Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton transactions' ; _publ_contact_author_phone '[351]234 370 729' _publ_contact_author_email 'vfelix@dq.ua.pt' _publ_contact_author_adress ; Prof. V. Felix Departamento de Quimica Universidade de Aveiro 3810-193 Aveiro Portugal -------------------------- data section of block-------------------------- data_Compound 1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 F12 Fe2 N4 P2' _chemical_formula_weight 984.45 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 25.253(28) _cell_length_b 17.104(19) _cell_length_c 10.541(13) _cell_angle_alpha 90.00 _cell_angle_beta 112.560(10) _cell_angle_gamma 90.00 _cell_volume 4205(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all' _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_process_details 'Walker et al., Acta Cryst 1983 A39 158' _exptl_absorpt_correction_T_min 0.773 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8665 _diffrn_reflns_av_R_equivalents 0.2158 _diffrn_reflns_av_sigmaI/netI 0.2725 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.83 _reflns_number_total 3465 _reflns_number_gt 1795 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 ; w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+94.3643P] 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 SHELXL _refine_ls_extinction_coef 0.00024(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3465 _refine_ls_number_parameters 281 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.2017 _refine_ls_R_factor_gt 0.1163 _refine_ls_wR_factor_ref 0.2413 _refine_ls_wR_factor_gt 0.2067 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.031 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.08564(7) 0.37383(10) -0.49951(16) 0.0176(5) Uani 1 d . . . C11 C 0.3694(5) 0.0224(7) 0.4308(12) 0.025(3) Uani 1 d . . . H11 H 0.3571 0.0008 0.3432 0.030 Uiso 1 calc R . . C12 C 0.3384(5) 0.0774(7) 0.4816(12) 0.025(3) Uani 1 d . . . C13 C 0.3729(6) 0.0914(8) 0.6214(13) 0.037(4) Uani 1 d . . . H13 H 0.3629 0.1230 0.6804 0.044 Uiso 1 calc R . . C14 C 0.4239(6) 0.0508(8) 0.6568(13) 0.037(4) Uani 1 d . . . H14 H 0.4543 0.0513 0.7418 0.044 Uiso 1 calc R . . C15 C 0.4212(5) 0.0085(7) 0.5401(14) 0.036(4) Uani 1 d . . . H15 H 0.4500 -0.0241 0.5364 0.043 Uiso 1 calc R . . C16 C 0.2784(5) 0.1081(7) 0.4006(11) 0.022(3) Uani 1 d U . . H16A H 0.2764 0.1635 0.4182 0.026 Uiso 1 calc R . . H16B H 0.2688 0.1010 0.3030 0.026 Uiso 1 calc R . . N17 N 0.2370(4) 0.0638(6) 0.4444(9) 0.020(2) Uani 1 d U . . H17 H 0.240(5) 0.011(7) 0.431(10) 0.024 Uiso 1 d . . . C18 C 0.1772(5) 0.0986(7) 0.3913(11) 0.030(3) Uani 1 d U . . H18A H 0.1803 0.1536 0.4155 0.036 Uiso 1 calc R . . H18B H 0.1554 0.0735 0.4383 0.036 Uiso 1 calc R . . C19 C 0.1426(5) 0.0912(8) 0.2326(11) 0.025(3) Uani 1 d U . . C20 C 0.1198(5) 0.0219(8) 0.1792(13) 0.032(3) Uani 1 d U . . H20 H 0.1263 -0.0224 0.2343 0.039 Uiso 1 calc R . . C21 C 0.0864(6) 0.0181(9) 0.0406(14) 0.045(4) Uani 1 d U . . H21 H 0.0693 -0.0292 0.0034 0.054 Uiso 1 calc R . . C22 C 0.0773(6) 0.0845(9) -0.0476(13) 0.045(4) Uani 1 d . . . H22 H 0.0549 0.0813 -0.1410 0.054 Uiso 1 calc R . . C23 C 0.1036(5) 0.1549(8) 0.0134(10) 0.023(3) Uani 1 d . . . C24 C 0.1373(5) 0.1590(7) 0.1530(11) 0.022(3) Uani 1 d U . . H24 H 0.1559 0.2051 0.1925 0.026 Uiso 1 calc R . . C25 C 0.0962(6) 0.2265(8) -0.0756(12) 0.035(4) Uani 1 d . . . H25A H 0.0638 0.2184 -0.1614 0.042 Uiso 1 calc R . . H25B H 0.0875 0.2709 -0.0297 0.042 Uiso 1 calc R . . N26 N 0.1470(4) 0.2449(6) -0.1057(9) 0.021(2) Uani 1 d . . . H261 H 0.152(5) 0.204(6) -0.171(11) 0.025 Uiso 1 d . . . H262 H 0.174(5) 0.257(6) -0.023(11) 0.025 Uiso 1 d . . . C27 C 0.1396(5) 0.3199(7) -0.1927(10) 0.022(3) Uani 1 d . . . H27A H 0.1279 0.3629 -0.1494 0.026 Uiso 1 calc R . . H27B H 0.1757 0.3336 -0.1991 0.026 Uiso 1 calc R . . C28 C 0.0945(5) 0.3054(7) -0.3347(11) 0.026(3) Uani 1 d . . . C29 C 0.0996(7) 0.2614(8) -0.4408(13) 0.044(4) Uani 1 d . . . H29 H 0.1321 0.2333 -0.4341 0.052 Uiso 1 calc R . . C30 C 0.0487(8) 0.2653(10) -0.5596(14) 0.055(5) Uani 1 d . . . H30 H 0.0412 0.2403 -0.6430 0.065 Uiso 1 calc R . . C31 C 0.0124(7) 0.3136(11) -0.5266(16) 0.066(6) Uani 1 d . . . H31 H -0.0246 0.3266 -0.5859 0.080 Uiso 1 calc R . . C32 C 0.0387(6) 0.3407(9) -0.3915(14) 0.042(4) Uani 1 d . . . H32 H 0.0230 0.3749 -0.3469 0.051 Uiso 1 calc R . . P1 P 0.24387(15) 0.64300(19) -0.2975(3) 0.0256(8) Uani 1 d . . . F11 F 0.3166(3) 0.6415(5) -0.2382(7) 0.045(2) Uani 1 d . . . F12 F 0.2447(3) 0.7315(4) -0.3683(6) 0.0293(18) Uani 1 d . . . F13 F 0.1724(3) 0.6465(4) -0.3597(7) 0.040(2) Uani 1 d . . . F14 F 0.2420(3) 0.5977(4) -0.4402(7) 0.042(2) Uani 1 d . . . F15 F 0.2467(3) 0.6864(4) -0.1524(6) 0.040(2) Uani 1 d . . . F16 F 0.2439(3) 0.5537(4) -0.2252(6) 0.0278(17) Uani 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 0.0080(9) 0.0266(11) 