Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Bunz, U.' 'Laskoski, Matthew' 'Smith, Mark D.' 'Steffen, Winfried' _publ_contact_author ; Dr U Bunz Dept of Chemistry and Biochemistry University of South Carolina Columbia SC 29208 USA ; _publ_contact_author_name 'Matt Laskoski' _publ_contact_author_email laskoski@mail.chem.sc.edu data_tbuf1t _database_code_CSD 157834 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H41 Fe O1.25' _chemical_formula_weight 621.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14.3045(13) _cell_length_b 14.9809(13) _cell_length_c 19.1578(17) _cell_angle_alpha 68.628(2) _cell_angle_beta 80.126(2) _cell_angle_gamma 73.762(2) _cell_volume 3659.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8282 _cell_measurement_theta_min 2.172 _cell_measurement_theta_max 24.292 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 0.442 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.5 _diffrn_reflns_number 30460 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0679 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.18 _reflns_number_total 12983 _reflns_number_gt 7496 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.619 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _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 [0.00000+1.00000exp(0.90(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.1306P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12983 _refine_ls_number_parameters 794 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.2221 _refine_ls_wR_factor_gt 0.1962 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.26309(4) 0.66463(4) 0.18355(3) 0.0560(2) Uani 1 1 d . . . C1 C 0.3854(3) 0.7197(3) 0.1564(2) 0.0500(10) Uani 1 1 d . . . C2 C 0.3905(3) 0.6530(3) 0.1178(2) 0.0598(11) Uani 1 1 d . . . H2 H 0.4385 0.5952 0.1219 0.072 Uiso 1 1 calc R . . C3 C 0.3113(3) 0.6887(3) 0.0726(2) 0.0648(12) Uani 1 1 d . . . H3 H 0.2991 0.6594 0.0409 0.078 Uiso 1 1 calc R . . C4 C 0.2538(3) 0.7762(3) 0.0837(2) 0.0601(11) Uani 1 1 d . . . H4 H 0.1964 0.8140 0.0610 0.072 Uiso 1 1 calc R . . C5 C 0.2983(3) 0.7975(3) 0.1357(2) 0.0531(10) Uani 1 1 d . . . C6 C 0.2589(3) 0.8808(3) 0.1600(2) 0.0565(10) Uani 1 1 d . . . C7 C 0.2203(3) 0.9530(3) 0.1760(3) 0.0601(11) Uani 1 1 d . . . C8 C 0.1694(3) 1.0382(3) 0.1972(2) 0.0575(11) Uani 1 1 d . . . C9 C 0.0791(3) 1.0944(3) 0.1703(3) 0.0708(13) Uani 1 1 d . . . H9 H 0.0530 1.0782 0.1365 0.085 Uiso 1 1 calc R . . C10 C 0.0279(4) 1.1729(3) 0.1925(3) 0.0707(13) Uani 1 1 d . . . H10 H -0.0327 1.2080 0.1743 0.085 Uiso 1 1 calc R . . C11 C 0.0644(3) 1.2013(3) 0.2415(3) 0.0625(11) Uani 1 1 d . . . C12 C 0.1552(3) 1.1475(3) 0.2666(3) 0.0633(12) Uani 1 1 d . . . H12 H 0.1818 1.1657 0.2990 0.076 Uiso 1 1 calc R . . C13 C 0.2078(3) 1.0674(3) 0.2452(3) 0.0602(11) Uani 1 1 d . . . C14 C 0.0068(3) 1.2885(3) 0.2673(3) 0.0714(13) Uani 1 1 d . . . C15 C 0.0655(6) 1.3674(5) 0.2432(5) 0.149(3) Uani 1 1 d . . . H15A H 0.0737 1.3929 0.1893 0.224 Uiso 1 1 calc R . . H15B H 0.1284 1.3388 0.2631 0.224 Uiso 1 1 calc R . . H15C H 0.0313 1.4199 0.2620 0.224 Uiso 1 1 calc R . . C16 C -0.0878(6) 1.3382(7) 0.2324(7) 0.216(6) Uani 1 1 d . . . H16A H -0.1250 1.2902 0.2412 0.324 Uiso 1 1 calc R . . H16B H -0.0755 1.3689 0.1792 0.324 Uiso 1 1 calc R . . H16C H -0.1238 1.3874 0.2542 0.324 Uiso 1 1 calc R . . C17 C -0.0094(8) 1.2562(6) 0.3494(5) 0.210(6) Uani 1 1 d . . . H17A H -0.0274 1.3127 0.3656 0.315 Uiso 1 1 calc R . . H17B H 0.0495 1.2129 0.3712 0.315 Uiso 1 1 calc R . . H17C H -0.0609 1.2218 0.3651 0.315 Uiso 1 1 calc R . . C18 C 0.3012(4) 1.0109(3) 0.2718(3) 0.0727(14) Uani 1 1 d . . . C19 C 0.3778(4) 0.9562(4) 0.2885(3) 0.0769(14) Uani 1 1 d . . . C20 C 0.4632(4) 0.8851(4) 0.3064(3) 0.0755(14) Uani 1 1 d . . . C21 C 0.5331(3) 0.8156(4) 0.3180(3) 0.0684(13) Uani 1 1 d . . . C22 C 0.6096(3) 0.7309(3) 0.3227(2) 0.0567(10) Uani 1 1 d . . . C23 C 0.6893(3) 0.7062(3) 0.3649(2) 0.0633(12) Uani 1 1 d . . . H23 H 0.6923 0.7465 0.3912 0.076 Uiso 1 1 calc R . . C24 C 0.7643(3) 0.6227(3) 0.3683(3) 0.0628(12) Uani 1 1 d . . . C25 C 0.7583(3) 0.5662(4) 0.3271(3) 0.0717(13) Uani 1 1 d . . . H25 H 0.8080 0.5104 0.3284 0.086 Uiso 1 1 calc R . . C26 C 0.6817(3) 0.5892(4) 0.2844(3) 0.0703(13) Uani 1 1 d . . . H26 H 0.6812 0.5498 0.2565 0.084 Uiso 1 1 calc R . . C27 C 0.6042(3) 0.6713(3) 0.2822(2) 0.0569(10) Uani 1 1 d . . . C28 C 0.8505(3) 0.5969(4) 0.4153(3) 0.0837(16) Uani 1 1 d . . . C29A C 0.8352(3) 0.6728(4) 0.4542(3) 0.26(2) Uani 0.50 1 d PR . . H29A H 0.8516 0.7319 0.4189 0.315 Uiso 0.50 1 calc PR . . H29B H 0.8763 0.6466 0.4952 0.315 Uiso 0.50 1 calc PR . . H29C H 0.7681 0.6877 0.4730 0.315 Uiso 0.50 1 calc PR . . C30A C 0.9439(3) 0.5987(4) 0.3636(3) 0.183(11) Uani 0.50 1 d PR . . H30A H 0.9288 0.6150 0.3128 0.220 Uiso 0.50 1 calc PR . . H30B H 0.9884 0.5350 0.3789 0.220 Uiso 0.50 1 calc PR . . H30C H 0.9736 0.6474 0.3663 0.220 Uiso 0.50 1 calc PR . . C31A C 0.8587(3) 0.4947(4) 0.4742(3) 0.178(9) Uani 0.50 1 d PR . . H31A H 0.8893 0.4456 0.4510 0.214 Uiso 0.50 1 calc PR . . H31B H 0.7946 0.4863 0.4956 0.214 Uiso 0.50 1 calc PR . . H31C H 0.8972 0.4877 0.5130 0.214 Uiso 0.50 1 calc PR . . C29B C 0.9233(3) 0.5047(4) 0.4071(3) 0.177(11) Uani 0.50 1 d PR . . H29D H 0.9460 0.5162 0.3551 0.213 Uiso 0.50 1 calc PR . . H29E H 0.8922 0.4505 0.4249 0.213 Uiso 0.50 1 calc PR . . H29F H 0.9777 0.4892 0.4361 0.213 Uiso 0.50 1 calc PR . . C30B C 0.8146(3) 0.5787(4) 0.4977(3) 0.159(10) Uani 0.50 1 d PR . . H30D H 0.7870 0.6408 0.5057 0.191 Uiso 0.50 1 calc PR . . H30E H 0.8684 0.5427 0.5284 0.191 Uiso 0.50 1 calc PR . . H30F H 0.7658 0.5412 0.5110 0.191 Uiso 0.50 1 calc PR . . C31B C 0.8999(3) 0.6828(4) 0.3871(3) 0.182(11) Uani 0.50 1 d PR . . H33D H 0.9225 0.6942 0.3352 0.219 Uiso 0.50 1 calc PR . . H33E H 0.9543 0.6673 0.4161 0.219 Uiso 0.50 1 calc PR . . H33F H 0.8540 0.7409 0.3924 0.219 Uiso 0.50 1 calc PR . . C32 C 0.5232(3) 0.6931(3) 0.2396(2) 0.0589(11) Uani 1 1 d . . . C33 C 0.4571(3) 0.7084(3) 0.2039(2) 0.0549(10) Uani 1 1 d . . . C34 C 0.2528(3) 0.5883(3) 0.2952(2) 0.0873(16) Uani 1 1 d G . . H34 H 0.2980 0.5764 0.3291 0.105 Uiso 1 1 calc R . . C35 C 0.2521(3) 0.5272(3) 0.2544(2) 0.0874(16) Uani 1 1 d G . . H35 H 0.2967 0.4678 0.2565 0.105 Uiso 1 1 calc R . . C36 C 0.1719(3) 0.5716(3) 0.2098(2) 0.0901(17) Uani 1 1 d G . . H36 H 0.1543 0.5468 0.1773 0.108 Uiso 1 1 calc R . . C37 C 0.1232(3) 0.6602(3) 0.2231(3) 0.0914(17) Uani 1 1 d G . . H37 H 0.0677 0.7043 0.2009 0.110 Uiso 1 1 calc R . . C38 C 0.1732(3) 0.6706(3) 0.2759(2) 0.0983(19) Uani 1 1 d G . . H38 H 0.1565 0.7226 0.2947 0.118 Uiso 1 1 calc R . . Fe2 Fe 0.67261(5) 0.66299(4) -0.04601(3) 0.0561(2) Uani 1 1 d . . . C51 C 0.7983(3) 0.5756(3) 0.0031(2) 0.0580(11) Uani 1 1 d . . . C52 C 0.8096(3) 0.6738(3) -0.0383(3) 0.0644(12) Uani 