# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_publication_text _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Prof. Dr. Joris van Slageren' _publ_contact_author_address ;Institut f\"ur Physikalische Chemie Universit\"at Stuttgart Pfaffenwaldring 55 D-70569 Stuttgart Germany ; _publ_contact_author_email ipcjosl@ipc.uni-stuttgart.de _publ_contact_author_phone +49(0)711685643 loop_ _publ_author_name _publ_author_address 'Piga, Francesco' ;School of Chemistry University of Nottingham University Park Nottingham NG7 1RD United Kingdom ; 'Moro, Fabrizio' ;School of Chemistry University of Nottingham University Park Nottingham NG7 1RD United Kingdom ; 'Krivokapic, Itana' ;School of Chemistry University of Nottingham University Park Nottingham NG7 1RD United Kingdom ; 'Blake, Alexander J.' ;School of Chemistry University of Nottingham University Park Nottingham NG7 1RD United Kingdom ; 'Edge, Ruth' ;School of Chemistry The University of Manchester Manchester M13 9PL United Kingdom ; 'McInnes, Eric J. L.' ;School of Chemistry The University of Manchester Manchester M13 9PL United Kingdom ; 'Luis, Fernando' ;Departamento de Fi?sica de la Materia Condensada Instituto de Ciencia de Materiales de Arago?n CSIC - Universidad de Zaragoza Zaragoza 50009 Spain ; 'Evangelisti, Marco' ;Departamento de Fi?sica de la Materia Condensada Instituto de Ciencia de Materiales de Arago?n CSIC - Universidad de Zaragoza Zaragoza 50009 Spain ; 'Evans, David J.' ;Department of Biological Chemistry John Innes Centre Norwich Research Park Norwich NR4 7UH United Kingdom ; 'McMaster, Jonathan' ;School of Chemistry University of Nottingham University Park Nottingham NG7 1RD United Kingdom ; 'van Slageren, Joris' ;Institut f\"ur Physikalische Chemie Universit\"at Stuttgart Pfaffenwaldring 55 D-70569 Stuttgart Germany ; data_fefplg _database_code_depnum_ccdc_archive 'CCDC 820008' _nottingham_internal_coll_name FEFPLG _nottingham_internal_coll_number 9129 _nottingham_internal_coll_client FP/JVS _nottingham_internal_coll_type hemisphere _nottingham_internal_coll_frame_time '45 s' _nottingham_internal_coll_frame_width '0.3 degrees' _nottingham_internal_coll_frame_method \w _nottingham_internal_coll_user FP _nottingham_internal_coll_date 21/01/2010 _nottingham_internal_process_user FP _nottingham_internal_process_date 13/09/2010 _nottingham_internal_solution_user FP _nottingham_internal_solution_date 20/10/2010 _nottingham_internal_refinement_user FP _nottingham_internal_refinement_date 20/10/2010 _nottingham_internal_validation_user ? _nottingham_internal_validation_date ? _nottingham_internal_archive_date ? _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 Cl2 Fe2 N2 O4' _chemical_formula_sum 'C28 H40 Cl4 Fe4 N4 O8' _chemical_formula_weight 925.84 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-42d ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 16.0765(6) _cell_length_b 16.0765(6) _cell_length_c 29.839(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7712.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.49 _exptl_crystal_description PLATE _exptl_crystal_colour ORANGE _exptl_crystal_size_min 0.028 _exptl_crystal_size_mid 0.068 _exptl_crystal_size_max 0.072 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3776 _exptl_absorpt_coefficient_mu 1.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.626 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23824 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.55 _reflns_number_total 4452 _reflns_number_gt 4145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' ? ' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0543P)^2^+13.3786P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 4452 _refine_ls_number_parameters 227 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.107 _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 0.48401(3) 0.40013(3) 0.036783(17) 0.01496(12) Uani 1 1 d . . . Cl1 Cl 0.57236(6) 0.28030(6) 0.04452(3) 0.0224(2) Uani 1 1 d D . . O10 O 0.41449(15) 0.51179(16) 0.03344(8) 0.0157(5) Uani 1 1 d . . . C11 C 0.3508(2) 0.5140(3) 0.06568(12) 0.0189(8) Uani 1 1 d . . . H11A H 0.3007 0.4859 0.0537 0.023 Uiso 1 1 calc R . . H11B H 0.3361 0.5725 0.0723 0.023 Uiso 1 1 calc R . . C12 C 0.3784(2) 0.4713(2) 0.10837(13) 0.0178(8) Uani 1 1 d . . . C13 C 0.3388(3) 0.4858(3) 0.14933(13) 0.0218(8) Uani 1 1 d . . . H13 H 0.2925 0.5223 0.1511 0.026 Uiso 1 1 calc R . . C14 C 0.3685(3) 0.4460(3) 0.18717(14) 0.0291(10) Uani 1 1 d . . . H14 H 0.3428 0.4549 0.2155 0.035 Uiso 1 1 calc R . . C15 C 0.4360(3) 0.3929(3) 0.18334(13) 0.0272(9) Uani 1 1 d . . . H15 H 0.4574 0.3652 0.2090 0.033 Uiso 1 1 calc R . . C16 C 0.4719(3) 0.3807(3) 0.14174(13) 0.0232(9) Uani 1 1 d . . . H16 H 0.5182 0.3442 0.1392 0.028 Uiso 1 1 calc R . . N17 N 0.4431(2) 0.4193(2) 0.10478(10) 0.0179(7) Uani 1 1 d . . . O18 O 0.37326(18) 0.32373(19) 0.02511(9) 0.0224(6) Uani 1 1 d D . . H18 H 0.338(3) 0.346(3) 0.0068(15) 0.019(12) Uiso 1 1 d D . . C19 C 0.3205(3) 0.2846(3) 0.05745(16) 0.0319(10) Uani 1 1 d D . . H19A H 0.3545 0.2614 0.0816 0.048 Uiso 1 1 calc R . . H19B H 0.2888 0.2399 0.0430 0.048 Uiso 1 1 calc R . . H19C H 0.2819 0.3259 0.0698 0.048 Uiso 1 1 calc R . . Fe2 Fe 0.07041(3) 0.57429(3) 0.213557(17) 0.01707(13) Uani 1 1 d . . . Cl2 Cl 0.06266(7) 0.72307(6) 0.20520(4) 0.0298(2) Uani 1 1 d D . . O20 O 0.06391(17) 0.44260(16) 0.21622(9) 0.0178(5) Uani 1 1 d . . . C21 C 0.1133(3) 0.4043(3) 0.18287(12) 0.0220(8) Uani 1 1 d . . . H21A H 0.0918 0.3477 0.1766 0.026 Uiso 1 1 calc R . . H21B H 0.1713 0.3990 0.1937 0.026 Uiso 1 1 calc R . . C22 C 0.1115(2) 0.4561(2) 0.14000(13) 0.0184(8) Uani 1 1 d . . . C23 C 0.1285(2) 0.4213(3) 0.09829(13) 0.0223(8) Uani 1 1 d . . . H23 H 0.1394 0.3635 0.0955 0.027 Uiso 1 1 calc R . . C24 C 0.1293(3) 0.4721(3) 0.06097(13) 0.0227(9) Uani 1 1 d . . . H24 H 0.1404 0.4497 0.0321 0.027 Uiso 1 1 calc R . . C25 C 0.1137(3) 0.5560(3) 0.06631(13) 0.0240(9) Uani 1 1 d . . . H25 H 0.1149 0.5924 0.0412 0.029 Uiso 1 1 calc R . . C26 C 0.0963(3) 0.5861(3) 0.10862(13) 0.0232(9) Uani 1 1 d . . . H26 H 0.0848 0.6437 0.1121 0.028 Uiso 1 1 calc R . . N27 N 0.0950(2) 0.5368(2) 0.14533(10) 0.0186(7) Uani 1 1 d . . . O28 O 0.20593(19) 0.5714(2) 0.22338(10) 0.0283(7) Uani 1 1 d D . . H28 H 0.223(4) 0.543(3) 0.2451(19) 0.06(2) Uiso 1 1 d D . . C29 C 0.2641(4) 0.6390(4) 0.2274(2) 0.0485(14) Uani 1 1 d D . . H29A H 0.2473 0.6845 0.2076 0.073 Uiso 1 1 calc R . . H29B H 0.3198 0.6197 0.2190 0.073 Uiso 1 1 calc R . . H29C H 0.2649 0.6588 0.2585 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0153(3) 0.0160(3) 0.0135(2) 0.0007(2) 0.0021(2) 0.00186(19) Cl1 0.0240(5) 0.0183(4) 0.0249(4) 0.0037(4) 0.0037(4) 0.0044(4) O10 