Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Leslie D. Field' ; School of Chemistry University of Sydney, Sydney N.S.W. 2006, Australia ; 'Warren J. Shaw ' ; School of Chemistry University of Sydney, Sydney N.S.W. 2006, Australia ; 'Peter Turner' ; School of Chemistry University of Sydney, Sydney N.S.W. 2006, Australia ; _publ_contact_author_name 'Prof Leslie Field' _publ_contact_author_address ; Chemistry University of Sydney Sydney NSW 2006 AUSTRALIA ; _publ_contact_author_phone '+61 2 9351 2060' _publ_contact_author_fax '+61 2 9351 6650 ' _publ_contact_author_email 'l.field@chem.usyd.edud.au' _publ_requested_journal ' Chem. Commun.' _publ_section_title ; Functionalisation of carbon dioxide by an iron(II) complex ; data_ldf117 _database_code_CSD 169564 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H39 Fe N O2 P4 S' _chemical_formula_weight 489.27 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.973(5) _cell_length_b 14.680(8) _cell_length_c 8.748(5) _cell_angle_alpha 104.586(8) _cell_angle_beta 99.791(8) _cell_angle_gamma 81.837(8) _cell_volume 1214.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 948 _cell_measurement_theta_min 2.383 _cell_measurement_theta_max 28.015 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.435 _exptl_crystal_size_mid 0.255 _exptl_crystal_size_min 0.184 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type 'numerical and empirical' _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_T_max 0.886 _exptl_absorpt_process_details ; Gaussian (XPREP, Bruker 1995; Coppens et al., 1965) and SADABS (Sheldrick, 1996) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 182 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.05 _diffrn_reflns_number 12316 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0130 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 28.24 _reflns_number_total 5495 _reflns_number_gt 5096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+1.3631P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5495 _refine_ls_number_parameters 224 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _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 0.85898(3) 0.28858(2) 0.73176(3) 0.02191(10) Uani 1 1 d . A . H1FE H 0.922(3) 0.339(2) 0.883(4) 0.051(9) Uiso 1 1 d . . . S1 S 0.77320(5) 0.19790(4) 0.49040(6) 0.02954(13) Uani 1 1 d . . . P1 P 0.95172(7) 0.15996(5) 0.81160(8) 0.03663(15) Uani 1 1 d . . . P2 P 1.05422(6) 0.28421(5) 0.64470(7) 0.03375(15) Uani 1 1 d D . . P3 P 0.78945(5) 0.43281(4) 0.69805(6) 0.02416(12) Uani 1 1 d . . . P4 P 0.67699(6) 0.30435(4) 0.84992(7) 0.02938(13) Uani 1 1 d . . . O1 O 0.36683(18) 0.31300(13) 0.3256(3) 0.0489(5) Uani 1 1 d . . . O2 O 0.3508(2) 0.20120(18) 0.0953(3) 0.0615(6) Uani 1 1 d . . . N1 N 0.54312(18) 0.19362(12) 0.2801(2) 0.0255(4) Uani 1 1 d . . . C1 C 0.6159(2) 0.23509(14) 0.4139(2) 0.0239(4) Uani 1 1 d . . . H1 H 0.570(3) 0.2918(19) 0.467(3) 0.029(6) Uiso 1 1 d . . . C2 C 0.4036(2) 0.24129(18) 0.2278(3) 0.0360(5) Uani 1 1 d . . . C3 C 0.5918(3) 0.10164(18) 0.1849(3) 0.0383(5) Uani 1 1 d . . . H3A H 0.6929 0.0958 0.1948 0.046 Uiso 1 1 calc R . . H3B H 0.5546 0.0971 0.0712 0.046 Uiso 1 1 calc R . . C4 C 0.5487(3) 0.02209(19) 0.2388(4) 0.0558(8) Uani 1 1 d . . . H4A H 0.5857 0.0264 0.3513 0.084 Uiso 1 1 calc R . . H4B H 0.5836 -0.0386 0.1742 0.084 Uiso 1 1 calc R . . H4C H 0.4486 0.0267 0.2261 0.084 Uiso 1 1 calc R . . C5A C 0.8788(6) 0.0507(4) 0.7311(7) 0.0604(13) Uiso 0.70 1 d P A 1 H5A1 H 0.7841 0.0584 0.7527 0.091 Uiso 0.70 1 calc PR A 1 H5A2 H 0.9321 0.0016 0.7808 0.091 Uiso 0.70 1 calc PR A 1 H5A3 H 0.8803 0.0321 0.6156 0.091 Uiso 0.70 1 calc PR A 1 C6A C 0.9893(6) 0.1633(4) 1.0263(7) 0.0584(14) Uiso 0.70 1 d P A 1 H6A1 H 1.0293 0.2219 1.0831 0.088 Uiso 0.70 1 calc PR A 1 H6A2 H 1.0542 0.1088 1.0431 0.088 Uiso 0.70 1 calc PR A 1 H6A3 H 0.9045 0.1610 1.0671 0.088 Uiso 0.70 1 calc PR A 1 C7A C 1.1265(4) 0.1286(3) 0.7553(5) 0.0436(8) Uiso 0.70 1 d P A 1 H7A1 H 1.1940 0.1561 0.8461 0.052 Uiso 0.70 1 calc PR A 1 H7A2 H 1.1480 0.0590 0.7302 0.052 Uiso 0.70 1 calc PR A 1 C8A C 1.1368(4) 0.1666(3) 0.6089(5) 0.0399(8) Uiso 0.70 1 d P A 1 H8A1 H 1.0909 0.1269 0.5105 0.048 Uiso 0.70 1 calc PR A 1 H8A2 H 1.2338 0.1664 0.5970 0.048 Uiso 0.70 1 calc PR A 1 C9A C 1.0596(4) 0.3207(3) 0.4602(5) 0.0417(8) Uiso 0.70 1 d P A 1 H9A1 H 1.0164 0.3857 0.4687 0.063 Uiso 0.70 1 calc PR A 1 H9A2 H 1.0104 0.2783 0.3698 0.063 Uiso 0.70 1 calc PR A 1 H9A3 H 1.1550 0.3175 0.4434 0.063 Uiso 0.70 1 calc PR A 1 C10A C 1.1892(4) 0.3508(3) 0.7837(5) 0.0417(8) Uiso 0.70 1 d P A 1 H10A H 1.1553 0.4180 0.8130 0.063 Uiso 0.70 1 calc PR A 1 H10B H 1.2708 0.3435 0.7314 0.063 Uiso 0.70 1 calc PR A 1 H10C H 1.2126 0.3260 0.8800 0.063 Uiso 0.70 1 calc PR A 1 C11A C 0.7183(4) 0.4589(2) 0.5044(4) 0.0313(7) Uiso 0.75 1 d P A 1 H11A H 0.7841 0.4335 0.4289 0.047 Uiso 0.75 1 calc PR A 1 H11B H 0.6998 0.5275 0.5170 0.047 Uiso 0.75 1 calc PR A 1 H11C H 0.6330 0.4295 0.4639 0.047 Uiso 0.75 1 calc PR A 1 C12A C 0.9030(3) 0.5303(2) 0.7742(4) 0.0307(7) Uiso 0.75 1 d P A 1 H12A H 0.9499 0.5271 0.8809 0.046 Uiso 0.75 1 calc PR A 1 H12B H 0.8477 0.5915 0.7795 0.046 Uiso 0.75 1 calc PR A 1 H12C H 0.9708 0.5234 0.7020 0.046 Uiso 0.75 1 calc PR A 1 C13A C 0.6459(3) 0.4876(2) 0.8137(4) 0.0256(5) Uiso 0.75 1 d P A 1 H13A H 0.6819 0.5149 0.9262 0.031 Uiso 0.75 1 calc PR A 1 H13B H 0.5916 0.5386 0.7676 0.031 Uiso 0.75 1 calc PR A 1 C14A C 0.5572(3) 0.4090(2) 0.8039(4) 0.0262(5) Uiso 0.75 1 d P A 1 H14A H 0.5049 0.3915 0.6958 0.031 Uiso 0.75 1 calc PR A 1 H14B H 0.4917 0.4303 0.8822 0.031 Uiso 0.75 1 calc PR A 1 C15A C 0.5594(5) 0.2154(3) 0.8058(6) 0.0445(12) Uiso 0.75 1 d P A 1 H15A H 0.5399 0.1914 0.6900 0.067 Uiso 0.75 1 calc PR A 1 H15B H 0.4741 0.2432 0.8482 0.067 Uiso 0.75 1 calc PR A 1 H15C H 0.6003 0.1631 0.8553 0.067 Uiso 0.75 1 calc PR A 1 C16A C 0.6926(4) 0.3363(3) 1.0655(4) 0.0428(8) Uiso 0.75 1 d P A 1 H16A H 0.7560 0.3848 1.1076 0.064 Uiso 0.75 1 calc PR A 1 H16B H 0.7274 0.2802 1.1074 0.064 Uiso 0.75 1 calc PR A 1 H16C H 0.6026 0.3612 1.0981 0.064 Uiso 0.75 1 calc PR A 1 C5B C 0.8480(8) 0.0526(5) 0.7816(9) 0.0247(14) Uiso 0.30 1 d P A 2 H5B1 H 0.7968 0.0399 0.6737 0.037 Uiso 0.30 1 calc PR A 2 H5B2 H 0.7841 0.0670 0.8601 