Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof A K Powell' _publ_contact_author_address ; Inst fuer Anorganische Chemie Universitaet Karlsruhe Engesserstrasse Geb. 30.45 Karlsruhe D76128 ; _publ_contact_author_email powell@chemie.uni-karlsruhe.de _publ_contact_author_phone '+44 721 608 2135' _publ_section_title ; Iron(III) Activation Hits a [4+4] Macrocycle ; loop_ _publ_author_name _publ_author_address 'Ian J. Hewitt' ; Institut fur Anorganische Chemie Universitat Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Jin-Kui Tang' ; Institut fur Anorganische Chemie Universitat Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'N.T. Madhu' ; Institut fur Anorganische Chemie Universitat Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Bernd Pilawa' ; Institut fur Physik Universitat Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Christopher E. Anson' ; Institut fur Anorganische Chemie Universitat Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Sally Brooker' ; Department of Chemistry University of Otago P.O. Box 56 Dunedin New Zealand ; ; A.K.Powell ; ; Institut fur Anorganische Chemie Universitat Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; data_ian73_5 _database_code_depnum_ccdc_archive 'CCDC 253351' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H184 Fe4 N16 O28' _chemical_formula_weight 2330.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3789(15) _cell_length_b 14.7358(17) _cell_length_c 17.610(2) _cell_angle_alpha 92.718(10) _cell_angle_beta 110.611(9) _cell_angle_gamma 116.077(8) _cell_volume 2833.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9274 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 23.99 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.582 _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 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14083 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 24.04 _reflns_number_total 8243 _reflns_number_gt 6397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.05 (Stoe & Cie GmbH, 2000)' _computing_cell_refinement 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_data_reduction 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_structure_solution 'XS: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'XL: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'XP: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'XCIF: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The water molecules of crystallisation were ordered ; _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^)+(0.1092P)^2^+1.7267P] 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 SHELXL _refine_ls_extinction_coef 0.032(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8243 _refine_ls_number_parameters 703 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1701 _refine_ls_wR_factor_gt 0.1576 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.14853(5) 0.32181(4) 0.46348(3) 0.0313(2) Uani 1 1 d . . . Fe2 Fe 0.12978(6) 0.17576(4) 0.31662(3) 0.0334(2) Uani 1 1 d . . . O1 O 0.2520(3) 0.28568(19) 0.42467(17) 0.0331(6) Uani 1 1 d . . . C1 C 0.3812(4) 0.3367(4) 0.4542(3) 0.0514(12) Uani 1 1 d . . . H1A H 0.4162 0.4021 0.4924 0.077 Uiso 1 1 calc R . . H1B H 0.4033 0.3486 0.4079 0.077 Uiso 1 1 calc R . . H1C H 0.4117 0.2939 0.4824 0.077 Uiso 1 1 calc R . . O2 O 0.0293(3) 0.1920(2) 0.37349(19) 0.0387(7) Uani 1 1 d D . . H2 H -0.039(4) 0.170(4) 0.351(3) 0.046 Uiso 1 1 d D . . C2 C 0.3023(4) 0.5534(3) 0.5395(3) 0.0324(9) Uani 1 1 d . . . O3 O 0.2747(3) 0.4549(2) 0.54347(17) 0.0353(7) Uani 1 1 d . . . C3 C 0.3383(4) 0.6280(3) 0.6102(3) 0.0326(9) Uani 1 1 d . . . C4 C 0.3752(4) 0.7311(3) 0.6057(3) 0.0360(10) Uani 1 1 d . . . H4A H 0.3997 0.7800 0.6530 0.043 Uiso 1 1 calc R . . C5 C 0.3769(4) 0.7638(3) 0.5335(3) 0.0374(10) Uani 1 1 d . . . C6 C 0.3325(4) 0.6882(3) 0.4621(3) 0.0384(10) Uani 1 1 d . . . H6A H 0.3286 0.7077 0.4121 0.046 Uiso 1 1 calc R . . C7 C 0.2937(4) 0.5835(3) 0.4634(3) 0.0341(9) Uani 1 1 d . . . C8 C 0.4172(5) 0.8768(3) 0.5310(3) 0.0558(14) Uani 1 1 d . . . H8A H 0.3468 0.8866 0.5107 0.084 Uiso 1 1 calc R . . H8B H 0.4582 0.8949 0.4945 0.084 Uiso 1 1 calc R . . H8C H 0.4720 0.9204 0.5862 0.084 Uiso 1 1 calc R . . C9 C 0.2430(4) 0.5043(3) 0.3846(3) 0.0391(10) Uani 1 1 d . . . H9A H 0.2323 0.5366 0.3378 0.047 Uiso 1 1 calc R . . H9B H 0.3014 0.4810 0.3875 0.047 Uiso 1 1 calc R . . N1 N 0.1244(3) 0.4131(3) 0.3697(2) 0.0368(8) Uani 1 1 d D . . H1 H 0.104(5) 0.372(3) 0.325(3) 0.044 Uiso 1 1 d D . . C10 C 0.0271(5) 0.4375(3) 0.3614(3) 0.0445(11) Uani 1 1 d . . . H10A H -0.0136 0.4377 0.3037 0.053 Uiso 1 1 calc R . . H10B H 0.0623 0.5065 0.3957 0.053 Uiso 1 1 calc R . . C11 C -0.0643(5) 0.3600(4) 0.3875(3) 0.0527(12) Uani 1 1 d . . . H11A H -0.1198 0.3837 0.3915 0.063 Uiso 1 1 calc R . . H11B H -0.1118 0.2934 0.3470 0.063 Uiso 1 1 calc R . . N2 N 0.0051(4) 0.3497(3) 0.4700(2) 0.0459(9) Uani 1 1 d D . . H2A H 0.005(5) 0.411(3) 0.472(3) 0.055 Uiso 1 1 d D . . C12 C -0.0684(4) 0.2747(4) 0.5086(3) 0.0444(11) Uani 1 1 d . . . H12A H -0.0985 0.2038 0.4805 0.053 Uiso 1 1 calc R . . H12B H -0.1380 0.2835 0.5036 0.053 Uiso 1 1 calc R . . C13 C 0.0139(4) 0.2969(3) 0.5992(3) 0.0367(10) Uani 1 1 d . . . C14 C 0.1232(4) 0.2934(3) 0.6208(3) 0.0334(9) Uani 1 1 d . . . O4 O 0.1507(3) 0.26187(19) 0.56103(17) 0.0334(6) Uani 1 1 d . . . C15 C 0.2045(4) 0.3225(3) 0.7055(3) 0.0358(10) Uani 1 1 d . . . C16 C 0.1734(5) 0.3527(3) 0.7664(3) 0.0425(11) Uani 1 1 d . . . H16 H 0.2276 0.3720 0.8223 0.051 Uiso 1 1 calc R . . C17 C 0.0656(5) 0.3551(3) 0.7467(3) 0.0456(12) Uani 1 1 d . . . C18 C -0.0136(5) 0.3269(3) 0.6625(3) 0.0422(11) Uani 1 1 d . . . H18 H -0.0869 0.3280 0.6480 0.051 Uiso 1 1 calc R . . C19 C 0.0354(7) 0.3918(5) 0.8129(4) 0.0698(17) Uani 1 1 d . . . H19A H 0.1019 0.4128 0.8667 0.105 Uiso 1 1 calc R . . H19B H -0.0376 0.3362 0.8128 0.105 Uiso 1 1 calc R . . H19C H 0.0227 0.4499 0.8012 0.105 Uiso 1 1 calc R . . C20 C 0.3225(4) 0.3212(3) 0.7286(3) 0.0390(10) Uani 1 1 d . . . H20A H 0.3653 0.3386 0.7890 0.047 Uiso 1 1 calc R . . H20B H 0.3058 0.2518 0.7073 0.047 Uiso 1 1 calc R . . N3 N 0.4020(3) 0.3971(3) 0.6938(2) 0.0355(8) Uani 1 1 d D . . H3 H 0.360(4) 0.392(4) 0.645(2) 0.043 Uiso 1 1 d D . . C21 C 0.5027(4) 0.3797(3) 0.6942(3) 0.0419(10) Uani 1 1 d . . . H21A H 0.5452 0.4269 0.6659 0.050 Uiso 1 1 calc R . . H21B H 0.4684 0.3092 0.6629 0.050 Uiso 1 1 calc R . . C22 C 0.5944(4) 0.3953(3) 0.7811(3) 0.0429(11) Uani 1 1 d . . . H22A H 0.5519 0.3495 0.8101 0.051 Uiso 1 1 calc R . . H22B H 0.6531 0.3761 0.7765 0.051 Uiso 1 1 calc R . . N4 N 0.6600(4) 0.5028(3) 0.8304(2) 0.0403(9) Uani 1 1 d D . . H4 H 0.685(5) 0.504(4) 0.882(2) 0.048 Uiso 1 1 d D . . C23 C 0.7596(4) 0.5694(3) 0.8096(3) 0.0391(10) Uani 1 1 d . . . H23A H 0.7250 0.5778 0.7537 0.047 Uiso 1 1 calc R . . H23B H 0.8060 0.5344 0.8085 0.047 Uiso 1 1 calc R . . C24 C 0.8465(4) 0.6758(3) 0.8680(2) 0.0336(9) Uani 1 1 d . . . C25 C 0.9163(4) 0.7541(3) 0.8365(2) 0.0348(9) Uani 1 1 d . . . O5 O 0.8985(3) 0.7334(2) 0.75550(17) 0.0353(7) Uani 1 1 d . . . C26 C 1.0070(4) 0.8525(3) 0.8903(3) 0.0425(11) Uani 1 1 d . . . C27 C 1.0192(5) 0.8733(3) 0.9720(3) 0.0481(12) Uani 1 1 d . . . H27 H 1.0777 0.9389 1.0069 0.058 Uiso 1 1 calc R . . C28 C 0.9470(5) 0.7996(3) 1.0028(3) 0.0451(11) Uani 1 1 d . . . C29 C 0.8627(4) 0.7001(3) 0.9498(3) 0.0409(10) Uani 1 1 d . . . H29 H 0.8161 0.6486 0.9704 0.049 Uiso 1 1 calc R . . C30 C 0.9550(6) 0.8254(4) 1.0894(3) 0.0682(17) Uani 1 1 d . . . H30A H 1.0378 0.8525 1.1296 0.102 Uiso 1 1 calc R . . H30B H 0.9025 0.7636 1.1010 0.102 Uiso 1 1 calc R . . H30C H 0.9296 0.8766 1.0926 0.102 Uiso 1 1 calc R . . C31 C 1.0883(5) 0.9314(4) 0.8571(3) 0.0605(15) Uani 1 1 d . . . H31A H 1.1471 0.9944 0.9010 0.073 Uiso 1 1 calc R . . H31B H 1.1333 0.9040 0.8403 0.073 Uiso 1 1 calc R . . N5 N 1.0180(4) 0.9559(3) 0.7867(3) 0.0517(11) Uani 1 1 d D . . H5 H 0.970(5) 0.975(4) 0.804(4) 0.062 Uiso 1 1 d D . . C32 C 1.0880(5) 1.0371(3) 0.7511(3) 0.0531(13) Uani 1 1 d . . . H32A H 1.1504 1.0997 0.7946 0.064 Uiso 1 1 calc R . . H32B H 1.1275 1.0125 0.7252 0.064 Uiso 1 1 calc R . . C33 C 0.9986(5) 1.0586(3) 0.6880(3) 0.0540(13) Uani 1 1 d . . . H33A H 0.9748 1.0984 0.7161 0.065 