1 1 d . . . H52 H 0.8559 0.6907 -0.0782 0.077 Uiso 1 1 calc R . . C53 C 0.7400(4) 0.7393(3) -0.0092(3) 0.0673(12) Uani 1 1 d . . . H53 H 0.7321 0.8074 -0.0263 0.081 Uiso 1 1 calc R . . C54 C 0.6822(4) 0.6849(3) 0.0515(3) 0.0619(11) Uani 1 1 d . . . H54 H 0.6307 0.7113 0.0805 0.074 Uiso 1 1 calc R . . C55 C 0.7181(3) 0.5829(3) 0.0593(2) 0.0540(10) Uani 1 1 d . . . C56 C 0.6775(3) 0.5069(3) 0.1143(2) 0.0583(11) Uani 1 1 d . . . C57 C 0.6382(3) 0.4509(3) 0.1641(2) 0.0608(11) Uani 1 1 d . . . C58 C 0.5869(3) 0.3858(3) 0.2238(2) 0.0566(11) Uani 1 1 d . . . C59 C 0.5201(3) 0.4197(3) 0.2748(3) 0.0657(12) Uani 1 1 d . . . H59 H 0.5084 0.4852 0.2719 0.079 Uiso 1 1 calc R . . C60 C 0.4704(3) 0.3570(3) 0.3301(2) 0.0644(12) Uani 1 1 d . . . H60 H 0.4257 0.3814 0.3640 0.077 Uiso 1 1 calc R . . C61 C 0.4850(3) 0.2572(3) 0.3371(2) 0.0583(11) Uani 1 1 d . . . C62 C 0.5510(3) 0.2252(3) 0.2860(2) 0.0618(11) Uani 1 1 d . . . H62 H 0.5610 0.1602 0.2882 0.074 Uiso 1 1 calc R . . C63 C 0.6042(3) 0.2856(3) 0.2305(2) 0.0578(11) Uani 1 1 d . . . C64 C 0.4240(4) 0.1930(4) 0.3975(3) 0.0715(13) Uani 1 1 d . . . C66 C 0.4515(5) 0.0881(4) 0.3959(4) 0.115(2) Uani 1 1 d . . . H66A H 0.4127 0.0493 0.4346 0.173 Uiso 1 1 calc R . . H66B H 0.5194 0.0600 0.4041 0.173 Uiso 1 1 calc R . . H66C H 0.4396 0.0889 0.3478 0.173 Uiso 1 1 calc R . . C65 C 0.4422(5) 0.1894(4) 0.4743(3) 0.0964(18) Uani 1 1 d . . . H65A H 0.4227 0.2548 0.4771 0.145 Uiso 1 1 calc R . . H65B H 0.5104 0.1629 0.4820 0.145 Uiso 1 1 calc R . . H65C H 0.4049 0.1482 0.5124 0.145 Uiso 1 1 calc R . . C67 C 0.3160(4) 0.2367(5) 0.3837(4) 0.107(2) Uani 1 1 d . . . H67A H 0.2772 0.1991 0.4234 0.161 Uiso 1 1 calc R . . H67B H 0.3045 0.2347 0.3364 0.161 Uiso 1 1 calc R . . H67C H 0.2983 0.3039 0.3827 0.161 Uiso 1 1 calc R . . C68 C 0.6782(4) 0.2492(3) 0.1804(3) 0.0635(12) Uani 1 1 d . . . C69 C 0.7457(4) 0.2318(3) 0.1365(3) 0.0617(11) Uani 1 1 d . . . C70 C 0.8225(4) 0.2257(3) 0.0846(3) 0.0586(11) Uani 1 1 d . . . C71 C 0.8900(3) 0.2307(3) 0.0381(3) 0.0572(11) Uani 1 1 d . . . C72 C 0.9666(3) 0.2485(3) -0.0181(2) 0.0546(10) Uani 1 1 d . . . C73 C 1.0277(3) 0.1739(3) -0.0417(2) 0.0588(11) Uani 1 1 d . . . H73 H 1.0175 0.1106 -0.0193 0.071 Uiso 1 1 calc R . . C74 C 1.1038(3) 0.1886(3) -0.0974(2) 0.0600(11) Uani 1 1 d . . . C75 C 1.1153(3) 0.2852(3) -0.1291(3) 0.0672(12) Uani 1 1 d . . . H75 H 1.1649 0.2991 -0.1667 0.081 Uiso 1 1 calc R . . C76 C 1.0555(3) 0.3603(3) -0.1060(3) 0.0675(12) Uani 1 1 d . . . H76 H 1.0664 0.4234 -0.1283 0.081 Uiso 1 1 calc R . . C77 C 0.9794(3) 0.3455(3) -0.0509(2) 0.0579(11) Uani 1 1 d . . . C78 C 1.1671(4) 0.1032(4) -0.1218(3) 0.0773(14) Uani 1 1 d . . . C79 C 1.2057(5) 0.0162(4) -0.0544(4) 0.133(3) Uani 1 1 d . . . H79A H 1.2398 -0.0390 -0.0702 0.199 Uiso 1 1 calc R . . H79B H 1.1522 -0.0010 -0.0187 0.199 Uiso 1 1 calc R . . H79C H 1.2496 0.0333 -0.0314 0.199 Uiso 1 1 calc R . . C80 C 1.2493(6) 0.1310(5) -0.1766(5) 0.168(4) Uani 1 1 d . . . H80A H 1.2241 0.1829 -0.2209 0.252 Uiso 1 1 calc R . . H80B H 1.2871 0.0747 -0.1899 0.252 Uiso 1 1 calc R . . H80C H 1.2899 0.1533 -0.1547 0.252 Uiso 1 1 calc R . . C81 C 1.1031(6) 0.0667(6) -0.1574(5) 0.155(3) Uani 1 1 d . . . H81A H 1.0833 0.1161 -0.2043 0.232 Uiso 1 1 calc R . . H81B H 1.0464 0.0544 -0.1240 0.232 Uiso 1 1 calc R . . H81C H 1.1398 0.0069 -0.1660 0.232 Uiso 1 1 calc R . . C82 C 0.9158(3) 0.4237(3) -0.0288(3) 0.0615(11) Uani 1 1 d . . . C83 C 0.8595(3) 0.4895(3) -0.0119(2) 0.0598(11) Uani 1 1 d . . . C84 C 0.6346(4) 0.5967(3) -0.1080(3) 0.102(2) Uani 1 1 d G . . H84 H 0.6655 0.5340 -0.1099 0.123 Uiso 1 1 calc R . . C85 C 0.6587(3) 0.6850(4) -0.1549(2) 0.0948(18) Uani 1 1 d G . . H85 H 0.7083 0.6913 -0.1934 0.114 Uiso 1 1 calc R . . C86 C 0.5948(4) 0.7621(3) -0.1338(3) 0.0931(18) Uani 1 1 d G . . H86 H 0.5946 0.8287 -0.1557 0.112 Uiso 1 1 calc R . . C87 C 0.5313(3) 0.7215(4) -0.0738(3) 0.0941(18) Uani 1 1 d G . . H87 H 0.4815 0.7563 -0.0489 0.113 Uiso 1 1 calc R . . C88 C 0.5559(4) 0.6192(4) -0.0578(3) 0.0993(19) Uani 1 1 d G . . H88 H 0.5254 0.5742 -0.0205 0.119 Uiso 1 1 calc R . . O100 O 0.2306(10) -0.0061(11) 0.5795(4) 1.05(4) Uani 1 1 d DU A 1 C100 C 0.2068 0.0000 0.6545 0.94(3) Uani 1 1 d DU A 1 H10A H 0.2419 -0.0569 0.6924 1.130 Uiso 1 1 calc R A 1 H10B H 0.2154 0.0604 0.6576 1.130 Uiso 1 1 calc R A 1 C101 C 0.1107 0.0000 0.6562 0.526(13) Uani 1 1 d DU A 1 H10C H 0.0711 0.0358 0.6885 0.631 Uiso 1 1 calc R A 1 H10D H 0.1028 -0.0672 0.6763 0.631 Uiso 1 1 calc R A 1 C102 C 0.0811 0.0444 0.5841 0.56(2) Uani 1 1 d DU A 1 H10E H 0.0252 0.0996 0.5821 0.669 Uiso 1 1 calc R A 1 H10F H 0.0626 -0.0024 0.5683 0.669 Uiso 1 1 calc R A 1 C103 C 0.1589 0.0768 0.5378 0.76(3) Uani 1 1 d DU A 1 H10G H 0.1646 0.1393 0.5388 0.909 Uiso 1 1 calc R A 1 H10H H 0.1584 0.0796 0.4865 0.909 Uiso 1 1 calc R A 1 O110 O 0.778(3) 0.229(3) 0.5771(16) 0.567(15) Uani 0.50 1 d PDU B 2 C110 C 0.815(3) 0.140(2) 0.557(2) 0.432(14) Uani 0.50 1 d PDU B 2 H11A H 0.8757 0.1382 0.5255 0.518 Uiso 0.50 1 calc PR B 2 H11B H 0.8185 0.0791 0.5998 0.518 Uiso 0.50 1 calc PR B 2 C111 C 0.733(3) 0.168(3) 0.519(2) 0.447(17) Uani 0.50 1 d PDU B 2 H11C H 0.7386 0.1267 0.4886 0.536 Uiso 0.50 1 calc PR B 2 H11D H 0.6754 0.1628 0.5534 0.536 Uiso 0.50 1 calc PR B 2 C112 C 0.728(3) 0.263(2) 0.4739(16) 0.394(16) Uani 0.50 1 d PDU B 2 H11E H 0.6634 0.3048 0.4801 0.473 Uiso 0.50 1 calc PR B 2 H11F H 0.7423 0.2687 0.4214 0.473 Uiso 0.50 1 calc PR B 2 C113 C 0.797(3) 0.288(2) 0.499(2) 0.473(16) Uani 0.50 1 d PDU B 2 H11G H 0.7836 0.3581 0.4916 0.567 Uiso 0.50 1 calc PR B 2 H11H H 0.8628 0.2659 0.4784 0.567 Uiso 0.50 1 calc PR B 2 O120 O 0.4434 0.5013 0.4568 0.294(9) Uiso 0.50 1 d P . 3 H12F H 0.4174 0.4860 0.4207 0.442 Uiso 0.50 1 d P C 3 C120 C 0.5338 0.4246 0.4838 0.276(14) Uiso 0.50 1 d P D 3 H12A H 0.5760 0.4237 0.4392 0.332 Uiso 0.50 1 d P E 3 H12B H 0.5145 0.3631 0.5025 0.332 Uiso 0.50 1 d P F 3 C121 C 0.5994 0.4173 0.5402 0.48(3) Uiso 0.50 1 d P . 3 H12C H 0.6520 0.3596 0.5459 0.714 Uiso 0.50 1 d P G 3 H12D H 0.6255 0.4748 0.5229 0.714 Uiso 0.50 1 d P H 3 H12E H 0.5626 0.4129 0.5877 0.714 Uiso 0.50 1 d P I 3 O130 O 0.4851 0.9235 1.0235 0.174(5) Uiso 0.50 1 d P . 4 H13D H 0.5015 0.8618 1.0310 0.261 Uiso 0.50 1 d P J 4 C130 C 0.5151 0.9781 0.9437 0.154(6) Uiso 0.50 1 d P . 4 H13A H 0.4847 0.9585 0.9124 0.185 Uiso 0.50 1 d P K 4 H13B H 0.5841 0.9528 0.9363 0.185 Uiso 0.50 1 d P L 4 C131 C 0.4971 1.0877 0.9120 0.257(12) Uiso 0.50 1 d P . 