# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Christophe Faulmann' 'Kane Jacob' 'Petra A. Szilagyi' 'Lydie Valade' _publ_contact_author_name 'Christophe Faulmann' _publ_contact_author_email CHRISTOPHE.FAULMANN@LCC-TOULOUSE.FR _publ_section_title ; Polymorphism and its effects on the magnetic properties of the [Fe(sal2-trien)][Ni(dmit)2] spin-crossover complex ; # Attachment 'm-1_180.cif' data_m-1_180 _database_code_depnum_ccdc_archive 'CCDC 729925' _audit_creation_method SHELXL-97 _chemical_name_systematic ; beta-(N,N'-3,6-diazaoctane-1,8-diylbis(salicylidenealdiminato))-iron(iii) bis(2-thioxo-1,3-dithiole-4,5-dithiolato)-nickel ; _chemical_name_common beta-[Fe(sal2-trien)][Ni(dmit)2] _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, C6 Ni S10' _chemical_formula_sum 'C26 H24 Fe N4 Ni O2 S10' _chemical_formula_weight 859.65 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 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 17.4443(8) _cell_length_b 10.6294(5) _cell_length_c 17.7187(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.511(4) _cell_angle_gamma 90.00 _cell_volume 3219.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 11350 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 32.1 _exptl_crystal_description 'thick plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.575 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.175 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 1.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4839 _exptl_absorpt_correction_T_max 0.8609 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'XCalibur Oxford Diffraction' _diffrn_measurement_method '\f scan' _diffrn_standards_decay_% negligible _diffrn_reflns_number 37828 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 32.29 _reflns_number_total 10845 _reflns_number_gt 8044 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction Ltd., 2003)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction Ltd., 2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction Ltd., 2003)' _computing_structure_solution 'Sir97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997); ; Cameron (Watkin, 1996)' _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^)+(0.0618P)^2^] 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 10845 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1111 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 0.665963(17) 0.25774(3) 0.452573(16) 0.01858(7) Uani 1 1 d . . . N1 N 0.65155(10) 0.08692(16) 0.50853(10) 0.0212(3) Uani 1 1 d . . . N2 N 0.76851(11) 0.24971(16) 0.54677(10) 0.0244(4) Uani 1 1 d . . . H2N H 0.7848 0.3313 0.5606 0.029 Uiso 1 1 calc R . . N3 N 0.75954(10) 0.21255(16) 0.39174(10) 0.0224(3) Uani 1 1 d . . . H3N H 0.7539 0.1293 0.3754 0.027 Uiso 1 1 calc R . . N4 N 0.69582(10) 0.43232(15) 0.41072(10) 0.0213(3) Uani 1 1 d . . . O1 O 0.58943(9) 0.19952(15) 0.36785(9) 0.0272(3) Uani 1 1 d . . . O2 O 0.60573(9) 0.34733(14) 0.51293(9) 0.0272(3) Uani 1 1 d . . . C1 C 0.54721(12) 0.0967(2) 0.35410(12) 0.0250(4) Uani 1 1 d . . . C2 C 0.49707(13) 0.0811(3) 0.28232(14) 0.0350(5) Uani 1 1 d . . . H2 H 0.4925 0.1463 0.2450 0.042 Uiso 1 1 calc R . . C3 C 0.45414(14) -0.0288(3) 0.26531(16) 0.0439(7) Uani 1 1 d . . . H3 H 0.4223 -0.0393 0.2156 0.053 Uiso 1 1 calc R . . C4 C 0.45682(15) -0.1230(3) 0.31932(17) 0.0437(7) Uani 1 1 d . . . H4 H 0.4265 -0.1972 0.3071 0.052 Uiso 1 1 calc R . . C5 C 0.50323(14) -0.1088(2) 0.39010(16) 0.0360(6) Uani 1 1 d . . . H5 H 0.5041 -0.1729 0.4276 0.043 Uiso 1 1 calc R . . C6 C 0.55029(12) -0.0005(2) 0.40927(13) 0.0256(4) Uani 1 1 d . . . C7 C 0.60059(12) 0.00179(19) 0.48352(13) 0.0250(4) Uani 1 1 d . . . H7 H 0.5959 -0.0657 0.5174 0.030 Uiso 1 1 calc R . . C8 C 0.70040(13) 0.0678(2) 0.58551(12) 0.0272(4) Uani 1 1 d . . . H8A H 0.7387 -0.0003 0.5835 0.033 Uiso 1 1 calc R . . H8B H 0.6671 0.0426 0.6221 0.033 Uiso 1 1 calc R . . C9 C 0.74321(14) 0.1887(2) 0.61261(12) 0.0310(5) Uani 1 1 d . . . H9A H 0.7082 0.2458 0.6342 0.037 Uiso 1 1 calc R . . H9B H 0.7893 0.1700 0.6536 0.037 Uiso 1 1 calc R . . C10 C 0.83265(13) 0.1821(2) 0.52136(13) 0.0307(5) Uani 1 1 d . . . H10A H 0.8224 0.0904 0.5201 0.037 Uiso 1 1 calc R . . H10B H 0.8827 0.1981 0.5577 0.037 Uiso 1 1 calc R . . C11 C 0.83769(13) 0.2280(2) 0.44206(14) 0.0287(5) Uani 1 1 d . . . H11A H 0.8534 0.3177 0.4442 0.034 Uiso 1 1 calc R . . H11B H 0.8771 0.1787 0.4216 0.034 Uiso 1 1 calc R . . C12 C 0.74606(13) 0.2952(2) 0.32318(12) 0.0271(4) Uani 1 1 d . . . H12A H 0.6970 0.2707 0.2877 0.032 Uiso 1 1 calc R . . H12B H 0.7897 0.2865 0.2954 0.032 Uiso 1 1 calc R . . C13 C 0.74047(13) 0.4295(2) 0.34867(12) 0.0261(4) Uani 1 1 d . . . H13A H 0.7935 0.4642 0.3674 0.031 Uiso 1 1 calc R . . H13B H 0.7139 0.4815 0.3048 0.031 Uiso 1 1 calc R . . C14 C 0.69098(12) 0.53906(19) 0.44490(12) 0.0236(4) Uani 1 1 d . . . H14 H 0.7156 0.6097 0.4270 0.028 Uiso 1 1 calc R . . C15 C 0.65133(12) 0.55935(19) 0.50796(12) 0.0237(4) Uani 1 1 d . . . C16 C 0.65459(14) 0.6808(2) 0.54016(14) 0.0312(5) Uani 1 1 d . . . H16 H 0.6828 0.7449 0.5202 0.037 Uiso 1 1 calc R . . C17 C 0.61807(15) 0.7084(2) 0.59939(15) 0.0338(5) Uani 1 1 d . . . H17 H 0.6220 0.7903 0.6212 0.041 Uiso 1 1 calc R . . C18 C 0.57504(14) 0.6156(2) 0.62777(14) 0.0331(5) Uani 1 1 d . . . H18 H 0.5483 0.6351 0.6681 0.040 Uiso 1 1 calc R . . C19 C 0.57101(13) 0.4954(2) 0.59764(13) 0.0305(5) Uani 1 1 d . . . H19 H 0.5416 0.4329 0.6176 0.037 Uiso 1 1 calc R . . C20 C 0.60972(11) 0.46431(19) 0.53809(12) 0.0225(4) Uani 1 1 d . . . Ni1 Ni 0.896968(15) 0.71396(2) 0.529404(14) 0.01919(7) Uani 1 1 d . . . S1 S 0.92216(4) 0.88810(5) 0.47837(3) 0.02760(12) Uani 1 1 d . . . S2 S 0.93709(3) 0.60309(5) 0.44289(3) 0.02479(11) Uani 1 1 d . . . S3 S 0.98777(3) 0.94594(5) 0.33757(3) 0.02476(11) Uani 1 1 d . . . S4 S 1.00586(3) 0.68194(5) 0.30496(3) 0.02558(11) Uani 1 1 d . . . S5 S 1.05829(4) 0.87206(6) 0.20447(3) 0.03462(14) Uani 1 1 d . . . S6 S 0.86147(3) 0.83097(5) 0.61591(3) 0.02454(11) Uani 1 1 d . . . S7 S 0.86463(3) 0.54115(4) 0.58037(3) 0.02163(10) Uani 1 1 d . . . S8 S 0.78667(3) 0.76684(5) 0.75001(3) 0.02560(12) Uani 1 1 d . . . S9 S 0.78578(3) 0.50201(5) 0.71747(3) 0.02694(12) Uani 1 1 d . . . S10 S 0.71360(4) 0.59453(6) 0.84630(4) 0.04060(16) Uani 1 1 d . . . C21 C 0.95704(12) 0.84093(19) 0.39982(11) 0.0211(4) Uani 1 1 d . . . C22 C 0.96499(12) 0.71505(19) 0.38458(11) 0.0202(4) Uani 1 1 d . . . C23 C 1.01913(12) 0.8363(2) 0.27858(12) 0.0227(4) Uani 1 1 d . . . C24 C 0.82691(11) 0.59762(19) 0.65679(11) 0.0204(4) Uani 1 1 d . . . C25 C 0.82661(12) 0.72286(19) 0.67164(11) 0.0210(4) Uani 1 1 d . . . C26 C 0.75931(13) 0.6193(2) 0.77511(12) 0.0253(4) 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 0.01828(14) 0.01766(14) 0.01972(14) 0.00067(10) 0.00359(10) -0.00047(10) N1 0.0217(8) 0.0193(8) 0.0229(8) 0.0006(7) 0.0055(7) 0.0021(6) N2 0.0253(9) 0.0233(9) 0.0226(9) -0.0037(7) -0.0003(7) -0.0037(7) N3 0.0234(9) 0.0222(8) 0.0226(8) -0.0027(7) 0.0074(7) -0.0009(6) N4 0.0213(8) 0.0195(8) 0.0227(8) 0.0048(7) 0.0033(7) -0.0007(6) O1 0.0235(8) 0.0308(8) 0.0251(8) 0.0024(6) -0.0004(6) -0.0047(6) O2 0.0279(8) 0.0192(7) 0.0383(9) -0.0002(6) 0.0155(7) 0.0009(6) C1 0.0163(9) 0.0320(11) 0.0278(11) -0.0076(9) 0.0068(8) -0.0023(8) C2 0.0240(11) 0.0530(15) 0.0275(11) -0.0070(11) 0.0043(9) -0.0059(10) C3 0.0239(12) 0.0656(19) 0.0410(15) -0.0239(14) 0.0037(10) -0.0105(12) C4 0.0298(13) 0.0432(15) 0.0598(18) -0.0255(13) 0.0131(12) -0.0136(11) C5 0.0275(12) 0.0299(12) 0.0537(16) -0.0134(11) 0.0151(11) -0.0050(9) C6 0.0212(10) 0.0241(10) 0.0327(11) -0.0086(9) 0.0084(8) -0.0025(8) C7 0.0262(11) 0.0190(9) 0.0318(11) 0.0004(8) 0.0105(9) 0.0009(8) C8 0.0299(11) 0.0269(11) 0.0245(10) 0.0073(8) 0.0045(8) 0.0045(8) C9 0.0361(13) 0.0369(13) 0.0190(10) -0.0003(9) 0.0028(9) -0.0008(10) C10 0.0214(11) 0.0369(12) 0.0326(12) 0.0046(10) 0.0026(9) 0.0041(9) C11 0.0195(10) 0.0339(12) 0.0337(12) 0.0049(9) 0.0078(8) 0.0028(8) C12 0.0248(11) 0.0396(12) 0.0184(9) -0.0004(9) 0.0083(8) -0.0058(9) C13 0.0265(11) 0.0291(11) 0.0240(10) 0.0064(8) 0.0084(8) -0.0013(8) C14 0.0208(10) 0.0211(10) 0.0276(10) 0.0056(8) 0.0017(8) -0.0015(7) C15 0.0208(10) 0.0213(10) 0.0270(10) 0.0034(8) -0.0002(8) 0.0007(7) C16 0.0327(12) 0.0209(10) 0.0387(13) 0.0017(9) 0.0043(10) 0.0007(9) C17 0.0419(14) 0.0207(10) 0.0377(13) -0.0052(9) 0.0052(10) 0.0049(9) C18 0.0360(13) 0.0329(12) 0.0318(12) -0.0009(10) 0.0097(10) 0.0089(10) C19 0.0321(12) 0.0256(11) 0.0358(12) 0.0020(9) 0.0118(10) 0.0056(9) C20 0.0190(10) 0.0210(9) 0.0271(10) 0.0022(8) 0.0036(8) 0.0042(7) Ni1 0.02215(14) 0.01606(13) 0.02082(13) 0.00034(9) 0.00777(10) -0.00088(9) S1 0.0421(3) 0.0160(2) 0.0304(3) -0.0003(2) 0.0209(2) -0.0006(2) S2 0.0368(3) 0.0162(2) 0.0243(2) 0.00038(19) 0.0130(2) -0.0002(2) S3 0.0310(3) 0.0202(2) 0.0260(3) 0.00358(19) 0.0125(2) 0.00004(19) S4 0.0344(3) 0.0228(2) 0.0219(2) 0.0008(2) 0.0114(2) 0.0042(2) S5 0.0384(3) 0.0400(3) 0.0311(3) 0.0103(2) 0.0203(2) 0.0080(3) S6 0.0340(3) 0.0158(2) 0.0275(3) -0.00028(19) 0.0147(2) -0.00164(19) S7 0.0266(3) 0.0161(2) 0.0239(2) -0.00100(18) 0.00912(19) -0.00190(18) S8 0.0320(3) 0.0228(2) 0.0248(3) -0.0023(2) 0.0124(2) -0.0027(2) S9 0.0330(3) 0.0210(2) 0.0300(3) 0.0022(2) 0.0139(2) -0.0040(2) S10 0.0531(4) 0.0364(3) 0.0414(3) 0.0077(3) 0.0312(3) 0.0015(3) C21 0.0205(9) 0.0223(10) 0.0209(9) 0.0011(8) 0.0053(7) -0.0029(7) C22 0.0194(9) 0.0234(10) 0.0178(9) 0.0010(7) 0.0039(7) 0.0007(7) C23 0.0192(9) 0.0259(10) 0.0228(10) 0.0052(8) 0.0036(7) 0.0022(8) C24 0.0188(9) 0.0217(9) 0.0209(9) 0.0028(7) 0.0042(7) -0.0022(7) C25 0.0202(9) 0.0240(10) 0.0196(9) 0.0005(7) 0.0060(7) -0.0014(7) C26 0.0256(10) 0.0261(11) 0.0254(10) 0.0045(8) 0.0079(8) -0.0023(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 O2 1.8982(15) . ? Fe1 O1 1.9024(15) . ? Fe1 N4 2.1021(16) . ? Fe1 N1 2.1078(17) . ? Fe1 N3 2.1816(17) . ? Fe1 N2 2.1913(17) . ? N1 C7 1.284(3) . ? N1 C8 1.471(3) . ? N2 C10 1.474(3) . ? N2 C9 1.477(3) . ? N2 H2N 0.9300 . ? N3 C12 1.480(3) . ? N3 C11 1.482(3) . ? N3 H3N 0.9300 . ? N4 C14 1.297(3) . ? N4 C13 1.469(3) . ? O1 C1 1.313(3) . ? O2 C20 1.318(2) . ? C1 C2 1.402(3) . ? C1 C6 1.416(3) . ? C2 C3 1.387(4) . ? C2 H2 0.9500 . ? C3 C4 1.380(4) . ? C3 H3 0.9500 . ? C4 C5 1.359(4) . ? C4 H4 0.9500 . ? C5 C6 1.415(3) . ? C5 H5 0.9500 . ? C6 C7 1.429(3) . ? C7 H7 0.9500 . ? C8 C9 1.515(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.507(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.506(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.443(3) . ? C14 H14 0.9500 . ? C15 C16 1.408(3) . ? C15 C20 1.410(3) . ? C16 C17 1.364(3) . ? C16 H16 0.9500 . ? C17 C18 1.392(4) . ? C17 H17 0.9500 . ? C18 C19 1.381(3) . ? C18 H18 0.9500 . ? C19 C20 1.401(3) . ? C19 H19 0.9500 . ? Ni1 S1 2.1437(6) . ? Ni1 S2 2.1578(6) . ? Ni1 S6 2.1584(6) . ? Ni1 S7 2.1706(5) . ? S1 C21 1.702(2) . ? S2 C22 1.709(2) . ? S3 C23 1.726(2) . ? S3 C21 1.728(2) . ? S4 C23 1.734(2) . ? S4 C22 1.739(2) . ? S5 C23 1.641(2) . ? S6 C25 1.704(2) . ? S7 C24 1.727(2) . ? S8 C26 1.723(2) . ? S8 C25 1.737(2) . ? S9 C26 1.732(2) . ? S9 C24 1.735(2) . ? S10 C26 1.642(2) . ? C21 C22 1.378(3) . ? C24 C25 1.357(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 O2 Fe1 O1 103.16(7) . . ? O2 Fe1 N4 87.70(7) . . ? O1 Fe1 N4 101.13(7) . . ? O2 Fe1 N1 92.05(6) . . ? O1 Fe1 N1 87.72(7) . . ? N4 Fe1 N1 170.98(7) . . ? O2 Fe1 N3 160.34(7) . . ? O1 Fe1 N3 90.86(7) . . ? N4 Fe1 N3 75.97(7) . . ? N1 Fe1 N3 102.36(6) . . ? O2 Fe1 N2 92.86(7) . . ? O1 Fe1 N2 157.83(7) . . ? N4 Fe1 N2 94.65(7) . . ? N1 Fe1 N2 76.35(7) . . ? N3 Fe1 N2 77.89(7) . . ? C7 N1 C8 117.12(18) . . ? C7 N1 Fe1 125.74(15) . . ? C8 N1 Fe1 116.98(13) . . ? C10 N2 C9 113.06(18) . . ? C10 N2 Fe1 109.90(13) . . ? C9 N2 Fe1 106.95(13) . . ? C10 N2 H2N 108.9 . . ? C9 N2 H2N 108.9 . . ? Fe1 N2 H2N 108.9 . . ? C12 N3 C11 113.86(17) . . ? C12 N3 Fe1 105.25(12) . . ? C11 N3 Fe1 111.57(13) . . ? C12 N3 H3N 108.7 . . ? C11 N3 H3N 108.7 . . ? Fe1 N3 H3N 108.7 . . ? C14 N4 C13 117.45(17) . . ? C14 N4 Fe1 124.32(14) . . ? C13 N4 Fe1 116.85(13) . . ? C1 O1 Fe1 134.13(14) . . ? C20 O2 Fe1 131.76(13) . . ? O1 C1 C2 119.5(2) . . ? O1 C1 C6 122.46(19) . . ? C2 C1 C6 118.1(2) . . ? C3 C2 C1 120.6(2) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 121.2(2) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.4(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.5(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 119.2(2) . . ? C5 C6 C7 117.1(2) . . ? C1 C6 C7 123.71(19) . . ? N1 C7 C6 125.9(2) . . ? N1 C7 H7 117.1 . . ? C6 C7 H7 117.1 . . ? N1 C8 C9 109.55(17) . . ? N1 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? N1 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? N2 C9 C8 109.16(17) . . ? N2 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? N2 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C11 108.42(18) . . ? N2 C10 H10A 110.0 . . ? C11 C10 H10A 110.0 . . ? N2 C10 H10B 110.0 . . ? C11 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? N3 C11 C10 107.90(18) . . ? N3 C11 H11A 110.1 . . ? C10 C11 H11A 110.1 . . ? N3 C11 H11B 110.1 . . ? C10 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? N3 C12 C13 109.01(17) . . ? N3 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? N3 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N4 C13 C12 108.63(17) . . ? N4 C13 H13A 110.0 . . ? C12 C13 H13A 110.0 . . ? N4 C13 H13B 110.0 . . ? C12 C13 H13B 110.0 . . ? H13A C13 H13B 108.3 . . ? N4 C14 C15 125.34(19) . . ? N4 C14 H14 117.3 . . ? C15 C14 H14 117.3 . . ? C16 C15 C20 119.1(2) . . ? C16 C15 C14 117.65(19) . . ? C20 C15 C14 123.29(19) . . ? C17 C16 C15 121.4(2) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 119.6(2) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 120.3(2) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.9(2) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? O2 C20 C19 118.44(19) . . ? O2 C20 C15 122.98(19) . . ? C19 C20 C15 118.6(2) . . ? S1 Ni1 S2 92.81(2) . . ? S1 Ni1 S6 85.07(2) . . ? S2 Ni1 S6 177.25(2) . . ? S1 Ni1 S7 176.75(2) . . ? S2 Ni1 S7 88.94(2) . . ? S6 Ni1 S7 93.27(2) . . ? C21 S1 Ni1 103.15(7) . . ? C22 S2 Ni1 102.77(7) . . ? C23 S3 C21 97.28(10) . . ? C23 S4 C22 97.21(10) . . ? C25 S6 Ni1 102.07(7) . . ? C24 S7 Ni1 101.74(7) . . ? C26 S8 C25 97.89(10) . . ? C26 S9 C24 97.80(10) . . ? C22 C21 S1 120.85(15) . . ? C22 C21 S3 116.50(15) . . ? S1 C21 S3 122.60(12) . . ? C21 C22 S2 120.38(15) . . ? C21 C22 S4 115.42(15) . . ? S2 C22 S4 124.19(12) . . ? S5 C23 S3 124.14(13) . . ? S5 C23 S4 122.27(13) . . ? S3 C23 S4 113.59(12) . . ? C25 C24 S7 120.65(16) . . ? C25 C24 S9 115.87(16) . . ? S7 C24 S9 123.47(12) . . ? C24 C25 S6 122.23(16) . . ? C24 C25 S8 115.88(15) . . ? S6 C25 S8 121.87(12) . . ? S10 C26 S8 123.09(14) . . ? S10 C26 S9 124.41(13) . . ? S8 C26 S9 112.50(12) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 32.29 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max '1.341 at 0.02 Ang. from Ni1' _refine_diff_density_min -0.609 _refine_diff_density_rms 0.107 # Attachment 'm-1_180.cif' data_m-1'_180 _database_code_depnum_ccdc_archive 'CCDC 729926' _audit_creation_method SHELXL-97 _chemical_name_systematic ; delta-(N,N'-3,6-diazaoctane-1,8-diylbis(salicylidenealdiminato))-iron(iii) bis(2-thioxo-1,3-dithiole-4,5-dithiolato)-nickel ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, C6 Ni S10' _chemical_formula_sum 'C26 H24 Fe N4 Ni O2 S10' _chemical_formula_weight 859.65 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 44.9352(18) _cell_length_b 13.5827(5) _cell_length_c 22.5430(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.386(2) _cell_angle_gamma 90.00 _cell_volume 13327.5(9) _cell_formula_units_Z 16 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 9858 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 31.01 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7008 _exptl_absorpt_coefficient_mu 1.