Uiso 1 1 calc R . . H33B H 1.0366 1.1000 0.6549 0.065 Uiso 1 1 calc R . . N6 N 0.8888(4) 0.9612(3) 0.6323(3) 0.0481(10) Uani 1 1 d D . . H6 H 0.896(5) 0.948(4) 0.590(3) 0.058 Uiso 1 1 d D . . C34 C 0.7757(5) 0.9693(4) 0.6067(3) 0.0527(13) Uani 1 1 d . . . H34A H 0.7076 0.9057 0.5665 0.063 Uiso 1 1 calc R . . H34B H 0.7847 1.0264 0.5796 0.063 Uiso 1 1 calc R . . C35 C 0.7484(5) 0.9868(3) 0.6799(3) 0.0449(11) Uani 1 1 d . . . C36 C 0.7367(4) 0.9159(3) 0.7313(3) 0.0366(10) Uani 1 1 d . . . O6 O 0.7531(3) 0.8342(2) 0.71643(18) 0.0401(7) Uani 1 1 d . . . C37 C 0.7095(4) 0.9316(3) 0.7989(3) 0.0400(10) Uani 1 1 d . . . C38 C 0.6934(5) 1.0174(3) 0.8136(4) 0.0539(13) Uani 1 1 d . . . H38 H 0.6736 1.0269 0.8579 0.065 Uiso 1 1 calc R . . C39 C 0.7061(6) 1.0891(4) 0.7641(4) 0.0619(15) Uani 1 1 d . . . C40 C 0.7340(5) 1.0725(3) 0.6971(4) 0.0545(13) Uani 1 1 d . . . H40 H 0.7432 1.1196 0.6634 0.065 Uiso 1 1 calc R . . C41 C 0.6911(9) 1.1828(5) 0.7837(7) 0.108(3) Uani 1 1 d . . . H41A H 0.6261 1.1627 0.8017 0.163 Uiso 1 1 calc R . . H41B H 0.6718 1.2086 0.7344 0.163 Uiso 1 1 calc R . . H41C H 0.7659 1.2365 0.8272 0.163 Uiso 1 1 calc R . . C42 C 0.6997(4) 0.8597(3) 0.8572(3) 0.0425(11) Uani 1 1 d . . . H42A H 0.7608 0.8381 0.8657 0.051 Uiso 1 1 calc R . . H42B H 0.7166 0.8971 0.9110 0.051 Uiso 1 1 calc R . . N7 N 0.5764(3) 0.7659(3) 0.8243(2) 0.0391(8) Uani 1 1 d . . . C43 C 0.5567(5) 0.7059(4) 0.8876(3) 0.0466(11) Uani 1 1 d . . . H43A H 0.5335 0.7364 0.9240 0.056 Uiso 1 1 calc R . . H43B H 0.6298 0.7032 0.9214 0.056 Uiso 1 1 calc R . . C44 C 0.4528(5) 0.5979(3) 0.8357(3) 0.0457(11) Uani 1 1 d . . . H44A H 0.4699 0.5445 0.8572 0.055 Uiso 1 1 calc R . . H44B H 0.3763 0.5871 0.8365 0.055 Uiso 1 1 calc R . . N8 N 0.4461(3) 0.5948(2) 0.7478(2) 0.0360(8) Uani 1 1 d . . . C45 C 0.5607(4) 0.6876(3) 0.7596(3) 0.0367(10) Uani 1 1 d . . . H45A H 0.6288 0.6736 0.7782 0.047(13) Uiso 1 1 calc R . . H45B H 0.5538 0.7105 0.7081 0.046(13) Uiso 1 1 calc R . . C46 C 0.3343(4) 0.5979(3) 0.6907(3) 0.0352(9) Uani 1 1 d . . . H46A H 0.3232 0.6472 0.7207 0.042 Uiso 1 1 calc R . . H46B H 0.2636 0.5299 0.6768 0.042 Uiso 1 1 calc R . . O51 O 0.1220(5) 0.0680(3) 0.5395(3) 0.0842(15) Uani 1 1 d . . . O52 O 0.4094(5) 0.8366(4) 0.8212(3) 0.0800(13) Uani 1 1 d . . . O53A O 1.449(5) 1.158(3) 0.868(3) 0.29(2) Uiso 0.50 1 d P . . O53B O 1.417(2) 1.1629(15) 0.9008(14) 0.157(7) Uiso 0.50 1 d P . . C53A C 1.525(5) 1.176(3) 0.912(3) 0.203(15) Uiso 0.50 1 d P . . C53B C 1.350(7) 1.227(5) 0.916(4) 0.34(3) Uiso 0.50 1 d P . . O54 O 0.2398(8) 0.6783(6) 0.8612(5) 0.142(2) Uiso 1 1 d . . . C54 C 0.1569(17) 0.7182(13) 0.8698(11) 0.187(6) Uiso 1 1 d . . . O55A O 0.5356(11) 0.5864(8) 1.0437(7) 0.178(3) Uiso 1 1 d . . . O55B O 0.4439(13) 0.4667(11) 0.9836(9) 0.121(4) Uiso 0.50 1 d P . . O55C O 0.3316(17) 0.6301(15) 1.0058(11) 0.148(5) Uiso 0.50 1 d P . . C55A C 0.3656(14) 0.4745(10) 0.9831(8) 0.146(4) Uiso 1 1 d . . . C55B C 0.406(4) 0.584(3) 1.020(2) 0.201(13) Uiso 0.50 1 d P . . C55C C 0.294(3) 0.553(3) 0.985(2) 0.165(10) Uiso 0.50 1 d P . . O56A O 0.2310(10) -0.1153(9) 0.7207(8) 0.032(3) Uiso 0.25 1 d P . . O56B O 0.3365(15) 0.0863(12) 0.6796(10) 0.064(4) Uiso 0.25 1 d P . . O56C O 0.3930(19) 0.0081(15) 0.7670(12) 0.086(5) Uiso 0.25 1 d P . . O56D O 0.2183(18) -0.0603(14) 0.6438(12) 0.078(5) Uiso 0.25 1 d P . . C56A C 0.233(2) -0.0975(17) 0.6888(16) 0.050(5) Uiso 0.25 1 d P . . C56B C 0.3139(17) 0.0043(14) 0.6928(11) 0.041(4) Uiso 0.25 1 d P . . C56C C 0.281(2) 0.0040(17) 0.6129(14) 0.056(5) Uiso 0.25 1 d P . . C56D C 0.388(3) 0.082(2) 0.640(2) 0.085(8) Uiso 0.25 1 d P . . O57A O 0.871(3) 0.437(2) 0.9472(19) 0.160(10) Uiso 0.30 1 d P . . O57B O 0.917(10) 0.375(8) 1.000(7) 0.35(5) Uiso 0.20 1 d P . . C57 C 1.0000 0.5000 1.0000 0.229(11) Uiso 1 2 d S . . O58 O 0.5825(16) 0.9613(13) 0.9904(10) 0.141(5) Uiso 0.50 1 d P . . C58 C 0.550(3) 1.017(3) 0.949(2) 0.183(11) Uiso 0.50 1 d P . . 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 0.0333(4) 0.0261(3) 0.0321(3) 0.0047(2) 0.0123(3) 0.0138(2) Fe2 0.0388(4) 0.0216(3) 0.0325(3) 0.0031(2) 0.0147(3) 0.0093(2) O1 0.0312(16) 0.0254(13) 0.0355(15) 0.0009(11) 0.0125(12) 0.0096(11) C1 0.033(3) 0.048(3) 0.060(3) -0.005(2) 0.014(2) 0.015(2) O2 0.0325(17) 0.0319(15) 0.0405(17) 0.0042(12) 0.0128(14) 0.0090(13) C2 0.034(2) 0.0249(18) 0.037(2) 0.0067(16) 0.0145(18) 0.0133(16) O3 0.0435(18) 0.0253(13) 0.0344(15) 0.0064(11) 0.0130(13) 0.0172(12) C3 0.027(2) 0.0275(19) 0.037(2) 0.0030(16) 0.0103(17) 0.0104(16) C4 0.030(2) 0.0267(19) 0.041(2) 0.0003(17) 0.0070(18) 0.0128(16) C5 0.033(2) 0.026(2) 0.044(2) 0.0098(17) 0.0099(19) 0.0115(17) C6 0.035(3) 0.034(2) 0.043(2) 0.0134(18) 0.0143(19) 0.0149(18) C7 0.036(2) 0.0299(19) 0.038(2) 0.0099(17) 0.0163(19) 0.0163(17) C8 0.059(3) 0.028(2) 0.060(3) 0.012(2) 0.011(3) 0.016(2) C9 0.050(3) 0.034(2) 0.036(2) 0.0079(17) 0.019(2) 0.0218(19) N1 0.042(2) 0.0305(17) 0.0335(18) 0.0032(14) 0.0111(16) 0.0187(16) C10 0.046(3) 0.041(2) 0.045(3) 0.011(2) 0.011(2) 0.025(2) C11 0.046(3) 0.054(3) 0.058(3) 0.015(2) 0.016(2) 0.029(2) N2 0.047(3) 0.055(2) 0.048(2) 0.0216(19) 0.0247(19) 0.031(2) C12 0.033(3) 0.046(2) 0.053(3) 0.008(2) 0.016(2) 0.020(2) C13 0.036(3) 0.030(2) 0.047(2) 0.0142(18) 0.022(2) 0.0145(17) C14 0.036(3) 0.0192(17) 0.040(2) 0.0071(16) 0.0170(19) 0.0085(16) O4 0.0377(17) 0.0281(13) 0.0355(15) 0.0076(11) 0.0163(13) 0.0161(12) C15 0.037(3) 0.0228(18) 0.042(2) 0.0077(16) 0.0183(19) 0.0084(16) C16 0.053(3) 0.031(2) 0.039(2) 0.0108(18) 0.023(2) 0.014(2) C17 0.059(3) 0.038(2) 0.054(3) 0.019(2) 0.037(3) 0.025(2) C18 0.046(3) 0.037(2) 0.056(3) 0.017(2) 0.031(2) 0.023(2) C19 0.098(5) 0.074(4) 0.073(4) 0.029(3) 0.059(4) 0.052(4) C20 0.040(3) 0.030(2) 0.040(2) 0.0126(17) 0.015(2) 0.0113(18) N3 0.036(2) 0.0315(17) 0.0331(18) 0.0084(15) 0.0134(16) 0.0124(15) C21 0.038(3) 0.030(2) 0.050(3) 0.0031(18) 0.017(2) 0.0116(18) C22 0.039(3) 0.031(2) 0.053(3) 0.0108(19) 0.016(2) 0.0144(19) N4 0.039(2) 0.0339(18) 0.0367(19) 0.0074(16) 0.0139(17) 0.0104(16) C23 0.043(3) 0.031(2) 0.037(2) 0.0050(17) 0.015(2) 0.0144(18) C24 0.034(2) 0.031(2) 0.032(2) 0.0040(16) 0.0090(18) 0.0165(17) C25 0.038(3) 0.030(2) 0.031(2) 0.0037(16) 0.0096(18) 0.0159(18) O5 0.0444(18) 0.0272(13) 0.0304(14) 0.0053(11) 0.0154(13) 0.0145(12) C26 0.042(3) 0.034(2) 0.034(2) 0.0033(18) 0.008(2) 0.0108(19) C27 0.053(3) 0.033(2) 0.036(2) -0.0012(18) 0.005(2) 0.014(2) C28 0.055(3) 0.040(2) 0.030(2) 0.0029(18) 0.010(2) 0.022(2) C29 0.046(3) 0.039(2) 0.036(2) 0.0108(18) 0.014(2) 0.021(2) C30 0.094(5) 0.052(3) 0.040(3) 0.000(2) 0.022(3) 0.026(3) C31 0.051(3) 0.038(2) 0.051(3) 0.002(2) 0.009(2) -0.002(2) N5 0.054(3) 0.0327(19) 0.045(2) 0.0056(17) 0.020(2) 0.0031(18) C32 0.060(3) 0.028(2) 0.052(3) 0.003(2) 0.031(3) 0.000(2) C33 0.069(4) 0.025(2) 0.070(3) 0.012(2) 0.043(3) 0.014(2) N6 0.074(3) 0.0309(18) 0.048(2) 0.0108(17) 0.036(2) 0.0234(19) C34 0.071(4) 0.035(2) 0.049(3) 0.015(2) 0.020(3) 0.027(2) C35 0.049(3) 0.034(2) 0.046(3) 0.0070(19) 0.015(2) 0.019(2) C36 0.038(3) 0.0264(19) 0.038(2) 0.0030(16) 0.0096(19) 0.0146(17) O6 0.054(2) 0.0280(14) 0.0424(16) 0.0095(12) 0.0238(15) 0.0206(13) C37 0.034(3) 0.030(2) 0.047(2) -0.0009(18) 0.011(2) 0.0126(17) C38 0.054(3) 0.033(2) 0.080(4) 0.004(2) 0.036(3) 0.020(2) C39 0.060(4) 0.040(3) 0.097(4) 0.015(3) 0.041(3) 0.027(2) C40 0.052(3) 0.033(2) 0.077(4) 0.015(2) 0.022(3) 0.023(2) C41 0.153(8) 0.051(3) 0.195(9) 0.050(5) 0.124(8) 0.067(5) C42 0.037(3) 0.037(2) 0.038(2) -0.0035(18) 0.012(2) 0.0091(19) N7 0.040(2) 0.0343(18) 0.0374(19) 0.0042(15) 0.0162(17) 0.0144(16) C43 0.053(3) 0.046(2) 0.037(2) 0.008(2) 0.021(2) 0.020(2) C44 0.056(3) 0.041(2) 0.038(2) 0.0114(19) 0.019(2) 0.022(2) N8 0.040(2) 0.0319(17) 0.0329(18) 0.0074(14) 0.0139(16) 0.0163(15) C45 0.038(3) 0.033(2) 0.038(2) 0.0061(17) 0.0150(19) 0.0172(18) C46 0.038(3) 0.031(2) 0.035(2) 0.0039(17) 0.0130(19) 0.0165(17) O51 0.159(5) 0.056(2) 0.079(3) 0.032(2) 0.073(3) 0.066(3) O52 0.092(3) 0.083(3) 0.087(3) 0.019(2) 0.044(3) 0.055(3) _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 O3 1.958(3) . ? Fe1 O4 1.966(3) . ? Fe1 O1 1.986(3) . ? Fe1 O2 1.991(3) . ? Fe1 N2 2.170(4) . ? Fe1 N1 2.204(4) . ? Fe2 O6 1.911(3) 2_666 ? Fe2 O5 1.954(3) 2_666 ? Fe2 O2 2.019(3) . ? Fe2 O1 