# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Ingleson, Michael' 'Zlatogorsky, Sergey' _publ_contact_author_name 'Ingleson, Michael' _publ_contact_author_email michael.ingleson@manchester.ac.uk _publ_section_title ; Synthesis, and solvent dependent reactivity of chelating Bis-N-Heterocyclic Carbene Complexes of Fe(II) hydrides. ; # Attachment '- final.cif' data_c:\workdo~1\crystals\omji68~1\test _database_code_depnum_ccdc_archive 'CCDC 851122' #TrackingRef '- final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H40 Cl Fe I N4' _chemical_formula_sum 'C31 H40 Cl Fe I N4' _chemical_formula_weight 686.87 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' I I -0.4742 1.8119 '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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7706(6) _cell_length_b 16.2518(8) _cell_length_c 15.7973(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.127(5) _cell_angle_gamma 90.00 _cell_volume 3205.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4992 _cell_measurement_theta_min 2.9096 _cell_measurement_theta_max 28.2237 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 1.542 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8016 _exptl_absorpt_correction_T_max 0.8931 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_reflns_number 8836 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.1603 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5494 _reflns_number_gt 2841 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1207P)^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 5494 _refine_ls_number_parameters 352 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1697 _refine_ls_R_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.2342 _refine_ls_wR_factor_gt 0.1985 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.028 _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 Cl1 Cl 0.2260(2) 0.14151(14) 0.03017(14) 0.0095(5) Uani 1 1 d U . . I1 I 0.33024(7) 0.01660(5) 0.26221(6) 0.0372(3) Uani 1 1 d . . . Fe1 Fe 0.24840(14) 0.15004(11) 0.17892(11) 0.0253(5) Uani 1 1 d . . . N1 N 0.4199(8) 0.2982(6) 0.2291(6) 0.028(2) Uani 1 1 d . . . N2 N 0.3323(8) 0.2652(6) 0.3241(6) 0.025(2) Uani 1 1 d . . . N3 N 0.1496(8) 0.2227(6) 0.3163(6) 0.023(2) Uani 1 1 d . . . N4 N 0.0154(8) 0.2042(6) 0.2126(6) 0.024(2) Uani 1 1 d . . . C1 C 0.3444(10) 0.2446(8) 0.2440(8) 0.030(3) Uani 1 1 d . . . C2 C 0.4536(11) 0.3504(8) 0.2986(8) 0.033(3) Uani 1 1 d . . . H2 H 0.5059 0.3927 0.3026 0.040 Uiso 1 1 calc R . . C3 C 0.3989(10) 0.3303(8) 0.3591(9) 0.037(3) Uani 1 1 d . . . H3 H 0.4042 0.3551 0.4143 0.044 Uiso 1 1 calc R . . C4 C 0.1224(9) 0.1919(7) 0.2350(8) 0.025(3) Uani 1 1 d . . . C5 C 0.0621(10) 0.2520(8) 0.3469(8) 0.029(3) Uani 1 1 d . . . H5 H 0.0611 0.2752 0.4019 0.035 Uiso 1 1 calc R . . C6 C -0.0217(10) 0.2396(8) 0.2793(8) 0.031(3) Uani 1 1 d . . . H6 H -0.0943 0.2532 0.2784 0.037 Uiso 1 1 calc R . . C7 C 0.2590(9) 0.2182(8) 0.3667(7) 0.027(3) Uani 1 1 d . . . H7A H 0.2821 0.1600 0.3728 0.033 Uiso 1 1 calc R . . H7B H 0.2618 0.2407 0.4254 0.033 Uiso 1 1 calc R . . C8 C 0.4563(10) 0.3035(7) 0.1493(7) 0.025(3) Uani 1 1 d . . . C9 C 0.5295(10) 0.2447(7) 0.1312(9) 0.031(3) Uani 1 1 d . . . C10 C 0.5639(10) 0.2539(8) 0.0565(8) 0.032(3) Uani 1 1 d . . . H10 H 0.6160 0.2164 0.0444 0.038 Uiso 1 1 calc R . . C11 C 0.5281(10) 0.3136(8) -0.0019(8) 0.033(3) Uani 1 1 d . . . H11 H 0.5502 0.3149 -0.0557 0.039 Uiso 1 1 calc R . . C12 C 0.4564(10) 0.3750(8) 0.0183(8) 0.030(3) Uani 1 1 d . . . H12 H 0.4353 0.4201 -0.0197 0.035 Uiso 1 1 calc R . . C13 C 0.4184(9) 0.3677(7) 0.0937(7) 0.024(3) Uani 1 1 d . . . C14 C 0.5732(11) 0.1777(8) 0.1957(9) 0.036(3) Uani 1 1 d . . . H14 H 0.5274 0.1739 0.2397 0.044 Uiso 1 1 calc R . . C15 C 0.5781(14) 0.0939(9) 0.1543(13) 0.066(5) Uani 1 1 d . . . H15A H 0.5066 0.0786 0.1219 0.100 Uiso 1 1 calc R . . H15B H 0.6030 0.0529 0.1996 0.100 Uiso 1 1 calc R . . H15C H 0.6278 0.0959 0.1148 0.100 Uiso 1 1 calc R . . C16 C 0.6878(12) 0.2002(10) 0.2415(11) 0.068(5) Uani 1 1 d . . . H16A H 0.7314 0.2097 0.1983 0.102 Uiso 1 1 calc R . . H16B H 0.7187 0.1549 0.2797 0.102 Uiso 1 1 calc R . . H16C H 0.6865 0.2502 0.2759 0.102 Uiso 1 1 calc R . . C17 C 0.3338(10) 0.4282(6) 0.1124(8) 0.022(3) Uani 1 1 d . . . H17 H 0.3360 0.4259 0.1760 0.027 Uiso 1 1 calc R . . C18 C 0.3575(10) 0.5162(7) 0.0908(8) 0.032(3) Uani 1 1 d . . . H18A H 0.3563 0.5206 0.0287 0.048 Uiso 1 1 calc R . . H18B H 0.4284 0.5320 0.1239 0.048 Uiso 1 1 calc R . . H18C H 0.3032 0.5528 0.1057 0.048 Uiso 1 1 calc R . . C19 C 0.2243(11) 0.4021(8) 0.0671(10) 0.046(4) Uani 1 1 d . . . H19A H 0.1710 0.4389 0.0833 0.069 Uiso 1 1 calc R . . H19B H 0.2111 0.3456 0.0838 0.069 Uiso 1 1 calc R . . H19C H 0.2189 0.4047 0.0043 0.069 Uiso 1 1 calc R . . C20 C -0.0538(9) 0.1808(7) 0.1332(8) 0.024(3) Uani 1 1 d . . . C21 C -0.0824(10) 0.0975(7) 0.1194(8) 0.026(3) Uani 1 1 d . . . C22 C -0.1529(11) 0.0772(8) 0.0436(9) 0.036(3) Uani 1 1 d . . . H22 H -0.1730 0.0212 0.0332 0.043 Uiso 1 1 calc R . . C23 C -0.1948(10) 0.1347(9) -0.0170(9) 0.039(4) Uani 1 1 d . . . H23 H -0.2417 0.1187 -0.0694 0.047 Uiso 1 1 calc R . . C24 C -0.1669(10) 0.2197(8) -0.0004(9) 0.031(3) Uani 1 1 d . . . H24 H -0.1977 0.2606 -0.0412 0.037 Uiso 1 1 calc R . . C25 C -0.0967(9) 0.2422(7) 0.0732(8) 0.023(3) Uani 1 1 d . . . C26 C -0.0362(11) 0.0295(7) 0.1823(9) 0.036(3) Uani 1 1 d . . . H26 H 0.0135 0.0554 0.2326 0.043 Uiso 1 1 calc R . . C27 C 0.0276(11) -0.0316(8) 0.1415(9) 0.041(4) Uani 1 1 d . . . H27A H -0.0215 -0.0663 0.1005 0.061 Uiso 1 1 calc R . . H27B H 0.0704 -0.0661 0.1867 0.061 Uiso 1 1 calc R . . H27C H 0.0751 -0.0019 0.1108 0.061 Uiso 1 1 calc R . . C28 C -0.1264(13) -0.0135(10) 0.2168(11) 0.062(5) Uani 1 1 d . . . H28A H -0.1749 -0.0412 0.1689 0.093 Uiso 1 1 calc R . . H28B H -0.1664 0.0274 0.2427 0.093 Uiso 1 1 calc R . . H28C H -0.0952 -0.0542 0.2607 0.093 Uiso 1 1 calc R . . C29 C -0.0698(10) 0.3325(7) 0.0898(8) 0.025(3) Uani 1 1 d . . . H29 H -0.0030 0.3368 0.1358 0.030 Uiso 1 1 calc R . . C30 C -0.1614(12) 0.3772(8) 0.1213(9) 0.039(4) Uani 1 1 d . . . H30A H -0.2286 0.3695 0.0789 0.059 Uiso 1 1 calc R . . H30B H -0.1450 0.4361 0.1279 0.059 Uiso 1 1 calc R . . H30C H -0.1687 0.3544 0.1772 0.059 Uiso 1 1 calc R . . C31 C -0.0516(11) 0.3768(8) 0.0075(8) 0.039(3) Uani 1 1 d . . . H31A H 0.0013 0.3463 -0.0169 0.058 Uiso 1 1 calc R . . H31B H -0.0251 0.4326 0.0225 0.058 Uiso 1 1 calc R . . H31C H -0.1193 0.3796 -0.0352 0.058 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 Cl1 0.0180(9) 0.0069(9) 0.0029(8) 0.0009(7) 0.0004(7) -0.0070(8) I1 0.0252(5) 0.0289(5) 0.0579(6) 0.0105(5) 0.0097(4) 0.0056(5) Fe1 0.0175(9) 0.0223(10) 0.0378(10) 0.0038(8) 0.0097(8) -0.0004(8) N1 0.018(5) 0.028(6) 0.038(6) 0.004(5) 0.008(5) -0.010(5) N2 0.020(5) 0.027(6) 0.024(5) 0.008(5) -0.003(4) -0.003(5) N3 0.021(5) 0.021(5) 0.028(6) 0.003(4) 0.008(5) -0.004(5) N4 0.019(5) 0.020(5) 0.034(6) 0.002(5) 0.010(5) 0.005(5) C1 0.029(7) 0.028(7) 0.039(8) 0.006(6) 0.018(6) 0.006(7) C2 0.034(8) 0.031(8) 0.031(7) 0.008(6) -0.002(6) -0.008(7) C3 0.027(7) 0.036(8) 0.042(8) 0.004(7) -0.005(6) -0.009(7) C4 0.017(6) 0.013(6) 0.048(8) 0.007(6) 0.014(6) 0.010(6) C5 0.026(7) 0.028(7) 0.035(7) 0.008(6) 0.013(6) -0.004(6) C6 0.019(7) 0.044(9) 0.032(7) 0.006(6) 0.008(6) 0.010(7) C7 0.018(6) 0.041(8) 0.021(6) 0.011(6) 0.001(5) -0.006(6) C8 0.023(7) 0.022(7) 0.029(7) 0.007(5) 0.004(6) -0.002(6) C9 0.017(6) 0.017(7) 0.053(8) 0.008(6) -0.003(6) 0.002(6) C10 0.024(7) 0.031(8) 0.044(8) 0.009(6) 0.017(6) 0.007(7) C11 0.023(7) 0.037(8) 0.041(8) -0.007(7) 0.013(6) -0.018(7) C12 0.018(6) 0.031(8) 0.039(7) 0.001(6) 0.007(6) -0.015(6) C13 0.014(6) 0.023(7) 0.035(7) -0.003(6) 0.009(5) -0.005(6) C14 0.029(7) 0.026(7) 0.054(9) 0.018(7) 0.011(7) 0.000(7) C15 0.056(11) 0.034(9) 0.122(15) 0.013(10) 0.045(11) 0.007(9) C16 0.037(10) 0.065(12) 0.086(12) 0.052(10) -0.023(9) 0.001(9) C17 0.025(7) 0.008(6) 0.033(7) 0.002(5) 0.003(6) 0.002(6) C18 0.028(7) 0.016(6) 0.050(8) 0.006(6) 0.004(6) 0.008(7) C19 0.033(8) 0.022(8) 0.081(11) -0.009(7) 0.010(8) -0.006(7) C20 0.017(6) 0.017(6) 0.037(7) -0.002(6) 0.006(6) -0.002(6) C21 0.029(7) 0.017(7) 0.035(7) 0.003(6) 0.014(6) -0.001(6) C22 0.040(8) 0.025(7) 0.047(8) 0.006(7) 0.018(7) 0.008(7) C23 0.014(6) 0.053(10) 0.047(8) -0.025(8) -0.001(6) 0.004(7) C24 0.018(7) 0.023(7) 0.050(8) -0.005(6) 0.003(6) 0.003(6) C25 0.019(6) 0.013(6) 0.040(7) 0.001(5) 0.013(6) 0.006(6) C26 0.045(9) 0.015(7) 0.050(8) -0.008(6) 0.017(7) -0.008(7) C27 0.028(7) 0.039(9) 0.053(9) -0.010(7) 0.003(7) -0.004(7) C28 0.050(10) 0.063(11) 0.079(12) 0.027(10) 0.028(9) 0.005(10) C29 0.020(6) 0.012(6) 0.043(7) -0.001(5) 0.004(6) -0.005(6) C30 0.043(9) 0.023(7) 0.052(9) 0.007(6) 0.011(7) 0.019(7) C31 0.024(7) 0.045(9) 0.049(8) 0.013(7) 0.012(7) 0.009(7) _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 Cl1 Fe1 2.311(3) . ? I1 Fe1 2.6360(19) . ? Fe1 C1 2.095(14) . ? Fe1 C4 2.105(11) . ? N1 C1 1.356(15) . ? N1 C2 1.383(15) . ? N1 C8 1.435(14) . ? N2 C1 1.349(15) . ? N2 C3 1.397(16) . ? N2 C7 1.477(14) . ? N3 C4 1.355(15) . ? N3 C5 1.391(15) . ? N3 C7 1.457(14) . ? N4 C4 1.353(14) . ? N4 C6 1.369(15) . ? N4 C20 1.426(15) . ? C2 C3 1.338(17) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C5 C6 1.358(17) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.384(16) . ? C8 C9 1.408(16) . ? C9 C10 1.351(17) . ? C9 C14 1.515(17) . ? C10 C11 1.351(17) . ? C10 H10 0.9500 . ? C11 C12 1.436(17) . ? C11 H11 0.9500 . ? C12 C13 1.383(15) . ? C12 H12 0.9500 . ? C13 C17 1.534(16) . ? C14 C15 1.518(19) . ? C14 C16 1.534(19) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.492(18) . ? C17 C18 1.517(15) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.407(16) . ? C20 C21 1.407(16) . ? C21 C22 1.380(18) . ? C21 C26 1.520(17) . ? C22 C23 1.364(18) . ? C22 H22 0.9500 . ? C23 C24 1.438(18) . ? C23 H23 0.9500 . ? C24 C25 1.361(17) . ? C24 H24 0.9500 . ? C25 C29 1.517(15) . ? C26 C27 1.512(17) . ? C26 C28 1.541(18) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.546(16) . ? C29 C31 1.546(16) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 C1 Fe1 C4 88.7(5) . . ? C1 Fe1 Cl1 118.5(3) . . ? C4 Fe1 Cl1 120.3(4) . . ? C1 Fe1 I1 103.2(4) . . ? C4 Fe1 I1 108.3(3) . . ? Cl1 Fe1 I1 114.17(9) . . ? C1 N1 C2 111.8(10) . . ? C1 N1 C8 124.3(10) . . ? C2 N1 C8 123.8(10) . . ? C1 N2 C3 112.4(10) . . ? C1 N2 C7 120.5(10) . . ? C3 N2 C7 127.1(10) . . ? C4 N3 C5 113.1(10) . . ? C4 N3 C7 121.6(10) . . ? C5 N3 C7 125.2(10) . . ? C4 N4 C6 110.8(10) . . ? C4 N4 C20 126.5(10) . . ? C6 N4 C20 122.5(9) . . ? N2 C1 N1 103.1(11) . . ? N2 C1 Fe1 118.2(8) . . ? N1 C1 Fe1 138.6(9) . . ? C3 C2 N1 107.2(11) . . ? C3 C2 H2 126.4 . . ? N1 C2 H2 126.4 . . ? C2 C3 N2 105.5(12) . . ? C2 C3 H3 127.3 . . ? N2 C3 H3 127.3 . . ? N4 C4 N3 103.6(9) . . ? N4 C4 Fe1 139.2(9) . . ? N3 C4 Fe1 116.9(8) . . ? C6 C5 N3 103.5(11) . . ? C6 C5 H5 128.2 . . ? N3 C5 H5 128.2 . . ? C5 C6 N4 108.9(11) . . ? C5 C6 H6 125.5 . . ? N4 C6 H6 125.5 . . ? N3 C7 N2 110.6(9) . . ? N3 C7 H7A 109.5 . . ? N2 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C13 C8 C9 122.7(11) . . ? C13 C8 N1 117.9(10) . . ? C9 C8 N1 119.3(10) . . ? C10 C9 C8 117.0(11) . . ? C10 C9 C14 121.7(11) . . ? C8 C9 C14 121.2(12) . . ? C9 C10 C11 123.4(12) . . ? C9 C10 H10 118.3 . . ? C11 C10 H10 118.3 . . ? C10 C11 C12 119.1(12) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 119.2(12) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C8 118.2(11) . . ? C12 C13 C17 120.0(11) . . ? C8 C13 C17 121.8(10) . . ? C9 C14 C15 113.5(13) . . ? C9 C14 C16 109.1(11) . . ? C15 C14 C16 107.2(13) . . ? C9 C14 H14 109.0 . . ? C15 C14 H14 109.0 . . ? C16 C14 H14 109.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 111.8(10) . . ? C19 C17 C13 110.7(10) . . ? C18 C17 C13 112.2(10) . . ? C19 C17 H17 107.3 . . ? C18 C17 H17 107.3 . . ? C13 C17 H17 107.3 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 121.8(11) . . ? C25 C20 N4 119.0(10) . . ? C21 C20 N4 119.1(10) . . ? C22 C21 C20 117.8(11) . . ? C22 C21 C26 119.1(11) . . ? C20 C21 C26 123.1(11) . . ? C23 C22 C21 122.3(12) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 C23 C24 119.0(13) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 120.5(12) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C20 118.6(11) . . ? C24 C25 C29 119.5(11) . . ? C20 C25 C29 121.9(11) . . ? C27 C26 C21 111.6(11) . . ? C27 C26 C28 111.3(11) . . ? C21 C26 C28 110.2(12) . . ? C27 C26 H26 107.9 . . ? C21 C26 H26 107.9 . . ? C28 C26 H26 107.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 C30 110.6(10) . . ? C25 C29 C31 111.9(10) . . ? C30 C29 C31 108.0(10) . . ? C25 C29 H29 108.7 . . ? C30 C29 H29 108.7 . . ? C31 C29 H29 108.