Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Ribbon Like Ferromagnetic Cyano-Bridged FeIII 2NiII Chains: A Magneto-Structural Study ; _publ_contact_author ; Catalina Ruiz-Perez Laboratorio de Rayos X y Materiales Moleculares DEPARTAMENTO DE FISICA FUNDAMENTAL II FACULTAD DE FISICA UNIVERSIDAD DE LA LAGUNA 38204 LA LAGUNA SPAIN ; _publ_contact_author_name 'Prof. Miguel Julve' _publ_contact_author_email MIGUEL.JULVE@UV.ES loop_ _publ_author_name L.M.Toma R.Lescouezec S.Uriel R.Llusar C.Ruiz-Perez J.Vaissermann F.Lloret M.Julve data_compound1 _database_code_depnum_ccdc_archive 'CCDC 623319' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum ' C40 H31 As1 Fe1 N7 ' _chemical_formula_moiety ' C14 H8 N6 Fe1 1-, C24 H20 As1 1+, C2 H3 N1' _chemical_formula_weight 740.49 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' As As 0.0499 2.0058 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.650(5) _cell_length_b 15.525(3) _cell_length_c 16.489(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.71(2) _cell_angle_gamma 90.00 _cell_volume 3552.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.8 _cell_measurement_theta_max 14.2 _exptl_crystal_description needle _exptl_crystal_colour brown-red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 1.388 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'refined from delta-F' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Enraf Nonius CAD4' _diffrn_measurement_method Omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 4.93 _diffrn_reflns_number 6970 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0773 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.98 _reflns_number_total 6970 _reflns_number_gt 3963 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius, CAD-4 EXPRESS, 1994' _computing_cell_refinement 'Enraf-Nonius, CAD-4 EXPRESS, 1994' _computing_data_reduction 'HELENA: Program for Data Reduction, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics CRYSTALMAKER _computing_publication_material 'PARST97 (Nardelli, 1997)' _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^)+(0.0710P)^2^+0.0000P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6970 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1322 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1010(3) 0.6862(2) 0.1776(2) 0.0397(9) Uani 1 1 d . . . C2 C 0.0105(3) 0.7774(2) 0.2727(2) 0.0380(9) Uani 1 1 d . . . C3 C 0.0075(3) 0.6066(3) 0.2704(2) 0.0412(9) Uani 1 1 d . . . C4 C -0.1575(3) 0.6978(2) 0.1960(2) 0.0368(9) Uani 1 1 d . . . C11 C -0.0595(3) 0.8639(2) 0.0947(2) 0.0385(9) Uani 1 1 d . . . H11 H -0.0429 0.8887 0.1489 0.046 Uiso 1 1 calc R . . C12 C -0.0797(3) 0.9168(2) 0.0244(3) 0.0465(10) Uani 1 1 d . . . H12 H -0.0774 0.9763 0.0312 0.056 Uiso 1 1 calc R . . C13 C -0.1032(3) 0.8816(3) -0.0555(3) 0.0484(10) Uani 1 1 d . . . H13 H -0.1163 0.9169 -0.1034 0.058 Uiso 1 1 calc R . . C14 C -0.1074(3) 0.7932(2) -0.0644(2) 0.0410(9) Uani 1 1 d . . . H14 H -0.1230 0.7680 -0.1183 0.049 Uiso 1 1 calc R . . C15 C -0.0879(2) 0.7429(2) 0.0082(2) 0.0307(8) Uani 1 1 d . . . C16 C -0.0952(2) 0.6482(2) 0.0074(2) 0.0313(8) Uani 1 1 d . . . C17 C -0.1227(3) 0.5996(2) -0.0664(2) 0.0392(9) Uani 1 1 d . . . H17 H -0.1348 0.6258 -0.1196 0.047 Uiso 1 1 calc R . . C18 C -0.1321(3) 0.5116(2) -0.0605(3) 0.0429(10) Uani 1 1 d . . . H18 H -0.1518 0.4776 -0.1095 0.051 Uiso 1 1 calc R . . C19 C -0.1119(3) 0.4751(2) 0.0190(3) 0.0426(9) Uani 1 1 d . . . H19 H -0.1185 0.4160 0.0243 0.051 Uiso 1 1 calc R . . C20 C -0.0817(3) 0.5259(2) 0.0909(2) 0.0358(8) Uani 1 1 d . . . H20 H -0.0664 0.5003 0.1446 0.043 