# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Christian Nather' 'Sina Sellmer' 'Mario Wriedt' _publ_contact_author_name 'Christian Nather' _publ_contact_author_email CNAETHER@AC.UNI-KIEL.DE _publ_section_title ; Coordination Polymer Changing its Magnetic Properties and Color by Thermal Decomposition: Synthesis, Structure and Properties of New Thiocyanato Iron(II) Coordination Polymers based on 4,4'-Bipyridine as Ligand ; # Attachment 'crystal_structures.CIF' data_for_compound_1II _database_code_depnum_ccdc_archive 'CCDC 734729' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'catena[bis(isothiocyanato-N)-diaqua-(\m2-4,4'-bipyridine-N,N') -iron(II) 4,4'-bipyridine solvate]' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Fe N4 O2 S2, (C10 H8 N2)' _chemical_formula_sum 'C22 H20 Fe N6 O2 S2' _chemical_formula_weight 520.41 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 C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.8760(13) _cell_length_b 11.5450(5) _cell_length_c 14.1520(10) _cell_angle_alpha 90.00 _cell_angle_beta 123.090(7) _cell_angle_gamma 90.00 _cell_volume 2447.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 8.95 _cell_measurement_theta_max 26.8 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_process_details 'X-Shape (STOE, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 'STOE IPDS-1' _diffrn_measurement_method 'Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% NONE _diffrn_reflns_number 13403 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.00 _reflns_number_total 2942 _reflns_number_gt 2358 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+1.2741P] 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 SHELXL _refine_ls_extinction_coef 0.0032(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2942 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _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 0.5000 0.10346(3) 0.2500 0.01316(12) Uani 1 2 d S . . N1 N 0.5000 0.29378(16) 0.2500 0.0139(4) Uani 1 2 d S . . N2 N 0.5000 0.91078(16) 0.2500 0.0166(4) Uani 1 2 d S . . C1 C 0.42698(10) 0.35471(14) 0.22455(13) 0.0145(3) Uani 1 1 d . . . H1 H 0.3749 0.3133 0.2068 0.017 Uiso 1 1 calc R . . C2 C 0.42392(10) 0.47442(14) 0.22290(13) 0.0137(3) Uani 1 1 d . . . H2 H 0.3705 0.5134 0.2035 0.016 Uiso 1 1 calc R . . C3 C 0.5000 0.53789(19) 0.2500 0.0122(4) Uani 1 2 d S . . C4 C 0.5000 0.66643(19) 0.2500 0.0134(4) Uani 1 2 d S . . C5 C 0.43376(11) 0.72989(14) 0.25082(15) 0.0183(3) Uani 1 1 d . . . H5 H 0.3868 0.6909 0.2504 0.022 Uiso 1 1 calc R . . C6 C 0.43684(11) 0.84971(15) 0.25218(15) 0.0197(3) Uani 1 1 d . . . H6 H 0.3920 0.8910 0.2548 0.024 Uiso 1 1 calc R . . S22 S 0.31353(4) 0.11138(5) 0.40878(5) 0.03307(16) Uani 1 1 d . . . O1 O 0.62261(8) 0.10118(10) 0.40884(10) 0.0201(3) Uani 1 1 d . . . H1O1 H 0.6297 0.0562 0.4598 0.030 Uiso 1 1 d R . . H2O1 H 0.6727 0.0884 0.4189 0.030 Uiso 1 1 d R . . N22 N 0.42838(11) 