# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1860 data_fab25 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C43 H48 F18 Fe N11 P3' _chemical_formula_weightical 1209.68 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 15.005(5) _cell_length_b 12.600(5) _cell_length_c 27.920(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 98.300(5) _cell_angle_gamma 90.000(5) _cell_volume 5223(3) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method ? _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6578 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.2562 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 22.21 _reflns_number_total 6424 _reflns_number_observed 1657 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0915P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00039(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6424 _refine_ls_number_parameters 700 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2266 _refine_ls_R_factor_obs 0.0569 _refine_ls_wR_factor_all 0.1588 _refine_ls_wR_factor_obs 0.1320 _refine_ls_goodness_of_fit_all 0.632 _refine_ls_goodness_of_fit_obs 1.273 _refine_ls_restrained_S_all 0.632 _refine_ls_restrained_S_obs 1.273 _refine_ls_shift/esd_max 0.568 _refine_ls_shift/esd_mean 0.036 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.78398(7) 0.26699(8) 0.57004(4) 0.0663(5) Uani 1 d . . N1 N 0.6962(5) 0.2176(5) 0.6101(3) 0.068(2) Uani 1 d . . N2 N 0.6961(5) 0.2092(5) 0.5187(3) 0.063(2) Uani 1 d . . N3 N 0.7288(5) 0.4098(5) 0.5621(3) 0.0609(19) Uani 1 d . . N4 N 0.8578(5) 0.3387(7) 0.6244(3) 0.067(2) Uani 1 d . . N5 N 0.8534(5) 0.1347(5) 0.5777(3) 0.067(2) Uani 1 d . . N6 N 0.8707(4) 0.3005(6) 0.5274(2) 0.065(2) Uani 1 d . . N7 N 0.6108(5) 0.3059(6) 0.3685(3) 0.098(3) Uani 1 d . . H7 H 0.5869 0.3544 0.3898 0.093(6) Uiso 1 calc R . N8 N 0.6236(6) 0.5851(6) 0.4351(4) 0.108(3) Uani 1 d . . H8A H 0.6553 0.5205 0.4307 0.149(10) Uiso 1 calc R . H8B H 0.6675 0.6402 0.4426 0.149(10) Uiso 1 calc R . N9 N 0.8447(5) 0.4706(6) 0.3935(3) 0.085(2) Uani 1 d . . H9 H 0.8094 0.4068 0.3915 0.093(6) Uiso 1 calc R . N10 N 0.6658(6) 0.5139(6) 0.3435(3) 0.094(2) Uani 1 d . . C1 C 0.7019(6) 0.2236(6) 0.6591(5) 0.078(3) Uani 1 d . . H1 H 0.7528 0.2593 0.6769 0.093(6) Uiso 1 calc R . C2 C 0.6398(9) 0.1819(8) 0.6840(4) 0.089(3) Uani 1 d . . H2 H 0.6493 0.1828 0.7187 0.093(6) Uiso 1 calc R . C3 C 0.5643(10) 0.1391(9) 0.6597(6) 0.115(5) Uani 1 d . . H3 H 0.5168 0.1154 0.6768 0.093(6) Uiso 1 calc R . C4 C 0.5560(7) 0.1298(7) 0.6101(6) 0.094(4) Uani 1 d . . H4 H 0.5058 0.0928 0.5924 0.093(6) Uiso 1 calc R . C5 C 0.6202(7) 0.1737(7) 0.5866(5) 0.070(3) Uani 1 d . . C6 C 0.6205(8) 0.1709(7) 0.5329(5) 0.073(3) Uani 1 d . . C7 C 0.5452(7) 0.1420(6) 0.5020(5) 0.084(3) Uani 1 d . . H7A H 0.4913 0.1182 