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N2 C1 N1 -0.2(13) . . . . ? C7 N2 C1 N1 -177.3(10) . . . . ? C3 N2 C1 Fe1 -178.4(8) . . . . ? C7 N2 C1 Fe1 4.4(14) . . . . ? C2 N1 C1 N2 0.2(13) . . . . ? C8 N1 C1 N2 -176.5(10) . . . . ? C2 N1 C1 Fe1 177.9(11) . . . . ? C8 N1 C1 Fe1 1(2) . . . . ? C4 Fe1 C1 N2 36.1(10) . . . . ? Cl1 Fe1 C1 N2 160.3(8) . . . . ? I1 Fe1 C1 N2 -72.4(9) . . . . ? C4 Fe1 C1 N1 -141.4(14) . . . . ? Cl1 Fe1 C1 N1 -17.1(15) . . . . ? I1 Fe1 C1 N1 110.2(13) . . . . ? C1 N1 C2 C3 -0.2(15) . . . . ? C8 N1 C2 C3 176.6(11) . . . . ? N1 C2 C3 N2 0.1(14) . . . . ? C1 N2 C3 C2 0.1(14) . . . . ? C7 N2 C3 C2 177.0(11) . . . . ? C6 N4 C4 N3 -1.5(13) . . . . ? C20 N4 C4 N3 -178.3(10) . . . . ? C6 N4 C4 Fe1 -175.6(10) . . . . ? C20 N4 C4 Fe1 8(2) . . . . ? C5 N3 C4 N4 1.8(13) . . . . ? C7 N3 C4 N4 177.1(10) . . . . ? C5 N3 C4 Fe1 177.5(7) . . . . ? C7 N3 C4 Fe1 -7.2(14) . . . . ? C1 Fe1 C4 N4 138.9(13) . . . . ? Cl1 Fe1 C4 N4 16.2(14) . . . . ? I1 Fe1 C4 N4 -117.7(12) . . . . ? C1 Fe1 C4 N3 -34.7(9) . . . . ? Cl1 Fe1 C4 N3 -157.4(7) . . . . ? I1 Fe1 C4 N3 68.8(9) . . . . ? C4 N3 C5 C6 -1.3(13) . . . . ? C7 N3 C5 C6 -176.4(11) . . . . ? N3 C5 C6 N4 0.3(14) . . . . ? C4 N4 C6 C5 0.8(14) . . . . ? C20 N4 C6 C5 177.7(10) . . . . ? C4 N3 C7 N2 62.8(14) . . . . ? C5 N3 C7 N2 -122.5(11) . . . . ? C1 N2 C7 N3 -60.9(15) . . . . ? C3 N2 C7 N3 122.4(12) . . . . ? C1 N1 C8 C13 103.0(14) . . . . ? C2 N1 C8 C13 -73.3(15) . . . . ? C1 N1 C8 C9 -77.9(15) . . . . ? C2 N1 C8 C9 105.7(14) . . . . ? C13 C8 C9 C10 1.0(18) . . . . ? N1 C8 C9 C10 -178.0(11) . . . . ? C13 C8 C9 C14 177.0(12) . . . . ? N1 C8 C9 C14 -2.0(17) . . . . ? C8 C9 C10 C11 -3.0(19) . . . . ? C14 C9 C10 C11 -178.9(12) . . . . ? C9 C10 C11 C12 5.2(19) . . . . ? C10 C11 C12 C13 -5.4(17) . . . . ? C11 C12 C13 C8 3.6(17) . . . . ? C11 C12 C13 C17 -174.4(10) . . . . ? C9 C8 C13 C12 -1.5(18) . . . . ? N1 C8 C13 C12 177.5(10) . . . . ? C9 C8 C13 C17 176.4(11) . . . . ? N1 C8 C13 C17 -4.5(17) . . . . ? C10 C9 C14 C15 -46.7(17) . . . . ? C8 C9 C14 C15 137.6(13) . . . . ? C10 C9 C14 C16 72.8(17) . . . . ? C8 C9 C14 C16 -103.0(15) . . . . ? C12 C13 C17 C19 82.7(14) . . . . ? C8 C13 C17 C19 -95.2(14) . . . . ? C12 C13 C17 C18 -42.9(15) . . . . ? C8 C13 C17 C18 139.2(12) . . . . ? C4 N4 C20 C25 -108.4(13) . . . . ? C6 N4 C20 C25 75.2(14) . . . . ? C4 N4 C20 C21 75.4(15) . . . . ? C6 N4 C20 C21 -101.0(14) . . . . ? C25 C20 C21 C22 1.3(17) . . . . ? N4 C20 C21 C22 177.4(10) . . . . ? C25 C20 C21 C26 179.0(11) . . . . ? N4 C20 C21 C26 -4.9(17) . . . . ? C20 C21 C22 C23 0.0(18) . . . . ? C26 C21 C22 C23 -177.9(11) . . . . ? C21 C22 C23 C24 -1.7(19) . . . . ? C22 C23 C24 C25 2.4(18) . . . . ? C23 C24 C25 C20 -1.2(17) . . . . ? C23 C24 C25 C29 -179.1(11) . . . . ? C21 C20 C25 C24 -0.6(17) . . . . ? N4 C20 C25 C24 -176.7(10) . . . . ? C21 C20 C25 C29 177.2(11) . . . . ? N4 C20 C25 C29 1.1(16) . . . . ? C22 C21 C26 C27 60.9(15) . . . . ? C20 C21 C26 C27 -116.8(13) . . . . ? C22 C21 C26 C28 -63.2(15) . . . . ? C20 C21 C26 C28 119.1(13) . . . . ? C24 C25 C29 C30 77.3(14) . . . . ? C20 C25 C29 C30 -100.5(13) . . . . ? C24 C25 C29 C31 -43.2(15) . . . . ? C20 C25 C29 C31 139.0(11) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 3.362 _refine_diff_density_min -1.196 _refine_diff_density_rms 0.178 #===END data_c:\workdo~1\crystals\omji74~1\omji74\omji74 _database_code_depnum_ccdc_archive 'CCDC 851123' #TrackingRef '- final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H46 B2 N4' _chemical_formula_sum 'C31 H46 B2 N4' _chemical_formula_weight 496.34 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.641(6) _cell_length_b 13.9423(16) _cell_length_c 16.592(5) _cell_angle_alpha 90.00 _cell_angle_beta 135.80(6) _cell_angle_gamma 90.00 _cell_volume 3168(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1762 _cell_measurement_theta_min 2.9692 _cell_measurement_theta_max 27.6109 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9705 _exptl_absorpt_correction_T_max 0.9970 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_reflns_number 8551 _diffrn_reflns_av_R_equivalents 0.1010 _diffrn_reflns_av_sigmaI/netI 0.1375 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2803 _reflns_number_gt 1198 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2803 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1627 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1810 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _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 B1 B 0.6637(3) 0.3565(3) 0.2606(4) 0.0474(11) Uani 1 1 d . . . H1 H 0.6934(19) 0.3568(19) 0.346(3) 0.041(8) Uiso 1 1 d . . . H4 H 0.706(2) 0.323(2) 0.256(3) 0.058(10) Uiso 1 1 d . . . H5 H 0.644(2) 0.435(3) 0.238(3) 0.067(10) Uiso 1 1 d . . . N1 N 0.48794(17) 0.32370(17) 0.16934(19) 0.0377(7) Uani 1 1 d . . . N2 N 0.52174(17) 0.24048(17) 0.09397(19) 0.0352(7) Uani 1 1 d . . . C1 C 0.5602(2) 0.3058(2) 0.1773(2) 0.0362(8) Uani 1 1 d . . . C2 C 0.4057(2) 0.2689(2) 0.0831(2) 0.0443(9) Uani 1 1 d . . . H2 H 0.3463 0.2679 0.0622 0.053 Uiso 1 1 calc R . . C3 C 0.4271(2) 0.2176(2) 0.0352(3) 0.0443(9) Uani 1 1 d . . . H3 H 0.3852 0.1738 -0.0274 0.053 Uiso 1 1 calc R . . C4 C 0.5000 0.3830(3) 0.2500 0.0421(12) Uani 1 2 d S . . H4A H 0.4420 0.4247 0.2076 0.050 Uiso 0.50 1 calc PR . . H4B H 0.5580 0.4247 0.2924 0.050 Uiso 0.50 1 calc PR . . C5 C 0.5712(2) 0.1967(2) 0.0681(2) 0.0413(8) Uani 1 1 d . . . C6 C 0.5670(2) 0.2423(2) -0.0096(3) 0.0511(9) Uani 1 1 d . . . C7 C 0.6140(3) 0.1970(3) -0.0337(3) 0.0683(12) Uani 1 1 d . . . H7 H 0.6131 0.2258 -0.0863 0.082 Uiso 1 1 calc R . . C8 C 0.6619(3) 0.1109(3) 0.0180(4) 0.0785(13) Uani 1 1 d . . . H8 H 0.6936 0.0807 0.0007 0.094 Uiso 1 1 calc R . . C9 C 0.6639(3) 0.0681(3) 0.0954(3) 0.0702(13) Uani 1 1 d . . . H9 H 0.6971 0.0088 0.1301 0.084 Uiso 1 1 calc R . . C10 C 0.6188(2) 0.1094(2) 0.1233(3) 0.0511(10) Uani 1 1 d . . . C11 C 0.5129(3) 0.3362(3) -0.0674(3) 0.0598(11) Uani 1 1 d . . . H11 H 0.4938 0.3604 -0.0291 0.072 Uiso 1 1 calc R . . C12 C 0.5759(4) 0.4109(3) -0.0522(4) 0.1126(19) Uani 1 1 d . . . H12A H 0.6345 0.4207 0.0304 0.169 Uiso 1 1 calc R . . H12B H 0.5395 0.4713 -0.0870 0.169 Uiso 1 1 calc R . . H12C H 0.5950 0.3898 -0.0901 0.169 Uiso 1 1 calc R . . C13 C 0.4199(3) 0.3212(3) -0.1942(3) 0.0781(13) Uani 1 1 d . . . H13A H 0.4359 0.2926 -0.2330 0.117 Uiso 1 1 calc R . . H13B H 0.3875 0.3831 -0.2301 0.117 Uiso 1 1 calc R . . H13C H 0.3762 0.2783 -0.2016 0.117 Uiso 1 1 calc R . . C14 C 0.6257(3) 0.0657(2) 0.2117(3) 0.0629(11) Uani 1 1 d . . . H14 H 0.5718 0.0929 0.1996 0.075 Uiso 1 1 calc R . . C15 C 0.6155(3) -0.0439(3) 0.2035(3) 0.0821(14) Uani 1 1 d . . . H15A H 0.5527 -0.0619 0.1263 0.123 Uiso 1 1 calc R . . H15B H 0.6185 -0.0673 0.2617 0.123 Uiso 1 1 calc R . . H15C H 0.6688 -0.0724 0.2174 0.123 Uiso 1 1 calc R . . C16 C 0.7228(3) 0.0941(3) 0.3329(3) 0.1083(19) Uani 1 1 d . . . H16A H 0.7769 0.0729 0.3444 0.162 Uiso 1 1 calc R . . H16B H 0.7284 0.0637 0.3907 0.162 Uiso 1 1 calc R . . H16C H 0.7254 0.1640 0.3413 0.162 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 B1 0.036(2) 0.042(3) 0.050(3) -0.010(2) 0.026(2) -0.006(2) N1 0.0308(15) 0.0379(16) 0.0258(13) -0.0008(12) 0.0140(12) -0.0019(13) N2 0.0296(14) 0.0297(15) 0.0255(13) 0.0012(12) 0.0127(12) 0.0004(13) C1 0.0334(17) 0.0286(18) 0.0278(16) 0.0037(14) 0.0156(14) 0.0024(15) C2 0.0265(17) 0.048(2) 0.0294(17) 0.0009(16) 0.0101(15) -0.0087(16) C3 0.0339(19) 0.039(2) 0.0303(18) -0.0032(15) 0.0129(16) -0.0072(16) C4 0.036(3) 0.037(3) 0.034(3) 0.000 0.018(2) 0.000 C5 0.0371(18) 0.036(2) 0.0284(17) -0.0036(15) 0.0161(15) 0.0020(16) C6 0.051(2) 0.049(2) 0.043(2) -0.0040(18) 0.0298(19) 0.0020(19) C7 0.072(3) 0.080(3) 0.052(2) -0.008(2) 0.044(2) 0.000(3) C8 0.061(3) 0.092(4) 0.060(3) -0.010(3) 0.036(2) 0.019(3) C9 0.051(2) 0.062(3) 0.045(2) -0.007(2) 0.016(2) 0.019(2) C10 0.042(2) 0.042(2) 0.0306(19) -0.0077(16) 0.0131(17) 0.0055(18) C11 0.082(3) 0.047(2) 0.054(2) 0.0030(18) 0.050(2) -0.001(2) C12 0.122(4) 0.069(3) 0.086(3) 0.007(3) 0.054(3) -0.028(3) C13 0.074(3) 0.069(3) 0.062(3) 0.012(2) 0.039(2) 0.019(2) C14 0.065(3) 0.035(2) 0.038(2) 0.0032(17) 0.020(2) 0.0086(19) C15 0.071(3) 0.045(2) 0.062(3) -0.014(2) 0.025(2) -0.007(2) C16 0.116(4) 0.063(3) 0.037(2) 0.000(2) 0.018(2) -0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 C1 1.584(5) . ? B1 H1 1.08(3) . ? B1 H4 1.01(3) . ? B1 H5 1.13(3) . ? N1 C1 1.351(4) . ? N1 C2 1.388(4) . ? N1 C4 1.441(3) . ? N2 C1 1.347(4) . ? N2 C3 1.381(4) . ? N2 C5 1.447(4) . ? C2 C3 1.341(4) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 N1 1.441(3) 2_655 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.386(4) . ? C5 C10 1.403(4) . ? C6 C7 1.394(5) . ? C6 C11 1.518(5) . ? C7 C8 1.380(6) . ? C7 H7 0.9500 . ? C8 C9 1.391(5) . ? C8 H8 0.9500 . ? C9 C10 1.386(5) . ? C9 H9 0.9500 . ? C10 C14 1.500(5) . ? C11 C12 1.494(5) . ? C11 C13 1.516(5) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.530(5) . ? C14 C15 1.534(5) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 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 C1 B1 H1 107.2(14) . . ? C1 B1 H4 110.2(18) . . ? H1 B1 H4 114(2) . . ? C1 B1 H5 103.0(16) . . ? H1 B1 H5 100(2) . . ? H4 B1 H5 121(2) . . ? C1 N1 C2 111.3(3) . . ? C1 N1 C4 123.6(2) . . ? C2 N1 C4 124.7(3) . . ? C1 N2 C3 111.2(3) . . ? C1 N2 C5 126.0(3) . . ? C3 N2 C5 122.8(2) . . ? N2 C1 N1 104.3(3) . . ? N2 C1 B1 128.4(3) . . ? N1 C1 B1 127.1(3) . . ? C3 C2 N1 106.1(3) . . ? C3 C2 H2 127.0 . . ? N1 C2 H2 127.0 . . ? C2 C3 N2 107.0(3) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? N1 C4 N1 110.0(3) . 2_655 ? N1 C4 H4A 109.7 . . ? N1 C4 H4A 109.7 2_655 . ? N1 C4 H4B 109.7 . . ? N1 C4 H4B 109.7 2_655 . ? H4A C4 H4B 108.2 . . ? C6 C5 C10 124.9(3) . . ? C6 C5 N2 118.5(3) . . ? C10 C5 N2 116.6(3) . . ? C5 C6 C7 116.8(3) . . ? C5 C6 C11 122.1(3) . . ? C7 C6 C11 121.1(4) . . ? C8 C7 C6 120.8(4) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 120.1(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 122.0(4) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C5 115.4(3) . . ? C9 C10 C14 121.8(3) . . ? C5 C10 C14 122.8(3) . . ? C12 C11 C13 111.0(3) . . ? C12 C11 C6 112.1(3) . . ? C13 C11 C6 111.1(3) . . ? C12 C11 H11 107.5 . . ? C13 C11 H11 107.5 . . ? C6 C11 H11 107.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 C16 109.5(3) . . ? C10 C14 C15 113.8(3) . . ? C16 C14 C15 109.6(3) . . ? C10 C14 H14 107.9 . . ? C16 C14 H14 107.9 . . ? C15 C14 H14 107.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N2 C1 N1 -0.2(3) . . . . ? C5 N2 C1 N1 -179.0(2) . . . . ? C3 N2 C1 B1 -176.3(3) . . . . ? C5 N2 C1 B1 4.9(5) . . . . ? C2 N1 C1 N2 1.0(3) . . . . ? C4 N1 C1 N2 173.7(3) . . . . ? C2 N1 C1 B1 177.1(3) . . . . ? C4 N1 C1 B1 -10.1(5) . . . . ? C1 N1 C2 C3 -1.3(3) . . . . ? C4 N1 C2 C3 -174.0(3) . . . . ? N1 C2 C3 N2 1.1(3) . . . . ? C1 N2 C3 C2 -0.6(3) . . . . ? C5 N2 C3 C2 178.3(3) . . . . ? C1 N1 C4 N1 -101.2(3) . . . 2_655 ? C2 N1 C4 N1 70.6(3) . . . 2_655 ? C1 N2 C5 C6 -88.4(4) . . . . ? C3 N2 C5 C6 92.9(4) . . . . ? C1 N2 C5 C10 92.6(4) . . . . ? C3 N2 C5 C10 -86.0(3) . . . . ? C10 C5 C6 C7 0.0(5) . . . . ? N2 C5 C6 C7 -178.9(3) . . . . ? C10 C5 C6 C11 179.2(3) . . . . ? N2 C5 C6 C11 0.3(4) . . . . ? C5 C6 C7 C8 0.1(5) . . . . ? C11 C6 C7 C8 -179.1(3) . . . . ? C6 C7 C8 C9 -0.1(6) . . . . ? C7 C8 C9 C10 0.0(6) . . . . ? C8 C9 C10 C5 0.1(5) . . . . ? C8 C9 C10 C14 -176.6(3) . . . . ? C6 C5 C10 C9 -0.1(5) . . . . ? N2 C5 C10 C9 178.8(3) . . . . ? C6 C5 C10 C14 176.6(3) . . . . ? N2 C5 C10 C14 -4.5(4) . . . . ? C5 C6 C11 C12 127.1(4) . . . . ? C7 C6 C11 C12 -53.7(5) . . . . ? C5 C6 C11 C13 -108.1(4) . . . . ? C7 C6 C11 C13 71.0(4) . . . . ? C9 C10 C14 C16 81.3(4) . . . . ? C5 C10 C14 C16 -95.2(4) . . . . ? C9 C10 C14 C15 -41.7(5) . . . . ? C5 C10 C14 C15 141.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.305 _refine_diff_density_min -0.161 _refine_diff_density_rms 0.045 #===END data_c:\workdo~1\crystals\omji77~1\bet3ad~1\omji77 _database_code_depnum_ccdc_archive 'CCDC 851124' #TrackingRef '- final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H70 B2 N4' _chemical_formula_sum 'C43 H70 B2 N4' _chemical_formula_weight 664.65 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' B B 0.0013 0.0007 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8268(6) _cell_length_b 9.5632(5) _cell_length_c 31.8206(17) _cell_angle_alpha 90.00 _cell_angle_beta 98.163(5) _cell_angle_gamma 90.00 _cell_volume 4165.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5898 _cell_measurement_theta_min 3.0684 _cell_measurement_theta_max 28.3544 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9532 _exptl_absorpt_correction_T_max 0.9910 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_reflns_number 23155 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7325 _reflns_number_gt 4159 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1415P)^2^+2.4643P] 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 7325 _refine_ls_number_parameters 456 _refine_ls_number_restraints 256 _refine_ls_R_factor_all 0.1475 _refine_ls_R_factor_gt 0.0939 _refine_ls_wR_factor_ref 0.2728 _refine_ls_wR_factor_gt 0.2496 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.068 _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 N1 N 0.4133(2) -0.0013(4) 0.12193(11) 0.0401(9) Uani 1 1 d . . . N2 N 0.3114(2) 0.1606(4) 0.10039(9) 0.0311(8) Uani 1 1 d . . . N3 N 0.5700(2) -0.1081(4) 0.12880(11) 0.0373(8) Uani 1 1 d . . . N4 N 0.7238(2) -0.1057(3) 0.14711(9) 0.0289(7) Uani 1 1 d . . . B1 B 0.2801(3) -0.0875(5) 0.05674(18) 0.0455(13) Uani 1 1 d . . . B2 B 0.6234(3) -0.2752(5) 0.19553(16) 0.0413(12) Uani 1 1 d . . . C1 C 0.3332(2) 0.0251(4) 0.09203(12) 0.0334(9) Uani 1 1 d . . . C2 C 0.4386(3) 0.1137(5) 0.14722(13) 0.0510(12) Uani 1 1 d U . . H2 H 0.4915 0.1195 0.1698 0.061 Uiso 1 1 calc R . . C3 C 0.3756(3) 0.2146(5) 0.13432(13) 0.0466(11) Uani 1 1 d U . . H3 H 0.3744 0.3061 0.1459 0.056 Uiso 1 1 calc R . . C4 C 0.4657(3) -0.1340(5) 0.12729(18) 0.0570(14) Uani 1 1 d . . . H4A H 0.4531 -0.1796 0.1539 0.068 Uiso 1 1 calc R . . H4B H 0.4425 -0.1971 0.1033 0.068 Uiso 1 1 calc R . . C5 C 0.3638(4) -0.1105(7) 0.0194(2) 0.107(2) Uani 1 1 d U . . H5A H 0.3700 -0.0197 0.0051 0.128 Uiso 1 1 calc R . . H5B H 0.4285 -0.1326 0.0356 0.128 Uiso 1 1 calc R . . C6 C 0.3420(5) -0.2150(8) -0.0129(2) 0.107(2) Uani 1 1 d U . . H6A H 0.3287 -0.3042 0.0003 0.161 Uiso 1 1 calc R . . H6B H 0.3980 -0.2257 -0.0284 0.161 Uiso 1 1 calc R . . H6C H 0.2845 -0.1864 -0.0326 0.161 Uiso 1 1 calc R . . C7 C 0.2575(4) -0.2308(6) 0.0804(2) 0.0756(16) Uani 1 1 d U . . H7A H 0.2150 -0.2903 0.0600 0.091 Uiso 1 1 calc R . . H7B H 0.3198 -0.2816 0.0885 0.091 Uiso 1 1 calc R . . C8 C 0.2098(4) -0.2117(6) 0.1188(2) 0.0870(18) Uani 1 1 d U . . H8A H 0.2529 -0.1577 0.1399 0.131 Uiso 1 1 calc R . . H8B H 0.1969 -0.3033 0.1306 0.131 Uiso 1 1 calc R . . H8C H 0.1480 -0.1614 0.1112 0.131 Uiso 1 1 calc R . . C9 C 0.1790(3) -0.0237(4) 0.03134(13) 0.0396(10) Uani 1 1 d U . . H9A H 0.1396 0.0133 0.0525 0.048 Uiso 1 1 calc R . . H9B H 0.1958 0.0564 0.0141 0.048 Uiso 1 1 calc R . . C10 C 0.1151(3) -0.1237(5) 0.00226(16) 0.0632(14) Uani 1 1 d U . . H10A H 0.1528 -0.1618 -0.0190 0.095 Uiso 1 1 calc R . . H10B H 0.0580 -0.0733 -0.0121 0.095 Uiso 1 1 calc R . . H10C H 0.0934 -0.2003 0.0191 0.095 Uiso 1 1 calc R . . C11 C 0.2407(3) 0.2533(4) 0.07688(12) 0.0293(8) Uani 1 1 d U . . C12 C 0.2703(3) 0.3292(4) 0.04321(12) 0.0300(8) Uani 1 1 d U . . C13 C 0.2052(3) 0.4268(4) 0.02360(13) 0.0371(9) Uani 1 1 d U . . H13 H 0.2228 0.4808 0.0008 0.045 Uiso 1 1 calc R . . C14 C 0.1153(3) 0.4472(4) 0.03653(14) 0.0406(9) Uani 1 1 d U . . H14 H 0.0720 0.5156 0.0228 0.049 Uiso 1 1 calc R . . C15 C 0.0879(3) 0.3694(4) 0.06906(13) 0.0380(9) Uani 1 1 d U . . H15 H 0.0250 0.3834 0.0770 0.046 Uiso 1 1 calc R . . C16 C 0.1495(3) 0.2709(4) 0.09062(12) 0.0309(8) Uani 1 1 d U . . C17 C 0.3695(3) 0.3122(4) 0.02974(12) 0.0352(9) Uani 1 1 d U . . H17 H 0.3984 0.2231 0.0423 0.042 Uiso 1 1 calc R . . C18 C 0.3650(3) 0.3031(5) -0.01833(13) 0.0403(10) Uani 1 1 d U . . H18A H 0.3209 0.2272 -0.0293 0.060 Uiso 1 1 calc R . . H18B H 0.4305 0.2845 -0.0254 0.060 Uiso 1 1 calc R . . H18C H 0.3407 0.3917 -0.0312 0.060 Uiso 1 1 calc R . . C19 C 0.4369(3) 0.4334(6) 0.04738(16) 0.0596(13) Uani 1 1 d U . . H19A H 0.4096 0.5222 0.0358 0.089 Uiso 1 1 calc R . . H19B H 0.5019 0.4198 0.0391 0.089 Uiso 1 1 calc R . . H19C H 0.4422 0.4351 0.0784 0.089 Uiso 1 1 calc R . . C20 C 0.1189(3) 0.1914(5) 0.12758(12) 0.0379(9) Uani 1 1 d U . . H20 H 0.1636 0.1094 0.1335 0.045 Uiso 1 1 calc R . . C21 C 0.1294(3) 0.2833(6) 0.16767(14) 0.0577(13) Uani 1 1 d U . . H21A H 0.1975 0.3135 0.1747 0.087 Uiso 1 1 calc R . . H21B H 0.1103 0.2293 0.1914 0.087 Uiso 1 1 calc R . . H21C H 0.0871 0.3654 0.1624 0.087 Uiso 1 1 calc R . . C22 C 0.0141(3) 0.1358(5) 0.11798(14) 0.0511(11) Uani 1 1 d U . . H22A H -0.0318 0.2145 0.1149 0.077 Uiso 1 1 calc R . . H22B H 0.0003 0.0756 0.1413 0.077 Uiso 1 1 calc R . . H22C H 0.0068 0.0817 0.0915 0.077 Uiso 1 1 calc R . . C23 C 0.6408(3) -0.1616(4) 