Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 _publ_section_title ; Enhanced substitutional lability of [Fe(CO)~2~{P(OPh)~3~}~2~(\n^2^-PHCCPh)]: facile insertion of CO and organoisocyanides into iron-alkyne bonds. ; loop_ _publ_author_name _publ_author_address 'Barrow, M.' ; Department of Chemistry, University College Dublin, Belfield, Dublin 4, Ireland ; 'Cromhout, N.L.' ; Department of Chemistry, University College Dublin, Belfield, Dublin 4, Ireland ; 'Manning, A.R.' ; Department of Chemistry, University College Dublin, Belfield, Dublin 4, Ireland ; 'Gallagher, J.F.' ; School of Chemical Sciences, Dublin City University, Dublin 9, Ireland ; data_NLC-23 _database_code_CSD 154303 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H25 Fe O8 P' _chemical_formula_weight 684.39 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' '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.508(3) _cell_length_b 10.766(3) _cell_length_c 16.973(7) _cell_angle_alpha 83.97(3) _cell_angle_beta 84.64(2) _cell_angle_gamma 66.84(2) _cell_volume 1586.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 13.85 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.99 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 4 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 5932 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_sigmaI/netI 0.132 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 25.2 _reflns_number_total 5572 _reflns_number_gt 2863 _reflns_threshold_expression >2\s(I) _computing_data_collection XSCANS (Siemens, 1998) _computing_cell_refinement XSCANS (Siemens, 1998) _computing_data_reduction XSCANS (Siemens, 1998) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material NRCVAX, PREP8 _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 w=1/[\s^2^(Fo^2^)+(0.044P)^2^+0.0P] 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 5572 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.158 _refine_ls_R_factor_gt 0.068 _refine_ls_wR_factor_ref 0.137 _refine_ls_wR_factor_gt 0.108 _refine_ls_goodness_of_fit_ref 0.99 _refine_ls_restrained_S_all 0.99 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.04308(10) 0.39648(8) 0.70205(5) 0.0413(3) Uani 1 d . . . P1 P 0.26888(17) 0.24873(14) 0.73543(8) 0.0370(4) Uani 1 d . . . O1 O -0.2762(6) 0.5228(5) 0.6597(3) 0.0914(17) Uani 1 d . . . C1 C -0.1513(8) 0.4788(6) 0.6763(3) 0.0570(17) Uani 1 d . . . O2 O 0.0188(6) 0.6262(4) 0.7944(3) 0.0877(16) Uani 1 d . . . C2 C 0.0349(7) 0.5366(6) 0.7600(3) 0.0541(17) Uani 1 d . . . O3 O 0.1493(5) 0.5003(4) 0.5492(3) 0.0761(14) Uani 1 d . . . C3 C 0.1158(7) 0.4586(5) 0.6080(4) 0.0511(16) Uani 1 d . . . O11 O 0.3818(4) 0.2966(4) 0.77759(19) 