.1(3) . . . . ? C14A C10A C15A O20A 3.4(5) . . . . ? C11A C10A C15A O20A -175.6(3) . . . . ? Fe1A C10A C15A O20A 93.5(4) . . . . ? C14A C10A C15A O16A 124.1(4) . . . . ? C11A C10A C15A O16A -54.9(4) . . . . ? Fe1A C10A C15A O16A -145.8(3) . . . . ? O20A C15A O16A C17A -63.3(4) . . . . ? C10A C15A O16A C17A 177.7(3) . . . . ? C15A O16A C17A C21A -178.7(3) . . . . ? C15A O16A C17A C18A 58.8(4) . . . . ? O16A C17A C18A C19A -54.3(6) . . . . ? C21A C17A C18A C19A -174.6(5) . . . . ? C17A C18A C19A O20A 53.7(6) . . . . ? O16A C15A O20A C19A 61.9(5) . . . . ? C10A C15A O20A C19A -179.4(4) . . . . ? C18A C19A O20A C15A -57.3(6) . . . . ? O16A C17A C21A O22A 78.8(5) . . . . ? C18A C17A C21A O22A -160.8(4) . . . . ? C17A C21A O22A C23A -179.5(6) . . . . ? C3B Fe1B C1B C5B 81.8(3) . . . . ? C2B Fe1B C1B C5B 119.8(4) . . . . ? C4B Fe1B C1B C5B 38.0(3) . . . . ? C14B Fe1B C1B C5B -38.1(7) . . . . ? C12B Fe1B C1B C5B -161.0(3) . . . . ? C10B Fe1B C1B C5B -75.5(3) . . . . ? C13B Fe1B C1B C5B 161.5(4) . . . . ? C11B Fe1B C1B C5B -117.6(3) . . . . ? C3B Fe1B C1B C2B -38.0(3) . . . . ? C5B Fe1B C1B C2B -119.8(4) . . . . ? C4B Fe1B C1B C2B -81.8(3) . . . . ? C14B Fe1B C1B C2B -157.9(5) . . . . ? C12B Fe1B C1B C2B 79.3(3) . . . . ? C10B Fe1B C1B C2B 164.7(2) . . . . ? C13B Fe1B C1B C2B 41.8(5) . . . . ? C11B Fe1B C1B C2B 122.6(2) . . . . ? C5B C1B C2B C3B 0.2(5) . . . . ? Fe1B C1B C2B C3B 59.5(3) . . . . ? C5B C1B C2B Fe1B -59.3(3) . . . . ? C1B Fe1B C2B C3B -118.6(4) . . . . ? C5B Fe1B C2B C3B -81.3(3) . . . . ? C4B Fe1B C2B C3B -37.8(3) . . . . ? C14B Fe1B C2B C3B 47.5(5) . . . . ? C12B Fe1B C2B C3B 122.3(3) . . . . ? C10B Fe1B C2B C3B -167.1(6) . . . . ? C13B Fe1B C2B C3B 79.9(3) . . . . ? C11B Fe1B C2B C3B 163.8(3) . . . . ? C3B Fe1B C2B C1B 118.6(4) . . . . ? C5B Fe1B C2B C1B 37.3(2) . . . . ? C4B Fe1B C2B C1B 80.9(3) . . . . ? C14B Fe1B C2B C1B 166.2(3) . . . . ? C12B Fe1B C2B C1B -119.1(3) . . . . ? C10B Fe1B C2B C1B -48.4(7) . . . . ? C13B Fe1B C2B C1B -161.5(2) . . . . ? C11B Fe1B C2B C1B -77.6(3) . . . . ? C1B C2B C3B C4B 0.3(5) . . . . ? Fe1B C2B C3B C4B 59.8(3) . . . . ? C1B C2B C3B Fe1B -59.5(3) . . . . ? C1B Fe1B C3B C4B -80.8(3) . . . . ? C5B Fe1B C3B C4B -37.0(3) . . . . ? C2B Fe1B C3B C4B -118.9(4) . . . . ? C14B Fe1B C3B C4B 83.0(3) . . . . ? C12B Fe1B C3B C4B 164.7(3) . . . . ? C10B Fe1B C3B C4B 52.5(6) . . . . ? C13B Fe1B C3B C4B 124.4(3) . . . . ? C11B Fe1B C3B C4B -165.1(5) . . . . ? C1B Fe1B C3B C2B 38.1(3) . . . . ? C5B Fe1B C3B C2B 81.9(3) . . . . ? C4B Fe1B C3B C2B 118.9(4) . . . . ? C14B Fe1B C3B C2B -158.1(3) . . . . ? C12B Fe1B C3B C2B -76.4(4) . . . . ? C10B Fe1B C3B C2B 171.4(4) . . . . ? C13B Fe1B C3B C2B -116.7(3) . . . . ? C11B Fe1B C3B C2B -46.2(7) . . . . ? C2B C3B C4B C5B -0.7(5) . . . . ? Fe1B C3B C4B C5B 59.0(3) . . . . ? C2B C3B C4B Fe1B -59.7(3) . . . . ? C3B Fe1B C4B C5B -120.2(4) . . . . ? C1B Fe1B C4B C5B -38.1(3) . . . . ? C2B Fe1B C4B C5B -82.3(3) . . . . ? C14B Fe1B C4B C5B 125.3(3) . . . . ? C12B Fe1B C4B C5B -161.6(5) . . . . ? C10B Fe1B C4B C5B 83.0(3) . . . . ? C13B Fe1B C4B C5B 166.7(2) . . . . ? C11B Fe1B C4B C5B 47.9(5) . . . . ? C1B Fe1B C4B C3B 82.1(3) . . . . ? C5B Fe1B C4B C3B 120.2(4) . . . . ? C2B Fe1B C4B C3B 37.9(3) . . . . ? C14B Fe1B C4B C3B -114.5(3) . . . . ? C12B Fe1B C4B C3B -41.5(7) . . . . ? C10B Fe1B C4B C3B -156.8(3) . . . . ? C13B Fe1B C4B C3B -73.2(3) . . . . ? C11B Fe1B C4B C3B 168.0(4) . . . . ? C3B C4B C5B C1B 0.8(5) . . . . ? Fe1B C4B C5B C1B 59.7(3) . . . . ? C3B C4B C5B Fe1B -58.9(3) . . . . ? C2B C1B C5B C4B -0.6(5) . . . . ? Fe1B C1B C5B C4B -59.9(3) . . . . ? C2B C1B C5B Fe1B 59.2(3) . . . . ? C3B Fe1B C5B C4B 37.1(3) . . . . ? C1B Fe1B C5B C4B 118.4(4) . . . . ? C2B Fe1B C5B C4B 80.9(3) . . . . ? C14B Fe1B C5B C4B -73.9(3) . . . . ? C12B Fe1B C5B C4B 164.3(4) . . . . ? C10B Fe1B C5B C4B -116.3(3) . . . . ? C13B Fe1B C5B C4B -37.0(7) . . . . ? C11B Fe1B C5B C4B -159.9(2) . . . . ? C3B Fe1B C5B C1B -81.3(3) . . . . ? C2B Fe1B C5B C1B -37.5(3) . . . . ? C4B Fe1B C5B C1B -118.4(4) . . . . ? C14B Fe1B C5B C1B 167.6(2) . . . . ? C12B Fe1B C5B C1B 45.9(5) . . . . ? C10B Fe1B C5B C1B 125.2(3) . . . . ? C13B Fe1B C5B C1B -155.4(5) . . . . ? C11B Fe1B C5B C1B 81.6(3) . . . . ? C3B Fe1B C10B C14B 42.9(5) . . . . ? C1B Fe1B C10B C14B 164.8(2) . . . . ? C5B Fe1B C10B C14B 123.0(3) . . . . ? C2B Fe1B C10B C14B -157.3(6) . . . . ? C4B Fe1B C10B C14B 80.1(3) . . . . ? C12B Fe1B C10B C14B -81.1(3) . . . . ? C13B Fe1B C10B C14B -37.3(2) . . . . ? C11B Fe1B C10B C14B -120.0(3) . . . . ? C3B Fe1B C10B C11B 162.9(4) . . . . ? C1B Fe1B C10B C11B -75.2(3) . . . . ? C5B Fe1B C10B C11B -117.0(2) . . . . ? C2B Fe1B C10B C11B -37.3(7) . . . . ? C4B Fe1B C10B C11B -159.9(2) . . . . ? C14B Fe1B C10B C11B 120.0(3) . . . . ? C12B Fe1B C10B C11B 38.9(2) . . . . ? C13B Fe1B C10B C11B 82.7(2) . . . . ? C3B Fe1B C10B C15B -77.9(6) . . . . ? C1B Fe1B C10B C15B 44.0(4) . . . . ? C5B Fe1B C10B C15B 2.3(4) . . . . ? C2B Fe1B C10B C15B 81.9(7) . . . . ? C4B Fe1B C10B C15B -40.7(4) . . . . ? C14B Fe1B C10B C15B -120.8(4) . . . . ? C12B Fe1B C10B C15B 158.1(4) . . . . ? C13B Fe1B C10B C15B -158.1(4) . . . . ? C11B Fe1B C10B C15B 119.2(4) . . . . ? C14B C10B C11B C12B -0.6(4) . . . . ? C15B C10B C11B C12B 176.4(3) . . . . ? Fe1B C10B C11B C12B -59.6(2) . . . . ? C14B C10B C11B Si1B -179.7(3) . . . . ? C15B C10B C11B Si1B -2.7(5) . . . . ? Fe1B C10B C11B Si1B 121.3(3) . . . . ? C14B C10B C11B Fe1B 59.0(3) . . . . ? C15B C10B C11B Fe1B -124.0(3) . . . . ? C24B Si1B C11B C12B 146.1(3) . . . . ? C25B Si1B C11B C12B -91.7(4) . . . . ? C26B Si1B C11B C12B 26.6(4) . . . . ? C24B Si1B C11B C10B -35.0(4) . . . . ? C25B Si1B C11B C10B 87.2(4) . . . . ? C26B Si1B C11B C10B -154.5(3) . . . . ? C24B Si1B C11B Fe1B 57.6(3) . . . . ? C25B Si1B C11B Fe1B 179.8(2) . . . . ? C26B Si1B C11B Fe1B -61.9(3) . . . . ? C3B Fe1B C11B C12B -39.6(7) . . . . ? C1B Fe1B C11B C12B -117.1(2) . . . . ? C5B Fe1B C11B C12B -159.9(2) . . . . ? C2B Fe1B C11B C12B -74.8(3) . . . . ? C4B Fe1B C11B C12B 165.6(4) . . . . ? C14B Fe1B C11B C12B 80.1(2) . . . . ? C10B Fe1B C11B C12B 117.3(3) . . . . ? C13B Fe1B C11B C12B 36.7(2) . . . . ? C3B Fe1B C11B C10B -156.9(6) . . . . ? C1B Fe1B C11B C10B 125.6(2) . . . . ? C5B Fe1B C11B C10B 82.9(3) . . . . ? C2B Fe1B C11B C10B 168.0(3) . . . . ? C4B Fe1B C11B C10B 48.3(5) . . . . ? C14B Fe1B C11B C10B -37.2(2) . . . . ? C12B Fe1B C11B C10B -117.3(3) . . . . ? C13B Fe1B C11B C10B -80.5(2) . . . . ? C3B Fe1B C11B Si1B 78.4(7) . . . . ? C1B Fe1B C11B Si1B 0.9(3) . . . . ? C5B Fe1B C11B Si1B -41.8(3) . . . . ? C2B Fe1B C11B Si1B 43.3(3) . . . . ? C4B Fe1B C11B Si1B -76.4(5) . . . . ? C14B Fe1B C11B Si1B -161.9(3) . . . . ? C12B Fe1B C11B Si1B 118.0(3) . . . . ? C10B Fe1B C11B Si1B -124.7(3) . . . . ? C13B Fe1B C11B Si1B 154.8(3) . . . . ? C10B C11B C12B C13B 0.8(4) . . . . ? Si1B C11B C12B C13B 179.9(3) . . . . ? Fe1B C11B C12B C13B -58.9(3) . . . . ? C10B C11B C12B Fe1B 59.6(2) . . . . ? Si1B C11B C12B Fe1B -121.3(3) . . . . ? C3B Fe1B C12B C13B -73.3(3) . . . . ? C1B Fe1B C12B C13B -157.0(2) . . . . ? C5B Fe1B C12B C13B 169.7(4) . . . . ? C2B Fe1B C12B C13B -114.8(3) . . . . ? C4B Fe1B C12B C13B -42.1(6) . . . . ? C14B Fe1B C12B C13B 37.8(2) . . . . ? C10B Fe1B C12B C13B 81.8(2) . . . . ? C11B Fe1B C12B C13B 120.7(3) . . . . ? C3B Fe1B C12B C11B 166.0(2) . . . . ? C1B Fe1B C12B C11B 82.3(3) . . . . ? C5B Fe1B C12B C11B 49.0(5) . . . . ? C2B Fe1B C12B C11B 124.5(2) . . . . ? C4B Fe1B C12B C11B -162.9(5) . . . . ? C14B Fe1B C12B C11B -83.0(2) . . . . ? C10B Fe1B C12B C11B -39.0(2) . . . . ? C13B Fe1B C12B C11B -120.7(3) . . . . ? C11B C12B C13B C14B -0.6(5) . . . . ? Fe1B C12B C13B C14B -59.5(3) . . . . ? C11B C12B C13B Fe1B 58.9(3) . . . . ? C3B Fe1B C13B C14B -116.9(3) . . . . ? C1B Fe1B C13B C14B 171.6(4) . . . . ? C5B Fe1B C13B C14B -48.7(6) . . . . ? C2B Fe1B C13B C14B -158.5(2) . . . . ? C4B Fe1B C13B C14B -76.7(3) . . . . ? C12B Fe1B C13B C14B 118.8(3) . . . . ? C10B Fe1B C13B C14B 37.6(2) . . . . ? C11B Fe1B C13B C14B 81.7(2) . . . . ? C3B Fe1B C13B C12B 124.3(3) . . . . ? C1B Fe1B C13B C12B 52.8(5) . . . . ? C5B Fe1B C13B C12B -167.5(5) . . . . ? C2B Fe1B C13B C12B 82.7(3) . . . . ? C4B Fe1B C13B C12B 164.5(3) . . . . ? C14B Fe1B C13B C12B -118.8(3) . . . . ? C10B Fe1B C13B C12B -81.2(2) . . . . ? C11B Fe1B C13B C12B -37.1(2) . . . . ? C12B C13B C14B C10B 0.2(5) . . . . ? Fe1B C13B C14B C10B -59.3(3) . . . . ? C12B C13B C14B Fe1B 59.5(3) . . . . ? C11B C10B C14B C13B 0.3(4) . . . . ? C15B C10B C14B C13B -176.7(4) . . . . ? Fe1B C10B C14B C13B 59.5(3) . . . . ? C11B C10B C14B Fe1B -59.2(2) . . . . ? C15B C10B C14B Fe1B 123.9(4) . . . . ? C3B Fe1B C14B C13B 79.6(3) . . . . ? C1B Fe1B C14B C13B -167.5(5) . . . . ? C5B Fe1B C14B C13B 162.8(3) . . . . ? C2B Fe1B C14B C13B 46.3(5) . . . . ? C4B Fe1B C14B C13B 122.1(3) . . . . ? C12B Fe1B C14B C13B -37.9(3) . . . . ? C10B Fe1B C14B C13B -119.6(3) . . . . ? C11B Fe1B C14B C13B -82.1(3) . . . . ? C3B Fe1B C14B C10B -160.8(3) . . . . ? C1B Fe1B C14B C10B -47.9(7) . . . . ? C5B Fe1B C14B C10B -77.6(3) . . . . ? C2B Fe1B C14B C10B 165.9(4) . . . . ? C4B Fe1B C14B C10B -118.3(3) . . . . ? C12B Fe1B C14B C10B 81.7(3) . . . . ? C13B Fe1B C14B C10B 119.6(3) . . . . ? C11B Fe1B C14B C10B 37.5(2) . . . . ? C14B C10B C15B O16B 121.9(4) . . . . ? C11B C10B C15B O16B -54.6(4) . . . . ? Fe1B C10B C15B O16B -146.1(2) . . . . ? C14B C10B C15B O20B 2.1(5) . . . . ? C11B C10B C15B O20B -174.4(3) . . . . ? Fe1B C10B C15B O20B 94.2(3) . . . . ? O20B C15B O16B C17B -62.8(3) . . . . ? C10B C15B O16B C17B 178.6(3) . . . . ? C15B O16B C17B C21B -177.0(3) . . . . ? C15B O16B C17B C18B 59.2(3) . . . . ? O16B C17B C18B C19B -53.8(4) . . . . ? C21B C17B C18B C19B -173.9(4) . . . . ? C17B C18B C19B O20B 52.9(5) . . . . ? O16B C15B O20B C19B 61.0(4) . . . . ? C10B C15B O20B C19B 178.8(3) . . . . ? C18B C19B O20B C15B -56.4(4) . . . . ? O16B C17B C21B O22B 81.9(4) . . . . ? C18B C17B C21B O22B -157.3(4) . . . . ? C17B C21B O22B C23B -173.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.724 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.059 # Attachment 'pR12.cif' data_erk4471 _database_code_depnum_ccdc_archive 'CCDC 714362' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H28 Fe O2 Si' _chemical_formula_weight 468.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.1788(3) _cell_length_b 13.0739(4) _cell_length_c 17.6425(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2347.80(15) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5395 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8142 _exptl_absorpt_correction_T_max 0.9320 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19459 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.1015 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.30 _reflns_number_total 4759 _reflns_number_gt 3305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _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 -0.01(2) _refine_ls_number_reflns 4759 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Fe Fe 0.16529(4) 0.05050(4) 0.76429(3) 0.03475(17) Uani 1 1 d . . . Si1 Si 0.57492(8) 0.04436(8) 0.86238(6) 0.0313(2) Uani 1 1 d . . . O1 O 0.4142(2) 0.01972(17) 0.85837(17) 0.0402(7) Uani 1 1 d . . . O2 O 0.0517(3) 0.0070(2) 0.9703(2) 0.0691(10) Uani 1 1 d . . . C1 C 0.3137(3) 0.0832(3) 0.8379(2) 0.0368(10) Uani 1 1 d . . . C2 C 0.1901(3) 0.0823(3) 0.8770(2) 0.0363(10) Uani 1 1 d . . . C3 C 0.1094(4) 0.1582(3) 0.8411(3) 0.0446(11) Uani 1 1 d . . . H3 H 0.0223 0.1744 0.8542 0.054 Uiso 1 1 calc R . . C4 C 0.1833(4) 0.2044(3) 0.7829(3) 0.0449(11) Uani 1 1 d . . . H4 H 0.1542 0.2575 0.7512 0.054 Uiso 1 1 calc R . . C5 C 0.3099(3) 0.1573(3) 0.7800(2) 0.0400(10) Uani 1 1 d . . . H5 H 0.3778 0.1729 0.7458 0.048 Uiso 1 1 calc R . . C6 C 0.2120(4) -0.0872(3) 0.7185(3) 0.0561(13) Uani 1 1 d . . . H6 H 0.2860 -0.1265 0.7316 0.067 Uiso 1 1 calc R . . C7 C 0.0868(4) -0.0924(3) 0.7526(3) 0.0536(13) Uani 1 1 d . . . H7 H 0.0633 -0.1370 0.7922 0.064 Uiso 1 1 calc R . . C8 C 0.0025(4) -0.0209(3) 0.7185(3) 0.0530(13) Uani 1 1 d . . . H8 H -0.0859 -0.0086 0.7311 0.064 Uiso 1 1 calc R . . C9 C 0.0765(4) 0.0292(3) 0.6615(3) 0.0499(12) Uani 1 1 d . . . H9 H 0.0456 0.0811 0.6292 0.060 Uiso 1 1 calc R . . C10 C 0.2057(4) -0.0124(3) 0.6614(3) 0.0534(13) Uani 1 1 d . . . H10 H 0.2747 0.0068 0.6290 0.064 Uiso 1 1 calc R . . C11 C 0.1540(4) 0.0085(3) 0.9347(3) 0.0504(11) Uani 1 1 d . . . H11 H 0.2155 -0.0431 0.9456 0.061 Uiso 1 1 calc R . . C21 C 0.6337(3) 0.0691(3) 0.7641(2) 0.0348(9) Uani 1 1 d . . . C22 C 0.6000(4) -0.0017(4) 0.7082(3) 0.0583(13) Uani 1 1 d . . . H22 H 0.5506 -0.0594 0.7224 0.070 Uiso 1 1 calc R . . C23 C 0.6353(4) 0.0088(4) 0.6339(3) 0.0683(15) Uani 1 1 d . . . H23 H 0.6104 -0.0407 0.5980 0.082 Uiso 1 1 calc R . . C24 C 0.7073(5) 0.0921(4) 0.6124(3) 0.0640(14) Uani 1 1 d . . . H24 H 0.7318 0.1003 0.5614 0.077 Uiso 1 1 calc R . . C25 C 0.7437(5) 0.1634(3) 0.6649(3) 0.0673(15) Uani 1 1 d . . . H25 H 0.7932 0.2207 0.6500 0.081 Uiso 1 1 calc R . . C26 C 0.7077(4) 0.1513(3) 0.7401(3) 0.0520(11) Uani 1 1 d . . . H26 H 0.7344 0.2006 0.7758 0.062 Uiso 1 1 calc R . . C31 C 0.6434(3) -0.0814(3) 0.8944(2) 0.0322(9) Uani 1 1 d . . . C32 C 0.5643(4) -0.1623(3) 0.9171(3) 0.0447(11) Uani 1 1 d . . . H32 H 0.4726 -0.1540 0.9176 0.054 Uiso 1 1 calc R . . C33 C 0.6184(5) -0.2555(3) 0.9393(3) 0.0525(13) Uani 1 1 d . . . H33 H 0.5632 -0.3100 0.9533 0.063 Uiso 1 1 calc R . . C34 C 0.7522(4) -0.2677(3) 0.9405(3) 0.0504(12) Uani 1 1 d . . . H34 H 0.7889 -0.3298 0.9572 0.060 Uiso 1 1 calc R . . C35 C 0.8331(4) -0.1891(3) 0.9173(3) 0.0467(10) Uani 1 1 d . . . H35 H 0.9248 -0.1977 0.9176 0.056 Uiso 1 1 calc R . . C36 C 0.7789(4) -0.0979(3) 0.8938(2) 0.0395(10) Uani 1 1 d . . . H36 H 0.8347 -0.0453 0.8769 0.047 Uiso 1 1 calc R . . C41 C 0.6026(4) 0.1490(3) 0.9343(2) 0.0360(10) Uani 1 1 d . . . C42 C 0.7511(4) 0.1693(4) 0.9473(3) 0.0621(15) Uani 1 1 d . . . H42A H 0.7894 0.1971 0.9013 0.093 Uiso 1 1 calc R . . H42B H 0.7947 0.1057 0.9602 0.093 Uiso 1 1 calc R . . H42C H 0.7619 0.2179 0.9883 0.093 Uiso 1 1 calc R . . C43 C 0.5370(4) 0.2503(3) 0.9117(3) 0.0476(12) Uani 1 1 d . . . H43A H 0.4427 0.2407 0.9083 0.071 Uiso 1 1 calc R . . H43B H 0.5706 0.2723 0.8628 0.071 Uiso 1 1 calc R . . H43C H 0.5564 0.3020 0.9495 0.071 Uiso 1 1 calc R . . C44 C 0.5423(5) 0.1128(4) 1.0093(3) 0.0601(13) Uani 1 1 d . . . H44A H 0.5560 0.1645 1.0480 0.090 Uiso 1 1 calc R . . H44B H 0.5840 0.0495 1.0249 0.090 Uiso 1 1 calc R . . H44C H 0.4489 0.1015 1.0026 0.090 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 Fe 0.0308(3) 0.0384(3) 0.0351(3) -0.0006(3) -0.0033(2) 0.0001(2) Si1 0.0255(5) 0.0393(6) 0.0289(6) 0.0027(6) 0.0001(4) 0.0005(5) O1 0.0249(13) 0.0480(17) 0.0477(19) 0.0112(13) -0.0032(11) 0.0013(11) O2 0.052(2) 0.093(2) 0.062(3) 0.0030(19) 0.0179(17) -0.0096(16) C1 0.030(2) 0.039(2) 0.041(3) 0.0000(18) -0.0042(17) -0.0012(15) C2 0.030(2) 0.049(2) 0.030(3) -0.0022(18) -0.0031(16) 0.0032(16) C3 0.035(2) 0.048(3) 0.051(3) -0.013(2) -0.0026(19) 0.0130(18) C4 0.051(2) 0.033(2) 0.051(3) 0.0017(19) -0.011(2) 0.0072(18) C5 0.039(2) 0.039(2) 0.043(3) 0.005(2) -0.0001(17) -0.0031(16) C6 0.052(3) 0.044(2) 0.072(4) -0.012(3) 0.004(2) 0.0021(19) C7 0.061(3) 0.043(2) 0.057(4) 0.005(2) -0.006(2) -0.018(2) C8 0.042(2) 0.060(3) 0.057(4) -0.001(2) -0.007(2) -0.008(2) C9 0.054(2) 0.059(3) 0.037(3) -0.006(2) -0.012(2) -0.006(2) C10 0.060(3) 0.056(3) 0.044(4) -0.020(3) 0.011(2) -0.009(2) C11 0.041(2) 0.065(3) 0.045(3) 0.000(2) 0.005(2) 0.002(2) C21 0.0321(18) 0.039(2) 0.034(2) 0.000(2) -0.0026(16) 0.0028(14) C22 0.058(3) 0.082(3) 0.035(3) -0.009(3) 0.009(2) -0.022(2) C23 0.067(3) 0.097(4) 0.041(4) -0.019(3) -0.002(2) -0.014(3) C24 0.085(4) 0.081(4) 0.027(3) 0.007(3) 0.005(2) 0.021(3) C25 0.099(4) 0.048(3) 0.055(4) 0.008(3) 0.022(3) -0.004(3) C26 0.079(3) 0.037(2) 0.039(3) 0.001(2) 0.014(2) -0.0004(19) C31 0.034(2) 0.037(2) 0.026(3) -0.0018(16) -0.0048(16) 0.0047(16) C32 0.039(2) 0.047(3) 0.048(3) 0.000(2) 0.0029(19) -0.002(2) C33 0.066(3) 0.035(3) 0.057(4) 0.003(2) 0.013(2) -0.007(2) C34 0.067(3) 0.046(3) 0.038(3) 0.007(2) 0.002(2) 0.016(2) C35 0.044(2) 0.053(3) 0.043(3) 0.001(2) -0.002(2) 0.016(2) C36 0.034(2) 0.047(2) 0.037(3) 0.003(2) -0.0005(17) 0.0034(17) C41 0.036(2) 0.041(2) 0.031(3) -0.0022(19) -0.0026(17) -0.0029(17) C42 0.049(3) 0.066(3) 0.071(5) -0.015(3) -0.019(2) 0.000(2) C43 0.047(2) 0.048(3) 0.048(3) -0.008(2) 0.004(2) 0.0025(19) C44 0.081(3) 0.064(3) 0.034(3) -0.007(2) 0.012(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C6 2.029(4) . ? Fe C10 2.034(4) . ? Fe C3 2.036(4) . ? Fe C1 2.037(4) . ? Fe C7 2.043(4) . ? Fe C9 2.045(4) . ? Fe C4 2.047(4) . ? Fe C2 2.048(4) . ? Fe C5 2.048(4) . ? Fe C8 2.066(4) . ? Si1 O1 1.669(2) . ? Si1 C21 1.863(4) . ? Si1 C31 1.873(4) . ? Si1 C41 1.887(4) . ? O1 C1 1.366(4) . ? O2 C11 1.216(5) . ? C1 C5 1.409(5) . ? C1 C2 1.435(5) . ? C2 C3 1.436(5) . ? C2 C11 1.449(6) . ? C3 C4 1.408(6) . ? C4 C5 1.428(5) . ? C6 C10 1.405(6) . ? C6 C7 1.411(6) . ? C7 C8 1.405(6) . ? C8 C9 1.418(6) . ? C9 C10 1.423(6) . ? C21 C26 1.380(5) . ? C21 C22 1.395(6) . ? C22 C23 1.367(7) . ? C23 C24 1.366(7) . ? C24 C25 1.365(7) . ? C25 C26 1.385(7) . ? C31 C32 1.388(5) . ? C31 C36 1.396(5) . ? C32 C33 1.393(6) . ? C33 C34 1.372(6) . ? C34 C35 1.379(6) . ? C35 C36 1.379(5) . ? C41 C44 1.533(6) . ? C41 C43 1.537(5) . ? C41 C42 1.551(5) . ? 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 C6 Fe C10 40.46(18) . . ? C6 Fe C3 160.7(2) . . ? C10 Fe C3 158.44(19) . . ? C6 Fe C1 105.43(17) . . ? C10 Fe C1 120.22(17) . . ? C3 Fe C1 68.76(15) . . ? C6 Fe C7 40.55(17) . . ? C10 Fe C7 67.64(19) . . ? C3 Fe C7 126.20(19) . . ? C1 Fe C7 123.10(17) . . ? C6 Fe C9 68.28(19) . . ? C10 Fe C9 40.83(17) . . ? C3 Fe C9 124.13(17) . . ? C1 Fe C9 157.11(17) . . ? C7 Fe C9 67.26(19) . . ? C6 Fe C4 156.18(18) . . ? C10 Fe C4 121.50(19) . . ? C3 Fe C4 40.36(17) . . ? C1 Fe C4 67.96(16) . . ? C7 Fe C4 161.89(17) . . ? C9 Fe C4 108.42(18) . . ? C6 Fe C2 122.52(19) . . ? C10 Fe C2 157.45(17) . . ? C3 Fe C2 41.18(15) . . ? C1 Fe C2 41.13(14) . . ? C7 Fe C2 109.38(18) . . ? C9 Fe C2 160.65(16) . . ? C4 Fe C2 68.48(17) . . ? C6 Fe C5 119.38(16) . . ? C10 Fe C5 104.54(17) . . ? C3 Fe C5 68.83(16) . . ? C1 Fe C5 40.35(15) . . ? C7 Fe C5 156.74(16) . . ? C9 Fe C5 122.02(17) . . ? C4 Fe C5 40.82(15) . . ? C2 Fe C5 68.99(16) . . ? C6 Fe C8 68.39(18) . . ? C10 Fe C8 68.35(18) . . ? C3 Fe C8 110.40(17) . . ? C1 Fe C8 159.81(17) . . ? C7 Fe C8 39.98(16) . . ? C9 Fe C8 40.33(18) . . ? C4 Fe C8 125.36(17) . . ? C2 Fe C8 124.77(17) . . ? C5 Fe C8 159.60(17) . . ? O1 Si1 C21 108.01(15) . . ? O1 Si1 C31 102.02(14) . . ? C21 Si1 C31 108.24(16) . . ? O1 Si1 C41 108.34(16) . . ? C21 Si1 C41 116.92(18) . . ? C31 Si1 C41 112.21(17) . . ? C1 O1 Si1 128.9(2) . . ? O1 C1 C5 129.1(3) . . ? O1 C1 C2 121.6(3) . . ? C5 C1 C2 109.3(3) . . ? O1 C1 Fe 126.6(3) . . ? C5 C1 Fe 70.2(2) . . ? C2 C1 Fe 69.8(2) . . ? C1 C2 C3 106.5(4) . . ? C1 C2 C11 124.4(3) . . ? C3 C2 C11 128.7(3) . . ? C1 C2 Fe 69.0(2) . . ? C3 C2 Fe 69.0(2) . . ? C11 C2 Fe 121.0(3) . . ? C4 C3 C2 108.2(3) . . ? C4 C3 Fe 70.2(2) . . ? C2 C3 Fe 69.8(2) . . ? C3 C4 C5 108.9(3) . . ? C3 C4 Fe 69.4(2) . . ? C5 C4 Fe 69.6(2) . . ? C1 C5 C4 107.1(3) . . ? C1 C5 Fe 69.4(2) . . ? C4 C5 Fe 69.6(2) . . ? C10 C6 C7 107.4(4) . . ? C10 C6 Fe 70.0(2) . . ? C7 C6 Fe 70.2(2) . . ? C8 C7 C6 109.7(4) . . ? C8 C7 Fe 70.9(2) . . ? C6 C7 Fe 69.2(2) . . ? C7 C8 C9 106.7(4) . . ? C7 C8 Fe 69.1(2) . . ? C9 C8 Fe 69.1(2) . . ? C8 C9 C10 108.4(4) . . ? C8 C9 Fe 70.6(3) . . ? C10 C9 Fe 69.2(2) . . ? C6 C10 C9 107.9(4) . . ? C6 C10 Fe 69.6(3) . . ? C9 C10 Fe 70.0(2) . . ? O2 C11 C2 126.2(4) . . ? C26 C21 C22 115.8(4) . . ? C26 C21 Si1 126.6(3) . . ? C22 C21 Si1 117.6(3) . . ? C23 C22 C21 123.1(4) . . ? C24 C23 C22 119.2(5) . . ? C25 C24 C23 120.1(5) . . ? C24 C25 C26 120.0(4) . . ? C21 C26 C25 121.8(5) . . ? C32 C31 C36 117.2(3) . . ? C32 C31 Si1 122.7(3) . . ? C36 C31 Si1 120.1(3) . . ? C31 C32 C33 121.3(4) . . ? C34 C33 C32 119.9(4) . . ? C33 C34 C35 120.1(4) . . ? C36 C35 C34 119.7(4) . . ? C35 C36 C31 121.8(4) . . ? C44 C41 C43 108.5(4) . . ? C44 C41 C42 108.4(4) . . ? C43 C41 C42 108.2(3) . . ? C44 C41 Si1 107.3(3) . . ? C43 C41 Si1 112.6(3) . . ? C42 C41 Si1 111.6(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 C21 Si1 O1 C1 -65.6(4) . . . . ? C31 Si1 O1 C1 -179.6(3) . . . . ? C41 Si1 O1 C1 61.9(4) . . . . ? Si1 O1 C1 C5 38.7(6) . . . . ? Si1 O1 C1 C2 -140.5(3) . . . . ? Si1 O1 C1 Fe 132.2(3) . . . . ? C6 Fe C1 O1 -7.1(4) . . . . ? C10 Fe C1 O1 -48.3(4) . . . . ? C3 Fe C1 O1 153.5(4) . . . . ? C7 Fe C1 O1 33.3(4) . . . . ? C9 Fe C1 O1 -77.7(5) . . . . ? C4 Fe C1 O1 -162.9(4) . . . . ? C2 Fe C1 O1 115.0(4) . . . . ? C5 Fe C1 O1 -124.6(4) . . . . ? C8 Fe C1 O1 62.0(6) . . . . ? C6 Fe C1 C5 117.5(3) . . . . ? C10 Fe C1 C5 76.3(3) . . . . ? C3 Fe C1 C5 -81.9(3) . . . . ? C7 Fe C1 C5 157.9(3) . . . . ? C9 Fe C1 C5 46.9(5) . . . . ? C4 Fe C1 C5 -38.3(2) . . . . ? C2 Fe C1 C5 -120.4(3) . . . . ? C8 Fe C1 C5 -173.4(4) . . . . ? C6 Fe C1 C2 -122.1(2) . . . . ? C10 Fe C1 C2 -163.3(2) . . . . ? C3 Fe C1 C2 38.5(2) . . . . ? C7 Fe C1 C2 -81.7(3) . . . . ? C9 Fe C1 C2 167.3(4) . . . . ? C4 Fe C1 C2 82.1(2) . . . . ? C5 Fe C1 C2 120.4(3) . . . . ? C8 Fe C1 C2 -53.0(5) . . . . ? O1 C1 C2 C3 179.6(3) . . . . ? C5 C1 C2 C3 0.3(5) . . . . ? Fe C1 C2 C3 -59.1(3) . . . . ? O1 C1 C2 C11 -7.4(6) . . . . ? C5 C1 C2 C11 173.3(4) . . . . ? Fe C1 C2 C11 114.0(4) . . . . ? O1 C1 C2 Fe -121.4(3) . . . . ? C5 C1 C2 Fe 59.3(3) . . . . ? C6 Fe C2 C1 75.5(3) . . . . ? C10 Fe C2 C1 40.3(5) . . . . ? C3 Fe C2 C1 -118.2(3) . . . . ? C7 Fe C2 C1 118.5(2) . . . . ? C9 Fe C2 C1 -165.1(5) . . . . ? C4 Fe C2 C1 -80.7(2) . . . . ? C5 Fe C2 C1 -36.7(2) . . . . ? C8 Fe C2 C1 160.4(2) . . . . ? C6 Fe C2 C3 -166.3(2) . . . . ? C10 Fe C2 C3 158.5(4) . . . . ? C1 Fe C2 C3 118.2(3) . . . . ? C7 Fe C2 C3 -123.3(2) . . . . ? C9 Fe C2 C3 -46.9(6) . . . . ? C4 Fe C2 C3 37.5(2) . . . . ? C5 Fe C2 C3 81.5(2) . . . . ? C8 Fe C2 C3 -81.4(3) . . . . ? C6 Fe C2 C11 -43.0(4) . . . . ? C10 Fe C2 C11 -78.1(5) . . . . ? C3 Fe C2 C11 123.4(4) . . . . ? C1 Fe C2 C11 -118.4(4) . . . . ? C7 Fe C2 C11 0.1(3) . . . . ? C9 Fe C2 C11 76.5(6) . . . . ? C4 Fe C2 C11 160.9(3) . . . . ? C5 Fe C2 C11 -155.2(3) . . . . ? C8 Fe C2 C11 41.9(4) . . . . ? C1 C2 C3 C4 -0.9(5) . . . . ? C11 C2 C3 C4 -173.6(4) . . . . ? Fe C2 C3 C4 -60.0(3) . . . . ? C1 C2 C3 Fe 59.1(3) . . . . ? C11 C2 C3 Fe -113.5(4) . . . . ? C6 Fe C3 C4 156.2(5) . . . . ? C10 Fe C3 C4 -38.5(5) . . . . ? C1 Fe C3 C4 80.5(3) . . . . ? C7 Fe C3 C4 -163.3(3) . . . . ? C9 Fe C3 C4 -78.0(3) . . . . ? C2 Fe C3 C4 119.0(3) . . . . ? C5 Fe C3 C4 37.1(2) . . . . ? C8 Fe C3 C4 -121.1(3) . . . . ? C6 Fe C3 C2 37.2(6) . . . . ? C10 Fe C3 C2 -157.5(4) . . . . ? C1 Fe C3 C2 -38.5(2) . . . . ? C7 Fe C3 C2 77.8(3) . . . . ? C9 Fe C3 C2 163.0(2) . . . . ? C4 Fe C3 C2 -119.0(3) . . . . ? C5 Fe C3 C2 -81.9(2) . . . . ? C8 Fe C3 C2 119.9(2) . . . . ? C2 C3 C4 C5 1.3(5) . . . . ? Fe C3 C4 C5 -58.5(3) . . . . ? C2 C3 C4 Fe 59.8(3) . . . . ? C6 Fe C4 C3 -160.8(4) . . . . ? C10 Fe C4 C3 164.4(2) . . . . ? C1 Fe C4 C3 -82.7(3) . . . . ? C7 Fe C4 C3 48.4(7) . . . . ? C9 Fe C4 C3 121.4(3) . . . . ? C2 Fe C4 C3 -38.2(2) . . . . ? C5 Fe C4 C3 -120.6(4) . . . . ? C8 Fe C4 C3 79.9(3) . . . . ? C6 Fe C4 C5 -40.2(6) . . . . ? C10 Fe C4 C5 -75.0(3) . . . . ? C3 Fe C4 C5 120.6(4) . . . . ? C1 Fe C4 C5 37.9(2) . . . . ? C7 Fe C4 C5 169.0(6) . . . . ? C9 Fe C4 C5 -118.0(3) . . . . ? C2 Fe C4 C5 82.3(2) . . . . ? C8 Fe C4 C5 -159.5(3) . . . . ? O1 C1 C5 C4 -178.7(4) . . . . ? C2 C1 C5 C4 0.5(4) . . . . ? Fe C1 C5 C4 59.6(3) . . . . ? O1 C1 C5 Fe 121.7(4) . . . . ? C2 C1 C5 Fe -59.1(3) . . . . ? C3 C4 C5 C1 -1.1(5) . . . . ? Fe C4 C5 C1 -59.5(3) . . . . ? C3 C4 C5 Fe 58.4(3) . . . . ? C6 Fe C5 C1 -79.0(3) . . . . ? C10 Fe C5 C1 -119.9(3) . . . . ? C3 Fe C5 C1 81.7(3) . . . . ? C7 Fe C5 C1 -52.9(6) . . . . ? C9 Fe C5 C1 -160.4(2) . . . . ? C4 Fe C5 C1 118.4(3) . . . . ? C2 Fe C5 C1 37.4(2) . . . . ? C8 Fe C5 C1 173.5(4) . . . . ? C6 Fe C5 C4 162.6(3) . . . . ? C10 Fe C5 C4 121.7(3) . . . . ? C3 Fe C5 C4 -36.7(2) . . . . ? C1 Fe C5 C4 -118.4(3) . . . . ? C7 Fe C5 C4 -171.4(5) . . . . ? C9 Fe C5 C4 81.2(3) . . . . ? C2 Fe C5 C4 -81.0(3) . . . . ? C8 Fe C5 C4 55.0(6) . . . . ? C3 Fe C6 C10 171.7(4) . . . . ? C1 Fe C6 C10 -118.8(3) . . . . ? C7 Fe C6 C10 117.9(4) . . . . ? C9 Fe C6 C10 38.0(3) . . . . ? C4 Fe C6 C10 -48.6(6) . . . . ? C2 Fe C6 C10 -160.1(2) . . . . ? C5 Fe C6 C10 -77.5(3) . . . . ? C8 Fe C6 C10 81.5(3) . . . . ? C10 Fe C6 C7 -117.9(4) . . . . ? C3 Fe C6 C7 53.8(6) . . . . ? C1 Fe C6 C7 123.3(3) . . . . ? C9 Fe C6 C7 -80.0(3) . . . . ? C4 Fe C6 C7 -166.5(4) . . . . ? C2 Fe C6 C7 82.0(3) . . . . ? C5 Fe C6 C7 164.5(3) . . . . ? C8 Fe C6 C7 -36.4(3) . . . . ? C10 C6 C7 C8 -0.9(5) . . . . ? Fe C6 C7 C8 59.5(3) . . . . ? C10 C6 C7 Fe -60.4(3) . . . . ? C6 Fe C7 C8 -120.8(5) . . . . ? C10 Fe C7 C8 -82.5(3) . . . . ? C3 Fe C7 C8 78.4(4) . . . . ? C1 Fe C7 C8 165.1(3) . . . . ? C9 Fe C7 C8 -38.1(3) . . . . ? C4 Fe C7 C8 41.5(8) . . . . ? C2 Fe C7 C8 121.4(3) . . . . ? C5 Fe C7 C8 -156.9(4) . . . . ? C10 Fe C7 C6 38.3(3) . . . . ? C3 Fe C7 C6 -160.8(3) . . . . ? C1 Fe C7 C6 -74.1(4) . . . . ? C9 Fe C7 C6 82.7(3) . . . . ? C4 Fe C7 C6 162.4(6) . . . . ? C2 Fe C7 C6 -117.7(3) . . . . ? C5 Fe C7 C6 -36.0(6) . . . . ? C8 Fe C7 C6 120.8(5) . . . . ? C6 C7 C8 C9 0.6(5) . . . . ? Fe C7 C8 C9 59.1(3) . . . . ? C6 C7 C8 Fe -58.5(3) . . . . ? C6 Fe C8 C7 36.9(3) . . . . ? C10 Fe C8 C7 80.6(3) . . . . ? C3 Fe C8 C7 -122.5(3) . . . . ? C1 Fe C8 C7 -38.7(6) . . . . ? C9 Fe C8 C7 118.4(4) . . . . ? C4 Fe C8 C7 -165.4(3) . . . . ? C2 Fe C8 C7 -78.5(3) . . . . ? C5 Fe C8 C7 153.6(4) . . . . ? C6 Fe C8 C9 -81.5(3) . . . . ? C10 Fe C8 C9 -37.8(3) . . . . ? C3 Fe C8 C9 119.1(3) . . . . ? C1 Fe C8 C9 -157.1(4) . . . . ? C7 Fe C8 C9 -118.4(4) . . . . ? C4 Fe C8 C9 76.3(3) . . . . ? C2 Fe C8 C9 163.1(2) . . . . ? C5 Fe C8 C9 35.2(6) . . . . ? C7 C8 C9 C10 -0.1(5) . . . . ? Fe C8 C9 C10 59.1(3) . . . . ? C7 C8 C9 Fe -59.1(3) . . . . ? C6 Fe C9 C8 81.8(3) . . . . ? C10 Fe C9 C8 119.4(4) . . . . ? C3 Fe C9 C8 -81.5(3) . . . . ? C1 Fe C9 C8 159.8(4) . . . . ? C7 Fe C9 C8 37.8(3) . . . . ? C4 Fe C9 C8 -123.4(3) . . . . ? C2 Fe C9 C8 -46.0(6) . . . . ? C5 Fe C9 C8 -166.3(2) . . . . ? C6 Fe C9 C10 -37.7(2) . . . . ? C3 Fe C9 C10 159.1(3) . . . . ? C1 Fe C9 C10 40.4(5) . . . . ? C7 Fe C9 C10 -81.6(3) . . . . ? C4 Fe C9 C10 117.2(3) . . . . ? C2 Fe C9 C10 -165.4(5) . . . . ? C5 Fe C9 C10 74.3(3) . . . . ? C8 Fe C9 C10 -119.4(4) . . . . ? C7 C6 C10 C9 0.8(5) . . . . ? Fe C6 C10 C9 -59.8(3) . . . . ? C7 C6 C10 Fe 60.6(3) . . . . ? C8 C9 C10 C6 -0.5(5) . . . . ? Fe C9 C10 C6 59.5(3) . . . . ? C8 C9 C10 Fe -60.0(3) . . . . ? C3 Fe C10 C6 -172.6(4) . . . . ? C1 Fe C10 C6 78.0(3) . . . . ? C7 Fe C10 C6 -38.4(2) . . . . ? C9 Fe C10 C6 -119.0(4) . . . . ? C4 Fe C10 C6 159.2(2) . . . . ? C2 Fe C10 C6 48.5(5) . . . . ? C5 Fe C10 C6 118.5(3) . . . . ? C8 Fe C10 C6 -81.7(3) . . . . ? C6 Fe C10 C9 119.0(4) . . . . ? C3 Fe C10 C9 -53.6(5) . . . . ? C1 Fe C10 C9 -163.1(2) . . . . ? C7 Fe C10 C9 80.6(3) . . . . ? C4 Fe C10 C9 -81.8(3) . . . . ? C2 Fe C10 C9 167.4(4) . . . . ? C5 Fe C10 C9 -122.5(2) . . . . ? C8 Fe C10 C9 37.3(2) . . . . ? C1 C2 C11 O2 178.1(4) . . . . ? C3 C2 C11 O2 -10.5(8) . . . . ? Fe C2 C11 O2 -97.3(5) . . . . ? O1 Si1 C21 C26 129.7(3) . . . . ? C31 Si1 C21 C26 -120.5(3) . . . . ? C41 Si1 C21 C26 7.3(4) . . . . ? O1 Si1 C21 C22 -49.9(3) . . . . ? C31 Si1 C21 C22 59.8(3) . . . . ? C41 Si1 C21 C22 -172.3(3) . . . . ? C26 C21 C22 C23 -0.8(6) . . . . ? Si1 C21 C22 C23 178.9(4) . . . . ? C21 C22 C23 C24 0.1(8) . . . . ? C22 C23 C24 C25 0.3(8) . . . . ? C23 C24 C25 C26 0.0(8) . . . . ? C22 C21 C26 C25 1.2(6) . . . . ? Si1 C21 C26 C25 -178.5(3) . . . . ? C24 C25 C26 C21 -0.8(7) . . . . ? O1 Si1 C31 C32 -7.8(4) . . . . ? C21 Si1 C31 C32 -121.6(3) . . . . ? C41 Si1 C31 C32 107.9(3) . . . . ? O1 Si1 C31 C36 170.2(3) . . . . ? C21 Si1 C31 C36 56.4(4) . . . . ? C41 Si1 C31 C36 -74.1(4) . . . . ? C36 C31 C32 C33 0.7(6) . . . . ? Si1 C31 C32 C33 178.8(3) . . . . ? C31 C32 C33 C34 1.6(7) . . . . ? C32 C33 C34 C35 -2.3(7) . . . . ? C33 C34 C35 C36 0.8(7) . . . . ? C34 C35 C36 C31 1.6(7) . . . . ? C32 C31 C36 C35 -2.3(6) . . . . ? Si1 C31 C36 C35 179.6(3) . . . . ? O1 Si1 C41 C44 55.8(3) . . . . ? C21 Si1 C41 C44 178.1(3) . . . . ? C31 Si1 C41 C44 -56.0(3) . . . . ? O1 Si1 C41 C43 -63.5(3) . . . . ? C21 Si1 C41 C43 58.8(3) . . . . ? C31 Si1 C41 C43 -175.3(3) . . . . ? O1 Si1 C41 C42 174.5(3) . . . . ? C21 Si1 C41 C42 -63.2(4) . . . . ? C31 Si1 C41 C42 62.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.810 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.132 # Attachment 'pR19a.cif' data_erk4343 _database_code_depnum_ccdc_archive 'CCDC 714363' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H45 Fe N O Si' _chemical_formula_weight 627.