Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Glen Berenger Deacon' 'Thomas Behrsing' 'Craig M. Forsyth' 'Maria Forsyth' 'Kristina Konstas' _publ_contact_author_name 'Prof Glen Berenger Deacon' _publ_contact_author_address ; School of Chemistry Monash University Wellington Rd Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email GLEN.DEACON@SCI.MONASH.EDU.AU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Heterobimetallic CeIII-FeIII-salicylate Networks: Models for Corrosion Mitigation of Steel Surfaces by the 'Green' Inhibitor Ce(salicylate)3 ; data_1 _database_code_CSD 188413 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis((2,2'-dipyridyl)(mu-2-(2-oxobenzoato-O,O',O")iron(iii)) (nitrato-O,O')triaquacerium(iii) ethanol solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H44 Ce Fe2 N5 O19' _chemical_formula_weight 1270.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5989(4) _cell_length_b 19.9199(7) _cell_length_c 20.6430(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.614(2) _cell_angle_gamma 90.00 _cell_volume 5092.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square plate' _exptl_crystal_colour red-purple _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2564 _exptl_absorpt_coefficient_mu 1.524 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'none' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Enraf Nonius Kappa CCD' _diffrn_measurement_method '1 deg scan in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'not measured' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29305 _diffrn_reflns_av_R_equivalents 0.1157 _diffrn_reflns_av_sigmaI/netI 0.2725 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.38 _reflns_number_total 12481 _reflns_number_gt 5319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'POVRAY 3.0' _computing_publication_material ? _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. Hydrogen atoms on water molecules were not included in the refined model. ; _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^)+(0.0432P)^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 12479 _refine_ls_number_parameters 695 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2037 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1360 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 0.922 _refine_ls_restrained_S_all 0.922 _refine_ls_shift/su_max 0.196 _refine_ls_shift/su_mean 0.010 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 Ce1 Ce 0.88638(3) 0.274604(18) 0.245908(18) 0.02753(13) Uani 1 1 d . . . Fe1 Fe 0.71336(8) 0.35747(5) -0.01103(4) 0.0302(3) Uani 1 1 d . . . O1 O 1.0994(4) 0.2796(3) 0.2632(2) 0.0536(14) Uani 1 1 d . . . N1 N 1.1049(6) 0.3436(3) 0.2675(3) 0.0397(17) Uani 1 1 d . . . C1 C 0.9064(6) 0.3133(4) 0.0850(3) 0.0331(18) Uani 1 1 d . . . Fe2 Fe 0.82659(8) 0.53562(4) 0.33020(4) 0.0275(3) Uani 1 1 d . . . O2 O 1.0192(4) 0.3736(2) 0.2745(2) 0.0451(14) Uani 1 1 d . . . N2 N 0.7430(4) 0.4542(3) -0.0528(3) 0.0308(14) Uani 1 1 d . . . C2 C 0.9375(6) 0.2682(3) 0.0338(3) 0.0342(18) Uani 1 1 d . . . O3 O 1.1898(5) 0.3732(3) 0.2650(3) 0.0652(17) Uani 1 1 d . . . N3 N 0.6384(4) 0.4344(3) 0.0431(3) 0.0326(14) Uani 1 1 d . . . C3 C 0.8895(6) 0.2722(3) -0.0338(3) 0.0319(17) Uani 1 1 d . . . O4 O 0.9547(4) 0.3073(2) 0.1441(2) 0.0327(12) Uani 1 1 d . . . N4 N 0.8389(5) 0.5806(2) 0.4269(2) 0.0260(14) Uani 1 1 d . . . C4 C 0.9293(6) 0.2280(4) -0.0765(3) 0.0378(18) Uani 1 1 d . . . H4 H 0.9016 0.2310 -0.1224 0.045 Uiso 1 1 calc R . . O5 O 0.8314(4) 0.3571(2) 0.0684(2) 0.0310(11) Uani 1 1 d . . . N5 N 0.9979(5) 0.5395(2) 0.3708(3) 0.0317(15) Uani 1 1 d . . . C5 C 1.0073(7) 0.1801(4) -0.0545(4) 0.048(2) Uani 1 1 d . . . H5 H 1.0326 0.1515 -0.0852 0.058 Uiso 1 1 calc R . . O6 O 0.8123(4) 0.3139(2) -0.0571(2) 0.0363(12) Uani 1 1 d . . . C6 C 1.0487(7) 0.1739(4) 0.0123(4) 0.057(2) Uani 1 1 d . . . H6 H 1.0990 0.1394 0.0279 0.068 Uiso 1 1 calc R . . O7 O 0.4703(4) 0.2857(2) -0.1545(2) 0.0366(12) Uani 1 1 d . . . C7 C 1.0162(6) 0.2179(4) 0.0552(4) 0.047(2) Uani 1 1 d . . . H7 H 1.0470 0.2148 0.1007 0.056 Uiso 1 1 calc R . . O8 O 0.5980(4) 0.3428(2) -0.0898(2) 0.0340(12) Uani 1 1 d . . . C8 C 0.5155(6) 0.3039(3) -0.0979(4) 0.0334(18) Uani 1 1 d . . . O9 O 0.6425(4) 0.2897(2) 0.03426(19) 0.0293(11) Uani 1 1 d . . . C9 C 0.4712(6) 0.2791(3) -0.0402(3) 0.0314(17) Uani 1 1 d . . . O10 O 0.8079(4) 0.3376(2) 0.32737(19) 0.0306(12) Uani 1 1 d . . . C10 C 0.5365(6) 0.2745(3) 0.0230(3) 0.0316(17) Uani 1 1 d . . . O11 O 0.8342(3) 0.44265(19) 0.3623(2) 0.0282(11) Uani 1 1 d . . . C11 C 0.4871(7) 0.2531(3) 0.0753(4) 0.042(2) Uani 1 1 d . . . H11 H 0.5292 0.2495 0.1183 0.050 Uiso 1 1 calc R . . O12 O 0.6705(3) 0.5312(2) 0.3210(2) 0.0314(11) Uani 1 1 d . . . C12 C 0.3791(7) 0.2372(3) 0.0652(4) 0.043(2) Uani 1 1 d . . . H12 H 0.3473 0.2231 0.1013 0.052 Uiso 1 1 calc R . . O13 O 0.7602(4) 0.7055(2) 0.2185(2) 0.0332(12) Uani 1 1 d . . . C13 C 0.3159(7) 0.2417(3) 0.0023(4) 0.043(2) Uani 1 1 d . . . H13 H 0.2411 0.2310 -0.0047 0.052 Uiso 1 1 calc R . . O14 O 0.8164(4) 0.62927(19) 0.2961(2) 0.0308(12) Uani 1 1 d . . . C14 C 0.3633(6) 0.2619(3) -0.0494(4) 0.0356(18) Uani 1 1 d . . . H14 H 0.3208 0.2640 -0.0924 0.043 Uiso 1 1 calc R . . O15 O 0.8508(3) 0.5063(2) 0.2449(2) 0.0301(11) Uani 1 1 d . . . C15 C 0.7911(5) 0.4594(3) -0.1055(3) 0.0361(18) Uani 1 1 d . . . H15 H 0.8186 0.4198 -0.1221 0.043 Uiso 1 1 calc R . . O16 O 0.7900(3) 0.37970(19) 0.19491(19) 0.0304(11) Uani 1 1 d . . . C16 C 0.8024(6) 0.5198(4) -0.1369(3) 0.042(2) Uani 1 1 d . . . H16 H 0.8367 0.5217 -0.1742 0.051 Uiso 1 1 calc R . . O17 O 0.7514(4) 0.2390(2) 0.14638(19) 0.0355(12) Uani 1 1 d . . . C17 C 0.7625(6) 0.5771(4) -0.1124(3) 0.042(2) Uani 1 1 d . . . H17 H 0.7676 0.6191 -0.1333 0.051 Uiso 1 1 calc R . . O18 O 0.9406(4) 0.1569(2) 0.2116(2) 0.0337(12) Uani 1 1 d . . . C18 C 0.7156(6) 0.5728(4) -0.0578(3) 0.0401(19) Uani 1 1 d . . . H18 H 0.6904 0.6121 -0.0395 0.048 Uiso 1 1 calc R . . O19 O 1.1524(5) 0.1300(3) 0.2729(3) 0.0669(17) Uani 1 1 d . . . H19 H 1.0875 0.1301 0.2538 0.080 Uiso 1 1 calc R . . C19 C 0.7053(5) 0.5108(3) -0.0295(3) 0.0289(17) Uani 1 1 d . . . C20 C 0.6550(6) 0.4994(3) 0.0285(3) 0.0342(18) Uani 1 1 d . . . C21 C 0.6259(6) 0.5517(3) 0.0671(3) 0.042(2) Uani 1 1 d . . . H21 H 0.6384 0.5971 0.0567 0.050 Uiso 1 1 calc R . . C22 C 0.5784(6) 0.5361(4) 0.1209(3) 0.044(2) Uani 1 1 d . . . H22 H 0.5587 0.5709 0.1478 0.052 Uiso 1 1 calc R . . C23 C 0.5602(5) 0.4702(4) 0.1348(3) 0.0359(18) Uani 1 1 d . . . H23 H 0.5263 0.4586 0.1707 0.043 Uiso 1 1 calc R . . C24 C 0.5922(6) 0.4212(3) 0.0953(3) 0.0353(18) Uani 1 1 d . . . H24 H 0.5810 0.3756 0.1057 0.042 Uiso 1 1 calc R . . C25 C 0.7717(6) 0.3945(4) 0.3339(3) 0.0270(17) Uani 1 1 d . . . C26 C 0.6558(6) 0.4097(3) 0.3106(3) 0.0314(18) Uani 1 1 d . . . C27 C 0.6112(6) 0.4757(3) 0.3096(3) 0.0293(17) Uani 1 1 d . . . C28 C 0.4981(6) 0.4815(3) 0.2941(3) 0.0317(18) Uani 1 1 d . . . H28 H 0.4666 0.5247 0.2955 0.038 Uiso 1 1 calc R . . C29 C 0.4308(6) 0.4270(4) 0.2769(3) 0.0373(19) Uani 1 1 d . . . H29 H 0.3546 0.4326 0.2677 0.045 Uiso 1 1 calc R . . C30 C 0.4765(6) 0.3633(4) 0.2733(3) 0.0375(19) Uani 1 1 d . . . H30 H 0.4318 0.3256 0.2594 0.045 Uiso 1 1 calc R . . C31 C 0.5857(6) 0.3557(3) 0.2900(3) 0.0309(17) Uani 1 1 d . . . H31 H 0.6157 0.3122 0.2877 0.037 Uiso 1 1 calc R . . C32 C 0.8064(6) 0.6510(3) 0.2364(3) 0.0329(18) Uani 1 1 d . . . C33 C 0.8541(5) 0.6118(3) 0.1869(3) 0.0270(17) Uani 1 1 d . . . C34 C 0.8736(5) 0.5421(3) 0.1944(3) 0.0254(16) Uani 1 1 d . . . C35 C 0.9179(5) 0.5105(3) 0.1443(3) 0.0328(18) Uani 1 1 d . . . H35 H 0.9358 0.4642 0.1491 0.039 Uiso 1 1 calc R . . C36 C 0.9358(6) 0.5424(3) 0.0908(3) 0.0357(19) Uani 1 1 d . . . H36 H 0.9617 0.5181 0.0573 0.043 Uiso 1 1 calc R . . C37 C 0.9165(6) 0.6119(4) 0.0835(4) 0.041(2) Uani 1 1 d . . . H37 H 0.9313 0.6350 0.0459 0.049 Uiso 1 1 calc R . . C38 C 0.8761(5) 0.6455(3) 0.1314(3) 0.0328(18) Uani 1 1 d . . . H38 H 0.8627 0.6924 0.1270 0.039 Uiso 1 1 calc R . . C39 C 0.7537(6) 0.6025(3) 0.4505(3) 0.0341(18) Uani 1 1 d . . . H39 H 0.6840 0.5988 0.4238 0.041 Uiso 1 1 calc R . . C40 C 0.7633(7) 0.6304(3) 0.5127(3) 0.040(2) Uani 1 1 d . . . H40 H 0.7013 0.6457 0.5284 0.048 Uiso 1 1 calc R . . C41 C 0.8646(8) 0.6356(3) 0.5515(3) 0.045(2) Uani 1 1 d . . . H41 H 0.8725 0.6544 0.5944 0.054 Uiso 1 1 calc R . . C42 C 0.9543(7) 0.6136(3) 0.5281(4) 0.041(2) Uani 1 1 d . . . H42 H 1.0244 0.6168 0.5544 0.049 Uiso 1 1 calc R . . C43 C 0.9391(6) 0.5864(3) 0.4647(3) 0.0299(17) Uani 1 1 d . . . C44 C 1.0287(6) 0.5614(3) 0.4332(3) 0.0327(18) Uani 1 1 d . . . C45 C 1.1357(6) 0.5599(3) 0.4654(4) 0.041(2) Uani 1 1 d . . . H45 H 1.1556 0.5762 0.5092 0.049 Uiso 1 1 calc R . . C46 C 1.2100(7) 0.5350(4) 0.4331(4) 0.048(2) Uani 1 1 d . . . H46 H 1.2836 0.5333 0.4543 0.058 Uiso 1 1 calc R . . C47 C 1.1798(7) 0.5115(3) 0.3687(4) 0.045(2) Uani 1 1 d . . . H47 H 1.2320 0.4939 0.3454 0.055 Uiso 1 1 calc R . . C48 C 1.0716(6) 0.5146(3) 0.3394(4) 0.0346(18) Uani 1 1 d . . . H48 H 1.0499 0.4985 0.2957 0.042 Uiso 1 1 calc R . . C49 C 1.2251(8) 0.1557(6) 0.2241(6) 0.107(4) Uani 1 1 d . . . H49A H 1.2160 0.1264 0.1848 0.128 Uiso 1 1 calc R . . H49B H 1.2035 0.2019 0.2094 0.128 Uiso 1 1 calc R . . C50 C 1.3375(10) 0.1552(6) 0.2575(5) 0.119(4) Uani 1 1 d . . . H50A H 1.3453 0.1826 0.2975 0.178 Uiso 1 1 calc R . . H50B H 1.3830 0.1736 0.2281 0.178 Uiso 1 1 calc R . . H50C H 1.3597 0.1090 0.2694 0.178 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0347(3) 0.0218(2) 0.0218(2) 0.00083(19) -0.00593(16) -0.0003(2) Fe1 0.0393(7) 0.0261(6) 0.0210(5) 0.0003(4) -0.0051(5) -0.0008(5) O1 0.037(4) 0.057(4) 0.060(4) 0.015(3) -0.009(3) -0.002(3) N1 0.045(5) 0.046(5) 0.024(4) 0.008(3) -0.006(3) -0.018(4) C1 0.033(5) 0.036(4) 0.027(4) 0.002(4) -0.001(4) -0.011(4) Fe2 0.0355(7) 0.0212(5) 0.0223(5) -0.0005(4) -0.0040(5) 0.0002(5) O2 0.040(4) 0.048(3) 0.044(3) -0.012(3) 0.000(3) -0.014(3) N2 0.035(4) 0.034(4) 0.022(3) 0.005(3) -0.001(3) 0.000(3) C2 0.037(5) 0.037(4) 0.029(4) 0.001(4) 0.009(4) -0.005(4) O3 0.064(5) 0.070(4) 0.062(4) -0.006(3) 0.012(3) -0.036(4) N3 0.037(4) 0.031(4) 0.025(3) 0.006(3) -0.007(3) 0.001(3) C3 0.038(5) 0.030(4) 0.029(4) -0.001(4) 0.008(4) -0.007(4) O4 0.034(3) 0.039(3) 0.022(3) -0.001(2) -0.004(2) -0.003(2) N4 0.036(4) 0.017(3) 0.023(3) -0.003(2) 0.000(3) 0.007(3) C4 0.039(5) 0.041(5) 0.032(4) 0.000(4) 0.004(4) -0.004(4) O5 0.037(3) 0.026(3) 0.025(3) -0.003(2) -0.008(2) 0.002(2) N5 0.042(4) 0.019(3) 0.031(4) 0.000(3) 0.000(3) 0.001(3) C5 0.057(6) 0.049(5) 0.044(5) -0.012(4) 0.022(5) 0.006(5) O6 0.043(4) 0.035(3) 0.028(3) 0.000(2) 0.000(2) 0.005(3) C6 0.066(7) 0.061(6) 0.042(5) 0.000(5) 0.008(5) 0.037(5) O7 0.042(3) 0.034(3) 0.029(3) -0.005(2) -0.008(2) -0.006(2) C7 0.047(6) 0.062(6) 0.030(4) 0.013(4) 0.003(4) 0.008(5) O8 0.044(3) 0.030(3) 0.024(3) 0.002(2) -0.004(2) -0.006(3) C8 0.033(5) 0.022(4) 0.039(5) -0.001(4) -0.010(4) 0.010(4) O9 0.033(3) 0.033(3) 0.018(2) 0.003(2) -0.007(2) -0.002(2) C9 0.038(5) 0.023(4) 0.029(4) 0.001(3) -0.004(3) 0.006(4) O10 0.042(3) 0.020(3) 0.027(3) 0.001(2) 0.000(2) 0.005(2) C10 0.042(5) 0.017(4) 0.035(4) 0.001(4) 0.004(4) 0.009(4) O11 0.032(3) 0.018(2) 0.030(3) -0.001(2) -0.006(2) 0.000(2) C11 0.050(6) 0.038(4) 0.034(5) 0.009(3) -0.002(4) -0.008(4) O12 0.034(3) 0.025(3) 0.032(3) -0.002(2) -0.005(2) -0.008(2) C12 0.058(6) 0.031(5) 0.045(5) 0.003(4) 0.021(5) 0.003(4) O13 0.046(3) 0.022(3) 0.028(3) 0.003(2) -0.001(2) 0.001(2) C13 0.054(6) 0.034(5) 0.039(5) 0.005(4) 0.003(4) -0.004(4) O14 0.048(3) 0.015(2) 0.024(3) 0.002(2) -0.007(2) 0.002(2) C14 0.037(5) 0.028(4) 0.036(4) -0.006(3) -0.009(4) 0.001(4) O15 0.039(3) 0.027(3) 0.022(3) 0.000(2) -0.002(2) 0.003(2) C15 0.028(5) 0.037(5) 0.040(5) 0.003(4) -0.002(4) 0.007(4) O16 0.038(3) 0.021(2) 0.028(3) 0.005(2) -0.005(2) 0.004(2) C16 0.048(6) 0.050(5) 0.028(4) 0.012(4) 0.007(4) -0.008(4) O17 0.044(3) 0.030(3) 0.025(3) 0.004(2) -0.015(2) -0.004(2) C17 0.051(6) 0.031(5) 0.040(5) 0.020(4) -0.003(4) -0.001(4) O18 0.040(3) 0.027(3) 0.028(3) -0.009(2) -0.007(2) 0.000(2) C18 0.040(5) 0.038(5) 0.038(5) 0.017(4) -0.006(4) -0.001(4) O19 0.042(4) 0.071(4) 0.074(4) -0.017(3) -0.027(3) 0.022(3) C19 0.027(5) 0.033(4) 0.023(4) 0.008(3) -0.006(3) 0.002(3) C20 0.034(5) 0.035(5) 0.026(4) -0.001(4) -0.014(3) -0.002(4) C21 0.054(6) 0.023(4) 0.043(5) -0.002(4) -0.004(4) 0.008(4) C22 0.047(6) 0.051(6) 0.033(5) -0.007(4) 0.006(4) 0.003(4) C23 0.036(5) 0.048(5) 0.022(4) -0.003(4) -0.001(3) -0.004(4) C24 0.045(5) 0.033(4) 0.021(4) -0.002(3) -0.012(4) 0.001(4) C25 0.034(5) 0.032(4) 0.014(4) 0.007(3) 0.003(3) 0.001(4) C26 0.036(5) 0.036(4) 0.020(4) -0.002(3) -0.001(3) 0.004(4) C27 0.033(5) 0.035(5) 0.017(4) 0.004(3) -0.001(3) 0.000(4) C28 0.042(5) 0.032(4) 0.020(4) 0.004(3) 0.003(4) 0.001(4) C29 0.043(5) 0.036(5) 0.032(4) 0.009(4) 0.004(4) -0.003(4) C30 0.039(5) 0.042(5) 0.029(4) 0.004(4) -0.002(4) -0.014(4) C31 0.034(5) 0.024(4) 0.032(4) 0.003(3) 0.001(4) 0.000(4) C32 0.042(5) 0.019(4) 0.035(5) -0.001(4) 0.003(4) -0.008(4) C33 0.023(4) 0.032(4) 0.022(4) -0.006(3) -0.005(3) -0.008(3) C34 0.022(4) 0.030(4) 0.020(4) 0.002(3) -0.008(3) -0.001(3) C35 0.033(5) 0.030(4) 0.036(4) 0.006(4) 0.007(4) 0.006(3) C36 0.041(5) 0.036(5) 0.031(4) -0.002(4) 0.007(4) -0.002(4) C37 0.038(5) 0.044(5) 0.040(5) 0.005(4) 0.002(4) -0.009(4) C38 0.035(5) 0.032(4) 0.030(4) 0.000(4) 0.003(4) -0.002(4) C39 0.044(6) 0.025(4) 0.032(4) 0.007(3) 0.002(4) -0.004(4) C40 0.064(6) 0.036(5) 0.022(4) 0.002(4) 0.009(4) 0.001(4) C41 0.089(7) 0.022(4) 0.018(4) 0.001(3) -0.006(5) -0.009(5) C42 0.050(6) 0.028(4) 0.037(5) -0.002(4) -0.013(4) -0.006(4) C43 0.038(5) 0.016(4) 0.031(4) 0.004(3) -0.005(4) -0.009(3) C44 0.041(5) 0.019(4) 0.035(5) 0.010(3) -0.001(4) -0.003(4) C45 0.036(6) 0.032(4) 0.045(5) 0.001(4) -0.016(4) -0.001(4) C46 0.031(6) 0.048(5) 0.059(6) 0.005(5) -0.009(5) -0.013(4) C47 