Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Evamarie Hey-Hawkins' _publ_contact_author_address ; Department of Inorganic Chemistry Universitat Leipzig Faculty of Chemistry and Mineralogy Leipzig Saxony 04103 GERMANY ; _publ_contact_author_email HEY@RZ.UNI-LEIPZIG.DE _publ_section_title ; Aminoalkylferrocenyldichlorophosphanes: Facile Synthesis of Versatile Chiral Starting Materials ; loop_ _publ_author_name E.Hey-Hawkins P.Lonnecke S.Tschirschwitz #------------------------------------------------------------------------------# # DATA BLOCK # #------------------------------------------------------------------------------# data_c2252fin _database_code_depnum_ccdc_archive 'CCDC 617193' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 Cl2 Fe N P' _chemical_formula_weight 358.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.2995(12) _cell_length_b 11.9091(16) _cell_length_c 15.662(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1548.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4404 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 28.29 _exptl_crystal_description 'small plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Bruker CCD area detector' _diffrn_measurement_method '\F and \W scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11360 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.33 _reflns_number_total 3683 _reflns_number_gt 3509 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (Giacovazzo 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0405P)^2^+0.0399P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(11) _refine_ls_number_reflns 3683 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0570 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.08987(3) 0.112663(18) 0.633400(14) 0.02716(7) Uani 1 1 d . . . Cl1 Cl -0.19960(6) 0.04983(5) 0.82237(4) 0.04989(13) Uani 1 1 d . . . Cl2 Cl 0.09186(8) 0.04808(5) 0.94788(3) 0.05057(13) Uani 1 1 d . . . P1 P 0.01954(6) 0.14310(4) 0.84292(3) 0.03436(11) Uani 1 1 d . . . N1 N 0.29758(19) 0.23792(13) 0.85265(10) 0.0347(3) Uani 1 1 d . . . C1 C 0.1322(2) 0.07892(13) 0.75880(11) 0.0275(3) Uani 1 1 d . . . C2 C 0.2656(2) 0.13875(14) 0.72177(11) 0.0298(3) Uani 1 1 d . . . C3 C 0.3274(2) 0.07293(17) 0.65385(12) 0.0370(4) Uani 1 1 d . . . C4 C 0.2324(2) -0.02679(16) 0.64826(12) 0.0372(4) Uani 1 1 d . . . C5 C 0.1127(2) -0.02369(13) 0.71228(11) 0.0316(4) Uani 1 1 d . . . C6 C -0.0794(3) 0.23677(16) 0.62178(13) 0.0446(5) Uani 1 1 d . . . C7 C 0.0568(3) 0.26094(18) 0.56988(16) 0.0517(6) Uani 1 1 d . . . C8 C 0.0745(3) 0.1720(2) 0.51120(13) 0.0502(5) Uani 1 1 d . . . C9 C -0.0503(3) 0.09320(17) 0.52646(12) 0.0419(5) Uani 1 1 d . . . C10 C -0.1447(2) 0.13297(16) 0.59478(13) 0.0377(4) Uani 1 1 d . . . C11 C 0.3168(2) 0.25047(15) 0.75886(12) 0.0352(4) Uani 1 1 d . . . C12 C 0.4813(3) 0.2892(3) 0.72745(17) 0.0558(6) Uani 1 1 d . . . C13 C 0.2802(3) 0.3462(2) 0.89594(17) 0.0501(5) Uani 1 1 d . . . C14 C 0.4266(3) 0.17184(19) 0.89144(14) 0.0450(5) Uani 1 1 d . . . H3 H 0.407(3) 0.0908(19) 0.6219(14) 0.038(6) Uiso 1 1 d . . . H4 H 0.241(3) -0.080(2) 0.6091(17) 0.049(7) Uiso 1 1 d . . . H5 H 0.035(3) -0.0789(17) 0.7234(14) 0.032(5) Uiso 1 1 d . . . H6 H -0.105(4) 0.283(3) 0.663(2) 0.083(10) Uiso 1 1 d . . . H7 H 0.130(3) 0.321(2) 0.5761(16) 0.054(7) Uiso 1 1 d . . . H8 H 0.159(4) 0.158(2) 0.4673(18) 0.061(8) Uiso 1 1 d . . . H9 H -0.071(3) 0.022(2) 0.4965(16) 0.050(7) Uiso 1 1 d . . . H10 H -0.246(3) 0.1049(19) 0.6169(14) 0.035(6) Uiso 1 1 d . . . H11 H 0.230(3) 0.3032(18) 0.7461(14) 0.034(5) Uiso 1 1 d . . . H12A H 0.477(4) 0.303(3) 0.669(2) 0.087(11) Uiso 1 1 d . . . H12B H 0.558(4) 0.233(3) 0.733(2) 0.079(11) Uiso 1 1 d . . . H12C H 0.509(4) 0.352(3) 0.757(2) 0.079(10) Uiso 1 1 d . . . H13A H 0.180(3) 0.389(2) 0.8783(17) 0.055(7) Uiso 1 1 d . . . H13B H 0.379(4) 0.390(2) 0.896(2) 0.071(9) Uiso 1 1 d . . . H13C H 0.257(3) 0.337(2) 0.954(2) 0.065(9) Uiso 1 1 d . . . H14A H 0.528(3) 0.214(2) 0.8826(17) 0.058(8) Uiso 1 1 d . . . H14B H 0.440(3) 0.101(2) 0.8599(15) 0.046(6) Uiso 1 1 d . . . H14C H 0.402(4) 0.159(2) 0.9502(18) 0.060(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.03074(12) 0.02932(11) 0.02141(11) 0.00289(8) -0.00268(10) 0.00174(9) Cl1 0.0343(2) 0.0619(3) 0.0534(3) 0.0053(3) 0.0086(2) -0.0008(2) Cl2 0.0685(3) 0.0588(3) 0.0244(2) 0.00869(18) 0.0004(2) -0.0004(3) P1 0.0378(2) 0.0365(2) 0.0288(2) 0.00005(17) 0.00432(18) 0.00925(18) N1 0.0367(8) 0.0377(7) 0.0297(8) -0.0029(6) -0.0077(7) 0.0071(6) C1 0.0295(9) 0.0303(7) 0.0226(8) 0.0030(6) -0.0015(6) 0.0051(6) C2 0.0294(8) 0.0365(8) 0.0235(8) 0.0029(6) -0.0035(6) 0.0018(6) C3 0.0319(10) 0.0494(10) 0.0296(9) 0.0016(8) 0.0026(8) 0.0088(7) C4 0.0439(10) 0.0404(9) 0.0273(9) -0.0034(7) -0.0028(8) 0.0122(7) C5 0.0374(10) 0.0298(8) 0.0276(8) 0.0035(6) -0.0050(8) 0.0059(7) C6 0.0561(12) 0.0339(9) 0.0438(11) -0.0016(7) -0.0186(10) 0.0136(8) C7 0.0596(14) 0.0389(10) 0.0566(13) 0.0189(10) -0.0246(11) -0.0105(9) C8 0.0509(12) 0.0689(14) 0.0309(10) 0.0205(9) -0.0050(10) 0.0002(11) C9 0.0518(12) 0.0430(10) 0.0309(9) -0.0017(8) -0.0146(9) 0.0045(8) C10 0.0359(9) 0.0398(9) 0.0373(10) 0.0074(8) -0.0104(8) 0.0018(7) C11 0.0376(10) 0.0373(9) 0.0306(9) 0.0031(7) -0.0062(8) -0.0034(8) C12 0.0501(14) 0.0710(16) 0.0463(13) 0.0046(12) -0.0028(11) -0.0249(12) C13 0.0553(14) 0.0463(11) 0.0488(13) -0.0156(10) -0.0140(11) 0.0074(10) C14 0.0407(11) 0.0574(12) 0.0369(10) 0.0009(9) -0.0101(9) 0.0117(9) _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 C2 2.0343(17) . ? Fe1 C1 2.0354(17) . ? Fe1 C8 2.0444(19) . ? Fe1 C7 2.045(2) . ? Fe1 C6 2.0475(19) . ? Fe1 C5 2.0492(16) . ? Fe1 C4 2.0524(18) . ? Fe1 C9 2.0525(19) . ? Fe1 C10 2.053(2) . ? Fe1 C3 2.0528(19) . ? Cl1 P1 2.1553(8) . ? Cl2 P1 2.0841(7) . ? P1 C1 1.7874(17) . ? N1 C14 1.461(2) . ? N1 C13 1.464(3) . ? N1 C11 1.485(2) . ? C1 C5 1.432(2) . ? C1 C2 1.438(2) . ? C2 C3 1.418(3) . ? C2 C11 1.513(2) . ? C3 C4 1.428(3) . ? C3 H3 0.85(2) . ? C4 C5 1.412(3) . ? C4 H4 0.89(3) . ? C5 H5 0.93(2) . ? C6 C10 1.414(3) . ? C6 C7 1.422(4) . ? C6 H6 0.87(3) . ? C7 C8 1.410(4) . ? C7 H7 0.95(3) . ? C8 C9 1.419(3) . ? C8 H8 0.99(3) . ? C9 C10 1.408(3) . ? C9 H9 0.98(2) . ? C10 H10 0.97(2) . ? C11 C12 1.523(3) . ? C11 H11 0.98(2) . ? C12 H12A 0.94(4) . ? C12 H12B 0.93(3) . ? C12 H12C 0.91(4) . ? C13 H13A 1.01(3) . ? C13 H13B 0.97(3) . ? C13 H13C 0.94(3) . ? C14 H14A 0.99(3) . ? C14 H14B 0.98(2) . ? C14 H14C 0.95(3) . ? 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 C2 Fe1 C1 41.39(7) . . ? C2 Fe1 C8 128.96(9) . . ? C1 Fe1 C8 169.25(8) . . ? C2 Fe1 C7 107.16(8) . . ? C1 Fe1 C7 131.53(8) . . ? C8 Fe1 C7 40.32(10) . . ? C2 Fe1 C6 116.24(7) . . ? C1 Fe1 C6 110.30(8) . . ? C8 Fe1 C6 67.93(10) . . ? C7 Fe1 C6 40.67(10) . . ? C2 Fe1 C5 69.18(7) . . ? C1 Fe1 C5 41.04(7) . . ? C8 Fe1 C5 147.60(9) . . ? C7 Fe1 C5 171.83(9) . . ? C6 Fe1 C5 133.56(9) . . ? C2 Fe1 C4 68.48(7) . . ? C1 Fe1 C4 68.36(7) . . ? C8 Fe1 C4 114.96(9) . . ? C7 Fe1 C4 146.21(10) . . ? C6 Fe1 C4 171.83(9) . . ? C5 Fe1 C4 40.27(8) . . ? C2 Fe1 C9 168.17(8) . . ? C1 Fe1 C9 149.67(8) . . ? C8 Fe1 C9 40.52(9) . . ? C7 Fe1 C9 67.95(9) . . ? C6 Fe1 C9 67.66(8) . . ? C5 Fe1 C9 117.06(8) . . ? C4 Fe1 C9 109.15(8) . . ? C2 Fe1 C10 149.57(8) . . ? C1 Fe1 C10 118.13(8) . . ? C8 Fe1 C10 67.93(9) . . ? C7 Fe1 C10 68.15(8) . . ? C6 Fe1 C10 40.35(8) . . ? C5 Fe1 C10 111.03(8) . . ? C4 Fe1 C10 132.49(8) . . ? C9 Fe1 C10 40.12(9) . . ? C2 Fe1 C3 40.59(7) . . ? C1 Fe1 C3 68.78(7) . . ? C8 Fe1 C3 106.60(9) . . ? C7 Fe1 C3 113.80(9) . . ? C6 Fe1 C3 147.08(9) . . ? C5 Fe1 C3 68.55(8) . . ? C4 Fe1 C3 40.72(8) . . ? C9 Fe1 C3 130.22(8) . . ? C10 Fe1 C3 169.73(8) . . ? C1 P1 Cl2 101.45(6) . . ? C1 P1 Cl1 96.38(6) . . ? Cl2 P1 Cl1 94.64(3) . . ? C14 N1 C13 110.74(16) . . ? C14 N1 C11 112.74(16) . . ? C13 N1 C11 112.34(17) . . ? C5 C1 C2 107.74(16) . . ? C5 C1 P1 132.91(14) . . ? C2 C1 P1 119.21(13) . . ? C5 C1 Fe1 70.00(10) . . ? C2 C1 Fe1 69.27(10) . . ? P1 C1 Fe1 122.44(8) . . ? C3 C2 C1 107.90(16) . . ? C3 C2 C11 132.26(17) . . ? C1 C2 C11 119.82(16) . . ? C3 C2 Fe1 70.40(10) . . ? C1 C2 Fe1 69.34(10) . . ? C11 C2 Fe1 126.67(12) . . ? C2 C3 C4 107.81(17) . . ? C2 C3 Fe1 69.01(10) . . ? C4 C3 Fe1 69.63(11) . . ? C2 C3 H3 125.5(15) . . ? C4 C3 H3 126.7(15) . . ? Fe1 C3 H3 126.3(14) . . ? C5 C4 C3 108.85(16) . . ? C5 C4 Fe1 69.74(10) . . ? C3 C4 Fe1 69.65(10) . . ? C5 C4 H4 124.7(16) . . ? C3 C4 H4 126.3(16) . . ? Fe1 C4 H4 123.4(16) . . ? C4 C5 C1 107.70(17) . . ? C4 C5 Fe1 69.99(10) . . ? C1 C5 Fe1 68.96(9) . . ? C4 C5 H5 126.6(13) . . ? C1 C5 H5 125.7(13) . . ? Fe1 C5 H5 127.3(13) . . ? C10 C6 C7 108.1(2) . . ? C10 C6 Fe1 70.02(11) . . ? C7 C6 Fe1 69.58(12) . . ? C10 C6 H6 133(2) . . ? C7 C6 H6 119(2) . . ? Fe1 C6 H6 124(2) . . ? C8 C7 C6 107.67(19) . . ? C8 C7 Fe1 69.81(11) . . ? C6 C7 Fe1 69.75(11) . . ? C8 C7 H7 124.8(16) . . ? C6 C7 H7 127.2(16) . . ? Fe1 C7 H7 121.4(16) . . ? C7 C8 C9 108.1(2) . . ? C7 C8 Fe1 69.87(12) . . ? C9 C8 Fe1 70.05(11) . . ? C7 C8 H8 130.6(16) . . ? C9 C8 H8 121.2(16) . . ? Fe1 C8 H8 123.1(16) . . ? C10 C9 C8 108.16(19) . . ? C10 C9 Fe1 69.95(11) . . ? C8 C9 Fe1 69.44(11) . . ? C10 C9 H9 123.6(15) . . ? C8 C9 H9 128.3(15) . . ? Fe1 C9 H9 126.0(14) . . ? C9 C10 C6 108.0(2) . . ? C9 C10 Fe1 69.93(12) . . ? C6 C10 Fe1 69.62(11) . . ? C9 C10 H10 129.7(14) . . ? C6 C10 H10 121.8(14) . . ? Fe1 C10 H10 132.5(13) . . ? N1 C11 C2 105.13(14) . . ? N1 C11 C12 116.52(17) . . ? C2 C11 C12 113.25(19) . . ? N1 C11 H11 100.8(13) . . ? C2 C11 H11 106.2(13) . . ? C12 C11 H11 113.7(13) . . ? C11 C12 H12A 109(2) . . ? C11 C12 H12B 111(2) . . ? H12A C12 H12B 104(3) . . ? C11 C12 H12C 109(2) . . ? H12A C12 H12C 111(3) . . ? H12B C12 H12C 112(3) . . ? N1 C13 H13A 113.4(15) . . ? N1 C13 H13B 113.0(18) . . ? H13A C13 H13B 115(2) . . ? N1 C13 H13C 111.4(18) . . ? H13A C13 H13C 99(2) . . ? H13B C13 H13C 104(3) . . ? N1 C14 H14A 106.8(15) . . ? N1 C14 H14B 109.5(13) . . ? H14A C14 H14B 106(2) . . ? N1 C14 H14C 109.2(17) . . ? H14A C14 H14C 114(2) . . ? H14B C14 H14C 112(2) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.176 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.065 #------------------------------------------------------------------------------# # NEXT STRUCTURE # #------------------------------------------------------------------------------# data_s032_fin _database_code_depnum_ccdc_archive 'CCDC 617194' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H16 Cl2 Fe N P' _chemical_formula_weight 343.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 10.2696(10) _cell_length_b 10.7620(9) _cell_length_c 13.4203(13) _cell_angle_alpha 90.00 _cell_angle_beta 100.198(12) _cell_angle_gamma 90.00 _cell_volume 1459.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 30.20 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.489 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6371 _exptl_absorpt_correction_T_max 0.7156 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'Stoe IPDS area detector' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22880 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 30.38 _reflns_number_total 4071 _reflns_number_gt 2763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0365P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4071 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0599 _refine_ls_wR_factor_gt 0.0573 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _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 0.069308(18) 0.759290(19) 0.233509(18) 0.02891(7) Uani 1 1 d . . . Cl1 Cl -0.42296(4) 0.73772(5) 0.14657(4) 0.05034(13) Uani 1 1 d . . . Cl2 Cl -0.23929(6) 0.89073(4) 0.02543(4) 0.05493(14) Uani 1 1 d . . . P1 P -0.24759(4) 0.84408(3) 0.18293(3) 0.02971(10) Uani 1 1 d . . . N1 N -0.23321(12) 0.78955(12) 0.36124(11) 0.0317(3) Uani 1 1 d . . . C1 C -0.12747(13) 0.72085(12) 0.19279(12) 0.0256(3) Uani 1 1 d . . . C2 C -0.07706(12) 0.66438(12) 0.28867(12) 0.0272(3) Uani 1 1 d . . . C3 C 0.02591(14) 0.58109(14) 0.27409(15) 0.0357(4) Uani 1 1 d . . . C4 C 0.03946(15) 0.58541(15) 0.17080(16) 0.0393(4) Uani 1 1 d . . . C5 C -0.05422(15) 0.67114(15) 0.11939(15) 0.0337(4) Uani 1 1 d . . . C6 C 0.10120(19) 0.94525(17) 0.26404(18) 0.0491(5) Uani 1 1 d . . . C7 C 0.16996(17) 0.87205(17) 0.34470(17) 0.0452(4) Uani 1 1 d . . . C8 C 0.25899(16) 0.79432(19) 0.30415(17) 0.0465(5) Uani 1 1 d . . . C9 C 0.24587(17) 0.8191(2) 0.20008(18) 0.0508(5) Uani 1 1 d . . . C10 C 0.14770(19) 0.91210(19) 0.17435(19) 0.0520(5) Uani 1 1 d . . . C11 C -0.13897(17) 0.68397(16) 0.37991(14) 0.0353(4) Uani 1 1 d . . . C12 C -0.35966(19) 0.7626(3) 0.3943(2) 0.0540(5) Uani 1 1 d . . . C13 C -0.1761(2) 0.90409(18) 0.41012(18) 0.0464(4) Uani 1 1 d . . . H3 H 0.0755(16) 0.5362(17) 0.3272(14) 0.035(5) Uiso 1 1 d . . . H4 H 0.1033(17) 0.5423(17) 0.1422(14) 0.040(5) Uiso 1 1 d . . . H5 H -0.0644(15) 0.6949(16) 0.0538(14) 0.031(5) Uiso 1 1 d . . . H6 H 0.0375(18) 1.0041(18) 0.2705(15) 0.044(5) Uiso 1 1 d . . . H7 H 0.155(2) 0.8723(19) 0.4110(18) 0.053(6) Uiso 1 1 d . . . H8 H 0.315(2) 0.734(2) 0.347(2) 0.070(7) Uiso 1 1 d . . . H9 H 0.287(2) 0.776(2) 0.1498(19) 0.060(6) Uiso 1 1 d . . . H10 H 0.114(2) 0.943(2) 0.1122(19) 0.061(7) Uiso 1 1 d . . . H11A H -0.0733(18) 0.7023(17) 0.4388(15) 0.039(5) Uiso 1 1 d . . . H11B H -0.1879(17) 0.6104(18) 0.3919(14) 0.042(5) Uiso 1 1 d . . . H12A H -0.345(2) 0.7520(19) 0.466(2) 0.058(6) Uiso 1 1 d . . . H12B H -0.387(2) 0.687(2) 0.3647(17) 0.052(6) Uiso 1 1 d . . . H12C H -0.421(2) 0.835(2) 0.3717(18) 0.065(7) Uiso 1 1 d . . . H13A H -0.168(2) 0.898(2) 0.481(2) 0.066(7) Uiso 1 1 d . . . H13B H -0.240(2) 0.975(2) 0.3889(16) 0.057(6) Uiso 1 1 d . . . H13C H -0.092(2) 0.9211(19) 0.3900(17) 0.061(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01988(9) 0.02668(11) 0.04078(15) -0.00139(9) 0.00701(8) -0.00335(8) Cl1 0.02367(17) 0.0639(3) 0.0597(3) -0.0039(2) -0.00300(17) 0.00049(17) Cl2 0.0899(4) 0.0440(3) 0.0323(3) 0.00860(19) 0.0149(2) 0.0164(2) P1 0.03234(18) 0.02430(18) 0.0324(3) 0.00176(15) 0.00560(16) 0.00511(14) N1 0.0309(6) 0.0323(7) 0.0334(9) 0.0018(5) 0.0101(6) 0.0012(5) C1 0.0198(6) 0.0240(7) 0.0331(9) -0.0026(6) 0.0051(5) -0.0011(5) C2 0.0210(6) 0.0208(6) 0.0389(10) 0.0013(6) 0.0029(6) -0.0034(5) C3 0.0253(7) 0.0229(7) 0.0566(13) 0.0022(7) 0.0015(7) 0.0024(5) C4 0.0292(7) 0.0311(8) 0.0588(13) -0.0123(8) 0.0113(8) 0.0027(6) C5 0.0295(7) 0.0357(8) 0.0368(12) -0.0099(7) 0.0085(7) -0.0022(6) C6 0.0436(9) 0.0289(9) 0.0769(16) -0.0045(9) 0.0161(10) -0.0130(7) C7 0.0404(9) 0.0460(10) 0.0496(13) -0.0104(9) 0.0091(9) -0.0214(8) C8 0.0235(7) 0.0531(11) 0.0609(15) -0.0018(9) 0.0020(8) -0.0114(7) C9 0.0297(8) 0.0625(12) 0.0645(15) -0.0060(10) 0.0203(9) -0.0171(8) C10 0.0475(10) 0.0498(11) 0.0591(16) 0.0140(10) 0.0107(10) -0.0211(8) C11 0.0390(8) 0.0315(8) 0.0356(11) 0.0085(7) 0.0074(8) 0.0016(6) C12 0.0390(9) 0.0761(16) 0.0516(15) 0.0101(12) 0.0206(9) 0.0006(10) C13 0.0615(12) 0.0373(10) 0.0403(14) -0.0066(8) 0.0088(10) 0.0021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 2.0403(13) . ? Fe1 C5 2.0413(17) . ? Fe1 C8 2.0449(17) . ? Fe1 C9 2.0473(16) . ? Fe1 C10 2.0517(18) . ? Fe1 C4 2.0524(16) . ? Fe1 C7 2.0547(19) . ? Fe1 C6 2.0574(18) . ? Fe1 C2 2.0603(13) . ? Fe1 C3 2.0637(16) . ? Cl1 P1 2.1167(6) . ? Cl2 P1 2.1887(7) . ? P1 C1 1.8000(14) . ? N1 C13 1.469(2) . ? N1 C12 1.474(2) . ? N1 C11 1.485(2) . ? C1 C2 1.434(2) . ? C1 C5 1.444(2) . ? C2 C3 1.426(2) . ? C2 C11 1.491(2) . ? C3 C4 1.418(3) . ? C4 C5 1.420(2) . ? C6 C10 1.417(3) . ? C6 C7 1.421(3) . ? C7 C8 1.417(3) . ? C8 C9 1.405(3) . ? C9 C10 1.419(3) . ? 