# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 182 _publ_contact_author_name 'Andreas Grohmann' _publ_contact_author_address ; Institut fuer Chemie Technische Universitaet Berlin Strasse des 17. Juni 135 Berlin 10623 GERMANY ; _publ_contact_author_phone '049 30 314 79877' _publ_contact_author_fax '049 30 314 22168' _publ_contact_author_email andreas.grohmann@chem.tu-berlin.de _publ_requested_journal 'Chem. Comm.' _publ_requested_coeditor_name ? _publ_section_title ; A non-heme dinuclear iron(II) complex containing a single, unsupported hydroxo bridge ; loop_ _publ_author_name _publ_author_address 'Pitarch Lopez, J.' ; Technische Universitat Berlin Institut fur Chemie, Sekr. C2 Str. des 17. Juni 135 D-10623 Berlin Bundesrepublik Deutschland ; 'Kampf, H.' ; Technische Universitat Berlin Institut fur Chemie, Sekr. C2 Str. des 17. Juni 135 D-10623 Berlin Bundesrepublik Deutschland ; 'Heinemann, F. W.' ; Institut fur Anorganische Chemie Universitat Erlangen-Nurnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; 'Prakash, R.' ; Institut fur Anorganische Chemie Universitat Erlangen-Nurnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; 'Grohmann, A.' ; Technische Universitat Berlin Institut fur Chemie, Sekr. C2 Str. des 17. Juni 135 D-10623 Berlin Bundesrepublik Deutschland ; data_ag0509 _database_code_depnum_ccdc_archive 'CCDC 293017' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H31 Fe N7, 2 (C F3 O3 S)' _chemical_formula_sum 'C19 H31 F6 Fe N7 O6 S2' _chemical_formula_weight 687.48 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1099(6) _cell_length_b 11.2823(9) _cell_length_c 24.199(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.774(7) _cell_angle_gamma 90.00 _cell_volume 2760.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 334 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description prism _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.787 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.085 -1 0 0 0.074 0 1 0 0.077 0 -1 0 0.078 0 0 1 0.100 0 0 -1 0.100 -1 1 0 0.064 1 -1 0 0.075 3 4 0 0.085 1 1 -5 0.077 1 1 2 0.094 -1 -1 5 0.085 -1 -1 -2 0.079 -1 -1 1 0.083 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.881 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 1.30 \% and 84 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80280 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.10 _reflns_number_total 6085 _reflns_number_gt 5220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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^)+(0.0103P)^2^+6.1909P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6085 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 0.007 _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 0.04133(3) 0.81971(3) 0.134381(14) 0.00889(8) Uani 1 1 d . . . N11 N 0.2087(2) 0.73459(18) 0.14205(8) 0.0111(4) Uani 1 1 d . . . N12 N -0.0446(2) 0.68523(19) 0.09158(8) 0.0119(4) Uani 1 1 d . . . H12A H -0.0834 0.6352 0.1166 0.014 Uiso 1 1 calc R . . H12B H -0.1114 0.7168 0.0700 0.014 Uiso 1 1 calc R . . N13 N 0.0969(2) 0.88161(19) 0.05927(8) 0.0128(4) Uani 