data_Fe(DABP)3LSO4(H2O)10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H80 Fe N22 O17 S' _chemical_formula_weight 1397.31 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 13.8120(14) _cell_length_b 13.8120(14) _cell_length_c 121.731(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 20112(3) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8832 _exptl_absorpt_coefficient_mu 0.339 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8821 _exptl_absorpt_correction_T_max 0.9171 _exptl_absorpt_process_details SADABS _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_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34970 _diffrn_reflns_av_R_equivalents 0.1247 _diffrn_reflns_av_sigmaI/netI 0.1312 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -151 _diffrn_reflns_limit_l_max 149 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.46 _reflns_number_total 4625 _reflns_number_gt 1269 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^ > 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^)+(0.1670P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4625 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2071 _refine_ls_R_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.2793 _refine_ls_wR_factor_gt 0.2384 _refine_ls_goodness_of_fit_ref 0.761 _refine_ls_restrained_S_all 0.761 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 0.0000 0.037755(10) 0.0725(5) Uani 1 3 d S . . S1 S 0.3333 0.6667 0.03624(3) 0.0989(9) Uani 1 3 d S . . N1 N 0.1238(3) 0.1222(4) 0.04610(4) 0.0758(12) Uani 1 1 d . . . N2 N 0.3164(4) 0.1873(4) 0.06921(4) 0.1109(17) Uani 1 1 d . . . H2A H 0.2920 0.1213 0.0718 0.133 Uiso 1 1 calc R . . H2B H 0.3720 0.2438 0.0723 0.133 Uiso 1 1 calc R . . N3 N 0.0153(4) 0.1270(4) 0.02897(4) 0.0798(13) Uani 1 1 d . . . N4 N -0.0880(6) 0.2011(5) 0.00475(5) 0.149(2) Uani 1 1 d . . . H4B H -0.0705 0.2591 0.0008 0.179 Uiso 1 1 calc R . . H4C H -0.1429 0.1371 0.0029 0.179 Uiso 1 1 calc R . . N5 N -0.1093(8) 0.4197(8) 0.02468(6) 0.146(2) Uani 1 1 d . . . N6 N 0.0654(6) 0.4633(5) 0.04864(7) 0.127(2) Uani 1 1 d . . . H6A H 0.1207 0.5238 0.0461 0.153 Uiso 1 1 calc R . . N7 N 0.1845(6) 0.4842(5) 0.06266(6) 0.1279(19) Uani 1 1 d . . . H7B H 0.2354 0.5328 0.0584 0.154 Uiso 1 1 calc R . . N8 N 0.3333 0.6667 0.07767(7) 0.108(3) Uani 1 3 d S . . C1 C 0.1765(5) 0.1119(5) 0.05512(5) 0.0813(16) Uani 1 1 d . . . H1A H 0.1514 0.0411 0.0581 0.098 Uiso 1 1 calc R . . C2 C 0.2658(5) 0.2026(6) 0.06004(5) 0.0896(17) Uani 1 1 d . . . C3 C 0.3006(5) 0.3100(5) 0.05584(7) 0.105(2) Uani 1 1 d . . . H3A H 0.3584 0.3734 0.0591 0.126 Uiso 1 1 calc R . . C4 C 0.2465(5) 0.3178(5) 0.04680(6) 0.0969(18) Uani 1 1 d . . . H4A H 0.2696 0.3881 0.0438 0.116 Uiso 1 1 calc R . . C5 C 0.1592(5) 0.2259(5) 0.04187(5) 0.0785(15) Uani 1 1 d . . . C6 C 0.0983(5) 0.2271(5) 0.03225(5) 0.0767(15) Uani 1 1 d . . . C7 C 0.1219(6) 0.3227(5) 0.02633(6) 0.0994(19) Uani 1 1 d . . . H7A H 0.1791 0.3925 0.0285 0.119 Uiso 1 1 calc R . . C8 C 0.0588(8) 0.3125(7) 0.01707(6) 0.117(2) Uani 1 1 d . . . H8A H 0.0764 0.3757 0.0129 0.140 Uiso 1 1 calc R . . C9 C -0.0294(7) 0.2104(7) 0.01393(6) 0.106(2) Uani 1 1 d . . . C10 C -0.0460(5) 0.1189(5) 0.02000(5) 0.0921(17) Uani 1 1 d . . . H10A H -0.1021 0.0484 0.0178 0.111 Uiso 1 1 calc R . . C11 C -0.0266(7) 0.4636(8) 0.03264(10) 0.138(3) Uani 1 1 d . . . H11A H 0.0337 0.5352 0.0316 0.165 Uiso 1 1 calc R . . C12 C -0.0286(9) 0.4072(8) 0.04202(9) 0.122(3) Uani 1 1 d . . . C13 C -0.1121(9) 0.3036(9) 0.04298(8) 0.150(3) Uani 1 1 d . . . H13A H -0.1109 0.2603 0.0488 0.181 Uiso 1 1 calc R . . C14 C -0.2004(10) 0.2572(9) 0.03582(10) 0.204(6) Uani 1 1 d . . . H14A H -0.2635 0.1890 0.0374 0.245 Uiso 1 1 calc R . . C15 C -0.1946(8) 0.3109(10) 0.02654(11) 0.165(4) Uani 1 1 d . . . H15A H -0.2491 0.2747 0.0212 0.198 Uiso 1 1 calc R . . C16 C 0.0765(8) 0.4308(7) 0.05860(10) 0.123(3) Uani 1 1 d . . . C17 C 0.2213(8) 0.4674(6) 0.07320(7) 0.157(3) Uani 1 1 d . . . H17A H 0.2898 0.4649 0.0722 0.189 Uiso 1 1 calc R . . H17B H 0.1652 0.3959 0.0762 0.189 Uiso 1 1 calc R . . C18 C 0.2414(7) 0.5559(7) 0.08109(6) 0.147(3) Uani 1 1 d . . . H18A H 0.2592 0.5370 0.0882 0.176 Uiso 1 1 calc R . . H18B H 0.1735 0.5597 0.0819 0.176 Uiso 1 1 calc R . . O1 O 0.0049(5) 0.3528(5) 0.06397(5) 0.182(3) Uani 1 1 d . . . O2 O 0.3333 0.6667 0.04786(9) 0.201(5) Uani 1 3 d S . . O3 O 0.3671(6) 0.5908(5) 0.03318(6) 0.206(3) Uani 1 1 d . . . O4 O 0.3639(9) 0.5408(11) 0.00854(8) 0.359(7) Uani 1 1 d . . . O5 O 0.4562(13) 0.3929(11) 0.00586(8) 0.426(9) Uani 1 1 d . . . O6 O -0.1460(9) 0.4461(10) 0.07314(12) 0.409(8) Uani 1 1 d . . . O7 O -0.3333 0.3333 0.0597(2) 0.514(19) Uani 1 3 d S . . 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 0.0684(6) 0.0684(6) 0.0808(9) 0.000 0.000 0.0342(3) S1 0.0991(13) 0.0991(13) 0.098(2) 0.000 0.000 0.0495(7) N1 0.062(3) 0.071(3) 0.087(3) -0.004(3) 0.010(3) 0.027(2) N2 0.086(3) 0.117(4) 0.106(4) -0.014(3) -0.018(3) 0.033(3) N3 0.075(3) 0.080(3) 0.085(3) 0.013(3) 0.008(3) 0.039(3) N4 0.216(7) 0.125(5) 0.112(4) 0.006(4) -0.045(5) 0.089(5) N5 0.136(6) 0.151(7) 0.166(6) 0.018(5) 0.025(6) 0.083(6) N6 0.106(5) 0.105(5) 0.154(6) -0.003(5) -0.020(5) 0.039(4) N7 0.149(6) 0.095(4) 0.114(5) 0.003(4) 0.015(4) 0.042(4) N8 0.112(4) 0.112(4) 0.101(6) 0.000 0.000 0.056(2) C1 0.069(4) 0.093(4) 0.075(4) -0.004(3) -0.004(3) 0.035(4) C2 0.071(4) 0.106(5) 0.086(4) -0.010(4) 0.001(4) 0.040(4) C3 0.082(4) 0.067(4) 0.147(6) -0.010(4) 0.002(5) 0.022(3) C4 0.087(5) 0.068(4) 0.131(6) -0.006(4) 0.007(4) 0.034(4) C5 0.069(4) 0.068(4) 0.100(4) -0.003(4) 0.013(4) 0.035(3) C6 0.077(4) 0.071(4) 0.087(4) 0.009(3) 0.018(3) 0.040(4) C7 0.116(5) 0.069(4) 0.108(5) 0.008(4) 0.022(4) 0.043(4) C8 0.181(8) 0.130(7) 0.080(5) 0.030(5) 0.035(5) 0.107(7) C9 0.120(6) 0.095(5) 0.101(6) -0.008(5) -0.004(5) 0.052(5) C10 0.100(4) 0.087(4) 0.095(4) 0.013(4) 0.000(4) 0.051(4) C11 0.104(6) 0.128(7) 0.174(8) -0.034(8) -0.014(6) 0.053(5) C12 0.137(8) 0.094(6) 0.154(8) 0.031(6) 0.036(7) 0.072(7) C13 0.117(7) 0.156(9) 0.177(9) 0.038(7) 0.006(7) 0.066(7) C14 0.154(9) 0.174(9) 0.230(11) 0.097(9) -0.048(9) 0.040(8) C15 0.109(7) 0.143(9) 0.237(12) -0.021(8) 0.000(7) 0.057(7) C16 0.101(7) 0.088(6) 0.158(8) -0.006(6) 0.031(7) 0.031(5) C17 0.215(9) 0.096(6) 0.114(6) 0.015(5) 0.010(7) 0.043(6) C18 0.145(7) 0.142(7) 0.120(6) 0.024(6) 0.007(5) 0.047(6) O1 0.149(5) 0.129(4) 0.208(6) 0.034(4) 