# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Christopher M. Kozak' _publ_contact_author_address ;Department of Chemistry Memorial University of Newfoundland St. John's, NL A1B 3X7 CANADA ; _publ_contact_author_email ckozak@mun.ca _publ_contact_author_phone 1-709-737-8082 _publ_contact_author_fax 1-709-737-3702 loop_ _publ_author_name _publ_author_address C.M.Kozak ;Department of Chemistry Memorial University of Newfoundland St. John's, NL A1B 3X7 CANADA ; X.Qian ;Department of Chemistry Memorial University of Newfoundland St. John's, NL A1B 3X7 CANADA ; L.N.Dawe ;Centre for Chemical Analysis, Research and Training Memorial University of Newfoundland St. John's, NL A1B 3X7 CANADA ; _publ_section_title ; 'Add Later' ; data_Complex1 _database_code_depnum_ccdc_archive 'CCDC 776031' _publ_section_abstract ; Please see full paper. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H78 Cl2 Fe2 N2 O4' _chemical_formula_sum 'C54 H78 Cl2 Fe2 N2 O4' _chemical_formula_weight 1001.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.997(6) _cell_length_b 11.386(8) _cell_length_c 12.879(9) _cell_angle_alpha 80.65(5) _cell_angle_beta 71.77(4) _cell_angle_gamma 73.69(5) _cell_volume 1331.9(16) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6015 _cell_measurement_theta_min 2.5223 _cell_measurement_theta_max 31.1149 _exptl_crystal_description Chunk _exptl_crystal_colour Black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9213 _exptl_absorpt_correction_T_min 0.8688 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 10935 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0524 _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 -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.50 _reflns_number_total 5309 _reflns_number_gt 4897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1420P)^2^+2.8333P] 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 SHELXL _refine_ls_extinction_coef 0.018(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5309 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_ref 0.2516 _refine_ls_wR_factor_gt 0.2463 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 0.37708(6) 0.60895(5) 0.44287(4) 0.0303(3) Uani 1 1 d . . . Cl1 Cl 0.44969(11) 0.39826(10) 0.45168(9) 0.0411(3) Uani 1 1 d . . . O1 O 0.4717(3) 0.7046(3) 0.3338(2) 0.0347(6) Uani 1 1 d . . . O2 O 0.2260(3) 0.6670(3) 0.5590(2) 0.0335(6) Uani 1 1 d . . . N1 N 0.2272(3) 0.6199(3) 0.3475(3) 0.0292(7) Uani 1 1 d . . . C1 C 0.4657(4) 0.7482(4) 0.2322(3) 0.0298(8) Uani 1 1 d . . . C2 C 0.5906(4) 0.7685(4) 0.1515(3) 0.0312(8) Uani 1 1 d . . . C3 C 0.7365(5) 0.7397(4) 0.1777(4) 0.0381(9) Uani 1 1 d . . . C4 C 0.7817(5) 0.6032(5) 0.2089(5) 0.0517(12) Uani 1 1 d . . . H1 H 0.7811 0.5572 0.1511 0.062 Uiso 1 1 calc R . . H2 H 0.7135 0.5817 0.2781 0.062 Uiso 1 1 calc R . . H3 H 0.8797 0.5823 0.2179 0.062 Uiso 1 1 calc R . . C5 C 0.7222(5) 0.8153(5) 0.2702(4) 0.0460(11) Uani 1 1 d . . . H4 H 0.6994 0.9029 0.2458 0.055 Uiso 1 1 calc R . . H5 H 0.8138 0.7933 0.2897 0.055 Uiso 1 1 calc R . . H6 H 0.6440 0.7983 0.3344 0.055 Uiso 1 1 calc R . . C6 C 0.8552(5) 0.7728(5) 0.0784(4) 0.0508(12) Uani 1 1 d . . . H7 H 0.8750 0.7188 0.0205 0.061 Uiso 1 1 calc R . . H8 H 0.9439 0.7626 0.0998 0.061 Uiso 1 1 calc R . . H9 H 0.8228 0.8584 0.0510 0.061 Uiso 1 1 calc R . . C7 C 0.5756(5) 0.8131(4) 0.0483(3) 0.0346(9) Uani 1 1 d . . . H10 H 0.6584 0.8288 -0.0074 0.042 Uiso 1 1 calc R . . C8 C 0.4463(5) 0.8359(4) 0.0219(3) 0.0358(9) Uani 1 1 d . . . C9 C 0.4402(6) 0.8801(5) -0.0930(4) 0.0458(11) Uani 1 1 d . . . H11 H 0.4881 0.8122 -0.1402 0.055 Uiso 1 1 calc R . . H12 H 0.4899 0.9467 -0.1200 0.055 Uiso 1 1 calc R . . H13 H 0.3386 0.9104 -0.0938 0.055 Uiso 1 1 calc R . . C10 C 0.3264(4) 0.8141(4) 0.1029(3) 0.0337(8) Uani 1 1 d . . . H14 H 0.2365 0.8296 0.0864 0.040 Uiso 1 1 calc R . . C11 C 0.3342(4) 0.7700(4) 0.2081(3) 0.0324(8) Uani 1 1 d . . . C12 C 0.2038(4) 0.7475(4) 0.2946(3) 0.0328(8) Uani 1 1 d . . . H15 H 0.1223 0.7634 0.2619 0.039 Uiso 1 1 calc R . . H16 H 0.1760 0.8060 0.3513 0.039 Uiso 1 1 calc R . . C13 C 0.2876(4) 0.5257(4) 0.2668(4) 0.0352(9) Uani 1 1 d . . . H17 H 0.2928 0.4437 0.3075 0.042 Uiso 1 1 calc R . . H18 H 0.3881 0.5301 0.2258 0.042 Uiso 1 1 calc R . . C14 C 0.2032(5) 0.5366(5) 0.1849(4) 0.0497(12) Uani 1 1 d . . . H19 H 0.1004 0.5383 0.2244 0.060 Uiso 1 1 calc R . . H20 H 0.2060 0.6143 0.1378 0.060 Uiso 1 1 calc R . . C15 C 0.2677(8) 0.4291(7) 0.1141(6) 0.0760(19) Uani 1 1 d . . . H21 H 0.3693 0.3942 0.1138 0.091 Uiso 1 1 calc R . . H22 H 0.2630 0.4574 0.0390 0.091 Uiso 1 1 calc R . . H23 H 0.2127 0.3664 0.1438 0.091 Uiso 1 1 calc R . . C16 C 0.0910(4) 0.5977(4) 0.4276(4) 0.0384(9) Uani 1 1 d . . . H24 H 0.1146 0.5175 0.4696 0.046 Uiso 1 1 calc R . . H25 H 0.0245 0.5919 0.3866 0.046 Uiso 1 1 calc R . . C17 C 0.0134(4) 0.6943(4) 0.5067(3) 0.0357(9) Uani 1 1 d . . . C18 C -0.1325(5) 0.7524(5) 0.5187(4) 0.0446(11) Uani 1 1 d . . . H26 H -0.1822 0.7323 0.4746 0.053 Uiso 1 1 calc R . . C19 C -0.2055(5) 0.8384(5) 0.5935(4) 0.0462(11) Uani 1 1 d . . . C20 C -0.3641(5) 0.9021(6) 0.6040(5) 0.0602(15) Uani 1 1 d . . . H27 H -0.3817 0.9124 0.5320 0.072 Uiso 1 1 calc R . . H28 H -0.3870 0.9828 0.6316 0.072 Uiso 1 1 calc R . . H29 H -0.4259 0.8522 0.6552 0.072 Uiso 1 1 calc R . . C21 C -0.1329(5) 0.8673(4) 0.6564(4) 0.0441(11) Uani 1 1 d . . . H30 H -0.1842 0.9278 0.7072 0.053 Uiso 1 1 calc R . . C22 C 0.0142(5) 0.8113(4) 0.6492(4) 0.0380(9) Uani 1 1 d . . . C23 C 0.0933(5) 0.8446(4) 0.7188(4) 0.0396(10) Uani 1 1 d . . . C24 C 0.1540(5) 0.7309(4) 0.7869(4) 0.0446(10) Uani 1 1 d . . . H34 H 0.2209 0.6688 0.7378 0.054 Uiso 1 1 calc R . . H35 H 0.0739 0.6974 0.8358 0.054 Uiso 1 1 calc R . . H36 H 0.2060 0.7534 0.8306 0.054 Uiso 1 1 calc R . . C25 C -0.0059(6) 0.9399(5) 0.7989(4) 0.0529(12) Uani 1 1 d . . . H31 H -0.0250 1.0207 0.7586 0.063 Uiso 1 1 calc R . . H32 H 0.0416 0.9432 0.8540 0.063 Uiso 1 1 calc R . . H33 H -0.0979 0.9168 0.8353 0.063 Uiso 1 1 calc R . . C26 C 0.2178(6) 0.8998(5) 0.6450(5) 0.0553(14) Uani 1 1 d . . . H37 H 0.2788 0.8443 0.5881 0.066 Uiso 1 1 calc R . . H38 H 0.2766 0.9108 0.6892 0.066 Uiso 1 1 calc R . . H39 H 0.1776 0.9795 0.6103 0.066 Uiso 1 1 calc R . . C27 C 0.0844(4) 0.7242(4) 0.5725(3) 0.0347(9) 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 0.0213(4) 0.0393(4) 0.0296(4) -0.0025(2) -0.0058(2) -0.0079(2) Cl1 0.0321(6) 0.0482(6) 0.0432(6) -0.0021(4) -0.0147(4) -0.0063(4) O1 0.0289(14) 0.0468(16) 0.0316(15) 0.0013(12) -0.0106(11) -0.0147(12) O2 0.0223(13) 0.0414(15) 0.0346(15) -0.0065(12) -0.0071(11) -0.0038(11) N1 0.0196(14) 0.0375(17) 0.0268(16) -0.0033(13) -0.0012(12) -0.0067(12) C1 0.0307(19) 0.0344(19) 0.0265(18) -0.0018(14) -0.0076(15) -0.0121(15) C2 0.0284(19) 0.0347(19) 0.032(2) -0.0038(15) -0.0063(15) -0.0117(15) C3 0.029(2) 0.050(2) 0.038(2) 0.0033(18) -0.0091(17) -0.0189(18) C4 0.030(2) 0.058(3) 0.061(3) 0.005(2) -0.012(2) -0.006(2) C5 0.043(2) 0.066(3) 0.042(2) 0.002(2) -0.018(2) -0.029(2) C6 0.035(2) 0.072(3) 0.047(3) 0.005(2) -0.012(2) -0.022(2) C7 0.037(2) 0.037(2) 0.031(2) -0.0021(15) -0.0090(16) -0.0125(17) C8 0.040(2) 0.037(2) 0.030(2) -0.0016(15) -0.0099(17) -0.0095(17) C9 0.054(3) 0.052(3) 0.035(2) 0.0001(19) -0.018(2) -0.015(2) C10 0.0287(19) 0.038(2) 0.033(2) -0.0054(15) -0.0104(16) -0.0036(16) C11 0.0259(18) 0.040(2) 0.032(2) -0.0051(15) -0.0087(15) -0.0062(15) C12 0.0197(17) 0.042(2) 0.033(2) -0.0079(16) -0.0050(15) -0.0023(15) C13 0.0256(18) 0.045(2) 0.038(2) -0.0098(17) -0.0110(16) -0.0071(16) C14 0.038(2) 0.068(3) 0.051(3) -0.019(2) -0.021(2) -0.008(2) C15 0.085(5) 0.080(4) 0.079(5) -0.035(4) -0.037(4) -0.014(4) C16 0.0223(18) 0.058(3) 0.037(2) -0.0070(18) -0.0028(16) -0.0168(18) C17 0.0232(18) 0.046(2) 0.033(2) -0.0002(17) -0.0022(15) -0.0095(16) C18 0.024(2) 0.071(3) 0.035(2) 0.005(2) -0.0071(16) -0.012(2) C19 0.024(2) 0.066(3) 0.035(2) 0.006(2) -0.0025(17) -0.0018(19) C20 0.027(2) 0.082(4) 0.048(3) 0.006(3) 0.002(2) 0.004(2) C21 0.032(2) 0.046(2) 0.038(2) 0.0029(18) 0.0013(18) -0.0003(18) C22 0.031(2) 0.037(2) 0.039(2) 0.0042(17) -0.0044(17) -0.0072(16) C23 0.038(2) 0.037(2) 0.040(2) -0.0068(17) -0.0029(18) -0.0093(18) C24 0.046(3) 0.044(2) 0.042(2) -0.0128(19) -0.013(2) -0.003(2) C25 0.054(3) 0.046(3) 0.049(3) -0.016(2) -0.005(2) -0.004(2) C26 0.045(3) 0.052(3) 0.069(4) -0.020(2) 0.001(2) -0.023(2) C27 0.0223(18) 0.038(2) 0.037(2) 0.0001(16) -0.0042(15) -0.0049(15) _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 O2 1.817(3) . ? Fe1 O1 1.818(3) . ? Fe1 N1 2.183(4) . ? Fe1 Cl1 