# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1467 data_fcno3pf6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H28 F6 Fe N O3 P' _chemical_formula_weight 519.24 _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' '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' '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 Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.049(3) _cell_length_b 10.353(4) _cell_length_c 13.905(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.24(3) _cell_angle_gamma 90.00 _cell_volume 1123.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 90 _cell_measurement_theta_min 3.87 _cell_measurement_theta_max 13.34 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method ? _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3167 _exptl_absorpt_correction_T_max 0.3474 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.92 _diffrn_reflns_number 3172 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 22.57 _reflns_number_total 2925 _reflns_number_observed 2127 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. 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^)+(0.1000P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(4) _refine_ls_number_reflns 2925 _refine_ls_number_parameters 280 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_obs 0.0524 _refine_ls_wR_factor_all 0.1500 _refine_ls_wR_factor_obs 0.1274 _refine_ls_goodness_of_fit_all 0.929 _refine_ls_goodness_of_fit_obs 0.939 _refine_ls_restrained_S_all 0.929 _refine_ls_restrained_S_obs 0.939 _refine_ls_shift/esd_max -0.038 _refine_ls_shift/esd_mean 0.003 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 0.20799(14) 0.05854(12) 0.96084(7) 0.0561(4) Uani 1 d . . N1 N 0.1512(8) -0.1530(6) 0.6770(5) 0.052(2) Uani 1 d . . H2N H 0.1439(8) -0.2292(6) 0.7083(5) 0.062 Uiso 1 calc R . O1 O -0.1623(8) -0.2954(7) 0.6586(5) 0.076(2) Uani 1 d . . O2 O 0.1182(7) -0.4550(7) 0.6564(4) 0.074(2) Uani 1 d . . O3 O 0.4094(8) -0.3290(7) 0.7637(5) 0.088(2) Uani 1 d . . C1 C 0.2420(10) -0.0477(8) 0.8442(6) 0.056(2) Uani 1 d . . C2 C 0.3811(11) 0.0377(10) 0.8790(7) 0.069(2) Uani 1 d . . H2A H 0.4165(11) 0.1017(10) 0.8416(7) 0.082 Uiso 1 calc R . C3 C 0.4575(14) 0.0102(13) 0.9794(9) 0.096(4) Uani 1 d . . H3A H 0.5500(14) 0.0534(13) 1.0199(9) 0.116 Uiso 1 calc R . C4 C 0.3715(16) -0.0910(13) 1.0062(8) 0.095(4) Uani 1 d . . H4A H 0.3978(16) -0.1296(13) 1.0685(8) 0.114 Uiso 1 calc R . C5 C 0.2358(13) -0.1294(8) 0.9254(7) 0.069(3) Uani 1 d . . H5A H 0.1576(13) -0.1954(8) 0.9256(7) 0.083 Uiso 1 calc R . C6 C -0.0377(18) 0.1180(18) 0.9422(12) 0.118(6) Uani 1 d . . H6A H -0.1334(18) 0.0835(18) 0.8981(12) 0.142 Uiso 1 calc R . C7 C 0.0543(29) 0.2134(19) 0.9187(12) 0.128(7) Uani 1 d . . H7A H 0.0370(29) 0.2538(19) 0.8573(12) 0.153 Uiso 1 calc R . C8 C 0.1840(20) 0.2419(12) 1.0049(19) 0.128(6) Uani 1 d . . H8A H 0.2687(20) 0.3049(12) 1.0131(19) 0.154 Uiso 1 calc R . C9 C 0.1546(17) 0.1514(14) 1.0767(8) 0.097(4) Uani 1 d . . H9A H 0.2182(17) 0.1447(14) 1.1421(8) 0.116 Uiso 1 calc R . C10 C 0.0182(16) 0.0769(14) 1.0330(12) 0.101(4) Uani 1 d . . H10A H -0.0271(16) 0.0092(14) 1.0624(12) 0.121 Uiso 1 calc R . C11 C 0.1216(12) -0.0471(9) 0.7457(6) 0.075(3) Uani 1 d . . H11A H 0.1297(12) 0.0356(9) 0.7145(6) 0.090 Uiso 1 calc R . H11B H 0.0060(12) -0.0552(9) 0.7542(6) 0.090 Uiso 1 calc R . C12 C 0.0099(13) -0.1539(9) 0.5821(6) 0.068(3) Uani 1 d . . H12A H 0.0051(13) -0.0699(9) 0.5508(6) 0.082 Uiso 1 calc R . H12B H 0.0377(13) -0.2171(9) 0.5370(6) 0.082 Uiso 1 calc R . C13 C -0.1628(12) -0.1849(10) 0.5986(8) 0.080(3) Uani 1 d . . H13A H -0.2030(12) -0.1114(10) 0.6297(8) 0.096 Uiso 1 calc R . H13B H -0.2428(12) -0.1988(10) 0.5348(8) 0.096 Uiso 1 calc R . C14 C -0.1748(11) -0.4171(9) 0.6083(8) 0.076(3) Uani 1 d . . H14A H -0.1613(11) -0.4046(9) 0.5415(8) 0.091 Uiso 1 calc R . H14B H -0.2867(11) -0.4550(9) 0.6038(8) 0.091 Uiso 1 calc R . C15 C -0.0410(13) -0.5033(9) 0.6632(8) 0.077(3) Uani 1 d . . H15A H -0.0457(13) -0.5077(9) 0.7322(8) 0.092 Uiso 1 calc R . H15B H -0.0577(13) -0.5896(9) 0.6354(8) 0.092 Uiso 1 calc R . C16 C 0.2648(15) -0.5239(9) 0.7160(9) 0.097(4) Uani 1 d . . H16A H 0.2732(15) -0.6088(9) 0.6881(9) 0.116 Uiso 1 calc R . H16B H 0.2524(15) -0.5346(9) 0.7832(9) 0.116 Uiso 1 calc R . C17 C 0.4187(12) -0.4484(14) 0.7166(8) 0.092(3) Uani 1 d . . H17A H 0.5198(12) -0.4954(14) 0.7517(8) 0.111 Uiso 1 calc R . H17B H 0.4273(12) -0.4340(14) 0.6490(8) 0.111 Uiso 1 calc R . C18 C 0.4582(15) -0.2122(12) 0.7277(12) 0.123(5) Uani 1 d . . H18A H 0.5535(15) -0.2284(12) 0.6981(12) 0.148 Uiso 1 calc R . H18B H 0.4979(15) -0.1536(12) 0.7830(12) 0.148 Uiso 1 calc R . C19 C 0.3213(13) -0.1505(10) 0.6548(8) 0.079(3) Uani 1 d . . H19A H 0.3120(13) -0.1922(10) 0.5912(8) 0.095 Uiso 1 calc R . H19B H 0.3529(13) -0.0611(10) 0.6481(8) 0.095 Uiso 1 calc R . P1 P 0.6214(3) 0.1808(2) 0.6398(2) 0.0548(6) Uani 1 d . . F1 F 0.5797(8) 0.2982(5) 0.5650(5) 0.103(2) Uani 1 d . . F2 F 0.8126(7) 0.1778(6) 0.6286(5) 0.101(2) Uani 1 d . . F3 F 0.6705(9) 0.2790(6) 0.7272(5) 0.114(2) Uani 1 d . . F4 F 0.5691(8) 0.0805(6) 0.5521(4) 0.103(2) Uani 1 d . . F5 F 0.4280(7) 0.1826(6) 0.6475(5) 0.099(2) Uani 1 d . . F6 F 0.6658(6) 0.0632(6) 0.7154(3) 0.0824(14) 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 0.0599(7) 0.0534(7) 0.0529(6) -0.0004(7) 0.0100(5) 0.0030(7) N1 0.055(4) 0.048(4) 0.054(4) -0.003(3) 0.017(3) 0.004(3) O1 0.070(4) 0.076(5) 0.085(4) -0.022(4) 0.027(3) 0.001(4) O2 0.068(4) 0.063(4) 0.093(4) 0.010(4) 0.025(3) 0.007(4) O3 0.069(4) 0.072(5) 0.119(5) 0.006(4) 0.017(4) 0.014(4) C1 0.056(5) 0.057(5) 0.056(5) -0.006(4) 0.014(4) -0.001(4) C2 0.071(5) 0.066(7) 0.074(6) -0.012(6) 0.030(5) -0.009(5) C3 0.066(7) 0.124(13) 0.092(9) -0.041(7) 0.005(6) -0.001(7) C4 0.111(11) 0.097(10) 0.063(7) 0.004(7) -0.004(7) 0.059(8) C5 0.088(7) 0.044(5) 0.087(7) 0.010(5) 0.042(6) 0.007(5) C6 0.089(9) 0.175(17) 0.080(9) -0.057(10) -0.001(7) 0.056(10) C7 0.172(18) 0.125(14) 0.110(12) 0.051(11) 0.079(12) 0.087(12) C8 0.105(12) 0.051(8) 0.241(21) -0.052(11) 0.067(13) -0.016(7) C9 0.107(9) 0.104(10) 0.065(7) -0.018(7) -0.004(7) 0.047(8) C10 0.096(8) 0.093(9) 0.132(11) -0.035(10) 0.063(8) -0.023(8) C11 0.081(7) 0.061(6) 0.076(6) -0.018(5) 0.005(5) 0.024(5) C12 0.101(8) 0.055(5) 0.044(5) -0.002(4) 0.009(5) 0.004(5) C13 0.062(7) 0.073(7) 0.094(7) -0.021(6) -0.003(5) 0.003(5) C14 0.061(5) 0.061(7) 0.110(7) -0.030(6) 0.027(5) -0.017(5) C15 0.082(7) 0.066(6) 0.092(7) -0.001(6) 0.040(6) -0.015(6) C16 0.093(9) 0.050(6) 0.132(10) 0.006(6) -0.004(7) 0.019(6) C17 0.067(6) 0.092(8) 0.114(7) -0.020(8) 0.014(5) 0.033(7) C18 0.072(8) 0.091(9) 0.220(16) 0.014(10) 0.061(10) -0.001(7) C19 0.079(8) 0.065(6) 0.105(8) 0.017(6) 0.042(6) -0.002(6) P1 0.0575(13) 0.0426(12) 0.0621(13) 0.0059(11) 0.0107(10) -0.0017(11) F1 0.111(5) 0.081(4) 0.115(5) 0.054(4) 0.021(4) 0.012(4) F2 0.069(3) 0.080(4) 0.160(6) 0.018(4) 0.039(4) 0.002(3) F3 0.158(6) 0.069(4) 0.092(4) -0.027(3) -0.011(4) 0.011(4) F4 0.117(4) 0.101(5) 0.081(3) -0.024(4) 0.002(3) 0.002(4) F5 0.067(3) 0.094(4) 0.143(5) 0.027(4) 0.042(3) 0.009(3) F6 0.100(4) 0.055(3) 0.089(3) 0.022(4) 0.017(3) 0.020(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 Fe1 C9 2.011(10) . ? Fe1 C2 2.016(8) . ? Fe1 C8 2.019(11) . ? Fe1 C7 2.022(12) . ? Fe1 C3 2.024(11) . ? Fe1 C6 2.026(12) . ? Fe1 C4 2.030(10) . ? Fe1 C10 2.033(10) . ? Fe1 C5 2.033(9) . ? Fe1 C1 2.033(8) . ? N1 C19 1.476(11) . ? N1 C11 1.510(10) . ? N1 C12 1.515(10) . ? O1 C13 1.415(11) . ? O1 C14 1.432(10) . ? O2 C15 1.400(11) . ? O2 C16 1.451(11) . ? O3 C18 1.401(13) . ? O3 C17 1.410(14) . ? C1 C2 1.415(12) . ? C1 C5 1.423(11) . ? C1 C11 1.469(11) . ? C2 C3 1.409(14) . ? C3 C4 1.36(2) . ? C4 C5 1.417(14) . ? C6 C10 1.30(2) . ? C6 C7 1.32(2) . ? C7 C8 1.41(2) . ? C8 C9 1.43(2) . ? C9 C10 1.36(2) . ? C12 C13 1.499(13) . ? C14 C15 1.462(13) . ? C16 C17 1.463(15) . ? C18 C19 1.45(2) . ? P1 F3 1.559(6) . ? P1 F4 1.578(6) . ? P1 F1 1.580(5) . ? P1 F2 1.584(6) . ? P1 F5 1.587(6) . ? P1 F6 1.592(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Fe1 C2 144.8(6) . . ? C9 Fe1 C8 41.6(6) . . ? C2 Fe1 C8 113.8(6) . . ? C9 Fe1 C7 67.5(5) . . ? C2 Fe1 C7 112.3(6) . . ? C8 Fe1 C7 41.0(6) . . ? C9 Fe1 C3 114.6(5) . . ? C2 Fe1 C3 40.8(4) . . ? C8 Fe1 C3 111.1(6) . . ? C7 Fe1 C3 138.6(9) . . ? C9 Fe1 C6 64.1(4) . . ? C2 Fe1 C6 138.5(6) . . ? C8 Fe1 C6 65.8(6) . . ? C7 Fe1 C6 38.2(6) . . ? C3 Fe1 C6 176.6(8) . . ? C9 Fe1 C4 111.5(4) . . ? C2 Fe1 C4 66.9(4) . . ? C8 Fe1 C4 136.6(8) . . ? C7 Fe1 C4 177.3(10) . . ? C3 Fe1 C4 39.1(5) . . ? C6 Fe1 C4 144.0(8) . . ? C9 Fe1 C10 39.2(5) . . ? C2 Fe1 C10 175.3(6) . . ? C8 Fe1 C10 67.8(6) . . ? C7 Fe1 C10 65.7(6) . . ? C3 Fe1 C10 143.4(6) . . ? C6 Fe1 C10 37.4(5) . . ? C4 Fe1 C10 115.3(6) . . ? C9 Fe1 C5 135.2(5) . . ? C2 Fe1 C5 68.2(4) . . ? C8 Fe1 C5 176.5(8) . . ? C7 Fe1 C5 141.7(8) . . ? C3 Fe1 C5 68.2(4) . . ? C6 Fe1 C5 115.0(6) . . ? C4 Fe1 C5 40.8(4) . . ? C10 Fe1 C5 110.5(5) . . ? C9 Fe1 C1 174.2(6) . . ? C2 Fe1 C1 40.9(3) . . ? C8 Fe1 C1 142.4(7) . . ? C7 Fe1 C1 113.0(5) . . ? C3 Fe1 C1 69.1(4) . . ? C6 Fe1 C1 112.4(4) . . ? C4 Fe1 C1 68.4(4) . . ? C10 Fe1 C1 135.2(5) . . ? C5 Fe1 C1 41.0(3) . . ? C19 N1 C11 114.7(7) . . ? C19 N1 C12 110.7(7) . . ? C11 N1 C12 110.7(6) . . ? C13 O1 C14 115.7(7) . . ? C15 O2 C16 114.5(8) . . ? C18 O3 C17 122.6(10) . . ? C2 