0.15825(12) 0.0311(9) Uani 1 1 d . . . C24 C 0.6071(3) -0.0238(4) 0.10008(13) 0.0388(10) Uani 1 1 d U . . H24 H 0.5711 0.0236 0.0767 0.047 Uiso 1 1 calc R . . C25 C 0.7041(3) -0.0215(4) 0.11155(12) 0.0369(9) Uani 1 1 d U . . H25 H 0.7504 0.0283 0.0979 0.044 Uiso 1 1 calc R . . C26 C 0.5590(4) -0.1890(7) 0.2305(2) 0.0837(19) Uani 1 1 d U . . H26A H 0.6044 -0.1687 0.2568 0.100 Uiso 1 1 calc R . . H26B H 0.5366 -0.0981 0.2177 0.100 Uiso 1 1 calc R . . C27 C 0.4738(4) -0.2634(7) 0.2423(2) 0.0903(19) Uani 1 1 d U . . H27A H 0.4217 -0.2656 0.2180 0.136 Uiso 1 1 calc R . . H27B H 0.4503 -0.2149 0.2661 0.136 Uiso 1 1 calc R . . H27C H 0.4925 -0.3592 0.2508 0.136 Uiso 1 1 calc R . . C28 C 0.5689(3) -0.4107(5) 0.17085(16) 0.0527(12) Uani 1 1 d U . . H28A H 0.5570 -0.4810 0.1924 0.063 Uiso 1 1 calc R . . H28B H 0.5043 -0.3802 0.1562 0.063 Uiso 1 1 calc R . . C29 C 0.6239(4) -0.4813(5) 0.13841(16) 0.0625(13) Uani 1 1 d U . . H29A H 0.6267 -0.4181 0.1144 0.094 Uiso 1 1 calc R . . H29B H 0.5900 -0.5675 0.1283 0.094 Uiso 1 1 calc R . . H29C H 0.6904 -0.5037 0.1517 0.094 Uiso 1 1 calc R . . C30 C 0.7258(3) -0.3267(4) 0.22313(12) 0.0350(9) Uani 1 1 d U . . H30A H 0.7674 -0.3685 0.2036 0.042 Uiso 1 1 calc R . . H30B H 0.7605 -0.2439 0.2365 0.042 Uiso 1 1 calc R . . C31 C 0.7131(3) -0.4333(5) 0.25783(13) 0.0427(10) Uani 1 1 d U . . H31A H 0.6716 -0.3933 0.2773 0.064 Uiso 1 1 calc R . . H31B H 0.7772 -0.4566 0.2736 0.064 Uiso 1 1 calc R . . H31C H 0.6825 -0.5181 0.2448 0.064 Uiso 1 1 calc R . . C32 C 0.8230(3) -0.1130(4) 0.17016(12) 0.0339(8) Uani 1 1 d U . . C33 C 0.8486(3) -0.0190(4) 0.20311(12) 0.0398(9) Uani 1 1 d U . . C34 C 0.9460(3) -0.0263(5) 0.22362(14) 0.0482(10) Uani 1 1 d U . . H34 H 0.9670 0.0347 0.2467 0.058 Uiso 1 1 calc R . . C35 C 1.0105(3) -0.1198(5) 0.21071(15) 0.0517(10) Uani 1 1 d U . . H35 H 1.0755 -0.1232 0.2251 0.062 Uiso 1 1 calc R . . C36 C 0.9830(3) -0.2079(5) 0.17770(14) 0.0493(10) Uani 1 1 d U . . H36 H 1.0294 -0.2713 0.1692 0.059 Uiso 1 1 calc R . . C37 C 0.8879(3) -0.2070(5) 0.15607(13) 0.0392(8) Uani 1 1 d U . . C38 C 0.7792(4) 0.0891(5) 0.21487(14) 0.0513(10) Uani 1 1 d U . . H38 H 0.7116 0.0607 0.2023 0.062 Uiso 1 1 calc R . . C39 C 0.8027(5) 0.2310(5) 0.19469(17) 0.0715(15) Uani 1 1 d U . . H39A H 0.8703 0.2578 0.2051 0.107 Uiso 1 1 calc R . . H39B H 0.7582 0.3031 0.2025 0.107 Uiso 1 1 calc R . . H39C H 0.7944 0.2216 0.1637 0.107 Uiso 1 1 calc R . . C40 C 0.7811(4) 0.1059(5) 0.26299(15) 0.0609(13) Uani 1 1 d U . . H40A H 0.7630 0.0172 0.2752 0.091 Uiso 1 1 calc R . . H40B H 0.7344 0.1786 0.2685 0.091 Uiso 1 1 calc R . . H40C H 0.8469 0.1329 0.2761 0.091 Uiso 1 1 calc R . . C41 C 0.8616(3) -0.3000(5) 0.11814(14) 0.0460(10) Uani 1 1 d U . . H41 H 0.7889 -0.2989 0.1107 0.055 Uiso 1 1 calc R . . C42 C 0.9054(3) -0.2435(6) 0.07956(15) 0.0649(13) Uani 1 1 d U . . H42A H 0.8832 -0.1472 0.0737 0.097 Uiso 1 1 calc R . . H42B H 0.8840 -0.3021 0.0547 0.097 Uiso 1 1 calc R . . H42C H 0.9769 -0.2451 0.0857 0.097 Uiso 1 1 calc R . . C43 C 0.8932(4) -0.4526(6) 0.12737(19) 0.0701(14) Uani 1 1 d U . . H43A H 0.9647 -0.4587 0.1312 0.105 Uiso 1 1 calc R . . H43B H 0.8658 -0.5120 0.1035 0.105 Uiso 1 1 calc R . . H43C H 0.8692 -0.4843 0.1533 0.105 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 N1 0.0222(16) 0.057(2) 0.039(2) 0.0114(18) -0.0020(14) 0.0140(16) N2 0.0213(15) 0.050(2) 0.0207(16) -0.0079(15) -0.0004(13) 0.0090(15) N3 0.0204(16) 0.051(2) 0.039(2) 0.0077(17) -0.0016(14) 0.0130(15) N4 0.0239(16) 0.0388(18) 0.0216(16) -0.0019(14) -0.0051(13) 0.0078(14) B1 0.029(2) 0.042(3) 0.063(4) -0.012(3) -0.003(2) 0.007(2) B2 0.028(2) 0.054(3) 0.042(3) 0.011(3) 0.008(2) 0.012(2) C1 0.0179(18) 0.049(3) 0.033(2) 0.006(2) 0.0044(16) 0.0099(18) C2 0.031(2) 0.090(3) 0.029(2) -0.011(2) -0.0044(17) 0.020(2) C3 0.029(2) 0.078(3) 0.030(2) -0.022(2) -0.0044(17) 0.0165(19) C4 0.024(2) 0.060(3) 0.084(4) 0.020(3) -0.002(2) 0.011(2) C5 0.056(3) 0.112(5) 0.139(5) -0.090(4) -0.031(3) 0.046(3) C6 0.097(4) 0.107(5) 0.118(5) -0.045(4) 0.014(4) 0.009(4) C7 0.038(3) 0.062(3) 0.122(5) 0.017(3) -0.006(3) 0.005(2) C8 0.052(3) 0.078(4) 0.131(5) 0.040(4) 0.012(3) 0.006(3) C9 0.034(2) 0.045(2) 0.037(2) -0.011(2) -0.0010(18) 0.0017(19) C10 0.053(3) 0.068(3) 0.063(3) -0.029(3) -0.012(2) 0.004(2) C11 0.0241(16) 0.0347(18) 0.0265(17) -0.0100(15) -0.0053(13) 0.0067(15) C12 0.0262(15) 0.0321(17) 0.0300(17) -0.0095(15) -0.0017(13) 0.0022(14) C13 0.0343(18) 0.0319(18) 0.044(2) -0.0023(16) 0.0020(16) 0.0025(15) C14 0.0328(18) 0.037(2) 0.050(2) -0.0005(17) -0.0026(16) 0.0120(16) C15 0.0274(17) 0.043(2) 0.043(2) -0.0066(16) 0.0025(15) 0.0097(16) C16 0.0250(16) 0.0373(18) 0.0294(16) -0.0081(14) 0.0007(13) 0.0082(14) C17 0.0279(17) 0.041(2) 0.0354(19) -0.0072(17) 0.0009(15) 0.0024(16) C18 0.034(2) 0.047(2) 0.040(2) -0.005(2) 0.0064(17) 0.0013(19) C19 0.034(2) 0.083(3) 0.063(3) -0.027(3) 0.008(2) -0.014(2) C20 0.0306(18) 0.053(2) 0.0302(19) -0.0050(16) 0.0034(15) 0.0163(17) C21 0.054(3) 0.085(3) 0.033(2) -0.015(2) -0.001(2) 0.030(2) C22 0.037(2) 0.075(3) 0.043(3) 0.007(2) 0.0119(19) 0.004(2) C23 0.025(2) 0.041(2) 0.026(2) -0.0036(18) -0.0011(16) 0.0135(18) C24 0.0324(19) 0.053(2) 0.029(2) 0.0047(19) -0.0045(16) 0.0151(19) C25 0.0331(19) 0.048(2) 0.028(2) 0.0072(18) -0.0014(16) 0.0108(18) C26 0.050(3) 0.110(4) 0.099(4) 0.062(4) 0.039(3) 0.047(3) C27 0.079(4) 0.098(4) 0.099(4) 0.031(4) 0.032(3) 0.018(3) C28 0.033(2) 0.059(3) 0.060(3) 0.019(2) -0.011(2) -0.001(2) C29 0.061(3) 0.056(3) 0.062(3) -0.005(3) -0.018(2) -0.002(2) C30 0.032(2) 0.043(2) 0.029(2) 0.0037(18) 0.0026(16) 0.0069(18) C31 0.037(2) 0.051(2) 0.040(2) 0.009(2) 0.0040(19) 0.009(2) C32 0.0266(17) 0.0448(19) 0.0272(18) 0.0071(15) -0.0065(14) 0.0006(15) C33 0.0420(18) 0.0438(18) 0.0298(18) 0.0075(15) -0.0076(15) -0.0026(16) C34 0.047(2) 0.054(2) 0.038(2) 0.0087(18) -0.0136(17) -0.0135(17) C35 0.0318(19) 0.069(3) 0.049(2) 0.016(2) -0.0115(18) -0.0028(18) C36 0.0278(18) 0.066(2) 0.050(2) 0.0132(19) -0.0057(17) 0.0057(18) C37 0.0241(16) 0.0528(19) 0.0393(18) 0.0099(16) -0.0005(14) 0.0049(16) C38 0.061(2) 0.050(2) 0.039(2) -0.0048(19) -0.0032(19) -0.0009(19) C39 0.111(4) 0.050(2) 0.054(3) 0.001(2) 0.011(3) 0.010(3) C40 0.074(3) 0.061(3) 0.048(2) -0.008(2) 0.006(2) -0.011(3) C41 0.0266(19) 0.063(2) 0.048(2) -0.0020(18) 0.0051(16) 0.0111(18) C42 0.043(3) 0.103(4) 0.050(3) -0.004(3) 0.010(2) -0.001(3) C43 0.055(3) 0.068(3) 0.089(4) -0.006(3) 0.018(3) 0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.377(5) . ? N1 C2 1.378(6) . ? N1 C4 1.459(5) . ? N2 C1 1.365(5) . ? N2 C3 1.396(5) . ? N2 C11 1.447(5) . ? N3 C23 1.356(5) . ? N3 C24 1.372(5) . ? N3 C4 1.458(5) . ? N4 C23 1.358(5) . ? N4 C25 1.384(5) . ? N4 C32 1.463(4) . ? B1 C7 1.616(8) . ? B1 C9 1.631(6) . ? B1 C1 1.651(6) . ? B1 C5 1.785(9) . ? B2 C30 1.632(6) . ? B2 C28 1.642(7) . ? B2 C23 1.651(6) . ? B2 C26 1.730(7) . ? C2 C3 1.326(6) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.434(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.481(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.522(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.402(5) . ? C11 C12 1.402(5) . ? C12 C13 1.382(5) . ? C12 C17 1.503(5) . ? C13 C14 1.378(5) . ? C13 H13 0.9500 . ? C14 C15 1.371(6) . ? C14 H14 0.9500 . ? C15 C16 1.385(5) . ? C15 H15 0.9500 . ? C16 C20 1.511(6) . ? C17 C18 1.525(5) . ? C17 C19 1.542(6) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.533(6) . ? C20 C21 1.538(6) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 C25 1.339(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.471(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.525(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.531(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.388(6) . ? C32 C37 1.389(6) . ? C33 C34 1.412(6) . ? C33 C38 1.494(6) . ? C34 C35 1.366(6) . ? C34 H34 0.9500 . ? C35 C36 1.358(6) . ? C35 H35 0.9500 . ? C36 C37 1.395(5) . ? C36 H36 0.9500 . ? C37 C41 1.502(6) . ? C38 C40 1.536(6) . ? C38 C39 1.556(7) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43 1.539(7) . ? C41 C42 1.542(6) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 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 C1 N1 C2 111.7(3) . . ? C1 N1 C4 125.3(4) . . ? C2 N1 C4 123.0(3) . . ? C1 N2 C3 111.6(3) . . ? C1 N2 C11 129.3(3) . . ? C3 N2 C11 118.8(3) . . ? C23 N3 C24 112.4(3) . . ? C23 N3 C4 125.0(4) . . ? C24 N3 C4 122.7(3) . . ? C23 N4 C25 111.6(3) . . ? C23 N4 C32 128.1(3) . . ? C25 N4 C32 120.0(3) . . ? C7 B1 C9 109.8(4) . . ? C7 B1 C1 109.5(4) . . ? C9 B1 C1 111.1(3) . . ? C7 B1 C5 113.0(4) . . ? C9 B1 C5 107.9(4) . . ? C1 B1 C5 105.4(3) . . ? C30 B2 C28 108.9(4) . . ? C30 B2 C23 112.4(3) . . ? C28 B2 C23 106.2(4) . . ? C30 B2 C26 106.5(4) . . ? C28 B2 C26 116.1(4) . . ? C23 B2 C26 106.8(3) . . ? N2 C1 N1 102.6(3) . . ? N2 C1 B1 131.5(3) . . ? N1 C1 B1 125.9(4) . . ? C3 C2 N1 107.4(4) . . ? C3 C2 H2 126.3 . . ? N1 C2 H2 126.3 . . ? C2 C3 N2 106.7(4) . . ? C2 C3 H3 126.6 . . ? N2 C3 H3 126.6 . . ? N3 C4 N1 109.2(4) . . ? N3 C4 H4A 109.8 . . ? N1 C4 H4A 109.8 . . ? N3 C4 H4B 109.8 . . ? N1 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? C6 C5 B1 118.2(6) . . ? C6 C5 H5A 107.8 . . ? B1 C5 H5A 107.8 . . ? C6 C5 H5B 107.8 . . ? B1 C5 H5B 107.8 . . ? H5A C5 H5B 107.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 B1 114.7(5) . . ? C8 C7 H7A 108.6 . . ? B1 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? B1 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 B1 116.7(4) . . ? C10 C9 H9A 108.1 . . ? B1 C9 H9A 108.1 . . ? C10 C9 H9B 108.1 . . ? B1 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 123.3(3) . . ? C16 C11 N2 118.9(3) . . ? C12 C11 N2 117.6(3) . . ? C13 C12 C11 116.9(3) . . ? C13 C12 C17 120.4(4) . . ? C11 C12 C17 122.6(3) . . ? C14 C13 C12 121.2(4) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 121.8(4) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C15 C16 C11 116.4(4) . . ? C15 C16 C20 120.5(3) . . ? C11 C16 C20 123.1(3) . . ? C12 C17 C18 112.5(3) . . ? C12 C17 C19 110.1(3) . . ? C18 C17 C19 110.1(4) . . ? C12 C17 H17 108.0 . . ? C18 C17 H17 108.0 . . ? C19 C17 H17 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 C22 112.4(3) . . ? C16 C20 C21 110.7(4) . . ? C22 C20 C21 109.8(3) . . ? C16 C20 H20 107.9 . . ? C22 C20 H20 107.9 . . ? C21 C20 H20 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 N4 103.0(3) . . ? N3 C23 B2 125.5(3) . . ? N4 C23 B2 131.4(3) . . ? C25 C24 N3 106.4(3) . . ? C25 C24 H24 126.8 . . ? N3 C24 H24 126.8 . . ? C24 C25 N4 106.6(4) . . ? C24 C25 H25 126.7 . . ? N4 C25 H25 126.7 . . ? C27 C26 B2 116.0(6) . . ? C27 C26 H26A 108.3 . . ? B2 C26 H26A 108.3 . . ? C27 C26 H26B 108.3 . . ? B2 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 B2 115.7(4) . . ? C29 C28 H28A 108.4 . . ? B2 C28 H28A 108.4 . . ? C29 C28 H28B 108.4 . . ? B2 C28 H28B 108.4 . . ? H28A C28 H28B 107.4 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 B2 114.2(3) . . ? C31 C30 H30A 108.7 . . ? B2 C30 H30A 108.7 . . ? C31 C30 H30B 108.7 . . ? B2 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 123.7(3) . . ? C33 C32 N4 117.9(3) . . ? C37 C32 N4 118.2(3) . . ? C32 C33 C34 116.2(4) . . ? C32 C33 C38 122.2(4) . . ? C34 C33 C38 121.5(4) . . ? C35 C34 C33 120.9(4) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C36 C35 C34 121.1(4) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C37 121.2(4) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C32 C37 C36 116.9(4) . . ? C32 C37 C41 123.3(3) . . ? C36 C37 C41 119.8(4) . . ? C33 C38 C40 113.7(4) . . ? C33 C38 C39 108.7(4) . . ? C40 C38 C39 110.2(4) . . ? C33 C38 H38 108.0 . . ? C40 C38 H38 108.0 . . ? C39 C38 H38 108.0 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C37 C41 C43 112.2(4) . . ? C37 C41 C42 110.7(4) . . ? C43 C41 C42 110.6(4) . . ? C37 C41 H41 107.7 . . ? C43 C41 H41 107.7 . . ? C42 C41 H41 107.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N2 C1 N1 -0.3(4) . . . . ? C11 N2 C1 N1 172.8(3) . . . . ? C3 N2 C1 B1 178.3(4) . . . . ? C11 N2 C1 B1 -8.6(7) . . . . ? C2 N1 C1 N2 0.0(4) . . . . ? C4 N1 C1 N2 179.3(4) . . . . ? C2 N1 C1 B1 -178.8(4) . . . . ? C4 N1 C1 B1 0.5(6) . . . . ? C7 B1 C1 N2 -127.6(4) . . . . ? C9 B1 C1 N2 -6.1(6) . . . . ? C5 B1 C1 N2 110.5(5) . . . . ? C7 B1 C1 N1 50.7(5) . . . . ? C9 B1 C1 N1 172.2(4) . . . . ? C5 B1 C1 N1 -71.2(5) . . . . ? C1 N1 C2 C3 0.3(5) . . . . ? C4 N1 C2 C3 -179.0(4) . . . . ? N1 C2 C3 N2 -0.5(5) . . . . ? C1 N2 C3 C2 0.5(5) . . . . ? C11 N2 C3 C2 -173.4(4) . . . . ? C23 N3 C4 N1 132.0(4) . . . . ? C24 N3 C4 N1 -47.2(6) . . . . ? C1 N1 C4 N3 130.1(4) . . . . ? C2 N1 C4 N3 -50.7(6) . . . . ? C7 B1 C5 C6 53.9(7) . . . . ? C9 B1 C5 C6 -67.8(7) . . . . ? C1 B1 C5 C6 173.4(5) . . . . ? C9 B1 C7 C8 -74.4(6) . . . . ? C1 B1 C7 C8 47.9(5) . . . . ? C5 B1 C7 C8 165.1(4) . . . . ? C7 B1 C9 C10 -50.4(6) . . . . ? C1 B1 C9 C10 -171.7(4) . . . . ? C5 B1 C9 C10 73.2(5) . . . . ? C1 N2 C11 C16 98.7(4) . . . . ? C3 N2 C11 C16 -88.7(4) . . . . ? C1 N2 C11 C12 -86.0(5) . . . . ? C3 N2 C11 C12 86.6(4) . . . . ? C16 C11 C12 C13 0.9(5) . . . . ? N2 C11 C12 C13 -174.2(3) . . . . ? C16 C11 C12 C17 178.1(3) . . . . ? N2 C11 C12 C17 3.0(5) . . . . ? C11 C12 C13 C14 -0.5(6) . . . . ? C17 C12 C13 C14 -177.7(4) . . . . ? C12 C13 C14 C15 -0.7(6) . . . . ? C13 C14 C15 C16 1.6(6) . . . . ? C14 C15 C16 C11 -1.1(6) . . . . ? C14 C15 C16 C20 177.3(4) . . . . ? C12 C11 C16 C15 -0.1(5) . . . . ? N2 C11 C16 C15 174.9(3) . . . . ? C12 C11 C16 C20 -178.5(4) . . . . ? N2 C11 C16 C20 -3.5(5) . . . . ? C13 C12 C17 C18 -47.3(5) . . . . ? C11 C12 C17 C18 135.6(4) . . . . ? C13 C12 C17 C19 76.0(5) . . . . ? C11 C12 C17 C19 -101.1(4) . . . . ? C15 C16 C20 C22 46.0(5) . . . . ? C11 C16 C20 C22 -135.7(4) . . . . ? C15 C16 C20 C21 -77.2(4) . . . . ? C11 C16 C20 C21 101.0(4) . . . . ? C24 N3 C23 N4 0.8(4) . . . . ? C4 N3 C23 N4 -178.5(4) . . . . ? C24 N3 C23 B2 -175.7(4) . . . . ? C4 N3 C23 B2 5.0(6) . . . . ? C25 N4 C23 N3 -0.6(4) . . . . ? C32 N4 C23 N3 172.4(3) . . . . ? C25 N4 C23 B2 175.6(4) . . . . ? C32 N4 C23 B2 -11.4(6) . . . . ? C30 B2 C23 N3 175.4(4) . . . . ? C28 B2 C23 N3 56.4(5) . . . . ? C26 B2 C23 N3 -68.1(5) . . . . ? C30 B2 C23 N4 0.0(6) . . . . ? C28 B2 C23 N4 -119.0(4) . . . . ? C26 B2 C23 N4 116.5(5) . . . . ? C23 N3 C24 C25 -0.7(5) . . . . ? C4 N3 C24 C25 178.6(4) . . . . ? N3 C24 C25 N4 0.3(4) . . . . ? C23 N4 C25 C24 0.2(4) . . . . ? C32 N4 C25 C24 -173.4(3) . . . . ? C30 B2 C26 C27 -107.3(5) . . . . ? C28 B2 C26 C27 14.1(6) . . . . ? C23 B2 C26 C27 132.3(5) . . . . ? C30 B2 C28 C29 -62.9(5) . . . . ? C23 B2 C28 C29 58.4(5) . . . . ? C26 B2 C28 C29 176.9(4) . . . . ? C28 B2 C30 C31 -62.0(5) . . . . ? C23 B2 C30 C31 -179.4(3) . . . . ? C26 B2 C30 C31 63.9(5) . . . . ? C23 N4 C32 C33 -82.0(5) . . . . ? C25 N4 C32 C33 90.5(4) . . . . ? C23 N4 C32 C37 102.2(5) . . . . ? C25 N4 C32 C37 -85.3(5) . . . . ? C37 C32 C33 C34 -2.4(6) . . . . ? N4 C32 C33 C34 -177.9(3) . . . . ? C37 C32 C33 C38 174.5(4) . . . . ? N4 C32 C33 C38 -1.1(6) . . . . ? C32 C33 C34 C35 1.1(6) . . . . ? C38 C33 C34 C35 -175.8(4) . . . . ? C33 C34 C35 C36 0.3(7) . . . . ? C34 C35 C36 C37 -0.6(7) . . . . ? C33 C32 C37 C36 2.1(6) . . . . ? N4 C32 C37 C36 177.7(4) . . . . ? C33 C32 C37 C41 -174.8(4) . . . . ? N4 C32 C37 C41 0.7(6) . . . . ? C35 C36 C37 C32 -0.6(6) . . . . ? C35 C36 C37 C41 176.5(4) . . . . ? C32 C33 C38 C40 137.7(4) . . . . ? C34 C33 C38 C40 -45.7(6) . . . . ? C32 C33 C38 C39 -99.2(5) . . . . ? C34 C33 C38 C39 77.4(5) . . . . ? C32 C37 C41 C43 -132.5(4) . . . . ? C36 C37 C41 C43 50.6(6) . . . . ? C32 C37 C41 C42 103.3(5) . . . . ? C36 C37 C41 C42 -73.