1 1 d . . . H13A H 0.0225 0.9088 0.0410 0.015 Uiso 1 1 calc R . . H13B H 0.1518 0.9456 0.0649 0.015 Uiso 1 1 calc R . . N14 N 0.1086(2) 0.96304(19) 0.17698(9) 0.0136(4) Uani 1 1 d . . . H14A H 0.1416 1.0165 0.1520 0.016 Uiso 1 1 calc R . . H14B H 0.0376 0.9984 0.1937 0.016 Uiso 1 1 calc R . . N15 N -0.0151(2) 0.75906(19) 0.20933(8) 0.0122(4) Uani 1 1 d . . . H15A H -0.0865 0.8033 0.2204 0.015 Uiso 1 1 calc R . . H15B H -0.0438 0.6822 0.2051 0.015 Uiso 1 1 calc R . . C11 C 0.2577(2) 0.6701(2) 0.09888(10) 0.0135(5) Uani 1 1 d . . . C12 C 0.3757(3) 0.6079(2) 0.10420(11) 0.0183(6) Uani 1 1 d . . . H12C H 0.4072 0.5624 0.0741 0.022 Uiso 1 1 calc R . . C13 C 0.4476(3) 0.6120(3) 0.15323(12) 0.0216(6) Uani 1 1 d . . . H13C H 0.5288 0.5701 0.1570 0.026 Uiso 1 1 calc R . . C14 C 0.3995(3) 0.6779(2) 0.19662(11) 0.0177(5) Uani 1 1 d . . . H14C H 0.4482 0.6827 0.2304 0.021 Uiso 1 1 calc R . . C15 C 0.2791(2) 0.7374(2) 0.19071(10) 0.0131(5) Uani 1 1 d . . . C16 C 0.0408(2) 0.6129(2) 0.05545(11) 0.0141(5) Uani 1 1 d . . . H16A H -0.0049 0.6009 0.0194 0.017 Uiso 1 1 calc R . . H16B H 0.0541 0.5340 0.0726 0.017 Uiso 1 1 calc R . . C17 C 0.1652(3) 0.7968(2) 0.02255(10) 0.0154(5) Uani 1 1 d . . . H17A H 0.2552 0.8272 0.0153 0.019 Uiso 1 1 calc R . . H17B H 0.1168 0.7938 -0.0133 0.019 Uiso 1 1 calc R . . C18 C 0.1770(2) 0.6700(2) 0.04540(10) 0.0137(5) Uani 1 1 d . . . C19 C 0.2420(3) 0.5956(2) -0.00008(11) 0.0183(6) Uani 1 1 d . . . H19A H 0.3295 0.6281 -0.0081 0.027 Uiso 1 1 calc R . . H19B H 0.1866 0.5979 -0.0336 0.027 Uiso 1 1 calc R . . H19C H 0.2512 0.5134 0.0125 0.027 Uiso 1 1 calc R . . C20 C 0.2116(3) 0.9413(2) 0.21971(11) 0.0156(5) Uani 1 1 d . . . H20A H 0.1923 0.9904 0.2525 0.019 Uiso 1 1 calc R . . H20B H 0.2983 0.9668 0.2053 0.019 Uiso 1 1 calc R . . C21 C 0.0860(3) 0.7611(3) 0.25452(11) 0.0187(6) Uani 1 1 d . . . H21A H 0.0981 0.6794 0.2686 0.022 Uiso 1 1 calc R . . H21B H 0.0520 0.8098 0.2852 0.022 Uiso 1 1 calc R . . C22 C 0.2216(3) 0.8102(2) 0.23767(10) 0.0149(5) Uani 1 1 d . . . C23 C 0.3102(3) 0.8093(3) 0.28971(11) 0.0221(6) Uani 1 1 d . . . H23A H 0.3228 0.7274 0.3023 0.033 Uiso 1 1 calc R . . H23B H 0.2680 0.8555 0.3189 0.033 Uiso 1 1 calc R . . H23C H 0.3962 0.8443 0.2812 0.033 Uiso 1 1 calc R . . N30 N -0.1298(2) 0.90846(19) 0.12519(8) 0.0122(4) Uani 1 1 d . . . C31 C -0.1439(3) 1.0250(2) 0.10830(11) 0.0169(5) Uani 1 1 d . . . H31A H -0.0731 1.0775 0.1004 0.020 Uiso 1 1 calc R . . C32 C -0.2747(3) 1.0531(2) 0.10466(11) 0.0187(6) Uani 1 1 d . . . H32A H -0.3117 1.1272 0.0941 0.022 Uiso 1 1 calc R . . N33 N -0.3423(2) 0.9529(2) 0.11934(9) 0.0163(5) Uani 1 1 d . . . C34 C -0.2520(3) 0.8690(2) 0.13140(10) 0.0149(5) Uani 1 1 d . . . H34A H -0.2734 0.7909 0.1430 0.018 Uiso 1 1 calc R . . C35 C -0.4854(3) 0.9417(3) 0.12347(13) 0.0245(6) Uani 1 1 d . . . H35A H -0.5088 0.8579 0.1277 0.037 Uiso 1 1 calc R . . H35B H -0.5276 0.9732 0.0899 0.037 Uiso 1 1 calc R . . H35C H -0.5159 0.9862 0.1556 0.037 Uiso 1 1 calc R . . S100 S 0.77760(6) 0.48753(6) 0.21638(3) 0.01424(13) Uani 1 1 d . . . O11 O 0.89801(19) 0.49194(19) 0.24863(8) 0.0245(4) Uani 1 1 d . . . O12 O 0.65684(19) 0.47369(17) 0.24692(8) 0.0195(4) Uani 1 1 d . . . O13 O 0.76978(19) 0.57520(17) 0.17262(8) 0.0212(4) Uani 1 1 d . . . C100 C 0.7889(3) 0.3482(3) 0.17841(11) 0.0212(6) Uani 1 1 d . . . F11 F 0.67993(17) 0.33038(17) 0.14755(8) 0.0328(4) Uani 1 1 d . . . F12 F 0.89218(17) 0.34640(17) 0.14475(7) 0.0309(4) Uani 1 1 d . . . F13 F 0.8018(2) 0.25663(15) 0.21322(8) 0.0353(5) Uani 1 1 d . . . S200 S 0.21963(6) 0.20463(6) 0.05111(3) 0.01348(13) Uani 1 1 d . . . O21 O 0.1562(2) 0.1558(2) 0.00231(8) 0.0286(5) Uani 1 1 d . . . O22 O 0.1741(2) 0.31898(19) 0.06764(9) 0.0296(5) Uani 1 1 d . . . O23 O 0.23937(19) 0.11881(17) 0.09500(8) 0.0206(4) Uani 1 1 d . . . C200 C 0.3880(3) 0.2323(3) 0.02809(13) 0.0273(7) Uani 1 1 d . . . F21 F 0.4618(2) 0.2793(2) 0.06830(9) 0.0534(6) Uani 1 1 d . . . F22 F 0.44709(19) 0.13278(19) 0.01234(8) 0.0439(5) Uani 1 1 d . . . F23 F 0.3882(2) 0.30624(19) -0.01498(9) 0.0453(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01001(17) 0.00782(16) 0.00884(16) 0.00069(13) 0.00045(12) 0.00012(14) N11 0.0114(10) 0.0085(10) 0.0134(10) 0.0021(8) 0.0017(8) -0.0025(8) N12 0.0120(10) 0.0121(10) 0.0117(10) 0.0001(8) 0.0009(8) -0.0007(9) N13 0.0139(11) 0.0113(10) 0.0131(10) 0.0015(8) -0.0011(8) -0.0007(8) N14 0.0162(11) 0.0117(10) 0.0130(10) 0.0010(8) 0.0009(8) -0.0021(9) N15 0.0123(10) 0.0119(10) 0.0124(10) 0.0004(8) 0.0016(8) -0.0004(8) C11 0.0140(12) 0.0092(11) 0.0175(12) 0.0028(10) 0.0044(10) -0.0017(10) C12 0.0173(13) 0.0161(13) 0.0217(14) 0.0011(11) 0.0044(11) 0.0043(11) C13 0.0160(13) 0.0194(14) 0.0293(15) 0.0050(12) 0.0009(11) 0.0049(11) C14 0.0157(13) 0.0180(13) 0.0194(13) 0.0051(11) -0.0024(10) -0.0015(11) C15 0.0129(12) 0.0123(12) 0.0140(12) 0.0051(10) -0.0009(10) -0.0026(10) C16 0.0149(12) 0.0112(12) 0.0164(12) -0.0029(10) 0.0023(10) -0.0006(10) C17 0.0204(13) 0.0146(13) 0.0114(12) 0.0019(10) 0.0045(10) 0.0000(10) C18 0.0152(12) 0.0128(12) 0.0131(12) -0.0007(10) 0.0032(10) 0.0002(10) C19 0.0221(14) 0.0162(13) 0.0170(13) -0.0030(11) 0.0070(11) -0.0005(11) C20 0.0184(13) 0.0134(12) 0.0148(12) -0.0027(10) -0.0025(10) -0.0007(10) C21 0.0168(13) 0.0278(15) 0.0114(12) 0.0059(11) 0.0009(10) -0.0001(12) C22 0.0155(13) 0.0162(13) 0.0130(12) 0.0019(10) -0.0009(10) -0.0012(11) C23 0.0219(14) 0.0305(16) 0.0137(13) 0.0010(12) -0.0022(11) 0.0006(13) N30 0.0142(11) 0.0123(10) 0.0100(10) -0.0001(8) -0.0002(8) 0.0014(8) C31 0.0185(13) 0.0142(13) 0.0181(13) 0.0016(10) 0.0011(10) -0.0002(11) C32 0.0231(14) 0.0148(13) 0.0181(13) 0.0022(11) -0.0012(11) 0.0045(11) N33 0.0151(11) 0.0187(11) 0.0151(11) 0.0029(9) 0.0016(9) 0.0027(9) C34 0.0167(13) 0.0153(12) 0.0128(12) 0.0008(10) 0.0003(10) 0.0016(11) C35 0.0154(14) 0.0294(16) 0.0287(16) 0.0025(13) 0.0027(12) 0.0038(12) S100 0.0146(3) 0.0144(3) 0.0137(3) 0.0023(2) 0.0000(2) -0.0031(2) O11 0.0221(11) 0.0290(11) 0.0221(10) 0.0003(9) -0.0054(8) -0.0025(9) O12 0.0211(10) 0.0190(10) 0.0185(9) 0.0017(8) 0.0058(8) -0.0034(8) O13 0.0186(10) 0.0213(10) 0.0237(10) 0.0095(8) 0.0034(8) -0.0027(8) C100 0.0206(14) 0.0228(15) 0.0201(14) -0.0006(11) -0.0023(11) 0.0015(11) F11 0.0252(9) 0.0363(10) 