0.0142(8) 0.0043(8) -0.0002(6) -0.0004(9) C11 0.018(7) 0.025(8) 0.024(6) 0.002(5) 0.001(5) -0.004(6) C12 0.031(9) 0.009(7) 0.039(8) 0.007(5) 0.018(6) -0.003(6) C13 0.023(9) 0.054(10) 0.035(8) 0.007(7) 0.013(6) 0.000(7) C14 0.023(8) 0.050(10) 0.032(8) 0.018(7) 0.005(6) 0.004(7) C15 0.008(7) 0.028(8) 0.069(10) 0.011(7) 0.014(7) 0.011(6) C16 0.021(3) 0.022(3) 0.022(3) 0.0001(10) 0.0080(14) 0.0001(10) N17 0.019(2) 0.019(2) 0.020(2) 0.0003(10) 0.0072(13) 0.0000(10) C18 0.029(3) 0.030(3) 0.030(3) 0.0001(10) 0.0116(15) 0.0003(10) C19 0.021(8) 0.035(7) 0.022(6) 0.007(4) 0.013(5) 0.007(6) C20 0.019(8) 0.026(6) 0.045(7) 0.010(6) 0.005(6) 0.012(6) C21 0.033(9) 0.051(10) 0.045(7) -0.005(7) 0.007(7) -0.016(8) C22 0.047(11) 0.049(10) 0.028(8) -0.009(7) 0.003(7) -0.011(8) C23 0.009(6) 0.048(9) 0.010(6) -0.001(5) 0.003(5) 0.006(6) C24 0.010(6) 0.025(6) 0.031(7) 0.002(5) 0.009(5) -0.004(5) C25 0.031(9) 0.055(10) 0.025(7) 0.013(6) 0.018(6) 0.001(7) N26 0.016(6) 0.040(7) 0.005(5) 0.006(4) 0.001(4) -0.001(5) C27 0.020(7) 0.029(8) 0.019(6) -0.006(5) 0.010(5) 0.003(6) C28 0.013(7) 0.037(9) 0.021(6) 0.010(6) -0.003(5) -0.013(6) C29 0.047(11) 0.041(9) 0.037(8) 0.009(7) 0.008(7) 0.007(8) C30 0.071(14) 0.052(11) 0.031(9) -0.007(7) 0.007(9) -0.014(10) C31 0.036(11) 0.078(14) 0.051(10) 0.039(9) -0.021(8) -0.025(10) C32 0.015(8) 0.057(11) 0.049(9) 0.027(7) 0.006(7) 0.006(7) P1 0.030(2) 0.019(2) 0.0284(18) -0.0042(14) 0.0112(15) -0.0086(16) F11 0.018(4) 0.044(5) 0.059(5) 0.014(4) -0.002(4) -0.006(4) F12 0.026(4) 0.031(5) 0.029(4) 0.003(3) 0.008(3) -0.003(3) F13 0.032(5) 0.043(5) 0.045(4) 0.002(4) 0.015(4) -0.016(4) F14 0.063(6) 0.039(5) 0.030(4) -0.010(3) 0.027(4) 0.003(4) F15 0.066(6) 0.036(5) 0.015(4) -0.009(3) 0.010(3) -0.008(4) F16 0.036(5) 0.016(4) 0.028(4) 0.001(3) 0.008(3) -0.007(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 Fe C29 2.010(14) . ? Fe C32 2.015(14) . ? Fe C13 2.032(13) 7 ? Fe C12 2.032(12) 7 ? Fe C28 2.034(11) . ? Fe C31 2.040(16) . ? Fe C14 2.040(12) 7 ? Fe C15 2.050(13) 7 ? Fe C30 2.066(16) . ? Fe C11 2.082(12) 7 ? C11 C15 1.393(16) . ? C11 C12 1.451(17) . ? C11 Fe 2.082(12) 7 ? C11 H11 0.9300 . ? C12 C13 1.415(17) . ? C12 C16 1.520(16) . ? C12 Fe 2.032(12) 7 ? C13 C14 1.382(17) . ? C13 Fe 2.032(13) 7 ? C13 H13 0.9300 . ? C14 C15 1.405(18) . ? C14 Fe 2.040(12) 7 ? C14 H14 0.9300 . ? C15 Fe 2.050(13) 7 ? C15 H15 0.9300 . ? C16 N17 1.500(14) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? N17 C18 1.517(15) . ? N17 H17 0.92(11) . ? C18 C19 1.567(16) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.343(17) . ? C19 C24 1.408(16) . ? C20 C21 1.380(17) . ? C20 H20 0.9300 . ? C21 C22 1.430(18) . ? C21 H21 0.9300 . ? C22 C23 1.407(17) . ? C22 H22 0.9300 . ? C23 C24 1.390(14) . ? C23 C25 1.509(16) . ? C24 H24 0.9300 . ? C25 N26 1.468(15) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? N26 C27 1.545(14) . ? N26 H261 1.01(11) . ? N26 H262 0.90(11) . ? C27 C28 1.514(15) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.394(18) . ? C28 C32 1.436(17) . ? C29 C30 1.411(19) . ? C29 H29 0.9300 . ? C30 C31 1.37(2) . ? C30 H30 0.9300 . ? C31 C32 1.40(2) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? P1 F13 1.668(8) . ? P1 F14 1.676(7) . ? P1 F15 1.677(7) . ? P1 F12 1.691(7) . ? P1 F11 1.699(8) . ? P1 F16 1.706(7) . ? 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 C29 Fe C32 68.2(6) . . ? C29 Fe C13 113.8(6) . 7 ? C32 Fe C13 175.5(5) . 7 ? C29 Fe C12 108.4(6) . 7 ? C32 Fe C12 143.3(5) . 7 ? C13 Fe C12 40.7(5) 7 7 ? C29 Fe C28 40.3(5) . . ? C32 Fe C28 41.6(5) . . ? C13 Fe C28 142.5(5) 7 . ? C12 Fe C28 111.4(5) 7 . ? C29 Fe C31 66.6(7) . . ? C32 Fe C31 40.4(6) . . ? C13 Fe C31 135.9(6) 7 . ? C12 Fe C31 173.3(7) 7 . ? C28 Fe C31 68.0(5) . . ? C29 Fe C14 143.8(6) . 7 ? C32 Fe C14 136.5(5) . 7 ? C13 Fe C14 39.7(5) 7 7 ? C12 Fe C14 68.2(5) 7 7 ? C28 Fe C14 175.8(6) . 7 ? C31 Fe C14 112.8(6) . 7 ? C29 Fe C15 173.8(6) . 7 ? C32 Fe C15 111.9(6) . 7 ? C13 Fe C15 66.6(5) 7 7 ? C12 Fe C15 67.5(5) 7 7 ? C28 Fe C15 135.7(6) . 7 ? C31 Fe C15 117.8(7) . 7 ? C14 Fe C15 40.2(5) 7 7 ? C29 Fe C30 40.5(6) . . ? C32 Fe C30 68.0(7) . . ? C13 Fe C30 110.6(6) 7 . ? C12 Fe C30 134.2(7) 7 . ? C28 Fe C30 68.5(5) . . ? C31 Fe C30 39.1(7) . . ? C14 Fe C30 114.9(6) 7 . ? C15 Fe C30 145.7(6) 7 . ? C29 Fe C11 134.5(5) . 7 ? C32 Fe C11 113.8(6) . 7 ? C13 Fe C11 68.0(5) 7 7 ? C12 Fe C11 41.3(5) 7 7 ? C28 Fe C11 109.0(5) . 7 ? C31 Fe C11 145.5(7) . 7 ? C14 Fe C11 67.8(5) 7 7 ? C15 Fe C11 39.4(5) 7 7 ? C30 Fe C11 174.4(6) . 7 ? C15 C11 C12 105.8(11) . . ? C15 C11 Fe 69.1(7) . 7 ? C12 C11 Fe 67.5(7) . 7 ? C15 C11 H11 127.1 . . ? C12 C11 H11 127.1 . . ? Fe C11 H11 127.8 7 . ? C13 C12 C11 106.9(11) . . ? C13 C12 C16 127.6(11) . . ? C11 C12 C16 125.4(11) . . ? C13 C12 Fe 69.6(7) . 7 ? C11 C12 Fe 71.2(7) . 7 ? C16 C12 Fe 127.8(8) . 