# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Orpen, A' _publ_contact_author_email GUY.ORPEN@BRIS.AC.UK _publ_section_title ; The use of [Fe(dithiooxalate)2(NO)]2- as a tecton in crystal engineering ; loop_ _publ_author_name H.Kara C.Adams B.Schwarz A.Orpen # Attachment '- cifs.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 761432' #TrackingRef '- cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Fe N3 O6 S4' _chemical_formula_weight 502.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.070(2) _cell_length_b 10.547(2) _cell_length_c 10.690(2) _cell_angle_alpha 71.61(3) _cell_angle_beta 68.23(3) _cell_angle_gamma 62.68(3) _cell_volume 922.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(3) _cell_measurement_reflns_used 4758 _cell_measurement_theta_min 2.208 _cell_measurement_theta_max 27.479 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 510 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.877 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10631 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _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 2.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4203 _reflns_number_gt 3716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SHELXTL (Bruker, 2002)' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0363P)^2^+0.6862P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4203 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.001 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 C1 C 0.1982(2) 1.27584(19) 0.7242(2) 0.0166(4) Uani 1 1 d . . . C2 C 0.3537(2) 1.29521(19) 0.66769(18) 0.0143(4) Uani 1 1 d . . . C3 C 0.6580(2) 0.70821(19) 0.99512(19) 0.0147(4) Uani 1 1 d . . . C4 C 0.5066(2) 0.68129(19) 1.04744(19) 0.0150(4) Uani 1 1 d . . . C5 C 0.2318(2) -0.1718(2) 0.6260(2) 0.0165(4) Uani 1 1 d . . . H5 H 0.2904 -0.1436 0.5374 0.020 Uiso 1 1 calc R . . C6 C 0.2860(2) -0.3125(2) 0.6931(2) 0.0186(4) Uani 1 1 d . . . H6 H 0.3832 -0.3809 0.6522 0.022 Uiso 1 1 calc R . . C7 C 0.0669(2) -0.2594(2) 0.8799(2) 0.0186(4) Uani 1 1 d . . . H7 H 0.0106 -0.2917 0.9678 0.022 Uiso 1 1 calc R . . C8 C 0.0097(2) -0.1160(2) 0.8181(2) 0.0170(4) Uani 1 1 d . . . H8 H -0.0846 -0.0488 0.8643 0.020 Uiso 1 1 calc R . . C9 C 0.0915(2) -0.07040(19) 0.68724(19) 0.0130(3) Uani 1 1 d . . . C10 C 0.0297(2) 0.08176(19) 0.61473(19) 0.0135(3) Uani 1 1 d . . . C11 C 0.1258(2) 0.1363(2) 0.5003(2) 0.0196(4) Uani 1 1 d . . . H11 H 0.2317 0.0762 0.4679 0.024 Uiso 1 1 calc R . . C12 C 0.0668(2) 0.2776(2) 0.4343(2) 0.0211(4) Uani 1 1 d . . . H12 H 0.1323 0.3156 0.3575 0.025 Uiso 1 1 calc R . . C13 C -0.1794(2) 0.3127(2) 0.5868(2) 0.0214(4) Uani 1 1 d . . . H13 H -0.2853 0.3748 0.6148 0.026 Uiso 1 1 calc R . . C14 C -0.1251(2) 0.1728(2) 0.6577(2) 0.0187(4) Uani 1 1 d . . . H14 H -0.1932 0.1389 0.7353 0.022 Uiso 1 1 calc R . . Fe1 Fe 0.44564(3) 0.95918(3) 0.80829(3) 0.01241(8) Uani 1 1 d . . . H2A H 0.233(3) -0.441(3) 0.852(2) 0.015 Uiso 1 1 d . . . H3A H -0.123(3) 0.450(2) 0.435(2) 0.015 Uiso 1 1 d . . . H6A H 0.327(3) 0.515(2) 0.182(2) 0.015 Uiso 1 1 d . . . H6B H 0.158(3) 0.555(2) 0.216(2) 0.015 Uiso 1 1 d . . . N1 N 0.50523(19) 0.87619(17) 0.67491(17) 0.0177(3) Uani 1 1 d . . . N2 N 0.20124(19) -0.35248(17) 0.81607(17) 0.0162(3) Uani 1 1 d . . . N3 N -0.0824(2) 0.36038(17) 0.47880(17) 0.0188(3) Uani 1 1 d . . . O1 O 0.08375(16) 1.37973(15) 0.69490(16) 0.0241(3) Uani 1 1 d . . . O2 O 0.35550(16) 1.41051(14) 0.59566(14) 0.0198(3) Uani 1 1 d . . . O3 O 0.76810(15) 0.62029(14) 1.04183(14) 0.0183(3) Uani 1 1 d . . . O4 O 0.50191(16) 0.57561(14) 1.13651(14) 0.0195(3) Uani 1 1 d . . . O5 O 0.5666(2) 0.8002(2) 0.59422(19) 0.0421(5) Uani 1 1 d . . . O6 O 0.2502(2) 0.47955(18) 0.2116(2) 0.0371(4) Uani 1 1 d . . . S1 S 0.19325(5) 1.11384(5) 0.82335(5) 0.01561(10) Uani 1 1 d . . . S2 S 0.51247(5) 1.15371(5) 0.71523(5) 0.01499(10) Uani 1 1 d . . . S3 S 0.66153(5) 0.86309(5) 0.87960(5) 0.01660(11) Uani 1 1 d . . . S4 S 0.35318(5) 0.80446(5) 0.98025(5) 0.01644(11) 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 