4 H13E H 0.5220 1.1069 0.8602 0.386 Uiso 0.50 1 d P M 4 H13C H 0.4282 1.1162 0.9155 0.386 Uiso 0.50 1 d P N 4 H13F H 0.5296 1.1104 0.9398 0.386 Uiso 0.50 1 d P O 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 Fe1 0.0606(4) 0.0452(3) 0.0655(4) -0.0180(3) -0.0216(3) -0.0085(3) C1 0.055(2) 0.044(2) 0.054(2) -0.0171(19) -0.0150(19) -0.0103(19) C2 0.067(3) 0.051(2) 0.060(3) -0.024(2) -0.018(2) 0.002(2) C3 0.084(3) 0.057(3) 0.061(3) -0.028(2) -0.026(2) -0.006(2) C4 0.073(3) 0.045(2) 0.063(3) -0.015(2) -0.032(2) -0.004(2) C5 0.063(3) 0.044(2) 0.057(2) -0.0190(19) -0.016(2) -0.011(2) C6 0.063(3) 0.043(2) 0.066(3) -0.018(2) -0.019(2) -0.008(2) C7 0.059(3) 0.047(2) 0.072(3) -0.018(2) -0.017(2) -0.005(2) C8 0.061(3) 0.041(2) 0.071(3) -0.022(2) -0.013(2) -0.005(2) C9 0.069(3) 0.058(3) 0.090(3) -0.034(3) -0.029(3) 0.002(2) C10 0.064(3) 0.056(3) 0.091(4) -0.026(3) -0.024(3) 0.001(2) C11 0.057(3) 0.048(2) 0.080(3) -0.024(2) -0.007(2) -0.005(2) C12 0.061(3) 0.053(2) 0.084(3) -0.033(2) -0.018(2) -0.006(2) C13 0.054(3) 0.042(2) 0.084(3) -0.024(2) -0.017(2) -0.001(2) C14 0.063(3) 0.053(3) 0.097(4) -0.034(3) -0.004(3) -0.001(2) C15 0.142(6) 0.084(4) 0.240(10) -0.096(6) 0.031(6) -0.027(4) C16 0.115(6) 0.182(9) 0.423(17) -0.229(11) -0.112(8) 0.080(6) C17 0.314(14) 0.108(6) 0.125(7) -0.049(5) 0.062(8) 0.041(7) C18 0.073(3) 0.059(3) 0.103(4) -0.048(3) -0.027(3) 0.001(3) C19 0.069(3) 0.064(3) 0.109(4) -0.050(3) -0.034(3) 0.012(3) C20 0.067(3) 0.080(3) 0.095(4) -0.050(3) -0.026(3) 0.000(3) C21 0.061(3) 0.074(3) 0.081(3) -0.038(3) -0.026(2) -0.004(3) C22 0.046(2) 0.060(3) 0.062(3) -0.022(2) -0.015(2) -0.001(2) C23 0.058(3) 0.071(3) 0.067(3) -0.035(2) -0.018(2) -0.003(2) C24 0.046(2) 0.072(3) 0.067(3) -0.028(2) -0.019(2) 0.005(2) C25 0.061(3) 0.068(3) 0.090(3) -0.041(3) -0.025(3) 0.010(2) C26 0.068(3) 0.072(3) 0.078(3) -0.039(3) -0.018(3) 0.000(3) C27 0.055(3) 0.058(3) 0.059(3) -0.020(2) -0.016(2) -0.008(2) C28 0.062(3) 0.095(4) 0.100(4) -0.047(3) -0.040(3) 0.011(3) C29A 0.18(2) 0.29(3) 0.42(4) -0.28(3) -0.24(3) 0.14(2) C30A 0.046(8) 0.36(3) 0.202(19) -0.15(2) -0.013(10) -0.047(14) C31A 0.168(19) 0.22(2) 0.118(14) 0.030(14) -0.084(13) -0.066(17) C29B 0.124(15) 0.20(2) 0.25(2) -0.18(2) -0.137(16) 0.099(14) C30B 0.102(10) 0.26(2) 0.083(9) -0.094(13) -0.051(8) 0.087(13) C31B 0.068(10) 0.172(16) 0.37(3) -0.16(2) -0.096(14) 0.029(10) C32 0.060(3) 0.056(3) 0.066(3) -0.023(2) -0.017(2) -0.009(2) C33 0.055(3) 0.051(2) 0.062(3) -0.022(2) -0.010(2) -0.010(2) C34 0.100(4) 0.097(4) 0.066(3) -0.014(3) -0.018(3) -0.037(4) C35 0.102(4) 0.057(3) 0.095(4) -0.001(3) -0.034(3) -0.024(3) C36 0.094(4) 0.073(4) 0.103(4) -0.003(3) -0.034(3) -0.039(3) C37 0.063(3) 0.093(4) 0.108(5) -0.018(4) -0.013(3) -0.019(3) C38 0.102(5) 0.094(4) 0.096(4) -0.040(4) 0.026(4) -0.028(4) Fe2 0.0687(4) 0.0399(3) 0.0581(4) -0.0120(3) -0.0107(3) -0.0127(3) C51 0.068(3) 0.043(2) 0.064(3) -0.013(2) -0.017(2) -0.014(2) C52 0.072(3) 0.053(3) 0.071(3) -0.016(2) -0.007(2) -0.024(2) C53 0.085(3) 0.039(2) 0.080(3) -0.017(2) -0.021(3) -0.012(2) C54 0.079(3) 0.046(2) 0.066(3) -0.023(2) -0.012(2) -0.013(2) C55 0.068(3) 0.041(2) 0.054(2) -0.0117(19) -0.016(2) -0.012(2) C56 0.073(3) 0.043(2) 0.055(3) -0.013(2) -0.015(2) -0.007(2) C57 0.072(3) 0.050(2) 0.057(3) -0.013(2) -0.015(2) -0.009(2) C58 0.069(3) 0.049(2) 0.047(2) -0.0059(19) -0.012(2) -0.015(2) C59 0.078(3) 0.051(2) 0.061(3) -0.013(2) -0.005(2) -0.009(2) C60 0.075(3) 0.055(3) 0.055(3) -0.014(2) -0.003(2) -0.008(2) C61 0.065(3) 0.056(3) 0.049(2) -0.012(2) -0.007(2) -0.013(2) C62 0.078(3) 0.047(2) 0.060(3) -0.016(2) -0.006(2) -0.016(2) C63 0.065(3) 0.056(3) 0.049(2) -0.015(2) -0.006(2) -0.011(2) C64 0.092(4) 0.065(3) 0.053(3) -0.011(2) 0.004(2) -0.028(3) C66 0.163(6) 0.079(4) 0.110(5) -0.039(4) 0.052(5) -0.065(4) C65 0.142(5) 0.092(4) 0.052(3) -0.013(3) 0.002(3) -0.043(4) C67 0.084(4) 0.125(5) 0.097(4) -0.009(4) 0.003(3) -0.043(4) C68 0.074(3) 0.052(3) 0.061(3) -0.011(2) -0.010(3) -0.019(2) C69 0.074(3) 0.052(3) 0.056(3) -0.017(2) -0.005(3) -0.013(2) C70 0.067(3) 0.049(2) 0.059(3) -0.019(2) -0.015(2) -0.006(2) C71 0.062(3) 0.053(2) 0.057(3) -0.021(2) -0.013(2) -0.006(2) C72 0.053(2) 0.055(2) 0.054(2) -0.018(2) -0.014(2) -0.005(2) C73 0.060(3) 0.049(2) 0.059(3) -0.012(2) -0.010(2) -0.005(2) C74 0.059(3) 0.051(2) 0.062(3) -0.014(2) -0.010(2) -0.005(2) C75 0.058(3) 0.064(3) 0.072(3) -0.014(2) -0.005(2) -0.012(2) C76 0.061(3) 0.051(3) 0.084(3) -0.015(2) -0.016(3) -0.007(2) C77 0.053(3) 0.052(2) 0.067(3) -0.018(2) -0.016(2) -0.006(2) C78 0.076(3) 0.059(3) 0.085(3) -0.024(3) 0.004(3) -0.003(3) C79 0.140(6) 0.073(4) 0.119(5) -0.004(4) 0.016(5) 0.022(4) C80 0.168(8) 0.094(5) 0.189(8) -0.048(5) 0.106(7) -0.019(5) C81 0.145(7) 0.160(7) 0.202(9) -0.136(7) -0.008(6) -0.006(6) C82 0.058(3) 0.051(3) 0.071(3) -0.016(2) -0.016(2) -0.006(2) C83 0.064(3) 0.048(2) 0.067(3) -0.013(2) -0.016(2) -0.014(2) C84 0.143(6) 0.074(4) 0.114(5) -0.048(4) -0.054(5) -0.012(4) C85 0.092(4) 0.136(6) 0.058(3) -0.033(4) -0.015(3) -0.022(4) C86 0.109(5) 0.069(3) 0.089(4) 0.002(3) -0.044(4) -0.017(3) C87 0.075(4) 0.104(5) 0.112(5) -0.050(4) -0.026(4) -0.005(3) C88 0.105(5) 0.126(6) 0.087(4) -0.029(4) -0.019(4) -0.062(4) O100 0.43(2) 1.12(8) 0.89(5) 0.51(4) 0.03(3) -0.29(3) C100 0.87(5) 0.50(6) 1.32(7) -0.03(6) -0.80(5) 0.12(5) C101 1.01(4) 0.53(3) 0.164(13) -0.047(17) 0.01(2) -0.500 C102 0.45(2) 0.73(5) 0.36(3) 0.11(3) -0.10(2) -0.28(3) C103 0.79(5) 0.41(3) 0.53(3) 0.28(3) 0.31(3) -0.10(3) O110 0.88(5) 0.80(5) 0.35(3) -0.37(4) 0.24(3) -0.640 C110 0.68(4) 0.60(3) 0.21(4) -0.14(2) 0.11(3) -0.542 C111 0.74(5) 0.52(3) 0.27(4) -0.11(3) 0.04(4) -0.520 C112 0.61(5) 0.38(3) 0.32(3) -0.25(2) 0.24(2) -0.32(3) C113 0.67(3) 0.52(2) 0.47(4) -0.35(3) 0.38(3) -0.509 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C38 2.015(4) . ? Fe1 C37 2.025(4) . ? Fe1 C4 2.026(4) . ? Fe1 C34 2.027(4) . ? Fe1 C5 2.031(4) . ? Fe1 C2 2.033(5) . ? Fe1 C36 2.043(4) . ? Fe1 C35 2.044(4) . ? Fe1 C1 2.049(4) . ? Fe1 C3 2.049(5) . ? C1 C33 1.420(6) . ? C1 C2 1.424(5) . ? C1 C5 1.445(5) . ? C2 C3 1.407(6) . ? C3 C4 1.407(6) . ? C4 C5 1.436(5) . ? C5 C6 1.426(5) . ? C6 C7 1.191(5) . ? C7 C8 1.442(6) . ? C8 C13 1.392(6) . ? C8 C9 1.396(6) . ? C9 C10 1.370(6) . ? C10 C11 1.385(6) . ? C11 C12 1.383(6) . ? C11 C14 1.535(6) . ? C12 C13 1.387(6) . ? C13 C18 1.431(6) . ? C14 C17 1.464(9) . ? C14 C16 1.489(9) . ? C14 C15 1.529(8) . ? C18 C19 1.184(6) . ? C19 C20 1.376(7) . ? C20 C21 1.208(6) . ? C21 C22 1.410(6) . ? C22 C23 1.397(6) . ? C22 C27 1.404(6) . ? C23 C24 1.390(6) . ? C24 C25 1.377(6) . ? C24 C28 1.531(5) . ? C25 C26 1.372(6) . ? C26 C27 1.400(6) . ? C27 C32 1.426(6) . ? C28 C31A 1.5219 . ? C28 C30B 1.5219 . ? C28 C30A 1.5220 . ? C28 C29A 1.5220 . ? C28 C29B 1.5220 . ? C28 C31B 1.5221 . ? C32 C33 1.184(5) . ? C34 C35 1.407(3) . ? C34 C38 1.408(3) . ? C35 C36 1.407(3) . ? C36 C37 1.407(3) . ? C37 C38 1.407(3) . ? Fe2 C84 2.019(4) . ? Fe2 C85 2.027(4) . ? Fe2 C88 2.029(4) . ? Fe2 C86 2.042(4) . ? Fe2 C53 2.042(4) . ? Fe2 C54 2.043(4) . ? Fe2 C87 2.043(4) . ? Fe2 C52 2.044(5) . ? Fe2 C55 2.045(4) . ? Fe2 C51 2.049(4) . ? C51 C52 1.433(6) . ? C51 C83 1.437(6) . ? C51 