0.0365(10) -0.0164(9) -0.0088(8) -0.0028(8) F12 0.0244(9) 0.0427(11) 0.0257(9) -0.0077(8) 0.0041(7) 0.0070(8) F13 0.0516(12) 0.0155(9) 0.0390(11) 0.0036(8) 0.0016(9) 0.0043(8) S200 0.0136(3) 0.0139(3) 0.0130(3) 0.0027(2) 0.0003(2) -0.0014(2) O21 0.0291(11) 0.0338(12) 0.0228(11) -0.0008(9) -0.0106(9) -0.0054(10) O22 0.0404(13) 0.0207(10) 0.0279(11) 0.0043(9) 0.0091(10) 0.0105(10) O23 0.0257(11) 0.0187(10) 0.0174(9) 0.0058(8) 0.0014(8) -0.0016(8) C200 0.0191(15) 0.0347(17) 0.0282(16) 0.0105(14) 0.0050(12) -0.0012(13) F21 0.0293(11) 0.0726(16) 0.0580(14) 0.0046(12) -0.0125(10) -0.0273(11) F22 0.0332(11) 0.0536(13) 0.0452(12) 0.0147(10) 0.0168(9) 0.0227(10) F23 0.0382(11) 0.0501(13) 0.0483(12) 0.0302(10) 0.0199(9) 0.0010(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N11 1.952(2) . ? Fe1 N30 2.009(2) . ? Fe1 N12 2.026(2) . ? Fe1 N15 2.028(2) . ? Fe1 N14 2.030(2) . ? Fe1 N13 2.033(2) . ? N11 C15 1.368(3) . ? N11 C11 1.371(3) . ? N12 C16 1.482(3) . ? N12 H12A 0.9200 . ? N12 H12B 0.9200 . ? N13 C17 1.483(3) . ? N13 H13A 0.9200 . ? N13 H13B 0.9200 . ? N14 C20 1.478(3) . ? N14 H14A 0.9200 . ? N14 H14B 0.9200 . ? N15 C21 1.487(3) . ? N15 H15A 0.9200 . ? N15 H15B 0.9200 . ? C11 C12 1.389(4) . ? C11 C18 1.521(3) . ? C12 C13 1.384(4) . ? C12 H12C 0.9500 . ? C13 C14 1.381(4) . ? C13 H13C 0.9500 . ? C14 C15 1.396(4) . ? C14 H14C 0.9500 . ? C15 C22 1.523(4) . ? C16 C18 1.543(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.538(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.539(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.544(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.539(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.535(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N30 C34 1.324(3) . ? N30 C31 1.384(3) . ? C31 C32 1.362(4) . ? C31 H31A 0.9500 . ? C32 N33 1.370(3) . ? C32 H32A 0.9500 . ? N33 C34 1.345(3) . ? N33 C35 1.456(3) . ? C34 H34A 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? S100 O11 1.438(2) . ? S100 O12 1.4441(19) . ? S100 O13 1.4505(19) . ? S100 C100 1.825(3) . ? C100 F12 1.333(3) . ? C100 F11 1.338(3) . ? C100 F13 1.339(3) . ? S200 O22 1.429(2) . ? S200 O21 1.445(2) . ? S200 O23 1.4491(19) . ? S200 C200 1.825(3) . ? C200 F21 1.329(4) . ? C200 F22 1.331(4) . ? C200 F23 1.335(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 N11 Fe1 N30 178.97(9) . . ? N11 Fe1 N12 92.60(8) . . ? N30 Fe1 N12 87.35(8) . . ? N11 Fe1 N15 90.18(8) . . ? N30 Fe1 N15 90.85(8) . . ? N12 Fe1 N15 94.62(8) . . ? N11 Fe1 N14 93.41(9) . . ? N30 Fe1 N14 86.64(9) . . ? N12 Fe1 N14 173.97(9) . . ? N15 Fe1 N14 84.90(8) . . ? N11 Fe1 N13 90.24(9) . . ? N30 Fe1 N13 88.73(8) . . ? N12 Fe1 N13 85.53(8) . . ? N15 Fe1 N13 179.55(9) . . ? N14 Fe1 N13 94.91(9) . . ? C15 N11 C11 118.6(2) . . ? C15 N11 Fe1 120.69(17) . . ? C11 N11 Fe1 120.68(17) . . ? C16 N12 Fe1 117.69(15) . . ? C16 N12 H12A 107.9 . . ? Fe1 N12 H12A 107.9 . . ? C16 N12 H12B 107.9 . . ? Fe1 N12 H12B 107.9 . . ? H12A N12 H12B 107.2 . . ? C17 N13 Fe1 116.79(15) . . ? C17 N13 H13A 108.1 . . ? Fe1 N13 H13A 108.1 . . ? C17 N13 H13B 108.1 . . ? Fe1 N13 H13B 108.1 . . ? H13A N13 H13B 107.3 . . ? C20 N14 Fe1 116.81(16) . . ? C20 N14 H14A 108.1 . . ? Fe1 N14 H14A 108.1 . . ? C20 N14 H14B 108.1 . . ? Fe1 N14 H14B 108.1 . . ? H14A N14 H14B 107.3 . . ? C21 N15 Fe1 116.97(16) . . ? C21 N15 H15A 108.1 . . ? Fe1 N15 H15A 108.1 . . ? C21 N15 H15B 108.1 . . ? Fe1 N15 H15B 108.1 . . ? H15A N15 H15B 107.3 . . ? N11 C11 C12 121.1(2) . . ? N11 C11 C18 117.0(2) . . ? C12 C11 C18 121.9(2) . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12C 119.9 . . ? C11 C12 H12C 119.9 . . ? C14 C13 C12 118.9(3) . . ? C14 C13 H13C 120.5 . . ? C12 C13 H13C 120.5 . . ? C13 C14 C15 119.8(2) . . ? C13 C14 H14C 120.1 . . ? C15 C14 H14C 120.1 . . ? N11 C15 C14 121.3(2) . . ? N11 C15 C22 117.1(2) . . ? C14 C15 C22 121.6(2) . . ? N12 C16 C18 113.0(2) . . ? N12 C16 H16A 109.0 . . ? C18 C16 H16A 109.0 . . ? N12 C16 H16B 109.0 . . ? C18 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? N13 C17 C18 114.8(2) . . ? N13 C17 H17A 108.6 . . ? C18 C17 H17A 108.6 . . ? N13 C17 H17B 108.6 . . ? C18 C17 H17B 108.6 . . ? H17A C17 H17B 107.5 . . ? C11 C18 C17 110.1(2) . . ? C11 C18 C19 112.3(2) . . ? C17 C18 C19 106.4(2) . . ? C11 C18 C16 109.6(2) . . ? C17 C18 C16 112.4(2) . . ? C19 C18 C16 106.0(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N14 C20 C22 113.5(2) . . ? N14 C20 H20A 108.9 . . ? C22 C20 H20A 108.9 . . ? N14 C20 H20B 108.9 . . ? C22 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? N15 C21 C22 114.6(2) . . ? N15 C21 H21A 108.6 . . ? C22 C21 H21A 108.6 . . ? N15 C21 H21B 108.6 . . ? C22 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C15 C22 C23 112.6(2) . . ? C15 C22 C21 110.7(2) . . ? C23 C22 C21 107.0(2) . . ? C15 C22 C20 109.3(2) . . ? C23 C22 C20 105.8(2) . . ? C21 C22 C20 111.3(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C34 N30 C31 105.1(2) . . ? C34 N30 Fe1 128.58(18) . . ? C31 N30 Fe1 126.25(18) . . ? C32 C31 N30 109.6(2) . . ? C32 C31 H31A 125.2 . . ? N30 C31 H31A 125.2 . . ? C31 C32 N33 106.2(2) . . ? C31 C32 H32A 126.9 . . ? N33 C32 H32A 126.9 . . ? C34 N33 C32 107.3(2) . . ? C34 N33 C35 126.5(2) . . ? C32 N33 C35 126.1(2) . . ? N30 C34 N33 111.7(2) . . ? N30 C34 H34A 124.1 . . ? N33 C34 H34A 124.1 . . ? N33 C35 H35A 109.5 . . ? N33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O11 S100 O12 116.19(12) . . ? O11 S100 O13 114.21(12) . . ? O12 S100 O13 114.16(11) . . ? O11 S100 C100 104.16(13) . . ? O12 S100 C100 102.93(12) . . ? O13 S100 C100 102.87(12) . . ? F12 C100 F11 107.6(2) . . ? F12 C100 F13 107.6(2) . . ? F11 C100 F13 107.9(2) . . ? F12 C100 S100 112.1(2) . . ? F11 C100 S100 110.73(19) . . ? F13 C100 S100 110.75(19) . . ? O22 S200 O21 115.60(13) . . ? O22 S200 O23 116.10(12) . . ? O21 S200 O23 113.53(12) . . ? O22 S200 C200 103.65(14) . . ? O21 S200 C200 102.78(14) . . ? O23 S200 C200 102.62(13) . . ? F21 C200 F22 107.2(3) . . ? F21 C200 F23 108.4(3) . . ? F22 C200 F23 107.4(2) . . ? F21 C200 S200 111.2(2) . . ? F22 C200 S200 111.6(2) . . ? F23 C200 S200 110.9(2) . . ? 