Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ; Dinuclear iron complexes based on parallel ?-diiminato binding sites: syntheses, structures and reaction with O2 ; _publ_contact_author_name 'Christian Limberg' _publ_contact_author_email CHRISTIAN.LIMBERG@CHEMIE.HU-BERLIN.DE loop_ _publ_author_name C.Limberg S.Demeshko F.Meyer M.F.Pilz B.Ziemer # Attachment '1.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 663093' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(C6H3Me2)Xanthdim]Fe2Cl3(Li(thf)3) ; _chemical_name_common ((C6H3Me2)Xanthdim)Fe2Cl3(Li(thf)3) _chemical_melting_point ? _chemical_formula_moiety 'C73 H92 Cl3 Fe2 Li N4 O4' _chemical_formula_sum 'C73 H92 Cl3 Fe2 Li N4 O4' _chemical_formula_weight 1314.50 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' Cl Cl 0.1484 0.1585 '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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.644(3) _cell_length_b 13.398(3) _cell_length_c 24.910(5) _cell_angle_alpha 90.309(18) _cell_angle_beta 94.277(19) _cell_angle_gamma 112.626(18) _cell_volume 3574.4(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 22 _exptl_crystal_description lath _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method none _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.566 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8761 _exptl_absorpt_correction_T_max 0.9561 _exptl_absorpt_process_details ; The crystal faces were indexed by microscope on the diffractometer. After that a numerical absorption correction basing on a Gaussian algorithsm was applied, which is implemented in the X-RED program (Stoe, 2002). ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a 2-circle goniometer supplied with an area detector. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'long fine focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_collimation '0.5 mm diameter monocapillary' _diffrn_measurement_device 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,240 exposures' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45190 _diffrn_reflns_av_R_equivalents 0.3793 _diffrn_reflns_av_sigmaI/netI 0.3346 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 22.50 _reflns_number_total 9315 _reflns_number_gt 3355 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0916P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9315 _refine_ls_number_parameters 785 _refine_ls_number_restraints 121 _refine_ls_R_factor_all 0.2905 _refine_ls_R_factor_gt 0.1411 _refine_ls_wR_factor_ref 0.3207 _refine_ls_wR_factor_gt 0.2500 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1812(8) 0.4853(6) 0.0875(3) 0.033(3) Uani 1 1 d . . . C2 C 0.1284(9) 0.3791(8) 0.0999(4) 0.049(3) Uani 1 1 d . . . C3 C 0.1068(8) 0.2990(6) 0.0582(3) 0.034(3) Uani 1 1 d . . . H3A H 0.0723 0.2248 0.0667 0.040 Uiso 1 1 calc R . . C4 C 0.1342(7) 0.3256(7) 0.0060(3) 0.030(3) Uani 1 1 d . . . C5 C 0.1892(8) 0.4350(7) -0.0043(3) 0.039(3) Uani 1 1 d . . . H5A H 0.2131 0.4553 -0.0395 0.047 Uiso 1 1 calc R . . C6 C 0.2110(8) 0.5166(6) 0.0352(4) 0.036(3) Uani 1 1 d . . . C7 C 0.2746(8) 0.6361(6) 0.0195(3) 0.032(3) Uani 1 1 d . . . C8 C 0.2838(7) 0.7103(6) 0.0674(3) 0.033(3) Uani 1 1 d . . . C9 C 0.3351(8) 0.8241(7) 0.0635(3) 0.041(3) Uani 1 1 d . . . H9A H 0.3680 0.8552 0.0310 0.050 Uiso 1 1 calc R . . C10 C 0.3378(11) 0.8902(8) 0.1066(4) 0.058(4) Uani 1 1 d . . . C11 C 0.2909(9) 0.8468(7) 0.1536(3) 0.040(3) Uani 1 1 d . . . H11A H 0.2940 0.8945 0.1826 0.049 Uiso 1 1 calc R . . C12 C 0.2385(8) 0.7356(6) 0.1610(3) 0.033(2) Uiso 1 1 d . . . C13 C 0.2410(8) 0.6706(6) 0.1171(4) 0.037(3) Uani 1 1 d . . . C14 C 0.1148(7) 0.2376(6) -0.0391(3) 0.026(2) Uani 1 1 d . . . C15 C 0.0471(11) 0.1257(7) -0.0203(4) 0.065(4) Uani 1 1 d . . . H15A H -0.0394 0.1151 -0.0152 0.078 Uiso 1 1 calc R . . H15B H 0.0885 0.1162 0.0138 0.078 Uiso 1 1 calc R . . H15C H 0.0478 0.0727 -0.0474 0.078 Uiso 1 1 calc R . . C16 C 0.0367(10) 0.2565(9) -0.0864(4) 0.063(4) Uani 1 1 d . . . H16A H 0.0814 0.3281 -0.1004 0.075 Uiso 1 1 calc R . . H16B H -0.0431 0.2528 -0.0744 0.075 Uiso 1 1 calc R . . H16C H 0.0213 0.2009 -0.1147 0.075 Uiso 1 1 calc R . . C17 C 0.2413(9) 0.2481(8) -0.0535(4) 0.064(4) Uani 1 1 d . . . H17A H 0.2875 0.2343 -0.0219 0.077 Uiso 1 1 calc R . . H17B H 0.2868 0.3215 -0.0654 0.077 Uiso 1 1 calc R . . H17C H 0.2324 0.1956 -0.0826 0.077 Uiso 1 1 calc R . . C18 C 0.1882(8) 0.6564(6) -0.0269(3) 0.039(3) Uani 1 1 d . . . H18A H 0.1031 0.6338 -0.0157 0.047 Uiso 1 1 calc R . . H18B H 0.1873 0.6144 -0.0594 0.047 Uiso 1 1 calc R . . H18C H 0.2201 0.7335 -0.0345 0.047 Uiso 1 1 calc R . . C19 C 0.4033(8) 0.6576(7) 0.0030(4) 0.045(3) Uani 1 1 d . . . H19A H 0.4480 0.7355 -0.0010 0.054 Uiso 1 1 calc R . . H19B H 0.3969 0.6192 -0.0314 0.054 Uiso 1 1 calc R . . H19C H 0.4490 0.6321 0.0306 0.054 Uiso 1 1 calc R . . C20 C 0.3948(8) 1.0170(7) 0.0989(3) 0.040(3) Uani 1 1 d . . . C21 C 0.3201(9) 1.0458(7) 0.0500(4) 0.055(3) Uani 1 1 d . . . H21A H 0.2313 1.0189 0.0562 0.066 Uiso 1 1 calc R . . H21B H 0.3304 1.0119 0.0167 0.066 Uiso 1 1 calc R . . H21C H 0.3521 1.1245 0.0466 0.066 Uiso 1 1 calc R . . C22 C 0.5274(9) 1.0535(7) 0.0870(4) 0.053(3) Uani 1 1 d . . . H22A H 0.5344 1.0092 0.0569 0.063 Uiso 1 1 calc R . . H22B H 0.5774 1.0457 0.1189 0.063 Uiso 1 1 calc R . . H22C H 0.5580 1.1295 0.0773 0.063 Uiso 1 1 calc R . . C23 C 0.3854(11) 1.0789(8) 0.1472(4) 0.065(4) Uani 1 1 d . . . H23A H 0.4318 1.0639 0.1785 0.079 Uiso 1 1 calc R . . H23B H 0.2975 1.0569 0.1543 0.079 Uiso 1 1 calc R . . H23C H 0.4208 1.1566 0.1407 0.079 Uiso 1 1 calc R . . C24 C 0.1787(7) 0.6914(6) 0.2099(3) 0.023(2) Uani 1 1 d . . . C25 C 0.2396(8) 0.7342(7) 0.2595(3) 0.037(3) Uani 1 1 d . . . H25A H 0.3216 0.7885 0.2603 0.044 Uiso 1 1 calc R . . C26 C 0.2715(9) 0.7699(7) 0.3522(3) 0.043(3) Uani 1 1 d . . . C27 C 0.3047(9) 0.8807(7) 0.3572(3) 0.044(3) Uani 1 1 d . . . C28 C 0.3862(9) 0.9429(8) 0.3984(4) 0.049(3) Uani 1 1 d . . . C29 C 0.4373(9) 0.8878(9) 0.4363(4) 0.063(4) Uani 1 1 d . . . H29A H 0.4977 0.9287 0.4641 0.075 Uiso 1 1 calc R . . C30 C 0.4023(11) 0.7805(9) 0.4334(4) 0.068(4) Uani 1 1 d . . . H30A H 0.4332 0.7456 0.4606 0.081 Uiso 1 1 calc R . . C31 C 0.3198(9) 0.7188(8) 0.3904(3) 0.053(3) Uani 1 1 d . . . H31A H 0.2974 0.6427 0.3876 0.064 Uiso 1 1 calc R . . C32 C 0.2497(10) 0.9390(8) 0.3147(4) 0.064(4) Uani 1 1 d . . . H32A H 0.1799 0.8851 0.2927 0.077 Uiso 1 1 calc R . . H32B H 0.3146 0.9805 0.2915 0.077 Uiso 1 1 calc R . . H32C H 0.2200 0.9881 0.3332 0.077 Uiso 1 1 calc R . . C33 C 0.4240(13) 1.0625(9) 0.4054(4) 0.091(5) Uani 1 1 d . . . H33C H 0.4860 1.0897 0.4364 0.110 Uiso 1 1 calc R . . H33B H 0.3505 1.0784 0.4116 0.110 Uiso 1 1 calc R . . H33A H 0.4602 1.0978 0.3729 0.110 Uiso 1 1 calc R . . C34 C 0.0521(7) 0.6177(7) 0.2033(3) 0.033(3) Uani 1 1 d . . . H34A H 0.0203 0.5977 0.1669 0.039 Uiso 1 1 calc R . . C35 C -0.1546(7) 0.5183(6) 0.2158(3) 0.025(2) Uiso 1 1 d . . . C36 C -0.2394(7) 0.5636(6) 0.2070(3) 0.025(2) Uiso 1 1 d . . . C37 C -0.3550(8) 0.5082(7) 0.1807(3) 0.038(3) Uani 1 1 d . . . C38 C -0.3889(8) 0.4006(7) 0.1641(4) 0.050(3) Uani 1 1 d . . . H38A H -0.4691 0.3624 0.1461 0.060 Uiso 1 1 calc R . . C39 C -0.3100(9) 0.3494(8) 0.1732(4) 0.060(4) Uani 1 1 d . . . H39A H -0.3336 0.2761 0.1614 0.072 Uiso 1 1 calc R . . C40 C -0.1927(10) 0.4062(8) 0.2004(4) 0.056(4) Uani 1 1 d . . . H40A H -0.1379 0.3701 0.2087 0.067 Uiso 1 1 calc R . . C41 C -0.1958(10) 0.6842(7) 0.2245(4) 0.061(4) Uani 1 1 d . . . H41A H -0.1784 0.7286 0.1927 0.073 Uiso 1 1 calc R . . H41B H -0.1198 0.7051 0.2490 0.073 Uiso 1 1 calc R . . H41C H -0.2615 0.6954 0.2430 0.073 Uiso 1 1 calc R . . C42 C -0.4445(8) 0.5652(8) 0.1664(4) 0.057(3) Uani 1 1 d . . . H42A H -0.3968 0.6392 0.1560 0.068 Uiso 1 1 calc R . . H42B H -0.4899 0.5672 0.1977 0.068 Uiso 1 1 calc R . . H42C H -0.5042 0.5254 0.1363 0.068 Uiso 1 1 calc R . . C43 C 0.1096(8) 0.3451(6) 0.1575(3) 0.033(3) Uani 1 1 d . . . C44 C 0.2113(9) 0.3955(7) 0.1953(3) 0.039(3) Uani 1 1 d . . . H44A H 0.2823 0.4504 0.1824 0.047 Uiso 1 1 calc R . . C45 C 0.3383(8) 0.4280(6) 0.2753(3) 0.039(3) Uani 1 1 d . . . C46 C 0.4201(9) 0.3758(7) 0.2866(3) 0.039(3) Uani 1 1 d . . . C47 C 0.5359(8) 0.4280(7) 0.3144(3) 0.038(3) Uani 1 1 d . . . C48 C 0.5740(10) 0.5364(8) 0.3320(4) 0.060(4) Uani 1 1 d . . . H48A H 0.6530 0.5728 0.3514 0.072 Uiso 1 1 calc R . . C49 C 0.4942(9) 0.5892(9) 0.3206(4) 0.055(4) Uani 1 1 d . . . H49A H 0.5186 0.6629 0.3317 0.066 Uiso 1 1 calc R . . C50 C 0.3803(9) 0.5353(8) 0.2933(4) 0.046(3) Uani 1 1 d . . . H50A H 0.3269 0.5732 0.2864 0.056 Uiso 1 1 calc R . . C51 C 0.3837(9) 0.2580(7) 0.2663(4) 0.052(3) Uani 1 1 d . . . H51A H 0.3245 0.2430 0.2343 0.063 Uiso 1 1 calc R . . H51B H 0.3448 0.2088 0.2946 0.063 Uiso 1 1 calc R . . H51C H 0.4585 0.2473 0.2571 0.063 Uiso 1 1 calc R . . C52 C 0.6245(10) 0.3720(8) 0.3275(4) 0.063(4) Uani 1 1 d . . . H52C H 0.7039 0.4246 0.3441 0.075 Uiso 1 1 calc R . . H52B H 0.6392 0.3408 0.2944 0.075 Uiso 1 1 calc R . . H52A H 0.5879 0.3144 0.3526 0.075 Uiso 1 1 calc R . . C53 C -0.0029(8) 0.2681(7) 0.1705(3) 0.037(3) Uani 1 1 d . . . H53A H -0.0644 0.2374 0.1413 0.044 Uiso 1 1 calc R . . C54 C -0.1537(8) 0.1486(7) 0.2271(3) 0.041(3) Uani 1 1 d . . . C55 C -0.1968(9) 0.0528(8) 0.1984(4) 0.053(3) Uani 1 1 d . . . C56 C -0.3168(9) -0.0261(8) 0.2081(4) 0.047(3) Uani 1 1 d . . . C57 C -0.3850(10) -0.0011(8) 0.2444(5) 0.068(4) Uani 1 1 d . . . H57A H -0.4653 -0.0536 0.2500 0.081 Uiso 1 1 calc R . . C58 C -0.3431(10) 0.0971(9) 0.2738(4) 0.066(4) Uani 1 1 d . . . H58A H -0.3936 0.1132 0.2980 0.080 Uiso 1 1 calc R . . C59 C -0.2225(9) 0.1706(8) 0.2657(4) 0.050(3) Uani 1 1 d . . . H59A H -0.1872 0.2363 0.2867 0.060 Uiso 1 1 calc R . . C60 C -0.1208(8) 0.0244(7) 0.1623(4) 0.050(3) Uani 1 1 d . . . H60A H -0.0323 0.0649 0.1735 0.059 Uiso 1 1 calc R . . H60B H -0.1393 0.0424 0.1254 0.059 Uiso 1 1 calc R . . H60C H -0.1396 -0.0534 0.1636 0.059 Uiso 1 1 calc R . . C61 C -0.3730(10) -0.1320(7) 0.1789(5) 0.071(4) Uani 1 1 d . . . H61C H -0.4486 -0.1777 0.1954 0.085 Uiso 1 1 calc R . . H61B H -0.3131 -0.1672 0.1806 0.085 Uiso 1 1 calc R . . H61A H -0.3948 -0.1216 0.1412 0.085 Uiso 1 1 calc R . . C62 C -0.2809(10) 0.5533(7) 0.5127(4) 0.164(7) Uani 1 1 d DU . . H62A H -0.1986 0.5483 0.5202 0.196 Uiso 1 1 calc R . . H62B H -0.3359 0.4895 0.4900 0.196 Uiso 1 1 calc R . . C63 C -0.3385(10) 0.5582(6) 0.5649(3) 0.130(6) Uani 1 1 d DU . . H63A H -0.2763 0.5698 0.5961 0.156 Uiso 1 1 calc R . . H63B H -0.4105 0.4897 0.5693 0.156 Uiso 1 1 calc R . . C64 C -0.3817(8) 0.6543(7) 0.5613(3) 0.110(5) Uani 1 1 d DU . . H64A H -0.4739 0.6276 0.5563 0.131 Uiso 1 1 calc R . . H64B H -0.3525 0.7011 0.5945 0.131 Uiso 1 1 calc R . . C65 C -0.3235(10) 0.7161(7) 0.5128(3) 0.114(5) Uani 1 1 d DU . . H65A H -0.3881 0.7269 0.4881 0.137 Uiso 1 1 calc R . . H65B H -0.2593 0.7879 0.5245 0.137 Uiso 1 1 calc R . . C66 C 0.1132(9) 0.8401(7) 0.5394(4) 0.158(7) Uani 1 1 d DU . . H66A H 0.0459 0.8495 0.5582 0.189 Uiso 1 1 calc R . . H66B H 0.1597 0.9083 0.5218 0.189 Uiso 1 1 calc R . . C67 C 0.2010(10) 0.8112(7) 0.5794(4) 0.182(8) Uani 1 1 d DU . . H67A H 0.1695 0.8018 0.6156 0.219 Uiso 1 1 calc R . . H67B H 0.2856 0.8692 0.5819 0.219 Uiso 1 1 calc R . . C68 C 0.2045(8) 0.7046(7) 0.5577(5) 0.166(8) Uani 1 1 d DU . . H68A H 0.2852 0.7180 0.5426 0.199 Uiso 1 1 calc R . . H68B H 0.1934 0.6525 0.5868 0.199 Uiso 1 1 calc R . . C69 C 0.0966(10) 0.6602(7) 0.5135(5) 0.147(7) Uani 1 1 d DU . . H69A H 0.1237 0.6341 0.4814 0.177 Uiso 1 1 calc R . . H69B H 0.0252 0.5998 0.5267 0.177 Uiso 1 1 calc R . . C70 C -0.2034(10) 0.9124(12) 0.4012(4) 0.253(9) Uani 1 1 d DU . . H70A H -0.1737 0.9912 0.4092 0.303 Uiso 1 1 calc R . . H70B H -0.2858 0.8759 0.4156 0.303 Uiso 1 1 calc R . . C71 C -0.2113(7) 0.8881(13) 0.3396(3) 0.199(7) Uani 1 1 d DU . . H71A H -0.2265 0.9450 0.3186 0.239 Uiso 1 1 calc R . . H71B H -0.2783 0.8170 0.3290 0.239 Uiso 1 1 calc R . . C72 C -0.0787(9) 0.8878(14) 0.3313(3) 0.199(8) Uani 1 1 d DU . . H72A H -0.0855 0.8169 0.3164 0.239 Uiso 1 1 calc R . . H72B H -0.0332 0.9452 0.3069 0.239 Uiso 1 1 calc R . . C73 C -0.0132(9) 0.9104(17) 0.3895(4) 0.194(8) Uani 1 1 d DU . . H73A H 0.0450 0.8728 0.3948 0.233 Uiso 1 1 calc R . . H73B H 0.0341 0.9890 0.3967 0.233 Uiso 1 1 calc R . . Cl1 Cl -0.0839(3) 0.6160(2) 0.38121(11) 0.0649(9) Uani 1 1 d D . . Cl2 Cl 0.0345(3) 0.4180(2) 0.34254(10) 0.0628(9) Uani 1 1 d . . . Cl3 Cl 0.0991(3) 0.1739(2) 0.34864(10) 0.0684(10) Uani 1 1 d . . . Fe1 Fe 0.02778(14) 0.58471(11) 0.31719(5) 0.0428(5) Uani 1 1 d . . . Fe2 Fe 0.07620(14) 0.29185(11) 0.28806(5) 0.0467(5) Uani 1 1 d . . . Li1 Li -0.0992(6) 0.7252(7) 0.4500(4) 0.20(2) Uani 1 1 d D . . N1 N 0.1899(7) 0.7038(5) 0.3066(3) 0.038(2) Uani 1 1 d . . . N2 N -0.0275(7) 0.5730(5) 0.2383(3) 0.037(2) Uani 1 1 d . . . N3 N 0.2196(7) 0.3749(6) 0.2481(3) 0.040(2) Uani 1 1 d . . . N4 N -0.0358(7) 0.2315(5) 0.2193(3) 0.039(2) Uani 1 1 d . . . O1 O 0.1949(5) 0.5612(4) 0.1278(2) 0.0353(19) Uani 1 1 d . . . O2 O -0.2672(7) 0.6522(6) 0.4858(3) 0.152(4) Uani 1 1 d DU . . O3 O 0.0621(7) 0.7531(7) 0.5005(3) 0.166(5) Uani 1 1 d DU . . O4 O -0.1131(9) 0.8690(8) 0.4242(3) 0.242(7) Uani 1 1 d DU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.043(5) 0.037(5) 0.007(4) 0.007(3) 0.003(4) 0.004(4) C2 0.034(6) 0.049(6) 0.038(5) -0.004(5) 0.005(5) -0.014(5) C3 0.034(5) 0.017(4) 0.032(5) 0.000(4) -0.004(4) -0.009(4) C4 0.021(4) 0.052(5) 0.018(4) 0.005(4) 0.004(4) 0.015(4) C5 0.041(5) 0.039(5) 0.027(4) 0.021(4) 0.007(4) 0.004(4) C6 0.032(5) 0.032(4) 0.046(5) -0.023(4) -0.020(4) 0.018(4) C7 0.039(5) 0.032(4) 0.025(4) 0.004(4) 0.004(4) 0.016(4) C8 0.022(4) 0.031(4) 0.040(5) 0.013(4) 0.011(4) 0.003(4) C9 0.042(6) 0.037(5) 0.025(5) 0.005(4) -0.001(4) -0.005(4) C10 0.083(8) 0.053(6) 0.019(5) 0.004(5) -0.010(5) 0.007(6) C11 0.050(6) 0.031(5) 0.026(5) -0.009(4) -0.004(4) 0.001(4) C13 0.028(5) 0.027(4) 0.044(5) 0.016(4) -0.006(4) 0.000(4) C14 0.028(4) 0.013(4) 0.036(5) 0.000(3) 0.000(4) 0.005(3) C15 0.101(8) 0.054(6) 0.033(5) -0.015(5) -0.035(6) 0.030(5) C16 0.076(7) 0.087(7) 0.030(5) -0.008(5) -0.012(5) 0.040(6) C17 0.064(7) 0.067(6) 0.056(6) -0.025(5) 0.011(6) 0.018(5) C18 0.060(6) 0.025(4) 0.034(5) 0.014(4) 0.007(4) 0.017(4) C19 0.057(6) 0.038(5) 0.045(5) -0.002(4) 0.012(5) 0.020(4) C20 0.049(5) 0.048(5) 0.025(4) -0.002(4) 0.007(4) 0.018(4) C21 0.056(6) 0.022(4) 0.077(7) 0.003(5) -0.032(6) 0.010(4) C22 0.081(7) 0.022(4) 0.048(6) 0.012(4) 0.006(5) 0.013(5) C23 0.106(9) 0.047(6) 0.028(5) 0.003(5) 0.012(6) 0.011(6) C24 0.023(4) 0.025(4) 0.022(4) -0.005(3) 0.010(3) 0.010(3) C25 0.031(5) 0.041(5) 0.032(5) 0.007(4) 0.005(4) 0.005(4) C26 0.059(6) 0.049(5) 0.028(5) 0.020(4) 0.008(4) 0.028(4) C27 0.054(6) 0.030(5) 0.033(5) 0.004(4) 0.006(5) -0.002(5) C28 0.048(6) 0.049(6) 0.030(5) -0.023(5) -0.014(5) 0.001(5) C29 0.053(7) 0.095(8) 