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.1488(2) _cell_length_b 11.8559(2) _cell_length_c 16.8475(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.095(1) _cell_angle_gamma 90.00 _cell_volume 1779.88(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3327 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.486 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7757 _exptl_absorpt_correction_T_max 0.8881 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12584 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.91 _reflns_number_total 7634 _reflns_number_gt 5448 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0434P)^2^+0.0216P] 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 riding _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 -0.036(12) _refine_ls_number_reflns 7634 _refine_ls_number_parameters 395 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Fe Fe 0.01333(4) 0.50358(3) 0.82255(2) 0.04303(12) Uani 1 1 d . . . C1 C 0.1114(6) 0.5663(5) 0.9337(3) 0.0914(16) Uani 1 1 d . . . H1 H 0.2026 0.6061 0.9467 0.110 Uiso 1 1 calc R . . C2 C -0.0343(8) 0.6133(4) 0.9047(3) 0.0970(18) Uani 1 1 d . . . H2 H -0.0583 0.6898 0.8946 0.116 Uiso 1 1 calc R . . C3 C -0.1325(5) 0.5244(6) 0.8945(2) 0.0917(14) Uani 1 1 d . . . H3 H -0.2372 0.5296 0.8758 0.110 Uiso 1 1 calc R . . C4 C -0.0541(6) 0.4276(4) 0.9158(3) 0.0852(13) Uani 1 1 d . . . H4 H -0.0960 0.3550 0.9144 0.102 Uiso 1 1 calc R . . C5 C 0.0931(6) 0.4520(4) 0.9392(2) 0.0720(12) Uani 1 1 d . . . H5 H 0.1706 0.3993 0.9565 0.086 Uiso 1 1 calc R . . C6 C 0.1254(3) 0.4260(2) 0.74512(17) 0.0360(7) Uani 1 1 d . . . C7 C 0.1362(3) 0.5451(2) 0.73858(17) 0.0365(6) Uani 1 1 d . . . C8 C -0.0145(3) 0.5876(3) 0.71510(18) 0.0431(7) Uani 1 1 d . . . H8 H -0.0429 0.6637 0.7070 0.052 Uiso 1 1 calc R . . C9 C -0.1126(3) 0.4935(3) 0.70646(16) 0.0485(7) Uani 1 1 d . . . H9 H -0.2178 0.4967 0.6903 0.058 Uiso 1 1 calc R . . C10 C -0.0267(4) 0.3941(2) 0.72607(19) 0.0462(7) Uani 1 1 d . . . H10 H -0.0642 0.3203 0.7263 0.055 Uiso 1 1 calc R . . C11 C 0.2762(3) 0.6056(2) 0.74967(16) 0.0366(6) Uani 1 1 d . . . H11 H 0.3654 0.5669 0.7727 0.044 Uiso 1 1 calc R . . N12 N 0.2854(2) 0.70911(19) 0.72984(13) 0.0406(6) Uani 1 1 d . . . C13 C 0.4326(3) 0.7566(2) 0.73982(17) 0.0372(6) Uani 1 1 d . . . C14 C 0.4880(3) 0.7697(3) 0.66893(18) 0.0492(8) Uani 1 1 d . . . C141 C 0.3974(4) 0.7350(3) 0.58608(19) 0.0631(9) Uani 1 1 d . . . H141 H 0.2967 0.7121 0.5925 0.076 Uiso 1 1 calc R . . C142 C 0.4684(6) 0.6327(4) 0.5534(3) 0.1155(17) Uani 1 1 d . . . H14A H 0.4700 0.5691 0.5898 0.173 Uiso 1 1 calc R . . H14B H 0.5702 0.6510 0.5501 0.173 Uiso 1 1 calc R . . H14C H 0.4099 0.6133 0.4996 0.173 Uiso 1 1 calc R . . C143 C 0.3765(6) 0.8315(4) 0.5252(3) 0.1097(17) Uani 1 1 d . . . H14D H 0.4738 0.8565 0.5182 0.165 Uiso 1 1 calc R . . H14E H 0.3260 0.8936 0.5452 0.165 Uiso 1 1 calc R . . H14F H 0.3165 0.8060 0.4732 0.165 Uiso 1 1 calc R . . C15 C 0.6298(4) 0.8163(3) 0.6778(2) 0.0629(9) Uani 1 1 d . . . H15 H 0.6709 0.8243 0.6318 0.075 Uiso 1 1 calc R . . C16 C 0.7110(4) 0.8508(3) 0.7522(3) 0.0693(10) Uani 1 1 d . . . H16 H 0.8069 0.8822 0.7566 0.083 Uiso 1 1 calc R . . C17 C 0.6541(4) 0.8401(3) 0.8200(2) 0.0601(9) Uani 1 1 d . . . H17 H 0.7109 0.8654 0.8705 0.072 Uiso 1 1 calc R . . C18 C 0.5133(3) 0.7925(3) 0.81560(19) 0.0457(8) Uani 1 1 d . . . C181 C 0.4529(4) 0.7807(2) 0.89228(17) 0.0510(8) Uani 1 1 d . . . H181 H 0.3451 0.7616 0.8746 0.061 Uiso 1 1 calc R . . C182 C 0.5292(5) 0.6831(3) 0.9460(2) 0.0751(11) Uani 1 1 d . . . H18A H 0.4855 0.6757 0.9931 0.113 Uiso 1 1 calc R . . H18B H 0.6358 0.6983 0.9639 0.113 Uiso 1 1 calc R . . H18C H 0.5145 0.6135 0.9149 0.113 Uiso 1 1 calc R . . C183 C 0.4635(4) 0.8900(3) 0.9415(2) 0.0704(10) Uani 1 1 d . . . H18D H 0.5681 0.9091 0.9627 0.106 Uiso 1 1 calc R . . H18E H 0.4147 0.8797 0.9865 0.106 Uiso 1 1 calc R . . H18F H 0.4143 0.9504 0.9067 0.106 Uiso 1 1 calc R . . O1 O 0.2504(2) 0.35849(14) 0.76430(11) 0.0402(5) Uani 1 1 d . . . Si1 Si 0.27297(8) 0.23639(6) 0.71909(4) 0.03756(19) Uani 1 1 d . . . C21 C 0.1864(3) 0.1244(2) 0.77177(17) 0.0384(6) Uani 1 1 d . . . C22 C 0.1327(3) 0.1539(3) 0.83978(17) 0.0485(7) Uani 1 1 d . . . H22 H 0.1381 0.2296 0.8566 0.058 Uiso 1 1 calc R . . C23 C 0.0718(4) 0.0754(3) 0.8834(2) 0.0579(9) Uani 1 1 d . . . H23 H 0.0346 0.0980 0.9285 0.070 Uiso 1 1 calc R . . C24 C 0.0658(3) -0.0363(2) 0.8605(2) 0.0532(8) Uani 1 1 d . . . H24 H 0.0268 -0.0904 0.8910 0.064 Uiso 1 1 calc R . . C25 C 0.1167(3) -0.0691(2) 0.79322(19) 0.0464(7) Uani 1 1 d . . . H25 H 0.1111 -0.1452 0.7773 0.056 Uiso 1 1 calc R . . C26 C 0.1759(3) 0.0098(3) 0.74916(15) 0.0403(6) Uani 1 1 d . . . H26 H 0.2100 -0.0133 0.7031 0.048 Uiso 1 1 calc R . . C31 C 0.1815(3) 0.2527(2) 0.60912(16) 0.0419(7) Uani 1 1 d . . . C32 C 0.0995(4) 0.1678(3) 0.56189(19) 0.0564(8) Uani 1 1 d . . . H32 H 0.0911 0.0971 0.5857 0.068 Uiso 1 1 calc R . . C33 C 0.0298(4) 0.1848(3) 0.4807(2) 0.0709(10) Uani 1 1 d . . . H33 H -0.0232 0.1254 0.4500 0.085 Uiso 1 1 calc R . . C34 C 0.0382(4) 0.2879(3) 0.44495(19) 0.0649(9) Uani 1 1 d . . . H34 H -0.0123 0.3002 0.3905 0.078 Uiso 1 1 calc R . . C35 C 0.1208(4) 0.3732(3) 0.48920(19) 0.0605(9) Uani 1 1 d . . . H35 H 0.1299 0.4431 0.4644 0.073 Uiso 1 1 calc R . . C36 C 0.1904(4) 0.3560(2) 0.57018(18) 0.0520(8) Uani 1 1 d . . . H36 H 0.2452 0.4154 0.5999 0.062 Uiso 1 1 calc R . . C41 C 0.4816(3) 0.2189(2) 0.73762(18) 0.0458(7) Uani 1 1 d . . . C42 C 0.5160(4) 0.1117(3) 0.6929(3) 0.0752(11) Uani 1 1 d . . . H42A H 0.4745 0.0463 0.7146 0.113 Uiso 1 1 calc R . . H42B H 0.6237 0.1028 0.7009 0.113 Uiso 1 1 calc R . . H42C H 0.4713 0.1187 0.6351 0.113 Uiso 1 1 calc R . . C43 C 0.5498(4) 0.2064(4) 0.8284(2) 0.0727(11) Uani 1 1 d . . . H43A H 0.5295 0.2739 0.8566 0.109 Uiso 1 1 calc R . . H43B H 0.6573 0.1959 0.8370 0.109 Uiso 1 1 calc R . . H43C H 0.5058 0.1416 0.8493 0.109 Uiso 1 1 calc R . . C44 C 0.5520(4) 0.3208(3) 0.7054(3) 0.0721(10) Uani 1 1 d . . . H44A H 0.6605 0.3146 0.7208 0.108 Uiso 1 1 calc R . . H44B H 0.5207 0.3892 0.7284 0.108 Uiso 1 1 calc R . . H44C H 0.5196 0.3233 0.6464 0.108 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 Fe 0.0399(2) 0.0522(2) 0.0408(2) 0.00195(19) 0.01724(17) 0.0013(2) C1 0.089(4) 0.144(5) 0.052(3) -0.038(3) 0.040(3) -0.054(3) C2 0.182(6) 0.059(3) 0.067(3) 0.0015(19) 0.064(4) 0.027(3) C3 0.062(3) 0.159(5) 0.065(3) -0.008(3) 0.037(2) 0.024(3) C4 0.105(4) 0.102(4) 0.061(3) 0.002(2) 0.046(3) -0.031(3) C5 0.084(3) 0.095(3) 0.035(2) 0.0030(18) 0.008(2) 0.025(2) C6 0.0344(17) 0.0427(16) 0.0318(15) -0.0050(11) 0.0097(13) -0.0020(12) C7 0.0350(17) 0.0471(16) 0.0286(15) -0.0024(11) 0.0100(12) -0.0022(11) C8 0.0426(19) 0.0493(16) 0.0372(17) 0.0037(12) 0.0085(14) -0.0020(14) C9 0.0332(14) 0.0616(19) 0.0497(16) 0.0039(16) 0.0071(12) -0.0015(16) C10 0.0418(18) 0.0496(17) 0.0470(19) -0.0029(13) 0.0097(15) -0.0107(14) C11 0.0368(17) 0.0408(17) 0.0328(16) -0.0037(11) 0.0094(13) -0.0020(12) N12 0.0356(14) 0.0510(16) 0.0374(13) -0.0072(10) 0.0130(11) -0.0063(10) C13 0.0320(16) 0.0372(15) 0.0433(16) 0.0013(11) 0.0104(13) 0.0036(11) C14 0.0452(19) 0.0515(19) 0.054(2) -0.0005(13) 0.0177(16) -0.0054(13) C141 0.063(2) 0.085(2) 0.048(2) -0.0024(17) 0.0264(17) -0.0162(18) C142 0.136(5) 0.118(4) 0.097(4) -0.048(3) 0.035(3) -0.007(3) C143 0.132(5) 0.129(4) 0.061(3) 0.014(3) 0.007(3) -0.022(3) C15 0.050(2) 0.073(2) 0.076(3) 0.0041(18) 0.034(2) -0.0045(17) C16 0.038(2) 0.078(2) 0.092(3) 0.002(2) 0.014(2) -0.0168(17) C17 0.041(2) 0.068(2) 0.065(2) -0.0028(16) -0.0022(18) -0.0083(16) C18 0.0343(18) 0.0445(16) 0.055(2) 0.0009(13) 0.0037(15) 0.0002(13) C181 0.0466(19) 0.0614(18) 0.0416(17) -0.0010(14) 0.0032(15) 0.0029(14) C182 0.087(3) 0.083(3) 0.055(2) 0.0075(17) 0.014(2) 0.019(2) C183 0.065(2) 0.076(2) 0.064(2) -0.0185(18) 0.0002(19) 0.0017(18) O1 0.0390(12) 0.0406(10) 0.0410(11) -0.0058(8) 0.0093(9) -0.0030(8) Si1 0.0380(5) 0.0416(4) 0.0349(4) -0.0016(3) 0.0121(3) -0.0037(3) C21 0.0342(16) 0.0454(16) 0.0348(16) 0.0010(11) 0.0064(13) -0.0051(12) C22 0.055(2) 0.0496(17) 0.0447(18) -0.0051(13) 0.0202(16) -0.0037(14) C23 0.073(2) 0.068(2) 0.0420(19) 0.0055(15) 0.0318(18) -0.0038(17) C24 0.048(2) 0.0542(19) 0.061(2) 0.0121(15) 0.0192(17) -0.0109(14) C25 0.0372(17) 0.0431(16) 0.0567(19) 0.0018(14) 0.0057(15) -0.0023(12) C26 0.0384(14) 0.0450(15) 0.0381(14) -0.0024(14) 0.0098(12) -0.0027(14) C31 0.0390(17) 0.0491(17) 0.0390(16) 0.0001(13) 0.0117(13) 0.0022(13) C32 0.065(2) 0.0560(18) 0.047(2) 0.0017(14) 0.0096(17) -0.0118(16) C33 0.079(3) 0.080(3) 0.046(2) -0.0075(17) -0.0013(19) -0.0052(19) C34 0.072(2) 0.085(2) 0.0342(18) -0.0014(17) 0.0062(17) 0.0135(19) C35 0.081(3) 0.062(2) 0.042(2) 0.0087(15) 0.0224(18) 0.0184(18) C36 0.063(2) 0.0511(18) 0.0434(19) -0.0021(13) 0.0158(16) 0.0036(14) C41 0.0389(17) 0.0514(17) 0.0497(18) 0.0034(13) 0.0152(15) -0.0001(13) C42 0.058(2) 0.076(3) 0.099(3) -0.010(2) 0.034(2) 0.0137(18) C43 0.050(2) 0.107(3) 0.056(2) 0.0082(19) 0.0013(18) -0.003(2) C44 0.044(2) 0.077(2) 0.101(3) 0.020(2) 0.028(2) -0.0068(17) _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 Fe C3 2.011(3) . ? Fe C2 2.018(4) . ? Fe C4 2.025(4) . ? Fe C1 2.026(4) . ? Fe C5 2.030(4) . ? Fe C8 2.031(3) . ? Fe C9 2.036(3) . ? Fe C10 2.047(3) . ? Fe C6 2.051(3) . ? Fe C7 2.056(3) . ? C1 C5 1.371(6) . ? C1 C2 1.426(7) . ? C2 C3 1.370(7) . ? C3 C4 1.358(6) . ? C4 C5 1.346(6) . ? C6 O1 1.373(3) . ? C6 C10 1.407(4) . ? C6 C7 1.421(4) . ? C7 C8 1.437(4) . ? C7 C11 1.443(4) . ? C8 C9 1.419(4) . ? C9 C10 1.413(4) . ? C11 N12 1.280(3) . ? N12 C13 1.434(3) . ? C13 C18 1.389(4) . ? C13 C14 1.408(4) . ? C14 C15 1.387(4) . ? C14 C141 1.510(4) . ? C141 C143 1.520(5) . ? C141 C142 1.536(6) . ? C15 C16 1.366(5) . ? C16 C17 1.365(5) . ? C17 C18 1.393(4) . ? C18 C181 1.522(4) . ? C181 C183 1.530(4) . ? C181 C182 1.537(4) . ? O1 Si1 1.6702(19) . ? Si1 C31 1.862(3) . ? Si1 C21 1.870(3) . ? Si1 C41 1.875(3) . ? C21 C22 1.390(4) . ? C21 C26 1.408(4) . ? C22 C23 1.379(4) . ? C23 C24 1.377(4) . ? C24 C25 1.375(4) . ? C25 C26 1.379(4) . ? C31 C32 1.392(4) . ? C31 C36 1.401(4) . ? C32 C33 1.387(4) . ? C33 C34 1.373(5) . ? C34 C35 1.376(5) . ? C35 C36 1.384(4) . ? C41 C43 1.522(4) . ? C41 C44 1.526(4) . ? C41 C42 1.545(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe C2 39.8(2) . . ? C3 Fe C4 39.33(19) . . ? C2 Fe C4 66.63(18) . . ? C3 Fe C1 67.23(18) . . ? C2 Fe C1 41.3(2) . . ? C4 Fe C1 66.09(18) . . ? C3 Fe C5 66.14(17) . . ? C2 Fe C5 67.44(17) . . ? C4 Fe C5 38.78(17) . . ? C1 Fe C5 39.52(16) . . ? C3 Fe C8 120.69(18) . . ? C2 Fe C8 106.98(15) . . ? C4 Fe C8 155.64(18) . . ? C1 Fe C8 125.72(18) . . ? C5 Fe C8 162.91(18) . . ? C3 Fe C9 106.14(15) . . ? C2 Fe C9 122.2(2) . . ? C4 Fe C9 120.91(17) . . ? C1 Fe C9 161.0(2) . . ? C5 Fe C9 155.99(17) . . ? C8 Fe C9 40.83(12) . . ? C3 Fe C10 122.18(19) . . ? C2 Fe C10 157.8(2) . . ? C4 Fe C10 107.63(16) . . ? C1 Fe C10 158.3(2) . . ? C5 Fe C10 122.55(15) . . ? C8 Fe C10 68.88(11) . . ? C9 Fe C10 40.50(13) . . ? C3 Fe C6 159.11(19) . . ? C2 Fe C6 160.5(2) . . ? C4 Fe C6 125.33(17) . . ? C1 Fe C6 124.91(17) . . ? C5 Fe C6 111.03(14) . . ? C8 Fe C6 68.47(12) . . ? C9 Fe C6 67.55(12) . . ? C10 Fe C6 40.17(12) . . ? C3 Fe C7 157.85(19) . . ? C2 Fe C7 123.68(18) . . ? C4 Fe C7 161.91(18) . . ? C1 Fe C7 110.60(14) . . ? C5 Fe C7 127.28(16) . . ? C8 Fe C7 41.17(12) . . ? C9 Fe C7 68.38(11) . . ? C10 Fe C7 68.45(11) . . ? C6 Fe C7 40.49(11) . . ? C5 C1 C2 106.9(4) . . ? C5 C1 Fe 70.4(3) . . ? C2 C1 Fe 69.0(2) . . ? C3 C2 C1 106.1(4) . . ? C3 C2 Fe 69.8(2) . . ? C1 C2 Fe 69.7(2) . . ? C4 C3 C2 109.0(4) . . ? C4 C3 Fe 70.9(2) . . ? C2 C3 Fe 70.4(2) . . ? C5 C4 C3 109.2(4) . . ? C5 C4 Fe 70.8(2) . . ? C3 C4 Fe 69.8(2) . . ? C4 C5 C1 108.8(4) . . ? C4 C5 Fe 70.4(2) . . ? C1 C5 Fe 70.1(3) . . ? O1 C6 C10 128.7(2) . . ? O1 C6 C7 121.9(3) . . ? C10 C6 C7 109.4(3) . . ? O1 C6 Fe 128.43(19) . . ? C10 C6 Fe 69.78(17) . . ? C7 C6 Fe 69.95(17) . . ? C6 C7 C8 106.9(3) . . ? C6 C7 C11 124.0(3) . . ? C8 C7 C11 129.0(2) . . ? C6 C7 Fe 69.56(18) . . ? C8 C7 Fe 68.50(16) . . ? C11 C7 Fe 129.6(2) . . ? C9 C8 C7 107.3(3) . . ? C9 C8 Fe 69.77(16) . . ? C7 C8 Fe 70.33(17) . . ? C10 C9 C8 109.1(2) . . ? C10 C9 Fe 70.18(17) . . ? C8 C9 Fe 69.41(16) . . ? C6 C10 C9 107.3(2) . . ? C6 C10 Fe 70.05(17) . . ? C9 C10 Fe 69.33(17) . . ? N12 C11 C7 123.5(3) . . ? C11 N12 C13 117.5(2) . . ? C18 C13 C14 121.8(3) . . ? C18 C13 N12 121.2(3) . . ? C14 C13 N12 116.9(2) . . ? C15 C14 C13 117.4(3) . . ? C15 C14 C141 120.8(3) . . ? C13 C14 C141 121.8(3) . . ? C14 C141 C143 112.2(3) . . ? C14 C141 C142 111.0(3) . . ? C143 C141 C142 110.5(3) . . ? C16 C15 C14 121.3(3) . . ? C17 C16 C15 120.6(3) . . ? C16 C17 C18 121.1(3) . . ? C13 C18 C17 117.8(3) . . ? C13 C18 C181 122.2(3) . . ? C17 C18 C181 120.1(3) . . ? C18 C181 C183 113.1(3) . . ? C18 C181 C182 111.4(3) . . ? C183 C181 C182 110.7(3) . . ? C6 O1 Si1 125.49(17) . . ? O1 Si1 C31 106.85(11) . . ? O1 Si1 C21 106.83(11) . . ? C31 Si1 C21 113.74(12) . . ? O1 Si1 C41 104.28(12) . . ? C31 Si1 C41 112.85(13) . . ? C21 Si1 C41 111.54(13) . . ? C22 C21 C26 116.8(3) . . ? C22 C21 Si1 118.7(2) . . ? C26 C21 Si1 124.5(2) . . ? C23 C22 C21 122.0(3) . . ? C24 C23 C22 119.7(3) . . ? C25 C24 C23 120.1(3) . . ? C24 C25 C26 120.0(3) . . ? C25 C26 C21 121.3(3) . . ? C32 C31 C36 116.4(3) . . ? C32 C31 Si1 123.8(2) . . ? C36 C31 Si1 119.7(2) . . ? C33 C32 C31 121.8(3) . . ? C34 C33 C32 120.2(3) . . ? C33 C34 C35 119.7(3) . . ? C34 C35 C36 120.0(3) . . ? C35 C36 C31 121.9(3) . . ? C43 C41 C44 109.0(3) . . ? C43 C41 C42 109.2(3) . . ? C44 C41 C42 109.2(3) . . ? C43 C41 Si1 110.3(2) . . ? C44 C41 Si1 110.4(2) . . ? C42 C41 Si1 108.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Fe C1 C5 79.6(3) . . . . ? C2 Fe C1 C5 117.8(4) . . . . ? C4 Fe C1 C5 36.6(3) . . . . ? C8 Fe C1 C5 -168.1(3) . . . . ? C9 Fe C1 C5 152.6(4) . . . . ? C10 Fe C1 C5 -40.8(6) . . . . ? C6 Fe C1 C5 -80.9(3) . . . . ? C7 Fe C1 C5 -124.1(3) . . . . ? C3 Fe C1 C2 -38.2(3) . . . . ? C4 Fe C1 C2 -81.2(3) . . . . ? C5 Fe C1 C2 -117.8(4) . . . . ? C8 Fe C1 C2 74.1(3) . . . . ? C9 Fe C1 C2 34.8(6) . . . . ? C10 Fe C1 C2 -158.7(4) . . . . ? C6 Fe C1 C2 161.3(3) . . . . ? C7 Fe C1 C2 118.0(3) . . . . ? C5 C1 C2 C3 0.2(5) . . . . ? Fe C1 C2 C3 60.7(3) . . . . ? C5 C1 C2 Fe -60.5(3) . . . . ? C4 Fe C2 C3 -37.0(3) . . . . ? C1 Fe C2 C3 -116.9(4) . . . . ? C5 Fe C2 C3 -79.3(3) . . . . ? C8 Fe C2 C3 117.9(3) . . . . ? C9 Fe C2 C3 75.9(3) . . . . ? C10 Fe C2 C3 42.3(5) . . . . ? C6 Fe C2 C3 -168.8(4) . . . . ? C7 Fe C2 C3 159.9(3) . . . . ? C3 Fe C2 C1 116.9(4) . . . . ? C4 Fe C2 C1 79.8(3) . . . . ? C5 Fe C2 C1 37.5(3) . . . . ? C8 Fe C2 C1 -125.3(3) . . . . ? C9 Fe C2 C1 -167.3(3) . . . . ? C10 Fe C2 C1 159.1(4) . . . . ? C6 Fe C2 C1 -52.0(6) . . . . ? C7 Fe C2 C1 -83.2(3) . . . . ? C1 C2 C3 C4 0.1(5) . . . . ? Fe C2 C3 C4 60.7(3) . . . . ? C1 C2 C3 Fe -60.6(3) . . . . ? C2 Fe C3 C4 -119.2(4) . . . . ? C1 Fe C3 C4 -79.6(3) . . . . ? C5 Fe C3 C4 -36.4(3) . . . . ? C8 Fe C3 C4 161.3(3) . . . . ? C9 Fe C3 C4 119.4(3) . . . . ? C10 Fe C3 C4 78.3(3) . . . . ? C6 Fe C3 C4 50.3(5) . . . . ? C7 Fe C3 C4 -168.5(4) . . . . ? C4 Fe C3 C2 119.2(4) . . . . ? C1 Fe C3 C2 39.7(3) . . . . ? C5 Fe C3 C2 82.9(3) . . . . ? C8 Fe C3 C2 -79.5(3) . . . . ? C9 Fe C3 C2 -121.4(3) . . . . ? C10 Fe C3 C2 -162.5(3) . . . . ? C6 Fe C3 C2 169.5(4) . . . . ? C7 Fe C3 C2 -49.2(5) . . . . ? C2 C3 C4 C5 -0.3(5) . . . . ? Fe C3 C4 C5 60.0(3) . . . . ? C2 C3 C4 Fe -60.4(3) . . . . ? C3 Fe C4 C5 -120.0(4) . . . . ? C2 Fe C4 C5 -82.6(3) . . . . ? C1 Fe C4 C5 -37.3(3) . . . . ? C8 Fe C4 C5 -162.0(3) . . . . ? C9 Fe C4 C5 162.7(2) . . . . ? C10 Fe C4 C5 120.4(3) . . . . ? C6 Fe C4 C5 79.6(3) . . . . ? C7 Fe C4 C5 45.9(6) . . . . ? C2 Fe C4 C3 37.4(3) . . . . ? C1 Fe C4 C3 82.7(3) . . . . ? C5 Fe C4 C3 120.0(4) . . . . ? C8 Fe C4 C3 -42.0(5) . . . . ? C9 Fe C4 C3 -77.3(3) . . . . ? C10 Fe C4 C3 -119.6(3) . . . . ? C6 Fe C4 C3 -160.4(3) . . . . ? C7 Fe C4 C3 165.9(4) . . . . ? C3 C4 C5 C1 0.4(5) . . . . ? Fe C4 C5 C1 59.8(3) . . . . ? C3 C4 C5 Fe -59.4(3) . . . . ? C2 C1 C5 C4 -0.4(5) . . . . ? Fe C1 C5 C4 -60.0(3) . . . . ? C2 C1 C5 Fe 59.7(3) . . . . ? C3 Fe C5 C4 36.9(3) . . . . ? C2 Fe C5 C4 80.3(3) . . . . ? C1 Fe C5 C4 119.5(4) . . . . ? C8 Fe C5 C4 154.3(5) . . . . ? C9 Fe C5 C4 -38.9(5) . . . . ? C10 Fe C5 C4 -77.2(3) . . . . ? C6 Fe C5 C4 -120.7(3) . . . . ? C7 Fe C5 C4 -163.7(2) . . . . ? C3 Fe C5 C1 -82.6(3) . . . . ? C2 Fe C5 C1 -39.2(3) . . . . ? C4 Fe C5 C1 -119.5(4) . . . . ? C8 Fe C5 C1 34.8(7) . . . . ? C9 Fe C5 C1 -158.3(3) . . . . ? C10 Fe C5 C1 163.3(3) . . . . ? C6 Fe C5 C1 119.8(3) . . . . ? C7 Fe C5 C1 76.8(3) . . . . ? C3 Fe C6 O1 -85.9(5) . . . . ? C2 Fe C6 O1 73.7(5) . . . . ? C4 Fe C6 O1 -49.2(3) . . . . ? C1 Fe C6 O1 34.4(3) . . . . ? C5 Fe C6 O1 -7.9(3) . . . . ? C8 Fe C6 O1 153.8(3) . . . . ? C9 Fe C6 O1 -162.1(3) . . . . ? C10 Fe C6 O1 -123.9(3) . . . . ? C7 Fe C6 O1 115.4(3) . . . . ? C3 Fe C6 C10 38.0(5) . . . . ? C2 Fe C6 C10 -162.4(5) . . . . ? C4 Fe C6 C10 74.7(3) . . . . ? C1 Fe C6 C10 158.3(2) . . . . ? C5 Fe C6 C10 116.0(2) . . . . ? C8 Fe C6 C10 -82.35(18) . . . . ? C9 Fe C6 C10 -38.17(18) . . . . ? C7 Fe C6 C10 -120.7(3) . . . . ? C3 Fe C6 C7 158.7(4) . . . . ? C2 Fe C6 C7 -41.7(6) . . . . ? C4 Fe C6 C7 -164.6(2) . . . . ? C1 Fe C6 C7 -81.0(3) . . . . ? C5 Fe C6 C7 -123.3(2) . . . . ? C8 Fe C6 C7 38.35(18) . . . . ? C9 Fe C6 C7 82.5(2) . . . . ? C10 Fe C6 C7 120.7(3) . . . . ? O1 C6 C7 C8 178.0(2) . . . . ? C10 C6 C7 C8 0.3(4) . . . . ? Fe C6 C7 C8 -58.5(2) . . . . ? O1 C6 C7 C11 1.2(5) . . . . ? C10 C6 C7 C11 -176.5(3) . . . . ? Fe C6 C7 C11 124.7(3) . . . . ? O1 C6 C7 Fe -123.5(3) . . . . ? C10 C6 C7 Fe 58.8(2) . . . . ? C3 Fe C7 C6 -159.9(4) . . . . ? C2 Fe C7 C6 164.5(3) . . . . ? C4 Fe C7 C6 44.2(6) . . . . ? C1 Fe C7 C6 120.1(3) . . . . ? C5 Fe C7 C6 78.6(2) . . . . ? C8 Fe C7 C6 -118.7(3) . . . . ? C9 Fe C7 C6 -80.3(2) . . . . ? C10 Fe C7 C6 -36.61(18) . . . . ? C3 Fe C7 C8 -41.2(5) . . . . ? C2 Fe C7 C8 -76.8(3) . . . . ? C4 Fe C7 C8 162.9(5) . . . . ? C1 Fe C7 C8 -121.2(3) . . . . ? C5 Fe C7 C8 -162.6(2) . . . . ? C9 Fe C7 C8 38.43(17) . . . . ? C10 Fe C7 C8 82.13(17) . . . . ? C6 Fe C7 C8 118.7(3) . . . . ? C3 Fe C7 C11 82.3(5) . . . . ? C2 Fe C7 C11 46.7(4) . . . . ? C4 Fe C7 C11 -73.6(6) . . . . ? C1 Fe C7 C11 2.3(3) . . . . ? C5 Fe C7 C11 -39.1(3) . . . . ? C8 Fe C7 C11 123.5(3) . . . . ? C9 Fe C7 C11 161.9(3) . . . . ? C10 Fe C7 C11 -154.4(3) . . . . ? C6 Fe C7 C11 -117.8(3) . . . . ? C6 C7 C8 C9 -1.1(3) . . . . ? C11 C7 C8 C9 175.5(3) . . . . ? Fe C7 C8 C9 -60.3(2) . . . . ? C6 C7 C8 Fe 59.2(2) . . . . ? C11 C7 C8 Fe -124.2(3) . . . . ? C3 Fe C8 C9 -78.9(3) . . . . ? C2 Fe C8 C9 -120.0(3) . . . . ? C4 Fe C8 C9 -49.3(4) . . . . ? C1 Fe C8 C9 -161.6(2) . . . . ? C5 Fe C8 C9 171.8(5) . . . . ? C10 Fe C8 C9 36.88(17) . . . . ? C6 Fe C8 C9 80.14(18) . . . . ? C7 Fe C8 C9 117.9(2) . . . . ? C3 Fe C8 C7 163.2(2) . . . . ? C2 Fe C8 C7 122.1(3) . . . . ? C4 Fe C8 C7 -167.2(4) . . . . ? C1 Fe C8 C7 80.6(3) . . . . ? C5 Fe C8 C7 54.0(6) . . . . ? C9 Fe C8 C7 -117.9(2) . . . . ? C10 Fe C8 C7 -81.00(17) . . . . ? C6 Fe C8 C7 -37.73(17) . . . . ? C7 C8 C9 C10 1.5(3) . . . . ? Fe C8 C9 C10 -59.1(2) . . . . ? C7 C8 C9 Fe 60.7(2) . . . . ? C3 Fe C9 C10 -121.0(3) . . . . ? C2 Fe C9 C10 -161.2(2) . . . . ? C4 Fe C9 C10 -80.9(2) . . . . ? C1 Fe C9 C10 172.4(4) . . . . ? C5 Fe C9 C10 -53.7(4) . . . . ? C8 Fe C9 C10 120.5(2) . . . . ? C6 Fe C9 C10 37.88(17) . . . . ? C7 Fe C9 C10 81.71(18) . . . . ? C3 Fe C9 C8 118.5(3) . . . . ? C2 Fe C9 C8 78.3(3) . . . . ? C4 Fe C9 C8 158.6(2) . . . . ? C1 Fe C9 C8 51.9(5) . . . . ? C5 Fe C9 C8 -174.1(3) . . . . ? C10 Fe C9 C8 -120.5(2) . . . . ? C6 Fe C9 C8 -82.57(18) . . . . ? C7 Fe C9 C8 -38.75(17) . . . . ? O1 C6 C10 C9 -176.8(3) . . . . ? C7 C6 C10 C9 0.7(4) . . . . ? Fe C6 C10 C9 59.6(2) . . . . ? O1 C6 C10 Fe 123.6(3) . . . . ? C7 C6 C10 Fe -58.9(2) . . . . ? C8 C9 C10 C6 -1.4(3) . . . . ? Fe C9 C10 C6 -60.0(2) . . . . ? C8 C9 C10 Fe 58.6(2) . . . . ? C3 Fe C10 C6 -165.0(2) . . . . ? C2 Fe C10 C6 164.5(4) . . . . ? C4 Fe C10 C6 -124.3(2) . . . . ? C1 Fe C10 C6 -54.9(5) . . . . ? C5 Fe C10 C6 -84.5(2) . . . . ? C8 Fe C10 C6 81.23(18) . . . . ? C9 Fe C10 C6 118.4(2) . . . . ? C7 Fe C10 C6 36.89(17) . . . . ? C3 Fe C10 C9 76.6(3) . . . . ? C2 Fe C10 C9 46.1(5) . . . . ? C4 Fe C10 C9 117.3(2) . . . . ? C1 Fe C10 C9 -173.3(4) . . . . ? C5 Fe C10 C9 157.1(2) . . . . ? C8 Fe C10 C9 -37.17(17) . . . . ? C6 Fe C10 C9 -118.4(2) . . . . ? C7 Fe C10 C9 -81.51(18) . . . . ? C6 C7 C11 N12 167.2(3) . . . . ? C8 C7 C11 N12 -8.9(5) . . . . ? Fe C7 C11 N12 -102.2(3) . . . . ? C7 C11 N12 C13 -176.4(2) . . . . ? C11 N12 C13 C18 -80.0(3) . . . . ? C11 N12 C13 C14 102.9(3) . . . . ? C18 C13 C14 C15 2.4(4) . . . . ? N12 C13 C14 C15 179.5(3) . . . . ? C18 C13 C14 C141 -177.5(3) . . . . ? N12 C13 C14 C141 -0.3(4) . . . . ? C15 C14 C141 C143 -55.6(5) . . . . ? C13 C14 C141 C143 124.2(4) . . . . ? C15 C14 C141 C142 68.6(4) . . . . ? C13 C14 C141 C142 -111.5(4) . . . . ? C13 C14 C15 C16 -1.7(5) . . . . ? C141 C14 C15 C16 178.2(3) . . . . ? C14 C15 C16 C17 0.0(6) . . . . ? C15 C16 C17 C18 0.9(6) . . . . ? C14 C13 C18 C17 -1.5(4) . . . . ? N12 C13 C18 C17 -178.5(3) . . . . ? C14 C13 C18 C181 178.8(3) . . . . ? N12 C13 C18 C181 1.8(4) . . . . ? C16 C17 C18 C13 -0.2(5) . . . . ? C16 C17 C18 C181 179.5(3) . . . . ? C13 C18 C181 C183 -130.4(3) . . . . ? C17 C18 C181 C183 49.9(4) . . . . ? C13 C18 C181 C182 104.1(3) . . . . ? C17 C18 C181 C182 -75.6(4) . . . . ? C10 C6 O1 Si1 40.8(4) . . . . ? C7 C6 O1 Si1 -136.4(2) . . . . ? Fe C6 O1 Si1 134.78(17) . . . . ? C6 O1 Si1 C31 36.6(2) . . . . ? C6 O1 Si1 C21 -85.4(2) . . . . ? C6 O1 Si1 C41 156.4(2) . . . . ? O1 Si1 C21 C22 -5.4(3) . . . . ? C31 Si1 C21 C22 -123.1(2) . . . . ? C41 Si1 C21 C22 107.9(2) . . . . ? O1 Si1 C21 C26 176.9(2) . . . . ? C31 Si1 C21 C26 59.3(3) . . . . ? C41 Si1 C21 C26 -69.7(3) . . . . ? C26 C21 C22 C23 -0.1(4) . . . . ? Si1 C21 C22 C23 -177.9(3) . . . . ? C21 C22 C23 C24 1.3(5) . . . . ? C22 C23 C24 C25 -1.7(5) . . . . ? C23 C24 C25 C26 0.9(5) . . . . ? C24 C25 C26 C21 0.3(4) . . . . ? C22 C21 C26 C25 -0.7(4) . . . . ? Si1 C21 C26 C25 177.0(2) . . . . ? O1 Si1 C31 C32 -141.2(2) . . . . ? C21 Si1 C31 C32 -23.5(3) . . . . ? C41 Si1 C31 C32 104.8(3) . . . . ? O1 Si1 C31 C36 37.2(3) . . . . ? C21 Si1 C31 C36 154.8(2) . . . . ? C41 Si1 C31 C36 -76.8(3) . . . . ? C36 C31 C32 C33 -0.2(5) . . . . ? Si1 C31 C32 C33 178.2(3) . . . . ? C31 C32 C33 C34 -1.2(5) . . . . ? C32 C33 C34 C35 2.5(5) . . . . ? C33 C34 C35 C36 -2.4(5) . . . . ? C34 C35 C36 C31 1.0(5) . . . . ? C32 C31 C36 C35 0.3(4) . . . . ? Si1 C31 C36 C35 -178.2(2) . . . . ? O1 Si1 C41 C43 64.2(3) . . . . ? C31 Si1 C41 C43 179.8(2) . . . . ? C21 Si1 C41 C43 -50.7(3) . . . . ? O1 Si1 C41 C44 -56.3(3) . . . . ? C31 Si1 C41 C44 59.3(3) . . . . ? C21 Si1 C41 C44 -171.2(2) . . . . ? O1 Si1 C41 C42 -176.1(2) . . . . ? C31 Si1 C41 C42 -60.5(3) . . . . ? C21 Si1 C41 C42 69.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.254 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.043 # Attachment 'pR2a.cif' data_erk4345 _database_code_depnum_ccdc_archive 'CCDC 714364' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H27 Fe N O' _chemical_formula_weight 389.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.0629(1) _cell_length_b 16.3389(3) _cell_length_c 20.3700(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2017.88(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3874 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7514 _exptl_absorpt_correction_T_max 0.9631 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13523 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.86 _reflns_number_total 4672 _reflns_number_gt 3317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0448P)^2^+0.0177P] 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 riding _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 0.010(19) _refine_ls_number_reflns 4672 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Fe Fe 0.86224(6) 0.20856(3) 0.845164(17) 0.03694(12) Uani 1 1 d . . . C1 C 0.8653(5) 0.17151(17) 0.94154(11) 0.0327(6) Uani 1 1 d . . . C2 C 1.0883(4) 0.18045(18) 0.91854(13) 0.0368(7) Uani 1 1 d . . . O1 O 1.2418(3) 0.12017(14) 0.91995(11) 0.0474(6) Uani 1 1 d . . . H1 H 1.1855 0.0776 0.9347 0.071 Uiso 1 1 calc R . . C3 C 1.1194(5) 0.26056(19) 0.89622(13) 0.0419(7) Uani 1 1 d . . . H3 H 1.2490 0.2819 0.8776 0.050 Uiso 1 1 calc R . . C4 C 0.9188(5) 0.3039(2) 0.90684(13) 0.0464(8) Uani 1 1 d . . . H4 H 0.8949 0.3594 0.8971 0.056 Uiso 1 1 calc R . . C5 C 0.7622(5) 0.2504(2) 0.93409(13) 0.0411(8) Uani 1 1 d . . . H5 H 0.6163 0.2637 0.9454 0.049 Uiso 1 1 calc R . . C6 C 0.7779(4) 0.09601(19) 0.96771(13) 0.0370(7) Uani 1 1 d . . . H6 H 0.6292 0.0928 0.9805 0.044 Uiso 1 1 calc R . . N1 N 0.9037(4) 0.03345(16) 0.97339(11) 0.0409(6) Uani 1 1 d . . . C7 C 0.8194(5) -0.04042(19) 1.00174(14) 0.0418(7) Uani 1 1 d . . . C8 C 0.8874(5) -0.0604(2) 1.06546(14) 0.0465(7) Uani 1 1 d . . . C9 C 0.8091(5) -0.1326(2) 1.09277(18) 0.0581(10) Uani 1 1 d . . . H9 H 0.8515 -0.1469 1.1357 0.070 Uiso 1 1 calc R . . C10 C 0.6715(6) -0.1835(2) 1.0585(2) 0.0669(10) Uani 1 1 d . . . H10 H 0.6168 -0.2313 1.0783 0.080 Uiso 1 1 calc R . . C11 C 0.6136(6) -0.1644(2) 0.99517(19) 0.0684(10) Uani 1 1 d . . . H11 H 0.5235 -0.2009 0.9716 0.082 Uiso 1 1 calc R . . C12 C 0.6840(5) -0.0929(2) 0.96485(17) 0.0538(9) Uani 1 1 d . . . C13 C 1.0393(5) -0.0044(2) 1.10339(15) 0.0522(9) Uani 1 1 d . . . H13 H 1.1012 0.0359 1.0721 0.063 Uiso 1 1 calc R . . C14 C 0.9124(7) 0.0425(3) 1.1551(2) 0.0901(13) Uani 1 1 d . . . H14A H 0.8482 0.0043 1.1862 0.135 Uiso 1 1 calc R . . H14B H 0.7960 0.0739 1.1343 0.135 Uiso 1 1 calc R . . H14C H 1.0116 0.0793 1.1780 0.135 Uiso 1 1 calc R . . C15 C 1.2303(7) -0.0484(3) 1.1355(3) 0.116(2) Uani 1 1 d . . . H15A H 1.3294 -0.0689 1.1019 0.174 Uiso 1 1 calc R . . H15B H 1.1749 -0.0938 1.1613 0.174 Uiso 1 1 calc R . . H15C H 1.3092 -0.0107 1.1638 0.174 Uiso 1 1 calc R . . C16 C 0.6220(8) -0.0740(2) 0.89390(18) 0.0729(11) Uani 1 1 d . . . H16 H 0.6605 -0.0162 0.8851 0.088 Uiso 1 1 calc R . . C17 C 0.7562(8) -0.1273(5) 0.8472(2) 0.146(3) Uani 1 1 d . . . H17A H 0.7350 -0.1845 0.8584 0.219 Uiso 1 1 calc R . . H17B H 0.9112 -0.1135 0.8511 0.219 Uiso 1 1 calc R . . H17C H 0.7077 -0.1179 0.8025 0.219 Uiso 1 1 calc R . . C18 C 0.3800(7) -0.0850(3) 0.8792(2) 0.0893(14) Uani 1 1 d . . . H18A H 0.2931 -0.0609 0.9142 0.134 Uiso 1 1 calc R . . H18B H 0.3465 -0.1429 0.8759 0.134 Uiso 1 1 calc R . . H18C H 0.3447 -0.0583 0.8380 0.134 Uiso 1 1 calc R . . C21 C 0.8637(8) 0.1180(2) 0.77722(15) 0.0674(10) Uani 1 1 d . . . H21 H 0.9295 0.0663 0.7824 0.081 Uiso 1 1 calc R . . C22 C 0.6475(8) 0.1391(3) 0.79363(14) 0.0691(12) Uani 1 1 d . . . H22 H 0.5417 0.1042 0.8124 0.083 Uiso 1 1 calc R . . C23 C 0.6159(6) 0.2211(3) 0.77721(14) 0.0663(11) Uani 1 1 d . . . H23 H 0.4846 0.2510 0.7825 0.080 Uiso 1 1 calc R . . C24 C 0.8117(6) 0.2508(3) 0.75187(15) 0.0641(11) Uani 1 1 d . . . H24 H 0.8368 0.3045 0.7373 0.077 Uiso 1 1 calc R . . C25 C 0.9639(6) 0.1880(3) 0.75161(15) 0.0657(12) Uani 1 1 d . . . H25 H 1.1103 0.1918 0.7367 0.079 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 Fe 0.0367(2) 0.0485(2) 0.02562(17) -0.0027(2) -0.00033(17) 0.0024(2) C1 0.0354(13) 0.0418(16) 0.0210(11) -0.0048(12) -0.0004(12) 0.0010(15) C2 0.0343(15) 0.0455(18) 0.0306(14) -0.0012(14) -0.0037(11) 0.0023(12) O1 0.0346(10) 0.0489(15) 0.0586(14) 0.0041(13) 0.0009(9) 0.0059(10) C3 0.0387(15) 0.0476(19) 0.0395(15) -0.0027(14) 0.0000(14) -0.0067(15) C4 0.063(2) 0.042(2) 0.0343(15) -0.0019(15) -0.0082(13) 0.0002(15) C5 0.0424(16) 0.053(2) 0.0284(15) -0.0070(15) 0.0018(12) 0.0090(14) C6 0.0298(14) 0.054(2) 0.0268(14) -0.0042(14) -0.0021(11) -0.0021(14) N1 0.0382(14) 0.0495(16) 0.0351(13) 0.0018(12) 0.0008(10) -0.0023(12) C7 0.0377(17) 0.0448(19) 0.0429(17) -0.0011(15) 0.0051(13) -0.0015(13) C8 0.0429(17) 0.051(2) 0.0452(16) 0.0076(15) 0.0089(15) 0.0021(16) C9 0.055(2) 0.061(3) 0.059(2) 0.013(2) 0.0092(16) 0.0037(18) C10 0.071(2) 0.051(2) 0.079(3) 0.013(2) 0.019(2) 0.000(2) C11 0.069(2) 0.050(2) 0.087(3) -0.008(2) 0.006(2) -0.015(2) C12 0.050(2) 0.054(2) 0.058(2) -0.0001(18) 0.0013(15) -0.0098(16) C13 0.056(2) 0.062(3) 0.0387(17) 0.0092(18) -0.0031(14) -0.0031(16) C14 0.090(3) 0.064(3) 0.117(4) -0.022(3) 0.009(3) -0.006(2) C15 0.075(3) 0.124(4) 0.148(5) -0.024(4) -0.049(3) 0.033(3) C16 0.091(3) 0.067(3) 0.060(2) -0.005(2) -0.022(2) -0.027(2) C17 0.085(3) 0.300(9) 0.053(3) -0.019(4) -0.004(2) 0.064(4) C18 0.080(3) 0.094(3) 0.094(3) -0.016(3) -0.022(3) 0.030(3) C21 0.105(3) 0.056(2) 0.0408(18) -0.0207(18) -0.016(2) 0.015(3) C22 0.077(3) 0.100(3) 0.0298(16) -0.005(2) -0.0034(19) -0.038(3) C23 0.055(2) 0.104(4) 0.0398(17) -0.009(2) -0.0157(16) 0.014(2) C24 0.092(3) 0.073(3) 0.0275(16) 0.0069(18) -0.0097(17) 0.000(2) C25 0.055(2) 0.110(4) 0.0324(17) -0.020(2) 0.0064(14) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C22 2.021(3) . ? Fe C21 2.027(3) . ? Fe C4 2.030(3) . ? Fe C5 2.029(3) . ? Fe C25 2.031(3) . ? Fe C24 2.045(3) . ? Fe C23 2.047(3) . ? Fe C1 2.054(2) . ? Fe C3 2.058(3) . ? Fe C2 2.079(3) . ? C1 C2 1.438(4) . ? C1 C5 1.441(4) . ? C1 C6 1.445(4) . ? C2 O1 1.356(3) . ? C2 C3 1.398(4) . ? C3 C4 1.424(4) . ? C4 C5 1.404(4) . ? C6 N1 1.280(4) . ? N1 C7 1.432(4) . ? C7 C8 1.401(4) . ? C7 C12 1.406(4) . ? C8 C9 1.388(4) . ? C8 C13 1.512(4) . ? C9 C10 1.368(5) . ? C10 C11 1.374(5) . ? C11 C12 1.388(5) . ? C12 C16 1.525(5) . ? C13 C15 1.512(5) . ? C13 C14 1.512(5) . ? C16 C18 1.509(6) . ? C16 C17 1.524(6) . ? C21 C25 1.397(5) . ? C21 C22 1.396(6) . ? C22 C23 1.394(5) . ? C23 C24 1.382(5) . ? C24 C25 1.379(5) . ? 