0.054(4) 0.025(4) O2 0.238(8) 0.238(8) 0.126(8) 0.000 0.000 0.119(4) O3 0.224(7) 0.164(5) 0.285(7) -0.035(5) -0.001(6) 0.137(5) O4 0.270(10) 0.469(18) 0.270(8) -0.123(11) -0.019(8) 0.134(11) O5 0.58(2) 0.444(15) 0.274(11) -0.202(11) -0.246(14) 0.269(17) O6 0.318(13) 0.303(13) 0.60(2) 0.162(13) -0.031(14) 0.146(11) O7 0.62(3) 0.62(3) 0.30(2) 0.000 0.000 0.311(16) _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 N3 1.973(4) . ? Fe1 N3 1.973(4) 2 ? Fe1 N3 1.973(4) 3 ? Fe1 N1 1.980(4) 3 ? Fe1 N1 1.980(4) 2 ? Fe1 N1 1.980(4) . ? S1 O3 1.394(6) 3_565 ? S1 O3 1.394(6) 2_665 ? S1 O3 1.394(6) . ? S1 O2 1.416(10) . ? N1 C5 1.361(6) . ? N1 C1 1.363(6) . ? N2 C2 1.388(7) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 C10 1.352(6) . ? N3 C6 1.341(7) . ? N4 C9 1.347(8) . ? N4 H4B 0.8600 . ? N4 H4C 0.8600 . ? N5 C15 1.389(10) . ? N5 C11 1.385(10) . ? N6 C16 1.328(10) . ? N6 C12 1.389(10) . ? N6 H6A 0.8600 . ? N7 C16 1.383(10) . ? N7 C17 1.441(9) . ? N7 H7B 0.8600 . ? N8 C18 1.478(8) 3_565 ? N8 C18 1.478(8) . ? N8 C18 1.478(8) 2_665 ? C1 C2 1.380(7) . ? C1 H1A 0.9300 . ? C2 C3 1.407(8) . ? C3 C4 1.364(8) . ? C3 H3A 0.9300 . ? C4 C5 1.377(7) . ? C4 H4A 0.9300 . ? C5 C6 1.447(7) . ? C6 C7 1.392(7) . ? C7 C8 1.388(9) . ? C7 H7A 0.9300 . ? C8 C9 1.379(9) . ? C8 H8A 0.9300 . ? C9 C10 1.380(8) . ? C10 H10A 0.9300 . ? C11 C12 1.375(10) . ? C11 H11A 0.9300 . ? C12 C13 1.319(11) . ? C13 C14 1.369(11) . ? C13 H13A 0.9300 . ? C14 C15 1.332(12) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 O1 1.225(8) . ? C17 C18 1.468(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? 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 N3 Fe1 N3 93.43(19) . 2 ? N3 Fe1 N3 93.43(19) . 3 ? N3 Fe1 N3 93.43(19) 2 3 ? N3 Fe1 N1 174.80(19) . 3 ? N3 Fe1 N1 88.90(16) 2 3 ? N3 Fe1 N1 81.8(2) 3 3 ? N3 Fe1 N1 88.90(16) . 2 ? N3 Fe1 N1 81.8(2) 2 2 ? N3 Fe1 N1 174.80(19) 3 2 ? N1 Fe1 N1 96.04(17) 3 2 ? N3 Fe1 N1 81.8(2) . . ? N3 Fe1 N1 174.80(19) 2 . ? N3 Fe1 N1 88.90(16) 3 . ? N1 Fe1 N1 96.04(17) 3 . ? N1 Fe1 N1 96.04(17) 2 . ? O3 S1 O3 113.2(3) 3_565 2_665 ? O3 S1 O3 113.2(3) 3_565 . ? O3 S1 O3 113.2(3) 2_665 . ? O3 S1 O2 105.5(3) 3_565 . ? O3 S1 O2 105.5(3) 2_665 . ? O3 S1 O2 105.5(3) . . ? C5 N1 C1 119.0(5) . . ? C5 N1 Fe1 113.9(4) . . ? C1 N1 Fe1 127.1(4) . . ? C2 N2 H2A 120.0 . . ? C2 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C10 N3 C6 120.2(5) . . ? C10 N3 Fe1 125.4(4) . . ? C6 N3 Fe1 114.3(4) . . ? C9 N4 H4B 120.0 . . ? C9 N4 H4C 120.0 . . ? H4B N4 H4C 120.0 . . ? C15 N5 C11 115.3(8) . . ? C16 N6 C12 125.1(8) . . ? C16 N6 H6A 117.5 . . ? C12 N6 H6A 117.5 . . ? C16 N7 C17 127.3(8) . . ? C16 N7 H7B 116.3 . . ? C17 N7 H7B 116.3 . . ? C18 N8 C18 112.4(4) 3_565 . ? C18 N8 C18 112.4(4) 3_565 2_665 ? C18 N8 C18 112.4(4) . 2_665 ? N1 C1 C2 122.4(6) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C1 C2 N2 120.0(6) . . ? C1 C2 C3 118.6(6) . . ? N2 C2 C3 121.4(6) . . ? C4 C3 C2 117.7(6) . . ? C4 C3 H3A 121.1 . . ? C2 C3 H3A 121.1 . . ? C3 C4 C5 122.7(6) . . ? C3 C4 H4A 118.7 . . ? C5 C4 H4A 118.7 . . ? N1 C5 C4 119.6(6) . . ? N1 C5 C6 114.4(5) . . ? C4 C5 C6 126.0(6) . . ? N3 C6 C7 119.8(6) . . ? N3 C6 C5 115.5(5) . . ? C7 C6 C5 124.6(6) . . ? C6 C7 C8 119.1(6) . . ? C6 C7 H7A 120.4 . . ? C8 C7 H7A 120.4 . . ? C9 C8 C7 121.2(7) . . ? C9 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? N4 C9 C8 120.6(7) . . ? N4 C9 C10 122.6(7) . . ? C8 C9 C10 116.4(7) . . ? N3 C10 C9 123.1(6) . . ? N3 C10 H10A 118.4 . . ? C9 C10 H10A 118.4 . . ? C12 C11 N5 123.6(10) . . ? C12 C11 H11A 118.2 . . ? N5 C11 H11A 118.2 . . ? C13 C12 C11 116.6(11) . . ? C13 C12 N6 128.4(10) . . ? C11 C12 N6 114.6(9) . . ? C12 C13 C14 122.9(10) . . ? C12 C13 H13A 118.6 . . ? C14 C13 H13A 118.6 . . ? C15 C14 C13 119.2(10) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C14 C15 N5 121.5(10) . . ? C14 C15 H15A 119.2 . . ? N5 C15 H15A 119.2 . . ? O1 C16 N6 127.2(10) . . ? O1 C16 N7 117.4(11) . . ? N6 C16 N7 115.0(8) . . ? N7 C17 C18 112.5(7) . . ? N7 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? N7 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? C17 C18 N8 112.6(7) . . ? C17 C18 H18A 109.1 . . ? N8 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? N8 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Fe1 N1 C5 -1.9(3) . . . . ? N3 Fe1 N1 C5 -25(2) 2 . . . ? N3 Fe1 N1 C5 91.7(4) 3 . . . ? N1 Fe1 N1 C5 173.3(3) 3 . . . ? N1 Fe1 N1 C5 -89.9(4) 2 . . . ? N3 Fe1 N1 C1 180(54) . . . . ? N3 Fe1 N1 C1 157(2) 2 . . . ? N3 Fe1 N1 C1 -86.4(4) 3 . . . ? N1 Fe1 N1 C1 -4.8(4) 3 . . . ? N1 Fe1 N1 C1 92.0(3) 2 . . . ? N3 Fe1 N3 C10 -2.9(5) 2 . . . ? N3 Fe1 N3 C10 90.7(3) 3 . . . ? N1 Fe1 N3 C10 114(2) 3 . . . ? N1 Fe1 N3 C10 -84.6(4) 2 . . . ? N1 Fe1 N3 C10 179(57) . . . . ? N3 Fe1 N3 C6 -180(57) 2 . . . ? N3 Fe1 N3 C6 -86.0(4) 3 . . . ? N1 Fe1 N3 C6 -63(2) 3 . . . ? N1 Fe1 N3 C6 98.7(4) 2 . . . ? N1 Fe1 N3 C6 2.4(3) . . . . ? C5 N1 C1 C2 -1.1(7) . . . . ? Fe1 N1 C1 C2 176.9(4) . . . . ? N1 C1 C2 N2 180.0(4) . . . . ? N1 C1 C2 C3 2.6(8) . . . . ? C1 C2 C3 C4 -2.7(9) . . . . ? N2 C2 C3 C4 -179.9(5) . . . . ? C2 C3 C4 C5 1.3(9) . . . . ? C1 N1 C5 C4 -0.4(7) . . . . ? Fe1 N1 C5 C4 -178.6(4) . . . . ? C1 N1 C5 C6 179.4(4) . . . . ? Fe1 N1 C5 C6 1.1(5) . . . . ? C3 C4 C5 N1 0.2(8) . . . . ? C3 C4 C5 C6 -179.5(6) . . . . ? C10 N3 C6 C7 -0.6(7) . . . . ? Fe1 N3 C6 C7 176.3(4) . . . . ? C10 N3 C6 C5 -179.4(5) . . . . ? Fe1 N3 C6 C5 -2.5(6) . . . . ? N1 C5 C6 N3 0.9(6) . . . . ? C4 C5 C6 N3 -179(74) . . . . ? N1 C5 C6 C7 -177.8(5) . . . . ? C4 C5 C6 C7 2.0(8) . . . . ? N3 C6 C7 C8 -0.1(8) . . . . ? C5 C6 C7 C8 178.5(5) . . . . ? C6 C7 C8 C9 2.8(9) . . . . ? C7 C8 C9 N4 -178.1(6) . . . . ? C7 C8 C9 C10 -4.4(10) . . . . ? C6 N3 C10 C9 -1.3(8) . . . . ? Fe1 N3 C10 C9 -177.8(4) . . . . ? N4 C9 C10 N3 177.3(6) . . . . ? C8 C9 C10 N3 3.7(10) . . . . ? C15 N5 C11 C12 -2.5(11) . . . . ? N5 C11 C12 C13 3.6(12) . . . . ? N5 C11 C12 N6 176.5(7) . . . . ? C16 N6 C12 C13 -15.8(13) . . . . ? C16 N6 C12 C11 172.3(7) . . . . ? C11 C12 C13 C14 -7.8(14) . . . . ? N6 C12 C13 C14 -179.5(9) . . . . ? C12 C13 C14 C15 11.0(17) . . . . ? C13 C14 C15 N5 -9.6(17) . . . . ? C11 N5 C15 C14 5.5(13) . . . . ? C12 N6 C16 O1 -6.2(13) . . . . ? C12 N6 C16 N7 166.0(6) . . . . ? C17 N7 C16 O1 -7.8(11) . . . . ? C17 N7 C16 N6 179.1(7) . . . . ? C16 N7 C17 C18 -101.7(9) . . . . ? N7 C17 C18 N8 -64.0(10) . . . . ? C18 N8 C18 C17 