C1 0.0192(10) 0.0129(8) 0.0172(9) -0.0003(7) -0.0073(8) -0.0054(7) C2 0.0163(9) 0.0127(8) 0.0121(9) -0.0009(7) -0.0044(7) -0.0045(7) C3 0.0153(9) 0.0119(8) 0.0144(9) -0.0014(7) -0.0036(7) -0.0042(7) C4 0.0155(9) 0.0138(8) 0.0153(9) -0.0017(7) -0.0050(7) -0.0053(7) C5 0.0171(9) 0.0156(9) 0.0149(9) 0.0001(7) -0.0032(7) -0.0073(7) C6 0.0154(9) 0.0148(9) 0.0209(10) -0.0024(7) -0.0037(8) -0.0035(7) C7 0.0177(9) 0.0180(9) 0.0173(10) 0.0017(7) -0.0039(8) -0.0084(8) C8 0.0129(9) 0.0155(9) 0.0175(9) -0.0010(7) -0.0014(7) -0.0046(7) C9 0.0124(8) 0.0128(8) 0.0151(9) -0.0003(7) -0.0051(7) -0.0064(7) C10 0.0152(9) 0.0124(8) 0.0149(9) -0.0006(7) -0.0067(7) -0.0061(7) C11 0.0168(9) 0.0139(9) 0.0221(10) -0.0003(7) -0.0026(8) -0.0049(7) C12 0.0240(10) 0.0161(9) 0.0206(10) 0.0028(7) -0.0059(8) -0.0097(8) C13 0.0175(10) 0.0176(9) 0.0219(10) -0.0014(8) -0.0074(8) -0.0008(7) C14 0.0164(9) 0.0176(9) 0.0171(9) 0.0014(7) -0.0044(8) -0.0054(7) Fe1 0.01322(14) 0.01096(13) 0.01169(14) 0.00018(9) -0.00408(10) -0.00439(10) N1 0.0182(8) 0.0198(8) 0.0154(8) -0.0020(6) -0.0049(6) -0.0082(7) N2 0.0192(8) 0.0094(7) 0.0193(8) 0.0028(6) -0.0090(7) -0.0055(6) N3 0.0229(9) 0.0123(7) 0.0190(8) 0.0022(6) -0.0104(7) -0.0046(7) O1 0.0166(7) 0.0166(7) 0.0321(8) 0.0053(6) -0.0104(6) -0.0041(6) O2 0.0217(7) 0.0142(6) 0.0208(7) 0.0024(5) -0.0069(6) -0.0075(5) O3 0.0153(7) 0.0146(6) 0.0213(7) 0.0025(5) -0.0069(6) -0.0049(5) O4 0.0183(7) 0.0152(6) 0.0216(7) 0.0047(5) -0.0065(6) -0.0082(5) O5 0.0322(10) 0.0624(12) 0.0400(10) -0.0354(9) 0.0005(8) -0.0162(9) O6 0.0252(9) 0.0254(8) 0.0568(12) -0.0086(8) -0.0021(8) -0.0126(7) S1 0.0144(2) 0.0133(2) 0.0177(2) 0.00244(17) -0.00632(18) -0.00594(17) S2 0.0127(2) 0.0134(2) 0.0151(2) 0.00179(16) -0.00334(17) -0.00499(17) S3 0.0139(2) 0.0135(2) 0.0194(2) 0.00454(17) -0.00631(18) -0.00618(17) S4 0.0140(2) 0.0141(2) 0.0198(2) 0.00304(17) -0.00695(18) -0.00630(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.232(2) . ? C1 C2 1.541(3) . ? C1 S1 1.7151(19) . ? C2 O2 1.221(2) . ? C2 S2 1.725(2) . ? C3 O3 1.230(2) . ? C3 C4 1.544(3) . ? C3 S3 1.7154(19) . ? C4 O4 1.223(2) . ? C4 S4 1.727(2) . ? C5 C6 1.375(3) . ? C5 C9 1.392(3) . ? C5 H5 0.9500 . ? C6 N2 1.335(3) . ? C6 H6 0.9500 . ? C7 N2 1.333(3) . ? C7 C8 1.381(3) . ? C7 H7 0.9500 . ? C8 C9 1.397(3) . ? C8 H8 0.9500 . ? C9 C10 1.490(2) . ? C10 C14 1.392(3) . ? C10 C11 1.397(3) . ? C11 C12 1.381(3) . ? C11 H11 0.9500 . ? C12 N3 1.332(3) . ? C12 H12 0.9500 . ? C13 N3 1.337(3) . ? C13 C14 1.383(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? Fe1 N1 1.6823(18) . ? Fe1 S3 2.2483(9) . ? Fe1 S2 2.2661(8) . ? Fe1 S4 2.2674(10) . ? Fe1 S1 2.2811(11) . ? N1 O5 1.164(2) . ? N2 H2A 0.84(2) . ? N3 H3A 0.88(2) . ? O6 H6A 0.92(2) . ? O6 H6B 0.90(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 O1 C1 C2 117.11(16) . . ? O1 C1 S1 123.93(16) . . ? C2 C1 S1 118.96(13) . . ? O2 C2 C1 118.06(16) . . ? O2 C2 S2 124.50(15) . . ? C1 C2 S2 117.41(13) . . ? O3 C3 C4 118.44(16) . . ? O3 C3 S3 123.30(15) . . ? C4 C3 S3 118.21(13) . . ? O4 C4 C3 117.67(16) . . ? O4 C4 S4 124.19(15) . . ? C3 C4 S4 118.12(13) . . ? C6 C5 C9 120.31(18) . . ? C6 C5 H5 119.8 . . ? C9 C5 H5 119.8 . . ? N2 C6 C5 119.59(18) . . ? N2 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? N2 C7 C8 120.06(18) . . ? N2 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C9 119.50(18) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C5 C9 C8 118.02(17) . . ? C5 C9 C10 120.94(17) . . ? C8 C9 C10 121.03(17) . . ? C14 C10 C11 118.18(17) . . ? C14 C10 C9 121.15(17) . . ? C11 C10 C9 120.66(17) . . ? C12 C11 C10 119.95(19) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? N3 C12 C11 119.66(19) . . ? N3 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? N3 C13 C14 119.83(19) . . ? N3 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C10 119.73(18) . . ? C13 C14 H14 120.1 . . ? C10 C14 H14 120.1 . . ? N1 Fe1 S3 101.94(7) . . ? N1 Fe1 S2 103.72(6) . . ? S3 Fe1 S2 83.70(3) . . ? N1 Fe1 S4 100.56(6) . . ? S3 Fe1 S4 89.16(4) . . ? S2 Fe1 S4 155.61(3) . . ? N1 Fe1 S1 106.82(7) . . ? S3 Fe1 S1 151.21(3) . . ? S2 Fe1 S1 88.26(3) . . ? S4 Fe1 S1 86.88(4) . . ? O5 N1 Fe1 167.73(17) . . ? C7 N2 C6 122.45(17) . . ? C7 N2 H2A 119.9(15) . . ? C6 N2 H2A 117.6(15) . . ? C12 N3 C13 122.63(17) . . ? C12 N3 H3A 121.0(15) . . ? C13 N3 H3A 116.4(15) . . ? H6A O6 H6B 108.7(19) . . ? C1 S1 Fe1 105.99(8) . . ? C2 S2 Fe1 106.54(7) . . ? C3 S3 Fe1 106.64(7) . . ? C4 S4 Fe1 106.04(7) . . ? 