# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1711 data_dr052 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H95 Fe2 N12' _chemical_formula_weight 892.01 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.342(2) _cell_length_b 12.080(2) _cell_length_c 21.651(4) _cell_angle_alpha 92.435(4) _cell_angle_beta 98.115(3) _cell_angle_gamma 106.672(4) _cell_volume 2555.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 'reflections from 60 data frames' _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 978 _exptl_absorpt_coefficient_mu 0.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.619623 _exptl_absorpt_correction_T_max 0.928075 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 16200 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.73 _reflns_number_total 11406 _reflns_number_gt 7957 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0300P)^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 11406 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.009 _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 0.37620(3) 0.03951(2) 0.218265(13) 0.02432(8) Uani 1 1 d . . . Fe2 Fe 0.55001(3) 0.26161(2) 0.314917(13) 0.02297(7) Uani 1 1 d . . . N1 N 0.19032(16) -0.08098(14) 0.17644(8) 0.0293(4) Uani 1 1 d . . . N2 N 0.38653(17) -0.08087(14) 0.14512(7) 0.0280(4) Uani 1 1 d . . . N3 N 0.17993(19) -0.22034(15) 0.09249(8) 0.0388(4) Uani 1 1 d . . . H3A H 0.1232 -0.2806 0.1045 0.047 Uiso 1 1 calc R . . N4 N 0.68158(16) 0.43474(13) 0.32504(8) 0.0276(4) Uani 1 1 d . . . N5 N 0.62502(16) 0.33687(13) 0.40692(7) 0.0271(4) Uani 1 1 d . . . N6 N 0.77012(18) 0.53008(14) 0.42960(8) 0.0355(4) Uani 1 1 d . . . H6A H 0.7399 0.5356 0.4648 0.043 Uiso 1 1 calc R . . N7 N 0.37688(17) 0.19898(13) 0.18658(7) 0.0271(4) Uani 1 1 d . . . N8 N 0.35832(16) 0.27334(13) 0.28347(7) 0.0246(3) Uani 1 1 d . . . N9 N 0.22890(17) 0.31598(13) 0.19228(8) 0.0305(4) Uani 1 1 d . . . H9A H 0.1607 0.2725 0.1655 0.037 Uiso 1 1 calc R . . N10 N 0.44224(16) -0.01187(13) 0.30354(7) 0.0248(3) Uani 1 1 d . . . N11 N 0.64111(16) 0.13340(13) 0.30163(7) 0.0246(3) Uani 1 1 d . . . N12 N 0.65174(16) -0.04790(13) 0.33926(8) 0.0283(4) Uani 1 1 d . . . H12A H 0.6233 -0.1190 0.3223 0.034 Uiso 1 1 calc R . . C1 C 0.0415(2) -0.10555(18) 0.16749(10) 0.0347(5) Uani 1 1 d . . . H1A H 0.0059 -0.1200 0.1221 0.042 Uiso 1 1 calc R . . C2 C 0.0078(2) 0.0008(2) 0.19309(12) 0.0449(6) Uani 1 1 d . . . H2A H 0.0492 0.0672 0.1714 0.067 Uiso 1 1 calc R . . H2B H 0.0434 0.0165 0.2375 0.067 Uiso 1 1 calc R . . H2C H -0.0906 -0.0138 0.1867 0.067 Uiso 1 1 calc R . . C3 C -0.0272(2) -0.2123(2) 0.19998(13) 0.0506(6) Uani 1 1 d . . . H3B H -0.0056 -0.2794 0.1833 0.076 Uiso 1 1 calc R . . H3C H -0.1255 -0.2262 0.1925 0.076 Uiso 1 1 calc R . . H3D H 0.0059 -0.1986 0.2447 0.076 Uiso 1 1 calc R . . C4 C 0.4771(2) -0.14291(18) 0.12285(9) 0.0307(5) Uani 1 1 d . . . H4A H 0.4200 -0.2189 0.1015 0.037 Uiso 1 1 calc R . . C5 C 0.5628(3) -0.0761(2) 0.07681(11) 0.0461(6) Uani 1 1 d . . . H5A H 0.5028 -0.0657 0.0403 0.069 Uiso 1 1 calc R . . H5B H 0.6219 -0.1194 0.0640 0.069 Uiso 1 1 calc R . . H5C H 0.6182 -0.0008 0.0969 0.069 Uiso 1 1 calc R . . C6 C 0.5724(2) -0.1641(2) 0.17831(10) 0.0422(6) Uani 1 1 d . . . H6B H 0.5187 -0.2071 0.2076 0.063 Uiso 1 1 calc R . . H6C H 0.6307 -0.0903 0.1990 0.063 Uiso 1 1 calc R . . H6D H 0.6285 -0.2085 0.1636 