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.683 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.063 #===END data_c:\workdo~1\crystals\omji78~1\fromch~1\omji78 _database_code_depnum_ccdc_archive 'CCDC 851125' #TrackingRef '- final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H40 Fe N4 O3' _chemical_formula_sum 'C40 H40 Fe N4 O3' _chemical_formula_weight 680.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6580(5) _cell_length_b 19.9015(7) _cell_length_c 17.2833(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.984(5) _cell_angle_gamma 90.00 _cell_volume 3610.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7240 _cell_measurement_theta_min 2.9232 _cell_measurement_theta_max 28.4801 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.460 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9136 _exptl_absorpt_correction_T_max 0.9555 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_reflns_number 20832 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6356 _reflns_number_gt 4936 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+2.7105P] 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 6356 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1083 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _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 0.35393(3) 0.777004(17) 0.77465(2) 0.01723(11) Uani 1 1 d . . . N1 N 0.32602(19) 0.74230(10) 0.60730(12) 0.0204(5) Uani 1 1 d . . . N2 N 0.14184(19) 0.77104(9) 0.62720(12) 0.0173(4) Uani 1 1 d . . . N3 N 0.48443(19) 0.67931(10) 0.68791(12) 0.0199(5) Uani 1 1 d . . . N4 N 0.51044(18) 0.64626(10) 0.80628(12) 0.0182(5) Uani 1 1 d . . . O1 O 0.48242(17) 0.80717(9) 0.93348(11) 0.0268(4) Uani 1 1 d . . . O2 O 0.4378(2) 0.90690(10) 0.72629(13) 0.0372(5) Uani 1 1 d . . . O3 O 0.12803(17) 0.76875(10) 0.84941(11) 0.0300(5) Uani 1 1 d . . . C1 C 0.4350(2) 0.79272(12) 0.87054(16) 0.0196(6) Uani 1 1 d . . . C2 C 0.4061(3) 0.85575(15) 0.74300(16) 0.0282(6) Uani 1 1 d . . . C3 C 0.2128(2) 0.76999(12) 0.81563(15) 0.0208(6) Uani 1 1 d . . . C4 C 0.2643(2) 0.76180(12) 0.66591(15) 0.0179(5) Uani 1 1 d . . . C5 C 0.2479(2) 0.74085(13) 0.53464(15) 0.0233(6) Uani 1 1 d . . . H5 H 0.2715 0.7294 0.4858 0.028 Uiso 1 1 calc R . . C6 C 0.1325(2) 0.75888(12) 0.54732(15) 0.0218(6) Uani 1 1 d . . . H6 H 0.0577 0.7627 0.5087 0.026 Uiso 1 1 calc R . . C7 C 0.4602(2) 0.72500(14) 0.62218(15) 0.0241(6) Uani 1 1 d . . . H7A H 0.4838 0.7036 0.5750 0.029 Uiso 1 1 calc R . . H7B H 0.5122 0.7661 0.6341 0.029 Uiso 1 1 calc R . . C8 C 0.4571(2) 0.69745(12) 0.75910(15) 0.0186(5) Uani 1 1 d . . . C9 C 0.5663(2) 0.59832(13) 0.76446(16) 0.0238(6) Uani 1 1 d . . . H9 H 0.6085 0.5585 0.7851 0.029 Uiso 1 1 calc R . . C10 C 0.5494(2) 0.61900(13) 0.68997(16) 0.0250(6) Uani 1 1 d . . . H10 H 0.5764 0.5968 0.6470 0.030 Uiso 1 1 calc R . . C11 C 0.0306(2) 0.78519(12) 0.66180(15) 0.0205(6) Uani 1 1 d . . . C12 C -0.0544(2) 0.73228(13) 0.66775(15) 0.0230(6) Uani 1 1 d . . . C13 C -0.1612(2) 0.74712(14) 0.70019(16) 0.0275(6) Uani 1 1 d . . . H13 H -0.2203 0.7124 0.7054 0.033 Uiso 1 1 calc R . . C14 C -0.1838(3) 0.81100(15) 0.72506(16) 0.0305(7) Uani 1 1 d . . . H14 H -0.2571 0.8198 0.7478 0.037 Uiso 1 1 calc R . . C15 C -0.1002(3) 0.86211(14) 0.71694(16) 0.0285(7) Uani 1 1 d . . . H15 H -0.1173 0.9061 0.7336 0.034 Uiso 1 1 calc R . . C16 C 0.0094(2) 0.85077(13) 0.68473(15) 0.0239(6) Uani 1 1 d . . . C17 C -0.0298(3) 0.66137(13) 0.64195(16) 0.0259(6) Uani 1 1 d . . . H17 H 0.0084 0.6649 0.5932 0.031 Uiso 1 1 calc R . . C18 C -0.1501(3) 0.61836(15) 0.62229(19) 0.0369(7) Uani 1 1 d . . . H18A H -0.1297 0.5764 0.5975 0.055 Uiso 1 1 calc R . . H18B H -0.2150 0.6430 0.5861 0.055 Uiso 1 1 calc R . . H18C H -0.1826 0.6081 0.6706 0.055 Uiso 1 1 calc R . . C19 C 0.0671(3) 0.62601(14) 0.70404(18) 0.0330(7) Uani 1 1 d . . . H19A H 0.1469 0.6516 0.7129 0.050 Uiso 1 1 calc R . . H19B H 0.0830 0.5807 0.6859 0.050 Uiso 1 1 calc R . . H19C H 0.0335 0.6231 0.7533 0.050 Uiso 1 1 calc R . . C20 C 0.0961(3) 0.90842(13) 0.67177(17) 0.0278(6) Uani 1 1 d . . . H20 H 0.1789 0.8889 0.6629 0.033 Uiso 1 1 calc R . . C21 C 0.0378(3) 0.94673(15) 0.59734(19) 0.0389(8) Uani 1 1 d . . . H21A H 0.0282 0.9163 0.5521 0.058 Uiso 1 1 calc R . . H21B H 0.0938 0.9841 0.5890 0.058 Uiso 1 1 calc R . . H21C H -0.0459 0.9643 0.6033 0.058 Uiso 1 1 calc R . . C22 C 0.1240(3) 0.95533(16) 0.7420(2) 0.0448(8) Uani 1 1 d . . . H22A H 0.0454 0.9781 0.7493 0.067 Uiso 1 1 calc R . . H22B H 0.1872 0.9888 0.7329 0.067 Uiso 1 1 calc R . . H22C H 0.1575 0.9293 0.7893 0.067 Uiso 1 1 calc R . . C23 C 0.5269(2) 0.64398(12) 0.89089(15) 0.0197(6) Uani 1 1 d . . . C24 C 0.4303(2) 0.61587(12) 0.92583(16) 0.0216(6) Uani 1 1 d . . . C25 C 0.4546(3) 0.60999(13) 1.00740(16) 0.0270(6) Uani 1 1 d . . . H25 H 0.3911 0.5918 1.0337 0.032 Uiso 1 1 calc R . . C26 C 0.5700(3) 0.63030(13) 1.05076(16) 0.0282(6) Uani 1 1 d . . . H26 H 0.5860 0.6243 1.1061 0.034 Uiso 1 1 calc R . . C27 C 0.6618(3) 0.65909(13) 1.01445(16) 0.0266(6) Uani 1 1 d . . . H27 H 0.7399 0.6734 1.0452 0.032 Uiso 1 1 calc R . . C28 C 0.6418(2) 0.66756(12) 0.93353(15) 0.0213(6) Uani 1 1 d . . . C29 C 0.3066(2) 0.59226(12) 0.87646(16) 0.0243(6) Uani 1 1 d . . . H29 H 0.2873 0.6229 0.8301 0.029 Uiso 1 1 calc R . . C31 C 0.3194(3) 0.52154(15) 0.8453(2) 0.0423(8) Uani 1 1 d . . . H31A H 0.3909 0.5200 0.8166 0.063 Uiso 1 1 calc R . . H31B H 0.2406 0.5092 0.8100 0.063 Uiso 1 1 calc R . . H31C H 0.3348 0.4899 0.8894 0.063 Uiso 1 1 calc R . . C30 C 0.1947(3) 0.59531(14) 0.91958(19) 0.0339(7) Uani 1 1 d . . . H30A H 0.2077 0.5631 0.9631 0.051 Uiso 1 1 calc R . . H30B H 0.1163 0.5840 0.8833 0.051 Uiso 1 1 calc R . . H30C H 0.1876 0.6408 0.9402 0.051 Uiso 1 1 calc R . . C32 C 0.7434(2) 0.69994(14) 0.89401(16) 0.0258(6) Uani 1 1 d . . . H32 H 0.7039 0.7105 0.8386 0.031 Uiso 1 1 calc R . . C33 C 0.8547(3) 0.65188(15) 0.89158(18) 0.0349(7) Uani 1 1 d . . . H33A H 0.8930 0.6392 0.9453 0.052 Uiso 1 1 calc R . . H33B H 0.9187 0.6741 0.8661 0.052 Uiso 1 1 calc R . . H33C H 0.8236 0.6115 0.8618 0.052 Uiso 1 1 calc R . . C34 C 0.7925(3) 0.76587(14) 0.93395(18) 0.0326(7) Uani 1 1 d . . . H34A H 0.7215 0.7974 0.9321 0.049 Uiso 1 1 calc R . . H34B H 0.8570 0.7853 0.9065 0.049 Uiso 1 1 calc R . . H34C H 0.8305 0.7570 0.9888 0.049 Uiso 1 1 calc R . . C50A C 0.2483(5) 0.5630(3) 0.5545(3) 0.048(3) Uani 0.50 1 d PG A 1 C51A C 0.2895(6) 0.5116(3) 0.6072(3) 0.039(2) Uani 0.50 1 d PG A 1 C52 C 0.3810(6) 0.4663(3) 0.5913(3) 0.072(3) Uani 0.50 1 d PG A 1 C53 C 0.4313(6) 0.4725(3) 0.5226(4) 0.104(4) Uani 0.50 1 d PG . 1 C54 C 0.3902(7) 0.5239(3) 0.4699(3) 0.100(4) Uani 0.50 1 d PG . 1 C55 C 0.2986(6) 0.5692(2) 0.4859(3) 0.057(2) Uani 0.50 1 d PG A 1 C50B C 0.2680(6) 0.5563(4) 0.5478(6) 0.145(10) Uani 0.50 1 d PG B 2 C51B C 0.2972(6) 0.5033(5) 0.6002(5) 0.144(9) Uani 0.50 1 d PG B 2 C56 C 0.2049(9) 0.4556(3) 0.6081(4) 0.081(3) Uani 0.50 1 d PG B 2 C57 C 0.0835(7) 0.4610(3) 0.5636(4) 0.087(3) Uani 0.50 1 d PG . 2 C58 C 0.0544(5) 0.5140(4) 0.5112(4) 0.081(3) Uani 0.50 1 d PG . 2 C59 C 0.1466(7) 0.5616(3) 0.5033(4) 0.074(3) Uani 0.50 1 d PG B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0174(2) 0.0199(2) 0.0140(2) 0.00021(15) 0.00172(14) 0.00055(15) N1 0.0184(11) 0.0306(12) 0.0119(11) 0.0013(9) 0.0017(9) 0.0023(9) N2 0.0178(11) 0.0193(11) 0.0145(11) 0.0013(8) 0.0016(8) 0.0020(8) N3 0.0158(11) 0.0296(12) 0.0147(12) -0.0005(9) 0.0039(9) 0.0026(9) N4 0.0160(11) 0.0222(11) 0.0158(12) 0.0000(9) 0.0008(9) 0.0034(8) O1 0.0253(10) 0.0371(11) 0.0170(11) -0.0063(8) 0.0007(8) -0.0020(8) O2 0.0437(13) 0.0248(11) 0.0455(14) -0.0002(9) 0.0144(10) -0.0170(9) O3 0.0201(10) 0.0509(13) 0.0197(11) 0.0037(9) 0.0052(8) 0.0052(9) C1 0.0169(13) 0.0218(13) 0.0226(16) 0.0026(11) 0.0101(11) 0.0018(10) C2 0.0279(16) 0.0369(17) 0.0197(15) -0.0012(12) 0.0036(12) 0.0048(13) C3 0.0212(14) 0.0254(14) 0.0130(13) -0.0008(10) -0.0047(11) 0.0023(11) C4 0.0190(13) 0.0189(13) 0.0169(14) 0.0014(10) 0.0057(11) 0.0012(10) C5 0.0235(14) 0.0314(15) 0.0143(14) 0.0025(11) 0.0016(11) 0.0016(11) C6 0.0206(14) 0.0266(14) 0.0169(14) 0.0019(11) -0.0005(11) 0.0012(11) C7 0.0179(13) 0.0390(16) 0.0163(14) 0.0036(12) 0.0055(11) 0.0031(11) C8 0.0149(13) 0.0245(13) 0.0160(14) -0.0006(10) 0.0011(10) -0.0041(10) C9 0.0206(14) 0.0275(14) 0.0229(16) -0.0040(11) 0.0028(11) 0.0080(11) C10 0.0177(14) 0.0323(15) 0.0253(16) -0.0080(12) 0.0045(11) 0.0072(11) C11 0.0194(13) 0.0276(14) 0.0138(13) 0.0037(10) 0.0014(10) 0.0074(11) C12 0.0188(13) 0.0336(15) 0.0151(14) 0.0056(11) -0.0009(10) 0.0022(11) C13 0.0205(14) 0.0388(16) 0.0230(16) 0.0055(12) 0.0032(12) 0.0029(12) C14 0.0225(15) 0.0476(18) 0.0220(16) 0.0073(13) 0.0057(12) 0.0111(13) C15 0.0321(16) 0.0299(15) 0.0226(16) 0.0028(12) 0.0020(12) 0.0157(12) C16 0.0249(15) 0.0282(14) 0.0173(14) 0.0040(11) -0.0004(11) 0.0085(11) C17 0.0264(15) 0.0291(15) 0.0236(16) 0.0021(11) 0.0080(12) -0.0029(12) C18 0.0332(17) 0.0392(17) 0.0381(19) -0.0006(14) 0.0057(14) -0.0113(13) C19 0.0349(17) 0.0269(15) 0.0362(19) 0.0008(13) 0.0033(14) 0.0018(12) C20 0.0321(16) 0.0234(14) 0.0275(16) 0.0020(11) 0.0046(12) 0.0090(12) C21 0.051(2) 0.0303(16) 0.0362(19) 0.0085(13) 0.0097(15) 0.0089(14) C22 0.060(2) 0.0377(18) 0.037(2) -0.0079(14) 0.0070(16) -0.0013(16) C23 0.0227(14) 0.0174(13) 0.0190(14) 0.0010(10) 0.0033(11) 0.0067(10) C24 0.0247(14) 0.0167(13) 0.0235(15) 0.0024(10) 0.0042(11) 0.0078(10) C25 0.0324(16) 0.0246(14) 0.0261(16) 0.0067(11) 0.0108(13) 0.0055(12) C26 0.0375(17) 0.0284(15) 0.0181(15) 0.0032(11) 0.0033(13) 0.0107(12) C27 0.0243(15) 0.0306(15) 0.0222(16) -0.0007(11) -0.0031(12) 0.0068(12) C28 0.0209(14) 0.0231(13) 0.0189(14) 0.0014(10) 0.0004(11) 0.0082(11) C29 0.0261(15) 0.0200(13) 0.0276(16) 0.0037(11) 0.0068(12) -0.0001(11) C31 0.0379(19) 0.0333(17) 0.058(2) -0.0129(15) 0.0139(16) -0.0049(14) C30 0.0299(16) 0.0296(16) 0.043(2) -0.0023(13) 0.0099(14) -0.0019(12) C32 0.0162(14) 0.0374(16) 0.0219(15) -0.0011(12) -0.0025(11) 0.0007(11) C33 0.0252(16) 0.0480(18) 0.0314(18) -0.0048(14) 0.0047(13) 0.0046(13) C34 0.0187(14) 0.0409(17) 0.0361(18) -0.0026(13) -0.0008(12) -0.0025(12) C50A 0.056(6) 0.057(7) 0.034(5) 0.009(4) 0.021(4) 0.017(5) C51A 0.036(5) 0.040(6) 0.045(6) -0.002(5) 0.013(4) 0.002(4) C52 0.100(7) 0.041(5) 0.065(6) -0.019(4) -0.013(5) 0.023(4) C53 0.167(12) 0.063(6) 0.093(9) -0.002(6) 0.053(8) 0.022(6) C54 0.169(11) 0.041(5) 0.103(9) 0.004(5) 0.056(8) 0.029(6) C55 0.084(7) 0.038(4) 0.055(5) -0.002(4) 0.030(4) -0.010(4) C50B 0.037(6) 0.053(9) 0.35(3) -0.022(12) 0.049(12) -0.016(6) C51B 0.17(2) 0.084(13) 0.18(2) 0.032(13) 0.045(17) 0.027(14) C56 0.075(7) 0.077(6) 0.096(8) -0.040(6) 0.033(6) -0.012(5) C57 0.109(9) 0.077(7) 0.090(8) -0.033(6) 0.059(7) -0.016(6) C58 0.072(6) 0.099(7) 0.077(7) -0.058(6) 0.025(5) -0.011(5) C59 0.083(7) 0.060(5) 0.079(7) -0.029(5) 0.014(5) -0.009(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 Fe1 C1 1.759(3) . ? Fe1 C3 1.775(3) . ? Fe1 C2 1.781(3) . ? Fe1 C8 1.973(3) . ? Fe1 C4 1.978(3) . ? N1 C4 1.357(3) . ? N1 C5 1.381(3) . ? N1 C7 1.450(3) . ? N2 C4 1.372(3) . ? N2 C6 1.388(3) . ? N2 C11 1.445(3) . ? N3 C8 1.361(3) . ? N3 C10 1.383(3) . ? N3 C7 1.443(3) . ? N4 C8 1.366(3) . ? N4 C9 1.391(3) . ? N4 C23 1.443(3) . ? O1 C1 1.154(3) . ? O2 C2 1.126(3) . ? O3 C3 1.158(3) . ? C5 C6 1.336(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C9 C10 1.334(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.394(4) . ? C11 C12 1.405(4) . ? C12 C13 1.385(4) . ? C12 C17 1.517(4) . ? C13 C14 1.377(4) . ? C13 H13 0.9500 . ? C14 C15 1.375(4) . ? C14 H14 0.9500 . ? C15 C16 1.397(4) . ? C15 H15 0.9500 . ? C16 C20 1.514(4) . ? C17 C19 1.526(4) . ? C17 C18 1.530(4) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.520(4) . ? C20 C21 1.532(4) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C28 1.396(4) . ? C23 C24 1.398(4) . ? C24 C25 1.394(4) . ? C24 C29 1.515(4) . ? C25 C26 1.385(4) . ? C25 H25 0.9500 . ? C26 C27 1.376(4) . ? C26 H26 0.9500 . ? C27 C28 1.388(4) . ? C27 H27 0.9500 . ? C28 C32 1.520(4) . ? C29 C30 1.513(4) . ? C29 C31 1.521(4) . ? C29 H29 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C32 C33 1.530(4) . ? C32 C34 1.532(4) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C50A C51A 1.3900 . ? C50A C55 1.3900 . ? C51A C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C53 C54 1.886(13) 3_666 ? C54 C55 1.3900 . ? C54 C53 1.886(14) 3_666 ? C50B C51B 1.3900 . ? C50B C59 1.3900 . ? C51B C56 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C57 C58 1.849(18) 3_566 ? C58 C58 1.283(11) 3_566 ? C58 C59 1.3900 . ? C58 C57 1.849(12) 3_566 ? 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 C1 Fe1 C3 87.11(11) . . ? C1 Fe1 C2 90.25(12) . . ? C3 Fe1 C2 121.55(12) . . ? C1 Fe1 C8 94.40(11) . . ? C3 Fe1 C8 121.48(11) . . ? C2 Fe1 C8 116.95(11) . . ? C1 Fe1 C4 178.41(11) . . ? C3 Fe1 C4 93.68(11) . . ? C2 Fe1 C4 88.16(11) . . ? C8 Fe1 C4 86.36(10) . . ? C4 N1 C5 113.0(2) . . ? C4 N1 C7 121.8(2) . . ? C5 N1 C7 125.2(2) . . ? C4 N2 C6 111.1(2) . . ? C4 N2 C11 127.1(2) . . ? C6 N2 C11 121.5(2) . . ? C8 N3 C10 113.0(2) . . ? C8 N3 C7 120.5(2) . . ? C10 N3 C7 126.0(2) . . ? C8 N4 C9 111.9(2) . . ? C8 N4 C23 126.4(2) . . ? C9 N4 C23 121.1(2) . . ? O1 C1 Fe1 174.9(2) . . ? O2 C2 Fe1 176.6(3) . . ? O3 C3 Fe1 172.7(2) . . ? N1 C4 N2 102.6(2) . . ? N1 C4 Fe1 122.44(18) . . ? N2 C4 Fe1 134.79(18) . . ? C6 C5 N1 105.8(2) . . ? C6 C5 H5 127.1 . . ? N1 C5 H5 127.1 . . ? C5 C6 N2 107.5(2) . . ? C5 C6 H6 126.2 . . ? N2 C6 H6 126.2 . . ? N3 C7 N1 109.0(2) . . ? N3 C7 H7A 109.9 . . ? N1 C7 H7A 109.9 . . ? N3 C7 H7B 109.9 . . ? N1 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? N3 C8 N4 102.1(2) . . ? N3 C8 Fe1 123.21(18) . . ? N4 C8 Fe1 134.54(19) . . ? C10 C9 N4 106.9(2) . . ? C10 C9 H9 126.5 . . ? N4 C9 H9 126.5 . . ? C9 C10 N3 106.0(2) . . ? C9 C10 H10 127.0 . . ? N3 C10 H10 127.0 . . ? C16 C11 C12 122.9(2) . . ? C16 C11 N2 119.0(2) . . ? C12 C11 N2 118.1(2) . . ? C13 C12 C11 117.1(2) . . ? C13 C12 C17 120.9(2) . . ? C11 C12 C17 122.0(2) . . ? C14 C13 C12 121.6(3) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C15 C14 C13 120.0(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 121.5(3) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C11 C16 C15 116.9(2) . . ? C11 C16 C20 122.3(2) . . ? C15 C16 C20 120.7(2) . . ? C12 C17 C19 110.7(2) . . ? C12 C17 C18 113.9(2) . . ? C19 C17 C18 109.7(2) . . ? C12 C17 H17 107.4 . . ? C19 C17 H17 107.4 . . ? C18 C17 H17 107.