Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'ProfD Kim R. Dunbar' _publ_contact_author_address ; Department of Chemistry Texas A&M University Mail Stop 3255 College Station TX 77842 UNITED STATES OF AMERICA ; _publ_contact_author_email DUNBAR@MAIL.CHEM.TAMU.EDU _publ_section_title ; Structural and magnetic properties of iron(II) complexes with 1,4,5,8,9,12-hexaazatriphenylene (HAT) ; loop_ _publ_author_name 'K. Dunbar' 'Abdellatif Chouai' 'Andrey V. Prosvirin' 'Mikhail Shatruk' data_d:\mike\X-ray\ms023\n_p21 _database_code_depnum_ccdc_archive 'CCDC 264315' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H30 Fe3 N6 O27.32 S3' _chemical_formula_weight 959.27 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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 18.097(17) _cell_length_b 12.469(8) _cell_length_c 15.390(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.460(10) _cell_angle_gamma 90.00 _cell_volume 3443(5) _cell_formula_units_Z 4 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used 68 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1954 _exptl_absorpt_coefficient_mu 1.537 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 383(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 SMART 1000' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8782 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 23.26 _reflns_number_total 2456 _reflns_number_gt 2187 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1996)' _computing_cell_refinement 'SMART (Bruker, 1996)' _computing_data_reduction 'SAINT (Bruker, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2001)' _computing_publication_material 'XSEED (Barbour, 2001)' _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. Only Fe and S atoms were refined anisotropically due to the poor quality of the crystal. C, N, and O atoms were refined isotropically. SIMU constraints were applied to some of the C, N, and O atoms. H atoms of the water molecules bonded to Fe atoms were located on the difference Fourier map and the O-H and H-H distances were fixed at 0.92 and 1.54 A, respectively. H atoms of the non-coordinated water molecules were not located. The atomic displacement parameters for disordered atoms appearing close to each other were set equal. ; _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^)+(0.0000P)^2^+187.7276P] 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 2456 _refine_ls_number_parameters 224 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0983 _refine_ls_wR_factor_ref 0.2039 _refine_ls_wR_factor_gt 0.1992 _refine_ls_goodness_of_fit_ref 1.246 _refine_ls_restrained_S_all 1.697 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.08669(10) 0.37051(17) -0.16238(13) 0.0220(5) Uani 1 1 d . . . Fe2 Fe 0.41489(9) 0.36845(13) 0.15745(11) 0.0033(4) Uani 1 1 d . . . Fe3 Fe 0.2529(3) 0.87251(10) -0.0019(4) 0.0102(3) Uani 1 1 d . . . S1 S 0.15354(15) 0.4467(2) 0.18512(18) 0.0075(7) Uani 1 1 d U . . S2 S 0.3371(2) 0.0484(4) 0.2993(2) 0.0327(11) Uani 1 1 d . . . S3 S 0.5000 0.0000 0.0000 0.051(2) Uani 1 2 d S . . S4 S 0.0000 0.0000 0.0000 0.0023(8) Uani 1 2 d SU . . O1 O 0.1657(5) 0.3355(7) 0.1445(6) 0.021(2) Uiso 1 1 d . . . O2 O 0.1443(4) 0.5428(7) 0.1327(5) 0.0144(18) Uiso 1 1 d . . . O3 O 0.0840(4) 0.4324(6) 0.2318(5) 0.005 Uiso 1 1 d U . . O4 O 0.2162(4) 0.4671(6) 0.2551(5) 0.0121(18) Uiso 1 1 d . . . O5 O 0.3605(4) -0.0216(6) 0.3828(5) 0.0071(17) Uiso 1 1 d . . . O6 O 0.2630(5) 0.0113(8) 0.2511(6) 0.028(2) Uiso 1 1 d . . . O7 O 0.3297(4) 0.1493(6) 0.3395(5) 0.0072(18) Uiso 1 1 d . . . O8 O 0.3972(5) 0.0483(9) 0.2445(7) 0.034(3) Uiso 1 1 d . . . O9 O 0.5424(10) 0.0922(15) 0.0600(12) 0.025(4) Uiso 0.50 1 d P . . O10 O 0.4434(8) 0.0325(12) -0.0766(9) 0.006(3) Uiso 0.50 1 d P . . O11 O 0.4550(11) -0.0399(17) 0.0710(13) 0.034(5) Uiso 0.50 1 d P . . O12 O 0.5536(12) -0.0702(18) -0.0188(14) 0.040(5) Uiso 0.50 1 d P . . O13 O 0.0535(10) 0.0458(16) 0.0579(12) 0.023(4) Uiso 0.50 1 d P . . O14 O -0.0324(8) 0.1084(12) -0.0426(10) 0.005(3) Uiso 0.50 1 d P . . O15 O -0.0636(8) -0.0601(12) 0.0260(9) 0.0022(15) Uiso 0.50 1 d PU . . O16 O 0.0318(7) -0.0661(12) -0.0712(9) 0.0018(15) Uiso 0.50 1 d PU . . O17 O 0.1569(5) 0.3443(6) -0.2651(6) 0.038(3) Uiso 1 1 d D . . O18 O 0.0495(4) 0.2110(6) -0.1619(5) 0.025 Uiso 1 1 d D . . O19 O 0.0119(3) 0.4220(6) -0.2636(4) 0.0082(17) Uiso 1 1 d D . . O20 O 0.0057(4) 0.4093(7) -0.0771(5) 0.025 Uiso 1 1 d D . . O21 O 0.4341(3) 0.2088(6) 0.1415(4) 0.0066(17) Uiso 1 1 d D . . O22 O 0.4965(4) 0.3985(6) 0.0687(5) 0.019(2) Uiso 1 1 d D . . O23 O 0.4985(4) 0.4023(6) 0.2601(5) 0.021(2) Uiso 1 1 d D . . O24 O 0.3447(4) 0.3400(5) 0.2547(4) 0.0016(16) Uiso 1 1 d D . . O25 O 0.3271(6) 0.8824(7) -0.0815(6) 0.048(3) Uiso 1 1 d D . . O26 O 0.3220(4) 0.9717(6) 0.0769(5) 0.025 Uiso 1 1 d D . . O27 O 0.1914(4) 0.9803(6) -0.0845(5) 0.021(2) Uiso 1 1 d D . . O28 O 0.1764(4) 0.8748(7) 0.1029(5) 0.025 Uiso 1 1 d D . . N1 N 0.1294(5) 0.5278(8) -0.1321(7) 0.015(2) Uiso 1 1 d . . . N2 N 0.1837(5) 0.3515(8) -0.0590(6) 0.009(2) Uiso 1 1 d . . . N3 N 0.3142(5) 0.3375(8) 0.0588(6) 0.0051(15) Uiso 1 1 d U . . N4 N 0.3732(5) 0.5410(7) 0.1255(6) 0.0013(16) Uiso 1 1 d U . . N5 N 0.3104(5) 0.7328(7) 0.0688(6) 0.0041(14) Uiso 1 1 d U . . N6 N 0.1881(6) 0.7281(9) -0.0545(7) 0.017(3) Uiso 1 1 d . . . C1 C 0.1921(2) 0.54089(18) -0.0629(2) 0.026(3) Uiso 1 1 d G . . C2 C 0.2215(2) 0.44291(18) -0.0324(3) 0.0076(18) Uiso 1 1 d GU . . C5 C 0.2839(2) 0.4400(2) 0.0306(3) 0.0044(14) Uiso 1 1 d GU . . C6 C 0.3168(2) 0.5350(2) 0.0632(3) 0.0020(14) Uiso 1 1 d GU . . C9 C 0.2873(2) 0.6330(2) 0.0327(3) 0.0037(14) Uiso 1 1 d GU . . C10 C 0.2250(2) 0.63592(18) -0.0304(3) 0.0086(18) Uiso 1 1 d GU . . C3 C 0.2112(2) 0.25563(18) -0.0299(3) 0.0113(19) Uiso 1 1 d GU . . H3 H 0.1867 0.1919 -0.0469 0.014 Uiso 1 1 calc R . . C4 C 0.2824(2) 0.2563(2) 0.0304(3) 0.0074(16) Uiso 1 1 d GU . . H4 H 0.3040 0.1906 0.0475 0.009 Uiso 1 1 calc R . . C7 C 0.3993(6) 0.6324(10) 0.1617(8) 0.016(3) Uiso 1 1 d . . . H7 H 0.4387 0.6328 0.2069 0.019 Uiso 1 1 calc R . . C8 C 0.3680(6) 0.7213(9) 0.1322(7) 0.0056(18) Uiso 1 1 d U . . H8 H 0.3879 0.7841 0.1581 0.007 Uiso 1 1 calc R . . C11 C 0.1268(7) 0.7298(11) -0.1136(8) 0.019(3) Uiso 1 1 d . . . H11 H 0.1028 0.7937 -0.1307 0.023 Uiso 1 1 calc R . . C12 C 0.0990(7) 0.6247(11) -0.1506(9) 0.019(3) Uiso 1 1 d . . . H12 H 0.0559 0.6264 -0.1908 0.023 Uiso 1 1 calc R . . H17A H 0.1603 0.2816 -0.3038 0.023 Uiso 1 1 d GD . . H17B H 0.1964 0.3904 -0.2494 0.023 Uiso 1 1 d GD . . H18A H 0.0774 0.1612 -0.1745 0.023 Uiso 1 1 d GD . . H18B H 0.0378 0.1721 -0.1139 0.023 Uiso 1 1 d GD . . H19A H 0.0210 0.4320 -0.3190 0.023 Uiso 1 1 d GD . . H19B H -0.0293 0.4504 -0.2511 0.023 Uiso 1 1 d GD . . H20A H -0.0486 0.4212 -0.0752 0.023 Uiso 1 1 d GD . . H20B H 0.0055 0.3680 -0.0281 0.023 