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 C22 Fe C21 40.35(17) . . ? C22 Fe C4 149.42(16) . . ? C21 Fe C4 169.20(17) . . ? C22 Fe C5 117.41(15) . . ? C21 Fe C5 149.01(16) . . ? C4 Fe C5 40.47(12) . . ? C22 Fe C25 67.39(14) . . ? C21 Fe C25 40.29(14) . . ? C4 Fe C25 131.01(15) . . ? C5 Fe C25 169.79(17) . . ? C22 Fe C24 67.05(15) . . ? C21 Fe C24 67.18(16) . . ? C4 Fe C24 110.00(14) . . ? C5 Fe C24 132.17(14) . . ? C25 Fe C24 39.56(15) . . ? C22 Fe C23 40.08(15) . . ? C21 Fe C23 67.32(16) . . ? C4 Fe C23 117.71(14) . . ? C5 Fe C23 110.61(13) . . ? C25 Fe C23 66.63(14) . . ? C24 Fe C23 39.48(14) . . ? C22 Fe C1 109.67(13) . . ? C21 Fe C1 115.94(14) . . ? C4 Fe C1 68.47(11) . . ? C5 Fe C1 41.32(12) . . ? C25 Fe C1 147.70(15) . . ? C24 Fe C1 171.44(15) . . ? C23 Fe C1 133.04(14) . . ? C22 Fe C3 169.24(17) . . ? C21 Fe C3 130.06(16) . . ? C4 Fe C3 40.76(12) . . ? C5 Fe C3 68.65(12) . . ? C25 Fe C3 108.21(13) . . ? C24 Fe C3 116.37(14) . . ? C23 Fe C3 148.58(15) . . ? C1 Fe C3 68.39(12) . . ? C22 Fe C2 132.37(15) . . ? C21 Fe C2 109.07(14) . . ? C4 Fe C2 67.25(11) . . ? C5 Fe C2 68.26(11) . . ? C25 Fe C2 115.97(13) . . ? C24 Fe C2 147.29(14) . . ? C23 Fe C2 171.62(15) . . ? C1 Fe C2 40.71(11) . . ? C3 Fe C2 39.51(11) . . ? C2 C1 C5 106.4(2) . . ? C2 C1 C6 123.5(3) . . ? C5 C1 C6 130.1(3) . . ? C2 C1 Fe 70.57(15) . . ? C5 C1 Fe 68.39(14) . . ? C6 C1 Fe 126.93(18) . . ? O1 C2 C3 126.5(2) . . ? O1 C2 C1 124.4(3) . . ? C3 C2 C1 109.1(2) . . ? O1 C2 Fe 128.9(2) . . ? C3 C2 Fe 69.41(17) . . ? C1 C2 Fe 68.72(14) . . ? C2 C3 C4 107.5(3) . . ? C2 C3 Fe 71.08(17) . . ? C4 C3 Fe 68.57(16) . . ? C5 C4 C3 109.2(3) . . ? C5 C4 Fe 69.73(17) . . ? C3 C4 Fe 70.67(17) . . ? C4 C5 C1 107.8(2) . . ? C4 C5 Fe 69.80(16) . . ? C1 C5 Fe 70.29(15) . . ? N1 C6 C1 119.8(3) . . ? C6 N1 C7 119.8(2) . . ? C8 C7 C12 121.6(3) . . ? C8 C7 N1 117.8(3) . . ? C12 C7 N1 120.5(3) . . ? C9 C8 C7 118.0(3) . . ? C9 C8 C13 121.2(3) . . ? C7 C8 C13 120.8(3) . . ? C10 C9 C8 121.3(3) . . ? C9 C10 C11 119.8(4) . . ? C10 C11 C12 122.0(4) . . ? C11 C12 C7 117.1(3) . . ? C11 C12 C16 121.1(3) . . ? C7 C12 C16 121.8(3) . . ? C15 C13 C8 113.5(3) . . ? C15 C13 C14 109.2(3) . . ? C8 C13 C14 110.6(3) . . ? C18 C16 C17 109.1(4) . . ? C18 C16 C12 113.8(4) . . ? C17 C16 C12 110.1(4) . . ? C25 C21 C22 107.2(4) . . ? C25 C21 Fe 70.02(19) . . ? C22 C21 Fe 69.6(2) . . ? C23 C22 C21 108.0(3) . . ? C23 C22 Fe 70.9(2) . . ? C21 C22 Fe 70.0(2) . . ? C24 C23 C22 108.0(4) . . ? C24 C23 Fe 70.18(18) . . ? C22 C23 Fe 69.0(2) . . ? C25 C24 C23 108.4(4) . . ? C25 C24 Fe 69.68(19) . . ? C23 C24 Fe 70.33(18) . . ? C24 C25 C21 108.4(3) . . ? C24 C25 Fe 70.76(19) . . ? C21 C25 Fe 69.69(18) . . ? 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 C22 Fe C1 C2 133.0(2) . . . . ? C21 Fe C1 C2 89.5(2) . . . . ? C4 Fe C1 C2 -79.69(17) . . . . ? C5 Fe C1 C2 -117.5(2) . . . . ? C25 Fe C1 C2 54.4(3) . . . . ? C23 Fe C1 C2 171.9(2) . . . . ? C3 Fe C1 C2 -35.71(16) . . . . ? C22 Fe C1 C5 -109.5(2) . . . . ? C21 Fe C1 C5 -152.9(2) . . . . ? C4 Fe C1 C5 37.83(17) . . . . ? C25 Fe C1 C5 171.9(3) . . . . ? C23 Fe C1 C5 -70.6(2) . . . . ? C3 Fe C1 C5 81.81(18) . . . . ? C2 Fe C1 C5 117.5(2) . . . . ? C22 Fe C1 C6 15.1(3) . . . . ? C21 Fe C1 C6 -28.3(3) . . . . ? C4 Fe C1 C6 162.5(3) . . . . ? C5 Fe C1 C6 124.6(3) . . . . ? C25 Fe C1 C6 -63.4(4) . . . . ? C23 Fe C1 C6 54.1(3) . . . . ? C3 Fe C1 C6 -153.5(3) . . . . ? C2 Fe C1 C6 -117.8(3) . . . . ? C5 C1 C2 O1 177.3(2) . . . . ? C6 C1 C2 O1 -1.4(4) . . . . ? Fe C1 C2 O1 -123.4(3) . . . . ? C5 C1 C2 C3 -1.6(3) . . . . ? C6 C1 C2 C3 179.7(2) . . . . ? Fe C1 C2 C3 57.69(19) . . . . ? C5 C1 C2 Fe -59.26(17) . . . . ? C6 C1 C2 Fe 122.0(2) . . . . ? C22 Fe C2 O1 48.9(3) . . . . ? C21 Fe C2 O1 9.8(3) . . . . ? C4 Fe C2 O1 -159.4(3) . . . . ? C5 Fe C2 O1 156.8(3) . . . . ? C25 Fe C2 O1 -33.4(3) . . . . ? C24 Fe C2 O1 -67.5(4) . . . . ? C1 Fe C2 O1 117.7(3) . . . . ? C3 Fe C2 O1 -120.9(3) . . . . ? C22 Fe C2 C3 169.7(2) . . . . ? C21 Fe C2 C3 130.6(2) . . . . ? C4 Fe C2 C3 -38.51(17) . . . . ? C5 Fe C2 C3 -82.39(19) . . . . ? C25 Fe C2 C3 87.5(2) . . . . ? C24 Fe C2 C3 53.4(3) . . . . ? C1 Fe C2 C3 -121.5(2) . . . . ? C22 Fe C2 C1 -68.8(2) . . . . ? C21 Fe C2 C1 -107.9(2) . . . . ? C4 Fe C2 C1 82.95(17) . . . . ? C5 Fe C2 C1 39.08(17) . . . . ? C25 Fe C2 C1 -151.09(19) . . . . ? C24 Fe C2 C1 174.9(3) . . . . ? C3 Fe C2 C1 121.5(2) . . . . ? O1 C2 C3 C4 -177.0(3) . . . . ? C1 C2 C3 C4 1.9(3) . . . . ? Fe C2 C3 C4 59.14(19) . . . . ? O1 C2 C3 Fe 123.9(3) . . . . ? C1 C2 C3 Fe -57.27(18) . . . . ? C22 Fe C3 C2 -44.9(7) . . . . ? C21 Fe C3 C2 -69.6(2) . . . . ? C4 Fe C3 C2 118.4(2) . . . . ? C5 Fe C3 C2 81.32(18) . . . . ? C25 Fe C3 C2 -109.0(2) . . . . ? C24 Fe C3 C2 -151.04(18) . . . . ? C23 Fe C3 C2 176.2(2) . . . . ? C1 Fe C3 C2 36.75(16) . . . . ? C22 Fe C3 C4 -163.3(6) . . . . ? C21 Fe C3 C4 172.0(2) . . . . ? C5 Fe C3 C4 -37.10(18) . . . . ? C25 Fe C3 C4 132.6(2) . . . . ? C24 Fe C3 C4 90.5(2) . . . . ? C23 Fe C3 C4 57.8(3) . . . . ? C1 Fe C3 C4 -81.66(18) . . . . ? C2 Fe C3 C4 -118.4(2) . . . . ? C2 C3 C4 C5 -1.4(3) . . . . ? Fe C3 C4 C5 59.3(2) . . . . ? C2 C3 C4 Fe -60.7(2) . . . . ? C22 Fe C4 C5 53.9(3) . . . . ? C21 Fe C4 C5 -154.8(7) . . . . ? C25 Fe C4 C5 172.0(2) . . . . ? C24 Fe C4 C5 132.4(2) . . . . ? C23 Fe C4 C5 89.8(2) . . . . ? C1 Fe C4 C5 -38.60(16) . . . . ? C3 Fe C4 C5 -120.0(3) . . . . ? C2 Fe C4 C5 -82.69(18) . . . . ? C22 Fe C4 C3 174.0(3) . . . . ? C21 Fe C4 C3 -34.7(8) . . . . ? C5 Fe C4 C3 120.0(3) . . . . ? C25 Fe C4 C3 -68.0(2) . . . . ? C24 Fe C4 C3 -107.6(2) . . . . ? C23 Fe C4 C3 -150.12(19) . . . . ? C1 Fe C4 C3 81.45(19) . . . . ? C2 Fe C4 C3 37.36(16) . . . . ? C3 C4 C5 C1 0.5(3) . . . . ? Fe C4 C5 C1 60.32(18) . . . . ? C3 C4 C5 Fe -59.9(2) . . . . ? C2 C1 C5 C4 0.7(3) . . . . ? C6 C1 C5 C4 179.2(3) . . . . ? Fe C1 C5 C4 -60.01(18) . . . . ? C2 C1 C5 Fe 60.68(17) . . . . ? C6 C1 C5 Fe -120.8(3) . . . . ? C22 Fe C5 C4 -152.4(2) . . . . ? C21 Fe C5 C4 171.1(3) . . . . ? C25 Fe C5 C4 -36.5(8) . . . . ? C24 Fe C5 C4 -69.5(2) . . . . ? C23 Fe C5 C4 -108.9(2) . . . . ? C1 Fe C5 C4 118.5(2) . . . . ? C3 Fe C5 C4 37.36(18) . . . . ? C2 Fe C5 C4 79.97(18) . . . . ? C22 Fe C5 C1 89.1(2) . . . . ? C21 Fe C5 C1 52.6(3) . . . . ? C4 Fe C5 C1 -118.5(2) . . . . ? C25 Fe C5 C1 -155.0(7) . . . . ? C24 Fe C5 C1 172.1(2) . . . . ? C23 Fe C5 C1 132.58(19) . . . . ? C3 Fe C5 C1 -81.13(17) . . . . ? C2 Fe C5 C1 -38.51(16) . . . . ? C2 C1 C6 N1 2.5(4) . . . . ? C5 C1 C6 N1 -175.9(3) . . . . ? Fe C1 C6 N1 92.4(3) . . . . ? C1 C6 N1 C7 177.5(2) . . . . ? C6 N1 C7 C8 -106.2(3) . . . . ? C6 N1 C7 C12 77.6(4) . . . . ? C12 C7 C8 C9 -2.8(4) . . . . ? N1 C7 C8 C9 -178.9(3) . . . . ? C12 C7 C8 C13 177.9(3) . . . . ? N1 C7 C8 C13 1.7(4) . . . . ? C7 C8 C9 C10 0.7(5) . . . . ? C13 C8 C9 C10 180.0(3) . . . . ? C8 C9 C10 C11 1.9(5) . . . . ? C9 C10 C11 C12 -2.4(6) . . . . ? C10 C11 C12 C7 0.4(5) . . . . ? C10 C11 C12 C16 178.5(4) . . . . ? C8 C7 C12 C11 2.3(5) . . . . ? N1 C7 C12 C11 178.3(3) . . . . ? C8 C7 C12 C16 -175.9(3) . . . . ? N1 C7 C12 C16 0.2(5) . . . . ? C9 C8 C13 C15 48.1(5) . . . . ? C7 C8 C13 C15 -132.6(3) . . . . ? C9 C8 C13 C14 -75.1(4) . . . . ? C7 C8 C13 C14 104.2(4) . . . . ? C11 C12 C16 C18 48.5(5) . . . . ? C7 C12 C16 C18 -133.4(4) . . . . ? C11 C12 C16 C17 -74.4(5) . . . . ? C7 C12 C16 C17 103.7(5) . . . . ? C22 Fe C21 C25 118.0(3) . . . . ? C4 Fe C21 C25 -39.8(9) . . . . ? C5 Fe C21 C25 172.7(2) . . . . ? C24 Fe C21 C25 37.1(2) . . . . ? C23 Fe C21 C25 80.1(2) . . . . ? C1 Fe C21 C25 -151.6(2) . . . . ? C3 Fe C21 C25 -68.9(3) . . . . ? C2 Fe C21 C25 -108.0(2) . . . . ? C4 Fe C21 C22 -157.8(7) . . . . ? C5 Fe C21 C22 54.7(4) . . . . ? C25 Fe C21 C22 -118.0(3) . . . . ? C24 Fe C21 C22 -80.9(2) . . . . ? C23 Fe C21 C22 -37.9(2) . . . . ? C1 Fe C21 C22 90.3(2) . . . . ? C3 Fe C21 C22 173.1(2) . . . . ? C2 Fe C21 C22 134.0(2) . . . . ? C25 C21 C22 C23 0.8(3) . . . . ? Fe C21 C22 C23 61.1(2) . . . . ? C25 C21 C22 Fe -60.2(2) . . . . ? C21 Fe C22 C23 -118.3(3) . . . . ? C4 Fe C22 C23 53.8(3) . . . . ? C5 Fe C22 C23 90.0(2) . . . . ? C25 Fe C22 C23 -80.1(2) . . . . ? C24 Fe C22 C23 -37.0(2) . . . . ? C1 Fe C22 C23 134.5(2) . . . . ? C3 Fe C22 C23 -147.8(6) . . . . ? C2 Fe C22 C23 174.72(19) . . . . ? C4 Fe C22 C21 172.0(3) . . . . ? C5 Fe C22 C21 -151.8(2) . . . . ? C25 Fe C22 C21 38.2(2) . . . . ? C24 Fe C22 C21 81.2(2) . . . . ? C23 Fe C22 C21 118.3(3) . . . . ? C1 Fe C22 C21 -107.2(2) . . . . ? C3 Fe C22 C21 -29.6(8) . . . . ? C2 Fe C22 C21 -67.0(2) . . . . ? C21 C22 C23 C24 -0.9(4) . . . . ? Fe C22 C23 C24 59.6(2) . . . . ? C21 C22 C23 Fe -60.5(2) . . . . ? C22 Fe C23 C24 -119.3(3) . . . . ? C21 Fe C23 C24 -81.2(3) . . . . ? C4 Fe C23 C24 88.3(2) . . . . ? C5 Fe C23 C24 132.2(2) . . . . ? C25 Fe C23 C24 -37.2(2) . . . . ? C1 Fe C23 C24 173.9(2) . . . . ? C3 Fe C23 C24 49.7(4) . . . . ? C21 Fe C23 C22 38.2(2) . . . . ? C4 Fe C23 C22 -152.4(2) . . . . ? C5 Fe C23 C22 -108.5(2) . . . . ? C25 Fe C23 C22 82.1(2) . . . . ? C24 Fe C23 C22 119.3(3) . . . . ? C1 Fe C23 C22 -66.8(3) . . . . ? C3 Fe C23 C22 169.0(2) . . . . ? C22 C23 C24 C25 0.7(4) . . . . ? Fe C23 C24 C25 59.5(2) . . . . ? C22 C23 C24 Fe -58.8(2) . . . . ? C22 Fe C24 C25 -81.8(3) . . . . ? C21 Fe C24 C25 -37.8(2) . . . . ? C4 Fe C24 C25 131.0(2) . . . . ? C5 Fe C24 C25 171.3(2) . . . . ? C23 Fe C24 C25 -119.3(3) . . . . ? C3 Fe C24 C25 87.0(3) . . . . ? C2 Fe C24 C25 52.2(4) . . . . ? C22 Fe C24 C23 37.6(2) . . . . ? C21 Fe C24 C23 81.5(3) . . . . ? C4 Fe C24 C23 -109.7(2) . . . . ? C5 Fe C24 C23 -69.4(3) . . . . ? C25 Fe C24 C23 119.3(3) . . . . ? C3 Fe C24 C23 -153.7(2) . . . . ? C2 Fe C24 C23 171.6(2) . . . . ? C23 C24 C25 C21 -0.1(4) . . . . ? Fe C24 C25 C21 59.7(2) . . . . ? C23 C24 C25 Fe -59.9(2) . . . . ? C22 C21 C25 C24 -0.4(4) . . . . ? Fe C21 C25 C24 -60.4(2) . . . . ? C22 C21 C25 Fe 60.0(2) . . . . ? C22 Fe C25 C24 80.8(3) . . . . ? C21 Fe C25 C24 119.1(3) . . . . ? C4 Fe C25 C24 -70.0(3) . . . . ? C5 Fe C25 C24 -39.2(8) . . . . ? C23 Fe C25 C24 37.1(2) . . . . ? C1 Fe C25 C24 172.2(2) . . . . ? C3 Fe C25 C24 -109.6(2) . . . . ? C2 Fe C25 C24 -151.6(2) . . . . ? C22 Fe C25 C21 -38.2(3) . . . . ? C4 Fe C25 C21 170.9(2) . . . . ? C5 Fe C25 C21 -158.3(7) . . . . ? C24 Fe C25 C21 -119.1(3) . . . . ? C23 Fe C25 C21 -81.9(3) . . . . ? C1 Fe C25 C21 53.1(4) . . . . ? C3 Fe C25 C21 131.3(2) . . . . ? C2 Fe C25 C21 89.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.197 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.053 # Attachment 'pS12.cif' data_erk3660 _database_code_depnum_ccdc_archive 'CCDC 714365' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H28 Fe O2 Si' _chemical_formula_weight 468.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.155(1) _cell_length_b 13.060(1) _cell_length_c 17.630(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2338.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 4363 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8410 _exptl_absorpt_correction_T_max 0.8698 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11052 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.92 _reflns_number_total 4550 _reflns_number_gt 3805 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.v., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0197P)^2^+0.7249P] 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 riding _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 -0.027(14) _refine_ls_number_reflns 4550 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Fe Fe 0.33492(4) 0.55043(3) 0.764199(19) 0.02855(10) Uani 1 1 d . . . Si1 Si -0.07520(7) 0.54371(6) 0.86233(4) 0.02546(16) Uani 1 1 d . . . O1 O 0.4487(2) 0.50687(17) 0.97037(12) 0.0560(6) Uani 1 1 d . . . O2 O 0.08563(18) 0.51863(13) 0.85800(10) 0.0336(4) Uani 1 1 d . . . C1 C 0.4123(3) 0.4066(2) 0.75302(18) 0.0463(8) Uani 1 1 d . . . H1 H 0.4353 0.3615 0.7932 0.056 Uiso 1 1 calc R . . C2 C 0.4979(3) 0.4790(2) 0.71835(16) 0.0427(8) Uani 1 1 d . . . H2 H 0.5874 0.4910 0.7311 0.051 Uiso 1 1 calc R . . C3 C 0.4249(3) 0.5296(2) 0.66141(16) 0.0447(8) Uani 1 1 d . . . H3 H 0.4567 0.5822 0.6291 0.054 Uiso 1 1 calc R . . C4 C 0.2957(3) 0.4882(2) 0.66089(16) 0.0449(8) Uani 1 1 d . . . H4 H 0.2264 0.5078 0.6277 0.054 Uiso 1 1 calc R . . C5 C 0.2877(3) 0.4128(2) 0.71805(19) 0.0468(8) Uani 1 1 d . . . H5 H 0.2122 0.3735 0.7307 0.056 Uiso 1 1 calc R . . C6 C 0.1860(3) 0.58219(19) 0.83790(14) 0.0295(6) Uani 1 1 d . . . C7 C 0.3101(3) 0.58212(19) 0.87668(13) 0.0293(6) Uani 1 1 d . . . C8 C 0.3914(3) 0.6586(2) 0.84128(16) 0.0367(7) Uani 1 1 d . . . H8 H 0.4795 0.6751 0.8546 0.044 Uiso 1 1 calc R . . C9 C 0.3164(3) 0.70465(19) 0.78318(16) 0.0392(7) Uani 1 1 d . . . H9 H 0.3457 0.7587 0.7513 0.047 Uiso 1 1 calc R . . C10 C 0.1898(3) 0.65740(19) 0.77969(15) 0.0344(7) Uani 1 1 d . . . H10 H 0.1211 0.6732 0.7450 0.041 Uiso 1 1 calc R . . C11 C 0.3459(3) 0.5075(2) 0.93471(15) 0.0413(7) Uani 1 1 d . . . H11 H 0.2839 0.4551 0.9456 0.050 Uiso 1 1 calc R . . C21 C -0.1445(3) 0.41778(19) 0.89416(13) 0.0280(6) Uani 1 1 d . . . C22 C -0.2801(3) 0.4020(2) 0.89377(14) 0.0341(7) Uani 1 1 d . . . H22 H -0.3365 0.4554 0.8770 0.041 Uiso 1 1 calc R . . C23 C -0.3346(3) 0.3101(2) 0.91722(14) 0.0394(7) Uani 1 1 d . . . H23 H -0.4274 0.3013 0.9172 0.047 Uiso 1 1 calc R . . C24 C -0.2534(3) 0.2310(2) 0.94068(17) 0.0438(8) Uani 1 1 d . . . H24 H -0.2904 0.1680 0.9572 0.053 Uiso 1 1 calc R . . C25 C -0.1197(4) 0.2440(2) 0.93993(19) 0.0472(9) Uani 1 1 d . . . H25 H -0.0639 0.1894 0.9553 0.057 Uiso 1 1 calc R . . C26 C -0.0648(3) 0.3364(2) 0.91695(17) 0.0408(7) Uani 1 1 d . . . H26 H 0.0282 0.3443 0.9168 0.049 Uiso 1 1 calc R . . C31 C -0.1340(2) 0.56858(18) 0.76359(14) 0.0290(6) Uani 1 1 d . . . C32 C -0.0990(3) 0.4970(3) 0.70833(16) 0.0499(9) Uani 1 1 d . . . H32 H -0.0490 0.4387 0.7226 0.060 Uiso 1 1 calc R . . C33 C -0.1355(4) 0.5091(3) 0.63306(18) 0.0584(10) Uani 1 1 d . . . H33 H -0.1101 0.4595 0.5964 0.070 Uiso 1 1 calc R . . C34 C -0.2082(4) 0.5925(3) 0.61174(17) 0.0545(10) Uani 1 1 d . . . H34 H -0.2333 0.6010 0.5602 0.065 Uiso 1 1 calc R . . C35 C -0.2447(4) 0.6635(3) 0.66455(18) 0.0579(10) Uani 1 1 d . . . H35 H -0.2949 0.7215 0.6497 0.070 Uiso 1 1 calc R . . C36 C -0.2086(3) 0.6512(2) 0.73993(17) 0.0441(8) Uani 1 1 d . . . H36 H -0.2359 0.7007 0.7762 0.053 Uiso 1 1 calc R . . C41 C -0.1034(3) 0.6494(2) 0.93432(15) 0.0310(6) Uani 1 1 d . . . C42 C -0.2512(3) 0.6699(3) 0.94743(19) 0.0505(9) Uani 1 1 d . . . H42A H -0.2619 0.7172 0.9902 0.076 Uiso 1 1 calc R . . H42B H -0.2961 0.6053 0.9588 0.076 Uiso 1 1 calc R . . H42C H -0.2895 0.7004 0.9017 0.076 Uiso 1 1 calc R . . C43 C -0.0367(3) 0.7502(2) 0.91151(17) 0.0398(7) Uani 1 1 d . . . H43A H -0.0736 0.7743 0.8634 0.060 Uiso 1 1 calc R . . H43B H 0.0582 0.7389 0.9056 0.060 Uiso 1 1 calc R . . H43C H -0.0519 0.8017 0.9510 0.060 Uiso 1 1 calc R . . C44 C -0.0421(4) 0.6118(3) 1.00965(16) 0.0536(9) Uani 1 1 d . . . H44A H -0.0542 0.6642 1.0488 0.080 Uiso 1 1 calc R . . H44B H 0.0522 0.5992 1.0023 0.080 Uiso 1 1 calc R . . H44C H -0.0853 0.5482 1.0255 0.080 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 Fe 0.0254(2) 0.02971(18) 0.03055(18) -0.00057(17) 0.00301(16) 0.00002(17) Si1 0.0222(4) 0.0298(4) 0.0244(3) 0.0014(3) -0.0002(3) -0.0007(3) O1 0.0460(17) 0.0741(16) 0.0479(13) 0.0022(12) -0.0162(11) 0.0061(11) O2 0.0188(12) 0.0393(11) 0.0429(11) 0.0099(8) 0.0039(8) -0.0004(8) C1 0.053(2) 0.0341(15) 0.052(2) -0.0019(14) 0.0064(16) 0.0161(14) C2 0.030(2) 0.051(2) 0.0468(18) -0.0038(13) 0.0072(13) 0.0078(13) C3 0.047(2) 0.053(2) 0.0343(16) -0.0033(14) 0.0107(13) 0.0070(15) C4 0.050(2) 0.0491(19) 0.0353(16) -0.0145(14) -0.0078(13) 0.0060(14) C5 0.046(2) 0.0345(16) 0.060(2) -0.0141(15) -0.0025(15) 0.0002(13) C6 0.0260(18) 0.0326(15) 0.0299(13) 0.0005(10) 0.0067(11) 0.0009(11) C7 0.0243(18) 0.0390(15) 0.0248(13) -0.0029(10) 0.0037(10) -0.0016(11) C8 0.0303(18) 0.0393(17) 0.0405(17) -0.0087(13) 0.0021(12) -0.0064(13) C9 0.047(2) 0.0230(14) 0.0480(18) -0.0009(12) 0.0115(14) -0.0036(12) C10 0.0343(19) 0.0314(14) 0.0374(16) 0.0029(12) 0.0035(11) 0.0050(12) C11 0.038(2) 0.0545(18) 0.0314(15) 0.0012(13) -0.0036(14) 0.0021(15) C21 0.031(2) 0.0304(14) 0.0227(13) -0.0009(10) 0.0014(11) -0.0032(11) C22 0.033(2) 0.0382(16) 0.0313(15) 0.0051(12) -0.0008(11) -0.0021(12) C23 0.0360(19) 0.0474(17) 0.0348(15) 0.0009(12) -0.0014(14) -0.0132(15) C24 0.057(3) 0.0363(18) 0.0383(19) 0.0065(14) -0.0022(15) -0.0110(15) C25 0.052(3) 0.0336(17) 0.056(2) 0.0093(15) -0.0113(15) 0.0040(14) C26 0.033(2) 0.0383(17) 0.0511(19) 0.0048(14) -0.0021(14) 0.0027(14) C31 0.0277(17) 0.0341(15) 0.0251(12) 0.0013(12) 0.0000(10) -0.0035(10) C32 0.049(2) 0.065(2) 0.0357(17) -0.0104(15) -0.0064(14) 0.0167(16) C33 0.062(3) 0.077(2) 0.0356(18) -0.0189(17) 0.0016(15) 0.0076(19) C34 0.068(3) 0.069(2) 0.0261(16) 0.0084(16) -0.0051(15) -0.0155(18) C35 0.086(3) 0.043(2) 0.044(2) 0.0104(16) -0.0207(18) 0.0048(18) C36 0.064(2) 0.0315(15) 0.0367(16) 0.0001(13) -0.0127(15) 0.0012(13) C41 0.0321(18) 0.0362(16) 0.0249(14) 0.0000(11) 0.0029(11) 0.0007(12) C42 0.048(2) 0.053(2) 0.051(2) -0.0108(16) 0.0139(16) -0.0007(17) C43 0.040(2) 0.0355(17) 0.0441(18) -0.0058(13) -0.0036(13) -0.0019(13) C44 0.076(3) 0.053(2) 0.0317(17) -0.0040(15) -0.0127(15) -0.0021(17) _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 Fe C5 2.030(3) . ? Fe C4 2.034(3) . ? Fe C6 2.036(3) . ? Fe C7 2.041(2) . ? Fe C8 2.042(3) . ? Fe C1 2.046(3) . ? Fe C3 2.048(3) . ? Fe C10 2.049(3) . ? Fe C9 2.050(3) . ? Fe C2 2.065(3) . ? Si1 O2 1.668(2) . ? Si1 C31 1.869(3) . ? Si1 C21 1.875(3) . ? Si1 C41 1.897(3) . ? O1 C11 1.218(3) . ? O2 C6 1.362(3) . ? C1 C5 1.409(4) . ? C1 C2 1.422(4) . ? C2 C3 1.412(4) . ? C3 C4 1.419(4) . ? C4 C5 1.411(4) . ? C6 C10 1.421(3) . ? C6 C7 1.433(4) . ? C7 C8 1.438(4) . ? C7 C11 1.459(4) . ? C8 C9 1.411(4) . ? C9 C10 1.427(4) . ? C21 C22 1.393(4) . ? C21 C26 1.395(4) . ? C22 C23 1.385(4) . ? C23 C24 1.384(4) . ? C24 C25 1.369(5) . ? C25 C26 1.390(4) . ? C31 C36 1.383(4) . ? C31 C32 1.396(4) . ? C32 C33 1.387(4) . ? C33 C34 1.369(5) . ? C34 C35 1.366(5) . ? C35 C36 1.388(4) . ? C41 C43 1.534(4) . ? C41 C42 1.542(4) . ? C41 C44 1.547(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Fe C4 40.62(12) . . ? C5 Fe C6 105.12(12) . . ? C4 Fe C6 120.49(12) . . ? C5 Fe C7 122.66(12) . . ? C4 Fe C7 157.92(12) . . ? C6 Fe C7 41.16(10) . . ? C5 Fe C8 160.96(12) . . ? C4 Fe C8 158.02(12) . . ? C6 Fe C8 69.07(11) . . ? C7 Fe C8 41.24(10) . . ? C5 Fe C1 40.46(12) . . ? C4 Fe C1 67.78(13) . . ? C6 Fe C1 122.26(11) . . ? C7 Fe C1 109.10(12) . . ? C8 Fe C1 126.26(13) . . ? C5 Fe C3 68.46(13) . . ? C4 Fe C3 40.69(12) . . ? C6 Fe C3 157.38(12) . . ? C7 Fe C3 160.36(12) . . ? C8 Fe C3 123.76(13) . . ? C1 Fe C3 67.75(12) . . ? C5 Fe C10 119.17(12) . . ? C4 Fe C10 104.54(12) . . ? C6 Fe C10 40.71(10) . . ? C7 Fe C10 69.11(10) . . ? C8 Fe C10 68.99(12) . . ? C1 Fe C10 156.24(12) . . ? C3 Fe C10 121.97(11) . . ? C5 Fe C9 155.98(13) . . ? C4 Fe C9 121.39(12) . . ? C6 Fe C9 68.15(11) . . ? C7 Fe C9 68.35(11) . . ? C8 Fe C9 40.32(11) . . ? C1 Fe C9 162.35(14) . . ? C3 Fe C9 108.42(12) . . ? C10 Fe C9 40.76(12) . . ? C5 Fe C2 68.42(13) . . ? C4 Fe C2 68.03(13) . . ? C6 Fe C2 159.56(11) . . ? C7 Fe C2 124.81(11) . . ? C8 Fe C2 110.38(12) . . ? C1 Fe C2 40.49(12) . . ? C3 Fe C2 40.17(12) . . ? C10 Fe C2 159.52(11) . . ? C9 Fe C2 125.54(13) . . ? O2 Si1 C31 107.72(10) . . ? O2 Si1 C21 102.07(11) . . ? C31 Si1 C21 108.14(11) . . ? O2 Si1 C41 108.74(12) . . ? C31 Si1 C41 116.66(12) . . ? C21 Si1 C41 112.42(12) . . ? C6 O2 Si1 128.73(16) . . ? C5 C1 C2 108.8(3) . . ? C5 C1 Fe 69.17(16) . . ? C2 C1 Fe 70.48(16) . . ? C3 C2 C1 107.2(3) . . ? C3 C2 Fe 69.27(17) . . ? C1 C2 Fe 69.04(16) . . ? C2 C3 C4 108.2(3) . . ? C2 C3 Fe 70.56(17) . . ? C4 C3 Fe 69.14(16) . . ? C5 C4 C3 108.3(3) . . ? C5 C4 Fe 69.53(16) . . ? C3 C4 Fe 70.17(16) . . ? C1 C5 C4 107.6(3) . . ? C1 C5 Fe 70.37(17) . . ? C4 C5 Fe 69.85(17) . . ? O2 C6 C10 129.0(2) . . ? O2 C6 C7 122.2(2) . . ? C10 C6 C7 108.7(2) . . ? O2 C6 Fe 126.72(17) . . ? C10 C6 Fe 70.12(14) . . ? C7 C6 Fe 69.62(14) . . ? C6 C7 C8 107.3(2) . . ? C6 C7 C11 123.6(2) . . ? C8 C7 C11 128.7(3) . . ? C6 C7 Fe 69.22(13) . . ? C8 C7 Fe 69.42(14) . . ? C11 C7 Fe 121.01(18) . . ? C9 C8 C7 107.6(3) . . ? C9 C8 Fe 70.14(16) . . ? C7 C8 Fe 69.34(14) . . ? C8 C9 C10 109.4(3) . . ? C8 C9 Fe 69.54(15) . . ? C10 C9 Fe 69.56(15) . . ? C6 C10 C9 107.0(2) . . ? C6 C10 Fe 69.17(15) . . ? C9 C10 Fe 69.68(15) . . ? O1 C11 C7 125.4(3) . . ? C22 C21 C26 117.5(3) . . ? C22 C21 Si1 120.0(2) . . ? C26 C21 Si1 122.5(2) . . ? C23 C22 C21 121.5(3) . . ? C22 C23 C24 119.9(3) . . ? C25 C24 C23 119.7(3) . . ? C24 C25 C26 120.5(3) . . ? C25 C26 C21 120.9(3) . . ? C36 C31 C32 116.8(3) . . ? C36 C31 Si1 126.3(2) . . ? C32 C31 Si1 116.9(2) . . ? C33 C32 C31 121.6(3) . . ? C34 C33 C32 119.8(3) . . ? C35 C34 C33 120.0(3) . . ? C34 C35 C36 120.1(3) . . ? C31 C36 C35 121.6(3) . . ? C43 C41 C42 108.6(3) . . ? C43 C41 C44 108.6(3) . . ? C42 C41 C44 108.6(3) . . ? C43 C41 Si1 112.48(19) . . ? C42 C41 Si1 112.0(2) . . ? C44 C41 Si1 106.4(2) . . ? 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 C31 Si1 O2 C6 66.2(2) . . . . ? C21 Si1 O2 C6 180.0(2) . . . . ? C41 Si1 O2 C6 -61.1(2) . . . . ? C4 Fe C1 C5 -38.31(19) . . . . ? C6 Fe C1 C5 74.7(2) . . . . ? C7 Fe C1 C5 118.31(19) . . . . ? C8 Fe C1 C5 161.18(18) . . . . ? C3 Fe C1 C5 -82.4(2) . . . . ? C10 Fe C1 C5 36.9(4) . . . . ? C9 Fe C1 C5 -163.2(4) . . . . ? C2 Fe C1 C5 -120.0(3) . . . . ? C5 Fe C1 C2 120.0(3) . . . . ? C4 Fe C1 C2 81.7(2) . . . . ? C6 Fe C1 C2 -165.31(17) . . . . ? C7 Fe C1 C2 -121.67(18) . . . . ? C8 Fe C1 C2 -78.8(2) . . . . ? C3 Fe C1 C2 37.59(19) . . . . ? C10 Fe C1 C2 157.0(3) . . . . ? C9 Fe C1 C2 -43.2(5) . . . . ? C5 C1 C2 C3 -0.3(3) . . . . ? Fe C1 C2 C3 -59.0(2) . . . . ? C5 C1 C2 Fe 58.73(19) . . . . ? C5 Fe C2 C3 81.7(2) . . . . ? C4 Fe C2 C3 37.85(19) . . . . ? C6 Fe C2 C3 156.8(3) . . . . ? C7 Fe C2 C3 -162.67(18) . . . . ? C8 Fe C2 C3 -118.62(19) . . . . ? C1 Fe C2 C3 118.9(3) . . . . ? C10 Fe C2 C3 -34.3(4) . . . . ? C9 Fe C2 C3 -75.9(2) . . . . ? C5 Fe C2 C1 -37.17(19) . . . . ? C4 Fe C2 C1 -81.1(2) . . . . ? C6 Fe C2 C1 37.9(4) . . . . ? C7 Fe C2 C1 78.4(2) . . . . ? C8 Fe C2 C1 122.5(2) . . . . ? C3 Fe C2 C1 -118.9(3) . . . . ? C10 Fe C2 C1 -153.2(3) . . . . ? C9 Fe C2 C1 165.22(18) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? Fe C2 C3 C4 -59.1(2) . . . . ? C1 C2 C3 Fe 58.83(19) . . . . ? C5 Fe C3 C2 -81.6(2) . . . . ? C4 Fe C3 C2 -119.2(3) . . . . ? C6 Fe C3 C2 -159.0(3) . . . . ? C7 Fe C3 C2 46.7(4) . . . . ? C8 Fe C3 C2 81.8(2) . . . . ? C1 Fe C3 C2 -37.88(19) . . . . ? C10 Fe C3 C2 166.57(17) . . . . ? C9 Fe C3 C2 123.73(19) . . . . ? C5 Fe C3 C4 37.57(18) . . . . ? C6 Fe C3 C4 -39.8(4) . . . . ? C7 Fe C3 C4 165.9(3) . . . . ? C8 Fe C3 C4 -158.98(18) . . . . ? C1 Fe C3 C4 81.33(19) . . . . ? C10 Fe C3 C4 -74.2(2) . . . . ? C9 Fe C3 C4 -117.06(19) . . . . ? C2 Fe C3 C4 119.2(3) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? Fe C3 C4 C5 -59.3(2) . . . . ? C2 C3 C4 Fe 60.0(2) . . . . ? C6 Fe C4 C5 -77.2(2) . . . . ? C7 Fe C4 C5 -48.0(4) . . . . ? C8 Fe C4 C5 172.2(3) . . . . ? C1 Fe C4 C5 38.17(18) . . . . ? C3 Fe C4 C5 119.4(3) . . . . ? C10 Fe C4 C5 -118.10(19) . . . . ? C9 Fe C4 C5 -158.77(19) . . . . ? C2 Fe C4 C5 82.0(2) . . . . ? C5 Fe C4 C3 -119.4(3) . . . . ? C6 Fe C4 C3 163.39(16) . . . . ? C7 Fe C4 C3 -167.4(3) . . . . ? C8 Fe C4 C3 52.8(4) . . . . ? C1 Fe C4 C3 -81.23(19) . . . . ? C10 Fe C4 C3 122.50(18) . . . . ? C9 Fe C4 C3 81.8(2) . . . . ? C2 Fe C4 C3 -37.38(17) . . . . ? C2 C1 C5 C4 0.7(3) . . . . ? Fe C1 C5 C4 60.2(2) . . . . ? C2 C1 C5 Fe -59.53(19) . . . . ? C3 C4 C5 C1 -0.9(3) . . . . ? Fe C4 C5 C1 -60.6(2) . . . . ? C3 C4 C5 Fe 59.7(2) . . . . ? C4 Fe C5 C1 118.2(3) . . . . ? C6 Fe C5 C1 -122.35(18) . . . . ? C7 Fe C5 C1 -81.2(2) . . . . ? C8 Fe C5 C1 -52.9(4) . . . . ? C3 Fe C5 C1 80.5(2) . . . . ? C10 Fe C5 C1 -163.91(17) . . . . ? C9 Fe C5 C1 167.6(3) . . . . ? C2 Fe C5 C1 37.19(18) . . . . ? C6 Fe C5 C4 119.48(19) . . . . ? C7 Fe C5 C4 160.62(18) . . . . ? C8 Fe C5 C4 -171.1(3) . . . . ? C1 Fe C5 C4 -118.2(3) . . . . ? C3 Fe C5 C4 -37.63(18) . . . . ? C10 Fe C5 C4 77.9(2) . . . . ? C9 Fe C5 C4 49.4(4) . . . . ? C2 Fe C5 C4 -81.0(2) . . . . ? Si1 O2 C6 C10 -39.2(4) . . . . ? Si1 O2 C6 C7 140.0(2) . . . . ? Si1 O2 C6 Fe -132.50(18) . . . . ? C5 Fe C6 O2 7.0(2) . . . . ? C4 Fe C6 O2 48.2(3) . . . . ? C7 Fe C6 O2 -115.7(3) . . . . ? C8 Fe C6 O2 -153.9(2) . . . . ? C1 Fe C6 O2 -33.4(3) . . . . ? C3 Fe C6 O2 77.2(4) . . . . ? C10 Fe C6 O2 124.4(3) . . . . ? C9 Fe C6 O2 162.7(3) . . . . ? C2 Fe C6 O2 -61.5(4) . . . . ? C5 Fe C6 C10 -117.38(18) . . . . ? C4 Fe C6 C10 -76.26(19) . . . . ? C7 Fe C6 C10 119.9(2) . . . . ? C8 Fe C6 C10 81.71(17) . . . . ? C1 Fe C6 C10 -157.79(18) . . . . ? C3 Fe C6 C10 -47.3(4) . . . . ? C9 Fe C6 C10 38.27(16) . . . . ? C2 Fe C6 C10 174.1(3) . . . . ? C5 Fe C6 C7 122.70(16) . . . . ? C4 Fe C6 C7 163.82(16) . . . . ? C8 Fe C6 C7 -38.21(15) . . . . ? C1 Fe C6 C7 82.29(19) . . . . ? C3 Fe C6 C7 -167.2(3) . . . . ? C10 Fe C6 C7 -119.9(2) . . . . ? C9 Fe C6 C7 -81.65(17) . . . . ? C2 Fe C6 C7 54.2(4) . . . . ? O2 C6 C7 C8 -179.5(2) . . . . ? C10 C6 C7 C8 -0.2(3) . . . . ? Fe C6 C7 C8 59.22(18) . . . . ? O2 C6 C7 C11 7.2(4) . . . . ? C10 C6 C7 C11 -173.6(2) . . . . ? Fe C6 C7 C11 -114.2(2) . . . . ? O2 C6 C7 Fe 121.3(2) . . . . ? C10 C6 C7 Fe -59.40(17) . . . . ? C5 Fe C7 C6 -74.78(19) . . . . ? C4 Fe C7 C6 -39.7(4) . . . . ? C8 Fe C7 C6 118.8(2) . . . . ? C1 Fe C7 C6 -117.53(17) . . . . ? C3 Fe C7 C6 165.3(3) . . . . ? C10 Fe C7 C6 37.24(15) . . . . ? C9 Fe C7 C6 81.12(17) . . . . ? C2 Fe C7 C6 -159.83(15) . . . . ? C5 Fe C7 C8 166.43(18) . . . . ? C4 Fe C7 C8 -158.5(3) . . . . ? C6 Fe C7 C8 -118.8(2) . . . . ? C1 Fe C7 C8 123.68(19) . . . . ? C3 Fe C7 C8 46.5(4) . . . . ? C10 Fe C7 C8 -81.55(18) . . . . ? C9 Fe C7 C8 -37.67(18) . . . . ? C2 Fe C7 C8 81.4(2) . . . . ? C5 Fe C7 C11 42.8(3) . . . . ? C4 Fe C7 C11 77.9(4) . . . . ? C6 Fe C7 C11 117.6(3) . . . . ? C8 Fe C7 C11 -123.6(3) . . . . ? C1 Fe C7 C11 0.1(3) . . . . ? C3 Fe C7 C11 -77.1(4) . . . . ? C10 Fe C7 C11 154.8(3) . . . . ? C9 Fe C7 C11 -161.3(3) . . . . ? C2 Fe C7 C11 -42.2(3) . . . . ? C6 C7 C8 C9 0.9(3) . . . . ? C11 C7 C8 C9 173.8(3) . . . . ? Fe C7 C8 C9 59.99(19) . . . . ? C6 C7 C8 Fe -59.10(17) . . . . ? C11 C7 C8 Fe 113.8(3) . . . . ? C5 Fe C8 C9 -155.9(4) . . . . ? C4 Fe C8 C9 39.8(4) . . . . ? C6 Fe C8 C9 -80.48(19) . . . . ? C7 Fe C8 C9 -118.6(3) . . . . ? C1 Fe C8 C9 164.17(19) . . . . ? C3 Fe C8 C9 78.4(2) . . . . ? C10 Fe C8 C9 -36.74(18) . . . . ? C2 Fe C8 C9 121.37(19) . . . . ? C5 Fe C8 C7 -37.3(5) . . . . ? C4 Fe C8 C7 158.4(3) . . . . ? C6 Fe C8 C7 38.14(16) . . . . ? C1 Fe C8 C7 -77.2(2) . . . . ? C3 Fe C8 C7 -162.94(17) . . . . ? C10 Fe C8 C7 81.88(17) . . . . ? C9 Fe C8 C7 118.6(3) . . . . ? C2 Fe C8 C7 -120.01(17) . . . . ? C7 C8 C9 C10 -1.3(3) . . . . ? Fe C8 C9 C10 58.20(19) . . . . ? C7 C8 C9 Fe -59.49(19) . . . . ? C5 Fe C9 C8 160.9(3) . . . . ? C4 Fe C9 C8 -163.71(17) . . . . ? C6 Fe C9 C8 82.99(18) . . . . ? C7 Fe C9 C8 38.51(17) . . . . ? C1 Fe C9 C8 -46.5(5) . . . . ? C3 Fe C9 C8 -120.85(19) . . . . ? C10 Fe C9 C8 121.2(2) . . . . ? C2 Fe C9 C8 -79.6(2) . . . . ? C5 Fe C9 C10 39.7(4) . . . . ? C4 Fe C9 C10 75.1(2) . . . . ? C6 Fe C9 C10 -38.23(15) . . . . ? C7 Fe C9 C10 -82.71(17) . . . . ? C8 Fe C9 C10 -121.2(2) . . . . ? C1 Fe C9 C10 -167.7(4) . . . . ? C3 Fe C9 C10 117.93(17) . . . . ? C2 Fe C9 C10 159.17(16) . . . . ? O2 C6 C10 C9 178.6(2) . . . . ? C7 C6 C10 C9 -0.6(3) . . . . ? Fe C6 C10 C9 -59.69(18) . . . . ? O2 C6 C10 Fe -121.7(3) . . . . ? C7 C6 C10 Fe 59.09(17) . . . . ? C8 C9 C10 C6 1.2(3) . . . . ? Fe C9 C10 C6 59.36(17) . . . . ? C8 C9 C10 Fe -58.18(19) . . . . ? C5 Fe C10 C6 79.02(19) . . . . ? C4 Fe C10 C6 120.14(17) . . . . ? C7 Fe C10 C6 -37.63(15) . . . . ? C8 Fe C10 C6 -81.94(17) . . . . ? C1 Fe C10 C6 52.5(4) . . . . ? C3 Fe C10 C6 160.54(16) . . . . ? C9 Fe C10 C6 -118.3(2) . . . . ? C2 Fe C10 C6 -174.1(3) . . . . ? C5 Fe C10 C9 -162.68(17) . . . . ? C4 Fe C10 C9 -121.56(17) . . . . ? C6 Fe C10 C9 118.3(2) . . . . ? C7 Fe C10 C9 80.67(17) . . . . ? C8 Fe C10 C9 36.36(16) . . . . ? C1 Fe C10 C9 170.8(3) . . . . ? C3 Fe C10 C9 -81.2(2) . . . . ? C2 Fe C10 C9 -55.8(4) . . . . ? C6 C7 C11 O1 -177.7(3) . . . . ? C8 C7 C11 O1 10.4(5) . . . . ? Fe C7 C11 O1 97.8(3) . . . . ? O2 Si1 C21 C22 -170.2(2) . . . . ? C31 Si1 C21 C22 -56.8(2) . . . . ? C41 Si1 C21 C22 73.4(2) . . . . ? O2 Si1 C21 C26 8.1(2) . . . . ? C31 Si1 C21 C26 121.5(2) . . . . ? C41 Si1 C21 C26 -108.3(2) . . . . ? C26 C21 C22 C23 1.9(4) . . . . ? Si1 C21 C22 C23 -179.72(19) . . . . ? C21 C22 C23 C24 -1.0(4) . . . . ? C22 C23 C24 C25 -0.5(5) . . . . ? C23 C24 C25 C26 1.0(5) . . . . ? C24 C25 C26 C21 0.0(5) . . . . ? C22 C21 C26 C25 -1.4(4) . . . . ? Si1 C21 C26 C25 -179.8(2) . . . . ? O2 Si1 C31 C36 -130.3(2) . . . . ? C21 Si1 C31 C36 120.1(3) . . . . ? C41 Si1 C31 C36 -7.7(3) . . . . ? O2 Si1 C31 C32 49.6(2) . . . . ? C21 Si1 C31 C32 -60.0(3) . . . . ? C41 Si1 C31 C32 172.1(2) . . . . ? C36 C31 C32 C33 1.0(5) . . . . ? Si1 C31 C32 C33 -178.9(3) . . . . ? C31 C32 C33 C34 -0.3(5) . . . . ? C32 C33 C34 C35 -0.1(6) . . . . ? C33 C34 C35 C36 -0.2(6) . . . . ? C32 C31 C36 C35 -1.3(4) . . . . ? Si1 C31 C36 C35 178.5(2) . . . . ? C34 C35 C36 C31 1.0(5) . . . . ? O2 Si1 C41 C43 62.9(2) . . . . ? C31 Si1 C41 C43 -59.1(3) . . . . ? C21 Si1 C41 C43 175.1(2) . . . . ? O2 Si1 C41 C42 -174.4(2) . . . . ? C31 Si1 C41 C42 63.6(2) . . . . ? C21 Si1 C41 C42 -62.2(3) . . . . ? O2 Si1 C41 C44 -56.0(2) . . . . ? C31 Si1 C41 C44 -178.0(2) . . . . ? C21 Si1 C41 C44 56.