0.0460(10) Uani 1 d . . . C11 C 0.3393(6) 0.3742(5) 0.8444(3) 0.0399(14) Uani 1 d . . . C12 C 0.2498(6) 0.3503(6) 0.9071(3) 0.0512(16) Uani 1 d . . . H12 H 0.2121 0.2827 0.9065 0.061 Uiso 1 calc R . . C13 C 0.2161(7) 0.4285(6) 0.9718(3) 0.0568(17) Uani 1 d . . . H13 H 0.1561 0.4128 1.0151 0.068 Uiso 1 calc R . . C14 C 0.2702(9) 0.5270(7) 0.9720(4) 0.073(2) Uani 1 d . . . H14 H 0.2463 0.5799 1.0151 0.088 Uiso 1 calc R . . C15 C 0.3594(9) 0.5491(7) 0.9095(4) 0.088(3) Uani 1 d . . . H15 H 0.3971 0.6167 0.9104 0.106 Uiso 1 calc R . . C16 C 0.3949(7) 0.4731(6) 0.8447(4) 0.0643(19) Uani 1 d . . . H16 H 0.4558 0.4889 0.8019 0.077 Uiso 1 calc R . . O21 O 0.3881(4) 0.1661(3) 0.66901(19) 0.0452(10) Uani 1 d . . . C21 C 0.4461(6) 0.2160(5) 0.5993(3) 0.0394(14) Uani 1 d . . . C22 C 0.5281(7) 0.2940(6) 0.6026(3) 0.0497(15) Uani 1 d . . . H22 H 0.5402 0.3223 0.6505 0.060 Uiso 1 calc R . . C23 C 0.5932(7) 0.3299(6) 0.5317(4) 0.0654(19) Uani 1 d . . . H23 H 0.6508 0.3824 0.5323 0.078 Uiso 1 calc R . . C24 C 0.5742(8) 0.2898(7) 0.4612(4) 0.068(2) Uani 1 d . . . H24 H 0.6171 0.3156 0.4141 0.082 Uiso 1 calc R . . C25 C 0.4913(7) 0.2110(7) 0.4608(3) 0.0642(19) Uani 1 d . . . H25 H 0.4787 0.1828 0.4130 0.077 Uiso 1 calc R . . C26 C 0.4259(7) 0.1728(6) 0.5302(3) 0.0507(16) Uani 1 d . . . H26 H 0.3696 0.1191 0.5298 0.061 Uiso 1 calc R . . O31 O 0.2606(4) 0.1238(3) 0.79175(19) 0.0404(9) Uani 1 d . . . C31 C 0.3814(6) -0.0033(5) 0.8008(3) 0.0374(13) Uani 1 d . . . C32 C 0.4970(7) -0.0266(6) 0.8492(3) 0.0476(15) Uani 1 d . . . H32 H 0.5012 0.0439 0.8749 0.057 Uiso 1 calc R . . C33 C 0.6075(7) -0.1555(7) 0.8598(4) 0.0620(18) Uani 1 d . . . H33 H 0.6866 -0.1721 0.8929 0.074 Uiso 1 calc R . . C34 C 0.6016(8) -0.2600(7) 0.8215(4) 0.0638(19) Uani 1 d . . . H34 H 0.6754 -0.3473 0.8293 0.077 Uiso 1 calc R . . C35 C 0.4860(8) -0.2343(6) 0.7720(4) 0.0569(17) Uani 1 d . . . H35 H 0.4829 -0.3043 0.7454 0.068 Uiso 1 calc R . . C36 C 0.3742(6) -0.1059(6) 0.7611(3) 0.0451(15) Uani 1 d . . . H36 H 0.2955 -0.0888 0.7276 0.054 Uiso 1 calc R . . O6 O 0.0606(5) 0.2223(4) 0.5815(2) 0.0633(13) Uani 1 d . . . C6 C 0.0264(6) 0.2421(5) 0.6512(3) 0.0391(14) Uani 1 d . . . O7 O -0.0854(5) 0.3663(4) 0.8591(2) 0.0642(13) Uani 1 d . . . C7 C -0.0477(6) 0.3181(5) 0.7956(3) 0.0415(14) Uani 1 d . . . C4 C -0.0393(5) 0.1565(5) 0.7049(3) 0.0362(13) Uani 1 d . . . C5 C -0.0709(6) 0.1921(5) 0.7808(3) 0.0371(13) Uani 1 d . . . C41 C -0.0669(6) 0.0448(5) 0.6737(3) 0.0355(13) Uani 1 d . . . C42 C 0.0356(6) -0.0362(5) 0.6173(3) 0.0447(15) Uani 1 d . . . H42 H 0.1249 -0.0230 0.6005 0.054 Uiso 1 calc R . . C43 C 0.0043(7) -0.1358(6) 0.5865(3) 0.0506(16) Uani 1 d . . . H43 H 0.0747 -0.1908 0.5503 0.061 Uiso 1 calc R . . C44 C -0.1277(7) -0.1549(6) 0.6083(3) 0.0567(17) Uani 1 d . . . H44 H -0.1486 -0.2204 0.5857 0.068 Uiso 1 calc R . . C45 C -0.2302(7) -0.0767(6) 0.6641(3) 0.0499(16) Uani 1 d . . . H45 H -0.3191 -0.0911 0.6804 0.060 Uiso 1 calc R . . C46 C -0.2002(6) 0.0228(6) 0.6953(3) 0.0433(14) Uani 1 d . . . H46 H -0.2710 0.0766 0.7319 0.052 Uiso 1 calc R . . C51 C -0.1168(6) 0.1168(6) 0.8493(3) 0.0389(13) Uani 1 d . . . C52 C -0.0323(7) -0.0165(6) 0.8683(3) 0.0519(16) Uani 1 d . . . H52 H 0.0523 -0.0623 0.8353 0.062 Uiso 1 calc R . . C53 C -0.0682(8) -0.0859(7) 0.9350(4) 0.071(2) Uani 1 d . . . H53 H -0.0074 -0.1765 0.9472 0.086 Uiso 1 calc R . . C54 C -0.1942(10) -0.0198(9) 0.9831(4) 0.080(2) Uani 1 d . . . H54 H -0.2196 -0.0656 1.0281 0.096 Uiso 1 calc R . . C55 C -0.2826(8) 0.1135(8) 0.9648(3) 0.070(2) Uani 1 d . . . H55 H -0.3688 0.1578 0.9972 0.084 Uiso 1 calc R . . C56 C -0.2454(6) 0.1827(6) 0.8990(3) 0.0518(16) Uani 1 d . . . H56 H -0.3057 0.2736 0.8875 0.062 Uiso 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 0.0434(6) 0.0369(5) 0.0419(5) -0.0102(4) 0.0026(4) -0.0131(4) P1 0.0417(10) 0.0354(8) 0.0346(8) -0.0087(7) 0.0067(7) -0.0161(8) O1 0.056(3) 0.095(4) 0.100(4) -0.028(3) -0.025(3) 0.005(3) C1 0.064(5) 0.053(4) 0.050(4) -0.013(3) -0.007(4) -0.015(4) O2 0.101(4) 0.051(3) 0.103(4) -0.035(3) -0.030(3) -0.009(3) C2 0.053(4) 0.045(4) 0.062(4) -0.009(3) -0.007(3) -0.014(3) O3 0.077(4) 0.071(3) 0.069(3) 0.016(3) 0.006(3) -0.024(3) C3 0.058(4) 0.030(3) 0.058(4) 0.005(3) 0.005(3) -0.012(3) O11 0.044(2) 0.053(2) 0.046(2) -0.0204(19) 0.0118(19) -0.024(2) C11 0.041(4) 0.048(4) 0.031(3) -0.012(3) 0.003(3) -0.017(3) C12 0.059(4) 0.056(4) 0.043(3) -0.009(3) 0.002(3) -0.026(3) C13 0.058(4) 0.072(5) 0.034(3) -0.009(3) 0.006(3) -0.020(4) C14 0.103(6) 0.077(5) 0.050(4) -0.027(4) 0.002(4) -0.043(5) C15 0.132(7) 0.102(6) 0.068(5) -0.043(4) 0.025(5) -0.083(6) C16 0.077(5) 0.077(5) 0.060(4) -0.024(4) 0.017(4) -0.053(4) O21 0.048(2) 0.041(2) 0.041(2) -0.0129(18) 0.0155(19) -0.014(2) C21 0.042(4) 0.039(3) 0.032(3) -0.008(3) 0.011(3) -0.012(3) C22 0.053(4) 0.056(4) 0.042(3) -0.008(3) 0.004(3) -0.023(3) C23 0.056(5) 0.075(5) 0.070(5) -0.001(4) 0.008(4) -0.034(4) C24 0.067(5) 0.089(5) 0.046(4) 0.002(4) 0.018(4) -0.034(4) C25 0.068(5) 0.089(5) 0.033(4) -0.009(3) 0.011(3) -0.030(4) C26 0.055(4) 0.062(4) 0.038(3) -0.010(3) 0.006(3) -0.026(3) O31 0.038(2) 0.039(2) 0.040(2) -0.0039(17) 0.0096(18) -0.013(2) C31 0.036(4) 0.040(3) 0.031(3) 0.000(3) 0.012(3) -0.014(3) C32 0.047(4) 0.053(4) 0.047(4) -0.009(3) 0.000(3) -0.023(3) C33 0.049(4) 0.063(5) 0.061(4) 0.015(4) -0.012(3) -0.011(4) C34 0.052(5) 0.046(4) 0.078(5) 0.003(4) 0.012(4) -0.007(4) C35 0.063(5) 0.040(4) 