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Bruker Apex2' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_decay_% negligible _diffrn_reflns_number 92000 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -65 _diffrn_reflns_limit_h_max 65 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 31.28 _reflns_number_total 21408 _reflns_number_gt 14482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Sir97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997); Diamond 3.1 (Brandenburg, 2008); Cameron (Watkin, 1996) ; _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^)+(0.0577P)^2^+30.9890P] 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 21408 _refine_ls_number_parameters 798 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.627738(9) 0.24191(3) 0.653519(18) 0.03359(9) Uani 1 1 d . . . O1 O 0.64908(5) 0.18891(19) 0.72959(10) 0.0489(6) Uani 1 1 d . . . O2 O 0.61946(5) 0.12642(16) 0.60701(12) 0.0453(5) Uani 1 1 d . . . N1 N 0.58790(5) 0.23356(18) 0.67719(11) 0.0346(5) Uani 1 1 d . . . N2 N 0.60060(6) 0.31675(19) 0.58090(11) 0.0415(6) Uani 1 1 d . . . H2N H 0.6079 0.3028 0.5467 0.050 Uiso 1 1 calc R . . N3 N 0.63785(8) 0.3810(2) 0.68636(13) 0.0556(8) Uani 1 1 d . . . H3N H 0.6350 0.3792 0.7258 0.067 Uiso 1 1 calc R . . N4 N 0.66828(7) 0.2538(2) 0.63330(13) 0.0519(7) Uani 1 1 d . . . C1 C 0.63938(7) 0.1703(2) 0.77880(14) 0.0386(6) Uani 1 1 d . . . C2 C 0.66111(8) 0.1405(3) 0.83237(16) 0.0507(8) Uani 1 1 d . . . H2 H 0.6822 0.1366 0.8322 0.061 Uiso 1 1 calc R . . C3 C 0.65231(9) 0.1172(3) 0.88468(17) 0.0571(9) Uani 1 1 d . . . H3 H 0.6674 0.0972 0.9202 0.068 Uiso 1 1 calc R . . C4 C 0.62176(10) 0.1223(3) 0.88642(16) 0.0598(10) Uani 1 1 d . . . H4 H 0.6158 0.1053 0.9227 0.072 Uiso 1 1 calc R . . C5 C 0.60014(8) 0.1522(3) 0.83538(15) 0.0476(7) Uani 1 1 d . . . H5 H 0.5792 0.1561 0.8368 0.057 Uiso 1 1 calc R . . C6 C 0.60823(7) 0.1772(2) 0.78112(13) 0.0366(6) Uani 1 1 d . . . C7 C 0.58411(6) 0.2073(2) 0.72932(13) 0.0354(6) Uani 1 1 d . . . H7 H 0.5637 0.2076 0.7343 0.042 Uiso 1 1 calc R . . C8 C 0.56047(7) 0.2633(3) 0.62958(15) 0.0453(7) Uani 1 1 d . . . H8A H 0.5527 0.3273 0.6404 0.054 Uiso 1 1 calc R . . H8B H 0.5440 0.2136 0.6261 0.054 Uiso 1 1 calc R . . C9 C 0.56935(7) 0.2718(3) 0.57030(14) 0.0458(7) Uani 1 1 d . . . H9A H 0.5542 0.3132 0.5415 0.055 Uiso 1 1 calc R . . H9B H 0.5694 0.2057 0.5518 0.055 Uiso 1 1 calc R . . C10 C 0.60257(11) 0.4234(3) 0.5901(2) 0.0697(12) Uani 1 1 d . . . H10A H 0.6165 0.4512 0.5666 0.084 Uiso 1 1 calc R . . H10B H 0.5820 0.4526 0.5737 0.084 Uiso 1 1 calc R . . C11 C 0.61330(15) 0.4501(3) 0.6519(2) 0.0933(18) Uani 1 1 d . . . H11A H 0.5959 0.4501 0.6715 0.112 Uiso 1 1 calc R . . H11B H 0.6217 0.5178 0.6544 0.112 Uiso 1 1 calc R . . C12 C 0.67055(14) 0.3984(4) 0.6952(2) 0.100(2) Uani 1 1 d . . . H12A H 0.6816 0.3737 0.7361 0.120 Uiso 1 1 calc R . . H12B H 0.6743 0.4701 0.6942 0.120 Uiso 1 1 calc R . . C13 C 0.68289(14) 0.3503(4) 0.6485(3) 0.103(2) Uani 1 1 d . . . H13A H 0.7054 0.3419 0.6639 0.123 Uiso 1 1 calc R . . H13B H 0.6790 0.3919 0.6113 0.123 Uiso 1 1 calc R . . C14 C 0.68265(7) 0.1836(3) 0.61428(14) 0.0513(9) Uani 1 1 d . . . H14 H 0.7034 0.1951 0.6137 0.062 Uiso 1 1 calc R . . C15 C 0.66981(7) 0.0894(3) 0.59390(13) 0.0418(7) Uani 1 1 d . . . C16 C 0.68832(8) 0.0186(3) 0.57472(15) 0.0532(9) Uani 1 1 d . . . H16 H 0.7094 0.0331 0.5782 0.064 Uiso 1 1 calc R . . C17 C 0.67689(8) -0.0707(3) 0.55122(16) 0.0563(9) Uani 1 1 d . . . H17 H 0.6899 -0.1179 0.5395 0.068 Uiso 1 1 calc R . . C18 C 0.64608(8) -0.0911(3) 0.54483(14) 0.0466(7) Uani 1 1 d . . . H18 H 0.6380 -0.1525 0.5281 0.056 Uiso 1 1 calc R . . C19 C 0.62704(7) -0.0236(2) 0.56244(14) 0.0403(6) Uani 1 1 d . . . H19 H 0.6059 -0.0387 0.5568 0.048 Uiso 1 1 calc R . . C20 C 0.63844(6) 0.0674(2) 0.58872(13) 0.0377(6) Uani 1 1 d . . . Fe2 Fe 0.871461(9) 0.24233(3) 0.777918(18) 0.03390(9) Uani 1 1 d . . . O21 O 0.88017(5) 0.12542(15) 0.74197(11) 0.0445(5) Uani 1 1 d . . . O22 O 0.84901(5) 0.1903(2) 0.83066(10) 0.0503(6) Uani 1 1 d . . . N21 N 0.83193(7) 0.2555(2) 0.71730(12) 0.0502(7) Uani 1 1 d . . . N22 N 0.86234(8) 0.3800(2) 0.80184(14) 0.0531(7) Uani 1 1 d . . . H22N H 0.8647 0.3775 0.8440 0.064 Uiso 1 1 calc R . . N23 N 0.89848(6) 0.31363(19) 0.73175(11) 0.0395(5) Uani 1 1 d . . . H23N H 0.8912 0.2979 0.6905 0.047 Uiso 1 1 calc R . . N24 N 0.91045(5) 0.23337(17) 0.84070(10) 0.0319(5) Uani 1 1 d . . . C21 C 0.86108(6) 0.0675(2) 0.70400(13) 0.0372(6) Uani 1 1 d . . . C22 C 0.87250(7) -0.0237(2) 0.68905(14) 0.0418(7) Uani 1 1 d . . . H22 H 0.8936 -0.0389 0.7048 0.050 Uiso 1 1 calc R . . C23 C 0.85367(8) -0.0908(3) 0.65220(14) 0.0474(8) Uani 1 1 d . . . H23 H 0.8618 -0.1524 0.6439 0.057 Uiso 1 1 calc R . . C24 C 0.82305(8) -0.0694(3) 0.62701(15) 0.0564(9) Uani 1 1 d . . . H24 H 0.8101 -0.1164 0.6020 0.068 Uiso 1 1 calc R . . C25 C 0.81167(7) 0.0201(3) 0.63858(14) 0.0534(9) Uani 1 1 d . . . H25 H 0.7908 0.0352 0.6203 0.064 Uiso 1 1 calc R . . C26 C 0.83000(6) 0.0907(3) 0.67676(13) 0.0410(7) Uani 1 1 d . . . C27 C 0.81751(7) 0.1861(3) 0.68411(14) 0.0504(9) Uani 1 1 d . . . H27 H 0.7968 0.1984 0.6625 0.061 Uiso 1 1 calc R . . C28 C 0.81823(13) 0.3530(4) 0.7172(2) 0.098(2) Uani 1 1 d . . . H28A H 0.8232 0.3937 0.6845 0.118 Uiso 1 1 calc R . . H28B H 0.7956 0.3468 0.7085 0.118 Uiso 1 1 calc R . . C29 C 0.82990(13) 0.4006(4) 0.7763(2) 0.0949(18) Uani 1 1 d . . . H29A H 0.8269 0.4727 0.7714 0.114 Uiso 1 1 calc R . . H29B H 0.8180 0.3774 0.8051 0.114 Uiso 1 1 calc R . . C30 C 0.88741(11) 0.4478(3) 0.79295(19) 0.0637(10) Uani 1 1 d . . . H30A H 0.8800 0.5167 0.7899 0.076 Uiso 1 1 calc R . . H30B H 0.9054 0.4430 0.8286 0.076 Uiso 1 1 calc R . . C31 C 0.89660(10) 0.4211(3) 0.73693(19) 0.0578(9) Uani 1 1 d . . . H31A H 0.9168 0.4508 0.7378 0.069 Uiso 1 1 calc R . . H31B H 0.8814 0.4475 0.7008 0.069 Uiso 1 1 calc R . . C32 C 0.92972(8) 0.2687(3) 0.75287(15) 0.0457(7) Uani 1 1 d . . . H32A H 0.9298 0.2021 0.7351 0.055 Uiso 1 1 calc R . . H32B H 0.9450 0.3096 0.7390 0.055 Uiso 1 1 calc R . . C33 C 0.93814(7) 0.2624(2) 0.82107(14) 0.0416(7) Uani 1 1 d . . . H33A H 0.9546 0.2131 0.8350 0.050 Uiso 1 1 calc R . . H33B H 0.9457 0.3270 0.8390 0.050 Uiso 1 1 calc R . . C34 C 0.91384(6) 0.2070(2) 0.89666(13) 0.0338(6) Uani 1 1 d . . . H34 H 0.9341 0.2061 0.9222 0.041 Uiso 1 1 calc R . . C35 C 0.88931(7) 0.1786(2) 0.92373(13) 0.0360(6) Uani 1 1 d . . . C36 C 0.89686(8) 0.1543(3) 0.98615(14) 0.0469(7) Uani 1 1 d . . . H36 H 0.9177 0.1581 1.0089 0.056 Uiso 1 1 calc R . . C37 C 0.87503(9) 0.1252(3) 1.01498(17) 0.0571(9) Uani 1 1 d . . . H37 H 0.8806 0.1085 1.0572 0.068 Uiso 1 1 calc R . . C38 C 0.84441(9) 0.1201(3) 0.98193(18) 0.0582(9) Uani 1 1 d . . . H38 H 0.8291 0.1004 1.0019 0.070 Uiso 1 1 calc R . . C39 C 0.83622(8) 0.1433(3) 0.92093(17) 0.0497(8) Uani 1 1 d . . . H39 H 0.8152 0.1396 0.8992 0.060 Uiso 1 1 calc R . . C40 C 0.85835(7) 0.1725(2) 0.88961(14) 0.0396(6) Uani 1 1 d . . . Ni1A Ni 0.7500 0.2500 0.0000 0.03153(11) Uani 1 2 d S . . S1A S 0.749439(19) 0.09890(5) -0.02786(4) 0.04066(16) Uani 1 1 d . . . S2A S 0.749948(18) 0.30489(5) -0.08983(4) 0.04215(17) Uani 1 1 d . . . S3A S 0.74939(2) 0.00715(6) -0.15063(4) 0.04442(18) Uani 1 1 d . . . S4A S 0.74955(2) 0.19709(7) -0.20803(4) 0.0499(2) Uani 1 1 d . . . S5A S 0.74949(3) 0.01442(9) -0.28199(5) 0.0661(3) Uani 1 1 d . . . C1A C 0.74943(6) 0.1093(2) -0.10364(14) 0.0357(6) Uani 1 1 d . . . C2A C 0.74957(6) 0.1987(2) -0.13047(14) 0.0370(6) Uani 1 1 d . . . C3A C 0.74957(7) 0.0698(3) -0.21707(16) 0.0462(7) Uani 1 1 d . . . Ni1B Ni 0.0000 0.51317(4) 0.7500 0.03482(11) Uani 1 2 d S . . S1B S 0.01035(2) 0.39682(6) 0.81725(4) 0.04377(18) Uani 1 1 d . . . S2B S 0.01040(2) 0.62812(6) 0.81840(4) 0.04576(18) Uani 1 1 d . . . S3B S 0.03143(2) 0.40306(7) 0.95517(4) 0.0486(2) Uani 1 1 d . . . S4B S 0.03216(2) 0.61571(7) 0.95727(4) 0.0519(2) Uani 1 1 d . . . S5B S 0.046033(19) 0.50513(8) 1.07502(4) 0.0527(2) Uani 1 1 d . . . C1B C 0.02157(7) 0.4611(2) 0.88418(14) 0.0392(6) Uani 1 1 d . . . C2B C 0.02184(7) 0.5615(2) 0.88513(14) 0.0405(7) Uani 1 1 d . . . C3B C 0.03722(7) 0.5083(3) 0.99980(15) 0.0444(7) Uani 1 1 d . . . Ni1C Ni 0.0000 0.0000 0.0000 0.03701(12) Uani 1 2 d S . . S1C S 0.01484(2) -0.11592(6) -0.05166(4) 0.04729(19) Uani 1 1 d . . . S2C S 0.00621(2) 0.11366(6) -0.06276(4) 0.04467(18) Uani 1 1 d . . . S3C S 0.03630(2) -0.10872(7) -0.16898(5) 0.0515(2) Uani 1 1 d . . . S4C S 0.02795(2) 0.10204(6) -0.17911(4) 0.04608(19) Uani 1 1 d . . . S5C S 0.046369(19) -0.00595(7) -0.27881(4) 0.0504(2) Uani 1 1 d . . . C1C C 0.02389(6) -0.0519(2) -0.11039(14) 0.0409(7) Uani 1 1 d . . . C2C C 0.01995(7) 0.0474(2) -0.11489(14) 0.0396(6) Uani 1 1 d . . . C3C C 0.03768(6) -0.0043(2) -0.21232(15) 0.0418(7) Uani 1 1 d . . . Ni1D Ni 0.7500 0.2500 0.5000 0.02608(9) Uani 1 2 d S . . S1D S 0.715649(16) 0.14320(5) 0.45773(3) 0.03500(15) Uani 1 1 d . . . S2D S 0.716348(15) 0.35932(5) 0.50785(3) 0.03535(15) Uani 1 1 d . . . S3D S 0.646138(16) 0.15280(6) 0.42779(3) 0.04006(16) Uani 1 1 d . . . S4D S 0.646862(16) 0.35504(6) 0.46777(4) 0.04073(17) Uani 1 1 d . . . S5D S 0.586843(18) 0.25711(9) 0.41681(4) 0.0579(3) Uani 1 1 d . . . C1D C 0.68227(6) 0.2056(2) 0.45549(12) 0.0302(5) Uani 1 1 d . . . C2D C 0.68255(6) 0.2991(2) 0.47644(12) 0.0313(5) Uani 1 1 d . . . C3D C 0.62463(6) 0.2549(2) 0.43640(13) 0.0404(7) 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 0.03209(19) 0.0396(2) 0.03065(19) 0.00130(16) 0.01080(15) -0.00600(16) O1 0.0304(10) 0.0700(16) 0.0456(12) 0.0143(11) 0.0081(9) 0.0047(10) O2 0.0330(10) 0.0354(11) 0.0685(15) -0.0049(10) 0.0144(10) -0.0036(9) N1 0.0299(10) 0.0367(12) 0.0359(12) -0.0023(10) 0.0058(9) 0.0034(9) N2 0.0538(15) 0.0423(14) 0.0276(11) 0.0005(10) 0.0086(11) 0.0014(12) N3 0.081(2) 0.0448(16) 0.0377(14) -0.0099(12) 0.0077(14) -0.0128(15) N4 0.0573(17) 0.0616(19) 0.0407(14) -0.0026(13) 0.0193(13) -0.0317(15) C1 0.0329(13) 0.0411(15) 0.0397(15) 0.0030(12) 0.0051(11) -0.0017(12) C2 0.0399(16) 0.054(2) 0.0516(19) 0.0060(16) -0.0011(14) 0.0017(15) C3 0.061(2) 0.058(2) 0.0436(18) 0.0091(16) -0.0030(16) 0.0000(18) C4 0.073(3) 0.068(2) 0.0374(17) 0.0065(17) 0.0119(17) -0.002(2) C5 0.0493(17) 0.055(2) 0.0403(16) 0.0006(14) 0.0151(14) -0.0020(15) C6 0.0396(14) 0.0344(14) 0.0361(14) -0.0023(11) 0.0100(12) -0.0016(12) C7 0.0313(12) 0.0361(14) 0.0393(15) -0.0038(12) 0.0097(11) -0.0015(11) C8 0.0344(14) 0.0545(19) 0.0445(17) 0.0004(14) 0.0049(12) 0.0102(13) C9 0.0435(16) 0.0535(19) 0.0353(15) -0.0029(14) 0.0002(13) 0.0064(14) C10 0.084(3) 0.0375(19) 0.077(3) 0.0066(18) 0.001(2) 0.0050(19) C11 0.154(5) 0.041(2) 0.066(3) -0.006(2) -0.006(3) 0.010(3) C12 0.126(4) 0.102(4) 0.084(3) -0.047(3) 0.048(3) -0.079(4) C13 0.123(4) 0.108(4) 0.096(4) -0.042(3) 0.064(3) -0.092(4) C14 0.0366(15) 0.084(3) 0.0353(15) 0.0098(17) 0.0124(13) -0.0192(17) C15 0.0320(13) 0.061(2) 0.0319(14) 0.0153(13) 0.0071(11) -0.0027(13) C16 0.0354(15) 0.090(3) 0.0355(16) 0.0123(17) 0.0121(13) 0.0093(17) C17 0.0501(19) 0.081(3) 0.0407(17) 0.0062(18) 0.0157(15) 0.0209(19) C18 0.0549(19) 0.0510(18) 0.0349(15) 0.0080(14) 0.0129(14) 0.0085(15) C19 0.0360(14) 0.0426(16) 0.0440(16) 0.0066(13) 0.0133(12) -0.0007(12) C20 0.0312(13) 0.0446(16) 0.0384(15) 0.0122(12) 0.0105(11) 0.0001(12) Fe2 0.0354(2) 0.0384(2) 0.02644(18) 0.00443(16) 0.00497(15) 0.00513(16) O21 0.0345(10) 0.0343(11) 0.0583(14) -0.0027(10) -0.0007(9) 0.0011(8) O22 0.0320(10) 0.0734(17) 0.0434(12) 0.0143(11) 0.0051(9) -0.0043(11) N21 0.0541(16) 0.0600(18) 0.0345(13) 0.0101(13) 0.0075(12) 0.0262(14) N22 0.075(2) 0.0452(15) 0.0461(16) -0.0023(12) 0.0272(15) 0.0130(14) N23 0.0531(15) 0.0385(13) 0.0291(11) 0.0017(10) 0.0144(11) -0.0023(11) N24 0.0311(10) 0.0336(11) 0.0314(11) -0.0024(9) 0.0084(9) -0.0037(9) C21 0.0332(13) 0.0410(15) 0.0358(14) 0.0096(12) 0.0054(11) -0.0031(12) C22 0.0393(15) 0.0436(16) 0.0407(16) 0.0054(13) 0.0067(13) -0.0039(13) C23 0.0557(19) 0.0511(18) 0.0366(16) 0.0003(14) 0.0141(14) -0.0139(15) C24 0.0508(19) 0.080(3) 0.0376(17) -0.0069(17) 0.0093(14) -0.0242(19) C25 0.0328(14) 0.093(3) 0.0331(15) 0.0048(17) 0.0051(12) -0.0139(17) C26 0.0303(13) 0.0601(19) 0.0318(14) 0.0125(13) 0.0064(11) -0.0019(13) C27 0.0338(14) 0.084(3) 0.0321(15) 0.0190(17) 0.0050(12) 0.0166(16) C28 0.113(4) 0.100(4) 0.065(3) -0.001(3) -0.010(3) 0.074(3) C29 0.103(4) 0.103(4) 0.073(3) -0.016(3) 0.012(3) 0.065(3) C30 0.090(3) 0.0426(19) 0.061(2) -0.0075(17) 0.024(2) 0.001(2) C31 0.075(2) 0.0379(17) 0.065(2) 0.0047(16) 0.026(2) -0.0027(17) C32 0.0470(17) 0.0514(18) 0.0438(17) -0.0034(14) 0.0211(14) -0.0028(14) C33 0.0352(14) 0.0475(17) 0.0434(16) 0.0010(13) 0.0122(12) -0.0055(13) C34 0.0319(12) 0.0345(14) 0.0328(13) -0.0030(11) 0.0039(10) 0.0001(11) C35 0.0367(14) 0.0376(14) 0.0333(14) 0.0022(11) 0.0080(11) 0.0021(12) C36 0.0492(17) 0.057(2) 0.0348(15) 0.0044(14) 0.0101(13) 0.0048(15) C37 0.064(2) 0.072(2) 0.0405(18) 0.0125(17) 0.0226(17) 0.0054(19) C38 0.060(2) 0.062(2) 0.062(2) 0.0101(18) 0.0329(19) 0.0004(18) C39 0.0407(16) 0.056(2) 0.056(2) 0.0108(16) 0.0183(15) -0.0008(15) C40 0.0339(13) 0.0423(16) 0.0431(16) 0.0071(13) 0.0106(12) 0.0005(12) Ni1A 0.0253(2) 0.0227(2) 0.0453(3) -0.00167(19) 0.00658(19) 0.00082(17) S1A 0.0502(4) 0.0243(3) 0.0482(4) -0.0018(3) 0.0136(3) 0.0004(3) S2A 0.0440(4) 0.0290(3) 0.0525(4) 0.0031(3) 0.0103(3) 0.0014(3) S3A 0.0467(4) 0.0384(4) 0.0487(4) -0.0098(3) 0.0128(3) -0.0010(3) S4A 0.0496(4) 0.0533(5) 0.0464(4) 0.0031(4) 0.0110(4) 0.0006(4) S5A 0.0668(6) 0.0840(7) 0.0489(5) -0.0176(5) 0.0169(5) -0.0014(5) C1A 0.0291(12) 0.0321(13) 0.0442(16) -0.0046(12) 0.0058(11) -0.0002(10) C2A 0.0246(11) 0.0395(15) 0.0450(16) -0.0010(12) 0.0053(11) 0.0014(11) C3A 0.0320(14) 0.0548(19) 0.0511(18) -0.0059(15) 0.0090(13) 0.0004(13) Ni1B 0.0300(2) 0.0369(3) 0.0408(3) 0.000 0.0149(2) 0.000 S1B 0.0566(5) 0.0378(4) 0.0382(4) -0.0035(3) 0.0142(3) 0.0081(3) S2B 0.0515(4) 0.0384(4) 0.0509(5) -0.0032(3) 0.0194(4) -0.0043(3) S3B 0.0542(5) 0.0511(5) 0.0382(4) -0.0046(3) 0.0070(3) 0.0211(4) S4B 0.0550(5) 0.0496(5) 0.0511(5) -0.0143(4) 0.0130(4) -0.0099(4) S5B 0.0357(4) 0.0777(6) 0.0413(4) -0.0144(4) 0.0030(3) 0.0062(4) C1B 0.0345(13) 0.0441(16) 0.0403(15) -0.0019(13) 0.0114(12) 0.0098(12) C2B 0.0331(13) 0.0496(17) 0.0402(15) -0.0081(13) 0.0120(12) -0.0044(13) C3B 0.0268(12) 0.059(2) 0.0457(17) -0.0102(14) 0.0064(12) 0.0077(13) Ni1C 0.0300(2) 0.0404(3) 0.0351(3) 0.0086(2) -0.0024(2) -0.0055(2) S1C 0.0468(4) 0.0420(4) 0.0520(5) 0.0139(4) 0.0102(4) 0.0039(3) S2C 0.0583(5) 0.0384(4) 0.0348(4) 0.0035(3) 0.0067(3) -0.0071(3) S3C 0.0469(4) 0.0477(5) 0.0621(5) 0.0072(4) 0.0176(4) 0.0090(4) S4C 0.0554(5) 0.0431(4) 0.0400(4) -0.0006(3) 0.0124(3) -0.0148(4) S5C 0.0357(4) 0.0671(6) 0.0492(5) -0.0037(4) 0.0121(3) -0.0014(4) C1C 0.0305(13) 0.0451(17) 0.0441(16) 0.0073(13) 0.0034(12) -0.0014(12) C2C 0.0349(14) 0.0434(16) 0.0370(15) 