Uiso 1 1 d GD . . H21A H 0.4721 0.1750 0.1253 0.023 Uiso 1 1 d GD . . H21B H 0.4354 0.1768 0.1850 0.023 Uiso 1 1 d GD . . H22A H 0.4878 0.3529 0.0163 0.023 Uiso 1 1 d GD . . H22B H 0.5491 0.4315 0.0816 0.023 Uiso 1 1 d GD . . H23A H 0.5292 0.4562 0.2531 0.023 Uiso 1 1 d GD . . H23B H 0.4801 0.4512 0.2981 0.023 Uiso 1 1 d GD . . H24A H 0.3180 0.3835 0.2827 0.023 Uiso 1 1 d GD . . H24B H 0.3395 0.2885 0.3037 0.023 Uiso 1 1 d GD . . H25A H 0.3212 0.8106 -0.1125 0.023 Uiso 1 1 d GD . . H25B H 0.2992 0.9040 -0.1304 0.023 Uiso 1 1 d GD . . H26A H 0.3434 1.0216 0.0553 0.023 Uiso 1 1 d GD . . H26B H 0.3122 0.9554 0.1327 0.023 Uiso 1 1 d GD . . H27A H 0.1507 0.9648 -0.1197 0.023 Uiso 1 1 d GD . . H27B H 0.1625 1.0220 -0.0641 0.023 Uiso 1 1 d GD . . H28A H 0.1216 0.8728 0.0915 0.023 Uiso 1 1 d GD . . H28B H 0.1722 0.8125 0.1478 0.023 Uiso 1 1 d GD . . O1S O 0.4724(2) 0.2738(3) -0.0666(4) 0.032(2) Uiso 1 1 d G . . O2S O 0.0294(2) 0.2824(3) 0.0684(3) 0.033(3) Uiso 1 1 d G . . O3S O 0.2714(5) -0.2093(3) 0.2778(5) 0.011(2) Uiso 0.33 1 d PG A -1 O4S O 0.3221(5) -0.2274(4) 0.3034(5) 0.011(2) Uiso 0.33 1 d PG B -2 O5S O 0.3787(5) -0.2309(4) 0.3261(5) 0.011(2) Uiso 0.34 1 d PG C -3 O6S O 0.2132(5) -0.2762(3) 0.2212(5) 0.011(2) Uiso 0.34 1 d PG D -4 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 0.0183(8) 0.0286(10) 0.0192(9) -0.0036(9) 0.0028(7) 0.0013(9) Fe2 0.0035(7) 0.0029(8) 0.0035(8) 0.0004(7) 0.0006(6) 0.0001(7) Fe3 0.0104(6) 0.0106(6) 0.0091(6) 0.003(3) 0.0000(5) -0.001(2) S1 0.0090(12) 0.0046(13) 0.0090(13) 0.0062(12) 0.0019(11) 0.0000(11) S2 0.0334(18) 0.054(2) 0.0135(17) 0.0136(17) 0.0147(14) 0.0313(17) S3 0.066(4) 0.028(3) 0.059(4) 0.009(3) 0.003(3) -0.013(3) S4 0.0019(13) 0.0027(14) 0.0023(14) -0.0019(13) 0.0001(12) -0.0002(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 Fe1 O19 2.031(6) . ? Fe1 O18 2.101(8) . ? Fe1 N1 2.137(10) . ? Fe1 O20 2.147(8) . ? Fe1 O17 2.177(10) . ? Fe1 N2 2.224(9) . ? Fe2 O21 2.041(7) . ? Fe2 O23 2.083(8) . ? Fe2 O24 2.114(7) . ? Fe2 O22 2.170(8) . ? Fe2 N3 2.249(9) . ? Fe2 N4 2.312(9) . ? Fe3 O25 1.936(12) . ? Fe3 O26 2.042(9) . ? Fe3 O27 2.072(9) . ? Fe3 N5 2.237(9) . ? Fe3 N6 2.242(11) . ? Fe3 O28 2.258(10) . ? S1 O2 1.442(9) . ? S1 O4 1.481(8) . ? S1 O3 1.537(8) . ? S1 O1 1.548(9) . ? S2 O7 1.416(9) . ? S2 O8 1.460(11) . ? S2 O6 1.517(10) . ? S2 O5 1.566(8) . ? S3 O12 1.36(2) 3_655 ? S3 O12 1.36(2) . ? S3 O10 1.513(14) 3_655 ? S3 O10 1.513(14) . ? S3 O11 1.53(2) . ? S3 O11 1.53(2) 3_655 ? S3 O9 1.606(18) . ? S3 O9 1.606(18) 3_655 ? S4 O13 1.355(18) . ? S4 O13 1.355(18) 3 ? S4 O15 1.471(15) . ? S4 O15 1.471(15) 3 ? S4 O16 1.541(14) . ? S4 O16 1.541(14) 3 ? S4 O14 1.581(15) . ? S4 O14 1.581(15) 3 ? O9 O10 1.59(2) 3_655 ? O9 O12 1.79(3) 3_655 ? O10 O12 1.54(3) 3_655 ? O10 O9 1.59(2) 3_655 ? O11 O12 1.59(3) 3_655 ? O12 O10 1.54(3) 3_655 ? O12 O11 1.59(3) 3_655 ? O12 O9 1.79(3) 3_655 ? O13 O15 1.34(2) 3 ? O13 O16 1.60(2) 3 ? O15 O13 1.34(2) 3 ? O15 O16 1.78(2) 3 ? O16 O13 1.60(2) 3 ? O16 O15 1.78(2) 3 ? O17 H17A 0.9896 . ? O17 H17B 0.9259 . ? O18 H18A 0.8381 . ? O18 H18B 0.9310 . ? O19 H19A 0.8978 . ? O19 H19B 0.8688 . ? O20 H20A 0.9971 . ? O20 H20B 0.9120 . ? O21 H21A 0.8696 . ? O21 H21B 0.7773 . ? O22 H22A 0.9832 . ? O22 H22B 1.0326 . ? O23 H23A 0.8883 . ? O23 H23B 0.9357 . ? O24 H24A 0.8764 . ? O24 H24B 1.0046 . ? O25 H25A 1.0142 . ? O25 H25B 0.8905 . ? O26 H26A 0.8256 . ? O26 H26B 0.9211 . ? O27 H27A 0.8775 . ? O27 H27B 0.8277 . ? O28 H28A 0.9840 . ? O28 H28B 1.0484 . ? N1 C12 1.343(17) . ? N1 C1 1.461(10) . ? N2 C3 1.348(10) . ? N2 C2 1.365(10) . ? N3 C4 1.217(10) . ? N3 C5 1.435(10) . ? N4 C6 1.309(9) . ? N4 C7 1.328(15) . ? N5 C8 1.341(13) . ? N5 C9 1.404(9) . ? N6 C11 1.339(16) . ? N6 C10 1.357(11) . ? C1 C2 1.3900 . ? C1 C10 1.3900 . ? C2 C5 1.3900 . ? C5 C6 1.3900 . ? C6 C9 1.3900 . ? C9 C10 1.3900 . ? C3 C4 1.4886 . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C7 C8 1.299(16) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C11 C12 1.491(19) . ? C11 H11 0.9300 . ? C12 H12 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 O19 Fe1 O18 96.9(3) . . ? O19 Fe1 N1 93.6(3) . . ? O18 Fe1 N1 167.3(4) . . ? O19 Fe1 O20 87.6(3) . . ? O18 Fe1 O20 88.1(3) . . ? N1 Fe1 O20 85.2(4) . . ? O19 Fe1 O17 83.4(3) . . ? O18 Fe1 O17 94.4(3) . . ? N1 Fe1 O17 93.9(4) . . ? O20 Fe1 O17 170.8(3) . . ? O19 Fe1 N2 165.6(3) . . ? O18 Fe1 N2 96.9(3) . . ? N1 Fe1 N2 73.3(4) . . ? O20 Fe1 N2 97.2(3) . . ? O17 Fe1 N2 91.3(3) . . ? O21 Fe2 O23 99.8(3) . . ? O21 Fe2 O24 92.8(3) . . ? O23 Fe2 O24 86.6(3) . . ? O21 Fe2 O22 87.3(3) . . ? O23 Fe2 O22 87.5(3) . . ? O24 Fe2 O22 174.0(3) . . ? O21 Fe2 N3 83.5(3) . . ? O23 Fe2 N3 172.5(3) . . ? O24 Fe2 N3 86.6(3) . . ? O22 Fe2 N3 99.4(3) . . ? O21 Fe2 N4 159.7(3) . . ? O23 Fe2 N4 99.1(3) . . ? O24 Fe2 N4 95.6(3) . . ? O22 Fe2 N4 86.3(3) . . ? N3 Fe2 N4 78.6(3) . . ? O25 Fe3 O26 85.1(4) . . ? O25 Fe3 O27 86.1(4) . . ? O26 Fe3 O27 102.1(3) . . ? O25 Fe3 N5 92.3(4) . . ? O26 Fe3 N5 88.4(4) . . ? O27 Fe3 N5 169.1(4) . . ? O25 Fe3 N6 101.3(4) . . ? O26 Fe3 N6 162.2(4) . . ? O27 Fe3 N6 94.9(4) . . ? N5 Fe3 N6 74.8(3) . . ? O25 Fe3 O28 172.5(4) . . ? O26 Fe3 O28 87.4(4) . . ? O27 Fe3 O28 95.7(3) . . ? N5 Fe3 O28 87.3(4) . . ? N6 Fe3 O28 85.9(4) . . ? O2 S1 O4 106.6(5) . . ? O2 S1 O3 108.3(5) . . ? O4 S1 O3 106.0(4) . . ? O2 S1 O1 122.1(5) . . ? O4 S1 O1 108.2(5) . . ? O3 S1 O1 104.6(5) . . ? O7 S2 O8 111.8(6) . . ? O7 S2 O6 111.0(5) . . ? O8 S2 O6 113.2(6) . . ? O7 S2 O5 99.6(5) . . ? O8 S2 O5 109.3(5) . . ? O6 S2 O5 111.0(5) . . ? O12 S3 O12 180(3) 3_655 . ? O12 S3 O10 115.7(10) 3_655 3_655 ? O12 S3 O10 64.3(10) . 3_655 ? O12 S3 O10 64.3(10) 3_655 . ? O12 S3 O10 115.7(10) . . ? O10 S3 O10 180.0(16) 3_655 . ? O12 S3 O11 66.3(12) 3_655 . ? O12 S3 O11 113.7(12) . . ? O10 S3 O11 74.0(9) 3_655 . ? O10 S3 O11 106.0(9) . . ? O12 S3 O11 113.7(12) 3_655 3_655 ? O12 S3 O11 66.3(12) . 3_655 ? O10 S3 O11 106.0(9) 3_655 3_655 ? O10 S3 O11 74.0(9) . 3_655 ? O11 S3 O11 180(2) . 3_655 ? O12 S3 O9 73.7(11) 3_655 . ? O12 S3 O9 106.3(11) . . ? O10 S3 O9 61.3(8) 3_655 . ? O10 S3 O9 118.7(8) . . ? O11 S3 O9 94.6(10) . . ? O11 S3 O9 85.4(10) 3_655 . ? O12 S3 O9 106.3(11) 3_655 3_655 ? O12 S3 O9 73.7(11) . 3_655 ? O10 S3 O9 118.7(8) 3_655 3_655 ? O10 S3 O9 61.3(8) . 3_655 ? O11 S3 O9 85.4(10) . 3_655 ? O11 S3 O9 94.6(10) 3_655 3_655 ? O9 S3 O9 180.0(19) . 3_655 ? O13 S4 O13 180(2) . 3 ? O13 S4 O15 123.6(10) . . ? O13 S4 O15 56.4(10) 3 . ? O13 S4 O15 56.4(10) . 3 ? O13 S4 O15 123.6(10) 3 3 ? O15 S4 O15 180.0(16) . 3 ? O13 S4 O16 113.1(9) . . ? O13 S4 O16 66.9(9) 3 . ? O15 S4 O16 107.4(8) . . ? O15 S4 O16 72.6(8) 3 . ? O13 S4 O16 66.9(9) . 3 ? O13 S4 O16 113.1(9) 3 3 ? O15 S4 O16 72.6(8) . 3 ? O15 S4 O16 107.4(8) 3 3 ? O16 S4 O16 180.0(14) . 3 ? O13 S4 O14 96.2(10) . . ? O13 S4 O14 83.8(10) 3 . ? O15 S4 O14 106.7(8) . . ? O15 S4 O14 73.3(8) 3 . ? O16 S4 O14 108.4(8) . . ? O16 S4 O14 71.6(8) 3 . ? O13 S4 O14 83.8(10) . 