C1 C5 106.2(7) . . ? C2 C1 C11 127.0(8) . . ? C5 C1 C11 126.8(8) . . ? C2 C1 Fe1 68.9(5) . . ? C5 C1 Fe1 69.5(5) . . ? C11 C1 Fe1 123.6(6) . . ? C3 C2 C1 109.2(9) . . ? C3 C2 Fe1 69.9(5) . . ? C1 C2 Fe1 70.2(5) . . ? C4 C3 C2 107.4(10) . . ? C4 C3 Fe1 70.7(7) . . ? C2 C3 Fe1 69.3(6) . . ? C3 C4 C5 110.1(10) . . ? C3 C4 Fe1 70.2(7) . . ? C5 C4 Fe1 69.7(5) . . ? C4 C5 C1 107.0(9) . . ? C4 C5 Fe1 69.5(6) . . ? C1 C5 Fe1 69.5(5) . . ? C10 C6 C7 113.7(14) . . ? C10 C6 Fe1 71.6(7) . . ? C7 C6 Fe1 70.7(8) . . ? C6 C7 C8 106.7(13) . . ? C6 C7 Fe1 71.1(8) . . ? C8 C7 Fe1 69.4(7) . . ? C7 C8 C9 103.9(12) . . ? C7 C8 Fe1 69.6(7) . . ? C9 C8 Fe1 68.9(6) . . ? C10 C9 C8 108.3(11) . . ? C10 C9 Fe1 71.3(6) . . ? C8 C9 Fe1 69.5(7) . . ? C6 C10 C9 107.3(13) . . ? C6 C10 Fe1 71.0(7) . . ? C9 C10 Fe1 69.5(6) . . ? C1 C11 N1 114.6(7) . . ? C13 C12 N1 113.2(7) . . ? O1 C13 C12 113.3(8) . . ? O1 C14 C15 109.1(8) . . ? O2 C15 C14 108.4(8) . . ? O2 C16 C17 108.0(8) . . ? O3 C17 C16 109.2(8) . . ? O3 C18 C19 113.5(10) . . ? C18 C19 N1 115.5(9) . . ? F3 P1 F4 179.0(4) . . ? F3 P1 F1 89.1(4) . . ? F4 P1 F1 91.4(4) . . ? F3 P1 F2 91.3(4) . . ? F4 P1 F2 89.6(3) . . ? F1 P1 F2 90.3(3) . . ? F3 P1 F5 90.2(4) . . ? F4 P1 F5 88.9(4) . . ? F1 P1 F5 89.0(3) . . ? F2 P1 F5 178.3(4) . . ? F3 P1 F6 90.6(3) . . ? F4 P1 F6 88.9(3) . . ? F1 P1 F6 179.3(4) . . ? F2 P1 F6 89.1(3) . . ? F5 P1 F6 91.6(3) . . ? _refine_diff_density_max 0.416 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.052 data_fc2n2o3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H48 Cl2 F12 Fe2 N2 O4 P2' _chemical_formula_weight 1009.27 _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' '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' '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' 'Cl' 'Cl' 0.1484 0.1585 '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 11.069(4) _cell_length_b 11.206(4) _cell_length_c 17.482(6) _cell_angle_alpha 85.12(3) _cell_angle_beta 75.06(3) _cell_angle_gamma 87.18(3) _cell_volume 2086.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 99 _cell_measurement_theta_min 4.63 _cell_measurement_theta_max 12.64 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method ? _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.992 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.73 _diffrn_reflns_number 5702 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5359 _reflns_number_observed 3380 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. 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^)+(0.1000P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5358 _refine_ls_number_parameters 576 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1213 _refine_ls_R_factor_obs 0.0714 _refine_ls_wR_factor_all 0.2140 _refine_ls_wR_factor_obs 0.1821 _refine_ls_goodness_of_fit_all 1.270 _refine_ls_goodness_of_fit_obs 1.404 _refine_ls_restrained_S_all 1.271 _refine_ls_restrained_S_obs 1.404 _refine_ls_shift/esd_max 0.014 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe -0.24628(11) 0.16019(10) 0.92110(7) 0.0644(4) Uani 1 d . . Fe2 Fe 0.36659(10) 0.71925(10) 0.46403(7) 0.0568(4) Uani 1 d . . N1 N -0.2844(6) 0.5321(5) 0.8184(4) 0.057(2) Uani 1 d . . HN1 H -0.2342(6) 0.5712(5) 0.7749(4) 0.069 Uiso 1 calc R . N2 N 0.0488(5) 0.7630(5) 0.6763(3) 0.050(2) Uani 1 d . . HN2 H -0.0273(5) 0.7289(5) 0.6879(3) 0.060 Uiso 1 calc R . O1 O -0.0950(5) 0.6782(5) 0.8205(3) 0.0597(14) Uani 1 d . . O2 O -0.3672(5) 0.6998(5) 0.7169(3) 0.067(2) Uani 1 d . . O3 O -0.1863(5) 0.8693(5) 0.6802(3) 0.0600(14) Uani 1 d . . O4 O -0.1241(5) 0.5812(5) 0.6631(3) 0.0607(14) Uani 1 d D . C1 C -0.2912(9) 0.3356(8) 0.8985(5) 0.070(2) Uani 1 d . . C2 C -0.3954(9) 0.2624(8) 0.9041(7) 0.098(4) Uani 1 d . . H2A H -0.4402(9) 0.2555(8) 0.8632(7) 0.117 Uiso 1 calc R . C3 C -0.4236(12) 0.2032(11) 0.9828(9) 0.118(5) Uani 1 d . . H3A H -0.4904(12) 0.1460(11) 1.0041(9) 0.142 Uiso 1 calc R . C4 C -0.3405(17) 0.2353(11) 1.0222(8) 0.132(6) Uani 1 d . . H4A H -0.3384(17) 0.2055(11) 1.0762(8) 0.158 Uiso 1 calc R . C5 C -0.2585(11) 0.3194(8) 0.9730(6) 0.091(3) Uani 1 d . . H5A H -0.1901(11) 0.3579(8) 0.9867(6) 0.110 Uiso 1 calc R . C6 C -0.0718(12) 0.0917(15) 0.9076(13) 0.123(4) Uani 1 d . . H6A H -0.0049(12) 0.1233(15) 0.9268(13) 0.147 Uiso 1 calc R . C7 C -0.0939(16) 0.1165(11) 0.8353(9) 0.108(5) Uani 1 d . . H7A H -0.0468(16) 0.1732(11) 0.7938(9) 0.129 Uiso 1 calc R . C8 C -0.1898(23) 0.0561(21) 0.8292(13) 0.145(7) Uani 1 d . . H8A H -0.2240(23) 0.0592(21) 0.7826(13) 0.174 Uiso 1 calc R . C9 C -0.2283(16) -0.0151(12) 0.8962(19) 0.156(8) Uani 1 d . . H9A H -0.2972(16) -0.0709(12) 0.9068(19) 0.187 Uiso 1 calc R . C10 C -0.1601(21) 0.0055(17) 0.9484(8) 0.140(7) Uani 1 d . . H10A H -0.1669(21) -0.0347(17) 1.0013(8) 0.167 Uiso 1 calc R . C11 C 0.2516(7) 0.7633(6) 0.5673(4) 0.047(2) Uani 1 d . . C12 C 0.2857(8) 0.8677(7) 0.5161(5) 0.068(2) Uani 1 d . . H12A H 0.2277(8) 0.9237(7) 0.4964(5) 0.081 Uiso 1 calc R . C13 C 0.4148(11) 0.8767(12) 0.4972(7) 0.101(4) Uani 1 d . . H13A H 0.4633(11) 0.9395(12) 0.4616(7) 0.121 Uiso 1 calc R . C14 C 0.4651(8) 0.7775(13) 0.5364(6) 0.099(4) Uani 1 d . . H14A H 0.5536(8) 0.7601(13) 0.5337(6) 0.118 Uiso 1 calc R . C15 C 0.3606(8) 0.7085(8) 0.5821(5) 0.065(2) Uani 1 d . . H15A H 0.3653(8) 0.6348(8) 0.6158(5) 0.077 Uiso 1 calc R . C16 C 0.2780(8) 0.5969(8) 0.4207(5) 0.066(2) Uani 1 d . . H16A H 0.1976(8) 0.5617(8) 0.4483(5) 0.079 Uiso 1 calc R . C17 C 0.2932(9) 0.7016(10) 0.3701(6) 0.080(3) Uani 1 d . . H17A H 0.2266(9) 0.7518(10) 0.3552(6) 0.096 Uiso 1 calc R . C18 C 0.4242(12) 0.7205(10) 0.3434(6) 0.091(3) Uani 1 d . . H18A H 0.4635(12) 0.7874(10) 0.3074(6) 0.109 Uiso 1 calc R . C19 C 0.4869(9) 0.6293(12) 0.3782(6) 0.093(3) Uani 1 d . . H19A H 0.5776(9) 0.6192(12) 0.3705(6) 0.111 Uiso 1 calc R . C20 C 0.3931(10) 0.5519(9) 0.4267(6) 0.079(3) Uani 1 d . . H20A H 0.4085(10) 0.4791(9) 0.4584(6) 0.095 Uiso 1 calc R . C21 C -0.2238(7) 0.4106(7) 0.8281(5) 0.057(2) Uani 1 d . . H21A H -0.2183(7) 0.3686(7) 0.7810(5) 0.068 Uiso 1 calc R . H21B H -0.1392(7) 0.4209(7) 0.8321(5) 0.068 Uiso 1 calc R . C22 C 0.1226(6) 0.7173(7) 0.5973(4) 0.049(2) Uani 1 d . . H22A H 0.1279(6) 0.6305(7) 0.6032(4) 0.058 Uiso 1 calc R . H22B H 0.0765(6) 0.7395(7) 0.5577(4) 0.058 Uiso 1 calc R . C23 C 0.1082(7) 0.7175(8) 0.7417(4) 0.060(2) Uani 1 d . . H23A H 0.1823(7) 0.7627(8) 0.7379(4) 0.072 Uiso 1 calc R . H23B H 0.1338(7) 0.6341(8) 0.7356(4) 0.072 Uiso 1 calc R . C24 C 0.0179(7) 0.7291(8) 0.8229(4) 0.062(2) Uani 1 d . . H24A H 0.0516(7) 0.6869(8) 0.8640(4) 0.075 Uiso 1 calc R . H24B H 0.0039(7) 0.8127(8) 0.8340(4) 0.075 Uiso 1 calc R . C25 C -0.1684(8) 0.6354(7) 0.8964(4) 0.063(2) Uani 1 d . . H25A H -0.1765(8) 0.6958(7) 0.9342(4) 0.075 Uiso 1 calc R . H25B H -0.1296(8) 0.5637(7) 0.9158(4) 0.075 Uiso 1 calc R . C26 C -0.2944(8) 0.6083(7) 0.8861(5) 0.064(2) Uani 1 d . . H26A H -0.3429(8) 0.5674(7) 0.9345(5) 0.077 Uiso 1 calc R . H26B H -0.3385(8) 0.6829(7) 0.8767(5) 0.077 Uiso 1 calc R . C27 C -0.4092(7) 0.5193(7) 0.7994(5) 0.068(2) Uani 1 d . . H27A H -0.3985(7) 0.4655(7) 0.7574(5) 0.082 Uiso 1 calc R . H27B H -0.4680(7) 0.4840(7) 0.8460(5) 0.082 Uiso 1 calc R . C28 C -0.4615(8) 0.6361(8) 0.7742(5) 0.073(3) Uani 1 d . . H28A H -0.5307(8) 0.6229(8) 0.7516(5) 0.088 Uiso 1 calc R . H28B H -0.4928(8) 0.6828(8) 0.8198(5) 0.088 Uiso 1 calc R . C29 C -0.3977(8) 0.8220(8) 0.7067(6) 0.072(2) Uani 1 d . . H29A H -0.4153(8) 0.8571(8) 0.7574(6) 0.086 Uiso 1 calc R . H29B H -0.4723(8) 0.8316(8) 0.6870(6) 0.086 Uiso 1 calc R . C30 C -0.2931(7) 0.8846(8) 0.6498(5) 0.066(2) Uani 1 d . . H30A H -0.2765(7) 0.8514(8) 0.5985(5) 0.080 Uiso 1 calc R . H30B H -0.3145(7) 0.9692(8) 0.6431(5) 0.080 Uiso 1 calc R . C31 C -0.0796(7) 0.9287(7) 0.6324(5) 0.059(2) Uani 1 d . . H31A H -0.0947(7) 1.0148(7) 0.6298(5) 0.071 Uiso 1 calc R . H31B H -0.0585(7) 0.9026(7) 0.5790(5) 0.071 Uiso 1 calc R . C32 C 0.0241(7) 0.8952(6) 0.6721(5) 0.055(2) Uani 1 d . . H32A H 0.0997(7) 0.9352(6) 0.6427(5) 0.066 Uiso 1 calc R . H32B H 0.0015(7) 0.9222(6) 0.7254(5) 0.066 Uiso 1 calc R . P1 P 0.7811(2) 0.5883(2) 0.13248(14) 0.0693(7) Uani 1 d . . F1 F 0.6883(5) 0.5800(7) 0.0766(4) 0.120(2) Uani 1 d . . F2 F 0.8746(7) 0.5861(9) 0.1838(4) 0.175(4) Uani 1 d . . F3 F 0.8192(7) 0.7138(6) 0.0911(4) 0.142(3) Uani 1 d . . F4 F 0.6676(7) 0.6420(7) 0.1948(4) 0.146(3) Uani 1 d . . F5 F 0.8869(6) 0.5298(7) 0.0656(4) 0.125(2) Uani 1 d . . F6 F 0.7398(6) 0.4583(6) 0.1717(4) 0.131(3) Uani 1 d . . P2 P 0.8883(2) 0.7105(2) 0.41708(15) 0.0699(7) Uani 1 d . . F7 F 0.8071(10) 0.6160(11) 0.3963(6) 0.205(5) Uani 1 d . . F8 F 0.9757(9) 0.7920(8) 0.4425(5) 0.175(4) Uani 1 d . . F10 F 0.8198(24) 0.7899(22) 0.3821(18) 0.245(14) Uani 0.63(2) d P 1 F13 F 0.7926(15) 0.6967(20) 0.4943(12) 0.158(10) Uani 0.63(2) d P 1 F11 F 0.9917(20) 0.7088(29) 0.3395(10) 0.181(11) Uani 0.63(2) d P 1 F12 F 0.9609(12) 0.6016(15) 0.4527(12) 0.132(7) Uani 0.63(2) d P 1 F14 F 0.7960(27) 0.8358(23) 0.4461(16) 0.162(13) Uani 0.37(2) d P 2 F15 F 0.8984(55) 0.7844(30) 0.3324(13) 0.182(21) Uani 0.37(2) d P 2 F16 F 0.9789(36) 0.6182(35) 0.3792(33) 0.226(24) Uani 0.37(2) d P 2 F9 F 0.8543(53) 0.6763(27) 0.5067(15) 0.197(24) Uani 0.37(2) d P 2 C33 C 0.7075(13) 0.9170(12) 0.2249(12) 0.156(6) Uani 1 d . . H33A H 0.7948(13) 0.8915(12) 0.2150(12) 0.187 Uiso 0.46(2) calc PR 