# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #=============================================================================== _audit_creation_date 2011-06-16 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Duncan Carmichael' _publ_contact_author_address ;Laboratoire DCPH Ecole Polytechnique Route de Saclay F91128 Palaiseau France ; _publ_contact_author_email duncan.carmichael@polytechnique.edu _publ_contact_author_phone 330169334415 _publ_contact_author_fax 330169334440 _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in CHEMICAL COMMUNICATION. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Stepwise syntheses of tri- and tetraphosphaporphyrinogensStepwise syntheses of tri- and tetraphosphaporphyrinogens ; _publ_author_address ; a) Laboratoire Heteroelements et Coordination, Ecole Polytechnique, CNRS F-91128 Palaiseau Cedex France ; #=============================================================================== # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ; _publ_section_exptl_prep ;All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990). ; _publ_section_references ;Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7 ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; loop_ _publ_author_name D.Carmichael A.Escalle-Lewis 'X.F.Le Goff' E.Muller #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. #=============================================================================== # compound 9 data_em463 _database_code_depnum_ccdc_archive 'CCDC 830881' #TrackingRef '2011_duncan_chem_commun.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H84 Fe2 O4 P4 Si2' _chemical_formula_sum 'C60 H84 Fe2 O4 P4 Si2' _chemical_formula_weight 1161.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pca21 ' _symmetry_space_group_name_Hall 'P 2c -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 23.209(1) _cell_length_b 25.099(1) _cell_length_c 20.610(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12005.8(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24379 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4928 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8883 _exptl_absorpt_correction_T_max 0.9607 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90852 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 27.46 _reflns_number_total 25709 _reflns_number_gt 16505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'PLATON (Spek, 2009)' _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. Crystal were found to be twinned (twin fraction 0.54/0.46) ; _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^)+(0.0974P)^2^+1.0595P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(4) _refine_ls_number_reflns 25709 _refine_ls_number_parameters 1331 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1470 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 -1.22597(6) -0.50343(2) 0.19028(7) 0.0254(3) Uani 1 1 d . . . Fe2 Fe -1.02209(6) -0.50453(3) -0.05222(7) 0.0299(3) Uani 1 1 d . . . P1 P -1.20569(13) -0.50605(6) 0.08323(13) 0.0323(5) Uani 1 1 d . . . P2 P -1.02882(12) -0.50458(5) 0.06061(13) 0.0278(5) Uani 1 1 d . . . P3 P -1.05985(9) -0.63235(7) 0.11460(10) 0.0305(4) Uani 1 1 d . . . P4 P -1.05606(9) -0.37611(7) 0.11384(10) 0.0309(4) Uani 1 1 d . . . Si1 Si -0.96040(10) -0.71922(8) 0.10802(11) 0.0286(5) Uani 1 1 d . . . Si2 Si -0.96034(11) -0.28428(8) 0.11057(11) 0.0315(5) Uani 1 1 d . . . O1 O -1.2234(2) -0.38850(19) 0.0791(2) 0.0508(13) Uani 1 1 d . . . O2 O -1.2308(2) -0.62468(19) 0.0926(3) 0.0644(17) Uani 1 1 d . . . O3 O -1.0566(3) -0.64474(19) -0.0181(3) 0.0432(13) Uani 1 1 d . . . O4 O -1.0490(3) -0.3635(2) -0.0189(3) 0.0500(14) Uani 1 1 d . . . C1 C -1.1806(4) -0.4002(3) 0.1100(4) 0.047(2) Uani 1 1 d . . . C2 C -1.1723(3) -0.4555(3) 0.1322(4) 0.0288(16) Uani 1 1 d . . . C3 C -1.1415(3) -0.4774(3) 0.1881(4) 0.0348(17) Uani 1 1 d . . . C4 C -1.1421(3) -0.5337(3) 0.1898(4) 0.0318(16) Uani 1 1 d . . . C5 C -1.1746(3) -0.5553(3) 0.1349(4) 0.0325(16) Uani 1 1 d . . . C6 C -1.1851(3) -0.6126(3) 0.1166(4) 0.0394(18) Uani 1 1 d . . . C7 C -1.1364(3) -0.6497(3) 0.1177(4) 0.0308(15) Uani 1 1 d . . . C8 C -1.1413(3) -0.7040(3) 0.1210(4) 0.0321(16) Uani 1 1 d . . . C9 C -1.0869(3) -0.7322(3) 0.1191(4) 0.0318(16) Uani 1 1 d . . . C10 C -1.0387(4) -0.7017(3) 0.1113(4) 0.0317(17) Uani 1 1 d . . . C11 C -1.0584(3) -0.6128(3) 0.0261(4) 0.0330(17) Uani 1 1 d . . . C12 C -1.0655(4) -0.5533(3) 0.0136(4) 0.0332(18) Uani 1 1 d . . . C13 C -1.1040(3) -0.5324(3) -0.0348(3) 0.0323(18) Uani 1 1 d . . . C14 C -1.1028(3) -0.4751(3) -0.0346(4) 0.0313(18) Uani 1 1 d . . . C15 C -1.0640(3) -0.4558(3) 0.0138(4) 0.0302(17) Uani 1 1 d . . . C16 C -1.0546(3) -0.3967(3) 0.0258(4) 0.0363(18) Uani 1 1 d . . . C17 C -1.0383(4) -0.3067(3) 0.1137(4) 0.0345(17) Uani 1 1 d . . . C18 C -1.0860(4) -0.2779(3) 0.1239(4) 0.0311(17) Uani 1 1 d . . . C19 C -1.1402(3) -0.3075(3) 0.1229(4) 0.0356(17) Uani 1 1 d . . . C20 C -1.1323(3) -0.3609(3) 0.1167(4) 0.0356(16) Uani 1 1 d . . . C21 C -1.1112(3) -0.4442(3) 0.2388(4) 0.0370(18) Uani 1 1 d . . . H21A H -1.1153 -0.4608 0.2805 0.055 Uiso 1 1 calc R . . H21B H -1.1279 -0.4092 0.2399 0.055 Uiso 1 1 calc R . . H21C H -1.0710 -0.4415 0.2281 0.055 Uiso 1 1 calc R . . C22 C -1.1140(4) -0.5649(3) 0.2414(4) 0.0413(19) Uani 1 1 d . . . H22A H -1.0743 -0.5706 0.2304 0.062 Uiso 1 1 calc R . . H22B H -1.1330 -0.5987 0.2457 0.062 Uiso 1 1 calc R . . H22C H -1.1164 -0.5459 0.2817 0.062 Uiso 1 1 calc R . . C23 C -1.1964(3) -0.7346(3) 0.1284(5) 0.0457(19) Uani 1 1 d . . . H23A H -1.2273 -0.7104 0.1383 0.069 Uiso 1 1 calc R . . H23B H -1.1925 -0.7600 0.1629 0.069 Uiso 1 1 calc R . . H23C H -1.2049 -0.7529 0.0886 0.069 Uiso 1 1 calc R . . C24 C -1.0876(3) -0.7919(3) 0.1232(5) 0.0453(19) Uani 1 1 d . . . H24A H -1.0488 -0.8051 0.1212 0.068 Uiso 1 1 calc R . . H24B H -1.1094 -0.8061 0.0876 0.068 Uiso 1 1 calc R . . H24C H -1.1049 -0.8026 0.1634 0.068 Uiso 1 1 calc R . . C25 C -1.1459(4) -0.5655(3) -0.0730(4) 0.0365(19) Uani 1 1 d . . . H25A H -1.1290 -0.5996 -0.0823 0.055 Uiso 1 1 calc R . . H25B H -1.1549 -0.5477 -0.1130 0.055 Uiso 1 1 calc R . . H25C H -1.1805 -0.5704 -0.0483 0.055 Uiso 1 1 calc R . . C26 C -1.1443(4) -0.4410(3) -0.0725(4) 0.039(2) Uani 1 1 d . . . H26A H -1.1520 -0.4575 -0.1136 0.058 Uiso 1 1 calc R . . H26B H -1.1277 -0.4065 -0.0794 0.058 Uiso 1 1 calc R . . H26C H -1.1796 -0.4374 -0.0486 0.058 Uiso 1 1 calc R . . C27 C -1.0890(4) -0.2185(2) 0.1314(5) 0.047(2) Uani 1 1 d . . . H27A H -1.0507 -0.2044 0.1354 0.071 Uiso 1 1 calc R . . H27B H -1.1108 -0.2098 0.1695 0.071 Uiso 1 1 calc R . . H27C H -1.1073 -0.2033 0.0940 0.071 Uiso 1 1 calc R . . C28 C -1.1969(4) -0.2788(3) 0.1304(5) 0.050(2) Uani 1 1 d . . . H28A H -1.2054 -0.2597 0.0912 0.075 Uiso 1 1 calc R . . H28B H -1.1944 -0.2542 0.1660 0.075 Uiso 1 1 calc R . . H28C H -1.2268 -0.3043 0.1387 0.075 Uiso 1 1 calc R . . C29 C -0.9448(3) -0.7778(3) 0.0541(4) 0.042(2) Uani 1 1 d . . . H29A H -0.9606 -0.8095 0.0731 0.063 Uiso 1 1 calc R . . H29B H -0.9039 -0.7818 0.0492 0.063 Uiso 1 1 calc R . . H29C H -0.9620 -0.7721 0.0123 0.063 Uiso 1 1 calc R . . C30 C -0.9242(4) -0.6577(3) 0.0732(4) 0.039(2) Uani 1 1 d . . . H30A H -0.9381 -0.6516 0.0299 0.058 Uiso 1 1 calc R . . H30B H -0.8832 -0.6630 0.0721 0.058 Uiso 1 1 calc R . . H30C H -0.9330 -0.6274 0.0998 0.058 Uiso 1 1 calc R . . C31 C -0.9299(4) -0.7322(3) 0.1918(5) 0.042(2) Uani 1 1 d . . . C32 C -0.9560(5) -0.7828(3) 0.2227(6) 0.070(3) Uani 1 1 d . . . H32A H -0.9361 -0.7908 0.2623 0.105 Uiso 1 1 calc R . . H32B H -0.9520 -0.8122 0.1932 0.105 Uiso 1 1 calc R . . H32C H -0.9961 -0.7769 0.2317 0.105 Uiso 1 1 calc R . . C33 C -0.8657(4) -0.7382(4) 0.1894(5) 0.067(3) Uani 1 1 d . . . H33A H -0.8490 -0.7070 0.1702 0.101 Uiso 1 1 calc R . . H33B H -0.8560 -0.7689 0.1638 0.101 Uiso 1 1 calc R . . H33C H -0.8511 -0.7427 0.2326 0.101 Uiso 1 1 calc R . . C34 C -0.9456(4) -0.6863(3) 0.2352(4) 0.048(2) Uani 1 1 d . . . H34A H -0.9866 -0.6813 0.2346 0.072 Uiso 1 1 calc R . . H34B H -0.9271 -0.6545 0.2199 0.072 Uiso 1 1 calc R . . H34C H -0.9332 -0.6937 0.2787 0.072 Uiso 1 1 calc R . . C35 C -0.9208(4) -0.3422(3) 0.0728(5) 0.046(2) Uani 1 1 d . . . H35A H -0.9318 -0.3746 0.0942 0.069 Uiso 1 1 calc R . . H35B H -0.8800 -0.3369 0.0773 0.069 Uiso 1 1 calc R . . H35C H -0.9304 -0.3445 0.0276 0.069 Uiso 1 1 calc R . . C36 C -0.9485(4) -0.2227(3) 0.0598(5) 0.061(3) Uani 1 1 d . . . H36A H -0.9080 -0.2177 0.0528 0.092 Uiso 1 1 calc R . . H36B H -0.9640 -0.1923 0.0820 0.092 Uiso 1 1 calc R . . H36C H -0.9676 -0.2269 0.0188 0.092 Uiso 1 1 calc R . . C37 C -0.9298(4) -0.2729(3) 0.1950(5) 0.046(2) Uani 1 1 d . . . C38 C -0.9398(4) -0.3211(4) 0.2360(4) 0.061(2) Uani 1 1 d . . . H38A H -0.9242 -0.3152 0.2786 0.091 Uiso 1 1 calc R . . H38B H -0.9212 -0.3513 0.2166 0.091 Uiso 1 1 calc R . . H38C H -0.9804 -0.3278 0.2392 0.091 Uiso 1 1 calc R . . C39 C -0.8654(5) -0.2625(4) 0.1912(6) 0.084(4) Uani 1 1 d . . . H39A H -0.8508 -0.2550 0.2339 0.127 Uiso 1 1 calc R . . H39B H -0.8583 -0.2325 0.1634 0.127 Uiso 1 1 calc R . . H39C H -0.8463 -0.2934 0.1741 0.127 Uiso 1 1 calc R . . C40 C -0.9587(6) -0.2261(4) 0.2283(6) 0.094(4) Uani 1 1 d . . . H40A H -0.9978 -0.2353 0.2386 0.141 Uiso 1 1 calc R . . H40B H -0.9584 -0.1958 0.1999 0.141 Uiso 1 1 calc R . . H40C H -0.9383 -0.2177 0.2675 0.141 Uiso 1 1 calc R . . C41 C -1.3057(4) -0.4689(3) 0.2013(5) 0.047(2) Uani 1 1 d . . . C42 C -1.3115(4) -0.5255(4) 0.1960(4) 0.046(2) Uani 1 1 d . . . C43 C -1.2808(3) -0.5487(3) 0.2474(5) 0.0368(18) Uani 1 1 d . . . C44 C -1.2551(5) -0.5067(2) 0.2871(5) 0.039(2) Uani 1 1 d . . . C45 C -1.2726(4) -0.4581(3) 0.2550(5) 0.048(2) Uani 1 1 d . . . C46 C -1.3340(4) -0.4270(4) 0.1585(6) 0.107(4) Uani 1 1 d . . . H46A H -1.3656 -0.4111 0.1814 0.160 Uiso 1 1 calc R . . H46B H -1.3479 -0.4435 0.1195 0.160 Uiso 1 1 calc R . . H46C H -1.3063 -0.4001 0.1476 0.160 Uiso 1 1 calc R . . C47 C -1.3462(4) -0.5537(4) 0.1448(5) 0.091(3) Uani 1 1 d . . . H47A H -1.3313 -0.5890 0.1386 0.137 Uiso 1 1 calc R . . H47B H -1.3438 -0.5343 0.1048 0.137 Uiso 1 1 calc R . . H47C H -1.3857 -0.5558 0.1583 0.137 Uiso 1 1 calc R . . C48 C -1.2771(4) -0.6088(3) 0.2596(5) 0.074(3) Uani 1 1 d . . . H48A H -1.3099 -0.6200 0.2844 0.111 Uiso 1 1 calc R . . H48B H -1.2425 -0.6167 0.2832 0.111 Uiso 1 1 calc R . . H48C H -1.2766 -0.6273 0.2188 0.111 Uiso 1 1 calc R . . C49 C -1.2219(5) -0.5144(4) 0.3446(5) 0.088(3) Uani 1 1 d . . . H49A H -1.2460 -0.5091 0.3820 0.132 Uiso 1 1 calc R . . H49B H -1.1907 -0.4893 0.3455 0.132 Uiso 1 1 calc R . . H49C H -1.2067 -0.5500 0.3452 0.132 Uiso 1 1 calc R . . C50 C -1.2552(5) -0.4029(3) 0.2808(5) 0.117(5) Uani 1 1 d . . . H50A H -1.2423 -0.3811 0.2454 0.176 Uiso 1 1 calc R . . H50B H -1.2246 -0.4068 0.3118 0.176 Uiso 1 1 calc R . . H50C H -1.2878 -0.3865 0.3012 0.176 Uiso 1 1 calc R . . C51 C -1.0087(4) -0.5254(3) -0.1478(4) 0.043(2) Uani 1 1 d . . . C52 C -0.9706(3) -0.5530(2) -0.1110(4) 0.0499(18) Uani 1 1 d . . . C53 C -0.9377(4) -0.5170(4) -0.0775(4) 0.060(2) Uani 1 1 d . . . C54 C -0.9544(4) -0.4657(4) -0.0934(5) 0.079(4) Uani 1 1 d . . . C55 C -1.0003(5) -0.4700(3) -0.1396(4) 0.051(2) Uani 1 1 d . . . C56 C -1.0519(4) -0.5439(3) -0.1970(4) 0.1018(12) Uani 1 1 d . . . H56A H -1.0867 -0.5236 -0.1926 0.153 Uiso 1 1 calc R . . H56B H -1.0602 -0.5810 -0.1901 0.153 Uiso 1 1 calc R . . H56C H -1.0365 -0.5391 -0.2399 0.153 Uiso 1 1 calc R . . C57 C -0.9657(4) -0.6136(3) -0.1171(4) 0.1018(12) Uani 1 1 d . . . H57A H -0.9437 -0.6224 -0.1550 0.153 Uiso 1 1 calc R . . H57B H -1.0036 -0.6288 -0.1207 0.153 Uiso 1 1 calc R . . H57C H -0.9469 -0.6277 -0.0793 0.153 Uiso 1 1 calc R . . C58 C -0.8888(4) -0.5380(4) -0.0323(4) 0.1018(12) Uani 1 1 d . . . H58A H -0.9053 -0.5507 0.0075 0.153 Uiso 1 1 calc R . . H58B H -0.8623 -0.5096 -0.0231 0.153 Uiso 1 1 calc R . . H58C H -0.8688 -0.5666 -0.0535 0.153 Uiso 1 1 calc R . . C59 C -0.9218(4) -0.4178(3) -0.0695(4) 0.1018(12) Uani 1 1 d . . . H59A H -0.8903 -0.4104 -0.0984 0.153 Uiso 1 1 calc R . . H59B H -0.9072 -0.4247 -0.0268 0.153 Uiso 1 1 calc R . . H59C H -0.9472 -0.3876 -0.0682 0.153 Uiso 1 1 calc R . . C60 C -1.0250(4) -0.4231(3) -0.1694(4) 0.1018(12) Uani 1 1 d . . . H60A H -1.0059 -0.4161 -0.2098 0.153 Uiso 1 1 calc R . . H60B H -1.0203 -0.3931 -0.1410 0.153 Uiso 1 1 calc R . . H60C H -1.0653 -0.4290 -0.1773 0.153 Uiso 1 1 calc R . . Fe3 Fe -0.77262(6) -0.99392(3) 0.59750(7) 0.0299(3) Uani 1 1 d . . . Fe4 Fe -0.97605(6) -0.99808(2) 0.35479(7) 0.0257(3) Uani 1 1 d . . . P5 P -0.77896(13) -0.99467(5) 0.48430(13) 0.0291(6) Uani 1 1 d . . . P6 P -0.95600(12) -0.99316(6) 0.46178(13) 0.0312(5) Uani 1 1 d . . . P7 P -0.80362(9) -1.12396(7) 0.43203(10) 0.0280(4) Uani 1 1 d . . . P8 P -0.81272(9) -0.86768(7) 0.42955(10) 0.0306(4) Uani 1 1 d . . . Si3 Si -0.70827(10) -1.21616(8) 0.43511(11) 0.0312(5) Uani 1 1 d . . . Si4 Si -0.71282(11) -0.78134(8) 0.43672(12) 0.0318(5) Uani 1 1 d . . . O5 O -0.8107(2) -0.85467(19) 0.5613(3) 0.0441(13) Uani 1 1 d . . . O6 O -0.7941(2) -1.1355(2) 0.5641(3) 0.0423(13) Uani 1 1 d . . . O7 O -0.9707(2) -1.10962(19) 0.4699(3) 0.0581(15) Uani 1 1 d . . . O8 O -0.9864(2) -0.87373(17) 0.4442(3) 0.0573(14) Uani 1 1 d . . . C61 C -0.8129(3) -0.8883(3) 0.5203(4) 0.0313(17) Uani 1 1 d . . . C62 C -0.8174(3) -0.9454(2) 0.5314(3) 0.0241(15) Uani 1 1 d . . . C63 C -0.8557(3) -0.9690(3) 0.5777(4) 0.0278(17) Uani 1 1 d . . . C64 C -0.8539(3) -1.0254(3) 0.5779(4) 0.0275(17) Uani 1 1 d . . . C65 C -0.8128(3) -1.0468(3) 0.5316(4) 0.0283(16) Uani 1 1 d . . . C66 C -0.8024(3) -1.1029(3) 0.5221(3) 0.0283(16) Uani 1 1 d . . . C67 C -0.7856(3) -1.1940(3) 0.4319(4) 0.0277(16) Uani 1 1 d . . . C68 C -0.8345(3) -1.2236(3) 0.4252(4) 0.0334(17) Uani 1 1 d . . . C69 C -0.8884(3) -1.1914(3) 0.4246(4) 0.0339(17) Uani 1 1 d . . . C70 C -0.8803(3) -1.1381(3) 0.4314(3) 0.0312(15) Uani 1 1 d . . . C71 C -0.9276(3) -1.0986(2) 0.4384(3) 0.0315(15) Uani 1 1 d . . . C72 C -0.9223(3) -1.0431(3) 0.4136(4) 0.0348(17) Uani 1 1 d . . . C73 C -0.8909(3) -1.0226(3) 0.3584(4) 0.0288(15) Uani 1 1 d . . . C74 C -0.8942(3) -0.9664(3) 0.3561(4) 0.0285(16) Uani 1 1 d . . . C75 