0.037 Uiso 0.30 1 calc PR A 2 H5B3 H 0.9110 -0.0033 0.7958 0.037 Uiso 0.30 1 calc PR A 2 C6B C 1.0324(11) 0.1638(7) 1.0126(11) 0.036(2) Uiso 0.30 1 d P A 2 H6B1 H 0.9694 0.1983 1.0871 0.053 Uiso 0.30 1 calc PR A 2 H6B2 H 1.1156 0.1960 1.0332 0.053 Uiso 0.30 1 calc PR A 2 H6B3 H 1.0564 0.0991 1.0272 0.053 Uiso 0.30 1 calc PR A 2 C7B C 1.0838(10) 0.0899(7) 0.6879(13) 0.052(2) Uiso 0.30 1 d PD A 2 H7B1 H 1.1407 0.0423 0.7401 0.062 Uiso 0.30 1 calc PR A 2 H7B2 H 1.0421 0.0582 0.5800 0.062 Uiso 0.30 1 calc PR A 2 C8B C 1.1636(10) 0.1675(6) 0.6829(14) 0.049(2) Uiso 0.30 1 d PD A 2 H8B1 H 1.2224 0.1434 0.5978 0.059 Uiso 0.30 1 calc PR A 2 H8B2 H 1.2245 0.1836 0.7855 0.059 Uiso 0.30 1 calc PR A 2 C9B C 1.0570(11) 0.2524(8) 0.4260(13) 0.055(2) Uiso 0.30 1 d P A 2 H9B1 H 0.9906 0.2069 0.3746 0.082 Uiso 0.30 1 calc PR A 2 H9B2 H 1.1488 0.2240 0.4037 0.082 Uiso 0.30 1 calc PR A 2 H9B3 H 1.0332 0.3094 0.3841 0.082 Uiso 0.30 1 calc PR A 2 C10B C 1.1773(9) 0.3671(6) 0.7207(11) 0.0359(17) Uiso 0.30 1 d P A 2 H10D H 1.1815 0.3879 0.8369 0.054 Uiso 0.30 1 calc PR A 2 H10E H 1.1508 0.4218 0.6731 0.054 Uiso 0.30 1 calc PR A 2 H10F H 1.2672 0.3371 0.6941 0.054 Uiso 0.30 1 calc PR A 2 C11B C 0.7652(11) 0.4507(6) 0.4933(10) 0.0228(18) Uiso 0.25 1 d P A 2 H11D H 0.7148 0.4005 0.4207 0.034 Uiso 0.25 1 calc PR A 2 H11E H 0.8546 0.4488 0.4597 0.034 Uiso 0.25 1 calc PR A 2 H11F H 0.7132 0.5124 0.4908 0.034 Uiso 0.25 1 calc PR A 2 C12B C 0.8776(11) 0.5233(7) 0.8153(13) 0.032(2) Uiso 0.25 1 d P A 2 H12D H 0.9731 0.5119 0.7958 0.048 Uiso 0.25 1 calc PR A 2 H12E H 0.8739 0.5267 0.9278 0.048 Uiso 0.25 1 calc PR A 2 H12F H 0.8362 0.5832 0.7893 0.048 Uiso 0.25 1 calc PR A 2 C13B C 0.6126(11) 0.4574(8) 0.7432(14) 0.040(2) Uiso 0.25 1 d P A 2 H13C H 0.5858 0.5266 0.7673 0.048 Uiso 0.25 1 calc PR A 2 H13D H 0.5497 0.4275 0.6495 0.048 Uiso 0.25 1 calc PR A 2 C14B C 0.6022(12) 0.4199(8) 0.8810(15) 0.044(2) Uiso 0.25 1 d P A 2 H14C H 0.5049 0.4222 0.8936 0.053 Uiso 0.25 1 calc PR A 2 H14D H 0.6494 0.4587 0.9795 0.053 Uiso 0.25 1 calc PR A 2 C15B C 0.5378(10) 0.2216(7) 0.7663(12) 0.021(2) Uiso 0.25 1 d P A 2 H15D H 0.5794 0.1559 0.7468 0.032 Uiso 0.25 1 calc PR A 2 H15E H 0.4892 0.2350 0.6659 0.032 Uiso 0.25 1 calc PR A 2 H15F H 0.4732 0.2314 0.8432 0.032 Uiso 0.25 1 calc PR A 2 C16B C 0.7131(13) 0.2943(10) 1.0673(14) 0.047(3) Uiso 0.25 1 d P A 2 H16D H 0.7554 0.2304 1.0721 0.071 Uiso 0.25 1 calc PR A 2 H16E H 0.6271 0.3066 1.1125 0.071 Uiso 0.25 1 calc PR A 2 H16F H 0.7753 0.3407 1.1286 0.071 Uiso 0.25 1 calc PR A 2 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 0.01776(15) 0.02700(16) 0.01873(15) 0.00342(11) -0.00039(10) -0.00190(11) S1 0.0235(3) 0.0321(3) 0.0244(2) -0.0016(2) -0.00406(19) 0.0020(2) P1 0.0351(3) 0.0376(3) 0.0337(3) 0.0127(3) -0.0025(2) 0.0065(3) P2 0.0187(3) 0.0472(4) 0.0315(3) 0.0024(2) 0.0032(2) -0.0034(2) P3 0.0205(2) 0.0293(3) 0.0230(2) 0.0074(2) 0.00296(18) -0.0017(2) P4 0.0304(3) 0.0293(3) 0.0307(3) 0.0050(2) 0.0112(2) -0.0057(2) O1 0.0308(9) 0.0394(10) 0.0652(13) 0.0067(9) -0.0061(8) 0.0089(8) O2 0.0387(11) 0.0819(16) 0.0475(12) 0.0070(11) -0.0211(9) 0.0001(10) N1 0.0230(8) 0.0263(8) 0.0250(8) 0.0057(7) -0.0027(6) -0.0029(7) C1 0.0233(9) 0.0228(9) 0.0245(9) 0.0046(7) 0.0008(7) -0.0029(8) C2 0.0247(11) 0.0416(13) 0.0414(13) 0.0166(11) -0.0058(9) -0.0025(9) C3 0.0329(12) 0.0392(13) 0.0297(11) -0.0072(9) -0.0054(9) 0.0003(10) C4 0.0486(16) 0.0280(12) 0.078(2) 0.0007(13) -0.0091(15) -0.0053(11) _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 P4 2.1941(11) . ? Fe1 P2 2.1954(12) . ? Fe1 P1 2.2038(11) . ? Fe1 P3 2.2089(12) . ? Fe1 S1 2.2925(10) . ? Fe1 H1FE 1.43(3) . ? S1 C1 1.670(2) . ? P1 C5A 1.785(5) . ? P1 C6B 1.796(9) . ? P1 C6A 1.842(6) . ? P1 C7A 1.855(4) . ? P1 C7B 1.872(10) . ? P1 C5B 1.946(7) . ? P2 C10B 1.780(8) . ? P2 C8A 1.781(4) . ? P2 C9A 1.835(4) . ? P2 C9B 1.856(11) . ? P2 C10A 1.861(4) . ? P2 C8B 1.967(9) . ? P3 C12B 1.711(10) . ? P3 C11A 1.833(3) . ? P3 C13B 1.839(11) . ? P3 C11B 1.846(9) . ? P3 C13A 1.864(3) . ? P3 C12A 1.870(3) . ? P4 C14B 1.728(11) . ? P4 C15A 1.805(5) . ? P4 C16A 1.810(4) . ? P4 C14A 1.891(3) . ? P4 C15B 1.903(9) . ? P4 C16B 1.914(12) . ? O1 C2 1.232(3) . ? O2 C2 1.226(3) . ? N1 C1 1.321(3) . ? N1 C3 1.462(3) . ? N1 C2 1.518(3) . ? C1 H1 0.94(3) . ? C3 C4 1.504(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A C8A 1.543(6) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A H8A1 0.9900 . ? C8A H8A2 0.9900 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C13A C14A 1.528(4) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C5B H5B1 0.9800 . ? C5B H5B2 0.9800 . ? C5B H5B3 0.9800 . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C7B C8B 1.492(5) . ? C7B H7B1 0.9900 . ? C7B H7B2 0.9900 . ? C8B H8B1 0.9900 . ? C8B H8B2 0.9900 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? C13B C14B 1.469(15) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 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 P4 Fe1 P2 172.14(3) . . ? P4 Fe1 P1 94.43(3) . . ? P2 Fe1 P1 85.29(3) . . ? P4 Fe1 P3 85.59(3) . . ? P2 Fe1 P3 93.07(3) . . ? P1 Fe1 P3 168.20(3) . . ? P4 Fe1 S1 97.48(4) . . ? P2 Fe1 S1 90.38(4) . . ? P1 Fe1 S1 90.39(4) . . ? P3 Fe1 S1 101.32(4) . . ? P4 Fe1 H1FE 85.2(13) . . ? P2 Fe1 H1FE 87.0(13) . . ? P1 Fe1 H1FE 85.5(12) . . ? P3 Fe1 H1FE 82.7(12) . . ? S1 Fe1 H1FE 175.3(13) . . ? C1 S1 Fe1 115.76(8) . . ? C5A P1 C6B 109.5(4) . . ? C5A P1 C6A 102.7(3) . . ? C6B P1 C6A 14.7(3) . . ? C5A P1 C7A 101.6(2) . . ? C6B P1 C7A 86.1(4) . . ? C6A P1 C7A 100.2(2) . . ? C5A P1 C7B 78.5(3) . . ? C6B P1 C7B 103.5(5) . . ? C6A P1 C7B 115.6(4) . . ? C7A P1 C7B 25.3(3) . . ? C5A P1 C5B 17.0(2) . . ? C6B P1 C5B 98.6(4) . . ? C6A P1 C5B 89.3(3) . . ? C7A P1 C5B 114.7(3) . . ? C7B P1 C5B 93.6(3) . . ? C5A P1 Fe1 120.45(18) . . ? C6B P1 Fe1 122.3(3) . . ? C6A P1 Fe1 119.78(18) . . ? C7A P1 Fe1 108.92(13) . . ? C7B P1 Fe1 112.8(3) . . ? C5B P1 Fe1 121.2(2) . . ? C10B P2 C8A 110.3(3) . . ? C10B P2 C9A 81.5(3) . . ? C8A P2 C9A 103.38(19) . . ? C10B P2 C9B 104.4(5) . . ? C8A P2 C9B 76.6(4) . . ? C9A P2 C9B 30.6(3) . . ? C10B P2 C10A 20.1(3) . . ? C8A P2 C10A 101.63(19) . . ? C9A P2 C10A 101.23(19) . . ? C9B P2 C10A 121.1(4) . . ? C10B P2 C8B 100.6(4) . . ? C8A P2 C8B 