146.6(9) 3_565 . . . ? C18 N8 C18 C17 -85.4(11) 2_665 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7B O2 0.86 2.10 2.940(9) 166.3 . N6 H6A O3 0.86 2.15 2.947(10) 154.2 3_565 N2 H2A O1 0.86 2.43 2.967(8) 121.2 3 N2 H2B O6 0.86 2.40 3.206(13) 156.1 2_665 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.603 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.076 ######### data_Fe(DABP)3LSO4(H2O)6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H72 Fe N22 O13 S' _chemical_formula_weight 1325.25 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' 'S' 'S' 0.1246 0.1234 '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 trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 14.1477(4) _cell_length_b 14.1477(4) _cell_length_c 18.8263(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3263.38(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8962 _exptl_absorpt_correction_T_max 0.9352 _exptl_absorpt_process_details SADABS _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_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16287 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.23 _reflns_number_total 3531 _reflns_number_gt 2078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^ > 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^)+(0.1529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3531 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.2350 _refine_ls_wR_factor_gt 0.1935 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.0000 0.0000 0.23784(6) 0.0560(4) Uani 1 3 d S . . N1 N 0.0141(3) 0.1231(3) 0.2949(2) 0.0539(10) Uani 1 1 d . . . N3 N 0.1152(3) 0.1225(3) 0.1820(2) 0.0621(11) Uani 1 1 d . . . C1 C -0.0311(4) 0.1161(4) 0.3596(3) 0.0551(12) Uani 1 1 d . . . H1A H -0.0860 0.0480 0.3748 0.066 Uiso 1 1 calc R . . N2 N -0.0378(3) 0.1872(3) 0.4730(2) 0.0711(12) Uani 1 1 d . . . H2A H -0.0800 0.1219 0.4880 0.085 Uiso 1 1 calc R . . H2B H -0.0190 0.2418 0.5009 0.085 Uiso 1 1 calc R . . C2 C -0.0006(4) 0.2043(4) 0.4044(3) 0.0568(12) Uani 1 1 d . . . C5 C 0.0895(4) 0.2236(4) 0.2715(3) 0.0562(12) Uani 1 1 d . . . C4 C 0.1172(4) 0.3169(4) 0.3117(3) 0.0635(13) Uani 1 1 d . . . H4A H 0.1656 0.3855 0.2934 0.076 Uiso 1 1 calc R . . C3 C 0.0739(4) 0.3077(4) 0.3775(3) 0.0642(13) Uani 1 1 d . . . H3A H 0.0936 0.3698 0.4046 0.077 Uiso 1 1 calc R . . C6 C 0.1424(4) 0.2225(4) 0.2054(2) 0.0584(12) Uani 1 1 d . . . C7 C 0.2176(4) 0.3148(4) 0.1692(3) 0.0718(14) Uani 1 1 d . . . H7A H 0.2344 0.3833 0.1859 0.086 Uiso 1 1 calc R . . C10 C 0.1648(5) 0.1134(5) 0.1238(3) 0.0803(16) Uani 1 1 d . . . H10A H 0.1469 0.0442 0.1078 0.096 Uiso 1 1 calc R . . C8 C 0.2668(5) 0.3070(5) 0.1101(3) 0.0831(17) Uani 1 1 d . . . H8A H 0.3163 0.3696 0.0858 0.100 Uiso 1 1 calc R . . C9 C 0.2433(5) 0.2055(6) 0.0859(3) 0.093(2) Uani 1 1 d . . . N4 N 0.2895(6) 0.1875(6) 0.0258(3) 0.155(3) Uani 1 1 d . . . H4B H 0.3363 0.2418 0.0010 0.186 Uiso 1 1 calc R . . H4C H 0.2713 0.1219 0.0136 0.186 Uiso 1 1 calc R . . S S 0.3333 0.6667 0.28583(12) 0.0649(6) Uani 1 3 d S . . O2 O 0.3333 0.6667 0.3638(4) 0.108(2) Uani 1 3 d S . . O3 O 0.4179(4) 0.6469(4) 0.2618(3) 0.1104(15) Uani 1 1 d . . . N8 N 0.3333 0.6667 0.5403(3) 0.0517(16) Uani 1 3 d S . . O1 O -0.0136(3) 0.6308(3) 0.4405(2) 0.0753(10) Uani 1 1 d . . . N7 N 0.1469(3) 0.6351(4) 0.4503(2) 0.0704(12) Uani 1 1 d . . . H7B H 0.1969 0.6275 0.4297 0.085 Uiso 1 1 calc R . . C16 C 0.0606(4) 0.6205(4) 0.4128(3) 0.0618(13) Uani 1 1 d . . . C18 C 0.2215(4) 0.6210(4) 0.5648(3) 0.0624(13) Uani 1 1 d . . . H18A H 0.2223 0.6368 0.6150 0.075 Uiso 1 1 calc R . . H18B H 0.1842 0.5423 0.5594 0.075 Uiso 1 1 calc R . . N6 N 0.0575(3) 0.5905(3) 0.3443(2) 0.0683(11) Uani 1 1 d . . . H6A H 0.1121 0.5855 0.3291 0.082 Uiso 1 1 calc R . . C17 C 0.1583(4) 0.6639(5) 0.5260(3) 0.0705(14) Uani 1 1 d . . . H17A H 0.0864 0.6341 0.5471 0.085 Uiso 1 1 calc R . . H17B H 0.1953 0.7427 0.5308 0.085 Uiso 1 1 calc R . . N5 N -0.1095(6) 0.4739(5) 0.1871(4) 0.128(2) Uani 1 1 d . . . C12 C -0.0258(4) 0.5671(4) 0.2962(3) 0.0708(14) Uani 1 1 d . . . C13 C -0.1000(5) 0.6023(5) 0.3008(3) 0.0905(19) Uani 1 1 d . . . H13A H -0.0987 0.6459 0.3381 0.109 Uiso 1 1 calc R . . C14 C -0.1785(6) 0.5688(8) 0.2459(5) 0.126(3) Uani 1 1 d . . . H14A H -0.2304 0.5908 0.2474 0.151 Uiso 1 1 calc R . . C11 C -0.0336(5) 0.5014(5) 0.2388(4) 0.0943(19) Uani 1 1 d . . . H11A H 0.0151 0.4755 0.2358 0.113 Uiso 1 1 calc R . . C15 C -0.1805(8) 0.5076(8) 0.1927(6) 0.137(4) Uani 1 1 d . . . H15A H -0.2340 0.4874 0.1580 0.165 Uiso 1 1 calc R . . O4 O 0.4441(13) 0.6312(12) 0.1160(5) 0.335(7) Uani 1 1 d . . . O5 O 0.4187(13) 0.4357(14) -0.0547(6) 0.562(18) 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 0.0576(5) 0.0576(5) 0.0530(7) 0.000 0.000 0.0288(3) N1 0.051(2) 0.055(2) 0.058(2) 0.0039(18) -0.0008(18) 0.0283(19) N3 0.061(2) 0.070(3) 0.053(2) 0.003(2) 0.001(2) 0.031(2) C1 0.053(3) 0.051(3) 0.065(3) 0.003(2) 0.005(2) 0.029(2) N2 0.081(3) 0.066(3) 0.066(3) -0.004(2) 0.014(2) 0.036(2) C2 0.049(3) 0.058(3) 0.071(3) -0.002(3) -0.002(2) 0.032(2) C5 0.048(3) 0.055(3) 0.065(3) 0.009(2) -0.002(2) 0.025(2) C4 0.057(3) 0.052(3) 0.079(4) 0.011(3) 0.008(3) 0.026(2) C3 0.056(3) 0.049(3) 0.086(4) -0.007(3) -0.003(3) 0.026(2) C6 0.054(3) 0.064(3) 0.057(3) 0.007(2) 0.001(2) 0.029(2) C7 0.062(3) 0.063(3) 0.075(4) 0.004(3) -0.005(3) 0.020(3) C10 0.086(4) 0.085(4) 0.060(3) -0.002(3) 0.007(3) 0.035(3) C8 0.071(4) 0.083(4) 0.064(4) 0.010(3) 0.008(3) 0.015(3) C9 0.083(4) 0.115(5) 0.063(4) 0.009(4) 0.024(3) 0.035(4) N4 0.165(6) 0.134(5) 0.096(4) -0.005(4) 0.074(5) 0.022(4) S 0.0686(9) 0.0686(9) 0.0574(14) 0.000 0.000 0.0343(5) O2 0.124(4) 0.124(4) 0.075(5) 0.000 0.000 0.0622(19) O3 0.092(3) 0.126(4) 0.136(4) 0.014(3) 0.025(3) 0.072(3) N8 0.049(2) 0.049(2) 0.058(4) 0.000 0.000 0.0244(11) O1 0.0464(19) 0.077(2) 0.098(3) -0.019(2) -0.0055(19) 0.0277(18) N7 0.056(2) 0.092(3) 0.073(3) -0.007(2) -0.004(2) 0.044(2) C16 0.050(3) 0.049(3) 0.080(4) -0.004(2) -0.005(3) 0.019(2) C18 0.057(3) 0.064(3) 0.064(3) 0.003(2) 0.010(2) 0.028(2) N6 0.056(2) 0.074(3) 0.073(3) -0.007(2) -0.004(2) 0.030(2) C17 0.056(3) 0.091(4) 0.070(4) -0.006(3) 0.000(3) 0.041(3) N5 0.120(5) 0.102(5) 0.114(5) -0.019(4) -0.045(5) 0.020(4) C12 0.061(3) 0.055(3) 0.077(4) 0.010(3) -0.006(3) 0.014(3) C13 0.067(4) 0.101(5) 0.095(5) 0.016(4) -0.005(3) 0.036(4) C14 0.068(4) 0.155(8) 0.144(7) 0.049(6) -0.004(5) 0.048(5) C11 