2.026(3) . ? Fe2 N5 2.178(4) 2_666 ? Fe2 N6 2.198(4) 2_666 ? O1 C1 1.419(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? O2 H2 0.76(4) . ? C2 O3 1.343(5) . ? C2 C3 1.405(6) . ? C2 C7 1.413(6) . ? C3 C4 1.392(6) . ? C3 C46 1.516(6) . ? C4 C5 1.386(6) . ? C4 H4A 0.9300 . ? C5 C6 1.391(6) . ? C5 C8 1.515(6) . ? C6 C7 1.399(6) . ? C6 H6A 0.9300 . ? C7 C9 1.495(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N1 1.481(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? N1 C10 1.459(6) . ? N1 H1 0.85(4) . ? C10 C11 1.493(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.481(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H2A 1.39(5) . ? N2 C12 1.494(6) . ? N2 H2A 0.91(4) . ? C12 C13 1.504(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.400(6) . ? C13 C18 1.401(6) . ? C14 O4 1.355(5) . ? C14 C15 1.407(6) . ? C15 C16 1.398(6) . ? C15 C20 1.495(7) . ? C16 C17 1.376(7) . ? C16 H16 0.9300 . ? C17 C18 1.393(7) . ? C17 C19 1.510(7) . ? C18 H18 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N3 1.495(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? N3 C21 1.476(6) . ? N3 H3 0.82(4) . ? C21 C22 1.515(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N4 1.464(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? N4 C23 1.448(6) . ? N4 H4 0.84(4) . ? C23 C24 1.506(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C29 1.384(6) . ? C24 C25 1.411(6) . ? C25 O5 1.357(5) . ? C25 C26 1.409(6) . ? O5 Fe2 1.954(3) 2_666 ? C26 C27 1.393(6) . ? C26 C31 1.509(7) . ? C27 C28 1.382(7) . ? C27 H27 0.9300 . ? C28 C29 1.403(6) . ? C28 C30 1.507(7) . ? C29 H29 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 N5 1.439(7) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? N5 C32 1.484(6) . ? N5 Fe2 2.178(4) 2_666 ? N5 H5 0.93(4) . ? C32 C33 1.483(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 N6 1.475(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? N6 C34 1.479(7) . ? N6 Fe2 2.198(4) 2_666 ? N6 H6 0.80(4) . ? C34 C35 1.499(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C40 1.393(7) . ? C35 C36 1.408(6) . ? C36 O6 1.346(5) . ? C36 C37 1.398(6) . ? O6 Fe2 1.911(3) 2_666 ? C37 C38 1.400(6) . ? C37 C42 1.506(7) . ? C38 C39 1.392(8) . ? C38 H38 0.9300 . ? C39 C40 1.398(8) . ? C39 C41 1.522(7) . ? C40 H40 0.9300 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N7 1.488(6) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? N7 C45 1.472(5) . ? N7 C43 1.479(6) . ? C43 C44 1.525(7) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 N8 1.516(6) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? N8 C45 1.473(6) . ? N8 C46 1.501(6) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? O53A O53B 0.85(5) . ? O53A C53A 0.95(6) . ? O53B C53A 1.31(5) . ? O53B C53B 1.63(7) . ? O54 C54 1.511(18) . ? O55A O55B 1.078(17) 2_667 ? O55A C55B 1.61(5) . ? O55A O55B 1.657(18) . ? O55B O55A 1.078(17) 2_667 ? O55B C55A 1.101(17) . ? O55B O55B 1.26(3) 2_667 ? O55C C55C 1.00(3) . ? O55C C55B 1.40(4) . ? C55A C55B 1.48(4) . ? C55A C55C 1.80(4) . ? C55B C55C 1.25(5) . ? O56A C56A 0.64(2) . ? O56A O56D 1.61(2) . ? O56A C56B 1.82(2) . ? O56B C56D 1.15(3) . ? O56B C56B 1.17(2) . ? O56B C56C 1.36(3) . ? O56C C56B 1.34(3) . ? O56C C56A 1.92(3) . ? O56D C56A 1.00(3) . ? O56D C56B 1.17(2) . ? O56D C56C 1.25(3) . ? C56A C56B 1.39(3) . ? C56B C56C 1.32(3) . ? C56B C56D 1.70(4) . ? C56C C56D 1.28(4) . ? O57A C57 1.44(3) . ? O57A O57B 1.49(11) . ? O57B C57 1.68(11) . ? C57 O57A 1.44(3) 2_767 ? C57 O57B 1.68(11) 2_767 ? O58 C58 1.24(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Fe1 O4 86.56(11) . . ? O3 Fe1 O1 99.62(12) . . ? O4 Fe1 O1 103.85(12) . . ? O3 Fe1 O2 173.55(12) . . ? O4 Fe1 O2 98.88(12) . . ? O1 Fe1 O2 75.80(12) . . ? O3 Fe1 N2 91.04(15) . . ? O4 Fe1 N2 87.85(13) . . ? O1 Fe1 N2 164.53(14) . . ? O2 Fe1 N2 92.61(15) . . ? O3 Fe1 N1 86.65(12) . . ? O4 Fe1 N1 163.05(13) . . ? O1 Fe1 N1 92.60(13) . . ? O2 Fe1 N1 89.01(13) . . ? N2 Fe1 N1 76.76(14) . . ? O6 Fe2 O5 95.30(12) 2_666 2_666 ? O6 Fe2 O2 169.28(13) 2_666 . ? O5 Fe2 O2 91.87(12) 2_666 . ? O6 Fe2 O1 96.68(12) 2_666 . ? O5 Fe2 O1 98.68(11) 2_666 . ? O2 Fe2 O1 74.31(12) . . ? O6 Fe2 N5 90.17(16) 2_666 2_666 ? O5 Fe2 N5 87.65(14) 2_666 2_666 ? O2 Fe2 N5 98.10(16) . 2_666 ? O1 Fe2 N5 170.17(13) . 2_666 ? O6 Fe2 N6 87.79(14) 2_666 2_666 ? O5 Fe2 N6 163.11(14) 2_666 2_666 ? O2 Fe2 N6 87.64(14) . 2_666 ? O1 Fe2 N6 97.43(13) . 2_666 ? N5 Fe2 N6 75.72(16) 2_666 2_666 ? C1 O1 Fe1 129.3(3) . . ? C1 O1 Fe2 126.2(3) . . ? Fe1 O1 Fe2 103.45(13) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Fe1 O2 Fe2 103.55(14) . . ? Fe1 O2 H2 127(4) . . ? Fe2 O2 H2 123(4) . . ? O3 C2 C3 120.9(4) . . ? O3 C2 C7 120.4(3) . . ? C3 C2 C7 118.7(3) . . ? C2 O3 Fe1 131.5(3) . . ? C4 C3 C2 119.4(4) . . ? C4 C3 C46 119.3(4) . . ? C2 C3 C46 121.3(3) . . ? C5 C4 C3 122.7(4) . . ? C5 C4 H4A 118.7 . . ? C3 C4 H4A 118.7 . . ? C4 C5 C6 117.5(4) . . ? C4 C5 C8 121.0(4) . . ? C6 C5 C8 121.3(4) . . ? C5 C6 C7 121.8(4) . . ? C5 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C6 C7 C2 119.6(4) . . ? C6 C7 C9 119.9(4) . . ? C2 C7 C9 120.5(3) . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C7 112.7(4) . . ? N1 C9 H9A 109.1 . . ? C7 C9 H9A 109.1 . . ? N1 C9 H9B 109.1 . . ? C7 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C10 N1 C9 114.5(3) . . ? C10 N1 Fe1 112.5(3) . . ? C9 N1 Fe1 110.7(3) . . ? C10 N1 H1 109(4) . . ? C9 N1 H1 106(3) . . ? Fe1 N1 H1 102(3) . . ? N1 C10 C11 111.1(4) . . ? N1 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N1 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N2 C11 C10 107.1(4) . . ? N2 C11 H11A 110.3 . . ? C10 C11 H11A 110.3 . . ? N2 C11 H11B 110.3 . . ? C10 C11 H11B 110.3 . . ? H11A C11 H11B 108.6 . . ? N2 C11 H2A 36.6(16) . . ? C10 C11 H2A 93(2) . . ? H11A C11 H2A 84.7 . . ? H11B C11 H2A 145.7 . . ? C11 N2 C12 116.5(4) . . ? C11 N2 Fe1 109.2(3) . . ? C12 N2 Fe1 112.7(3) . . ? C11 N2 H2A 67(3) . . ? C12 N2 H2A 116(4) . . ? Fe1 N2 H2A 126(4) . . ? N2 C12 C13 107.5(4) . . ? N2 C12 H12A 110.2 . . ? C13 C12 H12A 110.2 . . ? N2 C12 H12B 110.2 . . ? C13 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? C14 C13 C18 119.3(4) . . ? C14 C13 C12 119.8(4) . . ? C18 C13 C12 120.9(4) . . ? O4 C14 C13 120.6(4) . . ? O4 C14 C15 119.9(4) . . ? C13 C14 C15 119.4(4) . . ? C14 O4 Fe1 123.1(2) . . ? C16 C15 C14 119.2(4) . . ? C16 C15 C20 121.3(4) . . ? C14 C15 C20 119.5(4) . . ? C17 C16 C15 122.4(4) . . ? C17 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C16 C17 C18 117.8(4) . . ? C16 C17 C19 121.8(5) . . ? C18 C17 C19 120.3(5) . . ? C17 C18 C13 121.9(5) . . ? C17 C18 H18 119.0 . . ? C13 C18 H18 119.0 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C15 111.2(3) . . ? N3 C20 H20A 109.4 . . ? C15 C20 H20A 109.4 . . ? N3 C20 H20B 109.4 . . ? C15 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C21 N3 C20 113.5(3) . . ? C21 N3 H3 107(4) . . ? C20 N3 H3 109(4) . . ? N3 C21 C22 113.6(4) . . ? N3 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N3 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? N4 C22 C21 112.7(4) . . ? N4 C22 H22A 109.1 . . ? C21 C22 H22A 109.1 . . ? N4 C22 H22B 109.1 . . ? C21 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? C23 N4 C22 112.0(4) . . ? C23 N4 H4 111(4) . . ? C22 N4 H4 110(4) . . ? N4 C23 C24 115.5(4) . . ? N4 C23 H23A 108.4 . . ? C24 C23 H23A 108.4 . . ? N4 C23 H23B 108.4 . . ? C24 C23 H23B 108.4 . . ? H23A C23 H23B 107.5 . . ? C29 C24 C25 118.8(4) . . ? C29 C24 C23 124.1(4) . . ? C25 C24 C23 117.1(4) . . ? O5 C25 C26 120.4(4) . . ? O5 C25 C24 119.9(3) . . ? C26 C25 C24 119.7(4) . . ? C25 O5 Fe2 120.8(2) . 2_666 ? C27 C26 C25 119.1(4) . . ? C27 C26 C31 122.4(4) . . ? C25 C26 C31 118.5(4) . . ? C28 C27 C26 122.1(4) . . ? C28 C27 H27 118.9 . . ? C26 C27 H27 118.9 . . ? C27 C28 C29 117.7(4) . . ? C27 C28 C30 121.5(4) . . ? C29 C28 C30 120.7(5) . . ? C24 C29 C28 122.3(4) . . ? C24 C29 H29 118.8 . . ? C28 C29 H29 118.8 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 C26 111.3(5) . . ? N5 C31 H31A 109.4 . . ? C26 C31 H31A 109.4 . . ? N5 C31 H31B 109.4 . . ? C26 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 N5 C32 116.6(4) . . ? C31 N5 Fe2 116.1(3) . 2_666 ? C32 N5 Fe2 107.7(3) . 