0.040(6) 0.035(5) 0.063(6) 0.006(4) 0.012(5) 0.014(4) C48 0.033(5) 0.031(4) 0.036(5) -0.001(4) -0.001(4) 0.003(4) C49 0.050(8) 0.120(10) 0.143(11) -0.039(8) -0.005(8) 0.022(7) C50 0.113(11) 0.146(11) 0.088(9) -0.009(8) -0.009(8) -0.014(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 Ce1 O7 2.448(4) 4_666 ? Ce1 O10 2.448(4) . ? Ce1 O4 2.499(4) . ? Ce1 O17 2.515(4) . ? Ce1 O13 2.519(4) 2_645 ? Ce1 O16 2.549(4) . ? Ce1 O18 2.578(4) . ? Ce1 O2 2.584(5) . ? Ce1 O1 2.644(5) . ? Fe1 O6 1.910(4) . ? Fe1 O9 1.950(4) . ? Fe1 O8 1.992(5) . ? Fe1 O5 2.001(4) . ? Fe1 N2 2.171(5) . ? Fe1 N3 2.209(5) . ? O1 N1 1.277(7) . ? N1 O3 1.230(7) . ? N1 O2 1.266(7) . ? C1 O4 1.266(7) . ? C1 O5 1.285(8) . ? C1 C2 1.494(9) . ? Fe2 O15 1.932(4) . ? Fe2 O12 1.943(4) . ? Fe2 O11 1.963(4) . ? Fe2 O14 1.990(4) . ? Fe2 N4 2.168(5) . ? Fe2 N5 2.168(6) . ? N2 C15 1.343(8) . ? N2 C19 1.347(8) . ? C2 C3 1.417(9) . ? C2 C7 1.421(9) . ? N3 C24 1.341(8) . ? N3 C20 1.353(8) . ? C3 O6 1.302(8) . ? C3 C4 1.402(9) . ? N4 C39 1.332(8) . ? N4 C43 1.361(8) . ? C4 C5 1.385(9) . ? N5 C48 1.323(8) . ? N5 C44 1.346(8) . ? C5 C6 1.386(10) . ? C6 C7 1.362(9) . ? O7 C8 1.255(7) . ? O7 Ce1 2.448(4) 4_565 ? O8 C8 1.282(8) . ? C8 C9 1.490(9) . ? O9 C10 1.346(7) . ? C9 C14 1.382(9) . ? C9 C10 1.412(9) . ? O10 C25 1.239(7) . ? C10 C11 1.407(9) . ? O11 C25 1.309(7) . ? C11 C12 1.375(9) . ? O12 C27 1.331(7) . ? C12 C13 1.396(9) . ? O13 C32 1.256(7) . ? O13 Ce1 2.519(4) 2_655 ? C13 C14 1.375(9) . ? O14 C32 1.291(7) . ? O15 C34 1.338(7) . ? C15 C16 1.388(9) . ? C16 C17 1.379(9) . ? C17 C18 1.368(9) . ? C18 C19 1.383(8) . ? O19 C49 1.567(11) . ? C19 C20 1.472(9) . ? C20 C21 1.401(9) . ? C21 C22 1.389(9) . ? C22 C23 1.372(9) . ? C23 C24 1.377(8) . ? C25 C26 1.482(9) . ? C26 C31 1.406(9) . ? C26 C27 1.429(9) . ? C27 C28 1.407(9) . ? C28 C29 1.383(9) . ? C29 C30 1.402(9) . ? C30 C31 1.364(8) . ? C32 C33 1.497(9) . ? C33 C38 1.399(8) . ? C33 C34 1.413(8) . ? C34 C35 1.409(8) . ? C35 C36 1.329(8) . ? C36 C37 1.409(9) . ? C37 C38 1.369(9) . ? C39 C40 1.384(8) . ? C40 C41 1.379(10) . ? C41 C42 1.380(9) . ? C42 C43 1.398(9) . ? C43 C44 1.489(9) . ? C44 C45 1.389(9) . ? C45 C46 1.341(9) . ? C46 C47 1.396(10) . ? C47 C48 1.387(9) . ? C49 C50 1.455(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 O7 Ce1 O10 80.86(14) 4_666 . ? O7 Ce1 O4 132.21(15) 4_666 . ? O10 Ce1 O4 133.59(14) . . ? O7 Ce1 O17 132.10(14) 4_666 . ? O10 Ce1 O17 114.06(14) . . ? O4 Ce1 O17 70.86(14) . . ? O7 Ce1 O13 73.34(15) 4_666 2_645 ? O10 Ce1 O13 70.64(14) . 2_645 ? O4 Ce1 O13 140.55(14) . 2_645 ? O17 Ce1 O13 70.30(14) . 2_645 ? O7 Ce1 O16 148.17(13) 4_666 . ? O10 Ce1 O16 68.95(13) . . ? O4 Ce1 O16 69.54(13) . . ? O17 Ce1 O16 72.24(13) . . ? O13 Ce1 O16 104.47(14) 2_645 . ? O7 Ce1 O18 71.90(13) 4_666 . ? O10 Ce1 O18 144.70(13) . . ? O4 Ce1 O18 81.70(13) . . ? O17 Ce1 O18 72.09(13) . . ? O13 Ce1 O18 80.18(14) 2_645 . ? O16 Ce1 O18 139.79(13) . . ? O7 Ce1 O2 91.23(15) 4_666 . ? O10 Ce1 O2 77.23(15) . . ? O4 Ce1 O2 71.59(14) . . ? O17 Ce1 O2 135.51(14) . . ? O13 Ce1 O2 146.03(15) 2_645 . ? O16 Ce1 O2 72.94(16) . . ? O18 Ce1 O2 124.31(16) . . ? O7 Ce1 O1 68.56(15) 4_666 . ? O10 Ce1 O1 114.63(16) . . ? O4 Ce1 O1 66.74(15) . . ? O17 Ce1 O1 129.60(15) . . ? O13 Ce1 O1 139.66(15) 2_645 . ? O16 Ce1 O1 114.79(15) . . ? O18 Ce1 O1 75.97(16) . . ? O2 Ce1 O1 48.80(17) . . ? O6 Fe1 O9 108.84(19) . . ? O6 Fe1 O8 88.40(19) . . ? O9 Fe1 O8 87.70(18) . . ? O6 Fe1 O5 87.24(19) . . ? O9 Fe1 O5 86.63(18) . . ? O8 Fe1 O5 171.34(18) . . ? O6 Fe1 N2 91.7(2) . . ? O9 Fe1 N2 158.8(2) . . ? O8 Fe1 N2 87.65(19) . . ? O5 Fe1 N2 99.95(19) . . ? O6 Fe1 N3 161.1(2) . . ? O9 Fe1 N3 87.78(19) . . ? O8 Fe1 N3 101.49(19) . . ? O5 Fe1 N3 84.82(18) . . ? N2 Fe1 N3 72.9(2) . . ? N1 O1 Ce1 95.0(4) . . ? O3 N1 O2 122.9(7) . . ? O3 N1 O1 120.8(7) . . ? O2 N1 O1 116.3(6) . . ? O4 C1 O5 121.4(6) . . ? O4 C1 C2 118.8(7) . . ? O5 C1 C2 119.8(6) . . ? O15 Fe2 O12 102.98(18) . . ? O15 Fe2 O11 90.94(17) . . ? O12 Fe2 O11 88.62(18) . . ? O15 Fe2 O14 88.38(17) . . ? O12 Fe2 O14 90.54(18) . . ? O11 Fe2 O14 178.78(19) . . ? O15 Fe2 N4 165.4(2) . . ? O12 Fe2 N4 90.5(2) . . ? O11 Fe2 N4 95.07(18) . . ? O14 Fe2 N4 85.82(17) . . ? O15 Fe2 N5 92.9(2) . . ? O12 Fe2 N5 163.15(19) . . ? O11 Fe2 N5 85.40(18) . . ? O14 Fe2 N5 95.64(18) . . ? N4 Fe2 N5 74.4(2) . . ? N1 O2 Ce1 98.2(4) . . ? C15 N2 C19 117.9(5) . . ? C15 N2 Fe1 121.7(4) . . ? C19 N2 Fe1 120.2(4) . . ? C3 C2 C7 119.5(6) . . ? C3 C2 C1 122.8(7) . . ? C7 C2 C1 117.7(6) . . ? C24 N3 C20 118.3(6) . . ? C24 N3 Fe1 124.1(4) . . ? C20 N3 Fe1 116.9(4) . . ? O6 C3 C4 119.8(6) . . ? O6 C3 C2 123.7(6) . . ? C4 C3 C2 116.5(7) . . ? C1 O4 Ce1 131.1(4) . . ? C39 N4 C43 119.3(6) . . ? C39 N4 Fe2 123.1(5) . . ? C43 N4 Fe2 117.6(4) . . ? C5 C4 C3 122.8(7) . . ? C1 O5 Fe1 128.3(4) . . ? C48 N5 C44 119.0(6) . . ? C48 N5 Fe2 122.4(5) . . ? C44 N5 Fe2 118.2(5) . . ? C4 C5 C6 120.1(7) . . ? C3 O6 Fe1 128.1(4) . . ? C7 C6 C5 119.1(7) . . ? C8 O7 Ce1 167.3(4) . 4_565 ? C6 C7 C2 121.8(7) . . ? C8 O8 Fe1 130.3(4) . . ? O7 C8 O8 121.0(7) . . ? O7 C8 C9 118.4(7) . . ? O8 C8 C9 120.6(6) . . ? C10 O9 Fe1 126.9(4) . . ? C14 C9 C10 120.2(7) . . ? C14 C9 C8 118.5(6) . . ? C10 C9 C8 121.4(7) . . ? C25 O10 Ce1 138.3(4) . . ? O9 C10 C11 120.1(6) . . ? O9 C10 C9 122.3(6) . . ? C11 C10 C9 117.6(7) . . ? C25 O11 Fe2 123.5(4) . . ? C12 C11 C10 121.4(7) . . ? C27 O12 Fe2 125.4(4) . . ? C11 C12 C13 120.3(7) . . ? C32 O13 Ce1 135.4(4) . 2_655 ? C14 C13 C12 119.1(8) . . ? C32 O14 Fe2 129.9(4) . . ? C13 C14 C9 121.5(7) . . ? C34 O15 Fe2 129.9(4) . . ? N2 C15 C16 123.1(7) . . ? C17 C16 C15 118.1(7) . . ? C18 C17 C16 119.5(6) . . ? C17 C18 C19 119.5(7) . . ? N2 C19 C18 121.9(6) . . ? N2 C19 C20 113.2(6) . . ? C18 C19 C20 124.8(7) . . ? N3 C20 C21 121.2(6) . . ? N3 C20 C19 115.9(6) . . ? C21 C20 C19 122.9(6) . . ? C22 C21 C20 118.9(7) . . ? C23 C22 C21 119.6(7) . . ? C22 C23 C24 118.4(6) . . ? N3 C24 C23 123.6(6) . . ? O10 C25 O11 121.1(6) . . ? O10 C25 C26 120.7(6) . . ? O11 C25 C26 118.2(6) . . ? C31 C26 C27 118.5(7) . . ? C31 C26 C25 117.9(6) . . ? C27 C26 C25 123.6(6) . . ? O12 C27 C28 118.9(6) . . ? O12 C27 C26 123.8(7) . . ? C28 C27 C26 117.2(6) . . ? C29 C28 C27 122.8(7) . . ? C28 C29 C30 119.1(7) . . ? C31 C30 C29 119.5(7) . . ? C30 C31 C26 122.7(7) . . ? O13 C32 O14 122.0(6) . . ? O13 C32 C33 118.3(6) . . ? O14 C32 C33 119.7(6) . . ? C38 C33 C34 120.3(6) . . ? C38 C33 C32 118.2(6) . . ? C34 C33 C32 121.5(6) . . ? O15 C34 C35 120.3(6) . . ? O15 C34 C33 123.4(6) . . ? C35 C34 C33 116.3(6) . . ? C36 C35 C34 123.1(6) . . ? C35 C36 C37 120.5(6) . . ? C38 C37 C36 118.8(6) . . ? C37 C38 C33 120.9(6) . . ? N4 C39 C40 122.1(7) . . ? C41 C40 C39 118.8(7) . . ? C40 C41 C42 120.2(7) . . ? C41 C42 C43 118.1(7) . . ? N4 C43 C42 121.4(7) . . ? N4 C43 C44 114.8(6) . . ? C42 C43 C44 123.7(7) . . ? N5 C44 C45 122.3(7) . . ? N5 C44 C43 114.7(6) . . ? C45 C44 C43 123.0(7) . . ? C46 C45 C44 118.4(7) . . ? C45 C46 C47 120.3(8) . . ? C48 C47 C46 118.3(7) . . ? N5 C48 C47 121.7(7) . . ? C50 C49 O19 109.0(9) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.568 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.135 #========END data_2 _database_code_CSD 188414 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis((2,2'-dipyridyl)(mu-2-(2-oxobenzoato-O,O',O") iron(iii))endecaaquadicerium(iii).bis(2-hydroxybenzoate). ethanol.triaqua solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C112 H107 Ce2 Fe4 N8 O45' _chemical_formula_weight 2788.