0.0127(12) 0.0178(13) 0.0167(12) 0.0010(11) 0.0017(10) 0.0005(10) C11 0.0158(19) 0.022(2) 0.0185(18) 0.0022(15) 0.0015(15) 0.0046(16) C12 0.0186(19) 0.0166(19) 0.0181(19) 0.0035(14) 0.0005(14) 0.0015(15) C13 0.018(2) 0.026(2) 0.0220(19) 0.0000(16) 0.0054(15) 0.0041(17) C14 0.028(2) 0.042(3) 0.0170(19) 0.0012(18) 0.0081(16) 0.0030(19) C15 0.031(2) 0.033(2) 0.0173(18) 0.0052(16) -0.0006(17) 0.007(2) C16 0.022(2) 0.026(2) 0.0216(19) 0.0030(15) 0.0000(16) 0.0041(16) N17 0.0180(16) 0.0211(17) 0.0146(14) 0.0021(12) 0.0013(12) 0.0006(13) O18 0.0211(15) 0.0247(15) 0.0213(14) 0.0043(11) 0.0010(11) -0.0030(12) C19 0.027(2) 0.029(2) 0.040(3) 0.011(2) 0.0078(19) -0.0021(19) Fe2 0.0210(3) 0.0163(3) 0.0139(2) -0.0007(2) 0.0018(2) -0.0015(2) Cl2 0.0447(6) 0.0179(5) 0.0267(5) 0.0003(4) 0.0080(5) -0.0039(4) O20 0.0206(13) 0.0189(13) 0.0139(11) -0.0003(10) 0.0006(10) 0.0018(11) C21 0.026(2) 0.021(2) 0.0188(18) 0.0036(15) 0.0036(15) 0.0025(17) C22 0.0145(18) 0.0237(19) 0.0172(18) 0.0018(15) 0.0017(14) -0.0027(15) C23 0.023(2) 0.022(2) 0.0220(18) -0.0009(16) 0.0023(15) -0.0017(16) C24 0.021(2) 0.033(2) 0.0134(18) -0.0036(16) 0.0011(15) 0.0005(17) C25 0.027(2) 0.028(2) 0.0170(18) 0.0020(16) 0.0027(16) -0.0013(17) C26 0.023(2) 0.022(2) 0.0241(19) -0.0004(16) 0.0010(16) -0.0011(16) N27 0.0177(16) 0.0175(16) 0.0206(15) -0.0001(12) 0.0041(13) -0.0020(13) O28 0.0261(16) 0.0336(17) 0.0251(15) -0.0005(14) 0.0039(12) -0.0059(14) C29 0.034(3) 0.044(3) 0.068(4) -0.011(3) -0.003(3) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O10 2.109(2) 4_655 ? Fe1 O10 2.117(3) . ? Fe1 N17 2.155(3) . ? Fe1 O10 2.163(3) 2_665 ? Fe1 O18 2.191(3) . ? Fe1 Cl1 2.4045(11) . ? O10 C11 1.405(4) . ? O10 Fe1 2.109(2) 3_565 ? O10 Fe1 2.163(3) 2_665 ? C11 C12 1.513(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N17 1.339(5) . ? C12 C13 1.398(5) . ? C13 C14 1.383(6) . ? C13 H13 0.9500 . ? C14 C15 1.386(6) . ? C14 H14 0.9500 . ? C15 C16 1.383(6) . ? C15 H15 0.9500 . ? C16 N17 1.347(5) . ? C16 H16 0.9500 . ? O18 C19 1.430(5) . ? O18 H18 0.86(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? Fe2 O20 2.112(3) 12 ? Fe2 O20 2.121(3) . ? Fe2 N27 2.160(3) . ? Fe2 O20 2.178(3) 2_565 ? Fe2 O28 2.199(3) . ? Fe2 Cl2 2.4080(11) . ? O20 C21 1.414(5) . ? O20 Fe2 2.112(3) 11_455 ? O20 Fe2 2.178(3) 2_565 ? C21 C22 1.527(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N27 1.334(5) . ? C22 C23 1.391(5) . ? C23 C24 1.380(6) . ? C23 H23 0.9500 . ? C24 C25 1.381(6) . ? C24 H24 0.9500 . ? C25 C26 1.381(5) . ? C25 H25 0.9500 . ? C26 N27 1.352(5) . ? C26 H26 0.9500 . ? O28 C29 1.439(6) . ? O28 H28 0.84(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Fe1 O10 82.95(10) 4_655 . ? O10 Fe1 N17 158.36(12) 4_655 . ? O10 Fe1 N17 76.24(11) . . ? O10 Fe1 O10 81.86(10) 4_655 2_665 ? O10 Fe1 O10 80.85(10) . 2_665 ? N17 Fe1 O10 100.38(11) . 2_665 ? O10 Fe1 O18 85.95(10) 4_655 . ? O10 Fe1 O18 92.23(11) . . ? N17 Fe1 O18 88.95(12) . . ? O10 Fe1 O18 166.62(10) 2_665 . ? O10 Fe1 Cl1 99.45(8) 4_655 . ? O10 Fe1 Cl1 174.71(8) . . ? N17 Fe1 Cl1 101.79(9) . . ? O10 Fe1 Cl1 94.78(7) 2_665 . ? O18 Fe1 Cl1 92.64(9) . . ? C11 O10 Fe1 126.9(2) . 3_565 ? C11 O10 Fe1 111.9(2) . . ? Fe1 O10 Fe1 97.57(10) 3_565 . ? C11 O10 Fe1 120.1(2) . 2_665 ? Fe1 O10 Fe1 96.17(10) 3_565 2_665 ? Fe1 O10 Fe1 98.90(10) . 2_665 ? O10 C11 C12 110.6(3) . . ? O10 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? O10 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N17 C12 C13 121.9(4) . . ? N17 C12 C11 116.3(3) . . ? C13 C12 C11 121.8(4) . . ? C14 C13 C12 118.7(4) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C15 119.2(4) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 119.2(4) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? N17 C16 C15 121.7(4) . . ? N17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C12 N17 C16 119.3(3) . . ? C12 N17 Fe1 113.7(2) . . ? C16 N17 Fe1 126.9(3) . . ? C19 O18 Fe1 128.4(3) . . ? C19 O18 H18 103(3) . . ? Fe1 O18 H18 113(3) . . ? O18 C19 H19A 109.5 . . ? O18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O20 Fe2 O20 83.05(11) 12 . ? O20 Fe2 N27 158.60(12) 12 . ? O20 Fe2 N27 76.45(11) . . ? O20 Fe2 O20 81.71(11) 12 2_565 ? O20 Fe2 O20 79.94(11) . 2_565 ? N27 Fe2 O20 100.45(11) . 2_565 ? O20 Fe2 O28 87.95(11) 12 . ? O20 Fe2 O28 91.29(12) . . ? N27 Fe2 O28 86.44(12) . . ? O20 Fe2 O28 167.14(11) 2_565 . ? O20 Fe2 Cl2 100.15(8) 12 . ? O20 Fe2 Cl2 173.07(8) . . ? N27 Fe2 Cl2 100.90(9) . . ? O20 Fe2 Cl2 94.38(8) 2_565 . ? O28 Fe2 Cl2 94.95(10) . . ? C21 O20 Fe2 127.6(2) . 11_455 ? C21 O20 Fe2 112.4(2) . . ? Fe2 O20 Fe2 97.59(11) 11_455 . ? C21 O20 Fe2 118.5(2) . 2_565 ? Fe2 O20 Fe2 95.87(11) 11_455 2_565 ? Fe2 O20 Fe2 99.90(11) . 2_565 ? O20 C21 C22 110.0(3) . . ? O20 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? O20 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? N27 C22 C23 122.4(4) . . ? N27 C22 C21 115.8(3) . . ? C23 C22 C21 121.8(4) . . ? C24 C23 C22 119.1(4) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 118.8(4) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C26 C25 C24 119.0(4) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? N27 C26 C25 122.5(4) . . ? N27 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C22 N27 C26 118.1(3) . . ? C22 N27 Fe2 114.8(3) . . ? C26 N27 Fe2 127.1(3) . . ? C29 O28 Fe2 129.7(3) . . ? C29 O28 H28 98(4) . . ? Fe2 O28 H28 116(4) . . ? O28 C29 H29A 109.5 . . ? O28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? 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 O10 Fe1 O10 C11 144.2(2) 4_655 . . . ? N17 Fe1 O10 C11 -29.8(2) . . . . ? O10 Fe1 O10 C11 -133.0(2) 2_665 . . . ? O18 Fe1 O10 C11 58.6(2) . . . . ? Cl1 Fe1 O10 C11 -98.5(8) . . . . ? O10 Fe1 O10 Fe1 9.31(10) 4_655 . . 3_565 ? N17 Fe1 O10 Fe1 -164.71(14) . . . 3_565 ? O10 Fe1 O10 Fe1 92.15(9) 2_665 . . 3_565 ? O18 Fe1 O10 Fe1 -76.33(11) . . . 3_565 ? Cl1 Fe1 O10 Fe1 126.6(8) . . . 3_565 ? O10 Fe1 O10 Fe1 -88.19(10) 4_655 . . 2_665 ? N17 Fe1 O10 Fe1 97.80(12) . . . 2_665 ? O10 Fe1 O10 Fe1 -5.34(13) 2_665 . . 2_665 ? O18 Fe1 O10 Fe1 -173.83(10) . . . 2_665 ? Cl1 Fe1 O10 Fe1 29.1(9) . . . 