# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'Christophe Faulmann' _publ_contact_author_address ; CNRS Laboratoire de Chimie de Coordination 205 route de Narbonne Toulouse Cedex 04 31077 FRANCE ; _publ_contact_author_email FAULMANN@LCC-TOULOUSE.FR _publ_section_title ; [Fe(sal2-trien)][Ni(dmit)2]: Towards Switchable Spin Crossover Molecular Conductors ; loop_ _publ_author_name 'Christophe Faulmann' 'Stephane Dorbes' 'Jose A. Real' 'Lydie Valade' data_nife295 _database_code_depnum_ccdc_archive 'CCDC 246500' _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' _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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2530(9) _cell_length_b 11.7080(12) _cell_length_c 17.241(2) _cell_angle_alpha 79.490(13) _cell_angle_beta 78.107(13) _cell_angle_gamma 68.481(11) _cell_volume 1688.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 25.9 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.639 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.3984 _exptl_absorpt_correction_T_max 0.7123 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _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. 179 exposures (3 min per exposure) were obtained with 0 < \f < 251\% and with the crystals rotated through 1.4\% 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 6108 _diffrn_reflns_av_R_equivalents 0.1064 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.99 _reflns_number_total 6108 _reflns_number_gt 4811 _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) 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^)+(0.0650P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6108 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _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 0.07430(5) 0.18627(4) 0.67769(3) 0.04429(14) Uani 1 1 d . . . N1 N 0.1446(3) -0.0088(2) 0.68686(17) 0.0511(6) Uani 1 1 d . . . N2 N -0.1346(3) 0.1490(3) 0.74576(18) 0.0535(7) Uani 1 1 d . . . H2N H -0.2206 0.2125 0.7314 0.064 Uiso 1 1 calc R . . N3 N 0.0780(3) 0.2205(3) 0.79762(17) 0.0524(7) Uani 1 1 d . . . H3N H 0.1474 0.1524 0.8213 0.063 Uiso 1 1 calc R . . N4 N -0.0003(3) 0.3817(2) 0.67197(16) 0.0462(6) Uani 1 1 d . . . O1 O 0.2898(3) 0.1672(2) 0.64419(18) 0.0648(7) Uani 1 1 d . . . O2 O -0.0110(3) 0.2122(2) 0.58089(14) 0.0580(6) Uani 1 1 d . . . C1 C 0.4174(4) 0.0738(3) 0.6224(2) 0.0542(8) Uani 1 1 d . . . C2 C 0.5577(4) 0.0979(4) 0.5901(3) 0.0684(10) Uani 1 1 d . . . H2 H 0.5605 0.1773 0.5868 0.082 Uiso 1 1 calc R . . C3 C 0.6915(4) 0.0031(5) 0.5633(3) 0.0743(12) Uani 1 1 d . . . H3 H 0.7831 0.0201 0.5417 0.089 Uiso 1 1 calc R . . C4 C 0.6919(5) -0.1152(5) 0.5678(3) 0.0780(13) Uani 1 1 d . . . H4 H 0.7827 -0.1778 0.5496 0.094 Uiso 1 1 calc R . . C5 C 0.5561(5) -0.1396(4) 0.5997(3) 0.0728(12) Uani 1 1 d . . . H5 H 0.5556 -0.2197 0.6030 0.087 Uiso 1 1 calc R . . C6 C 0.4173(4) -0.0460(3) 0.6275(2) 0.0551(9) Uani 1 1 d . . . C7 C 0.2820(4) -0.0816(3) 0.6616(2) 0.0567(9) Uani 1 1 d . . . H7 H 0.2956 -0.1651 0.6657 0.068 Uiso 1 1 calc R . . C8 C 0.0232(5) -0.0630(4) 0.7230(3) 0.0675(10) Uani 1 1 d . . . H81 H 0.0366 -0.0970 0.7777 0.081 Uiso 1 1 calc R . . H82 H 0.0328 -0.1295 0.6938 0.081 Uiso 1 1 calc R . . C9 C -0.1370(5) 0.0352(4) 0.7209(3) 0.0717(11) Uani 1 1 d . . . H91 H -0.1632 0.0521 0.6673 0.086 Uiso 1 1 calc R . . H92 H -0.2159 0.0069 0.7567 0.086 Uiso 1 1 calc R . . C10 C -0.1388(5) 0.1447(4) 0.8317(2) 0.0629(9) Uani 1 1 d . . . H101 H -0.0733 0.0637 0.8527 