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 C5 41.44(6) . . ? C1 Fe1 C8 168.14(8) . . ? C5 Fe1 C8 147.99(7) . . ? C1 Fe1 C9 151.49(8) . . ? C5 Fe1 C9 116.02(8) . . ? C8 Fe1 C9 40.15(9) . . ? C1 Fe1 C10 119.79(8) . . ? C5 Fe1 C10 108.45(9) . . ? C8 Fe1 C10 67.96(9) . . ? C9 Fe1 C10 40.51(8) . . ? C1 Fe1 C4 68.68(6) . . ? C5 Fe1 C4 40.60(7) . . ? C8 Fe1 C4 114.77(7) . . ? C9 Fe1 C4 105.70(8) . . ? C10 Fe1 C4 127.77(9) . . ? C1 Fe1 C7 131.40(7) . . ? C5 Fe1 C7 170.16(7) . . ? C8 Fe1 C7 40.44(8) . . ? C9 Fe1 C7 67.80(8) . . ? C10 Fe1 C7 68.05(9) . . ? C4 Fe1 C7 148.83(8) . . ? C1 Fe1 C6 111.46(7) . . ? C5 Fe1 C6 131.10(8) . . ? C8 Fe1 C6 67.87(8) . . ? C9 Fe1 C6 67.77(8) . . ? C10 Fe1 C6 40.34(9) . . ? C4 Fe1 C6 167.29(8) . . ? C7 Fe1 C6 40.44(8) . . ? C1 Fe1 C2 40.95(6) . . ? C5 Fe1 C2 69.09(7) . . ? C8 Fe1 C2 128.35(7) . . ? C9 Fe1 C2 164.89(8) . . ? C10 Fe1 C2 153.85(7) . . ? C4 Fe1 C2 68.27(6) . . ? C7 Fe1 C2 109.70(7) . . ? C6 Fe1 C2 120.75(7) . . ? C1 Fe1 C3 68.43(6) . . ? C5 Fe1 C3 68.38(7) . . ? C8 Fe1 C3 106.35(8) . . ? C9 Fe1 C3 126.24(8) . . ? C10 Fe1 C3 164.77(8) . . ? C4 Fe1 C3 40.30(8) . . ? C7 Fe1 C3 117.49(8) . . ? C6 Fe1 C3 152.32(9) . . ? C2 Fe1 C3 40.46(6) . . ? C1 P1 Cl1 99.36(5) . . ? C1 P1 Cl2 95.55(5) . . ? Cl1 P1 Cl2 94.50(3) . . ? C13 N1 C12 109.52(16) . . ? C13 N1 C11 111.71(15) . . ? C12 N1 C11 112.40(15) . . ? C2 C1 C5 107.83(13) . . ? C2 C1 P1 120.79(11) . . ? C5 C1 P1 130.99(13) . . ? C2 C1 Fe1 70.28(8) . . ? C5 C1 Fe1 69.32(8) . . ? P1 C1 Fe1 120.25(7) . . ? C3 C2 C1 107.57(13) . . ? C3 C2 C11 129.49(15) . . ? C1 C2 C11 122.55(12) . . ? C3 C2 Fe1 69.90(8) . . ? C1 C2 Fe1 68.78(8) . . ? C11 C2 Fe1 132.01(11) . . ? C4 C3 C2 108.49(14) . . ? C4 C3 Fe1 69.42(9) . . ? C2 C3 Fe1 69.64(8) . . ? C3 C4 C5 108.72(14) . . ? C3 C4 Fe1 70.28(9) . . ? C5 C4 Fe1 69.28(9) . . ? C4 C5 C1 107.40(17) . . ? C4 C5 Fe1 70.12(10) . . ? C1 C5 Fe1 69.24(9) . . ? C10 C6 C7 108.11(18) . . ? C10 C6 Fe1 69.61(11) . . ? C7 C6 Fe1 69.68(10) . . ? C8 C7 C6 107.58(19) . . ? C8 C7 Fe1 69.41(11) . . ? C6 C7 Fe1 69.88(11) . . ? C9 C8 C7 108.35(19) . . ? C9 C8 Fe1 70.02(10) . . ? C7 C8 Fe1 70.15(10) . . ? C8 C9 C10 108.35(19) . . ? C8 C9 Fe1 69.83(9) . . ? C10 C9 Fe1 69.91(9) . . ? C6 C10 C9 107.6(2) . . ? C6 C10 Fe1 70.05(10) . . ? C9 C10 Fe1 69.58(11) . . ? N1 C11 C2 109.24(13) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 30.38 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.503 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.052 data_sqeeze _database_code_depnum_ccdc_archive 'CCDC 617195' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C114 H174 Fe6 Li12 N6 O3 P6' _chemical_formula_weight 2280.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 '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' O O 0.0106 0.0060 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 16.0644(16) _cell_length_b 26.933(3) _cell_length_c 28.661(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12401(2) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 24.00 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4824 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7650 _exptl_absorpt_correction_T_max 0.8400 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe IPDS area detector' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88150 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 24.09 _reflns_number_total 19542 _reflns_number_gt 12691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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. Two hexane solvent molecules removed with SQUEEZE ; _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^)+(0.0504P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.023(11) _refine_ls_number_reflns 19542 _refine_ls_number_parameters 1182 _refine_ls_number_restraints 77 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 0.804 _refine_ls_restrained_S_all 0.816 _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 0.51930(4) 0.30157(2) 0.36928(2) 0.04224(18) Uani 1 1 d . . . Fe2 Fe -0.07248(4) 0.22317(2) 0.29602(3) 0.04021(18) Uani 1 1 d . . . Fe3 Fe 0.17697(5) 0.13545(3) 0.10464(3) 0.0522(2) Uani 1 1 d . . . Fe4 Fe 0.39430(5) 0.11341(3) 0.51709(3) 0.0575(2) Uani 1 1 d . . . Fe5 Fe 0.64248(4) 0.05164(3) 0.30549(3) 0.0591(2) Uani 1 1 d . . . Fe6 Fe 0.02510(4) -0.02965(2) 0.27994(3) 0.04377(18) Uani 1 1 d . . . P1 P 0.34259(7) 0.23281(4) 0.32308(4) 0.0331(3) Uani 1 1 d . . . P2 P 0.14391(7) 0.20121(4) 0.31955(4) 0.0326(3) Uani 1 1 d . . . P3 P 0.28822(7) 0.13524(4) 0.21350(4) 0.0371(3) Uani 1 1 d . A . P4 P 0.28889(7) 0.10806(4) 0.40666(4) 0.0369(3) Uani 1 1 d . A . P5 P 0.43283(7) 0.09099(4) 0.28519(5) 0.0409(3) Uani 1 1 d . A . P6 P 0.18957(7) 0.04830(4) 0.32315(4) 0.0365(3) Uani 1 1 d . A . N1 N 0.5094(2) 0.22739(15) 0.23020(14) 0.0474(10) Uani 1 1 d . . . N2 N 0.0230(2) 0.12169(13) 0.40543(13) 0.0385(9) Uani 1 1 d . . . N3 N 0.2158(2) 0.26773(14) 0.19434(14) 0.0459(10) Uani 1 1 d . . . N4 N 0.2418(2) 0.23464(15) 0.45499(15) 0.0465(11) Uani 1 1 d . . . N5 N 0.4199(3) -0.01890(16) 0.36902(18) 0.0637(13) Uani 1 1 d . . . N6 N 0.2780(2) -0.01670(14) 0.21882(15) 0.0470(11) Uani 1 1 d . . . C1 C 0.4522(3) 0.24203(16) 0.33859(16) 0.0361(11) Uani 1 1 d . . . C2 C 0.5214(3) 0.25842(16) 0.31007(16) 0.0377(11) Uani 1 1 d . . . C3 C 0.5968(3) 0.2539(2) 0.3357(2) 0.0541(15) Uani 1 1 d . . . H3 H 0.6504 0.2616 0.3247 0.065 Uiso 1 1 calc R . . C4 C 0.5766(3) 0.23576(19) 0.3802(2) 0.0580(15) Uani 1 1 d . . . H4 H 0.6148 0.2291 0.4042 0.070 Uiso 1 1 calc R . . C5 C 0.4894(3) 0.22915(16) 0.38293(16) 0.0398(12) Uani 1 1 d . . . H5 H 0.4602 0.2181 0.4094 0.048 Uiso 1 1 calc R . . C6 C 0.4351(4) 0.35629(19) 0.3816(2) 0.0571(15) Uani 1 1 d . . . H6 H 0.3776 0.3541 0.3760 0.069 Uiso 1 1 calc R . . C7 C 0.4946(4) 0.37238(19) 0.3497(2) 0.0598(15) Uani 1 1 d . . . H7 H 0.4840 0.3828 0.3190 0.072 Uiso 1 1 calc R . . C8 C 0.5754(4) 0.37032(18) 0.3718(2) 0.0596(15) Uani 1 1 d . . . H8 H 0.6267 0.3795 0.3585 0.072 Uiso 1 1 calc R . . C9 C 0.5620(3) 0.35179(19) 0.4173(2) 0.0583(15) Uani 1 1 d . . . H9 H 0.6035 0.3457 0.4397 0.070 Uiso 1 1 calc R . . C10 C 0.4757(3) 0.34382(18) 0.42370(19) 0.0505(14) Uani 1 1 d . . . H10 H 0.4499 0.3323 0.4511 0.061 Uiso 1 1 calc R . . C11 C 0.5130(3) 0.27312(18) 0.25947(17) 0.0476(13) Uani 1 1 d . . . H11 H 0.4584 0.2899 0.2562 0.057 Uiso 1 1 calc R . . C12 C 0.5805(4) 0.3112(2) 0.2444(2) 0.0678(17) Uani 1 1 d . . . H12A H 0.6353 0.2976 0.2504 0.102 Uiso 1 1 calc R . . H12B H 0.5736 0.3417 0.2620 0.102 Uiso 1 1 calc R . . H12C H 0.5748 0.3183 0.2114 0.102 Uiso 1 1 calc R . . C13 C 0.4888(4) 0.2390(2) 0.18211(19) 0.0749(18) Uani 1 1 d . . . H13A H 0.5384 0.2501 0.1659 0.112 Uiso 1 1 calc R . . H13B H 0.4472 0.2650 0.1814 0.112 Uiso 1 1 calc R . . H13C H 0.4671 0.2095 0.1669 0.112 Uiso 1 1 calc R . . C14 C 0.5862(3) 0.1985(2) 0.23125(19) 0.0631(16) Uani 1 1 d . . . H14A H 0.5785 0.1680 0.2138 0.095 Uiso 1 1 calc R . . H14B H 0.6003 0.1906 0.2633 0.095 Uiso 1 1 calc R . . H14C H 0.6309 0.2177 0.2174 0.095 Uiso 1 1 calc R . . C15 C 0.0372(3) 0.18158(15) 0.30579(16) 0.0321(11) Uani 1 1 d . . . C16 C -0.0298(3) 0.16645(15) 0.33681(16) 0.0342(11) Uani 1 1 d . . . C17 C -0.0990(3) 0.15144(16) 0.31022(19) 0.0428(13) Uani 1 1 d . . . H17 H -0.1498 0.1398 0.3223 0.051 Uiso 1 1 calc R . . C18 C -0.0796(3) 0.15669(16) 0.26236(19) 0.0434(13) Uani 1 1 d . . . H18 H -0.1143 0.1489 0.2370 0.052 Uiso 1 1 calc R . . C19 C 0.0026(3) 0.17596(16) 0.26005(17) 0.0369(11) Uani 1 1 d . . . H19 H 0.0306 0.1840 0.2322 0.044 Uiso 1 1 calc R . . C20 C -0.0351(3) 0.29496(17) 0.2963(2) 0.0556(14) Uani 1 1 d . . . H20 H 0.0204 0.3061 0.2953 0.067 Uiso 1 1 calc R . . C21 C -0.0816(3) 0.28504(18) 0.3370(2) 0.0583(15) Uani 1 1 d . . . H21 H -0.0627 0.2880 0.3679 0.070 Uiso 1 1 calc R . . C22 C -0.1617(3) 0.26992(19) 0.3228(2) 0.0606(15) Uani 1 1 d . . . H22 H -0.2058 0.2614 0.3427 0.073 Uiso 1 1 calc R . . C23 C -0.1643(3) 0.2698(2) 0.2735(3) 0.0646(17) Uani 1 1 d . . . H23 H -0.2104 0.2610 0.2550 0.078 Uiso 1 1 calc R . . C24 C -0.0865(4) 0.28515(18) 0.2569(2) 0.0593(16) Uani 1 1 d . . . H24 H -0.0710 0.2884 0.2254 0.071 Uiso 1 1 calc R . . C25 C -0.0249(3) 0.16653(17) 0.38974(16) 0.0411(12) Uani 1 1 d . . . H25 H 0.0091 0.1958 0.3985 0.049 Uiso 1 1 calc R . . C26 C -0.1084(3) 0.1726(2) 0.41442(19) 0.0629(16) Uani 1 1 d . . . H26A H -0.1336 0.2038 0.4051 0.094 Uiso 1 1 calc R . . H26B H -0.0998 0.1725 0.4479 0.094 Uiso 1 1 calc R . . H26C H -0.1449 0.1454 0.4059 0.094 Uiso 1 1 calc R . . C27 C 0.0410(3) 0.1236(2) 0.45613(17) 0.0574(15) Uani 1 1 d . . . H27A H -0.0061 0.1104 0.4733 0.086 Uiso 1 1 calc R . . H27B H 0.0507 0.1578 0.4654 0.086 Uiso 1 1 calc R . . H27C H 0.0901 0.1039 0.4628 0.086 Uiso 1 1 calc R . . C28 C -0.0194(3) 0.07505(17) 0.3947(2) 0.0551(14) Uani 1 1 d . . . H28A H 0.0170 0.0474 0.4020 0.083 Uiso 1 1 calc R . . H28B H -0.0335 0.0742 0.3618 0.083 Uiso 1 1 calc R . . H28C H -0.0699 0.0726 0.4131 0.083 Uiso 1 1 calc R . . C29 C 0.1979(3) 0.14765(17) 0.17643(16) 0.0402(12) Uani 1 1 d . . . C30 C 0.1755(3) 0.19305(19) 0.15145(16) 0.0453(13) Uani 1 1 d . . . C31 C 0.0957(3) 0.1864(2) 0.12980(18) 0.0581(15) Uani 1 1 d . . . H31 H 0.0668 0.2102 0.1121 0.070 Uiso 1 1 calc R . . C32 C 0.0684(3) 0.1379(2) 0.1399(2) 0.0624(16) Uani 1 1 d . . . H32 H 0.0183 0.1236 0.1296 0.075 Uiso 1 1 calc R . . C33 C 0.1291(3) 0.11414(19) 0.16820(18) 0.0483(13) Uani 1 1 d . . . H33 H 0.1252 0.0816 0.1798 0.058 Uiso 1 1 calc R . . C34 C 0.2799(4) 0.0984(2) 0.0821(2) 0.0700(17) Uani 1 1 d . . . H34 H 0.3235 0.0872 0.1013 0.084 Uiso 1 1 calc R . . C35 C 0.2747(5) 0.1453(3) 0.0602(2) 0.082(2) Uani 1 1 d . . . H35 H 0.3146 0.1707 0.0622 0.098 Uiso 1 1 calc R . . C36 C 0.1996(5) 0.1476(3) 0.0348(2) 0.083(2) Uani 1 1 d . . . H36 H 0.1800 0.1746 0.0171 0.099 Uiso 1 1 calc R . . C37 C 0.1596(5) 0.1012(3) 0.0412(2) 0.091(2) Uani 1 1 d . . . H37 H 0.1083 0.0920 0.0281 0.110 Uiso 1 1 calc R . . C38 C 0.2082(5) 0.0714(2) 0.0701(2) 0.0763(19) Uani 1 1 d . . . H38 H 0.1953 0.0390 0.0799 0.092 Uiso 1 1 calc R . . C39 C 0.2294(3) 0.23958(18) 0.15047(17) 0.0477(13) Uani 1 1 d . . . H39 H 0.2883 0.2287 0.1501 0.057 Uiso 1 1 calc R . . C40 C 0.2146(4) 0.2707(2) 0.10606(19) 0.0731(18) Uani 1 1 d . . . H40A H 0.1577 0.2828 0.1059 0.110 Uiso 1 1 calc R . . H40B H 0.2239 0.2502 0.0787 0.110 Uiso 1 1 calc R . . H40C H 0.2528 0.2986 0.1056 0.110 Uiso 1 1 calc R . . C41 C 0.1304(3) 0.2858(2) 0.2010(2) 0.0639(16) Uani 1 1 d . . . H41A H 0.1264 0.3029 0.2306 0.096 Uiso 1 1 calc R . . H41B H 0.0922 0.2579 0.2007 0.096 Uiso 1 1 calc R . . H41C H 0.1162 0.3085 0.1759 0.096 Uiso 1 1 calc R . . C42 C 0.2739(4) 0.3104(2) 0.1973(2) 0.0679(16) Uani 1 1 d . . . H42A H 0.2552 0.3366 0.1765 0.102 Uiso 1 1 calc R . . H42B H 0.3292 0.2998 0.1882 0.102 Uiso 1 1 calc R . . H42C H 0.2751 0.3228 0.2290 0.102 Uiso 1 1 calc R . . C43 C 0.3614(3) 0.13543(17) 0.44906(16) 0.0379(11) Uani 1 1 d . . . C44 C 0.3454(3) 0.17368(18) 0.48356(16) 0.0420(12) Uani 1 1 d . . . C45 C 0.4226(3) 0.1861(2) 0.50653(17) 0.0534(14) Uani 1 1 d . . . H45 H 0.4296 0.2101 0.5301 0.064 Uiso 1 1 calc R . . C46 C 0.4854(3) 0.1559(2) 0.4873(2) 0.0606(16) Uani 1 1 d . . . H46 H 0.5420 0.1564 0.4954 0.073 Uiso 1 1 calc R . . C47 C 0.4486(3) 0.12487(18) 0.45394(18) 0.0479(13) Uani 1 1 d . . . H47 H 0.4772 0.1003 0.4370 0.057 Uiso 1 1 calc R . . C48 C 0.3342(4) 0.0478(2) 0.5275(2) 0.0642(16) Uani 1 1 d . . . H48 H 0.3036 0.0307 0.5046 0.077 Uiso 1 1 calc R . . C49 C 0.3020(5) 0.0833(2) 0.5572(2) 0.0773(19) Uani 1 1 d . . . H49 H 0.2462 0.0937 0.5581 0.093 Uiso 1 1 calc R . . C50 C 0.3678(9) 0.1014(3) 0.5863(3) 0.121(4) Uani 1 1 d . . . H50 H 0.3641 0.1257 0.6098 0.146 Uiso 1 1 calc R . . C51 C 0.4376(8) 0.0756(4) 0.5726(4) 0.142(5) Uani 1 1 d . . . H51 H 0.4909 0.0801 0.5854 0.171 Uiso 1 1 calc R . . C52 C 0.4188(5) 0.0412(3) 0.5364(3) 0.092(2) Uani 1 1 d . . . H52 H 0.4553 0.0188 0.5217 0.111 Uiso 1 1 calc R . . C53 C 0.2618(3) 0.19698(19) 0.49227(16) 0.0452(13) Uani 1 1 d . . . H53 H 0.2201 0.1701 0.4892 0.054 Uiso 1 1 calc R . . C54 C 0.2539(4) 0.2171(2) 0.54232(19) 0.079(2) Uani 1 1 d . . . H54A H 0.2721 0.1919 0.5643 0.118 Uiso 1 1 calc R . . H54B H 0.1963 0.2257 0.5485 0.118 Uiso 1 1 calc R . . H54C H 0.2884 0.2465 0.5457 0.118 Uiso 1 1 calc R . . C55 C 0.1567(3) 0.2549(2) 0.4597(2) 0.0728(18) Uani 1 1 d . . . H55A H 0.1547 0.2775 0.4859 0.109 Uiso 1 1 calc R . . H55B H 0.1178 0.2279 0.4647 0.109 Uiso 1 1 calc R . . H55C H 0.1418 0.2725 0.4314 0.109 Uiso 1 1 calc R . . C56 C 0.3012(3) 0.27665(19) 0.45488(19) 0.0587(15) Uani 1 1 d . . . H56A H 0.2886 0.2986 0.4290 0.088 Uiso 1 1 calc R . . H56B H 0.3575 0.2640 0.4515 0.088 Uiso 1 1 calc R . . H56C H 0.2966 0.2948 0.4840 0.088 Uiso 1 1 calc R . . C57 C 0.5217(3) 0.07497(18) 0.32311(18) 0.0479(13) Uani 1 1 d . . . C58 C 0.5438(3) 0.02828(19) 0.34449(18) 0.0510(14) Uani 1 1 d . . . C59 C 0.6147(4) 0.0343(2) 0.3727(2) 0.0669(17) Uani 1 1 d . . . H59 H 0.6406 0.0093 0.3905 0.080 Uiso 1 1 calc R . . C60 C 0.6404(4) 0.0843(2) 0.3696(2) 0.0671(17) Uani 1 1 d . . . H60 H 0.6859 0.0986 0.3853 0.080 Uiso 1 1 calc R . . C61 C 0.5850(3) 0.1096(2) 0.33841(19) 0.0540(14) Uani 1 1 d . . . H61 H 0.5891 0.1431 0.3294 0.065 Uiso 1 1 calc R . . C62 C 0.6483(4) 0.0565(3) 0.2351(2) 0.0767(19) Uani 1 1 d . . . H62 H 0.6083 0.0714 0.2157 0.092 Uiso 1 1 calc R . . C63 C 0.6477(4) 0.0072(3) 0.2492(3) 0.085(2) Uani 1 1 d . . . H63 H 0.6075 -0.0167 0.2411 0.102 Uiso 1 1 calc R . . C64 C 0.7192(4) -0.0009(3) 0.2783(3) 0.085(2) Uani 1 1 d . . . H64 H 0.7341 -0.0308 0.2930 0.102 Uiso 1 1 calc R . . C65 C 0.7631(4) 0.0444(3) 0.2806(3) 0.086(2) Uani 1 1 d . . . H65 H 0.8134 0.0500 0.2965 0.103 Uiso 1 1 calc R . . C66 C 0.7168(4) 0.0807(3) 0.2541(2) 0.0780(19) Uani 1 1 d . . . H66 H 0.7305 0.1144 0.2504 0.094 Uiso 1 1 calc R . . C67 C 0.4953(3) -0.01919(18) 0.3386(2) 0.0541(15) Uani 1 1 d . . . H67 H 0.4754 -0.0199 0.3059 0.065 Uiso 1 1 calc R . . C68 C 0.5507(4) -0.0663(2) 0.3457(3) 0.085(2) Uani 1 1 d . . . H68A H 0.5728 -0.0665 0.3772 0.128 Uiso 1 1 calc R . . H68B H 0.5963 -0.0658 0.3235 0.128 Uiso 1 1 calc R . . H68C H 0.5174 -0.0959 0.3408 0.128 Uiso 1 1 calc R . . C69 C 0.4391(4) -0.0152(2) 0.4186(2) 0.082(2) Uani 1 1 d . . . H69A H 0.4660 -0.0455 0.4289 0.123 Uiso 1 1 calc R . . H69B H 0.3880 -0.0104 0.4361 0.123 Uiso 1 1 calc R . . H69C H 0.4760 0.0127 0.4239 0.123 Uiso 1 1 calc R . . C70 C 0.3661(4) -0.0625(2) 0.3618(3) 0.086(2) Uani 1 1 d . . . H70A H 0.3895 -0.0908 0.3781 0.129 Uiso 1 1 calc R . . H70B H 0.3625 -0.0698 0.3288 0.129 Uiso 1 1 calc R . . H70C H 0.3109 -0.0555 0.3739 0.129 Uiso 1 1 calc R . . C71 C 0.1192(3) 0.02477(16) 0.27792(16) 0.0374(11) Uani 1 1 d . . . C72 C 0.1335(3) -0.01499(15) 0.24397(16) 0.0368(12) Uani 1 1 d . . . C73 C 0.0620(3) -0.01706(17) 0.21403(19) 0.0523(14) Uani 1 1 d . . . H73 H 0.0551 -0.0394 0.1892 0.063 Uiso 1 1 calc R . . C74 C 0.0050(3) 0.01851(18) 0.22705(18) 