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 O1 C1 C2 O2 -1.3(3) . . . . ? S1 C1 C2 O2 178.96(14) . . . . ? O1 C1 C2 S2 176.81(15) . . . . ? S1 C1 C2 S2 -3.0(2) . . . . ? O3 C3 C4 O4 2.3(3) . . . . ? S3 C3 C4 O4 -175.23(14) . . . . ? O3 C3 C4 S4 -179.46(14) . . . . ? S3 C3 C4 S4 3.0(2) . . . . ? C9 C5 C6 N2 1.8(3) . . . . ? N2 C7 C8 C9 1.7(3) . . . . ? C6 C5 C9 C8 0.6(3) . . . . ? C6 C5 C9 C10 -178.80(18) . . . . ? C7 C8 C9 C5 -2.3(3) . . . . ? C7 C8 C9 C10 177.11(17) . . . . ? C5 C9 C10 C14 163.22(19) . . . . ? C8 C9 C10 C14 -16.2(3) . . . . ? C5 C9 C10 C11 -15.9(3) . . . . ? C8 C9 C10 C11 164.69(18) . . . . ? C14 C10 C11 C12 0.9(3) . . . . ? C9 C10 C11 C12 -179.95(18) . . . . ? C10 C11 C12 N3 -1.2(3) . . . . ? N3 C13 C14 C10 -1.0(3) . . . . ? C11 C10 C14 C13 0.2(3) . . . . ? C9 C10 C14 C13 -178.96(18) . . . . ? S3 Fe1 N1 O5 22.4(8) . . . . ? S2 Fe1 N1 O5 108.8(8) . . . . ? S4 Fe1 N1 O5 -69.0(8) . . . . ? S1 Fe1 N1 O5 -158.9(8) . . . . ? C8 C7 N2 C6 0.8(3) . . . . ? C5 C6 N2 C7 -2.5(3) . . . . ? C11 C12 N3 C13 0.5(3) . . . . ? C14 C13 N3 C12 0.6(3) . . . . ? O1 C1 S1 Fe1 170.88(16) . . . . ? C2 C1 S1 Fe1 -9.37(16) . . . . ? N1 Fe1 S1 C1 -90.25(9) . . . . ? S3 Fe1 S1 C1 87.11(8) . . . . ? S2 Fe1 S1 C1 13.56(7) . . . . ? S4 Fe1 S1 C1 169.66(7) . . . . ? O2 C2 S2 Fe1 -168.30(15) . . . . ? C1 C2 S2 Fe1 13.75(15) . . . . ? N1 Fe1 S2 C2 91.92(9) . . . . ? S3 Fe1 S2 C2 -167.29(7) . . . . ? S4 Fe1 S2 C2 -93.51(9) . . . . ? S1 Fe1 S2 C2 -14.97(7) . . . . ? O3 C3 S3 Fe1 171.19(15) . . . . ? C4 C3 S3 Fe1 -11.44(15) . . . . ? N1 Fe1 S3 C3 -88.51(9) . . . . ? S2 Fe1 S3 C3 168.75(7) . . . . ? S4 Fe1 S3 C3 12.11(7) . . . . ? S1 Fe1 S3 C3 94.08(8) . . . . ? O4 C4 S4 Fe1 -174.91(15) . . . . ? C3 C4 S4 Fe1 6.95(15) . . . . ? N1 Fe1 S4 C4 91.30(9) . . . . ? S3 Fe1 S4 C4 -10.69(7) . . . . ? S2 Fe1 S4 C4 -83.33(9) . . . . ? S1 Fe1 S4 C4 -162.16(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.525 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.076 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 761433' #TrackingRef '- cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H20 Fe N5 O7 S4' _chemical_formula_weight 554.44 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 P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 13.464(3) _cell_length_b 12.053(2) _cell_length_c 14.304(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.68(3) _cell_angle_gamma 90.00 _cell_volume 2309.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2154 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.449 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 1.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_absorpt_correction_T_min 0.881 _exptl_absorpt_correction_T_max 0.900 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16036 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5306 _reflns_number_gt 4945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SHELXTL (Bruker, 2002)' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0358P)^2^+1.1655P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5306 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 C1 C 0.16366(12) 0.55804(13) 0.85367(11) 0.0150(3) Uani 1 1 d . . . C2 C 0.15596(12) 0.50812(13) 0.95181(11) 0.0159(3) Uani 1 1 d . . . C3 C 0.35137(11) 0.91860(12) 1.13508(11) 0.0139(3) Uani 1 1 d . . . C4 C 0.35899(12) 0.97126(13) 1.03810(11) 0.0157(3) Uani 1 1 d . . . C5 C 1.12991(17) 1.04677(16) 0.13091(17) 0.0359(5) Uani 1 1 d . . . H5A H 1.0975 1.0503 0.0666 0.054 Uiso 1 1 calc R . . H5B H 1.1567 0.9720 0.1434 0.054 Uiso 1 1 calc R . . H5C H 1.1845 1.1009 0.1384 0.054 