0.076 Uiso 1 1 calc R . . H102 H -0.2456 0.1595 0.8592 0.076 Uiso 1 1 calc R . . C11 C -0.0802(4) 0.2414(4) 0.8451(2) 0.0581(9) Uani 1 1 d . . . H111 H -0.1510 0.3230 0.8286 0.070 Uiso 1 1 calc R . . H112 H -0.0748 0.2360 0.9013 0.070 Uiso 1 1 calc R . . C12 C 0.1348(4) 0.3240(4) 0.7884(2) 0.0600(9) Uani 1 1 d . . . H121 H 0.2459 0.2977 0.7669 0.072 Uiso 1 1 calc R . . H122 H 0.1217 0.3512 0.8401 0.072 Uiso 1 1 calc R . . C13 C 0.0447(5) 0.4300(3) 0.7330(2) 0.0569(8) Uani 1 1 d . . . H131 H -0.0489 0.4825 0.7633 0.068 Uiso 1 1 calc R . . H132 H 0.1094 0.4795 0.7074 0.068 Uiso 1 1 calc R . . C14 C -0.0773(4) 0.4599(3) 0.61954(19) 0.0465(7) Uani 1 1 d . . . H14 H -0.0957 0.5429 0.6216 0.056 Uiso 1 1 calc R . . C15 C -0.1378(4) 0.4314(3) 0.55817(19) 0.0456(7) Uani 1 1 d . . . C16 C -0.2345(4) 0.5301(3) 0.5116(2) 0.0599(9) Uani 1 1 d . . . H16 H -0.2550 0.6106 0.5212 0.072 Uiso 1 1 calc R . . C17 C -0.2990(5) 0.5113(4) 0.4527(3) 0.0701(11) Uani 1 1 d . . . H17 H -0.3649 0.5780 0.4238 0.084 Uiso 1 1 calc R . . C18 C -0.2653(5) 0.3915(4) 0.4366(3) 0.0725(11) Uani 1 1 d . . . H18 H -0.3089 0.3779 0.3966 0.087 Uiso 1 1 calc R . . C19 C -0.1684(5) 0.2936(4) 0.4791(2) 0.0664(10) Uani 1 1 d . . . H19 H -0.1449 0.2142 0.4665 0.080 Uiso 1 1 calc R . . C20 C -0.1033(4) 0.3096(3) 0.54152(19) 0.0475(7) Uani 1 1 d . . . Ni1 Ni 0.35897(4) -0.06261(3) 0.89797(2) 0.04319(13) Uani 1 1 d . . . S1 S 0.55096(10) -0.17003(8) 0.81719(6) 0.0540(2) Uani 1 1 d . . . S2 S 0.22614(10) -0.18567(8) 0.91136(6) 0.0562(2) Uani 1 1 d . . . S3 S 0.59883(10) -0.40722(9) 0.75287(6) 0.0587(2) Uani 1 1 d . . . S4 S 0.30169(10) -0.42030(8) 0.83584(7) 0.0617(3) Uani 1 1 d . . . S5 S 0.50460(11) -0.61601(9) 0.73287(7) 0.0632(3) Uani 1 1 d . . . S6 S 0.48332(10) 0.06607(8) 0.87843(6) 0.0549(2) Uani 1 1 d . . . S7 S 0.17595(10) 0.04106(8) 0.98390(5) 0.0525(2) Uani 1 1 d . . . S8 S 0.41833(12) 0.29841(8) 0.95314(6) 0.0593(2) Uani 1 1 d . . . S9 S 0.13080(12) 0.27817(9) 1.04883(6) 0.0639(3) Uani 1 1 d . . . S10 S 0.22380(18) 0.49299(11) 1.05684(8) 0.0865(4) Uani 1 1 d . . . C21 C 0.4875(4) -0.2883(3) 0.8110(2) 0.0474(7) Uani 1 1 d . . . C22 C 0.3486(4) -0.2948(3) 0.8501(2) 0.0469(7) Uani 1 1 d . . . C23 C 0.4697(4) -0.4878(3) 0.7714(2) 0.0486(7) Uani 1 1 d . . . C24 C 0.2369(4) 0.1606(3) 0.98904(19) 0.0483(7) Uani 1 1 d . . . C25 C 0.3704(4) 0.1717(3) 0.9430(2) 0.0477(7) Uani 1 1 d . . . C26 C 0.2560(5) 0.3636(3) 1.0215(2) 0.0585(9) 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 0.0390(2) 0.0459(2) 0.0401(2) -0.00202(19) -0.00406(19) -0.00779(18) N1 0.0509(15) 0.0518(14) 0.0480(15) -0.0020(12) -0.0079(13) -0.0161(12) N2 0.0384(13) 0.0689(16) 0.0498(16) -0.0046(14) -0.0085(12) -0.0144(12) N3 0.0438(13) 0.0629(15) 0.0473(15) -0.0003(13) -0.0127(13) -0.0143(12) N4 0.0456(13) 0.0508(13) 0.0390(13) -0.0055(11) -0.0045(12) -0.0138(11) O1 0.0412(12) 0.0554(12) 0.087(2) -0.0114(13) 0.0084(13) -0.0129(10) O2 0.0755(16) 0.0487(11) 0.0420(12) -0.0056(10) -0.0142(12) -0.0092(11) C1 0.0414(16) 0.067(2) 0.0468(18) -0.0093(16) -0.0069(15) -0.0086(15) C2 0.0455(18) 0.085(2) 0.070(3) -0.016(2) 0.0008(19) -0.0188(18) C3 0.0420(18) 0.116(4) 0.054(2) -0.016(2) -0.0011(17) -0.016(2) C4 0.056(2) 0.093(3) 0.059(2) -0.021(2) 0.0033(19) 0.003(2) C5 0.066(2) 0.070(2) 0.063(2) -0.022(2) -0.004(2) 0.0024(19) C6 0.0510(18) 0.0622(19) 0.0402(17) -0.0115(15) -0.0086(15) -0.0023(15) C7 0.066(2) 0.0461(16) 0.0515(19) -0.0098(15) -0.0107(17) -0.0088(15) C8 0.073(2) 0.062(2) 