# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Chunming Cui Cui' _publ_contact_author_email CMCUI@NANKAI.EDU.CN _publ_section_title ; Azaphosphaallyl Anion Lithium [ArNC(But)PAr]-Li+(THF)4 and Its Monomeric Potassium and Thallium Complexes (Ar = 2,6-iPr2C6H3) ; loop_ _publ_author_name 'Chunming Cui Cui.' 'Xiaofei Li.' 'Hai-Bin Song.' # Attachment 'shelxltl.cif' data_shelxltl _database_code_depnum_ccdc_archive 'CCDC 736327' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H43 N P Tl' _chemical_formula_sum 'C29 H43 N P Tl' _chemical_formula_weight 640.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 14.442(3) _cell_length_b 10.787(2) _cell_length_c 18.310(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.105(4) _cell_angle_gamma 90.00 _cell_volume 2778.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7738 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour red-black _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 5.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4928 _exptl_absorpt_correction_T_max 0.5905 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34036 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.91 _reflns_number_total 6625 _reflns_number_gt 5739 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0274P)^2^+2.2748P] 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 6625 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _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 Tl1 Tl 0.137046(10) 0.046538(14) 1.042512(8) 0.02315(6) Uani 1 1 d . . . P1 P 0.11253(6) 0.04618(8) 0.88453(5) 0.01285(17) Uani 1 1 d . . . N1 N 0.29065(18) 0.1365(2) 0.90151(14) 0.0123(6) Uani 1 1 d . . . C1 C 0.2092(2) 0.1263(3) 0.85532(18) 0.0124(6) Uani 1 1 d . . . C2 C 0.2045(2) 0.1727(3) 0.77507(18) 0.0158(7) Uani 1 1 d . . . C3 C 0.1491(3) 0.2953(3) 0.7643(2) 0.0219(8) Uani 1 1 d . . . H3A H 0.1516 0.3314 0.7157 0.033 Uiso 1 1 calc R . . H3B H 0.1775 0.3530 0.8045 0.033 Uiso 1 1 calc R . . H3C H 0.0827 0.2796 0.7659 0.033 Uiso 1 1 calc R . . C4 C 0.1543(3) 0.0803(3) 0.71610(19) 0.0206(8) Uani 1 1 d . . . H4A H 0.0878 0.0716 0.7194 0.031 Uiso 1 1 calc R . . H4B H 0.1860 -0.0004 0.7250 0.031 Uiso 1 1 calc R . . H4C H 0.1568 0.1102 0.6661 0.031 Uiso 1 1 calc R . . C5 C 0.3044(3) 0.1971(4) 0.7634(2) 0.0255(8) Uani 1 1 d . . . H5A H 0.3000 0.2300 0.7129 0.038 Uiso 1 1 calc R . . H5B H 0.3405 0.1194 0.7693 0.038 Uiso 1 1 calc R . . H5C H 0.3367 0.2574 0.8006 0.038 Uiso 1 1 calc R . . C6 C 0.3065(2) 0.1107(3) 0.97842(18) 0.0135(7) Uani 1 1 d . . . C7 C 0.3073(2) 0.2115(3) 1.02818(19) 0.0159(7) Uani 1 1 d . . . C8 C 0.3369(2) 0.1908(3) 1.10557(19) 0.0196(8) Uani 1 1 d . . . H8 H 0.3389 0.2582 1.1393 0.023 Uiso 1 1 calc R . . C9 C 0.3631(3) 0.0742(3) 1.1334(2) 0.0219(8) Uani 1 1 d . . . H9 H 0.3838 0.0617 1.1859 0.026 Uiso 1 1 calc R . . C10 C 0.3592(3) -0.0245(3) 1.0848(2) 0.0196(8) Uani 1 1 d . . . H10 H 0.3762 -0.1048 1.1047 0.024 Uiso 1 1 calc R . . C11 C 0.3309(2) -0.0094(3) 1.00747(19) 0.0145(7) Uani 1 1 d . . . C12 C 0.2840(2) 0.3412(3) 0.9969(2) 0.0196(8) Uani 1 1 d . . . H12 H 0.2376 0.3323 0.9476 0.024 Uiso 1 1 calc R . . C13 C 0.3729(3) 0.4034(4) 0.9818(2) 0.0301(9) Uani 1 1 d . . . H13A H 0.4206 0.4120 1.0290 0.045 Uiso 1 1 calc R . . H13B H 0.3564 0.4856 0.9599 0.045 Uiso 1 1 calc R . . H13C H 0.3988 0.3525 0.9468 0.045 Uiso 1 1 calc R . . C14 C 0.2376(3) 0.4237(4) 1.0464(2) 0.0291(9) Uani 1 1 d . . . H14A H 0.1843 0.3793 1.0593 0.044 Uiso 1 1 calc R . . H14B H 0.2142 0.4998 1.0192 0.044 Uiso 1 1 calc R . . H14C H 0.2845 0.4448 1.0923 0.044 Uiso 1 1 calc R . . C15 C 0.3324(2) -0.1189(3) 0.95561(19) 0.0162(7) Uani 1 1 d . . . H15 H 0.3032 -0.0917 0.9032 0.019 Uiso 1 1 calc R . . C16 C 0.4346(3) -0.1573(4) 0.9586(2) 0.0322(10) Uani 1 1 d . . . H16A H 0.4697 -0.0865 0.9448 0.048 Uiso 1 1 calc R . . H16B H 0.4351 -0.2255 0.9233 0.048 Uiso 1 1 calc R . . H16C H 0.4647 -0.1844 1.0095 0.048 Uiso 1 1 calc R . . C17 C 0.2747(3) -0.2285(3) 0.9742(2) 0.0280(9) Uani 1 1 d . . . H17A H 0.3017 -0.2564 1.0256 0.042 Uiso 1 1 calc R . . H17B H 0.2769 -0.2965 0.9392 0.042 Uiso 1 1 calc R . . H17C H 0.2086 -0.2029 0.9698 0.042 Uiso 1 1 calc R . . C18 C -0.0076(2) 0.0906(3) 0.83031(18) 0.0123(6) Uani 1 1 d . . . C19 C -0.0620(2) -0.0021(3) 0.78382(18) 0.0148(7) Uani 1 1 d . . . C20 C -0.1593(3) 0.0156(3) 0.75717(19) 0.0192(8) Uani 1 1 d . . . H20 H -0.1959 -0.0466 0.7270 0.023 Uiso 1 1 calc R . . C21 C -0.2036(2) 0.1221(4) 0.7739(2) 0.0215(8) Uani 1 1 d . . . H21 H -0.2702 0.1321 0.7560 0.026 Uiso 1 1 calc R . . C22 C -0.1511(2) 0.2131(3) 0.8163(2) 0.0217(8) Uani 1 1 d . . . H22 H -0.1819 0.2869 0.8264 0.026 Uiso 1 1 calc R . . C23 C -0.0537(2) 0.2002(3) 0.84517(18) 0.0153(7) Uani 1 1 d . . . C24 C -0.0172(2) -0.1215(3) 0.76329(18) 0.0160(7) Uani 1 1 d . . . H24 H 0.0530 -0.1078 0.7729 0.019 Uiso 1 1 calc R . . C25 C -0.0520(3) -0.1543(4) 0.6804(2) 0.0279(9) Uani 1 1 d . . . H25A H -0.1200 -0.1738 0.6700 0.042 Uiso 1 1 calc R . . H25B H -0.0168 -0.2264 0.6686 0.042 Uiso 1 1 calc R . . H25C H -0.0415 -0.0837 0.6496 0.042 Uiso 1 1 calc R . . C26 C -0.0342(3) -0.2289(3) 0.8130(2) 0.0273(9) Uani 1 1 d . . . H26A H -0.0016 -0.2120 0.8651 0.041 Uiso 1 1 calc R . . H26B H -0.0093 -0.3056 0.7962 0.041 Uiso 1 1 calc R . . H26C H -0.1026 -0.2378 0.8097 0.041 Uiso 1 1 calc R . . C27 C -0.0019(3) 0.3030(3) 0.89508(19) 0.0178(7) Uani 1 1 d . . . H27 H 0.0678 0.2855 0.9048 0.021 Uiso 1 1 calc R . . C28 C -0.0191(3) 0.4323(3) 0.8603(2) 0.0260(9) Uani 1 1 d . . . H28A H -0.0048 0.4317 0.8105 0.039 Uiso 1 1 calc R . . H28B H 0.0222 0.4923 0.8923 0.039 Uiso 1 1 calc R . . H28C H -0.0858 0.4557 0.8558 0.039 Uiso 1 1 calc R . . C29 C -0.0306(3) 0.3029(4) 0.9707(2) 0.0255(8) Uani 1 1 d . . . H29A H -0.0981 0.3240 0.9630 0.038 Uiso 1 1 calc R . . H29B H 0.0075 0.3642 1.0041 0.038 Uiso 1 1 calc R . . H29C H -0.0196 0.2204 0.9935 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl1 0.02082(9) 0.03235(9) 0.01805(8) 0.00124(6) 0.00814(6) 0.00002(6) P1 0.0111(4) 0.0163(4) 0.0108(4) 0.0027(3) 0.0018(3) -0.0013(3) N1 0.0126(14) 0.0136(14) 0.0112(13) 0.0009(11) 0.0040(11) -0.0012(11) C1 0.0159(16) 0.0078(15) 0.0144(16) -0.0025(12) 0.0054(13) 0.0023(13) C2 0.0190(18) 0.0162(17) 0.0126(16) 0.0018(13) 0.0043(13) -0.0017(14) C3 0.029(2) 0.0201(19) 0.0182(18) 0.0055(14) 0.0077(15) 0.0031(16) C4 0.027(2) 0.0218(19) 0.0131(17) -0.0008(14) 0.0057(15) -0.0042(16) C5 0.026(2) 0.034(2) 0.0180(19) 0.0040(16) 0.0085(16) -0.0042(17) C6 0.0074(15) 0.0189(18) 0.0146(17) -0.0012(13) 0.0032(13) -0.0025(13) C7 0.0126(16) 0.0190(18) 0.0159(17) -0.0009(13) 0.0025(13) -0.0008(14) C8 0.0222(19) 0.0202(19) 0.0158(18) -0.0052(14) 0.0030(15) -0.0018(15) C9 0.0223(19) 0.033(2) 0.0080(16) 0.0010(14) -0.0009(14) 0.0004(16) C10 0.0201(19) 0.021(2) 0.0162(18) 0.0041(14) 0.0018(14) 0.0039(15) C11 0.0092(16) 0.0188(17) 0.0160(17) 0.0008(13) 0.0038(13) -0.0015(14) C12 0.0201(18) 0.0189(19) 0.0189(18) -0.0022(14) 0.0023(14) 0.0029(15) C13 0.035(2) 0.020(2) 0.038(2) 0.0044(17) 0.0144(19) 0.0017(17) C14 0.032(2) 0.025(2) 0.031(2) -0.0062(17) 0.0077(18) 0.0059(17) C15 0.0162(17) 0.0172(18) 0.0147(17) -0.0009(13) 0.0022(13) 0.0012(14) C16 0.022(2) 0.036(2) 0.038(2) -0.0146(19) 0.0048(18) 0.0037(18) C17 0.038(2) 0.019(2) 0.029(2) -0.0005(16) 0.0120(18) -0.0004(17) C18 0.0120(16) 0.0160(16) 0.0094(15) 0.0025(12) 0.0033(12) 0.0002(13) C19 0.0157(17) 0.0183(17) 0.0106(16) 0.0028(13) 0.0038(13) -0.0007(14) C20 0.0176(18) 0.028(2) 0.0112(17) 0.0004(14) 0.0010(14) -0.0041(15) C21 0.0106(17) 0.033(2) 0.0190(18) 0.0043(16) -0.0004(14) 0.0048(16) C22 0.0216(19) 0.0226(19) 0.0217(19) 0.0050(15) 0.0066(15) 0.0117(15) C23 0.0176(17) 0.0180(17) 0.0119(16) 0.0022(13) 0.0069(13) 0.0002(14) C24 0.0158(17) 0.0165(17) 0.0149(17) -0.0015(13) 0.0016(13) -0.0027(14) C25 0.028(2) 0.031(2) 0.022(2) -0.0123(17) 0.0013(16) 0.0001(18) C26 0.034(2) 0.0185(19) 0.031(2) -0.0015(16) 0.0099(18) -0.0027(17) C27 0.0227(19) 0.0154(17) 0.0158(17) 0.0008(13) 0.0055(14) 0.0009(14) C28 0.037(2) 0.020(2) 0.023(2) -0.0002(15) 0.0104(18) 0.0028(17) C29 0.031(2) 0.027(2) 0.0197(19) -0.0015(15) 0.0084(16) 0.0055(17) _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 Tl1 P1 2.8335(11) . ? P1 C1 1.822(3) . ? P1 C18 1.855(3) . ? N1 C1 1.288(4) . ? N1 C6 1.402(4) . ? C1 C2 1.539(4) . ? C2 C4 1.527(5) . ? C2 C5 1.528(5) . ? C2 C3 1.535(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.414(5) . ? C6 C7 1.417(5) . ? C7 C8 1.402(5) . ? C7 C12 1.520(5) . ? C8 C9 1.378(5) . ? C8 H8 0.9500 . ? C9 C10 1.380(5) . ? C9 H9 0.9500 . ? C10 C11 1.392(5) . ? C10 H10 0.9500 . ? C11 C15 1.519(5) . ? C12 C13 1.528(5) . ? C12 C14 1.529(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.522(5) . ? C15 C17 1.528(5) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.413(5) . ? C18 C19 1.428(5) . ? C19 C20 1.393(5) . ? C19 C24 1.526(5) . ? C20 C21 1.383(5) . ? C20 H20 0.9500 . ? C21 C22 1.369(5) . ? C21 H21 0.9500 . ? C22 C23 1.393(5) . ? C22 H22 0.9500 . ? C23 C27 1.521(5) . ? C24 C26 1.527(5) . ? C24 C25 1.528(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.531(5) . ? C27 C29 1.533(5) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C18 113.95(15) . . ? C1 P1 Tl1 111.86(11) . . ? C18 P1 Tl1 115.54(11) . . ? C1 N1 C6 124.0(3) . . ? N1 C1 C2 115.8(3) . . ? N1 C1 P1 119.6(2) . . ? C2 C1 P1 124.3(2) . . ? C4 C2 C5 109.0(3) . . ? C4 C2 C3 108.8(3) . . ? C5 C2 C3 108.4(3) . . ? C4 C2 C1 112.0(3) . . ? C5 C2 C1 110.5(3) . . ? C3 C2 C1 108.1(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C11 122.0(3) . . ? N1 C6 C7 117.9(3) . . ? C11 C6 C7 119.7(3) . . ? C8 C7 C6 118.9(3) . . ? C8 C7 C12 121.2(3) . . ? C6 C7 C12 119.7(3) . . ? C9 C8 C7 121.0(3) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 119.9(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 121.7(3) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 118.7(3) . . ? C10 C11 C15 120.2(3) . . ? C6 C11 C15 121.0(3) . . ? C7 C12 C13 110.4(3) . . ? C7 C12 C14 113.7(3) . . ? C13 C12 C14 110.6(3) . . ? C7 C12 H12 107.3 . . ? C13 C12 H12 107.3 . . ? C14 C12 H12 107.