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.830 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.830 _refine_diff_density_max 0.213 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.045 # Attachment 'pS19a.cif' data_erk3693 _database_code_depnum_ccdc_archive 'CCDC 714366' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H45 Fe N O Si' _chemical_formula_weight 627.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.144(1) _cell_length_b 11.841(1) _cell_length_c 16.838(1) _cell_angle_alpha 90.00 _cell_angle_beta 103.20(1) _cell_angle_gamma 90.00 _cell_volume 1775.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 2550 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8478 _exptl_absorpt_correction_T_max 0.9528 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9817 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.86 _reflns_number_total 6966 _reflns_number_gt 5788 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0239P)^2^+0.3119P] 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 riding _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 -0.021(11) _refine_ls_number_reflns 6966 _refine_ls_number_parameters 395 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Fe Fe 0.98681(3) 0.49638(3) 0.177680(18) 0.03457(10) Uani 1 1 d . . . C1 C 0.8879(5) 0.4320(4) 0.0666(2) 0.0733(12) Uani 1 1 d . . . H1 H 0.7956 0.3917 0.0541 0.088 Uiso 1 1 calc R . . C2 C 1.0341(6) 0.3855(3) 0.0958(2) 0.0801(14) Uani 1 1 d . . . H2 H 1.0584 0.3082 0.1066 0.096 Uiso 1 1 calc R . . C3 C 1.1340(4) 0.4752(5) 0.1055(2) 0.0791(13) Uani 1 1 d . . . H3 H 1.2399 0.4697 0.1240 0.095 Uiso 1 1 calc R . . C4 C 1.0557(5) 0.5727(4) 0.0843(2) 0.0729(11) Uani 1 1 d . . . H4 H 1.0979 0.6462 0.0860 0.088 Uiso 1 1 calc R . . C5 C 0.9069(4) 0.5473(3) 0.06021(18) 0.0609(10) Uani 1 1 d . . . H5 H 0.8285 0.6004 0.0419 0.073 Uiso 1 1 calc R . . C6 C 0.8738(3) 0.5742(2) 0.25484(14) 0.0287(5) Uani 1 1 d . . . C7 C 0.8635(3) 0.4550(2) 0.26123(14) 0.0288(5) Uani 1 1 d . . . C8 C 1.0151(3) 0.4124(2) 0.28557(15) 0.0356(6) Uani 1 1 d . . . H8 H 1.0441 0.3355 0.2943 0.043 Uiso 1 1 calc R . . C9 C 1.1126(2) 0.5070(3) 0.29398(13) 0.0397(6) Uani 1 1 d . . . H9 H 1.2190 0.5039 0.3104 0.048 Uiso 1 1 calc R . . C10 C 1.0270(3) 0.6067(2) 0.27421(16) 0.0361(6) Uani 1 1 d . . . H10 H 1.0650 0.6814 0.2739 0.043 Uiso 1 1 calc R . . C11 C 0.7238(3) 0.3939(2) 0.25036(13) 0.0284(5) Uani 1 1 d . . . H11 H 0.6334 0.4327 0.2267 0.034 Uiso 1 1 calc R . . N12 N 0.7148(2) 0.29106(18) 0.27060(12) 0.0320(5) Uani 1 1 d . . . C13 C 0.5679(3) 0.2434(2) 0.26080(15) 0.0304(5) Uani 1 1 d . . . C14 C 0.5117(3) 0.2297(2) 0.33156(15) 0.0404(6) Uani 1 1 d . . . C141 C 0.6022(3) 0.2649(3) 0.41449(16) 0.0557(8) Uani 1 1 d . . . H141 H 0.7039 0.2883 0.4079 0.067 Uiso 1 1 calc R . . C142 C 0.5316(6) 0.3670(4) 0.4471(3) 0.1022(15) Uani 1 1 d . . . H14A H 0.5270 0.4306 0.4094 0.153 Uiso 1 1 calc R . . H14B H 0.5928 0.3881 0.5008 0.153 Uiso 1 1 calc R . . H14C H 0.4299 0.3477 0.4521 0.153 Uiso 1 1 calc R . . C143 C 0.6243(5) 0.1680(4) 0.4755(2) 0.0979(15) Uani 1 1 d . . . H14D H 0.5267 0.1449 0.4848 0.147 Uiso 1 1 calc R . . H14E H 0.6895 0.1928 0.5271 0.147 Uiso 1 1 calc R . . H14F H 0.6710 0.1040 0.4538 0.147 Uiso 1 1 calc R . . C15 C 0.3697(3) 0.1834(3) 0.32242(19) 0.0534(8) Uani 1 1 d . . . H15 H 0.3284 0.1755 0.3690 0.064 Uiso 1 1 calc R . . C16 C 0.2874(3) 0.1488(3) 0.2481(2) 0.0587(8) Uani 1 1 d . . . H16 H 0.1905 0.1171 0.2437 0.070 Uiso 1 1 calc R . . C17 C 0.3449(3) 0.1600(3) 0.17987(19) 0.0518(7) Uani 1 1 d . . . H17 H 0.2872 0.1349 0.1287 0.062 Uiso 1 1 calc R . . C18 C 0.4862(3) 0.2074(2) 0.18427(16) 0.0370(6) Uani 1 1 d . . . C181 C 0.5469(3) 0.2191(2) 0.10758(15) 0.0414(6) Uani 1 1 d . . . H181 H 0.6559 0.2385 0.1255 0.050 Uiso 1 1 calc R . . C182 C 0.4701(4) 0.3164(3) 0.05370(18) 0.0634(9) Uani 1 1 d . . . H18A H 0.5144 0.3239 0.0062 0.095 Uiso 1 1 calc R . . H18B H 0.4845 0.3868 0.0851 0.095 Uiso 1 1 calc R . . H18C H 0.3625 0.3005 0.0354 0.095 Uiso 1 1 calc R . . C183 C 0.5361(4) 0.1090(3) 0.05888(19) 0.0599(9) Uani 1 1 d . . . H18D H 0.4302 0.0907 0.0363 0.090 Uiso 1 1 calc R . . H18E H 0.5834 0.0478 0.0949 0.090 Uiso 1 1 calc R . . H18F H 0.5878 0.1181 0.0143 0.090 Uiso 1 1 calc R . . O1 O 0.74865(18) 0.64159(14) 0.23534(10) 0.0323(4) Uani 1 1 d . . . Si1 Si 0.72636(7) 0.76380(6) 0.28068(4) 0.02933(15) Uani 1 1 d . . . C21 C 0.8140(3) 0.8758(2) 0.22838(14) 0.0309(5) Uani 1 1 d . . . C22 C 0.8664(3) 0.8462(2) 0.15969(15) 0.0394(6) Uani 1 1 d . . . H22 H 0.8607 0.7694 0.1428 0.047 Uiso 1 1 calc R . . C23 C 0.9262(3) 0.9247(3) 0.11550(17) 0.0483(7) Uani 1 1 d . . . H23 H 0.9616 0.9017 0.0692 0.058 Uiso 1 1 calc R . . C24 C 0.9344(3) 1.0368(2) 0.13867(16) 0.0431(7) Uani 1 1 d . . . H24 H 0.9752 1.0911 0.1082 0.052 Uiso 1 1 calc R . . C25 C 0.8833(3) 1.0696(2) 0.20616(17) 0.0397(6) Uani 1 1 d . . . H25 H 0.8891 1.1466 0.2223 0.048 Uiso 1 1 calc R . . C26 C 0.8238(2) 0.9907(2) 0.25024(13) 0.0334(5) Uani 1 1 d . . . H26 H 0.7885 1.0145 0.2964 0.040 Uiso 1 1 calc R . . C31 C 0.8186(3) 0.7473(2) 0.39120(14) 0.0347(6) Uani 1 1 d . . . C32 C 0.9009(3) 0.8326(3) 0.43793(16) 0.0478(7) Uani 1 1 d . . . H32 H 0.9092 0.9042 0.4138 0.057 Uiso 1 1 calc R . . C33 C 0.9714(4) 0.8149(3) 0.51956(16) 0.0585(8) Uani 1 1 d . . . H33 H 1.0262 0.8746 0.5505 0.070 Uiso 1 1 calc R . . C34 C 0.9622(3) 0.7120(3) 0.55549(16) 0.0550(8) Uani 1 1 d . . . H34 H 1.0123 0.6998 0.6108 0.066 Uiso 1 1 calc R . . C35 C 0.8799(3) 0.6263(3) 0.51081(16) 0.0492(7) Uani 1 1 d . . . H35 H 0.8714 0.5553 0.5356 0.059 Uiso 1 1 calc R . . C36 C 0.8096(3) 0.6439(2) 0.42976(15) 0.0432(6) Uani 1 1 d . . . H36 H 0.7538 0.5840 0.3996 0.052 Uiso 1 1 calc R . . C41 C 0.5176(3) 0.7819(2) 0.26241(15) 0.0372(6) Uani 1 1 d . . . C42 C 0.4828(3) 0.8889(3) 0.3066(2) 0.0620(9) Uani 1 1 d . . . H42A H 0.5204 0.9554 0.2829 0.093 Uiso 1 1 calc R . . H42B H 0.5318 0.8838 0.3647 0.093 Uiso 1 1 calc R . . H42C H 0.3740 0.8957 0.3004 0.093 Uiso 1 1 calc R . . C43 C 0.4485(4) 0.7939(3) 0.17131(18) 0.0625(10) Uani 1 1 d . . . H43A H 0.4684 0.7254 0.1429 0.094 Uiso 1 1 calc R . . H43B H 0.4929 0.8591 0.1498 0.094 Uiso 1 1 calc R . . H43C H 0.3398 0.8048 0.1628 0.094 Uiso 1 1 calc R . . C44 C 0.4480(3) 0.6795(3) 0.2957(2) 0.0626(9) Uani 1 1 d . . . H44A H 0.3383 0.6870 0.2824 0.094 Uiso 1 1 calc R . . H44B H 0.4848 0.6758 0.3551 0.094 Uiso 1 1 calc R . . H44C H 0.4762 0.6103 0.2710 0.094 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 Fe 0.03151(18) 0.0429(2) 0.03217(17) 0.00157(18) 0.01318(13) 0.00109(17) C1 0.076(3) 0.111(4) 0.0410(18) -0.031(2) 0.0312(18) -0.044(2) C2 0.151(4) 0.052(2) 0.050(2) 0.0013(18) 0.050(3) 0.032(3) C3 0.051(2) 0.140(4) 0.0557(19) -0.010(3) 0.0323(16) 0.017(3) C4 0.095(3) 0.085(3) 0.050(2) -0.001(2) 0.041(2) -0.027(2) C5 0.073(3) 0.081(3) 0.0275(15) 0.0029(16) 0.0106(15) 0.024(2) C6 0.0286(13) 0.0339(14) 0.0242(12) -0.0028(11) 0.0072(10) -0.0030(10) C7 0.0282(13) 0.0370(14) 0.0228(11) -0.0009(10) 0.0092(9) -0.0030(9) C8 0.0366(15) 0.0404(15) 0.0302(13) 0.0077(12) 0.0083(11) 0.0010(12) C9 0.0269(11) 0.0514(17) 0.0388(12) 0.0022(15) 0.0031(9) -0.0048(13) C10 0.0308(14) 0.0392(15) 0.0375(14) -0.0009(12) 0.0063(11) -0.0082(11) C11 0.0281(13) 0.0342(15) 0.0233(12) -0.0028(11) 0.0069(9) -0.0008(10) N12 0.0295(11) 0.0375(13) 0.0308(10) -0.0033(10) 0.0104(8) -0.0037(9) C13 0.0280(13) 0.0258(13) 0.0377(13) 0.0001(11) 0.0083(10) 0.0003(9) C14 0.0384(15) 0.0432(17) 0.0435(15) 0.0003(13) 0.0174(12) -0.0047(11) C141 0.0562(18) 0.075(2) 0.0424(15) -0.0030(16) 0.0240(13) -0.0157(16) C142 0.121(4) 0.097(3) 0.090(3) -0.044(3) 0.028(3) -0.008(3) C143 0.119(4) 0.119(4) 0.049(2) 0.015(2) 0.004(2) -0.016(3) C15 0.0415(17) 0.061(2) 0.0646(19) 0.0067(17) 0.0268(15) -0.0037(14) C16 0.0309(16) 0.065(2) 0.079(2) 0.0035(18) 0.0101(15) -0.0131(14) C17 0.0321(15) 0.0572(18) 0.0603(18) -0.0030(15) -0.0018(13) -0.0064(13) C18 0.0303(14) 0.0353(14) 0.0438(15) 0.0004(12) 0.0053(12) 0.0031(11) C181 0.0364(15) 0.0509(17) 0.0342(13) -0.0026(13) 0.0022(11) 0.0013(12) C182 0.076(2) 0.069(2) 0.0427(16) 0.0090(16) 0.0093(15) 0.0183(18) C183 0.0552(19) 0.067(2) 0.0517(18) -0.0173(16) -0.0001(15) 0.0015(16) O1 0.0312(9) 0.0313(9) 0.0341(9) -0.0047(8) 0.0073(7) -0.0027(7) Si1 0.0296(4) 0.0330(4) 0.0265(3) -0.0017(3) 0.0086(3) -0.0037(3) C21 0.0262(12) 0.0367(14) 0.0297(12) -0.0005(11) 0.0060(10) -0.0052(10) C22 0.0447(16) 0.0398(15) 0.0361(14) -0.0049(13) 0.0138(12) -0.0045(12) C23 0.0593(19) 0.0546(19) 0.0383(15) 0.0025(15) 0.0264(14) -0.0057(15) C24 0.0414(16) 0.0456(17) 0.0448(15) 0.0089(13) 0.0147(12) -0.0104(12) C25 0.0337(14) 0.0351(14) 0.0481(15) 0.0006(12) 0.0046(12) -0.0037(11) C26 0.0293(11) 0.0370(13) 0.0337(11) -0.0016(14) 0.0067(9) -0.0048(12) C31 0.0338(14) 0.0421(16) 0.0295(12) -0.0008(12) 0.0098(10) 0.0020(11) C32 0.0560(18) 0.0488(17) 0.0369(14) -0.0003(14) 0.0072(13) -0.0096(13) C33 0.064(2) 0.070(2) 0.0346(15) -0.0032(16) -0.0028(14) -0.0058(16) C34 0.062(2) 0.073(2) 0.0271(13) -0.0019(15) 0.0048(13) 0.0140(16) C35 0.066(2) 0.0495(18) 0.0353(14) 0.0074(14) 0.0177(14) 0.0158(14) C36 0.0529(17) 0.0438(16) 0.0337(14) -0.0028(13) 0.0115(12) 0.0022(13) C41 0.0281(13) 0.0397(15) 0.0447(14) 0.0017(13) 0.0102(11) -0.0028(11) C42 0.0459(19) 0.063(2) 0.082(2) -0.0103(18) 0.0253(17) 0.0114(15) C43 0.0451(18) 0.088(3) 0.0493(18) 0.0047(17) -0.0007(14) -0.0053(17) C44 0.0328(16) 0.069(2) 0.091(2) 0.0167(19) 0.0241(16) -0.0046(15) _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 Fe C2 2.020(3) . ? Fe C3 2.024(3) . ? Fe C1 2.030(3) . ? Fe C4 2.034(3) . ? Fe C8 2.035(3) . ? Fe C9 2.036(2) . ? Fe C5 2.037(3) . ? Fe C10 2.052(3) . ? Fe C7 2.053(2) . ? Fe C6 2.054(2) . ? C1 C5 1.384(5) . ? C1 C2 1.425(6) . ? C2 C3 1.386(6) . ? C3 C4 1.362(6) . ? C4 C5 1.361(5) . ? C6 O1 1.372(3) . ? C6 C10 1.417(3) . ? C6 C7 1.421(3) . ? C7 C11 1.443(3) . ? C7 C8 1.444(4) . ? C8 C9 1.419(4) . ? C9 C10 1.413(4) . ? C11 N12 1.272(3) . ? N12 C13 1.431(3) . ? C13 C18 1.400(4) . ? C13 C14 1.411(3) . ? C14 C15 1.385(4) . ? C14 C141 1.510(4) . ? C141 C143 1.523(5) . ? C141 C142 1.531(5) . ? C15 C16 1.367(4) . ? C16 C17 1.375(4) . ? C17 C18 1.395(4) . ? C18 C181 1.524(4) . ? C181 C183 1.531(4) . ? C181 C182 1.534(4) . ? O1 Si1 1.6702(18) . ? Si1 C31 1.870(2) . ? Si1 C21 1.871(2) . ? Si1 C41 1.875(3) . ? C21 C22 1.394(3) . ? C21 C26 1.406(4) . ? C22 C23 1.380(4) . ? C23 C24 1.380(4) . ? C24 C25 1.380(4) . ? C25 C26 1.380(4) . ? C31 C32 1.391(4) . ? C31 C36 1.397(4) . ? C32 C33 1.394(4) . ? C33 C34 1.372(4) . ? C34 C35 1.380(4) . ? C35 C36 1.385(4) . ? C41 C43 1.526(4) . ? C41 C44 1.534(4) . ? C41 C42 1.539(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe C3 40.08(17) . . ? C2 Fe C1 41.20(17) . . ? C3 Fe C1 67.55(15) . . ? C2 Fe C4 66.99(16) . . ? C3 Fe C4 39.22(16) . . ? C1 Fe C4 66.82(15) . . ? C2 Fe C8 106.74(13) . . ? C3 Fe C8 120.60(15) . . ? C1 Fe C8 125.29(15) . . ? C4 Fe C8 155.28(15) . . ? C2 Fe C9 122.31(16) . . ? C3 Fe C9 106.15(12) . . ? C1 Fe C9 160.73(16) . . ? C4 Fe C9 120.62(14) . . ? C8 Fe C9 40.79(11) . . ? C2 Fe C5 67.37(15) . . ? C3 Fe C5 66.04(15) . . ? C1 Fe C5 39.78(14) . . ? C4 Fe C5 39.07(15) . . ? C8 Fe C5 162.90(14) . . ? C9 Fe C5 156.08(14) . . ? C2 Fe C10 157.88(17) . . ? C3 Fe C10 122.05(15) . . ? C1 Fe C10 158.43(16) . . ? C4 Fe C10 107.34(13) . . ? C8 Fe C10 68.95(10) . . ? C9 Fe C10 40.45(11) . . ? C5 Fe C10 122.69(13) . . ? C2 Fe C7 123.29(15) . . ? C3 Fe C7 157.86(16) . . ? C1 Fe C7 110.03(12) . . ? C4 Fe C7 162.01(15) . . ? C8 Fe C7 41.37(10) . . ? C9 Fe C7 68.52(9) . . ? C5 Fe C7 127.20(13) . . ? C10 Fe C7 68.69(10) . . ? C2 Fe C6 160.08(17) . . ? C3 Fe C6 159.17(16) . . ? C1 Fe C6 124.65(14) . . ? C4 Fe C6 125.36(15) . . ? C8 Fe C6 68.56(10) . . ? C9 Fe C6 67.60(10) . . ? C5 Fe C6 111.14(12) . . ? C10 Fe C6 40.37(10) . . ? C7 Fe C6 40.49(10) . . ? C5 C1 C2 106.5(4) . . ? C5 C1 Fe 70.4(2) . . ? C2 C1 Fe 69.0(2) . . ? C3 C2 C1 106.6(3) . . ? C3 C2 Fe 70.1(2) . . ? C1 C2 Fe 69.78(19) . . ? C4 C3 C2 109.0(3) . . ? C4 C3 Fe 70.80(19) . . ? C2 C3 Fe 69.83(19) . . ? C5 C4 C3 108.7(4) . . ? C5 C4 Fe 70.59(19) . . ? C3 C4 Fe 70.0(2) . . ? C4 C5 C1 109.2(4) . . ? C4 C5 Fe 70.34(19) . . ? C1 C5 Fe 69.8(2) . . ? O1 C6 C10 128.6(2) . . ? O1 C6 C7 122.0(2) . . ? C10 C6 C7 109.4(2) . . ? O1 C6 Fe 128.47(17) . . ? C10 C6 Fe 69.75(15) . . ? C7 C6 Fe 69.74(15) . . ? C6 C7 C11 124.1(2) . . ? C6 C7 C8 107.0(2) . . ? C11 C7 C8 128.8(2) . . ? C6 C7 Fe 69.77(15) . . ? C11 C7 Fe 129.92(17) . . ? C8 C7 Fe 68.64(13) . . ? C9 C8 C7 107.1(2) . . ? C9 C8 Fe 69.64(14) . . ? C7 C8 Fe 70.00(14) . . ? C10 C9 C8 109.6(2) . . ? C10 C9 Fe 70.40(14) . . ? C8 C9 Fe 69.57(14) . . ? C9 C10 C6 107.0(2) . . ? C9 C10 Fe 69.16(15) . . ? C6 C10 Fe 69.87(15) . . ? N12 C11 C7 123.8(2) . . ? C11 N12 C13 117.6(2) . . ? C18 C13 C14 121.4(2) . . ? C18 C13 N12 121.0(2) . . ? C14 C13 N12 117.5(2) . . ? C15 C14 C13 117.7(2) . . ? C15 C14 C141 120.9(2) . . ? C13 C14 C141 121.4(2) . . ? C14 C141 C143 112.1(3) . . ? C14 C141 C142 111.3(3) . . ? C143 C141 C142 110.8(3) . . ? C16 C15 C14 121.8(3) . . ? C15 C16 C17 120.0(3) . . ? C16 C17 C18 121.4(3) . . ? C17 C18 C13 117.7(3) . . ? C17 C18 C181 120.2(2) . . ? C13 C18 C181 122.1(2) . . ? C18 C181 C183 112.6(2) . . ? C18 C181 C182 111.3(2) . . ? C183 C181 C182 111.0(2) . . ? C6 O1 Si1 125.20(15) . . ? O1 Si1 C31 106.87(10) . . ? O1 Si1 C21 106.80(10) . . ? C31 Si1 C21 113.47(11) . . ? O1 Si1 C41 104.47(10) . . ? C31 Si1 C41 112.71(11) . . ? C21 Si1 C41 111.79(12) . . ? C22 C21 C26 116.6(2) . . ? C22 C21 Si1 118.48(19) . . ? C26 C21 Si1 124.81(18) . . ? C23 C22 C21 122.1(3) . . ? C24 C23 C22 119.9(2) . . ? C25 C24 C23 119.8(2) . . ? C24 C25 C26 120.1(3) . . ? C25 C26 C21 121.5(2) . . ? C32 C31 C36 117.1(2) . . ? C32 C31 Si1 123.4(2) . . ? C36 C31 Si1 119.5(2) . . ? C31 C32 C33 121.1(3) . . ? C34 C33 C32 120.5(3) . . ? C33 C34 C35 119.6(3) . . ? C34 C35 C36 120.0(3) . . ? C35 C36 C31 121.8(3) . . ? C43 C41 C44 109.2(3) . . ? C43 C41 C42 109.0(3) . . ? C44 C41 C42 108.9(2) . . ? C43 C41 Si1 110.38(19) . . ? C44 C41 Si1 110.00(19) . . ? C42 C41 Si1 109.27(18) . . ? 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 Fe C1 C5 -117.3(3) . . . . ? C3 Fe C1 C5 -79.0(3) . . . . ? C4 Fe C1 C5 -36.3(2) . . . . ? C8 Fe C1 C5 168.5(2) . . . . ? C9 Fe C1 C5 -153.3(3) . . . . ? C10 Fe C1 C5 42.1(5) . . . . ? C7 Fe C1 C5 124.6(2) . . . . ? C6 Fe C1 C5 81.7(3) . . . . ? C3 Fe C1 C2 38.3(2) . . . . ? C4 Fe C1 C2 81.0(3) . . . . ? C8 Fe C1 C2 -74.2(3) . . . . ? C9 Fe C1 C2 -36.0(5) . . . . ? C5 Fe C1 C2 117.3(3) . . . . ? C10 Fe C1 C2 159.4(3) . . . . ? C7 Fe C1 C2 -118.1(2) . . . . ? C6 Fe C1 C2 -161.0(2) . . . . ? C5 C1 C2 C3 0.0(4) . . . . ? Fe C1 C2 C3 -60.8(2) . . . . ? C5 C1 C2 Fe 60.8(2) . . . . ? C1 Fe C2 C3 117.2(3) . . . . ? C4 Fe C2 C3 36.6(2) . . . . ? C8 Fe C2 C3 -117.9(2) . . . . ? C9 Fe C2 C3 -76.1(3) . . . . ? C5 Fe C2 C3 79.2(3) . . . . ? C10 Fe C2 C3 -42.7(5) . . . . ? C7 Fe C2 C3 -160.2(2) . . . . ? C6 Fe C2 C3 169.0(3) . . . . ? C3 Fe C2 C1 -117.2(3) . . . . ? C4 Fe C2 C1 -80.6(3) . . . . ? C8 Fe C2 C1 124.9(2) . . . . ? C9 Fe C2 C1 166.7(2) . . . . ? C5 Fe C2 C1 -38.0(2) . . . . ? C10 Fe C2 C1 -159.9(3) . . . . ? C7 Fe C2 C1 82.6(2) . . . . ? C6 Fe C2 C1 51.8(5) . . . . ? C1 C2 C3 C4 0.4(4) . . . . ? Fe C2 C3 C4 -60.2(2) . . . . ? C1 C2 C3 Fe 60.6(2) . . . . ? C2 Fe C3 C4 119.7(3) . . . . ? C1 Fe C3 C4 80.4(3) . . . . ? C8 Fe C3 C4 -160.8(2) . . . . ? C9 Fe C3 C4 -118.9(2) . . . . ? C5 Fe C3 C4 37.0(2) . . . . ? C10 Fe C3 C4 -77.8(3) . . . . ? C7 Fe C3 C4 168.5(3) . . . . ? C6 Fe C3 C4 -49.7(5) . . . . ? C1 Fe C3 C2 -39.3(3) . . . . ? C4 Fe C3 C2 -119.7(3) . . . . ? C8 Fe C3 C2 79.5(3) . . . . ? C9 Fe C3 C2 121.3(2) . . . . ? C5 Fe C3 C2 -82.8(3) . . . . ? C10 Fe C3 C2 162.5(2) . . . . ? C7 Fe C3 C2 48.8(4) . . . . ? C6 Fe C3 C2 -169.4(3) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? Fe C3 C4 C5 -60.2(2) . . . . ? C2 C3 C4 Fe 59.6(2) . . . . ? C2 Fe C4 C5 81.9(3) . . . . ? C3 Fe C4 C5 119.4(3) . . . . ? C1 Fe C4 C5 37.0(2) . . . . ? C8 Fe C4 C5 161.9(3) . . . . ? C9 Fe C4 C5 -163.0(2) . . . . ? C10 Fe C4 C5 -120.9(2) . . . . ? C7 Fe C4 C5 -46.6(5) . . . . ? C6 Fe C4 C5 -80.1(3) . . . . ? C2 Fe C4 C3 -37.4(2) . . . . ? C1 Fe C4 C3 -82.4(3) . . . . ? C8 Fe C4 C3 42.6(5) . . . . ? C9 Fe C4 C3 77.6(3) . . . . ? C5 Fe C4 C3 -119.4(3) . . . . ? C10 Fe C4 C3 119.8(2) . . . . ? C7 Fe C4 C3 -165.9(4) . . . . ? C6 Fe C4 C3 160.6(2) . . . . ? C3 C4 C5 C1 0.6(4) . . . . ? Fe C4 C5 C1 -59.2(3) . . . . ? C3 C4 C5 Fe 59.8(2) . . . . ? C2 C1 C5 C4 -0.4(4) . . . . ? Fe C1 C5 C4 59.5(2) . . . . ? C2 C1 C5 Fe -59.9(2) . . . . ? C2 Fe C5 C4 -80.9(3) . . . . ? C3 Fe C5 C4 -37.1(3) . . . . ? C1 Fe C5 C4 -120.2(3) . . . . ? C8 Fe C5 C4 -153.8(4) . . . . ? C9 Fe C5 C4 38.4(4) . . . . ? C10 Fe C5 C4 76.8(3) . . . . ? C7 Fe C5 C4 163.6(2) . . . . ? C6 Fe C5 C4 120.5(2) . . . . ? C2 Fe C5 C1 39.3(2) . . . . ? C3 Fe C5 C1 83.1(3) . . . . ? C4 Fe C5 C1 120.2(3) . . . . ? C8 Fe C5 C1 -33.6(6) . . . . ? C9 Fe C5 C1 158.6(3) . . . . ? C10 Fe C5 C1 -163.0(2) . . . . ? C7 Fe C5 C1 -76.1(3) . . . . ? C6 Fe C5 C1 -119.2(2) . . . . ? C2 Fe C6 O1 -74.0(5) . . . . ? C3 Fe C6 O1 85.8(4) . . . . ? C1 Fe C6 O1 -35.0(3) . . . . ? C4 Fe C6 O1 49.5(3) . . . . ? C8 Fe C6 O1 -153.9(2) . . . . ? C9 Fe C6 O1 162.0(2) . . . . ? C5 Fe C6 O1 7.8(3) . . . . ? C10 Fe C6 O1 123.8(3) . . . . ? C7 Fe C6 O1 -115.3(3) . . . . ? C2 Fe C6 C10 162.2(4) . . . . ? C3 Fe C6 C10 -38.1(4) . . . . ? C1 Fe C6 C10 -158.8(2) . . . . ? C4 Fe C6 C10 -74.3(2) . . . . ? C8 Fe C6 C10 82.32(16) . . . . ? C9 Fe C6 C10 38.20(16) . . . . ? C5 Fe C6 C10 -116.05(19) . . . . ? C7 Fe C6 C10 120.9(2) . . . . ? C2 Fe C6 C7 41.3(5) . . . . ? C3 Fe C6 C7 -159.0(3) . . . . ? C1 Fe C6 C7 80.3(2) . . . . ? C4 Fe C6 C7 164.79(19) . . . . ? C8 Fe C6 C7 -38.58(16) . . . . ? C9 Fe C6 C7 -82.69(18) . . . . ? C5 Fe C6 C7 123.06(19) . . . . ? C10 Fe C6 C7 -120.9(2) . . . . ? O1 C6 C7 C11 -1.7(4) . . . . ? C10 C6 C7 C11 176.2(2) . . . . ? Fe C6 C7 C11 -125.2(2) . . . . ? O1 C6 C7 C8 -177.77(19) . . . . ? C10 C6 C7 C8 0.2(3) . . . . ? Fe C6 C7 C8 58.78(17) . . . . ? O1 C6 C7 Fe 123.5(2) . . . . ? C10 C6 C7 Fe -58.60(19) . . . . ? C2 Fe C7 C6 -164.4(2) . . . . ? C3 Fe C7 C6 160.2(3) . . . . ? C1 Fe C7 C6 -120.3(2) . . . . ? C4 Fe C7 C6 -43.9(5) . . . . ? C8 Fe C7 C6 118.6(2) . . . . ? C9 Fe C7 C6 80.22(18) . . . . ? C5 Fe C7 C6 -78.9(2) . . . . ? C10 Fe C7 C6 36.63(16) . . . . ? C2 Fe C7 C11 -46.3(3) . . . . ? C3 Fe C7 C11 -81.7(4) . . . . ? C1 Fe C7 C11 -2.2(3) . . . . ? C4 Fe C7 C11 74.3(5) . . . . ? C8 Fe C7 C11 -123.3(3) . . . . ? C9 Fe C7 C11 -161.7(3) . . . . ? C5 Fe C7 C11 39.2(3) . . . . ? C10 Fe C7 C11 154.8(3) . . . . ? C6 Fe C7 C11 118.1(3) . . . . ? C2 Fe C7 C8 77.0(2) . . . . ? C3 Fe C7 C8 41.6(4) . . . . ? C1 Fe C7 C8 121.1(2) . . . . ? C4 Fe C7 C8 -162.4(4) . . . . ? C9 Fe C7 C8 -38.35(16) . . . . ? C5 Fe C7 C8 162.49(19) . . . . ? C10 Fe C7 C8 -81.94(15) . . . . ? C6 Fe C7 C8 -118.6(2) . . . . ? C6 C7 C8 C9 0.6(3) . . . . ? C11 C7 C8 C9 -175.2(2) . . . . ? Fe C7 C8 C9 60.07(16) . . . . ? C6 C7 C8 Fe -59.50(18) . . . . ? C11 C7 C8 Fe 124.7(3) . . . . ? C2 Fe C8 C9 120.4(2) . . . . ? C3 Fe C8 C9 79.0(2) . . . . ? C1 Fe C8 C9 161.82(19) . . . . ? C4 Fe C8 C9 49.2(4) . . . . ? C5 Fe C8 C9 -172.5(4) . . . . ? C10 Fe C8 C9 -36.66(15) . . . . ? C7 Fe C8 C9 -117.9(2) . . . . ? C6 Fe C8 C9 -80.12(16) . . . . ? C2 Fe C8 C7 -121.7(2) . . . . ? C3 Fe C8 C7 -163.1(2) . . . . ? C1 Fe C8 C7 -80.3(2) . . . . ? C4 Fe C8 C7 167.1(3) . . . . ? C9 Fe C8 C7 117.9(2) . . . . ? C5 Fe C8 C7 -54.6(5) . . . . ? C10 Fe C8 C7 81.24(15) . . . . ? C6 Fe C8 C7 37.78(15) . . . . ? C7 C8 C9 C10 -1.1(3) . . . . ? Fe C8 C9 C10 59.17(17) . . . . ? C7 C8 C9 Fe -60.30(16) . . . . ? C2 Fe C9 C10 161.4(2) . . . . ? C3 Fe C9 C10 120.8(2) . . . . ? C1 Fe C9 C10 -171.3(3) . . . . ? C4 Fe C9 C10 80.8(2) . . . . ? C8 Fe C9 C10 -120.8(2) . . . . ? C5 Fe C9 C10 53.7(3) . . . . ? C7 Fe C9 C10 -81.93(15) . . . . ? C6 Fe C9 C10 -38.13(15) . . . . ? C2 Fe C9 C8 -77.8(2) . . . . ? C3 Fe C9 C8 -118.4(2) . . . . ? C1 Fe C9 C8 -50.5(4) . . . . ? C4 Fe C9 C8 -158.41(19) . . . . ? C5 Fe C9 C8 174.6(3) . . . . ? C10 Fe C9 C8 120.8(2) . . . . ? C7 Fe C9 C8 38.88(15) . . . . ? C6 Fe C9 C8 82.68(16) . . . . ? C8 C9 C10 C6 1.2(3) . . . . ? Fe C9 C10 C6 59.91(18) . . . . ? C8 C9 C10 Fe -58.68(17) . . . . ? O1 C6 C10 C9 176.9(2) . . . . ? C7 C6 C10 C9 -0.9(3) . . . . ? Fe C6 C10 C9 -59.45(17) . . . . ? O1 C6 C10 Fe -123.6(3) . . . . ? C7 C6 C10 Fe 58.59(19) . . . . ? C2 Fe C10 C9 -45.7(4) . . . . ? C3 Fe C10 C9 -76.8(2) . . . . ? C1 Fe C10 C9 172.2(3) . . . . ? C4 Fe C10 C9 -117.14(19) . . . . ? C8 Fe C10 C9 36.95(14) . . . . ? C5 Fe C10 C9 -157.14(17) . . . . ? C7 Fe C10 C9 81.47(15) . . . . ? C6 Fe C10 C9 118.2(2) . . . . ? C2 Fe C10 C6 -163.9(3) . . . . ? C3 Fe C10 C6 165.01(19) . . . . ? C1 Fe C10 C6 54.0(4) . . . . ? C4 Fe C10 C6 124.7(2) . . . . ? C8 Fe C10 C6 -81.25(16) . . . . ? C9 Fe C10 C6 -118.2(2) . . . . ? C5 Fe C10 C6 84.7(2) . . . . ? C7 Fe C10 C6 -36.73(15) . . . . ? C6 C7 C11 N12 -166.5(2) . . . . ? C8 C7 C11 N12 8.6(4) . . . . ? Fe C7 C11 N12 102.2(3) . . . . ? C7 C11 N12 C13 176.3(2) . . . . ? C11 N12 C13 C18 79.3(3) . . . . ? C11 N12 C13 C14 -103.3(3) . . . . ? C18 C13 C14 C15 -2.6(4) . . . . ? N12 C13 C14 C15 -179.9(2) . . . . ? C18 C13 C14 C141 177.9(3) . . . . ? N12 C13 C14 C141 0.5(4) . . . . ? C15 C14 C141 C143 56.4(4) . . . . ? C13 C14 C141 C143 -124.0(3) . . . . ? C15 C14 C141 C142 -68.3(4) . . . . ? C13 C14 C141 C142 111.3(3) . . . . ? C13 C14 C15 C16 1.8(5) . . . . ? C141 C14 C15 C16 -178.6(3) . . . . ? C14 C15 C16 C17 -0.3(5) . . . . ? C15 C16 C17 C18 -0.7(5) . . . . ? C16 C17 C18 C13 0.0(5) . . . . ? C16 C17 C18 C181 -179.8(3) . . . . ? C14 C13 C18 C17 1.7(4) . . . . ? N12 C13 C18 C17 178.9(2) . . . . ? C14 C13 C18 C181 -178.6(3) . . . . ? N12 C13 C18 C181 -1.3(4) . . . . ? C17 C18 C181 C183 -50.2(4) . . . . ? C13 C18 C181 C183 130.1(3) . . . . ? C17 C18 C181 C182 75.2(4) . . . . ? C13 C18 C181 C182 -104.6(3) . . . . ? C10 C6 O1 Si1 -40.9(3) . . . . ? C7 C6 O1 Si1 136.6(2) . . . . ? Fe C6 O1 Si1 -134.83(16) . . . . ? C6 O1 Si1 C31 -36.5(2) . . . . ? C6 O1 Si1 C21 85.20(19) . . . . ? C6 O1 Si1 C41 -156.21(19) . . . . ? O1 Si1 C21 C22 6.2(2) . . . . ? C31 Si1 C21 C22 123.7(2) . . . . ? C41 Si1 C21 C22 -107.5(2) . . . . ? O1 Si1 C21 C26 -177.70(19) . . . . ? C31 Si1 C21 C26 -60.2(2) . . . . ? C41 Si1 C21 C26 68.6(2) . . . . ? C26 C21 C22 C23 0.6(4) . . . . ? Si1 C21 C22 C23 177.0(2) . . . . ? C21 C22 C23 C24 -0.5(5) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? C23 C24 C25 C26 -0.2(4) . . . . ? C24 C25 C26 C21 0.3(4) . . . . ? C22 C21 C26 C25 -0.5(3) . . . . ? Si1 C21 C26 C25 -176.66(18) . . . . ? O1 Si1 C31 C32 141.0(2) . . . . ? C21 Si1 C31 C32 23.6(3) . . . . ? C41 Si1 C31 C32 -104.8(2) . . . . ? O1 Si1 C31 C36 -37.1(2) . . . . ? C21 Si1 C31 C36 -154.58(19) . . . . ? C41 Si1 C31 C36 77.1(2) . . . . ? C36 C31 C32 C33 0.2(4) . . . . ? Si1 C31 C32 C33 -178.0(2) . . . . ? C31 C32 C33 C34 0.6(5) . . . . ? C32 C33 C34 C35 -1.3(5) . . . . ? C33 C34 C35 C36 1.2(4) . . . . ? C34 C35 C36 C31 -0.4(4) . . . . ? C32 C31 C36 C35 -0.3(4) . . . . ? Si1 C31 C36 C35 178.0(2) . . . . ? O1 Si1 C41 C43 -63.9(2) . . . . ? C31 Si1 C41 C43 -179.5(2) . . . . ? C21 Si1 C41 C43 51.3(2) . . . . ? O1 Si1 C41 C44 56.8(2) . . . . ? C31 Si1 C41 C44 -58.9(2) . . . . ? C21 Si1 C41 C44 171.9(2) . . . . ? O1 Si1 C41 C42 176.32(19) . . . . ? C31 Si1 C41 C42 60.7(2) . . . . ? C21 Si1 C41 C42 -68.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.269 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.042 # Attachment 'pS20.cif' data_erk4592 _database_code_depnum_ccdc_archive 'CCDC 714367' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H9 F4 Fe N O' _chemical_formula_weight 375.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.0568(3) _cell_length_b 7.2896(2) _cell_length_c 15.2684(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.131(1) _cell_angle_gamma 90.00 _cell_volume 1409.25(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2885 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5528 _exptl_absorpt_correction_T_max 0.9671 _exptl_absorpt_process_details 'Denzo (Otwinoski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11237 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6691 _reflns_number_gt 5682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0379P)^2^+0.3491P] 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 riding _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 -0.014(12) _refine_ls_number_reflns 6691 _refine_ls_number_parameters 433 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Fe1A Fe 0.15890(3) 0.98929(5) 0.33342(2) 0.03375(10) Uani 1 1 d . . . O1A O 0.32243(14) 0.9830(4) 0.51305(13) 0.0486(5) Uani 1 1 d . . . N1A N 0.13546(19) 1.0438(4) 0.59557(17) 0.0450(6) Uani 1 1 d . . . C1A C 0.2439(2) 0.8870(4) 0.4523(2) 0.0388(6) Uani 1 1 d . . . C2A C 0.1355(2) 0.8922(4) 0.45241(19) 0.0363(6) Uani 1 1 d . . . C3A C 0.0815(2) 0.7815(4) 0.3779(2) 0.0412(7) Uani 1 1 d . . . H3A H 0.0084 0.7593 0.3604 0.049 Uiso 1 1 calc R . . C4A C 0.1581(3) 0.7114(4) 0.3351(2) 0.0453(8) Uani 1 1 d . . . H4A H 0.1441 0.6342 0.2843 0.054 Uiso 1 1 calc R . . C5A C 0.2590(2) 0.7761(4) 0.3811(2) 0.0450(7) Uani 1 1 d . . . H5A H 0.3236 0.7501 0.3669 0.054 Uiso 1 1 calc R . . C6A C 0.0914(2) 0.9991(4) 0.51377(19) 0.0412(6) Uani 1 1 d . . . H6A H 0.0219 1.0411 0.4911 0.049 Uiso 1 1 calc R . . C7A C 0.23740(19) 0.9822(4) 0.63985(18) 0.0373(5) Uani 1 1 d . . . C8A C 0.2539(2) 0.9584(4) 0.73266(19) 0.0428(6) Uani 1 1 d . . . F8A F 0.17361(14) 0.9792(4) 0.77207(11) 0.0622(5) Uani 1 1 d . . . C9A C 0.3511(3) 0.9136(4) 0.7867(2) 0.0483(8) Uani 1 1 d . . . F9A F 0.36359(16) 0.8918(3) 0.87661(13) 0.0692(6) Uani 1 1 d . . . C10A C 0.4350(2) 0.8877(5) 0.7488(2) 0.0489(8) Uani 1 1 d . . . F10A F 0.53051(14) 0.8425(3) 0.80215(16) 0.0734(7) Uani 1 1 d . . . C11A C 0.4221(2) 0.9078(4) 0.6581(2) 0.0478(8) Uani 1 1 d . . . F11A F 0.50478(14) 0.8802(4) 0.62209(15) 0.0752(7) Uani 1 1 d . . . C12A C 0.3246(2) 0.9540(4) 0.60278(19) 0.0397(6) Uani 1 1 d . . . C13A C 0.2172(3) 1.2438(4) 0.3169(2) 0.0482(8) Uani 1 1 d . . . H13A H 0.2727 1.3034 0.3578 0.058 Uiso 1 1 calc R . . C14A C 0.1094(3) 1.2562(4) 0.3154(2) 0.0465(8) Uani 1 1 d . . . H14A H 0.0803 1.3258 0.3552 0.056 Uiso 1 1 calc R . . C15A C 0.0520(3) 1.1456(4) 0.2436(2) 0.0471(8) Uani 1 1 d . . . H15A H -0.0216 1.1295 0.2274 0.057 Uiso 1 1 calc R . . C16A C 0.1252(3) 1.0634(5) 0.2004(2) 0.0470(7) Uani 1 1 d . . . H16A H 0.1089 0.9827 0.1510 0.056 Uiso 1 1 calc R . . C17A C 0.2277(3) 1.1254(4) 0.2455(2) 0.0460(7) Uani 1 1 d . . . H17A H 0.2913 1.0938 0.2308 0.055 Uiso 1 1 calc R . . Fe1B Fe 0.78656(3) 0.96305(5) -0.00140(2) 0.03455(10) Uani 1 1 d . . . O1B O 0.77503(14) 1.0131(3) 0.19121(13) 0.0389(4) Uani 1 1 d . . . N1B N 0.53914(18) 0.9341(4) 0.12586(17) 0.0506(7) Uani 1 1 d . . . C1B C 0.7735(2) 0.8880(4) 0.12243(18) 0.0352(6) Uani 1 1 d . . . C2B C 0.6807(2) 0.8355(4) 0.05712(19) 0.0394(6) Uani 1 1 d . . . C3B C 0.7139(3) 0.7151(4) -0.0047(2) 0.0464(8) Uani 1 1 d . . . H3B H 0.6700 0.6598 -0.0559 0.056 Uiso 1 1 calc R . . C4B C 0.8243(3) 0.6945(4) 0.0252(2) 0.0485(8) Uani 1 1 d . . . H4B H 0.8662 0.6215 -0.0031 0.058 Uiso 1 1 calc R . . C5B C 0.8627(2) 0.8003(4) 0.1041(2) 0.0416(7) Uani 1 1 d . . . H5B H 0.9331 0.8103 0.1377 0.050 Uiso 1 1 calc R . . C6B C 0.5753(2) 0.8927(5) 0.0580(2) 0.0492(8) Uani 1 1 d . . . H6B H 0.5270 0.9005 0.0013 0.059 Uiso 1 1 calc R . . C7B C 0.6020(2) 0.9283(4) 0.21542(19) 0.0388(6) Uani 1 1 d . . . C8B C 0.5475(2) 0.8903(4) 0.2814(2) 0.0448(7) Uani 1 1 d . . . F8B F 0.44437(14) 0.8457(3) 0.25600(14) 0.0667(6) Uani 1 1 d . . . C9B C 0.5935(2) 0.8948(4) 0.3723(2) 0.0475(7) Uani 1 1 d . . . F9B F 0.53799(18) 0.8564(3) 0.43259(15) 0.0749(6) Uani 1 1 d . . . C10B C 0.6980(2) 0.9406(4) 0.40122(19) 0.0446(7) Uani 1 1 d . . . F10B F 0.74598(16) 0.9451(3) 0.48922(11) 0.0656(5) Uani 1 1 d . . . C11B C 0.75547(19) 0.9759(4) 0.33807(17) 0.0366(5) Uani 1 1 d . . . F11B F 0.85811(13) 1.0201(3) 0.36711(12) 0.0528(5) Uani 1 1 d . . . C12B C 0.70977(18) 0.9674(4) 0.24692(16) 0.0332(5) Uani 1 1 d . . . C13B C 0.7180(3) 1.1887(5) -0.0705(2) 0.0549(9) Uani 1 1 d . . . H13B H 0.6475 1.2266 -0.0783 0.066 Uiso 1 1 calc R . . C14B C 0.7560(3) 1.0715(5) -0.1287(2) 0.0504(8) Uani 1 1 d . . . H14B H 0.7156 1.0163 -0.1815 0.060 Uiso 1 1 calc R . . C15B C 0.8658(3) 1.0521(5) -0.0930(2) 0.0475(7) Uani 1 1 d . . . H15B H 0.9116 0.9812 -0.1181 0.057 Uiso 1 1 calc R . . C16B C 0.8948(3) 1.1572(4) -0.0133(2) 0.0503(8) Uani 1 1 d . . . H16B H 0.9635 1.1698 0.0236 0.060 Uiso 1 1 calc R . . C17B C 0.8033(3) 1.2397(5) 0.0012(2) 0.0527(9) Uani 1 1 d . . . H17B H 0.7997 1.3155 0.0501 0.063 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 Fe1A 0.03692(19) 0.0351(2) 0.03047(19) 0.00157(16) 0.01064(15) -0.00208(16) O1A 0.0320(9) 0.0708(14) 0.0414(11) 0.0116(12) 