7 ? C14 C13 C12 109.5(12) . . ? C14 C13 Fe 70.5(7) . 7 ? C12 C13 Fe 69.6(7) . 7 ? C14 C13 H13 125.2 . . ? C12 C13 H13 125.2 . . ? Fe C13 H13 126.2 7 . ? C13 C14 C15 107.1(11) . . ? C13 C14 Fe 69.8(7) . 7 ? C15 C14 Fe 70.3(7) . 7 ? C13 C14 H14 126.4 . . ? C15 C14 H14 126.4 . . ? Fe C14 H14 125.0 7 . ? C11 C15 C14 110.6(12) . . ? C11 C15 Fe 71.5(7) . 7 ? C14 C15 Fe 69.5(7) . 7 ? C11 C15 H15 124.7 . . ? C14 C15 H15 124.7 . . ? Fe C15 H15 125.8 7 . ? N17 C16 C12 108.4(9) . . ? N17 C16 H16A 110.0 . . ? C12 C16 H16A 110.0 . . ? N17 C16 H16B 110.0 . . ? C12 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? C16 N17 C18 113.6(9) . . ? C16 N17 H17 110(7) . . ? C18 N17 H17 117(7) . . ? N17 C18 C19 115.5(9) . . ? N17 C18 H18A 108.4 . . ? C19 C18 H18A 108.4 . . ? N17 C18 H18B 108.4 . . ? C19 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? C20 C19 C24 123.4(11) . . ? C20 C19 C18 119.5(11) . . ? C24 C19 C18 117.1(11) . . ? C19 C20 C21 118.3(12) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C20 C21 C22 122.1(13) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C23 C22 C21 116.9(11) . . ? C23 C22 H22 121.5 . . ? C21 C22 H22 121.5 . . ? C24 C23 C22 121.1(12) . . ? C24 C23 C25 119.8(11) . . ? C22 C23 C25 119.1(10) . . ? C23 C24 C19 118.0(11) . . ? C23 C24 H24 121.0 . . ? C19 C24 H24 121.0 . . ? N26 C25 C23 113.4(10) . . ? N26 C25 H25A 108.9 . . ? C23 C25 H25A 108.9 . . ? N26 C25 H25B 108.9 . . ? C23 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C25 N26 C27 112.9(9) . . ? C25 N26 H261 110(6) . . ? C27 N26 H261 101(6) . . ? C25 N26 H262 104(7) . . ? C27 N26 H262 105(7) . . ? H261 N26 H262 125(10) . . ? C28 C27 N26 109.0(9) . . ? C28 C27 H27A 109.9 . . ? N26 C27 H27A 109.9 . . ? C28 C27 H27B 109.9 . . ? N26 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? C29 C28 C32 105.7(11) . . ? C29 C28 C27 128.1(12) . . ? C32 C28 C27 126.1(12) . . ? C29 C28 Fe 68.9(7) . . ? C32 C28 Fe 68.5(7) . . ? C27 C28 Fe 123.1(8) . . ? C28 C29 C30 110.7(14) . . ? C28 C29 Fe 70.8(8) . . ? C30 C29 Fe 71.9(9) . . ? C28 C29 H29 124.6 . . ? C30 C29 H29 124.6 . . ? Fe C29 H29 124.3 . . ? C31 C30 C29 105.8(14) . . ? C31 C30 Fe 69.4(10) . . ? C29 C30 Fe 67.6(9) . . ? C31 C30 H30 127.1 . . ? C29 C30 H30 127.1 . . ? Fe C30 H30 127.4 . . ? C30 C31 C32 110.8(14) . . ? C30 C31 Fe 71.5(10) . . ? C32 C31 Fe 68.9(8) . . ? C30 C31 H31 124.6 . . ? C32 C31 H31 124.6 . . ? Fe C31 H31 126.6 . . ? C31 C32 C28 107.0(14) . . ? C31 C32 Fe 70.8(9) . . ? C28 C32 Fe 69.9(7) . . ? C31 C32 H32 126.5 . . ? C28 C32 H32 126.5 . . ? Fe C32 H32 124.4 . . ? F13 P1 F14 90.6(4) . . ? F13 P1 F15 90.2(4) . . ? F14 P1 F15 178.5(4) . . ? F13 P1 F12 89.3(4) . . ? F14 P1 F12 91.1(4) . . ? F15 P1 F12 90.2(4) . . ? F13 P1 F11 178.1(4) . . ? F14 P1 F11 88.7(4) . . ? F15 P1 F11 90.6(4) . . ? F12 P1 F11 89.0(4) . . ? F13 P1 F16 91.3(4) . . ? F14 P1 F16 89.0(4) . . ? F15 P1 F16 89.8(4) . . ? F12 P1 F16 179.3(4) . . ? F11 P1 F16 90.4(4) . . ? _refine_diff_density_max 0.791 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.153 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_Compound 2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H68 Fe2 N4 O12' _chemical_formula_weight 1124.86 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.680(11) _cell_length_b 11.633(13) _cell_length_c 13.107(16) _cell_angle_alpha 100.690(10) _cell_angle_beta 109.560(10) _cell_angle_gamma 96.920(10) _cell_volume 1340(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_process_details 'Walker et al., Acta Cryst 1983 A39 158' _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7789 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.89 _reflns_number_total 4755 _reflns_number_gt 3793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 ; w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+2.0649P] 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 SHELXL _refine_ls_extinction_coef 0.0054(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4755 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1244 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.58833(6) 0.92217(4) 0.80954(4) 0.02138(16) Uani 1 d . . . C11 C 0.4007(4) 0.8360(3) 0.6743(3) 0.0259(8) Uani 1 d . . . H11 H 0.3920 0.8227 0.6001 0.031 Uiso 1 calc R . . C12 C 0.4461(4) 0.7581(3) 0.7465(3) 0.0264(8) Uani 1 d . . . C13 C 0.4446(4) 0.8137(3) 0.8532(3) 0.0331(9) Uani 1 d . . . H13 H 0.4693 0.7826 0.9160 0.040 Uiso 1 calc R . . C14 C 0.3992(4) 0.9235(4) 0.8465(3) 0.0377(10) Uani 1 d . . . H14 H 0.3892 0.9774 0.9044 0.045 Uiso 1 calc R . . C15 C 0.3712(4) 0.9382(3) 0.7371(3) 0.0332(9) Uani 1 d . . . H15 H 0.3393 1.0030 0.7106 0.040 Uiso 1 calc R . . C16 C 0.4884(5) 0.6396(3) 0.7156(3) 0.0343(9) Uani 1 d . . . H16A H 0.5923 0.6535 0.7224 0.041 Uiso 1 calc R . . H16B H 0.4798 0.5933 0.7684 0.041 Uiso 1 calc R . . N17 N 0.3947(3) 0.5682(2) 0.6001(2) 