# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Controlling Carbon Monoxide Binding at Di-iron Units Related to the Iron-only Hydrogenase Sub-site ; _publ_contact_author_name 'Prof. C. Pickett' _publ_contact_author_email 'C.PICKETT@UEA.AC.UK, XIAOMING.LIU@NCU.EDU.CN' loop_ _publ_author_name C.Pickett D.Hughes S.K.Ibrahim 'Xiaoming Liu' 'Qiu-Yan Luo' ; C.Tard ; 'Xiufeng Wang' 'Fenfen Xu' 'Xi-Rui Zeng' 'Wei Zhong' # Attachment 'Fe2S2newCIFs.cif' # This file contains four .CIF files to accompany the MS: # # "Controlling carbon monoxide binding at di-iron units related to the # iron-only hydrogenase sub-site" # # by F. Xu, C. Tard, X. Wang, S.K. Ibrahim, D.L. Hughes, W. Zhong, X. # Zeng, Q. Luo, X. Liu and C.J. Pickett # data_xiaomingl8 _database_code_depnum_ccdc_archive 'CCDC 658089' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound A, X=CH2NH2' _chemical_melting_point ? _chemical_formula_structural '[Fe2 (CO)5 {MeC(SCH2)CH2NH2}].MeCN' _chemical_formula_moiety 'C10 H11 Fe2 N O5 S2, C2 H3 N' _chemical_formula_sum 'C12 H14 Fe2 N2 O5 S2' _chemical_formula_weight 442.07 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 orthorhombic _symmetry_space_group_name_H-M Pnma #(no. 62) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 17.9779(12) _cell_length_b 9.6907(7) _cell_length_c 9.6462(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1680.55(19) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 1.112 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 29453 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0140 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2582 _reflns_number_gt 2308 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0305P)^2^+0.6602P] 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 2582 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.002 _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 0.459987(15) 0.2500 0.10319(3) 0.01713(7) Uani 1 2 d S . . Fe2 Fe 0.434517(15) 0.2500 0.35689(3) 0.01792(7) Uani 1 2 d S . . S1 S 0.506190(17) 0.41095(3) 0.25024(3) 0.01935(8) Uani 1 1 d . . . C1 C 0.60250(7) 0.37963(15) 0.29964(15) 0.0246(3) Uani 1 1 d . . . H1A H 0.6321 0.3755 0.2156 0.029 Uiso 1 1 calc R . . H1B H 0.6197 0.4586 0.3524 0.029 Uiso 1 1 calc R . . C2 C 0.61846(10) 0.2500 0.38415(19) 0.0188(3) Uani 1 2 d S . . C21 C 0.70258(10) 0.2500 0.4152(2) 0.0250(4) Uani 1 2 d S . . H21A H 0.7151 0.3304 0.4685 0.037 Uiso 0.50 1 calc PR . . H21B H 0.7298 0.2509 0.3296 0.037 Uiso 1 2 calc SR . . H21C H 0.7152 0.1687 0.4669 0.037 Uiso 0.50 1 calc PR . . C3 C 0.57929(11) 0.2500 0.5261(2) 0.0249(4) Uani 1 2 d S . . H3A H 0.5967 0.1696 0.5765 0.030 Uiso 0.50 1 calc PR . . H3B H 0.5967 0.3304 0.5765 0.030 Uiso 0.50 1 calc PR . . N4 N 0.49820(10) 0.2500 0.53326(18) 0.0398(5) Uani 1 2 d S . . H4A H 0.4848 0.3245 0.5830 0.048 Uiso 0.50 1 calc PR . . H4B H 0.4848 0.1755 0.5830 0.048 Uiso 0.50 1 calc PR . . C11 C 0.52340(11) 0.2500 -0.0421(2) 0.0218(4) Uani 1 2 d S . . O11 O 0.56262(9) 0.2500 -0.13458(16) 0.0318(3) Uani 1 2 d S . . C12 C 0.39788(7) 0.11763(15) 0.04455(14) 0.0220(3) Uani 1 1 d . . . O12 O 0.35765(6) 0.03298(11) 0.01121(11) 0.0302(2) Uani 1 1 d . . . C22 C 0.36435(8) 0.12606(15) 0.37817(15) 0.0251(3) Uani 1 1 d . . . O22 O 0.31423(7) 0.05127(13) 0.38216(14) 0.0406(3) Uani 1 1 d . . . N5 N 0.37219(11) 0.2500 0.7383(2) 0.0367(4) Uani 1 2 d S . . C51 C 0.31093(12) 0.2500 0.7093(2) 0.0261(4) Uani 1 2 d S . . C52 C 0.23285(14) 0.2500 0.6710(3) 0.0438(6) Uani 1 2 d S . . H52A H 0.2148 0.1568 0.6688 0.066 Uiso 0.50 1 calc PR . . H52B H 0.2272 0.2911 0.5811 0.066 Uiso 0.50 1 calc PR . . H52C H 0.2050 0.3021 0.7378 0.066 Uiso 0.50 1 calc PR . . 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 0.01855(13) 0.01896(13) 0.01388(12) 0.000 -0.00003(9) 0.000 Fe2 0.01799(13) 0.02102(13) 0.01476(12) 0.000 0.00100(9) 0.000 S1 0.02161(15) 0.01692(14) 0.01952(14) 0.00069(11) -0.00142(11) -0.00021(11) C1 0.0202(6) 0.0257(7) 0.0278(7) 0.0072(5) -0.0013(5) -0.0053(5) C2 0.0170(8) 0.0205(8) 0.0189(8) 0.000 -0.0004(6) 0.000 C21 0.0192(9) 0.0292(10) 0.0266(9) 0.000 -0.0004(7) 0.000 C3 0.0205(9) 0.0354(11) 0.0189(9) 0.000 -0.0010(7) 0.000 N4 0.0195(8) 0.0829(16) 0.0169(8) 0.000 0.0009(7) 0.000 C11 0.0216(8) 0.0238(9) 0.0200(8) 0.000 -0.0023(7) 0.000 O11 0.0302(8) 0.0398(9) 0.0255(8) 0.000 0.0087(6) 0.000 C12 0.0217(6) 0.0265(6) 0.0177(6) 0.0009(5) 0.0010(5) 0.0031(5) O12 0.0289(5) 0.0287(5) 0.0329(5) -0.0044(4) -0.0025(4) -0.0050(4) C22 0.0258(6) 0.0260(7) 0.0236(7) 0.0070(5) 0.0025(5) 0.0031(5) O22 0.0330(6) 0.0348(6) 0.0541(7) 0.0117(6) 0.0052(5) -0.0093(5) N5 0.0283(9) 0.0533(13) 0.0284(9) 0.000 0.0014(8) 0.000 C51 0.0312(10) 0.0262(10) 0.0209(9) 0.000 0.0041(8) 0.000 C52 0.0284(11) 0.0595(17) 0.0433(14) 0.000 -0.0008(10) 0.000 _atom_sites_special_details ; We note that both the di-iron complex molecule and the acetonitrile molecule lie on mirror-planes and show crystallographic symmetry. ; _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 C12 1.7922(14) . ? Fe1 C12 1.7922(14) 6_565 ? Fe1 C11 1.807(2) . ? Fe1 S1 2.2660(4) . ? Fe1 S1 2.2660(4) 6_565 ? Fe1 Fe2 2.4897(4) . ? Fe2 C22 1.7538(15) . ? Fe2 C22 1.7538(15) 6_565 ? Fe2 N4 2.0507(18) . ? Fe2 S1 2.2697(4) 6_565 ? Fe2 S1 2.2697(4) . ? S1 C1 1.8213(14) . ? C1 C2 1.5248(17) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C1 1.5248(17) 6_565 ? C2 C3 1.540(3) . ? C2 C21 1.542(3) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C3 N4 1.460(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C11 O11 1.137(3) . ? C12 O12 1.1400(17) . ? C22 O22 1.1570(18) . ? N5 C51 1.136(3) . ? C51 C52 1.452(3) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? 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 C12 Fe1 C12 91.41(9) . 6_565 ? C12 Fe1 C11 98.53(6) . . ? C12 Fe1 C11 98.53(6) 6_565 . ? C12 Fe1 S1 156.72(5) . . ? C12 Fe1 S1 86.17(4) 6_565 . ? C11 Fe1 S1 104.73(4) . . ? C12 Fe1 S1 86.17(4) . 6_565 ? C12 Fe1 S1 156.72(5) 6_565 6_565 ? C11 Fe1 S1 104.73(4) . 