19.3(3) . . ? C9A P2 C8B 119.4(4) . . ? C9B P2 C8B 95.0(5) . . ? C10A P2 C8B 87.4(3) . . ? C10B P2 Fe1 126.3(3) . . ? C8A P2 Fe1 110.08(13) . . ? C9A P2 Fe1 120.85(13) . . ? C9B P2 Fe1 118.3(3) . . ? C10A P2 Fe1 117.21(14) . . ? C8B P2 Fe1 106.2(3) . . ? C12B P3 C11A 110.4(4) . . ? C12B P3 C13B 107.2(5) . . ? C11A P3 C13B 85.9(4) . . ? C12B P3 C11B 106.0(5) . . ? C11A P3 C11B 15.2(3) . . ? C13B P3 C11B 101.0(5) . . ? C12B P3 C13A 85.9(4) . . ? C11A P3 C13A 100.01(16) . . ? C13B P3 C13A 22.5(3) . . ? C11B P3 C13A 114.6(3) . . ? C12B P3 C12A 15.6(4) . . ? C11A P3 C12A 98.64(16) . . ? C13B P3 C12A 117.6(4) . . ? C11B P3 C12A 92.1(3) . . ? C13A P3 C12A 98.08(15) . . ? C12B P3 Fe1 117.6(3) . . ? C11A P3 Fe1 123.71(11) . . ? C13B P3 Fe1 105.4(3) . . ? C11B P3 Fe1 117.9(3) . . ? C13A P3 Fe1 110.68(9) . . ? C12A P3 Fe1 121.11(11) . . ? C14B P4 C15A 115.3(4) . . ? C14B P4 C16A 79.4(4) . . ? C15A P4 C16A 100.2(2) . . ? C14B P4 C14A 23.0(4) . . ? C15A P4 C14A 100.58(18) . . ? C16A P4 C14A 99.38(17) . . ? C14B P4 C15B 108.9(5) . . ? C15A P4 C15B 12.0(3) . . ? C16A P4 C15B 109.6(3) . . ? C14A P4 C15B 91.5(3) . . ? C14B P4 C16B 98.3(6) . . ? C15A P4 C16B 89.9(4) . . ? C16A P4 C16B 19.1(4) . . ? C14A P4 C16B 117.3(4) . . ? C15B P4 C16B 101.0(5) . . ? C14B P4 Fe1 110.4(4) . . ? C15A P4 Fe1 123.31(15) . . ? C16A P4 Fe1 119.95(13) . . ? C14A P4 Fe1 109.46(9) . . ? C15B P4 Fe1 120.6(3) . . ? C16B P4 Fe1 115.1(4) . . ? C1 N1 C3 121.49(18) . . ? C1 N1 C2 118.96(18) . . ? C3 N1 C2 119.52(18) . . ? N1 C1 S1 127.16(17) . . ? N1 C1 H1 113.0(16) . . ? S1 C1 H1 119.8(16) . . ? O2 C2 O1 132.9(2) . . ? O2 C2 N1 113.3(2) . . ? O1 C2 N1 113.8(2) . . ? N1 C3 C4 111.1(2) . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P1 C5A H5A1 109.5 . . ? P1 C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? P1 C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? P1 C6A H6A1 109.5 . . ? P1 C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? P1 C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C8A C7A P1 110.3(3) . . ? C8A C7A H7A1 109.6 . . ? P1 C7A H7A1 109.6 . . ? C8A C7A H7A2 109.6 . . ? P1 C7A H7A2 109.6 . . ? H7A1 C7A H7A2 108.1 . . ? C7A C8A P2 106.1(3) . . ? C7A C8A H8A1 110.5 . . ? P2 C8A H8A1 110.5 . . ? C7A C8A H8A2 110.5 . . ? P2 C8A H8A2 110.5 . . ? H8A1 C8A H8A2 108.7 . . ? P2 C9A H9A1 109.5 . . ? P2 C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? P2 C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? P2 C10A H10A 109.5 . . ? P2 C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? P2 C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? P3 C11A H11A 109.5 . . ? P3 C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? P3 C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? P3 C12A H12A 109.5 . . ? P3 C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? P3 C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? C14A C13A P3 106.92(19) . . ? C14A C13A H13A 110.3 . . ? P3 C13A H13A 110.3 . . ? C14A C13A H13B 110.3 . . ? P3 C13A H13B 110.3 . . ? H13A C13A H13B 108.6 . . ? C13A C14A P4 106.9(2) . . ? C13A C14A H14A 110.3 . . ? P4 C14A H14A 110.3 . . ? C13A C14A H14B 110.3 . . ? P4 C14A H14B 110.3 . . ? H14A C14A H14B 108.6 . . ? P4 C15A H15A 109.5 . . ? P4 C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? P4 C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? P4 C16A H16A 109.5 . . ? P4 C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? P4 C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? P1 C5B H5B1 109.5 . . ? P1 C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? P1 C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? P1 C6B H6B1 109.5 . . ? P1 C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? P1 C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C8B C7B P1 99.8(7) . . ? C8B C7B H7B1 111.8 . . ? P1 C7B H7B1 111.8 . . ? C8B C7B H7B2 111.8 . . ? P1 C7B H7B2 111.8 . . ? H7B1 C7B H7B2 109.5 . . ? C7B C8B P2 115.6(7) . . ? C7B C8B H8B1 108.4 . . ? P2 C8B H8B1 108.4 . . ? C7B C8B H8B2 108.4 . . ? P2 C8B H8B2 108.4 . . ? H8B1 C8B H8B2 107.4 . . ? P2 C9B H9B1 109.5 . . ? P2 C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? P2 C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? P2 C10B H10D 109.5 . . ? P2 C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? P2 C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? P3 C11B H11D 109.5 . . ? P3 C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? P3 C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? P3 C12B H12D 109.5 . . ? P3 C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? P3 C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C14B C13B P3 109.6(8) . . ? C14B C13B H13C 109.8 . . ? P3 C13B H13C 109.8 . . ? C14B C13B H13D 109.8 . . ? P3 C13B H13D 109.8 . . ? H13C C13B H13D 108.2 . . ? C13B C14B P4 108.7(8) . . ? C13B C14B H14C 109.9 . . ? P4 C14B H14C 109.9 . . ? C13B C14B H14D 109.9 . . ? P4 C14B H14D 109.9 . . ? H14C C14B H14D 108.3 . . ? P4 C15B H15D 109.5 . . ? P4 C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? P4 C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? P4 C16B H16D 109.5 . . ? P4 C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? P4 C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 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 P4 Fe1 S1 C1 46.28(9) . . . . ? P2 Fe1 S1 C1 -133.91(9) . . . . ? P1 Fe1 S1 C1 140.80(9) . . . . ? P3 Fe1 S1 C1 -40.70(9) . . . . ? P4 Fe1 P1 C5A 70.4(2) . . . . ? P2 Fe1 P1 C5A -117.5(2) . . . . ? P3 Fe1 P1 C5A 160.0(2) . . . . ? S1 Fe1 P1 C5A -27.2(2) . . . . ? P4 Fe1 P1 C6B -75.6(4) . . . . ? P2 Fe1 P1 C6B 96.6(4) . . . . ? P3 Fe1 P1 C6B 14.1(4) . . . . ? S1 Fe1 P1 C6B -173.1(4) . . . . ? P4 Fe1 P1 C6A -58.7(2) . . . . ? P2 Fe1 P1 C6A 113.5(2) . . . . ? P3 Fe1 P1 C6A 31.0(3) . . . . ? S1 Fe1 P1 C6A -156.2(2) . . . . ? P4 Fe1 P1 C7A -173.05(14) . . . . ? P2 Fe1 P1 C7A -0.93(14) . . . . ? P3 Fe1 P1 C7A -83.40(19) . . . . ? S1 Fe1 P1 C7A 89.41(14) . . . . ? P4 Fe1 P1 C7B 160.1(3) . . . . ? P2 Fe1 P1 C7B -27.7(3) . . . . ? P3 Fe1 P1 C7B -110.2(4) . . . . ? S1 Fe1 P1 C7B 62.6(3) . . . . ? P4 Fe1 P1 C5B 50.6(3) . . . . ? P2 Fe1 P1 C5B -137.3(3) . . . . ? P3 Fe1 P1 C5B 140.3(3) . . . . ? S1 Fe1 P1 C5B -46.9(3) . . . . ? P4 