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 109.8(3) . . ? C11 C15 C17 112.2(3) . . ? C16 C15 C17 110.8(3) . . ? C11 C15 H15 108.0 . . ? C16 C15 H15 108.0 . . ? C17 C15 H15 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 118.8(3) . . ? C23 C18 P1 122.5(2) . . ? C19 C18 P1 117.3(2) . . ? C20 C19 C18 119.2(3) . . ? C20 C19 C24 118.7(3) . . ? C18 C19 C24 122.1(3) . . ? C21 C20 C19 121.1(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 121.7(3) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 119.3(3) . . ? C22 C23 C27 118.2(3) . . ? C18 C23 C27 122.4(3) . . ? C19 C24 C26 111.1(3) . . ? C19 C24 C25 112.2(3) . . ? C26 C24 C25 110.8(3) . . ? C19 C24 H24 107.5 . . ? C26 C24 H24 107.5 . . ? C25 C24 H24 107.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 113.8(3) . . ? C23 C27 C29 110.2(3) . . ? C28 C27 C29 109.0(3) . . ? C23 C27 H27 107.9 . . ? C28 C27 H27 107.9 . . ? C29 C27 H27 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C1 C2 173.5(3) . . . . ? C6 N1 C1 P1 -12.5(4) . . . . ? C18 P1 C1 N1 157.1(2) . . . . ? Tl1 P1 C1 N1 23.7(3) . . . . ? C18 P1 C1 C2 -29.5(3) . . . . ? Tl1 P1 C1 C2 -162.8(2) . . . . ? N1 C1 C2 C4 133.5(3) . . . . ? P1 C1 C2 C4 -40.2(4) . . . . ? N1 C1 C2 C5 11.7(4) . . . . ? P1 C1 C2 C5 -161.9(3) . . . . ? N1 C1 C2 C3 -106.7(3) . . . . ? P1 C1 C2 C3 79.6(3) . . . . ? C1 N1 C6 C11 88.8(4) . . . . ? C1 N1 C6 C7 -97.8(4) . . . . ? N1 C6 C7 C8 -170.6(3) . . . . ? C11 C6 C7 C8 3.1(5) . . . . ? N1 C6 C7 C12 4.5(4) . . . . ? C11 C6 C7 C12 178.1(3) . . . . ? C6 C7 C8 C9 -1.3(5) . . . . ? C12 C7 C8 C9 -176.3(3) . . . . ? C7 C8 C9 C10 -0.8(6) . . . . ? C8 C9 C10 C11 1.2(6) . . . . ? C9 C10 C11 C6 0.5(5) . . . . ? C9 C10 C11 C15 176.9(3) . . . . ? N1 C6 C11 C10 170.7(3) . . . . ? C7 C6 C11 C10 -2.7(5) . . . . ? N1 C6 C11 C15 -5.6(5) . . . . ? C7 C6 C11 C15 -179.0(3) . . . . ? C8 C7 C12 C13 89.7(4) . . . . ? C6 C7 C12 C13 -85.2(4) . . . . ? C8 C7 C12 C14 -35.2(5) . . . . ? C6 C7 C12 C14 149.9(3) . . . . ? C10 C11 C15 C16 -68.6(4) . . . . ? C6 C11 C15 C16 107.7(4) . . . . ? C10 C11 C15 C17 55.0(4) . . . . ? C6 C11 C15 C17 -128.7(3) . . . . ? C1 P1 C18 C23 -80.1(3) . . . . ? Tl1 P1 C18 C23 51.5(3) . . . . ? C1 P1 C18 C19 113.6(3) . . . . ? Tl1 P1 C18 C19 -114.8(2) . . . . ? C23 C18 C19 C20 -2.7(5) . . . . ? P1 C18 C19 C20 164.1(3) . . . . ? C23 C18 C19 C24 178.3(3) . . . . ? P1 C18 C19 C24 -14.9(4) . . . . ? C18 C19 C20 C21 1.1(5) . . . . ? C24 C19 C20 C21 -179.9(3) . . . . ? C19 C20 C21 C22 1.1(5) . . . . ? C20 C21 C22 C23 -1.7(5) . . . . ? C21 C22 C23 C18 0.1(5) . . . . ? C21 C22 C23 C27 -176.9(3) . . . . ? C19 C18 C23 C22 2.1(5) . . . . ? P1 C18 C23 C22 -163.9(3) . . . . ? C19 C18 C23 C27 178.9(3) . . . . ? P1 C18 C23 C27 12.9(4) . . . . ? C20 C19 C24 C26 -79.8(4) . . . . ? C18 C19 C24 C26 99.2(4) . . . . ? C20 C19 C24 C25 44.8(4) . . . . ? C18 C19 C24 C25 -136.2(3) . . . . ? C22 C23 C27 C28 -52.3(4) . . . . ? C18 C23 C27 C28 130.9(3) . . . . ? C22 C23 C27 C29 70.4(4) . . . . ? C18 C23 C27 C29 -106.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.015 _refine_diff_density_min -1.219 _refine_diff_density_rms 0.125 # Attachment 'shelxlli.cif' data_shelxlli _database_code_depnum_ccdc_archive 'CCDC 736328' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H76 Li N O4 P' _chemical_formula_sum 'C45 H75 Li N O4 P' _chemical_formula_weight 731.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 14.626(7) _cell_length_b 18.619(8) _cell_length_c 16.409(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.021(6) _cell_angle_gamma 90.00 _cell_volume 4468(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 9438 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9762 _exptl_absorpt_correction_T_max 0.9782 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 38506 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7880 _reflns_number_gt 6834 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0576P)^2^+2.8376P] 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 7880 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.1798 _refine_ls_wR_factor_gt 0.1721 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_restrained_S_all 1.220 _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 P1 P 0.33547(5) 0.23795(4) 0.35979(4) 0.02738(19) Uani 1 1 d . . . Li1 Li 0.9598(3) 0.3215(3) 0.3297(3) 0.0374(12) Uani 1 1 d . . . N1 N 0.44776(14) 0.20978(12) 0.23564(13) 0.0255(5) Uani 1 1 d . . . O1 O 0.92757(14) 0.22252(11) 0.31983(12) 0.0374(5) Uani 1 1 d . . . O2 O 0.85573(14) 0.38405(11) 0.31079(13) 0.0432(5) Uani 1 1 d . . . O3 O 1.05272(14) 0.33676(13) 0.25083(13) 0.0456(6) Uani 1 1 d . . . O4 O 1.00585(15) 0.33708(11) 0.43918(12) 0.0408(5) Uani 1 1 d . . . C1 C 0.36386(18) 0.29227(15) 0.52134(17) 0.0291(6) Uani 1 1 d . . . C2 C 0.34411(19) 0.29374(16) 0.60457(17) 0.0321(7) Uani 1 1 d . . . H2 H 0.3591 0.3353 0.6356 0.039 Uiso 1 1 calc R . . C3 C 0.30325(19) 0.23599(16) 0.64250(16) 0.0333(7) Uani 1 1 d . . . H3 H 0.2902 0.2380 0.6990 0.040 Uiso 1 1 calc R . . C4 C 0.28164(18) 0.17537(16) 0.59754(16) 0.0309(6) Uani 1 1 d . . . H4 H 0.2544 0.1355 0.6239 0.037 Uiso 1 1 calc R . . C5 C 0.29897(18) 0.17156(15) 0.51415(16) 0.0278(6) Uani 1 1 d . . . C6 C 0.34013(17) 0.23132(15) 0.47382(16) 0.0262(6) Uani 1 1 d . . . C7 C 0.4060(2) 0.35873(15) 0.48351(18) 0.0332(7) Uani 1 1 d . . . H7 H 0.4290 0.3450 0.4286 0.040 Uiso 1 1 calc R . . C8 C 0.4876(2) 0.38890(18) 0.5336(2) 0.0459(8) Uani 1 1 d . . . H8A H 0.4659 0.4074 0.5857 0.069 Uiso 1 1 calc R . . H8B H 0.5164 0.4278 0.5031 0.069 Uiso 1 1 calc R . . H8C H 0.5323 0.3506 0.5437 0.069 Uiso 1 1 calc R . . C9 C 0.3331(2) 0.41720(17) 0.4709(2) 0.0440(8) Uani 1 1 d . . . H9A H 0.2850 0.3994 0.4337 0.066 Uiso 1 1 calc R . . H9B H 0.3613 0.4600 0.4475 0.066 Uiso 1 1 calc R . . H9C H 0.3063 0.4294 0.5234 0.066 Uiso 1 1 calc R . . C10 C 0.27106(19) 0.10366(15) 0.46806(17) 0.0314(7) Uani 1 1 d . . . H10 H 0.3055 0.1031 0.4159 0.038 Uiso 1 1 calc R . . C11 C 0.2946(2) 0.03408(17) 0.5139(2) 0.0428(8) Uani 1 1 d . . . H11A H 0.3599 0.0338 0.5286 0.064 Uiso 1 1 calc R . . H11B H 0.2805 -0.0073 0.4790 0.064 Uiso 1 1 calc R . . H11C H 0.2585 0.0313 0.5636 0.064 Uiso 1 1 calc R . . C12 C 0.1689(2) 0.10530(19) 0.4457(2) 0.0432(8) Uani 1 1 d . . . H12A H 0.1331 0.1060 0.4956 0.065 Uiso 1 1 calc R . . H12B H 0.1529 0.0625 0.4137 0.065 Uiso 1 1 calc R . . H12C H 0.1553 0.1484 0.4135 0.065 Uiso 1 1 calc R . . C13 C 0.43886(18) 0.20549(14) 0.31525(16) 0.0243(6) Uani 1 1 d . . . C14 C 0.52453(18) 0.17357(15) 0.35926(16) 0.0283(6) Uani 1 1 d . . . C15 C 0.5919(2) 0.1435(2) 0.2981(2) 0.0553(10) Uani 1 1 d . . . H15A H 0.6130 0.1823 0.2627 0.083 Uiso 1 1 calc R . . H15B H 0.5617 0.1065 0.2649 0.083 Uiso 1 1 calc R . . H15C H 0.6444 0.1225 0.3274 0.083 Uiso 1 1 calc R . . C16 C 0.5712(2) 0.23305(19) 0.4088(2) 0.0572(10) Uani 1 1 d . . . H16A H 0.5305 0.2490 0.4521 0.086 Uiso 1 1 calc R . . H16B H 0.5848 0.2736 0.3730 0.086 Uiso 1 1 calc R . . H16C H 0.6282 0.2147 0.4332 0.086 Uiso 1 1 calc R . . C17 C 0.4996(2) 0.1125(2) 0.4166(2) 0.0524(9) Uani 1 1 d . . . H17A H 0.5556 0.0914 0.4400 0.079 Uiso 1 1 calc R . . H17B H 0.4655 0.0757 0.3862 0.079 Uiso 1 1 calc R . . H17C H 0.4618 0.1312 0.4605 0.079 Uiso 1 1 calc R . . C18 C 0.38206(17) 0.24438(15) 0.18538(15) 0.0248(6) Uani 1 1 d . . . C19 C 0.31380(18) 0.20397(15) 0.14296(16) 0.0290(6) Uani 1 1 d . . . C20 C 0.25917(19) 0.23881(16) 0.08451(17) 0.0324(7) Uani 1 1 d . . . H20 H 0.2132 0.2123 0.0562 0.039 Uiso 1 1 calc R . . C21 C 0.2702(2) 0.31075(17) 0.06681(17) 0.0361(7) Uani 1 1 d . . . H21 H 0.2331 0.3330 0.0260 0.043 Uiso 1 1 calc R . . C22 C 0.3357(2) 0.35026(16) 0.10898(17) 0.0332(7) Uani 1 1 d . . . H22 H 0.3432 0.3998 0.0968 0.040 Uiso 1 1 calc R . . C23 C 0.39108(18) 0.31866(15) 0.16914(16) 0.0274(6) Uani 1 1 d . . . C24 C 0.3008(2) 0.12493(16) 0.16041(19) 0.0369(7) Uani 1 1 d . . . H24 H 0.3528 0.1088 0.1964 0.044 Uiso 1 1 calc R . . C25 C 0.2117(2) 0.11113(19) 0.2057(2) 0.0473(8) Uani 1 1 d . . . H25A H 0.2116 0.1394 0.2561 0.071 Uiso 1 1 calc R . . H25B H 0.2071 0.0600 0.2190 0.071 Uiso 1 1 calc R . . H25C H 0.1595 0.1252 0.1710 0.071 Uiso 1 1 calc R . . C26 C 0.3019(3) 0.07945(19) 0.0825(2) 0.0597(10) Uani 1 1 d . . . H26A H 0.2463 0.0889 0.0500 0.090 Uiso 1 1 calc R . . H26B H 0.3044 0.0284 0.0970 0.090 Uiso 1 1 calc R . . H26C H 0.3557 0.0920 0.0506 0.090 Uiso 1 1 calc R . . C27 C 0.46148(19) 0.36410(15) 0.21519(18) 0.0331(7) Uani 1 1 d . . . H27 H 0.4910 0.3329 0.2577 0.040 Uiso 1 1 calc R . . C28 C 0.4164(2) 0.42641(17) 0.25852(19) 0.0409(8) Uani 1 1 d . . . H28A H 0.3902 0.4596 0.2181 0.061 Uiso 1 1 calc R . . H28B H 0.4621 0.4517 