6_565 ? S1 Fe1 S1 86.996(19) . 6_565 ? C12 Fe1 Fe2 101.28(4) . . ? C12 Fe1 Fe2 101.28(4) 6_565 . ? C11 Fe1 Fe2 151.47(6) . . ? S1 Fe1 Fe2 56.778(11) . . ? S1 Fe1 Fe2 56.778(11) 6_565 . ? C22 Fe2 C22 86.45(9) . 6_565 ? C22 Fe2 N4 107.72(6) . . ? C22 Fe2 N4 107.72(6) 6_565 . ? C22 Fe2 S1 89.47(5) . 6_565 ? C22 Fe2 S1 158.75(5) 6_565 6_565 ? N4 Fe2 S1 93.39(4) . 6_565 ? C22 Fe2 S1 158.75(5) . . ? C22 Fe2 S1 89.47(5) 6_565 . ? N4 Fe2 S1 93.39(4) . . ? S1 Fe2 S1 86.819(19) 6_565 . ? C22 Fe2 Fe1 104.32(5) . . ? C22 Fe2 Fe1 104.32(5) 6_565 . ? N4 Fe2 Fe1 135.47(5) . . ? S1 Fe2 Fe1 56.637(11) 6_565 . ? S1 Fe2 Fe1 56.637(11) . . ? C1 S1 Fe1 113.42(5) . . ? C1 S1 Fe2 107.85(5) . . ? Fe1 S1 Fe2 66.585(13) . . ? C2 C1 S1 117.13(10) . . ? C2 C1 H1A 108.0 . . ? S1 C1 H1A 108.0 . . ? C2 C1 H1B 108.0 . . ? S1 C1 H1B 108.0 . . ? H1A C1 H1B 107.3 . . ? C1 C2 C1 110.94(16) 6_565 . ? C1 C2 C3 112.92(10) 6_565 . ? C1 C2 C3 112.92(10) . . ? C1 C2 C21 106.76(10) 6_565 . ? C1 C2 C21 106.76(10) . . ? C3 C2 C21 106.01(15) . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C3 C2 119.92(16) . . ? N4 C3 H3A 107.3 . . ? C2 C3 H3A 107.3 . . ? N4 C3 H3B 107.3 . . ? C2 C3 H3B 107.3 . . ? H3A C3 H3B 106.9 . . ? C3 N4 Fe2 121.23(13) . . ? C3 N4 H4A 107.0 . . ? Fe2 N4 H4A 107.0 . . ? C3 N4 H4B 107.0 . . ? Fe2 N4 H4B 107.0 . . ? H4A N4 H4B 106.8 . . ? O11 C11 Fe1 179.19(18) . . ? O12 C12 Fe1 177.96(13) . . ? O22 C22 Fe2 173.22(13) . . ? N5 C51 C52 179.5(2) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? 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 C12 Fe1 Fe2 C22 -1.90(6) . . . . ? C12 Fe1 Fe2 C22 91.85(7) 6_565 . . . ? C11 Fe1 Fe2 C22 -135.02(5) . . . . ? S1 Fe1 Fe2 C22 169.61(5) . . . . ? S1 Fe1 Fe2 C22 -79.66(5) 6_565 . . . ? C12 Fe1 Fe2 C22 -91.85(7) . . . 6_565 ? C12 Fe1 Fe2 C22 1.90(6) 6_565 . . 6_565 ? C11 Fe1 Fe2 C22 135.02(5) . . . 6_565 ? S1 Fe1 Fe2 C22 79.66(5) . . . 6_565 ? S1 Fe1 Fe2 C22 -169.61(5) 6_565 . . 6_565 ? C12 Fe1 Fe2 N4 133.13(4) . . . . ? C12 Fe1 Fe2 N4 -133.13(4) 6_565 . . . ? C11 Fe1 Fe2 N4 0.0 . . . . ? S1 Fe1 Fe2 N4 -55.367(11) . . . . ? S1 Fe1 Fe2 N4 55.367(11) 6_565 . . . ? C12 Fe1 Fe2 S1 77.76(5) . . . 6_565 ? C12 Fe1 Fe2 S1 171.51(5) 6_565 . . 6_565 ? C11 Fe1 Fe2 S1 -55.367(11) . . . 6_565 ? S1 Fe1 Fe2 S1 -110.73(2) . . . 6_565 ? C12 Fe1 Fe2 S1 -171.51(5) . . . . ? C12 Fe1 Fe2 S1 -77.76(5) 6_565 . . . ? C11 Fe1 Fe2 S1 55.367(11) . . . . ? S1 Fe1 Fe2 S1 110.73(2) 6_565 . . . ? C12 Fe1 S1 C1 121.66(12) . . . . ? C12 Fe1 S1 C1 -153.68(7) 6_565 . . . ? C11 Fe1 S1 C1 -55.86(7) . . . . ? S1 Fe1 S1 C1 48.59(5) 6_565 . . . ? Fe2 Fe1 S1 C1 100.16(5) . . . . ? C12 Fe1 S1 Fe2 21.50(11) . . . . ? C12 Fe1 S1 Fe2 106.15(4) 6_565 . . . ? C11 Fe1 S1 Fe2 -156.03(5) . . . . ? S1 Fe1 S1 Fe2 -51.578(14) 6_565 . . . ? C22 Fe2 S1 C1 -137.23(14) . . . . ? C22 Fe2 S1 C1 144.01(7) 6_565 . . . ? N4 Fe2 S1 C1 36.29(6) . . . . ? S1 Fe2 S1 C1 -56.93(6) 6_565 . . . ? Fe1 Fe2 S1 C1 -108.40(5) . . . . ? C22 Fe2 S1 Fe1 -28.83(14) . . . . ? C22 Fe2 S1 Fe1 -107.59(5) 6_565 . . . ? N4 Fe2 S1 Fe1 144.68(4) . . . . ? S1 Fe2 S1 Fe1 51.473(14) 6_565 . . . ? Fe1 S1 C1 C2 -65.03(12) . . . . ? Fe2 S1 C1 C2 6.58(13) . . . . ? S1 C1 C2 C1 65.52(18) . . . 6_565 ? S1 C1 C2 C3 -62.41(16) . . . . ? S1 C1 C2 C21 -178.52(11) . . . . ? C1 C2 C3 N4 -63.44(11) 6_565 . . . ? C1 C2 C3 N4 63.44(11) . . . . ? C21 C2 C3 N4 180.0 . . . . ? C2 C3 N4 Fe2 0.0 . . . . ? C22 Fe2 N4 C3 134.03(5) . . . . ? C22 Fe2 N4 C3 -134.03(5) 6_565 . . . ? S1 Fe2 N4 C3 43.505(10) 6_565 . . . ? S1 Fe2 N4 C3 -43.505(10) . . . . ? Fe1 Fe2 N4 C3 0.0 . . . . ? C12 Fe1 C11 O11 46.36(5) . . . . ? C12 Fe1 C11 O11 -46.37(4) 6_565 . . . ? S1 Fe1 C11 O11 -134.625(17) . . . . ? S1 Fe1 C11 O11 134.624(18) 6_565 . . . ? Fe2 Fe1 C11 O11 180.000(4) . . . . ? C12 Fe1 C12 O12 -100(4) 6_565 . . . ? C11 Fe1 C12 O12 161(4) . . . . ? S1 Fe1 C12 O12 -16(4) . . . . ? S1 Fe1 C12 O12 57(4) 6_565 . . . ? Fe2 Fe1 C12 O12 2(4) . . . . ? C22 Fe2 C22 O22 51.4(12) 6_565 . . . ? N4 Fe2 C22 O22 158.9(12) . . . . ? S1 Fe2 C22 O22 -107.7(12) 6_565 . . . ? S1 Fe2 C22 O22 -27.9(13) . . . . ? Fe1 Fe2 C22 O22 -52.5(12) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.575 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.063 #===END data_may905 _database_code_depnum_ccdc_archive 'CCDC 658090' _audit_creation_date 2005-05-13T12:32:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Compound B, X=NH2' _chemical_formula_structural '[Fe2 (CO)6 {MeC(CH2S)2-CH2NH2}]' _chemical_formula_moiety 'C11 H11 Fe2 N O6 S2' _chemical_formula_sum 'C11 H11 Fe2 N O6 S2' _chemical_formula_weight 429.03 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 26.7146(11) _cell_length_b 26.7146(11) _cell_length_c 8.8972(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6349.7(4) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19271 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.733 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.781 _exptl_absorpt_correction_T_max 0.961 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.363892E-1 _diffrn_orient_matrix_ub_12 -0.70028E-2 _diffrn_orient_matrix_ub_13 -0.158859E-1 _diffrn_orient_matrix_ub_21 0.55269E-2 _diffrn_orient_matrix_ub_22 -0.7547E-3 _diffrn_orient_matrix_ub_23 -0.11114 _diffrn_orient_matrix_ub_31 0.68179E-2 _diffrn_orient_matrix_ub_32 -0.367641E-1 _diffrn_orient_matrix_ub_33 0.53075E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_av_unetI/netI 0.0553 _diffrn_reflns_number 14820 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 26.67 _diffrn_reflns_theta_full 26.67 _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _reflns_number_total 3254 _reflns_number_gt 2408 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atoms on N were refined; other H atoms were in riding mode. 