0.0049(12) 0.0022(11) -0.0105(12) C3C 0.0261(12) 0.0499(18) 0.0465(17) -0.0012(14) 0.0036(12) -0.0072(12) Ni1D 0.0264(2) 0.0278(2) 0.0242(2) -0.00032(17) 0.00671(16) -0.00083(17) S1D 0.0313(3) 0.0316(3) 0.0402(4) -0.0068(3) 0.0052(3) -0.0003(3) S2D 0.0305(3) 0.0316(3) 0.0442(4) -0.0084(3) 0.0098(3) -0.0017(3) S3D 0.0319(3) 0.0473(4) 0.0381(4) -0.0039(3) 0.0033(3) -0.0077(3) S4D 0.0307(3) 0.0478(4) 0.0450(4) -0.0014(3) 0.0120(3) 0.0054(3) S5D 0.0275(3) 0.0969(8) 0.0481(5) 0.0000(5) 0.0069(3) -0.0011(4) C1D 0.0279(11) 0.0355(13) 0.0266(12) 0.0014(10) 0.0059(9) -0.0015(10) C2D 0.0286(12) 0.0373(14) 0.0290(12) 0.0003(11) 0.0092(10) 0.0013(10) C3D 0.0304(13) 0.063(2) 0.0280(13) 0.0043(13) 0.0074(10) -0.0017(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.872(2) . ? Fe1 O1 1.887(2) . ? Fe1 N4 1.991(3) . ? Fe1 N1 1.994(2) . ? Fe1 N3 2.039(3) . ? Fe1 N2 2.051(2) . ? O1 C1 1.313(4) . ? O2 C20 1.309(4) . ? N1 C7 1.279(4) . ? N1 C8 1.475(4) . ? N2 C10 1.463(5) . ? N2 C9 1.495(4) . ? N3 C12 1.452(6) . ? N3 C11 1.509(6) . ? N4 C14 1.283(5) . ? N4 C13 1.469(5) . ? C1 C2 1.410(4) . ? C1 C6 1.417(4) . ? C2 C3 1.371(5) . ? C3 C4 1.385(6) . ? C4 C5 1.370(5) . ? C5 C6 1.402(4) . ? C6 C7 1.441(4) . ? C8 C9 1.491(5) . ? C10 C11 1.403(6) . ? C12 C13 1.460(7) . ? C14 C15 1.432(5) . ? C15 C16 1.408(5) . ? C15 C20 1.417(4) . ? C16 C17 1.371(6) . ? C17 C18 1.384(5) . ? C18 C19 1.378(5) . ? C19 C20 1.412(4) . ? Fe2 O21 1.868(2) . ? Fe2 O22 1.878(2) . ? Fe2 N21 1.962(3) . ? Fe2 N24 1.964(2) . ? Fe2 N22 2.017(3) . ? Fe2 N23 2.031(2) . ? O21 C21 1.313(4) . ? O22 C40 1.313(4) . ? N21 C27 1.276(5) . ? N21 C28 1.459(5) . ? N22 C29 1.455(6) . ? N22 C30 1.506(5) . ? N23 C31 1.469(4) . ? N23 C32 1.496(4) . ? N24 C34 1.284(4) . ? N24 C33 1.475(4) . ? C21 C22 1.412(5) . ? C21 C26 1.414(4) . ? C22 C23 1.374(4) . ? C23 C24 1.382(5) . ? C24 C25 1.369(6) . ? C25 C26 1.409(5) . ? C26 C27 1.438(5) . ? C28 C29 1.457(7) . ? C30 C31 1.468(5) . ? C32 C33 1.492(4) . ? C34 C35 1.439(4) . ? C35 C36 1.403(4) . ? C35 C40 1.415(4) . ? C36 C37 1.363(5) . ? C37 C38 1.394(6) . ? C38 C39 1.369(5) . ? C39 C40 1.412(4) . ? Ni1A S1A 2.1446(7) 7_655 ? Ni1A S1A 2.1446(7) . ? Ni1A S2A 2.1573(8) . ? Ni1A S2A 2.1573(8) 7_655 ? S1A C1A 1.714(3) . ? S2A C2A 1.707(3) . ? S3A C3A 1.725(4) . ? S3A C1A 1.745(3) . ? S4A C3A 1.740(4) . ? S4A C2A 1.748(3) . ? S5A C3A 1.645(3) . ? C1A C2A 1.357(4) . ? Ni1B S1B 2.1591(9) 2_556 ? Ni1B S1B 2.1591(9) . ? Ni1B S2B 2.1623(9) . ? Ni1B S2B 2.1623(9) 2_556 ? S1B C1B 1.707(3) . ? S2B C2B 1.721(3) . ? S3B C3B 1.730(3) . ? S3B C1B 1.740(3) . ? S4B C3B 1.730(4) . ? S4B C2B 1.740(3) . ? S5B C3B 1.643(3) . ? C1B C2B 1.365(5) . ? Ni1C S2C 2.1585(8) . ? Ni1C S2C 2.1585(8) 5 ? Ni1C S1C 2.1600(9) 5 ? Ni1C S1C 2.1600(9) . ? S1C C1C 1.715(3) . ? S2C C2C 1.712(3) . ? S3C C3C 1.732(3) . ? S3C C1C 1.737(3) . ? S4C C3C 1.732(3) . ? S4C C2C 1.742(3) . ? S5C C3C 1.640(4) . ? C1C C2C 1.362(5) . ? Ni1D S2D 2.1577(7) . ? Ni1D S2D 2.1577(7) 7_656 ? Ni1D S1D 2.1596(7) . ? Ni1D S1D 2.1596(7) 7_656 ? S1D C1D 1.713(3) . ? S2D C2D 1.716(3) . ? S3D C3D 1.729(3) . ? S3D C1D 1.743(3) . ? S4D C3D 1.731(3) . ? S4D C2D 1.741(3) . ? S5D C3D 1.645(3) . ? C1D C2D 1.354(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe1 O1 100.06(11) . . ? O2 Fe1 N4 90.30(11) . . ? O1 Fe1 N4 87.23(11) . . ? O2 Fe1 N1 92.04(10) . . ? O1 Fe1 N1 91.29(10) . . ? N4 Fe1 N1 177.42(11) . . ? O2 Fe1 N3 167.21(12) . . ? O1 Fe1 N3 90.37(12) . . ? N4 Fe1 N3 82.77(13) . . ? N1 Fe1 N3 95.14(12) . . ? O2 Fe1 N2 88.42(10) . . ? O1 Fe1 N2 168.89(11) . . ? N4 Fe1 N2 100.00(12) . . ? N1 Fe1 N2 81.17(10) . . ? N3 Fe1 N2 82.26(11) . . ? C1 O1 Fe1 129.84(19) . . ? C20 O2 Fe1 129.41(19) . . ? C7 N1 C8 117.8(2) . . ? C7 N1 Fe1 126.5(2) . . ? C8 N1 Fe1 115.65(19) . . ? C10 N2 C9 116.7(3) . . ? C10 N2 Fe1 112.0(2) . . ? C9 N2 Fe1 105.88(19) . . ? C12 N3 C11 123.7(4) . . ? C12 N3 Fe1 109.1(3) . . ? C11 N3 Fe1 108.7(2) . . ? C14 N4 C13 120.5(3) . . ? C14 N4 Fe1 125.6(2) . . ? C13 N4 Fe1 113.6(3) . . ? O1 C1 C2 118.3(3) . . ? O1 C1 C6 123.8(3) . . ? C2 C1 C6 117.9(3) . . ? C3 C2 C1 121.1(3) . . ? C2 C3 C4 120.8(3) . . ? C5 C4 C3 119.5(3) . . ? C4 C5 C6 121.4(3) . . ? C5 C6 C1 119.3(3) . . ? C5 C6 C7 118.0(3) . . ? C1 C6 C7 122.7(3) . . ? N1 C7 C6 125.3(3) . . ? N1 C8 C9 108.2(2) . . ? C8 C9 N2 109.7(3) . . ? C11 C10 N2 113.0(3) . . ? C10 C11 N3 112.2(4) . . ? N3 C12 C13 112.4(4) . . ? C12 C13 N4 109.9(3) . . ? N4 C14 C15 125.1(3) . . ? C16 C15 C20 118.9(3) . . ? C16 C15 C14 119.2(3) . . ? C20 C15 C14 121.9(3) . . ? C17 C16 C15 122.0(3) . . ? C16 C17 C18 119.2(3) . . ? C19 C18 C17 120.8(4) . . ? C18 C19 C20 121.2(3) . . ? O2 C20 C19 118.1(3) . . ? O2 C20 C15 123.9(3) . . ? C19 C20 C15 118.0(3) . . ? O21 Fe2 O22 99.09(11) . . ? O21 Fe2 N21 91.52(11) . . ? O22 Fe2 N21 86.52(11) . . ? O21 Fe2 N24 90.83(9) . . ? O22 Fe2 N24 92.51(9) . . ? N21 Fe2 N24 177.58(11) . . ? O21 Fe2 N22 169.38(11) . . ? O22 Fe2 N22 90.18(12) . . ? N21 Fe2 N22 83.84(13) . . ? N24 Fe2 N22 93.95(12) . . ? O21 Fe2 N23 88.09(10) . . ? O22 Fe2 N23 170.99(11) . . ? N21 Fe2 N23 98.79(12) . . ? N24 Fe2 N23 81.89(10) . . ? N22 Fe2 N23 83.21(12) . . ? C21 O21 Fe2 128.26(19) . . ? C40 O22 Fe2 128.54(19) . . ? C27 N21 C28 121.1(3) . . ? C27 N21 Fe2 125.5(2) . . ? C28 N21 Fe2 113.1(3) . . ? C29 N22 C30 122.6(4) . . ? C29 N22 Fe2 108.8(3) . . ? C30 N22 Fe2 108.8(2) . . ? C31 N23 C32 116.6(3) . . ? C31 N23 Fe2 112.3(2) . . ? C32 N23 Fe2 106.02(18) . . ? C34 N24 C33 117.8(2) . . ? C34 N24 Fe2 126.33(19) . . ? C33 N24 Fe2 115.81(18) . . ? O21 C21 C22 117.6(3) . . ? O21 C21 C26 124.3(3) . . ? C22 C21 C26 118.0(3) . . ? C23 C22 C21 121.3(3) . . ? C22 C23 C24 120.7(4) . . ? C25 C24 C23 119.2(3) . . ? C24 C25 C26 122.1(3) . . ? C25 C26 C21 118.6(3) . . ? C25 C26 C27 119.8(3) . . ? C21 C26 C27 121.5(3) . . ? N21 C27 C26 125.3(3) . . ? C29 C28 N21 110.2(3) . . ? N22 C29 C28 112.0(4) . . ? C31 C30 N22 110.1(3) . . ? C30 C31 N23 110.4(3) . . ? C33 C32 N23 109.2(3) . . ? N24 C33 C32 107.9(2) . . ? N24 C34 C35 125.1(3) . . ? C36 C35 C40 119.4(3) . . ? C36 C35 C34 118.0(3) . . ? C40 C35 C34 122.6(3) . . ? C37 C36 C35 121.6(3) . . ? C36 C37 C38 119.4(3) . . ? C39 C38 C37 120.6(3) . . ? C38 C39 C40 121.3(3) . . ? O22 C40 C39 118.0(3) . . ? O22 C40 C35 124.3(3) . . ? C39 C40 C35 117.7(3) . . ? S1A Ni1A S1A 180.00(4) 7_655 . ? S1A Ni1A S2A 86.64(3) 7_655 . ? S1A Ni1A S2A 93.36(3) . . ? S1A Ni1A S2A 93.36(3) 7_655 7_655 ? S1A Ni1A S2A 86.64(3) . 7_655 ? S2A Ni1A S2A 180.00(6) . 7_655 ? C1A S1A Ni1A 102.14(10) . . ? C2A S2A Ni1A 102.08(11) . . ? C3A S3A C1A 97.77(16) . . ? C3A S4A C2A 97.42(16) . . ? C2A C1A S1A 121.3(2) . . ? C2A C1A S3A 116.1(2) . . ? S1A C1A S3A 122.64(17) . . ? C1A C2A S2A 121.2(2) . . ? C1A C2A S4A 115.8(2) . . ? S2A C2A S4A 123.00(18) . . ? S5A C3A S3A 123.2(2) . . ? S5A C3A S4A 124.0(2) . . ? S3A C3A S4A 112.86(19) . . ? S1B Ni1B S1B 85.90(5) 2_556 . ? S1B Ni1B S2B 179.16(4) 2_556 . ? S1B Ni1B S2B 93.28(3) . . ? S1B Ni1B S2B 93.28(3) 2_556 2_556 ? S1B Ni1B S2B 179.16(4) . 2_556 ? S2B Ni1B S2B 87.55(5) . 2_556 ? C1B S1B Ni1B 102.19(12) . . ? C2B S2B Ni1B 102.03(11) . . ? C3B S3B C1B 97.36(16) . . ? C3B S4B C2B 97.41(16) . . ? C2B C1B S1B 121.6(2) . . ? C2B C1B S3B 116.1(2) . . ? S1B C1B S3B 122.2(2) . . ? C1B C2B S2B 120.8(2) . . ? C1B C2B S4B 115.9(2) . . ? S2B C2B S4B 123.2(2) . . ? S5B C3B S3B 122.8(2) . . ? S5B C3B S4B 124.0(2) . . ? S3B C3B S4B 113.24(19) . . ? S2C Ni1C S2C 180.00(6) . 5 ? S2C Ni1C S1C 86.54(3) . 5 ? S2C Ni1C S1C 93.46(3) 5 5 ? S2C Ni1C S1C 93.46(3) . . ? S2C Ni1C S1C 86.54(3) 5 . ? S1C Ni1C S1C 180.00(5) 5 . ? C1C S1C Ni1C 102.18(12) . . ? C2C S2C Ni1C 101.62(11) . . ? C3C S3C C1C 97.38(16) . . ? C3C S4C C2C 97.51(16) . . ? C2C C1C S1C 120.6(3) . . ? C2C C1C S3C 116.4(2) . . ? S1C C1C S3C 123.0(2) . . ? C1C C2C S2C 122.1(2) . . ? C1C C2C S4C 115.7(3) . . ? S2C C2C S4C 122.06(19) . . ? S5C C3C S3C 123.7(2) . . ? S5C C3C S4C 123.3(2) . . ? S3C C3C S4C 112.99(19) . . ? S2D Ni1D S2D 180.00(4) . 7_656 ? S2D Ni1D S1D 93.43(3) . . ? S2D Ni1D S1D 86.57(3) 7_656 . ? S2D Ni1D S1D 86.57(3) . 7_656 ? S2D Ni1D S1D 93.43(3) 7_656 7_656 ? S1D Ni1D S1D 180.00(4) . 7_656 ? C1D S1D Ni1D 101.85(9) . . ? C2D S2D Ni1D 101.80(10) . . ? C3D S3D C1D 97.27(14) . . ? C3D S4D C2D 97.17(14) . . ? C2D C1D S1D 121.4(2) . . ? C2D C1D S3D 116.0(2) . . ? S1D C1D S3D 122.56(16) . . ? C1D C2D S2D 121.5(2) . . ? C1D C2D S4D 116.2(2) . . ? S2D C2D S4D 122.29(17) . . ? S5D C3D S3D 123.5(2) . . ? S5D C3D S4D 123.2(2) . . ? S3D C3D S4D 113.22(16) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 31.28 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.290 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.103 # Attachment 'm-1_293.cif' data_m-1_293 _database_code_depnum_ccdc_archive 'CCDC 729927' _audit_creation_method SHELXL-97 _chemical_name_systematic ; beta-(N,N'-3,6-diazaoctane-1,8-diylbis(salicylidenealdiminato))-iron(iii) bis(2-thioxo-1,3-dithiole-4,5-dithiolato)-nickel ; _chemical_name_common beta-[Fe(sal2-trien)][Ni(dmit)2] _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, C6 Ni S10' _chemical_formula_sum 'C26 H24 Fe N4 Ni O2 S10' _chemical_formula_weight 859.65 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 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 17.5888(14) _cell_length_b 10.7316(8) _cell_length_c 17.7742(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.342(9) _cell_angle_gamma 90.00 _cell_volume 3289.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.9 _exptl_crystal_description 'thick plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.575 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.175 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 1.683 _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 0.5343 _exptl_absorpt_correction_T_max 0.6675 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS) equipped with an Oxford Cryosystems cooler device. The crystal-to-detector distance was 70 mm. 167 exposures (2.5 min per exposure) were obtained with 0 < \f < 251\% and with the crystals rotated through 1.5\% in \f. Crystal decay was monitored by measuring 200 reflexions per image. ; _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 Imaging Plate Diffraction System' _diffrn_measurement_method '\f scan ' _diffrn_standards_decay_% negligible _diffrn_reflns_number 45235 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.98 _reflns_number_total 6410 _reflns_number_gt 4680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS software (Stoe, 1996)' _computing_cell_refinement 'IPDS software (Stoe, 1996)' _computing_data_reduction 'IPDS software (Stoe, 1996)' _computing_structure_solution 'Sir97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997), Mercury (Bruno et al., 2002) and Cameron (Watkin, 1993) ; _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^)+(0.0381P)^2^] 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 6410 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _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 0.668150(18) 0.25857(3) 0.451708(19) 0.03221(9) Uani 1 1 d . . . N1 N 0.65309(11) 0.08912(18) 0.50691(11) 0.0373(5) Uani 1 1 d . . . N2 N 0.77045(12) 0.2476(2) 0.54462(12) 0.0425(5) Uani 1 1 d . . . H2N H 0.7866 0.3262 0.5587 0.051 Uiso 1 1 calc R . . N3 N 0.75967(11) 0.21361(19) 0.38971(12) 0.0406(5) Uani 1 1 d . . . H3N H 0.7535 0.1332 0.3733 0.049 Uiso 1 1 calc R . . N4 N 0.69728(11) 0.43227(19) 0.41030(11) 0.0367(5) Uani 1 1 d . . . O1 O 0.59138(10) 0.20302(17) 0.36766(10) 0.0475(4) Uani 1 1 d . . . O2 O 0.60970(10) 0.34680(16) 0.51327(11) 0.0487(5) Uani 1 1 d . . . C1 C 0.54833(14) 0.1015(3) 0.35399(15) 0.0441(6) Uani 1 1 d . . . C2 C 0.49814(16) 0.0891(4) 0.28266(17) 0.0651(9) Uani 1 1 d . . . H2 H 0.4946 0.1525 0.2465 0.078 Uiso 1 1 calc R . . C3 C 0.45382(19) -0.0178(4) 0.2662(2) 0.0838(12) Uani 1 1 d . . . H3 H 0.4217 -0.0262 0.2182 0.101 Uiso 1 1 calc R . . C4 C 0.4564(2) -0.1111(4) 0.3191(3) 0.0833(12) Uani 1 1 d . . . H4 H 0.4258 -0.1817 0.3072 0.100 Uiso 1 1 calc R . . C5 C 0.50368(17) -0.1004(3) 0.3889(2) 0.0649(9) Uani 1 1 d . . . H5 H 0.5051 -0.1640 0.4246 0.078 Uiso 1 1 calc R . . C6 C 0.55063(14) 0.0057(2) 0.40795(16) 0.0441(6) Uani 1 1 d . . . C7 C 0.60178(15) 0.0064(2) 0.48131(16) 0.0431(6) Uani 1 1 d . . . H7 H 0.5974 -0.0599 0.5138 0.052 Uiso 1 1 calc R . . C8 C 0.70217(16) 0.0684(3) 0.58293(16) 0.0519(7) Uani 1 1 d . . . H8A H 0.7389 0.0020 0.5800 0.062 Uiso 1 1 calc R . . H8B H 0.6702 0.0436 0.6191 0.062 Uiso 1 1 calc R . . C9 C 0.74504(18) 0.1862(3) 0.61002(16) 0.0569(8) Uani 1 1 d . . . H9A H 0.7115 0.2418 0.6316 0.068 Uiso 1 1 calc R . . H9B H 0.7898 0.1669 0.6497 0.068 Uiso 1 1 calc R . . C10 C 0.83306(15) 0.1816(3) 0.51864(17) 0.0571(8) Uani 1 1 d . . . H10A H 0.8231 0.0926 0.5174 0.068 Uiso 1 1 calc R . . H10B H 0.8818 0.1969 0.5537 0.068 Uiso 1 1 calc R . . C11 C 0.83781(14) 0.2267(3) 0.44004(17) 0.0556(7) Uani 1 1 d . . . H11A H 0.8540 0.3133 0.4422 0.067 Uiso 1 1 calc R . . H11B H 0.8756 0.1780 0.4196 0.067 Uiso 1 1 calc R . . C12 C 0.74676(16) 0.2962(3) 0.32211(14) 0.0476(7) Uani 1 1 d . . . H12A H 0.6990 0.2733 0.2875 0.057 Uiso 1 1 calc R . . H12B H 0.7891 0.2876 0.2948 0.057 Uiso 1 1 calc R . . C13 C 0.74187(15) 0.4289(3) 0.34816(16) 0.0475(7) Uani 1 1 d . . . H13A H 0.7936 0.4617 0.3665 0.057 Uiso 1 1 calc R . . H13B H 0.7165 0.4800 0.3055 0.057 Uiso 1 1 calc R . . C14 C 0.69051(14) 0.5369(2) 0.44326(15) 0.0410(6) Uani 1 1 d . . . H14 H 0.7132 0.6060 0.4251 0.049 Uiso 1 1 calc R . . C15 C 0.65091(14) 0.5573(2) 0.50592(15) 0.0394(6) Uani 1 1 d . . . C16 C 0.65217(17) 0.6784(2) 0.53662(18) 0.0542(7) Uani 1 1 d . . . H16 H 0.6788 0.7411 0.5166 0.065 Uiso 1 1 calc R . . C17 C 0.61517(18) 0.7056(3) 0.59511(18) 0.0616(8) Uani 1 1 d . . . H17 H 0.6172 0.7857 0.6153 0.074 Uiso 1 1 calc R . . C18 C 0.57473(18) 0.6130(3) 0.62413(18) 0.0593(8) Uani 1 1 d . . . H18 H 0.5485 0.6320 0.6633 0.071 Uiso 1 1 calc R . . C19 C 0.57250(16) 0.4938(3) 0.59638(17) 0.0513(7) Uani 1 1 d . . . H19 H 0.5450 0.4329 0.6169 0.062 Uiso 1 1 calc R . . C20 C 0.61143(14) 0.4627(2) 0.53721(15) 0.0391(6) Uani 1 1 d . . . Ni1 Ni 0.896896(17) 0.71368(3) 0.529089(17) 0.03296(8) Uani 1 1 d . . . S1 S 0.92292(4) 0.88640(6) 0.47886(4) 0.04785(18) Uani 1 1 d . . . S2 S 0.93724(4) 0.60431(6) 0.44260(4) 0.04369(16) Uani 1 1 d . . . S3 S 0.98836(4) 0.94445(6) 0.33840(4) 0.04325(16) Uani 1 1 d . . . S4 S 1.00551(4) 0.68320(6) 0.30513(4) 0.04470(16) Uani 1 1 d . . . S5 S 1.05803(5) 0.87224(8) 0.20542(4) 0.0599(2) Uani 1 1 d . . . S6 S 0.86036(4) 0.82941(6) 0.61499(4) 0.04394(16) Uani 1 1 d . . . S7 S 0.86494(4) 0.54202(5) 0.57995(4) 0.03814(15) Uani 1 1 d . . . S8 S 0.78546(4) 0.76491(6) 0.74847(4) 0.04557(16) Uani 1 1 d . . . S9 S 0.78648(4) 0.50278(6) 0.71658(4) 0.04731(17) Uani 1 1 d . . . S10 S 0.71407(6) 0.59357(8) 0.84477(5) 0.0718(3) Uani 1 1 d . . . C21 C 0.95768(13) 0.8391(2) 0.40040(13) 0.0343(5) Uani 1 1 d . . . C22 C 0.96495(13) 0.7160(2) 0.38483(13) 0.0333(5) Uani 1 1 d . . . C23 C 1.01938(13) 0.8355(2) 0.27955(14) 0.0393(6) Uani 1 1 d . . . C24 C 0.82697(13) 0.5978(2) 0.65570(13) 0.0346(5) Uani 1 1 d . . . C25 C 0.82542(13) 0.7215(2) 0.67023(14) 0.0365(5) Uani 1 1 d . . . C26 C 0.75962(15) 0.6185(2) 0.77369(15) 0.0446(6) 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 0.03310(17) 0.03100(18) 0.03301(18) 0.00065(15) 0.00771(14) -0.00086(14) N1 