0.0060(8) -0.0054(11) N1A 0.0384(13) 0.0559(15) 0.0381(14) -0.0040(11) 0.0042(11) 0.0121(10) C1A 0.0372(15) 0.0439(15) 0.0364(16) 0.0075(12) 0.0109(12) 0.0021(12) C2A 0.0352(14) 0.0450(15) 0.0318(15) 0.0033(11) 0.0143(12) 0.0000(11) C3A 0.0473(17) 0.0403(15) 0.0389(17) 0.0011(12) 0.0159(14) -0.0093(12) C4A 0.065(2) 0.0309(15) 0.046(2) 0.0006(12) 0.0252(18) -0.0023(13) C5A 0.0470(18) 0.0449(16) 0.0499(19) 0.0096(14) 0.0247(15) 0.0095(13) C6A 0.0329(13) 0.0539(17) 0.0365(14) 0.0014(14) 0.0080(11) 0.0090(13) C7A 0.0367(13) 0.0333(13) 0.0392(14) -0.0039(13) 0.0039(11) 0.0038(12) C8A 0.0444(15) 0.0444(16) 0.0374(15) -0.0079(14) 0.0057(12) 0.0034(13) F8A 0.0577(10) 0.0905(13) 0.0381(9) -0.0109(11) 0.0111(8) 0.0156(12) C9A 0.0537(19) 0.0503(18) 0.0341(17) -0.0008(13) -0.0027(14) -0.0024(13) F9A 0.0657(13) 0.1000(16) 0.0327(10) 0.0017(10) -0.0057(9) 0.0003(11) C10A 0.0356(16) 0.0570(18) 0.0457(19) 0.0096(14) -0.0064(14) -0.0034(13) F10A 0.0390(11) 0.1029(17) 0.0643(14) 0.0241(13) -0.0143(10) -0.0012(10) C11A 0.0289(15) 0.062(2) 0.0495(19) 0.0122(15) 0.0044(13) -0.0026(13) F11A 0.0303(10) 0.125(2) 0.0703(15) 0.0251(13) 0.0133(10) 0.0073(11) C12A 0.0328(13) 0.0444(15) 0.0385(14) 0.0048(13) 0.0025(11) -0.0025(12) C13A 0.054(2) 0.0435(17) 0.0434(19) 0.0071(14) 0.0045(15) -0.0113(14) C14A 0.059(2) 0.0353(16) 0.047(2) 0.0028(13) 0.0168(16) 0.0024(14) C15A 0.0390(17) 0.0494(18) 0.0480(19) 0.0121(14) 0.0012(14) -0.0003(12) C16A 0.059(2) 0.0518(18) 0.0293(16) 0.0055(13) 0.0085(14) -0.0041(14) C17A 0.0460(18) 0.0510(18) 0.0439(18) 0.0134(13) 0.0168(15) -0.0027(13) Fe1B 0.03552(19) 0.0386(2) 0.03128(19) 0.00203(17) 0.01154(15) -0.00223(17) O1B 0.0317(9) 0.0544(12) 0.0311(10) -0.0047(8) 0.0087(8) -0.0110(8) N1B 0.0287(11) 0.083(2) 0.0378(14) 0.0017(13) 0.0042(10) -0.0030(12) C1B 0.0359(14) 0.0427(14) 0.0276(14) 0.0053(11) 0.0090(11) -0.0044(11) C2B 0.0371(15) 0.0498(16) 0.0318(15) 0.0026(12) 0.0095(12) -0.0118(12) C3B 0.057(2) 0.0447(17) 0.0402(18) -0.0043(13) 0.0180(15) -0.0151(14) C4B 0.064(2) 0.0345(16) 0.054(2) 0.0008(14) 0.0281(18) 0.0006(14) C5B 0.0415(16) 0.0409(15) 0.0440(18) 0.0098(12) 0.0136(14) 0.0022(12) C6B 0.0333(15) 0.079(2) 0.0323(16) 0.0038(14) 0.0017(13) -0.0098(14) C7B 0.0347(14) 0.0480(16) 0.0347(15) -0.0001(12) 0.0102(12) 0.0025(11) C8B 0.0346(15) 0.0555(17) 0.0476(19) -0.0018(14) 0.0163(13) -0.0016(13) F8B 0.0366(10) 0.1081(17) 0.0609(13) -0.0037(12) 0.0227(9) -0.0132(10) C9B 0.0512(18) 0.0554(18) 0.0429(18) 0.0008(14) 0.0248(15) -0.0026(14) F9B 0.0816(15) 0.1028(17) 0.0541(13) 0.0030(12) 0.0434(12) -0.0113(13) C10B 0.0600(18) 0.0442(16) 0.0288(14) -0.0027(12) 0.0094(13) 0.0025(13) F10B 0.0848(13) 0.0827(14) 0.0272(9) -0.0024(9) 0.0095(9) -0.0044(12) C11B 0.0355(13) 0.0386(13) 0.0330(13) -0.0031(13) 0.0031(10) -0.0002(13) F11B 0.0409(9) 0.0698(13) 0.0408(10) -0.0071(8) -0.0034(7) -0.0075(8) C12B 0.0320(12) 0.0371(13) 0.0307(12) 0.0011(12) 0.0080(10) 0.0004(12) C13B 0.048(2) 0.061(2) 0.060(2) 0.0257(17) 0.0212(17) 0.0144(15) C14B 0.055(2) 0.0616(19) 0.0344(17) 0.0117(14) 0.0097(15) -0.0054(16) C15B 0.0479(18) 0.0534(18) 0.0479(19) 0.0119(14) 0.0249(15) 0.0019(13) C16B 0.0467(19) 0.0539(19) 0.050(2) 0.0104(15) 0.0115(16) -0.0146(14) C17B 0.081(3) 0.0354(17) 0.048(2) 0.0046(13) 0.029(2) -0.0003(15) _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 Fe1A C1A 2.024(3) . ? Fe1A C4A 2.026(3) . ? Fe1A C3A 2.027(3) . ? Fe1A C2A 2.041(3) . ? Fe1A C16A 2.043(3) . ? Fe1A C13A 2.044(3) . ? Fe1A C17A 2.045(3) . ? Fe1A C14A 2.047(3) . ? Fe1A C15A 2.047(3) . ? Fe1A C5A 2.047(3) . ? O1A C12A 1.380(3) . ? O1A C1A 1.392(4) . ? N1A C6A 1.283(4) . ? N1A C7A 1.411(3) . ? C1A C5A 1.407(4) . ? C1A C2A 1.416(4) . ? C2A C3A 1.432(4) . ? C2A C6A 1.442(4) . ? C3A C4A 1.416(4) . ? C4A C5A 1.414(5) . ? C7A C8A 1.391(4) . ? C7A C12A 1.405(4) . ? C8A F8A 1.339(3) . ? C8A C9A 1.373(4) . ? C9A F9A 1.351(4) . ? C9A C10A 1.371(5) . ? C10A F10A 1.353(3) . ? C10A C11A 1.362(5) . ? C11A F11A 1.342(4) . ? C11A C12A 1.387(4) . ? C13A C14A 1.405(5) . ? C13A C17A 1.423(5) . ? C14A C15A 1.419(5) . ? C15A C16A 1.419(5) . ? C16A C17A 1.421(4) . ? Fe1B C1B 2.015(3) . ? Fe1B C17B 2.028(3) . ? Fe1B C4B 2.035(3) . ? Fe1B C3B 2.036(3) . ? Fe1B C15B 2.038(3) . ? Fe1B C16B 2.040(3) . ? Fe1B C13B 2.040(3) . ? Fe1B C2B 2.043(3) . ? Fe1B C14B 2.045(3) . ? Fe1B C5B 2.052(3) . ? O1B C12B 1.384(3) . ? O1B C1B 1.387(3) . ? N1B C6B 1.275(4) . ? N1B C7B 1.413(4) . ? C1B C5B 1.415(4) . ? C1B C2B 1.420(4) . ? C2B C3B 1.432(4) . ? C2B C6B 1.441(4) . ? C3B C4B 1.410(5) . ? C4B C5B 1.416(5) . ? C7B C8B 1.396(4) . ? C7B C12B 1.400(4) . ? C8B F8B 1.347(3) . ? C8B C9B 1.372(4) . ? C9B F9B 1.333(3) . ? C9B C10B 1.369(4) . ? C10B F10B 1.337(3) . ? C10B C11B 1.383(4) . ? C11B F11B 1.344(3) . ? C11B C12B 1.375(3) . ? C13B C17B 1.409(5) . ? C13B C14B 1.407(5) . ? C14B C15B 1.411(4) . ? C15B C16B 1.409(5) . ? C16B C17B 1.402(5) . ? 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 C1A Fe1A C4A 67.89(13) . . ? C1A Fe1A C3A 68.50(12) . . ? C4A Fe1A C3A 40.88(12) . . ? C1A Fe1A C2A 40.78(11) . . ? C4A Fe1A C2A 68.87(12) . . ? C3A Fe1A C2A 41.23(12) . . ? C1A Fe1A C16A 157.90(13) . . ? C4A Fe1A C16A 106.07(14) . . ? C3A Fe1A C16A 121.77(13) . . ? C2A Fe1A C16A 159.04(12) . . ? C1A Fe1A C13A 107.83(13) . . ? C4A Fe1A C13A 155.82(14) . . ? C3A Fe1A C13A 161.90(13) . . ? C2A Fe1A C13A 124.47(13) . . ? C16A Fe1A C13A 68.48(13) . . ? C1A Fe1A C17A 122.32(12) . . ? C4A Fe1A C17A 119.87(13) . . ? C3A Fe1A C17A 156.46(13) . . ? C2A Fe1A C17A 159.67(12) . . ? C16A Fe1A C17A 40.68(13) . . ? C13A Fe1A C17A 40.71(14) . . ? C1A Fe1A C14A 123.81(13) . . ? C4A Fe1A C14A 161.71(14) . . ? C3A Fe1A C14A 126.05(13) . . ? C2A Fe1A C14A 109.76(12) . . ? C16A Fe1A C14A 68.32(14) . . ? C13A Fe1A C14A 40.16(13) . . ? C17A Fe1A C14A 68.01(13) . . ? C1A Fe1A C15A 160.11(13) . . ? C4A Fe1A C15A 124.07(13) . . ? C3A Fe1A C15A 109.04(13) . . ? C2A Fe1A C15A 124.29(13) . . ? C16A Fe1A C15A 40.60(13) . . ? C13A Fe1A C15A 68.01(13) . . ? C17A Fe1A C15A 68.11(13) . . ? C14A Fe1A C15A 40.54(13) . . ? C1A Fe1A C5A 40.43(12) . . ? C4A Fe1A C5A 40.63(13) . . ? C3A Fe1A C5A 68.95(12) . . ? C2A Fe1A C5A 69.01(11) . . ? C16A Fe1A C5A 121.21(13) . . ? C13A Fe1A C5A 120.55(13) . . ? C17A Fe1A C5A 104.89(13) . . ? C14A Fe1A C5A 157.30(14) . . ? C15A Fe1A C5A 158.81(14) . . ? C12A O1A C1A 114.7(2) . . ? C6A N1A C7A 122.1(2) . . ? O1A C1A C5A 125.7(3) . . ? O1A C1A C2A 124.0(3) . . ? C5A C1A C2A 110.2(3) . . ? O1A C1A Fe1A 124.45(19) . . ? C5A C1A Fe1A 70.65(17) . . ? C2A C1A Fe1A 70.26(16) . . ? C1A C2A C3A 106.3(2) . . ? C1A C2A C6A 124.9(3) . . ? C3A C2A C6A 128.6(3) . . ? C1A C2A Fe1A 68.97(15) . . ? C3A C2A Fe1A 68.87(16) . . ? C6A C2A Fe1A 124.2(2) . . ? C4A C3A C2A 107.7(3) . . ? C4A C3A Fe1A 69.50(17) . . ? C2A C3A Fe1A 69.90(16) . . ? C5A C4A C3A 109.2(3) . . ? C5A C4A Fe1A 70.48(18) . . ? C3A C4A Fe1A 69.62(18) . . ? C1A C5A C4A 106.6(3) . . ? C1A C5A Fe1A 68.92(16) . . ? C4A C5A Fe1A 68.89(18) . . ? N1A C6A C2A 127.9(3) . . ? C8A C7A C12A 116.9(2) . . ? C8A C7A N1A 114.9(2) . . ? C12A C7A N1A 128.0(2) . . ? F8A C8A C9A 117.8(3) . . ? F8A C8A C7A 120.0(2) . . ? C9A C8A C7A 122.2(3) . . ? F9A C9A C10A 120.1(3) . . ? F9A C9A C8A 120.3(3) . . ? C10A C9A C8A 119.6(3) . . ? F10A C10A C11A 120.3(3) . . ? F10A C10A C9A 119.6(3) . . ? C11A C10A C9A 120.1(3) . . ? F11A C11A C10A 119.3(3) . . ? F11A C11A C12A 119.9(3) . . ? C10A C11A C12A 120.9(3) . . ? O1A C12A C11A 115.8(2) . . ? O1A C12A C7A 123.8(2) . . ? C11A C12A C7A 120.2(3) . . ? C14A C13A C17A 108.1(3) . . ? C14A C13A Fe1A 70.03(17) . . ? C17A C13A Fe1A 69.68(17) . . ? C13A C14A C15A 108.3(3) . . ? C13A C14A Fe1A 69.81(18) . . ? C15A C14A Fe1A 69.74(18) . . ? C14A C15A C16A 108.1(3) . . ? C14A C15A Fe1A 69.72(18) . . ? C16A C15A Fe1A 69.52(18) . . ? C15A C16A C17A 107.6(3) . . ? C15A C16A Fe1A 69.88(18) . . ? C17A C16A Fe1A 69.76(17) . . ? C16A C17A C13A 107.9(3) . . ? C16A C17A Fe1A 69.57(17) . . ? C13A C17A Fe1A 69.61(18) . . ? C1B Fe1B C17B 106.55(13) . . ? C1B Fe1B C4B 67.91(13) . . ? C17B Fe1B C4B 158.88(15) . . ? C1B Fe1B C3B 68.70(12) . . ? C17B Fe1B C3B 158.54(15) . . ? C4B Fe1B C3B 40.53(13) . . ? C1B Fe1B C15B 154.67(12) . . ? C17B Fe1B C15B 68.06(14) . . ? C4B Fe1B C15B 107.71(13) . . ? C3B Fe1B C15B 125.24(14) . . ? C1B Fe1B C16B 119.43(13) . . ? C17B Fe1B C16B 40.34(14) . . ? C4B Fe1B C16B 123.07(14) . . ? C3B Fe1B C16B 160.50(14) . . ? C15B Fe1B C16B 40.45(14) . . ? C1B Fe1B C13B 125.25(13) . . ? C17B Fe1B C13B 40.53(15) . . ? C4B Fe1B C13B 158.94(16) . . ? C3B Fe1B C13B 124.04(15) . . ? C15B Fe1B C13B 67.70(13) . . ? C16B Fe1B C13B 67.71(14) . . ? C1B Fe1B C2B 40.96(11) . . ? C17B Fe1B C2B 121.68(13) . . ? C4B Fe1B C2B 68.41(13) . . ? C3B Fe1B C2B 41.09(12) . . ? C15B Fe1B C2B 162.88(13) . . ? C16B Fe1B C2B 155.80(13) . . ? C13B Fe1B C2B 109.55(13) . . ? C1B Fe1B C14B 162.71(12) . . ? C17B Fe1B C14B 68.24(15) . . ? C4B Fe1B C14B 122.89(15) . . ? C3B Fe1B C14B 109.75(14) . . ? C15B Fe1B C14B 40.44(12) . . ? C16B Fe1B C14B 68.03(14) . . ? C13B Fe1B C14B 40.29(14) . . ? C2B Fe1B C14B 126.54(12) . . ? C1B Fe1B C5B 40.70(11) . . ? C17B Fe1B C5B 122.02(14) . . ? C4B Fe1B C5B 40.54(13) . . ? C3B Fe1B C5B 68.88(13) . . ? C15B Fe1B C5B 119.58(13) . . ? C16B Fe1B C5B 104.94(13) . . ? C13B Fe1B C5B 160.04(14) . . ? C2B Fe1B C5B 69.08(12) . . ? C14B Fe1B C5B 156.17(13) . . ? C12B O1B C1B 114.2(2) . . ? C6B N1B C7B 122.4(3) . . ? O1B C1B C5B 125.8(2) . . ? O1B C1B C2B 124.1(2) . . ? C5B C1B C2B 110.0(3) . . ? O1B C1B Fe1B 122.90(19) . . ? C5B C1B Fe1B 71.03(17) . . ? C2B C1B Fe1B 70.58(16) . . ? C1B C2B C3B 106.6(3) . . ? C1B C2B C6B 124.6(3) . . ? C3B C2B C6B 128.8(3) . . ? C1B C2B Fe1B 68.46(15) . . ? C3B C2B Fe1B 69.20(16) . . ? C6B C2B Fe1B 128.5(2) . . ? C4B C3B C2B 107.6(3) . . ? C4B C3B Fe1B 69.70(17) . . ? C2B C3B Fe1B 69.72(16) . . ? C3B C4B C5B 109.8(3) . . ? C3B C4B Fe1B 69.77(18) . . ? C5B C4B Fe1B 70.34(17) . . ? C4B C5B C1B 106.1(3) . . ? C4B C5B Fe1B 69.11(18) . . ? C1B C5B Fe1B 68.26(16) . . ? N1B C6B C2B 128.3(3) . . ? C8B C7B C12B 116.1(3) . . ? C8B C7B N1B 115.2(2) . . ? C12B C7B N1B 128.6(2) . . ? F8B C8B C9B 117.2(3) . . ? F8B C8B C7B 119.3(3) . . ? C9B C8B C7B 123.4(3) . . ? F9B C9B C10B 119.8(3) . . ? F9B C9B C8B 121.0(3) . . ? C10B C9B C8B 119.2(3) . . ? F10B C10B C9B 121.0(3) . . ? F10B C10B C11B 119.7(3) . . ? C9B C10B C11B 119.2(3) . . ? F11B C11B C12B 119.7(2) . . ? F11B C11B C10B 118.8(2) . . ? C12B C11B C10B 121.5(2) . . ? C11B C12B O1B 115.5(2) . . ? C11B C12B C7B 120.5(2) . . ? O1B C12B C7B 123.8(2) . . ? C17B C13B C14B 108.4(3) . . ? C17B C13B Fe1B 69.27(19) . . ? C14B C13B Fe1B 70.04(19) . . ? C13B C14B C15B 107.4(3) . . ? C13B C14B Fe1B 69.67(18) . . ? C15B C14B Fe1B 69.52(17) . . ? C16B C15B C14B 108.2(3) . . ? C16B C15B Fe1B 69.84(18) . . ? C14B C15B Fe1B 70.04(17) . . ? C17B C16B C15B 108.0(3) . . ? C17B C16B Fe1B 69.38(19) . . ? C15B C16B Fe1B 69.71(18) . . ? C16B C17B C13B 107.9(3) . . ? C16B C17B Fe1B 70.3(2) . . ? C13B C17B Fe1B 70.2(2) . . ? 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 C12A O1A C1A C5A -128.8(3) . . . . ? C12A O1A C1A C2A 53.0(4) . . . . ? C12A O1A C1A Fe1A 141.2(2) . . . . ? C4A Fe1A C1A O1A 158.8(3) . . . . ? C3A Fe1A C1A O1A -157.0(3) . . . . ? C2A Fe1A C1A O1A -118.3(3) . . . . ? C16A Fe1A C1A O1A 80.7(4) . . . . ? C13A Fe1A C1A O1A 4.2(3) . . . . ? C17A Fe1A C1A O1A 46.5(3) . . . . ? C14A Fe1A C1A O1A -37.2(3) . . . . ? C15A Fe1A C1A O1A -70.3(4) . . . . ? C5A Fe1A C1A O1A 120.6(3) . . . . ? C4A Fe1A C1A C5A 38.17(18) . . . . ? C3A Fe1A C1A C5A 82.36(19) . . . . ? C2A Fe1A C1A C5A 121.0(2) . . . . ? C16A Fe1A C1A C5A -39.9(4) . . . . ? C13A Fe1A C1A C5A -116.5(2) . . . . ? C17A Fe1A C1A C5A -74.1(2) . . . . ? C14A Fe1A C1A C5A -157.81(19) . . . . ? C15A Fe1A C1A C5A 169.0(3) . . . . ? C4A Fe1A C1A C2A -82.84(18) . . . . ? C3A Fe1A C1A C2A -38.65(17) . . . . ? C16A Fe1A C1A C2A -160.9(3) . . . . ? C13A Fe1A C1A C2A 122.51(18) . . . . ? C17A Fe1A C1A C2A 164.89(18) . . . . ? C14A Fe1A C1A C2A 81.2(2) . . . . ? C15A Fe1A C1A C2A 48.0(4) . . . . ? C5A Fe1A C1A C2A -121.0(2) . . . . ? O1A C1A C2A C3A 177.9(3) . . . . ? C5A C1A C2A C3A -0.5(3) . . . . ? Fe1A C1A C2A C3A 58.99(19) . . . . ? O1A C1A C2A C6A 1.1(4) . . . . ? C5A C1A C2A C6A -177.2(3) . . . . ? Fe1A C1A C2A C6A -117.7(3) . . . . ? O1A C1A C2A Fe1A 118.9(3) . . . . ? C5A C1A C2A Fe1A -59.5(2) . . . . ? C4A Fe1A C2A C1A 80.22(19) . . . . ? C3A Fe1A C2A C1A 118.1(2) . . . . ? C16A Fe1A C2A C1A 159.9(3) . . . . ? C13A Fe1A C2A C1A -76.9(2) . . . . ? C17A Fe1A C2A C1A -39.4(4) . . . . ? C14A Fe1A C2A C1A -119.26(18) . . . . ? C15A Fe1A C2A C1A -162.17(18) . . . . ? C5A Fe1A C2A C1A 36.54(18) . . . . ? C1A Fe1A C2A C3A -118.1(2) . . . . ? C4A Fe1A C2A C3A -37.92(18) . . . . ? C16A Fe1A C2A C3A 41.8(4) . . . . ? C13A Fe1A C2A C3A 165.01(19) . . . . ? C17A Fe1A C2A C3A -157.5(3) . . . . ? C14A Fe1A C2A C3A 122.60(19) . . . . ? C15A Fe1A C2A C3A 79.7(2) . . . . ? C5A Fe1A C2A C3A -81.60(19) . . . . ? C1A Fe1A C2A C6A 118.7(3) . . . . ? C4A Fe1A C2A C6A -161.1(3) . . . . ? C3A Fe1A C2A C6A -123.1(3) . . . . ? C16A Fe1A C2A C6A -81.4(4) . . . . ? C13A Fe1A C2A C6A 41.9(3) . . . . ? C17A Fe1A C2A C6A 79.4(4) . . . . ? C14A Fe1A C2A C6A -0.5(3) . . . . ? C15A Fe1A C2A C6A -43.4(3) . . . . ? C5A Fe1A C2A C6A 155.3(3) . . . . ? C1A C2A C3A C4A 0.4(3) . . . . ? C6A C2A C3A C4A 176.9(3) . . . . ? Fe1A C2A C3A C4A 59.4(2) . . . . ? C1A C2A C3A Fe1A -59.05(19) . . . . ? C6A C2A C3A Fe1A 117.5(3) . . . . ? C1A Fe1A C3A C4A -80.6(2) . . . . ? C2A Fe1A C3A C4A -118.9(3) . . . . ? C16A Fe1A C3A C4A 77.4(2) . . . . ? C13A Fe1A C3A C4A -162.2(4) . . . . ? C17A Fe1A C3A C4A 41.7(4) . . . . ? C14A Fe1A C3A C4A 162.5(2) . . . . ? C15A Fe1A C3A C4A 120.4(2) . . . . ? C5A Fe1A C3A C4A -37.08(19) . . . . ? C1A Fe1A C3A C2A 38.24(17) . . . . ? C4A Fe1A C3A C2A 118.9(3) . . . . ? C16A Fe1A C3A C2A -163.73(17) . . . . ? C13A Fe1A C3A C2A -43.4(5) . . . . ? C17A Fe1A C3A C2A 160.6(3) . . . . ? C14A Fe1A C3A C2A -78.7(2) . . . . ? C15A Fe1A C3A C2A -120.70(18) . . . . ? C5A Fe1A C3A C2A 81.78(19) . . . . ? C2A C3A C4A C5A -0.1(3) . . . . ? Fe1A C3A C4A C5A 59.6(2) . . . . ? C2A C3A C4A Fe1A -59.7(2) . . . . ? C1A Fe1A C4A C5A -37.99(17) . . . . ? C3A Fe1A C4A C5A -120.2(3) . . . . ? C2A Fe1A C4A C5A -81.99(19) . . . . ? C16A Fe1A C4A C5A 119.49(19) . . . . ? C13A Fe1A C4A C5A 46.4(4) . . . . ? C17A Fe1A C4A C5A 77.6(2) . . . . ? C14A Fe1A C4A C5A -171.2(4) . . . . ? C15A Fe1A C4A C5A 160.11(19) . . . . ? C1A Fe1A C4A C3A 82.24(19) . . . . ? C2A Fe1A C4A C3A 38.23(18) . . . . ? C16A Fe1A C4A C3A -120.29(19) . . . . ? C13A Fe1A C4A C3A 166.6(3) . . . . ? C17A Fe1A C4A C3A -162.15(18) . . . . ? C14A Fe1A C4A C3A -51.0(5) . . . . ? C15A Fe1A C4A C3A -79.7(2) . . . . ? C5A Fe1A C4A C3A 120.2(3) . . . . ? O1A C1A C5A C4A -177.9(3) . . . . ? C2A C1A C5A C4A 0.4(3) . . . . ? Fe1A C1A C5A C4A -58.8(2) . . . . ? O1A C1A C5A Fe1A -119.1(3) . . . . ? C2A C1A C5A Fe1A 59.3(2) . . . . ? C3A C4A C5A C1A -0.2(3) . . . . ? Fe1A C4A C5A C1A 58.9(2) . . . . ? C3A C4A C5A Fe1A -59.0(2) . . . . ? C4A Fe1A C5A C1A -118.5(2) . . . . ? C3A Fe1A C5A C1A -81.15(18) . . . . ? C2A Fe1A C5A C1A -36.84(17) . . . . ? C16A Fe1A C5A C1A 163.60(17) . . . . ? C13A Fe1A C5A C1A 81.7(2) . . . . ? C17A Fe1A C5A C1A 122.76(18) . . . . ? C14A Fe1A C5A C1A 54.4(4) . . . . ? C15A Fe1A C5A C1A -169.7(3) . . . . ? C1A Fe1A C5A C4A 118.5(2) . . . . ? C3A Fe1A C5A C4A 37.30(18) . . . . ? C2A Fe1A C5A C4A 81.62(19) . . . . ? C16A Fe1A C5A C4A -77.9(2) . . . . ? C13A Fe1A C5A C4A -159.86(19) . . . . ? C17A Fe1A C5A C4A -118.78(19) . . . . ? C14A Fe1A C5A C4A 172.8(3) . . . . ? C15A Fe1A C5A C4A -51.2(4) . . . . ? C7A N1A C6A C2A -3.4(5) . . . . ? C1A C2A C6A N1A -30.9(5) . . . . ? C3A C2A C6A N1A 153.1(3) . . . . ? Fe1A C2A C6A N1A -117.8(3) . . . . ? C6A N1A C7A C8A -148.8(3) . . . . ? C6A N1A C7A C12A 35.6(5) . . . . ? C12A C7A C8A F8A -178.5(3) . . . . ? N1A C7A C8A F8A 5.4(4) . . . . ? C12A C7A C8A C9A 1.5(5) . . . . ? N1A C7A C8A C9A -174.6(3) . . . . ? F8A C8A C9A F9A 0.0(5) . . . . ? C7A C8A C9A F9A 180.0(3) . . . . ? F8A C8A C9A C10A 178.8(3) . . . . ? C7A C8A C9A C10A -1.2(5) . . . . ? F9A C9A C10A F10A -0.8(5) . . . . ? C8A C9A C10A F10A -179.6(3) . . . . ? F9A C9A C10A C11A 179.3(3) . . . . ? C8A C9A C10A C11A 0.5(5) . . . . ? F10A C10A C11A F11A 0.8(5) . . . . ? C9A C10A C11A F11A -179.3(3) . . . . ? F10A C10A C11A C12A 180.0(3) . . . . ? C9A C10A C11A C12A -0.2(5) . . . . ? C1A O1A C12A C11A 129.4(3) . . . . ? C1A O1A C12A C7A -55.5(4) . . . . ? F11A C11A C12A O1A -5.1(4) . . . . ? C10A C11A C12A O1A 175.7(3) . . . . ? F11A C11A C12A C7A 179.6(3) . . . . ? C10A C11A C12A C7A 0.5(5) . . . . ? C8A C7A C12A O1A -175.9(3) . . . . ? N1A C7A C12A O1A -0.4(5) . . . . ? C8A C7A C12A C11A -1.1(4) . . . . ? N1A C7A C12A C11A 174.4(3) . . . . ? C1A Fe1A C13A C14A -121.7(2) . . . . ? C4A Fe1A C13A C14A 162.7(3) . . . . ? C3A Fe1A C13A C14A -46.5(5) . . . . ? C2A Fe1A C13A C14A -79.8(2) . . . . ? C16A Fe1A C13A C14A 81.5(2) . . . . ? C17A Fe1A C13A C14A 119.1(3) . . . . ? C15A Fe1A C13A C14A 37.6(2) . . . . ? C5A Fe1A C13A C14A -164.07(19) . . . . ? C1A Fe1A C13A C17A 119.2(2) . . . . ? C4A Fe1A C13A C17A 43.6(4) . . . . ? C3A Fe1A C13A C17A -165.6(4) . . . . ? C2A Fe1A C13A C17A 161.09(18) . . . . ? C16A Fe1A C13A C17A -37.67(19) . . . . ? C14A Fe1A C13A C17A -119.1(3) . . . . ? C15A Fe1A C13A C17A -81.5(2) . . . . ? C5A Fe1A C13A C17A 76.8(2) . . . . ? C17A C13A C14A C15A 0.2(4) . . . . ? Fe1A C13A C14A C15A -59.3(2) . . . . ? C17A C13A C14A Fe1A 59.5(2) . . . . ? C1A Fe1A C14A C13A 77.1(2) . . . . ? C4A Fe1A C14A C13A -157.2(4) . . . . ? C3A Fe1A C14A C13A 163.82(19) . . . . ? C2A Fe1A C14A C13A 120.4(2) . . . . ? C16A Fe1A C14A C13A -81.9(2) . . . . ? C17A Fe1A C14A C13A -37.9(2) . . . . ? C15A Fe1A C14A C13A -119.5(3) . . . . ? C5A Fe1A C14A C13A 37.8(4) . . . . ? C1A Fe1A C14A C15A -163.36(18) . . . . ? C4A Fe1A C14A C15A -37.7(5) . . . . ? C3A Fe1A C14A C15A -76.7(2) . . . . ? C2A Fe1A C14A C15A -120.1(2) . . . . ? C16A Fe1A C14A C15A 37.60(19) . . . . ? C13A Fe1A C14A C15A 119.5(3) . . . . ? C17A Fe1A C14A C15A 81.6(2) . . . . ? C5A Fe1A C14A C15A 157.2(3) . . . . ? C13A C14A C15A C16A 0.2(4) . . . . ? Fe1A C14A C15A C16A -59.2(2) . . . . ? C13A C14A C15A Fe1A 59.4(2) . . . . ? C1A Fe1A C15A C14A 44.4(4) . . . . ? C4A Fe1A C15A C14A 166.60(18) . . . . ? C3A Fe1A C15A C14A 123.66(19) . . . . ? C2A Fe1A C15A C14A 80.3(2) . . . . ? C16A Fe1A C15A C14A -119.4(3) . . . . ? C13A Fe1A C15A C14A -37.3(2) . . . . ? C17A Fe1A C15A C14A -81.3(2) . . . . ? C5A Fe1A C15A C14A -155.6(3) . . . . ? C1A Fe1A C15A C16A 163.8(3) . . . . ? C4A Fe1A C15A C16A -74.0(2) . . . . ? C3A Fe1A C15A C16A -116.95(19) . . . . ? C2A Fe1A C15A C16A -160.26(18) . . . . ? C13A Fe1A C15A C16A 82.1(2) . . . . ? C17A Fe1A C15A C16A 38.08(19) . . . . ? C14A Fe1A C15A C16A 119.4(3) . . . . ? C5A Fe1A C15A C16A -36.2(4) . . . . ? C14A C15A C16A C17A -0.5(3) . . . . ? Fe1A C15A C16A C17A -59.8(2) . . . . ? C14A C15A C16A Fe1A 59.3(2) . . . . ? C1A Fe1A C16A C15A -165.3(3) . . . . ? C4A Fe1A C16A C15A 124.03(19) . . . . ? C3A Fe1A C16A C15A 82.4(2) . . . . ? C2A Fe1A C16A C15A 51.3(4) . . . . ? C13A Fe1A C16A C15A -80.9(2) . . . . ? C17A Fe1A C16A C15A -118.6(3) . . . . ? C14A Fe1A C16A C15A -37.55(19) . . . . ? C5A Fe1A C16A C15A 165.54(18) . . . . ? C1A Fe1A C16A C17A -46.8(4) . . . . ? C4A Fe1A C16A C17A -117.4(2) . . . . ? C3A Fe1A C16A C17A -159.05(18) . . . . ? C2A Fe1A C16A C17A 169.9(3) . . . . ? C13A Fe1A C16A C17A 37.7(2) . . . . ? C14A Fe1A C16A C17A 81.0(2) . . . . ? C15A Fe1A C16A C17A 118.6(3) . . . . ? C5A Fe1A C16A C17A -75.9(2) . . . . ? C15A C16A C17A C13A 0.6(3) . . . . ? Fe1A C16A C17A C13A -59.2(2) . . . . ? C15A C16A C17A Fe1A 59.9(2) . . . . ? C14A C13A C17A C16A -0.5(3) . . . . ? Fe1A C13A C17A C16A 59.2(2) . . . . ? C14A C13A C17A Fe1A -59.7(2) . . . . ? C1A Fe1A C17A C16A 161.08(19) . . . . ? C4A Fe1A C17A C16A 79.7(2) . . . . ? C3A Fe1A C17A C16A 49.6(4) . . . . ? C2A Fe1A C17A C16A -169.6(3) . . . . ? C13A Fe1A C17A C16A -119.3(3) . . . . ? C14A Fe1A C17A C16A -81.9(2) . . . . ? C15A Fe1A C17A C16A -38.0(2) . . . . ? C5A Fe1A C17A C16A 120.9(2) . . . . ? C1A Fe1A C17A C13A -79.6(2) . . . . ? C4A Fe1A C17A C13A -161.0(2) . . . . ? C3A Fe1A C17A C13A 168.9(3) . . . . ? C2A Fe1A C17A C13A -50.3(4) . . . . ? C16A Fe1A C17A C13A 119.3(3) . . . . ? C14A Fe1A C17A C13A 37.4(2) . . . . ? C15A Fe1A C17A C13A 81.3(2) . . . . ? C5A Fe1A C17A C13A -119.8(2) . . . . ? C12B O1B C1B C5B -125.8(3) . . . . ? C12B O1B C1B C2B 57.1(3) . . . . ? C12B O1B C1B Fe1B 144.77(19) . . . . ? C17B Fe1B C1B O1B 0.8(2) . . . . ? C4B Fe1B C1B O1B 159.2(3) . . . . ? C3B Fe1B C1B O1B -157.0(3) . . . . ? C15B Fe1B C1B O1B 74.4(4) . . . . ? C16B Fe1B C1B O1B 42.6(3) . . . . ? C13B Fe1B C1B O1B -39.6(3) . . . . ? C2B Fe1B C1B O1B -118.7(3) . . . . ? C14B Fe1B C1B O1B -68.9(5) . . . . ? C5B Fe1B C1B O1B 121.0(3) . . . . ? C17B Fe1B C1B C5B -120.2(2) . . . . ? C4B Fe1B C1B C5B 38.21(19) . . . . ? C3B Fe1B C1B C5B 82.0(2) . . . . ? C15B Fe1B C1B C5B -46.6(4) . . . . ? C16B Fe1B C1B C5B -78.4(2) . . . . ? C13B Fe1B C1B C5B -160.63(19) . . . . ? C2B Fe1B C1B C5B 120.3(3) . . . . ? C14B Fe1B C1B C5B 170.1(4) . . . . ? C17B Fe1B C1B C2B 119.6(2) . . . . ? C4B Fe1B C1B C2B -82.1(2) . . . . ? C3B Fe1B C1B C2B -38.29(18) . . . . ? C15B Fe1B C1B C2B -166.9(3) . . . . ? C16B Fe1B C1B C2B 161.37(18) . . . . ? C13B Fe1B C1B C2B 79.1(2) . . . . ? C14B Fe1B C1B C2B 49.9(5) . . . . ? C5B Fe1B C1B C2B -120.3(3) . . . . ? O1B C1B C2B C3B 176.1(2) . . . . ? C5B C1B C2B C3B -1.4(3) . . . . ? Fe1B C1B C2B C3B 58.95(19) . . . . ? O1B C1B C2B C6B -5.5(4) . . . . ? C5B C1B C2B C6B 177.0(3) . . . . ? Fe1B C1B C2B C6B -122.7(3) . . . . ? O1B C1B C2B Fe1B 117.2(3) . . . . ? C5B C1B C2B Fe1B -60.3(2) . . . . ? C17B Fe1B C2B C1B -78.4(2) . . . . ? C4B Fe1B C2B C1B 80.7(2) . . . . ? C3B Fe1B C2B C1B 118.5(3) . . . . ? C15B Fe1B C2B C1B 160.7(4) . . . . ? C16B Fe1B C2B C1B -42.7(4) . . . . ? C13B Fe1B C2B C1B -121.7(2) . . . . ? C14B Fe1B C2B C1B -163.58(18) . . . . ? C5B Fe1B C2B C1B 37.08(18) . . . . ? C1B Fe1B C2B C3B -118.5(3) . . . . ? C17B Fe1B C2B C3B 163.0(2) . . . . ? C4B Fe1B C2B C3B -37.8(2) . . . . ? C15B Fe1B C2B C3B 42.2(5) . . . . ? C16B Fe1B C2B C3B -161.3(3) . . . . ? C13B Fe1B C2B C3B 119.8(2) . . . . ? C14B Fe1B C2B C3B 77.9(2) . . . . ? C5B Fe1B C2B C3B -81.5(2) . . . . ? C1B Fe1B C2B C6B 117.8(4) . . . . ? C17B Fe1B C2B C6B 39.3(3) . . . . ? C4B Fe1B C2B C6B -161.5(3) . . . . ? C3B Fe1B C2B C6B -123.7(4) . . . . ? C15B Fe1B C2B C6B -81.5(5) . . . . ? C16B Fe1B C2B C6B 75.0(4) . . . . ? C13B Fe1B C2B C6B -3.9(3) . . . . ? C14B Fe1B C2B C6B -45.8(3) . . . . ? C5B Fe1B C2B C6B 154.8(3) . . . . ? C1B C2B C3B C4B 1.2(3) . . . . ? C6B C2B C3B C4B -177.1(3) . . . . ? Fe1B C2B C3B C4B 59.7(2) . . . . ? C1B C2B C3B Fe1B -58.48(19) . . . . ? C6B C2B C3B Fe1B 123.3(3) . . . . ? C1B Fe1B C3B C4B -80.5(2) . . . . ? C17B Fe1B C3B C4B -161.5(4) . . . . ? C15B Fe1B C3B C4B 75.3(2) . . . . ? C16B Fe1B C3B C4B 38.1(5) . . . . ? C13B Fe1B C3B C4B 160.5(2) . . . . ? C2B Fe1B C3B C4B -118.7(3) . . . . ? C14B Fe1B C3B C4B 117.9(2) . . . . ? C5B Fe1B C3B C4B -36.70(19) . . . . ? C1B Fe1B C3B C2B 38.18(17) . . . . ? C17B Fe1B C3B C2B -42.8(5) . . . . ? C4B Fe1B C3B C2B 118.7(3) . . . . ? C15B Fe1B C3B C2B -165.99(18) . . . . ? C16B Fe1B C3B C2B 156.8(4) . . . . ? C13B Fe1B C3B C2B -80.8(2) . . . . ? C14B Fe1B C3B C2B -123.43(19) . . . . ? C5B Fe1B C3B C2B 81.98(19) . . . . ? C2B C3B C4B C5B -0.6(3) . . . . ? Fe1B C3B C4B C5B 59.1(2) . . . . ? C2B C3B C4B Fe1B -59.7(2) . . . . ? C1B Fe1B C4B C3B 82.61(19) . . . . ? C17B Fe1B C4B C3B 161.2(3) . . . . ? C15B Fe1B C4B C3B -124.0(2) . . . . ? C16B Fe1B C4B C3B -165.77(19) . . . . ? C13B Fe1B C4B C3B -50.2(4) . . . . ? C2B Fe1B C4B C3B 38.32(18) . . . . ? C14B Fe1B C4B C3B -82.1(2) . . . . ? C5B Fe1B C4B C3B 121.0(3) . . . . ? C1B Fe1B C4B C5B -38.35(17) . . . . ? C17B Fe1B C4B C5B 40.3(4) . . . . ? C3B Fe1B C4B C5B -121.0(3) . . . . ? C15B Fe1B C4B C5B 115.1(2) . . . . ? C16B Fe1B C4B C5B 73.3(2) . . . . ? C13B Fe1B C4B C5B -171.2(3) . . . . ? C2B Fe1B C4B C5B -82.64(19) . . . . ? C14B Fe1B C4B C5B 156.92(18) . . . . ? C3B C4B C5B C1B -0.3(3) . . . . ? Fe1B C4B C5B C1B 58.48(19) . . . . ? C3B C4B C5B Fe1B -58.8(2) . . . . ? O1B C1B C5B C4B -176.4(2) . . . . ? C2B C1B C5B C4B 1.1(3) . . . . ? Fe1B C1B C5B C4B -59.0(2) . . . . ? O1B C1B C5B Fe1B -117.4(3) . . . . ? C2B C1B C5B Fe1B 60.08(19) . . . . ? C1B Fe1B C5B C4B 118.2(3) . . . . ? C17B Fe1B C5B C4B -164.06(18) . . . . ? C3B Fe1B C5B C4B 36.68(18) . . . . ? C15B Fe1B C5B C4B -82.8(2) . . . . ? C16B Fe1B C5B C4B -123.8(2) . . . . ? C13B Fe1B C5B C4B 170.7(3) . . . . ? C2B Fe1B C5B C4B 80.8(2) . . . . ? C14B Fe1B C5B C4B -54.6(4) . . . . ? C17B Fe1B C5B C1B 77.8(2) . . . . ? C4B Fe1B C5B C1B -118.2(3) . . . . ? C3B Fe1B C5B C1B -81.47(18) . . . . ? C15B Fe1B C5B C1B 159.05(18) . . . . ? C16B Fe1B C5B C1B 118.00(18) . . . . ? C13B Fe1B C5B C1B 52.5(4) . . . . ? C2B Fe1B C5B C1B -37.31(17) . . . . ? C14B Fe1B C5B C1B -172.7(3) . . . . ? C7B N1B C6B C2B -0.3(6) . . . . ? C1B C2B C6B N1B -29.0(5) . . . . ? C3B C2B C6B N1B 149.0(4) . . . . ? Fe1B C2B C6B N1B -117.7(4) . . . . ? C6B N1B C7B C8B -150.8(3) . . . . ? C6B N1B C7B C12B 34.0(5) . . . . ? C12B C7B C8B F8B -177.9(3) . . . . ? N1B C7B C8B F8B 6.2(4) . . . . ? C12B C7B C8B C9B 1.7(4) . . . . ? N1B C7B C8B C9B -174.2(3) . . . . ? F8B C8B C9B F9B 0.0(5) . . . . ? C7B C8B C9B F9B -179.6(3) . . . . ? F8B C8B C9B C10B -179.6(3) . . . . ? C7B C8B C9B C10B 0.8(5) . . . . ? F9B C9B C10B F10B 1.0(5) . . . . ? C8B C9B C10B F10B -179.5(3) . . . . ? F9B C9B C10B C11B 178.5(3) . . . . ? C8B C9B C10B C11B -2.0(5) . . . . ? F10B C10B C11B F11B -2.2(4) . . . . ? C9B C10B C11B F11B -179.8(3) . . . . ? F10B C10B C11B C12B 178.1(3) . . . . ? C9B C10B C11B C12B 0.6(4) . . . . ? F11B C11B C12B O1B -2.2(4) . . . . ? C10B C11B C12B O1B 177.4(3) . . . . ? F11B C11B C12B C7B -177.6(3) . . . . ? C10B C11B C12B C7B 2.1(4) . . . . ? C1B O1B C12B C11B 131.2(3) . . . . ? C1B O1B C12B C7B -53.7(4) . . . . ? C8B C7B C12B C11B -3.1(4) . . . . ? N1B C7B C12B C11B 172.1(3) . . . . ? C8B C7B C12B O1B -178.1(3) . . . . ? N1B C7B C12B O1B -2.8(5) . . . . ? C1B Fe1B C13B C17B 73.2(2) . . . . ? C4B Fe1B C13B C17B -163.2(3) . . . . ? C3B Fe1B C13B C17B 159.75(19) . . . . ? C15B Fe1B C13B C17B -81.9(2) . . . . ? C16B Fe1B C13B C17B -38.0(2) . . . . ? C2B Fe1B C13B C17B 116.2(2) . . . . ? C14B Fe1B C13B C17B -119.8(3) . . . . ? C5B Fe1B C13B C17B 33.8(5) . . . . ? C1B Fe1B C13B C14B -167.02(18) . . . . ? C17B Fe1B C13B C14B 119.8(3) . . . . ? C4B Fe1B C13B C14B -43.4(5) . . . . ? C3B Fe1B C13B C14B -80.4(2) . . . . ? C15B Fe1B C13B C14B 38.0(2) . . . . ? C16B Fe1B C13B C14B 81.8(2) . . . . ? C2B Fe1B C13B C14B -123.9(2) . . . . ? C5B Fe1B C13B C14B 153.6(3) . . . . ? C17B C13B C14B C15B -0.7(4) . . . . ? Fe1B C13B C14B C15B -59.5(2) . . . . ? C17B C13B C14B Fe1B 58.8(2) . . . . ? C1B Fe1B C14B C13B 38.1(5) . . . . ? C17B Fe1B C14B C13B -37.4(2) . . . . ? C4B Fe1B C14B C13B 162.9(2) . . . . ? C3B Fe1B C14B C13B 119.8(2) . . . . ? C15B Fe1B C14B C13B -118.6(3) . . . . ? C16B Fe1B C14B C13B -81.0(2) . . . . ? C2B Fe1B C14B C13B 76.7(3) . . . . ? C5B Fe1B C14B C13B -158.0(3) . . . . ? C1B Fe1B C14B C15B 156.8(4) . . . . ? C17B Fe1B C14B C15B 81.3(2) . . . . ? C4B Fe1B C14B C15B -78.4(2) . . . . ? C3B Fe1B C14B C15B -121.6(2) . . . . ? C16B Fe1B C14B C15B 37.7(2) . . . . ? C13B Fe1B C14B C15B 118.6(3) . . . . ? C2B Fe1B C14B C15B -164.65(19) . . . . ? C5B Fe1B C14B C15B -39.3(4) . . . . ? C13B C14B C15B C16B 0.0(4) . . . . ? Fe1B C14B C15B C16B -59.6(2) . . . . ? C13B C14B C15B Fe1B 59.6(2) . . . . ? C1B Fe1B C15B C16B -44.9(4) . . . . ? C17B Fe1B C15B C16B 37.4(2) . . . . ? C4B Fe1B C15B C16B -120.6(2) . . . . ? C3B Fe1B C15B C16B -161.9(2) . . . . ? C13B Fe1B C15B C16B 81.3(2) . . . . ? C2B Fe1B C15B C16B 165.4(4) . . . . ? C14B Fe1B C15B C16B 119.2(3) . . . . ? C5B Fe1B C15B C16B -78.0(2) . . . . ? C1B Fe1B C15B C14B -164.1(3) . . . . ? C17B Fe1B C15B C14B -81.7(2) . . . . ? C4B Fe1B C15B C14B 120.3(2) . . . . ? C3B Fe1B C15B C14B 79.0(2) . . . . ? C16B Fe1B C15B C14B -119.2(3) . . . . ? C13B Fe1B C15B C14B -37.8(2) . . . . ? C2B Fe1B C15B C14B 46.3(5) . . . . ? C5B Fe1B C15B C14B 162.9(2) . . . . ? C14B C15B C16B C17B 0.8(4) . . . . ? Fe1B C15B C16B C17B -59.0(2) . . . . ? C14B C15B C16B Fe1B 59.8(2) . . . . ? C1B Fe1B C16B C17B -80.9(2) . . . . ? C4B Fe1B C16B C17B -162.3(2) . . . . ? C3B Fe1B C16B C17B 169.1(4) . . . . ? C15B Fe1B C16B C17B 119.4(3) . . . . ? C13B Fe1B C16B C17B 38.2(2) . . . . ? C2B Fe1B C16B C17B -50.1(4) . . . . ? C14B Fe1B C16B C17B 81.8(2) . . . . ? C5B Fe1B C16B C17B -122.2(2) . . . . ? C1B Fe1B C16B C15B 159.70(18) . . . . ? C17B Fe1B C16B C15B -119.4(3) . . . . ? C4B Fe1B C16B C15B 78.2(2) . . . . ? C3B Fe1B C16B C15B 49.6(5) . . . . ? C13B Fe1B C16B C15B -81.3(2) . . . . ? C2B Fe1B C16B C15B -169.6(3) . . . . ? C14B Fe1B C16B C15B -37.64(19) . . . . ? C5B Fe1B C16B C15B 118.3(2) . . . . ? C15B C16B C17B C13B -1.2(4) . . . . ? Fe1B C16B C17B C13B -60.4(2) . . . . ? C15B C16B C17B Fe1B 59.2(2) . . . . ? C14B C13B C17B C16B 1.2(4) . . . . ? Fe1B C13B C17B C16B 60.5(2) . . . . ? C14B C13B C17B Fe1B -59.3(2) . . . . ? C1B Fe1B C17B C16B 116.2(2) . . . . ? C4B Fe1B C17B C16B 44.8(4) . . . . ? C3B Fe1B C17B C16B -170.0(3) . . . . ? C15B Fe1B C17B C16B -37.5(2) . . . . ? C13B Fe1B C17B C16B -118.4(3) . . . . ? C2B Fe1B C17B C16B 158.30(19) . . . . ? C14B Fe1B C17B C16B -81.2(2) . . . . ? C5B Fe1B C17B C16B 74.5(2) . . . . ? C1B Fe1B C17B C13B -125.4(2) . . . . ? C4B Fe1B C17B C13B 163.2(3) . . . . ? C3B Fe1B C17B C13B -51.6(5) . . . . ? C15B Fe1B C17B C13B 80.9(2) . . . . ? C16B Fe1B C17B C13B 118.4(3) . . . . ? C2B Fe1B C17B C13B -83.3(2) . . . . ? C14B Fe1B C17B C13B 37.16(19) . . . . ? C5B Fe1B C17B C13B -167.05(18) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.218 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.049 # Attachment 'pS2c.cif' data_erk4403 _database_code_depnum_ccdc_archive 'CCDC 714368' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H10 F5 Fe N O' _chemical_formula_weight 395.