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 '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 13.8916(3) _cell_length_b 19.8401(5) _cell_length_c 22.2319(5) _cell_angle_alpha 86.592(1) _cell_angle_beta 78.871(1) _cell_angle_gamma 83.810(1) _cell_volume 5972(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2830 _exptl_absorpt_coefficient_mu 1.311 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'none' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Enraf-Nonius Kappa CCD' _diffrn_measurement_method '1 deg scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'not measured' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51308 _diffrn_reflns_av_R_equivalents 0.0976 _diffrn_reflns_av_sigmaI/netI 0.2934 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.30 _reflns_number_total 28519 _reflns_number_gt 11382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'POVRAY 3.0' _computing_publication_material ? _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. Carbon atoms were refined isotropically, full anisotropic refinedment gave unreasonable thermal envelopes for several carbon atoms associated with the bpy residues, possibly consequent upon unresolved disorder. Hydrogent atoms attached to oxygen of water molecules and the lattice components were not included in the refined model. ; _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^)+(0.1169P)^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 28519 _refine_ls_number_parameters 890 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2367 _refine_ls_R_factor_gt 0.0891 _refine_ls_wR_factor_ref 0.2627 _refine_ls_wR_factor_gt 0.2090 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.107 _refine_ls_shift/su_mean 0.011 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 Ce1 Ce 1.04068(4) 0.26030(3) 0.19026(2) 0.02807(17) Uani 1 1 d . . . Fe1 Fe 1.19071(11) 0.14125(7) -0.05650(6) 0.0354(4) Uani 1 1 d . . . O1 O 1.3998(5) 0.1327(4) -0.2179(3) 0.046(2) Uani 1 1 d . . . N1 N 1.1054(6) 0.0630(4) -0.0817(4) 0.043(2) Uiso 1 1 d . . . C1 C 1.3641(8) 0.1429(5) -0.1625(5) 0.041(3) Uiso 1 1 d . . . Ce2 Ce 0.81431(4) 0.75662(3) 0.32367(2) 0.03082(17) Uani 1 1 d . . . Fe2 Fe 0.92080(10) 0.53310(7) 0.18389(6) 0.0278(3) Uiso 1 1 d . . . O2 O 1.2735(5) 0.1317(3) -0.1400(3) 0.0391(17) Uani 1 1 d . . . N2 N 1.2346(7) 0.0463(5) -0.0090(4) 0.050(2) Uiso 1 1 d . . . C2 C 1.4217(8) 0.1711(5) -0.1223(5) 0.041(3) Uiso 1 1 d . . . Fe3 Fe 1.15744(11) 0.32211(7) 0.40908(6) 0.0343(4) Uani 1 1 d . . . O3 O 1.2971(6) 0.1793(4) -0.0317(3) 0.047(2) Uani 1 1 d . . . N3 N 1.0199(6) 0.5491(4) 0.0979(3) 0.0306(19) Uiso 1 1 d . . . C3 C 1.3884(9) 0.1849(6) -0.0611(5) 0.045(3) Uiso 1 1 d . . . Fe4 Fe 0.90413(13) 1.02720(7) 0.32581(7) 0.0466(5) Uani 1 1 d . . . O4 O 1.0014(5) 0.2222(4) 0.0949(3) 0.0397(18) Uani 1 1 d . . . N4 N 0.8312(6) 0.5921(4) 0.1245(3) 0.0302(19) Uiso 1 1 d . . . C4 C 1.4536(9) 0.2096(6) -0.0280(5) 0.051(3) Uiso 1 1 d . . . H4 H 1.4318 0.2168 0.0145 0.062 Uiso 1 1 calc R . . O5 O 1.1112(5) 0.1672(3) 0.0258(3) 0.0358(17) Uani 1 1 d . . . N5 N 1.2469(6) 0.4061(4) 0.4094(4) 0.036(2) Uiso 1 1 d . . . C5 C 1.5458(10) 0.2235(7) -0.0545(6) 0.068(4) Uiso 1 1 d . . . H5 H 1.5871 0.2398 -0.0304 0.082 Uiso 1 1 calc R . . O6 O 1.1073(5) 0.2104(3) -0.0920(3) 0.0340(17) Uani 1 1 d . . . N6 N 1.0555(6) 0.4144(4) 0.4109(4) 0.036(2) Uiso 1 1 d . . . C6 C 1.5808(11) 0.2142(7) -0.1164(6) 0.076(4) Uiso 1 1 d . . . H6 H 1.6440 0.2263 -0.1360 0.091 Uiso 1 1 calc R . . O7 O 0.8839(5) 0.3343(3) 0.1731(3) 0.0386(18) Uani 1 1 d . . . C7 C 1.5190(9) 0.1862(6) -0.1490(6) 0.060(3) Uiso 1 1 d . . . H7 H 1.5432 0.1769 -0.1909 0.072 Uiso 1 1 calc R . . O8 O 0.9155(5) 0.4412(3) 0.1567(3) 0.0328(16) Uani 1 1 d . . . C8 C 1.0308(8) 0.2052(5) 0.0402(5) 0.032(2) Uiso 1 1 d . . . O9 O 0.8032(5) 0.5228(3) 0.2434(3) 0.0320(16) Uani 1 1 d . . . C9 C 0.9722(7) 0.2301(5) -0.0073(4) 0.029(2) Uiso 1 1 d . . . O10 O 0.9779(5) 0.6931(3) 0.2761(3) 0.0354(17) Uani 1 1 d . . . C10 C 1.0139(8) 0.2309(5) -0.0696(4) 0.033(2) Uiso 1 1 d . . . O11 O 0.9343(5) 0.6216(3) 0.2166(3) 0.0308(16) Uani 1 1 d . . . C11 C 0.9515(8) 0.2559(5) -0.1112(5) 0.045(3) Uiso 1 1 d . . . H11 H 0.9785 0.2583 -0.1538 0.054 Uiso 1 1 calc R . . O12 O 1.0267(5) 0.4944(3) 0.2240(3) 0.0330(16) Uani 1 1 d . . . C12 C 0.8528(8) 0.2769(5) -0.0917(5) 0.046(3) Uiso 1 1 d . . . H12 H 0.8125 0.2920 -0.1208 0.055 Uiso 1 1 calc R . . O13 O 1.1918(5) 0.2797(3) 0.2268(3) 0.0355(17) Uani 1 1 d . . . C13 C 0.8131(9) 0.2756(6) -0.0295(5) 0.048(3) Uiso 1 1 d . . . H13 H 0.7454 0.2900 -0.0156 0.058 Uiso 1 1 calc R . . O14 O 1.1584(5) 0.3229(3) 0.3197(3) 0.0326(16) Uani 1 1 d . . . C14 C 0.8737(7) 0.2530(5) 0.0126(5) 0.036(2) Uiso 1 1 d . . . H14 H 0.8471 0.2533 0.0553 0.043 Uiso 1 1 calc R . . O15 O 1.2731(5) 0.2576(4) 0.3953(3) 0.0435(19) Uani 1 1 d . . . C15 C 1.0475(8) 0.0752(6) -0.1211(5) 0.048(3) Uiso 1 1 d . . . H15 H 1.0403 0.1194 -0.1396 0.057 Uiso 1 1 calc R . . O16 O 1.1006(5) 0.2945(3) 0.5970(3) 0.0403(18) Uani 1 1 d . . . C16 C 0.9949(9) 0.0238(6) -0.1370(6) 0.064(4) Uiso 1 1 d . . . H16 H 0.9527 0.0328 -0.1660 0.077 Uiso 1 1 calc R . . O17 O 1.1554(5) 0.3132(3) 0.4990(3) 0.0371(17) Uani 1 1 d . . . C17 C 1.0062(9) -0.0363(7) -0.1104(6) 0.063(3) Uiso 1 1 d . . . H17 H 0.9682 -0.0705 -0.1186 0.075 Uiso 1 1 calc R . . O18 O 1.0460(5) 0.2695(3) 0.4214(3) 0.0354(17) Uani 1 1 d . . . C18 C 1.0701(8) -0.0516(6) -0.0715(5) 0.052(3) Uiso 1 1 d . . . H18 H 1.0807 -0.0965 -0.0551 0.062 Uiso 1 1 calc R . . O19 O 0.9586(6) 0.8227(3) 0.3227(4) 0.054(2) Uani 1 1 d . . . C19 C 1.1188(8) -0.0006(5) -0.0567(5) 0.042(3) Uiso 1 1 d . . . O20 O 0.9168(6) 0.9293(3) 0.3500(3) 0.046(2) Uani 1 1 d . . . C20 C 1.1886(8) -0.0096(6) -0.0153(5) 0.050(3) Uiso 1 1 d . . . O21 O 1.0378(6) 1.0186(4) 0.2803(4) 0.053(2) Uani 1 1 d . . . C21 C 1.2070(10) -0.0705(7) 0.0187(6) 0.067(4) Uiso 1 1 d . . . H21 H 1.1750 -0.1093 0.0139 0.080 Uiso 1 1 calc R . . O22 O 0.8937(5) 1.2029(3) 0.2223(3) 0.0353(17) Uani 1 1 d . . . C22 C 1.2706(11) -0.0731(8) 0.0582(7) 0.087(5) Uiso 1 1 d . . . H22 H 1.2836 -0.1140 0.0810 0.104 Uiso 1 1 calc R . . O23 O 0.8944(5) 1.1215(3) 0.2949(3) 0.0412(18) Uani 1 1 d . . . C23 C 1.3155(12) -0.0182(8) 0.0652(7) 0.093(5) Uiso 1 1 d . . . H23 H 1.3597 -0.0200 0.0931 0.112 Uiso 1 1 calc R . . O24 O 0.8204(5) 1.0071(3) 0.2699(3) 0.049(2) Uani 1 1 d . . . C24 