2_666 ? C31 N5 H5 106(4) . . ? C32 N5 H5 111(4) . . ? Fe2 N5 H5 98(4) 2_666 . ? C33 C32 N5 106.6(4) . . ? C33 C32 H32A 110.4 . . ? N5 C32 H32A 110.4 . . ? C33 C32 H32B 110.4 . . ? N5 C32 H32B 110.4 . . ? H32A C32 H32B 108.6 . . ? N6 C33 C32 111.3(4) . . ? N6 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? N6 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C33 N6 C34 112.6(4) . . ? C33 N6 Fe2 113.0(3) . 2_666 ? C34 N6 Fe2 111.8(3) . 2_666 ? C33 N6 H6 109(4) . . ? C34 N6 H6 107(4) . . ? Fe2 N6 H6 103(4) 2_666 . ? N6 C34 C35 111.7(4) . . ? N6 C34 H34A 109.3 . . ? C35 C34 H34A 109.3 . . ? N6 C34 H34B 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 107.9 . . ? C40 C35 C36 119.8(5) . . ? C40 C35 C34 120.5(4) . . ? C36 C35 C34 119.7(4) . . ? O6 C36 C37 120.0(4) . . ? O6 C36 C35 120.4(4) . . ? C37 C36 C35 119.6(4) . . ? C36 O6 Fe2 130.6(3) . 2_666 ? C36 C37 C38 119.1(4) . . ? C36 C37 C42 121.6(4) . . ? C38 C37 C42 119.3(4) . . ? C39 C38 C37 122.1(5) . . ? C39 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? C38 C39 C40 118.0(4) . . ? C38 C39 C41 120.4(6) . . ? C40 C39 C41 121.7(6) . . ? C35 C40 C39 121.3(5) . . ? C35 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N7 C42 C37 112.2(4) . . ? N7 C42 H42A 109.2 . . ? C37 C42 H42A 109.2 . . ? N7 C42 H42B 109.2 . . ? C37 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C45 N7 C43 101.2(3) . . ? C45 N7 C42 112.2(4) . . ? C43 N7 C42 112.8(3) . . ? N7 C43 C44 103.7(3) . . ? N7 C43 H43A 111.0 . . ? C44 C43 H43A 111.0 . . ? N7 C43 H43B 111.0 . . ? C44 C43 H43B 111.0 . . ? H43A C43 H43B 109.0 . . ? N8 C44 C43 105.5(3) . . ? N8 C44 H44A 110.6 . . ? C43 C44 H44A 110.6 . . ? N8 C44 H44B 110.6 . . ? C43 C44 H44B 110.6 . . ? H44A C44 H44B 108.8 . . ? C45 N8 C46 112.7(3) . . ? C45 N8 C44 103.1(3) . . ? C46 N8 C44 111.0(3) . . ? N7 C45 N8 103.8(3) . . ? N7 C45 H45A 111.0 . . ? N8 C45 H45A 111.0 . . ? N7 C45 H45B 111.0 . . ? N8 C45 H45B 111.0 . . ? H45A C45 H45B 109.0 . . ? N8 C46 C3 114.7(3) . . ? N8 C46 H46A 108.6 . . ? C3 C46 H46A 108.6 . . ? N8 C46 H46B 108.6 . . ? C3 C46 H46B 108.6 . . ? H46A C46 H46B 107.6 . . ? O53B O53A C53A 94(6) . . ? O53A O53B C53A 46(4) . . ? O53A O53B C53B 136(5) . . ? C53A O53B C53B 141(4) . . ? O53A C53A O53B 40(4) . . ? O55B O55A C55B 129(2) 2_667 . ? O55B O55A O55B 49.6(14) 2_667 . ? C55B O55A O55B 81.3(16) . . ? O55A O55B C55A 141.0(18) 2_667 . ? O55A O55B O55B 90(2) 2_667 2_667 ? C55A O55B O55B 129(2) . 2_667 ? O55A O55B O55A 130.4(14) 2_667 . ? C55A O55B O55A 88.5(15) . . ? O55B O55B O55A 40.6(11) 2_667 . ? C55C O55C C55B 60(2) . . ? O55B C55A C55B 110(2) . . ? O55B C55A C55C 150.7(19) . . ? C55B C55A C55C 43.4(19) . . ? C55C C55B O55C 44(2) . . ? C55C C55B C55A 82(3) . . ? O55C C55B C55A 126(3) . . ? C55C C55B O55A 160(4) . . ? O55C C55B O55A 154(3) . . ? C55A C55B O55A 79(2) . . ? O55C C55C C55B 76(3) . . ? O55C C55C C55A 130(3) . . ? C55B C55C C55A 55(2) . . ? C56A O56A O56D 12(2) . . ? C56A O56A C56B 39(2) . . ? O56D O56A C56B 39.1(9) . . ? C56D O56B C56B 95(2) . . ? C56D O56B C56C 60.3(19) . . ? C56B O56B C56C 62.2(15) . . ? C56B O56C C56A 46.4(13) . . ? C56A O56D C56B 80(2) . . ? C56A O56D C56C 137(3) . . ? C56B O56D C56C 66.0(17) . . ? C56A O56D O56A 7.7(15) . . ? C56B O56D O56A 80.5(15) . . ? C56C O56D O56A 142(2) . . ? O56A C56A O56D 160(4) . . ? O56A C56A C56B 124(3) . . ? O56D C56A C56B 55.5(18) . . ? O56A C56A O56C 83(3) . . ? O56D C56A O56C 100(2) . . ? C56B C56A O56C 44.2(11) . . ? O56D C56B O56B 112(2) . . ? O56D C56B C56C 60.0(16) . . ? O56B C56B C56C 66.3(15) . . ? O56D C56B O56C 134(2) . . ? O56B C56B O56C 113.1(18) . . ? C56C C56B O56C 152(2) . . ? O56D C56B C56A 44.7(13) . . ? O56B C56B C56A 153(2) . . ? C56C C56B C56A 101.2(19) . . ? O56C C56B C56A 89.4(17) . . ? O56D C56B C56D 107.9(19) . . ? O56B C56B C56D 42.4(14) . . ? C56C C56B C56D 48.0(15) . . ? O56C C56B C56D 111.5(19) . . ? C56A C56B C56D 144.2(19) . . ? O56D C56B O56A 60.4(13) . . ? O56B C56B O56A 156.2(17) . . ? C56C C56B O56A 118.0(15) . . ? O56C C56B O56A 74.5(12) . . ? C56A C56B O56A 16.8(11) . . ? C56D C56B O56A 158.3(16) . . ? O56D C56C C56D 136(3) . . ? O56D C56C C56B 54.0(14) . . ? C56D C56C C56B 82(2) . . ? O56D C56C O56B 95.2(18) . . ? C56D C56C O56B 51.6(17) . . ? C56B C56C O56B 51.5(12) . . ? O56B C56D C56C 68(2) . . ? O56B C56D C56B 43.1(14) . . ? C56C C56D C56B 50.0(16) . . ? C57 O57A O57B 70(5) . . ? O57A O57B C57 54(4) . . ? O57A C57 O57A 180.000(8) 2_767 . ? O57A C57 O57B 123(4) 2_767 . ? O57A C57 O57B 57(4) . . ? O57A C57 O57B 57(4) 2_767 2_767 ? O57A C57 O57B 123(4) . 2_767 ? O57B C57 O57B 180.00(4) . 2_767 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O56A 0.76(4) 2.15(4) 2.907(12) 175(6) 2_556 O2 H2 O56D 0.76(4) 2.26(5) 2.90(2) 143(5) 2_556 N1 H1 O5 0.85(4) 2.03(4) 2.847(4) 160(5) 2_666 N3 H3 O3 0.82(4) 2.24(4) 2.991(5) 152(4) . N6 H6 O51 0.80(4) 2.20(4) 2.979(6) 162(6) 2_666 _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 24.04 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.664 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.084 data_femac _database_code_depnum_ccdc_archive 'CCDC 253352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H179 Cl Fe4 N16 O27' _chemical_formula_weight 2320.46 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' Cl Cl 0.1484 0.1585 '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 14.250(3) _cell_length_b 14.350(3) _cell_length_c 15.263(3) _cell_angle_alpha 73.057(14) _cell_angle_beta 71.696(13) _cell_angle_gamma 83.434(15) _cell_volume 2833.8(9) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13449 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 26.41 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.937 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_process_details 'XPREP: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18617 _diffrn_reflns_av_R_equivalents 0.1063 _diffrn_reflns_av_sigmaI/netI 0.1312 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.03 _reflns_number_total 11273 _reflns_number_gt 5597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.05 (Stoe & Cie GmbH, 2000)' _computing_cell_refinement 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_data_reduction 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1543P)^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 SHELXL _refine_ls_extinction_coef 0.059(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11273 _refine_ls_number_parameters 749 _refine_ls_number_restraints 121 _refine_ls_R_factor_all 0.1744 _refine_ls_R_factor_gt 0.0956 _refine_ls_wR_factor_ref 0.2877 _refine_ls_wR_factor_gt 0.2301 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.21915(7) 0.58521(7) 0.64393(7) 0.0454(3) Uani 1 1 d . . . Fe2 Fe 0.23470(7) 0.76151(7) 0.45775(7) 0.0462(3) Uani 1 1 d . . . O1 O 0.2916(3) 0.6262(3) 0.5048(3) 0.0437(10) Uani 1 1 d . . . C1 C 0.3782(6) 0.5832(6) 0.4526(6) 0.0576(19) Uani 1 1 d . . . H1A H 0.3972 0.5238 0.4954 0.086 Uiso 1 1 calc R . . H1B H 0.4322 0.6294 0.4268 0.086 Uiso 1 1 calc R . . H1C H 0.3648 0.5669 0.3997 0.086 Uiso 1 1 calc R . . O2 O 0.1457(4) 0.7051(4) 0.5920(4) 0.0505(11) Uani 1 1 d D . . H2 H 0.092(4) 0.732(5) 0.617(6) 0.061 Uiso 1 1 d D . . O3 O 0.3095(3) 0.4778(3) 0.6810(3) 0.0486(11) Uani 1 1 d . . . C2 C 0.3695(5) 0.4711(6) 0.7369(6) 0.0532(18) Uani 1 1 d . . . C3 C 0.3721(5) 0.3856(5) 0.8096(6) 0.0506(17) Uani 1 1 d . . . C4 C 0.4382(6) 0.3795(6) 0.8623(6) 0.060(2) Uani 1 1 d . . . H4 H 0.4424 0.3209 0.9101 0.072 Uiso 1 1 calc R . . C5 C 0.4996(6) 0.4581(6) 0.8468(7) 0.067(2) Uani 1 1 d . . . C6 C 0.5723(8) 0.4474(7) 0.9034(8) 0.083(3) Uani 1 1 d . . . H6A H 0.5686 0.3818 0.9473 0.124 Uiso 1 1 calc R . . H6B H 0.5559 0.4957 0.9403 0.124 Uiso 1 1 calc R . . H6C H 0.6394 0.4578 0.8593 0.124 Uiso 1 1 calc R . . C7 C 0.4883(6) 0.5411(6) 0.7797(6) 0.058(2) Uani 1 1 d . . . H7 H 0.5260 0.5955 0.7707 0.070 Uiso 1 1 calc R . . C8 C 0.4251(6) 0.5525(6) 0.7227(6) 0.0539(17) Uani 1 1 d . . . C9 C 0.4122(5) 0.6476(6) 0.6546(6) 0.0550(18) Uani 1 1 d . . . H9A H 0.4525 0.6970 0.6590 0.066 Uiso 1 1 calc R . . H9B H 0.4362 0.6411 0.5883 0.066 Uiso 1 1 calc R . . N1 N 0.3069(4) 0.6809(4) 0.6758(4) 0.0467(13) Uani 1 1 d D . . H1 H 0.299(6) 0.736(4) 0.638(5) 