0.063 Uiso 1 1 calc R . . C7 C 0.1960(3) -0.2197(2) 0.02597(11) 0.0507(6) Uani 1 1 d . . . H7A H 0.2905 -0.1726 0.0236 0.061 Uiso 1 1 calc R . . C8 C 0.1770(4) -0.3393(3) -0.00162(14) 0.1004(14) Uani 1 1 d . . . H8A H 0.2450 -0.3705 0.0207 0.151 Uiso 1 1 calc R . . H8B H 0.1875 -0.3372 -0.0454 0.151 Uiso 1 1 calc R . . H8C H 0.0863 -0.3881 0.0019 0.151 Uiso 1 1 calc R . . C9 C 0.0986(4) -0.1644(3) -0.01117(14) 0.0820(10) Uani 1 1 d . . . H9B H 0.1131 -0.1638 -0.0545 0.123 Uiso 1 1 calc R . . H9C H 0.1155 -0.0854 0.0065 0.123 Uiso 1 1 calc R . . H9D H 0.0050 -0.2087 -0.0092 0.123 Uiso 1 1 calc R . . C10 C 0.2515(2) -0.12887(17) 0.13687(9) 0.0300(5) Uani 1 1 d . . . C11 C 0.7132(2) 0.53785(16) 0.29017(9) 0.0316(5) Uani 1 1 d . . . H11A H 0.8110 0.5814 0.3030 0.038 Uiso 1 1 calc R . . C12 C 0.6270(2) 0.61815(18) 0.30238(11) 0.0424(6) Uani 1 1 d . . . H12B H 0.6448 0.6443 0.3466 0.064 Uiso 1 1 calc R . . H12C H 0.5308 0.5763 0.2902 0.064 Uiso 1 1 calc R . . H12D H 0.6508 0.6846 0.2781 0.064 Uiso 1 1 calc R . . C13 C 0.6891(3) 0.49778(19) 0.22074(10) 0.0453(6) Uani 1 1 d . . . H13A H 0.7457 0.4484 0.2136 0.068 Uiso 1 1 calc R . . H13B H 0.7125 0.5648 0.1968 0.068 Uiso 1 1 calc R . . H13C H 0.5936 0.4546 0.2076 0.068 Uiso 1 1 calc R . . C14 C 0.6433(2) 0.30961(17) 0.47190(9) 0.0308(4) Uani 1 1 d . . . H14A H 0.7398 0.3475 0.4908 0.037 Uiso 1 1 calc R . . C15 C 0.5519(3) 0.3512(2) 0.51132(10) 0.0450(6) Uani 1 1 d . . . H15A H 0.5727 0.4349 0.5118 0.067 Uiso 1 1 calc R . . H15B H 0.5683 0.3301 0.5538 0.067 Uiso 1 1 calc R . . H15C H 0.4567 0.3151 0.4934 0.067 Uiso 1 1 calc R . . C16 C 0.6157(3) 0.17958(19) 0.47253(10) 0.0448(6) Uani 1 1 d . . . H16A H 0.6750 0.1543 0.4479 0.067 Uiso 1 1 calc R . . H16B H 0.5210 0.1409 0.4548 0.067 Uiso 1 1 calc R . . H16C H 0.6334 0.1602 0.5153 0.067 Uiso 1 1 calc R . . C17 C 0.8947(2) 0.62046(17) 0.42185(10) 0.0364(5) Uani 1 1 d . . . H17A H 0.8709 0.6674 0.3881 0.044 Uiso 1 1 calc R . . C18 C 1.0044(2) 0.57024(19) 0.40385(12) 0.0474(6) Uani 1 1 d . . . H18A H 0.9707 0.5238 0.3641 0.071 Uiso 1 1 calc R . . H18B H 1.0271 0.5220 0.4358 0.071 Uiso 1 1 calc R . . H18C H 1.0854 0.6329 0.4002 0.071 Uiso 1 1 calc R . . C19 C 0.9449(3) 0.6984(2) 0.48236(11) 0.0513(6) Uani 1 1 d . . . H19A H 0.8725 0.7286 0.4927 0.077 Uiso 1 1 calc R . . H19B H 1.0235 0.7623 0.4773 0.077 Uiso 1 1 calc R . . H19C H 0.9708 0.6542 0.5158 0.077 Uiso 1 1 calc R . . C20 C 0.6955(2) 0.43751(16) 0.38759(9) 0.0272(4) Uani 1 1 d . . . C21 C 0.3816(2) 0.22342(18) 0.11996(9) 0.0333(5) Uani 1 1 d . . . H21A H 0.3748 0.3029 0.1154 0.040 Uiso 1 1 calc R . . C22 C 0.2644(2) 0.1397(2) 0.07555(10) 0.0439(6) Uani 1 1 d . . . H22A H 0.1782 0.1438 0.0866 0.066 Uiso 1 1 calc R . . H22B H 0.2704 0.0614 0.0786 0.066 Uiso 1 1 calc R . . H22C H 0.2698 0.1603 0.0330 0.066 Uiso 1 1 calc R . . C23 C 0.5172(2) 0.2190(2) 0.10248(10) 0.0428(6) Uani 1 1 d . . . H23A H 0.5915 0.2734 0.1307 0.064 Uiso 1 1 calc R . . H23B H 0.5217 0.2395 0.0598 0.064 Uiso 1 1 calc R . . H23C H 0.5248 0.1412 0.1057 0.064 Uiso 1 1 calc R . . C24 C 0.2645(2) 0.29889(17) 0.32385(9) 0.0292(4) Uani 1 1 d . . . H24A H 0.1806 0.3027 0.2967 0.035 Uiso 1 1 calc R . . C25 C 0.2251(2) 0.19938(19) 0.36559(10) 0.0363(5) Uani 1 1 d . . . H25A H 0.1839 0.1269 0.3396 0.054 Uiso 1 1 calc R . . H25B H 0.1601 0.2132 0.3909 0.054 Uiso 1 1 calc R . . H25C H 