C 1.2956(10) 0.0443(7) 0.0295(6) 0.067(4) Uiso 1 1 d . . . O25 O 0.5059(6) 0.7371(4) 0.4798(3) 0.060(2) Uani 1 1 d . . . C25 C 0.8565(7) 0.3964(5) 0.1782(4) 0.033(2) Uiso 1 1 d . . . O26 O 0.4820(6) 0.6282(4) 0.4762(3) 0.054(2) Uani 1 1 d . . . C26 C 0.7576(7) 0.4197(5) 0.2107(4) 0.033(2) Uiso 1 1 d . . . O27 O 0.3600(6) 0.5753(4) 0.5580(3) 0.050(2) Uani 1 1 d . . . C27 C 0.7332(7) 0.4823(5) 0.2413(4) 0.031(2) Uiso 1 1 d . . . O28 O 1.2617(5) 0.4041(4) 0.1112(3) 0.047(2) Uani 1 1 d . . . C28 C 0.6375(8) 0.4990(6) 0.2715(5) 0.047(3) Uiso 1 1 d . . . H28 H 0.6221 0.5395 0.2936 0.057 Uiso 1 1 calc R . . O29 O 1.3548(5) 0.3075(3) 0.0921(3) 0.0366(17) Uani 1 1 d . . . C29 C 0.5637(9) 0.4579(6) 0.2702(5) 0.050(3) Uiso 1 1 d . . . H29 H 0.4974 0.4718 0.2884 0.061 Uiso 1 1 calc R . . O30 O 1.5393(6) 0.3050(4) 0.0747(4) 0.062(2) Uani 1 1 d . . . C30 C 0.5869(9) 0.3960(6) 0.2420(5) 0.051(3) Uiso 1 1 d . . . H30 H 0.5360 0.3675 0.2425 0.062 Uiso 1 1 calc R . . O31 O 0.9993(5) 0.3618(3) 0.2625(3) 0.0309(16) Uani 1 1 d . . . C31 C 0.6826(8) 0.3744(6) 0.2131(5) 0.047(3) Uiso 1 1 d . . . H31 H 0.6979 0.3312 0.1956 0.056 Uiso 1 1 calc R . . O32 O 1.0874(5) 0.3608(3) 0.1253(3) 0.0318(16) Uani 1 1 d . . . C32 C 0.9955(7) 0.6383(5) 0.2487(4) 0.033(2) Uiso 1 1 d . . . O33 O 1.2057(5) 0.2268(3) 0.1117(3) 0.0332(16) Uani 1 1 d . . . C33 C 1.0874(7) 0.5955(5) 0.2511(4) 0.032(2) Uiso 1 1 d . . . O34 O 1.1012(5) 0.1318(3) 0.2014(3) 0.0361(17) Uani 1 1 d . . . C34 C 1.0996(7) 0.5264(5) 0.2392(4) 0.031(2) Uiso 1 1 d . . . O35 O 1.0207(5) 0.2202(3) 0.3069(3) 0.0387(18) Uani 1 1 d . . . C35 C 1.1877(7) 0.4887(5) 0.2445(4) 0.037(2) Uiso 1 1 d . . . H35 H 1.1954 0.4414 0.2379 0.045 Uiso 1 1 calc R . . O36 O 0.6968(5) 0.7195(3) 0.4228(3) 0.0418(18) Uani 1 1 d . . . C36 C 1.2625(9) 0.5183(6) 0.2588(5) 0.052(3) Uiso 1 1 d . . . H36 H 1.3227 0.4912 0.2605 0.062 Uiso 1 1 calc R . . O37 O 0.7606(6) 0.8554(4) 0.3967(3) 0.056(2) Uani 1 1 d . . . C37 C 1.2560(8) 0.5855(6) 0.2709(5) 0.046(3) Uiso 1 1 d . . . H37 H 1.3097 0.6052 0.2814 0.056 Uiso 1 1 calc R . . O38 O 0.8032(6) 0.8673(4) 0.2559(3) 0.056(2) Uani 1 1 d . . . C38 C 1.1679(8) 0.6236(6) 0.2673(5) 0.043(3) Uiso 1 1 d . . . H38 H 1.1611 0.6704 0.2759 0.052 Uiso 1 1 calc R . . O39 O 0.8112(5) 0.7353(3) 0.2112(3) 0.0373(17) Uani 1 1 d . . . C39 C 1.1162(7) 0.5243(5) 0.0878(4) 0.034(2) Uiso 1 1 d . . . H39 H 1.1434 0.5027 0.1208 0.041 Uiso 1 1 calc R . . O40 O 0.7722(5) 0.6357(3) 0.3205(3) 0.0361(17) Uani 1 1 d . . . C40 C 1.1759(8) 0.5296(5) 0.0306(4) 0.037(2) Uiso 1 1 d . . . H40 H 1.2428 0.5107 0.0243 0.044 Uiso 1 1 calc R . . O41 O 0.6361(5) 0.7842(5) 0.3122(3) 0.063(2) Uani 1 1 d . . . C41 C 1.1370(7) 0.5630(5) -0.0179(5) 0.038(3) Uiso 1 1 d . . . H41 H 1.1767 0.5673 -0.0576 0.045 Uiso 1 1 calc R . . O42 O 0.4735(14) 0.7420(7) 0.3468(7) 0.177(7) Uani 1 1 d . . . C42 C 1.0405(7) 0.5891(5) -0.0068(4) 0.033(2) Uiso 1 1 d . . . H42 H 1.0130 0.6128 -0.0389 0.040 Uiso 1 1 calc R . . O43 O 0.6603(6) 0.5674(4) 0.4164(4) 0.065(2) Uani 1 1 d . . . C43 C 0.9820(7) 0.5815(5) 0.0510(4) 0.030(2) Uiso 1 1 d . . . O44 O 0.7093(14) 0.8501(5) 0.5192(5) 0.185(8) Uani 1 1 d . . . C44 C 0.8765(7) 0.6069(5) 0.0669(4) 0.030(2) Uiso 1 1 d . . . O45 O 1.3066(8) 0.1164(5) 0.1744(6) 0.114(4) Uani 1 1 d . . . C45 C 0.8248(7) 0.6407(4) 0.0251(4) 0.028(2) Uiso 1 1 d . . . H45 H 0.8570 0.6499 -0.0158 0.033 Uiso 1 1 calc R . . C46 C 0.7269(8) 0.6609(5) 0.0432(5) 0.037(2) Uiso 1 1 d . . . H46 H 0.6907 0.6832 0.0144 0.044 Uiso 1 1 calc R . . C47 C 0.6809(8) 0.6495(5) 0.1014(5) 0.039(3) Uiso 1 1 d . . . H47 H 0.6136 0.6651 0.1150 0.046 Uiso 1 1 calc R . . C48 C 0.7373(7) 0.6135(5) 0.1413(5) 0.035(2) Uiso 1 1 d . . . H48 H 0.7060 0.6042 0.1824 0.042 Uiso 1 1 calc R . . C49 C 1.0876(8) 0.2941(5) 0.5428(5) 0.036(2) Uiso 1 1 d . . . C50 C 0.9925(7) 0.2774(5) 0.5313(4) 0.035(2) Uiso 1 1 d . . . C51 C 0.9750(7) 0.2652(5) 0.4725(4) 0.034(2) Uiso 1 1 d . . . C52 C 0.8822(8) 0.2494(5) 0.4671(5) 0.041(3) Uiso 1 1 d . . . H52 H 0.8696 0.2410 0.4279 0.049 Uiso 1 1 calc R . . C53 C 0.8088(9) 0.2458(6) 0.5176(5) 0.049(3) Uiso 1 1 d . . . H53 H 0.7455 0.2354 0.5131 0.059 Uiso 1 1 calc R . . C54 C 0.8265(9) 0.2576(6) 0.5764(5) 0.051(3) Uiso 1 1 d . . . H54 H 0.7754 0.2550 0.6114 0.061 Uiso 1 1 calc R . . C55 C 0.9158(8) 0.2724(5) 0.5823(5) 0.043(3) Uiso 1 1 d . . . H55 H 0.9277 0.2798 0.6220 0.052 Uiso 1 1 calc R . . C56 C 1.2174(7) 0.2885(5) 0.2773(5) 0.031(2) Uiso 1 1 d . . . C57 C 1.3157(7) 0.2640(5) 0.2852(4) 0.035(2) Uiso 1 1 d . . . C58 C 1.3377(8) 0.2487(5) 0.3447(5) 0.040(3) Uiso 1 1 d . . . C59 C 1.4359(9) 0.2228(6) 0.3491(5) 0.051(3) Uiso 1 1 d . . . H59 H 1.4524 0.2130 0.3885 0.062 Uiso 1 1 calc R . . C60 C 1.5089(10) 0.2116(6) 0.2962(6) 0.060(3) Uiso 1 1 d . . . H60 H 1.5737 0.1933 0.3000 0.073 Uiso 1 1 calc R . . C61 C 1.4864(9) 0.2270(6) 0.2393(6) 0.061(3) Uiso 1 1 d . . . H61 H 1.5357 0.2200 0.2035 0.073 Uiso 1 1 calc R . . C62 C 1.3897(8) 0.2533(5) 0.2340(5) 0.042(3) Uiso 1 1 d . . . H62 H 1.3749 0.2640 0.1943 0.051 Uiso 1 1 calc R . . C63 C 1.3431(9) 0.3985(6) 0.4088(5) 0.053(3) Uiso 1 1 d . . . H63 H 1.3770 0.3543 0.4057 0.064 Uiso 1 1 calc R . . C64 C 1.3962(10) 0.4539(6) 0.4128(5) 0.058(3) Uiso 1 1 d . . . H64 H 1.4655 0.4474 0.4107 0.070 Uiso 1 1 calc R . . C65 C 1.3490(9) 0.5149(6) 0.4194(5) 0.056(3) Uiso 1 1 d . . . H65 H 1.3851 0.5522 0.4223 0.067 Uiso 1 1 calc R . . C66 C 1.2489(9) 0.5261(6) 0.4221(5) 0.052(3) Uiso 1 1 d . . . H66 H 1.2153 0.5702 0.4279 0.063 Uiso 1 1 calc R . . C67 C 1.1970(8) 0.4695(5) 0.4161(5) 0.039(3) Uiso 1 1 d . . . C68 C 1.0912(8) 0.4762(5) 0.4132(5) 0.038(3) Uiso 1 1 d . . . C69 C 1.0314(9) 0.5360(6) 0.4147(5) 0.052(3) Uiso 1 1 d . . . H69 H 1.0583 0.5776 0.4168 0.062 Uiso 1 1 calc R . . C70 C 0.9354(9) 0.5364(6) 0.4132(5) 0.057(3) Uiso 1 1 d . . . H70 H 0.8943 0.5779 0.4143 0.069 Uiso 1 1 calc R . . C71 C 0.8957(9) 0.4739(6) 0.4099(5) 0.054(3) Uiso 1 1 d . . . H71 H 0.8282 0.4718 0.4084 0.065 Uiso 1 1 calc R . . C72 C 0.9616(8) 0.4163(5) 0.4089(5) 0.041(3) Uiso 1 1 d . . . H72 H 0.9363 0.3741 0.4066 0.049 Uiso 1 1 calc R . . C73 C 0.9787(8) 0.8813(6) 0.3232(5) 0.043(3) Uiso 1 1 d . . . C74 C 1.0731(8) 0.8986(6) 0.2940(5) 0.044(3) Uiso 1 1 d . . . C75 C 1.1034(10) 0.9636(6) 0.2764(5) 0.056(3) Uiso 1 1 d . . . C76 C 1.2003(12) 0.9717(9) 0.2517(7) 0.091(5) Uiso 1 1 d . . . H76 H 1.2192 1.0165 0.2436 0.109 Uiso 1 1 calc R . . C77 C 1.2742(13) 0.9154(9) 0.2375(7) 0.102(5) Uiso 1 1 d . . . H77 H 1.3399 0.9225 0.2186 0.122 Uiso 1 1 calc R . . C78 C 1.2456(12) 0.8485(9) 0.2526(7) 0.094(5) Uiso 1 1 d . . . H78 H 1.2920 0.8099 0.2439 0.113 Uiso 1 1 calc R . . C79 C 1.1466(10) 0.8411(7) 0.2806(6) 0.068(4) Uiso 1 1 d . . . H79 H 1.1275 0.7967 0.2911 0.081 Uiso 1 1 calc R . . C80 C 0.8657(7) 1.1480(5) 0.2452(4) 0.033(2) Uiso 1 1 d . . . C81 C 0.7966(7) 1.1130(5) 0.2173(4) 0.035(2) Uiso 1 1 d . . . C82 C 0.7763(8) 1.0476(5) 0.2313(5) 0.041(3) Uiso 1 