Fe1 P2 C10B -24.2(4) . . . . ? P1 Fe1 P2 C10B -112.5(4) . . . . ? P3 Fe1 P2 C10B 55.8(4) . . . . ? S1 Fe1 P2 C10B 157.1(4) . . . . ? P4 Fe1 P2 C8A 112.4(2) . . . . ? P1 Fe1 P2 C8A 24.12(15) . . . . ? P3 Fe1 P2 C8A -167.59(15) . . . . ? S1 Fe1 P2 C8A -66.23(16) . . . . ? P4 Fe1 P2 C9A -127.2(2) . . . . ? P1 Fe1 P2 C9A 144.48(15) . . . . ? P3 Fe1 P2 C9A -47.23(15) . . . . ? S1 Fe1 P2 C9A 54.12(15) . . . . ? P4 Fe1 P2 C9B -162.4(4) . . . . ? P1 Fe1 P2 C9B 109.3(4) . . . . ? P3 Fe1 P2 C9B -82.4(4) . . . . ? S1 Fe1 P2 C9B 18.9(4) . . . . ? P4 Fe1 P2 C10A -3.0(3) . . . . ? P1 Fe1 P2 C10A -91.31(16) . . . . ? P3 Fe1 P2 C10A 76.98(16) . . . . ? S1 Fe1 P2 C10A 178.34(16) . . . . ? P4 Fe1 P2 C8B 92.5(4) . . . . ? P1 Fe1 P2 C8B 4.2(3) . . . . ? P3 Fe1 P2 C8B 172.5(3) . . . . ? S1 Fe1 P2 C8B -86.1(4) . . . . ? P4 Fe1 P3 C12B 106.1(5) . . . . ? P2 Fe1 P3 C12B -66.2(5) . . . . ? P1 Fe1 P3 C12B 15.5(5) . . . . ? S1 Fe1 P3 C12B -157.2(5) . . . . ? P4 Fe1 P3 C11A -108.65(16) . . . . ? P2 Fe1 P3 C11A 79.12(16) . . . . ? P1 Fe1 P3 C11A 160.79(19) . . . . ? S1 Fe1 P3 C11A -11.89(16) . . . . ? P4 Fe1 P3 C13B -13.3(4) . . . . ? P2 Fe1 P3 C13B 174.5(4) . . . . ? P1 Fe1 P3 C13B -103.8(4) . . . . ? S1 Fe1 P3 C13B 83.5(4) . . . . ? P4 Fe1 P3 C11B -125.0(4) . . . . ? P2 Fe1 P3 C11B 62.8(4) . . . . ? P1 Fe1 P3 C11B 144.5(4) . . . . ? S1 Fe1 P3 C11B -28.2(4) . . . . ? P4 Fe1 P3 C13A 9.73(10) . . . . ? P2 Fe1 P3 C13A -162.51(10) . . . . ? P1 Fe1 P3 C13A -80.84(17) . . . . ? S1 Fe1 P3 C13A 106.49(11) . . . . ? P4 Fe1 P3 C12A 123.51(14) . . . . ? P2 Fe1 P3 C12A -48.72(14) . . . . ? P1 Fe1 P3 C12A 32.9(2) . . . . ? S1 Fe1 P3 C12A -139.72(14) . . . . ? P2 Fe1 P4 C14B 70.5(5) . . . . ? P1 Fe1 P4 C14B 158.1(5) . . . . ? P3 Fe1 P4 C14B -10.1(5) . . . . ? S1 Fe1 P4 C14B -110.9(5) . . . . ? P2 Fe1 P4 C15A -147.4(3) . . . . ? P1 Fe1 P4 C15A -59.7(2) . . . . ? P3 Fe1 P4 C15A 132.1(2) . . . . ? S1 Fe1 P4 C15A 31.23(19) . . . . ? P2 Fe1 P4 C16A -18.9(3) . . . . ? P1 Fe1 P4 C16A 68.77(17) . . . . ? P3 Fe1 P4 C16A -99.40(16) . . . . ? S1 Fe1 P4 C16A 159.74(16) . . . . ? P2 Fe1 P4 C14A 94.9(2) . . . . ? P1 Fe1 P4 C14A -177.46(10) . . . . ? P3 Fe1 P4 C14A 14.37(10) . . . . ? S1 Fe1 P4 C14A -86.49(11) . . . . ? P2 Fe1 P4 C15B -161.2(4) . . . . ? P1 Fe1 P4 C15B -73.5(4) . . . . ? P3 Fe1 P4 C15B 118.3(4) . . . . ? S1 Fe1 P4 C15B 17.5(4) . . . . ? P2 Fe1 P4 C16B -39.7(5) . . . . ? P1 Fe1 P4 C16B 48.0(5) . . . . ? P3 Fe1 P4 C16B -120.2(5) . . . . ? S1 Fe1 P4 C16B 138.9(5) . . . . ? C3 N1 C1 S1 4.7(3) . . . . ? C2 N1 C1 S1 -177.54(16) . . . . ? Fe1 S1 C1 N1 -177.59(16) . . . . ? C1 N1 C2 O2 173.7(2) . . . . ? C3 N1 C2 O2 -8.5(3) . . . . ? C1 N1 C2 O1 -5.4(3) . . . . ? C3 N1 C2 O1 172.4(2) . . . . ? C1 N1 C3 C4 88.4(3) . . . . ? C2 N1 C3 C4 -89.4(3) . . . . ? C5A P1 C7A C8A 101.9(3) . . . . ? C6B P1 C7A C8A -149.1(4) . . . . ? C6A P1 C7A C8A -152.8(3) . . . . ? C7B P1 C7A C8A 77.2(8) . . . . ? C5B P1 C7A C8A 113.3(4) . . . . ? Fe1 P1 C7A C8A -26.2(3) . . . . ? P1 C7A C8A P2 44.2(3) . . . . ? C10B P2 C8A C7A 98.3(4) . . . . ? C9A P2 C8A C7A -175.9(3) . . . . ? C9B P2 C8A C7A -161.0(5) . . . . ? C10A P2 C8A C7A 79.4(3) . . . . ? C8B P2 C8A C7A 36.0(8) . . . . ? Fe1 P2 C8A C7A -45.5(3) . . . . ? C12B P3 C13A C14A -155.5(4) . . . . ? C11A P3 C13A C14A 94.5(2) . . . . ? C13B P3 C13A C14A 42.8(9) . . . . ? C11B P3 C13A C14A 98.8(3) . . . . ? C12A P3 C13A C14A -165.2(2) . . . . ? Fe1 P3 C13A C14A -37.5(2) . . . . ? P3 C13A C14A P4 47.4(2) . . . . ? C14B P4 C14A C13A 55.5(10) . . . . ? C15A P4 C14A C13A -172.3(2) . . . . ? C16A P4 C14A C13A 85.4(2) . . . . ? C15B P4 C14A C13A -164.5(3) . . . . ? C16B P4 C14A C13A 92.3(5) . . . . ? Fe1 P4 C14A C13A -41.2(2) . . . . ? C5A P1 C7B C8B 165.5(7) . . . . ? C6B P1 C7B C8B -87.0(8) . . . . ? C6A P1 C7B C8B -95.9(7) . . . . ? C7A P1 C7B C8B -39.2(6) . . . . ? C5B P1 C7B C8B 173.2(7) . . . . ? Fe1 P1 C7B C8B 47.1(8) . . . . ? P1 C7B C8B P2 -43.5(9) . . . . ? C10B P2 C8B C7B 159.1(8) . . . . ? C8A P2 C8B C7B -78.5(11) . . . . ? C9A P2 C8B C7B -114.7(8) . . . . ? C9B P2 C8B C7B -95.2(9) . . . . ? C10A P2 C8B C7B 143.8(9) . . . . ? Fe1 P2 C8B C7B 26.2(9) . . . . ? C12B P3 C13B C14B -86.2(9) . . . . ? C11A P3 C13B C14B 163.7(8) . . . . ? C11B P3 C13B C14B 163.1(8) . . . . ? C13A P3 C13B C14B -67.1(10) . . . . ? C12A P3 C13B C14B -98.7(8) . . . . ? Fe1 P3 C13B C14B 39.8(9) . . . . ? P3 C13B C14B P4 -49.2(10) . . . . ? C15A P4 C14B C13B -107.9(8) . . . . ? C16A P4 C14B C13B 155.7(9) . . . . ? C14A P4 C14B C13B -54.3(9) . . . . ? C15B P4 C14B C13B -97.0(9) . . . . ? C16B P4 C14B C13B 158.3(9) . . . . ? Fe1 P4 C14B C13B 37.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.690 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.071 #--------------------------------------------------- #----END #--------------------------------------------------- data_ldf125 _database_code_CSD 169565 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H39 Fe N O2 P4 S' _chemical_formula_weight 489.27 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.989(9) _cell_length_b 12.561(6) _cell_length_c 20.303(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.604(8) _cell_angle_gamma 90.00 _cell_volume 4573(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 948 _cell_measurement_theta_min 2.791 _cell_measurement_theta_max 26.292 _exptl_crystal_description columnar _exptl_crystal_colour red _exptl_crystal_size_max 0.276 _exptl_crystal_size_mid 0.079 _exptl_crystal_size_min 0.052 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.042 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.821 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_process_details ; Gaussian (XPREP, Bruker 1995; Coppens et al., 1965) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 114 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 39164 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0917 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10548 _reflns_number_gt 5840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997), XSHELL (Bruker, 2000) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10548 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0489 _refine_ls_wR_factor_gt 0.0444 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.001 