Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _journal_volume ? _journal_year ? _journal_page_first ? loop_ _publ_author_name 'Piersandro Pallavicini' 'Valeria Amendola' 'Yuri Diaz Fernandez' 'Marco Ghisalberti' ; A.M.Lanfredi ; 'Laura Linati' 'Carlo Mangano' 'Chiara Massera' _publ_contact_author_name 'Dr Piersandro Pallavicini' _publ_contact_author_address ; Dr Piersandro Pallavicini Dipartimento di Chimica Generale Universitą di Pavia via Taramelli, 12 Pavia 27100 ITALY ; _publ_contact_author_email PSP@UNIPV.IT _publ_section_title ; Bis-bidentate vs bis-tridentate imino-heterocycle ligands in the formation of dinuclear helical complexes of Fe(II) ; #-------------------------------------- #Data for compound Fe(2)2(CF3SO3)2. data_pv1 _database_code_CSD 195651 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H38 F6 Fe N6 O6 S2' _chemical_formula_weight 860.67 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.825(5) _cell_length_b 18.356(5) _cell_length_c 19.223(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 3820(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type semiempirical _exptl_absorpt_correction_T_min 0.780493 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sad.abs _exptl_special_details ; ? ; _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 'area detector' _diffrn_measurement_method 'omega/2teta scan and profile analysis' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31878 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 23.28 _reflns_number_total 5491 _reflns_number_gt 4182 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(15) _refine_ls_number_reflns 5491 _refine_ls_number_parameters 651 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 0.770 _refine_ls_restrained_S_all 0.770 _refine_ls_shift/su_max 0.240 _refine_ls_shift/su_mean 0.010 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.18371(5) 0.02183(2) 0.68269(3) 0.03635(14) Uani 1 1 d . . . N1 N 0.1156(3) 0.04203(14) 0.77953(15) 0.0387(7) Uani 1 1 d . . . N2 N 0.3230(3) 0.06764(13) 0.72278(14) 0.0365(6) Uani 1 1 d . . . N3 N 0.2909(3) 0.02129(19) 0.59731(17) 0.0403(8) Uani 1 1 d . . . H3NA H 0.250(3) 0.022(2) 0.5575(19) 0.047(11) Uiso 1 1 d . . . H3NB H 0.329(3) -0.0153(19) 0.5905(16) 0.032(11) Uiso 1 1 d . . . N4 N 0.0773(3) 0.09994(14) 0.63814(14) 0.0369(7) Uani 1 1 d . . . N5 N 0.0694(3) -0.03851(15) 0.63487(14) 0.0391(7) Uani 1 1 d . . . N6 N 0.2506(3) -0.07435(17) 0.71643(19) 0.0442(8) Uani 1 1 d . . . H6NA H 0.270(3) -0.0741(17) 0.7627(19) 0.046(11) Uiso 1 1 d . . . H6NB H 0.324(3) -0.0910(18) 0.6977(18) 