1 H33B H 0.6581(13) 0.8457(12) 0.2329(12) 0.187 Uiso 0.46(2) calc PR 1 H33C H 0.6824(13) 0.8522(12) 0.2656(12) 0.187 Uiso 0.54(2) calc PR 2 H33D H 0.7879(13) 0.8951(12) 0.1906(12) 0.187 Uiso 0.54(2) calc PR 2 Cl1 Cl 0.6655(7) 0.9949(8) 0.3130(4) 0.081(3) Uani 0.46(2) d P 1 Cl2 Cl 0.6892(47) 0.9864(29) 0.1584(7) 0.404(26) Uani 0.46(2) d P 1 Cl3 Cl 0.7167(25) 1.0227(19) 0.2599(30) 0.437(21) Uani 0.54(2) d P 2 Cl4 Cl 0.5827(7) 0.9442(6) 0.1629(5) 0.107(3) Uani 0.54(2) d P 2 H2O4 H -0.0754(82) 0.5147(61) 0.6392(59) 0.128 Uiso 1 d D . H1O4 H -0.1798(76) 0.6190(87) 0.6340(54) 0.128 Uiso 1 d 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 0.0674(9) 0.0530(7) 0.0625(8) -0.0020(6) 0.0006(6) 0.0013(6) Fe2 0.0444(7) 0.0675(8) 0.0561(7) -0.0151(6) -0.0015(5) -0.0199(6) N1 0.059(4) 0.055(4) 0.053(4) 0.002(3) -0.005(3) -0.013(3) N2 0.048(4) 0.049(4) 0.052(4) 0.003(3) -0.015(3) -0.006(3) O1 0.060(3) 0.079(4) 0.037(3) -0.001(3) -0.005(3) -0.016(3) O2 0.051(3) 0.063(4) 0.079(4) 0.008(3) -0.006(3) 0.001(3) O3 0.052(3) 0.063(3) 0.064(3) 0.008(3) -0.018(3) 0.000(3) O4 0.053(4) 0.064(4) 0.063(4) -0.014(3) -0.006(3) -0.012(3) C1 0.078(6) 0.056(5) 0.069(6) 0.006(4) -0.009(5) -0.005(5) C2 0.063(6) 0.067(6) 0.148(10) 0.036(7) -0.012(7) -0.005(5) C3 0.093(9) 0.072(8) 0.135(12) 0.022(8) 0.057(8) 0.022(7) C4 0.209(17) 0.070(8) 0.071(8) 0.007(6) 0.036(10) 0.035(10) C5 0.149(10) 0.056(6) 0.059(6) -0.012(5) -0.007(6) 0.014(6) C6 0.070(8) 0.135(13) 0.169(15) -0.036(11) -0.040(9) 0.029(8) C7 0.113(11) 0.074(8) 0.094(10) 0.005(7) 0.038(8) 0.046(8) C8 0.176(19) 0.127(15) 0.151(16) -0.091(13) -0.064(14) 0.068(13) C9 0.131(14) 0.042(7) 0.259(25) -0.042(11) 0.024(17) 0.009(8) C10 0.180(18) 0.113(13) 0.090(10) 0.031(9) 0.004(11) 0.071(12) C11 0.046(5) 0.043(4) 0.053(5) -0.011(4) -0.011(4) -0.001(4) C12 0.073(6) 0.052(5) 0.070(6) -0.009(4) 0.002(5) -0.015(4) C13 0.094(9) 0.118(10) 0.087(8) -0.025(7) -0.001(7) -0.064(8) C14 0.039(5) 0.177(12) 0.086(8) -0.072(8) -0.001(5) -0.034(7) C15 0.056(5) 0.083(6) 0.060(5) -0.014(4) -0.020(4) -0.005(5) C16 0.060(6) 0.075(6) 0.065(6) -0.014(5) -0.014(5) -0.020(5) C17 0.065(7) 0.099(8) 0.081(7) -0.029(6) -0.022(5) 0.004(6) C18 0.115(10) 0.097(8) 0.055(6) -0.015(5) -0.001(6) -0.033(7) C19 0.044(6) 0.149(11) 0.083(7) -0.051(7) 0.001(5) -0.009(7) C20 0.091(8) 0.072(6) 0.080(6) -0.036(5) -0.024(6) 0.016(6) C21 0.058(5) 0.055(5) 0.056(5) -0.006(4) -0.011(4) -0.004(4) C22 0.047(5) 0.053(4) 0.043(4) -0.007(3) -0.005(4) -0.007(4) C23 0.052(5) 0.068(5) 0.058(5) 0.005(4) -0.016(4) 0.000(4) C24 0.063(6) 0.080(6) 0.045(5) -0.002(4) -0.017(4) -0.008(5) C25 0.078(6) 0.059(5) 0.050(5) -0.003(4) -0.013(4) -0.009(4) C26 0.068(6) 0.053(5) 0.062(5) -0.003(4) -0.002(4) -0.009(4) C27 0.051(5) 0.065(6) 0.086(6) 0.005(5) -0.016(5) -0.007(4) C28 0.057(6) 0.082(7) 0.075(6) 0.008(5) -0.011(5) -0.003(5) C29 0.054(6) 0.074(6) 0.089(7) -0.003(5) -0.024(5) 0.007(5) C30 0.059(6) 0.066(6) 0.076(6) 0.005(5) -0.027(5) 0.015(4) C31 0.055(5) 0.049(5) 0.064(5) 0.002(4) -0.003(4) 0.003(4) C32 0.054(5) 0.042(4) 0.069(5) -0.001(4) -0.015(4) -0.005(4) P1 0.0602(15) 0.083(2) 0.0583(14) 0.0005(12) -0.0051(12) -0.0076(12) F1 0.087(4) 0.175(6) 0.100(4) 0.003(4) -0.032(4) -0.005(4) F2 0.143(6) 0.287(11) 0.117(6) 0.018(6) -0.069(5) -0.092(7) F3 0.162(7) 0.082(4) 0.152(6) 0.005(4) 0.016(5) -0.029(4) F4 0.138(6) 0.159(7) 0.105(5) -0.043(5) 0.046(4) -0.007(5) F5 0.093(4) 0.163(6) 0.098(4) -0.015(4) 0.009(4) 0.024(4) F6 0.096(5) 0.111(5) 0.168(6) 0.057(5) -0.023(4) -0.010(4) P2 0.0559(15) 0.085(2) 0.070(2) 0.0013(13) -0.0180(13) -0.0142(13) F7 0.201(10) 0.257(12) 0.188(9) -0.020(8) -0.085(8) -0.116(9) F8 0.199(9) 0.169(8) 0.173(8) -0.033(6) -0.053(7) -0.092(7) F10 0.273(27) 0.238(25) 0.201(29) 0.047(24) -0.070(23) 0.163(22) F13 0.099(10) 0.169(19) 0.157(18) -0.027(14) 0.066(11) -0.025(10) F11 0.147(16) 0.274(31) 0.093(10) 0.019(15) 0.018(10) -0.054(18) F12 0.110(10) 0.135(12) 0.154(15) -0.002(11) -0.049(10) 0.025(8) F14 0.213(26) 0.146(21) 0.106(18) -0.052(15) -0.011(16) 0.117(18) F15 0.337(61) 0.148(21) 0.036(11) 0.038(12) -0.023(20) 0.028(27) F16 0.229(39) 0.177(31) 0.316(60) -0.202(38) -0.122(39) 0.171(31) F9 0.480(70) 0.080(17) 0.060(14) 0.019(12) -0.124(29) -0.044(30) C33 0.103(10) 0.090(9) 0.259(20) 0.010(12) -0.027(11) 0.009(8) Cl1 0.056(4) 0.087(5) 0.105(6) -0.020(4) -0.030(4) 0.014(3) Cl2 0.688(59) 0.341(26) 0.084(7) 0.008(11) 0.000(17) 0.371(34) Cl3 0.261(20) 0.213(15) 1.010(63) -0.290(28) -0.411(32) 0.078(14) Cl4 0.119(6) 0.079(4) 0.120(5) -0.013(3) -0.025(4) -0.004(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 Fe1 C6 2.006(11) . ? Fe1 C8 2.015(13) . ? Fe1 C10 2.019(12) . ? Fe1 C7 2.019(10) . ? Fe1 C2 2.033(10) . ? Fe1 C4 2.033(12) . ? Fe1 C9 2.038(12) . ? Fe1 C1 2.035(9) . ? Fe1 C3 2.038(11) . ? Fe1 C5 2.052(9) . ? Fe2 C11 2.007(7) . ? Fe2 C12 2.022(8) . ? Fe2 C20 2.021(9) . ? Fe2 C16 2.027(8) . ? Fe2 C14 2.034(9) . ? Fe2 C17 2.038(9) . ? Fe2 C19 2.033(9) . ? Fe2 C18 2.038(9) . ? Fe2 C13 2.039(10) . ? Fe2 C15 2.042(8) . ? N1 C26 1.496(9) . ? N1 C21 1.504(9) . ? N1 C27 1.518(9) . ? N2 C32 1.492(9) . ? N2 C23 1.501(9) . ? N2 C22 1.529(8) . ? O1 C24 1.411(9) . ? O1 C25 1.423(9) . ? O2 C29 1.402(10) . ? O2 C28 1.419(9) . ? O3 C30 1.413(9) . ? O3 C31 1.418(8) . ? C1 C2 1.426(12) . ? C1 C5 1.434(13) . ? C1 C21 1.478(11) . ? C2 C3 1.44(2) . ? C3 C4 1.36(2) . ? C4 C5 1.41(2) . ? C6 C7 1.35(2) . ? C6 C10 1.42(2) . ? C7 C8 1.32(2) . ? C8 C9 1.34(2) . ? C9 C10 1.37(2) . ? C11 C15 1.400(10) . ? C11 C12 1.416(10) . ? C11 C22 1.490(9) . ? C12 C13 1.388(13) . ? C13 C14 1.42(2) . ? C14 C15 1.442(12) . ? C16 C20 1.373(12) . ? C16 C17 1.398(12) . ? C17 C18 1.424(13) . ? C18 C19 1.392(15) . ? C19 C20 1.434(13) . ? C23 C24 1.522(10) . ? C25 C26 1.500(10) . ? C27 C28 1.483(11) . ? C29 C30 1.479(11) . ? C31 C32 1.505(10) . ? P1 F2 1.533(7) . ? P1 F3 1.552(6) . ? P1 F4 1.568(6) . ? P1 F5 1.586(6) . ? P1 F6 1.593(6) . ? P1 F1 1.600(6) . ? P2 F10 1.35(2) . ? P2 F16 1.48(2) . ? P2 F13 1.487(14) . ? P2 F11 1.53(2) . ? P2 F8 1.531(7) . ? P2 F9 1.53(2) . ? P2 F7 1.546(8) . ? P2 F12 1.598(12) . ? P2 F15 1.61(2) . ? P2 F14 1.73(2) . ? C33 Cl2 1.40(2) . ? C33 Cl3 1.40(2) . ? C33 Cl1 1.78(2) . ? C33 Cl4 1.96(2) . ? 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 C6 Fe1 C8 66.1(6) . . ? C6 Fe1 C10 41.3(6) . . ? C8 Fe1 C10 66.6(6) . . ? C6 Fe1 C7 39.2(5) . . ? C8 Fe1 C7 38.1(6) . . ? C10 Fe1 C7 66.7(5) . . ? C6 Fe1 C2 161.9(7) . . ? C8 Fe1 C2 107.8(6) . . ? C10 Fe1 C2 154.2(8) . . ? C7 Fe1 C2 125.6(6) . . ? C6 Fe1 C4 121.8(8) . . ? C8 Fe1 C4 165.1(10) . . ? C10 Fe1 C4 110.0(6) . . ? C7 Fe1 C4 155.6(9) . . ? C2 Fe1 C4 68.5(6) . . ? C6 Fe1 C9 66.3(7) . . ? C8 Fe1 C9 38.7(6) . . ? C10 Fe1 C9 39.4(7) . . ? C7 Fe1 C9 64.3(6) . . ? C2 Fe1 C9 120.5(8) . . ? C4 Fe1 C9 129.6(9) . . ? C6 Fe1 C1 125.2(6) . . ? C8 Fe1 C1 118.6(8) . . ? C10 Fe1 C1 164.4(9) . . ? C7 Fe1 C1 107.7(4) . . ? C2 Fe1 C1 41.0(4) . . ? C4 Fe1 C1 68.8(4) . . ? C9 Fe1 C1 152.9(10) . . ? C6 Fe1 C3 155.5(8) . . ? C8 Fe1 C3 129.0(9) . . ? C10 Fe1 C3 121.0(7) . . ? C7 Fe1 C3 164.1(8) . . ? C2 Fe1 C3 41.5(5) . . ? C4 Fe1 C3 39.0(5) . . ? C9 Fe1 C3 111.7(6) . . ? C1 Fe1 C3 68.5(4) . . ? C6 Fe1 C5 108.5(5) . . ? C8 Fe1 C5 153.2(9) . . ? C10 Fe1 C5 127.9(8) . . ? C7 Fe1 C5 120.9(6) . . ? C2 Fe1 C5 68.7(5) . . ? C4 Fe1 C5 40.5(5) . . ? C9 Fe1 C5 165.7(10) . . ? C1 Fe1 C5 41.1(4) . . ? C3 Fe1 C5 67.0(5) . . ? C11 Fe2 C12 41.1(3) . . ? C11 Fe2 C20 124.8(4) . . ? C12 Fe2 C20 162.1(4) . . ? C11 Fe2 C16 106.9(3) . . ? C12 Fe2 C16 125.5(4) . . ? C20 Fe2 C16 39.7(3) . . ? C11 Fe2 C14 69.2(3) . . ? C12 Fe2 C14 68.4(4) . . ? C20 Fe2 C14 121.5(5) . . ? C16 Fe2 C14 155.5(5) . . ? C11 Fe2 C17 118.9(3) . . ? C12 Fe2 C17 107.1(4) . . ? C20 Fe2 C17 67.7(4) . . ? C16 Fe2 C17 40.2(3) . . ? C14 Fe2 C17 163.2(5) . . ? C11 Fe2 C19 163.4(5) . . ? C12 Fe2 C19 154.6(4) . . ? C20 Fe2 C19 41.4(4) . . ? C16 Fe2 C19 68.2(4) . . ? C14 Fe2 C19 108.2(4) . . ? C17 Fe2 C19 68.4(4) . . ? C11 Fe2 C18 154.6(5) . . ? C12 Fe2 C18 120.3(4) . . ? C20 Fe2 C18 67.9(4) . . ? C16 Fe2 C18 67.8(4) . . ? C14 Fe2 C18 126.1(4) . . ? C17 Fe2 C18 40.9(4) . . ? C19 Fe2 C18 40.0(4) . . ? C11 Fe2 C13 68.6(4) . . ? C12 Fe2 C13 40.0(4) . . ? C20 Fe2 C13 156.9(5) . . ? C16 Fe2 C13 162.2(5) . . ? C14 Fe2 C13 40.9(4) . . ? C17 Fe2 C13 125.5(5) . . ? C19 Fe2 C13 120.9(4) . . ? C18 Fe2 C13 108.4(4) . . ? C11 Fe2 C15 40.4(3) . . ? C12 Fe2 C15 68.3(4) . . ? C20 Fe2 C15 108.3(4) . . ? C16 Fe2 C15 119.9(3) . . ? C14 Fe2 C15 41.4(4) . . ? C17 Fe2 C15 153.7(4) . . ? C19 Fe2 C15 126.9(5) . . ? C18 Fe2 C15 164.0(4) . . ? C13 Fe2 C15 68.6(4) . . ? C26 N1 C21 114.3(6) . . ? C26 N1 C27 112.5(6) . . ? C21 N1 C27 110.0(6) . . ? C32 N2 C23 113.9(6) . . ? C32 N2 C22 113.4(5) . . ? C23 N2 C22 110.5(6) . . ? C24 O1 C25 113.6(6) . . ? C29 O2 C28 112.9(7) . . ? C30 O3 C31 114.1(6) . . ? C2 C1 C5 107.5(9) . . ? C2 C1 C21 127.0(9) . . ? C5 C1 C21 125.4(9) . . ? C2 C1 Fe1 69.4(5) . . ? C5 C1 Fe1 70.1(5) . . ? C21 C1 Fe1 123.6(6) . . ? C1 C2 C3 106.2(11) . . ? C1 C2 Fe1 69.6(5) . . ? C3 C2 Fe1 69.5(6) . . ? C4 C3 C2 109.6(12) . . ? C4 C3 Fe1 70.3(8) . . ? C2 C3 Fe1 69.1(6) . . ? C3 C4 C5 109.1(12) . . ? C3 C4 Fe1 70.7(8) . . ? C5 C4 Fe1 70.5(6) . . ? C4 C5 C1 107.6(11) . . ? C4 C5 Fe1 69.0(6) . . ? C1 C5 Fe1 68.8(5) . . ? C7 C6 C10 106.4(13) . . ? C7 C6 Fe1 70.9(7) . . ? C10 C6 Fe1 