2_665 ? Fe1 O10 C11 C12 153.8(2) 3_565 . . . ? Fe1 O10 C11 C12 35.1(4) . . . . ? Fe1 O10 C11 C12 -80.1(4) 2_665 . . . ? O10 C11 C12 N17 -19.2(5) . . . . ? O10 C11 C12 C13 160.4(4) . . . . ? N17 C12 C13 C14 1.0(6) . . . . ? C11 C12 C13 C14 -178.6(4) . . . . ? C12 C13 C14 C15 -0.2(7) . . . . ? C13 C14 C15 C16 -0.3(7) . . . . ? C14 C15 C16 N17 0.2(7) . . . . ? C13 C12 N17 C16 -1.1(6) . . . . ? C11 C12 N17 C16 178.5(4) . . . . ? C13 C12 N17 Fe1 174.5(3) . . . . ? C11 C12 N17 Fe1 -5.9(4) . . . . ? C15 C16 N17 C12 0.5(6) . . . . ? C15 C16 N17 Fe1 -174.4(3) . . . . ? O10 Fe1 N17 C12 2.8(5) 4_655 . . . ? O10 Fe1 N17 C12 19.1(3) . . . . ? O10 Fe1 N17 C12 96.9(3) 2_665 . . . ? O18 Fe1 N17 C12 -73.4(3) . . . . ? Cl1 Fe1 N17 C12 -165.9(3) . . . . ? O10 Fe1 N17 C16 178.0(3) 4_655 . . . ? O10 Fe1 N17 C16 -165.7(4) . . . . ? O10 Fe1 N17 C16 -87.9(3) 2_665 . . . ? O18 Fe1 N17 C16 101.7(3) . . . . ? Cl1 Fe1 N17 C16 9.3(3) . . . . ? O10 Fe1 O18 C19 -177.7(3) 4_655 . . . ? O10 Fe1 O18 C19 -94.9(3) . . . . ? N17 Fe1 O18 C19 -18.7(3) . . . . ? O10 Fe1 O18 C19 -153.3(4) 2_665 . . . ? Cl1 Fe1 O18 C19 83.1(3) . . . . ? O20 Fe2 O20 C21 -146.5(3) 12 . . . ? N27 Fe2 O20 C21 27.3(2) . . . . ? O20 Fe2 O20 C21 130.8(2) 2_565 . . . ? O28 Fe2 O20 C21 -58.7(2) . . . . ? Cl2 Fe2 O20 C21 95.6(7) . . . . ? O20 Fe2 O20 Fe2 -10.34(11) 12 . . 11_455 ? N27 Fe2 O20 Fe2 163.46(14) . . . 11_455 ? O20 Fe2 O20 Fe2 -93.11(10) 2_565 . . 11_455 ? O28 Fe2 O20 Fe2 77.43(12) . . . 11_455 ? Cl2 Fe2 O20 Fe2 -128.3(6) . . . 11_455 ? O20 Fe2 O20 Fe2 87.01(11) 12 . . 2_565 ? N27 Fe2 O20 Fe2 -99.19(13) . . . 2_565 ? O20 Fe2 O20 Fe2 4.24(14) 2_565 . . 2_565 ? O28 Fe2 O20 Fe2 174.78(12) . . . 2_565 ? Cl2 Fe2 O20 Fe2 -31.0(8) . . . 2_565 ? Fe2 O20 C21 C22 -155.6(2) 11_455 . . . ? Fe2 O20 C21 C22 -35.8(4) . . . . ? Fe2 O20 C21 C22 80.0(3) 2_565 . . . ? O20 C21 C22 N27 25.0(5) . . . . ? O20 C21 C22 C23 -156.9(4) . . . . ? N27 C22 C23 C24 0.7(6) . . . . ? C21 C22 C23 C24 -177.3(4) . . . . ? C22 C23 C24 C25 0.4(6) . . . . ? C23 C24 C25 C26 -1.1(6) . . . . ? C24 C25 C26 N27 0.9(7) . . . . ? C23 C22 N27 C26 -1.0(6) . . . . ? C21 C22 N27 C26 177.2(4) . . . . ? C23 C22 N27 Fe2 179.8(3) . . . . ? C21 C22 N27 Fe2 -2.1(4) . . . . ? C25 C26 N27 C22 0.1(6) . . . . ? C25 C26 N27 Fe2 179.3(3) . . . . ? O20 Fe2 N27 C22 3.7(5) 12 . . . ? O20 Fe2 N27 C22 -13.4(3) . . . . ? O20 Fe2 N27 C22 -90.2(3) 2_565 . . . ? O28 Fe2 N27 C22 78.8(3) . . . . ? Cl2 Fe2 N27 C22 173.2(3) . . . . ? O20 Fe2 N27 C26 -175.5(3) 12 . . . ? O20 Fe2 N27 C26 167.5(4) . . . . ? O20 Fe2 N27 C26 90.6(3) 2_565 . . . ? O28 Fe2 N27 C26 -100.4(3) . . . . ? Cl2 Fe2 N27 C26 -6.0(4) . . . . ? O20 Fe2 O28 C29 -94.7(4) 12 . . . ? O20 Fe2 O28 C29 -177.7(4) . . . . ? N27 Fe2 O28 C29 105.9(4) . . . . ? O20 Fe2 O28 C29 -131.1(6) 2_565 . . . ? Cl2 Fe2 O28 C29 5.3(4) . . . . ? 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 O18 H18 Cl1 0.86(4) 2.22(4) 3.056(3) 163(4) 3_565 O28 H28 Cl2 0.84(5) 2.25(5) 3.043(4) 157(5) 11_455 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.606 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.103 data_fefpll _database_code_depnum_ccdc_archive 'CCDC 820009' _nottingham_internal_coll_name FEFPLL _nottingham_internal_coll_number 9444 _nottingham_internal_coll_client FP/JVS _nottingham_internal_coll_type hemisphere _nottingham_internal_coll_frame_time '30 s' _nottingham_internal_coll_frame_width '0.3 degrees' _nottingham_internal_coll_frame_method \w _nottingham_internal_coll_user FP _nottingham_internal_coll_date 25/05/2010 _nottingham_internal_process_user FP _nottingham_internal_process_date 13/09/2010 _nottingham_internal_solution_user FP _nottingham_internal_solution_date 13/09/2010 _nottingham_internal_refinement_user FP/SPA _nottingham_internal_refinement_date 15/09/2010 _nottingham_internal_validation_user ? _nottingham_internal_validation_date ? _nottingham_internal_archive_date ? _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 ethyl groups of ethanol moieties B and D were found to be disordered over two positions. The occupancies of the major components were found to be 0.83(1) and 0.52(1) respectively. The oxygens are pivot atoms in the disorder models; they formally have different positions in different components, but these turned out to be too close to distinguish, so they were treated as having the same positions in both components. The two atoms of the minor component of residue B were modelled isotropically. All other non-hydrogen atoms were modelled anisotropically. Geometric similarity restraints (SADI) were applied to the 1,2 and 1,3 of all the ethanol moieties. All hydrogen atoms except for those on the hydroxy groups of the ethanol moieties were refined using riding models. The four ethanol hydroxy hydrogens were located in the difference map and refined with thermal parameters fixed at 1.5 times that of their parent oxygen atoms. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H48 Cl4 Fe4 N4 O8' _chemical_formula_sum 'C32 H48 Cl4 Fe4 N4 O8' _chemical_formula_weight 981.94 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.8291(6) _cell_length_b 16.4962(6) _cell_length_c 29.6189(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8222.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 22939 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.53 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.202 _exptl_crystal_size_mid 0.195 _exptl_crystal_size_min 0.152 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 1.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 49721 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.54 _reflns_number_total 9452 _reflns_number_gt 8504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' ?' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0388P)^2^+6.0350P] 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 9452 _refine_ls_number_parameters 515 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1A Fe 0.119026(15) 0.280781(16) 0.337676(8) 0.01543(7) Uani 1 1 d . . . Cl2A Cl 0.24862(3) 0.22410(3) 0.327223(16) 0.02424(10) Uani 1 1 d . . . N11A N 0.08900(9) 0.31729(10) 0.26951(5) 0.0189(3) Uani 1 1 d . . . C12A C 0.02077(11) 0.35920(12) 0.26614(6) 0.0207(4) Uani 1 1 d . . . C13A C -0.00882(13) 0.38510(13) 0.22488(7) 0.0266(4) Uani 1 1 d . . . H13A H -0.0570 0.4150 0.2234 0.032 Uiso 1 1 calc R . . C14A C 0.03271(14) 0.36695(14) 0.18583(7) 0.0314(5) Uani 1 1 d . . . H14A H 0.0134 0.3839 0.1572 0.038 Uiso 1 1 calc R . . C15A C 0.10295(14) 0.32354(14) 0.18927(7) 0.0300(5) Uani 1 1 d . . . H15A H 0.1326 0.3102 0.1630 0.036 Uiso 1 1 calc R . . C16A C 0.12917(12) 0.29989(12) 0.23147(6) 0.0226(4) Uani 1 1 d . . . H16A H 0.1774 0.2702 0.2337 0.027 Uiso 1 1 calc R . . C17A C -0.02114(12) 0.37667(13) 0.31038(7) 0.0243(4) Uani 1 1 d . . . H17A H -0.0051 0.4307 0.3217 0.029 Uiso 1 1 calc R . . H17B H -0.0793 0.3772 0.3055 0.029 Uiso 1 1 calc R . . O18A O -0.00149(7) 0.31674(8) 0.34274(4) 0.0183(3) Uani 1 1 d . . . O21A O 0.16157(9) 0.40349(8) 0.35088(5) 0.0237(3) Uani 1 1 d D . . H21A H 0.1368(16) 0.4232(16) 0.3678(9) 0.036 Uiso 1 1 d . . . C22A C 0.19180(12) 0.46373(12) 0.32056(7) 0.0268(4) Uani 1 1 d D . . H22A H 0.1971 0.5162 0.3365 0.032 Uiso 1 1 calc R . . H22B H 0.1544 0.4712 0.2951 0.032 Uiso 1 1 calc R . . C23A C 0.27118(12) 