0.0245(6) Uani 1 d . . . H17A H 0.4234 0.4975 0.5893 0.029 Uiso 1 calc R . . H17B H 0.4129 0.6067 0.5510 0.029 Uiso 1 calc R . . C18 C 0.2296(4) 0.5452(4) 0.5754(3) 0.0361(9) Uani 1 d . . . H18A H 0.1951 0.6202 0.5768 0.043 Uiso 1 calc R . . H18B H 0.2098 0.5119 0.6328 0.043 Uiso 1 calc R . . C19 C 0.1438(4) 0.4599(3) 0.4623(3) 0.0273(8) Uani 1 d . . . C20 C 0.0879(5) 0.4996(3) 0.3656(4) 0.0373(10) Uani 1 d . . . H20 H 0.1055 0.5809 0.3692 0.045 Uiso 1 calc R . . C21 C 0.0063(5) 0.4200(4) 0.2641(4) 0.0406(10) Uani 1 d . . . H21 H -0.0316 0.4481 0.2004 0.049 Uiso 1 calc R . . C22 C -0.0190(4) 0.2990(4) 0.2570(3) 0.0334(9) Uani 1 d . . . H22 H -0.0729 0.2460 0.1884 0.040 Uiso 1 calc R . . C23 C 0.0358(4) 0.2559(3) 0.3520(3) 0.0265(8) Uani 1 d . . . C24 C 0.1147(4) 0.3375(3) 0.4534(3) 0.0275(8) Uani 1 d . . . H24 H 0.1491 0.3094 0.5176 0.033 Uiso 1 calc R . . C25 C 0.0068(4) 0.1234(3) 0.3448(3) 0.0312(9) Uani 1 d . . . H25A H -0.0699 0.1050 0.3749 0.037 Uiso 1 calc R . . H25B H -0.0308 0.0803 0.2671 0.037 Uiso 1 calc R . . N26 N 0.1434(3) 0.0812(3) 0.4068(3) 0.0278(7) Uani 1 d . . . H26A H 0.1192 0.0018 0.3973 0.033 Uiso 1 calc R . . H26B H 0.1707 0.1148 0.4800 0.033 Uiso 1 calc R . . C27 C 0.2765(4) 0.1075(3) 0.3737(3) 0.0293(8) Uani 1 d . . . H27A H 0.3055 0.1932 0.3864 0.035 Uiso 1 calc R . . H27B H 0.3595 0.0800 0.4216 0.035 Uiso 1 calc R . . C28 C 0.2498(4) 0.0512(3) 0.2551(3) 0.0282(8) Uani 1 d . . . C29 C 0.2852(5) -0.0605(3) 0.2147(4) 0.0363(9) Uani 1 d . . . H29 H 0.3210 -0.1138 0.2572 0.044 Uiso 1 calc R . . C30 C 0.2563(5) -0.0759(4) 0.0990(4) 0.0424(11) Uani 1 d . . . H30 H 0.2697 -0.1412 0.0528 0.051 Uiso 1 calc R . . C31 C 0.2044(4) 0.0234(4) 0.0660(4) 0.0438(11) Uani 1 d . . . H31 H 0.1781 0.0358 -0.0056 0.053 Uiso 1 calc R . . C32 C 0.1989(4) 0.1023(4) 0.1609(3) 0.0347(9) Uiso 1 d . . . H32 H 0.1674 0.1748 0.1617 0.042 Uiso 1 calc R . . C41 C 0.4751(4) 0.3217(3) 0.7806(3) 0.0295(8) Uani 1 d . . . C42 C 0.5972(4) 0.3364(3) 0.7453(3) 0.0265(8) Uani 1 d . . . C43 C 0.7393(5) 0.3826(4) 0.8258(3) 0.0399(10) Uani 1 d . . . H43 H 0.8211 0.3900 0.8036 0.048 Uiso 1 calc R . . C44 C 0.7621(5) 0.4180(4) 0.9380(4) 0.0530(13) Uani 1 d . . . H44 H 0.8580 0.4499 0.9902 0.064 Uiso 1 calc R . . C45 C 0.6416(6) 0.4054(4) 0.9721(4) 0.0513(12) Uani 1 d . . . H45 H 0.6561 0.4290 1.0473 0.062 Uiso 1 calc R . . C46 C 0.4999(5) 0.3579(4) 0.8943(3) 0.0416(10) Uani 1 d . . . H46 H 0.4193 0.3498 0.9177 0.050 Uiso 1 calc R . . C411 C 0.3190(5) 0.2598(4) 0.6988(4) 0.0378(10) Uani 1 d . . . O412 O 0.3087(3) 0.1757(3) 0.6221(3) 0.0458(8) Uani 1 d . . . O413 O 0.2095(4) 0.2983(4) 0.7163(3) 0.0728(11) Uani 1 d . . . C421 C 0.5836(4) 0.3103(3) 0.6251(3) 0.0278(8) Uani 1 d . . . O422 O 0.6606(3) 0.2417(3) 0.5951(2) 0.0462(8) Uani 1 d . . . O423 O 0.5030(3) 0.3661(2) 0.5613(2) 0.0318(6) Uani 1 d . . . O100 O 0.0796(5) -0.1555(3) 0.4083(3) 0.0506(9) Uani 1 d . . . H101 H 0.141(6) -0.184(5) 0.390(4) 0.058(18) Uiso 1 d . . . H102 H 0.006(7) -0.195(5) 0.369(5) 0.07(2) Uiso 1 d . . . O200 O -0.0855(7) 0.6493(5) 0.1366(5) 0.1067(16) Uani 1 d . . . H200 H -0.1007 0.6694 0.1946 0.128 Uiso 1 calc R . . C201 C -0.1015(9) 0.7435(8) 0.0787(7) 0.120(3) Uani 1 d . . . H20A H -0.1252 0.8093 0.1214 0.143 Uiso 1 calc R . . H20B H -0.1805 0.7147 0.0070 0.143 Uiso 1 calc R . . H20C H -0.0096 0.7693 0.0693 0.143 Uiso 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 Fe 0.0208(3) 0.0177(3) 0.0228(3) 0.00213(19) 0.0063(2) 0.00241(18) C11 0.0255(19) 0.0249(19) 0.0221(19) 0.0025(15) 0.0043(14) 0.0030(14) C12 0.0236(19) 0.0221(19) 0.030(2) 0.0048(15) 0.0081(15) 0.0004(14) C13 0.036(2) 0.036(2) 0.027(2) 0.0068(17) 0.0141(17) -0.0013(17) C14 0.031(2) 0.038(2) 0.039(2) -0.0071(18) 0.0166(18) 0.0022(17) C15 0.026(2) 0.031(2) 0.040(2) 0.0060(18) 0.0083(17) 0.0101(15) C16 0.041(2) 0.023(2) 0.031(2) 0.0046(16) 0.0046(17) 0.0054(16) N17 0.0265(16) 0.0193(15) 0.0285(17) 0.0053(12) 0.0113(13) 0.0048(12) C18 0.029(2) 0.030(2) 0.044(3) -0.0048(18) 0.0162(18) -0.0023(16) C19 0.0234(19) 0.0233(19) 0.034(2) 0.0019(16) 0.0114(15) 0.0041(14) C20 0.044(2) 0.022(2) 0.050(3) 0.0126(19) 0.021(2) 0.0065(17) C21 0.046(3) 0.045(3) 0.035(2) 0.019(2) 0.0127(19) 0.0117(19) C22 0.032(2) 0.036(2) 0.029(2) 0.0056(17) 0.0072(16) 0.0064(16) C23 0.0212(18) 0.0224(19) 0.035(2) 0.0044(16) 0.0103(15) 0.0054(14) C24 0.0250(19) 0.026(2) 0.030(2) 0.0077(16) 0.0070(15) 0.0059(14) C25 0.0214(19) 0.024(2) 0.044(2) 0.0048(17) 0.0102(16) 0.0029(14) N26 0.0281(17) 0.0225(16) 0.0352(18) 0.0068(13) 0.0153(14) 0.0028(12) C27 0.0233(19) 0.029(2) 0.036(2) 0.0072(17) 0.0127(16) 0.0037(15) C28 0.0236(19) 0.029(2) 0.032(2) 0.0090(16) 0.0092(15) 0.0036(15) C29 0.038(2) 0.0191(19) 0.053(3) 0.0057(18) 0.0206(19) 0.0026(16) C30 0.041(2) 0.032(2) 0.043(3) -0.0121(19) 0.018(2) -0.0083(18) C31 0.027(2) 0.059(3) 0.033(2) 0.003(2) 