0.5135 0.093(6) Uiso 1 calc R . C8 C 0.5516(7) 0.1493(7) 0.4524(5) 0.087(3) Uani 1 d . . H8 H 0.5007 0.1289 0.4293 0.093(6) Uiso 1 calc R . C9 C 0.6283(8) 0.1846(6) 0.4360(5) 0.074(3) Uani 1 d . . C10 C 0.6987(7) 0.2094(6) 0.4710(5) 0.071(3) Uani 1 d . . H10 H 0.7546 0.2286 0.4604 0.093(6) Uiso 1 calc R . C11 C 0.6667(6) 0.4412(7) 0.5266(4) 0.068(3) Uani 1 d . . H11 H 0.6384 0.3887 0.5045 0.093(6) Uiso 1 calc R . C12 C 0.6400(7) 0.5473(8) 0.5193(4) 0.075(3) Uani 1 d . . C13 C 0.6732(8) 0.6181(8) 0.5522(4) 0.089(3) Uani 1 d . . H13 H 0.6531 0.6904 0.5494 0.093(6) Uiso 1 calc R . C14 C 0.7368(8) 0.5878(8) 0.5902(4) 0.090(3) Uani 1 d . . H14 H 0.7615 0.6394 0.6137 0.093(6) Uiso 1 calc R . C15 C 0.7652(7) 0.4835(9) 0.5949(4) 0.073(3) Uani 1 d . . C16 C 0.8367(7) 0.4436(8) 0.6306(4) 0.073(3) Uani 1 d . . C17 C 0.8779(8) 0.5012(8) 0.6705(5) 0.092(3) Uani 1 d . . H17 H 0.8596 0.5729 0.6754 0.093(6) Uiso 1 calc R . C18 C 0.9434(9) 0.4559(12) 0.7022(4) 0.109(4) Uani 1 d . . H18 H 0.9730 0.4953 0.7293 0.093(6) Uiso 1 calc R . C19 C 0.9670(6) 0.3524(11) 0.6947(4) 0.089(3) Uani 1 d . . H19 H 1.0130 0.3186 0.7171 0.093(6) Uiso 1 calc R . C20 C 0.9251(7) 0.2973(8) 0.6556(4) 0.080(3) Uani 1 d . . H20 H 0.9447 0.2263 0.6502 0.093(6) Uiso 1 calc R . C21 C 0.8371(6) 0.0470(9) 0.6032(4) 0.089(3) Uani 1 d . . H21 H 0.7818 0.0444 0.6167 0.093(6) Uiso 1 calc R . C22 C 0.8927(8) -0.0363(8) 0.6109(4) 0.094(3) Uani 1 d . . H22 H 0.8783 -0.0962 0.6295 0.093(6) Uiso 1 calc R . C23 C 0.9676(9) -0.0329(8) 0.5919(4) 0.104(4) Uani 1 d . . H23 H 1.0093 -0.0907 0.5980 0.093(6) Uiso 1 calc R . C24 C 0.9890(6) 0.0505(10) 0.5635(4) 0.088(3) Uani 1 d . . H24 H 1.0436 0.0504 0.5493 0.093(6) Uiso 1 calc R . C25 C 0.9287(7) 0.1345(9) 0.5563(4) 0.073(3) Uani 1 d . . C27 C 1.0023(6) 0.2378(9) 0.4958(4) 0.084(3) Uani 1 d . . H27 H 1.0491 0.1857 0.4961 0.093(6) Uiso 1 calc R . C28 C 0.9990(7) 0.3250(10) 0.4657(4) 0.092(3) Uani 1 d . . H28 H 1.0446 0.3343 0.4452 0.093(6) Uiso 1 calc R . C26 C 0.9362(7) 0.2273(9) 0.5256(4) 0.078(3) Uani 1 d . . C29 C 0.9308(7) 0.3992(8) 0.4648(4) 0.067(2) Uani 1 d . . C30 C 0.8707(6) 0.3858(7) 0.4966(3) 0.067(2) Uani 1 d . . H30 H 0.8255 0.4394 0.4976 0.093(6) Uiso 1 calc R . C31 C 0.6391(6) 0.1987(7) 0.3822(4) 0.095(3) Uani 1 d . . H31A H 0.7007 0.1881 0.3779 0.149(10) Uiso 1 calc R . H31B H 0.6025 0.1481 0.3626 0.149(10) Uiso 1 calc R . C32 C 0.6222(7) 0.3322(9) 0.3193(4) 0.105(3) Uani 1 d . . H32A H 0.5832 0.2890 0.2970 0.149(10) Uiso 1 calc R . H32B H 0.6832 0.3187 0.3144 0.149(10) Uiso 1 calc R . C33 C 0.6002(7) 0.4473(9) 0.3102(4) 0.108(3) Uani 1 d . . H33A H 0.5398 0.4614 0.3161 0.149(10) Uiso 1 calc R . H33B H 0.6042 0.4648 0.2771 0.149(10) Uiso 1 calc R . C34 C 0.5754(6) 0.5723(7) 0.4747(4) 0.091(3) Uani 1 d . . H34A H 0.5325 0.5158 0.4681 