# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1623 data_sad1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H12 Fe2 Mn3 N20 O13' _chemical_formula_weight 1113.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mn' 'Mn' 0.3368 0.7283 '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' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 13.209(3) _cell_length_b 26.694(5) _cell_length_c 7.443(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.57(3) _cell_angle_gamma 90.00 _cell_volume 2528.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1102 _exptl_absorpt_coefficient_mu 1.359 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18980 _diffrn_reflns_av_R_equivalents 0.2250 _diffrn_reflns_av_sigmaI/netI 0.5006 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.33 _reflns_number_total 6134 _reflns_number_gt 1490 _reflns_threshold_expression >4sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 4sigma(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^)+(0.1061P)^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 SHELXL _refine_ls_extinction_coef 0.0344(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6134 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3042 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.2900 _refine_ls_wR_factor_gt 0.1630 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.261 _refine_ls_shift/su_mean 0.016 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 Mn1 Mn 0.5000 0.0000 1.0000 0.0370(8) Uani 1 2 d S . . Mn2 Mn 1.03068(14) 0.11434(8) 0.2501(2) 0.0376(7) Uani 1 1 d . . . Fe1 Fe 0.76787(14) 0.05570(8) 0.6274(2) 0.0382(6) Uani 1 1 d . . . O1 O 0.4423(14) 0.0771(5) 0.9596(15) 0.157(7) Uani 1 1 d . . . O2 O 1.1295(6) 0.1406(3) 0.0595(11) 0.050(2) Uani 1 1 d . . . N1 N 0.6591(10) 0.1591(6) 0.583(2) 0.084(5) Uani 1 1 d . . . N2 N 0.9284(8) 0.0938(4) 0.4220(12) 0.042(3) Uani 1 1 d . . . N3 N 0.9163(8) 0.0935(4) 0.9963(13) 0.047(3) Uani 1 1 d . . . N4 N 0.8710(9) -0.0491(5) 0.6834(13) 0.045(3) Uani 1 1 d . . . N5 N 0.6129(8) 0.0239(5) 0.2562(14) 0.072(5) Uani 1 1 d . . . N6 N 0.6090(9) 0.0204(5) 0.8357(14) 0.070(4) Uani 1 1 d . . . N7 N 1.1413(8) 0.1630(5) 0.4677(12) 0.044(3) Uani 1 1 d . . . N8 N 0.9640(8) 0.1942(4) 0.2278(12) 0.043(3) Uani 1 1 d . . . N9 N 1.0073(9) 0.2802(4) 0.3095(14) 0.044(3) Uani 1 1 d . . . N10 N 1.1869(8) 0.2474(4) 0.5594(13) 