0.2922 0.061 Uiso 1 1 calc R . . H28C H 0.3678 0.4082 0.2932 0.061 Uiso 1 1 calc R . . C29 C 0.5370(2) 0.39068(19) 0.1587(2) 0.0516(9) Uani 1 1 d . . . H29A H 0.5683 0.3494 0.1349 0.077 Uiso 1 1 calc R . . H29B H 0.5811 0.4196 0.1901 0.077 Uiso 1 1 calc R . . H29C H 0.5097 0.4200 0.1150 0.077 Uiso 1 1 calc R . . C30 C 0.9916(2) 0.17305(17) 0.28309(19) 0.0405(8) Uani 1 1 d . . . H30A H 1.0537 0.1798 0.3068 0.049 Uiso 1 1 calc R . . H30B H 0.9941 0.1810 0.2235 0.049 Uiso 1 1 calc R . . C31 C 0.9566(3) 0.09871(19) 0.3012(2) 0.0565(10) Uani 1 1 d . . . H31A H 1.0076 0.0646 0.3102 0.068 Uiso 1 1 calc R . . H31B H 0.9167 0.0808 0.2563 0.068 Uiso 1 1 calc R . . C32 C 0.9028(3) 0.10944(19) 0.3787(2) 0.0579(10) Uani 1 1 d . . . H32A H 0.8555 0.0719 0.3849 0.069 Uiso 1 1 calc R . . H32B H 0.9435 0.1097 0.4276 0.069 Uiso 1 1 calc R . . C33 C 0.8603(2) 0.18249(19) 0.3638(2) 0.0520(9) Uani 1 1 d . . . H33A H 0.8030 0.1780 0.3313 0.062 Uiso 1 1 calc R . . H33B H 0.8466 0.2064 0.4161 0.062 Uiso 1 1 calc R . . C34 C 0.7652(2) 0.37194(19) 0.3417(2) 0.0529(9) Uani 1 1 d . . . H34A H 0.7685 0.3457 0.3942 0.064 Uiso 1 1 calc R . . H34B H 0.7280 0.3436 0.3024 0.064 Uiso 1 1 calc R . . C35 C 0.7246(3) 0.4450(2) 0.3532(2) 0.0583(10) Uani 1 1 d . . . H35A H 0.7424 0.4654 0.4069 0.070 Uiso 1 1 calc R . . H35B H 0.6571 0.4436 0.3483 0.070 Uiso 1 1 calc R . . C36 C 0.7658(2) 0.48782(18) 0.2841(2) 0.0462(8) Uani 1 1 d . . . H36A H 0.7703 0.5394 0.2983 0.055 Uiso 1 1 calc R . . H36B H 0.7289 0.4826 0.2333 0.055 Uiso 1 1 calc R . . C37 C 0.8601(2) 0.45464(17) 0.2751(2) 0.0461(8) Uani 1 1 d . . . H37A H 0.8761 0.4513 0.2168 0.055 Uiso 1 1 calc R . . H37B H 0.9070 0.4842 0.3037 0.055 Uiso 1 1 calc R . . C38 C 1.0370(2) 0.34251(19) 0.16440(19) 0.0438(8) Uani 1 1 d . . . H38A H 0.9708 0.3398 0.1512 0.053 Uiso 1 1 calc R . . H38B H 1.0686 0.3032 0.1355 0.053 Uiso 1 1 calc R . . C39 C 1.0749(2) 0.4143(2) 0.1397(2) 0.0523(9) Uani 1 1 d . . . H39A H 1.0253 0.4501 0.1328 0.063 Uiso 1 1 calc R . . H39B H 1.1083 0.4104 0.0879 0.063 Uiso 1 1 calc R . . C40 C 1.1392(3) 0.4351(2) 0.2095(2) 0.0604(11) Uani 1 1 d . . . H40A H 1.2004 0.4478 0.1892 0.073 Uiso 1 1 calc R . . H40B H 1.1147 0.4763 0.2404 0.073 Uiso 1 1 calc R . . C41 C 1.1436(2) 0.3682(3) 0.2621(2) 0.0628(12) Uani 1 1 d . . . H41A H 1.1917 0.3350 0.2434 0.075 Uiso 1 1 calc R . . H41B H 1.1556 0.3805 0.3200 0.075 Uiso 1 1 calc R . . C42 C 1.0379(3) 0.40411(18) 0.4722(2) 0.0500(9) Uani 1 1 d . . . H42A H 0.9884 0.4404 0.4708 0.060 Uiso 1 1 calc R . . H42B H 1.0899 0.4225 0.4405 0.060 Uiso 1 1 calc R . . C43 C 1.0679(3) 0.3888(2) 0.5594(2) 0.0555(10) Uani 1 1 d . . . H43A H 1.1223 0.4176 0.5750 0.067 Uiso 1 1 calc R . . H43B H 1.0181 0.3991 0.5978 0.067 Uiso 1 1 calc R . . C44 C 1.0903(2) 0.3095(2) 0.5583(2) 0.0516(9) Uani 1 1 d . . . H44A H 1.0834 0.2877 0.6128 0.062 Uiso 1 1 calc R . . H44B H 1.1532 0.3009 0.5393 0.062 Uiso 1 1 calc R . . C45 C 1.0196(2) 0.28061(18) 0.4981(2) 0.0468(8) Uani 1 1 d . . . H45A H 1.0421 0.2365 0.4714 0.056 Uiso 1 1 calc R . . H45B H 0.9618 0.2694 0.5258 0.056 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 P1 0.0239(4) 0.0359(4) 0.0222(4) 0.0006(3) -0.0013(3) 0.0041(3) Li1 0.038(3) 0.039(3) 0.035(3) 0.004(2) 0.005(2) 0.000(2) N1 0.0218(11) 0.0287(12) 0.0260(12) -0.0006(10) -0.0030(9) 0.0001(9) O1 0.0356(11) 0.0382(12) 0.0386(12) -0.0010(9) 0.0039(9) 0.0000(9) O2 0.0396(12) 0.0396(13) 0.0506(14) 0.0055(11) 0.0045(10) 0.0038(10) O3 0.0342(12) 0.0680(16) 0.0346(12) 0.0088(11) 0.0004(9) -0.0063(11) O4 0.0533(14) 0.0342(12) 0.0346(12) 0.0042(10) -0.0066(10) -0.0009(10) C1 0.0244(14) 0.0342(16) 0.0284(15) -0.0012(12) -0.0036(11) 0.0050(12) C2 0.0307(15) 0.0390(17) 0.0265(15) -0.0063(13) -0.0060(12) 0.0041(13) C3 0.0328(15) 0.0475(18) 0.0195(13) -0.0023(13) -0.0013(11) 0.0041(14) C4 0.0256(14) 0.0399(17) 0.0272(15) 0.0036(13) 0.0002(11) 0.0019(12) C5 0.0243(14) 0.0350(16) 0.0239(14) 0.0012(12) -0.0031(11) 0.0055(12) C6 0.0202(13) 0.0332(16) 0.0252(14) 0.0001(12) -0.0033(10) 0.0044(11) C7 0.0364(16) 0.0299(16) 0.0330(16) -0.0010(13) -0.0035(13) 0.0022(13) C8 0.0478(19) 0.0434(19) 0.0463(19) -0.0027(16) -0.0072(15) -0.0118(16) C9 0.053(2) 0.0378(18) 0.0413(18) -0.0011(15) 0.0013(15) 0.0104(15) C10 0.0300(15) 0.0349(16) 0.0294(15) -0.0009(13) 0.0045(12) -0.0022(12) C11 0.0487(19) 0.0353(18) 0.0444(19) 0.0009(15) 0.0046(15) -0.0033(15) C12 0.0309(16) 0.055(2) 0.0441(19) -0.0101(16) -0.0014(14) -0.0058(15) C13 0.0244(13) 0.0237(14) 0.0248(14) -0.0023(11) -0.0022(11) -0.0023(11) C14 0.0239(14) 0.0320(16) 0.0289(15) -0.0020(12) -0.0019(11) 0.0045(12) C15 0.0411(19) 0.083(3) 0.0412(19) 0.0004(18) -0.0028(15) 0.0318(19) C16 0.0400(19) 0.052(2) 0.078(3) -0.008(2) -0.0315(18) 0.0056(16) C17 0.0358(18) 0.057(2) 0.064(2) 0.0243(19) 0.0000(16) 0.0138(16) C18 0.0204(13) 0.0335(15) 0.0206(13) -0.0032(12) 0.0026(10) 0.0012(11) C19 0.0268(14) 0.0336(16) 0.0268(14) -0.0040(12) 0.0004(11) 0.0014(12) C20 0.0278(14) 0.0424(18) 0.0268(15) -0.0048(13) -0.0040(11) -0.0015(13) C21 0.0365(17) 0.0460(19) 0.0255(15) 0.0033(13) -0.0060(12) 0.0038(14) C22 0.0374(16) 0.0329(16) 0.0294(15) 0.0029(13) 0.0007(12) -0.0002(13) C23 0.0247(14) 0.0332(16) 0.0244(14) 0.0008(12) 0.0027(11) -0.0005(12) C24 0.0286(15) 0.0348(17) 0.0469(18) -0.0010(14) -0.0082(13) -0.0004(13) C25 0.049(2) 0.048(2) 0.0456(19) 0.0044(16) 0.0027(15) -0.0156(16) C26 0.052(2) 0.045(2) 0.082(3) -0.022(2) 0.017(2) -0.0084(17) C27 0.0321(15) 0.0283(16) 0.0387(17) 0.0039(13) -0.0064(13) -0.0037(12) C28 0.0417(18) 0.0440(19) 0.0369(17) -0.0086(15) -0.0003(14) -0.0073(15) C29 0.0349(18) 0.052(2) 0.068(2) -0.0148(19) 0.0125(16) -0.0091(16) C30 0.0384(17) 0.0421(19) 0.0407(18) -0.0091(15) -0.0093(14) 0.0089(14) C31 0.078(3) 0.039(2) 0.052(2) -0.0013(17) -0.0091(19) 0.0048(18) C32 0.073(3) 0.043(2) 0.057(2) 0.0092(18) -0.007(2) -0.0118(19) C33 0.047(2) 0.051(2) 0.058(2) 0.0091(18) 0.0105(17) -0.0085(17) C34 0.052(2) 0.050(2) 0.057(2) -0.0020(18) 0.0180(17) 0.0030(17) C35 0.064(2) 0.057(2) 0.054(2) -0.0012(19) 0.0102(19) 0.0141(19) C36 0.0453(19) 0.0433(19) 0.050(2) -0.0012(16) -0.0072(15) 0.0070(15) C37 0.0433(19) 0.0377(18) 0.057(2) 0.0049(16) -0.0049(16) -0.0006(15) C38 0.0371(17) 0.060(2) 0.0344(17) 0.0032(16) 0.0003(13) -0.0088(16) C39 0.043(2) 0.057(2) 0.057(2) 0.0153(18) 0.0053(17) -0.0006(17) C40 0.047(2) 0.061(2) 0.073(3) -0.015(2) 0.0109(19) -0.0169(18) C41 0.0292(18) 0.121(4) 0.0378(19) -0.007(2) -0.0035(14) 0.000(2) C42 0.060(2) 0.041(2) 0.050(2) -0.0063(16) 0.0063(17) -0.0068(17) C43 0.052(2) 0.067(3) 0.048(2) -0.0155(19) -0.0072(17) -0.0064(19) C44 0.0429(19) 0.067(2) 0.044(2) -0.0005(18) -0.0069(15) 0.0054(18) C45 0.054(2) 0.045(2) 0.0409(18) 0.0048(15) -0.0024(16) 0.0035(16) _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 P1 C13 1.796(3) . ? P1 C6 1.875(3) . ? Li1 O1 1.909(6) . ? Li1 O3 1.914(5) . ? Li1 O4 1.929(6) . ? Li1 O2 1.937(6) . ? N1 C13 1.317(3) . ? N1 C18 1.411(3) . ? O1 C33 1.438(4) . ? O1 C30 1.452(4) . ? O2 C37 1.441(4) . ? O2 C34 1.444(4) . ? O3 C38 1.436(4) . ? O3 C41 1.461(4) . ? O4 C42 1.436(4) . ? O4 C45 1.440(4) . ? C1 C2 1.401(4) . ? C1 C6 1.416(4) . ? C1 C7 1.520(4) . ? C2 C3 1.383(4) . ? C2 H2 0.9500 . ? C3 C4 1.382(4) . ? C3 H3 0.9500 . ? C4 C5 1.398(4) . ? C4 H4 0.9500 . ? C5 C6 1.433(4) . ? C5 C10 1.525(4) . ? C7 C9 1.536(4) . ? C7 C8 1.542(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.533(4) . ? C10 C11 1.534(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.553(4) . ? C14 C17 1.523(4) . ? C14 C15 1.525(4) . ? C14 C16 1.528(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.415(4) . ? C18 C19 1.422(4) . ? C19 C20 1.397(4) . ? C19 C24 1.512(4) . ? C20 C21 1.381(4) . ? C20 H20 0.9500 . ? C21 C22 1.384(4) . ? C21 H21 0.9500 . ? C22 C23 1.396(4) . ? C22 H22 0.9500 . ? C23 C27 1.523(4) . ? C24 C25 1.533(4) . ? C24 C26 1.534(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.517(4) . ? C27 C29 1.536(4) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.508(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.520(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.513(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.498(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.519(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.522(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.505(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.520(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.516(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.516(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.512(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.516(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 P1 C6 111.59(12) . . ? O1 Li1 O3 105.2(3) . . ? O1 Li1 O4 107.8(3) . . ? O3 Li1 O4 111.5(3) . . ? O1 Li1 O2 112.0(3) . . ? O3 Li1 O2 111.6(3) . . ? O4 Li1 O2 108.6(3) . . ? C13 N1 C18 121.9(2) . . ? C33 O1 C30 109.3(2) . . ? C33 O1 Li1 128.9(2) . . ? C30 O1 Li1 119.2(2) . . ? C37 O2 C34 109.5(2) . . ? C37 O2 Li1 124.9(2) . . ? C34 O2 Li1 124.9(2) . . ? C38 O3 C41 102.9(2) . . ? C38 O3 Li1 125.1(2) . . ? C41 O3 Li1 129.0(3) . . ? C42 O4 C45 109.9(2) . . ? C42 O4 Li1 126.0(2) . . ? C45 O4 Li1 123.9(2) . . ? C2 C1 C6 120.0(3) . . ? C2 C1 C7 118.3(3) . . ? C6 C1 C7 121.6(2) . . ? C3 C2 C1 121.4(3) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C4 C3 C2 