0.0035(17) -0.0005(19) C41 0.043(2) 0.025(2) 0.030(2) 0.0133(16) 0.0201(17) 0.0136(16) C42 0.033(2) 0.0241(19) 0.026(2) 0.0081(15) 0.0135(16) 0.0111(15) C43 0.038(2) 0.047(3) 0.033(2) 0.0078(19) 0.0136(18) 0.0031(18) C44 0.044(3) 0.065(3) 0.034(3) -0.001(2) 0.007(2) -0.009(2) C45 0.067(3) 0.058(3) 0.025(2) 0.001(2) 0.020(2) 0.003(2) C46 0.053(3) 0.049(3) 0.029(2) 0.0089(19) 0.022(2) 0.011(2) C411 0.033(2) 0.058(3) 0.035(2) 0.030(2) 0.0163(18) 0.0160(19) O412 0.0508(19) 0.0387(17) 0.0396(18) 0.0101(14) 0.0067(14) 0.0059(14) O413 0.038(2) 0.127(4) 0.052(2) 0.010(2) 0.0179(16) 0.024(2) C421 0.031(2) 0.028(2) 0.028(2) 0.0089(16) 0.0143(16) 0.0070(15) O422 0.0508(19) 0.062(2) 0.0345(17) 0.0109(14) 0.0194(14) 0.0334(16) O423 0.0432(16) 0.0282(14) 0.0304(15) 0.0148(12) 0.0148(12) 0.0148(12) O100 0.041(2) 0.0306(18) 0.078(3) 0.0109(17) 0.022(2) 0.0060(16) O200 0.110(4) 0.118(4) 0.109(4) 0.028(3) 0.056(3) 0.034(3) C201 0.096(6) 0.140(7) 0.131(7) 0.091(6) 0.030(5) -0.001(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 Fe C32 2.030(5) 2_666 ? Fe C28 2.034(4) 2_666 ? Fe C29 2.041(4) 2_666 ? Fe C15 2.044(4) . ? Fe C14 2.046(4) . ? Fe C11 2.047(4) . ? Fe C31 2.051(4) 2_666 ? Fe C13 2.058(4) . ? Fe C12 2.059(4) . ? Fe C30 2.061(4) 2_666 ? C11 C12 1.430(5) . ? C11 C15 1.431(5) . ? C12 C13 1.433(5) . ? C12 C16 1.507(5) . ? C13 C14 1.408(6) . ? C14 C15 1.415(6) . ? C16 N17 1.496(5) . ? N17 C18 1.499(5) . ? C18 C19 1.518(5) . ? C19 C20 1.390(6) . ? C19 C24 1.393(5) . ? C20 C21 1.384(6) . ? C21 C22 1.379(6) . ? C22 C23 1.391(5) . ? C23 C24 1.389(5) . ? C23 C25 1.514(5) . ? C25 N26 1.494(5) . ? N26 C27 1.507(5) . ? C27 C28 1.491(5) . ? C28 C32 1.434(5) . ? C28 C29 1.436(5) . ? C28 Fe 2.034(4) 2_666 ? C29 C30 1.419(6) . ? C29 Fe 2.041(4) 2_666 ? C30 C31 1.398(6) . ? C30 Fe 2.061(4) 2_666 ? C31 C32 1.423(6) . ? C31 Fe 2.051(4) 2_666 ? C32 Fe 2.030(5) 2_666 ? C41 C46 1.400(6) . ? C41 C42 1.409(5) . ? C41 C411 1.522(6) . ? C42 C43 1.390(5) . ? C42 C421 1.505(5) . ? C43 C44 1.385(6) . ? C44 C45 1.384(7) . ? C45 C46 1.377(6) . ? C411 O412 1.234(5) . ? C411 O413 1.272(5) . ? C421 O422 1.253(4) . ? C421 O423 1.271(4) . ? O200 C201 1.439(8) . ? 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 C32 Fe C28 41.32(16) 2_666 2_666 ? C32 Fe C29 68.61(17) 2_666 2_666 ? C28 Fe C29 41.26(15) 2_666 2_666 ? C32 Fe C15 164.80(16) 2_666 . ? C28 Fe C15 125.26(17) 2_666 . ? C29 Fe C15 105.71(18) 2_666 . ? C32 Fe C14 153.81(17) 2_666 . ? C28 Fe C14 164.38(16) 2_666 . ? C29 Fe C14 127.72(17) 2_666 . ? C15 Fe C14 40.48(17) . . ? C32 Fe C11 127.32(16) 2_666 . ? C28 Fe C11 104.43(18) 2_666 . ? C29 Fe C11 115.06(18) 2_666 . ? C15 Fe C11 40.95(15) . . ? C14 Fe C11 68.47(18) . . ? C32 Fe C31 40.82(17) 2_666 2_666 ? C28 Fe C31 69.21(19) 2_666 2_666 ? C29 Fe C31 68.0(2) 2_666 2_666 ? C15 Fe C31 151.71(17) . 2_666 ? C14 Fe C31 120.41(19) . 2_666 ? C11 Fe C31 167.23(16) . 2_666 ? C32 Fe C13 120.40(17) 2_666 . ? C28 Fe C13 151.88(16) 2_666 . ? C29 Fe C13 166.77(15) 2_666 . ? C15 Fe C13 68.01(18) . . ? C14 Fe C13 40.15(17) . . ? C11 Fe C13 68.45(17) . . ? C31 Fe C13 111.62(19) 2_666 . ? C32 Fe C12 108.76(16) 2_666 . ? C28 Fe C12 116.14(16) 2_666 . ? C29 Fe C12 149.46(17) 2_666 . ? C15 Fe C12 68.51(16) . . ? C14 Fe C12 68.22(16) . . ? C11 Fe C12 40.77(14) . . ? C31 Fe C12 130.98(17) 2_666 . ? C13 Fe C12 40.75(15) . . ? C32 Fe C30 67.90(18) 2_666 2_666 ? C28 Fe C30 68.90(17) 2_666 2_666 ? C29 Fe C30 40.48(18) 2_666 2_666 ? C15 Fe C30 117.59(18) . 2_666 ? C14 Fe C30 109.77(17) . 2_666 ? C11 Fe C30 149.72(17) . 2_666 ? C31 Fe C30 39.75(18) 2_666 2_666 ? C13 Fe C30 130.85(18) . 2_666 ? C12 Fe C30 168.92(17) . 2_666 ? C12 C11 C15 107.7(3) . . ? C12 C11 Fe 70.1(2) . . ? C15 C11 Fe 69.4(2) . . ? C11 C12 C13 107.4(3) . . ? C11 C12 C16 126.0(3) . . ? C13 C12 C16 126.5(3) . . ? C11 C12 Fe 69.2(2) . . ? C13 C12 Fe 69.6(2) . . ? C16 C12 Fe 126.3(3) . . ? C14 C13 C12 108.2(3) . . ? C14 C13 Fe 69.5(2) . . ? C12 C13 Fe 69.7(2) . . ? C13 C14 C15 108.7(3) . . ? C13 C14 Fe 70.4(2) . . ? C15 C14 Fe 69.7(2) . . ? C14 C15 C11 108.0(3) . . ? C14 C15 Fe 69.8(2) . . ? C11 C15 Fe 69.6(2) . . ? N17 C16 C12 113.9(3) . . ? C16 N17 C18 114.8(3) . . ? N17 C18 C19 111.6(3) . . ? C20 C19 C24 117.7(3) . . ? C20 C19 C18 122.2(4) . . ? C24 C19 C18 120.1(3) . . ? C21 C20 C19 121.0(4) . . ? C22 C21 C20 120.3(4) . . ? C21 C22 C23 120.4(4) . . ? C24 C23 C22 118.5(3) . . ? C24 C23 C25 121.0(3) . . ? C22 C23 C25 120.6(3) . . ? C23 C24 C19 122.2(3) . . ? N26 C25 C23 112.9(3) . . ? C25 N26 C27 115.9(3) . . ? C28 C27 N26 114.2(3) . . ? C32 C28 C29 106.2(3) . . ? C32 C28 C27 127.3(3) . . ? C29 C28 C27 126.3(3) . . ? C32 C28 Fe 69.2(2) . 2_666 ? C29 C28 Fe 69.6(2) . 2_666 ? C27 C28 Fe 121.2(2) . 2_666 ? C30 C29 C28 108.5(4) . . ? C30 C29 Fe 70.5(2) . 2_666 ? C28 C29 Fe 69.1(2) . 2_666 ? C31 C30 C29 108.6(4) . . ? C31 C30 Fe 69.7(2) . 