0.029(5) -0.016(5) -0.013(5) 0.020(6) C30 0.104(8) 0.077(6) 0.029(5) -0.027(5) -0.031(6) 0.048(6) C31 0.070(6) 0.087(6) 0.024(5) -0.002(5) -0.015(5) 0.056(5) C32 0.095(8) 0.038(5) 0.052(6) -0.012(5) 0.007(6) 0.016(5) C33 0.138(11) 0.077(8) 0.027(5) -0.031(6) 0.002(7) 0.008(8) C34 0.029(5) 0.044(5) 0.020(4) -0.015(4) -0.004(4) 0.010(4) C37 0.026(5) 0.036(5) 0.041(5) 0.011(4) 0.017(4) -0.001(4) C38 0.031(5) 0.054(6) 0.060(6) 0.003(5) 0.015(5) 0.009(5) C39 0.043(6) 0.046(6) 0.084(8) 0.000(6) 0.017(6) 0.006(5) C40 0.049(6) 0.061(6) 0.045(6) -0.006(5) -0.004(5) 0.009(5) C41 0.079(7) 0.046(5) 0.066(7) 0.006(5) 0.022(6) 0.031(5) C42 0.028(5) 0.081(7) 0.057(6) 0.030(5) 0.011(5) 0.016(5) C43 0.059(6) 0.022(4) 0.013(4) -0.006(3) 0.007(4) 0.011(4) C44 0.063(6) 0.037(5) 0.017(4) 0.008(4) 0.000(4) 0.018(4) C45 0.049(6) 0.026(4) 0.035(5) 0.015(4) 0.021(4) 0.001(4) C46 0.061(6) 0.038(5) 0.016(4) -0.006(4) 0.020(4) 0.015(4) C47 0.049(5) 0.061(5) 0.014(4) -0.006(4) 0.005(4) 0.032(4) C48 0.085(7) 0.071(6) 0.027(5) 0.005(5) 0.009(5) 0.034(5) C49 0.053(7) 0.066(6) 0.030(5) 0.001(5) 0.002(5) 0.006(6) C50 0.040(5) 0.060(5) 0.044(6) -0.005(5) -0.003(5) 0.026(4) C51 0.068(6) 0.061(5) 0.046(6) 0.009(5) 0.018(5) 0.043(4) C52 0.071(7) 0.061(6) 0.063(7) -0.006(5) -0.001(6) 0.034(5) C53 0.042(5) 0.060(5) 0.021(4) 0.013(4) -0.001(4) 0.034(4) C54 0.038(5) 0.059(6) 0.016(4) 0.008(4) 0.002(4) 0.009(5) C55 0.051(5) 0.062(5) 0.060(6) 0.029(5) 0.018(5) 0.035(4) C56 0.053(5) 0.069(6) 0.032(5) -0.005(5) -0.018(5) 0.041(4) C57 0.051(7) 0.048(6) 0.089(8) 0.021(6) 0.002(7) 0.005(5) C58 0.040(6) 0.088(8) 0.056(6) 0.020(6) 0.016(5) 0.006(6) C59 0.045(6) 0.077(6) 0.030(5) 0.010(5) 0.003(5) 0.025(5) C60 0.045(5) 0.034(4) 0.075(7) 0.013(5) -0.009(5) 0.023(4) C61 0.090(7) 0.039(5) 0.105(9) -0.011(5) 0.026(7) 0.046(4) C62 0.226(12) 0.131(10) 0.148(11) 0.028(10) 0.040(11) 0.080(10) C63 0.198(12) 0.126(9) 0.067(8) 0.023(8) 0.029(9) 0.060(9) C64 0.178(10) 0.118(9) 0.037(6) 0.004(6) 0.003(7) 0.063(8) C65 0.208(9) 0.125(7) 0.064(7) 0.026(6) 0.063(7) 0.115(7) C66 0.132(11) 0.245(12) 0.065(7) -0.094(8) -0.029(8) 0.047(10) C67 0.121(11) 0.290(14) 0.092(10) -0.022(11) -0.025(10) 0.039(12) C68 0.115(11) 0.254(14) 0.100(10) 0.013(11) 0.000(9) 0.041(11) C69 0.136(10) 0.188(11) 0.125(11) 0.013(10) -0.027(10) 0.078(9) C70 0.316(14) 0.363(15) 0.128(12) 0.081(12) 0.040(13) 0.179(13) C71 0.297(13) 0.255(12) 0.097(10) 0.049(10) -0.014(11) 0.170(11) C72 0.317(14) 0.230(13) 0.072(9) -0.004(10) -0.023(11) 0.135(12) C73 0.298(14) 0.261(13) 0.054(8) 0.013(10) 0.040(10) 0.138(12) Cl1 0.0667(16) 0.0784(17) 0.0519(15) -0.0003(14) 0.0115(14) 0.0295(14) Cl2 0.102(2) 0.0418(13) 0.0458(14) 0.0034(11) 0.0128(14) 0.0274(13) Cl3 0.103(2) 0.0667(15) 0.0395(13) 0.0195(12) 0.0160(14) 0.0352(14) Fe1 0.0530(8) 0.0417(7) 0.0257(7) 0.0032(6) 0.0057(6) 0.0090(6) Fe2 0.0579(9) 0.0526(8) 0.0235(7) 0.0065(6) 0.0042(6) 0.0144(7) Li1 0.30(5) 0.16(3) 0.10(2) 0.02(2) -0.03(3) 0.06(3) N1 0.047(4) 0.039(4) 0.024(4) -0.013(3) -0.007(4) 0.013(3) N2 0.038(4) 0.028(4) 0.039(4) 0.004(3) 0.014(4) 0.002(3) N3 0.037(4) 0.040(4) 0.033(4) -0.008(3) -0.004(4) 0.004(4) N4 0.047(4) 0.037(4) 0.033(4) 0.001(3) 0.004(4) 0.015(3) O1 0.050(4) 0.032(3) 0.014(3) -0.004(2) -0.005(3) 0.006(3) O2 0.246(8) 0.169(7) 0.092(6) 0.034(6) 0.060(6) 0.129(6) O3 0.168(9) 0.199(9) 0.108(7) -0.055(7) -0.052(7) 0.059(8) O4 0.282(12) 0.355(13) 0.128(9) 0.055(10) 0.028(10) 0.162(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 C1 C2 1.362(12) . ? C1 O1 1.381(10) . ? C1 C6 1.398(11) . ? C2 C3 1.427(12) . ? C2 C43 1.512(12) . ? C3 C4 1.378(11) . ? C3 H3A 0.9500 . ? C4 C5 1.389(11) . ? C4 C14 1.566(11) . ? C5 C6 1.402(12) . ? C5 H5A 0.9500 . ? C6 C7 1.549(11) . ? C7 C19 1.504(13) . ? C7 C8 1.519(12) . ? C7 C18 1.570(12) . ? C8 C13 1.400(12) . ? C8 C9 1.414(11) . ? C9 C10 1.379(13) . ? C9 H9A 0.9500 . ? C10 C11 1.367(12) . ? C10 C20 1.587(13) . ? C11 C12 1.395(11) . ? C11 H11A 0.9500 . ? C12 C13 1.403(12) . ? C12 C24 1.463(11) . ? C13 O1 1.389(9) . ? C14 C17 1.495(13) . ? C14 C15 1.497(11) . ? C14 C16 1.515(13) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.483(14) . ? C20 C23 1.493(13) . ? C20 C21 1.579(13) . ? 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 C25 1.379(11) . ? C24 C34 1.420(10) . ? C25 N1 1.344(11) . ? C25 H25A 0.9500 . ? C26 C31 1.383(13) . ? C26 C27 1.385(12) . ? C26 N1 1.468(10) . ? C27 C28 1.374(12) . ? C27 C32 1.560(15) . ? C28 C29 1.432(15) . ? C28 C33 1.495(15) . ? C29 C30 1.335(15) . ? C29 H29A 0.9500 . ? C30 C31 1.409(12) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33C 0.9800 . ? C33 H33B 0.9800 . ? C33 H33A 0.9800 . ? C34 N2 1.294(10) . ? C34 H34A 0.9500 . ? C35 C36 1.350(12) . ? C35 C40 1.433(13) . ? C35 N2 1.442(10) . ? C36 C37 1.373(11) . ? C36 C41 1.545(12) . ? C37 C38 1.392(13) . ? C37 C42 1.535(15) . ? C38 C39 1.350(16) . ? C38 H38A 0.9500 . ? C39 C40 1.400(13) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C53 1.383(11) . ? C43 C44 1.400(11) . ? C44 N3 1.349(10) . ? C44 H44A 0.9500 . ? C45 C50 1.388(12) . ? C45 C46 1.397(14) . ? C45 N3 1.405(11) . ? C46 C47 1.385(12) . ? C46 C51 1.540(12) . ? C47 C48 1.402(13) . ? C47 C52 1.511(15) . ? C48 C49 1.383(17) . ? C48 H48A 0.9500 . ? C49 C50 1.366(12) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52C 0.9800 . ? C52 H52B 0.9800 . ? C52 H52A 0.9800 . ? C53 N4 1.341(10) . ? C53 H53A 0.9500 . ? C54 C55 1.361(13) . ? C54 C59 1.395(14) . ? C54 N4 1.423(10) . ? C55 C56 1.431(12) . ? C55 C60 1.453(15) . ? C56 C57 1.366(16) . ? C56 C61 1.475(13) . ? C57 C58 1.397(15) . ? C57 H57A 0.9500 . ? C58 C59 1.401(13) . ? C58 H58A 0.9500 . ? C59 H59A 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61C 0.9800 . ? C61 H61B 0.9800 . ? C61 H61A 0.9800 . ? C62 O2 1.446(11) . ? C62 C63 1.520(12) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.552(12) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.518(10) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 O2 1.451(11) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 O3 1.421(11) . ? C66 C67 1.531(12) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.541(12) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.534(12) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 O3 1.478(12) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 O4 1.469(14) . ? C70 C71 1.556(11) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.574(13) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.560(11) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 O4 1.437(12) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? Cl1 Fe1 2.265(3) . ? Cl1 Li1 2.307(10) . ? Cl2 Fe1 2.353(3) . ? Cl2 Fe2 2.375(3) . ? Cl3 Fe2 2.267(3) . ? Fe1 N1 1.985(7) . ? Fe1 N2 2.009(7) . ? Fe2 N3 1.961(7) . ? Fe2 N4 2.032(7) . ? Li1 O3 2.087(10) . ? Li1 O2 2.093(10) . ? Li1 O4 2.095(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 O1 117.1(7) . . ? C2 C1 C6 121.8(8) . . ? O1 C1 C6 120.9(7) . . ? C1 C2 C3 118.3(8) . . ? C1 C2 C43 121.7(8) . . ? C3 C2 C43 119.5(8) . . ? C4 C3 C2 122.2(8) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? C3 C4 C5 117.1(8) . . ? C3 C4 C14 122.0(7) . . ? C5 C4 C14 120.7(7) . . ? C4 C5 C6 122.7(8) . . ? C4 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? C1 C6 C5 117.9(7) . . ? C1 C6 C7 123.6(7) . . ? C5 C6 C7 118.4(7) . . ? C19 C7 C8 109.4(6) . . ? C19 C7 C6 110.0(8) . . ? C8 C7 C6 109.6(7) . . ? C19 C7 C18 112.3(7) . . ? C8 C7 C18 108.0(7) . . ? C6 C7 C18 107.4(6) . . ? C13 C8 C9 116.5(8) . . ? C13 C8 C7 122.3(7) . . ? C9 C8 C7 121.2(7) . . ? C10 C9 C8 120.5(8) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C11 C10 C9 120.5(9) . . ? C11 C10 C20 121.9(9) . . ? C9 C10 C20 117.5(8) . . ? C10 C11 C12 122.8(9) . . ? C10 C11 H11A 118.6 . . ? C12 C11 H11A 118.6 . . ? C11 C12 C13 115.3(7) . . ? C11 C12 C24 121.4(8) . . ? C13 C12 C24 123.2(7) . . ? O1 C13 C8 123.0(8) . . ? O1 C13 C12 112.8(7) . . ? C8 C13 C12 124.3(8) . . ? C17 C14 C15 108.9(8) . . ? C17 C14 C16 112.6(8) . . ? C15 C14 C16 108.2(7) . . ? C17 C14 C4 107.4(6) . . ? C15 C14 C4 111.7(7) . . ? C16 C14 C4 108.1(8) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C7 C18 H18A 109.5 . . ? C7 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C7 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C7 C19 H19A 109.5 . . ? C7 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C7 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C23 109.4(8) . . ? C22 C20 C21 108.3(7) . . ? C23 C20 C21 107.0(9) . . ? C22 C20 C10 110.3(9) . . ? C23 C20 C10 112.1(7) . . ? C21 C20 C10 109.6(7) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C34 123.1(7) . . ? C25 C24 C12 119.3(6) . . ? C34 C24 C12 116.9(7) . . ? N1 C25 C24 123.9(7) . . ? N1 C25 H25A 118.0 . . ? C24 C25 H25A 118.0 . . ? C31 C26 C27 119.4(8) . . ? C31 C26 N1 117.9(8) . . ? C27 C26 N1 122.7(8) . . ? C28 C27 C26 122.4(9) . . ? C28 C27 C32 117.8(8) . . ? C26 C27 C32 119.8(8) . . ? C27 C28 C29 116.7(9) . . ? C27 C28 C33 124.1(10) . . ? C29 C28 C33 119.2(9) . . ? C30 C29 C28 121.7(9) . . ? C30 C29 H29A 119.1 . . ? C28 C29 H29A 119.1 . . ? C29 C30 C31 120.3(10) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 119.9 . . ? C26 C31 C30 119.4(10) . . ? C26 C31 H31A 120.3 . . ? C30 C31 H31A 120.3 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33C 109.5 . . ? C28 C33 H33B 109.5 . . ? H33C C33 H33B 109.5 . . ? C28 C33 H33A 109.5 . . ? H33C C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? N2 C34 C24 131.2(7) . . ? N2 C34 H34A 114.4 . . ? C24 C34 H34A 114.4 . . ? C36 C35 C40 117.5(7) . . ? C36 C35 N2 125.9(7) . . ? C40 C35 N2 116.6(8) . . ? C35 C36 C37 122.1(8) . . ? C35 C36 C41 116.2(7) . . ? C37 C36 C41 121.5(9) . . ? C36 C37 C38 119.6(9) . . ? C36 C37 C42 120.9(8) . . ? C38 C37 C42 119.3(8) . . ? C39 C38 C37 121.2(9) . . ? C39 C38 H38A 119.4 . . ? C37 C38 H38A 119.4 . . ? C38 C39 C40 118.8(10) . . ? C38 C39 H39A 120.6 . . ? C40 C39 H39A 120.6 . . ? C39 C40 C35 120.6(11) . . ? C39 C40 H40A 119.7 . . ? C35 C40 H40A 119.7 . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C53 C43 C44 123.3(7) . . ? C53 C43 C2 120.4(7) . . ? C44 C43 C2 116.2(7) . . ? N3 C44 C43 127.3(7) . . ? N3 C44 H44A 116.4 . . ? C43 C44 H44A 116.4 . . ? C50 C45 C46 116.1(8) . . ? C50 C45 N3 121.8(9) . . ? C46 C45 N3 122.1(8) . . ? C47 C46 C45 121.8(8) . . ? C47 C46 C51 118.4(9) . . ? C45 C46 C51 119.8(8) . . ? C46 C47 C48 120.0(10) . . ? C46 C47 C52 122.4(8) . . ? C48 C47 C52 117.6(8) . . ? C49 C48 C47 118.6(9) . . ? C49 C48 H48A 120.7 . . ? C47 C48 H48A 120.7 . . ? C50 C49 C48 120.0(10) . . ? C50 C49 H49A 120.0 . . ? C48 C49 H49A 120.0 . . ? C49 C50 C45 123.5(11) . . ? C49 C50 H50A 118.3 . . ? C45 C50 H50A 118.3 . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C47 C52 H52C 109.5 . . ? C47 C52 H52B 109.5 . . ? H52C C52 H52B 109.5 . . ? C47 C52 H52A 109.5 . . ? H52C C52 H52A 109.5 . . ? H52B C52 H52A 109.5 . . ? N4 C53 C43 127.9(7) . . ? N4 C53 H53A 116.1 . . ? C43 C53 H53A 116.1 . . ? C55 C54 C59 121.8(8) . . ? C55 C54 N4 121.6(9) . . ? C59 C54 N4 116.6(8) . . ? C54 C55 C56 118.3(9) . . ? C54 C55 C60 122.3(8) . . ? C56 C55 C60 119.1(9) . . ? C57 C56 C55 118.9(9) . . ? C57 C56 C61 118.3(9) . . ? C55 C56 C61 122.8(9) . . ? C56 C57 C58 123.7(9) . . ? C56 C57 H57A 118.1 . . ? C58 C57 H57A 118.1 . . ? C57 C58 C59 116.2(11) . . ? C57 C58 H58A 121.9 . . ? C59 C58 H58A 121.9 . . ? C54 C59 C58 120.9(9) . . ? C54 C59 H59A 119.5 . . ? C58 C59 H59A 119.5 . . ? C55 C60 H60A 109.5 . . ? C55 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C55 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C56 C61 H61C 109.5 . . ? C56 C61 H61B 109.5 . . ? H61C C61 H61B 109.5 . . ? C56 C61 H61A 109.5 . . ? H61C C61 H61A 109.5 . . ? H61B C61 H61A 109.5 . . ? O2 C62 C63 106.1(8) . . ? O2 C62 H62A 110.5 . . ? C63 C62 H62A 110.5 . . ? O2 C62 H62B 110.5 . . ? C63 C62 H62B 110.5 . . ? H62A C62 H62B 108.7 . . ? C62 C63 C64 106.9(7) . . ? C62 C63 H63A 110.3 . . ? C64 C63 H63A 110.3 . . ? C62 C63 H63B 110.3 . . ? C64 C63 H63B 110.3 . . ? H63A C63 H63B 108.6 . . ? C65 C64 C63 105.4(7) . . ? C65 C64 H64A 110.7 . . ? C63 C64 H64A 110.7 . . ? C65 C64 H64B 110.7 . . ? C63 C64 H64B 110.7 . . ? H64A C64 H64B 108.8 . . ? O2 C65 C64 107.2(7) . . ? O2 C65 H65A 110.3 . . ? C64 C65 H65A 110.3 . . ? O2 C65 H65B 110.3 . . ? C64 C65 H65B 110.3 . . ? H65A C65 H65B 108.5 . . ? O3 C66 C67 106.8(8) . . ? O3 C66 H66A 110.4 . . ? C67 C66 H66A 110.4 . . ? O3 C66 H66B 110.4 . . ? C67 C66 H66B 110.4 . . ? H66A C66 H66B 108.6 . . ? C66 C67 C68 106.5(7) . . ? C66 C67 H67A 110.4 . . ? C68 C67 H67A 110.4 . . ? C66 C67 H67B 110.4 . . ? C68 C67 H67B 110.4 . . ? H67A C67 H67B 108.6 . . ? C69 C68 C67 106.1(7) . . ? C69 C68 H68A 110.5 . . ? C67 C68 H68A 110.5 . . ? C69 C68 H68B 110.5 . . ? C67 C68 H68B 110.5 . . ? H68A C68 H68B 108.7 . . ? O3 C69 C68 104.6(7) . . ? O3 C69 H69A 110.8 . . ? C68 C69 H69A 110.8 . . ? O3 C69 H69B 110.8 . . ? C68 C69 H69B 110.8 . . ? H69A C69 H69B 108.9 . . ? O4 C70 C71 104.0(9) . . ? O4 C70 H70A 110.9 . . ? C71 C70 H70A 110.9 . . ? O4 C70 H70B 111.0 . . ? C71 C70 H70B 111.0 . . ? H70A C70 H70B 109.0 . . ? C70 C71 C72 102.9(6) . . ? C70 C71 H71A 111.2 . . ? C72 C71 H71A 111.2 . . ? C70 C71 H71B 111.2 . . ? C72 C71 H71B 111.2 . . ? H71A C71 H71B 109.1 . . ? C73 C72 C71 102.8(7) . . ? C73 C72 H72A 111.2 . . ? C71 C72 H72A 111.2 . . ? C73 C72 H72B 111.2 . . ? C71 C72 H72B 111.2 . . ? H72A C72 H72B 109.1 . . ? O4 C73 C72 104.9(7) . . ? O4 C73 H73A 110.8 . . ? C72 C73 H73A 110.8 . . ? O4 C73 H73B 110.8 . . ? C72 C73 H73B 110.8 . . ? H73A C73 H73B 108.8 . . ? Fe1 Cl1 Li1 149.6(2) . . ? Fe1 Cl2 Fe2 127.47(12) . . ? N1 Fe1 N2 92.3(3) . . ? N1 Fe1 Cl1 116.1(2) . . ? N2 Fe1 Cl1 122.5(3) . . ? N1 Fe1 Cl2 116.8(3) . . ? N2 Fe1 Cl2 108.1(2) . . ? Cl1 Fe1 Cl2 101.81(12) . . ? N3 Fe2 N4 92.5(3) . . ? N3 Fe2 Cl3 118.2(3) . . ? N4 Fe2 Cl3 118.4(2) . . ? N3 Fe2 Cl2 107.0(2) . . ? N4 Fe2 Cl2 118.1(3) . . ? Cl3 Fe2 Cl2 102.84(11) . . ? O3 Li1 O2 115.3(6) . . ? O3 Li1 O4 112.4(5) . . ? O2 Li1 O4 101.1(5) . . ? O3 Li1 Cl1 103.2(5) . . ? O2 Li1 Cl1 111.2(4) . . ? O4 Li1 Cl1 114.0(5) . . ? C25 N1 C26 111.8(6) . . ? C25 N1 Fe1 126.5(5) . . ? C26 N1 Fe1 121.7(5) . . ? C34 N2 C35 114.7(7) . . ? C34 N2 Fe1 120.7(6) . . ? C35 N2 Fe1 124.6(5) . . ? C44 N3 C45 115.1(7) . . ? C44 N3 Fe2 124.1(6) . . ? C45 N3 Fe2 120.5(5) . . ? C53 N4 C54 122.4(7) . . ? C53 N4 Fe2 123.0(5) . . ? C54 N4 Fe2 114.6(5) . . ? C1 O1 C13 120.2(6) . . ? C62 O2 C65 113.0(7) . . ? C62 O2 Li1 114.7(7) . . ? C65 O2 Li1 121.5(6) . . ? C66 O3 C69 113.4(7) . . ? C66 O3 Li1 123.7(7) . . ? C69 O3 Li1 118.3(6) . . ? C73 O4 C70 102.5(9) . . ? C73 O4 Li1 102.8(11) . . ? C70 O4 Li1 142.0(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 176.6(8) . . . . ? C6 C1 C2 C3 1.8(15) . . . . ? O1 C1 C2 C43 -12.2(14) . . . . ? C6 C1 C2 C43 173.0(9) . . . . ? C1 C2 C3 C4 -1.9(15) . . . . ? C43 C2 C3 C4 -173.3(9) . . . . ? C2 C3 C4 C5 2.6(14) . . . . ? C2 C3 C4 C14 177.8(8) . . . . ? C3 C4 C5 C6 -3.3(14) . . . . ? C14 C4 C5 C6 -178.6(8) . . . . ? C2 C1 C6 C5 -2.5(14) . . . . ? O1 C1 C6 C5 -177.0(8) . . . . ? C2 C1 C6 C7 -178.2(9) . . . . ? O1 C1 C6 C7 7.2(14) . . . . ? C4 C5 C6 C1 3.3(14) . . . . ? C4 C5 C6 C7 179.2(8) . . . . ? C1 C6 C7 C19 113.6(10) . . . . ? C5 C6 C7 C19 -62.2(10) . . . . ? C1 C6 C7 C8 -6.7(12) . . . . ? C5 C6 C7 C8 177.6(8) . . . . ? C1 C6 C7 C18 -123.8(9) . . . . ? C5 C6 C7 C18 60.4(11) . . . . ? C19 C7 C8 C13 -119.7(9) . . . . ? C6 C7 C8 C13 1.0(12) . . . . ? C18 C7 C8 C13 117.7(9) . . . . ? C19 C7 C8 C9 61.1(11) . . . . ? C6 C7 C8 C9 -178.2(8) . . . . ? C18 C7 C8 C9 -61.5(10) . . . . ? C13 C8 C9 C10 -2.1(14) . . . . ? C7 C8 C9 C10 177.1(9) . . . . ? C8 C9 C10 C11 0.0(17) . . . . ? C8 C9 C10 C20 -179.0(9) . . . . ? C9 C10 C11 C12 0.0(17) . . . . ? C20 C10 C11 C12 178.9(9) . . . . ? C10 C11 C12 C13 2.1(15) . . . . ? C10 C11 C12 C24 -174.2(10) . . . . ? C9 C8 C13 O1 -176.2(8) . . . . ? C7 C8 C13 O1 4.6(14) . . . . ? C9 C8 C13 C12 4.5(14) . . . . ? C7 C8 C13 C12 -174.8(8) . . . . ? C11 C12 C13 O1 176.2(8) . . . . ? C24 C12 C13 O1 -7.6(12) . . . . ? C11 C12 C13 C8 -4.4(14) . . . . ? C24 C12 C13 C8 171.8(8) . . . . ? C3 C4 C14 C17 -110.8(9) . . . . ? C5 C4 C14 C17 64.2(11) . . . . ? C3 C4 C14 C15 8.5(12) . . . . ? C5 C4 C14 C15 -176.5(9) . . . . ? C3 C4 C14 C16 127.4(9) . . . . ? C5 C4 C14 C16 -57.6(10) . . . . ? C11 C10 C20 C22 119.9(11) . . . . ? C9 C10 C20 C22 -61.1(12) . . . . ? C11 C10 C20 C23 -2.3(15) . . . . ? C9 C10 C20 C23 176.7(10) . . . . ? C11 C10 C20 C21 -120.9(11) . . . . ? C9 C10 C20 C21 58.1(13) . . . . ? C11 C12 C24 C25 -48.1(13) . . . . ? C13 C12 C24 C25 135.9(9) . . . . ? C11 C12 C24 C34 122.4(9) . . . . ? C13 C12 C24 C34 -53.6(13) . . . . ? C34 C24 C25 N1 6.1(15) . . . . ? C12 C24 C25 N1 176.1(9) . . . . ? C31 C26 C27 C28 1.2(15) . . . . ? N1 C26 C27 C28 -176.6(9) . . . . ? C31 C26 C27 C32 -179.3(9) . . . . ? N1 C26 C27 C32 2.9(14) . . . . ? C26 C27 C28 C29 0.7(15) . . . . ? C32 C27 C28 C29 -178.8(9) . . . . ? C26 C27 C28 C33 -179.7(10) . . . . ? C32 C27 C28 C33 0.8(16) . . . . ? C27 C28 C29 C30 -3.6(16) . . . . ? C33 C28 C29 C30 176.8(11) . . . . ? C28 C29 C30 C31 4.6(17) . . . . ? C27 C26 C31 C30 -0.4(15) . . . . ? N1 C26 C31 C30 177.5(9) . . . . ? C29 C30 C31 C26 -2.5(16) . . . . ? C25 C24 C34 N2 -3.4(16) . . . . ? C12 C24 C34 N2 -173.5(10) . . . . ? C40 C35 C36 C37 -4.9(12) . . . . ? N2 C35 C36 C37 173.7(8) . . . . ? C40 C35 C36 C41 179.5(8) . . . . ? N2 C35 C36 C41 -2.0(12) . . . . ? C35 C36 C37 C38 2.5(13) . . . . ? C41 C36 C37 C38 177.9(8) . . . . ? C35 C36 C37 C42 -173.9(8) . . . . ? C41 C36 C37 C42 1.5(13) . . . . ? C36 C37 C38 C39 -0.3(14) . . . . ? C42 C37 C38 C39 176.2(9) . . . . ? C37 C38 C39 C40 0.7(15) . . . . ? C38 C39 C40 C35 -3.2(15) . . . . ? C36 C35 C40 C39 5.2(13) . . . . ? N2 C35 C40 C39 -173.4(8) . . . . ? C1 C2 C43 C53 134.0(10) . . . . ? C3 C2 C43 C53 -54.9(14) . . . . ? C1 C2 C43 C44 -46.0(15) . . . . ? C3 C2 C43 C44 125.1(10) . . . . ? C53 C43 C44 N3 3.7(17) . . . . ? C2 C43 C44 N3 -176.2(10) . . . . ? C50 C45 C46 C47 0.3(12) . . . . ? N3 C45 C46 C47 -178.5(7) . . . . ? C50 C45 C46 C51 -177.7(8) . . . . ? N3 C45 C46 C51 3.4(12) . . . . ? C45 C46 C47 C48 -0.1(12) . . . . ? C51 C46 C47 C48 177.9(8) . . . . ? C45 C46 C47 C52 179.2(8) . . . . ? C51 C46 C47 C52 -2.7(12) . . . . ? C46 C47 C48 C49 -0.4(13) . . . . ? C52 C47 C48 C49 -179.8(9) . . . . ? C47 C48 C49 C50 0.8(14) . . . . ? C48 C49 C50 C45 -0.7(15) . . . . ? C46 C45 C50 C49 0.1(13) . . . . ? N3 C45 C50 C49 178.9(8) . . . . ? C44 C43 C53 N4 2.2(17) . . . . ? C2 C43 C53 N4 -177.9(10) . . . . ? C59 C54 C55 C56 0.7(15) . . . . ? N4 C54 C55 C56 -179.4(9) . . . . ? C59 C54 C55 C60 -173.3(10) . . . . ? N4 C54 C55 C60 6.6(15) . . . . ? C54 C55 C56 C57 2.1(15) . . . . ? C60 C55 C56 C57 176.3(10) . . . . ? C54 C55 C56 C61 179.3(10) . . . . ? C60 C55 C56 C61 -6.5(15) . . . . ? C55 C56 C57 C58 -1.4(17) . . . . ? C61 C56 C57 C58 -178.8(11) . . . . ? C56 C57 C58 C59 -2.0(17) . . . . ? C55 C54 C59 C58 -4.3(16) . . . . ? N4 C54 C59 C58 175.8(9) . . . . ? C57 C58 C59 C54 4.8(16) . . . . ? O2 C62 C63 C64 11.1(10) . . . . ? C62 C63 C64 C65 -11.7(10) . . . . ? C63 C64 C65 O2 7.9(9) . . . . ? O3 C66 C67 C68 4.5(11) . . . . ? C66 C67 C68 C69 -13.0(11) . . . . ? C67 C68 C69 O3 16.2(11) . . . . ? O4 C70 C71 C72 -28.1(13) . . . . ? C70 C71 C72 C73 0.8(16) . . . . ? C71 C72 C73 O4 27.5(18) . . . . ? Li1 Cl1 Fe1 N1 -6.0(6) . . . . ? Li1 Cl1 Fe1 N2 -117.3(6) . . . . ? Li1 Cl1 Fe1 Cl2 122.0(5) . . . . ? Fe2 Cl2 Fe1 N1 -72.4(3) . . . . ? Fe2 Cl2 Fe1 N2 29.8(3) . . . . ? Fe2 Cl2 Fe1 Cl1 160.11(15) . . . . ? Fe1 Cl2 Fe2 N3 44.7(3) . . . . ? Fe1 Cl2 Fe2 N4 -57.7(3) . . . . ? Fe1 Cl2 Fe2 Cl3 169.85(16) . . . . ? Fe1 Cl1 Li1 O3 -52.1(7) . . . . ? Fe1 Cl1 Li1 O2 -176.2(4) . . . . ? Fe1 Cl1 Li1 O4 70.2(7) . . . . ? C24 C25 N1 C26 -174.9(9) . . . . ? C24 C25 N1 Fe1 5.6(14) . . . . ? C31 C26 N1 C25 -116.6(10) . . . . ? C27 C26 N1 C25 61.2(13) . . . . ? C31 C26 N1 Fe1 63.0(11) . . . . ? C27 C26 N1 Fe1 -119.2(9) . . . . ? N2 Fe1 N1 C25 -13.8(9) . . . . ? Cl1 Fe1 N1 C25 -142.0(8) . . . . ? Cl2 Fe1 N1 C25 97.8(8) . . . . ? N2 Fe1 N1 C26 166.7(7) . . . . ? Cl1 Fe1 N1 C26 38.5(8) . . . . ? Cl2 Fe1 N1 C26 -81.7(7) . . . . ? C24 C34 N2 C35 168.8(9) . . . . ? C24 C34 N2 Fe1 -10.1(14) . . . . ? C36 C35 N2 C34 -88.5(11) . . . . ? C40 C35 N2 C34 90.0(10) . . . . ? C36 C35 N2 Fe1 90.3(9) . . . . ? C40 C35 N2 Fe1 -91.2(9) . . . . ? N1 Fe1 N2 C34 15.1(8) . . . . ? Cl1 Fe1 N2 C34 138.3(7) . . . . ? Cl2 Fe1 N2 C34 -104.0(7) . . . . ? N1 Fe1 N2 C35 -163.6(7) . . . . ? Cl1 Fe1 N2 C35 -40.5(8) . . . . ? Cl2 Fe1 N2 C35 77.2(7) . . . . ? C43 C44 N3 C45 172.3(10) . . . . ? C43 C44 N3 Fe2 -14.9(15) . . . . ? C50 C45 N3 C44 80.4(11) . . . . ? C46 C45 N3 C44 -100.8(10) . . . . ? C50 C45 N3 Fe2 -92.7(9) . . . . ? C46 C45 N3 Fe2 86.1(10) . . . . ? N4 Fe2 N3 C44 15.4(8) . . . . ? Cl3 Fe2 N3 C44 139.7(7) . . . . ? Cl2 Fe2 N3 C44 -105.0(7) . . . . ? N4 Fe2 N3 C45 -172.2(7) . . . . ? Cl3 Fe2 N3 C45 -47.9(8) . . . . ? Cl2 Fe2 N3 C45 67.5(7) . . . . ? C43 C53 N4 C54 -177.6(10) . . . . ? C43 C53 N4 Fe2 3.9(14) . . . . ? C55 C54 N4 C53 51.7(14) . . . . ? C59 C54 N4 C53 -128.3(10) . . . . ? C55 C54 N4 Fe2 -129.7(8) . . . . ? C59 C54 N4 Fe2 50.3(11) . . . . ? N3 Fe2 N4 C53 -10.4(8) . . . . ? Cl3 Fe2 N4 C53 -134.5(7) . . . . ? Cl2 Fe2 N4 C53 100.4(8) . . . . ? N3 Fe2 N4 C54 171.0(7) . . . . ? Cl3 Fe2 N4 C54 46.9(8) . . . . ? Cl2 Fe2 N4 C54 -78.2(7) . . . . ? C2 C1 O1 C13 -176.0(9) . . . . ? C6 C1 O1 C13 -1.2(13) . . . . ? C8 C13 O1 C1 -4.7(13) . . . . ? C12 C13 O1 C1 174.7(8) . . . . ? C63 C62 O2 C65 -6.5(11) . . . . ? C63 C62 O2 Li1 138.5(7) . . . . ? C64 C65 O2 C62 -1.0(10) . . . . ? C64 C65 O2 Li1 -143.4(7) . . . . ? O3 Li1 O2 C62 -52.9(9) . . . . ? O4 Li1 O2 C62 -174.4(6) . . . . ? Cl1 Li1 O2 C62 64.1(7) . . . . ? O3 Li1 O2 C65 88.8(8) . . . . ? O4 Li1 O2 C65 -32.7(9) . . . . ? Cl1 Li1 O2 C65 -154.1(6) . . . . ? C67 C66 O3 C69 6.3(12) . . . . ? C67 C66 O3 Li1 161.6(7) . . . . ? C68 C69 O3 C66 -14.4(12) . . . . ? C68 C69 O3 Li1 -171.1(7) . . . . ? O2 Li1 O3 C66 -78.0(9) . . . . ? O4 Li1 O3 C66 37.2(10) . . . . ? Cl1 Li1 O3 C66 160.6(7) . . . . ? O2 Li1 O3 C69 76.2(10) . . . . ? O4 Li1 O3 C69 -168.6(8) . . . . ? Cl1 Li1 O3 C69 -45.2(9) . . . . ? C72 C73 O4 C70 -46.4(16) . . . . ? C72 C73 O4 Li1 104.9(13) . . . . ? C71 C70 O4 C73 46.8(12) . . . . ? C71 C70 O4 Li1 -83.8(13) . . . . ? O3 Li1 O4 C73 68.3(8) . . . . ? O2 Li1 O4 C73 -168.2(6) . . . . ? Cl1 Li1 O4 C73 -48.7(7) . . . . ? O3 Li1 O4 C70 -161.1(10) . . . . ? O2 Li1 O4 C70 -37.7(13) . . . . ? Cl1 Li1 O4 C70 81.8(12) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.085 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.094 # Attachment '2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 663094' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(C6H3F2)Xanthdim]Fe2Cl3(Li(thf)3) ; _chemical_name_common ((C6H3F2)Xanthdim)Fe2Cl3(Li(thf)3) _chemical_melting_point ? _chemical_formula_moiety 'C130 H136 Cl6 F16 Fe4 Li2 N8 O8, C6 H14' _chemical_formula_sum 'C136 H150 Cl6 F16 Fe4 Li2 N8 O8' _chemical_formula_weight 2778.62 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.284(5) _cell_length_b 15.375(8) _cell_length_c 16.471(8) _cell_angle_alpha 85.24(4) _cell_angle_beta 76.33(4) _cell_angle_gamma 89.89(4) _cell_volume 3502(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 14 _cell_measurement_theta_max 17 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.76 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method none _exptl_crystal_F_000 1442 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6464 _exptl_absorpt_correction_T_max 0.7624 _exptl_absorpt_process_details ; North,A.C.T., Phillips,D.C., Mathwes,F.S. (1968). Acta Cryst. A24, 351-359. ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of a cryostream cooler (Oxford Cryosystems). ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_measurement_device 'Stoe STADI4 diffractometer' _diffrn_measurement_method 2\Q/\w-scan,ratio=0.0,width(\w)=3.1-3.2\% _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 8.8 _diffrn_reflns_number 11732 _diffrn_reflns_av_R_equivalents 0.0889 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 23.00 _reflns_number_total 9729 _reflns_number_gt 6056 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'STADI4-1.06 (Stoe & Cie, 1997)' _computing_cell_refinement 'STADI4-1.06 (Stoe & Cie, 1997)' _computing_data_reduction 'XRED1.08 (Stoe & Cie, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+25.0548P] 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 9729 _refine_ls_number_parameters 816 _refine_ls_number_restraints 134 _refine_ls_R_factor_all 0.1499 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2635 _refine_ls_wR_factor_gt 0.2088 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1609(5) 0.5718(5) 0.2810(5) 0.0305(18) Uani 1 1 d . . . C2 C 0.2561(6) 0.5633(5) 0.2337(5) 0.0330(19) Uani 1 1 d . . . C3 C 0.3227(6) 0.6293(6) 0.2331(6) 0.043(2) Uani 1 1 d . . . H3 H 0.3870 0.6243 0.2013 0.052 Uiso 1 1 calc R . . C4 C 0.2984(7) 0.7019(6) 0.2772(6) 0.048(2) Uani 1 1 d . . . C5 C 0.2043(7) 0.7068(5) 0.3235(6) 0.044(2) Uani 1 1 d . . . H5 H 0.1868 0.7559 0.3548 0.052 Uiso 1 1 calc R . . C6 C 0.1341(6) 0.6433(5) 0.3263(5) 0.036(2) Uani 1 1 d . . . C7 C 0.0305(6) 0.6541(5) 0.3770(5) 0.037(2) Uani 1 1 d . . . C8 C -0.0294(6) 0.5732(5) 0.3746(5) 0.0323(19) Uani 1 1 d . . . C9 C -0.1249(6) 0.5664(5) 0.4205(5) 0.036(2) Uani 1 1 d . . . H9 H -0.1498 0.6117 0.4549 0.043 Uiso 1 1 calc R . . C10 C -0.1851(6) 0.4965(6) 0.4182(5) 0.037(2) Uani 1 1 d . . . C11 C -0.1458(5) 0.4310(5) 0.3670(5) 0.0334(19) Uani 1 1 d . . . H11 H -0.1854 0.3822 0.3646 0.040 Uiso 1 1 calc R . . C12 C -0.0516(5) 0.4345(5) 0.3198(5) 0.0296(18) Uani 1 1 d . . . C13 C 0.0050(5) 0.5054(5) 0.3251(5) 0.0300(18) Uani 1 1 d . . . C14 C 0.3748(8) 0.7718(7) 0.2783(8) 0.065(3) Uani 1 1 d . . . C15 C 0.433(2) 0.7944(17) 0.1946(12) 0.28(2) Uani 1 1 d . . . H15C H 0.4813 0.8385 0.1965 0.341 Uiso 1 1 calc R . . H15B H 0.3913 0.8178 0.1586 0.341 Uiso 1 1 calc R . . H15A H 0.4647 0.7422 0.1720 0.341 Uiso 1 1 calc R . . C16 C 0.4521(12) 0.7273(11) 0.3205(15) 0.165(10) Uani 1 1 d . . . H16A H 0.4800 0.6782 0.2891 0.199 Uiso 1 1 calc R . . H16B H 0.4216 0.7058 0.3784 0.199 Uiso 1 1 calc R . . H16C H 0.5031 0.7698 0.3203 0.199 Uiso 1 1 calc R . . C17 C 0.3406(10) 0.8411(10) 0.3317(15) 0.186(12) Uani 1 1 d . . . H17A H 0.3166 0.8162 0.3896 0.223 Uiso 1 1 calc R . . H17B H 0.2884 0.8716 0.3126 0.223 Uiso 1 1 calc R . . H17C H 0.3936 0.8824 0.3290 0.223 Uiso 1 1 calc R . . C18 C -0.0143(7) 0.7325(6) 0.3357(6) 0.047(2) Uani 1 1 d . . . H18A H -0.0153 0.7213 0.2782 0.057 Uiso 1 1 calc R . . H18B H 0.0242 0.7854 0.3348 0.057 Uiso 1 1 calc R . . H18C H -0.0804 0.7405 0.3680 0.057 Uiso 1 1 calc R . . C19 C 0.0322(7) 0.6689(6) 0.4673(5) 0.046(2) Uani 1 1 d . . . H19A H 0.0709 0.7215 0.4676 0.055 Uiso 1 1 calc R . . H19B H 0.0607 0.6184 0.4922 0.055 Uiso 1 1 calc R . . H19C H -0.0337 0.6764 0.5000 0.055 Uiso 1 1 calc R . . C20 C -0.2909(6) 0.4952(7) 0.4653(6) 0.046(2) Uani 1 1 d . . . C21 C -0.3420(8) 0.5635(12) 0.4217(9) 0.120(6) Uani 1 1 d . . . H21A H -0.3354 0.5505 0.3633 0.144 Uiso 1 1 calc R . . H21B H -0.3135 0.6211 0.4229 0.144 Uiso 1 1 calc R . . H21C H -0.4105 0.5631 0.4504 0.144 Uiso 1 1 calc R . . C22 C -0.2995(8) 0.5104(12) 0.5539(8) 0.117(6) Uani 1 1 d . . . H22A H -0.2702 0.5671 0.5572 0.140 Uiso 1 1 calc R . . H22B H -0.2664 0.4642 0.5802 0.140 Uiso 1 1 calc R . . H22C H -0.3678 0.5099 0.5832 0.140 Uiso 1 1 calc R . . C23 C -0.3406(9) 0.4084(9) 0.4630(11) 0.126(7) Uani 1 1 d . . . H23A H -0.3076 0.3613 0.4882 0.151 Uiso 1 1 calc R . . H23B H -0.3384 0.3979 0.4047 0.151 Uiso 1 1 calc R . . H23C H -0.4079 0.4099 0.4945 0.151 Uiso 1 1 calc R . . C24 C -0.0134(5) 0.3660(5) 0.2622(5) 0.0300(18) Uani 1 1 d . . . C25 C -0.0109(6) 0.2807(5) 0.2966(5) 0.036(2) Uani 1 1 d . B . H25 H -0.0316 0.2710 0.3559 0.043 Uiso 1 1 calc R . . C26 C 0.0117(7) 0.1296(5) 0.3035(6) 0.047(2) Uani 1 1 d . B . C27 C -0.0714(9) 0.1026(7) 0.3644(7) 0.062(3) Uani 1 1 d . . . C28 C -0.0792(12) 0.0232(7) 0.4122(8) 0.090(4) Uani 1 1 d . . . H28 H -0.1361 0.0062 0.4536 0.108 Uiso 1 1 calc R . . C29 C -0.0006(14) -0.0297(8) 0.3966(8) 0.093(5) Uani 1 1 d . . . C30 C 0.0798(11) -0.0079(7) 0.3353(9) 0.080(4) Uani 1 1 d . . . H30 H 0.1315 -0.0475 0.3248 0.096 Uiso 1 1 calc R . . C31 C 0.0866(9) 0.0722(6) 0.2877(8) 0.068(3) Uani 1 1 d . . . H31 H 0.1426 0.0871 0.2445 0.082 Uiso 1 1 calc R . . C32 C 0.0163(5) 0.3945(5) 0.1781(5) 0.0334(19) Uani 1 1 d . A . H32 H 0.0105 0.4553 0.1649 0.040 Uiso 1 1 calc R . . C33 C 0.0854(6) 0.3957(6) 0.0347(5) 0.039(2) Uani 1 1 d . A . C34 C 0.0867(8) 0.3604(8) -0.0390(7) 0.067(3) Uani 1 1 d DU . . H38S H 0.0640 0.3050 -0.0368 0.080 Uiso 0.252(16) 1 d PR A 2 C35 C 0.1223(10) 0.4014(12) -0.1191(7) 0.086(5) Uani 1 1 d . A . H35 H 0.1221 0.3738 -0.1686 0.103 Uiso 1 1 calc R . . C36 C 0.1568(9) 0.4822(13) -0.1211(9) 0.091(5) Uani 1 1 d . . . C37 C 0.1577(7) 0.5241(9) -0.0542(8) 0.070(3) Uani 1 1 d . A . H37 H 0.1821 0.5822 -0.0593 0.084 Uiso 1 1 calc R . . C38 C 0.1216(6) 0.4796(8) 0.0230(7) 0.056(3) Uani 1 1 d DU . . H38 H 0.1225 0.5102 0.0706 0.067 Uiso 0.748(16) 1 d PR A 1 C39 C 0.2835(5) 0.4836(5) 0.1882(5) 0.0288(18) Uani 1 1 d . . . C40 C 0.2787(5) 0.4048(5) 0.2368(5) 0.0310(18) Uani 1 1 d . B . H40 H 0.2587 0.4071 0.2958 0.037 Uiso 1 1 calc R . . C41 C 0.2903(6) 0.2540(5) 0.2706(5) 0.036(2) Uani 1 1 d . B . C42 C 0.2248(7) 0.2444(6) 0.3448(6) 0.044(2) Uani 1 1 d . . . C43 C 0.2163(9) 0.1709(7) 0.4017(7) 0.064(3) Uani 1 1 d . . . H43 H 0.1687 0.1655 0.4531 0.077 Uiso 1 1 calc R . . C44 C 0.2828(10) 