0.10652(12) 0.33147(14) 0.0217(3) Uani 1 1 d . . . C22 C 0.38084(11) 0.10774(14) 0.36369(14) 0.0177(3) Uani 1 1 d . . . N11 N 0.22244(10) 0.05409(17) 0.07530(13) 0.0303(4) Uani 1 1 d . . . C11 C 0.16542(13) 0.1407(2) 0.05346(17) 0.0294(4) Uani 1 1 d . . . H11 H 0.1858 0.2179 0.0588 0.035 Uiso 1 1 calc R . . C12 C 0.07800(12) 0.12396(17) 0.02334(15) 0.0248(4) Uani 1 1 d . . . H12 H 0.0399 0.1885 0.0075 0.030 Uiso 1 1 calc R . . C13 C 0.04673(11) 0.01155(16) 0.01658(13) 0.0199(4) Uani 1 1 d . . . C14 C 0.10664(13) -0.07884(18) 0.04062(17) 0.0277(4) Uani 1 1 d . . . H14 H 0.0888 -0.1570 0.0379 0.033 Uiso 1 1 calc R . . C15 C 0.19214(13) -0.0537(2) 0.06841(17) 0.0315(4) Uani 1 1 d . . . H15 H 0.2315 -0.1164 0.0834 0.038 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 0.01428(18) 0.00678(18) 0.02346(19) 0.000 0.01355(14) 0.000 N1 0.0164(9) 0.0080(9) 0.0195(9) 0.000 0.0112(8) 0.000 N2 0.0174(9) 0.0084(9) 0.0268(10) 0.000 0.0138(8) 0.000 C1 0.0146(7) 0.0100(7) 0.0200(7) -0.0005(6) 0.0101(6) -0.0017(5) C2 0.0137(7) 0.0107(7) 0.0181(7) 0.0001(5) 0.0096(6) 0.0015(5) C3 0.0161(10) 0.0092(10) 0.0123(9) 0.000 0.0084(8) 0.000 C4 0.0172(11) 0.0081(10) 0.0155(10) 0.000 0.0093(9) 0.000 C5 0.0196(8) 0.0103(8) 0.0307(9) -0.0005(6) 0.0174(7) -0.0017(6) C6 0.0192(8) 0.0106(8) 0.0338(9) -0.0009(6) 0.0174(7) 0.0007(6) S22 0.0304(3) 0.0414(3) 0.0440(3) 0.0121(2) 0.0311(2) 0.0078(2) O1 0.0163(6) 0.0184(6) 0.0264(6) 0.0034(5) 0.0121(5) 0.0021(4) N22 0.0261(8) 0.0155(7) 0.0348(8) 0.0008(6) 0.0238(7) -0.0001(6) C22 0.0194(8) 0.0114(8) 0.0240(8) 0.0029(6) 0.0129(7) 0.0009(6) N11 0.0157(7) 0.0487(11) 0.0254(8) 0.0002(7) 0.0106(7) -0.0023(7) C11 0.0238(9) 0.0359(11) 0.0300(9) -0.0028(8) 0.0157(8) -0.0068(8) C12 0.0196(9) 0.0306(11) 0.0255(9) -0.0006(7) 0.0131(7) 0.0014(7) C13 0.0160(8) 0.0311(10) 0.0137(7) 0.0011(6) 0.0088(7) 0.0005(7) C14 0.0206(9) 0.0297(10) 0.0321(10) 0.0071(8) 0.0140(8) 0.0043(7) C15 0.0187(9) 0.0410(12) 0.0338(10) 0.0050(9) 0.0136(8) 0.0062(8) _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 O1 2.1161(12) 2_655 ? Fe1 O1 2.1161(12) . ? Fe1 N22 2.1405(15) . ? Fe1 N22 2.1405(15) 2_655 ? Fe1 N1 2.1973(18) . ? Fe1 N2 2.2245(19) 1_545 ? N1 C1 1.3473(18) . ? N1 C1 1.3473(18) 2_655 ? N2 C6 1.3456(19) . ? N2 C6 1.3456(19) 2_655 ? N2 Fe1 2.2245(19) 1_565 ? C1 C2 1.383(2) . ? C2 C3 1.4015(19) . ? C3 C2 1.4015(19) 2_655 ? C3 C4 1.484(3) . ? C4 C5 1.3979(19) . ? C4 C5 1.3979(19) 2_655 ? C5 C6 1.384(2) . ? S22 C22 1.6416(17) . ? N22 C22 1.163(2) . ? N11 C11 1.338(3) . ? N11 C15 1.339(3) . ? C11 C12 1.391(3) . ? C12 C13 1.396(3) . ? C13 C14 1.398(3) . ? C13 C13 1.492(3) 5 ? C14 C15 1.385(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 O1 Fe1 O1 178.58(7) 2_655 . ? O1 Fe1 N22 89.72(6) 2_655 . ? O1 Fe1 N22 90.30(6) . . ? O1 Fe1 N22 90.30(6) 2_655 2_655 ? O1 Fe1 N22 89.72(6) . 2_655 ? N22 Fe1 N22 178.11(8) . 