0.056 Uiso 1 1 d D . . C10 C 0.2612(6) 0.6944(6) 0.7737(5) 0.0535(17) Uani 1 1 d . . . H10A H 0.2698 0.7623 0.7726 0.064 Uiso 1 1 calc R . . H10B H 0.2946 0.6502 0.8187 0.064 Uiso 1 1 calc R . . C11 C 0.1519(6) 0.6725(6) 0.8078(6) 0.0576(18) Uani 1 1 d . . . H11A H 0.1240 0.6698 0.8766 0.069 Uiso 1 1 calc R . . H11B H 0.1158 0.7242 0.7711 0.069 Uiso 1 1 calc R . . N2 N 0.1415(5) 0.5777(4) 0.7927(4) 0.0496(14) Uani 1 1 d D . . H2A H 0.167(6) 0.537(5) 0.835(5) 0.060 Uiso 1 1 d D . . C12 C 0.0383(5) 0.5432(5) 0.8234(6) 0.0530(17) Uani 1 1 d . . . H12A H 0.0015 0.5844 0.7801 0.064 Uiso 1 1 calc R . . H12B H 0.0038 0.5477 0.8893 0.064 Uiso 1 1 calc R . . C13 C 0.0423(5) 0.4388(5) 0.8198(6) 0.0523(17) Uani 1 1 d . . . C14 C 0.0910(5) 0.4173(5) 0.7303(5) 0.0488(16) Uani 1 1 d . . . O4 O 0.1268(3) 0.4897(3) 0.6505(3) 0.0465(11) Uani 1 1 d . . . C15 C 0.1033(5) 0.3186(5) 0.7286(5) 0.0461(15) Uani 1 1 d . . . C16 C 0.0663(6) 0.2450(6) 0.8126(6) 0.0585(19) Uani 1 1 d . . . H16 H 0.0741 0.1791 0.8099 0.070 Uiso 1 1 calc R . . C17 C 0.0186(6) 0.2647(6) 0.8995(6) 0.0591(19) Uani 1 1 d . . . C18 C -0.0149(7) 0.1819(7) 0.9906(7) 0.081(3) Uani 1 1 d . . . H18A H -0.0471 0.2089 1.0450 0.122 Uiso 1 1 calc R . . H18B H 0.0426 0.1415 1.0021 0.122 Uiso 1 1 calc R . . H18C H -0.0617 0.1419 0.9831 0.122 Uiso 1 1 calc R . . C19 C 0.0092(5) 0.3622(6) 0.9017(6) 0.0545(18) Uani 1 1 d . . . H19 H -0.0209 0.3768 0.9614 0.065 Uiso 1 1 calc R . . C20 C 0.1642(5) 0.2958(6) 0.6379(6) 0.0517(17) Uani 1 1 d . . . H20A H 0.1568 0.2264 0.6431 0.062 Uiso 1 1 calc R . . H20B H 0.1402 0.3361 0.5841 0.062 Uiso 1 1 calc R . . N3 N 0.2705(4) 0.3150(4) 0.6176(4) 0.0463(13) Uani 1 1 d D . . H3 H 0.270(6) 0.364(4) 0.638(6) 0.056 Uiso 1 1 d D . . C21 C 0.3324(6) 0.3099(6) 0.5199(6) 0.0579(18) Uani 1 1 d . . . H21A H 0.4003 0.3295 0.5093 0.069 Uiso 1 1 calc R . . H21B H 0.3052 0.3572 0.4717 0.069 Uiso 1 1 calc R . . C22 C 0.3369(6) 0.2098(7) 0.5048(7) 0.068(2) Uani 1 1 d . . . H22A H 0.2688 0.1899 0.5168 0.081 Uiso 1 1 calc R . . H22B H 0.3733 0.2137 0.4370 0.081 Uiso 1 1 calc R . . N4 N 0.3850(5) 0.1343(5) 0.5667(6) 0.0676(19) Uani 1 1 d . . . H4A H 0.3684 0.0735 0.5684 0.081 Uiso 0.50 1 calc PR . . H4B H 0.3632 0.1407 0.6281 0.081 Uiso 0.50 1 calc PR . . C23 C 0.4938(6) 0.1439(6) 0.5292(6) 0.0597(19) Uani 1 1 d . . . H23A H 0.5107 0.2065 0.5349 0.072 Uiso 1 1 calc R . . H23B H 0.5146 0.1471 0.4601 0.072 Uiso 1 1 calc R . . C24 C 0.5529(6) 0.0637(6) 0.5779(6) 0.0572(18) Uani 1 1 d . . . C25 C 0.6544(6) 0.0781(6) 0.5559(6) 0.0544(18) Uani 1 1 d . . . O5 O 0.6934(4) 0.1624(4) 0.4969(4) 0.0570(13) Uani 1 1 d . . . C26 C 0.7155(6) 0.0032(6) 0.5934(7) 0.065(2) Uani 1 1 d . . . C27 C 0.6740(6) -0.0798(6) 0.6620(8) 0.071(2) Uani 1 1 d . . . H27 H 0.7153 -0.1271 0.6912 0.086 Uiso 1 1 calc R . . C28 C 0.5704(7) -0.0957(6) 0.6899(7) 0.066(2) Uani 1 1 d . . . C29 C 0.5258(9) -0.1830(8) 0.7701(9) 0.094(3) Uani 1 1 d . . . H29A H 0.5786 -0.2256 0.7897 0.140 Uiso 1 1 calc R . . H29B H 0.4875 -0.2189 0.7479 0.140 Uiso 1 1 calc R . . H29C H 0.4822 -0.1613 0.8247 0.140 Uiso 1 1 calc R . . C30 C 0.5128(6) -0.0225(6) 0.6464(7) 0.064(2) Uani 1 1 d . . . H30 H 0.4436 -0.0313 0.6638 0.077 Uiso 1 1 calc R . . C31 C 0.8247(6) 0.0187(7) 0.5614(8) 0.075(3) Uani 1 1 d . . . H31A H 0.8585 -0.0401 0.5919 0.090 Uiso 1 1 calc R . . H31B H 0.8507 0.0297 0.4910 0.090 Uiso 1 1 calc R . . N5 N 0.8449(5) 0.1026(5) 0.5875(6) 0.070(2) Uani 1 1 d . . . H5 H 0.8171 0.0853 0.6537 0.084 Uiso 1 1 calc R . . C32 C 0.9445(7) 0.1236(7) 0.5765(8) 0.074(2) Uani 1 1 d . . . H32A H 0.9813 0.1447 0.5075 0.089 Uiso 1 1 calc R . . H32B H 0.9777 0.0640 0.6065 0.089 Uiso 1 1 calc R . . C33 C 0.9451(6) 0.2022(6) 0.6225(6) 0.061(2) Uani 1 1 d . . . H33A H 1.0129 0.2267 0.6026 0.073 Uiso 1 1 calc R . . H33B H 0.9239 0.1758 0.6932 0.073 Uiso 1 1 calc R . . N6 N 0.8763(5) 0.2835(5) 0.5930(5) 0.0510(14) Uani 1 1 d D . . H6 H 0.911(5) 0.327(5) 0.542(4) 0.061 Uiso 1 1 d D . . C34 C 0.8288(6) 0.3362(5) 0.6676(6) 0.0543(18) Uani 1 1 d . . . H34A H 0.7900 0.3929 0.6409 0.065 Uiso 1 1 calc R . . H34B H 0.8809 0.3610 0.6846 0.065 Uiso 1 1 calc R . . C35 C 0.7619(5) 0.2724(5) 0.7567(5) 0.0502(16) Uani 1 1 d . . . C36 C 0.6880(5) 0.2159(5) 0.7536(5) 0.0464(15) Uani 1 1 d . . . O6 O 0.6766(4) 0.2162(4) 0.6692(3) 0.0504(11) Uani 1 1 d . . . C37 C 0.6267(5) 0.1589(5) 0.8388(5) 0.0472(16) Uani 1 1 d . . . C38 C 0.6362(6) 0.1644(6) 0.9260(5) 0.0534(17) Uani 1 1 d . . . H38 H 0.5922 0.1282 0.9838 0.064 Uiso 1 1 calc R . . C39 C 0.7055(6) 0.2193(6) 0.9325(5) 0.0559(18) Uani 1 1 d . . . C40 C 0.7129(7) 0.2271(8) 1.0277(6) 0.071(2) Uani 1 1 d . . . H40A H 0.6627 0.1866 1.0806 0.107 Uiso 1 1 calc R . . H40B H 0.7020 0.2951 1.0300 0.107 Uiso 1 1 calc R . . H40C H 0.7788 0.2045 1.0336 0.107 Uiso 1 1 calc R . . C41 C 0.7701(5) 0.2716(5) 0.8467(5) 0.0511(16) Uani 1 1 d . . . H41 H 0.8208 0.3076 0.8490 0.061 Uiso 1 1 calc R . . C42 C 0.5526(5) 0.0897(5) 0.8396(6) 0.0489(16) Uani 1 1 d . . . H42A H 0.5767 0.0681 0.7802 0.059 Uiso 1 1 calc R . . H42B H 0.5479 0.0313 0.8946 0.059 Uiso 1 1 calc R . . N7 N 0.4532(4) 0.1360(4) 0.8465(4) 0.0474(13) Uani 1 1 d . . . C43 C 0.3752(6) 0.0682(6) 0.8616(6) 0.0560(18) Uani 1 1 d . . . H43A H 0.3477 0.0347 0.9305 0.067 Uiso 1 1 calc R . . H43B H 0.4015 0.0186 0.8259 0.067 Uiso 1 1 calc R . . C44 C 0.2962(6) 0.1338(6) 0.8228(6) 0.0593(19) Uani 1 1 d . . . H44A H 0.2779 0.1075 0.7774 0.071 Uiso 1 1 calc R . . H44B H 0.2361 0.1391 0.8758 0.071 Uiso 1 1 calc R . . C45 C 0.4495(5) 0.2088(5) 0.7562(5) 0.0483(16) Uani 1 1 d . . . H45A H 0.4872 0.2672 0.7448 0.058 Uiso 1 1 calc R . . H45B H 0.4765 0.1809 0.7008 0.058 Uiso 1 1 calc R . . N8 N 0.3438(4) 0.2327(4) 0.7721(4) 0.0487(13) Uani 1 1 d . . . C46 C 0.3054(5) 0.3018(5) 0.8337(5) 0.0514(17) Uani 1 1 d . . . H46A H 0.2957 0.2650 0.9016 0.062 Uiso 1 1 calc R . . H46B H 0.2399 0.3283 0.8269 0.062 Uiso 1 1 calc R . . O11 O 1.0049(4) 0.4367(4) 0.4484(4) 0.0625(14) Uani 1 1 d D . . H111 H 1.0000 0.5000 0.5000 0.094 Uiso 1 2 d S . . H112 H 1.062(5) 0.422(8) 0.408(6) 0.094 Uiso 1 1 d D . . H113 H 0.965(7) 0.463(7) 0.413(7) 0.094 Uiso 1 1 d D . . Cl1 Cl -0.0453(12) 0.8182(9) 0.7063(10) 0.084(3) Uani 0.50 1 d PU A 1 O12 O -0.055(3) 0.792(2) 0.687(2) 0.098(10) Uani 0.50 1 d PU B 2 O13 O 0.6338(7) -0.1508(7) 0.9491(6) 0.118(3) Uani 1 1 d . . . O14 O 0.1739(5) 0.4582(5) 0.9756(4) 0.0803(18) Uani 1 1 d . . . C54 C 0.2350(9) 0.4937(9) 1.0158(9) 0.097(3) Uani 1 1 d . . . O15 O -0.1556(7) 0.7574(7) 0.8917(7) 0.101(3) Uani 1 1 d DU . . C55A C -0.174(3) 0.7092(18) 0.9322(19) 0.164(12) Uani 0.70 1 d PDU . . C55B C -0.245(5) 0.695(5) 0.895(5) 0.144(13) Uiso 0.30 1 d PDU . . O16A O 1.2599(11) -0.0665(10) 0.6584(11) 0.115(4) Uani 0.65 1 d PU . . O16B O 1.1121(19) 0.0372(19) 0.7187(19) 0.108(7) Uiso 0.35 1 d PU . . C56A C 1.1736(16) -0.0442(13) 0.7193(18) 0.104(6) Uani 0.65 1 d PU . . C56B C 1.162(4) -0.014(4) 0.671(4) 0.128(12) Uiso 0.35 1 d PU . . O17A O 0.8079(11) -0.0290(9) 0.8007(10) 0.108(4) Uani 0.65 1 d PU . . O17B O 0.925(3) -0.018(2) 0.808(3) 0.100(8) Uiso 0.25 1 d PU . . O17C O 0.817(7) -0.087(7) 0.943(7) 0.123(17) Uiso 0.10 1 d PU . . C57A C 0.861(3) 0.015(3) 0.880(3) 0.160(13) Uani 0.65 1 d PU . . C57B C 0.861(6) -0.003(5) 0.862(5) 0.100(10) Uiso 0.35 1 d PU . . O18A O 1.147(2) 0.312(3) 0.377(3) 0.126(10) Uani 0.60 1 d PU . . O18B O 1.175(3) 0.339(4) 0.369(4) 0.117(11) Uani 0.40 1 d PU . . C58A C 1.2254(18) 0.380(2) 0.2896(19) 0.098(6) Uani 0.60 1 d PU . . C58B C 1.207(6) 0.430(6) 0.268(6) 0.112(14) Uiso 0.20 1 d PU . . C58C C 1.277(5) 0.360(5) 0.269(5) 0.087(13) Uiso 0.20 1 d PU . . 