0.051(11) Uiso 1 1 d . . . C1 C -0.0016(3) 0.03514(17) 0.80738(19) 0.0400(9) Uani 1 1 d . . . C2 C -0.1022(4) 0.0120(2) 0.7657(2) 0.0508(11) Uani 1 1 d . . . H2 H -0.087(3) 0.0004(18) 0.719(2) 0.057(12) Uiso 1 1 d . . . C3 C -0.2182(4) 0.0072(2) 0.7925(2) 0.0558(12) Uani 1 1 d . . . H3 H -0.287(4) -0.0080(19) 0.7623(19) 0.066(13) Uiso 1 1 d . . . C4 C -0.2424(5) 0.0252(3) 0.8617(2) 0.0656(12) Uani 1 1 d . . . H4 H -0.323(4) 0.023(2) 0.880(2) 0.069(12) Uiso 1 1 d . . . C5 C -0.1482(4) 0.0467(2) 0.9035(3) 0.0626(13) Uani 1 1 d . . . H5 H -0.159(4) 0.0610(19) 0.9494(19) 0.059(12) Uiso 1 1 d . . . C6 C -0.0260(4) 0.05303(18) 0.8782(2) 0.0437(10) Uani 1 1 d . . . C7 C 0.0710(4) 0.0762(2) 0.9208(2) 0.0487(11) Uani 1 1 d . . . H7 H 0.057(3) 0.088(2) 0.9676(19) 0.058(12) Uiso 1 1 d . . . C8 C 0.1843(5) 0.08372(19) 0.89288(19) 0.0466(10) Uani 1 1 d . . . H8 H 0.241(3) 0.1006(18) 0.9184(17) 0.037(11) Uiso 1 1 d . . . C9 C 0.2045(3) 0.06775(16) 0.82250(19) 0.0399(9) Uani 1 1 d . . . C10 C 0.3224(4) 0.07838(18) 0.7887(2) 0.0427(9) Uani 1 1 d . . . H10 H 0.393(3) 0.0914(15) 0.8113(16) 0.027(8) Uiso 1 1 d . . . C11 C 0.4325(3) 0.07549(19) 0.6779(2) 0.0409(9) Uani 1 1 d . . . H11 H 0.468(2) 0.0288(14) 0.6851(13) 0.010(6) Uiso 1 1 d . . . C12 C 0.5177(4) 0.1396(3) 0.6945(3) 0.0564(11) Uani 1 1 d . . . H12A H 0.460(3) 0.1853(17) 0.6891(17) 0.039(9) Uiso 1 1 d . . . H12B H 0.552(4) 0.135(2) 0.737(2) 0.060(13) Uiso 1 1 d . . . C13 C 0.6195(4) 0.1433(3) 0.6406(2) 0.0629(13) Uani 1 1 d . . . H13A H 0.665(4) 0.105(2) 0.648(2) 0.072(16) Uiso 1 1 d . . . H13B H 0.675(4) 0.188(2) 0.6499(19) 0.073(12) Uiso 1 1 d . . . C14 C 0.5694(5) 0.1463(3) 0.5667(2) 0.0590(12) Uani 1 1 d . . . H14A H 0.519(4) 0.193(2) 0.564(2) 0.072(14) Uiso 1 1 d . . . H14B H 0.632(3) 0.1461(19) 0.5332(18) 0.055(12) Uiso 1 1 d . . . C15 C 0.4847(4) 0.0829(2) 0.5516(2) 0.0499(11) Uani 1 1 d . . . H15A H 0.449(3) 0.0826(17) 0.5050(18) 0.042(11) Uiso 1 1 d . . . H15B H 0.537(3) 0.0389(19) 0.5569(16) 0.041(10) Uiso 1 1 d . . . C16 C 0.3826(3) 0.0807(2) 0.60455(19) 0.0393(9) Uani 1 1 d . . . H16 H 0.331(3) 0.1208(17) 0.6027(14) 0.035(9) Uiso 1 1 d . . . C17 C 0.0824(3) 0.1750(2) 0.64155(18) 0.0419(9) Uani 1 1 d . . . C18 C 0.1737(4) 0.20936(19) 0.6817(2) 0.0474(9) Uani 1 1 d . . . H18 H 0.236(3) 0.1783(16) 0.7078(15) 0.038(9) Uiso 1 1 d . . . C19 C 0.1799(5) 0.2846(2) 0.6839(2) 0.0593(10) Uani 1 1 d . . . H19 H 0.253(3) 0.3046(18) 0.7131(18) 0.055(12) Uiso 1 1 d . . . C20 C 0.0954(5) 0.3268(3) 0.6476(3) 0.0663(13) Uani 1 1 d . . . H20 H 0.099(3) 0.378(2) 0.6486(18) 0.064(13) Uiso 1 1 