0.1059(7) 0.3777(8) 0.071(3) Uani 1 1 d . . . C45 C 0.3479(9) 0.1115(7) 0.3038(8) 0.066(3) Uani 1 1 d . . . H45 H 0.3893 0.0639 0.2893 0.080 Uiso 1 1 calc R . . C46 C 0.3557(9) 0.1843(6) 0.2490(8) 0.065(3) Uani 1 1 d . . . H46 H 0.4035 0.1886 0.1977 0.079 Uiso 1 1 calc R . . C47 C 0.3139(5) 0.4944(5) 0.1014(5) 0.0336(19) Uani 1 1 d . B . H47 H 0.3169 0.5528 0.0769 0.040 Uiso 1 1 calc R . . C48 C 0.3775(5) 0.4615(6) -0.0377(5) 0.034(2) Uani 1 1 d . B . C49 C 0.3664(6) 0.4093(6) -0.0987(6) 0.045(2) Uani 1 1 d . . . C50 C 0.4001(7) 0.4316(7) -0.1825(6) 0.054(3) Uani 1 1 d . . . H50 H 0.3909 0.3941 -0.2231 0.064 Uiso 1 1 calc R . . C51 C 0.4480(7) 0.5106(8) -0.2056(6) 0.058(3) Uani 1 1 d . . . C52 C 0.4636(6) 0.5649(7) -0.1497(6) 0.055(3) Uani 1 1 d . . . H52 H 0.4975 0.6188 -0.1676 0.066 Uiso 1 1 calc R . . C53 C 0.4285(6) 0.5392(6) -0.0650(6) 0.047(2) Uani 1 1 d . . . H53 H 0.4398 0.5761 -0.0246 0.056 Uiso 1 1 calc R . . C54 C -0.2289(12) 0.2048(9) -0.0280(8) 0.108(5) Uani 1 1 d DU B . H54A H -0.2179 0.2416 0.0155 0.130 Uiso 1 1 calc R . . H54B H -0.2941 0.2163 -0.0369 0.130 Uiso 1 1 calc R . . C55 C -0.1565(12) 0.2245(10) -0.1057(9) 0.107(5) Uani 1 1 d U . . H55A H -0.1866 0.2522 -0.1494 0.129 Uiso 1 1 calc R . . H55B H -0.1068 0.2651 -0.0969 0.129 Uiso 1 1 calc R . . C56 C -0.1147(16) 0.1446(12) -0.1304(11) 0.158(8) Uani 1 1 d U . . H56A H -0.0446 0.1468 -0.1338 0.189 Uiso 1 1 calc R . . H56B H -0.1243 0.1340 -0.1863 0.189 Uiso 1 1 calc R . . C57 C -0.1594(9) 0.0756(8) -0.0699(7) 0.078(3) Uani 1 1 d DU B . H57A H -0.1975 0.0365 -0.0952 0.093 Uiso 1 1 calc R . . H57B H -0.1100 0.0407 -0.0495 0.093 Uiso 1 1 calc R . . C58 C -0.212(2) -0.0485(12) 0.2325(11) 0.253(11) Uani 1 1 d DU . . H58A H -0.2672 -0.0392 0.2798 0.303 Uiso 1 1 calc R . . H58B H -0.1558 -0.0142 0.2387 0.303 Uiso 1 1 calc R . . C59 C -0.189(2) -0.1407(14) 0.2308(16) 0.241(11) Uani 1 1 d DU . . H59A H -0.2018 -0.1712 0.2878 0.289 Uiso 1 1 calc R . . H59B H -0.1220 -0.1503 0.2004 0.289 Uiso 1 1 calc R . . C60 C -0.261(2) -0.1661(12) 0.1830(15) 0.240(11) Uani 1 1 d DU B . H60A H -0.3283 -0.1662 0.2169 0.288 Uiso 1 1 calc R . . H60B H -0.2468 -0.2230 0.1591 0.288 Uiso 1 1 calc R . . C61 C -0.238(2) -0.0901(11) 0.1175(10) 0.199(9) Uani 1 1 d DU . . H61A H -0.1760 -0.0983 0.0775 0.239 Uiso 1 1 calc R B . H61B H -0.2894 -0.0838 0.0860 0.239 Uiso 1 1 calc R . . C62 C -0.3580(15) 0.1656(15) 0.2008(14) 0.106(7) Uiso 0.655(7) 1 d PDU B 3 H62A H -0.3813 0.1052 0.2208 0.128 Uiso 0.655(7) 1 calc PR B 3 H62B H -0.3833 0.1841 0.1512 0.128 Uiso 0.655(7) 1 calc PR B 3 C63 C -0.3910(18) 0.221(2) 0.2636(18) 0.144(10) Uiso 0.655(7) 1 d PDU B 3 H63A H -0.4491 0.2519 0.2551 0.173 Uiso 0.655(7) 1 calc PR B 3 H63B H -0.4062 0.1881 0.3196 0.173 Uiso 0.655(7) 1 calc PR B 3 C64 C -0.3202(18) 0.2742(17) 0.2561(18) 0.142(10) Uiso 0.655(7) 1 d PDU B 3 H64A H -0.3153 0.2884 0.3125 0.171 Uiso 0.655(7) 1 calc PR B 3 H64B H -0.3324 0.3290 0.2245 0.171 Uiso 0.655(7) 1 calc PR B 3 C65 C -0.2282(15) 0.2376(13) 0.2122(13) 0.100(7) Uiso 0.655(7) 1 d PDU B 3 H65A H -0.1910 0.2790 0.1669 0.120 Uiso 0.655(7) 1 calc PR B 3 H65B H -0.1878 0.2177 0.2511 0.120 Uiso 0.655(7) 1 calc PR B 3 C66 C -0.427(2) -0.024(2) -0.0015(19) 0.073(10) Uiso 0.345(7) 1 d PDU B -4 H66A H -0.4290 -0.0884 0.0122 0.087 Uiso 0.345(7) 1 calc PR B -4 H66B H -0.3659 -0.0104 -0.0440 0.087 Uiso 0.345(7) 1 calc PR B -4 C67 C -0.506(2) -0.003(3) -0.0405(17) 0.080(10) Uiso 0.345(7) 1 d PDU B -4 H67A H -0.5233 -0.0499 -0.0717 0.096 Uiso 0.345(7) 1 calc PR B -4 H67B H -0.4953 0.0534 -0.0761 0.096 Uiso 0.345(7) 1 calc PR B -4 C68 C -0.5738(17) 0.0042(19) 0.0436(15) 0.049(7) Uiso 0.345(7) 1 d PDU B -4 H68A H -0.6228 0.0490 0.0396 0.059 Uiso 0.345(7) 1 calc PR B -4 H68B H -0.6071 -0.0525 0.0648 0.059 Uiso 0.345(7) 1 calc PR B -4 C69 C -0.5143(14) 0.0289(18) 0.0991(16) 0.052(7) Uiso 0.345(7) 1 d PDU B -4 H69A H -0.5218 0.0918 0.1072 0.062 Uiso 0.345(7) 1 calc PR B -4 H69B H -0.5361 -0.0043 0.1546 0.062 Uiso 0.345(7) 1 calc PR B -4 C70 C 0.442(3) 0.2012(18) 0.504(2) 0.29(2) Uani 1 1 d . . . H70A H 0.3972 0.2352 0.5431 0.437 Uiso 1 1 calc R . . H70B H 0.4222 0.2044 0.4501 0.437 Uiso 1 1 calc R . . H70C H 0.5072 0.2249 0.4943 0.437 Uiso 1 1 calc R . . C71 C 0.438(3) 0.104(2) 0.540(2) 0.29(2) Uani 1 1 d . . . H71A H 0.4557 0.1015 0.5951 0.350 Uiso 1 1 calc R . . H71B H 0.3717 0.0807 0.5500 0.350 Uiso 1 1 calc R . . C72 C 0.5023(19) 0.0488(14) 0.4864(18) 0.184(11) Uani 1 1 d . . . H72A H 0.5692 0.0699 0.4808 0.220 Uiso 1 1 calc R . . H72B H 0.4888 0.0566 0.4300 0.220 Uiso 1 1 calc R . . Cl1 Cl -0.0133(2) 0.10804(19) 0.0861(2) 0.0731(9) Uani 1 1 d . . . Cl2 Cl 0.22920(16) 0.19109(15) 0.07772(16) 0.0520(6) Uani 1 1 d . . . Cl3 Cl 0.48668(17) 0.25472(16) 0.02656(18) 0.0603(7) Uani 1 1 d . . . F1 F -0.1478(5) 0.1537(4) 0.3804(4) 0.086(2) Uani 1 1 d . . . F2 F -0.0045(8) -0.1058(4) 0.4439(5) 0.131(4) Uani 1 1 d . . . F3 F 0.0538(7) 0.2809(6) -0.0347(5) 0.078(3) Uani 0.748(16) 1 d PDU A 1 F3S F 0.1298(14) 0.5243(13) 0.0789(12) 0.051(8) Uani 0.252(16) 1 d PDU A 2 F4 F 0.1951(5) 0.5226(7) -0.1995(4) 0.130(4) Uani 1 1 d . A . F5 F 0.1599(4) 0.3049(4) 0.3674(4) 0.0706(17) Uani 1 1 d . . . F6 F 0.2750(6) 0.0336(4) 0.4325(5) 0.099(2) Uani 1 1 d . . . F7 F 0.3193(4) 0.3319(4) -0.0749(3) 0.0556(14) Uani 1 1 d . . . F8 F 0.4816(4) 0.5341(5) -0.2888(3) 0.081(2) Uani 1 1 d . . . Fe1 Fe 0.06376(9) 0.21749(8) 0.12907(8) 0.0428(4) Uani 1 1 d . A . Fe2 Fe 0.33842(9) 0.30468(8) 0.08600(8) 0.0392(4) Uani 1 1 d . B . Li1 Li -0.1865(18) 0.0932(8) 0.1061(6) 0.089(10) Uiso 0.655(7) 1 d PD B 3 Li1S Li -0.3065(14) 0.056(2) 0.0965(17) 0.056(12) Uiso 0.345(7) 1 d PD B -4 N1 N 0.0172(5) 0.2122(4) 0.2552(4) 0.0382(17) Uani 1 1 d . . . N2 N 0.0518(5) 0.3485(4) 0.1132(4) 0.0378(17) Uani 1 1 d . . . N3 N 0.2989(4) 0.3269(4) 0.2096(4) 0.0335(16) Uani 1 1 d . . . N4 N 0.3393(5) 0.4334(4) 0.0487(4) 0.0343(16) Uani 1 1 d . . . O1 O 0.0996(4) 0.5050(3) 0.2777(3) 0.0325(13) Uani 1 1 d . . . O2 O -0.2206(5) 0.1158(5) -0.0026(4) 0.067(2) Uani 1 1 d DU . . O3 O -0.2345(9) -0.0236(8) 0.1571(7) 0.138(4) Uani 1 1 d DU B . O4 O -0.2681(11) 0.1678(10) 0.1810(9) 0.110(5) Uiso 0.655(7) 1 d PDU B 3 O5 O -0.4216(11) 0.0127(11) 0.0670(11) 0.049(5) Uiso 0.345(7) 1 d PDU B -4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(4) 0.028(4) 0.038(5) -0.005(4) -0.009(4) -0.003(3) C2 0.034(5) 0.030(4) 0.035(5) -0.008(4) -0.006(4) 0.001(4) C3 0.030(5) 0.046(5) 0.053(6) -0.007(4) -0.007(4) 0.001(4) C4 0.043(6) 0.035(5) 0.067(7) -0.014(5) -0.011(5) -0.005(4) C5 0.053(6) 0.029(5) 0.052(6) -0.012(4) -0.015(5) 0.003(4) C6 0.041(5) 0.031(5) 0.037(5) -0.010(4) -0.008(4) 0.007(4) C7 0.043(5) 0.027(4) 0.040(5) -0.011(4) -0.006(4) 0.006(4) C8 0.036(5) 0.033(5) 0.029(4) -0.007(4) -0.008(4) 0.009(4) C9 0.035(5) 0.037(5) 0.036(5) -0.013(4) -0.003(4) 0.010(4) C10 0.031(4) 0.049(5) 0.032(5) -0.007(4) -0.007(4) 0.008(4) C11 0.028(4) 0.037(5) 0.032(5) -0.002(4) -0.002(4) -0.001(4) C12 0.029(4) 0.030(4) 0.029(4) -0.003(3) -0.002(3) 0.003(3) C13 0.022(4) 0.038(5) 0.029(4) -0.009(4) -0.002(3) 0.002(3) C14 0.057(7) 0.049(6) 0.090(9) -0.017(6) -0.018(6) -0.023(5) C15 0.41(4) 0.31(3) 0.114(15) 0.031(18) -0.04(2) -0.34(3) C16 0.094(12) 0.110(13) 0.33(3) -0.066(16) -0.101(16) -0.009(10) C17 0.076(10) 0.103(12) 0.38(3) -0.164(17) -0.009(14) -0.023(9) C18 0.051(6) 0.035(5) 0.057(6) -0.007(4) -0.013(5) 0.015(4) C19 0.049(6) 0.047(6) 0.046(6) -0.019(4) -0.012(4) 0.001(4) C20 0.026(5) 0.070(7) 0.042(5) -0.015(5) -0.006(4) 0.008(4) C21 0.039(7) 0.201(18) 0.106(11) 0.018(11) -0.004(7) 0.042(9) C22 0.042(7) 0.24(2) 0.065(8) -0.061(10) 0.008(6) -0.007(9) C23 0.050(8) 0.097(11) 0.194(18) -0.024(11) 0.047(9) 0.000(7) C24 0.026(4) 0.035(5) 0.030(5) -0.011(4) -0.006(3) 0.000(3) C25 0.031(5) 0.039(5) 0.037(5) -0.004(4) -0.009(4) -0.004(4) C26 0.069(7) 0.024(5) 0.054(6) -0.009(4) -0.025(5) -0.003(5) C27 0.074(8) 0.041(6) 0.069(7) -0.007(5) -0.009(6) 0.002(6) C28 0.155(14) 0.035(7) 0.070(8) 0.004(6) -0.013(8) -0.020(8) C29 0.187(17) 0.043(7) 0.057(8) -0.010(6) -0.043(10) 0.009(9) C30 0.126(12) 0.049(7) 0.086(10) -0.033(7) -0.058(9) 0.040(7) C31 0.098(9) 0.038(6) 0.083(8) -0.019(6) -0.047(7) 0.016(6) C32 0.029(4) 0.032(4) 0.042(5) -0.008(4) -0.011(4) 0.004(4) C33 0.031(5) 0.059(6) 0.029(5) -0.006(4) -0.009(4) 0.015(4) C34 0.071(8) 0.079(9) 0.059(8) -0.022(6) -0.026(6) 0.037(7) C35 0.074(9) 0.161(14) 0.030(7) -0.023(8) -0.023(6) 0.074(10) C36 0.055(8) 0.153(15) 0.052(9) 0.023(10) 0.002(6) 0.047(9) C37 0.041(6) 0.098(9) 0.060(8) 0.027(7) -0.003(5) 0.021(6) C38 0.023(5) 0.094(9) 0.043(6) 0.023(6) -0.005(4) 0.015(5) C39 0.017(4) 0.035(5) 0.034(5) -0.007(4) -0.004(3) 0.000(3) C40 0.026(4) 0.032(5) 0.035(5) -0.009(4) -0.005(3) -0.006(3) C41 0.043(5) 0.032(5) 0.034(5) -0.008(4) -0.010(4) -0.002(4) C42 0.052(6) 0.036(5) 0.046(6) -0.009(4) -0.011(5) -0.002(4) C43 0.087(8) 0.052(7) 0.051(6) 0.003(5) -0.016(6) -0.022(6) C44 0.104(10) 0.033(6) 0.085(9) 0.016(6) -0.047(8) -0.010(6) C45 0.079(8) 0.047(7) 0.074(8) -0.008(6) -0.020(7) 0.011(6) C46 0.089(8) 0.032(5) 0.099(9) -0.006(6) -0.070(7) 0.007(5) C47 0.018(4) 0.035(5) 0.047(5) 0.000(4) -0.007(4) -0.004(3) C48 0.018(4) 0.047(5) 0.039(5) -0.005(4) -0.008(4) 0.010(4) C49 0.036(5) 0.054(6) 0.047(6) -0.008(5) -0.014(4) 0.015(4) C50 0.043(6) 0.082(8) 0.041(6) -0.010(5) -0.019(5) 0.025(6) C51 0.042(6) 0.096(9) 0.035(6) 0.003(6) -0.009(5) 0.024(6) C52 0.033(5) 0.081(8) 0.044(6) 0.014(6) -0.003(4) 0.001(5) C53 0.024(4) 0.067(7) 0.046(6) 0.005(5) -0.005(4) 0.009(4) C54 0.136(12) 0.088(10) 0.088(10) -0.002(8) -0.003(9) 0.021(9) C55 0.137(13) 0.098(11) 0.085(10) 0.020(8) -0.032(9) -0.009(10) C56 0.208(18) 0.121(14) 0.100(12) 0.013(11) 0.045(12) 0.021(13) C57 0.091(9) 0.086(9) 0.062(7) -0.021(7) -0.026(7) 0.015(7) C58 0.36(3) 0.21(2) 0.20(2) 0.05(2) -0.11(2) -0.02(2) C59 0.36(3) 0.158(19) 0.25(2) 0.051(18) -0.186(19) 0.07(2) C60 0.36(3) 0.171(19) 0.19(2) -0.037(16) -0.07(2) -0.09(2) C61 0.35(2) 0.161(19) 0.084(13) -0.019(13) -0.043(16) -0.039(19) C70 0.40(5) 0.15(2) 0.44(5) -0.10(3) -0.31(5) 0.08(3) C71 0.32(4) 0.24(4) 0.42(6) -0.21(4) -0.25(4) 0.14(3) C72 0.19(2) 0.17(2) 0.22(3) -0.04(2) -0.13(2) -0.04(2) Cl1 0.0699(18) 0.0657(18) 0.098(2) -0.0431(16) -0.0371(16) 0.0014(14) Cl2 0.0405(13) 0.0468(14) 0.0679(16) -0.0266(12) -0.0037(11) 0.0023(10) Cl3 0.0381(13) 0.0538(15) 0.0786(18) -0.0071(13) 0.0074(12) 0.0153(11) F1 0.084(5) 0.068(4) 0.086(5) 0.012(4) 0.011(4) -0.014(4) F2 0.289(12) 0.030(4) 0.087(5) 0.000(3) -0.070(7) 0.008(5) F3 0.112(8) 0.082(7) 0.053(5) -0.027(5) -0.037(5) 0.030(6) F3S 0.043(13) 0.058(15) 0.053(15) 0.017(11) -0.025(11) 0.000(10) F4 0.076(5) 0.242(11) 0.049(4) 0.054(5) 0.004(4) 0.063(6) F5 0.063(4) 0.073(4) 0.066(4) -0.002(3) 0.004(3) -0.003(3) F6 0.147(7) 0.059(4) 0.096(5) 0.030(4) -0.051(5) -0.011(4) F7 0.059(3) 0.055(3) 0.054(3) -0.018(3) -0.011(3) 0.008(3) F8 0.066(4) 0.129(6) 0.039(3) 0.012(3) 0.000(3) 0.012(4) Fe1 0.0413(7) 0.0388(7) 0.0485(8) -0.0195(6) -0.0054(6) 0.0015(6) Fe2 0.0352(7) 0.0360(7) 0.0427(8) -0.0115(6) 0.0008(6) 0.0026(5) N1 0.041(4) 0.032(4) 0.045(4) -0.014(3) -0.015(3) 0.005(3) N2 0.034(4) 0.043(4) 0.038(4) -0.011(3) -0.008(3) 0.004(3) N3 0.029(4) 0.031(4) 0.039(4) -0.008(3) -0.004(3) 0.001(3) N4 0.030(4) 0.040(4) 0.033(4) -0.006(3) -0.007(3) 0.004(3) O1 0.027(3) 0.028(3) 0.040(3) -0.012(2) 0.000(2) -0.001(2) O2 0.070(5) 0.063(5) 0.061(5) -0.004(4) -0.003(4) 0.012(4) O3 0.179(11) 0.132(10) 0.082(8) 0.035(7) -0.003(8) 0.035(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.364(9) . ? C1 C6 1.383(11) . ? C1 C2 1.410(11) . ? C2 C3 1.390(11) . ? C2 C39 1.493(11) . ? C3 C4 1.381(12) . ? C3 H3 0.9500 . ? C4 C5 1.385(13) . ? C4 C14 1.538(12) . ? C5 C6 1.391(12) . ? C5 H5 0.9500 . ? C6 C7 1.533(11) . ? C7 C8 1.519(11) . ? C7 C19 1.530(12) . ? C7 C18 1.547(12) . ? C8 C13 1.393(11) . ? C8 C9 1.394(11) . ? C9 C10 1.386(12) . ? C9 H9 0.9500 . ? C10 C11 1.397(11) . ? C10 C20 1.527(11) . ? C11 C12 1.385(11) . ? C11 H11 0.9500 . ? C12 C13 1.379(11) . ? C12 C24 1.492(10) . ? C13 O1 1.392(9) . ? C14 C15 1.44(2) . ? C14 C17 1.449(17) . ? C14 C16 1.57(2) . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C15 H15A 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.472(14) . ? C20 C21 1.508(16) . ? C20 C23 1.521(16) . ? 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 C32 1.383(11) . ? C24 C25 1.389(11) . ? C25 N1 1.313(10) . ? C25 H25 0.9500 . ? C26 C31 1.376(14) . ? C26 C27 1.400(14) . ? C26 N1 1.433(11) . ? C27 F1 1.332(12) . ? C27 C28 1.386(15) . ? C28 C29 1.37(2) . ? C28 H28 0.9500 . ? C29 F2 1.345(13) . ? C29 C30 1.359(19) . ? C30 C31 1.395(16) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 N2 1.330(10) . ? C32 H32 0.9500 . ? C33 C34 1.367(13) . ? C33 C38 1.373(14) . ? C33 N2 1.407(11) . ? C34 F3 1.301(12) . ? C34 C35 1.394(17) . ? C34 H38S 0.9073 . ? C35 C36 1.33(2) . ? C35 H35 0.9500 . ? C36 C37 1.32(2) . ? C36 F4 1.374(14) . ? C37 C38 1.378(14) . ? C37 H37 0.9500 . ? C38 F3S 1.221(16) . ? C38 H38 0.9500 . ? C39 C40 1.388(11) . ? C39 C47 1.389(11) . ? C40 N3 1.321(10) . ? C40 H40 0.9500 . ? C41 C42 1.350(12) . ? C41 N3 1.427(10) . ? C41 C46 1.431(13) . ? C42 F5 1.325(10) . ? C42 C43 1.393(13) . ? C43 C44 1.393(16) . ? C43 H43 0.9500 . ? C44 C45 1.343(16) . ? C44 F6 1.360(12) . ? C45 C46 1.367(15) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 N4 1.322(10) . ? C47 H47 0.9500 . ? C48 C49 1.374(12) . ? C48 C53 1.385(12) . ? C48 N4 1.429(10) . ? C49 F7 1.351(11) . ? C49 C50 1.365(13) . ? C50 C51 1.375(15) . ? C50 H50 0.9500 . ? C51 C52 1.349(15) . ? C51 F8 1.358(11) . ? C52 C53 1.391(13) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 O2 1.410(14) . ? C54 C55 1.452(18) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.41(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.432(19) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 O2 1.425(12) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 O3 1.379(13) . ? C58 C59 1.454(19) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.503(18) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.504(18) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 O3 1.265(13) . ? C61 Li1S 2.47(4) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 O4 1.25(2) . ? C62 C63 1.39(3) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.28(3) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.476(17) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 O4 1.40(2) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 O5 1.323(18) . ? C66 C67 1.45(2) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.506(19) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.46(2) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 O5 1.335(17) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.56(4) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.44(4) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C72 1.53(4) 2_656 ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? Cl1 Fe1 2.262(3) . ? Cl1 Li1 2.43(3) . ? Cl2 Fe1 2.361(3) . ? Cl2 Fe2 2.378(3) . ? Cl3 Fe2 2.274(3) . ? F3 H38S 0.3942 . ? F3S H38 0.2967 . ? Fe1 N1 2.021(7) . ? Fe1 N2 2.022(7) . ? Fe2 N4 2.022(7) . ? Fe2 N3 2.038(7) . ? Li1 O4 1.936(15) . ? Li1 O2 1.968(14) . ? Li1 O3 1.971(14) . ? Li1S O5 1.954(17) . ? Li1S O3 1.955(16) . ? Li1S O2 1.957(17) . ? 