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 0.0416(5) 0.0530(6) 0.0427(6) -0.0196(4) -0.0101(5) 0.0057(4) Fe2 0.0414(5) 0.0522(6) 0.0467(6) -0.0186(4) -0.0123(5) 0.0032(4) O1 0.041(2) 0.049(3) 0.042(3) -0.017(2) -0.011(2) 0.0044(19) C1 0.053(4) 0.066(5) 0.055(5) -0.026(4) -0.014(4) 0.015(3) O2 0.041(3) 0.059(3) 0.049(3) -0.022(2) -0.006(2) 0.009(2) O3 0.043(3) 0.062(3) 0.050(3) -0.026(2) -0.018(2) 0.003(2) C2 0.039(4) 0.066(5) 0.065(5) -0.037(4) -0.016(4) 0.010(3) C3 0.047(4) 0.053(4) 0.057(4) -0.024(3) -0.019(4) 0.012(3) C4 0.061(5) 0.065(5) 0.065(5) -0.027(4) -0.030(4) 0.020(4) C5 0.057(5) 0.074(5) 0.092(7) -0.043(5) -0.039(5) 0.014(4) C6 0.085(7) 0.074(6) 0.121(9) -0.044(6) -0.066(7) 0.019(5) C7 0.054(4) 0.056(4) 0.081(6) -0.033(4) -0.035(4) 0.011(3) C8 0.045(4) 0.066(4) 0.057(5) -0.031(4) -0.013(4) 0.010(3) C9 0.044(4) 0.061(4) 0.062(5) -0.025(4) -0.012(4) 0.004(3) N1 0.043(3) 0.050(3) 0.050(3) -0.022(3) -0.014(3) 0.006(2) C10 0.060(4) 0.060(4) 0.041(4) -0.021(3) -0.014(4) 0.011(3) C11 0.053(4) 0.069(5) 0.049(4) -0.028(4) -0.004(4) 0.006(3) N2 0.051(3) 0.055(3) 0.045(3) -0.020(3) -0.014(3) 0.005(3) C12 0.045(4) 0.060(4) 0.050(4) -0.021(3) -0.005(4) 0.001(3) C13 0.041(4) 0.060(4) 0.051(4) -0.020(3) -0.005(3) 0.006(3) C14 0.041(4) 0.054(4) 0.051(4) -0.019(3) -0.011(3) 0.004(3) O4 0.041(2) 0.057(3) 0.042(3) -0.017(2) -0.010(2) 0.001(2) C15 0.035(3) 0.057(4) 0.047(4) -0.017(3) -0.011(3) 0.004(3) C16 0.048(4) 0.059(4) 0.066(5) -0.020(4) -0.014(4) 0.007(3) C17 0.051(4) 0.065(5) 0.057(5) -0.015(4) -0.012(4) 0.005(3) C18 0.073(6) 0.075(6) 0.069(6) -0.006(5) 0.000(5) 0.008(5) C19 0.045(4) 0.061(4) 0.050(4) -0.014(3) -0.008(4) 0.007(3) C20 0.038(4) 0.066(4) 0.057(4) -0.025(4) -0.015(4) 0.002(3) N3 0.038(3) 0.058(3) 0.045(3) -0.024(3) -0.007(3) 0.004(2) C21 0.048(4) 0.072(5) 0.055(5) -0.028(4) -0.008(4) 0.003(3) C22 0.050(4) 0.096(6) 0.069(6) -0.045(5) -0.018(4) 0.006(4) N4 0.047(4) 0.070(4) 0.093(5) -0.051(4) -0.004(4) -0.005(3) C23 0.055(4) 0.071(5) 0.058(5) -0.030(4) -0.013(4) 0.003(4) C24 0.055(4) 0.059(4) 0.061(5) -0.035(4) -0.007(4) 0.001(3) C25 0.046(4) 0.063(5) 0.061(5) -0.036(4) -0.009(4) 0.000(3) O5 0.053(3) 0.062(3) 0.056(3) -0.018(3) -0.011(3) -0.009(2) C26 0.055(5) 0.053(4) 0.084(6) -0.030(4) -0.006(5) -0.004(3) C27 0.057(5) 0.063(5) 0.098(7) -0.044(5) -0.011(5) 0.011(4) C28 0.063(5) 0.059(5) 0.078(6) -0.041(4) -0.006(5) -0.001(4) C29 0.085(7) 0.078(7) 0.106(9) -0.036(6) 0.002(7) -0.014(5) C30 0.050(4) 0.067(5) 0.086(6) -0.050(5) -0.008(4) -0.003(4) C31 0.055(5) 0.073(5) 0.105(8) -0.034(5) -0.033(5) 0.016(4) N5 0.062(4) 0.056(4) 0.101(6) -0.022(4) -0.038(4) 0.005(3) C32 0.060(5) 0.075(6) 0.094(7) -0.031(5) -0.028(5) 0.012(4) C33 0.039(4) 0.081(5) 0.074(5) -0.032(4) -0.028(4) 0.007(3) N6 0.044(3) 0.057(4) 0.053(4) -0.018(3) -0.012(3) -0.003(3) C34 0.057(4) 0.058(4) 0.060(5) -0.027(4) -0.023(4) -0.003(3) C35 0.049(4) 0.049(4) 0.051(4) -0.015(3) -0.012(3) 0.001(3) C36 0.047(4) 0.043(3) 0.046(4) -0.017(3) -0.008(3) 0.006(3) O6 0.048(3) 0.064(3) 0.047(3) -0.023(2) -0.017(2) -0.002(2) C37 0.045(4) 0.047(4) 0.049(4) -0.013(3) -0.016(3) 0.009(3) C38 0.051(4) 0.062(4) 0.044(4) -0.011(3) -0.016(4) 0.010(3) C39 0.052(4) 0.072(5) 0.047(4) -0.021(4) -0.019(4) 0.005(4) C40 0.065(5) 0.104(7) 0.051(5) -0.024(5) -0.021(4) -0.002(5) C41 0.046(4) 0.061(4) 0.050(4) -0.024(3) -0.013(4) 0.005(3) C42 0.044(4) 0.047(4) 0.053(4) -0.014(3) -0.011(3) 0.002(3) N7 0.037(3) 0.050(3) 0.053(3) -0.015(3) -0.011(3) 0.003(2) C43 0.051(4) 0.059(4) 0.056(5) -0.020(4) -0.010(4) 0.002(3) C44 0.050(4) 0.059(4) 0.061(5) -0.006(4) -0.015(4) -0.003(3) C45 0.041(4) 0.051(4) 0.053(4) -0.019(3) -0.013(3) 0.008(3) N8 0.044(3) 0.050(3) 0.055(4) -0.018(3) -0.016(3) 0.003(2) C46 0.049(4) 0.055(4) 0.049(4) -0.017(3) -0.014(4) 0.008(3) O11 0.055(3) 0.070(3) 0.063(4) -0.017(3) -0.021(3) 0.003(3) Cl1 0.091(7) 0.075(4) 0.067(4) -0.022(3) -0.008(4) 0.042(5) O12 0.051(9) 0.102(19) 0.089(19) 0.041(13) -0.014(13) 0.009(13) O13 0.134(7) 0.125(7) 0.092(6) -0.017(5) -0.036(6) -0.013(6) O14 0.076(4) 0.109(5) 0.061(4) -0.029(3) -0.027(3) 0.010(4) C54 0.093(8) 0.120(9) 0.094(8) -0.035(7) -0.043(7) -0.005(7) O15 0.122(7) 0.087(6) 0.102(7) -0.040(5) -0.039(6) 0.018(5) C55A 0.20(2) 0.094(14) 0.105(15) 0.034(12) 0.025(15) 0.009(15) O16A 0.115(10) 0.097(8) 0.121(10) -0.018(7) -0.029(9) 0.004(7) C56A 0.104(12) 0.070(9) 0.115(14) -0.019(9) -0.015(11) 0.029(8) O17A 0.119(10) 0.091(8) 0.109(9) -0.042(7) -0.022(8) 0.020(7) C57A 0.136(15) 0.119(17) 0.120(19) 0.029(14) 0.027(14) 0.070(13) O18A 0.076(14) 0.16(2) 0.128(14) -0.052(14) -0.011(12) 0.025(12) O18B 0.10(2) 0.14(2) 0.115(17) -0.029(17) -0.051(16) 0.036(17) C58A 0.078(11) 0.127(15) 0.081(12) -0.032(12) -0.015(11) 0.020(11) _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 O3 1.962(5) . ? Fe1 O4 1.967(5) . ? Fe1 O1 1.989(5) . ? Fe1 O2 2.000(5) . ? Fe1 N2 2.168(6) . ? Fe1 N1 2.202(6) . ? Fe2 O6 1.910(5) 2_666 ? Fe2 O5 1.966(5) 2_666 ? Fe2 O2 2.025(5) . ? Fe2 O1 2.034(4) . ? Fe2 N5 2.183(7) 2_666 ? Fe2 N6 2.194(6) 2_666 ? O1 C1 1.426(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 H2 0.84(4) . ? O3 C2 1.365(8) . ? C2 C3 1.400(11) . ? C2 C8 1.412(11) . ? C3 C4 1.399(10) . ? C3 C46 1.507(10) . ? C4 C5 1.426(12) . ? C4 H4 0.9500 . ? C5 C7 1.356(12) . ? C5 C6 1.514(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.405(10) . ? C7 H7 0.9500 . ? C8 C9 1.488(11) . ? C9 N1 1.485(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? N1 C10 1.491(9) . ? N1 H1 0.85(4) . ? C10 C11 1.518(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N2 1.474(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N2 C12 1.492(9) . ? N2 H2A 0.87(4) . ? C12 C13 1.509(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C19 1.393(11) . ? C13 C14 1.430(11) . ? C14 O4 1.347(9) . ? C14 C15 1.415(10) . ? C15 C16 1.396(11) . ? C15 C20 1.491(11) . ? C16 C17 1.382(12) . ? C16 H16 0.9500 . ? C17 C19 1.399(12) . ? C17 C18 1.525(12) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19 0.9500 . ? C20 N3 1.489(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N3 C21 1.492(10) . ? N3 H3 0.85(4) . ? C21 C22 1.511(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N4 1.475(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N4 C23 1.483(10) . ? N4 H4A 0.9200 . ? N4 H4B 0.9200 . ? C23 C24 1.503(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.403(11) . ? C24 C30 1.408(12) . ? C25 O5 1.336(9) . ? C25 C26 1.407(11) . ? O5 Fe2 1.966(5) 2_666 ? C26 C27 1.382(13) . ? C26 C31 1.500(12) . ? C27 C28 1.428(12) . ? C27 H27 0.9500 . ? C28 C30 1.400(12) . ? C28 C29 1.507(14) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30 0.9500 . ? C31 N5 1.458(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? N5 C32 1.432(11) . ? N5 Fe2 2.183(7) 2_666 ? N5 H5 0.9300 . ? C32 C33 1.494(12) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N6 1.496(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? N6 C34 1.493(10) . ? N6 Fe2 2.194(6) 2_666 ? N6 H6 0.88(4) . ? C34 C35 1.502(11) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C41 1.411(10) . ? C35 C36 1.421(10) . ? C36 O6 1.347(8) . ? C36 C37 1.398(10) . ? O6 Fe2 1.910(5) 2_666 ? C37 C38 1.404(10) . ? C37 C42 1.526(10) . ? C38 C39 1.375(11) . ? C38 H38 0.9500 . ? C39 C41 1.398(11) . ? C39 C40 1.525(11) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41 0.9500 . ? C42 N7 1.480(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? N7 C45 1.479(9) . ? N7 C43 1.481(9) . ? C43 C44 1.534(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N8 1.524(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 N8 1.466(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? N8 C46 1.504(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? O11 H111 1.349(6) . ? O11 H112 0.90(4) . ? O11 H113 0.88(4) . ? O14 C54 1.419(12) . ? O15 C55A 0.788(18) . ? O15 C55B 1.61(6) . ? C55A C55B 1.36(6) . ? O16A C56A 1.36(2) . ? O16A C56B 1.49(6) . ? O16B C56B 1.21(6) . ? O16B C56A 1.38(3) . ? C56A C56B 0.80(5) . ? O17A C57B 1.52(6) . ? O17A O17B 1.73(4) . ? O17A C57A 1.89(5) . ? O17B C57B 1.07(7) . ? O17B C57A 1.35(6) . ? O17C C57B 1.49(12) . ? O17C C57A 1.57(11) . ? O18A O18B 0.55(7) . ? O18A C58A 1.59(4) . ? O18B C58A 1.21(6) . ? O18B C58B 1.67(9) . ? O18B C58C 1.72(9) . ? C58A C58B 0.75(8) . ? C58A C58C 0.76(7) . ? C58B C58C 1.32(10) . ? 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 O3 Fe1 O4 89.37(19) . . ? O3 Fe1 O1 97.3(2) . . ? O4 Fe1 O1 102.58(19) . . ? O3 Fe1 O2 171.2(2) . . ? O4 Fe1 O2 97.2(2) . . ? O1 Fe1 O2 75.6(2) . . ? O3 Fe1 N2 91.5(2) . . ? O4 Fe1 N2 88.2(2) . . ? O1 Fe1 N2 166.1(2) . . ? O2 Fe1 N2 94.5(2) . . ? O3 Fe1 N1 87.7(2) . . ? O4 Fe1 N1 165.7(2) . . ? O1 Fe1 N1 91.7(2) . . ? O2 Fe1 N1 87.3(2) . . ? N2 Fe1 N1 77.9(2) . . ? O6 Fe2 O5 96.2(2) 2_666 2_666 ? O6 Fe2 O2 166.7(2) 2_666 . ? O5 Fe2 O2 92.1(2) 2_666 . ? O6 Fe2 O1 94.2(2) 2_666 . ? O5 Fe2 O1 99.7(2) 2_666 . ? O2 Fe2 O1 74.11(19) . . ? O6 Fe2 N5 89.7(3) 2_666 2_666 ? O5 Fe2 N5 86.3(2) 2_666 2_666 ? O2 Fe2 N5 101.2(3) . 