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.1035(1) _cell_length_b 9.8860(2) _cell_length_c 12.2284(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.327(1) _cell_angle_gamma 90.00 _cell_volume 734.67(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1333 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 1.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6399 _exptl_absorpt_correction_T_max 0.8989 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4869 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.88 _reflns_number_total 2991 _reflns_number_gt 2725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0372P)^2^+0.2065P] 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 riding _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 -0.004(17) _refine_ls_number_reflns 2991 _refine_ls_number_parameters 227 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Fe1 Fe 0.68166(6) 0.72558(5) 0.14516(3) 0.03140(11) Uani 1 1 d . . . N1 N 0.6676(4) 1.0944(2) 0.2465(2) 0.0307(5) Uani 1 1 d . . . O1 O 0.3094(3) 0.9335(3) 0.18209(19) 0.0425(5) Uani 1 1 d . . . H1 H 0.3717 0.9922 0.2224 0.064 Uiso 1 1 calc R . . C1 C 0.4549(4) 0.8812(3) 0.1150(2) 0.0333(6) Uani 1 1 d . . . C2 C 0.6754(5) 0.9282(3) 0.1087(2) 0.0336(6) Uani 1 1 d . . . C3 C 0.7672(5) 0.8503(3) 0.0253(2) 0.0372(7) Uani 1 1 d . . . H3 H 0.9102 0.8589 0.0034 0.045 Uiso 1 1 calc R . . C4 C 0.6041(5) 0.7581(3) -0.0183(2) 0.0415(8) Uani 1 1 d . . . H4 H 0.6197 0.6957 -0.0751 0.050 Uiso 1 1 calc R . . C5 C 0.4129(5) 0.7758(3) 0.0384(2) 0.0380(7) Uani 1 1 d . . . H5 H 0.2817 0.7259 0.0268 0.046 Uiso 1 1 calc R . . C6 C 0.7917(7) 0.6933(4) 0.3052(3) 0.0608(11) Uani 1 1 d . . . H6 H 0.8060 0.7598 0.3604 0.073 Uiso 1 1 calc R . . C7 C 0.9507(6) 0.6588(7) 0.2373(6) 0.103(2) Uani 1 1 d . . . H7 H 1.0924 0.6960 0.2370 0.123 Uiso 1 1 calc R . . C8 C 0.8534(18) 0.5530(8) 0.1664(4) 0.134(4) Uani 1 1 d . . . H8 H 0.9194 0.5078 0.1103 0.161 Uiso 1 1 calc R . . C9 C 0.6492(12) 0.5324(4) 0.1969(5) 0.097(2) Uani 1 1 d . . . H9 H 0.5474 0.4690 0.1653 0.116 Uiso 1 1 calc R . . C10 C 0.6144(7) 0.6172(5) 0.2799(3) 0.0589(11) Uani 1 1 d . . . H10 H 0.4838 0.6218 0.3149 0.071 Uiso 1 1 calc R . . C11 C 0.7833(4) 1.0267(3) 0.1821(2) 0.0327(6) Uani 1 1 d . . . H11 H 0.9356 1.0415 0.1831 0.039 Uiso 1 1 calc R . . C12 C 0.7605(4) 1.1941(3) 0.3184(2) 0.0305(6) Uani 1 1 d . . . C13 C 0.9553(5) 1.2649(3) 0.3126(3) 0.0366(7) Uani 1 1 d . . . C14 C 1.0248(5) 1.3638(3) 0.3868(3) 0.0409(7) Uani 1 1 d . . . C15 C 0.9020(6) 1.3964(3) 0.4712(3) 0.0414(7) Uani 1 1 d . . . C16 C 0.7073(6) 1.3284(3) 0.4800(2) 0.0410(7) Uani 1 1 d . . . C17 C 0.6398(4) 1.2297(4) 0.4063(2) 0.0334(5) Uani 1 1 d . . . F1 F 1.0810(3) 1.2422(3) 0.22883(16) 0.0537(5) Uani 1 1 d . . . F2 F 1.2157(3) 1.4301(2) 0.3768(2) 0.0591(6) Uani 1 1 d . . . F3 F 0.9684(4) 1.4915(2) 0.54462(19) 0.0643(6) Uani 1 1 d . . . F4 F 0.5837(4) 1.3591(2) 0.56225(18) 0.0647(6) Uani 1 1 d . . . F5 F 0.4491(3) 1.1656(2) 0.41791(16) 0.0472(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.03347(18) 0.02891(19) 0.03177(18) -0.00013(18) 0.00277(13) 0.00275(19) N1 0.0312(11) 0.0250(12) 0.0355(12) 0.0015(9) 0.0011(10) -0.0004(9) O1 0.0296(10) 0.0455(14) 0.0534(13) -0.0089(11) 0.0089(9) 0.0020(9) C1 0.0287(13) 0.0348(16) 0.0359(14) -0.0002(12) -0.0004(11) 0.0051(11) C2 0.0325(14) 0.0330(16) 0.0355(14) -0.0014(13) 0.0035(11) 0.0015(12) C3 0.0386(15) 0.0363(17) 0.0377(15) 0.0039(13) 0.0100(12) 0.0011(13) C4 0.0470(16) 0.045(2) 0.0323(13) -0.0041(12) 0.0025(12) 0.0034(13) C5 0.0374(15) 0.0359(16) 0.0390(15) -0.0041(13) -0.0047(12) -0.0024(12) C6 0.082(3) 0.052(3) 0.0439(18) 0.0066(16) -0.0186(18) -0.0003(19) C7 0.0315(18) 0.135(5) 0.140(5) 0.101(5) 0.001(2) 0.010(2) C8 0.234(9) 0.116(5) 0.063(3) 0.046(3) 0.068(5) 0.145(6) C9 0.181(6) 0.024(2) 0.073(3) 0.015(2) -0.054(4) -0.017(3) C10 0.054(2) 0.066(3) 0.057(2) 0.030(2) 0.0055(18) -0.0036(18) C11 0.0272(12) 0.0290(15) 0.0416(15) 0.0044(12) 0.0013(11) 0.0003(11) C12 0.0316(12) 0.0247(17) 0.0340(13) 0.0038(10) -0.0038(10) -0.0002(10) C13 0.0310(13) 0.0297(16) 0.0493(16) 0.0050(12) 0.0045(12) -0.0005(11) C14 0.0306(14) 0.0311(16) 0.0591(19) 0.0044(14) -0.0064(14) -0.0063(12) C15 0.0511(18) 0.0281(17) 0.0420(17) -0.0043(13) -0.0110(14) -0.0048(13) C16 0.0570(18) 0.0344(16) 0.0315(15) 0.0002(12) 0.0038(14) -0.0021(15) C17 0.0362(12) 0.0269(12) 0.0372(12) 0.0046(16) 0.0038(10) 0.0006(16) F1 0.0419(9) 0.0514(14) 0.0714(11) -0.0045(11) 0.0243(8) -0.0080(10) F2 0.0380(10) 0.0433(12) 0.0945(16) -0.0007(12) -0.0021(10) -0.0167(9) F3 0.0784(15) 0.0447(13) 0.0658(14) -0.0172(11) -0.0139(12) -0.0137(11) F4 0.0881(16) 0.0569(14) 0.0527(12) -0.0168(11) 0.0255(11) -0.0141(12) F5 0.0457(10) 0.0395(10) 0.0592(11) -0.0078(9) 0.0196(9) -0.0124(8) _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 C8 2.006(4) . ? Fe1 C7 2.014(4) . ? Fe1 C3 2.021(3) . ? Fe1 C9 2.027(4) . ? Fe1 C6 2.034(3) . ? Fe1 C4 2.036(3) . ? Fe1 C10 2.039(4) . ? Fe1 C2 2.052(3) . ? Fe1 C5 2.060(3) . ? Fe1 C1 2.080(3) . ? N1 C11 1.292(4) . ? N1 C12 1.406(4) . ? O1 C1 1.365(4) . ? C1 C5 1.409(4) . ? C1 C2 1.432(4) . ? C2 C3 1.434(4) . ? C2 C11 1.441(4) . ? C3 C4 1.417(5) . ? C4 C5 1.422(4) . ? C6 C10 1.331(6) . ? C6 C7 1.378(8) . ? C7 C8 1.450(10) . ? C8 C9 1.349(10) . ? C9 C10 1.348(8) . ? C12 C13 1.387(4) . ? C12 C17 1.402(4) . ? C13 F1 1.354(4) . ? C13 C14 1.374(5) . ? C14 F2 1.353(3) . ? C14 C15 1.369(5) . ? C15 F3 1.337(4) . ? C15 C16 1.378(5) . ? C16 F4 1.347(4) . ? C16 C17 1.366(5) . ? C17 F5 1.344(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 Fe1 C7 42.3(3) . . ? C8 Fe1 C3 116.4(2) . . ? C7 Fe1 C3 110.69(16) . . ? C8 Fe1 C9 39.1(3) . . ? C7 Fe1 C9 67.4(2) . . ? C3 Fe1 C9 147.2(2) . . ? C8 Fe1 C6 67.7(2) . . ? C7 Fe1 C6 39.8(2) . . ? C3 Fe1 C6 135.15(16) . . ? C9 Fe1 C6 65.49(18) . . ? C8 Fe1 C4 109.39(19) . . ? C7 Fe1 C4 134.7(2) . . ? C3 Fe1 C4 40.88(13) . . ? C9 Fe1 C4 115.75(17) . . ? C6 Fe1 C4 174.19(16) . . ? C8 Fe1 C10 65.8(2) . . ? C7 Fe1 C10 65.84(18) . . ? C3 Fe1 C10 172.66(17) . . ? C9 Fe1 C10 38.7(2) . . ? C6 Fe1 C10 38.13(17) . . ? C4 Fe1 C10 146.13(16) . . ? C8 Fe1 C2 149.0(3) . . ? C7 Fe1 C2 116.1(2) . . ? C3 Fe1 C2 41.21(12) . . ? C9 Fe1 C2 170.8(2) . . ? C6 Fe1 C2 111.09(15) . . ? C4 Fe1 C2 68.58(13) . . ? C10 Fe1 C2 133.42(16) . . ? C8 Fe1 C5 131.5(3) . . ? C7 Fe1 C5 173.3(3) . . ? C3 Fe1 C5 68.75(13) . . ? C9 Fe1 C5 109.24(19) . . ? C6 Fe1 C5 145.06(16) . . ? C4 Fe1 C5 40.63(12) . . ? C10 Fe1 C5 115.51(15) . . ? C2 Fe1 C5 68.26(12) . . ? C8 Fe1 C1 169.5(4) . . ? C7 Fe1 C1 146.7(3) . . ? C3 Fe1 C1 68.44(12) . . ? C9 Fe1 C1 132.0(2) . . ? C6 Fe1 C1 116.19(15) . . ? C4 Fe1 C1 67.61(12) . . ? C10 Fe1 C1 110.57(15) . . ? C2 Fe1 C1 40.57(11) . . ? C5 Fe1 C1 39.81(12) . . ? C11 N1 C12 122.2(2) . . ? O1 C1 C5 126.3(3) . . ? O1 C1 C2 125.2(3) . . ? C5 C1 C2 108.5(3) . . ? O1 C1 Fe1 129.3(2) . . ? C5 C1 Fe1 69.35(17) . . ? C2 C1 Fe1 68.67(17) . . ? C1 C2 C3 107.2(3) . . ? C1 C2 C11 124.3(3) . . ? C3 C2 C11 128.3(3) . . ? C1 C2 Fe1 70.76(18) . . ? C3 C2 Fe1 68.25(18) . . ? C11 C2 Fe1 121.7(2) . . ? C4 C3 C2 107.8(3) . . ? C4 C3 Fe1 70.13(18) . . ? C2 C3 Fe1 70.54(17) . . ? C3 C4 C5 108.5(3) . . ? C3 C4 Fe1 68.99(17) . . ? C5 C4 Fe1 70.59(17) . . ? C1 C5 C4 107.9(3) . . ? C1 C5 Fe1 70.84(17) . . ? C4 C5 Fe1 68.79(16) . . ? C10 C6 C7 108.8(5) . . ? C10 C6 Fe1 71.1(2) . . ? C7 C6 Fe1 69.3(2) . . ? C6 C7 C8 105.5(4) . . ? C6 C7 Fe1 70.9(2) . . ? C8 C7 Fe1 68.6(3) . . ? C9 C8 C7 106.3(4) . . ? C9 C8 Fe1 71.3(3) . . ? C7 C8 Fe1 69.2(3) . . ? C10 C9 C8 109.2(5) . . ? C10 C9 Fe1 71.1(2) . . ? C8 C9 Fe1 69.6(3) . . ? C6 C10 C9 110.2(5) . . ? C6 C10 Fe1 70.7(2) . . ? C9 C10 Fe1 70.2(2) . . ? N1 C11 C2 119.0(3) . . ? C13 C12 C17 115.3(3) . . ? C13 C12 N1 128.3(3) . . ? C17 C12 N1 116.4(3) . . ? F1 C13 C14 117.1(3) . . ? F1 C13 C12 120.2(3) . . ? C14 C13 C12 122.6(3) . . ? F2 C14 C15 119.4(3) . . ? F2 C14 C13 120.0(3) . . ? C15 C14 C13 120.6(3) . . ? F3 C15 C14 121.2(3) . . ? F3 C15 C16 120.1(3) . . ? C14 C15 C16 118.7(3) . . ? F4 C16 C17 119.9(3) . . ? F4 C16 C15 119.7(3) . . ? C17 C16 C15 120.4(3) . . ? F5 C17 C16 118.5(3) . . ? F5 C17 C12 119.0(3) . . ? C16 C17 C12 122.5(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 C8 Fe1 C1 O1 83.1(9) . . . . ? C7 Fe1 C1 O1 -62.0(4) . . . . ? C3 Fe1 C1 O1 -157.2(3) . . . . ? C9 Fe1 C1 O1 53.4(4) . . . . ? C6 Fe1 C1 O1 -26.3(3) . . . . ? C4 Fe1 C1 O1 158.6(3) . . . . ? C10 Fe1 C1 O1 15.0(3) . . . . ? C2 Fe1 C1 O1 -118.7(3) . . . . ? C5 Fe1 C1 O1 120.5(4) . . . . ? C8 Fe1 C1 C5 -37.4(9) . . . . ? C7 Fe1 C1 C5 177.4(3) . . . . ? C3 Fe1 C1 C5 82.3(2) . . . . ? C9 Fe1 C1 C5 -67.1(3) . . . . ? C6 Fe1 C1 C5 -146.8(2) . . . . ? C4 Fe1 C1 C5 38.02(18) . . . . ? C10 Fe1 C1 C5 -105.5(2) . . . . ? C2 Fe1 C1 C5 120.8(3) . . . . ? C8 Fe1 C1 C2 -158.2(8) . . . . ? C7 Fe1 C1 C2 56.7(3) . . . . ? C3 Fe1 C1 C2 -38.53(18) . . . . ? C9 Fe1 C1 C2 172.1(2) . . . . ? C6 Fe1 C1 C2 92.4(2) . . . . ? C4 Fe1 C1 C2 -82.76(19) . . . . ? C10 Fe1 C1 C2 133.7(2) . . . . ? C5 Fe1 C1 C2 -120.8(3) . . . . ? O1 C1 C2 C3 -177.4(3) . . . . ? C5 C1 C2 C3 0.8(3) . . . . ? Fe1 C1 C2 C3 58.7(2) . . . . ? O1 C1 C2 C11 7.9(5) . . . . ? C5 C1 C2 C11 -173.9(3) . . . . ? Fe1 C1 C2 C11 -115.9(3) . . . . ? O1 C1 C2 Fe1 123.8(3) . . . . ? C5 C1 C2 Fe1 -58.0(2) . . . . ? C8 Fe1 C2 C1 172.4(4) . . . . ? C7 Fe1 C2 C1 -149.3(3) . . . . ? C3 Fe1 C2 C1 118.4(3) . . . . ? C6 Fe1 C2 C1 -106.1(2) . . . . ? C4 Fe1 C2 C1 80.15(18) . . . . ? C10 Fe1 C2 C1 -68.8(2) . . . . ? C5 Fe1 C2 C1 36.31(17) . . . . ? C8 Fe1 C2 C3 54.0(5) . . . . ? C7 Fe1 C2 C3 92.2(3) . . . . ? C6 Fe1 C2 C3 135.5(2) . . . . ? C4 Fe1 C2 C3 -38.29(18) . . . . ? C10 Fe1 C2 C3 172.8(2) . . . . ? C5 Fe1 C2 C3 -82.13(19) . . . . ? C1 Fe1 C2 C3 -118.4(3) . . . . ? C8 Fe1 C2 C11 -68.5(5) . . . . ? C7 Fe1 C2 C11 -30.3(3) . . . . ? C3 Fe1 C2 C11 -122.5(3) . . . . ? C6 Fe1 C2 C11 13.0(3) . . . . ? C4 Fe1 C2 C11 -160.8(3) . . . . ? C10 Fe1 C2 C11 50.2(3) . . . . ? C5 Fe1 C2 C11 155.3(3) . . . . ? C1 Fe1 C2 C11 119.0(3) . . . . ? C1 C2 C3 C4 0.2(3) . . . . ? C11 C2 C3 C4 174.5(3) . . . . ? Fe1 C2 C3 C4 60.5(2) . . . . ? C1 C2 C3 Fe1 -60.3(2) . . . . ? C11 C2 C3 Fe1 114.0(3) . . . . ? C8 Fe1 C3 C4 89.5(4) . . . . ? C7 Fe1 C3 C4 135.5(3) . . . . ? C9 Fe1 C3 C4 55.5(4) . . . . ? C6 Fe1 C3 C4 173.7(2) . . . . ? C2 Fe1 C3 C4 -118.2(3) . . . . ? C5 Fe1 C3 C4 -37.35(18) . . . . ? C1 Fe1 C3 C4 -80.25(19) . . . . ? C8 Fe1 C3 C2 -152.3(4) . . . . ? C7 Fe1 C3 C2 -106.3(3) . . . . ? C9 Fe1 C3 C2 173.7(4) . . . . ? C6 Fe1 C3 C2 -68.1(3) . . . . ? C4 Fe1 C3 C2 118.2(3) . . . . ? C5 Fe1 C3 C2 80.84(18) . . . . ? C1 Fe1 C3 C2 37.94(17) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? Fe1 C3 C4 C5 59.7(2) . . . . ? C2 C3 C4 Fe1 -60.8(2) . . . . ? C8 Fe1 C4 C3 -108.3(4) . . . . ? C7 Fe1 C4 C3 -67.4(4) . . . . ? C9 Fe1 C4 C3 -150.3(3) . . . . ? C10 Fe1 C4 C3 176.4(3) . . . . ? C2 Fe1 C4 C3 38.59(18) . . . . ? C5 Fe1 C4 C3 119.7(3) . . . . ? C1 Fe1 C4 C3 82.5(2) . . . . ? C8 Fe1 C4 C5 131.9(4) . . . . ? C7 Fe1 C4 C5 172.9(3) . . . . ? C3 Fe1 C4 C5 -119.7(3) . . . . ? C9 Fe1 C4 C5 90.0(3) . . . . ? C10 Fe1 C4 C5 56.6(3) . . . . ? C2 Fe1 C4 C5 -81.14(19) . . . . ? C1 Fe1 C4 C5 -37.28(18) . . . . ? O1 C1 C5 C4 176.8(3) . . . . ? C2 C1 C5 C4 -1.4(3) . . . . ? Fe1 C1 C5 C4 -59.0(2) . . . . ? O1 C1 C5 Fe1 -124.2(3) . . . . ? C2 C1 C5 Fe1 57.6(2) . . . . ? C3 C4 C5 C1 1.5(3) . . . . ? Fe1 C4 C5 C1 60.3(2) . . . . ? C3 C4 C5 Fe1 -58.7(2) . . . . ? C8 Fe1 C5 C1 171.5(3) . . . . ? C3 Fe1 C5 C1 -81.43(19) . . . . ? C9 Fe1 C5 C1 133.6(3) . . . . ? C6 Fe1 C5 C1 59.1(3) . . . . ? C4 Fe1 C5 C1 -119.0(3) . . . . ? C10 Fe1 C5 C1 92.0(2) . . . . ? C2 Fe1 C5 C1 -36.98(17) . . . . ? C8 Fe1 C5 C4 -69.5(4) . . . . ? C3 Fe1 C5 C4 37.57(19) . . . . ? C9 Fe1 C5 C4 -107.4(3) . . . . ? C6 Fe1 C5 C4 178.1(3) . . . . ? C10 Fe1 C5 C4 -149.0(2) . . . . ? C2 Fe1 C5 C4 82.02(19) . . . . ? C1 Fe1 C5 C4 119.0(3) . . . . ? C8 Fe1 C6 C10 -78.8(5) . . . . ? C7 Fe1 C6 C10 -119.6(5) . . . . ? C3 Fe1 C6 C10 175.5(3) . . . . ? C9 Fe1 C6 C10 -36.1(3) . . . . ? C2 Fe1 C6 C10 134.6(3) . . . . ? C5 Fe1 C6 C10 52.7(4) . . . . ? C1 Fe1 C6 C10 90.4(3) . . . . ? C8 Fe1 C6 C7 40.8(4) . . . . ? C3 Fe1 C6 C7 -64.9(4) . . . . ? C9 Fe1 C6 C7 83.5(4) . . . . ? C10 Fe1 C6 C7 119.6(5) . . . . ? C2 Fe1 C6 C7 -105.8(4) . . . . ? C5 Fe1 C6 C7 172.3(4) . . . . ? C1 Fe1 C6 C7 -150.0(3) . . . . ? C10 C6 C7 C8 0.2(5) . . . . ? Fe1 C6 C7 C8 -60.2(3) . . . . ? C10 C6 C7 Fe1 60.4(3) . . . . ? C8 Fe1 C7 C6 -116.1(4) . . . . ? C3 Fe1 C7 C6 136.9(3) . . . . ? C9 Fe1 C7 C6 -78.4(3) . . . . ? C4 Fe1 C7 C6 177.2(2) . . . . ? C10 Fe1 C7 C6 -36.0(3) . . . . ? C2 Fe1 C7 C6 92.2(3) . . . . ? C1 Fe1 C7 C6 55.0(4) . . . . ? C3 Fe1 C7 C8 -107.0(4) . . . . ? C9 Fe1 C7 C8 37.7(3) . . . . ? C6 Fe1 C7 C8 116.1(4) . . . . ? C4 Fe1 C7 C8 -66.8(4) . . . . ? C10 Fe1 C7 C8 80.0(4) . . . . ? C2 Fe1 C7 C8 -151.7(3) . . . . ? C1 Fe1 C7 C8 171.1(4) . . . . ? C6 C7 C8 C9 -0.3(5) . . . . ? Fe1 C7 C8 C9 -62.0(3) . . . . ? C6 C7 C8 Fe1 61.7(3) . . . . ? C7 Fe1 C8 C9 116.5(4) . . . . ? C3 Fe1 C8 C9 -151.2(3) . . . . ? C6 Fe1 C8 C9 78.1(3) . . . . ? C4 Fe1 C8 C9 -107.3(3) . . . . ? C10 Fe1 C8 C9 36.5(3) . . . . ? C2 Fe1 C8 C9 172.3(3) . . . . ? C5 Fe1 C8 C9 -67.0(4) . . . . ? C1 Fe1 C8 C9 -35.7(10) . . . . ? C3 Fe1 C8 C7 92.3(3) . . . . ? C9 Fe1 C8 C7 -116.5(4) . . . . ? C6 Fe1 C8 C7 -38.4(3) . . . . ? C4 Fe1 C8 C7 136.2(3) . . . . ? C10 Fe1 C8 C7 -80.0(3) . . . . ? C2 Fe1 C8 C7 55.7(4) . . . . ? C5 Fe1 C8 C7 176.5(3) . . . . ? C1 Fe1 C8 C7 -152.2(8) . . . . ? C7 C8 C9 C10 0.3(5) . . . . ? Fe1 C8 C9 C10 -60.3(3) . . . . ? C7 C8 C9 Fe1 60.6(3) . . . . ? C8 Fe1 C9 C10 119.8(5) . . . . ? C7 Fe1 C9 C10 79.1(4) . . . . ? C3 Fe1 C9 C10 172.5(3) . . . . ? C6 Fe1 C9 C10 35.6(3) . . . . ? C4 Fe1 C9 C10 -150.7(3) . . . . ? C5 Fe1 C9 C10 -107.1(3) . . . . ? C1 Fe1 C9 C10 -68.4(3) . . . . ? C7 Fe1 C9 C8 -40.7(4) . . . . ? C3 Fe1 C9 C8 52.7(5) . . . . ? C6 Fe1 C9 C8 -84.3(4) . . . . ? C4 Fe1 C9 C8 89.5(4) . . . . ? C10 Fe1 C9 C8 -119.8(5) . . . . ? C5 Fe1 C9 C8 133.1(4) . . . . ? C1 Fe1 C9 C8 171.7(4) . . . . ? C7 C6 C10 C9 0.0(5) . . . . ? Fe1 C6 C10 C9 59.2(3) . . . . ? C7 C6 C10 Fe1 -59.3(3) . . . . ? C8 C9 C10 C6 -0.2(5) . . . . ? Fe1 C9 C10 C6 -59.6(3) . . . . ? C8 C9 C10 Fe1 59.4(3) . . . . ? C8 Fe1 C10 C6 84.1(5) . . . . ? C7 Fe1 C10 C6 37.6(4) . . . . ? C9 Fe1 C10 C6 121.0(4) . . . . ? C4 Fe1 C10 C6 173.3(3) . . . . ? C2 Fe1 C10 C6 -66.2(3) . . . . ? C5 Fe1 C10 C6 -149.7(3) . . . . ? C1 Fe1 C10 C6 -106.6(3) . . . . ? C8 Fe1 C10 C9 -36.8(4) . . . . ? C7 Fe1 C10 C9 -83.4(4) . . . . ? C6 Fe1 C10 C9 -121.0(4) . . . . ? C4 Fe1 C10 C9 52.3(5) . . . . ? C2 Fe1 C10 C9 172.8(3) . . . . ? C5 Fe1 C10 C9 89.4(4) . . . . ? C1 Fe1 C10 C9 132.5(3) . . . . ? C12 N1 C11 C2 -178.5(3) . . . . ? C1 C2 C11 N1 -11.9(5) . . . . ? C3 C2 C11 N1 174.7(3) . . . . ? Fe1 C2 C11 N1 -99.2(3) . . . . ? C11 N1 C12 C13 21.0(5) . . . . ? C11 N1 C12 C17 -160.6(3) . . . . ? C17 C12 C13 F1 -177.7(3) . . . . ? N1 C12 C13 F1 0.7(5) . . . . ? C17 C12 C13 C14 -0.5(4) . . . . ? N1 C12 C13 C14 177.9(3) . . . . ? F1 C13 C14 F2 -2.4(4) . . . . ? C12 C13 C14 F2 -179.6(3) . . . . ? F1 C13 C14 C15 177.4(3) . . . . ? C12 C13 C14 C15 0.2(5) . . . . ? F2 C14 C15 F3 -0.7(5) . . . . ? C13 C14 C15 F3 179.5(3) . . . . ? F2 C14 C15 C16 179.6(3) . . . . ? C13 C14 C15 C16 -0.2(5) . . . . ? F3 C15 C16 F4 0.5(5) . . . . ? C14 C15 C16 F4 -179.9(3) . . . . ? F3 C15 C16 C17 -179.1(3) . . . . ? C14 C15 C16 C17 0.6(5) . . . . ? F4 C16 C17 F5 0.3(5) . . . . ? C15 C16 C17 F5 179.8(3) . . . . ? F4 C16 C17 C12 179.4(3) . . . . ? C15 C16 C17 C12 -1.0(5) . . . . ? C13 C12 C17 F5 -179.9(3) . . . . ? N1 C12 C17 F5 1.5(4) . . . . ? C13 C12 C17 C16 0.9(4) . . . . ? N1 C12 C17 C16 -177.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.348 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.053 # Attachment 'rac10.cif' data_erk3377 _database_code_depnum_ccdc_archive 'CCDC 714369' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 Fe O4' _chemical_formula_weight 330.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.662(1) _cell_length_b 7.647(1) _cell_length_c 11.332(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.75(1) _cell_angle_gamma 90.00 _cell_volume 1443.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4862 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8575 _exptl_absorpt_correction_T_max 0.9393 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappeCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9482 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3519 _reflns_number_gt 2514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0268P)^2^+1.0472P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3519 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Fe Fe 0.14073(2) 0.34388(5) 0.12858(3) 0.03633(13) Uani 1 1 d . . . O1 O 0.39849(11) 0.4024(3) 0.11702(18) 0.0469(5) Uani 1 1 d . . . O2 O 0.33290(12) 0.2852(3) 0.27818(18) 0.0499(5) Uani 1 1 d . . . O3 O 0.22583(12) 0.5622(2) 0.31733(17) 0.0430(5) Uani 1 1 d . . . O4 O 0.31803(17) 0.7640(4) 0.2726(2) 0.0772(8) Uani 1 1 d . . . C1 C 0.25771(15) 0.4200(3) 0.1244(2) 0.0358(6) Uani 1 1 d . . . C2 C 0.21203(16) 0.5340(3) 0.1969(2) 0.0379(6) Uani 1 1 d . . . C3 C 0.14994(17) 0.6112(4) 0.1293(3) 0.0438(7) Uani 1 1 d . . . H3A H 0.1096 0.6938 0.1577 0.053 Uiso 1 1 calc R . . C4 C 0.15606(18) 0.5452(4) 0.0124(3) 0.0455(7) Uani 1 1 d . . . H4A H 0.1204 0.5741 -0.0542 0.055 Uiso 1 1 calc R . . C5 C 0.22249(17) 0.4285(4) 0.0091(3) 0.0425(7) Uani 1 1 d . . . H5A H 0.2404 0.3635 -0.0602 0.051 Uiso 1 1 calc R . . C6 C 0.32967(16) 0.3128(4) 0.1565(3) 0.0391(6) Uani 1 1 d . . . H6A H 0.3260 0.1996 0.1163 0.047 Uiso 1 1 calc R . . C7 C 0.46939(18) 0.3002(4) 0.1402(3) 0.0551(8) Uani 1 1 d . . . H7A H 0.5164 0.3647 0.1154 0.066 Uiso 1 1 calc R . . H7B H 0.4668 0.1924 0.0952 0.066 Uiso 1 1 calc R . . C8 C 0.47660(18) 0.2589(4) 0.2692(3) 0.0557(9) Uani 1 1 d . . . H8A H 0.4866 0.3654 0.3136 0.067 Uiso 1 1 calc R . . H8B H 0.5213 0.1800 0.2829 0.067 Uiso 1 1 calc R . . C9 C 0.40027(18) 0.1753(4) 0.3097(3) 0.0556(8) Uani 1 1 d . . . H9A H 0.3940 0.0615 0.2730 0.067 Uiso 1 1 calc R . . H9B H 0.4024 0.1591 0.3946 0.067 Uiso 1 1 calc R . . C10 C 0.28819(18) 0.6726(4) 0.3444(3) 0.0461(7) Uani 1 1 d . . . C11 C 0.3121(2) 0.6566(5) 0.4706(3) 0.0590(9) Uani 1 1 d . . . H11A H 0.3375 0.7630 0.4962 0.089 Uiso 1 1 calc R . . H11B H 0.3491 0.5611 0.4800 0.089 Uiso 1 1 calc R . . H11C H 0.2654 0.6354 0.5171 0.089 Uiso 1 1 calc R . . C21 C 0.09529(19) 0.2118(4) 0.2679(3) 0.0506(8) Uani 1 1 d . . . H21A H 0.1062 0.2364 0.3515 0.061 Uiso 1 1 calc R . . C22 C 0.13959(19) 0.0963(4) 0.1950(3) 0.0501(8) Uani 1 1 d . . . H22A H 0.1867 0.0278 0.2192 0.060 Uiso 1 1 calc R . . C23 C 0.10343(19) 0.0976(4) 0.0817(3) 0.0505(8) Uani 1 1 d . . . H23A H 0.1216 0.0312 0.0131 0.061 Uiso 1 1 calc R . . C24 C 0.03754(18) 0.2138(4) 0.0835(3) 0.0525(8) Uani 1 1 d . . . H24A H 0.0019 0.2414 0.0166 0.063 Uiso 1 1 calc R . . C25 C 0.03206(18) 0.2833(4) 0.1983(3) 0.0514(8) Uani 1 1 d . . . H25A H -0.0082 0.3673 0.2251 0.062 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 Fe 0.0310(2) 0.0381(2) 0.0398(2) -0.00109(18) -0.00043(15) 0.00069(17) O1 0.0305(10) 0.0540(12) 0.0564(13) 0.0059(10) 0.0030(9) -0.0014(9) O2 0.0410(11) 0.0599(13) 0.0488(13) 0.0102(10) 0.0041(10) 0.0127(10) O3 0.0445(11) 0.0431(11) 0.0413(12) -0.0062(9) 0.0012(9) -0.0048(9) O4 0.093(2) 0.0782(18) 0.0608(16) 0.0015(14) 0.0001(14) -0.0434(15) C1 0.0307(13) 0.0370(14) 0.0399(16) 0.0013(12) 0.0025(11) -0.0026(11) C2 0.0370(14) 0.0377(15) 0.0390(16) -0.0026(12) 0.0011(12) -0.0029(12) C3 0.0446(17) 0.0355(15) 0.0514(18) 0.0026(13) 0.0028(14) 0.0035(12) C4 0.0444(17) 0.0459(17) 0.0462(18) 0.0062(13) -0.0038(13) 0.0030(13) C5 0.0413(16) 0.0455(17) 0.0410(17) 0.0011(13) 0.0044(13) -0.0018(13) C6 0.0314(13) 0.0398(15) 0.0459(17) -0.0053(12) 0.0005(12) -0.0024(12) C7 0.0324(15) 0.062(2) 0.072(2) -0.0026(17) 0.0030(15) -0.0005(14) C8 0.0408(17) 0.0516(19) 0.074(2) -0.0022(17) -0.0126(16) 0.0019(14) C9 0.0456(18) 0.0572(19) 0.064(2) 0.0124(16) -0.0036(15) 0.0115(15) C10 0.0447(16) 0.0418(16) 0.0518(19) -0.0103(14) 0.0001(14) 0.0000(14) C11 0.060(2) 0.064(2) 0.053(2) -0.0082(16) -0.0085(16) 0.0028(17) C21 0.0526(19) 0.0552(19) 0.0441(18) 0.0048(14) 0.0045(15) -0.0127(15) C22 0.0480(18) 0.0440(17) 0.058(2) 0.0059(15) -0.0008(15) -0.0043(14) C23 0.0500(18) 0.0476(17) 0.054(2) -0.0107(14) 0.0017(15) -0.0103(15) C24 0.0373(16) 0.062(2) 0.058(2) -0.0009(16) -0.0096(15) -0.0087(15) C25 0.0332(15) 0.0587(19) 0.063(2) -0.0021(16) 0.0122(14) -0.0061(14) _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 Fe C2 2.025(3) . ? Fe C21 2.029(3) . ? Fe C1 2.035(3) . ? Fe C22 2.037(3) . ? Fe C25 2.038(3) . ? Fe C5 2.039(3) . ? Fe C4 2.044(3) . ? Fe C24 2.045(3) . ? Fe C3 2.050(3) . ? Fe C23 2.051(3) . ? O1 C6 1.414(3) . ? O1 C7 1.438(3) . ? O2 C6 1.395(3) . ? O2 C9 1.443(3) . ? O3 C10 1.370(3) . ? O3 C2 1.397(3) . ? O4 C10 1.187(4) . ? C1 C2 1.425(4) . ? C1 C5 1.426(4) . ? C1 C6 1.494(4) . ? C2 C3 1.409(4) . ? C3 C4 1.422(4) . ? C4 C5 1.422(4) . ? C7 C8 1.500(5) . ? C8 C9 1.500(4) . ? C10 C11 1.484(4) . ? C21 C25 1.418(4) . ? C21 C22 1.422(4) . ? C22 C23 1.411(4) . ? C23 C24 1.413(4) . ? C24 C25 1.409(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe C21 106.43(12) . . ? C2 Fe C1 41.10(11) . . ? C21 Fe C1 121.86(12) . . ? C2 Fe C22 122.29(12) . . ? C21 Fe C22 40.94(13) . . ? C1 Fe C22 106.74(12) . . ? C2 Fe C25 122.32(12) . . ? C21 Fe C25 40.80(13) . . ? C1 Fe C25 158.43(12) . . ? C22 Fe C25 68.48(13) . . ? C2 Fe C5 68.42(11) . . ? C21 Fe C5 159.09(13) . . ? C1 Fe C5 40.99(11) . . ? C22 Fe C5 123.36(12) . . ? C25 Fe C5 159.10(13) . . ? C2 Fe C4 68.16(12) . . ? C21 Fe C4 158.01(13) . . ? C1 Fe C4 69.00(11) . . ? C22 Fe C4 159.99(13) . . ? C25 Fe C4 122.67(13) . . ? C5 Fe C4 40.78(11) . . ? C2 Fe C24 158.69(12) . . ? C21 Fe C24 68.35(13) . . ? C1 Fe C24 159.30(12) . . ? C22 Fe C24 68.19(13) . . ? C25 Fe C24 40.36(12) . . ? C5 Fe C24 123.75(13) . . ? C4 Fe C24 108.50(13) . . ? C2 Fe C3 40.45(11) . . ? C21 Fe C3 121.47(13) . . ? C1 Fe C3 69.09(11) . . ? C22 Fe C3 157.85(13) . . ? C25 Fe C3 106.97(13) . . ? C5 Fe C3 68.61(12) . . ? C4 Fe C3 40.67(11) . . ? C24 Fe C3 123.27(13) . . ? C2 Fe C23 158.84(12) . . ? C21 Fe C23 68.24(13) . . ? C1 Fe C23 122.93(12) . . ? C22 Fe C23 40.36(12) . . ? C25 Fe C23 67.91(13) . . ? C5 Fe C23 108.82(12) . . ? C4 Fe C23 124.40(13) . . ? C24 Fe C23 40.35(12) . . ? C3 Fe C23 159.91(12) . . ? C6 O1 C7 110.3(2) . . ? C6 O2 C9 110.6(2) . . ? C10 O3 C2 115.3(2) . . ? C2 C1 C5 106.5(2) . . ? C2 C1 C6 128.9(3) . . ? C5 C1 C6 124.6(2) . . ? C2 C1 Fe 69.07(15) . . ? C5 C1 Fe 69.63(15) . . ? C6 C1 Fe 127.10(19) . . ? O3 C2 C3 125.2(2) . . ? O3 C2 C1 125.1(2) . . ? C3 C2 C1 109.6(2) . . ? O3 C2 Fe 124.91(18) . . ? C3 C2 Fe 70.71(16) . . ? C1 C2 Fe 69.83(15) . . ? C2 C3 C4 107.3(3) . . ? C2 C3 Fe 68.85(16) . . ? C4 C3 Fe 69.44(17) . . ? C5 C4 C3 108.2(3) . . ? C5 C4 Fe 69.42(16) . . ? C3 C4 Fe 69.89(16) . . ? C4 C5 C1 108.4(3) . . ? C4 C5 Fe 69.80(17) . . ? C1 C5 Fe 69.38(15) . . ? O2 C6 O1 111.4(2) . . ? O2 C6 C1 110.1(2) . . ? O1 C6 C1 108.0(2) . . ? O1 C7 C8 110.4(3) . . ? C7 C8 C9 109.3(3) . . ? O2 C9 C8 109.6(3) . . ? O4 C10 O3 122.2(3) . . ? O4 C10 C11 126.8(3) . . ? O3 C10 C11 111.0(3) . . ? C25 C21 C22 107.7(3) . . ? C25 C21 Fe 69.94(17) . . ? C22 C21 Fe 69.83(18) . . ? C23 C22 C21 107.8(3) . . ? C23 C22 Fe 70.34(18) . . ? C21 C22 Fe 69.23(18) . . ? C22 C23 C24 108.3(3) . . ? C22 C23 Fe 69.29(17) . . ? C24 C23 Fe 69.61(17) . . ? C25 C24 C23 108.1(3) . . ? C25 C24 Fe 69.55(17) . . ? C23 C24 Fe 70.04(17) . . ? C24 C25 C21 108.1(3) . . ? C24 C25 Fe 70.09(17) . . ? C21 C25 Fe 69.26(17) . . ? 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 C21 Fe C1 C2 -78.1(2) . . . . ? C22 Fe C1 C2 -120.24(17) . . . . ? C25 Fe C1 C2 -46.6(4) . . . . ? C5 Fe C1 C2 117.8(2) . . . . ? C4 Fe C1 C2 80.44(17) . . . . ? C24 Fe C1 C2 167.3(3) . . . . ? C3 Fe C1 C2 36.74(16) . . . . ? C23 Fe C1 C2 -161.38(17) . . . . ? C2 Fe C1 C5 -117.8(2) . . . . ? C21 Fe C1 C5 164.08(17) . . . . ? C22 Fe C1 C5 121.96(18) . . . . ? C25 Fe C1 C5 -164.4(3) . . . . ? C4 Fe C1 C5 -37.36(17) . . . . ? C24 Fe C1 C5 49.5(4) . . . . ? C3 Fe C1 C5 -81.05(18) . . . . ? C23 Fe C1 C5 80.8(2) . . . . ? C2 Fe C1 C6 123.6(3) . . . . ? C21 Fe C1 C6 45.5(3) . . . . ? C22 Fe C1 C6 3.4(3) . . . . ? C25 Fe C1 C6 77.1(4) . . . . ? C5 Fe C1 C6 -118.6(3) . . . . ? C4 Fe C1 C6 -155.9(3) . . . . ? C24 Fe C1 C6 -69.1(4) . . . . ? C3 Fe C1 C6 160.4(3) . . . . ? C23 Fe C1 C6 -37.8(3) . . . . ? C10 O3 C2 C3 -103.0(3) . . . . ? C10 O3 C2 C1 78.3(3) . . . . ? C10 O3 C2 Fe 167.0(2) . . . . ? C5 C1 C2 O3 179.0(2) . . . . ? C6 C1 C2 O3 -2.3(4) . . . . ? Fe C1 C2 O3 119.1(3) . . . . ? C5 C1 C2 C3 0.2(3) . . . . ? C6 C1 C2 C3 178.9(3) . . . . ? Fe C1 C2 C3 -59.7(2) . . . . ? C5 C1 C2 Fe 59.87(18) . . . . ? C6 C1 C2 Fe -121.4(3) . . . . ? C21 Fe C2 O3 0.5(3) . . . . ? C1 Fe C2 O3 -119.4(3) . . . . ? C22 Fe C2 O3 -41.3(3) . . . . ? C25 Fe C2 O3 42.2(3) . . . . ? C5 Fe C2 O3 -158.0(3) . . . . ? C4 Fe C2 O3 157.9(3) . . . . ? C24 Fe C2 O3 72.9(4) . . . . ? C3 Fe C2 O3 120.1(3) . . . . ? C23 Fe C2 O3 -71.5(4) . . . . ? C21 Fe C2 C3 -119.54(18) . . . . ? C1 Fe C2 C3 120.5(2) . . . . ? C22 Fe C2 C3 -161.36(18) . . . . ? C25 Fe C2 C3 -77.9(2) . . . . ? C5 Fe C2 C3 81.92(18) . . . . ? C4 Fe C2 C3 37.87(17) . . . . ? C24 Fe C2 C3 -47.1(4) . . . . ? C23 Fe C2 C3 168.4(3) . . . . ? C21 Fe C2 C1 119.94(17) . . . . ? C22 Fe C2 C1 78.1(2) . . . . ? C25 Fe C2 C1 161.59(17) . . . . ? C5 Fe C2 C1 -38.60(16) . . . . ? C4 Fe C2 C1 -82.65(17) . . . . ? C24 Fe C2 C1 -167.7(3) . . . . ? C3 Fe C2 C1 -120.5(2) . . . . ? C23 Fe C2 C1 47.9(4) . . . . ? O3 C2 C3 C4 -178.7(2) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? Fe C2 C3 C4 -59.0(2) . . . . ? O3 C2 C3 Fe -119.7(3) . . . . ? C1 C2 C3 Fe 59.15(19) . . . . ? C21 Fe C3 C2 78.1(2) . . . . ? C1 Fe C3 C2 -37.32(16) . . . . ? C22 Fe C3 C2 45.8(4) . . . . ? C25 Fe C3 C2 120.24(18) . . . . ? C5 Fe C3 C2 -81.41(18) . . . . ? C4 Fe C3 C2 -119.0(2) . . . . ? C24 Fe C3 C2 161.42(17) . . . . ? C23 Fe C3 C2 -167.8(3) . . . . ? C2 Fe C3 C4 119.0(2) . . . . ? C21 Fe C3 C4 -162.90(18) . . . . ? C1 Fe C3 C4 81.71(18) . . . . ? C22 Fe C3 C4 164.8(3) . . . . ? C25 Fe C3 C4 -120.73(19) . . . . ? C5 Fe C3 C4 37.62(17) . . . . ? C24 Fe C3 C4 -79.6(2) . . . . ? C23 Fe C3 C4 -48.8(4) . . . . ? C2 C3 C4 C5 -0.4(3) . . . . ? Fe C3 C4 C5 -59.0(2) . . . . ? C2 C3 C4 Fe 58.65(19) . . . . ? C2 Fe C4 C5 81.84(18) . . . . ? C21 Fe C4 C5 161.6(3) . . . . ? C1 Fe C4 C5 37.54(17) . . . . ? C22 Fe C4 C5 -43.7(4) . . . . ? C25 Fe C4 C5 -162.87(18) . . . . ? C24 Fe C4 C5 -120.60(19) . . . . ? C3 Fe C4 C5 119.5(2) . . . . ? C23 Fe C4 C5 -78.7(2) . . . . ? C2 Fe C4 C3 -37.67(17) . . . . ? C21 Fe C4 C3 42.0(4) . . . . ? C1 Fe C4 C3 -81.97(18) . . . . ? C22 Fe C4 C3 -163.2(3) . . . . ? C25 Fe C4 C3 77.6(2) . . . . ? C5 Fe C4 C3 -119.5(2) . . . . ? C24 Fe C4 C3 119.89(18) . . . . ? C23 Fe C4 C3 161.74(17) . . . . ? C3 C4 C5 C1 0.5(3) . . . . ? Fe C4 C5 C1 -58.81(19) . . . . ? C3 C4 C5 Fe 59.3(2) . . . . ? C2 C1 C5 C4 -0.4(3) . . . . ? C6 C1 C5 C4 -179.2(2) . . . . ? Fe C1 C5 C4 59.1(2) . . . . ? C2 C1 C5 Fe -59.51(18) . . . . ? C6 C1 C5 Fe 121.7(3) . . . . ? C2 Fe C5 C4 -81.14(18) . . . . ? C21 Fe C5 C4 -160.6(3) . . . . ? C1 Fe C5 C4 -119.8(2) . . . . ? C22 Fe C5 C4 163.56(18) . . . . ? C25 Fe C5 C4 44.0(4) . . . . ? C24 Fe C5 C4 79.0(2) . . . . ? C3 Fe C5 C4 -37.52(17) . . . . ? C23 Fe C5 C4 121.24(19) . . . . ? C2 Fe C5 C1 38.71(16) . . . . ? C21 Fe C5 C1 -40.8(4) . . . . ? C22 Fe C5 C1 -76.6(2) . . . . ? C25 Fe C5 C1 163.9(3) . . . . ? C4 Fe C5 C1 119.8(2) . . . . ? C24 Fe C5 C1 -161.13(17) . . . . ? C3 Fe C5 C1 82.32(18) . . . . ? C23 Fe C5 C1 -118.91(17) . . . . ? C9 O2 C6 O1 -62.7(3) . . . . ? C9 O2 C6 C1 177.5(2) . . . . ? C7 O1 C6 O2 62.0(3) . . . . ? C7 O1 C6 C1 -176.9(2) . . . . ? C2 C1 C6 O2 21.5(4) . . . . ? C5 C1 C6 O2 -160.0(2) . . . . ? Fe C1 C6 O2 -70.5(3) . . . . ? C2 C1 C6 O1 -100.4(3) . . . . ? C5 C1 C6 O1 78.1(3) . . . . ? Fe C1 C6 O1 167.61(19) . . . . ? C6 O1 C7 C8 -57.2(3) . . . . ? O1 C7 C8 C9 53.6(3) . . . . ? C6 O2 C9 C8 58.3(3) . . . . ? C7 C8 C9 O2 -53.6(4) . . . . ? C2 O3 C10 O4 14.2(4) . . . . ? C2 O3 C10 C11 -164.5(2) . . . . ? C2 Fe C21 C25 120.75(19) . . . . ? C1 Fe C21 C25 162.87(18) . . . . ? C22 Fe C21 C25 -118.6(3) . . . . ? C5 Fe C21 C25 -166.9(3) . . . . ? C4 Fe C21 C25 48.5(4) . . . . ? C24 Fe C21 C25 -37.37(19) . . . . ? C3 Fe C21 C25 79.3(2) . . . . ? C23 Fe C21 C25 -81.0(2) . . . . ? C2 Fe C21 C22 -120.66(19) . . . . ? C1 Fe C21 C22 -78.5(2) . . . . ? C25 Fe C21 C22 118.6(3) . . . . ? C5 Fe C21 C22 -48.3(4) . . . . ? C4 Fe C21 C22 167.1(3) . . . . ? C24 Fe C21 C22 81.2(2) . . . . ? C3 Fe C21 C22 -162.09(18) . . . . ? C23 Fe C21 C22 37.64(19) . . . . ? C25 C21 C22 C23 -0.1(3) . . . . ? Fe C21 C22 C23 -60.0(2) . . . . ? C25 C21 C22 Fe 60.0(2) . . . . ? C2 Fe C22 C23 -163.72(18) . . . . ? C21 Fe C22 C23 118.9(3) . . . . ? C1 Fe C22 C23 -121.52(19) . . . . ? C25 Fe C22 C23 80.8(2) . . . . ? C5 Fe C22 C23 -79.7(2) . . . . ? C4 Fe C22 C23 -47.0(4) . . . . ? C24 Fe C22 C23 37.20(19) . . . . ? C3 Fe C22 C23 162.9(3) . . . . ? C2 Fe C22 C21 77.4(2) . . . . ? C1 Fe C22 C21 119.63(19) . . . . ? C25 Fe C22 C21 -38.08(19) . . . . ? C5 Fe C22 C21 161.41(18) . . . . ? C4 Fe C22 C21 -165.9(3) . . . . ? C24 Fe C22 C21 -81.7(2) . . . . ? C3 Fe C22 C21 44.1(4) . . . . ? C23 Fe C22 C21 -118.9(3) . . . . ? C21 C22 C23 C24 0.5(3) . . . . ? Fe C22 C23 C24 -58.8(2) . . . . ? C21 C22 C23 Fe 59.3(2) . . . . ? C2 Fe C23 C22 41.0(4) . . . . ? C21 Fe C23 C22 -38.17(19) . . . . ? C1 Fe C23 C22 76.6(2) . . . . ? C25 Fe C23 C22 -82.3(2) . . . . ? C5 Fe C23 C22 119.74(19) . . . . ? C4 Fe C23 C22 162.33(18) . . . . ? C24 Fe C23 C22 -119.9(3) . . . . ? C3 Fe C23 C22 -161.2(3) . . . . ? C2 Fe C23 C24 160.9(3) . . . . ? C21 Fe C23 C24 81.7(2) . . . . ? C1 Fe C23 C24 -163.52(18) . . . . ? C22 Fe C23 C24 119.9(3) . . . . ? C25 Fe C23 C24 37.59(19) . . . . ? C5 Fe C23 C24 -120.4(2) . . . . ? C4 Fe C23 C24 -77.8(2) . . . . ? C3 Fe C23 C24 -41.3(4) . . . . ? C22 C23 C24 C25 -0.7(4) . . . . ? Fe C23 C24 C25 -59.4(2) . . . . ? C22 C23 C24 Fe 58.7(2) . . . . ? C2 Fe C24 C25 -41.9(4) . . . . ? C21 Fe C24 C25 37.77(19) . . . . ? C1 Fe C24 C25 161.6(3) . . . . ? C22 Fe C24 C25 82.0(2) . . . . ? C5 Fe C24 C25 -161.58(19) . . . . ? C4 Fe C24 C25 -119.0(2) . . . . ? C3 Fe C24 C25 -76.5(2) . . . . ? C23 Fe C24 C25 119.2(3) . . . . ? C2 Fe C24 C23 -161.1(3) . . . . ? C21 Fe C24 C23 -81.4(2) . . . . ? C1 Fe C24 C23 42.3(4) . . . . ? C22 Fe C24 C23 -37.21(19) . . . . ? C25 Fe C24 C23 -119.2(3) . . . . ? C5 Fe C24 C23 79.2(2) . . . . ? C4 Fe C24 C23 121.8(2) . . . . ? C3 Fe C24 C23 164.27(18) . . . . ? C23 C24 C25 C21 0.7(4) . . . . ? Fe C24 C25 C21 -59.0(2) . . . . ? C23 C24 C25 Fe 59.7(2) . . . . ? C22 C21 C25 C24 -0.4(3) . . . . ? Fe C21 C25 C24 59.5(2) . . . . ? C22 C21 C25 Fe -59.9(2) . . . . ? C2 Fe C25 C24 163.32(18) . . . . ? C21 Fe C25 C24 -119.4(3) . . . . ? C1 Fe C25 C24 -162.3(3) . . . . ? C22 Fe C25 C24 -81.2(2) . . . . ? C5 Fe C25 C24 47.4(4) . . . . ? C4 Fe C25 C24 80.1(2) . . . . ? C3 Fe C25 C24 121.8(2) . . . . ? C23 Fe C25 C24 -37.59(19) . . . . ? C2 Fe C25 C21 -77.3(2) . . . . ? C1 Fe C25 C21 -42.9(4) . . . . ? C22 Fe C25 C21 38.21(19) . . . . ? C5 Fe C25 C21 166.8(3) . . . . ? C4 Fe C25 C21 -160.52(18) . . . . ? C24 Fe C25 C21 119.4(3) . . . . ? C3 Fe C25 C21 -118.8(2) . . . . ? C23 Fe C25 C21 81.