Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_[Fe(L1)(L2)](PF6)3 _database_code_depnum_ccdc_archive 'CCDC 240419' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 F18 Fe1 N9 O2 P3' _chemical_formula_sum 'C36 H36 F18 Fe N9 O2 P3' _chemical_formula_weight 1117.50 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 9.449(5) _cell_length_b 15.793(8) _cell_length_c 17.694(9) _cell_angle_alpha 108.047(8) _cell_angle_beta 102.452(9) _cell_angle_gamma 107.097(8) _cell_volume 2259(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 26.21 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6631 _exptl_absorpt_correction_T_max 0.8547 _exptl_absorpt_process_details 'SADABS (Sheldrick 97)' _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 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23215 _diffrn_reflns_av_R_equivalents 0.1018 _diffrn_reflns_av_sigmaI/netI 0.1498 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 26.21 _reflns_number_total 8909 _reflns_number_gt 4105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1278P)^2^+2.4628P] 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 8909 _refine_ls_number_parameters 630 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1856 _refine_ls_R_factor_gt 0.0929 _refine_ls_wR_factor_ref 0.2557 _refine_ls_wR_factor_gt 0.2076 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.004 _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 0.23532(11) 0.19033(7) 0.31166(6) 0.0365(3) Uani 1 1 d . . . O1 O 0.2858(6) 0.1063(4) 0.1144(3) 0.0669(15) Uani 1 1 d . . . N3 N 0.3469(7) 0.1125(4) 0.2529(3) 0.0470(15) Uani 1 1 d . . . O2 O 0.1931(6) -0.0675(4) 0.2655(3) 0.0492(13) Uani 1 1 d . . . N1 N 0.1161(6) 0.2689(4) 0.3530(3) 0.0425(14) Uani 1 1 d . . . N2 N 0.2652(7) 0.2724(4) 0.2472(3) 0.0463(14) Uani 1 1 d . . . N4 N 0.0432(6) 0.0907(4) 0.2145(3) 0.0418(13) Uani 1 1 d . . . N5 N 0.4240(6) 0.2797(4) 0.4131(3) 0.0391(13) Uani 1 1 d . . . N6 N 0.2126(6) 0.1137(4) 0.3824(3) 0.0370(13) Uani 1 1 d . . . N7 N -0.0802(6) -0.2180(4) 0.2427(4) 0.0433(14) Uani 1 1 d . . . N8 N -0.1952(6) -0.3211(4) 0.1112(4) 0.0470(14) Uani 1 1 d . . . N9 N 0.2127(7) -0.2514(4) 0.2221(4) 0.0534(16) Uani 1 1 d . . . C1 C 0.0496(8) 0.2697(5) 0.4135(5) 0.0533(19) Uani 1 1 d . . . H1 H 0.0674 0.2345 0.4454 0.064 Uiso 1 1 calc R . . C2 C -0.0449(9) 0.3216(6) 0.4296(6) 0.067(2) Uani 1 1 d . . . H2 H -0.0895 0.3206 0.4715 0.080 Uiso 1 1 calc R . . C3 C -0.0718(10) 0.3744(6) 0.3830(6) 