0.3062 0.1949 0.3927 0.054 Uiso 1 1 calc R . . C26 C 0.3257(2) 0.41291(18) 0.36475(10) 0.0385(5) Uani 1 1 d . . . H26A H 0.3501 0.4762 0.3384 0.058 Uiso 1 1 calc R . . H26B H 0.4068 0.4098 0.3924 0.058 Uiso 1 1 calc R . . H26C H 0.2592 0.4254 0.3896 0.058 Uiso 1 1 calc R . . C27 C 0.2365(2) 0.43864(17) 0.20360(10) 0.0334(5) Uani 1 1 d . . . H27A H 0.2949 0.4690 0.2446 0.040 Uiso 1 1 calc R . . C28 C 0.3013(3) 0.5092(2) 0.15358(13) 0.0572(7) Uani 1 1 d . . . H28A H 0.3899 0.4981 0.1515 0.086 Uiso 1 1 calc R . . H28B H 0.3127 0.5907 0.1640 0.086 Uiso 1 1 calc R . . H28C H 0.2428 0.4839 0.1134 0.086 Uiso 1 1 calc R . . C29 C 0.0960(3) 0.4521(2) 0.20657(15) 0.0621(8) Uani 1 1 d . . . H29A H 0.0558 0.4062 0.2385 0.093 Uiso 1 1 calc R . . H29B H 0.0381 0.4255 0.1663 0.093 Uiso 1 1 calc R . . H29C H 0.1045 0.5331 0.2168 0.093 Uiso 1 1 calc R . . C30 C 0.32313(19) 0.26407(16) 0.22139(9) 0.0250(4) Uani 1 1 d . . . C31 C 0.3690(2) -0.11034(17) 0.33643(9) 0.0298(4) Uani 1 1 d . . . H31A H 0.4306 -0.1149 0.3750 0.036 Uiso 1 1 calc R . . C32 C 0.2427(2) -0.08689(19) 0.35580(11) 0.0391(5) Uani 1 1 d . . . H32A H 0.2697 -0.0139 0.3816 0.059 Uiso 1 1 calc R . . H32B H 0.1979 -0.1491 0.3794 0.059 Uiso 1 1 calc R . . H32C H 0.1802 -0.0828 0.3187 0.059 Uiso 1 1 calc R . . C33 C 0.3296(2) -0.22659(17) 0.29755(11) 0.0378(5) Uani 1 1 d . . . H33A H 0.4110 -0.2405 0.2857 0.057 Uiso 1 1 calc R . . H33B H 0.2664 -0.2253 0.2602 0.057 Uiso 1 1 calc R . . H33C H 0.2863 -0.2880 0.3220 0.057 Uiso 1 1 calc R . . C34 C 0.7827(2) 0.15965(17) 0.28769(9) 0.0291(4) Uani 1 1 d . . . H34A H 0.8126 0.0891 0.2917 0.035 Uiso 1 1 calc R . . C35 C 0.7843(2) 0.19271(19) 0.22039(10) 0.0404(5) Uani 1 1 d . . . H35A H 0.7216 0.1299 0.1919 0.061 Uiso 1 1 calc R . . H35B H 0.8760 0.2067 0.2106 0.061 Uiso 1 1 calc R . . H35C H 0.7563 0.2624 0.2160 0.061 Uiso 1 1 calc R . . C36 C 0.8808(2) 0.25674(19) 0.33293(10) 0.0384(5) Uani 1 1 d . . . H36A H 0.8811 0.2338 0.3753 0.058 Uiso 1 1 calc R . . H36B H 0.8520 0.3262 0.3299 0.058 Uiso 1 1 calc R . . H36C H 0.9722 0.2722 0.3225 0.058 Uiso 1 1 calc R . . C37 C 0.7708(2) -0.01982(17) 0.38914(9) 0.0308(5) Uani 1 1 d . . . H37A H 0.8050 0.0655 0.3982 0.037 Uiso 1 1 calc R . . C38 C 0.7292(3) -0.0737(2) 0.44867(10) 0.0457(6) Uani 1 1 d . . . H38A H 0.6585 -0.0442 0.4618 0.068 Uiso 1 1 calc R . . H38B H 0.8081 -0.0538 0.4816 0.068 Uiso 1 1 calc R . . H38C H 0.6945 -0.1574 0.4404 0.068 Uiso 1 1 calc R . . C39 C 0.8857(2) -0.0622(2) 0.36903(12) 0.0448(6) Uani 1 1 d . . . H39A H 0.9123 -0.0265 0.3317 0.067 Uiso 1 1 calc R . . H39B H 0.8539 -0.1458 0.3603 0.067 Uiso 1 1 calc R . . H39C H 0.9637 -0.0411 0.4024 0.067 Uiso 1 1 calc R . . C40 C 0.5791(2) 0.02603(16) 0.31590(8) 0.0238(4) Uani 1 1 d . . . C41 C 0.2679(9) 0.3831(6) -0.0499(3) 0.191(3) Uani 1 1 d . . . H41A H 0.2314 0.3219 -0.0837 0.286 Uiso 1 1 calc R . . H41B H 0.2250 0.4441 -0.0571 0.286 Uiso 1 1 calc R . . H41C H 0.2492 0.3518 -0.0105 0.286 Uiso 1 1 calc R . . C42 C 0.3902(8) 0.4225(10) -0.0479(4) 0.225(5) Uani 1 1 d . . . H42A H 0.4086 0.4669 -0.0842 0.270 Uiso 1 1 calc R . . H42B H 0.4311 0.3588 -0.0499 0.270 Uiso 1 1 calc R . . C43 C 0.4442(6) 0.4879(6) 0.0022(4) 0.139(2) Uani 1 1 d . . . H43A H 0.4116 0.5564 0.0038 0.167 Uiso 1 1 calc R . . H43B H 0.4261 0.4462 0.0394 0.167 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 0.02466(15) 