# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _audit_creation_date 10-03-06 _publ_contact_author_name 'Prof. Pierre Braunstein' _publ_contact_author_address ; Institut Le Bel, rue Blaise Pascal, 67000 STRASBOURG, FRANCE ; _publ_contact_author_phone 0390241308 _publ_contact_author_fax 0390241322 _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_contact_letter ; ; _publ_requested_category FM _publ_section_title ; Nickel and iron complexes with N,P,N-type ligands: synthesis, structure and catalytic oligomerization of ethylene ; loop_ _publ_author_name _publ_author_address A.Kermagoret ; Laboratoire de Chimie de coordination, UMR CNRS 7177 Universit\'e Louis Pasteur Strasbourg France ; F.Tomicki ; Laboratoire de Chimie de coordination, UMR CNRS 7177 Universit\'e Louis Pasteur Strasbourg France ; P.Braunstein ; Laboratoire de Chimie de coordination, UMR CNRS 7177 Universit\'e Louis Pasteur Strasbourg France ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Dowty, E. (1994). ATOMS for Mac. Version 3.0. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, E-U. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. Spek, A.L., PLATON 98, Utrecht University, The Netherland, 1998. ; data_kerma_fepyrid _database_code_depnum_ccdc_archive 'CCDC 676912' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H34 Fe N4 P2, 1/2(C H2 Cl2), Fe2 O Cl6' _chemical_formula_sum 'C36.50 H35 Cl7 Fe3 N4 O P2' _chemical_formula_weight 1023.33 _chemical_absolute_configuration . 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' P P 0.1023 0.0942 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 12.6010(3) _cell_length_b 16.6710(5) _cell_length_c 20.3170(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4268.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6260 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 29.131 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2068 _exptl_absorpt_coefficient_mu 1.555 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9257 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4894 _reflns_number_gt 3202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+14.1864P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4894 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1464 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.1681 _refine_ls_wR_factor_gt 0.1510 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.2500 0.2500 0.18208(5) 0.0311(3) Uani 1 2 d S . . Fe2 Fe 0.24991(8) 0.64745(5) 0.14198(4) 0.0450(3) Uani 1 1 d . . . Cl1 Cl 0.17540(13) 0.57985(10) 0.22427(8) 0.0573(4) Uani 1 1 d . . . Cl2 Cl 0.41695(14) 0.60715(13) 0.13180(9) 0.0696(5) Uani 1 1 d . . . Cl3 Cl 0.16518(16) 0.62300(14) 0.04820(10) 0.0777(6) Uani 1 1 d . . . Cl4 Cl 0.6956(4) 0.3226(4) 0.1256(3) 0.125(2) Uani 0.50 1 d P . . P P 0.15362(12) 0.18295(8) 0.25107(7) 0.0337(3) Uani 1 1 d . . . O1 O 0.2500 0.7500 0.1613(4) 0.077(2) Uani 1 2 d S . . N1 N 0.1531(4) 0.1897(3) 0.1143(2) 0.0367(11) Uani 1 1 d . . . N2 N 0.1276(4) 0.3284(2) 0.1794(2) 0.0334(10) Uani 1 1 d . . . C1 C 0.1824(5) 0.1426(3) 0.3321(3) 0.0347(13) Uani 1 1 d . . . C2 C 0.2813(5) 0.1096(4) 0.3449(3) 0.0469(16) Uani 1 1 d . . . H2 H 0.3349 0.1112 0.3121 0.056 Uiso 1 1 calc . . . C3 C 0.3023(6) 0.0744(4) 0.4051(3) 0.0583(18) Uani 1 1 