69.8(7) . . ? C8 C7 C6 110.4(14) . . ? C8 C7 Fe1 70.8(8) . . ? C6 C7 Fe1 69.9(7) . . ? C7 C8 C9 108.2(18) . . ? C7 C8 Fe1 71.1(7) . . ? C9 C8 Fe1 71.5(9) . . ? C10 C9 C8 109.6(17) . . ? C10 C9 Fe1 69.6(9) . . ? C8 C9 Fe1 69.7(8) . . ? C9 C10 C6 105.2(14) . . ? C9 C10 Fe1 71.1(8) . . ? C6 C10 Fe1 68.9(7) . . ? C15 C11 C12 108.2(7) . . ? C15 C11 C22 126.1(7) . . ? C12 C11 C22 125.7(7) . . ? C15 C11 Fe2 71.1(4) . . ? C12 C11 Fe2 70.0(4) . . ? C22 C11 Fe2 122.6(5) . . ? C13 C12 C11 108.8(9) . . ? C13 C12 Fe2 70.7(6) . . ? C11 C12 Fe2 68.8(4) . . ? C12 C13 C14 108.4(9) . . ? C12 C13 Fe2 69.4(5) . . ? C14 C13 Fe2 69.4(6) . . ? C13 C14 C15 106.9(8) . . ? C13 C14 Fe2 69.8(6) . . ? C15 C14 Fe2 69.6(4) . . ? C11 C15 C14 107.6(9) . . ? C11 C15 Fe2 68.4(4) . . ? C14 C15 Fe2 69.0(5) . . ? C20 C16 C17 109.4(8) . . ? C20 C16 Fe2 69.9(5) . . ? C17 C16 Fe2 70.3(5) . . ? C16 C17 C18 106.9(9) . . ? C16 C17 Fe2 69.4(5) . . ? C18 C17 Fe2 69.5(5) . . ? C19 C18 C17 108.7(9) . . ? C19 C18 Fe2 69.8(6) . . ? C17 C18 Fe2 69.6(5) . . ? C18 C19 C20 106.7(9) . . ? C18 C19 Fe2 70.2(6) . . ? C20 C19 Fe2 68.8(5) . . ? C16 C20 C19 108.4(9) . . ? C16 C20 Fe2 70.4(5) . . ? C19 C20 Fe2 69.7(5) . . ? C1 C21 N1 113.9(7) . . ? C11 C22 N2 114.8(5) . . ? N2 C23 C24 111.2(6) . . ? O1 C24 C23 106.8(6) . . ? O1 C25 C26 106.8(6) . . ? N1 C26 C25 112.0(7) . . ? C28 C27 N1 112.1(7) . . ? O2 C28 C27 109.7(7) . . ? O2 C29 C30 110.3(7) . . ? O3 C30 C29 108.2(7) . . ? O3 C31 C32 105.6(6) . . ? N2 C32 C31 111.2(6) . . ? F2 P1 F3 93.9(5) . . ? F2 P1 F4 96.3(5) . . ? F3 P1 F4 92.3(4) . . ? F2 P1 F5 88.7(4) . . ? F3 P1 F5 89.1(4) . . ? F4 P1 F5 174.8(4) . . ? F2 P1 F6 88.4(4) . . ? F3 P1 F6 177.5(4) . . ? F4 P1 F6 88.4(4) . . ? F5 P1 F6 90.0(4) . . ? F2 P1 F1 175.2(5) . . ? F3 P1 F1 89.0(4) . . ? F4 P1 F1 87.4(4) . . ? F5 P1 F1 87.6(4) . . ? F6 P1 F1 88.7(4) . . ? F10 P2 F13 95.3(15) . . ? F10 P2 F11 90.6(13) . . ? F13 P2 F11 173.0(15) . . ? F10 P2 F8 102.2(14) . . ? F16 P2 F8 100.5(16) . . ? F13 P2 F8 97.7(9) . . ? F11 P2 F8 84.5(9) . . ? F16 P2 F9 107.1(24) . . ? F8 P2 F9 80.2(15) . . ? F10 P2 F7 84.5(13) . . ? F16 P2 F7 75.3(16) . . ? F13 P2 F7 81.1(9) . . ? F11 P2 F7 95.9(9) . . ? F8 P2 F7 173.3(6) . . ? F9 P2 F7 95.9(14) . . ? F10 P2 F12 171.5(15) . . ? F13 P2 F12 85.3(10) . . ? F11 P2 F12 88.3(12) . . ? F8 P2 F12 86.1(8) . . ? F7 P2 F12 87.2(8) . . ? F16 P2 F15 91.1(23) . . ? F8 P2 F15 94.4(16) . . ? F9 P2 F15 161.6(21) . . ? F7 P2 F15 91.0(16) . . ? F16 P2 F14 169.2(25) . . ? F8 P2 F14 76.0(11) . . ? F9 P2 F14 82.6(17) . . ? F7 P2 F14 109.1(12) . . ? F15 P2 F14 79.1(15) . . ? Cl2 C33 Cl1 112.9(13) . . ? Cl3 C33 Cl4 108.3(13) . . ? _refine_diff_density_max 0.549 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.076 data_n2o2fc4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C50.50 H58 Cl F12 Fe4 N2 O2 P2' _chemical_formula_weight 1273.78 _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' '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' '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' 'Cl' 'Cl' 0.1484 0.1585 '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 13.956(3) _cell_length_b 14.524(2) _cell_length_c 16.619(2) _cell_angle_alpha 67.298(10) _cell_angle_beta 65.209(12) _cell_angle_gamma 69.930(13) _cell_volume 2754.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 47 _cell_measurement_theta_min 3.84 _cell_measurement_theta_max 11.94 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method ? _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 1.220 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5699 _exptl_absorpt_correction_T_max 0.5846 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.13 _diffrn_reflns_number 7444 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.2045 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 22.50 _reflns_number_total 7086 _reflns_number_observed 2801 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. 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^)+(0.1000P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7082 _refine_ls_number_parameters 665 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2466 _refine_ls_R_factor_obs 0.1017 _refine_ls_wR_factor_all 0.2815 _refine_ls_wR_factor_obs 0.2096 _refine_ls_goodness_of_fit_all 1.136 _refine_ls_goodness_of_fit_obs 1.439 _refine_ls_restrained_S_all 1.476 _refine_ls_restrained_S_obs 2.172 _refine_ls_shift/esd_max -13.477 _refine_ls_shift/esd_mean 0.169 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 0.5683(2) 0.7063(2) 0.1719(2) 0.0736(11) Uani 1 d . . Fe2 Fe 0.7074(2) 0.1161(2) 0.1042(2) 0.0555(9) Uani 1 d . . Fe3 Fe -0.0153(2) 0.6718(2) 0.2716(2) 0.0548(9) Uani 1 d . . Fe4 Fe 0.1026(3) 0.0581(2) 0.2760(2) 0.0754(11) Uani 1 d . . N1 N 0.6350(11) 0.3730(12) 0.2169(10) 0.055(4) Uani 1 d . . HN1 H 0.5644(11) 0.3819(12) 0.2243(10) 0.066 Uiso 1 calc R . N2 N 0.1385(11) 0.3523(10) 0.2690(9) 0.041(4) Uani 1 d . . HN2 H 0.1151(11) 0.3348(10) 0.3318(9) 0.049 Uiso 1 calc R . O1 O 0.4574(10) 0.3449(10) 0.3683(8) 0.062(4) Uani 1 d . . O2 O 0.2414(11) 0.3133(12) 0.3950(11) 0.083(4) Uani 1 d . . C1 C 0.5871(18) 0.5539(16) 0.2235(13) 0.065(6) Uani 1 d . . C2 C 0.4782(16) 0.6008(17) 0.2234(15) 0.079(7) Uani 1 d . . H2A H 0.4430(16) 0.5910(17) 0.1916(15) 0.095 Uiso 1 calc R . C3 C 0.4360(19) 0.6651(17) 0.2817(16) 0.090(8) Uani 1 d . . H3A H 0.3659(19) 0.7040(17) 0.2976(16) 0.108 Uiso 1 calc R . C4 C 0.5213(24) 0.6595(19) 0.3122(19) 0.102(9) Uani 1 d . . H4A H 0.5164(24) 0.6969(19) 0.3488(19) 0.123 Uiso 1 calc R . C5 C 0.6086(20) 0.5914(17) 0.2791(14) 0.075(7) Uani 1 d . . H5A H 0.6733(20) 0.5720(17) 0.2910(14) 0.090 Uiso 1 calc R . C6 C 0.5327(29) 0.8491(22) 0.1002(23) 0.141(13) Uani 1 d . . H6A H 0.4666(29) 0.8947(22) 0.1149(23) 0.169 Uiso 1 calc R . C7 C 0.6227(57) 0.8327(36) 0.1348(24) 0.236(31) Uani 1 d . . H7A H 0.6250(57) 0.8571(36) 0.1779(24) 0.283 Uiso 1 calc R . C8 C 0.6979(32) 0.7726(36) 0.0847(22) 0.166(22) Uani 1 d . . H8A H 0.7695(32) 0.7537(36) 0.0825(22) 0.199 Uiso 1 calc R . C9 C 0.6659(26) 0.7423(22) 0.0399(20) 0.119(11) Uani 1 d . . H9A H 0.7092(26) 0.6944(22) 0.0077(20) 0.142 Uiso 1 calc R . C10 C 0.5601(27) 0.7883(22) 0.0442(18) 0.100(8) Uani 1 d . . H10A H 0.5185(27) 0.7803(22) 0.0168(18) 0.120 Uiso 1 calc R . C11 C 0.6636(14) 0.2087(16) 0.1833(12) 0.054(5) Uani 1 d . . C12 C 0.7083(18) 0.1086(16) 0.2300(13) 0.072(6) Uani 1 d . . H12A H 0.7675(18) 0.0899(16) 0.2495(13) 0.087 Uiso 1 calc R . C13 C 0.6449(20) 0.0415(17) 0.2417(14) 0.081(7) Uani 1 d . . H13A H 0.6564(20) -0.0287(17) 0.2695(14) 0.097 Uiso 1 calc R . C14 C 0.5618(16) 0.1014(15) 0.2031(14) 0.064(6) Uani 1 d . . H14A H 0.5102(16) 0.0765(15) 0.2008(14) 0.077 Uiso 1 calc R . C15 C 0.5698(14) 0.2039(15) 0.1691(13) 0.059(5) Uani 1 d . . H15A H 0.5236(14) 0.2588(15) 0.1422(13) 0.070 Uiso 1 calc R . C16 C 0.8647(17) 0.0740(19) 0.0253(15) 0.082(7) Uani 1 d . . H16A H 0.9249(17) 0.0551(19) 0.0436(15) 0.098 Uiso 1 calc R . C17 C 0.8041(20) 0.0066(18) 0.0370(14) 0.078(7) Uani 1 d . . H17A H 0.8167(20) -0.0636(18) 0.0648(14) 0.093 Uiso 1 calc R . C18 C 0.7191(19) 0.0662(18) -0.0022(14) 0.080(7) Uani 1 d . . H18A H 0.6684(19) 0.0416(18) -0.0063(14) 0.096 Uiso 1 calc R . C19 C 0.7281(19) 0.1700(20) -0.0333(14) 0.083(7) Uani 1 d . . H19A H 0.6811(19) 0.2253(20) -0.0590(14) 0.099 Uiso 1 calc R . C20 C 0.8184(18) 0.1774(18) -0.0197(14) 0.075(7) Uani 1 d . . H20A H 0.8430(18) 0.2362(18) -0.0362(14) 0.090 Uiso 1 calc R . C21 C 0.0820(14) 0.5333(13) 0.2773(13) 0.049(5) Uani 1 d . . C22 C 0.0235(16) 0.5423(14) 0.3683(14) 0.057(6) Uani 1 d . . H22A H -0.0237(16) 0.5024(14) 0.4158(14) 0.068 Uiso 1 calc R . C23 C 0.0521(21) 0.6236(16) 0.3712(18) 0.081(7) Uani 1 d . . H23A H 0.0248(21) 0.6470(16) 0.4231(18) 0.097 Uiso 1 calc R . C25 C 0.1457(14) 0.6084(14) 0.2275(14) 0.059(6) Uani 1 d . . H25A H 0.1918(14) 0.6179(14) 0.1666(14) 0.071 Uiso 1 calc R . C24 C 0.1272(19) 0.6669(16) 0.2865(20) 0.083(8) Uani 1 d . . H24A H 0.1576(19) 0.7214(16) 0.2725(20) 0.100 Uiso 1 calc R . C26 C -0.0794(21) 0.8184(19) 0.2069(26) 0.097(9) Uani 1 d . . H26A H -0.0493(21) 0.8754(19) 0.1831(26) 0.117 Uiso 1 calc R . C27 C -0.0655(19) 0.7542(20) 0.1591(17) 0.083(8) Uani 1 d . . H27A H -0.0233(19) 0.7595(20) 0.0975(17) 0.100 Uiso 1 calc R . C28 C -0.1239(17) 0.6804(18) 0.2166(16) 0.072(7) Uani 1 d . . H28A H -0.1270(17) 0.6270(18) 0.2007(16) 0.086 Uiso 1 calc R . C29 C -0.1777(17) 0.6986(20) 0.3026(18) 0.083(7) Uani 1 d . . H29A H -0.2252(17) 0.6615(20) 0.3533(18) 0.099 Uiso 1 calc R . C30 C -0.1472(23) 0.7838(24) 0.2988(24) 0.104(10) Uani 1 d . . H30A H -0.1675(23) 0.8115(24) 0.3471(24) 0.124 Uiso 1 calc R . C31 C 0.1553(15) 0.1695(16) 0.2750(14) 0.052(5) Uani 1 d . . C32 C 0.2431(16) 0.1049(19) 0.2226(16) 0.077(7) Uani 1 d . . H32A H 0.2841(16) 0.1254(19) 0.1605(16) 0.092 Uiso 1 calc R . C33 C 0.2553(21) 0.0048(18) 0.2829(22) 0.093(8) Uani 1 d . . H33A H 0.3043(21) -0.0527(18) 0.2667(22) 0.111 Uiso 1 calc R . C34 C 0.1810(22) 0.0067(19) 0.3718(19) 0.090(8) Uani 1 d . . H34A H 0.1734(22) -0.0488(19) 0.4246(19) 0.108 Uiso 1 calc R . C35 C 0.1205(18) 0.1073(18) 0.3665(16) 0.071(6) Uani 1 d . . H35A H 0.0659(18) 0.1294(18) 0.4157(16) 0.085 Uiso 1 calc R . C36 C 0.0115(37) -0.0446(25) 0.3084(32) 0.146(15) Uani 1 d . . H36A H 0.0158(37) -0.1077(25) 0.3527(32) 0.175 Uiso 1 calc R . C37 C 