C55 1.443(6) . ? C52 C53 1.389(6) . ? C53 C54 1.433(6) . ? C54 C55 1.429(5) . ? C55 C56 1.425(6) . ? C56 C57 1.194(6) . ? C57 C58 1.448(6) . ? C58 C59 1.378(6) . ? C58 C63 1.412(6) . ? C59 C60 1.378(6) . ? C60 C61 1.410(6) . ? C61 C62 1.361(6) . ? C61 C64 1.528(6) . ? C62 C63 1.391(6) . ? C63 C68 1.432(6) . ? C64 C65 1.517(7) . ? C64 C66 1.520(7) . ? C64 C67 1.528(7) . ? C68 C69 1.204(6) . ? C69 C70 1.355(7) . ? C70 C71 1.196(6) . ? C71 C72 1.408(6) . ? C72 C73 1.379(6) . ? C72 C77 1.409(6) . ? C73 C74 1.392(6) . ? C74 C75 1.396(6) . ? C74 C78 1.522(6) . ? C75 C76 1.374(6) . ? C76 C77 1.385(6) . ? C77 C82 1.419(6) . ? C78 C80 1.480(8) . ? C78 C79 1.513(8) . ? C78 C81 1.538(9) . ? C82 C83 1.194(6) . ? C84 C88 1.399(3) . ? C84 C85 1.399(3) . ? C85 C86 1.399(3) . ? C86 C87 1.399(3) . ? C87 C88 1.399(3) . ? O100 C103 1.441(7) . ? O100 C100 1.449(7) . ? C100 C101 1.36914(13) . ? C101 C102 1.37973(13) . ? C102 C103 1.3820 . ? O110 C110 1.453(17) . ? O110 C113 1.457(16) . ? C110 C111 1.373(17) . ? C111 C112 1.359(18) . ? C112 C113 1.368(16) . ? O120 C121 1.21861(10) 2_666 ? O120 C120 1.49292(10) . ? C120 C121 1.50384(11) . ? C121 O120 1.2186 2_666 ? O130 C131 1.24663(13) 2_677 ? O130 C130 1.49985(11) . ? O130 C130 1.80132(13) 2_677 ? C130 C131 1.49048(16) . ? C130 O130 1.80132(13) 2_677 ? C131 O130 1.24663(12) 2_677 ? 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 C38 Fe1 C37 40.76(9) . . ? C38 Fe1 C4 123.81(19) . . ? C37 Fe1 C4 105.25(18) . . ? C38 Fe1 C34 40.75(9) . . ? C37 Fe1 C34 68.37(14) . . ? C4 Fe1 C34 162.25(18) . . ? C38 Fe1 C5 106.87(17) . . ? C37 Fe1 C5 119.15(17) . . ? C4 Fe1 C5 41.45(16) . . ? C34 Fe1 C5 125.87(16) . . ? C38 Fe1 C2 158.10(19) . . ? C37 Fe1 C2 160.30(19) . . ? C4 Fe1 C2 68.37(18) . . ? C34 Fe1 C2 123.06(18) . . ? C5 Fe1 C2 69.22(17) . . ? C38 Fe1 C36 68.26(14) . . ? C37 Fe1 C36 40.48(9) . . ? C4 Fe1 C36 118.60(17) . . ? C34 Fe1 C36 68.04(14) . . ? C5 Fe1 C36 154.08(17) . . ? C2 Fe1 C36 124.78(18) . . ? C38 Fe1 C35 68.23(14) . . ? C37 Fe1 C35 68.05(14) . . ? C4 Fe1 C35 154.30(17) . . ? C34 Fe1 C35 40.44(9) . . ? C5 Fe1 C35 163.68(16) . . ? C2 Fe1 C35 109.15(17) . . ? C36 Fe1 C35 40.28(9) . . ? C38 Fe1 C1 122.05(17) . . ? C37 Fe1 C1 156.28(18) . . ? C4 Fe1 C1 69.19(17) . . ? C34 Fe1 C1 109.59(16) . . ? C5 Fe1 C1 41.49(16) . . ? C2 Fe1 C1 40.84(16) . . ? C36 Fe1 C1 162.58(17) . . ? C35 Fe1 C1 126.76(16) . . ? C38 Fe1 C3 160.18(19) . . ? C37 Fe1 C3 123.00(19) . . ? C4 Fe1 C3 40.40(17) . . ? C34 Fe1 C3 156.92(18) . . ? C5 Fe1 C3 68.96(17) . . ? C2 Fe1 C3 40.32(17) . . ? C36 Fe1 C3 106.55(18) . . ? C35 Fe1 C3 121.00(18) . . ? C1 Fe1 C3 68.48(17) . . ? C33 C1 C2 123.6(4) . . ? C33 C1 C5 129.2(4) . . ? C2 C1 C5 107.1(3) . . ? C33 C1 Fe1 128.7(3) . . ? C2 C1 Fe1 69.0(2) . . ? C5 C1 Fe1 68.6(2) . . ? C3 C2 C1 109.1(4) . . ? C3 C2 Fe1 70.5(3) . . ? C1 C2 Fe1 70.2(2) . . ? C2 C3 C4 108.3(4) . . ? C2 C3 Fe1 69.2(3) . . ? C4 C3 Fe1 68.9(2) . . ? C3 C4 C5 108.7(4) . . ? C3 C4 Fe1 70.7(2) . . ? C5 C4 Fe1 69.5(2) . . ? C6 C5 C4 123.8(4) . . ? C6 C5 C1 129.4(4) . . ? C4 C5 C1 106.8(3) . . ? C6 C5 Fe1 125.6(3) . . ? C4 C5 Fe1 69.1(2) . . ? C1 C5 Fe1 69.9(2) . . ? C7 C6 C5 174.4(4) . . ? C6 C7 C8 177.1(5) . . ? C13 C8 C9 117.5(4) . . ? C13 C8 C7 121.7(4) . . ? C9 C8 C7 120.8(4) . . ? C10 C9 C8 121.5(4) . . ? C9 C10 C11 121.5(4) . . ? C12 C11 C10 117.2(4) . . ? C12 C11 C14 121.2(4) . . ? C10 C11 C14 121.7(4) . . ? C11 C12 C13 122.2(4) . . ? C12 C13 C8 120.1(4) . . ? C12 C13 C18 122.3(4) . . ? C8 C13 C18 117.6(4) . . ? C17 C14 C16 110.3(7) . . ? C17 C14 C15 107.7(7) . . ? C16 C14 C15 105.9(6) . . ? C17 C14 C11 110.4(5) . . ? C16 C14 C11 112.8(5) . . ? C15 C14 C11 109.6(4) . . ? C19 C18 C13 171.0(5) . . ? C18 C19 C20 173.8(5) . . ? C21 C20 C19 171.1(5) . . ? C20 C21 C22 170.9(5) . . ? C23 C22 C27 120.0(4) . . ? C23 C22 C21 122.4(4) . . ? C27 C22 C21 117.6(4) . . ? C24 C23 C22 121.5(4) . . ? C25 C24 C23 117.5(4) . . ? C25 C24 C28 122.0(4) . . ? C23 C24 C28 120.4(4) . . ? C26 C25 C24 122.4(4) . . ? C25 C26 C27 120.7(4) . . ? C26 C27 C22 117.8(4) . . ? C26 C27 C32 120.5(4) . . ? C22 C27 C32 121.7(4) . . ? C31A C28 C30B 56.3 . . ? C31A C28 C30A 109.5 . . ? C30B C28 C30A 141.1 . . ? C31A C28 C29A 109.5 . . ? C30B C28 C29A 56.3 . . ? C30A C28 C29A 109.5 . . ? C31A C28 C29B 56.2 . . ? C30B C28 C29B 109.5 . . ? C30A C28 C29B 56.2 . . ? C29A C28 C29B 141.1 . . ? C31A C28 C31B 141.1 . . ? C30B C28 C31B 109.5 . . ? C30A C28 C31B 56.2 . . ? C29A C28 C31B 56.3 . . ? C29B C28 C31B 109.5 . . ? C31A C28 C24 110.2(3) . . ? C30B C28 C24 110.0(3) . . ? C30A C28 C24 108.9(3) . . ? C29A C28 C24 109.3(2) . . ? C29B C28 C24 109.7(2) . . ? C31B C28 C24 108.7(3) . . ? C33 C32 C27 177.9(5) . . ? C32 C33 C1 173.3(5) . . ? C35 C34 C38 108.0 . . ? C35 C34 Fe1 70.43(14) . . ? C38 C34 Fe1 69.17(14) . . ? C34 C35 C36 108.0 . . ? C34 C35 Fe1 69.13(14) . . ? C36 C35 Fe1 69.81(14) . . ? C35 C36 C37 108.0 . . ? C35 C36 Fe1 69.91(14) . . ? C37 C36 Fe1 69.08(14) . . ? C38 C37 C36 108.0 . . ? C38 C37 Fe1 69.24(14) . . ? C36 C37 Fe1 70.44(14) . . ? C37 C38 C34 108.0 . . ? C37 C38 Fe1 69.99(14) . . ? C34 C38 Fe1 70.08(14) . . ? C84 Fe2 C85 40.47(9) . . ? C84 Fe2 C88 40.44(9) . . ? C85 Fe2 C88 67.87(14) . . ? C84 Fe2 C86 67.77(14) . . ? C85 Fe2 C86 40.23(9) . . ? C88 Fe2 C86 67.58(14) . . ? C84 Fe2 C53 163.4(2) . . ? C85 Fe2 C53 125.7(2) . . ? C88 Fe2 C53 154.2(2) . . ? C86 Fe2 C53 107.38(17) . . ? C84 Fe2 C54 154.7(2) . . ? C85 Fe2 C54 163.0(2) . . ? C88 Fe2 C54 119.8(2) . . ? C86 Fe2 C54 125.73(19) . . ? C53 Fe2 C54 41.08(18) . . ? C84 Fe2 C87 67.74(14) . . ? C85 Fe2 C87 67.60(13) . . ? C88 Fe2 C87 40.19(9) . . ? C86 Fe2 C87 40.07(9) . . ? C53 Fe2 C87 119.58(19) . . ? C54 Fe2 C87 107.61(18) . . ? C84 Fe2 C52 127.3(2) . . ? C85 Fe2 C52 108.05(19) . . ? C88 Fe2 C52 165.2(2) . . ? C86 Fe2 C52 119.21(19) . . ? C53 Fe2 C52 39.75(17) . . ? C54 Fe2 C52 68.34(19) . . ? C87 Fe2 C52 153.0(2) . . ? C84 Fe2 C55 120.39(18) . . ? C85 Fe2 C55 154.99(19) . . ? C88 Fe2 C55 108.28(17) . . ? C86 Fe2 C55 163.3(2) . . ? C53 Fe2 C55 68.86(17) . . ? C54 Fe2 C55 40.91(16) . . ? C87 Fe2 C55 126.45(19) . . ? C52 Fe2 C55 69.01(18) . . ? C84 Fe2 C51 108.65(17) . . ? C85 Fe2 C51 120.08(19) . . ? C88 Fe2 C51 127.51(19) . . ? C86 Fe2 C51 154.0(2) . . ? C53 Fe2 C51 68.26(17) . . ? C54 Fe2 C51 68.88(18) . . ? C87 Fe2 C51 164.7(2) . . ? C52 Fe2 C51 41.00(16) . . ? C55 Fe2 C51 41.29(17) . . ? C52 C51 C83 123.4(4) . . ? C52 C51 C55 107.3(4) . . ? C83 C51 C55 129.3(4) . . ? C52 C51 Fe2 69.3(2) . . ? C83 C51 Fe2 127.0(3) . . ? C55 C51 Fe2 69.2(2) . . ? C53 C52 C51 108.8(4) . . ? C53 C52 Fe2 70.0(3) . . ? C51 C52 Fe2 69.7(2) . . ? C52 C53 C54 108.9(4) . . ? C52 C53 Fe2 70.2(3) . . ? C54 C53 Fe2 69.5(2) . . ? C55 C54 C53 107.7(4) . . ? C55 C54 Fe2 69.6(2) . . ? C53 C54 Fe2 69.4(3) . . ? C56 C55 C54 