d . . . H3 H 0.3704 0.0523 0.4136 0.070 Uiso 1 1 calc . . . C4 C 0.2253(6) 0.0714(4) 0.4525(3) 0.0505(17) Uani 1 1 d . . . H4 H 0.2399 0.0468 0.4937 0.061 Uiso 1 1 calc . . . C5 C 0.1274(5) 0.1037(4) 0.4407(3) 0.0464(15) Uani 1 1 d . . . H5 H 0.0741 0.1015 0.4738 0.056 Uiso 1 1 calc . . . C6 C 0.1056(5) 0.1396(4) 0.3807(3) 0.0404(14) Uani 1 1 d . . . H6 H 0.0375 0.1622 0.3729 0.049 Uiso 1 1 calc . . . C7 C 0.1154(5) 0.0946(3) 0.2031(3) 0.0435(14) Uani 1 1 d . . . H7A H 0.1729 0.0542 0.2031 0.052 Uiso 1 1 calc . . . H7B H 0.0503 0.0698 0.2213 0.052 Uiso 1 1 calc . . . C8 C 0.0958(5) 0.1256(3) 0.1345(3) 0.0467(16) Uani 1 1 d . . . C9 C 0.0168(8) 0.0941(5) 0.0960(4) 0.093(3) Uani 1 1 d . . . H9 H -0.0237 0.0498 0.1112 0.112 Uiso 1 1 calc . . . C10 C -0.0038(8) 0.1270(5) 0.0347(4) 0.100(3) Uani 1 1 d . . . H10 H -0.0558 0.1038 0.0067 0.121 Uiso 1 1 calc . . . C11 C 0.0509(7) 0.1924(4) 0.0153(4) 0.073(2) Uani 1 1 d . . . H11 H 0.0361 0.2174 -0.0257 0.087 Uiso 1 1 calc . . . C12 C 0.1281(5) 0.2218(4) 0.0560(3) 0.0457(15) Uani 1 1 d . . . H12 H 0.1663 0.2679 0.0420 0.055 Uiso 1 1 calc . . . C13 C 0.0342(5) 0.2438(4) 0.2598(3) 0.0447(14) Uani 1 1 d . . . H13A H -0.0293 0.2099 0.2529 0.054 Uiso 1 1 calc . . . H13B H 0.0308 0.2663 0.3048 0.054 Uiso 1 1 calc . . . C14 C 0.0350(5) 0.3110(3) 0.2103(3) 0.0388(13) Uani 1 1 d . . . C15 C -0.0563(5) 0.3547(4) 0.1980(3) 0.0507(16) Uani 1 1 d . . . H15 H -0.1207 0.3404 0.2194 0.061 Uiso 1 1 calc . . . C16 C -0.0548(6) 0.4182(4) 0.1558(3) 0.0560(17) Uani 1 1 d . . . H16 H -0.1175 0.4482 0.1473 0.067 Uiso 1 1 calc . . . C17 C 0.0386(6) 0.4376(4) 0.1258(3) 0.0510(17) Uani 1 1 d . . . H17 H 0.0424 0.4823 0.0969 0.061 Uiso 1 1 calc . . . C18 C 0.1267(5) 0.3922(3) 0.1380(3) 0.0420(14) Uani 1 1 d . . . H18 H 0.1909 0.4061 0.1163 0.050 Uiso 1 1 calc . . . C19 C 0.7500 0.2500 0.0840(14) 0.101(8) Uiso 0.50 2 d SP . . H19A H 0.6950 0.2264 0.0551 0.122 Uiso 0.25 1 calc P . . H19B H 0.8050 0.2736 0.0551 0.122 Uiso 0.25 1 calc P . . 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 0.0372(6) 0.0234(5) 0.0328(5) 0.000 0.000 -0.0018(5) Fe2 0.0477(5) 0.0309(4) 0.0564(5) -0.0008(4) 0.0083(5) -0.0018(4) Cl1 0.0514(10) 0.0546(10) 0.0658(10) 0.0087(8) 0.0145(8) -0.0019(8) Cl2 0.0486(10) 0.0853(14) 0.0750(12) 0.0078(10) 0.0193(9) 0.0075(10) Cl3 0.0705(13) 0.0959(16) 0.0667(12) 0.0003(11) -0.0036(10) -0.0194(11) Cl4 0.073(3) 0.122(5) 0.181(6) 0.006(4) -0.030(4) -0.004(3) P 0.0373(8) 0.0257(7) 0.0381(7) 0.0007(6) 0.0004(6) -0.0037(6) O1 0.107(6) 0.031(3) 0.092(5) 0.000 0.000 0.004(4) N1 0.047(3) 0.030(2) 0.033(2) -0.004(2) -0.003(2) 0.000(2) N2 0.040(3) 0.025(2) 0.035(2) -0.002(2) -0.001(2) -0.003(2) C1 0.048(4) 0.024(3) 0.032(3) 0.000(2) 0.003(3) -0.008(3) C2 0.047(4) 0.045(4) 0.049(4) 0.016(3) 0.017(3) 0.011(3) C3 0.063(4) 0.053(4) 0.059(4) 0.019(3) 0.005(4) 0.016(4) C4 0.068(5) 0.040(3) 0.043(3) 0.005(3) 0.001(3) -0.008(3) C5 0.045(4) 0.053(4) 0.041(3) -0.001(3) 0.006(3) -0.010(3) C6 0.036(3) 0.046(4) 0.039(3) -0.001(3) 0.001(3) -0.003(3) C7 0.051(4) 0.029(3) 0.051(3) -0.002(3) -0.001(3) -0.009(3) C8 0.062(4) 0.032(3) 0.046(3) 0.000(3) -0.013(3) -0.005(3) C9 0.135(8) 0.062(5) 0.083(6) 0.020(4) -0.057(6) -0.054(5) C10 0.138(8) 0.078(6) 0.086(6) 0.011(5) -0.068(6) -0.044(6) C11 0.107(7) 0.055(5) 0.056(4) 