0.02551(15) 0.02539(16) 0.00597(12) 0.00495(12) 0.01051(12) Fe2 0.01978(14) 0.02373(15) 0.02754(16) 0.00421(12) 0.00407(12) 0.00939(11) N1 0.0229(9) 0.0309(9) 0.0351(10) 0.0010(7) 0.0046(7) 0.0096(7) N2 0.0269(9) 0.0320(9) 0.0287(9) 0.0025(7) 0.0045(7) 0.0144(7) N3 0.0370(11) 0.0346(10) 0.0414(11) -0.0048(8) 0.0033(9) 0.0079(8) N4 0.0259(9) 0.0254(9) 0.0302(9) 0.0073(7) 0.0023(7) 0.0061(7) N5 0.0278(9) 0.0267(9) 0.0269(9) 0.0063(7) 0.0035(7) 0.0084(7) N6 0.0355(10) 0.0335(10) 0.0321(10) 0.0001(8) 0.0029(8) 0.0034(8) N7 0.0307(9) 0.0293(9) 0.0257(9) 0.0075(7) 0.0078(7) 0.0138(7) N8 0.0229(8) 0.0274(8) 0.0264(9) 0.0033(7) 0.0055(7) 0.0111(7) N9 0.0285(9) 0.0268(9) 0.0363(10) 0.0043(7) -0.0029(8) 0.0120(7) N10 0.0235(8) 0.0257(8) 0.0271(8) 0.0087(7) 0.0064(7) 0.0083(7) N11 0.0216(8) 0.0253(8) 0.0300(9) 0.0067(7) 0.0073(7) 0.0096(7) N12 0.0262(9) 0.0228(8) 0.0368(10) 0.0038(7) -0.0001(7) 0.0106(7) C1 0.0239(11) 0.0394(12) 0.0402(12) 0.0018(10) 0.0020(9) 0.0103(9) C2 0.0291(12) 0.0476(14) 0.0630(16) 0.0040(12) 0.0114(11) 0.0177(11) C3 0.0290(12) 0.0477(14) 0.0736(18) 0.0078(13) 0.0110(12) 0.0074(11) C4 0.0314(11) 0.0336(11) 0.0317(11) 0.0014(9) 0.0084(9) 0.0152(9) C5 0.0536(16) 0.0561(15) 0.0409(13) 0.0099(12) 0.0228(12) 0.0277(13) C6 0.0382(13) 0.0586(15) 0.0413(13) 0.0112(11) 0.0114(11) 0.0289(12) C7 0.0415(14) 0.0673(17) 0.0403(14) -0.0118(12) -0.0041(11) 0.0187(13) C8 0.169(4) 0.087(2) 0.057(2) -0.0212(18) -0.005(2) 0.071(3) C9 0.113(3) 0.075(2) 0.0571(19) 0.0000(16) -0.0134(19) 0.040(2) C10 0.0323(11) 0.0306(11) 0.0295(11) 0.0055(9) 0.0013(9) 0.0147(9) C11 0.0284(11) 0.0264(11) 0.0363(12) 0.0086(9) -0.0011(9) 0.0046(9) C12 0.0430(14) 0.0351(12) 0.0507(14) 0.0114(11) 0.0006(11) 0.0161(11) C13 0.0572(16) 0.0363(13) 0.0395(13) 0.0141(10) 0.0070(12) 0.0082(11) C14 0.0304(11) 0.0346(11) 0.0272(11) 0.0065(9) 0.0024(9) 0.0098(9) C15 0.0612(16) 0.0450(14) 0.0345(13) 0.0035(11) 0.0140(12) 0.0217(12) C16 0.0672(17) 0.0432(13) 0.0364(13) 0.0177(11) 0.0188(12) 0.0288(13) C17 0.0348(12) 0.0246(11) 0.0432(13) 0.0060(9) -0.0058(10) 0.0038(9) C18 0.0333(13) 0.0380(13) 0.0635(16) 0.0076(12) -0.0001(12) 0.0022(11) C19 0.0542(16) 0.0359(13) 0.0521(15) 0.0024(11) -0.0115(13) 0.0045(12) C20 0.0219(10) 0.0268(10) 0.0347(11) 0.0024(9) 0.0027(9) 0.0107(8) C21 0.0445(13) 0.0351(11) 0.0271(11) 0.0111(9) 0.0104(10) 0.0192(10) C22 0.0513(15) 0.0529(15) 0.0294(12) 0.0085(11) 0.0018(11) 0.0198(12) C23 0.0494(15) 0.0521(14) 0.0335(12) 0.0118(11) 0.0169(11) 0.0194(12) C24 0.0243(10) 0.0352(11) 0.0328(11) 0.0035(9) 0.0075(9) 0.0148(9) C25 0.0337(12) 0.0443(13) 0.0357(12) 0.0068(10) 0.0123(10) 0.0154(10) C26 0.0414(13) 0.0408(13) 0.0399(13) -0.0003(10) 0.0110(11) 0.0211(11) C27 0.0355(12) 0.0266(11) 0.0413(12) 0.0075(9) 0.0039(10) 0.0148(9) C28 0.0655(19) 0.0436(15) 0.0728(19) 0.0266(13) 0.0249(15) 0.0228(13) C29 0.0507(16) 0.0436(15) 0.107(2) 0.0191(15) 0.0261(16) 0.0296(13) C30 0.0204(9) 0.0237(10) 0.0314(11) 0.0061(8) 0.0040(8) 0.0068(8) C31 0.0264(11) 0.0320(11) 0.0334(11) 0.0114(9) 0.0089(9) 0.0092(9) C32 0.0354(12) 0.0403(13) 0.0471(14) 0.0150(10) 0.0186(11) 0.0125(10) C33 0.0364(12) 0.0294(11) 0.0502(14) 0.0112(10) 0.0141(11) 0.0092(10) C34 0.0234(10) 0.0297(11) 0.0410(12) 0.0112(9) 0.0141(9) 0.0133(9) C35 0.0416(13) 0.0408(13) 0.0451(13) 0.0137(11) 0.0213(11) 0.0139(11) C36 0.0210(10) 0.0436(13) 0.0507(14) 