2_666 ? O1 Fe2 N5 172.4(2) . 2_666 ? O6 Fe2 N6 88.8(2) 2_666 2_666 ? O5 Fe2 N6 162.2(2) 2_666 2_666 ? O2 Fe2 N6 86.5(2) . 2_666 ? O1 Fe2 N6 97.0(2) . 2_666 ? N5 Fe2 N6 76.6(2) 2_666 2_666 ? C1 O1 Fe1 128.8(4) . . ? C1 O1 Fe2 125.7(4) . . ? Fe1 O1 Fe2 104.1(2) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Fe1 O2 Fe2 104.1(2) . . ? Fe1 O2 H2 132(6) . . ? Fe2 O2 H2 124(6) . . ? C2 O3 Fe1 128.4(4) . . ? O3 C2 C3 119.7(6) . . ? O3 C2 C8 119.1(7) . . ? C3 C2 C8 121.1(6) . . ? C4 C3 C2 118.1(7) . . ? C4 C3 C46 119.5(7) . . ? C2 C3 C46 122.4(6) . . ? C3 C4 C5 122.4(7) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C7 C5 C4 116.2(7) . . ? C7 C5 C6 123.1(8) . . ? C4 C5 C6 120.7(8) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 C8 124.8(7) . . ? C5 C7 H7 117.6 . . ? C8 C7 H7 117.6 . . ? C7 C8 C2 117.0(7) . . ? C7 C8 C9 121.7(7) . . ? C2 C8 C9 121.2(6) . . ? N1 C9 C8 111.3(6) . . ? N1 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? N1 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 N1 C10 115.1(6) . . ? C9 N1 Fe1 110.3(4) . . ? C10 N1 Fe1 111.7(5) . . ? C9 N1 H1 112(6) . . ? C10 N1 H1 105(6) . . ? Fe1 N1 H1 102(5) . . ? N1 C10 C11 110.0(6) . . ? N1 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? N1 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C10 108.0(6) . . ? N2 C11 H11A 110.1 . . ? C10 C11 H11A 110.1 . . ? N2 C11 H11B 110.1 . . ? C10 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? C11 N2 C12 115.7(6) . . ? C11 N2 Fe1 107.4(5) . . ? C12 N2 Fe1 113.1(5) . . ? C11 N2 H2A 103(5) . . ? C12 N2 H2A 102(5) . . ? Fe1 N2 H2A 116(6) . . ? N2 C12 C13 108.6(6) . . ? N2 C12 H12A 110.0 . . ? C13 C12 H12A 110.0 . . ? N2 C12 H12B 110.0 . . ? C13 C12 H12B 110.0 . . ? H12A C12 H12B 108.3 . . ? C19 C13 C14 119.1(7) . . ? C19 C13 C12 122.4(7) . . ? C14 C13 C12 118.2(7) . . ? O4 C14 C15 121.3(7) . . ? O4 C14 C13 120.4(6) . . ? C15 C14 C13 118.3(7) . . ? C14 O4 Fe1 122.3(4) . . ? C16 C15 C14 120.1(7) . . ? C16 C15 C20 121.5(7) . . ? C14 C15 C20 118.1(7) . . ? C17 C16 C15 122.2(8) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C16 C17 C19 117.7(8) . . ? C16 C17 C18 120.4(8) . . ? C19 C17 C18 121.7(9) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C19 C17 122.6(8) . . ? C13 C19 H19 118.7 . . ? C17 C19 H19 118.7 . . ? N3 C20 C15 111.1(6) . . ? N3 C20 H20A 109.4 . . ? C15 C20 H20A 109.4 . . ? N3 C20 H20B 109.4 . . ? C15 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C20 N3 C21 113.4(6) . . ? C20 N3 H3 105(6) . . ? C21 N3 H3 122(6) . . ? N3 C21 C22 113.4(7) . . ? N3 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? N3 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? N4 C22 C21 114.2(7) . . ? N4 C22 H22A 108.7 . . ? C21 C22 H22A 108.7 . . ? N4 C22 H22B 108.7 . . ? C21 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C22 N4 C23 110.0(7) . . ? C22 N4 H4A 109.7 . . ? C23 N4 H4A 109.7 . . ? C22 N4 H4B 109.7 . . ? C23 N4 H4B 109.7 . . ? H4A N4 H4B 108.2 . . ? N4 C23 C24 115.6(7) . . ? N4 C23 H23A 108.4 . . ? C24 C23 H23A 108.4 . . ? N4 C23 H23B 108.4 . . ? C24 C23 H23B 108.4 . . ? H23A C23 H23B 107.4 . . ? C25 C24 C30 118.2(7) . . ? C25 C24 C23 117.2(7) . . ? C30 C24 C23 124.5(7) . . ? O5 C25 C24 119.7(7) . . ? O5 C25 C26 120.1(7) . . ? C24 C25 C26 120.2(7) . . ? C25 O5 Fe2 118.8(5) . 2_666 ? C27 C26 C25 120.0(8) . . ? C27 C26 C31 121.5(8) . . ? C25 C26 C31 118.4(8) . . ? C26 C27 C28 121.3(9) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C30 C28 C27 117.0(8) . . ? C30 C28 C29 122.4(9) . . ? C27 C28 C29 120.3(9) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 C24 122.8(8) . . ? C28 C30 H30 118.6 . . ? C24 C30 H30 118.6 . . ? N5 C31 C26 110.0(8) . . ? N5 C31 H31A 109.7 . . ? C26 C31 H31A 109.7 . . ? N5 C31 H31B 109.7 . . ? C26 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C32 N5 C31 120.1(7) . . ? C32 N5 Fe2 109.3(5) . 2_666 ? C31 N5 Fe2 116.8(5) . 2_666 ? C32 N5 H5 102.5 . . ? C31 N5 H5 102.5 . . ? Fe2 N5 H5 102.5 2_666 . ? N5 C32 C33 110.1(8) . . ? N5 C32 H32A 109.6 . . ? C33 C32 H32A 109.6 . . ? N5 C32 H32B 109.6 . . ? C33 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C32 C33 N6 109.3(6) . . ? C32 C33 H33A 109.8 . . ? N6 C33 H33A 109.8 . . ? C32 C33 H33B 109.8 . . ? N6 C33 H33B 109.8 . . ? H33A C33 H33B 108.3 . . ? C34 N6 C33 113.5(6) . . ? C34 N6 Fe2 111.0(4) . 2_666 ? C33 N6 Fe2 113.2(4) . 2_666 ? C34 N6 H6 106(6) . . ? C33 N6 H6 108(6) . . ? Fe2 N6 H6 104(5) 2_666 . ? N6 C34 C35 112.5(6) . . ? N6 C34 H34A 109.1 . . ? C35 C34 H34A 109.1 . . ? N6 C34 H34B 109.1 . . ? C35 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? C41 C35 C36 118.9(7) . . ? C41 C35 C34 118.9(6) . . ? C36 C35 C34 122.1(6) . . ? O6 C36 C37 119.5(6) . . ? O6 C36 C35 120.7(6) . . ? C37 C36 C35 119.8(6) . . ? C36 O6 Fe2 132.9(4) . 2_666 ? C36 C37 C38 118.3(7) . . ? C36 C37 C42 122.1(6) . . ? C38 C37 C42 119.6(7) . . ? C39 C38 C37 123.8(7) . . ? C39 C38 H38 118.1 . . ? C37 C38 H38 118.1 . . ? C38 C39 C41 117.2(7) . . ? C38 C39 C40 123.2(7) . . ? C41 C39 C40 119.5(7) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 C35 121.8(7) . . ? C39 C41 H41 119.1 . . ? C35 C41 H41 119.1 . . ? N7 C42 C37 112.1(6) . . ? N7 C42 H42A 109.2 . . ? C37 C42 H42A 109.2 . . ? N7 C42 H42B 109.2 . . ? C37 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C45 N7 C42 112.2(6) . . ? C45 N7 C43 102.2(5) . . ? C42 N7 C43 114.3(5) . . ? N7 C43 C44 104.3(6) . . ? N7 C43 H43A 110.9 . . ? C44 C43 H43A 110.9 . . ? N7 C43 H43B 110.9 . . ? C44 C43 H43B 110.9 . . ? H43A C43 H43B 108.9 . . ? N8 C44 C43 105.2(6) . . ? N8 C44 H44A 110.7 . . ? C43 C44 H44A 110.7 . . ? N8 C44 H44B 110.7 . . ? C43 C44 H44B 110.7 . . ? H44A C44 H44B 108.8 . . ? N8 C45 N7 103.5(6) . . ? N8 C45 H45A 111.1 . . ? N7 C45 H45A 111.1 . . ? N8 C45 H45B 111.1 . . ? N7 C45 H45B 111.1 . . ? H45A C45 H45B 109.0 . . ? C45 N8 C46 113.5(5) . . ? C45 N8 C44 102.9(5) . . ? C46 N8 C44 110.3(6) . . ? N8 C46 C3 114.1(6) . . ? N8 C46 H46A 108.7 . . ? C3 C46 H46A 108.7 . . ? N8 C46 H46B 108.7 . . ? C3 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? H111 O11 H112 122(7) . . ? H111 O11 H113 104(7) . . ? H112 O11 H113 106(10) . . ? C55A O15 C55B 57(4) . . ? O15 C55A C55B 93(4) . . ? C55A C55B O15 29.2(14) . . ? C56A O16A C56B 32(2) . . ? C56B O16B C56A 35(2) . . ? C56B C56A O16A 83(5) . . ? C56B C56A O16B 61(5) . . ? O16A C56A O16B 134(2) . . ? C56A C56B O16B 84(5) . . ? C56A C56B O16A 65(4) . . ? O16B C56B O16A 138(5) . . ? C57B O17A O17B 38(3) . . ? C57B O17A C57A 7(4) . . ? O17B O17A C57A 44(2) . . ? C57B O17B C57A 15(5) . . ? C57B O17B O17A 61(4) . . ? C57A O17B O17A 75(3) . . ? C57B O17C C57A 16(4) . . ? O17B C57A O17C 96(5) . . ? O17B C57A O17A 62(2) . . ? O17C C57A O17A 75(4) . . ? O17B C57B O17C 117(7) . . ? O17B C57B O17A 82(4) . . ? O17C C57B O17A 90(5) . . ? O18B O18A C58A 38(10) . . ? O18A O18B C58A 125(10) . . ? O18A O18B C58B 126(10) . . ? C58A O18B C58B 24(3) . . ? O18A O18B C58C 124(10) . . ? C58A O18B C58C 22(3) . . ? C58B O18B C58C 46(4) . . ? C58B C58A C58C 123(10) . . ? C58B C58A O18B 115(8) . . ? C58C C58A O18B 121(7) . . ? C58B C58A O18A 116(8) . . ? C58C C58A O18A 121(6) . . ? O18B C58A O18A 16(4) . . ? C58A C58B C58C 29(6) . . ? C58A C58B O18B 41(6) . . ? C58C C58B O18B 69(5) . . ? C58A C58C C58B 29(5) . . ? C58A C58C O18B 37(5) . . ? C58B C58C O18B 65(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Fe1 O1 C1 3.5(6) . . . . ? O4 Fe1 O1 C1 -87.5(6) . . . . ? O2 Fe1 O1 C1 178.2(6) . . . . ? N2 Fe1 O1 C1 132.6(9) . . . . ? N1 Fe1 O1 C1 91.3(6) . . . . ? O3 Fe1 O1 Fe2 -163.64(19) . . . . ? O4 Fe1 O1 Fe2 105.4(2) . . . . ? O2 Fe1 O1 Fe2 11.0(2) . . . . ? N2 Fe1 O1 Fe2 -34.5(9) . . . . ? N1 Fe1 O1 Fe2 -75.8(2) . . . . ? O6 Fe2 O1 C1 7.8(5) 2_666 . . . ? O5 Fe2 O1 C1 -89.2(5) 2_666 . . . ? O2 Fe2 O1 C1 -178.6(6) . . . . ? N5 Fe2 O1 C1 129(2) 2_666 . . . ? N6 Fe2 O1 C1 97.0(5) 2_666 . . . ? O6 Fe2 O1 Fe1 175.4(2) 2_666 . . . ? O5 Fe2 O1 Fe1 78.4(2) 2_666 . . . ? O2 Fe2 O1 Fe1 -11.0(2) . . . . ? N5 Fe2 O1 Fe1 -63(2) 2_666 . . . ? N6 Fe2 O1 Fe1 -95.3(2) 2_666 . . . ? O3 