0.090(4) 0.071(4) 0.099(5) -0.013(4) -0.027(4) 0.023(3) C15 0.111(7) 0.132(8) 0.118(7) 0.001(6) -0.040(6) 0.023(6) O4 0.49(2) 0.431(18) 0.177(8) -0.045(11) 0.023(11) 0.297(17) O5 0.437(19) 0.51(2) 0.203(10) -0.092(12) 0.214(12) -0.166(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1 1.969(4) . ? Fe N1 1.969(4) 2 ? Fe N1 1.969(4) 3 ? Fe N3 1.985(4) 2 ? Fe N3 1.985(4) 3 ? Fe N3 1.985(4) . ? N1 C5 1.356(6) . ? N1 C1 1.357(6) . ? N3 C6 1.340(6) . ? N3 C10 1.343(6) . ? C1 C2 1.385(6) . ? C1 H1A 0.9300 . ? N2 C2 1.369(6) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? C2 C3 1.402(7) . ? C5 C4 1.396(7) . ? C5 C6 1.457(7) . ? C4 C3 1.359(7) . ? C4 H4A 0.9300 . ? C3 H3A 0.9300 . ? C6 C7 1.384(7) . ? C7 C8 1.345(8) . ? C7 H7A 0.9300 . ? C10 C9 1.412(8) . ? C10 H10A 0.9300 . ? C8 C9 1.379(9) . ? C8 H8A 0.9300 . ? C9 N4 1.392(8) . ? N4 H4B 0.8600 . ? N4 H4C 0.8600 . ? S O3 1.432(4) 2_665 ? S O3 1.432(4) 3_565 ? S O3 1.432(4) . ? S O2 1.468(7) . ? N8 C18 1.454(5) . ? N8 C18 1.454(5) 3_565 ? N8 C18 1.454(5) 2_665 ? O1 C16 1.243(6) . ? N7 C16 1.333(6) . ? N7 C17 1.468(6) . ? N7 H7B 0.8600 . ? C16 N6 1.353(6) . ? C18 C17 1.498(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? N6 C12 1.388(6) . ? N6 H6A 0.8600 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? N5 C15 1.313(12) . ? N5 C11 1.354(8) . ? C12 C13 1.370(8) . ? C12 C11 1.393(8) . ? C13 C14 1.415(10) . ? C13 H13A 0.9300 . ? C14 C15 1.314(12) . ? C14 H14A 0.9300 . ? C11 H11A 0.9300 . ? C15 H15A 0.9300 . ? 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 N1 Fe N1 93.08(15) . 2 ? N1 Fe N1 93.08(15) . 3 ? N1 Fe N1 93.08(15) 2 3 ? N1 Fe N3 91.99(15) . 2 ? N1 Fe N3 80.83(16) 2 2 ? N1 Fe N3 172.28(16) 3 2 ? N1 Fe N3 172.28(16) . 3 ? N1 Fe N3 91.99(15) 2 3 ? N1 Fe N3 80.83(16) 3 3 ? N3 Fe N3 94.56(16) 2 3 ? N1 Fe N3 80.83(16) . . ? N1 Fe N3 172.28(16) 2 . ? N1 Fe N3 91.99(15) 3 . ? N3 Fe N3 94.56(16) 2 . ? N3 Fe N3 94.56(16) 3 . ? C5 N1 C1 117.6(4) . . ? C5 N1 Fe 115.4(3) . . ? C1 N1 Fe 126.2(3) . . ? C6 N3 C10 118.7(5) . . ? C6 N3 Fe 115.2(3) . . ? C10 N3 Fe 126.1(4) . . ? N1 C1 C2 124.0(4) . . ? N1 C1 H1A 118.0 . . ? C2 C1 H1A 118.0 . . ? C2 N2 H2A 120.0 . . ? C2 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? N2 C2 C1 119.7(4) . . ? N2 C2 C3 123.2(5) . . ? C1 C2 C3 116.9(5) . . ? N1 C5 C4 121.2(4) . . ? N1 C5 C6 113.9(4) . . ? C4 C5 C6 124.8(4) . . ? C3 C4 C5 120.3(5) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? N3 C6 C7 121.0(5) . . ? N3 C6 C5 114.5(4) . . ? C7 C6 C5 124.5(5) . . ? C8 C7 C6 121.0(5) . . ? C8 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? N3 C10 C9 122.1(6) . . ? N3 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? C7 C8 C9 119.6(5) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C8 C9 N4 124.7(6) . . ? C8 C9 C10 117.6(6) . . ? N4 C9 C10 117.7(7) . . ? C9 N4 H4B 120.0 . . ? C9 N4 H4C 120.0 . . ? H4B N4 H4C 120.0 . . ? O3 S O3 110.5(2) 2_665 3_565 ? O3 S O3 110.5(2) 2_665 . ? O3 S O3 110.5(2) 3_565 . ? O3 S O2 108.4(2) 2_665 . ? O3 S O2 108.4(2) 3_565 . ? O3 S O2 108.4(2) . . ? C18 N8 C18 110.4(3) . 3_565 ? C18 N8 C18 110.4(3) . 2_665 ? C18 N8 C18 110.4(3) 3_565 2_665 ? C16 N7 C17 121.4(4) . . ? C16 N7 H7B 119.3 . . ? C17 N7 H7B 119.3 . . ? O1 C16 N7 121.4(5) . . ? O1 C16 N6 122.7(5) . . ? N7 C16 N6 115.9(5) . . ? N8 C18 C17 113.7(4) . . ? N8 C18 H18A 108.8 . . ? C17 C18 H18A 108.8 . . ? N8 C18 H18B 108.8 . . ? C17 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C16 N6 C12 126.0(4) . . ? C16 N6 H6A 117.0 . . ? C12 N6 H6A 117.0 . . ? N7 C17 C18 111.5(4) . . ? N7 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N7 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C15 N5 C11 118.6(8) . . ? C13 C12 N6 125.8(6) . . ? C13 C12 C11 118.1(6) . . ? N6 C12 C11 116.1(5) . . ? C12 C13 C14 116.6(7) . . ? C12 C13 H13A 121.7 . . ? C14 C13 H13A 121.7 . . ? C15 C14 C13 122.1(9) . . ? C15 C14 H14A 118.9 . . ? C13 C14 H14A 118.9 . . ? N5 C11 C12 122.4(7) . . ? N5 C11 H11A 118.8 . . ? C12 C11 H11A 118.8 . . ? N5 C15 C14 122.2(9) . . ? N5 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe N1 C5 -175.8(3) 2 . . . ? N1 Fe N1 C5 91.0(4) 3 . . . ? N3 Fe N1 C5 -94.9(3) 2 . . . ? N3 Fe N1 C5 53.2(13) 3 . . . ? N3 Fe N1 C5 -0.6(3) . . . . ? N1 Fe N1 C1 15.0(4) 2 . . . ? N1 Fe N1 C1 -78.3(3) 3 . . . ? N3 Fe N1 C1 95.9(4) 2 . . . ? N3 Fe N1 C1 -116.0(12) 3 . . . ? N3 Fe N1 C1 -169.8(4) . . . . ? N1 Fe N3 C6 -2.7(3) . . . . ? N1 Fe N3 C6 35.6(14) 2 . . . ? N1 Fe N3 C6 -95.5(3) 3 . . . ? N3 Fe N3 C6 88.6(4) 2 . . . ? N3 Fe N3 C6 -176.4(3) 3 . . . ? N1 Fe N3 C10 178.7(4) . . . . ? N1 Fe N3 C10 -143.0(11) 2 . . . ? N1 Fe N3 C10 85.9(4) 3 . . . ? N3 Fe N3 C10 -90.0(4) 2 . . . ? N3 Fe N3 C10 4.9(4) 3 . . . ? C5 N1 C1 C2 -3.7(7) . . . . ? Fe N1 C1 C2 165.3(3) . . . . ? N1 C1 C2 N2 -169.5(4) . . . . ? N1 C1 C2 C3 6.5(7) . . . . ? C1 N1 C5 C4 -1.8(6) . . . . ? Fe N1 C5 C4 -172.0(3) . . . . ? C1 N1 C5 C6 173.6(4) . . . . ? Fe N1 C5 C6 3.4(5) . . . . ? N1 C5 C4 C3 4.2(7) . . . . ? C6 C5 C4 C3 -170.6(4) . . . . ? C5 C4 C3 C2 -1.3(7) . . . . ? N2 C2 C3 C4 172.0(4) . . . . ? C1 C2 C3 C4 -3.8(7) . . . . ? C10 N3 C6 C7 2.1(7) . . . . ? Fe N3 C6 C7 -176.7(4) . . . . ? C10 N3 C6 C5 -176.0(4) . . . . ? Fe N3 C6 C5 5.2(5) . . . . ? N1 C5 C6 N3 -5.6(6) . . . . ? C4 C5 C6 N3 169.6(4) . . . . ? N1 C5 C6 C7 176.3(4) . . . . ? C4 C5 C6 C7 -8.5(8) . . . . ? N3 C6 C7 C8 -1.1(8) . . . . ? C5 C6 C7 C8 176.8(5) . . . . ? C6 N3 C10 C9 -1.0(8) . . . . ? Fe N3 C10 C9 177.6(4) . . . . ? C6 C7 C8 C9 -1.0(9) . . . . ? C7 C8 C9 N4 -179.6(7) . . . . ? C7 C8 C9 C10 2.0(9) . . . . ? N3 C10 C9 C8 -1.0(9) . . . . ? N3 C10 C9 N4 -179.6(6) . . . . ? C17 N7 C16 O1 0.0(7) . . . . ? C17 N7 C16 N6 -177.8(4) . . . . ? C18 N8 C18 C17 74.0(7) 3_565 . . . ? C18 N8 C18 C17 -163.6(4) 2_665 . . . ? O1 C16 N6 C12 -0.2(8) . . . . ? N7 C16 N6 C12 177.6(4) . . . . ? C16 N7 C17 C18 150.3(5) . . . . ? N8 C18 C17 N7 62.9(6) . . . . ? C16 N6 C12 C13 22.3(8) . . . . ? C16 N6 C12 C11 -157.3(5) . . . . ? N6 C12 C13 C14 -180.0(5) . . . . ? C11 C12 C13 C14 -0.4(8) . . . . ? C12 C13 C14 C15 -0.3(11) . . . . ? C15 N5 C11 C12 -2.3(11) . . . . ? C13 C12 C11 N5 1.7(9) . . . . ? N6 C12 C11 N5 -178.6(6) . . . . ? C11 N5 C15 C14 1.6(14) . . . . ? C13 C14 C15 N5 -0.3(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6A O3 0.86 2.10 2.932(6) 162.2 3_565 N7 H7B O2 0.86 2.12 2.938(6) 158.4 . N2 H2B O1 0.86 1.96 