0.065(4) -0.014(3) 0.015(4) -0.019(4) C36 0.042(4) 0.049(4) 0.048(3) -0.006(3) 0.006(3) -0.023(3) O6 0.096(4) 0.080(3) 0.033(2) -0.019(2) 0.018(2) -0.057(3) C6 0.038(4) 0.043(3) 0.038(3) -0.008(3) 0.002(3) -0.018(3) O7 0.081(3) 0.081(3) 0.051(2) -0.043(2) 0.030(2) -0.052(3) C7 0.039(4) 0.041(3) 0.045(3) -0.018(3) 0.009(3) -0.014(3) C4 0.025(3) 0.044(3) 0.038(3) -0.016(3) 0.003(3) -0.009(3) C5 0.030(3) 0.046(3) 0.036(3) -0.016(3) 0.008(3) -0.015(3) C41 0.037(3) 0.036(3) 0.028(3) -0.005(2) -0.001(3) -0.008(3) C42 0.035(3) 0.058(4) 0.045(3) -0.019(3) 0.009(3) -0.020(3) C43 0.052(4) 0.052(4) 0.046(4) -0.024(3) 0.005(3) -0.015(3) C44 0.068(5) 0.055(4) 0.057(4) -0.018(3) -0.006(4) -0.030(4) C45 0.047(4) 0.062(4) 0.055(4) -0.007(3) -0.001(3) -0.036(3) C46 0.037(4) 0.056(4) 0.040(3) -0.013(3) 0.005(3) -0.020(3) C51 0.036(3) 0.049(4) 0.034(3) -0.009(3) 0.003(3) -0.018(3) C52 0.054(4) 0.057(4) 0.045(4) -0.005(3) 0.005(3) -0.022(4) C53 0.078(6) 0.072(5) 0.064(5) -0.001(4) -0.007(4) -0.029(4) C54 0.126(8) 0.099(6) 0.050(4) -0.002(4) 0.010(5) -0.084(6) C55 0.093(6) 0.100(6) 0.043(4) -0.026(4) 0.035(4) -0.069(5) C56 0.044(4) 0.062(4) 0.054(4) -0.021(3) 0.011(3) -0.024(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 C1 1.781(7) . ? Fe1 C3 1.846(6) . ? Fe1 C2 1.859(6) . ? Fe1 C7 2.003(5) . ? Fe1 C6 2.017(5) . ? Fe1 P1 2.1937(19) . ? P1 O21 1.589(3) . ? P1 O31 1.590(4) . ? P1 O11 1.608(4) . ? O1 C1 1.143(6) . ? O2 C2 1.131(6) . ? O3 C3 1.123(6) . ? O11 C11 1.413(5) . ? C11 C16 1.363(7) . ? C11 C12 1.366(7) . ? C12 C13 1.390(7) . ? C12 H12 0.9300 . ? C13 C14 1.349(8) . ? C13 H13 0.9300 . ? C14 C15 1.356(8) . ? C14 H14 0.9300 . ? C15 C16 1.377(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? O21 C21 1.404(6) . ? C21 C22 1.360(7) . ? C21 C26 1.363(7) . ? C22 C23 1.390(7) . ? C22 H22 0.9300 . ? C23 C24 1.363(8) . ? C23 H23 0.9300 . ? C24 C25 1.367(8) . ? C24 H24 0.9300 . ? C25 C26 1.380(7) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? O31 C31 1.403(6) . ? C31 C32 1.363(7) . ? C31 C36 1.379(7) . ? C32 C33 1.377(8) . ? C32 H32 0.9300 . ? C33 C34 1.380(8) . ? C33 H33 0.9300 . ? C34 C35 1.369(8) . ? C34 H34 0.9300 . ? C35 C36 1.380(7) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? O6 C6 1.215(5) . ? C6 C4 1.496(7) . ? O7 C7 1.208(5) . ? C7 C5 1.507(7) . ? C4 C5 1.356(6) . ? C4 C41 1.483(7) . ? C5 C51 1.478(7) . ? C41 C46 1.389(7) . ? C41 C42 1.400(6) . ? C42 C43 1.381(7) . ? C42 H42 0.9300 . ? C43 C44 1.362(7) . ? C43 H43 0.9300 . ? C44 C45 1.380(7) . ? C44 H44 0.9300 . ? C45 C46 1.378(7) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C52 1.361(7) . ? C51 C56 1.401(7) . ? C52 C53 1.381(8) . ? C52 H52 0.9300 . ? C53 C54 1.370(9) . ? C53 H53 0.9300 . ? C54 C55 1.367(9) . ? C54 H54 0.9300 . ? C55 C56 1.373(7) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? 