0.149(10) Uiso 1 calc R . H34B H 0.5431 0.6364 0.4795 0.149(10) Uiso 1 calc R . C35 C 0.5666(8) 0.6118(8) 0.3897(4) 0.132(4) Uani 1 d . . H35A H 0.5364 0.6779 0.3931 0.149(10) Uiso 1 calc R . H35B H 0.5217 0.5578 0.3819 0.149(10) Uiso 1 calc R . C36 C 0.6241(7) 0.6204(8) 0.3496(4) 0.116(4) Uani 1 d . . H36A H 0.5877 0.6414 0.3200 0.149(10) Uiso 1 calc R . H36B H 0.6702 0.6728 0.3578 0.149(10) Uiso 1 calc R . C37 C 0.9190(6) 0.4914(7) 0.4304(4) 0.085(3) Uani 1 d . . H37A H 0.9080 0.5551 0.4475 0.149(10) Uiso 1 calc R . H37B H 0.9728 0.5014 0.4160 0.149(10) Uiso 1 calc R . C38 C 0.8292(8) 0.5573(8) 0.3598(4) 0.108(3) Uani 1 d . . H38A H 0.8817 0.5685 0.3444 0.149(10) Uiso 1 calc R . H38B H 0.8178 0.6212 0.3766 0.149(10) Uiso 1 calc R . C39 C 0.7482(8) 0.5316(7) 0.3215(4) 0.102(3) Uani 1 d . . H39A H 0.7384 0.5892 0.2988 0.149(10) Uiso 1 calc R . H39B H 0.7611 0.4692 0.3040 0.149(10) Uiso 1 calc R . P1 P 0.9205(2) 0.2470(2) 0.29582(13) 0.0958(9) Uani 1 d . . F11 F 0.9358(5) 0.1267(4) 0.2932(3) 0.186(3) Uani 1 d . . F21 F 0.9695(6) 0.2683(6) 0.2544(3) 0.217(4) Uani 1 d . . F31 F 0.8314(5) 0.2311(6) 0.2633(3) 0.211(4) Uani 1 d . . F41 F 0.8673(5) 0.2309(6) 0.3392(3) 0.187(3) Uani 1 d . . F51 F 0.9018(5) 0.3692(5) 0.2994(3) 0.179(3) Uani 1 d . . F61 F 1.0045(5) 0.2609(6) 0.3312(3) 0.195(3) Uani 1 d . . P2 P 1.3491(2) 0.1869(3) 0.31834(15) 0.1067(10) Uani 1 d . . F12 F 1.4396(4) 0.1244(5) 0.3199(2) 0.158(3) Uani 1 d . . F22 F 1.3942(4) 0.2625(6) 0.3566(3) 0.206(4) Uani 1 d . . F32 F 1.2610(4) 0.2486(7) 0.3176(3) 0.233(5) Uani 1 d . . F42 F 1.3102(5) 0.1313(10) 0.2728(4) 0.272(6) Uani 1 d . . F52 F 1.3873(7) 0.2618(8) 0.2829(4) 0.251(4) Uani 1 d . . F62 F 1.3185(7) 0.1108(9) 0.3504(5) 0.342(8) Uani 1 d . . P3 P 1.2650(2) 0.1166(2) 0.53525(13) 0.0993(10) Uani 1 d . . F13 F 1.3114(4) 0.0457(5) 0.4978(3) 0.177(3) Uani 1 d . . F23 F 1.2219(6) 0.1829(5) 0.5711(3) 0.203(3) Uani 1 d . . F33 F 1.3431(5) 0.1934(5) 0.5296(3) 0.206(4) Uani 1 d . . F43 F 1.3256(5) 0.0563(7) 0.5749(3) 0.202(4) Uani 1 d . . F53 F 1.2086(5) 0.1766(8) 0.4939(3) 0.244(5) Uani 1 d . . F63 F 1.1951(5) 0.0369(6) 0.5345(4) 0.259(5) Uani 1 d . . C1G C 0.6801(13) 0.3901(13) 0.1874(5) 0.142(5) Uani 1 d . . C2G C 0.7516(11) 0.4646(10) 0.1825(5) 0.169(6) Uani 1 d . . H2G1 H 0.7363 0.5329 0.1941 0.32(4) Uiso 1 calc R . H2G2 H 0.7591 0.4701 0.1490 0.32(4) Uiso 1 calc R . H2G3 H 0.8067 0.4402 0.2010 0.32(4) Uiso 1 calc R . N1G N 0.6250(11) 0.3330(12) 0.1922(6) 0.219(7) Uani 1 d . . C1S C 0.1305(14) 0.0145(18) 0.2111(12) 0.183(13) Uani 1 d . . C2S C 0.1298(10) -0.0083(15) 0.2636(6) 0.202(8) Uani 1 d . . H2S1 H 0.1881 0.0069 0.2814 0.32(4) Uiso 1 calc R . H2S2 H 0.1155 -0.0817 0.2677 0.32(4) Uiso 1 calc R . H2S3 H 0.0854 0.0354 0.2755 0.32(4) Uiso 1 calc R . N1S N 0.1322(14) 0.0505(14) 