123.2(4) . . ? C56 C55 C51 129.4(4) . . ? C54 C55 C51 107.4(4) . . ? C56 C55 Fe2 126.2(3) . . ? C54 C55 Fe2 69.5(2) . . ? C51 C55 Fe2 69.5(2) . . ? C57 C56 C55 172.6(5) . . ? C56 C57 C58 177.7(5) . . ? C59 C58 C63 118.5(4) . . ? C59 C58 C57 121.2(4) . . ? C63 C58 C57 120.3(4) . . ? C58 C59 C60 120.3(4) . . ? C59 C60 C61 122.3(4) . . ? C62 C61 C60 116.5(4) . . ? C62 C61 C64 123.9(4) . . ? C60 C61 C64 119.5(4) . . ? C61 C62 C63 122.8(4) . . ? C62 C63 C58 119.6(4) . . ? C62 C63 C68 122.2(4) . . ? C58 C63 C68 118.3(4) . . ? C65 C64 C66 108.3(5) . . ? C65 C64 C67 110.2(5) . . ? C66 C64 C67 108.7(5) . . ? C65 C64 C61 109.3(4) . . ? C66 C64 C61 111.2(4) . . ? C67 C64 C61 109.3(4) . . ? C69 C68 C63 169.5(5) . . ? C68 C69 C70 171.8(5) . . ? C71 C70 C69 172.8(5) . . ? C70 C71 C72 173.3(5) . . ? C73 C72 C71 121.7(4) . . ? C73 C72 C77 120.1(4) . . ? C71 C72 C77 118.3(4) . . ? C72 C73 C74 123.4(4) . . ? C73 C74 C75 115.6(4) . . ? C73 C74 C78 120.5(4) . . ? C75 C74 C78 123.8(4) . . ? C76 C75 C74 121.8(4) . . ? C75 C76 C77 122.4(4) . . ? C76 C77 C72 116.7(4) . . ? C76 C77 C82 122.3(4) . . ? C72 C77 C82 121.0(4) . . ? C80 C78 C79 109.8(6) . . ? C80 C78 C74 112.7(4) . . ? C79 C78 C74 110.7(5) . . ? C80 C78 C81 108.9(6) . . ? C79 C78 C81 105.6(6) . . ? C74 C78 C81 108.9(5) . . ? C83 C82 C77 177.3(5) . . ? C82 C83 C51 173.7(5) . . ? C88 C84 C85 108.0 . . ? C88 C84 Fe2 70.17(15) . . ? C85 C84 Fe2 70.06(15) . . ? C86 C85 C84 108.0 . . ? C86 C85 Fe2 70.46(15) . . ? C84 C85 Fe2 69.46(15) . . ? C85 C86 C87 108.0 . . ? C85 C86 Fe2 69.31(15) . . ? C87 C86 Fe2 70.03(15) . . ? C88 C87 C86 108.0 . . ? C88 C87 Fe2 69.36(15) . . ? C86 C87 Fe2 69.90(15) . . ? C87 C88 C84 108.0 . . ? C87 C88 Fe2 70.45(15) . . ? C84 C88 Fe2 69.38(15) . . ? C103 O100 C100 101.3(5) . . ? C101 C100 O100 94.0(7) . . ? C100 C101 C102 108.914(4) . . ? C101 C102 C103 107.308(5) . . ? C102 C103 O100 93.5(7) . . ? C110 O110 C113 89.9(19) . . ? C111 C110 O110 87.5(18) . . ? C112 C111 C110 106.2(17) . . ? C111 C112 C113 102.7(15) . . ? C112 C113 O110 93.5(17) . . ? C121 O120 C120 138.454(3) 2_666 . ? O120 C120 C121 128.813(5) . . ? O120 C121 C120 92.077(4) 2_666 . ? C131 O130 C130 138.204(5) 2_677 . ? C131 O130 C130 54.980(4) 2_677 2_677 ? C130 O130 C130 93.558(7) . 2_677 ? C131 C130 O130 123.268(2) . . ? C131 C130 O130 43.233(5) . 2_677 ? O130 C130 O130 86.442(7) . 2_677 ? O130 C131 C130 81.787(4) 2_677 . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.993 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.083 data_fmthlt1s _database_code_CSD 157835 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.50 H27 Cl3 Fe O4' _chemical_formula_weight 679.77 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' '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 11.7194(8) _cell_length_b 16.5664(11) _cell_length_c 17.0129(12) _cell_angle_alpha 79.1350(10) _cell_angle_beta 79.5180(10) _cell_angle_gamma 74.5570(10) _cell_volume 3096.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 211(2) _cell_measurement_reflns_used 9589 _cell_measurement_theta_min 2.335 _cell_measurement_theta_max 25.047 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 0.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8343 _exptl_absorpt_correction_T_max 0.9422 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 211(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 21689 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.05 _reflns_number_total 10912 _reflns_number_gt 7881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.619 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _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^)+(0.1184P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10912 _refine_ls_number_parameters 792 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1917 _refine_ls_wR_factor_gt 0.1785 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.59821(5) 0.73680(3) 0.09633(4) 0.01999(18) Uani 1 1 d . . . C1 C 0.5584(3) 0.8652(2) 0.0581(3) 0.0204(9) Uani 1 1 d . . . C2 C 0.4673(4) 0.8293(2) 0.0445(3) 0.0222(9) Uani 1 1 d . . . H2 H 0.4435 0.8317 -0.0060 0.027 Uiso 1 1 calc R . . C3 C 0.4182(4) 0.7893(2) 0.1198(3) 0.0239(10) Uani 1 1 d . . . H3 H 0.3564 0.7610 0.1277 0.029 Uiso 1 1 calc R . . C4 C 0.4780(4) 0.7994(2) 0.1803(3) 0.0242(10) Uani 1 1 d . . . H4 H 0.4632 0.7784 0.2355 0.029 Uiso 1 1 calc R . . C5 C 0.5657(4) 0.8470(2) 0.1440(3) 0.0211(9) Uani 1 1 d . . . C6 C 0.6383(4) 0.8727(2) 0.1885(3) 0.0230(9) Uani 1 1 d . . . C7 C 0.6910(4) 0.8957(3) 0.2317(3) 0.0246(10) Uani 1 1 d . . . C8 C 0.7489(4) 0.9244(3) 0.2844(3) 0.0232(9) Uani 1 1 d . . . C9 C 0.8210(4) 0.9826(3) 0.2548(3) 0.0243(9) Uani 1 1 d . . . C10 C 0.8681(4) 1.0142(3) 0.3092(3) 0.0302(11) Uani 1 1 d . . . H10 H 0.9143 1.0540 0.2893 0.036 Uiso 1 1 calc R . . C11 C 0.8485(4) 0.9883(3) 0.3911(3) 0.0322(11) Uani 1 1 d . . . C12 C 0.7826(4) 0.9261(3) 0.4206(3) 0.0319(11) Uani 1 1 d . . . C13 C 0.7329(4) 0.8964(3) 0.3679(3) 0.0271(10) Uani 1 1 d . . . H13 H 0.6870 0.8564 0.3883 0.033 Uiso 1 1 calc R . . C14 C 0.7103(5) 0.8365(3) 0.5333(3) 0.0429(13) Uani 1 1 d . . . H14A H 0.6263 0.8608 0.5289 0.064 Uiso 1 1 calc R . . H14B H 0.7200 0.8165 0.5896 0.064 Uiso 1 1 calc R . . H14C H 0.7398 0.7896 0.5026 0.064 Uiso 1 1 calc R . . C15 C 0.9591(6) 1.0793(4) 0.4170(4) 0.0566(17) Uani 1 1 d . . . H15A H 1.0313 1.0541 0.3836 0.085 Uiso 1 1 calc R . . H15B H 0.9801 1.0979 0.4621 0.085 Uiso 1 1 calc R . . H15C H 0.9128 1.1275 0.3850 0.085 Uiso 1 1 calc R . . C16 C 0.8410(4) 1.0090(3) 0.1703(3) 0.0238(10) Uani 1 1 d . . . C17 C 0.8487(4) 1.0258(2) 0.0979(3) 0.0223(9) Uani 1 1 d . . . C18 C 0.8449(4) 1.0395(2) 0.0171(3) 0.0237(10) Uani 1 1 d . . . C19 C 0.8331(4) 1.0452(2) -0.0529(3) 0.0232(10) Uani 1 1 d . . . C20 C 0.8026(4) 1.0450(2) -0.1301(3) 0.0220(9) Uani 1 1 d . . . C21 C 0.8494(4) 1.0908(2) -0.2005(3) 0.0226(9) Uani 1 1 d . . . H21 H 0.9053 1.1213 -0.1978 0.027 Uiso 1 1 calc R . . C22 C 0.8151(4) 1.0917(3) -0.2734(3) 0.0263(10) Uani 1 1 d . . . C23 C 0.7317(4) 1.0454(3) -0.2783(3) 0.0252(10) Uani 1 1 d . . . C24 C 0.6858(4) 0.9991(3) -0.2094(3) 0.0244(10) Uani 1 1 d . . . H24 H 0.6315 0.9677 -0.2130 0.029 Uiso 1 1 calc R . . C25 C 0.7190(4) 0.9984(2) -0.1341(3) 0.0228(9) Uani 1 1 d . . . C26 C 0.6120(4) 1.0094(3) -0.3581(3) 0.0364(12) Uani 1 1 d . . . H26A H 0.6355 0.9500 -0.3356 0.055 Uiso 1 1 calc R . . H26B H 0.6016 1.0143 -0.4142 0.055 Uiso 1 1 calc R . . H26C H 0.5373 1.0359 -0.3278 0.055 Uiso 1 1 calc R . . C27 C 0.9214(5) 1.1954(3) -0.3400(3) 0.0376(12) Uani 1 1 d . . . H27A H 0.8732 1.2370 -0.3065 0.056 Uiso 1 1 calc R . . H27B H 0.9432 1.2238 -0.3938 0.056 Uiso 1 1 calc R . . H27C H 0.9932 1.1655 -0.3164 0.056 Uiso 1 1 calc R . . C28 C 0.6679(4) 0.9517(2) -0.0631(3) 0.0222(9) Uani 1 1 d . . . C29 C 