0.005(4) -0.032(4) -0.008(5) C12 0.061(4) 0.037(3) 0.040(3) -0.002(3) -0.005(3) -0.001(3) C13 0.043(3) 0.039(3) 0.052(3) 0.006(3) 0.007(3) -0.001(3) C14 0.043(3) 0.034(3) 0.040(3) -0.004(3) -0.007(3) 0.000(3) C15 0.039(4) 0.054(4) 0.060(4) 0.005(3) 0.002(3) 0.005(3) C16 0.056(4) 0.049(4) 0.064(4) 0.008(3) -0.006(3) 0.015(3) C17 0.066(5) 0.037(4) 0.050(4) 0.011(3) -0.006(3) 0.006(3) C18 0.050(4) 0.031(3) 0.044(3) 0.002(3) -0.001(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.022(4) 2 ? Fe1 N2 2.022(4) . ? Fe1 N1 2.097(4) . ? Fe1 N1 2.098(4) 2 ? Fe1 P 2.1654(16) 2 ? Fe1 P 2.1655(15) . ? Fe2 O1 1.7542(19) . ? Fe2 Cl2 2.219(2) . ? Fe2 Cl3 2.222(2) . ? Fe2 Cl1 2.2243(18) . ? Cl4 C19 1.628(16) . ? P C1 1.816(5) . ? P C13 1.823(6) . ? P C7 1.831(6) . ? O1 Fe2 1.7543(19) 2_565 ? N1 C12 1.337(7) . ? N1 C8 1.355(7) . ? N2 C18 1.356(7) . ? N2 C14 1.356(7) . ? C1 C6 1.384(8) . ? C1 C2 1.386(8) . ? C2 C3 1.381(8) . ? C2 H2 0.9500 . ? C3 C4 1.368(9) . ? C3 H3 0.9500 . ? C4 C5 1.367(9) . ? C4 H4 0.9500 . ? C5 C6 1.386(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.506(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.370(9) . ? C9 C10 1.384(11) . ? C9 H9 0.9500 . ? C10 C11 1.348(11) . ? C10 H10 0.9500 . ? C11 C12 1.368(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.506(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.385(8) . ? C15 C16 1.363(9) . ? C15 H15 0.9500 . ? C16 C17 1.364(9) . ? C16 H16 0.9500 . ? C17 C18 1.367(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 Cl4 1.628(16) 2_655 ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N2 176.9(2) 2 . ? N2 Fe1 N1 96.67(18) 2 . ? N2 Fe1 N1 81.26(17) . . ? N2 Fe1 N1 81.26(17) 2 2 ? N2 Fe1 N1 96.66(18) . 2 ? N1 Fe1 N1 97.9(3) . 2 ? N2 Fe1 P 85.62(13) 2 2 ? N2 Fe1 P 96.42(13) . 2 ? N1 Fe1 P 177.50(13) . 2 ? N1 Fe1 P 81.46(13) 2 2 ? N2 Fe1 P 96.42(12) 2 . ? N2 Fe1 P 85.62(13) . . ? N1 Fe1 P 81.46(13) . . ? N1 Fe1 P 177.50(13) 2 . ? P Fe1 P 99.33(9) 2 . ? O1 Fe2 Cl2 108.38(7) . . ? O1 Fe2 Cl3 111.8(2) . . ? Cl2 Fe2 Cl3 108.68(9) . . ? O1 Fe2 Cl1 109.0(2) . . ? Cl2 Fe2 Cl1 108.48(8) . . ? Cl3 Fe2 Cl1 110.41(8) . . ? C1 P C13 106.4(3) . . ? C1 P C7 103.8(3) . . ? C13 P C7 106.4(3) . . ? C1 P Fe1 131.77(19) . . ? C13 P Fe1 103.80(19) . . ? C7 P Fe1 102.61(19) . . ? Fe2 O1 Fe2 154.1(5) . 2_565 ? C12 N1 C8 117.3(5) . . ? C12 N1 Fe1 121.8(4) . . ? C8 N1 Fe1 119.3(4) . . ? C18 N2 C14 116.6(5) . . ? C18 N2 Fe1 122.0(4) . . ? C14 N2 Fe1 120.4(4) . . ? C6 C1 C2 118.7(5) . . ? C6 C1 P 121.4(5) . . ? C2 C1 P 119.8(4) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 120.2(6) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 120.1(6) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.2(6) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 120.3(5) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 P 105.1(4) . . ? C8 C7 H7A 110.7 . . ? P C7 H7A 110.7 . . ? C8 C7 H7B 110.7 . . ? P C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? N1 C8 C9 121.1(6) . . ? N1 C8 C7 117.6(5) . . ? C9 C8 C7 121.1(6) . . ? C8 C9 C10 119.9(7) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 119.2(7) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 118.5(6) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? N1 C12 C11 124.0(6) . . ? N1 C12 H12 118.0 . . ? C11 C12 H12 118.0 . . ? C14 C13 P 110.1(4) . . ? C14 C13 H13A 109.6 . . ? P C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? P C13 H13B 109.6 . . ? H13A C13 H13B 108.2 . . ? N2 C14 C15 121.3(5) . . ? N2 C14 C13 118.3(5) . . ? C15 C14 C13 120.4(5) . . ? C16 C15 C14 120.7(6) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 118.5(6) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C16 C17 C18 119.3(6) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? N2 C18 C17 123.6(6) . . ? N2 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? Cl4 C19 Cl4 117.4(18) 2_655 . ? Cl4 C19 H19A 107.9 2_655 . ? Cl4 C19 H19A 107.9 . . ? Cl4 C19 H19B 107.9 2_655 . ? Cl4 C19 H19B 107.9 . . ? H19A C19 H19B 107.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 P C1 53.5(3) 2 . . . ? N2 Fe1 P C1 -128.9(3) . . . . ? N1 Fe1 P C1 149.3(3) . . . . ? N1 Fe1 P C1 75(3) 2 . . . ? P Fe1 P C1 -33.1(2) 2 . . . ? N2 Fe1 P C13 -179.0(2) 2 . . . ? N2 Fe1 P C13 -1.4(2) . . . . ? N1 Fe1 P C13 -83.2(2) . . . . ? N1 Fe1 P C13 -157(3) 2 . . . ? P Fe1 P C13 94.4(2) 2 . . . ? N2 Fe1 P C7 -68.3(2) 2 . . . ? N2 Fe1 P C7 109.3(2) . . . . ? N1 Fe1 P C7 27.5(2) . . . . ? N1 Fe1 P C7 -47(3) 2 . . . ? P Fe1 P C7 -154.9(2) 2 . . . ? Cl2 Fe2 O1 Fe2 88.61(10) . . . 2_565 ? Cl3 Fe2 O1 Fe2 -31.16(8) . . . 2_565 ? Cl1 Fe2 O1 Fe2 -153.50(8) . . . 2_565 ? N2 Fe1 N1 C12 -114.7(5) 2 . . . ? N2 Fe1 N1 C12 62.9(5) . . . . ? N1 Fe1 N1 C12 -32.7(4) 2 . . . ? P Fe1 N1 C12 41(3) 2 . . . ? P Fe1 N1 C12 149.7(5) . . . . ? N2 Fe1 N1 C8 79.9(5) 2 . . . ? N2 Fe1 N1 C8 -102.5(5) . . . . ? N1 Fe1 N1 C8 162.0(5) 2 . . . ? P Fe1 N1 C8 -124(3) 2 . . . ? P Fe1 N1 C8 -15.6(4) . . . . ? N2 Fe1 N2 C18 -44.4(4) 2 . . . ? N1 Fe1 N2 C18 -93.1(4) . . . . ? N1 Fe1 N2 C18 3.9(4) 2 . . . ? P Fe1 N2 C18 86.0(4) 2 . . . ? P Fe1 N2 C18 -175.1(4) . . . . ? N2 Fe1 N2 C14 123.6(4) 2 . . . ? N1 Fe1 N2 C14 74.9(4) . . . . ? N1 Fe1 N2 C14 171.9(4) 2 . . . ? P Fe1 N2 C14 -106.0(4) 2 . . . ? P Fe1 N2 C14 -7.1(4) . . . . ? C13 P C1 C6 19.1(5) . . . . ? C7 P C1 C6 -92.9(5) . . . . ? Fe1 P C1 C6 145.8(4) . . . . ? C13 P C1 C2 -164.9(5) . . . . ? C7 P C1 C2 83.1(5) . . . . ? Fe1 P C1 C2 -38.2(6) . . . . ? C6 C1 C2 C3 0.0(9) . . . . ? P C1 C2 C3 -176.1(5) . . . . ? C1 C2 C3 C4 0.4(11) . . . . ? C2 C3 C4 C5 -0.5(11) . . . . ? C3 C4 C5 C6 0.1(10) . . . . ? C2 C1 C6 C5 -0.4(9) . . . . ? P C1 C6 C5 175.7(4) . . . . ? C4 C5 C6 C1 0.4(9) . . . . ? C1 P C7 C8 -177.4(4) . . . . ? C13 P C7 C8 70.5(5) . . . . ? Fe1 P C7 C8 -38.2(4) . . . . ? C12 N1 C8 C9 1.3(10) . . . . ? Fe1 N1 C8 C9 167.3(7) . . . . ? C12 N1 C8 C7 -173.5(5) . . . . ? Fe1 N1 C8 C7 -7.5(7) . . . . ? P C7 C8 N1 30.8(7) . . . . ? P C7 C8 C9 -144.0(7) . . . . ? N1 C8 C9 C10 1.3(14) . . . . ? C7 C8 C9 C10 176.0(9) . . . . ? C8 C9 C10 C11 -3.4(16) . . . . ? C9 C10 C11 C12 2.7(15) . . . . ? C8 N1 C12 C11 -2.0(9) . . . . ? Fe1 N1 C12 C11 -167.7(6) . . . . ? C10 C11 C12 N1 0.0(12) . . . . ? C1 P C13 C14 150.4(4) . . . . ? C7 P C13 C14 -99.4(4) . . . . ? Fe1 P C13 C14 8.4(4) . . . . ? C18 N2 C14 C15 2.3(8) . . . . ? Fe1 N2 C14 C15 -166.3(5) . . . . ? C18 N2 C14 C13 -176.3(5) . . . . ? Fe1 N2 C14 C13 15.1(7) . . . . ? P C13 C14 N2 -15.0(6) . . . . ? P C13 C14 C15 166.5(5) . . . . ? N2 C14 C15 C16 -1.8(9) . . . . ? C13 C14 C15 C16 176.7(6) . . . . ? C14 