Uiso 1 1 calc R . . C6 C 1.05606(12) 1.07256(13) 0.19788(12) 0.0173(3) Uani 1 1 d . . . C7 C 1.0000 1.00270(18) 0.2500 0.0147(4) Uani 1 2 d S . . C8 C 1.0000 0.88059(17) 0.2500 0.0142(4) Uani 1 2 d S . . C9 C 0.92938(12) 0.81126(12) 0.20151(11) 0.0155(3) Uani 1 1 d . . . C10 C 0.83756(13) 0.83843(14) 0.13919(13) 0.0212(3) Uani 1 1 d . . . H10A H 0.8342 0.7916 0.0830 0.032 Uiso 1 1 calc R . . H10B H 0.8392 0.9167 0.1207 0.032 Uiso 1 1 calc R . . H10C H 0.7787 0.8249 0.1728 0.032 Uiso 1 1 calc R . . C11 C 0.59206(14) 0.53050(15) 0.10091(13) 0.0244(4) Uani 1 1 d . . . H11A H 0.5547 0.5634 0.0455 0.037 Uiso 1 1 calc R . . H11B H 0.5972 0.4502 0.0921 0.037 Uiso 1 1 calc R . . H11C H 0.6591 0.5629 0.1095 0.037 Uiso 1 1 calc R . . C12 C 0.53930(11) 0.55330(12) 0.18515(11) 0.0144(3) Uani 1 1 d . . . C13 C 0.5000 0.48320(17) 0.2500 0.0132(4) Uani 1 2 d S . . C14 C 0.5000 0.36100(17) 0.2500 0.0139(4) Uani 1 2 d S . . C15 C 0.43557(12) 0.29134(13) 0.19425(11) 0.0149(3) Uani 1 1 d . . . C16 C 0.35007(13) 0.31831(14) 0.12344(12) 0.0201(3) Uani 1 1 d . . . H16A H 0.3553 0.2744 0.0664 0.030 Uiso 1 1 calc R . . H16B H 0.3516 0.3975 0.1080 0.030 Uiso 1 1 calc R . . H16C H 0.2872 0.3008 0.1493 0.030 Uiso 1 1 calc R . . Fe1 Fe 0.223409(16) 0.756844(17) 0.994172(15) 0.01166(7) Uani 1 1 d . . . H6A H 0.4066(14) 0.1115(17) 0.8263(15) 0.014 Uiso 1 1 d . . . H7A H 0.0800(14) 0.6251(16) 0.5809(16) 0.014 Uiso 1 1 d . . . H6B H 0.4191(14) 0.1293(16) 0.9176(16) 0.014 Uiso 1 1 d . . . H7B H 0.0914(15) 0.5895(17) 0.6676(15) 0.014 Uiso 1 1 d . . . N1 N 0.10705(10) 0.80551(12) 0.99881(10) 0.0196(3) Uani 1 1 d . . . N2 N 1.03368(10) 1.17696(11) 0.21844(10) 0.0161(3) Uani 1 1 d . . . H2 H 1.0591 1.2365 0.1944 0.019 Uiso 1 1 calc R . . N3 N 0.95752(10) 0.70671(11) 0.22104(10) 0.0171(3) Uani 1 1 d . . . H3 H 0.9254 0.6471 0.1993 0.020 Uiso 1 1 calc R . . N4 N 0.52357(10) 0.65796(11) 0.21089(10) 0.0161(3) Uani 1 1 d . . . H4 H 0.5414 0.7175 0.1811 0.019 Uiso 1 1 calc R . . N5 N 0.46151(10) 0.18686(11) 0.21628(10) 0.0166(3) Uani 1 1 d . . . H5 H 0.4327 0.1272 0.1906 0.020 Uiso 1 1 calc R . . O1 O 0.13416(9) 0.50078(9) 0.78550(8) 0.0198(3) Uani 1 1 d . . . O2 O 0.12267(10) 0.41334(10) 0.95511(9) 0.0230(3) Uani 1 1 d . . . O3 O 0.38411(9) 0.97278(9) 1.20442(8) 0.0179(2) Uani 1 1 d . . . O4 O 0.39620(10) 1.06427(9) 1.03773(8) 0.0221(3) Uani 1 1 d . . . O5 O 0.02307(10) 0.81255(14) 1.01209(12) 0.0408(4) Uani 1 1 d . . . O6 O 0.42516(10) 0.15456(10) 0.86608(9) 0.0218(3) Uani 1 1 d . . . O7 O 0.06419(11) 0.63325(10) 0.63336(9) 0.0228(3) Uani 1 1 d . . . S1 S 0.21732(3) 0.68664(3) 0.84673(3) 0.01624(9) Uani 1 1 d . . . S2 S 0.19821(3) 0.58502(3) 1.04883(3) 0.01862(10) Uani 1 1 d . . . S3 S 0.29739(3) 0.79009(3) 1.14055(3) 0.01529(9) Uani 1 1 d . . . S4 S 0.31689(3) 0.89665(3) 0.93970(3) 0.01869(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 C1 0.0196(7) 0.0119(7) 0.0135(7) -0.0006(6) 0.0014(6) -0.0012(6) C2 0.0230(8) 0.0122(7) 0.0127(7) -0.0002(5) 0.0020(6) -0.0018(6) C3 0.0149(7) 0.0113(7) 0.0153(8) 0.0008(5) 0.0005(6) 0.0001(5) C4 0.0199(7) 0.0126(7) 0.0143(8) 0.0007(6) 0.0010(6) -0.0012(6) C5 0.0469(12) 0.0182(9) 0.0479(13) 0.0042(8) 0.0320(11) 0.0069(8) C6 0.0211(8) 0.0106(7) 0.0207(8) 0.0006(6) 0.0050(7) 0.0028(6) C7 0.0174(10) 0.0104(10) 0.0163(11) 0.000 0.0014(9) 0.000 C8 0.0190(10) 0.0091(10) 0.0148(11) 0.000 0.0025(9) 0.000 C9 0.0207(8) 0.0111(7) 0.0147(7) 0.0002(6) 0.0025(6) 0.0008(6) C10 0.0223(8) 0.0175(8) 0.0227(9) 0.0003(6) -0.0027(7) 0.0021(6) C11 0.0328(9) 0.0185(8) 0.0240(9) 0.0027(7) 0.0127(8) 0.0039(7) C12 0.0161(7) 0.0110(7) 0.0159(8) 0.0009(6) 0.0004(6) 0.0011(6) C13 0.0151(10) 0.0099(10) 0.0143(10) 0.000 0.0001(8) 0.000 C14 0.0173(10) 0.0101(10) 0.0147(10) 0.000 0.0035(8) 0.000 C15 0.0186(7) 0.0114(7) 0.0149(7) 0.0007(6) 0.0034(6) 0.0004(6) C16 0.0234(8) 0.0167(8) 0.0191(8) 0.0009(6) -0.0037(7) 0.0002(6) Fe1 0.01464(12) 0.00873(11) 0.01140(12) -0.00059(7) 0.00020(9) -0.00097(8) N1 0.0192(7) 0.0210(7) 0.0179(7) -0.0057(5) -0.0013(6) 0.0025(6) N2 0.0208(7) 0.0099(6) 0.0187(7) 