2.298(2) . ? Fe1 Cl1 2.4911(18) 2_666 ? Cl1 Fe1 2.4912(18) 2_666 ? O1 C1 1.335(5) . ? O2 C27 1.350(5) . ? N1 C13 1.484(5) . ? N1 C16 1.487(5) . ? N1 C12 1.489(5) . ? C1 C11 1.390(6) . ? C1 C2 1.402(5) . ? C2 C7 1.381(6) . ? C2 C3 1.534(6) . ? C3 C4 1.516(7) . ? C3 C6 1.527(6) . ? C3 C5 1.529(7) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.382(6) . ? C7 H10 0.9500 . ? C8 C10 1.374(6) . ? C8 C9 1.498(6) . ? C9 H11 0.9800 . ? C9 H12 0.9800 . ? C9 H13 0.9800 . ? C10 C11 1.385(6) . ? C10 H14 0.9500 . ? C11 C12 1.480(5) . ? C12 H15 0.9900 . ? C12 H16 0.9900 . ? C13 C14 1.516(6) . ? C13 H17 0.9900 . ? C13 H18 0.9900 . ? C14 C15 1.515(8) . ? C14 H19 0.9900 . ? C14 H20 0.9900 . ? C15 H21 0.9800 . ? C15 H22 0.9800 . ? C15 H23 0.9800 . ? C16 C17 1.497(6) . ? C16 H24 0.9900 . ? C16 H25 0.9900 . ? C17 C18 1.393(6) . ? C17 C27 1.394(6) . ? C18 C19 1.373(7) . ? C18 H26 0.9500 . ? C19 C21 1.371(7) . ? C19 C20 1.520(6) . ? C20 H27 0.9800 . ? C20 H28 0.9800 . ? C20 H29 0.9800 . ? C21 C22 1.409(6) . ? C21 H30 0.9500 . ? C22 C27 1.396(6) . ? C22 C23 1.514(7) . ? C23 C24 1.528(7) . ? C23 C25 1.531(6) . ? C23 C26 1.534(6) . ? C24 H34 0.9800 . ? C24 H35 0.9800 . ? C24 H36 0.9800 . ? C25 H31 0.9800 . ? C25 H32 0.9800 . ? C25 H33 0.9800 . ? C26 H37 0.9800 . ? C26 H38 0.9800 . ? C26 H39 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 O2 Fe1 O1 124.63(14) . . ? O2 Fe1 N1 90.62(13) . . ? O1 Fe1 N1 88.99(13) . . ? O2 Fe1 Cl1 113.18(11) . . ? O1 Fe1 Cl1 122.08(12) . . ? N1 Fe1 Cl1 93.92(10) . . ? O2 Fe1 Cl1 89.86(11) . 2_666 ? O1 Fe1 Cl1 89.41(11) . 2_666 ? N1 Fe1 Cl1 178.32(9) . 2_666 ? Cl1 Fe1 Cl1 87.36(6) . 2_666 ? Fe1 Cl1 Fe1 92.64(6) . 2_666 ? C1 O1 Fe1 135.5(2) . . ? C27 O2 Fe1 134.6(3) . . ? C13 N1 C16 110.0(3) . . ? C13 N1 C12 112.7(3) . . ? C16 N1 C12 111.3(3) . . ? C13 N1 Fe1 111.0(2) . . ? C16 N1 Fe1 106.3(2) . . ? C12 N1 Fe1 105.3(2) . . ? O1 C1 C11 118.5(3) . . ? O1 C1 C2 120.3(4) . . ? C11 C1 C2 121.2(4) . . ? C7 C2 C1 116.8(4) . . ? C7 C2 C3 122.5(4) . . ? C1 C2 C3 120.8(4) . . ? C4 C3 C6 108.1(4) . . ? C4 C3 C5 111.5(4) . . ? C6 C3 C5 107.6(4) . . ? C4 C3 C2 108.8(4) . . ? C6 C3 C2 111.2(4) . . ? C5 C3 C2 109.7(4) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C2 C7 C8 123.4(4) . . ? C2 C7 H10 118.3 . . ? C8 C7 H10 118.3 . . ? C10 C8 C7 118.2(4) . . ? C10 C8 C9 121.6(4) . . ? C7 C8 C9 120.2(4) . . ? C8 C9 H11 109.5 . . ? C8 C9 H12 109.5 . . ? H11 C9 H12 109.5 . . ? C8 C9 H13 109.5 . . ? H11 C9 H13 109.5 . . ? H12 C9 H13 109.5 . . ? C8 C10 C11 121.2(4) . . ? C8 C10 H14 119.4 . . ? C11 C10 H14 119.4 . . ? C10 C11 C1 119.3(4) . . ? C10 C11 C12 120.5(4) . . ? C1 C11 C12 120.2(4) . . ? C11 C12 N1 112.8(3) . . ? C11 C12 H15 109.0 . . ? N1 C12 H15 109.0 . . ? C11 C12 H16 109.0 . . ? N1 C12 H16 109.0 . . ? H15 C12 H16 107.8 . . ? N1 C13 C14 115.5(4) . . ? N1 C13 H17 108.4 . . ? C14 C13 H17 108.4 . . ? N1 C13 H18 108.4 . . ? C14 C13 H18 108.4 . . ? H17 C13 H18 107.5 . . ? C15 C14 C13 110.3(4) . . ? C15 C14 H19 109.6 . . ? C13 C14 H19 109.6 . . ? C15 C14 H20 109.6 . . ? C13 C14 H20 109.6 . . ? H19 C14 H20 108.1 . . ? C14 C15 H21 109.5 . . ? C14 C15 H22 109.5 . . ? H21 C15 H22 109.5 . . ? C14 C15 H23 109.5 . . ? H21 C15 H23 109.5 . . ? H22 C15 H23 109.5 . . ? N1 C16 C17 114.4(4) . . ? N1 C16 H24 108.7 . . ? C17 C16 H24 108.7 . . ? N1 C16 H25 108.7 . . ? C17 C16 H25 108.7 . . ? H24 C16 H25 107.6 . . ? C18 C17 C27 119.0(4) . . ? C18 C17 C16 120.5(4) . . ? C27 C17 C16 120.5(4) . . ? C19 C18 C17 120.7(5) . . ? C19 C18 H26 119.6 . . ? C17 C18 H26 119.6 . . ? C21 C19 C18 119.3(4) . . ? C21 C19 C20 120.9(5) . . ? C18 C19 C20 119.8(5) . . ? C19 C20 H27 109.5 . . ? C19 C20 H28 109.5 . . ? H27 C20 H28 109.5 . . ? C19 C20 H29 109.5 . . ? H27 C20 H29 109.5 . . ? H28 C20 H29 109.5 . . ? C19 C21 C22 123.0(5) . . ? C19 C21 H30 118.5 . . ? C22 C21 H30 118.5 . . ? C27 C22 C21 116.0(4) . . ? C27 C22 C23 121.5(4) . . ? C21 C22 C23 122.4(4) . . ? C22 C23 C24 110.3(4) . . ? C22 C23 C25 112.4(4) . . ? C24 C23 C25 107.3(4) . . ? C22 C23 C26 109.9(4) . . ? C24 C23 C26 109.6(4) . . ? C25 C23 C26 107.2(4) . . ? C23 C24 H34 109.5 . . ? C23 C24 H35 109.5 . . ? H34 C24 H35 109.5 . . ? C23 C24 H36 109.5 . . ? H34 C24 H36 109.5 . . ? H35 C24 H36 109.5 . . ? C23 C25 H31 109.5 . . ? C23 C25 H32 109.5 . . ? H31 C25 H32 109.5 . . ? C23 C25 H33 109.5 . . ? H31 C25 H33 109.5 . . ? H32 C25 H33 109.5 . . ? C23 C26 H37 109.5 . . ? C23 C26 H38 109.5 . . ? H37 C26 H38 109.5 . . ? C23 C26 H39 109.5 . . ? H37 C26 H39 109.5 . . ? H38 C26 H39 109.5 . . ? O2 C27 C17 117.8(4) . . ? O2 C27 C22 120.1(4) . . ? C17 C27 C22 122.0(4) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.065 _refine_diff_density_min -1.094 _refine_diff_density_rms 0.131 #===END data_Complex2 _database_code_depnum_ccdc_archive 'CCDC 793580' _publ_section_abstract ; Not for publication ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C33 H48 N O2)2 Fe2] Cl2' _chemical_formula_sum 'C66 H102 Cl2 Fe2 N2 O4' _chemical_formula_weight 1170.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.248(8) _cell_length_b 11.616(9) _cell_length_c 14.662(12) _cell_angle_alpha 99.827(14) _cell_angle_beta 104.057(12) _cell_angle_gamma 92.03(2) _cell_volume 1663(2) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6683 _cell_measurement_theta_min 2.7660 _cell_measurement_theta_max 30.8904 _exptl_crystal_description Irrgular _exptl_crystal_colour 'Dark Brown' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 630 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9484 _exptl_absorpt_correction_T_min 0.9193 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; The bulk sample contained crystals of very poor quality (irregular in shape/cracked, etc...) Data was collected for one crystal, and this .cif contains the refinement details for this crystal. This .cif was prepared in order to confirm the similarity in connectivity to a 'sister' complex, and is not intended as a stand-alone report for publication. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 11654 _diffrn_reflns_av_R_equivalents 0.1134 _diffrn_reflns_av_sigmaI/netI 0.0943 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5702 _reflns_number_gt 5163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'DIRDIF99-ORIENT (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5702 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1381 _refine_ls_R_factor_gt 0.1327 _refine_ls_wR_factor_ref 0.3897 _refine_ls_wR_factor_gt 0.3793 _refine_ls_goodness_of_fit_ref 1.627 _refine_ls_restrained_S_all 1.627 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.57077(7) 0.48558(6) 0.40684(5) 0.0357(4) Uani 1 1 d . . . Cl1 Cl 0.6384(2) 0.59507(18) 0.56020(14) 0.0715(6) Uani 1 1 d . . . O1 O 0.6329(3) 0.3391(3) 0.3998(3) 0.0390(8) Uani 1 1 d . . . O2 O 0.4663(3) 0.5505(3) 0.3123(3) 0.0408(9) Uani 1 1 d . . . N1 N 0.7477(4) 0.5540(4) 0.3689(3) 0.0332(9) Uani 1 1 d . . . C1 C 0.7282(5) 0.2857(4) 0.3623(3) 0.0322(10) Uani 1 1 d . . . C2 C 0.7145(5) 0.1643(4) 0.3267(3) 0.0341(11) Uani 1 1 d . . . C3 C 0.5987(5) 0.0842(5) 0.3365(4) 0.0412(12) Uani 1 1 d . . . C4 C 0.6002(8) 0.1021(6) 0.4433(5) 0.0666(19) Uani 1 1 d . . . H1 H 0.6367 0.1822 0.4745 0.080 Uiso 1 1 calc R . . H2 H 0.6568 0.0460 0.4737 0.080 Uiso 1 1 calc R . . H3 H 0.5080 0.0896 0.4497 0.080 Uiso 1 1 calc R . . C5 C 0.4642(6) 0.1165(5) 0.2769(5) 0.0602(17) Uani 1 1 d . . . H4 H 0.4007 0.0465 0.2541 0.072 Uiso 1 1 calc R . . H5 H 0.4798 0.1476 0.2221 0.072 Uiso 1 1 calc R . . H6 H 0.4263 0.1761 0.3167 0.072 Uiso 1 1 calc R . . C6 C 0.6115(6) -0.0438(5) 0.3034(5) 0.0511(14) Uani 1 1 d . . . H7 H 0.5696 -0.0904 0.3400 0.061 Uiso 1 1 calc R . . H8 H 0.7072 -0.0581 0.3135 0.061 Uiso 1 1 calc R . . H9 H 0.5662 -0.0663 0.2353 0.061 Uiso 1 1 calc R . . C7 C 0.8106(5) 0.1203(5) 0.2822(4) 0.0376(11) Uani 1 1 d . . . H10 H 0.8013 0.0389 0.2559 0.045 Uiso 1 1 calc R . . C8 C 0.9215(5) 0.1877(5) 0.2732(4) 0.0403(12) Uani 1 1 d . . . C9 C 1.0204(6) 0.1318(6) 0.2210(5) 0.0585(16) Uani 1 1 d . . . C10 C 0.9491(9) 0.0668(12) 0.1232(9) 0.142(6) Uani 1 1 d . . . H11 H 0.9234 -0.0141 0.1268 0.170 Uiso 1 1 calc R . . H12 H 1.0093 0.0665 0.0805 0.170 Uiso 1 1 calc R . . H13 H 0.8680 0.1054 0.0983 0.170 Uiso 1 1 calc R . . C11 C 1.0939(9) 0.0444(8) 0.2772(9) 0.110(4) Uani 1 1 d . . . H14 H 1.1751 0.0842 0.3236 0.132 Uiso 1 1 calc R . . H15 H 1.1195 -0.0189 0.2331 0.132 Uiso 1 1 calc R . . H16 H 1.0344 0.0114 0.3111 0.132 Uiso 1 1 calc R . . C12 C 1.1272(6) 0.2179(6) 0.2101(6) 0.0627(17) Uani 1 1 d . . . H17 H 1.2102 0.1790 0.2092 0.075 Uiso 1 1 