0.070(3) -0.0081(19) -0.001(2) -0.0307(19) C9 0.063(2) 0.092(3) 0.070(3) -0.008(2) -0.006(2) -0.041(2) C10 0.057(2) 0.083(2) 0.0460(19) -0.0048(18) 0.0017(17) -0.0272(19) C11 0.060(2) 0.072(2) 0.0389(17) -0.0050(16) -0.0013(16) -0.0226(17) C12 0.0519(18) 0.080(2) 0.054(2) -0.0066(19) -0.0157(17) -0.0251(17) C13 0.062(2) 0.0611(19) 0.052(2) -0.0097(16) -0.0124(17) -0.0227(16) C14 0.0437(15) 0.0440(14) 0.0434(17) -0.0055(13) 0.0027(14) -0.0102(13) C15 0.0380(14) 0.0515(16) 0.0395(16) -0.0024(13) 0.0008(13) -0.0113(12) C16 0.0533(19) 0.0561(18) 0.058(2) 0.0002(17) -0.0097(17) -0.0078(15) C17 0.062(2) 0.075(2) 0.060(2) 0.006(2) -0.022(2) -0.0091(19) C18 0.079(3) 0.086(3) 0.059(2) 0.003(2) -0.029(2) -0.031(2) C19 0.086(3) 0.067(2) 0.052(2) 0.0016(18) -0.019(2) -0.032(2) C20 0.0481(16) 0.0529(16) 0.0340(15) 0.0017(13) -0.0006(13) -0.0147(13) Ni1 0.0365(2) 0.0464(2) 0.0424(2) -0.00275(18) -0.00333(18) -0.01187(16) S1 0.0437(4) 0.0629(5) 0.0569(5) -0.0154(4) 0.0061(4) -0.0233(4) S2 0.0403(4) 0.0550(4) 0.0686(6) -0.0155(4) 0.0101(4) -0.0167(3) S3 0.0446(4) 0.0646(5) 0.0645(6) -0.0220(4) 0.0091(4) -0.0185(4) S4 0.0452(4) 0.0534(4) 0.0841(7) -0.0187(5) 0.0080(4) -0.0184(4) S5 0.0525(5) 0.0607(5) 0.0763(6) -0.0230(5) -0.0095(5) -0.0123(4) S6 0.0447(4) 0.0556(4) 0.0617(5) -0.0162(4) 0.0094(4) -0.0190(4) S7 0.0443(4) 0.0616(5) 0.0471(5) -0.0067(4) 0.0030(4) -0.0180(4) S8 0.0653(5) 0.0532(4) 0.0590(5) -0.0126(4) -0.0024(4) -0.0206(4) S9 0.0583(5) 0.0741(6) 0.0524(5) -0.0227(5) 0.0035(4) -0.0138(4) S10 0.1139(10) 0.0680(6) 0.0745(7) -0.0305(6) -0.0101(7) -0.0192(6) C21 0.0392(14) 0.0508(15) 0.0463(17) -0.0096(14) -0.0021(14) -0.0090(13) C22 0.0407(15) 0.0457(15) 0.0497(18) -0.0064(14) -0.0029(14) -0.0111(12) C23 0.0404(15) 0.0521(16) 0.0492(18) -0.0063(14) -0.0086(14) -0.0099(13) C24 0.0449(16) 0.0544(16) 0.0382(16) -0.0067(14) -0.0063(14) -0.0075(13) C25 0.0468(16) 0.0484(15) 0.0433(17) -0.0078(14) -0.0089(14) -0.0089(13) C26 0.068(2) 0.0552(18) 0.0443(18) -0.0101(15) -0.0116(17) -0.0087(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.899(2) . ? Fe1 O2 1.919(2) . ? Fe1 N1 2.118(3) . ? Fe1 N4 2.124(3) . ? Fe1 N3 2.186(3) . ? Fe1 N2 2.191(3) . ? N1 C7 1.283(4) . ? N1 C8 1.464(5) . ? N2 C10 1.467(5) . ? N2 C9 1.481(5) . ? N2 H2N 0.9100 . ? N3 C12 1.460(5) . ? N3 C11 1.480(4) . ? N3 H3N 0.9100 . ? N4 C14 1.284(4) . ? N4 C13 1.473(4) . ? O1 C1 1.323(4) . ? O2 C20 1.316(4) . ? C1 C6 1.390(5) . ? C1 C2 1.410(6) . ? C2 C3 1.386(5) . ? C2 H2 0.9300 . ? C3 C4 1.371(7) . ? C3 H3 0.9300 . ? C4 C5 1.373(7) . ? C4 H4 0.9300 . ? C5 C6 1.409(4) . ? C5 H5 0.9300 . ? C6 C7 1.441(6) . ? C7 H7 0.9300 . ? C8 C9 1.509(6) . ? C8 H81 0.9700 . ? C8 H82 0.9700 . ? C9 H91 0.9700 . ? C9 H92 0.9700 . ? C10 C11 1.493(6) . ? C10 H101 0.9700 . ? C10 H102 0.9700 . ? C11 H111 0.9700 . ? C11 H112 0.9700 . ? C12 C13 1.511(5) . ? C12 H121 0.9700 . ? C12 H122 0.9700 . ? C13 H131 0.9700 . ? C13 H132 0.9700 . ? C14 C15 1.433(5) . ? C14 H14 0.9300 . ? C15 C16 1.407(5) . ? C15 C20 1.412(5) . ? C16 C17 1.364(6) . ? C16 H16 0.9300 . ? C17 C18 1.388(6) . ? C17 H17 0.9300 . ? C18 C19 1.367(6) . ? C18 H18 0.9300 . ? C19 C20 1.407(5) . ? C19 H19 0.9300 . ? Ni1 S6 2.1527(10) . ? Ni1 S7 2.1564(10) . ? Ni1 S1 2.1581(9) . ? Ni1 S2 2.1681(10) . ? S1 C21 1.718(4) . ? S2 C22 1.723(3) . ? S3 C23 1.726(4) . ? S3 C21 1.742(3) . ? S4 C23 1.727(3) . ? S4 C22 1.747(3) . ? S5 C23 1.648(3) . ? S6 C25 1.713(3) . ? S7 C24 1.711(4) . ? S8 C26 1.728(4) . ? S8 C25 1.743(3) . ? S9 C26 1.737(5) . ? S9 