1 d . . . C83 C 0.7096(9) 1.0221(6) 0.2021(5) 0.054(3) Uiso 1 1 d . . . H83 H 0.6932 0.9770 0.2123 0.065 Uiso 1 1 calc R . . C84 C 0.6660(10) 1.0599(7) 0.1586(6) 0.065(4) Uiso 1 1 d . . . H84 H 0.6210 1.0406 0.1390 0.077 Uiso 1 1 calc R . . C85 C 0.6874(9) 1.1239(6) 0.1441(5) 0.052(3) Uiso 1 1 d . . . H85 H 0.6578 1.1503 0.1141 0.063 Uiso 1 1 calc R . . C86 C 0.7524(8) 1.1510(6) 0.1729(5) 0.047(3) Uiso 1 1 d . . . H86 H 0.7678 1.1963 0.1625 0.056 Uiso 1 1 calc R . . N7 N 0.7688(8) 1.0375(5) 0.3988(5) 0.097(4) Uiso 1 1 d G . . C87 C 0.6771(11) 1.0309(7) 0.3847(6) 0.147(8) Uiso 1 1 d G . . H87 H 0.6727 1.0171 0.3452 0.176 Uiso 1 1 calc R . . C88 C 0.5920(8) 1.0445(9) 0.4283(9) 0.290(18) Uiso 1 1 d G . . H88 H 0.5293 1.0401 0.4186 0.349 Uiso 1 1 calc R . . C89 C 0.5984(11) 1.0648(8) 0.4860(7) 0.205(12) Uiso 1 1 d G . . H89 H 0.5402 1.0741 0.5159 0.246 Uiso 1 1 calc R . . C90 C 0.6901(14) 1.0713(7) 0.5002(5) 0.156(8) Uiso 1 1 d G . . H90 H 0.6945 1.0851 0.5397 0.188 Uiso 1 1 calc R . . C91 C 0.7752(10) 1.0577(7) 0.4566(7) 0.177(10) Uiso 1 1 d G . . N8 N 0.9477(4) 1.0602(2) 0.4041(3) 0.091(4) Uiso 1 1 d G . . C92 C 0.8790(4) 1.0684(2) 0.4582(3) 0.091(5) Uiso 1 1 d G . . C93 C 0.9078(4) 1.0879(2) 0.5106(3) 0.155(8) Uiso 1 1 d G . . H93 H 0.8608 1.0936 0.5476 0.186 Uiso 1 1 calc R . . C94 C 1.0054(4) 1.0993(2) 0.5088(3) 0.099(5) Uiso 1 1 d G . . H94 H 1.0251 1.1126 0.5445 0.118 Uiso 1 1 calc R . . C95 C 1.0741(4) 1.0910(2) 0.4546(3) 0.154(8) Uiso 1 1 d G . . H95 H 1.1407 1.0988 0.4534 0.185 Uiso 1 1 calc R . . C96 C 1.0452(4) 1.0715(2) 0.4023(3) 0.085(4) Uiso 1 1 d G . . H96 H 1.0922 1.0659 0.3653 0.102 Uiso 1 1 calc R . . C97 C 0.4641(3) 0.6854(2) 0.50010(19) 0.040(3) Uiso 1 1 d G . . C98 C 0.3846(3) 0.6930(2) 0.55788(19) 0.041(3) Uiso 1 1 d G . . C99 C 0.3361(3) 0.6374(2) 0.5845(2) 0.039(3) Uiso 1 1 d G . . C100 C 0.2658(3) 0.6415(2) 0.6381(2) 0.043(3) Uiso 1 1 d G . . H100 H 0.2352 0.6030 0.6567 0.051 Uiso 1 1 calc R . . C101 C 0.2432(8) 0.7034(6) 0.6622(5) 0.049(3) Uiso 1 1 d . . . H101 H 0.1953 0.7076 0.6989 0.058 Uiso 1 1 calc R . . C102 C 0.2867(3) 0.7628(2) 0.6361(2) 0.047(3) Uiso 1 1 d G . . H102 H 0.2661 0.8057 0.6535 0.056 Uiso 1 1 calc R . . C103 C 0.3610(8) 0.7556(5) 0.5836(5) 0.042(3) Uiso 1 1 d . . . H103 H 0.3946 0.7934 0.5660 0.050 Uiso 1 1 calc R . . C104 C 1.3417(8) 0.3703(6) 0.0998(5) 0.036(2) Uiso 1 1 d . . . C105 C 1.4305(8) 0.4086(5) 0.0952(5) 0.040(3) Uiso 1 1 d . . . C106 C 1.5253(8) 0.3726(6) 0.0816(5) 0.048(3) Uiso 1 1 d . . . C107 C 1.6083(5) 0.4083(4) 0.0763(4) 0.058(3) Uiso 1 1 d G . . H107 H 1.6728 0.3855 0.0667 0.069 Uiso 1 1 calc R . . C108 C 1.5945(10) 0.4791(7) 0.0854(6) 0.067(4) Uiso 1 1 d . . . H108 H 1.6504 0.5033 0.0839 0.080 Uiso 1 1 calc R . . C109 C 1.5042(9) 0.5126(6) 0.0961(5) 0.056(3) Uiso 1 1 d . . . H109 H 1.4965 0.5605 0.0993 0.068 Uiso 1 1 calc R . . C110 C 1.4208(9) 0.4763(6) 0.1025(5) 0.054(3) Uiso 1 1 d . . . H110 H 1.3568 0.4998 0.1121 0.064 Uiso 1 1 calc R . . C111 C 0.4775(19) 0.6733(14) 0.3303(11) 0.177(10) Uiso 1 1 d . . . H11A H 0.4188 0.6523 0.3529 0.212 Uiso 1 1 calc R . . H11B H 0.5372 0.6469 0.3405 0.212 Uiso 1 1 calc R . . C112 C 0.4801(4) 0.6738(3) 0.2569(2) 0.203(11) Uiso 1 1 d G . . H11C H 0.4868 0.6270 0.2437 0.304 Uiso 1 1 calc R . . H11D H 0.5363 0.6970 0.2352 0.304 Uiso 1 1 calc R . . H11E H 0.4189 0.6976 0.2477 0.304 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0365(4) 0.0264(3) 0.0217(3) -0.0050(2) -0.0039(3) -0.0058(3) Fe1 0.0486(10) 0.0305(8) 0.0287(8) -0.0070(6) -0.0079(7) -0.0062(7) O1 0.048(5) 0.057(5) 0.036(4) -0.003(4) -0.014(4) -0.011(4) Ce2 0.0421(4) 0.0279(3) 0.0225(3) -0.0042(2) -0.0045(3) -0.0049(3) O2 0.046(5) 0.032(4) 0.039(4) -0.011(3) -0.003(3) -0.009(3) Fe3 0.0468(10) 0.0367(9) 0.0220(7) -0.0018(6) -0.0097(7) -0.0094(7) O3 0.053(5) 0.047(5) 0.045(5) -0.012(4) -0.015(4) -0.005(4) Fe4 0.0818(13) 0.0254(8) 0.0330(9) -0.0022(7) -0.0079(9) -0.0124(8) O4 0.042(5) 0.052(5) 0.026(4) -0.012(3) -0.005(3) -0.010(4) O5 0.050(5) 0.033(4) 0.026(4) -0.004(3) -0.011(3) -0.006(4) O6 0.041(5) 0.036(4) 0.027(4) 0.000(3) -0.007(3) -0.012(3) O7 0.040(5) 0.036(4) 0.042(4) -0.006(3) -0.010(3) -0.007(3) O8 0.045(4) 0.022(4) 0.031(4) -0.001(3) -0.005(3) -0.006(3) O9 0.031(4) 0.032(4) 0.031(4) -0.001(3) -0.003(3) -0.004(3) O10 0.046(5) 0.027(4) 0.033(4) -0.008(3) -0.005(3) -0.006(3) O11 0.040(4) 0.026(4) 0.030(4) -0.009(3) -0.012(3) -0.005(3) O12 0.044(5) 0.026(4) 0.030(4) 0.000(3) -0.007(3) -0.003(3) O13 0.039(4) 0.042(4) 0.025(4) -0.010(3) -0.003(3) -0.003(3) O14 0.039(4) 0.033(4) 0.029(4) -0.007(3) -0.014(3) -0.002(3) O15 0.042(5) 0.063(5) 0.026(4) 0.003(4) -0.012(3) 0.001(4) O16 0.058(5) 0.041(4) 0.022(4) 0.003(3) -0.009(3) -0.005(4) O17 0.042(5) 0.048(4) 0.023(4) -0.006(3) -0.005(3) -0.011(4) O18 0.043(5) 0.042(4) 0.024(4) -0.004(3) -0.006(3) -0.012(3) O19 0.063(6) 0.025(4) 0.075(6) -0.008(4) -0.014(4) -0.010(4) O20 0.078(6) 0.026(4) 0.038(4) 0.003(3) -0.016(4) -0.011(4) O21 0.059(6) 0.037(5) 0.071(6) 0.007(4) -0.027(5) -0.012(4) O22 0.043(5) 0.029(4) 0.032(4) 0.000(3) -0.002(3) -0.007(3) O23 0.062(5) 0.032(4) 0.032(4) -0.004(3) -0.008(4) -0.017(4) O24 0.045(5) 0.031(4) 0.074(5) -0.001(4) -0.018(4) -0.013(4) O25 0.057(6) 0.057(5) 0.053(5) 0.014(4) 0.015(4) 0.000(4) O26 0.052(5) 0.058(5) 0.047(5) -0.013(4) 0.006(4) -0.004(4) O27 0.056(5) 0.051(5) 0.044(5) -0.011(4) -0.008(4) -0.005(4) O28 0.034(5) 0.042(5) 0.067(5) -0.001(4) -0.012(4) -0.002(4) O29 0.041(5) 0.034(4) 0.035(4) -0.009(3) -0.007(3) -0.004(3) O30 0.050(6) 0.048(5) 0.087(6) -0.026(4) -0.004(5) -0.006(4) O31 0.034(4) 0.036(4) 0.023(3) -0.004(3) -0.002(3) -0.005(3) O32 0.045(4) 0.026(4) 0.027(4) -0.008(3) -0.008(3) -0.008(3) O33 0.037(4) 0.035(4) 0.027(4) -0.010(3) 0.000(3) -0.004(3) O34 0.044(5) 0.024(4) 0.042(4) -0.003(3) -0.008(3) -0.006(3) O35 0.052(5) 0.037(4) 0.030(4) -0.007(3) -0.008(3) -0.011(4) O36 0.059(5) 0.038(4) 0.026(4) -0.009(3) -0.003(3) -0.002(4) O37 0.089(7) 0.041(5) 0.040(5) -0.007(4) -0.012(4) -0.013(4) O38 0.094(7) 0.036(4) 0.041(5) -0.002(4) -0.026(4) -0.004(4) O39 0.046(5) 0.040(4) 0.024(4) -0.006(3) -0.003(3) 0.001(3) O40 0.040(4) 0.040(4) 0.028(4) -0.005(3) 0.002(3) -0.017(3) O41 0.039(5) 0.109(7) 0.032(4) -0.006(4) 0.007(4) 0.017(5) O42 0.29(2) 0.108(11) 0.158(13) -0.030(10) -0.084(13) -0.063(12) O43 0.066(6) 0.049(5) 0.068(6) 0.002(4) 0.021(4) -0.017(4) O44 0.42(2) 0.055(7) 0.049(7) 0.008(6) 0.004(10) 0.043(10) O45 0.088(8) 0.066(7) 0.186(12) 0.014(7) -0.022(8) -0.017(6) _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 Ce1 O22 2.412(6) 1_545 ? Ce1 O32 2.460(6) . ? Ce1 O13 2.467(6) . ? Ce1 O4 2.468(6) . ? Ce1 O7 2.571(7) . ? Ce1 O31 2.598(7) . ? Ce1 O34 2.610(6) . ? Ce1 O35 2.639(6) . ? Ce1 O33 2.648(7) . ? Fe1 O3 1.914(7) . ? Fe1 O6 1.931(6) . ? Fe1 O2 1.995(7) . ? Fe1 O5 2.009(7) . ? Fe1 N2 2.191(9) . ? Fe1 N1 2.211(9) . ? O1 C1 1.255(12) . ? N1 C15 1.295(12) . ? N1 C19 1.357(12) . ? C1 O2 1.299(12) . ? C1 