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 C1 Fe1 C3 92.9(3) . . ? C1 Fe1 C2 93.8(3) . . ? C3 Fe1 C2 95.6(3) . . ? C1 Fe1 C7 83.4(3) . . ? C3 Fe1 C7 172.7(2) . . ? C2 Fe1 C7 90.9(2) . . ? C1 Fe1 C6 82.0(2) . . ? C3 Fe1 C6 92.3(2) . . ? C2 Fe1 C6 171.2(2) . . ? C7 Fe1 C6 81.0(2) . . ? C1 Fe1 P1 165.3(2) . . ? C3 Fe1 P1 94.66(19) . . ? C2 Fe1 P1 98.01(19) . . ? C7 Fe1 P1 87.73(16) . . ? C6 Fe1 P1 85.15(16) . . ? O21 P1 O31 98.25(19) . . ? O21 P1 O11 98.08(19) . . ? O31 P1 O11 104.41(19) . . ? O21 P1 Fe1 119.55(15) . . ? O31 P1 Fe1 113.18(15) . . ? O11 P1 Fe1 120.04(15) . . ? O1 C1 Fe1 175.2(6) . . ? O2 C2 Fe1 175.0(6) . . ? O3 C3 Fe1 175.0(6) . . ? C11 O11 P1 124.6(3) . . ? C16 C11 C12 121.0(5) . . ? C16 C11 O11 116.8(5) . . ? C12 C11 O11 122.2(5) . . ? C11 C12 C13 119.0(6) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 120.2(6) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.2(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.9(6) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C11 C16 C15 118.8(6) . . ? C11 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C21 O21 P1 128.6(3) . . ? C22 C21 C26 122.8(5) . . ? C22 C21 O21 120.9(5) . . ? C26 C21 O21 116.1(5) . . ? C21 C22 C23 117.6(5) . . ? C21 C22 H22 121.2 . . ? C23 C22 H22 121.2 . . ? C24 C23 C22 121.3(6) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 119.1(6) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C24 C25 C26 121.2(6) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C21 C26 C25 118.0(6) . . ? C21 C26 H26 121.0 . . ? C25 C26 H26 121.0 . . ? C31 O31 P1 124.8(3) . . ? C32 C31 C36 121.3(5) . . ? C32 C31 O31 121.8(5) . . ? C36 C31 O31 116.8(5) . . ? C31 C32 C33 119.4(6) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C32 C33 C34 120.3(6) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C35 C34 C33 119.5(6) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 120.9(6) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C31 C36 C35 118.7(6) . . ? C31 C36 H36 120.7 . . ? C35 C36 H36 120.7 . . ? O6 C6 C4 121.8(5) . . ? O6 C6 Fe1 123.2(4) . . ? C4 C6 Fe1 115.0(3) . . ? O7 C7 C5 120.7(5) . . ? O7 C7 Fe1 124.7(4) . . ? C5 C7 Fe1 114.5(3) . . ? C5 C4 C41 125.3(5) . . ? C5 C4 C6 114.2(5) . . ? C41 C4 C6 120.5(4) . . ? C4 C5 C51 126.8(5) . . ? C4 C5 C7 115.0(5) . . ? C51 C5 C7 118.1(4) . . ? C46 C41 C42 117.5(5) . . ? C46 C41 C4 121.2(4) . . ? C42 C41 C4 121.2(5) . . ? C43 C42 C41 120.2(5) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 121.2(5) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 