3 ? O13 S4 O14 96.2(10) 3 3 ? O15 S4 O14 73.3(8) . 3 ? O15 S4 O14 106.7(8) 3 3 ? O16 S4 O14 71.6(8) . 3 ? O16 S4 O14 108.4(8) 3 3 ? O14 S4 O14 180.0(15) . 3 ? O10 O9 S3 56.5(8) 3_655 . ? O10 O9 O12 92.0(12) 3_655 3_655 ? S3 O9 O12 47.0(8) . 3_655 ? S3 O10 O12 53.2(9) . 3_655 ? S3 O10 O9 62.3(8) . 3_655 ? O12 O10 O9 99.2(13) 3_655 3_655 ? S3 O11 O12 51.9(10) . 3_655 ? S3 O12 O10 62.6(11) . 3_655 ? S3 O12 O11 61.8(12) . 3_655 ? O10 O12 O11 102.1(16) 3_655 3_655 ? S3 O12 O9 59.4(10) . 3_655 ? O10 O12 O9 107.3(15) 3_655 3_655 ? O11 O12 O9 85.8(13) 3_655 3_655 ? O15 O13 S4 66.2(10) 3 . ? O15 O13 O16 110.8(14) 3 3 ? S4 O13 O16 62.1(9) . 3 ? O13 O15 S4 57.4(10) 3 . ? O13 O15 O16 100.5(13) 3 3 ? S4 O15 O16 55.5(7) . 3 ? S4 O16 O13 51.0(8) . 3 ? S4 O16 O15 51.9(6) . 3 ? O13 O16 O15 94.5(11) 3 3 ? Fe1 O17 H17A 130.1 . . ? Fe1 O17 H17B 102.9 . . ? H17A O17 H17B 122.7 . . ? Fe1 O18 H18A 119.8 . . ? Fe1 O18 H18B 127.0 . . ? H18A O18 H18B 90.2 . . ? Fe1 O19 H19A 125.8 . . ? Fe1 O19 H19B 117.7 . . ? H19A O19 H19B 115.0 . . ? Fe1 O20 H20A 143.5 . . ? Fe1 O20 H20B 117.0 . . ? H20A O20 H20B 87.3 . . ? Fe2 O21 H21A 131.3 . . ? Fe2 O21 H21B 112.5 . . ? H21A O21 H21B 93.7 . . ? Fe2 O22 H22A 111.6 . . ? Fe2 O22 H22B 129.4 . . ? H22A O22 H22B 115.6 . . ? Fe2 O23 H23A 117.7 . . ? Fe2 O23 H23B 108.9 . . ? H23A O23 H23B 82.1 . . ? Fe2 O24 H24A 131.7 . . ? Fe2 O24 H24B 139.7 . . ? H24A O24 H24B 85.1 . . ? Fe3 O25 H25A 101.7 . . ? Fe3 O25 H25B 101.0 . . ? H25A O25 H25B 81.8 . . ? Fe3 O26 H26A 120.0 . . ? Fe3 O26 H26B 104.0 . . ? H26A O26 H26B 134.3 . . ? Fe3 O27 H27A 125.3 . . ? Fe3 O27 H27B 119.4 . . ? H27A O27 H27B 81.5 . . ? Fe3 O28 H28A 124.6 . . ? Fe3 O28 H28B 124.4 . . ? H28A O28 H28B 86.7 . . ? C12 N1 C1 108.2(9) . . ? C12 N1 Fe1 130.7(8) . . ? C1 N1 Fe1 119.1(6) . . ? C3 N2 C2 119.5(7) . . ? C3 N2 Fe1 123.7(6) . . ? C2 N2 Fe1 116.3(6) . . ? C4 N3 C5 119.2(7) . . ? C4 N3 Fe2 133.5(6) . . ? C5 N3 Fe2 107.2(5) . . ? C6 N4 C7 123.9(9) . . ? C6 N4 Fe2 107.7(5) . . ? C7 N4 Fe2 128.4(7) . . ? C8 N5 C9 110.8(8) . . ? C8 N5 Fe3 134.9(8) . . ? C9 N5 Fe3 113.8(5) . . ? C11 N6 C10 122.3(10) . . ? C11 N6 Fe3 125.5(9) . . ? C10 N6 Fe3 111.5(6) . . ? C2 C1 C10 120.0 . . ? C2 C1 N1 112.0(4) . . ? C10 C1 N1 127.9(4) . . ? N2 C2 C1 118.5(4) . . ? N2 C2 C5 121.1(4) . . ? C1 C2 C5 120.0 . . ? C6 C5 C2 120.0 . . ? C6 C5 N3 121.4(4) . . ? C2 C5 N3 118.6(4) . . ? N4 C6 C5 124.8(4) . . ? N4 C6 C9 115.2(4) . . ? C5 C6 C9 120.0 . . ? C6 C9 C10 120.0 . . ? C6 C9 N5 124.4(4) . . ? C10 C9 N5 115.1(4) . . ? N6 C10 C9 122.7(5) . . ? N6 C10 C1 116.8(5) . . ? C9 C10 C1 120.0 . . ? N2 C3 C4 117.0(4) . . ? N2 C3 H3 121.5 . . ? C4 C3 H3 121.5 . . ? N3 C4 C3 124.0(5) . . ? N3 C4 H4 118.0 . . ? C3 C4 H4 118.0 . . ? C8 C7 N4 118.0(10) . . ? C8 C7 H7 121.0 . . ? N4 C7 H7 121.0 . . ? C7 C8 N5 127.5(11) . . ? C7 C8 H8 116.2 . . ? N5 C8 H8 116.2 . . ? N6 C11 C12 117.1(12) . . ? N6 C11 H11 121.5 . . ? C12 C11 H11 121.5 . . ? N1 C12 C11 126.9(11) . . ? N1 C12 H12 116.5 . . ? C11 C12 H12 116.5 . . ? _diffrn_measured_fraction_theta_max 0.498 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.498 _refine_diff_density_max 1.033 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.165 #=== END data_d:\mike\X-ray\ms038\try1 _database_code_depnum_ccdc_archive 'CCDC 264316' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12.82 H23.27 Fe2 N6 O15.82 S2' _chemical_formula_weight 690.36 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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 6.5269(8) _cell_length_b 29.457(4) _cell_length_c 12.5004(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.396(2) _cell_angle_gamma 90.00 _cell_volume 2402.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used 179 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1411 _exptl_absorpt_coefficient_mu 1.471 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 383(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 SMART 1000' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22199 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4913 _reflns_number_gt 4227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1996)' _computing_cell_refinement 'SMART (Bruker, 1996)' _computing_data_reduction 'SAINT (Bruker, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2001)' _computing_publication_material 'XSEED (Barbour, 2001)' _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. Hydrogen atoms of water molecules were located on the difference Fourier map and the O-H and H-H distances were fixed at 0.92 and 1.54 A, respectively. ; _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^)+(0.0336P)^2^+6.1640P] 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 0.00061(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4913 _refine_ls_number_parameters 400 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.47167(5) 0.691966(11) 0.00807(3) 0.01650(7) Uani 1 1 d . . . Fe2 Fe 0.23476(5) 0.554428(10) 0.46072(2) 0.01348(7) Uani 1 1 d . . . S1 S 0.25897(8) 0.458469(19) 0.59147(4) 0.01574(12) Uani 1 1 d . . . S2 S 0.04404(9) 0.69789(2) -0.30111(5) 0.01982(13) Uani 1 1 d . . . O1 O 0.1928(3) 0.72580(7) -0.02500(14) 0.0305(5) Uani 1 1 d D . . O2 O 0.5627(3) 0.70717(7) -0.14420(13) 0.0268(4) Uani 1 1 d D . . O3 O 0.5628(3) 0.75153(6) 0.08725(14) 0.0251(4) Uani 1 1 d D . . O4 O 0.7622(3) 0.66561(6) 0.05523(14) 0.0251(4) Uani 1 1 d D . . O5 O 0.2563(3) 0.60690(6) 0.57276(15) 0.0362(5) Uani 1 1 d D . . O6 O 0.4396(2) 0.44672(6) 0.52713(13) 0.0205(4) Uani 1 1 d . . . O7 O 0.0861(2) 0.43111(5) 0.54641(13) 0.0203(4) Uani 1 1 d . . . O8 O 0.2096(2) 0.50722(5) 0.57777(13) 0.0191(4) Uani 1 1 d . . . O9 O 0.2959(3) 0.44903(6) 0.70457(14) 0.0285(4) Uani 1 1 d . . . O10 O 0.2687(3) 0.70221(6) -0.29784(13) 0.0245(4) Uiso 1 1 d . A . O11A O -0.0146(3) 0.64923(7) -0.30301(16) 0.0291(5) Uiso 0.905(2) 1 d P A -1 O12A O -0.0428(3) 0.71855(6) -0.20356(15) 0.0219(4) Uiso 0.905(2) 1 d P A -1 O13A O -0.0403(3) 0.72091(6) -0.39614(15) 0.0243(4) Uiso 0.905(2) 1 d P A -1 O11B O -0.021(4) 0.6672(8) -0.3819(19) 0.045(6) Uiso 0.095(2) 1 d P A -2 O12B O -0.044(2) 0.6976(5) -0.2013(12) 0.011(3) Uiso 0.095(2) 1 d P A -2 O13B O -0.038(3) 0.7453(6) -0.3610(13) 0.018(4) Uiso 0.095(2) 1 d P A -2 N1 N 0.3700(3) 0.62214(7) -0.04381(14) 0.0170(4) Uani 1 1 d . . . N2 N 0.3569(3) 0.65999(7) 0.15499(15) 0.0202(5) Uani 1 1 d . . . N3 N 0.2741(3) 0.60616(6) 0.33324(14) 0.0153(4) Uani 1 1 d . . . N4 N 0.2143(3) 0.51512(6) 0.31063(15) 0.0161(4) Uani 1 1 d . . . N5 N 0.2101(3) 0.47517(6) 0.10564(15) 0.0180(4) Uani 1 1 d . . . N6 N 0.2841(3) 0.52889(7) -0.07268(15) 0.0185(4) Uani 1 1 d . . . C1 C 0.3224(3) 0.55653(8) -0.15408(18) 0.0205(5) Uani 1 1 d . . . H1 H 0.3196 0.5447 -0.2231 0.025 Uiso 1 1 calc