0.1796(8) 0.165(7) Uani 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 0.0732(8) 0.0603(8) 0.0686(10) 0.0001(8) 0.0209(7) 0.0045(7) N1 0.085(6) 0.066(5) 0.062(6) 0.026(5) 0.046(5) 0.021(5) N2 0.047(5) 0.048(4) 0.095(8) -0.001(5) 0.015(5) -0.002(4) N3 0.071(5) 0.050(5) 0.066(6) 0.004(5) 0.024(4) 0.003(4) N4 0.060(5) 0.079(6) 0.062(6) -0.001(5) 0.006(5) -0.013(4) N5 0.073(5) 0.055(5) 0.073(6) 0.003(4) 0.009(5) 0.011(4) N6 0.074(5) 0.065(5) 0.060(6) -0.004(4) 0.020(4) -0.002(4) N7 0.132(7) 0.069(6) 0.097(8) -0.013(5) 0.029(6) 0.017(5) N8 0.121(7) 0.089(6) 0.114(9) 0.018(6) 0.017(7) 0.045(5) N9 0.085(5) 0.083(6) 0.087(7) 0.019(5) 0.014(5) -0.020(5) N10 0.101(6) 0.080(6) 0.105(8) -0.019(5) 0.025(6) 0.027(5) C1 0.077(7) 0.063(6) 0.106(10) 0.000(7) 0.049(7) -0.013(5) C2 0.101(8) 0.102(8) 0.071(9) 0.023(7) 0.035(8) 0.016(7) C3 0.108(11) 0.093(9) 0.161(16) 0.027(10) 0.073(12) 0.031(8) C4 0.078(8) 0.047(6) 0.163(13) -0.009(8) 0.044(10) 0.003(5) C5 0.044(7) 0.048(5) 0.126(12) 0.004(7) 0.042(8) 0.000(5) C6 0.053(7) 0.055(6) 0.109(11) -0.010(6) 0.003(9) 0.005(5) C7 0.072(9) 0.059(6) 0.122(11) -0.002(7) 0.021(9) 0.010(5) C8 0.056(8) 0.067(7) 0.134(13) -0.012(7) 0.000(8) 0.009(5) C9 0.070(7) 0.046(5) 0.104(11) -0.020(6) 0.006(9) -0.001(5) C10 0.090(8) 0.063(6) 0.061(8) 0.003(6) 0.012(7) -0.002(5) C11 0.076(6) 0.061(7) 0.068(8) 0.005(6) 0.021(6) 0.006(5) C12 0.104(8) 0.056(7) 0.070(9) -0.010(7) 0.030(7) 0.021(6) C13 0.133(9) 0.073(7) 0.062(8) 0.005(8) 0.021(7) 0.034(7) C14 0.155(10) 0.051(7) 0.073(9) -0.001(6) 0.045(8) 0.012(6) C15 0.080(7) 0.068(8) 0.072(9) -0.006(7) 0.019(6) -0.003(7) C16 0.090(8) 0.057(7) 0.074(9) -0.019(7) 0.023(7) -0.022(7) C17 0.118(9) 0.089(8) 0.072(9) -0.022(8) 0.021(7) -0.025(8) C18 0.154(12) 0.116(11) 0.056(9) -0.031(8) 0.008(8) -0.034(9) C19 0.090(7) 0.128(10) 0.046(8) 0.008(7) 0.003(7) -0.019(8) C20 0.076(7) 0.119(8) 0.046(7) 0.001(7) 0.013(6) -0.002(7) C21 0.097(8) 0.062(7) 0.111(10) 0.014(6) 0.024(7) 0.018(7) C22 0.097(8) 0.078(8) 0.113(10) 0.025(6) 0.036(7) 0.020(7) C23 0.128(11) 0.072(8) 0.108(10) 0.019(7) 0.004(8) 0.028(8) C24 0.082(7) 0.094(8) 0.089(9) -0.007(7) 0.022(6) 0.018(7) C25 0.073(8) 0.080(8) 0.064(8) -0.005(6) 0.003(6) 0.002(7) C27 0.075(7) 0.109(9) 0.073(7) -0.007(7) 0.028(6) 0.021(7) C28 0.078(8) 0.100(8) 0.102(10) -0.024(8) 0.026(7) -0.025(7) C26 0.068(7) 0.084(8) 0.087(8) -0.032(7) 0.022(6) -0.007(7) C29 0.069(7) 0.069(7) 0.064(8) 0.002(6) 0.017(6) -0.009(6) C30 0.078(7) 0.080(7) 0.043(7) -0.009(6) 0.009(6) -0.021(5) C31 0.120(8) 0.078(8) 0.087(10) -0.028(6) 0.013(7) 0.017(6) C32 0.116(9) 0.108(9) 0.091(10) 0.005(8) 0.019(7) -0.002(7) C33 0.100(8) 0.123(10) 0.103(10) 0.014(8) 0.025(7) 0.019(8) C34 0.098(8) 0.101(8) 0.083(9) 0.020(7) 0.044(8) 0.019(6) C35 0.174(11) 0.140(10) 0.077(9) 0.013(8) -0.002(9) 