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^)+(0.0280P)^2^+32.4101P] 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_number_reflns 3254 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.102 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.279 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.087 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.31128(2) 0.32584(2) -0.14884(6) 0.02910(17) Uani 1 1 d . . . Fe2 Fe 0.28528(2) 0.35729(2) 0.10394(7) 0.02905(17) Uani 1 1 d . . . S1 S 0.27921(4) 0.27635(4) 0.03456(13) 0.0322(3) Uani 1 1 d . . . S2 S 0.36578(4) 0.34857(4) 0.03272(12) 0.0307(3) Uani 1 1 d . . . O1 O 0.36033(14) 0.26401(14) -0.3787(4) 0.0585(10) Uani 1 1 d . . . O2 O 0.33561(15) 0.42157(14) -0.2943(4) 0.0585(10) Uani 1 1 d . . . O3 O 0.21252(12) 0.32561(13) -0.2937(4) 0.0494(9) Uani 1 1 d . . . O4 O 0.29905(14) 0.46590(13) 0.0679(4) 0.0538(10) Uani 1 1 d . . . O5 O 0.17596(13) 0.36514(14) 0.0830(4) 0.0546(10) Uani 1 1 d . . . O6 O 0.29356(15) 0.34972(15) 0.4318(4) 0.0603(10) Uani 1 1 d . . . N N 0.4414(2) 0.22552(18) -0.0599(6) 0.0660(15) Uani 1 1 d . . . H1Y H 0.439(3) 0.258(3) -0.091(8) 0.099 Uiso 1 1 d . . . H1X H 0.466(2) 0.239(3) 0.034(8) 0.099 Uiso 1 1 d . . . C1 C 0.34221(18) 0.28710(17) -0.2863(5) 0.0377(11) Uani 1 1 d . . . C2 C 0.32599(18) 0.38461(19) -0.2382(5) 0.0405(11) Uani 1 1 d . . . C3 C 0.25062(18) 0.32532(16) -0.2378(5) 0.0353(10) Uani 1 1 d . . . C4 C 0.29315(17) 0.42355(18) 0.0812(5) 0.0365(11) Uani 1 1 d . . . C5 C 0.21863(19) 0.36213(17) 0.0894(5) 0.0363(10) Uani 1 1 d . . . C6 C 0.29023(17) 0.35301(17) 0.3051(5) 0.0384(11) Uani 1 1 d . . . C7 C 0.32277(18) 0.23784(17) 0.1444(6) 0.0417(11) Uani 1 1 d . . . H7B H 0.3143 0.2428 0.2517 0.05 Uiso 1 1 calc R . . H7A H 0.3153 0.2024 0.1205 0.05 Uiso 1 1 calc R . . C8 C 0.37882(18) 0.24461(16) 0.1294(5) 0.0371(11) Uani 1 1 d . . . C9 C 0.39529(17) 0.29912(18) 0.1426(6) 0.0416(11) Uani 1 1 d . . . H9B H 0.4315 0.3001 0.1192 0.05 Uiso 1 1 calc R . . H9A H 0.3918 0.3086 0.2497 0.05 Uiso 1 1 calc R . . C10 C 0.4047(2) 0.21552(19) 0.2577(6) 0.0510(13) Uani 1 1 d . . . H10C H 0.3933 0.2287 0.3547 0.077 Uiso 1 1 calc R . . H10B H 0.441 0.2195 0.2494 0.077 Uiso 1 1 calc R . . H10A H 0.396 0.18 0.2503 0.077 Uiso 1 1 calc R . . C11 C 0.3940(2) 0.2207(2) -0.0196(6) 0.0625(17) Uani 1 1 d . . . H11B H 0.3861 0.1846 -0.0144 0.075 Uiso 1 1 calc R . . H11A H 0.3729 0.2354 -0.0999 0.075 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 0.0326(4) 0.0308(3) 0.0239(3) -0.0021(3) -0.0008(3) -0.0006(3) Fe2 0.0322(3) 0.0299(3) 0.0250(3) -0.0023(3) -0.0008(3) 0.0030(3) S1 0.0349(6) 0.0296(6) 0.0320(6) -0.0003(5) -0.0009(5) -0.0025(5) S2 0.0304(6) 0.0309(6) 0.0307(6) -0.0026(5) -0.0029(5) -0.0004(4) O1 0.072(3) 0.063(2) 0.041(2) -0.0110(19) 0.0127(19) 0.015(2) O2 0.074(3) 0.047(2) 0.054(2) 0.0163(19) -0.007(2) -0.011(2) O3 0.0367(19) 0.065(2) 0.047(2) -0.0100(18) -0.0110(16) 0.0049(17) O4 0.067(3) 0.033(2) 0.062(2) -0.0051(17) -0.0152(19) 0.0024(17) O5 0.037(2) 0.066(2) 0.061(2) 0.0171(19) -0.0001(18) 0.0096(18) O6 0.076(3) 0.076(3) 0.029(2) 0.0009(18) -0.0019(18) -0.003(2) N 0.075(4) 0.040(3) 0.083(4) 0.011(3) 0.035(3) 0.013(3) C1 0.043(3) 0.038(3) 0.031(2) 0.001(2) 0.001(2) 0.001(2) C2 0.044(3) 0.045(3) 0.033(3) 0.000(2) -0.008(2) -0.004(2) C3 0.045(3) 0.034(2) 0.028(2) -0.0034(19) 0.000(2) 0.001(2) C4 0.036(3) 0.043(3) 0.031(2) -0.006(2) -0.007(2) 0.006(2) C5 0.046(3) 0.036(3) 0.027(2) 0.005(2) 0.001(2) 0.006(2) C6 0.039(3) 0.040(3) 0.036(3) 0.000(2) 0.002(2) 0.003(2) C7 0.049(3) 0.034(3) 0.042(3) 0.006(2) -0.002(2) 0.003(2) C8 0.045(3) 0.030(2) 0.036(3) 0.002(2) 0.002(2) 0.012(2) C9 0.032(2) 0.048(3) 0.046(3) -0.003(2) -0.008(2) 0.006(2) C10 0.057(3) 0.049(3) 0.048(3) 0.009(2) -0.007(3) 0.010(3) C11 0.088(5) 0.058(4) 0.042(3) 0.003(3) 0.012(3) 0.032(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 1.802(5) . ? Fe1 C2 1.803(5) . ? Fe1 C3 1.804(5) . ? Fe1 S2 2.2578(12) . ? Fe1 S1 2.2683(12) . ? Fe1 Fe2 2.4992(8) . ? Fe2 C5 1.790(5) . ? Fe2 C4 1.794(5) . ? Fe2 C6 1.798(5) . ? Fe2 S2 2.2539(12) . ? Fe2 S1 2.2547(12) . ? S1 C7 1.835(5) . ? S2 C9 1.823(5) . ? O1 C1 1.136(5) . ? O2 C2 1.136(5) . ? O3 C3 1.133(5) . ? O4 C4 1.148(5) . ? O5 C5 1.144(5) . ? O6 C6 1.134(6) . ? N C11 1.323(7) . ? N H1Y 0.91(7) . ? N H1X 1.13(7) . ? C7 C8 1.514(6) . ? C7 H7B 0.99 . ? C7 H7A 0.99 . ? C8 C9 1.526(6) . ? C8 C11 1.526(7) . ? C8 C10 1.544(6) . ? C9 H9B 0.99 . ? C9 H9A 0.99 . ? C10 H10C 0.98 . ? C10 H10B 0.98 . ? C10 H10A 0.98 . ? C11 H11B 0.99 . ? C11 H11A 0.99 . ? 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 C1 Fe1 C2 95.8(2) . . ? C1 Fe1 C3 96.3(2) . . ? C2 Fe1 C3 90.5(2) . . ? C1 Fe1 S2 110.12(15) . . ? C2 Fe1 S2 86.61(15) . . ? C3 Fe1 S2 153.58(14) . . ? C1 Fe1 S1 109.05(15) . . ? C2 Fe1 S1 155.10(16) . . ? C3 Fe1 S1 88.39(15) . . ? S2 Fe1 S1 83.43(4) . . ? C1 Fe1 Fe2 158.56(15) . . ? C2 Fe1 Fe2 99.48(15) . . ? C3 Fe1 Fe2 98.51(14) . . ? S2 Fe1 Fe2 56.29(3) . . ? S1 Fe1 Fe2 56.20(3) . . ? C5 Fe2 C4 92.1(2) . . ? C5 Fe2 C6 98.6(2) . . ? C4 Fe2 C6 99.6(2) . . ? C5 Fe2 S2 159.43(15) . . ? C4 Fe2 S2 87.63(15) . . ? C6 Fe2 S2 101.72(15) . . ? C5 Fe2 S1 88.74(15) . . ? C4 Fe2 S1 157.51(15) . . ? C6 Fe2 S1 102.52(15) . . ? S2 Fe2 S1 83.83(4) . . ? C5 Fe2 Fe1 103.63(14) . . ? C4 Fe2 Fe1 101.41(15) . . ? C6 Fe2 Fe1 148.63(15) . . ? S2 Fe2 Fe1 56.44(3) . . ? S1 Fe2 Fe1 56.72(3) . . ? C7 S1 Fe2 110.26(16) . . ? C7 S1 Fe1 118.05(16) . . ? Fe2 S1 Fe1 67.09(4) . . ? C9 S2 Fe2 109.68(16) . . ? C9 S2 Fe1 117.89(16) . . ? Fe2 S2 Fe1 67.28(4) . . ? C11 N H1Y 96(4) . . ? C11 N H1X 113(3) . . ? H1Y N H1X 87(5) . . ? O1 C1 Fe1 176.3(4) . . ? O2 C2 Fe1 179.5(5) . . ? O3 C3 Fe1 179.2(4) . . ? O4 C4 Fe2 178.7(4) . . ? O5 C5 Fe2 178.7(4) . . ? O6 C6 Fe2 179.2(5) . . ? C8 C7 S1 120.9(3) . . ? C8 C7 H7B 107.1 . . ? S1 C7 H7B 107.1 . . ? C8 C7 H7A 107.1 . . ? S1 C7 H7A 107.1 . . ? H7B C7 H7A 106.8 . . ? C7 C8 C9 113.1(4) . . ? C7 C8 C11 106.8(4) . . ? C9 C8 C11 112.9(4) . . ? C7 C8 C10 108.5(4) . . ? C9 C8 C10 107.1(4) . . ? C11 C8 C10 108.3(4) . . ? C8 C9 S2 121.7(3) . . ? C8 C9 H9B 106.9 . . ? S2 C9 H9B 106.9 . . ? C8 C9 H9A 106.9 . . ? S2 C9 H9A 106.9 . . ? H9B