calc R . . H18 H 1.1453 0.2842 0.2639 0.075 Uiso 1 1 calc R . . H19 H 1.0951 0.2465 0.1501 0.075 Uiso 1 1 calc R . . C13 C 0.9340(5) 0.3046(4) 0.3133(4) 0.0393(11) Uani 1 1 d . . . H20 H 1.0090 0.3526 0.3098 0.047 Uiso 1 1 calc R . . C14 C 0.8405(5) 0.3547(4) 0.3586(3) 0.0350(11) Uani 1 1 d . . . C15 C 0.8602(5) 0.4806(4) 0.4054(4) 0.0373(11) Uani 1 1 d . . . H21 H 0.9451 0.5149 0.3967 0.045 Uiso 1 1 calc R . . H22 H 0.8712 0.4854 0.4750 0.045 Uiso 1 1 calc R . . C16 C 0.7864(5) 0.6794(4) 0.4110(4) 0.0392(11) Uani 1 1 d . . . H23 H 0.8174 0.6867 0.4813 0.047 Uiso 1 1 calc R . . H24 H 0.7046 0.7228 0.3974 0.047 Uiso 1 1 calc R . . C17 C 0.8947(6) 0.7382(5) 0.3771(4) 0.0488(14) Uani 1 1 d . . . H25 H 0.9648 0.6835 0.3698 0.059 Uiso 1 1 calc R . . H26 H 0.8547 0.7583 0.3137 0.059 Uiso 1 1 calc R . . C18 C 0.9582(6) 0.8479(5) 0.4468(5) 0.0586(17) Uani 1 1 d . . . H27 H 0.9534 0.8395 0.5114 0.070 Uiso 1 1 calc R . . H28 H 0.9097 0.9151 0.4289 0.070 Uiso 1 1 calc R . . H29 H 1.0528 0.8603 0.4457 0.070 Uiso 1 1 calc R . . C19 C 0.7142(4) 0.5314(4) 0.2623(3) 0.0325(10) Uani 1 1 d . . . H30 H 0.7970 0.5486 0.2420 0.039 Uiso 1 1 calc R . . H31 H 0.6859 0.4470 0.2386 0.039 Uiso 1 1 calc R . . C20 C 0.6063(5) 0.6004(4) 0.2157(4) 0.0369(11) Uani 1 1 d . . . C21 C 0.6233(5) 0.6486(4) 0.1396(3) 0.0388(11) Uani 1 1 d . . . H32 H 0.7081 0.6472 0.1242 0.047 Uiso 1 1 calc R . . C22 C 0.5186(6) 0.6994(5) 0.0846(4) 0.0457(13) Uani 1 1 d . . . C23 C 0.5362(7) 0.7481(5) -0.0032(4) 0.0535(15) Uani 1 1 d . . . C24 C 0.5950(9) 0.6571(6) -0.0656(5) 0.071(2) Uani 1 1 d . . . H33 H 0.5650 0.5784 -0.0592 0.085 Uiso 1 1 calc R . . H34 H 0.6937 0.6679 -0.0454 0.085 Uiso 1 1 calc R . . H35 H 0.5641 0.6660 -0.1326 0.085 Uiso 1 1 calc R . . C25 C 0.6305(11) 0.8580(7) 0.0286(5) 0.093(3) Uani 1 1 d . . . H36 H 0.6948 0.8541 0.0894 0.112 Uiso 1 1 calc R . . H37 H 0.5783 0.9264 0.0372 0.112 Uiso 1 1 calc R . . H38 H 0.6797 0.8651 -0.0200 0.112 Uiso 1 1 calc R . . C26 C 0.4002(9) 0.7739(10) -0.0654(6) 0.096(3) Uani 1 1 d . . . H39 H 0.3611 0.7040 -0.1133 0.115 Uiso 1 1 calc R . . H40 H 0.4145 0.8388 -0.0976 0.115 Uiso 1 1 calc R . . H41 H 0.3385 0.7955 -0.0248 0.115 Uiso 1 1 calc R . . C27 C 0.3984(6) 0.7028(5) 0.1119(4) 0.0439(13) Uani 1 1 d . . . H42 H 0.3272 0.7396 0.0762 0.053 Uiso 1 1 calc R . . C28 C 0.3755(5) 0.6564(4) 0.1876(4) 0.0408(12) Uani 1 1 d . . . C29 C 0.2410(5) 0.6630(5) 0.2172(5) 0.0501(14) Uani 1 1 d . . . C30 C 0.1379(6) 0.7238(6) 0.1482(6) 0.0652(18) Uani 1 1 d . . . H43 H 0.1471 0.8084 0.1728 0.078 Uiso 1 1 calc R . . H44 H 0.0461 0.6923 0.1438 0.078 Uiso 1 1 calc R . . H45 H 0.1555 0.7090 0.0847 0.078 Uiso 1 1 calc R . . C31 C 0.1770(6) 0.5368(6) 0.2092(6) 0.0628(18) Uani 1 1 d . . . H46 H 0.1198 0.5096 0.1444 0.075 Uiso 1 1 calc R . . H47 H 0.1223 0.5376 0.2556 0.075 Uiso 1 1 calc R . . H48 H 0.2488 0.4839 0.2227 0.075 Uiso 1 1 calc R . . C32 C 0.2622(6) 0.7312(6) 0.3165(5) 0.0576(16) Uani 1 1 d . . . H49 H 0.1806 0.7700 0.3223 0.069 Uiso 1 1 calc R . . H50 H 0.3384 0.7903 0.3298 0.069 Uiso 1 1 calc R . . H51 H 0.2817 0.6780 0.3624 0.069 Uiso 1 1 calc R . . C33 C 0.4835(5) 0.6023(4) 0.2397(3) 0.0351(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0325(6) 0.0302(6) 0.0465(6) 0.0091(4) 0.0124(4) 0.0031(4) Cl1 0.0826(14) 0.0702(12) 0.0745(12) 0.0176(9) 0.0403(10) 0.0127(10) O1 0.0324(18) 0.0310(18) 0.055(2) 0.0095(14) 0.0137(15) -0.0009(15) O2 0.0275(17) 0.040(2) 0.056(2) 0.0153(15) 0.0087(15) 0.0029(15) N1 0.026(2) 0.025(2) 0.043(2) 0.0048(16) 0.0014(16) -0.0006(16) C1 0.024(2) 0.034(2) 0.038(2) 0.0084(18) 0.0055(18) 0.0018(19) C2 0.027(2) 0.030(2) 0.043(3) 0.0108(19) 0.0016(19) -0.005(2) C3 0.034(3) 0.033(3) 0.055(3) 0.011(2) 0.007(2) -0.004(2) C4 0.088(5) 0.050(4) 0.075(4) 0.021(3) 0.042(4) -0.011(4) C5 0.031(3) 0.043(3) 0.105(5) 0.024(3) 0.007(3) -0.008(3) C6 0.038(3) 0.039(3) 0.076(4) 0.009(3) 0.016(3) -0.004(2) C7 0.026(2) 0.035(3) 0.047(3) 0.004(2) 0.003(2) 0.001(2) C8 0.025(2) 0.033(3) 0.058(3) 0.010(2) 0.004(2) -0.003(2) C9 0.038(3) 0.049(3) 0.085(4) -0.006(3) 0.023(3) -0.001(3) C10 0.056(5) 0.179(12) 0.151(10) -0.090(9) 0.044(6) -0.040(6) C11 0.080(6) 0.074(6) 0.232(12) 0.076(7) 0.107(7) 0.047(5) C12 0.041(3) 0.058(4) 0.098(5) 0.016(3) 0.035(3) 0.006(3) C13 0.025(2) 0.031(3) 0.059(3) 0.010(2) 0.004(2) -0.001(2) C14 0.026(2) 0.027(2) 0.047(3) 0.0059(19) 0.0007(19) -0.0007(19) C15 0.025(2) 0.032(3) 0.051(3) 0.008(2) 0.003(2) 0.003(2) C16 0.039(3) 0.022(2) 0.053(3) 0.0000(19) 0.009(2) 0.001(2) C17 0.039(3) 0.029(3) 0.073(4) 0.008(2) 0.004(3) -0.005(2) C18 0.046(3) 0.042(3) 0.071(4) 0.008(3) -0.011(3) -0.016(3) C19 0.024(2) 0.031(2) 0.040(2) 0.0017(18) 0.0069(18) 0.0005(19) C20 0.033(2) 0.027(2) 0.048(3) 0.0082(19) 0.004(2) -0.004(2) C21 0.043(3) 0.032(2) 0.039(3) 0.0028(19) 0.010(2) -0.008(2) C22 0.054(3) 0.033(3) 0.043(3) 0.010(2) -0.002(2) -0.008(2) C23 0.073(4) 0.041(3) 0.042(3) 0.015(2) 0.003(3) -0.008(3) C24 0.100(6) 0.058(4) 0.054(4) 0.012(3) 0.021(4) -0.017(4) C25 0.156(9) 0.059(4) 0.056(4) 0.013(3) 0.017(5) -0.048(5) C26 0.083(6) 0.141(9) 0.074(5) 0.056(5) 0.014(4) 0.014(6) C27 0.040(3) 0.027(2) 0.059(3) 0.009(2) 0.002(2) 0.003(2) C28 0.028(2) 0.028(2) 0.062(3) 0.007(2) 0.004(2) -0.003(2) C29 0.028(3) 0.040(3) 0.087(4) 0.017(3) 0.019(3) 0.006(2) C30 0.037(3) 0.057(4) 0.103(5) 0.023(3) 0.014(3) 0.021(3) C31 0.025(3) 0.043(3) 0.117(6) 0.023(3) 0.008(3) -0.004(2) C32 0.040(3) 0.050(4) 0.090(5) 0.011(3) 0.031(3) 0.007(3) C33 0.029(2) 0.025(2) 0.048(3) 0.0058(19) 0.005(2) -0.0051(19) _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 O2 1.825(4) . ? Fe1 O1 1.834(4) . ? Fe1 N1 2.184(4) . ? Fe1 Cl1 2.315(3) . ? Fe1 Cl1 2.495(3) 2_666 ? Cl1 Fe1 2.495(3) 2_666 ? O1 C1 1.351(6) . ? O2 C33 1.353(6) . ? N1 C16 1.480(6) . ? N1 C19 1.491(6) . ? N1 C15 1.506(6) . ? C1 C14 1.397(7) . ? C1 C2 1.407(7) . ? C2 C7 1.376(7) . ? C2 C3 1.532(7) . ? C3 C6 1.504(8) . ? C3 C5 1.539(7) . ? C3 C4 1.540(8) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.402(7) . ? C7 H10 0.9500 . ? C8 C13 1.373(7) . ? C8 C9 1.512(8) . ? C9 C10 1.498(12) . ? C9 C12 1.512(9) . ? C9 C11 1.522(11) . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C11 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C12 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C13 C14 1.383(7) . ? C13 H20 0.9500 . ? C14 C15 1.491(7) . ? C15 H21 0.9900 . ? C15 H22 0.9900 . ? C16 C17 1.509(8) . ? C16 H23 0.9900 . ? C16 H24 0.9900 . ? C17 C18 1.505(8) . ? C17 H25 0.9900 . ? C17 H26 0.9900 . ? C18 H27 0.9800 . ? C18 H28 0.9800 . ? C18 H29 0.9800 . ? C19 C20 1.488(6) . ? C19 H30 0.9900 . ? C19 H31 0.9900 . ? C20 C21 1.375(7) . ? C20 C33 1.387(7) . ? C21 C22 1.391(8) . ? C21 H32 0.9500 . ? C22 C27 1.384(9) . ? C22 C23 1.539(8) . ? C23 C25 1.507(9) . ? C23 C24 1.517(11) . ? C23 C26 1.538(10) . ? C24 H33 0.9800 . ? C24 H34 0.9800 . ? C24 H35 0.9800 . ? C25 H36 0.9800 . ? C25 H37 0.9800 . ? C25 H38 0.9800 . ? C26 H39 0.9800 . ? C26 H40 0.9800 . ? C26 H41 0.9800 . ? C27 C28 1.377(8) . ? C27 H42 0.9500 . ? C28 C33 1.415(7) . ? C28 C29 1.544(8) . ? C29 C32 1.495(10) . ? C29 C30 1.554(8) . ? C29 C31 1.558(8) . ? C30 H43 0.9800 . ? C30 H44 0.9800 . ? C30 H45 0.9800 . ? C31 H46 0.9800 . ? C31 H47 0.9800 . ? C31 H48 0.9800 . ? C32 H49 0.9800 . ? C32 H50 0.9800 . ? C32 H51 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 O2 Fe1 O1 128.99(17) . . ? O2 Fe1 N1 88.04(16) . . ? O1 Fe1 N1 90.93(16) . . ? O2 Fe1 Cl1 118.89(14) . . ? O1 Fe1 Cl1 112.12(13) . . ? N1 Fe1 Cl1 91.86(12) . . ? O2 Fe1 Cl1 89.23(13) . 2_666 ? O1 Fe1 Cl1 89.18(12) . 2_666 ? N1 Fe1 Cl1 176.57(11) . 2_666 ? Cl1 Fe1 Cl1 91.27(9) . 2_666 ? Fe1 Cl1 Fe1 88.73(9) . 