Uiso 1 1 calc R . . C21 C 0.4032(3) 0.8848(3) 0.2573(2) 0.0408(9) Uani 1 1 d . . . C22 C 0.4208(3) 0.9677(3) 0.2876(3) 0.0606(12) Uani 1 1 d . . . H22 H 0.4810 0.9925 0.2965 0.073 Uiso 1 1 calc R . . C23 C 0.3488(4) 1.0139(3) 0.3046(4) 0.0756(16) Uani 1 1 d . . . H23 H 0.3607 1.0701 0.3250 0.091 Uiso 1 1 calc R . . C24 C 0.2619(4) 0.9788(4) 0.2922(4) 0.0764(16) Uani 1 1 d . . . H24 H 0.2135 1.0109 0.3031 0.092 Uiso 1 1 calc R . . C25 C 0.2442(4) 0.8959(4) 0.2635(4) 0.0726(15) Uani 1 1 d . . . H25 H 0.1839 0.8717 0.2557 0.087 Uiso 1 1 calc R . . C26 C 0.3146(3) 0.8483(3) 0.2462(3) 0.0562(12) Uani 1 1 d . . . H26 H 0.3025 0.7918 0.2271 0.067 Uiso 1 1 calc R . . C31 C 0.5788(3) 0.7685(3) 0.3404(3) 0.0443(9) Uani 1 1 d . . . C32 C 0.6065(4) 0.8192(3) 0.4124(3) 0.0681(14) Uani 1 1 d . . . H32 H 0.5903 0.8774 0.4082 0.082 Uiso 1 1 calc R . . C33 C 0.6579(4) 0.7850(5) 0.4907(3) 0.0802(17) Uani 1 1 d . . . H33 H 0.6778 0.8199 0.5390 0.096 Uiso 1 1 calc R . . C34 C 0.6793(4) 0.6995(4) 0.4966(4) 0.0770(17) Uani 1 1 d . . . H34 H 0.7133 0.6760 0.5496 0.092 Uiso 1 1 calc R . . C35 C 0.6521(4) 0.6484(4) 0.4271(4) 0.090(2) Uani 1 1 d . . . H35 H 0.6664 0.5899 0.4325 0.108 Uiso 1 1 calc R . . C36 C 0.6022(4) 0.6831(3) 0.3467(4) 0.0707(15) Uani 1 1 d . . . H36 H 0.5852 0.6484 0.2982 0.085 Uiso 1 1 calc R . . C41 C 0.5851(3) 0.8981(3) 0.1993(3) 0.0433(9) Uani 1 1 d . . . C42 C 0.5441(4) 0.9646(3) 0.1436(3) 0.0661(14) Uani 1 1 d . . . H42 H 0.4776 0.9716 0.1220 0.079 Uiso 1 1 calc R . . C43 C 0.6059(4) 1.0205(4) 0.1212(4) 0.0866(18) Uani 1 1 d . . . H43 H 0.5806 1.0652 0.0830 0.104 Uiso 1 1 calc R . . C44 C 0.7034(4) 1.0108(4) 0.1543(3) 0.0747(16) Uani 1 1 d . . . H44 H 0.7439 1.0504 0.1408 0.090 Uiso 1 1 calc R . . C45 C 0.7415(3) 0.9437(4) 0.2069(3) 0.0629(13) Uani 1 1 d . . . H45 H 0.8079 0.9363 0.2276 0.075 Uiso 1 1 calc R . . C46 C 0.6826(3) 0.8867(3) 0.2298(3) 0.0515(11) Uani 1 1 d . . . H46 H 0.7088 0.8407 0.2659 0.062 Uiso 1 1 calc R . . C51 C 0.4521(3) 0.7320(3) 0.1528(3) 0.0479(10) Uani 1 1 d . . . C52 C 0.4010(3) 0.6655(3) 0.1715(3) 0.0570(12) Uani 1 1 d . . . H52 H 0.3936 0.6621 0.2253 0.068 Uiso 1 1 calc R . . C53 C 0.3609(3) 0.6040(3) 0.1113(4) 0.0766(16) Uani 1 1 d . . . H53 H 0.3274 0.5580 0.1243 0.092 Uiso 1 1 calc R . . C54 C 0.3704(5) 0.6107(5) 0.0329(5) 0.105(3) Uani 1 1 d . . . H54 H 0.3423 0.5692 -0.0082 0.126 Uiso 1 1 calc R . . C55 C 0.4196(5) 0.6763(5) 0.0125(4) 0.114(3) Uani 1 1 d . . . H55 H 0.4248 0.6796 -0.0422 0.136 Uiso 1 1 calc R . . C56 C 0.4628(4) 0.7393(4) 0.0735(3) 0.0839(18) Uani 1 1 d . . . H56 H 0.4976 0.7844 0.0607 0.101 Uiso 1 1 calc R . . As1 As 0.50440(3) 0.82051(3) 0.23545(2) 0.03895(13) Uani 1 1 d . . . Fe1 Fe -0.02927(4) 0.69335(3) 0.18360(3) 0.02907(14) Uani 1 1 d . . . N1 N 0.1772(3) 0.6786(2) 0.1743(3) 0.0643(11) Uani 1 1 d . . . N2 N 0.0327(3) 0.8294(2) 0.3246(2) 0.0571(10) Uani 1 1 d . . . N3 N 0.0301(3) 0.5531(3) 0.3201(2) 0.0679(11) Uani 1 1 d . . . N4 N -0.2319(3) 0.6999(2) 0.2048(2) 0.0565(10) Uani 1 1 d . . . N11 N -0.0630(2) 0.77723(18) 0.08791(17) 0.0295(6) Uani 1 1 d . . . N12 N -0.0737(2) 0.61153(18) 0.08533(18) 0.0301(6) Uani 1 1 d . . . C9 C 0.1650(5) 0.8047(4) 0.9919(5) 0.113(3) Uani 1 1 d . A 1 C10 C 0.2407(4) 0.8684(4) 1.0201(3) 0.0773(16) Uani 1 1 d . A 1 N10 N 0.2994(4) 0.9173(4) 1.0433(3) 0.113(2) Uani 1 1 d . A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.043(2) 0.031(2) 0.044(2) -0.0116(16) 0.0136(18) -0.0091(17) C2 0.046(2) 0.033(2) 0.034(2) 0.0002(18) 0.0119(17) -0.0020(17) C3 0.050(2) 0.037(2) 0.034(2) -0.0008(18) 0.0098(18) 0.0030(18) C4 0.047(2) 0.037(2) 