C15 C16 C17 -0.1(10) . . . . ? C15 C16 C17 C18 1.4(10) . . . . ? C14 N2 C18 C17 -0.9(8) . . . . ? Fe1 N2 C18 C17 167.4(5) . . . . ? C16 C17 C18 N2 -0.9(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.687 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.086 # Attachment 'cif_FeOx2_11.cif' data_kerma_feox2 _database_code_depnum_ccdc_archive 'CCDC 676913' _audit_creation_date 10-03-06 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 Fe N4 O5 P2, 4(C2 H3 N), Fe2 Cl6 O' _chemical_formula_sum 'C36 H46 Cl6 Fe3 N8 O5 P2' _chemical_formula_weight 1113.00 _chemical_absolute_configuration . 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' P P 0.1023 0.0942 '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' 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 C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.3270(7) _cell_length_b 21.8930(12) _cell_length_c 15.4880(9) _cell_angle_alpha 90.00 _cell_angle_beta 110.368(2) _cell_angle_gamma 90.00 _cell_volume 4872.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6590 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 1.323 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12328 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7114 _reflns_number_gt 5370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+4.8417P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7114 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 0.346081(18) 0.2500 0.02233(10) Uani 1 2 d S . . Fe2 Fe 0.39922(2) 0.133776(14) 0.27738(2) 0.03321(9) Uani 1 1 d . . . Cl1 Cl 0.37786(5) 0.05726(3) 0.36310(4) 0.04886(16) Uani 1 1 d . . . Cl2 Cl 0.41128(5) 0.21857(3) 0.35971(5) 0.05718(19) Uani 1 1 d . . . Cl3 Cl 0.27481(5) 0.14031(3) 0.15039(4) 0.05134(17) Uani 1 1 d . . . P P 0.10833(4) 0.27949(2) 0.31781(4) 0.02697(12) Uani 1 1 d . . . O1 O 0.22454(11) 0.42875(7) 0.45051(11) 0.0440(4) Uani 1 1 d . . . O2 O 0.16641(12) 0.31358(8) 0.09472(12) 0.0500(5) Uani 1 1 d . . . O3 O 0.5000 0.12120(12) 0.2500 0.0576(7) Uani 1 2 d S . . N1 N 0.09457(11) 0.40644(7) 0.33157(11) 0.0271(4) Uani 1 1 d . . . N2 N 0.06403(12) 0.34685(8) 0.15820(11) 0.0276(4) Uani 1 1 d . . . N3 N 0.2076(2) 0.10848(16) 0.7249(3) 0.0989(11) Uani 1 1 d . . . N4 N 0.3998(2) 0.43424(15) 0.0932(3) 0.0983(11) Uani 1 1 d . . . C1 C 0.09429(14) 0.20640(9) 0.36585(13) 0.0294(4) Uani 1 1 d . . . C2 C 0.1228(2) 0.15140(11) 0.34107(17) 0.0461(6) Uani 1 1 d . . . H2 H 0.1552 0.1507 0.2988 0.055 Uiso 1 1 calc . . . C3 C 0.1043(2) 0.09719(11) 0.37758(18) 0.0583(8) Uani 1 1 d . . . H3 H 0.1239 0.0595 0.3599 0.070 Uiso 1 1 calc . . . C4 C 0.0584(2) 0.09745(13) 0.4384(2) 0.0579(8) Uani 1 1 d . . . H4 H 0.0451 0.0601 0.4623 0.069 Uiso 1 1 calc . . . C5 C 0.0315(2) 0.15153(15) 0.4649(2) 0.0728(10) Uani 1 1 d . . . H5 H 0.0008 0.1519 0.5087 0.087 Uiso 1 1 calc . . . C6 C 0.0489(2) 0.20597(12) 0.4282(2) 0.0558(7) Uani 1 1 d . . . H6 H 0.0291 0.2434 0.4463 0.067 Uiso 1 1 calc . . . C7 C 0.19369(16) 0.32191(11) 0.41256(16) 0.0407(6) Uani 1 1 d . . . H7A H 0.1908 0.3089 0.4727 0.049 Uiso 1 1 calc . . . H7B H 0.2576 0.3149 0.4127 0.049 Uiso 1 1 calc . . . C8 C 0.16759(15) 0.38730(10) 0.39503(14) 0.0327(5) Uani 1 1 d . . . C9 C 0.17588(17) 0.48691(11) 0.42732(16) 0.0425(6) Uani 1 1 d . . . H9A H 0.2177 0.5193 0.4199 0.051 Uiso 