0.069(2) Uani 1 1 d . . . H3 H -0.1349 0.4091 0.3931 0.082 Uiso 1 1 calc R . . C4 C -0.0036(9) 0.3752(5) 0.3206(5) 0.063(2) Uani 1 1 d . . . H4 H -0.0219 0.4094 0.2878 0.076 Uiso 1 1 calc R . . C5 C 0.0911(8) 0.3245(5) 0.3085(4) 0.0457(17) Uani 1 1 d . . . C6 C 0.1815(9) 0.3232(5) 0.2511(5) 0.055(2) Uani 1 1 d . . . H6 H 0.1782 0.3587 0.2180 0.066 Uiso 1 1 calc R . . C7 C 0.3696(10) 0.2790(6) 0.1942(5) 0.066(2) Uani 1 1 d . . . H7A H 0.3140 0.2824 0.1431 0.079 Uiso 1 1 calc R . . H7B H 0.4623 0.3385 0.2251 0.079 Uiso 1 1 calc R . . C8 C 0.4207(10) 0.1964(6) 0.1704(5) 0.062(2) Uani 1 1 d . . . H8 H 0.4962 0.2094 0.1411 0.075 Uiso 1 1 calc R . . C9 C 0.4919(9) 0.1725(6) 0.2427(5) 0.060(2) Uani 1 1 d . . . H9A H 0.5556 0.1360 0.2280 0.072 Uiso 1 1 calc R . . H9B H 0.5553 0.2304 0.2936 0.072 Uiso 1 1 calc R . . C10 C 0.2402(9) 0.0500(5) 0.1614(4) 0.0522(19) Uani 1 1 d . . . H10 H 0.2572 -0.0102 0.1411 0.063 Uiso 1 1 calc R . . C11 C 0.0716(8) 0.0281(5) 0.1525(4) 0.0476(18) Uani 1 1 d . . . C12 C -0.0517(10) -0.0488(5) 0.0831(4) 0.060(2) Uani 1 1 d . . . H12 H -0.0306 -0.0913 0.0416 0.072 Uiso 1 1 calc R . . C13 C -0.2036(11) -0.0604(6) 0.0775(5) 0.073(3) Uani 1 1 d . . . H13 H -0.2865 -0.1105 0.0314 0.087 Uiso 1 1 calc R . . C14 C -0.2345(9) 0.0029(6) 0.1406(5) 0.063(2) Uani 1 1 d . . . H14 H -0.3372 -0.0051 0.1379 0.076 Uiso 1 1 calc R . . C15 C -0.1089(9) 0.0771(5) 0.2069(5) 0.0520(19) Uani 1 1 d . . . H15 H -0.1288 0.1202 0.2485 0.062 Uiso 1 1 calc R . . C16 C 0.5256(8) 0.3690(5) 0.4297(4) 0.0484(18) Uani 1 1 d . . . H16 H 0.5115 0.3938 0.3886 0.058 Uiso 1 1 calc R . . C17 C 0.6506(9) 0.4259(5) 0.5053(5) 0.060(2) Uani 1 1 d . . . H17 H 0.7180 0.4873 0.5147 0.073 Uiso 1 1 calc R . . C18 C 0.6718(10) 0.3886(6) 0.5658(5) 0.075(3) Uani 1 1 d . . . H18 H 0.7549 0.4250 0.6166 0.090 Uiso 1 1 calc R . . C19 C 0.5723(10) 0.2994(6) 0.5518(5) 0.070(2) Uani 1 1 d . . . H19 H 0.5873 0.2737 0.5922 0.084 Uiso 1 1 calc R . . C20 C 0.4455(8) 0.2460(5) 0.4748(4) 0.0435(17) Uani 1 1 d . . . C21 C 0.3267(8) 0.1524(5) 0.4543(4) 0.0466(17) Uani 1 1 d . . . H21 H 0.3317 0.1212 0.4910 0.056 Uiso 1 1 calc R . . C22 C 0.0920(7) 0.0176(4) 0.3629(4) 0.0406(16) Uani 1 1 d . . . H22A H 0.0011 0.0029 0.3158 0.049 Uiso 1 1 calc R . . H22B H 0.0584 0.0200 0.4113 0.049 Uiso 1 1 calc R . . C23 C 0.1541(8) -0.0629(5) 0.3408(4) 0.0443(17) Uani 1 1 d . . . H23 H 0.2508 -0.0445 0.3868 0.053 Uiso 1 1 calc R . . C24 C 0.0357(8) -0.1619(5) 0.3290(4) 0.0444(17) Uani 