0.0507(14) Uani 1 1 d . . . H74 H -0.0464 0.0248 0.2125 0.061 Uiso 1 1 calc R . . C75 C 0.0377(3) 0.04429(16) 0.26663(16) 0.0389(12) Uani 1 1 d . . . H75 H 0.0105 0.0700 0.2828 0.047 Uiso 1 1 calc R . . C76 C 0.0195(4) -0.0520(2) 0.3471(2) 0.0647(16) Uani 1 1 d . . . H76 H 0.0490 -0.0376 0.3720 0.078 Uiso 1 1 calc R . . C77 C 0.0480(4) -0.0911(2) 0.3191(2) 0.0669(17) Uani 1 1 d . . . H77 H 0.0995 -0.1075 0.3216 0.080 Uiso 1 1 calc R . . C78 C -0.0157(4) -0.10147(18) 0.2861(2) 0.0717(18) Uani 1 1 d . . . H78 H -0.0143 -0.1263 0.2630 0.086 Uiso 1 1 calc R . . C79 C -0.0819(3) -0.06774(19) 0.2942(2) 0.0630(16) Uani 1 1 d . . . H79 H -0.1317 -0.0660 0.2770 0.076 Uiso 1 1 calc R . . C80 C -0.0608(4) -0.0375(2) 0.3318(2) 0.0623(16) Uani 1 1 d . . . H80 H -0.0938 -0.0122 0.3447 0.075 Uiso 1 1 calc R . . C81 C 0.2106(3) -0.04591(16) 0.24216(18) 0.0434(12) Uani 1 1 d . . . H81 H 0.2284 -0.0513 0.2748 0.052 Uiso 1 1 calc R . . C82 C 0.1967(3) -0.09720(17) 0.2208(2) 0.0641(16) Uani 1 1 d . . . H82A H 0.1801 -0.0936 0.1884 0.096 Uiso 1 1 calc R . . H82B H 0.1533 -0.1144 0.2379 0.096 Uiso 1 1 calc R . . H82C H 0.2479 -0.1162 0.2224 0.096 Uiso 1 1 calc R . . C83 C 0.3599(3) -0.0411(2) 0.2235(2) 0.0667(17) Uani 1 1 d . . . H83A H 0.3687 -0.0506 0.2558 0.100 Uiso 1 1 calc R . . H83B H 0.4033 -0.0183 0.2139 0.100 Uiso 1 1 calc R . . H83C H 0.3614 -0.0705 0.2039 0.100 Uiso 1 1 calc R . . C84 C 0.2610(4) -0.0074(2) 0.1690(2) 0.0644(16) Uani 1 1 d . . . H84A H 0.2670 -0.0382 0.1516 0.097 Uiso 1 1 calc R . . H84B H 0.3001 0.0169 0.1571 0.097 Uiso 1 1 calc R . . H84C H 0.2047 0.0050 0.1654 0.097 Uiso 1 1 calc R . . O1 O 0.1930(2) 0.35204(12) 0.33148(16) 0.0728(12) Uani 1 1 d . . . C85 C 0.1311(4) 0.3761(2) 0.3594(3) 0.102(3) Uani 1 1 d . . . H85A H 0.1375 0.3669 0.3923 0.122 Uiso 1 1 calc R . . H85B H 0.0752 0.3666 0.3491 0.122 Uiso 1 1 calc R . . C86 C 0.1441(5) 0.4304(3) 0.3533(3) 0.105(3) Uani 1 1 d . . . H86A H 0.1042 0.4439 0.3308 0.125 Uiso 1 1 calc R . . H86B H 0.1375 0.4478 0.3830 0.125 Uiso 1 1 calc R . . C87 C 0.2288(6) 0.4354(2) 0.3360(3) 0.107(3) Uani 1 1 d . . . H87A H 0.2685 0.4383 0.3618 0.129 Uiso 1 1 calc R . . H87B H 0.2342 0.4646 0.3157 0.129 Uiso 1 1 calc R . . C88 C 0.2423(4) 0.3889(2) 0.3094(2) 0.0724(18) Uani 1 1 d . . . H88A H 0.2252 0.3931 0.2769 0.087 Uiso 1 1 calc R . . H88B H 0.3012 0.3795 0.3101 0.087 Uiso 1 1 calc R . . Li1 Li 0.2146(5) 0.2828(3) 0.3281(3) 0.0420(19) Uani 1 1 d . . . Li2 Li 0.2454(5) 0.2171(3) 0.2499(3) 0.042(2) Uani 1 1 d D . . Li3 Li 0.2513(5) 0.1984(3) 0.3892(3) 0.046(2) Uani 1 1 d D . . Li4 Li 0.4108(5) 0.1825(3) 0.2579(3) 0.045(2) Uani 1 1 d . A . Li5 Li 0.4088(5) 0.1502(3) 0.3564(3) 0.048(2) Uani 1 1 d . . . Li6 Li 0.1402(5) 0.1234(3) 0.3700(3) 0.0382(18) Uani 1 1 d . A . Li7 Li 0.1509(5) 0.1213(3) 0.2659(3) 0.050(2) Uani 1 1 d . . . Li8 Li 0.2797(5) 0.1375(3) 0.3118(3) 0.044(2) Uani 1 1 d . . . Li9 Li 0.3475(5) 0.0458(3) 0.3480(3) 0.051(2) Uani 1 1 d . A . Li10 Li 0.2905(5) 0.0510(3) 0.2554(3) 0.043(2) Uani 1 1 d . A . Li11 Li 0.2039(5) 0.0332(3) 0.4074(3) 0.052(2) Uani 1 1 d . . . Li12 Li 0.4188(5) 0.0912(3) 0.2002(3) 0.055(2) Uani 1 1 d . . . O2 O 0.1553(6) -0.0069(3) 0.4599(3) 0.069(3) Uiso 0.474(8) 1 d PD A -1 C89 C 0.1569(10) -0.0595(4) 0.4610(5) 0.0936(17) Uiso 0.474(8) 1 d PD A -1 H89A H 0.2080 -0.0725 0.4751 0.112 Uiso 0.474(8) 1 calc PR A -1 H89B H 0.1487 -0.0742 0.4300 0.112 Uiso 0.474(8) 1 calc PR A -1 C90 C 0.0790(17) -0.0666(7) 0.4934(12) 0.273(6) Uiso 0.474(8) 1 d PD A -1 H90A H 0.0918 -0.0911 0.5177 0.328 Uiso 0.474(8) 1 calc PR A -1 H90B H 0.0322 -0.0792 0.4750 0.328 Uiso 0.474(8) 1 calc PR A -1 C91 C 0.0541(13) -0.0157(9) 0.5169(9) 0.273(6) Uiso 0.474(8) 1 d PD A -1 H91A H 0.0069 0.0004 0.5014 0.328 Uiso 0.474(8) 1 calc PR A -1 H91B H 0.0431 -0.0190 0.5504 0.328 Uiso 0.474(8) 1 calc PR A -1 C92 C 0.1365(9) 0.0097(5) 0.5067(4) 0.0936(17) Uiso 0.474(8) 1 d PD A -1 H92A H 0.1309 0.0459 0.5080 0.112 Uiso 0.474(8) 1 calc PR A -1 H92B H 0.1796 -0.0009 0.5288 0.112 Uiso 0.474(8) 1 calc PR A -1 O3 O 0.4810(5) 0.0768(3) 0.1411(3) 0.058(3) Uiso 0.519(8) 1 d PD B -1 C93 C 0.5231(9) 0.0313(4) 0.1274(5) 0.0936(17) Uiso 0.519(8) 1 d PD B -1 H93A H 0.5130 0.0045 0.1498 0.112 Uiso 0.519(8) 1 calc PR B -1 H93B H 0.5832 0.0364 0.1240 0.112 Uiso 0.519(8) 1 calc PR B -1 C94 C 0.4801(19) 0.0203(7) 0.0785(6) 0.273(6) Uiso 0.519(8) 1 d PD B -1 H94A H 0.5117 -0.0029 0.0590 0.328 Uiso 0.519(8) 1 calc PR B -1 H94B H 0.4220 0.0096 0.0813 0.328 Uiso 0.519(8) 1 calc PR B -1 C95 C 0.490(2) 0.0766(8) 0.0631(4) 0.273(6) Uiso 0.519(8) 1 d PD B -1 H95A H 0.4425 0.0860 0.0435 0.328 Uiso 0.519(8) 1 calc PR B -1 H95B H 0.5406 0.0801 0.0443 0.328 Uiso 0.519(8) 1 calc PR B -1 C96 C 0.4951(9) 0.1129(4) 0.1067(4) 0.0936(17) Uiso 0.519(8) 1 d PD B -1 H96A H 0.5499 0.1286 0.1098 0.112 Uiso 0.519(8) 1 calc PR B -1 H96B H 0.4515 0.1384 0.1062 0.112 Uiso 0.519(8) 1 calc PR B -1 O2F O 0.1656(5) -0.0204(3) 0.4467(3) 0.053(3) Uiso 0.526(8) 1 d PD A -2 C89F C 0.1890(8) -0.0697(4) 0.4386(5) 0.0936(17) Uiso 0.526(8) 1 d PD A -2 H89C H 0.2368 -0.0788 0.4581 0.112 Uiso 0.526(8) 1 calc PR A -2 H89D H 0.2037 -0.0747 0.4058 0.112 Uiso 0.526(8) 1 calc PR A -2 C90F C 0.1132(13) -0.1005(5) 0.4516(11) 0.273(6) Uiso 0.526(8) 1 d PD A -2 H90C H 0.1284 -0.1275 0.4728 0.328 Uiso 0.526(8) 1 calc PR A -2 H90D H 0.0870 -0.1146 0.4237 0.328 Uiso 0.526(8) 1 calc PR A -2 C91F C 0.0544(13) -0.0631(8) 0.4758(10) 0.273(6) Uiso 0.526(8) 1 d PD A -2 H91C H 0.0078 -0.0542 0.4555 0.328 Uiso 0.526(8) 1 calc PR A -2 H91D H 0.0325 -0.0768 0.5050 0.328 Uiso 0.526(8) 1 calc PR A -2 C92F C 0.1101(7) -0.0181(5) 0.4853(4) 0.0936(17) Uiso 0.526(8) 1 d PD A -2 H92C H 0.0781 0.0129 0.4853 0.112 Uiso 0.526(8) 1 calc PR A -2 H92D H 0.1398 -0.0214 0.5150 0.112 Uiso 0.526(8) 1 calc PR A -2 O3F O 0.4821(5) 0.0617(4) 0.1499(3) 0.064(3) Uiso 0.481(8) 1 d PD B -2 C93F C 0.4996(10) 0.0113(4) 0.1414(5) 0.0936(17) Uiso 0.481(8) 1 d PD B -2 H93C H 0.4506 -0.0093 0.1476 0.112 Uiso 0.481(8) 1 calc PR B -2 H93D H 0.5456 -0.0001 0.1611 0.112 Uiso 0.481(8) 1 calc PR B -2 C94F C 0.5232(19) 0.0091(8) 0.0902(6) 0.273(6) Uiso 0.481(8) 1 d PD B -2 H94C H 0.4778 0.0181 0.0691 0.328 Uiso 0.481(8) 1 calc PR B -2 H94D H 0.5485 -0.0225 0.0809 0.328 Uiso 0.481(8) 1 calc PR B -2 C95F C 0.5887(14) 0.0522(8) 0.0982(10) 0.273(6) Uiso 0.481(8) 1 d PD B -2 H95C H 0.6340 0.0416 0.1188 0.328 Uiso 0.481(8) 1 calc PR B -2 H95D H 0.6120 0.0639 0.0686 0.328 Uiso 0.481(8) 1 calc PR B -2 C96F C 0.5333(9) 0.0928(4) 0.1217(5) 0.0936(17) Uiso 0.481(8) 1 d PD B -2 H96C H 0.5663 0.1158 0.1406 0.112 Uiso 0.481(8) 1 calc PR B -2 H96D H 0.5006 0.1114 0.0988 0.112 Uiso 0.481(8) 1 calc PR B -2 C100 C 0.7454(13) 0.3113(7) 0.1168(7) 0.356(11) Uiso 1 1 d D . . H10A H 0.7653 0.3417 0.1310 0.535 Uiso 1 1 calc R . . H10B H 0.6877 0.3059 0.1253 0.535 Uiso 1 1 calc R . . H10C H 0.7500 0.3138 0.0831 0.535 Uiso 1 1 calc R . . C101 C 0.7978(14) 0.2678(7) 0.1340(8) 0.390(13) Uiso 1 1 d D . . H10D H 0.8565 0.2738 0.1264 0.469 Uiso 1 1 calc R . . H10E H 0.7928 0.2650 0.1679 0.469 Uiso 1 1 calc R . . C102 C 0.7706(14) 0.2213(7) 0.1122(8) 0.374(13) Uiso 1 1 d D . . H10F H 0.7770 0.2241 0.0783 0.449 Uiso 1 1 calc R . . H10G H 0.7114 0.2162 0.1189 0.449 Uiso 1 1 calc R . . C103 C 0.8183(13) 0.1771(6) 0.1288(8) 0.350(11) Uiso 1 1 d D . . H10H H 0.8707 0.1757 0.1113 0.420 Uiso 1 1 calc R . . H10I H 0.8327 0.1825 0.1617 0.420 Uiso 1 1 calc R . . C104 C 0.7794(12) 0.1307(7) 0.1252(8) 0.353(11) Uiso 1 1 d D . . H10J H 0.7474 0.1319 0.0961 0.424 Uiso 1 1 calc R . . H10K H 0.7384 0.1298 0.1505 0.424 Uiso 1 1 calc R . . C105 C 0.8202(12) 0.0806(6) 0.1256(7) 0.335(10) Uiso 1 1 d D . . H10L H 0.7780 0.0550 0.1229 0.503 Uiso 1 1 calc R . . H10M H 0.8504 0.0763 0.1547 0.503 Uiso 1 1 calc R . . H10N H 0.8586 0.0781 0.0996 0.503 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 0.0390(4) 0.0399(4) 0.0478(4) -0.0029(3) -0.0037(3) -0.0119(3) Fe2 0.0288(3) 0.0347(4) 0.0572(5) -0.0010(3) -0.0023(3) 0.0036(3) Fe3 0.0596(5) 0.0568(5) 0.0403(4) -0.0098(4) -0.0050(4) 0.0001(4) Fe4 0.0663(5) 0.0609(5) 0.0453(5) 0.0160(4) -0.0183(4) -0.0233(4) Fe5 0.0361(4) 0.0625(5) 0.0789(6) -0.0181(5) -0.0130(4) 0.0093(4) Fe6 0.0367(4) 0.0313(4) 0.0633(5) -0.0074(3) -0.0065(4) -0.0038(3) P1 0.0298(6) 0.0338(7) 0.0357(7) -0.0054(6) -0.0002(5) -0.0035(5) P2 0.0265(6) 0.0310(6) 0.0404(7) -0.0004(6) 0.0000(5) -0.0004(5) P3 0.0381(7) 0.0347(6) 0.0383(7) -0.0070(6) -0.0007(6) 0.0014(5) P4 0.0386(7) 0.0352(7) 0.0370(7) -0.0018(6) -0.0060(6) -0.0005(6) P5 0.0321(6) 0.0398(7) 0.0506(8) -0.0087(6) -0.0004(6) 0.0054(5) P6 0.0354(7) 0.0296(6) 0.0443(8) -0.0047(6) -0.0035(6) -0.0017(5) N1 0.043(2) 0.057(3) 0.042(3) -0.007(2) 0.004(2) -0.006(2) N2 0.045(2) 0.034(2) 0.036(2) 0.0011(18) 0.0055(19) -0.0049(19) N3 0.052(2) 0.039(2) 0.046(3) 0.004(2) 0.005(2) 0.006(2) N4 0.039(2) 0.044(3) 0.057(3) -0.013(2) 0.011(2) -0.0035(19) N5 0.064(3) 0.047(3) 0.080(4) 0.007(3) -0.008(3) 0.015(2) N6 0.041(2) 0.040(2) 0.060(3) -0.014(2) -0.001(2) 0.0019(19) C1 0.036(3) 0.032(3) 0.041(3) -0.006(2) -0.002(2) 0.000(2) C2 0.028(2) 0.043(3) 0.042(3) -0.001(2) 0.000(2) -0.011(2) C3 0.034(3) 0.066(4) 0.062(4) -0.010(3) 0.001(3) -0.017(3) C4 0.044(3) 0.052(3) 0.078(5) 0.000(3) -0.023(3) -0.004(3) C5 0.045(3) 0.039(3) 0.035(3) 0.001(2) -0.005(2) -0.005(2) C6 0.053(3) 0.051(3) 0.068(4) -0.002(3) -0.010(3) -0.013(3) C7 0.076(4) 0.046(3) 0.057(4) 0.006(3) -0.007(3) -0.007(3) C8 0.063(4) 0.047(3) 0.069(4) 0.005(3) 0.000(3) -0.021(3) C9 0.060(4) 0.053(3) 0.062(4) -0.006(3) -0.006(3) -0.020(3) C10 0.053(3) 0.048(3) 0.050(4) -0.015(3) 0.008(3) -0.018(3) C11 0.039(3) 0.053(3) 0.051(3) -0.007(3) 0.008(2) -0.007(2) C12 0.071(4) 0.066(4) 0.066(4) 0.002(3) 0.018(3) -0.027(3) C13 0.069(4) 0.103(5) 0.052(4) -0.001(4) 0.002(3) -0.009(4) C14 0.052(3) 0.071(4) 0.066(4) -0.022(3) 0.016(3) 0.002(3) C15 0.030(2) 0.026(2) 0.041(3) 0.001(2) 0.005(2) 0.0062(19) C16 0.030(2) 0.028(2) 0.044(3) -0.001(2) 0.007(2) 0.002(2) C17 0.026(2) 0.040(3) 0.062(4) -0.007(3) 0.004(3) -0.004(2) C18 0.038(3) 0.041(3) 0.051(4) -0.004(2) -0.013(3) -0.005(2) C19 0.039(3) 0.034(3) 0.038(3) 0.005(2) -0.005(2) -0.002(2) C20 0.048(3) 0.040(3) 0.079(4) 0.002(3) -0.002(3) 0.009(2) C21 0.055(4) 0.042(3) 0.078(4) -0.018(3) -0.002(3) 0.009(3) C22 0.041(3) 0.050(3) 0.090(5) 0.004(3) 0.010(3) 0.014(3) C23 0.041(3) 0.048(3) 0.105(6) -0.001(3) -0.019(3) 0.015(3) C24 0.068(4) 0.041(3) 0.069(4) 0.015(3) -0.001(3) 0.019(3) C25 0.040(3) 0.044(3) 0.039(3) -0.004(2) 0.013(2) -0.004(2) C26 0.058(4) 0.071(4) 0.060(4) 0.005(3) 0.023(3) 0.015(3) C27 0.070(4) 0.060(4) 0.042(3) 0.001(3) 0.009(3) -0.006(3) C28 0.056(3) 0.041(3) 0.068(4) 0.004(3) 0.010(3) -0.001(3) C29 0.038(3) 0.041(3) 0.042(3) -0.005(2) 0.013(2) 0.003(2) C30 0.043(3) 0.053(3) 0.041(3) 0.001(3) 0.002(2) 0.008(3) C31 0.052(3) 0.078(4) 0.045(3) 0.000(3) -0.016(3) 0.010(3) C32 0.041(3) 0.073(4) 0.073(4) -0.015(3) -0.015(3) -0.004(3) C33 0.042(3) 0.046(3) 0.057(4) -0.010(3) 0.000(3) -0.006(2) C34 0.086(5) 0.068(4) 0.056(4) -0.017(3) 0.012(3) 0.005(4) C35 0.109(6) 0.078(5) 0.058(4) -0.018(4) 0.030(4) -0.011(4) C36 0.123(6) 0.084(5) 0.041(4) -0.005(3) -0.005(4) 0.014(5) C37 0.105(6) 0.108(6) 0.061(5) -0.036(4) -0.004(4) -0.009(5) C38 0.110(6) 0.064(4) 0.055(4) -0.019(3) 0.004(4) 0.002(4) C39 0.057(3) 0.046(3) 0.040(3) -0.002(3) 0.007(3) 0.001(3) C40 0.110(5) 0.058(4) 0.052(4) 0.008(3) 0.011(4) 0.002(4) C41 0.066(4) 0.059(4) 0.067(4) -0.006(3) 0.006(3) 0.015(3) C42 0.080(4) 0.049(3) 0.074(4) -0.008(3) -0.001(3) -0.007(3) C43 0.032(3) 0.044(3) 0.038(3) 0.005(2) -0.001(2) -0.006(2) C44 0.046(3) 0.052(3) 0.027(3) 0.001(2) 0.001(2) -0.021(2) C45 0.059(4) 0.063(4) 0.038(3) -0.001(3) -0.012(3) -0.024(3) C46 0.043(3) 0.065(4) 0.074(4) 0.021(3) -0.026(3) -0.023(3) C47 0.036(3) 0.045(3) 0.063(4) 0.008(3) -0.009(3) -0.005(2) C48 0.074(4) 0.059(4) 0.059(4) 0.018(3) -0.009(3) -0.023(3) C49 0.109(6) 0.063(4) 0.060(4) 0.013(4) 0.019(4) -0.019(4) C50 0.246(13) 0.075(6) 0.044(5) 0.012(4) 0.016(7) -0.046(7) C51 0.191(12) 0.150(10) 0.086(8) 0.062(7) -0.077(8) -0.072(9) C52 0.110(6) 0.078(5) 0.090(6) 0.039(4) -0.009(5) -0.008(4) C53 0.047(3) 0.049(3) 0.040(3) -0.010(3) 0.013(2) -0.019(2) C54 0.096(5) 0.087(5) 0.053(4) -0.023(4) 0.027(3) -0.019(4) C55 0.051(4) 0.067(4) 0.100(5) -0.020(4) 0.016(3) -0.001(3) C56 0.070(4) 0.046(3) 0.060(4) -0.010(3) 0.006(3) -0.018(3) C57 0.047(3) 0.046(3) 0.050(3) -0.015(3) 0.004(3) 0.007(3) C58 0.051(3) 0.044(3) 0.058(4) -0.008(3) -0.020(3) 0.014(3) C59 0.070(4) 0.055(4) 0.076(4) -0.001(3) -0.035(3) 0.003(3) C60 0.059(4) 0.076(4) 0.066(4) -0.019(3) -0.023(3) 0.006(3) C61 0.047(3) 0.054(3) 0.060(4) -0.018(3) -0.008(3) -0.002(3) C62 0.044(4) 0.107(6) 0.079(5) -0.020(4) 0.001(3) 0.020(4) C63 0.042(4) 0.100(6) 0.113(6) -0.048(5) 0.010(4) 0.000(4) C64 0.046(4) 0.086(5) 0.123(6) -0.025(4) -0.002(4) 0.024(4) C65 0.036(3) 0.101(5) 0.121(6) -0.033(5) -0.007(4) 0.007(4) C66 0.045(4) 0.097(5) 0.092(5) -0.007(4) 0.007(4) 0.001(4) C67 0.043(3) 0.049(3) 0.070(4) -0.014(3) -0.011(3) 0.011(2) C68 0.078(5) 0.053(4) 0.125(6) -0.009(4) -0.013(4) 0.014(3) C69 0.105(5) 0.059(4) 0.081(5) 0.006(4) -0.006(4) 0.027(4) C70 0.078(4) 0.048(4) 0.134(6) 0.012(4) -0.001(4) -0.005(3) C71 0.039(3) 0.031(2) 0.043(3) 0.002(2) -0.002(2) -0.001(2) C72 0.045(3) 0.026(3) 0.040(3) -0.008(2) -0.009(2) -0.002(2) C73 0.047(3) 0.039(3) 0.071(4) -0.020(3) -0.013(3) -0.001(2) C74 0.043(3) 0.048(3) 0.061(4) -0.006(3) -0.012(3) 0.000(2) C75 0.035(3) 0.033(3) 0.049(3) -0.002(2) -0.004(2) 0.002(2) C76 0.070(4) 0.053(4) 0.071(4) 0.013(3) -0.011(3) -0.019(3) C77 0.055(4) 0.047(3) 0.099(5) 0.011(3) 0.000(4) 0.003(3) C78 0.068(4) 0.040(3) 0.107(5) -0.020(3) 0.024(4) -0.017(3) C79 0.038(3) 0.057(3) 0.093(5) -0.020(3) -0.001(3) -0.005(3) C80 0.057(4) 0.050(3) 0.080(4) -0.010(3) 0.015(3) -0.009(3) C81 0.040(3) 0.030(3) 0.060(3) -0.012(2) -0.001(2) -0.004(2) C82 0.066(4) 0.035(3) 0.092(4) -0.023(3) 0.008(3) -0.004(3) C83 0.046(3) 0.058(4) 0.096(5) -0.033(3) 0.008(3) 0.016(3) C84 0.068(4) 0.062(4) 0.063(4) -0.013(3) 0.014(3) -0.005(3) O1 0.069(3) 0.037(2) 0.113(3) -0.010(2) 0.012(2) 0.0038(19) C85 0.087(5) 0.056(4) 0.163(7) -0.046(5) 0.034(5) 0.002(4) C86 0.106(6) 0.080(5) 0.127(7) -0.018(5) 0.025(5) 0.022(4) C87 0.162(8) 0.054(4) 0.107(6) -0.009(4) 0.046(6) -0.038(4) C88 0.098(5) 0.051(4) 0.069(4) 0.001(3) 0.004(4) -0.006(3) Li1 0.039(4) 0.036(4) 0.051(5) -0.009(4) 0.003(4) -0.003(4) Li2 0.049(5) 0.033(4) 0.044(5) 0.002(4) 0.003(4) 0.001(4) Li3 0.040(4) 0.045(5) 0.055(5) -0.008(4) 0.007(4) -0.005(4) Li4 0.035(4) 0.048(5) 0.052(5) -0.014(4) -0.001(4) -0.003(4) Li5 0.046(5) 0.046(5) 0.053(6) -0.005(4) 0.000(4) -0.002(4) Li6 0.047(5) 0.034(4) 0.034(4) -0.008(4) 0.005(4) 0.009(4) Li7 0.050(5) 0.050(5) 0.050(5) 0.002(4) -0.006(4) 0.002(4) Li8 0.043(4) 0.048(5) 0.042(5) -0.013(4) -0.004(4) 0.003(4) Li9 0.046(5) 0.038(5) 0.070(6) -0.008(4) -0.001(4) 0.001(4) Li10 0.047(5) 0.033(4) 0.049(5) -0.008(4) 0.008(4) 0.000(4) Li11 0.054(5) 0.054(5) 0.049(5) 0.010(4) -0.008(4) -0.008(4) Li12 0.052(5) 0.067(6) 0.047(5) -0.025(5) -0.003(4) 0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C4 2.022(5) . ? Fe1 C7 2.027(5) . ? Fe1 C6 2.031(6) . ? Fe1 C3 2.031(5) . ? Fe1 C5 2.046(4) . ? Fe1 C9 2.048(5) . ? Fe1 C10 2.054(5) . ? Fe1 C2 