0.0078(11) 0.0087(10) 0.0079(10) C37 0.0278(11) 0.0299(11) 0.0361(12) 0.0084(9) 0.0024(9) 0.0111(9) C38 0.0493(15) 0.0524(15) 0.0403(13) 0.0170(11) 0.0055(11) 0.0221(12) C39 0.0302(12) 0.0485(14) 0.0633(16) 0.0169(12) 0.0089(11) 0.0211(11) C40 0.0278(10) 0.0261(10) 0.0205(10) 0.0032(8) 0.0051(8) 0.0117(8) C41 0.305(11) 0.127(5) 0.134(5) 0.014(4) 0.052(7) 0.045(6) C42 0.169(9) 0.350(15) 0.150(7) 0.027(8) 0.049(7) 0.054(9) C43 0.129(6) 0.150(5) 0.154(5) 0.006(4) 0.059(5) 0.050(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 N10 2.0604(15) . ? Fe1 N7 2.0707(15) . ? Fe1 N1 2.1037(17) . ? Fe1 N2 2.1390(16) . ? Fe2 N8 2.0500(16) . ? Fe2 N11 2.0604(15) . ? Fe2 N5 2.0979(16) . ? Fe2 N4 2.1255(16) . ? N1 C10 1.338(2) . ? N1 C1 1.464(2) . ? N2 C10 1.332(3) . ? N2 C4 1.473(2) . ? N3 C10 1.390(3) . ? N3 C7 1.473(3) . ? N4 C20 1.340(2) . ? N4 C11 1.464(2) . ? N5 C20 1.344(2) . ? N5 C14 1.457(2) . ? N6 C20 1.376(3) . ? N6 C17 1.466(3) . ? N7 C30 1.347(2) . ? N7 C21 1.489(2) . ? N8 C30 1.333(2) . ? N8 C24 1.480(2) . ? N9 C30 1.397(2) . ? N9 C27 1.469(2) . ? N10 C40 1.340(2) . ? N10 C31 1.484(2) . ? N11 C40 1.342(2) . ? N11 C34 1.484(2) . ? N12 C40 1.391(2) . ? N12 C37 1.467(3) . ? C1 C2 1.526(3) . ? C1 C3 1.535(3) . ? C4 C6 1.522(3) . ? C4 C5 1.529(3) . ? C7 C8 1.488(4) . ? C7 C9 1.520(4) . ? C11 C13 1.523(3) . ? C11 C12 1.532(3) . ? C14 C16 1.515(3) . ? C14 C15 1.529(3) . ? C17 C19 1.515(3) . ? C17 C18 1.519(3) . ? C21 C22 1.517(3) . ? C21 C23 1.518(3) . ? C24 C26 1.523(3) . ? C24 C25 1.531(3) . ? C27 C29 1.517(3) . ? C27 C28 1.518(3) . ? C31 C32 1.523(3) . ? C31 C33 1.524(3) . ? C34 C36 1.518(3) . ? C34 C35 1.528(3) . ? C37 C39 1.529(3) . ? C37 C38 1.529(3) . ? C41 C42 1.211(9) . ? C42 C43 1.272(10) . ? C42 C43 1.858(11) 2_665 ? C43 C43 1.126(10) 2_665 ? C43 C42 1.858(11) 2_665 ? 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 N10 Fe1 N7 133.53(6) . . ? N10 Fe1 N1 109.69(6) . . ? N7 Fe1 N1 107.15(7) . . ? N10 Fe1 N2 109.17(6) . . ? N7 Fe1 N2 112.17(6) . . ? N1 Fe1 N2 63.36(6) . . ? N8 Fe2 N11 132.32(6) . . ? N8 Fe2 N5 112.32(6) . . ? N11 Fe2 N5 106.71(6) . . ? N8 Fe2 N4 105.51(6) . . ? N11 Fe2 N4 115.93(6) . . ? N5 Fe2 N4 63.62(6) . . ? C10 N1 C1 121.47(18) . . ? C10 N1 Fe1 92.43(12) . . ? C1 N1 Fe1 143.87(13) . . ? C10 N2 C4 121.32(17) . . ? C10 N2 Fe1 91.06(12) . . ? C4 N2 Fe1 142.61(13) . . ? C10 N3 C7 122.87(19) . . ? C20 N4 C11 124.32(16) . . ? C20 N4 Fe2 91.57(12) . . ? C11 N4 Fe2 140.24(13) . . ? C20 N5 C14 122.80(17) . . ? C20 N5 Fe2 92.66(12) . . ? C14 N5 Fe2 142.95(13) . . ? C20 N6 C17 127.42(17) . . ? C30 N7 C21 117.48(15) . . ? C30 N7 Fe1 115.63(12) . . ? C21 N7 Fe1 122.65(12) . . ? C30 N8 C24 119.54(16) . . ? C30 N8 Fe2 115.25(12) . . ? C24 N8 Fe2 125.06(12) . . ? C30 N9 C27 124.84(17) . . ? C40 N10 C31 118.79(15) . . ? C40 N10 Fe1 109.36(11) . . ? C31 N10 Fe1 127.80(13) . . ? C40 N11 C34 118.58(15) . . ? C40 N11 Fe2 118.47(12) . . ? C34 N11 Fe2 122.07(12) . . ? C40 N12 C37 127.52(16) . . ? N1 C1 C2 108.64(17) . . ? N1 C1 C3 112.05(17) . . ? C2 C1 C3 110.02(18) . . ? N2 C4 C6 109.77(16) . . ? N2 C4 C5 112.35(16) . . ? C6 C4 C5 108.96(18) . . ? N3 C7 C8 110.6(2) . . ? N3 C7 C9 111.6(2) . . ? C8 C7 C9 110.9(2) . . ? N2 C10 N1 113.14(18) . . ? N2 C10 N3 124.20(18) . . ? N1 C10 N3 122.66(19) . . ? N4 C11 C13 108.07(16) . . ? N4 C11 C12 112.41(17) . . ? C13 C11 C12 110.34(17) . . ? N5 