2.818(5) 174.2 4_566 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.23 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.634 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.072 ###### data_compound2' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H72 Fe N22 O13 S' _chemical_formula_weight 1325.25 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' 'S' 'S' 0.1246 0.1234 '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 trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 14.1477(4) _cell_length_b 14.1477(4) _cell_length_c 18.8263(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3263.38(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8962 _exptl_absorpt_correction_T_max 0.9352 _exptl_absorpt_process_details SADABS _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_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16287 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.23 _reflns_number_total 3531 _reflns_number_gt 2078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^ > 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^)+(0.1529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3531 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.2350 _refine_ls_wR_factor_gt 0.1935 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.0000 0.0000 0.23784(6) 0.0560(4) Uani 1 3 d S . . N1 N 0.0141(3) 0.1231(3) 0.2949(2) 0.0539(10) Uani 1 1 d . . . N3 N 0.1152(3) 0.1225(3) 0.1820(2) 0.0621(11) Uani 1 1 d . . . C1 C -0.0311(4) 0.1161(4) 0.3596(3) 0.0551(12) Uani 1 1 d . . . H1A H -0.0860 0.0480 0.3748 0.066 Uiso 1 1 calc R . . N2 N -0.0378(3) 0.1872(3) 0.4730(2) 0.0711(12) Uani 1 1 d . . . H2A H -0.0800 0.1219 0.4880 0.085 Uiso 1 1 calc R . . H2B H -0.0190 0.2418 0.5009 0.085 Uiso 1 1 calc R . . C2 C -0.0006(4) 0.2043(4) 0.4044(3) 0.0568(12) Uani 1 1 d . . . C5 C 0.0895(4) 0.2236(4) 0.2715(3) 0.0562(12) Uani 1 1 d . . . C4 C 0.1172(4) 0.3169(4) 0.3117(3) 0.0635(13) Uani 1 1 d . . . H4A H 0.1656 0.3855 0.2934 0.076 Uiso 1 1 calc R . . C3 C 0.0739(4) 0.3077(4) 0.3775(3) 0.0642(13) Uani 1 1 d . . . H3A H 0.0936 0.3698 0.4046 0.077 Uiso 1 1 calc R . . C6 C 0.1424(4) 0.2225(4) 0.2054(2) 0.0584(12) Uani 1 1 d . . . C7 C 0.2176(4) 0.3148(4) 0.1692(3) 0.0718(14) Uani 1 1 d . . . H7A H 0.2344 0.3833 0.1859 0.086 Uiso 1 1 calc R . . C10 C 0.1648(5) 0.1134(5) 0.1238(3) 0.0803(16) Uani 1 1 d . . . H10A H 0.1469 0.0442 0.1078 0.096 Uiso 1 1 calc R . . C8 C 0.2668(5) 0.3070(5) 0.1101(3) 0.0831(17) Uani 1 1 d . . . H8A H 0.3163 0.3696 0.0858 0.100 Uiso 1 1 calc R . . C9 C 0.2433(5) 0.2055(6) 0.0859(3) 0.093(2) Uani 1 1 d . . . N4 N 0.2895(6) 0.1875(6) 0.0258(3) 0.155(3) Uani 1 1 d . . . H4B H 0.3363 0.2418 0.0010 0.186 Uiso 1 1 calc R . . H4C H 0.2713 0.1219 0.0136 0.186 Uiso 1 1 calc R . . S S 0.3333 0.6667 0.28583(12) 0.0649(6) Uani 1 3 d S . . O2 O 0.3333 0.6667 0.3638(4) 0.108(2) Uani 1 3 d S . . O3 O 0.4179(4) 0.6469(4) 0.2618(3) 0.1104(15) Uani 1 1 d . . . N8 N 0.3333 0.6667 0.5403(3) 0.0517(16) Uani 1 3 d S . . O1 O -0.0136(3) 0.6308(3) 0.4405(2) 0.0753(10) Uani 1 1 d . . . N7 N 0.1469(3) 0.6351(4) 0.4503(2) 0.0704(12) Uani 1 1 d . . . H7B H 0.1969 0.6275 0.4297 0.085 Uiso 1 1 calc R . . C16 C 0.0606(4) 0.6205(4) 0.4128(3) 0.0618(13) Uani 1 1 d . . . C18 C 0.2215(4) 0.6210(4) 0.5648(3) 0.0624(13) Uani 1 1 d . . . H18A H 0.2223 0.6368 0.6150 0.075 Uiso 1 1 calc R . . H18B H 0.1842 0.5423 0.5594 0.075 Uiso 1 1 calc R . . N6 N 0.0575(3) 0.5905(3) 0.3443(2) 0.0683(11) Uani 1 1 d . . . H6A H 0.1121 0.5855 0.3291 0.082 Uiso 1 1 calc R . . C17 C 0.1583(4) 0.6639(5) 0.5260(3) 0.0705(14) Uani 1 1 d . . . H17A H 0.0864 0.6341 0.5471 0.085 Uiso 1 1 calc R . . H17B H 0.1953 0.7427 0.5308 0.085 Uiso 1 1 calc R . . N5 N -0.1095(6) 0.4739(5) 0.1871(4) 0.128(2) Uani 1 1 d . . . C12 C -0.0258(4) 0.5671(4) 0.2962(3) 0.0708(14) Uani 1 1 d . . . C13 C -0.1000(5) 0.6023(5) 0.3008(3) 0.0905(19) Uani 1 1 d . . . H13A H -0.0987 0.6459 0.3381 0.109 Uiso 1 1 calc R . . C14 C -0.1785(6) 0.5688(8) 0.2459(5) 0.126(3) Uani 1 1 d . . . H14A H -0.2304 0.5908 0.2474 0.151 Uiso 1 1 calc R . . C11 C -0.0336(5) 0.5014(5) 0.2388(4) 0.0943(19) Uani 1 1 d . . . H11A H 0.0151 0.4755 0.2358 0.113 Uiso 1 1 calc R . . C15 C -0.1805(8) 0.5076(8) 0.1927(6) 0.137(4) Uani 1 1 d . . . H15A H -0.2340 0.4874 0.1580 0.165 Uiso 1 1 calc R . . O4 O 0.4441(13) 0.6312(12) 0.1160(5) 0.335(7) Uani 1 1 d . . . O5 O 0.4187(13) 0.4357(14) -0.0547(6) 0.562(18) 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 0.0576(5) 0.0576(5) 0.0530(7) 0.000 0.000 0.0288(3) N1 0.051(2) 0.055(2) 0.058(2) 0.0039(18) -0.0008(18) 0.0283(19) N3 0.061(2) 0.070(3) 0.053(2) 0.003(2) 0.001(2) 0.031(2) C1 0.053(3) 0.051(3) 0.065(3) 0.003(2) 0.005(2) 0.029(2) N2 0.081(3) 0.066(3) 0.066(3) -0.004(2) 0.014(2) 0.036(2) C2 0.049(3) 0.058(3) 0.071(3) -0.002(3) -0.002(2) 0.032(2) C5 0.048(3) 0.055(3) 0.065(3) 0.009(2) -0.002(2) 0.025(2) C4 0.057(3) 0.052(3) 0.079(4) 0.011(3) 0.008(3) 0.026(2) C3 0.056(3) 0.049(3) 0.086(4) -0.007(3) -0.003(3) 0.026(2) C6 0.054(3) 0.064(3) 0.057(3) 0.007(2) 0.001(2) 0.029(2) C7 0.062(3) 0.063(3) 0.075(4) 0.004(3) -0.005(3) 0.020(3) C10 0.086(4) 0.085(4) 0.060(3) -0.002(3) 0.007(3) 0.035(3) C8 0.071(4) 0.083(4) 0.064(4) 0.010(3) 0.008(3) 0.015(3) C9 0.083(4) 0.115(5) 0.063(4) 0.009(4) 0.024(3) 0.035(4) N4 0.165(6) 0.134(5) 0.096(4) -0.005(4) 0.074(5) 0.022(4) S 0.0686(9) 0.0686(9) 0.0574(14) 0.000 0.000 0.0343(5) O2 0.124(4) 0.124(4) 0.075(5) 0.000 0.000 0.0622(19) O3 0.092(3) 0.126(4) 0.136(4) 0.014(3) 0.025(3) 0.072(3) N8 0.049(2) 0.049(2) 0.058(4) 0.000 0.000 0.0244(11) O1 0.0464(19) 0.077(2) 0.098(3) -0.019(2) -0.0055(19) 0.0277(18) N7 0.056(2) 0.092(3) 0.073(3) -0.007(2) -0.004(2) 0.044(2) C16 0.050(3) 0.049(3) 0.080(4) -0.004(2) -0.005(3) 0.019(2) C18 0.057(3) 0.064(3) 0.064(3) 0.003(2) 0.010(2) 0.028(2) N6 0.056(2) 0.074(3) 0.073(3) -0.007(2) -0.004(2) 0.030(2) C17 0.056(3) 0.091(4) 0.070(4) -0.006(3) 0.000(3) 0.041(3) N5 0.120(5) 0.102(5) 0.114(5) -0.019(4) -0.045(5) 0.020(4) C12 0.061(3) 0.055(3) 0.077(4) 0.010(3) -0.006(3) 0.014(3) C13 0.067(4) 0.101(5) 0.095(5) 0.016(4) -0.005(3) 0.036(4) C14 0.068(4) 0.155(8) 0.144(7) 0.049(6) -0.004(5) 0.048(5) C11 0.090(4) 0.071(4) 0.099(5) -0.013(4) -0.027(4) 0.023(3) C15 0.111(7) 0.132(8) 0.118(7) 0.001(6) -0.040(6) 0.023(6) O4 0.49(2) 0.431(18) 0.177(8) -0.045(11) 0.023(11) 0.297(17) O5 0.437(19) 0.51(2) 