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 N12 H12A O13 0.92 2.13 3.001(3) 156.8 1_455 N12 H12B O21 0.92 2.30 3.096(3) 143.9 3_565 N13 H13A O21 0.92 2.20 2.974(3) 141.2 3_565 N13 H13B O23 0.92 2.26 3.154(3) 163.5 1_565 N14 H14A O23 0.92 2.06 2.974(3) 171.3 1_565 N14 H14B O12 0.92 2.47 3.277(3) 147.2 2 N15 H15A O12 0.92 2.20 3.013(3) 146.9 2 N15 H15B O13 0.92 2.36 3.125(3) 140.2 1_455 N15 H15B O11 0.92 2.47 3.283(3) 148.1 1_455 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.439 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.103 # END OF DATA FOR 2 # 4.2 RESULTS FOR 3 data_jp0304 _database_code_depnum_ccdc_archive 'CCDC 293018' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H51 Fe2 N10 O, 2(Cl O4), Br' _chemical_formula_sum 'C26 H51 Br Cl2 Fe2 N10 O9' _chemical_formula_weight 910.28 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-42(1)m _symmetry_space_group_name_Hall P-42ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 15.094(1) _cell_length_b 15.094(1) _cell_length_c 8.1109(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1847.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 228 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 2.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.837 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS, Bruker-Nonius, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-scans with 2.00 \% and 80 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32119 _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 29.01 _reflns_number_total 2575 _reflns_number_gt 2101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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^)+(0.0318P)^2^+1.0651P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack H D (1983), Acta Cryst. A39, 876-881 1115 Friedel pairs used in the refinement of Flack parameter ; _refine_ls_abs_structure_Flack 0.501(12) _refine_ls_number_reflns 2575 _refine_ls_number_parameters 178 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.003 _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 0.40990(3) -0.09010(3) 0.20308(7) 0.01018(14) Uani 1 2 d S . . O1 O 0.5000 0.0000 0.1322(5) 0.0110(8) Uani 1 4 d SD . . H1 H 0.5000 0.0000 0.0278(14) 0.013 Uiso 1 4 d SD . . Br1 Br 0.5000 0.0000 0.71664(7) 0.01259(14) Uani 1 4 d S . . Cl1 Cl 0.23420(5) -0.26580(5) -0.23834(12) 0.0130(2) Uani 1 2 d S . . N11 N 0.30716(15) -0.19284(15) 0.2530(4) 0.0081(7) Uani 1 2 d S . . C11 C 0.22045(18) -0.1699(2) 0.2505(3) 0.0129(7) Uani 1 1 d . . . O11 O 0.17085(14) -0.32915(14) -0.1733(4) 0.0158(7) Uani 1 2 d S . . N12 N 0.34140(17) -0.00592(19) 0.3806(3) 0.0134(5) Uani 1 1 d . . . H12A H 0.376(2) -0.003(3) 0.473(4) 0.016 Uiso 1 1 d . . . H12B H 0.344(2) 0.052(2) 0.341(4) 0.016 Uiso 1 1 d . . . C12 C 0.1540(2) -0.2342(2) 0.2410(4) 0.0149(6) Uani 1 1 d . . . H12 H 0.093(2) -0.215(2) 0.237(4) 0.018 Uiso 1 1 d . . . O12 O 0.1932(3) -0.1808(3) -0.2479(8) 0.0362(14) Uani 0.50 1 d P . . N13 N 0.3079(2) -0.0422(3) 0.0272(5) 0.0436(11) Uani 1 1 d D . . H13A H 0.322(3) 0.0114(12) 0.011(6) 0.052 Uiso 1 1 d D . . H13B H 0.297(3) -0.069(3) -0.057(6) 0.052 Uiso 1 1 d . . . C13 C 0.1773(2) -0.3227(2) 0.2354(5) 0.0149(9) Uani 1 2 d S . . H13 H 0.133(2) -0.367(2) 