0.0713(27) -0.0217(32) 0.2126(27) 0.133(14) Uani 1 d . . H37A H 0.1171(27) -0.0707(32) 0.1822(27) 0.160 Uiso 1 calc R . C38 C 0.0541(33) 0.0775(36) 0.1716(23) 0.127(12) Uani 1 d . . H38A H 0.0896(33) 0.1114(36) 0.1112(23) 0.153 Uiso 1 calc R . C39 C -0.0284(32) 0.1198(32) 0.2385(43) 0.142(17) Uani 1 d . . H39A H -0.0615(32) 0.1889(32) 0.2280(43) 0.170 Uiso 1 calc R . C40 C -0.0553(32) 0.0487(49) 0.3212(30) 0.160(23) Uani 1 d . . H40A H -0.1081(32) 0.0600(49) 0.3759(30) 0.192 Uiso 1 calc R . C41 C 0.6635(15) 0.4753(14) 0.1721(12) 0.056(5) Uani 1 d . . H41A H 0.6620(15) 0.4999(14) 0.1094(12) 0.068 Uiso 1 calc R . H41B H 0.7366(15) 0.4682(14) 0.1689(12) 0.068 Uiso 1 calc R . C42 C 0.7018(14) 0.3053(14) 0.1540(13) 0.058(5) Uani 1 d . . H42A H 0.7003(14) 0.3435(14) 0.0920(13) 0.069 Uiso 1 calc R . H42B H 0.7762(14) 0.2874(14) 0.1521(13) 0.069 Uiso 1 calc R . C43 C 0.6489(16) 0.3185(18) 0.3109(14) 0.078(7) Uani 1 d . . H43A H 0.6645(16) 0.2451(18) 0.3217(14) 0.094 Uiso 1 calc R . H43B H 0.7089(16) 0.3357(18) 0.3130(14) 0.094 Uiso 1 calc R . C44 C 0.5472(16) 0.3501(15) 0.3840(13) 0.060(6) Uani 1 d . . H44A H 0.5492(16) 0.3053(15) 0.4445(13) 0.072 Uiso 1 calc R . H44B H 0.5407(16) 0.4194(15) 0.3825(13) 0.072 Uiso 1 calc R . C45 C 0.3579(17) 0.3684(20) 0.4358(15) 0.095(8) Uani 1 d . . H45A H 0.3577(17) 0.4257(20) 0.4522(15) 0.114 Uiso 1 calc R . H45B H 0.3516(17) 0.3104(20) 0.4907(15) 0.114 Uiso 1 calc R . C46 C 0.2617(17) 0.3941(19) 0.4081(17) 0.093(8) Uani 1 d . . H46A H 0.1987(17) 0.4194(19) 0.4550(17) 0.112 Uiso 1 calc R . H46B H 0.2703(17) 0.4493(19) 0.3510(17) 0.112 Uiso 1 calc R . C47 C 0.3013(17) 0.2905(23) 0.3117(20) 0.119(11) Uani 1 d . . H47A H 0.3118(17) 0.2176(23) 0.3228(20) 0.143 Uiso 1 calc R . H47B H 0.3720(17) 0.3052(23) 0.2908(20) 0.143 Uiso 1 calc R . C48 C 0.2561(14) 0.3438(15) 0.2374(13) 0.059(6) Uani 1 d . . H48A H 0.2915(14) 0.3077(15) 0.1905(13) 0.071 Uiso 1 calc R . H48B H 0.2710(14) 0.4118(15) 0.2093(13) 0.071 Uiso 1 calc R . C49 C 0.0762(15) 0.4600(12) 0.2363(12) 0.054(5) Uani 1 d . . H49A H 0.1052(15) 0.4842(12) 0.1695(12) 0.065 Uiso 1 calc R . H49B H 0.0011(15) 0.4587(12) 0.2531(12) 0.065 Uiso 1 calc R . C50 C 0.1062(14) 0.2787(13) 0.2419(12) 0.046(5) Uani 1 d . . H50A H 0.0281(14) 0.2875(13) 0.2668(12) 0.055 Uiso 1 calc R . H50B H 0.1271(14) 0.2979(13) 0.1751(12) 0.055 Uiso 1 calc R . P1 P 0.0000 0.5000 0.0000 0.093(3) Uani 1 d S . F1 F -0.0116(31) 0.6053(21) -0.0072(25) 0.327(20) Uani 1 d . . F2 F 0.1080(12) 0.4687(22) 0.0175(10) 0.206(12) Uani 1 d . . F3 F -0.0615(12) 0.4784(20) 0.1037(10) 0.202(11) Uani 1 d . . P2 P 0.5000 0.5000 0.0000 0.057(2) Uani 1 d S . F6 F 0.4891(9) 0.4516(8) 0.1077(7) 0.072(3) Uani 1 d . . F4 F 0.3877(13) 0.5697(14) 0.0280(9) 0.168(8) Uani 1 d . . F5 F 0.4454(16) 0.4185(12) 0.0099(10) 0.153(7) Uani 1 d . . P3 P 0.8168(4) 0.3307(5) 0.4607(4) 0.058(2) Uani 1 d . . F7 F 0.8293(11) 0.3935(12) 0.3586(9) 0.133(6) Uani 1 d . . F8 F 0.8420(12) 0.2324(11) 0.4317(11) 0.139(6) Uani 1 d . . F9 F 0.7963(11) 0.4248(11) 0.4911(12) 0.134(6) Uani 1 d . . F10 F 0.6946(9) 0.3448(13) 0.4816(9) 0.122(5) Uani 1 d . . F11 F 0.8091(11) 0.2627(11) 0.5611(9) 0.118(5) Uani 1 d . . F12 F 0.9444(8) 0.3163(9) 0.4369(7) 0.081(4) Uani 1 d . . Cl2 Cl -0.4582(19) 0.0998(19) 0.5642(17) 0.228(10) Uiso 0.50 d PD . C60 C -0.5365(61) -0.0123(68) 0.5681(55) 0.264(52) Uiso 0.50 d PD . Cl1 Cl -0.6593(18) 0.0235(18) 0.5191(16) 0.237(9) Uiso 0.50 d PD . 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 0.076(2) 0.068(2) 0.087(3) -0.029(2) -0.026(2) -0.020(2) Fe2 0.052(2) 0.044(2) 0.059(2) -0.011(2) -0.018(2) -0.0022(14) Fe3 0.064(2) 0.046(2) 0.063(2) -0.006(2) -0.036(2) -0.015(2) Fe4 0.087(2) 0.063(2) 0.091(3) -0.043(2) -0.020(2) -0.020(2) N1 0.044(10) 0.069(12) 0.053(11) -0.016(10) -0.013(9) -0.018(9) N2 0.060(10) 0.038(9) 0.040(9) -0.001(7) -0.032(8) -0.022(8) O1 0.040(8) 0.095(10) 0.059(9) -0.038(8) -0.007(7) -0.020(7) O2 0.063(10) 0.098(12) 0.092(12) -0.020(10) -0.028(9) -0.027(9) C1 0.078(17) 0.075(16) 0.044(13) -0.018(12) -0.006(12) -0.038(13) C2 0.037(14) 0.099(19) 0.085(17) -0.038(15) 0.013(12) -0.025(13) C3 0.068(16) 0.080(19) 0.078(18) -0.043(15) 0.019(14) 0.004(14) C4 0.113(23) 0.072(19) 0.154(28) -0.071(19) -0.047(21) -0.011(17) C5 0.112(20) 0.060(16) 0.078(17) -0.025(13) -0.039(15) -0.032(15) C6 0.192(36) 0.075(21) 0.106(27) -0.051(20) -0.006(24) 0.002(21) C7 0.536(88) 0.224(45) 0.058(25) 0.011(25) -0.076(38) -0.297(55) C8 0.215(42) 0.286(57) 0.072(26) 0.034(26) -0.081(26) -0.197(43) C9 0.074(22) 0.112(24) 0.094(24) 0.001(18) 0.002(18) -0.004(19) C10 0.120(25) 0.098(22) 0.084(21) -0.004(17) -0.042(19) -0.041(19) C11 0.035(12) 0.079(17) 0.038(13) -0.014(12) -0.008(10) -0.008(11) C12 0.090(17) 0.060(15) 0.062(16) 0.010(13) -0.038(13) -0.027(14) C13 0.100(19) 0.055(15) 0.059(16) -0.003(12) -0.019(14) -0.007(15) C14 0.065(15) 0.039(13) 0.072(16) 0.005(12) -0.017(13) -0.024(12) C15 0.033(11) 0.060(15) 0.063(14) -0.022(11) 0.004(10) -0.006(10) C16 0.047(14) 0.083(18) 0.075(17) -0.014(14) -0.013(13) 0.014(14) C17 0.098(19) 0.069(17) 0.061(16) -0.018(13) -0.021(15) -0.020(16) C18 0.106(20) 0.061(17) 0.065(16) -0.006(13) -0.048(15) 0.004(15) C19 0.075(18) 0.088(21) 0.057(16) 0.000(14) -0.015(13) -0.017(15) C20 0.050(14) 0.078(19) 0.056(15) -0.014(14) 0.013(12) -0.009(13) C21 0.053(13) 0.045(13) 0.053(14) -0.007(11) -0.024(11) -0.015(10) C22 0.080(15) 0.050(14) 0.059(15) -0.006(11) -0.045(13) -0.018(12) C23 0.129(22) 0.056(15) 0.103(21) -0.026(14) -0.089(19) -0.004(15) C25 0.052(13) 0.043(13) 0.072(15) 0.012(12) -0.031(11) -0.016(11) C24 0.089(18) 0.046(15) 0.141(25) -0.024(16) -0.057(18) -0.024(13) C26 0.085(20) 0.052(17) 0.154(30) -0.012(20) -0.063(21) -0.003(15) C27 0.088(19) 0.065(17) 0.079(19) 0.021(16) -0.032(15) -0.037(15) C28 0.074(15) 0.097(19) 0.049(15) -0.018(15) -0.042(13) 0.000(15) C29 0.053(15) 0.110(22) 0.080(20) -0.015(16) -0.031(14) -0.015(14) C30 0.095(22) 0.113(24) 0.149(29) -0.093(23) -0.079(21) 0.036(18) C31 0.044(13) 0.067(16) 0.059(15) -0.022(13) -0.019(11) -0.022(12) C32 0.046(14) 0.085(19) 0.080(17) -0.034(16) 0.009(12) -0.017(13) C33 0.104(22) 0.046(17) 0.132(26) -0.029(17) -0.062(20) 0.013(15) C34 0.115(23) 0.065(20) 0.075(20) 0.012(15) -0.037(18) -0.031(17) C35 0.097(18) 0.063(16) 0.070(18) -0.039(14) -0.032(14) -0.009(15) C36 0.242(42) 0.113(27) 0.151(38) -0.060(26) -0.047(32) -0.116(30) C37 0.185(33) 0.147(36) 0.087(26) -0.062(24) 0.021(24) -0.107(30) C38 0.198(39) 0.129(32) 0.106(27) -0.015(28) -0.076(29) -0.084(32) C39 0.089(27) 0.174(41) 0.270(52) -0.166(45) -0.104(31) 0.020(26) C40 0.124(31) 0.281(68) 0.143(35) -0.117(41) 0.016(27) -0.136(42) C41 0.064(14) 0.066(15) 0.049(13) -0.011(12) -0.021(11) -0.029(12) C42 0.048(13) 0.059(14) 0.067(15) -0.019(12) -0.027(11) -0.001(11) C43 0.054(14) 0.122(20) 0.064(17) -0.030(15) -0.013(13) -0.028(14) C44 0.076(16) 0.062(14) 0.057(14) -0.002(11) -0.031(13) -0.037(12) C45 0.058(16) 0.167(26) 0.087(18) -0.083(18) -0.017(14) -0.015(16) C46 0.065(16) 0.124(23) 0.128(22) -0.077(18) -0.029(15) -0.019(15) C47 0.038(15) 0.212(33) 0.135(26) -0.114(25) -0.029(17) 0.016(17) C48 0.038(13) 0.078(16) 0.074(15) -0.026(12) -0.017(11) -0.023(11) C49 0.072(14) 0.031(11) 0.051(13) -0.002(10) -0.028(11) -0.003(10) C50 0.053(12) 0.043(12) 0.060(13) -0.028(10) -0.025(10) -0.008(10) P1 0.063(7) 0.153(12) 0.064(8) -0.055(7) -0.023(6) 0.006(7) F1 0.404(48) 0.170(23) 0.362(42) -0.132(26) -0.004(33) -0.102(29) F2 0.072(11) 0.429(38) 0.093(12) -0.072(16) -0.040(9) -0.014(16) F3 0.093(11) 0.452(35) 0.071(11) -0.099(16) -0.001(9) -0.077(16) P2 0.068(6) 0.049(5) 0.063(6) -0.024(4) -0.030(4) -0.003(4) F6 0.100(9) 0.068(8) 0.059(8) -0.014(6) -0.044(7) -0.012(7) F4 0.137(13) 0.187(17) 0.071(10) -0.028(10) -0.036(9) 0.087(13) F5 0.280(22) 0.143(14) 0.116(12) -0.003(10) -0.100(13) -0.135(15) P3 0.056(4) 0.074(4) 0.060(4) -0.031(4) -0.019(3) -0.018(3) F7 0.115(11) 0.192(16) 0.077(10) 0.036(10) -0.055(9) -0.073(11) F8 0.145(13) 0.124(13) 0.190(16) -0.094(12) -0.043(12) -0.037(10) F9 0.101(10) 0.119(12) 0.239(18) -0.119(13) -0.075(11) 0.011(9) F10 0.064(9) 0.235(17) 0.097(10) -0.074(11) -0.025(7) -0.038(10) F11 0.108(11) 0.138(13) 0.093(11) -0.011(10) -0.036(9) -0.032(10) F12 0.058(8) 0.119(10) 0.076(8) -0.042(7) -0.011(6) -0.029(7) _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 C6 1.96(3) . ? Fe1 C7 2.00(3) . ? Fe1 C1 2.01(2) . ? Fe1 C9 2.01(3) . ? Fe1 C2 2.02(2) . ? Fe1 C10 2.02(2) . ? Fe1 C4 2.03(3) . ? Fe1 C5 2.04(2) . ? Fe1 C3 2.05(2) . ? Fe1 C8 2.05(3) . ? Fe2 C11 2.01(2) . ? Fe2 C14 2.03(2) . ? Fe2 C19 2.03(2) . ? Fe2 C15 2.03(2) . ? Fe2 C16 2.05(2) . ? Fe2 C17 2.06(2) . ? Fe2 C13 2.05(2) . ? Fe2 C12 2.06(2) . ? Fe2 C20 2.07(2) . ? Fe2 C18 2.08(2) . ? Fe3 C21 2.00(2) . ? Fe3 C30 2.01(2) . ? Fe3 C23 2.02(2) . ? Fe3 C28 2.02(2) . ? Fe3 C29 2.03(2) . ? Fe3 C22 2.03(2) . ? Fe3 C25 2.04(2) . ? Fe3 C27 2.05(2) . ? Fe3 C26 2.05(2) . ? Fe3 C24 2.08(2) . ? Fe4 C31 1.99(2) . ? Fe4 C39 1.98(3) . ? Fe4 C38 2.01(3) . ? Fe4 C32 2.02(2) . ? Fe4 C35 2.02(2) . ? Fe4 C33 2.04(2) . ? Fe4 C40 2.05(3) . ? Fe4 C36 2.06(3) . ? Fe4 C34 2.07(2) . ? Fe4 C37 2.08(3) . ? N1 C41 1.49(2) . ? N1 C42 1.51(2) . ? N1 C43 1.52(2) . ? N2 C48 1.47(2) . ? N2 C49 1.52(2) . ? N2 C50 1.56(2) . ? O1 C45 1.40(2) . ? O1 C44 1.41(2) . ? O2 C47 1.39(2) . ? O2 C46 1.41(2) . ? C1 C5 1.40(2) . ? C1 