1 1 d . . . H24A H 0.0938 -0.1999 0.3424 0.053 Uiso 1 1 calc R . . H24B H -0.0202 -0.1511 0.3688 0.053 Uiso 1 1 calc R . . C25 C -0.2172(9) -0.2076(5) 0.2134(5) 0.0525(19) Uani 1 1 d . . . H25 H -0.2532 -0.1644 0.2443 0.063 Uiso 1 1 calc R . . C26 C -0.2927(8) -0.2714(5) 0.1310(5) 0.0503(18) Uani 1 1 d . . . C27 C -0.4385(9) -0.2966(6) 0.0667(5) 0.063(2) Uani 1 1 d . . . H27 H -0.5075 -0.2670 0.0784 0.075 Uiso 1 1 calc R . . C28 C -0.4737(10) -0.3651(7) -0.0121(6) 0.073(3) Uani 1 1 d . . . H28 H -0.5660 -0.3806 -0.0546 0.088 Uiso 1 1 calc R . . C29 C -0.3724(10) -0.4124(6) -0.0295(5) 0.073(2) Uani 1 1 d . . . H29 H -0.4009 -0.4597 -0.0832 0.087 Uiso 1 1 calc R . . C30 C -0.2353(10) -0.3916(6) 0.0290(5) 0.066(2) Uani 1 1 d . . . H30 H -0.1688 -0.4227 0.0158 0.079 Uiso 1 1 calc R . . C31 C -0.0649(8) -0.2877(5) 0.1798(4) 0.0409(16) Uani 1 1 d . . . C32 C 0.0650(9) -0.3222(5) 0.1863(4) 0.0483(18) Uani 1 1 d . . . C33 C 0.0369(10) -0.4191(6) 0.1587(5) 0.064(2) Uani 1 1 d . . . H33 H -0.0656 -0.4652 0.1356 0.077 Uiso 1 1 calc R . . C34 C 0.1631(12) -0.4466(6) 0.1661(5) 0.072(2) Uani 1 1 d . . . H34 H 0.1473 -0.5117 0.1475 0.086 Uiso 1 1 calc R . . C35 C 0.3136(12) -0.3759(7) 0.2016(5) 0.076(3) Uani 1 1 d . . . H35 H 0.4007 -0.3926 0.2063 0.091 Uiso 1 1 calc R . . C36 C 0.3327(9) -0.2799(6) 0.2299(5) 0.064(2) Uani 1 1 d . . . H36 H 0.4344 -0.2328 0.2558 0.077 Uiso 1 1 calc R . . H38 H 0.358(7) 0.066(4) 0.274(4) 0.039(18) Uiso 1 1 d . . . H37 H 0.220(7) -0.116(4) 0.253(4) 0.031(18) Uiso 1 1 d . . . P1 P -0.2840(3) -0.43024(16) 0.31286(15) 0.0637(7) Uani 1 1 d . . . P2 P -0.1667(3) 0.2479(2) 0.02787(18) 0.0807(8) Uani 1 1 d . . . P3 P 0.3375(2) 0.98207(17) 0.61013(13) 0.0560(6) Uani 1 1 d . . . F11 F -0.3086(8) -0.4269(5) 0.2226(4) 0.121(2) Uani 1 1 d . . . F12 F -0.2784(7) -0.5334(4) 0.2771(5) 0.137(3) Uani 1 1 d . . . F13 F -0.2614(9) -0.4367(7) 0.4006(4) 0.179(4) Uani 1 1 d . . . F14 F -0.2904(9) -0.3275(4) 0.3467(5) 0.140(3) Uani 1 1 d . . . F15 F -0.0990(6) -0.3811(5) 0.3351(5) 0.130(2) Uani 1 1 d . . . F16 F -0.4714(6) -0.4809(4) 0.2872(4) 0.0938(17) Uani 1 1 d . . . F21 F 0.0114(10) 0.3073(7) 0.0685(6) 0.198(5) Uani 1 1 d . . . F22 F -0.178(2) 0.2993(13) 0.1090(9) 0.323(9) Uani 1 1 d . . . F23 F -0.3376(10) 0.1966(10) -0.0055(13) 0.322(10) Uani 1 1 d . . . F24 F -0.129(2) 0.2079(8) -0.0541(6) 0.259(7) Uani 1 1 d . . . F25 F -0.1845(8) 0.3307(5) -0.0027(4) 0.130(2) Uani 1 1 d . . . F26 F -0.1411(10) 0.1665(6) 