C24 1.741(3) . ? S10 C26 1.639(4) . ? C21 C22 1.344(5) . ? C24 C25 1.360(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 105.06(13) . . ? O1 Fe1 N1 86.93(11) . . ? O2 Fe1 N1 94.00(10) . . ? O1 Fe1 N4 94.21(11) . . ? O2 Fe1 N4 86.96(10) . . ? N1 Fe1 N4 178.28(11) . . ? O1 Fe1 N3 92.84(12) . . ? O2 Fe1 N3 155.72(10) . . ? N1 Fe1 N3 103.37(11) . . ? N4 Fe1 N3 75.30(11) . . ? O1 Fe1 N2 159.02(12) . . ? O2 Fe1 N2 89.78(12) . . ? N1 Fe1 N2 77.14(11) . . ? N4 Fe1 N2 101.44(11) . . ? N3 Fe1 N2 77.93(11) . . ? C7 N1 C8 118.1(3) . . ? C7 N1 Fe1 125.5(3) . . ? C8 N1 Fe1 116.3(2) . . ? C10 N2 C9 114.7(3) . . ? C10 N2 Fe1 111.0(2) . . ? C9 N2 Fe1 107.6(2) . . ? C10 N2 H2N 107.7 . . ? C9 N2 H2N 107.7 . . ? Fe1 N2 H2N 107.7 . . ? C12 N3 C11 114.5(3) . . ? C12 N3 Fe1 107.1(2) . . ? C11 N3 Fe1 109.2(2) . . ? C12 N3 H3N 108.7 . . ? C11 N3 H3N 108.7 . . ? Fe1 N3 H3N 108.7 . . ? C14 N4 C13 118.0(3) . . ? C14 N4 Fe1 125.8(2) . . ? C13 N4 Fe1 116.2(2) . . ? C1 O1 Fe1 134.3(2) . . ? C20 O2 Fe1 133.8(2) . . ? O1 C1 C6 122.7(3) . . ? O1 C1 C2 118.5(3) . . ? C6 C1 C2 118.8(3) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C4 C3 C2 121.6(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 118.9(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C4 C5 C6 121.4(4) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 119.4(4) . . ? C1 C6 C7 123.4(3) . . ? C5 C6 C7 117.2(4) . . ? N1 C7 C6 126.0(3) . . ? N1 C7 H7 117.0 . . ? C6 C7 H7 117.0 . . ? N1 C8 C9 109.5(3) . . ? N1 C8 H81 109.8 . . ? C9 C8 H81 109.8 . . ? N1 C8 H82 109.8 . . ? C9 C8 H82 109.8 . . ? H81 C8 H82 108.2 . . ? N2 C9 C8 108.7(3) . . ? N2 C9 H91 109.9 . . ? C8 C9 H91 109.9 . . ? N2 C9 H92 109.9 . . ? C8 C9 H92 109.9 . . ? H91 C9 H92 108.3 . . ? N2 C10 C11 108.8(3) . . ? N2 C10 H101 109.9 . . ? C11 C10 H101 109.9 . . ? N2 C10 H102 109.9 . . ? C11 C10 H102 109.9 . . ? H101 C10 H102 108.3 . . ? N3 C11 C10 108.1(3) . . ? N3 C11 H111 110.1 . . ? C10 C11 H111 110.1 . . ? N3 C11 H112 110.1 . . ? C10 C11 H112 110.1 . . ? H111 C11 H112 108.4 . . ? N3 C12 C13 110.2(3) . . ? N3 C12 H121 109.6 . . ? C13 C12 H121 109.6 . . ? N3 C12 H122 109.6 . . ? C13 C12 H122 109.6 . . ? H121 C12 H122 108.1 . . ? N4 C13 C12 109.9(3) . . ? N4 C13 H131 109.7 . . ? C12 C13 H131 109.7 . . ? N4 C13 H132 109.7 . . ? C12 C13 H132 109.7 . . ? H131 C13 H132 108.2 . . ? N4 C14 C15 126.2(3) . . ? N4 C14 H14 116.9 . . ? C15 C14 H14 116.9 . . ? C16 C15 C20 118.6(3) . . ? C16 C15 C14 118.1(3) . . ? C20 C15 C14 123.3(3) . . ? C17 C16 C15 122.0(4) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C16 C17 C18 119.3(4) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 120.3(4) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 121.8(4) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? O2 C20 C19 119.5(3) . . ? O2 C20 C15 122.6(3) . . ? C19 C20 C15 118.0(3) . . ? S6 Ni1 S7 92.98(4) . . ? S6 Ni1 S1 86.17(4) . . ? S7 Ni1 S1 176.68(4) . . ? S6 Ni1 S2 176.39(4) . . ? S7 Ni1 S2 87.20(4) . . ? S1 Ni1 S2 93.85(4) . . ? C21 S1 Ni1 101.22(11) . . ? C22 S2 Ni1 101.21(12) . . ? C23 S3 C21 98.08(16) . . ? C23 S4 C22 97.65(16) . . ? C25 S6 Ni1 102.49(13) . . ? C24 S7 Ni1 102.45(11) . . ? C26 S8 C25 97.16(18) . . ? C26 S9 C24 97.41(17) . . ? C22 C21 S1 122.3(2) . . ? C22 C21 S3 115.7(3) . . ? S1 C21 S3 122.0(2) . . ? C21 C22 S2 121.4(3) . . ? C21 C22 S4 116.2(2) . . ? S2 C22 S4 122.4(2) . . ? S5 C23 S3 123.64(19) . . ? S5 C23 S4 123.9(2) . . ? S3 C23 S4 112.40(18) . . ? C25 C24 S7 121.0(2) . . ? C25 C24 