0.0012(5) 0.0071(6) -0.0002(5) N3 0.0225(7) 0.0099(6) 0.0179(7) -0.0008(5) -0.0028(6) -0.0013(5) N4 0.0205(7) 0.0103(6) 0.0178(7) 0.0019(5) 0.0036(5) 0.0001(5) N5 0.0212(7) 0.0098(6) 0.0180(7) -0.0014(5) -0.0019(6) -0.0012(5) O1 0.0325(7) 0.0126(5) 0.0138(6) -0.0020(4) 0.0005(5) -0.0061(5) O2 0.0393(7) 0.0137(6) 0.0162(6) -0.0014(4) 0.0042(5) -0.0103(5) O3 0.0260(6) 0.0137(5) 0.0133(6) -0.0011(4) -0.0019(5) -0.0049(5) O4 0.0359(7) 0.0137(5) 0.0164(6) -0.0003(4) 0.0013(5) -0.0101(5) O5 0.0208(7) 0.0580(10) 0.0445(9) -0.0157(8) 0.0080(6) 0.0049(7) O6 0.0385(7) 0.0136(6) 0.0135(6) -0.0002(5) 0.0039(5) -0.0080(5) O7 0.0416(8) 0.0135(6) 0.0142(6) 0.0009(5) 0.0067(6) 0.0096(5) S1 0.0260(2) 0.01075(17) 0.01188(19) 0.00030(13) 0.00141(15) -0.00526(14) S2 0.0327(2) 0.01200(18) 0.01081(19) 0.00020(13) 0.00042(16) -0.00758(16) S3 0.0221(2) 0.01125(18) 0.01198(18) 0.00104(13) -0.00117(15) -0.00478(14) S4 0.0304(2) 0.01375(18) 0.01164(19) -0.00003(14) 0.00090(16) -0.00871(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.2281(19) . ? C1 C2 1.540(2) . ? C1 S1 1.7172(16) . ? C2 O2 1.2298(19) . ? C2 S2 1.7183(17) . ? C3 O3 1.2321(19) . ? C3 C4 1.538(2) . ? C3 S3 1.7160(16) . ? C4 O4 1.2282(19) . ? C4 S4 1.7186(17) . ? C5 C6 1.480(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N2 1.333(2) . ? C6 C7 1.395(2) . ? C7 C6 1.395(2) 2_755 ? C7 C8 1.472(3) . ? C8 C9 1.398(2) . ? C8 C9 1.398(2) 2_755 ? C9 N3 1.337(2) . ? C9 C10 1.487(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.484(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N4 1.337(2) . ? C12 C13 1.397(2) . ? C13 C12 1.397(2) 2_655 ? C13 C14 1.473(3) . ? C14 C15 1.399(2) . ? C14 C15 1.399(2) 2_655 ? C15 N5 1.336(2) . ? C15 C16 1.492(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? Fe1 N1 1.6803(15) . ? Fe1 S2 2.2512(6) . ? Fe1 S3 2.2636(7) . ? Fe1 S1 2.2664(6) . ? Fe1 S4 2.2857(6) . ? N1 O5 1.168(2) . ? N2 N2 1.342(3) 2_755 ? N2 H2 0.8800 . ? N3 N3 1.344(3) 2_755 ? N3 H3 0.8800 . ? N4 N4 1.340(3) 2_655 ? N4 H4 0.8800 . ? N5 N5 1.344(3) 2_655 ? N5 H5 0.8800 . ? O6 H6A 0.79(2) . ? O6 H6B 0.81(2) . ? O7 H7A 0.81(2) . ? O7 H7B 0.78(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 O1 C1 C2 117.30(14) . . ? O1 C1 S1 124.48(13) . . ? C2 C1 S1 118.16(11) . . ? O2 C2 C1 117.09(14) . . ? O2 C2 S2 124.26(13) . . ? C1 C2 S2 118.60(11) . . ? O3 C3 C4 117.19(13) . . ? O3 C3 S3 124.13(12) . . ? C4 C3 S3 118.68(11) . . ? O4 C4 C3 116.37(14) . . ? O4 C4 S4 125.15(13) . . ? C3 C4 S4 118.48(11) . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 107.80(14) . . ? N2 C6 C5 121.45(15) . . ? C7 C6 C5 130.74(15) . . ? C6 C7 C6 105.74(19) 2_755 . ? C6 C7 C8 127.13(10) 2_755 . ? C6 C7 C8 127.13(10) . . ? C9 C8 C9 106.55(19) . 2_755 ? C9 C8 C7 126.72(9) . . ? C9 C8 C7 126.72(9) 2_755 . ? N3 C9 C8 107.15(15) . . ? N3 C9 C10 122.29(14) . . ? C8 C9 C10 130.56(14) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C13 107.88(14) . . ? N4 C12 C11 120.01(14) . . ? C13 C12 C11 132.11(15) . . ? C12 C13 C12 105.57(19) 2_655 . ? C12 C13 C14 127.22(9) 2_655 . ? C12 C13 C14 127.22(9) . . ? C15 C14 C15 106.22(19) . 2_655 ? C15 C14 C13 126.89(10) . . ? C15 C14 C13 126.89(10) 2_655 . ? N5 C15 C14 107.36(15) . . ? N5 C15 C16 122.12(14) . . ? C14 C15 C16 130.51(15) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 Fe1 S2 97.72(5) . . ? N1 Fe1 S3 103.20(6) . . ? S2 Fe1 S3 84.793(18) . . ? N1 Fe1 S1 102.65(6) . . ? S2 Fe1 S1 89.25(2) . . ? S3 Fe1 S1 154.02(2) . . ? N1 Fe1 S4 107.64(5) . . ? S2 Fe1 S4 154.63(2) . . ? S3 Fe1 S4 88.74(2) . . ? S1 Fe1 S4 85.90(2) . . ? O5 N1 Fe1 162.39(15) . . ? C6 N2 N2 109.33(9) . 2_755 ? C6 N2 H2 125.3 . . ? N2 N2 H2 125.3 2_755 . ? C9 N3 N3 109.57(9) . 2_755 ? C9 N3 H3 125.2 . . ? N3 N3 H3 125.2 2_755 . ? C12 N4 N4 109.33(9) . 2_655 ? C12 N4 H4 125.3 . . ? N4 N4 H4 125.3 2_655 . ? C15 N5 N5 109.53(9) . 2_655 ? C15 N5 H5 125.2 . . ? N5 N5 H5 125.2 2_655 . ? H6A O6 H6B 111(2) . . ? H7A O7 H7B 110(2) . . ? C1 S1 Fe1 105.06(6) . . ? C2 S2 Fe1 105.36(6) . . ? C3 S3 Fe1 105.50(6) . . ? C4 S4 Fe1 104.75(6) . . ? 