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.272 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.062 # Attachment 'rac11.cif' data_erk3374 _database_code_depnum_ccdc_archive 'CCDC 714370' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 Fe O3 Si' _chemical_formula_weight 526.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.465(1) _cell_length_b 12.947(1) _cell_length_c 14.191(1) _cell_angle_alpha 102.67(1) _cell_angle_beta 92.54(1) _cell_angle_gamma 95.95(1) _cell_volume 1327.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 12352 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9098 _exptl_absorpt_correction_T_max 0.9386 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12783 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.30 _reflns_number_total 5383 _reflns_number_gt 3905 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'DEnzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0398P)^2^+0.4290P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5383 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Fe Fe 0.17833(5) 0.14771(3) 0.91168(2) 0.02348(12) Uani 1 1 d . . . Si1 Si 0.36309(9) 0.34236(6) 0.69796(5) 0.02302(17) Uani 1 1 d . . . O1 O 0.3610(2) 0.24554(13) 0.75759(11) 0.0253(4) Uani 1 1 d . . . O2 O 0.3691(2) -0.01105(14) 0.64213(11) 0.0313(4) Uani 1 1 d . . . O3 O 0.3556(2) -0.08263(14) 0.77888(12) 0.0308(4) Uani 1 1 d . . . C1 C 0.2166(3) 0.1830(2) 0.78024(16) 0.0230(6) Uani 1 1 d . . . C2 C 0.2176(3) 0.0725(2) 0.77427(16) 0.0243(6) Uani 1 1 d . . . C3 C 0.0458(3) 0.0340(2) 0.80164(17) 0.0291(6) Uani 1 1 d . . . H3 H 0.0068 -0.0377 0.8035 0.035 Uiso 1 1 calc R . . C4 C -0.0563(3) 0.1215(2) 0.82563(17) 0.0299(6) Uani 1 1 d . . . H4 H -0.1753 0.1185 0.8467 0.036 Uiso 1 1 calc R . . C5 C 0.0493(3) 0.2141(2) 0.81276(17) 0.0289(6) Uani 1 1 d . . . H5 H 0.0145 0.2841 0.8238 0.035 Uiso 1 1 calc R . . C6 C 0.3710(3) 0.0112(2) 0.74407(16) 0.0259(6) Uani 1 1 d . . . H6 H 0.4868 0.0555 0.7720 0.031 Uiso 1 1 calc R . . C7 C 0.5216(4) -0.0654(2) 0.60995(19) 0.0389(7) Uani 1 1 d . . . H7A H 0.6349 -0.0188 0.6351 0.047 Uiso 1 1 calc R . . H7B H 0.5179 -0.0820 0.5383 0.047 Uiso 1 1 calc R . . C8 C 0.5186(4) -0.1674(2) 0.64531(18) 0.0356(7) Uani 1 1 d . . . H8A H 0.6296 -0.2011 0.6287 0.043 Uiso 1 1 calc R . . H8B H 0.4133 -0.2181 0.6139 0.043 Uiso 1 1 calc R . . C9 C 0.5066(4) -0.1412(2) 0.75400(19) 0.0365(7) Uani 1 1 d . . . H9A H 0.4923 -0.2079 0.7776 0.044 Uiso 1 1 calc R . . H9B H 0.6194 -0.0982 0.7856 0.044 Uiso 1 1 calc R . . C10 C 0.6087(3) 0.3709(2) 0.67807(17) 0.0290(6) Uani 1 1 d . . . C11 C 0.6822(4) 0.2670(2) 0.6303(2) 0.0431(8) Uani 1 1 d . . . H11A H 0.6148 0.2360 0.5679 0.065 Uiso 1 1 calc R . . H11B H 0.6683 0.2164 0.6725 0.065 Uiso 1 1 calc R . . H11C H 0.8103 0.2820 0.6199 0.065 Uiso 1 1 calc R . . C12 C 0.7155(4) 0.4177(3) 0.7758(2) 0.0442(8) Uani 1 1 d . . . H12A H 0.8441 0.4302 0.7654 0.066 Uiso 1 1 calc R . . H12B H 0.6981 0.3674 0.8181 0.066 Uiso 1 1 calc R . . H12C H 0.6723 0.4852 0.8062 0.066 Uiso 1 1 calc R . . C13 C 0.6348(4) 0.4497(3) 0.6122(2) 0.0600(10) Uani 1 1 d . . . H13A H 0.5966 0.5181 0.6442 0.090 Uiso 1 1 calc R . . H13B H 0.5621 0.4214 0.5510 0.090 Uiso 1 1 calc R . . H13C H 0.7625 0.4600 0.5992 0.090 Uiso 1 1 calc R . . C14 C 0.2163(3) 0.2931(2) 0.58297(17) 0.0260(6) Uani 1 1 d . . . C15 C 0.1650(4) 0.3610(2) 0.52495(19) 0.0358(7) Uani 1 1 d . . . H15 H 0.2055 0.4350 0.5440 0.043 Uiso 1 1 calc R . . C16 C 0.0562(4) 0.3223(3) 0.44008(19) 0.0395(7) Uani 1 1 d . . . H16 H 0.0242 0.3698 0.4014 0.047 Uiso 1 1 calc R . . C17 C -0.0053(3) 0.2158(2) 0.41172(19) 0.0360(7) Uani 1 1 d . . . H17 H -0.0814 0.1896 0.3542 0.043 Uiso 1 1 calc R . . C18 C 0.0441(4) 0.1468(2) 0.46723(18) 0.0356(7) Uani 1 1 d . . . H18 H 0.0020 0.0730 0.4478 0.043 Uiso 1 1 calc R . . C19 C 0.1549(3) 0.1851(2) 0.55142(17) 0.0292(6) Uani 1 1 d . . . H19 H 0.1897 0.1366 0.5883 0.035 Uiso 1 1 calc R . . C20 C 0.2832(3) 0.4603(2) 0.77996(17) 0.0273(6) Uani 1 1 d . . . C21 C 0.2766(4) 0.4613(2) 0.87825(18) 0.0369(7) Uani 1 1 d . . . H21 H 0.3105 0.4019 0.9010 0.044 Uiso 1 1 calc R . . C22 C 0.2222(4) 0.5464(3) 0.9436(2) 0.0459(8) Uani 1 1 d . . . H22 H 0.2159 0.5438 1.0098 0.055 Uiso 1 1 calc R . . C23 C 0.1773(4) 0.6341(3) 0.9131(2) 0.0455(8) Uani 1 1 d . . . H23 H 0.1414 0.6928 0.9581 0.055 Uiso 1 1 calc R . . C24 C 0.1845(4) 0.6371(3) 0.8172(2) 0.0524(9) Uani 1 1 d . . . H24 H 0.1538 0.6980 0.7957 0.063 Uiso 1 1 calc R . . C25 C 0.2364(4) 0.5512(2) 0.7518(2) 0.0431(8) Uani 1 1 d . . . H25 H 0.2404 0.5543 0.6856 0.052 Uiso 1 1 calc R . . C31 C 0.3908(3) 0.1166(2) 0.99024(18) 0.0348(7) Uani 1 1 d . . . H31 H 0.4836 0.0760 0.9648 0.042 Uiso 1 1 calc R . . C32 C 0.3927(4) 0.2273(2) 1.00148(18) 0.0370(7) Uani 1 1 d . . . H32 H 0.4865 0.2742 0.9851 0.044 Uiso 1 1 calc R . . C33 C 0.2306(4) 0.2563(2) 1.04146(18) 0.0360(7) Uani 1 1 d . . . H33 H 0.1960 0.3264 1.0566 0.043 Uiso 1 1 calc R . . C34 C 0.1288(4) 0.1632(2) 1.05507(17) 0.0327(6) Uani 1 1 d . . . H34 H 0.0139 0.1596 1.0811 0.039 Uiso 1 1 calc R . . C35 C 0.2284(4) 0.0759(2) 1.02303(17) 0.0321(6) Uani 1 1 d . . . H35 H 0.1924 0.0035 1.0236 0.039 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 Fe 0.02328(19) 0.0277(2) 0.02178(19) 0.01116(16) 0.00031(15) 0.00249(15) Si1 0.0217(3) 0.0269(4) 0.0227(3) 0.0120(3) -0.0003(3) 0.0005(3) O1 0.0225(9) 0.0288(11) 0.0278(9) 0.0147(8) 0.0011(7) -0.0001(8) O2 0.0402(10) 0.0344(11) 0.0223(9) 0.0090(8) 0.0037(8) 0.0123(9) O3 0.0361(10) 0.0313(11) 0.0304(9) 0.0151(8) 0.0056(8) 0.0094(8) C1 0.0210(12) 0.0301(16) 0.0205(12) 0.0134(11) -0.0007(10) -0.0004(11) C2 0.0249(13) 0.0294(16) 0.0202(12) 0.0107(11) -0.0021(11) 0.0009(11) C3 0.0285(13) 0.0339(17) 0.0244(13) 0.0100(12) -0.0033(11) -0.0044(12) C4 0.0206(13) 0.0409(18) 0.0308(14) 0.0157(13) -0.0004(11) 0.0000(12) C5 0.0277(13) 0.0360(17) 0.0281(13) 0.0159(12) 0.0012(11) 0.0091(12) C6 0.0295(13) 0.0276(15) 0.0220(12) 0.0097(11) -0.0001(11) 0.0014(11) C7 0.0451(17) 0.0402(19) 0.0342(15) 0.0084(13) 0.0123(14) 0.0140(14) C8 0.0364(15) 0.0345(18) 0.0356(15) 0.0045(13) 0.0028(13) 0.0104(13) C9 0.0385(16) 0.0362(18) 0.0389(15) 0.0128(13) 0.0010(13) 0.0150(14) C10 0.0245(13) 0.0360(17) 0.0290(13) 0.0155(12) -0.0002(11) -0.0011(12) C11 0.0316(15) 0.058(2) 0.0388(16) 0.0056(15) 0.0075(13) 0.0081(14) C12 0.0257(14) 0.051(2) 0.0477(18) -0.0019(15) -0.0063(13) -0.0014(14) C13 0.0381(17) 0.077(3) 0.082(2) 0.058(2) 0.0110(18) -0.0027(17) C14 0.0208(12) 0.0325(17) 0.0266(13) 0.0120(12) 0.0032(11) 0.0002(11) C15 0.0382(15) 0.0327(17) 0.0378(15) 0.0146(13) -0.0068(13) 0.0003(13) C16 0.0413(16) 0.046(2) 0.0340(15) 0.0175(14) -0.0126(13) 0.0039(15) C17 0.0273(14) 0.050(2) 0.0291(14) 0.0080(14) -0.0041(12) 0.0004(13) C18 0.0377(15) 0.0374(18) 0.0295(14) 0.0062(13) 0.0017(13) -0.0024(13) C19 0.0311(14) 0.0341(17) 0.0253(13) 0.0121(12) 0.0023(12) 0.0048(12) C20 0.0211(12) 0.0291(16) 0.0316(14) 0.0093(12) -0.0027(11) -0.0002(11) C21 0.0464(17) 0.0317(17) 0.0320(14) 0.0084(13) -0.0008(13) 0.0015(14) C22 0.0525(19) 0.048(2) 0.0317(15) -0.0009(15) 0.0011(14) -0.0001(16) C23 0.0355(16) 0.043(2) 0.0498(18) -0.0070(15) -0.0035(14) 0.0089(15) C24 0.058(2) 0.041(2) 0.060(2) 0.0101(16) -0.0045(17) 0.0225(17) C25 0.0521(18) 0.044(2) 0.0375(16) 0.0135(14) -0.0007(14) 0.0175(16) C31 0.0304(14) 0.049(2) 0.0295(14) 0.0157(13) -0.0036(12) 0.0136(14) C32 0.0326(15) 0.046(2) 0.0323(15) 0.0166(14) -0.0105(12) -0.0071(14) C33 0.0502(17) 0.0298(17) 0.0259(13) 0.0037(12) -0.0066(13) 0.0044(14) C34 0.0393(15) 0.0381(18) 0.0231(13) 0.0108(12) 0.0039(12) 0.0074(13) C35 0.0441(16) 0.0312(17) 0.0258(13) 0.0165(12) -0.0011(12) 0.0054(13) _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 Fe C31 2.023(2) . ? Fe C2 2.028(2) . ? Fe C3 2.034(3) . ? Fe C32 2.036(3) . ? Fe C1 2.040(2) . ? Fe C35 2.041(2) . ? Fe C4 2.044(2) . ? Fe C33 2.052(3) . ? Fe C5 2.054(2) . ? Fe C34 2.054(2) . ? Si1 O1 1.6584(16) . ? Si1 C14 1.874(3) . ? Si1 C20 1.874(3) . ? Si1 C10 1.879(2) . ? O1 C1 1.373(3) . ? O2 C6 1.411(3) . ? O2 C7 1.439(3) . ? O3 C6 1.404(3) . ? O3 C9 1.437(3) . ? C1 C2 1.414(3) . ? C1 C5 1.417(3) . ? C2 C3 1.429(3) . ? C2 C6 1.486(3) . ? C3 C4 1.419(4) . ? C4 C5 1.416(4) . ? C7 C8 1.511(4) . ? C8 C9 1.514(3) . ? C10 C13 1.532(3) . ? C10 C12 1.536(4) . ? C10 C11 1.535(4) . ? C14 C19 1.393(4) . ? C14 C15 1.398(3) . ? C15 C16 1.388(4) . ? C16 C17 1.373(4) . ? C17 C18 1.380(4) . ? C18 C19 1.388(4) . ? C20 C25 1.395(4) . ? C20 C21 1.395(3) . ? C21 C22 1.384(4) . ? C22 C23 1.368(4) . ? C23 C24 1.373(4) . ? C24 C25 1.384(4) . ? C31 C32 1.404(4) . ? C31 C35 1.411(4) . ? C32 C33 1.410(4) . ? C33 C34 1.412(4) . ? C34 C35 1.420(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31 Fe C2 103.47(10) . . ? C31 Fe C3 121.26(11) . . ? C2 Fe C3 41.19(9) . . ? C31 Fe C32 40.48(11) . . ? C2 Fe C32 119.82(10) . . ? C3 Fe C32 156.85(11) . . ? C31 Fe C1 119.49(10) . . ? C2 Fe C1 40.68(10) . . ? C3 Fe C1 68.21(10) . . ? C32 Fe C1 106.01(10) . . ? C31 Fe C35 40.61(10) . . ? C2 Fe C35 119.67(10) . . ? C3 Fe C35 107.08(11) . . ? C32 Fe C35 68.28(11) . . ? C1 Fe C35 155.28(10) . . ? C31 Fe C4 159.46(11) . . ? C2 Fe C4 68.94(10) . . ? C3 Fe C4 40.73(10) . . ? C32 Fe C4 159.85(11) . . ? C1 Fe C4 67.89(9) . . ? C35 Fe C4 125.35(11) . . ? C31 Fe C33 67.90(11) . . ? C2 Fe C33 157.52(11) . . ? C3 Fe C33 160.98(10) . . ? C32 Fe C33 40.36(11) . . ? C1 Fe C33 124.02(11) . . ? C35 Fe C33 68.11(11) . . ? C4 Fe C33 125.96(11) . . ? C31 Fe C5 156.41(10) . . ? C2 Fe C5 68.92(10) . . ? C3 Fe C5 68.47(10) . . ? C32 Fe C5 122.61(11) . . ? C1 Fe C5 40.51(9) . . ? C35 Fe C5 162.48(10) . . ? C4 Fe C5 40.41(10) . . ? C33 Fe C5 110.25(11) . . ? C31 Fe C34 67.97(10) . . ? C2 Fe C34 157.65(10) . . ? C3 Fe C34 124.29(11) . . ? C32 Fe C34 67.87(11) . . ? C1 Fe C34 161.54(10) . . ? C35 Fe C34 40.58(10) . . ? C4 Fe C34 111.50(10) . . ? C33 Fe C34 40.23(10) . . ? C5 Fe C34 126.90(10) . . ? O1 Si1 C14 108.74(11) . . ? O1 Si1 C20 107.53(10) . . ? C14 Si1 C20 112.83(11) . . ? O1 Si1 C10 103.12(10) . . ? C14 Si1 C10 113.59(10) . . ? C20 Si1 C10 110.39(12) . . ? C1 O1 Si1 129.32(14) . . ? C6 O2 C7 110.18(18) . . ? C6 O3 C9 110.63(18) . . ? O1 C1 C2 122.6(2) . . ? O1 C1 C5 128.1(2) . . ? C2 C1 C5 109.3(2) . . ? O1 C1 Fe 126.32(16) . . ? C2 C1 Fe 69.19(12) . . ? C5 C1 Fe 70.25(12) . . ? C1 C2 C3 106.9(2) . . ? C1 C2 C6 125.0(2) . . ? C3 C2 C6 128.0(2) . . ? C1 C2 Fe 70.13(13) . . ? C3 C2 Fe 69.63(13) . . ? C6 C2 Fe 125.68(17) . . ? C4 C3 C2 108.1(2) . . ? C4 C3 Fe 70.03(15) . . ? C2 C3 Fe 69.18(14) . . ? C5 C4 C3 108.4(2) . . ? C5 C4 Fe 70.15(14) . . ? C3 C4 Fe 69.24(14) . . ? C4 C5 C1 107.3(2) . . ? C4 C5 Fe 69.44(14) . . ? C1 C5 Fe 69.24(13) . . ? O3 C6 O2 111.6(2) . . ? O3 C6 C2 109.61(18) . . ? O2 C6 C2 108.33(19) . . ? O2 C7 C8 110.1(2) . . ? C7 C8 C9 108.6(2) . . ? O3 C9 C8 110.0(2) . . ? C13 C10 C12 109.5(2) . . ? C13 C10 C11 108.8(2) . . ? C12 C10 C11 108.6(2) . . ? C13 C10 Si1 110.63(18) . . ? C12 C10 Si1 109.65(16) . . ? C11 C10 Si1 109.61(19) . . ? C19 C14 C15 117.1(2) . . ? C19 C14 Si1 120.31(18) . . ? C15 C14 Si1 122.5(2) . . ? C16 C15 C14 121.3(3) . . ? C17 C16 C15 120.3(3) . . ? C16 C17 C18 119.7(3) . . ? C17 C18 C19 120.1(3) . . ? C18 C19 C14 121.4(2) . . ? C25 C20 C21 116.1(2) . . ? C25 C20 Si1 125.27(19) . . ? C21 C20 Si1 118.53(19) . . ? C22 C21 C20 121.9(3) . . ? C23 C22 C21 120.2(3) . . ? C22 C23 C24 119.8(3) . . ? C23 C24 C25 119.9(3) . . ? C24 C25 C20 122.1(3) . . ? C32 C31 C35 108.8(2) . . ? C32 C31 Fe 70.26(15) . . ? C35 C31 Fe 70.38(14) . . ? C31 C32 C33 107.9(2) . . ? C31 C32 Fe 69.26(16) . . ? C33 C32 Fe 70.41(16) . . ? C32 C33 C34 108.0(2) . . ? C32 C33 Fe 69.24(16) . . ? C34 C33 Fe 69.99(15) . . ? C33 C34 C35 108.0(2) . . ? C33 C34 Fe 69.78(14) . . ? C35 C34 Fe 69.21(13) . . ? C31 C35 C34 107.3(2) . . ? C31 C35 Fe 69.01(13) . . ? C34 C35 Fe 70.21(13) . . ? 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 C14 Si1 O1 C1 -49.4(2) . . . . ? C20 Si1 O1 C1 73.0(2) . . . . ? C10 Si1 O1 C1 -170.3(2) . . . . ? Si1 O1 C1 C2 139.38(19) . . . . ? Si1 O1 C1 C5 -41.2(3) . . . . ? Si1 O1 C1 Fe -133.69(15) . . . . ? C31 Fe C1 O1 -40.1(2) . . . . ? C2 Fe C1 O1 -115.8(2) . . . . ? C3 Fe C1 O1 -154.7(2) . . . . ? C32 Fe C1 O1 1.6(2) . . . . ? C35 Fe C1 O1 -71.1(4) . . . . ? C4 Fe C1 O1 161.2(2) . . . . ? C33 Fe C1 O1 41.8(2) . . . . ? C5 Fe C1 O1 123.4(3) . . . . ? C34 Fe C1 O1 69.3(4) . . . . ? C31 Fe C1 C2 75.69(17) . . . . ? C3 Fe C1 C2 -38.90(14) . . . . ? C32 Fe C1 C2 117.37(15) . . . . ? C35 Fe C1 C2 44.7(3) . . . . ? C4 Fe C1 C2 -82.97(16) . . . . ? C33 Fe C1 C2 157.66(15) . . . . ? C5 Fe C1 C2 -120.8(2) . . . . ? C34 Fe C1 C2 -174.8(3) . . . . ? C31 Fe C1 C5 -163.50(16) . . . . ? C2 Fe C1 C5 120.8(2) . . . . ? C3 Fe C1 C5 81.91(17) . . . . ? C32 Fe C1 C5 -121.82(17) . . . . ? C35 Fe C1 C5 165.5(2) . . . . ? C4 Fe C1 C5 37.84(16) . . . . ? C33 Fe C1 C5 -81.53(19) . . . . ? C34 Fe C1 C5 -54.0(4) . . . . ? O1 C1 C2 C3 -179.2(2) . . . . ? C5 C1 C2 C3 1.3(3) . . . . ? Fe C1 C2 C3 60.19(16) . . . . ? O1 C1 C2 C6 0.3(4) . . . . ? C5 C1 C2 C6 -179.2(2) . . . . ? Fe C1 C2 C6 -120.3(2) . . . . ? O1 C1 C2 Fe 120.6(2) . . . . ? C5 C1 C2 Fe -58.93(17) . . . . ? C31 Fe C2 C1 -119.85(15) . . . . ? C3 Fe C2 C1 117.7(2) . . . . ? C32 Fe C2 C1 -79.69(16) . . . . ? C35 Fe C2 C1 -160.22(14) . . . . ? C4 Fe C2 C1 80.17(15) . . . . ? C33 Fe C2 C1 -55.5(3) . . . . ? C5 Fe C2 C1 36.72(14) . . . . ? C34 Fe C2 C1 175.7(2) . . . . ? C31 Fe C2 C3 122.45(16) . . . . ? C32 Fe C2 C3 162.62(15) . . . . ? C1 Fe C2 C3 -117.7(2) . . . . ? C35 Fe C2 C3 82.09(17) . . . . ? C4 Fe C2 C3 -37.53(15) . . . . ? C33 Fe C2 C3 -173.2(2) . . . . ? C5 Fe C2 C3 -80.97(15) . . . . ? C34 Fe C2 C3 58.0(3) . . . . ? C31 Fe C2 C6 -0.4(2) . . . . ? C3 Fe C2 C6 -122.9(3) . . . . ? C32 Fe C2 C6 39.8(2) . . . . ? C1 Fe C2 C6 119.4(3) . . . . ? C35 Fe C2 C6 -40.8(2) . . . . ? C4 Fe C2 C6 -160.4(2) . . . . ? C33 Fe C2 C6 64.0(4) . . . . ? C5 Fe C2 C6 156.2(2) . . . . ? C34 Fe C2 C6 -64.9(4) . . . . ? C1 C2 C3 C4 -1.1(3) . . . . ? C6 C2 C3 C4 179.4(2) . . . . ? Fe C2 C3 C4 59.45(17) . . . . ? C1 C2 C3 Fe -60.51(16) . . . . ? C6 C2 C3 Fe 120.0(2) . . . . ? C31 Fe C3 C4 166.85(14) . . . . ? C2 Fe C3 C4 -119.4(2) . . . . ? C32 Fe C3 C4 -160.6(2) . . . . ? C1 Fe C3 C4 -80.97(14) . . . . ? C35 Fe C3 C4 124.80(14) . . . . ? C33 Fe C3 C4 52.6(4) . . . . ? C5 Fe C3 C4 -37.23(13) . . . . ? C34 Fe C3 C4 83.57(17) . . . . ? C31 Fe C3 C2 -73.75(17) . . . . ? C32 Fe C3 C2 -41.2(3) . . . . ? C1 Fe C3 C2 38.43(14) . . . . ? C35 Fe C3 C2 -115.80(15) . . . . ? C4 Fe C3 C2 119.4(2) . . . . ? C33 Fe C3 C2 172.0(3) . . . . ? C5 Fe C3 C2 82.17(14) . . . . ? C34 Fe C3 C2 -157.02(14) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? Fe C3 C4 C5 59.40(17) . . . . ? C2 C3 C4 Fe -58.92(17) . . . . ? C31 Fe C4 C5 -153.4(3) . . . . ? C2 Fe C4 C5 -81.82(15) . . . . ? C3 Fe C4 C5 -119.8(2) . . . . ? C32 Fe C4 C5 38.0(3) . . . . ? C1 Fe C4 C5 -37.93(14) . . . . ? C35 Fe C4 C5 166.02(14) . . . . ? C33 Fe C4 C5 78.90(17) . . . . ? C34 Fe C4 C5 122.19(15) . . . . ? C31 Fe C4 C3 -33.7(3) . . . . ? C2 Fe C4 C3 37.93(14) . . . . ? C32 Fe C4 C3 157.8(3) . . . . ? C1 Fe C4 C3 81.82(15) . . . . ? C35 Fe C4 C3 -74.23(17) . . . . ? C33 Fe C4 C3 -161.35(14) . . . . ? C5 Fe C4 C3 119.8(2) . . . . ? C34 Fe C4 C3 -118.06(15) . . . . ? C3 C4 C5 C1 0.3(3) . . . . ? Fe C4 C5 C1 59.14(16) . . . . ? C3 C4 C5 Fe -58.84(17) . . . . ? O1 C1 C5 C4 179.5(2) . . . . ? C2 C1 C5 C4 -1.0(3) . . . . ? Fe C1 C5 C4 -59.26(17) . . . . ? O1 C1 C5 Fe -121.2(2) . . . . ? C2 C1 C5 Fe 58.29(16) . . . . ? C31 Fe C5 C4 156.9(2) . . . . ? C2 Fe C5 C4 81.88(16) . . . . ? C3 Fe C5 C4 37.52(15) . . . . ? C32 Fe C5 C4 -165.41(15) . . . . ? C1 Fe C5 C4 118.8(2) . . . . ? C35 Fe C5 C4 -40.9(4) . . . . ? C33 Fe C5 C4 -122.15(16) . . . . ? C34 Fe C5 C4 -79.94(19) . . . . ? C31 Fe C5 C1 38.1(3) . . . . ? C2 Fe C5 C1 -36.87(15) . . . . ? C3 Fe C5 C1 -81.23(16) . . . . ? C32 Fe C5 C1 75.84(19) . . . . ? C35 Fe C5 C1 -159.6(3) . . . . ? C4 Fe C5 C1 -118.8(2) . . . . ? C33 Fe C5 C1 119.10(16) . . . . ? C34 Fe C5 C1 161.31(16) . . . . ? C9 O3 C6 O2 62.4(3) . . . . ? C9 O3 C6 C2 -177.6(2) . . . . ? C7 O2 C6 O3 -62.4(3) . . . . ? C7 O2 C6 C2 176.9(2) . . . . ? C1 C2 C6 O3 158.6(2) . . . . ? C3 C2 C6 O3 -21.9(3) . . . . ? Fe C2 C6 O3 69.1(3) . . . . ? C1 C2 C6 O2 -79.4(3) . . . . ? C3 C2 C6 O2 100.1(3) . . . . ? Fe C2 C6 O2 -168.91(16) . . . . ? C6 O2 C7 C8 58.2(3) . . . . ? O2 C7 C8 C9 -54.1(3) . . . . ? C6 O3 C9 C8 -57.9(3) . . . . ? C7 C8 C9 O3 53.7(3) . . . . ? O1 Si1 C10 C13 172.9(2) . . . . ? C14 Si1 C10 C13 55.4(2) . . . . ? C20 Si1 C10 C13 -72.5(2) . . . . ? O1 Si1 C10 C12 -66.3(2) . . . . ? C14 Si1 C10 C12 176.24(18) . . . . ? C20 Si1 C10 C12 48.4(2) . . . . ? O1 Si1 C10 C11 52.89(19) . . . . ? C14 Si1 C10 C11 -64.6(2) . . . . ? C20 Si1 C10 C11 167.51(17) . . . . ? O1 Si1 C14 C19 -12.0(2) . . . . ? C20 Si1 C14 C19 -131.16(18) . . . . ? C10 Si1 C14 C19 102.2(2) . . . . ? O1 Si1 C14 C15 168.66(18) . . . . ? C20 Si1 C14 C15 49.5(2) . . . . ? C10 Si1 C14 C15 -77.2(2) . . . . ? C19 C14 C15 C16 0.6(4) . . . . ? Si1 C14 C15 C16 179.98(19) . . . . ? C14 C15 C16 C17 0.7(4) . . . . ? C15 C16 C17 C18 -1.0(4) . . . . ? C16 C17 C18 C19 0.1(4) . . . . ? C17 C18 C19 C14 1.2(4) . . . . ? C15 C14 C19 C18 -1.5(3) . . . . ? Si1 C14 C19 C18 179.09(18) . . . . ? O1 Si1 C20 C25 -168.5(2) . . . . ? C14 Si1 C20 C25 -48.6(3) . . . . ? C10 Si1 C20 C25 79.7(3) . . . . ? O1 Si1 C20 C21 14.6(2) . . . . ? C14 Si1 C20 C21 134.5(2) . . . . ? C10 Si1 C20 C21 -97.2(2) . . . . ? C25 C20 C21 C22 1.7(4) . . . . ? Si1 C20 C21 C22 178.9(2) . . . . ? C20 C21 C22 C23 -1.7(5) . . . . ? C21 C22 C23 C24 0.8(5) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? C23 C24 C25 C20 -0.2(5) . . . . ? C21 C20 C25 C24 -0.7(4) . . . . ? Si1 C20 C25 C24 -177.7(2) . . . . ? C2 Fe C31 C32 120.46(15) . . . . ? C3 Fe C31 C32 161.01(14) . . . . ? C1 Fe C31 C32 79.95(17) . . . . ? C35 Fe C31 C32 -119.4(2) . . . . ? C4 Fe C31 C32 -174.0(2) . . . . ? C33 Fe C31 C32 -37.70(15) . . . . ? C5 Fe C31 C32 52.5(3) . . . . ? C34 Fe C31 C32 -81.26(16) . . . . ? C2 Fe C31 C35 -120.17(16) . . . . ? C3 Fe C31 C35 -79.62(18) . . . . ? C32 Fe C31 C35 119.4(2) . . . . ? C1 Fe C31 C35 -160.67(15) . . . . ? C4 Fe C31 C35 -54.6(3) . . . . ? C33 Fe C31 C35 81.68(17) . . . . ? C5 Fe C31 C35 171.9(2) . . . . ? C34 Fe C31 C35 38.11(16) . . . . ? C35 C31 C32 C33 0.0(3) . . . . ? Fe C31 C32 C33 60.04(18) . . . . ? C35 C31 C32 Fe -60.09(18) . . . . ? C2 Fe C32 C31 -75.06(17) . . . . ? C3 Fe C32 C31 -45.0(3) . . . . ? C1 Fe C32 C31 -116.91(15) . . . . ? C35 Fe C32 C31 37.63(14) . . . . ? C4 Fe C32 C31 173.9(2) . . . . ? C33 Fe C32 C31 118.9(2) . . . . ? C5 Fe C32 C31 -157.85(14) . . . . ? C34 Fe C32 C31 81.53(16) . . . . ? C31 Fe C32 C33 -118.9(2) . . . . ? C2 Fe C32 C33 165.99(14) . . . . ? C3 Fe C32 C33 -164.0(2) . . . . ? C1 Fe C32 C33 124.14(16) . . . . ? C35 Fe C32 C33 -81.32(16) . . . . ? C4 Fe C32 C33 54.9(3) . . . . ? C5 Fe C32 C33 83.20(17) . . . . ? C34 Fe C32 C33 -37.41(15) . . . . ? C31 C32 C33 C34 0.1(3) . . . . ? Fe C32 C33 C34 59.45(18) . . . . ? C31 C32 C33 Fe -59.32(18) . . . . ? C31 Fe C33 C32 37.81(15) . . . . ? C2 Fe C33 C32 -33.3(3) . . . . ? C3 Fe C33 C32 160.6(3) . . . . ? C1 Fe C33 C32 -73.71(18) . . . . ? C35 Fe C33 C32 81.77(17) . . . . ? C4 Fe C33 C32 -159.62(15) . . . . ? C5 Fe C33 C32 -116.93(16) . . . . ? C34 Fe C33 C32 119.4(2) . . . . ? C31 Fe C33 C34 -81.56(17) . . . . ? C2 Fe C33 C34 -152.7(2) . . . . ? C3 Fe C33 C34 41.2(4) . . . . ? C32 Fe C33 C34 -119.4(2) . . . . ? C1 Fe C33 C34 166.92(14) . . . . ? C35 Fe C33 C34 -37.60(15) . . . . ? C4 Fe C33 C34 81.00(18) . . . . ? C5 Fe C33 C34 123.70(16) . . . . ? C32 C33 C34 C35 -0.2(3) . . . . ? Fe C33 C34 C35 58.82(17) . . . . ? C32 C33 C34 Fe -58.98(18) . . . . ? C31 Fe C34 C33 81.37(18) . . . . ? C2 Fe C34 C33 152.5(2) . . . . ? C3 Fe C34 C33 -164.94(15) . . . . ? C32 Fe C34 C33 37.53(16) . . . . ? C1 Fe C34 C33 -36.3(4) . . . . ? C35 Fe C34 C33 119.5(2) . . . . ? C4 Fe C34 C33 -120.76(17) . . . . ? C5 Fe C34 C33 -77.4(2) . . . . ? C31 Fe C34 C35 -38.14(17) . . . . ? C2 Fe C34 C35 33.0(3) . . . . ? C3 Fe C34 C35 75.55(19) . . . . ? C32 Fe C34 C35 -81.98(18) . . . . ? C1 Fe C34 C35 -155.9(3) . . . . ? C4 Fe C34 C35 119.73(17) . . . . ? C33 Fe C34 C35 -119.5(2) . . . . ? C5 Fe C34 C35 163.05(16) . . . . ? C32 C31 C35 C34 0.0(3) . . . . ? Fe C31 C35 C34 -60.07(17) . . . . ? C32 C31 C35 Fe 60.02(18) . . . . ? C33 C34 C35 C31 0.1(3) . . . . ? Fe C34 C35 C31 59.31(17) . . . . ? C33 C34 C35 Fe -59.18(17) . . . . ? C2 Fe C35 C31 75.38(19) . . . . ? C3 Fe C35 C31 118.41(17) . . . . ? C32 Fe C35 C31 -37.51(16) . . . . ? C1 Fe C35 C31 43.5(3) . . . . ? C4 Fe C35 C31 159.47(16) . . . . ? C33 Fe C35 C31 -81.13(18) . . . . ? C5 Fe C35 C31 -169.2(3) . . . . ? C34 Fe C35 C31 -118.4(2) . . . . ? C31 Fe C35 C34 118.4(2) . . . . ? C2 Fe C35 C34 -166.20(16) . . . . ? C3 Fe C35 C34 -123.18(17) . . . . ? C32 Fe C35 C34 80.90(18) . . . . ? C1 Fe C35 C34 162.0(2) . . . . ? C4 Fe C35 C34 -82.11(19) . . . . ? C33 Fe C35 C34 37.28(17) . . . . ? C5 Fe C35 C34 -50.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.373 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.063 # Attachment 'rac12.cif' data_erk3373 _database_code_depnum_ccdc_archive 'CCDC 714371' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H28 Fe O2 Si' _chemical_formula_weight 468.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.377(1) _cell_length_b 10.308(1) _cell_length_c 12.984(1) _cell_angle_alpha 91.75(1) _cell_angle_beta 103.04(1) _cell_angle_gamma 106.67(1) _cell_volume 1165.14(19) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 11999 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8130 _exptl_absorpt_correction_T_max 0.9315 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10991 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.30 _reflns_number_total 4713 _reflns_number_gt 3438 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0612P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4713 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 Fe Fe 0.98804(4) 0.34131(4) 0.24019(2) 0.03397(14) Uani 1 1 d . . . Si1 Si 0.78177(8) -0.11016(7) 0.23554(5) 0.02699(18) Uani 1 1 d . . . O1 O 0.7819(2) 0.04990(16) 0.22693(11) 0.0343(4) Uani 1 1 d . . . O2 O 0.5830(3) 0.3616(2) 0.24757(17) 0.0680(7) Uani 1 1 d . . . C1 C 0.8615(3) 0.1692(2) 0.28849(17) 0.0322(6) Uani 1 1 d . . . C2 C 0.7961(3) 0.2775(3) 0.29727(18) 0.0351(6) Uani 1 1 d . . . C3 C 0.9118(4) 0.3864(3) 0.36679(18) 0.0430(7) Uani 1 1 d . . . H3 H 0.9020 0.4724 0.3863 0.052 Uiso 1 1 calc R . . C4 C 1.0420(4) 0.3437(3) 0.40080(18) 0.0470(8) Uani 1 1 d . . . H4 H 1.1351 0.3964 0.4483 0.056 Uiso 1 1 calc R . . C5 C 1.0140(3) 0.2103(3) 0.35370(18) 0.0405(7) Uani 1 1 d . . . H5 H 1.0838 0.1581 0.3637 0.049 Uiso 1 1 calc R . . C6 C 0.6446(4) 0.2755(3) 0.2373(2) 0.0455(7) Uani 1 1 d . . . H6 H 0.5893 0.2002 0.1856 0.055 Uiso 1 1 calc R . . C7 C 0.6659(3) -0.1949(3) 0.09895(17) 0.0339(6) Uani 1 1 d . . . C8 C 0.4979(3) -0.2049(4) 0.0870(2) 0.0584(9) Uani 1 1 d . . . H8A H 0.4392 -0.2442 0.0149 0.088 Uiso 1 1 calc R . . H8B H 0.4886 -0.1139 0.1000 0.088 Uiso 1 1 calc R . . H8C H 0.4574 -0.2632 0.1385 0.088 Uiso 1 1 calc R . . C9 C 0.6816(4) -0.3368(3) 0.0783(2) 0.0500(8) Uani 1 1 d . . . H9A H 0.6166 -0.3790 0.0083 0.075 Uiso 1 1 calc R . . H9B H 0.6495 -0.3934 0.1332 0.075 Uiso 1 1 calc R . . H9C H 0.7889 -0.3288 0.0802 0.075 Uiso 1 1 calc R . . C10 C 0.7244(4) -0.1078(3) 0.01428(18) 0.0441(7) Uani 1 1 d . . . H10A H 0.8329 -0.0998 0.0210 0.066 Uiso 1 1 calc R . . H10B H 0.7132 -0.0170 0.0245 0.066 Uiso 1 1 calc R . . H10C H 0.6644 -0.1511 -0.0566 0.066 Uiso 1 1 calc R . . C11 C 0.6888(3) -0.1764(2) 0.34402(16) 0.0283(5) Uani 1 1 d . . . C12 C 0.6172(3) -0.3138(3) 0.34487(19) 0.0423(7) Uani 1 1 d . . . H12 H 0.6173 -0.3761 0.2895 0.051 Uiso 1 1 calc R . . C13 C 0.5453(4) -0.3632(3) 0.42416(19) 0.0495(8) Uani 1 1 d . . . H13 H 0.4951 -0.4578 0.4220 0.059 Uiso 1 1 calc R . . C14 C 0.5472(4) -0.2737(3) 0.5066(2) 0.0483(8) Uani 1 1 d . . . H14 H 0.4993 -0.3066 0.5618 0.058 Uiso 1 1 calc R . . C15 C 0.6185(4) -0.1375(3) 0.50791(19) 0.0448(7) Uani 1 1 d . . . H15 H 0.6205 -0.0761 0.5647 0.054 Uiso 1 1 calc R . . C16 C 0.6880(3) -0.0879(3) 0.42744(17) 0.0374(6) Uani 1 1 d . . . H16 H 0.7354 0.0071 0.4291 0.045 Uiso 1 1 calc R . . C17 C 0.9801(3) -0.1242(2) 0.26606(17) 0.0297(6) Uani 1 1 d . . . C18 C 1.0290(3) -0.1988(3) 0.34795(18) 0.0353(6) Uani 1 1 d . . . H18 H 0.9623 -0.2367 0.3919 0.042 Uiso 1 1 calc R . . C19 C 1.1716(3) -0.2186(3) 0.36630(19) 0.0409(7) Uani 1 1 d . . . H19 H 1.2017 -0.2700 0.4221 0.049 Uiso 1 1 calc R . . C20 C 1.2703(3) -0.1645(3) 0.3043(2) 0.0419(7) Uani 1 1 d . . . H20 H 1.3679 -0.1793 0.3165 0.050 Uiso 1 1 calc R . . C21 C 1.2271(3) -0.0884(3) 0.2241(2) 0.0438(7) Uani 1 1 d . . . H21 H 1.2954 -0.0500 0.1814 0.053 Uiso 1 1 calc R . . C22 C 1.0850(3) -0.0684(3) 0.20617(19) 0.0377(6) Uani 1 1 d . . . H22 H 1.0574 -0.0148 0.1513 0.045 Uiso 1 1 calc R . . C31 C 0.9301(4) 0.3978(3) 0.09027(19) 0.0520(8) Uani 1 1 d . . . H31 H 0.8296 0.3924 0.0511 0.062 Uiso 1 1 calc R . . C32 C 1.0021(4) 0.2946(3) 0.0900(2) 0.0573(9) Uani 1 1 d . . . H32 H 0.9581 0.2075 0.0506 0.069 Uiso 1 1 calc R . . C33 C 1.1496(4) 0.3432(4) 0.1579(2) 0.0608(9) Uani 1 1 d . . . H33 H 1.2231 0.2949 0.1728 0.073 Uiso 1 1 calc R . . C34 C 1.1691(4) 0.4765(3) 0.2001(2) 0.0495(8) Uani 1 1 d . . . H34 H 1.2586 0.5340 0.2483 0.059 Uiso 1 1 calc R . . C35 C 1.0339(4) 0.5099(3) 0.1589(2) 0.0460(7) Uani 1 1 d . . . H35 H 1.0157 0.5935 0.1747 0.055 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 Fe 0.0422(3) 0.0313(2) 0.0299(2) 0.00333(14) 0.01182(16) 0.01088(19) Si1 0.0291(4) 0.0262(4) 0.0289(3) 0.0046(3) 0.0082(3) 0.0124(3) O1 0.0399(12) 0.0261(10) 0.0373(9) 0.0038(7) 0.0044(8) 0.0144(9) O2 0.0672(18) 0.0612(16) 0.0981(16) 0.0146(12) 0.0306(13) 0.0452(14) C1 0.0427(17) 0.0288(14) 0.0275(11) 0.0050(9) 0.0107(11) 0.0129(13) C2 0.0473(18) 0.0332(15) 0.0345(12) 0.0087(10) 0.0206(12) 0.0185(14) C3 0.065(2) 0.0351(16) 0.0318(13) 0.0003(11) 0.0174(13) 0.0150(15) C4 0.059(2) 0.0416(17) 0.0300(13) 0.0015(11) 0.0053(13) 0.0046(15) C5 0.0440(19) 0.0408(17) 0.0357(13) 0.0069(11) 0.0038(12) 0.0159(14) C6 0.049(2) 