0.248(6) 0.018 Uiso 1 2 d S . . O13 O 0.2394(4) -0.1914(4) -0.1287(6) 0.0339(14) Uani 0.50 1 d P . . O14 O 0.2059(4) -0.2364(4) -0.3953(5) 0.0389(15) Uani 0.50 1 d P . . C16 C 0.2479(2) -0.0290(3) 0.4106(5) 0.0206(8) Uani 1 1 d . . . H16A H 0.222(3) 0.020(3) 0.434(4) 0.025 Uiso 1 1 d . . . H16B H 0.245(3) -0.065(3) 0.501(5) 0.025 Uiso 1 1 d . . . C17 C 0.2193(3) -0.0227(3) 0.0963(5) 0.0298(10) Uani 1 1 d . . . H17A H 0.207(3) 0.045(3) 0.120(5) 0.036 Uiso 1 1 d . . . H17B H 0.166(3) -0.038(3) 0.016(4) 0.036 Uiso 1 1 d . . . C18 C 0.19922(19) -0.0707(2) 0.2604(4) 0.0217(8) Uani 1 1 d . . . C19 C 0.0995(2) -0.0555(2) 0.2918(8) 0.0414(11) Uani 1 1 d D . . H19A H 0.062(3) -0.082(3) 0.194(4) 0.062 Uiso 1 1 d D . . H19B H 0.094(3) 0.0138(7) 0.289(6) 0.062 Uiso 1 1 d D . . H19C H 0.078(3) -0.082(3) 0.404(3) 0.062 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01081(19) 0.01081(19) 0.0089(3) 0.00012(18) 0.00012(18) -0.0052(2) O1 0.0126(13) 0.0126(13) 0.0077(18) 0.000 0.000 -0.006(2) Br1 0.01508(19) 0.01508(19) 0.0076(3) 0.000 0.000 0.0061(2) Cl1 0.0140(3) 0.0140(3) 0.0108(5) -0.0015(3) -0.0015(3) -0.0035(4) N11 0.0097(10) 0.0097(10) 0.0049(19) -0.0003(9) -0.0003(9) -0.0042(14) C11 0.0128(15) 0.0118(15) 0.0141(17) 0.0026(12) -0.0017(12) -0.0023(11) O11 0.0146(10) 0.0146(10) 0.0183(18) 0.0008(9) 0.0008(9) -0.0050(13) N12 0.0115(13) 0.0098(13) 0.0188(14) 0.0003(12) -0.0031(10) -0.0004(12) C12 0.0084(15) 0.0171(15) 0.0191(17) 0.0019(14) -0.0024(12) -0.0051(12) O12 0.031(3) 0.012(2) 0.066(5) 0.012(3) 0.007(3) 0.001(2) N13 0.029(2) 0.067(3) 0.035(2) 0.039(2) -0.0217(16) -0.0344(19) C13 0.0157(14) 0.0157(14) 0.013(2) 0.0001(12) 0.0001(12) -0.0088(18) O13 0.051(4) 0.025(3) 0.026(3) -0.018(2) 0.013(3) -0.021(3) O14 0.052(4) 0.054(4) 0.011(2) 0.015(2) -0.013(2) -0.013(3) C16 0.014(2) 0.0098(17) 0.038(2) -0.0051(14) 0.0042(16) 0.0015(14) C17 0.029(2) 0.019(2) 0.041(2) 0.0136(16) -0.0248(19) -0.0088(15) C18 0.0091(15) 0.0126(16) 0.043(2) 0.0052(15) -0.0070(15) -0.0006(11) C19 0.0090(18) 0.0179(18) 0.097(4) 0.000(2) -0.006(2) 0.0012(14) _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 O1 2.0075(12) . ? Fe1 N12 2.181(3) 8_545 ? Fe1 N12 2.181(3) . ? Fe1 N13 2.220(3) 8_545 ? Fe1 N13 2.220(3) . ? Fe1 N11 2.230(3) . ? O1 Fe1 2.0075(12) 2_655 ? O1 H1 0.847(10) . ? Cl1 O14 1.414(5) 8_545 ? Cl1 O14 1.414(5) . ? Cl1 O12 1.426(5) 8_545 ? Cl1 O12 1.426(5) . ? Cl1 O13 1.435(5) 8_545 ? Cl1 O13 1.435(5) . ? Cl1 O11 1.452(3) . ? N11 C11 1.354(3) 8_545 ? N11 C11 1.354(3) . ? C11 C12 1.398(4) . ? C11 C18 1.533(4) . ? N12 C16 1.473(4) . ? N12 H12A 0.91(3) . ? N12 H12B 0.93(3) . ? C12 C13 1.382(4) . ? C12 H12 0.96(3) . ? O12 O13 1.203(7) . ? O12 O14 1.473(8) . ? N13 C17 1.480(6) . ? N13 H13A 0.847(10) . ? N13 H13B 0.81(5) . ? C13 C12 1.382(4) 8_545 ? C13 H13 0.96(5) . ? O13 O13 1.479(12) 8_545 ? O14 O14 1.231(12) 8_545 ? C16 C18 1.556(5) . ? C16 H16A 0.86(4) . ? C16 H16B 0.91(4) . ? C17 C18 1.546(5) . ? C17 H17A 1.06(4) . ? C17 H17B 1.05(4) . ? C18 C19 1.544(5) . ? C19 H19A 1.054(10) . ? C19 H19B 1.050(10) . ? C19 H19C 1.042(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 O1 Fe1 N12 96.64(10) . 