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.66641(2) 0.66509(3) 0.11268(2) 0.01513(11) Uani 1 1 d . . . Fe2 Fe 0.16037(2) 0.74926(3) 0.11345(2) 0.01398(10) Uani 1 1 d . . . S1 S 0.54478(4) 0.60665(6) 0.08443(4) 0.02223(19) Uani 1 1 d . . . S2 S 0.03652(4) 0.69548(6) 0.08993(4) 0.02015(18) Uani 1 1 d . . . P1 P 0.62972(4) 0.82968(7) 0.12162(4) 0.0211(2) Uani 1 1 d . . . P2 P 0.64509(4) 0.65218(6) 0.22092(4) 0.01970(19) Uani 1 1 d . . . P3 P 0.78978(4) 0.69053(7) 0.12530(4) 0.02056(19) Uani 1 1 d . . . P4 P 0.67827(4) 0.68000(6) 0.00489(4) 0.01988(19) Uani 1 1 d . . . P5 P 0.12700(4) 0.91536(6) 0.12319(4) 0.01836(18) Uani 1 1 d . . . P6 P 0.14637(4) 0.73937(6) 0.22347(4) 0.01722(19) Uani 1 1 d . . . P7 P 0.28395(4) 0.77123(6) 0.12154(4) 0.01808(18) Uani 1 1 d . . . P8 P 0.16717(4) 0.76295(6) 0.00509(4) 0.01765(18) Uani 1 1 d . . . O1 O 0.70169(9) 0.51024(15) 0.10639(9) 0.0200(5) Uani 1 1 d . . . O2 O 0.71305(10) 0.38075(16) 0.18304(10) 0.0311(6) Uani 1 1 d . . . O3 O 0.19107(9) 0.59253(16) 0.10711(9) 0.0185(5) Uani 1 1 d . . . O4 O 0.20332(10) 0.46583(16) 0.18528(10) 0.0280(5) Uani 1 1 d . . . N1 N 0.60163(12) 0.40900(19) 0.12525(12) 0.0221(6) Uani 1 1 d . . . N2 N 0.09006(12) 0.49757(18) 0.13102(11) 0.0187(6) Uani 1 1 d . . . C1 C 0.67614(15) 0.4337(2) 0.14007(15) 0.0213(7) Uani 1 1 d . . . C2 C 0.56128(15) 0.4645(2) 0.07119(15) 0.0251(8) Uani 1 1 d . . . H2A H 0.5124 0.4291 0.0617 0.030 Uiso 1 1 calc R . . H2B H 0.5893 0.4568 0.0314 0.030 Uiso 1 1 calc R . . C3 C 0.56725(15) 0.3210(2) 0.15688(15) 0.0251(7) Uani 1 1 d . . . H3A H 0.5129 0.3342 0.1560 0.030 Uiso 1 1 calc R . . H3B H 0.5872 0.3181 0.2037 0.030 Uiso 1 1 calc R . . C4 C 0.57971(16) 0.2138(2) 0.12512(16) 0.0322(9) Uani 1 1 d . . . H4A H 0.5628 0.2170 0.0781 0.048 Uiso 1 1 calc R . . H4B H 0.5515 0.1590 0.1467 0.048 Uiso 1 1 calc R . . H4C H 0.6329 0.1962 0.1300 0.048 Uiso 1 1 calc R . . C5 C 0.53255(15) 0.8598(2) 0.09537(16) 0.0315(8) Uani 1 1 d . . . H5A H 0.4999 0.8103 0.1167 0.047 Uiso 1 1 calc R . . H5B H 0.5245 0.8525 0.0473 0.047 Uiso 1 1 calc R . . H5C H 0.5211 0.9329 0.1081 0.047 Uiso 1 1 calc R . . C6 C 0.67437(16) 0.9455(2) 0.08633(16) 0.0343(9) Uani 1 1 d . . . H6A H 0.6778 0.9342 0.0389 0.051 Uiso 1 1 calc R . . H6B H 0.7245 0.9547 0.1082 0.051 Uiso 1 1 calc R . . H6C H 0.6446 1.0093 0.0930 0.051 Uiso 1 1 calc R . . C7 C 0.63279(17) 0.8687(2) 0.20921(14) 0.0265(8) Uani 1 1 d . . . H7A H 0.6847 0.8841 0.2264 0.032 Uiso 1 1 calc R . . H7B H 0.6022 0.9332 0.2144 0.032 Uiso 1 1 calc R . . C8 C 0.60202(16) 0.7761(2) 0.24623(15) 0.0274(8) Uani 1 1 d . . . H8A H 0.5473 0.7721 0.2366 0.033 Uiso 1 1 calc R . . H8B H 0.6127 0.7866 0.2944 0.033 Uiso 1 1 calc R . . C9 C 0.58020(16) 0.5550(2) 0.25046(14) 0.0301(8) Uani 1 1 d . . . H9A H 0.6029 0.4841 0.2507 0.045 Uiso 1 1 calc R . . H9B H 0.5342 0.5549 0.2212 0.045 Uiso 1 1 calc R . . H9C H 0.5687 0.5739 0.2954 0.045 Uiso 1 1 calc R . . C10 C 0.72236(15) 0.6368(2) 0.28394(14) 0.0320(8) Uani 1 1 d . . . H10A H 0.7029 0.6315 0.3275 0.048 Uiso 1 1 calc R . . H10B H 0.7555 0.6986 0.2830 0.048 Uiso 1 1 calc R . . H10C H 0.7503 0.5720 0.2752 0.048 Uiso 1 1 calc R . . C11 C 0.83534(15) 0.8134(2) 0.15411(16) 0.0305(8) Uani 1 1 d . . . H11A H 0.8189 0.8323 0.1974 0.046 Uiso 1 1 calc R . . H11B H 0.8221 0.8707 0.1226 0.046 Uiso 1 1 calc R . . H11C H 0.8895 0.8032 0.1578 0.046 Uiso 1 1 calc R . . C12 C 0.84851(15) 0.5943(2) 0.17191(16) 0.0311(8) Uani 1 1 d . . . H12A H 0.8973 0.5908 0.1537 0.047 Uiso 1 1 calc R . . H12B H 0.8248 0.5240 0.1688 0.047 Uiso 1 1 calc R . . H12C H 0.8551 0.6163 0.2183 0.047 Uiso 1 1 calc R . . C13 C 0.82470(15) 0.6768(2) 0.04279(14) 0.0262(8) Uani 1 1 d . . . H13A H 0.8747 0.7098 0.0428 0.031 Uiso 1 1 calc R . . H13B H 0.8293 0.6005 0.0317 0.031 Uiso 1 1 calc R . . C14 C 0.77163(14) 0.7306(2) -0.00834(14) 0.0278(8) Uani 1 1 d . . . H14A H 0.7849 0.7131 -0.0535 0.033 Uiso 1 1 calc R . . H14B H 0.7735 0.8089 -0.0027 0.033 Uiso 1 1 calc R . . C15 C 0.61619(16) 0.7650(2) -0.04772(14) 0.0302(8) Uani 1 1 d . . . H15A H 0.6264 0.7550 -0.0940 0.045 Uiso 1 1 calc R . . H15B H 0.6246 0.8396 -0.0353 0.045 Uiso 1 1 calc R . . H15C H 0.5642 0.7459 -0.0421 0.045 Uiso 1 1 calc R . . C16 C 0.67547(15) 0.5603(2) -0.04532(14) 0.0271(8) Uani 1 1 d . . . H16A H 0.6236 0.5376 -0.0546 0.041 Uiso 1 1 calc R . . H16B H 0.7038 0.5037 -0.0215 0.041 Uiso 1 1 calc R . . H16C H 0.6975 0.5751 -0.0870 0.041 Uiso 1 1 calc R . . C17 C 0.16525(16) 0.5178(2) 0.14275(14) 0.0200(7) Uani 1 1 d . . . C18 C 0.04819(15) 0.5527(2) 0.07841(15) 0.0228(8) Uani 1 1 d . . . H18A H -0.0019 0.5199 0.0720 0.027 Uiso 1 1 calc R . . H18B H 0.0731 0.5415 0.0372 0.027 Uiso 1 1 calc R . . C19 C 0.05565(15) 0.4106(2) 0.16515(15) 0.0245(7) Uani 1 1 d . . . H19A H 0.0022 0.4271 0.1682 0.029 Uiso 1 1 calc R . . H19B H 0.0794 0.4055 0.2107 0.029 Uiso 1 1 calc R . . C20 C 0.06215(17) 0.3047(2) 0.13148(16) 0.0339(9) Uani 1 1 d . . . H20A H 0.0399 0.3096 0.0859 0.051 Uiso 1 1 calc R . . H20B H 0.0359 0.2504 0.1553 0.051 Uiso 1 1 calc R . . H20C H 0.1149 0.2852 0.1313 0.051 Uiso 1 1 calc R . . C21 C 0.02905(14) 0.9483(2) 0.10181(15) 0.0267(8) Uani 1 1 d . . . H21A H -0.0026 0.9036 0.1275 0.040 Uiso 1 1 calc R . . H21B H 0.0167 0.9357 0.0546 0.040 Uiso 1 1 calc R . . H21C H 0.0205 1.0234 0.1119 0.040 Uiso 1 1 calc R . . C22 C 0.17003(16) 1.0297(2) 0.08481(15) 0.0293(8) Uani 1 1 d . . . H22A H 0.1611 1.0248 0.0367 0.044 Uiso 1 1 calc R . . H22B H 0.2238 1.0296 0.0971 0.044 Uiso 1 1 calc R . . H22C H 0.1482 1.0958 0.1002 0.044 Uiso 1 1 calc R . . C23 C 0.13695(16) 0.9565(2) 0.21018(14) 0.0246(8) Uani 1 1 d . . . H23A H 0.1900 0.9707 0.2244 0.029 Uiso 1 1 calc R . . H23B H 0.1079 1.0222 0.2165 0.029 Uiso 1 1 calc R . . C24 C 0.10749(15) 0.8651(2) 0.25023(14) 0.0240(7) Uani 1 1 d . . . H24A H 0.0524 0.8628 0.2438 0.029 Uiso 1 1 calc R . . H24B H 0.1218 0.8764 0.2978 0.029 Uiso 1 1 calc R . . C25 C 0.08321(16) 0.6442(2) 0.25692(14) 0.0274(8) Uani 1 1 d . . . H25A H 0.1058 0.5732 0.2576 0.041 Uiso 1 1 calc R . . H25B H 0.0361 0.6430 0.2292 0.041 Uiso 1 1 calc R . . H25C H 0.0737 0.6651 0.3020 0.041 Uiso 1 1 calc R . . C26 C 0.22704(15) 0.7219(2) 0.28230(14) 0.0256(8) Uani 1 1 d . . . H26A H 0.2609 0.7825 0.2793 