R . . C2 C 0.3667(3) 0.60272(8) -0.14005(18) 0.0192(5) Uani 1 1 d . . . H2 H 0.3946 0.6203 -0.1997 0.023 Uiso 1 1 calc R . . C3 C 0.3481(4) 0.67760(8) 0.25282(19) 0.0253(6) Uani 1 1 d . . . H3 H 0.3700 0.7085 0.2625 0.030 Uiso 1 1 calc R . . C4 C 0.3063(4) 0.65021(8) 0.34172(19) 0.0231(6) Uani 1 1 d . . . H4 H 0.3012 0.6636 0.4089 0.028 Uiso 1 1 calc R . . C5 C 0.1790(3) 0.47098(8) 0.29637(19) 0.0193(5) Uani 1 1 d . . . H5 H 0.1552 0.4527 0.3555 0.023 Uiso 1 1 calc R . . C6 C 0.1770(3) 0.45146(8) 0.19380(19) 0.0192(5) Uani 1 1 d . . . H6 H 0.1514 0.4205 0.1874 0.023 Uiso 1 1 calc R . . C7 C 0.2858(3) 0.54815(8) 0.02527(17) 0.0161(5) Uani 1 1 d . . . C8 C 0.3256(3) 0.59458(8) 0.03963(17) 0.0153(5) Uani 1 1 d . . . C9 C 0.3205(3) 0.61483(8) 0.14529(17) 0.0161(5) Uani 1 1 d . . . C10 C 0.2798(3) 0.58825(7) 0.23347(17) 0.0148(5) Uani 1 1 d . . . C11 C 0.2464(3) 0.53974(7) 0.22064(17) 0.0149(5) Uani 1 1 d . . . C12 C 0.2460(3) 0.52005(8) 0.11910(18) 0.0160(5) Uani 1 1 d . . . H1A H 0.124(3) 0.7412(6) 0.0264(11) 0.019 Uiso 1 1 d D . . H2A H 0.4630(18) 0.7062(9) -0.1961(14) 0.019 Uiso 1 1 d D . . H3A H 0.6930(16) 0.7615(7) 0.089(2) 0.019 Uiso 1 1 d D . . H4A H 0.811(3) 0.6773(5) 0.1199(12) 0.019 Uiso 1 1 d D . . H5A H 0.3846(16) 0.6168(8) 0.5821(19) 0.019 Uiso 1 1 d D . . H1B H 0.113(3) 0.7185(7) -0.0830(11) 0.019 Uiso 1 1 d D . . H2B H 0.6912(17) 0.7078(9) -0.1706(17) 0.019 Uiso 1 1 d D . . H3B H 0.469(2) 0.7732(6) 0.1077(19) 0.019 Uiso 1 1 d D . . H4B H 0.782(4) 0.6353(4) 0.0507(16) 0.019 Uiso 1 1 d D . . H5B H 0.161(2) 0.6228(7) 0.6103(17) 0.019 Uiso 1 1 d D . . O1S O 0.8253(3) 0.57692(5) 0.09308(13) 0.0221(4) Uani 1 1 d D . . H1SA H 0.803(4) 0.5530(5) 0.0454(11) 0.019 Uiso 1 1 d D . . H1SB H 0.787(4) 0.5677(7) 0.1603(9) 0.019 Uiso 1 1 d D . . O2S O 0.1132(4) 0.31025(8) 0.7437(2) 0.0451(8) Uani 0.818(4) 1 d P B -3 H2S H 0.0914 0.2829 0.7409 0.054 Uiso 0.818(4) 1 calc PR B -3 C2S C 0.1804(7) 0.32532(16) 0.6444(5) 0.0733(18) Uani 0.818(4) 1 d P B -3 H2S1 H 0.2356 0.3554 0.6518 0.110 Uiso 0.818(4) 1 calc PR B -3 H2S2 H 0.0671 0.3257 0.5940 0.110 Uiso 0.818(4) 1 calc PR B -3 H2S3 H 0.2845 0.3052 0.6194 0.110 Uiso 0.818(4) 1 calc PR B -3 O3S O 0.3738(5) 0.36598(12) 0.4040(4) 0.1181(14) Uani 0.818(4) 1 d PD B -3 O4S O 0.2868(18) 0.3487(5) 0.5247(13) 0.1181(14) Uani 0.18 1 d PD B -4 H3S H 0.360(10) 0.3905(6) 0.3601(15) 0.142 Uiso 0.818(4) 1 d PD B -3 H4S H 0.293(5) 0.3277(10) 0.470(2) 0.142 Uiso 0.182(4) 1 d PD B -4 H3T H 0.342(8) 0.3702(14) 0.4746(12) 0.142 Uiso 0.818(4) 1 d PD B -3 H4T H 0.164(3) 0.348(2) 0.560(3) 0.142 Uiso 0.182(4) 1 d PD B -4 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 0.01626(15) 0.01866(15) 0.01456(15) 0.00308(12) -0.00022(12) -0.00053(13) Fe2 0.01181(14) 0.01505(14) 0.01358(14) 0.00048(12) 0.00029(11) 0.00027(12) S1 0.0109(2) 0.0198(3) 0.0166(2) 0.0047(2) 0.0011(2) 0.0013(2) S2 0.0163(3) 0.0260(3) 0.0171(3) 0.0001(2) -0.0005(2) 0.0022(2) O1 0.0227(9) 0.0469(11) 0.0217(9) -0.0087(8) -0.0040(7) 0.0132(8) O2 0.0164(8) 0.0460(11) 0.0181(8) 0.0064(8) 0.0013(7) -0.0027(8) O3 0.0173(8) 0.0241(8) 0.0340(9) -0.0064(7) 0.0008(7) 0.0006(7) O4 0.0222(8) 0.0206(8) 0.0319(9) 0.0004(7) -0.0081(7) 0.0009(7) O5 0.0452(11) 0.0319(10) 0.0320(10) -0.0150(8) 0.0096(9) -0.0063(9) O6 0.0112(7) 0.0290(9) 0.0216(8) 0.0015(7) 0.0016(6) 0.0015(7) O7 0.0136(7) 0.0177(7) 0.0296(9) 0.0017(7) 0.0016(7) -0.0005(6) O8 0.0190(8) 0.0176(8) 0.0209(8) 0.0027(6) 0.0037(7) -0.0006(6) O9 0.0241(9) 0.0419(10) 0.0195(8) 0.0107(8) 0.0004(7) 0.0055(8) O1S 0.0296(9) 0.0181(8) 0.0185(8) -0.0007(6) 0.0027(7) 0.0002(7) N1 0.0133(8) 0.0233(9) 0.0145(9) 0.0012(8) -0.0005(7) 0.0001(8) N2 0.0235(10) 0.0187(9) 0.0183(9) -0.0009(8) 0.0001(8) -0.0027(8) N3 0.0130(8) 0.0170(9) 0.0160(9) -0.0011(7) 0.0006(7) 0.0004(7) N4 0.0110(8) 0.0204(9) 0.0170(9) 0.0000(7) 0.0010(7) -0.0005(7) N5 0.0145(9) 0.0183(9) 0.0211(9) -0.0018(8) 0.0009(8) -0.0010(7) N6 0.0154(9) 0.0226(10) 0.0173(9) -0.0035(8) -0.0005(7) 0.0001(8) C1 0.0163(10) 0.0294(12) 0.0157(11) -0.0021(9) 0.0004(9) -0.0003(10) C2 0.0174(10) 0.0243(11) 0.0159(10) 0.0020(9) -0.0009(9) 0.0002(9) C3 0.0383(14) 0.0174(11) 0.0200(11) -0.0018(9) 0.0003(10) -0.0031(10) C4 0.0332(13) 0.0182(11) 0.0178(11) -0.0020(9) 0.0005(10) -0.0001(10) C5 0.0193(11) 0.0187(11) 0.0200(11) 0.0026(9) 0.0029(9) -0.0019(9) C6 0.0172(10) 0.0160(10) 0.0246(12) -0.0003(9) 0.0025(9) -0.0019(9) C7 0.0106(9) 0.0205(11) 0.0170(10) -0.0013(9) -0.0012(8) 0.0003(8) C8 0.0111(9) 0.0195(10) 0.0151(10) 0.0010(8) -0.0019(8) -0.0001(8) C9 0.0109(9) 0.0199(11) 0.0175(10) 0.0006(9) -0.0009(8) -0.0005(8) C10 0.0095(9) 0.0179(10) 0.0169(10) -0.0008(8) 0.0000(8) -0.0001(8) C11 0.0099(9) 0.0173(10) 0.0175(10) 0.0007(9) -0.0007(8) -0.0010(8) C12 0.0100(9) 0.0195(11) 0.0184(10) -0.0010(9) -0.0005(8) 0.0017(8) O2S 0.0657(17) 0.0261(12) 0.0423(14) -0.0043(11) -0.0241(13) 0.0034(12) C2S 0.040(2) 0.046(3) 0.134(5) -0.011(3) -0.006(3) 0.003(2) O3S 0.0292(16) 0.100(2) 0.224(4) -0.125(2) -0.0178(19) 0.0112(15) O4S 0.0292(16) 0.100(2) 0.224(4) -0.125(2) -0.0178(19) 0.0112(15) _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 O2 2.0572(17) . ? Fe1 O3 2.0935(17) . ? Fe1 O1 2.1072(18) . ? Fe1 O4 2.1192(17) . ? Fe1 N2 2.211(2) . ? Fe1 N1 2.2517(19) . ? Fe2 O8 2.0281(16) . ? Fe2 O5 2.0883(19) . ? Fe2 O6 2.1273(16) 3_666 ? Fe2 O7 2.1370(16) 3_566 ? Fe2 N4 2.2060(19) . ? Fe2 N3 2.2243(19) . ? S1 O9 1.4552(18) . ? S1 O8 1.4809(16) . ? S1 O6 1.4843(16) . ? S1 O7 1.4861(17) . ? S2 O12B 1.386(15) . ? S2 O11B 1.41(2) . ? S2 O13A 1.464(2) . ? S2 O10 1.4717(18) . ? S2 O11A 1.484(2) . ? S2 O12A 1.4873(19) . ? S2 O13B 1.665(17) . ? O6 Fe2 2.1273(15) 3_666 ? O7 Fe2 2.1370(16) 3_566 ? N1 C2 1.332(3) . ? N1 C8 1.359(3) . ? N2 C3 1.331(3) . ? N2 C9 1.356(3) . ? N3 C4 1.318(3) . ? N3 C10 1.355(3) . ? N4 C5 1.332(3) . ? N4 C11 1.359(3) . ? N5 C6 1.327(3) . ? N5 C12 1.353(3) . ? N6 C1 1.332(3) . ? N6 C7 1.349(3) . ? C1 C2 1.401(3) . ? C3 C4 1.405(3) . ? C5 C6 1.405(3) . ? C7 C8 1.403(3) . ? C7 C12 1.464(3) . ? C8 C9 1.450(3) . ? C9 C10 1.383(3) . ? C10 C11 1.454(3) . ? C11 C12 1.395(3) . ? O2S C2S 1.398(6) . ? 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 O2 Fe1 O3 99.78(7) . . ? O2 Fe1 O1 89.04(7) . . ? O3 Fe1 O1 86.01(7) . . ? O2 Fe1 O4 93.46(7) . . ? O3 Fe1 O4 86.19(7) . . ? O1 Fe1 O4 172.11(7) . . ? O2 Fe1 N2 166.58(7) . . ? O3 Fe1 N2 93.58(7) . . ? O1 Fe1 N2 93.21(7) . . ? O4 Fe1 N2 86.09(7) . . ? O2 Fe1 N1 91.27(7) . . ? O3 Fe1 N1 168.52(7) . . ? O1 Fe1 N1 97.38(7) . . ? O4 Fe1 N1 90.05(7) . . ? N2 Fe1 N1 75.33(7) . . ? O8 Fe2 O5 91.66(7) . . ? O8 Fe2 O6 92.06(6) . 3_666 ? O5 Fe2 O6 85.01(7) . 3_666 ? O8 Fe2 O7 94.02(6) . 3_566 ? O5 Fe2 O7 86.01(7) . 