0.43738(14) 0.30303(8) 0.0331(5) Uani 1 1 d D . . H23A H 0.3082 0.4311 0.3283 0.050 Uiso 1 1 calc R . . H23B H 0.2917 0.4783 0.2821 0.050 Uiso 1 1 calc R . . H23C H 0.2656 0.3855 0.2872 0.050 Uiso 1 1 calc R . . Fe1B Fe -0.057939(16) 0.199187(18) 0.338939(9) 0.01978(7) Uani 1 1 d . A . Cl2B Cl -0.19057(3) 0.25322(4) 0.332425(18) 0.03899(15) Uani 1 1 d . . . N11B N -0.03302(10) 0.16432(10) 0.26993(5) 0.0201(3) Uani 1 1 d . . . C12B C 0.03278(11) 0.11920(11) 0.26520(6) 0.0196(4) Uani 1 1 d . . . C13B C 0.05512(12) 0.08737(12) 0.22354(7) 0.0237(4) Uani 1 1 d . . . H13B H 0.1021 0.0557 0.2209 0.028 Uiso 1 1 calc R . . C14B C 0.00834(13) 0.10224(13) 0.18601(7) 0.0259(4) Uani 1 1 d . . . H14B H 0.0227 0.0811 0.1573 0.031 Uiso 1 1 calc R . . C15B C -0.05984(12) 0.14865(13) 0.19104(7) 0.0243(4) Uani 1 1 d . . . H15B H -0.0932 0.1596 0.1659 0.029 Uiso 1 1 calc R . . C16B C -0.07842(12) 0.17863(13) 0.23329(6) 0.0225(4) Uani 1 1 d . . . H16B H -0.1250 0.2106 0.2367 0.027 Uiso 1 1 calc R . . C17B C 0.08048(11) 0.10395(12) 0.30765(6) 0.0201(4) Uani 1 1 d . . . H17C H 0.0687 0.0489 0.3192 0.024 Uiso 1 1 calc R . . H17D H 0.1379 0.1066 0.3005 0.024 Uiso 1 1 calc R . . O18B O 0.06204(7) 0.16185(8) 0.34108(4) 0.0171(3) Uani 1 1 d . . . O21B O -0.09423(10) 0.07287(11) 0.34771(6) 0.0366(4) Uani 1 1 d D . . H21B H -0.075(2) 0.058(2) 0.3661(11) 0.055 Uiso 1 1 d . . . C22B C -0.17051(15) 0.03812(19) 0.35024(9) 0.0349(8) Uani 0.834(6) 1 d PD A 1 H22C H -0.2052 0.0724 0.3693 0.042 Uiso 0.834(6) 1 calc PR A 1 H22D H -0.1670 -0.0161 0.3644 0.042 Uiso 0.834(6) 1 calc PR A 1 C23B C -0.2058(2) 0.0305(3) 0.30378(10) 0.0438(9) Uani 0.834(6) 1 d PD A 1 H23D H -0.2148 0.0847 0.2912 0.066 Uiso 0.834(6) 1 calc PR A 1 H23E H -0.2565 0.0015 0.3056 0.066 Uiso 0.834(6) 1 calc PR A 1 H23F H -0.1692 0.0005 0.2843 0.066 Uiso 0.834(6) 1 calc PR A 1 C22F C -0.1463(5) 0.0258(6) 0.3207(4) 0.025(3) Uiso 0.166(6) 1 d PD A 2 H22E H -0.1611 -0.0236 0.3378 0.030 Uiso 0.166(6) 1 calc PR A 2 H22F H -0.1172 0.0081 0.2934 0.030 Uiso 0.166(6) 1 calc PR A 2 C23F C -0.2204(7) 0.0679(10) 0.3064(6) 0.044(5) Uiso 0.166(6) 1 d PD A 2 H23G H -0.2480 0.0890 0.3331 0.066 Uiso 0.166(6) 1 calc PR A 2 H23H H -0.2550 0.0296 0.2905 0.066 Uiso 0.166(6) 1 calc PR A 2 H23I H -0.2069 0.1129 0.2862 0.066 Uiso 0.166(6) 1 calc PR A 2 Fe1C Fe 0.072643(15) 0.146975(16) 0.411818(8) 0.01542(7) Uani 1 1 d . A . Cl2C Cl 0.01899(3) 0.01292(3) 0.420244(17) 0.02654(11) Uani 1 1 d . . . N11C N 0.10849(9) 0.17560(9) 0.48032(5) 0.0168(3) Uani 1 1 d . . . C12C C 0.15354(10) 0.24274(11) 0.48361(6) 0.0172(3) Uani 1 1 d . . . C13C C 0.18529(12) 0.26802(12) 0.52452(7) 0.0229(4) Uani 1 1 d . . . H13C H 0.2176 0.3152 0.5259 0.028 Uiso 1 1 calc R . . C14C C 0.16949(13) 0.22404(14) 0.56321(7) 0.0288(5) Uani 1 1 d . . . H14C H 0.1909 0.2402 0.5915 0.035 Uiso 1 1 calc R . . C15C C 0.12163(12) 0.15564(13) 0.55981(7) 0.0266(4) Uani 1 1 d . . . H15C H 0.1090 0.1248 0.5859 0.032 Uiso 1 1 calc R . . C16C C 0.09261(11) 0.13303(12) 0.51806(6) 0.0206(4) Uani 1 1 d . . . H16C H 0.0604 0.0859 0.5159 0.025 Uiso 1 1 calc R . . C17C C 0.16769(11) 0.28864(11) 0.44027(6) 0.0185(4) Uani 1 1 d . . . H17E H 0.1674 0.3476 0.4464 0.022 Uiso 1 1 calc R . . H17F H 0.2204 0.2741 0.4279 0.022 Uiso 1 1 calc R . . O18C O 0.10796(7) 0.26983(7) 0.40832(4) 0.0154(2) Uani 1 1 d . . . O21C O 0.19355(8) 0.10552(8) 0.39916(5) 0.0219(3) Uani 1 1 d D . . H21C H 0.2133(15) 0.1349(16) 0.3800(9) 0.033 Uiso 1 1 d . . . C22C C 0.25406(12) 0.07799(12) 0.42957(7) 0.0256(4) Uani 1 1 d D . . H22G H 0.2612 0.1179 0.4542 0.031 Uiso 1 1 calc R . . H22H H 0.3051 0.0725 0.4133 0.031 Uiso 1 1 calc R . . C23C C 0.23002(14) -0.00268(13) 0.44897(8) 0.0328(5) Uani 1 1 d D . . H23J H 0.1806 0.0035 0.4661 0.049 Uiso 1 1 calc R . . H23K H 0.2720 -0.0225 0.4690 0.049 Uiso 1 1 calc R . . H23L H 0.2218 -0.0416 0.4244 0.049 Uiso 1 1 calc R . . Fe1D Fe -0.007515(15) 0.327476(16) 0.413826(9) 0.01697(7) Uani 1 1 d . A . Cl2D Cl 0.04590(3) 0.46176(3) 0.423688(18) 0.02980(12) Uani 1 1 d . . . N11D N -0.04164(9) 0.29837(10) 0.48255(5) 0.0191(3) Uani 1 1 d . . . C12D C -0.08377(11) 0.22936(11) 0.48664(6) 0.0189(4) Uani 1 1 d . . . C13D C -0.11074(12) 0.20213(12) 0.52827(7) 0.0223(4) Uani 1 1 d . . . H13D H -0.1402 0.1532 0.5304 0.027 Uiso 1 1 calc R . . C14D C -0.09423(12) 0.24695(13) 0.56650(7) 0.0261(4) Uani 1 1 d . . . H14D H -0.1120 0.2292 0.5953 0.031 Uiso 1 1 calc R . . C15D C -0.05134(13) 0.31836(13) 0.56219(7) 0.0269(4) Uani 1 1 d . . . H15D H -0.0395 0.3505 0.5879 0.032 Uiso 1 1 calc R . . C16D C -0.02610(12) 0.34191(12) 0.51978(7) 0.0227(4) Uani 1 1 d . . . H16D H 0.0034 0.3908 0.5169 0.027 Uiso 1 1 calc R . . C17D C -0.10049(11) 0.18438(13) 0.44325(6) 0.0226(4) Uani 1 1 d . A . H17G H -0.0988 0.1253 0.4489 0.027 Uiso 1 1 calc R . . H17H H -0.1544 0.1983 0.4324 0.027 Uiso 1 1 calc R . . O18D O -0.04401(8) 0.20466(8) 0.40984(4) 0.0183(3) Uani 1 1 d . . . O21D O -0.12859(10) 0.36894(12) 0.40473(6) 0.0397(4) Uani 1 1 d D . . H21D H -0.149(2) 0.346(2) 0.3884(12) 0.060 Uiso 1 1 d . . . C23D C -0.1560(4) 0.5139(3) 0.4216(3) 0.079(3) Uani 0.525(7) 1 d PD A 1 H23M H -0.0990 0.5254 0.4242 0.118 Uiso 0.525(7) 1 calc PR A 1 H23N H -0.1855 0.5483 0.4427 0.118 Uiso 0.525(7) 1 calc PR A 1 H23O H -0.1736 0.5251 0.3906 0.118 Uiso 0.525(7) 1 calc PR A 1 C22D C -0.1709(3) 0.4273(3) 0.43243(16) 0.0378(13) Uani 0.525(7) 1 d PD A 1 H22I H -0.1563 0.4179 0.4644 0.045 Uiso 0.525(7) 1 calc PR A 1 H22J H -0.2286 0.4167 0.4295 0.045 Uiso 0.525(7) 1 calc PR A 1 C23H C -0.1795(4) 0.4759(4) 0.44553(18) 0.0498(17) Uani 0.475(7) 1 d PD A 2 H23P H -0.2150 0.4401 0.4625 0.075 Uiso 0.475(7) 1 calc PR A 2 H23Q H -0.2033 0.5300 0.4433 0.075 Uiso 0.475(7) 1 calc PR A 2 H23R H -0.1283 0.4798 0.4612 0.075 Uiso 0.475(7) 1 calc PR A 2 C22H C -0.1669(3) 0.4422(3) 0.39916(16) 0.0392(15) Uani 0.475(7) 1 d PD A 2 H22K H -0.2185 0.4343 0.3837 0.047 Uiso 0.475(7) 1 calc PR A 2 H22L H -0.1340 0.4796 0.3809 0.047 Uiso 0.475(7) 1 calc PR A 2 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 Fe1A 0.01498(13) 0.01915(13) 0.01217(13) 0.00282(9) 0.00127(9) 0.00339(9) Cl2A 0.0185(2) 0.0311(2) 0.0232(2) 0.00809(19) 0.00570(18) 0.00764(17) N11A 0.0193(7) 0.0220(8) 0.0155(7) 0.0034(6) 0.0018(6) 0.0030(6) C12A 0.0228(9) 0.0221(9) 0.0171(9) 0.0048(7) 0.0018(7) 0.0030(7) C13A 0.0275(10) 0.0316(11) 0.0208(10) 0.0068(8) -0.0002(8) 0.0098(8) C14A 0.0380(12) 0.0402(12) 0.0161(10) 0.0076(9) -0.0013(9) 0.0088(10) C15A 0.0366(12) 0.0383(12) 0.0150(9) 0.0027(8) 0.0060(8) 0.0091(9) C16A 0.0244(9) 0.0256(9) 0.0177(9) 0.0026(8) 0.0044(8) 0.0042(7) C17A 0.0237(9) 0.0317(10) 0.0174(9) 0.0071(8) 0.0040(8) 0.0128(8) O18A 0.0172(6) 0.0244(7) 0.0134(6) 0.0049(5) 0.0022(5) 