0.042(3) Uani 1 1 d . . . C1 C 0.6992(11) 0.1203(6) 0.5972(18) 0.051(4) Uani 1 1 d . . . C2 C 0.8694(10) 0.0787(5) 0.4979(15) 0.042(3) Uani 1 1 d . . . C3 C 0.8610(10) 0.0793(5) 0.8623(16) 0.039(3) Uani 1 1 d . . . C4 C 0.8327(10) -0.0103(6) 0.6585(16) 0.037(3) Uani 1 1 d . . . C5 C 0.6736(11) 0.0370(6) 0.3939(17) 0.051(4) Uani 1 1 d . . . C6 C 0.6702(10) 0.0340(5) 0.7615(16) 0.044(4) Uani 1 1 d . . . C7 C 0.8717(11) 0.2098(7) 0.1167(17) 0.057(4) Uani 1 1 d . . . H7 H 0.8237 0.1857 0.0488 0.050 Uiso 1 1 calc . . . C8 C 0.8443(11) 0.2597(7) 0.0977(16) 0.053(4) Uani 1 1 d . . . H8 H 0.7784 0.2706 0.0205 0.050 Uiso 1 1 calc . . . C9 C 0.9168(12) 0.2925(6) 0.1954(18) 0.060(5) Uani 1 1 d . . . H9 H 0.9006 0.3272 0.1797 0.050 Uiso 1 1 calc . . . C10 C 1.0259(10) 0.2313(6) 0.3236(14) 0.037(3) Uani 1 1 d . . . C11 C 1.1247(10) 0.2132(6) 0.4578(16) 0.040(3) Uani 1 1 d . . . C12 C 1.2755(11) 0.2299(6) 0.6810(16) 0.052(4) Uani 1 1 d . . . H12 H 1.3241 0.2532 0.7531 0.050 Uiso 1 1 calc . . . C13 C 1.2982(11) 0.1786(6) 0.7042(17) 0.056(4) Uani 1 1 d . . . H13 H 1.3593 0.1668 0.7931 0.050 Uiso 1 1 calc . . . C14 C 1.2287(11) 0.1467(5) 0.5938(18) 0.052(4) Uani 1 1 d . . . H14 H 1.2421 0.1117 0.6055 0.050 Uiso 1 1 calc . . . O101 O 0.3542(10) 0.1394(5) 0.2308(18) 0.113(4) Uiso 1 1 d . . . O102 O 0.4315(10) 0.0799(5) 0.5067(18) 0.110(4) Uiso 1 1 d . . . O103 O 0.241(3) 0.0688(13) 0.899(4) 0.077(11) Uiso 0.33 1 d P A 1 O104 O 0.142(3) 0.0446(12) 0.826(4) 0.063(11) Uiso 0.33 1 d P B 2 O105 O 0.188(2) 0.0526(10) 0.858(3) 0.020(6) Uiso 0.33 1 d P C 3 O106 O 0.534(3) 0.2526(15) 0.519(5) 0.105(12) Uiso 0.33 1 d P D 4 O107 O 0.513(4) 0.2959(18) 0.640(7) 0.148(17) Uiso 0.33 1 d P E 5 O108 O 0.511(4) 0.2158(19) 1.385(7) 0.153(17) Uiso 0.33 1 d P F 6 O109 O 0.627(2) 0.1497(10) 1.047(4) 0.122(9) Uiso 0.50 1 d P G 7 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 Mn1 0.0350(16) 0.061(2) 0.0141(12) -0.0023(12) 0.0056(11) -0.0171(15) Mn2 0.0374(12) 0.0580(16) 0.0171(9) -0.0018(9) 0.0068(8) -0.0139(11) Fe1 0.0372(11) 0.0617(16) 0.0151(8) -0.0029(8) 0.0062(7) -0.0158(10) O1 0.31(2) 0.119(13) 0.060(8) 0.038(8) 0.086(11) 0.109(13) O2 0.057(6) 0.064(7) 0.032(5) 0.005(4) 0.018(4) -0.012(5) N1 0.042(8) 0.067(12) 0.138(13) 0.019(10) 0.014(8) 0.002(8) N2 0.044(6) 0.062(9) 0.023(5) 0.000(5) 0.016(5) -0.015(6) N3 0.047(7) 0.073(9) 0.020(5) -0.003(5) 