2_666 ? C29 C30 Fe 69.0(2) . 2_666 ? C30 C31 C32 108.2(4) . . ? C30 C31 Fe 70.5(2) . 2_666 ? C32 C31 Fe 68.8(2) . 2_666 ? C31 C32 C28 108.6(4) . . ? C31 C32 Fe 70.4(2) . 2_666 ? C28 C32 Fe 69.5(2) . 2_666 ? C46 C41 C42 119.2(4) . . ? C46 C41 C411 119.3(4) . . ? C42 C41 C411 121.4(3) . . ? C43 C42 C41 118.5(4) . . ? C43 C42 C421 117.2(3) . . ? C41 C42 C421 124.2(3) . . ? C44 C43 C42 121.7(4) . . ? C45 C44 C43 119.6(4) . . ? C46 C45 C44 119.9(4) . . ? C45 C46 C41 121.1(4) . . ? O412 C411 O413 125.3(4) . . ? O412 C411 C41 117.7(4) . . ? O413 C411 C41 117.0(4) . . ? O422 C421 O423 123.3(3) . . ? O422 C421 C42 118.5(3) . . ? O423 C421 C42 118.0(3) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.656 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.068 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_compound 3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H80 Fe2 N4 O12 S4' _chemical_formula_weight 1337.26 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' 'S' 'S' 0.1246 0.1234 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 11.443(13) _cell_length_b 18.95(2) _cell_length_c 15.740(17) _cell_angle_alpha 90.00 _cell_angle_beta 104.860(10) _cell_angle_gamma 90.00 _cell_volume 3299(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all' _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.628 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_process_details 'Walker et al., Acta Cryst 1983 A39 158' _exptl_absorpt_correction_T_min 0.824 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14601 _diffrn_reflns_av_R_equivalents 0.0857 _diffrn_reflns_av_sigmaI/netI 0.1333 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.77 _reflns_number_total 5574 _reflns_number_gt 3715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 ; w=1/[\s^2^(Fo^2^)+(0.1517P)^2^+16.0388P] 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 5574 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1316 _refine_ls_R_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.2539 _refine_ls_wR_factor_gt 0.2354 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.883 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.97879(9) 0.97026(5) 0.81378(6) 0.0216(3) Uani 1 d . . . C11 C 1.0414(7) 1.0502(4) 0.7517(5) 0.0348(18) Uani 1 d . . . H11 H 1.0446 1.0498 0.6932 0.042 Uiso 1 calc R . . C12 C 0.9432(6) 1.0739(3) 0.7830(4) 0.0212(14) Uani 1 d . . . C13 C 0.9751(7) 1.0649(4) 0.8752(5) 0.0313(17) Uani 1 d . . . H13 H 0.9270 1.0767 0.9126 0.038 Uiso 1 calc R . . C14 C 1.0931(7) 1.0348(4) 0.9015(5) 0.0375(18) Uani 1 d . . . H14 H 1.1350 1.0224 0.9584 0.045 Uiso 1 calc R . . C15 C 1.1341(7) 1.0272(5) 0.8243(6) 0.045(2) Uani 1 d . . . H15 H 1.2093 1.0100 0.8218 0.054 Uiso 1 calc R . . C16 C 0.8261(6) 1.1060(3) 0.7297(4) 0.0266(15) Uani 1 d . . . H16A H 0.8151 1.0947 0.6680 0.032 Uiso 1 calc R . . H16B H 0.7587 1.0862 0.7486 0.032 Uiso 1 calc R . . N17 N 0.8284(5) 1.1843(3) 0.7414(3) 0.0211(12) Uani 1 d . . . H17A H 0.8861 1.2025 0.7183 0.025 Uiso 1 calc R . . H17B H 0.8488 1.1941 0.7993 0.025 Uiso 1 calc R . . C18 C 0.7102(7) 1.2202(4) 0.6996(4) 0.0302(16) Uani 1 d . . . H18A H 0.7165 1.2697 0.7157 0.036 Uiso 1 calc R . . H18B H 0.6473 1.1995 0.7229 0.036 Uiso 1 calc R . . C19 C 0.6734(6) 1.2143(3) 0.6001(4) 0.0256(15) Uani 1 d . . . C20 C 0.7105(7) 1.2651(4) 0.5490(4) 0.0332(17) Uani 1 d . . . H20 H 0.7665 1.2990 0.5760 0.040 Uiso 1 calc R . . C21 C 0.6639(7) 1.2660(4) 0.4558(5) 0.0396(19) Uani 1 d . . . H21 H 0.6866 1.3011 0.4219 0.047 Uiso 1 calc R . . C22 C 0.5843(7) 1.2134(4) 0.4174(5) 0.0375(18) Uani 1 d . . . H22 H 0.5552 1.2128 0.3566 0.045 Uiso 1 calc R . . C23 C 0.5451(7) 1.1602(4) 0.4679(5) 0.0310(16) Uani 1 d . . . C24 C 0.5923(6) 1.1627(4) 0.5575(5) 0.0309(16) Uani 1 d . . . H24 H 0.5689 1.1280 0.5916 0.037 Uiso 1 calc R . . C25 C 0.4639(7) 1.1007(4) 0.4254(5) 0.0389(19) Uani 1 d . . . H25A H 0.5098 1.0681 0.3991 0.047 Uiso 1 calc R . . H25B H 0.4366 1.0753 0.4703 0.047 Uiso 1 calc R . . N26 N 0.3579(5) 1.1250(3) 0.3575(3) 0.0229(12) Uani 1 d . . . H26A H 0.3824 1.1462 0.3139 0.028 Uiso 1 calc R . . H26B H 0.3167 1.1569 0.3808 0.028 Uiso 1 calc R . . C27 C 0.2756(7) 1.0635(4) 0.3205(5) 0.0308(17) Uani 1 d . . . H27A H 0.2504 1.0401 0.3677 0.037 Uiso 1 calc R . . H27B H 0.3195 1.0296 0.2943 0.037 Uiso 1 calc R . . C28 C 0.1647(7) 1.0888(4) 0.2514(4) 0.0299(16) Uani 1 d . . . C29 C 0.1513(8) 1.0917(4) 0.1583(5) 0.0382(19) Uani 1 d . . . H29 H 0.2081 1.0769 0.1292 0.046 Uiso 1 calc R . . C30 C 0.0351(8) 1.1213(4) 0.1180(5) 0.047(2) Uani 1 d . . . H30 H 0.0032 1.1297 0.0584 0.056 Uiso 1 calc R . . C31 C -0.0217(8) 1.1352(4) 0.1858(6) 0.044(2) Uani 1 d . . . H31 H -0.0987 1.1539 0.1790 0.053 Uiso 1 calc R . . C32 C 0.0604(8) 1.1154(4) 0.2667(5) 0.043(2) Uani 1 d . . . H31 H 0.0455 1.1198 0.3218 0.052 Uiso 1 calc R . . C41 C 