0.0053(5) O21A 0.0270(7) 0.0233(7) 0.0209(7) 0.0017(6) 0.0089(6) -0.0020(6) C22A 0.0329(11) 0.0250(10) 0.0224(10) 0.0038(8) 0.0035(8) -0.0052(8) C23A 0.0301(11) 0.0375(12) 0.0318(12) 0.0037(10) 0.0082(9) -0.0093(9) Fe1B 0.01583(13) 0.03186(16) 0.01164(13) -0.00073(10) 0.00019(9) -0.00004(10) Cl2B 0.0163(2) 0.0778(4) 0.0229(3) -0.0023(3) -0.00228(19) 0.0088(2) N11B 0.0196(8) 0.0263(8) 0.0145(8) -0.0009(6) -0.0011(6) -0.0004(6) C12B 0.0232(9) 0.0207(9) 0.0148(9) 0.0002(7) -0.0014(7) 0.0000(7) C13B 0.0285(10) 0.0241(9) 0.0185(9) -0.0023(8) -0.0012(8) 0.0059(8) C14B 0.0343(11) 0.0307(10) 0.0127(9) -0.0034(8) 0.0003(8) 0.0029(8) C15B 0.0262(10) 0.0319(10) 0.0147(9) 0.0010(8) -0.0047(8) 0.0006(8) C16B 0.0196(9) 0.0315(10) 0.0163(9) 0.0010(8) -0.0019(7) 0.0012(8) C17B 0.0240(9) 0.0225(9) 0.0139(8) -0.0026(7) -0.0025(7) 0.0045(7) O18B 0.0190(6) 0.0210(6) 0.0112(6) -0.0012(5) -0.0001(5) 0.0016(5) O21B 0.0401(9) 0.0477(10) 0.0222(8) 0.0061(7) -0.0105(7) -0.0206(8) C22B 0.0264(13) 0.0460(17) 0.0323(16) 0.0023(12) -0.0036(11) -0.0106(12) C23B 0.0387(18) 0.058(2) 0.0344(17) -0.0083(16) -0.0127(13) -0.0127(16) Fe1C 0.01775(13) 0.01713(13) 0.01138(12) 0.00063(9) -0.00094(9) -0.00168(9) Cl2C 0.0352(3) 0.0223(2) 0.0221(2) 0.00276(18) -0.00096(19) -0.00907(19) N11C 0.0180(7) 0.0195(7) 0.0129(7) 0.0011(6) 0.0003(6) 0.0007(6) C12C 0.0156(8) 0.0217(9) 0.0143(8) 0.0010(7) 0.0004(7) 0.0016(7) C13C 0.0213(9) 0.0291(10) 0.0184(9) -0.0004(8) -0.0022(7) -0.0051(8) C14C 0.0310(11) 0.0420(12) 0.0135(9) 0.0001(8) -0.0055(8) -0.0067(9) C15C 0.0295(10) 0.0358(11) 0.0145(9) 0.0065(8) -0.0006(8) -0.0051(8) C16C 0.0219(9) 0.0236(9) 0.0164(9) 0.0037(7) 0.0006(7) -0.0008(7) C17C 0.0187(8) 0.0215(9) 0.0152(8) 0.0019(7) -0.0020(7) -0.0039(7) O18C 0.0160(6) 0.0178(6) 0.0124(6) 0.0011(5) -0.0012(5) -0.0002(5) O21C 0.0213(7) 0.0236(7) 0.0207(7) 0.0060(6) 0.0000(5) 0.0044(5) C22C 0.0245(9) 0.0264(10) 0.0258(10) 0.0030(8) -0.0032(8) 0.0071(8) C23C 0.0377(12) 0.0292(11) 0.0315(12) 0.0094(9) 0.0001(10) 0.0111(9) Fe1D 0.01681(13) 0.02065(14) 0.01345(13) 0.00165(10) 0.00303(9) 0.00182(10) Cl2D 0.0389(3) 0.0185(2) 0.0320(3) -0.00137(19) 0.0158(2) -0.00016(19) N11D 0.0191(8) 0.0220(8) 0.0161(8) -0.0005(6) 0.0027(6) 0.0005(6) C12D 0.0169(8) 0.0250(9) 0.0147(9) -0.0002(7) 0.0017(7) -0.0001(7) C13D 0.0214(9) 0.0267(10) 0.0188(9) 0.0008(8) 0.0043(7) -0.0019(7) C14D 0.0307(11) 0.0325(11) 0.0151(9) 0.0010(8) 0.0055(8) 0.0006(9) C15D 0.0326(11) 0.0310(11) 0.0170(9) -0.0059(8) 0.0027(8) 0.0003(8) C16D 0.0257(10) 0.0238(9) 0.0185(9) -0.0028(7) 0.0040(8) 0.0001(7) C17D 0.0191(9) 0.0326(10) 0.0162(9) -0.0020(8) 0.0035(7) -0.0071(8) O18D 0.0164(6) 0.0270(7) 0.0114(6) -0.0008(5) 0.0020(5) -0.0020(5) O21D 0.0271(8) 0.0608(12) 0.0310(9) -0.0064(8) 0.0011(7) 0.0219(8) C23D 0.045(4) 0.065(4) 0.127(8) -0.041(5) -0.012(4) 0.021(3) C22D 0.036(2) 0.043(3) 0.034(3) 0.003(2) 0.017(2) 0.020(2) C23H 0.046(4) 0.057(5) 0.046(4) -0.009(3) 0.014(3) 0.005(3) C22H 0.038(3) 0.041(3) 0.039(3) 0.003(2) -0.003(2) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1A O18C 2.1085(12) . ? Fe1A O18A 2.1184(13) . ? Fe1A N11A 2.1667(16) . ? Fe1A O21A 2.1824(14) . ? Fe1A O18B 2.1861(13) . ? Fe1A Cl2A 2.3930(5) . ? N11A C12A 1.344(2) . ? N11A C16A 1.345(2) . ? C12A C13A 1.387(3) . ? C12A C17A 1.516(3) . ? C13A C14A 1.384(3) . ? C13A H13A 0.9500 . ? C14A C15A 1.386(3) . ? C14A H14A 0.9500 . ? C15A C16A 1.382(3) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C17A O18A 1.416(2) . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? O18A Fe1D 2.1154(13) . ? O18A Fe1B 2.1623(14) . ? O21A C22A 1.433(2) . ? O21A H21A 0.73(3) . ? C22A C23A 1.498(3) . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? Fe1B O18B 2.1120(13) . ? Fe1B O18D 2.1150(13) . ? Fe1B N11B 2.1643(16) . ? Fe1B O21B 2.1870(18) . ? Fe1B Cl2B 2.4112(6) . ? N11B C12B 1.342(2) . ? N11B C16B 1.348(2) . ? C12B C13B 1.393(3) . ? C12B C17B 1.513(2) . ? C13B C14B 1.384(3) . ? C13B H13B 0.9500 . ? C14B C15B 1.387(3) . ? C14B H14B 0.9500 . ? C15B C16B 1.381(3) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? C17B O18B 1.410(2) . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? O18B Fe1C 2.1171(12) . ? O21B C22B 1.408(3) . ? O21B C22F 1.418(4) . ? O21B H21B 0.67(3) . ? C22B C23B 1.504(3) . ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C22F C23F 1.490(5) . ? C22F H22E 0.9900 . ? C22F H22F 0.9900 . ? C23F H23G 0.9800 . ? C23F H23H 0.9800 . ? C23F H23I 0.9800 . ? Fe1C O18C 2.1146(13) . ? Fe1C N11C 2.1688(15) . ? Fe1C O21C 2.1791(13) . ? Fe1C O18D 2.1824(13) . ? Fe1C Cl2C 2.4017(5) . ? N11C C12C 1.346(2) . ? N11C C16C 1.347(2) . ? C12C C13C 1.388(3) . ? C12C C17C 1.509(2) . ? C13C C14C 1.382(3) . ? C13C H13C 0.9500 . ? C14C C15C 1.390(3) . ? C14C H14C 0.9500 . ? C15C C16C 1.381(3) . ? C15C H15C 0.9500 . ? C16C H16C 0.9500 . ? C17C O18C 1.415(2) . ? C17C H17E 0.9900 . ? C17C H17F 0.9900 . ? O18C Fe1D 2.1696(13) . ? O21C C22C 1.433(2) . ? O21C H21C 0.82(3) . ? C22C C23C 1.505(3) . ? C22C H22G 0.9900 . ? C22C H22H 0.9900 . ? C23C H23J 0.9800 . ? C23C H23K 0.9800 . ? C23C H23L 0.9800 . ? Fe1D O18D 2.1203(14) . ? Fe1D O21D 2.1661(16) . ? Fe1D N11D 2.1689(16) . ? Fe1D Cl2D 2.4084(6) . ? N11D C16D 1.342(2) . ? N11D C12D 1.347(2) . ? C12D C13D 1.389(3) . ? C12D C17D 1.510(3) . ? C13D C14D 1.381(3) . ? C13D H13D 0.9500 . ? C14D C15D 1.387(3) . ? C14D H14D 0.9500 . ? C15D C16D 1.382(3) . ? C15D H15D 0.9500 . ? C16D H16D 0.9500 . ? C17D O18D 1.412(2) . ? C17D H17G 0.9900 . ? C17D H17H 0.9900 . ? O21D C22H 1.380(3) . ? O21D C22D 1.451(3) . ? O21D H21D 0.70(3) . ? C23D C22D 1.486(4) . ? C23D H23M 0.9800 . ? C23D H23N 0.9800 . ? C23D H23O 0.9800 . ? C22D H22I 0.9900 . ? C22D H22J 0.9900 . ? C23H C22H 1.497(4) . ? C23H H23P 0.9800 . ? C23H H23Q 0.9800 . ? C23H H23R 0.9800 . ? C22H H22K 0.9900 . ? C22H H22L 0.9900 . ? 