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 C22 112.8(2) . . ? C16 C20 C21 109.4(2) . . ? C22 C20 C21 111.1(2) . . ? C16 C20 H20 107.8 . . ? C22 C20 H20 107.8 . . ? C21 C20 H20 107.8 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 123.4(2) . . ? C28 C23 N4 117.8(2) . . ? C24 C23 N4 118.7(2) . . ? C25 C24 C23 116.7(2) . . ? C25 C24 C29 122.3(2) . . ? C23 C24 C29 121.0(2) . . ? C26 C25 C24 121.0(3) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C27 C26 C25 120.7(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 120.9(3) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C27 C28 C23 117.3(2) . . ? C27 C28 C32 120.5(2) . . ? C23 C28 C32 122.2(2) . . ? C30 C29 C24 113.1(2) . . ? C30 C29 C31 109.7(2) . . ? C24 C29 C31 111.3(2) . . ? C30 C29 H29 107.5 . . ? C24 C29 H29 107.5 . . ? C31 C29 H29 107.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C32 C33 111.3(2) . . ? C28 C32 C34 112.0(2) . . ? C33 C32 C34 110.0(2) . . ? C28 C32 H32 107.8 . . ? C33 C32 H32 107.8 . . ? C34 C32 H32 107.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C51A C50A C55 120.0 . . ? C52 C51A C50A 120.0 . . ? C51A C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C54 C53 C54 102.5(7) . 3_666 ? C52 C53 C54 118.6(8) . 3_666 ? C55 C54 C53 120.0 . . ? C55 C54 C53 134.1(7) . 3_666 ? C53 C54 C53 77.5(7) . 3_666 ? C54 C55 C50A 120.0 . . ? C51B C50B C59 120.0 . . ? C50B C51B C56 120.0 . . ? C57 C56 C51B 120.0 . . ? C56 C57 C58 120.0 . . ? C56 C57 C58 163.3(7) . 3_566 ? C58 C57 C58 43.9(7) . 3_566 ? C58 C58 C59 152.1(12) 3_566 . ? C58 C58 C57 87.4(12) 3_566 . ? C59 C58 C57 120.0 . . ? C58 C58 C57 48.7(4) 3_566 3_566 ? C59 C58 C57 103.7(10) . 3_566 ? C57 C58 C57 136.1(10) . 3_566 ? C58 C59 C50B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Fe1 C1 O1 -61(3) . . . . ? C2 Fe1 C1 O1 61(3) . . . . ? C8 Fe1 C1 O1 178(100) . . . . ? C4 Fe1 C1 O1 59(5) . . . . ? C1 Fe1 C2 O2 -43(4) . . . . ? C3 Fe1 C2 O2 44(4) . . . . ? C8 Fe1 C2 O2 -138(4) . . . . ? C4 Fe1 C2 O2 137(4) . . . . ? C1 Fe1 C3 O3 16.0(18) . . . . ? C2 Fe1 C3 O3 -72.5(18) . . . . ? C8 Fe1 C3 O3 109.4(18) . . . . ? C4 Fe1 C3 O3 -162.6(18) . . . . ? C5 N1 C4 N2 1.5(3) . . . . ? C7 N1 C4 N2 -178.3(2) . . . . ? C5 N1 C4 Fe1 -174.11(17) . . . . ? C7 N1 C4 Fe1 6.1(3) . . . . ? C6 N2 C4 N1 -1.5(3) . . . . ? C11 N2 C4 N1 172.9(2) . . . . ? C6 N2 C4 Fe1 173.33(19) . . . . ? C11 N2 C4 Fe1 -12.3(4) . . . . ? C1 Fe1 C4 N1 79(4) . . . . ? C3 Fe1 C4 N1 -160.7(2) . . . . ? C2 Fe1 C4 N1 77.8(2) . . . . ? C8 Fe1 C4 N1 -39.4(2) . . . . ? C1 Fe1 C4 N2 -94(4) . . . . ? C3 Fe1 C4 N2 25.3(3) . . . . ? C2 Fe1 C4 N2 -96.2(3) . . . . ? C8 Fe1 C4 N2 146.7(2) . . . . ? C4 N1 C5 C6 -1.0(3) . . . . ? C7 N1 C5 C6 178.8(2) . . . . ? N1 C5 C6 N2 0.0(3) . . . . ? C4 N2 C6 C5 0.9(3) . . . . ? C11 N2 C6 C5 -173.8(2) . . . . ? C8 N3 C7 N1 -58.4(3) . . . . ? C10 N3 C7 N1 130.1(2) . . . . ? C4 N1 C7 N3 48.3(3) . . . . ? C5 N1 C7 N3 -131.5(2) . . . . ? C10 N3 C8 N4 1.2(3) . . . . ? C7 N3 C8 N4 -171.3(2) . . . . ? C10 N3 C8 Fe1 -175.11(17) . . . . ? C7 N3 C8 Fe1 12.4(3) . . . . ? C9 N4 C8 N3 -0.9(3) . . . . ? C23 N4 C8 N3 170.2(2) . . . . ? C9 N4 C8 Fe1 174.8(2) . . . . ? C23 N4 C8 Fe1 -14.1(4) . . . . ? C1 Fe1 C8 N3 -148.3(2) . . . . ? C3 Fe1 C8 N3 122.4(2) . . . . ? C2 Fe1 C8 N3 -55.8(2) . . . . ? C4 Fe1 C8 N3 30.3(2) . . . . ? C1 Fe1 C8 N4 36.8(3) . . . . ? C3 Fe1 C8 N4 -52.5(3) . . . . ? C2 Fe1 C8 N4 129.3(2) . . . . ? C4 Fe1 C8 N4 -144.6(3) . . . . ? C8 N4 C9 C10 0.3(3) . . . . ? C23 N4 C9 C10 -171.4(2) . . . . ? N4 C9 C10 N3 0.4(3) . . . . ? C8 N3 C10 C9 -1.1(3) . . . . ? C7 N3 C10 C9 170.9(2) . . . . ? C4 N2 C11 C16 80.2(3) . . . . ? C6 N2 C11 C16 -106.0(3) . . . . ? C4 N2 C11 C12 -102.4(3) . . . . ? C6 N2 C11 C12 71.4(3) . . . . ? C16 C11 C12 C13 -1.9(4) . . . . ? N2 C11 C12 C13 -179.2(2) . . . . ? C16 C11 C12 C17 179.6(2) . . . . ? N2 C11 C12 C17 2.3(4) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? C17 C12 C13 C14 178.9(2) . . . . ? C12 C13 C14 C15 0.9(4) . . . . ? C13 C14 C15 C16 -0.9(4) . . . . ? C12 C11 C16 C15 2.0(4) . . . . ? N2 C11 C16 C15 179.2(2) . . . . ? C12 C11 C16 C20 -174.8(2) . . . . ? N2 C11 C16 C20 2.5(4) . . . . ? C14 C15 C16 C11 -0.5(4) . . . . ? C14 C15 C16 C20 176.3(2) . . . . ? C13 C12 C17 C19 -99.7(3) . . . . ? C11 C12 C17 C19 78.7(3) . . . . ? C13 C12 C17 C18 24.4(4) . . . . ? C11 C12 C17 C18 -157.2(2) . . . . ? C11 C16 C20 C22 -137.7(3) . . . . ? C15 C16 C20 C22 45.7(3) . . . . ? C11 C16 C20 C21 98.1(3) . . . . ? C15 C16 C20 C21 -78.5(3) . . . . ? C8 N4 C23 C28 -91.9(3) . . . . ? C9 N4 C23 C28 78.5(3) . . . . ? C8 N4 C23 C24 90.8(3) . . . . ? C9 N4 C23 C24 -98.8(3) . . . . ? C28 C23 C24 C25 -2.0(4) . . . . ? N4 C23 C24 C25 175.1(2) . . . . ? C28 C23 C24 C29 178.9(2) . . . . ? N4 C23 C24 C29 -3.9(3) . . . . ? C23 C24 C25 C26 -0.9(4) . . . . ? C29 C24 C25 C26 178.2(2) . . . . ? C24 C25 C26 C27 2.4(4) . . . . ? C25 C26 C27 C28 -1.0(4) . . . . ? C26 C27 C28 C23 -1.8(4) . . . . ? C26 C27 C28 C32 179.5(2) . . . . ? C24 C23 C28 C27 3.3(4) . . . . ? N4 C23 C28 C27 -173.8(2) . . . . ? C24 C23 C28 C32 -178.0(2) . . . . ? N4 C23 C28 C32 4.9(3) . . . . ? C25 C24 C29 C30 28.8(3) . . . . ? C23 C24 C29 C30 -152.2(2) . . . . ? C25 C24 C29 C31 -95.3(3) . . . . ? C23 C24 C29 C31 83.7(3) . . . . ? C27 C28 C32 C33 74.3(3) . . . . ? C23 C28 C32 C33 -104.3(3) . . . . ? C27 C28 C32 C34 -49.3(3) . . . . ? C23 C28 C32 C34 132.1(3) . . . . ? C55 C50A C51A C52 0.0 . . . . ? C50A C51A C52 C53 0.0 . . . . ? C51A C52 C53 C54 0.0 . . . . ? C51A C52 C53 C54 126.9(8) . . . 3_666 ? C52 C53 C54 C55 0.0 . . . . ? C54 C53 C54 C55 -134.0(8) 3_666 . . . ? C52 C53 C54 C53 134.0(8) . . . 3_666 ? C54 C53 C54 C53 0.0(3) 3_666 . . 3_666 ? C53 C54 C55 C50A 0.0 . . . . ? C53 C54 C55 C50A -102.2(10) 3_666 . . . ? C51A C50A C55 C54 0.0 . . . . ? C59 C50B C51B C56 0.0 . . . . ? C50B C51B C56 C57 0.0 . . . . ? C51B C56 C57 C58 0.0 . . . . ? C51B C56 C57 C58 13(2) . . . 3_566 ? C56 C57 C58 C58 174.6(10) . . . 3_566 ? C56 C57 C58 C59 0.0 . . . . ? C58 C57 C58 C59 -174.6(10) 3_566 . . . ? C56 C57 C58 C57 174.6(12) . . . 3_566 ? C58 C57 C58 C57 0.0(5) 3_566 . . 3_566 ? C58 C58 C59 C50B -168(2) 3_566 . . . ? C57 C58 C59 C50B 0.0 . . . . ? C57 C58 C59 C50B -176.2(8) 3_566 . . . ? C51B C50B C59 C58 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.413 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.059 #===END data_c:\workdo~1\crystals\omji94~1\fromch~1\omji94 _database_code_depnum_ccdc_archive 'CCDC 851126' #TrackingRef '- final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H62 B Fe N4' _chemical_formula_sum 'C44 H62 B Fe N4' _chemical_formula_weight 713.64 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.8336(9) _cell_length_b 16.747(2) _cell_length_c 25.057(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4126.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6136 _cell_measurement_theta_min 2.9282 _cell_measurement_theta_max 28.5296 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 0.399 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7406 _exptl_absorpt_correction_T_max 0.9803 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_reflns_number 26707 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0845 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7246 _reflns_number_gt 5018 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+2.7180P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_number_reflns 7246 _refine_ls_number_parameters 483 _refine_ls_number_restraints 327 _refine_ls_R_factor_all 0.1120 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.2013 _refine_ls_wR_factor_gt 0.1743 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 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 0.40795(8) 0.03417(5) 0.98289(3) 0.0431(3) Uani 1 1 d . . . B1 B 0.1740(14) -0.2329(5) 0.8787(3) 0.086(3) Uani 1 1 d . . . N1 N 0.2915(6) -0.1067(3) 0.93020(17) 0.0451(13) Uani 1 1 d . . . N2 N 0.2893(4) -0.0124(2) 0.87285(16) 0.0314(10) Uani 1 1 d . . . N3 N 0.2827(6) -0.1090(3) 1.02523(18) 0.0554(15) Uani 1 1 d . . . N4 N 0.2560(5) -0.0206(3) 1.08494(17) 0.0434(12) Uani 1 1 d . . . C1 C 0.3270(5) -0.0276(3) 0.92421(18) 0.0333(12) Uani 1 1 d . . . C2 C 0.2324(8) -0.1412(3) 0.8847(2) 0.0503(16) Uani 1 1 d U . . C3 C 0.2331(7) -0.0798(3) 0.8499(2) 0.0425(14) Uani 1 1 d U . . H3 H 0.1994 -0.0826 0.8144 0.051 Uiso 1 1 calc R . . C4 C 0.3261(9) -0.1498(3) 0.9781(2) 0.063(2) Uani 1 1 d . . . H4A H 0.2832 -0.2033 0.9769 0.076 Uiso 1 1 calc R . . H4B H 0.4259 -0.1574 0.9795 0.076 Uiso 1 1 calc R . . C5 C 0.3079(6) -0.0312(4) 1.03515(18) 0.0375(13) Uani 1 1 d . . . C6 C 0.2173(11) -0.1461(4) 1.0668(3) 0.087(3) Uani 1 1 d U . . H6 H 0.1881 -0.2001 1.0682 0.104 Uiso 1 1 calc R . . C7 C 0.2032(10) -0.0920(4) 1.1042(3) 0.074(2) Uani 1 1 d U . . H7 H 0.1639 -0.1001 1.1384 0.089 Uiso 1 1 calc R . . C8 C 0.3169(7) 0.0587(3) 0.8419(2) 0.0442(13) Uani 1 1 d U . . C9 C 0.4309(8) 0.0540(4) 0.8061(2) 0.0622(15) Uani 1 1 d U . . C10 C 0.4533(10) 0.1224(6) 0.7746(3) 0.086(2) Uani 1 1 d U . . H10 H 0.5261 0.1231 0.7497 0.103 Uiso 1 1 calc R . . C11 C 0.3754(11) 0.1846(5) 0.7793(3) 0.087(2) Uani 1 1 d U . . H11 H 0.3975 0.2300 0.7582 0.105 Uiso 1 1 calc R . . C12 C 0.2633(11) 0.1908(4) 0.8122(3) 0.079(2) Uani 1 1 d U . . H12 H 0.2084 0.2375 0.8125 0.095 Uiso 1 1 calc R . . C13 C 0.2326(9) 0.1231(4) 0.8462(2) 0.0596(15) Uani 1 1 d U . . C14 C 0.5183(8) -0.0188(6) 0.7999(3) 0.0787(19) Uani 1 1 d U . . H14 H 0.5030 -0.0556 0.8307 0.094 Uiso 1 1 calc R . . C15 C 0.6699(8) 0.0057(9) 0.7979(3) 0.129(4) Uani 1 1 d U . . H15A H 0.6959 0.0169 0.7609 0.194 Uiso 1 1 calc R . . H15B H 0.7260 -0.0379 0.8118 0.194 Uiso 1 1 calc R . . H15C H 0.6837 0.0536 0.8196 0.194 Uiso 1 1 calc R . . C16 C 0.4798(10) -0.0604(7) 0.7488(3) 0.105(3) Uani 1 1 d U . . H16A H 0.3824 -0.0728 0.7493 0.157 Uiso 1 1 calc R . . H16B H 0.5320 -0.1101 0.7455 0.157 Uiso 1 1 calc R . . H16C H 0.5000 -0.0255 0.7184 0.157 Uiso 1 1 calc R . . C17 C 0.1119(9) 0.1233(4) 0.8829(3) 0.0751(19) Uani 1 1 d U . . H17 H 0.1355 0.0911 0.9152 0.090 Uiso 1 1 calc R . . C18 C 0.0782(13) 0.2100(5) 0.9014(4) 0.129(4) Uani 1 1 d U . . H18A H 0.0694 0.2447 0.8701 0.194 Uiso 1 1 calc R . . H18B H 0.1515 0.2299 0.9243 0.194 Uiso 1 1 calc R . . H18C H -0.0075 0.2099 0.9213 0.194 Uiso 1 1 calc R . . C19 C -0.0124(10) 0.0863(6) 0.8572(4) 0.107(3) Uani 1 1 d U . . H19A H -0.0266 0.1100 0.8219 0.160 Uiso 1 1 calc R . . H19B H -0.0923 0.0963 0.8796 0.160 Uiso 1 1 calc R . . H19C H 0.0013 0.0286 0.8535 0.160 Uiso 1 1 calc R . . C20 C 0.2504(6) 0.0531(3) 1.1154(2) 0.0408(13) Uani 1 1 d U . . C21 C 0.1445(7) 0.1062(4) 1.1069(2) 0.0531(14) Uani 1 1 d U B . C22 C 0.1475(9) 0.1775(5) 1.1363(3) 0.0703(18) Uani 1 1 d U . . H22 H 0.0800 0.2170 1.1302 0.084 Uiso 1 1 calc R . . C23 C 0.2459(9) 0.1906(4) 1.1733(3) 0.0676(18) Uani 1 1 d U . . H23 H 0.2471 0.2395 1.1925 0.081 Uiso 1 1 calc R . . C24 C 0.3429(7) 0.1346(4) 1.1831(2) 0.0545(15) Uani 1 1 d U . . H24 H 0.4083 0.1444 1.2103 0.065 Uiso 1 1 calc R . . C25 C 0.3491(6) 0.0642(4) 1.1550(2) 0.0445(13) Uani 1 1 d U . . C26 C 0.0300(8) 0.0846(5) 1.0690(3) 0.0781(19) Uani 1 1 d U . . H26 H 0.0747 0.0556 1.0389 0.094 Uiso 1 1 calc R A 1 C27A C 0.042(2) 0.1379(11) 1.0186(7) 0.091(4) Uani 0.50 1 d PU B 2 H27A H -0.0393 0.1313 0.9965 0.136 Uiso 0.50 1 calc PR B 2 H27B H 0.1227 0.1222 0.9982 0.136 Uiso 0.50 1 calc PR B 2 H27C H 0.0504 0.1940 1.0294 0.136 Uiso 0.50 1 calc PR B 2 C28A C -0.1051(16) 0.1204(12) 1.0979(7) 0.084(4) Uani 0.50 1 d PU B 2 H28A H -0.0931 0.1778 1.1042 0.125 Uiso 0.50 1 calc PR B 2 H28B H -0.1193 0.0932 1.1321 0.125 Uiso 0.50 1 calc PR B 2 H28C H -0.1844 0.1119 1.0749 0.125 Uiso 0.50 1 calc PR B 2 C28B C -0.0734(15) 0.0213(12) 1.0950(7) 0.090(4) Uani 0.50 1 d PU B 1 H28D H -0.1247 0.0470 1.1238 0.135 Uiso 0.50 1 calc PR B 1 H28E H -0.0220 -0.0239 1.1094 0.135 Uiso 0.50 1 calc PR B 1 H28F H -0.1366 0.0022 1.0676 0.135 Uiso 0.50 1 calc PR B 1 C27B C -0.0562(18) 0.1389(11) 1.0451(8) 0.093(4) Uani 0.50 1 d PU B 1 H27D H -0.0030 0.1834 1.0307 0.139 Uiso 0.50 1 calc PR B 1 H27E H -0.1210 0.1592 1.0716 0.139 Uiso 0.50 1 calc PR B 1 H27F H -0.1060 0.1127 1.0161 0.139 Uiso 0.50 1 calc PR B 1 C29 C 0.4551(7) 0.0020(5) 1.1673(2) 0.0633(18) Uani 1 1 d U . . H29 H 0.4637 -0.0343 1.1358 0.076 Uiso 1 1 calc R . . C30 C 0.5974(8) 0.0410(7) 1.1784(3) 0.109(3) Uani 1 1 d U . . H30A H 0.6178 0.0801 1.1504 0.164 Uiso 1 1 calc R . . H30B H 0.6676 -0.0005 1.1785 0.164 Uiso 1 1 calc R . . H30C H 0.5958 0.0678 1.2131 0.164 Uiso 1 1 calc R . . C31 C 0.4077(11) -0.0474(5) 1.2154(3) 0.096(3) Uani 1 1 d U . . H31A H 0.3989 -0.0126 1.2466 0.144 Uiso 1 1 calc R . . H31B H 0.4745 -0.0894 1.2229 0.144 Uiso 1 1 calc R . . H31C H 0.3195 -0.0719 1.2074 0.144 Uiso 1 1 calc R . . C32 C 0.6226(7) 0.0315(7) 0.9766(4) 0.099(2) Uani 1 1 d U . . C33 C 0.5837(9) 0.0530(7) 1.0285(3) 0.097(2) Uani 1 1 d U . . H33 H 0.6196 0.0243 1.0580 0.117 Uiso 1 1 calc R . . C34 C 0.4928(10) 0.1163(6) 1.0378(3) 0.086(2) Uani 1 1 d U . . H34 H 0.4721 0.1308 1.0736 0.103 Uiso 1 1 calc R . . C35 C 0.4322(10) 0.1584(5) 0.9964(3) 0.087(2) Uani 1 1 d U . . H35 H 0.3661 0.1986 1.0031 0.104 Uiso 1 1 calc R . . C36 C 0.4718(9) 0.1396(5) 0.9454(3) 0.076(2) Uani 1 1 d U . . H36 H 0.4344 0.1686 0.9164 0.091 Uiso 1 1 calc R . . C37 C 0.5646(8) 0.0794(6) 0.9352(3) 0.083(2) Uani 1 1 d U . . H37 H 0.5909 0.0695 0.8993 0.100 Uiso 1 1 calc R . . C38 C 0.7119(12) -0.0431(9) 0.9670(6) 0.170(5) Uani 1 1 d U . . H38A H 0.7165 -0.0748 0.9998 0.255 Uiso 1 1 calc R . . H38B H 0.8037 -0.0264 0.9567 0.255 Uiso 1 1 calc R . . H38C H 0.6721 -0.0755 0.9384 0.255 Uiso 1 1 calc R . . C39 C 0.0651(12) -0.2560(4) 0.9260(3) 0.099(3) Uani 1 1 d U . . H39A H 0.0081 -0.3007 0.9130 0.118 Uiso 1 1 calc R . . H39B H 0.1170 -0.2758 0.9572 0.118 Uiso 1 1 calc R . . C40 C -0.0344(11) -0.1855(5) 0.9460(4) 0.100(3) Uani 1 1 d U . . H40A H 0.0202 -0.1406 0.9591 0.150 Uiso 1 1 calc R . . H40B H -0.0926 -0.2054 0.9748 0.150 Uiso 1 1 calc R . . H40C H -0.0911 -0.1675 0.9162 0.150 Uiso 1 1 calc R . . C41 C 0.3036(13) -0.2923(5) 0.8833(3) 0.113(4) Uani 1 1 d U . . H41A H 0.3402 -0.2896 0.9200 0.135 Uiso 1 1 calc R . . H41B H 0.2729 -0.3478 0.8769 0.135 Uiso 1 1 calc R . . C42 C 0.4128(14) -0.2732(8) 0.8455(5) 0.158(5) Uani 1 1 d U . . H42A H 0.3735 -0.2624 0.8103 0.237 Uiso 1 1 calc R . . H42B H 0.4756 -0.3184 0.8430 0.237 Uiso 1 1 calc R . . H42C H 0.4621 -0.2259 0.8580 0.237 Uiso 1 1 calc R . . C43 C 0.1018(12) -0.2413(4) 0.8195(3) 0.093(3) Uani 1 1 d U . . H43A H 0.1641 -0.2167 0.7931 0.111 Uiso 1 1 calc R . . H43B H 0.0969 -0.2989 0.8109 0.111 Uiso 1 1 calc R . . C44 C -0.0352(12) -0.2072(6) 0.8101(4) 0.118(4) Uani 1 1 d U . . H44A H -0.1010 -0.2333 0.8338 0.177 Uiso 1 1 calc