0.0515(6) 0.176(4) Uani 1 1 d . . . F31 F 0.4245(9) 0.9142(6) 0.6128(5) 0.142(3) Uani 1 1 d . . . F32 F 0.4429(12) 1.0418(6) 0.7073(5) 0.187(4) Uani 1 1 d . . . F33 F 0.2604(9) 1.0591(5) 0.6158(6) 0.160(3) Uani 1 1 d . . . F34 F 0.2430(13) 0.9288(7) 0.5190(4) 0.226(5) Uani 1 1 d . . . F35 F 0.4699(8) 1.0522(6) 0.5914(5) 0.139(3) Uani 1 1 d . . . F36 F 0.2085(7) 0.9210(6) 0.6346(5) 0.143(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 0.0385(5) 0.0390(5) 0.0314(5) 0.0142(4) 0.0125(4) 0.0137(4) O1 0.082(4) 0.064(3) 0.038(3) 0.018(3) 0.027(3) 0.005(3) N3 0.054(4) 0.054(4) 0.035(3) 0.018(3) 0.021(3) 0.020(3) O2 0.060(3) 0.047(3) 0.056(3) 0.023(3) 0.035(3) 0.027(3) N1 0.045(3) 0.038(3) 0.038(3) 0.011(3) 0.009(3) 0.016(3) N2 0.054(4) 0.042(3) 0.033(3) 0.015(3) 0.010(3) 0.010(3) N4 0.047(4) 0.050(3) 0.032(3) 0.018(3) 0.015(3) 0.020(3) N5 0.041(3) 0.044(3) 0.041(3) 0.022(3) 0.018(3) 0.019(3) N6 0.036(3) 0.039(3) 0.037(3) 0.010(3) 0.016(3) 0.018(3) N7 0.038(3) 0.048(3) 0.051(4) 0.025(3) 0.020(3) 0.018(3) N8 0.040(3) 0.054(4) 0.047(4) 0.019(3) 0.019(3) 0.017(3) N9 0.048(4) 0.056(4) 0.050(4) 0.017(3) 0.016(3) 0.017(3) C1 0.047(5) 0.058(5) 0.050(5) 0.021(4) 0.014(4) 0.017(4) C2 0.063(5) 0.073(6) 0.081(6) 0.028(5) 0.040(5) 0.042(5) C3 0.060(5) 0.061(5) 0.086(7) 0.023(5) 0.022(5) 0.034(5) C4 0.060(5) 0.051(5) 0.066(5) 0.020(4) 0.000(4) 0.023(4) C5 0.045(4) 0.038(4) 0.049(4) 0.016(3) 0.009(3) 0.017(3) C6 0.063(5) 0.048(4) 0.048(5) 0.027(4) 0.007(4) 0.015(4) C7 0.080(6) 0.062(5) 0.044(4) 0.028(4) 0.019(4) 0.006(5) C8 0.065(5) 0.068(6) 0.058(5) 0.031(4) 0.036(4) 0.014(5) C9 0.061(5) 0.071(5) 0.054(5) 0.025(4) 0.033(4) 0.024(4) C10 0.067(5) 0.043(4) 0.040(4) 0.012(3) 0.024(4) 0.016(4) C11 0.052(5) 0.050(4) 0.039(4) 0.022(4) 0.016(4) 0.013(4) C12 0.070(6) 0.057(5) 0.032(4) 0.008(4) 0.013(4) 0.008(4) C13 0.074(7) 0.069(6) 0.040(5) 0.020(4) 0.000(4) -0.003(5) C14 0.042(5) 0.080(6) 0.055(5) 0.027(5) 0.011(4) 0.009(4) C15 0.050(5) 0.059(5) 0.047(4) 0.025(4) 0.014(4) 0.021(4) C16 0.048(4) 0.045(4) 0.045(4) 0.013(3) 0.014(3) 0.014(4) C17 0.053(5) 0.049(5) 0.050(5) 0.007(4) 0.009(4) 0.000(4) C18 0.072(6) 0.066(6) 0.048(5) 0.015(4) -0.007(4) 0.002(5) C19 0.080(6) 0.068(6) 0.040(5) 0.020(4) 0.001(4) 0.015(5) C20 0.048(4) 0.042(4) 0.042(4) 0.017(3) 0.016(3) 0.019(3) C21 0.055(5) 0.050(4) 0.036(4) 0.018(3) 0.015(4) 0.021(4) C22 0.038(4) 0.047(4) 0.042(4) 0.020(3) 0.020(3) 0.018(3) C23 0.041(4) 0.055(4) 0.043(4) 0.021(3) 0.021(3) 0.020(4) C24 