d . . . C21 C 0.0040(5) 0.2956(2) 0.6101(2) 0.0600(12) Uani 1 1 d . . . H21 H -0.062(3) 0.3204(15) 0.5851(15) 0.025(8) Uiso 1 1 d . . . C22 C -0.0046(4) 0.2188(2) 0.6056(2) 0.0470(10) Uani 1 1 d . . . C23 C -0.0965(4) 0.1849(3) 0.5648(2) 0.0552(12) Uani 1 1 d . . . H23 H -0.151(4) 0.209(2) 0.5397(19) 0.059(13) Uiso 1 1 d . . . C24 C -0.0994(4) 0.1108(3) 0.5609(2) 0.0508(11) Uani 1 1 d . . . H24 H -0.167(4) 0.0856(18) 0.5363(16) 0.050(11) Uiso 1 1 d . . . C25 C -0.0114(3) 0.0701(2) 0.59750(18) 0.0413(9) Uani 1 1 d . . . C26 C -0.0111(4) -0.0093(2) 0.5948(2) 0.0451(10) Uani 1 1 d . . . H26 H -0.060(3) -0.034(2) 0.5661(19) 0.055(12) Uiso 1 1 d . . . C27 C 0.0957(4) -0.11730(19) 0.6367(2) 0.0432(10) Uani 1 1 d . . . H27 H 0.158(3) -0.1270(14) 0.5987(13) 0.023(8) Uiso 1 1 d . . . C28 C -0.0120(5) -0.1686(2) 0.6233(4) 0.0675(14) Uani 1 1 d . . . H28A H -0.052(4) -0.161(2) 0.582(2) 0.057(14) Uiso 1 1 d . . . H28B H -0.070(3) -0.1640(18) 0.6587(18) 0.046(13) Uiso 1 1 d . . . C29 C 0.0324(6) -0.2474(3) 0.6304(4) 0.088(2) Uani 1 1 d . . . H29A H -0.034(4) -0.280(2) 0.620(2) 0.084(15) Uiso 1 1 d . . . H29B H 0.087(4) -0.254(2) 0.596(2) 0.050(14) Uiso 1 1 d . . . C30 C 0.0980(5) -0.2624(3) 0.6975(3) 0.0773(15) Uani 1 1 d . . . H30A H 0.129(3) -0.313(2) 0.701(2) 0.077(14) Uiso 1 1 d . . . H30B H 0.043(7) -0.252(4) 0.753(4) 0.20(3) Uiso 1 1 d . . . C31 C 0.2020(5) -0.2090(2) 0.7110(3) 0.0590(12) Uani 1 1 d . . . H31A H 0.244(4) -0.217(2) 0.752(3) 0.092(19) Uiso 1 1 d . . . H31B H 0.273(4) -0.218(2) 0.680(2) 0.074(14) Uiso 1 1 d . . . C32 C 0.1552(4) -0.13126(18) 0.70600(19) 0.0435(10) Uani 1 1 d . . . H32 H 0.097(3) -0.1261(17) 0.7394(17) 0.041(11) Uiso 1 1 d . . . S1 S 0.33265(10) -0.10224(6) 0.92300(5) 0.0551(3) Uani 1 1 d . . . S2 S 0.58570(12) -0.12490(6) 0.62165(6) 0.0678(4) Uani 1 1 d . . . C33 C 0.4680(4) -0.1214(3) 0.8701(2) 0.0638(12) Uani 1 1 d . . . C34 C 0.5918(7) -0.2222(4) 0.6153(4) 0.108(2) Uani 1 1 d . . . O1 O 0.2388(2) -0.09176(14) 0.87087(13) 0.0593(7) Uani 1 1 d . . . O2 O 0.3657(3) -0.03820(17) 0.96076(15) 0.0825(10) Uani 1 1 d . . . O3 O 0.3177(3) -0.16568(18) 0.96587(15) 0.0940(10) Uani 1 1 d . . . O4 O 0.4593(3) -0.11035(18) 0.6066(2) 0.1030(12) Uani 1 1 d . . . O5 O 0.6194(5) -0.1118(2) 0.6903(2) 0.164(2) Uani 1 1 d . . . O6 O 0.6683(4) -0.0989(2) 0.5710(2) 0.1304(16) Uani 1 1 d . . . F1 F 0.5693(2) -0.13213(19) 0.90638(14) 0.1078(11) Uani 1 1 d . . . F2 F 0.4887(2) -0.06518(16) 0.82747(16) 0.0972(9) Uani 1 1 d . . . F3 F 0.4514(3) -0.17779(16) 0.82932(17) 0.1061(10) Uani 1 1 d . . . F4 F 0.5182(4) -0.2555(2) 0.6552(4) 