0.100(9) C36 0.176(10) 0.113(9) 0.062(8) -0.004(7) 0.031(8) 0.059(8) C37 0.093(7) 0.083(7) 0.081(8) 0.016(7) 0.021(7) -0.024(6) C38 0.146(10) 0.095(8) 0.088(10) 0.021(8) 0.027(8) -0.002(7) C39 0.138(10) 0.094(8) 0.077(9) 0.015(6) 0.026(9) 0.015(7) P1 0.099(2) 0.088(3) 0.104(3) -0.012(2) 0.025(2) 0.0029(18) F11 0.251(8) 0.068(4) 0.250(9) -0.022(4) 0.074(7) 0.020(4) F21 0.324(10) 0.203(7) 0.168(7) -0.003(6) 0.183(8) -0.010(7) F31 0.157(6) 0.237(9) 0.211(8) -0.017(7) -0.062(6) -0.026(6) F41 0.234(7) 0.194(7) 0.156(6) -0.027(6) 0.109(6) -0.032(6) F51 0.233(7) 0.094(5) 0.219(8) -0.014(5) 0.061(6) 0.034(5) F61 0.158(6) 0.219(8) 0.184(7) 0.022(6) -0.058(6) -0.028(6) P2 0.104(3) 0.110(2) 0.105(3) -0.015(3) 0.013(2) -0.002(2) F12 0.115(5) 0.158(5) 0.196(7) -0.031(5) 0.001(4) 0.040(4) F22 0.140(6) 0.225(8) 0.250(10) -0.143(8) 0.022(6) -0.001(6) F32 0.120(5) 0.338(11) 0.226(8) -0.149(8) -0.024(5) 0.103(6) F42 0.152(7) 0.427(15) 0.236(10) -0.238(12) 0.023(7) -0.033(8) F52 0.332(12) 0.209(9) 0.236(11) 0.053(9) 0.118(10) 0.069(9) F62 0.300(12) 0.311(12) 0.47(2) 0.254(14) 0.252(13) 0.067(10) P3 0.086(2) 0.087(2) 0.125(3) 0.006(2) 0.016(2) 0.005(2) F13 0.172(6) 0.178(7) 0.192(8) -0.015(5) 0.062(6) 0.069(5) F23 0.300(9) 0.145(6) 0.168(7) -0.054(5) 0.047(7) 0.089(6) F33 0.153(6) 0.114(5) 0.360(12) -0.011(6) 0.064(7) -0.024(5) F43 0.223(8) 0.272(9) 0.111(6) 0.048(6) 0.021(6) 0.105(7) F53 0.181(7) 0.355(12) 0.198(9) 0.111(8) 0.037(6) 0.142(8) F63 0.156(6) 0.177(7) 0.479(16) -0.115(9) 0.162(9) -0.080(6) C1G 0.213(18) 0.126(14) 0.089(11) -0.020(10) 0.025(11) -0.026(11) C2G 0.255(17) 0.122(11) 0.153(14) -0.023(9) 0.103(12) -0.017(12) N1G 0.287(18) 0.211(15) 0.170(13) -0.037(11) 0.062(12) -0.115(12) C1S 0.121(13) 0.101(16) 0.35(5) 0.00(2) 0.12(2) -0.029(11) C2S 0.178(14) 0.27(2) 0.158(17) -0.044(16) 0.033(13) -0.047(13) N1S 0.166(12) 0.096(12) 0.24(2) 0.004(10) 0.063(12) -0.021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N6 1.933(7) . ? Fe1 N1 1.950(7) . ? Fe1 N2 1.944(7) . ? Fe1 N5 1.961(6) . ? Fe1 N4 1.964(7) . ? Fe1 N3 1.980(7) . ? N1 C5 1.349(10) . ? N1 C1 1.360(10) . ? N2 C6 1.344(10) . ? N2 C10 1.338(9) . ? N3 C11 1.318(9) . ? N3 C15 1.363(10) . ? N4 C20 1.340(9) . ? N4 C16 1.376(9) . ? N5 C25 1.354(10) . ? N5 C21 1.355(10) . ? N6 C26 1.353(10) . ? N6 C30 1.376(9) . ? N7 C31 1.450(10) . ? N7 C32 1.446(10) . ? N7 H7 0.9600 . ? N8 C34 1.416(10) . ? N8 C35 1.461(11) . ? N8 H8A 0.9600 . ? N8 H8B 0.9600 . ? N9 C37 1.428(9) . ? N9 C38 1.439(10) . ? N9 H9 0.9600 . ? N10 C39 1.476(10) . ? N10 C36 1.502(10) . ? N10 C33 1.507(11) . ? C1 C2 1.346(11) . ? C1 H1 0.9600 . ? C2 C3 1.346(13) . ? C2 H2 0.9600 . ? C3 C4 1.379(13) . ? C3 H3 0.9600 . ? C4 C5 1.358(12) . ? C4 H4 0.9600 . ? C5 C6 1.500(12) . ? C6 C7 1.370(11) . ? C7 C8 1.403(11) . ? C7 H7A 