0.006(5) -0.018(6) N4 0.053(8) 0.057(9) 0.024(5) 0.002(6) 0.009(5) -0.017(7) N5 0.048(8) 0.144(14) 0.028(6) -0.021(7) 0.019(6) -0.054(8) N6 0.051(8) 0.132(13) 0.027(6) -0.007(7) 0.008(6) -0.047(8) N7 0.044(6) 0.058(9) 0.020(5) 0.003(5) -0.006(5) 0.003(6) N8 0.041(6) 0.068(9) 0.018(5) 0.002(5) 0.007(5) 0.000(6) N9 0.059(8) 0.040(8) 0.041(6) 0.007(6) 0.026(6) 0.009(6) N10 0.047(7) 0.050(8) 0.032(6) -0.001(5) 0.012(5) -0.008(6) C1 0.035(8) 0.070(13) 0.044(8) 0.012(8) 0.004(6) -0.014(8) C2 0.048(8) 0.048(10) 0.022(6) -0.004(6) -0.002(6) -0.011(7) C3 0.042(8) 0.055(10) 0.027(7) 0.000(6) 0.020(6) -0.015(7) C4 0.046(8) 0.044(11) 0.024(6) -0.010(6) 0.014(6) -0.020(7) C5 0.050(9) 0.084(12) 0.025(7) 0.002(7) 0.018(6) -0.025(8) C6 0.036(8) 0.065(11) 0.026(7) -0.007(6) 0.000(6) -0.012(7) C7 0.045(9) 0.099(14) 0.024(7) 0.009(7) 0.006(6) 0.005(9) C8 0.057(10) 0.081(13) 0.019(6) 0.008(7) 0.006(6) 0.036(9) C9 0.067(11) 0.089(14) 0.029(7) 0.015(8) 0.023(7) 0.036(10) C10 0.051(8) 0.054(11) 0.011(5) 0.013(6) 0.016(5) 0.001(7) C11 0.044(8) 0.043(10) 0.032(7) 0.002(6) 0.009(6) -0.005(7) C12 0.065(10) 0.064(12) 0.028(7) -0.010(7) 0.012(7) -0.029(9) C13 0.067(10) 0.054(12) 0.038(8) -0.012(7) -0.001(7) -0.012(8) C14 0.055(9) 0.042(10) 0.045(8) -0.010(7) -0.010(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 Mn1 N5 2.177(10) 3_656 ? Mn1 N5 2.177(10) 1_556 ? Mn1 O1 2.187(12) 3_657 ? Mn1 O1 2.187(12) . ? Mn1 N6 2.193(11) 3_657 ? Mn1 N6 2.193(11) . ? Mn2 N3 2.152(10) 1_554 ? Mn2 N4 2.148(13) 3_756 ? Mn2 N2 2.166(10) . ? Mn2 O2 2.282(8) . ? Mn2 N8 2.296(11) . ? Mn2 N7 2.275(10) . ? Fe1 C1 1.933(18) . ? Fe1 C5 1.912(13) . ? Fe1 C2 1.949(14) . ? Fe1 C4 1.946(16) . ? Fe1 C6 1.920(14) . ? Fe1 C3 1.953(12) . ? N1 C1 1.157(17) . ? N2 C2 1.150(14) . ? N3 C3 1.131(13) . ? N3 Mn2 2.152(10) 1_556 ? N4 C4 1.146(14) . ? N4 Mn2 2.148(13) 3_756 ? N5 C5 1.173(14) . ? N5 Mn1 2.177(10) 1_554 ? N6 C6 1.153(14) . ? N7 C11 1.357(16) . ? N7 C14 1.350(14) . ? N8 C7 1.342(15) . ? N8 C10 1.359(15) . ? N9 C9 1.309(16) . ? N9 C10 1.327(15) . ? N10 C11 1.322(15) . ? N10 C12 1.357(16) . ? C7 C8 1.378(19) . ? C7 H7 0.9499 . ? C8 C9 1.36(2) . ? C8 H8 0.9499 . ? C9 H9 0.9501 . ? C10 C11 1.495(16) . ? C12 C13 1.401(19) . ? C12 H12 0.9504 . ? C13 C14 1.356(17) . ? C13 H13 0.9505 . ? C14 H14 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Mn1 N5 180.000(2) 3_656 1_556 ? N5 Mn1 O1 88.6(6) 3_656 3_657 ? N5 Mn1 O1 91.4(6) 1_556 3_657 ? N5 Mn1 O1 91.4(6) 3_656 . ? N5 Mn1 O1 88.6(6) 1_556 . ? O1 Mn1 O1 180.000(2) 3_657 . ? N5 Mn1 N6 91.0(4) 3_656 3_657 ? N5 Mn1 N6 89.0(4) 1_556 3_657 ? O1 Mn1 N6 86.9(5) 3_657 3_657 ? O1 Mn1 N6 93.1(5) . 