2.057(5) . ? Fe1 C8 2.060(5) . ? Fe1 C1 2.123(4) . ? Fe2 C17 2.020(5) . ? Fe2 C24 2.023(5) . ? Fe2 C20 2.025(5) . ? Fe2 C19 2.034(5) . ? Fe2 C18 2.037(5) . ? Fe2 C16 2.042(4) . ? Fe2 C23 2.042(5) . ? Fe2 C21 2.044(5) . ? Fe2 C22 2.056(5) . ? Fe2 C15 2.106(4) . ? Fe3 C32 2.016(6) . ? Fe3 C31 2.028(5) . ? Fe3 C34 2.036(6) . ? Fe3 C35 2.039(6) . ? Fe3 C38 2.050(6) . ? Fe3 C30 2.051(5) . ? Fe3 C37 2.057(6) . ? Fe3 C33 2.058(5) . ? Fe3 C36 2.061(6) . ? Fe3 C29 2.111(5) . ? Fe4 C51 2.012(8) . ? Fe4 C47 2.032(5) . ? Fe4 C45 2.034(5) . ? Fe4 C48 2.034(5) . ? Fe4 C44 2.043(5) . ? Fe4 C46 2.044(5) . ? Fe4 C49 2.044(6) . ? Fe4 C50 2.055(8) . ? Fe4 C52 2.060(7) . ? Fe4 C43 2.105(5) . ? Fe5 C63 2.011(6) . ? Fe5 C62 2.023(7) . ? Fe5 C59 2.032(6) . ? Fe5 C64 2.033(6) . ? Fe5 C60 2.038(6) . ? Fe5 C58 2.040(5) . ? Fe5 C61 2.044(5) . ? Fe5 C66 2.051(6) . ? Fe5 C65 2.074(6) . ? Fe5 C57 2.100(5) . ? Fe6 C73 2.009(6) . ? Fe6 C76 2.018(6) . ? Fe6 C74 2.021(5) . ? Fe6 C77 2.034(6) . ? Fe6 C75 2.038(4) . ? Fe6 C80 2.039(5) . ? Fe6 C79 2.043(5) . ? Fe6 C78 2.050(5) . ? Fe6 C72 2.062(5) . ? Fe6 C71 2.106(4) . ? P1 C1 1.834(4) . ? P1 Li1 2.462(8) . ? P1 Li4 2.555(8) . ? P1 Li3 2.569(8) . ? P1 Li5 2.644(8) . ? P1 Li2 2.647(8) . ? P1 Li8 2.779(8) . ? P2 C15 1.837(4) . ? P2 Li1 2.485(7) . ? P2 Li6 2.548(8) . ? P2 Li2 2.612(8) . ? P2 Li3 2.640(8) . ? P2 Li7 2.648(8) . ? P2 Li8 2.785(8) . ? P3 C29 1.829(5) . ? P3 Li12 2.440(8) . ? P3 Li2 2.536(8) . ? P3 Li10 2.567(8) . ? P3 Li4 2.668(8) . ? P3 Li7 2.695(9) . ? P3 Li8 2.822(8) . ? P4 C43 1.838(5) . ? P4 Li11 2.435(8) . ? P4 Li9 2.555(8) . ? P4 Li3 2.555(8) . ? P4 Li6 2.641(8) . ? P4 Li5 2.659(8) . ? P4 Li8 2.835(8) . ? P5 C57 1.846(5) . ? P5 Li12 2.448(9) . ? P5 Li9 2.568(9) . ? P5 Li4 2.610(8) . ? P5 Li5 2.620(8) . ? P5 Li10 2.669(8) . ? P5 Li8 2.864(8) . ? P6 C71 1.833(5) . ? P6 Li11 2.459(8) . ? P6 Li10 2.531(8) . ? P6 Li6 2.554(7) . ? P6 Li7 2.636(8) . ? P6 Li9 2.636(8) . ? P6 Li8 2.823(8) . ? N1 C13 1.451(6) . ? N1 C14 1.459(6) . ? N1 C11 1.491(6) . ? N1 Li4 2.146(9) . ? N2 C28 1.462(6) . ? N2 C27 1.482(6) . ? N2 C25 1.501(6) . ? N2 Li6 2.139(8) . ? N3 C41 1.467(6) . ? N3 C42 1.483(6) . ? N3 C39 1.484(6) . ? N3 Li2 2.150(8) . ? N4 C55 1.477(6) . ? N4 C56 1.480(6) . ? N4 C53 1.508(6) . ? N4 Li3 2.129(8) . ? N5 C69 1.459(7) . ? N5 C70 1.471(7) . ? N5 C67 1.493(7) . ? N5 Li9 2.180(9) . ? N6 C84 1.475(7) . ? N6 C83 1.477(6) . ? N6 C81 1.496(6) . ? N6 Li10 2.112(8) . ? C1 C5 1.446(6) . ? C1 C2 1.449(6) . ? C1 Li5 2.620(9) . ? C2 C3 1.420(7) . ? C2 C11 1.510(6) . ? C3 C4 1.405(7) . ? C4 C5 1.414(7) . ? C5 Li5 2.602(9) . ? C6 C7 1.391(7) . ? C6 C10 1.411(7) . ? C7 C8 1.445(7) . ? C8 C9 1.413(7) . ? C9 C10 1.415(7) . ? C11 C12 1.555(7) . ? C15 C19 1.432(6) . ? C15 C16 1.454(6) . ? C15 Li7 2.698(9) . ? C16 C17 1.407(6) . ? C16 C25 1.519(6) . ? C17 C18 1.414(7) . ? C18 C19 1.420(6) . ? C20 C21 1.412(7) . ? C20 C24 1.424(7) . ? C21 C22 1.409(7) . ? C22 C23 1.414(8) . ? C23 C24 1.399(7) . ? C25 C26 1.526(6) . ? C29 C33 1.446(6) . ? C29 C30 1.462(6) . ? C29 Li7 2.765(10) . ? C30 C31 1.436(7) . ? C30 C39 1.523(7) . ? C31 C32 1.408(8) . ? C32 C33 1.422(7) . ? C34 C38 1.403(8) . ? C34 C35 1.415(8) . ? C35 C36 1.410(9) . ? C36 C37 1.417(9) . ? C37 C38 1.393(9) . ? C39 C40 1.542(7) . ? C43 C47 1.435(6) . ? C43 C44 1.451(6) . ? C43 Li5 2.790(10) . ? C44 C45 1.443(6) . ? C44 C53 1.503(7) . ? C45 C46 1.410(7) . ? C46 C47 1.400(7) . ? C48 C49 1.379(8) . ? C48 C52 1.394(9) . ? C49 C50 1.433(12) . ? C50 C51 1.377(13) . ? C51 C52 1.422(12) . ? C53 C54 1.539(7) . ? C57 C58 1.443(7) . ? C57 C61 1.448(7) . ? C58 C59 1.407(7) . ? C58 C67 1.506(7) . ? C59 C60 1.412(8) . ? C60 C61 1.434(7) . ? C62 C63 1.389(9) . ? C62 C66 1.389(8) . ? C63 C64 1.437(9) . ? C64 C65 1.411(8) . ? C65 C66 1.444(9) . ? C67 C68 1.563(7) . ? C71 C75 1.447(6) . ? C71 C72 1.465(6) . ? C71 Li7 2.672(9) . ? C72 C73 1.435(6) . ? C72 C81 1.492(6) . ? C73 C74 1.377(6) . ? C74 C75 1.430(6) . ? C75 Li7 2.758(9) . ? C76 C77 1.402(8) . ? C76 C80 1.418(8) . ? C77 C78 1.421(8) . ? C78 C79 1.418(7) . ? C79 C80 1.392(7) . ? C81 C82 1.528(6) . ? O1 C88 1.418(6) . ? O1 C85 1.433(7) . ? O1 Li1 1.899(8) . ? C85 C86 1.486(9) . ? C86 C87 1.453(9) . ? C87 C88 1.483(8) . ? Li1 Li2 2.896(11) . ? Li1 Li3 2.931(12) . ? Li2 Li4 2.825(11) . ? Li2 Li8 2.838(11) . ? Li2 Li7 3.030(11) . ? Li3 Li6 2.750(11) . ? Li3 Li8 2.796(10) . ? Li3 Li5 2.993(11) . ? Li4 Li8 2.880(11) . ? Li4 Li5 2.954(12) . ? Li4 Li12 2.967(11) . ? Li5 Li8 2.460(11) . ? Li5 Li9 2.989(11) . ? Li6 Li8 2.819(11) . ? Li6 Li11 2.845(11) . ? Li6 Li7 2.991(11) . ? Li7 Li8 2.491(11) . ? Li7 Li10 2.950(11) . ? Li8 Li10 2.841(11) . ? Li9 Li10 2.812(12) . ? Li9 Li11 2.888(12) . ? Li10 Li12 2.815(12) . ? Li11 O2F 1.932(10) . ? Li11 O2 2.010(11) . ? Li12 O3F 1.933(11) . ? Li12 O3 2.005(11) . ? O2 C89 1.417(8) . ? O2 C92 1.447(8) . ? C89 C90 1.569(8) . ? C90 C91 1.579(9) . ? C91 C92 1.518(9) . ? O3 C96 1.403(8) . ? O3 C93 1.453(8) . ? C93 C94 1.589(10) . ? C94 C95 1.588(10) . ? C95 C96 1.591(9) . ? O2F C89F 1.400(7) . ? O2F C92F 1.422(7) . ? C89F C90F 1.518(8) . ? C90F C91F 1.545(9) . ? C91F C92F 1.531(8) . ? O3F C93F 1.407(7) . ? O3F C96F 1.425(8) . ? C93F C94F 1.516(9) . ? C94F C95F 1.583(9) . ? C95F C96F 1.562(9) . ? C100 C101 1.524(16) . ? C101 C102 1.466(16) . ? C102 C103 1.493(15) . ? C103 C104 1.401(15) . ? C104 C105 1.500(15) . ? 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 C4 Fe1 C7 163.1(2) . . ? C4 Fe1 C6 155.9(2) . . ? C7 Fe1 C6 40.1(2) . . ? C4 Fe1 C3 40.5(2) . . ? C7 Fe1 C3 125.7(2) . . ? C6 Fe1 C3 161.6(2) . . ? C4 Fe1 C5 40.68(19) . . ? C7 Fe1 C5 154.6(2) . . ? C6 Fe1 C5 120.2(2) . . ? C3 Fe1 C5 68.4(2) . . ? C4 Fe1 C9 108.8(2) . . ? C7 Fe1 C9 68.3(2) . . ? C6 Fe1 C9 68.1(2) . . ? C3 Fe1 C9 122.1(2) . . ? C5 Fe1 C9 125.4(2) . . ? C4 Fe1 C10 121.6(2) . . ? C7 Fe1 C10 67.8(2) . . ? C6 Fe1 C10 40.4(2) . . ? C3 Fe1 C10 156.9(2) . . ? C5 Fe1 C10 107.63(19) . . ? C9 Fe1 C10 40.4(2) . . ? C4 Fe1 C2 68.0(2) . . ? C7 Fe1 C2 107.9(2) . . ? C6 Fe1 C2 124.4(2) . . ? C3 Fe1 C2 40.64(18) . . ? C5 Fe1 C2 67.86(18) . . ? C9 Fe1 C2 157.2(2) . . ? C10 Fe1 C2 160.93(19) . . ? C4 Fe1 C8 125.7(2) . . ? C7 Fe1 C8 41.4(2) . . ? C6 Fe1 C8 68.5(2) . . ? C3 Fe1 C8 108.5(2) . . ? C5 Fe1 C8 162.3(2) . . ? C9 Fe1 C8 40.2(2) . . ? C10 Fe1 C8 68.0(2) . . ? C2 Fe1 C8 121.9(2) . . ? C4 Fe1 C1 68.47(18) . . ? C7 Fe1 C1 119.8(2) . . ? C6 Fe1 C1 106.41(19) . . ? C3 Fe1 C1 68.69(18) . . ? C5 Fe1 C1 40.55(17) . . ? C9 Fe1 C1 161.3(2) . . ? C10 Fe1 C1 124.06(19) . . ? C2 Fe1 C1 40.52(16) . . ? C8 Fe1 C1 156.2(2) . . ? C17 Fe2 C24 151.3(2) . . ? C17 Fe2 C20 167.2(2) . . ? C24 Fe2 C20 41.2(2) . . ? C17 Fe2 C19 68.23(18) . . ? C24 Fe2 C19 107.5(2) . . ? C20 Fe2 C19 115.0(2) . . ? C17 Fe2 C18 40.79(19) . . ? C24 Fe2 C18 117.2(2) . . ? C20 Fe2 C18 149.1(2) . . ? C19 Fe2 C18 40.84(18) . . ? C17 Fe2 C16 40.53(18) . . ? C24 Fe2 C16 166.3(2) . . ? C20 Fe2 C16 127.8(2) . . ? C19 Fe2 C16 67.86(18) . . ? C18 Fe2 C16 68.43(19) . . ? C17 Fe2 C23 120.0(2) . . ? C24 Fe2 C23 40.3(2) . . ? C20 Fe2 C23 68.2(2) . . ? C19 Fe2 C23 130.8(2) . . ? C18 Fe2 C23 110.5(2) . . ? C16 Fe2 C23 152.1(2) . . ? C17 Fe2 C21 130.4(2) . . ? C24 Fe2 C21 68.8(2) . . ? C20 Fe2 C21 40.6(2) . . ? C19 Fe2 C21 147.5(2) . . ? C18 Fe2 C21 170.0(2) . . ? C16 Fe2 C21 107.8(2) . . ? C23 Fe2 C21 68.2(2) . . ? C17 Fe2 C22 111.3(2) . . ? C24 Fe2 C22 67.9(2) . . ? C20 Fe2 C22 67.7(2) . . ? C19 Fe2 C22 170.3(2) . . ? C18 Fe2 C22 132.6(2) . . ? C16 Fe2 C22 118.6(2) . . ? C23 Fe2 C22 40.4(2) . . ? C21 Fe2 C22 40.2(2) . . ? C17 Fe2 C15 68.94(17) . . ? C24 Fe2 C15 127.3(2) . . ? C20 Fe2 C15 105.02(19) . . ? C19 Fe2 C15 40.41(16) . . ? C18 Fe2 C15 69.03(18) . . ? C16 Fe2 C15 40.98(16) . . ? C23 Fe2 C15 166.7(2) . . ? C21 Fe2 C15 114.66(19) . . ? C22 Fe2 C15 149.2(2) . . ? C32 Fe3 C31 40.8(2) . . ? C32 Fe3 C34 151.3(3) . . ? C31 Fe3 C34 165.4(3) . . ? C32 Fe3 C35 167.0(3) . . ? C31 Fe3 C35 129.0(3) . . ? C34 Fe3 C35 40.6(2) . . ? C32 Fe3 C38 118.7(3) . . ? C31 Fe3 C38 154.0(3) . . ? C34 Fe3 C38 40.2(2) . . ? C35 Fe3 C38 67.7(3) . . ? C32 Fe3 C30 68.8(2) . . ? C31 Fe3 C30 41.23(19) . . ? C34 Fe3 C30 126.0(2) . . ? C35 Fe3 C30 108.6(2) . . ? C38 Fe3 C30 162.6(3) . . ? C32 Fe3 C37 109.9(3) . . ? C31 Fe3 C37 122.0(3) . . ? C34 Fe3 C37 67.1(3) . . ? C35 Fe3 C37 67.1(3) . . ? C38 Fe3 C37 39.7(3) . . ? C30 Fe3 C37 156.3(3) . . ? C32 Fe3 C33 40.8(2) . . ? C31 Fe3 C33 68.5(2) . . ? C34 Fe3 C33 116.5(2) . . ? C35 Fe3 C33 151.2(3) . . ? C38 Fe3 C33 106.5(2) . . ? C30 Fe3 C33 68.2(2) . . ? C37 Fe3 C33 127.3(3) . . ? C32 Fe3 C36 129.3(3) . . ? C31 Fe3 C36 110.6(3) . . ? C34 Fe3 C36 68.1(3) . . ? C35 Fe3 C36 40.2(3) . . ? C38 Fe3 C36 67.8(3) . . ? C30 Fe3 C36 121.1(3) . . ? C37 Fe3 C36 40.3(3) . . ? C33 Fe3 C36 165.9(3) . . ? C32 Fe3 C29 69.19(19) . . ? C31 Fe3 C29 69.55(19) . . ? C34 Fe3 C29 104.8(2) . . ? C35 Fe3 C29 117.8(3) . . ? C38 Fe3 C29 124.2(2) . . ? C30 Fe3 C29 41.10(18) . . ? C37 Fe3 C29 162.3(3) . . ? C33 Fe3 C29 40.56(17) . . ? C36 Fe3 C29 153.4(3) . . ? C51 Fe4 C47 129.2(5) . . ? C51 Fe4 C45 121.9(3) . . ? C47 Fe4 C45 68.0(2) . . ? C51 Fe4 C48 66.9(3) . . ? C47 Fe4 C48 117.8(2) . . ? C45 Fe4 C48 164.5(3) . . ? C51 Fe4 C44 155.1(4) . . ? C47 Fe4 C44 68.00(19) . . ? C45 Fe4 C44 41.45(18) . . ? C48 Fe4 C44 125.2(2) . . ? C51 Fe4 C46 111.5(4) . . ? C47 Fe4 C46 40.2(2) . . ? C45 Fe4 C46 40.4(2) . . ? C48 Fe4 C46 152.5(3) . . ? C44 Fe4 C46 68.5(2) . . ? C51 Fe4 C49 66.8(4) . . ? C47 Fe4 C49 150.7(3) . . ? C45 Fe4 C49 128.9(3) . . ? C48 Fe4 C49 39.5(2) . . ? C44 Fe4 C49 107.5(2) . . ? C46 Fe4 C49 167.5(3) . . ? C51 Fe4 C50 39.6(4) . . ? C47 Fe4 C50 166.6(4) . . ? C45 Fe4 C50 110.0(3) . . ? C48 Fe4 C50 67.9(3) . . ? C44 Fe4 C50 120.0(4) . . ? C46 Fe4 C50 129.8(4) . . ? C49 Fe4 C50 40.9(3) . . ? C51 Fe4 C52 40.9(3) . . ? C47 Fe4 C52 107.5(3) . . ? C45 Fe4 C52 155.1(3) . . ? C48 Fe4 C52 39.8(2) . . ? C44 Fe4 C52 161.7(3) . . ? C46 Fe4 C52 120.3(3) . . ? C49 Fe4 C52 67.2(3) . . ? C50 Fe4 C52 68.4(3) . . ? C51 Fe4 C43 163.9(5) . . ? C47 Fe4 C43 40.53(17) . . ? C45 Fe4 C43 69.31(18) . . ? C48 Fe4 C43 105.2(2) . . ? C44 Fe4 C43 40.91(17) . . ? C46 Fe4 C43 68.57(19) . . ? C49 Fe4 C43 116.8(3) . . ? C50 Fe4 C43 152.4(4) . . ? C52 Fe4 C43 124.2(3) . . ? C63 Fe5 C62 40.3(3) . . ? C63 Fe5 C59 129.3(3) . . ? C62 Fe5 C59 166.0(3) . . ? C63 Fe5 C64 41.6(3) . . ? C62 Fe5 C64 68.6(3) . . ? C59 Fe5 C64 109.6(3) . . ? C63 Fe5 C60 168.9(3) . . ? C62 Fe5 C60 150.7(3) . . ? C59 Fe5 C60 40.6(2) . . ? C64 Fe5 C60 131.0(3) . . ? C63 Fe5 C58 106.8(2) . . ? C62 Fe5 C58 127.0(2) . . ? C59 Fe5 C58 40.44(19) . . ? C64 Fe5 C58 117.8(3) . . ? C60 Fe5 C58 68.1(2) . . ? C63 Fe5 C61 147.5(3) . . ? C62 Fe5 C61 115.5(3) . . ? C59 Fe5 C61 68.8(2) . . ? C64 Fe5 C61 169.3(2) . . ? C60 Fe5 C61 41.1(2) . . ? C58 Fe5 C61 68.4(2) . . ? C63 Fe5 C66 68.1(3) . . ? C62 Fe5 C66 39.9(2) . . ? C59 Fe5 C66 153.7(2) . . ? C64 Fe5 C66 68.7(3) . . ? C60 Fe5 C66 119.5(3) . . ? C58 Fe5 C66 164.5(2) . . ? C61 Fe5 C66 107.6(3) . . ? C63 Fe5 C65 68.2(3) . . ? C62 Fe5 C65 67.7(3) . . ? C59 Fe5 C65 120.6(3) . . ? C64 Fe5 C65 40.2(2) . . ? C60 Fe5 C65 111.5(3) . . ? C58 Fe5 C65 152.4(3) . . ? C61 Fe5 C65 130.7(2) . . ? C66 Fe5 C65 41.0(2) . . ? C63 Fe5 C57 114.2(2) . . ? C62 Fe5 C57 105.2(2) . . ? C59 Fe5 C57 68.8(2) . . ? C64 Fe5 C57 149.4(2) . . ? C60 Fe5 C57 68.8(2) . . ? C58 Fe5 C57 40.76(19) . . ? C61 Fe5 C57 40.86(18) . . ? C66 Fe5 C57 126.6(2) . . ? C65 Fe5 C57 166.8(3) . . ? C73 Fe6 C76 163.8(2) . . ? C73 Fe6 C74 39.96(19) . . ? C76 Fe6 C74 154.1(2) . . ? C73 Fe6 C77 127.1(2) . . ? C76 Fe6 C77 40.5(2) . . ? C74 Fe6 C77 164.9(2) . . ? C73 Fe6 C75 68.26(19) . . ? C76 Fe6 C75 118.3(2) . . ? C74 Fe6 C75 41.26(18) . . ? C77 Fe6 C75 151.8(2) . . ? C73 Fe6 C80 154.5(2) . . ? C76 Fe6 C80 40.9(2) . . ? C74 Fe6 C80 120.3(2) . . ? C77 Fe6 C80 68.6(2) . . ? C75 Fe6 C80 107.8(2) . . ? C73 Fe6 C79 121.4(2) . . ? C76 Fe6 C79 67.8(2) . . ? C74 Fe6 C79 109.7(2) . . ? C77 Fe6 C79 68.5(2) . . ? C75 Fe6 C79 127.7(2) . . ? C80 Fe6 C79 39.9(2) . . ? C73 Fe6 C78 109.6(2) . . ? C76 Fe6 C78 67.8(2) . . ? C74 Fe6 C78 128.2(2) . . ? C77 Fe6 C78 40.7(2) . . ? C75 Fe6 C78 165.9(2) . . ? C80 Fe6 C78 67.8(2) . . ? C79 Fe6 C78 40.5(2) . . ? C73 Fe6 C72 41.26(18) . . ? C76 Fe6 C72 124.8(2) . . ? C74 Fe6 C72 68.73(19) . . ? C77 Fe6 C72 106.2(2) . . ? C75 Fe6 C72 68.60(17) . . ? C80 Fe6 C72 162.9(2) . . ? C79 Fe6 C72 155.1(2) . . ? C78 Fe6 C72 119.6(2) . . ? C73 Fe6 C71 69.20(18) . . ? C76 Fe6 C71 105.4(2) . . ? C74 Fe6 C71 69.36(18) . . ? C77 Fe6 C71 116.9(2) . . ? C75 Fe6 C71 40.84(16) . . ? C80 Fe6 C71 125.3(2) . . ? C79 Fe6 C71 163.5(2) . . ? C78 Fe6 C71 152.7(2) . . ? C72 Fe6 C71 41.14(17) . . ? C1 P1 Li1 135.6(2) . . ? C1 P1 Li4 80.6(2) . . ? Li1 P1 Li4 133.7(3) . . ? C1 P1 Li3 114.7(2) . . ? Li1 P1 Li3 71.2(3) . . ? Li4 P1 Li3 126.3(3) . . ? C1 P1 Li5 68.9(2) . . ? Li1 P1 Li5 140.8(3) . . ? Li4 P1 Li5 69.2(3) . . ? Li3 P1 Li5 70.1(3) . . ? C1 P1 Li2 141.3(2) . . ? Li1 P1 Li2 68.9(3) . . ? Li4 P1 Li2 65.8(2) . . ? Li3 P1 Li2 101.0(2) . . ? Li5 P1 Li2 112.9(2) . . ? C1 P1 Li8 120.2(2) . . ? Li1 P1 Li8 102.0(2) . . ? Li4 P1 Li8 65.2(2) . . ? Li3 P1 Li8 62.9(2) . . ? Li5 P1 Li8 53.9(2) . . ? Li2 P1 Li8 63.0(2) . . ? C15 P2 Li1 134.6(2) . . ? C15 P2 Li6 82.1(2) . . ? Li1 P2 Li6 133.0(3) . . ? C15 P2 Li2 117.8(2) . . ? Li1 P2 Li2 69.2(3) . . ? Li6 P2 Li2 125.7(2) . . ? C15 P2 Li3 139.8(2) . . ? Li1 P2 Li3 69.7(3) . . ? Li6 P2 Li3 64.0(2) . . ? Li2 P2 Li3 100.0(2) . . ? C15 P2 Li7 71.4(2) . . ? Li1 P2 Li7 139.2(3) . . ? Li6 P2 Li7 70.3(2) . . ? Li2 P2 Li7 70.3(3) . . ? Li3 P2 Li7 112.8(2) . . ? C15 P2 Li8 122.4(2) . . ? Li1 P2 Li8 101.3(2) . . ? Li6 P2 Li8 63.6(2) . . ? Li2 P2 Li8 63.4(2) . . ? Li3 P2 Li8 62.0(2) . . ? Li7 P2 Li8 54.5(2) . . ? C29 P3 Li12 132.8(2) . . ? C29 P3 Li2 82.3(2) . . ? Li12 P3 Li2 136.1(3) . . ? C29 P3 Li10 116.4(2) . . ? Li12 P3 Li10 68.4(3) . . ? Li2 P3 Li10 125.5(2) . . ? C29 P3 Li4 140.8(2) . . ? Li12 P3 Li4 70.9(3) . . ? Li2 P3 Li4 65.7(2) . . ? Li10 P3 Li4 100.9(3) . . ? C29 P3 Li7 72.5(2) . . ? Li12 P3 Li7 136.3(3) . . ? Li2 P3 Li7 70.7(2) . . ? Li10 P3 Li7 68.2(2) . . ? Li4 P3 Li7 113.9(2) . . ? C29 P3 Li8 122.5(2) . . ? Li12 P3 Li8 102.0(3) . . ? Li2 P3 Li8 63.7(2) . . ? Li10 P3 Li8 63.4(2) . . ? Li4 P3 Li8 63.2(2) . . ? Li7 P3 Li8 53.6(2) . . ? C43 P4 Li11 133.0(2) . . ? C43 P4 Li9 117.7(2) . . ? Li11 P4 Li9 70.7(3) . . ? C43 P4 Li3 84.1(2) . . ? Li11 P4 Li3 131.1(3) . . ? Li9 P4 Li3 125.6(3) . . ? C43 P4 Li6 140.7(2) . . ? Li11 P4 Li6 68.0(3) . . ? Li9 P4 Li6 100.0(2) . . ? Li3 P4 Li6 63.9(2) . . ? C43 P4 Li5 74.2(2) . . ? Li11 P4 Li5 139.8(3) . . ? Li9 P4 Li5 69.9(3) . . ? Li3 P4 Li5 70.0(2) . . ? Li6 P4 Li5 111.9(2) . . ? C43 P4 Li8 123.7(2) . . ? Li11 P4 Li8 102.1(3) . . ? Li9 P4 Li8 64.6(3) . . ? Li3 P4 Li8 62.2(2) . . ? Li6 P4 Li8 61.8(2) . . ? Li5 P4 Li8 53.1(2) . . ? C57 P5 Li12 131.2(2) . . ? C57 P5 Li9 83.7(3) . . ? Li12 P5 Li9 130.5(3) . . ? C57 P5 Li4 120.1(2) . . ? Li12 P5 Li4 71.8(3) . . ? Li9 P5 Li4 125.8(3) . . ? C57 P5 Li5 78.3(2) . . ? Li12 P5 Li5 139.6(3) . . ? Li9 P5 Li5 70.4(3) . . ? Li4 P5 Li5 68.8(3) . . ? C57 P5 Li10 139.2(2) . . ? Li12 P5 Li10 66.6(3) . . ? Li9 P5 Li10 64.9(3) . . ? Li4 P5 Li10 99.7(2) . . ? Li5 P5 Li10 111.7(2) . . ? C57 P5 Li8 127.6(2) . . ? Li12 P5 Li8 100.7(2) . . ? Li9 P5 Li8 64.0(2) . . ? Li4 