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 O1 C1 C2 O2 1.5(2) . . . . ? S1 C1 C2 O2 -175.85(13) . . . . ? O1 C1 C2 S2 179.05(12) . . . . ? S1 C1 C2 S2 1.73(18) . . . . ? O3 C3 C4 O4 -0.9(2) . . . . ? S3 C3 C4 O4 178.47(12) . . . . ? O3 C3 C4 S4 178.42(12) . . . . ? S3 C3 C4 S4 -2.21(18) . . . . ? N2 C6 C7 C6 -0.11(8) . . . 2_755 ? C5 C6 C7 C6 179.2(2) . . . 2_755 ? N2 C6 C7 C8 179.89(8) . . . . ? C5 C6 C7 C8 -0.8(2) . . . . ? C6 C7 C8 C9 79.88(12) 2_755 . . . ? C6 C7 C8 C9 -100.12(12) . . . . ? C6 C7 C8 C9 -100.12(12) 2_755 . . 2_755 ? C6 C7 C8 C9 79.88(12) . . . 2_755 ? C9 C8 C9 N3 0.11(8) 2_755 . . . ? C7 C8 C9 N3 -179.89(8) . . . . ? C9 C8 C9 C10 179.6(2) 2_755 . . . ? C7 C8 C9 C10 -0.4(2) . . . . ? N4 C12 C13 C12 -0.07(8) . . . 2_655 ? C11 C12 C13 C12 179.0(2) . . . 2_655 ? N4 C12 C13 C14 179.93(8) . . . . ? C11 C12 C13 C14 -1.0(2) . . . . ? C12 C13 C14 C15 101.26(12) 2_655 . . . ? C12 C13 C14 C15 -78.74(12) . . . . ? C12 C13 C14 C15 -78.74(12) 2_655 . . 2_655 ? C12 C13 C14 C15 101.26(12) . . . 2_655 ? C15 C14 C15 N5 -0.21(8) 2_655 . . . ? C13 C14 C15 N5 179.79(8) . . . . ? C15 C14 C15 C16 178.2(2) 2_655 . . . ? C13 C14 C15 C16 -1.8(2) . . . . ? S2 Fe1 N1 O5 3.5(5) . . . . ? S3 Fe1 N1 O5 -82.9(5) . . . . ? S1 Fe1 N1 O5 94.5(5) . . . . ? S4 Fe1 N1 O5 -175.8(5) . . . . ? C7 C6 N2 N2 0.3(2) . . . 2_755 ? C5 C6 N2 N2 -179.07(19) . . . 2_755 ? C8 C9 N3 N3 -0.3(2) . . . 2_755 ? C10 C9 N3 N3 -179.80(17) . . . 2_755 ? C13 C12 N4 N4 0.2(2) . . . 2_655 ? C11 C12 N4 N4 -179.03(17) . . . 2_655 ? C14 C15 N5 N5 0.6(2) . . . 2_655 ? C16 C15 N5 N5 -178.05(17) . . . 2_655 ? O1 C1 S1 Fe1 168.74(13) . . . . ? C2 C1 S1 Fe1 -14.15(13) . . . . ? N1 Fe1 S1 C1 -81.25(8) . . . . ? S2 Fe1 S1 C1 16.50(6) . . . . ? S3 Fe1 S1 C1 92.96(7) . . . . ? S4 Fe1 S1 C1 171.58(6) . . . . ? O2 C2 S2 Fe1 -170.83(14) . . . . ? C1 C2 S2 Fe1 11.78(14) . . . . ? N1 Fe1 S2 C2 86.95(8) . . . . ? S3 Fe1 S2 C2 -170.40(6) . . . . ? S1 Fe1 S2 C2 -15.72(6) . . . . ? S4 Fe1 S2 C2 -94.50(8) . . . . ? O3 C3 S3 Fe1 167.31(13) . . . . ? C4 C3 S3 Fe1 -12.01(13) . . . . ? N1 Fe1 S3 C3 -91.62(8) . . . . ? S2 Fe1 S3 C3 171.66(6) . . . . ? S1 Fe1 S3 C3 94.19(7) . . . . ? S4 Fe1 S3 C3 16.22(6) . . . . ? O4 C4 S4 Fe1 -165.76(14) . . . . ? C3 C4 S4 Fe1 14.99(13) . . . . ? N1 Fe1 S4 C4 86.33(8) . . . . ? S2 Fe1 S4 C4 -92.17(7) . . . . ? S3 Fe1 S4 C4 -17.12(6) . . . . ? S1 Fe1 S4 C4 -171.68(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.877 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.075 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 761434' #TrackingRef '- cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 Fe N3 O5 S4' _chemical_formula_weight 484.34 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.093(3) _cell_length_b 13.984(3) _cell_length_c 16.470(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3706.4(13) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7860 _cell_measurement_theta_min 2.2915 _cell_measurement_theta_max 27.4725 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 0.878 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24467 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4244 _reflns_number_gt 3693 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SHELXTL (Bruker, 2002)' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0375P)^2^+1.5111P] 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 4244 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 C1 C 0.18477(11) 0.20372(12) 0.46320(10) 0.0194(3) Uani 1 1 d . . . C2 C 0.20341(10) 0.29501(12) 0.51238(10) 0.0187(3) Uani 1 1 d . . . C3 C 0.10446(11) 0.54138(13) 0.22368(10) 0.0203(3) Uani 1 1 d . . . C4 C 0.08034(11) 0.45061(13) 0.17561(10) 0.0196(3) Uani 1 1 d . . . C5 C 0.94198(12) 0.20597(14) 0.48543(11) 0.0269(4) Uani 1 1 d . . . H5 H 0.9621 0.2274 0.4343 0.032 Uiso 1 1 calc R . . C6 C 0.94156(13) 0.26677(14) 0.55147(11) 0.0286(4) Uani 1 1 d . . . H6 H 0.9611 0.3306 0.5464 0.034 Uiso 1 1 calc R . . C7 C 0.91219(12) 0.23312(13) 0.62514(11) 0.0222(4) Uani 1 1 d . . . H7 H 