0.0289(19) -0.0005(15) 0.0165(17) -0.0029(17) C11 0.052(2) 0.0296(19) 0.035(2) -0.0025(15) 0.0153(18) -0.0021(17) C12 0.068(3) 0.029(2) 0.046(2) 0.0035(17) 0.022(2) -0.0025(19) C13 0.067(3) 0.039(2) 0.044(2) 0.0114(19) 0.024(2) 0.001(2) C14 0.051(2) 0.043(2) 0.0304(19) 0.0015(16) 0.0154(18) 0.0000(18) C15 0.0307(19) 0.0337(19) 0.0288(18) 0.0020(15) 0.0109(15) 0.0015(15) C16 0.0293(19) 0.0295(18) 0.0358(19) -0.0030(15) 0.0112(16) 0.0011(14) C17 0.041(2) 0.042(2) 0.034(2) -0.0074(16) 0.0107(17) -0.0011(17) C18 0.039(2) 0.039(2) 0.049(2) -0.0184(18) 0.0120(19) -0.0059(17) C19 0.043(2) 0.029(2) 0.055(3) -0.0081(18) 0.0149(19) -0.0069(17) C20 0.040(2) 0.0259(18) 0.044(2) -0.0005(16) 0.0166(18) -0.0019(16) C21 0.037(2) 0.042(2) 0.042(2) 0.0031(18) 0.0123(17) 0.0037(18) C22 0.058(3) 0.047(3) 0.084(3) -0.008(2) 0.034(3) -0.006(2) C23 0.083(4) 0.046(3) 0.113(5) -0.011(3) 0.053(4) 0.003(3) C24 0.077(4) 0.066(3) 0.109(5) 0.003(3) 0.062(4) 0.016(3) C25 0.043(3) 0.081(4) 0.103(4) -0.003(3) 0.037(3) -0.003(3) C26 0.046(3) 0.056(3) 0.071(3) -0.007(2) 0.024(2) -0.007(2) C31 0.039(2) 0.050(2) 0.044(2) 0.0063(19) 0.0125(18) -0.0012(19) C32 0.073(4) 0.076(4) 0.048(3) -0.001(3) 0.010(2) 0.015(3) C33 0.070(4) 0.116(5) 0.050(3) 0.005(3) 0.012(3) 0.012(4) C34 0.052(3) 0.107(5) 0.067(3) 0.040(3) 0.011(3) -0.001(3) C35 0.055(3) 0.061(3) 0.128(6) 0.035(4) -0.005(3) 0.000(3) C36 0.056(3) 0.056(3) 0.080(4) -0.001(3) -0.005(3) 0.000(2) C41 0.037(2) 0.050(2) 0.044(2) -0.0023(18) 0.0159(18) -0.0071(18) C42 0.054(3) 0.075(3) 0.067(3) 0.028(3) 0.017(2) 0.001(3) C43 0.090(4) 0.083(4) 0.088(4) 0.037(3) 0.031(4) -0.009(3) C44 0.068(4) 0.102(4) 0.058(3) 0.000(3) 0.027(3) -0.038(3) C45 0.045(3) 0.094(4) 0.051(3) -0.004(3) 0.018(2) -0.013(3) C46 0.046(3) 0.063(3) 0.047(2) -0.002(2) 0.016(2) -0.006(2) C51 0.037(2) 0.054(3) 0.053(2) -0.019(2) 0.0143(19) 0.0000(19) C52 0.048(3) 0.055(3) 0.067(3) -0.015(2) 0.017(2) -0.006(2) C53 0.046(3) 0.065(3) 0.113(5) -0.029(3) 0.018(3) -0.004(2) C54 0.071(4) 0.131(6) 0.112(6) -0.079(5) 0.028(4) -0.026(4) C55 0.102(5) 0.173(8) 0.080(4) -0.066(5) 0.049(4) -0.039(5) C56 0.078(4) 0.117(5) 0.064(3) -0.035(3) 0.033(3) -0.029(4) As1 0.0347(2) 0.0420(2) 0.0395(2) -0.00232(18) 0.01102(17) -0.00304(18) Fe1 0.0355(3) 0.0255(2) 0.0269(3) -0.0008(2) 0.0111(2) -0.0016(2) N1 0.046(2) 0.057(2) 0.096(3) -0.023(2) 0.031(2) -0.0109(19) N2 0.083(3) 0.050(2) 0.041(2) -0.0144(18) 0.0228(19) -0.008(2) N3 0.102(3) 0.053(2) 0.044(2) 0.0175(19) 0.018(2) 0.014(2) N4 0.055(2) 0.062(2) 0.062(2) 0.0004(19) 0.031(2) -0.0006(19) N11 0.0370(17) 0.0241(14) 0.0296(15) -0.0006(12) 0.0136(13) -0.0024(12) N12 0.0310(16) 0.0278(15) 0.0334(16) -0.0015(12) 0.0130(13) -0.0002(12) C9 0.087(5) 0.110(6) 0.115(5) 0.024(4) -0.006(4) -0.038(4) C10 0.063(4) 0.099(4) 0.062(3) 0.026(3) 0.009(3) -0.005(3) N10 0.106(4) 0.132(5) 0.084(4) 0.023(3) 0.006(3) -0.048(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.141(5) . ? C1 Fe1 1.946(4) . ? C2 N2 1.145(5) . ? C2 Fe1 1.911(4) . ? C3 N3 1.140(5) . ? C3 Fe1 1.912(4) . ? C4 N4 1.145(5) . ? C4 Fe1 1.955(4) . ? C11 N11 1.350(4) . ? C11 C12 1.373(5) . ? C12 C13 1.364(6) . ? C13 C14 1.380(5) . ? C14 C15 1.380(5) . ? C15 N11 1.355(4) . ? C15 C16 1.474(5) . ? C16 N12 1.347(4) . ? C16 C17 1.379(5) . ? C17 C18 1.380(5) . ? C18 C19 1.370(5) . ? C19 C20 1.374(5) . ? C20 N12 1.341(4) . ? C21 C26 1.374(6) . ? C21 C22 1.374(6) . ? C21 As1 1.915(4) . ? C22 C23 1.377(6) . ? C23 C24 1.339(7) . ? C24 C25 1.367(7) . ? C25 C26 1.372(6) . ? C31 C36 1.364(6) . ? C31 C32 1.373(6) . ? C31 As1 1.904(4) . ? C32 C33 1.376(7) . ? C33 C34 1.359(8) . ? C34 C35 1.345(8) . ? C35 C36 1.400(7) . ? C41 C46 1.365(6) . ? C41 C42 1.384(6) . ? C41 As1 1.912(4) . ? C42 C43 1.388(7) . ? C43 C44 1.363(7) . ? C44 C45 1.356(7) . ? C45 C46 1.371(6) . ? C51 C52 1.366(6) . ? C51 C56 1.371(7) . ? C51 As1 1.913(4) . ? C52 C53 1.367(6) . ? C53 C54 1.347(9) . ? C54 C55 1.351(9) . ? C55 C56 1.400(8) . ? Fe1 N11 1.982(3) . ? Fe1 N12 1.997(3) . ? C9 C10 1.447(8) . ? C10 N10 1.118(7) . ? 