119.4(3) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 121.4(3) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 C10 118.4(3) . . ? C6 C5 C10 121.7(2) . . ? C1 C6 C5 118.0(2) . . ? C1 C6 P1 120.0(2) . . ? C5 C6 P1 120.3(2) . . ? C1 C7 C9 110.3(2) . . ? C1 C7 C8 113.2(2) . . ? C9 C7 C8 110.0(3) . . ? C1 C7 H7 107.7 . . ? C9 C7 H7 107.7 . . ? C8 C7 H7 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 C12 110.7(2) . . ? C5 C10 C11 113.6(2) . . ? C12 C10 C11 110.1(3) . . ? C5 C10 H10 107.4 . . ? C12 C10 H10 107.4 . . ? C11 C10 H10 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 113.0(2) . . ? N1 C13 P1 118.8(2) . . ? C14 C13 P1 128.14(19) . . ? C17 C14 C15 107.3(3) . . ? C17 C14 C16 108.8(3) . . ? C15 C14 C16 109.1(3) . . ? C17 C14 C13 111.9(2) . . ? C15 C14 C13 111.1(2) . . ? C16 C14 C13 108.6(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 C23 119.4(2) . . ? N1 C18 C19 120.6(2) . . ? C23 C18 C19 119.5(2) . . ? C20 C19 C18 118.6(3) . . ? C20 C19 C24 120.7(3) . . ? C18 C19 C24 120.8(2) . . ? C21 C20 C19 121.8(3) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C22 119.5(3) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 121.2(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 119.4(3) . . ? C22 C23 C27 119.7(3) . . ? C18 C23 C27 120.9(2) . . ? C19 C24 C25 111.4(3) . . ? C19 C24 C26 112.1(3) . . ? C25 C24 C26 109.5(3) . . ? C19 C24 H24 107.9 . . ? C25 C24 H24 107.9 . . ? C26 C24 H24 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C23 111.2(2) . . ? C28 C27 C29 111.1(3) . . ? C23 C27 C29 111.5(3) . . ? C28 C27 H27 107.6 . . ? C23 C27 H27 107.6 . . ? C29 C27 H27 107.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 C31 106.0(3) . . ? O1 C30 H30A 110.5 . . ? C31 C30 H30A 110.5 . . ? O1 C30 H30B 110.5 . . ? C31 C30 H30B 110.5 . . ? H30A C30 H30B 108.7 . . ? C30 C31 C32 103.1(3) . . ? C30 C31 H31A 111.1 . . ? C32 C31 H31A 111.1 . . ? C30 C31 H31B 111.1 . . ? C32 C31 H31B 111.1 . . ? H31A C31 H31B 109.1 . . ? C33 C32 C31 101.5(3) . . ? C33 C32 H32A 111.5 . . ? C31 C32 H32A 111.5 . . ? C33 C32 H32B 111.5 . . ? C31 C32 H32B 111.5 . . ? H32A C32 H32B 109.3 . . ? O1 C33 C32 105.3(3) . . ? O1 C33 H33A 110.7 . . ? C32 C33 H33A 110.7 . . ? O1 C33 H33B 110.7 . . ? C32 C33 H33B 110.7 . . ? H33A C33 H33B 108.8 . . ? O2 C34 C35 105.7(3) . . ? O2 C34 H34A 110.6 . . ? C35 C34 H34A 110.6 . . ? O2 C34 H34B 110.6 . . ? C35 C34 H34B 110.6 . . ? H34A C34 H34B 108.7 . . ? C34 C35 C36 102.7(3) . . ? C34 C35 H35A 111.2 . . ? C36 C35 H35A 111.2 . . ? C34 C35 H35B 111.2 . . ? C36 C35 H35B 111.2 . . ? H35A C35 H35B 109.1 . . ? C35 C36 C37 103.4(3) . . ? C35 C36 H36A 111.1 . . ? C37 C36 H36A 111.1 . . ? C35 C36 H36B 111.1 . . ? C37 C36 H36B 111.1 . . ? H36A C36 H36B 109.0 . . ? O2 C37 C36 106.5(3) . . ? O2 C37 H37A 110.4 . . ? C36 C37 H37A 110.4 . . ? O2 C37 H37B 110.4 . . ? C36 C37 H37B 110.4 . . ? H37A C37 H37B 108.6 . . ? O3 C38 C39 106.2(3) . . ? O3 C38 H38A 110.5 . . ? C39 C38 H38A 110.5 . . ? O3 C38 H38B 110.5 . . ? C39 C38 H38B 110.5 . . ? H38A C38 H38B 108.7 . . ? C38 C39 C40 104.4(3) . . ? C38 C39 H39A 110.9 . . ? C40 C39 H39A 110.9 . . ? C38 C39 H39B 110.9 . . ? C40 C39 H39B 110.9 . . ? H39A C39 H39B 108.9 . . ? C41 C40 C39 103.8(3) . . ? C41 C40 H40A 111.0 . . ? C39 C40 H40A 111.0 . . ? C41 C40 H40B 111.0 . . ? C39 C40 H40B 111.0 . . ? H40A C40 H40B 109.0 . . ? O3 C41 C40 103.2(3) . . ? O3 C41 H41A 111.1 . . ? C40 C41 H41A 111.1 . . ? O3 C41 H41B 111.1 . . ? C40 C41 H41B 111.1 . . ? H41A C41 H41B 109.1 . . ? O4 C42 C43 106.2(3) . . ? O4 C42 H42A 110.5 . . ? C43 C42 H42A 110.5 . . ? O4 C42 H42B 110.5 . . ? C43 C42 H42B 110.5 . . ? H42A C42 H42B 108.7 . . ? C44 C43 C42 103.4(3) . . ? C44 C43 H43A 111.1 . . ? C42 C43 H43A 111.1 . . ? C44 C43 H43B 111.1 . . ? C42 C43 H43B 111.1 . . ? H43A C43 H43B 109.1 . . ? C43 C44 C45 102.1(3) . . ? C43 C44 H44A 111.4 . . ? C45 C44 H44A 111.4 . . ? C43 C44 H44B 111.4 . . ? C45 C44 H44B 111.4 . . ? H44A C44 H44B 109.2 . . ? O4 C45 C44 105.3(3) . . ? O4 C45 H45A 110.7 . . ? C44 C45 H45A 110.7 . . ? O4 C45 H45B 110.7 . . ? C44 C45 H45B 110.7 . . ? H45A C45 H45B 108.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Li1 O1 C33 -179.1(3) . . . . ? O4 Li1 O1 C33 61.7(4) . . . . ? O2 Li1 O1 C33 -57.7(4) . . . . ? O3 Li1 O1 C30 21.1(4) . . . . ? O4 Li1 O1 C30 -98.0(3) . . . . ? O2 Li1 O1 C30 142.6(2) . . . . ? O1 Li1 O2 C37 -148.0(3) . . . . ? O3 Li1 O2 C37 -30.3(4) . . . . ? O4 Li1 O2 C37 93.1(3) . . . . ? O1 Li1 O2 C34 42.3(4) . . . . ? O3 Li1 O2 C34 160.0(3) . . . . ? O4 Li1 O2 C34 -76.6(4) . . . . ? O1 Li1 O3 C38 75.5(4) . . . . ? O4 Li1 O3 C38 -167.9(3) . . . . ? O2 Li1 O3 C38 -46.2(4) . . . . ? O1 Li1 O3 C41 -127.4(3) . . . . ? O4 Li1 O3 C41 -10.7(5) . . . . ? O2 Li1 O3 C41 111.0(4) . . . . ? O1 Li1 O4 C42 179.8(3) . . . . ? O3 Li1 O4 C42 64.8(4) . . . . ? O2 Li1 O4 C42 -58.6(4) . . . . ? O1 Li1 O4 C45 5.0(4) . . . . ? O3 Li1 O4 C45 -110.1(3) . . . . ? O2 Li1 O4 C45 126.5(3) . . . . ? C6 C1 C2 C3 1.4(4) . . . . ? C7 C1 C2 C3 178.1(3) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C3 C4 C5 C10 -178.5(3) . . . . ? C2 C1 C6 C5 -2.1(4) . . . . ? C7 C1 C6 C5 -178.7(2) . . . . ? C2 C1 C6 P1 162.9(2) . . . . ? C7 C1 C6 P1 -13.7(3) . . . . ? C4 C5 C6 C1 1.4(4) . . . . ? C10 C5 C6 C1 180.0(2) . . . . ? C4 C5 C6 P1 -163.6(2) . . . . ? C10 C5 C6 P1 15.0(3) . . . . ? C13 P1 C6 C1 97.8(2) . . . . ? C13 P1 C6 C5 -97.5(2) . . . . ? C2 C1 C7 C9 -75.9(3) . . . . ? C6 C1 C7 C9 100.8(3) . . . . ? C2 C1 C7 C8 47.9(4) . . . . ? C6 C1 C7 C8 -135.5(3) . . . . ? C4 C5 C10 C12 81.1(3) . . . . ? C6 C5 C10 C12 -97.5(3) . . . . ? C4 C5 C10 C11 -43.4(3) . . . . ? C6 C5 C10 C11 138.0(3) . . . . ? C18 N1 C13 C14 -172.9(2) . . . . ? C18 N1 C13 P1 5.4(3) . . . . ? C6 P1 C13 N1 -176.8(2) . . . . ? C6 P1 C13 C14 1.1(3) . . . . ? N1 C13 C14 C17 -129.3(3) . . . . ? P1 C13 C14 C17 52.6(3) . . . . ? N1 C13 C14 C15 -9.4(3) . . . . ? P1 C13 C14 C15 172.5(2) . . . . ? N1 C13 C14 C16 110.7(3) . . . . ? P1 C13 C14 C16 -67.4(3) . . . . ? C13 N1 C18 C23 89.8(3) . . . . ? C13 N1 C18 C19 -98.1(3) . . . . ? N1 C18 C19 C20 -170.3(2) . . . . ? C23 C18 C19 C20 1.8(4) . . . . ? N1 C18 C19 C24 9.4(4) . . . . ? C23 C18 C19 C24 -178.5(2) . . . . ? C18 C19 C20 C21 0.4(4) . . . . ? C24 C19 C20 C21 -179.3(3) . . . . ? C19 C20 C21 C22 -1.4(4) . . . . ? C20 C21 C22 C23 0.1(4) . . . . ? C21 C22 C23 C18 2.1(4) . . . . ? C21 C22 C23 C27 -179.1(3) . . . . ? N1 C18 C23 C22 169.2(2) . . . . ? C19 C18 C23 C22 -3.0(4) . . . . ? N1 C18 C23 C27 -9.6(4) . . . . ? C19 C18 C23 C27 178.2(2) . . . . ? C20 C19 C24 C25 -71.3(3) . . . . ? C18 C19 C24 C25 109.0(3) . . . . ? C20 C19 C24 C26 51.7(4) . . . . ? C18 C19 C24 C26 -128.0(3) . . . . ? C22 C23 C27 C28 58.6(3) . . . . ? C18 C23 C27 C28 -122.6(3) . . . . ? C22 C23 C27 C29 -65.9(3) . . . . ? C18 C23 C27 C29 112.9(3) . . . . ? C33 O1 C30 C31 4.2(3) . . . . ? Li1 O1 C30 C31 167.6(3) . . . . ? O1 C30 C31 C32 -26.1(3) . . . . ? C30 C31 C32 C33 36.9(4) . . . . ? C30 O1 C33 C32 19.7(4) . . . . ? Li1 O1 C33 C32 -141.6(3) . . . . ? C31 C32 C33 O1 -35.1(4) . . . . ? C37 O2 C34 C35 -21.1(4) . . . . ? Li1 O2 C34 C35 149.9(3) . . . . ? O2 C34 C35 C36 33.7(4) . . . . ? C34 C35 C36 C37 -33.2(4) . . . . ? C34 O2 C37 C36 -0.4(4) . . . . ? Li1 O2 C37 C36 -171.5(3) . . . . ? C35 C36 C37 O2 21.3(4) . . . . ? C41 O3 C38 C39 -39.5(3) . . . . ? Li1 O3 C38 C39 122.5(3) . . . . ? O3 C38 C39 C40 18.8(4) . . . . ? C38 C39 C40 C41 8.4(4) . . . . ? C38 O3 C41 C40 44.4(3) . . . . ? Li1 O3 C41 C40 -116.7(3) . . . . ? C39 C40 C41 O3 -32.0(4) . . . . ? C45 O4 C42 C43 -3.8(4) . . . . ? Li1 O4 C42 C43 -179.2(3) . . . . ? O4 C42 C43 C44 24.7(4) . . . . ? C42 C43 C44 C45 -35.0(4) . . . . ? C42 O4 C45 C44 -18.8(4) . . . . ? Li1 O4 C45 C44 156.8(3) . . . . ? C43 C44 C45 O4 33.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.397 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.050 # Attachment 'shelxlk.cif' data_shelxlk _database_code_depnum_ccdc_archive 'CCDC 736329' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H75 K N O4 P' _chemical_formula_sum 'C45 H75 K N O4 P' _chemical_formula_weight 764.