0.207(3) Uani 1 1 d . . . F5 F 0.7042(3) -0.24545(18) 0.6310(3) 0.184(2) Uani 1 1 d . . . F6 F 0.5665(7) -0.2435(3) 0.5542(3) 0.234(3) 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 0.0387(3) 0.0333(3) 0.0371(3) 0.0004(2) -0.0004(3) -0.0002(2) N1 0.0421(18) 0.0318(17) 0.0421(17) 0.0033(13) -0.0008(15) 0.0031(14) N2 0.0404(17) 0.0308(15) 0.0382(17) -0.0007(13) -0.0036(16) 0.0025(15) N3 0.042(2) 0.0356(19) 0.043(2) -0.0034(17) -0.0045(16) 0.0005(18) N4 0.0382(17) 0.0338(18) 0.0388(18) 0.0046(14) 0.0030(15) 0.0015(14) N5 0.0399(17) 0.0382(18) 0.0394(18) 0.0007(14) 0.0026(15) -0.0010(14) N6 0.049(2) 0.0382(19) 0.046(2) -0.0012(16) -0.0002(19) -0.0034(17) C1 0.046(2) 0.029(2) 0.045(2) 0.0036(18) 0.007(2) 0.0004(17) C2 0.051(3) 0.051(3) 0.051(3) -0.006(2) 0.006(2) 0.001(2) C3 0.043(3) 0.060(3) 0.064(3) -0.003(2) 0.004(2) -0.006(2) C4 0.060(3) 0.074(3) 0.062(3) -0.006(3) 0.024(3) 0.000(3) C5 0.072(3) 0.067(3) 0.049(3) 0.000(2) 0.020(3) 0.001(2) C6 0.059(3) 0.032(2) 0.040(2) 0.0051(17) 0.005(2) 0.0029(18) C7 0.077(3) 0.036(2) 0.033(2) -0.0020(19) 0.012(3) 0.004(2) C8 0.066(3) 0.039(2) 0.035(2) -0.0028(18) -0.009(3) 0.005(2) C9 0.053(2) 0.0266(17) 0.040(2) 0.0031(17) 0.000(2) 0.0049(17) C10 0.044(2) 0.036(2) 0.048(3) 0.0009(17) -0.012(2) -0.004(2) C11 0.040(2) 0.034(2) 0.049(2) 0.0043(19) 0.003(2) 0.0014(17) C12 0.043(3) 0.065(3) 0.061(3) -0.007(3) -0.003(3) -0.012(2) C13 0.045(3) 0.073(4) 0.071(3) -0.003(3) 0.002(2) -0.015(3) C14 0.054(3) 0.062(3) 0.060(3) 0.003(2) 0.010(3) -0.014(3) C15 0.042(3) 0.057(3) 0.051(3) 0.004(2) 0.003(2) -0.003(2) C16 0.036(2) 0.034(2) 0.048(2) -0.0004(18) 0.0019(19) -0.0003(19) C17 0.045(2) 0.042(2) 0.038(2) 0.0046(18) 0.0112(19) 0.0066(19) C18 0.050(2) 0.037(2) 0.055(2) -0.001(2) -0.004(3) 0.005(2) C19 0.068(3) 0.040(2) 0.070(3) 0.000(2) 0.008(3) -0.002(2) C20 0.083(4) 0.037(3) 0.079(4) 0.004(2) 0.007(3) 0.004(3) C21 0.065(3) 0.054(3) 0.061(3) 0.014(2) 0.012(3) 0.023(3) C22 0.044(3) 0.051(3) 0.046(3) 0.009(2) 0.014(2) 0.015(2) C23 0.042(3) 0.071(3) 0.053(3) 0.019(2) 0.001(2) 0.018(2) C24 0.037(2) 0.060(3) 0.055(3) 0.008(2) -0.003(2) 0.006(2) C25 0.035(2) 0.051(3) 0.039(2) 0.0022(19) 0.007(2) 0.004(2) C26 0.040(2) 0.051(3) 0.045(2) -0.007(2) -0.003(2) -0.007(2) C27 0.049(2) 0.033(2) 0.049(3) -0.0042(19) 0.001(2) -0.0017(19) C28 0.067(3) 0.046(3) 0.090(4) -0.006(3) -0.015(4) -0.013(2) C29 0.090(5) 0.037(3) 0.137(6) -0.021(3) 0.002(5) -0.016(3) C30 0.093(4) 0.039(3) 0.100(5) 0.002(3) -0.008(4) -0.008(3) C31 0.071(3) 0.035(2) 0.071(3) 0.001(2) 0.003(3) 0.002(2) C32 0.055(3) 0.031(2) 0.044(2) 0.0011(16) 