2_655 ? O1 Fe1 N1 90.71(3) 2_655 . ? O1 Fe1 N1 90.71(3) . . ? N22 Fe1 N1 89.05(4) . . ? N22 Fe1 N1 89.05(4) 2_655 . ? O1 Fe1 N2 89.29(3) 2_655 1_545 ? O1 Fe1 N2 89.29(3) . 1_545 ? N22 Fe1 N2 90.95(4) . 1_545 ? N22 Fe1 N2 90.95(4) 2_655 1_545 ? N1 Fe1 N2 180.0 . 1_545 ? C1 N1 C1 117.05(19) . 2_655 ? C1 N1 Fe1 121.47(9) . . ? C1 N1 Fe1 121.47(9) 2_655 . ? C6 N2 C6 116.8(2) . 2_655 ? C6 N2 Fe1 121.60(10) . 1_565 ? C6 N2 Fe1 121.60(10) 2_655 1_565 ? N1 C1 C2 123.36(15) . . ? C1 C2 C3 119.63(15) . . ? C2 C3 C2 117.0(2) . 2_655 ? C2 C3 C4 121.52(10) . . ? C2 C3 C4 121.52(10) 2_655 . ? C5 C4 C5 116.8(2) . 2_655 ? C5 C4 C3 121.61(10) . . ? C5 C4 C3 121.61(10) 2_655 . ? C6 C5 C4 119.77(15) . . ? N2 C6 C5 123.42(15) . . ? C22 N22 Fe1 172.34(15) . . ? N22 C22 S22 179.21(15) . . ? C11 N11 C15 116.79(17) . . ? N11 C11 C12 123.6(2) . . ? C11 C12 C13 119.43(18) . . ? C12 C13 C14 116.92(16) . . ? C12 C13 C13 121.7(2) . 5 ? C14 C13 C13 121.4(2) . 5 ? C15 C14 C13 119.49(19) . . ? N11 C15 C14 123.74(19) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.505 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.082 #===END data_for_compound_3 _database_code_depnum_ccdc_archive 'CCDC 734730' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'poly[bis(\m2-thiocyanato-N,S)-(\m2-4,4'-bipyridine-N,N')-iron(II)]' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 Fe N4 S2' _chemical_formula_sum 'C12 H8 Fe N4 S2' _chemical_formula_weight 328.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.1738(10) _cell_length_b 11.5606(12) _cell_length_c 11.4572(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.087(9) _cell_angle_gamma 90.00 _cell_volume 1371.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 5.7 _cell_measurement_theta_max 27.7 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.879 _exptl_absorpt_process_details 'X-Shape (STOE, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-1' _diffrn_measurement_method 'Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% NONE _diffrn_reflns_number 6331 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 27.81 _reflns_number_total 1623 _reflns_number_gt 1309 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.9860P] 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 SHELXL _refine_ls_extinction_coef 0.0063(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1623 _refine_ls_number_parameters 90 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.5000 0.01523(3) 0.7500 0.02023(16) Uani 1 2 d S . . N1 N 0.5000 0.20682(19) 0.7500 0.0236(5) Uani 1 2 d S . . N2 N 0.5000 0.8224(2) 0.7500 0.0303(6) Uani 1 2 d S . . C1 C 0.5790(2) 0.26766(18) 0.7094(2) 0.0315(5) Uani 1 1 d . . . H1 H 0.6351 0.2275 0.6813 0.038 Uiso 1 1 calc R . . C2 C 0.5811(2) 0.38761(17) 0.7073(2) 0.0310(5) Uani 1 1 d . . . H2 H 0.6368 0.4259 0.6773 0.037 Uiso 1 1 calc R . . C3 C 0.5000 0.4503(2) 0.7500 0.0219(5) Uani 1 2 d S . . C4 C 0.5000 0.5787(2) 0.7500 0.0252(6) Uani 1 2 d S . . C5 C 0.4757(3) 0.64152(18) 0.8419(2) 0.0377(6) Uani 