C9 H9A 106.7 . . ? C8 C10 H10C 109.5 . . ? C8 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? C8 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? N C11 C8 116.7(6) . . ? N C11 H11B 108.1 . . ? C8 C11 H11B 108.1 . . ? N C11 H11A 108.1 . . ? C8 C11 H11A 108.1 . . ? H11B C11 H11A 107.3 . . ? #===END data_1x _database_code_depnum_ccdc_archive 'CCDC 658091' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound A, X=2-pyridine' _chemical_melting_point ? _chemical_formula_structural 'Fe2 (CO)5 {MeC(CH2S)2-Py}]' _chemical_formula_moiety 'C14 H11 Fe2 N O5 S2 ' _chemical_formula_sum 'C14 H11 Fe2 N O5 S2' _chemical_formula_weight 449.06 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 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5512(6) _cell_length_b 11.9757(8) _cell_length_c 14.9165(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.1280(10) _cell_angle_gamma 90.00 _cell_volume 1703.64(19) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.22 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.971 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5114 _exptl_absorpt_correction_T_max 0.7964 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11353 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.70 _reflns_number_total 3517 _reflns_number_gt 3033 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _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 'SHELXP-97 (Sheldrick, 1990)' _computing_publication_material 'SHELXP-97 (Sheldrick, 1990)' _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^)+(0.0340P)^2^+0.1723P] 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 3517 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0575 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _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 -0.03814(2) 0.197035(18) 0.199020(14) 0.03411(7) Uani 1 1 d . . . Fe2 Fe 0.04438(3) 0.076699(19) 0.331160(16) 0.04002(8) Uani 1 1 d . . . S1 S 0.18191(4) 0.19951(3) 0.26177(3) 0.03966(10) Uani 1 1 d . . . S2 S -0.01979(4) 0.01021(3) 0.19339(3) 0.04218(11) Uani 1 1 d . . . C1 C 0.13791(17) 0.16640(13) 0.04120(11) 0.0393(4) Uani 1 1 d . . . C2 C 0.1782(2) 0.19261(16) -0.04500(12) 0.0522(5) Uani 1 1 d . . . H2 H 0.2549 0.1565 -0.0677 0.063 Uiso 1 1 calc R . . C3 C 0.1066(2) 0.27053(18) -0.09646(13) 0.0615(5) Uani 1 1 d . . . H3 H 0.1340 0.2873 -0.1538 0.074 Uiso 1 1 calc R . . C4 C -0.0055(2) 0.32323(18) -0.06265(13) 0.0597(5) Uani 1 1 d . . . H4 H -0.0556 0.3768 -0.0962 0.072 Uiso 1 1 calc R . . C5 C -0.0424(2) 0.29542(15) 0.02188(12) 0.0489(4) Uani 1 1 d . . . H5 H -0.1196 0.3309 0.0444 0.059 Uiso 1 1 calc R . . C6 C 0.22017(18) 0.07976(14) 0.09895(12) 0.0439(4) Uani 1 1 d . . . C7 C 0.3385(2) 0.02656(18) 0.04676(15) 0.0659(6) Uani 1 1 d . . . H7A H 0.4033 0.0835 0.0306 0.099 Uiso 1 1 calc R . . H7B H 0.2989 -0.0087 -0.0066 0.099 Uiso 1 1 calc R . . H7C H 0.3869 -0.0282 0.0839 0.099 Uiso 1 1 calc R . . C8 C 0.12755(19) -0.01838(14) 0.12582(12) 0.0478(4) Uani 1 1 d . . . H8A H 0.1874 -0.0720 0.1581 0.057 Uiso 1 1 calc R . . H8B H 0.0917 -0.0545 0.0711 0.057 Uiso 1 1 calc R . . C9 C 0.29314(17) 0.13360(15) 0.18228(12) 0.0479(4) Uani 1 1 d . . . H9A H 0.3581 0.1894 0.1622 0.057 Uiso 1 1 calc R . . H9B H 0.3482 0.0765 0.2140 0.057 Uiso 1 1 calc R . . C10 C -0.22144(19) 0.18386(15) 0.18061(11) 0.0460(4) Uani 1 1 d . . . C11 C -0.0599(2) 0.33354(16) 0.24045(13) 0.0523(4) Uani 1 1 d . . . C12 C -0.1121(2) 0.01501(17) 0.36864(13) 0.0564(5) Uani 1 1 d . . . C13 C 0.1705(2) -0.02464(16) 0.37300(13) 0.0575(5) Uani 1 1 d . . . C14 C 0.0488(2) 0.17295(16) 0.42281(13) 0.0539(5) Uani 1 1 d . . . O1 O -0.34124(14) 0.17679(15) 0.17109(10) 0.0738(4) Uani 1 1 d . . . O2 O -0.0753(2) 0.42029(13) 0.27068(13) 0.0944(6) Uani 1 1 d . . . O3 O -0.21167(19) -0.02371(16) 0.39355(12) 0.0888(5) Uani 1 1 d . . . O4 O 0.2509(2) -0.08709(15) 0.39911(14) 0.0997(6) Uani 1 1 d . . . O5 O 0.0507(2) 0.23459(15) 0.48061(12) 0.0911(5) Uani 1 1 d . . . N1 N 0.02692(14) 0.21934(10) 0.07439(9) 0.0372(3) 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 Fe1 0.03084(13) 0.03794(13) 0.03354(13) -0.00364(9) 0.00174(9) 0.00176(9) Fe2 0.04477(15) 0.03777(13) 0.03723(14) 0.00073(9) -0.00032(10) -0.00022(10) S1 0.0351(2) 0.0390(2) 0.0443(2) -0.00333(16) -0.00400(17) -0.00283(16) S2 0.0452(2) 0.0376(2) 0.0439(2) -0.00622(17) 0.00427(18) -0.00763(17) C1 0.0341(9) 0.0424(8) 0.0421(9) -0.0071(7) 0.0068(7) -0.0047(7) C2 0.0478(11) 0.0638(11) 0.0465(10) -0.0090(9) 0.0152(8) -0.0062(9) C3 0.0734(14) 0.0752(13) 0.0367(10) 0.0045(9) 0.0097(9) -0.0117(12) C4 0.0634(13) 0.0696(12) 0.0457(11) 0.0118(9) -0.0018(9) 0.0035(10) C5 0.0475(11) 0.0548(10) 0.0443(10) 0.0032(8) 0.0011(8) 0.0079(8) C6 0.0359(9) 0.0441(8) 0.0525(10) -0.0062(7) 0.0095(7) 0.0048(7) C7 0.0530(12) 0.0684(13) 0.0785(15) -0.0075(11) 0.0234(10) 0.0184(11) C8 0.0531(11) 0.0378(8) 0.0530(11) -0.0088(8) 0.0077(8) 0.0032(8) C9 0.0313(9) 0.0537(10) 0.0584(11) -0.0017(8) 0.0007(8) 0.0045(8) C10 0.0408(10) 0.0611(11) 0.0363(9) -0.0007(8) 0.0039(7) 0.0007(8) C11 0.0489(11) 0.0530(10) 0.0539(11) -0.0101(9) -0.0065(8) 0.0100(9) C12 0.0659(13) 0.0579(11) 0.0454(10) 0.0028(9) 0.0041(9) -0.0124(10) C13 0.0707(13) 0.0486(10) 0.0523(11) -0.0006(9) -0.0027(9) 0.0071(10) C14 0.0611(12) 0.0524(10) 0.0480(11) -0.0014(9) 0.0012(9) 0.0026(9) O1 0.0344(8) 0.1162(13) 0.0706(10) 0.0050(9) 0.0013(6) -0.0036(8) O2 0.1015(14) 0.0634(10) 0.1155(16) -0.0421(9) -0.0206(12) 0.0271(9) O3 0.0826(12) 0.1056(13) 0.0802(11) 0.0041(10) 0.0221(9) -0.0365(11) O4 0.1145(15) 0.0811(11) 0.1007(15) 0.0067(10) -0.0206(12) 0.0488(11) O5 0.1239(16) 0.0821(11) 0.0665(11) -0.0323(9) -0.0012(10) 0.0071(11) N1 0.0347(7) 0.0408(7) 0.0362(7) -0.0023(6) 0.0016(5) -0.0004(6) _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 C11 1.7639(18) . ? Fe1 C10 1.7643(18) . ? Fe1 N1 2.0099(14) . ? Fe1 S2 2.2461(5) . ? Fe1 S1 2.2538(5) . ? Fe1 Fe2 2.5325(3) . ? Fe2 C12 1.784(2) . ? Fe2 C14 1.787(2) . ? Fe2 C13 