0.008(2) -0.0037(19) S1 0.0533(7) 0.0654(7) 0.0465(6) 0.0006(5) -0.0033(6) 0.0091(6) S2 0.0811(9) 0.0635(8) 0.0587(8) 0.0070(6) 0.0043(7) 0.0215(7) C33 0.066(3) 0.067(3) 0.058(3) -0.004(3) -0.002(3) 0.004(2) C34 0.100(5) 0.093(5) 0.131(6) -0.007(4) 0.003(5) 0.037(4) O1 0.0531(16) 0.0713(19) 0.0536(17) 0.0018(14) -0.0112(14) 0.0042(14) O2 0.087(2) 0.085(2) 0.075(2) -0.0343(17) -0.0175(17) 0.0164(18) O3 0.094(2) 0.114(2) 0.073(2) 0.0516(19) 0.001(2) 0.011(2) O4 0.083(2) 0.079(2) 0.147(3) 0.022(2) 0.007(2) 0.0413(19) O5 0.261(6) 0.148(4) 0.084(3) -0.033(3) -0.045(3) -0.011(4) O6 0.107(3) 0.144(4) 0.141(3) 0.075(3) 0.047(3) 0.042(3) F1 0.0603(17) 0.179(3) 0.0839(19) -0.005(2) -0.0085(16) 0.0372(19) F2 0.0819(19) 0.115(2) 0.095(2) 0.0239(19) 0.0210(18) -0.0120(16) F3 0.116(2) 0.095(2) 0.107(2) -0.0490(19) 0.009(2) 0.0206(17) F4 0.142(4) 0.107(3) 0.374(9) 0.102(4) 0.052(5) 0.010(3) F5 0.111(3) 0.092(2) 0.350(7) 0.018(3) -0.022(4) 0.044(2) F6 0.362(9) 0.166(5) 0.173(5) -0.102(4) -0.017(5) 0.005(5) _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 N2 1.891(3) . ? Fe1 N5 1.898(3) . ? Fe1 N3 2.010(3) . ? Fe1 N6 2.015(3) . ? Fe1 N4 2.029(3) . ? Fe1 N1 2.036(3) . ? N1 C9 1.353(4) . ? N1 C1 1.382(4) . ? N2 C10 1.282(4) . ? N2 C11 1.474(4) . ? N3 C16 1.481(4) . ? N4 C25 1.353(4) . ? N4 C17 1.381(4) . ? N5 C26 1.281(5) . ? N5 C27 1.474(4) . ? N6 C32 1.482(5) . ? C1 C2 1.418(5) . ? C1 C6 1.426(5) . ? C2 C3 1.360(5) . ? C3 C4 1.394(6) . ? C4 C5 1.358(6) . ? C5 C6 1.413(5) . ? C6 C7 1.398(5) . ? C7 C8 1.346(6) . ? C8 C9 1.401(5) . ? C9 C10 1.446(5) . ? C11 C16 1.513(5) . ? C11 C12 1.529(5) . ? C12 C13 1.514(6) . ? C13 C14 1.521(6) . ? C14 C15 1.510(6) . ? C15 C16 1.503(5) . ? C17 C18 1.404(5) . ? C17 C22 1.418(5) . ? C18 C19 1.384(5) . ? C19 C20 1.386(6) . ? C20 C21 1.351(6) . ? C21 C22 1.415(6) . ? C22 C23 1.411(6) . ? C23 C24 1.361(6) . ? C24 C25 1.401(5) . ? C25 C26 1.458(5) . ? C27 C32 1.503(5) . ? C27 C28 1.520(6) . ? C28 C29 1.530(7) . ? C29 C30 1.498(8) . ? C30 C31 1.515(7) . ? C31 C32 1.517(5) . ? S1 O2 1.427(3) . ? S1 O3 1.436(3) . ? S1 O1 1.440(3) . ? S1 C33 1.818(5) . ? S2 O5 1.389(4) . ? S2 O6 1.406(4) . ? S2 O4 1.424(3) . ? S2 C34 1.792(6) . ? C33 F3 1.311(5) . ? C33 F1 1.315(5) . ? C33 F2 1.337(5) . ? C34 F4 1.264(8) . ? C34 F6 1.268(8) . ? C34 F5 1.325(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 N2 Fe1 N5 167.64(12) . . ? N2 Fe1 N3 82.80(13) . . ? N5 Fe1 N3 88.73(12) . . ? N2 Fe1 N6 88.39(12) . . ? N5 Fe1 N6 83.04(13) . . ? N3 Fe1 N6 92.93(16) . . ? N2 Fe1 N4 108.10(12) . . ? N5 Fe1 N4 80.66(12) . . ? N3 Fe1 N4 