Fe1 O2 Fe2 26.1(15) . . . . ? O4 Fe1 O2 Fe2 -112.3(2) . . . . ? O1 Fe1 O2 Fe2 -11.1(2) . . . . ? N2 Fe1 O2 Fe2 159.0(2) . . . . ? N1 Fe1 O2 Fe2 81.4(2) . . . . ? O6 Fe2 O2 Fe1 39.9(10) 2_666 . . . ? O5 Fe2 O2 Fe1 -88.6(2) 2_666 . . . ? O1 Fe2 O2 Fe1 10.9(2) . . . . ? N5 Fe2 O2 Fe1 -175.2(2) 2_666 . . . ? N6 Fe2 O2 Fe1 109.2(3) 2_666 . . . ? O4 Fe1 O3 C2 -144.7(6) . . . . ? O1 Fe1 O3 C2 112.7(6) . . . . ? O2 Fe1 O3 C2 76.5(15) . . . . ? N2 Fe1 O3 C2 -56.6(6) . . . . ? N1 Fe1 O3 C2 21.2(6) . . . . ? Fe1 O3 C2 C3 133.6(6) . . . . ? Fe1 O3 C2 C8 -43.9(9) . . . . ? O3 C2 C3 C4 176.8(7) . . . . ? C8 C2 C3 C4 -5.7(11) . . . . ? O3 C2 C3 C46 -4.4(11) . . . . ? C8 C2 C3 C46 173.1(7) . . . . ? C2 C3 C4 C5 2.3(12) . . . . ? C46 C3 C4 C5 -176.5(7) . . . . ? C3 C4 C5 C7 2.1(12) . . . . ? C3 C4 C5 C6 -178.2(8) . . . . ? C4 C5 C7 C8 -3.3(13) . . . . ? C6 C5 C7 C8 177.0(9) . . . . ? C5 C7 C8 C2 0.1(12) . . . . ? C5 C7 C8 C9 176.4(8) . . . . ? O3 C2 C8 C7 -177.9(7) . . . . ? C3 C2 C8 C7 4.6(11) . . . . ? O3 C2 C8 C9 5.8(11) . . . . ? C3 C2 C8 C9 -171.7(7) . . . . ? C7 C8 C9 N1 -122.4(8) . . . . ? C2 C8 C9 N1 53.7(9) . . . . ? C8 C9 N1 C10 59.3(8) . . . . ? C8 C9 N1 Fe1 -68.3(7) . . . . ? O3 Fe1 N1 C9 32.2(5) . . . . ? O4 Fe1 N1 C9 110.4(9) . . . . ? O1 Fe1 N1 C9 -65.1(5) . . . . ? O2 Fe1 N1 C9 -140.6(5) . . . . ? N2 Fe1 N1 C9 124.2(5) . . . . ? O3 Fe1 N1 C10 -97.3(4) . . . . ? O4 Fe1 N1 C10 -19.1(11) . . . . ? O1 Fe1 N1 C10 165.5(4) . . . . ? O2 Fe1 N1 C10 89.9(4) . . . . ? N2 Fe1 N1 C10 -5.2(4) . . . . ? C9 N1 C10 C11 -148.6(6) . . . . ? Fe1 N1 C10 C11 -21.7(7) . . . . ? N1 C10 C11 N2 49.7(8) . . . . ? C10 C11 N2 C12 179.3(6) . . . . ? C10 C11 N2 Fe1 -53.3(6) . . . . ? O3 Fe1 N2 C11 119.0(5) . . . . ? O4 Fe1 N2 C11 -151.7(5) . . . . ? O1 Fe1 N2 C11 -10.6(11) . . . . ? O2 Fe1 N2 C11 -54.6(5) . . . . ? N1 Fe1 N2 C11 31.7(4) . . . . ? O3 Fe1 N2 C12 -112.1(5) . . . . ? O4 Fe1 N2 C12 -22.8(5) . . . . ? O1 Fe1 N2 C12 118.3(8) . . . . ? O2 Fe1 N2 C12 74.3(5) . . . . ? N1 Fe1 N2 C12 160.6(5) . . . . ? C11 N2 C12 C13 -169.9(6) . . . . ? Fe1 N2 C12 C13 65.6(7) . . . . ? N2 C12 C13 C19 114.9(8) . . . . ? N2 C12 C13 C14 -58.6(8) . . . . ? C19 C13 C14 O4 -177.7(6) . . . . ? C12 C13 C14 O4 -3.9(10) . . . . ? C19 C13 C14 C15 0.2(10) . . . . ? C12 C13 C14 C15 174.0(6) . . . . ? C15 C14 O4 Fe1 -123.5(6) . . . . ? C13 C14 O4 Fe1 54.4(8) . . . . ? O3 Fe1 O4 C14 56.4(5) . . . . ? O1 Fe1 O4 C14 153.8(5) . . . . ? O2 Fe1 O4 C14 -129.4(5) . . . . ? N2 Fe1 O4 C14 -35.2(5) . . . . ? N1 Fe1 O4 C14 -21.6(11) . . . . ? O4 C14 C15 C16 179.3(6) . . . . ? C13 C14 C15 C16 1.4(10) . . . . ? O4 C14 C15 C20 4.9(9) . . . . ? C13 C14 C15 C20 -173.0(6) . . . . ? C14 C15 C16 C17 -1.1(11) . . . . ? C20 C15 C16 C17 173.1(7) . . . . ? C15 C16 C17 C19 -0.9(11) . . . . ? C15 C16 C17 C18 -176.1(7) . . . . ? C14 C13 C19 C17 -2.3(11) . . . . ? C12 C13 C19 C17 -175.8(7) . . . . ? C16 C17 C19 C13 2.6(11) . . . . ? C18 C17 C19 C13 177.8(7) . . . . ? C16 C15 C20 N3 -105.3(8) . . . . ? C14 C15 C20 N3 69.1(8) . . . . ? C15 C20 N3 C21 -170.1(6) . . . . ? C20 N3 C21 C22 -63.9(8) . . . . ? N3 C21 C22 N4 -64.1(9) . . . . ? C21 C22 N4 C23 -77.2(9) . . . . ? C22 N4 C23 C24 -172.4(7) . . . . ? N4 C23 C24 C25 -169.6(7) . . . . ? N4 C23 C24 C30 7.8(11) . . . . ? C30 C24 C25 O5 -174.8(7) . . . . ? C23 C24 C25 O5 2.8(11) . . . . ? C30 C24 C25 C26 7.1(12) . . . . ? C23 C24 C25 C26 -175.3(7) . . . . ? C24 C25 O5 Fe2 123.6(7) . . . 2_666 ? C26 C25 O5 Fe2 -58.3(9) . . . 2_666 ? O5 C25 C26 C27 173.2(8) . . . . ? C24 C25 C26 C27 -8.7(13) . . . . ? O5 C25 C26 C31 -3.2(12) . . . . ? C24 C25 C26 C31 174.9(8) . . . . ? C25 C26 C27 C28 5.9(14) . . . . ? C31 C26 C27 C28 -177.9(9) . . . . ? C26 C27 C28 C30 -1.6(13) . . . . ? C26 C27 C28 C29 -175.5(9) . . . . ? C27 C28 C30 C24 0.1(12) . . . . ? C29 C28 C30 C24 173.8(9) . . . . ? C25 C24 C30 C28 -2.8(12) . . . . ? C23 C24 C30 C28 179.8(8) . . . . ? C27 C26 C31 N5 -115.6(10) . . . . ? C25 C26 C31 N5 60.8(12) . . . . ? C26 C31 N5 C32 171.2(8) . . . . ? C26 C31 N5 Fe2 -52.6(10) . . . 2_666 ? C31 N5 C32 C33 -170.7(8) . . . . ? Fe2 N5 C32 C33 50.2(9) 2_666 . . . ? N5 C32 C33 N6 -46.8(10) . . . . ? C32 C33 N6 C34 148.7(7) . . . . ? C32 C33 N6 Fe2 21.0(9) . . . 2_666 ? C33 N6 C34 C35 -64.6(8) . . . . ? Fe2 N6 C34 C35 64.2(7) 2_666 . . . ? N6 C34 C35 C41 132.3(7) . . . . ? N6 C34 C35 C36 -50.3(9) . . . . ? C41 C35 C36 O6 178.8(6) . . . . ? C34 C35 C36 O6 1.3(10) . . . . ? C41 C35 C36 C37 -1.6(10) . . . . ? C34 C35 C36 C37 -179.0(7) . . . . ? C37 C36 O6 Fe2 -152.6(5) . . . 2_666 ? C35 C36 O6 Fe2 27.0(9) . . . 2_666 ? O6 C36 C37 C38 -176.3(6) . . . . ? C35 C36 C37 C38 4.1(10) . . . . ? O6 C36 C37 C42 5.4(10) . . . . ? C35 C36 C37 C42 -174.2(6) . . . . ? C36 C37 C38 C39 -3.1(11) . . . . ? C42 C37 C38 C39 175.2(7) . . . . ? C37 C38 C39 C41 -0.4(11) . . . . ? C37 C38 C39 C40 178.1(8) . . . . ? C38 C39 C41 C35 3.1(11) . . . . ? C40 C39 C41 C35 -175.5(7) . . . . ? C36 C35 C41 C39 -2.1(11) . . . . ? C34 C35 C41 C39 175.4(7) . . . . ? C36 C37 C42 N7 -93.6(8) . . . . ? C38 C37 C42 N7 88.0(8) . . . . ? C37 C42 N7 C45 72.6(7) . . . . ? C37 C42 N7 C43 -171.7(6) . . . . ? C45 N7 C43 C44 -34.3(7) . . . . ? C42 N7 C43 C44 -155.7(6) . . . . ? N7 C43 C44 N8 9.7(8) . . . . ? C42 N7 C45 N8 170.5(5) . . . . ? C43 N7 C45 N8 47.7(7) . . . . ? N7 C45 N8 C46 78.4(7) . . . . ? N7 C45 N8 C44 -40.8(7) . . . . ? C43 C44 N8 C45 18.8(8) . . . . ? C43 C44 N8 C46 -102.6(7) . . . . ? C45 N8 C46 C3 43.3(8) . . . . ? C44 N8 C46 C3 158.2(6) . . . . ? C4 C3 C46 N8 -96.5(8) . . . . ? C2 C3 C46 N8 84.7(8) . . . . ? C56B O16A C56A O16B -36(4) . . . . ? C56B O16B C56A O16A 42(5) . . . . ? O16A C56A C56B O16B -151(3) . . . . ? O16B C56A C56B O16A 151(3) . . . . ? C56A O16B C56B O16A -41(5) . . . . ? C56A O16A C56B O16B 46(5) . . . . ? C57A O17A O17B C57B 6(5) . . . . ? C57B O17A O17B C57A -6(5) . . . . ? C57B O17B C57A O17C 50(19) . . . . ? O17A O17B C57A O17C 70(4) . . . . ? C57B O17B C57A O17A -19(19) . . . . ? C57B O17C C57A O17B -32(14) . . . . ? C57B O17C C57A O17A 27(15) . . . . ? C57B O17A C57A O17B 29(31) . . . . ? C57B O17A C57A O17C -76(31) . . . . ? O17B O17A C57A O17C -106(4) . . . . ? C57A O17B C57B O17C -115(22) . . . . ? O17A O17B C57B O17C 86(6) . . . . ? C57A O17B C57B O17A 159(21) . . . . ? C57A O17C C57B O17B 132(19) . . . . ? C57A O17C C57B O17A -147(18) . . . . ? C57A O17A C57B O17B -147(34) . . . . ? O17B O17A C57B O17C -117(7) . . . . ? C57A O17A C57B O17C 97(33) . . . . ? C58A O18A O18B C58B 30(6) . . . . ? C58A O18A O18B C58C -27(6) . . . . ? O18A O18B C58A C58B 100(15) . . . . ? C58C O18B C58A C58B -166(13) . . . . ? O18A O18B C58A C58C -94(14) . . . . ? C58B O18B C58A C58C 166(13) . . . . ? C58B O18B C58A O18A -100(15) . . . . ? C58C O18B C58A O18A 94(14) . . . . ? O18B O18A C58A C58B -88(15) . . . . ? O18B O18A C58A C58C 96(14) . . . . ? O18B C58A C58B C58C 166(13) . . . . ? O18A C58A C58B C58C -176(13) . . . . ? C58C C58A C58B O18B -166(13) . . . . ? O18A C58A C58B O18B 18(5) . . . . ? O18A O18B C58B C58A -98(17) . . . . ? C58C O18B C58B C58A 7(7) . . . . ? O18A O18B C58B C58C -105(15) . . . . ? C58A O18B C58B C58C -7(7) . . . . ? O18B C58A C58C C58B -165(14) . . . . ? O18A C58A C58C C58B 176(13) . . . . ? C58B C58A C58C O18B 165(14) . . . . ? O18A C58A C58C O18B -19(5) . . . . ? O18B C58B C58C C58A 10(9) . . . . ? C58A C58B C58C O18B -10(9) . . . . ? O18A O18B C58C C58A 101(14) . . . . ? C58B O18B C58C C58A -8(8) . . . . ? O18A O18B C58C C58B 109(12) . . . . ? C58A O18B C58C C58B 8(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O12 0.84(4) 2.23(5) 3.08(3) 176(8) . O2 H2 Cl1 0.84(4) 2.45(4) 3.277(12) 168(8) . N1 H1 O5 0.85(4) 2.13(5) 2.925(8) 156(8) 2_666 N2 H2A O14 0.87(4) 2.15(5) 2.964(8) 156(8) . N3 H3 O3 0.85(4) 2.12(4) 2.942(8) 165(8) . N4 H4A O16A 0.92 2.47 3.270(15) 146.0 1_455 N5 H5 O17A 0.93 2.34 3.162(16) 147.8 . N6 H6 O11 0.88(4) 2.08(4) 2.935(9) 166(8) . O11 H111 O11 1.349(6) 1.349(6) 2.698(12) 180.0(4) 2_766 O11 H112 O18A 0.90(4) 1.96(8) 2.73(4) 142(9) . O11 H112 O18B 0.90(4) 1.94(8) 2.77(6) 154(10) . O11 H113 O4 0.88(4) 1.83(4) 2.704(7) 175(10) 2_666 _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.550 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.112