3_566 ? O6 Fe2 O7 169.29(6) 3_666 3_566 ? O8 Fe2 N4 104.44(7) . . ? O5 Fe2 N4 163.86(7) . . ? O6 Fe2 N4 95.28(7) 3_666 . ? O7 Fe2 N4 91.73(7) 3_566 . ? O8 Fe2 N3 178.01(7) . . ? O5 Fe2 N3 88.07(7) . . ? O6 Fe2 N3 85.95(6) 3_666 . ? O7 Fe2 N3 87.92(6) 3_566 . ? N4 Fe2 N3 75.87(7) . . ? O9 S1 O8 109.15(10) . . ? O9 S1 O6 111.54(10) . . ? O8 S1 O6 109.70(9) . . ? O9 S1 O7 111.76(10) . . ? O8 S1 O7 108.72(9) . . ? O6 S1 O7 105.89(9) . . ? O12B S2 O11B 121.1(12) . . ? O12B S2 O13A 125.3(6) . . ? O11B S2 O13A 67.4(10) . . ? O12B S2 O10 114.2(6) . . ? O11B S2 O10 110.9(10) . . ? O13A S2 O10 109.73(11) . . ? O12B S2 O11A 84.0(7) . . ? O11B S2 O11A 45.4(10) . . ? O13A S2 O11A 110.05(11) . . ? O10 S2 O11A 109.90(11) . . ? O12B S2 O12A 24.5(7) . . ? O11B S2 O12A 137.2(10) . . ? O13A S2 O12A 109.42(11) . . ? O10 S2 O12A 109.95(10) . . ? O11A S2 O12A 107.77(11) . . ? O12B S2 O13B 106.0(9) . . ? O11B S2 O13B 97.3(11) . . ? O13A S2 O13B 30.3(6) . . ? O10 S2 O13B 104.3(6) . . ? O11A S2 O13B 136.3(6) . . ? O12A S2 O13B 84.4(6) . . ? S1 O6 Fe2 140.39(10) . 3_666 ? S1 O7 Fe2 129.93(10) . 3_566 ? S1 O8 Fe2 136.65(10) . . ? C2 N1 C8 115.9(2) . . ? C2 N1 Fe1 130.61(16) . . ? C8 N1 Fe1 113.05(14) . . ? C3 N2 C9 116.9(2) . . ? C3 N2 Fe1 128.34(16) . . ? C9 N2 Fe1 113.94(15) . . ? C4 N3 C10 116.69(19) . . ? C4 N3 Fe2 129.62(15) . . ? C10 N3 Fe2 113.50(14) . . ? C5 N4 C11 116.09(19) . . ? C5 N4 Fe2 129.27(15) . . ? C11 N4 Fe2 114.62(14) . . ? C6 N5 C12 116.3(2) . . ? C1 N6 C7 116.0(2) . . ? N6 C1 C2 122.7(2) . . ? N1 C2 C1 121.9(2) . . ? N2 C3 C4 121.1(2) . . ? N3 C4 C3 122.3(2) . . ? N4 C5 C6 121.3(2) . . ? N5 C6 C5 123.0(2) . . ? N6 C7 C8 121.6(2) . . ? N6 C7 C12 119.5(2) . . ? C8 C7 C12 118.98(19) . . ? N1 C8 C7 121.8(2) . . ? N1 C8 C9 117.6(2) . . ? C7 C8 C9 120.6(2) . . ? N2 C9 C10 121.4(2) . . ? N2 C9 C8 118.5(2) . . ? C10 C9 C8 120.1(2) . . ? N3 C10 C9 121.5(2) . . ? N3 C10 C11 118.47(19) . . ? C9 C10 C11 120.0(2) . . ? N4 C11 C12 122.3(2) . . ? N4 C11 C10 117.31(19) . . ? C12 C11 C10 120.4(2) . . ? N5 C12 C11 121.1(2) . . ? N5 C12 C7 119.1(2) . . ? C11 C12 C7 119.8(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.408 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.087 #=== END data_d:\mike\X-ray\ms035\msii48 _database_code_depnum_ccdc_archive 'CCDC 264317' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 Fe2 N6 O16 S2' _chemical_formula_weight 682.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 6.4492(5) _cell_length_b 25.388(2) _cell_length_c 14.1833(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.952(5) _cell_angle_gamma 90.00 _cell_volume 2322.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 12.564 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker GADDS' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18627 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 59.10 _reflns_number_total 3285 _reflns_number_gt 2518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1996)' _computing_cell_refinement 'SMART (Bruker, 1996)' _computing_data_reduction 'SAINT (Bruker, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2001)' _computing_publication_material 'XSEED (Barbour, 2001)' _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. Hydrogen atoms of water molecules were located on the difference Fourier map and the O-H and H-H distances were fixed at 0.92 and 1.54 A, respectively. ; _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^)+(0.0631P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3285 _refine_ls_number_parameters 376 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.04906(8) 0.32414(2) 0.88263(4) 0.01068(15) Uani 1 1 d . . . Fe2 Fe 0.25412(8) 0.54698(2) 0.58968(4) 0.00970(14) Uani 1 1 d . . . S1 S -0.49140(14) 0.27349(3) 0.59910(6) 0.0113(2) Uani 1 1 d . . . S2 S -0.25437(13) 0.52086(3) 0.61088(6) 0.0104(2) Uani 1 1 d . . . O1 O -0.7138(4) 0.28169(10) 0.57931(17) 0.0163(7) Uani 1 1 d . . . O2 O -0.4110(4) 0.23370(9) 0.53284(17) 0.0142(6) Uani 1 1 d . . . O3 O -0.3770(4) 0.32318(10) 0.58755(18) 0.0202(7) Uani 1 1 d . . . O4 O -0.4636(4) 0.25435(10) 0.69745(17) 0.0159(7) Uani 1 1 d . . . O5 O -0.3060(4) 0.49892(9) 0.70212(16) 0.0136(6) Uani 1 1 d . . . O6 O -0.0683(4) 0.55416(9) 0.61878(18) 0.0159(7) Uani 1 1 d . . . O7 O -0.2149(4) 0.47725(9) 0.54492(17) 0.0166(7) Uani 1 1 d . . . O8 O -0.4234(4) 0.55538(9) 0.57344(17) 0.0154(7) Uani 1 1 d . . . O9 O 0.2222(4) 0.62920(9) 0.56659(17) 0.0149(6) Uani 1 1 d D . . O10 O -0.0083(4) 0.28384(10) 1.00466(18) 0.0188(7) Uani 1 1 d D . . O11 O -0.2442(4) 0.36097(10) 0.89204(17) 0.0162(7) Uani 1 1 d D . . O12 O -0.0675(4) 0.27293(9) 0.77972(18) 0.0172(7) Uani 1 1 d D . . O13 O 0.3437(4) 0.28811(10) 0.87041(17) 0.0167(7) Uani 1 1 d D . . O1S O -0.3940(4) 0.39502(9) 0.73115(17) 0.0167(7) Uani 1 1 d D . . O2S O 0.1794(4) 0.31047(9) 1.23660(18) 0.0197(7) Uani 1 1 d D . . O3S O -0.7981(4) 0.34240(10) 0.42288(18) 0.0214(7) Uani 1 1 d D . . N1 N 0.1687(4) 0.39329(11) 0.9680(2) 0.0094(7) Uani 1 1 d . . . N2 N 0.1316(4) 0.38453(11) 0.7781(2) 0.0095(8) Uani 1 1 d . . . N3 N 0.2221(4) 0.47073(11) 0.6624(2) 0.0079(7) Uani 1 1 d . . . N4 N 0.2946(4) 0.56651(11) 0.7409(2) 0.0107(8) Uani 1 1 d . . . N5 N 0.3107(5) 0.57988(12) 0.9366(2) 0.0154(8) Uani 1 1 d . . . N6 N 0.2510(4) 0.49123(12) 1.0528(2) 0.0124(8) Uani 1 1 d . . . C1 C 0.2175(5) 0.44812(14) 1.1027(3) 0.0137(10) Uani 1 1 d . . . H1 H 0.2209 0.4504 1.1681 0.016 Uiso 1 1 calc R . . C2 C 0.1770(5) 0.39906(14) 1.0608(2) 0.0113(9) Uani 1 1 d . . . H2 H 0.1556 0.3699 1.0991 0.014 Uiso 1 1 calc R . . C3 C 0.1211(5) 0.38152(14) 0.6851(3) 0.0120(9) Uani 1 1 d . . . H3 H 0.0799 0.3500 0.6573 0.014 Uiso 1 1 calc R . . C4 C 0.1698(5) 0.42435(14) 0.6269(3) 0.0108(9) Uani 1 1 d . . . H4 H 0.1653 0.4200 0.5618 0.013 Uiso 1 1 calc R . . C5 C 0.3276(5) 0.61327(14) 0.7798(3) 0.0125(10) Uani 1 1 d . . . H5 H 0.3463 0.6425 0.7414 0.015 Uiso 1 1 calc R . . C6 C 0.3346(5) 0.61918(14) 0.8774(3) 0.0123(9) Uani 1 1 d . . . H6 H 0.3575 0.6527 0.9020 0.015 Uiso 1 1 calc R . . C7 C 0.2463(5) 0.48589(14) 0.9581(3) 0.0111(9) Uani 1 1 d U . . C8 C 0.2030(5) 0.43741(13) 0.9160(2) 0.0092(8) Uiso 1 1 d U . . C9 C 0.1889(5) 0.43182(14) 0.8149(3) 0.0099(9) Uani 1 1 d . . . C10 C 0.2282(5) 0.47485(13) 0.7581(2) 0.0084(8) Uiso 1 1 d U . . C11 C 0.2703(5) 0.52563(13) 0.7996(2) 0.0096(8) Uiso 1 1 d U . . C12 C 0.2757(5) 0.53184(14) 0.8975(3) 0.0118(9) Uani 1 1 d . . . H9A H 0.286(3) 0.6466(10) 0.5173(13) 0.014 Uiso 1 1 d D . . H10A H 0.082(2) 0.2613(9) 1.033(2) 0.014 Uiso 1 1 d D . . H11A H -0.284(5) 0.3745(10) 0.8356(9) 0.014 Uiso 1 1 d D . . H12A H 0.019(2) 0.2463(8) 0.763(2) 0.014 Uiso 1 1 d D . . H13A H 0.403(4) 0.2828(13) 0.8129(8) 0.014 Uiso 1 1 d D . . H9B H 0.088(2) 0.6399(12) 0.5748(18) 0.014 Uiso 1 1 d D . . H10B H -0.1442(18) 0.2789(11) 1.019(2) 0.014 Uiso 1 1 d D . . H11B H -0.245(5) 0.3845(8) 0.9414(10) 0.014 Uiso 1 1 d D . . H12B H -0.198(2) 0.2699(11) 0.755(2) 0.014 Uiso 1 1 d D . . H13B H 0.428(3) 0.2833(13) 0.9205(10) 