0.203(10) -0.092(12) 0.214(12) -0.166(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1 1.969(4) . ? Fe N1 1.969(4) 2 ? Fe N1 1.969(4) 3 ? Fe N3 1.985(4) 2 ? Fe N3 1.985(4) 3 ? Fe N3 1.985(4) . ? N1 C5 1.356(6) . ? N1 C1 1.357(6) . ? N3 C6 1.340(6) . ? N3 C10 1.343(6) . ? C1 C2 1.385(6) . ? C1 H1A 0.9300 . ? N2 C2 1.369(6) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? C2 C3 1.402(7) . ? C5 C4 1.396(7) . ? C5 C6 1.457(7) . ? C4 C3 1.359(7) . ? C4 H4A 0.9300 . ? C3 H3A 0.9300 . ? C6 C7 1.384(7) . ? C7 C8 1.345(8) . ? C7 H7A 0.9300 . ? C10 C9 1.412(8) . ? C10 H10A 0.9300 . ? C8 C9 1.379(9) . ? C8 H8A 0.9300 . ? C9 N4 1.392(8) . ? N4 H4B 0.8600 . ? N4 H4C 0.8600 . ? S O3 1.432(4) 2_665 ? S O3 1.432(4) 3_565 ? S O3 1.432(4) . ? S O2 1.468(7) . ? N8 C18 1.454(5) . ? N8 C18 1.454(5) 3_565 ? N8 C18 1.454(5) 2_665 ? O1 C16 1.243(6) . ? N7 C16 1.333(6) . ? N7 C17 1.468(6) . ? N7 H7B 0.8600 . ? C16 N6 1.353(6) . ? C18 C17 1.498(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? N6 C12 1.388(6) . ? N6 H6A 0.8600 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? N5 C15 1.313(12) . ? N5 C11 1.354(8) . ? C12 C13 1.370(8) . ? C12 C11 1.393(8) . ? C13 C14 1.415(10) . ? C13 H13A 0.9300 . ? C14 C15 1.314(12) . ? C14 H14A 0.9300 . ? C11 H11A 0.9300 . ? C15 H15A 0.9300 . ? 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 N1 Fe N1 93.08(15) . 2 ? N1 Fe N1 93.08(15) . 3 ? N1 Fe N1 93.08(15) 2 3 ? N1 Fe N3 91.99(15) . 2 ? N1 Fe N3 80.83(16) 2 2 ? N1 Fe N3 172.28(16) 3 2 ? N1 Fe N3 172.28(16) . 3 ? N1 Fe N3 91.99(15) 2 3 ? N1 Fe N3 80.83(16) 3 3 ? N3 Fe N3 94.56(16) 2 3 ? N1 Fe N3 80.83(16) . . ? N1 Fe N3 172.28(16) 2 . ? N1 Fe N3 91.99(15) 3 . ? N3 Fe N3 94.56(16) 2 . ? N3 Fe N3 94.56(16) 3 . ? C5 N1 C1 117.6(4) . . ? C5 N1 Fe 115.4(3) . . ? C1 N1 Fe 126.2(3) . . ? C6 N3 C10 118.7(5) . . ? C6 N3 Fe 115.2(3) . . ? C10 N3 Fe 126.1(4) . . ? N1 C1 C2 124.0(4) . . ? N1 C1 H1A 118.0 . . ? C2 C1 H1A 118.0 . . ? C2 N2 H2A 120.0 . . ? C2 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? N2 C2 C1 119.7(4) . . ? N2 C2 C3 123.2(5) . . ? C1 C2 C3 116.9(5) . . ? N1 C5 C4 121.2(4) . . ? N1 C5 C6 113.9(4) . . ? C4 C5 C6 124.8(4) . . ? C3 C4 C5 120.3(5) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? N3 C6 C7 121.0(5) . . ? N3 C6 C5 114.5(4) . . ? C7 C6 C5 124.5(5) . . ? C8 C7 C6 121.0(5) . . ? C8 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? N3 C10 C9 122.1(6) . . ? N3 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? C7 C8 C9 119.6(5) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C8 C9 N4 124.7(6) . . ? C8 C9 C10 117.6(6) . . ? N4 C9 C10 117.7(7) . . ? C9 N4 H4B 120.0 . . ? C9 N4 H4C 120.0 . . ? H4B N4 H4C 120.0 . . ? O3 S O3 110.5(2) 2_665 3_565 ? O3 S O3 110.5(2) 2_665 . ? O3 S O3 110.5(2) 3_565 . ? O3 S O2 108.4(2) 2_665 . ? O3 S O2 108.4(2) 3_565 . ? O3 S O2 108.4(2) . . ? C18 N8 C18 110.4(3) . 3_565 ? C18 N8 C18 110.4(3) . 2_665 ? C18 N8 C18 110.4(3) 3_565 2_665 ? C16 N7 C17 121.4(4) . . ? C16 N7 H7B 119.3 . . ? C17 N7 H7B 119.3 . . ? O1 C16 N7 121.4(5) . . ? O1 C16 N6 122.7(5) . . ? N7 C16 N6 115.9(5) . . ? N8 C18 C17 113.7(4) . . ? N8 C18 H18A 108.8 . . ? C17 C18 H18A 108.8 . . ? N8 C18 H18B 108.8 . . ? C17 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C16 N6 C12 126.0(4) . . ? C16 N6 H6A 117.0 . . ? C12 N6 H6A 117.0 . . ? N7 C17 C18 111.5(4) . . ? N7 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N7 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C15 N5 C11 118.6(8) . . ? C13 C12 N6 125.8(6) . . ? C13 C12 C11 118.1(6) . . ? N6 C12 C11 116.1(5) . . ? C12 C13 C14 116.6(7) . . ? C12 C13 H13A 121.7 . . ? C14 C13 H13A 121.7 . . ? C15 C14 C13 122.1(9) . . ? C15 C14 H14A 118.9 . . ? C13 C14 H14A 118.9 . . ? N5 C11 C12 122.4(7) . . ? N5 C11 H11A 118.8 . . ? C12 C11 H11A 118.8 . . ? N5 C15 C14 122.2(9) . . ? N5 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe N1 C5 -175.8(3) 2 . . . ? N1 Fe N1 C5 91.0(4) 3 . . . ? N3 Fe N1 C5 -94.9(3) 2 . . . ? N3 Fe N1 C5 53.2(13) 3 . . . ? N3 Fe N1 C5 -0.6(3) . . . . ? N1 Fe N1 C1 15.0(4) 2 . . . ? N1 Fe N1 C1 -78.3(3) 3 . . . ? N3 Fe N1 C1 95.9(4) 2 . . . ? N3 Fe N1 C1 -116.0(12) 3 . . . ? N3 Fe N1 C1 -169.8(4) . . . . ? N1 Fe N3 C6 -2.7(3) . . . . ? N1 Fe N3 C6 35.6(14) 2 . . . ? N1 Fe N3 C6 -95.5(3) 3 . . . ? N3 Fe N3 C6 88.6(4) 2 . . . ? N3 Fe N3 C6 -176.4(3) 3 . . . ? N1 Fe N3 C10 178.7(4) . . . . ? N1 Fe N3 C10 -143.0(11) 2 . . . ? N1 Fe N3 C10 85.9(4) 3 . . . ? N3 Fe N3 C10 -90.0(4) 2 . . . ? N3 Fe N3 C10 4.9(4) 3 . . . ? C5 N1 C1 C2 -3.7(7) . . . . ? Fe N1 C1 C2 165.3(3) . . . . ? N1 C1 C2 N2 -169.5(4) . . . . ? N1 C1 C2 C3 6.5(7) . . . . ? C1 N1 C5 C4 -1.8(6) . . . . ? Fe N1 C5 C4 -172.0(3) . . . . ? C1 N1 C5 C6 173.6(4) . . . . ? Fe N1 C5 C6 3.4(5) . . . . ? N1 C5 C4 C3 4.2(7) . . . . ? C6 C5 C4 C3 -170.6(4) . . . . ? C5 C4 C3 C2 -1.3(7) . . . . ? N2 C2 C3 C4 172.0(4) . . . . ? C1 C2 C3 C4 -3.8(7) . . . . ? C10 N3 C6 C7 2.1(7) . . . . ? Fe N3 C6 C7 -176.7(4) . . . . ? C10 N3 C6 C5 -176.0(4) . . . . ? Fe N3 C6 C5 5.2(5) . . . . ? N1 C5 C6 N3 -5.6(6) . . . . ? C4 C5 C6 N3 169.6(4) . . . . ? N1 C5 C6 C7 176.3(4) . . . . ? C4 C5 C6 C7 -8.5(8) . . . . ? N3 C6 C7 C8 -1.1(8) . . . . ? C5 C6 C7 C8 176.8(5) . . . . ? C6 N3 C10 C9 -1.0(8) . . . . ? Fe N3 C10 C9 177.6(4) . . . . ? C6 C7 C8 C9 -1.0(9) . . . . ? C7 C8 C9 N4 -179.6(7) . . . . ? C7 C8 C9 C10 2.0(9) . . . . ? N3 C10 C9 C8 -1.0(9) . . . . ? N3 C10 C9 N4 -179.6(6) . . . . ? C17 N7 C16 O1 0.0(7) . . . . ? C17 N7 C16 N6 -177.8(4) . . . . ? C18 N8 C18 C17 74.0(7) 3_565 . . . ? C18 N8 C18 C17 -163.6(4) 2_665 . . . ? O1 C16 N6 C12 -0.2(8) . . . . ? N7 C16 N6 C12 177.6(4) . . . . ? C16 N7 C17 C18 150.3(5) . . . . ? N8 C18 C17 N7 62.9(6) . . . . ? C16 N6 C12 C13 22.3(8) . . . . ? C16 N6 C12 C11 -157.3(5) . . . . ? N6 C12 C13 C14 -180.0(5) . . . . ? C11 C12 C13 C14 -0.4(8) . . . . ? C12 C13 C14 C15 -0.3(11) . . . . ? C15 N5 C11 C12 -2.3(11) . . . . ? C13 C12 C11 N5 1.7(9) . . . . ? N6 C12 C11 N5 -178.6(6) . . . . ? C11 N5 C15 C14 1.6(14) . . . . ? C13 C14 C15 N5 -0.3(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6A O3 0.86 2.10 2.932(6) 162.2 3_565 N7 H7B O2 0.86 2.12 2.938(6) 158.4 . N2 H2B O1 0.86 1.96 2.818(5) 174.2 4_566 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.23 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.634 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.072 ########### data_Fe(BIPY)3LSO4(H2O)9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H72 Fe N16 O16 S' _chemical_formula_weight 1289.19 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 13.9945(9) _cell_length_b 13.9945(9) _cell_length_c 116.519(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 19763(3) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8136 _exptl_absorpt_coefficient_mu 0.335 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8917 _exptl_absorpt_correction_T_max 0.9061 _exptl_absorpt_process_details SADABS _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_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40415 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -137 _diffrn_reflns_limit_l_max 136 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.77 _reflns_number_total 3783 _reflns_number_gt 2297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^ > 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^)+(0.1925P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3783 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.2907 _refine_ls_wR_factor_gt 0.2435 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.041 0.333 0.083 77 8 ' ' 2 0.000 0.626 0.250 75 8 ' ' 3 0.000 0.000 0.250 20 2 ' ' 4 -0.041 0.292 0.417 76 8 ' ' 5 0.041 0.708 0.583 76 8 ' ' 6 0.000 0.374 0.750 75 8 ' ' 7 0.000 0.000 0.750 20 2 ' ' 8 -0.041 0.667 0.917 77 8 ' ' 9 0.292 0.959 0.083 76 8 ' ' 10 0.292 0.333 0.583 76 8 ' ' 11 0.333 0.041 0.417 76 8 ' ' 12 0.333 0.292 0.917 76 8 ' ' 13 0.374 0.374 0.250 76 8 ' ' 14 0.374 1.000 0.750 75 8 ' ' 15 0.333 0.667 0.417 22 2 ' ' 16 0.333 0.667 0.917 22 2 ' ' 17 0.626 1.000 0.250 75 8 ' ' 18 0.626 0.626 0.750 76 8 ' ' 19 0.667 0.708 0.083 76 8 ' ' 20 0.667 0.959 0.583 76 8 ' ' 21 0.708 0.667 0.417 76 8 ' ' 22 0.708 1.041 0.917 76 8 ' ' 23 0.667 0.333 0.083 22 2 ' ' 24 0.667 0.333 0.583 22 2 ' ' 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 0.0000 0.046998(8) 0.0548(4) Uani 1 3 d S . . N1 N 0.1231(3) 0.1159(4) 0.05602(3) 0.0680(11) Uani 1 1 d . . . N2 N 0.0236(3) 0.1299(3) 0.03814(3) 0.0568(9) Uani 1 1 d . . . N5 N 0.5265(4) 0.4108(5) 0.05347(5) 0.1011(16) Uani 1 1 d . . . N6 N 0.4097(3) 0.4628(3) 0.02779(4) 0.0746(11) Uani 1 1 d . . . H6 H 0.4144 0.5226 0.0304 0.089 Uiso 1 1 calc R . . N7 N 0.3321(4) 0.4943(4) 0.01219(4) 0.0876(14) Uani 1 1 d . . . H7B H 0.3321 0.5462 0.0161 0.105 Uiso 1 1 calc R . . N8 N 0.3333 0.6667 -0.00301(6) 0.0665(17) Uani 1 3 d S . . O1 O 0.3704(4) 0.3560(3) 0.01179(4) 0.0913(12) Uani 1 1 d . . . S1 S 0.3333 0.6667 0.03930(2) 0.0660(6) Uani 1 3 d S . . O2 O 0.3333 0.6667 0.02673(6) 0.100(2) Uani 1 3 d S . . O3 O 0.3958(5) 0.7774(4) 0.04350(4) 0.135(2) Uani 1 1 d . . . O4 O 0.9893(3) 0.8214(4) 0.00549(4) 0.0984(12) Uani 1 1 d . . . O5 O 0.8937(18) 0.4178(11) 0.07591(11) 0.64(3) Uani 1 1 d . . . O6 O 0.1720(15) 0.547(3) 0.06808(13) 0.503(18) Uani 1 1 d . . . C1 C 0.1728(5) 0.1005(6) 0.06504(5) 0.0896(17) Uani 1 1 d . . . H1 H 0.1508 0.0291 0.0675 0.107 Uiso 1 1 calc R . . C2 C 0.2576(6) 0.1904(7) 0.07093(5) 0.100(2) Uani 1 1 d . . . H2 H 0.2914 0.1781 0.0772 0.120 Uiso 1 1 calc R . . C3 C 0.2899(6) 0.2930(7) 0.06763(6) 0.108(2) Uani 1 1 d . . . H3 H 0.3448 0.3526 0.0717 0.129 Uiso 1 1 calc R . . C4 C 0.2414(5) 0.3099(5) 0.05825(5) 0.0936(18) Uani 1 1 d . . . H4 H 0.2635 0.3811 0.0558 0.112 Uiso 1 1 calc R . . C5 C 0.1593(4) 0.2198(4) 0.05256(4) 0.0687(13) Uani 1 1 d . . . C6 C 0.1017(4) 0.2289(4) 0.04250(4) 0.0629(12) Uani 1 1 d . . . C7 C 0.1237(5) 0.3271(4) 0.03749(5) 0.0829(16) Uani 1 1 d . . . H7A H 0.1765 0.3941 0.0406 0.100 Uiso 1 1 calc R . . C8 C 0.0666(6) 0.3244(5) 0.02784(6) 0.0891(17) Uani 1 1 d . . . H8 H 0.0798 0.3896 0.0244 0.107 Uiso 1 1 calc R . . C9 C -0.0089(5) 0.2260(5) 0.02346(5) 0.0832(16) Uani 1 1 d . . . H9 H -0.0473 0.2234 0.0168 0.100 Uiso 1 1 calc R . . C10 C -0.0294(4) 0.1304(4) 0.02869(4) 0.0687(13) Uani 1 1 d . . . H10 H -0.0820 0.0634 0.0255 0.082 Uiso 1 1 calc R . . C11 C 0.4948(4) 0.4574(5) 0.04515(6) 0.0839(16) Uani 1 1 d . . . H11 H 0.5098 0.5294 0.0463 0.101 Uiso 1 1 calc R . . C12 C 0.4431(4) 0.4069(4) 0.03533(5) 0.0734(13) Uani 1 1 d . . . C13 C 0.4216(6) 0.2992(5) 0.03337(6) 0.0993(19) Uani 1 1 d . . . H13 H 0.3854 0.2600 0.0268 0.119 Uiso 1 1 calc R . . C14 C 0.4569(8) 0.2550(7) 0.04169(8) 0.119(3) Uani 1 1 d . . . H14 H 0.4473 0.1850 0.0406 0.142 Uiso 1 1 calc R . . C15 C 0.5037(6) 0.3075(7) 0.05119(7) 0.109(2) Uani 1 1 d . . . H15 H 0.5222 0.2711 0.0567 0.130 Uiso 1 1 calc R . . C16 C 0.3711(4) 0.4343(4) 0.01701(5) 0.0729(14) Uani 1 1 d . . . C17 C 0.2898(7) 0.4757(5) 0.00057(6) 0.107(2) Uani 1 1 d . . . H17A H 0.2119 0.4527 0.0008 0.128 Uiso 1 1 calc R . . H17B H 0.2969 0.4163 -0.0028 0.128 Uiso 1 1 calc R . . C18 C 0.3491(5) 0.5767(5) -0.00681(5) 0.0867(16) Uani 1 1 d . . . H18A H 0.4274 0.6013 -0.0068 0.104 Uiso 1 1 calc R . . H18B H 0.3230 0.5577 -0.0146 0.104 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 0.0554(5) 0.0554(5) 0.0536(7) 0.000 0.000 0.0277(3) N1 0.068(2) 0.078(3) 0.056(2) -0.0091(19) -0.0061(19) 0.035(2) N2 0.058(2) 0.053(2) 0.062(2) -0.0013(17) 0.0042(17) 0.0295(18) N5 0.088(3) 0.118(4) 0.112(4) 0.001(3) -0.011(3) 0.063(3) N6 0.071(3) 0.061(2) 0.094(3) -0.011(2) -0.009(2) 0.035(2) N7 0.105(4) 0.063(3) 0.101(3) -0.017(2) -0.027(3) 0.047(3) N8 0.064(3) 0.064(3) 0.071(4) 0.000 0.000 0.0321(13) O1 0.097(3) 0.077(2) 0.116(3) -0.018(2) -0.008(2) 0.055(2) S1 0.0565(8) 0.0565(8) 0.0848(14) 0.000 0.000 0.0283(4) O2 0.105(3) 0.105(3) 0.091(5) 0.000 0.000 0.0524(17) O3 0.168(5) 0.072(3) 0.121(4) -0.010(3) 0.032(3) 0.028(3) O4 0.083(3) 0.102(3) 0.119(3) 0.007(2) 0.008(2) 0.053(2) O5 0.89(5) 0.239(12) 0.266(13) 0.125(10) -0.32(2) -0.113(18) O6 0.39(2) 0.96(6) 0.269(14) -0.08(2) 0.032(15) 0.42(3) C1 0.090(4) 0.108(5) 0.070(3) -0.015(3) -0.021(3) 0.049(4) C2 0.090(4) 0.115(6) 0.080(4) -0.021(4) -0.029(3) 0.040(4) C3 0.083(4) 0.113(6) 0.094(4) -0.030(4) -0.016(4) 0.025(4) C4 0.075(4) 0.084(4) 0.092(4) -0.019(3) 0.002(3) 0.017(3) C5 0.061(3) 0.065(3) 0.068(3) -0.012(2) 0.007(2) 0.022(2) C6 0.063(3) 0.057(3) 0.067(3) -0.004(2) 0.009(2) 0.029(2) C7 0.083(4) 0.050(3) 0.103(4) -0.006(3) 0.008(3) 0.023(3) C8 0.113(5) 0.071(4) 0.096(4) 0.017(3) 0.020(4) 0.055(4) C9 0.104(4) 0.078(4) 0.082(3) 0.011(3) -0.003(3) 0.056(4) C10 0.084(4) 0.068(3) 0.065(3) 0.003(2) -0.004(2) 0.047(3) C11 0.061(3) 0.079(4) 