2_666 ? C1 O1 Fe1 134.8(3) . . ? C33 O2 Fe1 137.5(3) . . ? C16 N1 C19 112.5(4) . . ? C16 N1 C15 110.2(4) . . ? C19 N1 C15 109.0(4) . . ? C16 N1 Fe1 113.0(3) . . ? C19 N1 Fe1 105.9(3) . . ? C15 N1 Fe1 105.9(3) . . ? O1 C1 C14 118.2(4) . . ? O1 C1 C2 121.3(4) . . ? C14 C1 C2 120.6(4) . . ? C7 C2 C1 116.7(4) . . ? C7 C2 C3 121.1(4) . . ? C1 C2 C3 122.2(4) . . ? C6 C3 C2 113.4(5) . . ? C6 C3 C5 108.0(5) . . ? C2 C3 C5 109.3(4) . . ? C6 C3 C4 107.6(5) . . ? C2 C3 C4 107.7(4) . . ? C5 C3 C4 110.8(5) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C2 C7 C8 124.3(5) . . ? C2 C7 H10 117.9 . . ? C8 C7 H10 117.9 . . ? C13 C8 C7 116.7(5) . . ? C13 C8 C9 122.9(5) . . ? C7 C8 C9 120.4(5) . . ? C10 C9 C8 111.1(6) . . ? C10 C9 C12 107.8(7) . . ? C8 C9 C12 113.9(5) . . ? C10 C9 C11 108.0(9) . . ? C8 C9 C11 108.9(6) . . ? C12 C9 C11 106.9(6) . . ? C9 C10 H11 109.5 . . ? C9 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C9 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C9 C11 H14 109.5 . . ? C9 C11 H15 109.5 . . ? H14 C11 H15 109.5 . . ? C9 C11 H16 109.5 . . ? H14 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C9 C12 H17 109.5 . . ? C9 C12 H18 109.5 . . ? H17 C12 H18 109.5 . . ? C9 C12 H19 109.5 . . ? H17 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? C8 C13 C14 122.0(5) . . ? C8 C13 H20 119.0 . . ? C14 C13 H20 119.0 . . ? C13 C14 C1 119.6(4) . . ? C13 C14 C15 120.7(4) . . ? C1 C14 C15 119.7(4) . . ? C14 C15 N1 115.1(4) . . ? C14 C15 H21 108.5 . . ? N1 C15 H21 108.5 . . ? C14 C15 H22 108.5 . . ? N1 C15 H22 108.5 . . ? H21 C15 H22 107.5 . . ? N1 C16 C17 116.4(4) . . ? N1 C16 H23 108.2 . . ? C17 C16 H23 108.2 . . ? N1 C16 H24 108.2 . . ? C17 C16 H24 108.2 . . ? H23 C16 H24 107.3 . . ? C18 C17 C16 110.9(5) . . ? C18 C17 H25 109.5 . . ? C16 C17 H25 109.5 . . ? C18 C17 H26 109.5 . . ? C16 C17 H26 109.5 . . ? H25 C17 H26 108.1 . . ? C17 C18 H27 109.5 . . ? C17 C18 H28 109.5 . . ? H27 C18 H28 109.5 . . ? C17 C18 H29 109.5 . . ? H27 C18 H29 109.5 . . ? H28 C18 H29 109.5 . . ? C20 C19 N1 115.1(4) . . ? C20 C19 H30 108.5 . . ? N1 C19 H30 108.5 . . ? C20 C19 H31 108.5 . . ? N1 C19 H31 108.5 . . ? H30 C19 H31 107.5 . . ? C21 C20 C33 120.2(5) . . ? C21 C20 C19 118.7(5) . . ? C33 C20 C19 120.5(4) . . ? C20 C21 C22 121.3(5) . . ? C20 C21 H32 119.4 . . ? C22 C21 H32 119.4 . . ? C27 C22 C21 117.1(5) . . ? C27 C22 C23 121.8(5) . . ? C21 C22 C23 121.0(6) . . ? C25 C23 C24 109.3(7) . . ? C25 C23 C26 109.9(7) . . ? C24 C23 C26 106.8(6) . . ? C25 C23 C22 109.8(5) . . ? C24 C23 C22 109.2(5) . . ? C26 C23 C22 111.7(6) . . ? C23 C24 H33 109.5 . . ? C23 C24 H34 109.5 . . ? H33 C24 H34 109.5 . . ? C23 C24 H35 109.5 . . ? H33 C24 H35 109.5 . . ? H34 C24 H35 109.5 . . ? C23 C25 H36 109.5 . . ? C23 C25 H37 109.5 . . ? H36 C25 H37 109.5 . . ? C23 C25 H38 109.5 . . ? H36 C25 H38 109.5 . . ? H37 C25 H38 109.5 . . ? C23 C26 H39 109.5 . . ? C23 C26 H40 109.5 . . ? H39 C26 H40 109.5 . . ? C23 C26 H41 109.5 . . ? H39 C26 H41 109.5 . . ? H40 C26 H41 109.5 . . ? C28 C27 C22 124.2(5) . . ? C28 C27 H42 117.9 . . ? C22 C27 H42 117.9 . . ? C27 C28 C33 116.7(5) . . ? C27 C28 C29 123.1(5) . . ? C33 C28 C29 120.2(5) . . ? C32 C29 C28 110.8(5) . . ? C32 C29 C30 108.3(5) . . ? C28 C29 C30 110.5(5) . . ? C32 C29 C31 110.8(6) . . ? C28 C29 C31 109.7(5) . . ? C30 C29 C31 106.6(5) . . ? C29 C30 H43 109.5 . . ? C29 C30 H44 109.5 . . ? H43 C30 H44 109.5 . . ? C29 C30 H45 109.5 . . ? H43 C30 H45 109.5 . . ? H44 C30 H45 109.5 . . ? C29 C31 H46 109.5 . . ? C29 C31 H47 109.5 . . ? H46 C31 H47 109.5 . . ? C29 C31 H48 109.5 . . ? H46 C31 H48 109.5 . . ? H47 C31 H48 109.5 . . ? C29 C32 H49 109.5 . . ? C29 C32 H50 109.5 . . ? H49 C32 H50 109.5 . . ? C29 C32 H51 109.5 . . ? H49 C32 H51 109.5 . . ? H50 C32 H51 109.5 . . ? O2 C33 C20 119.7(4) . . ? O2 C33 C28 119.9(4) . . ? C20 C33 C28 120.4(5) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.987 _refine_diff_density_min -1.674 _refine_diff_density_rms 0.161 #===END data_Complex3 _database_code_depnum_ccdc_archive 'CCDC 793581' _publ_section_abstract ; Please see full paper. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H78 Cl2 Fe2 N2 O4' _chemical_formula_sum 'C62 H78 Cl2 Fe2 N2 O4' _chemical_formula_weight 1097.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.052(3) _cell_length_b 13.686(3) _cell_length_c 18.072(3) _cell_angle_alpha 100.960(2) _cell_angle_beta 101.664(3) _cell_angle_gamma 106.866(2) _cell_volume 2917.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 12746 _cell_measurement_theta_min 2.3254 _cell_measurement_theta_max 30.5381 _exptl_crystal_description Prism _exptl_crystal_colour 'Dark Purple' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 0.635 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9167 _exptl_absorpt_correction_T_min 0.8456 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_decay_% ? _diffrn_reflns_number 27483 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.50 _reflns_number_total 11990 _reflns_number_gt 11300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.0465P)^2^+1.2641P] 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 11990 _refine_ls_number_parameters 650 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.441538(18) 0.111531(16) 0.213096(12) 0.02060(6) Uani 1 1 d . . . Fe2 Fe 0.590396(18) 0.390200(17) 0.279837(12) 0.02162(7) Uani 1 1 d . . . Cl1 Cl 0.48159(4) 0.25071(3) 0.15472(2) 0.02914(10) Uani 1 1 d . . . Cl2 Cl 0.56740(4) 0.24786(3) 0.33562(2) 0.03047(10) Uani 1 1 d . . . O1 O 0.54147(9) 0.04148(9) 0.21899(6) 0.0271(2) Uani 1 1 d . . . O2 O 0.32774(9) 0.07571(9) 0.25798(6) 0.0288(2) Uani 1 1 d . . . O3 O 0.47425(9) 0.43831(9) 0.28147(6) 0.0283(2) Uani 1 1 d . . . O4 O 0.69582(10) 0.44494(9) 0.23176(7) 0.0300(3) Uani 1 1 d . . . N1 N 0.33726(10) -0.00409(10) 0.10325(7) 0.0198(2) Uani 1 1 d . . . N2 N 0.68966(11) 0.50789(10) 0.38954(7) 0.0207(3) Uani 1 1 d . . . C1 C 0.54314(12) -0.05108(12) 0.17876(9) 0.0222(3) Uani 1 1 d . . . C2 C 0.60314(13) -0.10678(13) 0.21698(9) 0.0246(3) Uani 1 1 d . . . C3 C 0.65370(15) -0.07199(14) 0.30648(10) 0.0303(4) Uani 1 1 d . . . C4 C 0.56196(17) -0.06612(16) 0.34702(11) 0.0396(4) Uani 1 1 d . . . H1 H 0.5390 -0.0077 0.3384 0.048 Uiso 1 1 calc R . . H2 H 0.5902 -0.0562 0.4023 0.048 Uiso 1 1 calc R . . H3 H 0.4994 -0.1308 0.3257 0.048 Uiso 1 1 calc R . . C5 C 0.74634(16) 0.03624(16) 0.33246(11) 0.0403(4) Uani 1 1 d . . . H4 H 0.7187 0.0865 0.3124 0.048 Uiso 1 1 calc R . . H5 H 0.8079 0.0306 0.3126 0.048 Uiso 1 1 calc R . . H6 H 0.7706 0.0595 0.3887 0.048 Uiso 1 1 calc R . . C6 C 0.7020(2) -0.15221(19) 0.33475(12) 0.0508(6) Uani 1 1 d . . . H7 H 0.7297 -0.1302 0.3908 0.061 Uiso 1 1 calc R . . H8 H 0.7618 -0.1560 0.3122 0.061 Uiso 1 1 calc R . . H9 H 0.6449 -0.2206 0.3189 0.061 Uiso 1 1 calc R . . C7 C 0.61103(13) -0.19588(13) 0.16951(10) 0.0266(3) Uani 1 1 d . . . H10 H 0.6522 -0.2326 0.1928 0.032 Uiso 1 1 calc R . . C8 C 0.56068(13) -0.23295(13) 0.08909(10) 0.0257(3) Uani 1 1 d . . . C9 C 0.57728(15) -0.32731(14) 0.04084(11) 0.0327(4) Uani 1 1 d . . . H11 H 0.6290 -0.3035 0.0117 0.039 Uiso 1 1 calc R . . H12 H 0.5073 -0.3737 0.0053 0.039 Uiso 1 1 calc R . . H13 H 0.6061 -0.3647 0.0750 0.039 Uiso 1 1 calc R . . C10 C 0.49393(13) -0.18132(12) 0.05500(9) 0.0237(3) Uani 1 1 d . . . H14 H 0.4552 -0.2077 0.0022 0.028 Uiso 1 1 calc R . . C11 C 0.48457(12) -0.09052(12) 0.09927(9) 0.0220(3) Uani 1 1 d . . . C12 C 0.41460(13) -0.03391(12) 0.05994(9) 0.0226(3) Uani 1 1 d . . . H15 H 0.4641 0.0299 0.0531 0.027 Uiso 1 1 calc R . . H16 H 0.3711 -0.0791 0.0082 0.027 Uiso 1 1 calc R . . C13 C 0.26528(13) 0.04348(12) 0.05558(9) 0.0253(3) Uani 1 1 d . . . H17 H 0.2223 0.0690 0.0876 0.030 Uiso 1 1 calc R . . H18 H 0.3140 0.1046 0.0450 0.030 Uiso 1 1 calc R . . C14 C 0.18558(13) -0.02802(12) -0.02155(9) 0.0245(3) Uani 1 1 d . . . C15 C 0.21992(15) -0.03686(14) -0.08979(10) 0.0318(4) Uani 1 1 d . . . H19 H 0.2929 0.0003 -0.0878 0.038 Uiso 1 1 calc R . . C16 C 0.14590(17) -0.10086(16) -0.16076(10) 0.0388(4) Uani 1 1 d . . . H20 H 0.1701 -0.1081 -0.2058 0.047 Uiso 1 1 calc R . . C17 C 0.03679(17) -0.15372(15) -0.16479(11) 0.0401(4) Uani 1 1 d . . . H21 H -0.0125 -0.1965 -0.2125 0.048 Uiso 1 1 calc R . . C18 C 0.00090(15) -0.14311(15) -0.09806(11) 0.0375(4) Uani 1 1 d . . . H22 H -0.0730 -0.1780 -0.1008 0.045 Uiso 1 1 calc R . . C19 C 0.07470(14) -0.08061(14) -0.02673(10) 0.0308(4) Uani 1 1 d . . . H23 H 0.0499 -0.0737 0.0181 0.037 Uiso 1 1 calc R . . C20 C 0.26963(13) -0.09773(12) 0.12465(9) 0.0233(3) Uani 1 1 d . . . H24 H 0.3198 -0.1228 0.1571 0.028 Uiso 1 1 calc R . . H25 H 0.2292 -0.1541 0.0771 0.028 Uiso 1 1 calc R . . C21 C 0.18775(13) -0.07597(12) 0.16773(9) 0.0240(3) Uani 1 1 d . . . C22 C 0.07713(13) -0.14412(13) 0.14238(9) 0.0266(3) Uani 1 1 d . . . H26 H 0.0552 -0.2016 0.0987 0.032 Uiso 1 1 calc R . . C23 C -0.00042(13) -0.12787(13) 0.18091(10) 0.0287(3) Uani 1 1 d . . . C24 C -0.12099(14) -0.19832(15) 0.15094(12) 0.0385(4) Uani 1 1 d . . . H27 H -0.1667 -0.1563 0.1398 0.046 Uiso 1 1 calc R . . H28 H -0.1417 -0.2327 0.1900 0.046 Uiso 1 1 calc R . . H29 H -0.1312 -0.2508 0.1039 0.046 Uiso 1 1 calc R . . C25 C 0.03599(14) -0.04382(14) 0.24789(10) 0.0297(3) Uani 1 1 d . . . H30 H -0.0157 -0.0331 0.2743 0.036 Uiso 1 1 calc R . . C26 C 0.14590(13) 0.02526(13) 0.27764(9) 0.0267(3) Uani 1 1 d . . . C27 C 0.18520(15) 0.11193(14) 0.35508(10) 0.0333(4) Uani 1 1 d . . . C28 C 0.08868(18) 0.11498(19) 0.39089(13) 