C -0.9269(3) -0.9440(3) 0.4079(4) 0.0310(16) Uani 1 1 d . . . C76 C -0.9372(3) -0.8887(3) 0.4256(3) 0.0355(17) Uani 1 1 d . . . C77 C -0.8888(3) -0.8493(3) 0.4259(4) 0.0326(16) Uani 1 1 d . . . C78 C -0.8941(3) -0.7950(3) 0.4221(4) 0.0328(16) Uani 1 1 d . . . C79 C -0.8390(3) -0.7664(3) 0.4255(4) 0.0308(17) Uani 1 1 d . . . C80 C -0.7906(3) -0.7981(3) 0.4322(4) 0.0314(17) Uani 1 1 d . . . C81 C -0.8968(3) -0.9366(3) 0.6187(4) 0.0386(19) Uani 1 1 d . . . H81A H -0.9315 -0.9301 0.5947 0.058 Uiso 1 1 calc R . . H81B H -0.8791 -0.9033 0.6298 0.058 Uiso 1 1 calc R . . H81C H -0.9058 -0.9559 0.6576 0.058 Uiso 1 1 calc R . . C82 C -0.8919(3) -1.0601(3) 0.6191(4) 0.0372(19) Uani 1 1 d . . . H82A H -0.9002 -1.0423 0.6592 0.056 Uiso 1 1 calc R . . H82B H -0.8725 -1.0931 0.6279 0.056 Uiso 1 1 calc R . . H82C H -0.9273 -1.0672 0.5965 0.056 Uiso 1 1 calc R . . C83 C -0.8370(4) -1.2836(3) 0.4173(5) 0.053(2) Uani 1 1 d . . . H83A H -0.7991 -1.2983 0.4230 0.079 Uiso 1 1 calc R . . H83B H -0.8508 -1.2922 0.3746 0.079 Uiso 1 1 calc R . . H83C H -0.8625 -1.2984 0.4491 0.079 Uiso 1 1 calc R . . C84 C -0.9457(4) -1.2199(3) 0.4196(4) 0.0432(18) Uani 1 1 d . . . H84A H -0.9511 -1.2421 0.4571 0.065 Uiso 1 1 calc R . . H84B H -0.9462 -1.2416 0.3812 0.065 Uiso 1 1 calc R . . H84C H -0.9763 -1.1942 0.4174 0.065 Uiso 1 1 calc R . . C85 C -0.8604(3) -1.0563(3) 0.3080(4) 0.0406(19) Uani 1 1 d . . . H85A H -0.8687 -1.0427 0.2655 0.061 Uiso 1 1 calc R . . H85B H -0.8735 -1.0925 0.3111 0.061 Uiso 1 1 calc R . . H85C H -0.8196 -1.0551 0.3155 0.061 Uiso 1 1 calc R . . C86 C -0.8657(3) -0.9331(3) 0.3022(4) 0.0382(18) Uani 1 1 d . . . H86A H -0.8841 -0.8989 0.2996 0.057 Uiso 1 1 calc R . . H86B H -0.8697 -0.9513 0.2614 0.057 Uiso 1 1 calc R . . H86C H -0.8256 -0.9284 0.3119 0.057 Uiso 1 1 calc R . . C87 C -0.9487(3) -0.7646(3) 0.4141(4) 0.0417(18) Uani 1 1 d . . . H87A H -0.9805 -0.7890 0.4120 0.063 Uiso 1 1 calc R . . H87B H -0.9471 -0.7441 0.3748 0.063 Uiso 1 1 calc R . . H87C H -0.9538 -0.7411 0.4504 0.063 Uiso 1 1 calc R . . C88 C -0.8373(4) -0.7062(2) 0.4209(5) 0.0429(18) Uani 1 1 d . . . H88A H -0.7992 -0.6938 0.4312 0.064 Uiso 1 1 calc R . . H88B H -0.8644 -0.6912 0.4510 0.064 Uiso 1 1 calc R . . H88C H -0.8471 -0.6954 0.3776 0.064 Uiso 1 1 calc R . . C89 C -0.6983(4) -1.2761(3) 0.4864(4) 0.055(3) Uani 1 1 d . . . H89A H -0.6957 -1.2656 0.5311 0.083 Uiso 1 1 calc R . . H89B H -0.6634 -1.2940 0.4739 0.083 Uiso 1 1 calc R . . H89C H -0.7304 -1.2997 0.4808 0.083 Uiso 1 1 calc R . . C90 C -0.6690(3) -1.1600(3) 0.4726(5) 0.045(2) Uani 1 1 d . . . H90A H -0.6830 -1.1270 0.4550 0.068 Uiso 1 1 calc R . . H90B H -0.6286 -1.1634 0.4635 0.068 Uiso 1 1 calc R . . H90C H -0.6751 -1.1604 0.5186 0.068 Uiso 1 1 calc R . . C91 C -0.6781(4) -1.2303(3) 0.3508(4) 0.035(2) Uani 1 1 d . . . C92 C -0.6122(4) -1.2401(4) 0.3581(4) 0.056(2) Uani 1 1 d . . . H92A H -0.6059 -1.2697 0.3867 0.084 Uiso 1 1 calc R . . H92B H -0.5943 -1.2088 0.3757 0.084 Uiso 1 1 calc R . . H92C H -0.5959 -1.2479 0.3163 0.084 Uiso 1 1 calc R . . C93 C -0.7053(4) -1.2802(3) 0.3219(4) 0.052(2) Uani 1 1 d . . . H93A H -0.6901 -1.2861 0.2792 0.078 Uiso 1 1 calc R . . H93B H -0.7463 -1.2757 0.3194 0.078 Uiso 1 1 calc R . . H93C H -0.6966 -1.3103 0.3489 0.078 Uiso 1 1 calc R . . C94 C -0.6873(4) -1.1815(3) 0.3051(4) 0.053(2) Uani 1 1 d . . . H94A H -0.6696 -1.1884 0.2639 0.080 Uiso 1 1 calc R . . H94B H -0.6702 -1.1504 0.3242 0.080 Uiso 1 1 calc R . . H94C H -0.7278 -1.1756 0.2990 0.080 Uiso 1 1 calc R . . C95 C -0.6783(3) -0.8413(3) 0.4718(4) 0.042(2) Uani 1 1 d . . . H95A H -0.6918 -0.8464 0.5154 0.063 Uiso 1 1 calc R . . H95B H -0.6372 -0.8366 0.4721 0.063 Uiso 1 1 calc R . . H95C H -0.6880 -0.8719 0.4461 0.063 Uiso 1 1 calc R . . C96 C -0.6987(4) -0.7236(3) 0.4905(5) 0.052(2) Uani 1 1 d . . . H96A H -0.7318 -0.7007 0.4909 0.077 Uiso 1 1 calc R . . H96B H -0.6659 -0.7043 0.4748 0.077 Uiso 1 1 calc R . . H96C H -0.6912 -0.7361 0.5337 0.077 Uiso 1 1 calc R . . C97 C -0.6818(4) -0.7675(3) 0.3522(4) 0.038(2) Uani 1 1 d . . . C98 C -0.6959(4) -0.8142(3) 0.3057(4) 0.058(3) Uani 1 1 d . . . H98A H -0.6772 -0.8083 0.2648 0.086 Uiso 1 1 calc R . . H98B H -0.7368 -0.8161 0.2992 0.086 Uiso 1 1 calc R . . H98C H -0.6824 -0.8470 0.3242 0.086 Uiso 1 1 calc R . . C99 C -0.6143(3) -0.7614(3) 0.3591(4) 0.050(2) Uani 1 1 d . . . H99A H -0.5978 -0.7543 0.3173 0.075 Uiso 1 1 calc R . . H99B H -0.5984 -0.7937 0.3763 0.075 Uiso 1 1 calc R . . H99C H -0.6058 -0.7324 0.3879 0.075 Uiso 1 1 calc R . . C100 C -0.7048(4) -0.7146(3) 0.3261(4) 0.051(2) Uani 1 1 d . . . H10A H -0.6960 -0.6866 0.3563 0.077 Uiso 1 1 calc R . . H10B H -0.7458 -0.7170 0.3206 0.077 Uiso 1 1 calc R . . H10C H -0.6871 -0.7070 0.2851 0.077 Uiso 1 1 calc R . . C101 C -0.6873(3) -0.9750(3) 0.6202(4) 0.0431(18) Uani 1 1 d . . . C102 C -0.6995(4) -1.0307(3) 0.6346(4) 0.046(2) Uani 1 1 d . . . C103 C -0.7463(5) -1.0293(3) 0.6819(4) 0.055(3) Uani 1 1 d . . . C104 C -0.7591(4) -0.9755(3) 0.6947(4) 0.044(2) Uani 1 1 d . . . C105 C -0.7226(3) -0.9434(2) 0.6572(3) 0.0491(17) Uani 1 1 d . . . C106 C -0.6388(2) -0.9599(3) 0.5750(3) 0.0590(17) Uani 1 1 d . . . H10D H -0.6075 -0.9454 0.5997 0.088 Uiso 1 1 calc R . . H10E H -0.6523 -0.9337 0.5446 0.088 Uiso 1 1 calc R . . H10F H -0.6259 -0.9909 0.5519 0.088 Uiso 1 1 calc R . . C107 C -0.6697(3) -1.0801(3) 0.6129(4) 0.132(4) Uani 1 1 d . . . H10G H -0.6612 -1.0775 0.5674 0.199 Uiso 1 1 calc R . . H10H H -0.6941 -1.1103 0.6205 0.199 Uiso 1 1 calc R . . H10I H -0.6344 -1.0843 0.6367 0.199 Uiso 1 1 calc R . . C108 C -0.7764(4) -1.0764(3) 0.7169(4) 0.121(4) Uani 1 1 d . . . H10J H -0.7500 -1.0927 0.7466 0.182 Uiso 1 1 calc R . . H10K H -0.7887 -1.1022 0.6854 0.182 Uiso 1 1 calc R . . H10L H -0.8093 -1.0634 0.7403 0.182 Uiso 1 1 calc R . . C109 C -0.8016(3) -0.9541(3) 0.7435(3) 0.0615(17) Uani 1 1 d . . . H10M H -0.7827 -0.9496 0.7846 0.092 Uiso 1 1 calc R . . H10N H -0.8330 -0.9787 0.7481 0.092 Uiso 1 1 calc R . . H10O H -0.8160 -0.9203 0.7289 0.092 Uiso 1 1 calc R . . C110 C -0.7161(3) -0.88391(18) 0.6594(3) 0.0504(14) Uani 1 1 d . . . H11A H -0.7531 -0.8675 0.6538 0.076 Uiso 1 1 calc R . . H11B H -0.6907 -0.8726 0.6253 0.076 Uiso 1 1 calc R . . H11C H -0.7003 -0.8736 0.7006 0.076 Uiso 1 1 calc R . . C111 C -1.0313(3) -0.9547(3) 0.2962(5) 0.0386(19) Uani 1 1 d . . . C112 C -1.0045(6) -0.9955(3) 0.2608(6) 0.048(3) Uani 1 1 d . . . C113 C -1.0194(3) -1.0458(3) 0.2896(5) 0.047(2) Uani 1 1 d . . . C114 C -1.0563(3) -1.0335(3) 0.3428(5) 0.044(2) Uani 1 1 d . . . C115 C -1.0630(3) -0.9797(3) 0.3464(4) 0.0351(17) Uani 1 1 d . . . C116 C -1.0298(4) -0.8971(3) 0.2806(4) 0.071(3) Uani 1 1 d . . . H11D H -1.0614 -0.8884 0.2524 0.107 Uiso 1 1 calc R . . H11E H -0.9941 -0.8887 0.2593 0.107 Uiso 1 1 calc R . . H11F H -1.0329 -0.8767 0.3199 0.107 Uiso 1 1 calc R . . C117 C -0.9708(5) -0.9887(3) 0.1968(5) 0.067(2) Uani 1 1 d . . . H11G H -0.9956 -0.9968 0.1608 0.100 Uiso 1 1 calc R . . H11H H -0.9384 -1.0124 0.1965 0.100 Uiso 1 1 calc R . . H11I H -0.9576 -0.9526 0.1931 0.100 Uiso 1 1 calc R . . C118 C -1.0027(4) -1.0990(3) 0.2635(4) 0.075(3) Uani 1 1 d . . . H11J H -0.9810 -1.1181 0.2956 0.112 Uiso 1 1 calc R . . H11K H -0.9795 -1.0944 0.2253 0.112 Uiso 1 1 calc R . . H11L H -1.0368 -1.1188 0.2527 0.112 Uiso 1 1 calc R . . C119 C -1.0845(4) -1.0741(3) 0.3868(4) 0.077(3) Uani 1 1 d . . . H11M H -1.0774 -1.0648 0.4313 0.115 Uiso 1 1 calc R . . H11N H -1.0687 -1.1087 0.3782 0.115 Uiso 1 1 calc R . . H11O H -1.1253 -1.0746 0.3789 0.115 Uiso 1 1 calc R . . C120 C -1.1002(3) -0.9500(3) 0.3952(4) 0.062(2) Uani 1 1 d . . . H12A H -1.1384 -0.9458 0.3780 0.093 Uiso 1 1 calc R . . H12B H -1.0837 -0.9155 0.4034 0.093 Uiso 1 1 calc R . . H12C H -1.1019 -0.9698 0.4350 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0267(8) 0.0197(5) 0.0300(8) -0.0007(3) 0.0015(6) -0.0005(3) Fe2 0.0341(7) 0.0325(5) 0.0232(6) -0.0002(4) 0.0022(5) 0.0010(3) P1 0.0302(12) 0.0381(9) 0.0285(11) -0.0014(7) -0.0043(8) -0.0007(7) P2 0.0334(13) 0.0252(8) 0.0247(11) -0.0012(6) 0.0011(8) -0.0023(6) P3 0.0356(10) 0.0250(8) 0.0307(9) -0.0010(7) -0.0003(7) 0.0046(7) P4 0.0377(10) 0.0240(8) 0.0309(9) 0.0004(7) 0.0007(7) -0.0063(7) Si1 0.0314(12) 0.0224(9) 0.0321(13) -0.0021(8) 0.0009(10) 0.0017(8) Si2 0.0348(12) 0.0259(10) 0.0339(13) 0.0042(9) 0.0000(10) -0.0045(9) O1 0.042(3) 0.044(3) 0.067(3) 0.023(2) -0.026(2) -0.012(2) O2 0.048(3) 0.045(3) 0.100(4) -0.044(3) -0.037(3) 0.022(2) O3 0.067(3) 0.027(2) 0.035(2) -0.0098(18) -0.007(2) 0.012(2) O4 0.084(4) 0.033(2) 0.033(3) 0.0040(19) 0.001(2) -0.019(2) C1 0.056(5) 0.047(4) 0.037(4) 0.010(3) 0.004(3) -0.015(3) C2 0.021(3) 0.034(3) 0.031(3) 0.001(2) -0.004(3) -0.008(2) C3 0.031(4) 0.047(4) 0.026(3) 0.009(3) -0.003(3) -0.007(3) C4 0.030(4) 0.040(3) 0.026(3) -0.006(2) -0.003(3) 0.005(3) C5 0.029(4) 0.030(3) 0.039(4) -0.008(3) -0.005(3) 0.010(3) C6 0.043(4) 0.036(3) 0.039(4) -0.015(3) -0.007(3) 0.006(3) C7 0.031(3) 0.030(3) 0.032(3) -0.002(2) -0.003(3) 0.005(3) C8 0.036(4) 0.034(3) 0.026(3) -0.004(2) 0.003(3) -0.001(3) C9 0.031(4) 0.035(3) 0.029(3) 0.007(2) 0.002(3) 0.001(3) C10 0.043(4) 0.023(3) 0.030(4) 0.002(3) -0.001(3) -0.002(3) C11 0.042(4) 0.021(3) 0.036(4) 0.001(2) 0.000(3) 0.003(3) C12 0.044(4) 0.028(3) 0.028(4) -0.001(3) 0.004(3) 0.005(3) C13 0.047(4) 0.030(3) 0.021(3) -0.003(2) -0.001(3) 0.009(3) C14 0.042(4) 0.030(4) 0.022(3) 0.000(3) 0.004(3) -0.007(3) C15 0.045(4) 0.017(3) 0.028(3) 0.005(2) 0.005(3) -0.002(3) C16 0.041(4) 0.029(3) 0.039(4) 0.003(3) -0.002(3) -0.002(3) C17 0.047(4) 0.023(3) 0.033(4) 0.000(3) -0.001(3) 0.002(3) C18 0.041(4) 0.021(3) 0.031(3) -0.005(2) 0.001(3) -0.001(3) C19 0.040(4) 0.035(4) 0.031(3) -0.005(3) 0.002(3) 0.002(3) C20 0.036(4) 0.037(3) 0.034(3) 0.002(3) 0.001(3) -0.006(3) C21 0.042(4) 0.034(3) 0.034(4) 0.002(3) -0.005(3) -0.013(3) C22 0.042(5) 0.043(4) 0.038(4) -0.006(3) -0.009(3) 0.015(3) C23 0.028(4) 0.047(4) 0.062(4) -0.001(3) 0.000(3) -0.004(3) C24 0.033(4) 0.039(4) 0.064(5) 0.000(3) 0.008(3) -0.006(3) C25 0.043(5) 0.028(3) 0.039(4) -0.004(3) 0.000(3) 0.005(3) C26 0.049(5) 0.026(3) 0.040(5) -0.001(3) 0.001(4) -0.005(3) C27 0.038(4) 0.024(3) 0.079(5) -0.002(3) 0.001(4) -0.004(3) C28 0.032(4) 0.051(4) 0.066(5) -0.007(3) -0.004(3) 0.000(3) C29 0.032(4) 0.041(4) 0.053(5) -0.022(3) 0.001(4) 0.007(3) C30 0.036(4) 0.033(4) 0.049(5) 0.002(3) 0.003(3) -0.006(3) C31 0.039(5) 0.036(4) 0.053(5) 0.005(3) -0.006(4) -0.003(3) C32 0.110(8) 0.038(4) 0.062(6) 0.006(4) -0.007(5) -0.006(5) C33 0.063(7) 0.050(5) 0.088(7) -0.006(5) -0.011(6) 0.006(5) C34 0.059(5) 0.051(4) 0.035(4) -0.006(3) -0.008(3) -0.007(4) C35 0.047(5) 0.043(4) 0.049(5) -0.006(3) 0.011(4) 0.006(4) C36 0.051(5) 0.049(5) 0.083(7) 0.048(4) -0.008(5) -0.014(4) C37 0.038(5) 0.043(4) 0.057(5) -0.006(4) -0.011(4) 0.002(3) C38 0.070(6) 0.075(6) 0.037(4) 0.008(4) -0.012(4) -0.009(4) C39 0.079(8) 0.071(7) 0.103(8) 0.031(6) -0.028(7) -0.024(6) C40 0.163(11) 0.062(6) 0.058(6) -0.018(4) -0.024(6) 0.054(6) C41 0.038(4) 0.048(4) 0.057(5) 0.018(3) 0.015(4) 0.018(3) C42 0.038(4) 0.063(5) 0.038(4) -0.009(3) 0.007(3) -0.004(4) C43 0.031(4) 0.028(3) 0.052(4) 0.005(3) 0.007(3) -0.001(3) C44 0.030(5) 0.056(4) 0.032(5) 0.000(3) 0.005(4) -0.007(3) C45 0.060(5) 0.026(4) 0.058(5) -0.011(3) 0.032(4) -0.006(3) C46 0.064(6) 0.091(7) 0.166(10) 0.055(7) 0.038(6) 0.047(5) C47 0.043(5) 0.147(9) 0.084(6) -0.013(6) 0.002(4) -0.036(5) C48 0.088(6) 0.031(3) 0.103(6) 0.014(3) 0.028(5) -0.011(3) C49 0.060(6) 0.175(8) 0.029(5) 0.000(6) 0.011(4) -0.020(7) C50 0.147(10) 0.064(6) 0.140(9) -0.067(6) 0.092(7) -0.041(6) C51 0.050(5) 0.064(5) 0.014(3) -0.007(3) 0.004(3) -0.004(4) C52 0.063(5) 0.034(3) 0.053(4) 0.000(3) 0.027(3) 0.014(3) C53 0.044(5) 0.101(7) 0.036(4) 0.015(5) 0.015(3) 0.009(5) C54 0.082(7) 0.102(7) 0.054(6) -0.057(5) 0.055(5) -0.074(6) C55 0.079(6) 0.043(4) 0.032(4) 0.017(3) 0.023(4) 0.022(4) C56 0.124(3) 0.099(3) 0.082(2) -0.006(2) 0.031(2) 0.000(3) C57 0.124(3) 0.099(3) 0.082(2) -0.006(2) 0.031(2) 0.000(3) C58 0.124(3) 0.099(3) 0.082(2) -0.006(2) 0.031(2) 0.000(3) C59 0.124(3) 0.099(3) 0.082(2) -0.006(2) 0.031(2) 0.000(3) C60 0.124(3) 0.099(3) 0.082(2) -0.006(2) 0.031(2) 0.000(3) Fe3 0.0378(7) 0.0266(4) 0.0252(6) -0.0004(5) -0.0031(5) -0.0033(3) Fe4 0.0256(8) 0.0245(6) 0.0271(7) -0.0006(3) 0.0011(6) -0.0004(3) P5 0.0378(14) 0.0251(8) 0.0244(11) -0.0004(6) 0.0003(9) -0.0038(6) P6 0.0312(12) 0.0333(8) 0.0290(11) -0.0012(8) 0.0039(8) -0.0027(7) P7 0.0309(9) 0.0219(7) 0.0313(9) -0.0008(6) 0.0004(7) 0.0019(6) P8 0.0378(10) 0.0215(7) 0.0324(9) 0.0009(7) 0.0005(8) -0.0057(7) Si3 0.0315(12) 0.0259(10) 0.0362(13) 0.0014(9) -0.0014(10) 0.0033(8) Si4 0.0343(12) 0.0235(9) 0.0376(13) -0.0013(9) -0.0032(11) -0.0018(8) O5 0.070(3) 0.028(2) 0.035(3) -0.0047(18) 0.001(2) -0.009(2) O6 0.063(3) 0.031(2) 0.033(2) 0.0053(19) -0.004(2) 0.003(2) O7 0.053(3) 0.047(3) 0.074(3) 0.022(2) 0.028(3) 0.014(2) O8 0.049(3) 0.039(2) 0.083(4) -0.016(2) 0.020(3) -0.011(2) C61 0.033(4) 0.030(3) 0.031(4) -0.005(2) 0.003(3) -0.006(3) C62 0.030(3) 0.020(3) 0.022(3) -0.003(2) -0.002(3) -0.001(2) C63 0.031(4) 0.019(3) 0.034(4) 0.000(2) -0.001(3) 0.006(3) C64 0.027(4) 0.022(3) 0.034(4) -0.002(3) 0.000(3) -0.005(3) C65 0.031(4) 0.031(3) 0.023(3) 0.001(2) -0.002(3) -0.003(3) C66 0.030(3) 0.029(3) 0.026(3) -0.007(2) -0.006(2) 0.000(2) C67 0.028(3) 0.020(3) 0.035(4) 0.001(2) -0.001(3) 0.003(2) C68 0.033(4) 0.030(3) 0.037(4) 0.003(3) 0.003(3) -0.002(3) C69 0.030(4) 0.042(4) 0.030(3) 0.004(3) -0.001(3) 0.000(3) C70 0.034(3) 0.029(3) 0.031(3) 0.005(2) 0.002(3) 0.002(3) C71 0.025(3) 0.031(3) 0.038(3) 0.001(2) 0.008(3) 0.001(2) C72 0.031(4) 0.040(4) 0.033(3) 0.006(3) -0.001(3) 0.004(3) C73 0.023(3) 0.033(4) 0.031(3) -0.004(3) -0.002(3) 0.001(3) C74 0.024(3) 0.028(3) 0.033(4) 0.000(2) -0.003(3) -0.006(2) C75 0.027(4) 0.039(4) 0.027(3) -0.005(3) -0.001(3) -0.005(3) C76 0.026(3) 0.037(3) 0.043(4) -0.010(3) 0.014(3) -0.012(3) C77 0.035(4) 0.033(3) 0.029(3) -0.003(3) 0.001(3) -0.007(3) C78 0.033(4) 0.028(3) 0.038(3) 0.002(2) 0.001(3) -0.002(2) C79 0.034(4) 0.019(3) 0.040(4) -0.003(2) -0.002(3) -0.001(2) C80 0.033(4) 0.022(3) 0.039(4) 0.001(3) -0.005(3) -0.011(3) C81 0.041(4) 0.038(4) 