0.9600 . ? C8 C9 1.374(11) . ? C8 H8 0.9600 . ? C9 C10 1.368(11) . ? C9 C31 1.542(12) . ? C10 H10 0.9600 . ? C11 C12 1.402(10) . ? C11 H11 0.9600 . ? C12 C13 1.324(11) . ? C12 C34 1.498(11) . ? C13 C14 1.375(11) . ? C13 H13 0.9600 . ? C14 C15 1.381(11) . ? C14 H14 0.9600 . ? C15 C16 1.445(11) . ? C16 C17 1.396(11) . ? C17 C18 1.351(12) . ? C17 H17 0.9600 . ? C18 C19 1.376(12) . ? C18 H18 0.9600 . ? C19 C20 1.369(11) . ? C19 H19 0.9600 . ? C20 H20 0.9600 . ? C21 C22 1.338(10) . ? C21 H21 0.9600 . ? C22 C23 1.310(11) . ? C22 H22 0.9600 . ? C23 C24 1.382(11) . ? C23 H23 0.9600 . ? C24 C25 1.388(11) . ? C24 H24 0.9600 . ? C25 C26 1.463(11) . ? C27 C26 1.392(11) . ? C27 C28 1.379(11) . ? C27 H27 0.9600 . ? C28 C29 1.384(11) . ? C28 H28 0.9600 . ? C29 C30 1.365(10) . ? C29 C37 1.502(11) . ? C30 H30 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C32 C33 1.501(11) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C35 C36 1.512(12) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C38 C39 1.533(11) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? P1 F21 1.481(6) . ? P1 F61 1.495(6) . ? P1 F31 1.518(7) . ? P1 F11 1.536(6) . ? P1 F41 1.557(7) . ? P1 F51 1.571(6) . ? P2 F62 1.431(8) . ? P2 F42 1.495(8) . ? P2 F22 1.516(7) . ? P2 F52 1.538(10) . ? P2 F32 1.530(6) . ? P2 F12 1.565(6) . ? P3 F63 1.451(7) . ? P3 F23 1.518(7) . ? P3 F53 1.530(7) . ? P3 F33 1.545(7) . ? P3 F43 1.529(7) . ? P3 F13 1.607(7) . ? C1G N1G 1.119(16) . ? C1G C2G 1.447(16) . ? C2G H2G1 0.9600 . ? C2G H2G2 0.9600 . ? C2G H2G3 0.9600 . ? C1S N1S 0.99(3) . ? C1S C2S 1.50(3) . ? C2S H2S1 0.9599 . ? C2S H2S2 0.9599 . ? C2S H2S3 0.9599 . ? 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 N6 Fe1 N1 173.7(3) . . ? N6 Fe1 N2 94.2(3) . . ? N1 Fe1 N2 82.0(4) . . ? N6 Fe1 N5 81.9(4) . . ? N1 Fe1 N5 93.3(3) . . ? N2 Fe1 N5 93.2(3) . . ? N6 Fe1 N4 91.2(3) . . ? N1 Fe1 N4 93.2(4) . . ? N2 Fe1 N4 171.4(3) . . ? N5 Fe1 N4 94.3(3) . . ? N6 Fe1 N3 92.3(3) . . ? N1 Fe1 N3 92.8(2) . . ? N2 Fe1 N3 91.7(3) . . ? N5 Fe1 N3 172.7(3) . . ? N4 Fe1 N3 81.3(4) . . ? C5 N1 C1 116.0(9) . . ? C5 N1 Fe1 116.4(7) . . ? C1 N1 Fe1 127.6(8) . . ? C6 N2 C10 116.2(9) . . ? C6 N2 Fe1 115.3(8) . . ? C10 N2 Fe1 128.3(8) . . ? C11 N3 C15 118.2(8) . . ? C11 N3 Fe1 126.6(7) . . ? C15 N3 Fe1 115.0(7) . . ? C20 N4 C16 117.2(9) . . ? C20 N4 Fe1 127.7(8) . . ? C16 N4 Fe1 115.1(7) . . ? C25 N5 C21 117.1(8) . . ? C25 N5 Fe1 114.6(7) . . ? C21 N5 Fe1 128.2(7) . . ? C26 N6 C30 116.4(8) . . ? C26 N6 Fe1 115.5(7) . . ? C30 N6 Fe1 128.0(7) . . ? C31 N7 C32 113.3(9) . . ? C31 N7 H7 123.3(6) . . ? C32 N7 H7 123.3(5) . . ? C34 N8 C35 113.7(9) . . ? C34 N8 H8A 108.8(5) . . ? C35 N8 H8A 108.8(5) . . ? C34 N8 H8B 108.8(6) . . ? C35 N8 H8B 108.8(6) . . ? H8A N8 H8B 107.7 . . ? C37 N9 C38 111.6(8) . . ? C37 N9 H9 