S9 115.7(3) . . ? S7 C24 S9 123.2(2) . . ? C24 C25 S6 121.0(3) . . ? C24 C25 S8 116.5(2) . . ? S6 C25 S8 122.5(2) . . ? S10 C26 S8 123.3(3) . . ? S10 C26 S9 123.5(2) . . ? S8 C26 S9 113.2(2) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.842 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.084 data_nife180 _database_code_depnum_ccdc_archive 'CCDC 246501' _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' _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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8880(10) _cell_length_b 12.2520(14) _cell_length_c 15.911(2) _cell_angle_alpha 81.612(15) _cell_angle_beta 82.187(15) _cell_angle_gamma 74.322(13) _cell_volume 1641.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.85 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.686 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7584 _exptl_absorpt_correction_T_max 1.1807 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _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 (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 180(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 5908 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1015 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.85 _reflns_number_total 5908 _reflns_number_gt 3594 _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) 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^)+(0.0474P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5908 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 0.865 _refine_ls_restrained_S_all 0.865 _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 0.10078(7) 0.19018(5) 0.66419(4) 0.02536(18) Uani 1 1 d . . . N1 N 0.2253(4) 0.0343(3) 0.6708(2) 0.0287(9) Uani 1 1 d . . . N2 N -0.0822(4) 0.1200(3) 0.6958(3) 0.0361(11) Uani 1 1 d . . . H2N H -0.1546 0.1533 0.6565 0.043 Uiso 1 1 calc R . . N3 N 0.0910(4) 0.1978(3) 0.7893(2) 0.0320(10) Uani 1 1 d . . . H3N H 0.1874 0.1563 0.8074 0.038 Uiso 1 1 calc R . . N4 N -0.0311(4) 0.3440(3) 0.6642(2) 0.0303(10) Uani 1 1 d . . . O1 O 0.2764(3) 0.2497(2) 0.64402(19) 0.0286(8) Uani 1 1 d . . . O2 O 0.0907(3) 0.1828(2) 0.54790(19) 0.0275(7) Uani 1 1 d . . . C1 C 0.4142(5) 0.1972(4) 0.6059(3) 0.0258(11) Uani 1 1 d . . . C2 C 0.5130(5) 0.2645(4) 0.5650(3) 0.0375(13) Uani 1 1 d . . . H2 H 0.4807 0.3449 0.5657 0.045 Uiso 1 1 calc R . . C3 C 0.6560(5) 0.2156(5) 0.5238(3) 0.0470(15) Uani 1 1 d . . . H3 H 0.7194 0.2633 0.4945 0.056 Uiso 1 1 calc R . . C4 C 0.7104(5) 0.0985(5) 0.5240(3) 0.0458(15) Uani 1 1 d . . . H4 H 0.8111 0.0658 0.4966 0.055 Uiso 1 1 calc R . . C5 C 0.6167(5) 0.0308(5) 0.5642(3) 0.0393(14) Uani 1 1 d . . . H5 H 0.6540 -0.0497 0.5651 0.047 Uiso 1 1 calc R . . C6 C 0.4654(5) 0.0776(4) 0.6044(3) 0.0298(11) Uani 1 1 d . . . C7 C 0.3710(5) 0.0017(4) 0.6420(3) 0.0326(12) Uani 1 1 d . . . H7 H 0.4191 -0.0779 0.6461 0.039 Uiso 1 1 calc R . . C8 C 0.1393(6) -0.0500(4) 0.7099(4) 0.0409(13) Uani 1 1 d . . . H81 H 0.1397 -0.0600 0.7727 0.049 Uiso 1 1 calc R . . H82 H 0.1883 -0.1246 0.6883 0.049 Uiso 1 1 calc R . . C9 C -0.0274(6) -0.0043(4) 0.6856(4) 0.0436(14) Uani 1 1 d . . . H91 H -0.0308 -0.0158 0.6256 0.052 Uiso 1 1 calc R . . H92 H -0.0974 -0.0460 0.7227 0.052 Uiso 1 1 calc R . . C10 C -0.1596(5) 0.1492(5) 0.7809(3) 0.0484(16) Uani 1 1 d . . . H101 H -0.2210 0.0939 0.8062 0.058 Uiso 1 1 calc R . . H102 H -0.2323 0.2264 0.7755 0.058 Uiso 1 1 calc R . . C11 C -0.0330(5) 0.1458(5) 0.8384(3) 0.0463(15) Uani 1 1 d . . . H111 H -0.0812 0.1883 0.8878 0.056 Uiso 1 1 calc R . . H112 H 0.0149 0.0658 0.8604 0.056 Uiso 1 1 calc R . . C12 C 0.0709(5) 0.3196(4) 0.8006(3) 0.0406(14) Uani 1 1 d . . . H121 H 0.1702 0.3420 0.7817 0.049 Uiso 1 1 calc R . . H122 H 0.0409 0.3315 0.8615 0.049 Uiso 1 1 calc R . . C13 C -0.0580(5) 0.3902(4) 0.7467(3) 0.0363(13) Uani 1 1 d . . . H131 H -0.1623 0.3854 0.7756 0.044 Uiso 1 1 calc R . . H132 H -0.0547 0.4712 0.7380 0.044 Uiso 1 1 calc R . . C14 C -0.0939(5) 0.4066(4) 0.5995(3) 0.0346(12) Uani 1 1 d . . . H14 H -0.1592 0.4801 0.6086 0.041 Uiso 1 1 calc R . . C15 C -0.0732(5) 0.3744(4) 0.5154(3) 0.0299(11) Uani 1 1 d . . . C16 C -0.1559(6) 0.4509(4) 0.4520(4) 0.0423(14) Uani 1 1 d . . . H16 H -0.2226 0.5214 0.4672 0.051 Uiso 1 1 calc R . . C17 C -0.1445(6) 0.4281(4) 0.3703(4) 0.0446(14) Uani 1 1 d . . . H17 H -0.2033 0.4810 0.3294 0.054 Uiso 1 1 calc R . . C18 C -0.0440(6) 0.3247(4) 0.3470(3) 0.0404(13) Uani 1 1 d . . . H18 H -0.0327 0.3081 0.2897 0.049 Uiso 1 1 calc R . . C19 C 0.0381(5) 0.2476(4) 0.4071(3) 0.0348(12) Uani 1 1 d . . . H19 H 0.1090 0.1796 0.3900 0.042 Uiso 1 1 calc R . . C20 C 0.0194(5) 0.2671(4) 0.4930(3) 0.0270(11) Uani 1 1 d . . . Ni1 Ni 0.36008(6) -0.03881(5) 0.91265(4) 0.02632(16) Uani 1 1 d . . . S1 S 0.54188(13) -0.12215(10) 0.82161(8) 0.0324(3) Uani 1 1 d . . . S2 S 0.24500(13) -0.17772(10) 0.93391(8) 0.0304(3) Uani 1 1 d . . . S3 S 0.59125(14) -0.34510(11) 0.74723(9) 0.0391(3) Uani 1 1 d . . . S4 S 0.32218(14) -0.39869(10) 0.85164(9) 0.0364(3) Uani 1 1 d . . . S5 S 0.51111(15) -0.56290(12) 0.73313(10) 0.0491(4) Uani 1 1 d . . . S6 S 0.46203(13) 0.10502(10) 0.88047(8) 0.0322(3) Uani 1 1 d . . . S7 S 0.19197(13) 0.04317(10) 1.01070(8) 0.0329(3) Uani 1 1 d . . . S8 S 0.39058(15) 0.33039(10) 0.95299(9) 0.0386(3) Uani 1 1 d . . . S9 S 0.12481(15) 0.28127(11) 1.06513(8) 0.0414(4) Uani 1 1 d . . . S10 S 0.2048(2) 0.50289(12) 1.06440(10) 0.0639(5) Uani 1 1 d . . . C21 C 0.4880(5) -0.2458(4) 0.8165(3) 0.0310(12) Uani 1 1 d . . . C22 C 0.3615(5) -0.2697(4) 0.8640(3) 0.0277(11) Uani 1 1 d . . . C23 C 0.4760(5) -0.4423(4) 0.7749(3) 0.0355(13) Uani 1 1 d . . . C24 C 0.2319(5) 0.1734(4) 1.0035(3) 0.0311(12) Uani 1 1 d . . . C25 C 0.3536(5) 0.2000(4) 0.9497(3) 0.0296(11) Uani 1 1 d . . . C26 C 0.2389(6) 0.3781(4) 1.0301(3) 0.0413(14) 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 0.0182(3) 0.0291(4) 0.0236(4) 0.0043(3) 0.0022(3) -0.0032(3) N1 0.031(2) 0.025(2) 0.030(2) 0.0061(17) -0.0080(17) -0.0072(17) N2 0.0234(18) 0.050(3) 0.031(2) 0.012(2) -0.0049(17) -0.0110(19) N3 0.0222(18) 0.039(2) 0.026(2) 0.0021(18) 0.0038(16) 0.0020(17) N4 0.0214(18) 0.036(2) 0.026(2) -0.0017(18) 0.0050(16) -0.0001(17) O1 0.0226(15) 0.0266(17) 0.0334(19) -0.0046(14) 0.0048(13) -0.0038(13) O2 0.0278(15) 0.0261(16) 0.0238(17) 0.0038(13) 0.0001(13) -0.0036(13) C1 0.017(2) 0.035(3) 0.025(3) -0.008(2) 0.0013(18) -0.007(2) C2 0.029(2) 0.042(3) 0.044(3) -0.008(2) 0.005(2) -0.017(2) C3 0.027(3) 0.082(4) 0.036(3) -0.014(3) 0.009(2) -0.024(3) C4 0.016(2) 0.086(5) 0.035(3) -0.025(3) 0.007(2) -0.009(3) C5 0.022(2) 0.054(3) 0.035(3) -0.018(3) -0.005(2) 0.009(2) C6 0.026(2) 0.038(3) 0.025(3) -0.010(2) -0.0024(19) -0.004(2) C7 0.035(3) 0.024(2) 0.034(3) -0.001(2) -0.008(2) 0.004(2) C8 0.049(3) 0.028(3) 0.045(3) 0.008(2) -0.005(3) -0.014(2) C9 0.042(3) 0.050(3) 0.045(3) 0.011(3) -0.008(2) -0.029(3) C10 0.026(2) 0.064(4) 0.044(3) 0.013(3) 0.010(2) -0.012(3) C11 0.035(3) 0.065(4) 0.027(3) 0.013(3) 0.008(2) -0.007(3) C12 0.030(2) 