89.23(14) . . ? N6 Fe1 N4 163.51(12) . . ? N2 Fe1 N1 80.52(12) . . ? N5 Fe1 N1 108.23(12) . . ? N3 Fe1 N1 163.03(12) . . ? N6 Fe1 N1 89.74(13) . . ? N4 Fe1 N1 92.95(11) . . ? C9 N1 C1 116.6(3) . . ? C9 N1 Fe1 111.3(2) . . ? C1 N1 Fe1 132.0(2) . . ? C10 N2 C11 124.6(3) . . ? C10 N2 Fe1 117.9(3) . . ? C11 N2 Fe1 116.5(2) . . ? C16 N3 Fe1 107.8(2) . . ? C25 N4 C17 117.4(3) . . ? C25 N4 Fe1 111.1(2) . . ? C17 N4 Fe1 131.5(3) . . ? C26 N5 C27 123.8(3) . . ? C26 N5 Fe1 119.3(3) . . ? C27 N5 Fe1 115.8(2) . . ? C32 N6 Fe1 108.9(2) . . ? N1 C1 C2 120.9(3) . . ? N1 C1 C6 121.3(3) . . ? C2 C1 C6 117.8(3) . . ? C3 C2 C1 120.9(4) . . ? C2 C3 C4 121.3(5) . . ? C5 C4 C3 119.5(5) . . ? C4 C5 C6 121.5(4) . . ? C7 C6 C5 121.7(4) . . ? C7 C6 C1 119.3(4) . . ? C5 C6 C1 118.9(4) . . ? C8 C7 C6 118.8(4) . . ? C7 C8 C9 120.4(4) . . ? N1 C9 C8 123.5(4) . . ? N1 C9 C10 113.6(3) . . ? C8 C9 C10 122.9(4) . . ? N2 C10 C9 115.3(4) . . ? N2 C11 C16 105.3(3) . . ? N2 C11 C12 116.0(3) . . ? C16 C11 C12 111.2(3) . . ? C13 C12 C11 109.3(4) . . ? C12 C13 C14 112.4(4) . . ? C15 C14 C13 111.6(4) . . ? C16 C15 C14 109.7(4) . . ? N3 C16 C15 116.7(3) . . ? N3 C16 C11 106.3(3) . . ? C15 C16 C11 111.7(3) . . ? N4 C17 C18 120.2(3) . . ? N4 C17 C22 121.1(4) . . ? C18 C17 C22 118.7(4) . . ? C19 C18 C17 119.9(4) . . ? C18 C19 C20 120.7(5) . . ? C21 C20 C19 121.0(5) . . ? C20 C21 C22 120.1(4) . . ? C23 C22 C17 119.2(4) . . ? C23 C22 C21 121.3(4) . . ? C17 C22 C21 119.5(4) . . ? C24 C23 C22 119.2(4) . . ? C23 C24 C25 119.3(4) . . ? N4 C25 C24 123.8(4) . . ? N4 C25 C26 115.0(3) . . ? C24 C25 C26 121.1(4) . . ? N5 C26 C25 113.5(4) . . ? N5 C27 C32 105.7(3) . . ? N5 C27 C28 117.1(3) . . ? C32 C27 C28 111.9(4) . . ? C27 C28 C29 109.2(4) . . ? C30 C29 C28 113.6(5) . . ? C29 C30 C31 112.3(5) . . ? C32 C31 C30 110.5(4) . . ? N6 C32 C27 107.4(3) . . ? N6 C32 C31 115.0(3) . . ? C27 C32 C31 111.1(3) . . ? O2 S1 O3 113.9(2) . . ? O2 S1 O1 114.89(17) . . ? O3 S1 O1 115.3(2) . . ? O2 S1 C33 104.0(2) . . ? O3 S1 C33 104.8(2) . . ? O1 S1 C33 101.83(19) . . ? O5 S2 O6 115.6(3) . . ? O5 S2 O4 114.4(3) . . ? O6 S2 O4 114.1(2) . . ? O5 S2 C34 103.2(3) . . ? O6 S2 C34 105.5(3) . . ? O4 S2 C34 102.0(3) . . ? F3 C33 F1 108.2(4) . . ? F3 C33 F2 105.4(4) . . ? F1 C33 F2 107.5(4) . . ? F3 C33 S1 112.2(3) . . ? F1 C33 S1 113.9(3) . . ? F2 C33 S1 109.2(3) . . ? F4 C34 F6 106.1(7) . . ? F4 C34 F5 106.6(6) . . ? F6 C34 F5 108.1(6) . . ? F4 C34 S2 114.6(5) . . ? F6 C34 S2 111.3(6) . . ? F5 C34 S2 109.8(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.226 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.036