0.0539(6) Uani 1 1 d . . . H31 H 0.0325 0.1278 0.3546 0.065 Uiso 1 1 calc R . . H32 H 0.1158 0.1707 0.4387 0.065 Uiso 1 1 calc R . . H33 H 0.0573 0.0484 0.4018 0.065 Uiso 1 1 calc R . . C29 C 0.27198(17) 0.08774(16) 0.41383(10) 0.0392(4) Uani 1 1 d . . . H34 H 0.2379 0.0209 0.4235 0.047 Uiso 1 1 calc R . . H35 H 0.2991 0.1426 0.4621 0.047 Uiso 1 1 calc R . . H36 H 0.3329 0.0847 0.3923 0.047 Uiso 1 1 calc R . . C30 C 0.23707(17) 0.22229(15) 0.34356(12) 0.0410(4) Uani 1 1 d . . . H37 H 0.2429 0.2756 0.3888 0.049 Uiso 1 1 calc R . . H38 H 0.1908 0.2299 0.2980 0.049 Uiso 1 1 calc R . . H39 H 0.3098 0.2303 0.3367 0.049 Uiso 1 1 calc R . . C31 C 0.22129(13) 0.00900(12) 0.23449(9) 0.0240(3) Uani 1 1 d . . . C32 C 0.46184(13) 0.52397(12) 0.32409(9) 0.0233(3) Uani 1 1 d . . . C33 C 0.38614(13) 0.56867(13) 0.28912(9) 0.0248(3) Uani 1 1 d . . . C34 C 0.32503(14) 0.52705(14) 0.20125(9) 0.0304(4) Uani 1 1 d . . . C35 C 0.40973(16) 0.53539(16) 0.15292(10) 0.0358(4) Uani 1 1 d . . . H40 H 0.4575 0.6078 0.1652 0.043 Uiso 1 1 calc R . . H41 H 0.3711 0.5114 0.0981 0.043 Uiso 1 1 calc R . . H42 H 0.4536 0.4922 0.1652 0.043 Uiso 1 1 calc R . . C36 C 0.24882(16) 0.41136(17) 0.18152(11) 0.0434(5) Uani 1 1 d . . . H43 H 0.2929 0.3681 0.1931 0.052 Uiso 1 1 calc R . . H44 H 0.2094 0.3878 0.1269 0.052 Uiso 1 1 calc R . . H45 H 0.1965 0.4058 0.2123 0.052 Uiso 1 1 calc R . . C37 C 0.2533(2) 0.5923(2) 0.17631(12) 0.0528(6) Uani 1 1 d . . . H46 H 0.2131 0.5624 0.1220 0.063 Uiso 1 1 calc R . . H47 H 0.3002 0.6640 0.1840 0.063 Uiso 1 1 calc R . . H48 H 0.2016 0.5916 0.2074 0.063 Uiso 1 1 calc R . . C38 C 0.37325(13) 0.65404(14) 0.33790(10) 0.0283(3) Uani 1 1 d . . . H49 H 0.3230 0.6842 0.3166 0.034 Uiso 1 1 calc R . . C39 C 0.43189(13) 0.69623(13) 0.41684(9) 0.0270(3) Uani 1 1 d . . . C40 C 0.41129(15) 0.78734(15) 0.46631(10) 0.0351(4) Uani 1 1 d . . . H50 H 0.4057 0.8381 0.4370 0.042 Uiso 1 1 calc R . . H51 H 0.4719 0.8206 0.5130 0.042 Uiso 1 1 calc R . . H52 H 0.3432 0.7611 0.4802 0.042 Uiso 1 1 calc R . . C41 C 0.50968(13) 0.65337(13) 0.44792(9) 0.0250(3) Uani 1 1 d . . . H53 H 0.5515 0.6823 0.5000 0.030 Uiso 1 1 calc R . . C42 C 0.52610(13) 0.56767(13) 0.40248(9) 0.0239(3) Uani 1 1 d . . . C43 C 0.61097(13) 0.52193(13) 0.43754(9) 0.0248(3) Uani 1 1 d . . . H54 H 0.6540 0.5681 0.4891 0.030 Uiso 1 1 calc R . . H55 H 0.5718 0.4537 0.4443 0.030 Uiso 1 1 calc R . . C44 C 0.77535(13) 0.46784(12) 0.43016(9) 0.0250(3) Uani 1 1 d . . . H56 H 0.8193 0.4543 0.3947 0.030 Uiso 1 1 calc R . . H57 H 0.7361 0.4002 0.4378 0.030 Uiso 1 1 calc R . . C45 C 0.85527(14) 0.53618(13) 0.50828(9) 0.0261(3) Uani 1 1 d . . . C46 C 0.83411(17) 0.51900(18) 0.57785(11) 0.0424(5) Uani 1 1 d . . . H58 H 0.7660 0.4717 0.5768 0.051 Uiso 1 1 calc R . . C47 C 0.9136(2) 0.5717(2) 0.64859(12) 0.0609(7) Uani 1 1 d . . . H59 H 0.8992 0.5582 0.6947 0.073 Uiso 1 1 calc R . . C48 C 1.01401(19) 0.6441(2) 0.65152(12) 0.0550(6) Uani 1 1 d . . . H60 H 1.0667 0.6800 0.6994 0.066 Uiso 1 1 calc R . . C49 C 1.03568(17) 0.66297(15) 0.58336(12) 0.0439(5) Uani 1 1 d . . . H61 H 1.1027 0.7126 0.5850 0.053 Uiso 1 1 calc R . . C50 C 0.95737(15) 0.60782(14) 0.51205(11) 0.0334(4) Uani 1 1 d . . . H62 H 0.9737 0.6191 0.4659 0.040 Uiso 1 1 calc R . . C51 C 0.74054(13) 0.60864(12) 0.36937(9) 0.0240(3) Uani 1 1 d . . . H63 H 0.7782 0.6644 0.4177 0.029 Uiso 1 1 calc R . . H64 H 0.6813 0.6275 0.3406 0.029 Uiso 1 1 calc R . . C52 C 0.82220(13) 0.60520(12) 0.32161(9) 0.0236(3) Uani 1 1 d . . . C53 C 0.92564(13) 0.68559(12) 0.34442(10) 0.0266(3) Uani 1 1 d . . . H65 H 0.9438 0.7395 0.3899 0.032 Uiso 1 1 calc R . . C54 C 1.00178(13) 0.68701(13) 0.30110(10) 0.0284(3) Uani 1 1 d . . . C55 C 1.11754(15) 0.76813(15) 0.33044(12) 0.0380(4) Uani 1 1 d . . . H66 H 1.1156 0.8325 0.3615 0.046 Uiso 1 1 calc R . . H67 H 1.1448 0.7820 0.2866 0.046 Uiso 1 1 calc R . . H68 H 1.1659 0.7415 0.3619 0.046 Uiso 1 1 calc R . . C56 C 0.96943(14) 0.60907(14) 0.23074(10) 0.0294(3) Uani 1 1 d . . . H69 H 1.0194 0.6112 0.2005 0.035 Uiso 1 1 calc R . . C57 C 0.86663(13) 0.52830(13) 0.20327(9) 0.0250(3) Uani 1 1 d . . . C58 C 0.83140(14) 0.44790(14) 0.12305(10) 0.0292(3) Uani 1 1 d . . . C59 C 0.92056(17) 0.46966(19) 0.07877(12) 0.0482(5) Uani 1 1 d . . . H70 H 0.9394 0.5414 0.0750 0.058 Uiso 1 1 calc R . . H71 H 0.8924 0.4221 0.0271 0.058 Uiso 1 1 calc R . . H72 H 0.9857 0.4591 0.1065 0.058 Uiso 1 1 calc R . . C60 C 0.8090(2) 0.33476(15) 0.13178(11) 0.0437(5) Uani 1 1 d . . . H73 H 0.8766 0.3290 0.1604 0.052 Uiso 1 1 calc R . . H74 H 0.7829 0.2856 0.0808 0.052 Uiso 1 1 calc R . . H75 H 0.7536 0.3189 0.1596 0.052 Uiso 1 1 calc R . . C61 C 0.72620(15) 0.45530(15) 0.07216(10) 0.0350(4) Uani 1 1 d . . . H76 H 0.7402 0.5264 0.0674 0.042 Uiso 1 1 calc R . . H77 H 0.6665 0.4367 0.0961 0.042 Uiso 1 1 calc R . . H78 H 0.7060 0.4075 0.0211 0.042 Uiso 1 1 calc R . . C62 C 0.79388(13) 0.52515(12) 0.25206(9) 0.0239(3) 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 0.01893(11) 0.01673(11) 0.02156(12) 0.00299(8) 0.00228(8) 0.00296(8) Fe2 0.02199(12) 0.01731(11) 0.02049(11) 0.00328(8) 0.00263(9) 0.00257(9) Cl1 0.0380(2) 0.01936(18) 0.01931(17) 0.00364(14) 0.00098(15) -0.00034(16) Cl2 0.0387(2) 0.01943(18) 0.02082(18) 0.00465(14) -0.00315(16) -0.00010(16) O1 0.0259(6) 0.0231(6) 0.0264(6) 0.0009(4) -0.0005(5) 0.0086(5) O2 0.0203(5) 0.0294(6) 0.0254(6) -0.0016(5) 0.0040(4) -0.0009(5) O3 0.0246(6) 0.0279(6) 0.0242(6) -0.0004(4) -0.0011(4) 0.0069(5) O4 0.0277(6) 0.0254(6) 0.0260(6) -0.0001(4) 0.0063(5) -0.0018(5) N1 0.0177(6) 0.0186(6) 0.0204(6) 0.0046(5) 0.0023(5) 0.0048(5) N2 0.0207(6) 0.0192(6) 0.0198(6) 0.0052(5) 0.0025(5) 0.0054(5) C1 0.0192(7) 0.0215(7) 0.0254(7) 0.0057(6) 0.0062(6) 0.0066(6) C2 0.0213(7) 0.0267(8) 0.0254(8) 0.0083(6) 0.0058(6) 0.0075(6) C3 0.0331(9) 0.0347(9) 0.0257(8) 0.0114(7) 0.0054(7) 0.0150(7) C4 0.0462(11) 0.0446(11) 0.0305(9) 0.0135(8) 0.0159(8) 0.0133(9) C5 0.0316(9) 0.0500(12) 0.0293(9) 0.0106(8) -0.0027(7) 0.0067(8) C6 0.0716(15) 0.0609(14) 0.0325(10) 0.0183(9) 0.0069(10) 0.0422(12) C7 0.0232(8) 0.0274(8) 0.0323(8) 0.0116(7) 0.0074(6) 0.0108(6) C8 0.0208(7) 0.0238(8) 0.0331(8) 0.0070(6) 0.0101(6) 0.0067(6) C9 0.0297(9) 0.0316(9) 0.0380(9) 0.0047(7) 0.0087(7) 0.0155(7) C10 0.0200(7) 0.0247(8) 0.0239(7) 0.0050(6) 0.0058(6) 0.0048(6) C11 0.0184(7) 0.0225(7) 0.0234(7) 0.0062(6) 0.0058(6) 0.0047(6) C12 0.0241(7) 0.0232(7) 0.0192(7) 0.0043(6) 0.0047(6) 0.0078(6) C13 0.0244(8) 0.0217(7) 0.0250(8) 0.0030(6) -0.0010(6) 0.0082(6) C14 0.0248(8) 0.0217(7) 0.0235(7) 0.0040(6) -0.0014(6) 0.0095(6) C15 0.0312(9) 0.0342(9) 0.0286(8) 0.0122(7) 0.0045(7) 0.0091(7) C16 0.0468(11) 0.0436(11) 0.0240(8) 0.0084(7) 0.0033(8) 0.0172(9) C17 0.0422(11) 0.0356(10) 0.0290(9) 0.0001(7) -0.0102(8) 0.0124(8) C18 0.0239(8) 0.0351(10) 0.0425(10) 0.0069(8) -0.0055(7) 0.0061(7) C19 0.0252(8) 0.0344(9) 0.0308(9) 0.0072(7) 0.0025(7) 0.0116(7) C20 0.0230(7) 0.0181(7) 0.0234(7) 0.0028(6) 0.0036(6) 0.0026(6) C21 0.0201(7) 0.0229(8) 0.0253(7) 0.0047(6) 0.0036(6) 0.0048(6) C22 0.0211(8) 0.0233(8) 0.0283(8) 0.0028(6) 0.0023(6) 0.0028(6) C23 0.0192(8) 0.0279(8) 0.0340(9) 0.0060(7) 0.0038(6) 0.0043(6) C24 0.0203(8) 0.0392(10) 0.0471(11) 0.0048(8) 0.0051(8) 0.0044(7) C25 0.0214(8) 0.0324(9) 0.0349(9) 0.0074(7) 0.0084(7) 0.0090(7) C26 0.0237(8) 0.0268(8) 0.0264(8) 0.0037(6) 0.0042(6) 0.0077(6) C27 0.0285(9) 0.0347(9) 0.0301(9) -0.0021(7) 0.0074(7) 0.0084(7) C28 0.0392(11) 0.0588(14) 0.0496(12) -0.0142(10) 0.0193(10) 0.0094(10) C29 0.0410(10) 0.0408(10) 0.0245(8) 0.0024(7) 0.0034(8) 0.0053(8) C30 0.0399(10) 0.0301(9) 0.0417(10) -0.0030(8) 0.0004(8) 0.0108(8) C31 0.0188(7) 0.0229(7) 0.0243(7) 0.0042(6) 0.0019(6) 0.0024(6) C32 0.0201(7) 0.0244(8) 0.0219(7) 0.0043(6) 0.0044(6) 0.0044(6) C33 0.0177(7) 0.0318(8) 0.0221(7) 0.0072(6) 0.0037(6) 0.0055(6) C34 0.0226(8) 0.0410(10) 0.0231(8) 0.0058(7) 0.0010(6) 0.0097(7) C35 0.0360(10) 0.0455(11) 0.0245(8) 0.0113(7) 0.0084(7) 0.0107(8) C36 0.0266(9) 0.0529(12) 0.0324(9) 0.0023(8) 0.0009(7) -0.0024(8) C37 0.0509(13) 0.0761(16) 0.0307(10) 0.0044(10) -0.0062(9) 0.0385(12) C38 0.0208(7) 0.0368(9) 0.0285(8) 0.0093(7) 0.0063(6) 0.0115(7) C39 0.0225(8) 0.0316(9) 0.0261(8) 0.0062(6) 0.0089(6) 0.0074(7) C40 0.0337(9) 0.0431(10) 0.0303(9) 0.0044(7) 0.0090(7) 0.0187(8) C41 0.0220(7) 0.0297(8) 0.0194(7) 0.0050(6) 0.0040(6) 0.0051(6) C42 0.0200(7) 0.0272(8) 0.0216(7) 0.0066(6) 0.0030(6) 0.0054(6) C43 0.0256(8) 0.0269(8) 0.0190(7) 0.0053(6) 0.0029(6) 0.0076(6) C44 0.0247(8) 0.0219(7) 0.0245(8) 0.0040(6) -0.0005(6) 0.0085(6) C45 0.0260(8) 0.0256(8) 0.0253(8) 