0.6239(4) 0.9120(2) -0.0047(3) 0.0210(9) Uani 1 1 d . . . C30 C 0.7606(4) 0.6822(3) 0.0373(3) 0.0243(9) Uani 1 1 d . . . H30 H 0.8107 0.7111 -0.0004 0.029 Uiso 1 1 calc R . . C31 C 0.6693(4) 0.6494(3) 0.0196(3) 0.0298(11) Uani 1 1 d . . . H31 H 0.6491 0.6523 -0.0320 0.036 Uiso 1 1 calc R . . C32 C 0.6144(4) 0.6117(2) 0.0930(3) 0.0320(12) Uani 1 1 d . . . H32 H 0.5507 0.5855 0.0991 0.038 Uiso 1 1 calc R . . C33 C 0.6725(4) 0.6205(3) 0.1560(3) 0.0317(11) Uani 1 1 d . . . H33 H 0.6541 0.6009 0.2113 0.038 Uiso 1 1 calc R . . C34 C 0.7627(4) 0.6637(3) 0.1214(3) 0.0265(10) Uani 1 1 d . . . H34 H 0.8149 0.6777 0.1496 0.032 Uiso 1 1 calc R . . O1 O 0.7757(3) 0.8991(2) 0.50213(19) 0.0382(8) Uani 1 1 d . . . O2 O 0.8889(3) 1.0173(2) 0.4474(2) 0.0441(9) Uani 1 1 d . . . O3 O 0.7028(3) 1.0506(2) -0.35302(19) 0.0331(8) Uani 1 1 d . . . O4 O 0.8539(3) 1.13608(19) -0.34488(18) 0.0332(8) Uani 1 1 d . . . Fe2 Fe 0.56843(5) 0.24959(3) 0.17647(4) 0.02200(18) Uani 1 1 d . . . C40 C 0.6503(4) 0.3437(3) 0.1793(3) 0.0224(9) Uani 1 1 d . . . C41 C 0.7364(4) 0.2696(3) 0.1581(3) 0.0255(10) Uani 1 1 d . . . H41 H 0.7993 0.2385 0.1870 0.031 Uiso 1 1 calc R . . C42 C 0.7118(4) 0.2508(3) 0.0868(3) 0.0250(10) Uani 1 1 d . . . H42 H 0.7562 0.2056 0.0594 0.030 Uiso 1 1 calc R . . C43 C 0.6090(4) 0.3111(2) 0.0630(3) 0.0237(9) Uani 1 1 d . . . H43 H 0.5731 0.3126 0.0174 0.028 Uiso 1 1 calc R . . C44 C 0.5692(4) 0.3693(2) 0.1200(3) 0.0212(9) Uani 1 1 d . . . C45 C 0.4638(4) 0.4381(2) 0.1179(3) 0.0221(9) Uani 1 1 d . . . C46 C 0.3756(4) 0.4920(3) 0.1111(3) 0.0240(10) Uani 1 1 d . . . C47 C 0.2697(4) 0.5575(2) 0.0965(3) 0.0226(9) Uani 1 1 d . . . C48 C 0.2274(4) 0.6228(2) 0.1438(3) 0.0231(9) Uani 1 1 d . . . C49 C 0.1292(4) 0.6892(2) 0.1225(3) 0.0223(9) Uani 1 1 d . . . H49 H 0.1009 0.7339 0.1532 0.027 Uiso 1 1 calc R . . C50 C 0.0748(3) 0.6893(2) 0.0576(3) 0.0209(9) Uani 1 1 d . . . C51 C 0.1136(4) 0.6209(3) 0.0133(3) 0.0224(9) Uani 1 1 d . . . C52 C 0.2115(4) 0.5569(3) 0.0324(3) 0.0241(10) Uani 1 1 d . . . H52 H 0.2393 0.5123 0.0016 0.029 Uiso 1 1 calc R . . C53 C 0.0884(4) 0.5562(3) -0.0942(3) 0.0352(11) Uani 1 1 d . . . H53A H 0.1687 0.5544 -0.1223 0.053 Uiso 1 1 calc R . . H53B H 0.0340 0.5644 -0.1333 0.053 Uiso 1 1 calc R . . H53C H 0.0876 0.5033 -0.0585 0.053 Uiso 1 1 calc R . . C54 C -0.0633(4) 0.8214(3) 0.0750(3) 0.0277(10) Uani 1 1 d . . . H54A H -0.0891 0.8004 0.1308 0.042 Uiso 1 1 calc R . . H54B H -0.1307 0.8599 0.0516 0.042 Uiso 1 1 calc R . . H54C H -0.0013 0.8509 0.0728 0.042 Uiso 1 1 calc R . . C55 C 0.2855(4) 0.6199(2) 0.2110(3) 0.0237(10) Uani 1 1 d . . . C56 C 0.3451(4) 0.6077(3) 0.2650(3) 0.0247(10) Uani 1 1 d . . . C57 C 0.4251(4) 0.5861(3) 0.3191(3) 0.0262(10) Uani 1 1 d . . . C58 C 0.5038(4) 0.5589(3) 0.3617(3) 0.0279(10) Uani 1 1 d . . . C59 C 0.6062(4) 0.5179(3) 0.3998(3) 0.0254(10) Uani 1 1 d . . . C60 C 0.6331(4) 0.5445(3) 0.4665(3) 0.0276(10) Uani 1 1 d . . . H60 H 0.5796 0.5905 0.4887 0.033 Uiso 1 1 calc R . . C61 C 0.7350(4) 0.5054(3) 0.4997(3) 0.0272(10) Uani 1 1 d . . . C62 C 0.8164(4) 0.4367(3) 0.4667(3) 0.0301(10) Uani 1 1 d . . . C63 C 0.7907(4) 0.4090(3) 0.4024(3) 0.0306(11) Uani 1 1 d . . . H63 H 0.8448 0.3628 0.3809 0.037 Uiso 1 1 calc R . . C64 C 0.6858(4) 0.4479(3) 0.3678(3) 0.0274(10) Uani 1 1 d . . . C65 C 0.6872(4) 0.5950(3) 0.6020(3) 0.0380(12) Uani 1 1 d . . . H65A H 0.6755 0.6464 0.5631 0.057 Uiso 1 1 calc R . . H65B H 0.7201 0.6039 0.6471 0.057 Uiso 1 1 calc R . . H65C H 0.6112 0.5803 0.6214 0.057 Uiso 1 1 calc R . . C66 C 1.0095(4) 0.3415(3) 0.4632(3) 0.0404(12) Uani 1 1 d . . . H66A H 0.9821 0.2904 0.4668 0.061 Uiso 1 1 calc R . . H66B H 1.0803 0.3283 0.4896 0.061 Uiso 1 1 calc R . . H66C H 1.0285 0.3641 0.4069 0.061 Uiso 1 1 calc R . . C67 C 0.6634(4) 0.4155(3) 0.3012(3) 0.0275(10) Uani 1 1 d . . . C68 C 0.6513(4) 0.3841(3) 0.2464(3) 0.0258(10) Uani 1 1 d . . . C69 C 0.4736(4) 0.2274(3) 0.2874(3) 0.0360(12) Uani 1 1 d . . . H69 H 0.4687 0.2553 0.3316 0.043 Uiso 1 1 calc R . . C70 C 0.5604(4) 0.1523(3) 0.2691(3) 0.0341(11) Uani 1 1 d . . . H70 H 0.6226 0.1223 0.2990 0.041 Uiso 1 1 calc R . . C71 C 0.5363(4) 0.1311(3) 0.1980(3) 0.0320(11) Uani 1 1 d . . . H71 H 0.5796 0.0846 0.1721 0.038 Uiso 1 1 calc R . . C72 C 0.4342(4) 0.1933(3) 0.1728(3) 0.0324(11) Uani 1 1 d . . . H72 H 0.3982 0.1946 0.1274 0.039 Uiso 1 1 calc R . . C73 C 0.3962(4) 0.2527(3) 0.2279(3) 0.0310(11) Uani 1 1 d . . . H73 H 0.3312 0.3003 0.2253 0.037 Uiso 1 1 calc R . . O5 O 0.0517(3) 0.62444(18) -0.04812(19) 0.0287(7) Uani 1 1 d . . . O6 O -0.0171(2) 0.75165(17) 0.03034(18) 0.0260(7) Uani 1 1 d . . . O7 O 0.9168(3) 0.4033(2) 0.5023(2) 0.0378(8) Uani 1 1 d . . . O8 O 0.7684(3) 0.5275(2) 0.5641(2) 0.0344(8) Uani 1 1 d . . . C80 C 0.6419(6) 0.2329(5) 0.5385(4) 0.075(2) Uani 1 1 d . . . H80A H 0.6629 0.2856 0.5413 0.090 Uiso 1 1 calc R . . H80B H 0.7015 0.1858 0.5628 0.090 Uiso 1 1 calc R . . Cl1 Cl 0.6475(2) 0.22355(17) 0.43847(14) 0.1101(8) Uani 1 1 d . . . Cl2 Cl 0.50023(17) 0.23294(11) 0.59470(12) 0.0731(5) Uani 1 1 d . . . C81 C 1.0058(6) 0.5738(4) 0.3380(4) 0.0553(16) Uani 1 1 d . . . H81A H 1.0826 0.5886 0.3332 0.066 Uiso 1 1 calc R . . H81B H 0.9909 0.5420 0.3921 0.066 Uiso 1 1 calc R . . Cl3 Cl 0.89082(16) 0.66794(11) 0.32682(11) 0.0718(5) Uani 1 1 d . . . Cl4 Cl 1.01387(18) 0.50998(11) 0.26566(10) 0.0695(5) Uani 1 1 d . . . C82 C 0.9073(5) 0.7832(4) 0.8250(4) 0.0593(16) Uani 1 1 d . . . H82A H 0.8207 0.8067 0.8345 0.071 Uiso 1 1 calc R . . H82B H 0.9275 0.7364 0.8688 0.071 Uiso 1 1 calc R . . Cl5 Cl 0.9732(2) 0.85548(14) 0.8306(2) 0.1188(9) Uani 1 1 d . . . Cl6 Cl 0.9410(3) 0.7437(2) 0.73671(19) 0.1445(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0202(3) 0.0147(3) 0.0253(4) -0.0048(2) 0.0000(3) -0.0056(2) C1 0.018(2) 0.0134(19) 0.027(2) -0.0061(17) 0.0016(18) -0.0001(16) C2 0.020(2) 0.019(2) 0.028(2) -0.0078(18) -0.0001(19) -0.0046(17) C3 0.021(2) 0.017(2) 0.034(3) -0.0057(18) -0.001(2) -0.0042(17) C4 0.025(2) 0.017(2) 0.028(3) -0.0045(18) 0.004(2) -0.0044(17) C5 0.021(2) 0.0140(19) 0.026(2) -0.0071(17) 0.0013(19) -0.0003(16) C6 0.023(2) 0.018(2) 0.024(2) -0.0043(18) 0.0061(19) -0.0046(17) C7 0.025(2) 0.021(2) 0.026(2) -0.0061(19) 0.001(2) -0.0044(18) C8 0.019(2) 0.025(2) 0.024(2) -0.0087(18) 0.0005(19) -0.0012(17) C9 0.025(2) 0.021(2) 0.026(2) -0.0050(18) -0.003(2) -0.0038(18) C10 0.032(2) 0.028(2) 0.034(3) -0.003(2) -0.011(2) -0.010(2) C11 0.040(3) 0.031(3) 0.029(3) -0.007(2) -0.007(2) -0.010(2) C12 0.034(3) 0.031(2) 0.028(3) -0.005(2) -0.001(2) -0.006(2) C13 0.029(2) 0.025(2) 0.027(3) -0.0062(19) 0.000(2) -0.0064(19) C14 0.061(3) 0.039(3) 0.027(3) -0.002(2) 0.003(3) -0.016(3) C15 0.083(4) 0.054(4) 0.052(4) 0.001(3) -0.037(3) -0.037(3) C16 0.022(2) 0.019(2) 0.032(3) -0.0076(19) -0.003(2) -0.0056(17) C17 0.022(2) 0.016(2) 