124.2(5) . . ? C38 N9 H9 124.2(6) . . ? C39 N10 C36 107.5(8) . . ? C39 N10 C33 109.8(8) . . ? C36 N10 C33 108.7(8) . . ? N1 C1 C2 123.3(9) . . ? N1 C1 H1 118.4(6) . . ? C2 C1 H1 118.4(8) . . ? C3 C2 C1 119.5(12) . . ? C3 C2 H2 120.3(9) . . ? C1 C2 H2 120.3(7) . . ? C2 C3 C4 119.1(13) . . ? C2 C3 H3 120.5(9) . . ? C4 C3 H3 120.4(9) . . ? C3 C4 C5 118.9(13) . . ? C3 C4 H4 120.5(9) . . ? C5 C4 H4 120.6(8) . . ? N1 C5 C4 122.7(12) . . ? N1 C5 C6 111.8(10) . . ? C4 C5 C6 125.3(13) . . ? N2 C6 C7 124.3(11) . . ? N2 C6 C5 114.3(10) . . ? C7 C6 C5 121.0(12) . . ? C6 C7 C8 115.9(11) . . ? C6 C7 H7A 122.0(8) . . ? C8 C7 H7A 122.0(7) . . ? C9 C8 C7 122.0(11) . . ? C9 C8 H8 119.0(8) . . ? C7 C8 H8 119.0(7) . . ? C10 C9 C8 115.7(11) . . ? C10 C9 C31 119.3(10) . . ? C8 C9 C31 125.0(12) . . ? N2 C10 C9 125.5(10) . . ? N2 C10 H10 117.3(6) . . ? C9 C10 H10 117.3(7) . . ? N3 C11 C12 123.5(9) . . ? N3 C11 H11 118.3(5) . . ? C12 C11 H11 118.3(7) . . ? C13 C12 C11 118.1(10) . . ? C13 C12 C34 124.6(10) . . ? C11 C12 C34 117.3(10) . . ? C12 C13 C14 119.8(10) . . ? C12 C13 H13 120.1(7) . . ? C14 C13 H13 120.0(6) . . ? C13 C14 C15 120.5(10) . . ? C13 C14 H14 119.8(6) . . ? C15 C14 H14 119.7(7) . . ? N3 C15 C14 119.7(10) . . ? N3 C15 C16 114.4(10) . . ? C14 C15 C16 125.8(11) . . ? N4 C16 C17 121.1(10) . . ? N4 C16 C15 114.1(10) . . ? C17 C16 C15 124.6(11) . . ? C18 C17 C16 120.0(11) . . ? C18 C17 H17 120.0(8) . . ? C16 C17 H17 120.0(7) . . ? C19 C18 C17 118.7(11) . . ? C19 C18 H18 120.6(8) . . ? C17 C18 H18 120.6(8) . . ? C18 C19 C20 120.2(11) . . ? C18 C19 H19 119.9(8) . . ? C20 C19 H19 119.9(7) . . ? N4 C20 C19 122.6(10) . . ? N4 C20 H20 118.7(6) . . ? C19 C20 H20 118.7(7) . . ? N5 C21 C22 124.6(9) . . ? N5 C21 H21 117.7(6) . . ? C22 C21 H21 117.7(7) . . ? C23 C22 C21 117.4(10) . . ? C23 C22 H22 121.3(7) . . ? C21 C22 H22 121.3(7) . . ? C22 C23 C24 122.8(11) . . ? C22 C23 H23 118.6(7) . . ? C24 C23 H23 118.6(7) . . ? C23 C24 C25 117.5(10) . . ? C23 C24 H24 121.2(7) . . ? C25 C24 H24 121.2(7) . . ? N5 C25 C24 120.4(10) . . ? N5 C25 C26 113.4(10) . . ? C24 C25 C26 126.2(11) . . ? C26 C27 C28 118.3(10) . . ? C26 C27 H27 120.9(7) . . ? C28 C27 H27 120.8(6) . . ? C29 C28 C27 120.7(9) . . ? C29 C28 H28 119.6(7) . . ? C27 C28 H28 119.7(7) . . ? N6 C26 C27 122.8(10) . . ? N6 C26 C25 114.0(10) . . ? C27 C26 C25 123.2(11) . . ? C28 C29 C30 117.4(9) . . ? C28 C29 C37 123.5(10) . . ? C30 C29 C37 119.0(10) . . ? N6 C30 C29 124.2(9) . . ? N6 C30 H30 117.9(5) . . ? C29 C30 H30 117.9(6) . . ? N7 C31 C9 107.3(7) . . ? N7 C31 H31A 110.2(5) . . ? C9 C31 H31A 110.3(5) . . ? N7 C31 H31B 110.2(5) . . ? C9 C31 H31B 110.3(5) . . ? H31A C31 H31B 108.5 . . ? N7 C32 C33 109.2(9) . . ? N7 C32 H32A 109.8(5) . . ? C33 C32 H32A 109.8(6) . . ? N7 C32 H32B 109.8(5) . . ? C33 C32 H32B 