0.0405(11) 0.0348(11) 0.0378(11) 0.0018(9) 0.0106(9) 0.0017(9) N2 0.0445(12) 0.0428(12) 0.0370(11) -0.0049(10) -0.0002(9) -0.0055(10) N3 0.0434(11) 0.0409(12) 0.0408(12) -0.0060(10) 0.0160(10) -0.0008(9) N4 0.0355(11) 0.0389(12) 0.0363(11) 0.0071(9) 0.0088(9) -0.0001(9) O1 0.0401(10) 0.0553(11) 0.0438(10) 0.0033(9) 0.0005(8) -0.0081(9) O2 0.0539(11) 0.0365(10) 0.0636(12) -0.0010(9) 0.0306(9) -0.0013(8) C1 0.0287(12) 0.0598(17) 0.0451(15) -0.0161(14) 0.0105(11) -0.0040(12) C2 0.0405(16) 0.105(3) 0.0484(18) -0.0169(18) 0.0044(14) -0.0148(17) C3 0.0457(19) 0.138(4) 0.065(2) -0.043(3) 0.0038(17) -0.022(2) C4 0.057(2) 0.095(3) 0.100(3) -0.052(3) 0.023(2) -0.030(2) C5 0.0517(18) 0.0548(18) 0.094(3) -0.0246(18) 0.0289(18) -0.0135(14) C6 0.0336(13) 0.0444(15) 0.0579(18) -0.0149(13) 0.0176(13) -0.0040(11) C7 0.0457(15) 0.0314(13) 0.0577(18) -0.0005(12) 0.0234(14) 0.0009(12) C8 0.0541(16) 0.0561(17) 0.0465(16) 0.0148(14) 0.0128(13) 0.0056(14) C9 0.0618(18) 0.072(2) 0.0341(15) 0.0005(14) 0.0029(13) 0.0022(15) C10 0.0379(15) 0.074(2) 0.0569(18) 0.0057(16) 0.0034(13) 0.0061(14) C11 0.0334(14) 0.0693(19) 0.0666(19) 0.0148(16) 0.0160(13) 0.0101(13) C12 0.0475(15) 0.0642(18) 0.0339(14) -0.0026(13) 0.0150(12) -0.0064(13) C13 0.0444(15) 0.0561(16) 0.0454(16) 0.0123(14) 0.0176(12) -0.0040(13) C14 0.0379(13) 0.0355(14) 0.0481(16) 0.0098(12) 0.0049(12) -0.0020(11) C15 0.0353(13) 0.0365(13) 0.0446(15) 0.0025(12) 0.0039(11) 0.0056(11) C16 0.0616(18) 0.0366(14) 0.0657(19) 0.0010(14) 0.0158(15) 0.0013(13) C17 0.073(2) 0.0435(16) 0.069(2) -0.0099(16) 0.0163(17) 0.0110(15) C18 0.0671(19) 0.0539(18) 0.062(2) -0.0025(16) 0.0254(16) 0.0176(15) C19 0.0521(16) 0.0475(16) 0.0601(19) 0.0013(14) 0.0253(14) 0.0077(13) C20 0.0341(13) 0.0355(13) 0.0474(15) 0.0002(12) 0.0073(11) 0.0050(11) Ni1 0.03894(17) 0.02829(16) 0.03483(17) 0.00062(13) 0.01504(13) -0.00152(13) S1 0.0729(5) 0.0283(3) 0.0529(4) 0.0004(3) 0.0380(4) -0.0005(3) S2 0.0663(4) 0.0291(3) 0.0416(4) -0.0001(3) 0.0249(3) -0.0001(3) S3 0.0554(4) 0.0358(3) 0.0444(4) 0.0071(3) 0.0240(3) 0.0010(3) S4 0.0608(4) 0.0413(4) 0.0369(3) 0.0011(3) 0.0217(3) 0.0076(3) S5 0.0675(5) 0.0693(5) 0.0529(4) 0.0166(4) 0.0365(4) 0.0136(4) S6 0.0628(4) 0.0288(3) 0.0478(4) -0.0004(3) 0.0294(3) -0.0030(3) S7 0.0479(4) 0.0282(3) 0.0418(4) -0.0014(3) 0.0174(3) -0.0033(3) S8 0.0584(4) 0.0417(4) 0.0429(4) -0.0030(3) 0.0254(3) -0.0036(3) S9 0.0586(4) 0.0376(3) 0.0518(4) 0.0053(3) 0.0255(3) -0.0070(3) S10 0.0939(6) 0.0660(5) 0.0721(6) 0.0140(4) 0.0569(5) 0.0029(5) C21 0.0348(12) 0.0347(13) 0.0353(13) 0.0021(11) 0.0120(11) -0.0009(10) C22 0.0348(12) 0.0360(13) 0.0299(12) 0.0000(10) 0.0084(10) 0.0020(10) C23 0.0350(13) 0.0465(15) 0.0373(14) 0.0056(12) 0.0097(11) 0.0044(11) C24 0.0358(13) 0.0336(13) 0.0360(13) 0.0028(11) 0.0109(11) -0.0031(10) C25 0.0384(13) 0.0362(13) 0.0372(13) -0.0014(11) 0.0133(11) -0.0023(11) C26 0.0438(14) 0.0471(15) 0.0453(15) 0.0053(13) 0.0145(12) -0.0026(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.8956(17) . ? Fe1 O1 1.9018(17) . ? Fe1 N4 2.104(2) . ? Fe1 N1 2.108(2) . ? Fe1 N3 2.1763(19) . ? Fe1 N2 2.193(2) . ? N1 C7 1.283(3) . ? N1 C8 1.470(3) . ? N2 C10 1.459(3) . ? N2 C9 1.480(3) . ? N2 H2N 0.9100 . ? N3 C12 1.474(3) . ? N3 C11 1.492(3) . ? N3 H3N 0.9100 . ? N4 C14 1.283(3) . ? N4 C13 1.475(3) . ? O1 C1 1.322(3) . ? O2 C20 1.313(3) . ? C1 C6 1.401(4) . ? C1 C2 1.401(4) . ? C2 C3 1.385(5) . ? C2 H2 0.9300 . ? C3 C4 1.368(6) . ? C3 H3 0.9300 . ? C4 C5 1.356(5) . ? C4 H4 0.9300 . ? C5 C6 1.409(4) . ? C5 H5 0.9300 . ? C6 C7 1.431(4) . ? C7 H7 0.9300 . ? C8 C9 1.502(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.497(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.505(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.442(3) . ? C14 H14 0.9300 . ? C15 C20 1.405(3) . ? C15 C16 1.408(4) . ? C16 C17 1.362(4) . ? C16 H16 0.9300 . ? C17 C18 1.379(4) . ? C17 H17 0.9300 . ? C18 C19 1.369(4) . ? C18 H18 0.9300 . ? C19 C20 1.403(3) . ? C19 H19 0.9300 . ? Ni1 S1 2.1455(7) . ? Ni1 S6 2.1616(7) . ? Ni1 S2 2.1618(7) . ? Ni1 S7 2.1741(7) . ? S1 C21 1.707(2) . ? S2 C22 1.711(2) . ? S3 C23 1.727(3) . ? S3 C21 1.737(2) . ? S4 C23 1.727(3) . ? S4 C22 1.743(2) . ? S5 C23 1.645(2) . ? S6 C25 1.709(2) . ? S7 C24 1.724(2) . ? S8 C26 1.719(3) . ? S8 C25 1.740(2) . ? S9 C26 1.728(3) . ? S9 C24 1.738(2) . ? S10 C26 1.646(3) . ? C21 C22 1.360(3) . ? C24 C25 1.354(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 O2 Fe1 O1 103.19(8) . . ? O2 Fe1 N4 87.50(7) . . ? O1 Fe1 N4 100.78(8) . . ? O2 Fe1 N1 91.73(8) . . ? O1 Fe1 N1 87.73(8) . . ? N4 Fe1 N1 171.41(8) . . ? O2 Fe1 N3 160.42(8) . . ? O1 Fe1 N3 90.83(8) . . ? N4 Fe1 N3 76.35(8) . . ? N1 Fe1 N3 102.57(8) . . ? O2 Fe1 N2 92.87(8) . . ? O1 Fe1 N2 157.70(8) . . ? N4 Fe1 N2 95.22(8) . . ? N1 Fe1 N2 76.27(8) . . ? N3 Fe1 N2 77.90(8) . . ? C7 N1 C8 117.8(2) . . ? C7 N1 Fe1 125.13(18) . . ? C8 N1 Fe1 116.98(16) . . ? C10 N2 C9 113.3(2) . . ? C10 N2 Fe1 110.27(16) . . ? C9 N2 Fe1 106.60(16) . . ? C10 N2 H2N 108.8 . . ? C9 N2 H2N 108.8 . . ? Fe1 N2 H2N 108.8 . . ? C12 N3 C11 114.1(2) . . ? C12 N3 Fe1 105.59(15) . . ? C11 N3 Fe1 111.19(15) . . ? C12 N3 H3N 108.6 . . ? C11 N3 H3N 108.6 . . ? Fe1 N3 H3N 108.6 . . ? C14 N4 C13 118.3(2) . . ? C14 N4 Fe1 124.40(17) . . ? C13 N4 Fe1 116.22(16) . . ? C1 O1 Fe1 134.06(17) . . ? C20 O2 Fe1 132.82(16) . . ? O1 C1 C6 122.7(2) . . ? O1 C1 C2 118.7(3) . . ? C6 C1 C2 118.6(3) . . ? C3 C2 C1 119.8(4) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C4 C3 C2 121.3(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.9(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 119.4(3) . . ? C1 C6 C7 123.3(2) . . ? C5 C6 C7 117.2(3) . . ? N1 C7 C6 126.8(2) . . ? N1 C7 H7 116.6 . . ? C6 C7 H7 116.6 . . ? N1 C8 C9 109.5(2) . . ? N1 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? N1 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? N2 C9 C8 109.5(2) . . ? N2 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? N2 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? N2 C10 C11 108.8(2) . . ? N2 C10 H10A 109.9 . . ? C11 C10 H10A 109.9 . . ? N2 C10 H10B 109.9 . . ? C11 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N3 C11 C10 108.4(2) . . ? N3 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? N3 C11 H11B 110.0 . . ? C10 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N3 C12 C13 109.1(2) . . ? N3 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? N3 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N4 C13 C12 108.9(2) . . ? N4 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? N4 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N4 C14 C15 126.0(2) . . ? N4 C14 H14 117.0 . . ? C15 C14 H14 117.0 . . ? C20 C15 C16 119.0(2) . . ? C20 C15 C14 123.2(2) . . ? C16 C15 C14 117.8(2) . . ? C17 C16 C15 121.3(3) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 119.3(3) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? O2 C20 C19 119.0(2) . . ? O2 C20 C15 122.5(2) . . ? C19 C20 C15 118.5(2) . . ? S1 Ni1 S6 85.12(3) . . ? S1 Ni1 S2 92.66(3) . . ? S6 Ni1 S2 177.41(3) . . ? S1 Ni1 S7 177.25(3) . . ? S6 Ni1 S7 93.22(3) . . ? S2 Ni1 S7 89.05(3) . . ? C21 S1 Ni1 102.88(8) . . ? C22 S2 Ni1 102.62(8) . . ? C23 S3 C21 96.78(11) . . ? C23 S4 C22 97.14(11) . . ? C25 S6 Ni1 101.95(8) . . ? C24 S7 Ni1 101.66(8) . . ? C26 S8 C25 97.64(12) . . ? C26 S9 C24 97.88(12) . . ? C22 C21 S1 121.23(18) . . ? C22 C21 S3 116.72(17) . . ? S1 C21 S3 122.03(14) . . ? C21 C22 S2 120.59(17) . . ? C21 C22 S4 115.56(17) . . ? S2 C22 S4 123.84(14) . . ? S5 C23 S4 122.66(15) . . ? S5 C23 S3 123.54(16) . . ? S4 C23 S3 113.79(13) . . ? C25 C24 S7 120.99(18) . . ? C25 C24 S9 115.49(18) . . ? S7 C24 S9 123.50(14) . . ? C24 C25 S6 122.13(18) . . ? C24 C25 S8 116.18(18) . . ? S6 C25 S8 121.69(14) . . ? S10 C26 S8 122.84(16) . . ? S10 C26 S9 124.40(16) . . ? S8 C26 S9 112.76(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.297 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.060 # Attachment 'm-1_295.cif' data_m-1'_295 _database_code_depnum_ccdc_archive 'CCDC 729928' _audit_creation_method SHELXL-97 _chemical_name_systematic ; delta-(N,N'-3,6-diazaoctane-1,8-diylbis(salicylidenealdiminato))-iron(iii) bis(2-thioxo-1,3-dithiole-4,5-dithiolato)-nickel ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, C6 Ni S10' _chemical_formula_sum 'C26 H24 Fe N4 Ni O2 S10' _chemical_formula_weight 859.65 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' Ni Ni 0.3393 1.1124 '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 ' 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 45.1691(11) _cell_length_b 13.7916(3) _cell_length_c 22.6893(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.5410(10) _cell_angle_gamma 90.00 _cell_volume 13681.6(6) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9856 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.61 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7008 _exptl_absorpt_coefficient_mu 1.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker Apex2' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_decay_% negligible _diffrn_reflns_number 83938 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -57 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 26.78 _reflns_number_total 14573 _reflns_number_gt 9032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Sir97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997); Diamond 3.1 (Brandenburg, 2008); Cameron (Watkin, 1996) ; _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^)+(0.0793P)^2^+21.9716P] 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 14573 _refine_ls_number_parameters 798 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1623 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.003 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 0.628303(15) 0.24473(5) 0.65753(3) 0.06429(18) Uani 1 1 d . . . O1 O 0.64770(7) 0.2009(3) 0.73705(16) 0.0896(11) Uani 1 1 d . . . O2 O 0.62222(7) 0.1304(2) 0.61096(18) 0.0846(10) Uani 1 1 d . . . N1 N 0.58693(8) 0.2364(3) 0.68137(17) 0.0641(9) Uani 1 1 d . . . N2 N 0.59836(10) 0.3177(3) 0.58265(17) 0.0780(11) Uani 1 1 d . . . H2N H 0.6053 0.3060 0.5490 0.094 Uiso 1 1 calc R . . N3 N 0.63898(12) 0.3918(3) 0.68241(19) 0.0920(14) Uani 1 1 d . . . H3N H 0.6368 0.3984 0.7210 0.110 Uiso 1 1 calc R . . N4 N 0.67110(10) 0.2548(3) 0.6389(2) 0.0845(13) Uani 1 1 d . . . C1 C 0.63790(11) 0.1787(3) 0.7852(2) 0.0687(12) Uani 1 1 d . . . C2 C 0.65922(13) 0.1492(4) 0.8384(3) 0.0864(15) Uani 1 1 d . . . H2 H 0.6799 0.1481 0.8393 0.104 Uiso 1 1 calc R . . C3 C 0.65001(17) 0.1221(5) 0.8886(3) 0.1053(19) Uani 1 1 d . . . H3 H 0.6644 0.1023 0.9234 0.126 Uiso 1 1 calc R . . C4 C 0.61958(18) 0.1239(6) 0.8883(3) 0.119(2) Uani 1 1 d . . . H4 H 0.6134 0.1044 0.9226 0.143 Uiso 1 1 calc R . . C5 C 0.59843(14) 0.1542(5) 0.8376(2) 0.0953(17) Uani 1 1 d . . . H5 H 0.5779 0.1562 0.8380 0.114 Uiso 1 1 calc R . . C6 C 0.60695(11) 0.1824(3) 0.7851(2) 0.0666(11) Uani 1 1 d . . . C7 C 0.58316(11) 0.2107(3) 0.7331(2) 0.0676(11) Uani 1 1 d . . . H7 H 0.5632 0.2102 0.7375 0.081 Uiso 1 1 calc R . . C8 C 0.55983(11) 0.2624(4) 0.6327(2) 0.0837(15) Uani 1 1 d . . . H8A H 0.5519 0.3244 0.6419 0.100 Uiso 1 1 calc R . . H8B H 0.5440 0.2140 0.6302 0.100 Uiso 1 1 calc R . . C9 C 0.56824(13) 0.2685(4) 0.5735(2) 0.0916(17) Uani 1 1 d . . . H9A H 0.5527 0.3047 0.5444 0.110 Uiso 1 1 calc R . . H9B H 0.5694 0.2039 0.5573 0.110 Uiso 1 1 calc R . . C10 C 0.59890(19) 0.4220(5) 0.5918(4) 0.129(3) Uani 1 1 d . . . H10A H 0.6060 0.4522 0.5592 0.155 Uiso 1 1 calc R . . H10B H 0.5781 0.4437 0.5882 0.155 Uiso 1 1 calc R . . C11 C 0.6162(3) 0.4539(5) 0.6447(4) 0.199(6) Uani 1 1 d . . . H11A H 0.6026 0.4745 0.6691 0.239 Uiso 1 1 calc R . . H11B H 0.6267 0.5115 0.6360 0.239 Uiso 1 1 calc R . . C12 C 0.6701(2) 0.4089(8) 0.6859(6) 0.235(7) Uani 1 1 d . . . H12A H 0.6715 0.4724 0.6684 0.283 Uiso 1 1 calc R . . H12B H 0.6805 0.4135 0.7288 0.283 Uiso 1 1 calc R . . C13 C 0.68687(19) 0.3459(6) 0.6597(4) 0.148(3) Uani 1 1 d . . . H13A H 0.7060 0.3314 0.6891 0.177 Uiso 1 1 calc R . . H13B H 0.6918 0.3779 0.6253 0.177 Uiso 1 1 calc R . . C14 C 0.68464(12) 0.1851(5) 0.6185(2) 0.0839(16) Uani 1 1 d . . . H14 H 0.7050 0.1950 0.6186 0.101 Uiso 1 1 calc R . . C15 C 0.67150(10) 0.0942(4) 0.5957(2) 0.0711(13) Uani 1 1 d . . . C16 C 0.68974(12) 0.0252(6) 0.5753(2) 0.0947(19) Uani 1 1 d . . . H16 H 0.7102 0.0390 0.5781 0.114 Uiso 1 1 calc R . . C17 C 0.67776(15) -0.0616(5) 0.5514(3) 0.0997(19) Uani 1 1 d . . . H17 H 0.6901 -0.1069 0.5388 0.120 Uiso 1 1 calc R . . C18 C 0.64805(14) -0.0813(4) 0.5462(2) 0.0857(15) Uani 1 1 d . . . H18 H 0.6400 -0.1403 0.5297 0.103 Uiso 1 1 calc R . . C19 C 0.62943(12) -0.0160(4) 0.5648(2) 0.0741(13) Uani 1 1 d . . . H19 H 0.6088 -0.0307 0.5597 0.089 Uiso 1 1 calc R . . C20 C 0.64077(10) 0.0722(4) 0.5914(2) 0.0653(11) Uani 1 1 d . . . Fe2 Fe 0.871506(15) 0.24367(5) 0.78070(3) 0.06543(18) Uani 1 1 d . . . O21 O 0.87764(7) 0.1296(2) 0.74049(17) 0.0860(10) Uani 1 1 d . . . O22 O 0.85131(7) 0.1991(3) 0.83927(16) 0.0864(10) Uani 1 1 d . . . N21 N 0.82922(11) 0.2546(4) 0.7190(2) 0.0875(13) Uani 1 1 d . . . N22 N 0.86118(12) 0.3899(3) 0.7954(2) 0.0944(14) Uani 1 1 d . . . H22N H 0.8638 0.3964 0.8363 0.113 Uiso 1 1 calc R . . N23 N 0.90181(11) 0.3156(3) 0.73688(18) 0.0808(12) Uani 1 1 d . . . H23N H 0.8950 0.3038 0.6963 0.097 Uiso 1 1 calc R . . N24 N 0.91208(8) 0.2350(3) 0.84620(17) 0.0632(9) Uani 1 1 d . . . C21 C 0.85897(10) 0.0715(4) 0.70193(19) 0.0668(11) Uani 1 1 d . . . C22 C 0.87013(12) -0.0171(4) 0.6874(2) 0.0744(13) Uani 1 1 d . . . H22 H 0.8907 -0.0321 0.7032 0.089 Uiso 1 1 calc R . . C23 C 0.85145(14) -0.0828(4) 0.6504(2) 0.0867(15) Uani 1 1 d . . . H23 H 0.8593 -0.1423 0.6422 0.104 Uiso 1 1 calc R . . C24 C 0.82180(16) -0.0616(6) 0.6259(3) 0.105(2) Uani 1 1 d . . . H24 H 0.8093 -0.1064 0.6007 0.126 Uiso 1 1 calc R . . C25 C 0.80991(12) 0.0250(6) 0.6376(2) 0.098(2) Uani 1 1 d . . . H25 H 0.7894 0.0385 0.6200 0.118 Uiso 1 1 calc R . . C26 C 0.82828(11) 0.0950(4) 0.6762(2) 0.0740(13) Uani 1 1 d . . . C27 C 0.81554(12) 0.1867(5) 0.6853(2) 0.0883(18) Uani 1 1 d . . . H27 H 0.7953 0.1976 0.6647 0.106 Uiso 1 1 calc R . . C28 C 0.8140(2) 0.3472(6) 0.7233(4) 0.154(4) Uani 1 1 d . . . H28A H 0.8109 0.3809 0.6847 0.185 Uiso 1 1 calc R . . H28B H 0.7940 0.3341 0.7300 0.185 Uiso 1 1 calc R . . C29 C 0.8298(3) 0.4073(8) 0.7690(6) 0.232(7) Uani 1 1 d . . . H29A H 0.8193 0.4058 0.8015 0.278 Uiso 1 1 calc R . . H29B H 0.8279 0.4729 0.7530 0.278 Uiso 1 1 calc R . . C30 C 0.8836(2) 0.4523(5) 0.7794(5) 0.181(5) Uani 1 1 d . . . H30A H 0.8728 0.5084 0.7588 0.217 Uiso 1 1 calc R . . H30B H 0.8970 0.4755 0.8172 0.217 Uiso 1 1 calc R . . C31 C 0.9014(2) 0.4200(4) 0.7453(4) 0.133(3) Uani 1 1 d . . . H31A H 0.9221 0.4413 0.7633 0.160 Uiso 1 1 calc R . . H31B H 0.8949 0.4501 0.7055 0.160 Uiso 1 1 calc R . . C32 C 0.93166(13) 0.2659(4) 0.7584(3) 0.0881(16) Uani 1 1 d . . . H32A H 0.9473 0.3017 0.7452 0.106 Uiso 1 1 calc R . . H32B H 0.9304 0.2013 0.7409 0.106 Uiso 1 1 calc R . . C33 C 0.93993(11) 0.2591(4) 0.8260(2) 0.0789(14) Uani 1 1 d . . . H33A H 0.9553 0.2092 0.8393 0.095 Uiso 1 1 calc R . . H33B H 0.9483 0.3204 0.8436 0.095 Uiso 1 1 calc R . . C34 C 0.91560(10) 0.2113(3) 0.9022(2) 0.0675(11) Uani 1 1 d . . . H34 H 0.9354 0.2115 0.9270 0.081 Uiso 1 1 calc R . . C35 C 0.89129(10) 