0.038 Uiso 1 1 calc R . . H26B H 0.2530 0.6560 0.2722 0.038 Uiso 1 1 calc R . . H26C H 0.2107 0.7177 0.3271 0.038 Uiso 1 1 calc R . . C27 C 0.33069(15) 0.8941(2) 0.15057(15) 0.0276(8) Uani 1 1 d . . . H27A H 0.3126 0.9151 0.1929 0.041 Uiso 1 1 calc R . . H27B H 0.3199 0.9507 0.1180 0.041 Uiso 1 1 calc R . . H27C H 0.3847 0.8821 0.1563 0.041 Uiso 1 1 calc R . . C28 C 0.34381(15) 0.6731(2) 0.16568(15) 0.0262(8) Uani 1 1 d . . . H28A H 0.3907 0.6669 0.1445 0.039 Uiso 1 1 calc R . . H28B H 0.3185 0.6040 0.1646 0.039 Uiso 1 1 calc R . . H28C H 0.3544 0.6958 0.2117 0.039 Uiso 1 1 calc R . . C29 C 0.31535(15) 0.7592(2) 0.03718(14) 0.0258(8) Uani 1 1 d . . . H29A H 0.3648 0.7931 0.0356 0.031 Uiso 1 1 calc R . . H29B H 0.3202 0.6830 0.0257 0.031 Uiso 1 1 calc R . . C30 C 0.25980(14) 0.8123(2) -0.01215(14) 0.0258(8) Uani 1 1 d . . . H30A H 0.2706 0.7939 -0.0578 0.031 Uiso 1 1 calc R . . H30B H 0.2622 0.8906 -0.0071 0.031 Uiso 1 1 calc R . . C31 C 0.10367(15) 0.8473(2) -0.04594(14) 0.0260(8) Uani 1 1 d . . . H31A H 0.1130 0.8383 -0.0925 0.039 Uiso 1 1 calc R . . H31B H 0.1117 0.9219 -0.0331 0.039 Uiso 1 1 calc R . . H31C H 0.0521 0.8272 -0.0397 0.039 Uiso 1 1 calc R . . C32 C 0.16131(15) 0.6415(2) -0.04409(14) 0.0250(7) Uani 1 1 d . . . H32A H 0.1094 0.6174 -0.0496 0.038 Uiso 1 1 calc R . . H32B H 0.1922 0.5861 -0.0216 0.038 Uiso 1 1 calc R . . H32C H 0.1793 0.6556 -0.0876 0.038 Uiso 1 1 calc R . . 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 0.0131(2) 0.0171(3) 0.0153(2) -0.0002(2) 0.00119(18) -0.00042(19) Fe2 0.0116(2) 0.0151(2) 0.0152(2) 0.0000(2) 0.00106(17) 0.00000(19) S1 0.0155(4) 0.0252(5) 0.0256(5) -0.0017(4) -0.0011(3) -0.0015(3) S2 0.0135(4) 0.0213(5) 0.0252(5) 0.0022(4) -0.0013(3) -0.0009(3) P1 0.0183(4) 0.0196(5) 0.0252(5) -0.0008(4) 0.0010(4) 0.0000(4) P2 0.0203(4) 0.0238(5) 0.0152(4) -0.0016(4) 0.0023(3) -0.0018(4) P3 0.0146(4) 0.0234(5) 0.0236(5) 0.0011(4) 0.0007(3) -0.0021(4) P4 0.0189(4) 0.0243(5) 0.0165(5) 0.0015(4) 0.0015(3) 0.0011(4) P5 0.0183(4) 0.0158(4) 0.0212(5) 0.0004(4) 0.0027(3) 0.0014(3) P6 0.0179(4) 0.0183(5) 0.0156(4) -0.0007(4) 0.0022(3) 0.0000(4) P7 0.0133(4) 0.0209(5) 0.0201(5) 0.0001(4) 0.0013(3) -0.0006(3) P8 0.0166(4) 0.0208(5) 0.0156(4) 0.0016(4) 0.0016(3) 0.0002(3) O1 0.0182(10) 0.0179(12) 0.0241(12) 0.0024(10) 0.0036(9) 0.0007(9) O2 0.0258(12) 0.0345(15) 0.0318(14) 0.0123(11) -0.0049(10) 0.0000(10) O3 0.0175(10) 0.0168(12) 0.0217(12) 0.0011(10) 0.0043(9) -0.0006(9) O4 0.0241(11) 0.0284(14) 0.0300(13) 0.0113(11) -0.0064(10) 0.0019(10) N1 0.0194(13) 0.0220(16) 0.0246(15) 0.0043(13) -0.0006(11) -0.0068(12) N2 0.0152(12) 0.0164(14) 0.0237(14) 0.0033(12) -0.0027(11) -0.0055(11) C1 0.0208(16) 0.0212(19) 0.0219(18) -0.0062(15) 0.0025(14) 0.0022(14) C2 0.0219(16) 0.0245(19) 0.0287(19) -0.0007(15) 0.0007(14) -0.0061(14) C3 0.0199(16) 0.0262(19) 0.0297(19) -0.0006(16) 0.0054(14) -0.0015(14) C4 0.0267(18) 0.031(2) 0.041(2) -0.0039(17) 0.0161(16) -0.0004(15) C5 0.0256(17) 0.029(2) 0.039(2) -0.0030(17) 0.0012(15) 0.0100(15) C6 0.0351(19) 0.026(2) 0.041(2) 0.0039(17) 0.0041(17) 0.0016(16) C7 0.0327(19) 0.0178(19) 0.029(2) -0.0055(16) 0.0009(15) 0.0052(15) C8 0.0319(18) 0.033(2) 0.0172(18) -0.0011(16) 0.0053(14) 0.0037(16) C9 0.0356(19) 0.035(2) 0.0202(18) -0.0005(15) 0.0075(15) -0.0097(16) C10 0.0280(18) 0.042(2) 0.0253(19) 0.0014(17) -0.0002(15) -0.0022(16) C11 0.0253(17) 0.028(2) 0.038(2) -0.0043(17) 0.0042(15) -0.0062(15) C12 0.0177(16) 0.036(2) 0.039(2) 0.0072(17) -0.0053(14) 0.0001(15) C13 0.0175(16) 0.032(2) 0.0295(19) -0.0004(16) 0.0035(14) -0.0032(14) C14 0.0234(16) 0.037(2) 0.0239(18) 0.0076(16) 0.0096(14) -0.0045(15) C15 0.0363(18) 0.034(2) 0.0207(18) 0.0064(16) 0.0025(15) 0.0060(16) C16 0.0286(17) 0.033(2) 0.0196(18) -0.0009(15) 0.0017(14) 0.0007(15) C17 0.0248(17) 0.0148(17) 0.0204(18) -0.0042(14) 0.0029(14) 0.0012(14) C18 0.0179(16) 0.028(2) 0.0224(18) -0.0007(15) -0.0006(14) -0.0071(14) C19 0.0234(16) 0.0218(18) 0.0285(19) 0.0011(15) 0.0034(14) -0.0030(14) C20 0.0377(19) 0.024(2) 0.041(2) -0.0022(17) 0.0084(17) -0.0083(16) C21 0.0252(17) 0.0220(19) 0.033(2) 0.0005(15) 0.0006(15) 0.0078(14) C22 0.0323(18) 0.0183(19) 0.038(2) 0.0008(16) 0.0098(16) 0.0006(14) C23 0.0261(17) 0.0223(19) 0.0255(19) -0.0071(15) 0.0034(15) 0.0039(14) C24 0.0246(17) 0.0276(19) 0.0205(18) -0.0032(15) 0.0056(14) 0.0057(14) C25 0.0349(18) 0.027(2) 0.0205(18) -0.0017(15) 0.0056(15) -0.0069(15) C26 0.0267(17) 0.033(2) 0.0166(17) 0.0020(15) -0.0022(14) 0.0021(15) C27 0.0198(16) 0.032(2) 0.031(2) -0.0024(16) 0.0013(14) -0.0067(14) C28 0.0212(16) 0.030(2) 0.0274(19) 0.0018(16) -0.0009(14) 0.0036(14) C29 0.0155(15) 0.034(2) 0.0288(19) -0.0007(16) 0.0061(14) -0.0010(14) C30 0.0243(16) 0.034(2) 0.0203(18) 0.0026(15) 0.0074(14) -0.0064(15) C31 0.0273(17) 0.031(2) 0.0189(18) 0.0025(15) -0.0011(14) 0.0029(15) C32 0.0264(17) 0.0255(19) 0.0234(18) -0.0006(15) 0.0030(14) 0.0031(14) _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 O1 2.053(2) . ? Fe1 P1 2.1821(13) . ? Fe1 P4 2.2238(14) . ? Fe1 P3 2.2366(13) . ? Fe1 P2 2.2668(14) . ? Fe1 S1 2.3354(13) . ? Fe2 O3 2.052(2) . ? Fe2 P5 2.1842(13) . ? Fe2 P8 2.2199(14) . ? Fe2 P7 2.2332(13) . ? Fe2 P6 2.2713(14) . ? Fe2 S2 2.3403(13) . ? S1 C2 1.833(3) . ? S2 C18 1.822(3) . ? P1 C5 1.826(3) . ? P1 C6 1.835(3) . ? P1 C7 1.841(3) . ? P2 C10 1.822(3) . ? P2 C9 1.823(3) . ? P2 C8 1.830(3) . ? P3 C12 1.820(3) . ? P3 C11 1.822(3) . ? P3 C13 1.844(3) . ? P4 C16 1.815(3) . ? P4 C15 1.827(3) . ? P4 C14 1.835(3) . ? P5 C21 1.828(3) . ? P5 C22 1.835(3) . ? P5 C23 1.835(3) . ? P6 C26 1.817(3) . ? P6 C25 1.818(3) . ? P6 C24 1.827(3) . ? P7 C28 1.824(3) . ? P7 C27 1.832(3) . ? P7 C29 1.852(3) . ? P8 C31 1.820(3) . ? P8 C32 1.822(3) . ? P8 C30 1.838(3) . ? O1 C1 1.286(3) . ? O2 C1 1.246(3) . ? O3 C17 1.294(3) . ? O4 C17 1.244(3) . ? N1 C1 1.385(3) . ? N1 C3 1.443(3) . ? N1 C2 1.446(3) . ? N2 C17 1.378(3) . ? N2 C18 1.435(3) . ? N2 C19 1.458(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.517(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.513(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.512(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.504(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.527(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.512(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 