R . . H44B H -0.0616 -0.2159 0.7729 0.177 Uiso 1 1 calc R . . H44C H -0.0336 -0.1497 0.8176 0.177 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0485(4) 0.0599(5) 0.0210(3) 0.0005(4) -0.0036(4) -0.0128(5) B1 0.175(11) 0.034(4) 0.049(5) 0.004(4) -0.003(6) -0.019(6) N1 0.079(4) 0.030(2) 0.027(2) 0.0070(19) -0.009(2) 0.008(3) N2 0.040(2) 0.034(2) 0.020(2) 0.0010(17) -0.0050(19) -0.003(2) N3 0.103(4) 0.039(3) 0.024(3) 0.010(2) -0.008(3) 0.001(3) N4 0.054(3) 0.052(3) 0.024(2) 0.001(2) 0.000(2) -0.006(3) C1 0.036(3) 0.041(3) 0.022(2) 0.003(2) -0.004(2) 0.006(3) C2 0.087(4) 0.036(3) 0.027(3) -0.001(2) -0.001(3) 0.000(3) C3 0.064(4) 0.034(3) 0.030(3) -0.005(2) -0.008(3) -0.008(3) C4 0.126(6) 0.036(3) 0.027(3) 0.004(3) -0.005(4) 0.017(4) C5 0.048(3) 0.045(3) 0.020(2) 0.003(2) -0.008(2) -0.001(3) C6 0.171(8) 0.057(4) 0.033(3) 0.009(3) 0.006(4) -0.043(5) C7 0.140(7) 0.050(4) 0.032(3) 0.006(3) 0.020(4) -0.037(4) C8 0.065(3) 0.041(3) 0.026(3) 0.005(2) -0.014(2) -0.010(3) C9 0.077(4) 0.084(4) 0.026(3) 0.008(3) -0.008(3) -0.032(3) C10 0.111(6) 0.098(5) 0.047(4) 0.006(4) 0.000(4) -0.041(4) C11 0.137(6) 0.068(4) 0.057(4) 0.003(4) -0.017(4) -0.035(4) C12 0.133(6) 0.046(3) 0.059(4) -0.005(3) -0.031(4) 0.000(4) C13 0.106(4) 0.038(3) 0.035(3) -0.005(2) -0.029(3) 0.007(3) C14 0.058(4) 0.137(5) 0.041(3) -0.006(4) 0.001(3) -0.005(4) C15 0.057(4) 0.281(13) 0.050(4) -0.017(6) 0.009(4) -0.007(6) C16 0.095(6) 0.167(9) 0.053(4) -0.036(5) -0.012(4) 0.025(6) C17 0.107(5) 0.059(4) 0.059(4) -0.019(3) -0.025(3) 0.035(4) C18 0.199(10) 0.101(6) 0.087(6) -0.035(5) -0.015(7) 0.086(7) C19 0.083(5) 0.156(8) 0.082(6) -0.039(6) -0.006(5) 0.048(5) C20 0.040(3) 0.056(3) 0.026(2) 0.000(2) 0.005(2) -0.004(3) C21 0.054(3) 0.068(3) 0.037(3) 0.008(3) 0.005(3) 0.012(3) C22 0.091(5) 0.070(4) 0.050(4) 0.009(3) 0.004(3) 0.035(4) C23 0.106(5) 0.061(4) 0.036(3) -0.001(3) 0.006(3) 0.006(4) C24 0.068(4) 0.065(4) 0.030(3) -0.004(3) 0.002(3) -0.011(3) C25 0.046(3) 0.067(3) 0.021(2) 0.003(2) 0.006(2) 0.000(3) C26 0.056(4) 0.123(5) 0.056(4) 0.022(4) -0.002(3) 0.013(4) C27A 0.110(10) 0.110(10) 0.052(7) 0.009(7) -0.009(7) 0.013(9) C28A 0.051(6) 0.130(10) 0.070(7) 0.005(8) -0.010(6) 0.004(8) C28B 0.054(7) 0.139(10) 0.076(8) 0.023(8) -0.029(7) -0.015(7) C27B 0.076(9) 0.114(9) 0.088(9) 0.013(8) -0.018(7) 0.029(8) C29 0.062(4) 0.110(5) 0.018(2) -0.003(3) 0.002(3) 0.035(3) C30 0.054(4) 0.237(10) 0.037(3) -0.031(5) -0.011(3) 0.031(6) C31 0.133(7) 0.112(6) 0.042(4) 0.018(4) 0.020(5) 0.066(6) C32 0.050(4) 0.168(6) 0.079(4) 0.000(5) -0.009(3) -0.019(4) C33 0.074(4) 0.169(6) 0.050(4) 0.018(4) -0.029(4) -0.047(4) C34 0.098(5) 0.125(6) 0.035(3) -0.019(3) 0.006(3) -0.082(4) C35 0.109(5) 0.090(5) 0.062(4) -0.016(3) 0.011(4) -0.053(4) C36 0.091(5) 0.094(5) 0.043(3) 0.004(3) -0.008(4) -0.054(4) C37 0.064(4) 0.151(6) 0.033(3) -0.011(4) 0.005(3) -0.050(4) C38 0.092(7) 0.255(12) 0.163(10) -0.006(9) 0.000(7) 0.042(8) C39 0.183(10) 0.048(4) 0.064(5) 0.016(4) -0.007(6) -0.033(5) C40 0.152(9) 0.067(5) 0.080(6) 0.013(4) 0.013(6) -0.027(5) C41 0.216(12) 0.078(5) 0.044(4) -0.011(4) -0.008(6) 0.036(7) C42 0.189(12) 0.167(10) 0.118(9) -0.010(8) 0.027(8) 0.082(10) C43 0.177(9) 0.049(4) 0.052(4) -0.002(3) -0.010(6) -0.042(6) C44 0.155(9) 0.126(8) 0.072(6) 0.021(6) -0.026(6) -0.058(7) _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 C1 1.966(5) . ? Fe1 C5 1.970(5) . ? Fe1 C37 2.092(7) . ? Fe1 C36 2.095(7) . ? Fe1 C33 2.097(7) . ? Fe1 C34 2.117(7) . ? Fe1 C32 2.117(7) . ? Fe1 C35 2.122(8) . ? B1 C41 1.620(16) . ? B1 C39 1.643(14) . ? B1 C2 1.647(10) . ? B1 C43 1.652(12) . ? N1 C1 1.378(7) . ? N1 C2 1.403(7) . ? N1 C4 1.440(7) . ? N2 C1 1.363(6) . ? N2 C3 1.382(7) . ? N2 C8 1.448(7) . ? N3 C5 1.349(8) . ? N3 C6 1.373(8) . ? N3 C4 1.430(7) . ? N4 C5 1.360(6) . ? N4 C7 1.390(8) . ? N4 C20 1.452(7) . ? C2 C3 1.347(8) . ? C3 H3 0.9500 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C6 C7 1.310(9) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.364(9) . ? C8 C9 1.438(10) . ? C9 C10 1.408(10) . ? C9 C14 1.500(11) . ? C10 C11 1.299(12) . ? C10 H10 0.9500 . ? C11 C12 1.379(13) . ? C11 H11 0.9500 . ? C12 C13 1.450(10) . ? C12 H12 0.9500 . ? C13 C17 1.502(11) . ? C14 C16 1.505(10) . ? C14 C15 1.547(11) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.514(12) . ? C17 C18 1.559(10) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.385(8) . ? C20 C25 1.400(8) . ? C21 C22 1.402(10) . ? C21 C26 1.517(10) . ? C22 C23 1.358(10) . ? C22 H22 0.9500 . ? C23 C24 1.361(10) . ? C23 H23 0.9500 . ? C24 C25 1.375(9) . ? C24 H24 0.9500 . ? C25 C29 1.506(9) . ? C26 C27B 1.380(17) . ? C26 C27A 1.551(18) . ? C26 C28B 1.607(18) . ? C26 C28A 1.628(18) . ? C26 H26 1.0000 . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? C29 C31 1.535(10) . ? C29 C30 1.569(11) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.404(12) . ? C32 C37 1.429(13) . ? C32 C38 1.547(15) . ? C33 C34 1.407(13) . ? C33 H33 0.9500 . ? C34 C35 1.388(12) . ? C34 H34 0.9500 . ? C35 C36 1.372(10) . ? C35 H35 0.9500 . ? C36 C37 1.384(12) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.614(12) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.466(16) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.481(14) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 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 C1 Fe1 C5 90.1(2) . . ? C1 Fe1 C37 93.5(2) . . ? C5 Fe1 C37 161.6(3) . . ? C1 Fe1 C36 103.3(2) . . ? C5 Fe1 C36 156.3(3) . . ? C37 Fe1 C36 38.6(3) . . ? C1 Fe1 C33 145.2(4) . . ? C5 Fe1 C33 97.6(3) . . ? C37 Fe1 C33 69.5(3) . . ? C36 Fe1 C33 82.6(3) . . ? C1 Fe1 C34 170.9(3) . . ? C5 Fe1 C34 97.3(3) . . ? C37 Fe1 C34 81.1(3) . . ? C36 Fe1 C34 68.0(3) . . ? C33 Fe1 C34 39.0(4) . . ? C1 Fe1 C32 109.7(3) . . ? C5 Fe1 C32 122.4(3) . . ? C37 Fe1 C32 39.7(4) . . ? C36 Fe1 C32 71.7(4) . . ? C33 Fe1 C32 38.9(3) . . ? C34 Fe1 C32 70.7(4) . . ? C1 Fe1 C35 132.9(3) . . ? C5 Fe1 C35 119.7(3) . . ? C37 Fe1 C35 69.7(3) . . ? C36 Fe1 C35 38.0(3) . . ? C33 Fe1 C35 70.9(4) . . ? C34 Fe1 C35 38.2(3) . . ? C32 Fe1 C35 85.5(4) . . ? C41 B1 C39 108.5(7) . . ? C41 B1 C2 107.0(9) . . ? C39 B1 C2 112.4(6) . . ? C41 B1 C43 110.5(7) . . ? C39 B1 C43 110.3(9) . . ? C2 B1 C43 108.1(6) . . ? C1 N1 C2 114.3(4) . . ? C1 N1 C4 120.9(5) . . ? C2 N1 C4 124.5(5) . . ? C1 N2 C3 110.4(4) . . ? C1 N2 C8 127.5(4) . . ? C3 N2 C8 121.6(4) . . ? C5 N3 C6 112.5(5) . . ? C5 N3 C4 123.9(5) . . ? C6 N3 C4 123.5(5) . . ? C5 N4 C7 110.2(5) . . ? C5 N4 C20 127.5(5) . . ? C7 N4 C20 122.3(5) . . ? N2 C1 N1 102.3(4) . . ? N2 C1 Fe1 135.9(4) . . ? N1 C1 Fe1 121.8(3) . . ? C3 C2 N1 102.1(5) . . ? C3 C2 B1 130.8(6) . . ? N1 C2 B1 127.1(5) . . ? C2 C3 N2 110.8(5) . . ? C2 C3 H3 124.6 . . ? N2 C3 H3 124.6 . . ? N3 C4 N1 112.2(5) . . ? N3 C4 H4A 109.2 . . ? N1 C4 H4A 109.2 . . ? N3 C4 H4B 109.2 . . ? N1 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N3 C5 N4 103.1(5) . . ? N3 C5 Fe1 120.4(4) . . ? N4 C5 Fe1 136.4(5) . . ? C7 C6 N3 106.2(6) . . ? C7 C6 H6 126.9 . . ? N3 C6 H6 126.9 . . ? C6 C7 N4 107.9(6) . . ? C6 C7 H7 126.0 . . ? N4 C7 H7 126.0 . . ? C13 C8 C9 124.5(6) . . ? C13 C8 N2 119.6(6) . . ? C9 C8 N2 115.8(5) . . ? C10 C9 C8 115.2(8) . . ? C10 C9 C14 120.9(7) . . ? C8 C9 C14 123.8(6) . . ? C11 C10 C9 120.7(9) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 125.8(8) . . ? C10 C11 H11 117.1 . . ? C12 C11 H11 117.1 . . ? C11 C12 C13 117.3(8) . . ? C11 C12 H12 121.3 . . ? C13 C12 H12 121.3 . . ? C8 C13 C12 116.4(8) . . ? C8 C13 C17 122.1(6) . . ? C12 C13 C17 121.5(7) . . ? C9 C14 C16 108.7(7) . . ? C9 C14 C15 109.9(9) . . ? C16 C14 C15 109.7(7) . . ? C9 C14 H14 109.5 . . ? C16 C14 H14 109.5 . . ? C15 C14 H14 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 C19 112.1(6) . . ? C13 C17 C18 110.6(8) . . ? C19 C17 C18 109.6(8) . . ? C13 C17 H17 108.1 . . ? C19 C17 H17 108.1 . . ? C18 C17 H17 108.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 123.0(6) . . ? C21 C20 N4 119.6(5) . . ? C25 C20 N4 117.3(5) . . ? C20 C21 C22 116.8(6) . . ? C20 C21 C26 120.1(7) . . ? C22 C21 C26 123.1(7) . . ? C23 C22 C21 120.7(7) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.8(7) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C25 121.9(7) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C24 C25 C20 116.5(6) . . ? C24 C25 C29 121.2(6) . . ? C20 C25 C29 122.3(6) . . ? C27B C26 C21 124.8(11) . . ? C27B C26 C27A 46.7(10) . . ? C21 C26 C27A 108.4(9) . . ? C27B C26 C28B 102.8(11) . . ? C21 C26 C28B 112.0(7) . . ? C27A C26 C28B 139.3(11) . . ? C27B C26 C28A 56.6(10) . . ? C21 C26 C28A 103.9(8) . . ? C27A C26 C28A 102.3(11) . . ? C28B C26 C28A 63.0(9) . . ? C27B C26 H26 105.2 . . ? C21 C26 H26 105.2 . . ? C27A C26 H26 68.4 . . ? C28B C26 H26 105.2 . . ? C28A C26 H26 150.9 . . ? C26 C27A H27A 109.5 . . ? C26 C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C26 C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C26 C28A H28A 109.5 . . ? C26 C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C26 C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C26 C28B H28D 109.5 . . ? C26 C28B H28E 109.5 . . ? C26 C28B H28F 109.5 . . ? C26 C27B H27D 109.5 . . ? C26 C27B H27E 109.5 . . ? C26 C27B H27F 109.5 . . ? C25 C29 C31 108.9(5) . . ? C25 C29 C30 111.5(7) . . ? C31 C29 C30 110.9(6) . . ? C25 C29 H29 108.5 . . ? C31 C29 H29 108.5 . . ? C30 C29 H29 108.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 114.9(9) . . ? C33 C32 C38 120.4(10) . . ? C37 C32 C38 124.6(9) . . ? C33 C32 Fe1 69.8(5) . . ? C37 C32 Fe1 69.2(4) . . ? C38 C32 Fe1 126.5(7) . . ? C32 C33 C34 121.3(8) . . ? C32 C33 Fe1 71.3(4) . . ? C34 C33 Fe1 71.3(5) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? Fe1 C33 H33 130.9 . . ? C35 C34 C33 122.2(7) . . ? C35 C34 Fe1 71.1(4) . . ? C33 C34 Fe1 69.7(4) . . ? C35 C34 H34 118.9 . . ? C33 C34 H34 118.9 . . ? Fe1 C34 H34 134.0 . . ? C36 C35 C34 117.2(9) . . ? C36 C35 Fe1 70.0(5) . . ? C34 C35 Fe1 70.7(5) . . ? C36 C35 H35 121.4 . . ? C34 C35 H35 121.4 . . ? Fe1 C35 H35 130.2 . . ? C35 C36 C37 121.8(9) . . ? C35 C36 Fe1 72.1(5) . . ? C37 C36 Fe1 70.6(5) . . ? C35 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? Fe1 C36 H36 131.2 . . ? C36 C37 C32 122.5(7) . . ? C36 C37 Fe1 70.8(4) . . ? C32 C37 Fe1 71.1(4) . . ? C36 C37 H37 118.7 . . ? C32 C37 H37 118.8 . . ? Fe1 C37 H37 132.7 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 B1 116.5(6) . . ? C40 C39 H39A 108.2 . . ? B1 C39 H39A 108.2 . . ? C40 C39 H39B 108.2 . . ? B1 C39 H39B 108.2 . . ? H39A C39 H39B 107.3 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 B1 113.3(8) . . ? C42 C41 H41A 108.9 . . ? B1 C41 H41A 108.9 . . ? C42 C41 H41B 108.9 . . ? B1 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 B1 120.1(9) . . ? C44 C43 H43A 107.3 . . ? B1 C43 H43A 107.3 . . ? C44 C43 H43B 107.3 . . ? B1 C43 H43B 107.3 . . ? H43A C43 H43B 106.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N2 C1 N1 0.4(6) . . . . ? C8 N2 C1 N1 -171.8(5) . . . . ? C3 N2 C1 Fe1 -178.4(5) . . . . ? C8 N2 C1 Fe1 9.4(9) . . . . ? C2 N1 C1 N2 -0.4(6) . . . . ? C4 N1 C1 N2 174.0(6) . . . . ? C2 N1 C1 Fe1 178.7(4) . . . . ? C4 N1 C1 Fe1 -6.9(8) . . . . ? C5 Fe1 C1 N2 148.5(6) . . . . ? C37 Fe1 C1 N2 -49.6(6) . . . . ? C36 Fe1 C1 N2 -11.8(6) . . . . ? C33 Fe1 C1 N2 -107.9(7) . . . . ? C34 Fe1 C1 N2 4(2) . . . . ? C32 Fe1 C1 N2 -86.8(6) . . . . ? C35 Fe1 C1 N2 15.8(7) . . . . ? C5 Fe1 C1 N1 -30.2(4) . . . . ? C37 Fe1 C1 N1 131.7(5) . . . . ? C36 Fe1 C1 N1 169.5(5) . . . . ? C33 Fe1 C1 N1 73.5(7) . . . . ? C34 Fe1 C1 N1 -174.8(19) . . . . ? C32 Fe1 C1 N1 94.5(5) . . . . ? C35 Fe1 C1 N1 -162.9(5) . . . . ? C1 N1 C2 C3 0.2(7) . . . . ? C4 N1 C2 C3 -174.0(6) . . . . ? C1 N1 C2 B1 -177.9(8) . . . . ? C4 N1 C2 B1 7.9(12) . . . . ? C41 B1 C2 C3 116.1(9) . . . . ? C39 B1 C2 C3 -124.9(9) . . . . ? C43 B1 C2 C3 -2.9(14) . . . . ? C41 B1 C2 N1 -66.3(10) . . . . ? C39 B1 C2 N1 52.7(12) . . . . ? C43 B1 C2 N1 174.7(7) . . . . ? N1 C2 C3 N2 0.1(7) . . . . ? B1 C2 C3 N2 178.1(8) . . . . ? C1 N2 C3 C2 -0.3(7) . . . . ? C8 N2 C3 C2 172.4(6) . . . . ? C5 N3 C4 N1 -49.5(9) . . . . ? C6 N3 C4 N1 134.3(8) . . . . ? C1 N1 C4 N3 52.2(9) . . . . ? C2 N1 C4 N3 -134.0(7) . . . . ? C6 N3 C5 N4 0.2(8) . . . . ? C4 N3 C5 N4 -176.4(6) . . . . ? C6 N3 C5 Fe1 177.4(6) . . . . ? C4 N3 C5 Fe1 0.8(8) . . . . ? C7 N4 C5 N3 1.0(7) . . . . ? C20 N4 C5 N3 -177.6(5) . . . . ? C7 N4 C5 Fe1 -175.4(6) . . . . ? C20 N4 C5 Fe1 5.9(9) . . . . ? C1 Fe1 C5 N3 33.2(5) . . . . ? C37 Fe1 C5 N3 -68.4(10) . . . . ? C36 Fe1 C5 N3 158.4(6) . . . . ? C33 Fe1 C5 N3 -112.7(5) . . . . ? C34 Fe1 C5 N3 -152.0(6) . . . . ? C32 Fe1 C5 N3 -80.3(6) . . . . ? C35 Fe1 C5 N3 175.0(5) . . . . ? C1 Fe1 C5 N4 -150.7(6) . . . . ? C37 Fe1 C5 N4 107.6(10) . . . . ? C36 Fe1 C5 N4 -25.6(10) . . . . ? C33 Fe1 C5 N4 63.3(7) . . . . ? C34 Fe1 C5 N4 24.0(7) . . . . ? C32 Fe1 C5 N4 95.7(7) . . . . ? C35 Fe1 C5 N4 -9.0(7) . . . . ? C5 N3 C6 C7 -1.4(10) . . . . ? C4 N3 C6 C7 175.2(8) . . . . ? N3 C6 C7 N4 2.0(11) . . . . ? C5 N4 C7 C6 -2.0(10) . . . . ? C20 N4 C7 C6 176.8(7) . . . . ? C1 N2 C8 C13 -84.8(7) . . . . ? C3 N2 C8 C13 103.8(6) . . . . ? C1 N2 C8 C9 98.1(6) . . . . ? C3 N2 C8 C9 -73.3(7) . . . . ? C13 C8 C9 C10 0.6(9) . . . . ? N2 C8 C9 C10 177.5(5) . . . . ? C13 C8 C9 C14 -176.8(6) . . . . ? N2 C8 C9 C14 0.2(8) . . . . ? C8 C9 C10 C11 1.0(11) . . . . ? C14 C9 C10 C11 178.4(7) . . . . ? C9 C10 C11 C12 -2.7(14) . . . . ? C10 C11 C12 C13 2.7(13) . . . . ? C9 C8 C13 C12 -0.6(9) . . . . ? N2 C8 C13 C12 -177.4(5) . . . . ? C9 C8 C13 C17 177.8(6) . . . . ? N2 C8 C13 C17 0.9(9) . . . . ? C11 C12 C13 C8 -0.9(10) . . . . ? C11 C12 C13 C17 -179.3(7) . . . . ? C10 C9 C14 C16 -73.9(9) . . . . ? C8 C9 C14 C16 103.3(8) . . . . ? C10 C9 C14 C15 46.1(9) . . . . ? C8 C9 C14 C15 -136.6(7) . . . . ? C8 C13 C17 C19 -85.2(8) . . . . ? C12 C13 C17 C19 93.1(8) . . . . ? C8 C13 C17 C18 152.2(7) . . . . ? C12 C13 C17 C18 -29.6(9) . . . . ? C5 N4 C20 C21 83.8(7) . . . . ? C7 N4 C20 C21 -94.7(8) . . . . ? C5 N4 C20 C25 -100.5(6) . . . . ? C7 N4 C20 C25 81.0(8) . . . . ? C25 C20 C21 C22 6.7(9) . . . . ? N4 C20 C21 C22 -177.9(6) . . . . ? C25 C20 C21 C26 -171.1(6) . . . . ? N4 C20 C21 C26 4.4(8) . . . . ? C20 C21 C22 C23 -3.7(10) . . . . ? C26 C21 C22 C23 173.9(7) . . . . ? C21 C22 C23 C24 -0.8(11) . . . . ? C22 C23 C24 C25 2.6(11) . . . . ? C23 C24 C25 C20 0.1(9) . . . . ? C23 C24 C25 C29 -178.5(6) . . . . ? C21 C20 C25 C24 -4.9(9) . . . . ? N4 C20 C25 C24 179.5(5) . . . . ? C21 C20 C25 C29 173.7(6) . . . . ? N4 C20 C25 C29 -1.9(8) . . . . ? C20 C21 C26 C27B -159.4(12) . . . . ? C22 C21 C26 C27B 23.1(15) . . . . ? C20 C21 C26 C27A -109.8(10) . . . . ? C22 C21 C26 C27A 72.6(11) . . . . ? C20 C21 C26 C28B 75.8(11) . . . . ? C22 C21 C26 C28B -101.8(11) . . . . ? C20 C21 C26 C28A 141.9(9) . . . . ? C22 C21 C26 C28A -35.6(11) . . . . ? C24 C25 C29 C31 81.3(8) . . . . ? C20 C25 C29 C31 -97.2(7) . . . . ? C24 C25 C29 C30 -41.3(7) . . . . ? C20 C25 C29 C30 140.1(6) . . . . ? C1 