0.014 Uiso 1 1 d D . . H1S H -0.380(5) 0.3727(6) 0.6820(13) 0.014 Uiso 1 1 d D . . H2S H -0.355(5) 0.4288(5) 0.7217(19) 0.014 Uiso 1 1 d D . . H3S H 0.285(3) 0.2877(8) 1.2206(16) 0.014 Uiso 1 1 d D . . H4S H 0.201(4) 0.3241(9) 1.2960(11) 0.014 Uiso 1 1 d D . . H5S H -0.733(4) 0.3736(5) 0.4204(18) 0.014 Uiso 1 1 d D . . H6S H -0.762(5) 0.3226(7) 0.4751(13) 0.014 Uiso 1 1 d 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 Fe1 0.0087(3) 0.0111(3) 0.0124(3) 0.0009(2) 0.0016(3) -0.0011(2) Fe2 0.0073(3) 0.0112(3) 0.0107(3) -0.0006(2) 0.0019(3) 0.0003(2) S1 0.0104(4) 0.0124(4) 0.0112(5) -0.0005(4) 0.0011(4) -0.0008(4) S2 0.0066(4) 0.0134(4) 0.0113(5) -0.0005(4) -0.0004(4) 0.0000(4) O1 0.0098(13) 0.0234(14) 0.0156(14) -0.0035(11) -0.0011(12) 0.0026(11) O2 0.0145(13) 0.0136(13) 0.0144(13) -0.0064(11) 0.0012(12) 0.0019(11) O3 0.0264(15) 0.0177(14) 0.0167(14) -0.0049(12) 0.0025(13) -0.0080(12) O4 0.0130(13) 0.0229(14) 0.0118(14) 0.0021(11) 0.0014(12) -0.0030(12) O5 0.0173(14) 0.0139(12) 0.0095(13) 0.0009(11) 0.0019(12) 0.0018(11) O6 0.0043(12) 0.0139(13) 0.0295(15) -0.0008(12) -0.0013(12) -0.0004(11) O7 0.0216(14) 0.0168(13) 0.0115(13) -0.0035(11) 0.0002(12) 0.0052(12) O8 0.0110(13) 0.0169(13) 0.0182(14) 0.0023(11) 0.0004(12) 0.0024(11) O9 0.0136(13) 0.0132(13) 0.0182(14) 0.0038(11) 0.0045(12) 0.0045(11) O10 0.0096(13) 0.0245(14) 0.0224(15) 0.0095(12) 0.0025(12) 0.0029(12) O11 0.0176(14) 0.0194(13) 0.0116(13) -0.0016(11) -0.0005(12) -0.0002(12) O12 0.0101(13) 0.0172(13) 0.0242(15) -0.0070(12) -0.0033(13) 0.0003(11) O13 0.0130(13) 0.0237(14) 0.0136(13) -0.0022(12) 0.0034(12) 0.0026(12) O1S 0.0180(14) 0.0139(13) 0.0183(14) -0.0028(12) 0.0009(12) -0.0014(12) O2S 0.0252(15) 0.0175(14) 0.0167(14) -0.0007(12) 0.0032(13) 0.0033(12) O3S 0.0296(16) 0.0121(13) 0.0227(15) 0.0041(12) 0.0001(14) 0.0022(12) N1 0.0043(15) 0.0145(15) 0.0093(16) 0.0012(13) 0.0013(14) 0.0022(13) N2 0.0060(15) 0.0103(15) 0.0121(16) -0.0023(13) 0.0011(14) -0.0001(13) N3 0.0030(14) 0.0133(15) 0.0074(15) -0.0023(13) 0.0030(13) 0.0011(13) N4 0.0073(15) 0.0123(15) 0.0126(16) -0.0009(13) 0.0005(14) 0.0010(13) N5 0.0137(17) 0.0153(16) 0.0174(17) -0.0016(14) 0.0033(15) -0.0011(14) N6 0.0065(16) 0.0213(17) 0.0094(16) -0.0012(14) 0.0038(14) -0.0009(14) C1 0.0108(19) 0.019(2) 0.012(2) 0.0028(17) 0.0069(17) 0.0006(17) C2 0.0083(18) 0.0152(19) 0.0105(19) 0.0045(16) 0.0015(17) -0.0001(16) C3 0.0105(19) 0.0129(19) 0.013(2) -0.0047(16) 0.0020(17) 0.0014(16) C4 0.0103(19) 0.0169(19) 0.0051(18) -0.0027(16) -0.0010(17) 0.0038(16) C5 0.0105(19) 0.0090(18) 0.018(2) 0.0025(16) 0.0009(18) 0.0006(16) C6 0.0086(18) 0.0136(19) 0.015(2) -0.0049(16) -0.0017(17) 0.0013(16) C7 0.0062(19) 0.0150(19) 0.012(2) 0.0005(16) 0.0020(17) 0.0025(16) C9 0.0016(17) 0.0150(19) 0.0129(19) -0.0005(16) -0.0017(17) 0.0014(16) C12 0.0021(18) 0.019(2) 0.015(2) 0.0008(17) -0.0006(17) 0.0016(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 O10 2.050(3) . ? Fe1 O12 2.086(2) . ? Fe1 O11 2.116(3) . ? Fe1 O13 2.119(3) . ? Fe1 N2 2.205(3) . ? Fe1 N1 2.261(3) . ? Fe2 O7 2.018(2) 3_566 ? Fe2 O8 2.107(2) 1_655 ? Fe2 O9 2.122(2) . ? Fe2 O6 2.134(2) . ? Fe2 N3 2.205(3) . ? Fe2 N4 2.212(3) . ? S1 O1 1.472(3) . ? S1 O3 1.472(3) . ? S1 O2 1.479(2) . ? S1 O4 1.485(3) . ? S2 O5 1.453(2) . ? S2 O6 1.471(2) . ? S2 O7 1.474(3) . ? S2 O8 1.490(3) . ? O7 Fe2 2.018(2) 3_566 ? O8 Fe2 2.107(2) 1_455 ? N1 C2 1.325(4) . ? N1 C8 1.361(4) . ? N2 C3 1.321(5) . ? N2 C9 1.358(4) . ? N3 C4 1.322(4) . ? N3 C10 1.361(4) . ? N4 C5 1.325(4) . ? N4 C11 1.342(4) . ? N5 C6 1.315(5) . ? N5 C12 1.357(5) . ? N6 C1 1.323(5) . ? N6 C7 1.350(5) . ? C1 C2 1.402(5) . ? C3 C4 1.404(5) . ? C5 C6 1.392(5) . ? C7 C8 1.394(5) . ? C7 C12 1.463(5) . ? C8 C9 1.442(5) . ? C9 C10 1.383(5) . ? C10 C11 1.441(5) . ? C11 C12 1.398(5) . ? 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 O10 Fe1 O12 102.23(10) . . ? O10 Fe1 O11 89.62(10) . . ? O12 Fe1 O11 90.43(10) . . ? O10 Fe1 O13 91.62(10) . . ? O12 Fe1 O13 89.25(10) . . ? O11 Fe1 O13 178.76(10) . . ? O10 Fe1 N2 164.64(11) . . ? O12 Fe1 N2 92.93(10) . . ? O11 Fe1 N2 87.77(10) . . ? O13 Fe1 N2 91.05(10) . . ? O10 Fe1 N1 90.01(10) . . ? O12 Fe1 N1 167.06(10) . . ? O11 Fe1 N1 85.43(10) . . ? O13 Fe1 N1 94.62(10) . . ? N2 Fe1 N1 74.69(10) . . ? O7 Fe2 O8 92.06(10) 3_566 1_655 ? O7 Fe2 O9 98.26(10) 3_566 . ? O8 Fe2 O9 88.69(9) 1_655 . ? O7 Fe2 O6 95.84(10) 3_566 . ? O8 Fe2 O6 168.23(10) 1_655 . ? O9 Fe2 O6 81.57(9) . . ? O7 Fe2 N3 99.43(10) 3_566 . ? O8 Fe2 N3 103.90(10) 1_655 . ? O9 Fe2 N3 157.83(10) . . ? O6 Fe2 N3 83.42(10) . . ? O7 Fe2 N4 175.16(10) 3_566 . ? O8 Fe2 N4 88.99(10) 1_655 . ? O9 Fe2 N4 86.49(10) . . ? O6 Fe2 N4 83.87(10) . . ? N3 Fe2 N4 75.74(10) . . ? O1 S1 O3 110.26(15) . . ? O1 S1 O2 109.04(14) . . ? O3 S1 O2 109.45(15) . . ? O1 S1 O4 109.12(15) . . ? O3 S1 O4 109.38(15) . . ? O2 S1 O4 109.58(14) . . ? O5 S2 O6 110.57(15) . . ? O5 S2 O7 108.78(14) . . ? O6 S2 O7 109.31(15) . . ? O5 S2 O8 111.47(14) . . ? O6 S2 O8 106.27(14) . . ? O7 S2 O8 110.41(15) . . ? S2 O6 Fe2 137.08(15) . . ? S2 O7 Fe2 144.01(16) . 3_566 ? S2 O8 Fe2 128.26(15) . 1_455 ? C2 N1 C8 116.3(3) . . ? C2 N1 Fe1 128.7(2) . . ? C8 N1 Fe1 113.9(2) . . ? C3 N2 C9 116.4(3) . . ? C3 N2 Fe1 128.5(2) . . ? C9 N2 Fe1 115.1(2) . . ? C4 N3 C10 116.8(3) . . ? C4 N3 Fe2 129.0(2) . . ? C10 N3 Fe2 113.4(2) . . ? C5 N4 C11 117.0(3) . . ? C5 N4 Fe2 128.3(2) . . ? C11 N4 Fe2 114.5(2) . . ? C6 N5 C12 116.2(3) . . ? C1 N6 C7 116.6(3) . . ? N6 C1 C2 122.6(3) . . ? N1 C2 C1 121.6(3) . . ? N2 C3 C4 122.3(3) . . ? N3 C4 C3 121.6(3) . . ? N4 C5 C6 120.9(3) . . ? N5 C6 C5 123.4(3) . . ? N6 C7 C8 121.1(3) . . ? N6 C7 C12 120.2(3) . . ? C8 C7 C12 118.7(3) . . ? N1 C8 C7 121.8(3) . . ? N1 C8 C9 116.7(3) . . ? C7 C8 C9 121.4(3) . . ? N2 C9 C10 121.7(3) . . ? N2 C9 C8 118.8(3) . . ? C10 C9 C8 119.5(3) . . ? N3 C10 C9 121.1(3) . . ? N3 C10 C11 118.5(3) . . ? C9 C10 C11 120.3(3) . . ? N4 C11 C12 121.9(3) . . ? N4 C11 C10 117.5(3) . . ? C12 C11 C10 120.5(3) . . ? N5 C12 C11 120.6(3) . . ? N5 C12 C7 120.0(3) . . ? C11 C12 C7 119.5(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 59.10 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.520 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.122 #=== END data_d:\mike\X-ray\ms026\try1 _database_code_depnum_ccdc_archive 'CCDC 264318' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H40.24 Cl6 Fe3 N6 O9.12' _chemical_formula_weight 882.29 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' Cl Cl 0.1484 0.1585 '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 7.9876(9) _cell_length_b 16.123(2) _cell_length_c 17.516(2) _cell_angle_alpha 72.224(3) _cell_angle_beta 80.061(3) _cell_angle_gamma 80.739(3) _cell_volume 2101.