0.029(3) -0.0046(18) -0.003(2) -0.0040(17) C18 0.021(2) 0.016(2) 0.035(3) -0.0033(19) -0.002(2) -0.0057(17) C19 0.022(2) 0.014(2) 0.033(3) -0.0034(18) 0.000(2) -0.0052(17) C20 0.023(2) 0.016(2) 0.025(2) -0.0031(18) -0.0002(19) -0.0040(17) C21 0.023(2) 0.019(2) 0.025(2) -0.0018(18) -0.0017(19) -0.0062(17) C22 0.025(2) 0.021(2) 0.029(3) -0.0015(19) 0.003(2) -0.0051(18) C23 0.028(2) 0.025(2) 0.022(2) -0.0059(19) -0.002(2) -0.0037(18) C24 0.025(2) 0.019(2) 0.030(3) -0.0071(19) -0.002(2) -0.0043(18) C25 0.022(2) 0.016(2) 0.028(2) -0.0020(18) -0.0010(19) -0.0024(17) C26 0.040(3) 0.043(3) 0.031(3) -0.010(2) -0.005(2) -0.016(2) C27 0.050(3) 0.037(3) 0.028(3) 0.007(2) 0.000(2) -0.026(2) C28 0.020(2) 0.016(2) 0.031(3) -0.0064(19) -0.003(2) -0.0037(17) C29 0.020(2) 0.016(2) 0.027(2) -0.0060(18) -0.0048(19) -0.0022(17) C30 0.021(2) 0.021(2) 0.030(3) -0.0087(19) -0.0001(19) -0.0012(17) C31 0.025(2) 0.025(2) 0.041(3) -0.018(2) -0.005(2) 0.0020(19) C32 0.023(2) 0.011(2) 0.061(3) -0.010(2) 0.002(2) -0.0044(17) C33 0.034(3) 0.015(2) 0.038(3) 0.001(2) 0.002(2) 0.0011(19) C34 0.024(2) 0.021(2) 0.032(3) -0.0064(19) -0.006(2) 0.0013(18) O1 0.053(2) 0.046(2) 0.0205(18) -0.0031(15) -0.0031(16) -0.0219(17) O2 0.063(2) 0.048(2) 0.033(2) 0.0001(17) -0.0220(19) -0.0290(19) O3 0.0389(18) 0.0407(19) 0.0246(18) -0.0051(15) -0.0060(15) -0.0168(15) O4 0.0410(19) 0.0369(18) 0.0229(17) 0.0058(14) -0.0036(15) -0.0194(15) Fe2 0.0210(3) 0.0164(3) 0.0277(4) -0.0045(3) -0.0002(3) -0.0042(2) C40 0.023(2) 0.022(2) 0.023(2) -0.0009(18) -0.0044(19) -0.0070(17) C41 0.017(2) 0.025(2) 0.033(3) -0.0011(19) -0.0011(19) -0.0063(17) C42 0.018(2) 0.019(2) 0.034(3) -0.0060(19) 0.003(2) -0.0025(17) C43 0.025(2) 0.021(2) 0.027(2) -0.0076(18) -0.0002(19) -0.0078(18) C44 0.021(2) 0.019(2) 0.025(2) -0.0041(18) -0.0023(19) -0.0071(17) C45 0.023(2) 0.018(2) 0.027(3) -0.0055(18) -0.0033(19) -0.0082(19) C46 0.026(2) 0.020(2) 0.028(3) -0.0060(19) -0.003(2) -0.007(2) C47 0.022(2) 0.016(2) 0.030(3) -0.0042(18) -0.0027(19) -0.0049(17) C48 0.024(2) 0.020(2) 0.027(2) -0.0030(18) -0.0033(19) -0.0096(18) C49 0.019(2) 0.016(2) 0.029(3) -0.0049(18) 0.0016(19) -0.0022(17) C50 0.0137(19) 0.019(2) 0.030(3) -0.0049(18) -0.0021(18) -0.0043(16) C51 0.019(2) 0.024(2) 0.025(2) -0.0038(18) -0.0038(19) -0.0063(17) C52 0.026(2) 0.020(2) 0.027(2) -0.0085(18) -0.001(2) -0.0047(18) C53 0.040(3) 0.033(3) 0.036(3) -0.014(2) -0.015(2) -0.003(2) C54 0.022(2) 0.018(2) 0.043(3) -0.009(2) -0.007(2) 0.0004(17) C55 0.026(2) 0.015(2) 0.029(3) -0.0027(18) -0.002(2) -0.0039(17) C56 0.027(2) 0.018(2) 0.028(3) -0.0024(18) -0.003(2) -0.0052(18) C57 0.031(2) 0.023(2) 0.026(3) -0.0072(19) -0.002(2) -0.0075(19) C58 0.033(3) 0.029(2) 0.023(2) -0.007(2) 0.000(2) -0.011(2) C59 0.028(2) 0.027(2) 0.023(2) -0.0033(19) -0.003(2) -0.0101(19) C60 0.030(2) 0.028(2) 0.026(3) -0.0040(19) 0.000(2) -0.0105(19) C61 0.032(2) 0.033(2) 0.020(2) -0.0061(19) -0.004(2) -0.012(2) C62 0.028(2) 0.036(3) 0.027(3) -0.005(2) -0.007(2) -0.007(2) C63 0.031(2) 0.030(2) 0.029(3) -0.007(2) -0.001(2) -0.004(2) C64 0.030(2) 0.030(2) 0.024(2) -0.0007(19) -0.005(2) -0.012(2) C65 0.044(3) 0.040(3) 0.038(3) -0.016(2) -0.010(2) -0.014(2) C66 0.032(3) 0.048(3) 0.035(3) -0.008(2) -0.007(2) 0.003(2) C67 0.028(2) 0.029(2) 0.025(3) -0.002(2) -0.001(2) -0.0081(19) C68 0.026(2) 0.024(2) 0.028(3) -0.0014(19) -0.003(2) -0.0091(18) C69 0.041(3) 0.034(3) 0.031(3) -0.005(2) 0.009(2) -0.016(2) C70 0.034(3) 0.023(2) 0.040(3) 0.004(2) 0.000(2) -0.008(2) C71 0.035(3) 0.020(2) 0.042(3) -0.006(2) 0.003(2) -0.012(2) C72 0.027(2) 0.030(2) 0.041(3) -0.007(2) 0.003(2) -0.013(2) C73 0.019(2) 0.030(2) 0.042(3) -0.004(2) 0.005(2) -0.0088(19) O5 0.0301(16) 0.0234(16) 0.0347(19) -0.0110(14) -0.0110(15) -0.0011(13) O6 0.0246(16) 0.0187(15) 0.0349(19) -0.0069(13) -0.0094(14) 0.0002(12) O7 0.0309(18) 0.048(2) 0.034(2) -0.0132(16) -0.0117(16) 0.0010(15) O8 0.0335(18) 0.0391(19) 0.0344(19) -0.0143(15) -0.0120(16) -0.0039(15) C80 0.076(5) 0.081(5) 0.074(5) 0.019(4) -0.033(4) -0.036(4) Cl1 0.1212(19) 0.144(2) 0.0680(14) -0.0078(14) -0.0257(14) -0.0347(17) Cl2 0.0835(12) 0.0573(10) 0.0829(13) 0.0048(9) -0.0212(10) -0.0284(9) C81 0.068(4) 0.065(4) 0.044(4) -0.014(3) -0.014(3) -0.027(3) Cl3 0.0720(11) 0.0719(11) 0.0698(12) -0.0081(9) -0.0214(10) -0.0081(9) Cl4 0.1078(14) 0.0680(10) 0.0474(9) -0.0125(8) -0.0058(9) -0.0469(10) C82 0.048(3) 0.054(4) 0.072(5) -0.015(3) -0.009(3) -0.003(3) Cl5 0.0718(13) 0.0748(14) 0.195(3) -0.0024(16) -0.0088(16) -0.0117(11) Cl6 0.152(3) 0.165(3) 0.128(2) -0.040(2) 0.009(2) -0.065(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C4 2.037(4) . ? Fe1 C32 2.041(4) . ? Fe1 C31 2.042(4) . ? Fe1 C30 2.044(4) . ? Fe1 C33 2.048(4) . ? Fe1 C5 2.052(4) . ? Fe1 C3 2.052(4) . ? Fe1 C2 2.053(4) . ? Fe1 C34 2.055(4) . ? Fe1 C1 2.056(4) . ? C1 C2 1.424(5) . ? C1 C29 1.427(6) . ? C1 C5 1.448(6) . ? C2 C3 1.424(6) . ? C3 C4 1.402(6) . ? C4 C5 1.442(6) . ? C5 C6 1.424(6) . ? C6 C7 1.210(6) . ? C7 C8 1.428(6) . ? C8 C13 1.403(6) . ? C8 C9 1.412(6) . ? C9 C10 1.400(6) . ? C9 C16 1.417(6) . ? C10 C11 1.374(6) . ? C11 O2 1.353(5) . ? C11 C12 1.414(6) . ? C12 O1 1.369(6) . ? C12 C13 1.378(6) . ? C14 O1 1.418(6) . ? C15 O2 1.447(6) . ? C16 C17 1.202(6) . ? C17 C18 1.357(6) . ? C18 C19 1.207(6) . ? C19 C20 1.425(6) . ? C20 C21 1.396(6) . ? C20 C25 1.417(5) . ? C21 C22 1.368(6) . ? C22 O4 1.366(5) . ? C22 C23 1.416(6) . ? C23 O3 1.355(5) . ? C23 C24 1.378(6) . ? C24 C25 1.402(6) . ? C25 C28 1.430(6) . ? C26 O3 1.432(5) . ? C27 O4 1.438(5) . ? C28 C29 1.198(6) . ? C30 C34 1.409(6) . ? C30 C31 1.421(6) . ? C31 C32 1.412(7) . ? C32 C33 1.418(7) . ? C33 C34 1.413(6) . ? Fe2 C69 2.031(5) . ? Fe2 C44 2.036(4) . ? Fe2 C70 2.040(5) . ? Fe2 C73 2.040(4) . ? Fe2 C41 2.042(4) . ? Fe2 C43 2.043(4) . ? Fe2 C72 2.046(4) . ? Fe2 C40 2.048(4) . ? Fe2 C71 2.050(4) . ? Fe2 C42 2.055(4) . ? C40 C41 1.425(6) . ? C40 C68 1.432(6) . ? C40 C44 1.440(6) . ? C41 C42 1.403(6) . ? C42 C43 1.413(6) . ? C43 C44 1.427(5) . ? C44 C45 1.441(6) . ? C45 C46 1.179(6) . ? C46 C47 1.440(6) . ? C47 C52 1.390(6) . ? C47 C48 1.399(6) . ? C48 C49 1.412(6) . ? C48 C55 1.422(6) . ? C49 C50 1.372(6) . ? C50 O6 1.360(5) . ? C50 C51 1.408(5) . ? C51 O5 1.361(5) . ? C51 C52 1.380(6) . ? C53 O5 1.425(5) . ? C54 O6 1.432(5) . ? C55 C56 1.208(6) . ? C56 C57 1.365(6) . ? C57 C58 1.217(6) . ? C58 C59 1.416(6) . ? C59 C60 1.404(6) . ? C59 C64 1.410(6) . ? C60 C61 1.364(6) . ? C61 O8 1.368(5) . ? C61 C62 1.410(6) . ? C62 O7 1.358(5) . ? C62 C63 1.371(6) . ? C63 C64 1.405(6) . ? C64 C67 1.432(6) . ? C65 O8 1.432(5) . ? C66 O7 1.439(5) . ? C67 C68 1.197(6) . ? C69 C73 1.413(7) . ? C69 C70 1.427(7) . ? C70 C71 1.416(7) . ? C71 C72 1.429(7) . ? C72 C73 1.415(6) . ? C80 Cl1 1.726(7) . ? C80 Cl2 1.759(7) . ? C81 Cl4 1.742(5) . ? C81 Cl3 1.774(6) . ? C82 Cl5 1.612(6) . ? C82 Cl6 1.692(7) . ? 