Fe1 C32 C33 -160.9(6) . . . . ? C5 Fe1 C32 C33 -57.6(7) . . . . ? C37 Fe1 C32 C33 128.3(9) . . . . ? C36 Fe1 C32 C33 101.1(7) . . . . ? C34 Fe1 C32 C33 28.7(6) . . . . ? C35 Fe1 C32 C33 64.9(6) . . . . ? C1 Fe1 C32 C37 70.8(6) . . . . ? C5 Fe1 C32 C37 174.1(5) . . . . ? C36 Fe1 C32 C37 -27.1(5) . . . . ? C33 Fe1 C32 C37 -128.3(9) . . . . ? C34 Fe1 C32 C37 -99.5(6) . . . . ? C35 Fe1 C32 C37 -63.4(5) . . . . ? C1 Fe1 C32 C38 -47.5(10) . . . . ? C5 Fe1 C32 C38 55.8(10) . . . . ? C37 Fe1 C32 C38 -118.3(11) . . . . ? C36 Fe1 C32 C38 -145.4(10) . . . . ? C33 Fe1 C32 C38 113.5(12) . . . . ? C34 Fe1 C32 C38 142.2(10) . . . . ? C35 Fe1 C32 C38 178.4(10) . . . . ? C37 C32 C33 C34 1.0(12) . . . . ? C38 C32 C33 C34 -174.3(9) . . . . ? Fe1 C32 C33 C34 -53.0(7) . . . . ? C37 C32 C33 Fe1 54.0(6) . . . . ? C38 C32 C33 Fe1 -121.3(9) . . . . ? C1 Fe1 C33 C32 32.6(9) . . . . ? C5 Fe1 C33 C32 134.0(6) . . . . ? C37 Fe1 C33 C32 -32.4(6) . . . . ? C36 Fe1 C33 C32 -69.9(7) . . . . ? C34 Fe1 C33 C32 -133.9(9) . . . . ? C35 Fe1 C33 C32 -107.2(7) . . . . ? C1 Fe1 C33 C34 166.5(4) . . . . ? C5 Fe1 C33 C34 -92.1(5) . . . . ? C37 Fe1 C33 C34 101.5(6) . . . . ? C36 Fe1 C33 C34 64.0(5) . . . . ? C32 Fe1 C33 C34 133.9(9) . . . . ? C35 Fe1 C33 C34 26.7(5) . . . . ? C32 C33 C34 C35 2.9(13) . . . . ? Fe1 C33 C34 C35 -50.1(7) . . . . ? C32 C33 C34 Fe1 53.0(7) . . . . ? C1 Fe1 C34 C35 14(2) . . . . ? C5 Fe1 C34 C35 -130.2(5) . . . . ? C37 Fe1 C34 C35 68.4(6) . . . . ? C36 Fe1 C34 C35 30.6(5) . . . . ? C33 Fe1 C34 C35 136.6(7) . . . . ? C32 Fe1 C34 C35 108.0(6) . . . . ? C1 Fe1 C34 C33 -123(2) . . . . ? C5 Fe1 C34 C33 93.2(5) . . . . ? C37 Fe1 C34 C33 -68.3(5) . . . . ? C36 Fe1 C34 C33 -106.1(6) . . . . ? C32 Fe1 C34 C33 -28.7(5) . . . . ? C35 Fe1 C34 C33 -136.6(7) . . . . ? C33 C34 C35 C36 -4.5(11) . . . . ? Fe1 C34 C35 C36 -54.0(6) . . . . ? C33 C34 C35 Fe1 49.5(7) . . . . ? C1 Fe1 C35 C36 -47.0(7) . . . . ? C5 Fe1 C35 C36 -169.3(5) . . . . ? C37 Fe1 C35 C36 28.3(5) . . . . ? C33 Fe1 C35 C36 102.8(6) . . . . ? C34 Fe1 C35 C36 130.0(8) . . . . ? C32 Fe1 C35 C36 65.7(6) . . . . ? C1 Fe1 C35 C34 -177.0(5) . . . . ? C5 Fe1 C35 C34 60.8(6) . . . . ? C37 Fe1 C35 C34 -101.7(6) . . . . ? C36 Fe1 C35 C34 -130.0(8) . . . . ? C33 Fe1 C35 C34 -27.2(5) . . . . ? C32 Fe1 C35 C34 -64.2(6) . . . . ? C34 C35 C36 C37 2.2(11) . . . . ? Fe1 C35 C36 C37 -52.2(7) . . . . ? C34 C35 C36 Fe1 54.4(6) . . . . ? C1 Fe1 C36 C35 146.6(6) . . . . ? C5 Fe1 C36 C35 23.7(10) . . . . ? C37 Fe1 C36 C35 -134.6(8) . . . . ? C33 Fe1 C36 C35 -68.3(6) . . . . ? C34 Fe1 C36 C35 -30.8(6) . . . . ? C32 Fe1 C36 C35 -106.8(6) . . . . ? C1 Fe1 C36 C37 -78.8(4) . . . . ? C5 Fe1 C36 C37 158.3(6) . . . . ? C33 Fe1 C36 C37 66.3(5) . . . . ? C34 Fe1 C36 C37 103.8(6) . . . . ? C32 Fe1 C36 C37 27.8(5) . . . . ? C35 Fe1 C36 C37 134.6(8) . . . . ? C35 C36 C37 C32 1.8(12) . . . . ? Fe1 C36 C37 C32 -51.1(7) . . . . ? C35 C36 C37 Fe1 52.9(7) . . . . ? C33 C32 C37 C36 -3.3(11) . . . . ? C38 C32 C37 C36 171.7(9) . . . . ? Fe1 C32 C37 C36 51.0(7) . . . . ? C33 C32 C37 Fe1 -54.3(6) . . . . ? C38 C32 C37 Fe1 120.8(9) . . . . ? C1 Fe1 C37 C36 106.9(4) . . . . ? C5 Fe1 C37 C36 -152.0(8) . . . . ? C33 Fe1 C37 C36 -104.3(5) . . . . ? C34 Fe1 C37 C36 -65.7(5) . . . . ? C32 Fe1 C37 C36 -136.1(7) . . . . ? C35 Fe1 C37 C36 -27.8(5) . . . . ? C1 Fe1 C37 C32 -117.0(6) . . . . ? C5 Fe1 C37 C32 -15.9(11) . . . . ? C36 Fe1 C37 C32 136.1(7) . . . . ? C33 Fe1 C37 C32 31.8(6) . . . . ? C34 Fe1 C37 C32 70.4(6) . . . . ? C35 Fe1 C37 C32 108.2(6) . . . . ? C41 B1 C39 C40 154.0(8) . . . . ? C2 B1 C39 C40 35.9(12) . . . . ? C43 B1 C39 C40 -84.8(9) . . . . ? C39 B1 C41 C42 -175.5(8) . . . . ? C2 B1 C41 C42 -54.1(10) . . . . ? C43 B1 C41 C42 63.4(11) . . . . ? C41 B1 C43 C44 166.2(8) . . . . ? C39 B1 C43 C44 46.2(9) . . . . ? C2 B1 C43 C44 -77.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.504 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.066 #===END data_c:\workdo~1\crystals\omji89~1\omji89 _database_code_depnum_ccdc_archive 'CCDC 851127' #TrackingRef '- final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H57 Fe I N4' _chemical_formula_sum 'C45 H57 Fe I N4' _chemical_formula_weight 836.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.295(2) _cell_length_b 23.9333(10) _cell_length_c 24.0891(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8241.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15852 _cell_measurement_theta_min 2.9070 _cell_measurement_theta_max 28.6191 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3472 _exptl_absorpt_coefficient_mu 1.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7619 _exptl_absorpt_correction_T_max 0.8936 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49276 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7255 _reflns_number_gt 5214 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7255 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _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 I1 I 0.202141(13) 0.479520(8) 0.029696(8) 0.02848(7) Uani 1 1 d . . . Fe1 Fe 0.28183(2) 0.145106(16) -0.108588(15) 0.01937(10) Uani 1 1 d . . . N1 N 0.42429(14) 0.11839(9) -0.02598(9) 0.0197(5) Uani 1 1 d . . . N2 N 0.33235(15) 0.17808(9) 0.01087(9) 0.0206(5) Uani 1 1 d . . . N3 N 0.47170(14) 0.10118(9) -0.11802(9) 0.0204(5) Uani 1 1 d . . . N4 N 0.44046(14) 0.14191(9) -0.19471(9) 0.0187(5) Uani 1 1 d . . . C1 C 0.34472(17) 0.14769(10) -0.03672(10) 0.0195(6) Uani 1 1 d . . . C2 C 0.46105(19) 0.13001(11) 0.02567(11) 0.0246(6) Uani 1 1 d . . . H2 H 0.5161 0.1145 0.0415 0.030 Uiso 1 1 calc R . . C3 C 0.40406(19) 0.16721(12) 0.04887(11) 0.0254(7) Uani 1 1 d . . . H3 H 0.4108 0.1834 0.0846 0.031 Uiso 1 1 calc R . . C4 C 0.45829(19) 0.07602(11) -0.06365(11) 0.0228(6) Uani 1 1 d . . . H4A H 0.4125 0.0451 -0.0662 0.027 Uiso 1 1 calc R . . H4B H 0.5183 0.0607 -0.0499 0.027 Uiso 1 1 calc R . . C5 C 0.40191(18) 0.12973(10) -0.14397(11) 0.0188(6) Uani 1 1 d . . . C6 C 0.55104(18) 0.09585(11) -0.15061(11) 0.0235(6) Uani 1 1 d . . . H6 H 0.6077 0.0776 -0.1410 0.028 Uiso 1 1 calc R . . C7 C 0.53161(18) 0.12162(11) -0.19828(11) 0.0225(6) Uani 1 1 d . . . H7 H 0.5725 0.1255 -0.2291 0.027 Uiso 1 1 calc R . . C8 C 0.25137(18) 0.21139(11) 0.02589(10) 0.0193(6) Uani 1 1 d . . . C9 C 0.17816(18) 0.18455(11) 0.05476(11) 0.0219(6) Uani 1 1 d . . . C10 C 0.1016(2) 0.21718(12) 0.06926(11) 0.0232(6) Uani 1 1 d . . . C11 C 0.09900(19) 0.27389(12) 0.05753(11) 0.0267(7) Uani 1 1 d . . . H11 H 0.0459 0.2954 0.0679 0.032 Uiso 1 1 calc R . . C12 C 0.1735(2) 0.29932(12) 0.03073(11) 0.0255(6) Uani 1 1 d . . . H12 H 0.1716 0.3383 0.0235 0.031 Uiso 1 1 calc R . . C13 C 0.25168(19) 0.26824(11) 0.01419(10) 0.0218(6) Uani 1 1 d . . . C14 C 0.18410(18) 0.12361(11) 0.07171(11) 0.0245(6) Uani 1 1 d . . . H14 H 0.2284 0.1045 0.0458 0.029 Uiso 1 1 calc R . . C15 C 0.0901(2) 0.09268(12) 0.06887(13) 0.0338(7) Uani 1 1 d . . . H15A H 0.0500 0.1049 0.0996 0.051 Uiso 1 1 calc R . . H15B H 0.1009 0.0524 0.0718 0.051 Uiso 1 1 calc R . . H15C H 0.0593 0.1010 0.0335 0.051 Uiso 1 1 calc R . . C16 C 0.2240(2) 0.11865(12) 0.13074(12) 0.0332(7) Uani 1 1 d . . . H16A H 0.2849 0.1374 0.1325 0.050 Uiso 1 1 calc R . . H16B H 0.2316 0.0791 0.1403 0.050 Uiso 1 1 calc R . . H16C H 0.1810 0.1363 0.1571 0.050 Uiso 1 1 calc R . . C17 C 0.3352(2) 0.29666(12) -0.01247(11) 0.0272(7) Uani 1 1 d . . . H17 H 0.3731 0.2674 -0.0318 0.033 Uiso 1 1 calc R . . C18 C 0.3968(2) 0.32383(15) 0.03140(12) 0.0429(8) Uani 1 1 d . . . H18A H 0.3626 0.3546 0.0490 0.064 Uiso 1 1 calc R . . H18B H 0.4537 0.3383 0.0139 0.064 Uiso 1 1 calc R . . H18C H 0.4137 0.2960 0.0596 0.064 Uiso 1 1 calc R . . C19 C 0.3062(2) 0.34034(13) -0.05553(12) 0.0369(8) Uani 1 1 d . . . H19A H 0.2653 0.3230 -0.0832 0.055 Uiso 1 1 calc R . . H19B H 0.3621 0.3552 -0.0739 0.055 Uiso 1 1 calc R . . H19C H 0.2727 0.3708 -0.0370 0.055 Uiso 1 1 calc R . . C20 C 0.39318(18) 0.16862(11) -0.24093(10) 0.0204(6) Uani 1 1 d . . . C21 C 0.38651(19) 0.22678(11) -0.24193(11) 0.0252(6) Uani 1 1 d . . . C22 C 0.3352(2) 0.25058(12) -0.28509(11) 0.0309(7) Uani 1 1 d . . . H22 H 0.3282 0.2900 -0.2864 0.037 Uiso 1 1 calc R . . C23 C 0.2943(2) 0.21855(13) -0.32586(12) 0.0331(7) Uani 1 1 d . . . H23 H 0.2574 0.2357 -0.3539 0.040 Uiso 1 1 calc R . . C24 C 0.30717(19) 0.16133(13) -0.32571(11) 0.0282(7) Uani 1 1 d . . . H24 H 0.2812 0.1395 -0.3548 0.034 Uiso 1 1 calc R . . C25 C 0.35751(18) 0.13502(11) -0.28364(11) 0.0229(6) Uani 1 1 d . . . C26 C 0.4396(2) 0.26267(11) -0.20010(12) 0.0266(7) Uani 1 1 d . . . H26 H 0.4390 0.2430 -0.1635 0.032 Uiso 1 1 calc R . . C27 C 0.5414(2) 0.26892(13) -0.21874(12) 0.0361(8) Uani 1 1 d . . . H27A H 0.5699 0.2319 -0.2226 0.054 Uiso 1 1 calc R . . H27B H 0.5761 0.2906 -0.1910 0.054 Uiso 1 1 calc R . . H27C H 0.5435 0.2883 -0.2545 0.054 Uiso 1 1 calc R . . C28 C 0.3959(2) 0.32017(12) -0.19228(13) 0.0396(8) Uani 1 1 d . . . H28A H 0.4292 0.3403 -0.1629 0.059 Uiso 1 1 calc R . . H28B H 0.3300 0.3160 -0.1819 0.059 Uiso 1 1 calc R . . H28C H 0.4003 0.3413 -0.2271 0.059 Uiso 1 1 calc R . . C29 C 0.37627(19) 0.07248(12) -0.28719(11) 0.0260(7) Uani 1 1 d . . . H29 H 0.3946 0.0588 -0.2495 0.031 Uiso 1 1 calc R . . C30 C 0.2903(2) 0.03936(12) -0.30654(13) 0.0337(7) Uani 1 1 d . . . H30A H 0.2354 0.0511 -0.2851 0.051 Uiso 1 1 calc R . . H30B H 0.3013 -0.0006 -0.3008 0.051 Uiso 1 1 calc R . . H30C H 0.2794 0.0465 -0.3461 0.051 Uiso 1 1 calc R . . C31 C 0.4579(2) 0.06148(13) -0.32748(12) 0.0365(8) Uani 1 1 d . . . H31A H 0.4405 0.0740 -0.3648 0.055 Uiso 1 1 calc R . . H31B H 0.4719 0.0214 -0.3282 0.055 Uiso 1 1 calc R . . H31C H 0.5134 0.0821 -0.3150 0.055 Uiso 1 1 calc R . . C32 C 0.14952(18) 0.18058(13) -0.12824(12) 0.0295(7) Uani 1 1 d . . . C33 C 0.18866(19) 0.15402(13) -0.17546(12) 0.0293(7) Uani 1 1 d . . . H33 H 0.1942 0.1738 -0.2095 0.035 Uiso 1 1 calc R . . C34 C 0.21908(19) 0.09873(13) -0.17187(13) 0.0335(8) Uani 1 1 d . . . H34 H 0.2458 0.0816 -0.2037 0.040 Uiso 1 1 calc R . . C35 C 0.21146(18) 0.06728(12) -0.12223(13) 0.0312(7) Uani 1 1 d . . . H35 H 0.2314 0.0294 -0.1207 0.037 Uiso 1 1 calc R . . C36 C 0.17403(19) 0.09354(13) -0.07613(13) 0.0327(8) Uani 1 1 d . . . H36 H 0.1702 0.0739 -0.0419 0.039 Uiso 1 1 calc R . . C37 C 0.14169(17) 0.14875(13) -0.07932(12) 0.0281(7) Uani 1 1 d . . . H37 H 0.1136 0.1652 -0.0475 0.034 Uiso 1 1 calc R . . C38 C 0.1156(2) 0.23937(13) -0.13081(14) 0.0449(9) Uani 1 1 d . . . H38A H 0.1560 0.2610 -0.1557 0.067 Uiso 1 1 calc R . . H38B H 0.1174 0.2558 -0.0936 0.067 Uiso 1 1 calc R . . H38C H 0.0513 0.2400 -0.1448 0.067 Uiso 1 1 calc R . . C39 C 0.0093(2) 0.44360(12) -0.20495(14) 0.0379(8) Uani 1 1 d . . . C40 C 0.0779(2) 0.42277(13) -0.23930(14) 0.0380(8) Uani 1 1 d . . . H40 H 0.0645 0.4174 -0.2776 0.046 Uiso 1 1 calc R . . C41 C 0.1660(2) 0.40946(13) -0.21927(13) 0.0372(8) Uani 1 1 d . . . H41 H 0.2113 0.3939 -0.2437 0.045 Uiso 1 1 calc R . . C42 C 0.1884(2) 0.41838(13) -0.16513(13) 0.0376(8) Uani 1 1 d . . . H42 H 0.2494 0.4104 -0.1517 0.045 Uiso 1 1 calc R . . C43 C 0.1197(2) 0.43943(13) -0.12977(13) 0.0408(8) Uani 1 1 d . . . H43 H 0.1339 0.4454 -0.0917 0.049 Uiso 1 1 calc R . . C44 C 0.0318(2) 0.45168(12) -0.14934(14) 0.0390(8) Uani 1 1 d . . . H44 H -0.0142 0.4658 -0.1246 0.047 Uiso 1 1 calc R . . C45 C -0.0852(2) 0.45940(15) -0.22697(18) 0.0598(11) Uani 1 1 d . . . H45A H -0.1333 0.4490 -0.1999 0.090 Uiso 1 1 calc R . . H45B H -0.0966 0.4397 -0.2620 0.090 Uiso 1 1 calc R . . H45C H -0.0874 0.4998 -0.2334 0.090 Uiso 1 1 calc R . . H1 H 0.3150(18) 0.2020(11) -0.1133(11) 0.036(8) Uiso 1 1 d . . . H10 H 0.0522(17) 0.1991(10) 0.0855(10) 0.015(7) Uiso 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 I1 0.03017(11) 0.02623(11) 0.02902(12) 0.00483(8) -0.00015(8) -0.00582(8) Fe1 0.0194(2) 0.0208(2) 0.0179(2) 0.00075(16) -0.00038(15) 0.00205(16) N1 0.0192(12) 0.0190(12) 0.0209(12) 0.0072(10) 0.0004(9) 0.0042(9) N2 0.0231(12) 0.0206(13) 0.0182(12) 0.0029(10) 0.0003(9) 0.0025(10) N3 0.0191(12) 0.0200(12) 0.0221(13) 0.0033(10) 0.0018(9) 0.0030(9) N4 0.0211(12) 0.0167(12) 0.0184(12) -0.0011(10) -0.0008(9) -0.0003(9) C1 0.0206(14) 0.0175(14) 0.0206(15) 0.0054(11) 0.0017(11) -0.0005(11) C2 0.0256(15) 0.0290(16) 0.0193(16) 0.0087(13) -0.0032(12) 0.0024(12) C3 0.0291(16) 0.0323(17) 0.0149(14) 0.0059(12) -0.0036(12) -0.0003(13) C4 0.0238(15) 0.0203(15) 0.0242(16) 0.0039(12) 0.0020(12) 0.0051(12) C5 0.0223(15) 0.0122(13) 0.0220(15) -0.0015(11) -0.0017(11) -0.0004(11) C6 0.0213(15) 0.0192(15) 0.0299(17) -0.0019(12) 0.0014(12) 0.0025(12) C7 0.0206(15) 0.0229(15) 0.0241(16) -0.0015(12) 0.0029(12) 0.0012(12) C8 0.0224(15) 0.0229(14) 0.0126(14) -0.0012(11) -0.0022(11) 0.0038(12) C9 0.0285(16) 0.0206(15) 0.0167(14) -0.0013(12) -0.0036(11) 0.0020(12) C10 0.0253(16) 0.0272(17) 0.0172(15) 0.0008(12) 0.0024(12) 0.0007(13) C11 0.0301(17) 0.0277(17) 0.0222(16) -0.0023(13) 0.0005(12) 0.0084(13) C12 0.0378(17) 0.0181(15) 0.0207(15) 0.0048(12) -0.0017(13) 0.0043(12) C13 0.0256(15) 0.0254(16) 0.0143(14) 0.0013(12) -0.0024(11) 0.0011(12) C14 0.0285(16) 0.0207(15) 0.0243(16) 0.0017(12) 0.0060(12) 0.0038(12) C15 0.0362(18) 0.0256(17) 0.0396(19) 0.0053(14) 0.0076(14) -0.0006(14) C16 0.046(2) 0.0284(17) 0.0255(17) 0.0078(13) 0.0047(14) 0.0053(14) C17 0.0312(16) 0.0252(16) 0.0253(16) 0.0033(13) 0.0033(12) 0.0014(13) C18 0.0385(19) 0.059(2) 0.0315(19) 0.0123(17) -0.0016(15) -0.0151(17) C19 0.046(2) 0.0368(19) 0.0274(17) 0.0117(15) 0.0011(14) -0.0088(15) C20 0.0219(15) 0.0218(15) 0.0175(15) 0.0013(12) 0.0004(11) 0.0012(12) C21 0.0304(16) 0.0243(16) 0.0208(16) 0.0007(12) 0.0047(12) 0.0000(13) C22 0.0424(18) 0.0222(16) 0.0282(18) 0.0044(13) 0.0004(14) 0.0065(14) C23 0.0380(18) 0.0374(19) 0.0239(17) 0.0093(14) -0.0037(13) 0.0057(15) C24 0.0306(17) 0.0359(18) 0.0181(15) 0.0001(13) -0.0011(12) -0.0027(13) C25 0.0211(15) 0.0253(16) 0.0223(16) -0.0004(12) 0.0044(11) -0.0008(12) C26 0.0413(18) 0.0187(15) 0.0198(15) -0.0009(12) 0.0025(13) -0.0020(13) C27 0.042(2) 0.0335(19) 0.0332(19) -0.0078(15) 0.0012(14) -0.0081(15) C28 0.051(2) 0.0277(18) 0.040(2) -0.0075(15) -0.0008(16) 0.0021(15) C29 0.0288(16) 0.0276(16) 0.0215(16) -0.0030(12) -0.0031(12) -0.0013(13) C30 0.0421(19) 0.0269(16) 0.0322(18) -0.0059(13) -0.0040(14) -0.0059(14) C31 0.0395(19) 0.0347(19) 0.0353(19) -0.0073(15) 0.0029(14) 0.0018(15) C32 0.0172(15) 0.0383(18) 0.0329(18) -0.0004(14) -0.0087(12) 0.0078(13) C33 0.0243(16) 0.045(2) 0.0189(16) 0.0040(14) -0.0061(12) -0.0041(14) C34 0.0216(16) 0.047(2) 0.0319(18) -0.0147(15) 0.0001(13) -0.0049(14) C35 0.0232(16) 0.0227(16) 0.048(2) -0.0049(14) -0.0028(14) -0.0045(13) C36 0.0212(16) 0.044(2) 0.0333(18) 0.0135(15) -0.0057(13) -0.0076(14) C37 0.0124(14) 0.0426(19) 0.0291(17) -0.0024(14) 0.0023(11) 0.0021(13) C38 0.040(2) 0.043(2) 0.052(2) 0.0057(17) -0.0132(16) 0.0133(16) C39 0.0341(19) 0.0235(17) 0.056(2) -0.0026(16) 0.0020(16) -0.0054(14) C40 0.043(2) 0.0355(19) 0.036(2) -0.0062(15) -0.0018(15) -0.0020(15) C41 