0.9125 0.2741 0.6712 0.027 Uiso 1 1 calc R . . C8 C 0.88242(10) 0.14066(12) 0.63268(10) 0.0170(3) Uani 1 1 d . . . C9 C 0.85081(10) 0.10274(12) 0.71098(10) 0.0169(3) Uani 1 1 d . . . C10 C 0.81568(10) 0.16395(13) 0.76765(10) 0.0187(3) Uani 1 1 d . . . H10 H 0.8123 0.2306 0.7568 0.022 Uiso 1 1 calc R . . C11 C 0.78806(11) 0.03594(14) 0.85631(11) 0.0231(4) Uani 1 1 d . . . H11 H 0.7651 0.0141 0.9061 0.028 Uiso 1 1 calc R . . C12 C 0.82312(12) -0.02802(13) 0.80286(11) 0.0253(4) Uani 1 1 d . . . H12 H 0.8253 -0.0943 0.8154 0.030 Uiso 1 1 calc R . . C13 C 0.85509(12) 0.00593(13) 0.73051(10) 0.0221(4) Uani 1 1 d . . . H13 H 0.8803 -0.0374 0.6936 0.027 Uiso 1 1 calc R . . C14 C 0.88407(10) 0.08230(13) 0.56430(10) 0.0189(3) Uani 1 1 d . . . H14 H 0.8642 0.0184 0.5674 0.023 Uiso 1 1 calc R . . Fe1 Fe 0.104265(15) 0.375986(17) 0.357296(14) 0.01511(7) Uani 1 1 d . . . N1 N 0.00825(9) 0.39863(11) 0.39440(9) 0.0214(3) Uani 1 1 d . . . N2 N 0.91369(9) 0.11645(11) 0.49414(9) 0.0208(3) Uani 1 1 d . . . H2 H 0.9146 0.0783 0.4517 0.025 Uiso 1 1 calc R . . N3 N 0.78644(9) 0.12888(11) 0.83788(9) 0.0211(3) Uani 1 1 d . . . H3 H 0.7652 0.1690 0.8734 0.025 Uiso 1 1 calc R . . O1 O 0.20426(9) 0.12687(9) 0.49236(8) 0.0278(3) Uani 1 1 d . . . O2 O 0.23809(8) 0.28666(9) 0.57875(7) 0.0260(3) Uani 1 1 d . . . O3 O 0.10205(9) 0.61836(9) 0.18868(8) 0.0284(3) Uani 1 1 d . . . O4 O 0.06225(8) 0.46120(10) 0.10345(7) 0.0260(3) Uani 1 1 d . . . O5 O -0.04412(9) 0.44414(12) 0.42533(9) 0.0397(4) Uani 1 1 d . . . S1 S 0.13822(3) 0.21832(3) 0.36895(3) 0.02367(11) Uani 1 1 d . . . S2 S 0.17705(3) 0.40362(3) 0.47168(3) 0.02120(10) Uani 1 1 d . . . S3 S 0.13691(3) 0.52706(3) 0.32330(3) 0.02359(11) Uani 1 1 d . . . S4 S 0.08218(3) 0.34221(3) 0.22407(3) 0.02020(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 C1 0.0208(8) 0.0169(9) 0.0204(8) -0.0019(6) -0.0009(7) 0.0022(7) C2 0.0173(8) 0.0180(9) 0.0207(8) -0.0019(6) 0.0006(6) 0.0020(6) C3 0.0247(9) 0.0178(9) 0.0184(8) 0.0010(6) 0.0037(7) -0.0017(7) C4 0.0209(8) 0.0192(9) 0.0189(8) 0.0008(7) 0.0029(6) -0.0020(7) C5 0.0325(10) 0.0285(10) 0.0196(9) -0.0004(7) 0.0051(7) -0.0057(8) C6 0.0422(11) 0.0204(10) 0.0233(9) -0.0008(7) 0.0043(8) -0.0089(8) C7 0.0301(9) 0.0178(9) 0.0188(8) -0.0032(7) 0.0015(7) -0.0015(7) C8 0.0184(8) 0.0161(8) 0.0165(8) -0.0018(6) 0.0006(6) 0.0022(6) C9 0.0175(8) 0.0180(8) 0.0152(8) -0.0025(6) -0.0011(6) -0.0007(6) C10 0.0200(8) 0.0177(9) 0.0186(8) 0.0002(6) -0.0001(6) 0.0031(6) C11 0.0221(9) 0.0283(10) 0.0189(8) 0.0052(7) -0.0023(7) -0.0007(7) C12 0.0329(10) 0.0186(9) 0.0243(9) 0.0023(7) -0.0027(8) -0.0023(7) C13 0.0310(10) 0.0161(9) 0.0193(8) -0.0046(7) -0.0012(7) -0.0009(7) C14 0.0199(8) 0.0175(8) 0.0193(8) -0.0029(6) -0.0003(6) 0.0006(6) Fe1 0.01713(13) 0.01320(13) 0.01499(12) -0.00028(8) 0.00083(9) -0.00015(9) N1 0.0183(7) 0.0269(8) 0.0190(7) 0.0052(6) 0.0007(6) 0.0022(6) N2 0.0233(8) 0.0226(8) 0.0166(7) -0.0055(6) 0.0014(6) -0.0002(6) N3 0.0211(8) 0.0261(8) 0.0162(7) -0.0004(6) 0.0021(6) 0.0069(6) O1 0.0390(8) 0.0161(7) 0.0284(7) -0.0005(5) -0.0086(6) 0.0050(5) O2 0.0331(7) 0.0217(7) 0.0232(6) -0.0032(5) -0.0095(5) 0.0052(5) O3 0.0428(9) 0.0196(7) 0.0227(7) 0.0040(5) 0.0005(6) -0.0022(6) O4 0.0358(7) 0.0249(7) 0.0173(6) 0.0029(5) 0.0001(5) -0.0055(6) O5 0.0282(8) 0.0519(10) 0.0389(8) 0.0042(7) 0.0076(6) 0.0175(7) S1 0.0355(3) 0.0139(2) 0.0216(2) -0.00369(16) -0.00886(18) 0.00274(18) S2 0.0293(2) 0.0138(2) 0.0205(2) -0.00317(16) -0.00531(17) 0.00139(17) S3 0.0371(3) 0.0149(2) 0.0188(2) 0.00010(16) -0.00198(18) -0.00418(18) S4 0.0277(2) 0.0164(2) 0.0164(2) -0.00034(15) -0.00113(16) -0.00277(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.218(2) . ? C1 C2 1.541(2) . ? C1 S1 1.7356(18) . ? C2 O2 1.233(2) . ? C2 S2 1.7134(18) . ? C3 O3 1.222(2) . ? C3 C4 1.545(2) . ? C3 S3 1.7335(18) . ? C4 O4 1.233(2) . ? C4 S4 1.7134(18) . ? C5 N2 1.340(2) . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 C7 1.385(3) . ? C6 H6 0.9500 . ? C7 C8 1.384(2) . ? C7 H7 0.9500 . ? C8 C14 1.391(2) . ? C8 C9 1.484(2) . ? C9 C10 1.387(2) . ? C9 C13 1.393(2) . ? C10 N3 1.341(2) . ? C10 H10 0.9500 . ? C11 N3 1.335(2) . ? C11 C12 1.376(3) . ? C11 H11 0.9500 . ? C12 C13 1.382(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 N2 1.338(2) . ? C14 H14 0.9500 . ? Fe1 N1 1.6916(15) . ? Fe1 S3 2.2478(6) . ? Fe1 S2 2.2517(6) . ? Fe1 S4 2.2724(6) . ? Fe1 S1 2.2795(7) . ? N1 O5 1.172(2) . ? N2 H2 0.8800 . ? N3 H3 0.8800 . ? 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 C1 C2 118.25(15) . . ? O1 C1 S1 124.58(14) . . ? C2 C1 S1 117.16(12) . . ? O2 C2 C1 118.40(15) . . ? O2 C2 S2 122.88(13) . . ? C1 C2 S2 118.71(12) . . ? O3 C3 C4 118.30(15) . . ? O3 C3 S3 123.91(14) . . ? C4 C3 S3 117.75(12) . . ? O4 C4 C3 117.04(15) . . ? O4 C4 S4 124.02(14) . . ? C3 C4 S4 118.93(12) . . ? N2 C5 C6 119.30(17) . . ? N2 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C5 C6 C7 118.87(17) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C8 C7 C6 120.94(16) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C14 117.95(16) . . ? C7 C8 C9 122.02(15) . . ? C14 C8 C9 120.02(16) . . ? C10 C9 C13 117.68(16) . . ? C10 C9 C8 120.26(15) . . ? C13 C9 C8 122.06(15) . . ? N3 C10 C9 119.84(16) . . ? N3 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? N3 C11 C12 119.69(17) . . ? N3 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C13 118.75(17) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C12 C13 C9 120.97(17) . . ? C12 C13 H13 119.5 . . ? C9 C13 H13 119.5 . . ? N2 C14 C8 119.77(16) . . ? N2 C14 H14 120.1 . . ? C8 C14 H14 120.1 . . ? N1 Fe1 S3 97.33(6) . . ? N1 Fe1 S2 98.09(5) . . ? S3 Fe1 S2 85.727(19) . . ? N1 Fe1 S4 104.17(5) . . ? S3 Fe1 S4 89.510(19) . . ? S2 Fe1 S4 157.65(2) . . ? N1 Fe1 S1 111.69(5) . . ? S3 Fe1 S1 150.92(2) . . ? S2 Fe1 S1 88.329(18) . . ? S4 Fe1 S1 85.282(18) . . ? O5 N1 Fe1 156.23(15) . . ? C14 N2 C5 123.16(15) . . ? C14 N2 H2 118.4 . . ? C5 N2 H2 118.4 . . ? C11 N3 C10 123.03(16) . . ? C11 N3 H3 118.5 . . ? C10 N3 H3 118.5 . . ? C1 S1 Fe1 107.01(6) . . ? C2 S2 Fe1 107.70(6) . . ? C3 S3 Fe1 105.89(6) . . ? C4 S4 Fe1 105.58(6) . . ? 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 O1 C1 C2 O2 0.8(3) . . . . ? S1 C1 C2 O2 -178.46(13) . . . . ? O1 C1 C2 S2 179.49(14) . . . . ? S1 C1 C2 S2 0.24(19) . . . . ? O3 C3 C4 O4 2.1(3) . . . . ? S3 C3 C4 O4 -175.71(13) . . . . ? O3 C3 C4 S4 -179.23(14) . . . . ? S3 C3 C4 S4 2.99(19) . . . . ? N2 C5 C6 C7 0.3(3) . . . . ? C5 C6 C7 C8 -1.0(3) . . . . ? C6 C7 C8 C14 0.9(3) . . . . ? C6 C7 C8 C9 179.83(17) . . . . ? C7 C8 C9 C10 28.7(2) . . . . ? C14 C8 C9 C10 -152.36(17) . . . . ? C7 C8 C9 C13 -151.21(18) . . . . ? C14 C8 C9 C13 27.7(2) . . . . ? C13 C9 C10 N3 -0.8(2) . . . . ? C8 C9 C10 N3 179.26(15) . . . . ? N3 C11 C12 C13 -0.8(3) . . . . ? C11 C12 C13 C9 -1.1(3) . . . . ? C10 C9 C13 C12 1.9(3) . . . . ? C8 C9 C13 C12 -178.18(17) . . . . ? C7 C8 C14 N2 -0.1(2) . . . . ? C9 C8 C14 N2 -179.08(15) . . . . ? S3 Fe1 N1 O5 -28.7(3) . . . . ? S2 Fe1 N1 O5 58.0(3) . . . . ? S4 Fe1 N1 O5 -120.1(3) . . . . ? S1 Fe1 N1 O5 149.4(3) . . . . ? C8 C14 N2 C5 -0.6(3) . . . . ? C6 C5 N2 C14 0.4(3) . . . . ? C12 C11 N3 C10 1.9(3) . . . . ? C9 C10 N3 C11 -1.1(3) . . . . ? O1 C1 S1 Fe1 173.41(15) . . . . ? C2 C1 S1 Fe1 -7.39(14) . . . . ? N1 Fe1 S1 C1 -89.03(8) . . . . ? S3 Fe1 S1 C1 87.14(7) . . . . ? S2 Fe1 S1 C1 9.01(6) . . . . ? S4 Fe1 S1 C1 167.58(6) . . . . ? O2 C2 S2 Fe1 -174.21(13) . . . . ? C1 C2 S2 Fe1 7.16(14) . . . . ? N1 Fe1 S2 C2 102.74(8) . . . . ? S3 Fe1 S2 C2 -160.45(6) . . . . ? S4 Fe1 S2 C2 -82.24(8) . . . . ? S1 Fe1 S2 C2 -8.94(6) . . . . ? O3 C3 S3 Fe1 169.74(15) . . . . ? C4 C3 S3 Fe1 -12.61(14) . . . . ? N1 Fe1 S3 C3 -90.61(8) . . . . ? S2 Fe1 S3 C3 171.76(6) . . . . ? S4 Fe1 S3 C3 13.61(6) . . . . ? S1 Fe1 S3 C3 92.98(7) . . . . ? O4 C4 S4 Fe1 -173.20(14) . . . . ? C3 C4 S4 Fe1 8.19(14) . . . . ? N1 Fe1 S4 C4 85.16(8) . . . . ? S3 Fe1 S4 C4 -12.28(7) . . . . ? S2 Fe1 S4 C4 -89.76(8) . . . . ? S1 Fe1 S4 C4 -163.64(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.501 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.075 #===END