0.037(4) -0.003(3) 0.014(3) 0.007(3) C82 0.042(4) 0.034(4) 0.036(4) 0.001(3) 0.014(3) -0.018(3) C83 0.055(5) 0.030(3) 0.072(5) -0.012(3) 0.005(4) -0.014(3) C84 0.040(4) 0.048(4) 0.042(4) 0.001(3) -0.001(3) -0.004(3) C85 0.035(4) 0.055(4) 0.032(4) 0.006(3) 0.008(3) 0.015(3) C86 0.033(4) 0.046(4) 0.035(4) 0.002(3) 0.001(3) -0.003(3) C87 0.038(4) 0.043(4) 0.044(4) 0.002(3) 0.001(3) -0.004(3) C88 0.044(4) 0.017(3) 0.068(5) 0.004(3) -0.002(3) -0.003(3) C89 0.065(6) 0.050(5) 0.050(5) 0.000(4) -0.001(5) 0.009(4) C90 0.040(5) 0.048(5) 0.048(5) -0.003(4) -0.005(4) 0.007(4) C91 0.050(5) 0.024(3) 0.030(4) 0.001(3) 0.007(4) 0.006(3) C92 0.038(5) 0.081(7) 0.049(5) -0.004(4) 0.021(4) 0.014(4) C93 0.063(5) 0.048(4) 0.046(4) -0.025(3) 0.014(4) -0.012(4) C94 0.080(6) 0.038(4) 0.041(4) 0.007(3) 0.017(4) -0.001(4) C95 0.036(4) 0.049(5) 0.041(5) 0.003(3) 0.000(3) 0.005(3) C96 0.049(6) 0.052(5) 0.054(5) -0.002(4) -0.003(4) 0.000(4) C97 0.062(6) 0.022(3) 0.032(4) 0.000(3) 0.006(4) -0.001(3) C98 0.102(7) 0.036(4) 0.035(4) -0.002(3) 0.002(4) -0.016(4) C99 0.043(5) 0.057(5) 0.049(5) 0.006(4) 0.020(4) -0.003(4) C100 0.066(5) 0.038(4) 0.049(4) 0.022(3) 0.009(4) 0.008(3) C101 0.049(4) 0.037(3) 0.044(4) 0.015(3) -0.018(3) -0.012(3) C102 0.064(5) 0.026(3) 0.049(4) -0.013(3) -0.033(4) 0.007(3) C103 0.071(6) 0.047(4) 0.047(5) 0.026(4) -0.033(5) -0.028(4) C104 0.050(5) 0.047(4) 0.036(4) -0.011(3) -0.009(3) -0.008(3) C105 0.068(5) 0.039(3) 0.040(3) -0.010(3) -0.019(3) 0.007(3) C106 0.033(3) 0.103(5) 0.041(3) 0.020(3) -0.005(2) -0.007(3) C107 0.133(7) 0.087(5) 0.177(8) -0.097(5) -0.133(6) 0.095(5) C108 0.173(8) 0.104(6) 0.087(5) 0.088(4) -0.087(5) -0.111(6) C109 0.066(4) 0.091(5) 0.028(3) -0.021(3) 0.002(3) -0.005(3) C110 0.077(4) 0.028(3) 0.046(3) 0.001(2) -0.023(3) -0.027(3) C111 0.037(4) 0.034(4) 0.044(4) 0.008(3) -0.012(3) -0.001(3) C112 0.032(6) 0.077(6) 0.035(5) -0.002(3) -0.009(4) -0.003(3) C113 0.046(5) 0.036(4) 0.059(5) -0.019(3) -0.028(4) 0.015(3) C114 0.029(4) 0.053(4) 0.050(5) 0.011(4) -0.006(4) -0.017(3) C115 0.018(3) 0.047(4) 0.040(4) 0.001(3) -0.004(3) 0.002(3) C116 0.082(6) 0.027(3) 0.105(6) 0.011(3) -0.042(4) -0.013(3) C117 0.041(5) 0.116(6) 0.043(5) 0.016(4) 0.006(3) 0.000(4) C118 0.103(7) 0.043(4) 0.077(5) -0.019(3) -0.040(5) 0.010(4) C119 0.080(7) 0.085(6) 0.064(5) 0.038(4) -0.016(4) -0.050(5) C120 0.044(4) 0.085(6) 0.057(4) -0.026(4) 0.006(3) 0.015(4) _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 C41 2.055(8) . ? Fe1 C42 2.065(9) . ? Fe1 C45 2.061(8) . ? Fe1 C43 2.072(8) . ? Fe1 C3 2.066(8) . ? Fe1 C4 2.088(8) . ? Fe1 C2 2.105(8) . ? Fe1 C44 2.108(11) . ? Fe1 C5 2.103(8) . ? Fe1 P1 2.257(3) . ? Fe2 C54 2.035(8) . ? Fe2 C14 2.047(8) . ? Fe2 C13 2.058(8) . ? Fe2 C55 2.062(8) . ? Fe2 C53 2.051(8) . ? Fe2 C51 2.063(8) . ? Fe2 C15 2.072(7) . ? Fe2 C12 2.088(8) . ? Fe2 C52 2.092(6) . ? Fe2 P2 2.331(3) . ? P1 C5 1.784(8) . ? P1 C2 1.798(7) . ? P2 C15 1.761(7) . ? P2 C12 1.777(8) . ? P3 C10 1.809(7) . ? P3 C7 1.830(8) . ? P3 C11 1.888(8) . ? P4 C17 1.790(7) . ? P4 C20 1.811(8) . ? P4 C16 1.887(9) . ? Si1 C10 1.872(8) . ? Si1 C29 1.879(7) . ? Si1 C31 1.894(10) . ? Si1 C30 1.899(8) . ? Si2 C35 1.887(8) . ? Si2 C17 1.897(9) . ? Si2 C36 1.886(7) . ? Si2 C37 1.900(10) . ? O1 C1 1.216(9) . ? O2 C6 1.208(8) . ? O3 C11 1.216(9) . ? O4 C16 1.248(9) . ? C1 C2 1.474(10) . ? C1 C20 1.501(11) . ? C2 C3 1.462(11) . ? C3 C4 1.414(12) . ? C3 C21 1.510(10) . ? C4 C5 1.464(11) . ? C4 C22 1.473(11) . ? C5 C6 1.506(9) . ? C6 C7 1.466(10) . ? C7 C8 1.367(9) . ? C8 C9 1.448(10) . ? C8 C23 1.500(11) . ? C9 C10 1.365(11) . ? C9 C24 1.501(10) . ? C11 C12 1.523(9) . ? C12 C13 1.439(11) . ? C13 C14 1.439(13) . ? C13 C25 1.501(10) . ? C14 C15 1.429(11) . ? C14 C26 1.505(10) . ? C15 C16 1.519(9) . ? C17 C18 1.339(11) . ? C18 C19 1.459(11) . ? C18 C27 1.501(9) . ? C19 C20 1.358(10) . ? C19 C28 1.508(11) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9601 . ? C25 H25B 0.9601 . ? C25 H25C 0.9600 . ? C26 H26A 0.9601 . ? C26 H26B 0.9601 . ? C26 H26C 0.9601 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C33 1.497(12) . ? C31 C34 1.504(12) . ? C31 C32 1.545(13) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9601 . ? C33 H33B 0.9601 . ? C33 H33C 0.9601 . ? C34 H34A 0.9602 . ? C34 H34B 0.9602 . ? C34 H34C 0.9602 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.495(12) . ? C37 C39 1.519(13) . ? C37 C40 1.517(13) . ? C38 H38A 0.9603 . ? C38 H38B 0.9603 . ? C38 H38C 0.9603 . ? C39 H39A 0.9601 . ? C39 H39B 0.9601 . ? C39 H39C 0.9601 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C45 1.375(13) . ? C41 C42 1.432(16) . ? C41 C46 1.521(12) . ? C42 C43 1.403(12) . ? C42 C47 1.504(13) . ? C43 C44 1.461(11) . ? C43 C48 1.531(10) . ? C44 C45 1.446(11) . ? C44 C49 1.427(15) . ? C45 C50 1.536(10) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.357(11) . ? C51 C55 1.416(14) . ? C51 C56 1.500(12) . ? C52 C53 1.369(11) . ? C52 C57 1.532(9) . ? C53 C54 1.384(15) . ? C53 C58 1.560(11) . ? C54 C55 1.433(14) . ? C54 C59 1.504(10) . ? C55 C60 1.446(11) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? Fe3 C103 2.046(7) . ? Fe3 C102 2.078(8) . ? Fe3 C104 2.079(8) . ? Fe3 C63 2.068(7) . ? Fe3 C101 2.089(8) . ? Fe3 C64 2.085(7) . ? Fe3 C62 2.103(7) . ? Fe3 C65 2.115(7) . ? Fe3 C105 2.114(6) . ? Fe3 P5 2.338(3) . ? Fe4 C112 2.047(12) . ? Fe4 C113 2.062(8) . ? Fe4 C74 2.060(7) . ? Fe4 C73 2.072(7) . ? Fe4 C72 2.074(8) . ? Fe4 C115 2.078(7) . ? Fe4 C111 2.071(8) . ? Fe4 C114 2.080(8) . ? Fe4 C75 2.083(7) . ? Fe4 P6 2.257(3) . ? P5 C65 1.810(7) . ? P5 C62 1.809(7) . ? P6 C72 1.779(8) . ? P6 C75 1.792(8) . ? P7 C67 1.807(7) . ? P7 C70 1.814(8) . ? P7 C66 1.931(7) . ? P8 C80 1.822(7) . ? P8 C77 1.828(8) . ? P8 C61 1.940(8) . ? Si3 C90 1.847(8) . ? Si3 C89 1.853(9) . ? Si3 C67 1.879(7) . ? Si3 C91 1.905(9) . ? Si4 C95 1.851(8) . ? Si4 C96 1.853(9) . ? Si4 C80 1.856(8) . ? Si4 C97 1.917(9) . ? O5 C61 1.196(8) . ? O6 C66 1.205(8) . ? O7 C71 1.223(8) . ? O8 C76 1.263(8) . ? C61 C62 1.454(9) . ? C62 C63 1.431(10) . ? C63 C64 1.415(12) . ? C63 C81 1.511(9) . ? C64 C65 1.453(10) . ? C64 C82 1.503(9) . ? C65 C66 1.443(9) . ? C67 C68 1.363(10) . ? C68 C69 1.490(10) . ? C68 C83 1.518(10) . ? C69 C70 1.358(9) . ? C69 C84 1.515(10) . ? C70 C71 1.488(9) . ? C71 C72 1.488(9) . ? C72 C73 1.446(11) . ? C73 C74 1.415(11) . ? C73 C85 1.515(10) . ? C74 C75 1.425(11) . ? C74 C86 1.539(10) . ? C75 C76 1.455(10) . ? C76 C77 1.495(9) . ? C77 C78 1.369(9) . ? C78 C79 1.468(10) . ? C78 C87 1.490(10) . ? C79 C80 1.382(10) . ? C79 C88 1.515(8) . ? C81 H81A 0.9601 . ? C81 H81B 0.9601 . ? C81 H81C 0.9601 . ? C82 H82A 0.9601 . ? C82 H82B 0.9601 . ? C82 H82C 0.9601 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 C93 1.525(11) . ? C91 C94 1.561(11) . ? C91 C92 1.556(12) . ? C92 H92A 0.9601 . ? C92 H92B 0.9601 . ? C92 H92C 0.9601 . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C94 H94A 0.9602 . ? C94 H94B 0.9602 . ? C94 H94C 0.9602 . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C95 H95C 0.9600 . ? C96 H96A 0.9600 . ? C96 H96B 0.9600 . ? C96 H96C 0.9600 . ? C97 C100 1.529(11) . ? C97 C98 1.548(11) . ? C97 C99 1.579(12) . ? C98 H98A 0.9603 . ? C98 H98B 0.9603 . ? C98 H98C 0.9603 . ? C99 H99A 0.9601 . ? C99 H99B 0.9601 . ? C99 H99C 0.9601 . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? C101 C105 1.372(10) . ? C101 C102 1.457(11) . ? C101 C106 1.509(9) . ? C102 C103 1.459(13) . ? C102 C107 1.488(9) . ? C103 C104 1.407(13) . ? C103 C108 1.552(9) . ? C104 C105 1.401(11) . ? C104 C109 1.509(10) . ? C105 C110 1.502(7) . ? C106 H10D 0.9600 . ? C106 H10E 0.9600 . ? C106 H10F 0.9600 . ? C107 H10G 0.9601 . ? C107 H10H 0.9601 . ? C107 H10I 0.9601 . ? C108 H10J 0.9600 . ? C108 H10K 0.9600 . ? C108 H10L 0.9600 . ? C109 H10M 0.9600 . ? C109 H10N 0.9600 . ? C109 H10O 0.9600 . ? C110 H11A 0.9600 . ? C110 H11B 0.9600 . ? C110 H11C 0.9600 . ? C111 C112 1.403(13) . ? C111 C115 1.418(12) . ? C111 C116 1.482(10) . ? C112 C113 1.438(11) . ? C112 C117 1.544(16) . ? C113 C114 1.426(12) . ? C113 C118 1.491(10) . ? C114 C115 1.361(13) . ? C114 C119 1.512(10) . ? C115 C120 1.520(10) . ? C116 H11D 0.9600 . ? C116 H11E 0.9600 . ? C116 H11F 0.9600 . ? C117 H11G 0.9600 . ? C117 H11H 0.9600 . ? C117 H11I 0.9600 . ? C118 H11J 0.9600 . ? C118 H11K 0.9600 . ? C118 H11L 0.9600 . ? C119 H11M 0.9600 . ? C119 H11N 0.9600 . ? C119 H11O 0.9600 . ? C120 H12A 0.9600 . ? C120 H12B 0.9600 . ? C120 H12C 0.9600 . ? 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 C41 Fe1 C42 40.7(4) . . ? C41 Fe1 C45 39.0(4) . . ? C42 Fe1 C45 66.9(3) . . ? C41 Fe1 C43 67.4(3) . . ? C42 Fe1 C43 39.6(3) . . ? C45 Fe1 C43 67.2(4) . . ? C41 Fe1 C3 136.3(3) . . ? C42 Fe1 C3 176.5(3) . . ? C45 Fe1 C3 109.7(3) . . ? C43 Fe1 C3 140.2(3) . . ? C41 Fe1 C4 172.8(4) . . ? C42 Fe1 C4 143.0(3) . . ? C45 Fe1 C4 133.8(4) . . ? C43 Fe1 C4 112.0(3) . . ? C3 Fe1 C4 39.8(4) . . ? C41 Fe1 C2 110.8(3) . . ? C42 Fe1 C2 139.0(4) . . ? C45 Fe1 C2 111.3(3) . . ? C43 Fe1 C2 178.2(3) . . ? C3 Fe1 C2 41.0(3) . . ? C4 Fe1 C2 69.8(3) . . ? C41 Fe1 C44 67.8(4) . . ? C42 Fe1 C44 68.1(4) . . ? C45 Fe1 C44 40.6(3) . . ? C43 Fe1 C44 40.9(3) . . ? C3 Fe1 C44 109.7(4) . . ? C4 Fe1 C44 106.8(4) . . ? C2 Fe1 C44 138.6(3) . . ? C41 Fe1 C5 146.3(4) . . ? C42 Fe1 C5 114.2(3) . . ? C45 Fe1 C5 172.5(4) . . ? C43 Fe1 C5 108.5(3) . . ? C3 Fe1 C5 69.3(3) . . ? C4 Fe1 C5 40.9(3) . . ? C2 Fe1 C5 73.1(4) . . ? C44 Fe1 C5 132.2(3) . . ? C41 Fe1 P1 107.9(3) . . ? C42 Fe1 P1 104.4(3) . . ? C45 Fe1 P1 139.3(3) . . ? C43 Fe1 P1 131.9(3) . . ? C3 Fe1 P1 77.9(2) . . ? C4 Fe1 P1 77.9(2) . . ? C2 Fe1 P1 48.5(2) . . ? C44 Fe1 P1 172.3(3) . . ? C5 Fe1 P1 48.2(2) . . ? C54 Fe2 C14 127.5(4) . . ? C54 Fe2 C13 161.7(4) . . ? C14 Fe2 C13 41.0(4) . . ? C54 Fe2 C55 40.9(4) . . ? C14 Fe2 C55 103.1(4) . . ? C13 Fe2 C55 121.5(4) . . ? C54 Fe2 C53 39.6(4) . . ? C14 Fe2 C53 167.1(3) . . ? C13 Fe2 C53 151.0(4) . . ? C55 Fe2 C53 66.9(4) . . ? C54 Fe2 C51 66.8(3) . . ? C14 Fe2 C51 113.5(3) . . ? C13 Fe2 C51 102.7(3) . . ? C55 Fe2 C51 40.1(4) . . ? C53 Fe2 C51 64.8(4) . . ? C54 Fe2 C15 110.7(3) . . ? C14 Fe2 C15 40.6(3) . . ? C13 Fe2 C15 69.6(3) . . ? C55 Fe2 C15 116.1(3) . . ? C53 Fe2 C15 134.9(4) . . ? C51 Fe2 C15 148.0(3) . . ? C54 Fe2 C12 157.7(4) . . ? C14 Fe2 C12 69.8(3) . . ? C13 Fe2 C12 40.6(3) . . ? C55 Fe2 C12 158.9(4) . . ? C53 Fe2 C12 122.5(3) . . ? C51 Fe2 C12 123.0(3) . . ? C15 Fe2 C12 72.1(3) . . ? C54 Fe2 C52 66.1(3) . . ? C14 Fe2 C52 146.7(3) . . ? C13 Fe2 C52 115.6(3) . . ? C55 Fe2 C52 66.4(3) . . ? C53 Fe2 C52 38.6(3) . . ? C51 Fe2 C52 38.1(3) . . ? C15 Fe2 C52 172.6(3) . . ? C12 Fe2 C52 108.2(3) . . ? C54 Fe2 P2 117.9(3) . . ? C14 Fe2 P2 76.2(2) . . ? C13 Fe2 P2 76.3(2) . . ? C55 Fe2 P2 152.6(3) . . ? C53 Fe2 P2 108.5(3) . . ? C51 Fe2 P2 164.4(2) . . ? C15 Fe2 P2 46.7(2) . . ? C12 Fe2 P2 47.0(2) . . ? C52 Fe2 P2 128.0(2) . . ? C5 P1 C2 88.8(5) . . ? C5 P1 Fe1 61.4(3) . . ? C2 P1 Fe1 61.3(3) . . ? C15 P2 C12 87.6(5) . . ? C15 P2 Fe2 58.9(3) . . ? C12 P2 Fe2 59.3(3) . . ? C10 P3 C7 92.0(3) . . ? C10 P3 C11 102.1(3) . . ? C7 P3 C11 96.5(3) . . ? C17 P4 C20 91.1(4) . . ? C17 P4 C16 105.1(4) . . ? C20 P4 C16 96.1(4) . . ? C10 Si1 C29 113.1(3) . . ? C10 Si1 C31 111.8(4) . . ? C29 Si1 C31 109.4(4) . . ? C10 Si1 C30 104.6(3) . . ? C29 Si1 C30 109.1(4) . . ? C31 Si1 C30 108.6(4) . . ? C35 Si2 C17 104.5(4) . . ? C35 Si2 C36 109.3(5) . . ? C17 Si2 C36 113.6(4) . . ? C35 Si2 C37 108.2(4) . . ? C17 Si2 C37 111.7(4) . . ? C36 Si2 C37 109.3(4) . . ? O1 C1 C2 119.9(7) . . ? O1 C1 C20 120.0(7) . . ? C2 C1 C20 119.5(7) . . ? C3 C2 C1 131.5(7) . . ? C3 C2 P1 112.8(5) . . ? C1 C2 P1 115.6(6) . . ? C3 C2 Fe1 68.1(4) . . ? C1 C2 Fe1 129.6(6) . . ? P1 C2 Fe1 70.1(3) . . ? C4 C3 C2 113.0(5) . . ? C4 C3 C21 122.6(5) . . ? C2 C3 C21 124.4(7) . . ? C4 C3 Fe1 70.9(3) . . ? C2 C3 Fe1 70.9(4) . . ? C21 C3 Fe1 127.0(6) . . ? C3 C4 C5 110.9(5) . . ? C3 C4 C22 123.1(5) . . ? C5 C4 C22 126.0(7) . . ? C3 C4 Fe1 69.3(3) . . ? C5 C4 Fe1 70.1(4) . . ? C22 C4 Fe1 127.1(6) . . ? C4 C5 C6 129.1(7) . . ? C4 C5 P1 114.4(5) . . ? C6 C5 P1 116.5(6) . . ? C4 C5 Fe1 69.0(4) . . ? C6 C5 Fe1 129.4(6) . . ? P1 C5 Fe1 70.4(3) . . ? O2 C6 C7 121.6(6) . . ? O2 C6 C5 119.0(6) . . ? C7 C6 C5 118.6(7) . . ? C8 C7 C6 124.6(7) . . ? C8 C7 P3 108.7(6) . . ? C6 C7 P3 126.6(5) . . ? C7 C8 C9 114.3(7) . . ? C7 C8 C23 125.9(7) . . ? C9 C8 C23 119.7(6) . . ? C10 C9 C8 116.3(7) . . ? C10 C9 C24 125.1(7) . . ? C8 C9 C24 118.6(7) . . ? C9 C10 P3 108.3(6) . . ? C9 C10 Si1 131.9(6) . . ? P3 C10 Si1 119.4(4) . . ? O3 C11 C12 121.6(7) . . ? O3 C11 P3 123.6(5) . . ? C12 C11 P3 114.6(5) . . ? C13 C12 C11 122.8(7) . . ? C13 C12 P2 115.2(5) . . ? C11 C12 P2 122.0(6) . . ? C13 C12 Fe2 68.6(4) . . ? C11 C12 Fe2 129.2(5) . . ? P2 C12 Fe2 73.7(3) . . ? C14 C13 C12 110.5(5) . . ? C14 C13 C25 124.6(5) . . ? C12 C13 C25 124.3(6) . . ? C14 C13 Fe2 69.1(3) . . ? C12 C13 Fe2 70.8(5) . . ? C25 C13 Fe2 133.9(5) . . ? C13 C14 C15 110.7(5) . . ? C13 C14 C26 123.6(5) . . ? C15 C14 C26 124.9(6) . . ? C13 C14 Fe2 69.9(3) . . ? C15 C14 Fe2 70.7(5) . . ? C26 C14 Fe2 134.3(5) . . ? C14 C15 C16 122.4(6) . . ? C14 C15 P2 116.0(5) . . ? C16 C15 P2 121.5(6) . . ? C14 C15 Fe2 68.8(4) . . ? C16 C15 Fe2 128.0(5) . . ? P2 C15 Fe2 74.4(3) . . ? O4 C16 C15 123.1(7) . . ? O4 C16 P4 121.9(6) . . ? C15 C16 P4 114.9(5) . . ? C18 C17 P4 109.6(6) . . ? C18 C17 Si2 129.4(6) . . ? P4 C17 Si2 120.6(4) . . ? C17 C18 C19 115.8(6) . . ? C17 C18 C27 126.2(7) . . ? C19 C18 C27 117.9(7) . . ? C20 C19 C18 112.8(7) . . ? C20 C19 C28 126.7(8) . . ? C18 C19 C28 120.5(6) . . ? C19 C20 C1 123.9(8) . . ? C19 C20 P4 110.1(6) . . ? C1 C20 P4 126.0(6) . . ? C3 C21 H21A 109.4 . . ? C3 C21 H21B 109.8 . . ? H21A C21 H21B 109.5 . . ? C3 C21 H21C 109.2 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C4 C22 H22A 109.1 . . ? C4 C22 H22B 109.9 . . ? H22A C22 H22B 109.5 . . ? C4 C22 H22C 109.4 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C8 C23 H23A 109.4 . . ? C8 C23 H23B 109.8 . . ? H23A C23 H23B 109.5 . . ? C8 C23 H23C 109.2 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C9 C24 H24A 109.2 . . ? C9 C24 H24B 109.6 . . ? H24A C24 H24B 109.5 . . ? C9 C24 H24C 109.6 