1 1 calc . . . H9B H 0.1507 0.4995 0.4754 0.051 Uiso 1 1 calc . . . C10 C 0.09787(16) 0.47403(10) 0.33663(15) 0.0347(5) Uani 1 1 d . . . H10A H 0.0380 0.4909 0.3368 0.042 Uiso 1 1 calc . . . H10B H 0.1121 0.4917 0.2842 0.042 Uiso 1 1 calc . . . C11 C 0.16550(17) 0.26354(11) 0.23393(17) 0.0418(6) Uani 1 1 d . . . H11A H 0.2340 0.2666 0.2632 0.050 Uiso 1 1 calc . . . H11B H 0.1495 0.2221 0.2077 0.050 Uiso 1 1 calc . . . C12 C 0.12995(16) 0.31034(10) 0.16177(15) 0.0354(5) Uani 1 1 d . . . C13 C 0.12296(19) 0.36674(13) 0.03909(17) 0.0503(7) Uani 1 1 d . . . H13A H 0.0966 0.3559 -0.0270 0.060 Uiso 1 1 calc . . . H13B H 0.1687 0.4001 0.0472 0.060 Uiso 1 1 calc . . . C14 C 0.04652(17) 0.38551(10) 0.07508(15) 0.0372(5) Uani 1 1 d . . . H14A H 0.0511 0.4294 0.0912 0.045 Uiso 1 1 calc . . . H14B H -0.0158 0.3772 0.0290 0.045 Uiso 1 1 calc . . . C15 C 0.1753(2) 0.06189(16) 0.7076(2) 0.0621(8) Uani 1 1 d . . . C16 C 0.1351(2) 0.00256(17) 0.6835(3) 0.0795(10) Uani 1 1 d . . . H16A H 0.1240 -0.0054 0.6183 0.119 Uiso 1 1 calc . . . H16B H 0.0759 0.0007 0.6946 0.119 Uiso 1 1 calc . . . H16C H 0.1778 -0.0283 0.7213 0.119 Uiso 1 1 calc . . . C17 C 0.3938(2) 0.38462(18) 0.1064(3) 0.0737(10) Uani 1 1 d . . . C18 C 0.3831(3) 0.31935(19) 0.1184(4) 0.1129(16) Uani 1 1 d . . . H18A H 0.3522 0.3003 0.0582 0.169 Uiso 1 1 calc . . . H18B H 0.3454 0.3130 0.1574 0.169 Uiso 1 1 calc . . . H18C H 0.4445 0.3008 0.1478 0.169 Uiso 1 1 calc . . . 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 0.0237(2) 0.0248(2) 0.01846(18) 0.000 0.00742(15) 0.000 Fe2 0.03003(17) 0.03362(17) 0.03976(19) -0.00471(14) 0.01691(14) -0.00110(13) Cl1 0.0678(4) 0.0466(3) 0.0389(3) -0.0032(3) 0.0271(3) -0.0084(3) Cl2 0.0532(4) 0.0422(3) 0.0637(4) -0.0194(3) 0.0048(3) 0.0006(3) Cl3 0.0538(4) 0.0594(4) 0.0363(3) -0.0096(3) 0.0100(3) 0.0096(3) P 0.0282(3) 0.0291(3) 0.0231(2) 0.0036(2) 0.0083(2) 0.0031(2) O1 0.0382(9) 0.0428(9) 0.0400(9) -0.0035(7) -0.0004(7) -0.0122(7) O2 0.0606(11) 0.0575(11) 0.0488(10) 0.0189(8) 0.0404(9) 0.0209(9) O3 0.0439(14) 0.0507(15) 0.093(2) 0.000 0.0432(15) 0.000 N1 0.0284(9) 0.0283(9) 0.0252(8) -0.0002(7) 0.0099(7) -0.0031(7) N2 0.0323(9) 0.0308(9) 0.0216(8) 0.0036(7) 0.0120(7) 0.0011(7) N3 0.103(3) 0.099(2) 0.122(3) -0.017(2) 0.074(2) -0.034(2) N4 0.116(3) 0.067(2) 0.132(3) -0.013(2) 0.067(2) 0.0022(19) C1 0.0329(11) 0.0306(11) 0.0218(9) 0.0046(8) 0.0058(8) 0.0025(9) C2 0.0667(17) 0.0369(13) 0.0351(12) 0.0043(10) 0.0182(12) 0.0095(12) C3 0.092(2) 0.0318(13) 0.0394(14) 0.0017(11) 0.0087(15) 0.0028(14) C4 0.0656(18) 0.0445(15) 0.0524(17) 0.0190(13) 0.0064(14) -0.0122(14) C5 0.091(2) 0.067(2) 0.084(2) 0.0380(18) 0.061(2) 0.0171(17) C6 0.082(2) 0.0433(14) 0.0596(17) 0.0164(13) 0.0460(16) 0.0155(14) C7 0.0344(12) 0.0394(13) 0.0367(12) 0.0041(10) -0.0023(10) -0.0014(10) C8 0.0305(11) 0.0351(11) 0.0299(11) 0.0004(9) 0.0072(9) -0.0069(9) C9 0.0526(15) 0.0347(12) 0.0395(13) -0.0051(10) 0.0149(11) -0.0121(11) C10 0.0425(13) 0.0278(11) 0.0336(11) -0.0012(9) 0.0132(10) -0.0050(9) C11 0.0464(14) 0.0455(13) 0.0421(13) 0.0144(11) 0.0265(11) 0.0178(11) C12 0.0402(13) 0.0395(12) 0.0333(11) 0.0072(10) 0.0214(10) 0.0057(10) C13 0.0573(16) 0.0613(17) 0.0415(14) 0.0211(12) 0.0287(13) 0.0158(13) C14 0.0515(14) 0.0392(12) 0.0263(11) 0.0090(9) 0.0200(10) 0.0069(11) C15 