0.0038(6) 0.0004(6) 0.0130(7) C46 0.0349(10) 0.0639(13) 0.0303(9) 0.0133(9) 0.0067(8) 0.0209(10) C47 0.0578(15) 0.105(2) 0.0241(10) 0.0076(11) 0.0062(10) 0.0437(15) C48 0.0467(13) 0.0677(15) 0.0337(11) -0.0153(10) -0.0163(9) 0.0321(12) C49 0.0329(10) 0.0314(10) 0.0515(12) -0.0003(8) -0.0133(9) 0.0117(8) C50 0.0288(9) 0.0299(9) 0.0343(9) 0.0085(7) -0.0040(7) 0.0082(7) C51 0.0243(7) 0.0179(7) 0.0253(7) 0.0043(6) 0.0029(6) 0.0044(6) C52 0.0226(7) 0.0210(7) 0.0247(7) 0.0069(6) 0.0025(6) 0.0061(6) C53 0.0245(8) 0.0208(7) 0.0284(8) 0.0056(6) 0.0007(6) 0.0041(6) C54 0.0211(8) 0.0268(8) 0.0345(9) 0.0121(7) 0.0019(7) 0.0057(6) C55 0.0242(9) 0.0364(10) 0.0439(10) 0.0090(8) 0.0030(8) 0.0016(7) C56 0.0210(8) 0.0343(9) 0.0334(9) 0.0116(7) 0.0061(7) 0.0093(7) C57 0.0231(8) 0.0267(8) 0.0248(8) 0.0084(6) 0.0033(6) 0.0093(6) C58 0.0261(8) 0.0343(9) 0.0264(8) 0.0065(7) 0.0061(7) 0.0110(7) C59 0.0351(10) 0.0642(14) 0.0365(10) 0.0003(9) 0.0142(9) 0.0093(10) C60 0.0617(13) 0.0365(10) 0.0349(10) 0.0054(8) 0.0111(9) 0.0237(10) C61 0.0325(9) 0.0403(10) 0.0264(8) 0.0049(7) 0.0011(7) 0.0110(8) C62 0.0211(7) 0.0216(7) 0.0245(7) 0.0062(6) 0.0021(6) 0.0033(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.8222(12) . ? Fe1 O1 1.8276(12) . ? Fe1 N1 2.1818(13) . ? Fe1 Cl1 2.3290(5) . ? Fe1 Cl2 2.5026(5) . ? Fe2 O3 1.8227(12) . ? Fe2 O4 1.8283(12) . ? Fe2 N2 2.1771(13) . ? Fe2 Cl2 2.3306(5) . ? Fe2 Cl1 2.5023(5) . ? O1 C1 1.3438(18) . ? O2 C31 1.3500(18) . ? O3 C32 1.3458(19) . ? O4 C62 1.3489(18) . ? N1 C12 1.4951(19) . ? N1 C20 1.4972(19) . ? N1 C13 1.5132(19) . ? N2 C51 1.4945(19) . ? N2 C43 1.502(2) . ? N2 C44 1.5057(19) . ? C1 C11 1.400(2) . ? C1 C2 1.414(2) . ? C2 C7 1.394(2) . ? C2 C3 1.540(2) . ? C3 C5 1.531(3) . ? C3 C6 1.533(2) . ? C3 C4 1.538(3) . ? C4 H1 0.9600 . ? C4 H2 0.9600 . ? C4 H3 0.9600 . ? C5 H4 0.9600 . ? C5 H5 0.9600 . ? C5 H6 0.9600 . ? C6 H7 0.9600 . ? C6 H8 0.9600 . ? C6 H9 0.9600 . ? C7 C8 1.393(2) . ? C7 H10 0.9300 . ? C8 C10 1.394(2) . ? C8 C9 1.512(2) . ? C9 H11 0.9600 . ? C9 H12 0.9600 . ? C9 H13 0.9600 . ? C10 C11 1.396(2) . ? C10 H14 0.9300 . ? C11 C12 1.516(2) . ? C12 H15 0.9700 . ? C12 H16 0.9700 . ? C13 C14 1.512(2) . ? C13 H17 0.9700 . ? C13 H18 0.9700 . ? C14 C15 1.391(2) . ? C14 C19 1.392(2) . ? C15 C16 1.388(2) . ? C15 H19 0.9300 . ? C16 C17 1.377(3) . ? C16 H20 0.9300 . ? C17 C18 1.377(3) . ? C17 H21 0.9300 . ? C18 C19 1.386(2) . ? C18 H22 0.9300 . ? C19 H23 0.9300 . ? C20 C21 1.507(2) . ? C20 H24 0.9700 . ? C20 H25 0.9700 . ? C21 C22 1.398(2) . ? C21 C31 1.399(2) . ? C22 C23 1.384(2) . ? C22 H26 0.9300 . ? C23 C25 1.391(2) . ? C23 C24 1.509(2) . ? C24 H27 0.9600 . ? C24 H28 0.9600 . ? C24 H29 0.9600 . ? C25 C26 1.396(2) . ? C25 H30 0.9300 . ? C26 C31 1.413(2) . ? C26 C27 1.534(2) . ? C27 C28 1.535(3) . ? C27 C30 1.538(3) . ? C27 C29 1.544(3) . ? C28 H31 0.9600 . ? C28 H32 0.9600 . ? C28 H33 0.9600 . ? C29 H34 0.9600 . ? C29 H35 0.9600 . ? C29 H36 0.9600 . ? C30 H37 0.9600 . ? C30 H38 0.9600 . ? C30 H39 0.9600 . ? C32 C42 1.405(2) . ? C32 C33 1.413(2) . ? C33 C38 1.397(2) . ? C33 C34 1.537(2) . ? C34 C37 1.532(3) . ? C34 C36 1.534(3) . ? C34 C35 1.534(2) . ? C35 H40 0.9600 . ? C35 H41 0.9600 . ? C35 H42 0.9600 . ? C36 H43 0.9600 . ? C36 H44 0.9600 . ? C36 H45 0.9600 . ? C37 H46 0.9600 . ? C37 H47 0.9600 . ? C37 H48 0.9600 . ? C38 C39 1.394(2) . ? C38 H49 0.9300 . ? C39 C41 1.390(2) . ? C39 C40 1.515(2) . ? C40 H50 0.9600 . ? C40 H51 0.9600 . ? C40 H52 0.9600 . ? C41 C42 1.395(2) . ? C41 H53 0.9300 . ? C42 C43 1.513(2) . ? C43 H54 0.9700 . ? C43 H55 0.9700 . ? C44 C45 1.514(2) . ? C44 H56 0.9700 . ? C44 H57 0.9700 . ? C45 C50 1.386(2) . ? C45 C46 1.388(3) . ? C46 C47 1.382(3) . ? C46 H58 0.9300 . ? C47 C48 1.379(4) . ? C47 H59 0.9300 . ? C48 C49 1.372(3) . ? C48 H60 0.9300 . ? C49 C50 1.387(2) . ? C49 H61 0.9300 . ? C50 H62 0.9300 . ? C51 C52 1.506(2) . ? C51 H63 0.9700 . ? C51 H64 0.9700 . ? C52 C53 1.394(2) . ? C52 C62 1.404(2) . ? C53 C54 1.382(2) . ? C53 H65 0.9300 . ? C54 C56 1.392(2) . ? C54 C55 1.508(2) . ? C55 H66 0.9600 . ? C55 H67 0.9600 . ? C55 H68 0.9600 . ? C56 C57 1.389(2) . ? C56 H69 0.9300 . ? C57 C62 1.418(2) . ? C57 C58 1.534(2) . ? C58 C61 1.532(2) . ? C58 C59 1.533(2) . ? C58 C60 1.535(3) . ? C59 H70 0.9600 . ? C59 H71 0.9600 . ? C59 H72 0.9600 . ? C60 H73 0.9600 . ? C60 H74 0.9600 . ? C60 H75 0.9600 . ? C61 H76 0.9600 . ? C61 H77 0.9600 . ? C61 H78 0.9600 . ? 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 O2 Fe1 O1 119.36(6) . . ? O2 Fe1 N1 90.03(5) . . ? O1 Fe1 N1 90.38(5) . . ? O2 Fe1 Cl1 125.52(4) . . ? O1 Fe1 Cl1 114.96(4) . . ? N1 Fe1 Cl1 93.59(4) . . ? O2 Fe1 Cl2 92.60(4) . . ? O1 Fe1 Cl2 88.91(4) . . ? N1 Fe1 Cl2 177.29(4) . . ? Cl1 Fe1 Cl2 84.343(19) . . ? O3 Fe2 O4 121.10(6) . . ? O3 Fe2 N2 90.60(5) . . ? O4 Fe2 N2 89.97(5) . . ? O3 Fe2 Cl2 109.27(4) . . ? O4 Fe2 Cl2 129.39(4) . . ? N2 Fe2 Cl2 94.22(4) . . ? O3 Fe2 Cl1 91.63(4) . . ? O4 Fe2 Cl1 89.53(4) . . ? N2 Fe2 Cl1 177.64(4) . . ? Cl2 Fe2 Cl1 84.32(2) . . ? Fe1 Cl1 Fe2 95.38(2) . . ? Fe2 Cl2 Fe1 95.34(2) . . ? C1 O1 Fe1 134.95(10) . . ? C31 O2 Fe1 136.28(10) . . ? C32 O3 Fe2 134.55(10) . . ? C62 O4 Fe2 136.88(10) . . ? C12 N1 C20 110.37(12) . . ? C12 N1 C13 110.28(12) . . ? C20 N1 C13 112.28(12) . . ? C12 N1 Fe1 106.54(9) . . ? C20 N1 Fe1 106.64(9) . . ? C13 N1 Fe1 110.51(9) . . ? C51 N2 C43 109.95(12) . . ? C51 N2 C44 112.72(12) . . ? C43 N2 C44 111.35(12) . . ? C51 N2 Fe2 107.00(9) . . ? C43 N2 Fe2 106.94(9) . . ? C44 N2 Fe2 108.61(9) . . ? O1 C1 C11 118.82(13) . . ? O1 C1 C2 119.87(14) . . ? C11 C1 C2 121.30(14) . . ? C7 C2 C1 116.35(14) . . ? C7 C2 C3 122.30(14) . . ? C1 C2 C3 121.33(14) . . ? C5 C3 C6 108.39(16) . . ? C5 C3 C4 109.28(15) . . ? C6 C3 C4 107.02(16) . . ? C5 C3 C2 111.29(14) . . ? C6 C3 C2 111.36(15) . . ? C4 C3 C2 109.38(14) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C8 C7 C2 123.66(15) . . ? C8 C7 H10 118.2 . . ? C2 C7 H10 118.2 . . ? C7 C8 C10 118.06(15) . . ? C7 C8 C9 120.61(15) . . ? C10 C8 C9 121.32(15) . . ? C8 C9 H11 109.5 . . ? C8 C9 H12 109.5 . . ? H11 C9 H12 109.5 . . ? C8 C9 H13 109.5 . . ? H11 C9 H13 109.5 . . ? H12 C9 H13 109.5 . . ? C8 C10 C11 120.74(14) . . ? C8 C10 H14 119.6 . . ? C11 C10 H14 119.6 . . ? C10 C11 C1 119.42(14) . . ? C10 C11 C12 119.53(13) . . ? C1 C11 C12 121.01(13) . . ? N1 C12 C11 114.95(12) . . ? N1 C12 H15 108.5 . . ? C11 C12 H15 108.5 . . ? N1 C12 H16 108.5 . . ? C11 C12 H16 108.5 . . ? H15 C12 H16 107.5 . . ? C14 C13 N1 116.95(12) . . ? C14 C13 H17 108.1 . . ? N1 C13 H17 108.1 . . ? C14 C13 H18 108.1 . . ? N1 C13 H18 108.1 . . ? H17 C13 H18 107.3 . . ? C15 C14 C19 118.60(15) . . ? C15 C14 C13 120.49(15) . . ? C19 C14 C13 120.77(15) . . ? C16 C15 C14 120.34(17) . . ? C16 C15 H19 119.8 . . ? C14 C15 H19 119.8 . . ? C17 C16 C15 120.36(18) . . ? C17 C16 H20 119.8 . . ? C15 C16 H20 119.8 . . ? C18 C17 C16 119.85(17) . . ? C18 C17 H21 120.1 . . ? C16 C17 H21 120.1 . . ? C17 C18 C19 120.15(18) . . ? C17 C18 H22 119.9 . . ? C19 C18 H22 119.9 . . ? C18 C19 C14 120.64(17) . . ? C18 C19 H23 119.7 . . ? C14 C19 H23 119.7 . . ? N1 C20 C21 114.40(13) . . ? N1 C20 H24 108.7 . . ? C21 C20 H24 108.7 . . ? N1 C20 H25 108.7 . . ? C21 C20 H25 108.7 . . ? H24 C20 H25 107.6 . . ? C22 C21 C31 119.27(15) . . ? C22 C21 C20 119.49(14) . . ? C31 C21 C20 121.20(14) . . ? C23 C22 C21 121.36(15) . . ? C23 C22 H26 119.3 . . ? C21 C22 H26 119.3 . . ? C22 C23 C25 117.94(15) . . ? C22 C23 C24 121.18(15) . . ? C25 C23 C24 120.88(15) . . ? C23 C24 H27 109.5 . . ? C23 C24 H28 109.5 . . ? H27 C24 H28 109.5 . . ? C23 C24 H29 109.5 . . ? H27 C24 H29 109.5 . . ? H28 C24 H29 109.5 . . ? C23 C25 C26 123.55(15) . . ? C23 C25 H30 118.2 . . ? C26 C25 H30 118.2 . . ? C25 C26 C31 116.71(15) . . ? C25 C26 C27 122.19(15) . . ? C31 C26 C27 121.05(14) . . ? C26 C27 C28 111.64(15) . . ? C26 C27 C30 111.50(15) . . ? C28 C27 C30 107.41(17) . . ? C26 C27 C29 108.49(14) . . ? C28 C27 C29 108.03(17) . . ? C30 C27 C29 109.71(15) . . ? C27 C28 H31 109.5 . . ? C27 C28 H32 109.5 . . ? H31 C28 H32 109.5 . . ? C27 C28 H33 109.5 . . ? H31 C28 H33 109.5 . . ? H32 C28 H33 109.5 . . ? C27 C29 H34 109.5 . . ? C27 C29 H35 109.5 . . ? H34 C29 H35 109.5 . . ? C27 C29 H36 109.5 . . ? H34 C29 H36 109.5 . . ? H35 C29 H36 109.5 . . ? C27 C30 H37 109.5 . . ? C27 C30 H38 109.5 . . ? H37 C30 H38 109.5 . . ? C27 C30 H39 109.5 . . ? H37 C30 H39 109.5 . . ? H38 C30 H39 109.5 . . ? O2 C31 C21 119.07(14) . . ? O2 C31 C26 119.87(14) . . ? C21 C31 C26 121.06(14) . . ? O3 C32 C42 118.82(14) . . ? O3 C32 C33 119.63(14) . . ? C42 C32 C33 121.54(14) . . ? C38 