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C13 C25 H25A 109.5 . . ? C13 C25 H25B 109.7 . . ? H25A C25 H25B 109.5 . . ? C13 C25 H25C 109.3 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C14 C26 H26A 109.6 . . ? C14 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C14 C26 H26C 109.3 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C18 C27 H27A 109.2 . . ? C18 C27 H27B 109.6 . . ? H27A C27 H27B 109.5 . . ? C18 C27 H27C 109.7 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C19 C28 H28A 109.2 . . ? C19 C28 H28B 109.8 . . ? H28A C28 H28B 109.5 . . ? C19 C28 H28C 109.4 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si1 C29 H29A 109.5 . . ? Si1 C29 H29B 109.6 . . ? H29A C29 H29B 109.5 . . ? Si1 C29 H29C 109.4 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si1 C30 H30A 109.6 . . ? Si1 C30 H30B 109.3 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C34 109.8(8) . . ? C33 C31 C32 108.7(8) . . ? C34 C31 C32 106.9(8) . . ? C33 C31 Si1 111.1(7) . . ? C34 C31 Si1 108.6(6) . . ? C32 C31 Si1 111.7(6) . . ? C31 C32 H32A 109.4 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.7 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.0 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.9 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.4 . . ? C31 C34 H34A 109.8 . . ? C31 C34 H34B 109.0 . . ? H34A C34 H34B 109.4 . . ? C31 C34 H34C 109.7 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.6 . . ? Si2 C35 H35B 109.3 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.6 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si2 C36 H36A 109.5 . . ? Si2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si2 C36 H36C 109.4 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 108.7(8) . . ? C38 C37 C40 107.5(9) . . ? C39 C37 C40 109.0(9) . . ? C38 C37 Si2 109.8(6) . . ? C39 C37 Si2 110.3(8) . . ? C40 C37 Si2 111.4(7) . . ? C37 C38 H38A 109.6 . . ? C37 C38 H38B 109.0 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.8 . . ? H38A C38 H38C 109.4 . . ? H38B C38 H38C 109.4 . . ? C37 C39 H39A 109.9 . . ? C37 C39 H39B 109.1 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.6 . . ? C37 C40 H40B 109.4 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.4 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C45 C41 C42 108.1(6) . . ? C45 C41 C46 124.9(9) . . ? C42 C41 C46 126.9(7) . . ? C45 C41 Fe1 70.7(5) . . ? C42 C41 Fe1 70.0(4) . . ? C46 C41 Fe1 128.0(6) . . ? C43 C42 C41 107.7(6) . . ? C43 C42 C47 127.4(9) . . ? C41 C42 C47 124.8(7) . . ? C43 C42 Fe1 70.4(5) . . ? C41 C42 Fe1 69.3(3) . . ? C47 C42 Fe1 127.0(6) . . ? C42 C43 C44 109.4(7) . . ? C42 C43 C48 124.0(8) . . ? C44 C43 C48 126.6(8) . . ? C42 C43 Fe1 69.9(5) . . ? C44 C43 Fe1 70.9(5) . . ? C48 C43 Fe1 126.8(6) . . ? C45 C44 C43 103.8(10) . . ? C45 C44 C49 130.2(8) . . ? C43 C44 C49 126.0(7) . . ? C45 C44 Fe1 68.0(5) . . ? C43 C44 Fe1 68.2(5) . . ? C49 C44 Fe1 128.2(8) . . ? C41 C45 C44 110.9(7) . . ? C41 C45 C50 127.1(9) . . ? C44 C45 C50 121.9(10) . . ? C41 C45 Fe1 70.3(5) . . ? C44 C45 Fe1 71.5(5) . . ? C50 C45 Fe1 125.7(6) . . ? C41 C46 H46A 109.7 . . ? C41 C46 H46B 109.3 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.4 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C42 C47 H47A 109.6 . . ? C42 C47 H47B 109.2 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.7 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.4 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C44 C49 H49A 109.2 . . ? C44 C49 H49B 109.6 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.6 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C45 C50 H50A 109.4 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C55 110.2(6) . . ? C52 C51 C56 131.1(8) . . ? C55 C51 C56 118.5(7) . . ? C52 C51 Fe2 72.1(4) . . ? C55 C51 Fe2 69.9(3) . . ? C56 C51 Fe2 128.6(6) . . ? C53 C52 C51 108.0(7) . . ? C53 C52 C57 131.0(8) . . ? C51 C52 C57 120.6(8) . . ? C53 C52 Fe2 69.1(4) . . ? C51 C52 Fe2 69.8(4) . . ? C57 C52 Fe2 131.9(5) . . ? C52 C53 C54 109.8(7) . . ? C52 C53 C58 118.9(9) . . ? C54 C53 C58 131.3(9) . . ? C52 C53 Fe2 72.3(5) . . ? C54 C53 Fe2 69.6(4) . . ? C58 C53 Fe2 126.5(6) . . ? C53 C54 C55 107.2(6) . . ? C53 C54 C59 121.8(11) . . ? C55 C54 C59 130.6(11) . . ? C53 C54 Fe2 70.8(4) . . ? C55 C54 Fe2 70.5(5) . . ? C59 C54 Fe2 129.4(5) . . ? C51 C55 C54 104.8(6) . . ? C51 C55 C60 134.0(8) . . ? C54 C55 C60 121.1(10) . . ? C51 C55 Fe2 70.0(3) . . ? C54 C55 Fe2 68.5(4) . . ? C60 C55 Fe2 128.1(6) . . ? C51 C56 H56A 109.7 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.2 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.4 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C53 C58 H58A 109.7 . . ? C53 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C53 C58 H58C 109.3 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C54 C59 H59A 109.2 . . ? C54 C59 H59B 109.6 . . ? H59A C59 H59B 109.5 . . ? C54 C59 H59C 109.6 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C55 C60 H60A 109.2 . . ? C55 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C55 C60 H60C 109.7 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C103 Fe3 C102 41.4(4) . . ? C103 Fe3 C104 39.9(4) . . ? C102 Fe3 C104 67.7(3) . . ? C103 Fe3 C63 125.3(4) . . ? C102 Fe3 C63 165.6(3) . . ? C104 Fe3 C63 105.3(3) . . ? C103 Fe3 C101 68.0(3) . . ? C102 Fe3 C101 40.9(3) . . ? C104 Fe3 C101 65.8(3) . . ? C63 Fe3 C101 149.3(3) . . ? C103 Fe3 C64 105.7(3) . . ? C102 Fe3 C64 130.0(3) . . ? C104 Fe3 C64 114.1(3) . . ? C63 Fe3 C64 39.8(4) . . ? C101 Fe3 C64 170.8(3) . . ? C103 Fe3 C62 161.8(4) . . ? C102 Fe3 C62 154.1(3) . . ? C104 Fe3 C62 124.8(3) . . ? C63 Fe3 C62 40.1(3) . . ? C101 Fe3 C62 118.8(3) . . ? C64 Fe3 C62 69.3(3) . . ? C103 Fe3 C65 113.9(3) . . ? C102 Fe3 C65 108.5(3) . . ? C104 Fe3 C65 145.5(3) . . ? C63 Fe3 C65 69.6(3) . . ? C101 Fe3 C65 134.7(3) . . ? C64 Fe3 C65 40.5(3) . . ? C62 Fe3 C65 74.3(3) . . ? C103 Fe3 C105 66.5(3) . . ? C102 Fe3 C105 66.7(2) . . ? C104 Fe3 C105 39.0(3) . . ? C63 Fe3 C105 116.5(3) . . ? C101 Fe3 C105 38.1(3) . . ? C64 Fe3 C105 146.8(3) . . ? C62 Fe3 C105 107.5(2) . . ? C65 Fe3 C105 172.7(3) . . ? C103 Fe3 P5 149.7(3) . . ? C102 Fe3 P5 114.5(3) . . ? C104 Fe3 P5 166.6(2) . . ? C63 Fe3 P5 75.3(2) . . ? C101 Fe3 P5 106.6(2) . . ? C64 Fe3 P5 75.3(2) . . ? C62 Fe3 P5 47.72(19) . . ? C65 Fe3 P5 47.6(2) . . ? C105 Fe3 P5 128.4(2) . . ? C112 Fe4 C113 41.0(3) . . ? C112 Fe4 C74 107.3(4) . . ? C113 Fe4 C74 133.1(3) . . ? C112 Fe4 C73 110.6(4) . . ? C113 Fe4 C73 108.4(3) . . ? C74 Fe4 C73 40.1(3) . . ? C112 Fe4 C72 139.9(4) . . ? C113 Fe4 C72 110.9(3) . . ? C74 Fe4 C72 69.4(3) . . ? C73 Fe4 C72 40.8(3) . . ? C112 Fe4 C115 66.5(4) . . ? C113 Fe4 C115 66.5(3) . . ? C74 Fe4 C115 144.3(3) . . ? C73 Fe4 C115 174.8(3) . . ? C72 Fe4 C115 138.9(3) . . ? C112 Fe4 C111 39.8(4) . . ? C113 Fe4 C111 67.9(4) . . ? C74 Fe4 C111 112.1(3) . . ? C73 Fe4 C111 140.2(3) . . ? C72 Fe4 C111 178.5(3) . . ? C115 Fe4 C111 40.0(3) . . ? C112 Fe4 C114 67.2(4) . . ? C113 Fe4 C114 40.3(3) . . ? C74 Fe4 C114 173.4(4) . . ? C73 Fe4 C114 137.0(3) . . ? C72 Fe4 C114 112.0(3) . . ? C115 Fe4 C114 38.2(4) . . ? C111 Fe4 C114 66.5(3) . . ? C112 Fe4 C75 130.7(3) . . ? C113 Fe4 C75 171.0(4) . . ? C74 Fe4 C75 40.2(3) . . ? C73 Fe4 C75 69.7(3) . . ? C72 Fe4 C75 73.7(4) . . ? C115 Fe4 C75 115.5(3) . . ? C111 Fe4 C75 107.6(3) . . ? C114 Fe4 C75 146.2(4) . . ? C112 Fe4 P6 171.5(3) . . ? C113 Fe4 P6 140.2(3) . . ? C74 Fe4 P6 77.0(2) . . ? C73 Fe4 P6 77.5(2) . . ? C72 Fe4 P6 48.3(2) . . ? C115 Fe4 P6 105.6(3) . . ? C111 Fe4 P6 131.9(3) . . ? C114 Fe4 P6 108.9(3) . . ? C75 Fe4 P6 48.6(2) . . ? C65 P5 C62 89.5(4) . . ? C65 P5 Fe3 59.7(2) . . ? C62 P5 Fe3 59.3(2) . . ? C72 P6 C75 88.5(5) . . ? C72 P6 Fe4 60.5(3) . . ? C75 P6 Fe4 60.6(3) . . ? C67 P7 C70 92.1(3) . . ? C67 P7 C66 105.3(3) . . ? C70 P7 C66 94.3(3) . . ? C80 P8 C77 91.8(3) . . ? C80 P8 C61 103.2(3) . . ? C77 P8 C61 96.0(3) . . ? C90 Si3 C89 108.6(4) . . ? C90 Si3 C67 105.0(3) . . ? C89 Si3 C67 112.3(4) . . ? C90 Si3 C91 110.0(4) . . ? C89 Si3 C91 108.8(4) . . ? C67 Si3 C91 111.9(4) . . ? C95 Si4 C96 109.0(4) . . ? C95 Si4 C80 104.9(4) . . ? C96 Si4 C80 112.3(4) . . ? C95 Si4 C97 109.8(4) . . ? C96 Si4 C97 109.6(4) . . ? C80 Si4 C97 111.1(4) . . ? O5 C61 C62 125.9(7) . . ? O5 C61 P8 119.5(5) . . ? C62 C61 P8 114.5(5) . . ? C63 C62 C61 124.0(6) . . ? C63 C62 P5 112.3(5) . . ? C61 C62 P5 123.6(5) . . ? C63 C62 Fe3 68.6(4) . . ? C61 C62 Fe3 129.6(5) . . ? P5 C62 Fe3 73.0(2) . . ? C64 C63 C62 113.5(4) . . ? C64 C63 C81 123.6(5) . . ? C62 C63 C81 122.7(6) . . ? C64 C63 Fe3 70.8(3) . . ? C62 C63 Fe3 71.3(4) . . ? C81 C63 Fe3 129.8(6) . . ? C63 C64 C65 112.7(5) . . ? C63 C64 C82 124.4(5) . . ? C65 C64 C82 122.8(6) . . ? C63 C64 Fe3 69.4(3) . . ? C65 C64 Fe3 70.9(4) . . ? C82 C64 Fe3 129.8(6) . . ? C64 C65 C66 124.0(6) . . ? C64 C65 P5 111.8(5) . . ? C66 C65 P5 124.1(6) . . ? C64 C65 Fe3 68.7(4) . . ? C66 C65 Fe3 128.7(5) . . ? P5 C65 Fe3 72.6(3) . . ? O6 C66 C65 126.3(7) . . ? O6 C66 P7 120.5(5) . . ? C65 C66 P7 113.2(5) . . ? C68 C67 P7 109.7(6) . . ? C68 C67 Si3 129.6(6) . . ? P7 C67 Si3 120.6(4) . . ? C67 C68 C69 113.9(6) . . ? C67 C68 C83 125.7(8) . . ? C69 C68 C83 120.3(7) . . ? C70 C69 C68 114.6(7) . . ? C70 C69 C84 126.5(7) . . ? C68 C69 C84 118.9(6) . . ? C69 C70 C71 124.3(7) . . ? C69 C70 P7 109.3(6) . . ? C71 C70 P7 126.4(5) . . ? O7 C71 C70 120.2(6) . . ? O7 C71 C72 117.5(6) . . ? C70 C71 C72 122.0(6) . . ? C73 C72 C71 130.1(7) . . ? C73 C72 P6 114.2(5) . . ? C71 C72 P6 115.6(6) . . ? C73 C72 Fe4 69.5(4) . . ? C71 C72 Fe4 131.4(5) . . ? P6 C72 Fe4 71.2(3) . . ? C74 C73 C72 110.7(5) . . ? C74 C73 C85 124.0(5) . . ? C72 C73 C85 125.3(7) . . ? C74 C73 Fe4 69.5(3) . . ? C72 C73 Fe4 69.7(4) . . ? C85 C73 Fe4 126.0(5) . . ? C75 C74 C73 113.4(5) . . ? C75 C74 C86 123.8(6) . . ? C73 C74 C86 122.8(5) . . ? C75 C74 Fe4 70.8(4) . . ? C73 C74 Fe4 70.4(3) . . ? C86 C74 Fe4 126.5(5) . . ? C74 C75 C76 130.6(7) . . ? C74 C75 P6 113.2(5) . . ? C76 C75 P6 116.1(6) . . ? C74 C75 Fe4 69.0(4) . . ? C76 C75 Fe4 131.7(5) . . ? P6 C75 Fe4 70.8(3) . . ? O8 C76 C75 120.5(6) . . ? O8 C76 C77 118.8(6) . . ? C75 C76 C77 120.6(6) . . ? C78 C77 C76 126.2(7) . . ? C78 C77 P8 109.8(6) . . ? C76 C77 P8 123.9(5) . . ? C77 C78 C79 114.0(7) . . ? C77 C78 C87 126.2(7) . . ? C79 C78 C87 119.8(6) . . ? C80 C79 C78 115.5(6) . . ? C80 C79 C88 124.0(7) . . ? C78 C79 C88 120.5(7) . . ? C79 C80 P8 108.6(5) . . ? C79 C80 Si4 131.7(5) . . ? P8 C80 Si4 119.5(4) . . ? C63 C81 H81A 109.8 . . ? C63 C81 H81B 109.4 . . ? H81A C81 H81B 109.5 . . ? C63 C81 H81C 109.3 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C64 C82 H82A 109.3 . . ? C64 C82 H82B 109.4 . . ? H82A C82 H82B 109.5 . . ? C64 C82 H82C 109.7 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C68 C83 H83A 109.7 . . ? C68 C83 H83B 109.4 . . ? H83A C83 H83B 109.5 . . ? C68 C83 H83C 109.2 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C69 C84 H84A 109.7 . . ? C69 C84 H84B 109.1 . . ? H84A C84 H84B 109.5 . . ? C69 C84 H84C 109.6 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C73 C85 H85A 109.5 . . ? C73 C85 H85B 109.1 . . ? H85A C85 H85B 109.5 . . ? C73 C85 H85C 109.8 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C74 C86 H86A 109.1 . . ? C74 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C74 C86 H86C 109.8 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C78 C87 H87A 109.6 . . ? C78 C87 H87B 109.1 . . ? H87A C87 H87B 109.5 . . ? C78 C87 H87C 109.7 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C79 C88 H88A 109.7 . . ? C79 C88 H88B 109.3 . . ? H88A C88 H88B 109.5 . . ? C79 C88 H88C 109.4 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? Si3 C89 H89A 109.5 . . ? Si3 C89 H89B 109.4 . . ? H89A C89 H89B 109.5 . . ? Si3 C89 H89C 109.6 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? Si3 C90 H90A 109.4 . . ? Si3 C90 H90B 109.6 . . ? H90A C90 H90B 109.5 . . ? Si3 C90 H90C 109.4 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C93 C91 C94 110.6(8) . . ? C93 C91 C92 108.3(7) . . ? C94 C91 C92 108.5(7) . . ? C93 C91 Si3 110.9(6) . . ? C94 C91 Si3 110.8(5) . . ? C92 C91 Si3 107.6(6) . . ? C91 C92 H92A 109.8 . . ? C91 C92 H92B 109.4 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.3 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C91 C93 H93A 109.5 . . ? C91 C93 H93B 109.3 . . ? H93A C93 H93B 109.5 . . ? C91 C93 H93C 109.6 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C91 C94 H94A 109.4 . . ? C91 C94 H94B 109.9 . . ? H94A C94 H94B 109.5 . . ? C91 C94 H94C 109.2 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.4 . . ? Si4 C95 H95A 109.4 . . ? Si4 C95 H95B 109.6 . . ? H95A C95 H95B 109.5 . . ? Si4 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? Si4 C96 H96A 109.5 . . ? Si4 C96 H96B 109.4 . . ? H96A C96 H96B 109.5 . . ? Si4 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C100 C97 C98 111.4(8) . . ? C100 C97 C99 107.1(7) . . ? C98 C97 C99 109.8(7) . . ? C100 C97 Si4 110.2(6) . . ? C98 C97 Si4 110.2(6) . . ? C99 C97 Si4 108.0(6) . . ? C97 C98 H98A 109.4 . . ? C97 C98 H98B 109.2 . . ? H98A C98 H98B 109.4 . . ? C97 C98 H98C 109.9 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.4 . . ? C97 C99 H99A 109.2 . . ? C97 C99 H99B 109.3 . . ? H99A C99 H99B 109.5 . . ? C97 C99 H99C 109.9 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C97 C100 H10A 109.6 . . ? C97 C100 H10B 109.3 . . ? H10A C100 H10B 109.5 . . ? C97 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C105 C101 C102 109.0(6) . . ? C105 C101 C106 130.0(7) . . ? C102 C101 C106 120.8(6) . . ? C105 C101 Fe3 71.9(5) . . ? C102 C101 Fe3 69.1(3) . . ? C106 C101 Fe3 128.7(5) . . ? C101 C102 C103 104.9(6) . . ? C101 C102 C107 130.4(8) . . ? C103 C102 C107 124.6(8) . . ? C101 C102 Fe3 70.0(3) . . ? C103 C102 Fe3 68.1(5) . . ? C107 C102 Fe3 129.8(5) . . ? C104 C103 C102 107.8(6) . . ? C104 C103 C108 123.2(9) . . ? C102 C103 C108 128.9(8) . . ? C104 C103 Fe3 71.3(4) . . ? C102 C103 Fe3 70.4(4) . . ? C108 C103 Fe3 126.2(6) . . ? C105 C104 C103 108.7(7) . . ? C105 C104 C109 123.9(7) . . ? C103 C104 C109 127.3(7) . . ? C105 C104 Fe3 71.8(5) . . ? C103 C104 Fe3 68.8(3) . . ? C109 