1.798(2) . ? Fe2 S2 2.2572(5) . ? Fe2 S1 2.2602(5) . ? S1 C9 1.8152(18) . ? S2 C8 1.8079(18) . ? C1 N1 1.352(2) . ? C1 C2 1.398(2) . ? C1 C6 1.537(2) . ? C2 C3 1.368(3) . ? C2 H2 0.9300 . ? C3 C4 1.363(3) . ? C3 H3 0.9300 . ? C4 C5 1.369(3) . ? C4 H4 0.9300 . ? C5 N1 1.351(2) . ? C5 H5 0.9300 . ? C6 C9 1.534(2) . ? C6 C8 1.537(2) . ? C6 C7 1.545(2) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O1 1.148(2) . ? C11 O2 1.145(2) . ? C12 O3 1.139(2) . ? C13 O4 1.126(2) . ? C14 O5 1.135(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Fe1 C10 90.15(9) . . ? C11 Fe1 N1 104.42(8) . . ? C10 Fe1 N1 102.83(7) . . ? C11 Fe1 S2 161.29(7) . . ? C10 Fe1 S2 89.08(6) . . ? N1 Fe1 S2 93.96(4) . . ? C11 Fe1 S1 88.12(6) . . ? C10 Fe1 S1 163.89(6) . . ? N1 Fe1 S1 93.10(4) . . ? S2 Fe1 S1 87.463(16) . . ? C11 Fe1 Fe2 106.99(6) . . ? C10 Fe1 Fe2 109.53(6) . . ? N1 Fe1 Fe2 134.17(4) . . ? S2 Fe1 Fe2 55.990(13) . . ? S1 Fe1 Fe2 55.991(13) . . ? C12 Fe2 C14 90.73(9) . . ? C12 Fe2 C13 99.70(10) . . ? C14 Fe2 C13 100.51(9) . . ? C12 Fe2 S2 87.06(6) . . ? C14 Fe2 S2 156.63(6) . . ? C13 Fe2 S2 102.80(6) . . ? C12 Fe2 S1 158.54(7) . . ? C14 Fe2 S1 86.58(7) . . ? C13 Fe2 S1 101.72(7) . . ? S2 Fe2 S1 87.040(18) . . ? C12 Fe2 Fe1 104.42(6) . . ? C14 Fe2 Fe1 102.82(6) . . ? C13 Fe2 Fe1 145.95(7) . . ? S2 Fe2 Fe1 55.573(13) . . ? S1 Fe2 Fe1 55.754(13) . . ? C9 S1 Fe1 106.78(6) . . ? C9 S1 Fe2 113.06(6) . . ? Fe1 S1 Fe2 68.255(14) . . ? C8 S2 Fe1 105.91(6) . . ? C8 S2 Fe2 113.17(6) . . ? Fe1 S2 Fe2 68.438(14) . . ? N1 C1 C2 119.48(16) . . ? N1 C1 C6 119.90(15) . . ? C2 C1 C6 120.61(15) . . ? C3 C2 C1 121.01(18) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 119.15(18) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 118.39(19) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 123.72(18) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C9 C6 C1 111.49(13) . . ? C9 C6 C8 110.65(15) . . ? C1 C6 C8 112.23(14) . . ? C9 C6 C7 105.62(15) . . ? C1 C6 C7 111.20(16) . . ? C8 C6 C7 105.27(14) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 S2 118.50(11) . . ? C6 C8 H8A 107.7 . . ? S2 C8 H8A 107.7 . . ? C6 C8 H8B 107.7 . . ? S2 C8 H8B 107.7 . . ? H8A C8 H8B 107.1 . . ? C6 C9 S1 117.13(12) . . ? C6 C9 H9A 108.0 . . ? S1 C9 H9A 108.0 . . ? C6 C9 H9B 108.0 . . ? S1 C9 H9B 108.0 . . ? H9A C9 H9B 107.3 . . ? O1 C10 Fe1 177.93(17) . . ? O2 C11 Fe1 177.2(2) . . ? O3 C12 Fe2 179.1(2) . . ? O4 C13 Fe2 179.1(2) . . ? O5 C14 Fe2 179.4(2) . . ? C5 N1 C1 118.25(15) . . ? C5 N1 Fe1 117.34(12) . . ? C1 N1 Fe1 124.36(11) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.70 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.275 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.043 #===END data_70122am _database_code_depnum_ccdc_archive 'CCDC 658092' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound C, X=2-pyridinium' _chemical_melting_point ? _chemical_formula_structural '[Fe2 (CO)6 {MeC(CH2S)2-PyH}].BF4' _chemical_formula_moiety 'C15 H12 Fe2 N O6 S2, B F4 ' _chemical_formula_sum 'C15 H12 B F4 Fe2 N O6 S2' _chemical_formula_weight 564.89 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 21/c' 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 14.5080(4) _cell_length_b 11.7408(3) _cell_length_c 13.0329(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.12 _cell_angle_gamma 90.00 _cell_volume 2109.86(10) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.16 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6566 _exptl_absorpt_correction_T_max 0.7142 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15591 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.24 _reflns_number_total 5108 _reflns_number_gt 4168 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _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 'SHELXP-97 (Sheldrick, 1990)' _computing_publication_material 'SHELXP-97 (Sheldrick, 1990)' _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^)+(0.0455P)^2^+0.1447P] 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 5108 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _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 0.105872(17) 0.77899(2) 0.463179(19) 0.03173(8) Uani 1 1 d . . . Fe2 Fe 0.158074(18) 0.58619(2) 0.42167(2) 0.03433(8) Uani 1 1 d . . . S1 S 0.17539(3) 0.74494(4) 0.33139(3) 0.03375(11) Uani 1 1 d . . . S2 S 0.23769(3) 0.68816(4) 0.56950(3) 0.03366(11) Uani 1 1 d . . . C1 C 0.32557(12) 0.94358(16) 0.48637(14) 0.0354(4) Uani 1 1 d . . . N1 N 0.35278(11) 0.99136(15) 0.58582(13) 0.0417(4) Uani 1 1 d . . . H1 H 0.3819 0.9489 0.6400 0.050 Uiso 1 1 calc R . . C2 C 0.33724(16) 1.1011(2) 0.6054(2) 0.0527(5) Uani 1 1 d . . . H2 H 0.3579 1.1289 0.6757 0.063 Uiso 1 1 calc R . . C3 C 0.29140(17) 1.1712(2) 0.5224(2) 0.0617(6) Uani 1 1 d . . . H3 H 0.2799 1.2471 0.5348 0.074 Uiso 1 1 calc R . . C4 C 0.26243(18) 1.1275(2) 0.4197(2) 0.0642(7) Uani 1 1 d . . . H4 H 0.2313 1.1743 0.3616 0.077 Uiso 1 1 calc R . . C5 C 0.27916(15) 1.01407(19) 0.40169(17) 0.0488(5) Uani 1 1 d . . . H5 H 0.2588 0.9853 0.3317 0.059 Uiso 1 1 calc R . . C6 C 0.35904(12) 0.82305(16) 0.47491(14) 0.0335(4) Uani 1 1 d . . . C7 C 0.46740(13) 0.83236(19) 0.48183(17) 0.0467(5) Uani 1 1 d . . . H7A H 0.4740 0.8842 0.4275 0.070 Uiso 1 1 calc R . . H7B H 0.4911 0.7587 0.4703 0.070 Uiso 1 1 calc R . . H7C H 0.5042 0.8600 0.5519 0.070 Uiso 1 1 calc R . . C8 C 0.30559(13) 0.77235(17) 0.36434(15) 0.0378(4) Uani 1 1 d . . . H8A H 0.3369 0.7009 0.3578 0.045 Uiso 1 1 calc R . . H8B H 0.3149 0.8233 0.3098 0.045 Uiso 1 1 calc R . . C9 C 0.35454(13) 0.74017(17) 0.56402(14) 0.0359(4) Uani 1 1 d . . . H9A H 0.3867 0.7766 0.6326 0.043 Uiso 1 1 calc R . . H9B H 0.3932 0.6741 0.5592 0.043 Uiso 1 1 calc R . . C10 C -0.00883(14) 0.79481(16) 0.35846(15) 0.0378(4) Uani 1 1 d . . . C11 C 0.04059(14) 0.7349(2) 0.55234(16) 0.0451(5) Uani 1 1 d . . . C12 C 0.11728(14) 0.92478(19) 0.50813(19) 0.0486(5) Uani 1 1 d . . . C13 C 0.05064(15) 0.55151(18) 0.31322(17) 0.0453(5) Uani 1 1 d . . . C14 C 0.13502(15) 0.48873(19) 0.51624(18) 0.0486(5) Uani 1 1 d . . . C15 C 0.24226(16) 0.4967(2) 0.38222(17) 0.0480(5) Uani 1 1 d . . . O1 O -0.08260(10) 0.80155(14) 0.29484(12) 0.0540(4) Uani 1 1 d . . . O2 O -0.00393(13) 0.70841(18) 0.60558(13) 0.0737(6) Uani 1 1 d . . . O3 O 0.11789(13) 1.01459(16) 0.54001(19) 0.0830(6) Uani 1 1 d . . . O4 O -0.01812(12) 0.53318(15) 0.24378(13) 0.0673(5) Uani 1 1 d . . . O5 O 0.12610(14) 0.42903(17) 0.58154(15) 0.0781(6) Uani 1 1 d . . . O6 O 0.29256(14) 0.44117(18) 0.35201(15) 0.0791(6) Uani 1 1 d . . . B1 B 0.4362(2) 0.0746(3) 0.1945(2) 0.0608(7) Uani 1 1 d . . . F1 F 0.43034(15) -0.02216(17) 0.24927(16) 0.1092(7) Uani 1 1 d . . . F2 F 0.39673(15) 0.06529(18) 0.08785(13) 0.1094(7) Uani 1 1 d . . . F3 F 0.53359(13) 0.10292(17) 0.22184(13) 0.0932(6) Uani 1 1 d . . . F4 F 0.3921(2) 0.1619(2) 0.2325(2) 0.1493(10) 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 Fe1 0.02850(13) 0.03638(15) 0.03061(14) -0.00288(10) 0.00965(10) -0.00383(10) Fe2 0.03346(14) 0.03357(15) 0.03425(14) -0.00374(10) 0.00801(11) -0.00547(11) S1 0.0310(2) 0.0433(3) 0.0256(2) -0.00067(17) 0.00680(17) -0.00368(19) S2 0.0334(2) 0.0402(3) 0.0262(2) 0.00153(16) 0.00754(17) -0.00519(19) C1 0.0268(8) 0.0396(10) 0.0402(9) -0.0001(8) 0.0110(7) -0.0074(8) N1 0.0374(8) 0.0435(10) 0.0435(9) -0.0017(7) 0.0114(7) -0.0066(7) C2 0.0457(12) 0.0486(13) 0.0655(14) -0.0155(11) 0.0195(11) -0.0112(10) C3 0.0535(13) 0.0402(13) 0.0911(19) -0.0029(12) 0.0218(13) -0.0047(11) C4 0.0578(14) 0.0470(14) 0.0825(18) 0.0195(12) 0.0141(13) 0.0035(11) C5 0.0477(11) 0.0467(12) 0.0481(11) 0.0068(9) 0.0091(9) -0.0029(10) C6 0.0277(8) 0.0388(10) 0.0337(9) 0.0011(7) 0.0092(7) -0.0042(7) C7 0.0289(9) 0.0575(13) 0.0547(12) -0.0002(10) 0.0143(9) -0.0062(9) C8 0.0324(9) 0.0485(11) 0.0346(9) -0.0013(8) 0.0134(8) -0.0048(8) C9 0.0281(8) 0.0403(10) 0.0344(9) 0.0034(7) 0.0024(7) -0.0036(8) C10 0.0383(10) 0.0383(10) 0.0394(10) -0.0011(8) 0.0156(8) -0.0007(8) C11 0.0354(10) 0.0648(14) 0.0342(10) -0.0051(9) 0.0098(8) -0.0110(9) C12 0.0330(10) 0.0506(13) 0.0667(14) -0.0146(10) 0.0220(10) -0.0069(9) C13 0.0459(11) 0.0371(11) 0.0498(11) -0.0079(9) 0.0107(10) -0.0045(9) C14 0.0456(11) 0.0456(12) 0.0522(12) -0.0016(10) 0.0116(9) -0.0124(10) C15 0.0483(11) 0.0475(12) 0.0450(11) -0.0052(9) 0.0097(9) -0.0021(10) O1 0.0369(7) 0.0693(11) 0.0490(8) 0.0032(7) 0.0039(7) 0.0029(7) O2 0.0615(11) 0.1204(17) 0.0456(9) -0.0074(9) 0.0260(8) -0.0326(11) O3 0.0607(10) 0.0585(12) 0.1434(18) -0.0486(12) 0.0515(11) -0.0168(9) O4 0.0545(9) 0.0631(11) 0.0655(11) -0.0185(8) -0.0086(8) -0.0075(8) O5 0.0897(14) 0.0723(13) 0.0718(12) 0.0177(9) 0.0247(10) -0.0297(11) O6 0.0771(12) 0.0860(14) 0.0768(12) -0.0180(10) 0.0277(10) 0.0225(11) B1 0.0693(18) 0.0549(17) 0.0474(14) 0.0092(11) 0.0026(13) -0.0078(14) F1 0.1166(15) 0.0932(14) 0.1004(14) 0.0408(11) 0.0087(11) -0.0306(12) F2 0.1199(15) 0.1245(17) 0.0519(9) 0.0037(9) -0.0193(9) -0.0309(13) F3 0.0859(12) 0.1217(15) 0.0581(9) 0.0100(9) 0.0022(8) -0.0394(11) F4 0.194(3) 0.134(2) 0.1244(19) 0.0221(16) 0.0556(18) 0.0724(19) _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 C11 1.789(2) . ? Fe1 C12 1.800(2) . ? Fe1 C10 1.804(2) . ? Fe1 S2 2.2509(5) . ? Fe1 S1 2.2814(5) . ? Fe1 Fe2 2.4990(4) . ? Fe2 C14 1.788(2) . ? Fe2 C13 1.795(2) . ? Fe2 C15 1.803(2) . ? Fe2 S2 2.2573(5) . ? Fe2 S1 2.2595(5) . ? S1 C8 1.8307(19) . ? S2 C9 1.8241(18) . ? C1 N1 1.354(2) . ? C1 C5 1.376(3) . ? C1 C6 1.518(3) . ? N1 C2 1.346(3) . ? N1 H1 0.8600 . ? C2 C3 1.358(3) . ? C2 H2 0.9300 . ? C3 C4 1.372(4) . ? C3 H3 0.9300 . ? C4 C5 1.386(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C8 1.529(2) . ? C6 C9 1.532(2) . ? C6 C7 1.550(2) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O1 1.134(2) . ? C11 O2 1.129(2) . ? C12 O3 1.132(3) . ? C13 O4 1.140(2) . ? C14 O5 1.141(3) . ? C15 O6 1.136(3) . ? B1 F2 1.333(3) . ? B1 F1 1.358(3) . ? B1 F4 1.379(4) . ? B1 F3 1.387(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Fe1 C12 94.43(10) . . ? C11 Fe1 C10 88.34(9) . . ? C12 Fe1 C10 96.78(9) . . ? C11 Fe1 S2 89.04(7) . . ? C12 Fe1 S2 106.00(7) . . ? C10 Fe1 S2 157.20(6) . . ? C11 Fe1 S1 152.35(7) . . ? C12 Fe1 S1 113.22(7) . . ? C10 Fe1 S1 88.18(6) . . ? S2 Fe1 S1 83.717(18) . . ? C11 Fe1 Fe2 97.82(7) . . ? C12 Fe1 Fe2 158.19(6) . . ? C10 Fe1 Fe2 101.53(6) . . ? S2 Fe1 Fe2 56.458(14) . . ? S1 Fe1 Fe2 56.191(15) . . ? C14 Fe2 C13 95.44(10) . . ? C14 Fe2 C15 96.44(10) . . ? C13 Fe2 C15 98.20(9) . . ? C14 Fe2 S2 84.65(7) . . ? C13 Fe2 S2 151.74(7) . . ? C15 Fe2 S2 109.89(7) . . ? C14 Fe2 S1 164.12(8) . . ? C13 Fe2 S1 89.26(7) . . ? C15 Fe2 S1 97.89(7) . . ? S2 Fe2 S1 84.072(18) . . ? C14 Fe2 Fe1 107.23(7) . . ? C13 Fe2 Fe1 97.39(7) . . ? C15 Fe2 Fe1 150.15(7) . . ? S2 Fe2 Fe1 56.212(14) . . ? S1 Fe2 Fe1 57.031(14) . . ? C8 S1 Fe2 107.25(7) . . ? C8 S1 Fe1 117.26(6) . . ? Fe2 S1 Fe1 66.778(15) . . ? C9 S2 Fe1 116.06(6) . . ? C9 S2 Fe2 112.28(6) . . ? Fe1 S2 Fe2 67.330(15) . . ? N1 C1 C5 116.29(19) . . ? N1 C1 C6 118.26(16) . . ? C5 C1 C6 124.97(18) . . ? C2 N1 C1 124.21(19) . . ? C2 N1 H1 117.9 . . ? C1 N1 H1 117.9 . . ? N1 C2 C3 119.9(2) . . ? N1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 118.5(2) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C3 C4 C5 120.5(2) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C1 C5 C4 120.6(2) . . ? C1 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C1 C6 C8 111.82(15) . . ? C1 C6 C9 115.28(15) . . ? C8 C6 C9 109.78(15) . . ? C1 C6 C7 106.15(15) . . ? C8 C6 C7 106.87(15) . . ? C9 C6 C7 106.39(15) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 S1 118.26(12) . . ? C6 C8 H8A 107.7 . . ? S1 C8 H8A 107.7 . . ? C6 C8 H8B 107.7 . . ? S1 C8 H8B 107.7 . . ? H8A C8 H8B 107.1 . . ? C6 C9 S2 120.10(12) . . ? C6 C9 H9A 107.3 . . ? S2 C9 H9A 107.3 . . ? C6 C9 H9B 107.3 . . ? S2 C9 H9B 107.3 . . ? H9A C9 H9B 106.9 . . ? O1 C10 Fe1 177.11(18) . . ? O2 C11 Fe1 177.3(2) . . ? O3 C12 Fe1 173.89(19) . . ? O4 C13 Fe2 177.8(2) . . ? O5 C14 Fe2 175.3(2) . . ? O6 C15 Fe2 176.5(2) . . ? F2 B1 F1 113.8(2) . . ? F2 B1 F4 109.8(3) . . ? F1 B1 F4 108.8(3) . . ? F2 B1 F3 111.1(3) . . ? F1 B1 F3 106.9(2) . . ? F4 B1 F3 106.2(3) . . ? 