1.0688(6) 1.3348(4) 0.6079(4) 0.0226(14) Uani 1 d . . . C42 C 1.1265(6) 1.2897(3) 0.5596(4) 0.0225(14) Uani 1 d . . . H42 H 1.1254 1.2410 0.5674 0.027 Uiso 1 calc R . . C43 C 1.1848(6) 1.3184(4) 0.5006(4) 0.0262(15) Uani 1 d . . . C44 C 1.1827(7) 1.3914(4) 0.4864(5) 0.0359(18) Uani 1 d . . . H44 H 1.2210 1.4104 0.4461 0.043 Uiso 1 calc R . . C45 C 1.1236(7) 1.4355(4) 0.5322(6) 0.042(2) Uani 1 d . . . H45 H 1.1213 1.4840 0.5227 0.051 Uiso 1 calc R . . C46 C 1.0664(7) 1.4051(4) 0.5945(5) 0.0362(18) Uani 1 d . . . H46 H 1.0271 1.4342 0.6260 0.043 Uiso 1 calc R . . C411 C 1.0046(6) 1.3021(4) 0.6734(4) 0.0244(15) Uani 1 d . . . O412 O 0.9478(5) 1.3442(3) 0.7109(3) 0.0376(13) Uani 1 d . . . O413 O 1.0160(5) 1.2366(3) 0.6861(4) 0.0481(15) Uani 1 d . . . O432 O 1.2280(6) 1.2059(3) 0.4466(4) 0.0534(16) Uani 1 d . . . C431 C 1.2490(7) 1.2718(4) 0.4476(4) 0.0303(17) Uani 1 d . . . O433 O 1.3166(5) 1.3014(3) 0.4083(3) 0.0495(15) Uani 1 d . . . S500 S 0.8541(4) 0.0458(2) 0.4432(3) 0.1106(14) Uani 1 d . . . O501 O 0.7730(13) 0.0237(6) 0.4970(7) 0.151(5) Uani 1 d . . . C502 C 0.7645(13) 0.0842(7) 0.3454(8) 0.093(4) Uani 1 d . . . H50A H 0.7034 0.0512 0.3166 0.111 Uiso 1 calc R . . H50B H 0.8148 0.0958 0.3071 0.111 Uiso 1 calc R . . H50C H 0.7267 0.1262 0.3596 0.111 Uiso 1 calc R . . C503 C 0.919(2) 0.1202(8) 0.4887(8) 0.175(11) Uani 1 d . . . H50D H 0.9482 0.1139 0.5511 0.210 Uiso 1 calc R . . H50E H 0.8604 0.1577 0.4771 0.210 Uiso 1 calc R . . H50F H 0.9850 0.1320 0.4643 0.210 Uiso 1 calc R . . S600 S 0.3992(3) 0.0950(2) 0.7506(3) 0.0980(12) Uani 1 d . . . O601 O 0.5219(8) 0.0844(6) 0.7390(7) 0.114(3) Uani 1 d . . . C602 C 0.4042(18) 0.1642(13) 0.8150(13) 0.172(9) Uani 1 d . . . H60A H 0.4650 0.1570 0.8690 0.206 Uiso 1 calc R . . H60B H 0.3270 0.1704 0.8274 0.206 Uiso 1 calc R . . H60C H 0.4236 0.2055 0.7861 0.206 Uiso 1 calc R . . C603 C 0.3069(16) 0.1329(10) 0.6528(12) 0.153(8) Uani 1 d . . . H60D H 0.3463 0.1739 0.6373 0.183 Uiso 1 calc R . . H60E H 0.2304 0.1464 0.6625 0.183 Uiso 1 calc R . . H60F H 0.2942 0.0990 0.6060 0.183 Uiso 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 Fe 0.0282(5) 0.0200(5) 0.0153(5) 0.0003(4) 0.0031(3) -0.0018(5) C11 0.046(5) 0.025(4) 0.040(4) 0.003(3) 0.022(4) -0.005(3) C12 0.033(4) 0.012(3) 0.016(3) -0.013(2) 0.001(3) -0.013(3) C13 0.036(4) 0.033(4) 0.026(4) 0.001(3) 0.010(3) 0.000(3) C14 0.041(4) 0.037(4) 0.030(4) -0.010(3) 0.003(3) -0.005(4) C15 0.035(4) 0.043(5) 0.054(5) 0.003(4) 0.005(4) -0.009(4) C16 0.037(4) 0.017(3) 0.025(4) 0.000(3) 0.006(3) -0.005(3) N17 0.030(3) 0.019(3) 0.015(3) 0.001(2) 0.007(2) 0.003(2) C18 0.042(4) 0.024(4) 0.028(4) -0.005(3) 0.014(3) 0.006(3) C19 0.034(4) 0.017(3) 0.024(4) -0.004(3) 0.005(3) 0.004(3) C20 0.036(4) 0.035(4) 0.026(4) -0.002(3) 0.004(3) 0.002(4) C21 0.042(5) 0.045(5) 0.031(4) -0.002(4) 0.008(3) -0.005(4) C22 0.041(4) 0.033(4) 0.032(4) 0.002(3) -0.002(3) 0.007(4) C23 0.034(4) 0.024(4) 0.030(4) 0.003(3) 0.000(3) 0.000(3) C24 0.031(4) 0.032(4) 0.030(4) 0.005(3) 0.007(3) -0.003(3) C25 0.047(5) 0.036(4) 0.031(4) 0.003(3) 0.006(4) 0.002(4) N26 0.032(3) 0.023(3) 0.012(3) -0.001(2) 0.002(2) -0.005(3) C27 0.035(4) 0.021(4) 0.030(4) -0.001(3) -0.002(3) -0.011(3) C28 0.044(4) 0.021(4) 0.022(4) 0.001(3) 0.005(3) 0.006(3) C29 0.054(5) 0.039(4) 0.023(4) 0.003(3) 0.013(4) -0.008(4) C30 0.063(6) 0.037(5) 0.033(4) 0.007(4) -0.003(4) -0.027(4) C31 0.048(5) 0.022(4) 0.055(5) 0.003(4) 0.000(4) 0.015(4) C32 0.056(5) 0.042(5) 0.027(4) -0.002(3) 0.003(4) 0.002(4) C41 0.022(3) 0.032(4) 0.014(3) 0.006(3) 0.006(3) 0.000(3) C42 0.028(4) 0.017(3) 0.024(3) 0.002(3) 0.011(3) -0.002(3) C43 0.024(4) 0.038(4) 0.017(3) -0.004(3) 0.007(3) -0.006(3) C44 0.043(5) 0.035(4) 0.038(4) 0.011(3) 0.025(4) -0.003(4) C45 0.044(5) 0.025(4) 0.064(6) 0.007(4) 0.026(4) -0.001(4) C46 0.047(5) 0.034(4) 0.034(4) -0.008(3) 0.020(4) 0.001(4) C411 0.020(3) 0.042(4) 0.008(3) 0.001(3) -0.002(3) 0.008(3) O412 0.044(3) 0.046(3) 0.029(3) 0.003(2) 0.020(2) 0.004(3) O413 0.060(4) 0.049(3) 0.048(3) 0.019(3) 0.036(3) 0.009(3) O432 0.066(4) 0.049(4) 0.055(4) -0.018(3) 0.035(3) 0.000(3) C431 0.038(4) 0.043(4) 0.012(3) -0.009(3) 0.012(3) -0.003(4) O433 0.061(4) 0.067(4) 0.031(3) 0.003(3) 0.031(3) 0.002(3) S500 0.149(4) 0.097(3) 0.092(3) 0.004(2) 0.041(3) 0.030(3) O501 0.225(14) 0.147(10) 0.108(8) 0.029(7) 0.093(9) 0.007(10) C502 0.115(11) 0.098(10) 0.067(8) -0.008(7) 0.027(7) 0.004(9) C503 0.40(3) 0.101(11) 0.044(7) 0.013(7) 0.085(12) 0.131(16) S600 0.079(2) 0.123(3) 0.098(3) 0.040(2) 0.034(2) 0.004(2) O601 0.090(7) 0.136(9) 0.125(8) 0.045(7) 0.044(6) 0.011(6) C602 0.136(16) 0.25(3) 0.142(17) 0.011(17) 0.053(13) 0.064(17) C603 0.122(14) 0.182(19) 0.144(15) 0.091(14) 0.016(12) 0.013(13) _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 C11 2.031(7) . ? Fe C29 2.030(8) 3_676 ? Fe C28 2.034(8) 3_676 ? Fe C32 2.036(8) 3_676 ? Fe