C104 Fe3 128.5(6) . . ? C101 C105 C104 109.5(6) . . ? C101 C105 C110 122.1(7) . . ? C104 C105 C110 128.0(7) . . ? C101 C105 Fe3 70.0(4) . . ? C104 C105 Fe3 69.2(4) . . ? C110 C105 Fe3 132.0(4) . . ? C101 C106 H10D 109.7 . . ? C101 C106 H10E 109.3 . . ? H10D C106 H10E 109.5 . . ? C101 C106 H10F 109.4 . . ? H10D C106 H10F 109.5 . . ? H10E C106 H10F 109.5 . . ? C102 C107 H10G 109.3 . . ? C102 C107 H10H 109.4 . . ? H10G C107 H10H 109.5 . . ? C102 C107 H10I 109.8 . . ? H10G C107 H10I 109.5 . . ? H10H C107 H10I 109.5 . . ? C103 C108 H10J 109.8 . . ? C103 C108 H10K 109.4 . . ? H10J C108 H10K 109.5 . . ? C103 C108 H10L 109.3 . . ? H10J C108 H10L 109.5 . . ? H10K C108 H10L 109.5 . . ? C104 C109 H10M 109.7 . . ? C104 C109 H10N 109.4 . . ? H10M C109 H10N 109.5 . . ? C104 C109 H10O 109.3 . . ? H10M C109 H10O 109.5 . . ? H10N C109 H10O 109.5 . . ? C105 C110 H11A 109.4 . . ? C105 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? C105 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? C112 C111 C115 106.6(8) . . ? C112 C111 C116 126.1(9) . . ? C115 C111 C116 127.2(8) . . ? C112 C111 Fe4 69.1(6) . . ? C115 C111 Fe4 70.3(5) . . ? C116 C111 Fe4 128.7(6) . . ? C111 C112 C113 108.7(11) . . ? C111 C112 C117 126.0(7) . . ? C113 C112 C117 124.9(8) . . ? C111 C112 Fe4 71.0(6) . . ? C113 C112 Fe4 70.1(6) . . ? C117 C112 Fe4 130.5(9) . . ? C114 C113 C112 105.7(8) . . ? C114 C113 C118 128.9(8) . . ? C112 C113 C118 125.1(9) . . ? C114 C113 Fe4 70.5(5) . . ? C112 C113 Fe4 68.9(6) . . ? C118 C113 Fe4 129.0(5) . . ? C115 C114 C113 109.0(6) . . ? C115 C114 C119 125.9(7) . . ? C113 C114 C119 125.1(8) . . ? C115 C114 Fe4 70.8(3) . . ? C113 C114 Fe4 69.2(4) . . ? C119 C114 Fe4 127.2(6) . . ? C114 C115 C111 110.0(6) . . ? C114 C115 C120 126.0(6) . . ? C111 C115 C120 124.0(7) . . ? C114 C115 Fe4 71.0(3) . . ? C111 C115 Fe4 69.8(4) . . ? C120 C115 Fe4 127.2(6) . . ? C111 C116 H11D 109.4 . . ? C111 C116 H11E 109.5 . . ? H11D C116 H11E 109.5 . . ? C111 C116 H11F 109.5 . . ? H11D C116 H11F 109.5 . . ? H11E C116 H11F 109.5 . . ? C112 C117 H11G 109.6 . . ? C112 C117 H11H 109.4 . . ? H11G C117 H11H 109.5 . . ? C112 C117 H11I 109.4 . . ? H11G C117 H11I 109.5 . . ? H11H C117 H11I 109.5 . . ? C113 C118 H11J 109.5 . . ? C113 C118 H11K 109.5 . . ? H11J C118 H11K 109.5 . . ? C113 C118 H11L 109.4 . . ? H11J C118 H11L 109.5 . . ? H11K C118 H11L 109.5 . . ? C114 C119 H11M 109.7 . . ? C114 C119 H11N 109.4 . . ? H11M C119 H11N 109.5 . . ? C114 C119 H11O 109.3 . . ? H11M C119 H11O 109.5 . . ? H11N C119 H11O 109.5 . . ? C115 C120 H12A 109.3 . . ? C115 C120 H12B 109.4 . . ? H12A C120 H12B 109.5 . . ? C115 C120 H12C 109.8 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.164 _refine_diff_density_min -0.115 _refine_diff_density_rms 0.024 #===END # compound 10 data_em485 _database_code_depnum_ccdc_archive 'CCDC 830882' #TrackingRef '2011_duncan_chem_commun.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H54 Fe2 O4 P4, 2(C16 H30 K N2 O6), 2(C2 H3 N)' _chemical_formula_sum 'C84 H120 Fe2 K2 N6 O16 P4' _chemical_formula_weight 1783.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 '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 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.995(1) _cell_length_b 14.050(1) _cell_length_c 14.447(1) _cell_angle_alpha 108.305(1) _cell_angle_beta 106.230(1) _cell_angle_gamma 109.092(1) _cell_volume 2305.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 7960 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8137 _exptl_absorpt_correction_T_max 0.8728 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28523 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 29.97 _reflns_number_total 13331 _reflns_number_gt 10339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0498P)^2^+0.1565P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13331 _refine_ls_number_parameters 526 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Fe1 Fe 0.654892(14) 0.356004(15) 0.271820(13) 0.02202(6) Uani 1 1 d . . . P1 P 0.53005(3) 0.18241(3) 0.13064(3) 0.02419(8) Uani 1 1 d . . . P2 P 0.51548(3) 0.05990(3) -0.09513(3) 0.02353(8) Uani 1 1 d . . . O1 O 0.61677(11) 0.16148(9) 0.40201(8) 0.0471(3) Uani 1 1 d . . . O2 O 0.69390(10) 0.39102(9) 0.03719(8) 0.0430(3) Uani 1 1 d . . . C1 C 0.58972(11) 0.11802(12) 0.30371(10) 0.0277(3) Uani 1 1 d . . . C2 C 0.62224(11) 0.19023(11) 0.24879(10) 0.0246(3) Uani 1 1 d . . . C3 C 0.73697(11) 0.25942(11) 0.27868(10) 0.0263(3) Uani 1 1 d . . . C4 C 0.75145(11) 0.30458(11) 0.20460(11) 0.0267(3) Uani 1 1 d . . . C5 C 0.64679(11) 0.26983(11) 0.11938(10) 0.0248(3) Uani 1 1 d . . . C6 C 0.63910(11) 0.29440(11) 0.02354(11) 0.0278(3) Uani 1 1 d . . . C7 C 0.57252(10) 0.19701(11) -0.08225(10) 0.0233(2) Uani 1 1 d . . . C8 C 0.55319(11) 0.19740(11) -0.18503(10) 0.0247(3) Uani 1 1 d . . . C9 C 0.49466(10) 0.08996(11) -0.27018(10) 0.0241(3) Uani 1 1 d . . . C10 C 0.53220(10) -0.00315(11) 0.23542(10) 0.0227(2) Uani 1 1 d . . . C11 C 0.83226(13) 0.27464(14) 0.37202(13) 0.0409(4) Uani 1 1 d . . . H11A H 0.8085 0.2702 0.4289 0.061 Uiso 1 1 calc R . . H11B H 0.8959 0.3484 0.4003 0.061 Uiso 1 1 calc R . . H11C H 0.8544 0.2153 0.3476 0.061 Uiso 1 1 calc R . . C12 C 0.86476(12) 0.37108(14) 0.21152(14) 0.0393(4) Uani 1 1 d . . . H12A H 0.8953 0.3198 0.1859 0.059 Uiso 1 1 calc R . . H12B H 0.9153 0.4263 0.2865 0.059 Uiso 1 1 calc R . . H12C H 0.8573 0.4103 0.1666 0.059 Uiso 1 1 calc R . . C13 C 0.58967(15) 0.30522(13) -0.19734(12) 0.0381(4) Uani 1 1 d . . . H13A H 0.6707 0.3400 -0.1743 0.057 Uiso 1 1 calc R . . H13B H 0.5701 0.3573 -0.1526 0.057 Uiso 1 1 calc R . . H13C H 0.5517 0.2880 -0.2730 0.057 Uiso 1 1 calc R . . C14 C 0.45886(13) 0.06428(13) -0.38756(11) 0.0344(3) Uani 1 1 d . . . H14A H 0.4830 0.1349 -0.3938 0.052 Uiso 1 1 calc R . . H14B H 0.3773 0.0212 -0.4260 0.052 Uiso 1 1 calc R . . H14C H 0.4930 0.0201 -0.4191 0.052 Uiso 1 1 calc R . . C15 C 0.63159(12) 0.43498(12) 0.40617(11) 0.0305(3) Uani 1 1 d . . . C16 C 0.74062(12) 0.49944(12) 0.41742(10) 0.0290(3) Uani 1 1 d . . . C17 C 0.72881(12) 0.52782(12) 0.32929(11) 0.0302(3) Uani 1 1 d . . . C18 C 0.61215(13) 0.48026(13) 0.26320(11) 0.0333(3) Uani 1 1 d . . . C19 C 0.55239(12) 0.42307(13) 0.31040(12) 0.0349(3) Uani 1 1 d . . . C20 C 0.60437(15) 0.39457(15) 0.48449(13) 0.0430(4) Uani 1 1 d . . . H20A H 0.6717 0.4000 0.5350 0.064 Uiso 1 1 calc R . . H20B H 0.5466 0.3160 0.4451 0.064 Uiso 1 1 calc R . . H20C H 0.5770 0.4412 0.5245 0.064 Uiso 1 1 calc R . . C21 C 0.84886(13) 0.53589(13) 0.50918(12) 0.0393(4) Uani 1 1 d . . . H21A H 0.9078 0.5438 0.4839 0.059 Uiso 1 1 calc R . . H21B H 0.8402 0.4793 0.5364 0.059 Uiso 1 1 calc R . . H21C H 0.8691 0.6083 0.5671 0.059 Uiso 1 1 calc R . . C22 C 0.82074(14) 0.59784(13) 0.30989(13) 0.0416(4) Uani 1 1 d . . . H22A H 0.8288 0.6746 0.3340 0.062 Uiso 1 1 calc R . . H22B H 0.8025 0.5650 0.2328 0.062 Uiso 1 1 calc R . . H22C H 0.8910 0.5997 0.3502 0.062 Uiso 1 1 calc R . . C23 C 0.56147(17) 0.49326(17) 0.16451(14) 0.0521(5) Uani 1 1 d . . . H23A H 0.4910 0.4255 0.1135 0.078 Uiso 1 1 calc R . . H23B H 0.6132 0.5040 0.1306 0.078 Uiso 1 1 calc R . . H23C H 0.5470 0.5588 0.1849 0.078 Uiso 1 1 calc R . . C24 C 0.42721(14) 0.36513(18) 0.27002(15) 0.0531(5) Uani 1 1 d . . . H24A H 0.4013 0.4211 0.2948 0.080 Uiso 1 1 calc R . . H24B H 0.4066 0.3100 0.2979 0.080 Uiso 1 1 calc R . . H24C H 0.3923 0.3266 0.1911 0.080 Uiso 1 1 calc R . . K1 K 0.00401(2) 0.89241(3) 0.22413(2) 0.03087(7) Uani 1 1 d . . . O3 O 0.16776(8) 0.85459(9) 0.16713(8) 0.0336(2) Uani 1 1 d . . . O4 O -0.05526(8) 0.69371(8) 0.04803(8) 0.0311(2) Uani 1 1 d . . . O5 O -0.21359(8) 0.72148(9) 0.12812(8) 0.0324(2) Uani 1 1 d . . . O6 O -0.16073(8) 0.93620(9) 0.27436(8) 0.0317(2) Uani 1 1 d . . . O7 O 0.07056(8) 1.08606(9) 0.41082(8) 0.0342(2) Uani 1 1 d . . . O8 O 0.22353(8) 1.07233(9) 0.31982(8) 0.0363(2) Uani 1 1 d . . . N1 N -0.09629(15) 0.96983(17) 0.07421(16) 0.0661(5) Uani 1 1 d . . . N2 N 0.09204(15) 0.81001(17) 0.36970(14) 0.0596(4) Uani 1 1 d . . . C25 C 0.12998(13) 0.76632(14) 0.06387(12) 0.0386(3) Uani 1 1 d . . . H25A H 0.1912 0.7475 0.0589 0.046 Uiso 1 1 calc R . . H25B H 0.1063 0.7902 0.0075 0.046 Uiso 1 1 calc R . . C26 C 0.03370(13) 0.66567(14) 0.04736(13) 0.0380(3) Uani 1 1 d . . . H26A H 0.0091 0.6014 -0.0223 0.046 Uiso 1 1 calc R . . H26B H 0.0563 0.6439 0.1057 0.046 Uiso 1 1 calc R . . C27 C -0.15044(12) 0.60159(13) 0.03326(13) 0.0360(3) Uani 1 1 d . . . H27A H -0.1313 0.5829 0.0944 0.043 Uiso 1 1 calc R . . H27B H -0.1741 0.5345 -0.0338 0.043 Uiso 1 1 calc R . . C28 C -0.24363(12) 0.63348(13) 0.02659(12) 0.0359(3) Uani 1 1 d . . . H28A H -0.2578 0.6591 -0.0301 0.043 Uiso 1 1 calc R . . H28B H -0.3129 0.5673 0.0074 0.043 Uiso 1 1 calc R . . C29 C -0.29691(12) 0.75894(13) 0.12701(13) 0.0360(3) Uani 1 1 d . . . H29A H -0.3702 0.6940 0.1005 0.043 Uiso 1 1 calc R . . H29B H -0.3034 0.7950 0.0782 0.043 Uiso 1 1 calc R . . C30 C -0.26450(12) 0.84137(14) 0.23872(13) 0.0377(3) Uani 1 1 d . . . H30A H -0.3230 0.8660 0.2399 0.045 Uiso 1 1 calc R . . H30B H -0.2571 0.8055 0.2876 0.045 Uiso 1 1 calc R . . C31 C -0.12142(13) 1.01544(14) 0.38263(12) 0.0384(3) Uani 1 1 d . . . H31A H -0.1049 0.9811 0.4315 0.046 Uiso 1 1 calc R . . H31B H -0.1794 1.0384 0.3912 0.046 Uiso 1 1 calc R . . C32 C -0.01767(13) 1.11617(14) 0.41069(13) 0.0395(4) Uani 1 1 d . . . H32A H -0.0328 1.1461 0.3576 0.047 Uiso 1 1 calc R . . H32B H 0.0051 1.1759 0.4828 0.047 Uiso 1 1 calc R . . C33 C 0.17131(13) 1.18020(14) 0.43910(13) 0.0415(4) Uani 1 1 d . . . H33A H 0.1981 1.2370 0.5138 0.050 Uiso 1 1 calc R . . H33B H 0.1575 1.2153 0.3904 0.050 Uiso 1 1 calc R . . C34 C 0.25770(13) 1.14237(15) 0.43012(13) 0.0419(4) Uani 1 1 d . . . H34A H 0.3307 1.2084 0.4585 0.050 Uiso 1 1 calc R . . H34B H 0.2659 1.1001 0.4727 0.050 Uiso 1 1 calc R . . C35 C 0.30483(12) 1.03691(15) 0.30374(14) 0.0441(4) Uani 1 1 d . . . H35A H 0.3230 1.0010 0.3506 0.053 Uiso 1 1 calc R . . H35B H 0.3743 1.1027 0.3226 0.053 Uiso 1 1 calc R . . C36 C 0.25799(13) 0.95485(15) 0.18804(14) 0.0417(4) Uani 1 1 d . . . H36A H 0.2312 0.9876 0.1410 0.050 Uiso 1 1 calc R . . H36B H 0.3167 0.9376 0.1727 0.050 Uiso 1 1 calc R . . C37 C -0.15965(13) 1.00179(15) 0.08233(13) 0.0390(4) Uani 1 1 d . . . C38 C -0.23993(13) 1.04294(15) 0.09367(14) 0.0418(4) Uani 1 1 d . . . H38A H -0.3070 1.0024 0.0252 0.063 Uiso 1 1 calc R . . H38B H -0.2070 1.1236 0.1134 0.063 Uiso 1 1 calc R . . H38C H -0.2602 1.0307 0.1501 0.063 Uiso 1 1 calc R . . C39 C 0.15570(16) 0.77904(16) 0.36053(13) 0.0457(4) Uani 1 1 d . . . C40 C 0.23954(18) 0.7417(2) 0.34755(14) 0.0615(6) Uani 1 1 d . . . H40A H 0.2064 0.6596 0.3187 0.092 Uiso 1 1 calc R . . H40B H 0.3033 0.7763 0.4177 0.092 Uiso 1 1 calc R . . H40C H 0.2649 0.7643 0.2976 0.092 Uiso 1 1 calc R . . N3 N 0.1585(2) 0.4423(2) 0.22787(16) 0.0927(7) Uani 1 1 d . . . C41 C 0.14392(17) 0.3528(3) 0.20009(17) 0.0631(6) Uani 1 1 d . . . C42 C 0.12574(19) 0.2383(2) 0.1633(2) 0.0821(8) Uani 1 1 d . . . H42A H 0.1166 0.2084 0.0886 0.123 Uiso 1 1 calc R . . H42B H 0.0582 0.1931 0.1672 0.123 Uiso 1 1 calc R . . H42C H 0.1901 0.2352 0.2089 0.123 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02097(9) 0.01973(10) 0.01805(9) 0.00310(7) 0.00537(7) 0.00877(7) P1 0.02200(16) 0.02239(17) 0.01777(15) 0.00437(13) 0.00545(12) 0.00555(13) P2 0.02671(16) 0.01975(17) 0.01802(15) 0.00520(13) 0.00934(13) 0.00709(13) O1 0.0740(8) 0.0302(6) 0.0186(5) 0.0056(4) 0.0127(5) 0.0144(6) O2 0.0584(7) 0.0221(5) 0.0319(5) 0.0084(5) 0.0190(5) 0.0039(5) C1 0.0296(7) 0.0252(7) 0.0204(6) 0.0062(5) 0.0068(5) 0.0106(6) C2 0.0264(6) 0.0201(6) 0.0189(6) 0.0033(5) 0.0069(5) 0.0086(5) C3 0.0240(6) 0.0210(6) 0.0254(6) 0.0034(5) 0.0063(5) 0.0111(5) C4 0.0240(6) 0.0199(6) 0.0289(6) 0.0036(5) 0.0116(5) 0.0086(5) C5 0.0279(6) 0.0190(6) 0.0208(6) 0.0035(5) 0.0109(5) 0.0081(5) C6 0.0311(7) 0.0209(7) 0.0262(6) 0.0060(5) 0.0142(6) 0.0090(6) C7 0.0226(6) 0.0211(6) 0.0226(6) 0.0066(5) 0.0100(5) 0.0085(5) C8 0.0254(6) 0.0249(7) 0.0257(6) 0.0105(5) 0.0126(5) 0.0129(5) C9 0.0235(6) 0.0276(7) 0.0221(6) 0.0103(5) 0.0099(5) 0.0131(5) C10 0.0207(6) 0.0233(6) 0.0201(6) 0.0068(5) 0.0079(5) 0.0092(5) C11 0.0321(7) 0.0367(9) 0.0419(9) 0.0111(7) 0.0030(7) 0.0193(7) C12 0.0282(7) 0.0328(9) 0.0462(9) 0.0088(7) 0.0181(7) 0.0085(6) C13 0.0566(10) 0.0282(8) 0.0320(7) 0.0157(6) 0.0205(7) 0.0188(7) C14 0.0426(8) 0.0364(8) 0.0243(7) 0.0144(6) 0.0133(6) 0.0181(7) C15 0.0351(7) 0.0293(8) 0.0261(6) 0.0062(6) 0.0151(6) 0.0178(6) C16 0.0343(7) 0.0220(7) 0.0189(6) 0.0007(5) 0.0063(5) 0.0123(6) C17 0.0373(7) 0.0203(7) 0.0261(6) 0.0042(5) 0.0114(6) 0.0133(6) C18 0.0423(8) 0.0312(8) 0.0270(7) 0.0079(6) 0.0111(6) 0.0252(7) C19 0.0342(7) 0.0360(8) 0.0317(7) 0.0066(6) 0.0129(6) 0.0220(7) C20 0.0533(10) 0.0439(10) 0.0346(8) 0.0137(7) 0.0263(8) 0.0226(8) C21 0.0364(8) 0.0320(8) 0.0257(7) 0.0023(6) 0.0012(6) 0.0096(7) C22 0.0538(10) 0.0234(8) 0.0382(8) 0.0094(7) 0.0204(7) 0.0107(7) C23 0.0660(12) 0.0605(12) 0.0400(9) 0.0243(9) 0.0151(8) 0.0446(10) C24 0.0356(9) 0.0675(13) 0.0498(10) 0.0123(9) 0.0171(8) 0.0303(9) K1 0.02402(14) 0.03039(17) 0.03275(16) 0.00772(13) 0.01117(12) 0.01324(13) O3 0.0272(5) 0.0373(6) 0.0308(5) 0.0090(5) 0.0149(4) 0.0123(5) O4 0.0292(5) 0.0271(5) 0.0337(5) 0.0105(4) 0.0140(4) 0.0116(4) O5 0.0273(5) 0.0323(6) 0.0334(5) 0.0123(4) 0.0105(4) 0.0131(4) O6 0.0282(5) 0.0360(6) 0.0323(5) 0.0134(5) 0.0155(4) 0.0157(4) O7 0.0326(5) 0.0343(6) 0.0356(5) 0.0119(5) 0.0138(4) 0.0194(5) O8 0.0276(5) 0.0387(6) 0.0354(5) 0.0089(5) 0.0119(4) 0.0158(5) N1 0.0741(11) 0.0952(15) 0.0889(13) 0.0686(12) 0.0564(11) 0.0602(12) N2 0.0718(11) 0.0789(13) 0.0570(10) 0.0407(10) 0.0381(9) 0.0475(11) C25 0.0349(8) 0.0454(10) 0.0324(7) 0.0089(7) 0.0186(6) 0.0194(7) C26 0.0394(8) 0.0352(9) 0.0356(8) 0.0077(7) 0.0158(7) 0.0208(7) C27 0.0367(8) 0.0249(7) 0.0374(8) 0.0099(6) 0.0151(6) 0.0084(6) C28 0.0315(7) 0.0296(8) 0.0342(7) 0.0110(6) 0.0099(6) 0.0069(6) C29 0.0237(7) 0.0352(9) 0.0469(9) 0.0195(7) 0.0130(6) 0.0118(6) C30 0.0297(7) 0.0427(9) 0.0486(9) 0.0227(8) 0.0225(7) 0.0181(7) C31 0.0407(8) 0.0458(10) 0.0345(8) 0.0139(7) 0.0209(7) 0.0258(8) C32 0.0414(8) 0.0400(9) 0.0390(8) 