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 N1 H1 F3 0.86 1.93 2.767(2) 162.4 3_666 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.388 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.055 #===END data_apr1505a _database_code_depnum_ccdc_archive 'CCDC 658093' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound B, X=CH2OH' _chemical_formula_moiety 'C11 H10 Fe2 O7 S2' _chemical_formula_sum 'C11 H10 Fe2 O7 S2' _chemical_formula_weight 430.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/a _symmetry_space_group_name_Hall 'I 4bw -1bw' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, -z+1/4' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, y, -z+3/4' 'y+1/2, -x+1/2, -z+1/2' 'y+1/2, -x, z+3/4' '-y, x+1/2, z+1/4' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, -z+3/4' '-x+1, -y+1, z+1' 'x+1, y+1/2, -z+5/4' 'y+1, -x+1, -z+1' 'y+1, -x+1/2, z+5/4' '-y+1/2, x+1, z+3/4' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 26.6984(14) _cell_length_b 26.6984(14) _cell_length_c 8.9118(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6352.4(6) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 138472 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 22.986 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 2.117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.586 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details 'r.h. blessing, acta cryst. (1995), a51, 33-38' _exptl_special_details ; ? ; _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.185923E-1 _diffrn_orient_matrix_ub_12 -0.22189E-2 _diffrn_orient_matrix_ub_13 0.971835E-1 _diffrn_orient_matrix_ub_21 -0.323001E-1 _diffrn_orient_matrix_ub_22 -0.30305E-2 _diffrn_orient_matrix_ub_23 -0.560814E-1 _diffrn_orient_matrix_ub_31 0.37336E-2 _diffrn_orient_matrix_ub_32 -0.372666E-1 _diffrn_orient_matrix_ub_33 -0.12259E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_number 31557 _diffrn_reflns_av_R_equivalents 0.1901 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 22.92 _reflns_number_total 2194 _reflns_number_gt 1745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0003P)^2^+112.8422P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 10(10) _refine_ls_number_reflns 2194 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1502 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.217 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.57590(5) 0.31151(5) 0.52391(15) 0.0393(4) Uani 1 1 d . . . Fe2 Fe 0.60728(5) 0.28529(5) 0.27131(15) 0.0396(4) Uani 1 1 d . . . S1 S 0.52620(9) 0.27936(10) 0.3410(3) 0.0427(7) Uani 1 1 d . . . S2 S 0.59907(9) 0.36580(9) 0.3427(3) 0.0414(6) Uani 1 1 d . . . O1 O 0.5136(3) 0.3602(3) 0.7554(9) 0.070(2) Uani 1 1 d . . . O2 O 0.6716(3) 0.3360(3) 0.6704(9) 0.071(2) Uani 1 1 d . . . O3 O 0.5757(3) 0.2127(3) 0.6689(9) 0.059(2) Uani 1 1 d . . . O4 O 0.7161(3) 0.2992(3) 0.3087(9) 0.065(2) Uani 1 1 d . . . O5 O 0.6148(3) 0.1758(3) 0.2917(9) 0.063(2) Uani 1 1 d . . . O6 O 0.5995(3) 0.2932(3) -0.0554(9) 0.071(2) Uani 1 1 d . . . O7 O 0.4771(4) 0.4435(5) 0.4290(14) 0.092(4) Uani 0.77 1 d P . . O7A O 0.4768(17) 0.4636(17) 0.127(5) 0.105(14) Uiso 0.23 1 d P A 2 C1 C 0.5366(4) 0.3425(4) 0.6613(12) 0.049(3) Uani 1 1 d . . . C2 C 0.6346(5) 0.3262(4) 0.6130(11) 0.049(3) Uani 1 1 d . . . C3 C 0.5749(3) 0.2513(4) 0.6133(11) 0.044(3) Uani 1 1 d . . . C4 C 0.6739(4) 0.2926(4) 0.2956(12) 0.047(3) Uani 1 1 d . . . C5 C 0.6121(4) 0.2191(5) 0.2855(11) 0.046(3) Uani 1 1 d . . . C6 C 0.6030(4) 0.2902(4) 0.0727(14) 0.052(3) Uani 1 1 d . . . C7 C 0.4874(4) 0.3236(4) 0.2329(13) 0.058(3) Uani 1 1 d . B . H7B H 0.4914 0.3148 0.1257 0.070 Uiso 1 1 calc R . . H7A H 0.4521 0.3167 0.2592 0.070 Uiso 1 1 calc R . . C8 C 0.4948(4) 0.3795(4) 0.2455(11) 0.047(3) Uani 1 1 d . . . C9 C 0.5492(4) 0.3958(4) 0.2309(12) 0.052(3) Uani 1 1 d . B . H9B H 0.5504 0.4321 0.2535 0.063 Uiso 1 1 calc R . . H9A H 0.5585 0.3920 0.1240 0.063 Uiso 1 1 calc R . . C10 C 0.4659(4) 0.4045(4) 0.1160(13) 0.060(3) Uani 1 1 d . B 1 H10C H 0.4789 0.3924 0.0198 0.090 Uiso 1 1 calc R B 1 H10B H 0.4700 0.4409 0.1218 0.090 Uiso 1 1 calc R B 1 H10A H 0.4302 0.3961 0.1239 0.090 Uiso 1 1 calc R B 1 C11 C 0.4718(5) 0.3964(6) 0.3938(15) 0.083(4) Uani 1 1 d . B . H11B H 0.4356 0.3887 0.3910 0.099 Uiso 1 1 calc R . . H11A H 0.4867 0.3760 0.4752 0.099 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 0.0415(9) 0.0436(9) 0.0329(8) 0.0012(7) 0.0027(6) 0.0002(7) Fe2 0.0403(8) 0.0431(9) 0.0355(8) 0.0018(7) 0.0028(6) 0.0032(7) S1 0.0406(14) 0.0464(15) 0.0410(15) 0.0034(12) -0.0002(12) -0.0001(12) S2 0.0400(14) 0.0427(15) 0.0417(15) 0.0028(12) 0.0043(12) 0.0004(11) O1 0.077(6) 0.088(6) 0.046(5) -0.014(5) 0.011(4) 0.011(5) O2 0.057(5) 0.094(6) 0.061(6) 0.003(5) -0.017(4) -0.013(5) O3 0.070(5) 0.050(5) 0.058(5) 0.008(4) 0.002(4) 0.009(4) O4 0.035(4) 0.080(6) 0.080(6) 0.011(5) 0.000(4) -0.005(4) O5 0.079(6) 0.045(5) 0.067(6) 0.001(4) -0.012(4) 0.009(4) O6 0.090(6) 0.088(6) 0.034(5) -0.002(4) -0.004(4) 0.000(5) O7 0.064(7) 0.105(10) 0.107(10) -0.064(8) -0.017(7) 0.023(7) C1 0.058(7) 0.054(7) 0.035(6) 0.008(5) -0.007(6) -0.012(6) C2 0.072(8) 0.044(6) 0.031(6) 0.008(5) 0.004(6) 0.011(6) C3 0.033(6) 0.064(7) 0.034(6) -0.002(6) -0.006(5) 0.002(5) C4 0.062(8) 0.038(6) 0.042(7) 0.003(5) 0.000(6) 0.003(5) C5 0.039(6) 0.067(8) 0.033(6) 0.002(6) -0.008(5) 0.013(5) C6 0.044(6) 0.055(7) 0.057(8) -0.014(6) -0.001(6) 0.007(5) C7 0.048(7) 0.063(7) 0.063(8) 0.005(6) -0.003(6) 0.007(6) C8 0.051(6) 0.049(6) 0.040(6) -0.004(5) 0.007(5) 0.016(5) C9 0.063(7) 0.043(6) 0.050(7) 0.010(5) 0.003(6) 0.008(5) C10 0.061(8) 0.057(7) 0.062(8) 0.011(6) -0.011(6) 0.012(6) C11 0.069(9) 0.120(13) 0.059(9) -0.013(8) -0.001(7) 0.042(9) _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 C3 1.794(12) . ? Fe1 C2 1.800(13) . ? Fe1 C1 1.812(12) . ? Fe1 S2 2.256(3) . ? Fe1 S1 2.270(3) . ? Fe1 Fe2 2.5019(19) . ? Fe2 C5 1.776(12) . ? Fe2 C6 1.779(12) . ? Fe2 C4 1.802(12) . ? Fe2 S2 2.253(3) . ? Fe2 S1 2.258(3) . ? S1 C7 1.843(11) . ? S2 C9 1.846(10) . ? O1 C1 1.142(12) . ? O2 C2 1.142(12) . ? O3 C3 1.144(12) . ? O4 C4 1.146(12) . ? O5 C5 1.161(12) . ? O6 C6 1.148(12) . ? O7 C11 1.305(17) . ? C7 C8 1.510(14) . ? C7 H7B 0.9900 . ? C7 H7A 0.9900 . ? C8 C9 1.522(14) . ? C8 C11 1.525(15) . ? C8 C10 1.541(14) . ? C9 H9B 0.9900 . ? C9 H9A 0.9900 . ? C10 H10C 0.9800 . ? C10 H10B 0.9800 . ? C10 H10A 0.9800 . ? C11 H11B 0.9900 . ? C11 H11A 0.9900 . ? 