8_545 ? O1 Fe1 N12 96.64(10) . . ? N12 Fe1 N12 96.70(15) 8_545 . ? O1 Fe1 N13 93.72(11) . 8_545 ? N12 Fe1 N13 84.57(15) 8_545 8_545 ? N12 Fe1 N13 169.34(12) . 8_545 ? O1 Fe1 N13 93.72(11) . . ? N12 Fe1 N13 169.34(12) 8_545 . ? N12 Fe1 N13 84.57(15) . . ? N13 Fe1 N13 92.3(3) 8_545 . ? O1 Fe1 N11 173.82(14) . . ? N12 Fe1 N11 87.45(9) 8_545 . ? N12 Fe1 N11 87.45(9) . . ? N13 Fe1 N11 82.02(11) 8_545 . ? N13 Fe1 N11 82.02(11) . . ? Fe1 O1 Fe1 146.7(2) 2_655 . ? Fe1 O1 H1 106.65(10) 2_655 . ? Fe1 O1 H1 106.65(10) . . ? O14 Cl1 O14 51.6(5) 8_545 . ? O14 Cl1 O12 62.5(3) 8_545 8_545 ? O14 Cl1 O12 111.0(3) . 8_545 ? O14 Cl1 O12 111.0(3) 8_545 . ? O14 Cl1 O12 62.5(3) . . ? O12 Cl1 O12 141.0(4) 8_545 . ? O14 Cl1 O13 109.2(3) 8_545 8_545 ? O14 Cl1 O13 141.0(3) . 8_545 ? O12 Cl1 O13 49.7(3) 8_545 8_545 ? O12 Cl1 O13 108.9(4) . 8_545 ? O14 Cl1 O13 141.0(3) 8_545 . ? O14 Cl1 O13 109.2(3) . . ? O12 Cl1 O13 108.9(4) 8_545 . ? O12 Cl1 O13 49.7(3) . . ? O13 Cl1 O13 62.0(5) 8_545 . ? O14 Cl1 O11 109.6(3) 8_545 . ? O14 Cl1 O11 109.6(3) . . ? O12 Cl1 O11 109.0(2) 8_545 . ? O12 Cl1 O11 109.0(2) . . ? O13 Cl1 O11 109.0(2) 8_545 . ? O13 Cl1 O11 109.0(2) . . ? C11 N11 C11 119.7(3) 8_545 . ? C11 N11 Fe1 119.42(17) 8_545 . ? C11 N11 Fe1 119.42(17) . . ? N11 C11 C12 121.1(3) . . ? N11 C11 C18 116.8(3) . . ? C12 C11 C18 122.1(3) . . ? C16 N12 Fe1 115.2(2) . . ? C16 N12 H12A 115(2) . . ? Fe1 N12 H12A 108(2) . . ? C16 N12 H12B 109(2) . . ? Fe1 N12 H12B 108(2) . . ? H12A N12 H12B 102(3) . . ? C13 C12 C11 119.3(3) . . ? C13 C12 H12 122.5(19) . . ? C11 C12 H12 118.2(19) . . ? O13 O12 Cl1 65.5(4) . . ? O13 O12 O14 120.1(5) . . ? Cl1 O12 O14 58.3(3) . . ? C17 N13 Fe1 116.7(3) . . ? C17 N13 H13A 96(3) . . ? Fe1 N13 H13A 104(3) . . ? C17 N13 H13B 104(4) . . ? Fe1 N13 H13B 121(4) . . ? H13A N13 H13B 114(5) . . ? C12 C13 C12 119.4(4) 8_545 . ? C12 C13 H13 119.8(4) 8_545 . ? C12 C13 H13 119.8(4) . . ? O12 O13 Cl1 64.8(3) . . ? O12 O13 O13 120.2(4) . 8_545 ? Cl1 O13 O13 59.0(3) . 8_545 ? O14 O14 Cl1 64.2(2) 8_545 . ? O14 O14 O12 119.7(3) 8_545 . ? Cl1 O14 O12 59.2(3) . . ? N12 C16 C18 114.8(3) . . ? N12 C16 H16A 105(2) . . ? C18 C16 H16A 108(3) . . ? N12 C16 H16B 109(2) . . ? C18 C16 H16B 112(2) . . ? H16A C16 H16B 108(3) . . ? N13 C17 C18 114.2(3) . . ? N13 C17 H17A 115(2) . . ? C18 C17 H17A 105(2) . . ? N13 C17 H17B 114(2) . . ? C18 C17 H17B 107(2) . . ? H17A C17 H17B 101(3) . . ? C11 C18 C19 110.9(3) . . ? C11 C18 C17 111.8(3) . . ? C19 C18 C17 105.3(3) . . ? C11 C18 C16 109.7(3) . . ? C19 C18 C16 105.8(3) . . ? C17 C18 C16 113.1(3) . . ? C18 C19 H19A 110(3) . . ? C18 C19 H19B 103(2) . . ? H19A C19 H19B 109(4) . . ? C18 C19 H19C 113(3) . . ? H19A C19 H19C 110(3) . . ? H19B C19 H19C 112(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 O1 H1 Br1 0.847(10) 2.523(11) 3.370(4) 180.0 1_554 N12 H12A Br1 0.91(3) 2.73(3) 3.629(3) 171(3) . N12 H12B O11 0.93(3) 2.26(4) 3.159(4) 161(3) 4 N13 H13B O13 0.81(5) 2.13(5) 2.782(6) 138(5) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.440 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.097 #===END OF ALL DATA