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 893 _exptl_absorpt_coefficient_mu 1.447 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Scheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 383(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 SMART 1000' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21685 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0772 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8551 _reflns_number_gt 5778 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1996)' _computing_cell_refinement 'SMART (Bruker, 1996)' _computing_data_reduction 'SAINT (Bruker, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2001)' _computing_publication_material 'XSEED (Barbour, 2001)' _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. Hydrogen atoms of water molecules were located on the difference Fourier map and the O-H and H-H distances were fixed at 0.92 and 1.54 A, respectively. The atomic displacement parameters for disordered atoms appearing close to each other were set equal. ; _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^)+(0.1255P)^2^+2.1383P] 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 8551 _refine_ls_number_parameters 454 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.2183 _refine_ls_wR_factor_gt 0.1945 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.91680(9) 0.92497(5) 0.46225(4) 0.01521(19) Uani 1 1 d . . . Fe2 Fe 1.34600(11) 0.56768(5) 0.30709(5) 0.0224(2) Uani 1 1 d . . . Fe3 Fe 1.51732(10) 1.01636(5) 0.09411(5) 0.01689(19) Uani 1 1 d . . . Cl1 Cl 0.83655(16) 1.07683(8) 0.46607(8) 0.0183(3) Uani 1 1 d . . . Cl2 Cl 0.75156(19) 0.84300(10) 0.57621(9) 0.0296(4) Uani 1 1 d . . . Cl3 Cl 1.2098(2) 0.45040(9) 0.39902(10) 0.0315(4) Uani 1 1 d . . . Cl4 Cl 1.5049(2) 1.16979(9) 0.06628(9) 0.0285(3) Uani 1 1 d . . . Cl5 Cl 1.28080(16) 1.01698(9) 0.01625(8) 0.0197(3) Uani 1 1 d . . . Cl6 Cl 0.7827(2) 0.80916(10) 0.28397(9) 0.0296(3) Uani 1 1 d . . . O1 O 0.7345(5) 0.9416(3) 0.3818(2) 0.0243(9) Uani 1 1 d . . . H1A H 0.7468 0.9054 0.3565 0.037 Uiso 1 1 calc R . . O2 O 1.1775(8) 0.5918(4) 0.2184(3) 0.0524(17) Uani 0.645(10) 1 d PD A 1 H2A H 1.1443 0.6397 0.1888 0.079 Uiso 1 1 calc R A 1 O3 O 1.5365(6) 0.5636(4) 0.3824(3) 0.0487(16) Uani 0.823(10) 1 d PD B 1 O4 O 1.5423(8) 0.5012(3) 0.2312(4) 0.0524(15) Uani 1 1 d D . . O5 O 1.7152(5) 0.9936(3) 0.1689(2) 0.0254(9) Uani 1 1 d . . . H5A H 1.7343 0.9427 0.1963 0.038 Uiso 1 1 calc R . . O2A O 1.1775(8) 0.5918(4) 0.2184(3) 0.0524(17) Uani 0.36 1 d P A 2 H2B H 1.2012 0.6214 0.2450 0.079 Uiso 0.355(10) 1 calc PR A 2 O3A O 1.5365(6) 0.5636(4) 0.3824(3) 0.0487(16) Uani 0.18 1 d P B 2 O4Q O 1.278(5) 0.566(3) -0.007(3) 0.149(16) Uiso 0.25 1 d PD C 4 O5Q O 1.677(3) 0.2294(17) 0.1858(12) 0.072(7) Uiso 0.25 1 d PD D 6 H5Q H 1.7752 0.2425 0.1788 0.108 Uiso 0.25 1 calc PR D 6 O1S O 1.900(2) 0.3147(10) 0.3340(10) 0.129(8) Uani 0.50 1 d PD . . H1S H 1.9522 0.3369 0.2897 0.194 Uiso 0.50 1 calc PR . . O2S O 1.5513(11) 0.3638(5) 0.4947(5) 0.103(3) Uani 1 1 d D . . H2S H 1.5186 0.3820 0.5343 0.154 Uiso 1 1 calc R . . O3S O 0.0170(11) 0.7415(5) 0.1528(4) 0.097(3) Uani 1 1 d . . . H3S H -0.0542 0.7612 0.1845 0.145 Uiso 1 1 calc R . . O4S O 1.519(4) 0.5576(19) 0.0739(17) 0.088(9) Uiso 0.25 1 d PD E 3 H4S H 1.6162 0.5662 0.0513 0.132 Uiso 0.25 1 calc PR E 3 O5S O 1.541(2) 0.2516(11) 0.2967(12) 0.042(5) Uiso 0.25 1 d PD F 5 H5S H 1.5940 0.2610 0.3287 0.063 Uiso 0.25 1 calc PR F 5 O6S O 0.959(4) 0.6854(19) -0.1451(17) 0.081(6) Uiso 0.25 1 d PD G 7 H6S H 0.8602 0.6742 -0.1366 0.122 Uiso 0.25 1 calc PR G 7 O7S O 0.849(4) 0.6002(17) 0.0148(17) 0.081(6) Uiso 0.25 1 d PD H 8 H7S H 0.8836 0.5832 0.0592 0.122 Uiso 0.25 1 calc PR H 8 O3W O 0.612(3) 0.3546(16) 0.2034(15) 0.003(8) Uiso 0.119(12) 1 d P . . N1 N 1.0937(6) 0.9723(3) 0.3468(3) 0.0157(9) Uani 1 1 d . . . N2 N 1.0311(5) 0.8044(3) 0.4282(3) 0.0152(9) Uani 1 1 d . . . N3 N 1.1946(6) 0.6655(3) 0.3662(3) 0.0209(10) Uani 1 1 d . . . N4 N 1.4316(6) 0.6985(3) 0.2304(3) 0.0198(10) Uani 1 1 d . . . N5 N 1.4974(6) 0.8716(3) 0.1478(3) 0.0159(9) Uani 1 1 d . . . N6 N 1.3289(6) 1.0070(3) 0.2040(3) 0.0164(10) Uani 1 1 d . . . C1 C 0.9992(7) 0.7219(4) 0.4630(3) 0.0215(12) Uani 1 1 d . . . H1 H 0.9210 0.7094 0.5098 0.026 Uiso 1 1 calc R . . C2 C 1.0793(7) 0.6530(4) 0.4316(3) 0.0218(12) Uani 1 1 d . . . H2 H 1.0505 0.5966 0.4575 0.026 Uiso 1 1 calc R . . C3 C 1.5439(7) 0.7169(4) 0.1645(3) 0.0234(13) Uani 1 1 d . . . H3 H 1.6034 0.6712 0.1454 0.028 Uiso 1 1 calc R . . C4 C 1.5772(7) 0.8047(4) 0.1215(3) 0.0198(12) Uani 1 1 d . . . H4 H 1.6554 0.8151 0.0746 0.024 Uiso 1 1 calc R . . C5 C 1.2444(7) 1.0704(3) 0.2339(3) 0.0169(11) Uani 1 1 d . . . H5 H 1.2642 1.1281 0.2072 0.020 Uiso 1 1 calc R . . C6 C 1.1250(7) 1.0531(4) 0.3051(3) 0.0190(12) Uani 1 1 d . . . H6 H 1.0669 1.0998 0.3231 0.023 Uiso 1 1 calc R . . C7 C 1.1464(6) 0.8182(3) 0.3601(3) 0.0148(11) Uani 1 1 d . . . C8 C 1.2285(7) 0.7494(3) 0.3289(3) 0.0167(11) Uani 1 1 d . . . C9 C 1.3509(7) 0.7664(4) 0.2570(3) 0.0179(12) Uani 1 1 d . . . C10 C 1.3831(7) 0.8530(4) 0.2164(3) 0.0166(11) Uani 1 1 d . . . C11 C 1.2967(7) 0.9239(3) 0.2461(3) 0.0150(11) Uani 1 1 d . . . C12 C 1.1787(6) 0.9071(3) 0.3171(3) 0.0133(11) Uani 1 1 d . . . C13 C 0.5583(8) 0.9718(6) 0.3956(5) 0.0455(19) Uani 1 1 d . . . H13A H 0.4983 0.9245 0.4311 0.068 Uiso 1 1 calc R . . H13B H 0.5124 0.9927 0.3451 0.068 Uiso 1 1 calc R . . H13C H 0.5449 1.0186 0.4201 0.068 Uiso 1 1 calc R . . C14 C 0.996(3) 0.5843(17) 0.2349(15) 0.061(3) Uiso 0.355(10) 1 d PD A 2 H14A H 0.9424 0.6170 0.1878 0.091 Uiso 0.355(10) 1 calc PR A 2 H14B H 0.9461 0.6073 0.2793 0.091 Uiso 0.355(10) 1 calc PR A 2 H14C H 0.9777 0.5238 0.2484 0.091 Uiso 0.355(10) 1 calc PR A 2 C15 C 1.1058(18) 0.5227(9) 0.2004(8) 0.061(3) Uiso 0.645(10) 1 d PD A 1 H15A H 1.1621 0.5151 0.1496 0.091 Uiso 0.645(10) 1 calc PR A 1 H15B H 0.9856 0.5391 0.1975 0.091 Uiso 0.645(10) 1 calc PR A 1 H15C H 1.1229 0.4688 0.2424 0.091 Uiso 0.645(10) 1 calc PR A 1 C16 C 1.644(5) 0.490(3) 0.417(2) 0.060(3) Uani 0.177(10) 1 d PD B 2 H16A H 1.7609 0.5015 0.4007 0.090 Uiso 0.177(10) 1 calc PR B 2 H16B H 1.6263 0.4415 0.3988 0.090 Uiso 0.177(10) 1 calc PR B 2 H16C H 1.6189 0.4749 0.4746 0.090 Uiso 0.177(10) 1 calc PR B 2 C17 C 1.7113(12) 0.5601(7) 0.3694(7) 0.060(3) Uani 0.823(10) 1 d PD B 1 H17A H 1.7601 0.5061 0.3579 0.090 Uiso 0.823(10) 1 calc PR B 1 H17B H 1.7518 0.5632 0.4169 0.090 Uiso 0.823(10) 1 calc PR B 1 H17C H 1.7446 0.6086 0.3244 0.090 Uiso 0.823(10) 1 calc PR B 1 C18 C 1.8711(8) 1.0330(5) 0.1450(4) 0.0402(18) Uani 1 1 d . . . H18A H 1.9455 1.0062 0.1077 0.060 Uiso 1 1 calc R . . H18B H 1.9261 1.0247 0.1918 0.060 Uiso 1 1 calc R . . H18C H 1.8466 1.0946 0.1194 0.060 Uiso 1 1 calc R . . C4Q C 1.394(3) 0.6076(16) 0.0187(15) 0.096(7) Uiso 0.25 1 d PD C 4 C5Q C 1.637(2) 0.1823(10) 0.2652(9) 0.053(4) Uiso 0.25 1 d P D 6 C1S C 1.716(2) 0.3558(10) 0.3374(15) 0.088(8) Uani 0.50 1 d PD . . H1S1 H 1.6501 0.3232 