C12 2.038(7) . ? Fe C14 2.046(7) . ? Fe C13 2.043(8) . ? Fe C15 2.049(8) . ? Fe C31 2.057(8) 3_676 ? Fe C30 2.068(8) 3_676 ? C11 C12 1.411(10) . ? C11 C15 1.415(11) . ? C12 C13 1.413(9) . ? C12 C16 1.514(10) . ? C13 C14 1.426(11) . ? C14 C15 1.418(11) . ? C16 N17 1.496(8) . ? N17 C18 1.505(9) . ? C18 C19 1.518(9) . ? C19 C20 1.388(10) . ? C19 C24 1.396(9) . ? C20 C21 1.427(10) . ? C21 C22 1.381(11) . ? C22 C23 1.426(10) . ? C23 C24 1.376(10) . ? C23 C25 1.505(10) . ? C25 N26 1.470(9) . ? N26 C27 1.518(8) . ? C27 C28 1.522(10) . ? C28 C32 1.371(11) . ? C28 C29 1.434(9) . ? C28 Fe 2.034(8) 3_676 ? C29 C30 1.432(12) . ? C29 Fe 2.030(8) 3_676 ? C30 C31 1.410(12) . ? C30 Fe 2.068(8) 3_676 ? C31 C32 1.425(11) . ? C31 Fe 2.057(8) 3_676 ? C32 Fe 2.036(8) 3_676 ? C41 C46 1.349(10) . ? C41 C42 1.415(9) . ? C41 C411 1.540(9) . ? C42 C43 1.386(9) . ? C43 C44 1.401(10) . ? C43 C431 1.526(9) . ? C44 C45 1.388(11) . ? C45 C46 1.433(10) . ? C411 O413 1.259(9) . ? C411 O412 1.266(8) . ? O432 C431 1.270(9) . ? C431 O433 1.242(8) . ? S500 O501 1.468(11) . ? S500 C503 1.668(19) . ? S500 C502 1.772(13) . ? S600 O601 1.476(9) . ? S600 C602 1.65(2) . ? S600 C603 1.779(15) . ? 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 C11 Fe C29 154.7(3) . 3_676 ? C11 Fe C28 120.4(3) . 3_676 ? C29 Fe C28 41.3(3) 3_676 3_676 ? C11 Fe C32 110.1(3) . 3_676 ? C29 Fe C32 67.5(3) 3_676 3_676 ? C28 Fe C32 39.4(3) 3_676 3_676 ? C11 Fe C12 40.6(3) . . ? C29 Fe C12 119.7(3) 3_676 . ? C28 Fe C12 108.9(3) 3_676 . ? C32 Fe C12 128.4(3) 3_676 . ? C11 Fe C14 68.7(3) . . ? C29 Fe C14 125.2(3) 3_676 . ? C28 Fe C14 164.3(3) 3_676 . ? C32 Fe C14 153.7(3) 3_676 . ? C12 Fe C14 68.8(3) . . ? C11 Fe C13 68.0(3) . . ? C29 Fe C13 107.5(3) 3_676 . ? C28 Fe C13 127.6(3) 3_676 . ? C32 Fe C13 165.0(3) 3_676 . ? C12 Fe C13 40.5(3) . . ? C14 Fe C13 40.8(3) . . ? C11 Fe C15 40.6(3) . . ? C29 Fe C15 162.9(3) 3_676 . ? C28 Fe C15 154.4(3) 3_676 . ? C32 Fe C15 121.2(4) 3_676 . ? C12 Fe C15 68.2(3) . . ? C14 Fe C15 40.5(3) . . ? C13 Fe C15 67.8(3) . . ? C11 Fe C31 127.8(3) . 3_676 ? C29 Fe C31 68.0(4) 3_676 3_676 ? C28 Fe C31 68.2(3) 3_676 3_676 ? C32 Fe C31 40.7(3) 3_676 3_676 ? C12 Fe C31 165.8(3) . 3_676 ? C14 Fe C31 117.9(3) . 3_676 ? C13 Fe C31 152.3(3) . 3_676 ? C15 Fe C31 108.1(4) . 3_676 ? C11 Fe C30 163.7(4) . 3_676 ? C29 Fe C30 40.9(3) 3_676 3_676 ? C28 Fe C30 68.9(3) 3_676 3_676 ? C32 Fe C30 67.7(3) 3_676 3_676 ? C12 Fe C30 153.4(3) . 3_676 ? C14 Fe C30 105.8(3) . 3_676 ? C13 Fe C30 118.5(3) . 3_676 ? C15 Fe C30 125.5(3) . 3_676 ? C31 Fe C30 40.0(4) 3_676 3_676 ? C12 C11 C15 108.3(7) . . ? C12 C11 Fe 70.0(4) . . ? C15 C11 Fe 70.4(4) . . ? C11 C12 C13 107.6(6) . . ? C11 C12 C16 127.2(6) . . ? C13 C12 C16 125.2(6) . . ? C11 C12 Fe 69.4(4) . . ? C13 C12 Fe 69.9(4) . . ? C16 C12 Fe 127.8(4) . . ? C12 C13 C14 108.8(6) . . ? C12 C13 Fe 69.6(4) . . ? C14 C13 Fe 69.7(4) . . ? C15 C14 C13 106.7(7) . . ? C15 C14 Fe 69.9(4) . . ? C13 C14 Fe 69.5(4) . . ? C14 C15 C11 108.5(7) . . ? C14 C15 Fe 69.6(4) . . ? C11 C15 Fe 69.0(4) . . ? N17 C16 C12 110.2(5) . . ? C16 N17 C18 114.1(5) . . ? N17 C18 C19 113.5(5) . . ? C20 C19 C24 118.1(6) . . ? C20 C19 C18 120.1(6) . . ? C24 C19 C18 121.4(6) . . ? C19 C20 C21 121.0(7) . . ? C22 C21 C20 118.1(7) . . ? C21 C22 C23 122.3(7) . . ? C24 C23 C22 116.7(7) . . ? C24 C23 C25 121.1(6) . . ? C22 C23 C25 122.0(6) . . ? C23 C24 C19 123.7(7) . . ? N26 C25 C23 112.9(6) . . ? C25 N26 C27 110.7(5) . . ? N26 C27 C28 110.7(6) . . ? C32 C28 C29 107.1(7) . . ? C32 C28 C27 126.5(7) . . ? C29 C28 C27 126.4(7) . . ? C32 C28 Fe 70.4(5) . 3_676 ? C29 C28 Fe 69.2(4) . 3_676 ? C27 C28 Fe 127.2(5) . 3_676 ? C28 C29 C30 108.2(7) . . ? C28 C29 Fe 69.5(4) . 3_676 ? C30 C29 Fe 71.0(5) . 3_676 ? C31 C30 C29 107.1(7) . . ? C31 C30 Fe 69.6(4) . 3_676 ? C29 C30 Fe 68.1(4) . 3_676 ? C30 C31 C32 107.5(8) . . ? C30 C31 Fe 70.4(5) . 3_676 ? C32 C31 Fe 68.8(4) . 3_676 ? C28 C32 C31 110.2(7) . . ? C28 C32 Fe 70.2(5) . 3_676 ? C31 C32 Fe 70.4(4) . 3_676 ? C46 C41 C42 120.4(6) . . ? C46 C41 C411 120.5(6) . . ? C42 C41 C411 119.0(6) . . ? C43 C42 C41 119.6(6) . . ? C44 C43 C42 120.3(6) . . ? C44 C43 C431 118.4(6) . . ? C42 C43 C431 121.4(6) . . ? C43 C44 C45 120.2(6) . . ? C44 C45 C46 118.8(7) . . ? C41 C46 C45 120.7(7) . . ? O413 C411 O412 126.2(6) . . ? O413 C411 C41 117.1(6) . . ? O412 C411 C41 116.7(6) . . ? O433 C431 O432 125.3(7) . . ? O433 C431 C43 117.4(7) . . ? O432 C431 C43 117.4(6) . . ? O501 S500 C503 105.7(8) . . ? O501 S500 C502 107.9(8) . . ? C503 S500 C502 96.9(7) . . ? O601 S600 C602 107.4(9) . . ? O601 S600 C603 108.7(7) . . ? C602 S600 C603 97.5(11) . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 25.77 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 0.978 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.113 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END