0.0099(7) 0.0184(7) 0.0269(8) C33 0.0381(8) 0.0322(9) 0.0402(8) 0.0045(7) 0.0144(7) 0.0136(7) C34 0.0316(8) 0.0407(9) 0.0353(8) 0.0044(7) 0.0084(6) 0.0134(7) C35 0.0232(7) 0.0424(10) 0.0523(10) 0.0080(8) 0.0149(7) 0.0124(7) C36 0.0292(7) 0.0439(10) 0.0481(9) 0.0134(8) 0.0231(7) 0.0135(7) C37 0.0396(8) 0.0425(9) 0.0435(9) 0.0256(8) 0.0210(7) 0.0193(7) C38 0.0362(8) 0.0413(10) 0.0443(9) 0.0160(8) 0.0143(7) 0.0189(7) C39 0.0594(11) 0.0523(11) 0.0308(8) 0.0202(8) 0.0179(8) 0.0310(9) C40 0.0720(13) 0.0803(15) 0.0329(9) 0.0167(9) 0.0123(9) 0.0522(12) N3 0.0918(16) 0.103(2) 0.0488(11) 0.0077(12) 0.0202(11) 0.0394(16) C41 0.0449(11) 0.0876(19) 0.0387(10) 0.0236(12) 0.0137(9) 0.0181(12) C42 0.0555(13) 0.097(2) 0.0697(15) 0.0484(16) 0.0125(11) 0.0097(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 Fe1 C18 2.0493(14) . ? Fe1 C3 2.0522(13) . ? Fe1 C17 2.0528(14) . ? Fe1 C4 2.0549(14) . ? Fe1 C19 2.0634(15) . ? Fe1 C16 2.0664(13) . ? Fe1 C15 2.0838(14) . ? Fe1 C5 2.1034(13) . ? Fe1 C2 2.1158(13) . ? Fe1 P1 2.2928(4) . ? P1 C2 1.7745(13) . ? P1 C5 1.7793(13) . ? P2 C7 1.7518(13) . ? P2 C10 1.7521(13) 2_655 ? O1 C1 1.2396(16) . ? O2 C6 1.2395(16) . ? C1 C10 1.4575(19) . ? C1 C2 1.5071(18) . ? C2 C3 1.4274(18) . ? C3 C4 1.4327(19) . ? C3 C11 1.5066(18) . ? C4 C5 1.4304(18) . ? C4 C12 1.5104(19) . ? C5 C6 1.5130(18) . ? C6 C7 1.4604(18) . ? C7 C8 1.4352(17) . ? C8 C9 1.3872(19) . ? C8 C13 1.5170(19) . ? C9 C10 1.4391(17) 2_655 ? C9 C14 1.5098(18) . ? C10 C9 1.4391(17) 2_655 ? C10 P2 1.7521(13) 2_655 ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.428(2) . ? C15 C19 1.4306(19) . ? C15 C20 1.500(2) . ? C16 C17 1.4324(19) . ? C16 C21 1.5026(18) . ? C17 C18 1.428(2) . ? C17 C22 1.500(2) . ? C18 C19 1.426(2) . ? C18 C23 1.501(2) . ? C19 C24 1.507(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? K1 O5 2.7798(10) . ? K1 O3 2.7909(11) . ? K1 O4 2.7926(11) . ? K1 O6 2.7934(10) . ? K1 O7 2.8058(11) . ? K1 O8 2.8443(11) . ? K1 N2 2.8803(16) . ? K1 N1 2.9366(15) . ? O3 C25 1.4181(18) . ? O3 C36 1.4233(19) . ? O4 C26 1.4249(18) . ? O4 C27 1.4265(17) . ? O5 C28 1.4258(18) . ? O5 C29 1.4259(17) . ? O6 C31 1.4188(18) . ? O6 C30 1.4264(18) . ? O7 C33 1.4223(19) . ? O7 C32 1.4300(17) . ? O8 C34 1.4203(19) . ? O8 C35 1.4290(18) . ? N1 C37 1.134(2) . ? N2 C39 1.133(2) . ? C25 C26 1.495(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.500(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.492(2) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.497(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.492(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.495(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.446(2) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.466(3) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N3 C41 1.120(3) . ? C41 C42 1.433(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? 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 C18 Fe1 C3 163.92(6) . . ? C18 Fe1 C17 40.73(6) . . ? C3 Fe1 C17 125.89(6) . . ? C18 Fe1 C4 125.96(6) . . ? C3 Fe1 C4 40.83(5) . . ? C17 Fe1 C4 104.88(6) . . ? C18 Fe1 C19 40.58(6) . . ? C3 Fe1 C19 153.61(6) . . ? C17 Fe1 C19 68.24(6) . . ? C4 Fe1 C19 165.34(6) . . ? C18 Fe1 C16 68.29(6) . . ? C3 Fe1 C16 107.11(5) . . ? C17 Fe1 C16 40.69(5) . . ? C4 Fe1 C16 116.00(6) . . ? C19 Fe1 C16 67.86(6) . . ? C18 Fe1 C15 68.20(6) . . ? C3 Fe1 C15 118.97(5) . . ? C17 Fe1 C15 68.20(6) . . ? C4 Fe1 C15 150.79(5) . . ? C19 Fe1 C15 40.36(5) . . ? C16 Fe1 C15 40.25(6) . . ? C18 Fe1 C5 105.55(5) . . ? C3 Fe1 C5 69.55(5) . . ? C17 Fe1 C5 113.49(5) . . ? C4 Fe1 C5 40.22(5) . . ? C19 Fe1 C5 129.16(5) . . ? C16 Fe1 C5 147.35(6) . . ? C15 Fe1 C5 168.99(5) . . ? C18 Fe1 C2 154.91(6) . . ? C3 Fe1 C2 40.02(5) . . ? C17 Fe1 C2 163.33(5) . . ? C4 Fe1 C2 69.46(5) . . ? C19 Fe1 C2 120.76(6) . . ? C16 Fe1 C2 126.44(5) . . ? C15 Fe1 C2 108.66(5) . . ? C5 Fe1 C2 72.91(5) . . ? C18 Fe1 P1 112.75(4) . . ? C3 Fe1 P1 75.84(4) . . ? C17 Fe1 P1 148.34(4) . . ? C4 Fe1 P1 76.04(4) . . ? C19 Fe1 P1 102.82(4) . . ? C16 Fe1 P1 165.14(4) . . ? C15 Fe1 P1 125.31(4) . . ? C5 Fe1 P1 47.51(4) . . ? C2 Fe1 P1 47.26(3) . . ? C2 P1 C5 89.73(6) . . ? C2 P1 Fe1 61.13(4) . . ? C5 P1 Fe1 60.66(4) . . ? C7 P2 C10 91.07(6) . 2_655 ? O1 C1 C10 123.66(12) . . ? O1 C1 C2 120.52(13) . . ? C10 C1 C2 115.71(11) . . ? C3 C2 C1 120.84(11) . . ? C3 C2 P1 113.00(9) . . ? C1 C2 P1 125.36(10) . . ? C3 C2 Fe1 67.59(7) . . ? C1 C2 Fe1 137.26(10) . . ? P1 C2 Fe1 71.61(5) . . ? C2 C3 C4 112.39(11) . . ? C2 C3 C11 123.54(13) . . ? C4 C3 C11 123.86(13) . . ? C2 C3 Fe1 72.39(8) . . ? C4 C3 Fe1 69.69(7) . . ? C11 C3 Fe1 129.95(10) . . ? C5 C4 C3 111.77(11) . . ? C5 C4 C12 124.96(12) . . ? C3 C4 C12 123.01(12) . . ? C5 C4 Fe1 71.72(8) . . ? C3 C4 Fe1 69.48(8) . . ? C12 C4 Fe1 130.92(11) . . ? C4 C5 C6 122.39(12) . . ? C4 C5 P1 113.08(9) . . ? C6 C5 P1 124.15(9) . . ? C4 C5 Fe1 68.07(7) . . ? C6 C5 Fe1 134.13(10) . . ? P1 C5 Fe1 71.84(5) . . ? O2 C6 C7 123.58(12) . . ? O2 C6 C5 120.30(12) . . ? C7 C6 C5 115.90(11) . . ? C8 C7 C6 126.85(12) . . ? C8 C7 P2 111.73(10) . . ? C6 C7 P2 121.21(9) . . ? C9 C8 C7 112.84(11) . . ? C9 C8 C13 124.53(12) . . ? C7 C8 C13 122.59(12) . . ? C8 C9 C10 112.74(11) . 2_655 ? C8 C9 C14 124.72(12) . . ? C10 C9 C14 122.51(12) 2_655 . ? C9 C10 C1 126.69(11) 2_655 . ? C9 C10 P2 111.61(9) 2_655 2_655 ? C1 C10 P2 121.70(9) . 2_655 ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C19 107.47(12) . . ? C16 C15 C20 126.47(13) . . ? C19 C15 C20 125.91(14) . . ? C16 C15 Fe1 69.22(8) . . ? C19 C15 Fe1 69.05(8) . . ? C20 C15 Fe1 130.48(11) . . ? C15 C16 C17 108.35(12) . . ? C15 C16 C21 125.59(12) . . ? C17 C16 C21 125.99(13) . . ? C15 C16 Fe1 70.53(8) . . ? C17 C16 Fe1 69.14(8) . . ? C21 C16 Fe1 128.34(11) . . ? C18 C17 C16 107.75(13) . . ? C18 C17 C22 125.14(13) . . ? C16 C17 C22 127.09(13) . . ? C18 C17 Fe1 69.50(8) . . ? C16 C17 Fe1 70.16(8) . . ? C22 C17 Fe1 127.24(11) . . ? C19 C18 C17 108.01(12) . . ? C19 C18 C23 126.05(14) . . ? C17 C18 C23 125.88(15) . . ? C19 C18 Fe1 70.24(8) . . ? C17 C18 Fe1 69.77(8) . . ? C23 C18 Fe1 127.86(11) . . ? C18 C19 C15 108.42(13) . . ? C18 C19 C24 126.00(14) . . ? C15 C19 C24 125.50(15) . . ? C18 C19 Fe1 69.18(8) . . ? C15 C19 Fe1 70.59(8) . . ? C24 C19 Fe1 128.45(12) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O5 K1 O3 120.65(3) . . ? O5 K1 O4 61.49(3) . . ? O3 K1 O4 59.82(3) . . ? O5 K1 O6 60.04(3) . . ? O3 K1 O6 176.96(3) . . ? O4 K1 O6 120.28(3) . . ? O5 K1 O7 119.10(3) . . ? O3 K1 O7 118.77(3) . . ? O4 K1 O7 175.82(3) . . ? O6 K1 O7 61.37(3) . . ? O5 K1 O8 177.89(3) . . ? O3 K1 O8 60.54(3) . . ? O4 K1 O8 119.36(3) . . ? O6 K1 O8 118.67(3) . . ? O7 K1 O8 60.21(3) . . ? O5 K1 N2 95.19(4) . . ? O3 K1 N2 77.23(4) . . ? O4 K1 N2 90.33(4) . . ? O6 K1 N2 105.75(4) . . ? O7 K1 N2 85.50(4) . . ? O8 K1 N2 86.77(4) . . ? O5 K1 N1 82.26(4) . . ? O3 K1 N1 104.75(4) . . ? O4 K1 N1 89.16(5) . . ? O6 K1 N1 72.29(4) . . ? O7 K1 N1 95.02(5) . . ? O8 K1 N1 95.77(4) . . ? N2 K1 N1 177.32(5) . . ? C25 O3 C36 112.14(12) . . ? C25 O3 K1 116.69(8) . . ? C36 O3 K1 113.31(9) . . ? C26 O4 C27 111.68(11) . . ? C26 O4 K1 115.00(8) . . ? C27 O4 K1 111.74(8) . . ? C28 O5 C29 112.55(11) . . ? C28 O5 K1 114.85(8) . . ? C29 O5 K1 114.90(8) . . ? C31 O6 C30 112.38(11) . . ? C31 O6 K1 114.14(8) . . ? C30 O6 K1 116.99(9) . . ? C33 O7 C32 111.79(12) . . ? C33 O7 K1 115.49(9) . . ? C32 O7 K1 112.58(8) . . ? C34 O8 C35 111.96(11) . . ? C34 O8 K1 112.26(9) . . ? C35 O8 K1 113.73(9) . . ? C37 N1 K1 122.20(13) . . ? C39 N2 K1 119.29(13) . . ? O3 C25 C26 108.67(12) . . ? O3 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? O3 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? H25A C25 H25B 108.3 . . ? O4 C26 C25 108.35(13) . . ? O4 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? O4 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? O4 C27 C28 109.05(12) . . ? O4 C27 H27A 109.9 . . ? C28 C27 H27A 109.9 . . ? O4 C27 H27B 109.9 . . ? C28 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? O5 C28 C27 109.31(12) . . ? O5 C28 H28A 109.8 . . ? C27 C28 H28A 109.8 . . ? O5 C28 H28B 109.8 . . ? C27 C28 H28B 109.8 . . ? H28A C28 H28B 108.3 . . ? O5 C29 C30 108.80(12) . . ? O5 C29 H29A 109.9 . . ? C30 C29 H29A 109.9 . . ? O5 C29 H29B 109.9 . . ? C30 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? O6 C30 C29 109.27(12) . . ? O6 C30 H30A 109.8 . . ? C29 C30 H30A 109.8 . . ? O6 C30 H30B 109.8 . . ? C29 C30 H30B 109.8 . . ? H30A C30 H30B 108.3 . . ? O6 C31 C32 108.99(12) . . ? O6 C31 H31A 109.9 . . ? C32 C31 H31A 109.9 . . ? O6 C31 H31B 109.9 . . ? C32 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? O7 C32 C31 110.12(13) . . ? O7 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? O7 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.2 . . ? O7 C33 C34 109.43(13) . . ? O7 C33 H33A 109.8 . . ? C34 C33 H33A 109.8 . . ? O7 C33 H33B 109.8 . . ? C34 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? O8 C34 C33 108.51(12) . . ? O8 C34 H34A 110.0 . . ? C33 C34 H34A 110.0 . . ? O8 C34 H34B 110.0 . . ? C33 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? O8 C35 C36 108.62(12) . . ? O8 C35 H35A 110.0 . . ? C36 C35 H35A 110.0 . . ? O8 C35 H35B 110.0 . . ? C36 C35 H35B 110.0 . . ? H35A C35 H35B 108.3 . . ? O3 C36 C35 108.76(13) . . ? O3 C36 H36A 109.9 . . ? C35 C36 H36A 109.9 . . ? O3 C36 H36B 109.9 . . ? C35 C36 H36B 109.9 . . ? H36A C36 H36B 108.3 . . ? N1 C37 C38 179.51(18) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N2 C39 C40 178.2(2) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 C41 C42 179.2(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.580 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.051 #===END # compound 11 data_ae490 _database_code_depnum_ccdc_archive 'CCDC 830883' #TrackingRef '2011_duncan_chem_commun.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H84 Fe K2 N O16 P3, C2 H3 N' _chemical_formula_sum 'C63 H87 Fe K2 N2 O16 P3' _chemical_formula_weight 1355.31 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 '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 ' _symmetry_space_group_name_Hall '-P 2ybc' 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 17.606(1) _cell_length_b 16.733(1) _cell_length_c 27.421(1) _cell_angle_alpha 90.00 _cell_angle_beta 125.457(2) _cell_angle_gamma 90.00 _cell_volume 6580.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 797 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2864 _exptl_absorpt_coefficient_mu 0.496 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8987 _exptl_absorpt_correction_T_max 0.9902 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58153 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.02 _reflns_number_total 11464 _reflns_number_gt 8811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0105P)^2^+32.3497P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11464 _refine_ls_number_parameters 796 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1279 _refine_ls_R_factor_gt 0.0968 _refine_ls_wR_factor_ref 0.1767 _refine_ls_wR_factor_gt 0.1646 _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_restrained_S_all 1.209 _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 0.62533(5) 0.55269(5) 0.22189(4) 0.0292(2) Uani 1 1 d . . . K1 K 1.00647(9) 0.03498(8) 0.38636(6) 0.0371(3) Uani 1 1 d . . . K2 K 0.61966(9) 0.11240(8) 0.10204(7) 0.0405(4) Uani 1 1 d . . . P1 P 0.73458(10) 0.45553(9) 0.25143(7) 0.0287(3) Uani 1 1 d . . . P2 P 0.93257(10) 0.44842(9) 0.31152(7) 0.0313(4) Uani 1 1 d . . . P3 P 0.74273(10) 0.29767(9) 0.20932(7) 0.0308(4) Uani 1 1 d . . . O1 O 0.8512(3) 0.6696(2) 0.29468(19) 0.0393(10) Uani 1 1 d . . . O2 O 1.1582(3) 0.3411(3) 0.4426(2) 0.0505(13) Uani 1 1 d . . . O3 O 0.8377(3) 0.0882(2) 0.2897(2) 0.0400(11) Uani 1 1 d . . . O4 O 0.4890(3) 0.3864(2) 0.11035(19) 0.0395(10) Uani 1 1 d . . . O5 O 0.9365(3) 0.1111(3) 0.4453(2) 0.0432(11) Uani 1 1 d . . . O6 O 1.1264(3) 0.1307(3) 0.4932(2) 0.0463(11) Uani 1 1 d . . . O7 O 1.2000(3) 0.0599(3) 0.43632(19) 0.0420(11) Uani 1 1 d . . . O8 O 1.1121(3) -0.0775(2) 0.3690(2) 0.0419(11) Uani 1 1 d . . . O9 O 0.9277(3) -0.1111(2) 0.3275(2) 0.0425(11) Uani 1 1 d . . . O10 O 0.8618(3) -0.0378(3) 0.3874(2) 0.0422(11) Uani 1 1 d . . . O11 O 0.4837(4) -0.0058(3) 0.0819(3) 0.088(2) Uani 1 1 d . . . O12 O 0.4297(3) 0.1385(3) 0.0227(2) 0.0538(13) Uani 1 1 d . . . O13 O 0.5404(4) 0.2403(3) 0.0117(4) 0.095(2) Uani 1 1 d . . . O14 O 0.7199(3) 0.1802(3) 0.0628(2) 0.0535(13) Uani 1 1 d . . . O15 O 0.7949(3) 0.0543(3) 0.1442(2) 0.0563(13) Uani 1 1 d . . . O16 O 0.6680(3) -0.0504(3) 0.1385(2) 0.0601(14) Uani 1 1 d . . . N1 N 0.9509(3) 0.2597(3) 0.3279(2) 0.0312(11) Uani 1 1 d . . . C1 C 0.6335(4) 0.4553(3) 0.1765(2) 0.0277(13) Uani 1 1 d . . . C2 C 0.6181(4) 0.5294(3) 0.1459(3) 0.0293(13) Uani 1 1 d . . . C3 C 0.6899(4) 0.5859(3) 0.1820(3) 0.0314(14) Uani 1 1 d . . . C4 C 0.7588(4) 0.5549(3) 0.2405(3) 0.0295(13) Uani 1 1 d . . . C5 C 0.8451(4) 0.5955(4) 0.2914(3) 0.0319(14) Uani 1 1 d . . . C6 C 0.9187(4) 0.5415(3) 0.3346(3) 0.0303(13) Uani 1 1 d . . . C7 C 0.9841(4) 0.5541(3) 0.3974(3) 0.0318(13) Uani 1 1 d . . . C8 C 1.0425(4) 0.4879(4) 0.4260(3) 0.0381(15) Uani 1 1 d . . . C9 C 1.0246(4) 0.4247(3) 0.3857(3) 0.0306(14) Uani 1 1 d . . . C10 C 1.0781(4) 0.3544(4) 0.3974(3) 0.0344(14) Uani 1 1 d . . . C11 C 1.0379(4) 0.2874(3) 0.3508(3) 0.0318(14) Uani 1 1 d . . . C12 C 1.0936(4) 0.2543(4) 0.3358(3) 0.0391(16) Uani 1 1 d . . . H12 H 1.1548 0.2743 0.3533 0.047 Uiso 1 1 calc R . . C13 C 1.0606(4) 0.1922(4) 0.2956(3) 0.0411(16) Uani 1 1 d . . . H13 H 1.0970 0.1708 0.2834 0.049 Uiso 1 1 calc R . . C14 C 0.9729(4) 0.1616(4) 0.2734(3) 0.0395(15) Uani 1 1 d . . . H14 H 0.9491 0.1171 0.2470 0.047 Uiso 1 1 calc R . . C15 C 0.9210(4) 0.1973(3) 0.2905(3) 0.0303(13) Uani 1 1 d . . . C16 C 0.8289(4) 0.1574(3) 0.2711(3) 0.0289(13) Uani 1 1 d . . . C17 C 0.7431(4) 0.2012(3) 0.2343(2) 0.0268(13) Uani 1 1 d . . . C18 C 0.6518(4) 0.1778(3) 0.2173(3) 0.0293(13) Uani 1 1 d . . . C19 C 0.5861(4) 0.2375(3) 0.1862(3) 0.0291(13) Uani 1 1 d . . . C20 C 0.6235(4) 0.3074(3) 0.1786(2) 0.0274(13) Uani 1 1 d . . . C21 C 