0.057(3) 0.026(3) -0.010(2) 0.001(2) 0.005(2) C13 0.031(2) 0.040(3) 0.028(3) -0.006(2) 0.004(2) 0.004(2) C14 0.027(2) 0.030(3) 0.039(3) -0.001(2) 0.003(2) 0.001(2) C15 0.024(2) 0.026(2) 0.037(3) 0.003(2) -0.001(2) -0.006(2) C16 0.039(3) 0.031(3) 0.051(4) 0.007(2) -0.014(3) 0.000(2) C17 0.050(3) 0.039(3) 0.045(4) 0.014(3) -0.027(3) -0.011(3) C18 0.044(3) 0.048(3) 0.034(3) 0.001(2) -0.009(2) -0.022(3) C19 0.034(3) 0.037(3) 0.034(3) 0.003(2) -0.005(2) -0.011(2) C20 0.022(2) 0.026(2) 0.031(3) 0.006(2) -0.0030(19) -0.0079(19) Ni1 0.0234(3) 0.0231(3) 0.0270(3) -0.0003(2) 0.0026(2) -0.0004(2) S1 0.0276(6) 0.0301(6) 0.0336(7) -0.0033(5) 0.0065(5) -0.0024(5) S2 0.0301(6) 0.0255(6) 0.0304(7) -0.0028(5) 0.0063(5) -0.0030(5) S3 0.0334(6) 0.0396(7) 0.0392(8) -0.0139(6) 0.0055(6) -0.0003(6) S4 0.0345(6) 0.0282(6) 0.0430(8) -0.0073(6) 0.0011(6) -0.0027(5) S5 0.0387(7) 0.0438(8) 0.0646(10) -0.0283(7) -0.0093(7) 0.0034(6) S6 0.0264(6) 0.0257(6) 0.0388(7) -0.0037(5) 0.0079(5) -0.0027(5) S7 0.0296(6) 0.0325(6) 0.0304(7) -0.0019(5) 0.0067(5) -0.0032(5) S8 0.0434(7) 0.0241(6) 0.0441(8) -0.0053(6) -0.0031(6) -0.0015(6) S9 0.0424(7) 0.0383(7) 0.0320(7) -0.0085(6) 0.0018(6) 0.0085(6) S10 0.0969(12) 0.0336(8) 0.0522(10) -0.0190(7) -0.0117(9) 0.0079(8) C21 0.031(2) 0.027(2) 0.027(3) -0.005(2) -0.002(2) 0.005(2) C22 0.026(2) 0.024(2) 0.028(3) -0.001(2) -0.001(2) 0.000(2) C23 0.027(2) 0.034(3) 0.040(3) -0.006(2) -0.008(2) 0.003(2) C24 0.032(2) 0.025(2) 0.029(3) -0.006(2) -0.005(2) 0.006(2) C25 0.025(2) 0.023(2) 0.034(3) 0.001(2) -0.002(2) 0.0034(19) C26 0.050(3) 0.030(3) 0.037(3) -0.004(2) -0.012(2) 0.007(2) _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 1.866(3) . ? Fe1 O2 1.881(3) . ? Fe1 N1 1.927(3) . ? Fe1 N4 1.931(3) . ? Fe1 N3 1.995(4) . ? Fe1 N2 2.011(4) . ? N1 C7 1.288(5) . ? N1 C8 1.465(6) . ? N2 C10 1.480(6) . ? N2 C9 1.494(6) . ? N2 H2N 0.9300 . ? N3 C12 1.488(7) . ? N3 C11 1.494(6) . ? N3 H3N 0.9300 . ? N4 C14 1.285(6) . ? N4 C13 1.469(6) . ? O1 C1 1.330(4) . ? O2 C20 1.329(5) . ? C1 C2 1.398(7) . ? C1 C6 1.415(6) . ? C2 C3 1.371(6) . ? C2 H2 0.9500 . ? C3 C4 1.385(8) . ? C3 H3 0.9500 . ? C4 C5 1.365(8) . ? C4 H4 0.9500 . ? C5 C6 1.415(6) . ? C5 H5 0.9500 . ? C6 C7 1.431(7) . ? C7 H7 0.9500 . ? C8 C9 1.517(7) . ? C8 H81 0.9900 . ? C8 H82 0.9900 . ? C9 H91 0.9900 . ? C9 H92 0.9900 . ? C10 C11 1.532(8) . ? C10 H101 0.9900 . ? C10 H102 0.9900 . ? C11 H111 0.9900 . ? C11 H112 0.9900 . ? C12 C13 1.521(6) . ? C12 H121 0.9900 . ? C12 H122 0.9900 . ? C13 H131 0.9900 . ? C13 H132 0.9900 . ? C14 C15 1.425(7) . ? C14 H14 0.9500 . ? C15 C16 1.410(6) . ? C15 C20 1.415(6) . ? C16 C17 1.353(7) . ? C16 H16 0.9500 . ? C17 C18 1.405(7) . ? C17 H17 0.9500 . ? C18 C19 1.376(6) . ? C18 H18 0.9500 . ? C19 C20 1.401(7) . ? C19 H19 0.9500 . ? Ni1 S1 2.1576(12) . ? Ni1 S6 2.1591(14) . ? Ni1 S7 2.1651(13) . ? Ni1 S2 2.1763(15) . ? S1 C21 1.724(5) . ? S2 C22 1.733(4) . ? S3 C23 1.745(6) . ? S3 C21 1.746(4) . ? S4 C23 1.729(5) . ? S4 C22 1.751(5) . ? S5 C23 1.644(5) . ? S6 C25 1.725(4) . ? S7 C24 1.710(5) . ? S8 C25 1.725(5) . ? S8 C26 1.731(5) . ? S9 C26 1.747(6) . ? S9 C24 1.749(4) . ? S10 C26 1.635(5) . ? C21 C22 1.343(6) . ? C24 C25 1.367(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 O1 Fe1 O2 94.08(14) . . ? O1 Fe1 N1 93.37(14) . . ? O2 Fe1 N1 87.90(14) . . ? O1 Fe1 N4 88.87(14) . . ? O2 Fe1 N4 94.66(14) . . ? N1 Fe1 N4 176.47(16) . . ? O1 Fe1 N3 90.78(15) . . ? O2 Fe1 N3 174.79(15) . . ? N1 Fe1 N3 93.71(15) . . ? N4 Fe1 N3 