P5 Li8 63.3(2) . . ? Li5 P5 Li8 53.1(2) . . ? Li10 P5 Li8 61.7(2) . . ? C71 P6 Li11 134.0(2) . . ? C71 P6 Li10 82.1(2) . . ? Li11 P6 Li10 134.3(3) . . ? C71 P6 Li6 117.0(2) . . ? Li11 P6 Li6 69.1(3) . . ? Li10 P6 Li6 125.4(2) . . ? C71 P6 Li7 70.8(2) . . ? Li11 P6 Li7 139.2(3) . . ? Li10 P6 Li7 69.6(3) . . ? Li6 P6 Li7 70.4(2) . . ? C71 P6 Li9 140.9(2) . . ? Li11 P6 Li9 68.9(3) . . ? Li10 P6 Li9 65.9(3) . . ? Li6 P6 Li9 100.2(2) . . ? Li7 P6 Li9 114.5(3) . . ? C71 P6 Li8 121.9(2) . . ? Li11 P6 Li8 101.9(3) . . ? Li10 P6 Li8 63.8(2) . . ? Li6 P6 Li8 63.0(2) . . ? Li7 P6 Li8 54.2(2) . . ? Li9 P6 Li8 63.8(2) . . ? C13 N1 C14 109.1(4) . . ? C13 N1 C11 111.4(4) . . ? C14 N1 C11 113.4(4) . . ? C13 N1 Li4 107.7(4) . . ? C14 N1 Li4 108.4(4) . . ? C11 N1 Li4 106.6(3) . . ? C28 N2 C27 109.1(4) . . ? C28 N2 C25 112.9(4) . . ? C27 N2 C25 111.4(4) . . ? C28 N2 Li6 109.2(3) . . ? C27 N2 Li6 107.0(4) . . ? C25 N2 Li6 107.0(3) . . ? C41 N3 C42 108.9(4) . . ? C41 N3 C39 114.6(4) . . ? C42 N3 C39 110.6(4) . . ? C41 N3 Li2 108.8(4) . . ? C42 N3 Li2 108.0(4) . . ? C39 N3 Li2 105.8(3) . . ? C55 N4 C56 108.3(4) . . ? C55 N4 C53 112.4(4) . . ? C56 N4 C53 112.2(4) . . ? C55 N4 Li3 108.4(4) . . ? C56 N4 Li3 107.6(4) . . ? C53 N4 Li3 107.7(3) . . ? C69 N5 C70 108.3(5) . . ? C69 N5 C67 113.5(5) . . ? C70 N5 C67 113.0(5) . . ? C69 N5 Li9 109.2(4) . . ? C70 N5 Li9 106.6(4) . . ? C67 N5 Li9 106.0(4) . . ? C84 N6 C83 109.1(4) . . ? C84 N6 C81 112.8(4) . . ? C83 N6 C81 111.7(4) . . ? C84 N6 Li10 110.6(4) . . ? C83 N6 Li10 104.7(4) . . ? C81 N6 Li10 107.5(3) . . ? C5 C1 C2 104.6(4) . . ? C5 C1 P1 125.3(3) . . ? C2 C1 P1 129.9(3) . . ? C5 C1 Fe1 66.9(2) . . ? C2 C1 Fe1 67.3(2) . . ? P1 C1 Fe1 133.7(2) . . ? C5 C1 Li5 73.3(3) . . ? C2 C1 Li5 127.0(3) . . ? P1 C1 Li5 70.3(2) . . ? Fe1 C1 Li5 140.1(3) . . ? C3 C2 C1 109.7(4) . . ? C3 C2 C11 126.6(4) . . ? C1 C2 C11 123.5(4) . . ? C3 C2 Fe1 68.7(3) . . ? C1 C2 Fe1 72.2(3) . . ? C11 C2 Fe1 130.0(3) . . ? C4 C3 C2 107.6(4) . . ? C4 C3 Fe1 69.4(3) . . ? C2 C3 Fe1 70.6(3) . . ? C3 C4 C5 108.8(5) . . ? C3 C4 Fe1 70.1(3) . . ? C5 C4 Fe1 70.6(3) . . ? C4 C5 C1 109.3(4) . . ? C4 C5 Fe1 68.7(3) . . ? C1 C5 Fe1 72.6(3) . . ? C4 C5 Li5 125.4(4) . . ? C1 C5 Li5 74.6(3) . . ? Fe1 C5 Li5 147.1(3) . . ? C7 C6 C10 108.6(5) . . ? C7 C6 Fe1 69.8(3) . . ? C10 C6 Fe1 70.7(3) . . ? C6 C7 C8 108.5(5) . . ? C6 C7 Fe1 70.1(3) . . ? C8 C7 Fe1 70.5(3) . . ? C9 C8 C7 106.3(5) . . ? C9 C8 Fe1 69.4(3) . . ? C7 C8 Fe1 68.1(3) . . ? C8 C9 C10 108.8(5) . . ? C8 C9 Fe1 70.4(3) . . ? C10 C9 Fe1 70.1(3) . . ? C6 C10 C9 107.8(5) . . ? C6 C10 Fe1 68.9(3) . . ? C9 C10 Fe1 69.6(3) . . ? N1 C11 C2 109.1(4) . . ? N1 C11 C12 114.6(4) . . ? C2 C11 C12 112.1(4) . . ? C19 C15 C16 104.1(4) . . ? C19 C15 P2 126.1(3) . . ? C16 C15 P2 129.8(3) . . ? C19 C15 Fe2 67.1(2) . . ? C16 C15 Fe2 67.1(2) . . ? P2 C15 Fe2 131.0(2) . . ? C19 C15 Li7 79.1(3) . . ? C16 C15 Li7 126.3(3) . . ? P2 C15 Li7 68.4(2) . . ? Fe2 C15 Li7 146.1(3) . . ? C17 C16 C15 109.5(4) . . ? C17 C16 C25 125.6(4) . . ? C15 C16 C25 124.9(4) . . ? C17 C16 Fe2 68.9(3) . . ? C15 C16 Fe2 71.9(2) . . ? C25 C16 Fe2 126.0(3) . . ? C16 C17 C18 108.8(4) . . ? C16 C17 Fe2 70.6(2) . . ? C18 C17 Fe2 70.3(3) . . ? C17 C18 C19 106.7(4) . . ? C17 C18 Fe2 68.9(3) . . ? C19 C18 Fe2 69.4(3) . . ? C18 C19 C15 110.9(4) . . ? C18 C19 Fe2 69.7(3) . . ? C15 C19 Fe2 72.5(3) . . ? C21 C20 C24 108.2(5) . . ? C21 C20 Fe2 70.4(3) . . ? C24 C20 Fe2 69.3(3) . . ? C22 C21 C20 107.4(5) . . ? C22 C21 Fe2 70.4(3) . . ? C20 C21 Fe2 69.0(3) . . ? C21 C22 C23 108.5(5) . . ? C21 C22 Fe2 69.4(3) . . ? C23 C22 Fe2 69.3(3) . . ? C24 C23 C22 108.2(5) . . ? C24 C23 Fe2 69.1(3) . . ? C22 C23 Fe2 70.3(3) . . ? C23 C24 C20 107.7(5) . . ? C23 C24 Fe2 70.6(3) . . ? C20 C24 Fe2 69.5(3) . . ? N2 C25 C16 109.0(4) . . ? N2 C25 C26 113.5(4) . . ? C16 C25 C26 114.7(4) . . ? C33 C29 C30 104.7(4) . . ? C33 C29 P3 125.9(4) . . ? C30 C29 P3 129.2(4) . . ? C33 C29 Fe3 67.8(3) . . ? C30 C29 Fe3 67.3(3) . . ? P3 C29 Fe3 131.6(2) . . ? C33 C29 Li7 77.4(3) . . ? C30 C29 Li7 127.0(3) . . ? P3 C29 Li7 68.4(2) . . ? Fe3 C29 Li7 145.1(3) . . ? C31 C30 C29 109.1(5) . . ? C31 C30 C39 127.0(5) . . ? C29 C30 C39 123.9(4) . . ? C31 C30 Fe3 68.5(3) . . ? C29 C30 Fe3 71.6(3) . . ? C39 C30 Fe3 127.2(3) . . ? C32 C31 C30 107.7(5) . . ? C32 C31 Fe3 69.2(3) . . ? C30 C31 Fe3 70.3(3) . . ? C31 C32 C33 108.8(5) . . ? C31 C32 Fe3 70.1(3) . . ? C33 C32 Fe3 71.2(3) . . ? C32 C33 C29 109.7(5) . . ? C32 C33 Fe3 68.0(3) . . ? C29 C33 Fe3 71.7(3) . . ? C38 C34 C35 107.8(6) . . ? C38 C34 Fe3 70.5(4) . . ? C35 C34 Fe3 69.8(4) . . ? C36 C35 C34 108.6(6) . . ? C36 C35 Fe3 70.7(4) . . ? C34 C35 Fe3 69.6(4) . . ? C35 C36 C37 106.3(6) . . ? C35 C36 Fe3 69.0(4) . . ? C37 C36 Fe3 69.7(4) . . ? C38 C37 C36 109.4(7) . . ? C38 C37 Fe3 69.9(4) . . ? C36 C37 Fe3 70.1(4) . . ? C37 C38 C34 107.9(6) . . ? C37 C38 Fe3 70.4(4) . . ? C34 C38 Fe3 69.4(3) . . ? N3 C39 C30 108.7(4) . . ? N3 C39 C40 113.5(4) . . ? C30 C39 C40 112.0(4) . . ? C47 C43 C44 104.3(4) . . ? C47 C43 P4 127.1(4) . . ? C44 C43 P4 128.5(3) . . ? C47 C43 Fe4 67.0(3) . . ? C44 C43 Fe4 67.3(3) . . ? P4 C43 Fe4 131.2(2) . . ? C47 C43 Li5 81.7(3) . . ? C44 C43 Li5 126.5(3) . . ? P4 C43 Li5 66.5(2) . . ? Fe4 C43 Li5 148.6(3) . . ? C45 C44 C43 108.9(4) . . ? C45 C44 C53 126.5(4) . . ? C43 C44 C53 124.6(4) . . ? C45 C44 Fe4 68.9(3) . . ? C43 C44 Fe4 71.8(3) . . ? C53 C44 Fe4 126.6(3) . . ? C46 C45 C44 107.6(4) . . ? C46 C45 Fe4 70.2(3) . . ? C44 C45 Fe4 69.6(3) . . ? C47 C46 C45 108.1(4) . . ? C47 C46 Fe4 69.5(3) . . ? C45 C46 Fe4 69.4(3) . . ? C46 C47 C43 111.1(5) . . ? C46 C47 Fe4 70.4(3) . . ? C43 C47 Fe4 72.5(3) . . ? C49 C48 C52 110.0(6) . . ? C49 C48 Fe4 70.6(4) . . ? C52 C48 Fe4 71.1(4) . . ? C48 C49 C50 108.5(7) . . ? C48 C49 Fe4 69.9(4) . . ? C50 C49 Fe4 69.9(4) . . ? C51 C50 C49 105.2(8) . . ? C51 C50 Fe4 68.6(5) . . ? C49 C50 Fe4 69.2(4) . . ? C50 C51 C52 111.3(9) . . ? C50 C51 Fe4 71.9(6) . . ? C52 C51 Fe4 71.4(4) . . ? C48 C52 C51 104.9(8) . . ? C48 C52 Fe4 69.1(4) . . ? C51 C52 Fe4 67.8(5) . . ? C44 C53 N4 110.7(4) . . ? C44 C53 C54 112.1(4) . . ? N4 C53 C54 113.9(4) . . ? C58 C57 C61 105.1(4) . . ? C58 C57 P5 130.0(4) . . ? C61 C57 P5 124.8(4) . . ? C58 C57 Fe5 67.4(3) . . ? C61 C57 Fe5 67.5(3) . . ? P5 C57 Fe5 130.0(3) . . ? C59 C58 C57 110.0(5) . . ? C59 C58 C67 125.5(5) . . ? C57 C58 C67 124.4(4) . . ? C59 C58 Fe5 69.5(3) . . ? C57 C58 Fe5 71.9(3) . . ? C67 C58 Fe5 127.0(4) . . ? C58 C59 C60 108.1(5) . . ? C58 C59 Fe5 70.1(3) . . ? C60 C59 Fe5 70.0(4) . . ? C59 C60 C61 108.1(5) . . ? C59 C60 Fe5 69.4(3) . . ? C61 C60 Fe5 69.7(3) . . ? C60 C61 C57 108.6(5) . . ? C60 C61 Fe5 69.2(3) . . ? C57 C61 Fe5 71.6(3) . . ? C63 C62 C66 109.9(6) . . ? C63 C62 Fe5 69.4(4) . . ? C66 C62 Fe5 71.2(4) . . ? C62 C63 C64 108.0(6) . . ? C62 C63 Fe5 70.3(4) . . ? C64 C63 Fe5 70.0(4) . . ? C65 C64 C63 107.1(6) . . ? C65 C64 Fe5 71.5(4) . . ? C63 C64 Fe5 68.3(3) . . ? C64 C65 C66 107.7(6) . . ? C64 C65 Fe5 68.4(3) . . ? C66 C65 Fe5 68.7(3) . . ? C62 C66 C65 107.3(6) . . ? C62 C66 Fe5 69.0(4) . . ? C65 C66 Fe5 70.4(4) . . ? N5 C67 C58 110.4(4) . . ? N5 C67 C68 113.0(5) . . ? C58 C67 C68 112.4(4) . . ? C75 C71 C72 105.0(4) . . ? C75 C71 P6 126.2(3) . . ? C72 C71 P6 128.7(3) . . ? C75 C71 Fe6 67.0(2) . . ? C72 C71 Fe6 67.8(2) . . ? P6 C71 Fe6 131.6(2) . . ? C75 C71 Li7 77.9(3) . . ? C72 C71 Li7 126.5(4) . . ? P6 C71 Li7 68.7(2) . . ? Fe6 C71 Li7 144.8(3) . . ? C73 C72 C71 107.4(4) . . ? C73 C72 C81 128.4(4) . . ? C71 C72 C81 124.1(4) . . ? C73 C72 Fe6 67.4(3) . . ? C71 C72 Fe6 71.0(3) . . ? C81 C72 Fe6 127.6(3) . . ? C74 C73 C72 110.1(4) . . ? C74 C73 Fe6 70.5(3) . . ? C72 C73 Fe6 71.4(3) . . ? C73 C74 C75 107.9(4) . . ? C73 C74 Fe6 69.5(3) . . ? C75 C74 Fe6 70.0(3) . . ? C74 C75 C71 109.5(4) . . ? C74 C75 Fe6 68.7(3) . . ? C71 C75 Fe6 72.1(2) . . ? C74 C75 Li7 127.0(4) . . ? C71 C75 Li7 71.3(3) . . ? Fe6 C75 Li7 143.3(3) . . ? C77 C76 C80 109.0(5) . . ? C77 C76 Fe6 70.3(4) . . ? C80 C76 Fe6 70.4(3) . . ? C76 C77 C78 107.1(5) . . ? C76 C77 Fe6 69.2(3) . . ? C78 C77 Fe6 70.3(3) . . ? C79 C78 C77 107.8(5) . . ? C79 C78 Fe6 69.5(3) . . ? C77 C78 Fe6 69.0(3) . . ? C80 C79 C78 108.6(5) . . ? C80 C79 Fe6 69.9(3) . . ? C78 C79 Fe6 70.0(3) . . ? C79 C80 C76 107.5(5) . . ? C79 C80 Fe6 70.2(3) . . ? C76 C80 Fe6 68.8(3) . . ? C72 C81 N6 108.8(4) . . ? C72 C81 C82 113.4(4) . . ? N6 C81 C82 113.7(4) . . ? C88 O1 C85 108.6(4) . . ? C88 O1 Li1 124.2(4) . . ? C85 O1 Li1 126.9(4) . . ? O1 C85 C86 106.3(6) . . ? C87 C86 C85 105.4(6) . . ? C86 C87 C88 103.4(6) . . ? O1 C88 C87 106.3(5) . . ? O1 Li1 P1 133.8(4) . . ? O1 Li1 P2 142.2(4) . . ? P1 Li1 P2 83.8(2) . . ? O1 Li1 Li2 132.1(4) . . ? P1 Li1 Li2 58.5(2) . . ? P2 Li1 Li2 57.5(2) . . ? O1 Li1 Li3 140.2(4) . . ? P1 Li1 Li3 56.1(2) . . ? P2 Li1 Li3 57.6(2) . . ? Li2 Li1 Li3 87.4(3) . . ? N3 Li2 P3 107.8(3) . . ? N3 Li2 P2 122.1(3) . . ? P3 Li2 P2 109.9(3) . . ? N3 Li2 P1 128.1(3) . . ? P3 Li2 P1 107.8(3) . . ? P2 Li2 P1 77.9(2) . . ? N3 Li2 Li4 118.5(4) . . ? P3 Li2 Li4 59.4(2) . . ? P2 Li2 Li4 118.1(3) . . ? P1 Li2 Li4 55.5(2) . . ? N3 Li2 Li8 170.2(4) . . ? P3 Li2 Li8 63.1(2) . . ? P2 Li2 Li8 61.3(2) . . ? P1 Li2 Li8 60.8(2) . . ? Li4 Li2 Li8 61.1(3) . . ? N3 Li2 Li1 98.5(3) . . ? P3 Li2 Li1 153.7(3) . . ? P2 Li2 Li1 53.3(2) . . ? P1 Li2 Li1 52.5(2) . . ? Li4 Li2 Li1 107.5(3) . . ? Li8 Li2 Li1 90.7(3) . . ? N3 Li2 Li7 122.7(4) . . ? P3 Li2 Li7 57.1(2) . . ? P2 Li2 Li7 55.4(2) . . ? P1 Li2 Li7 108.2(3) . . ? Li4 Li2 Li7 100.2(3) . . ? Li8 Li2 Li7 50.1(2) . . ? Li1 Li2 Li7 108.5(3) . . ? N4 Li3 P4 106.3(4) . . ? N4 Li3 P1 121.9(4) . . ? P4 Li3 P1 110.7(3) . . ? N4 Li3 P2 127.5(4) . . ? P4 Li3 P2 109.3(3) . . ? P1 Li3 P2 78.7(2) . . ? N4 Li3 Li6 117.8(4) . . ? P4 Li3 Li6 59.6(2) . . ? P1 Li3 Li6 119.2(3) . . ? P2 Li3 Li6 56.4(2) . . ? N4 Li3 Li8 169.6(5) . . ? P4 Li3 Li8 63.8(2) . . ? P1 Li3 Li8 62.2(2) . . ? P2 Li3 Li8 61.6(2) . . ? Li6 Li3 Li8 61.1(3) . . ? N4 Li3 Li1 99.1(3) . . ? P4 Li3 Li1 154.6(3) . . ? P1 Li3 Li1 52.7(2) . . ? P2 Li3 Li1 52.7(2) . . ? Li6 Li3 Li1 108.6(3) . . ? Li8 Li3 Li1 90.8(3) . . ? N4 Li3 Li5 122.5(4) . . ? P4 Li3 Li5 56.6(2) . . ? P1 Li3 Li5 56.1(2) . . ? P2 Li3 Li5 109.1(3) . . ? Li6 Li3 Li5 99.7(3) . . ? Li8 Li3 Li5 50.2(3) . . ? Li1 Li3 Li5 108.6(3) . . ? N1 Li4 P1 106.8(3) . . ? N1 Li4 P5 122.9(3) . . ? P1 Li4 P5 109.9(3) . . ? N1 Li4 P3 129.6(4) . . ? P1 Li4 P3 106.6(3) . . ? P5 Li4 P3 78.0(2) . . ? N1 Li4 Li2 118.6(4) . . ? P1 Li4 Li2 58.7(2) . . ? P5 Li4 Li2 117.6(3) . . ? P3 Li4 Li2 54.9(2) . . ? N1 Li4 Li8 167.4(4) . . ? P1 Li4 Li8 61.2(2) . . ? P5 Li4 Li8 62.7(2) . . ? P3 Li4 Li8 61.0(2) . . ? Li2 Li4 Li8 59.7(3) . . ? N1 Li4 Li5 121.9(4) . . ? P1 Li4 Li5 56.8(2) . . ? P5 Li4 Li5 55.8(2) . . ? P3 Li4 Li5 107.9(3) . . ? Li2 Li4 Li5 99.4(3) . . ? Li8 Li4 Li5 49.9(3) . . ? N1 Li4 Li12 103.2(4) . . ? P1 Li4 Li12 150.0(4) . . ? P5 Li4 Li12 51.6(2) . . ? P3 Li4 Li12 51.0(2) . . ? Li2 Li4 Li12 105.6(3) . . ? Li8 Li4 Li12 89.0(3) . . ? Li5 Li4 Li12 106.9(3) . . ? Li8 Li5 C5 133.3(4) . . ? Li8 Li5 C1 104.8(4) . . ? C5 Li5 C1 32.16(17) . . ? Li8 Li5 P5 68.5(3) . . ? C5 Li5 P5 130.6(3) . . ? C1 Li5 P5 112.5(3) . . ? Li8 Li5 P1 65.8(3) . . ? C5 Li5 P1 67.6(2) . . ? C1 Li5 P1 40.77(16) . . ? P5 Li5 P1 106.8(3) . . ? Li8 Li5 P4 67.1(3) . . ? C5 Li5 P4 123.5(3) . . ? C1 Li5 P4 134.6(3) . . ? P5 Li5 P4 105.6(3) . . ? P1 Li5 P4 105.3(3) . . ? Li8 Li5 C43 104.2(3) . . ? C5 Li5 C43 88.6(3) . . ? C1 Li5 C43 113.2(3) . . ? P5 Li5 C43 134.0(3) . . ? P1 Li5 C43 110.8(3) . . ? P4 Li5 C43 39.34(15) . . ? Li8 Li5 Li4 63.5(3) . . ? C5 Li5 Li4 91.9(3) . . ? C1 Li5 Li4 62.1(2) . . ? P5 Li5 Li4 55.4(2) . . ? P1 Li5 Li4 54.0(2) . . ? P4 Li5 Li4 130.6(3) . . ? C43 Li5 Li4 162.6(4) . . ? Li8 Li5 Li9 63.2(3) . . ? C5 Li5 Li9 162.9(4) . . ? C1 Li5 Li9 163.7(4) . . ? P5 Li5 Li9 54.0(2) . . ? P1 Li5 Li9 129.0(3) . . ? P4 Li5 Li9 53.4(2) . . ? C43 Li5 Li9 81.6(3) . . ? Li4 Li5 Li9 101.7(3) . . ? Li8 Li5 Li3 60.8(3) . . ? C5 Li5 Li3 88.6(3) . . ? C1 Li5 Li3 83.0(3) . . ? P5 Li5 Li3 129.3(3) . . ? P1 Li5 Li3 53.8(2) . . ? P4 Li5 Li3 53.4(2) . . ? C43 Li5 Li3 62.2(3) . . ? Li4 Li5 Li3 100.5(3) . . ? Li9 Li5 Li3 98.9(3) . . ? N2 Li6 P2 107.9(3) . . ? N2 Li6 P6 120.4(3) . . ? P2 Li6 P6 110.2(3) . . ? N2 Li6 P4 127.2(3) . . ? P2 Li6 P4 109.5(3) . . ? P6 Li6 P4 78.7(2) . . ? N2 Li6 Li3 119.5(3) . . ? P2 Li6 Li3 59.6(2) . . ? P6 Li6 Li3 119.0(3) . . ? P4 Li6 Li3 56.5(2) . . ? N2 Li6 Li8 169.4(4) . . ? P2 Li6 Li8 62.3(2) . . ? P6 Li6 Li8 63.2(2) . . ? P4 Li6 Li8 62.5(2) . . ? Li3 Li6 Li8 60.2(3) . . ? N2 Li6 Li11 96.9(3) . . ? P2 Li6 Li11 155.2(4) . . ? P6 Li6 Li11 53.9(2) . . ? P4 Li6 Li11 52.6(2) . . ? Li3 Li6 Li11 108.6(3) . . ? Li8 Li6 Li11 93.0(3) . . ? N2 Li6 Li7 121.5(4) . . ? P2 Li6 Li7 56.4(2) . . ? P6 Li6 Li7 56.1(2) . . ? P4 Li6 Li7 110.0(3) . . ? Li3 Li6 Li7 100.1(3) . . ? Li8 Li6 Li7 50.7(3) . . ? Li11 Li6 Li7 109.8(3) . . ? Li8 Li7 P6 66.7(3) . . ? Li8 Li7 P2 65.5(3) . . ? P6 Li7 P2 104.7(3) . . ? Li8 Li7 C71 105.1(4) . . ? P6 Li7 C71 40.41(16) . . ? P2 Li7 C71 135.1(4) . . ? Li8 Li7 P3 65.8(3) . . ? P6 Li7 P3 104.9(3) . . ? P2 Li7 P3 104.2(3) . . ? C71 Li7 P3 111.3(3) . . ? Li8 Li7 C15 103.5(3) . . ? P6 Li7 C15 110.1(3) . . ? P2 Li7 C15 40.18(15) . . ? C71 Li7 C15 113.7(3) . . ? P3 Li7 C15 134.9(3) . . ? Li8 Li7 C75 132.4(4) . . ? P6 Li7 C75 65.8(2) . . ? P2 Li7 C75 125.4(3) . . ? C71 Li7 C75 30.86(16) . . ? P3 Li7 C75 130.5(3) . . ? C15 Li7 C75 90.2(3) . . ? Li8 Li7 C29 102.6(4) . . ? P6 Li7 C29 134.8(3) . . ? P2 Li7 C29 110.0(3) . . ? C71 Li7 C29 114.9(3) . . ? P3 Li7 C29 39.11(15) . . ? C15 Li7 C29 115.1(3) . . ? C75 Li7 C29 112.4(3) . . ? Li8 Li7 Li10 62.3(3) . . ? P6 Li7 Li10 53.5(2) . . ? P2 Li7 Li10 127.8(3) . . ? C71 Li7 Li10 62.2(2) . . ? P3 Li7 Li10 53.9(2) . . ? C15 Li7 Li10 160.7(4) . . ? C75 Li7 Li10 91.1(3) . . ? C29 Li7 Li10 82.1(3) . . ? Li8 Li7 Li6 61.1(3) . . ? P6 Li7 Li6 53.5(2) . . ? P2 Li7 Li6 53.3(2) . . ? C71 Li7 Li6 83.0(3) . . ? P3 Li7 Li6 126.9(3) . . ? C15 Li7 Li6 61.8(2) . . ? C75 Li7 Li6 88.2(3) . . ? C29 Li7 Li6 159.4(4) . . ? Li10 Li7 Li6 99.1(3) . . ? Li8 Li7 Li2 60.9(3) . . ? P6 Li7 Li2 127.7(3) . . ? P2 Li7 Li2 54.3(2) . . ? C71 Li7 Li2 160.8(4) . . ? P3 Li7 Li2 52.2(2) . . ? C15 Li7 Li2 83.7(3) . . ? C75 Li7 Li2 166.5(4) . . ? C29 Li7 Li2 60.3(2) . . ? Li10 Li7 Li2 98.6(3) . . ? Li6 Li7 Li2 99.4(3) . . ? Li5 Li8 Li7 177.8(5) . . ? Li5 Li8 P1 60.3(3) . . ? Li7 Li8 P1 121.7(4) . . ? Li5 Li8 P2 122.2(3) . . ? Li7 Li8 P2 59.9(3) . . ? P1 Li8 P2 72.9(2) . . ? Li5 Li8 Li3 69.1(3) . . ? Li7 Li8 Li3 112.7(4) . . ? P1 Li8 Li3 54.9(2) . . ? P2 Li8 Li3 56.5(2) . . ? Li5 Li8 Li6 112.4(4) . . ? Li7 Li8 Li6 68.2(3) . . ? P1 Li8 Li6 110.2(3) . . ? P2 Li8 Li6 54.1(2) . . ? Li3 Li8 Li6 58.7(3) . . ? Li5 Li8 P3 118.8(4) . . ? Li7 Li8 P3 60.6(3) . . ? P1 Li8 P3 96.8(3) . . ? P2 Li8 P3 97.5(2) . . ? Li3 Li8 P3 144.3(4) . . ? Li6 Li8 P3 128.8(3) . . ? Li5 Li8 P6 119.4(4) . . ? Li7 Li8 P6 59.1(3) . . ? P1 Li8 P6 163.6(3) . . ? P2 Li8 P6 96.5(2) . . ? Li3 Li8 P6 108.9(3) . . ? Li6 Li8 P6 53.8(2) . . ? P3 Li8 P6 97.0(2) . . ? Li5 Li8 P4 59.8(3) . . ? Li7 Li8 P4 120.1(4) . . ? P1 Li8 P4 97.3(2) . . ? P2 Li8 P4 97.9(2) . . ? Li3 Li8 P4 54.0(2) . . ? Li6 Li8 P4 55.7(2) . . ? P3 Li8 P4 161.6(3) . . ? P6 Li8 P4 71.3(2) . . ? Li5 Li8 Li2 112.5(4) . . ? Li7 Li8 Li2 