0.0523(17) 0.079(2) 0.0645(19) 0.0069(17) 0.0328(15) -0.0088(16) C16 0.068(2) 0.080(2) 0.091(2) 0.011(2) 0.0288(19) -0.0106(18) C17 0.068(2) 0.071(2) 0.103(3) 0.001(2) 0.055(2) 0.0141(18) C18 0.099(3) 0.082(3) 0.202(5) 0.035(3) 0.108(3) 0.028(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.9891(17) . ? Fe1 N2 1.9892(17) 2 ? Fe1 N1 2.0416(16) 2 ? Fe1 N1 2.0417(16) . ? Fe1 P 2.1842(6) 2 ? Fe1 P 2.1843(6) . ? Fe2 O3 1.7600(5) . ? Fe2 Cl3 2.2169(7) . ? Fe2 Cl2 2.2231(7) . ? Fe2 Cl1 2.2311(7) . ? P C1 1.809(2) . ? P C11 1.836(2) . ? P C7 1.841(2) . ? O1 C8 1.342(2) . ? O1 C9 1.456(3) . ? O2 C12 1.341(3) . ? O2 C13 1.463(3) . ? O3 Fe2 1.7599(5) 2_655 ? N1 C8 1.276(3) . ? N1 C10 1.482(3) . ? N2 C12 1.274(3) . ? N2 C14 1.485(3) . ? N3 C15 1.125(4) . ? N4 C17 1.115(4) . ? C1 C6 1.372(3) . ? C1 C2 1.380(3) . ? C2 C3 1.386(4) . ? C2 H2 0.9500 . ? C3 C4 1.357(4) . ? C3 H3 0.9500 . ? C4 C5 1.363(4) . ? C4 H4 0.9500 . ? C5 C6 1.386(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.486(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C9 C10 1.521(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.474(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 C14 1.519(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.430(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.458(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N2 179.03(10) . 2 ? N2 Fe1 N1 88.45(7) . 2 ? N2 Fe1 N1 90.92(7) 2 2 ? N2 Fe1 N1 90.92(7) . . ? N2 Fe1 N1 88.44(7) 2 . ? N1 Fe1 N1 99.34(9) 2 . ? N2 Fe1 P 98.25(5) . 2 ? N2 Fe1 P 82.41(5) 2 2 ? N1 Fe1 P 82.95(5) 2 2 ? N1 Fe1 P 170.62(5) . 2 ? N2 Fe1 P 82.40(5) . . ? N2 Fe1 P 98.25(5) 2 . ? N1 Fe1 P 170.62(5) 2 . ? N1 Fe1 P 82.95(5) . . ? P Fe1 P 96.26(3) 2 . ? O3 Fe2 Cl3 110.63(2) . . ? O3 Fe2 Cl2 111.36(7) . . ? Cl3 Fe2 Cl2 109.21(3) . . ? O3 Fe2 Cl1 110.41(7) . . ? Cl3 Fe2 Cl1 108.50(3) . . ? Cl2 Fe2 Cl1 106.61(3) . . ? C1 P C11 106.09(10) . . ? C1 P C7 105.76(10) . . ? C11 P C7 106.15(12) . . ? C1 P Fe1 127.51(7) . . ? C11 P Fe1 104.88(7) . . ? C7 P Fe1 104.89(8) . . ? C8 O1 C9 105.68(16) . . ? C12 O2 C13 105.73(17) . . ? Fe2 O3 Fe2 162.00(16) 2_655 . ? C8 N1 C10 106.41(17) . . ? C8 N1 Fe1 120.50(14) . . ? C10 N1 Fe1 133.07(13) . . ? C12 N2 C14 107.25(18) . . ? C12 N2 Fe1 123.00(14) . . ? C14 N2 Fe1 129.74(14) . . ? C6 C1 C2 118.4(2) . . ? C6 C1 P 117.22(17) . . ? C2 C1 P 124.27(18) . . ? C1 C2 C3 120.3(3) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 120.6(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.8(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 120.8(3) . . ? C1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 P 105.60(14) . . ? C8 C7 H7A 110.6 . . ? P C7 H7A 110.6 . . ? C8 C7 H7B 110.6 . . ? P C7 H7B 110.6 . . ? H7A C7 H7B 108.8 . . ? N1 C8 O1 118.14(19) . . ? N1 C8 C7 124.42(19) . . ? O1 C8 C7 117.43(18) . . ? O1 C9 C10 103.67(17) . . ? O1 C9 H9A 111.0 . . ? C10 C9 H9A 111.0 . . ? O1 C9 H9B 111.0 . . ? C10 C9 H9B 111.0 . . ? H9A C9 H9B 109.0 . . ? N1 C10 C9 103.61(17) . . ? N1 C10 H10A 111.0 . . ? C9 C10 H10A 111.0 . . ? N1 C10 H10B 111.0 . . ? C9 C10 H10B 111.0 . . ? H10A C10 H10B 109.0 . . ? C12 C11 P 105.25(15) . . ? C12 C11 H11A 110.7 . . ? P C11 H11A 110.7 . . ? C12 C11 H11B 110.7 . . ? P C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? N2 