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 O1 C1 C6 123.9(7) . . ? O1 C1 C2 114.8(6) . . ? C6 C1 C2 121.3(7) . . ? C3 C2 C1 118.2(7) . . ? C3 C2 C39 121.9(7) . . ? C1 C2 C39 119.8(7) . . ? C4 C3 C2 122.1(8) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 117.5(8) . . ? C3 C4 C14 120.8(8) . . ? C5 C4 C14 121.6(8) . . ? C4 C5 C6 123.3(8) . . ? C4 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C1 C6 C5 117.6(8) . . ? C1 C6 C7 121.8(7) . . ? C5 C6 C7 120.5(7) . . ? C8 C7 C19 110.7(7) . . ? C8 C7 C6 109.8(6) . . ? C19 C7 C6 109.0(7) . . ? C8 C7 C18 107.7(7) . . ? C19 C7 C18 110.9(7) . . ? C6 C7 C18 108.7(7) . . ? C13 C8 C9 117.0(7) . . ? C13 C8 C7 123.1(7) . . ? C9 C8 C7 119.8(7) . . ? C10 C9 C8 123.0(7) . . ? C10 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? C9 C10 C11 116.9(7) . . ? C9 C10 C20 120.7(7) . . ? C11 C10 C20 122.3(8) . . ? C12 C11 C10 122.6(8) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C13 C12 C11 117.8(7) . . ? C13 C12 C24 120.8(7) . . ? C11 C12 C24 121.3(7) . . ? C12 C13 O1 115.6(6) . . ? C12 C13 C8 122.7(7) . . ? O1 C13 C8 121.7(7) . . ? C15 C14 C17 118.9(16) . . ? C15 C14 C4 110.5(10) . . ? C17 C14 C4 114.8(10) . . ? C15 C14 C16 100.4(17) . . ? C17 C14 C16 102.6(14) . . ? C4 C14 C16 107.6(10) . . ? C14 C15 H15C 109.5 . . ? C14 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C14 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C7 C18 H18A 109.5 . . ? C7 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C7 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C7 C19 H19A 109.5 . . ? C7 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C7 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C21 112.0(11) . . ? C22 C20 C23 107.8(11) . . ? C21 C20 C23 106.5(11) . . ? C22 C20 C10 110.4(8) . . ? C21 C20 C10 108.0(8) . . ? C23 C20 C10 112.0(8) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C32 C24 C25 126.0(7) . . ? C32 C24 C12 115.7(7) . . ? C25 C24 C12 118.3(7) . . ? N1 C25 C24 126.4(8) . . ? N1 C25 H25 116.8 . . ? C24 C25 H25 116.8 . . ? C31 C26 C27 117.9(9) . . ? C31 C26 N1 120.6(10) . . ? C27 C26 N1 121.4(9) . . ? F1 C27 C28 116.2(11) . . ? F1 C27 C26 120.8(9) . . ? C28 C27 C26 123.0(12) . . ? C29 C28 C27 116.6(13) . . ? C29 C28 H28 121.7 . . ? C27 C28 H28 121.7 . . ? F2 C29 C30 119.5(15) . . ? F2 C29 C28 118.1(15) . . ? C30 C29 C28 122.4(12) . . ? C29 C30 C31 120.3(12) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C26 C31 C30 119.7(12) . . ? C26 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? N2 C32 C24 128.9(8) . . ? N2 C32 H32 115.5 . . ? C24 C32 H32 115.5 . . ? C34 C33 C38 112.8(10) . . ? C34 C33 N2 122.3(9) . . ? C38 C33 N2 125.0(8) . . ? F3 C34 C33 117.6(11) . . ? F3 C34 C35 116.6(12) . . ? C33 C34 C35 125.8(13) . . ? C33 C34 H38S 118.4 . . ? C35 C34 H38S 115.8 . . ? C36 C35 C34 114.9(12) . . ? C36 C35 H35 122.5 . . ? C34 C35 H35 122.5 . . ? C37 C36 C35 125.0(13) . . ? C37 C36 F4 119.2(17) . . ? C35 C36 F4 115.8(16) . . ? C36 C37 C38 117.0(14) . . ? C36 C37 H37 121.5 . . ? C38 C37 H37 121.5 . . ? F3S C38 C33 125.1(13) . . ? F3S C38 C37 110.3(15) . . ? C33 C38 C37 124.5(13) . . ? C33 C38 H38 119.1 . . ? C37 C38 H38 116.4 . . ? C40 C39 C47 125.4(7) . . ? C40 C39 C2 117.0(7) . . ? C47 C39 C2 117.6(7) . . ? N3 C40 C39 126.9(8) . . ? N3 C40 H40 116.6 . . ? C39 C40 H40 116.6 . . ? C42 C41 N3 125.8(8) . . ? C42 C41 C46 117.9(9) . . ? N3 C41 C46 116.2(8) . . ? F5 C42 C41 121.1(8) . . ? F5 C42 C43 114.5(9) . . ? C41 C42 C43 124.3(9) . . ? C44 C43 C42 115.1(10) . . ? C44 C43 H43 122.5 . . ? C42 C43 H43 122.5 . . ? C45 C44 F6 121.4(11) . . ? C45 C44 C43 122.8(10) . . ? F6 C44 C43 115.7(12) . . ? C44 C45 C46 121.2(11) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C45 C46 C41 118.5(11) . . ? C45 C46 H46 120.7 . . ? C41 C46 H46 120.7 . . ? N4 C47 C39 128.0(8) . . ? N4 C47 H47 116.0 . . ? C39 C47 H47 116.0 . . ? C49 C48 C53 116.5(8) . . ? C49 C48 N4 119.9(8) . . ? C53 C48 N4 123.6(8) . . ? F7 C49 C50 117.9(9) . . ? F7 C49 C48 118.6(8) . . ? C50 C49 C48 123.5(10) . . ? C49 C50 C51 117.2(10) . . ? C49 C50 H50 121.4 . . ? C51 C50 H50 121.4 . . ? C52 C51 F8 118.9(11) . . ? C52 C51 C50 123.0(9) . . ? F8 C51 C50 118.0(10) . . ? C51 C52 C53 117.8(10) . . ? C51 C52 H52 121.1 . . ? C53 C52 H52 121.1 . . ? C48 C53 C52 121.9(10) . . ? C48 C53 H53 119.0 . . ? C52 C53 H53 119.0 . . ? O2 C54 C55 107.3(12) . . ? O2 C54 H54A 110.3 . . ? C55 C54 H54A 110.3 . . ? O2 C54 H54B 110.3 . . ? C55 C54 H54B 110.3 . . ? H54A C54 H54B 108.5 . . ? C56 C55 C54 107.1(13) . . ? C56 C55 H55A 110.3 . . ? C54 C55 H55A 110.3 . . ? C56 C55 H55B 110.3 . . ? C54 C55 H55B 110.3 . . ? H55A C55 H55B 108.6 . . ? C55 C56 C57 108.9(14) . . ? C55 C56 H56A 109.9 . . ? C57 C56 H56A 109.9 . . ? C55 C56 H56B 109.9 . . ? C57 C56 H56B 109.9 . . ? H56A C56 H56B 108.3 . . ? O2 C57 C56 106.7(11) . . ? O2 C57 H57A 110.4 . . ? C56 C57 H57A 110.4 . . ? O2 C57 H57B 110.4 . . ? C56 C57 H57B 110.4 . . ? H57A C57 H57B 108.6 . . ? O3 C58 C59 106.2(12) . . ? O3 C58 H58A 110.5 . . ? C59 C58 H58A 110.5 . . ? O3 C58 H58B 110.5 . . ? C59 C58 H58B 110.5 . . ? H58A C58 H58B 108.7 . . ? C58 C59 C60 97.5(12) . . ? C58 C59 H59A 112.3 . . ? C60 C59 H59A 112.3 . . ? C58 C59 H59B 112.3 . . ? C60 C59 H59B 112.3 . . ? H59A C59 H59B 109.9 . . ? C59 C60 C61 95.5(11) . . ? C59 C60 H60A 112.6 . . ? C61 C60 H60A 112.6 . . ? C59 C60 H60B 112.6 . . ? C61 C60 H60B 112.6 . . ? H60A C60 H60B 110.1 . . ? O3 C61 C60 105.8(12) . . ? O3 C61 Li1S 51.5(12) . . ? C60 C61 Li1S 136(2) . . ? O3 C61 H61A 110.6 . . ? C60 C61 H61A 110.6 . . ? Li1S C61 H61A 113.0 . . ? O3 C61 H61B 110.6 . . ? C60 C61 H61B 110.6 . . ? Li1S C61 H61B 61.2 . . ? H61A C61 H61B 108.7 . . ? O4 C62 C63 110(2) . . ? O4 C62 H62A 109.8 . . ? C63 C62 H62A 109.8 . . ? O4 C62 H62B 109.8 . . ? C63 C62 H62B 109.8 . . ? H62A C62 H62B 108.2 . . ? C64 C63 C62 103.5(17) . . ? C64 C63 H63A 111.1 . . ? C62 C63 H63A 111.1 . . ? C64 C63 H63B 111.1 . . ? C62 C63 H63B 111.1 . . ? H63A C63 H63B 109.0 . . ? C63 C64 C65 111.9(16) . . ? C63 C64 H64A 109.2 . . ? C65 C64 H64A 109.2 . . ? C63 C64 H64B 109.2 . . ? C65 C64 H64B 109.2 . . ? H64A C64 H64B 107.9 . . ? O4 C65 C64 96.9(17) . . ? O4 C65 H65A 112.4 . . ? C64 C65 H65A 112.4 . . ? O4 C65 H65B 112.4 . . ? C64 C65 H65B 112.4 . . ? H65A C65 H65B 109.9 . . ? O5 C66 C67 119(3) . . ? O5 C66 H66A 107.6 . . ? C67 C66 H66A 107.6 . . ? O5 C66 H66B 107.6 . . ? C67 C66 H66B 107.6 . . ? H66A C66 H66B 107.0 . . ? C66 C67 C68 91(2) . . ? C66 C67 H67A 113.4 . . ? C68 C67 H67A 113.4 . . ? C66 C67 H67B 113.4 . . ? C68 C67 H67B 113.4 . . ? H67A C67 H67B 110.7 . . ? C69 C68 C67 106(2) . . ? C69 C68 H68A 110.6 . . ? C67 C68 H68A 110.6 . . ? C69 C68 H68B 110.6 . . ? C67 C68 H68B 110.6 . . ? H68A C68 H68B 108.7 . . ? O5 C69 C68 111(2) . . ? O5 C69 H69A 109.5 . . ? C68 C69 H69A 109.5 . . ? O5 C69 H69B 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 108.1 . . ? C71 C70 H70A 109.5 . . ? C71 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C71 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 C70 113(4) . . ? C72 C71 H71A 108.9 . . ? C70 C71 H71A 108.9 . . ? C72 C71 H71B 108.9 . . ? C70 C71 H71B 108.9 . . ? H71A C71 H71B 107.7 . . ? C71 C72 C72 117(4) . 2_656 ? C71 C72 H72A 108.0 . . ? C72 C72 H72A 108.0 2_656 . ? C71 C72 H72B 108.0 . . ? C72 C72 H72B 108.0 2_656 . ? H72A C72 H72B 107.3 . . ? Fe1 Cl1 Li1 125.4(3) . . ? Fe1 Cl2 Fe2 116.52(10) . . ? N1 Fe1 N2 94.1(3) . . ? N1 Fe1 Cl1 106.7(2) . . ? N2 Fe1 Cl1 131.1(2) . . ? N1 Fe1 Cl2 115.7(2) . . ? N2 Fe1 Cl2 105.0(2) . . ? Cl1 Fe1 Cl2 104.76(11) . . ? N4 Fe2 N3 92.5(3) . . ? N4 Fe2 Cl3 106.6(2) . . ? N3 Fe2 Cl3 122.0(2) . . ? N4 Fe2 Cl2 130.2(2) . . ? N3 Fe2 Cl2 102.2(2) . . ? Cl3 Fe2 Cl2 104.90(10) . . ? O4 Li1 O2 105.7(10) . . ? O4 Li1 O3 101.5(10) . . ? O2 Li1 O3 109.7(9) . . ? O4 Li1 Cl1 118.2(9) . . ? O2 Li1 Cl1 109.4(7) . . ? O3 Li1 Cl1 111.9(8) . . ? O5 Li1S O3 119.4(15) . . ? O5 Li1S O2 109.7(12) . . ? O3 Li1S O2 110.9(11) . . ? O5 Li1S C61 95.3(14) . . ? O2 Li1S C61 106.7(15) . . ? C25 N1 C26 117.0(7) . . ? C25 N1 Fe1 123.6(6) . . ? C26 N1 Fe1 119.4(5) . . ? C32 N2 C33 116.9(7) . . ? C32 N2 Fe1 120.9(6) . . ? C33 N2 Fe1 122.1(5) . . ? C40 N3 C41 117.9(7) . . ? C40 N3 Fe2 123.8(6) . . ? C41 N3 Fe2 118.3(5) . . ? C47 N4 C48 117.5(7) . . ? C47 N4 Fe2 123.3(6) . . ? C48 N4 Fe2 119.0(5) . . ? C1 O1 C13 119.2(6) . . ? C54 O2 C57 108.7(9) . . ? C54 O2 Li1S 123.2(13) . . ? C57 O2 Li1S 126.3(13) . . ? C54 O2 Li1 114.7(8) . . ? C57 O2 Li1 114.5(8) . . ? C61 O3 C58 109.7(13) . . ? C61 O3 Li1S 98.1(17) . . ? C58 O3 Li1S 146.8(18) . . ? C61 O3 Li1 125.5(10) . . ? C58 O3 Li1 115.2(10) . . ? C62 O4 C65 113.1(16) . . ? C62 O4 Li1 126.0(15) . . ? C65 O4 Li1 120.6(13) . . ? C66 O5 C69 101(2) . . ? C66 O5 Li1S 128(2) . . ? C69 O5 Li1S 129.6(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 179.3(7) . . . . ? C6 C1 C2 C3 -0.5(12) . . . . ? O1 C1 C2 C39 -2.7(11) . . . . ? C6 C1 C2 C39 177.6(8) . . . . ? C1 C2 C3 C4 0.1(13) . . . . ? C39 C2 C3 C4 -177.9(8) . . . . ? C2 C3 C4 C5 0.6(14) . . . . ? C2 C3 C4 C14 177.3(9) . . . . ? C3 C4 C5 C6 -1.0(15) . . . . ? C14 C4 C5 C6 -177.7(9) . . . . ? O1 C1 C6 C5 -179.6(8) . . . . ? C2 C1 C6 C5 0.1(12) . . . . ? O1 C1 C6 C7 -0.7(13) . . . . ? C2 C1 C6 C7 179.1(8) . . . . ? C4 C5 C6 C1 0.6(14) . . . . ? C4 C5 C6 C7 -178.3(9) . . . . ? C1 C6 C7 C8 5.1(11) . . . . ? C5 C6 C7 C8 -176.0(8) . . . . ? C1 C6 C7 C19 126.4(8) . . . . ? C5 C6 C7 C19 -54.7(10) . . . . ? C1 C6 C7 C18 -112.6(9) . . . . ? C5 C6 C7 C18 66.3(10) . . . . ? C19 C7 C8 C13 -126.9(8) . . . . ? C6 C7 C8 C13 -6.6(11) . . . . ? C18 C7 C8 C13 111.7(9) . . . . ? C19 C7 C8 C9 56.1(10) . . . . ? C6 C7 C8 C9 176.4(7) . . . . ? C18 C7 C8 C9 -65.3(10) . . . . ? C13 C8 C9 C10 -0.3(12) . . . . ? C7 C8 C9 C10 176.9(8) . . . . ? C8 C9 C10 C11 0.2(13) . . . . ? C8 C9 C10 C20 -176.1(8) . . . . ? C9 C10 C11 C12 -0.4(12) . . . . ? C20 C10 C11 C12 175.7(8) . . . . ? C10 C11 C12 C13 0.9(12) . . . . ? C10 C11 C12 C24 -176.6(8) . . . . ? C11 C12 C13 O1 178.8(7) . . . . ? C24 C12 C13 O1 -3.7(11) . . . . ? C11 C12 C13 C8 -1.1(12) . . . . ? C24 C12 C13 C8 176.4(7) . . . . ? C9 C8 C13 C12 0.8(12) . . . . ? C7 C8 C13 C12 -176.3(8) . . . . ? C9 C8 C13 O1 -179.1(7) . . . . ? C7 C8 C13 O1 3.8(12) . . . . ? C3 C4 C14 C15 46(2) . . . . ? C5 C4 C14 C15 -137.1(18) . . . . ? C3 C4 C14 C17 -175.9(14) . . . . ? C5 C4 C14 C17 0.7(19) . . . . ? C3 C4 C14 C16 -62.4(15) . . . . ? C5 C4 C14 C16 114.2(13) . . . . ? C9 C10 C20 C22 -53.0(13) . . . . ? C11 C10 C20 C22 131.0(11) . . . . ? C9 C10 C20 C21 69.8(12) . . . . ? C11 C10 C20 C21 -106.2(12) . . . . ? C9 C10 C20 C23 -173.2(11) . . . . ? C11 C10 C20 C23 10.8(14) . . . . ? C13 C12 C24 C32 -59.6(10) . . . . ? C11 C12 C24 C32 117.8(8) . . . . ? C13 C12 C24 C25 120.6(9) . . . . ? C11 C12 C24 C25 -62.0(10) . . . . ? C32 C24 C25 N1 -2.2(13) . . . . ? C12 C24 C25 N1 177.6(8) . . . . ? C31 C26 C27 F1 -177.4(9) . . . . ? N1 C26 C27 F1 -1.2(15) . . . . ? C31 C26 C27 C28 3.8(16) . . . . ? N1 C26 C27 C28 179.9(10) . . . . ? F1 C27 C28 C29 -179.5(11) . . . . ? C26 C27 C28 C29 -0.6(18) . . . . ? C27 C28 C29 F2 177.7(11) . . . . ? C27 C28 C29 C30 -3(2) . . . . ? F2 C29 C30 C31 -177.6(10) . . . . ? C28 C29 C30 C31 3(2) . . . . ? C27 C26 C31 C30 -3.6(15) . . . . ? N1 C26 C31 C30 -179.9(9) . . . . ? C29 C30 C31 C26 0.5(17) . . . . ? C25 C24 C32 N2 0.7(14) . . . . ? C12 C24 C32 N2 -179.1(8) . . . . ? C38 C33 C34 F3 180.0(9) . . . . ? N2 C33 C34 F3 1.2(14) . . . . ? C38 C33 C34 C35 1.5(14) . . . . ? N2 C33 C34 C35 -177.2(9) . . . . ? F3 C34 C35 C36 -179.0(11) . . . . ? C33 C34 C35 C36 -0.5(17) . . . . ? C34 C35 C36 C37 -1.0(19) . . . . ? C34 C35 C36 F4 178.0(9) . . . . ? C35 C36 C37 C38 1.2(18) . . . . ? F4 C36 C37 C38 -177.7(9) . . . . ? C34 C33 C38 F3S -178.5(14) . . . . ? N2 C33 C38 F3S 0.2(18) . . . . ? C34 C33 C38 C37 -1.2(13) . . . . ? N2 C33 C38 C37 177.4(8) . . . . ? C36 C37 C38 F3S 177.6(13) . . . . ? C36 C37 C38 C33 0.0(15) . . . . ? C3 C2 C39 C40 114.0(9) . . . . ? C1 C2 C39 C40 -64.0(10) . . . . ? C3 C2 C39 C47 -64.4(11) . . . . ? C1 C2 C39 C47 117.6(8) . . . . ? C47 C39 C40 N3 -2.3(13) . . . . ? C2 C39 C40 N3 179.5(7) . . . . ? N3 C41 C42 F5 0.5(14) . . . . ? C46 C41 C42 F5 -177.6(8) . . . . ? N3 C41 C42 C43 177.7(9) . . . . ? C46 C41 C42 C43 -0.4(14) . . . . ? F5 C42 C43 C44 178.6(9) . . . . ? C41 C42 C43 C44 1.2(15) . . . . ? C42 C43 C44 C45 -2.7(17) . . . . ? C42 C43 C44 F6 -179.7(9) . . . . ? F6 C44 C45 C46 -179.8(10) . . . . ? C43 C44 C45 C46 3.3(18) . . . . ? C44 C45 C46 C41 -2.3(16) . . . . ? C42 C41 C46 C45 0.8(13) . . . . ? N3 C41 C46 C45 -177.4(8) . . . . ? C40 C39 C47 N4 3.4(13) . . . . ? C2 C39 C47 N4 -178.3(7) . . . . ? C53 C48 C49 F7 178.3(7) . . . . ? N4 C48 C49 F7 -0.2(11) . . . . ? C53 C48 C49 C50 -1.9(12) . . . . ? N4 C48 C49 C50 179.6(8) . . . . ? F7 C49 C50 C51 -179.9(8) . . . . ? C48 C49 C50 C51 0.3(13) . . . . ? C49 C50 C51 C52 1.0(14) . . . . ? C49 C50 C51 F8 -179.6(8) . . . . ? F8 C51 C52 C53 -180.0(8) . . . . ? C50 C51 C52 C53 -0.6(14) . . . . ? C49 C48 C53 C52 2.3(12) . . . . ? N4 C48 C53 C52 -179.3(8) . . . . ? C51 C52 C53 C48 -1.1(13) . . . . ? O2 C54 C55 C56 7(2) . . . . ? C54 C55 C56 C57 0(2) . . . . ? C55 C56 C57 O2 -7(2) . . . . ? O3 C58 C59 C60 -35(3) . . . . ? C58 C59 C60 C61 46(3) . . . . ? C59 C60 C61 O3 -45(3) . . . . ? C59 C60 C61 Li1S -96(2) . . . . ? O4 C62 C63 C64 22(4) . . . . ? C62 C63 C64 C65 -22(4) . . . . ? C63 C64 C65 O4 14(3) . . . . ? O5 C66 C67 C68 -36(4) . . . . ? C66 C67 C68 C69 28(3) . . . . ? C67 C68 C69 O5 -18(3) . . . . ? C70 C71 C72 C72 -175(2) . . . 