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 9.885(4) _cell_length_b 23.726(10) _cell_length_c 19.383(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.308(7) _cell_angle_gamma 90.00 _cell_volume 4545(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8137 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9591 _exptl_absorpt_correction_T_max 0.9700 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39550 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8025 _reflns_number_gt 6328 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0930P)^2^+7.8429P] 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 8025 _refine_ls_number_parameters 572 _refine_ls_number_restraints 446 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.2081 _refine_ls_wR_factor_gt 0.1932 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.220 _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 P1 P 0.70761(10) 0.16263(4) 0.84095(5) 0.0223(3) Uani 1 1 d . A . K1 K 0.66410(9) 0.28176(4) 0.76959(4) 0.0318(3) Uani 1 1 d D . . N1 N 0.8617(3) 0.20187(13) 0.94521(16) 0.0241(7) Uani 1 1 d . . . C1 C 0.7165(4) 0.28507(16) 0.94332(19) 0.0253(8) Uani 1 1 d . A . C2 C 0.6982(4) 0.34110(17) 0.9240(2) 0.0322(9) Uani 1 1 d . A . H2 H 0.6208 0.3628 0.9430 0.039 Uiso 1 1 calc R . . C3 C 0.7878(5) 0.36807(17) 0.8809(2) 0.0368(10) Uani 1 1 d . A . H3 H 0.7803 0.4096 0.8729 0.044 Uiso 1 1 calc R . . C4 C 0.8975(4) 0.33843(17) 0.8560(2) 0.0346(10) Uani 1 1 d . A . H4 H 0.9695 0.3595 0.8313 0.042 Uiso 1 1 calc R . . C5 C 0.9201(4) 0.28230(17) 0.8736(2) 0.0281(9) Uani 1 1 d . A . C6 C 0.8299(4) 0.25538(15) 0.91882(18) 0.0224(8) Uani 1 1 d . A . C7 C 0.6198(4) 0.25609(17) 0.9916(2) 0.0279(9) Uani 1 1 d . . . H7 H 0.6230 0.2148 0.9811 0.033 Uiso 1 1 calc R A . C8 C 0.4744(5) 0.2749(3) 0.9810(3) 0.073(2) Uani 1 1 d . A . H8A H 0.4157 0.2521 1.0101 0.110 Uiso 1 1 calc R . . H8B H 0.4473 0.2700 0.9324 0.110 Uiso 1 1 calc R . . H8C H 0.4663 0.3147 0.9937 0.110 Uiso 1 1 calc R . . C9 C 0.6661(6) 0.2634(3) 1.0662(2) 0.0630(17) Uani 1 1 d . A . H9A H 0.6598 0.3033 1.0790 0.095 Uiso 1 1 calc R . . H9B H 0.7602 0.2508 1.0716 0.095 Uiso 1 1 calc R . . H9C H 0.6084 0.2409 1.0960 0.095 Uiso 1 1 calc R . . C10 C 1.0416(4) 0.25111(19) 0.8462(2) 0.0357(10) Uani 1 1 d . . . H10 H 1.0352 0.2109 0.8614 0.043 Uiso 1 1 calc R A . C11 C 1.1714(5) 0.2753(3) 0.8766(3) 0.0588(15) Uani 1 1 d . A . H11A H 1.1740 0.3160 0.8681 0.088 Uiso 1 1 calc R . . H11B H 1.2490 0.2573 0.8549 0.088 Uiso 1 1 calc R . . H11C H 1.1754 0.2683 0.9264 0.088 Uiso 1 1 calc R . . C12 C 1.0448(5) 0.2517(2) 0.7676(3) 0.0501(13) Uani 1 1 d . A . H12A H 1.0481 0.2908 0.7513 0.075 Uiso 1 1 calc R . . H12B H 0.9633 0.2333 0.7487 0.075 Uiso 1 1 calc R . . H12C H 1.1251 0.2315 0.7523 0.075 Uiso 1 1 calc R . . C13 C 0.8175(4) 0.15606(15) 0.91518(18) 0.0219(8) Uani 1 1 d . A . C14 C 0.8633(4) 0.10124(16) 0.9520(2) 0.0282(9) Uani 1 1 d . . . C15 C 0.9654(6) 0.1145(2) 1.0105(3) 0.0514(13) Uani 1 1 d . A . H15A H 0.9935 0.0794 1.0333 0.077 Uiso 1 1 calc R . . H15B H 0.9233 0.1395 1.0441 0.077 Uiso 1 1 calc R . . H15C H 1.0447 0.1332 0.9914 0.077 Uiso 1 1 calc R . . C16 C 0.9345(5) 0.06120(18) 0.9024(2) 0.0403(11) Uani 1 1 d . A . H16A H 1.0090 0.0811 0.8805 0.061 Uiso 1 1 calc R . . H16B H 0.8696 0.0481 0.8669 0.061 Uiso 1 1 calc R . . H16C H 0.9704 0.0287 0.9282 0.061 Uiso 1 1 calc R . . C17 C 0.7408(5) 0.0722(2) 0.9818(2) 0.0441(12) Uani 1 1 d . A . H17A H 0.7701 0.0388 1.0077 0.066 Uiso 1 1 calc R . . H17B H 0.6785 0.0610 0.9442 0.066 Uiso 1 1 calc R . . H17C H 0.6948 0.0983 1.0127 0.066 Uiso 1 1 calc R . . C18 C 0.6610(4) 0.09377(15) 0.80161(19) 0.0248(8) Uani 1 1 d . . . C19 C 0.7411(4) 0.07014(16) 0.7485(2) 0.0282(9) Uani 1 1 d . A . C20 C 0.6910(5) 0.02566(18) 0.7091(2) 0.0387(10) Uani 1 1 d . . . H20 H 0.7454 0.0098 0.6743 0.046 Uiso 1 1 calc R A . C21 C 0.5633(5) 0.0040(2) 0.7198(3) 0.0476(12) Uani 1 1 d . A . H21 H 0.5296 -0.0261 0.6919 0.057 Uiso 1 1 calc R . . C22 C 0.4856(5) 0.02627(19) 0.7709(2) 0.0430(11) Uani 1 1 d . . . H22 H 0.3982 0.0110 0.7781 0.052 Uiso 1 1 calc R A . C23 C 0.5313(4) 0.07051(16) 0.8124(2) 0.0298(9) Uani 1 1 d . A . C24 C 0.8787(4) 0.09402(18) 0.7313(2) 0.0328(9) Uani 1 1 d . . . H24 H 0.9093 0.1183 0.7708 0.039 Uiso 1 1 calc R A . C25 C 0.8678(5) 0.1316(2) 0.6670(2) 0.0430(11) Uani 1 1 d . A . H25A H 0.8377 0.1088 0.6273 0.065 Uiso 1 1 calc R . . H25B H 0.9564 0.1481 0.6578 0.065 Uiso 1 1 calc R . . H25C H 0.8022 0.1617 0.6748 0.065 Uiso 1 1 calc R . . C26 C 0.9867(5) 0.0487(2) 0.7212(3) 0.0517(13) Uani 1 1 d . A . H26A H 0.9874 0.0228 0.7606 0.078 Uiso 1 1 calc R . . H26B H 1.0757 0.0666 0.7178 0.078 Uiso 1 1 calc R . . H26C H 0.9663 0.0277 0.6787 0.078 Uiso 1 1 calc R . . C27 C 0.4374(4) 0.09301(18) 0.8676(2) 0.0359(10) Uani 1 1 d . . . H27 H 0.4931 0.1167 0.9000 0.043 Uiso 1 1 calc R A . C28 C 0.3725(5) 0.0463(2) 0.9099(3) 0.0521(13) Uani 1 1 d . A . H28A H 0.3194 0.0631 0.9467 0.078 Uiso 1 1 calc R . . H28B H 0.4434 0.0222 0.9303 0.078 Uiso 1 1 calc R . . H28C H 0.3130 0.0235 0.8799 0.078 Uiso 1 1 calc R . . C29 C 0.3274(5) 0.1308(2) 0.8357(3) 0.0558(14) Uani 1 1 d . A . H29A H 0.2724 0.1089 0.8026 0.084 Uiso 1 1 calc R . . H29B H 0.3695 0.1625 0.8119 0.084 Uiso 1 1 calc R . . H29C H 0.2696 0.1451 0.8722 0.084 Uiso 1 1 calc R . . O2 O 0.4374(3) 0.34148(13) 0.76376(16) 0.0438(8) Uani 1 1 d . A . C34 C 0.3612(5) 0.3446(2) 0.7006(3) 0.0465(12) Uani 1 1 d . . . H34A H 0.2843 0.3178 0.7010 0.056 Uiso 1 1 calc R A . H34B H 0.4188 0.3355 0.6610 0.056 Uiso 1 1 calc R . . C35 C 0.3105(5) 0.4048(2) 0.6958(3) 0.0493(12) Uani 1 1 d . A . H35A H 0.2241 0.4071 0.6691 0.059 Uiso 1 1 calc R . . H35B H 0.3780 0.4297 0.6743 0.059 Uiso 1 1 calc R . . C36 C 0.2915(5) 0.4198(2) 0.7711(3) 0.0427(11) Uani 1 1 d . . . H36A H 0.2969 0.4610 0.7787 0.051 Uiso 1 1 calc R A . H36B H 0.2039 0.4057 0.7879 0.051 Uiso 1 1 calc R . . C37 C 0.4094(5) 0.38954(19) 0.8054(2) 0.0422(11) Uani 1 1 d . A . H37A H 0.4894 0.4146 0.8085 0.051 Uiso 1 1 calc R . . H37B H 0.3860 0.3777 0.8526 0.051 Uiso 1 1 calc R . . O3 O 0.5728(4) 0.23021(15) 0.65264(16) 0.0512(9) Uani 1 1 d D A . C38 C 0.4720(6) 0.1847(2) 0.6696(2) 0.0648(17) Uani 1 1 d D A . H38A H 0.4955 0.1672 0.7147 0.078 Uiso 1 1 calc R . . H38B H 0.3796 0.2006 0.6719 0.078 Uiso 1 1 calc R . . C39 C 0.4791(7) 0.1438(2) 0.6150(3) 0.078(2) Uani 1 1 d D . . H39A H 0.3872 0.1310 0.6008 0.093 Uiso 1 1 calc R A . H39B H 0.5324 0.1106 0.6304 0.093 Uiso 1 1 calc R . . C40 C 0.5478(8) 0.1730(3) 0.5550(3) 0.085(2) Uani 1 1 d D A . H40A H 0.4873 0.1739 0.5136 0.102 Uiso 1 1 calc R . . H40B H 0.6327 0.1534 0.5433 0.102 Uiso 1 1 calc R . . C41 C 0.5773(6) 0.2327(2) 0.5809(2) 0.0612(15) Uani 1 1 d D . . H41A H 0.6677 0.2452 0.5662 0.073 Uiso 1 1 calc R A . H41B H 0.5085 0.2594 0.5624 0.073 Uiso 1 1 calc R . . O1 O 0.7905(9) 0.3566(4) 0.6841(5) 0.046(2) Uani 0.493(11) 1 d PDU A 1 C30 C 0.7048(12) 0.4052(5) 0.6595(7) 0.052(3) Uani 0.493(11) 1 d PDU A 1 H30C H 0.6169 0.3920 0.6400 0.063 Uiso 0.493(11) 1 calc PR A 1 H30D H 0.6882 0.4322 0.6974 0.063 Uiso 0.493(11) 1 calc PR A 1 C31 C 0.7895(13) 0.4311(5) 0.6052(8) 0.061(3) Uani 0.493(11) 1 d PDU A 1 H31C H 0.8117 0.4707 0.6169 0.073 Uiso 0.493(11) 1 calc PR A 1 H31D H 0.7417 0.4302 0.5598 0.073 Uiso 0.493(11) 1 calc PR A 1 C32 C 0.9184(12) 0.3949(6) 0.6041(8) 0.077(3) Uani 0.493(11) 1 d PDU A 1 H32C H 0.9429 0.3873 0.5557 0.093 Uiso 0.493(11) 1 calc PR A 1 H32D H 0.9942 0.4156 0.6267 0.093 Uiso 0.493(11) 1 calc PR A 1 C33 C 0.8970(14) 0.3421(5) 0.6397(7) 0.068(3) Uani 0.493(11) 1 d PDU A 1 H33C H 0.8695 0.3118 0.6072 0.081 Uiso 0.493(11) 1 calc PR A 1 H33D H 0.9790 0.3302 0.6661 0.081 Uiso 0.493(11) 1 calc PR A 1 O1' O 0.7411(11) 0.3477(4) 0.6694(5) 0.051(2) Uani 0.507(11) 1 d PDU A 2 C30' C 0.7358(15) 0.4070(4) 0.6719(7) 0.055(3) Uani 0.507(11) 1 d PDU A 2 H30A H 0.7692 0.4206 0.7175 0.066 Uiso 0.507(11) 1 calc PR A 2 H30B H 0.6414 0.4200 0.6648 0.066 Uiso 0.507(11) 1 calc PR A 2 C31' C 0.8244(17) 0.4298(4) 0.6150(8) 0.067(3) Uani 0.507(11) 1 d PDU A 2 H31A H 0.9032 0.4506 0.6347 0.080 Uiso 0.507(11) 1 calc PR A 2 H31B H 0.7723 0.4553 0.5839 0.080 Uiso 0.507(11) 1 calc PR A 2 C32' C 0.8711(14) 0.3755(5) 0.5755(6) 0.065(2) Uani 0.507(11) 1 d PDU A 2 H32A H 0.8338 0.3754 0.5277 0.078 Uiso 0.507(11) 1 calc PR A 2 H32B H 0.9711 0.3739 0.5739 0.078 Uiso 0.507(11) 1 calc PR A 2 C33' C 0.8195(14) 0.3282(4) 0.6139(6) 0.060(3) Uani 0.507(11) 1 d PDU A 2 H33A H 0.7630 0.3042 0.5830 0.072 Uiso 0.507(11) 1 calc PR A 2 H33B H 0.8959 0.3052 0.6320 0.072 Uiso 0.507(11) 1 calc PR A 2 O4 O 0.8822(12) 0.0115(5) 0.4262(7) 0.085(3) Uani 0.599(12) 1 d PDU B 3 C42 C 0.8512(12) 0.0468(5) 0.4829(5) 0.066(3) Uani 0.599(12) 1 d PDU B 3 H42A H 0.8210 0.0844 0.4666 0.079 Uiso 0.599(12) 1 calc PR B 3 H42B H 0.9314 0.0516 0.5138 0.079 Uiso 0.599(12) 1 calc PR B 3 C43 C 0.7382(13) 0.0170(5) 0.5203(5) 0.083(3) Uani 0.599(12) 1 d PDU B 3 H43A H 0.6747 0.0447 0.5398 0.099 Uiso 0.599(12) 1 calc PR B 3 H43B H 0.7756 -0.0066 0.5583 0.099 Uiso 0.599(12) 1 calc PR B 3 C44 C 0.6660(15) -0.0197(7) 0.4655(9) 0.082(3) Uani 0.599(12) 1 d PDU B 3 H44A H 0.6336 -0.0554 0.4859 0.098 Uiso 0.599(12) 1 calc PR B 3 H44B H 0.5881 0.0005 0.4442 0.098 Uiso 0.599(12) 1 calc PR B 3 C45 C 0.7746(14) -0.0310(6) 0.4127(6) 0.081(3) Uani 0.599(12) 1 d PDU B 3 H45A H 0.8112 -0.0696 0.4183 0.097 Uiso 0.599(12) 1 calc PR B 3 H45B H 0.7368 -0.0269 0.3653 0.097 Uiso 0.599(12) 1 calc PR B 3 O4' O 0.848(2) 0.0230(7) 0.4189(10) 0.083(3) Uani 0.401(12) 1 d PDU B 4 C42' C 0.8028(19) 0.0676(7) 0.4627(11) 0.079(4) Uani 0.401(12) 1 d PDU B 4 H42C H 0.7888 0.1032 0.4370 0.094 Uiso 0.401(12) 1 calc PR B 4 H42D H 0.8654 0.0740 0.5024 0.094 Uiso 0.401(12) 1 calc PR B 4 C43' C 0.6747(17) 0.0426(7) 0.4838(11) 0.085(3) Uani 0.401(12) 1 d PDU B 4 H43C H 0.5991 0.0593 0.4563 0.102 Uiso 0.401(12) 1 calc PR B 4 H43D H 0.6598 0.0511 0.5330 0.102 Uiso 0.401(12) 1 calc PR B 4 C44' C 0.677(2) -0.0210(8) 0.4731(16) 0.084(3) Uani 0.401(12) 1 d PDU B 4 H44C H 0.6835 -0.0406 0.5182 0.100 Uiso 0.401(12) 1 calc PR B 4 H44D H 0.5926 -0.0334 0.4489 0.100 Uiso 0.401(12) 1 calc PR B 4 C45' C 0.799(2) -0.0345(7) 0.4302(12) 0.084(3) Uani 0.401(12) 1 d PDU B 4 H45C H 0.8658 -0.0580 0.4559 0.101 Uiso 0.401(12) 1 calc PR B 4 H45D H 0.7728 -0.0534 0.3863 0.101 Uiso 0.401(12) 1 calc PRU B 4 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 P1 0.0268(5) 0.0180(5) 0.0219(5) 0.0008(4) -0.0034(4) -0.0008(4) K1 0.0398(5) 0.0267(5) 0.0289(5) 0.0056(4) 0.0007(4) 0.0071(4) N1 0.0243(16) 0.0249(17) 0.0230(16) 0.0009(13) -0.0029(13) -0.0010(13) C1 0.028(2) 0.029(2) 0.0193(18) -0.0016(15) -0.0026(15) -0.0031(16) C2 