0.111(4) -0.003(3) -0.001(3) 0.035(3) C12 0.060(3) 0.062(3) 0.103(4) 0.001(3) 0.000(3) 0.034(2) C13 0.109(5) 0.083(4) 0.121(5) -0.004(4) -0.003(4) 0.059(4) C14 0.155(7) 0.096(5) 0.136(6) 0.004(5) -0.023(5) 0.086(5) C15 0.111(5) 0.118(6) 0.130(6) 0.014(5) -0.002(5) 0.082(5) C16 0.060(3) 0.057(3) 0.102(4) -0.002(3) -0.002(3) 0.029(2) C17 0.131(6) 0.074(4) 0.119(5) -0.026(4) -0.036(4) 0.054(4) C18 0.096(4) 0.088(4) 0.081(3) -0.018(3) -0.010(3) 0.050(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 Fe1 N2 1.970(4) . ? Fe1 N2 1.970(4) 2 ? Fe1 N2 1.970(4) 3 ? Fe1 N1 1.977(4) 3 ? Fe1 N1 1.977(4) 2 ? Fe1 N1 1.977(4) . ? N1 C1 1.336(7) . ? N1 C5 1.341(7) . ? N2 C10 1.329(6) . ? N2 C6 1.362(6) . ? N5 C15 1.342(9) . ? N5 C11 1.362(8) . ? N6 C16 1.347(7) . ? N6 C12 1.403(7) . ? N6 H6 0.8600 . ? N7 C16 1.332(7) . ? N7 C17 1.448(8) . ? N7 H7B 0.8600 . ? N8 C18 1.452(6) 3_565 ? N8 C18 1.452(6) 2_665 ? N8 C18 1.452(6) . ? O1 C16 1.248(6) . ? S1 O3 1.431(5) 2_665 ? S1 O3 1.431(5) . ? S1 O3 1.431(5) 3_565 ? S1 O2 1.464(8) . ? C1 C2 1.403(9) . ? C1 H1 0.9300 . ? C2 C3 1.328(10) . ? C2 H2 0.9300 . ? C3 C4 1.368(10) . ? C3 H3 0.9300 . ? C4 C5 1.379(7) . ? C4 H4 0.9300 . ? C5 C6 1.464(7) . ? C6 C7 1.380(7) . ? C7 C8 1.368(9) . ? C7 H7A 0.9300 . ? C8 C9 1.348(8) . ? C8 H8 0.9300 . ? C9 C10 1.364(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.349(8) . ? C11 H11 0.9300 . ? C12 C13 1.401(8) . ? C13 C14 1.368(9) . ? C13 H13 0.9300 . ? C14 C15 1.308(10) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C17 C18 1.502(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? 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 Fe1 N2 95.08(14) . 2 ? N2 Fe1 N2 95.08(14) . 3 ? N2 Fe1 N2 95.08(14) 2 3 ? N2 Fe1 N1 174.19(16) . 3 ? N2 Fe1 N1 89.67(15) 2 3 ? N2 Fe1 N1 81.15(16) 3 3 ? N2 Fe1 N1 89.67(15) . 2 ? N2 Fe1 N1 81.15(16) 2 2 ? N2 Fe1 N1 174.19(16) 3 2 ? N1 Fe1 N1 94.37(16) 3 2 ? N2 Fe1 N1 81.15(16) . . ? N2 Fe1 N1 174.19(16) 2 . ? N2 Fe1 N1 89.67(15) 3 . ? N1 Fe1 N1 94.37(16) 3 . ? N1 Fe1 N1 94.37(16) 2 . ? C1 N1 C5 117.8(5) . . ? C1 N1 Fe1 126.6(4) . . ? C5 N1 Fe1 115.6(3) . . ? C10 N2 C6 118.0(4) . . ? C10 N2 Fe1 127.0(3) . . ? C6 N2 Fe1 114.9(3) . . ? C15 N5 C11 114.7(6) . . ? C16 N6 C12 127.9(4) . . ? C16 N6 H6 116.0 . . ? C12 N6 H6 116.0 . . ? C16 N7 C17 122.7(5) . . ? C16 N7 H7B 118.7 . . ? C17 N7 H7B 118.7 . . ? C18 N8 C18 111.1(3) 3_565 2_665 ? C18 N8 C18 111.1(3) 3_565 . ? C18 N8 C18 111.1(3) 2_665 . ? O3 S1 O3 109.0(2) 2_665 . ? O3 S1 O3 109.0(2) 2_665 3_565 ? O3 S1 O3 109.0(2) . 3_565 ? O3 S1 O2 110.0(2) 2_665 . ? O3 S1 O2 110.0(2) . . ? O3 S1 O2 110.0(2) 3_565 . ? N1 C1 C2 121.0(6) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 120.4(6) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 119.2(6) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.0(7) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.5(5) . . ? N1 C5 C6 114.1(4) . . ? C4 C5 C6 123.3(5) . . ? N2 C6 C7 121.4(5) . . ? N2 C6 C5 114.1(4) . . ? C7 C6 C5 124.5(5) . . ? C8 C7 C6 118.9(5) . . ? C8 C7 H7A 120.6 . . ? C6 C7 H7A 120.6 . . ? C9 C8 C7 119.3(5) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 120.3(6) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? N2 C10 C9 122.0(5) . . ? N2 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C12 C11 N5 124.8(6) . . ? C12 C11 H11 117.6 . . ? N5 C11 H11 117.6 . . ? C11 C12 C13 118.2(6) . . ? C11 C12 N6 118.7(5) . . ? C13 C12 N6 123.1(5) . . ? C14 C13 C12 116.0(7) . . ? C14 C13 H13 122.0 . . ? C12 C13 H13 122.0 . . ? C15 C14 C13 122.6(7) . . ? C15 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? C14 C15 N5 123.6(7) . . ? C14 C15 H15 118.2 . . ? N5 C15 H15 118.2 . . ? O1 C16 N7 121.5(5) . . ? O1 C16 N6 122.8(5) . . ? N7 C16 N6 115.8(5) . . ? N7 C17 C18 112.5(5) . . ? N7 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? N7 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? N8 C18 C17 112.9(5) . . ? N8 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? N8 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 N1 C1 -177.4(5) . . . . ? N2 Fe1 N1 C1 132.9(15) 2 . . . ? N2 Fe1 N1 C1 -82.2(4) 3 . . . ? N1 Fe1 N1 C1 -1.1(5) 3 . . . ? N1 Fe1 N1 C1 93.6(4) 2 . . . ? N2 Fe1 N1 C5 2.4(3) . . . . ? N2 Fe1 N1 C5 -47.3(17) 2 . . . ? N2 Fe1 N1 C5 97.6(4) 3 . . . ? N1 Fe1 N1 C5 178.7(3) 3 . . . ? N1 Fe1 N1 C5 -86.6(4) 2 . . . ? N2 Fe1 N2 C10 -6.8(4) 2 . . . ? N2 Fe1 N2 C10 88.8(3) 3 . . . ? N1 Fe1 N2 C10 138.0(15) 3 . . . ? N1 Fe1 N2 C10 -87.9(4) 2 . . . ? N1 Fe1 N2 C10 177.7(4) . . . . ? N2 Fe1 N2 C6 172.0(3) 2 . . . ? N2 Fe1 N2 C6 -92.4(4) 3 . . . ? N1 Fe1 N2 C6 -43.2(17) 3 . . . ? N1 Fe1 N2 C6 90.9(3) 2 . . . ? N1 Fe1 N2 C6 -3.6(3) . . . . ? C5 N1 C1 C2 2.0(8) . . . . ? Fe1 N1 C1 C2 -178.2(4) . . . . ? N1 C1 C2 C3 0.3(10) . . . . ? C1 C2 C3 C4 -1.7(11) . . . . ? C2 C3 C4 C5 0.8(10) . . . . ? C1 N1 C5 C4 -2.9(7) . . . . ? Fe1 N1 C5 C4 177.2(4) . . . . ? C1 N1 C5 C6 178.9(4) . . . . ? Fe1 N1 C5 C6 -0.9(5) . . . . ? C3 C4 C5 N1 1.5(9) . . . . ? C3 C4 C5 C6 179.6(5) . . . . ? C10 N2 C6 C7 1.7(7) . . . . ? Fe1 N2 C6 C7 -177.2(4) . . . . ? C10 N2 C6 C5 -177.1(4) . . . . ? Fe1 N2 C6 C5 4.0(5) . . . . ? N1 C5 C6 N2 -2.0(6) . . . . ? C4 C5 C6 N2 179.8(5) . . . . ? N1 C5 C6 C7 179(58) . . . . ? C4 C5 C6 C7 1.1(8) . . . . ? N2 C6 C7 C8 -0.9(8) . . . . ? C5 C6 C7 C8 177.7(5) . . . . ? C6 C7 C8 C9 -0.5(9) . . . . ? C7 C8 C9 C10 1.0(9) . . . . ? C6 N2 C10 C9 -1.1(7) . . . . ? Fe1 N2 C10 C9 177.6(4) . . . . ? C8 C9 C10 N2 -0.2(9) . . . . ? C15 N5 C11 C12 0.8(9) . . . . ? N5 C11 C12 C13 -1.0(9) . . . . ? N5 C11 C12 N6 176.5(5) . . . . ? C16 N6 C12 C11 170.2(5) . . . . ? C16 N6 C12 C13 -12.4(9) . . . . ? C11 C12 C13 C14 -0.8(9) . . . . ? N6 C12 C13 C14 -178.2(6) . . . . ? C12 C13 C14 C15 3.0(12) . . . . ? C13 C14 C15 N5 -3.4(14) . . . . ? C11 N5 C15 C14 1.4(11) . . . . ? C17 N7 C16 O1 -1.9(9) . . . . ? C17 N7 C16 N6 178.7(5) . . . . ? C12 N6 C16 O1 -7.5(8) . . . . ? C12 N6 C16 N7 171.9(5) . . . . ? C16 N7 C17 C18 -122.7(6) . . . . ? C18 N8 C18 C17 -79.9(8) 3_565 . . . ? C18 N8 C18 C17 155.8(6) 2_665 . . . ? N7 C17 C18 N8 -64.7(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7B O2 0.86 2.08 2.941(6) 176.0 . N6 H6 O3 0.86 2.09 2.863(7) 148.8 3_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.77 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.802 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.102 ############END