109.8(6) . . ? H32A C32 H32B 108.3 . . ? C32 C33 N10 108.9(8) . . ? C32 C33 H33A 109.9(6) . . ? N10 C33 H33A 109.9(5) . . ? C32 C33 H33B 109.9(6) . . ? N10 C33 H33B 109.9(5) . . ? H33A C33 H33B 108.3 . . ? N8 C34 C12 109.4(8) . . ? N8 C34 H34A 109.8(6) . . ? C12 C34 H34A 109.8(5) . . ? N8 C34 H34B 109.8(5) . . ? C12 C34 H34B 109.8(5) . . ? H34A C34 H34B 108.2 . . ? N8 C35 C36 109.5(10) . . ? N8 C35 H35A 109.8(5) . . ? C36 C35 H35A 109.8(5) . . ? N8 C35 H35B 109.8(6) . . ? C36 C35 H35B 109.7(6) . . ? H35A C35 H35B 108.2 . . ? N10 C36 C35 108.1(8) . . ? N10 C36 H36A 110.1(5) . . ? C35 C36 H36A 110.1(6) . . ? N10 C36 H36B 110.1(6) . . ? C35 C36 H36B 110.0(6) . . ? H36A C36 H36B 108.4 . . ? N9 C37 C29 109.1(7) . . ? N9 C37 H37A 109.9(5) . . ? C29 C37 H37A 109.9(5) . . ? N9 C37 H37B 109.8(4) . . ? C29 C37 H37B 109.8(5) . . ? H37A C37 H37B 108.3 . . ? N9 C38 C39 109.4(8) . . ? N9 C38 H38A 109.8(5) . . ? C39 C38 H38A 109.8(6) . . ? N9 C38 H38B 109.8(5) . . ? C39 C38 H38B 109.8(5) . . ? H38A C38 H38B 108.3 . . ? N10 C39 C38 111.7(9) . . ? N10 C39 H39A 109.3(5) . . ? C38 C39 H39A 109.3(5) . . ? N10 C39 H39B 109.3(5) . . ? C38 C39 H39B 109.3(6) . . ? H39A C39 H39B 107.9 . . ? F21 P1 F61 91.6(5) . . ? F21 P1 F31 92.9(5) . . ? F61 P1 F31 175.5(5) . . ? F21 P1 F11 92.8(4) . . ? F61 P1 F11 91.7(4) . . ? F31 P1 F11 88.1(4) . . ? F21 P1 F41 176.9(5) . . ? F61 P1 F41 88.9(4) . . ? F31 P1 F41 86.7(4) . . ? F11 P1 F41 90.3(4) . . ? F21 P1 F51 89.1(4) . . ? F61 P1 F51 89.2(4) . . ? F31 P1 F51 91.0(4) . . ? F11 P1 F51 177.9(4) . . ? F41 P1 F51 87.8(4) . . ? F62 P2 F42 95.6(8) . . ? F62 P2 F22 97.6(8) . . ? F42 P2 F22 166.8(7) . . ? F62 P2 F52 175.4(6) . . ? F42 P2 F52 82.9(6) . . ? F22 P2 F52 84.1(5) . . ? F62 P2 F32 89.7(5) . . ? F42 P2 F32 89.8(4) . . ? F22 P2 F32 89.3(4) . . ? F52 P2 F32 94.6(5) . . ? F62 P2 F12 90.1(5) . . ? F42 P2 F12 91.1(4) . . ? F22 P2 F12 89.9(4) . . ? F52 P2 F12 85.6(5) . . ? F32 P2 F12 179.1(4) . . ? F63 P3 F23 90.8(5) . . ? F63 P3 F53 90.6(6) . . ? F23 P3 F53 89.0(4) . . ? F63 P3 F33 171.8(5) . . ? F23 P3 F33 97.1(5) . . ? F53 P3 F33 87.6(5) . . ? F63 P3 F43 91.2(6) . . ? F23 P3 F43 93.5(4) . . ? F53 P3 F43 176.9(5) . . ? F33 P3 F43 90.3(5) . . ? F63 P3 F13 89.2(4) . . ? F23 P3 F13 179.4(4) . . ? F53 P3 F13 91.7(5) . . ? F33 P3 F13 82.8(4) . . ? F43 P3 F13 85.8(4) . . ? N1G C1G C2G 178.7(17) . . ? C1G C2G H2G1 109.5(7) . . ? C1G C2G H2G2 109.5(7) . . ? H2G1 C2G H2G2 109.5 . . ? C1G C2G H2G3 109.4(8) . . ? H2G1 C2G H2G3 109.5 . . ? H2G2 C2G H2G3 109.5 . . ? N1S C1S C2S 164(4) . . ? C1S C2S H2S1 109.3(10) . . ? C1S C2S H2S2 109.5(11) . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.6(11) . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? _refine_diff_density_max 0.559 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.059