0.038(2) 0.026(2) 0.032(2) -0.0040(17) -0.0027(18) 0.0046(17) C3 0.051(3) 0.020(2) 0.039(2) 0.0006(18) 0.002(2) -0.0022(19) C4 0.039(2) 0.027(2) 0.037(2) 0.0001(18) 0.0036(19) -0.0109(18) C5 0.025(2) 0.029(2) 0.031(2) -0.0015(17) 0.0003(16) -0.0065(16) C6 0.0238(19) 0.0223(19) 0.0210(18) -0.0038(15) -0.0033(15) -0.0033(15) C7 0.027(2) 0.031(2) 0.027(2) -0.0012(17) 0.0014(16) -0.0013(16) C8 0.028(3) 0.100(5) 0.091(5) 0.046(4) 0.001(3) -0.004(3) C9 0.056(3) 0.105(5) 0.029(3) 0.001(3) 0.004(2) -0.029(3) C10 0.027(2) 0.038(2) 0.042(2) -0.0001(19) 0.0054(18) -0.0043(18) C11 0.031(3) 0.085(4) 0.061(3) -0.018(3) 0.002(2) -0.001(3) C12 0.039(3) 0.063(3) 0.048(3) -0.011(3) 0.009(2) 0.004(2) C13 0.0221(18) 0.0208(19) 0.0227(18) 0.0018(15) 0.0009(15) 0.0007(14) C14 0.034(2) 0.025(2) 0.025(2) 0.0056(16) -0.0039(16) 0.0025(17) C15 0.071(4) 0.041(3) 0.041(3) 0.005(2) -0.024(2) 0.009(2) C16 0.046(3) 0.031(2) 0.044(3) 0.0056(19) 0.001(2) 0.014(2) C17 0.051(3) 0.037(3) 0.045(3) 0.018(2) 0.011(2) 0.005(2) C18 0.029(2) 0.0206(19) 0.0251(19) 0.0028(15) -0.0010(16) -0.0007(15) C19 0.033(2) 0.023(2) 0.029(2) 0.0009(16) 0.0010(17) 0.0012(16) C20 0.056(3) 0.030(2) 0.031(2) -0.0086(18) 0.007(2) 0.000(2) C21 0.062(3) 0.034(3) 0.047(3) -0.017(2) 0.002(2) -0.017(2) C22 0.041(3) 0.041(3) 0.047(3) -0.007(2) 0.002(2) -0.018(2) C23 0.035(2) 0.023(2) 0.031(2) -0.0003(16) -0.0001(17) -0.0045(17) C24 0.033(2) 0.034(2) 0.032(2) -0.0029(18) 0.0057(17) 0.0027(18) C25 0.049(3) 0.045(3) 0.035(2) 0.001(2) 0.009(2) -0.006(2) C26 0.045(3) 0.055(3) 0.055(3) -0.010(3) 0.008(2) 0.014(2) C27 0.036(2) 0.037(2) 0.035(2) -0.0004(19) 0.0083(19) -0.0083(19) C28 0.051(3) 0.054(3) 0.051(3) 0.001(2) 0.016(2) -0.018(2) C29 0.041(3) 0.069(4) 0.058(3) 0.005(3) 0.010(2) 0.009(3) O2 0.0482(19) 0.0431(19) 0.0400(18) 0.0007(14) -0.0014(15) 0.0169(15) C34 0.045(3) 0.049(3) 0.045(3) -0.003(2) -0.007(2) 0.004(2) C35 0.048(3) 0.048(3) 0.052(3) 0.011(2) -0.007(2) 0.007(2) C36 0.034(2) 0.038(3) 0.056(3) 0.001(2) -0.001(2) 0.0090(19) C37 0.041(3) 0.039(3) 0.046(3) 0.002(2) -0.001(2) 0.009(2) O3 0.064(2) 0.058(2) 0.0319(17) 0.0001(15) -0.0069(16) 0.0083(18) C38 0.059(4) 0.091(5) 0.045(3) 0.030(3) -0.008(3) 0.008(3) C39 0.073(4) 0.057(4) 0.102(5) -0.018(4) -0.027(4) 0.012(3) C40 0.127(6) 0.091(5) 0.037(3) -0.008(3) -0.020(4) 0.056(5) C41 0.065(4) 0.085(4) 0.034(3) 0.008(3) -0.003(2) 0.005(3) O1 0.056(4) 0.041(4) 0.043(4) 0.013(3) 0.009(3) -0.006(3) C30 0.060(5) 0.047(4) 0.050(5) 0.006(4) -0.001(4) 0.000(4) C31 0.061(5) 0.050(4) 0.071(5) 0.016(4) 0.001(4) -0.005(4) C32 0.066(5) 0.083(5) 0.082(5) 0.004(5) 0.009(5) -0.006(5) C33 0.068(5) 0.069(5) 0.067(5) 0.010(4) 0.018(4) 0.010(4) O1' 0.069(5) 0.035(3) 0.048(4) 0.000(3) 0.021(4) -0.006(3) C30' 0.066(5) 0.044(4) 0.055(5) 0.011(4) -0.002(4) 0.005(4) C31' 0.074(5) 0.054(4) 0.072(5) 0.017(4) 0.002(5) -0.005(4) C32' 0.063(5) 0.065(4) 0.068(5) 0.009(4) 0.021(4) -0.002(4) C33' 0.065(5) 0.057(4) 0.057(5) -0.001(4) 0.018(4) 0.005(4) O4 0.097(5) 0.079(5) 0.080(4) -0.007(4) 0.022(4) -0.013(4) C42 0.102(5) 0.052(4) 0.045(4) -0.011(4) 0.014(4) -0.019(4) C43 0.105(5) 0.077(5) 0.068(5) -0.014(4) 0.017(4) -0.008(4) C44 0.094(5) 0.077(4) 0.075(5) -0.012(4) 0.014(4) -0.007(4) C45 0.091(5) 0.076(4) 0.077(5) -0.009(4) 0.012(4) -0.014(4) O4' 0.099(5) 0.075(5) 0.076(5) -0.005(4) 0.021(4) -0.013(4) C42' 0.096(6) 0.069(6) 0.071(6) -0.013(5) 0.022(5) -0.008(5) C43' 0.097(6) 0.075(5) 0.083(6) -0.014(5) 0.012(5) 0.002(5) C44' 0.095(5) 0.078(5) 0.079(5) -0.006(5) 0.013(5) -0.006(5) C45' 0.096(5) 0.078(5) 0.080(5) -0.006(4) 0.017(4) -0.010(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 P1 C13 1.790(4) . ? P1 C18 1.856(4) . ? P1 K1 3.1718(17) . ? K1 O1' 2.620(9) . ? K1 O2 2.651(3) . ? K1 O3 2.712(3) . ? K1 O1 2.750(9) . ? K1 C4 3.124(4) . ? K1 C3 3.197(4) . ? K1 C5 3.199(4) . ? K1 C2 3.318(4) . ? K1 C6 3.351(4) . ? K1 C1 3.396(4) . ? K1 C38 3.535(5) . ? N1 C13 1.304(5) . ? N1 C6 1.402(5) . ? C1 C2 1.392(6) . ? C1 C6 1.415(5) . ? C1 C7 1.518(5) . ? C2 C3 1.387(6) . ? C2 H2 1.0000 . ? C3 C4 1.388(6) . ? C3 H3 1.0000 . ? C4 C5 1.391(6) . ? C4 H4 1.0000 . ? C5 C6 1.417(5) . ? C5 C10 1.517(6) . ? C7 C8 1.514(6) . ? C7 C9 1.517(6) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.513(6) . ? C10 C12 1.525(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.546(5) . ? C14 C17 1.518(6) . ? C14 C15 1.533(6) . ? C14 C16 1.534(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.416(5) . ? C18 C19 1.427(5) . ? C19 C20 1.387(6) . ? C19 C24 1.518(6) . ? C20 C21 1.383(7) . ? C20 H20 0.9500 . ? C21 C22 1.373(7) . ? C21 H21 0.9500 . ? C22 C23 1.391(6) . ? C22 H22 0.9500 . ? C23 C27 1.529(6) . ? C24 C26 1.531(6) . ? C24 C25 1.533(6) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.528(7) . ? C27 C28 1.530(6) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? O2 C34 1.424(6) . ? O2 C37 1.428(5) . ? C34 C35 1.517(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.519(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.510(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? O3 C41 1.394(5) . ? O3 C38 1.510(6) . ? C38 C39 1.441(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.527(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.527(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? O1 C33 1.417(9) . ? O1 C30 1.502(9) . ? C30 C31 1.493(9) . ? C30 H30C 0.9900 . ? C30 H30D 0.9900 . ? C31 C32 1.538(9) . ? C31 H31C 0.9900 . ? C31 H31D 0.9900 . ? C32 C33 1.447(10) . ? C32 H32C 0.9900 . ? C32 H32D 0.9900 . ? C33 H33C 0.9900 . ? C33 H33D 0.9900 . ? O1' C30' 1.409(10) . ? O1' C33' 1.417(9) . ? C30' C31' 1.524(10) . ? C30' H30A 0.9900 . ? C30' H30B 0.9900 . ? C31' C32' 1.573(10) . ? C31' H31A 0.9900 . ? C31' H31B 0.9900 . ? C32' C33' 1.446(9) . ? C32' H32A 0.9900 . ? C32' H32B 0.9900 . ? C33' H33A 0.9900 . ? C33' H33B 0.9900 . ? O4 C42 1.420(9) . ? O4 C45 1.485(10) . ? C42 C43 1.519(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.537(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.523(10) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? O4' C42' 1.434(11) . ? O4' C45' 1.469(11) . ? C42' C43' 1.464(10) . ? C42' H42C 0.9900 . ? C42' H42D 0.9900 . ? C43' C44' 1.524(11) . ? C43' H43C 0.9900 . ? C43' H43D 0.9900 . ? C44' C45' 1.517(11) . ? C44' H44C 0.9900 . ? C44' H44D 0.9900 . ? C45' H45C 0.9900 . ? C45' H45D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 P1 C18 113.19(17) . . ? C13 P1 K1 120.13(12) . . ? C18 P1 K1 125.12(12) . . ? O1' K1 O2 84.8(2) . . ? O1' K1 O3 75.3(2) . . ? O2 K1 O3 86.59(11) . . ? O1' K1 O1 12.5(3) . . ? O2 K1 O1 91.40(19) . . ? O3 K1 O1 86.3(2) . . ? O1' K1 C4 85.2(3) . . ? O2 K1 C4 113.95(12) . . ? O3 K1 C4 150.43(12) . . ? O1 K1 C4 72.8(2) . . ? O1' K1 P1 144.72(19) . . ? O2 K1 P1 126.93(8) . . ? O3 K1 P1 90.11(8) . . ? O1 K1 P1 141.23(18) . . ? C4 K1 P1 93.37(9) . . ? O1' K1 C3 90.3(2) . . ? O2 K1 C3 89.79(11) . . ? O3 K1 C3 165.39(11) . . ? O1 K1 C3 79.7(2) . . ? C4 K1 C3 25.34(11) . . ? P1 K1 C3 103.33(9) . . ? O1' K1 C5 103.0(3) . . ? O2 K1 C5 132.86(11) . . ? O3 K1 C5 140.53(11) . . ? O1 K1 C5 90.8(2) . . ? C4 K1 C5 25.39(11) . . ? P1 K1 C5 68.37(7) . . ? C3 K1 C5 44.55(11) . . ? O1' K1 C2 113.0(2) . . ? O2 K1 C2 83.11(10) . . ? O3 K1 C2 166.02(11) . . ? O1 K1 C2 103.4(2) . . ? C4 K1 C2 43.55(11) . . ? P1 K1 C2 88.56(8) . . ? C3 K1 C2 24.50(10) . . ? C5 K1 C2 50.74(10) . . ? O1' K1 C6 127.4(3) . . ? O2 K1 C6 122.19(10) . . ? O3 K1 C6 141.65(10) . . ? O1 K1 C6 114.9(2) . . ? C4 K1 C6 43.70(10) . . ? P1 K1 C6 53.01(7) . . ? C3 K1 C6 50.59(10) . . ? C5 K1 C6 24.85(9) . . ? C2 K1 C6 42.51(10) . . ? O1' K1 C1 132.9(2) . . ? O2 K1 C1 98.02(10) . . ? O3 K1 C1 151.58(10) . . ? O1 K1 C1 121.4(2) . . ? C4 K1 C1 50.54(10) . . ? P1 K1 C1 64.67(7) . . ? C3 K1 C1 43.01(10) . . ? C5 K1 C1 43.49(10) . . ? C2 K1 C1 23.89(10) . . ? C6 K1 C1 24.19(9) . . ? O1' K1 C38 98.3(3) . . ? O2 K1 C38 83.21(13) . . ? O3 K1 C38 23.61(10) . . ? O1 K1 C38 109.7(2) . . ? C4 K1 C38 162.78(13) . . ? P1 K1 C38 74.00(9) . . ? C3 K1 C38 168.38(12) . . ? C5 K1 C38 139.06(12) . . ? C2 K1 C38 144.41(12) . . ? C6 K1 C38 126.70(11) . . ? C1 K1 C38 128.79(11) . . ? C13 N1 C6 121.5(3) . . ? C2 C1 C6 119.0(4) . . ? C2 C1 C7 121.3(4) . . ? C6 C1 C7 119.7(3) . . ? C2 C1 K1 74.9(2) . . ? C6 C1 K1 76.1(2) . . ? C7 C1 K1 121.1(2) . . ? C3 C2 C1 121.4(4) . . ? C3 C2 K1 72.9(2) . . ? C1 C2 K1 81.2(2) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? K1 C2 H2 119.3 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 K1 82.6(2) . . ? C4 C3 K1 74.4(2) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? K1 C3 H3 120.1 . . ? C3 C4 C5 121.4(4) . . ? C3 C4 K1 80.3(3) . . ? C5 C4 K1 80.3(2) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? K1 C4 H4 118.9 . . ? C4 C5 C6 118.9(4) . . ? C4 C5 C10 120.3(4) . . ? C6 C5 C10 120.7(4) . . ? C4 C5 K1 74.3(2) . . ? C6 C5 K1 83.6(2) . . ? C10 C5 K1 113.5(3) . . ? N1 C6 C1 120.1(3) . . ? N1 C6 C5 119.7(3) . . ? C1 C6 C5 119.8(3) . . ? N1 C6 K1 125.8(2) . . ? C1 C6 K1 79.7(2) . . ? C5 C6 K1 71.6(2) . . ? C8 C7 C9 111.1(4) . . ? C8 C7 C1 113.1(4) . . ? C9 C7 C1 110.8(3) . . ? C8 C7 H7 107.2 . . ? C9 C7 H7 107.2 . . ? C1 C7 H7 107.