0.1846(3) 0.9296(2) 0.0664(11) Uani 1 1 d . . . C36 C 0.89909(13) 0.1587(5) 0.9913(2) 0.0938(17) Uani 1 1 d . . . H36 H 0.9195 0.1609 1.0128 0.113 Uiso 1 1 calc R . . C37 C 0.87793(17) 0.1307(6) 1.0208(3) 0.121(2) Uani 1 1 d . . . H37 H 0.8838 0.1138 1.0618 0.145 Uiso 1 1 calc R . . C38 C 0.84774(16) 0.1276(5) 0.9893(3) 0.107(2) Uani 1 1 d . . . H38 H 0.8331 0.1080 1.0091 0.129 Uiso 1 1 calc R . . C39 C 0.83892(13) 0.1526(4) 0.9295(3) 0.0877(15) Uani 1 1 d . . . H39 H 0.8183 0.1516 0.9093 0.105 Uiso 1 1 calc R . . C40 C 0.86069(11) 0.1801(4) 0.8977(2) 0.0697(12) Uani 1 1 d . . . Ni1A Ni 0.7500 0.2500 0.0000 0.05536(19) Uani 1 2 d S . . S1A S 0.74954(3) 0.10082(8) -0.02697(6) 0.0732(3) Uani 1 1 d . . . S2A S 0.75028(3) 0.30258(8) -0.08931(6) 0.0765(3) Uani 1 1 d . . . S3A S 0.74950(3) 0.00947(9) -0.14862(6) 0.0784(4) Uani 1 1 d . . . S4A S 0.74998(3) 0.19505(11) -0.20602(6) 0.0842(4) Uani 1 1 d . . . S5A S 0.74958(4) 0.01500(14) -0.27916(7) 0.1047(5) Uani 1 1 d . . . C1A C 0.74957(9) 0.1102(3) -0.1022(2) 0.0578(10) Uani 1 1 d . . . C2A C 0.74993(9) 0.1977(3) -0.1291(2) 0.0614(10) Uani 1 1 d . . . C3A C 0.74964(10) 0.0704(4) -0.2151(2) 0.0736(12) Uani 1 1 d . . . Ni1B Ni 0.0000 0.51330(6) 0.7500 0.0647(2) Uani 1 2 d S . . S1B S 0.01127(3) 0.39954(10) 0.81725(6) 0.0806(4) Uani 1 1 d . . . S2B S 0.00961(3) 0.62667(10) 0.81769(7) 0.0843(4) Uani 1 1 d . . . S3B S 0.03241(3) 0.40739(11) 0.95450(6) 0.0899(4) Uani 1 1 d . . . S4B S 0.03144(4) 0.61606(12) 0.95579(7) 0.0958(4) Uani 1 1 d . . . S5B S 0.04701(3) 0.50893(13) 1.07341(7) 0.0996(5) Uani 1 1 d . . . C1B C 0.02189(10) 0.4634(4) 0.8836(2) 0.0695(12) Uani 1 1 d . . . C2B C 0.02142(10) 0.5624(4) 0.8839(2) 0.0703(12) Uani 1 1 d . . . C3B C 0.03781(10) 0.5107(4) 0.9985(2) 0.0810(15) Uani 1 1 d . . . Ni1C Ni 0.0000 0.0000 0.0000 0.0647(2) Uani 1 2 d S . . S1C S 0.01343(3) -0.11549(10) -0.05216(6) 0.0820(4) Uani 1 1 d . . . S2C S 0.00760(3) 0.11109(10) -0.06163(6) 0.0820(4) Uani 1 1 d . . . S3C S 0.03514(3) -0.11045(11) -0.16835(7) 0.0903(4) Uani 1 1 d . . . S4C S 0.02902(4) 0.09728(11) -0.17742(6) 0.0873(4) Uani 1 1 d . . . S5C S 0.04723(3) -0.01061(13) -0.27588(7) 0.0940(5) Uani 1 1 d . . . C1C C 0.02318(10) -0.0543(4) -0.1101(2) 0.0709(12) Uani 1 1 d . . . C2C C 0.02034(10) 0.0446(4) -0.11415(19) 0.0686(12) Uani 1 1 d . . . C3C C 0.03799(11) -0.0080(4) -0.2101(2) 0.0776(14) Uani 1 1 d . . . Ni1D Ni 0.7500 0.2500 0.5000 0.05097(18) Uani 1 2 d S . . S1D S 0.71584(3) 0.14682(8) 0.45506(6) 0.0679(3) Uani 1 1 d . . . S2D S 0.71640(3) 0.35542(8) 0.51065(6) 0.0680(3) Uani 1 1 d . . . S3D S 0.64672(3) 0.15591(11) 0.42510(6) 0.0802(4) Uani 1 1 d . . . S4D S 0.64733(3) 0.35104(11) 0.47050(6) 0.0813(4) Uani 1 1 d . . . S5D S 0.58778(3) 0.25597(16) 0.41708(8) 0.1168(6) Uani 1 1 d . . . C1D C 0.68279(10) 0.2070(3) 0.45458(18) 0.0591(10) Uani 1 1 d . . . C2D C 0.68273(10) 0.2969(3) 0.47734(18) 0.0593(10) Uani 1 1 d . . . C3D C 0.62526(12) 0.2544(4) 0.4363(2) 0.0798(15) 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 0.0623(4) 0.0754(4) 0.0597(4) -0.0004(3) 0.0238(3) -0.0073(3) O1 0.057(2) 0.128(3) 0.083(2) 0.027(2) 0.0159(17) 0.0031(19) O2 0.0590(19) 0.079(2) 0.124(3) -0.017(2) 0.0366(19) -0.0101(16) N1 0.056(2) 0.076(2) 0.059(2) -0.0018(18) 0.0134(17) 0.0064(17) N2 0.099(3) 0.086(3) 0.051(2) 0.0024(19) 0.023(2) 0.011(2) N3 0.136(4) 0.081(3) 0.063(2) -0.010(2) 0.034(3) -0.022(3) N4 0.077(3) 0.107(3) 0.073(3) 0.003(2) 0.025(2) -0.040(3) C1 0.068(3) 0.074(3) 0.062(3) 0.003(2) 0.014(2) -0.003(2) C2 0.075(3) 0.096(4) 0.082(4) 0.007(3) 0.007(3) 0.003(3) C3 0.109(5) 0.124(5) 0.072(4) 0.010(3) 0.002(3) 0.007(4) C4 0.124(6) 0.169(7) 0.066(4) 0.026(4) 0.025(4) 0.011(5) C5 0.090(4) 0.133(5) 0.073(3) 0.004(3) 0.037(3) 0.002(3) C6 0.065(3) 0.072(3) 0.063(3) -0.002(2) 0.016(2) 0.000(2) C7 0.061(3) 0.078(3) 0.066(3) -0.005(2) 0.021(2) 0.005(2) C8 0.062(3) 0.108(4) 0.078(3) 0.007(3) 0.011(3) 0.017(3) C9 0.085(4) 0.118(4) 0.066(3) -0.003(3) 0.009(3) 0.019(3) C10 0.158(7) 0.087(5) 0.134(6) 0.017(4) 0.018(5) 0.022(4) C11 0.312(14) 0.067(4) 0.147(7) -0.007(5) -0.075(8) 0.018(6) C12 0.196(10) 0.195(10) 0.359(17) -0.166(12) 0.150(11) -0.145(9) C13 0.146(7) 0.152(7) 0.161(7) -0.044(6) 0.069(6) -0.096(6) C14 0.057(3) 0.139(5) 0.062(3) 0.019(3) 0.026(2) -0.012(3) C15 0.057(3) 0.105(4) 0.054(2) 0.018(2) 0.018(2) 0.000(3) C16 0.061(3) 0.164(6) 0.063(3) 0.016(4) 0.023(3) 0.025(4) C17 0.093(5) 0.132(5) 0.072(4) -0.009(4) 0.017(3) 0.031(4) C18 0.100(4) 0.098(4) 0.062(3) 0.002(3) 0.025(3) 0.019(3) C19 0.073(3) 0.080(3) 0.073(3) 0.004(3) 0.026(3) -0.002(2) C20 0.056(3) 0.082(3) 0.062(3) 0.010(2) 0.021(2) 0.001(2) Fe2 0.0677(4) 0.0766(4) 0.0491(3) 0.0031(3) 0.0093(3) 0.0091(3) O21 0.067(2) 0.078(2) 0.101(3) -0.0142(19) -0.0020(18) 0.0065(16) O22 0.060(2) 0.120(3) 0.079(2) 0.018(2) 0.0151(17) -0.0020(18) N21 0.085(3) 0.112(4) 0.062(3) 0.021(2) 0.012(2) 0.043(3) N22 0.140(4) 0.079(3) 0.071(3) 0.002(2) 0.039(3) 0.027(3) N23 0.114(4) 0.077(3) 0.056(2) 0.0027(19) 0.032(2) -0.003(2) N24 0.061(2) 0.072(2) 0.058(2) -0.0039(17) 0.0178(17) -0.0055(17) C21 0.061(3) 0.083(3) 0.055(2) 0.012(2) 0.011(2) -0.005(2) C22 0.075(3) 0.079(3) 0.067(3) 0.000(2) 0.015(2) -0.005(2) C23 0.093(4) 0.101(4) 0.069(3) -0.009(3) 0.025(3) -0.025(3) C24 0.101(5) 0.142(6) 0.076(4) -0.032(4) 0.032(4) -0.040(4) C25 0.059(3) 0.181(7) 0.053(3) -0.001(3) 0.010(2) -0.023(4) C26 0.060(3) 0.112(4) 0.050(2) 0.017(3) 0.014(2) -0.001(3) C27 0.060(3) 0.158(6) 0.044(3) 0.027(3) 0.008(2) 0.018(3) C28 0.157(7) 0.168(8) 0.117(6) 0.001(5) -0.004(5) 0.107(6) C29 0.199(11) 0.202(10) 0.247(13) -0.082(10) -0.034(9) 0.144(9) C30 0.267(12) 0.066(4) 0.271(12) -0.028(6) 0.180(11) -0.024(6) C31 0.180(7) 0.074(4) 0.171(7) -0.001(4) 0.091(6) -0.012(4) C32 0.088(4) 0.104(4) 0.082(4) -0.007(3) 0.040(3) -0.013(3) C33 0.065(3) 0.101(4) 0.074(3) 0.001(3) 0.023(2) -0.013(3) C34 0.056(3) 0.077(3) 0.067(3) -0.008(2) 0.011(2) -0.001(2) C35 0.064(3) 0.074(3) 0.061(3) -0.003(2) 0.015(2) 0.000(2) C36 0.080(4) 0.133(5) 0.065(3) 0.009(3) 0.012(3) 0.007(3) C37 0.104(5) 0.185(7) 0.079(4) 0.032(4) 0.035(4) 0.003(5) C38 0.103(5) 0.138(6) 0.096(4) 0.021(4) 0.053(4) -0.006(4) C39 0.070(3) 0.101(4) 0.098(4) 0.008(3) 0.032(3) 0.000(3) C40 0.063(3) 0.080(3) 0.069(3) 0.005(2) 0.022(2) 0.002(2) Ni1A 0.0474(4) 0.0446(4) 0.0729(5) -0.0004(3) 0.0128(3) 0.0016(3) S1A 0.1022(9) 0.0462(5) 0.0740(7) 0.0003(5) 0.0274(7) 0.0001(6) S2A 0.0941(9) 0.0510(6) 0.0853(8) 0.0075(6) 0.0245(7) 0.0018(6) S3A 0.0990(10) 0.0644(7) 0.0739(8) -0.0088(6) 0.0257(7) -0.0007(6) S4A 0.0907(9) 0.0881(9) 0.0752(8) 0.0105(7) 0.0232(7) 0.0010(7) S5A 0.1110(13) 0.1321(14) 0.0743(9) -0.0173(8) 0.0291(8) -0.0018(10) C1A 0.051(2) 0.054(2) 0.068(3) -0.002(2) 0.0128(19) -0.0016(17) C2A 0.046(2) 0.064(3) 0.072(3) 0.001(2) 0.011(2) 0.0002(18) C3A 0.053(3) 0.093(3) 0.072(3) -0.002(3) 0.011(2) 0.001(2) Ni1B 0.0517(5) 0.0773(5) 0.0701(5) 0.000 0.0247(4) 0.000 S1B 0.1024(10) 0.0768(8) 0.0630(7) -0.0073(6) 0.0216(7) 0.0121(7) S2B 0.0931(10) 0.0764(8) 0.0892(9) -0.0070(7) 0.0334(8) -0.0058(7) S3B 0.0983(10) 0.1035(10) 0.0633(7) -0.0111(7) 0.0119(7) 0.0350(8) S4B 0.0997(11) 0.0978(10) 0.0897(10) -0.0291(8) 0.0234(8) -0.0163(8) S5B 0.0720(9) 0.1489(15) 0.0714(9) -0.0299(9) 0.0061(7) 0.0125(8) C1B 0.061(3) 0.084(3) 0.065(3) -0.007(2) 0.018(2) 0.013(2) C2B 0.057(3) 0.088(3) 0.069(3) -0.015(2) 0.022(2) -0.002(2) C3B 0.046(3) 0.115(4) 0.080(3) -0.024(3) 0.011(2) 0.013(2) Ni1C 0.0513(4) 0.0796(5) 0.0563(5) 0.0079(4) 0.0007(3) -0.0048(4) S1C 0.0853(9) 0.0789(8) 0.0831(9) 0.0142(7) 0.0238(7) 0.0074(7) S2C 0.1066(10) 0.0776(8) 0.0615(7) 0.0013(6) 0.0206(7) -0.0089(7) S3C 0.0841(9) 0.0944(10) 0.0969(10) 0.0028(8) 0.0311(8) 0.0157(7) S4C 0.1086(11) 0.0903(9) 0.0670(8) -0.0063(7) 0.0298(7) -0.0255(8) S5C 0.0720(9) 0.1336(13) 0.0812(9) -0.0126(8) 0.0285(7) -0.0068(8) C1C 0.059(3) 0.085(3) 0.067(3) 0.004(2) 0.010(2) -0.002(2) C2C 0.061(3) 0.087(3) 0.055(2) -0.003(2) 0.008(2) -0.017(2) C3C 0.049(3) 0.101(4) 0.080(3) -0.006(3) 0.012(2) -0.010(2) Ni1D 0.0553(4) 0.0546(4) 0.0442(4) -0.0009(3) 0.0149(3) -0.0015(3) S1D 0.0643(7) 0.0626(6) 0.0742(7) -0.0147(5) 0.0126(5) -0.0016(5) S2D 0.0635(7) 0.0630(6) 0.0790(8) -0.0151(6) 0.0208(6) -0.0009(5) S3D 0.0655(7) 0.0990(9) 0.0716(8) -0.0076(7) 0.0086(6) -0.0168(6) S4D 0.0640(7) 0.1010(10) 0.0824(8) -0.0033(7) 0.0254(6) 0.0126(7) S5D 0.0566(8) 0.197(2) 0.0945(11) 0.0040(11) 0.0156(7) -0.0030(9) C1D 0.060(3) 0.072(3) 0.046(2) -0.001(2) 0.0126(18) -0.011(2) C2D 0.058(2) 0.073(3) 0.051(2) 0.006(2) 0.0220(19) 0.004(2) C3D 0.073(3) 0.121(4) 0.048(2) 0.010(3) 0.019(2) -0.009(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 O2 1.879(3) . ? Fe1 O1 1.896(3) . ? Fe1 N1 2.075(4) . ? Fe1 N4 2.085(5) . ? Fe1 N3 2.128(4) . ? Fe1 N2 2.139(4) . ? O1 C1 1.314(6) . ? O2 C20 1.315(5) . ? N1 C7 1.278(6) . ? N1 C8 1.473(6) . ? N2 C10 1.452(7) . ? N2 C9 1.488(7) . ? N3 C12 1.409(10) . ? N3 C11 1.442(9) . ? N4 C14 1.286(7) . ? N4 C13 1.462(7) . ? C1 C6 1.398(6) . ? C1 C2 1.401(7) . ? C2 C3 1.360(8) . ? C3 C4 1.373(9) . ? C4 C5 1.363(8) . ? C5 C6 1.395(7) . ? C6 C7 1.436(6) . ? C8 C9 1.488(7) . ? C10 C11 1.331(9) . ? C12 C13 1.382(11) . ? C14 C15 1.428(8) . ? C15 C20 1.399(6) . ? C15 C16 1.411(7) . ? C16 C17 1.369(9) . ? C17 C18 1.345(8) . ? C18 C19 1.369(7) . ? C19 C20 1.397(7) . ? Fe2 O21 1.874(3) . ? Fe2 O22 1.893(3) . ? Fe2 N24 2.053(4) . ? Fe2 N21 2.071(5) . ? Fe2 N22 2.115(4) . ? Fe2 N23 2.128(4) . ? O21 C21 1.322(5) . ? O22 C40 1.314(5) . ? N21 C27 1.266(7) . ? N21 C28 1.466(8) . ? N22 C29 1.416(10) . ? N22 C30 1.444(9) . ? N23 C31 1.453(7) . ? N23 C32 1.482(7) . ? N24 C34 1.283(6) . ? N24 C33 1.482(6) . ? C21 C22 1.392(7) . ? C21 C26 1.401(6) . ? C22 C23 1.372(7) . ? C23 C24 1.348(8) . ? C24 C25 1.362(9) . ? C25 C26 1.422(8) . ? C26 C27 1.425(8) . ? C28 C29 1.378(11) . ? C30 C31 1.325(9) . ? C32 C33 1.487(7) . ? C34 C35 1.440(6) . ? C35 C40 1.391(6) . ? C35 C36 1.401(7) . ? C36 C37 1.354(8) . ? C37 C38 1.372(9) . ? C38 C39 1.359(8) . ? C39 C40 1.409(7) . ? Ni1A S1A 2.1452(11) . ? Ni1A S1A 2.1452(11) 7_655 ? Ni1A S2A 2.1552(13) . ? Ni1A S2A 2.1552(13) 7_655 ? S1A C1A 1.712(5) . ? S2A C2A 1.704(5) . ? S3A C3A 1.728(5) . ? S3A C1A 1.743(4) . ? S4A C3A 1.731(6) . ? S4A C2A 1.746(5) . ? S5A C3A 1.641(5) . ? C1A C2A 1.354(6) . ? Ni1B S2B 2.1580(15) . ? Ni1B S2B 2.1580(15) 2_556 ? Ni1B S1B 2.1584(15) 2_556 ? Ni1B S1B 2.1584(15) . ? S1B C1B 1.705(5) . ? S2B C2B 1.711(5) . ? S3B C3B 1.723(5) . ? S3B C1B 1.740(5) . ? S4B C3B 1.730(6) . ? S4B C2B 1.744(5) . ? S5B C3B 1.645(5) . ? C1B C2B 1.366(7) . ? Ni1C S2C 2.1590(13) 5 ? Ni1C S2C 2.1590(13) . ? Ni1C S1C 2.1602(14) . ? Ni1C S1C 2.1602(14) 5 ? S1C C1C 1.710(5) . ? S2C C2C 1.714(5) . ? S3C C3C 1.724(6) . ? S3C C1C 1.732(5) . ? S4C C3C 1.725(6) . ? S4C C2C 1.740(5) . ? S5C C3C 1.647(6) . ? C1C C2C 1.370(7) . ? Ni1D S1D 2.1576(11) . ? Ni1D S1D 2.1576(11) 7_656 ? Ni1D S2D 2.1586(11) 7_656 ? Ni1D S2D 2.1586(11) . ? S1D C1D 1.706(5) . ? S2D C2D 1.720(4) . ? S3D C3D 1.725(6) . ? S3D C1D 1.747(4) . ? S4D C3D 1.727(5) . ? S4D C2D 1.736(4) . ? S5D C3D 1.639(5) . ? C1D C2D 1.343(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe1 O1 103.58(18) . . ? O2 Fe1 N1 94.93(14) . . ? O1 Fe1 N1 88.02(14) . . ? O2 Fe1 N4 87.35(16) . . ? O1 Fe1 N4 89.09(16) . . ? N1 Fe1 N4 176.67(16) . . ? O2 Fe1 N3 160.07(17) . . ? O1 Fe1 N3 91.83(18) . . ? N1 Fe1 N3 98.21(17) . . ? N4 Fe1 N3 80.23(19) . . ? O2 Fe1 N2 88.52(16) . . ? O1 Fe1 N2 162.74(16) . . ? N1 Fe1 N2 78.59(16) . . ? N4 Fe1 N2 103.93(17) . . ? N3 Fe1 N2 79.52(18) . . ? C1 O1 Fe1 133.9(3) . . ? C20 O2 Fe1 133.3(3) . . ? C7 N1 C8 118.6(4) . . ? C7 N1 Fe1 126.3(3) . . ? C8 N1 Fe1 115.1(3) . . ? C10 N2 C9 117.0(5) . . ? C10 N2 Fe1 111.6(4) . . ? C9 N2 Fe1 105.7(3) . . ? C12 N3 C11 119.1(8) . . ? C12 N3 Fe1 109.4(5) . . ? C11 N3 Fe1 109.2(4) . . ? C14 N4 C13 121.4(6) . . ? C14 N4 Fe1 124.9(4) . . ? C13 N4 Fe1 113.1(5) . . ? O1 C1 C6 122.4(4) . . ? O1 C1 C2 118.8(5) . . ? C6 C1 C2 118.9(5) . . ? C3 C2 C1 120.8(5) . . ? C2 C3 C4 120.5(6) . . ? C5 C4 C3 119.9(6) . . ? C4 C5 C6 121.3(6) . . ? C5 C6 C1 118.6(5) . . ? C5 C6 C7 117.8(5) . . ? C1 C6 C7 123.6(4) . . ? N1 C7 C6 125.8(4) . . ? N1 C8 C9 109.8(4) . . ? C8 C9 N2 109.3(4) . . ? C11 C10 N2 116.2(6) . . ? C10 C11 N3 120.6(7) . . ? C13 C12 N3 121.1(7) . . ? C12 C13 N4 113.9(6) . . ? N4 C14 C15 126.5(5) . . ? C20 C15 C16 118.8(5) . . ? C20 C15 C14 122.1(5) . . ? C16 C15 C14 119.1(5) . . ? C17 C16 C15 121.0(5) . . ? C18 C17 C16 119.8(6) . . ? C17 C18 C19 121.1(6) . . ? C18 C19 C20 121.2(5) . . ? O2 C20 C19 118.8(4) . . ? O2 C20 C15 123.3(5) . . ? C19 C20 C15 118.0(5) . . ? O21 Fe2 O22 103.04(18) . . ? O21 Fe2 N24 95.12(14) . . ? O22 Fe2 N24 88.44(14) . . ? O21 Fe2 N21 87.46(17) . . ? O22 Fe2 N21 88.46(17) . . ? N24 Fe2 N21 176.36(16) . . ? O21 Fe2 N22 160.52(17) . . ? O22 Fe2 N22 91.96(18) . . ? N24 Fe2 N22 97.67(18) . . ? N21 Fe2 N22 80.5(2) . . ? O21 Fe2 N23 88.44(16) . . ? O22 Fe2 N23 163.52(16) . . ? N24 Fe2 N23 78.66(16) . . ? N21 Fe2 N23 104.02(18) . . ? N22 Fe2 N23 79.79(18) . . ? C21 O21 Fe2 133.1(3) . . ? C40 O22 Fe2 133.1(3) . . ? C27 N21 C28 121.2(6) . . ? C27 N21 Fe2 125.6(4) . . ? C28 N21 Fe2 112.7(5) . . ? C29 N22 C30 119.0(8) . . ? C29 N22 Fe2 109.4(5) . . ? C30 N22 Fe2 109.4(4) . . ? C31 N23 C32 117.1(5) . . ? C31 N23 Fe2 111.7(4) . . ? C32 N23 Fe2 105.6(3) . . ? C34 N24 C33 117.4(4) . . ? C34 N24 Fe2 126.8(3) . . ? C33 N24 Fe2 115.8(3) . . ? O21 C21 C22 118.7(4) . . ? O21 C21 C26 122.4(5) . . ? C22 C21 C26 119.0(5) . . ? C23 C22 C21 121.4(5) . . ? C24 C23 C22 120.3(6) . . ? C23 C24 C25 120.6(6) . . ? C24 C25 C26 121.2(5) . . ? C21 C26 C25 117.5(5) . . ? C21 C26 C27 122.6(5) . . ? C25 C26 C27 119.9(5) . . ? N21 C27 C26 126.1(5) . . ? C29 C28 N21 114.4(6) . . ? C28 C29 N22 119.4(7) . . ? C31 C30 N22 120.9(6) . . ? C30 C31 N23 116.1(6) . . ? N23 C32 C33 109.9(4) . . ? N24 C33 C32 108.7(4) . . ? N24 C34 C35 125.1(4) . . ? C40 C35 C36 118.5(5) . . ? C40 C35 C34 123.5(4) . . ? C36 C35 C34 118.0(4) . . ? C37 C36 C35 122.3(5) . . ? C36 C37 C38 118.9(6) . . ? C39 C38 C37 121.1(6) . . ? C38 C39 C40 120.8(5) . . ? O22 C40 C35 122.9(4) . . ? O22 C40 C39 118.7(4) . . ? C35 C40 C39 118.4(5) . . ? S1A Ni1A S1A 180.00(7) . 7_655 ? S1A Ni1A S2A 93.24(5) . . ? S1A Ni1A S2A 86.76(5) 7_655 . ? S1A Ni1A S2A 86.76(5) . 7_655 ? S1A Ni1A S2A 93.24(5) 7_655 7_655 ? S2A Ni1A S2A 180.00(9) . 7_655 ? C1A S1A Ni1A 102.09(14) . . ? C2A S2A Ni1A 102.20(16) . . ? C3A S3A C1A 98.1(2) . . ? C3A S4A C2A 97.9(2) . . ? C2A C1A S1A 121.4(3) . . ? C2A C1A S3A 115.8(3) . . ? S1A C1A S3A 122.8(2) . . ? C1A C2A S2A 121.1(4) . . ? C1A C2A S4A 115.8(3) . . ? S2A C2A S4A 123.1(3) . . ? S5A C3A S3A 123.1(3) . . ? S5A C3A S4A 124.5(3) . . ? S3A C3A S4A 112.4(3) . . ? S2B Ni1B S2B 87.14(8) . 2_556 ? S2B Ni1B S1B 177.92(5) . 2_556 ? S2B Ni1B S1B 93.09(5) 2_556 2_556 ? S2B Ni1B S1B 93.09(5) . . ? S2B Ni1B S1B 177.92(5) 2_556 . ? S1B Ni1B S1B 86.75(7) 2_556 . ? C1B S1B Ni1B 102.28(18) . . ? C2B S2B Ni1B 102.27(17) . . ? C3B S3B C1B 97.8(3) . . ? C3B S4B C2B 97.8(2) . . ? C2B C1B S1B 121.3(4) . . ? C2B C1B S3B 116.1(4) . . ? S1B C1B S3B 122.5(3) . . ? C1B C2B S2B 121.0(4) . . ? C1B C2B S4B 115.4(4) . . ? S2B C2B S4B 123.5(3) . . ? S5B C3B S3B 123.3(4) . . ? S5B C3B S4B 123.7(3) . . ? S3B C3B S4B 113.0(3) . . ? S2C Ni1C S2C 180.00(9) 5 . ? S2C Ni1C S1C 86.78(5) 5 . ? S2C Ni1C S1C 93.22(5) . . ? S2C Ni1C S1C 93.22(5) 5 5 ? S2C Ni1C S1C 86.78(5) . 