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 O1 Fe1 P1 178.77(6) . . ? O1 Fe1 P4 87.94(6) . . ? P1 Fe1 P4 93.19(4) . . ? O1 Fe1 P3 80.42(6) . . ? P1 Fe1 P3 99.15(4) . . ? P4 Fe1 P3 85.87(3) . . ? O1 Fe1 P2 94.00(6) . . ? P1 Fe1 P2 84.91(4) . . ? P4 Fe1 P2 175.73(4) . . ? P3 Fe1 P2 98.20(4) . . ? O1 Fe1 S1 88.58(6) . . ? P1 Fe1 S1 91.98(4) . . ? P4 Fe1 S1 86.95(4) . . ? P3 Fe1 S1 167.06(4) . . ? P2 Fe1 S1 89.29(4) . . ? O3 Fe2 P5 178.33(6) . . ? O3 Fe2 P8 88.60(6) . . ? P5 Fe2 P8 93.04(3) . . ? O3 Fe2 P7 81.47(6) . . ? P5 Fe2 P7 98.89(4) . . ? P8 Fe2 P7 85.96(3) . . ? O3 Fe2 P6 93.49(6) . . ? P5 Fe2 P6 84.85(3) . . ? P8 Fe2 P6 176.55(4) . . ? P7 Fe2 P6 97.05(3) . . ? O3 Fe2 S2 88.10(6) . . ? P5 Fe2 S2 91.73(4) . . ? P8 Fe2 S2 86.99(3) . . ? P7 Fe2 S2 167.54(4) . . ? P6 Fe2 S2 90.35(3) . . ? C2 S1 Fe1 100.52(9) . . ? C18 S2 Fe2 101.11(9) . . ? C5 P1 C6 99.23(14) . . ? C5 P1 C7 100.41(14) . . ? C6 P1 C7 100.74(14) . . ? C5 P1 Fe1 117.45(10) . . ? C6 P1 Fe1 125.01(11) . . ? C7 P1 Fe1 110.27(10) . . ? C10 P2 C9 99.82(14) . . ? C10 P2 C8 102.08(15) . . ? C9 P2 C8 100.38(15) . . ? C10 P2 Fe1 120.62(10) . . ? C9 P2 Fe1 121.96(10) . . ? C8 P2 Fe1 108.64(10) . . ? C12 P3 C11 99.69(15) . . ? C12 P3 C13 100.64(14) . . ? C11 P3 C13 101.15(14) . . ? C12 P3 Fe1 119.61(10) . . ? C11 P3 Fe1 125.07(10) . . ? C13 P3 Fe1 106.85(9) . . ? C16 P4 C15 99.64(14) . . ? C16 P4 C14 100.90(14) . . ? C15 P4 C14 103.63(13) . . ? C16 P4 Fe1 118.86(10) . . ? C15 P4 Fe1 121.49(10) . . ? C14 P4 Fe1 109.54(10) . . ? C21 P5 C22 98.81(14) . . ? C21 P5 C23 100.50(14) . . ? C22 P5 C23 100.15(14) . . ? C21 P5 Fe2 117.49(10) . . ? C22 P5 Fe2 125.52(10) . . ? C23 P5 Fe2 110.49(10) . . ? C26 P6 C25 99.49(14) . . ? C26 P6 C24 102.33(14) . . ? C25 P6 C24 101.04(14) . . ? C26 P6 Fe2 120.48(10) . . ? C25 P6 Fe2 121.69(10) . . ? C24 P6 Fe2 108.70(10) . . ? C28 P7 C27 99.97(15) . . ? C28 P7 C29 100.79(14) . . ? C27 P7 C29 101.56(14) . . ? C28 P7 Fe2 119.85(10) . . ? C27 P7 Fe2 123.80(10) . . ? C29 P7 Fe2 107.31(9) . . ? C31 P8 C32 99.77(14) . . ? C31 P8 C30 103.44(13) . . ? C32 P8 C30 101.04(13) . . ? C31 P8 Fe2 121.83(10) . . ? C32 P8 Fe2 118.23(10) . . ? C30 P8 Fe2 109.75(10) . . ? C1 O1 Fe1 123.34(18) . . ? C17 O3 Fe2 123.39(18) . . ? C1 N1 C3 121.1(3) . . ? C1 N1 C2 118.3(2) . . ? C3 N1 C2 120.0(2) . . ? C17 N2 C18 119.3(2) . . ? C17 N2 C19 120.3(2) . . ? C18 N2 C19 119.9(2) . . ? O2 C1 O1 125.4(3) . . ? O2 C1 N1 119.0(3) . . ? O1 C1 N1 115.7(3) . . ? N1 C2 S1 115.8(2) . . ? N1 C2 H2A 108.3 . . ? S1 C2 H2A 108.3 . . ? N1 C2 H2B 108.3 . . ? S1 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? N1 C3 C4 114.0(2) . . ? N1 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P1 C5 H5A 109.5 . . ? P1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P1 C6 H6A 109.5 . . ? P1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 P1 106.9(2) . . ? C8 C7 H7A 110.3 . . ? P1 C7 H7A 110.3 . . ? C8 C7 H7B 110.3 . . ? P1 C7 H7B 110.3 . . ? H7A C7 H7B 108.6 . . ? C7 C8 P2 109.5(2) . . ? C7 C8 H8A 109.8 . . ? P2 C8 H8A 109.8 . . ? C7 C8 H8B 109.8 . . ? P2 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? P2 C9 H9A 109.5 . . ? P2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P2 C10 H10A 109.5 . . ? P2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P3 C11 H11A 109.5 . . ? P3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P3 C12 H12A 109.5 . . ? P3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P3 109.9(2) . . ? C14 C13 H13A 109.7 . . ? P3 C13 H13A 109.7 . . ? C14 C13 H13B 109.7 . . ? P3 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C13 C14 P4 106.24(19) . . ? C13 C14 H14A 110.5 . . ? P4 C14 H14A 110.5 . . ? C13 C14 H14B 110.5 . . ? P4 C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? P4 C15 H15A 109.5 . . ? P4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P4 C16 H16A 109.5 . . ? P4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C17 O3 124.5(3) . . ? O4 C17 N2 120.1(3) . . ? O3 C17 N2 115.4(3) . . ? N2 C18 S2 116.0(2) . . ? N2 C18 H18A 108.3 . . ? S2 C18 H18A 108.3 . . ? N2 C18 H18B 108.3 . . ? S2 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? N2 C19 C20 113.3(2) . . ? N2 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? N2 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P5 C21 H21A 109.5 . . ? P5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P5 C22 H22A 109.5 . . ? P5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 P5 106.8(2) . . ? C24 C23 H23A 110.4 . . ? P5 C23 H23A 110.4 . . ? C24 C23 H23B 110.4 . . ? P5 C23 H23B 110.4 . . ? H23A C23 H23B 108.6 . . ? C23 C24 P6 109.5(2) . . ? C23 C24 H24A 109.8 . . ? P6 C24 H24A 109.8 . . ? C23 C24 H24B 109.8 . . ? P6 C24 H24B 109.8 . . ? H24A C24 H24B 108.2 . . ? P6 C25 H25A 109.5 . . ? P6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? P6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? P6 C26 H26A 109.5 . . ? P6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? P7 C27 H27A 109.5 . . ? P7 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? P7 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? P7 C28 H28A 109.5 . . ? P7 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? P7 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 P7 110.00(19) . . ? C30 C29 H29A 109.7 . . ? P7 C29 H29A 109.7 . . ? C30 C29 H29B 109.7 . . ? P7 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C29 C30 P8 106.62(19) . . ? C29 C30 H30A 110.4 . . ? P8 C30 H30A 110.4 . . ? C29 C30 H30B 110.4 . . ? P8 C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? P8 C31 H31A 109.5 . . ? P8 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P8 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? P8 C32 H32A 109.5 . . ? P8 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P8 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 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 O1 Fe1 S1 C2 -2.80(11) . . . . ? P1 Fe1 S1 C2 178.30(10) . . . . ? P4 Fe1 S1 C2 85.21(10) . . . . ? P3 Fe1 S1 C2 28.8(2) . . . . ? P2 Fe1 S1 C2 -96.82(10) . . . . ? O3 Fe2 S2 C18 -2.03(11) . . . . ? P5 Fe2 S2 C18 179.62(10) . . . . ? P8 Fe2 S2 C18 86.67(10) . . . . ? P7 Fe2 S2 