C14 C16 108.25(16) . . ? N5 C14 C15 113.46(16) . . ? C16 C14 C15 110.22(17) . . ? N6 C17 C19 107.98(18) . . ? N6 C17 C18 112.31(17) . . ? C19 C17 C18 111.45(19) . . ? N4 C20 N5 112.14(17) . . ? N4 C20 N6 126.46(18) . . ? N5 C20 N6 121.39(18) . . ? N7 C21 C22 112.27(17) . . ? N7 C21 C23 109.92(16) . . ? C22 C21 C23 109.94(18) . . ? N8 C24 C26 113.33(17) . . ? N8 C24 C25 108.60(15) . . ? C26 C24 C25 109.33(17) . . ? N9 C27 C29 111.05(18) . . ? N9 C27 C28 110.85(18) . . ? C29 C27 C28 110.44(18) . . ? N8 C30 N7 118.36(16) . . ? N8 C30 N9 121.80(16) . . ? N7 C30 N9 119.80(17) . . ? N10 C31 C32 109.54(15) . . ? N10 C31 C33 113.07(16) . . ? C32 C31 C33 110.38(17) . . ? N11 C34 C36 111.38(16) . . ? N11 C34 C35 109.27(16) . . ? C36 C34 C35 110.20(17) . . ? N12 C37 C39 111.13(17) . . ? N12 C37 C38 109.95(17) . . ? C39 C37 C38 110.20(17) . . ? N10 C40 N11 117.74(16) . . ? N10 C40 N12 119.75(16) . . ? N11 C40 N12 122.40(17) . . ? C41 C42 C43 110.8(9) . . ? C41 C42 C43 147.1(9) . 2_665 ? C43 C42 C43 36.4(5) . 2_665 ? C43 C43 C42 101.4(9) 2_665 . ? C43 C43 C42 42.1(6) 2_665 2_665 ? C42 C43 C42 143.6(5) . 2_665 ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 28.73 _diffrn_measured_fraction_theta_full 0.862 _refine_diff_density_max 0.483 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.058 ### END data_dr165a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H79 Fe2 N11' _chemical_formula_weight 789.81 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 19.572(6) _cell_length_b 12.747(4) _cell_length_c 18.649(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4653(3) _cell_formula_units_Z 4 _cell_measurement_temperature 238(2) _cell_measurement_reflns_used 'reflections from 60 data frames' _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 28.29 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max .40 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.302480 _exptl_absorpt_correction_T_max 0.928074 _exptl_absorpt_process_details 'Blessing,R., Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 238(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 29549 _diffrn_reflns_av_R_equivalents 0.2975 _diffrn_reflns_av_sigmaI/netI 0.2467 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 20.81 _reflns_number_total 2444 _reflns_number_gt 1426 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0600P)^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 2444 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.003 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 Fe Fe 0.30412(4) 0.07473(6) 0.35751(4) 0.0375(3) Uani 1 1 d . . . N1 N 0.3466(3) -0.0502(4) 0.2972(3) 0.0383(14) Uani 1 1 d . . . N2 N 0.3351(2) -0.0538(3) 0.4155(3) 0.0375(13) Uani 1 1 d . . . N3 N 0.3896(3) -0.2010(3) 0.3595(3) 0.0486(14) Uani 1 1 d . . . H3A H 0.3758 -0.2499 0.3303 0.058 Uiso 1 1 calc R . . N4 N 0.3570(3) 0.2140(3) 0.3618(2) 0.0367(13) Uani 1 1 d . . . N5 N 0.2958(3) 0.3778(3) 0.3341(2) 0.0353(13) Uani 1 1 d . . . N6 N 0.2500 0.2500 0.4063(4) 0.052(2) Uani 1 2 d S . . C1 C 0.3782(3) -0.0807(5) 0.2291(3) 0.0434(17) Uani 1 1 d . . . H1A H 0.4256 -0.1041 0.2383 0.052 Uiso 1 1 calc R . . C2 C 0.3798(4) 0.0141(5) 0.1798(3) 0.075(3) Uani 1 1 d . . . H2A H 0.4057 0.0700 0.2023 0.113 Uiso 1 1 calc R . . H2B H 0.3334 0.0379 0.1710 0.113 Uiso 1 1 calc R . . H2C H 0.4011 -0.0050 0.1348 0.113 Uiso 1 