C2 1.478(14) . ? Ce2 O16 2.423(6) 2_766 ? Ce2 O19 2.507(7) . ? Ce2 O41 2.535(7) . ? Ce2 O40 2.538(6) . ? Ce2 O10 2.546(7) . ? Ce2 O39 2.570(6) . ? Ce2 O37 2.574(8) . ? Ce2 O36 2.596(7) . ? Ce2 O38 2.596(6) . ? Fe2 O9 1.915(6) . ? Fe2 O12 1.931(6) . ? Fe2 O8 1.968(6) . ? Fe2 O11 1.980(6) . ? Fe2 N3 2.157(8) . ? Fe2 N4 2.190(7) . ? N2 C24 1.311(14) . ? N2 C20 1.365(13) . ? C2 C3 1.383(15) . ? C2 C7 1.424(15) . ? Fe3 O18 1.927(6) . ? Fe3 O15 1.930(7) . ? Fe3 O14 1.983(6) . ? Fe3 O17 1.991(6) . ? Fe3 N5 2.185(8) . ? Fe3 N6 2.188(8) . ? O3 C3 1.323(12) . ? N3 C39 1.356(12) . ? N3 C43 1.356(10) . ? C3 C4 1.414(15) . ? Fe4 O21 1.930(8) . ? Fe4 O24 1.942(7) . ? Fe4 O23 1.955(6) . ? Fe4 O20 1.982(6) . ? Fe4 N8 2.109(6) . ? Fe4 N7 2.234(11) . ? O4 C8 1.261(11) . ? N4 C48 1.317(12) . ? N4 C44 1.344(11) . ? C4 C5 1.353(16) . ? O5 C8 1.276(12) . ? N5 C63 1.325(13) . ? N5 C67 1.372(13) . ? C5 C6 1.384(18) . ? O6 C10 1.327(12) . ? N6 C72 1.310(12) . ? N6 C68 1.378(12) . ? C6 C7 1.400(16) . ? O7 C25 1.255(11) . ? O8 C25 1.283(11) . ? C8 C9 1.484(12) . ? O9 C27 1.335(11) . ? C9 C14 1.390(13) . ? C9 C10 1.394(13) . ? O10 C32 1.255(11) . ? C10 C11 1.420(13) . ? O11 C32 1.289(11) . ? C11 C12 1.381(15) . ? O12 C34 1.356(11) . ? C12 C13 1.387(15) . ? O13 C56 1.268(11) . ? C13 C14 1.400(13) . ? O14 C56 1.298(12) . ? O15 C58 1.305(12) . ? C15 C16 1.415(15) . ? O16 C49 1.253(11) . ? O16 Ce2 2.423(6) 2_766 ? C16 C17 1.307(15) . ? O17 C49 1.287(11) . ? C17 C18 1.354(15) . ? O18 C51 1.358(11) . ? C18 C19 1.364(14) . ? O19 C73 1.225(12) . ? C19 C20 1.451(14) . ? O20 C73 1.301(13) . ? C20 C21 1.413(15) . ? O21 C75 1.341(14) . ? C21 C22 1.356(17) . ? O22 C80 1.245(10) . ? O22 Ce1 2.412(6) 1_565 ? C22 C23 1.342(19) . ? O23 C80 1.307(10) . ? C23 C24 1.463(18) . ? O24 C82 1.331(11) . ? O25 C97 1.252(8) . ? C25 C26 1.465(14) . ? O26 C97 1.261(9) . ? C26 C27 1.426(14) . ? C26 C31 1.438(14) . ? O27 C99 1.378(9) . ? C27 C28 1.385(14) . ? O28 C104 1.225(12) . ? C28 C29 1.382(14) . ? O29 C104 1.257(12) . ? C29 C30 1.389(15) . ? O30 C106 1.348(13) . ? C30 C31 1.394(15) . ? C32 C33 1.463(13) . ? C33 C34 1.399(13) . ? C33 C38 1.416(13) . ? C34 C35 1.385(13) . ? C35 C36 1.344(14) . ? C36 C37 1.367(15) . ? C37 C38 1.381(14) . ? C39 C40 1.382(13) . ? C40 C41 1.399(12) . ? C41 C42 1.366(13) . ? O42 C111 1.42(3) . ? C42 C43 1.391(13) . ? C43 C44 1.479(13) . ? C44 C45 1.381(11) . ? C45 C46 1.364(13) . ? C46 C47 1.345(13) . ? C47 C48 1.408(13) . ? C49 C50 1.467(13) . ? C50 C55 1.404(14) . ? C50 C51 1.414(13) . ? C51 C52 1.388(13) . ? C52 C53 1.368(14) . ? C53 C54 1.412(15) . ? C54 C55 1.339(14) . ? C56 C57 1.439(13) . ? C57 C62 1.389(14) . ? C57 C58 1.422(13) . ? C58 C59 1.425(15) . ? C59 C60 1.409(16) . ? C60 C61 1.371(15) . ? C61 C62 1.413(15) . ? C63 C64 1.405(15) . ? C64 C65 1.314(16) . ? C65 C66 1.376(15) . ? C66 C67 1.423(14) . ? C67 C68 1.476(14) . ? C68 C69 1.371(15) . ? C69 C70 1.339(15) . ? C70 C71 1.421(15) . ? C71 C72 1.382(15) . ? C73 C74 1.415(14) . ? C74 C75 1.409(15) . ? C74 C79 1.451(17) . ? C75 C76 1.374(18) . ? C76 C77 1.44(2) . ? C77 C78 1.43(2) . ? C78 C79 1.416(18) . ? C80 C81 1.488(13) . ? C81 C82 1.362(13) . ? C81 C86 1.403(13) . ? C82 C83 1.382(14) . ? C83 C84 1.382(15) . ? C84 C85 1.343(15) . ? C85 C86 1.373(14) . ? N7 C87 1.3900 . ? N7 C91 1.3900 . ? C87 C88 1.3900 . ? C88 C89 1.3900 . ? C89 C90 1.3900 . ? C90 C91 1.3900 . ? C91 C92 1.486(12) . ? N8 C92 1.3900 . ? N8 C96 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C95 C96 1.3900 . ? C97 C98 1.5266 . ? C98 C103 1.379(12) . ? C98 C99 1.3965 . ? C99 C100 1.3877 . ? C100 C101 1.351(12) . ? C101 C102 1.423(11) . ? C102 C103 1.404(12) . ? C104 C105 1.501(14) . ? C105 C110 1.352(15) . ? C105 C106 1.416(15) . ? C106 C107 1.400(13) . ? C107 C108 1.418(15) . ? C108 C109 1.339(16) . ? C109 C110 1.408(15) . ? C111 C112 1.62(2) . ? 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 O22 Ce1 O32 136.4(2) 1_545 . ? O22 Ce1 O13 140.0(2) 1_545 . ? O32 Ce1 O13 80.4(2) . . ? O22 Ce1 O4 74.7(2) 1_545 . ? O32 Ce1 O4 83.1(2) . . ? O13 Ce1 O4 136.1(2) . . ? O22 Ce1 O7 67.3(2) 1_545 . ? O32 Ce1 O7 70.7(2) . . ? O13 Ce1 O7 135.3(2) . . ? O4 Ce1 O7 74.0(2) . . ? O22 Ce1 O31 100.0(2) 1_545 . ? O32 Ce1 O31 74.41(19) . . ? O13 Ce1 O31 71.8(2) . . ? O4 Ce1 O31 140.5(2) . . ? O7 Ce1 O31 68.1(2) . . ? O22 Ce1 O34 74.2(2) 1_545 . ? O32 Ce1 O34 139.0(2) . . ? O13 Ce1 O34 85.0(2) . . ? O4 Ce1 O34 81.4(2) . . ? O7 Ce1 O34 138.5(2) . . ? O31 Ce1 O34 135.79(19) . . ? O22 Ce1 O35 69.2(2) 1_545 . ? O32 Ce1 O35 138.3(2) . . ? O13 Ce1 O35 71.6(2) . . ? O4 Ce1 O35 138.2(2) . . ? O7 Ce1 O35 109.2(2) . . ? O31 Ce1 O35 67.95(19) . . ? O34 Ce1 O35 69.2(2) . . ? O22 Ce1 O33 131.2(2) 1_545 . ? O32 Ce1 O33 71.0(2) . . ? O13 Ce1 O33 65.9(2) . . ? O4 Ce1 O33 70.2(2) . . ? O7 Ce1 O33 129.8(2) . . ? O31 Ce1 O33 128.60(19) . . ? O34 Ce1 O33 68.1(2) . . ? O35 Ce1 O33 120.9(2) . . ? O3 Fe1 O6 111.0(3) . . ? O3 Fe1 O2 88.5(3) . . ? O6 Fe1 O2 87.5(3) . . ? O3 Fe1 O5 86.1(3) . . ? O6 Fe1 O5 87.1(3) . . ? O2 Fe1 O5 170.5(3) . . ? O3 Fe1 N2 87.8(3) . . ? O6 Fe1 N2 159.1(3) . . ? O2 Fe1 N2 102.4(3) . . ? O5 Fe1 N2 85.2(3) . . ? O3 Fe1 N1 158.6(3) . . ? O6 Fe1 N1 89.5(3) . . ? O2 Fe1 N1 86.3(3) . . ? O5 Fe1 N1 101.4(3) . . ? N2 Fe1 N1 73.1(3) . . ? C15 N1 C19 119.8(10) . . ? C15 N1 Fe1 122.3(7) . . ? C19 N1 Fe1 117.9(6) . . ? O1 C1 O2 120.3(9) . . ? O1 C1 C2 121.2(10) . . ? O2 C1 C2 118.4(10) . . ? O16 Ce2 O19 73.1(2) 2_766 . ? O16 Ce2 O41 136.0(2) 2_766 . ? O19 Ce2 O41 136.1(3) . . ? O16 Ce2 O40 81.5(2) 2_766 . ? O19 Ce2 O40 141.0(2) . . ? O41 Ce2 O40 82.4(3) . . ? O16 Ce2 O10 69.6(2) 2_766 . ? O19 Ce2 O10 67.2(2) . . ? O41 Ce2 O10 143.6(2) . . ? O40 Ce2 O10 76.5(2) . . ? O16 Ce2 O39 137.1(2) 2_766 . ? O19 Ce2 O39 106.7(2) . . ? O41 Ce2 O39 74.5(2) . . ? O40 Ce2 O39 73.1(2) . . ? O10 Ce2 O39 71.2(2) . . ? O16 Ce2 O37 84.9(2) 2_766 . ? O19 Ce2 O37 70.9(3) . . ? O41 Ce2 O37 79.2(3) . . ? O40 Ce2 O37 136.3(2) . . ? O10 Ce2 O37 135.6(2) . . ? O39 Ce2 O37 136.7(2) . . ? O16 Ce2 O36 66.3(2) 2_766 . ? O19 Ce2 O36 124.0(2) . . ? O41 Ce2 O36 69.6(2) . . ? O40 Ce2 O36 67.7(2) . . ? O10 Ce2 O36 126.1(2) . . ? O39 Ce2 O36 129.3(2) . . ? O37 Ce2 O36 68.7(2) . . ? O16 Ce2 O38 140.4(2) 2_766 . ? O19 Ce2 O38 68.8(2) . . ? O41 Ce2 O38 72.2(3) . . ? O40 Ce2 O38 136.7(2) . . ? O10 Ce2 O38 104.2(2) . . ? O39 Ce2 O38 66.7(2) . . ? O37 Ce2 O38 72.9(2) . . ? O36 Ce2 O38 129.6(2) . . ? O9 Fe2 O12 104.7(3) . . ? O9 Fe2 O8 89.2(3) . . ? O12 Fe2 O8 86.8(3) . . ? O9 Fe2 O11 91.1(3) . . ? O12 Fe2 O11 87.9(3) . . ? O8 Fe2 O11 174.5(2) . . ? O9 Fe2 N3 161.9(3) . . ? O12 Fe2 N3 92.6(3) . . ? O8 Fe2 N3 86.4(3) . . ? O11 Fe2 N3 95.0(3) . . ? O9 Fe2 N4 89.0(3) . . ? O12 Fe2 N4 164.9(3) . . ? O8 Fe2 N4 99.9(3) . . ? O11 Fe2 N4 85.5(3) . . ? N3 Fe2 N4 74.5(3) . . ? C1 O2 Fe1 132.6(7) . . ? C24 N2 C20 120.2(10) . . ? C24 N2 Fe1 121.4(8) . . ? C20 N2 Fe1 118.0(7) . . ? C3 C2 C7 117.3(10) . . ? C3 C2 C1 125.5(10) . . ? C7 