C33 C32 116.51(14) . . ? C38 C33 C34 122.44(14) . . ? C32 C33 C34 121.01(14) . . ? C37 C34 C36 108.06(16) . . ? C37 C34 C35 107.37(16) . . ? C36 C34 C35 109.35(15) . . ? C37 C34 C33 111.25(15) . . ? C36 C34 C33 110.81(14) . . ? C35 C34 C33 109.92(14) . . ? C34 C35 H40 109.5 . . ? C34 C35 H41 109.5 . . ? H40 C35 H41 109.5 . . ? C34 C35 H42 109.5 . . ? H40 C35 H42 109.5 . . ? H41 C35 H42 109.5 . . ? C34 C36 H43 109.5 . . ? C34 C36 H44 109.5 . . ? H43 C36 H44 109.5 . . ? C34 C36 H45 109.5 . . ? H43 C36 H45 109.5 . . ? H44 C36 H45 109.5 . . ? C34 C37 H46 109.5 . . ? C34 C37 H47 109.5 . . ? H46 C37 H47 109.5 . . ? C34 C37 H48 109.5 . . ? H46 C37 H48 109.5 . . ? H47 C37 H48 109.5 . . ? C39 C38 C33 123.34(15) . . ? C39 C38 H49 118.3 . . ? C33 C38 H49 118.3 . . ? C41 C39 C38 118.28(15) . . ? C41 C39 C40 121.57(15) . . ? C38 C39 C40 120.15(15) . . ? C39 C40 H50 109.5 . . ? C39 C40 H51 109.5 . . ? H50 C40 H51 109.5 . . ? C39 C40 H52 109.5 . . ? H50 C40 H52 109.5 . . ? H51 C40 H52 109.5 . . ? C39 C41 C42 121.19(14) . . ? C39 C41 H53 119.4 . . ? C42 C41 H53 119.4 . . ? C41 C42 C32 118.98(14) . . ? C41 C42 C43 120.36(14) . . ? C32 C42 C43 120.66(14) . . ? N2 C43 C42 114.42(12) . . ? N2 C43 H54 108.7 . . ? C42 C43 H54 108.7 . . ? N2 C43 H55 108.7 . . ? C42 C43 H55 108.7 . . ? H54 C43 H55 107.6 . . ? N2 C44 C45 118.71(13) . . ? N2 C44 H56 107.6 . . ? C45 C44 H56 107.6 . . ? N2 C44 H57 107.6 . . ? C45 C44 H57 107.6 . . ? H56 C44 H57 107.1 . . ? C50 C45 C46 118.21(16) . . ? C50 C45 C44 120.81(15) . . ? C46 C45 C44 120.48(16) . . ? C47 C46 C45 120.5(2) . . ? C47 C46 H58 119.8 . . ? C45 C46 H58 119.8 . . ? C48 C47 C46 120.7(2) . . ? C48 C47 H59 119.7 . . ? C46 C47 H59 119.7 . . ? C49 C48 C47 119.60(18) . . ? C49 C48 H60 120.2 . . ? C47 C48 H60 120.2 . . ? C48 C49 C50 119.8(2) . . ? C48 C49 H61 120.1 . . ? C50 C49 H61 120.1 . . ? C45 C50 C49 121.19(18) . . ? C45 C50 H62 119.4 . . ? C49 C50 H62 119.4 . . ? N2 C51 C52 115.18(12) . . ? N2 C51 H63 108.5 . . ? C52 C51 H63 108.5 . . ? N2 C51 H64 108.5 . . ? C52 C51 H64 108.5 . . ? H63 C51 H64 107.5 . . ? C53 C52 C62 119.14(15) . . ? C53 C52 C51 119.70(14) . . ? C62 C52 C51 121.08(14) . . ? C54 C53 C52 121.56(15) . . ? C54 C53 H65 119.2 . . ? C52 C53 H65 119.2 . . ? C53 C54 C56 117.87(15) . . ? C53 C54 C55 121.04(16) . . ? C56 C54 C55 121.05(16) . . ? C54 C55 H66 109.5 . . ? C54 C55 H67 109.5 . . ? H66 C55 H67 109.5 . . ? C54 C55 H68 109.5 . . ? H66 C55 H68 109.5 . . ? H67 C55 H68 109.5 . . ? C57 C56 C54 123.62(16) . . ? C57 C56 H69 118.2 . . ? C54 C56 H69 118.2 . . ? C56 C57 C62 116.80(15) . . ? C56 C57 C58 121.99(15) . . ? C62 C57 C58 121.20(14) . . ? C61 C58 C59 106.98(15) . . ? C61 C58 C57 109.28(14) . . ? C59 C58 C57 112.24(15) . . ? C61 C58 C60 109.71(15) . . ? C59 C58 C60 107.51(16) . . ? C57 C58 C60 111.01(14) . . ? C58 C59 H70 109.5 . . ? C58 C59 H71 109.5 . . ? H70 C59 H71 109.5 . . ? C58 C59 H72 109.5 . . ? H70 C59 H72 109.5 . . ? H71 C59 H72 109.5 . . ? C58 C60 H73 109.5 . . ? C58 C60 H74 109.5 . . ? H73 C60 H74 109.5 . . ? C58 C60 H75 109.5 . . ? H73 C60 H75 109.5 . . ? H74 C60 H75 109.5 . . ? C58 C61 H76 109.5 . . ? C58 C61 H77 109.5 . . ? H76 C61 H77 109.5 . . ? C58 C61 H78 109.5 . . ? H76 C61 H78 109.5 . . ? H77 C61 H78 109.5 . . ? O4 C62 C52 119.10(14) . . ? O4 C62 C57 120.12(14) . . ? C52 C62 C57 120.78(14) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.344 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.049 #===END data_Complex4 _database_code_depnum_ccdc_archive 'CCDC 793582' _publ_section_abstract ; Please see full paper. ; # start Validation Reply Form _vrf_PLAT220_XQ008 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.67 Ratio RESPONSE: This is a partial occupancy, disordered, methyl carbon on a pendant N-propyl group. It was refined anisotropically. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C27 H40 O2 N1) Fe Br2] (C7 H8)0.5' _chemical_formula_sum 'C30.50 H44 Br2 Fe N O2' _chemical_formula_weight 672.34 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' Br Br -0.2901 2.4595 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 11.5336(18) _cell_length_b 16.678(3) _cell_length_c 16.891(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.510(3) _cell_angle_gamma 90.00 _cell_volume 3213.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 128(2) _cell_measurement_reflns_used 11993 _cell_measurement_theta_min 2.3498 _cell_measurement_theta_max 30.8607 _exptl_crystal_description Irregular _exptl_crystal_colour Black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 2.982 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.6202 _exptl_absorpt_correction_T_min 0.4747 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 128(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 40002 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6630 _reflns_number_gt 6091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.0825P)^2^+10.9641P] 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 SHELXL _refine_ls_extinction_coef 0.0029(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6630 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1674 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Br1 Br 0.96970(4) 0.95583(3) 0.78021(3) 0.03772(17) Uani 1 1 d . . . Br2 Br 0.70445(5) 0.84632(3) 0.66105(3) 0.04415(18) Uani 1 1 d . . . Fe1 Fe 0.84796(5) 0.84203(3) 0.77712(4) 0.02741(18) Uani 1 1 d . . . O1 O 0.9340(3) 0.75006(18) 0.7764(2) 0.0327(7) Uani 1 1 d . . . O2 O 0.7739(3) 0.8339(2) 0.8658(2) 0.0348(7) Uani 1 1 d . . . N6 N 0.7405(3) 0.6647(2) 0.8401(2) 0.0300(8) Uani 1 1 d . A . H17 H 0.7859 0.7012 0.8589 0.035 Uiso 1 1 d . . . C1 C 0.9736(4) 0.6758(2) 0.7670(2) 0.0261(8) Uani 1 1 d . . . C2 C 1.0930(4) 0.6601(2) 0.7621(3) 0.0272(8) Uani 1 1 d . . . C3 C 1.1831(4) 0.7278(3) 0.7639(3) 0.0310(9) Uani 1 1 d . . . C4 C 1.1922(4) 0.7733(3) 0.8444(3) 0.0373(10) Uani 1 1 d . . . H1 H 1.1754 0.7364 0.8864 0.045 Uiso 1 1 calc R . . H2 H 1.1354 0.8174 0.8393 0.045 Uiso 1 1 calc R . . H3 H 1.2716 0.7950 0.8585 0.045 Uiso 1 1 calc R . . C5 C 1.1475(4) 0.7851(3) 0.6930(3) 0.0378(10) Uani 1 1 d . . . H4 H 1.0619 0.7855 0.6792 0.045 Uiso 1 1 calc R . . H5 H 1.1826 0.7669 0.6467 0.045 Uiso 1 1 calc R . . H6 H 1.1752 0.8393 0.7079 0.045 Uiso 1 1 calc R . . C6 C 1.3058(4) 0.6955(3) 0.7562(3) 0.0421(11) Uani 1 1 d . . . H7 H 1.3485 0.6843 0.8096 0.051 Uiso 1 1 calc R . . H8 H 1.3487 0.7356 0.7296 0.051 Uiso 1 1 calc R . . H9 H 1.2983 0.6460 0.7245 0.051 Uiso 1 1 calc R . . C7 C 1.1245(4) 0.5800(3) 0.7549(3) 0.0327(9) Uani 1 1 d . . . H10 H 1.2046 0.5683 0.7528 0.039 Uiso 1 1 calc R . . C8 C 1.0459(4) 0.5159(3) 0.7507(3) 0.0342(9) Uani 1 1 d . . . C9 C 1.0856(5) 0.4304(3) 0.7410(4) 0.0494(13) Uani 1 1 d . . . H11 H 1.1672 0.4245 0.7664 0.059 Uiso 1 1 calc R . . H12 H 1.0796 0.4176 0.6839 0.059 Uiso 1 1 calc R . . H13 H 1.0358 0.3938 0.7664 0.059 Uiso 1 1 calc R . . C10 C 0.9294(4) 0.5332(3) 0.7548(3) 0.0331(9) Uani 1 1 d . . . H14 H 0.8740 0.4908 0.7525 0.040 Uiso 1 1 calc R . . C11 C 0.8926(4) 0.6118(3) 0.7624(3) 0.0282(8) Uani 1 1 d . . . C12 C 0.7653(4) 0.6302(3) 0.7618(3) 0.0316(9) Uani 1 1 d . . . H15 H 0.7192 0.5805 0.7502 0.038 Uiso 1 1 calc R . . H16 H 0.7395 0.6689 0.7183 0.038 Uiso 1 1 calc R . . C13 C 0.6219(4) 0.7060(3) 0.8278(3) 0.0352(10) Uani 1 1 d . . . H18 H 0.6126 0.7361 0.7768 0.042 Uiso 1 1 calc R . . H19 H 0.5594 0.6649 0.8238 0.042 Uiso 1 1 calc R . . C14 C 0.6081(4) 0.7622(3) 0.8945(3) 0.0334(9) Uani 1 1 d . . . C15 C 0.5170(4) 0.7518(3) 0.9396(3) 0.0343(9) Uani 1 1 d . . . H20 H 0.4659 0.7072 0.9292 0.041 Uiso 1 1 calc R . . C16 C 0.5002(4) 0.8059(3) 0.9995(3) 0.0340(9) Uani 1 1 d . . . C17 C 0.3995(4) 0.7948(3) 1.0472(3) 0.0393(10) Uani 1 1 d . . . H21 H 0.3819 0.7376 1.0507 0.047 Uiso 1 1 calc R . . H22 H 0.3301 0.8230 1.0204 0.047 Uiso 1 1 calc R . . H23 H 0.4217 0.8166 1.1012 0.047 Uiso 1 1 calc R . . C18 C 0.5788(4) 0.8681(3) 1.0152(3) 0.0340(9) Uani 1 1 d . . . H24 H 0.5684 0.9040 1.0572 0.041 Uiso 1 1 calc R . . C19 C 0.6738(4) 0.8818(3) 0.9730(3) 0.0318(9) Uani 1 1 d . . . C20 C 0.7619(4) 0.9498(3) 0.9965(3) 0.0335(9) Uani 1 1 d . . . C21 C 0.7308(5) 0.9987(3) 1.0682(3) 0.0426(11) Uani 1 1 d . . . H25 H 0.6917 0.9638 1.1027 0.051 Uiso 1 1 calc R . . H26 H 0.6783 1.0429 1.0484 0.051 Uiso 1 1 calc R . . H27 H 0.8027 1.0204 1.0988 0.051 Uiso 1 1 calc R . . C22 C 0.7604(5) 1.0083(3) 0.9267(3) 0.0431(11) Uani 1 1 d . . . H28 H 0.6825 1.0081 0.8943 0.052 Uiso 1 1 calc R . . H29 H 0.8191 0.9920 0.8935 0.052 Uiso 1 1 calc R . . H30 H 0.7785 1.0624 0.9476 