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 N1 C1 Fe1 177.4(4) . . ? N2 C2 Fe1 178.0(4) . . ? N3 C3 Fe1 177.7(4) . . ? N4 C4 Fe1 178.7(4) . . ? N11 C11 C12 122.3(3) . . ? C13 C12 C11 119.7(4) . . ? C12 C13 C14 119.4(4) . . ? C13 C14 C15 118.6(4) . . ? N11 C15 C14 122.4(3) . . ? N11 C15 C16 113.4(3) . . ? C14 C15 C16 124.2(3) . . ? N12 C16 C17 121.5(3) . . ? N12 C16 C15 114.8(3) . . ? C17 C16 C15 123.6(3) . . ? C16 C17 C18 119.2(4) . . ? C19 C18 C17 118.8(4) . . ? C18 C19 C20 120.0(4) . . ? N12 C20 C19 121.4(4) . . ? C26 C21 C22 119.6(4) . . ? C26 C21 As1 121.0(3) . . ? C22 C21 As1 119.4(3) . . ? C21 C22 C23 119.7(4) . . ? C24 C23 C22 120.6(5) . . ? C23 C24 C25 120.1(5) . . ? C24 C25 C26 120.5(5) . . ? C25 C26 C21 119.4(4) . . ? C36 C31 C32 119.6(4) . . ? C36 C31 As1 122.5(4) . . ? C32 C31 As1 117.8(3) . . ? C31 C32 C33 120.7(5) . . ? C34 C33 C32 119.3(6) . . ? C35 C34 C33 121.1(5) . . ? C34 C35 C36 120.1(5) . . ? C31 C36 C35 119.2(5) . . ? C46 C41 C42 121.4(4) . . ? C46 C41 As1 118.8(3) . . ? C42 C41 As1 119.8(3) . . ? C41 C42 C43 117.5(5) . . ? C44 C43 C42 120.9(5) . . ? C45 C44 C43 120.3(5) . . ? C44 C45 C46 120.4(5) . . ? C41 C46 C45 119.4(4) . . ? C52 C51 C56 121.0(4) . . ? C52 C51 As1 120.4(3) . . ? C56 C51 As1 118.5(4) . . ? C51 C52 C53 120.2(5) . . ? C54 C53 C52 119.3(6) . . ? C53 C54 C55 121.7(6) . . ? C54 C55 C56 120.1(6) . . ? C51 C56 C55 117.7(6) . . ? C31 As1 C41 108.64(18) . . ? C31 As1 C51 108.93(19) . . ? C41 As1 C51 112.15(18) . . ? C31 As1 C21 107.59(17) . . ? C41 As1 C21 108.85(18) . . ? C51 As1 C21 110.55(17) . . ? C2 Fe1 C3 87.82(16) . . ? C2 Fe1 C1 90.91(16) . . ? C3 Fe1 C1 87.25(17) . . ? C2 Fe1 C4 87.80(16) . . ? C3 Fe1 C4 89.80(16) . . ? C1 Fe1 C4 176.82(16) . . ? C2 Fe1 N11 95.76(14) . . ? C3 Fe1 N11 175.35(14) . . ? C1 Fe1 N11 89.72(14) . . ? C4 Fe1 N11 93.31(13) . . ? C2 Fe1 N12 176.45(14) . . ? C3 Fe1 N12 95.72(14) . . ? C1 Fe1 N12 89.54(13) . . ? C4 Fe1 N12 91.93(13) . . ? N11 Fe1 N12 80.72(12) . . ? C11 N11 C15 117.6(3) . . ? C11 N11 Fe1 126.6(2) . . ? C15 N11 Fe1 115.8(2) . . ? C20 N12 C16 119.1(3) . . ? C20 N12 Fe1 126.0(2) . . ? C16 N12 Fe1 114.9(2) . . ? N10 C10 C9 178.8(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.403 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.112 # Attachment 'compound-2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 623320' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 Fe2 N12 Ni O6' _chemical_formula_weight 799.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.5343(4) _cell_length_b 15.2390(9) _cell_length_c 14.7064(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.8420(10) _cell_angle_gamma 90.00 _cell_volume 1686.44(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.461 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min 0.846879 _exptl_absorpt_correction_T_max 0.970313 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10537 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3447 _reflns_number_gt 2558 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3447 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 1.0000 0.02112(13) Uani 1 2 d S . . O1 O 0.0074(3) 0.11831(16) 1.07114(17) 0.0397(5) Uani 1 1 d . . . H1B H -0.079(4) 0.151(2) 1.0647(19) 0.036(10) Uiso 1 1 d . . . H1A H 0.014(6) 0.102(3) 1.125(3) 0.080(15) Uiso 1 1 d . . . O2 O 0.0173(5) 0.0744(3) 1.2529(2) 0.0673(9) Uani 1 1 d . . . H2A H -0.011(8) 0.121(4) 1.285(4) 0.15(3) Uiso 1 1 d . . . H2B H -0.032(10) 0.047(5) 1.270(5) 0.18(4) Uiso 1 1 d . . . O3 O -0.2992(4) 0.2234(2) 1.0392(2) 0.0656(8) Uani 1 1 d . . . H3B H -0.308(6) 0.270(3) 1.056(3) 0.077(18) Uiso 1 1 d . . . H3A H -0.371(6) 0.210(3) 1.000(3) 0.095(19) Uiso 1 1 d . . . Fe1 Fe 0.47939(5) 0.07639(2) 0.77732(2) 0.02163(11) Uani 1 1 d . . . C1 C 0.3138(4) 0.05255(18) 0.87039(17) 0.0263(6) Uani 1 1 d . . . N1 N 0.2053(3) 0.04041(16) 0.91982(15) 0.0309(5) Uani 1 1 d . . . C2 C 0.6885(4) 0.05950(18) 0.85947(17) 0.0257(6) Uani 1 1 d . . . N2 N 0.8099(3) 0.04769(15) 0.90796(15) 0.0295(5) Uani 1 1 d . . . C3 C 0.2739(4) 0.09456(18) 0.69343(19) 0.0300(6) Uani 1 1 d . . . N3 N 0.1614(4) 0.1061(2) 0.64063(19) 0.0549(8) Uani 1 1 d . . . C4 C 0.4723(4) 0.1948(2) 0.82009(18) 0.0299(6) Uani 1 1 d . . . N4 N 0.4754(4) 0.26474(18) 0.84868(18) 0.0492(7) Uani 1 1 d . . . N5 N 0.6247(3) 0.09950(14) 0.67084(14) 0.0263(5) Uani 1 1 d . . . N6 N 0.5045(3) -0.04605(15) 0.73400(14) 0.0264(5) Uani 1 1 d . . . C5 C 0.6739(4) 0.1786(2) 0.6412(2) 0.0368(7) Uani 1 1 d . . . H5 H 0.6536 0.2275 0.6771 0.044 Uiso 1 1 calc R . . C6 C 0.7535(4) 0.1904(2) 0.5595(2) 0.0446(8) Uani 1 1 d . . . H6 H 0.7829 0.2463 0.5397 0.054 Uiso 1 1 calc R . . C7 C 0.7880(4) 0.1176(3) 0.5083(2) 0.0494(9) Uani 1 1 d . . . H7 H 0.8442 0.1236 0.4538 0.059 Uiso 1 1 calc R . . C8 C 0.7397(4) 0.0364(2) 0.53764(19) 0.0422(8) Uani 1 1 d . . . H8 H 0.7629 -0.0130 0.5031 0.051 Uiso 1 1 calc R . . C9 C 0.6562(4) 0.02779(18) 0.61896(18) 0.0282(6) Uani 1 1 d . . . C10 C 0.5907(4) -0.05504(19) 0.65586(18) 0.0288(6) Uani 1 1 d . . . C11 C 0.6135(4) -0.1360(2) 0.6162(2) 0.0431(8) Uani 1 1 d . . . H11 H 0.6717 -0.1409 0.5621 0.052 Uiso 1 1 calc R . . C12 C 0.5489(5) -0.2094(2) 0.6576(2) 0.0514(9) Uani 1 1 d . . . H12 H 0.5615 -0.2644 0.6314 0.062 Uiso 1 1 calc R . . C13 C 0.4664(5) -0.2008(2) 0.7374(2) 0.0486(9) Uani 1 1 d . . . H13 H 0.4251 -0.2501 0.7671 0.058 Uiso 1 1 calc R . . C14 C 0.4446(4) -0.1181(2) 0.7739(2) 0.0389(8) Uani 1 1 d . . . H14 H 0.3864 -0.1125 0.8279 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0175(2) 0.0263(3) 0.0197(2) 0.0012(2) 0.00274(19) 0.0002(2) O1 0.0416(14) 0.0366(13) 0.0412(14) -0.0082(11) 0.0048(11) 0.0029(11) O2 0.082(2) 0.067(2) 0.0529(16) -0.0180(16) -0.0020(15) 0.0022(19) O3 0.075(2) 0.065(2) 0.0563(18) -0.0083(16) -0.0037(16) 0.0130(17) Fe1 0.0201(2) 0.0246(2) 0.02029(19) 0.00186(16) 0.00247(15) 0.00127(16) C1 0.0234(15) 0.0286(16) 0.0267(14) 0.0023(12) 0.0000(12) 0.0019(12) N1 0.0241(13) 0.0422(15) 0.0270(12) 0.0046(11) 0.0069(11) -0.0023(11) C2 0.0279(15) 0.0266(16) 0.0232(13) -0.0018(11) 0.0072(12) -0.0014(12) N2 0.0258(13) 0.0363(14) 0.0262(12) 0.0012(10) -0.0014(10) 0.0042(10) C3 0.0308(16) 0.0299(17) 0.0294(15) -0.0054(12) 0.0025(13) 0.0039(12) N3 0.0495(18) 0.060(2) 0.0527(18) -0.0113(14) -0.0198(15) 0.0172(15) C4 0.0306(16) 0.0322(17) 0.0273(14) -0.0018(13) 0.0049(12) 0.0015(13) N4 0.0600(19) 0.0371(18) 0.0514(17) -0.0091(14) 0.0116(15) 0.0009(14) N5 0.0257(13) 0.0283(13) 0.0249(11) 0.0039(10) 0.0021(10) -0.0006(9) N6 0.0228(12) 0.0256(12) 0.0306(12) 0.0030(10) 0.0002(10) 0.0008(10) C5 0.0344(17) 0.0374(18) 0.0390(17) 0.0037(14) 0.0065(14) -0.0039(14) C6 0.0384(19) 0.052(2) 0.0439(18) 0.0160(17) 0.0101(15) -0.0030(15) C7 0.044(2) 0.073(3) 0.0323(17) 0.0141(18) 0.0134(15) -0.0037(18) C8 0.0434(19) 0.058(2) 0.0266(15) -0.0053(15) 