68.9(3) . . ? P1 Li8 Li2 56.2(2) . . ? P2 Li8 Li2 55.4(2) . . ? Li3 Li8 Li2 91.2(3) . . ? Li6 Li8 Li2 108.5(3) . . ? P3 Li8 Li2 53.2(2) . . ? P6 Li8 Li2 128.0(3) . . ? P4 Li8 Li2 145.1(3) . . ? Li5 Li8 Li10 111.1(4) . . ? Li7 Li8 Li10 66.8(3) . . ? P1 Li8 Li10 143.3(3) . . ? P2 Li8 Li10 126.8(3) . . ? Li3 Li8 Li10 160.5(4) . . ? Li6 Li8 Li10 106.0(3) . . ? P3 Li8 Li10 53.9(2) . . ? P6 Li8 Li10 53.1(2) . . ? P4 Li8 Li10 108.3(3) . . ? Li2 Li8 Li10 106.0(3) . . ? Li5 Li8 P5 58.4(3) . . ? Li7 Li8 P5 119.8(3) . . ? P1 Li8 P5 97.0(2) . . ? P2 Li8 P5 164.5(3) . . ? Li3 Li8 P5 127.4(3) . . ? Li6 Li8 P5 141.4(3) . . ? P3 Li8 P5 71.52(18) . . ? P6 Li8 P5 95.7(2) . . ? P4 Li8 P5 95.1(2) . . ? Li2 Li8 P5 109.3(3) . . ? Li10 Li8 P5 55.8(2) . . ? N5 Li9 P4 122.6(4) . . ? N5 Li9 P5 106.7(4) . . ? P4 Li9 P5 110.3(3) . . ? N5 Li9 P6 127.5(4) . . ? P4 Li9 P6 78.8(2) . . ? P5 Li9 P6 108.2(3) . . ? N5 Li9 Li10 118.3(4) . . ? P4 Li9 Li10 118.0(3) . . ? P5 Li9 Li10 59.3(3) . . ? P6 Li9 Li10 55.3(2) . . ? N5 Li9 Li11 99.7(4) . . ? P4 Li9 Li11 52.7(2) . . ? P5 Li9 Li11 153.6(4) . . ? P6 Li9 Li11 52.6(2) . . ? Li10 Li9 Li11 107.6(3) . . ? N5 Li9 Li8 169.4(4) . . ? P4 Li9 Li8 62.4(2) . . ? P5 Li9 Li8 63.0(2) . . ? P6 Li9 Li8 61.2(2) . . ? Li10 Li9 Li8 59.8(3) . . ? Li11 Li9 Li8 90.6(3) . . ? N5 Li9 Li5 123.6(4) . . ? P4 Li9 Li5 56.7(2) . . ? P5 Li9 Li5 55.6(2) . . ? P6 Li9 Li5 108.4(3) . . ? Li10 Li9 Li5 97.9(3) . . ? Li11 Li9 Li5 109.0(3) . . ? Li8 Li9 Li5 49.4(3) . . ? N6 Li10 P6 107.2(3) . . ? N6 Li10 P3 122.0(4) . . ? P6 Li10 P3 112.0(3) . . ? N6 Li10 P5 126.1(3) . . ? P6 Li10 P5 108.3(3) . . ? P3 Li10 P5 78.8(2) . . ? N6 Li10 Li9 117.1(4) . . ? P6 Li10 Li9 58.8(2) . . ? P3 Li10 Li9 119.3(3) . . ? P5 Li10 Li9 55.8(2) . . ? N6 Li10 Li12 97.1(3) . . ? P6 Li10 Li12 155.7(4) . . ? P3 Li10 Li12 53.7(2) . . ? P5 Li10 Li12 52.9(2) . . ? Li9 Li10 Li12 108.1(4) . . ? N6 Li10 Li8 169.8(4) . . ? P6 Li10 Li8 63.1(2) . . ? P3 Li10 Li8 62.7(2) . . ? P5 Li10 Li8 62.5(2) . . ? Li9 Li10 Li8 61.5(3) . . ? Li12 Li10 Li8 92.8(3) . . ? N6 Li10 Li7 122.2(4) . . ? P6 Li10 Li7 56.9(2) . . ? P3 Li10 Li7 58.0(2) . . ? P5 Li10 Li7 111.1(3) . . ? Li9 Li10 Li7 100.6(3) . . ? Li12 Li10 Li7 111.5(4) . . ? Li8 Li10 Li7 50.9(3) . . ? O2F Li11 O2 15.9(3) . . ? O2F Li11 P4 143.3(5) . . ? O2 Li11 P4 132.0(5) . . ? O2F Li11 P6 131.8(5) . . ? O2 Li11 P6 141.9(5) . . ? P4 Li11 P6 84.7(3) . . ? O2F Li11 Li6 138.0(5) . . ? O2 Li11 Li6 126.9(5) . . ? P4 Li11 Li6 59.4(2) . . ? P6 Li11 Li6 57.0(2) . . ? O2F Li11 Li9 133.4(5) . . ? O2 Li11 Li9 144.6(5) . . ? P4 Li11 Li9 56.6(2) . . ? P6 Li11 Li9 58.4(3) . . ? Li6 Li11 Li9 88.0(3) . . ? O3F Li12 O3 13.8(4) . . ? O3F Li12 P3 140.2(5) . . ? O3 Li12 P3 130.9(5) . . ? O3F Li12 P5 133.8(5) . . ? O3 Li12 P5 142.7(5) . . ? P3 Li12 P5 85.7(3) . . ? O3F Li12 Li10 130.2(5) . . ? O3 Li12 Li10 139.9(5) . . ? P3 Li12 Li10 57.9(2) . . ? P5 Li12 Li10 60.5(3) . . ? O3F Li12 Li4 141.2(5) . . ? O3 Li12 Li4 130.8(5) . . ? P3 Li12 Li4 58.2(2) . . ? P5 Li12 Li4 56.7(2) . . ? Li10 Li12 Li4 88.5(3) . . ? C89 O2 C92 106.9(7) . . ? C89 O2 Li11 123.2(8) . . ? C92 O2 Li11 127.6(8) . . ? O2 C89 C90 96.9(7) . . ? C89 C90 C91 110.5(7) . . ? C92 C91 C90 95.0(10) . . ? O2 C92 C91 102.9(7) . . ? C96 O3 C93 108.7(7) . . ? C96 O3 Li12 122.6(7) . . ? C93 O3 Li12 128.6(8) . . ? O3 C93 C94 101.1(8) . . ? C95 C94 C93 91.3(11) . . ? C94 C95 C96 111.9(7) . . ? O3 C96 C95 96.7(7) . . ? C89F O2F C92F 109.8(6) . . ? C89F O2F Li11 121.8(7) . . ? C92F O2F Li11 128.4(7) . . ? O2F C89F C90F 105.2(7) . . ? C89F C90F C91F 104.1(7) . . ? C92F C91F C90F 103.8(10) . . ? O2F C92F C91F 101.2(7) . . ? C93F O3F C96F 110.6(6) . . ? C93F O3F Li12 129.1(8) . . ? C96F O3F Li12 119.0(8) . . ? O3F C93F C94F 104.9(7) . . ? C93F C94F C95F 89.9(10) . . ? C96F C95F C94F 101.4(10) . . ? O3F C96F C95F 99.4(7) . . ? C102 C101 C100 110.8(16) . . ? C101 C102 C103 113.1(15) . . ? C104 C103 C102 117.3(16) . . ? C103 C104 C105 127.4(18) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.09 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.534 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.059 #------------------------------------------------------------------------------# # NEW STRUCTURE # #------------------------------------------------------------------------------# data_c2101fin _database_code_depnum_ccdc_archive 'CCDC 628374' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H32 Fe N P Si' _chemical_formula_weight 533.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 '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' Si Si 0.0817 0.0704 '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' 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' _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 10.0968(15) _cell_length_b 12.1986(18) _cell_length_c 12.968(2) _cell_angle_alpha 65.532(3) _cell_angle_beta 71.067(3) _cell_angle_gamma 85.882(3) _cell_volume 1371.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 3647 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.21 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Bruker CCD area detector' _diffrn_measurement_method '\W scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8247 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 28.52 _reflns_number_total 6459 _reflns_number_gt 5151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0533P)^2^+1.1246P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6459 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _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 0.40239(4) 0.29906(4) 0.83541(4) 0.03465(13) Uani 1 1 d . . . P1 P 0.11351(12) 0.44781(10) 0.89701(10) 0.0616(3) Uani 1 1 d . . . Si1 Si 0.42730(8) 0.18796(7) 0.61276(7) 0.03222(17) Uani 1 1 d . . . N1 N 0.0400(3) 0.2082(3) 0.7607(3) 0.0464(6) Uani 1 1 d . . . C1 C 0.2469(3) 0.4037(3) 0.7919(3) 0.0399(6) Uani 1 1 d . . . C2 C 0.2417(3) 0.2951(3) 0.7751(2) 0.0341(6) Uani 1 1 d . . . C3 C 0.3732(3) 0.2920(2) 0.6886(2) 0.0329(6) Uani 1 1 d . . . C4 C 0.4565(3) 0.3988(3) 0.6559(3) 0.0364(6) Uani 1 1 d . . . C5 C 0.3794(3) 0.4666(3) 0.7182(3) 0.0405(7) Uani 1 1 d . . . C6 C 0.3607(5) 0.2386(4) 1.0152(3) 0.0646(11) Uani 1 1 d . . . C7 C 0.3923(5) 0.1424(4) 0.9808(3) 0.0599(10) Uani 1 1 d . . . C8 C 0.5275(5) 0.1673(4) 0.8985(4) 0.0617(10) Uani 1 1 d . . . C9 C 0.5789(5) 0.2807(4) 0.8809(4) 0.0676(11) Uani 1 1 d . . . C10 C 0.4754(5) 0.3241(4) 0.9527(4) 0.0669(11) Uani 1 1 d . . . C11 C 0.1217(3) 0.2021(3) 0.8372(3) 0.0392(6) Uani 1 1 d . . . C12 C -0.0253(4) 0.3213(4) 0.7259(4) 0.0605(10) Uani 1 1 d . . . C13 C -0.0633(4) 0.1062(5) 0.8229(4) 0.0631(11) Uani 1 1 d . . . C14 C 0.3868(3) 0.2601(2) 0.4688(2) 0.0339(6) Uani 1 1 d . . . C15 C 0.4526(4) 0.2294(3) 0.3733(3) 0.0440(7) Uani 1 1 d . . . C16 C 0.4177(4) 0.2791(3) 0.2693(3) 0.0538(9) Uani 1 1 d . . . C17 C 0.3154(4) 0.3598(3) 0.2593(3) 0.0530(9) Uani 1 1 d . . . C18 C 0.2500(4) 0.3929(3) 0.3514(3) 0.0512(8) Uani 1 1 d . . . C19 C 0.2851(3) 0.3426(3) 0.4556(3) 0.0431(7) Uani 1 1 d . . . C20 C 0.3304(3) 0.0356(3) 0.7016(3) 0.0363(6) Uani 1 1 d . . . C21 C 0.2438(4) -0.0042(3) 0.6574(3) 0.0438(7) Uani 1 1 d . . . C22 C 0.1707(4) -0.1157(3) 0.7213(4) 0.0550(9) Uani 1 1 d . . . C23 C 0.1805(5) -0.1898(3) 0.8313(4) 0.0600(10) Uani 1 1 d . . . C24 C 0.2657(5) -0.1534(3) 0.8767(3) 0.0559(9) Uani 1 1 d . . . C25 C 0.3393(4) -0.0426(3) 0.8134(3) 0.0470(8) Uani 1 1 d . . . C26 C 0.6218(3) 0.1727(3) 0.5773(3) 0.0391(6) Uani 1 1 d . . . C27 C 0.6779(4) 0.0626(3) 0.6255(3) 0.0500(8) Uani 1 1 d . . . C28 C 0.8223(5) 0.0559(5) 0.5977(5) 0.0675(12) Uani 1 1 d . . . C29 C 0.9117(5) 0.1556(5) 0.5254(4) 0.0696(12) Uani 1 1 d . . . C30 C 0.8596(4) 0.2639(5) 0.4763(4) 0.0628(10) Uani 1 1 d . . . C31 C 0.7164(3) 0.2719(4) 0.5007(3) 0.0489(8) Uani 1 1 d . . . H1P H 0.064(5) 0.545(4) 0.817(4) 0.096(15) Uiso 1 1 d . . . H2P H 0.199(5) 0.512(5) 0.915(5) 0.109(17) Uiso 1 1 d . . . H4 H 0.551(4) 0.416(3) 0.607(3) 0.039(8) Uiso 1 1 d . . . H5 H 0.406(4) 0.535(3) 0.718(3) 0.053(10) Uiso 1 1 d . . . H6 H 0.273(5) 0.244(4) 1.064(4) 0.074(14) Uiso 1 1 d . . . H7 H 0.337(5) 0.077(5) 1.006(5) 0.093(17) Uiso 1 1 d . . . H8 H 0.573(5) 0.122(4) 0.856(4) 0.074(13) Uiso 1 1 d . . . H9 H 0.670(5) 0.318(4) 0.821(4) 0.071(13) Uiso 1 1 d . . . H10 H 0.485(4) 0.400(4) 0.953(4) 0.061(11) Uiso 1 1 d . . . H11A H 0.060(4) 0.212(3) 0.909(3) 0.050(10) Uiso 1 1 d . . . H11B H 0.157(3) 0.123(3) 0.861(3) 0.040(9) Uiso 1 1 d . . . H12A H -0.074(4) 0.320(4) 0.674(4) 0.067(12) Uiso 1 1 d . . . H12B H 0.051(4) 0.391(3) 0.680(3) 0.052(10) Uiso 1 1 d . . . H12C H -0.087(4) 0.330(4) 0.794(4) 0.060(11) Uiso 1 1 d . . . H13A H -0.123(4) 0.105(3) 0.896(4) 0.052(10) Uiso 1 1 d . . . H13B H -0.115(5) 0.106(4) 0.776(4) 0.077(14) Uiso 1 1 d . . . H13C H -0.010(5) 0.029(4) 0.840(4) 0.073(13) Uiso 1 1 d . . . H15 H 0.527(4) 0.175(3) 0.381(3) 0.050(10) Uiso 1 1 d . . . H16 H 0.464(4) 0.255(4) 0.204(4) 0.071(12) Uiso 1 1 d . . . H17 H 0.289(4) 0.394(4) 0.194(4) 0.063(11) Uiso 1 1 d . . . H18 H 0.189(4) 0.444(4) 0.345(4) 0.063(12) Uiso 1 1 d . . . H19 H 0.240(3) 0.366(3) 0.517(3) 0.038(8) Uiso 1 1 d . . . H21 H 0.238(3) 0.041(3) 0.584(3) 0.042(9) Uiso 1 1 d . . . H22 H 0.122(4) -0.140(4) 0.690(4) 0.071(13) Uiso 1 1 d . . . H23 H 0.130(5) -0.257(4) 0.869(4) 0.069(13) Uiso 1 1 d . . . H24 H 0.276(4) -0.200(4) 0.946(4) 0.067(12) Uiso 1 1 d . . . H25 H 0.400(4) -0.018(3) 0.844(4) 0.061(11) Uiso 1 1 d . . . H27 H 0.616(4) -0.007(3) 0.675(3) 0.054(11) Uiso 1 1 d . . . H28 H 0.839(5) -0.011(4) 0.634(4) 0.085(16) Uiso 1 1 d . . . H29 H 1.013(6) 0.156(5) 0.504(5) 0.116(19) Uiso 1 1 d . . . H30 H 0.916(4) 0.328(3) 0.425(3) 0.053(11) Uiso 1 1 d . . . H31 H 0.682(4) 0.347(4) 0.466(3) 0.059(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0383(2) 0.0345(2) 0.0317(2) -0.01296(17) -0.01261(17) 0.00103(16) P1 0.0614(6) 0.0536(6) 0.0654(6) -0.0361(5) -0.0012(5) 0.0102(5) Si1 0.0342(4) 0.0330(4) 0.0310(4) -0.0140(3) -0.0121(3) 0.0045(3) N1 0.0357(14) 0.0573(17) 0.0512(16) -0.0285(14) -0.0122(12) 0.0022(12) C1 0.0422(16) 0.0340(14) 0.0412(16) -0.0169(13) -0.0099(13) 0.0080(12) C2 0.0329(14) 0.0357(14) 0.0344(14) -0.0150(12) -0.0119(11) 0.0052(11) C3 0.0368(14) 0.0332(14) 0.0286(13) -0.0126(11) -0.0109(11) 0.0032(11) C4 0.0350(15) 0.0351(14) 0.0321(14) -0.0095(12) -0.0065(12) -0.0048(11) C5 0.0518(18) 0.0275(14) 0.0391(16) -0.0111(12) -0.0137(13) 0.0000(13) C6 0.079(3) 0.080(3) 0.0367(18) -0.0228(19) -0.0232(19) 0.010(2) C7 0.078(3) 0.050(2) 0.046(2) -0.0032(17) -0.034(2) -0.0012(19) C8 0.071(3) 0.063(2) 0.062(2) -0.024(2) -0.044(2) 0.028(2) C9 0.055(2) 0.082(3) 0.060(2) -0.012(2) -0.034(2) -0.002(2) C10 0.097(3) 0.061(2) 0.065(2) -0.029(2) -0.050(2) 0.003(2) C11 0.0337(15) 0.0405(16) 0.0414(16) -0.0192(14) -0.0067(12) 0.0015(12) C12 0.044(2) 0.077(3) 0.067(3) -0.031(2) -0.0251(19) 0.016(2) C13 0.042(2) 0.084(3) 0.072(3) -0.047(2) -0.0070(19) -0.012(2) C14 0.0342(14) 0.0333(14) 0.0326(13) -0.0120(11) -0.0107(11) 0.0000(11) C15 0.058(2) 0.0390(16) 0.0389(16) -0.0176(13) -0.0205(15) 0.0101(14) C16 0.078(3) 0.052(2) 0.0387(17) -0.0217(16) -0.0245(17) 0.0071(18) C17 0.067(2) 0.052(2) 0.0426(18) -0.0110(16) -0.0325(17) 0.0026(17) C18 0.0452(19) 0.051(2) 0.052(2) -0.0127(16) -0.0232(16) 0.0098(16) C19 0.0381(16) 0.0493(18) 0.0377(16) -0.0159(14) -0.0107(13) 0.0066(13) C20 0.0425(16) 0.0329(14) 0.0332(14) -0.0153(12) -0.0107(12) 0.0072(12) C21 0.0484(18) 0.0435(17) 0.0410(17) -0.0181(14) -0.0153(14) 0.0010(14) C22 0.061(2) 0.0471(19) 0.060(2) -0.0267(18) -0.0151(18) -0.0073(16) C23 0.074(3) 0.0373(18) 0.053(2) -0.0150(17) -0.0036(19) -0.0088(17) C24 0.079(3) 0.0377(17) 0.0410(18) -0.0109(15) -0.0143(18) 0.0063(17) C25 0.063(2) 0.0397(17) 0.0407(17) -0.0162(14) -0.0221(16) 0.0090(15) C26 0.0397(16) 0.0475(17) 0.0392(15) -0.0237(14) -0.0183(13) 0.0114(13) C27 0.049(2) 0.054(2) 0.056(2) -0.0282(18) -0.0241(16) 0.0176(16) C28 0.065(3) 0.083(3) 0.077(3) -0.047(3) -0.040(2) 0.040(3) C29 0.042(2) 0.110(4) 0.075(3) -0.053(3) -0.027(2) 0.023(2) C30 0.041(2) 0.090(3) 0.060(2) -0.037(2) -0.0113(18) -0.001(2) C31 0.0387(17) 0.060(2) 0.0460(18) -0.0218(16) -0.0111(14) 0.0060(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C9 2.022(4) . ? Fe1 C10 2.024(4) . ? Fe1 C1 2.026(3) . ? Fe1 C2 2.029(3) . ? Fe1 C4 2.030(3) . ? Fe1 C5 2.032(3) . ? Fe1 C7 2.034(4) . ? Fe1 C8 2.034(4) . ? Fe1 C6 2.035(4) . ? Fe1 C3 2.054(3) . ? P1 C1 1.809(3) . ? P1 H1P 1.40(5) . ? P1 H2P 1.33(5) . ? Si1 C3 1.861(3) . ? Si1 C20 1.869(3) . ? Si1 C14 1.873(3) . ? Si1 C26 1.880(3) . ? N1 C12 1.445(5) . ? N1 C13 1.447(5) . ? N1 C11 1.460(4) . ? C1 C5 1.415(4) . ? C1 C2 1.437(4) . ? C2 C3 1.443(4) . ? C2 C11 1.486(4) . ? C3 C4 1.432(4) . ? C4 C5 1.414(4) . ? C4 H4 0.94(3) . ? C5 H5 0.89(4) . ? C6 C10 1.397(6) . ? C6 C7 1.403(6) . ? C6 H6 0.92(5) . ? C7 C8 1.393(6) . ? C7 H7 0.88(5) . ? C8 C9 1.414(6) . ? C8 H8 0.94(4) . ? C9 C10 1.392(7) . ? C9 H9 0.98(4) . ? C10 H10 0.94(4) . ? C11 H11A 0.99(4) . ? C11 H11B 0.96(3) . ? C12 H12A 0.96(4) . ? C12 H12B 1.02(4) . ? C12 H12C 0.94(4) . ? C13 H13A 0.94(4) . ? C13 H13B 0.92(5) . ? C13 H13C 1.03(4) . ? C14 C19 1.386(4) . ? C14 C15 1.389(4) . ? C15 C16 1.382(4) . ? C15 H15 0.97(4) . ? C16 C17 1.374(5) . ? C16 H16 0.97(4) . ? C17 C18 1.370(5) . ? C17 H17 0.90(4) . ? C18 C19 1.385(5) . ? C18 H18 0.84(4) . ? C19 H19 0.92(3) . ? C20 C21 1.394(4) . ? C20 C25 1.396(4) . ? C21 C22 1.377(5) . ? C21 H21 0.90(3) . ? C22 C23 1.368(6) . ? C22 H22 0.86(4) . ? C23 C24 1.373(6) . ? C23 H23 0.86(4) . ? C24 C25 1.371(5) . ? C24 H24 0.88(4) . ? C25 H25 0.94(4) . ? C26 C31 1.385(5) . ? C26 C27 1.393(4) . ? C27 C28 1.388(6) . ? C27 H27 0.94(4) . ? C28 C29 1.355(7) . ? C28 H28 0.79(5) . ? C29 C30 1.360(7) . ? C29 H29 0.96(6) . ? C30 C31 1.382(5) . ? C30 H30 0.87(4) . ? C31 H31 0.94(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Fe1 C10 40.23(19) . . ? C9 Fe1 C1 148.42(17) . . ? C10 Fe1 C1 115.54(16) . . ? C9 Fe1 C2 168.90(17) . . ? C10 Fe1 C2 150.05(17) . . ? C1 Fe1 C2 41.52(11) . . ? C9 Fe1 C4 107.78(16) . . ? C10 Fe1 C4 127.57(16) . . ? C1 Fe1 C4 68.74(12) . . ? C2 Fe1 C4 69.06(12) . . ? C9 Fe1 C5 115.74(16) . . ? C10 Fe1 C5 106.04(16) . . ? C1 Fe1 C5 40.82(13) . . ? C2 Fe1 C5 69.31(12) . . ? C4 Fe1 C5 40.73(12) . . ? C9 Fe1 C7 67.96(18) . . ? C10 Fe1 C7 68.05(18) . . ? C1 Fe1 C7 129.77(16) . . ? C2 Fe1 C7 109.52(15) . . ? C4 Fe1 C7 152.09(16) . . ? C5 Fe1 C7 166.84(16) . . ? C9 Fe1 C8 40.81(18) . . ? C10 Fe1 C8 68.10(18) . . ? C1 Fe1 C8 168.62(16) . . ? C2 Fe1 C8 130.43(15) . . ? C4 Fe1 C8 118.45(16) . . ? C5 Fe1 C8 150.26(17) . . ? C7 Fe1 C8 40.07(17) . . ? C9 Fe1 C6 67.51(19) . . ? C10 Fe1 C6 40.26(18) . . ? C1 Fe1 C6 107.74(16) . . ? C2 Fe1 C6 118.13(16) . . ? C4 Fe1 C6 165.72(16) . . ? C5 Fe1 C6 127.76(16) . . ? C7 Fe1 C6 40.34(17) . . ? C8 Fe1 C6 67.51(19) . . ? C9 Fe1 C3 129.40(17) . . ? C10 Fe1 C3 166.67(17) . . ? C1 Fe1 C3 69.67(12) . . ? C2 Fe1 C3 41.40(11) . . ? C4 Fe1 C3 41.04(11) . . ? C5 Fe1 C3 69.32(12) . . ? C7 Fe1 C3 119.07(14) . . ? C8 Fe1 C3 109.35(15) . . ? C6 Fe1 C3 152.17(16) . . ? C1 P1 H1P 100(2) . . ? C1 P1 H2P 97(2) . . ? H1P P1 H2P 98(3) . . ? C3 Si1 C20 113.31(13) . . ? C3 Si1 C14 106.51(12) . . ? C20 Si1 C14 108.25(13) . . ? C3 Si1 C26 109.76(13) . . ? C20 Si1 C26 110.13(14) . . ? C14 Si1 C26 108.73(13) . . ? C12 N1 C13 111.4(3) . . ? C12 N1 C11 111.1(3) . . ? C13 N1 C11 109.1(3) . . ? C5 C1 C2 108.1(3) . . ? C5 C1 P1 125.5(2) . . ? C2 C1 P1 126.3(2) . . ? C5 C1 Fe1 69.83(18) . . ? C2 C1 Fe1 69.35(16) . . ? P1 C1 Fe1 123.00(17) . . ? C1 C2 C3 108.0(3) . . ? C1 C2 C11 125.6(3) . . ? C3 C2 C11 126.4(3) . . ? C1 C2 Fe1 69.13(17) . . ? C3 C2 Fe1 70.24(15) . . ? C11 C2 Fe1 125.7(2) . . ? C4 C3 C2 106.3(2) . . ? C4 C3 Si1 123.0(2) . . ? C2 C3 Si1 130.2(2) . . ? C4 C3 Fe1 68.59(15) . . ? C2 C3 Fe1 68.36(15) . . ? Si1 C3 Fe1 133.61(15) . . ? C5 C4 C3 109.5(3) . . ? C5 C4 Fe1 69.70(17) . . ? C3 C4 Fe1 70.37(16) . . ? C5 C4 H4 126(2) . . ? C3 C4 H4 124(2) . . ? Fe1 C4 H4 121(2) . . ? C4 C5 C1 108.1(3) . . ? C4 C5 Fe1 69.57(17) . . ? C1 C5 Fe1 69.35(17) . . ? C4 C5 H5 129(2) . . ? C1 C5 H5 123(2) . . ? Fe1 C5 H5 124(2) . . ? C10 C6 C7 108.4(4) . . ? C10 C6 Fe1 69.5(2) . . ? C7 C6 Fe1 69.8(2) . . ? C10 C6 H6 129(3) . . ? C7 C6 H6 123(3) . . ? Fe1 C6 H6 121(3) . . ? C8 C7 C6 107.9(4) . . ? C8 C7 Fe1 70.0(2) . . ? C6 C7 Fe1 69.9(2) . . ? C8 C7 H7 125(3) . . ? C6 C7 H7 127(3) . . ? Fe1 C7 H7 126(3) . . ? C7 C8 C9 107.7(4) . . ? C7 C8 Fe1 69.9(2) . . ? C9 C8 Fe1 69.1(2) . . ? C7 C8 H8 126(3) . . ? C9 C8 H8 126(3) . . ? Fe1 C8 H8 121(3) . . ? C10 C9 C8 108.2(4) . . ? C10 C9 Fe1 70.0(2) . . ? C8 C9 Fe1 70.0(2) . . ? C10 C9 H9 131(3) . . ? C8 C9 H9 121(3) . . ? Fe1 C9 H9 121(2) . . ? C9 C10 C6 107.9(4) . . ? C9 C10 Fe1 69.8(2) . . ? C6 C10 Fe1 70.3(2) . . ? C9 C10 H10 123(3) . . ? C6 C10 H10 129(3) . . ? Fe1 C10 H10 123(2) . . ? N1 C11 C2 112.8(3) . . ? N1 C11 H11A 110(2) . . ? C2 C11 H11A 109(2) . . ? N1 C11 H11B 106(2) . . ? C2 C11 H11B 109(2) . . ? H11A C11 H11B 110(3) . . ? N1 C12 H12A 106(2) . . ? N1 C12 H12B 109(2) . . ? H12A C12 H12B 110(3) . . ? N1 C12 H12C 110(2) . . ? H12A C12 H12C 111(3) . . ? H12B C12 H12C 110(3) . . ? N1 C13 H13A 111(2) . . ? N1 C13 H13B 111(3) . . ? H13A C13 H13B 110(4) . . ? N1 C13 H13C 108(2) . . ? H13A C13 H13C 109(3) . . ? H13B C13 H13C 108(4) . . ? C19 C14 C15 117.4(3) . . ? C19 C14 Si1 121.0(2) . . ? C15 C14 Si1 121.6(2) . . ? C16 C15 C14 121.2(3) . . ? C16 C15 H15 121(2) . . ? C14 C15 H15 118(2) . . ? C17 C16 C15 120.0(3) . . ? C17 C16 H16 120(2) . . ? C15 C16 H16 120(3) . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17 117(3) . . ? C16 C17 H17 123(3) . . ? C17 C18 C19 119.7(3) . . ? C17 C18 H18 121(3) . . ? C19 C18 H18 119(3) . . ? C18 C19 C14 121.6(3) . . ? C18 C19 H19 119(2) . . ? C14 C19 H19 119(2) . . ? C21 C20 C25 116.9(3) . . ? C21 C20 Si1 120.3(2) . . ? C25 C20 Si1 122.8(2) . . ? C22 C21 C20 121.5(3) . . ? C22 C21 H21 118(2) . . ? C20 C21 H21 120(2) . . ? C23 C22 C21 120.1(4) . . ? C23 C22 H22 120(3) . . ? C21 C22 H22 120(3) . . ? C22 C23 C24 119.7(4) . . ? C22 C23 H23 116(3) . . ? C24 C23 H23 124(3) . . ? C25 C24 C23 120.5(4) . . ? C25 C24 H24 118(3) . . ? C23 C24 H24 122(3) . . ? C24 C25 C20 121.3(3) . . ? C24 C25 H25 120(2) . . ? C20 C25 H25 118(2) . . ? C31 C26 C27 116.9(3) . . ? C31 C26 Si1 120.9(2) . . ? C27 C26 Si1 122.3(3) . . ? C28 C27 C26 120.3(4) . . ? C28 C27 H27 121(2) . . ? C26 C27 H27 118(2) . . ? C29 C28 C27 121.3(4) . . ? C29 C28 H28 129(4) . . ? C27 C28 H28 110(4) . . ? C28 C29 C30 119.5(4) . . ? C28 C29 H29 125(3) . . ? C30 C29 H29 116(3) . . ? C29 C30 C31 120.0(4) . . ? C29 C30 H30 121(3) . . ? C31 C30 H30 119(3) . . ? C30 C31 C26 122.0(4) . . ? C30 C31 H31 119(2) . . ? C26 C31 H31 119(2) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 28.52 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.558 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.064 #------------------------------------------------------------------------------# # NEW STRUCTURE # #------------------------------------------------------------------------------# data_s039_fin _database_code_depnum_ccdc_archive 'CCDC 628375' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H31 Fe N Si' _chemical_formula_weight 501.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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' _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 10.4014(9) _cell_length_b 10.6429(11) _cell_length_c 13.2272(12) _cell_angle_alpha 74.919(11) _cell_angle_beta 75.272(10) _cell_angle_gamma 69.639(11) _cell_volume 1303.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 30.25 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 0.644 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8047 _exptl_absorpt_correction_T_max 0.8778 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe IPDS area detector' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17134 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 30.30 _reflns_number_total 7088 _reflns_number_gt 4503 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0360P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7088 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 0.804 _refine_ls_restrained_S_all 0.804 _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 Fe01 Fe 0.744225(19) 0.15780(2) 0.108706(18) 0.02797(7) Uani 1 1 d . . . Si1 Si 0.67209(4) 0.29798(4) 0.34123(3) 0.02543(9) Uani 1 1 d . . . N1 N 1.04342(12) 0.31989(13) 0.18635(11) 0.0341(3) Uani 1 1 d . . . C1 C 0.78355(13) 0.18023(14) 0.24756(11) 0.0262(3) Uani 1 1 d . . . C2 C 0.89588(13) 0.19833(15) 0.15879(12) 0.0278(3) Uani 1 1 d . . . C3 C 0.95273(13) 0.07716(16) 0.11565(13) 0.0316(3) Uani 1 1 d . . . H3 H 1.0262 0.0625 0.0573 0.038 Uiso 1 1 calc R . . C4 C 0.88104(14) -0.01815(15) 0.17455(13) 0.0332(3) Uani 1 1 d . . . H4 H 0.8985 -0.1063 0.1624 0.040 Uiso 1 1 calc R . . C5 C 0.77789(14) 0.04403(15) 0.25544(12) 0.0305(3) Uani 1 1 d . . . H5 H 0.7157 0.0030 0.3062 0.037 Uiso 1 1 calc R . . C6 C 0.54785(15) 0.28574(17) 0.08889(14) 0.0390(4) Uani 1 1 d . . . H6 H 0.4839 0.3392 0.1372 0.047 Uiso 1 1 calc R . . C7 C 0.64989(16) 0.32679(18) 0.00533(14) 0.0426(4) Uani 1 1 d . . . H7 H 0.6659 0.4122 -0.0115 0.051 Uiso 1 1 calc R . . C8 C 0.72342(17) 0.2160(2) -0.04819(14) 0.0498(5) Uani 1 1 d . . . H8 H 0.7967 0.2152 -0.1070 0.060 Uiso 1 1 calc R . . C9 C 0.66758(17) 0.10665(19) 0.00199(16) 0.0493(5) Uani 1 1 d . . . H9 H 0.6972 0.0208 -0.0176 0.059 Uiso 1 1 calc R . . C10 C 0.55953(15) 0.14924(18) 0.08662(16) 0.0440(4) Uani 1 1 d . . . H10 H 0.5048 0.0966 0.1334 0.053 Uiso 1 1 calc R . . C11 C 0.48263(14) 0.30273(16) 0.37163(12) 0.0308(3) Uani 1 1 d . . . C12 C 0.44148(16) 0.18453(18) 0.40321(15) 0.0431(4) Uani 1 1 d . . . H12 H 0.5098 0.0988 0.4069 0.052 Uiso 1 1 calc R . . C13 C 0.30059(18) 0.1913(2) 0.42939(17) 0.0529(5) Uani 1 1 d . . . H13 H 0.2749 0.1106 0.4501 0.063 Uiso 1 1 calc R . . C14 C 0.19885(17) 0.3171(2) 0.42472(16) 0.0534(5) Uani 1 1 d . . . H14 H 0.1040 0.3221 0.4416 0.064 Uiso 1 1 calc R . . C15 C 0.23708(16) 0.4341(2) 0.39541(16) 0.0491(5) Uani 1 1 d . . . H15 H 0.1682 0.5195 0.3932 0.059 Uiso 1 1 calc R . . C16 C 0.37782(15) 0.42742(17) 0.36875(14) 0.0397(4) Uani 1 1 d . . . H16 H 0.4023 0.5087 0.3485 0.048 Uiso 1 1 calc R . . C17 C 0.74083(14) 0.23268(14) 0.46969(12) 0.0272(3) Uani 1 1 d . . . C18 C 0.65259(16) 0.22760(17) 0.56880(13) 0.0407(4) Uani 1 1 d . . . H18 H 0.5556 0.2551 0.5720 0.049 Uiso 1 1 calc R . . C19 C 0.70551(18) 0.1827(2) 0.66272(14) 0.0504(5) Uani 1 1 d . . . H19 H 0.6443 0.1799 0.7286 0.060 Uiso 1 1 calc R . . C20 C 0.84692(17) 0.14238(18) 0.65982(14) 0.0437(4) Uani 1 1 d . . . H20 H 0.8824 0.1131 0.7235 0.052 Uiso 1 1 calc R . . C21 C 0.93601(16) 0.14523(19) 0.56325(15) 0.0462(4) Uani 1 1 d . . . H21 H 1.0328 0.1166 0.5608 0.055 Uiso 1 1 calc R . . C22 C 0.88364(16) 0.19009(18) 0.46941(14) 0.0411(4) Uani 1 1 d . . . H22 H 0.9459 0.1918 0.4040 0.049 Uiso 1 1 calc R . . C23 C 0.67792(13) 0.47826(14) 0.28622(12) 0.0283(3) Uani 1 1 d . . . C24 C 0.62310(15) 0.55541(15) 0.19465(13) 0.0345(3) Uani 1 1 d . . . H24 H 0.5836 0.5156 0.1596 0.041 Uiso 1 1 calc R . . C25 C 0.62578(16) 0.68869(16) 0.15459(14) 0.0410(4) Uani 1 1 d . . . H25 H 0.5898 0.7376 0.0925 0.049 Uiso 1 1 calc R . . C26 C 0.68155(17) 0.74945(17) 0.20621(16) 0.0463(4) Uani 1 1 d . . . H26 H 0.6830 0.8400 0.1796 0.056 Uiso 1 1 calc R . . C27 C 0.73515(18) 0.67652(17) 0.29699(16) 0.0468(4) Uani 1 1 d . . . H27 H 0.7726 0.7179 0.3323 0.056 Uiso 1 1 calc R . . C28 C 0.73403(15) 0.54242(16) 0.33632(13) 0.0356(3) Uani 1 1 d . . . H28 H 0.7717 0.4939 0.3978 0.043 Uiso 1 1 calc R . . C29 C 0.95168(14) 0.31858(15) 0.11902(12) 0.0307(3) Uani 1 1 d . . . H29A H 1.0036 0.3157 0.0462 0.037 Uiso 1 1 calc R . . H29B H 0.8735 0.4031 0.1172 0.037 Uiso 1 1 calc R . . C30 C 1.17082(17) 0.20530(19) 0.18006(17) 0.0509(5) Uani 1 1 d . . . H30A H 1.2194 0.2096 0.1068 0.076 Uiso 1 1 calc R . . H30B H 1.1475 0.1204 0.2051 0.076 Uiso 1 1 calc R . . H30C H 1.2303 0.2097 0.2241 0.076 Uiso 1 1 calc R . . C31 C 1.0787(2) 0.44761(19) 0.15300(17) 0.0525(5) Uani 1 1 d . . . H31A H 1.1375 0.4492 0.1988 0.079 Uiso 1 1 calc R . . H31B H 0.9940 0.5238 0.1582 0.079 Uiso 1 1 calc R . . H31C H 1.1282 0.4547 0.0799 0.079 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 Fe01 0.02332(10) 0.03410(12) 0.02781(13) -0.00848(9) -0.00990(7) -0.00462(8) Si1 0.02731(18) 0.0268(2) 0.0235(2) -0.00330(16) -0.00670(14) -0.00935(15) N1 0.0360(6) 0.0390(7) 0.0317(8) -0.0006(6) -0.0094(5) -0.0189(5) C1 0.0262(6) 0.0291(7) 0.0248(8) -0.0032(6) -0.0100(5) -0.0079(5) C2 0.0242(6) 0.0345(8) 0.0257(8) -0.0039(6) -0.0092(5) -0.0082(5) C3 0.0219(6) 0.0392(8) 0.0322(8) -0.0099(6) -0.0087(5) -0.0025(5) C4 0.0321(7) 0.0287(7) 0.0411(10) -0.0098(7) -0.0165(6) -0.0026(6) C5 0.0343(7) 0.0295(7) 0.0301(9) -0.0021(6) -0.0110(6) -0.0116(6) C6 0.0287(7) 0.0446(9) 0.0411(10) -0.0118(8) -0.0170(6) 0.0023(6) C7 0.0436(9) 0.0446(10) 0.0384(10) 0.0028(8) -0.0219(7) -0.0094(7) C8 0.0406(9) 0.0746(13) 0.0284(10) -0.0130(9) -0.0153(7) -0.0016(8) C9 0.0438(9) 0.0529(11) 0.0596(13) -0.0267(9) -0.0316(8) 0.0027(8) C10 0.0301(7) 0.0485(10) 0.0598(12) -0.0109(9) -0.0227(7) -0.0088(7) C11 0.0312(7) 0.0403(8) 0.0237(8) -0.0069(6) -0.0055(5) -0.0131(6) C12 0.0379(8) 0.0419(9) 0.0482(11) -0.0059(8) -0.0023(7) -0.0161(7) C13 0.0458(9) 0.0615(12) 0.0597(13) -0.0107(10) -0.0009(8) -0.0330(9) C14 0.0334(8) 0.0773(14) 0.0556(13) -0.0125(10) -0.0075(8) -0.0245(9) C15 0.0314(8) 0.0590(11) 0.0536(12) -0.0131(9) -0.0092(7) -0.0066(7) C16 0.0342(8) 0.0430(9) 0.0446(10) -0.0114(8) -0.0085(7) -0.0118(7) C17 0.0324(7) 0.0250(7) 0.0255(8) -0.0046(6) -0.0075(5) -0.0087(5) C18 0.0346(7) 0.0487(10) 0.0311(9) -0.0076(8) -0.0065(6) -0.0027(7) C19 0.0492(9) 0.0657(12) 0.0250(9) -0.0055(8) -0.0049(7) -0.0071(8) C20 0.0542(10) 0.0446(10) 0.0324(10) -0.0004(8) -0.0217(7) -0.0101(7) C21 0.0363(8) 0.0601(11) 0.0427(11) -0.0020(9) -0.0167(7) -0.0139(7) C22 0.0352(8) 0.0581(11) 0.0289(9) -0.0027(8) -0.0065(6) -0.0163(7) C23 0.0289(6) 0.0283(7) 0.0281(8) -0.0058(6) -0.0046(5) -0.0090(5) C24 0.0377(7) 0.0336(8) 0.0342(9) -0.0053(7) -0.0115(6) -0.0105(6) C25 0.0400(8) 0.0363(9) 0.0409(10) 0.0042(7) -0.0132(7) -0.0085(7) C26 0.0459(9) 0.0309(9) 0.0608(13) 0.0024(8) -0.0129(8) -0.0158(7) C27 0.0530(10) 0.0373(9) 0.0606(13) -0.0093(8) -0.0186(8) -0.0203(7) C28 0.0405(8) 0.0346(8) 0.0350(9) -0.0039(7) -0.0123(6) -0.0133(6) C29 0.0277(7) 0.0363(8) 0.0261(8) -0.0007(6) -0.0059(5) -0.0104(6) C30 0.0361(8) 0.0580(11) 0.0629(13) -0.0064(9) -0.0234(8) -0.0129(8) C31 0.0617(11) 0.0543(11) 0.0531(12) 0.0019(9) -0.0166(9) -0.0358(9) _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 Fe01 C5 2.0453(15) . ? Fe01 C9 2.0490(18) . ? Fe01 C8 2.0502(17) . ? Fe01 C10 2.0506(15) . ? Fe01 C3 2.0527(13) . ? Fe01 C4 2.0536(14) . ? Fe01 C7 2.0595(16) . ? Fe01 C6 2.0606(14) . ? Fe01 C2 2.0656(14) . ? Fe01 C1 2.0677(15) . ? Si1 C1 1.8751(15) . ? Si1 C17 1.8812(15) . ? Si1 C23 1.8832(15) . ? Si1 C11 1.8936(14) . ? N1 C30 1.457(2) . ? N1 C31 1.460(2) . ? N1 C29 1.4668(19) . ? C1 C5 1.447(2) . ? C1 C2 1.4568(19) . ? C2 C3 1.421(2) . ? C2 C29 1.504(2) . ? C3 C4 1.418(2) . ? C4 C5 1.423(2) . ? C6 C7 1.419(2) . ? C6 C10 1.423(2) . ? C7 C8 1.417(3) . ? C8 C9 1.416(3) . ? C9 C10 1.411(3) . ? C11 C16 1.393(2) . ? C11 C12 1.397(2) . ? C12 C13 1.398(2) . ? C13 C14 1.386(3) . ? C14 C15 1.368(3) . ? C15 C16 1.397(2) . ? C17 C22 1.393(2) . ? C17 C18 1.396(2) . ? C18 C19 1.389(2) . ? C19 C20 1.375(2) . ? C20 C21 1.374(3) . ? C21 C22 1.386(2) . ? C23 C28 1.398(2) . ? C23 C24 1.405(2) . ? C24 C25 1.387(2) . ? C25 C26 1.383(3) . ? C26 C27 1.382(3) . ? C27 C28 1.389(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Fe01 C9 125.60(7) . . ? C5 Fe01 C8 163.08(7) . . ? C9 Fe01 C8 40.41(8) . . ? C5 Fe01 C10 107.47(7) . . ? C9 Fe01 C10 40.27(8) . . ? C8 Fe01 C10 67.77(8) . . ? C5 Fe01 C3 67.97(6) . . ? C9 Fe01 C3 119.31(7) . . ? C8 Fe01 C3 108.43(7) . . ? C10 Fe01 C3 153.07(7) . . ? C5 Fe01 C4 40.62(6) . . ? C9 Fe01 C4 106.82(7) . . ? C8 Fe01 C4 126.00(7) . . ? C10 Fe01 C4 118.67(7) . . ? C3 Fe01 C4 40.41(6) . . ? C5 Fe01 C7 154.74(7) . . ? C9 Fe01 C7 67.97(8) . . ? C8 Fe01 C7 40.34(7) . . ? C10 Fe01 C7 67.94(7) . . ? C3 Fe01 C7 127.53(7) . . ? C4 Fe01 C7 163.89(7) . . ? C5 Fe01 C6 120.00(6) . . ? C9 Fe01 C6 67.89(7) . . ? C8 Fe01 C6 67.73(7) . . ? C10 Fe01 C6 40.50(7) . . ? C3 Fe01 C6 165.03(7) . . ? C4 Fe01 C6 153.61(6) . . ? C7 Fe01 C6 40.29(7) . . ? C5 Fe01 C2 68.47(6) . . ? C9 Fe01 C2 153.83(7) . . ? C8 Fe01 C2 120.30(7) . . ? C10 Fe01 C2 164.96(7) . . ? C3 Fe01 C2 40.36(6) . . ? C4 Fe01 C2 68.37(6) . . ? C7 Fe01 C2 109.14(6) . . ? C6 Fe01 C2 127.84(6) . . ? C5 Fe01 C1 41.18(6) . . ? C9 Fe01 C1 163.34(7) . . ? C8 Fe01 C1 154.67(7) . . ? C10 Fe01 C1 126.22(7) . . ? C3 Fe01 C1 68.92(6) . . ? C4 Fe01 C1 69.31(6) . . ? C7 Fe01 C1 120.08(7) . . ? C6 Fe01 C1 107.96(6) . . ? C2 Fe01 C1 41.28(5) . . ? C1 Si1 C17 107.35(6) . . ? C1 Si1 C23 111.60(6) . . ? C17 Si1 C23 109.62(7) . . ? C1 Si1 C11 112.78(7) . . ? C17 Si1 C11 107.99(6) . . ? C23 Si1 C11 107.42(6) . . ? C30 N1 C31 109.49(13) . . ? C30 N1 C29 111.18(13) . . ? C31 N1 C29 109.63(12) . . ? C5 C1 C2 105.61(13) . . ? C5 C1 Si1 124.66(11) . . ? C2 C1 Si1 129.64(11) . . ? C5 C1 Fe01 68.58(9) . . ? C2 C1 Fe01 69.28(8) . . ? Si1 C1 Fe01 129.11(7) . . ? C3 C2 C1 108.22(13) . . ? C3 C2 C29 123.54(13) . . ? C1 C2 C29 128.18(14) . . ? C3 C2 Fe01 69.33(8) . . ? C1 C2 Fe01 69.44(7) . . ? C29 C2 Fe01 129.04(10) . . ? C4 C3 C2 109.20(13) . . ? C4 C3 Fe01 69.83(8) . . ? C2 C3 Fe01 70.31(7) . . ? C3 C4 C5 107.47(13) . . ? C3 C4 Fe01 69.76(8) . . ? C5 C4 Fe01 69.38(8) . . ? C4 C5 C1 109.50(13) . . ? C4 C5 Fe01 70.00(9) . . ? C1 C5 Fe01 70.24(8) . . ? C7 C6 C10 107.83(16) . . ? C7 C6 Fe01 69.81(8) . . ? C10 C6 Fe01 69.38(8) . . ? C8 C7 C6 107.73(16) . . ? C8 C7 Fe01 69.48(9) . . ? C6 C7 Fe01 69.89(9) . . ? C9 C8 C7 108.34(16) . . ? C9 C8 Fe01 69.75(10) . . ? C7 C8 Fe01 70.18(10) . . ? C10 C9 C8 107.96(16) . . ? C10 C9 Fe01 69.93(10) . . ? C8 C9 Fe01 69.84(10) . . ? C9 C10 C6 108.14(16) . . ? C9 C10 Fe01 69.80(9) . . ? C6 C10 Fe01 70.13(9) . . ? C16 C11 C12 117.37(13) . . ? C16 C11 Si1 119.96(12) . . ? C12 C11 Si1 122.57(11) . . ? C11 C12 C13 121.27(16) . . ? C14 C13 C12 119.89(17) . . ? C15 C14 C13 119.72(15) . . ? C14 C15 C16 120.41(16) . . ? C11 C16 C15 121.33(16) . . ? C22 C17 C18 117.08(14) . . ? C22 C17 Si1 120.75(11) . . ? C18 C17 Si1 122.16(11) . . ? C19 C18 C17 121.19(14) . . ? C20 C19 C18 120.36(16) . . ? C21 C20 C19 119.55(16) . . ? C20 C21 C22 120.25(15) . . ? C21 C22 C17 121.57(15) . . ? C28 C23 C24 117.03(13) . . ? C28 C23 Si1 121.38(11) . . ? C24 C23 Si1 121.57(11) . . ? C25 C24 C23 121.75(15) . . ? C26 C25 C24 119.82(15) . . ? C27 C26 C25 119.74(15) . . ? C26 C27 C28 120.40(16) . . ? C27 C28 C23 121.25(15) . . ? N1 C29 C2 112.08(11) . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 30.30 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.335 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.044 #------------------------------------------------------------------------------# # NEW STRUCTURE # #------------------------------------------------------------------------------# #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2006-11-14 at 12:23:49 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\xray\wingx\files\archive.dat # CIF files read : x0062fin x0062 data_x0062fin _database_code_depnum_ccdc_archive 'CCDC 628376' _audit_creation_date 2006-11-14T12:23:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C37 H44 Cl2 Fe N P Si' _chemical_formula_weight 688.54 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 10.29870(10) _cell_length_b 21.9790(2) _cell_length_c 14.68120(10) _cell_angle_alpha 90 _cell_angle_beta 95.2190(10) _cell_angle_gamma 90 _cell_volume 3309.39(5) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 32151 _cell_measurement_theta_min 2.6828 _cell_measurement_theta_max 32.2282 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.73 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.83904 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 -0.0036132007 _diffrn_orient_matrix_ub_12 0.0317572015 _diffrn_orient_matrix_ub_13 -0.0076322812 _diffrn_orient_matrix_ub_21 0.028396904 _diffrn_orient_matrix_ub_22 -0.003807979 _diffrn_orient_matrix_ub_23 -0.041842872 _diffrn_orient_matrix_ub_31 -0.0629361235 _diffrn_orient_matrix_ub_32 -0.0035572133 _diffrn_orient_matrix_ub_33 -0.0233075638 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_unetI/netI 0.0279 _diffrn_reflns_number 49152 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 9966 _reflns_number_gt 8304 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0471P)^2^+2.1585P] 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_number_reflns 9966 _refine_ls_number_parameters 355 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1042 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.54 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.13073(2) 0.102868(10) 0.925701(14) 0.01772(6) Uani 1 1 d . A . Cl1 Cl 0.18594(5) -0.05318(2) 0.82009(3) 0.03573(11) Uani 1 1 d . . . Cl2 Cl 0.48721(5) -0.03561(2) 0.84733(3) 0.03384(10) Uani 1 1 d . . . P1 P 0.32639(4) 0.01901(2) 0.80882(3) 0.02365(9) Uani 1 1 d . . . Si1 Si 0.28864(4) 0.21916(2) 1.05960(3) 0.01901(9) Uani 1 1 d . . . N1 N 0.48410(13) 0.10640(6) 0.81694(9) 0.0222(3) Uani 1 1 d . . . C1 C 0.29925(15) 0.05628(7) 0.91422(10) 0.0190(3) Uani 1 1 d . A . C2 C 0.32514(14) 0.12036(7) 0.92349(10) 0.0178(3) Uani 1 1 d . . . C3 C 0.28203(14) 0.14143(7) 1.00856(10) 0.0180(3) Uani 1 1 d . A . C4 C 0.23020(15) 0.08847(7) 1.05077(10) 0.0208(3) Uani 1 1 d . . . H4 H 0.1947 0.0882 1.1083 0.025 Uiso 1 1 calc R A . C5 C 0.24007(15) 0.03704(7) 0.99386(11) 0.0207(3) Uani 1 1 d . A . H5 H 0.2124 -0.0031 1.0063 0.025 Uiso 1 1 calc R . . C6 C 0.01581(17) 0.09142(9) 0.80550(12) 0.0300(4) Uani 1 1 d . . . H6 H 0.0403 0.0726 0.7514 0.036 Uiso 1 1 calc R A . C7 C 0.02846(17) 0.15413(9) 0.82697(12) 0.0292(4) Uani 1 1 d . A . H7 H 0.0639 0.1845 0.7904 0.035 Uiso 1 1 calc R . . C8 C -0.02148(16) 0.16332(9) 0.91318(12) 0.0281(3) Uani 1 1 d . . . H8 H -0.026 0.2011 0.944 0.034 Uiso 1 1 calc R A . C9 C -0.06345(16) 0.10621(9) 0.94524(12) 0.0282(4) Uani 1 1 d . A . H9 H -0.1007 0.0991 1.0011 0.034 Uiso 1 1 calc R . . C10 C -0.03960(16) 0.06143(9) 0.87835(13) 0.0301(4) Uani 1 1 d . A . H10 H -0.0576 0.0192 0.8819 0.036 Uiso 1 1 calc R . . C11 C 0.39518(15) 0.15177(7) 0.85141(11) 0.0208(3) Uani 1 1 d . A . H11A H 0.3322 0.1663 0.8012 0.025 Uiso 1 1 calc R . . H11B H 0.445 0.1871 0.8778 0.025 Uiso 1 1 calc R . . C12 C 0.60079(17) 0.09967(9) 0.88139(13) 0.0298(4) Uani 1 1 d . . . H12A H 0.6597 0.0698 0.8575 0.045 Uiso 1 1 calc R . . H12B H 0.5753 0.0857 0.9406 0.045 Uiso 1 1 calc R . . H12C H 0.6454 0.139 0.8891 0.045 Uiso 1 1 calc R . . C13 C 0.5203(2) 0.12256(10) 0.72588(13) 0.0349(4) Uani 1 1 d . . . H13A H 0.4415 0.1255 0.6833 0.052 Uiso 1 1 calc R . . H13B H 0.578 0.0912 0.7046 0.052 Uiso 1 1 calc R . . H13C H 0.5656 0.1618 0.7288 0.052 Uiso 1 1 calc R . . C14 C 0.46476(16) 0.24222(8) 1.07832(10) 0.0228(3) Uani 1 1 d . A . C15 C 0.56349(18) 0.19853(9) 1.08462(13) 0.0296(4) Uani 1 1 d . . . H15 H 0.541 0.1566 1.0807 0.036 Uiso 1 1 calc R A . C16 C 0.69383(19) 0.21509(11) 1.09651(14) 0.0377(4) Uani 1 1 d . A . H16 H 0.7598 0.1848 1.1 0.045 Uiso 1 1 calc R . . C17 C 0.7274(2) 0.27612(12) 1.10325(14) 0.0423(5) Uani 1 1 d . . . H17 H 0.8166 0.2877 1.1115 0.051 Uiso 1 1 calc R A . C18 C 0.6317(2) 0.31970(10) 1.09795(14) 0.0416(5) Uani 1 1 d . A . H18 H 0.655 0.3615 1.103 0.05 Uiso 1 1 calc R . . C19 C 0.5015(2) 0.30339(9) 1.08535(13) 0.0330(4) Uani 1 1 d . . . H19 H 0.4363 0.3341 1.0814 0.04 Uiso 1 1 calc R A . C26 C 0.21269(16) 0.21407(7) 1.17073(10) 0.0205(3) Uani 1 1 d . A . C27 C 0.08370(17) 0.19400(9) 1.17354(12) 0.0288(4) Uani 1 1 d . . . H27 H 0.034 0.1837 1.118 0.035 Uiso 1 1 calc R A . C28 C 0.02714(18) 0.18890(9) 1.25538(13) 0.0315(4) Uani 1 1 d . A . H28 H -0.0603 0.1752 1.2557 0.038 Uiso 1 1 calc R . . C29 C 0.09862(19) 0.20393(9) 1.33662(12) 0.0292(4) Uani 1 1 d . . . H29 H 0.0604 0.2004 1.3929 0.035 Uiso 1 1 calc R A . C30 C 0.2252(2) 0.22394(10) 1.33595(12) 0.0344(4) Uani 1 1 d . A . H30 H 0.274 0.2346 1.3917 0.041 Uiso 1 1 calc R . . C31 C 0.28187(18) 0.22862(9) 1.25363(12) 0.0288(4) Uani 1 1 d . . . H31 H 0.3696 0.242 1.2541 0.035 Uiso 1 1 calc R A . C20 C 0.1951(2) 0.27720(11) 0.98520(18) 0.0209(4) Uani 0.853(3) 1 d PD A 1 C21 C 0.2258(6) 0.2903(2) 0.8969(3) 0.0318(4) Uani 0.853(3) 1 d PD A 1 H21 H 0.2963 0.2693 0.8736 0.038 Uiso 0.853(3) 1 calc PR A 1 C22 C 0.1578(4) 0.3327(2) 0.8418(3) 0.0376(8) Uani 0.853(3) 1 d PD A 1 H22 H 0.1834 0.3414 0.7827 0.045 Uiso 0.853(3) 1 calc PR A 1 C23 C 0.0536(3) 0.36201(13) 0.87267(18) 0.0445(7) Uani 0.853(3) 1 d PD A 1 H23 H 0.0067 0.3912 0.8351 0.053 Uiso 0.853(3) 1 calc PR A 1 C24 C 0.0165(3) 0.34917(14) 0.9584(2) 0.0501(7) Uani 0.853(3) 1 d PD A 1 H24 H -0.0579 0.3686 0.9792 0.06 Uiso 0.853(3) 1 calc PR A 1 C25 C 0.0879(3) 0.30778(12) 1.01468(16) 0.0379(5) Uani 0.853(3) 1 d PD A 1 H25 H 0.063 0.3002 1.0744 0.046 Uiso 0.853(3) 1 calc PR A 1 C20F C 0.2295(15) 0.2847(7) 0.9893(12) 0.0209(4) Uani 0.147(3) 1 d PD A 2 C21F C 0.228(3) 0.2868(13) 0.8943(15) 0.0318(4) Uani 0.147(3) 1 d PD A 2 H21F H 0.2619 0.2537 0.8624 0.038 Uiso 0.147(3) 1 calc PR A 2 C22F C 0.177(3) 0.3368(12) 0.8463(18) 0.0376(8) Uani 0.147(3) 1 d PD A 2 H22F H 0.1751 0.3369 0.7814 0.045 Uiso 0.147(3) 1 calc PR A 2 C23F C 0.1313(16) 0.3857(8) 0.8893(9) 0.0445(7) Uani 0.147(3) 1 d PD A 2 H23F H 0.1041 0.421 0.8555 0.053 Uiso 0.147(3) 1 calc PR A 2 C24F C 0.1242(15) 0.3837(7) 0.9827(9) 0.0501(7) Uani 0.147(3) 1 d PD A 2 H24F H 0.0807 0.4149 1.0127 0.06 Uiso 0.147(3) 1 calc PR A 2 C25F C 0.1822(13) 0.3348(6) 1.0325(8) 0.0379(5) Uani 0.147(3) 1 d PD A 2 H25F H 0.1891 0.3362 1.0974 0.046 Uiso 0.147(3) 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 0.01433(10) 0.02270(11) 0.01618(10) -0.00114(8) 0.00166(7) -0.00109(8) Cl1 0.0369(2) 0.0296(2) 0.0417(2) -0.01307(18) 0.00900(19) -0.00790(18) Cl2 0.0311(2) 0.0269(2) 0.0442(3) -0.00028(17) 0.00696(18) 0.00903(17) P1 0.0249(2) 0.0259(2) 0.02055(18) -0.00280(15) 0.00424(15) 0.00301(16) Si1 0.0208(2) 0.0212(2) 0.01515(18) -0.00042(14) 0.00229(15) -0.00117(15) N1 0.0192(6) 0.0274(7) 0.0207(6) 0.0047(5) 0.0067(5) 0.0043(5) C1 0.0192(7) 0.0200(7) 0.0179(6) 0.0002(5) 0.0026(5) 0.0008(5) C2 0.0149(6) 0.0212(7) 0.0175(6) 0.0012(5) 0.0017(5) 0.0003(5) C3 0.0160(6) 0.0222(7) 0.0156(6) 0.0001(5) 0.0003(5) -0.0006(5) C4 0.0214(7) 0.0246(7) 0.0166(6) 0.0028(5) 0.0026(5) 0.0003(6) C5 0.0206(7) 0.0211(7) 0.0206(7) 0.0031(5) 0.0036(6) -0.0008(6) C6 0.0201(8) 0.0448(10) 0.0243(8) -0.0075(7) -0.0027(6) 0.0000(7) C7 0.0225(8) 0.0390(10) 0.0249(8) 0.0037(7) -0.0048(6) 0.0020(7) C8 0.0172(7) 0.0347(9) 0.0314(8) -0.0046(7) -0.0027(6) 0.0058(6) C9 0.0146(7) 0.0419(10) 0.0283(8) -0.0053(7) 0.0031(6) -0.0009(7) C10 0.0175(7) 0.0382(10) 0.0345(9) -0.0091(7) 0.0022(6) -0.0060(7) C11 0.0197(7) 0.0218(7) 0.0217(7) 0.0035(5) 0.0058(6) 0.0010(6) C12 0.0178(7) 0.0344(9) 0.0370(9) 0.0028(7) 0.0016(7) 0.0024(7) C13 0.0413(11) 0.0391(10) 0.0269(9) 0.0074(7) 0.0179(8) 0.0081(8) C14 0.0264(8) 0.0264(8) 0.0161(6) -0.0009(5) 0.0045(6) -0.0078(6) C15 0.0249(8) 0.0341(9) 0.0293(8) 0.0005(7) -0.0009(7) -0.0079(7) C16 0.0247(9) 0.0519(12) 0.0363(10) -0.0052(9) 0.0013(7) -0.0066(8) C17 0.0324(10) 0.0631(14) 0.0325(10) -0.0142(9) 0.0089(8) -0.0252(10) C18 0.0509(13) 0.0415(11) 0.0339(10) -0.0132(8) 0.0122(9) -0.0262(10) C19 0.0420(10) 0.0300(9) 0.0281(8) -0.0081(7) 0.0095(8) -0.0115(8) C26 0.0224(7) 0.0222(7) 0.0172(6) -0.0015(5) 0.0029(5) 0.0002(6) C27 0.0221(8) 0.0430(10) 0.0213(7) -0.0088(7) 0.0026(6) -0.0010(7) C28 0.0236(8) 0.0434(10) 0.0289(8) -0.0074(7) 0.0100(7) -0.0022(7) C29 0.0343(9) 0.0341(9) 0.0205(7) 0.0002(6) 0.0094(7) 0.0014(7) C30 0.0349(10) 0.0529(12) 0.0153(7) -0.0025(7) 0.0012(7) -0.0087(9) C31 0.0271(8) 0.0383(10) 0.0210(7) -0.0018(7) 0.0020(6) -0.0095(7) C20 0.0208(12) 0.0226(9) 0.0191(7) 0.0000(7) 0.0015(9) -0.0014(8) C21 0.0359(10) 0.0343(11) 0.0272(9) 0.0085(7) 0.0140(8) 0.0084(8) C22 0.044(2) 0.0426(13) 0.0268(10) 0.0124(9) 0.0089(12) 0.0078(13) C23 0.0475(15) 0.0500(16) 0.0362(12) 0.0165(11) 0.0043(11) 0.0183(12) C24 0.0498(15) 0.0560(17) 0.0468(15) 0.0156(12) 0.0165(12) 0.0275(13) C25 0.0468(14) 0.0418(13) 0.0270(10) 0.0067(9) 0.0132(10) 0.0164(10) C20F 0.0208(12) 0.0226(9) 0.0191(7) 0.0000(7) 0.0015(9) -0.0014(8) C21F 0.0359(10) 0.0343(11) 0.0272(9) 0.0085(7) 0.0140(8) 0.0084(8) C22F 0.044(2) 0.0426(13) 0.0268(10) 0.0124(9) 0.0089(12) 0.0078(13) C23F 0.0475(15) 0.0500(16) 0.0362(12) 0.0165(11) 0.0043(11) 0.0183(12) C24F 0.0498(15) 0.0560(17) 0.0468(15) 0.0156(12) 0.0165(12) 0.0275(13) C25F 0.0468(14) 0.0418(13) 0.0270(10) 0.0067(9) 0.0132(10) 0.0164(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.0352(15) . ? Fe1 C5 2.0390(16) . ? Fe1 C10 2.0416(17) . ? Fe1 C2 2.0418(15) . ? Fe1 C4 2.0442(16) . ? Fe1 C9 2.0473(16) . ? Fe1 C6 2.0489(17) . ? Fe1 C7 2.0499(18) . ? Fe1 C8 2.0503(17) . ? Fe1 C3 2.0691(15) . ? Cl1 P1 2.1635(6) . ? Cl2 P1 2.0817(6) . ? P1 C1 1.7952(15) . ? Si1 C20F 1.842(18) . ? Si1 C3 1.8644(16) . ? Si1 C26 1.8757(15) . ? Si1 C14 1.8793(17) . ? Si1 C20 1.886(3) . ? N1 C13 1.464(2) . ? N1 C12 1.468(2) . ? N1 C11 1.474(2) . ? C1 C5 1.431(2) . ? C1 C2 1.438(2) . ? C2 C3 1.440(2) . ? C2 C11 1.502(2) . ? C3 C4 1.444(2) . ? C4 C5 1.415(2) . ? C6 C7 1.417(3) . ? C6 C10 1.419(3) . ? C7 C8 1.423(3) . ? C8 C9 1.421(3) . ? C9 C10 1.427(3) . ? C14 C15 1.395(3) . ? C14 C19 1.398(2) . ? C15 C16 1.386(3) . ? C16 C17 1.387(3) . ? C17 C18 1.371(4) . ? C18 C19 1.385(3) . ? C26 C31 1.390(2) . ? C26 C27 1.404(2) . ? C27 C28 1.387(2) . ? C28 C29 1.383(3) . ? C29 C30 1.377(3) . ? C30 C31 1.393(2) . ? C20 C21 1.393(4) . ? C20 C25 1.395(3) . ? C21 C22 1.382(4) . ? C22 C23 1.363(4) . ? C23 C24 1.378(4) . ? C24 C25 1.393(3) . ? C20F C25F 1.382(15) . ? C20F C21F 1.394(16) . ? C21F C22F 1.382(16) . ? C22F C23F 1.354(17) . ? C23F C24F 1.380(15) . ? C24F C25F 1.402(14) . ? 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 C5 41.12(6) . . ? C1 Fe1 C10 117.40(7) . . ? C5 Fe1 C10 105.64(7) . . ? C1 Fe1 C2 41.29(6) . . ? C5 Fe1 C2 69.08(6) . . ? C10 Fe1 C2 153.12(7) . . ? C1 Fe1 C4 68.60(6) . . ? C5 Fe1 C4 40.55(6) . . ? C10 Fe1 C4 125.57(7) . . ? C2 Fe1 C4 68.38(6) . . ? C1 Fe1 C9 151.75(7) . . ? C5 Fe1 C9 117.36(7) . . ? C10 Fe1 C9 40.86(7) . . ? C2 Fe1 C9 165.28(7) . . ? C4 Fe1 C9 107.20(7) . . ? C1 Fe1 C6 107.28(7) . . ? C5 Fe1 C6 125.84(7) . . ? C10 Fe1 C6 40.61(8) . . ? C2 Fe1 C6 119.99(7) . . ? C4 Fe1 C6 163.25(8) . . ? C9 Fe1 C6 68.28(7) . . ? C1 Fe1 C7 127.24(7) . . ? C5 Fe1 C7 164.22(7) . . ? C10 Fe1 C7 68.53(8) . . ? C2 Fe1 C7 109.07(7) . . ? C4 Fe1 C7 154.62(7) . . ? C9 Fe1 C7 68.51(8) . . ? C6 Fe1 C7 40.46(8) . . ? C1 Fe1 C8 165.78(7) . . ? C5 Fe1 C8 152.55(7) . . ? C10 Fe1 C8 68.42(8) . . ? C2 Fe1 C8 128.27(7) . . ? C4 Fe1 C8 119.83(7) . . ? C9 Fe1 C8 40.60(8) . . ? C6 Fe1 C8 68.00(7) . . ? C7 Fe1 C8 40.62(7) . . ? C1 Fe1 C3 69.67(6) . . ? C5 Fe1 C3 69.48(6) . . ? C10 Fe1 C3 163.88(7) . . ? C2 Fe1 C3 40.99(6) . . ? C4 Fe1 C3 41.09(6) . . ? C9 Fe1 C3 126.58(7) . . ? C6 Fe1 C3 154.39(7) . . ? C7 Fe1 C3 120.11(7) . . ? C8 Fe1 C3 108.42(7) . . ? C1 P1 Cl2 102.21(6) . . ? C1 P1 Cl1 96.39(5) . . ? Cl2 P1 Cl1 94.43(3) . . ? C20F Si1 C3 119.5(5) . . ? C20F Si1 C26 113.0(5) . . ? C3 Si1 C26 106.98(7) . . ? C20F Si1 C14 97.8(5) . . ? C3 Si1 C14 107.78(7) . . ? C26 Si1 C14 111.24(7) . . ? C20F Si1 C20 11.9(5) . . ? C3 Si1 C20 112.89(9) . . ? C26 Si1 C20 108.22(9) . . ? C14 Si1 C20 109.73(8) . . ? C13 N1 C12 110.58(14) . . ? C13 N1 C11 111.53(13) . . ? C12 N1 C11 110.16(14) . . ? C5 C1 C2 107.54(13) . . ? C5 C1 P1 132.91(12) . . ? C2 C1 P1 119.12(11) . . ? C5 C1 Fe1 69.59(9) . . ? C2 C1 Fe1 69.60(8) . . ? P1 C1 Fe1 120.12(8) . . ? C1 C2 C3 109.15(13) . . ? C1 C2 C11 118.71(13) . . ? C3 C2 C11 132.02(14) . . ? C1 C2 Fe1 69.11(8) . . ? C3 C2 Fe1 70.52(8) . . ? C11 C2 Fe1 129.22(11) . . ? C2 C3 C4 105.57(13) . . ? C2 C3 Si1 129.84(11) . . ? C4 C3 Si1 124.59(11) . . ? C2 C3 Fe1 68.49(8) . . ? C4 C3 Fe1 68.53(9) . . ? Si1 C3 Fe1 127.56(8) . . ? C5 C4 C3 109.96(13) . . ? C5 C4 Fe1 69.53(9) . . ? C3 C4 Fe1 70.38(8) . . ? C4 C5 C1 107.77(13) . . ? C4 C5 Fe1 69.93(9) . . ? C1 C5 Fe1 69.30(9) . . ? C7 C6 C10 108.61(16) . . ? C7 C6 Fe1 69.81(10) . . ? C10 C6 Fe1 69.42(10) . . ? C6 C7 C8 107.60(17) . . ? C6 C7 Fe1 69.74(10) . . ? C8 C7 Fe1 69.71(10) . . ? C9 C8 C7 108.33(16) . . ? C9 C8 Fe1 69.59(10) . . ? C7 C8 Fe1 69.67(10) . . ? C8 C9 C10 107.73(16) . . ? C8 C9 Fe1 69.82(9) . . ? C10 C9 Fe1 69.36(9) . . ? C6 C10 C9 107.72(17) . . ? C6 C10 Fe1 69.98(10) . . ? C9 C10 Fe1 69.78(10) . . ? N1 C11 C2 106.51(12) . . ? C15 C14 C19 117.79(17) . . ? C15 C14 Si1 120.79(13) . . ? C19 C14 Si1 121.41(14) . . ? C16 C15 C14 121.27(18) . . ? C15 C16 C17 119.7(2) . . ? C18 C17 C16 119.90(19) . . ? C17 C18 C19 120.61(19) . . ? C18 C19 C14 120.7(2) . . ? C31 C26 C27 117.22(14) . . ? C31 C26 Si1 121.78(12) . . ? C27 C26 Si1 120.99(12) . . ? C28 C27 C26 121.61(16) . . ? C29 C28 C27 119.68(17) . . ? C30 C29 C28 120.00(16) . . ? C29 C30 C31 120.10(17) . . ? C26 C31 C30 121.38(16) . . ? C21 C20 C25 116.3(3) . . ? C21 C20 Si1 122.1(2) . . ? C25 C20 Si1 121.55(18) . . ? C22 C21 C20 122.5(4) . . ? C23 C22 C21 119.8(4) . . ? C22 C23 C24 119.9(3) . . ? C23 C24 C25 120.0(2) . . ? C24 C25 C20 121.4(2) . . ? C25F C20F C21F 117.3(15) . . ? C25F C20F Si1 118.6(12) . . ? C21F C20F Si1 124.1(14) . . ? C22F C21F C20F 120(2) . . ? C23F C22F C21F 122(2) . . ? C22F C23F C24F 119.4(15) . . ? C23F C24F C25F 119.0(12) . . ? C20F C25F C24F 121.5(12) . . ? #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------#