2_656 ? Li1 Cl1 Fe1 N1 61.0(4) . . . . ? Li1 Cl1 Fe1 N2 -50.1(5) . . . . ? Li1 Cl1 Fe1 Cl2 -175.9(3) . . . . ? Fe2 Cl2 Fe1 N1 -73.9(3) . . . . ? Fe2 Cl2 Fe1 N2 28.3(2) . . . . ? Fe2 Cl2 Fe1 Cl1 168.97(13) . . . . ? Fe1 Cl2 Fe2 N4 -50.2(3) . . . . ? Fe1 Cl2 Fe2 N3 53.7(2) . . . . ? Fe1 Cl2 Fe2 Cl3 -178.04(13) . . . . ? Fe1 Cl1 Li1 O4 -11.5(9) . . . . ? Fe1 Cl1 Li1 O2 109.5(5) . . . . ? Fe1 Cl1 Li1 O3 -128.7(5) . . . . ? O3 C61 Li1S O5 -144.6(17) . . . . ? C60 C61 Li1S O5 -73(2) . . . . ? C60 C61 Li1S O3 71.3(16) . . . . ? O3 C61 Li1S O2 102.9(16) . . . . ? C60 C61 Li1S O2 174.3(16) . . . . ? C24 C25 N1 C26 -178.6(8) . . . . ? C24 C25 N1 Fe1 -0.1(12) . . . . ? C31 C26 N1 C25 -135.8(9) . . . . ? C27 C26 N1 C25 48.2(12) . . . . ? C31 C26 N1 Fe1 45.6(11) . . . . ? C27 C26 N1 Fe1 -130.5(8) . . . . ? N2 Fe1 N1 C25 2.4(7) . . . . ? Cl1 Fe1 N1 C25 -132.8(6) . . . . ? Cl2 Fe1 N1 C25 111.1(6) . . . . ? N2 Fe1 N1 C26 -179.1(6) . . . . ? Cl1 Fe1 N1 C26 45.7(7) . . . . ? Cl2 Fe1 N1 C26 -70.3(7) . . . . ? C24 C32 N2 C33 -173.8(8) . . . . ? C24 C32 N2 Fe1 2.6(11) . . . . ? C34 C33 N2 C32 -153.0(8) . . . . ? C38 C33 N2 C32 28.4(12) . . . . ? C34 C33 N2 Fe1 30.6(11) . . . . ? C38 C33 N2 Fe1 -147.9(7) . . . . ? N1 Fe1 N2 C32 -3.4(6) . . . . ? Cl1 Fe1 N2 C32 112.9(6) . . . . ? Cl2 Fe1 N2 C32 -121.4(6) . . . . ? N1 Fe1 N2 C33 172.8(6) . . . . ? Cl1 Fe1 N2 C33 -70.9(7) . . . . ? Cl2 Fe1 N2 C33 54.8(6) . . . . ? C39 C40 N3 C41 179.2(7) . . . . ? C39 C40 N3 Fe2 -2.3(11) . . . . ? C42 C41 N3 C40 34.0(12) . . . . ? C46 C41 N3 C40 -147.9(8) . . . . ? C42 C41 N3 Fe2 -144.6(7) . . . . ? C46 C41 N3 Fe2 33.5(9) . . . . ? N4 Fe2 N3 C40 4.2(6) . . . . ? Cl3 Fe2 N3 C40 115.6(6) . . . . ? Cl2 Fe2 N3 C40 -128.0(6) . . . . ? N4 Fe2 N3 C41 -177.4(6) . . . . ? Cl3 Fe2 N3 C41 -65.9(6) . . . . ? Cl2 Fe2 N3 C41 50.5(6) . . . . ? C39 C47 N4 C48 -173.8(7) . . . . ? C39 C47 N4 Fe2 0.2(11) . . . . ? C49 C48 N4 C47 -151.7(7) . . . . ? C53 C48 N4 C47 29.9(11) . . . . ? C49 C48 N4 Fe2 34.0(9) . . . . ? C53 C48 N4 Fe2 -144.4(7) . . . . ? N3 Fe2 N4 C47 -3.2(6) . . . . ? Cl3 Fe2 N4 C47 -127.7(6) . . . . ? Cl2 Fe2 N4 C47 105.1(6) . . . . ? N3 Fe2 N4 C48 170.7(6) . . . . ? Cl3 Fe2 N4 C48 46.2(6) . . . . ? Cl2 Fe2 N4 C48 -81.0(6) . . . . ? C6 C1 O1 C13 -2.9(11) . . . . ? C2 C1 O1 C13 177.3(7) . . . . ? C12 C13 O1 C1 -178.5(7) . . . . ? C8 C13 O1 C1 1.4(11) . . . . ? C55 C54 O2 C57 -11.6(16) . . . . ? C55 C54 O2 Li1S -177.2(12) . . . . ? C55 C54 O2 Li1 118.1(13) . . . . ? C56 C57 O2 C54 11.6(17) . . . . ? C56 C57 O2 Li1S 176.6(14) . . . . ? C56 C57 O2 Li1 -118.2(14) . . . . ? O5 Li1S O2 C54 86(2) . . . . ? O3 Li1S O2 C54 -139.6(16) . . . . ? C61 Li1S O2 C54 -171.5(11) . . . . ? O5 Li1S O2 C57 -76.7(17) . . . . ? O3 Li1S O2 C57 57(2) . . . . ? C61 Li1S O2 C57 25.5(16) . . . . ? O5 Li1S O2 Li1 -174(2) . . . . ? O3 Li1S O2 Li1 -40.1(10) . . . . ? C61 Li1S O2 Li1 -72.0(8) . . . . ? O4 Li1 O2 C54 45.3(14) . . . . ? O3 Li1 O2 C54 154.0(10) . . . . ? Cl1 Li1 O2 C54 -82.9(10) . . . . ? O4 Li1 O2 C57 172.1(10) . . . . ? O3 Li1 O2 C57 -79.3(13) . . . . ? Cl1 Li1 O2 C57 43.8(10) . . . . ? O4 Li1 O2 Li1S -69.3(18) . . . . ? O3 Li1 O2 Li1S 39.3(13) . . . . ? Cl1 Li1 O2 Li1S 162.4(15) . . . . ? C60 C61 O3 C58 25(3) . . . . ? Li1S C61 O3 C58 161.6(19) . . . . ? C60 C61 O3 Li1S -136.6(18) . . . . ? C60 C61 O3 Li1 169.2(17) . . . . ? Li1S C61 O3 Li1 -54.1(15) . . . . ? C59 C58 O3 C61 7(3) . . . . ? C59 C58 O3 Li1S 152(2) . . . . ? C59 C58 O3 Li1 -141(2) . . . . ? O5 Li1S O3 C61 41(2) . . . . ? O2 Li1S O3 C61 -88(2) . . . . ? O5 Li1S O3 C58 -106(3) . . . . ? O2 Li1S O3 C58 125(3) . . . . ? C61 Li1S O3 C58 -147(3) . . . . ? O5 Li1S O3 Li1 169(3) . . . . ? O2 Li1S O3 Li1 40.0(10) . . . . ? C61 Li1S O3 Li1 127.6(16) . . . . ? O4 Li1 O3 C61 146.5(19) . . . . ? O2 Li1 O3 C61 35(2) . . . . ? Cl1 Li1 O3 C61 -86.5(19) . . . . ? O4 Li1 O3 C58 -70.9(19) . . . . ? O2 Li1 O3 C58 177.7(17) . . . . ? Cl1 Li1 O3 C58 56.1(18) . . . . ? O4 Li1 O3 Li1S 72.0(18) . . . . ? O2 Li1 O3 Li1S -39.4(13) . . . . ? Cl1 Li1 O3 Li1S -161.0(14) . . . . ? C63 C62 O4 C65 -14(3) . . . . ? C63 C62 O4 Li1 172.5(18) . . . . ? C64 C65 O4 C62 1(3) . . . . ? C64 C65 O4 Li1 174.8(16) . . . . ? O2 Li1 O4 C62 61(2) . . . . ? O3 Li1 O4 C62 -54(2) . . . . ? Cl1 Li1 O4 C62 -176.6(18) . . . . ? O2 Li1 O4 C65 -112.9(17) . . . . ? O3 Li1 O4 C65 132.6(17) . . . . ? Cl1 Li1 O4 C65 10.0(18) . . . . ? C67 C66 O5 C69 27(4) . . . . ? C67 C66 O5 Li1S -140(3) . . . . ? C68 C69 O5 C66 -3(3) . . . . ? C68 C69 O5 Li1S 163.6(19) . . . . ? O3 Li1S O5 C66 -88(3) . . . . ? O2 Li1S O5 C66 41(3) . . . . ? C61 Li1S O5 C66 -69(3) . . . . ? O3 Li1S O5 C69 108(3) . . . . ? O2 Li1S O5 C69 -123(2) . . . . ? C61 Li1S O5 C69 127(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.043 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.104 # Attachment '3.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 663095' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(C6 H3 Me2)Xanthdim]Fe2Cl2O ; _chemical_name_common '((C6 H3 Me2)Xanthdim)Fe2Cl2O' _chemical_melting_point ? _chemical_formula_moiety 'C129 H144 Cl4 Fe4 N8 O4, 2(C7 H8)' _chemical_formula_sum 'C143 H160 Cl4 Fe4 N8 O4' _chemical_formula_weight 2419.99 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' Cl Cl 0.1484 0.1585 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7523(5) _cell_length_b 14.5416(6) _cell_length_c 18.6438(8) _cell_angle_alpha 89.961(3) _cell_angle_beta 107.582(3) _cell_angle_gamma 104.126(3) _cell_volume 3186.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method none _exptl_crystal_F_000 1278 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7196 _exptl_absorpt_correction_T_max 0.7781 _exptl_absorpt_process_details ; The crystal faces were indexed by microscope on the diffractometer. After that a numerical absorption correction basing on a Gaussian algorithsm was applied, which is implemented in the X-RED program (Stoe, 2002). ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a 2-circle goniometer supplied with an area detector. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'long fine focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_collimation '0.5 mm diameter monocapillary' _diffrn_measurement_device 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,220 exposures' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 58833 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 29.31 _reflns_number_total 17124 _reflns_number_gt 13017 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17124 _refine_ls_number_parameters 763 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.33294(13) 0.24668(11) 0.27004(9) 0.0135(3) Uani 1 1 d . . . C2 C -0.26219(13) 0.32299(12) 0.24762(9) 0.0149(3) Uani 1 1 d . . . C3 C -0.29113(14) 0.40896(12) 0.24048(9) 0.0174(3) Uani 1 1 d . . . H3 H -0.2439 0.4608 0.2247 0.021 Uiso 1 1 calc R . . C4 C -0.38759(14) 0.42232(12) 0.25571(9) 0.0166(3) Uani 1 1 d . . . C5 C -0.45498(14) 0.34463(11) 0.27792(9) 0.0157(3) Uani 1 1 d . . . H5 H -0.5209 0.3519 0.2886 0.019 Uiso 1 1 calc R . . C6 C -0.42961(13) 0.25565(11) 0.28534(9) 0.0135(3) Uani 1 1 d . . . C7 C -0.50680(13) 0.17314(11) 0.31044(10) 0.0155(3) Uani 1 1 d . . . C8 C -0.46685(13) 0.08322(11) 0.30768(8) 0.0129(3) Uani 1 1 d . . . C9 C -0.52939(14) -0.00270(11) 0.32414(9) 0.0151(3) Uani 1 1 d . . . H9 H -0.5959 -0.0029 0.3372 0.018 Uiso 1 1 calc R . . C10 C -0.49882(14) -0.08770(12) 0.32228(10) 0.0177(3) Uani 1 1 d . . . C11 C -0.40086(15) -0.08488(12) 0.30240(10) 0.0200(3) Uani 1 1 d . . . H11 H -0.3786 -0.1423 0.3000 0.024 Uiso 1 1 calc R . . C12 C -0.33488(14) -0.00160(12) 0.28608(10) 0.0174(3) Uani 1 1 d . . . C13 C -0.36930(13) 0.08255(11) 0.28923(9) 0.0138(3) Uani 1 1 d . . . C14 C -0.41613(15) 0.51867(12) 0.24540(11) 0.0211(3) Uani 1 1 d . . . C15 C -0.31018(16) 0.59961(13) 0.28400(12) 0.0255(4) Uani 1 1 d . . . H15A H -0.2508 0.5994 0.2607 0.031 Uiso 1 1 calc R . . H15B H -0.2820 0.5903 0.3378 0.031 Uiso 1 1 calc R . . H15C H -0.3302 0.6607 0.2780 0.031 Uiso 1 1 calc R . . C16 C -0.4575(2) 0.53146(15) 0.16045(12) 0.0342(5) Uani 1 1 d . . . H16A H -0.5279 0.4824 0.1363 0.041 Uiso 1 1 calc R . . H16B H -0.3991 0.5256 0.1379 0.041 Uiso 1 1 calc R . . H16C H -0.4719 0.5945 0.1530 0.041 Uiso 1 1 calc R . . C17 C -0.50899(16) 0.52617(13) 0.27939(14) 0.0299(4) Uani 1 1 d . . . H17A H -0.4856 0.5139 0.3329 0.036 Uiso 1 1 calc R . . H17B H -0.5799 0.4792 0.2525 0.036 Uiso 1 1 calc R . . H17C H -0.5211 0.5902 0.2746 0.036 Uiso 1 1 calc R . . C18 C -0.5021(2) 0.19799(13) 0.39188(12) 0.0309(5) Uani 1 1 d . . . H18A H -0.5265 0.2566 0.3939 0.037 Uiso 1 1 calc R . . H18B H -0.4240 0.2073 0.4255 0.037 Uiso 1 1 calc R . . H18C H -0.5528 0.1459 0.4080 0.037 Uiso 1 1 calc R . . C19 C -0.62929(16) 0.15581(14) 0.25747(15) 0.0345(5) Uani 1 1 d . . . H19A H -0.6314 0.1405 0.2058 0.041 Uiso 1 1 calc R . . H19B H -0.6561 0.2132 0.2592 0.041 Uiso 1 1 calc R . . H19C H -0.6786 0.1027 0.2736 0.041 Uiso 1 1 calc R . . C20 C -0.57028(15) -0.18175(12) 0.33814(10) 0.0199(3) Uani 1 1 d . . . C21 C -0.6571(2) -0.16647(15) 0.37549(15) 0.0369(5) Uani 1 1 d . . . H21A H -0.7122 -0.1376 0.3406 0.044 Uiso 1 1 calc R . . H21B H -0.6176 -0.1242 0.4217 0.044 Uiso 1 1 calc R . . H21C H -0.6970 -0.2278 0.3881 0.044 Uiso 1 1 calc R . . C22 C -0.63478(19) -0.24175(14) 0.26334(12) 0.0351(5) Uani 1 1 d . . . H22A H -0.5806 -0.2501 0.2377 0.042 Uiso 1 1 calc R . . H22B H -0.6887 -0.2094 0.2312 0.042 Uiso 1 1 calc R . . H22C H -0.6763 -0.3041 0.2732 0.042 Uiso 1 1 calc R . . C23 C -0.49433(18) -0.23638(14) 0.39061(12) 0.0285(4) Uani 1 1 d . . . H23A H -0.4532 -0.1983 0.4387 0.034 Uiso 1 1 calc R . . H23B H -0.4397 -0.2493 0.3672 0.034 Uiso 1 1 calc R . . H23C H -0.5414 -0.2966 0.3997 0.034 Uiso 1 1 calc R . . C24 C -0.15594(13) 0.31324(11) 0.23345(9) 0.0152(3) Uani 1 1 d . . . C25 C -0.15660(13) 0.30285(11) 0.15870(9) 0.0141(3) Uani 1 1 d . . . H25 H -0.2261 0.3001 0.1201 0.017 Uiso 1 1 calc R . . C26 C -0.07702(13) 0.30116(11) 0.05907(9) 0.0133(3) Uani 1 1 d . . . C27 C -0.03897(14) 0.23401(12) 0.02751(9) 0.0165(3) Uani 1 1 d . . . H27 H -0.0081 0.1888 0.0581 0.020 Uiso 1 1 calc R . . C28 C -0.04568(15) 0.23261(13) -0.04776(10) 0.0212(3) Uani 1 1 d . . . H28 H -0.0200 0.1865 -0.0692 0.025 Uiso 1 1 calc R . . C29 C -0.09026(15) 0.29919(14) -0.09172(10) 0.0228(4) Uani 1 1 d . . . H29 H -0.0975 0.2969 -0.1440 0.027 Uiso 1 1 calc R . . C30 C -0.12462(15) 0.36918(13) -0.06086(10) 0.0208(3) Uani 1 1 d . . . C31 C -0.11659(13) 0.37237(11) 0.01621(9) 0.0160(3) Uani 1 1 d . . . C32 C -0.16937(18) 0.44242(15) -0.10986(11) 0.0316(4) Uani 1 1 d . . . H32A H -0.1724 0.4283 -0.1619 0.038 Uiso 1 1 calc R . . H32B H -0.1188 0.5058 -0.0911 0.038 Uiso 1 1 calc R . . H32C H -0.2459 0.4408 -0.1083 0.038 Uiso 1 1 calc R . . C33 C -0.14385(16) 0.45378(12) 0.05045(11) 0.0226(4) Uani 1 1 d . . . H33A H -0.1095 0.4588 0.1054 0.027 Uiso 1 1 calc R . . H33B H -0.2266 0.4425 0.0379 0.027 Uiso 1 1 calc R . . H33C H -0.1132 0.5131 0.0303 0.027 Uiso 1 1 calc R . . C34 C -0.05897(10) 0.32769(9) 0.29633(6) 0.0166(3) Uani 1 1 d . . . H34 H -0.0678 0.3404 0.3439 0.020 Uiso 1 1 calc R . . C35 C 0.13416(10) 0.34744(9) 0.36656(6) 0.0222(4) Uani 1 1 d RD . . C36 C 0.13819(10) 0.27427(9) 0.41452(6) 0.0287(9) Uani 0.512(3) 1 d PRDU A 1 H36 H 0.0807 0.2161 0.4003 0.034 Uiso 0.512(3) 1 d PR A 1 C36S C 0.1892(3) 0.2850(2) 0.39548(17) 0.0349(10) Uiso 0.488(3) 1 d PDU A 2 H36S H 0.1714 0.2254 0.3678 0.042 Uiso 0.488(3) 1 d PR A 2 C37 C 0.2260(3) 0.2849(2) 0.48387(17) 0.0334(10) Uani 0.512(3) 1 d PRDU A 1 H37 H 0.2320 0.2349 0.5164 0.040 Uiso 0.512(3) 1 d PR A 1 C37S C 0.27139(12) 0.30171(10) 0.46413(8) 0.0438(13) Uiso 0.488(3) 1 d PDU A 2 H37S H 0.3033 0.2509 0.4839 0.053 Uiso 0.488(3) 1 d PR A 2 C38 C 0.30674(12) 0.37805(10) 0.50189(8) 0.0443(6) Uani 1 1 d RD . . H38 H 0.3619 0.3929 0.5505 0.053 Uiso 1 1 d R . . C39 C 0.30424(12) 0.44556(10) 0.44901(8) 0.0261(8) Uani 0.512(3) 1 d PRDU A 1 C39S C 0.26145(12) 0.46587(10) 0.46860(8) 0.0301(9) Uiso 0.488(3) 1 d PRDU A 2 C40 C 0.21430(12) 0.42735(10) 0.38338(8) 0.0180(7) Uani 0.512(3) 1 d PRDU A 1 C40S C 0.17379(12) 0.44876(10) 0.39849(8) 0.0205(7) Uiso 0.488(3) 1 d PRDU A 2 C41 C 0.39521(12) 0.53322(10) 0.47267(8) 0.0355(10) Uani 0.512(3) 1 d PRD A 1 H41A H 0.3842 0.5779 0.4334 0.053 Uiso 0.512(3) 1 d PR A 1 H41B H 0.4689 0.5187 0.4807 0.053 Uiso 0.512(3) 1 d PR A 1 H41C H 0.3936 0.5618 0.5198 0.053 Uiso 0.512(3) 1 d PR A 1 C41S C 0.3035(5) 0.5657(4) 0.5092(3) 0.0453(12) Uiso 0.488(3) 1 d PD A 2 H41D H 0.3638 0.5661 0.5566 0.068 Uiso 0.488(3) 1 d PR A 2 H41E H 0.2402 0.5835 0.5200 0.068 Uiso 0.488(3) 1 d PR A 2 H41F H 0.3335 0.6112 0.4770 0.068 Uiso 0.488(3) 1 d PR A 2 C42 C 0.2098(3) 0.5051(2) 0.32953(19) 0.0217(7) Uani 0.512(3) 1 d PD A 1 H42A H 0.1434 0.4836 0.2845 0.033 Uiso 0.512(3) 1 d PR A 1 H42B H 0.2793 0.5201 0.3148 0.033 Uiso 0.512(3) 1 d PR A 1 H42C H 0.2039 0.5621 0.3544 0.033 Uiso 0.512(3) 1 d PR A 1 C42S C 0.1233(4) 0.5272(3) 0.3603(3) 0.0336(10) Uiso 0.488(3) 1 d PD A 2 H42D H 0.0643 0.5009 0.3126 0.050 Uiso 0.488(3) 1 d PR A 2 H42E H 0.1833 0.5770 0.3503 0.050 Uiso 0.488(3) 1 d PR A 2 H42F H 0.0898 0.5543 0.3934 0.050 Uiso 0.488(3) 1 d PR A 2 C43 C -0.22941(14) -0.00304(12) 0.26679(10) 0.0170(3) Uani 1 1 d . . . C44 C -0.24067(14) -0.02646(11) 0.19131(10) 0.0164(3) Uani 1 1 d . . . H44 H -0.3149 -0.0398 0.1559 0.020 Uiso 1 1 calc R . . C45 C -0.18215(13) -0.07811(11) 0.09246(9) 0.0144(3) Uani 1 1 d . . . C46 C -0.21297(14) -0.17743(11) 0.08277(9) 0.0158(3) Uani 1 1 d . . . C47 C -0.23184(14) -0.22092(12) 0.01136(9) 0.0170(3) Uani 1 1 d . . . C48 C -0.21865(15) -0.16502(13) -0.04719(10) 0.0215(3) Uani 1 1 d . . . H48 H -0.2315 -0.1948 -0.0955 0.026 Uiso 1 1 calc R . . C49 C -0.18724(18) -0.06688(14) -0.03675(10) 0.0262(4) Uani 1 1 d . . . H49 H -0.1785 -0.0297 -0.0775 0.031 Uiso 1 1 calc R . . C50 C -0.16865(16) -0.02307(12) 0.03351(10) 0.0224(4) Uani 1 1 d . . . H50 H -0.1468 0.0444 0.0413 0.027 Uiso 1 1 calc R . . C51 C -0.2223(2) -0.23677(13) 0.14802(11) 0.0293(4) Uani 1 1 d . . . H51A H -0.2906 -0.2333 0.1606 0.035 Uiso 1 1 d R . . H51B H -0.1549 -0.2125 0.1919 0.035 Uiso 1 1 d R . . H51C H -0.2276 -0.3030 0.1339 0.035 Uiso 1 1 d R . . C52 C -0.26212(19) -0.32749(13) -0.00124(12) 0.0289(4) Uani 1 1 d . . . H52A H -0.3298 -0.3548 0.0138 0.035 Uiso 1 1 calc R . . H52B H -0.1984 -0.3515 0.0290 0.035 Uiso 1 1 calc R . . H52C H -0.2779 -0.3457 -0.0548 0.035 Uiso 1 1 calc R . . C53 C -0.13120(8) -0.00177(6) 0.32595(5) 0.0177(3) Uani 1 1 d . . . H53 H -0.1365 0.0029 0.3755 0.021 Uiso 1 1 calc R . . C54 C 0.05141(8) -0.02635(6) 0.38600(5) 0.0183(3) Uani 1 1 d RD . . C55 C 0.01438(8) -0.09459(6) 0.43130(5) 0.0198(7) Uani 0.524(3) 1 d PRDU B 3 C55S C 0.04526(8) -0.11528(6) 0.41564(5) 0.0193(8) Uiso 0.476(3) 1 d PRDU B 4 C56 C 0.09561(8) -0.11176(6) 0.49710(5) 0.0214(7) Uani 0.524(3) 1 d PRDU B 3 C56S C 0.13503(8) -0.12848(6) 0.47680(5) 0.0210(8) Uiso 0.476(3) 1 d PRDU B 4 C57 C 0.21967(8) -0.05991(6) 0.51003(5) 0.0379(5) Uani 1 1 d RD . . H57 H 0.2790 -0.0788 0.5467 0.045 Uiso 1 1 d R . . C58 C 0.24399(18) 0.01464(19) 0.46768(12) 0.0365(5) Uani 1 1 d D B . H58 H 0.3190 0.0549 0.4808 0.044 Uiso 1 1 calc R . . C59 C 0.15979(17) 0.03174(17) 0.40574(12) 0.0338(5) Uani 1 1 d D B . H59 H 0.1773 0.0839 0.3769 0.041 Uiso 1 1 calc R . . C60 C -0.1078(3) -0.1606(2) 0.4136(2) 0.0243(8) Uani 0.524(3) 1 d PDU B 3 H60A H -0.1096 -0.2054 0.4527 0.036 Uiso 0.524(3) 1 d PR B 3 H60B H -0.1293 -0.1960 0.3644 0.036 Uiso 0.524(3) 1 d PR B 3 H60C H -0.1614 -0.1221 0.4123 0.036 Uiso 0.524(3) 1 d PR B 3 C60S C -0.0574(4) -0.1946(3) 0.3811(3) 0.0358(11) Uiso 0.476(3) 1 d PDU B 4 