1 1 d . . . H5 H 0.4583 0.6034 0.9053 0.045 Uiso 1 1 calc R . . C6 C 0.4774(3) 0.76106(19) 0.8387(2) 0.0410(6) Uani 1 1 d . . . H6 H 0.4619 0.8012 0.9019 0.049 Uiso 1 1 calc R . . N11 N 0.38291(18) -0.01469(14) 0.35795(18) 0.0250(4) Uani 1 1 d . . . C11 C 0.34357(19) -0.00203(15) 0.4369(2) 0.0217(4) Uani 1 1 d . . . S11 S 0.28875(6) 0.01838(7) 0.54959(6) 0.0400(2) 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 0.0312(2) 0.0171(2) 0.0191(2) 0.000 0.01725(17) 0.000 N1 0.0300(12) 0.0175(11) 0.0287(13) 0.000 0.0173(10) 0.000 N2 0.0481(15) 0.0203(11) 0.0291(14) 0.000 0.0222(12) 0.000 C1 0.0395(12) 0.0210(10) 0.0474(15) -0.0057(9) 0.0315(11) -0.0023(8) C2 0.0404(12) 0.0200(10) 0.0451(14) -0.0035(8) 0.0302(11) -0.0069(8) C3 0.0272(14) 0.0160(11) 0.0237(14) 0.000 0.0108(11) 0.000 C4 0.0320(15) 0.0191(13) 0.0281(15) 0.000 0.0153(12) 0.000 C5 0.0691(16) 0.0201(10) 0.0372(13) 0.0046(9) 0.0353(12) 0.0051(10) C6 0.0771(18) 0.0221(10) 0.0400(14) 0.0017(9) 0.0405(14) 0.0071(10) N11 0.0313(9) 0.0275(8) 0.0213(8) -0.0003(7) 0.0158(7) 0.0014(6) C11 0.0244(9) 0.0220(9) 0.0206(9) 0.0006(7) 0.0106(7) -0.0010(7) S11 0.0286(3) 0.0763(5) 0.0221(3) -0.0059(3) 0.0175(2) -0.0022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N11 2.1114(18) 6_556 ? Fe1 N11 2.1114(18) 5_656 ? Fe1 N1 2.215(2) . ? Fe1 N2 2.229(2) 1_545 ? Fe1 S11 2.6018(7) 2_656 ? Fe1 S11 2.6018(7) . ? N1 C1 1.341(2) 2_656 ? N1 C1 1.341(2) . ? N2 C6 1.339(3) . ? N2 C6 1.339(3) 2_656 ? N2 Fe1 2.229(2) 1_565 ? C1 C2 1.387(3) . ? C2 C3 1.385(2) . ? C3 C2 1.385(2) 2_656 ? C3 C4 1.485(4) . ? C4 C5 1.387(3) . ? C4 C5 1.387(3) 2_656 ? C5 C6 1.383(3) . ? N11 C11 1.154(3) . ? N11 Fe1 2.1114(18) 5_656 ? C11 S11 1.641(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 N11 Fe1 N11 179.66(9) 6_556 5_656 ? N11 Fe1 N1 90.17(5) 6_556 . ? N11 Fe1 N1 90.17(5) 5_656 . ? N11 Fe1 N2 89.83(5) 6_556 1_545 ? N11 Fe1 N2 89.83(5) 5_656 1_545 ? N1 Fe1 N2 180.0 . 1_545 ? N11 Fe1 S11 92.26(5) 6_556 2_656 ? N11 Fe1 S11 87.74(5) 5_656 2_656 ? N1 Fe1 S11 89.198(18) . 2_656 ? N2 Fe1 S11 90.802(18) 1_545 2_656 ? N11 Fe1 S11 87.74(5) 6_556 . ? N11 Fe1 S11 92.26(5) 5_656 . ? N1 Fe1 S11 89.198(18) . . ? N2 Fe1 S11 90.802(18) 1_545 . ? S11 Fe1 S11 178.40(4) 2_656 . ? C1 N1 C1 116.7(2) 2_656 . ? C1 N1 Fe1 121.63(12) 2_656 . ? C1 N1 Fe1 121.63(12) . . ? C6 N2 C6 116.0(3) . 2_656 ? C6 N2 Fe1 121.99(13) . 1_565 ? C6 N2 Fe1 121.99(13) 2_656 1_565 ? N1 C1 C2 123.20(19) . . ? C3 C2 C1 119.98(19) . . ? C2 C3 C2 116.9(2) 2_656 . ? C2 C3 C4 121.55(12) 2_656 . ? C2 C3 C4 121.55(12) . . ? C5 C4 C5 116.9(3) . 2_656 ? C5 C4 C3 121.55(13) . . ? C5 C4 C3 121.55(13) 2_656 . ? C6 C5 C4 119.6(2) . . ? N2 C6 C5 123.9(2) . . ? C11 N11 Fe1 164.16(17) . 5_656 ? N11 C11 S11 178.95(18) . . ? C11 S11 Fe1 102.08(8) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.81 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.380 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.073