1 calc R . . C3 C 0.3390(4) -0.1693(5) 0.1918(3) 0.066(2) Uani 1 1 d . . . H3B H 0.3385 -0.2309 0.2224 0.099 Uiso 1 1 calc R . . H3C H 0.3612 -0.1863 0.1468 0.099 Uiso 1 1 calc R . . H3D H 0.2924 -0.1470 0.1826 0.099 Uiso 1 1 calc R . . C4 C 0.3154(4) -0.1068(4) 0.4814(3) 0.051(2) Uani 1 1 d . . . H4A H 0.3305 -0.1808 0.4784 0.061 Uiso 1 1 calc R . . C5 C 0.2373(4) -0.1050(5) 0.4894(4) 0.078(3) Uani 1 1 d . . . H5A H 0.2166 -0.1402 0.4488 0.117 Uiso 1 1 calc R . . H5B H 0.2216 -0.0328 0.4912 0.117 Uiso 1 1 calc R . . H5C H 0.2245 -0.1407 0.5334 0.117 Uiso 1 1 calc R . . C6 C 0.3503(4) -0.0559(5) 0.5452(3) 0.083(3) Uani 1 1 d . . . H6A H 0.3994 -0.0591 0.5390 0.124 Uiso 1 1 calc R . . H6B H 0.3376 -0.0928 0.5887 0.124 Uiso 1 1 calc R . . H6C H 0.3361 0.0168 0.5488 0.124 Uiso 1 1 calc R . . C7 C 0.4457(4) -0.2240(5) 0.4094(4) 0.054(2) Uani 1 1 d . . . H7A H 0.4303 -0.2071 0.4586 0.065 Uiso 1 1 calc R . . C8 C 0.5071(4) -0.1598(7) 0.3933(5) 0.136(4) Uani 1 1 d . . . H8A H 0.4957 -0.0860 0.3975 0.205 Uiso 1 1 calc R . . H8B H 0.5224 -0.1744 0.3448 0.205 Uiso 1 1 calc R . . H8C H 0.5432 -0.1770 0.4269 0.205 Uiso 1 1 calc R . . C9 C 0.4616(4) -0.3395(5) 0.4061(4) 0.108(3) Uani 1 1 d . . . H9A H 0.4211 -0.3794 0.4185 0.163 Uiso 1 1 calc R . . H9B H 0.4979 -0.3558 0.4397 0.163 Uiso 1 1 calc R . . H9C H 0.4761 -0.3579 0.3580 0.163 Uiso 1 1 calc R . . C10 C 0.3577(3) -0.1033(4) 0.3573(4) 0.0371(15) Uani 1 1 d . . . C11 C 0.4284(3) 0.2390(5) 0.3429(3) 0.0471(18) Uani 1 1 d . . . H11A H 0.4304 0.2642 0.2927 0.057 Uiso 1 1 calc R . . C12 C 0.4569(3) 0.3231(5) 0.3925(3) 0.061(2) Uani 1 1 d . . . H12A H 0.4304 0.3870 0.3871 0.091 Uiso 1 1 calc R . . H12B H 0.5042 0.3370 0.3802 0.091 Uiso 1 1 calc R . . H12C H 0.4542 0.2991 0.4417 0.091 Uiso 1 1 calc R . . C13 C 0.4710(3) 0.1386(5) 0.3499(4) 0.071(2) Uani 1 1 d . . . H13A H 0.4530 0.0855 0.3178 0.106 Uiso 1 1 calc R . . H13B H 0.4688 0.1134 0.3989 0.106 Uiso 1 1 calc R . . H13C H 0.5181 0.1535 0.3374 0.106 Uiso 1 1 calc R . . C14 C 0.3387(3) 0.4178(5) 0.2758(3) 0.0448(17) Uani 1 1 d . . . H14A H 0.3870 0.4029 0.2877 0.054 Uiso 1 1 calc R . . C15 C 0.3302(4) 0.5359(5) 0.2698(4) 0.075(2) Uani 1 1 d . . . H15A H 0.3431 0.5686 0.3147 0.113 Uiso 1 1 calc R . . H15B H 0.2828 0.5523 0.2592 0.113 Uiso 1 1 calc R . . H15C H 0.3591 0.5623 0.2316 0.113 Uiso 1 1 calc R . . C16 C 0.3217(4) 0.3619(5) 0.2076(3) 0.071(2) Uani 1 1 d . . . H16A H 0.3294 0.2872 0.2136 0.106 Uiso 1 1 calc R . . H16B H 0.3505 0.3881 0.1692 0.106 Uiso 1 1 calc R . . H16C H 0.2741 0.3740 0.1956 0.106 Uiso 1 1 calc R . . C17 C 0.256(2) 0.268(3) 0.4805(6) 0.078(10) Uani 0.50 1 d P . 1 H17A H 0.2335 0.3372 0.4803 0.093 Uiso 0.50 1 calc PR . 1 C18 C 0.3074(4) 0.2956(5) 0.5193(3) 0.056(2) Uani 1 1 d . A 1 H18A H 0.2959 0.2879 0.5696 0.084 Uiso 1 1 calc R A 1 H18B H 0.3186 0.3683 0.5094 0.084 Uiso 1 1 calc R A 1 H18C H 0.3465 0.2517 0.5080 0.084 Uiso 1 1 calc R A 1 C19 C 0.3074(3) 0.2861(4) 0.3635(3) 0.0346(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0489(6) 0.0236(5) 0.0398(5) -0.0008(4) 0.0000(5) 0.0019(5) N1 0.056(4) 0.033(3) 0.025(3) -0.002(3) 0.003(3) 0.008(3) N2 0.054(4) 0.022(3) 0.037(3) 0.004(3) 0.004(3) 0.003(2) N3 0.071(4) 0.021(3) 0.054(3) -0.011(3) -0.017(3) 0.013(3) N4 0.037(4) 0.033(3) 0.040(3) 0.000(3) 0.000(3) 0.003(3) N5 0.048(4) 0.020(3) 0.038(3) 0.008(2) -0.003(3) -0.005(3) N6 