83.53(16) . . ? O1 Fe1 N2 175.06(15) . . ? O2 Fe1 N2 90.26(16) . . ? N1 Fe1 N2 84.42(16) . . ? N4 Fe1 N2 93.13(16) . . ? N3 Fe1 N2 84.97(17) . . ? C7 N1 C8 120.3(4) . . ? C7 N1 Fe1 125.2(3) . . ? C8 N1 Fe1 114.5(3) . . ? C10 N2 C9 116.1(4) . . ? C10 N2 Fe1 109.7(3) . . ? C9 N2 Fe1 108.8(3) . . ? C10 N2 H2N 107.3 . . ? C9 N2 H2N 107.3 . . ? Fe1 N2 H2N 107.3 . . ? C12 N3 C11 114.4(4) . . ? C12 N3 Fe1 106.8(3) . . ? C11 N3 Fe1 111.6(3) . . ? C12 N3 H3N 107.9 . . ? C11 N3 H3N 107.9 . . ? Fe1 N3 H3N 107.9 . . ? C14 N4 C13 119.2(4) . . ? C14 N4 Fe1 125.8(3) . . ? C13 N4 Fe1 115.0(3) . . ? C1 O1 Fe1 124.1(3) . . ? C20 O2 Fe1 126.1(3) . . ? O1 C1 C2 117.8(4) . . ? O1 C1 C6 123.6(4) . . ? C2 C1 C6 118.6(4) . . ? C3 C2 C1 120.6(5) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 121.6(5) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 118.8(4) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.6(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 118.6(5) . . ? C5 C6 C7 118.5(4) . . ? C1 C6 C7 122.9(4) . . ? N1 C7 C6 124.3(4) . . ? N1 C7 H7 117.8 . . ? C6 C7 H7 117.8 . . ? N1 C8 C9 106.6(4) . . ? N1 C8 H81 110.4 . . ? C9 C8 H81 110.4 . . ? N1 C8 H82 110.4 . . ? C9 C8 H82 110.4 . . ? H81 C8 H82 108.6 . . ? N2 C9 C8 109.3(5) . . ? N2 C9 H91 109.8 . . ? C8 C9 H91 109.8 . . ? N2 C9 H92 109.8 . . ? C8 C9 H92 109.8 . . ? H91 C9 H92 108.3 . . ? N2 C10 C11 108.7(4) . . ? N2 C10 H101 109.9 . . ? C11 C10 H101 109.9 . . ? N2 C10 H102 109.9 . . ? C11 C10 H102 109.9 . . ? H101 C10 H102 108.3 . . ? N3 C11 C10 110.1(4) . . ? N3 C11 H111 109.6 . . ? C10 C11 H111 109.6 . . ? N3 C11 H112 109.6 . . ? C10 C11 H112 109.6 . . ? H111 C11 H112 108.2 . . ? N3 C12 C13 107.1(4) . . ? N3 C12 H121 110.3 . . ? C13 C12 H121 110.3 . . ? N3 C12 H122 110.3 . . ? C13 C12 H122 110.3 . . ? H121 C12 H122 108.6 . . ? N4 C13 C12 107.6(3) . . ? N4 C13 H131 110.2 . . ? C12 C13 H131 110.2 . . ? N4 C13 H132 110.2 . . ? C12 C13 H132 110.2 . . ? H131 C13 H132 108.5 . . ? N4 C14 C15 125.2(4) . . ? N4 C14 H14 117.4 . . ? C15 C14 H14 117.4 . . ? C16 C15 C20 118.1(5) . . ? C16 C15 C14 118.4(4) . . ? C20 C15 C14 123.4(4) . . ? C17 C16 C15 122.8(5) . . ? C17 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? C16 C17 C18 118.8(5) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C19 C18 C17 120.1(5) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 121.5(4) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? O2 C20 C19 117.2(4) . . ? O2 C20 C15 124.5(4) . . ? C19 C20 C15 118.2(4) . . ? S1 Ni1 S6 85.83(5) . . ? S1 Ni1 S7 175.44(6) . . ? S6 Ni1 S7 92.77(5) . . ? S1 Ni1 S2 93.43(5) . . ? S6 Ni1 S2 174.34(6) . . ? S7 Ni1 S2 88.39(5) . . ? C21 S1 Ni1 101.95(15) . . ? C22 S2 Ni1 101.34(17) . . ? C23 S3 C21 97.3(2) . . ? C23 S4 C22 97.4(2) . . ? C25 S6 Ni1 103.00(17) . . ? C24 S7 Ni1 102.34(15) . . ? C25 S8 C26 97.0(2) . . ? C26 S9 C24 97.2(2) . . ? C22 C21 S1 121.8(3) . . ? C22 C21 S3 116.2(4) . . ? S1 C21 S3 122.0(3) . . ? C21 C22 S2 121.5(4) . . ? C21 C22 S4 116.3(3) . . ? S2 C22 S4 122.2(3) . . ? S5 C23 S4 123.7(3) . . ? S5 C23 S3 123.6(3) . . ? S4 C23 S3 112.7(3) . . ? C25 C24 S7 121.9(3) . . ? C25 C24 S9 114.7(4) . . ? S7 C24 S9 123.3(3) . . ? C24 C25 S6 119.8(4) . . ? C24 C25 S8 117.8(3) . . ? S6 C25 S8 122.4(3) . . ? S10 C26 S8 122.9(4) . . ? S10 C26 S9 123.9(3) . . ? S8 C26 S9 113.2(3) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.85 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.532 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.105