0.0103(14) 0.0064(16) C9 0.0235(15) 0.0351(17) 0.0261(14) -0.0018(12) 0.0013(11) 0.0026(12) C10 0.0233(14) 0.0330(17) 0.0298(14) -0.0032(12) -0.0020(12) 0.0036(12) C11 0.048(2) 0.038(2) 0.0438(18) -0.0127(15) 0.0039(15) 0.0077(15) C12 0.056(2) 0.034(2) 0.064(2) -0.0136(17) -0.0042(19) 0.0066(16) C13 0.053(2) 0.0253(18) 0.067(2) 0.0077(16) -0.0023(18) -0.0015(15) C14 0.0373(18) 0.0303(17) 0.0498(19) 0.0093(15) 0.0077(15) -0.0004(14) _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 Ni1 N2 2.054(2) 1_455 ? Ni1 N2 2.054(2) 3_657 ? Ni1 O1 2.084(2) . ? Ni1 O1 2.084(2) 3_557 ? Ni1 N1 2.084(2) . ? Ni1 N1 2.084(2) 3_557 ? Fe1 C4 1.912(3) . ? Fe1 C1 1.931(3) . ? Fe1 C3 1.951(3) . ? Fe1 C2 1.954(3) . ? Fe1 N6 1.984(2) . ? Fe1 N5 1.986(2) . ? C1 N1 1.136(3) . ? C2 N2 1.146(3) . ? N2 Ni1 2.054(2) 1_655 ? C3 N3 1.134(4) . ? C4 N4 1.146(3) . ? N5 C5 1.340(3) . ? N5 C9 1.360(3) . ? N6 C14 1.334(3) . ? N6 C10 1.355(3) . ? C5 C6 1.380(4) . ? C6 C7 1.374(5) . ? C7 C8 1.366(5) . ? C8 C9 1.385(4) . ? C9 C10 1.469(4) . ? C10 C11 1.379(4) . ? C11 C12 1.374(5) . ? C12 C13 1.361(5) . ? C13 C14 1.382(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 N2 Ni1 N2 180.000(1) 1_455 3_657 ? N2 Ni1 O1 91.44(10) 1_455 . ? N2 Ni1 O1 88.56(10) 3_657 . ? N2 Ni1 O1 88.56(10) 1_455 3_557 ? N2 Ni1 O1 91.44(10) 3_657 3_557 ? O1 Ni1 O1 180.0 . 3_557 ? N2 Ni1 N1 92.03(9) 1_455 . ? N2 Ni1 N1 87.97(9) 3_657 . ? O1 Ni1 N1 91.51(9) . . ? O1 Ni1 N1 88.49(9) 3_557 . ? N2 Ni1 N1 87.97(9) 1_455 3_557 ? N2 Ni1 N1 92.03(9) 3_657 3_557 ? O1 Ni1 N1 88.49(9) . 3_557 ? O1 Ni1 N1 91.51(9) 3_557 3_557 ? N1 Ni1 N1 180.0 . 3_557 ? C4 Fe1 C1 85.12(11) . . ? C4 Fe1 C3 92.29(12) . . ? C1 Fe1 C3 87.40(11) . . ? C4 Fe1 C2 87.45(12) . . ? C1 Fe1 C2 93.80(11) . . ? C3 Fe1 C2 178.75(11) . . ? C4 Fe1 N6 176.12(11) . . ? C1 Fe1 N6 97.23(10) . . ? C3 Fe1 N6 90.90(10) . . ? C2 Fe1 N6 89.31(10) . . ? C4 Fe1 N5 96.75(10) . . ? C1 Fe1 N5 173.05(10) . . ? C3 Fe1 N5 85.84(10) . . ? C2 Fe1 N5 92.97(10) . . ? N6 Fe1 N5 81.29(9) . . ? N1 C1 Fe1 174.2(2) . . ? C1 N1 Ni1 171.2(2) . . ? N2 C2 Fe1 178.4(3) . . ? C2 N2 Ni1 167.1(2) . 1_655 ? N3 C3 Fe1 175.8(3) . . ? N4 C4 Fe1 176.5(3) . . ? C5 N5 C9 118.8(2) . . ? C5 N5 Fe1 126.04(19) . . ? C9 N5 Fe1 114.71(18) . . ? C14 N6 C10 118.5(2) . . ? C14 N6 Fe1 126.4(2) . . ? C10 N6 Fe1 115.14(17) . . ? N5 C5 C6 122.7(3) . . ? C7 C6 C5 118.3(3) . . ? C8 C7 C6 119.9(3) . . ? C7 C8 C9 119.8(3) . . ? N5 C9 C8 120.5(3) . . ? N5 C9 C10 114.3(2) . . ? C8 C9 C10 125.1(3) . . ? N6 C10 C11 121.6(3) . . ? N6 C10 C9 114.2(2) . . ? C11 C10 C9 124.2(3) . . ? C12 C11 C10 119.1(3) . . ? C13 C12 C11 119.4(3) . . ? C12 C13 C14 119.3(3) . . ? N6 C14 C13 122.1(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.289 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.067 # Attachment 'compound3-new.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 623321' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 Fe2 N12 Ni O6' _chemical_formula_weight 847.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.3716(6) _cell_length_b 15.6150(11) _cell_length_c 15.2953(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.457(5) _cell_angle_gamma 90.00 _cell_volume 1757.