0.052 Uiso 1 1 calc R . . C23 C 0.8850(4) 0.9139(3) 1.0209(3) 0.0407(11) Uani 1 1 d . . . H31 H 0.8974 0.9028 1.0785 0.049 Uiso 1 1 calc R . . H32 H 0.9442 0.9520 1.0083 0.049 Uiso 1 1 calc R . . H33 H 0.8916 0.8638 0.9915 0.049 Uiso 1 1 calc R . . C24 C 0.6858(4) 0.8275(3) 0.9106(3) 0.0313(9) Uani 1 1 d . . . C25 C 0.7526(5) 0.6042(3) 0.9078(3) 0.0438(11) Uani 1 1 d . . . C26 C 0.8140(18) 0.6459(10) 0.9871(10) 0.062(4) Uani 0.40 1 d P A 1 C26A C 0.8737(9) 0.5976(8) 0.9551(6) 0.061(3) Uani 0.60 1 d P A 1 C27A C 0.909(3) 0.6752(18) 0.997(2) 0.121(15) Uani 0.60 1 d P B 2 C27 C 0.946(4) 0.669(4) 0.988(3) 0.109(17) Uani 0.40 1 d P C 2 C28 C 0.7800(15) 0.9316(9) 0.4627(9) 0.073(4) Uani 0.50 1 d P . . H34 H 0.7497 0.9208 0.5129 0.088 Uiso 0.50 1 calc PR . . H35 H 0.7825 0.8815 0.4327 0.088 Uiso 0.50 1 calc PR . . H36 H 0.7285 0.9700 0.4307 0.088 Uiso 0.50 1 calc PR . . C29 C 0.8897(9) 0.9627(5) 0.4792(6) 0.082(2) Uani 1 1 d . . . C30 C 0.9616(8) 0.9477(5) 0.5529(5) 0.074(2) Uani 1 1 d . . . H37 H 0.9347 0.9114 0.5895 0.089 Uiso 1 1 calc R . . C31 C 1.0691(9) 0.9837(5) 0.5737(5) 0.082(2) Uani 1 1 d . . . H38 H 1.1151 0.9722 0.6239 0.099 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 Br1 0.0429(3) 0.0260(3) 0.0446(3) -0.00194(17) 0.0074(2) -0.00224(17) Br2 0.0426(3) 0.0466(3) 0.0392(3) -0.0043(2) -0.0074(2) 0.0094(2) Fe1 0.0280(3) 0.0240(3) 0.0302(3) -0.0022(2) 0.0041(2) 0.0030(2) O1 0.0281(14) 0.0250(15) 0.0448(17) -0.0059(13) 0.0050(12) -0.0008(12) O2 0.0302(15) 0.0410(18) 0.0342(16) -0.0061(13) 0.0080(13) -0.0027(13) N6 0.0243(17) 0.0292(18) 0.037(2) -0.0050(15) 0.0059(14) -0.0008(14) C1 0.0276(19) 0.0204(18) 0.030(2) -0.0007(15) 0.0034(15) 0.0005(15) C2 0.0261(19) 0.025(2) 0.029(2) -0.0020(15) 0.0010(15) 0.0012(15) C3 0.0259(19) 0.030(2) 0.037(2) -0.0064(17) 0.0038(16) -0.0010(16) C4 0.031(2) 0.040(2) 0.041(2) -0.012(2) 0.0009(18) -0.0036(18) C5 0.035(2) 0.034(2) 0.045(3) 0.001(2) 0.0060(19) -0.0039(18) C6 0.028(2) 0.044(3) 0.054(3) -0.011(2) 0.006(2) -0.001(2) C7 0.028(2) 0.033(2) 0.038(2) -0.0036(18) 0.0038(17) 0.0055(17) C8 0.038(2) 0.023(2) 0.043(2) -0.0017(18) 0.0085(19) 0.0045(17) C9 0.049(3) 0.026(2) 0.077(4) 0.000(2) 0.020(3) 0.008(2) C10 0.035(2) 0.024(2) 0.040(2) -0.0023(17) 0.0078(19) -0.0024(17) C11 0.0267(19) 0.024(2) 0.034(2) -0.0045(16) 0.0059(16) -0.0010(15) C12 0.027(2) 0.028(2) 0.040(2) -0.0098(18) 0.0060(17) -0.0017(16) C13 0.0236(19) 0.039(2) 0.043(2) -0.011(2) 0.0042(17) 0.0020(17) C14 0.026(2) 0.039(2) 0.035(2) -0.0056(18) 0.0028(17) 0.0033(17) C15 0.028(2) 0.039(2) 0.036(2) -0.0019(18) 0.0028(17) 0.0001(18) C16 0.031(2) 0.039(2) 0.032(2) -0.0004(18) 0.0048(17) 0.0062(18) C17 0.036(2) 0.046(3) 0.037(2) -0.003(2) 0.0100(19) 0.001(2) C18 0.036(2) 0.038(2) 0.029(2) -0.0034(18) 0.0061(17) 0.0038(19) C19 0.034(2) 0.030(2) 0.031(2) -0.0028(17) 0.0016(17) 0.0038(17) C20 0.041(2) 0.029(2) 0.031(2) -0.0039(17) 0.0083(18) -0.0018(18) C21 0.054(3) 0.042(3) 0.034(2) -0.010(2) 0.012(2) -0.008(2) C22 0.059(3) 0.032(2) 0.040(3) -0.001(2) 0.012(2) 0.006(2) C23 0.039(2) 0.040(3) 0.041(3) -0.002(2) 0.001(2) -0.005(2) C24 0.029(2) 0.035(2) 0.030(2) -0.0042(17) 0.0031(16) 0.0036(17) C25 0.047(3) 0.043(3) 0.042(3) 0.009(2) 0.008(2) -0.003(2) C26 0.082(12) 0.057(9) 0.046(8) 0.020(7) 0.005(8) 0.013(9) C26A 0.054(6) 0.080(8) 0.050(5) 0.029(5) 0.007(4) 0.025(5) C27A 0.11(2) 0.077(11) 0.14(2) -0.019(12) -0.11(2) 0.004(13) C27 0.053(17) 0.15(4) 0.11(3) 0.05(2) -0.035(16) -0.013(18) C28 0.097(12) 0.062(8) 0.058(8) -0.013(7) 0.002(7) 0.009(8) C29 0.112(7) 0.056(4) 0.084(6) -0.001(4) 0.037(5) 0.021(4) C30 0.112(7) 0.058(4) 0.059(4) 0.020(3) 0.033(4) 0.021(4) C31 0.118(7) 0.062(4) 0.076(5) 0.014(4) 0.041(5) 0.018(5) _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 Br1 Fe1 2.3569(8) . ? Br2 Fe1 2.3723(8) . ? Fe1 O1 1.828(3) . ? Fe1 O2 1.836(3) . ? O1 C1 1.337(5) . ? O2 C24 1.357(5) . ? N6 C12 1.509(6) . ? N6 C25 1.516(6) . ? N6 C13 1.517(5) . ? N6 H17 0.8348 . ? C1 C11 1.414(6) . ? C1 C2 1.417(6) . ? C2 C7 1.394(6) . ? C2 C3 1.532(6) . ? C3 C6 1.538(6) . ? C3 C5 1.539(7) . ? C3 C4 1.548(6) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.398(7) . ? C7 H10 0.9500 . ? C8 C10 1.386(6) . ? C8 C9 1.513(6) . ? C9 H11 0.9800 . ? C9 H12 0.9800 . ? C9 H13 0.9800 . ? C10 C11 1.389(6) . ? C10 H14 0.9500 . ? C11 C12 1.498(6) . ? C12 H15 0.9900 . ? C12 H16 0.9900 . ? C13 C14 1.493(6) . ? C13 H18 0.9900 . ? C13 H19 0.9900 . ? C14 C15 1.396(6) . ? C14 C24 1.411(7) . ? C15 C16 1.391(6) . ? C15 H20 0.9500 . ? C16 C18 1.376(7) . ? C16 C17 1.520(6) . ? C17 H21 0.9800 . ? C17 H22 0.9800 . ? C17 H23 0.9800 . ? C18 C19 1.412(6) . ? C18 H24 0.9500 . ? C19 C24 1.412(6) . ? C19 C20 1.535(6) . ? C20 C22 1.528(7) . ? C20 C23 1.540(7) . ? C20 C21 1.546(6) . ? C21 H25 0.9800 . ? C21 H26 0.9800 . ? C21 H27 0.9800 . ? C22 H28 0.9800 . ? C22 H29 0.9800 . ? C22 H30 0.9800 . ? C23 H31 0.9800 . ? C23 H32 0.9800 . ? C23 H33 0.9800 . ? C25 C26A 1.507(12) . ? C25 C26 1.58(2) . ? C26 C26A 1.24(2) . ? C28 C29 1.358(18) . ? C28 H34 0.9800 . ? C28 H35 0.9800 . ? C28 H36 0.9800 . ? C29 C31 1.396(11) 3_776 ? C29 C30 1.413(13) . ? C30 C31 1.376(13) . ? C30 H37 0.9500 . ? C31 C29 1.396(11) 3_776 ? C31 H38 0.9500 . ? 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 O2 105.23(15) . . ? O1 Fe1 Br1 110.72(10) . . ? O2 Fe1 Br1 112.88(11) . . ? O1 Fe1 Br2 109.41(10) . . ? O2 Fe1 Br2 108.93(11) . . ? Br1 Fe1 Br2 109.55(3) . . ? C1 O1 Fe1 166.7(3) . . ? C24 O2 Fe1 159.6(3) . . ? C12 N6 C25 113.5(4) . . ? C12 N6 C13 109.7(3) . . ? C25 N6 C13 112.7(4) . . ? C12 N6 H17 115.0 . . ? C25 N6 H17 102.5 . . ? C13 N6 H17 103.0 . . ? O1 C1 C11 118.2(4) . . ? O1 C1 C2 122.0(4) . . ? C11 C1 C2 119.8(4) . . ? C7 C2 C1 116.8(4) . . ? C7 C2 C3 121.6(4) . . ? C1 C2 C3 121.7(4) . . ? C2 C3 C6 111.7(4) . . ? C2 C3 C5 109.9(4) . . ? C6 C3 C5 107.2(4) . . ? C2 C3 C4 109.6(4) . . ? C6 C3 C4 107.6(4) . . ? C5 C3 C4 110.8(4) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C2 C7 C8 124.2(4) . . ? C2 C7 H10 117.9 . . ? C8 C7 H10 117.9 . . ? C10 C8 C7 117.6(4) . . ? C10 C8 C9 120.9(4) . . ? C7 C8 C9 121.5(4) . . ? C8 C9 H11 109.5 . . ? C8 C9 H12 109.5 . . ? H11 C9 H12 109.5 . . ? C8 C9 H13 109.5 . . ? H11 C9 H13 109.5 . . ? H12 C9 H13 109.5 . . ? C8 C10 C11 120.9(4) . . ? C8 C10 H14 119.6 . . ? C11 C10 H14 119.6 . . ? C10 C11 C1 120.7(4) . . ? C10 C11 C12 120.4(4) . . ? C1 C11 C12 118.9(4) . . ? C11 C12 N6 112.7(3) . . ? C11 C12 H15 109.1 . . ? N6 C12 H15 109.1 . . ? C11 C12 H16 109.1 . . ? N6 C12 H16 109.1 . . ? H15 C12 H16 107.8 . . ? C14 C13 N6 112.2(4) . . ? C14 C13 H18 109.2 . . ? N6 C13 H18 109.2 . . ? C14 C13 H19 109.2 . . ? N6 C13 H19 109.2 . . ? H18 C13 H19 107.9 . . ? C15 C14 C24 119.9(4) . . ? C15 C14 C13 120.5(4) . . ? C24 C14 C13 119.6(4) . . ? C16 C15 C14 120.9(4) . . ? C16 C15 H20 119.5 . . ? C14 C15 H20 119.5 . . ? C18 C16 C15 118.0(4) . . ? C18 C16 C17 121.5(4) . . ? C15 C16 C17 120.4(4) . . ? C16 C17 H21 109.5 . . ? C16 C17 H22 109.5 . . ? H21 C17 H22 109.5 . . ? C16 C17 H23 109.5 . . ? H21 C17 H23 109.5 . . ? H22 C17 H23 109.5 . . ? C16 C18 C19 124.3(4) . . ? C16 C18 H24 117.9 . . ? C19 C18 H24 117.9 . . ? C18 C19 C24 116.2(4) . . ? C18 C19 C20 121.6(4) . . ? C24 C19 C20 122.2(4) . . ? C22 C20 C19 109.9(4) . . ? C22 C20 C23 111.1(4) . . ? C19 C20 C23 109.3(4) . . ? C22 C20 C21 106.8(4) . . ? C19 C20 C21 111.8(4) . . ? C23 C20 C21 107.9(4) . . ? C20 C21 H25 109.5 . . ? C20 C21 H26 109.5 . . ? H25 C21 H26 109.5 . . ? C20 C21 H27 109.5 . . ? H25 C21 H27 109.5 . . ? H26 C21 H27 109.5 . . ? C20 C22 H28 109.5 . . ? C20 C22 H29 109.5 . . ? H28 C22 H29 109.5 . . ? C20 C22 H30 109.5 . . ? H28 C22 H30 109.5 . . ? H29 C22 H30 109.5 . . ? C20 C23 H31 109.5 . . ? C20 C23 H32 109.5 . . ? H31 C23 H32 109.5 . . ? C20 C23 H33 109.5 . . ? H31 C23 H33 109.5 . . ? H32 C23 H33 109.5 . . ? O2 C24 C14 117.4(4) . . ? O2 C24 C19 121.9(4) . . ? C14 C24 C19 120.6(4) . . ? C26A C25 N6 115.0(5) . . ? C26A C25 C26 47.1(8) . . ? N6 C25 C26 109.0(7) . . ? C26A C26 C25 63.3(10) . . ? C26 C26A C25 69.6(10) . . ? C29 C28 H34 109.5 . . ? C29 C28 H35 109.5 . . ? H34 C28 H35 109.5 . . ? C29 C28 H36 109.5 . . ? H34 C28 H36 109.5 . . ? H35 C28 H36 109.5 . . ? C28 C29 C31 120.6(11) . 3_776 ? C28 C29 C30 121.4(10) . . ? C31 C29 C30 117.8(9) 3_776 . ? C31 C30 C29 122.5(8) . . ? C31 C30 H37 118.8 . . ? C29 C30 H37 118.8 . . ? C30 C31 C29 119.7(9) . 3_776 ? C30 C31 H38 120.1 . . ? C29 C31 H38 120.1 3_776 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.684 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.114 #===END