119.7(5) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C46 C45 C44 119.6(5) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C41 121.8(5) . . ? C45 C46 H46 119.1 . . ? C41 C46 H46 119.1 . . ? C52 C51 C56 117.9(5) . . ? C52 C51 C5 121.4(5) . . ? C56 C51 C5 120.7(5) . . ? C51 C52 C53 122.1(6) . . ? C51 C52 H52 119.0 . . ? C53 C52 H52 119.0 . . ? C54 C53 C52 119.3(7) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C55 C54 C53 119.9(7) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C54 C55 C56 120.6(6) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C55 C56 C51 120.2(6) . . ? C55 C56 H56 119.9 . . ? C51 C56 H56 119.9 . . ? 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 C1 Fe1 P1 O21 82.1(8) . . . . ? C3 Fe1 P1 O21 -38.5(2) . . . . ? C2 Fe1 P1 O21 -134.9(2) . . . . ? C7 Fe1 P1 O21 134.6(2) . . . . ? C6 Fe1 P1 O21 53.4(2) . . . . ? C1 Fe1 P1 O31 -32.9(8) . . . . ? C3 Fe1 P1 O31 -153.5(2) . . . . ? C2 Fe1 P1 O31 110.2(2) . . . . ? C7 Fe1 P1 O31 19.6(2) . . . . ? C6 Fe1 P1 O31 -61.5(2) . . . . ? C1 Fe1 P1 O11 -157.0(8) . . . . ? C3 Fe1 P1 O11 82.4(2) . . . . ? C2 Fe1 P1 O11 -13.9(2) . . . . ? C7 Fe1 P1 O11 -104.4(2) . . . . ? C6 Fe1 P1 O11 174.4(2) . . . . ? C3 Fe1 C1 O1 115(7) . . . . ? C2 Fe1 C1 O1 -149(7) . . . . ? C7 Fe1 C1 O1 -59(7) . . . . ? C6 Fe1 C1 O1 23(7) . . . . ? P1 Fe1 C1 O1 -6(8) . . . . ? C1 Fe1 C2 O2 6(7) . . . . ? C3 Fe1 C2 O2 99(6) . . . . ? C7 Fe1 C2 O2 -78(6) . . . . ? C6 Fe1 C2 O2 -55(7) . . . . ? P1 Fe1 C2 O2 -165(6) . . . . ? C1 Fe1 C3 O3 -4(6) . . . . ? C2 Fe1 C3 O3 -98(6) . . . . ? C7 Fe1 C3 O3 54(7) . . . . ? C6 Fe1 C3 O3 78(6) . . . . ? P1 Fe1 C3 O3 163(6) . . . . ? O21 P1 O11 C11 -178.6(4) . . . . ? O31 P1 O11 C11 -77.9(4) . . . . ? Fe1 P1 O11 C11 50.3(4) . . . . ? P1 O11 C11 C16 -139.9(5) . . . . ? P1 O11 C11 C12 41.7(7) . . . . ? C16 C11 C12 C13 -0.1(9) . . . . ? O11 C11 C12 C13 178.3(5) . . . . ? C11 C12 C13 C14 0.5(9) . . . . ? C12 C13 C14 C15 -0.8(11) . . . . ? C13 C14 C15 C16 0.7(12) . . . . ? C12 C11 C16 C15 -0.1(10) . . . . ? O11 C11 C16 C15 -178.5(6) . . . . ? C14 C15 C16 C11 -0.2(11) . . . . ? O31 P1 O21 C21 179.1(4) . . . . ? O11 P1 O21 C21 -75.0(4) . . . . ? Fe1 P1 O21 C21 56.5(5) . . . . ? P1 O21 C21 C22 61.3(7) . . . . ? P1 O21 C21 C26 -123.7(5) . . . . ? C26 C21 C22 C23 -0.1(9) . . . . ? O21 C21 C22 C23 174.5(5) . . . . ? C21 C22 C23 C24 0.7(9) . . . . ? C22 C23 C24 C25 -0.9(10) . . . . ? C23 C24 C25 C26 0.5(10) . . . . ? C22 C21 C26 C25 -0.3(9) . . . . ? O21 C21 C26 C25 -175.2(5) . . . . ? C24 C25 C26 C21 0.1(9) . . . . ? O21 P1 O31 C31 30.5(4) . . . . ? O11 P1 O31 C31 -70.1(4) . . . . ? Fe1 P1 O31 C31 157.7(3) . . . . ? P1 O31 C31 C32 80.9(5) . . . . ? P1 O31 C31 C36 -102.0(5) . . . . ? C36 C31 C32 C33 -1.1(8) . . . . ? O31 C31 C32 C33 175.9(5) . . . . ? C31 C32 C33 C34 0.2(9) . . . . ? C32 C33 C34 C35 0.9(9) . . . . ? C33 C34 C35 C36 -1.2(9) . . . . ? C32 C31 C36 C35 0.8(8) . . . . ? O31 C31 C36 C35 -176.3(5) . . . . ? C34 C35 C36 C31 0.3(8) . . . . ? C1 Fe1 C6 O6 92.6(5) . . . . ? C3 Fe1 C6 O6 0.0(5) . . . . ? C2 Fe1 C6 O6 154.1(14) . . . . ? C7 Fe1 C6 O6 177.1(5) . . . . ? P1 Fe1 C6 O6 -94.5(5) . . . . ? C1 Fe1 C6 C4 -84.5(4) . . . . ? C3 Fe1 C6 C4 -177.0(4) . . . . ? C2 Fe1 C6 C4 -23.0(18) . . . . ? C7 Fe1 C6 C4 0.0(4) . . . . ? P1 Fe1 C6 C4 88.5(4) . . . . ? C1 Fe1 C7 O7 -92.9(5) . . . . ? C3 Fe1 C7 O7 -151.8(17) . . . . ? C2 Fe1 C7 O7 0.8(5) . . . . ? C6 Fe1 C7 O7 -175.7(5) . . . . ? P1 Fe1 C7 O7 98.8(5) . . . . ? C1 Fe1 C7 C5 85.6(4) . . . . ? C3 Fe1 C7 C5 27(2) . . . . ? C2 Fe1 C7 C5 179.3(4) . . . . ? C6 Fe1 C7 C5 2.7(4) . . . . ? P1 Fe1 C7 C5 -82.8(4) . . . . ? O6 C6 C4 C5 179.9(5) . . . . ? Fe1 C6 C4 C5 -3.0(6) . . . . ? O6 C6 C4 C41 -0.9(8) . . . . ? Fe1 C6 C4 C41 176.2(4) . . . . ? C41 C4 C5 C51 9.5(9) . . . . ? C6 C4 C5 C51 -171.4(5) . . . . ? C41 C4 C5 C7 -173.9(5) . . . . ? C6 C4 C5 C7 5.2(7) . . . . ? O7 C7 C5 C4 173.2(5) . . . . ? Fe1 C7 C5 C4 -5.3(6) . . . . ? O7 C7 C5 C51 -9.9(8) . . . . ? Fe1 C7 C5 C51 171.6(4) . . . . ? C5 C4 C41 C46 41.7(8) . . . . ? C6 C4 C41 C46 -137.5(5) . . . . ? C5 C4 C41 C42 -142.8(5) . . . . ? C6 C4 C41 C42 38.1(7) . . . . ? C46 C41 C42 C43 -1.4(8) . . . . ? C4 C41 C42 C43 -177.1(5) . . . . ? C41 C42 C43 C44 1.9(9) . . . . ? C42 C43 C44 C45 -2.2(9) . . . . ? C43 C44 C45 C46 2.0(9) . . . . ? C44 C45 C46 C41 -1.6(9) . . . . ? C42 C41 C46 C45 1.3(8) . . . . ? C4 C41 C46 C45 177.0(5) . . . . ? C4 C5 C51 C52 53.2(8) . . . . ? C7 C5 C51 C52 -123.3(6) . . . . ? C4 C5 C51 C56 -129.8(6) . . . . ? C7 C5 C51 C56 53.6(7) . . . . ? C56 C51 C52 C53 -1.3(9) . . . . ? C5 C51 C52 C53 175.7(5) . . . . ? C51 C52 C53 C54 1.2(10) . . . . ? C52 C53 C54 C55 -0.1(10) . . . . ? C53 C54 C55 C56 -0.8(10) . . . . ? C54 C55 C56 C51 0.7(9) . . . . ? C52 C51 C56 C55 0.3(8) . . . . ? C5 C51 C56 C55 -176.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C14 H14 O7 0.93 2.49 3.284(7) 143.8 2_567 C22 H22 O11 0.93 2.57 3.159(6) 121.8 . C42 H42 O6 0.93 2.46 2.883(7) 107.9 . C45 H45 C31 0.93 3.22 4.017(8) 144.7 1_455 C45 H45 C32 0.93 3.21 3.825(8) 125.8 1_455 C45 H45 C33 0.93 3.13 3.690(8) 120.7 1_455 C45 H45 C34 0.93 3.07 3.765(8) 132.6 1_455 C45 H45 C35 0.93 3.07 3.942(8) 156.5 1_455 C45 H45 C36 0.93 3.16 4.077(8) 169.5 1_455 _diffrn_measured_fraction_theta_max 1.00 _diffrn_reflns_theta_full 25.2 _diffrn_measured_fraction_theta_full 1.00 _refine_diff_density_max 0.30 _refine_diff_density_min -0.29 _refine_diff_density_rms 0.07