C2 1.44(3) . ? C1 C41 1.52(2) . ? C2 C3 1.42(3) . ? C3 C4 1.45(3) . ? C4 C5 1.34(3) . ? C6 C10 1.38(4) . ? C6 C7 1.50(5) . ? C7 C8 1.32(6) . ? C8 C9 1.27(4) . ? C9 C10 1.38(3) . ? C11 C12 1.42(2) . ? C11 C15 1.45(2) . ? C11 C42 1.50(2) . ? C12 C13 1.44(3) . ? C13 C14 1.42(3) . ? C14 C15 1.40(2) . ? C16 C17 1.41(3) . ? C16 C20 1.45(3) . ? C17 C18 1.45(3) . ? C18 C19 1.43(3) . ? C19 C20 1.41(3) . ? C21 C25 1.42(2) . ? C21 C22 1.42(2) . ? C21 C49 1.51(2) . ? C22 C23 1.39(2) . ? C23 C24 1.42(3) . ? C25 C24 1.42(3) . ? C26 C27 1.36(3) . ? C26 C30 1.41(3) . ? C27 C28 1.37(3) . ? C28 C29 1.39(3) . ? C29 C30 1.41(3) . ? C31 C35 1.41(2) . ? C31 C32 1.45(2) . ? C31 C50 1.48(2) . ? C32 C33 1.41(3) . ? C33 C34 1.41(3) . ? C34 C35 1.40(3) . ? C36 C40 1.39(5) . ? C36 C37 1.42(4) . ? C37 C38 1.32(4) . ? C38 C39 1.38(4) . ? C39 C40 1.35(5) . ? C43 C44 1.50(2) . ? C45 C46 1.48(3) . ? C47 C48 1.45(3) . ? P1 F1 1.44(2) 2_565 ? P1 F1 1.44(2) . ? P1 F3 1.528(14) 2_565 ? P1 F3 1.528(14) . ? P1 F2 1.536(14) . ? P1 F2 1.536(14) 2_565 ? P2 F4 1.537(14) 2_665 ? P2 F4 1.537(14) . ? P2 F5 1.540(12) . ? P2 F5 1.540(12) 2_665 ? P2 F6 1.611(10) 2_665 ? P2 F6 1.611(10) . ? P3 F9 1.532(13) . ? P3 F10 1.545(12) . ? P3 F7 1.551(13) . ? P3 F11 1.557(14) . ? P3 F8 1.561(13) . ? P3 F12 1.609(11) . ? Cl2 C60 2.22(5) . ? Cl2 Cl1 2.41(3) 2_456 ? C60 C60 1.99(17) 2_456 ? C60 Cl1 2.03(5) . ? C60 Cl1 2.48(8) 2_456 ? Cl1 C60 2.48(8) 2_456 ? Cl1 Cl2 2.41(3) 2_456 ? 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 C6 Fe1 C7 44.5(16) . . ? C6 Fe1 C1 163.9(15) . . ? C7 Fe1 C1 149.4(21) . . ? C6 Fe1 C9 64.7(12) . . ? C7 Fe1 C9 66.4(14) . . ? C1 Fe1 C9 109.9(10) . . ? C6 Fe1 C2 126.7(14) . . ? C7 Fe1 C2 165.8(21) . . ? C1 Fe1 C2 41.8(8) . . ? C9 Fe1 C2 123.2(13) . . ? C6 Fe1 C10 40.4(11) . . ? C7 Fe1 C10 72.6(13) . . ? C1 Fe1 C10 125.5(11) . . ? C9 Fe1 C10 40.0(9) . . ? C2 Fe1 C10 107.4(10) . . ? C6 Fe1 C4 123.4(12) . . ? C7 Fe1 C4 104.9(11) . . ? C1 Fe1 C4 67.3(8) . . ? C9 Fe1 C4 159.2(14) . . ? C2 Fe1 C4 69.6(9) . . ? C10 Fe1 C4 158.4(13) . . ? C6 Fe1 C5 155.1(14) . . ? C7 Fe1 C5 115.1(16) . . ? C1 Fe1 C5 40.5(7) . . ? C9 Fe1 C5 126.1(12) . . ? C2 Fe1 C5 69.3(9) . . ? C10 Fe1 C5 162.2(12) . . ? C4 Fe1 C5 38.4(8) . . ? C6 Fe1 C3 110.9(11) . . ? C7 Fe1 C3 126.7(17) . . ? C1 Fe1 C3 68.1(8) . . ? C9 Fe1 C3 158.5(14) . . ? C2 Fe1 C3 40.8(8) . . ? C10 Fe1 C3 122.4(12) . . ? C4 Fe1 C3 41.5(9) . . ? C5 Fe1 C3 67.3(10) . . ? C6 Fe1 C8 64.4(17) . . ? C7 Fe1 C8 38.1(18) . . ? C1 Fe1 C8 121.2(16) . . ? C9 Fe1 C8 36.4(11) . . ? C2 Fe1 C8 155.4(15) . . ? C10 Fe1 C8 65.5(12) . . ? C4 Fe1 C8 125.9(12) . . ? C5 Fe1 C8 109.7(12) . . ? C3 Fe1 C8 163.2(15) . . ? C11 Fe2 C14 69.5(8) . . ? C11 Fe2 C19 122.6(9) . . ? C14 Fe2 C19 123.0(9) . . ? C11 Fe2 C15 42.1(7) . . ? C14 Fe2 C15 40.4(7) . . ? C19 Fe2 C15 107.4(9) . . ? C11 Fe2 C16 122.2(9) . . ? C14 Fe2 C16 158.9(9) . . ? C19 Fe2 C16 68.0(9) . . ? C15 Fe2 C16 159.6(9) . . ? C11 Fe2 C17 158.0(9) . . ? C14 Fe2 C17 122.9(9) . . ? C19 Fe2 C17 68.4(9) . . ? C15 Fe2 C17 158.6(9) . . ? C16 Fe2 C17 40.3(8) . . ? C11 Fe2 C13 69.1(8) . . ? C14 Fe2 C13 40.7(7) . . ? C19 Fe2 C13 159.1(10) . . ? C15 Fe2 C13 68.5(8) . . ? C16 Fe2 C13 123.0(9) . . ? C17 Fe2 C13 107.4(9) . . ? C11 Fe2 C12 40.9(7) . . ? C14 Fe2 C12 68.9(8) . . ? C19 Fe2 C12 158.7(9) . . ? C15 Fe2 C12 69.3(8) . . ? C16 Fe2 C12 107.3(9) . . ? C17 Fe2 C12 122.3(9) . . ? C13 Fe2 C12 41.0(7) . . ? C11 Fe2 C20 106.3(9) . . ? C14 Fe2 C20 158.4(9) . . ? C19 Fe2 C20 40.3(8) . . ? C15 Fe2 C20 122.4(8) . . ? C16 Fe2 C20 41.2(7) . . ? C17 Fe2 C20 68.9(9) . . ? C13 Fe2 C20 159.3(10) . . ? C12 Fe2 C20 122.5(9) . . ? C11 Fe2 C18 159.1(8) . . ? C14 Fe2 C18 107.7(9) . . ? C19 Fe2 C18 40.5(8) . . ? C15 Fe2 C18 122.4(9) . . ? C16 Fe2 C18 67.9(10) . . ? C17 Fe2 C18 40.8(8) . . ? C13 Fe2 C18 123.1(9) . . ? C12 Fe2 C18 159.0(9) . . ? C20 Fe2 C18 68.4(9) . . ? C21 Fe3 C30 161.3(12) . . ? C21 Fe3 C23 67.6(8) . . ? C30 Fe3 C23 109.2(10) . . ? C21 Fe3 C28 106.7(8) . . ? C30 Fe3 C28 68.1(9) . . ? C23 Fe3 C28 155.3(11) . . ? C21 Fe3 C29 123.7(9) . . ? C30 Fe3 C29 40.9(9) . . ? C23 Fe3 C29 121.5(11) . . ? C28 Fe3 C29 40.1(8) . . ? C21 Fe3 C22 41.3(7) . . ? C30 Fe3 C22 124.2(12) . . ? C23 Fe3 C22 40.3(7) . . ? C28 Fe3 C22 119.4(9) . . ? C29 Fe3 C22 106.1(9) . . ? C21 Fe3 C25 41.2(6) . . ? C30 Fe3 C25 156.3(12) . . ? C23 Fe3 C25 67.3(9) . . ? C28 Fe3 C25 125.3(9) . . ? C29 Fe3 C25 161.5(10) . . ? C22 Fe3 C25 69.3(8) . . ? C21 Fe3 C27 120.7(10) . . ? C30 Fe3 C27 67.4(10) . . ? C23 Fe3 C27 164.3(10) . . ? C28 Fe3 C27 39.4(7) . . ? C29 Fe3 C27 66.7(9) . . ? C22 Fe3 C27 154.6(10) . . ? C25 Fe3 C27 109.3(9) . . ? C21 Fe3 C26 155.3(12) . . ? C30 Fe3 C26 40.7(9) . . ? C23 Fe3 C26 128.8(11) . . ? C28 Fe3 C26 66.2(10) . . ? C29 Fe3 C26 67.2(10) . . ? C22 Fe3 C26 163.2(13) . . ? C25 Fe3 C26 121.9(10) . . ? C27 Fe3 C26 38.8(9) . . ? C21 Fe3 C24 69.0(8) . . ? C30 Fe3 C24 121.3(10) . . ? C23 Fe3 C24 40.4(8) . . ? C28 Fe3 C24 162.4(11) . . ? C29 Fe3 C24 156.4(11) . . ? C22 Fe3 C24 69.4(8) . . ? C25 Fe3 C24 40.4(7) . . ? C27 Fe3 C24 127.0(10) . . ? C26 Fe3 C24 110.2(10) . . ? C31 Fe4 C39 108.4(12) . . ? C31 Fe4 C38 119.0(13) . . ? C39 Fe4 C38 40.5(12) . . ? C31 Fe4 C32 42.3(7) . . ? C39 Fe4 C32 129.5(18) . . ? C38 Fe4 C32 108.5(12) . . ? C31 Fe4 C35 41.1(7) . . ? C39 Fe4 C35 119.8(13) . . ? C38 Fe4 C35 153.7(16) . . ? C32 Fe4 C35 68.9(9) . . ? C31 Fe4 C33 69.8(8) . . ? C39 Fe4 C33 166.9(20) . . ? C38 Fe4 C33 128.1(15) . . ? C32 Fe4 C33 40.7(8) . . ? C35 Fe4 C33 68.0(9) . . ? C31 Fe4 C40 126.1(16) . . ? C39 Fe4 C40 39.3(14) . . ? C38 Fe4 C40 68.1(14) . . ? C32 Fe4 C40 165.8(19) . . ? C35 Fe4 C40 107.6(12) . . ? C33 Fe4 C40 152.1(19) . . ? C31 Fe4 C36 163.4(15) . . ? C39 Fe4 C36 66.0(17) . . ? C38 Fe4 C36 67.8(13) . . ? C32 Fe4 C36 153.3(15) . . ? C35 Fe4 C36 126.4(14) . . ? C33 Fe4 C36 119.3(14) . . ? C40 Fe4 C36 39.7(14) . . ? C31 Fe4 C34 69.0(9) . . ? C39 Fe4 C34 152.4(18) . . ? C38 Fe4 C34 165.2(17) . . ? C32 Fe4 C34 68.2(9) . . ? C35 Fe4 C34 40.1(8) . . ? C33 Fe4 C34 40.2(8) . . ? C40 Fe4 C34 118.7(16) . . ? C36 Fe4 C34 108.2(12) . . ? C31 Fe4 C37 153.2(13) . . ? C39 Fe4 C37 63.4(14) . . ? C38 Fe4 C37 37.6(11) . . ? C32 Fe4 C37 121.2(11) . . ? C35 Fe4 C37 165.6(14) . . ? C33 Fe4 C37 112.0(13) . . ? C40 Fe4 C37 65.2(14) . . ? C36 Fe4 C37 40.1(10) . . ? C34 Fe4 C37 130.7(15) . . ? C41 N1 C42 109.5(14) . . ? C41 N1 C43 114.9(15) . . ? C42 N1 C43 108.9(15) . . ? C48 N2 C49 113.5(13) . . ? C48 N2 C50 113.9(13) . . ? C49 N2 C50 108.2(12) . . ? C45 O1 C44 113.9(14) . . ? C47 O2 C46 117.2(19) . . ? C5 C1 C2 108.7(20) . . ? C5 C1 C41 127.1(21) . . ? C2 C1 C41 124.2(19) . . ? C5 C1 Fe1 71.1(12) . . ? C2 C1 Fe1 69.4(12) . . ? C41 C1 Fe1 126.1(13) . . ? C3 C2 C1 105.4(21) . . ? C3 C2 Fe1 70.8(13) . . ? C1 C2 Fe1 68.7(11) . . ? C2 C3 C4 107.7(20) . . ? C2 C3 Fe1 68.5(11) . . ? C4 C3 Fe1 68.7(15) . . ? C5 C4 C3 108.7(21) . . ? C5 C4 Fe1 71.2(16) . . ? C3 C4 Fe1 69.8(15) . . ? C4 C5 C1 109.3(22) . . ? C4 C5 Fe1 70.4(16) . . ? C1 C5 Fe1 68.4(12) . . ? C10 C6 C7 111.7(33) . . ? C10 C6 Fe1 72.2(16) . . ? C7 C6 Fe1 69.2(20) . . ? C8 C7 C6 98.2(26) . . ? C8 C7 Fe1 73.0(23) . . ? C6 C7 Fe1 66.2(18) . . ? C9 C8 C7 115.7(45) . . ? C9 C8 Fe1 69.9(18) . . ? C7 C8 Fe1 68.9(23) . . ? C8 C9 C10 112.8(36) . . ? C8 C9 Fe1 73.7(21) . . ? C10 C9 Fe1 70.5(15) . . ? C6 C10 C9 100.9(29) . . ? C6 C10 Fe1 67.4(17) . . ? C9 C10 Fe1 69.4(16) . . ? C12 C11 C15 108.0(18) . . ? C12 C11 C42 127.8(17) . . ? C15 C11 C42 124.2(18) . . ? C12 C11 Fe2 71.4(12) . . ? C15 C11 Fe2 69.7(10) . . ? C42 C11 Fe2 125.5(13) . . ? C11 C12 C13 107.3(19) . . ? C11 C12 Fe2 67.7(11) . . ? C13 C12 Fe2 69.4(12) . . ? C14 C13 C12 107.9(19) . . ? C14 C13 Fe2 68.5(11) . . ? C12 C13 Fe2 69.6(11) . . ? C15 C14 C13 109.3(19) . . ? C15 C14 Fe2 70.0(10) . . ? C13 C14 Fe2 70.8(12) . . ? C14 C15 C11 107.4(18) . . ? C14 C15 Fe2 69.7(11) . . ? C11 C15 Fe2 68.2(10) . . ? C17 C16 C20 109.3(21) . . ? C17 C16 Fe2 70.2(12) . . ? C20 C16 Fe2 70.2(11) . . ? C16 C17 C18 107.7(21) . . ? C16 C17 Fe2 69.5(12) . . ? C18 C17 Fe2 70.6(13) . . ? C19 C18 C17 106.6(21) . . ? C19 C18 Fe2 67.9(13) . . ? C17 C18 Fe2 68.6(12) . . ? C20 C19 C18 110.5(22) . . ? C20 C19 Fe2 71.2(12) . . ? C18 C19 Fe2 71.6(12) . . ? C19 C20 C16 105.7(21) . . ? C19 C20 Fe2 68.5(11) . . ? C16 C20 Fe2 68.6(11) . . ? C25 C21 C22 109.1(17) . . ? C25 C21 C49 124.0(19) . . ? C22 C21 C49 126.9(16) . . ? C25 C21 Fe3 71.0(11) . . ? C22 C21 Fe3 70.6(11) . . ? C49 C21 Fe3 122.7(12) . . ? C23 C22 C21 105.2(19) . . ? C23 C22 Fe3 69.5(11) . . ? C21 C22 Fe3 68.1(10) . . ? C22 C23 C24 112.6(20) . . ? C22 C23 Fe3 70.2(11) . . ? C24 C23 Fe3 72.1(13) . . ? C21 C25 C24 108.6(19) . . ? C21 C25 Fe3 67.8(10) . . ? C24 C25 Fe3 71.3(12) . . ? C23 C24 C25 104.6(18) . . ? C23 C24 Fe3 67.5(12) . . ? C25 C24 Fe3 68.2(11) . . ? C27 C26 C30 108.6(24) . . ? C27 C26 Fe3 70.5(14) . . ? C30 C26 Fe3 68.1(14) . . ? C26 C27 C28 108.9(24) . . ? C26 C27 Fe3 70.7(15) . . ? C28 C27 Fe3 69.1(12) . . ? C27 C28 C29 108.7(23) . . ? C27 C28 Fe3 71.5(13) . . ? C29 C28 Fe3 70.3(12) . . ? C28 C29 C30 107.5(22) . . ? C28 C29 Fe3 69.6(12) . . ? C30 C29 Fe3 68.9(12) . . ? C29 C30 C26 106.1(23) . . ? C29 C30 Fe3 70.2(13) . . ? C26 C30 Fe3 71.2(14) . . ? C35 C31 C32 106.6(19) . . ? C35 C31 C50 124.8(19) . . ? C32 C31 C50 128.5(20) . . ? C35 C31 Fe4 70.9(11) . . ? C32 C31 Fe4 70.1(11) . . ? C50 C31 Fe4 122.4(12) . . ? C33 C32 C31 107.5(20) . . ? C33 C32 Fe4 70.3(13) . . ? C31 C32 Fe4 67.6(10) . . ? C34 C33 C32 108.6(21) . . ? C34 C33 Fe4 71.0(15) . . ? C32 C33 Fe4 69.0(12) . . ? C35 C34 C33 107.8(21) . . ? C35 C34 Fe4 68.3(13) . . ? C33 C34 Fe4 68.9(14) . . ? C34 C35 C31 109.4(21) . . ? C34 C35 Fe4 71.5(13) . . ? C31 C35 Fe4 68.0(11) . . ? C40 C36 C37 104.5(35) . . ? C40 C36 Fe4 69.6(16) . . ? C37 C36 Fe4 70.7(17) . . ? C38 C37 C36 111.9(32) . . ? C38 C37 Fe4 68.2(17) . . ? C36 C37 Fe4 69.2(15) . . ? C37 C38 C39 104.6(36) . . ? C37 C38 Fe4 74.2(19) . . ? C39 C38 Fe4 68.9(17) . . ? C40 C39 C38 112.0(42) . . ? C40 C39 Fe4 72.8(24) . . ? C38 C39 Fe4 70.7(18) . . ? C39 C40 C36 106.5(38) . . ? C39 C40 Fe4 67.9(18) . . ? C36 C40 Fe4 70.7(21) . . ? N1 C41 C1 112.9(14) . . ? C11 C42 N1 113.7(15) . . ? C44 C43 N1 109.3(16) . . ? O1 C44 C43 109.3(15) . . ? O1 C45 C46 115.0(17) . . ? O2 C46 C45 115.5(20) . . ? O2 C47 C48 116.6(19) . . ? C47 C48 N2 112.8(16) . . ? C21 C49 N2 112.4(14) . . ? C31 C50 N2 114.3(13) . . ? F1 P1 F1 180.000(2) 2_565 . ? F1 P1 F3 90.6(14) 2_565 2_565 ? F1 P1 F3 89.4(14) . 