0.052(4) 0.045(4) 0.040(4) 0.018(3) 0.022(3) 0.016(3) C25 0.051(5) 0.051(4) 0.064(5) 0.027(4) 0.030(4) 0.019(4) C26 0.042(4) 0.054(5) 0.058(5) 0.026(4) 0.020(4) 0.016(4) C27 0.043(5) 0.077(6) 0.073(6) 0.034(5) 0.020(4) 0.027(4) C28 0.057(6) 0.094(7) 0.060(6) 0.037(5) 0.006(5) 0.021(5) C29 0.063(6) 0.082(6) 0.051(5) 0.012(5) 0.012(5) 0.020(5) C30 0.064(6) 0.067(5) 0.053(5) 0.012(4) 0.021(4) 0.019(4) C31 0.040(4) 0.038(4) 0.044(4) 0.013(3) 0.016(3) 0.017(3) C32 0.059(5) 0.046(4) 0.049(4) 0.024(4) 0.024(4) 0.024(4) C33 0.071(6) 0.051(5) 0.068(5) 0.021(4) 0.025(5) 0.024(4) C34 0.099(8) 0.053(5) 0.073(6) 0.023(5) 0.035(6) 0.041(6) C35 0.083(7) 0.091(7) 0.070(6) 0.032(5) 0.020(5) 0.062(6) C36 0.048(5) 0.083(6) 0.060(5) 0.022(5) 0.017(4) 0.033(5) P1 0.0603(14) 0.0598(14) 0.0666(15) 0.0368(12) 0.0126(12) 0.0118(11) P2 0.0683(18) 0.0901(19) 0.0763(18) 0.0298(15) 0.0109(14) 0.0342(15) P3 0.0534(13) 0.0795(15) 0.0524(13) 0.0336(12) 0.0283(11) 0.0337(12) F11 0.127(5) 0.156(6) 0.083(4) 0.068(4) 0.032(4) 0.037(4) F12 0.075(4) 0.088(4) 0.242(9) 0.068(5) 0.029(5) 0.038(3) F13 0.162(7) 0.229(9) 0.102(5) 0.117(6) 0.010(5) -0.013(6) F14 0.169(7) 0.071(4) 0.171(7) 0.033(4) 0.081(6) 0.032(4) F15 0.065(4) 0.135(5) 0.155(6) 0.075(5) 0.006(4) -0.003(4) F16 0.064(3) 0.084(4) 0.130(5) 0.044(3) 0.028(3) 0.026(3) F21 0.115(6) 0.212(9) 0.211(10) 0.115(8) -0.029(6) 0.017(6) F22 0.46(2) 0.44(2) 0.219(12) 0.130(14) 0.257(16) 0.29(2) F23 0.082(6) 0.260(12) 0.59(3) 0.287(16) -0.046(10) 0.003(7) F24 0.53(2) 0.221(10) 0.126(7) 0.093(7) 0.151(11) 0.236(14) F25 0.136(6) 0.128(5) 0.143(6) 0.070(5) 0.033(5) 0.066(5) F26 0.181(8) 0.191(8) 0.281(11) 0.186(8) 0.117(8) 0.113(7) F31 0.148(6) 0.167(6) 0.185(7) 0.098(6) 0.077(6) 0.115(6) F32 0.235(10) 0.152(7) 0.086(5) 0.034(5) 0.008(6) 0.005(7) F33 0.135(6) 0.139(6) 0.289(11) 0.121(7) 0.125(7) 0.089(5) F34 0.282(12) 0.209(9) 0.055(4) 0.030(5) -0.049(6) 0.019(8) F35 0.109(5) 0.192(7) 0.200(8) 0.138(6) 0.101(5) 0.074(5) F36 0.109(5) 0.179(7) 0.210(8) 0.139(6) 0.097(5) 0.052(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 1.975(6) . ? Fe1 N1 1.990(6) . ? Fe1 N5 1.991(5) . ? Fe1 N6 1.995(5) . ? Fe1 N4 2.007(5) . ? Fe1 N3 2.036(6) . ? O1 C10 1.434(8) . ? O1 C8 1.465(9) . ? N3 C9 1.502(9) . ? N3 C10 1.527(8) . ? O2 C23 1.444(8) . ? N1 C1 1.352(9) . ? N1 C5 1.385(8) . ? N2 C6 1.280(9) . ? N2 C7 1.503(10) . ? N4 C15 1.359(9) . ? N4 C11 1.365(9) . ? N5 C16 1.350(8) . ? N5 C20 1.358(8) . ? N6 C21 1.301(8) . ? N6 C22 