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C5 110.5(4) . . ? C11 C10 C12 110.4(4) . . ? C5 C10 C12 112.3(4) . . ? C11 C10 H10 107.8 . . ? C5 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 113.8(3) . . ? N1 C13 P1 118.5(3) . . ? C14 C13 P1 127.6(3) . . ? C17 C14 C15 109.2(4) . . ? C17 C14 C16 109.8(4) . . ? C15 C14 C16 106.7(4) . . ? C17 C14 C13 109.2(3) . . ? C15 C14 C13 110.4(3) . . ? C16 C14 C13 111.4(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 118.2(3) . . ? C23 C18 P1 120.0(3) . . ? C19 C18 P1 120.4(3) . . ? C20 C19 C18 119.9(4) . . ? C20 C19 C24 118.2(4) . . ? C18 C19 C24 121.8(3) . . ? C21 C20 C19 121.1(4) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 119.5(4) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 121.9(4) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C22 C23 C18 119.5(4) . . ? C22 C23 C27 118.2(4) . . ? C18 C23 C27 122.3(4) . . ? C19 C24 C26 113.4(4) . . ? C19 C24 C25 110.4(4) . . ? C26 C24 C25 109.9(4) . . ? C19 C24 H24 107.6 . . ? C26 C24 H24 107.6 . . ? C25 C24 H24 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C23 111.1(4) . . ? C29 C27 C28 109.8(4) . . ? C23 C27 C28 113.0(4) . . ? C29 C27 H27 107.6 . . ? C23 C27 H27 107.6 . . ? C28 C27 H27 107.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C34 O2 C37 109.8(3) . . ? C34 O2 K1 119.6(3) . . ? C37 O2 K1 125.3(3) . . ? O2 C34 C35 105.6(4) . . ? O2 C34 H34A 110.6 . . ? C35 C34 H34A 110.6 . . ? O2 C34 H34B 110.6 . . ? C35 C34 H34B 110.6 . . ? H34A C34 H34B 108.7 . . ? C34 C35 C36 102.0(4) . . ? C34 C35 H35A 111.4 . . ? C36 C35 H35A 111.4 . . ? C34 C35 H35B 111.4 . . ? C36 C35 H35B 111.4 . . ? H35A C35 H35B 109.2 . . ? C37 C36 C35 101.6(4) . . ? C37 C36 H36A 111.5 . . ? C35 C36 H36A 111.5 . . ? C37 C36 H36B 111.5 . . ? C35 C36 H36B 111.5 . . ? H36A C36 H36B 109.3 . . ? O2 C37 C36 106.8(4) . . ? O2 C37 H37A 110.4 . . ? C36 C37 H37A 110.4 . . ? O2 C37 H37B 110.4 . . ? C36 C37 H37B 110.4 . . ? H37A C37 H37B 108.6 . . ? C41 O3 C38 106.5(4) . . ? C41 O3 K1 142.9(3) . . ? C38 O3 K1 110.4(2) . . ? C39 C38 O3 106.2(4) . . ? C39 C38 K1 143.9(4) . . ? O3 C38 K1 45.99(18) . . ? C39 C38 H38A 110.5 . . ? O3 C38 H38A 110.5 . . ? K1 C38 H38A 71.2 . . ? C39 C38 H38B 110.5 . . ? O3 C38 H38B 110.5 . . ? K1 C38 H38B 102.2 . . ? H38A C38 H38B 108.7 . . ? C38 C39 C40 106.5(4) . . ? C38 C39 H39A 110.4 . . ? C40 C39 H39A 110.4 . . ? C38 C39 H39B 110.4 . . ? C40 C39 H39B 110.4 . . ? H39A C39 H39B 108.6 . . ? C39 C40 C41 104.8(4) . . ? C39 C40 H40A 110.8 . . ? C41 C40 H40A 110.8 . . ? C39 C40 H40B 110.8 . . ? C41 C40 H40B 110.8 . . ? H40A C40 H40B 108.9 . . ? O3 C41 C40 106.2(4) . . ? O3 C41 H41A 110.5 . . ? C40 C41 H41A 110.5 . . ? O3 C41 H41B 110.5 . . ? C40 C41 H41B 110.5 . . ? H41A C41 H41B 108.7 . . ? C33 O1 C30 114.6(9) . . ? C33 O1 K1 124.3(6) . . ? C30 O1 K1 115.2(6) . . ? C31 C30 O1 102.6(8) . . ? C31 C30 H30C 111.2 . . ? O1 C30 H30C 111.2 . . ? C31 C30 H30D 111.2 . . ? O1 C30 H30D 111.2 . . ? H30C C30 H30D 109.2 . . ? C30 C31 C32 104.9(7) . . ? C30 C31 H31C 110.8 . . ? C32 C31 H31C 110.8 . . ? C30 C31 H31D 110.8 . . ? C32 C31 H31D 110.8 . . ? H31C C31 H31D 108.8 . . ? C33 C32 C31 110.3(7) . . ? C33 C32 H32C 109.6 . . ? C31 C32 H32C 109.6 . . ? C33 C32 H32D 109.6 . . ? C31 C32 H32D 109.6 . . ? H32C C32 H32D 108.1 . . ? O1 C33 C32 101.4(8) . . ? O1 C33 H33C 111.5 . . ? C32 C33 H33C 111.5 . . ? O1 C33 H33D 111.5 . . ? C32 C33 H33D 111.5 . . ? H33C C33 H33D 109.3 . . ? C30' O1' C33' 111.9(9) . . ? C30' O1' K1 124.0(7) . . ? C33' O1' K1 122.8(6) . . ? O1' C30' C31' 108.0(8) . . ? O1' C30' H30A 110.1 . . ? C31' C30' H30A 110.1 . . ? O1' C30' H30B 110.1 . . ? C31' C30' H30B 110.1 . . ? H30A C30' H30B 108.4 . . ? C30' C31' C32' 103.9(7) . . ? C30' C31' H31A 111.0 . . ? C32' C31' H31A 111.0 . . ? C30' C31' H31B 111.0 . . ? C32' C31' H31B 111.0 . . ? H31A C31' H31B 109.0 . . ? C33' C32' C31' 105.9(6) . . ? C33' C32' H32A 110.5 . . ? C31' C32' H32A 110.5 . . ? C33' C32' H32B 110.5 . . ? C31' C32' H32B 110.6 . . ? H32A C32' H32B 108.7 . . ? O1' C33' C32' 110.1(8) . . ? O1' C33' H33A 109.6 . . ? C32' C33' H33A 109.6 . . ? O1' C33' H33B 109.6 . . ? C32' C33' H33B 109.6 . . ? H33A C33' H33B 108.2 . . ? C42 O4 C45 111.7(9) . . ? O4 C42 C43 105.6(8) . . ? O4 C42 H42A 110.6 . . ? C43 C42 H42A 110.6 . . ? O4 C42 H42B 110.6 . . ? C43 C42 H42B 110.6 . . ? H42A C42 H42B 108.7 . . ? C42 C43 C44 105.6(7) . . ? C42 C43 H43A 110.6 . . ? C44 C43 H43A 110.6 . . ? C42 C43 H43B 110.6 . . ? C44 C43 H43B 110.6 . . ? H43A C43 H43B 108.8 . . ? C45 C44 C43 103.9(7) . . ? C45 C44 H44A 111.0 . . ? C43 C44 H44A 111.0 . . ? C45 C44 H44B 111.0 . . ? C43 C44 H44B 111.0 . . ? H44A C44 H44B 109.0 . . ? O4 C45 C44 106.0(8) . . ? O4 C45 H45A 110.5 . . ? C44 C45 H45A 110.5 . . ? O4 C45 H45B 110.5 . . ? C44 C45 H45B 110.5 . . ? H45A C45 H45B 108.7 . . ? C42' O4' C45' 119.2(14) . . ? O4' C42' C43' 98.8(12) . . ? O4' C42' H42C 112.0 . . ? C43' C42' H42C 112.0 . . ? O4' C42' H42D 112.0 . . ? C43' C42' H42D 112.0 . . ? H42C C42' H42D 109.7 . . ? C42' C43' C44' 110.4(8) . . ? C42' C43' H43C 109.6 . . ? C44' C43' H43C 109.6 . . ? C42' C43' H43D 109.6 . . ? C44' C43' H43D 109.6 . . ? H43C C43' H43D 108.1 . . ? C45' C44' C43' 107.3(9) . . ? C45' C44' H44C 110.3 . . ? C43' C44' H44C 110.3 . . ? C45' C44' H44D 110.3 . . ? C43' C44' H44D 110.3 . . ? H44C C44' H44D 108.5 . . ? O4' C45' C44' 99.0(12) . . ? O4' C45' H45C 112.0 . . ? C44' C45' H45C 112.0 . . ? O4' C45' H45D 112.0 . . ? C44' C45' H45D 112.0 . . ? H45C C45' H45D 109.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 P1 K1 O1' 96.5(5) . . . . ? C18 P1 K1 O1' -68.2(5) . . . . ? C13 P1 K1 O2 -113.53(17) . . . . ? C18 P1 K1 O2 81.71(18) . . . . ? C13 P1 K1 O3 160.66(16) . . . . ? C18 P1 K1 O3 -4.10(17) . . . . ? C13 P1 K1 O1 76.5(4) . . . . ? C18 P1 K1 O1 -88.3(4) . . . . ? C13 P1 K1 C4 10.04(16) . . . . ? C18 P1 K1 C4 -154.72(17) . . . . ? C13 P1 K1 C3 -13.55(16) . . . . ? C18 P1 K1 C3 -178.31(17) . . . . ? C13 P1 K1 C5 14.59(16) . . . . ? C18 P1 K1 C5 -150.17(17) . . . . ? C13 P1 K1 C2 -33.26(16) . . . . ? C18 P1 K1 C2 161.98(17) . . . . ? C13 P1 K1 C6 -7.97(16) . . . . ? C18 P1 K1 C6 -172.73(18) . . . . ? C13 P1 K1 C1 -32.89(15) . . . . ? C18 P1 K1 C1 162.35(17) . . . . ? C13 P1 K1 C38 178.15(17) . . . . ? C18 P1 K1 C38 13.39(18) . . . . ? O1' K1 C1 C2 38.4(4) . . . . ? O2 K1 C1 C2 -51.9(3) . . . . ? O3 K1 C1 C2 -149.6(3) . . . . ? O1 K1 C1 C2 44.7(3) . . . . ? C4 K1 C1 C2 62.6(2) . . . . ? P1 K1 C1 C2 -179.1(3) . . . . ? C3 K1 C1 C2 29.1(2) . . . . ? C5 K1 C1 C2 96.3(3) . . . . ? C6 K1 C1 C2 125.7(4) . . . . ? C38 K1 C1 C2 -139.6(3) . . . . ? O1' K1 C1 C6 -87.3(4) . . . . ? O2 K1 C1 C6 -177.6(2) . . . . ? O3 K1 C1 C6 84.7(3) . . . . ? O1 K1 C1 C6 -81.0(3) . . . . ? C4 K1 C1 C6 -63.1(2) . . . . ? P1 K1 C1 C6 55.2(2) . . . . ? C3 K1 C1 C6 -96.6(3) . . . . ? C5 K1 C1 C6 -29.4(2) . . . . ? C2 K1 C1 C6 -125.7(3) . . . . ? C38 K1 C1 C6 94.7(2) . . . . ? O1' K1 C1 C7 156.1(4) . . . . ? O2 K1 C1 C7 65.8(3) . . . . ? O3 K1 C1 C7 -31.9(4) . . . . ? O1 K1 C1 C7 162.4(3) . . . . ? C4 K1 C1 C7 -179.7(3) . . . . ? P1 K1 C1 C7 -61.4(3) . . . . ? C3 K1 C1 C7 146.8(3) . . . . ? C5 K1 C1 C7 -146.0(3) . . . . ? C2 K1 C1 C7 117.7(4) . . . . ? C6 K1 C1 C7 -116.6(4) . . . . ? C38 K1 C1 C7 -21.9(3) . . . . ? C6 C1 C2 C3 0.6(6) . . . . ? C7 C1 C2 C3 178.8(4) . . . . ? K1 C1 C2 C3 -63.7(4) . . . . ? C6 C1 C2 K1 64.3(3) . . . . ? C7 C1 C2 K1 -117.5(3) . . . . ? O1' K1 C2 C3 -23.5(4) . . . . ? O2 K1 C2 C3 -104.8(3) . . . . ? O3 K1 C2 C3 -147.7(4) . . . . ? O1 K1 C2 C3 -15.0(3) . . . . ? C4 K1 C2 C3 31.3(2) . . . . ? P1 K1 C2 C3 127.7(3) . . . . ? C5 K1 C2 C3 64.8(3) . . . . ? C6 K1 C2 C3 97.4(3) . . . . ? C1 K1 C2 C3 126.9(4) . . . . ? C38 K1 C2 C3 -172.9(3) . . . . ? O1' K1 C2 C1 -150.4(3) . . . . ? O2 K1 C2 C1 128.3(3) . . . . ? O3 K1 C2 C1 85.5(5) . . . . ? O1 K1 C2 C1 -141.9(3) . . . . ? C4 K1 C2 C1 -95.6(3) . . . . ? P1 K1 C2 C1 0.8(2) . . . . ? C3 K1 C2 C1 -126.9(4) . . . . ? C5 K1 C2 C1 -62.1(2) . . . . ? C6 K1 C2 C1 -29.5(2) . . . . ? C38 K1 C2 C1 60.2(3) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? K1 C2 C3 C4 -67.4(4) . . . . ? C1 C2 C3 K1 68.0(4) . . . . ? O1' K1 C3 C2 158.5(3) . . . . ? O2 K1 C3 C2 73.7(3) . . . . ? O3 K1 C3 C2 149.2(4) . . . . ? O1 K1 C3 C2 165.1(3) . . . . ? C4 K1 C3 C2 -123.3(4) . . . . ? P1 K1 C3 C2 -54.4(3) . . . . ? C5 K1 C3 C2 -93.1(3) . . . . ? C6 K1 C3 C2 -60.2(2) . . . . ? C1 K1 C3 C2 -28.4(2) . . . . ? C38 K1 C3 C2 20.9(7) . . . . ? O1' K1 C3 C4 -78.2(3) . . . . ? O2 K1 C3 C4 -163.0(3) . . . . ? O3 K1 C3 C4 -87.5(5) . . . . ? O1 K1 C3 C4 -71.5(3) . . . . ? P1 K1 C3 C4 68.9(2) . . . . ? C5 K1 C3 C4 30.3(2) . . . . ? C2 K1 C3 C4 123.3(4) . . . . ? C6 K1 C3 C4 63.2(2) . . . . ? C1 K1 C3 C4 95.0(3) . . . . ? C38 K1 C3 C4 144.2(6) . . . . ? C2 C3 C4 C5 -0.4(7) . . . . ? K1 C3 C4 C5 -72.3(4) . . . . ? C2 C3 C4 K1 71.9(4) . . . . ? O1' K1 C4 C3 100.8(3) . . . . ? O2 K1 C4 C3 18.7(3) . . . . ? O3 K1 C4 C3 149.3(3) . . . . ? O1 K1 C4 C3 102.4(3) . . . . ? P1 K1 C4 C3 -114.5(2) . . . . ? C5 K1 C4 C3 -124.4(4) . . . . ? C2 K1 C4 C3 -30.2(2) . . . . ? C6 K1 C4 C3 -93.6(3) . . . . ? C1 K1 C4 C3 -61.7(2) . . . . ? C38 K1 C4 C3 -156.5(4) . . . . ? O1' K1 C4 C5 -134.8(3) . . . . ? O2 K1 C4 C5 143.1(2) . . . . ? O3 K1 C4 C5 -86.3(3) . . . . ? O1 K1 C4 C5 -133.2(3) . . . . ? P1 K1 C4 C5 9.9(2) . . . . ? C3 K1 C4 C5 124.4(4) . . . . ? C2 K1 C4 C5 94.3(3) . . . . ? C6 K1 C4 C5 30.9(2) . . . . ? C1 K1 C4 C5 62.8(2) . . . . ? C38 K1 C4 C5 -32.1(5) . . . . ? C3 C4 C5 C6 -1.0(6) . . . . ? K1 C4 C5 C6 -73.2(3) . . . . ? C3 C4 C5 C10 -179.4(4) . . . . ? K1 C4 C5 C10 108.4(4) . . . . ? C3 C4 C5 K1 72.3(4) . . . . ? O1' K1 C5 C4 46.6(3) . . . . ? O2 K1 C5 C4 -48.4(3) . . . . ? O3 K1 C5 C4 129.2(3) . . . . ? O1 K1 C5 C4 44.2(3) . . . . ? P1 K1 C5 C4 -169.4(3) . . . . ? C3 K1 C5 C4 -30.2(2) . . . . ? C2 K1 C5 C4 -62.5(2) . . . . ? C6 K1 C5 C4 -122.5(4) . . . . ? C1 K1 C5 C4 -93.9(3) . . . . ? C38 K1 C5 C4 166.1(2) . . . . ? O1' K1 C5 C6 169.1(3) . . . . ? O2 K1 C5 C6 74.1(3) . . . . ? O3 K1 C5 C6 -108.3(2) . . . . ? O1 K1 C5 C6 166.7(3) . . . . ? C4 K1 C5 C6 122.5(4) . . . . ? P1 K1 C5 C6 -46.8(2) . . . . ? C3 K1 C5 C6 92.3(3) . . . . ? C2 K1 C5 C6 60.0(2) . . . . ? C1 K1 C5 C6 28.6(2) . . . . ? C38 K1 C5 C6 -71.4(3) . . . . ? O1' K1 C5 C10 -70.1(3) . . . . ? O2 K1 C5 C10 -165.1(2) . . . . ? O3 K1 C5 C10 12.5(4) . . . . ? O1 K1 C5 C10 -72.5(3) . . . . ? C4 K1 C5 C10 -116.7(4) . . . . ? P1 K1 C5 C10 73.9(3) . . . . ? C3 K1 C5 C10 -146.9(3) . . . . ? C2 K1 C5 C10 -179.2(3) . . . . ? C6 K1 C5 C10 120.8(4) . . . . ? C1 K1 C5 C10 149.4(3) . . . . ? C38 K1 C5 C10 49.4(3) . . . . ? C13 N1 C6 C1 93.4(4) . . . . ? C13 N1 C6 C5 -93.9(4) . . . . ? C13 N1 C6 K1 -6.1(5) . . . . ? C2 C1 C6 N1 170.7(3) . . . . ? C7 C1 C6 N1 -7.5(5) . . . . ? K1 C1 C6 N1 -125.6(3) . . . . ? C2 C1 C6 C5 -2.0(5) . . . . ? C7 C1 C6 C5 179.8(3) . . . . ? K1 C1 C6 C5 61.7(3) . . . . ? C2 C1 C6 K1 -63.6(3) . . . . ? C7 C1 C6 K1 118.1(3) . . . . ? C4 C5 C6 N1 -170.6(3) . . . . ? C10 C5 C6 N1 7.8(5) . . . . ? K1 C5 C6 N1 121.4(3) . . . . ? C4 C5 C6 C1 2.1(6) . . . . ? C10 C5 C6 C1 -179.5(3) . . . . ? K1 C5 C6 C1 -65.9(3) . . . . ? C4 C5 C6 K1 68.0(3) . . . . ? C10 C5 C6 K1 -113.6(4) . . . . ? O1' K1 C6 N1 -127.2(3) . . . . ? O2 K1 C6 N1 122.7(3) . . . . ? O3 K1 C6 N1 -10.4(4) . . . . ? O1 K1 C6 N1 -128.4(3) . . . . ? C4 K1 C6 N1 -145.3(3) . . . . ? P1 K1 C6 N1 8.2(2) . . . . ? C3 K1 C6 N1 -178.9(3) . . . . ? C5 K1 C6 N1 -113.7(4) . . . . ? C2 K1 C6 N1 149.0(3) . . . . ? C1 K1 C6 N1 119.8(4) . . . . ? C38 K1 C6 N1 15.5(3) . . . . ? O1' K1 C6 C1 113.0(3) . . . . ? O2 K1 C6 C1 2.8(3) . . . . ? O3 K1 C6 C1 -130.2(2) . . . . ? O1 K1 C6 C1 111.7(3) . . . . ? C4 K1 C6 C1 94.9(3) . . . . ? P1 K1 C6 C1 -111.7(2) . . . . ? C3 K1 C6 C1 61.3(2) . . . . ? C5 K1 C6 C1 126.4(3) . . . . ? C2 K1 C6 C1 29.1(2) . . . . ? C38 K1 C6 C1 -104.3(2) . . . . ? O1' K1 C6 C5 -13.4(3) . . . . ? O2 K1 C6 C5 -123.6(2) . . . . ? O3 K1 C6 C5 103.4(3) . . . . ? O1 K1 C6 C5 -14.7(3) . . . . ? C4 K1 C6 C5 -31.6(2) . . . . ? P1 K1 C6 C5 121.9(2) . . . . ? C3 K1 C6 C5 -65.1(2) . . . . ? C2 K1 C6 C5 -97.3(3) . . . . ? C1 K1 C6 C5 -126.4(3) . . . . ? C38 K1 C6 C5 129.2(2) . . . . ? C2 C1 C7 C8 35.7(6) . . . . ? C6 C1 C7 C8 -146.1(4) . . . . ? K1 C1 C7 C8 -54.9(5) . . . . ? C2 C1 C7 C9 -89.8(5) . . . . ? C6 C1 C7 C9 88.4(5) . . . . ? K1 C1 C7 C9 179.6(3) . . . . ? C4 C5 C10 C11 67.1(5) . . . . ? C6 C5 C10 C11 -111.2(5) . . . . ? K1 C5 C10 C11 152.1(3) . . . . ? C4 C5 C10 C12 -56.6(5) . . . . ? C6 C5 C10 C12 125.0(4) . . . . ? K1 C5 C10 C12 28.3(4) . . . . ? C6 N1 C13 C14 -180.0(3) . . . . ? C6 N1 C13 P1 -2.9(5) . . . . ? C18 P1 C13 N1 177.0(3) . . . . ? K1 P1 C13 N1 10.5(3) . . . . ? C18 P1 C13 C14 -6.4(4) . . . . ? K1 P1 C13 C14 -172.8(3) . . . . ? N1 C13 C14 C17 113.0(4) . . . . ? P1 C13 C14 C17 -63.8(4) . . . . ? N1 C13 C14 C15 -7.2(5) . . . . ? P1 C13 C14 C15 176.0(3) . . . . ? N1 C13 C14 C16 -125.5(4) . . . . ? P1 C13 C14 C16 57.7(5) . . . . ? C13 P1 C18 C23 103.5(3) . . . . ? K1 P1 C18 C23 -90.8(3) . . . . ? C13 P1 C18 C19 -90.7(3) . . . . ? K1 P1 C18 C19 74.9(3) . . . . ? C23 C18 C19 C20 0.1(6) . . . . ? P1 C18 C19 C20 -166.0(3) . . . . ? C23 C18 C19 C24 177.3(4) . . . . ? P1 C18 C19 C24 11.3(5) . . . . ? C18 C19 C20 C21 0.8(7) . . . . ? C24 C19 C20 C21 -176.5(4) . . . . ? C19 C20 C21 C22 -1.1(8) . . . . ? C20 C21 C22 C23 0.4(8) . . . . ? C21 C22 C23 C18 0.5(7) . . . . ? C21 C22 C23 C27 179.4(4) . . . . ? C19 C18 C23 C22 -0.7(6) . . . . ? P1 C18 C23 C22 165.4(3) . . . . ? C19 C18 C23 C27 -179.6(4) . . . . ? P1 C18 C23 C27 -13.5(5) . . . . ? C20 C19 C24 C26 -47.0(5) . . . . ? C18 C19 C24 C26 135.7(4) . . . . ? C20 C19 C24 C25 76.9(5) . . . . ? C18 C19 C24 C25 -100.4(4) . . . . ? C22 C23 C27 C29 -77.3(5) . . . . ? C18 C23 C27 C29 101.6(5) . . . . ? C22 C23 C27 C28 46.6(6) . . . . ? C18 C23 C27 C28 -134.5(4) . . . . ? O1' K1 O2 C34 57.5(4) . . . . ? O3 K1 O2 C34 -18.1(3) . . . . ? O1 K1 O2 C34 68.1(4) . . . . ? C4 K1 O2 C34 139.9(3) . . . . ? P1 K1 O2 C34 -105.6(3) . . . . ? C3 K1 O2 C34 147.8(3) . . . . ? C5 K1 O2 C34 160.5(3) . . . . ? C2 K1 O2 C34 171.4(3) . . . . ? C6 K1 O2 C34 -171.0(3) . . . . ? C1 K1 O2 C34 -169.9(3) . . . . ? C38 K1 O2 C34 -41.5(3) . . . . ? O1' K1 O2 C37 -94.1(4) . . . . ? O3 K1 O2 C37 -169.7(3) . . . . ? O1 K1 O2 C37 -83.5(4) . . . . ? C4 K1 O2 C37 -11.7(4) . . . . ? P1 K1 O2 C37 102.8(3) . . . . ? C3 K1 O2 C37 -3.8(3) . . . . ? C5 K1 O2 C37 8.8(4) . . . . ? C2 K1 O2 C37 19.8(3) . . . . ? C6 K1 O2 C37 37.3(4) . . . . ? C1 K1 O2 C37 38.5(3) . . . . ? C38 K1 O2 C37 166.9(3) . . . . ? C37 O2 C34 C35 14.7(5) . . . . ? K1 O2 C34 C35 -141.0(3) . . . . ? O2 C34 C35 C36 -32.4(5) . . . . ? C34 C35 C36 C37 36.8(5) . . . . ? C34 O2 C37 C36 9.5(5) . . . . ? K1 O2 C37 C36 163.4(3) . . . . ? C35 C36 C37 O2 -29.2(5) . . . . ? O1' K1 O3 C41 7.3(6) . . . . ? O2 K1 O3 C41 92.7(5) . . . . ? O1 K1 O3 C41 1.1(6) . . . . ? C4 K1 O3 C41 -43.2(6) . . . . ? P1 K1 O3 C41 -140.3(5) . . . . ? C3 K1 O3 C41 16.8(8) . . . . ? C5 K1 O3 C41 -85.5(6) . . . . ? C2 K1 O3 C41 135.3(6) . . . . ? C6 K1 O3 C41 -125.6(5) . . . . ? C1 K1 O3 C41 -166.7(5) . . . . ? C38 K1 O3 C41 173.6(7) . . . . ? O1' K1 O3 C38 -166.3(4) . . . . ? O2 K1 O3 C38 -80.8(3) . . . . ? O1 K1 O3 C38 -172.5(3) . . . . ? C4 K1 O3 C38 143.2(3) . . . . ? P1 K1 O3 C38 46.2(3) . . . . ? C3 K1 O3 C38 -156.8(4) . . . . ? C5 K1 O3 C38 100.9(3) . . . . ? C2 K1 O3 C38 -38.3(6) . . . . ? C6 K1 O3 C38 60.9(4) . . . . ? C1 K1 O3 C38 19.7(4) . . . . ? C41 O3 C38 C39 31.2(6) . . . . ? K1 O3 C38 C39 -152.8(4) . . . . ? C41 O3 C38 K1 -176.0(4) . . . . ? O1' K1 C38 C39 61.4(7) . . . . ? O2 K1 C38 C39 145.1(6) . . . . ? O3 K1 C38 C39 48.1(6) . . . . ? O1 K1 C38 C39 56.1(7) . . . . ? C4 K1 C38 C39 -39.3(8) . . . . ? P1 K1 C38 C39 -83.3(6) . . . . ? C3 K1 C38 C39 -161.5(6) . . . . ? C5 K1 C38 C39 -59.6(7) . . . . ? C2 K1 C38 C39 -146.8(6) . . . . ? C6 K1 C38 C39 -89.4(6) . . . . ? C1 K1 C38 C39 -120.0(6) . . . . ? O1' K1 C38 O3 13.4(4) . . . . ? O2 K1 C38 O3 97.0(3) . . . . ? O1 K1 C38 O3 8.0(4) . . . . ? C4 K1 C38 O3 -87.4(5) . . . . ? P1 K1 C38 O3 -131.4(3) . . . . ? C3 K1 C38 O3 150.4(5) . . . . ? C5 K1 C38 O3 -107.7(3) . . . . ? C2 K1 C38 O3 165.1(2) . . . . ? C6 K1 C38 O3 -137.5(3) . . . . ? C1 K1 C38 O3 -168.1(3) . . . . ? O3 C38 C39 C40 -17.8(6) . . . . ? K1 C38 C39 C40 -51.7(8) . . . . ? C38 C39 C40 C41 -0.1(7) . . . . ? C38 O3 C41 C40 -30.7(6) . . . . ? K1 O3 C41 C40 155.5(4) . . . . ? C39 C40 C41 O3 19.5(6) . . . . ? O1' K1 O1 C33 -93.9(18) . . . . ? O2 K1 O1 C33 -151.9(10) . . . . ? O3 K1 O1 C33 -65.4(10) . . . . ? C4 K1 O1 C33 93.4(10) . . . . ? P1 K1 O1 C33 20.1(11) . . . . ? C3 K1 O1 C33 118.6(10) . . . . ? C5 K1 O1 C33 75.2(10) . . . . ? C2 K1 O1 C33 124.8(9) . . . . ? C6 K1 O1 C33 81.3(10) . . . . ? C1 K1 O1 C33 107.8(10) . . . . ? C38 K1 O1 C33 -68.6(10) . . . . ? O1' K1 O1 C30 57.3(15) . . . . ? O2 K1 O1 C30 -0.7(10) . . . . ? O3 K1 O1 C30 85.8(10) . . . . ? C4 K1 O1 C30 -115.3(10) . . . . ? P1 K1 O1 C30 171.3(8) . . . . ? C3 K1 O1 C30 -90.2(10) . . . . ? C5 K1 O1 C30 -133.6(10) . . . . ? C2 K1 O1 C30 -83.9(10) . . . . ? C6 K1 O1 C30 -127.4(9) . . . . ? C1 K1 O1 C30 -100.9(10) . . . . ? C38 K1 O1 C30 82.6(10) . . . . ? C33 O1 C30 C31 -15.5(15) . . . . ? K1 O1 C30 C31 -169.6(9) . . . . ? O1 C30 C31 C32 -0.6(15) . . . . ? C30 C31 C32 C33 15.7(18) . . . . ? C30 O1 C33 C32 24.8(16) . . . . ? K1 O1 C33 C32 176.2(8) . . . . ? C31 C32 C33 O1 -24.0(17) . . . . ? O2 K1 O1' C30' 51.5(13) . . . . ? O3 K1 O1' C30' 139.4(13) . . . . ? O1 K1 O1' C30' -70.1(17) . . . . ? C4 K1 O1' C30' -63.1(13) . . . . ? P1 K1 O1' C30' -152.2(10) . . . . ? C3 K1 O1' C30' -38.2(13) . . . . ? C5 K1 O1' C30' -81.3(13) . . . . ? C2 K1 O1' C30' -28.7(13) . . . . ? C6 K1 O1' C30' -75.6(13) . . . . ? C1 K1 O1' C30' -44.6(14) . . . . ? C38 K1 O1' C30' 133.9(13) . . . . ? O2 K1 O1' C33' -142.8(9) . . . . ? O3 K1 O1' C33' -55.0(9) . . . . ? O1 K1 O1' C33' 95.5(18) . . . . ? C4 K1 O1' C33' 102.6(9) . . . . ? P1 K1 O1' C33' 13.5(12) . . . . ? C3 K1 O1' C33' 127.4(9) . . . . ? C5 K1 O1' C33' 84.3(9) . . . . ? C2 K1 O1' C33' 136.9(9) . . . . ? C6 K1 O1' C33' 90.1(9) . . . . ? C1 K1 O1' C33' 121.1(9) . . . . ? C38 K1 O1' C33' -60.5(9) . . . . ? C33' O1' C30' C31' -3.0(16) . . . . ? K1 O1' C30' C31' 164.0(9) . . . . ? O1' C30' C31' C32' 4.8(15) . . . . ? C30' C31' C32' C33' -4.8(16) . . . . ? C30' O1' C33' C32' -0.2(17) . . . . ? K1 O1' C33' C32' -167.4(9) . . . . ? C31' C32' C33' O1' 3.3(17) . . . . ? C45 O4 C42 C43 15.3(15) . . . . ? O4 C42 C43 C44 -25.7(15) . . . . ? C42 C43 C44 C45 26.0(16) . . . . ? C42 O4 C45 C44 1.2(17) . . . . ? C43 C44 C45 O4 -16.9(17) . . . . ? C45' O4' C42' C43' -24(3) . . . . ? O4' C42' C43' C44' 20(2) . . . . ? C42' C43' C44' C45' -12(3) . . . . ? C42' O4' C45' C44' 18(3) . . . . ? C43' C44' C45' O4' -2(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.084 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.068