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 O18C Fe1A O18A 82.48(5) . . ? O18C Fe1A N11A 158.12(5) . . ? O18A Fe1A N11A 76.40(5) . . ? O18C Fe1A O21A 86.02(5) . . ? O18A Fe1A O21A 92.39(5) . . ? N11A Fe1A O21A 89.18(6) . . ? O18C Fe1A O18B 80.71(5) . . ? O18A Fe1A O18B 80.10(5) . . ? N11A Fe1A O18B 100.96(5) . . ? O21A Fe1A O18B 165.47(5) . . ? O18C Fe1A Cl2A 100.10(4) . . ? O18A Fe1A Cl2A 172.35(4) . . ? N11A Fe1A Cl2A 101.57(4) . . ? O21A Fe1A Cl2A 94.97(4) . . ? O18B Fe1A Cl2A 93.16(4) . . ? C12A N11A C16A 118.49(16) . . ? C12A N11A Fe1A 114.29(12) . . ? C16A N11A Fe1A 127.17(13) . . ? N11A C12A C13A 122.05(18) . . ? N11A C12A C17A 115.54(16) . . ? C13A C12A C17A 122.41(17) . . ? C14A C13A C12A 119.23(19) . . ? C14A C13A H13A 120.4 . . ? C12A C13A H13A 120.4 . . ? C13A C14A C15A 118.75(19) . . ? C13A C14A H14A 120.6 . . ? C15A C14A H14A 120.6 . . ? C16A C15A C14A 119.00(19) . . ? C16A C15A H15A 120.5 . . ? C14A C15A H15A 120.5 . . ? N11A C16A C15A 122.49(18) . . ? N11A C16A H16A 118.8 . . ? C15A C16A H16A 118.8 . . ? O18A C17A C12A 110.10(15) . . ? O18A C17A H17A 109.6 . . ? C12A C17A H17A 109.6 . . ? O18A C17A H17B 109.6 . . ? C12A C17A H17B 109.6 . . ? H17A C17A H17B 108.2 . . ? C17A O18A Fe1D 127.16(12) . . ? C17A O18A Fe1A 111.79(11) . . ? Fe1D O18A Fe1A 98.04(5) . . ? C17A O18A Fe1B 119.22(12) . . ? Fe1D O18A Fe1B 96.07(5) . . ? Fe1A O18A Fe1B 99.55(5) . . ? C22A O21A Fe1A 130.35(12) . . ? C22A O21A H21A 109(2) . . ? Fe1A O21A H21A 110(2) . . ? O21A C22A C23A 109.43(17) . . ? O21A C22A H22A 109.8 . . ? C23A C22A H22A 109.8 . . ? O21A C22A H22B 109.8 . . ? C23A C22A H22B 109.8 . . ? H22A C22A H22B 108.2 . . ? C22A C23A H23A 109.5 . . ? C22A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? C22A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? O18B Fe1B O18D 82.92(5) . . ? O18B Fe1B O18A 80.79(5) . . ? O18D Fe1B O18A 82.03(5) . . ? O18B Fe1B N11B 76.44(5) . . ? O18D Fe1B N11B 158.06(6) . . ? O18A Fe1B N11B 101.68(6) . . ? O18B Fe1B O21B 89.17(6) . . ? O18D Fe1B O21B 87.35(6) . . ? O18A Fe1B O21B 166.17(6) . . ? N11B Fe1B O21B 85.01(6) . . ? O18B Fe1B Cl2B 174.41(4) . . ? O18D Fe1B Cl2B 99.57(4) . . ? O18A Fe1B Cl2B 94.55(4) . . ? N11B Fe1B Cl2B 101.65(5) . . ? O21B Fe1B Cl2B 95.92(5) . . ? C12B N11B C16B 118.74(17) . . ? C12B N11B Fe1B 113.95(12) . . ? C16B N11B Fe1B 127.15(13) . . ? N11B C12B C13B 121.63(17) . . ? N11B C12B C17B 116.33(16) . . ? C13B C12B C17B 122.03(17) . . ? C14B C13B C12B 119.42(18) . . ? C14B C13B H13B 120.3 . . ? C12B C13B H13B 120.3 . . ? C13B C14B C15B 118.81(18) . . ? C13B C14B H14B 120.6 . . ? C15B C14B H14B 120.6 . . ? C16B C15B C14B 118.82(18) . . ? C16B C15B H15B 120.6 . . ? C14B C15B H15B 120.6 . . ? N11B C16B C15B 122.57(18) . . ? N11B C16B H16B 118.7 . . ? C15B C16B H16B 118.7 . . ? O18B C17B C12B 110.74(15) . . ? O18B C17B H17C 109.5 . . ? C12B C17B H17C 109.5 . . ? O18B C17B H17D 109.5 . . ? C12B C17B H17D 109.5 . . ? H17C C17B H17D 108.1 . . ? C17B O18B Fe1B 112.75(11) . . ? C17B O18B Fe1C 126.71(11) . . ? Fe1B O18B Fe1C 98.28(5) . . ? C17B O18B Fe1A 118.62(11) . . ? Fe1B O18B Fe1A 98.99(5) . . ? Fe1C O18B Fe1A 96.47(5) . . ? C22B O21B C22F 40.9(5) . . ? C22B O21B Fe1B 130.46(18) . . ? C22F O21B Fe1B 128.9(5) . . ? C22B O21B H21B 104(3) . . ? C22F O21B H21B 124(3) . . ? Fe1B O21B H21B 108(3) . . ? O21B C22B C23B 110.2(2) . . ? O21B C22B H22C 109.6 . . ? C23B C22B H22C 109.6 . . ? O21B C22B H22D 109.6 . . ? C23B C22B H22D 109.6 . . ? H22C C22B H22D 108.1 . . ? O21B C22F C23F 114.9(6) . . ? O21B C22F H22E 108.5 . . ? C23F C22F H22E 108.5 . . ? O21B C22F H22F 108.5 . . ? C23F C22F H22F 108.5 . . ? H22E C22F H22F 107.5 . . ? C22F C23F H23G 109.5 . . ? C22F C23F H23H 109.5 . . ? H23G C23F H23H 109.5 . . ? C22F C23F H23I 109.5 . . ? H23G C23F H23I 109.5 . . ? H23H C23F H23I 109.5 . . ? O18C Fe1C O18B 82.19(5) . . ? O18C Fe1C N11C 76.05(5) . . ? O18B Fe1C N11C 157.53(6) . . ? O18C Fe1C O21C 91.72(5) . . ? O18B Fe1C O21C 86.83(5) . . ? N11C Fe1C O21C 88.26(5) . . ? O18C Fe1C O18D 80.42(5) . . ? O18B Fe1C O18D 81.21(5) . . ? N11C Fe1C O18D 100.39(5) . . ? O21C Fe1C O18D 166.45(5) . . ? O18C Fe1C Cl2C 173.35(4) . . ? O18B Fe1C Cl2C 100.25(4) . . ? N11C Fe1C Cl2C 102.00(4) . . ? O21C Fe1C Cl2C 94.58(4) . . ? O18D Fe1C Cl2C 93.79(4) . . ? C12C N11C C16C 118.74(16) . . ? C12C N11C Fe1C 113.80(12) . . ? C16C N11C Fe1C 127.43(13) . . ? N11C C12C C13C 121.81(17) . . ? N11C C12C C17C 116.12(15) . . ? C13C C12C C17C 122.07(17) . . ? C14C C13C C12C 119.47(18) . . ? C14C C13C H13C 120.3 . . ? C12C C13C H13C 120.3 . . ? C13C C14C C15C 118.53(18) . . ? C13C C14C H14C 120.7 . . ? C15C C14C H14C 120.7 . . ? C16C C15C C14C 119.28(19) . . ? C16C C15C H15C 120.4 . . ? C14C C15C H15C 120.4 . . ? N11C C16C C15C 122.16(18) . . ? N11C C16C H16C 118.9 . . ? C15C C16C H16C 118.9 . . ? O18C C17C C12C 110.28(14) . . ? O18C C17C H17E 109.6 . . ? C12C C17C H17E 109.6 . . ? O18C C17C H17F 109.6 . . ? C12C C17C H17F 109.6 . . ? H17E C17C H17F 108.1 . . ? C17C O18C Fe1A 125.60(11) . . ? C17C O18C Fe1C 112.15(10) . . ? Fe1A O18C Fe1C 98.95(5) . . ? C17C O18C Fe1D 119.34(11) . . ? Fe1A O18C Fe1D 96.67(5) . . ? Fe1C O18C Fe1D 99.48(5) . . ? C22C O21C Fe1C 130.90(12) . . ? C22C O21C H21C 109.6(18) . . ? Fe1C O21C H21C 108.3(18) . . ? O21C C22C C23C 109.21(17) . . ? O21C C22C H22G 109.8 . . ? C23C C22C H22G 109.8 . . ? O21C C22C H22H 109.8 . . ? C23C C22C H22H 109.8 . . ? H22G C22C H22H 108.3 . . ? C22C C23C H23J 109.5 . . ? C22C C23C H23K 109.5 . . ? H23J C23C H23K 109.5 . . ? C22C C23C H23L 109.5 . . ? H23J C23C H23L 109.5 . . ? H23K C23C H23L 109.5 . . ? O18A Fe1D O18D 83.02(5) . . ? O18A Fe1D O21D 87.01(6) . . ? O18D Fe1D O21D 91.28(7) . . ? O18A Fe1D N11D 158.18(6) . . ? O18D Fe1D N11D 76.35(5) . . ? O21D Fe1D N11D 86.42(6) . . ? O18A Fe1D O18C 81.12(5) . . ? O18D Fe1D O18C 80.59(5) . . ? O21D Fe1D O18C 166.31(6) . . ? N11D Fe1D O18C 102.16(5) . . ? O18A Fe1D Cl2D 100.36(4) . . ? O18D Fe1D Cl2D 173.57(4) . . ? O21D Fe1D Cl2D 94.34(6) . . ? N11D Fe1D Cl2D 100.87(5) . . ? O18C Fe1D Cl2D 94.47(4) . . ? C16D N11D C12D 118.77(16) . . ? C16D N11D Fe1D 126.96(13) . . ? C12D N11D Fe1D 114.26(12) . . ? N11D C12D C13D 121.69(17) . . ? N11D C12D C17D 115.92(16) . . ? C13D C12D C17D 122.39(17) . . ? C14D C13D C12D 119.30(18) . . ? C14D C13D H13D 120.4 . . ? C12D C13D H13D 120.4 . . ? C13D C14D C15D 118.94(18) . . ? C13D C14D H14D 120.5 . . ? C15D C14D H14D 120.5 . . ? C16D C15D C14D 118.83(19) . . ? C16D C15D H15D 120.6 . . ? C14D C15D H15D 120.6 . . ? N11D C16D C15D 122.46(19) . . ? N11D C16D H16D 118.8 . . ? C15D C16D H16D 118.8 . . ? O18D C17D C12D 110.75(15) . . ? O18D C17D H17G 109.5 . . ? C12D C17D H17G 109.5 . . ? O18D C17D H17H 109.5 . . ? C12D C17D H17H 109.5 . . ? H17G C17D H17H 108.1 . . ? C17D O18D Fe1B 127.66(11) . . ? C17D O18D Fe1D 112.48(11) . . ? Fe1B O18D Fe1D 97.37(5) . . ? C17D O18D Fe1C 118.90(12) . . ? Fe1B O18D Fe1C 96.18(5) . . ? Fe1D O18D Fe1C 98.89(5) . . ? C22H O21D C22D 42.1(3) . . ? C22H O21D Fe1D 137.0(3) . . ? C22D O21D Fe1D 126.9(2) . . ? C22H O21D H21D 99(3) . . ? C22D O21D H21D 120(3) . . ? Fe1D O21D H21D 112(3) . . ? O21D C22D C23D 115.6(4) . . ? O21D C22D H22I 108.4 . . ? C23D C22D H22I 108.4 . . ? O21D C22D H22J 108.4 . . ? C23D C22D H22J 108.4 . . ? H22I C22D H22J 107.4 . . ? C22H C23H H23P 109.5 . . ? C22H C23H H23Q 109.5 . . ? H23P C23H H23Q 109.5 . . ? C22H C23H H23R 109.5 . . ? H23P C23H H23R 109.5 . . ? H23Q C23H H23R 109.5 . . ? O21D C22H C23H 106.4(4) . . ? O21D C22H H22K 110.5 . . ? C23H C22H H22K 110.5 . . ? O21D C22H H22L 110.5 . . ? C23H C22H H22L 110.5 . . ? H22K C22H H22L 108.6 . . ? 