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular sheet' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.013 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 1.407 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.510 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_number 12622 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 6.42 _diffrn_reflns_theta_max 29.99 _reflns_number_total 4875 _reflns_number_gt 3372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms from water molecules haven't been included in the refinement ; _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^)+(0.0346P)^2^+2.6650P] 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 4875 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6820(4) 0.0701(2) 0.61621(19) 0.0237(7) Uani 1 1 d . . . C2 C 0.3087(4) 0.0778(2) 0.63006(19) 0.0232(7) Uani 1 1 d . . . C3 C 0.7438(4) 0.1196(2) 0.7815(2) 0.0245(7) Uani 1 1 d . . . C4 C 0.5289(4) 0.2159(2) 0.6650(2) 0.0271(7) Uani 1 1 d . . . C5 C 0.3402(4) 0.2085(2) 0.8390(2) 0.0297(7) Uani 1 1 d . . . H5 H 0.3606 0.2561 0.8043 0.036 Uiso 1 1 calc R . . C6 C 0.2621(5) 0.2203(3) 0.9193(2) 0.0377(9) Uani 1 1 d . . . H6 H 0.2343 0.2750 0.9383 0.045 Uiso 1 1 calc R . . C7 C 0.2274(5) 0.1511(3) 0.9691(2) 0.0385(9) Uani 1 1 d . . . H7 H 0.1731 0.1585 1.0220 0.046 Uiso 1 1 calc R . . C8 C 0.2725(4) 0.0688(3) 0.9418(2) 0.0300(8) Uani 1 1 d . . . C9 C 0.3557(4) 0.0624(2) 0.86221(18) 0.0232(7) Uani 1 1 d . . . C10 C 0.4154(4) -0.0178(2) 0.8321(2) 0.0242(7) Uani 1 1 d . . . C11 C 0.3876(5) -0.0923(2) 0.8799(2) 0.0332(8) Uani 1 1 d . . . C12 C 0.4479(6) -0.1690(3) 0.8450(3) 0.0432(10) Uani 1 1 d . . . H12 H 0.4337 -0.2203 0.8746 0.052 Uiso 1 1 calc R . . C13 C 0.5284(6) -0.1678(3) 0.7666(3) 0.0451(10) Uani 1 1 d . . . H13 H 0.5669 -0.2187 0.7421 0.054 Uiso 1 1 calc R . . C14 C 0.5527(5) -0.0910(2) 0.7237(2) 0.0353(8) Uani 1 1 d . . . H14 H 0.6085 -0.0915 0.6708 0.042 Uiso 1 1 calc R . . C15 C 0.2462(5) -0.0085(3) 0.9898(2) 0.0413(10) Uani 1 1 d . . . H15 H 0.1895 -0.0060 1.0425 0.050 Uiso 1 1 calc R . . C16 C 0.3012(5) -0.0839(3) 0.9606(2) 0.0424(10) Uani 1 1 d . . . H16 H 0.2827 -0.1327 0.9938 0.051 Uiso 1 1 calc R . . Fe1 Fe 0.52422(6) 0.10081(3) 0.70696(3) 0.01827(12) Uani 1 1 d . . . N1 N 0.7865(4) 0.05112(19) 0.56718(17) 0.0278(6) Uani 1 1 d . . . N2 N 0.1871(4) 0.0593(2) 0.58450(17) 0.0289(6) Uani 1 1 d . . . N3 N 0.8680(4) 0.1300(2) 0.8283(2) 0.0458(9) Uani 1 1 d . . . N4 N 0.5221(5) 0.2857(2) 0.6426(2) 0.0458(8) Uani 1 1 d . . . N5 N 0.3863(3) 0.13126(17) 0.81076(15) 0.0210(5) Uani 1 1 d . . . N6 N 0.4993(3) -0.01667(17) 0.75526(16) 0.0232(6) Uani 1 1 d . . . Ni1 Ni 0.0000 0.0000 0.5000 0.01841(14) Uani 1 2 d S . . O1W O -0.0002(3) 0.10444(16) 0.41501(15) 0.0347(6) Uani 1 1 d . . . O2W O -0.0037(4) 0.0572(2) 0.24218(18) 0.0560(8) Uani 1 1 d . . . O3W O 0.3080(5) 0.2125(2) 0.4435(2) 0.0610(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 C1 0.0192(15) 0.0305(18) 0.0212(15) -0.0035(13) -0.0012(11) -0.0025(13) C2 0.0220(16) 0.0285(17) 0.0196(15) -0.0032(12) 0.0061(12) -0.0026(13) C3 0.0229(16) 0.0287(18) 0.0217(15) 0.0003(13) 0.0005(12) -0.0016(13) C4 0.0244(16) 0.034(2) 0.0233(16) 0.0005(14) 0.0051(12) -0.0012(14) C5 0.0263(17) 0.0321(19) 0.0313(17) -0.0078(14) 0.0076(13) -0.0006(15) C6 0.0320(19) 0.044(2) 0.038(2) -0.0146(17) 0.0086(15) 0.0025(17) C7 0.0282(19) 0.063(3) 0.0251(17) -0.0109(17) 0.0067(14) 0.0006(18) C8 0.0189(16) 0.049(2) 0.0218(16) 0.0018(14) 0.0006(12) -0.0050(15) C9 0.0164(15) 0.0351(19) 0.0180(14) -0.0011(13) 0.0003(11) -0.0035(13) C10 0.0182(15) 0.0288(18) 0.0253(16) 0.0026(13) -0.0022(11) -0.0050(13) C11 0.0285(18) 0.035(2) 0.0352(19) 0.0079(16) -0.0058(14) -0.0055(16) C12 0.043(2) 0.028(2) 0.058(3) 0.0126(18) -0.0067(19) -0.0042(17) C13 0.043(2) 0.027(2) 0.065(3) -0.0060(19) -0.0016(19) 0.0030(18) C14 0.034(2) 0.031(2) 0.042(2) -0.0079(16) 0.0049(15) 0.0012(16) C15 0.034(2) 0.065(3) 0.0247(17) 0.0096(18) 0.0070(14) -0.006(2) C16 0.039(2) 0.053(3) 0.036(2) 0.0196(18) 