C2 C1 117.2(10) . . ? O18 Fe3 O15 106.0(3) . . ? O18 Fe3 O14 88.0(3) . . ? O15 Fe3 O14 87.9(3) . . ? O18 Fe3 O17 88.8(3) . . ? O15 Fe3 O17 89.8(3) . . ? O14 Fe3 O17 175.3(3) . . ? O18 Fe3 N5 161.4(3) . . ? O15 Fe3 N5 91.7(3) . . ? O14 Fe3 N5 98.5(3) . . ? O17 Fe3 N5 85.6(3) . . ? O18 Fe3 N6 88.8(3) . . ? O15 Fe3 N6 164.0(3) . . ? O14 Fe3 N6 86.6(3) . . ? O17 Fe3 N6 96.7(3) . . ? N5 Fe3 N6 74.3(3) . . ? C3 O3 Fe1 130.3(7) . . ? C39 N3 C43 118.9(8) . . ? C39 N3 Fe2 122.9(6) . . ? C43 N3 Fe2 118.0(6) . . ? O3 C3 C2 124.1(10) . . ? O3 C3 C4 117.0(10) . . ? C2 C3 C4 118.8(11) . . ? O21 Fe4 O24 106.6(3) . . ? O21 Fe4 O23 87.3(3) . . ? O24 Fe4 O23 88.5(3) . . ? O21 Fe4 O20 90.1(3) . . ? O24 Fe4 O20 88.4(3) . . ? O23 Fe4 O20 175.2(3) . . ? O21 Fe4 N8 92.5(3) . . ? O24 Fe4 N8 160.4(3) . . ? O23 Fe4 N8 88.6(2) . . ? O20 Fe4 N8 95.5(2) . . ? O21 Fe4 N7 165.4(4) . . ? O24 Fe4 N7 87.7(4) . . ? O23 Fe4 N7 96.4(3) . . ? O20 Fe4 N7 87.1(4) . . ? N8 Fe4 N7 73.4(4) . . ? C8 O4 Ce1 148.6(6) . . ? C48 N4 C44 118.5(8) . . ? C48 N4 Fe2 124.7(6) . . ? C44 N4 Fe2 116.8(6) . . ? C5 C4 C3 122.5(12) . . ? C8 O5 Fe1 131.1(6) . . ? C63 N5 C67 119.2(9) . . ? C63 N5 Fe3 124.2(7) . . ? C67 N5 Fe3 116.4(6) . . ? C4 C5 C6 120.9(13) . . ? C10 O6 Fe1 126.7(5) . . ? C72 N6 C68 116.1(9) . . ? C72 N6 Fe3 125.1(7) . . ? C68 N6 Fe3 118.8(6) . . ? C5 C6 C7 117.1(14) . . ? C25 O7 Ce1 133.1(6) . . ? C6 C7 C2 123.2(13) . . ? C25 O8 Fe2 130.2(7) . . ? O4 C8 O5 119.9(9) . . ? O4 C8 C9 119.7(10) . . ? O5 C8 C9 120.4(9) . . ? C27 O9 Fe2 127.5(6) . . ? C14 C9 C10 120.8(8) . . ? C14 C9 C8 117.5(9) . . ? C10 C9 C8 121.7(9) . . ? C32 O10 Ce2 130.3(6) . . ? O6 C10 C9 124.3(8) . . ? O6 C10 C11 118.5(9) . . ? C9 C10 C11 117.2(10) . . ? C32 O11 Fe2 130.7(6) . . ? C12 C11 C10 122.1(10) . . ? C34 O12 Fe2 128.0(5) . . ? C11 C12 C13 119.6(10) . . ? C56 O13 Ce1 138.0(6) . . ? C12 C13 C14 119.4(11) . . ? C56 O14 Fe3 129.5(6) . . ? C9 C14 C13 120.8(10) . . ? C58 O15 Fe3 127.8(6) . . ? N1 C15 C16 121.1(10) . . ? C49 O16 Ce2 148.1(7) . 2_766 ? C17 C16 C15 117.9(12) . . ? C49 O17 Fe3 129.6(6) . . ? C16 C17 C18 122.4(13) . . ? C51 O18 Fe3 127.3(6) . . ? C17 C18 C19 118.1(11) . . ? C73 O19 Ce2 140.7(8) . . ? N1 C19 C18 120.7(9) . . ? N1 C19 C20 115.3(9) . . ? C18 C19 C20 124.0(10) . . ? C73 O20 Fe4 128.0(7) . . ? N2 C20 C21 120.7(10) . . ? N2 C20 C19 115.6(9) . . ? C21 C20 C19 123.7(11) . . ? C75 O21 Fe4 127.9(7) . . ? C22 C21 C20 119.4(13) . . ? C80 O22 Ce1 141.6(6) . 1_565 ? C23 C22 C21 120.4(15) . . ? C80 O23 Fe4 130.0(6) . . ? C22 C23 C24 119.3(14) . . ? C82 O24 Fe4 130.6(6) . . ? N2 C24 C23 120.0(12) . . ? O7 C25 O8 120.9(10) . . ? O7 C25 C26 120.9(9) . . ? O8 C25 C26 118.1(9) . . ? C27 C26 C31 119.4(10) . . ? C27 C26 C25 124.2(9) . . ? C31 C26 C25 116.4(10) . . ? O9 C27 C28 120.1(10) . . ? O9 C27 C26 120.3(9) . . ? C28 C27 C26 119.5(9) . . ? C29 C28 C27 121.3(12) . . ? C28 C29 C30 119.6(12) . . ? C29 C30 C31 122.1(11) . . ? C30 C31 C26 117.9(11) . . ? O10 C32 O11 119.8(9) . . ? O10 C32 C33 119.7(9) . . ? O11 C32 C33 120.5(9) . . ? C34 C33 C38 117.3(9) . . ? C34 C33 C32 122.8(9) . . ? C38 C33 C32 119.9(9) . . ? O12 C34 C35 118.6(9) . . ? O12 C34 C33 121.9(9) . . ? C35 C34 C33 119.4(9) . . ? C36 C35 C34 120.7(10) . . ? C35 C36 C37 123.1(12) . . ? C36 C37 C38 116.9(11) . . ? C37 C38 C33 122.5(10) . . ? N3 C39 C40 121.8(9) . . ? C39 C40 C41 119.4(10) . . ? C42 C41 C40 118.3(10) . . ? C41 C42 C43 120.7(9) . . ? N3 C43 C42 120.8(9) . . ? N3 C43 C44 114.7(8) . . ? C42 C43 C44 124.5(8) . . ? N4 C44 C45 121.0(9) . . ? N4 C44 C43 115.8(8) . . ? C45 C44 C43 123.2(9) . . ? C46 C45 C44 119.4(9) . . ? C47 C46 C45 120.8(9) . . ? C46 C47 C48 116.9(10) . . ? N4 C48 C47 123.3(9) . . ? O16 C49 O17 118.9(9) . . ? O16 C49 C50 119.2(9) . . ? O17 C49 C50 121.8(9) . . ? C55 C50 C51 119.0(9) . . ? C55 C50 C49 117.3(9) . . ? C51 C50 C49 123.7(9) . . ? O18 C51 C52 119.4(9) . . ? O18 C51 C50 121.8(9) . . ? C52 C51 C50 118.8(9) . . ? C53 C52 C51 120.7(10) . . ? C52 C53 C54 120.5(11) . . ? C55 C54 C53 119.4(11) . . ? C54 C55 C50 121.6(11) . . ? O13 C56 O14 120.7(9) . . ? O13 C56 C57 118.9(10) . . ? O14 C56 C57 120.3(9) . . ? C62 C57 C58 119.4(10) . . ? C62 C57 C56 119.6(9) . . ? C58 C57 C56 120.9(10) . . ? O15 C58 C57 123.6(10) . . ? O15 C58 C59 118.3(9) . . ? C57 C58 C59 118.1(10) . . ? C60 C59 C58 121.1(11) . . ? C61 C60 C59 119.9(12) . . ? C60 C61 C62 119.8(12) . . ? C57 C62 C61 121.7(10) . . ? N5 C63 C64 122.0(12) . . ? C65 C64 C63 119.3(13) . . ? C64 C65 C66 121.8(12) . . ? C65 C66 C67 117.9(11) . . ? N5 C67 C66 119.8(10) . . ? N5 C67 C68 117.3(9) . . ? C66 C67 C68 122.8(10) . . ? C69 C68 N6 121.9(10) . . ? C69 C68 C67 125.4(10) . . ? N6 C68 C67 112.7(9) . . ? C70 C69 C68 120.8(12) . . ? C69 C70 C71 119.3(12) . . ? C72 C71 C70 115.8(11) . . ? N6 C72 C71 126.3(10) . . ? O19 C73 O20 122.9(11) . . ? O19 C73 C74 119.6(12) . . ? O20 C73 C74 117.5(10) . . ? C75 C74 C73 128.4(11) . . ? C75 C74 C79 117.1(11) . . ? C73 C74 C79 114.5(10) . . ? O21 C75 C76 118.2(12) . . ? O21 C75 C74 120.8(11) . . ? C76 C75 C74 120.9(13) . . ? C75 C76 C77 122.8(15) . . ? C78 C77 C76 118.0(17) . . ? C79 C78 C77 118.5(16) . . ? C78 C79 C74 122.6(13) . . ? O22 C80 O23 120.4(9) . . ? O22 C80 C81 120.0(8) . . ? O23 C80 C81 119.5(8) . . ? C82 C81 C86 119.6(9) . . ? C82 C81 C80 124.3(9) . . ? C86 C81 C80 116.0(9) . . ? O24 C82 C81 123.0(9) . . ? O24 C82 C83 119.1(9) . . ? C81 C82 C83 117.9(10) . . ? C82 C83 C84 122.2(11) . . ? C85 C84 C83 119.8(12) . . ? C84 C85 C86 119.4(11) . . ? C85 C86 C81 121.1(10) . . ? C87 N7 C91 120.0 . . ? C87 N7 Fe4 120.0(8) . . ? C91 N7 Fe4 119.6(9) . . ? N7 C87 C88 120.0 . . ? C89 C88 C87 120.0 . . ? C90 C89 C88 120.0 . . ? C89 C90 C91 120.0 . . ? C90 C91 N7 120.0 . . ? C90 C91 C92 129.8(11) . . ? N7 C91 C92 109.8(11) . . ? C92 N8 C96 120.0 . . ? C92 N8 Fe4 119.66(14) . . ? C96 N8 Fe4 120.31(15) . . ? C93 C92 N8 120.0 . . ? C93 C92 C91 122.6(6) . . ? N8 C92 C91 117.4(6) . . ? C92 C93 C94 120.0 . . ? C95 C94 C93 120.0 . . ? C94 C95 C96 120.0 . . ? C95 C96 N8 120.0 . . ? O25 C97 O26 125.0(6) . . ? O25 C97 C98 116.8(4) . . ? O26 C97 C98 118.1(4) . . ? C103 C98 C99 120.2(5) . . ? C103 C98 C97 119.3(5) . . ? C99 C98 C97 120.5 . . ? O27 C99 C100 117.9(4) . . ? O27 C99 C98 119.5(4) . . ? C100 C99 C98 122.5 . . ? C101 C100 C99 116.3(5) . . ? C100 C101 C102 124.1(9) . . ? C103 C102 C101 117.7(7) . . ? C98 C103 C102 119.1(8) . . ? O28 C104 O29 125.7(10) . . ? O28 C104 C105 115.8(10) . . ? O29 C104 C105 118.5(10) . . ? C110 C105 C106 120.3(10) . . ? C110 C105 C104 121.1(11) . . ? C106 C105 C104 118.6(10) . . ? O30 C106 C107 118.3(10) . . ? O30 C106 C105 122.8(10) . . ? C107 C106 C105 118.8(10) . . ? C106 C107 C108 118.8(9) . . ? C109 C108 C107 121.3(12) . . ? C108 C109 C110 119.6(13) . . ? C105 C110 C109 121.0(12) . . ? O42 C111 C112 107.5(16) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 2.317 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.166