0.0453(18) 0.0535(16) 0.0106(13) 0.0215(14) 0.0246(16) C7 0.0337(16) 0.0392(16) 0.0298(12) 0.0046(10) 0.0094(10) 0.0113(13) C8 0.0355(19) 0.095(3) 0.0390(15) 0.0015(15) 0.0022(12) 0.0172(18) C9 0.069(2) 0.0338(16) 0.0419(15) -0.0022(11) 0.0125(14) 0.0096(15) C10 0.053(2) 0.0479(18) 0.0317(13) 0.0057(11) 0.0086(12) 0.0163(15) C11 0.0252(14) 0.0315(14) 0.0296(11) 0.0053(9) 0.0029(10) 0.0133(12) C12 0.061(2) 0.0372(17) 0.0360(13) 0.0071(11) 0.0157(13) 0.0231(15) C13 0.070(2) 0.0382(17) 0.0423(15) 0.0161(12) 0.0200(14) 0.0141(16) C14 0.060(2) 0.056(2) 0.0390(14) 0.0181(13) 0.0229(13) 0.0236(17) C15 0.053(2) 0.0503(19) 0.0333(13) 0.0006(11) 0.0126(12) 0.0177(16) C16 0.0393(17) 0.0352(15) 0.0362(13) 0.0019(11) 0.0102(12) 0.0083(13) C17 0.0307(15) 0.0278(14) 0.0316(11) 0.0009(9) 0.0066(10) 0.0115(12) C18 0.0375(17) 0.0350(15) 0.0352(12) 0.0055(10) 0.0085(11) 0.0135(13) C19 0.0360(17) 0.0432(17) 0.0439(14) 0.0072(12) 0.0018(12) 0.0186(14) C20 0.0333(17) 0.0440(17) 0.0507(15) -0.0034(12) 0.0076(13) 0.0182(14) C21 0.0341(17) 0.0511(19) 0.0507(15) 0.0063(13) 0.0167(13) 0.0149(15) C22 0.0350(17) 0.0425(17) 0.0396(13) 0.0105(11) 0.0098(12) 0.0169(14) C31 0.055(2) 0.060(2) 0.0330(14) 0.0121(13) 0.0124(13) 0.0029(17) C32 0.082(3) 0.0414(18) 0.0444(16) -0.0034(13) 0.0355(17) -0.0017(18) C33 0.064(3) 0.065(2) 0.068(2) 0.0106(17) 0.0395(19) 0.025(2) C34 0.042(2) 0.051(2) 0.0514(16) 0.0064(13) 0.0196(14) 0.0005(15) C35 0.056(2) 0.0367(17) 0.0436(15) 0.0113(12) 0.0164(14) 0.0069(15) _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 Fe C3 2.026(3) . ? Fe C4 2.029(2) . ? Fe C1 2.036(3) . ? Fe C32 2.036(3) . ? Fe C33 2.037(3) . ? Fe C2 2.043(3) . ? Fe C34 2.044(3) . ? Fe C31 2.049(2) . ? Fe C5 2.051(2) . ? Fe C35 2.051(3) . ? Si1 O1 1.6567(16) . ? Si1 C17 1.860(3) . ? Si1 C11 1.866(2) . ? Si1 C7 1.892(2) . ? O1 C1 1.361(3) . ? O2 C6 1.209(3) . ? C1 C5 1.423(4) . ? C1 C2 1.432(3) . ? C2 C3 1.432(4) . ? C2 C6 1.452(4) . ? C3 C4 1.398(4) . ? C4 C5 1.416(4) . ? C7 C8 1.521(4) . ? C7 C9 1.534(4) . ? C7 C10 1.538(3) . ? C11 C12 1.384(4) . ? C11 C16 1.397(3) . ? C12 C13 1.386(4) . ? C13 C14 1.385(4) . ? C14 C15 1.369(4) . ? C15 C16 1.388(4) . ? C17 C22 1.397(4) . ? C17 C18 1.402(3) . ? C18 C19 1.380(4) . ? C19 C20 1.372(4) . ? C20 C21 1.380(4) . ? C21 C22 1.376(4) . ? C31 C35 1.406(4) . ? C31 C32 1.414(4) . ? C32 C33 1.402(5) . ? C33 C34 1.410(4) . ? C34 C35 1.403(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe C4 40.34(11) . . ? C3 Fe C1 69.13(10) . . ? C4 Fe C1 68.29(11) . . ? C3 Fe C32 163.32(14) . . ? C4 Fe C32 155.16(14) . . ? C1 Fe C32 107.68(11) . . ? C3 Fe C33 155.24(14) . . ? C4 Fe C33 119.97(14) . . ? C1 Fe C33 123.38(12) . . ? C32 Fe C33 40.27(14) . . ? C3 Fe C2 41.22(11) . . ? C4 Fe C2 68.33(12) . . ? C1 Fe C2 41.12(10) . . ? C32 Fe C2 125.76(13) . . ? C33 Fe C2 161.35(12) . . ? C3 Fe C34 121.06(12) . . ? C4 Fe C34 107.30(12) . . ? C1 Fe C34 159.90(11) . . ? C32 Fe C34 67.59(12) . . ? C33 Fe C34 40.41(12) . . ? C2 Fe C34 157.37(11) . . ? C3 Fe C31 126.40(13) . . ? C4 Fe C31 162.17(12) . . ? C1 Fe C31 122.63(11) . . ? C32 Fe C31 40.51(12) . . ? C33 Fe C31 67.88(13) . . ? C2 Fe C31 109.57(12) . . ? C34 Fe C31 67.40(12) . . ? C3 Fe C5 68.76(11) . . ? C4 Fe C5 40.61(10) . . ? C1 Fe C5 40.76(10) . . ? C32 Fe C5 120.23(12) . . ? C33 Fe C5 105.76(12) . . ? C2 Fe C5 68.88(11) . . ? C34 Fe C5 123.19(12) . . ? C31 Fe C5 156.69(12) . . ? C3 Fe C35 108.75(11) . . ? C4 Fe C35 124.97(11) . . ? C1 Fe C35 158.27(12) . . ? C32 Fe C35 67.78(12) . . ? C33 Fe C35 67.86(13) . . ? C2 Fe C35 122.99(11) . . ? C34 Fe C35 40.06(12) . . ? C31 Fe C35 40.13(11) . . ? C5 Fe C35 160.30(12) . . ? O1 Si1 C17 111.57(10) . . ? O1 Si1 C11 108.25(10) . . ? C17 Si1 C11 109.08(10) . . ? O1 Si1 C7 102.34(10) . . ? C17 Si1 C7 112.24(11) . . ? C11 Si1 C7 113.17(12) . . ? C1 O1 Si1 134.10(14) . . ? O1 C1 C5 129.3(2) . . ? O1 C1 C2 122.4(2) . . ? C5 C1 C2 108.3(2) . . ? O1 C1 Fe 126.27(15) . . ? C5 C1 Fe 70.17(15) . . ? C2 C1 Fe 69.70(15) . . ? C3 C2 C1 107.1(2) . . ? C3 C2 C6 128.6(2) . . ? C1 C2 C6 124.1(2) . . ? C3 C2 Fe 68.74(16) . . ? C1 C2 Fe 69.18(15) . . ? C6 C2 Fe 123.10(17) . . ? C4 C3 C2 107.8(2) . . ? C4 C3 Fe 69.98(15) . . ? C2 C3 Fe 70.04(14) . . ? C3 C4 C5 109.8(3) . . ? C3 C4 Fe 69.68(14) . . ? C5 C4 Fe 70.50(14) . . ? C4 C5 C1 107.0(2) . . ? C4 C5 Fe 68.89(14) . . ? C1 C5 Fe 69.07(13) . . ? O2 C6 C2 125.5(3) . . ? C8 C7 C9 109.9(2) . . ? C8 C7 C10 108.3(2) . . ? C9 C7 C10 107.7(2) . . ? C8 C7 Si1 109.74(17) . . ? C9 C7 Si1 111.88(17) . . ? C10 C7 Si1 109.18(18) . . ? C12 C11 C16 117.4(2) . . ? C12 C11 Si1 121.75(18) . . ? C16 C11 Si1 120.8(2) . . ? C11 C12 C13 122.0(2) . . ? C14 C13 C12 119.5(3) . . ? C15 C14 C13 119.5(3) . . ? C14 C15 C16 120.9(2) . . ? C15 C16 C11 120.7(3) . . ? C22 C17 C18 116.3(2) . . ? C22 C17 Si1 122.61(17) . . ? C18 C17 Si1 121.0(2) . . ? C19 C18 C17 121.6(3) . . ? C20 C19 C18 120.3(2) . . ? C19 C20 C21 119.7(3) . . ? C22 C21 C20 119.9(3) . . ? C21 C22 C17 122.1(2) . . ? C35 C31 C32 107.8(3) . . ? C35 C31 Fe 70.03(14) . . ? C32 C31 Fe 69.27(15) . . ? C33 C32 C31 108.2(3) . . ? C33 C32 Fe 69.91(16) . . ? C31 C32 Fe 70.22(15) . . ? C32 C33 C34 107.6(3) . . ? C32 C33 Fe 69.82(18) . . ? C34 C33 Fe 70.07(17) . . ? C35 C34 C33 108.5(3) . . ? C35 C34 Fe 70.22(17) . . ? C33 C34 Fe 69.52(18) . . ? C34 C35 C31 107.9(3) . . ? C34 C35 Fe 69.72(16) . . ? C31 C35 Fe 69.85(15) . . ? 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 C17 Si1 O1 C1 -47.8(2) . . . . ? C11 Si1 O1 C1 72.3(2) . . . . ? C7 Si1 O1 C1 -168.0(2) . . . . ? Si1 O1 C1 C5 31.6(4) . . . . ? Si1 O1 C1 C2 -147.69(19) . . . . ? Si1 O1 C1 Fe 124.86(18) . . . . ? C3 Fe C1 O1 153.9(2) . . . . ? C4 Fe C1 O1 -162.7(2) . . . . ? C32 Fe C1 O1 -8.7(3) . . . . ? C33 Fe C1 O1 -50.2(3) . . . . ? C2 Fe C1 O1 115.9(3) . . . . ? C34 Fe C1 O1 -81.7(4) . . . . ? C31 Fe C1 O1 33.3(3) . . . . ? C5 Fe C1 O1 -124.8(3) . . . . ? C35 Fe C1 O1 65.5(4) . . . . ? C3 Fe C1 C5 -81.28(16) . . . . ? C4 Fe C1 C5 -37.86(16) . . . . ? C32 Fe C1 C5 116.08(18) . . . . ? C33 Fe C1 C5 74.58(19) . . . . ? C2 Fe C1 C5 -119.3(2) . . . . ? C34 Fe C1 C5 43.1(3) . . . . ? C31 Fe C1 C5 158.05(16) . . . . ? C35 Fe C1 C5 -169.7(3) . . . . ? C3 Fe C1 C2 38.05(14) . . . . ? C4 Fe C1 C2 81.48(16) . . . . ? C32 Fe C1 C2 -124.59(17) . . . . ? C33 Fe C1 C2 -166.09(16) . . . . ? C34 Fe C1 C2 162.5(3) . . . . ? C31 Fe C1 C2 -82.61(18) . . . . ? C5 Fe C1 C2 119.3(2) . . . . ? C35 Fe C1 C2 -50.4(3) . . . . ? O1 C1 C2 C3 -179.3(2) . . . . ? C5 C1 C2 C3 1.3(3) . . . . ? Fe C1 C2 C3 -58.47(17) . . . . ? O1 C1 C2 C6 -4.2(4) . . . . ? C5 C1 C2 C6 176.4(2) . . . . ? Fe C1 C2 C6 116.6(2) . . . . ? O1 C1 C2 Fe -120.8(2) . . . . ? C5 C1 C2 Fe 59.76(17) . . . . ? C4 Fe C2 C3 37.70(15) . . . . ? C1 Fe C2 C3 119.1(2) . . . . ? C32 Fe C2 C3 -165.77(17) . . . . ? C33 Fe C2 C3 158.0(3) . . . . ? C34 Fe C2 C3 -45.3(3) . . . . ? C31 Fe C2 C3 -123.37(17) . . . . ? C5 Fe C2 C3 81.46(16) . . . . ? C35 Fe C2 C3 -80.82(17) . . . . ? C3 Fe C2 C1 -119.1(2) . . . . ? C4 Fe C2 C1 -81.36(15) . . . . ? C32 Fe C2 C1 75.17(18) . . . . ? C33 Fe C2 C1 38.9(4) . . . . ? C34 Fe C2 C1 -164.4(2) . . . . ? C31 Fe C2 C1 117.57(15) . . . . ? C5 Fe C2 C1 -37.60(14) . . . . ? C35 Fe C2 C1 160.12(14) . . . . ? C3 Fe C2 C6 123.0(3) . . . . ? C4 Fe C2 C6 160.7(3) . . . . ? C1 Fe C2 C6 -117.9(3) . . . . ? C32 Fe C2 C6 -42.8(3) . . . . ? C33 Fe C2 C6 -79.0(4) . . . . ? C34 Fe C2 C6 77.7(4) . . . . ? C31 Fe C2 C6 -0.4(3) . . . . ? C5 Fe C2 C6 -155.5(2) . . . . ? C35 Fe C2 C6 42.2(3) . . . . ? C1 C2 C3 C4 -1.3(3) . . . . ? C6 C2 C3 C4 -176.1(2) . . . . ? Fe C2 C3 C4 -60.05(18) . . . . ? C1 C2 C3 Fe 58.75(16) . . . . ? C6 C2 C3 Fe -116.1(3) . . . . ? C1 Fe C3 C4 80.64(18) . . . . ? C32 Fe C3 C4 162.6(4) . . . . ? C33 Fe C3 C4 -44.7(3) . . . . ? C2 Fe C3 C4 118.6(2) . . . . ? C34 Fe C3 C4 -80.0(2) . . . . ? C31 Fe C3 C4 -163.53(17) . . . . ? C5 Fe C3 C4 36.81(17) . . . . ? C35 Fe C3 C4 -122.37(18) . . . . ? C4 Fe C3 C2 -118.6(2) . . . . ? C1 Fe C3 C2 -37.96(14) . . . . ? C32 Fe C3 C2 44.0(4) . . . . ? C33 Fe C3 C2 -163.3(3) . . . . ? C34 Fe C3 C2 161.37(15) . . . . ? C31 Fe C3 C2 77.87(19) . . . . ? C5 Fe C3 C2 -81.79(16) . . . . ? C35 Fe C3 C2 119.03(16) . . . . ? C2 C3 C4 C5 0.8(3) . . . . ? Fe C3 C4 C5 -59.25(19) . . . . ? C2 C3 C4 Fe 60.09(17) . . . . ? C1 Fe C4 C3 -82.91(18) . . . . ? C32 Fe C4 C3 -168.2(3) . . . . ? C33 Fe C4 C3 160.10(18) . . . . ? C2 Fe C4 C3 -38.50(16) . . . . ? C34 Fe C4 C3 117.92(18) . . . . ? C31 Fe C4 C3 48.2(5) . . . . ? C5 Fe C4 C3 -120.9(3) . . . . ? C35 Fe C4 C3 77.4(2) . . . . ? C3 Fe C4 C5 120.9(3) . . . . ? C1 Fe C4 C5 37.99(17) . . . . ? C32 Fe C4 C5 -47.3(4) . . . . ? C33 Fe C4 C5 -79.0(2) . . . . ? C2 Fe C4 C5 82.40(18) . . . . ? C34 Fe C4 C5 -121.18(18) . . . . ? C31 Fe C4 C5 169.1(4) . . . . ? C35 Fe C4 C5 -161.67(17) . . . . ? C3 C4 C5 C1 0.0(3) . . . . ? Fe C4 C5 C1 -58.79(17) . . . . ? C3 C4 C5 Fe 58.76(18) . . . . ? O1 C1 C5 C4 179.9(2) . . . . ? C2 C1 C5 C4 -0.8(3) . . . . ? Fe C1 C5 C4 58.68(18) . . . . ? O1 C1 C5 Fe 121.2(2) . . . . ? C2 C1 C5 Fe -59.47(17) . . . . ? C3 Fe C5 C4 -36.57(18) . . . . ? C1 Fe C5 C4 -118.8(2) . . . . ? C32 Fe C5 C4 159.1(2) . . . . ? C33 Fe C5 C4 117.9(2) . . . . ? C2 Fe C5 C4 -80.93(19) . . . . ? C34 Fe C5 C4 77.5(2) . . . . ? C31 Fe C5 C4 -171.6(3) . . . . ? C35 Fe C5 C4 49.8(4) . . . . ? C3 Fe C5 C1 82.27(17) . . . . ? C4 Fe C5 C1 118.8(2) . . . . ? C32 Fe C5 C1 -82.09(19) . . . . ? C33 Fe C5 C1 -123.23(17) . . . . ? C2 Fe C5 C1 37.92(14) . . . . ? C34 Fe C5 C1 -163.69(15) . . . . ? C31 Fe C5 C1 -52.7(4) . . . . ? C35 Fe C5 C1 168.7(3) . . . . ? C3 C2 C6 O2 -10.6(4) . . . . ? C1 C2 C6 O2 175.4(3) . . . . ? Fe C2 C6 O2 -98.7(3) . . . . ? O1 Si1 C7 C8 -71.4(2) . . . . ? C17 Si1 C7 C8 168.87(19) . . . . ? C11 Si1 C7 C8 44.9(2) . . . . ? O1 Si1 C7 C9 166.33(19) . . . . ? C17 Si1 C7 C9 46.6(2) . . . . ? C11 Si1 C7 C9 -77.4(2) . . . . ? O1 Si1 C7 C10 47.2(2) . . . . ? C17 Si1 C7 C10 -72.5(2) . . . . ? C11 Si1 C7 C10 163.48(17) . . . . ? O1 Si1 C11 C12 154.0(2) . . . . ? C17 Si1 C11 C12 -84.4(2) . . . . ? C7 Si1 C11 C12 41.3(2) . . . . ? O1 Si1 C11 C16 -25.4(2) . . . . ? C17 Si1 C11 C16 96.2(2) . . . . ? C7 Si1 C11 C16 -138.1(2) . . . . ? C16 C11 C12 C13 0.8(4) . . . . ? Si1 C11 C12 C13 -178.7(2) . . . . ? C11 C12 C13 C14 -1.4(4) . . . . ? C12 C13 C14 C15 0.7(4) . . . . ? C13 C14 C15 C16 0.5(4) . . . . ? C14 C15 C16 C11 -1.1(4) . . . . ? C12 C11 C16 C15 0.5(4) . . . . ? Si1 C11 C16 C15 179.9(2) . . . . ? O1 Si1 C17 C22 -52.8(2) . . . . ? C11 Si1 C17 C22 -172.3(2) . . . . ? C7 Si1 C17 C22 61.4(2) . . . . ? O1 Si1 C17 C18 130.81(19) . . . . ? C11 Si1 C17 C18 11.3(2) . . . . ? C7 Si1 C17 C18 -115.0(2) . . . . ? C22 C17 C18 C19 -1.6(4) . . . . ? Si1 C17 C18 C19 175.06(19) . . . . ? C17 C18 C19 C20 0.3(4) . . . . ? C18 C19 C20 C21 0.8(4) . . . . ? C19 C20 C21 C22 -0.6(4) . . . . ? C20 C21 C22 C17 -0.8(4) . . . . ? C18 C17 C22 C21 1.8(4) . . . . ? Si1 C17 C22 C21 -174.7(2) . . . . ? C3 Fe C31 C35 75.2(2) . . . . ? C4 Fe C31 C35 38.4(5) . . . . ? C1 Fe C31 C35 162.15(17) . . . . ? C32 Fe C31 C35 -119.0(3) . . . . ? C33 Fe C31 C35 -81.4(2) . . . . ? C2 Fe C31 C35 118.36(19) . . . . ? C34 Fe C31 C35 -37.58(18) . . . . ? C5 Fe C31 C35 -159.8(3) . . . . ? C3 Fe C31 C32 -165.74(19) . . . . ? C4 Fe C31 C32 157.4(4) . . . . ? C1 Fe C31 C32 -78.8(2) . . . . ? C33 Fe C31 C32 37.6(2) . . . . ? C2 Fe C31 C32 -122.6(2) . . . . ? C34 Fe C31 C32 81.5(2) . . . . ? C5 Fe C31 C32 -40.7(4) . . . . ? C35 Fe C31 C32 119.0(3) . . . . ? C35 C31 C32 C33 -0.2(3) . . . . ? Fe C31 C32 C33 -59.8(2) . . . . ? C35 C31 C32 Fe 59.66(18) . . . . ? C3 Fe C32 C33 162.7(4) . . . . ? C4 Fe C32 C33 -44.8(4) . . . . ? C1 Fe C32 C33 -121.13(19) . . . . ? C2 Fe C32 C33 -162.98(17) . . . . ? C34 Fe C32 C33 38.05(19) . . . . ? C31 Fe C32 C33 119.0(3) . . . . ? C5 Fe C32 C33 -78.4(2) . . . . ? C35 Fe C32 C33 81.5(2) . . . . ? C3 Fe C32 C31 43.7(5) . . . . ? C4 Fe C32 C31 -163.8(3) . . . . ? C1 Fe C32 C31 119.87(19) . . . . ? C33 Fe C32 C31 -119.0(3) . . . . ? C2 Fe C32 C31 78.0(2) . . . . ? C34 Fe C32 C31 -81.0(2) . . . . ? C5 Fe C32 C31 162.62(18) . . . . ? C35 Fe C32 C31 -37.49(19) . . . . ? C31 C32 C33 C34 -0.1(3) . . . . ? Fe C32 C33 C34 -60.1(2) . . . . ? C31 C32 C33 Fe 60.03(19) . . . . ? C3 Fe C33 C32 -168.2(2) . . . . ? C4 Fe C33 C32 160.03(18) . . . . ? C1 Fe C33 C32 77.6(2) . . . . ? C2 Fe C33 C32 48.0(4) . . . . ? C34 Fe C33 C32 -118.5(3) . . . . ? C31 Fe C33 C32 -37.82(18) . . . . ? C5 Fe C33 C32 118.43(19) . . . . ? C35 Fe C33 C32 -81.3(2) . . . . ? C3 Fe C33 C34 -49.8(4) . . . . ? C4 Fe C33 C34 -81.5(2) . . . . ? C1 Fe C33 C34 -163.93(16) . . . . ? C32 Fe C33 C34 118.5(3) . . . . ? C2 Fe C33 C34 166.4(3) . . . . ? C31 Fe C33 C34 80.65(19) . . . . ? C5 Fe C33 C34 -123.09(18) . . . . ? C35 Fe C33 C34 37.18(17) . . . . ? C32 C33 C34 C35 0.3(3) . . . . ? Fe C33 C34 C35 -59.6(2) . . . . ? C32 C33 C34 Fe 60.0(2) . . . . ? C3 Fe C34 C35 -82.34(19) . . . . ? C4 Fe C34 C35 -124.23(17) . . . . ? C1 Fe C34 C35 161.8(3) . . . . ? C32 Fe C34 C35 81.65(19) . . . . ? C33 Fe C34 C35 119.6(3) . . . . ? C2 Fe C34 C35 -49.2(3) . . . . ? C31 Fe C34 C35 37.64(17) . . . . ? C5 Fe C34 C35 -165.95(15) . . . . ? C3 Fe C34 C33 158.08(19) . . . . ? C4 Fe C34 C33 116.2(2) . . . . ? C1 Fe C34 C33 42.2(4) . . . . ? C32 Fe C34 C33 -37.92(19) . . . . ? C2 Fe C34 C33 -168.8(2) . . . . ? C31 Fe C34 C33 -81.9(2) . . . . ? C5 Fe C34 C33 74.5(2) . . . . ? C35 Fe C34 C33 -119.6(3) . . . . ? C33 C34 C35 C31 -0.4(3) . . . . ? Fe C34 C35 C31 -59.65(19) . . . . ? C33 C34 C35 Fe 59.2(2) . . . . ? C32 C31 C35 C34 0.4(3) . . . . ? Fe C31 C35 C34 59.57(18) . . . . ? C32 C31 C35 Fe -59.19(18) . . . . ? C3 Fe C35 C34 116.29(18) . . . . ? C4 Fe C35 C34 74.4(2) . . . . ? C1 Fe C35 C34 -163.2(2) . . . . ? C32 Fe C35 C34 -81.1(2) . . . . ? C33 Fe C35 C34 -37.49(17) . . . . ? C2 Fe C35 C34 159.68(16) . . . . ? C31 Fe C35 C34 -119.0(3) . . . . ? C5 Fe C35 C34 37.1(4) . . . . ? C3 Fe C35 C31 -124.73(19) . . . . ? C4 Fe C35 C31 -166.58(19) . . . . ? C1 Fe C35 C31 -44.2(4) . . . . ? C32 Fe C35 C31 37.8(2) . . . . ? C33 Fe C35 C31 81.5(2) . . . . ? C2 Fe C35 C31 -81.3(2) . . . . ? C34 Fe C35 C31 119.0(3) . . . . ? C5 Fe C35 C31 156.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.417 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.061 # Attachment 'rac9.cif' data_erk3375 _database_code_depnum_ccdc_archive 'CCDC 714372' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H15 Fe I O2' _chemical_formula_weight 398.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.938(1) _cell_length_b 9.716(1) _cell_length_c 17.680(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1363.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 12373 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 3.360 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3467 _exptl_absorpt_correction_T_max 0.5530 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9338 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3270 _reflns_number_gt 3182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0148P)^2^+1.5797P] 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 riding _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 -0.03(2) _refine_ls_number_reflns 3270 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0485 _refine_ls_wR_factor_gt 0.0479 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.68479(5) 0.55581(4) 0.312344(19) 0.02074(8) Uani 1 1 d . . . I1 I 0.68255(3) 0.617875(19) 0.517416(10) 0.03402(6) Uani 1 1 d . . . O1 O 0.5444(3) 0.2277(2) 0.46408(13) 0.0364(5) Uani 1 1 d . . . O2 O 0.7195(3) 0.2134(2) 0.35914(11) 0.0308(5) Uani 1 1 d . . . C1 C 0.5777(3) 0.4201(3) 0.38513(14) 0.0216(5) Uani 1 1 d . . . C2 C 0.5771(3) 0.5569(3) 0.41513(14) 0.0216(5) Uani 1 1 d . . . C3 C 0.4843(3) 0.6442(3) 0.36579(15) 0.0275(6) Uani 1 1 d . . . H3A H 0.4647 0.7451 0.3727 0.033 Uiso 1 1 calc R . . C4 C 0.4277(4) 0.5630(3) 0.30453(17) 0.0323(6) Uani 1 1 d . . . H4A H 0.3619 0.5970 0.2600 0.039 Uiso 1 1 calc R . . C5 C 0.4833(3) 0.4253(3) 0.31603(17) 0.0282(6) Uani 1 1 d . . . H5A H 0.4630 0.3461 0.2811 0.034 Uiso 1 1 calc R . . C6 C 0.6619(4) 0.2970(3) 0.41804(14) 0.0226(5) Uani 1 1 d . . . H6A H 0.7598 0.3272 0.4496 0.027 Uiso 1 1 calc R . . C7 C 0.6240(4) 0.1113(4) 0.4995(2) 0.0477(9) Uani 1 1 d . . . H7A H 0.5406 0.0610 0.5306 0.057 Uiso 1 1 calc R . . H7B H 0.7153 0.1435 0.5333 0.057 Uiso 1 1 calc R . . C8 C 0.6955(5) 0.0166(3) 0.4408(2) 0.0483(9) Uani 1 1 d . . . H8A H 0.6029 -0.0261 0.4115 0.058 Uiso 1 1 calc R . . H8B H 0.7604 -0.0578 0.4656 0.058 Uiso 1 1 calc R . . C9 C 0.8084(4) 0.0963(3) 0.38860(19) 0.0366(6) Uani 1 1 d . . . H9A H 0.9097 0.1274 0.4164 0.044 Uiso 1 1 calc R . . H9B H 0.8454 0.0365 0.3464 0.044 Uiso 1 1 calc R . . C21 C 0.7798(4) 0.6153(4) 0.20979(17) 0.0396(7) Uani 1 1 d . . . H21A H 0.7128 0.6409 0.1640 0.047 Uiso 1 1 calc R . . C22 C 0.8363(5) 0.4798(4) 0.22949(17) 0.0389(7) Uani 1 1 d . . . H22A H 0.8169 0.3938 0.1997 0.047 Uiso 1 1 calc R . . C23 C 0.9268(4) 0.4905(4) 0.29833(17) 0.0351(7) Uani 1 1 d . . . H23A H 0.9808 0.4123 0.3260 0.042 Uiso 1 1 calc R . . C24 C 0.9268(4) 0.6294(4) 0.32206(19) 0.0376(7) Uani 1 1 d . . . H24A H 0.9804 0.6668 0.3689 0.045 Uiso 1 1 calc R . . C25 C 0.8350(4) 0.7059(3) 0.26707(19) 0.0392(7) Uani 1 1 d . . . H25A H 0.8123 0.8071 0.2690 0.047 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 Fe 0.02619(17) 0.01936(16) 0.01666(15) 0.00007(13) 0.00233(16) 0.00085(18) I1 0.05191(11) 0.02941(9) 0.02075(8) -0.00600(7) -0.00252(9) -0.00085(10) O1 0.0336(11) 0.0312(11) 0.0445(12) 0.0164(9) 0.0114(10) 0.0016(9) O2 0.0435(13) 0.0234(9) 0.0254(10) -0.0041(8) -0.0001(8) 0.0078(9) C1 0.0246(12) 0.0192(12) 0.0209(11) -0.0006(9) 0.0022(9) -0.0028(10) C2 0.0261(12) 0.0215(13) 0.0171(11) -0.0026(9) 0.0024(9) -0.0020(11) C3 0.0299(13) 0.0259(14) 0.0266(13) 0.0022(11) 0.0059(10) 0.0055(11) C4 0.0307(14) 0.0346(15) 0.0318(14) 0.0022(13) -0.0060(12) 0.0021(13) C5 0.0282(13) 0.0274(14) 0.0292(13) -0.0040(11) -0.0065(11) -0.0047(11) C6 0.0288(13) 0.0181(11) 0.0210(11) 0.0001(9) 0.0019(10) -0.0019(11) C7 0.0474(17) 0.0398(18) 0.056(2) 0.0282(17) 0.0156(15) 0.0062(15) C8 0.0406(17) 0.0216(14) 0.083(3) 0.0129(15) -0.002(2) -0.0012(15) C9 0.0425(16) 0.0241(13) 0.0432(16) -0.0021(12) -0.0023(15) 0.0092(14) C21 0.0476(19) 0.0454(18) 0.0257(14) 0.0117(14) 0.0112(12) 0.0074(16) C22 0.051(2) 0.0406(17) 0.0255(14) 0.0023(12) 0.0175(14) 0.0109(16) C23 0.0301(15) 0.0434(18) 0.0318(16) 0.0089(14) 0.0115(12) 0.0092(14) C24 0.0255(13) 0.0465(19) 0.0407(16) 0.0021(16) 0.0041(12) -0.0083(15) C25 0.0382(16) 0.0309(14) 0.0485(18) 0.0115(13) 0.0155(15) -0.0046(14) _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 Fe C2 2.008(2) . ? Fe C1 2.029(3) . ? Fe C22 2.034(3) . ? Fe C23 2.038(3) . ? Fe C3 2.040(3) . ? Fe C5 2.042(3) . ? Fe C4 2.047(3) . ? Fe C25 2.047(3) . ? Fe C21 2.047(3) . ? Fe C24 2.057(3) . ? I1 C2 2.079(3) . ? O1 C6 1.410(3) . ? O1 C7 1.439(4) . ? O2 C6 1.398(3) . ? O2 C9 1.436(3) . ? C1 C2 1.431(4) . ? C1 C5 1.434(4) . ? C1 C6 1.488(4) . ? C2 C3 1.422(4) . ? C3 C4 1.413(4) . ? C4 C5 1.424(4) . ? C7 C8 1.499(5) . ? C8 C9 1.501(5) . ? C21 C25 1.412(5) . ? C21 C22 1.434(5) . ? C22 C23 1.417(5) . ? C23 C24 1.413(5) . ? C24 C25 1.424(5) . ? 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 Fe C1 41.52(10) . . ? C2 Fe C22 154.86(12) . . ? C1 Fe C22 117.94(12) . . ? C2 Fe C23 120.85(12) . . ? C1 Fe C23 105.65(12) . . ? C22 Fe C23 40.73(14) . . ? C2 Fe C3 41.12(11) . . ? C1 Fe C3 69.70(11) . . ? C22 Fe C3 161.35(13) . . ? C23 Fe C3 157.28(13) . . ? C2 Fe C5 68.98(11) . . ? C1 Fe C5 41.25(11) . . ? C22 Fe C5 105.10(14) . . ? C23 Fe C5 123.28(14) . . ? C3 Fe C5 68.65(12) . . ? C2 Fe C4 68.69(12) . . ? C1 Fe C4 69.35(12) . . ? C22 Fe C4 123.60(14) . . ? C23 Fe C4 160.44(15) . . ? C3 Fe C4 40.46(12) . . ? C5 Fe C4 40.76(12) . . ? C2 Fe C25 126.72(13) . . ? C1 Fe C25 162.75(13) . . ? C22 Fe C25 68.45(14) . . ? C23 Fe C25 67.98(14) . . ? C3 Fe C25 109.61(13) . . ? C5 Fe C25 155.68(14) . . ? C4 Fe C25 122.02(14) . . ? C2 Fe C21 163.09(14) . . ? C1 Fe C21 154.11(13) . . ? C22 Fe C21 41.14(13) . . ? C23 Fe C21 68.46(13) . . ? C3 Fe C21 125.36(12) . . ? C5 Fe C21 119.49(13) . . ? C4 Fe C21 107.34(13) . . ? C25 Fe C21 40.34(14) . . ? C2 Fe C24 108.66(12) . . ? C1 Fe C24 124.34(12) . . ? C22 Fe C24 68.54(15) . . ? C23 Fe C24 40.36(15) . . ? C3 Fe C24 122.92(14) . . ? C5 Fe C24 160.83(14) . . ? C4 Fe C24 157.67(15) . . ? C25 Fe C24 40.61(14) . . ? C21 Fe C24 68.38(14) . . ? C6 O1 C7 109.6(2) . . ? C6 O2 C9 110.5(2) . . ? C2 C1 C5 106.4(2) . . ? C2 C1 C6 127.1(2) . . ? C5 C1 C6 126.6(2) . . ? C2 C1 Fe 68.47(14) . . ? C5 C1 Fe 69.86(16) . . ? C6 C1 Fe 125.58(18) . . ? C3 C2 C1 109.2(2) . . ? C3 C2 Fe 70.65(15) . . ? C1 C2 Fe 70.01(14) . . ? C3 C2 I1 124.9(2) . . ? C1 C2 I1 125.85(19) . . ? Fe C2 I1 128.13(13) . . ? C4 C3 C2 107.6(2) . . ? C4 C3 Fe 70.02(16) . . ? C2 C3 Fe 68.23(15) . . ? C3 C4 C5 108.4(3) . . ? C3 C4 Fe 69.51(16) . . ? C5 C4 Fe 69.43(17) . . ? C4 C5 C1 108.5(2) . . ? C4 C5 Fe 69.81(17) . . ? C1 C5 Fe 68.89(14) . . ? O2 C6 O1 111.6(2) . . ? O2 C6 C1 108.8(2) . . ? O1 C6 C1 108.2(2) . . ? O1 C7 C8 110.4(3) . . ? C7 C8 C9 109.5(3) . . ? O2 C9 C8 109.8(3) . . ? C25 C21 C22 107.5(3) . . ? C25 C21 Fe 69.83(17) . . ? C22 C21 Fe 68.94(17) . . ? C23 C22 C21 107.4(3) . . ? C23 C22 Fe 69.80(17) . . ? C21 C22 Fe 69.92(17) . . ? C24 C23 C22 109.0(3) . . ? C24 C23 Fe 70.52(18) . . ? C22 C23 Fe 69.47(18) . . ? C23 C24 C25 107.2(3) . . ? C23 C24 Fe 69.12(19) . . ? C25 C24 Fe 69.33(17) . . ? C21 C25 C24 108.8(3) . . ? C21 C25 Fe 69.83(18) . . ? C24 C25 Fe 70.06(17) . . ? 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 C22 Fe C1 C2 161.22(18) . . . . ? C23 Fe C1 C2 119.14(17) . . . . ? C3 Fe C1 C2 -37.46(16) . . . . ? C5 Fe C1 C2 -117.8(2) . . . . ? C4 Fe C1 C2 -80.78(17) . . . . ? C25 Fe C1 C2 53.4(5) . . . . ? C21 Fe C1 C2 -168.1(2) . . . . ? C24 Fe C1 C2 79.2(2) . . . . ? C2 Fe C1 C5 117.8(2) . . . . ? C22 Fe C1 C5 -80.9(2) . . . . ? C23 Fe C1 C5 -123.01(18) . . . . ? C3 Fe C1 C5 80.39(18) . . . . ? C4 Fe C1 C5 37.07(17) . . . . ? C25 Fe C1 C5 171.3(4) . . . . ? C21 Fe C1 C5 -50.2(3) . . . . ? C24 Fe C1 C5 -162.93(19) . . . . ? C2 Fe C1 C6 -121.0(3) . . . . ? C22 Fe C1 C6 40.3(3) . . . . ? C23 Fe C1 C6 -1.8(3) . . . . ? C3 Fe C1 C6 -158.4(2) . . . . ? C5 Fe C1 C6 121.2(3) . . . . ? C4 Fe C1 C6 158.3(3) . . . . ? C25 Fe C1 C6 -67.5(5) . . . . ? C21 Fe C1 C6 71.0(4) . . . . ? C24 Fe C1 C6 -41.7(3) . . . . ? C5 C1 C2 C3 0.1(3) . . . . ? C6 C1 C2 C3 179.1(2) . . . . ? Fe C1 C2 C3 60.02(19) . . . . ? C5 C1 C2 Fe -59.90(19) . . . . ? C6 C1 C2 Fe 119.1(3) . . . . ? C5 C1 C2 I1 176.88(19) . . . . ? C6 C1 C2 I1 -4.1(4) . . . . ? Fe C1 C2 I1 -123.2(2) . . . . ? C1 Fe C2 C3 -119.9(2) . . . . ? C22 Fe C2 C3 -161.9(3) . . . . ? C23 Fe C2 C3 161.71(18) . . . . ? C5 Fe C2 C3 -81.21(18) . . . . ? C4 Fe C2 C3 -37.35(17) . . . . ? C25 Fe C2 C3 77.4(2) . . . . ? C21 Fe C2 C3 42.1(5) . . . . ? C24 Fe C2 C3 119.03(19) . . . . ? C22 Fe C2 C1 -42.0(4) . . . . ? C23 Fe C2 C1 -78.4(2) . . . . ? C3 Fe C2 C1 119.9(2) . . . . ? C5 Fe C2 C1 38.65(16) . . . . ? C4 Fe C2 C1 82.50(17) . . . . ? C25 Fe C2 C1 -162.72(17) . . . . ? C21 Fe C2 C1 161.9(4) . . . . ? C24 Fe C2 C1 -121.11(18) . . . . ? C1 Fe C2 I1 120.4(2) . . . . ? C22 Fe C2 I1 78.4(4) . . . . ? C23 Fe C2 I1 42.0(2) . . . . ? C3 Fe C2 I1 -119.7(2) . . . . ? C5 Fe C2 I1 159.1(2) . . . . ? C4 Fe C2 I1 -157.0(2) . . . . ? C25 Fe C2 I1 -42.3(2) . . . . ? C21 Fe C2 I1 -77.6(5) . . . . ? C24 Fe C2 I1 -0.7(2) . . . . ? C1 C2 C3 C4 -0.5(3) . . . . ? Fe C2 C3 C4 59.2(2) . . . . ? I1 C2 C3 C4 -177.26(19) . . . . ? C1 C2 C3 Fe -59.63(18) . . . . ? I1 C2 C3 Fe 123.6(2) . . . . ? C2 Fe C3 C4 -119.4(2) . . . . ? C1 Fe C3 C4 -81.62(18) . . . . ? C22 Fe C3 C4 36.2(5) . . . . ? C23 Fe C3 C4 -163.6(3) . . . . ? C5 Fe C3 C4 -37.36(18) . . . . ? C25 Fe C3 C4 116.7(2) . . . . ? C21 Fe C3 C4 74.4(2) . . . . ? C24 Fe C3 C4 159.89(19) . . . . ? C1 Fe C3 C2 37.81(16) . . . . ? C22 Fe C3 C2 155.6(4) . . . . ? C23 Fe C3 C2 -44.2(4) . . . . ? C5 Fe C3 C2 82.07(17) . . . . ? C4 Fe C3 C2 119.4(2) . . . . ? C25 Fe C3 C2 -123.85(18) . . . . ? C21 Fe C3 C2 -166.17(18) . . . . ? C24 Fe C3 C2 -80.7(2) . . . . ? C2 C3 C4 C5 0.6(3) . . . . ? Fe C3 C4 C5 58.7(2) . . . . ? C2 C3 C4 Fe -58.05(19) . . . . ? C2 Fe C4 C3 37.94(16) . . . . ? C1 Fe C4 C3 82.56(17) . . . . ? C22 Fe C4 C3 -166.90(17) . . . . ? C23 Fe C4 C3 161.0(3) . . . . ? C5 Fe C4 C3 120.1(2) . . . . ? C25 Fe C4 C3 -82.9(2) . . . . ? C21 Fe C4 C3 -124.62(19) . . . . ? C24 Fe C4 C3 -49.4(4) . . . . ? C2 Fe C4 C5 -82.11(19) . . . . ? C1 Fe C4 C5 -37.49(17) . . . . ? C22 Fe C4 C5 73.0(2) . . . . ? C23 Fe C4 C5 41.0(4) . . . . ? C3 Fe C4 C5 -120.1(2) . . . . ? C25 Fe C4 C5 157.03(18) . . . . ? C21 Fe C4 C5 115.3(2) . . . . ? C24 Fe C4 C5 -169.5(3) . . . . ? C3 C4 C5 C1 -0.6(3) . . . . ? Fe C4 C5 C1 58.17(19) . . . . ? C3 C4 C5 Fe -58.7(2) . . . . ? C2 C1 C5 C4 0.3(3) . . . . ? C6 C1 C5 C4 -178.7(3) . . . . ? Fe C1 C5 C4 -58.7(2) . . . . ? C2 C1 C5 Fe 59.00(18) . . . . ? C6 C1 C5 Fe -120.0(3) . . . . ? C2 Fe C5 C4 81.35(19) . . . . ? C1 Fe C5 C4 120.2(2) . . . . ? C22 Fe C5 C4 -124.39(19) . . . . ? C23 Fe C5 C4 -164.77(18) . . . . ? C3 Fe C5 C4 37.09(17) . . . . ? C25 Fe C5 C4 -53.5(4) . . . . ? C21 Fe C5 C4 -82.4(2) . . . . ? C24 Fe C5 C4 167.8(4) . . . . ? C2 Fe C5 C1 -38.90(16) . . . . ? C22 Fe C5 C1 115.36(17) . . . . ? C23 Fe C5 C1 75.0(2) . . . . ? C3 Fe C5 C1 -83.15(17) . . . . ? C4 Fe C5 C1 -120.2(2) . . . . ? C25 Fe C5 C1 -173.7(3) . . . . ? C21 Fe C5 C1 157.32(17) . . . . ? C24 Fe C5 C1 47.6(4) . . . . ? C9 O2 C6 O1 -63.2(3) . . . . ? C9 O2 C6 C1 177.4(2) . . . . ? C7 O1 C6 O2 62.8(3) . . . . ? C7 O1 C6 C1 -177.5(3) . . . . ? C2 C1 C6 O2 -145.5(3) . . . . ? C5 C1 C6 O2 33.2(4) . . . . ? Fe C1 C6 O2 -57.0(3) . . . . ? C2 C1 C6 O1 93.0(3) . . . . ? C5 C1 C6 O1 -88.3(3) . . . . ? Fe C1 C6 O1 -178.47(18) . . . . ? C6 O1 C7 C8 -57.6(4) . . . . ? O1 C7 C8 C9 53.4(4) . . . . ? C6 O2 C9 C8 57.6(3) . . . . ? C7 C8 C9 O2 -52.9(4) . . . . ? C2 Fe C21 C25 45.8(5) . . . . ? C1 Fe C21 C25 -162.3(3) . . . . ? C22 Fe C21 C25 -119.0(3) . . . . ? C23 Fe C21 C25 -80.9(2) . . . . ? C3 Fe C21 C25 78.5(2) . . . . ? C5 Fe C21 C25 162.06(19) . . . . ? C4 Fe C21 C25 119.4(2) . . . . ? C24 Fe C21 C25 -37.4(2) . . . . ? C2 Fe C21 C22 164.8(4) . . . . ? C1 Fe C21 C22 -43.3(4) . . . . ? C23 Fe C21 C22 38.1(2) . . . . ? C3 Fe C21 C22 -162.5(2) . . . . ? C5 Fe C21 C22 -78.9(2) . . . . ? C4 Fe C21 C22 -121.6(2) . . . . ? C25 Fe C21 C22 119.0(3) . . . . ? C24 Fe C21 C22 81.7(2) . . . . ? C25 C21 C22 C23 -0.6(4) . . . . ? Fe C21 C22 C23 -60.0(2) . . . . ? C25 C21 C22 Fe 59.4(2) . . . . ? C2 Fe C22 C23 -51.3(4) . . . . ? C1 Fe C22 C23 -81.5(2) . . . . ? C3 Fe C22 C23 168.4(4) . . . . ? C5 Fe C22 C23 -123.9(2) . . . . ? C4 Fe C22 C23 -164.2(2) . . . . ? C25 Fe C22 C23 80.8(2) . . . . ? C21 Fe C22 C23 118.3(3) . . . . ? C24 Fe C22 C23 37.0(2) . . . . ? C2 Fe C22 C21 -169.7(3) . . . . ? C1 Fe C22 C21 160.19(19) . . . . ? C23 Fe C22 C21 -118.3(3) . . . . ? C3 Fe C22 C21 50.1(5) . . . . ? C5 Fe C22 C21 117.8(2) . . . . ? C4 Fe C22 C21 77.5(2) . . . . ? C25 Fe C22 C21 -37.5(2) . . . . ? C24 Fe C22 C21 -81.3(2) . . . . ? C21 C22 C23 C24 0.4(4) . . . . ? Fe C22 C23 C24 -59.7(2) . . . . ? C21 C22 C23 Fe 60.1(2) . . . . ? C2 Fe C23 C24 -82.7(2) . . . . ? C1 Fe C23 C24 -125.10(19) . . . . ? C22 Fe C23 C24 120.0(3) . . . . ? C3 Fe C23 C24 -50.4(4) . . . . ? C5 Fe C23 C24 -166.50(18) . . . . ? C4 Fe C23 C24 162.7(3) . . . . ? C25 Fe C23 C24 37.95(19) . . . . ? C21 Fe C23 C24 81.5(2) . . . . ? C2 Fe C23 C22 157.27(19) . . . . ? C1 Fe C23 C22 114.9(2) . . . . ? C3 Fe C23 C22 -170.4(3) . . . . ? C5 Fe C23 C22 73.5(2) . . . . ? C4 Fe C23 C22 42.6(5) . . . . ? C25 Fe C23 C22 -82.1(2) . . . . ? C21 Fe C23 C22 -38.5(2) . . . . ? C24 Fe C23 C22 -120.0(3) . . . . ? C22 C23 C24 C25 -0.1(4) . . . . ? Fe C23 C24 C25 -59.1(2) . . . . ? C22 C23 C24 Fe 59.0(2) . . . . ? C2 Fe C24 C23 116.00(19) . . . . ? C1 Fe C24 C23 72.6(2) . . . . ? C22 Fe C24 C23 -37.37(19) . . . . ? C3 Fe C24 C23 159.24(17) . . . . ? C5 Fe C24 C23 36.5(5) . . . . ? C4 Fe C24 C23 -164.8(3) . . . . ? C25 Fe C24 C23 -118.9(3) . . . . ? C21 Fe C24 C23 -81.7(2) . . . . ? C2 Fe C24 C25 -125.1(2) . . . . ? C1 Fe C24 C25 -168.56(18) . . . . ? C22 Fe C24 C25 81.5(2) . . . . ? C23 Fe C24 C25 118.9(3) . . . . ? C3 Fe C24 C25 -81.9(2) . . . . ? C5 Fe C24 C25 155.3(4) . . . . ? C4 Fe C24 C25 -45.9(4) . . . . ? C21 Fe C24 C25 37.1(2) . . . . ? C22 C21 C25 C24 0.6(4) . . . . ? Fe C21 C25 C24 59.4(2) . . . . ? C22 C21 C25 Fe -58.8(2) . . . . ? C23 C24 C25 C21 -0.3(3) . . . . ? Fe C24 C25 C21 -59.3(2) . . . . ? C23 C24 C25 Fe 58.9(2) . . . . ? C2 Fe C25 C21 -164.93(18) . . . . ? C1 Fe C25 C21 153.5(4) . . . . ? C22 Fe C25 C21 38.2(2) . . . . ? C23 Fe C25 C21 82.2(2) . . . . ? C3 Fe C25 C21 -122.0(2) . . . . ? C5 Fe C25 C21 -40.6(4) . . . . ? C4 Fe C25 C21 -78.9(2) . . . . ? C24 Fe C25 C21 119.9(3) . . . . ? C2 Fe C25 C24 75.1(2) . . . . ? C1 Fe C25 C24 33.5(5) . . . . ? C22 Fe C25 C24 -81.7(2) . . . . ? C23 Fe C25 C24 -37.7(2) . . . . ? C3 Fe C25 C24 118.1(2) . . . . ? C5 Fe C25 C24 -160.6(3) . . . . ? C4 Fe C25 C24 161.2(2) . . . . ? C21 Fe C25 C24 -119.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.731 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.069