0.5734(4) 0.3828(4) 0.1512(3) 0.0314(13) Uani 1 1 d . . . C22 C 0.5397(4) 0.5431(4) 0.0811(3) 0.0423(16) Uani 1 1 d . . . H22A H 0.5589 0.5251 0.0558 0.064 Uiso 1 1 calc R . . H22B H 0.5246 0.6002 0.0743 0.064 Uiso 1 1 calc R . . H22C H 0.4847 0.5129 0.0710 0.064 Uiso 1 1 calc R . . C23 C 0.6959(4) 0.6668(3) 0.1596(3) 0.0376(15) Uani 1 1 d . . . H23A H 0.7363 0.7021 0.1938 0.056 Uiso 1 1 calc R . . H23B H 0.6334 0.6902 0.1341 0.056 Uiso 1 1 calc R . . H23C H 0.7218 0.6604 0.1364 0.056 Uiso 1 1 calc R . . C24 C 0.9879(4) 0.6281(4) 0.4304(3) 0.0421(16) Uani 1 1 d . . . H24A H 0.9393 0.6656 0.4019 0.063 Uiso 1 1 calc R . . H24B H 1.0492 0.6534 0.4498 0.063 Uiso 1 1 calc R . . H24C H 0.9778 0.6132 0.4608 0.063 Uiso 1 1 calc R . . C25 C 1.1158(4) 0.4844(4) 0.4932(3) 0.0483(18) Uani 1 1 d . . . H25A H 1.1680 0.5194 0.5040 0.072 Uiso 1 1 calc R . . H25B H 1.1383 0.4293 0.5050 0.072 Uiso 1 1 calc R . . H25C H 1.0884 0.5021 0.5139 0.072 Uiso 1 1 calc R . . C26 C 0.6304(4) 0.1002(4) 0.2342(3) 0.0451(17) Uani 1 1 d . . . H26A H 0.6375 0.1066 0.2721 0.068 Uiso 1 1 calc R . . H26B H 0.6736 0.0590 0.2386 0.068 Uiso 1 1 calc R . . H26C H 0.5662 0.0843 0.2028 0.068 Uiso 1 1 calc R . . C27 C 0.4874(4) 0.2305(4) 0.1675(3) 0.0448(17) Uani 1 1 d . . . H27A H 0.4582 0.1830 0.1423 0.067 Uiso 1 1 calc R . . H27B H 0.4522 0.2782 0.1448 0.067 Uiso 1 1 calc R . . H27C H 0.4875 0.2257 0.2031 0.067 Uiso 1 1 calc R . . C28 C 0.5196(4) 0.5269(4) 0.2301(3) 0.0419(16) Uani 1 1 d . . . C29 C 0.4970(4) 0.5951(4) 0.1947(3) 0.0371(15) Uani 1 1 d . . . C30 C 0.5675(5) 0.6538(4) 0.2301(3) 0.0441(17) Uani 1 1 d . . . C31 C 0.6328(5) 0.6201(5) 0.2873(3) 0.0494(19) Uani 1 1 d . . . C32 C 0.6037(4) 0.5420(4) 0.2877(3) 0.0449(17) Uani 1 1 d . . . C33 C 0.4629(5) 0.4516(4) 0.2121(4) 0.063(2) Uani 1 1 d . . . H33A H 0.4160 0.4571 0.2204 0.095 Uiso 1 1 calc R . . H33B H 0.5040 0.4065 0.2350 0.095 Uiso 1 1 calc R . . H33C H 0.4318 0.4421 0.1693 0.095 Uiso 1 1 calc R . . C34 C 0.4114(5) 0.6071(5) 0.1324(3) 0.063(2) Uani 1 1 d . . . H34A H 0.3614 0.6290 0.1342 0.094 Uiso 1 1 calc R . . H34B H 0.3915 0.5558 0.1114 0.094 Uiso 1 1 calc R . . H34C H 0.4252 0.6445 0.1110 0.094 Uiso 1 1 calc R . . C35 C 0.5697(6) 0.7383(4) 0.2116(5) 0.074(3) Uani 1 1 d . . . H35A H 0.5415 0.7397 0.1685 0.112 Uiso 1 1 calc R . . H35B H 0.6345 0.7567 0.2337 0.112 Uiso 1 1 calc R . . H35C H 0.5346 0.7734 0.2205 0.112 Uiso 1 1 calc R . . C36 C 0.7162(5) 0.6621(6) 0.3403(4) 0.088(3) Uani 1 1 d . . . H36A H 0.7410 0.7008 0.3261 0.132 Uiso 1 1 calc R . . H36B H 0.7644 0.6227 0.3662 0.132 Uiso 1 1 calc R . . H36C H 0.6971 0.6900 0.3630 0.132 Uiso 1 1 calc R . . C37 C 0.6484(6) 0.4849(6) 0.3398(4) 0.084(3) Uani 1 1 d . . . H37A H 0.7160 0.4935 0.3653 0.126 Uiso 1 1 calc R . . H37B H 0.6349 0.4298 0.3249 0.126 Uiso 1 1 calc R . . H37C H 0.6233 0.4943 0.3632 0.126 Uiso 1 1 calc R . . C38 C 0.9971(5) 0.1587(4) 0.4971(3) 0.0467(17) Uani 1 1 d . . . H38A H 1.0258 0.1253 0.5335 0.056 Uiso 1 1 calc R . . H38B H 0.9612 0.2019 0.4996 0.056 Uiso 1 1 calc R . . C39 C 1.0718(5) 0.1940(4) 0.4932(3) 0.0528(19) Uani 1 1 d . . . H39A H 1.0431 0.2258 0.4560 0.063 Uiso 1 1 calc R . . H39B H 1.1120 0.2298 0.5277 0.063 Uiso 1 1 calc R . . C40 C 1.2098(4) 0.1589(4) 0.5023(3) 0.0492(18) Uani 1 1 d . . . H40A H 1.2512 0.1825 0.5428 0.059 Uiso 1 1 calc R . . H40B H 1.1951 0.2007 0.4724 0.059 Uiso 1 1 calc R . . C41 C 1.2575(4) 0.0895(4) 0.4957(3) 0.0457(17) Uani 1 1 d . . . H41A H 1.3182 0.1069 0.5049 0.055 Uiso 1 1 calc R . . H41B H 1.2692 0.0467 0.5243 0.055 Uiso 1 1 calc R . . C42 C 1.2464(4) 0.0014(4) 0.4249(3) 0.0533(19) Uani 1 1 d . . . H42A H 1.2732 -0.0403 0.4564 0.064 Uiso 1 1 calc R . . H42B H 1.2980 0.0266 0.4257 0.064 Uiso 1 1 calc R . . C43 C 1.1790(5) -0.0353(4) 0.3655(3) 0.0493(18) Uani 1 1 d . . . H43A H 1.1480 0.0065 0.3342 0.059 Uiso 1 1 calc R . . H43B H 1.2116 -0.0724 0.3552 0.059 Uiso 1 1 calc R . . C44 C 1.0518(5) -0.1263(4) 0.3175(3) 0.0473(17) Uani 1 1 d . . . H44A H 1.0889 -0.1656 0.3125 0.057 Uiso 1 1 calc R . . H44B H 1.0164 -0.0928 0.2811 0.057 Uiso 1 1 calc R . . C45 C 0.9867(5) -0.1684(4) 0.3266(3) 0.0458(17) Uani 1 1 d . . . H45A H 0.9486 -0.2071 0.2937 0.055 Uiso 1 1 calc R . . H45B H 1.0224 -0.1982 0.3648 0.055 Uiso 1 1 calc R . . C46 C 0.8592(5) -0.1485(4) 0.3319(3) 0.0461(17) Uani 1 1 d . . . H46A H 0.8899 -0.1825 0.3682 0.055 Uiso 1 1 calc R . . H46B H 0.8183 -0.1827 0.2965 0.055 Uiso 1 1 calc R . . C47 C 0.8029(4) -0.0851(4) 0.3354(3) 0.0456(17) Uani 1 1 d . . . H47A H 0.7726 -0.0510 0.2992 0.055 Uiso 1 1 calc R . . H47B H 0.7534 -0.1101 0.3370 0.055 Uiso 1 1 calc R . . C48 C 0.8099(4) 0.0199(4) 0.3947(3) 0.0467(17) Uani 1 1 d . . . H48A H 0.7613 -0.0070 0.3963 0.056 Uiso 1 1 calc R . . H48B H 0.7787 0.0572 0.3603 0.056 Uiso 1 1 calc R . . C49 C 0.8748(5) 0.0650(4) 0.4515(3) 0.0485(18) Uani 1 1 d . . . H49A H 0.8388 0.1005 0.4600 0.058 Uiso 1 1 calc R . . H49B H 0.9109 0.0271 0.4853 0.058 Uiso 1 1 calc R . . C50 C 0.3984(6) 0.0052(5) 0.0375(4) 0.077(3) Uani 1 1 d D . . H50A H 0.3582 -0.0215 0.0470 0.093 Uiso 1 1 calc R . . H50B H 0.3883 -0.0223 0.0022 0.093 Uiso 1 1 calc R . . C51 C 0.3657(5) 0.0895(5) 0.0201(5) 0.113(4) Uani 1 1 d D . . H51A H 0.3080 0.0901 -0.0211 0.136 Uiso 1 1 calc R . . H51B H 0.3502 0.1108 0.0470 0.136 Uiso 1 1 calc R . . C52 C 0.3954(6) 0.2092(6) -0.0016(6) 0.120(5) Uani 1 1 d D . . H52A H 0.3653 0.2325 0.0165 0.145 Uiso 1 1 calc R . . H52B H 0.3465 0.2019 -0.0449 0.145 Uiso 1 1 calc R . . C53 C 0.4660(6) 0.2672(5) 0.0059(4) 0.080(3) Uani 1 1 d D . . H53A H 0.4337 0.3034 -0.0292 0.096 Uiso 1 1 calc R . . H53B H 0.4869 0.3002 0.0415 0.096 Uiso 1 1 calc R . . C54 C 0.6049(6) 0.2847(6) 0.0224(6) 0.120(5) Uani 1 1 d D . . H54A H 0.6161 0.3220 0.0539 0.143 Uiso 1 1 calc R . . H54B H 0.5794 0.3173 -0.0141 0.143 Uiso 1 1 calc R . . C55 C 0.6990(6) 0.2575(5) 0.0409(5) 0.084(3) Uani 1 1 d D . . H55A H 0.7021 0.2610 0.0061 0.101 Uiso 1 1 calc R . . H55B H 0.7468 0.2941 0.0722 0.101 Uiso 1 1 calc R . . C56 C 0.8153(5) 0.1643(4) 0.0982(4) 0.065(2) Uani 1 1 d D . . H56A H 0.8462 0.1971 0.1350 0.078 Uiso 1 1 calc R . . H56B H 0.8419 0.1793 0.0761 0.078 Uiso 1 1 calc R . . C57 C 0.8342(5) 0.0778(4) 0.1148(3) 0.055(2) Uani 1 1 d D . . H57A H 0.8079 0.0452 0.0782 0.066 Uiso 1 1 calc R . . H57B H 0.9024 0.0686 0.1412 0.066 Uiso 1 1 calc R . . C58 C 0.8168(5) -0.0254(5) 0.1611(4) 0.080(3) Uani 1 1 d D . . H58A H 0.8837 -0.0295 0.1946 0.096 Uiso 1 1 calc R . . H58B H 0.8066 -0.0564 0.1271 0.096 Uiso 1 1 calc R . . C59 C 0.7601(6) -0.0615(6) 0.1801(5) 0.102(4) Uani 1 1 d D . . H59A H 0.7733 -0.1195 0.1869 0.122 Uiso 1 1 calc R . . H59B H 0.7783 -0.0371 0.2184 0.122 Uiso 1 1 calc R . . C60 C 0.6130(5) -0.0967(6) 0.1407(6) 0.138(6) Uani 1 1 d D . . H60A H 0.6271 -0.0924 0.1812 0.166 Uiso 1 1 calc R . . H60B H 0.6274 -0.1522 0.1361 0.166 Uiso 1 1 calc R . . C61 C 0.5107(5) -0.0838(4) 0.0960(4) 0.072(3) Uani 1 1 d D . . H61A H 0.4904 -0.1127 0.0588 0.087 Uiso 1 1 calc R . . H61B H 0.4777 -0.1079 0.1118 0.087 Uiso 1 1 calc R . . N2 N 0.7504(8) 0.2866(7) 0.4356(5) 0.130(4) Uani 1 1 d . . . C62 C 0.7779(7) 0.2940(6) 0.4087(4) 0.077(3) Uani 1 1 d . . . C63 C 0.8159(9) 0.3043(8) 0.3760(5) 0.127(5) Uani 1 1 d . . . H63A H 0.8506 0.3547 0.3877 0.190 Uiso 1 1 calc R . . H63B H 0.7655 0.3056 0.3331 0.190 Uiso 1 1 calc R . . H63C H 0.8581 0.2598 0.3843 0.190 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0209(4) 0.0278(4) 0.0368(5) 0.0023(4) 0.0156(4) 0.0017(4) K1 0.0286(7) 0.0352(7) 0.0433(8) -0.0005(6) 0.0185(6) 0.0015(6) K2 0.0319(7) 0.0399(8) 0.0472(9) 0.0058(7) 0.0217(7) 0.0039(6) P1 0.0205(7) 0.0249(8) 0.0335(9) 0.0004(7) 0.0115(7) -0.0005(6) P2 0.0206(7) 0.0292(8) 0.0345(9) -0.0017(7) 0.0104(7) -0.0008(6) P3 0.0210(7) 0.0298(8) 0.0364(9) 0.0011(7) 0.0136(7) -0.0021(6) O1 0.032(2) 0.027(2) 0.051(3) -0.001(2) 0.020(2) -0.0025(18) O2 0.022(2) 0.037(3) 0.052(3) 0.000(2) -0.002(2) -0.0009(19) O3 0.029(2) 0.027(2) 0.054(3) 0.004(2) 0.019(2) -0.0019(18) O4 0.020(2) 0.038(2) 0.041(3) 0.002(2) 0.006(2) 0.0004(18) O5 0.042(2) 0.040(3) 0.047(3) 0.000(2) 0.026(2) 0.002(2) O6 0.043(3) 0.036(3) 0.059(3) -0.005(2) 0.029(2) -0.004(2) O7 0.029(2) 0.039(2) 0.048(3) -0.001(2) 0.017(2) 0.0009(19) O8 0.040(2) 0.039(2) 0.053(3) -0.002(2) 0.031(2) 0.000(2) O9 0.034(2) 0.032(2) 0.058(3) -0.001(2) 0.025(2) 0.0016(19) O10 0.035(2) 0.039(2) 0.053(3) -0.001(2) 0.025(2) 0.003(2) O11 0.035(3) 0.057(4) 0.113(5) 0.023(3) 0.009(3) -0.010(3) O12 0.035(3) 0.055(3) 0.054(3) 0.009(3) 0.016(2) 0.010(2) O13 0.064(4) 0.043(3) 0.179(7) 0.023(4) 0.072(5) 0.009(3) O14 0.046(3) 0.045(3) 0.069(3) 0.014(3) 0.033(3) 0.002(2) O15 0.036(3) 0.052(3) 0.083(4) 0.015(3) 0.036(3) 0.017(2) O16 0.049(3) 0.042(3) 0.085(4) 0.017(3) 0.036(3) 0.004(2) N1 0.026(3) 0.025(3) 0.040(3) 0.003(2) 0.018(2) 0.000(2) C1 0.020(3) 0.029(3) 0.031(3) -0.001(3) 0.013(3) 0.001(2) C2 0.023(3) 0.032(3) 0.033(3) 0.002(3) 0.016(3) 0.005(2) C3 0.024(3) 0.028(3) 0.042(4) 0.005(3) 0.019(3) 0.006(2) C4 0.026(3) 0.026(3) 0.042(4) -0.001(3) 0.023(3) 0.001(2) C5 0.024(3) 0.032(4) 0.041(4) -0.002(3) 0.020(3) -0.003(3) C6 0.021(3) 0.029(3) 0.039(3) -0.002(3) 0.016(3) -0.005(2) C7 0.022(3) 0.030(3) 0.042(4) -0.005(3) 0.018(3) -0.006(3) C8 0.027(3) 0.044(4) 0.037(4) -0.003(3) 0.015(3) -0.010(3) C9 0.020(3) 0.030(3) 0.035(3) 0.007(3) 0.012(3) -0.001(2) C10 0.022(3) 0.035(3) 0.036(4) 0.006(3) 0.012(3) -0.010(3) C11 0.022(3) 0.026(3) 0.041(4) 0.007(3) 0.014(3) 0.004(2) C12 0.023(3) 0.042(4) 0.046(4) 0.009(3) 0.015(3) 0.001(3) C13 0.029(3) 0.052(4) 0.050(4) 0.006(3) 0.027(3) 0.011(3) C14 0.037(3) 0.034(3) 0.043(4) -0.001(3) 0.021(3) 0.003(3) C15 0.025(3) 0.026(3) 0.036(3) 0.007(3) 0.016(3) 0.003(2) C16 0.029(3) 0.027(3) 0.026(3) -0.005(3) 0.013(3) -0.005(2) C17 0.021(3) 0.027(3) 0.027(3) -0.002(2) 0.011(3) -0.003(2) C18 0.030(3) 0.024(3) 0.038(4) -0.008(3) 0.022(3) -0.007(2) C19 0.023(3) 0.030(3) 0.033(3) -0.008(3) 0.015(3) -0.003(2) C20 0.019(3) 0.034(3) 0.026(3) -0.005(3) 0.011(2) 0.000(2) C21 0.023(3) 0.035(3) 0.032(3) -0.001(3) 0.013(3) -0.001(3) C22 0.032(3) 0.044(4) 0.044(4) 0.005(3) 0.018(3) 0.002(3) C23 0.029(3) 0.033(3) 0.044(4) 0.008(3) 0.017(3) 0.002(3) C24 0.032(3) 0.044(4) 0.047(4) -0.010(3) 0.022(3) -0.008(3) C25 0.034(4) 0.058(4) 0.035(4) -0.001(3) 0.009(3) -0.003(3) C26 0.031(3) 0.039(4) 0.063(5) 0.006(3) 0.026(3) -0.001(3) C27 0.032(3) 0.036(4) 0.066(5) 0.003(3) 0.028(4) -0.003(3) C28 0.032(3) 0.037(4) 0.066(5) 0.002(3) 0.034(4) 0.004(3) C29 0.026(3) 0.042(4) 0.048(4) 0.004(3) 0.025(3) 0.011(3) C30 0.047(4) 0.028(3) 0.075(5) -0.006(3) 0.046(4) -0.002(3) C31 0.035(4) 0.065(5) 0.054(5) -0.026(4) 0.030(4) -0.005(4) C32 0.039(4) 0.055(4) 0.052(4) 0.009(4) 0.033(4) 0.013(3) C33 0.066(5) 0.038(4) 0.116(7) -0.009(4) 0.070(5) -0.010(4) C34 0.031(4) 0.085(6) 0.064(5) 0.008(5) 0.022(4) 0.014(4) C35 0.094(7) 0.035(4) 0.137(9) 0.009(5) 0.091(7) 0.012(4) C36 0.047(5) 0.137(9) 0.085(7) -0.062(6) 0.041(5) -0.029(5) C37 0.091(7) 0.121(8) 0.066(6) 0.040(6) 0.060(6) 0.046(6) C38 0.045(4) 0.046(4) 0.045(4) -0.003(3) 0.024(3) 0.008(3) C39 0.055(4) 0.036(4) 0.055(5) -0.008(3) 0.025(4) 0.002(3) C40 0.040(4) 0.042(4) 0.049(4) -0.003(3) 0.016(3) -0.008(3) C41 0.025(3) 0.045(4) 0.049(4) 0.005(3) 0.011(3) 0.000(3) C42 0.031(4) 0.053(4) 0.072(5) 0.001(4) 0.028(4) 0.005(3) C43 0.047(4) 0.047(4) 0.066(5) -0.003(4) 0.040(4) 0.000(3) C44 0.049(4) 0.046(4) 0.046(4) -0.006(3) 0.027(4) 0.003(3) C45 0.047(4) 0.038(4) 0.055(5) -0.009(3) 0.031(4) 0.003(3) C46 0.044(4) 0.034(4) 0.058(5) -0.002(3) 0.029(4) -0.001(3) C47 0.038(4) 0.034(4) 0.065(5) -0.001(3) 0.029(4) -0.001(3) C48 0.036(4) 0.049(4) 0.064(5) 0.005(4) 0.035(4) 0.004(3) C49 0.050(4) 0.047(4) 0.061(5) 0.008(4) 0.040(4) 0.009(3) C50 0.054(5) 0.073(6) 0.095(7) -0.004(5) 0.037(5) -0.012(5) C51 0.027(4) 0.141(10) 0.127(9) 0.060(8) 0.020(5) 0.000(5) C52 0.079(7) 0.096(8) 0.203(13) 0.082(9) 0.091(9) 0.053(6) C53 0.088(7) 0.051(5) 0.074(6) 0.023(5) 0.031(5) 0.033(5) C54 0.075(7) 0.067(6) 0.176(12) 0.076(7) 0.049(8) 0.017(6) C55 0.092(7) 0.054(5) 0.139(9) 0.022(6) 0.086(7) 0.004(5) C56 0.043(4) 0.070(5) 0.088(6) 0.006(5) 0.041(5) -0.002(4) C57 0.032(4) 0.077(6) 0.053(5) 0.000(4) 0.024(4) 0.009(4) C58 0.050(5) 0.068(6) 0.114(8) 0.028(5) 0.044(5) 0.031(4) C59 0.053(5) 0.071(6) 0.130(9) 0.043(6) 0.024(6) 0.020(5) C60 0.074(7) 0.050(6) 0.182(13) 0.049(7) 0.012(8) -0.006(5) C61 0.093(7) 0.036(4) 0.109(8) -0.001(5) 0.071(6) -0.010(4) N2 0.150(9) 0.153(10) 0.127(9) -0.027(7) 0.103(8) -0.054(8) C62 0.094(7) 0.072(6) 0.078(7) 0.000(5) 0.059(6) -0.001(5) C63 0.164(11) 0.162(11) 0.116(9) 0.085(8) 0.117(9) 0.108(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C28 2.048(6) . ? Fe1 C2 2.049(6) . ? Fe1 C29 2.052(5) . ? Fe1 C30 2.053(6) . ? Fe1 C31 2.057(6) . ? Fe1 C32 2.058(6) . ? Fe1 C3 2.060(6) . ? Fe1 C4 2.097(5) . ? Fe1 C1 2.106(6) . ? Fe1 P1 2.2783(16) . ? K1 O3 2.741(4) . ? K1 O9 2.811(4) . ? K1 O10 2.838(4) . ? K1 O5 2.839(4) . ? K1 O7 2.872(4) . ? K1 O8 2.874(4) . ? K1 O6 2.904(5) . ? K1 C15 3.458(6) . ? K1 C14 3.508(7) . ? K1 C16 3.534(6) . ? K2 O15 2.767(4) . ? K2 O12 2.768(5) . ? K2 O14 2.786(5) . ? K2 O16 2.856(5) . ? K2 O11 2.900(5) . ? K2 O13 2.942(6) . ? K2 C18 3.071(6) . ? K2 C17 3.307(6) . ? K2 C19 3.411(6) . ? K2 C54 3.535(9) . ? P1 C1 1.775(6) . ? P1 C4 1.785(6) . ? P2 C6 1.752(6) . ? P2 C9 1.759(6) . ? P3 C17 1.752(6) . ? P3 C20 1.757(5) . ? O1 C5 1.244(7) . ? O2 C10 1.244(7) . ? O3 C16 1.237(7) . ? O4 C21 1.238(6) . ? O5 C49 1.420(8) . ? O5 C38 1.425(8) . ? O6 C40 1.421(8) . ? O6 C39 1.430(8) . ? O7 C41 1.418(8) . ? O7 C42 1.420(8) . ? O8 C43 1.425(7) . ? O8 C44 1.431(8) . ? O9 C46 1.425(7) . ? O9 C45 1.425(7) . ? O10 C48 1.422(7) . ? O10 C47 1.422(8) . ? O11 C50 1.284(9) . ? O11 C61 1.367(9) . ? O12 C52 1.320(9) . ? O12 C51 1.361(9) . ? O13 C54 1.242(9) . ? O13 C53 1.305(9) . ? O14 C55 1.384(9) . ? O14 C56 1.394(8) . ? O15 C57 1.391(8) . ? O15 C58 1.391(9) . ? O16 C60 1.269(11) . ? O16 C59 1.349(9) . ? N1 C15 1.337(7) . ? N1 C11 1.356(7) . ? C1 C2 1.431(8) . ? C1 C21 1.490(8) . ? C2 C3 1.421(8) . ? C2 C22 1.507(8) . ? C3 C4 1.433(8) . ? C3 C23 1.515(8) . ? C4 C5 1.502(8) . ? C5 C6 1.456(8) . ? C6 C7 1.426(8) . ? C7 C8 1.401(8) . ? C7 C24 1.512(8) . ? C8 C9 1.427(9) . ? C8 C25 1.518(9) . ? C9 C10 1.423(8) . ? C10 C11 1.530(8) . ? C11 C12 1.380(8) . ? C12 C13 1.373(9) . ? C12 H12 0.9500 . ? C13 C14 1.388(8) . ? C13 H13 0.9500 . ? C14 C15 1.383(8) . ? C14 H14 0.9500 . ? C15 C16 1.536(8) . ? C16 C17 1.438(8) . ? C17 C18 1.444(7) . ? C18 C19 1.385(8) . ? C18 C26 1.498(8) . ? C19 C20 1.416(8) . ? C19 C27 1.505(8) . ? C20 C21 1.472(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.400(9) . ? C28 C32 1.427(9) . ? C28 C33 1.501(9) . ? C29 C30 1.431(9) . ? C29 C34 1.496(9) . ? C30 C31 1.418(10) . ? C30 C35 1.512(9) . ? C31 C32 1.406(10) . ? C31 C36 1.512(10) . ? C32 C37 1.505(10) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.501(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.503(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.483(10) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.482(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.491(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.496(10) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.4944(10) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.4940(10) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.4940(10) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.4948(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.4940(10) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.4941(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? N2 C62 1.101(11) . ? C62 C63 1.407(13) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? 