C12 O2 118.09(19) . . ? N2 C12 C11 123.2(2) . . ? O2 C12 C11 118.70(19) . . ? O2 C13 C14 104.49(18) . . ? O2 C13 H13A 110.9 . . ? C14 C13 H13A 110.9 . . ? O2 C13 H13B 110.9 . . ? C14 C13 H13B 110.9 . . ? H13A C13 H13B 108.9 . . ? N2 C14 C13 103.54(18) . . ? N2 C14 H14A 111.1 . . ? C13 C14 H14A 111.1 . . ? N2 C14 H14B 111.1 . . ? C13 C14 H14B 111.1 . . ? H14A C14 H14B 109.0 . . ? N3 C15 C16 178.5(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 C18 177.0(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 P C1 -133.47(10) . . . . ? N2 Fe1 P C1 47.26(10) 2 . . . ? N1 Fe1 P C1 -120.6(3) 2 . . . ? N1 Fe1 P C1 134.65(10) . . . . ? P Fe1 P C1 -35.94(8) 2 . . . ? N2 Fe1 P C11 -9.03(10) . . . . ? N2 Fe1 P C11 171.70(10) 2 . . . ? N1 Fe1 P C11 3.9(3) 2 . . . ? N1 Fe1 P C11 -100.91(10) . . . . ? P Fe1 P C11 88.50(9) 2 . . . ? N2 Fe1 P C7 102.59(10) . . . . ? N2 Fe1 P C7 -76.68(10) 2 . . . ? N1 Fe1 P C7 115.5(3) 2 . . . ? N1 Fe1 P C7 10.71(10) . . . . ? P Fe1 P C7 -159.88(9) 2 . . . ? Cl3 Fe2 O3 Fe2 89.42(4) . . . 2_655 ? Cl2 Fe2 O3 Fe2 -32.23(3) . . . 2_655 ? Cl1 Fe2 O3 Fe2 -150.45(3) . . . 2_655 ? N2 Fe1 N1 C8 -91.77(17) . . . . ? N2 Fe1 N1 C8 88.97(17) 2 . . . ? N1 Fe1 N1 C8 179.7(2) 2 . . . ? P Fe1 N1 C8 76.2(4) 2 . . . ? P Fe1 N1 C8 -9.54(16) . . . . ? N2 Fe1 N1 C10 90.16(19) . . . . ? N2 Fe1 N1 C10 -89.09(19) 2 . . . ? N1 Fe1 N1 C10 1.59(16) 2 . . . ? P Fe1 N1 C10 -101.8(3) 2 . . . ? P Fe1 N1 C10 172.39(19) . . . . ? N2 Fe1 N2 C12 138.88(18) 2 . . . ? N1 Fe1 N2 C12 -171.44(18) 2 . . . ? N1 Fe1 N2 C12 89.24(18) . . . . ? P Fe1 N2 C12 -88.80(18) 2 . . . ? P Fe1 N2 C12 6.48(17) . . . . ? N2 Fe1 N2 C14 -42.78(18) 2 . . . ? N1 Fe1 N2 C14 6.90(18) 2 . . . ? N1 Fe1 N2 C14 -92.42(18) . . . . ? P Fe1 N2 C14 89.55(17) 2 . . . ? P Fe1 N2 C14 -175.18(18) . . . . ? C11 P C1 C6 -177.2(2) . . . . ? C7 P C1 C6 70.4(2) . . . . ? Fe1 P C1 C6 -53.2(2) . . . . ? C11 P C1 C2 0.1(2) . . . . ? C7 P C1 C2 -112.4(2) . . . . ? Fe1 P C1 C2 124.03(19) . . . . ? C6 C1 C2 C3 1.0(4) . . . . ? P C1 C2 C3 -176.23(19) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C3 C4 C5 C6 1.6(5) . . . . ? C2 C1 C6 C5 -0.4(4) . . . . ? P C1 C6 C5 177.0(3) . . . . ? C4 C5 C6 C1 -0.9(5) . . . . ? C1 P C7 C8 -148.64(16) . . . . ? C11 P C7 C8 98.93(17) . . . . ? Fe1 P C7 C8 -11.78(18) . . . . ? C10 N1 C8 O1 2.7(3) . . . . ? Fe1 N1 C8 O1 -175.81(15) . . . . ? C10 N1 C8 C7 -177.9(2) . . . . ? Fe1 N1 C8 C7 3.5(3) . . . . ? C9 O1 C8 N1 7.8(3) . . . . ? C9 O1 C8 C7 -171.6(2) . . . . ? P C7 C8 N1 6.4(3) . . . . ? P C7 C8 O1 -174.25(17) . . . . ? C8 O1 C9 C10 -14.1(2) . . . . ? C8 N1 C10 C9 -11.4(2) . . . . ? Fe1 N1 C10 C9 166.84(15) . . . . ? O1 C9 C10 N1 15.3(2) . . . . ? C1 P C11 C12 148.29(16) . . . . ? C7 P C11 C12 -99.51(17) . . . . ? Fe1 P C11 C12 11.20(18) . . . . ? C14 N2 C12 O2 -0.6(3) . . . . ? Fe1 N2 C12 O2 178.03(15) . . . . ? C14 N2 C12 C11 -178.4(2) . . . . ? Fe1 N2 C12 C11 0.3(3) . . . . ? C13 O2 C12 N2 6.6(3) . . . . ? C13 O2 C12 C11 -175.5(2) . . . . ? P C11 C12 N2 -8.3(3) . . . . ? P C11 C12 O2 173.92(18) . . . . ? C12 O2 C13 C14 -9.2(3) . . . . ? C12 N2 C14 C13 -5.3(2) . . . . ? Fe1 N2 C14 C13 176.11(16) . . . . ? O2 C13 C14 N2 8.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.411 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.060