C18 31.1(2) . . . . ? P6 Fe2 S2 C18 -95.52(10) . . . . ? O1 Fe1 P1 C5 -125(3) . . . . ? P4 Fe1 P1 C5 79.26(13) . . . . ? P3 Fe1 P1 C5 165.58(12) . . . . ? P2 Fe1 P1 C5 -96.91(12) . . . . ? S1 Fe1 P1 C5 -7.80(12) . . . . ? O1 Fe1 P1 C6 109(3) . . . . ? P4 Fe1 P1 C6 -46.52(13) . . . . ? P3 Fe1 P1 C6 39.80(13) . . . . ? P2 Fe1 P1 C6 137.31(13) . . . . ? S1 Fe1 P1 C6 -133.58(13) . . . . ? O1 Fe1 P1 C7 -11(3) . . . . ? P4 Fe1 P1 C7 -166.61(11) . . . . ? P3 Fe1 P1 C7 -80.28(11) . . . . ? P2 Fe1 P1 C7 17.23(11) . . . . ? S1 Fe1 P1 C7 106.34(11) . . . . ? O1 Fe1 P2 C10 68.51(13) . . . . ? P1 Fe1 P2 C10 -110.92(13) . . . . ? P4 Fe1 P2 C10 -174.7(5) . . . . ? P3 Fe1 P2 C10 -12.38(13) . . . . ? S1 Fe1 P2 C10 157.03(13) . . . . ? O1 Fe1 P2 C9 -58.58(14) . . . . ? P1 Fe1 P2 C9 122.00(13) . . . . ? P4 Fe1 P2 C9 58.3(6) . . . . ? P3 Fe1 P2 C9 -139.46(12) . . . . ? S1 Fe1 P2 C9 29.95(13) . . . . ? O1 Fe1 P2 C8 -174.33(12) . . . . ? P1 Fe1 P2 C8 6.24(11) . . . . ? P4 Fe1 P2 C8 -57.5(6) . . . . ? P3 Fe1 P2 C8 104.78(11) . . . . ? S1 Fe1 P2 C8 -85.81(11) . . . . ? O1 Fe1 P3 C12 -37.07(14) . . . . ? P1 Fe1 P3 C12 141.76(13) . . . . ? P4 Fe1 P3 C12 -125.67(13) . . . . ? P2 Fe1 P3 C12 55.63(13) . . . . ? S1 Fe1 P3 C12 -69.2(2) . . . . ? O1 Fe1 P3 C11 -166.51(14) . . . . ? P1 Fe1 P3 C11 12.31(14) . . . . ? P4 Fe1 P3 C11 104.88(13) . . . . ? P2 Fe1 P3 C11 -73.81(13) . . . . ? S1 Fe1 P3 C11 161.35(19) . . . . ? O1 Fe1 P3 C13 76.13(12) . . . . ? P1 Fe1 P3 C13 -105.04(11) . . . . ? P4 Fe1 P3 C13 -12.47(11) . . . . ? P2 Fe1 P3 C13 168.84(11) . . . . ? S1 Fe1 P3 C13 44.0(2) . . . . ? O1 Fe1 P4 C16 22.70(12) . . . . ? P1 Fe1 P4 C16 -157.81(11) . . . . ? P3 Fe1 P4 C16 103.24(11) . . . . ? P2 Fe1 P4 C16 -94.3(5) . . . . ? S1 Fe1 P4 C16 -65.99(11) . . . . ? O1 Fe1 P4 C15 146.86(13) . . . . ? P1 Fe1 P4 C15 -33.64(12) . . . . ? P3 Fe1 P4 C15 -132.60(13) . . . . ? P2 Fe1 P4 C15 29.8(6) . . . . ? S1 Fe1 P4 C15 58.18(13) . . . . ? O1 Fe1 P4 C14 -92.43(12) . . . . ? P1 Fe1 P4 C14 87.07(11) . . . . ? P3 Fe1 P4 C14 -11.89(11) . . . . ? P2 Fe1 P4 C14 150.5(5) . . . . ? S1 Fe1 P4 C14 178.89(11) . . . . ? O3 Fe2 P5 C21 -91(2) . . . . ? P8 Fe2 P5 C21 80.34(12) . . . . ? P7 Fe2 P5 C21 166.73(12) . . . . ? P6 Fe2 P5 C21 -96.92(12) . . . . ? S2 Fe2 P5 C21 -6.73(12) . . . . ? O3 Fe2 P5 C22 143(2) . . . . ? P8 Fe2 P5 C22 -45.36(13) . . . . ? P7 Fe2 P5 C22 41.02(13) . . . . ? P6 Fe2 P5 C22 137.37(13) . . . . ? S2 Fe2 P5 C22 -132.44(13) . . . . ? O3 Fe2 P5 C23 24(2) . . . . ? P8 Fe2 P5 C23 -165.22(10) . . . . ? P7 Fe2 P5 C23 -78.84(10) . . . . ? P6 Fe2 P5 C23 17.52(10) . . . . ? S2 Fe2 P5 C23 107.71(10) . . . . ? O3 Fe2 P6 C26 68.84(13) . . . . ? P5 Fe2 P6 C26 -111.34(12) . . . . ? P8 Fe2 P6 C26 -163.8(6) . . . . ? P7 Fe2 P6 C26 -12.99(12) . . . . ? S2 Fe2 P6 C26 156.96(12) . . . . ? O3 Fe2 P6 C25 -57.20(14) . . . . ? P5 Fe2 P6 C25 122.62(13) . . . . ? P8 Fe2 P6 C25 70.1(7) . . . . ? P7 Fe2 P6 C25 -139.03(12) . . . . ? S2 Fe2 P6 C25 30.92(12) . . . . ? O3 Fe2 P6 C24 -173.72(11) . . . . ? P5 Fe2 P6 C24 6.10(10) . . . . ? P8 Fe2 P6 C24 -46.4(7) . . . . ? P7 Fe2 P6 C24 104.45(11) . . . . ? S2 Fe2 P6 C24 -85.60(11) . . . . ? O3 Fe2 P7 C28 -35.88(13) . . . . ? P5 Fe2 P7 C28 142.48(12) . . . . ? P8 Fe2 P7 C28 -125.07(12) . . . . ? P6 Fe2 P7 C28 56.62(12) . . . . ? S2 Fe2 P7 C28 -69.4(2) . . . . ? O3 Fe2 P7 C27 -164.52(13) . . . . ? P5 Fe2 P7 C27 13.83(13) . . . . ? P8 Fe2 P7 C27 106.29(12) . . . . ? P6 Fe2 P7 C27 -72.03(13) . . . . ? S2 Fe2 P7 C27 161.96(18) . . . . ? O3 Fe2 P7 C29 78.01(12) . . . . ? P5 Fe2 P7 C29 -103.63(11) . . . . ? P8 Fe2 P7 C29 -11.18(11) . . . . ? P6 Fe2 P7 C29 170.51(11) . . . . ? S2 Fe2 P7 C29 44.5(2) . . . . ? O3 Fe2 P8 C31 145.01(13) . . . . ? P5 Fe2 P8 C31 -34.73(12) . . . . ? P7 Fe2 P8 C31 -133.44(12) . . . . ? P6 Fe2 P8 C31 17.6(7) . . . . ? S2 Fe2 P8 C31 56.84(12) . . . . ? O3 Fe2 P8 C32 20.97(12) . . . . ? P5 Fe2 P8 C32 -158.77(11) . . . . ? P7 Fe2 P8 C32 102.52(11) . . . . ? P6 Fe2 P8 C32 -106.5(7) . . . . ? S2 Fe2 P8 C32 -67.20(11) . . . . ? O3 Fe2 P8 C30 -94.09(12) . . . . ? P5 Fe2 P8 C30 86.16(11) . . . . ? P7 Fe2 P8 C30 -12.54(11) . . . . ? P6 Fe2 P8 C30 138.5(6) . . . . ? S2 Fe2 P8 C30 177.74(11) . . . . ? P1 Fe1 O1 C1 60(3) . . . . ? P4 Fe1 O1 C1 -143.7(2) . . . . ? P3 Fe1 O1 C1 130.1(2) . . . . ? P2 Fe1 O1 C1 32.5(2) . . . . ? S1 Fe1 O1 C1 -56.7(2) . . . . ? P5 Fe2 O3 C17 27(2) . . . . ? P8 Fe2 O3 C17 -143.9(2) . . . . ? P7 Fe2 O3 C17 129.9(2) . . . . ? P6 Fe2 O3 C17 33.3(2) . . . . ? S2 Fe2 O3 C17 -56.9(2) . . . . ? Fe1 O1 C1 O2 -115.6(3) . . . . ? Fe1 O1 C1 N1 65.6(3) . . . . ? C3 N1 C1 O2 -2.3(4) . . . . ? C2 N1 C1 O2 -174.4(3) . . . . ? C3 N1 C1 O1 176.5(2) . . . . ? C2 N1 C1 O1 4.4(4) . . . . ? C1 N1 C2 S1 -68.4(3) . . . . ? C3 N1 C2 S1 119.4(2) . . . . ? Fe1 S1 C2 N1 54.2(2) . . . . ? C1 N1 C3 C4 -83.2(3) . . . . ? C2 N1 C3 C4 88.8(3) . . . . ? C5 P1 C7 C8 82.2(2) . . . . ? C6 P1 C7 C8 -176.2(2) . . . . ? Fe1 P1 C7 C8 -42.4(2) . . . . ? P1 C7 C8 P2 47.1(2) . . . . ? C10 P2 C8 C7 94.4(2) . . . . ? C9 P2 C8 C7 -163.1(2) . . . . ? Fe1 P2 C8 C7 -34.0(2) . . . . ? C12 P3 C13 C14 166.6(2) . . . . ? C11 P3 C13 C14 -91.2(2) . . . . ? Fe1 P3 C13 C14 41.0(2) . . . . ? P3 C13 C14 P4 -50.2(2) . . . . ? C16 P4 C14 C13 -87.0(2) . . . . ? C15 P4 C14 C13 170.2(2) . . . . ? Fe1 P4 C14 C13 39.2(2) . . . . ? Fe2 O3 C17 O4 -114.4(3) . . . . ? Fe2 O3 C17 N2 65.5(3) . . . . ? C18 N2 C17 O4 -175.4(3) . . . . ? C19 N2 C17 O4 -4.0(4) . . . . ? C18 N2 C17 O3 4.7(4) . . . . ? C19 N2 C17 O3 176.1(2) . . . . ? C17 N2 C18 S2 -67.8(3) . . . . ? C19 N2 C18 S2 120.9(2) . . . . ? Fe2 S2 C18 N2 53.0(2) . . . . ? C17 N2 C19 C20 -85.0(3) . . . . ? C18 N2 C19 C20 86.2(3) . . . . ? C21 P5 C23 C24 82.4(2) . . . . ? C22 P5 C23 C24 -176.59(19) . . . . ? Fe2 P5 C23 C24 -42.4(2) . . . . ? P5 C23 C24 P6 46.9(2) . . . . ? C26 P6 C24 C23 94.8(2) . . . . ? C25 P6 C24 C23 -162.8(2) . . . . ? Fe2 P6 C24 C23 -33.7(2) . . . . ? C28 P7 C29 C30 165.2(2) . . . . ? C27 P7 C29 C30 -92.2(2) . . . . ? Fe2 P7 C29 C30 39.0(2) . . . . ? P7 C29 C30 P8 -48.6(2) . . . . ? C31 P8 C30 C29 170.4(2) . . . . ? C32 P8 C30 C29 -86.6(2) . . . . ? Fe2 P8 C30 C29 39.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.614 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.074