1.486(8) . ? N7 C25 1.363(8) . ? N7 C31 1.370(8) . ? N7 C24 1.478(8) . ? N8 C31 1.359(8) . ? N8 C26 1.408(9) . ? N8 C30 1.416(9) . ? N9 C36 1.334(9) . ? N9 C32 1.364(9) . ? C1 C2 1.395(10) . ? C2 C3 1.378(11) . ? C3 C4 1.395(12) . ? C4 C5 1.373(10) . ? C5 C6 1.460(11) . ? C7 C8 1.492(11) . ? C8 C9 1.520(11) . ? C10 C11 1.489(10) . ? C11 C12 1.402(9) . ? C12 C13 1.370(12) . ? C13 C14 1.398(12) . ? C14 C15 1.374(10) . ? C16 C17 1.394(9) . ? C17 C18 1.378(11) . ? C18 C19 1.354(11) . ? C19 C20 1.412(10) . ? C20 C21 1.446(10) . ? C22 C23 1.530(9) . ? C23 C24 1.553(9) . ? C25 C26 1.368(10) . ? C26 C27 1.439(10) . ? C27 C28 1.371(12) . ? C28 C29 1.405(12) . ? C29 C30 1.348(11) . ? C31 C32 1.479(9) . ? C32 C33 1.375(10) . ? C33 C34 1.380(11) . ? C34 C35 1.382(12) . ? C35 C36 1.382(11) . ? P1 F13 1.560(6) . ? P1 F14 1.571(7) . ? P1 F12 1.576(6) . ? P1 F11 1.583(6) . ? P1 F15 1.591(6) . ? P1 F16 1.605(5) . ? P2 F22 1.460(10) . ? P2 F23 1.462(9) . ? P2 F26 1.535(7) . ? P2 F21 1.537(8) . ? P2 F24 1.554(10) . ? P2 F25 1.601(7) . ? P3 F34 1.484(6) . ? P3 F31 1.536(6) . ? P3 F36 1.549(6) . ? P3 F35 1.579(6) . ? P3 F33 1.581(7) . ? P3 F32 1.594(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 N1 81.2(3) . . ? N2 Fe1 N5 95.9(2) . . ? N1 Fe1 N5 89.7(2) . . ? N2 Fe1 N6 176.9(2) . . ? N1 Fe1 N6 97.8(2) . . ? N5 Fe1 N6 81.2(2) . . ? N2 Fe1 N4 89.7(2) . . ? N1 Fe1 N4 92.0(2) . . ? N5 Fe1 N4 174.4(2) . . ? N6 Fe1 N4 93.2(2) . . ? N2 Fe1 N3 91.5(3) . . ? N1 Fe1 N3 171.4(2) . . ? N5 Fe1 N3 95.5(2) . . ? N6 Fe1 N3 89.8(2) . . ? N4 Fe1 N3 83.5(2) . . ? C10 O1 C8 109.7(5) . . ? C9 N3 C10 102.3(5) . . ? C9 N3 Fe1 114.2(5) . . ? C10 N3 Fe1 108.5(4) . . ? C1 N1 C5 117.4(6) . . ? C1 N1 Fe1 128.8(5) . . ? C5 N1 Fe1 113.7(5) . . ? C6 N2 C7 118.4(6) . . ? C6 N2 Fe1 114.0(5) . . ? C7 N2 Fe1 127.6(5) . . ? C15 N4 C11 118.1(6) . . ? C15 N4 Fe1 126.8(5) . . ? C11 N4 Fe1 115.0(5) . . ? C16 N5 C20 117.2(6) . . ? C16 N5 Fe1 129.1(5) . . ? C20 N5 Fe1 113.6(4) . . ? C21 N6 C22 116.2(6) . . ? C21 N6 Fe1 113.8(5) . . ? C22 N6 Fe1 129.8(4) . . ? C25 N7 C31 109.8(6) . . ? C25 N7 C24 125.4(6) . . ? C31 N7 C24 124.8(6) . . ? C31 N8 C26 109.6(6) . . ? C31 N8 C30 129.2(6) . . ? C26 N8 C30 121.2(6) . . ? C36 N9 C32 116.9(7) . . ? N1 C1 C2 122.1(7) . . ? C3 C2 C1 119.5(8) . . ? C2 C3 C4 119.4(8) . . ? C5 C4 C3 118.7(8) . . ? C4 C5 N1 122.8(7) . . ? C4 C5 C6 126.3(7) . . ? N1 C5 C6 111.0(6) . . ? N2 C6 C5 118.9(6) . . ? C8 C7 N2 114.2(6) . . ? O1 C8 C7 110.7(7) . . ? O1 