H60D H -0.1100 -0.1723 0.3389 0.054 Uiso 0.476(3) 1 d PR B 4 H60E H -0.0950 -0.2162 0.4190 0.054 Uiso 0.476(3) 1 d PR B 4 H60F H -0.0348 -0.2474 0.3626 0.054 Uiso 0.476(3) 1 d PR B 4 C61 C 0.0616(4) -0.1825(3) 0.5520(2) 0.0279(9) Uani 0.524(3) 1 d PDU B 3 H61A H -0.0189 -0.2164 0.5306 0.042 Uiso 0.524(3) 1 d PR B 3 H61B H 0.0735 -0.1482 0.6002 0.042 Uiso 0.524(3) 1 d PR B 3 H61C H 0.1083 -0.2284 0.5603 0.042 Uiso 0.524(3) 1 d PR B 3 C61S C 0.1265(5) -0.2219(4) 0.5118(3) 0.0390(11) Uiso 0.476(3) 1 d PDU B 4 H61D H 0.0615 -0.2700 0.4791 0.058 Uiso 0.476(3) 1 d PR B 4 H61E H 0.1158 -0.2148 0.5612 0.058 Uiso 0.476(3) 1 d PR B 4 H61F H 0.1965 -0.2420 0.5181 0.058 Uiso 0.476(3) 1 d PR B 4 C62 C 0.40364(17) 0.84223(16) 0.03311(12) 0.0323(5) Uani 1 1 d . . . C63 C 0.42049(18) 0.75151(17) 0.04448(13) 0.0365(5) Uani 1 1 d . . . H63 H 0.4086 0.7214 0.0876 0.044 Uiso 1 1 calc R . . C64 C 0.45410(19) 0.70442(18) -0.00560(14) 0.0397(5) Uani 1 1 d . . . H64 H 0.4648 0.6425 0.0034 0.048 Uiso 1 1 calc R . . C65 C 0.47224(19) 0.74681(19) -0.06875(13) 0.0411(6) Uani 1 1 d . . . H65 H 0.4966 0.7150 -0.1028 0.049 Uiso 1 1 calc R . . C66 C 0.4543(2) 0.83595(18) -0.08134(12) 0.0428(6) Uani 1 1 d . . . H66 H 0.4657 0.8655 -0.1248 0.051 Uiso 1 1 calc R . . C67 C 0.4201(2) 0.88276(16) -0.03158(12) 0.0387(5) Uani 1 1 d . . . H67 H 0.4075 0.9439 -0.0417 0.046 Uiso 1 1 calc R . . C68 C 0.3695(2) 0.89415(18) 0.08818(14) 0.0400(5) Uani 1 1 d . . . H68A H 0.4243 0.8981 0.1386 0.048 Uiso 1 1 calc R . . H68B H 0.2935 0.8598 0.0891 0.048 Uiso 1 1 calc R . . H68C H 0.3681 0.9584 0.0728 0.048 Uiso 1 1 calc R . . C69 C 0.0598(2) 0.63031(17) 0.41068(13) 0.0265(8) Uani 0.50 1 d PG C -1 C70 C -0.01779(19) 0.54433(19) 0.41006(13) 0.0326(9) Uani 0.50 1 d PG C -1 H70 H -0.0846 0.5236 0.3680 0.039 Uiso 0.50 1 calc PR C -1 C71 C 0.0023(2) 0.48877(16) 0.47097(16) 0.0393(10) Uani 0.50 1 d PG C -1 H71 H -0.0508 0.4300 0.4705 0.047 Uiso 0.50 1 calc PR C -1 C72 C 0.1000(3) 0.5192(2) 0.53250(13) 0.0391(10) Uani 0.50 1 d PG C -1 H72 H 0.1137 0.4812 0.5741 0.047 Uiso 0.50 1 calc PR C -1 C73 C 0.17761(19) 0.6051(2) 0.53312(13) 0.0371(10) Uani 0.50 1 d PG C -1 H73 H 0.2444 0.6259 0.5752 0.045 Uiso 0.50 1 calc PR C -1 C74 C 0.1575(2) 0.66072(17) 0.47221(15) 0.0356(10) Uani 0.50 1 d PG C -1 H74 H 0.2106 0.7195 0.4726 0.043 Uiso 0.50 1 calc PR C -1 C75 C 0.0390(4) 0.6896(3) 0.3428(3) 0.0356(9) Uani 0.50 1 d P C -1 H75A H -0.0337 0.7060 0.3343 0.043 Uiso 0.50 1 calc PR C -1 H75B H 0.0367 0.6529 0.2981 0.043 Uiso 0.50 1 calc PR C -1 H75C H 0.1007 0.7480 0.3526 0.043 Uiso 0.50 1 calc PR C -1 Cl1 Cl 0.22695(3) 0.34714(3) 0.19306(2) 0.01800(8) Uani 1 1 d . A . Cl2 Cl 0.11692(3) -0.06844(3) 0.21048(2) 0.01975(8) Uani 1 1 d . A . Fe1 Fe 0.066884(19) 0.266544(16) 0.208827(12) 0.01205(5) Uani 1 1 d . . . Fe2 Fe 0.005615(19) 0.019531(16) 0.225444(12) 0.01179(5) Uani 1 1 d . . . N1 N -0.06829(11) 0.29649(9) 0.13709(7) 0.0128(2) Uani 1 1 d . A . N2 N 0.04371(12) 0.32548(10) 0.29627(8) 0.0155(3) Uani 1 1 d . A . N3 N -0.15644(12) -0.03141(9) 0.16577(8) 0.0148(3) Uani 1 1 d . A . N4 N -0.03133(12) -0.00635(10) 0.32088(7) 0.0147(3) Uani 1 1 d . A . O1 O -0.29892(10) 0.16306(8) 0.27432(7) 0.0158(2) Uani 1 1 d . . . O2 O 0.05044(10) 0.14295(8) 0.21664(7) 0.0178(2) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0133(7) 0.0140(7) 0.0124(7) 0.0018(5) 0.0020(5) 0.0046(6) C2 0.0107(7) 0.0201(8) 0.0129(7) 0.0012(6) 0.0026(6) 0.0037(6) C3 0.0145(7) 0.0180(8) 0.0179(7) 0.0046(6) 0.0039(6) 0.0022(6) C4 0.0142(7) 0.0154(7) 0.0188(8) 0.0036(6) 0.0024(6) 0.0042(6) C5 0.0122(7) 0.0159(7) 0.0185(7) 0.0029(6) 0.0032(6) 0.0047(6) C6 0.0112(7) 0.0151(7) 0.0138(7) 0.0028(5) 0.0026(5) 0.0042(6) C7 0.0127(7) 0.0133(7) 0.0239(8) 0.0055(6) 0.0089(6) 0.0057(6) C8 0.0117(7) 0.0152(7) 0.0120(7) 0.0013(5) 0.0021(5) 0.0057(5) C9 0.0133(7) 0.0159(7) 0.0169(7) 0.0023(6) 0.0048(6) 0.0051(6) C10 0.0163(8) 0.0145(7) 0.0214(8) 0.0006(6) 0.0040(6) 0.0046(6) C11 0.0189(8) 0.0149(7) 0.0278(9) -0.0015(6) 0.0075(7) 0.0069(6) C12 0.0141(7) 0.0176(8) 0.0215(8) -0.0032(6) 0.0055(6) 0.0058(6) C13 0.0124(7) 0.0153(7) 0.0128(7) 0.0005(5) 0.0025(6) 0.0034(6) C14 0.0176(8) 0.0130(7) 0.0299(9) 0.0053(6) 0.0031(7) 0.0041(6) C15 0.0192(9) 0.0166(8) 0.0368(10) 0.0031(7) 0.0067(8) 0.0002(7) C16 0.0389(12) 0.0223(9) 0.0332(11) 0.0081(8) -0.0032(9) 0.0110(8) C17 0.0186(9) 0.0131(8) 0.0578(13) -0.0004(8) 0.0112(9) 0.0044(7) C18 0.0515(13) 0.0171(8) 0.0386(11) 0.0049(7) 0.0340(10) 0.0100(8) C19 0.0112(8) 0.0208(9) 0.0655(15) 0.0190(9) 0.0031(9) 0.0043(7) C20 0.0193(8) 0.0131(7) 0.0266(9) 0.0043(6) 0.0053(7) 0.0054(6) C21 0.0354(11) 0.0219(9) 0.0667(16) 0.0193(10) 0.0318(11) 0.0118(8) C22 0.0346(11) 0.0224(9) 0.0312(10) 0.0073(8) -0.0047(9) -0.0053(8) C23 0.0293(10) 0.0265(9) 0.0288(10) 0.0078(8) 0.0031(8) 0.0127(8) C24 0.0113(7) 0.0165(7) 0.0180(7) 0.0028(6) 0.0056(6) 0.0027(6) C25 0.0104(7) 0.0140(7) 0.0159(7) 0.0026(5) 0.0023(6) 0.0020(5) C26 0.0102(7) 0.0145(7) 0.0130(7) 0.0025(5) 0.0018(5) 0.0014(5) C27 0.0150(7) 0.0163(7) 0.0166(7) 0.0003(6) 0.0025(6) 0.0043(6) C28 0.0176(8) 0.0252(9) 0.0183(8) -0.0049(6) 0.0045(6) 0.0025(7) C29 0.0186(8) 0.0319(9) 0.0126(7) 0.0009(6) 0.0025(6) -0.0002(7) C30 0.0167(8) 0.0232(8) 0.0171(8) 0.0071(6) 0.0011(6) 0.0005(6) C31 0.0112(7) 0.0156(7) 0.0192(8) 0.0044(6) 0.0025(6) 0.0026(6) C32 0.0303(10) 0.0336(10) 0.0247(9) 0.0152(8) 0.0012(8) 0.0063(8) C33 0.0214(8) 0.0182(8) 0.0308(9) 0.0074(7) 0.0083(7) 0.0094(7) C34 0.0151(7) 0.0218(8) 0.0141(7) 0.0030(6) 0.0052(6) 0.0061(6) C35 0.0157(8) 0.0360(10) 0.0149(8) -0.0022(7) 0.0013(6) 0.0110(7) C36 0.0244(19) 0.0248(18) 0.0261(19) 0.0053(14) -0.0051(15) 0.0028(14) C37 0.030(2) 0.032(2) 0.028(2) 0.0128(16) -0.0053(16) 0.0097(17) C38 0.0245(11) 0.0768(18) 0.0222(10) 0.0027(11) -0.0022(8) 0.0075(11) C39 0.0175(17) 0.0294(19) 0.0305(19) -0.0066(15) 0.0086(14) 0.0027(14) C40 0.0201(16) 0.0195(15) 0.0185(15) 0.0029(12) 0.0082(13) 0.0099(12) C41 0.028(2) 0.038(2) 0.027(2) -0.0012(16) -0.0012(16) -0.0033(17) C42 0.0268(18) 0.0202(16) 0.0187(16) 0.0011(12) 0.0072(13) 0.0066(13) C43 0.0141(7) 0.0149(7) 0.0242(8) -0.0013(6) 0.0074(6) 0.0057(6) C44 0.0140(7) 0.0128(7) 0.0220(8) 0.0007(6) 0.0034(6) 0.0055(6) C45 0.0120(7) 0.0167(7) 0.0131(7) 0.0001(6) 0.0013(5) 0.0042(6) C46 0.0161(7) 0.0143(7) 0.0158(7) 0.0018(6) 0.0038(6) 0.0031(6) C47 0.0145(7) 0.0176(7) 0.0181(8) -0.0012(6) 0.0038(6) 0.0043(6) C48 0.0208(8) 0.0290(9) 0.0151(8) 0.0004(6) 0.0032(6) 0.0106(7) C49 0.0342(10) 0.0284(9) 0.0188(8) 0.0098(7) 0.0101(7) 0.0106(8) C50 0.0293(9) 0.0151(7) 0.0234(9) 0.0056(6) 0.0096(7) 0.0047(7) C51 0.0470(12) 0.0180(8) 0.0231(9) 0.0047(7) 0.0140(9) 0.0049(8) C52 0.0362(11) 0.0193(9) 0.0289(10) -0.0061(7) 0.0097(8) 0.0032(8) C53 0.0198(8) 0.0165(7) 0.0185(8) 0.0001(6) 0.0083(6) 0.0051(6) C54 0.0245(8) 0.0190(8) 0.0128(7) 0.0005(6) 0.0030(6) 0.0115(7) C55 0.0284(18) 0.0175(15) 0.0130(14) -0.0014(11) 0.0009(13) 0.0119(13) C56 0.0295(18) 0.0182(15) 0.0161(15) 0.0015(12) 0.0036(13) 0.0101(13) C57 0.0529(14) 0.0322(11) 0.0194(9) -0.0020(8) -0.0123(9) 0.0237(10) C58 0.0219(10) 0.0639(15) 0.0245(10) 0.0104(10) 0.0028(8) 0.0183(10) C59 0.0208(9) 0.0506(13) 0.0299(10) 0.0199(9) 0.0052(8) 0.0123(9) C60 0.0247(18) 0.0207(16) 0.0227(17) 0.0095(13) 0.0019(13) 0.0039(13) C61 0.035(2) 0.0260(18) 0.0202(17) 0.0097(13) 0.0028(15) 0.0113(15) C62 0.0173(9) 0.0359(11) 0.0332(11) 0.0127(9) -0.0014(8) -0.0006(8) C63 0.0244(10) 0.0449(13) 0.0404(12) 0.0238(10) 0.0085(9) 0.0114(9) C64 0.0241(10) 0.0448(13) 0.0466(13) 0.0146(10) 0.0043(9) 0.0109(9) C65 0.0221(10) 0.0537(14) 0.0320(11) -0.0008(10) -0.0031(8) -0.0041(10) C66 0.0411(13) 0.0430(13) 0.0222(10) 0.0049(9) -0.0035(9) -0.0129(10) C67 0.0386(12) 0.0300(10) 0.0268(10) 0.0097(8) -0.0061(9) -0.0086(9) C68 0.0327(12) 0.0412(12) 0.0436(13) 0.0165(10) 0.0074(10) 0.0106(10) C69 0.0224(18) 0.0306(19) 0.0286(19) -0.0047(15) 0.0104(15) 0.0074(15) C70 0.029(2) 0.031(2) 0.033(2) -0.0056(17) 0.0049(17) 0.0046(17) C71 0.041(3) 0.030(2) 0.042(2) 0.0007(19) 0.012(2) 0.0008(19) C72 0.048(3) 0.049(3) 0.029(2) 0.0069(19) 0.015(2) 0.024(2) C73 0.027(2) 0.058(3) 0.025(2) -0.0081(19) 0.0064(16) 0.011(2) C74 0.026(2) 0.046(3) 0.033(2) -0.0067(19) 0.0141(17) -0.0003(18) C75 0.035(2) 0.037(2) 0.038(2) 0.0029(18) 0.0143(19) 0.0126(19) Cl1 0.01225(17) 0.01784(18) 0.02277(19) 0.00329(14) 0.00501(14) 0.00236(14) Cl2 0.01883(19) 0.02178(19) 0.02152(19) -0.00208(15) 0.00539(15) 0.01157(15) Fe1 0.01047(10) 0.01269(10) 0.01315(10) 0.00277(8) 0.00284(8) 0.00434(8) Fe2 0.01197(10) 0.01174(10) 0.01257(10) 0.00089(8) 0.00336(8) 0.00524(8) N1 0.0126(6) 0.0137(6) 0.0121(6) 0.0025(5) 0.0031(5) 0.0043(5) N2 0.0139(6) 0.0185(6) 0.0141(6) 0.0021(5) 0.0024(5) 0.0064(5) N3 0.0149(6) 0.0134(6) 0.0160(6) 0.0001(5) 0.0031(5) 0.0053(5) N4 0.0159(6) 0.0159(6) 0.0133(6) 0.0025(5) 0.0034(5) 0.0072(5) O1 0.0127(5) 0.0156(5) 0.0217(6) 0.0034(4) 0.0078(4) 0.0054(4) O2 0.0183(6) 0.0147(5) 0.0199(6) 0.0044(4) 0.0044(5) 0.0055(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 C1 C6 1.382(2) . ? C1 O1 1.3818(19) . ? C1 C2 1.399(2) . ? C2 C3 1.383(2) . ? C2 C24 1.495(2) . ? C3 C4 1.400(2) . ? C3 H3 0.9500 . ? C4 C5 1.388(2) . ? C4 C14 1.529(2) . ? C5 C6 1.405(2) . ? C5 H5 0.9500 . ? C6 C7 1.526(2) . ? C7 C8 1.521(2) . ? C7 C19 1.535(2) . ? C7 C18 1.541(3) . ? C8 C13 1.389(2) . ? C8 C9 1.397(2) . ? C9 C10 1.387(2) . ? C9 H9 0.9500 . ? C10 C11 1.398(2) . ? C10 C20 1.530(2) . ? C11 C12 1.387(2) . ? C11 H11 0.9500 . ? C12 C13 1.404(2) . ? C12 C43 1.498(2) . ? C13 O1 1.3750(19) . ? C14 C17 1.527(3) . ? C14 C16 1.538(3) . ? C14 C15 1.538(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C23 1.526(2) . ? C20 C22 1.530(3) . ? C20 C21 1.532(3) . ? 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 C34 1.3948(19) . ? C24 C25 1.399(2) . ? C25 N1 1.328(2) . ? C25 H25 0.9500 . ? C26 C27 1.393(2) . ? C26 C31 1.405(2) . ? C26 N1 1.428(2) . ? C27 C28 1.380(2) . ? C27 H27 0.9500 . ? C28 C29 1.385(3) . ? C28 H28 0.9500 . ? C29 C30 1.389(3) . ? C29 H29 0.9500 . ? C30 C31 1.409(2) . ? C30 C32 1.508(3) . ? C31 C33 1.505(2) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 N2 1.3179(18) . ? C34 H34 0.9500 . ? C35 C36S 1.300(3) . ? C35 C40 1.3116(18) . ? C35 C36 1.3900 . ? C35 N2 1.4344(17) . ? C35 C40S 1.4955(19) . ? C36 C37 1.411(3) . ? C36 H36 0.9500 . ? C36S C37S 1.364(3) . ? C36S H36S 0.9500 . ? C37 C38 1.455(3) . ? C37 H37 0.9500 . ? C37S H37S 0.9500 . ? C38 C39 1.3900 . ? C38 H38 0.9500 . ? C39 C40 1.3737 . ? C39 C41 1.4612 . ? C39S C40S 1.4149 . ? C39S C41S 1.530(5) . ? C40 C42 1.512(4) . ? C40S C42S 1.517(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C41S H41D 0.9800 . ? C41S H41E 0.9800 . ? C41S H41F 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C42S H42D 0.9800 . ? C42S H42E 0.9800 . ? C42S H42F 0.9800 . ? C43 C53 1.3927(19) . ? C43 C44 1.404(2) . ? C44 N3 1.316(2) . ? C44 H44 0.9500 . ? C45 C50 1.387(2) . ? C45 C46 1.398(2) . ? C45 N3 1.435(2) . ? C46 C47 1.401(2) . ? C46 C51 1.508(2) . ? C47 C48 1.387(2) . ? C47 C52 1.503(2) . ? C48 C49 1.382(3) . ? C48 H48 0.9500 . ? C49 C50 1.385(3) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 N4 1.3226(17) . ? C53 H53 0.9500 . ? C54 C59 1.372(2) . ? C54 C55 1.3900 . ? C54 C55S 1.3999 . ? C54 N4 1.4308(16) . ? C55 C56 1.4137 . ? C55 C60 1.555(4) . ? C55S C56S 1.4021 . ? C55S C60S 1.488(5) . ? C56 C57 1.5223 . ? C56 C61 1.531(4) . ? C56S C61S 1.502(5) . ? C57 C58 1.370(3) . ? C57 H57 0.9500 . ? C58 C59 1.389(3) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C60S H60D 0.9800 . ? C60S H60E 0.9800 . ? C60S H60F 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C61S H61D 0.9800 . ? C61S H61E 0.9800 . ? C61S H61F 0.9800 . ? C62 C67 1.392(3) . ? C62 C63 1.393(3) . ? C62 C68 1.499(4) . ? C63 C64 1.382(4) . ? C63 H63 0.9500 . ? C64 C65 1.383(3) . ? C64 H64 0.9500 . ? C65 C66 1.378(4) . ? C65 H65 0.9500 . ? C66 C67 1.380(4) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.3900 . ? C69 C74 1.3900 . ? C69 C75 1.523(5) . ? C70 C71 1.3900 . ? C70 H70 0.9500 . ? C71 C72 1.3900 . ? C71 H71 0.9500 . ? C72 C73 1.3900 . ? C72 H72 0.9500 . ? C73 C74 1.3900 . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? Cl1 Fe1 2.1957(4) . ? Cl2 Fe2 2.2034(4) . ? Fe1 O2 1.7690(12) . ? Fe1 N2 1.9739(14) . ? Fe1 N1 1.9805(13) . ? Fe2 O2 1.7692(12) . ? Fe2 N3 1.9804(14) . ? Fe2 N4 1.9871(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 O1 123.65(14) . . ? C6 C1 C2 121.66(15) . . ? O1 C1 C2 114.68(14) . . ? C3 C2 C1 118.51(15) . . ? C3 C2 C24 120.31(14) . . ? C1 C2 C24 121.17(15) . . ? C2 C3 C4 122.30(15) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C5 C4 C3 117.07(15) . . ? C5 C4 C14 123.12(15) . . ? C3 C4 C14 119.79(15) . . ? C4 C5 C6 122.70(15) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C1 C6 C5 117.76(14) . . ? C1 C6 C7 122.08(14) . . ? C5 C6 C7 120.16(14) . . ? C8 C7 C6 109.92(13) . . ? C8 C7 C19 108.85(14) . . ? C6 C7 C19 109.66(14) . . ? C8 C7 C18 109.44(14) . . ? C6 C7 C18 108.97(14) . . ? C19 C7 C18 109.99(17) . . ? C13 C8 C9 117.81(14) . . ? C13 C8 C7 122.48(14) . . ? C9 C8 C7 119.70(14) . . ? C10 C9 C8 123.04(15) . . ? C10 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? C9 C10 C11 116.95(15) . . ? C9 C10 C20 122.34(15) . . ? C11 C10 C20 120.67(15) . . ? C12 C11 C10 122.59(15) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C11 C12 C13 118.12(15) . . ? C11 C12 C43 119.94(15) . . ? C13 C12 C43 121.94(15) . . ? O1 C13 C8 123.15(14) . . ? O1 C13 C12 115.36(14) . . ? C8 C13 C12 121.48(15) . . ? C17 C14 C4 112.09(14) . . ? C17 C14 C16 108.78(17) . . ? C4 C14 C16 108.54(15) . . ? C17 C14 C15 107.64(16) . . ? C4 C14 C15 110.39(15) . . ? C16 C14 C15 109.35(15) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C7 C18 H18A 109.5 . . ? C7 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C7 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C7 C19 H19A 109.5 . . ? C7 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C7 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C23 C20 C22 109.25(16) . . ? C23 C20 C10 110.60(15) . . ? C22 C20 C10 108.74(15) . . ? C23 C20 C21 107.73(16) . . ? C22 C20 C21 108.40(18) . . ? C10 C20 C21 112.07(15) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C34 C24 C25 124.55(14) . . ? C34 C24 C2 116.42(13) . . ? C25 C24 C2 118.49(14) . . ? N1 C25 C24 125.55(14) . . ? N1 C25 H25 117.2 . . ? C24 C25 H25 117.2 . . ? C27 C26 C31 120.76(15) . . ? C27 C26 N1 116.75(14) . . ? C31 C26 N1 122.41(14) . . ? C28 C27 C26 120.57(16) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.24(17) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C30 121.23(16) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C29 C30 C31 120.10(16) . . ? C29 C30 C32 119.82(17) . . ? C31 C30 C32 120.07(17) . . ? C26 C31 C30 117.91(16) . . ? C26 C31 C33 122.54(15) . . ? C30 C31 C33 119.45(15) . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N2 C34 C24 126.38(12) . . ? N2 C34 H34 116.8 . . ? C24 C34 H34 116.8 . . ? C40 C35 C36 120.79(8) . . ? C40 C35 N2 123.61(12) . . ? C36 C35 N2 115.37(7) . . ? C36S C35 C40S 121.32(17) . . ? C36 C35 C40S 120.08(7) . . ? N2 C35 C40S 116.99(11) . . ? C35 C36 C37 121.13(14) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.5 . . ? C37S C36S H36S 118.7 . . ? C36 C37 C38 115.2(2) . . ? C36 C37 H37 122.4 . . ? C38 C37 H37 122.4 . . ? C36S C37S H37S 118.0 . . ? H37 C37S H37S 54.7 . . ? C39 C38 C37 120.88(13) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.6 . . ? C40 C39 C38 118.2 . . ? C40 C39 C41 126.6 . . ? C38 C39 C41 115.1 . . ? C40S C39S C41S 119.2(2) . . ? C35 C40 C39 123.21(8) . . ? C35 C40 C42 119.95(17) . . ? C39 C40 C42 116.84(15) . . ? C39S C40S C35 114.51(7) . . ? C39S C40S C42S 122.16(18) . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39S C41S H41D 109.5 . . ? C39S C41S H41E 109.5 . . ? H41D C41S H41E 109.5 . . ? C39S C41S H41F 109.5 . . ? H41D C41S H41F 109.5 . . ? H41E C41S H41F 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40S C42S H42D 109.5 . . ? H42C C42S H42D 114.3 . . ? C40S C42S H42E 109.4 . . ? H42D C42S H42E 109.5 . . ? C40S C42S H42F 109.5 . . ? H42D C42S H42F 109.5 . . ? H42E C42S H42F 109.5 . . ? C53 C43 C44 122.59(14) . . ? C53 C43 C12 117.88(14) . . ? C44 C43 C12 117.99(15) . . ? N3 C44 C43 125.12(15) . . ? N3 C44 H44 117.4 . . ? C43 C44 H44 117.4 . . ? C50 C45 C46 121.31(15) . . ? C50 C45 N3 118.73(15) . . ? C46 C45 N3 119.83(14) . . ? C45 C46 C47 118.46(15) . . ? C45 C46 C51 120.98(15) . . ? C47 C46 C51 120.53(15) . . ? C48 C47 C46 119.62(15) . . ? C48 C47 C52 120.00(16) . . ? C46 C47 C52 120.35(15) . . ? C49 C48 C47 121.38(16) . . ? C49 C48 H48 119.3 . . ? C47 C48 H48 119.3 . . ? C48 C49 C50 119.53(16) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C49 C50 C45 119.69(16) . . ? C49 C50 H50 120.2 . . ? C45 C50 H50 120.2 . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N4 C53 C43 127.28(11) . . ? N4 C53 H53 116.4 . . ? C43 C53 H53 116.4 . . ? C59 C54 C55 123.33(9) . . ? C59 C54 C55S 113.54(10) . . ? C59 C54 N4 117.83(12) . . ? C55 C54 N4 118.23(7) . . ? C55S C54 N4 124.81(7) . . ? C54 C55 C56 118.1 . . ? C54 C55 C60 126.03(13) . . ? C56 C55 C60 115.66(13) . . ? C54 C55S C56S 120.0 . . ? C54 C55S C60S 118.9(2) . . ? C56S C55S C60S 121.1(2) . . ? C55 C56 C57 117.4 . . ? C55 C56 C61 121.67(15) . . ? C57 C56 C61 120.87(15) . . ? C57 C56S C55S 121.7 . . ? C57 C56S C61S 117.3(2) . . ? C55S C56S C61S 120.4(2) . . ? C56S C57 C58 116.06(10) . . ? C58 C57 C56 118.54(10) . . ? C58 C57 H57 120.7 . . ? C56 C57 H57 120.7 . . ? C57 C58 C59 120.5(2) . . ? C57 C58 H58 119.8 . . ? C59 C58 H58 119.8 . . ? C54 C59 C58 120.27(19) . . ? C54 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C55 C60 H60A 109.5 . . ? C55 C60 H60B 109.4 . . ? H60A C60 H60B 109.5 . . ? C55 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C55S C60S H60D 109.4 . . ? C55S C60S H60E 109.5 . . ? H60D C60S H60E 109.5 . . ? C55S C60S H60F 109.5 . . ? H60D C60S H60F 109.5 . . ? H60E C60S H60F 109.5 . . ? C56 C61 H61A 109.4 . . ? C56 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C56 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C56S C61S H61D 109.5 . . ? H61C C61S H61D 100.0 . . ? C56S C61S H61E 109.4 . . ? H61D C61S H61E 109.5 . . ? C56S C61S H61F 109.5 . . ? H61C C61S H61F 108.3 . . ? H61D C61S H61F 109.5 . . ? H61E C61S H61F 109.5 . . ? C67 C62 C63 117.2(2) . . ? C67 C62 C68 121.3(2) . . ? C63 C62 C68 121.5(2) . . ? C64 C63 C62 121.5(2) . . ? C64 C63 H63 119.3 . . ? C62 C63 H63 119.3 . . ? C63 C64 C65 120.4(2) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? C66 C65 C64 118.8(3) . . ? C66 C65 H65 120.6 . . ? C64 C65 H65 120.6 . . ? C65 C66 C67 120.8(2) . . ? C65 C66 H66 119.6 . . ? C67 C66 H66 119.6 . . ? C66 C67 C62 121.3(2) . . ? C66 C67 H67 119.3 . . ? C62 C67 H67 119.3 . . ? C62 C68 H68A 109.5 . . ? C62 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C62 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C70 C69 C74 120.0 . . ? C70 C69 C75 119.8(2) . . ? C74 C69 C75 120.2(2) . . ? C71 C70 C69 120.0 . . ? C71 C70 H70 120.0 . . ? C69 C70 H70 120.0 . . ? C70 C71 C72 120.0 . . ? C70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C71 C72 C73 120.0 . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73 120.0 . . ? C72 C73 H73 120.0 . . ? C73 C74 C69 120.0 . . ? C73 C74 H74 120.0 . . ? C69 C74 H74 120.0 . . ? C69 C75 H75A 109.5 . . ? C69 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C69 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? O2 Fe1 N2 110.31(6) . . ? O2 Fe1 N1 112.79(6) . . ? N2 Fe1 N1 92.59(6) . . ? O2 Fe1 Cl1 116.44(4) . . ? N2 Fe1 Cl1 109.56(4) . . ? N1 Fe1 Cl1 112.57(4) . . ? O2 Fe2 N3 110.57(6) . . ? O2 Fe2 N4 111.81(6) . . ? N3 Fe2 N4 90.73(6) . . ? O2 Fe2 Cl2 116.90(4) . . ? N3 Fe2 Cl2 113.79(4) . . ? N4 Fe2 Cl2 110.10(4) . . ? C25 N1 C26 118.83(13) . . ? C25 N1 Fe1 121.03(11) . . ? C26 N1 Fe1 119.78(10) . . ? C34 N2 C35 118.01(13) . . ? C34 N2 Fe1 120.94(10) . . ? C35 N2 Fe1 119.66(9) . . ? C44 N3 C45 119.03(14) . . ? C44 N3 Fe2 122.87(11) . . ? C45 N3 Fe2 118.08(10) . . ? C53 N4 C54 119.05(12) . . ? C53 N4 Fe2 120.45(9) . . ? C54 N4 Fe2 120.45(9) . . ? C13 O1 C1 118.24(12) . . ? Fe1 O2 Fe2 168.04(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.3(2) . . . . ? O1 C1 C2 C3 178.81(14) . . . . ? C6 C1 C2 C24 178.16(14) . . . . ? O1 C1 C2 C24 -2.7(2) . . . . ? C1 C2 C3 C4 0.7(2) . . . . ? C24 C2 C3 C4 -177.74(15) . . . . ? C2 C3 C4 C5 -0.6(2) . . . . ? C2 C3 C4 C14 -178.92(16) . . . . ? C3 C4 C5 C6 0.0(2) . . . . ? C14 C4 C5 C6 178.29(16) . . . . ? O1 C1 C6 C5 -179.26(14) . . . . ? C2 C1 C6 C5 -0.2(2) . . . . ? O1 C1 C6 C7 1.5(2) . . . . ? C2 C1 C6 C7 -179.50(14) . . . . ? C4 C5 C6 C1 0.4(2) . . . . ? C4 C5 C6 C7 179.66(15) . . . . ? C1 C6 C7 C8 -5.5(2) . . . . ? C5 C6 C7 C8 175.27(14) . . . . ? C1 C6 C7 C19 -125.11(18) . . . . ? C5 C6 C7 C19 55.6(2) . . . . ? C1 C6 C7 C18 114.45(17) . . . . ? C5 C6 C7 C18 -64.8(2) . . . . ? C6 C7 C8 C13 3.8(2) . . . . ? C19 C7 C8 C13 123.91(17) . . . . ? C18 C7 C8 C13 -115.85(17) . . . . ? C6 C7 C8 C9 -176.22(14) . . . . ? C19 C7 C8 C9 -56.1(2) . . . . ? C18 C7 C8 C9 64.14(19) . . . . ? C13 C8 C9 C10 -0.5(2) . . . . ? C7 C8 C9 C10 179.53(15) . . . . ? C8 C9 C10 C11 -0.4(2) . . . . ? C8 C9 C10 C20 -178.11(15) . . . . ? C9 C10 C11 C12 0.9(3) . . . . ? C20 C10 C11 C12 178.68(16) . . . . ? C10 C11 C12 C13 -0.6(3) . . . . ? C10 C11 C12 C43 178.66(16) . . . . ? C9 C8 C13 O1 -177.87(14) . . . . ? C7 C8 C13 O1 2.1(2) . . . . ? C9 C8 C13 C12 0.9(2) . . . . ? C7 C8 C13 C12 -179.15(15) . . . . ? C11 C12 C13 O1 178.45(15) . . . . ? C43 C12 C13 O1 -0.7(2) . . . . ? C11 C12 C13 C8 -0.4(2) . . . . ? C43 C12 C13 C8 -179.56(15) . . . . ? C5 C4 C14 C17 13.3(2) . . . . ? C3 C4 C14 C17 -168.49(16) . . . . ? C5 C4 C14 C16 -106.9(2) . . . . ? C3 C4 C14 C16 71.3(2) . . . . ? C5 C4 C14 C15 133.28(18) . . . . ? C3 C4 C14 C15 -48.5(2) . . . . ? C9 C10 C20 C23 -135.26(18) . . . . ? C11 C10 C20 C23 47.1(2) . . . . ? C9 C10 C20 C22 104.8(2) . . . . ? C11 C10 C20 C22 -72.9(2) . . . . ? C9 C10 C20 C21 -15.0(2) . . . . ? C11 C10 C20 C21 167.30(18) . . . . ? C3 C2 C24 C34 93.60(18) . . . . ? C1 C2 C24 C34 -84.84(19) . . . . ? C3 C2 C24 C25 -78.3(2) . . . . ? C1 C2 C24 C25 103.24(18) . . . . ? C34 C24 C25 N1 6.5(3) . . . . ? C2 C24 C25 N1 177.73(15) . . . . ? C31 C26 C27 C28 -3.9(2) . . . . ? N1 C26 C27 C28 179.14(15) . . . . ? C26 C27 C28 C29 0.3(3) . . . . ? C27 C28 C29 C30 2.2(3) . . . . ? C28 C29 C30 C31 -1.3(3) . . . . ? C28 C29 C30 C32 178.09(17) . . . . ? C27 C26 C31 C30 4.7(2) . . . . ? N1 C26 C31 C30 -178.44(14) . . . . ? C27 C26 C31 C33 -171.72(15) . . . . ? N1 C26 C31 C33 5.1(2) . . . . ? C29 C30 C31 C26 -2.2(2) . . . . ? C32 C30 C31 C26 178.45(16) . . . . ? C29 C30 C31 C33 174.37(16) . . . . ? C32 C30 C31 C33 -5.0(2) . . . . ? C25 C24 C34 N2 -6.4(2) . . . . ? C2 C24 C34 N2 -177.77(14) . . . . ? C36S C35 C36 C37 68.5(2) . . . . ? C40 C35 C36 C37 2.37(18) . . . . ? N2 C35 C36 C37 177.0(2) . . . . ? C40S C35 C36 C37 -34.25(18) . . . . ? C40 C35 C36S C37S 40.8(3) . . . . ? C36 C35 C36S C37S -85.6(3) . . . . ? N2 C35 C36S C37S -176.3(2) . . . . ? C40S C35 C36S C37S 13.3(4) . . . . ? C35 C36 C37 C38 2.6(3) . . . . ? C35 C36S C37S C38 -5.7(4) . . . . ? C36S C37S C38 C39 -34.98(18) . . . . ? C36S C37S C38 C37 91.3(3) . . . . ? C36S C37S C38 C39S -3.81(18) . . . . ? C36 C37 C38 C37S -73.8(3) . . . . ? C36 C37 C38 C39 -8.3(3) . . . . ? C36 C37 C38 C39S 28.6(3) . . . . ? C37S C38 C39 C40 38.7 . . . . ? C37 C38 C39 C40 8.94(17) . . . . ? C39S C38 C39 C40 -83.9 . . . . ? C37S C38 C39 C41 -146.0 . . . . ? C37 C38 C39 C41 -175.70(17) . . . . ? C39S C38 C39 C41 91.5 . . . . ? C37S C38 C39S C40S 5.4 . . . . ? C39 C38 C39S C40S 74.8 . . . . ? C37 C38 C39S C40S -30.80(16) . . . . ? C37S C38 C39S C41S -177.2(3) . . . . ? C39 C38 C39S C41S -107.8(3) . . . . ? C37 C38 C39S C41S 146.6(3) . . . . ? C36S C35 C40 C39 -34.54(19) . . . . ? C36 C35 C40 C39 -1.97(11) . . . . ? N2 C35 C40 C39 -176.12(9) . . . . ? C40S C35 C40 C39 96.31(6) . . . . ? C36S C35 C40 C42 145.9(2) . . . . ? C36 C35 C40 C42 178.50(17) . . . . ? N2 C35 C40 C42 4.4(3) . . . . ? C40S C35 C40 C42 -83.22(19) . . . . ? C38 C39 C40 C35 -3.72(10) . . . . ? C41 C39 C40 C35 -178.47(10) . . . . ? C38 C39 C40 C42 175.82(17) . . . . ? C41 C39 C40 C42 1.07(17) . . . . ? C41S C39S C40S C35 -176.1(3) . . . . ? C38 C39S C40S C35 1.49(8) . . . . ? C41S C39S C40S C42S 2.7(3) . . . . ? C38 C39S C40S C42S -179.7(2) . . . . ? C36S C35 C40S C39S -10.5(2) . . . . ? C40 C35 C40S C39S -70.29(6) . . . . ? C36 C35 C40S C39S 30.46(7) . . . . ? N2 C35 C40S C39S 178.74(8) . . . . ? C36S C35 C40S C42S 170.7(3) . . . . ? C40 C35 C40S C42S 110.9(2) . . . . ? C36 C35 C40S C42S -148.3(2) . . . . ? N2 C35 C40S C42S 0.0(3) . . . . ? C11 C12 C43 C53 -80.3(2) . . . . ? C13 C12 C43 C53 98.86(19) . . . . ? C11 C12 C43 C44 85.9(2) . . . . ? C13 C12 C43 C44 -94.9(2) . . . . ? C53 C43 C44 N3 -13.9(3) . . . . ? C12 C43 C44 N3 -179.46(15) . . . . ? C50 C45 C46 C47 -0.9(2) . . . . ? N3 C45 C46 C47 -176.75(14) . . . . ? C50 C45 C46 C51 177.22(18) . . . . ? N3 C45 C46 C51 1.4(2) . . . . ? C45 C46 C47 C48 0.6(2) . . . . ? C51 C46 C47 C48 -177.60(17) . . . . ? C45 C46 C47 C52 178.38(16) . . . . ? C51 C46 C47 C52 0.2(3) . . . . ? C46 C47 C48 C49 0.0(3) . . . . ? C52 C47 C48 C49 -177.87(18) . . . . ? C47 C48 C49 C50 -0.1(3) . . . . ? C48 C49 C50 C45 -0.2(3) . . . . ? C46 C45 C50 C49 0.8(3) . . . . ? N3 C45 C50 C49 176.64(17) . . . . ? C44 C43 C53 N4 11.6(2) . . . . ? C12 C43 C53 N4 177.20(13) . . . . ? C59 C54 C55 C56 -6.91(13) . . . . ? C55S C54 C55 C56 70.6 . . . . ? N4 C54 C55 C56 -177.72(7) . . . . ? C59 C54 C55 C60 178.1(2) . . . . ? C55S C54 C55 C60 -104.40(19) . . . . ? N4 C54 C55 C60 7.32(19) . . . . ? C59 C54 C55S C56S 18.36(12) . . . . ? C55 C54 C55S C56S -98.8 . . . . ? N4 C54 C55S C56S 175.73(8) . . . . ? C59 C54 C55S C60S -161.5(3) . . . . ? C55 C54 C55S C60S 81.3(2) . . . . ? N4 C54 C55S C60S -4.2(2) . . . . ? C54 C55 C56 C57 -5.0 . . . . ? C60 C55 C56 C57 170.51(17) . . . . ? C54 C55 C56 C61 177.37(18) . . . . ? C60 C55 C56 C61 -7.2(2) . . . . ? C54 C55S C56S C57 4.9 . . . . ? C60S C55S C56S C57 -175.3(2) . . . . ? C54 C55S C56S C61S 176.5(2) . . . . ? C60S C55S C56S C61S -3.6(3) . . . . ? C55S C56S C57 C58 -26.05(12) . . . . ? C61S C56S C57 C58 162.0(3) . . . . ? C55S C56S C57 C56 76.6 . . . . ? C61S C56S C57 C56 -95.3(2) . . . . ? C55 C56 C57 C56S -80.0 . . . . ? C61 C56 C57 C56S 97.64(18) . . . . ? C55 C56 C57 C58 13.90(12) . . . . ? C61 C56 C57 C58 -168.4(2) . . . . ? C56S C57 C58 C59 24.2(3) . . . . ? C56 C57 C58 C59 -11.2(3) . . . . ? C55 C54 C59 C58 10.2(3) . . . . ? C55S C54 C59 C58 -19.8(3) . . . . ? N4 C54 C59 C58 -178.90(19) . . . . ? C57 C58 C59 C54 -0.5(3) . . . . ? C67 C62 C63 C64 1.1(3) . . . . ? C68 C62 C63 C64 -178.8(2) . . . . ? C62 C63 C64 C65 0.2(3) . . . . ? C63 C64 C65 C66 -1.1(3) . . . . ? C64 C65 C66 C67 0.7(3) . . . . ? C65 C66 C67 C62 0.6(3) . . . . ? C63 C62 C67 C66 -1.5(3) . . . . ? C68 C62 C67 C66 178.4(2) . . . . ? C74 C69 C70 C71 0.0 . . . . ? C75 C69 C70 C71 178.3(3) . . . . ? C69 C70 C71 C72 0.0 . . . . ? C70 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C69 0.0 . . . . ? C70 C69 C74 C73 0.0 . . . . ? C75 C69 C74 C73 -178.3(3) . . . . ? C24 C25 N1 C26 -170.24(15) . . . . ? C24 C25 N1 Fe1 16.6(2) . . . . ? C27 C26 N1 C25 -134.33(15) . . . . ? C31 C26 N1 C25 48.7(2) . . . . ? C27 C26 N1 Fe1 38.91(18) . . . . ? C31 C26 N1 Fe1 -138.02(13) . . . . ? O2 Fe1 N1 C25 84.35(13) . . . . ? N2 Fe1 N1 C25 -28.98(13) . . . . ? Cl1 Fe1 N1 C25 -141.42(11) . . . . ? O2 Fe1 N1 C26 -88.74(12) . . . . ? N2 Fe1 N1 C26 157.93(11) . . . . ? Cl1 Fe1 N1 C26 45.49(12) . . . . ? C24 C34 N2 C35 176.58(10) . . . . ? C24 C34 N2 Fe1 -16.9(2) . . . . ? C36S C35 N2 C34 118.4(2) . . . . ? C40 C35 N2 C34 -106.65(16) . . . . ? C36 C35 N2 C34 78.91(14) . . . . ? C40S C35 N2 C34 -70.86(18) . . . . ? C36S C35 N2 Fe1 -48.3(2) . . . . ? C40 C35 N2 Fe1 86.69(16) . . . . ? C36 C35 N2 Fe1 -87.75(9) . . . . ? C40S C35 N2 Fe1 122.49(11) . . . . ? O2 Fe1 N2 C34 -86.39(12) . . . . ? N1 Fe1 N2 C34 29.09(12) . . . . ? Cl1 Fe1 N2 C34 144.16(10) . . . . ? O2 Fe1 N2 C35 79.86(12) . . . . ? N1 Fe1 N2 C35 -164.66(11) . . . . ? Cl1 Fe1 N2 C35 -49.59(11) . . . . ? C43 C44 N3 C45 164.82(15) . . . . ? C43 C44 N3 Fe2 -13.3(2) . . . . ? C50 C45 N3 C44 106.57(19) . . . . ? C46 C45 N3 C44 -77.5(2) . . . . ? C50 C45 N3 Fe2 -75.26(18) . . . . ? C46 C45 N3 Fe2 100.67(15) . . . . ? O2 Fe2 N3 C44 -83.52(14) . . . . ? N4 Fe2 N3 C44 30.17(13) . . . . ? Cl2 Fe2 N3 C44 142.57(12) . . . . ? O2 Fe2 N3 C45 98.38(12) . . . . ? N4 Fe2 N3 C45 -147.93(12) . . . . ? Cl2 Fe2 N3 C45 -35.52(12) . . . . ? C43 C53 N4 C54 -165.53(10) . . . . ? C43 C53 N4 Fe2 17.01(18) . . . . ? C59 C54 N4 C53 -130.73(15) . . . . ? C55 C54 N4 C53 40.60(14) . . . . ? C55S C54 N4 C53 72.78(14) . . . . ? C59 C54 N4 Fe2 46.73(17) . . . . ? C55 C54 N4 Fe2 -141.94(6) . . . . ? C55S C54 N4 Fe2 -109.76(8) . . . . ? O2 Fe2 N4 C53 81.22(11) . . . . ? N3 Fe2 N4 C53 -31.34(11) . . . . ? Cl2 Fe2 N4 C53 -147.07(9) . . . . ? O2 Fe2 N4 C54 -96.20(10) . . . . ? N3 Fe2 N4 C54 151.24(10) . . . . ? Cl2 Fe2 N4 C54 35.51(11) . . . . ? C8 C13 O1 C1 -6.7(2) . . . . ? C12 C13 O1 C1 174.48(14) . . . . ? C6 C1 O1 C13 4.9(2) . . . . ? C2 C1 O1 C13 -174.17(13) . . . . ? N2 Fe1 O2 Fe2 57.1(4) . . . . ? N1 Fe1 O2 Fe2 -44.9(4) . . . . ? Cl1 Fe1 O2 Fe2 -177.3(4) . . . . ? N3 Fe2 O2 Fe1 39.5(4) . . . . ? N4 Fe2 O2 Fe1 -60.0(4) . . . . ? Cl2 Fe2 O2 Fe1 171.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 29.31 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.811 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.060