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 O18C Fe1A N11A C12A -1.6(2) . . . . ? O18A Fe1A N11A C12A 13.90(13) . . . . ? O21A Fe1A N11A C12A -78.75(14) . . . . ? O18B Fe1A N11A C12A 90.78(14) . . . . ? Cl2A Fe1A N11A C12A -173.66(13) . . . . ? O18C Fe1A N11A C16A -178.89(15) . . . . ? O18A Fe1A N11A C16A -163.42(17) . . . . ? O21A Fe1A N11A C16A 103.93(17) . . . . ? O18B Fe1A N11A C16A -86.54(17) . . . . ? Cl2A Fe1A N11A C16A 9.02(17) . . . . ? C16A N11A C12A C13A -0.3(3) . . . . ? Fe1A N11A C12A C13A -177.90(16) . . . . ? C16A N11A C12A C17A -179.91(18) . . . . ? Fe1A N11A C12A C17A 2.5(2) . . . . ? N11A C12A C13A C14A 0.4(3) . . . . ? C17A C12A C13A C14A 180.0(2) . . . . ? C12A C13A C14A C15A -0.2(3) . . . . ? C13A C14A C15A C16A 0.0(4) . . . . ? C12A N11A C16A C15A 0.1(3) . . . . ? Fe1A N11A C16A C15A 177.29(16) . . . . ? C14A C15A C16A N11A 0.1(3) . . . . ? N11A C12A C17A O18A -26.7(2) . . . . ? C13A C12A C17A O18A 153.74(19) . . . . ? C12A C17A O18A Fe1D 157.42(12) . . . . ? C12A C17A O18A Fe1A 37.96(19) . . . . ? C12A C17A O18A Fe1B -77.40(18) . . . . ? O18C Fe1A O18A C17A 145.58(13) . . . . ? N11A Fe1A O18A C17A -28.66(13) . . . . ? O21A Fe1A O18A C17A 59.92(13) . . . . ? O18B Fe1A O18A C17A -132.59(13) . . . . ? Cl2A Fe1A O18A C17A -104.1(3) . . . . ? O18C Fe1A O18A Fe1D 10.07(5) . . . . ? N11A Fe1A O18A Fe1D -164.17(7) . . . . ? O21A Fe1A O18A Fe1D -75.59(6) . . . . ? O18B Fe1A O18A Fe1D 91.89(5) . . . . ? Cl2A Fe1A O18A Fe1D 120.4(3) . . . . ? O18C Fe1A O18A Fe1B -87.52(5) . . . . ? N11A Fe1A O18A Fe1B 98.24(6) . . . . ? O21A Fe1A O18A Fe1B -173.18(5) . . . . ? O18B Fe1A O18A Fe1B -5.70(5) . . . . ? Cl2A Fe1A O18A Fe1B 22.8(3) . . . . ? O18C Fe1A O21A C22A 175.34(16) . . . . ? O18A Fe1A O21A C22A -102.37(16) . . . . ? N11A Fe1A O21A C22A -26.02(16) . . . . ? O18B Fe1A O21A C22A -160.68(19) . . . . ? Cl2A Fe1A O21A C22A 75.53(16) . . . . ? Fe1A O21A C22A C23A -69.3(2) . . . . ? C17A O18A Fe1B O18B 127.58(12) . . . . ? Fe1D O18A Fe1B O18B -93.35(5) . . . . ? Fe1A O18A Fe1B O18B 5.88(5) . . . . ? C17A O18A Fe1B O18D -148.36(12) . . . . ? Fe1D O18A Fe1B O18D -9.29(5) . . . . ? Fe1A O18A Fe1B O18D 89.95(5) . . . . ? C17A O18A Fe1B N11B 53.60(13) . . . . ? Fe1D O18A Fe1B N11B -167.33(5) . . . . ? Fe1A O18A Fe1B N11B -68.10(6) . . . . ? C17A O18A Fe1B O21B 171.5(2) . . . . ? Fe1D O18A Fe1B O21B -49.4(3) . . . . ? Fe1A O18A Fe1B O21B 49.8(3) . . . . ? C17A O18A Fe1B Cl2B -49.31(12) . . . . ? Fe1D O18A Fe1B Cl2B 89.76(4) . . . . ? Fe1A O18A Fe1B Cl2B -171.00(4) . . . . ? O18B Fe1B N11B C12B 16.32(13) . . . . ? O18D Fe1B N11B C12B -4.0(2) . . . . ? O18A Fe1B N11B C12B 93.73(13) . . . . ? O21B Fe1B N11B C12B -74.04(14) . . . . ? Cl2B Fe1B N11B C12B -169.07(12) . . . . ? O18B Fe1B N11B C16B -168.26(18) . . . . ? O18D Fe1B N11B C16B 171.45(15) . . . . ? O18A Fe1B N11B C16B -90.85(17) . . . . ? O21B Fe1B N11B C16B 101.39(17) . . . . ? Cl2B Fe1B N11B C16B 6.36(17) . . . . ? C16B N11B C12B C13B 0.2(3) . . . . ? Fe1B N11B C12B C13B 176.08(15) . . . . ? C16B N11B C12B C17B -178.93(17) . . . . ? Fe1B N11B C12B C17B -3.1(2) . . . . ? N11B C12B C13B C14B -0.2(3) . . . . ? C17B C12B C13B C14B 178.90(19) . . . . ? C12B C13B C14B C15B 0.0(3) . . . . ? C13B C14B C15B C16B 0.3(3) . . . . ? C12B N11B C16B C15B 0.0(3) . . . . ? Fe1B N11B C16B C15B -175.23(15) . . . . ? C14B C15B C16B N11B -0.3(3) . . . . ? N11B C12B C17B O18B -20.0(2) . . . . ? C13B C12B C17B O18B 160.85(17) . . . . ? C12B C17B O18B Fe1B 33.67(18) . . . . ? C12B C17B O18B Fe1C 154.17(12) . . . . ? C12B C17B O18B Fe1A -81.28(16) . . . . ? O18D Fe1B O18B C17B 144.97(12) . . . . ? O18A Fe1B O18B C17B -132.01(12) . . . . ? N11B Fe1B O18B C17B -27.53(12) . . . . ? O21B Fe1B O18B C17B 57.54(12) . . . . ? Cl2B Fe1B O18B C17B -98.3(4) . . . . ? O18D Fe1B O18B Fe1C 9.23(5) . . . . ? O18A Fe1B O18B Fe1C 92.26(5) . . . . ? N11B Fe1B O18B Fe1C -163.27(7) . . . . ? O21B Fe1B O18B Fe1C -78.20(6) . . . . ? Cl2B Fe1B O18B Fe1C 126.0(4) . . . . ? O18D Fe1B O18B Fe1A -88.72(5) . . . . ? O18A Fe1B O18B Fe1A -5.69(5) . . . . ? N11B Fe1B O18B Fe1A 98.78(6) . . . . ? O21B Fe1B O18B Fe1A -176.15(6) . . . . ? Cl2B Fe1B O18B Fe1A 28.1(4) . . . . ? O18C Fe1A O18B C17B -148.10(12) . . . . ? O18A Fe1A O18B C17B 127.99(12) . . . . ? N11A Fe1A O18B C17B 54.06(13) . . . . ? O21A Fe1A O18B C17B -172.35(19) . . . . ? Cl2A Fe1A O18B C17B -48.37(12) . . . . ? O18C Fe1A O18B Fe1B 89.74(5) . . . . ? O18A Fe1A O18B Fe1B 5.82(5) . . . . ? N11A Fe1A O18B Fe1B -68.10(6) . . . . ? O21A Fe1A O18B Fe1B 65.5(2) . . . . ? Cl2A Fe1A O18B Fe1B -170.53(4) . . . . ? O18C Fe1A O18B Fe1C -9.75(5) . . . . ? O18A Fe1A O18B Fe1C -93.66(5) . . . . ? N11A Fe1A O18B Fe1C -167.58(5) . . . . ? O21A Fe1A O18B Fe1C -34.0(2) . . . . ? Cl2A Fe1A O18B Fe1C 89.99(4) . . . . ? O18B Fe1B O21B C22B -179.82(19) . . . . ? O18D Fe1B O21B C22B 97.2(2) . . . . ? O18A Fe1B O21B C22B 136.9(2) . . . . ? N11B Fe1B O21B C22B -103.4(2) . . . . ? Cl2B Fe1B O21B C22B -2.1(2) . . . . ? O18B Fe1B O21B C22F -125.9(6) . . . . ? O18D Fe1B O21B C22F 151.1(6) . . . . ? O18A Fe1B O21B C22F -169.2(6) . . . . ? N11B Fe1B O21B C22F -49.5(6) . . . . ? Cl2B Fe1B O21B C22F 51.8(6) . . . . ? C22F O21B C22B C23B -27.5(6) . . . . ? Fe1B O21B C22B C23B 78.4(3) . . . . ? C22B O21B C22F C23F 66.2(11) . . . . ? Fe1B O21B C22F C23F -43.8(15) . . . . ? C17B O18B Fe1C O18C 142.98(14) . . . . ? Fe1B O18B Fe1C O18C -90.43(5) . . . . ? Fe1A O18B Fe1C O18C 9.68(5) . . . . ? C17B O18B Fe1C N11C 128.49(17) . . . . ? Fe1B O18B Fe1C N11C -104.92(14) . . . . ? Fe1A O18B Fe1C N11C -4.81(16) . . . . ? C17B O18B Fe1C O21C 50.81(14) . . . . ? Fe1B O18B Fe1C O21C 177.40(6) . . . . ? Fe1A O18B Fe1C O21C -82.49(5) . . . . ? C17B O18B Fe1C O18D -135.57(14) . . . . ? Fe1B O18B Fe1C O18D -8.98(5) . . . . ? Fe1A O18B Fe1C O18D 91.12(5) . . . . ? C17B O18B Fe1C Cl2C -43.28(14) . . . . ? Fe1B O18B Fe1C Cl2C 83.31(5) . . . . ? Fe1A O18B Fe1C Cl2C -176.58(3) . . . . ? O18C Fe1C N11C C12C -17.62(12) . . . . ? O18B Fe1C N11C C12C -2.8(2) . . . . ? O21C Fe1C N11C C12C 74.59(13) . . . . ? O18D Fe1C N11C C12C -94.92(12) . . . . ? Cl2C Fe1C N11C C12C 168.90(11) . . . . ? O18C Fe1C N11C C16C 164.48(16) . . . . ? O18B Fe1C N11C C16C 179.28(14) . . . . ? O21C Fe1C N11C C16C -103.32(16) . . . . ? O18D Fe1C N11C C16C 87.18(16) . . . . ? Cl2C Fe1C N11C C16C -9.00(16) . . . . ? C16C N11C C12C C13C 1.4(3) . . . . ? Fe1C N11C C12C C13C -176.66(14) . . . . ? C16C N11C C12C C17C -178.76(16) . . . . ? Fe1C N11C C12C C17C 3.14(19) . . . . ? N11C C12C C13C C14C -1.0(3) . . . . ? C17C C12C C13C C14C 179.22(19) . . . . ? C12C C13C C14C C15C -0.3(3) . . . . ? C13C C14C C15C C16C 1.1(3) . . . . ? C12C N11C C16C C15C -0.6(3) . . . . ? Fe1C N11C C16C C15C 177.21(15) . . . . ? C14C C15C C16C N11C -0.7(3) . . . . ? N11C C12C C17C O18C 21.8(2) . . . . ? C13C C12C C17C O18C -158.36(17) . . . . ? C12C C17C O18C Fe1A -156.45(11) . . . . ? C12C C17C O18C Fe1C -36.59(17) . . . . ? C12C C17C O18C Fe1D 79.05(16) . . . . ? O18A Fe1A O18C C17C -143.45(13) . . . . ? N11A Fe1A O18C C17C -128.29(17) . . . . ? O21A Fe1A O18C C17C -50.51(13) . . . . ? O18B Fe1A O18C C17C 135.42(13) . . . . ? Cl2A Fe1A O18C C17C 43.84(13) . . . . ? O18A Fe1A O18C Fe1C 90.95(5) . . . . ? N11A Fe1A O18C Fe1C 106.11(15) . . . . ? O21A Fe1A O18C Fe1C -176.11(6) . . . . ? O18B Fe1A O18C Fe1C 9.81(5) . . . . ? Cl2A Fe1A O18C Fe1C -81.76(4) . . . . ? O18A Fe1A O18C Fe1D -9.79(5) . . . . ? N11A Fe1A O18C Fe1D 5.38(17) . . . . ? O21A Fe1A O18C Fe1D 83.16(5) . . . . ? O18B Fe1A O18C Fe1D -90.92(5) . . . . ? Cl2A Fe1A O18C Fe1D 177.50(3) . . . . ? O18B Fe1C O18C C17C -144.55(11) . . . . ? N11C Fe1C O18C C17C 29.79(11) . . . . ? O21C Fe1C O18C C17C -57.98(11) . . . . ? O18D Fe1C O18C C17C 133.11(11) . . . . ? Cl2C Fe1C O18C C17C 103.5(3) . . . . ? O18B Fe1C O18C Fe1A -10.10(5) . . . . ? N11C Fe1C O18C Fe1A 164.25(6) . . . . ? O21C Fe1C O18C Fe1A 76.47(5) . . . . ? O18D Fe1C O18C Fe1A -92.43(5) . . . . ? Cl2C Fe1C O18C Fe1A -122.1(3) . . . . ? O18B Fe1C O18C Fe1D 88.27(5) . . . . ? N11C Fe1C O18C Fe1D -97.39(6) . . . . ? O21C Fe1C O18C Fe1D 174.83(5) . . . . ? O18D Fe1C O18C Fe1D 5.93(5) . . . . ? Cl2C Fe1C O18C Fe1D -23.7(4) . . . . ? O18C Fe1C O21C C22C 98.76(15) . . . . ? O18B Fe1C O21C C22C -179.16(16) . . . . ? N11C Fe1C O21C C22C 22.78(16) . . . . ? O18D Fe1C O21C C22C 152.9(2) . . . . ? Cl2C Fe1C O21C C22C -79.12(15) . . . . ? Fe1C O21C C22C C23C 69.1(2) . . . . ? C17A O18A Fe1D O18D 143.40(15) . . . . ? Fe1A O18A Fe1D O18D -91.33(6) . . . . ? Fe1B O18A Fe1D O18D 9.24(5) . . . . ? C17A O18A Fe1D O21D 51.74(15) . . . . ? Fe1A O18A Fe1D O21D 177.01(7) . . . . ? Fe1B O18A Fe1D O21D -82.42(7) . . . . ? C17A O18A Fe1D N11D 124.35(18) . . . . ? Fe1A O18A Fe1D N11D -110.38(14) . . . . ? Fe1B O18A Fe1D N11D -9.81(17) . . . . ? C17A O18A Fe1D O18C -135.09(15) . . . . ? Fe1A O18A Fe1D O18C -9.82(5) . . . . ? Fe1B O18A Fe1D O18C 90.75(5) . . . . ? C17A O18A Fe1D Cl2D -42.13(15) . . . . ? Fe1A O18A Fe1D Cl2D 83.14(5) . . . . ? Fe1B O18A Fe1D Cl2D -176.29(3) . . . . ? C17C O18C Fe1D O18A 147.40(12) . . . . ? Fe1A O18C Fe1D O18A 9.83(5) . . . . ? Fe1C O18C Fe1D O18A -90.43(5) . . . . ? C17C O18C Fe1D O18D -128.27(12) . . . . ? Fe1A O18C Fe1D O18D 94.17(5) . . . . ? Fe1C O18C Fe1D O18D -6.10(5) . . . . ? C17C O18C Fe1D O21D 177.5(3) . . . . ? Fe1A O18C Fe1D O21D 39.9(3) . . . . ? Fe1C O18C Fe1D O21D -60.3(3) . . . . ? C17C O18C Fe1D N11D -54.55(12) . . . . ? Fe1A O18C Fe1D N11D 167.88(5) . . . . ? Fe1C O18C Fe1D N11D 67.62(6) . . . . ? C17C O18C Fe1D Cl2D 47.59(12) . . . . ? Fe1A O18C Fe1D Cl2D -89.97(4) . . . . ? Fe1C O18C Fe1D Cl2D 169.76(4) . . . . ? O18A Fe1D N11D C16D -173.86(15) . . . . ? O18D Fe1D N11D C16D 166.67(17) . . . . ? O21D Fe1D N11D C16D -101.14(17) . . . . ? O18C Fe1D N11D C16D 89.64(16) . . . . ? Cl2D Fe1D N11D C16D -7.40(17) . . . . ? O18A Fe1D N11D C12D 5.1(2) . . . . ? O18D Fe1D N11D C12D -14.34(12) . . . . ? O21D Fe1D N11D C12D 77.85(14) . . . . ? O18C Fe1D N11D C12D -91.37(13) . . . . ? Cl2D Fe1D N11D C12D 171.60(12) . . . . ? C16D N11D C12D C13D -0.5(3) . . . . ? Fe1D N11D C12D C13D -179.60(15) . . . . ? C16D N11D C12D C17D 178.78(17) . . . . ? Fe1D N11D C12D C17D -0.3(2) . . . . ? N11D C12D C13D C14D 0.2(3) . . . . ? C17D C12D C13D C14D -179.06(19) . . . . ? C12D C13D C14D C15D 0.3(3) . . . . ? C13D C14D C15D C16D -0.5(3) . . . . ? C12D N11D C16D C15D 0.4(3) . . . . ? Fe1D N11D C16D C15D 179.31(15) . . . . ? C14D C15D C16D N11D 0.1(3) . . . . ? N11D C12D C17D O18D 23.3(2) . . . . ? C13D C12D C17D O18D -157.40(18) . . . . ? C12D C17D O18D Fe1B -154.82(12) . . . . ? C12D C17D O18D Fe1D -35.18(19) . . . . ? C12D C17D O18D Fe1C 79.63(18) . . . . ? O18B Fe1B O18D C17D -143.15(15) . . . . ? O18A Fe1B O18D C17D 135.22(15) . . . . ? N11B Fe1B O18D C17D -123.29(19) . . . . ? O21B Fe1B O18D C17D -53.65(16) . . . . ? Cl2B Fe1B O18D C17D 41.91(15) . . . . ? O18B Fe1B O18D Fe1D 90.92(5) . . . . ? O18A Fe1B O18D Fe1D 9.29(5) . . . . ? N11B Fe1B O18D Fe1D 110.78(15) . . . . ? O21B Fe1B O18D Fe1D -179.58(6) . . . . ? Cl2B Fe1B O18D Fe1D -84.02(5) . . . . ? O18B Fe1B O18D Fe1C -8.91(5) . . . . ? O18A Fe1B O18D Fe1C -90.54(5) . . . . ? N11B Fe1B O18D Fe1C 10.95(18) . . . . ? O21B Fe1B O18D Fe1C 80.59(6) . . . . ? Cl2B Fe1B O18D Fe1C 176.15(4) . . . . ? O18A Fe1D O18D C17D -145.55(12) . . . . ? O21D Fe1D O18D C17D -58.72(12) . . . . ? N11D Fe1D O18D C17D 27.28(12) . . . . ? O18C Fe1D O18D C17D 132.35(12) . . . . ? Cl2D Fe1D O18D C17D 92.3(4) . . . . ? O18A Fe1D O18D Fe1B -9.48(5) . . . . ? O21D Fe1D O18D Fe1B 77.35(6) . . . . ? N11D Fe1D O18D Fe1B 163.35(7) . . . . ? O18C Fe1D O18D Fe1B -91.58(5) . . . . ? Cl2D Fe1D O18D Fe1B -131.6(3) . . . . ? O18A Fe1D O18D Fe1C 88.00(5) . . . . ? O21D Fe1D O18D Fe1C 174.83(6) . . . . ? N11D Fe1D O18D Fe1C -99.17(6) . . . . ? O18C Fe1D O18D Fe1C 5.90(5) . . . . ? Cl2D Fe1D O18D Fe1C -34.1(4) . . . . ? O18C Fe1C O18D C17D -127.96(13) . . . . ? O18B Fe1C O18D C17D 148.55(13) . . . . ? N11C Fe1C O18D C17D -54.19(13) . . . . ? O21C Fe1C O18D C17D 176.8(2) . . . . ? Cl2C Fe1C O18D C17D 48.75(12) . . . . ? O18C Fe1C O18D Fe1B 92.42(5) . . . . ? O18B Fe1C O18D Fe1B 8.93(5) . . . . ? N11C Fe1C O18D Fe1B 166.19(5) . . . . ? O21C Fe1C O18D Fe1B 37.2(2) . . . . ? Cl2C Fe1C O18D Fe1B -90.87(4) . . . . ? O18C Fe1C O18D Fe1D -6.06(5) . . . . ? O18B Fe1C O18D Fe1D -89.55(5) . . . . ? N11C Fe1C O18D Fe1D 67.71(6) . . . . ? O21C Fe1C O18D Fe1D -61.3(2) . . . . ? Cl2C Fe1C O18D Fe1D 170.65(4) . . . . ? O18A Fe1D O21D C22H -91.3(3) . . . . ? O18D Fe1D O21D C22H -174.2(3) . . . . ? N11D Fe1D O21D C22H 109.6(3) . . . . ? O18C Fe1D O21D C22H -121.0(4) . . . . ? Cl2D Fe1D O21D C22H 8.9(3) . . . . ? O18A Fe1D O21D C22D -147.5(3) . . . . ? O18D Fe1D O21D C22D 129.6(3) . . . . ? N11D Fe1D O21D C22D 53.4(3) . . . . ? O18C Fe1D O21D C22D -177.2(3) . . . . ? Cl2D Fe1D O21D C22D -47.3(3) . . . . ? C22H O21D C22D C23D -39.1(5) . . . . ? Fe1D O21D C22D C23D 83.0(5) . . . . ? C22D O21D C22H C23H 13.4(4) . . . . ? Fe1D O21D C22H C23H -83.9(5) . . . . ? 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 O21A H21A Cl2D 0.73(3) 2.34(3) 3.0599(15) 169(3) . O21B H21B Cl2C 0.67(3) 2.38(3) 3.0372(17) 166(4) . O21C H21C Cl2A 0.82(3) 2.23(3) 3.0373(15) 171(2) . O21D H21D Cl2B 0.70(3) 2.36(3) 3.0527(19) 167(4) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.632 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.072