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 C4 Fe1 C32 121.48(18) . . ? C4 Fe1 C31 158.15(17) . . ? C32 Fe1 C31 40.46(19) . . ? C4 Fe1 C30 158.61(17) . . ? C32 Fe1 C30 68.28(17) . . ? C31 Fe1 C30 40.70(16) . . ? C4 Fe1 C33 106.21(18) . . ? C32 Fe1 C33 40.58(19) . . ? C31 Fe1 C33 67.9(2) . . ? C30 Fe1 C33 67.86(18) . . ? C4 Fe1 C5 41.31(15) . . ? C32 Fe1 C5 158.77(19) . . ? C31 Fe1 C5 159.48(18) . . ? C30 Fe1 C5 123.35(16) . . ? C33 Fe1 C5 123.11(18) . . ? C4 Fe1 C3 40.09(17) . . ? C32 Fe1 C3 105.90(16) . . ? C31 Fe1 C3 123.20(17) . . ? C30 Fe1 C3 160.82(18) . . ? C33 Fe1 C3 120.41(18) . . ? C5 Fe1 C3 68.65(16) . . ? C4 Fe1 C2 68.09(18) . . ? C32 Fe1 C2 121.36(18) . . ? C31 Fe1 C2 108.36(18) . . ? C30 Fe1 C2 125.55(18) . . ? C33 Fe1 C2 156.42(17) . . ? C5 Fe1 C2 68.67(16) . . ? C3 Fe1 C2 40.60(17) . . ? C4 Fe1 C34 122.11(18) . . ? C32 Fe1 C34 68.08(17) . . ? C31 Fe1 C34 67.92(18) . . ? C30 Fe1 C34 40.21(17) . . ? C33 Fe1 C34 40.28(17) . . ? C5 Fe1 C34 108.25(17) . . ? C3 Fe1 C34 156.41(18) . . ? C2 Fe1 C34 162.00(17) . . ? C4 Fe1 C1 69.03(16) . . ? C32 Fe1 C1 157.70(19) . . ? C31 Fe1 C1 123.26(18) . . ? C30 Fe1 C1 109.48(16) . . ? C33 Fe1 C1 160.97(18) . . ? C5 Fe1 C1 41.29(16) . . ? C3 Fe1 C1 68.56(16) . . ? C2 Fe1 C1 40.55(15) . . ? C34 Fe1 C1 125.52(16) . . ? C2 C1 C29 123.2(4) . . ? C2 C1 C5 107.4(4) . . ? C29 C1 C5 129.4(4) . . ? C2 C1 Fe1 69.6(2) . . ? C29 C1 Fe1 127.8(3) . . ? C5 C1 Fe1 69.2(2) . . ? C1 C2 C3 108.7(4) . . ? C1 C2 Fe1 69.8(2) . . ? C3 C2 Fe1 69.7(2) . . ? C4 C3 C2 108.2(4) . . ? C4 C3 Fe1 69.3(2) . . ? C2 C3 Fe1 69.7(2) . . ? C3 C4 C5 108.9(4) . . ? C3 C4 Fe1 70.6(2) . . ? C5 C4 Fe1 69.9(2) . . ? C6 C5 C4 124.0(4) . . ? C6 C5 C1 129.3(4) . . ? C4 C5 C1 106.7(4) . . ? C6 C5 Fe1 129.0(3) . . ? C4 C5 Fe1 68.8(2) . . ? C1 C5 Fe1 69.5(2) . . ? C7 C6 C5 174.0(4) . . ? C6 C7 C8 177.8(4) . . ? C13 C8 C9 118.2(4) . . ? C13 C8 C7 120.2(4) . . ? C9 C8 C7 121.5(4) . . ? C10 C9 C8 119.5(4) . . ? C10 C9 C16 121.9(4) . . ? C8 C9 C16 118.6(4) . . ? C11 C10 C9 121.7(4) . . ? O2 C11 C10 125.0(4) . . ? O2 C11 C12 116.1(4) . . ? C10 C11 C12 119.0(4) . . ? O1 C12 C13 125.1(4) . . ? O1 C12 C11 115.0(4) . . ? C13 C12 C11 119.8(4) . . ? C12 C13 C8 121.6(4) . . ? C17 C16 C9 172.2(4) . . ? C16 C17 C18 172.1(4) . . ? C19 C18 C17 172.5(4) . . ? C18 C19 C20 170.1(4) . . ? C21 C20 C25 119.8(4) . . ? C21 C20 C19 122.3(4) . . ? C25 C20 C19 117.9(4) . . ? C22 C21 C20 120.8(4) . . ? O4 C22 C21 125.0(4) . . ? O4 C22 C23 115.0(4) . . ? C21 C22 C23 120.0(4) . . ? O3 C23 C24 124.7(4) . . ? O3 C23 C22 115.6(4) . . ? C24 C23 C22 119.7(4) . . ? C23 C24 C25 121.0(4) . . ? C24 C25 C20 118.7(4) . . ? C24 C25 C28 120.0(4) . . ? C20 C25 C28 121.3(4) . . ? C29 C28 C25 178.6(4) . . ? C28 C29 C1 171.8(4) . . ? C34 C30 C31 107.9(4) . . ? C34 C30 Fe1 70.3(2) . . ? C31 C30 Fe1 69.6(2) . . ? C32 C31 C30 108.1(4) . . ? C32 C31 Fe1 69.7(2) . . ? C30 C31 Fe1 69.7(2) . . ? C31 C32 C33 107.7(4) . . ? C31 C32 Fe1 69.8(2) . . ? C33 C32 Fe1 70.0(2) . . ? C34 C33 C32 108.2(4) . . ? C34 C33 Fe1 70.2(2) . . ? C32 C33 Fe1 69.4(2) . . ? C30 C34 C33 108.1(4) . . ? C30 C34 Fe1 69.5(2) . . ? C33 C34 Fe1 69.6(3) . . ? C12 O1 C14 116.2(4) . . ? C11 O2 C15 116.0(4) . . ? C23 O3 C26 116.3(4) . . ? C22 O4 C27 116.4(3) . . ? C69 Fe2 C44 121.68(18) . . ? C69 Fe2 C70 41.04(19) . . ? C44 Fe2 C70 158.57(18) . . ? C69 Fe2 C73 40.6(2) . . ? C44 Fe2 C73 106.09(17) . . ? C70 Fe2 C73 68.77(19) . . ? C69 Fe2 C41 123.9(2) . . ? C44 Fe2 C41 68.94(17) . . ? C70 Fe2 C41 108.23(19) . . ? C73 Fe2 C41 159.58(18) . . ? C69 Fe2 C43 157.90(19) . . ? C44 Fe2 C43 40.95(16) . . ? C70 Fe2 C43 159.42(17) . . ? C73 Fe2 C43 121.91(19) . . ? C41 Fe2 C43 68.11(18) . . ? C69 Fe2 C72 68.1(2) . . ? C44 Fe2 C72 122.14(18) . . ? C70 Fe2 C72 68.3(2) . . ? C73 Fe2 C72 40.52(18) . . ? C41 Fe2 C72 158.85(18) . . ? C43 Fe2 C72 107.39(19) . . ? C69 Fe2 C40 107.26(18) . . ? C44 Fe2 C40 41.30(16) . . ? C70 Fe2 C40 122.67(19) . . ? C73 Fe2 C40 122.56(17) . . ? C41 Fe2 C40 40.79(16) . . ? C43 Fe2 C40 68.71(16) . . ? C72 Fe2 C40 158.85(18) . . ? C69 Fe2 C71 68.54(19) . . ? C44 Fe2 C71 158.90(19) . . ? C70 Fe2 C71 40.50(19) . . ? C73 Fe2 C71 68.75(18) . . ? C41 Fe2 C71 122.95(18) . . ? C43 Fe2 C71 123.14(18) . . ? C72 Fe2 C71 40.84(19) . . ? C40 Fe2 C71 158.67(19) . . ? C69 Fe2 C42 160.2(2) . . ? C44 Fe2 C42 68.43(16) . . ? C70 Fe2 C42 123.93(18) . . ? C73 Fe2 C42 158.30(19) . . ? C41 Fe2 C42 40.04(17) . . ? C43 Fe2 C42 40.34(17) . . ? C72 Fe2 C42 123.28(18) . . ? C40 Fe2 C42 68.05(16) . . ? C71 Fe2 C42 108.39(17) . . ? C41 C40 C68 124.2(4) . . ? C41 C40 C44 107.3(4) . . ? C68 C40 C44 128.5(4) . . ? C41 C40 Fe2 69.4(2) . . ? C68 C40 Fe2 128.5(3) . . ? C44 C40 Fe2 68.9(2) . . ? C42 C41 C40 108.6(4) . . ? C42 C41 Fe2 70.5(2) . . ? C40 C41 Fe2 69.8(2) . . ? C41 C42 C43 108.7(4) . . ? C41 C42 Fe2 69.5(2) . . ? C43 C42 Fe2 69.4(2) . . ? C42 C43 C44 108.2(4) . . ? C42 C43 Fe2 70.3(3) . . ? C44 C43 Fe2 69.3(2) . . ? C43 C44 C40 107.3(4) . . ? C43 C44 C45 124.6(4) . . ? C40 C44 C45 128.1(4) . . ? C43 C44 Fe2 69.8(2) . . ? C40 C44 Fe2 69.8(2) . . ? C45 C44 Fe2 123.7(3) . . ? C46 C45 C44 174.7(4) . . ? C45 C46 C47 175.8(5) . . ? C52 C47 C48 119.9(4) . . ? C52 C47 C46 118.9(4) . . ? C48 C47 C46 121.2(4) . . ? C47 C48 C49 118.8(4) . . ? C47 C48 C55 118.7(4) . . ? C49 C48 C55 122.5(4) . . ? C50 C49 C48 120.8(4) . . ? O6 C50 C49 125.4(4) . . ? O6 C50 C51 114.7(4) . . ? C49 C50 C51 119.9(4) . . ? O5 C51 C52 124.4(4) . . ? O5 C51 C50 116.2(4) . . ? C52 C51 C50 119.4(4) . . ? C51 C52 C47 121.0(4) . . ? C56 C55 C48 171.3(4) . . ? C55 C56 C57 171.3(5) . . ? C58 C57 C56 171.9(4) . . ? C57 C58 C59 169.3(5) . . ? C60 C59 C64 118.8(4) . . ? C60 C59 C58 123.3(4) . . ? C64 C59 C58 117.9(4) . . ? C61 C60 C59 121.6(4) . . ? C60 C61 O8 125.4(4) . . ? C60 C61 C62 119.8(4) . . ? O8 C61 C62 114.8(4) . . ? O7 C62 C63 125.0(4) . . ? O7 C62 C61 115.7(4) . . ? C63 C62 C61 119.3(4) . . ? C62 C63 C64 121.7(4) . . ? C63 C64 C59 118.6(4) . . ? C63 C64 C67 119.1(4) . . ? C59 C64 C67 122.3(4) . . ? C68 C67 C64 175.6(5) . . ? C67 C68 C40 173.9(5) . . ? C73 C69 C70 108.5(4) . . ? C73 C69 Fe2 70.0(3) . . ? C70 C69 Fe2 69.8(3) . . ? C71 C70 C69 107.9(4) . . ? C71 C70 Fe2 70.1(3) . . ? C69 C70 Fe2 69.2(3) . . ? C70 C71 C72 107.4(4) . . ? C70 C71 Fe2 69.4(2) . . ? C72 C71 Fe2 69.4(2) . . ? C73 C72 C71 108.6(4) . . ? C73 C72 Fe2 69.5(2) . . ? C71 C72 Fe2 69.7(2) . . ? C69 C73 C72 107.6(4) . . ? C69 C73 Fe2 69.3(3) . . ? C72 C73 Fe2 70.0(2) . . ? C51 O5 C53 117.7(3) . . ? C50 O6 C54 117.1(3) . . ? C62 O7 C66 117.1(4) . . ? C61 O8 C65 117.3(4) . . ? Cl1 C80 Cl2 112.6(4) . . ? Cl4 C81 Cl3 111.8(3) . . ? Cl5 C82 Cl6 115.8(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.810 _refine_diff_density_min -1.546 _refine_diff_density_rms 0.101