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 C3 Fe1 C2 90.7(4) . . ? C3 Fe1 C1 95.7(4) . . ? C2 Fe1 C1 96.1(5) . . ? C3 Fe1 S2 153.8(3) . . ? C2 Fe1 S2 86.4(3) . . ? C1 Fe1 S2 110.4(3) . . ? C3 Fe1 S1 88.4(3) . . ? C2 Fe1 S1 155.2(3) . . ? C1 Fe1 S1 108.6(3) . . ? S2 Fe1 S1 83.65(10) . . ? C3 Fe1 Fe2 98.9(3) . . ? C2 Fe1 Fe2 99.6(3) . . ? C1 Fe1 Fe2 158.4(3) . . ? S2 Fe1 Fe2 56.22(8) . . ? S1 Fe1 Fe2 56.22(8) . . ? C5 Fe2 C6 98.5(5) . . ? C5 Fe2 C4 91.6(4) . . ? C6 Fe2 C4 100.1(5) . . ? C5 Fe2 S2 159.4(3) . . ? C6 Fe2 S2 101.8(4) . . ? C4 Fe2 S2 87.6(3) . . ? C5 Fe2 S1 88.9(3) . . ? C6 Fe2 S1 102.6(3) . . ? C4 Fe2 S1 157.0(3) . . ? S2 Fe2 S1 84.02(10) . . ? C5 Fe2 Fe1 103.8(3) . . ? C6 Fe2 Fe1 148.6(3) . . ? C4 Fe2 Fe1 101.1(3) . . ? S2 Fe2 Fe1 56.37(8) . . ? S1 Fe2 Fe1 56.69(8) . . ? C7 S1 Fe2 110.5(4) . . ? C7 S1 Fe1 117.5(4) . . ? Fe2 S1 Fe1 67.08(9) . . ? C9 S2 Fe2 109.4(4) . . ? C9 S2 Fe1 117.9(3) . . ? Fe2 S2 Fe1 67.41(9) . . ? O1 C1 Fe1 175.2(10) . . ? O2 C2 Fe1 179.1(10) . . ? O3 C3 Fe1 177.9(9) . . ? O4 C4 Fe2 177.2(9) . . ? O5 C5 Fe2 178.4(9) . . ? O6 C6 Fe2 179.0(10) . . ? C8 C7 S1 121.4(8) . . ? C8 C7 H7B 107.0 . . ? S1 C7 H7B 107.0 . . ? C8 C7 H7A 107.0 . . ? S1 C7 H7A 107.0 . . ? H7B C7 H7A 106.7 . . ? C7 C8 C9 113.7(8) . . ? C7 C8 C11 107.7(10) . . ? C9 C8 C11 111.9(10) . . ? C7 C8 C10 107.9(9) . . ? C9 C8 C10 106.9(8) . . ? C11 C8 C10 108.6(8) . . ? C8 C9 S2 121.2(7) . . ? C8 C9 H9B 107.0 . . ? S2 C9 H9B 107.0 . . ? C8 C9 H9A 107.0 . . ? S2 C9 H9A 107.0 . . ? H9B C9 H9A 106.8 . . ? C8 C10 H10C 109.5 . . ? C8 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? C8 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? O7 C11 C8 116.7(13) . . ? O7 C11 H11B 108.1 . . ? C8 C11 H11B 108.1 . . ? O7 C11 H11A 108.1 . . ? C8 C11 H11A 108.1 . . ? H11B C11 H11A 107.3 . . ? 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 C3 Fe1 Fe2 C5 2.7(4) . . . . ? C2 Fe1 Fe2 C5 94.9(4) . . . . ? C1 Fe1 Fe2 C5 -129.1(9) . . . . ? S2 Fe1 Fe2 C5 174.0(3) . . . . ? S1 Fe1 Fe2 C5 -79.3(3) . . . . ? C3 Fe1 Fe2 C6 136.8(7) . . . . ? C2 Fe1 Fe2 C6 -131.0(8) . . . . ? C1 Fe1 Fe2 C6 4.9(11) . . . . ? S2 Fe1 Fe2 C6 -51.9(7) . . . . ? S1 Fe1 Fe2 C6 54.8(7) . . . . ? C3 Fe1 Fe2 C4 -91.7(4) . . . . ? C2 Fe1 Fe2 C4 0.5(4) . . . . ? C1 Fe1 Fe2 C4 136.4(9) . . . . ? S2 Fe1 Fe2 C4 79.6(3) . . . . ? S1 Fe1 Fe2 C4 -173.7(3) . . . . ? C3 Fe1 Fe2 S2 -171.3(3) . . . . ? C2 Fe1 Fe2 S2 -79.1(3) . . . . ? C1 Fe1 Fe2 S2 56.9(9) . . . . ? S1 Fe1 Fe2 S2 106.69(12) . . . . ? C3 Fe1 Fe2 S1 82.0(3) . . . . ? C2 Fe1 Fe2 S1 174.2(3) . . . . ? C1 Fe1 Fe2 S1 -49.8(9) . . . . ? S2 Fe1 Fe2 S1 -106.69(12) . . . . ? C5 Fe2 S1 C7 -140.5(5) . . . . ? C6 Fe2 S1 C7 -42.0(5) . . . . ? C4 Fe2 S1 C7 128.1(9) . . . . ? S2 Fe2 S1 C7 58.8(4) . . . . ? Fe1 Fe2 S1 C7 112.1(4) . . . . ? C5 Fe2 S1 Fe1 107.4(3) . . . . ? C6 Fe2 S1 Fe1 -154.1(4) . . . . ? C4 Fe2 S1 Fe1 15.9(8) . . . . ? S2 Fe2 S1 Fe1 -53.31(9) . . . . ? C3 Fe1 S1 C7 156.2(5) . . . . ? C2 Fe1 S1 C7 -115.7(9) . . . . ? C1 Fe1 S1 C7 60.7(5) . . . . ? S2 Fe1 S1 C7 -48.8(4) . . . . ? Fe2 Fe1 S1 C7 -102.0(4) . . . . ? C3 Fe1 S1 Fe2 -101.8(3) . . . . ? C2 Fe1 S1 Fe2 -13.7(8) . . . . ? C1 Fe1 S1 Fe2 162.7(3) . . . . ? S2 Fe1 S1 Fe2 53.23(9) . . . . ? C5 Fe2 S2 C9 -129.8(10) . . . . ? C6 Fe2 S2 C9 42.2(5) . . . . ? C4 Fe2 S2 C9 142.0(5) . . . . ? S1 Fe2 S2 C9 -59.4(4) . . . . ? Fe1 Fe2 S2 C9 -113.0(4) . . . . ? C5 Fe2 S2 Fe1 -16.9(9) . . . . ? C6 Fe2 S2 Fe1 155.2(3) . . . . ? C4 Fe2 S2 Fe1 -105.0(3) . . . . ? S1 Fe2 S2 Fe1 53.60(9) . . . . ? C3 Fe1 S2 C9 120.6(8) . . . . ? C2 Fe1 S2 C9 -155.2(5) . . . . ? C1 Fe1 S2 C9 -60.0(5) . . . . ? S1 Fe1 S2 C9 47.5(4) . . . . ? Fe2 Fe1 S2 C9 100.8(4) . . . . ? C3 Fe1 S2 Fe2 19.8(7) . . . . ? C2 Fe1 S2 Fe2 104.0(3) . . . . ? C1 Fe1 S2 Fe2 -160.8(4) . . . . ? S1 Fe1 S2 Fe2 -53.23(9) . . . . ? C3 Fe1 C1 O1 40(12) . . . . ? C2 Fe1 C1 O1 -51(12) . . . . ? S2 Fe1 C1 O1 -139(12) . . . . ? S1 Fe1 C1 O1 131(12) . . . . ? Fe2 Fe1 C1 O1 173(11) . . . . ? C3 Fe1 C2 O2 -117(76) . . . . ? C1 Fe1 C2 O2 -21(76) . . . . ? S2 Fe1 C2 O2 89(76) . . . . ? S1 Fe1 C2 O2 155(100) . . . . ? Fe2 Fe1 C2 O2 144(76) . . . . ? C2 Fe1 C3 O3 -50(26) . . . . ? C1 Fe1 C3 O3 -146(26) . . . . ? S2 Fe1 C3 O3 33(27) . . . . ? S1 Fe1 C3 O3 105(26) . . . . ? Fe2 Fe1 C3 O3 50(26) . . . . ? C5 Fe2 C4 O4 161(21) . . . . ? C6 Fe2 C4 O4 62(21) . . . . ? S2 Fe2 C4 O4 -40(21) . . . . ? S1 Fe2 C4 O4 -108(20) . . . . ? Fe1 Fe2 C4 O4 -95(21) . . . . ? C6 Fe2 C5 O5 -24(38) . . . . ? C4 Fe2 C5 O5 -124(38) . . . . ? S2 Fe2 C5 O5 148(38) . . . . ? S1 Fe2 C5 O5 79(38) . . . . ? Fe1 Fe2 C5 O5 134(38) . . . . ? C5 Fe2 C6 O6 88(55) . . . . ? C4 Fe2 C6 O6 -178(100) . . . . ? S2 Fe2 C6 O6 -89(55) . . . . ? S1 Fe2 C6 O6 -2(55) . . . . ? Fe1 Fe2 C6 O6 -47(56) . . . . ? Fe2 S1 C7 C8 -63.5(9) . . . . ? Fe1 S1 C7 C8 10.6(10) . . . . ? S1 C7 C8 C9 48.5(12) . . . . ? S1 C7 C8 C11 -76.0(11) . . . . ? S1 C7 C8 C10 166.9(8) . . . . ? C7 C8 C9 S2 -50.0(12) . . . . ? C11 C8 C9 S2 72.2(11) . . . . ? C10 C8 C9 S2 -169.0(8) . . . . ? Fe2 S2 C9 C8 66.0(9) . . . . ? Fe1 S2 C9 C8 -8.1(10) . . . . ? C7 C8 C11 O7 176.1(11) . . . . ? C9 C8 C11 O7 50.5(14) . . . . ? C10 C8 C11 O7 -67.2(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.92 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.701 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.114