0.0006(16) -0.0109(19) Fe1 0.0152(2) 0.0238(2) 0.0159(2) -0.00285(17) 0.00172(14) -0.00118(18) N1 0.0220(14) 0.0385(17) 0.0234(13) -0.0051(12) 0.0057(10) 0.0026(12) N2 0.0233(14) 0.0397(18) 0.0234(13) -0.0047(12) -0.0012(11) -0.0034(13) N3 0.0374(18) 0.057(2) 0.0412(18) 0.0071(16) -0.0129(14) -0.0104(17) N4 0.055(2) 0.038(2) 0.0466(19) 0.0117(16) 0.0203(16) 0.0034(17) N5 0.0181(13) 0.0259(14) 0.0193(12) -0.0026(10) 0.0032(9) -0.0012(11) N6 0.0209(13) 0.0237(15) 0.0251(13) -0.0041(10) 0.0019(10) -0.0012(11) Ni1 0.0132(3) 0.0263(3) 0.0158(3) -0.0027(2) 0.00138(18) 0.0002(2) O1W 0.0376(14) 0.0336(14) 0.0332(13) 0.0064(11) 0.0056(10) 0.0038(12) O2W 0.069(2) 0.056(2) 0.0419(16) 0.0032(14) -0.0057(14) 0.0052(17) O3W 0.069(2) 0.057(2) 0.0569(19) 0.0009(16) 0.0082(15) -0.0144(18) _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. Electron density synthesis with coefficients Fo-Fc Highest peak 0.89 at 0.0495 0.2346 0.6164 [ 0.73 A from H12 ] Deepest hole -0.57 at 0.4348 0.1094 0.6985 [ 0.68 A from FE1 ] ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.146(4) . ? C1 Fe1 1.925(3) . ? C2 N2 1.139(4) . ? C2 Fe1 1.952(3) . ? C3 N3 1.139(4) . ? C3 Fe1 1.945(3) . ? C4 N4 1.144(4) . ? C4 Fe1 1.909(4) . ? C5 N5 1.332(4) . ? C5 C6 1.399(5) . ? C6 C7 1.355(6) . ? C7 C8 1.397(5) . ? C8 C9 1.400(4) . ? C8 C15 1.432(5) . ? C9 N5 1.359(4) . ? C9 C10 1.413(5) . ? C10 N6 1.361(4) . ? C10 C11 1.396(5) . ? C11 C12 1.394(5) . ? C11 C16 1.429(5) . ? C12 C13 1.370(6) . ? C13 C14 1.383(6) . ? C14 N6 1.326(4) . ? C15 C16 1.331(6) . ? Fe1 N6 1.990(3) . ? Fe1 N5 1.994(2) . ? N1 Ni1 2.089(3) 1_655 ? N2 Ni1 2.053(3) . ? Ni1 N2 2.053(3) 3_556 ? Ni1 O1W 2.085(2) 3_556 ? Ni1 O1W 2.085(2) . ? Ni1 N1 2.089(3) 3_656 ? Ni1 N1 2.089(3) 1_455 ? 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 N1 C1 Fe1 174.7(3) . . ? N2 C2 Fe1 175.7(3) . . ? N3 C3 Fe1 177.1(3) . . ? N4 C4 Fe1 175.7(3) . . ? N5 C5 C6 122.0(3) . . ? C7 C6 C5 119.4(4) . . ? C6 C7 C8 120.5(3) . . ? C7 C8 C9 116.8(3) . . ? C7 C8 C15 125.4(3) . . ? C9 C8 C15 117.7(3) . . ? N5 C9 C8 122.9(3) . . ? N5 C9 C10 116.5(3) . . ? C8 C9 C10 120.5(3) . . ? N6 C10 C11 123.5(3) . . ? N6 C10 C9 115.9(3) . . ? C11 C10 C9 120.7(3) . . ? C12 C11 C10 117.1(3) . . ? C12 C11 C16 125.3(4) . . ? C10 C11 C16 117.6(3) . . ? C13 C12 C11 119.2(4) . . ? C12 C13 C14 120.1(4) . . ? N6 C14 C13 122.5(3) . . ? C16 C15 C8 121.3(3) . . ? C15 C16 C11 122.2(3) . . ? C4 Fe1 C1 88.17(14) . . ? C4 Fe1 C3 91.41(14) . . ? C1 Fe1 C3 86.73(13) . . ? C4 Fe1 C2 90.07(14) . . ? C1 Fe1 C2 91.42(12) . . ? C3 Fe1 C2 177.59(14) . . ? C4 Fe1 N6 175.06(12) . . ? C1 Fe1 N6 96.38(13) . . ? C3 Fe1 N6 90.76(12) . . ? C2 Fe1 N6 87.92(12) . . ? C4 Fe1 N5 93.66(12) . . ? C1 Fe1 N5 173.26(11) . . ? C3 Fe1 N5 86.74(12) . . ? C2 Fe1 N5 95.06(11) . . ? N6 Fe1 N5 82.03(11) . . ? C1 N1 Ni1 167.6(3) . 1_655 ? C2 N2 Ni1 166.8(3) . . ? C5 N5 C9 118.3(3) . . ? C5 N5 Fe1 128.8(2) . . ? C9 N5 Fe1 112.5(2) . . ? C14 N6 C10 117.6(3) . . ? C14 N6 Fe1 129.5(2) . . ? C10 N6 Fe1 112.9(2) . . ? N2 Ni1 N2 180.0 . 3_556 ? N2 Ni1 O1W 89.14(11) . 3_556 ? N2 Ni1 O1W 90.86(11) 3_556 3_556 ? N2 Ni1 O1W 90.86(11) . . ? N2 Ni1 O1W 89.14(11) 3_556 . ? O1W Ni1 O1W 180.0 3_556 . ? N2 Ni1 N1 89.11(11) . 3_656 ? N2 Ni1 N1 90.89(11) 3_556 3_656 ? O1W Ni1 N1 92.04(10) 3_556 3_656 ? O1W Ni1 N1 87.96(10) . 3_656 ? N2 Ni1 N1 90.89(11) . 1_455 ? N2 Ni1 N1 89.11(11) 3_556 1_455 ? O1W Ni1 N1 87.96(10) 3_556 1_455 ? O1W Ni1 N1 92.04(10) . 1_455 ? N1 Ni1 N1 180.00(12) 3_656 1_455 ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.885 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.100