C8 C9 103.1(6) . . ? C7 C8 C9 115.7(7) . . ? N3 C9 C8 101.3(6) . . ? O1 C10 C11 109.7(6) . . ? O1 C10 N3 105.4(5) . . ? C11 C10 N3 111.3(6) . . ? N4 C11 C12 121.4(7) . . ? N4 C11 C10 115.7(6) . . ? C12 C11 C10 122.8(7) . . ? C13 C12 C11 118.9(8) . . ? C12 C13 C14 120.3(8) . . ? C15 C14 C13 118.2(8) . . ? N4 C15 C14 123.1(7) . . ? N5 C16 C17 123.2(7) . . ? C18 C17 C16 118.2(7) . . ? C19 C18 C17 120.4(8) . . ? C18 C19 C20 118.9(8) . . ? N5 C20 C19 122.0(6) . . ? N5 C20 C21 113.9(6) . . ? C19 C20 C21 124.1(7) . . ? N6 C21 C20 117.3(6) . . ? N6 C22 C23 112.2(5) . . ? O2 C23 C22 107.0(5) . . ? O2 C23 C24 111.7(5) . . ? C22 C23 C24 113.0(6) . . ? N7 C24 C23 113.5(5) . . ? N7 C25 C26 108.5(7) . . ? C25 C26 N8 105.8(6) . . ? C25 C26 C27 135.6(8) . . ? N8 C26 C27 118.5(7) . . ? C28 C27 C26 118.7(8) . . ? C27 C28 C29 121.0(8) . . ? C30 C29 C28 122.3(8) . . ? C29 C30 N8 118.3(8) . . ? N8 C31 N7 106.4(6) . . ? N8 C31 C32 126.8(6) . . ? N7 C31 C32 126.8(6) . . ? N9 C32 C33 123.1(7) . . ? N9 C32 C31 115.2(6) . . ? C33 C32 C31 121.7(7) . . ? C32 C33 C34 118.9(8) . . ? C35 C34 C33 118.8(8) . . ? C34 C35 C36 119.0(8) . . ? N9 C36 C35 123.3(8) . . ? F13 P1 F14 92.9(5) . . ? F13 P1 F12 88.3(5) . . ? F14 P1 F12 178.8(5) . . ? F13 P1 F11 178.4(5) . . ? F14 P1 F11 88.6(4) . . ? F12 P1 F11 90.2(4) . . ? F13 P1 F15 91.3(4) . . ? F14 P1 F15 89.8(4) . . ? F12 P1 F15 90.2(4) . . ? F11 P1 F15 89.3(4) . . ? F13 P1 F16 90.4(4) . . ? F14 P1 F16 90.8(4) . . ? F12 P1 F16 89.1(3) . . ? F11 P1 F16 89.0(3) . . ? F15 P1 F16 178.1(4) . . ? F22 P2 F23 89.3(10) . . ? F22 P2 F26 94.3(7) . . ? F23 P2 F26 92.7(5) . . ? F22 P2 F21 86.5(9) . . ? F23 P2 F21 175.7(10) . . ? F26 P2 F21 88.8(5) . . ? F22 P2 F24 170.6(10) . . ? F23 P2 F24 99.1(10) . . ? F26 P2 F24 89.6(5) . . ? F21 P2 F24 85.0(7) . . ? F22 P2 F25 90.5(7) . . ? F23 P2 F25 89.8(5) . . ? F26 P2 F25 174.6(5) . . ? F21 P2 F25 89.0(4) . . ? F24 P2 F25 85.4(5) . . ? F34 P3 F31 95.4(6) . . ? F34 P3 F36 91.6(6) . . ? F31 P3 F36 90.1(4) . . ? F34 P3 F35 91.8(5) . . ? F31 P3 F35 93.0(4) . . ? F36 P3 F35 175.1(5) . . ? F34 P3 F33 89.9(6) . . ? F31 P3 F33 174.5(5) . . ? F36 P3 F33 91.2(4) . . ? F35 P3 F33 85.3(4) . . ? F34 P3 F32 178.1(6) . . ? F31 P3 F32 84.9(5) . . ? F36 P3 F32 90.3(5) . . ? F35 P3 F32 86.3(5) . . ? F33 P3 F32 89.8(5) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.21 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.946 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.108