3_657 ? N5 Mn1 N6 89.0(4) 3_656 . ? N5 Mn1 N6 91.0(4) 1_556 . ? O1 Mn1 N6 93.1(5) 3_657 . ? O1 Mn1 N6 86.9(5) . . ? N6 Mn1 N6 180.000(1) 3_657 . ? N3 Mn2 N4 103.4(4) 1_554 3_756 ? N3 Mn2 N2 92.9(4) 1_554 . ? N4 Mn2 N2 95.4(4) 3_756 . ? N3 Mn2 O2 85.3(3) 1_554 . ? N4 Mn2 O2 88.9(4) 3_756 . ? N2 Mn2 O2 175.6(4) . . ? N3 Mn2 N8 90.7(4) 1_554 . ? N4 Mn2 N8 164.9(4) 3_756 . ? N2 Mn2 N8 89.4(4) . . ? O2 Mn2 N8 86.7(3) . . ? N3 Mn2 N7 159.8(4) 1_554 . ? N4 Mn2 N7 93.8(4) 3_756 . ? N2 Mn2 N7 96.2(4) . . ? O2 Mn2 N7 84.3(3) . . ? N8 Mn2 N7 71.5(4) . . ? C1 Fe1 C5 87.5(6) . . ? C1 Fe1 C2 91.4(6) . . ? C5 Fe1 C2 90.0(5) . . ? C1 Fe1 C4 178.1(6) . . ? C5 Fe1 C4 91.7(6) . . ? C2 Fe1 C4 90.3(5) . . ? C1 Fe1 C6 88.3(6) . . ? C5 Fe1 C6 91.7(5) . . ? C2 Fe1 C6 178.3(5) . . ? C4 Fe1 C6 90.0(6) . . ? C1 Fe1 C3 88.8(6) . . ? C5 Fe1 C3 176.3(6) . . ? C2 Fe1 C3 89.4(5) . . ? C4 Fe1 C3 92.0(5) . . ? C6 Fe1 C3 88.9(5) . . ? C2 N2 Mn2 172.0(10) . . ? C3 N3 Mn2 174.5(12) . 1_556 ? C4 N4 Mn2 169.4(11) . 3_756 ? C5 N5 Mn1 179.7(15) . 1_554 ? C6 N6 Mn1 174.1(11) . . ? C11 N7 C14 116.9(11) . . ? C11 N7 Mn2 117.5(7) . . ? C14 N7 Mn2 125.2(9) . . ? C7 N8 C10 114.5(13) . . ? C7 N8 Mn2 126.9(10) . . ? C10 N8 Mn2 118.3(8) . . ? C9 N9 C10 114.5(13) . . ? C11 N10 C12 115.8(12) . . ? N1 C1 Fe1 178.4(15) . . ? N2 C2 Fe1 177.8(13) . . ? N3 C3 Fe1 178.5(11) . . ? N4 C4 Fe1 177.5(11) . . ? N5 C5 Fe1 176.3(11) . . ? N6 C6 Fe1 177.4(11) . . ? N8 C7 C8 122.3(14) . . ? N8 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C9 C8 C7 116.2(13) . . ? C9 C8 H8 121.9 . . ? C7 C8 H8 121.9 . . ? N9 C9 C8 125.2(15) . . ? N9 C9 H9 117.4 . . ? C8 C9 H9 117.4 . . ? N9 C10 N8 127.1(12) . . ? N9 C10 C11 118.7(12) . . ? N8 C10 C11 114.1(12) . . ? N10 C11 N7 125.8(12) . . ? N10 C11 C10 117.1(13) . . ? N7 C11 C10 117.1(11) . . ? N10 C12 C13 122.5(12) . . ? N10 C12 H12 118.8 . . ? C13 C12 H12 118.7 . . ? C12 C13 C14 116.8(13) . . ? C12 C13 H13 121.6 . . ? C14 C13 H13 121.6 . . ? N7 C14 C13 122.2(14) . . ? N7 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.957 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.214