0.0400(19) 0.038(2) 0.0337(19) -0.0049(15) 0.0039(15) 0.0038(15) C42 0.044(2) 0.0325(18) 0.036(2) 0.0032(15) -0.0050(15) 0.0006(15) C43 0.061(2) 0.0310(18) 0.0308(19) 0.0036(15) 0.0078(16) -0.0043(17) C44 0.049(2) 0.0268(18) 0.041(2) -0.0013(15) 0.0172(16) -0.0012(16) C45 0.037(2) 0.038(2) 0.103(3) -0.015(2) -0.005(2) -0.0002(17) _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 C5 1.951(3) . ? Fe1 C1 1.952(3) . ? Fe1 C34 2.088(3) . ? Fe1 C33 2.101(3) . ? Fe1 C36 2.123(3) . ? Fe1 C37 2.126(3) . ? Fe1 C32 2.126(3) . ? Fe1 C35 2.142(3) . ? Fe1 H1 1.45(3) . ? N1 C1 1.361(3) . ? N1 C2 1.379(3) . ? N1 C4 1.445(3) . ? N2 C1 1.369(3) . ? N2 C3 1.399(3) . ? N2 C8 1.451(3) . ? N3 C5 1.361(3) . ? N3 C6 1.385(3) . ? N3 C4 1.454(3) . ? N4 C5 1.372(3) . ? N4 C7 1.393(3) . ? N4 C20 1.451(3) . ? C2 C3 1.330(4) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C6 C7 1.333(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.389(4) . ? C8 C9 1.411(4) . ? C9 C10 1.389(4) . ? C9 C14 1.517(4) . ? C10 C11 1.387(4) . ? C10 H10 0.92(2) . ? C11 C12 1.386(4) . ? C11 H11 0.9500 . ? C12 C13 1.400(4) . ? C12 H12 0.9500 . ? C13 C17 1.517(4) . ? C14 C15 1.536(4) . ? C14 C16 1.537(4) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.521(4) . ? C17 C19 1.530(4) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.395(4) . ? C20 C25 1.402(4) . ? C21 C22 1.394(4) . ? C21 C26 1.526(4) . ? C22 C23 1.376(4) . ? C22 H22 0.9500 . ? C23 C24 1.382(4) . ? C23 H23 0.9500 . ? C24 C25 1.393(4) . ? C24 H24 0.9500 . ? C25 C29 1.523(4) . ? C26 C28 1.523(4) . ? C26 C27 1.531(4) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.534(4) . ? C29 C31 1.541(4) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.408(4) . ? C32 C33 1.418(4) . ? C32 C38 1.489(4) . ? C33 C34 1.396(4) . ? C33 H33 0.9500 . ? C34 C35 1.417(4) . ? C34 H34 0.9500 . ? C35 C36 1.384(4) . ? C35 H35 0.9500 . ? C36 C37 1.402(4) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.376(4) . ? C39 C44 1.391(4) . ? C39 C45 1.500(4) . ? C40 C41 1.386(4) . ? C40 H40 0.9500 . ? C41 C42 1.360(4) . ? C41 H41 0.9500 . ? C42 C43 1.394(4) . ? C42 H42 0.9500 . ? C43 C44 1.374(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 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 C5 Fe1 C1 89.33(11) . . ? C5 Fe1 C34 87.64(11) . . ? C1 Fe1 C34 149.57(12) . . ? C5 Fe1 C33 104.00(11) . . ? C1 Fe1 C33 165.66(11) . . ? C34 Fe1 C33 38.92(11) . . ? C5 Fe1 C36 133.59(11) . . ? C1 Fe1 C36 91.49(11) . . ? C34 Fe1 C36 69.40(12) . . ? C33 Fe1 C36 83.18(11) . . ? C5 Fe1 C37 169.00(11) . . ? C1 Fe1 C37 97.97(11) . . ? C34 Fe1 C37 81.90(11) . . ? C33 Fe1 C37 69.67(11) . . ? C36 Fe1 C37 38.53(11) . . ? C5 Fe1 C32 139.50(11) . . ? C1 Fe1 C32 126.48(11) . . ? C34 Fe1 C32 70.58(11) . . ? C33 Fe1 C32 39.19(11) . . ? C36 Fe1 C32 70.65(11) . . ? C37 Fe1 C32 38.67(11) . . ? C5 Fe1 C35 100.49(11) . . ? C1 Fe1 C35 112.33(11) . . ? C34 Fe1 C35 39.11(11) . . ? C33 Fe1 C35 70.91(11) . . ? C36 Fe1 C35 37.85(11) . . ? C37 Fe1 C35 69.14(11) . . ? C32 Fe1 C35 83.99(11) . . ? C5 Fe1 H1 81.7(10) . . ? C1 Fe1 H1 83.6(10) . . ? C34 Fe1 H1 125.8(10) . . ? C33 Fe1 H1 93.0(10) . . ? C36 Fe1 H1 144.5(10) . . ? C37 Fe1 H1 107.2(10) . . ? C32 Fe1 H1 84.2(10) . . ? C35 Fe1 H1 163.9(10) . . ? C1 N1 C2 112.7(2) . . ? C1 N1 C4 121.5(2) . . ? C2 N1 C4 125.5(2) . . ? C1 N2 C3 110.8(2) . . ? C1 N2 C8 127.1(2) . . ? C3 N2 C8 121.6(2) . . ? C5 N3 C6 112.7(2) . . ? C5 N3 C4 121.7(2) . . ? C6 N3 C4 125.5(2) . . ? C5 N4 C7 110.9(2) . . ? C5 N4 C20 126.2(2) . . ? C7 N4 C20 122.8(2) . . ? N1 C1 N2 102.9(2) . . ? N1 C1 Fe1 122.49(18) . . ? N2 C1 Fe1 134.43(19) . . ? C3 C2 N1 106.3(2) . . ? C3 C2 H2 126.9 . . ? N1 C2 H2 126.9 . . ? C2 C3 N2 107.4(2) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? N1 C4 N3 108.6(2) . . ? N1 C4 H4A 110.0 . . ? N3 C4 H4A 110.0 . . ? N1 C4 H4B 110.0 . . ? N3 C4 H4B 110.0 . . ? H4A C4 H4B 108.3 . . ? N3 C5 N4 102.8(2) . . ? N3 C5 Fe1 122.60(18) . . ? N4 C5 Fe1 134.61(19) . . ? C7 C6 N3 106.0(2) . . ? C7 C6 H6 127.0 . . ? N3 C6 H6 127.0 . . ? C6 C7 N4 107.6(2) . . ? C6 C7 H7 126.2 . . ? N4 C7 H7 126.2 . . ? C13 C8 C9 123.2(2) . . ? C13 C8 N2 119.0(2) . . ? C9 C8 N2 117.7(2) . . ? C10 C9 C8 116.9(2) . . ? C10 C9 C14 121.1(2) . . ? C8 C9 C14 121.9(2) . . ? C11 C10 C9 121.4(3) . . ? C11 C10 H10 121.9(16) . . ? C9 C10 H10 116.6(16) . . ? C12 C11 C10 120.2(3) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.8(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C8 C13 C12 117.4(3) . . ? C8 C13 C17 121.8(2) . . ? C12 C13 C17 120.7(2) . . ? C9 C14 C15 113.7(2) . . ? C9 C14 C16 110.1(2) . . ? C15 C14 C16 109.2(2) . . ? C9 C14 H14 107.9 . . ? C15 C14 H14 107.9 . . ? C16 C14 H14 107.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 C18 110.7(2) . . ? C13 C17 C19 112.3(2) . . ? C18 C17 C19 109.6(2) . . ? C13 C17 H17 108.0 . . ? C18 C17 H17 108.0 . . ? C19 C17 H17 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 122.3(2) . . ? C21 C20 N4 119.0(2) . . ? C25 C20 N4 118.7(2) . . ? C22 C21 C20 117.1(3) . . ? C22 C21 C26 121.6(3) . . ? C20 C21 C26 121.1(2) . . ? C23 C22 C21 121.9(3) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C22 C23 C24 119.6(3) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C23 C24 C25 121.2(3) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C24 C25 C20 117.5(3) . . ? C24 C25 C29 119.6(2) . . ? C20 C25 C29 122.8(2) . . ? C28 C26 C21 112.7(2) . . ? C28 C26 C27 109.8(2) . . ? C21 C26 C27 109.5(2) . . ? C28 C26 H26 108.2 . . ? C21 C26 H26 108.2 . . ? C27 C26 H26 108.2 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 C30 112.6(2) . . ? C25 C29 C31 109.7(2) . . ? C30 C29 C31 109.1(2) . . ? C25 C29 H29 108.5 . . ? C30 C29 H29 108.5 . . ? C31 C29 H29 108.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 117.4(3) . . ? C37 C32 C38 121.3(3) . . ? C33 C32 C38 121.2(3) . . ? C37 C32 Fe1 70.63(15) . . ? C33 C32 Fe1 69.44(15) . . ? C38 C32 Fe1 132.5(2) . . ? C34 C33 C32 119.9(3) . . ? C34 C33 Fe1 70.04(16) . . ? C32 C33 Fe1 71.37(15) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? Fe1 C33 H33 131.3 . . ? C33 C34 C35 122.1(3) . . ? C33 C34 Fe1 71.04(16) . . ? C35 C34 Fe1 72.51(16) . . ? C33 C34 H34 118.9 . . ? C35 C34 H34 118.9 . . ? Fe1 C34 H34 130.3 . . ? C36 C35 C34 117.8(3) . . ? C36 C35 Fe1 70.34(17) . . ? C34 C35 Fe1 68.38(16) . . ? C36 C35 H35 121.1 . . ? C34 C35 H35 121.1 . . ? Fe1 C35 H35 133.0 . . ? C35 C36 C37 120.8(3) . . ? C35 C36 Fe1 71.81(17) . . ? C37 C36 Fe1 70.82(16) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? Fe1 C36 H36 130.4 . . ? C36 C37 C32 122.0(3) . . ? C36 C37 Fe1 70.65(16) . . ? C32 C37 Fe1 70.70(15) . . ? C36 C37 H37 119.0 . . ? C32 C37 H37 119.0 . . ? Fe1 C37 H37 133.0 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 117.7(3) . . ? C40 C39 C45 121.4(3) . . ? C44 C39 C45 120.9(3) . . ? C39 C40 C41 121.4(3) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C42 C41 C40 120.8(3) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C41 C42 C43 118.5(3) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? C44 C43 C42 120.8(3) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C39 120.8(3) . . ? C43 C44 H44 119.6 . . ? C39 C44 H44 119.6 . . ? C39 C45 H45A 109.5 . . ? C39 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C39 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 -0.5(3) . . . . ? C4 N1 C1 N2 173.6(2) . . . . ? C2 N1 C1 Fe1 174.81(18) . . . . ? C4 N1 C1 Fe1 -11.0(3) . . . . ? C3 N2 C1 N1 0.5(3) . . . . ? C8 N2 C1 N1 -171.1(2) . . . . ? C3 N2 C1 Fe1 -174.0(2) . . . . ? C8 N2 C1 Fe1 14.4(4) . . . . ? C5 Fe1 C1 N1 -28.3(2) . . . . ? C34 Fe1 C1 N1 55.9(3) . . . . ? C33 Fe1 C1 N1 173.2(4) . . . . ? C36 Fe1 C1 N1 105.3(2) . . . . ? C37 Fe1 C1 N1 143.5(2) . . . . ? C32 Fe1 C1 N1 172.19(19) . . . . ? C35 Fe1 C1 N1 72.8(2) . . . . ? C5 Fe1 C1 N2 145.4(3) . . . . ? C34 Fe1 C1 N2 -130.4(3) . . . . ? C33 Fe1 C1 N2 -13.2(6) . . . . ? C36 Fe1 C1 N2 -81.0(3) . . . . ? C37 Fe1 C1 N2 -42.9(3) . . . . ? C32 Fe1 C1 N2 -14.2(3) . . . . ? C35 Fe1 C1 N2 -113.5(3) . . . . ? C1 N1 C2 C3 0.3(3) . . . . ? C4 N1 C2 C3 -173.6(2) . . . . ? N1 C2 C3 N2 0.0(3) . . . . ? C1 N2 C3 C2 -0.3(3) . . . . ? C8 N2 C3 C2 171.8(2) . . . . ? C1 N1 C4 N3 56.9(3) . . . . ? C2 N1 C4 N3 -129.7(2) . . . . ? C5 N3 C4 N1 -53.7(3) . . . . ? C6 N3 C4 N1 131.4(2) . . . . ? C6 N3 C5 N4 0.4(3) . . . . ? C4 N3 C5 N4 -175.1(2) . . . . ? C6 N3 C5 Fe1 -179.13(17) . . . . ? C4 N3 C5 Fe1 5.4(3) . . . . ? C7 N4 C5 N3 -0.8(3) . . . . ? C20 N4 C5 N3 175.0(2) . . . . ? C7 N4 C5 Fe1 178.7(2) . . . . ? C20 N4 C5 Fe1 -5.5(4) . . . . ? C1 Fe1 C5 N3 30.9(2) . . . . ? C34 Fe1 C5 N3 -118.8(2) . . . . ? C33 Fe1 C5 N3 -154.4(2) . . . . ? C36 Fe1 C5 N3 -60.5(3) . . . . ? C37 Fe1 C5 N3 -100.8(6) . . . . ? C32 Fe1 C5 N3 -174.71(19) . . . . ? C35 Fe1 C5 N3 -81.7(2) . . . . ? C1 Fe1 C5 N4 -148.5(3) . . . . ? C34 Fe1 C5 N4 61.8(3) . . . . ? C33 Fe1 C5 N4 26.2(3) . . . . ? C36 Fe1 C5 N4 120.1(3) . . . . ? C37 Fe1 C5 N4 79.8(6) . . . . ? C32 Fe1 C5 N4 5.9(3) . . . . ? C35 Fe1 C5 N4 98.9(3) . . . . ? C5 N3 C6 C7 0.1(3) . . . . ? C4 N3 C6 C7 175.4(2) . . . . ? N3 C6 C7 N4 -0.6(3) . . . . ? C5 N4 C7 C6 1.0(3) . . . . ? C20 N4 C7 C6 -175.1(2) . . . . ? C1 N2 C8 C13 -94.7(3) . . . . ? C3 N2 C8 C13 94.5(3) . . . . ? C1 N2 C8 C9 88.9(3) . . . . ? C3 N2 C8 C9 -81.9(3) . . . . ? C13 C8 C9 C10 3.2(4) . . . . ? N2 C8 C9 C10 179.4(2) . . . . ? C13 C8 C9 C14 -174.0(2) . . . . ? N2 C8 C9 C14 2.2(4) . . . . ? C8 C9 C10 C11 -2.1(4) . . . . ? C14 C9 C10 C11 175.1(2) . . . . ? C9 C10 C11 C12 0.1(4) . . . . ? C10 C11 C12 C13 1.2(4) . . . . ? C9 C8 C13 C12 -2.0(4) . . . . ? N2 C8 C13 C12 -178.2(2) . . . . ? C9 C8 C13 C17 174.6(2) . . . . ? N2 C8 C13 C17 -1.6(4) . . . . ? C11 C12 C13 C8 -0.2(4) . . . . ? C11 C12 C13 C17 -176.9(2) . . . . ? C10 C9 C14 C15 38.3(4) . . . . ? C8 C9 C14 C15 -144.6(3) . . . . ? C10 C9 C14 C16 -84.6(3) . . . . ? C8 C9 C14 C16 92.4(3) . . . . ? C8 C13 C17 C18 -96.7(3) . . . . ? C12 C13 C17 C18 79.7(3) . . . . ? C8 C13 C17 C19 140.4(3) . . . . ? C12 C13 C17 C19 -43.2(3) . . . . ? C5 N4 C20 C21 83.0(3) . . . . ? C7 N4 C20 C21 -101.6(3) . . . . ? C5 N4 C20 C25 -98.3(3) . . . . ? C7 N4 C20 C25 77.1(3) . . . . ? C25 C20 C21 C22 5.5(4) . . . . ? N4 C20 C21 C22 -175.8(2) . . . . ? C25 C20 C21 C26 -169.8(2) . . . . ? N4 C20 C21 C26 8.8(4) . . . . ? C20 C21 C22 C23 -1.4(4) . . . . ? C26 C21 C22 C23 173.9(3) . . . . ? C21 C22 C23 C24 -2.7(5) . . . . ? C22 C23 C24 C25 2.8(4) . . . . ? C23 C24 C25 C20 1.1(4) . . . . ? C23 C24 C25 C29 -175.5(3) . . . . ? C21 C20 C25 C24 -5.4(4) . . . . ? N4 C20 C25 C24 175.9(2) . . . . ? C21 C20 C25 C29 171.1(3) . . . . ? N4 C20 C25 C29 -7.6(4) . . . . ? C22 C21 C26 C28 27.8(4) . . . . ? C20 C21 C26 C28 -157.1(3) . . . . ? C22 C21 C26 C27 -94.8(3) . . . . ? C20 C21 C26 C27 80.4(3) . . . . ? C24 C25 C29 C30 -42.6(3) . . . . ? C20 C25 C29 C30 140.9(3) . . . . ? C24 C25 C29 C31 79.0(3) . . . . ? C20 C25 C29 C31 -97.4(3) . . . . ? C5 Fe1 C32 C37 162.93(17) . . . . ? C1 Fe1 C32 C37 -49.6(2) . . . . ? C34 Fe1 C32 C37 101.61(19) . . . . ? C33 Fe1 C32 C37 130.8(3) . . . . ? C36 Fe1 C32 C37 27.37(17) . . . . ? C35 Fe1 C32 C37 63.80(18) . . . . ? C5 Fe1 C32 C33 32.2(3) . . . . ? C1 Fe1 C32 C33 179.62(16) . . . . ? C34 Fe1 C32 C33 -29.16(17) . . . . ? C36 Fe1 C32 C33 -103.40(19) . . . . ? C37 Fe1 C32 C33 -130.8(3) . . . . ? C35 Fe1 C32 C33 -66.97(18) . . . . ? C5 Fe1 C32 C38 -81.9(3) . . . . ? C1 Fe1 C32 C38 65.6(3) . . . . ? C34 Fe1 C32 C38 -143.2(3) . . . . ? C33 Fe1 C32 C38 -114.0(4) . . . . ? C36 Fe1 C32 C38 142.6(3) . . . . ? C37 Fe1 C32 C38 115.2(4) . . . . ? C35 Fe1 C32 C38 179.0(3) . . . . ? C37 C32 C33 C34 -1.1(4) . . . . ? C38 C32 C33 C34 -179.5(3) . . . . ? Fe1 C32 C33 C34 52.5(2) . . . . ? C37 C32 C33 Fe1 -53.6(2) . . . . ? C38 C32 C33 Fe1 128.1(3) . . . . ? C5 Fe1 C33 C34 67.90(18) . . . . ? C1 Fe1 C33 C34 -134.2(4) . . . . ? C36 Fe1 C33 C34 -65.41(18) . . . . ? C37 Fe1 C33 C34 -102.68(19) . . . . ? C32 Fe1 C33 C34 -133.0(3) . . . . ? C35 Fe1 C33 C34 -28.55(17) . . . . ? C5 Fe1 C33 C32 -159.13(17) . . . . ? C1 Fe1 C33 C32 -1.2(5) . . . . ? C34 Fe1 C33 C32 133.0(3) . . . . ? C36 Fe1 C33 C32 67.57(18) . . . . ? C37 Fe1 C33 C32 30.30(17) . . . . ? C35 Fe1 C33 C32 104.42(19) . . . . ? C32 C33 C34 C35 0.7(4) . . . . ? Fe1 C33 C34 C35 53.8(2) . . . . ? C32 C33 C34 Fe1 -53.1(2) . . . . ? C5 Fe1 C34 C33 -115.87(18) . . . . ? C1 Fe1 C34 C33 159.5(2) . . . . ? C36 Fe1 C34 C33 105.29(19) . . . . ? C37 Fe1 C34 C33 67.53(18) . . . . ? C32 Fe1 C34 C33 29.35(17) . . . . ? C35 Fe1 C34 C33 134.3(2) . . . . ? C5 Fe1 C34 C35 109.85(17) . . . . ? C1 Fe1 C34 C35 25.2(3) . . . . ? C33 Fe1 C34 C35 -134.3(2) . . . . ? C36 Fe1 C34 C35 -28.98(16) . . . . ? C37 Fe1 C34 C35 -66.74(17) . . . . ? C32 Fe1 C34 C35 -104.92(18) . . . . ? C33 C34 C35 C36 -1.2(4) . . . . ? Fe1 C34 C35 C36 51.9(2) . . . . ? C33 C34 C35 Fe1 -53.1(2) . . . . ? C5 Fe1 C35 C36 154.76(17) . . . . ? C1 Fe1 C35 C36 61.14(19) . . . . ? C34 Fe1 C35 C36 -132.3(2) . . . . ? C33 Fe1 C35 C36 -103.92(19) . . . . ? C37 Fe1 C35 C36 -29.08(17) . . . . ? C32 Fe1 C35 C36 -65.94(18) . . . . ? C5 Fe1 C35 C34 -72.89(18) . . . . ? C1 Fe1 C35 C34 -166.51(16) . . . . ? C33 Fe1 C35 C34 28.42(17) . . . . ? C36 Fe1 C35 C34 132.3(2) . . . . ? C37 Fe1 C35 C34 103.26(18) . . . . ? C32 Fe1 C35 C34 66.40(17) . . . . ? C34 C35 C36 C37 2.3(4) . . . . ? Fe1 C35 C36 C37 53.3(2) . . . . ? C34 C35 C36 Fe1 -50.9(2) . . . . ? C5 Fe1 C36 C35 -35.4(2) . . . . ? C1 Fe1 C36 C35 -125.86(18) . . . . ? C34 Fe1 C36 C35 29.88(17) . . . . ? C33 Fe1 C36 C35 67.49(18) . . . . ? C37 Fe1 C36 C35 133.2(3) . . . . ? C32 Fe1 C36 C35 105.73(19) . . . . ? C5 Fe1 C36 C37 -168.56(16) . . . . ? C1 Fe1 C36 C37 100.95(18) . . . . ? C34 Fe1 C36 C37 -103.31(19) . . . . ? C33 Fe1 C36 C37 -65.70(18) . . . . ? C32 Fe1 C36 C37 -27.46(16) . . . . ? C35 Fe1 C36 C37 -133.2(3) . . . . ? C35 C36 C37 C32 -2.9(4) . . . . ? Fe1 C36 C37 C32 50.8(2) . . . . ? C35 C36 C37 Fe1 -53.7(2) . . . . ? C33 C32 C37 C36 2.2(4) . . . . ? C38 C32 C37 C36 -179.4(3) . . . . ? Fe1 C32 C37 C36 -50.8(2) . . . . ? C33 C32 C37 Fe1 53.0(2) . . . . ? C38 C32 C37 Fe1 -128.6(3) . . . . ? C5 Fe1 C37 C36 48.8(6) . . . . ? C1 Fe1 C37 C36 -82.33(18) . . . . ? C34 Fe1 C37 C36 66.94(18) . . . . ? C33 Fe1 C37 C36 105.19(19) . . . . ? C32 Fe1 C37 C36 135.9(3) . . . . ? C35 Fe1 C37 C36 28.60(17) . . . . ? C5 Fe1 C37 C32 -87.1(6) . . . . ? C1 Fe1 C37 C32 141.80(17) . . . . ? C34 Fe1 C37 C32 -68.93(18) . . . . ? C33 Fe1 C37 C32 -30.68(17) . . . . ? C36 Fe1 C37 C32 -135.9(3) . . . . ? C35 Fe1 C37 C32 -107.27(19) . . . . ? C44 C39 C40 C41 0.9(5) . . . . ? C45 C39 C40 C41 178.4(3) . . . . ? C39 C40 C41 C42 -2.2(5) . . . . ? C40 C41 C42 C43 2.2(5) . . . . ? C41 C42 C43 C44 -0.9(5) . . . . ? C42 C43 C44 C39 -0.3(5) . . . . ? C40 C39 C44 C43 0.3(5) . . . . ? C45 C39 C44 C43 -177.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.882 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.073 #===END