2_565 ? F1 P1 F3 89.4(14) 2_565 . ? F1 P1 F3 90.6(14) . . ? F3 P1 F3 180.000(2) 2_565 . ? F1 P1 F2 88.5(16) 2_565 . ? F1 P1 F2 91.5(16) . . ? F3 P1 F2 89.3(8) 2_565 . ? F3 P1 F2 90.7(8) . . ? F1 P1 F2 91.5(16) 2_565 2_565 ? F1 P1 F2 88.5(16) . 2_565 ? F3 P1 F2 90.7(8) 2_565 2_565 ? F3 P1 F2 89.3(8) . 2_565 ? F2 P1 F2 180.000(1) . 2_565 ? F4 P2 F4 180.000(2) 2_665 . ? F4 P2 F5 90.9(10) 2_665 . ? F4 P2 F5 89.1(10) . . ? F4 P2 F5 89.1(10) 2_665 2_665 ? F4 P2 F5 90.9(10) . 2_665 ? F5 P2 F5 180.000(2) . 2_665 ? F4 P2 F6 88.8(6) 2_665 2_665 ? F4 P2 F6 91.2(6) . 2_665 ? F5 P2 F6 91.0(6) . 2_665 ? F5 P2 F6 89.0(6) 2_665 2_665 ? F4 P2 F6 91.2(6) 2_665 . ? F4 P2 F6 88.8(6) . . ? F5 P2 F6 89.0(6) . . ? F5 P2 F6 91.0(6) 2_665 . ? F6 P2 F6 180.0 2_665 . ? F9 P3 F10 91.3(8) . . ? F9 P3 F7 93.5(10) . . ? F10 P3 F7 89.9(8) . . ? F9 P3 F11 89.1(9) . . ? F10 P3 F11 91.8(8) . . ? F7 P3 F11 176.8(10) . . ? F9 P3 F8 177.3(9) . . ? F10 P3 F8 90.8(8) . . ? F7 P3 F8 88.1(9) . . ? F11 P3 F8 89.2(9) . . ? F9 P3 F12 89.2(7) . . ? F10 P3 F12 179.0(7) . . ? F7 P3 F12 89.2(7) . . ? F11 P3 F12 89.1(7) . . ? F8 P3 F12 88.8(7) . . ? C60 Cl2 Cl1 64.6(27) . 2_456 ? C60 C60 Cl2 89.4(33) 2_456 . ? C60 C60 Cl1 76.2(28) 2_456 . ? Cl2 C60 Cl1 125.1(42) . . ? C60 C60 Cl1 52.5(31) 2_456 2_456 ? Cl2 C60 Cl1 61.4(17) . 2_456 ? Cl1 C60 Cl1 128.6(36) . 2_456 ? C60 Cl1 C60 51.4(36) . 2_456 ? C60 Cl1 Cl2 83.6(30) . 2_456 ? C60 Cl1 Cl2 54.0(18) 2_456 2_456 ? _refine_diff_density_max 1.200 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.106 data_n2o2cu1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum ; 'C44.80 H60.80 F19.20 Fe3.20 N3.20 O3.20 P3.20' ; _chemical_formula_weight 1337.99 _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' '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' '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' _symmetry_cell_setting Orthorrombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 41.858(8) _cell_length_b 9.543(3) _cell_length_c 16.801(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6711.5(29) _cell_formula_units_Z 5 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method ? _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4389 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1115 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4389 _reflns_number_observed 2211 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. 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^)+(0.1000P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4387 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1548 _refine_ls_R_factor_obs 0.0655 _refine_ls_wR_factor_all 0.2021 _refine_ls_wR_factor_obs 0.1453 _refine_ls_goodness_of_fit_all 0.956 _refine_ls_goodness_of_fit_obs 1.021 _refine_ls_restrained_S_all 0.964 _refine_ls_restrained_S_obs 1.021 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.19659(3) -0.44660(15) 0.69231(8) 0.0323(4) Uani 1 d . . Fe2 Fe 0.18173(4) 0.0468(2) 0.43935(9) 0.0387(4) Uani 1 d . . N1 N 0.0931(2) -0.4375(9) 0.6494(5) 0.040(2) Uani 1 d . . H1A H 0.0925(2) -0.3671(9) 0.6851(5) 0.048 Uiso 1 calc R . H1B H 0.0909(2) -0.3999(9) 0.6006(5) 0.048 Uiso 1 calc R . N2 N 0.0802(2) -0.0648(9) 0.4087(5) 0.044(2) Uani 1 d . . H2A H 0.0795(2) -0.1277(9) 0.4486(5) 0.053 Uiso 1 calc R . H2C H 0.0844(2) -0.1118(9) 0.3635(5) 0.053 Uiso 1 calc R . O1 O 0.0310(2) -0.4029(8) 0.5833(4) 0.053(2) Uani 1 d . . O2 O 0.0233(2) -0.1650(8) 0.4782(5) 0.054(2) Uani 1 d . . C1 C 0.1518(2) -0.4062(10) 0.6533(6) 0.036(3) Uani 1 d . . C2 C 0.1743(2) -0.3849(11) 0.5903(6) 0.043(3) Uani 1 d . . H2B H 0.1748(2) -0.4332(11) 0.5389(6) 0.051 Uiso 1 calc R . C3 C 0.1959(3) -0.2809(11) 0.6171(7) 0.045(3) Uani 1 d . . H3A H 0.2143(3) -0.2454(11) 0.5871(7) 0.055 Uiso 1 calc R . C4 C 0.1870(2) -0.2380(11) 0.6949(7) 0.049(3) Uani 1 d . . H4A H 0.1980(2) -0.1679(11) 0.7275(7) 0.059 Uiso 1 calc R . C5 C 0.1599(2) -0.3146(10) 0.7173(7) 0.039(3) Uani 1 d . . H6B H 0.1486(2) -0.3075(10) 0.7683(7) 0.047 Uiso 1 calc R . C6 C 0.1998(3) -0.6551(12) 0.7172(8) 0.055(3) Uani 1 d . . H6A H 0.1835(3) -0.7267(12) 0.7067(8) 0.066 Uiso 1 calc R . C7 C 0.2242(3) -0.6146(12) 0.6670(8) 0.054(3) Uani 1 d . . H7A H 0.2279(3) -0.6522(12) 0.6135(8) 0.065 Uiso 1 calc R . C8 C 0.2426(2) -0.5098(12) 0.7033(7) 0.053(3) Uani 1 d . . H8A H 0.2615(2) -0.4635(12) 0.6806(7) 0.064 Uiso 1 calc R . C9 C 0.2294(3) -0.4851(13) 0.7782(7) 0.059(3) Uani 1 d . . H9A H 0.2372(3) -0.4170(13) 0.8172(7) 0.071 Uiso 1 calc R . C10 C 0.2029(3) -0.5717(13) 0.7877(7) 0.060(4) Uani 1 d . . H10A H 0.1891(3) -0.5761(13) 0.8347(7) 0.072 Uiso 1 calc R . C11 C 0.1385(2) -0.0294(10) 0.4078(6) 0.034(2) Uani 1 d . . C12 C 0.1570(2) -0.0090(11) 0.3398(6) 0.042(3) Uani 1 d . . H12A H 0.1516(2) 0.0538(11) 0.2956(6) 0.050 Uiso 1 calc R . C13 C 0.1853(3) -0.0886(11) 0.3461(7) 0.049(3) Uani 1 d . . H13A H 0.2026(3) -0.0925(11) 0.3070(7) 0.059 Uiso 1 calc R . C14 C 0.1838(3) -0.1630(11) 0.4194(7) 0.052(3) Uani 1 d . . H14A H 0.2000(3) -0.2276(11) 0.4401(7) 0.062 Uiso 1 calc R . C15 C 0.1547(2) -0.1261(10) 0.4575(6) 0.037(3) Uani 1 d . . H15A H 0.1473(2) -0.1609(10) 0.5091(6) 0.045 Uiso 1 calc R . C16 C 0.1744(3) 0.2175(13) 0.5086(8) 0.065(4) Uani 1 d . . H16A H 0.1535(3) 0.2544(13) 0.5245(8) 0.078 Uiso 1 calc R . C17 C 0.1916(3) 0.2572(11) 0.4400(9) 0.061(4) Uani 1 d . . H17A H 0.1847(3) 0.3255(11) 0.4000(9) 0.073 Uiso 1 calc R . C18 C 0.2199(3) 0.1775(13) 0.4379(8) 0.061(3) Uani 1 d . . H18A H 0.2364(3) 0.1816(13) 0.3964(8) 0.073 Uiso 1 calc R . C19 C 0.2209(3) 0.0947(13) 0.5059(9) 0.072(4) Uani 1 d . . H19A H 0.2381(3) 0.0293(13) 0.5195(9) 0.086 Uiso 1 calc R . C20 C 0.1923(3) 0.1150(13) 0.5510(8) 0.066(4) Uani 1 d . . H20A H 0.1865(3) 0.0701(13) 0.6014(8) 0.079 Uiso 1 calc R . C21 C 0.1251(2) -0.5094(10) 0.6547(6) 0.037(3) Uani 1 d . . H21A H 0.1261(2) -0.5634(10) 0.7035(6) 0.045 Uiso 1 calc R . H21B H 0.1274(2) -0.5737(10) 0.6104(6) 0.045 Uiso 1 calc R . C22 C 0.0661(2) -0.5339(11) 0.6647(6) 0.047(3) Uani 1 d . . H22A H 0.0686(2) -0.5770(11) 0.7166(6) 0.057 Uiso 1 calc R . H22B H 0.0660(2) -0.6077(11) 0.6250(6) 0.057 Uiso 1 calc R . C23 C 0.0348(2) -0.4548(13) 0.6616(6) 0.053(3) Uani 1 d . . H23A H 0.0173(2) -0.5166(13) 0.6751(6) 0.063 Uiso 1 calc R . H23B H 0.0351(2) -0.3779(13) 0.6994(6) 0.063 Uiso 1 calc R . C24 C 0.0025(2) -0.3233(11) 0.5720(8) 0.058(4) Uani 1 d . . H24A H 0.0022(2) -0.2444(11) 0.6084(8) 0.070 Uiso 1 calc R . H24B H -0.0160(2) -0.3813(11) 0.5832(8) 0.070 Uiso 1 calc R . C25 C 0.0010(3) -0.2721(12) 0.4889(8) 0.058(3) Uani 1 d . . H25A H 0.0056(3) -0.3485(12) 0.4525(8) 0.070 Uiso 1 calc R . H25B H -0.0203(3) -0.2374(12) 0.4774(8) 0.070 Uiso 1 calc R . C26 C 0.0220(3) -0.1038(13) 0.4029(7) 0.059(3) Uani 1 d . . H26A H 0.0015(3) -0.0591(13) 0.3945(7) 0.071 Uiso 1 calc R . H26B H 0.0252(3) -0.1738(13) 0.3619(7) 0.071 Uiso 1 calc R . C27 C 0.0480(2) 0.0013(12) 0.4012(7) 0.053(3) Uani 1 d . . H27A H 0.0450(2) 0.0673(12) 0.4445(7) 0.063 Uiso 1 calc R . H27B H 0.0470(2) 0.0531(12) 0.3516(7) 0.063 Uiso 1 calc R . C28 C 0.1067(2) 0.0354(11) 0.4242(6) 0.044(3) Uani 1 d . . H28A H 0.1058(2) 0.0654(11) 0.4793(6) 0.053 Uiso 1 calc R . H28B H 0.1040(2) 0.1175(11) 0.3909(6) 0.053 Uiso 1 calc R . P1 P 0.08164(8) -0.0091(3) 0.6653(2) 0.0534(9) Uani 1 d . . P2 P 0.40428(7) 0.0182(3) 0.4037(2) 0.0452(8) Uani 1 d . . F1 F 0.0465(2) -0.0565(10) 0.6839(5) 0.111(3) Uani 1 d . . F2 F 0.1167(2) 0.0357(11) 0.6494(5) 0.118(3) Uani 1 d . . F3 F 0.0929(2) -0.1235(8) 0.7278(4) 0.089(2) Uani 1 d . . F4 F 0.0692(2) 0.1019(8) 0.6037(5) 0.110(3) Uani 1 d . . F5 F 0.0792(2) 0.1020(8) 0.7349(4) 0.108(3) Uani 1 d . . F6 F 0.0845(2) -0.1227(8) 0.5960(4) 0.099(3) Uani 1 d . . F7 F 0.3691(2) -0.0208(10) 0.4236(5) 0.115(3) Uani 1 d . . F8 F 0.4392(2) 0.0613(9) 0.3826(5) 0.102(3) Uani 1 d . . F9 F 0.4040(2) 0.1321(7) 0.4743(4) 0.075(2) Uani 1 d . . F10 F 0.4049(2) -0.0928(7) 0.3328(4) 0.086(2) Uani 1 d . . F11 F 0.4172(2) -0.0966(8) 0.4640(4) 0.109(3) Uani 1 d . . F12 F 0.3922(2) 0.1340(8) 0.3444(4) 0.092(3) 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 0.0320(8) 0.0325(8) 0.0323(9) 0.0028(7) -0.0017(7) 0.0038(7) Fe2 0.0484(9) 0.0322(9) 0.0354(9) -0.0041(8) -0.0044(7) 