0.3852 0.131 Uiso 0.50 1 calc PR . . H1S2 H 1.6700 0.3550 0.2904 0.131 Uiso 0.50 1 calc PR . . H1S3 H 1.7106 0.4153 0.3386 0.131 Uiso 0.50 1 calc PR . . C2S C 1.5080(11) 0.2745(5) 0.5129(6) 0.059(2) Uani 1 1 d D . . H2S1 H 1.6077 0.2372 0.4992 0.089 Uiso 1 1 calc R . . H2S2 H 1.4199 0.2744 0.4819 0.089 Uiso 1 1 calc R . . H2S3 H 1.4679 0.2532 0.5695 0.089 Uiso 1 1 calc R . . C3S C 0.0767(11) 0.8114(6) 0.0879(5) 0.058(2) Uani 1 1 d . . . C4S C 1.394(3) 0.6076(16) 0.0187(15) 0.096(7) Uiso 0.25 1 d PD E 3 C5S C 1.637(2) 0.1823(10) 0.2652(9) 0.053(4) Uiso 0.25 1 d PD F 5 C6S C 0.987(5) 0.726(3) -0.088(3) 0.109(15) Uani 0.25 1 d PD G 7 C7S C 0.902(5) 0.685(2) -0.028(3) 0.109(15) Uani 0.25 1 d PD H 8 H19A H 1.557(17) 0.441(2) 0.260(5) 0.163 Uiso 1 1 d D . . H19B H 1.535(16) 0.498(6) 0.179(3) 0.163 Uiso 1 1 d 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 Fe1 0.0134(4) 0.0173(4) 0.0150(4) -0.0053(3) 0.0003(3) -0.0026(3) Fe2 0.0266(5) 0.0165(4) 0.0219(4) -0.0049(3) 0.0028(3) -0.0039(3) Fe3 0.0165(4) 0.0203(4) 0.0123(4) -0.0019(3) 0.0006(3) -0.0058(3) Cl1 0.0160(6) 0.0203(6) 0.0195(6) -0.0079(5) -0.0033(5) 0.0010(5) Cl2 0.0287(8) 0.0323(8) 0.0275(8) -0.0099(6) 0.0048(6) -0.0089(6) Cl3 0.0387(9) 0.0188(7) 0.0329(8) -0.0039(6) 0.0044(7) -0.0087(6) Cl4 0.0372(8) 0.0227(7) 0.0238(7) -0.0024(6) -0.0006(6) -0.0102(6) Cl5 0.0137(6) 0.0293(7) 0.0133(6) -0.0018(5) 0.0010(5) -0.0057(5) Cl6 0.0369(8) 0.0292(8) 0.0250(7) -0.0095(6) -0.0119(6) 0.0017(6) O1 0.017(2) 0.036(2) 0.027(2) -0.0195(18) -0.0066(17) 0.0017(17) O2 0.072(4) 0.051(3) 0.040(3) -0.004(3) -0.025(3) -0.021(3) O3 0.033(3) 0.055(3) 0.052(3) -0.003(3) -0.010(2) -0.009(2) O4 0.068(4) 0.014(2) 0.065(4) -0.003(2) 0.004(3) -0.006(2) O5 0.021(2) 0.034(2) 0.021(2) -0.0024(18) -0.0041(17) -0.0117(18) O2A 0.072(4) 0.051(3) 0.040(3) -0.004(3) -0.025(3) -0.021(3) O3A 0.033(3) 0.055(3) 0.052(3) -0.003(3) -0.010(2) -0.009(2) O1S 0.192(18) 0.081(11) 0.108(12) 0.054(9) -0.101(13) -0.071(12) O2S 0.110(6) 0.130(7) 0.096(6) -0.070(5) 0.031(5) -0.070(5) O3S 0.104(6) 0.089(5) 0.060(5) -0.006(4) 0.021(4) 0.030(5) N1 0.015(2) 0.017(2) 0.014(2) -0.0026(18) -0.0044(18) -0.0021(18) N2 0.011(2) 0.017(2) 0.017(2) -0.0038(18) -0.0004(17) -0.0009(17) N3 0.021(2) 0.016(2) 0.023(3) -0.0036(19) 0.000(2) -0.0042(19) N4 0.019(2) 0.018(2) 0.020(2) -0.0047(19) 0.0022(19) -0.0002(19) N5 0.016(2) 0.021(2) 0.012(2) -0.0053(18) -0.0015(17) -0.0036(18) N6 0.013(2) 0.021(2) 0.015(2) -0.0050(18) 0.0008(18) -0.0045(18) C1 0.022(3) 0.021(3) 0.018(3) -0.002(2) 0.004(2) -0.008(2) C2 0.022(3) 0.021(3) 0.018(3) -0.003(2) 0.006(2) -0.004(2) C3 0.025(3) 0.021(3) 0.022(3) -0.009(2) 0.005(2) 0.000(2) C4 0.016(3) 0.024(3) 0.018(3) -0.006(2) 0.001(2) -0.002(2) C5 0.020(3) 0.013(3) 0.018(3) -0.001(2) -0.005(2) -0.004(2) C6 0.018(3) 0.016(3) 0.023(3) -0.007(2) -0.004(2) 0.002(2) C7 0.011(2) 0.018(3) 0.016(3) -0.005(2) 0.000(2) -0.004(2) C8 0.016(3) 0.012(2) 0.020(3) -0.002(2) -0.001(2) 0.000(2) C9 0.014(3) 0.017(3) 0.021(3) -0.004(2) -0.002(2) -0.002(2) C10 0.012(3) 0.022(3) 0.015(3) -0.003(2) -0.003(2) -0.004(2) C11 0.014(3) 0.018(3) 0.012(2) -0.003(2) -0.002(2) -0.002(2) C12 0.011(2) 0.018(3) 0.012(2) -0.005(2) -0.0005(19) -0.004(2) C13 0.019(3) 0.070(5) 0.057(5) -0.037(4) -0.014(3) 0.016(3) C16 0.044(6) 0.042(6) 0.086(8) -0.003(5) -0.015(5) -0.004(4) C17 0.044(6) 0.042(6) 0.086(8) -0.003(5) -0.015(5) -0.004(4) C18 0.026(3) 0.055(5) 0.040(4) -0.004(3) -0.009(3) -0.020(3) C1S 0.057(11) 0.030(9) 0.15(2) 0.033(11) -0.052(13) -0.018(8) C2S 0.057(5) 0.052(5) 0.078(6) -0.027(5) -0.027(5) 0.002(4) C3S 0.053(5) 0.055(5) 0.050(5) 0.000(4) 0.017(4) -0.019(4) C6S 0.034(16) 0.08(2) 0.24(5) -0.06(3) -0.05(2) -0.014(13) C7S 0.034(16) 0.08(2) 0.24(5) -0.06(3) -0.05(2) -0.014(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 Fe1 N2 2.217(4) . ? Fe1 N1 2.256(4) . ? Fe1 Cl2 2.3483(16) . ? Fe1 Cl1 2.4475(15) . ? Fe1 Cl1 2.5044(15) 2_776 ? Fe2 N3 2.231(5) . ? Fe2 O4 2.233(6) . ? Fe2 N4 2.267(5) . ? Fe2 Cl3 2.3559(16) . ? Fe3 N6 2.210(4) . ? Fe3 N5 2.255(4) . ? Fe3 Cl4 2.3597(17) . ? Fe3 Cl5 2.4302(15) 2_875 ? Fe3 Cl5 2.5108(15) . ? Cl1 Fe1 2.5044(15) 2_776 ? Cl5 Fe3 2.4302(15) 2_875 ? O1 C13 1.418(7) . ? O2 C15 1.467(14) . ? O3 C17 1.371(11) . ? O5 C18 1.429(7) . ? O4Q C4Q 1.429(19) . ? O5Q C5Q 1.378(17) . ? O1S C1S 1.510(16) . ? O2S C2S 1.462(10) . ? O3S C3S 1.411(10) . ? O6S C6S 1.413(19) . ? O7S C7S 1.435(19) . ? N1 C6 1.325(7) . ? N1 C12 1.347(7) . ? N2 C1 1.330(7) . ? N2 C7 1.358(7) . ? N3 C2 1.324(7) . ? N3 C8 1.358(7) . ? N4 C3 1.320(7) . ? N4 C9 1.346(7) . ? N5 C4 1.328(7) . ? N5 C10 1.362(7) . ? N6 C5 1.326(7) . ? N6 C11 1.359(7) . ? C1 C2 1.404(8) . ? C3 C4 1.429(8) . ? C5 C6 1.417(8) . ? C7 C8 1.405(7) . ? C7 C12 1.443(7) . ? C8 C9 1.438(7) . ? C9 C10 1.402(8) . ? C10 C11 1.428(8) . ? C11 C12 1.407(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 N2 Fe1 N1 75.13(16) . . ? N2 Fe1 Cl2 91.13(12) . . ? N1 Fe1 Cl2 166.21(13) . . ? N2 Fe1 Cl1 164.63(12) . . ? N1 Fe1 Cl1 89.51(12) . . ? Cl2 Fe1 Cl1 104.21(6) . . ? N2 Fe1 Cl1 92.66(12) . 2_776 ? N1 Fe1 Cl1 86.09(12) . 2_776 ? Cl2 Fe1 Cl1 95.86(6) . 2_776 ? Cl1 Fe1 Cl1 86.72(5) . 2_776 ? N3 Fe2 O4 163.65(18) . . ? N3 Fe2 N4 75.16(16) . . ? O4 Fe2 N4 89.15(17) . . ? N3 Fe2 Cl3 92.85(12) . . ? O4 Fe2 Cl3 103.01(13) . . ? N4 Fe2 Cl3 167.73(13) . . ? N6 Fe3 N5 75.35(16) . . ? N6 Fe3 Cl4 92.09(13) . . ? N5 Fe3 Cl4 167.12(12) . . ? N6 Fe3 Cl5 163.98(13) . 2_875 ? N5 Fe3 Cl5 88.69(12) . 2_875 ? Cl4 Fe3 Cl5 103.92(6) . 2_875 ? N6 Fe3 Cl5 89.41(12) . . ? N5 Fe3 Cl5 85.86(12) . . ? Cl4 Fe3 Cl5 97.03(6) . . ? Cl5 Fe3 Cl5 87.94(5) 2_875 . ? Fe1 Cl1 Fe1 93.28(5) . 2_776 ? Fe3 Cl5 Fe3 92.06(5) 2_875 . ? C6 N1 C12 116.6(5) . . ? C6 N1 Fe1 129.7(4) . . ? C12 N1 Fe1 113.6(3) . . ? C1 N2 C7 115.9(5) . . ? C1 N2 Fe1 129.5(4) . . ? C7 N2 Fe1 114.5(3) . . ? C2 N3 C8 116.8(5) . . ? C2 N3 Fe2 129.2(4) . . ? C8 N3 Fe2 114.0(4) . . ? C3 N4 C9 117.0(5) . . ? C3 N4 Fe2 129.8(4) . . ? C9 N4 Fe2 113.1(3) . . ? C4 N5 C10 117.5(5) . . ? C4 N5 Fe3 129.5(4) . . ? C10 N5 Fe3 113.1(3) . . ? C5 N6 C11 116.4(4) . . ? C5 N6 Fe3 129.2(4) . . ? C11 N6 Fe3 114.4(3) . . ? N2 C1 C2 122.3(5) . . ? N3 C2 C1 122.2(5) . . ? N4 C3 C4 122.3(5) . . ? N5 C4 C3 120.5(5) . . ? N6 C5 C6 122.1(5) . . ? N1 C6 C5 121.9(5) . . ? N2 C7 C8 122.1(5) . . ? N2 C7 C12 118.4(5) . . ? C8 C7 C12 119.5(5) . . ? N3 C8 C7 120.7(5) . . ? N3 C8 C9 118.8(5) . . ? C7 C8 C9 120.5(5) . . ? N4 C9 C10 121.7(5) . . ? N4 C9 C8 118.9(5) . . ? C10 C9 C8 119.4(5) . . ? N5 C10 C9 121.0(5) . . ? N5 C10 C11 118.3(5) . . ? C9 C10 C11 120.7(5) . . ? N6 C11 C12 121.2(5) . . ? N6 C11 C10 118.8(5) . . ? C12 C11 C10 120.0(5) . . ? N1 C12 C11 121.8(5) . . ? N1 C12 C7 118.3(4) . . ? C11 C12 C7 119.9(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.253 _refine_diff_density_min -1.167 _refine_diff_density_rms 0.174