0.049(6) 0.078(6) 0.028(5) 0.000 0.000 -0.021(5) C1 0.057(5) 0.039(4) 0.034(4) 0.005(4) 0.006(3) 0.010(4) C2 0.113(8) 0.064(5) 0.048(4) 0.012(4) 0.023(4) 0.009(5) C3 0.080(6) 0.069(5) 0.049(5) -0.015(4) -0.007(4) 0.015(4) C4 0.084(7) 0.026(4) 0.042(5) 0.003(3) 0.004(4) 0.011(4) C5 0.085(7) 0.052(5) 0.097(6) 0.010(4) 0.040(5) 0.003(4) C6 0.153(9) 0.058(5) 0.036(4) 0.000(4) -0.018(5) 0.007(5) C7 0.060(6) 0.042(4) 0.059(5) -0.001(4) -0.011(4) 0.013(4) C8 0.074(8) 0.148(9) 0.187(10) 0.067(8) -0.058(7) -0.025(7) C9 0.129(9) 0.070(6) 0.126(7) -0.018(5) -0.054(6) 0.048(6) C10 0.042(4) 0.033(4) 0.036(4) -0.006(4) 0.000(4) -0.004(3) C11 0.042(5) 0.040(4) 0.059(5) 0.013(3) 0.004(4) 0.003(3) C12 0.048(5) 0.065(5) 0.069(5) 0.003(4) -0.003(4) -0.016(4) C13 0.045(5) 0.051(4) 0.116(6) 0.006(5) 0.000(5) 0.002(4) C14 0.047(5) 0.033(4) 0.055(5) 0.018(4) 0.001(3) 0.002(3) C15 0.061(6) 0.051(5) 0.113(7) 0.034(4) 0.000(5) -0.010(4) C16 0.094(7) 0.079(5) 0.040(5) 0.020(4) 0.013(4) -0.004(5) C17 0.072(15) 0.14(3) 0.016(7) -0.013(10) 0.042(13) -0.105(18) C18 0.083(6) 0.041(4) 0.043(4) 0.000(3) -0.018(4) 0.002(4) C19 0.037(4) 0.044(4) 0.024(3) -0.003(3) -0.001(4) -0.009(4) _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 Fe N2 2.054(4) . ? Fe N4 2.056(5) . ? Fe N5 2.093(5) 2 ? Fe N1 2.119(4) . ? Fe C10 2.499(6) . ? N1 C10 1.327(7) . ? N1 C1 1.465(7) . ? N2 C10 1.331(7) . ? N2 C4 1.454(7) . ? N3 C10 1.394(6) . ? N3 C7 1.469(7) . ? N4 C19 1.336(7) . ? N4 C11 1.477(7) . ? N5 C19 1.311(7) . ? N5 C14 1.466(7) . ? N5 Fe 2.093(5) 2 ? N6 C17 1.407(13) . ? N6 C19 1.453(6) . ? N6 C19 1.453(6) 2 ? C1 C2 1.518(8) . ? C1 C3 1.533(8) . ? C4 C6 1.519(8) . ? C4 C5 1.535(9) . ? C7 C8 1.484(9) . ? C7 C9 1.506(8) . ? C11 C12 1.521(8) . ? C11 C13 1.532(8) . ? C14 C16 1.496(8) . ? C14 C15 1.518(8) . ? C17 C18 1.29(3) . ? C17 C18 1.65(3) 2 ? 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 N2 Fe N4 121.32(19) . . ? N2 Fe N5 127.99(18) . 2 ? N4 Fe N5 103.21(18) . 2 ? N2 Fe N1 64.18(18) . . ? N4 Fe N1 118.2(2) . . ? N5 Fe N1 118.24(18) 2 . ? N2 Fe C10 32.14(17) . . ? N4 Fe C10 124.95(19) . . ? N5 Fe C10 130.84(18) 2 . ? N1 Fe C10 32.06(16) . . ? C10 N1 C1 121.9(5) . . ? C10 N1 Fe 89.9(3) . . ? C1 N1 Fe 145.5(4) . . ? C10 N2 C4 123.8(5) . . ? C10 N2 Fe 92.7(3) . . ? C4 N2 Fe 137.5(4) . . ? C10 N3 C7 122.1(5) . . ? C19 N4 C11 123.0(5) . . ? C19 N4 Fe 103.2(4) . . ? C11 N4 Fe 130.8(4) . . ? C19 N5 C14 121.4(5) . . ? C19 N5 Fe 109.4(4) . 2 ? C14 N5 Fe 126.1(4) . 2 ? C17 N6 C19 115.1(13) . . ? C17 N6 C19 131.0(15) . 2 ? C19 N6 C19 113.4(7) . 2 ? N1 C1 C2 108.8(5) . . ? N1 C1 C3 112.1(5) . . ? C2 C1 C3 108.8(5) . . ? N2 C4 C6 110.2(5) . . ? N2 C4 C5 109.8(5) . . ? C6 C4 C5 111.4(6) . . ? N3 C7 C8 111.5(6) . . ? N3 C7 C9 108.9(5) . . ? C8 C7 C9 111.4(7) . . ? N1 C10 N2 113.2(5) . . ? N1 C10 N3 123.6(6) . . ? N2 C10 N3 123.3(6) . . ? N1 C10 Fe 58.0(3) . . ? N2 C10 Fe 55.2(3) . . ? N3 C10 Fe 177.5(5) . . ? N4 C11 C12 110.7(5) . . ? N4 C11 C13 108.3(5) . . ? C12 C11 C13 109.8(5) . . ? N5 C14 C16 109.7(5) . . ? N5 C14 C15 109.7(5) . . ? C16 C14 C15 112.7(5) . . ? C18 C17 N6 131(2) . . ? C18 C17 C18 118.5(12) . 2 ? N6 C17 C18 106.8(17) . 2 ? N5 C19 N4 136.8(6) . . ? N5 C19 N6 112.2(5) . . ? N4 C19 N6 111.0(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.299 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.063 ### END