5 ? S1C Ni1C S1C 180.00(10) . 5 ? C1C S1C Ni1C 102.64(18) . . ? C2C S2C Ni1C 101.90(17) . . ? C3C S3C C1C 97.7(3) . . ? C3C S4C C2C 97.4(3) . . ? C2C C1C S1C 120.3(4) . . ? C2C C1C S3C 115.8(4) . . ? S1C C1C S3C 123.7(3) . . ? C1C C2C S2C 121.9(4) . . ? C1C C2C S4C 115.8(4) . . ? S2C C2C S4C 122.3(3) . . ? S5C C3C S3C 123.4(3) . . ? S5C C3C S4C 123.3(3) . . ? S3C C3C S4C 113.3(3) . . ? S1D Ni1D S1D 180.00(5) . 7_656 ? S1D Ni1D S2D 86.69(4) . 7_656 ? S1D Ni1D S2D 93.31(4) 7_656 7_656 ? S1D Ni1D S2D 93.31(4) . . ? S1D Ni1D S2D 86.69(4) 7_656 . ? S2D Ni1D S2D 180.00(7) 7_656 . ? C1D S1D Ni1D 101.70(15) . . ? C2D S2D Ni1D 101.76(15) . . ? C3D S3D C1D 97.5(2) . . ? C3D S4D C2D 97.1(2) . . ? C2D C1D S1D 122.2(3) . . ? C2D C1D S3D 115.3(3) . . ? S1D C1D S3D 122.5(3) . . ? C1D C2D S2D 121.0(3) . . ? C1D C2D S4D 117.0(3) . . ? S2D C2D S4D 122.0(3) . . ? S5D C3D S3D 123.5(3) . . ? S5D C3D S4D 123.4(3) . . ? S3D C3D S4D 113.1(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.78 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.586 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.084 # Attachment 't-1_100.cif' data_t-1'-100 _database_code_depnum_ccdc_archive 'CCDC 729929' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, C6 Ni S10, C3 H6 O, C2 H3 N' _chemical_formula_sum 'C31 H33 Fe N5 Ni O3 S10' _chemical_formula_weight 958.78 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' Ni Ni 0.3393 1.1124 '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 11.825(5) _cell_length_b 12.542(5) _cell_length_c 13.795(5) _cell_angle_alpha 106.884(5) _cell_angle_beta 90.945(5) _cell_angle_gamma 93.107(5) _cell_volume 1953.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.8 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5436 _exptl_absorpt_correction_T_max 0.7486 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS) equipped with an Oxford Cryosystems cooler device. The crystal-to-detector distance was 70 mm. 192 exposures (2.5 min per exposure) were obtained with 0 < \f < 251\% and with the crystals rotated through 1.3\% in \f. Crystal decay was monitored by measuring 200 reflexions per image. ; _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 'STOE Imaging Plate Diffraction System' _diffrn_measurement_method '\f scan ' _diffrn_standards_decay_% negligible _diffrn_reflns_number 18822 _diffrn_reflns_av_R_equivalents 0.0731 _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.79 _reflns_number_total 6964 _reflns_number_gt 4636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS software (Stoe, 1996)' _computing_cell_refinement 'IPDS software (Stoe, 1996)' _computing_data_reduction 'IPDS software (Stoe, 1996)' _computing_structure_solution 'Sir97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997), Mercury (Bruno et al., 2002) and Cameron (Watkin, 1993)' _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^)+(0.0754P)^2^] 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 6964 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 0.34180(6) 0.77059(6) 0.13942(6) 0.01705(19) Uani 1 1 d . . . O1 O 0.3655(3) 0.7167(3) 0.0001(3) 0.0212(8) Uani 1 1 d . . . O2 O 0.4922(3) 0.8194(3) 0.1791(3) 0.0190(8) Uani 1 1 d . . . N1 N 0.3196(3) 0.9204(4) 0.1350(3) 0.0192(10) Uani 1 1 d . . . N2 N 0.2996(3) 0.8295(4) 0.2846(3) 0.0183(10) Uani 1 1 d . . . H2N H 0.3487 0.8015 0.3233 0.022 Uiso 1 1 calc R . . N3 N 0.1777(4) 0.7173(4) 0.1156(3) 0.0215(10) Uani 1 1 d . . . H3N H 0.1508 0.7398 0.0613 0.026 Uiso 1 1 calc R . . N4 N 0.3649(3) 0.6204(4) 0.1417(3) 0.0199(10) Uani 1 1 d . . . C1 C 0.3865(4) 0.7780(4) -0.0630(4) 0.0207(12) Uani 1 1 d . . . C2 C 0.4163(4) 0.7214(5) -0.1624(4) 0.0238(12) Uani 1 1 d . . . H2 H 0.4226 0.6429 -0.1812 0.029 Uiso 1 1 calc R . . C3 C 0.4368(5) 0.7791(5) -0.2338(4) 0.0269(13) Uani 1 1 d . . . H3 H 0.4566 0.7399 -0.3006 0.032 Uiso 1 1 calc R . . C4 C 0.4279(5) 0.8951(5) -0.2064(4) 0.0278(13) Uani 1 1 d . . . H4 H 0.4411 0.9348 -0.2545 0.033 Uiso 1 1 calc R . . C5 C 0.4000(5) 0.9504(5) -0.1098(4) 0.0258(13) Uani 1 1 d . . . H5 H 0.3955 1.0291 -0.0914 0.031 Uiso 1 1 calc R . . C6 C 0.3779(4) 0.8944(5) -0.0368(4) 0.0227(12) Uani 1 1 d . . . C7 C 0.3440(4) 0.9594(5) 0.0608(4) 0.0232(12) Uani 1 1 d . . . H7 H 0.3391 1.0373 0.0716 0.028 Uiso 1 1 calc R . . C8 C 0.2827(5) 0.9971(5) 0.2293(4) 0.0256(13) Uani 1 1 d . . . H8A H 0.1992 1.0002 0.2276 0.031 Uiso 1 1 calc R . . H8B H 0.3171 1.0733 0.2385 0.031 Uiso 1 1 calc R . . C9 C 0.3208(5) 0.9532(5) 0.3155(4) 0.0241(12) Uani 1 1 d . . . H9A H 0.4026 0.9731 0.3315 0.029 Uiso 1 1 calc R . . H9B H 0.2784 0.9873 0.3769 0.029 Uiso 1 1 calc R . . C10 C 0.1817(4) 0.7906(5) 0.3009(4) 0.0210(11) Uani 1 1 d . . . H10A H 0.1482 0.8475 0.3568 0.025 Uiso 1 1 calc R . . H10B H 0.1829 0.7204 0.3199 0.025 Uiso 1 1 calc R . . C11 C 0.1109(4) 0.7715(5) 0.2045(4) 0.0233(12) Uani 1 1 d . . . H11A H 0.0423 0.7235 0.2063 0.028 Uiso 1 1 calc R . . H11B H 0.0866 0.8438 0.1987 0.028 Uiso 1 1 calc R . . C12 C 0.1715(4) 0.5933(5) 0.0829(4) 0.0267(13) Uani 1 1 d . . . H12A H 0.1839 0.5655 0.0092 0.032 Uiso 1 1 calc R . . H12B H 0.0953 0.5646 0.0958 0.032 Uiso 1 1 calc R . . C13 C 0.2608(4) 0.5513(5) 0.1408(4) 0.0248(12) Uani 1 1 d . . . H13A H 0.2372 0.5588 0.2108 0.030 Uiso 1 1 calc R . . H13B H 0.2727 0.4718 0.1068 0.030 Uiso 1 1 calc R . . C14 C 0.4613(4) 0.5754(5) 0.1322(4) 0.0205(11) Uani 1 1 d . . . H14 H 0.4615 0.4969 0.1205 0.025 Uiso 1 1 calc R . . C15 C 0.5684(4) 0.6373(4) 0.1383(4) 0.0179(11) Uani 1 1 d . . . C16 C 0.6681(4) 0.5777(5) 0.1225(4) 0.0232(12) Uani 1 1 d . . . H16 H 0.6617 0.4985 0.1043 0.028 Uiso 1 1 calc R . . C17 C 0.7729(4) 0.6310(5) 0.1325(4) 0.0247(12) Uani 1 1 d . . . H17 H 0.8386 0.5893 0.1208 0.030 Uiso 1 1 calc R . . C18 C 0.7829(4) 0.7475(5) 0.1603(4) 0.0274(13) Uani 1 1 d . . . H18 H 0.8558 0.7852 0.1675 0.033 Uiso 1 1 calc R . . C19 C 0.6879(4) 0.8079(5) 0.1772(4) 0.0202(11) Uani 1 1 d . . . H19 H 0.6961 0.8871 0.1983 0.024 Uiso 1 1 calc R . . C20 C 0.5787(4) 0.7544(4) 0.1638(4) 0.0184(11) Uani 1 1 d . . . Ni1 Ni 0.48538(5) 0.71852(6) 0.45784(5) 0.01733(17) Uani 1 1 d . . . S1 S 0.32288(10) 0.63477(11) 0.46656(11) 0.0213(3) Uani 1 1 d . . . S2 S 0.42593(10) 0.88319(11) 0.52530(10) 0.0196(3) Uani 1 1 d . . . S3 S 0.09928(10) 0.72767(12) 0.54489(10) 0.0221(3) Uani 1 1 d . . . S4 S 0.19308(11) 0.95649(12) 0.59614(11) 0.0232(3) Uani 1 1 d . . . S5 S -0.05232(11) 0.91348(13) 0.62312(12) 0.0323(4) Uani 1 1 d . . . S6 S 0.54616(10) 0.55399(11) 0.39392(11) 0.0222(3) Uani 1 1 d . . . S7 S 0.64835(10) 0.80197(11) 0.45048(11) 0.0221(3) Uani 1 1 d . . . S8 S 0.78224(10) 0.48043(11) 0.33851(11) 0.0233(3) Uani 1 1 d . . . S9 S 0.87645(10) 0.70843(11) 0.39021(11) 0.0217(3) Uani 1 1 d . . . S10 S 1.02803(11) 0.52213(13) 0.31248(12) 0.0304(3) Uani 1 1 d . . . C21 C 0.2427(4) 0.7456(5) 0.5226(4) 0.0205(12) Uani 1 1 d . . . C22 C 0.2864(4) 0.8514(4) 0.5470(4) 0.0209(12) Uani 1 1 d . . . C23 C 0.0744(4) 0.8677(5) 0.5907(4) 0.0238(12) Uani 1 1 d . . . C24 C 0.7317(4) 0.6915(5) 0.4052(4) 0.0215(12) Uani 1 1 d . . . C25 C 0.6869(4) 0.5844(5) 0.3802(4) 0.0210(12) Uani 1 1 d . . . C26 C 0.9009(4) 0.5678(5) 0.3444(4) 0.0218(12) Uani 1 1 d . . . C30 C 0.0998(5) 0.8652(6) 0.9150(5) 0.0431(17) Uani 1 1 d . . . C32 C 0.1063(7) 0.7688(7) 0.8299(6) 0.060(2) Uani 1 1 d . . . H32A H 0.0985 0.7016 0.8523 0.089 Uiso 1 1 calc R . . H32B H 0.1797 0.7718 0.7984 0.089 Uiso 1 1 calc R . . H32C H 0.0452 0.7670 0.7804 0.089 Uiso 1 1 calc R . . C31 C 0.0964(7) 0.9753(7) 0.8946(7) 0.061(2) Uani 1 1 d . . . H31A H 0.0184 0.9874 0.8774 0.092 Uiso 1 1 calc R . . H31B H 0.1449 0.9762 0.8379 0.092 Uiso 1 1 calc R . . H31C H 0.1237 1.0347 0.9552 0.092 Uiso 1 1 calc R . . O30 O 0.0948(4) 0.8592(5) 1.0032(4) 0.0525(14) Uani 1 1 d . . . C40 C 0.2559(7) 0.3282(7) 0.3356(7) 0.061(2) Uani 1 1 d . . . H40A H 0.2033 0.3862 0.3635 0.091 Uiso 1 1 calc R . . H40B H 0.3339 0.3609 0.3472 0.091 Uiso 1 1 calc R . . H40C H 0.2465 0.2694 0.3691 0.091 Uiso 1 1 calc R . . C41 C 0.2325(8) 0.2811(8) 0.2282(8) 0.067(3) Uani 1 1 d . . . N40 N 0.2058(10) 0.2390(9) 0.1449(7) 0.114(4) 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 0.0147(3) 0.0195(4) 0.0175(4) 0.0058(3) 0.0006(3) 0.0033(3) O1 0.0232(18) 0.022(2) 0.020(2) 0.0088(17) 0.0017(15) 0.0036(15) O2 0.0189(18) 0.0169(19) 0.0210(19) 0.0039(17) 0.0013(15) 0.0073(15) N1 0.017(2) 0.025(3) 0.014(2) 0.003(2) 0.0010(18) 0.0039(19) N2 0.012(2) 0.024(2) 0.021(2) 0.011(2) -0.0016(17) 0.0037(18) N3 0.021(2) 0.026(3) 0.017(2) 0.006(2) -0.0005(18) 0.0047(19) N4 0.016(2) 0.024(2) 0.021(2) 0.009(2) 0.0030(18) -0.0014(18) C1 0.019(2) 0.024(3) 0.019(3) 0.006(2) -0.002(2) 0.000(2) C2 0.023(3) 0.028(3) 0.022(3) 0.009(3) 0.001(2) 0.004(2) C3 0.026(3) 0.036(4) 0.019(3) 0.010(3) 0.001(2) 0.001(3) C4 0.031(3) 0.035(3) 0.021(3) 0.016(3) -0.001(2) -0.004(3) C5 0.032(3) 0.023(3) 0.023(3) 0.009(3) -0.004(2) 0.001(2) C6 0.021(3) 0.027(3) 0.022(3) 0.012(3) -0.004(2) 0.000(2) C7 0.026(3) 0.021(3) 0.024(3) 0.008(3) -0.005(2) 0.007(2) C8 0.025(3) 0.030(3) 0.024(3) 0.011(3) 0.002(2) 0.007(2) C9 0.026(3) 0.026(3) 0.019(3) 0.004(3) -0.003(2) 0.002(2) C10 0.017(2) 0.023(3) 0.021(3) 0.004(2) 0.001(2) 0.000(2) C11 0.013(2) 0.033(3) 0.023(3) 0.006(3) 0.000(2) 0.007(2) C12 0.014(3) 0.031(3) 0.030(3) 0.002(3) -0.003(2) -0.001(2) C13 0.018(3) 0.022(3) 0.035(3) 0.010(3) 0.005(2) -0.003(2) C14 0.020(3) 0.021(3) 0.020(3) 0.005(2) 0.002(2) 0.004(2) C15 0.015(2) 0.022(3) 0.017(3) 0.005(2) 0.001(2) 0.006(2) C16 0.024(3) 0.023(3) 0.023(3) 0.006(3) 0.000(2) 0.007(2) C17 0.017(3) 0.028(3) 0.029(3) 0.006(3) 0.002(2) 0.009(2) C18 0.017(3) 0.032(3) 0.035(3) 0.012(3) 0.000(2) 0.001(2) C19 0.020(3) 0.020(3) 0.021(3) 0.007(2) -0.001(2) 0.004(2) C20 0.019(2) 0.022(3) 0.016(3) 0.007(2) -0.001(2) 0.006(2) Ni1 0.0109(3) 0.0214(4) 0.0205(4) 0.0070(3) 0.0015(3) 0.0027(3) S1 0.0135(6) 0.0204(7) 0.0304(8) 0.0078(6) 0.0035(5) 0.0033(5) S2 0.0140(6) 0.0218(7) 0.0228(7) 0.0063(6) 0.0013(5) 0.0013(5) S3 0.0122(6) 0.0264(8) 0.0276(8) 0.0070(7) 0.0028(5) 0.0030(5) S4 0.0157(6) 0.0246(7) 0.0273(8) 0.0039(6) 0.0019(5) 0.0039(5) S5 0.0177(7) 0.0356(9) 0.0393(9) 0.0024(8) 0.0072(6) 0.0093(6) S6 0.0131(6) 0.0221(7) 0.0314(8) 0.0075(6) 0.0047(5) 0.0017(5) S7 0.0139(6) 0.0205(7) 0.0300(8) 0.0041(6) 0.0033(5) 0.0012(5) S8 0.0136(6) 0.0218(7) 0.0345(8) 0.0076(7) 0.0050(6) 0.0036(5) S9 0.0120(6) 0.0230(7) 0.0292(8) 0.0058(6) 0.0025(5) 0.0016(5) S10 0.0156(6) 0.0305(8) 0.0439(9) 0.0081(8) 0.0084(6) 0.0042(6) C21 0.013(2) 0.026(3) 0.023(3) 0.007(3) 0.000(2) 0.004(2) C22 0.022(3) 0.023(3) 0.021(3) 0.009(3) 0.001(2) 0.005(2) C23 0.019(3) 0.033(3) 0.021(3) 0.010(3) 0.003(2) 0.004(2) C24 0.014(2) 0.027(3) 0.024(3) 0.008(3) -0.003(2) -0.001(2) C25 0.015(2) 0.025(3) 0.024(3) 0.007(3) 0.002(2) 0.004(2) C26 0.017(2) 0.025(3) 0.023(3) 0.006(3) -0.003(2) 0.002(2) C30 0.035(4) 0.059(5) 0.037(4) 0.016(4) -0.004(3) 0.011(3) C32 0.070(5) 0.056(5) 0.046(5) 0.004(4) -0.008(4) 0.004(4) C31 0.068(5) 0.066(6) 0.059(5) 0.031(5) 0.003(4) 0.013(4) O30 0.046(3) 0.071(4) 0.044(3) 0.022(3) -0.008(2) 0.011(3) C40 0.064(5) 0.047(5) 0.067(6) 0.008(4) 0.001(4) 0.015(4) C41 0.089(7) 0.053(5) 0.067(6) 0.024(5) 0.006(5) 0.038(5) N40 0.182(11) 0.101(8) 0.060(6) 0.023(6) -0.014(6) 0.043(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.868(3) . ? Fe1 O1 1.874(4) . ? Fe1 N4 1.928(4) . ? Fe1 N1 1.930(4) . ? Fe1 N2 2.004(5) . ? Fe1 N3 2.007(4) . ? O1 C1 1.335(6) . ? O2 C20 1.324(6) . ? N1 C7 1.286(7) . ? N1 C8 1.465(7) . ? N2 C9 1.490(7) . ? N2 C10 1.495(6) . ? N2 H2N 0.9300 . ? N3 C11 1.482(7) . ? N3 C12 1.486(7) . ? N3 H3N 0.9300 . ? N4 C14 1.292(7) . ? N4 C13 1.463(6) . ? C1 C6 1.409(8) . ? C1 C2 1.410(8) . ? C2 C3 1.397(7) . ? C2 H2 0.9500 . ? C3 C4 1.403(8) . ? C3 H3 0.9500 . ? C4 C5 1.367(8) . ? C4 H4 0.9500 . ? C5 C6 1.404(7) . ? C5 H5 0.9500 . ? C6 C7 1.433(8) . ? C7 H7 0.9500 . ? C8 C9 1.520(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.511(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.520(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.437(7) . ? C14 H14 0.9500 . ? C15 C20 1.406(7) . ? C15 C16 1.417(7) . ? C16 C17 1.360(7) . ? C16 H16 0.9500 . ? C17 C18 1.397(8) . ? C17 H17 0.9500 . ? C18 C19 1.374(7) . ? C18 H18 0.9500 . ? C19 C20 1.406(7) . ? C19 H19 0.9500 . ? Ni1 S7 2.1608(16) . ? Ni1 S1 2.1615(16) . ? Ni1 S6 2.1627(17) . ? Ni1 S2 2.1652(17) . ? S1 C21 1.724(6) . ? S2 C22 1.728(5) . ? S3 C23 1.728(6) . ? S3 C21 1.743(5) . ? S4 C23 1.730(6) . ? S4 C22 1.754(6) . ? S5 C23 1.656(6) . ? S6 C25 1.713(5) . ? S7 C24 1.717(6) . ? S8 C26 1.719(5) . ? S8 C25 1.746(5) . ? S9 C26 1.734(6) . ? S9 C24 1.736(5) . ? S10 C26 1.658(5) . ? C21 C22 1.342(8) . ? C24 C25 1.360(8) . ? C30 O30 1.243(8) . ? C30 C32 1.426(11) . ? C30 C31 1.489(10) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C40 C41 1.443(13) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 N40 1.148(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe1 O1 96.67(16) . . ? O2 Fe1 N4 92.98(16) . . ? O1 Fe1 N4 85.40(17) . . ? O2 Fe1 N1 86.91(16) . . ? O1 Fe1 N1 93.73(16) . . ? N4 Fe1 N1 179.1(2) . . ? O2 Fe1 N2 88.80(16) . . ? O1 Fe1 N2 174.08(15) . . ? N4 Fe1 N2 96.63(18) . . ? N1 Fe1 N2 84.26(18) . . ? O2 Fe1 N3 172.47(16) . . ? O1 Fe1 N3 90.29(17) . . ? N4 Fe1 N3 84.67(17) . . ? N1 Fe1 N3 95.55(17) . . ? N2 Fe1 N3 84.37(17) . . ? C1 O1 Fe1 126.5(3) . . ? C20 O2 Fe1 124.9(3) . . ? C7 N1 C8 118.6(5) . . ? C7 N1 Fe1 125.6(4) . . ? C8 N1 Fe1 115.4(3) . . ? C9 N2 C10 114.3(4) . . ? C9 N2 Fe1 107.7(3) . . ? C10 N2 Fe1 111.8(3) . . ? C9 N2 H2N 107.6 . . ? C10 N2 H2N 107.6 . . ? Fe1 N2 H2N 107.6 . . ? C11 N3 C12 116.3(4) . . ? C11 N3 Fe1 110.8(3) . . ? C12 N3 Fe1 107.9(3) . . ? C11 N3 H3N 107.2 . . ? C12 N3 H3N 107.2 . . ? Fe1 N3 H3N 107.2 . . ? C14 N4 C13 119.6(5) . . ? C14 N4 Fe1 125.0(4) . . ? C13 N4 Fe1 114.8(3) . . ? O1 C1 C6 124.0(5) . . ? O1 C1 C2 117.5(5) . . ? C6 C1 C2 118.5(5) . . ? C3 C2 C1 121.0(5) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 119.7(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.5(5) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 122.0(5) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 119.3(5) . . ? C5 C6 C7 117.7(5) . . ? C1 C6 C7 123.0(5) . . ? N1 C7 C6 125.1(5) . . ? N1 C7 H7 117.4 . . ? C6 C7 H7 117.4 . . ? N1 C8 C9 107.2(4) . . ? N1 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? N1 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.5 . . ? N2 C9 C8 109.1(4) . . ? N2 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? N2 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C11 109.2(4) . . ? N2 C10 H10A 109.8 . . ? C11 C10 H10A 109.8 . . ? N2 C10 H10B 109.8 . . ? C11 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? N3 C11 C10 110.0(4) . . ? N3 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? N3 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N3 C12 C13 109.9(4) . . ? N3 C12 H12A 109.7 . . ? C13 C12 H12A 109.7 . . ? N3 C12 H12B 109.7 . . ? C13 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N4 C13 C12 106.3(4) . . ? N4 C13 H13A 110.5 . . ? C12 C13 H13A 110.5 . . ? N4 C13 H13B 110.5 . . ? C12 C13 H13B 110.5 . . ? H13A C13 H13B 108.7 . . ? N4 C14 C15 123.7(5) . . ? N4 C14 H14 118.1 . . ? C15 C14 H14 118.1 . . ? C20 C15 C16 118.7(5) . . ? C20 C15 C14 122.9(5) . . ? C16 C15 C14 118.4(5) . . ? C17 C16 C15 121.7(5) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 119.4(5) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 120.4(5) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 121.1(5) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? O2 C20 C15 124.5(4) . . ? O2 C20 C19 116.9(5) . . ? C15 C20 C19 118.6(4) . . ? S7 Ni1 S1 179.44(6) . . ? S7 Ni1 S6 93.36(6) . . ? S1 Ni1 S6 86.56(6) . . ? S7 Ni1 S2 86.53(6) . . ? S1 Ni1 S2 93.54(6) . . ? S6 Ni1 S2 178.66(6) . . ? C21 S1 Ni1 101.75(18) . . ? C22 S2 Ni1 101.43(19) . . ? C23 S3 C21 96.9(3) . . ? C23 S4 C22 96.1(3) . . ? C25 S6 Ni1 101.8(2) . . ? C24 S7 Ni1 102.03(18) . . ? C26 S8 C25 97.0(3) . . ? C26 S9 C24 96.9(3) . . ? C22 C21 S1 121.5(4) . . ? C22 C21 S3 116.2(4) . . ? S1 C21 S3 122.2(3) . . ? C21 C22 S2 121.7(4) . . ? C21 C22 S4 116.8(4) . . ? S2 C22 S4 121.4(3) . . ? S5 C23 S3 123.2(3) . . ? S5 C23 S4 122.7(4) . . ? S3 C23 S4 114.0(3) . . ? C25 C24 S7 121.0(4) . . ? C25 C24 S9 116.2(4) . . ? S7 C24 S9 122.8(3) . . ? C24 C25 S6 121.7(4) . . ? C24 C25 S8 116.1(4) . . ? S6 C25 S8 122.2(3) . . ? S10 C26 S8 123.2(3) . . ? S10 C26 S9 123.0(3) . . ? S8 C26 S9 113.8(3) . . ? O30 C30 C32 122.3(7) . . ? O30 C30 C31 120.2(7) . . ? C32 C30 C31 117.5(7) . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N40 C41 C40 174.1(12) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.79 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.675 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.116 # Attachment 't-1_250.cif' data_t-1'-250 _database_code_depnum_ccdc_archive 'CCDC 729930' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, C6 Ni S10,C2 H3 N, C3 H6 O' _chemical_formula_sum 'C31 H33 Fe N5 Ni O3 S10' _chemical_formula_weight 958.78 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' Ni Ni 0.3393 1.1124 '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 11.8510(6) _cell_length_b 12.6497(5) _cell_length_c 13.9373(7) _cell_angle_alpha 106.764(4) _cell_angle_beta 90.695(4) _cell_angle_gamma 92.602(4) _cell_volume 1997.81(16) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6373 _exptl_absorpt_correction_T_max 0.6583 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(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 'XCalibur Oxford Diffraction' _diffrn_measurement_method '\f scan' _diffrn_standards_decay_% negligible _diffrn_reflns_number 21275 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 32.00 _reflns_number_total 12574 _reflns_number_gt 8131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction Ltd., 2003)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction Ltd., 2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction Ltd., 2003)' _computing_structure_solution 'Sir97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997); ; Cameron (Watkin, 1996)' _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^)+(0.0489P)^2^+1.7151P] 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 12574 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 0.34548(3) 0.77255(3) 0.13847(3) 0.02581(9) Uani 1 1 d . . . O1 O 0.36603(17) 0.71763(15) -0.00070(14) 0.0334(4) Uani 1 1 d . . . O2 O 0.49598(16) 0.81810(15) 0.17344(15) 0.0335(4) Uani 1 1 d . . . N1 N 0.32359(19) 0.92093(18) 0.13429(16) 0.0296(5) Uani 1 1 d . . . N2 N 0.30534(19) 0.83266(19) 0.28332(16) 0.0295(5) Uani 1 1 d . . . H2N H 0.3546 0.8049 0.3203 0.035 Uiso 1 1 calc R . . N3 N 0.18164(19) 0.72292(19) 0.11868(17) 0.0321(5) Uani 1 1 d . . . H3N H 0.1540 0.7459 0.0664 0.038 Uiso 1 1 calc R . . N4 N 0.36732(19) 0.62352(18) 0.14176(17) 0.0293(5) Uani 1 1 d . . . C1 C 0.3855(2) 0.7775(2) -0.0628(2) 0.0319(6) Uani 1 1 d . . . C2 C 0.4123(3) 0.7217(3) -0.1620(2) 0.0431(7) Uani 1 1 d . . . H2 H 0.4183 0.6446 -0.1811 0.052 Uiso 1 1 calc R . . C3 C 0.4299(3) 0.7790(3) -0.2317(2) 0.0489(8) Uani 1 1 d . . . H3 H 0.4462 0.7400 -0.2979 0.059 Uiso 1 1 calc R . . C4 C 0.4242(3) 0.8925(3) -0.2058(2) 0.0506(8) Uani 1 1 d . . . H4 H 0.4375 0.9306 -0.2537 0.061 Uiso 1 1 calc R . . C5 C 0.3989(3) 0.9488(3) -0.1099(2) 0.0446(8) Uani 1 1 d . . . H5 H 0.3951 1.0261 -0.0921 0.054 Uiso 1 1 calc R . . C6 C 0.3784(2) 0.8935(2) -0.0369(2) 0.0341(6) Uani 1 1 d . . . C7 C 0.3455(3) 0.9592(2) 0.0603(2) 0.0356(6) Uani 1 1 d . . . H7 H 0.3397 1.0354 0.0703 0.043 Uiso 1 1 calc R . . C8 C 0.2878(3) 0.9968(2) 0.2279(2) 0.0385(6) Uani 1 1 d . . . H8A H 0.2053 0.9999 0.2277 0.046 Uiso 1 1 calc R . . H8B H 0.3208 1.0714 0.2358 0.046 Uiso 1 1 calc R . . C9 C 0.3277(3) 0.9546(2) 0.3126(2) 0.0376(6) Uani 1 1 d . . . H9A H 0.4088 0.9727 0.3260 0.045 Uiso 1 1 calc R . . H9B H 0.2874 0.9895 0.3737 0.045 Uiso 1 1 calc R . . C10 C 0.1899(2) 0.7948(3) 0.3019(2) 0.0364(6) Uani 1 1 d . . . H10A H 0.1578 0.8504 0.3577 0.044 Uiso 1 1 calc R . . H10B H 0.1926 0.7257 0.3200 0.044 Uiso 1 1 calc R . . C11 C 0.1165(2) 0.7769(3) 0.2083(2) 0.0389(6) Uani 1 1 d . . . H11A H 0.0493 0.7301 0.2117 0.047 Uiso 1 1 calc R . . H11B H 0.0916 0.8480 0.2035 0.047 Uiso 1 1 calc R . . C12 C 0.1739(3) 0.6003(3) 0.0861(3) 0.0431(7) Uani 1 1 d . . . H12A H 0.1850 0.5731 0.0137 0.052 Uiso 1 1 calc R . . H12B H 0.0987 0.5736 0.1001 0.052 Uiso 1 1 calc R . . C13 C 0.2629(3) 0.5568(2) 0.1413(3) 0.0408(7) Uani 1 1 d . . . H13A H 0.2399 0.5636 0.2100 0.049 Uiso 1 1 calc R . . H13B H 0.2739 0.4787 0.1072 0.049 Uiso 1 1 calc R . . C14 C 0.4630(2) 0.5788(2) 0.1327(2) 0.0340(6) Uani 1 1 d . . . H14 H 0.4628 0.5021 0.1229 0.041 Uiso 1 1 calc R . . C15 C 0.5708(2) 0.6370(2) 0.1363(2) 0.0306(5) Uani 1 1 d . . . C16 C 0.6686(3) 0.5761(3) 0.1216(2) 0.0405(7) Uani 1 1 d . . . H16 H 0.6615 0.4986 0.1053 0.049 Uiso 1 1 calc R . . C17 C 0.7741(3) 0.6276(3) 0.1305(3) 0.0469(8) Uani 1 1 d . . . H17 H 0.8388 0.5859 0.1201 0.056 Uiso 1 1 calc R . . C18 C 0.7844(3) 0.7423(3) 0.1550(3) 0.0481(8) Uani 1 1 d . . . H18 H 0.8566 0.7779 0.1607 0.058 Uiso 1 1 calc R . . C19 C 0.6908(2) 0.8042(3) 0.1711(2) 0.0391(7) Uani 1 1 d . . . H19 H 0.6996 0.8818 0.1901 0.047 Uiso 1 1 calc R . . C20 C 0.5819(2) 0.7531(2) 0.1594(2) 0.0304(5) Uani 1 1 d . . . Ni1 Ni 0.48530(3) 0.72206(3) 0.45952(3) 0.02637(8) Uani 1 1 d . . . S1 S 0.32387(5) 0.64007(6) 0.46992(6) 0.03389(15) Uani 1 1 d . . . S2 S 0.42446(5) 0.88486(5) 0.52537(5) 0.02914(14) Uani 1 1 d . . . S3 S 0.09964(6) 0.73290(6) 0.54678(6) 0.03639(16) Uani 1 1 d . . . S4 S 0.19195(6) 0.95827(6) 0.59555(6) 0.03745(16) Uani 1 1 d . . . S5 S -0.05249(7) 0.91713(8) 0.62209(8) 0.0585(3) Uani 1 1 d . . . S6 S 0.54818(6) 0.55930(6) 0.39789(6) 0.03656(16) Uani 1 1 d . . . S7 S 0.64656(6) 0.80452(6) 0.44948(6) 0.03576(16) Uani 1 1 d . . . S8 S 0.78444(6) 0.48722(6) 0.34296(6) 0.03952(17) Uani 1 1 d . . . S9 S 0.87508(6) 0.71264(6) 0.38961(6) 0.03644(16) Uani 1 1 d . . . S10 S 1.02869(7) 0.52946(8) 0.31541(8) 0.0553(2) Uani 1 1 d . . . C21 C 0.2426(2) 0.7494(2) 0.5246(2) 0.0290(5) Uani 1 1 d . . . C22 C 0.2858(2) 0.8553(2) 0.5479(2) 0.0289(5) Uani 1 1 d . . . C23 C 0.0738(2) 0.8717(3) 0.5906(2) 0.0369(6) Uani 1 1 d . . . C24 C 0.7308(2) 0.6955(2) 0.4054(2) 0.0302(5) Uani 1 1 d . . . C25 C 0.6882(2) 0.5893(2) 0.3836(2) 0.0317(6) Uani 1 1 d . . . C26 C 0.9019(2) 0.5743(2) 0.3465(2) 0.0361(6) Uani 1 1 d . . . C30 C 0.0939(3) 0.8559(4) 0.9159(3) 0.0666(11) Uani 1 1 d . . . C32 C 0.1006(6) 0.7540(6) 0.8336(5) 0.125(2) Uani 1 1 d . . . H32A H 0.0965 0.6910 0.8601 0.187 Uiso 1 1 calc R . . H32B H 0.1715 0.7556 0.7999 0.187 Uiso 1 1 calc R . . H32C H 0.0382 0.7479 0.7863 0.187 Uiso 1 1 calc R . . C31 C 0.0935(5) 0.9619(5) 0.8880(4) 0.105(2) Uani 1 1 d . . . H31A H 0.0198 0.9690 0.8601 0.158 Uiso 1 1 calc R . . H31B H 0.1506 0.9615 0.8387 0.158 Uiso 1 1 calc R . . H31C H 0.1098 1.0237 0.9473 0.158 Uiso 1 1 calc R . . O30 O 0.0933(3) 0.8553(3) 1.0022(2) 0.0716(8) Uani 1 1 d . . . C40 C 0.2601(6) 0.3314(5) 0.3386(5) 0.110(2) Uani 1 1 d . . . H40A H 0.1868 0.3439 0.3689 0.164 Uiso 1 1 calc R . . H40B H 0.3053 0.4004 0.3556 0.164 Uiso 1 1 calc R . . H40C H 0.2981 0.2779 0.3636 0.164 Uiso 1 1 calc R . . C41 C 0.2457(6) 0.2904(5) 0.2333(6) 0.108(2) Uani 1 1 d . . . N40 N 0.2253(9) 0.2521(8) 0.1524(6) 0.215(5) 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 0.02808(18) 0.02622(18) 0.02398(18) 0.00804(14) 0.00276(14) 0.00466(14) O1 0.0480(12) 0.0274(9) 0.0256(9) 0.0084(7) 0.0069(8) 0.0043(8) O2 0.0303(10) 0.0252(9) 0.0443(11) 0.0088(8) 0.0004(8) 0.0034(7) N1 0.0321(11) 0.0308(11) 0.0265(11) 0.0083(9) 0.0019(9) 0.0074(9) N2 0.0312(11) 0.0343(12) 0.0229(10) 0.0073(9) 0.0012(8) 0.0062(9) N3 0.0313(12) 0.0369(13) 0.0268(11) 0.0069(9) 0.0003(9) 0.0035(9) N4 0.0316(11) 0.0272(11) 0.0303(11) 0.0099(9) 0.0048(9) 0.0015(9) C1 0.0371(14) 0.0333(14) 0.0260(13) 0.0096(11) 0.0017(11) 0.0018(11) C2 0.0541(19) 0.0446(17) 0.0289(15) 0.0077(13) 0.0089(13) 0.0013(14) C3 0.058(2) 0.063(2) 0.0242(14) 0.0108(14) 0.0056(13) -0.0060(17) C4 0.059(2) 0.064(2) 0.0342(16) 0.0259(16) -0.0010(15) -0.0082(17) C5 0.055(2) 0.0445(18) 0.0400(17) 0.0229(14) -0.0069(14) -0.0091(15) C6 0.0382(15) 0.0384(15) 0.0274(13) 0.0132(11) -0.0026(11) -0.0024(12) C7 0.0417(15) 0.0290(14) 0.0366(15) 0.0104(11) -0.0038(12) 0.0035(11) C8 0.0474(17) 0.0287(14) 0.0374(15) 0.0045(11) 0.0075(13) 0.0131(12) C9 0.0461(17) 0.0325(14) 0.0291(14) 0.0009(11) 0.0016(12) 0.0028(12) C10 0.0401(16) 0.0406(16) 0.0289(14) 0.0104(12) 0.0082(11) 0.0027(12) C11 0.0292(14) 0.0484(17) 0.0369(15) 0.0080(13) 0.0079(11) 0.0065(12) C12 0.0369(16) 0.0395(16) 0.0474(18) 0.0045(14) 0.0024(13) -0.0033(13) C13 0.0382(16) 0.0326(15) 0.0519(19) 0.0129(13) 0.0124(13) -0.0022(12) C14 0.0400(15) 0.0268(13) 0.0362(15) 0.0105(11) 0.0045(12) 0.0049(11) C15 0.0337(14) 0.0302(13) 0.0289(13) 0.0090(10) 0.0036(10) 0.0093(11) C16 0.0394(16) 0.0386(16) 0.0434(17) 0.0097(13) 0.0064(13) 0.0140(13) C17 0.0370(16) 0.0515(19) 0.0493(19) 0.0077(15) 0.0023(14) 0.0157(14) C18 0.0294(15) 0.055(2) 0.058(2) 0.0149(17) -0.0032(14) 0.0036(14) C19 0.0324(14) 0.0350(15) 0.0495(18) 0.0116(13) -0.0039(13) 0.0017(12) C20 0.0303(13) 0.0337(14) 0.0289(13) 0.0112(11) 0.0028(10) 0.0060(10) Ni1 0.01965(15) 0.03058(17) 0.02998(17) 0.01005(13) 0.00414(12) 0.00341(12) S1 0.0227(3) 0.0281(3) 0.0506(4) 0.0103(3) 0.0077(3) 0.0039(2) S2 0.0235(3) 0.0307(3) 0.0322(3) 0.0076(3) 0.0031(2) 0.0004(2) S3 0.0214(3) 0.0402(4) 0.0469(4) 0.0109(3) 0.0082(3) 0.0044(3) S4 0.0310(3) 0.0342(4) 0.0421(4) 0.0020(3) 0.0069(3) 0.0079(3) S5 0.0313(4) 0.0639(6) 0.0703(6) 0.0005(5) 0.0156(4) 0.0183(4) S6 0.0228(3) 0.0297(3) 0.0564(5) 0.0108(3) 0.0108(3) 0.0012(2) S7 0.0240(3) 0.0285(3) 0.0521(4) 0.0070(3) 0.0094(3) 0.0023(2) S8 0.0273(3) 0.0315(4) 0.0590(5) 0.0106(3) 0.0140(3) 0.0056(3) S9 0.0216(3) 0.0348(4) 0.0501(4) 0.0076(3) 0.0080(3) 0.0004(3) S10 0.0285(4) 0.0487(5) 0.0844(7) 0.0106(5) 0.0222(4) 0.0094(3) C21 0.0189(11) 0.0386(14) 0.0299(13) 0.0096(11) 0.0049(9) 0.0064(10) C22 0.0224(11) 0.0377(14) 0.0284(13) 0.0111(11) 0.0054(9) 0.0104(10) C23 0.0304(14) 0.0425(16) 0.0355(15) 0.0066(12) 0.0037(11) 0.0071(12) C24 0.0202(11) 0.0367(14) 0.0331(14) 0.0087(11) 0.0057(10) 0.0022(10) C25 0.0222(12) 0.0353(14) 0.0383(15) 0.0108(12) 0.0048(10) 0.0066(10) C26 0.0264(13) 0.0377(15) 0.0424(16) 0.0084(12) 0.0074(11) 0.0031(11) C30 0.054(2) 0.083(3) 0.059(2) 0.013(2) -0.0086(18) 0.025(2) C32 0.133(6) 0.125(5) 0.084(4) -0.021(4) -0.029(4) 0.019(4) C31 0.100(4) 0.146(6) 0.099(4) 0.074(4) 0.021(3) 0.050(4) O30 0.076(2) 0.091(2) 0.0552(17) 0.0288(16) -0.0040(14) 0.0278(17) C40 0.123(5) 0.067(3) 0.132(6) 0.018(3) -0.020(4) 0.012(3) C41 0.141(6) 0.086(4) 0.114(5) 0.049(4) 0.001(5) 0.044(4) N40 0.360(14) 0.201(9) 0.102(5) 0.054(6) 0.001(7) 0.131(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 O2 1.8639(19) . ? Fe1 O1 1.8851(18) . ? Fe1 N1 1.924(2) . ? Fe1 N4 1.928(2) . ? Fe1 N3 2.004(2) . ? Fe1 N2 2.013(2) . ? O1 C1 1.320(3) . ? O2 C20 1.318(3) . ? N1 C7 1.284(4) . ? N1 C8 1.460(3) . ? N2 C10 1.479(4) . ? N2 C9 1.488(4) . ? N2 H2N 0.9200 . ? N3 C11 1.483(4) . ? N3 C12 1.484(4) . ? N3 H3N 0.9200 . ? N4 C14 1.282(3) . ? N4 C13 1.465(4) . ? C1 C2 1.406(4) . ? C1 C6 1.413(4) . ? C2 C3 1.382(4) . ? C2 H2 0.9400 . ? C3 C4 1.381(5) . ? C3 H3 0.9400 . ? C4 C5 1.365(5) . ? C4 H4 0.9400 . ? C5 C6 1.408(4) . ? C5 H5 0.9400 . ? C6 C7 1.439(4) . ? C7 H7 0.9400 . ? C8 C9 1.509(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.514(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.511(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.438(4) . ? C14 H14 0.9400 . ? C15 C16 1.405(4) . ? C15 C20 1.409(4) . ? C16 C17 1.371(5) . ? C16 H16 0.9400 . ? C17 C18 1.391(5) . ? C17 H17 0.9400 . ? C18 C19 1.370(4) . ? C18 H18 0.9400 . ? C19 C20 1.403(4) . ? C19 H19 0.9400 . ? Ni1 S2 2.1596(7) . ? Ni1 S6 2.1602(8) . ? Ni1 S7 2.1609(8) . ? Ni1 S1 2.1610(7) . ? S1 C21 1.718(3) . ? S2 C22 1.722(3) . ? S3 C23 1.728(3) . ? S3 C21 1.740(3) . ? S4 C23 1.726(3) . ? S4 C22 1.739(3) . ? S5 C23 1.646(3) . ? S6 C25 1.713(3) . ? S7 C24 1.711(3) . ? S8 C26 1.727(3) . ? S8 C25 1.736(3) . ? S9 C26 1.724(3) . ? S9 C24 1.738(3) . ? S10 C26 1.649(3) . ? C21 C22 1.358(4) . ? C24 C25 1.360(4) . ? C30 O30 1.206(5) . ? C30 C32 1.463(7) . ? C30 C31 1.500(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C40 C41 1.414(9) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 N40 1.111(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe1 O1 96.55(9) . . ? O2 Fe1 N1 86.90(9) . . ? O1 Fe1 N1 93.96(9) . . ? O2 Fe1 N4 93.22(9) . . ? O1 Fe1 N4 85.69(9) . . ? N1 Fe1 N4 179.64(10) . . ? O2 Fe1 N3 172.78(9) . . ? O1 Fe1 N3 90.11(9) . . ? N1 Fe1 N3 95.42(10) . . ? N4 Fe1 N3 84.51(10) . . ? O2 Fe1 N2 89.37(9) . . ? O1 Fe1 N2 173.62(9) . . ? N1 Fe1 N2 83.95(9) . . ? N4 Fe1 N2 96.39(9) . . ? N3 Fe1 N2 84.09(9) . . ? C1 O1 Fe1 126.12(17) . . ? C20 O2 Fe1 125.65(17) . . ? C7 N1 C8 118.7(2) . . ? C7 N1 Fe1 125.87(19) . . ? C8 N1 Fe1 115.24(17) . . ? C10 N2 C9 115.5(2) . . ? C10 N2 Fe1 111.74(17) . . ? C9 N2 Fe1 107.57(17) . . ? C10 N2 H2N 107.2 . . ? C9 N2 H2N 107.2 . . ? Fe1 N2 H2N 107.2 . . ? C11 N3 C12 115.9(2) . . ? C11 N3 Fe1 111.11(17) . . ? C12 N3 Fe1 108.05(17) . . ? C11 N3 H3N 107.1 . . ? C12 N3 H3N 107.1 . . ? Fe1 N3 H3N 107.1 . . ? C14 N4 C13 120.3(2) . . ? C14 N4 Fe1 124.40(19) . . ? C13 N4 Fe1 114.76(18) . . ? O1 C1 C2 117.8(3) . . ? O1 C1 C6 124.3(2) . . ? C2 C1 C6 117.9(3) . . ? C3 C2 C1 120.7(3) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 121.3(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.3(3) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.4(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.6(3) . . ? C5 C6 C7 117.2(3) . . ? C1 C6 C7 123.2(2) . . ? N1 C7 C6 124.6(3) . . ? N1 C7 H7 117.7 . . ? C6 C7 H7 117.7 . . ? N1 C8 C9 107.7(2) . . ? N1 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? N1 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? N2 C9 C8 108.5(2) . . ? N2 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? N2 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N2 C10 C11 109.5(2) . . ? N2 C10 H10A 109.8 . . ? C11 C10 H10A 109.8 . . ? N2 C10 H10B 109.8 . . ? C11 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? N3 C11 C10 109.6(2) . . ? N3 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? N3 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N3 C12 C13 109.8(2) . . ? N3 C12 H12A 109.7 . . ? C13 C12 H12A 109.7 . . ? N3 C12 H12B 109.7 . . ? C13 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N4 C13 C12 106.8(2) . . ? N4 C13 H13A 110.4 . . ? C12 C13 H13A 110.4 . . ? N4 C13 H13B 110.4 . . ? C12 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? N4 C14 C15 125.0(3) . . ? N4 C14 H14 117.5 . . ? C15 C14 H14 117.5 . . ? C16 C15 C20 119.2(3) . . ? C16 C15 C14 118.5(3) . . ? C20 C15 C14 122.2(2) . . ? C17 C16 C15 121.2(3) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 119.3(3) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 120.9(3) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 120.7(3) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? O2 C20 C19 117.2(2) . . ? O2 C20 C15 124.2(2) . . ? C19 C20 C15 118.6(2) . . ? S2 Ni1 S6 178.32(3) . . ? S2 Ni1 S7 86.54(3) . . ? S6 Ni1 S7 93.23(3) . . ? S2 Ni1 S1 93.29(3) . . ? S6 Ni1 S1 86.94(3) . . ? S7 Ni1 S1 179.81(4) . . ? C21 S1 Ni1 102.17(9) . . ? C22 S2 Ni1 102.09(9) . . ? C23 S3 C21 97.01(14) . . ? C23 S4 C22 96.88(14) . . ? C25 S6 Ni1 101.92(10) . . ? C24 S7 Ni1 102.07(9) . . ? C26 S8 C25 97.07(14) . . ? C26 S9 C24 97.07(13) . . ? C22 C21 S1 121.21(19) . . ? C22 C21 S3 115.93(19) . . ? S1 C21 S3 122.75(17) . . ? C21 C22 S2 121.23(19) . . ? C21 C22 S4 116.40(19) . . ? S2 C22 S4 122.30(17) . . ? S5 C23 S4 123.18(19) . . ? S5 C23 S3 123.05(19) . . ? S4 C23 S3 113.75(16) . . ? C25 C24 S7 121.2(2) . . ? C25 C24 S9 116.1(2) . . ? S7 C24 S9 122.70(16) . . ? C24 C25 S6 121.5(2) . . ? C24 C25 S8 116.1(2) . . ? S6 C25 S8 122.43(17) . . ? S10 C26 S9 123.14(18) . . ? S10 C26 S8 123.19(18) . . ? S9 C26 S8 113.63(15) . . ? O30 C30 C32 121.7(5) . . ? O30 C30 C31 121.4(4) . . ? C32 C30 C31 116.8(5) . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N40 C41 C40 172.9(10) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 0.816 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.098 # Attachment 't-1_293.cif' data_t-1'' _database_code_depnum_ccdc_archive 'CCDC 729931' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (N,N'-3,6-diazaoctane-1,8-diylbis(salicylidenealdiminato))-iron(iii) bis(2-thioxo-1,3-dithiole-4,5-dithiolato)-nickel, acetone solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, C6 Ni S10, C3 H6 O' _chemical_formula_sum 'C29 H30 Fe N4 Ni O3 S10' _chemical_formula_weight 917.73 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' Ni Ni 0.3393 1.1124 '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 11.9290(15) _cell_length_b 12.0800(16) _cell_length_c 16.541(2) _cell_angle_alpha 111.183(16) _cell_angle_beta 76.940(16) _cell_angle_gamma 115.272(14) _cell_volume 2002.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 24.8 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 1.389 _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 0.628 _exptl_absorpt_correction_T_max 0.757 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS).The crystal-to-detector distance was 80 mm. 250 exposures (3 min per exposure) were obtained with 0 < \f < 251\% and with the crystals rotated through 1.5\% in \f. Crystal decay was monitored by measuring 200 reflexions per image. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE Imaging Plate Diffraction System' _diffrn_measurement_method '\f scan ' _diffrn_standards_decay_% negligible _diffrn_reflns_number 16210 _diffrn_reflns_av_R_equivalents 0.1113 _diffrn_reflns_av_sigmaI/netI 0.1052 _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 -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.12 _reflns_number_total 5975 _reflns_number_gt 3712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS software (Stoe, 1996)' _computing_cell_refinement 'IPDS software (Stoe, 1996)' _computing_data_reduction 'IPDS software (Stoe, 1996)' _computing_structure_solution 'Sir97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997), Mercury (Bruno et al., 2002) and Cameron (Watkin, 1993) ; _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^)+(0.0859P)^2^] 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 5975 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1439 _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 -0.02137(8) 0.63900(8) 0.31064(6) 0.0381(3) Uani 1 1 d . . . N1 N -0.1258(4) 0.5417(5) 0.3893(4) 0.0466(15) Uani 1 1 d . . . N2 N -0.1285(5) 0.4919(5) 0.2204(4) 0.0509(15) Uani 1 1 d . . . HN2 H -0.0766 0.4694 0.1738 0.061 Uiso 1 1 calc R . . N3 N -0.1370(5) 0.7219(6) 0.3129(4) 0.0543(16) Uani 1 1 d . . . H3N H -0.1677 0.7465 0.3692 0.065 Uiso 1 1 calc R . . N4 N 0.0831(5) 0.7354(5) 0.2323(3) 0.0446(14) Uani 1 1 d . . . O1 O 0.0596(4) 0.7809(4) 0.4016(3) 0.0482(12) Uani 1 1 d . . . O2 O 0.0851(4) 0.5540(4) 0.2965(3) 0.0452(12) Uani 1 1 d . . . C1 C 0.0664(6) 0.7805(6) 0.4789(4) 0.0442(16) Uani 1 1 d . . . C2 C 0.1494(7) 0.8892(7) 0.5321(5) 0.058(2) Uani 1 1 d . . . H2 H 0.1983 0.9585 0.5109 0.070 Uiso 1 1 calc R . . C3 C 0.1616(9) 0.8977(8) 0.6149(5) 0.072(2) Uani 1 1 d . . . H3 H 0.2188 0.9719 0.6484 0.087 Uiso 1 1 calc R . . C4 C 0.0918(9) 0.7996(9) 0.6487(5) 0.080(3) Uani 1 1 d . . . H4 H 0.1013 0.8063 0.7048 0.096 Uiso 1 1 calc R . . C5 C 0.0070(8) 0.6903(8) 0.5996(5) 0.070(2) Uani 1 1 d . . . H5 H -0.0416 0.6236 0.6232 0.084 Uiso 1 1 calc R . . C6 C -0.0081(6) 0.6771(7) 0.5133(4) 0.0463(17) Uani 1 1 d . . . C7 C -0.1020(6) 0.5653(7) 0.4677(5) 0.0535(19) Uani 1 1 d . . . H7 H -0.1502 0.5041 0.4961 0.064 Uiso 1 1 calc R . . C8 C -0.2300(6) 0.4271(7) 0.3498(5) 0.064(2) Uani 1 1 d . . . H8A H -0.3030 0.4473 0.3580 0.077 Uiso 1 1 calc R . . H8B H -0.2496 0.3611 0.3768 0.077 Uiso 1 1 calc R . . C9 C -0.1936(7) 0.3806(7) 0.2553(5) 0.067(2) Uani 1 1 d . . . H9A H -0.1392 0.3356 0.2465 0.081 Uiso 1 1 calc R . . H9B H -0.2671 0.3214 0.2246 0.081 Uiso 1 1 calc R . . C10 C -0.2092(7) 0.5313(8) 0.1900(5) 0.072(2) Uani 1 1 d . . . H10A H -0.2837 0.4573 0.1698 0.086 Uiso 1 1 calc R . . H10B H -0.1656 0.5647 0.1416 0.086 Uiso 1 1 calc R . . C11 C -0.2447(7) 0.6320(8) 0.2619(5) 0.070(2) Uani 1 1 d . . . H11A H -0.2710 0.6783 0.2376 0.084 Uiso 1 1 calc R . . H11B H -0.3137 0.5920 0.2993 0.084 Uiso 1 1 calc R . . C12 C -0.0612(8) 0.8408(8) 0.2882(5) 0.064(2) Uani 1 1 d . . . H12A H -0.0153 0.9073 0.3364 0.077 Uiso 1 1 calc R . . H12B H -0.1147 0.8714 0.2733 0.077 Uiso 1 1 calc R . . C13 C 0.0263(7) 0.8107(7) 0.2120(5) 0.061(2) Uani 1 1 d . . . H13A H 0.0903 0.8892 0.2026 0.074 Uiso 1 1 calc R . . H13B H -0.0178 0.7607 0.1600 0.074 Uiso 1 1 calc R . . C14 C 0.1956(7) 0.7475(6) 0.2049(4) 0.0491(19) Uani 1 1 d . . . H14 H 0.2391 0.8030 0.1715 0.059 Uiso 1 1 calc R . . C15 C 0.2591(6) 0.6835(6) 0.2211(4) 0.0427(17) Uani 1 1 d . . . C16 C 0.3839(6) 0.7136(8) 0.1889(5) 0.062(2) Uani 1 1 d . . . H16 H 0.4215 0.7751 0.1596 0.075 Uiso 1 1 calc R . . C17 C 0.4506(7) 0.6544(8) 0.1999(6) 0.071(2) Uani 1 1 d . . . H17 H 0.5335 0.6751 0.1780 0.085 Uiso 1 1 calc R . . C18 C 0.3961(6) 0.5627(8) 0.2439(6) 0.067(2) Uani 1 1 d . . . H18 H 0.4425 0.5224 0.2515 0.081 Uiso 1 1 calc R . . C19 C 0.2756(6) 0.5323(7) 0.2757(5) 0.057(2) Uani 1 1 d . . . H19 H 0.2400 0.4702 0.3046 0.069 Uiso 1 1 calc R . . C20 C 0.2032(6) 0.5916(6) 0.2665(4) 0.0430(17) Uani 1 1 d . . . Ni1 Ni 0.46710(7) 0.18709(7) 0.10049(5) 0.0367(2) Uani 1 1 d . . . S1 S 0.64316(15) 0.18978(17) 0.02945(11) 0.0446(4) Uani 1 1 d . . . S2 S 0.47201(15) 0.08027(18) 0.17924(12) 0.0484(5) Uani 1 1 d . . . S3 S 0.82145(15) 0.08022(17) 0.04196(11) 0.0456(4) Uani 1 1 d . . . S4 S 0.66674(15) -0.01913(17) 0.18018(12) 0.0495(5) Uani 1 1 d . . . S5 S 0.90636(18) -0.05451(19) 0.11883(14) 0.0602(5) Uani 1 1 d . . . S6 S 0.47433(15) 0.30464(18) 0.02680(13) 0.0519(5) Uani 1 1 d . . . S7 S 0.28065(14) 0.17047(17) 0.15885(11) 0.0434(4) Uani 1 1 d . . . S8 S 0.28152(16) 0.38829(17) 0.00497(12) 0.0504(5) Uani 1 1 d . . . S9 S 0.10014(15) 0.26163(17) 0.12243(11) 0.0441(4) Uani 1 1 d . . . S10 S 0.03329(18) 0.3995(2) 0.03496(13) 0.0571(5) Uani 1 1 d . . . C21 C 0.6822(5) 0.1064(6) 0.0751(4) 0.0358(15) Uani 1 1 d . . . C22 C 0.6094(5) 0.0592(6) 0.1391(4) 0.0351(15) Uani 1 1 d . . . C23 C 0.8033(6) -0.0011(6) 0.1140(4) 0.0401(15) Uani 1 1 d . . . C24 C 0.2431(5) 0.2498(6) 0.1079(4) 0.0343(14) Uani 1 1 d . . . C25 C 0.3284(5) 0.3080(6) 0.0507(4) 0.0406(16) Uani 1 1 d . . . C26 C 0.1334(6) 0.3516(6) 0.0541(4) 0.0415(16) Uani 1 1 d . . . C30 C 0.3000(10) 0.2470(13) 0.4447(7) 0.103(4) Uani 1 1 d . . . C31 C 0.2156(10) 0.1303(11) 0.3923(8) 0.119(4) Uani 1 1 d . . . H31A H 0.1582 0.0806 0.4290 0.179 Uiso 1 1 calc R . . H31B H 0.2614 0.0819 0.3511 0.179 Uiso 1 1 calc R . . H31C H 0.1705 0.1501 0.3618 0.179 Uiso 1 1 calc R . . C32 C 0.3970(13) 0.3381(13) 0.3968(9) 0.179(7) Uani 1 1 d . . . H52A H 0.3680 0.4018 0.3984 0.269 Uiso 1 1 calc R . . H52B H 0.4110 0.2908 0.3374 0.269 Uiso 1 1 calc R . . H52C H 0.4734 0.3794 0.4243 0.269 Uiso 1 1 calc R . . O30 O 0.2950(8) 0.2786(11) 0.5230(5) 0.150(4) 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 0.0370(5) 0.0427(5) 0.0354(5) 0.0135(4) 0.0004(4) 0.0161(4) N1 0.033(3) 0.048(3) 0.051(4) 0.015(3) 0.010(3) 0.014(3) N2 0.045(3) 0.057(4) 0.043(3) 0.006(3) -0.003(3) 0.021(3) N3 0.065(4) 0.070(4) 0.039(3) 0.012(3) -0.001(3) 0.042(3) N4 0.050(3) 0.043(3) 0.042(3) 0.016(3) -0.005(3) 0.015(3) O1 0.061(3) 0.046(3) 0.039(3) 0.019(2) -0.012(2) 0.013(2) O2 0.033(2) 0.046(3) 0.064(3) 0.032(2) 0.009(2) 0.015(2) C1 0.054(4) 0.048(4) 0.038(4) 0.011(3) -0.008(3) 0.026(3) C2 0.073(5) 0.054(4) 0.048(5) 0.011(4) -0.019(4) 0.022(4) C3 0.103(7) 0.074(6) 0.051(5) 0.007(4) -0.030(5) 0.042(5) C4 0.111(7) 0.095(7) 0.041(5) 0.017(5) -0.014(5) 0.045(6) C5 0.087(6) 0.082(6) 0.057(5) 0.036(5) 0.011(5) 0.044(5) C6 0.056(4) 0.057(4) 0.036(4) 0.020(3) 0.000(3) 0.027(4) C7 0.050(4) 0.062(5) 0.048(5) 0.030(4) 0.018(4) 0.021(4) C8 0.044(4) 0.068(5) 0.065(5) 0.024(4) 0.002(4) 0.007(4) C9 0.055(5) 0.056(5) 0.071(6) 0.009(4) -0.010(4) 0.009(4) C10 0.060(5) 0.084(6) 0.067(5) 0.007(5) -0.021(4) 0.028(5) C11 0.061(5) 0.090(6) 0.067(6) 0.008(5) -0.019(4) 0.043(5) C12 0.093(6) 0.071(5) 0.054(5) 0.016(4) -0.009(4) 0.055(5) C13 0.081(5) 0.061(5) 0.067(5) 0.034(4) -0.013(4) 0.035(4) C14 0.055(4) 0.047(4) 0.041(4) 0.021(3) -0.003(3) 0.009(4) C15 0.036(3) 0.047(4) 0.041(4) 0.017(3) 0.001(3) 0.011(3) C16 0.034(4) 0.071(5) 0.079(6) 0.036(5) 0.010(4) 0.012(4) C17 0.035(4) 0.083(6) 0.086(6) 0.037(5) 0.016(4) 0.017(4) C18 0.037(4) 0.081(6) 0.090(6) 0.030(5) 0.004(4) 0.029(4) C19 0.045(4) 0.058(4) 0.080(6) 0.032(4) 0.001(4) 0.024(4) C20 0.036(4) 0.044(4) 0.047(4) 0.016(3) -0.002(3) 0.011(3) Ni1 0.0293(4) 0.0438(5) 0.0408(5) 0.0154(4) -0.0037(3) 0.0147(4) S1 0.0409(9) 0.0621(11) 0.0444(10) 0.0253(9) 0.0032(7) 0.0278(8) S2 0.0337(8) 0.0633(11) 0.0587(12) 0.0341(9) 0.0038(8) 0.0190(8) S3 0.0449(9) 0.0619(11) 0.0440(10) 0.0199(9) 0.0013(8) 0.0323(8) S4 0.0428(9) 0.0558(11) 0.0611(12) 0.0311(9) -0.0058(8) 0.0171(8) S5 0.0684(12) 0.0712(12) 0.0670(13) 0.0235(11) -0.0072(10) 0.0474(11) S6 0.0335(9) 0.0692(12) 0.0676(13) 0.0424(10) 0.0109(8) 0.0224(8) S7 0.0349(8) 0.0589(10) 0.0488(10) 0.0303(9) 0.0034(7) 0.0210(8) S8 0.0448(10) 0.0596(11) 0.0637(12) 0.0390(10) 0.0060(8) 0.0238(9) S9 0.0364(8) 0.0610(11) 0.0502(10) 0.0290(9) 0.0052(7) 0.0270(8) S10 0.0635(12) 0.0828(13) 0.0544(12) 0.0314(10) 0.0083(9) 0.0522(11) C21 0.031(3) 0.040(3) 0.041(4) 0.013(3) -0.006(3) 0.016(3) C22 0.029(3) 0.038(3) 0.039(4) 0.012(3) -0.007(3) 0.010(3) C23 0.048(4) 0.039(3) 0.039(4) 0.007(3) -0.011(3) 0.021(3) C24 0.027(3) 0.041(3) 0.040(4) 0.019(3) 0.001(3) 0.015(3) C25 0.034(3) 0.040(3) 0.053(4) 0.023(3) -0.005(3) 0.011(3) C26 0.047(4) 0.048(4) 0.039(4) 0.016(3) 0.000(3) 0.026(3) C30 0.088(7) 0.155(11) 0.069(7) 0.036(7) 0.028(6) 0.065(7) C31 0.114(9) 0.111(9) 0.105(9) 0.042(7) -0.014(7) 0.009(7) C32 0.154(12) 0.152(13) 0.121(11) 0.018(10) 0.010(9) -0.013(10) O30 0.135(7) 0.266(12) 0.060(5) 0.038(6) 0.024(4) 0.113(7) _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 1.874(4) . ? Fe1 O2 1.878(4) . ? Fe1 N4 1.927(5) . ? Fe1 N1 1.936(5) . ? Fe1 N2 2.006(5) . ? Fe1 N3 2.010(6) . ? N1 C7 1.293(9) . ? N1 C8 1.461(8) . ? N2 C10 1.480(10) . ? N2 C9 1.486(9) . ? N3 C11 1.476(9) . ? N3 C12 1.482(9) . ? N4 C14 1.278(8) . ? N4 C13 1.498(9) . ? O1 C1 1.301(8) . ? O2 C20 1.318(7) . ? C1 C2 1.388(9) . ? C1 C6 1.419(9) . ? C2 C3 1.373(10) . ? C3 C4 1.355(11) . ? C4 C5 1.372(11) . ? C5 C6 1.421(10) . ? C6 C7 1.415(10) . ? C8 C9 1.488(10) . ? C10 C11 1.496(11) . ? C12 C13 1.486(10) . ? C14 C15 1.409(10) . ? C15 C16 1.397(9) . ? C15 C20 1.409(9) . ? C16 C17 1.350(11) . ? C17 C18 1.390(11) . ? C18 C19 1.350(9) . ? C19 C20 1.397(10) . ? Ni1 S6 2.147(2) . ? Ni1 S1 2.1556(18) . ? Ni1 S2 2.163(2) . ? Ni1 S7 2.1697(18) . ? S1 C21 1.706(7) . ? S2 C22 1.713(6) . ? S3 C23 1.726(7) . ? S3 C21 1.752(6) . ? S4 C23 1.721(7) . ? S4 C22 1.747(7) . ? S5 C23 1.641(7) . ? S6 C25 1.711(6) . ? S7 C24 1.717(6) . ? S8 C26 1.709(6) . ? S8 C25 1.735(7) . ? S9 C26 1.713(7) . ? S9 C24 1.728(6) . ? S10 C26 1.660(7) . ? C21 C22 1.342(8) . ? C24 C25 1.364(8) . ? C30 O30 1.206(12) . ? C30 C31 1.432(14) . ? C30 C32 1.519(15) . ? 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 O2 95.0(2) . . ? O1 Fe1 N4 87.3(2) . . ? O2 Fe1 N4 93.4(2) . . ? O1 Fe1 N1 92.7(2) . . ? O2 Fe1 N1 86.3(2) . . ? N4 Fe1 N1 179.7(3) . . ? O1 Fe1 N2 172.4(2) . . ? O2 Fe1 N2 91.7(2) . . ? N4 Fe1 N2 95.9(2) . . ? N1 Fe1 N2 84.1(2) . . ? O1 Fe1 N3 89.9(2) . . ? O2 Fe1 N3 174.3(2) . . ? N4 Fe1 N3 83.8(2) . . ? N1 Fe1 N3 96.5(2) . . ? N2 Fe1 N3 83.6(2) . . ? C7 N1 C8 120.8(6) . . ? C7 N1 Fe1 124.7(4) . . ? C8 N1 Fe1 114.1(5) . . ? C10 N2 C9 115.8(6) . . ? C10 N2 Fe1 111.1(4) . . ? C9 N2 Fe1 108.4(4) . . ? C11 N3 C12 115.6(7) . . ? C11 N3 Fe1 112.5(5) . . ? C12 N3 Fe1 107.6(5) . . ? C14 N4 C13 120.4(6) . . ? C14 N4 Fe1 125.3(5) . . ? C13 N4 Fe1 114.0(4) . . ? C1 O1 Fe1 126.6(4) . . ? C20 O2 Fe1 125.8(4) . . ? O1 C1 C2 118.2(6) . . ? O1 C1 C6 124.1(6) . . ? C2 C1 C6 117.7(6) . . ? C3 C2 C1 122.0(7) . . ? C4 C3 C2 121.1(8) . . ? C3 C4 C5 119.5(8) . . ? C4 C5 C6 121.4(8) . . ? C7 C6 C1 122.8(6) . . ? C7 C6 C5 118.7(7) . . ? C1 C6 C5 118.3(6) . . ? N1 C7 C6 124.9(6) . . ? N1 C8 C9 108.2(6) . . ? N2 C9 C8 109.3(6) . . ? N2 C10 C11 110.6(6) . . ? N3 C11 C10 109.5(6) . . ? N3 C12 C13 108.1(6) . . ? C12 C13 N4 106.8(6) . . ? N4 C14 C15 125.4(6) . . ? C16 C15 C20 119.4(7) . . ? C16 C15 C14 117.0(7) . . ? C20 C15 C14 123.6(6) . . ? C17 C16 C15 120.7(7) . . ? C16 C17 C18 120.4(7) . . ? C19 C18 C17 120.0(8) . . ? C18 C19 C20 121.7(7) . . ? O2 C20 C19 118.4(6) . . ? O2 C20 C15 123.7(7) . . ? C19 C20 C15 117.8(6) . . ? S6 Ni1 S1 85.03(7) . . ? S6 Ni1 S2 175.70(8) . . ? S1 Ni1 S2 93.12(7) . . ? S6 Ni1 S7 93.08(7) . . ? S1 Ni1 S7 173.73(8) . . ? S2 Ni1 S7 89.16(7) . . ? C21 S1 Ni1 101.8(2) . . ? C22 S2 Ni1 101.7(2) . . ? C23 S3 C21 97.2(3) . . ? C23 S4 C22 97.9(3) . . ? C25 S6 Ni1 102.3(2) . . ? C24 S7 Ni1 102.3(2) . . ? C26 S8 C25 97.0(3) . . ? C26 S9 C24 97.7(3) . . ? C22 C21 S1 122.0(5) . . ? C22 C21 S3 116.3(5) . . ? S1 C21 S3 121.6(4) . . ? C21 C22 S2 121.3(5) . . ? C21 C22 S4 115.6(5) . . ? S2 C22 S4 123.1(4) . . ? S5 C23 S4 123.9(4) . . ? S5 C23 S3 123.2(4) . . ? S4 C23 S3 112.9(4) . . ? C25 C24 S7 120.2(5) . . ? C25 C24 S9 115.2(5) . . ? S7 C24 S9 124.6(3) . . ? C24 C25 S6 121.9(5) . . ? C24 C25 S8 116.2(5) . . ? S6 C25 S8 121.8(4) . . ? S10 C26 S8 121.8(4) . . ? S10 C26 S9 124.4(4) . . ? S8 C26 S9 113.8(4) . . ? O30 C30 C31 124.4(11) . . ? O30 C30 C32 119.1(12) . . ? C31 C30 C32 116.4(10) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 24.12 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.069 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.113