0.0003(7) N1 0.033(5) 0.045(6) 0.042(5) 0.003(5) 0.002(4) -0.004(4) N2 0.045(5) 0.042(5) 0.046(6) 0.004(5) -0.003(4) 0.008(5) O1 0.039(4) 0.071(5) 0.048(5) 0.001(4) 0.003(4) 0.006(4) O2 0.043(5) 0.059(5) 0.058(6) 0.000(4) -0.002(4) -0.014(4) C1 0.041(6) 0.029(6) 0.037(6) 0.007(5) -0.011(5) 0.001(5) C2 0.040(6) 0.063(8) 0.024(6) 0.022(6) -0.002(5) -0.003(6) C3 0.047(7) 0.039(7) 0.050(8) 0.023(6) -0.004(6) -0.008(6) C4 0.039(7) 0.045(7) 0.063(9) -0.005(7) -0.004(6) -0.002(5) C5 0.024(6) 0.039(6) 0.055(7) -0.003(6) 0.002(5) 0.005(5) C6 0.059(9) 0.037(7) 0.069(9) 0.006(7) -0.026(8) 0.010(6) C7 0.044(7) 0.055(8) 0.062(9) -0.006(7) 0.000(7) 0.012(6) C8 0.033(6) 0.062(8) 0.063(9) 0.001(7) 0.002(6) 0.016(6) C9 0.058(8) 0.069(9) 0.051(8) 0.002(7) -0.016(7) 0.017(7) C10 0.069(9) 0.058(8) 0.053(9) 0.035(7) 0.004(7) 0.019(7) C11 0.040(6) 0.028(6) 0.035(6) 0.001(5) -0.005(5) -0.005(5) C12 0.059(7) 0.041(6) 0.026(6) -0.002(5) 0.003(6) -0.014(6) C13 0.056(8) 0.050(7) 0.043(8) -0.022(6) 0.014(6) -0.004(6) C14 0.067(8) 0.033(6) 0.055(9) -0.017(6) 0.002(7) 0.007(6) C15 0.054(7) 0.028(6) 0.029(6) -0.001(5) -0.002(5) 0.003(5) C16 0.075(9) 0.059(9) 0.062(9) -0.036(8) -0.002(8) 0.015(7) C17 0.076(9) 0.021(6) 0.085(11) -0.010(7) -0.004(9) 0.001(6) C18 0.063(9) 0.052(8) 0.068(10) -0.017(8) -0.009(7) -0.010(7) C19 0.067(9) 0.055(9) 0.094(12) -0.010(9) -0.044(9) 0.013(7) C20 0.087(10) 0.055(8) 0.055(9) -0.025(7) -0.013(8) -0.006(8) C21 0.031(6) 0.038(6) 0.042(7) 0.001(5) 0.001(5) 0.001(5) C22 0.048(7) 0.053(7) 0.042(7) 0.004(6) -0.003(5) -0.023(6) C23 0.034(6) 0.081(9) 0.043(7) -0.002(7) 0.004(5) -0.005(6) C24 0.020(6) 0.054(7) 0.100(11) -0.006(8) -0.001(7) 0.007(6) C25 0.039(7) 0.062(8) 0.073(10) 0.001(7) -0.006(7) 0.011(6) C26 0.049(8) 0.074(9) 0.054(9) 0.007(7) -0.009(6) -0.003(7) C27 0.052(7) 0.063(8) 0.044(7) 0.000(6) 0.001(6) 0.030(7) C28 0.060(7) 0.038(7) 0.034(7) -0.002(6) -0.004(6) 0.001(6) P1 0.064(2) 0.060(2) 0.036(2) -0.002(2) -0.010(2) 0.008(2) P2 0.050(2) 0.052(2) 0.034(2) -0.0024(15) -0.0036(14) -0.006(2) F1 0.072(5) 0.162(9) 0.098(7) 0.008(6) -0.006(5) -0.014(5) F2 0.084(6) 0.175(10) 0.097(7) -0.010(7) 0.012(5) -0.037(6) F3 0.108(6) 0.096(6) 0.061(5) 0.026(4) -0.015(4) 0.027(5) F4 0.170(8) 0.097(7) 0.062(5) 0.022(5) -0.006(5) 0.053(6) F5 0.195(9) 0.080(6) 0.048(5) -0.026(4) 0.012(5) 0.003(6) F6 0.151(7) 0.084(6) 0.061(5) -0.021(5) -0.002(5) 0.014(5) F7 0.073(5) 0.164(9) 0.109(7) -0.025(6) 0.021(5) -0.056(6) F8 0.063(5) 0.131(7) 0.112(7) -0.027(6) 0.014(5) -0.029(5) F9 0.112(6) 0.068(5) 0.045(4) -0.009(4) -0.004(4) 0.011(4) F10 0.139(7) 0.062(5) 0.057(5) -0.019(4) -0.006(5) 0.001(4) F11 0.188(9) 0.076(6) 0.063(5) 0.013(4) -0.034(6) 0.027(6) F12 0.144(7) 0.077(5) 0.055(5) 0.007(4) -0.025(5) 0.031(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 C10 2.017(11) . ? Fe1 C7 2.022(11) . ? Fe1 C1 2.024(9) . ? Fe1 C3 2.024(10) . ? Fe1 C9 2.025(11) . ? Fe1 C8 2.028(10) . ? Fe1 C5 2.031(9) . ? Fe1 C4 2.032(11) . ? Fe1 C6 2.037(11) . ? Fe1 C2 2.037(9) . ? Fe2 C15 2.022(10) . ? Fe2 C11 2.023(9) . ? Fe2 C16 2.026(11) . ? Fe2 C18 2.029(12) . ? Fe2 C14 2.032(10) . ? Fe2 C20 2.034(12) . ? Fe2 C13 2.036(10) . ? Fe2 C19 2.037(11) . ? Fe2 C12 2.038(10) . ? Fe2 C17 2.050(11) . ? N1 C22 1.480(11) . ? N1 C21 1.507(11) . ? N2 C28 1.488(12) . ? N2 C27 1.491(11) . ? O1 C23 1.415(12) . ? O1 C24 1.429(11) . ? O2 C26 1.394(13) . ? O2 C25 1.396(13) . ? C1 C5 1.427(13) . ? C1 C2 1.432(13) . ? C1 C21 1.489(13) . ? C2 C3 1.416(13) . ? C3 C4 1.420(15) . ? C4 C5 1.402(13) . ? C6 C7 1.38(2) . ? C6 C10 1.43(2) . ? C7 C8 1.402(15) . ? C8 C9 1.40(2) . ? C9 C10 1.39(2) . ? C11 C12 1.394(13) . ? C11 C15 1.420(13) . ? C11 C28 1.493(13) . ? C12 C13 1.411(14) . ? C13 C14 1.424(15) . ? C14 C15 1.417(14) . ? C16 C17 1.41(2) . ? C16 C20 1.42(2) . ? C17 C18 1.411(15) . ? C18 C19 1.39(2) . ? C19 C20 1.43(2) . ? C22 C23 1.512(14) . ? C24 C25 1.48(2) . ? C26 C27 1.481(14) . ? P1 F2 1.552(8) . ? P1 F1 1.570(8) . ? P1 F4 1.570(8) . ? P1 F5 1.582(7) . ? P1 F3 1.587(7) . ? P1 F6 1.596(8) . ? P2 F7 1.556(7) . ? P2 F8 1.558(7) . ? P2 F12 1.573(7) . ? P2 F11 1.585(7) . ? P2 F10 1.595(7) . ? P2 F9 1.609(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 C10 Fe1 C7 67.8(5) . . ? C10 Fe1 C1 119.5(5) . . ? C7 Fe1 C1 127.8(5) . . ? C10 Fe1 C3 163.9(5) . . ? C7 Fe1 C3 119.7(5) . . ? C1 Fe1 C3 68.7(4) . . ? C10 Fe1 C9 40.2(5) . . ? C7 Fe1 C9 67.6(5) . . ? C1 Fe1 C9 153.3(5) . . ? C3 Fe1 C9 126.6(5) . . ? C10 Fe1 C8 68.1(5) . . ? C7 Fe1 C8 40.5(4) . . ? C1 Fe1 C8 165.2(5) . . ? C3 Fe1 C8 107.6(5) . . ? C9 Fe1 C8 40.3(4) . . ? C10 Fe1 C5 107.6(5) . . ? C7 Fe1 C5 165.5(4) . . ? C1 Fe1 C5 41.2(4) . . ? C3 Fe1 C5 68.6(4) . . ? C9 Fe1 C5 118.5(5) . . ? C8 Fe1 C5 152.2(5) . . ? C10 Fe1 C4 126.1(5) . . ? C7 Fe1 C4 153.4(5) . . ? C1 Fe1 C4 68.7(4) . . ? C3 Fe1 C4 41.0(4) . . ? C9 Fe1 C4 107.2(5) . . ? C8 Fe1 C4 118.5(5) . . ? C5 Fe1 C4 40.4(4) . . ? C10 Fe1 C6 41.4(4) . . ? C7 Fe1 C6 39.8(4) . . ? C1 Fe1 C6 108.2(4) . . ? C3 Fe1 C6 153.1(5) . . ? C9 Fe1 C6 68.4(5) . . ? C8 Fe1 C6 68.2(5) . . ? C5 Fe1 C6 127.8(5) . . ? C4 Fe1 C6 164.9(5) . . ? C10 Fe1 C2 154.1(5) . . ? C7 Fe1 C2 108.3(5) . . ? C1 Fe1 C2 41.3(4) . . ? C3 Fe1 C2 40.8(4) . . ? C9 Fe1 C2 164.1(5) . . ? C8 Fe1 C2 126.7(4) . . ? C5 Fe1 C2 69.4(4) . . ? C4 Fe1 C2 69.2(5) . . ? C6 Fe1 C2 119.0(5) . . ? C15 Fe2 C11 41.1(4) . . ? C15 Fe2 C16 119.0(5) . . ? C11 Fe2 C16 107.7(5) . . ? C15 Fe2 C18 160.7(5) . . ? C11 Fe2 C18 157.5(5) . . ? C16 Fe2 C18 68.4(5) . . ? C15 Fe2 C14 40.9(4) . . ? C11 Fe2 C14 68.9(4) . . ? C16 Fe2 C14 153.3(6) . . ? C18 Fe2 C14 124.8(5) . . ? C15 Fe2 C20 104.1(5) . . ? C11 Fe2 C20 123.4(5) . . ? C16 Fe2 C20 41.0(5) . . ? C18 Fe2 C20 69.1(5) . . ? C14 Fe2 C20 117.3(5) . . ? C15 Fe2 C13 68.9(4) . . ? C11 Fe2 C13 68.6(4) . . ? C16 Fe2 C13 164.4(5) . . ? C18 Fe2 C13 108.9(5) . . ? C14 Fe2 C13 41.0(4) . . ? C20 Fe2 C13 153.8(5) . . ? C15 Fe2 C19 123.4(5) . . ? C11 Fe2 C19 161.1(6) . . ? C16 Fe2 C19 68.1(5) . . ? C18 Fe2 C19 40.0(5) . . ? C14 Fe2 C19 106.2(5) . . ? C20 Fe2 C19 41.2(5) . . ? C13 Fe2 C19 120.4(5) . . ? C15 Fe2 C12 68.1(4) . . ? C11 Fe2 C12 40.1(4) . . ? C16 Fe2 C12 127.1(5) . . ? C18 Fe2 C12 123.5(5) . . ? C14 Fe2 C12 68.2(5) . . ? C20 Fe2 C12 161.9(5) . . ? C13 Fe2 C12 40.5(4) . . ? C19 Fe2 C12 156.7(6) . . ? C15 Fe2 C17 155.5(5) . . ? C11 Fe2 C17 122.2(4) . . ? C16 Fe2 C17 40.5(5) . . ? C18 Fe2 C17 40.5(4) . . ? C14 Fe2 C17 163.3(5) . . ? C20 Fe2 C17 68.8(5) . . ? C13 Fe2 C17 127.7(5) . . ? C19 Fe2 C17 67.4(5) . . ? C12 Fe2 C17 111.2(5) . . ? C22 N1 C21 112.7(8) . . ? C28 N2 C27 114.6(8) . . ? C23 O1 C24 113.8(8) . . ? C26 O2 C25 113.4(9) . . ? C5 C1 C2 108.3(9) . . ? C5 C1 C21 124.8(9) . . ? C2 C1 C21 126.9(10) . . ? C5 C1 Fe1 69.7(5) . . ? C2 C1 Fe1 69.9(5) . . ? C21 C1 Fe1 124.3(7) . . ? C3 C2 C1 106.6(10) . . ? C3 C2 Fe1 69.1(6) . . ? C1 C2 Fe1 68.9(5) . . ? C2 C3 C4 109.0(10) . . ? C2 C3 Fe1 70.1(5) . . ? C4 C3 Fe1 69.8(6) . . ? C5 C4 C3 108.1(10) . . ? C5 C4 Fe1 69.8(6) . . ? C3 C4 Fe1 69.2(6) . . ? C4 C5 C1 108.0(10) . . ? C4 C5 Fe1 69.8(6) . . ? C1 C5 Fe1 69.1(6) . . ? C7 C6 C10 106.3(11) . . ? C7 C6 Fe1 69.5(7) . . ? C10 C6 Fe1 68.5(6) . . ? C6 C7 C8 109.9(11) . . ? C6 C7 Fe1 70.7(6) . . ? C8 C7 Fe1 70.0(6) . . ? C9 C8 C7 107.1(11) . . ? C9 C8 Fe1 69.7(6) . . ? C7 C8 Fe1 69.5(6) . . ? C10 C9 C8 108.7(11) . . ? C10 C9 Fe1 69.6(6) . . ? C8 C9 Fe1 70.0(6) . . ? C9 C10 C6 108.0(11) . . ? C9 C10 Fe1 70.2(6) . . ? C6 C10 Fe1 70.1(6) . . ? C12 C11 C15 107.8(9) . . ? C12 C11 C28 126.1(9) . . ? C15 C11 C28 126.0(9) . . ? C12 C11 Fe2 70.5(6) . . ? C15 C11 Fe2 69.4(5) . . ? C28 C11 Fe2 126.9(7) . . ? C11 C12 C13 109.3(10) . . ? C11 C12 Fe2 69.3(6) . . ? C13 C12 Fe2 69.7(6) . . ? C12 C13 C14 107.2(10) . . ? C12 C13 Fe2 69.8(6) . . ? C14 C13 Fe2 69.3(6) . . ? C15 C14 C13 107.7(10) . . ? C15 C14 Fe2 69.2(6) . . ? C13 C14 Fe2 69.7(6) . . ? C14 C15 C11 107.9(9) . . ? C14 C15 Fe2 69.9(6) . . ? C11 C15 Fe2 69.5(5) . . ? C17 C16 C20 109.0(12) . . ? C17 C16 Fe2 70.7(6) . . ? C20 C16 Fe2 69.8(7) . . ? C16 C17 C18 107.7(12) . . ? C16 C17 Fe2 68.8(7) . . ? C18 C17 Fe2 68.9(6) . . ? C19 C18 C17 108.1(12) . . ? C19 C18 Fe2 70.4(7) . . ? C17 C18 Fe2 70.6(7) . . ? C18 C19 C20 109.5(11) . . ? C18 C19 Fe2 69.7(7) . . ? C20 C19 Fe2 69.3(7) . . ? C16 C20 C19 105.6(12) . . ? C16 C20 Fe2 69.2(7) . . ? C19 C20 Fe2 69.5(7) . . ? C1 C21 N1 111.4(8) . . ? N1 C22 C23 110.2(9) . . ? O1 C23 C22 107.7(8) . . ? O1 C24 C25 109.6(10) . . ? O2 C25 C24 109.6(10) . . ? O2 C26 C27 105.8(9) . . ? C26 C27 N2 112.1(9) . . ? N2 C28 C11 111.5(8) . . ? F2 P1 F1 178.2(5) . . ? F2 P1 F4 90.9(5) . . ? F1 P1 F4 90.8(5) . . ? F2 P1 F5 90.2(5) . . ? F1 P1 F5 89.2(5) . . ? F4 P1 F5 90.8(4) . . ? F2 P1 F3 91.2(5) . . ? F1 P1 F3 87.1(5) . . ? F4 P1 F3 177.9(5) . . ? F5 P1 F3 89.5(4) . . ? F2 P1 F6 89.4(5) . . ? F1 P1 F6 91.2(5) . . ? F4 P1 F6 90.1(4) . . ? F5 P1 F6 179.0(5) . . ? F3 P1 F6 89.6(4) . . ? F7 P2 F8 178.3(6) . . ? F7 P2 F12 90.0(5) . . ? F8 P2 F12 88.3(5) . . ? F7 P2 F11 91.1(5) . . ? F8 P2 F11 90.5(5) . . ? F12 P2 F11 178.7(5) . . ? F7 P2 F10 91.0(5) . . ? F8 P2 F10 89.4(4) . . ? F12 P2 F10 89.9(4) . . ? F11 P2 F10 90.7(4) . . ? F7 P2 F9 89.8(4) . . ? F8 P2 F9 89.8(4) . . ? F12 P2 F9 89.4(4) . . ? F11 P2 F9 89.9(4) . . ? F10 P2 F9 178.9(4) . . ? _refine_diff_density_max 0.375 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.080