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 C28 Fe1 C2 123.2(3) . . ? C28 Fe1 C29 39.9(2) . . ? C2 Fe1 C29 106.8(2) . . ? C28 Fe1 C30 67.7(2) . . ? C2 Fe1 C30 121.7(3) . . ? C29 Fe1 C30 40.8(3) . . ? C28 Fe1 C31 67.8(3) . . ? C2 Fe1 C31 157.7(3) . . ? C29 Fe1 C31 68.1(3) . . ? C30 Fe1 C31 40.4(3) . . ? C28 Fe1 C32 40.7(3) . . ? C2 Fe1 C32 160.3(3) . . ? C29 Fe1 C32 67.9(3) . . ? C30 Fe1 C32 67.6(3) . . ? C31 Fe1 C32 40.0(3) . . ? C28 Fe1 C3 158.9(3) . . ? C2 Fe1 C3 40.5(2) . . ? C29 Fe1 C3 123.0(2) . . ? C30 Fe1 C3 107.4(2) . . ? C31 Fe1 C3 122.7(3) . . ? C32 Fe1 C3 158.4(3) . . ? C28 Fe1 C4 160.0(3) . . ? C2 Fe1 C4 69.5(2) . . ? C29 Fe1 C4 157.7(2) . . ? C30 Fe1 C4 121.1(2) . . ? C31 Fe1 C4 106.4(2) . . ? C32 Fe1 C4 122.7(2) . . ? C3 Fe1 C4 40.3(2) . . ? C28 Fe1 C1 106.3(2) . . ? C2 Fe1 C1 40.3(2) . . ? C29 Fe1 C1 119.4(2) . . ? C30 Fe1 C1 155.6(3) . . ? C31 Fe1 C1 161.4(3) . . ? C32 Fe1 C1 124.2(3) . . ? C3 Fe1 C1 69.3(2) . . ? C4 Fe1 C1 72.9(2) . . ? C28 Fe1 P1 116.39(18) . . ? C2 Fe1 P1 76.57(16) . . ? C29 Fe1 P1 154.24(19) . . ? C30 Fe1 P1 156.8(2) . . ? C31 Fe1 P1 117.9(2) . . ? C32 Fe1 P1 99.99(19) . . ? C3 Fe1 P1 76.63(16) . . ? C4 Fe1 P1 47.95(16) . . ? C1 Fe1 P1 47.55(15) . . ? O3 K1 O9 80.25(13) . . ? O3 K1 O10 70.94(13) . . ? O9 K1 O10 59.08(12) . . ? O3 K1 O5 79.61(13) . . ? O9 K1 O5 118.96(13) . . ? O10 K1 O5 59.89(13) . . ? O3 K1 O7 137.31(13) . . ? O9 K1 O7 116.96(13) . . ? O10 K1 O7 151.75(13) . . ? O5 K1 O7 116.76(13) . . ? O3 K1 O8 119.71(14) . . ? O9 K1 O8 59.09(12) . . ? O10 K1 O8 113.04(13) . . ? O5 K1 O8 157.58(14) . . ? O7 K1 O8 58.07(12) . . ? O3 K1 O6 122.85(13) . . ? O9 K1 O6 152.43(14) . . ? O10 K1 O6 110.97(13) . . ? O5 K1 O6 58.65(13) . . ? O7 K1 O6 58.11(13) . . ? O8 K1 O6 111.53(13) . . ? O3 K1 C15 42.27(12) . . ? O9 K1 C15 113.23(14) . . ? O10 K1 C15 110.32(13) . . ? O5 K1 C15 86.50(14) . . ? O7 K1 C15 96.98(13) . . ? O8 K1 C15 115.27(14) . . ? O6 K1 C15 94.29(14) . . ? O3 K1 C14 54.34(13) . . ? O9 K1 C14 104.11(15) . . ? O10 K1 C14 125.14(14) . . ? O5 K1 C14 108.99(14) . . ? O7 K1 C14 83.05(14) . . ? O8 K1 C14 92.47(14) . . ? O6 K1 C14 102.09(15) . . ? C15 K1 C14 22.88(14) . . ? O3 K1 C16 17.53(12) . . ? O9 K1 C16 96.01(13) . . ? O10 K1 C16 85.64(13) . . ? O5 K1 C16 78.35(13) . . ? O7 K1 C16 122.14(13) . . ? O8 K1 C16 123.60(14) . . ? O6 K1 C16 109.32(13) . . ? C15 K1 C16 25.35(12) . . ? C14 K1 C16 41.61(13) . . ? O15 K2 O12 158.33(16) . . ? O15 K2 O14 60.16(14) . . ? O12 K2 O14 112.28(15) . . ? O15 K2 O16 59.00(14) . . ? O12 K2 O16 113.86(15) . . ? O14 K2 O16 113.35(15) . . ? O15 K2 O11 115.91(16) . . ? O12 K2 O11 58.04(15) . . ? O14 K2 O11 147.31(19) . . ? O16 K2 O11 57.45(15) . . ? O15 K2 O13 118.47(16) . . ? O12 K2 O13 57.11(16) . . ? O14 K2 O13 58.38(15) . . ? O16 K2 O13 152.62(19) . . ? O11 K2 O13 113.56(17) . . ? O15 K2 C18 101.50(16) . . ? O12 K2 C18 99.78(15) . . ? O14 K2 C18 118.20(15) . . ? O16 K2 C18 98.06(16) . . ? O11 K2 C18 94.48(18) . . ? O13 K2 C18 108.77(19) . . ? O15 K2 C17 80.49(15) . . ? O12 K2 C17 121.11(15) . . ? O14 K2 C17 94.59(15) . . ? O16 K2 C17 99.88(15) . . ? O11 K2 C17 117.39(18) . . ? O13 K2 C17 106.61(18) . . ? C18 K2 C17 25.83(13) . . ? O15 K2 C19 121.40(15) . . ? O12 K2 C19 80.23(14) . . ? O14 K2 C19 114.12(15) . . ? O16 K2 C19 118.82(16) . . ? O11 K2 C19 95.71(18) . . ? O13 K2 C19 86.54(18) . . ? C18 K2 C19 23.95(14) . . ? C17 K2 C19 40.91(13) . . ? O15 K2 C54 102.08(16) . . ? O12 K2 C54 76.32(17) . . ? O14 K2 C54 42.70(16) . . ? O16 K2 C54 153.4(2) . . ? O11 K2 C54 132.99(19) . . ? O13 K2 C54 19.48(17) . . ? C18 K2 C54 104.4(3) . . ? C17 K2 C54 94.4(2) . . ? C19 K2 C54 86.4(2) . . ? C1 P1 C4 89.1(3) . . ? C1 P1 Fe1 61.13(18) . . ? C4 P1 Fe1 60.69(17) . . ? C6 P2 C9 90.6(3) . . ? C17 P3 C20 90.3(3) . . ? C16 O3 K1 120.6(4) . . ? C49 O5 C38 111.5(5) . . ? C49 O5 K1 116.1(4) . . ? C38 O5 K1 119.8(4) . . ? C40 O6 C39 112.4(5) . . ? C40 O6 K1 115.6(4) . . ? C39 O6 K1 108.2(4) . . ? C41 O7 C42 112.1(5) . . ? C41 O7 K1 117.2(4) . . ? C42 O7 K1 118.0(4) . . ? C43 O8 C44 112.7(5) . . ? C43 O8 K1 109.1(4) . . ? C44 O8 K1 110.9(3) . . ? C46 O9 C45 111.6(5) . . ? C46 O9 K1 119.5(4) . . ? C45 O9 K1 118.3(3) . . ? C48 O10 C47 111.4(5) . . ? C48 O10 K1 111.3(3) . . ? C47 O10 K1 111.4(4) . . ? C50 O11 C61 115.3(6) . . ? C50 O11 K2 117.7(5) . . ? C61 O11 K2 119.0(4) . . ? C52 O12 C51 113.0(6) . . ? C52 O12 K2 121.9(5) . . ? C51 O12 K2 122.1(4) . . ? C54 O13 C53 122.5(7) . . ? C54 O13 K2 108.3(6) . . ? C53 O13 K2 107.8(5) . . ? C55 O14 C56 113.0(5) . . ? C55 O14 K2 118.7(4) . . ? C56 O14 K2 115.5(4) . . ? C57 O15 C58 109.2(5) . . ? C57 O15 K2 117.9(4) . . ? C58 O15 K2 120.2(4) . . ? C60 O16 C59 116.9(6) . . ? C60 O16 K2 121.2(5) . . ? C59 O16 K2 113.3(5) . . ? C15 N1 C11 117.4(5) . . ? C2 C1 C21 126.2(5) . . ? C2 C1 P1 113.4(4) . . ? C21 C1 P1 120.3(4) . . ? C2 C1 Fe1 67.7(3) . . ? C21 C1 Fe1 129.2(4) . . ? P1 C1 Fe1 71.3(2) . . ? C3 C2 C1 112.3(5) . . ? C3 C2 C22 123.8(5) . . ? C1 C2 C22 123.7(5) . . ? C3 C2 Fe1 70.2(3) . . ? C1 C2 Fe1 72.0(3) . . ? C22 C2 Fe1 130.2(4) . . ? C2 C3 C4 111.9(5) . . ? C2 C3 C23 123.7(5) . . ? C4 C3 C23 124.3(5) . . ? C2 C3 Fe1 69.3(3) . . ? C4 C3 Fe1 71.2(3) . . ? C23 C3 Fe1 130.2(4) . . ? C3 C4 C5 128.3(5) . . ? C3 C4 P1 113.3(4) . . ? C5 C4 P1 118.4(4) . . ? C3 C4 Fe1 68.5(3) . . ? C5 C4 Fe1 128.3(4) . . ? P1 C4 Fe1 71.36(19) . . ? O1 C5 C6 124.1(5) . . ? O1 C5 C4 121.1(5) . . ? C6 C5 C4 114.7(5) . . ? C7 C6 C5 127.3(5) . . ? C7 C6 P2 112.5(4) . . ? C5 C6 P2 120.2(4) . . ? C8 C7 C6 112.1(5) . . ? C8 C7 C24 123.2(6) . . ? C6 C7 C24 124.5(5) . . ? C7 C8 C9 113.0(5) . . ? C7 C8 C25 122.8(6) . . ? C9 C8 C25 124.2(6) . . ? C10 C9 C8 128.2(5) . . ? C10 C9 P2 119.5(5) . . ? C8 C9 P2 111.7(4) . . ? O2 C10 C9 126.3(6) . . ? O2 C10 C11 114.2(5) . . ? C9 C10 C11 119.5(5) . . ? N1 C11 C12 122.1(6) . . ? N1 C11 C10 119.2(5) . . ? C12 C11 C10 118.6(5) . . ? C13 C12 C11 120.0(6) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 118.5(6) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 118.5(6) . . ? C15 C14 K1 76.5(4) . . ? C13 C14 K1 105.1(4) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? K1 C14 H14 88.5 . . ? N1 C15 C14 123.6(5) . . ? N1 C15 C16 118.2(5) . . ? C14 C15 C16 117.9(5) . . ? N1 C15 K1 103.1(3) . . ? C14 C15 K1 80.6(4) . . ? C16 C15 K1 80.1(3) . . ? O3 C16 C17 126.6(5) . . ? O3 C16 C15 114.2(5) . . ? C17 C16 C15 119.3(5) . . ? O3 C16 K1 41.9(3) . . ? C17 C16 K1 161.3(4) . . ? C15 C16 K1 74.6(3) . . ? C16 C17 C18 127.4(5) . . ? C16 C17 P3 120.6(4) . . ? C18 C17 P3 111.8(4) . . ? C16 C17 K2 107.2(3) . . ? C18 C17 K2 67.9(3) . . ? P3 C17 K2 97.7(2) . . ? C19 C18 C17 112.3(5) . . ? C19 C18 C26 123.0(5) . . ? C17 C18 C26 124.6(5) . . ? C19 C18 K2 91.9(4) . . ? C17 C18 K2 86.3(3) . . ? C26 C18 K2 94.6(4) . . ? C18 C19 C20 113.1(5) . . ? C18 C19 C27 122.7(5) . . ? C20 C19 C27 123.9(5) . . ? C18 C19 K2 64.1(3) . . ? C20 C19 K2 97.4(3) . . ? C27 C19 K2 109.9(4) . . ? C19 C20 C21 126.2(5) . . ? C19 C20 P3 112.4(4) . . ? C21 C20 P3 121.3(4) . . ? O4 C21 C20 123.6(5) . . ? O4 C21 C1 122.4(5) . . ? C20 C21 C1 114.0(5) . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C23 H23A 109.5 . . ? C3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C7 C24 H24A 109.5 . . ? C7 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C7 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C8 C25 H25A 109.5 . . ? C8 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C8 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C18 C26 H26A 109.5 . . ? C18 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C18 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C19 C27 H27A 109.5 . . ? C19 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C19 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C32 108.6(6) . . ? C29 C28 C33 126.1(7) . . ? C32 C28 C33 125.3(7) . . ? C29 C28 Fe1 70.2(3) . . ? C32 C28 Fe1 70.0(3) . . ? C33 C28 Fe1 127.9(5) . . ? C28 C29 C30 107.6(6) . . ? C28 C29 C34 126.5(6) . . ? C30 C29 C34 125.8(6) . . ? C28 C29 Fe1 69.9(3) . . ? C30 C29 Fe1 69.6(3) . . ? C34 C29 Fe1 129.0(5) . . ? C31 C30 C29 107.8(6) . . ? C31 C30 C35 125.6(7) . . ? C29 C30 C35 126.5(7) . . ? C31 C30 Fe1 70.0(4) . . ? C29 C30 Fe1 69.6(3) . . ? C35 C30 Fe1 128.5(5) . . ? C32 C31 C30 108.2(6) . . ? C32 C31 C36 125.4(8) . . ? C30 C31 C36 126.2(8) . . ? C32 C31 Fe1 70.0(4) . . ? C30 C31 Fe1 69.7(4) . . ? C36 C31 Fe1 128.9(5) . . ? C31 C32 C28 107.7(6) . . ? C31 C32 C37 127.2(7) . . ? C28 C32 C37 125.0(7) . . ? C31 C32 Fe1 70.0(4) . . ? C28 C32 Fe1 69.3(4) . . ? C37 C32 Fe1 128.8(5) . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O5 C38 C39 109.2(6) . . ? O5 C38 H38A 109.8 . . ? C39 C38 H38A 109.8 . . ? O5 C38 H38B 109.8 . . ? C39 C38 H38B 109.8 . . ? H38A C38 H38B 108.3 . . ? O6 C39 C38 109.0(5) . . ? O6 C39 H39A 109.9 . . ? C38 C39 H39A 109.9 . . ? O6 C39 H39B 109.9 . . ? C38 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? O6 C40 C41 108.3(5) . . ? O6 C40 H40A 110.0 . . ? C41 C40 H40A 110.0 . . ? O6 C40 H40B 110.0 . . ? C41 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? O7 C41 C40 109.4(5) . . ? O7 C41 H41A 109.8 . . ? C40 C41 H41A 109.8 . . ? O7 C41 H41B 109.8 . . ? C40 C41 H41B 109.8 . . ? H41A C41 H41B 108.2 . . ? O7 C42 C43 109.4(5) . . ? O7 C42 H42A 109.8 . . ? C43 C42 H42A 109.8 . . ? O7 C42 H42B 109.8 . . ? C43 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? O8 C43 C42 107.2(6) . . ? O8 C43 H43A 110.3 . . ? C42 C43 H43A 110.3 . . ? O8 C43 H43B 110.3 . . ? C42 C43 H43B 110.3 . . ? H43A C43 H43B 108.5 . . ? O8 C44 C45 108.1(5) . . ? O8 C44 H44A 110.1 . . ? C45 C44 H44A 110.1 . . ? O8 C44 H44B 110.1 . . ? C45 C44 H44B 110.1 . . ? H44A C44 H44B 108.4 . . ? O9 C45 C44 109.0(5) . . ? O9 C45 H45A 109.9 . . ? C44 C45 H45A 109.9 . . ? O9 C45 H45B 109.9 . . ? C44 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? O9 C46 C47 108.7(5) . . ? O9 C46 H46A 110.0 . . ? C47 C46 H46A 110.0 . . ? O9 C46 H46B 110.0 . . ? C47 C46 H46B 110.0 . . ? H46A C46 H46B 108.3 . . ? O10 C47 C46 109.5(5) . . ? O10 C47 H47A 109.8 . . ? C46 C47 H47A 109.8 . . ? O10 C47 H47B 109.8 . . ? C46 C47 H47B 109.8 . . ? H47A C47 H47B 108.2 . . ? O10 C48 C49 108.9(5) . . ? O10 C48 H48A 109.9 . . ? C49 C48 H48A 109.9 . . ? O10 C48 H48B 109.9 . . ? C49 C48 H48B 109.9 . . ? H48A C48 H48B 108.3 . . ? O5 C49 C48 108.9(6) . . ? O5 C49 H49A 109.9 . . ? C48 C49 H49A 109.9 . . ? O5 C49 H49B 109.9 . . ? C48 C49 H49B 109.9 . . ? H49A C49 H49B 108.3 . . ? O11 C50 C51 117.3(7) . . ? O11 C50 H50A 108.0 . . ? C51 C50 H50A 108.0 . . ? O11 C50 H50B 108.0 . . ? C51 C50 H50B 108.0 . . ? H50A C50 H50B 107.2 . . ? O12 C51 C50 113.5(7) . . ? O12 C51 H51A 108.9 . . ? C50 C51 H51A 108.9 . . ? O12 C51 H51B 108.9 . . ? C50 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? O12 C52 C53 114.3(7) . . ? O12 C52 H52A 108.7 . . ? C53 C52 H52A 108.7 . . ? O12 C52 H52B 108.7 . . ? C53 C52 H52B 108.7 . . ? H52A C52 H52B 107.6 . . ? O13 C53 C52 119.3(7) . . ? O13 C53 H53A 107.5 . . ? C52 C53 H53A 107.5 . . ? O13 C53 H53B 107.5 . . ? C52 C53 H53B 107.5 . . ? H53A C53 H53B 107.0 . . ? O13 C54 C55 125.4(8) . . ? O13 C54 K2 52.2(5) . . ? C55 C54 K2 82.6(5) . . ? O13 C54 H54A 106.0 . . ? C55 C54 H54A 106.0 . . ? K2 C54 H54A 93.9 . . ? O13 C54 H54B 106.0 . . ? C55 C54 H54B 106.0 . . ? K2 C54 H54B 154.4 . . ? H54A C54 H54B 106.3 . . ? O14 C55 C54 113.3(6) . . ? O14 C55 H55A 108.9 . . ? C54 C55 H55A 108.9 . . ? O14 C55 H55B 108.9 . . ? C54 C55 H55B 108.9 . . ? H55A C55 H55B 107.7 . . ? O14 C56 C57 111.2(6) . . ? O14 C56 H56A 109.4 . . ? C57 C56 H56A 109.4 . . ? O14 C56 H56B 109.4 . . ? C57 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? O15 C57 C56 110.7(6) . . ? O15 C57 H57A 109.5 . . ? C56 C57 H57A 109.5 . . ? O15 C57 H57B 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 108.1 . . ? O15 C58 C59 113.1(6) . . ? O15 C58 H58A 109.0 . . ? C59 C58 H58A 109.0 . . ? O15 C58 H58B 109.0 . . ? C59 C58 H58B 109.0 . . ? H58A C58 H58B 107.8 . . ? O16 C59 C58 111.6(7) . . ? O16 C59 H59A 109.3 . . ? C58 C59 H59A 109.3 . . ? O16 C59 H59B 109.3 . . ? C58 C59 H59B 109.3 . . ? H59A C59 H59B 108.0 . . ? O16 C60 C61 117.6(8) . . ? O16 C60 H60A 107.9 . . ? C61 C60 H60A 107.9 . . ? O16 C60 H60B 107.9 . . ? C61 C60 H60B 107.9 . . ? H60A C60 H60B 107.2 . . ? O11 C61 C60 115.2(7) . . ? O11 C61 H61A 108.5 . . ? C60 C61 H61A 108.5 . . ? O11 C61 H61B 108.5 . . ? C60 C61 H61B 108.5 . . ? H61A C61 H61B 107.5 . . ? N2 C62 C63 178.1(13) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.641 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.081 #===END